Ticket #4479: ms4689_0.cif

 
data_shelxl 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C35 H29 Cl2 N2 O P Pd' 
_chemical_formula_weight          701.87 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'P'  'P'   0.1023   0.0942 
 '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    'P 21 21 21'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 
_cell_length_a                    9.0587(5) 
_cell_length_b                    18.1738(10) 
_cell_length_c                    18.8006(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3095.2(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(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           0.30 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.506 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1424 
_exptl_absorpt_coefficient_mu     0.855 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7834 
_exptl_absorpt_correction_T_max   0.9347 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71070 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku Mercury CCD'
_diffrn_measurement_method        \w-scans
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14524 
_diffrn_reflns_av_R_equivalents   0.0421 
_diffrn_reflns_av_sigmaI/netI     0.0478 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          2.44 
_diffrn_reflns_theta_max          30.68 
_reflns_number_total              6720 
_reflns_number_gt                 5741 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0243P)^2^+3.2468P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.00(3) 
_refine_ls_number_reflns          6720 
_refine_ls_number_parameters      380 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0548 
_refine_ls_R_factor_gt            0.0409 
_refine_ls_wR_factor_ref          0.0904 
_refine_ls_wR_factor_gt           0.0806 
_refine_ls_goodness_of_fit_ref    1.099 
_refine_ls_restrained_S_all       1.099 
_refine_ls_shift/su_max           2.661 
_refine_ls_shift/su_mean          0.007 
 
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 0.04625(3) 0.199295(17) 0.771534(14) 0.02776(7) Uani 1 1 d . . . 
Cl1 Cl -0.17263(13) 0.20502(8) 0.83206(6) 0.0492(3) Uani 1 1 d . . . 
Cl2 Cl -0.02476(12) 0.29667(7) 0.69503(5) 0.0431(2) Uani 1 1 d . . . 
P1 P 0.11852(11) 0.09701(6) 0.82726(5) 0.0277(2) Uani 1 1 d . . . 
O1 O 0.5967(4) 0.0638(2) 0.7252(2) 0.0529(9) Uani 1 1 d . . . 
N1 N 0.2534(3) 0.20162(19) 0.72821(16) 0.0273(6) Uani 1 1 d . . . 
N2 N 0.4775(4) 0.1682(2) 0.68919(18) 0.0337(8) Uani 1 1 d . . . 
C1 C 0.4982(6) 0.1013(4) 0.9448(4) 0.074(2) Uani 1 1 d . . . 
C2 C 0.3379(5) 0.1473(2) 0.71074(18) 0.0269(8) Uani 1 1 d . . . 
C9 C 0.0283(6) -0.0028(3) 0.9320(2) 0.0461(11) Uani 1 1 d . . . 
C11 C 0.6019(5) 0.1205(3) 0.6930(2) 0.0374(10) Uani 1 1 d . . . 
C12 C -0.0123(5) 0.0363(3) 0.8713(2) 0.0328(9) Uani 1 1 d . . . 
C13 C 0.2607(5) 0.1151(2) 0.8928(2) 0.0332(9) Uani 1 1 d . . . 
C14 C 0.1551(6) -0.0338(3) 0.7498(2) 0.0416(11) Uani 1 1 d . . . 
C15 C 0.2234(6) 0.1643(3) 0.9473(2) 0.0451(11) Uani 1 1 d . . . 
C16 C 0.3458(5) 0.3120(3) 0.7922(2) 0.0354(9) Uani 1 1 d . . . 
C17 C 0.4385(7) 0.2460(3) 0.5547(3) 0.0525(13) Uani 1 1 d . . . 
C19 C 0.7337(5) 0.1459(3) 0.6524(3) 0.0515(13) Uani 1 1 d . . . 
C20 C -0.2419(6) -0.0303(3) 0.8686(3) 0.0537(14) Uani 1 1 d . . . 
C21 C 0.1954(4) 0.0389(2) 0.75712(19) 0.0299(8) Uani 1 1 d . . . 
C22 C -0.0646(8) -0.0554(3) 0.9597(3) 0.0598(16) Uani 1 1 d . . . 
C23 C 0.5062(5) 0.2799(3) 0.6122(2) 0.0357(10) Uani 1 1 d . . . 
C24 C 0.4852(5) 0.2496(3) 0.6875(2) 0.0330(9) Uani 1 1 d . . . 
C25 C 0.4575(8) 0.1469(4) 1.0004(3) 0.0686(17) Uani 1 1 d . . . 
C26 C 0.2873(5) 0.0702(2) 0.7051(2) 0.0299(9) Uani 1 1 d . . . 
C27 C -0.1474(5) 0.0228(3) 0.8407(3) 0.0433(11) Uani 1 1 d . . . 
C28 C 0.2822(7) -0.0432(3) 0.6390(3) 0.0527(14) Uani 1 1 d . . . 
C29 C 0.3303(6) 0.0282(3) 0.6465(2) 0.0420(11) Uani 1 1 d . . . 
C30 C 0.3360(4) 0.2724(2) 0.7211(2) 0.0294(8) Uani 1 1 d . . . 
C31 C 0.3992(6) 0.0846(4) 0.8910(3) 0.0568(15) Uani 1 1 d . . . 
C32 C 0.5941(7) 0.3406(4) 0.6022(3) 0.0586(15) Uani 1 1 d . . . 
C33 C -0.2015(7) -0.0685(3) 0.9283(3) 0.0597(16) Uani 1 1 d . . . 
C34 C 0.6106(8) 0.3682(5) 0.5319(4) 0.083(2) Uani 1 1 d . . . 
C36 C 0.4408(8) 0.3218(4) 0.9101(3) 0.073(2) Uani 1 1 d . . . 
C38 C 0.1980(7) -0.0753(3) 0.6911(3) 0.0553(15) Uani 1 1 d . . . 
C39 C 0.3221(7) 0.1786(3) 1.0011(3) 0.0582(16) Uani 1 1 d . . . 
C40 C 0.4395(7) 0.2860(3) 0.8450(3) 0.0549(14) Uani 1 1 d . . . 
C41 C 0.4582(9) 0.2731(4) 0.4870(3) 0.0674(18) Uani 1 1 d . . . 
C42 C 0.5475(9) 0.3343(4) 0.4759(3) 0.074(2) Uani 1 1 d . . . 
C43 C 0.2654(9) 0.4080(4) 0.8702(4) 0.080(2) Uani 1 1 d . . . 
C45 C 0.3568(9) 0.3824(5) 0.9225(4) 0.082(2) Uani 1 1 d . . . 
C47 C 0.2574(7) 0.3729(3) 0.8046(3) 0.0563(14) Uani 1 1 d . . . 
H1 H -0.1770 0.0502 0.7999 0.053 Uiso 1 1 d . . . 
H2 H -0.3349 -0.0397 0.8457 0.067 Uiso 1 1 d . . . 
H3 H -0.2665 -0.1035 0.9494 0.074 Uiso 1 1 d . . . 
H4 H -0.0334 -0.0847 0.9990 0.070 Uiso 1 1 d . . . 
H5 H 0.1191 0.0079 0.9551 0.058 Uiso 1 1 d . . . 
H6 H 0.0982 -0.0567 0.7862 0.052 Uiso 1 1 d . . . 
H7 H 0.1696 -0.1260 0.6871 0.066 Uiso 1 1 d . . . 
H8 H 0.3061 -0.0698 0.5967 0.067 Uiso 1 1 d . . . 
H9 H 0.3956 0.0491 0.6122 0.052 Uiso 1 1 d . . . 
H10 H 0.3767 0.2047 0.5620 0.065 Uiso 1 1 d . . . 
H11 H 0.4099 0.2505 0.4475 0.082 Uiso 1 1 d . . . 
H12 H 0.5638 0.3519 0.4288 0.093 Uiso 1 1 d . . . 
H13 H 0.6704 0.4104 0.5244 0.098 Uiso 1 1 d . . . 
H14 H 0.6424 0.3641 0.6410 0.074 Uiso 1 1 d . . . 
H15 H 0.1941 0.3915 0.7685 0.071 Uiso 1 1 d . . . 
H17 H 0.3643 0.4063 0.9669 0.104 Uiso 1 1 d . . . 
H18 H 0.5039 0.3039 0.9470 0.088 Uiso 1 1 d . . . 
H19 H 0.5023 0.2446 0.8370 0.068 Uiso 1 1 d . . . 
H20 H 0.1289 0.1882 0.9468 0.057 Uiso 1 1 d . . . 
H21 H 0.5262 0.1559 1.0379 0.086 Uiso 1 1 d . . . 
H22 H 0.2957 0.2113 1.0391 0.072 Uiso 1 1 d . . . 
H23 H 0.5951 0.0812 0.9432 0.092 Uiso 1 1 d . . . 
H24 H 0.4271 0.0530 0.8537 0.071 Uiso 1 1 d . . . 
H28 H 0.2850 0.3031 0.6883 0.038 Uiso 1 1 d . . . 
H29 H 0.5636 0.2656 0.7170 0.041 Uiso 1 1 d . . . 
H33 H 0.2014 0.4484 0.8809 0.094 Uiso 1 1 d . . . 
H16 H 0.8158 0.1503 0.6828 0.063 Uiso 1 1 d . . . 
H25 H 0.7555 0.1105 0.6158 0.063 Uiso 1 1 d . . . 
H26 H 0.7130 0.1918 0.6305 0.063 Uiso 1 1 d . . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Pd1 0.02760(13) 0.02776(15) 0.02791(11) -0.00275(12) 0.00183(12) 0.00157(13) 
Cl1 0.0408(6) 0.0500(8) 0.0567(6) -0.0038(6) 0.0195(5) 0.0071(6) 
Cl2 0.0469(6) 0.0348(6) 0.0476(5) 0.0057(5) -0.0040(5) 0.0059(6) 
P1 0.0285(5) 0.0289(6) 0.0257(4) -0.0001(4) 0.0017(4) -0.0004(4) 
O1 0.0435(18) 0.043(2) 0.072(2) 0.0106(19) -0.003(2) 0.0058(15) 
N1 0.0285(14) 0.0251(16) 0.0282(12) 0.0007(16) 0.0004(13) -0.0027(14) 
N2 0.0302(19) 0.033(2) 0.0373(17) 0.0016(14) 0.0056(15) 0.0004(15) 
C1 0.048(3) 0.090(6) 0.085(4) -0.012(4) -0.032(3) 0.010(3) 
C2 0.0290(19) 0.029(2) 0.0222(17) 0.0000(13) -0.0005(14) -0.0024(16) 
C9 0.055(3) 0.047(3) 0.037(2) 0.0070(18) 0.000(2) -0.007(3) 
C11 0.031(2) 0.041(3) 0.041(2) -0.0051(18) 0.0010(18) 0.0051(19) 
C12 0.035(2) 0.035(2) 0.0290(18) 0.0000(15) 0.0098(15) -0.0024(17) 
C13 0.036(2) 0.034(3) 0.0287(18) 0.0010(15) -0.0016(17) -0.0030(18) 
C14 0.052(3) 0.028(3) 0.045(2) -0.0045(16) 0.014(2) -0.006(2) 
C15 0.042(3) 0.057(3) 0.037(2) -0.012(2) 0.001(2) -0.006(2) 
C16 0.040(2) 0.030(3) 0.0361(19) -0.0035(15) 0.0064(16) -0.0107(18) 
C17 0.062(3) 0.055(3) 0.041(2) 0.002(2) -0.008(3) -0.006(3) 
C19 0.032(2) 0.065(4) 0.058(3) -0.002(2) 0.006(2) 0.002(2) 
C20 0.037(3) 0.051(4) 0.073(4) -0.006(3) 0.006(3) -0.010(2) 
C21 0.032(2) 0.029(2) 0.0282(18) -0.0011(14) 0.0030(15) 0.0005(16) 
C22 0.080(4) 0.053(4) 0.046(3) 0.014(2) 0.006(3) -0.014(3) 
C23 0.033(2) 0.039(3) 0.0347(19) 0.0020(16) 0.0048(16) -0.0014(16) 
C24 0.032(2) 0.036(3) 0.0304(19) 0.0013(15) 0.0016(16) -0.0083(17) 
C25 0.065(4) 0.086(5) 0.055(3) -0.007(3) -0.029(3) -0.003(4) 
C26 0.031(2) 0.024(2) 0.0351(19) -0.0022(14) 0.0021(16) -0.0025(16) 
C27 0.036(2) 0.040(3) 0.054(3) 0.002(2) 0.004(2) 0.000(2) 
C28 0.064(4) 0.045(3) 0.049(3) -0.020(2) 0.017(3) -0.008(3) 
C29 0.047(3) 0.043(3) 0.036(2) -0.0066(18) 0.012(2) -0.003(2) 
C30 0.0310(19) 0.026(2) 0.0316(19) 0.0001(15) 0.0007(17) -0.0059(15) 
C31 0.045(3) 0.077(4) 0.049(3) -0.014(3) -0.011(2) 0.014(3) 
C32 0.054(3) 0.060(4) 0.062(3) 0.017(3) 0.003(3) -0.021(3) 
C33 0.066(4) 0.055(4) 0.059(3) 0.006(3) 0.020(3) -0.017(3) 
C34 0.062(4) 0.089(6) 0.099(5) 0.052(4) 0.008(4) -0.022(4) 
C36 0.073(4) 0.108(6) 0.039(2) -0.008(3) -0.006(3) -0.043(4) 
C38 0.068(4) 0.035(3) 0.063(3) -0.016(2) 0.020(3) -0.012(2) 
C39 0.071(4) 0.066(4) 0.037(2) -0.012(2) -0.002(3) -0.009(3) 
C40 0.060(3) 0.060(4) 0.044(2) -0.003(2) -0.006(3) -0.017(3) 
C41 0.084(4) 0.085(5) 0.033(2) 0.002(2) -0.003(3) 0.020(4) 
C42 0.064(4) 0.109(6) 0.047(3) 0.027(3) 0.018(3) 0.024(4) 
C43 0.088(5) 0.066(5) 0.086(5) -0.039(4) 0.033(4) -0.014(4) 
C45 0.093(5) 0.094(6) 0.058(4) -0.035(4) 0.021(4) -0.045(5) 
C47 0.069(4) 0.041(3) 0.058(3) -0.011(2) 0.011(3) -0.001(3) 
 
_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 2.046(3) . ? 
Pd1 P1 2.2320(11) . ? 
Pd1 Cl1 2.2884(11) . ? 
Pd1 Cl2 2.3694(12) . ? 
P1 C13 1.813(4) . ? 
P1 C12 1.818(4) . ? 
P1 C21 1.827(4) . ? 
O1 C11 1.196(6) . ? 
N1 C2 1.292(5) . ? 
N1 C30 1.494(5) . ? 
N2 C2 1.381(5) . ? 
N2 C11 1.424(6) . ? 
N2 C24 1.481(6) . ? 
C1 C25 1.383(9) . ? 
C1 C31 1.385(7) . ? 
C1 H23 0.951(6) . ? 
C2 C26 1.478(6) . ? 
C9 C22 1.376(8) . ? 
C9 C12 1.394(6) . ? 
C9 H5 0.951(5) . ? 
C11 C19 1.490(7) . ? 
C12 C27 1.375(7) . ? 
C13 C31 1.373(7) . ? 
C13 C15 1.401(6) . ? 
C14 C21 1.377(6) . ? 
C14 C38 1.393(7) . ? 
C14 H6 0.952(4) . ? 
C15 C39 1.375(7) . ? 
C15 H20 0.960(5) . ? 
C16 C47 1.385(7) . ? 
C16 C40 1.390(7) . ? 
C16 C30 1.521(6) . ? 
C17 C41 1.377(7) . ? 
C17 C23 1.388(7) . ? 
C17 H10 0.946(6) . ? 
C19 H16 0.941(5) . ? 
C19 H25 0.962(6) . ? 
C19 H26 0.950(6) . ? 
C20 C33 1.370(9) . ? 
C20 C27 1.392(7) . ? 
C20 H2 0.962(6) . ? 
C21 C26 1.405(6) . ? 
C22 C33 1.394(10) . ? 
C22 H4 0.953(5) . ? 
C23 C32 1.375(7) . ? 
C23 C24 1.530(6) . ? 
C24 C30 1.549(6) . ? 
C24 H29 0.948(4) . ? 
C25 C39 1.355(10) . ? 
C25 H21 0.955(6) . ? 
C26 C29 1.395(6) . ? 
C27 H1 0.952(5) . ? 
C28 C38 1.372(8) . ? 
C28 C29 1.376(7) . ? 
C28 H8 0.954(5) . ? 
C29 H9 0.954(5) . ? 
C30 H28 0.950(4) . ? 
C31 H24 0.941(5) . ? 
C32 C34 1.420(8) . ? 
C32 H14 0.951(6) . ? 
C33 H3 0.953(5) . ? 
C34 C42 1.347(11) . ? 
C34 H13 0.949(7) . ? 
C36 C45 1.360(11) . ? 
C36 C40 1.386(7) . ? 
C36 H18 0.956(7) . ? 
C38 H7 0.960(5) . ? 
C39 H22 0.960(5) . ? 
C40 H19 0.955(6) . ? 
C41 C42 1.390(10) . ? 
C41 H11 0.955(6) . ? 
C42 H12 0.953(5) . ? 
C43 C45 1.367(11) . ? 
C43 C47 1.391(8) . ? 
C43 H33 0.957(7) . ? 
C45 H17 0.943(6) . ? 
C47 H15 0.952(6) . ? 
 
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 P1 86.27(10) . . ? 
N1 Pd1 Cl1 172.57(9) . . ? 
P1 Pd1 Cl1 93.36(4) . . ? 
N1 Pd1 Cl2 89.54(9) . . ? 
P1 Pd1 Cl2 170.61(4) . . ? 
Cl1 Pd1 Cl2 91.87(5) . . ? 
C13 P1 C12 105.28(19) . . ? 
C13 P1 C21 108.94(19) . . ? 
C12 P1 C21 103.1(2) . . ? 
C13 P1 Pd1 112.10(15) . . ? 
C12 P1 Pd1 121.86(15) . . ? 
C21 P1 Pd1 104.74(14) . . ? 
C2 N1 C30 109.8(3) . . ? 
C2 N1 Pd1 129.0(3) . . ? 
C30 N1 Pd1 120.8(2) . . ? 
C2 N2 C11 122.8(4) . . ? 
C2 N2 C24 108.9(4) . . ? 
C11 N2 C24 124.9(4) . . ? 
C25 C1 C31 120.7(6) . . ? 
C25 C1 H23 119.9(6) . . ? 
C31 C1 H23 119.4(7) . . ? 
N1 C2 N2 114.0(4) . . ? 
N1 C2 C26 124.0(4) . . ? 
N2 C2 C26 121.6(4) . . ? 
C22 C9 C12 120.2(5) . . ? 
C22 C9 H5 119.9(5) . . ? 
C12 C9 H5 119.8(5) . . ? 
O1 C11 N2 121.2(4) . . ? 
O1 C11 C19 123.9(4) . . ? 
N2 C11 C19 114.8(4) . . ? 
C27 C12 C9 119.1(4) . . ? 
C27 C12 P1 119.9(3) . . ? 
C9 C12 P1 120.7(4) . . ? 
C31 C13 C15 119.7(4) . . ? 
C31 C13 P1 124.0(4) . . ? 
C15 C13 P1 116.2(4) . . ? 
C21 C14 C38 121.6(4) . . ? 
C21 C14 H6 119.4(4) . . ? 
C38 C14 H6 118.9(5) . . ? 
C39 C15 C13 120.1(5) . . ? 
C39 C15 H20 120.1(5) . . ? 
C13 C15 H20 119.8(4) . . ? 
C47 C16 C40 120.3(4) . . ? 
C47 C16 C30 119.5(4) . . ? 
C40 C16 C30 120.2(4) . . ? 
C41 C17 C23 120.3(6) . . ? 
C41 C17 H10 119.8(6) . . ? 
C23 C17 H10 119.9(5) . . ? 
C11 C19 H16 110.4(5) . . ? 
C11 C19 H25 108.9(5) . . ? 
H16 C19 H25 109.2(5) . . ? 
C11 C19 H26 109.7(5) . . ? 
H16 C19 H26 110.3(6) . . ? 
H25 C19 H26 108.4(6) . . ? 
C33 C20 C27 119.7(5) . . ? 
C33 C20 H2 120.7(6) . . ? 
C27 C20 H2 119.5(6) . . ? 
C14 C21 C26 118.4(4) . . ? 
C14 C21 P1 121.7(3) . . ? 
C26 C21 P1 119.7(3) . . ? 
C9 C22 C33 120.2(5) . . ? 
C9 C22 H4 120.0(7) . . ? 
C33 C22 H4 119.8(6) . . ? 
C32 C23 C17 120.4(4) . . ? 
C32 C23 C24 119.2(4) . . ? 
C17 C23 C24 120.4(4) . . ? 
N2 C24 C23 112.7(4) . . ? 
N2 C24 C30 102.6(3) . . ? 
C23 C24 C30 112.9(4) . . ? 
N2 C24 H29 109.2(4) . . ? 
C23 C24 H29 109.8(4) . . ? 
C30 C24 H29 109.4(4) . . ? 
C39 C25 C1 120.2(5) . . ? 
C39 C25 H21 120.6(7) . . ? 
C1 C25 H21 119.2(7) . . ? 
C29 C26 C21 119.6(4) . . ? 
C29 C26 C2 119.3(4) . . ? 
C21 C26 C2 121.1(4) . . ? 
C12 C27 C20 120.9(5) . . ? 
C12 C27 H1 119.6(5) . . ? 
C20 C27 H1 119.5(5) . . ? 
C38 C28 C29 120.2(4) . . ? 
C38 C28 H8 120.4(6) . . ? 
C29 C28 H8 119.4(5) . . ? 
C28 C29 C26 120.6(4) . . ? 
C28 C29 H9 120.2(5) . . ? 
C26 C29 H9 119.2(5) . . ? 
N1 C30 C16 111.0(3) . . ? 
N1 C30 C24 104.0(3) . . ? 
C16 C30 C24 115.8(3) . . ? 
N1 C30 H28 108.6(3) . . ? 
C16 C30 H28 108.7(4) . . ? 
C24 C30 H28 108.5(4) . . ? 
C13 C31 C1 119.0(5) . . ? 
C13 C31 H24 120.7(5) . . ? 
C1 C31 H24 120.3(5) . . ? 
C23 C32 C34 118.1(6) . . ? 
C23 C32 H14 121.4(5) . . ? 
C34 C32 H14 120.4(6) . . ? 
C20 C33 C22 119.9(5) . . ? 
C20 C33 H3 121.0(7) . . ? 
C22 C33 H3 119.2(6) . . ? 
C42 C34 C32 121.4(6) . . ? 
C42 C34 H13 119.6(7) . . ? 
C32 C34 H13 118.9(8) . . ? 
C45 C36 C40 121.9(7) . . ? 
C45 C36 H18 119.0(6) . . ? 
C40 C36 H18 119.1(8) . . ? 
C28 C38 C14 119.4(5) . . ? 
C28 C38 H7 120.0(5) . . ? 
C14 C38 H7 120.6(6) . . ? 
C25 C39 C15 120.1(5) . . ? 
C25 C39 H22 119.8(6) . . ? 
C15 C39 H22 120.1(6) . . ? 
C36 C40 C16 118.4(6) . . ? 
C36 C40 H19 120.3(6) . . ? 
C16 C40 H19 121.2(5) . . ? 
C17 C41 C42 120.1(6) . . ? 
C17 C41 H11 120.2(7) . . ? 
C42 C41 H11 119.7(6) . . ? 
C34 C42 C41 119.7(5) . . ? 
C34 C42 H12 120.5(8) . . ? 
C41 C42 H12 119.8(8) . . ? 
C45 C43 C47 120.9(7) . . ? 
C45 C43 H33 118.5(7) . . ? 
C47 C43 H33 120.4(9) . . ? 
C36 C45 C43 119.4(5) . . ? 
C36 C45 H17 119.0(9) . . ? 
C43 C45 H17 121.6(9) . . ? 
C16 C47 C43 119.1(6) . . ? 
C16 C47 H15 120.8(5) . . ? 
C43 C47 H15 120.1(7) . . ? 
 
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 Pd1 P1 C13 67.06(17) . . . . ? 
Cl1 Pd1 P1 C13 -105.51(15) . . . . ? 
Cl2 Pd1 P1 C13 130.8(3) . . . . ? 
N1 Pd1 P1 C12 -166.98(18) . . . . ? 
Cl1 Pd1 P1 C12 20.45(16) . . . . ? 
Cl2 Pd1 P1 C12 -103.3(3) . . . . ? 
N1 Pd1 P1 C21 -50.92(16) . . . . ? 
Cl1 Pd1 P1 C21 136.52(14) . . . . ? 
Cl2 Pd1 P1 C21 12.8(3) . . . . ? 
P1 Pd1 N1 C2 33.1(3) . . . . ? 
Cl1 Pd1 N1 C2 120.5(7) . . . . ? 
Cl2 Pd1 N1 C2 -138.5(3) . . . . ? 
P1 Pd1 N1 C30 -138.9(3) . . . . ? 
Cl1 Pd1 N1 C30 -51.5(9) . . . . ? 
Cl2 Pd1 N1 C30 49.5(3) . . . . ? 
C30 N1 C2 N2 -1.3(4) . . . . ? 
Pd1 N1 C2 N2 -174.0(2) . . . . ? 
C30 N1 C2 C26 -173.9(3) . . . . ? 
Pd1 N1 C2 C26 13.4(5) . . . . ? 
C11 N2 C2 N1 156.0(4) . . . . ? 
C24 N2 C2 N1 -4.2(5) . . . . ? 
C11 N2 C2 C26 -31.2(6) . . . . ? 
C24 N2 C2 C26 168.6(3) . . . . ? 
C2 N2 C11 O1 -11.8(7) . . . . ? 
C24 N2 C11 O1 145.3(5) . . . . ? 
C2 N2 C11 C19 166.5(4) . . . . ? 
C24 N2 C11 C19 -36.5(6) . . . . ? 
C22 C9 C12 C27 1.5(8) . . . . ? 
C22 C9 C12 P1 -171.8(5) . . . . ? 
C13 P1 C12 C27 168.1(4) . . . . ? 
C21 P1 C12 C27 -77.8(4) . . . . ? 
Pd1 P1 C12 C27 39.1(4) . . . . ? 
C13 P1 C12 C9 -18.7(4) . . . . ? 
C21 P1 C12 C9 95.5(4) . . . . ? 
Pd1 P1 C12 C9 -147.7(3) . . . . ? 
C12 P1 C13 C31 105.5(5) . . . . ? 
C21 P1 C13 C31 -4.5(5) . . . . ? 
Pd1 P1 C13 C31 -119.9(5) . . . . ? 
C12 P1 C13 C15 -75.3(4) . . . . ? 
C21 P1 C13 C15 174.7(4) . . . . ? 
Pd1 P1 C13 C15 59.3(4) . . . . ? 
C31 C13 C15 C39 -3.9(8) . . . . ? 
P1 C13 C15 C39 176.9(4) . . . . ? 
C38 C14 C21 C26 -2.8(7) . . . . ? 
C38 C14 C21 P1 171.2(4) . . . . ? 
C13 P1 C21 C14 108.8(4) . . . . ? 
C12 P1 C21 C14 -2.6(4) . . . . ? 
Pd1 P1 C21 C14 -131.1(4) . . . . ? 
C13 P1 C21 C26 -77.2(4) . . . . ? 
C12 P1 C21 C26 171.3(3) . . . . ? 
Pd1 P1 C21 C26 42.9(4) . . . . ? 
C12 C9 C22 C33 -1.7(9) . . . . ? 
C41 C17 C23 C32 -0.3(9) . . . . ? 
C41 C17 C23 C24 -179.6(6) . . . . ? 
C2 N2 C24 C23 -114.3(4) . . . . ? 
C11 N2 C24 C23 86.0(5) . . . . ? 
C2 N2 C24 C30 7.4(4) . . . . ? 
C11 N2 C24 C30 -152.3(4) . . . . ? 
C32 C23 C24 N2 -143.1(5) . . . . ? 
C17 C23 C24 N2 36.2(6) . . . . ? 
C32 C23 C24 C30 101.2(5) . . . . ? 
C17 C23 C24 C30 -79.4(6) . . . . ? 
C31 C1 C25 C39 -3.1(12) . . . . ? 
C14 C21 C26 C29 2.5(7) . . . . ? 
P1 C21 C26 C29 -171.7(4) . . . . ? 
C14 C21 C26 C2 -178.3(4) . . . . ? 
P1 C21 C26 C2 7.5(6) . . . . ? 
N1 C2 C26 C29 134.9(4) . . . . ? 
N2 C2 C26 C29 -37.1(6) . . . . ? 
N1 C2 C26 C21 -44.3(6) . . . . ? 
N2 C2 C26 C21 143.7(4) . . . . ? 
C9 C12 C27 C20 -1.4(7) . . . . ? 
P1 C12 C27 C20 172.0(4) . . . . ? 
C33 C20 C27 C12 1.5(9) . . . . ? 
C38 C28 C29 C26 -3.6(9) . . . . ? 
C21 C26 C29 C28 0.7(7) . . . . ? 
C2 C26 C29 C28 -178.5(5) . . . . ? 
C2 N1 C30 C16 -119.3(4) . . . . ? 
Pd1 N1 C30 C16 54.1(4) . . . . ? 
C2 N1 C30 C24 5.9(4) . . . . ? 
Pd1 N1 C30 C24 179.3(2) . . . . ? 
C47 C16 C30 N1 -104.7(5) . . . . ? 
C40 C16 C30 N1 73.3(5) . . . . ? 
C47 C16 C30 C24 137.0(5) . . . . ? 
C40 C16 C30 C24 -45.0(6) . . . . ? 
N2 C24 C30 N1 -7.7(4) . . . . ? 
C23 C24 C30 N1 113.8(4) . . . . ? 
N2 C24 C30 C16 114.3(4) . . . . ? 
C23 C24 C30 C16 -124.2(4) . . . . ? 
C15 C13 C31 C1 2.1(9) . . . . ? 
P1 C13 C31 C1 -178.8(5) . . . . ? 
C25 C1 C31 C13 1.3(11) . . . . ? 
C17 C23 C32 C34 1.3(9) . . . . ? 
C24 C23 C32 C34 -179.3(6) . . . . ? 
C27 C20 C33 C22 -1.6(10) . . . . ? 
C9 C22 C33 C20 1.8(10) . . . . ? 
C23 C32 C34 C42 -2.8(12) . . . . ? 
C29 C28 C38 C14 3.3(10) . . . . ? 
C21 C14 C38 C28 -0.1(9) . . . . ? 
C1 C25 C39 C15 1.3(11) . . . . ? 
C13 C15 C39 C25 2.1(9) . . . . ? 
C45 C36 C40 C16 -2.0(10) . . . . ? 
C47 C16 C40 C36 0.6(8) . . . . ? 
C30 C16 C40 C36 -177.4(5) . . . . ? 
C23 C17 C41 C42 0.7(10) . . . . ? 
C32 C34 C42 C41 3.2(12) . . . . ? 
C17 C41 C42 C34 -2.1(11) . . . . ? 
C40 C36 C45 C43 1.7(11) . . . . ? 
C47 C43 C45 C36 -0.1(11) . . . . ? 
C40 C16 C47 C43 0.9(9) . . . . ? 
C30 C16 C47 C43 178.9(5) . . . . ? 
C45 C43 C47 C16 -1.2(11) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.761 
_diffrn_reflns_theta_full              30.68 
_diffrn_measured_fraction_theta_full   0.761 
_refine_diff_density_max    1.023 
_refine_diff_density_min   -0.948 
_refine_diff_density_rms    0.094