 
data_l 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C14 H19 B F4 N4 O2 Pd' 
_chemical_formula_weight          468.54 
 
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' 
 'B'  'B'   0.0013   0.0007 
 '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' 
 'F'  'F'   0.0171   0.0103 
 '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            orthorhombic 
_symmetry_space_group_name_H-M    Pnma 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z' 
 '-x-1/2, y-1/2, z-1/2' 
 
_cell_length_a                    25.328(5) 
_cell_length_b                    6.6951(13) 
_cell_length_c                    10.795(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1830.6(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        plate 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.2 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.700 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              936 
_exptl_absorpt_coefficient_mu     1.068 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.215 
_exptl_absorpt_correction_T_max   0.291 
_exptl_absorpt_process_details    'sadabs' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(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   'CCD area detector' 
_diffrn_measurement_method        'omega scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11933 
_diffrn_reflns_av_R_equivalents   0.0573 
_diffrn_reflns_av_sigmaI/netI     0.0346 
_diffrn_reflns_limit_h_min        -31 
_diffrn_reflns_limit_h_max        28 
_diffrn_reflns_limit_k_min        -8 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.05 
_diffrn_reflns_theta_max          26.76 
_reflns_number_total              2076 
_reflns_number_gt                 1847 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0516P)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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0040(7) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2076 
_refine_ls_number_parameters      193 
_refine_ls_number_restraints      12 
_refine_ls_R_factor_all           0.0455 
_refine_ls_R_factor_gt            0.0392 
_refine_ls_wR_factor_ref          0.1010 
_refine_ls_wR_factor_gt           0.0989 
_refine_ls_goodness_of_fit_ref    1.345 
_refine_ls_restrained_S_all       1.342 
_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 
B B 0.7970(3) 0.7500 0.5625(6) 0.0487(16) Uani 1 2 d S . . 
C1 C 1.1670(2) 0.2500 -0.1426(5) 0.0400(13) Uani 1 2 d S . . 
C2 C 1.10798(17) 0.2500 0.0302(4) 0.0250(9) Uani 1 2 d S . . 
C3 C 1.06304(15) 0.2500 -0.0420(5) 0.0259(10) Uani 1 2 d S . . 
H3 H 1.0657 0.2500 -0.1279 0.031 Uiso 1 2 calc SR . . 
C4 C 1.01423(17) 0.2500 0.0141(4) 0.0278(10) Uani 1 2 d S . . 
H4 H 0.9844 0.2500 -0.0363 0.033 Uiso 1 2 calc SR . . 
C5 C 1.00701(15) 0.2500 0.1414(4) 0.0195(8) Uani 1 2 d S . . 
C6 C 1.05302(18) 0.2500 0.2130(4) 0.0228(9) Uani 1 2 d S . . 
C7 C 1.10267(16) 0.2500 0.1582(4) 0.0226(9) Uani 1 2 d S . . 
H7 H 1.1327 0.2500 0.2078 0.027 Uiso 1 2 calc SR . . 
C8 C 1.01369(17) 0.2500 0.4234(4) 0.0251(9) Uani 1 2 d S . . 
C9 C 1.0772(2) 0.2500 0.5942(5) 0.0469(15) Uani 1 2 d SD . . 
C10 C 0.9815(2) 0.2500 0.6360(5) 0.0341(11) Uani 1 2 d SD . . 
C11 C 0.87021(17) 0.2500 -0.0273(5) 0.0279(10) Uani 1 2 d S . . 
C12 C 0.83642(19) 0.2500 -0.1359(5) 0.0349(11) Uani 1 2 d SD . . 
C13 C 0.82026(19) 0.2500 0.3480(4) 0.0325(10) Uani 1 2 d S . . 
C14 C 0.76825(19) 0.2500 0.4028(6) 0.0405(13) Uani 1 2 d SD . . 
F1 F 0.79500(13) 0.7500 0.4347(3) 0.0542(9) Uani 1 2 d S . . 
F2 F 0.82573(15) 0.9112(4) 0.6026(3) 0.0958(12) Uani 1 1 d . . . 
F3 F 0.74933(17) 0.8216(9) 0.6066(4) 0.073(2) Uani 0.50 1 d P . . 
H1A H 1.204(3) 0.2500 -0.146(6) 0.061(19) Uiso 1 2 d S . . 
H9A H 1.069(2) 0.2500 0.6814(18) 0.12(4) Uiso 1 2 d SD . . 
H10A H 0.9479(11) 0.2500 0.595(4) 0.053(18) Uiso 1 2 d SD . . 
H12A H 0.8000(7) 0.2500 -0.114(4) 0.052(17) Uiso 1 2 d SD . . 
H14A H 0.741(2) 0.2500 0.341(5) 0.09(3) Uiso 1 2 d SD . . 
H1B H 1.1525(14) 0.131(5) -0.179(4) 0.038(10) Uiso 1 1 d . . . 
H9B H 1.0986(14) 0.135(4) 0.578(3) 0.065(14) Uiso 1 1 d D . . 
H10B H 0.9836(11) 0.131(3) 0.686(3) 0.031(9) Uiso 1 1 d D . . 
H12B H 0.8436(13) 0.142(5) -0.191(3) 0.073(16) Uiso 1 1 d D . . 
H14B H 0.7640(19) 0.135(5) 0.454(4) 0.12(2) Uiso 1 1 d D . . 
N1 N 1.05423(14) 0.2500 0.3448(4) 0.0237(8) Uani 1 2 d S . . 
H1 H 1.0851 0.2500 0.3779 0.028 Uiso 1 2 calc SR . . 
N2 N 1.02393(15) 0.2500 0.5451(4) 0.0309(9) Uani 1 2 d S . . 
N3 N 0.89804(14) 0.2500 0.0556(4) 0.0289(9) Uani 1 2 d S . . 
N4 N 0.86080(16) 0.2500 0.3057(4) 0.0304(9) Uani 1 2 d S . . 
O1 O 1.15893(13) 0.2500 -0.0112(3) 0.0375(9) Uani 1 2 d S . . 
O2 O 0.96607(12) 0.2500 0.3877(3) 0.0290(7) Uani 1 2 d S . . 
Pd Pd 0.935908(12) 0.2500 0.21770(3) 0.02396(17) 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 
B F2 1.372(5) . ? 
B F2 1.372(5) 7_575 ? 
B F1 1.381(7) . ? 
B F3 1.384(8) 7_575 ? 
B F3 1.384(8) . ? 
C1 O1 1.433(6) . ? 
C1 H1A 0.93(6) . ? 
C1 H1B 0.96(4) . ? 
C2 O1 1.366(5) . ? 
C2 C3 1.380(6) . ? 
C2 C7 1.388(6) . ? 
C3 C4 1.377(6) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.387(6) . ? 
C4 H4 0.9300 . ? 
C5 C6 1.399(6) . ? 
C5 Pd 1.980(4) . ? 
C6 C7 1.390(6) . ? 
C6 N1 1.422(6) . ? 
C7 H7 0.9300 . ? 
C8 O2 1.266(5) . ? 
C8 N1 1.332(6) . ? 
C8 N2 1.340(6) . ? 
C9 N2 1.449(7) . ? 
C9 H9A 0.961(10) . ? 
C9 H9B 0.961(10) . ? 
C10 N2 1.455(6) . ? 
C10 H10A 0.958(10) . ? 
C10 H10B 0.961(10) . ? 
C11 N3 1.139(6) . ? 
C11 C12 1.451(7) . ? 
C12 H12A 0.951(10) . ? 
C12 H12B 0.952(10) . ? 
C13 N4 1.123(6) . ? 
C13 C14 1.444(7) . ? 
C14 H14A 0.956(10) . ? 
C14 H14B 0.953(10) . ? 
F3 F3 0.959(12) 7_575 ? 
N1 H1 0.8600 . ? 
N3 Pd 1.995(4) . ? 
N4 Pd 2.127(4) . ? 
O2 Pd 1.987(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 
F2 B F2 103.8(5) . 7_575 ? 
F2 B F1 109.6(4) . . ? 
F2 B F1 109.6(4) 7_575 . ? 
F2 B F3 128.8(5) . 7_575 ? 
F2 B F3 94.7(4) 7_575 7_575 ? 
F1 B F3 108.1(5) . 7_575 ? 
F2 B F3 94.7(4) . . ? 
F2 B F3 128.8(5) 7_575 . ? 
F1 B F3 108.1(5) . . ? 
F3 B F3 40.6(5) 7_575 . ? 
O1 C1 H1A 100(4) . . ? 
O1 C1 H1B 110(2) . . ? 
H1A C1 H1B 112(3) . . ? 
O1 C2 C3 126.5(4) . . ? 
O1 C2 C7 114.7(4) . . ? 
C3 C2 C7 118.9(4) . . ? 
C4 C3 C2 119.5(5) . . ? 
C4 C3 H3 120.3 . . ? 
C2 C3 H3 120.3 . . ? 
C3 C4 C5 123.7(4) . . ? 
C3 C4 H4 118.2 . . ? 
C5 C4 H4 118.2 . . ? 
C4 C5 C6 116.0(4) . . ? 
C4 C5 Pd 122.1(3) . . ? 
C6 C5 Pd 121.9(3) . . ? 
C7 C6 C5 121.2(4) . . ? 
C7 C6 N1 114.0(4) . . ? 
C5 C6 N1 124.8(4) . . ? 
C2 C7 C6 120.8(4) . . ? 
C2 C7 H7 119.6 . . ? 
C6 C7 H7 119.6 . . ? 
O2 C8 N1 122.7(4) . . ? 
O2 C8 N2 118.9(4) . . ? 
N1 C8 N2 118.4(4) . . ? 
N2 C9 H9A 100(4) . . ? 
N2 C9 H9B 117(3) . . ? 
H9A C9 H9B 107.2(15) . . ? 
N2 C10 H10A 110(3) . . ? 
N2 C10 H10B 109.6(19) . . ? 
H10A C10 H10B 107.9(14) . . ? 
N3 C11 C12 177.9(5) . . ? 
C11 C12 H12A 112(3) . . ? 
C11 C12 H12B 113(3) . . ? 
H12A C12 H12B 109.7(15) . . ? 
N4 C13 C14 179.7(5) . . ? 
C13 C14 H14A 111(4) . . ? 
C13 C14 H14B 110(3) . . ? 
H14A C14 H14B 108.9(15) . . ? 
F3 F3 B 69.7(3) 7_575 . ? 
C8 N1 C6 128.3(4) . . ? 
C8 N1 H1 115.8 . . ? 
C6 N1 H1 115.8 . . ? 
C8 N2 C9 122.6(4) . . ? 
C8 N2 C10 121.2(4) . . ? 
C9 N2 C10 116.2(4) . . ? 
C11 N3 Pd 170.5(4) . . ? 
C13 N4 Pd 177.4(4) . . ? 
C2 O1 C1 117.4(4) . . ? 
C8 O2 Pd 130.3(3) . . ? 
C5 Pd O2 91.97(15) . . ? 
C5 Pd N3 94.16(16) . . ? 
O2 Pd N3 173.87(14) . . ? 
C5 Pd N4 178.02(16) . . ? 
O2 Pd N4 86.05(14) . . ? 
N3 Pd N4 87.82(15) . . ? 
 
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 
O1 C2 C3 C4 180.0 . . . . ? 
C7 C2 C3 C4 0.0 . . . . ? 
C2 C3 C4 C5 0.0 . . . . ? 
C3 C4 C5 C6 0.0 . . . . ? 
C3 C4 C5 Pd 180.0 . . . . ? 
C4 C5 C6 C7 0.0 . . . . ? 
Pd C5 C6 C7 180.0 . . . . ? 
C4 C5 C6 N1 180.0 . . . . ? 
Pd C5 C6 N1 0.0 . . . . ? 
O1 C2 C7 C6 180.0 . . . . ? 
C3 C2 C7 C6 0.0 . . . . ? 
C5 C6 C7 C2 0.0 . . . . ? 
N1 C6 C7 C2 180.0 . . . . ? 
F2 B F3 F3 -150.7(4) . . . 7_575 ? 
F2 B F3 F3 -38.8(4) 7_575 . . 7_575 ? 
F1 B F3 F3 97.0(2) . . . 7_575 ? 
O2 C8 N1 C6 0.0 . . . . ? 
N2 C8 N1 C6 180.0 . . . . ? 
C7 C6 N1 C8 180.0 . . . . ? 
C5 C6 N1 C8 0.0 . . . . ? 
O2 C8 N2 C9 180.0 . . . . ? 
N1 C8 N2 C9 0.0 . . . . ? 
O2 C8 N2 C10 0.0 . . . . ? 
N1 C8 N2 C10 180.0 . . . . ? 
C12 C11 N3 Pd 180.000(3) . . . . ? 
C14 C13 N4 Pd 180.0(3) . . . . ? 
C3 C2 O1 C1 0.0 . . . . ? 
C7 C2 O1 C1 180.0 . . . . ? 
N1 C8 O2 Pd 0.0 . . . . ? 
N2 C8 O2 Pd 180.0 . . . . ? 
C4 C5 Pd O2 180.0 . . . . ? 
C6 C5 Pd O2 0.0 . . . . ? 
C4 C5 Pd N3 0.0 . . . . ? 
C6 C5 Pd N3 180.0 . . . . ? 
C4 C5 Pd N4 180.000(4) . . . . ? 
C6 C5 Pd N4 0.000(4) . . . . ? 
C8 O2 Pd C5 0.0 . . . . ? 
C8 O2 Pd N3 180.0 . . . . ? 
C8 O2 Pd N4 180.0 . . . . ? 
C11 N3 Pd C5 180.0 . . . . ? 
C11 N3 Pd O2 0.000(1) . . . . ? 
C11 N3 Pd N4 0.0 . . . . ? 
C13 N4 Pd C5 180.000(7) . . . . ? 
C13 N4 Pd O2 180.000(6) . . . . ? 
C13 N4 Pd N3 0.000(6) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.978 
_diffrn_reflns_theta_full              26.76 
_diffrn_measured_fraction_theta_full   0.978 
_refine_diff_density_max    0.789 
_refine_diff_density_min   -0.815 
_refine_diff_density_rms    0.154 
