 
data_new 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C46 H56 N6 O4 Pd'  
_chemical_formula_sum 
 'C46 H56 N6 O4 Pd' 
_chemical_formula_weight          863.37 
 
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' 
 '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                    13.426(2) 
_cell_length_b                    10.1901(18) 
_cell_length_c                    16.699(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.720(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      2188.1(6) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     682
_cell_measurement_theta_min       2.55 
_cell_measurement_theta_max       17.97 
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             Colourless 
_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     1.310 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              904 
_exptl_absorpt_coefficient_mu     0.473 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8910 
_exptl_absorpt_correction_T_max   0.9325 
_exptl_absorpt_process_details    'SADABS (Bruker,2004)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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 APEXII CCD Area Detector' 
_diffrn_measurement_method        'Phi and Omega Scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8624 
_diffrn_reflns_av_R_equivalents   0.0901 
_diffrn_reflns_av_sigmaI/netI     0.0827 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.30 
_diffrn_reflns_theta_max          21.21 
_reflns_number_total              2386 
_reflns_number_gt                 1518 
_reflns_threshold_expression      >2sigma(I) 


_computing_data_collection        'APEXII,Bruker,2004'

_computing_cell_refinement        'APEXII,Bruker,2004'

_computing_data_reduction         'SAINT,Bruker,2004'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics     'ORTEP-3 (Farrugia, 1997)'

_computing_publication_material   'SHELXL-97 (Sheldrick, 2008)'

 
_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)+(0.0440P)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_coef        ? 
_refine_ls_number_reflns          2386 
_refine_ls_number_parameters      267 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0882 
_refine_ls_R_factor_gt            0.0417 
_refine_ls_wR_factor_ref          0.1014 
_refine_ls_wR_factor_gt           0.0840 
_refine_ls_goodness_of_fit_ref    0.999 
_refine_ls_restrained_S_all       0.999 
_refine_ls_shift/su_max           0.008 
_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 
C1 C 0.0383(5) 0.1643(6) 0.0709(3) 0.0368(16) Uani 1 1 d . . . 
C2 C 0.1177(5) 0.2535(6) 0.0767(4) 0.0404(17) Uani 1 1 d . . . 
C3 C 0.2033(5) 0.2618(6) 0.0373(4) 0.0424(17) Uani 1 1 d . . . 
C4 C 0.3060(5) 0.2427(6) 0.0857(4) 0.0446(18) Uani 1 1 d . . . 
C5 C 0.3847(5) 0.2614(7) 0.0493(5) 0.060(2) Uani 1 1 d . . . 
H5 H 0.4531 0.2524 0.0822 0.073 Uiso 1 1 calc R . . 
C6 C 0.3665(6) 0.2927(7) -0.0342(5) 0.0551(19) Uani 1 1 d . . . 
C7 C 0.2655(6) 0.3034(7) -0.0816(4) 0.058(2) Uani 1 1 d . . . 
H7 H 0.2517 0.3210 -0.1384 0.069 Uiso 1 1 calc R . . 
C8 C 0.1831(5) 0.2893(7) -0.0486(4) 0.048(2) Uani 1 1 d . . . 
C9 C 0.3297(5) 0.2018(7) 0.1768(4) 0.062(2) Uani 1 1 d . . . 
H9A H 0.3315 0.2780 0.2109 0.094 Uiso 1 1 calc R . . 
H9B H 0.3960 0.1584 0.1938 0.094 Uiso 1 1 calc R . . 
H9C H 0.2767 0.1429 0.1831 0.094 Uiso 1 1 calc R . . 
C10 C 0.4555(6) 0.3174(9) -0.0711(5) 0.093(3) Uani 1 1 d . . . 
H10A H 0.4286 0.3275 -0.1306 0.140 Uiso 1 1 calc R . . 
H10B H 0.5027 0.2445 -0.0587 0.140 Uiso 1 1 calc R . . 
H10C H 0.4915 0.3960 -0.0473 0.140 Uiso 1 1 calc R . . 
C11 C 0.0730(5) 0.3050(8) -0.1020(4) 0.073(2) Uani 1 1 d . . . 
H11A H 0.0715 0.3086 -0.1598 0.109 Uiso 1 1 calc R . . 
H11B H 0.0446 0.3847 -0.0871 0.109 Uiso 1 1 calc R . . 
H11C H 0.0323 0.2317 -0.0933 0.109 Uiso 1 1 calc R . . 
C12 C -0.1003(5) 0.1675(7) 0.1475(4) 0.0427(17) Uani 1 1 d . . . 
C13 C -0.1957(5) 0.2280(7) 0.1146(4) 0.0474(18) Uani 1 1 d . . . 
C14 C -0.2799(6) 0.1733(8) 0.1327(4) 0.062(2) Uani 1 1 d . . . 
H14 H -0.3447 0.2125 0.1111 0.074 Uiso 1 1 calc R . . 
C15 C -0.2729(6) 0.0638(9) 0.1811(5) 0.063(2) Uani 1 1 d . . . 
C16 C -0.1765(6) 0.0080(9) 0.2158(4) 0.0675(19) Uani 1 1 d . . . 
H16 H -0.1708 -0.0653 0.2500 0.081 Uiso 1 1 calc R . . 
C17 C -0.0878(6) 0.0591(7) 0.2005(4) 0.0523(19) Uani 1 1 d . . . 
C18 C -0.2052(6) 0.3463(8) 0.0599(5) 0.075(3) Uani 1 1 d . . . 
H18A H -0.2769 0.3718 0.0398 0.112 Uiso 1 1 calc R . . 
H18B H -0.1795 0.3260 0.0134 0.112 Uiso 1 1 calc R . . 
H18C H -0.1654 0.4170 0.0915 0.112 Uiso 1 1 calc R . . 
C19 C -0.3677(6) 0.0010(10) 0.1966(5) 0.102(3) Uani 1 1 d . . . 
H19A H -0.4053 0.0655 0.2181 0.153 Uiso 1 1 calc R . . 
H19B H -0.3463 -0.0689 0.2364 0.153 Uiso 1 1 calc R . . 
H19C H -0.4117 -0.0336 0.1450 0.153 Uiso 1 1 calc R . . 
C20 C 0.0186(5) 0.0013(9) 0.2413(4) 0.082(2) Uani 1 1 d . . . 
H20A H 0.0654 0.0699 0.2679 0.123 Uiso 1 1 calc R . . 
H20B H 0.0442 -0.0401 0.1995 0.123 Uiso 1 1 calc R . . 
H20C H 0.0135 -0.0624 0.2823 0.123 Uiso 1 1 calc R . . 
C21 C -0.1971(6) 0.1063(8) -0.0884(5) 0.059(2) Uani 1 1 d . . . 
C22 C -0.3178(5) 0.1228(9) -0.0980(5) 0.091(3) Uani 1 1 d . . . 
H22A H -0.3334 0.2139 -0.0934 0.137 Uiso 1 1 calc R . . 
H22B H -0.3354 0.0741 -0.0547 0.137 Uiso 1 1 calc R . . 
H22C H -0.3575 0.0902 -0.1516 0.137 Uiso 1 1 calc R . . 
C23 C 0.1720(5) 0.4696(7) 0.1573(5) 0.079(3) Uani 1 1 d . . . 
H23A H 0.1277 0.5399 0.1644 0.118 Uiso 1 1 calc R . . 
H23B H 0.2047 0.4932 0.1153 0.118 Uiso 1 1 calc R . . 
H23C H 0.2243 0.4535 0.2092 0.118 Uiso 1 1 calc R . . 
N1 N -0.0101(4) 0.2170(5) 0.1260(3) 0.0419(14) Uani 1 1 d . . . 
N2 N 0.0318(4) 0.3286(6) 0.1634(3) 0.0566(16) Uani 1 1 d . . . 
N3 N 0.1090(4) 0.3493(5) 0.1310(3) 0.0507(15) Uani 1 1 d . . . 
O1 O -0.1533(3) 0.0429(4) -0.0269(3) 0.0534(14) Uani 1 1 d . . . 
O2 O -0.1654(5) 0.1517(8) -0.1387(4) 0.130(3) Uani 1 1 d . . . 
Pd1 Pd 0.0000 0.0000 0.0000 0.0349(2) Uani 1 2 d S . . 
 
 
_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 
C1 N1 1.379(7) . ? 
C1 C2 1.383(8) . ? 
C1 Pd1 2.030(6) . ? 
C2 N3 1.360(7) . ? 
C2 C3 1.482(8) . ? 
C3 C4 1.397(8) . ? 
C3 C8 1.409(8) . ? 
C4 C5 1.376(8) . ? 
C4 C9 1.519(8) . ? 
C5 C6 1.381(9) . ? 
C5 H5 0.9300 . ? 
C6 C7 1.363(9) . ? 
C6 C10 1.515(9) . ? 
C7 C8 1.378(8) . ? 
C7 H7 0.9300 . ? 
C8 C11 1.499(8) . ? 
C9 H9A 0.9600 . ? 
C9 H9B 0.9600 . ? 
C9 H9C 0.9600 . ? 
C10 H10A 0.9600 . ? 
C10 H10B 0.9600 . ? 
C10 H10C 0.9600 . ? 
C11 H11A 0.9600 . ? 
C11 H11B 0.9600 . ? 
C11 H11C 0.9600 . ? 
C12 C13 1.386(9) . ? 
C12 C17 1.395(9) . ? 
C12 N1 1.449(7) . ? 
C13 C14 1.370(9) . ? 
C13 C18 1.495(9) . ? 
C14 C15 1.365(9) . ? 
C14 H14 0.9300 . ? 
C15 C16 1.379(9) . ? 
C15 C19 1.512(9) . ? 
C16 C17 1.389(9) . ? 
C16 H16 0.9300 . ? 
C17 C20 1.514(9) . ? 
C18 H18A 0.9600 . ? 
C18 H18B 0.9600 . ? 
C18 H18C 0.9600 . ? 
C19 H19A 0.9600 . ? 
C19 H19B 0.9600 . ? 
C19 H19C 0.9600 . ? 
C20 H20A 0.9600 . ? 
C20 H20B 0.9600 . ? 
C20 H20C 0.9600 . ? 
C21 O2 1.143(8) . ? 
C21 O1 1.213(8) . ? 
C21 C22 1.591(10) . ? 
C22 H22A 0.9600 . ? 
C22 H22B 0.9600 . ? 
C22 H22C 0.9600 . ? 
C23 N3 1.482(8) . ? 
C23 H23A 0.9600 . ? 
C23 H23B 0.9600 . ? 
C23 H23C 0.9600 . ? 
N1 N2 1.341(7) . ? 
N2 N3 1.317(7) . ? 
O1 Pd1 2.024(4) . ? 
Pd1 O1 2.024(4) 3 ? 
Pd1 C1 2.030(6) 3 ? 
 
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 C1 C2 101.5(5) . . ? 
N1 C1 Pd1 128.4(5) . . ? 
C2 C1 Pd1 130.1(5) . . ? 
N3 C2 C1 107.8(6) . . ? 
N3 C2 C3 118.8(6) . . ? 
C1 C2 C3 133.4(6) . . ? 
C4 C3 C8 119.0(6) . . ? 
C4 C3 C2 119.8(6) . . ? 
C8 C3 C2 121.2(6) . . ? 
C5 C4 C3 118.7(6) . . ? 
C5 C4 C9 120.9(6) . . ? 
C3 C4 C9 120.4(6) . . ? 
C4 C5 C6 122.9(6) . . ? 
C4 C5 H5 118.6 . . ? 
C6 C5 H5 118.6 . . ? 
C7 C6 C5 117.5(7) . . ? 
C7 C6 C10 121.3(7) . . ? 
C5 C6 C10 121.2(7) . . ? 
C6 C7 C8 122.5(7) . . ? 
C6 C7 H7 118.7 . . ? 
C8 C7 H7 118.7 . . ? 
C7 C8 C3 119.1(6) . . ? 
C7 C8 C11 121.3(6) . . ? 
C3 C8 C11 119.6(6) . . ? 
C4 C9 H9A 109.5 . . ? 
C4 C9 H9B 109.5 . . ? 
H9A C9 H9B 109.5 . . ? 
C4 C9 H9C 109.5 . . ? 
H9A C9 H9C 109.5 . . ? 
H9B C9 H9C 109.5 . . ? 
C6 C10 H10A 109.5 . . ? 
C6 C10 H10B 109.5 . . ? 
H10A C10 H10B 109.5 . . ? 
C6 C10 H10C 109.5 . . ? 
H10A C10 H10C 109.5 . . ? 
H10B C10 H10C 109.5 . . ? 
C8 C11 H11A 109.5 . . ? 
C8 C11 H11B 109.5 . . ? 
H11A C11 H11B 109.5 . . ? 
C8 C11 H11C 109.5 . . ? 
H11A C11 H11C 109.5 . . ? 
H11B C11 H11C 109.5 . . ? 
C13 C12 C17 122.2(7) . . ? 
C13 C12 N1 119.4(6) . . ? 
C17 C12 N1 118.5(6) . . ? 
C14 C13 C12 117.3(7) . . ? 
C14 C13 C18 122.2(7) . . ? 
C12 C13 C18 120.5(7) . . ? 
C15 C14 C13 122.9(7) . . ? 
C15 C14 H14 118.6 . . ? 
C13 C14 H14 118.6 . . ? 
C14 C15 C16 118.8(7) . . ? 
C14 C15 C19 122.0(8) . . ? 
C16 C15 C19 119.2(8) . . ? 
C15 C16 C17 121.2(8) . . ? 
C15 C16 H16 119.4 . . ? 
C17 C16 H16 119.4 . . ? 
C16 C17 C12 117.5(7) . . ? 
C16 C17 C20 121.3(7) . . ? 
C12 C17 C20 121.3(7) . . ? 
C13 C18 H18A 109.5 . . ? 
C13 C18 H18B 109.5 . . ? 
H18A C18 H18B 109.5 . . ? 
C13 C18 H18C 109.5 . . ? 
H18A C18 H18C 109.5 . . ? 
H18B C18 H18C 109.5 . . ? 
C15 C19 H19A 109.5 . . ? 
C15 C19 H19B 109.5 . . ? 
H19A C19 H19B 109.5 . . ? 
C15 C19 H19C 109.5 . . ? 
H19A C19 H19C 109.5 . . ? 
H19B C19 H19C 109.5 . . ? 
C17 C20 H20A 109.5 . . ? 
C17 C20 H20B 109.5 . . ? 
H20A C20 H20B 109.5 . . ? 
C17 C20 H20C 109.5 . . ? 
H20A C20 H20C 109.5 . . ? 
H20B C20 H20C 109.5 . . ? 
O2 C21 O1 130.2(9) . . ? 
O2 C21 C22 117.9(8) . . ? 
O1 C21 C22 111.9(8) . . ? 
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 . . ? 
N3 C23 H23A 109.5 . . ? 
N3 C23 H23B 109.5 . . ? 
H23A C23 H23B 109.5 . . ? 
N3 C23 H23C 109.5 . . ? 
H23A C23 H23C 109.5 . . ? 
H23B C23 H23C 109.5 . . ? 
N2 N1 C1 115.2(5) . . ? 
N2 N1 C12 116.6(5) . . ? 
C1 N1 C12 128.2(5) . . ? 
N3 N2 N1 102.7(5) . . ? 
N2 N3 C2 112.8(5) . . ? 
N2 N3 C23 117.4(6) . . ? 
C2 N3 C23 129.8(6) . . ? 
C21 O1 Pd1 121.1(5) . . ? 
O1 Pd1 O1 180.0(3) 3 . ? 
O1 Pd1 C1 91.3(2) 3 3 ? 
O1 Pd1 C1 88.7(2) . 3 ? 
O1 Pd1 C1 88.7(2) 3 . ? 
O1 Pd1 C1 91.3(2) . . ? 
C1 Pd1 C1 180.0(3) 3 . ? 
 
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 
N1 C1 C2 N3 -1.3(7) . . . . ? 
Pd1 C1 C2 N3 178.1(4) . . . . ? 
N1 C1 C2 C3 178.7(6) . . . . ? 
Pd1 C1 C2 C3 -2.0(11) . . . . ? 
N3 C2 C3 C4 69.5(8) . . . . ? 
C1 C2 C3 C4 -110.4(8) . . . . ? 
N3 C2 C3 C8 -110.2(7) . . . . ? 
C1 C2 C3 C8 69.9(10) . . . . ? 
C8 C3 C4 C5 4.9(9) . . . . ? 
C2 C3 C4 C5 -174.8(6) . . . . ? 
C8 C3 C4 C9 -174.9(6) . . . . ? 
C2 C3 C4 C9 5.5(9) . . . . ? 
C3 C4 C5 C6 -2.8(11) . . . . ? 
C9 C4 C5 C6 176.9(7) . . . . ? 
C4 C5 C6 C7 -0.9(11) . . . . ? 
C4 C5 C6 C10 177.6(7) . . . . ? 
C5 C6 C7 C8 2.6(11) . . . . ? 
C10 C6 C7 C8 -176.0(7) . . . . ? 
C6 C7 C8 C3 -0.4(11) . . . . ? 
C6 C7 C8 C11 178.4(7) . . . . ? 
C4 C3 C8 C7 -3.4(10) . . . . ? 
C2 C3 C8 C7 176.3(6) . . . . ? 
C4 C3 C8 C11 177.7(6) . . . . ? 
C2 C3 C8 C11 -2.6(10) . . . . ? 
C17 C12 C13 C14 -3.1(10) . . . . ? 
N1 C12 C13 C14 176.4(6) . . . . ? 
C17 C12 C13 C18 178.3(6) . . . . ? 
N1 C12 C13 C18 -2.3(9) . . . . ? 
C12 C13 C14 C15 0.0(11) . . . . ? 
C18 C13 C14 C15 178.6(7) . . . . ? 
C13 C14 C15 C16 2.3(11) . . . . ? 
C13 C14 C15 C19 -176.6(7) . . . . ? 
C14 C15 C16 C17 -1.6(11) . . . . ? 
C19 C15 C16 C17 177.3(7) . . . . ? 
C15 C16 C17 C12 -1.2(10) . . . . ? 
C15 C16 C17 C20 177.5(7) . . . . ? 
C13 C12 C17 C16 3.6(10) . . . . ? 
N1 C12 C17 C16 -175.8(6) . . . . ? 
C13 C12 C17 C20 -175.0(6) . . . . ? 
N1 C12 C17 C20 5.5(9) . . . . ? 
C2 C1 N1 N2 0.4(7) . . . . ? 
Pd1 C1 N1 N2 -178.9(4) . . . . ? 
C2 C1 N1 C12 179.8(6) . . . . ? 
Pd1 C1 N1 C12 0.4(9) . . . . ? 
C13 C12 N1 N2 75.4(7) . . . . ? 
C17 C12 N1 N2 -105.1(7) . . . . ? 
C13 C12 N1 C1 -103.9(7) . . . . ? 
C17 C12 N1 C1 75.5(8) . . . . ? 
C1 N1 N2 N3 0.6(7) . . . . ? 
C12 N1 N2 N3 -178.9(5) . . . . ? 
N1 N2 N3 C2 -1.4(7) . . . . ? 
N1 N2 N3 C23 178.3(5) . . . . ? 
C1 C2 N3 N2 1.8(8) . . . . ? 
C3 C2 N3 N2 -178.2(5) . . . . ? 
C1 C2 N3 C23 -177.9(6) . . . . ? 
C3 C2 N3 C23 2.1(10) . . . . ? 
O2 C21 O1 Pd1 -0.7(13) . . . . ? 
C22 C21 O1 Pd1 177.9(4) . . . . ? 
C21 O1 Pd1 O1 164.6(5) . . . 3 ? 
C21 O1 Pd1 C1 -88.5(5) . . . 3 ? 
C21 O1 Pd1 C1 91.5(5) . . . . ? 
N1 C1 Pd1 O1 -139.3(5) . . . 3 ? 
C2 C1 Pd1 O1 41.5(6) . . . 3 ? 
N1 C1 Pd1 O1 40.7(5) . . . . ? 
C2 C1 Pd1 O1 -138.5(6) . . . . ? 
N1 C1 Pd1 C1 -3(6) . . . 3 ? 
C2 C1 Pd1 C1 178(6) . . . 3 ? 
 
_diffrn_measured_fraction_theta_max    0.985 
_diffrn_reflns_theta_full              21.21 
_diffrn_measured_fraction_theta_full   0.985 
_refine_diff_density_max    0.382 
_refine_diff_density_min   -0.507 
_refine_diff_density_rms    0.067 


_vrf_THETM01_new
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:  Even though crystal data was collected up to 0.73 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.

;
_vrf_PLAT023_new
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      21.21 Deg. 
RESPONSE: Even though crystal data was collected up to 0.73 \%A 
resolution, the crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.

;
# end Validation Reply Form