#=============================================================================80
# Data Global for compounds 4a, 4b, 4c and 5a
#=============================================================================80
 
data_global

_publ_section_title                                     
;
 Isolation and X-ray characterization of palladium N-complexes in the
 guanylation of aromatic amines. Mechanistic implications
; 
#
# Abdessamad Grirrane, Hermenegildo Garc\'ia, and Eleuterio \'Alvarez 
# 
# 
# 
# To be submitted to Beilstein J. Org. Chem.
# Manuscript number ...........
#=============================================================================80
# Person for contact

_publ_contact_author_name             'Prof. Hermenegildo García'
_publ_contact_author_address
;
 Instituto Universitario de Tecnología Química CSIC-UPV, Universidad
 Politécnica de Valencia, Av.De los Naranjos s/n, 46022 Valencia (Spain).
;
_publ_contact_author_phone        '+34 963 877000 (78572)'
_publ_contact_author_fax          '+34 963 877943'
_publ_contact_author_email     hgarcia@qim.upv.es

#=============================================================================80
# Publication details

loop_
_publ_author_name
_publ_author_address

   'Abdessamad Grirrane' 
;
    Instituto Universitario de Tecnología Química CSIC-UPV, Universidad
    Politécnica de Valencia, Av.De los Naranjos s/n, 46022 Valencia (Spain).
; 
   'Hermenegildo García'
;
    Instituto Universitario de Tecnología Química CSIC-UPV, Universidad
    Politécnica de Valencia, Av.De los Naranjos s/n, 46022 Valencia (Spain).
; 
   'Eleuterio Álvarez'
;
     Instituto de Investigaciones Químicas, C.S.I.C-Universidad de Sevilla,
     Avd. Américo Vespucio, 49., Isla de la Cartuja, E-41092 Sevilla,  Spain  
; 
   
 _publ_requested_journal   'Beilstein J. Org. Chem.'
 _journal_name_full
;
 Beilstein Journal of Organic Chemistry
;

 _journal_volume                '?'
 _journal_page_first            '?'
 _journal_page_last             '?'
 _journal_year                  '2013'


#=========================================================================
# Six crystal structures follow, separated/terminaed by #===END.
# The CIF has been tested by program checkCIF.
#=========================================================================


#=========================================================================
# Data for compound 4a (local labelling  as ea02413x)
#=========================================================================
  
data_4a 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C28 H46 Cl2 N6 O2 Pd' 
_chemical_formula_sum             'C28 H46 Cl2 N6 O2 Pd' 
_chemical_formula_weight          676.01 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pd'  'Pd'  -0.9988   1.0072 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'P 21/c'
_symmetry_space_group_name_Hall    '-P 2ybc'  
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    11.3420(5) 
_cell_length_b                    18.0868(7) 
_cell_length_c                    7.6720(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.4700(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1566.67(11) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     5694 
_cell_measurement_theta_min       2.89 
_cell_measurement_theta_max       30.50 
  
_exptl_crystal_description        prism 
_exptl_crystal_colour             orange 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.433 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              704 
_exptl_absorpt_coefficient_mu     0.798 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8258 
_exptl_absorpt_correction_T_max   0.8869 
_exptl_absorpt_process_details 
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   
;
 Bruker-Nonius X8kappa APEX II CCD area detector
; 
_diffrn_measurement_method        'phi and omega scans with narrow frames' 
_diffrn_detector_area_resol_mean   8.26
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             20959 
_diffrn_reflns_av_R_equivalents   0.0188 
_diffrn_reflns_av_unetI/netI     0.0159 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          1.80 
_diffrn_reflns_theta_max          30.52 
_reflns_number_total              4738 
_reflns_number_gt                 4281 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement        'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction         'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution     'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material   'SHELXTL and publCIF (Westrip, 2010)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0336P)²+0.7100P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4738 
_refine_ls_number_parameters      189 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0271 
_refine_ls_R_factor_gt            0.0239 
_refine_ls_wR_factor_ref          0.0641 
_refine_ls_wR_factor_gt           0.0627 
_refine_ls_goodness_of_fit_ref    1.060 
_refine_ls_restrained_S_all       1.043 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd1 Pd 0.0000 0.0000 0.0000 0.01717(5) Uani 1 2 d SU . . 
Cl1 Cl 0.01006(3) 0.100100(19) -0.18805(4) 0.02740(7) Uani 1 1 d U . . 
O1 O -0.37074(10) 0.19677(7) 0.46223(17) 0.0372(3) Uani 1 1 d U . . 
N1 N 0.02781(9) 0.07090(6) 0.20498(14) 0.0193(2) Uani 1 1 d U . . 
N2 N 0.22744(10) 0.07692(6) 0.17113(14) 0.0205(2) Uani 1 1 d DU . . 
H2N H 0.2040(17) 0.0720(11) 0.0666(19) 0.031 Uiso 1 1 d D . . 
N3 N 0.16080(10) 0.11016(6) 0.43885(14) 0.0201(2) Uani 1 1 d DU . . 
H3N H 0.1041(14) 0.1086(11) 0.498(2) 0.030 Uiso 1 1 d D . . 
C1 C 0.13611(11) 0.08602(6) 0.27259(16) 0.0176(2) Uani 1 1 d U . . 
C2 C -0.07121(11) 0.10472(7) 0.27456(16) 0.0191(2) Uani 1 1 d U . . 
C3 C -0.16010(12) 0.06120(8) 0.33522(18) 0.0242(3) Uani 1 1 d U . . 
H3 H -0.1533 0.0089 0.3344 0.029 Uiso 1 1 calc R . . 
C4 C -0.25811(13) 0.09408(8) 0.39663(19) 0.0272(3) Uani 1 1 d U . . 
H4 H -0.3185 0.0641 0.4373 0.033 Uiso 1 1 calc R . . 
C5 C -0.26910(13) 0.17047(8) 0.39943(19) 0.0261(3) Uani 1 1 d U . . 
C6 C -0.18170(13) 0.21426(8) 0.3393(2) 0.0296(3) Uani 1 1 d U . . 
H6 H -0.1882 0.2666 0.3419 0.036 Uiso 1 1 calc R . . 
C7 C -0.08405(13) 0.18096(8) 0.2749(2) 0.0270(3) Uani 1 1 d U . . 
H7 H -0.0251 0.2110 0.2304 0.032 Uiso 1 1 calc R . . 
C8 C -0.39286(17) 0.27325(10) 0.4442(2) 0.0410(4) Uani 1 1 d U . . 
H8A H -0.3316 0.3008 0.5159 0.061 Uiso 1 1 calc R . . 
H8B H -0.4707 0.2846 0.4831 0.061 Uiso 1 1 calc R . . 
H8C H -0.3917 0.2875 0.3211 0.061 Uiso 1 1 calc R . . 
C9 C 0.33559(12) 0.03549(8) 0.22765(18) 0.0241(3) Uani 1 1 d U . . 
H9 H 0.3469 0.0361 0.3585 0.029 Uiso 1 1 calc R . . 
C10 C 0.32361(15) -0.04453(9) 0.1673(2) 0.0358(3) Uani 1 1 d U . . 
H10A H 0.2551 -0.0671 0.2153 0.054 Uiso 1 1 calc R . . 
H10B H 0.3955 -0.0718 0.2087 0.054 Uiso 1 1 calc R . . 
H10C H 0.3125 -0.0462 0.0391 0.054 Uiso 1 1 calc R . . 
C11 C 0.44141(14) 0.07329(10) 0.1586(2) 0.0365(3) Uani 1 1 d U . . 
H11A H 0.4290 0.0766 0.0307 0.055 Uiso 1 1 calc R . . 
H11B H 0.5132 0.0446 0.1924 0.055 Uiso 1 1 calc R . . 
H11C H 0.4503 0.1231 0.2082 0.055 Uiso 1 1 calc R . . 
C12 C 0.25706(12) 0.16110(8) 0.49845(18) 0.0241(3) Uani 1 1 d U . . 
H12 H 0.3101 0.1670 0.4025 0.029 Uiso 1 1 calc R . . 
C13 C 0.20680(17) 0.23622(9) 0.5391(2) 0.0353(3) Uani 1 1 d U . . 
H13A H 0.1613 0.2558 0.4342 0.053 Uiso 1 1 calc R . . 
H13B H 0.2718 0.2702 0.5759 0.053 Uiso 1 1 calc R . . 
H13C H 0.1549 0.2312 0.6334 0.053 Uiso 1 1 calc R . . 
C14 C 0.32948(15) 0.12975(10) 0.6594(2) 0.0381(4) Uani 1 1 d U . . 
H14A H 0.2785 0.1238 0.7546 0.057 Uiso 1 1 calc R . . 
H14B H 0.3944 0.1637 0.6964 0.057 Uiso 1 1 calc R . . 
H14C H 0.3621 0.0816 0.6305 0.057 Uiso 1 1 calc R . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pd1 N1 2.0304(10) . ? 
Pd1 N1 2.0304(10) 3 ? 
Pd1 Cl1 2.3246(3) . ? 
Pd1 Cl1 2.3246(3) 3 ? 
Pd1 H2N 2.662(19) . ? 
O1 C5 1.3759(17) . ? 
O1 C8 1.410(2) . ? 
N1 C1 1.3157(16) . ? 
N1 C2 1.4264(16) . ? 
N2 C1 1.3637(16) . ? 
N2 C9 1.4673(17) . ? 
N2 H2N 0.825(14) . ? 
N3 C1 1.3520(16) . ? 
N3 C12 1.4679(17) . ? 
N3 H3N 0.822(14) . ? 
C2 C7 1.3866(18) . ? 
C2 C3 1.3935(18) . ? 
C3 C4 1.3824(19) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.388(2) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.382(2) . ? 
C6 C7 1.392(2) . ? 
C6 H6 0.9500 . ? 
C7 H7 0.9500 . ? 
C8 H8A 0.9800 . ? 
C8 H8B 0.9800 . ? 
C8 H8C 0.9800 . ? 
C9 C11 1.520(2) . ? 
C9 C10 1.522(2) . ? 
C9 H9 1.0000 . ? 
C10 H10A 0.9800 . ? 
C10 H10B 0.9800 . ? 
C10 H10C 0.9800 . ? 
C11 H11A 0.9800 . ? 
C11 H11B 0.9800 . ? 
C11 H11C 0.9800 . ? 
C12 C13 1.517(2) . ? 
C12 C14 1.525(2) . ? 
C12 H12 1.0000 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C14 H14C 0.9800 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Pd1 N1 180.0 . 3 ? 
N1 Pd1 Cl1 88.60(3) . . ? 
N1 Pd1 Cl1 91.40(3) 3 . ? 
N1 Pd1 Cl1 91.40(3) . 3 ? 
N1 Pd1 Cl1 88.60(3) 3 3 ? 
Cl1 Pd1 Cl1 180.0 . 3 ? 
N1 Pd1 H2N 58.3(4) . . ? 
N1 Pd1 H2N 121.7(4) 3 . ? 
Cl1 Pd1 H2N 69.2(4) . . ? 
Cl1 Pd1 H2N 110.8(4) 3 . ? 
C5 O1 C8 116.87(13) . . ? 
C1 N1 C2 120.14(10) . . ? 
C1 N1 Pd1 120.45(8) . . ? 
C2 N1 Pd1 119.40(8) . . ? 
C1 N2 C9 123.51(11) . . ? 
C1 N2 H2N 112.1(14) . . ? 
C9 N2 H2N 114.5(14) . . ? 
C1 N3 C12 125.28(11) . . ? 
C1 N3 H3N 114.0(13) . . ? 
C12 N3 H3N 116.6(13) . . ? 
N1 C1 N3 122.73(11) . . ? 
N1 C1 N2 118.77(11) . . ? 
N3 C1 N2 118.50(11) . . ? 
C7 C2 C3 118.79(12) . . ? 
C7 C2 N1 120.91(12) . . ? 
C3 C2 N1 120.22(12) . . ? 
C4 C3 C2 120.11(13) . . ? 
C4 C3 H3 119.9 . . ? 
C2 C3 H3 119.9 . . ? 
C3 C4 C5 120.66(13) . . ? 
C3 C4 H4 119.7 . . ? 
C5 C4 H4 119.7 . . ? 
O1 C5 C6 124.77(14) . . ? 
O1 C5 C4 115.42(13) . . ? 
C6 C5 C4 119.80(13) . . ? 
C5 C6 C7 119.40(13) . . ? 
C5 C6 H6 120.3 . . ? 
C7 C6 H6 120.3 . . ? 
C2 C7 C6 121.20(13) . . ? 
C2 C7 H7 119.4 . . ? 
C6 C7 H7 119.4 . . ? 
O1 C8 H8A 109.5 . . ? 
O1 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
O1 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
N2 C9 C11 109.45(12) . . ? 
N2 C9 C10 110.37(11) . . ? 
C11 C9 C10 111.87(12) . . ? 
N2 C9 H9 108.4 . . ? 
C11 C9 H9 108.4 . . ? 
C10 C9 H9 108.4 . . ? 
C9 C10 H10A 109.5 . . ? 
C9 C10 H10B 109.5 . . ? 
H10A C10 H10B 109.5 . . ? 
C9 C10 H10C 109.5 . . ? 
H10A C10 H10C 109.5 . . ? 
H10B C10 H10C 109.5 . . ? 
C9 C11 H11A 109.5 . . ? 
C9 C11 H11B 109.5 . . ? 
H11A C11 H11B 109.5 . . ? 
C9 C11 H11C 109.5 . . ? 
H11A C11 H11C 109.5 . . ? 
H11B C11 H11C 109.5 . . ? 
N3 C12 C13 110.07(12) . . ? 
N3 C12 C14 110.24(12) . . ? 
C13 C12 C14 110.51(12) . . ? 
N3 C12 H12 108.7 . . ? 
C13 C12 H12 108.7 . . ? 
C14 C12 H12 108.7 . . ? 
C12 C13 H13A 109.5 . . ? 
C12 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C12 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C12 C14 H14A 109.5 . . ? 
C12 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
C12 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
Cl1 Pd1 N1 C1 -89.73(10) . . . . ? 
Cl1 Pd1 N1 C1 90.27(10) 3 . . . ? 
H2N Pd1 N1 C1 -23.5(5) . . . . ? 
Cl1 Pd1 N1 C2 89.82(9) . . . . ? 
Cl1 Pd1 N1 C2 -90.18(9) 3 . . . ? 
H2N Pd1 N1 C2 156.1(5) . . . . ? 
C2 N1 C1 N3 24.25(18) . . . . ? 
Pd1 N1 C1 N3 -156.20(10) . . . . ? 
C2 N1 C1 N2 -155.85(12) . . . . ? 
Pd1 N1 C1 N2 23.70(16) . . . . ? 
C12 N3 C1 N1 -147.57(13) . . . . ? 
C12 N3 C1 N2 32.52(18) . . . . ? 
C9 N2 C1 N1 -129.76(13) . . . . ? 
C9 N2 C1 N3 50.15(17) . . . . ? 
C1 N1 C2 C7 59.99(17) . . . . ? 
Pd1 N1 C2 C7 -119.56(12) . . . . ? 
C1 N1 C2 C3 -123.36(14) . . . . ? 
Pd1 N1 C2 C3 57.09(15) . . . . ? 
C7 C2 C3 C4 -0.9(2) . . . . ? 
N1 C2 C3 C4 -177.62(12) . . . . ? 
C2 C3 C4 C5 -0.3(2) . . . . ? 
C8 O1 C5 C6 7.8(2) . . . . ? 
C8 O1 C5 C4 -171.36(14) . . . . ? 
C3 C4 C5 O1 179.59(13) . . . . ? 
C3 C4 C5 C6 0.4(2) . . . . ? 
O1 C5 C6 C7 -178.46(14) . . . . ? 
C4 C5 C6 C7 0.6(2) . . . . ? 
C3 C2 C7 C6 2.0(2) . . . . ? 
N1 C2 C7 C6 178.67(13) . . . . ? 
C5 C6 C7 C2 -1.9(2) . . . . ? 
C1 N2 C9 C11 -143.12(13) . . . . ? 
C1 N2 C9 C10 93.34(15) . . . . ? 
C1 N3 C12 C13 107.98(15) . . . . ? 
C1 N3 C12 C14 -129.85(14) . . . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N3 H3N Cl1  0.822(14) 2.730(15) 3.4759(12) 151.7(17) 1_556 
N2 H2N Cl1  0.825(14) 2.845(16) 3.5430(12) 143.5(17) . 
  
_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              30.52 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    1.051 
_refine_diff_density_min   -0.611 
_refine_diff_density_rms    0.064 

###END


#=========================================================================
# Data for compound 4b (local labelling  as ea02513a)
#=========================================================================

  
data_4b 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C28 H42 Cl2 N6 O4 Pd' 
_chemical_formula_sum             'C28 H42 Cl2 N6 O4 Pd' 
_chemical_formula_weight          703.98 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pd'  'Pd'  -0.9988   1.0072 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'P 21/n' 
_symmetry_space_group_name_Hall    '-P 2yn'

  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    11.2008(3) 
_cell_length_b                    13.5909(4) 
_cell_length_c                    11.5265(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  111.5630(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1631.86(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     6629 
_cell_measurement_theta_min       2.42 
_cell_measurement_theta_max       29.43 
  
_exptl_crystal_description        prism 
_exptl_crystal_colour             orange 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.433 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              728 
_exptl_absorpt_coefficient_mu     0.774 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8301 
_exptl_absorpt_correction_T_max   0.8905 
_exptl_absorpt_process_details 
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   
;
 Bruker-Nonius X8kappa APEX II CCD area detector
; 
_diffrn_measurement_method        'phi and omega scans with narrow frames' 
_diffrn_detector_area_resol_mean   8.26
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             14535 
_diffrn_reflns_av_R_equivalents   0.0231 
_diffrn_reflns_av_unetI/netI     0.0173 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          25.25 
_reflns_number_total              2945 
_reflns_number_gt                 2498 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement        'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction         'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution     'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material   'SHELXTL and publCIF (Westrip, 2010)'
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0560P)²+0.3946P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2945 
_refine_ls_number_parameters      197 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0307 
_refine_ls_R_factor_gt            0.0261 
_refine_ls_wR_factor_ref          0.0822 
_refine_ls_wR_factor_gt           0.0796 
_refine_ls_goodness_of_fit_ref    1.081 
_refine_ls_restrained_S_all       1.080 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pd1 Pd 0.5000 0.0000 0.5000 0.02334(11) Uani 1 2 d S . . 
Cl1 Cl 0.34466(6) 0.07500(4) 0.33335(6) 0.03800(17) Uani 1 1 d . . . 
O1 O 0.02578(18) 0.09278(13) 0.6749(2) 0.0522(5) Uani 1 1 d . . . 
O2 O 0.02206(18) -0.07391(13) 0.7132(2) 0.0513(5) Uani 1 1 d . . . 
N1 N 0.43754(17) 0.07421(12) 0.61909(17) 0.0281(4) Uani 1 1 d . . . 
N2 N 0.5154(2) 0.21973(13) 0.5761(2) 0.0332(5) Uani 1 1 d D . . 
H2N H 0.489(2) 0.200(3) 0.5001(18) 0.050 Uiso 1 1 d D . . 
N3 N 0.4970(2) 0.19921(14) 0.7696(2) 0.0346(5) Uani 1 1 d D . . 
H3N H 0.514(3) 0.2603(13) 0.779(3) 0.052 Uiso 1 1 d D . . 
C1 C 0.4838(2) 0.16307(15) 0.6560(2) 0.0279(5) Uani 1 1 d . . . 
C2 C 0.3384(2) 0.03387(17) 0.6532(2) 0.0264(5) Uani 1 1 d . . . 
C3 C 0.2342(2) 0.09383(16) 0.6494(2) 0.0321(5) Uani 1 1 d . . . 
H3 H 0.2328 0.1623 0.6322 0.039 Uiso 1 1 calc R . . 
C4 C 0.1356(2) 0.04923(17) 0.6716(2) 0.0342(5) Uani 1 1 d . . . 
C5 C 0.1345(2) -0.05010(18) 0.6948(2) 0.0345(5) Uani 1 1 d . . . 
C6 C 0.2343(2) -0.10961(17) 0.7000(2) 0.0370(6) Uani 1 1 d . . . 
H6 H 0.2337 -0.1780 0.7170 0.044 Uiso 1 1 calc R . . 
C7 C 0.3375(2) -0.06569(16) 0.6791(2) 0.0324(5) Uani 1 1 d . . . 
H7 H 0.4089 -0.1051 0.6828 0.039 Uiso 1 1 calc R . . 
C8 C -0.0552(3) 0.01288(17) 0.6801(3) 0.0439(7) Uani 1 1 d . . . 
H8A H -0.1253 0.0040 0.5980 0.053 Uiso 1 1 calc R . . 
H8B H -0.0940 0.0265 0.7430 0.053 Uiso 1 1 calc R . . 
C9 C 0.6252(3) 0.28730(17) 0.6082(3) 0.0403(6) Uani 1 1 d . . . 
H9 H 0.6370 0.3194 0.6897 0.048 Uiso 1 1 calc R . . 
C10 C 0.7467(3) 0.2278(2) 0.6231(4) 0.0646(9) Uani 1 1 d . . . 
H10A H 0.7601 0.1776 0.6877 0.097 Uiso 1 1 calc R . . 
H10B H 0.8210 0.2720 0.6472 0.097 Uiso 1 1 calc R . . 
H10C H 0.7364 0.1958 0.5437 0.097 Uiso 1 1 calc R . . 
C11 C 0.5966(4) 0.3643(3) 0.5113(4) 0.0833(12) Uani 1 1 d . . . 
H11A H 0.5739 0.3334 0.4292 0.125 Uiso 1 1 calc R . . 
H11B H 0.6725 0.4061 0.5277 0.125 Uiso 1 1 calc R . . 
H11C H 0.5247 0.4046 0.5129 0.125 Uiso 1 1 calc R . . 
C12 C 0.5383(3) 0.13981(19) 0.8833(2) 0.0431(6) Uani 1 1 d . . . 
H12 H 0.5052 0.0714 0.8603 0.052 Uiso 1 1 calc R . . 
C13 C 0.4821(3) 0.1798(3) 0.9735(3) 0.0706(11) Uani 1 1 d . . . 
H13A H 0.5074 0.2488 0.9918 0.106 Uiso 1 1 calc R . . 
H13B H 0.5140 0.1415 1.0509 0.106 Uiso 1 1 calc R . . 
H13C H 0.3883 0.1752 0.9368 0.106 Uiso 1 1 calc R . . 
C14 C 0.6838(3) 0.1351(3) 0.9412(3) 0.0803(11) Uani 1 1 d . . . 
H14A H 0.7171 0.1055 0.8817 0.120 Uiso 1 1 calc R . . 
H14B H 0.7097 0.0951 1.0172 0.120 Uiso 1 1 calc R . . 
H14C H 0.7184 0.2018 0.9620 0.120 Uiso 1 1 calc R . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Pd1 N1 2.0241(17) . ? 
Pd1 N1 2.0241(17) 3_656 ? 
Pd1 Cl1 2.3021(6) . ? 
Pd1 Cl1 2.3021(6) 3_656 ? 
O1 C4 1.378(3) . ? 
O1 C8 1.430(3) . ? 
O2 C5 1.390(3) . ? 
O2 C8 1.430(3) . ? 
N1 C1 1.322(3) . ? 
N1 C2 1.418(3) . ? 
N2 C1 1.344(3) . ? 
N2 C9 1.469(3) . ? 
N2 H2N 0.858(17) . ? 
N3 C1 1.355(3) . ? 
N3 C12 1.462(3) . ? 
N3 H3N 0.849(17) . ? 
C2 C7 1.387(3) . ? 
C2 C3 1.411(3) . ? 
C3 C4 1.364(3) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.377(4) . ? 
C5 C6 1.364(3) . ? 
C6 C7 1.398(3) . ? 
C6 H6 0.9500 . ? 
C7 H7 0.9500 . ? 
C8 H8A 0.9900 . ? 
C8 H8B 0.9900 . ? 
C9 C11 1.477(4) . ? 
C9 C10 1.538(4) . ? 
C9 H9 1.0000 . ? 
C10 H10A 0.9800 . ? 
C10 H10B 0.9800 . ? 
C10 H10C 0.9800 . ? 
C11 H11A 0.9800 . ? 
C11 H11B 0.9800 . ? 
C11 H11C 0.9800 . ? 
C12 C13 1.501(4) . ? 
C12 C14 1.518(4) . ? 
C12 H12 1.0000 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C14 H14C 0.9800 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Pd1 N1 180.00(7) . 3_656 ? 
N1 Pd1 Cl1 90.09(6) . . ? 
N1 Pd1 Cl1 89.91(6) 3_656 . ? 
N1 Pd1 Cl1 89.91(6) . 3_656 ? 
N1 Pd1 Cl1 90.09(6) 3_656 3_656 ? 
Cl1 Pd1 Cl1 180.00(3) . 3_656 ? 
C4 O1 C8 105.16(19) . . ? 
C5 O2 C8 105.13(18) . . ? 
C1 N1 C2 121.25(17) . . ? 
C1 N1 Pd1 118.77(14) . . ? 
C2 N1 Pd1 119.78(13) . . ? 
C1 N2 C9 126.3(2) . . ? 
C1 N2 H2N 116(2) . . ? 
C9 N2 H2N 113(2) . . ? 
C1 N3 C12 123.53(19) . . ? 
C1 N3 H3N 114(2) . . ? 
C12 N3 H3N 117(2) . . ? 
N1 C1 N2 118.3(2) . . ? 
N1 C1 N3 122.2(2) . . ? 
N2 C1 N3 119.48(19) . . ? 
C7 C2 C3 119.93(19) . . ? 
C7 C2 N1 120.37(19) . . ? 
C3 C2 N1 119.4(2) . . ? 
C4 C3 C2 117.1(2) . . ? 
C4 C3 H3 121.5 . . ? 
C2 C3 H3 121.5 . . ? 
C3 C4 O1 127.4(2) . . ? 
C3 C4 C5 122.5(2) . . ? 
O1 C4 C5 110.08(19) . . ? 
C6 C5 O2 129.0(2) . . ? 
C6 C5 C4 121.6(2) . . ? 
O2 C5 C4 109.36(19) . . ? 
C5 C6 C7 117.1(2) . . ? 
C5 C6 H6 121.4 . . ? 
C7 C6 H6 121.4 . . ? 
C2 C7 C6 121.7(2) . . ? 
C2 C7 H7 119.1 . . ? 
C6 C7 H7 119.1 . . ? 
O1 C8 O2 107.8(2) . . ? 
O1 C8 H8A 110.1 . . ? 
O2 C8 H8A 110.1 . . ? 
O1 C8 H8B 110.1 . . ? 
O2 C8 H8B 110.1 . . ? 
H8A C8 H8B 108.5 . . ? 
N2 C9 C11 108.9(3) . . ? 
N2 C9 C10 108.9(2) . . ? 
C11 C9 C10 113.2(3) . . ? 
N2 C9 H9 108.6 . . ? 
C11 C9 H9 108.6 . . ? 
C10 C9 H9 108.6 . . ? 
C9 C10 H10A 109.5 . . ? 
C9 C10 H10B 109.5 . . ? 
H10A C10 H10B 109.5 . . ? 
C9 C10 H10C 109.5 . . ? 
H10A C10 H10C 109.5 . . ? 
H10B C10 H10C 109.5 . . ? 
C9 C11 H11A 109.5 . . ? 
C9 C11 H11B 109.5 . . ? 
H11A C11 H11B 109.5 . . ? 
C9 C11 H11C 109.5 . . ? 
H11A C11 H11C 109.5 . . ? 
H11B C11 H11C 109.5 . . ? 
N3 C12 C13 110.3(2) . . ? 
N3 C12 C14 110.6(3) . . ? 
C13 C12 C14 111.5(3) . . ? 
N3 C12 H12 108.1 . . ? 
C13 C12 H12 108.1 . . ? 
C14 C12 H12 108.1 . . ? 
C12 C13 H13A 109.5 . . ? 
C12 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C12 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C12 C14 H14A 109.5 . . ? 
C12 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
C12 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
Cl1 Pd1 N1 C1 -86.74(17) . . . . ? 
Cl1 Pd1 N1 C1 93.26(17) 3_656 . . . ? 
Cl1 Pd1 N1 C2 88.22(16) . . . . ? 
Cl1 Pd1 N1 C2 -91.78(16) 3_656 . . . ? 
C2 N1 C1 N2 -142.4(2) . . . . ? 
Pd1 N1 C1 N2 32.5(3) . . . . ? 
C2 N1 C1 N3 35.9(3) . . . . ? 
Pd1 N1 C1 N3 -149.27(17) . . . . ? 
C9 N2 C1 N1 -142.8(2) . . . . ? 
C9 N2 C1 N3 38.9(3) . . . . ? 
C12 N3 C1 N1 38.4(3) . . . . ? 
C12 N3 C1 N2 -143.4(2) . . . . ? 
C1 N1 C2 C7 -143.5(2) . . . . ? 
Pd1 N1 C2 C7 41.6(3) . . . . ? 
C1 N1 C2 C3 42.3(3) . . . . ? 
Pd1 N1 C2 C3 -132.52(18) . . . . ? 
C7 C2 C3 C4 -0.3(3) . . . . ? 
N1 C2 C3 C4 173.9(2) . . . . ? 
C2 C3 C4 O1 178.7(2) . . . . ? 
C2 C3 C4 C5 -1.0(4) . . . . ? 
C8 O1 C4 C3 170.4(3) . . . . ? 
C8 O1 C4 C5 -9.8(3) . . . . ? 
C8 O2 C5 C6 -172.3(3) . . . . ? 
C8 O2 C5 C4 9.1(3) . . . . ? 
C3 C4 C5 C6 1.6(4) . . . . ? 
O1 C4 C5 C6 -178.2(3) . . . . ? 
C3 C4 C5 O2 -179.7(3) . . . . ? 
O1 C4 C5 O2 0.4(3) . . . . ? 
O2 C5 C6 C7 -179.1(3) . . . . ? 
C4 C5 C6 C7 -0.7(4) . . . . ? 
C3 C2 C7 C6 1.1(3) . . . . ? 
N1 C2 C7 C6 -173.1(2) . . . . ? 
C5 C6 C7 C2 -0.6(4) . . . . ? 
C4 O1 C8 O2 15.3(3) . . . . ? 
C5 O2 C8 O1 -15.1(3) . . . . ? 
C1 N2 C9 C11 -155.5(3) . . . . ? 
C1 N2 C9 C10 80.6(3) . . . . ? 
C1 N3 C12 C13 -151.1(3) . . . . ? 
C1 N3 C12 C14 85.1(3) . . . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N2 H2N Cl1  0.858(17) 2.63(2) 3.380(2) 147(3) . 
N3 H3N O2  0.849(17) 2.298(19) 3.102(3) 158(3) 2_556 
  
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              25.25 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.404 
_refine_diff_density_min   -0.203 
_refine_diff_density_rms    0.057 

###END


#=========================================================================
# Data for compound 4c (local labelling  as ea02613x)
#=========================================================================
  
data_4c 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C26 H38 Cl2 F2 I2 N6 Pd' 
_chemical_formula_sum             'C26 H38 Cl2 F2 I2 N6 Pd' 
_chemical_formula_weight          903.72 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pd'  'Pd'  -0.9988   1.0072 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'P 21/c'
_symmetry_space_group_name_Hall    '-P 2ybc' 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    24.0900(11) 
_cell_length_b                    11.4512(5) 
_cell_length_c                    20.3122(8) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  114.6710(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      5091.8(4) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     6121 
_cell_measurement_theta_min       2.21 
_cell_measurement_theta_max       22.39 
  
_exptl_crystal_description        prism 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.768 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2640 
_exptl_absorpt_coefficient_mu     2.559 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.7819 
_exptl_absorpt_correction_T_max   0.8154 
_exptl_absorpt_process_details 
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   
;
 Bruker-Nonius X8kappa APEX II CCD area detector
; 
_diffrn_measurement_method        'phi and omega scans with narrow frames' 
_diffrn_detector_area_resol_mean   8.26
_diffrn_standards_decay_%         0  
_diffrn_reflns_number             53653 
_diffrn_reflns_av_R_equivalents   0.0636 
_diffrn_reflns_av_sigmaI/netI     0.0704 
_diffrn_reflns_limit_h_min        -28 
_diffrn_reflns_limit_h_max        28 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.01 
_diffrn_reflns_theta_max          25.25 
_reflns_number_total              9183 
_reflns_number_gt                 6888 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement        'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction         'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution     'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material   'SHELXTL and publCIF (Westrip, 2010)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0190P)²+15.6467P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          9183 
_refine_ls_number_parameters      556 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0675 
_refine_ls_R_factor_gt            0.0452 
_refine_ls_wR_factor_ref          0.1160 
_refine_ls_wR_factor_gt           0.1072 
_refine_ls_goodness_of_fit_ref    1.071 
_refine_ls_restrained_S_all       1.095 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
I1 I 0.19652(2) 1.25245(5) 0.02790(2) 0.04838(15) Uani 1 1 d U . . 
I2 I 0.17662(2) 0.82086(6) 0.70879(3) 0.06087(17) Uani 1 1 d U . . 
Pd1 Pd 0.168658(19) 1.02074(4) 0.35222(2) 0.02840(12) Uani 1 1 d U . . 
Cl1 Cl 0.23715(7) 1.17599(14) 0.39444(9) 0.0375(4) Uani 1 1 d U . . 
Cl2 Cl 0.10421(8) 0.86450(15) 0.30054(9) 0.0447(4) Uani 1 1 d U . . 
F1 F 0.1111(2) 1.3511(4) 0.2266(2) 0.0561(10) Uani 1 1 d U . . 
F2 F 0.31848(17) 0.9266(4) 0.5715(2) 0.0589(11) Uani 1 1 d U . . 
N1 N 0.1109(2) 1.1235(5) 0.2729(3) 0.0333(9) Uani 1 1 d U . . 
N2 N 0.0578(2) 1.1844(5) 0.3375(3) 0.0379(10) Uani 1 1 d DU . . 
H2N H 0.089(2) 1.163(6) 0.375(2) 0.057 Uiso 1 1 d D . . 
N3 N 0.0094(2) 1.1831(5) 0.2122(3) 0.0365(10) Uani 1 1 d DU . . 
H3N H -0.016(2) 1.225(5) 0.220(4) 0.055 Uiso 1 1 d D . . 
N4 N 0.2248(2) 0.9140(5) 0.4315(3) 0.0364(10) Uani 1 1 d U . . 
N5 N 0.2919(3) 0.9130(5) 0.3798(3) 0.0464(11) Uani 1 1 d DU . . 
H5N H 0.287(4) 0.9866(11) 0.376(4) 0.070 Uiso 1 1 d D . . 
N6 N 0.2932(2) 0.7562(5) 0.4520(3) 0.0440(11) Uani 1 1 d DU . . 
H6N H 0.3287(15) 0.739(7) 0.456(4) 0.066 Uiso 1 1 d D . . 
C1 C 0.0586(3) 1.1631(5) 0.2729(3) 0.0334(10) Uani 1 1 d U . . 
C2 C 0.1262(3) 1.1503(6) 0.2147(3) 0.0348(10) Uani 1 1 d U . . 
C3 C 0.1278(3) 1.2655(6) 0.1932(4) 0.0402(11) Uani 1 1 d U . . 
C4 C 0.1469(3) 1.2967(6) 0.1401(4) 0.0422(12) Uani 1 1 d U . . 
H4 H 0.1474 1.3760 0.1267 0.051 Uiso 1 1 calc R . . 
C5 C 0.1651(3) 1.2086(6) 0.1072(4) 0.0418(12) Uani 1 1 d U . . 
C6 C 0.1649(3) 1.0931(6) 0.1272(3) 0.0419(12) Uani 1 1 d U . . 
H6 H 0.1779 1.0336 0.1042 0.050 Uiso 1 1 calc R . . 
C7 C 0.1457(3) 1.0642(6) 0.1806(3) 0.0396(12) Uani 1 1 d U . . 
H7 H 0.1459 0.9847 0.1942 0.048 Uiso 1 1 calc R . . 
C8 C 0.0045(3) 1.1695(6) 0.3553(4) 0.0417(13) Uani 1 1 d U . . 
H8 H -0.0335 1.1717 0.3092 0.050 Uiso 1 1 calc R . . 
C9 C 0.0078(4) 1.0522(7) 0.3910(5) 0.0612(19) Uani 1 1 d U . . 
H9A H 0.0069 0.9898 0.3576 0.092 Uiso 1 1 calc R . . 
H9B H -0.0272 1.0437 0.4035 0.092 Uiso 1 1 calc R . . 
H9C H 0.0458 1.0472 0.4352 0.092 Uiso 1 1 calc R . . 
C10 C 0.0023(3) 1.2688(7) 0.4026(4) 0.0540(17) Uani 1 1 d U . . 
H10A H 0.0409 1.2721 0.4461 0.081 Uiso 1 1 calc R . . 
H10B H -0.0315 1.2565 0.4167 0.081 Uiso 1 1 calc R . . 
H10C H -0.0039 1.3424 0.3758 0.081 Uiso 1 1 calc R . . 
C11 C -0.0135(3) 1.1022(6) 0.1502(4) 0.0452(13) Uani 1 1 d U . . 
H11 H 0.0183 1.0408 0.1588 0.054 Uiso 1 1 calc R . . 
C12 C -0.0705(3) 1.0424(8) 0.1469(5) 0.067(2) Uani 1 1 d U . . 
H12A H -0.0608 0.9978 0.1915 0.101 Uiso 1 1 calc R . . 
H12B H -0.0862 0.9894 0.1052 0.101 Uiso 1 1 calc R . . 
H12C H -0.1016 1.1012 0.1418 0.101 Uiso 1 1 calc R . . 
C13 C -0.0237(4) 1.1642(8) 0.0803(4) 0.071(2) Uani 1 1 d U . . 
H13A H -0.0545 1.2254 0.0708 0.106 Uiso 1 1 calc R . . 
H13B H -0.0378 1.1079 0.0403 0.106 Uiso 1 1 calc R . . 
H13C H 0.0148 1.1994 0.0846 0.106 Uiso 1 1 calc R . . 
C14 C 0.2704(3) 0.8585(6) 0.4231(4) 0.0395(11) Uani 1 1 d U . . 
C15 C 0.2146(3) 0.9004(6) 0.4949(3) 0.0364(11) Uani 1 1 d U . . 
C16 C 0.2607(3) 0.9058(6) 0.5637(3) 0.0407(12) Uani 1 1 d U . . 
C17 C 0.2516(3) 0.8865(6) 0.6253(4) 0.0434(12) Uani 1 1 d U . . 
H17 H 0.2851 0.8871 0.6716 0.052 Uiso 1 1 calc R . . 
C18 C 0.1929(3) 0.8664(6) 0.6185(3) 0.0412(12) Uani 1 1 d U . . 
C19 C 0.1456(3) 0.8692(6) 0.5516(3) 0.0398(12) Uani 1 1 d U . . 
H19 H 0.1049 0.8595 0.5468 0.048 Uiso 1 1 calc R . . 
C20 C 0.1564(3) 0.8860(6) 0.4906(3) 0.0378(12) Uani 1 1 d U . . 
H20 H 0.1227 0.8877 0.4444 0.045 Uiso 1 1 calc R . . 
C21 C 0.3353(3) 0.8700(7) 0.3528(4) 0.0516(14) Uani 1 1 d U . . 
H21 H 0.3312 0.7833 0.3473 0.062 Uiso 1 1 calc R . . 
C22 C 0.3180(4) 0.9249(8) 0.2790(5) 0.081(2) Uani 1 1 d U . . 
H22A H 0.2764 0.9013 0.2465 0.121 Uiso 1 1 calc R . . 
H22B H 0.3465 0.8988 0.2590 0.121 Uiso 1 1 calc R . . 
H22C H 0.3199 1.0102 0.2838 0.121 Uiso 1 1 calc R . . 
C23 C 0.3997(4) 0.8997(8) 0.4045(6) 0.081(2) Uani 1 1 d U . . 
H23A H 0.4041 0.9847 0.4098 0.122 Uiso 1 1 calc R . . 
H23B H 0.4282 0.8694 0.3856 0.122 Uiso 1 1 calc R . . 
H23C H 0.4087 0.8643 0.4518 0.122 Uiso 1 1 calc R . . 
C24 C 0.2616(3) 0.6628(6) 0.4720(4) 0.0457(13) Uani 1 1 d U . . 
H24 H 0.2221 0.6939 0.4697 0.055 Uiso 1 1 calc R . . 
C25 C 0.2485(4) 0.5606(7) 0.4211(4) 0.0578(18) Uani 1 1 d U . . 
H25A H 0.2229 0.5863 0.3716 0.087 Uiso 1 1 calc R . . 
H25B H 0.2270 0.4999 0.4354 0.087 Uiso 1 1 calc R . . 
H25C H 0.2870 0.5291 0.4231 0.087 Uiso 1 1 calc R . . 
C26 C 0.3015(4) 0.6258(8) 0.5500(4) 0.073(2) Uani 1 1 d U . . 
H26A H 0.3394 0.5908 0.5522 0.109 Uiso 1 1 calc R . . 
H26B H 0.2795 0.5685 0.5659 0.109 Uiso 1 1 calc R . . 
H26C H 0.3113 0.6943 0.5817 0.109 Uiso 1 1 calc R . . 
I3 I 0.57633(2) 0.16869(4) 0.23043(3) 0.04926(14) Uani 1 1 d U . . 
Pd2 Pd 0.5000 0.5000 0.5000 0.03928(19) Uani 1 2 d SU . . 
Cl3 Cl 0.41006(8) 0.59587(15) 0.43170(9) 0.0465(4) Uani 1 1 d U . . 
F3 F 0.4849(2) 0.1182(4) 0.4283(2) 0.0613(11) Uani 1 1 d U . . 
N7 N 0.4638(3) 0.3519(5) 0.4415(3) 0.0447(10) Uani 1 1 d U . . 
N8 N 0.3895(3) 0.2986(6) 0.4856(4) 0.0691(14) Uani 1 1 d DU . . 
H8N H 0.3629 0.2365 0.4720 0.104 Uiso 1 1 d RD . . 
N9 N 0.3677(3) 0.2712(6) 0.3691(4) 0.0555(12) Uani 1 1 d DU . . 
H9N H 0.339(3) 0.230(6) 0.370(5) 0.083 Uiso 1 1 d D . . 
C27 C 0.4095(4) 0.3083(6) 0.4333(4) 0.0522(12) Uani 1 1 d U . . 
C28 C 0.4899(3) 0.3117(6) 0.3944(3) 0.0391(10) Uani 1 1 d U . . 
C29 C 0.5006(3) 0.1949(6) 0.3887(4) 0.0424(11) Uani 1 1 d U . . 
C30 C 0.5258(3) 0.1523(6) 0.3444(4) 0.0411(12) Uani 1 1 d U . . 
H30 H 0.5314 0.0707 0.3412 0.049 Uiso 1 1 calc R . . 
C31 C 0.5431(3) 0.2300(6) 0.3049(4) 0.0395(12) Uani 1 1 d U . . 
C32 C 0.5360(3) 0.3490(6) 0.3106(4) 0.0418(12) Uani 1 1 d U . . 
H32 H 0.5485 0.4028 0.2838 0.050 Uiso 1 1 calc R . . 
C33 C 0.5103(3) 0.3878(6) 0.3560(4) 0.0431(12) Uani 1 1 d U . . 
H33 H 0.5066 0.4695 0.3613 0.052 Uiso 1 1 calc R . . 
C34 C 0.4256(5) 0.2809(8) 0.5578(5) 0.0720(17) Uani 1 1 d U . . 
H34 H 0.4672 0.3137 0.5705 0.086 Uiso 1 1 calc R . . 
C35 C 0.3944(4) 0.3459(8) 0.6019(5) 0.0669(19) Uani 1 1 d U . . 
H35A H 0.3930 0.4299 0.5921 0.100 Uiso 1 1 calc R . . 
H35B H 0.4181 0.3319 0.6538 0.100 Uiso 1 1 calc R . . 
H35C H 0.3528 0.3163 0.5872 0.100 Uiso 1 1 calc R . . 
C36 C 0.4302(5) 0.1505(8) 0.5761(6) 0.089(2) Uani 1 1 d U . . 
H36A H 0.3892 0.1186 0.5628 0.134 Uiso 1 1 calc R . . 
H36B H 0.4547 0.1399 0.6282 0.134 Uiso 1 1 calc R . . 
H36C H 0.4498 0.1096 0.5490 0.134 Uiso 1 1 calc R . . 
C37 C 0.3516(4) 0.3343(7) 0.3009(4) 0.0554(15) Uani 1 1 d U . . 
H37 H 0.3842 0.3936 0.3090 0.066 Uiso 1 1 calc R . . 
C38 C 0.2928(4) 0.3988(8) 0.2809(5) 0.072(2) Uani 1 1 d U . . 
H38A H 0.2601 0.3432 0.2747 0.109 Uiso 1 1 calc R . . 
H38B H 0.2828 0.4413 0.2355 0.109 Uiso 1 1 calc R . . 
H38C H 0.2970 0.4543 0.3194 0.109 Uiso 1 1 calc R . . 
C39 C 0.3498(5) 0.2544(9) 0.2407(5) 0.090(3) Uani 1 1 d U . . 
H39A H 0.3888 0.2130 0.2561 0.135 Uiso 1 1 calc R . . 
H39B H 0.3427 0.3008 0.1974 0.135 Uiso 1 1 calc R . . 
H39C H 0.3166 0.1976 0.2296 0.135 Uiso 1 1 calc R . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
I1 C5 2.106(6) . ? 
I2 C18 2.095(6) . ? 
Pd1 N1 2.012(5) . ? 
Pd1 N4 2.025(5) . ? 
Pd1 Cl2 2.3136(17) . ? 
Pd1 Cl1 2.3318(16) . ? 
F1 C3 1.345(8) . ? 
F2 C16 1.356(7) . ? 
N1 C1 1.338(7) . ? 
N1 C2 1.412(7) . ? 
N2 C1 1.342(8) . ? 
N2 C8 1.482(7) . ? 
N2 H2N 0.849(5) . ? 
N3 C1 1.326(8) . ? 
N3 C11 1.473(8) . ? 
N3 H3N 0.849(5) . ? 
N4 C14 1.339(8) . ? 
N4 C15 1.415(8) . ? 
N5 C14 1.345(8) . ? 
N5 C21 1.454(8) . ? 
N5 H5N 0.851(5) . ? 
N6 C14 1.322(8) . ? 
N6 C24 1.466(9) . ? 
N6 H6N 0.850(5) . ? 
C2 C7 1.394(9) . ? 
C2 C3 1.395(9) . ? 
C3 C4 1.384(9) . ? 
C4 C5 1.379(9) . ? 
C4 H4 0.9500 . ? 
C5 C6 1.383(10) . ? 
C6 C7 1.386(8) . ? 
C6 H6 0.9500 . ? 
C7 H7 0.9500 . ? 
C8 C10 1.503(9) . ? 
C8 C9 1.513(10) . ? 
C8 H8 1.0000 . ? 
C9 H9A 0.9800 . ? 
C9 H9B 0.9800 . ? 
C9 H9C 0.9800 . ? 
C10 H10A 0.9800 . ? 
C10 H10B 0.9800 . ? 
C10 H10C 0.9800 . ? 
C11 C12 1.511(10) . ? 
C11 C13 1.513(10) . ? 
C11 H11 1.0000 . ? 
C12 H12A 0.9800 . ? 
C12 H12B 0.9800 . ? 
C12 H12C 0.9800 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C15 C16 1.376(9) . ? 
C15 C20 1.379(8) . ? 
C16 C17 1.373(9) . ? 
C17 C18 1.381(9) . ? 
C17 H17 0.9500 . ? 
C18 C19 1.363(9) . ? 
C19 C20 1.380(9) . ? 
C19 H19 0.9500 . ? 
C20 H20 0.9500 . ? 
C21 C23 1.505(11) . ? 
C21 C22 1.516(11) . ? 
C21 H21 1.0000 . ? 
C22 H22A 0.9800 . ? 
C22 H22B 0.9800 . ? 
C22 H22C 0.9800 . ? 
C23 H23A 0.9800 . ? 
C23 H23B 0.9800 . ? 
C23 H23C 0.9800 . ? 
C24 C25 1.506(10) . ? 
C24 C26 1.529(10) . ? 
C24 H24 1.0000 . ? 
C25 H25A 0.9800 . ? 
C25 H25B 0.9800 . ? 
C25 H25C 0.9800 . ? 
C26 H26A 0.9800 . ? 
C26 H26B 0.9800 . ? 
C26 H26C 0.9800 . ? 
I3 C31 2.105(6) . ? 
Pd2 N7 2.045(6) 3_666 ? 
Pd2 N7 2.045(6) . ? 
Pd2 Cl3 2.3054(16) 3_666 ? 
Pd2 Cl3 2.3054(16) . ? 
F3 C29 1.349(8) . ? 
N7 C27 1.344(9) . ? 
N7 C28 1.423(8) . ? 
N8 C27 1.340(9) . ? 
N8 C34 1.372(11) . ? 
N8 H8N 0.9200 . ? 
N9 C27 1.341(10) . ? 
N9 C37 1.465(10) . ? 
N9 H9N 0.850(5) . ? 
C28 C29 1.376(9) . ? 
C28 C33 1.389(9) . ? 
C29 C30 1.369(9) . ? 
C30 C31 1.375(9) . ? 
C30 H30 0.9500 . ? 
C31 C32 1.383(9) . ? 
C32 C33 1.382(9) . ? 
C32 H32 0.9500 . ? 
C33 H33 0.9500 . ? 
C34 C36 1.531(12) . ? 
C34 C35 1.575(11) . ? 
C34 H34 1.0000 . ? 
C35 H35A 0.9800 . ? 
C35 H35B 0.9800 . ? 
C35 H35C 0.9800 . ? 
C36 H36A 0.9800 . ? 
C36 H36B 0.9800 . ? 
C36 H36C 0.9800 . ? 
C37 C38 1.495(10) . ? 
C37 C39 1.512(11) . ? 
C37 H37 1.0000 . ? 
C38 H38A 0.9800 . ? 
C38 H38B 0.9800 . ? 
C38 H38C 0.9800 . ? 
C39 H39A 0.9800 . ? 
C39 H39B 0.9800 . ? 
C39 H39C 0.9800 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Pd1 N4 178.3(2) . . ? 
N1 Pd1 Cl2 88.85(16) . . ? 
N4 Pd1 Cl2 89.60(16) . . ? 
N1 Pd1 Cl1 89.75(15) . . ? 
N4 Pd1 Cl1 91.86(16) . . ? 
Cl2 Pd1 Cl1 173.87(6) . . ? 
C1 N1 C2 120.1(5) . . ? 
C1 N1 Pd1 122.3(4) . . ? 
C2 N1 Pd1 117.6(4) . . ? 
C1 N2 C8 125.8(5) . . ? 
C1 N2 H2N 117(5) . . ? 
C8 N2 H2N 106(5) . . ? 
C1 N3 C11 123.8(5) . . ? 
C1 N3 H3N 111(5) . . ? 
C11 N3 H3N 119(5) . . ? 
C14 N4 C15 121.7(5) . . ? 
C14 N4 Pd1 119.7(4) . . ? 
C15 N4 Pd1 118.6(4) . . ? 
C14 N5 C21 128.6(6) . . ? 
C14 N5 H5N 116(6) . . ? 
C21 N5 H5N 113(6) . . ? 
C14 N6 C24 127.0(5) . . ? 
C14 N6 H6N 117(5) . . ? 
C24 N6 H6N 115(5) . . ? 
N3 C1 N1 122.3(5) . . ? 
N3 C1 N2 120.3(5) . . ? 
N1 C1 N2 117.3(5) . . ? 
C7 C2 C3 117.1(5) . . ? 
C7 C2 N1 121.4(6) . . ? 
C3 C2 N1 121.2(6) . . ? 
F1 C3 C4 118.2(6) . . ? 
F1 C3 C2 118.5(5) . . ? 
C4 C3 C2 123.3(6) . . ? 
C5 C4 C3 117.8(6) . . ? 
C5 C4 H4 121.1 . . ? 
C3 C4 H4 121.1 . . ? 
C4 C5 C6 121.1(6) . . ? 
C4 C5 I1 119.0(5) . . ? 
C6 C5 I1 119.9(5) . . ? 
C5 C6 C7 120.1(6) . . ? 
C5 C6 H6 119.9 . . ? 
C7 C6 H6 119.9 . . ? 
C6 C7 C2 120.7(6) . . ? 
C6 C7 H7 119.6 . . ? 
C2 C7 H7 119.6 . . ? 
N2 C8 C10 109.5(6) . . ? 
N2 C8 C9 110.0(5) . . ? 
C10 C8 C9 111.9(6) . . ? 
N2 C8 H8 108.5 . . ? 
C10 C8 H8 108.5 . . ? 
C9 C8 H8 108.5 . . ? 
C8 C9 H9A 109.5 . . ? 
C8 C9 H9B 109.5 . . ? 
H9A C9 H9B 109.5 . . ? 
C8 C9 H9C 109.5 . . ? 
H9A C9 H9C 109.5 . . ? 
H9B C9 H9C 109.5 . . ? 
C8 C10 H10A 109.5 . . ? 
C8 C10 H10B 109.5 . . ? 
H10A C10 H10B 109.5 . . ? 
C8 C10 H10C 109.5 . . ? 
H10A C10 H10C 109.5 . . ? 
H10B C10 H10C 109.5 . . ? 
N3 C11 C12 109.4(6) . . ? 
N3 C11 C13 111.3(6) . . ? 
C12 C11 C13 112.5(7) . . ? 
N3 C11 H11 107.8 . . ? 
C12 C11 H11 107.8 . . ? 
C13 C11 H11 107.8 . . ? 
C11 C12 H12A 109.5 . . ? 
C11 C12 H12B 109.5 . . ? 
H12A C12 H12B 109.5 . . ? 
C11 C12 H12C 109.5 . . ? 
H12A C12 H12C 109.5 . . ? 
H12B C12 H12C 109.5 . . ? 
C11 C13 H13A 109.5 . . ? 
C11 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C11 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
N6 C14 N4 125.1(6) . . ? 
N6 C14 N5 119.8(6) . . ? 
N4 C14 N5 115.0(6) . . ? 
C16 C15 C20 115.9(6) . . ? 
C16 C15 N4 123.2(5) . . ? 
C20 C15 N4 120.9(6) . . ? 
F2 C16 C17 117.9(6) . . ? 
F2 C16 C15 118.6(6) . . ? 
C17 C16 C15 123.4(6) . . ? 
C16 C17 C18 118.8(6) . . ? 
C16 C17 H17 120.6 . . ? 
C18 C17 H17 120.6 . . ? 
C19 C18 C17 119.3(6) . . ? 
C19 C18 I2 119.7(5) . . ? 
C17 C18 I2 120.9(5) . . ? 
C18 C19 C20 120.4(6) . . ? 
C18 C19 H19 119.8 . . ? 
C20 C19 H19 119.8 . . ? 
C15 C20 C19 121.8(6) . . ? 
C15 C20 H20 119.1 . . ? 
C19 C20 H20 119.1 . . ? 
N5 C21 C23 110.8(7) . . ? 
N5 C21 C22 106.8(6) . . ? 
C23 C21 C22 112.0(7) . . ? 
N5 C21 H21 109.1 . . ? 
C23 C21 H21 109.1 . . ? 
C22 C21 H21 109.1 . . ? 
C21 C22 H22A 109.5 . . ? 
C21 C22 H22B 109.5 . . ? 
H22A C22 H22B 109.5 . . ? 
C21 C22 H22C 109.5 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 
C21 C23 H23A 109.5 . . ? 
C21 C23 H23B 109.5 . . ? 
H23A C23 H23B 109.5 . . ? 
C21 C23 H23C 109.5 . . ? 
H23A C23 H23C 109.5 . . ? 
H23B C23 H23C 109.5 . . ? 
N6 C24 C25 111.1(6) . . ? 
N6 C24 C26 108.4(6) . . ? 
C25 C24 C26 110.9(6) . . ? 
N6 C24 H24 108.8 . . ? 
C25 C24 H24 108.8 . . ? 
C26 C24 H24 108.8 . . ? 
C24 C25 H25A 109.5 . . ? 
C24 C25 H25B 109.5 . . ? 
H25A C25 H25B 109.5 . . ? 
C24 C25 H25C 109.5 . . ? 
H25A C25 H25C 109.5 . . ? 
H25B C25 H25C 109.5 . . ? 
C24 C26 H26A 109.5 . . ? 
C24 C26 H26B 109.5 . . ? 
H26A C26 H26B 109.5 . . ? 
C24 C26 H26C 109.5 . . ? 
H26A C26 H26C 109.5 . . ? 
H26B C26 H26C 109.5 . . ? 
N7 Pd2 N7 180.000(1) 3_666 . ? 
N7 Pd2 Cl3 88.81(16) 3_666 3_666 ? 
N7 Pd2 Cl3 91.19(16) . 3_666 ? 
N7 Pd2 Cl3 91.19(16) 3_666 . ? 
N7 Pd2 Cl3 88.81(16) . . ? 
Cl3 Pd2 Cl3 180.0 3_666 . ? 
C27 N7 C28 118.4(6) . . ? 
C27 N7 Pd2 122.5(5) . . ? 
C28 N7 Pd2 117.3(4) . . ? 
C27 N8 C34 125.6(8) . . ? 
C27 N8 H8N 105.3 . . ? 
C34 N8 H8N 104.9 . . ? 
C27 N9 C37 124.0(7) . . ? 
C27 N9 H9N 116(6) . . ? 
C37 N9 H9N 114(6) . . ? 
N8 C27 N9 111.9(7) . . ? 
N8 C27 N7 125.8(8) . . ? 
N9 C27 N7 122.3(7) . . ? 
C29 C28 C33 116.1(6) . . ? 
C29 C28 N7 121.5(6) . . ? 
C33 C28 N7 122.3(6) . . ? 
F3 C29 C30 118.2(6) . . ? 
F3 C29 C28 118.3(6) . . ? 
C30 C29 C28 123.5(6) . . ? 
C29 C30 C31 118.6(6) . . ? 
C29 C30 H30 120.7 . . ? 
C31 C30 H30 120.7 . . ? 
C30 C31 C32 120.7(6) . . ? 
C30 C31 I3 120.1(5) . . ? 
C32 C31 I3 119.1(5) . . ? 
C33 C32 C31 118.5(6) . . ? 
C33 C32 H32 120.7 . . ? 
C31 C32 H32 120.7 . . ? 
C32 C33 C28 122.4(6) . . ? 
C32 C33 H33 118.8 . . ? 
C28 C33 H33 118.8 . . ? 
N8 C34 C36 110.7(8) . . ? 
N8 C34 C35 107.4(7) . . ? 
C36 C34 C35 109.1(8) . . ? 
N8 C34 H34 109.9 . . ? 
C36 C34 H34 109.9 . . ? 
C35 C34 H34 109.9 . . ? 
C34 C35 H35A 109.5 . . ? 
C34 C35 H35B 109.5 . . ? 
H35A C35 H35B 109.5 . . ? 
C34 C35 H35C 109.5 . . ? 
H35A C35 H35C 109.5 . . ? 
H35B C35 H35C 109.5 . . ? 
C34 C36 H36A 109.5 . . ? 
C34 C36 H36B 109.5 . . ? 
H36A C36 H36B 109.5 . . ? 
C34 C36 H36C 109.5 . . ? 
H36A C36 H36C 109.5 . . ? 
H36B C36 H36C 109.5 . . ? 
N9 C37 C38 110.4(7) . . ? 
N9 C37 C39 111.9(7) . . ? 
C38 C37 C39 112.0(8) . . ? 
N9 C37 H37 107.4 . . ? 
C38 C37 H37 107.4 . . ? 
C39 C37 H37 107.4 . . ? 
C37 C38 H38A 109.5 . . ? 
C37 C38 H38B 109.5 . . ? 
H38A C38 H38B 109.5 . . ? 
C37 C38 H38C 109.5 . . ? 
H38A C38 H38C 109.5 . . ? 
H38B C38 H38C 109.5 . . ? 
C37 C39 H39A 109.5 . . ? 
C37 C39 H39B 109.5 . . ? 
H39A C39 H39B 109.5 . . ? 
C37 C39 H39C 109.5 . . ? 
H39A C39 H39C 109.5 . . ? 
H39B C39 H39C 109.5 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
Cl2 Pd1 N1 C1 77.7(5) . . . . ? 
Cl1 Pd1 N1 C1 -108.3(5) . . . . ? 
Cl2 Pd1 N1 C2 -100.3(4) . . . . ? 
Cl1 Pd1 N1 C2 73.7(4) . . . . ? 
Cl2 Pd1 N4 C14 90.6(5) . . . . ? 
Cl1 Pd1 N4 C14 -83.4(5) . . . . ?  
Cl2 Pd1 N4 C15 -89.5(5) . . . . ? 
Cl1 Pd1 N4 C15 96.5(5) . . . . ? 
C11 N3 C1 N1 45.2(9) . . . . ? 
C11 N3 C1 N2 -136.0(6) . . . . ? 
C2 N1 C1 N3 29.1(9) . . . . ? 
Pd1 N1 C1 N3 -148.9(5) . . . . ? 
C2 N1 C1 N2 -149.8(6) . . . . ? 
Pd1 N1 C1 N2 32.3(8) . . . . ? 
C8 N2 C1 N3 34.2(10) . . . . ? 
C8 N2 C1 N1 -146.9(6) . . . . ? 
C1 N1 C2 C7 -131.7(7) . . . . ? 
Pd1 N1 C2 C7 46.4(7) . . . . ? 
C1 N1 C2 C3 54.3(9) . . . . ? 
Pd1 N1 C2 C3 -127.6(5) . . . . ? 
C7 C2 C3 F1 -177.9(6) . . . . ? 
N1 C2 C3 F1 -3.7(9) . . . . ? 
C7 C2 C3 C4 0.8(10) . . . . ? 
N1 C2 C3 C4 175.1(6) . . . . ? 
F1 C3 C4 C5 178.7(6) . . . . ? 
C2 C3 C4 C5 -0.1(10) . . . . ? 
C3 C4 C5 C6 -0.6(10) . . . . ? 
C3 C4 C5 I1 -178.5(5) . . . . ? 
C4 C5 C6 C7 0.5(10) . . . . ? 
I1 C5 C6 C7 178.4(5) . . . . ? 
C5 C6 C7 C2 0.3(10) . . . . ? 
C3 C2 C7 C6 -0.9(9) . . . . ? 
N1 C2 C7 C6 -175.2(6) . . . . ? 
C1 N2 C8 C10 -139.9(7) . . . . ? 
C1 N2 C8 C9 96.7(8) . . . . ? 
C1 N3 C11 C12 106.4(7) . . . . ? 
C1 N3 C11 C13 -128.6(7) . . . . ? 
C24 N6 C14 N4 26.8(11) . . . . ? 
C24 N6 C14 N5 -151.1(7) . . . . ? 
C15 N4 C14 N6 29.6(10) . . . . ? 
Pd1 N4 C14 N6 -150.5(6) . . . . ? 
C15 N4 C14 N5 -152.3(6) . . . . ? 
Pd1 N4 C14 N5 27.5(8) . . . . ? 
C21 N5 C14 N6 6.3(12) . . . . ? 
C21 N5 C14 N4 -171.8(7) . . . . ? 
C14 N4 C15 C16 46.3(10) . . . . ? 
Pd1 N4 C15 C16 -133.6(6) . . . . ? 
C14 N4 C15 C20 -136.8(7) . . . . ? 
Pd1 N4 C15 C20 43.4(8) . . . . ? 
C20 C15 C16 F2 -176.2(6) . . . . ? 
N4 C15 C16 F2 0.9(10) . . . . ? 
C20 C15 C16 C17 6.5(10) . . . . ? 
N4 C15 C16 C17 -176.5(7) . . . . ? 
F2 C16 C17 C18 179.3(6) . . . . ? 
C15 C16 C17 C18 -3.3(11) . . . . ? 
C16 C17 C18 C19 -1.7(11) . . . . ? 
C16 C17 C18 I2 174.2(5) . . . . ? 
C17 C18 C19 C20 3.3(11) . . . . ? 
I2 C18 C19 C20 -172.6(5) . . . . ? 
C16 C15 C20 C19 -4.7(10) . . . . ? 
N4 C15 C20 C19 178.1(6) . . . . ? 
C18 C19 C20 C15 0.0(11) . . . . ? 
C14 N5 C21 C23 -89.5(9) . . . . ? 
C14 N5 C21 C22 148.3(8) . . . . ? 
C14 N6 C24 C25 108.6(8) . . . . ? 
C14 N6 C24 C26 -129.3(8) . . . . ?  
Cl3 Pd2 N7 C27 127.0(6) 3_666 . . . ? 
Cl3 Pd2 N7 C27 -53.0(6) . . . . ?  
Cl3 Pd2 N7 C28 -68.4(4) 3_666 . . . ? 
Cl3 Pd2 N7 C28 111.6(4) . . . . ? 
C34 N8 C27 N9 150.8(8) . . . . ? 
C34 N8 C27 N7 -30.8(13) . . . . ? 
C37 N9 C27 N8 134.6(7) . . . . ? 
C37 N9 C27 N7 -43.8(11) . . . . ? 
C28 N7 C27 N8 152.5(7) . . . . ? 
Pd2 N7 C27 N8 -43.1(10) . . . . ? 
C28 N7 C27 N9 -29.3(10) . . . . ? 
Pd2 N7 C27 N9 135.1(6) . . . . ? 
C27 N7 C28 C29 -56.5(9) . . . . ? 
Pd2 N7 C28 C29 138.3(6) . . . . ? 
C27 N7 C28 C33 128.7(7) . . . . ? 
Pd2 N7 C28 C33 -36.5(8) . . . . ? 
C33 C28 C29 F3 176.1(6) . . . . ? 
N7 C28 C29 F3 0.9(10) . . . . ? 
C33 C28 C29 C30 -4.4(10) . . . . ? 
N7 C28 C29 C30 -179.6(6) . . . . ? 
F3 C29 C30 C31 -178.8(6) . . . . ? 
C28 C29 C30 C31 1.7(10) . . . . ? 
C29 C30 C31 C32 1.1(10) . . . . ? 
C29 C30 C31 I3 -175.6(5) . . . . ? 
C30 C31 C32 C33 -1.0(10) . . . . ? 
I3 C31 C32 C33 175.8(5) . . . . ? 
C31 C32 C33 C28 -2.0(10) . . . . ? 
C29 C28 C33 C32 4.5(10) . . . . ? 
N7 C28 C33 C32 179.6(6) . . . . ? 
C27 N8 C34 C36 -93.9(11) . . . . ? 
C27 N8 C34 C35 147.1(8) . . . . ? 
C27 N9 C37 C38 -101.4(9) . . . . ? 
C27 N9 C37 C39 133.1(8) . . . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N9 H9N Cl1  0.850(5) 2.76(3) 3.564(6) 158(8) 1_545 
N8 H8N Cl1  0.92 2.86 3.634(8) 143.2 1_545 
N6 H6N Cl3  0.850(5) 2.75(4) 3.526(6) 153(7) . 
N5 H5N Cl1  0.851(5) 2.58(4) 3.350(6) 151(7) . 
N3 H3N Cl2  0.849(5) 2.55(2) 3.358(5) 161(6) 2 
N2 H2N I1  0.849(5) 3.25(4) 3.983(5) 145(6) 4_586 
  
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.25 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    1.902 
_refine_diff_density_min   -1.513 
_refine_diff_density_rms    0.127 


###END


#=========================================================================
# Data for compound 5a (local labelling  as ea19311x)
#=========================================================================
  
data_5a 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C14 H23 N3 O' 
_chemical_formula_sum             'C14 H23 N3 O' 
_chemical_formula_weight          249.35 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'C c' 
_symmetry_space_group_name_Hall   'C -2yc'
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x, -y, z+1/2' 
 'x+1/2, y+1/2, z' 
 'x+1/2, -y+1/2, z+1/2' 
  
_cell_length_a                    12.900(7) 
_cell_length_b                    13.630(7) 
_cell_length_c                    8.531(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.176(16) 
_cell_angle_gamma                 90.00 
_cell_volume                      1500.0(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     1555 
_cell_measurement_theta_min       2.17 
_cell_measurement_theta_max       20.00 
  
_exptl_crystal_description        needle 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.35 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.104 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              544 
_exptl_absorpt_coefficient_mu     0.071 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9755 
_exptl_absorpt_correction_T_max   0.9929 
_exptl_absorpt_process_details 
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   
;
 Bruker-Nonius X8kappa APEX II CCD area detector
; 
_diffrn_measurement_method        'phi and omega scans with narrow frames' 
_diffrn_detector_area_resol_mean   8.26
_diffrn_standards_decay_%         0  
_diffrn_reflns_number             6674 
_diffrn_reflns_av_R_equivalents   0.0947 
_diffrn_reflns_av_UnetI/netI     0.0774 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          25.27 
_reflns_number_total              1371 
_reflns_number_gt                 924 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX2 Software Suite (Bruker, 2007)'
_computing_cell_refinement        'APEX2 Software Suite (Bruker, 2007)'
_computing_data_reduction         'APEX2 Software Suite (Bruker, 2007)'
_computing_structure_solution     'SIR2002 (Burla et al., 2003)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material   'SHELXTL and publCIF (Westrip, 2010)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1371 
_refine_ls_number_parameters      169 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0805 
_refine_ls_R_factor_gt            0.0681 
_refine_ls_wR_factor_ref          0.1870 
_refine_ls_wR_factor_gt           0.1352 
_refine_ls_goodness_of_fit_ref    1.015 
_refine_ls_restrained_S_all       1.049 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
O1 O 0.0766(11) 0.4864(9) 0.3648(14) 0.072(3) Uani 1 1 d U . . 
N1 N 0.1195(12) 0.0840(10) 0.2223(15) 0.061(3) Uani 1 1 d U . . 
N2 N 0.0723(12) 0.0898(10) -0.0511(15) 0.062(3) Uani 1 1 d U . . 
H2N H 0.0678 0.0396 -0.1229 0.074 Uiso 1 1 d R . . 
N3 N 0.1689(12) -0.0369(10) 0.0581(16) 0.066(3) Uani 1 1 d U . . 
H3N H 0.1857 -0.0419 -0.0463 0.079 Uiso 1 1 d R . . 
C1 C 0.1256(15) 0.0528(12) 0.082(2) 0.062(3) Uani 1 1 d U . . 
C2 C -0.0294(16) 0.1415(13) -0.0465(19) 0.064(3) Uani 1 1 d U . . 
H2 H -0.0208 0.2007 0.0217 0.077 Uiso 1 1 calc R . . 
C3 C -0.1156(15) 0.0850(16) 0.015(2) 0.070(4) Uani 1 1 d U . . 
H3C H -0.1811 0.1159 -0.0163 0.106 Uiso 1 1 calc R . . 
H3D H -0.1111 0.0828 0.1296 0.106 Uiso 1 1 calc R . . 
H3E H -0.1129 0.0181 -0.0270 0.106 Uiso 1 1 calc R . . 
C4 C -0.0510(16) 0.1776(15) -0.212(2) 0.072(4) Uani 1 1 d U . . 
H4A H 0.0119 0.2073 -0.2556 0.108 Uiso 1 1 calc R . . 
H4B H -0.1067 0.2264 -0.2101 0.108 Uiso 1 1 calc R . . 
H4C H -0.0721 0.1221 -0.2782 0.108 Uiso 1 1 calc R . . 
C5 C 0.2596(17) -0.0664(14) 0.151(2) 0.070(3) Uani 1 1 d U . . 
H5 H 0.2448 -0.0535 0.2642 0.084 Uiso 1 1 calc R . . 
C6 C 0.2776(18) -0.1746(15) 0.130(2) 0.079(4) Uani 1 1 d U . . 
H6A H 0.2226 -0.2114 0.1824 0.118 Uiso 1 1 calc R . . 
H6B H 0.3449 -0.1925 0.1748 0.118 Uiso 1 1 calc R . . 
H6C H 0.2770 -0.1904 0.0175 0.118 Uiso 1 1 calc R . . 
C7 C 0.3532(19) -0.0065(17) 0.103(3) 0.085(4) Uani 1 1 d U . . 
H7A H 0.3674 -0.0171 -0.0083 0.127 Uiso 1 1 calc R . . 
H7B H 0.4135 -0.0269 0.1654 0.127 Uiso 1 1 calc R . . 
H7C H 0.3393 0.0632 0.1216 0.127 Uiso 1 1 calc R . . 
C8 C 0.1059(14) 0.1926(13) 0.2440(16) 0.061(3) Uani 1 1 d U . . 
C9 C 0.1661(15) 0.2616(12) 0.161(2) 0.063(3) Uani 1 1 d U . . 
H9 H 0.2112 0.2416 0.0791 0.075 Uiso 1 1 calc R . . 
C10 C 0.1569(15) 0.3627(12) 0.2046(19) 0.066(3) Uani 1 1 d U . . 
H10 H 0.2006 0.4102 0.1569 0.079 Uiso 1 1 calc R . . 
C11 C 0.0869(16) 0.3912(13) 0.313(2) 0.067(3) Uani 1 1 d U . . 
C12 C 0.0384(16) 0.3230(13) 0.399(2) 0.067(3) Uani 1 1 d U . . 
H12 H -0.0016 0.3432 0.4869 0.081 Uiso 1 1 calc R . . 
C13 C 0.0449(15) 0.2256(12) 0.3651(19) 0.064(3) Uani 1 1 d U . . 
H13 H 0.0068 0.1798 0.4258 0.077 Uiso 1 1 calc R . . 
C14 C 0.1323(17) 0.5590(12) 0.294(2) 0.071(4) Uani 1 1 d U . . 
H14A H 0.2048 0.5553 0.3278 0.107 Uiso 1 1 calc R . . 
H14B H 0.1035 0.6230 0.3224 0.107 Uiso 1 1 calc R . . 
H14C H 0.1286 0.5507 0.1797 0.107 Uiso 1 1 calc R . . 
  
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
O1 C14 1.37(2) . ? 
O1 C11 1.38(2) . ? 
N1 C1 1.27(2) . ? 
N1 C8 1.50(2) . ? 
N2 C1 1.42(2) . ? 
N2 C2 1.49(2) . ? 
N2 H2N 0.9200 . ? 
N3 C1 1.36(2) . ? 
N3 C5 1.47(3) . ? 
N3 H3N 0.9200 . ? 
C2 C3 1.45(3) . ? 
C2 C4 1.52(2) . ? 
C2 H2 1.0000 . ? 
C3 H3C 0.9800 . ? 
C3 H3D 0.9800 . ? 
C3 H3E 0.9800 . ? 
C4 H4A 0.9800 . ? 
C4 H4B 0.9800 . ? 
C4 H4C 0.9800 . ? 
C5 C6 1.50(3) . ? 
C5 C7 1.51(3) . ? 
C5 H5 1.0000 . ? 
C6 H6A 0.9800 . ? 
C6 H6B 0.9800 . ? 
C6 H6C 0.9800 . ? 
C7 H7A 0.9800 . ? 
C7 H7B 0.9800 . ? 
C7 H7C 0.9800 . ? 
C8 C13 1.38(3) . ? 
C8 C9 1.41(3) . ? 
C9 C10 1.43(2) . ? 
C9 H9 0.9500 . ? 
C10 C11 1.35(3) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.35(3) . ? 
C12 C13 1.36(2) . ? 
C12 H12 0.9500 . ? 
C13 H13 0.9500 . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C14 H14C 0.9800 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C14 O1 C11 119.0(15) . . ? 
C1 N1 C8 116.9(13) . . ? 
C1 N2 C2 124.9(14) . . ? 
C1 N2 H2N 107.4 . . ? 
C2 N2 H2N 108.4 . . ? 
C1 N3 C5 119.5(14) . . ? 
C1 N3 H3N 108.1 . . ? 
C5 N3 H3N 108.2 . . ? 
N1 C1 N3 117.9(15) . . ? 
N1 C1 N2 127.1(16) . . ? 
N3 C1 N2 113.4(13) . . ? 
C3 C2 N2 115.7(14) . . ? 
C3 C2 C4 111.6(16) . . ? 
N2 C2 C4 106.7(14) . . ? 
C3 C2 H2 107.5 . . ? 
N2 C2 H2 107.5 . . ? 
C4 C2 H2 107.5 . . ? 
C2 C3 H3C 109.5 . . ? 
C2 C3 H3D 109.5 . . ? 
H3C C3 H3D 109.5 . . ? 
C2 C3 H3E 109.5 . . ? 
H3C C3 H3E 109.5 . . ? 
H3D C3 H3E 109.5 . . ? 
C2 C4 H4A 109.5 . . ? 
C2 C4 H4B 109.5 . . ? 
H4A C4 H4B 109.5 . . ? 
C2 C4 H4C 109.5 . . ? 
H4A C4 H4C 109.5 . . ? 
H4B C4 H4C 109.5 . . ? 
N3 C5 C6 109.1(16) . . ? 
N3 C5 C7 109.9(16) . . ? 
C6 C5 C7 111.8(18) . . ? 
N3 C5 H5 108.6 . . ? 
C6 C5 H5 108.6 . . ? 
C7 C5 H5 108.6 . . ? 
C5 C6 H6A 109.5 . . ? 
C5 C6 H6B 109.5 . . ? 
H6A C6 H6B 109.5 . . ? 
C5 C6 H6C 109.5 . . ? 
H6A C6 H6C 109.5 . . ? 
H6B C6 H6C 109.5 . . ? 
C5 C7 H7A 109.5 . . ? 
C5 C7 H7B 109.5 . . ? 
H7A C7 H7B 109.5 . . ? 
C5 C7 H7C 109.5 . . ? 
H7A C7 H7C 109.5 . . ? 
H7B C7 H7C 109.5 . . ? 
C13 C8 C9 118.4(15) . . ? 
C13 C8 N1 118.8(14) . . ? 
C9 C8 N1 122.0(14) . . ? 
C8 C9 C10 117.7(17) . . ? 
C8 C9 H9 121.2 . . ? 
C10 C9 H9 121.2 . . ? 
C11 C10 C9 120.7(17) . . ? 
C11 C10 H10 119.6 . . ? 
C9 C10 H10 119.6 . . ? 
C12 C11 C10 119.3(16) . . ? 
C12 C11 O1 115.3(17) . . ? 
C10 C11 O1 123.9(17) . . ? 
C11 C12 C13 121.8(18) . . ? 
C11 C12 H12 119.1 . . ? 
C13 C12 H12 119.1 . . ? 
C12 C13 C8 121.0(17) . . ? 
C12 C13 H13 119.5 . . ? 
C8 C13 H13 119.5 . . ? 
O1 C14 H14A 109.5 . . ? 
O1 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
O1 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C8 N1 C1 N3 160.1(16) . . . . ? 
C8 N1 C1 N2 -35(3) . . . . ? 
C5 N3 C1 N1 -39(2) . . . . ? 
C5 N3 C1 N2 154.1(17) . . . . ? 
C2 N2 C1 N1 -27(3) . . . . ? 
C2 N2 C1 N3 138.6(17) . . . . ? 
C1 N2 C2 C3 -61(2) . . . . ? 
C1 N2 C2 C4 173.9(16) . . . . ? 
C1 N3 C5 C6 167.3(17) . . . . ? 
C1 N3 C5 C7 -70(2) . . . . ? 
C1 N1 C8 C13 144.2(17) . . . . ? 
C1 N1 C8 C9 -46(2) . . . . ? 
C13 C8 C9 C10 -2(2) . . . . ? 
N1 C8 C9 C10 -172.0(14) . . . . ? 
C8 C9 C10 C11 -5(3) . . . . ? 
C9 C10 C11 C12 12(3) . . . . ? 
C9 C10 C11 O1 177.3(16) . . . . ? 
C14 O1 C11 C12 173.1(16) . . . . ? 
C14 O1 C11 C10 7(2) . . . . ? 
C10 C11 C12 C13 -11(3) . . . . ? 
O1 C11 C12 C13 -177.6(16) . . . . ? 
C11 C12 C13 C8 3(3) . . . . ? 
C9 C8 C13 C12 3(2) . . . . ? 
N1 C8 C13 C12 173.4(14) . . . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N3 H3N N1  0.92 2.22 3.002(19) 142.0 2_554 
N2 H2N N1  0.92 2.24 3.118(19) 158.7 2_554 
  
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              25.27 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.333 
_refine_diff_density_min   -0.308 
_refine_diff_density_rms    0.303 

###END



