# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/253 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; - ; _chemical_name_common - _chemical_formula_moiety 'C18 H16 Cl N2 P' _chemical_formula_structural 'C18 H16 Cl N2 P' _chemical_formula_analytical 'C18 H16 Cl N2 P' _chemical_formula_sum 'C18 H16 Cl N2 P' _chemical_formula_weight 326.75 _chemical_melting_point - _chemical_compound_source - 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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 13.3340(12) _cell_length_b 5.8545(5) _cell_length_c 21.617(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.761(2) _cell_angle_gamma 90.00 _cell_volume 1687.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max .08 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .32 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method - _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.319 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.125186 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; - ; _diffrn_ambient_temperature 293(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 6101 _diffrn_reflns_av_R_equivalents 0.2699 _diffrn_reflns_av_sigmaI/netI 0.1642 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2325 _reflns_number_observed 1695 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 60 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.6808P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0113(51) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2265 _refine_ls_number_parameters 228 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1537 _refine_ls_R_factor_obs 0.0881 _refine_ls_wR_factor_all 0.3183 _refine_ls_wR_factor_obs 0.1656 _refine_ls_goodness_of_fit_all 1.142 _refine_ls_goodness_of_fit_obs 1.197 _refine_ls_restrained_S_all 1.959 _refine_ls_restrained_S_obs 1.197 _refine_ls_shift/esd_max -0.103 _refine_ls_shift/esd_mean 0.009 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.23268(8) 0.0598(2) 0.09204(5) 0.0504(5) Uani 1 d . . C1 C 0.2792(3) 0.1615(7) 0.1669(2) 0.0499(11) Uani 1 d G . C2 C 0.3600(3) 0.0663(9) 0.1991(2) 0.0627(13) Uani 1 d G . H2A H 0.3927(23) -0.0602(50) 0.1829(12) 0.075 Uiso 1 calc R . C3 C 0.3921(5) 0.1577(13) 0.2548(3) 0.085(2) Uani 1 d G . H3A H 0.4466(5) 0.0934(13) 0.2757(3) 0.102 Uiso 1 calc R . C4 C 0.3447(6) 0.3397(15) 0.2790(3) 0.103(2) Uani 1 d G . H4A H 0.3660(6) 0.3980(15) 0.3170(3) 0.124 Uiso 1 calc R . C5 C 0.2658(5) 0.4396(11) 0.2485(3) 0.088(2) Uani 1 d G . H5A H 0.2335(5) 0.5650(11) 0.2655(3) 0.106 Uiso 1 calc R . C6 C 0.2347(4) 0.3527(9) 0.1922(2) 0.0657(14) Uani 1 d G . H6A H 0.1826(4) 0.4241(9) 0.1707(2) 0.079 Uiso 1 calc R . C7 C 0.1150(3) -0.0819(9) 0.1130(2) 0.0573(13) Uani 1 d G . C8 C 0.0812(4) -0.1019(10) 0.1733(2) 0.0696(15) Uani 1 d G . H8A H 0.1196(20) -0.0446(80) 0.2060(3) 0.084 Uiso 1 calc R . C9 C -0.0104(5) -0.2078(12) 0.1847(3) 0.100(2) Uani 1 d G . H9A H -0.0327(5) -0.2215(12) 0.2251(3) 0.121 Uiso 1 calc R . C10 C -0.0660(5) -0.2895(15) 0.1381(5) 0.136(3) Uani 1 d G . H10A H -0.1282(5) -0.3540(15) 0.1462(5) 0.163 Uiso 1 calc R . C11 C -0.0337(5) -0.2802(20) 0.0797(4) 0.167(5) Uani 1 d G . H11A H -0.0712(5) -0.3471(20) 0.0480(4) 0.200 Uiso 1 calc R . C12 C 0.0563(4) -0.1700(16) 0.0667(3) 0.119(3) Uani 1 d G . H12A H 0.0766(4) -0.1564(16) 0.0259(3) 0.143 Uiso 1 calc R . C13 C 0.3082(3) -0.1992(8) 0.0805(2) 0.0528(12) Uani 1 d . . H13A H 0.3127(3) -0.2836(8) 0.1190(2) 0.063 Uiso 1 calc R . H13B H 0.2753(3) -0.2960(8) 0.0500(2) 0.063 Uiso 1 calc R . N14 N 0.4093(2) -0.1442(6) 0.0597(2) 0.0483(10) Uani 1 d D . H14N H 0.4136(27) -0.0219(46) 0.0290(13) 0.042(11) Uiso 1 d D . C15 C 0.4867(3) -0.2950(7) 0.0660(2) 0.0431(11) Uani 1 d . . N16 N 0.5754(2) -0.2228(6) 0.0429(2) 0.0490(10) Uani 1 d . . C17 C 0.6545(3) -0.3623(8) 0.0502(2) 0.0514(12) Uani 1 d . . H17A H 0.7159(3) -0.3138(8) 0.0352(2) 0.062 Uiso 1 calc R . C18 C 0.6505(3) -0.5726(8) 0.0787(2) 0.0476(11) Uani 1 d . . Cl18 Cl 0.75722(9) -0.7422(2) 0.08559(6) 0.0700(5) Uani 1 d . . C19 C 0.5600(3) -0.6449(8) 0.1001(2) 0.0557(12) Uani 1 d . . H19A H 0.5543(3) -0.7876(8) 0.1186(2) 0.067 Uiso 1 calc R . C20 C 0.4778(3) -0.5068(8) 0.0942(2) 0.0506(12) Uani 1 d . . H20A H 0.4161(3) -0.5546(8) 0.1090(2) 0.061 Uiso 1 calc R . 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 P1 0.0458(7) 0.0589(8) 0.0467(8) 0.0037(6) 0.0106(5) -0.0017(6) C1 0.050(2) 0.047(3) 0.053(3) -0.003(2) 0.013(2) -0.007(2) C2 0.066(3) 0.068(4) 0.054(3) 0.003(3) 0.003(2) -0.001(3) C3 0.089(4) 0.106(5) 0.059(4) -0.004(4) -0.009(3) -0.011(4) C4 0.128(6) 0.122(6) 0.060(4) -0.024(4) 0.005(4) -0.044(5) C5 0.111(5) 0.076(4) 0.078(5) -0.026(4) 0.032(4) -0.020(4) C6 0.071(3) 0.058(3) 0.069(4) -0.004(3) 0.022(3) -0.010(3) C7 0.044(2) 0.073(3) 0.055(3) -0.010(2) 0.006(2) -0.001(2) C8 0.060(3) 0.081(4) 0.068(3) -0.005(3) 0.020(3) -0.012(3) C9 0.083(4) 0.112(5) 0.107(5) -0.019(4) 0.049(4) -0.035(4) C10 0.069(4) 0.166(8) 0.173(9) -0.062(7) 0.040(5) -0.053(5) C11 0.078(5) 0.300(14) 0.123(7) -0.082(8) 0.019(4) -0.081(6) C12 0.064(4) 0.214(9) 0.080(4) -0.047(5) 0.011(3) -0.033(5) C13 0.051(2) 0.062(3) 0.046(3) -0.004(2) 0.013(2) -0.011(2) N14 0.043(2) 0.047(2) 0.055(2) 0.010(2) 0.014(2) -0.002(2) C15 0.046(2) 0.046(3) 0.037(2) -0.002(2) 0.010(2) -0.010(2) N16 0.041(2) 0.051(2) 0.055(2) 0.004(2) 0.014(2) -0.006(2) C17 0.046(2) 0.056(3) 0.053(3) 0.004(2) 0.008(2) -0.005(2) C18 0.049(2) 0.049(3) 0.044(3) -0.002(2) 0.001(2) -0.001(2) Cl18 0.0558(8) 0.0687(9) 0.0856(10) 0.0112(7) -0.0012(6) 0.0080(6) C19 0.057(3) 0.047(3) 0.063(3) 0.010(2) 0.004(2) -0.008(2) C20 0.045(2) 0.053(3) 0.054(3) 0.004(2) 0.009(2) -0.012(2) _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 P1 C1 1.826(4) . ? P1 C13 1.840(5) . ? P1 C7 1.837(4) . ? C1 C2 1.39 . ? C1 C6 1.383(7) . ? C2 C3 1.381(7) . ? C3 C4 1.348(10) . ? C4 C5 1.366(9) . ? C5 C6 1.377(8) . ? C7 C8 1.39 . ? C7 C12 1.363(7) . ? C8 C9 1.394(7) . ? C9 C10 1.330(10) . ? C10 C11 1.340(11) . ? C11 C12 1.395(9) . ? C13 N14 1.462(5) . ? N14 C15 1.363(5) . ? C15 N16 1.357(5) . ? C15 C20 1.387(6) . ? N16 C17 1.342(6) . ? C17 C18 1.378(6) . ? C18 C19 1.366(6) . ? C18 Cl18 1.740(4) . ? C19 C20 1.367(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 C1 P1 C13 102.1(2) . . ? C1 P1 C7 102.1(2) . . ? C13 P1 C7 97.6(2) . . ? C2 C1 C6 117.4(5) . . ? C2 C1 P1 124.3(4) . . ? C6 C1 P1 118.1(3) . . ? C1 C2 C3 120.6(5) . . ? C4 C3 C2 120.2(6) . . ? C3 C4 C5 120.8(6) . . ? C4 C5 C6 119.3(6) . . ? C5 C6 C1 121.5(5) . . ? C8 C7 C12 117.8(5) . . ? C8 C7 P1 123.9(4) . . ? C12 C7 P1 118.3(4) . . ? C9 C8 C7 119.9(5) . . ? C10 C9 C8 120.5(6) . . ? C9 C10 C11 121.0(6) . . ? C12 C11 C10 119.8(7) . . ? C11 C12 C7 120.9(6) . . ? N14 C13 P1 111.6(3) . . ? C15 N14 C13 121.7(4) . . ? N16 C15 N14 115.0(4) . . ? N16 C15 C20 121.3(4) . . ? N14 C15 C20 123.6(4) . . ? C17 N16 C15 117.0(4) . . ? N16 C17 C18 124.2(4) . . ? C19 C18 C17 117.8(4) . . ? C19 C18 Cl18 121.3(4) . . ? C17 C18 Cl18 120.9(3) . . ? C18 C19 C20 119.8(4) . . ? C19 C20 C15 119.8(4) . . ? 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 C13 P1 C1 C2 6.3(4) . . . . ? C7 P1 C1 C2 107.0(4) . . . . ? C13 P1 C1 C6 -177.0(3) . . . . ? C7 P1 C1 C6 -76.4(4) . . . . ? C6 C1 C2 C3 1.5(7) . . . . ? P1 C1 C2 C3 178.2(4) . . . . ? C1 C2 C3 C4 0.6(9) . . . . ? C2 C3 C4 C5 -1.3(10) . . . . ? C3 C4 C5 C6 -0.1(10) . . . . ? C4 C5 C6 C1 2.3(8) . . . . ? C2 C1 C6 C5 -3.0(7) . . . . ? P1 C1 C6 C5 -179.9(4) . . . . ? C1 P1 C7 C8 -2.3(5) . . . . ? C13 P1 C7 C8 101.9(5) . . . . ? C1 P1 C7 C12 176.7(6) . . . . ? C13 P1 C7 C12 -79.1(6) . . . . ? C12 C7 C8 C9 -0.5(9) . . . . ? P1 C7 C8 C9 178.5(5) . . . . ? C7 C8 C9 C10 -0.2(11) . . . . ? C8 C9 C10 C11 2.7(15) . . . . ? C9 C10 C11 C12 -4.3(17) . . . . ? C10 C11 C12 C7 3.6(16) . . . . ? C8 C7 C12 C11 -1.2(12) . . . . ? P1 C7 C12 C11 179.8(8) . . . . ? C1 P1 C13 N14 -78.6(3) . . . . ? C7 P1 C13 N14 177.2(3) . . . . ? P1 C13 N14 C15 159.7(3) . . . . ? C13 N14 C15 N16 178.1(4) . . . . ? C13 N14 C15 C20 -2.4(6) . . . . ? N14 C15 N16 C17 177.5(4) . . . . ? C20 C15 N16 C17 -2.0(6) . . . . ? C15 N16 C17 C18 0.9(6) . . . . ? N16 C17 C18 C19 0.8(7) . . . . ? N16 C17 C18 Cl18 179.6(3) . . . . ? C17 C18 C19 C20 -1.6(7) . . . . ? Cl18 C18 C19 C20 179.7(3) . . . . ? C18 C19 C20 C15 0.6(7) . . . . ? N16 C15 C20 C19 1.2(7) . . . . ? N14 C15 C20 C19 -178.2(4) . . . . ? _refine_diff_density_max 0.484 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.136 #---end data_6 #------------------------------------------------------------------------------ _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.849(3) _cell_length_b 11.647(3) _cell_length_c 9.054(2) _cell_angle_alpha 109.31(2) _cell_angle_beta 95.75(3) _cell_angle_gamma 102.41(3) _cell_volume 940.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.5 _cell_measurement_theta_max 13.7 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 559.18 _chemical_formula_analytical 'C18 H16 Au Cl2 N2 P ' _chemical_formula_sum 'C18 H16 Au Cl2 N2 P ' _chemical_formula_moiety 'C18 H16 Au Cl2 N2 P ' _chemical_formula_structural 'C18 H16 Au Cl2 N2 P ' _chemical_compound_source - _exptl_crystal_F_000 532.00 _exptl_absorpt_coefficient_mu 8.168 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.476 _exptl_special_details ; The scan width was (1.00+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 12). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.35 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -1 1 -3 -1 0 -3 0 -1 _diffrn_reflns_number 3514 _reflns_number_total 3306 _reflns_number_gt 2436 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.02916 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06904 _diffrn_orient_matrix_UB_12 -0.02833 _diffrn_orient_matrix_UB_13 -0.10197 _diffrn_orient_matrix_UB_21 -0.00200 _diffrn_orient_matrix_UB_22 -0.08976 _diffrn_orient_matrix_UB_23 -0.01730 _diffrn_orient_matrix_UB_31 -0.08015 _diffrn_orient_matrix_UB_32 -0.00626 _diffrn_orient_matrix_UB_33 0.05906 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 36 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 32 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Au 0 2 -2.688 8.798 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Au(1) 0.05990(3) 0.29706(3) 0.48272(3) 0.04357(8) 1.000 . Uani d ? Cl(1) 0.0476(2) 0.3338(2) 0.2486(2) 0.0594(6) 1.000 . Uani d ? Cl(18) 0.5902(2) 0.7810(3) 0.5838(3) 0.098(1) 1.000 . Uani d ? P(1) 0.0586(2) 0.2717(2) 0.7163(2) 0.0404(5) 1.000 . Uani d ? N(14) 0.3038(5) 0.4527(5) 0.8849(6) 0.044(2) 1.000 . Uani d ? N(16) 0.5049(5) 0.5649(5) 0.8381(7) 0.047(2) 1.000 . Uani d ? C(1) 0.1365(6) 0.1505(6) 0.7438(8) 0.042(2) 1.000 . Uani d ? C(2) 0.1856(7) 0.0745(7) 0.6209(8) 0.045(2) 1.000 . Uani d ? C(3) 0.2489(8) -0.0147(7) 0.6445(9) 0.058(2) 1.000 . Uani d ? C(4) 0.2626(9) -0.0282(8) 0.790(1) 0.070(3) 1.000 . Uani d ? C(5) 0.2131(9) 0.0471(9) 0.913(1) 0.073(3) 1.000 . Uani d ? C(6) 0.1504(8) 0.1365(8) 0.8911(8) 0.061(3) 1.000 . Uani d ? C(7) -0.1182(6) 0.2461(6) 0.7584(7) 0.038(2) 1.000 . Uani d ? C(8) -0.1848(7) 0.1455(7) 0.8003(8) 0.053(2) 1.000 . Uani d ? C(9) -0.3214(8) 0.1312(8) 0.826(1) 0.068(3) 1.000 . Uani d ? C(10) -0.3941(8) 0.2181(9) 0.8142(9) 0.065(3) 1.000 . Uani d ? C(11) -0.3300(8) 0.3165(8) 0.7734(9) 0.060(3) 1.000 . Uani d ? C(12) -0.1939(7) 0.3311(7) 0.7451(8) 0.049(2) 1.000 . Uani d ? C(13) 0.1561(7) 0.4167(6) 0.8873(7) 0.043(2) 1.000 . Uani d ? C(15) 0.3631(6) 0.5323(6) 0.8131(7) 0.039(2) 1.000 . Uani d ? C(17) 0.5689(7) 0.6385(7) 0.7660(9) 0.057(3) 1.000 . Uani d ? C(18) 0.4978(7) 0.6852(7) 0.6718(9) 0.056(2) 1.000 . Uani d ? C(19) 0.3520(7) 0.6543(7) 0.6482(8) 0.051(2) 1.000 . Uani d ? C(20) 0.2829(6) 0.5768(6) 0.7184(8) 0.043(2) 1.000 . Uani d ? H(2) 0.1762 0.0832 0.5201 0.055 1.000 . Uiso c ? H(3) 0.2830 -0.0671 0.5597 0.070 1.000 . Uiso c ? H(4) 0.3064 -0.0898 0.8058 0.084 1.000 . Uiso c ? H(5) 0.2222 0.0370 1.0129 0.088 1.000 . Uiso c ? H(6) 0.1166 0.1881 0.9763 0.074 1.000 . Uiso c ? H(8) -0.1350 0.0864 0.8109 0.063 1.000 . Uiso c ? H(9) -0.3662 0.0611 0.8513 0.082 1.000 . Uiso c ? H(10) -0.4878 0.2091 0.8343 0.078 1.000 . Uiso c ? H(11) -0.3802 0.3757 0.7645 0.073 1.000 . Uiso c ? H(12) -0.1514 0.3997 0.7157 0.058 1.000 . Uiso c ? H(13a) 0.1179 0.4841 0.8835 0.052 1.000 . Uiso c ? H(13b) 0.1442 0.4027 0.9832 0.052 1.000 . Uiso c ? H(14n) 0.3744 0.4468 0.9600 0.073 1.000 . Uiso c ? H(17) 0.6693 0.6597 0.7804 0.069 1.000 . Uiso c ? H(19) 0.2997 0.6865 0.5843 0.062 1.000 . Uiso c ? H(20) 0.1826 0.5542 0.7033 0.052 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au(1) 0.0474(2) 0.0525(2) 0.0376(2) 0.0137(1) 0.0102(1) 0.0238(1) Cl(1) 0.065(1) 0.087(2) 0.048(1) 0.032(1) 0.0202(9) 0.042(1) Cl(18) 0.076(2) 0.119(2) 0.116(2) -0.008(1) 0.007(1) 0.088(2) P(1) 0.044(1) 0.046(1) 0.0359(9) 0.0112(9) 0.0077(8) 0.0211(9) N(14) 0.035(3) 0.054(4) 0.050(3) 0.010(3) 0.002(3) 0.029(3) N(16) 0.037(3) 0.054(4) 0.062(4) 0.014(3) 0.009(3) 0.034(3) C(1) 0.041(4) 0.046(4) 0.045(4) 0.010(3) 0.010(3) 0.022(3) C(2) 0.050(4) 0.041(4) 0.040(4) 0.006(3) 0.005(3) 0.016(3) C(3) 0.058(5) 0.049(5) 0.059(5) 0.014(4) 0.006(4) 0.010(4) C(4) 0.084(6) 0.058(6) 0.077(6) 0.036(5) 0.006(5) 0.027(5) C(5) 0.103(7) 0.078(7) 0.060(5) 0.046(6) 0.020(5) 0.036(5) C(6) 0.079(6) 0.074(6) 0.048(5) 0.036(5) 0.021(4) 0.032(4) C(7) 0.042(4) 0.038(4) 0.032(3) 0.008(3) 0.002(3) 0.013(3) C(8) 0.054(4) 0.057(5) 0.061(5) 0.017(4) 0.017(4) 0.036(4) C(9) 0.055(5) 0.080(7) 0.083(6) 0.008(5) 0.017(4) 0.052(5) C(10) 0.045(4) 0.087(7) 0.062(5) 0.010(5) 0.014(4) 0.028(5) C(11) 0.053(5) 0.060(6) 0.063(5) 0.024(4) 0.003(4) 0.013(4) C(12) 0.053(4) 0.042(5) 0.051(4) 0.010(4) 0.006(3) 0.019(4) C(13) 0.042(4) 0.046(5) 0.042(4) 0.007(3) 0.008(3) 0.018(3) C(15) 0.036(4) 0.043(4) 0.041(4) 0.013(3) 0.006(3) 0.016(3) C(17) 0.037(4) 0.072(6) 0.070(5) 0.010(4) 0.006(4) 0.040(5) C(18) 0.048(4) 0.061(5) 0.064(5) 0.002(4) 0.010(4) 0.039(4) C(19) 0.057(5) 0.052(5) 0.051(4) 0.019(4) 0.002(4) 0.027(4) C(20) 0.039(4) 0.045(5) 0.052(4) 0.014(3) 0.002(3) 0.024(4) #------------------------------------------------------------------------------ _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000058(4) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2436 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_all 0.0245 _refine_ls_wR_factor_ref 0.0245 _refine_ls_goodness_of_fit_all 1.349 _refine_ls_goodness_of_fit_ref 1.349 _refine_ls_shift/esd_max 0.0046 _refine_ls_shift/esd_mean 0.0572 _refine_diff_density_min -0.80 _refine_diff_density_max 1.39 #------------------------------------------------------------------------------ _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au(1) Cl(1) 2.294(2) . . yes Au(1) P(1) 2.231(2) . . yes Cl(18) C(18) 1.734(7) . . yes P(1) C(1) 1.817(7) . . yes P(1) C(7) 1.803(6) . . yes P(1) C(13) 1.857(7) . . yes N(14) C(13) 1.429(7) . . yes N(14) C(15) 1.366(7) . . yes N(14) H(14n) 0.95 . . no N(16) C(15) 1.340(7) . . yes N(16) C(17) 1.333(8) . . yes C(1) C(2) 1.377(9) . . yes C(1) C(6) 1.393(8) . . yes C(2) C(3) 1.383(9) . . yes C(2) H(2) 0.95 . . no C(3) C(4) 1.38(1) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.37(1) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.375(9) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.400(9) . . yes C(7) C(12) 1.390(8) . . yes C(8) C(9) 1.372(9) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.38(1) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.37(1) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.375(9) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) H(13a) 0.95 . . no C(13) H(13b) 0.95 . . no C(15) C(20) 1.401(7) . . yes C(17) C(18) 1.365(8) . . yes C(17) H(17) 0.95 . . no C(18) C(19) 1.379(9) . . yes C(19) C(20) 1.373(9) . . yes C(19) H(19) 0.95 . . no C(20) H(20) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Au(1) P(1) 174.96(7) . . . yes Au(1) P(1) C(1) 116.8(2) . . . yes Au(1) P(1) C(7) 110.7(2) . . . yes Au(1) P(1) C(13) 112.7(2) . . . yes C(1) P(1) C(7) 109.3(3) . . . yes C(1) P(1) C(13) 103.9(3) . . . yes C(7) P(1) C(13) 102.4(3) . . . yes C(13) N(14) C(15) 124.4(5) . . . yes C(13) N(14) H(14n) 122.6 . . . no C(15) N(14) H(14n) 110.1 . . . no C(15) N(16) C(17) 118.2(5) . . . yes P(1) C(1) C(2) 120.3(5) . . . yes P(1) C(1) C(6) 120.0(6) . . . yes C(2) C(1) C(6) 119.6(6) . . . yes C(1) C(2) C(3) 119.9(6) . . . yes C(1) C(2) H(2) 120.2 . . . no C(3) C(2) H(2) 119.9 . . . no C(2) C(3) C(4) 120.3(7) . . . yes C(2) C(3) H(3) 119.9 . . . no C(4) C(3) H(3) 119.8 . . . no C(3) C(4) C(5) 119.9(7) . . . yes C(3) C(4) H(4) 119.8 . . . no C(5) C(4) H(4) 120.3 . . . no C(4) C(5) C(6) 120.5(7) . . . yes C(4) C(5) H(5) 119.5 . . . no C(6) C(5) H(5) 120.0 . . . no C(1) C(6) C(5) 119.8(7) . . . yes C(1) C(6) H(6) 120.3 . . . no C(5) C(6) H(6) 119.9 . . . no P(1) C(7) C(8) 124.6(5) . . . yes P(1) C(7) C(12) 117.4(5) . . . yes C(8) C(7) C(12) 118.0(6) . . . yes C(7) C(8) C(9) 120.7(7) . . . yes C(7) C(8) H(8) 119.6 . . . no C(9) C(8) H(8) 119.7 . . . no C(8) C(9) C(10) 120.2(7) . . . yes C(8) C(9) H(9) 119.8 . . . no C(10) C(9) H(9) 119.9 . . . no C(9) C(10) C(11) 119.5(7) . . . yes C(9) C(10) H(10) 120.1 . . . no C(11) C(10) H(10) 120.3 . . . no C(10) C(11) C(12) 121.0(7) . . . yes C(10) C(11) H(11) 119.5 . . . no C(12) C(11) H(11) 119.6 . . . no C(7) C(12) C(11) 120.5(7) . . . yes C(7) C(12) H(12) 119.7 . . . no C(11) C(12) H(12) 119.8 . . . no P(1) C(13) N(14) 112.8(5) . . . yes P(1) C(13) H(13a) 108.7 . . . no P(1) C(13) H(13b) 108.7 . . . no N(14) C(13) H(13a) 107.8 . . . no N(14) C(13) H(13b) 109.1 . . . no H(13a) C(13) H(13b) 109.7 . . . no N(14) C(15) N(16) 115.4(5) . . . yes N(14) C(15) C(20) 123.0(6) . . . yes N(16) C(15) C(20) 121.6(6) . . . yes N(16) C(17) C(18) 123.4(6) . . . yes N(16) C(17) H(17) 118.6 . . . no C(18) C(17) H(17) 118.0 . . . no Cl(18) C(18) C(17) 120.1(5) . . . yes Cl(18) C(18) C(19) 121.1(5) . . . yes C(17) C(18) C(19) 118.8(6) . . . yes C(18) C(19) C(20) 119.2(6) . . . yes C(18) C(19) H(19) 120.6 . . . no C(20) C(19) H(19) 120.3 . . . no C(15) C(20) C(19) 118.8(6) . . . yes C(15) C(20) H(20) 120.7 . . . no C(19) C(20) H(20) 120.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(18) C(2) 3.525(7) . 2_666 no N(14) N(16) 3.073(7) . 2_667 no N(14) C(11) 3.303(9) . 2_567 no N(16) C(11) 3.529(9) . 1_655 no C(10) C(15) 3.59(1) . 2_567 no C(11) C(13) 3.52(1) . 2_567 no C(12) C(13) 3.56(1) . 2_567 no #---end data_5 #------------------------------------------------------------------------------ _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution 'teXsan (MSC, 1992-1997)' _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 11.944(3) _cell_length_b 14.623(2) _cell_length_c 16.140(2) _cell_angle_alpha 90 _cell_angle_beta 91.36(2) _cell_angle_gamma 90 _cell_volume 2818.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 6.7 _cell_measurement_theta_max 8.3 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourlessprism' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 638.85 _chemical_formula_analytical 'C30 H28 Cl2 N3 P Pd ' _chemical_formula_sum 'C30 H28 Cl2 N3 P Pd ' _chemical_formula_moiety 'C30 H28 Cl2 N3 P Pd ' _chemical_formula_structural 'C30 H28 Cl2 N3 P Pd ' _chemical_compound_source 'C30 H28 Cl2 N3 P Pd ' _exptl_crystal_F_000 1296.00 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.559 _exptl_special_details ; The scan width was (0.89+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 12). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.52 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 6 -4 2 2 2 4 3 _diffrn_reflns_number 5437 _reflns_number_total 5175 _reflns_number_gt 2869 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04939 _diffrn_reflns_av_sigmaI/netI 0.100 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05330 _diffrn_orient_matrix_UB_12 0.05196 _diffrn_orient_matrix_UB_13 0.00727 _diffrn_orient_matrix_UB_21 -0.04496 _diffrn_orient_matrix_UB_22 -0.03828 _diffrn_orient_matrix_UB_23 0.03832 _diffrn_orient_matrix_UB_31 0.04638 _diffrn_orient_matrix_UB_32 0.02261 _diffrn_orient_matrix_UB_33 0.04816 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 120 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 112 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 12 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 4 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd(1) 0.18577(3) 0.70875(3) 0.65076(2) 0.0306(1) 1.000 . Uani d ? Cl(1) 0.1055(1) 0.7770(1) 0.52741(9) 0.0499(4) 1.000 . Uani d ? Cl(18) 0.2450(2) 1.3572(1) 0.6481(1) 0.0669(6) 1.000 . Uani d ? P(1) 0.3222(1) 0.81474(9) 0.65913(8) 0.0307(4) 1.000 . Uani d ? N(14) 0.2154(3) 0.9645(3) 0.5872(3) 0.046(1) 1.000 . Uani d ? N(16) 0.3194(4) 1.0940(3) 0.6204(3) 0.044(1) 1.000 . Uani d ? N(28) 0.0492(3) 0.6130(3) 0.6568(3) 0.036(1) 1.000 . Uani d ?C(1) 0.3337(4) 0.8737(4) 0.7581(3) 0.037(1) 1.000 . Uani d ? C(2) 0.2652(4) 0.8502(4) 0.8227(3) 0.038(2) 1.000 . Uani d ? C(3) 0.2731(5) 0.8960(4) 0.8976(4) 0.051(2) 1.000 . Uani d ? C(4) 0.3482(6) 0.9663(4) 0.9084(4) 0.062(2) 1.000 . Uani d ? C(5) 0.4158(6) 0.9916(5) 0.8462(4) 0.063(2) 1.000 . Uani d ? C(6) 0.4085(5) 0.9463(4) 0.7693(4) 0.047(2) 1.000 . Uani d ? C(7) 0.4585(4) 0.7710(3) 0.6298(3) 0.032(1) 1.000 . Uani d ? C(8) 0.4616(4) 0.7236(4) 0.5558(3) 0.042(2) 1.000 . Uani d ? C(9) 0.5617(5) 0.6943(4) 0.5254(4) 0.054(2) 1.000 . Uani d ? C(10) 0.6598(5) 0.7105(4) 0.5690(4) 0.053(2) 1.000 . Uani d ? C(11) 0.6588(4) 0.7559(4) 0.6429(4) 0.048(2) 1.000 . Uani d ? C(12) 0.5579(4) 0.7867(4) 0.6739(3) 0.041(2) 1.000 . Uani d ? C(13) 0.3130(4) 0.9084(4) 0.5814(3) 0.038(2) 1.000 . Uani d ? C(15) 0.2200(4) 1.0568(4) 0.5996(3) 0.040(2) 1.000 . Uani d ? C(17) 0.3242(5) 1.1840(4) 0.6344(4) 0.048(2) 1.000 . Uani d ? C(18) 0.2321(5) 1.2405(4) 0.6291(4) 0.047(2) 1.000 . Uani d ? C(19) 0.1290(5) 1.2030(4) 0.6072(3) 0.047(2) 1.000 . Uani d ? C(20) 0.1235(4) 1.1104(4) 0.5926(4) 0.047(2) 1.000 . Uani d ? C(21) 0.2491(4) 0.6338(3) 0.7450(3) 0.031(1) 1.000 . Uani d ? C(21) 0.1749(4) 0.5630(3) 0.7692(3) 0.030(1) 1.000 . Uani d ? C(22) 0.3513(4) 0.6385(4) 0.7855(3) 0.038(1) 1.000 . Uani d ? C(23) 0.3792(4) 0.5775(4) 0.8512(3) 0.043(2) 1.000 . Uani d ? C(24) 0.3076(5) 0.5113(4) 0.8760(3) 0.042(2) 1.000 . Uani d ? C(24) 0.2023(5) 0.5026(4) 0.8353(3) 0.040(2) 1.000 . Uani d ? C(25) 0.1245(5) 0.4330(4) 0.8567(4) 0.052(2) 1.000 . Uani d ? C(26) 0.0261(5) 0.4228(4) 0.8120(5) 0.059(2) 1.000 . Uani d ? C(27) -0.0009(5) 0.4826(4) 0.7471(4) 0.049(2) 1.000 . Uani d ? C(28) 0.0711(4) 0.5497(4) 0.7254(3) 0.035(1) 1.000 . Uani d ? C(29) -0.0555(5) 0.6647(5) 0.6713(4) 0.059(2) 1.000 . Uani d ? C(30) 0.0361(5) 0.5605(5) 0.5779(4) 0.063(2) 1.000 . Uani d ? H(2) 0.2122 0.8022 0.8155 0.046 1.000 . Uiso c ? H(3) 0.2263 0.8786 0.9418 0.061 1.000 . Uiso c ? H(4) 0.3525 0.9977 0.9600 0.074 1.000 . Uiso c ? H(5) 0.4685 1.0397 0.8546 0.075 1.000 . Uiso c ? H(6) 0.4543 0.9651 0.7250 0.057 1.000 . Uiso c ? H(8) 0.3939 0.7112 0.5257 0.051 1.000 . Uiso c ? H(9) 0.5632 0.6626 0.4740 0.064 1.000 . Uiso c ? H(10) 0.7289 0.6900 0.5476 0.063 1.000 . Uiso c ? H(11) 0.7270 0.7663 0.6730 0.058 1.000 . Uiso c ? H(12) 0.5571 0.8186 0.7253 0.050 1.000 . Uiso c ? H(13) 0.3771 0.9462 0.5886 0.046 1.000 . Uiso c ?H(13) 0.3130 0.8816 0.5277 0.046 1.000 . Uiso c ? H(14) 0.1428 0.9468 0.5668 0.060 1.000 . Uiso c ? H(17) 0.3948 1.2104 0.6488 0.057 1.000 . Uiso c ? H(19) 0.0639 1.2402 0.6024 0.056 1.000 . Uiso c ? H(20) 0.0538 1.0828 0.5777 0.056 1.000 . Uiso c ? H(22) 0.4041 0.6833 0.7693 0.045 1.000 . Uiso c ? H(23) 0.4501 0.5831 0.8787 0.052 1.000 . Uiso c ? H(24) 0.3281 0.4714 0.9202 0.050 1.000 . Uiso c ? H(25) 0.1408 0.3934 0.9021 0.062 1.000 . Uiso c ? H(26) -0.0240 0.3748 0.8252 0.071 1.000 . Uiso c ? H(27) -0.0706 0.4762 0.7178 0.059 1.000 . Uiso c ? H(29) -0.0416 0.7101 0.7122 0.071 1.000 . Uiso c ? H(29) -0.0800 0.6928 0.6210 0.071 1.000 . Uiso c ? H(29) -0.1115 0.6238 0.6897 0.071 1.000 . Uiso c ? H(30) -0.0202 0.5153 0.5839 0.076 1.000 . Uiso c ? H(30) 0.0151 0.6011 0.5343 0.076 1.000 . Uiso c ? H(30) 0.1051 0.5319 0.5656 0.076 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd(1) 0.0261(2) 0.0317(2) 0.0338(2) 0.0007(2) -0.0020(1) -0.0012(2) Cl(1) 0.0540(8) 0.0495(9) 0.0453(8) 0.0043(7) -0.0163(7) -0.0001(7) Cl(18) 0.082(1) 0.0436(9) 0.075(1) 0.0162(9) 0.0029(9) -0.0094(9) P(1) 0.0294(7) 0.0311(8) 0.0316(7) -0.0000(5) 0.0004(5) 0.0033(6) N(14) 0.036(2) 0.037(3) 0.066(3) 0.002(2) -0.002(2) 0.010(2) N(16) 0.038(3) 0.035(3) 0.059(3) 0.005(2) -0.004(2) 0.004(2) N(28) 0.025(2) 0.046(3) 0.038(3) -0.005(2) -0.004(2) -0.009(2) C(1) 0.034(3) 0.032(3) 0.046(3) 0.004(2) -0.002(2) -0.003(3) C(2) 0.039(3) 0.031(3) 0.045(3) 0.004(2) 0.005(3) 0.002(2) C(3) 0.063(4) 0.051(4) 0.039(3) 0.007(3) 0.013(3) 0.005(3) C(4) 0.096(5) 0.047(4) 0.042(4) -0.001(4) 0.002(4) -0.008(3) C(5) 0.076(5) 0.054(4) 0.059(4) -0.015(4) -0.006(4) -0.016(3) C(6) 0.057(4) 0.043(3) 0.043(3) -0.014(3) 0.009(3) -0.001(3) C(7) 0.031(3) 0.027(3) 0.039(3) 0.002(2) 0.002(2) 0.005(2) C(8) 0.039(3) 0.043(4) 0.045(3) 0.002(3) -0.003(2) -0.009(3) C(9) 0.053(4) 0.061(4) 0.047(4) 0.009(3) 0.011(3) 0.002(3) C(10) 0.041(3) 0.051(4) 0.068(4) 0.012(3) 0.017(3) 0.014(4) C(11) 0.030(3) 0.057(4) 0.058(4) 0.002(3) -0.007(3) 0.003(3) C(12) 0.037(3) 0.043(3) 0.045(3) 0.001(3) 0.004(2) 0.003(3) C(13) 0.038(3) 0.036(3) 0.041(3) 0.001(2) 0.002(2) 0.010(2) C(15) 0.038(3) 0.042(4) 0.040(3) 0.009(3) 0.002(3) 0.014(3) C(17) 0.042(3) 0.044(4) 0.057(4) 0.004(3) -0.009(3) 0.002(3) C(18) 0.054(4) 0.044(4) 0.044(3) 0.016(3) 0.002(3) 0.006(3) C(19) 0.044(3) 0.049(4) 0.047(3) 0.018(3) 0.005(3) 0.012(3) C(20) 0.035(3) 0.051(4) 0.054(4) 0.007(3) -0.002(3) 0.007(3) C(21) 0.039(3) 0.029(3) 0.026(3) 0.002(2) 0.002(2) 0.003(2) C(21) 0.032(3) 0.027(3) 0.031(3) 0.000(2) 0.008(2) -0.003(2) C(22) 0.032(3) 0.040(3) 0.040(3) 0.001(2) -0.002(2) 0.003(3) C(23) 0.041(3) 0.045(3) 0.043(3) 0.005(3) -0.008(3) -0.000(3) C(24) 0.052(4) 0.036(3) 0.039(3) 0.008(3) 0.002(3) 0.009(3) C(24) 0.047(3) 0.030(3) 0.044(3) 0.003(2) 0.013(3) -0.006(3) C(25) 0.063(4) 0.041(4) 0.053(4) 0.002(3) 0.026(3) 0.005(3) C(26) 0.053(4) 0.040(4) 0.086(5) -0.011(3) 0.023(4) -0.009(4) C(27) 0.034(3) 0.043(4) 0.071(4) -0.008(3) 0.007(3) -0.004(3) C(28) 0.031(3) 0.034(3) 0.041(3) -0.000(2) 0.005(2) -0.006(2) C(29) 0.028(3) 0.072(5) 0.078(5) 0.004(3) 0.008(3) 0.009(4) C(30) 0.078(5) 0.057(4) 0.055(4) -0.023(4) -0.004(3) -0.016(3) #------------------------------------------------------------------------------ _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00029|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2869 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_all 0.0481 _refine_ls_wR_factor_ref 0.0481 _refine_ls_goodness_of_fit_all 1.438 _refine_ls_goodness_of_fit_ref 1.438 _refine_ls_shift/esd_max 1.3150 _refine_ls_shift/esd_mean 0.0300 _refine_diff_density_min -0.48 _refine_diff_density_max 0.55 #------------------------------------------------------------------------------ _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd(1) Cl(1) 2.406(2) . . yes Pd(1) P(1) 2.250(2) . . yes Pd(1) N(28) 2.153(5) . . yes Pd(1) C(21) 2.009(6) . . yes Cl(18) C(18) 1.740(7) . . yes P(1) C(1) 1.817(6) . . yes P(1) C(7) 1.822(6) . . yes P(1) C(13) 1.859(6) . . yes N(14) C(13) 1.431(8) . . yes N(14) C(15) 1.366(8) . . yes N(14) H(14n) 0.955(5) . . yes N(16) C(15) 1.342(8) . . yes N(16) C(17) 1.336(8) . . yes N(28) C(28) 1.461(8) . . yes N(28) C(29) 1.484(8) . . yes N(28) C(30) 1.492(8) . . yes C(1) C(2) 1.384(9) . . yes C(1) C(6) 1.396(9) . . yes C(2) C(3) 1.382(9) . . yes C(2) H(2) 0.95 . . no C(3) C(4) 1.37(1) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.36(1) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.408(9) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.383(8) . . yes C(7) C(12) 1.389(8) . . yes C(8) C(9) 1.372(9) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.37(1) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.36(1) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.391(9) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) H(13a) 0.949(6) . . yes C(13) H(13b) 0.951(6) . . yes C(15) C(20) 1.396(8) . . yes C(17) C(18) 1.377(9) . . yes C(17) H(17) 0.95 . . no C(18) C(19) 1.39(1) . . yes C(19) C(20) 1.38(1) . . yes C(19) H(19) 0.95 . . no C(20) H(20) 0.95 . . no C(21) C(21a) 1.423(8) . . yes C(21) C(22) 1.372(8) . . yes C(21a) C(24a) 1.417(8) . . yes C(21a) C(28) 1.427(7) . . yes C(22) C(23) 1.420(8) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.358(9) . . yes C(23) H(23) 0.95 . . no C(24) C(24a) 1.411(9) . . yes C(24) H(24) 0.95 . . no C(24a) C(25) 1.426(9) . . yes C(25) C(26) 1.37(1) . . yes C(25) H(25) 0.95 . . no C(26) C(27) 1.40(1) . . yes C(26) H(26) 0.95 . . no C(27) C(28) 1.356(9) . . yes C(27) H(27) 0.95 . . no C(29) H(29a) 0.949(9) . . yes C(29) H(29b) 0.950(8) . . yes C(29) H(29c) 0.950(7) . . yes C(30) H(30a) 0.949(7) . . yes C(30) H(30b) 0.949(8) . . yes C(30) H(30c) 0.950(8) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Pd(1) P(1) 92.15(6) . . . yes Cl(1) Pd(1) N(28) 91.2(1) . . . yes Cl(1) Pd(1) C(21) 171.4(2) . . . yes P(1) Pd(1) N(28) 173.2(1) . . . yes P(1) Pd(1) C(21) 94.1(2) . . . yes N(28) Pd(1) C(21) 83.3(2) . . . yes Pd(1) P(1) C(1) 114.8(2) . . . yes Pd(1) P(1) C(7) 113.1(2) . . . yes Pd(1) P(1) C(13) 115.8(2) . . . yes C(1) P(1) C(7) 110.2(3) . . . yes C(1) P(1) C(13) 104.2(3) . . . yes C(7) P(1) C(13) 97.0(3) . . . yes C(13) N(14) C(15) 123.1(5) . . . yes C(13) N(14) H(14n) 123.8(6) . . . yes C(15) N(14) H(14n) 110.5(5) . . . yes C(15) N(16) C(17) 118.4(6) . . . yes Pd(1) N(28) C(28) 108.9(3) . . . yes Pd(1) N(28) C(29) 108.5(4) . . . yes Pd(1) N(28) C(30) 111.1(4) . . . yes C(28) N(28) C(29) 109.8(5) . . . yes C(28) N(28) C(30) 109.5(5) . . . yes C(29) N(28) C(30) 108.9(5) . . . yes P(1) C(1) C(2) 120.7(5) . . . yes P(1) C(1) C(6) 120.6(5) . . . yes C(2) C(1) C(6) 118.6(6) . . . yes C(1) C(2) C(3) 120.7(6) . . . yes C(1) C(2) H(2) 119.7 . . . no C(3) C(2) H(2) 119.7 . . . no C(2) C(3) C(4) 120.3(7) . . . yes C(2) C(3) H(3) 119.8 . . . no C(4) C(3) H(3) 119.9 . . . no C(3) C(4) C(5) 120.6(7) . . . yes C(3) C(4) H(4) 119.7 . . . no C(5) C(4) H(4) 119.8 . . . no C(4) C(5) C(6) 120.0(7) . . . yes C(4) C(5) H(5) 120.0 . . . no C(6) C(5) H(5) 120.1 . . . no C(1) C(6) C(5) 119.9(7) . . . yes C(1) C(6) H(6) 120.0 . . . no C(5) C(6) H(6) 120.1 . . . no P(1) C(7) C(8) 116.3(5) . . . yes P(1) C(7) C(12) 124.6(5) . . . yes C(8) C(7) C(12) 119.0(6) . . . yes C(7) C(8) C(9) 120.5(6) . . . yes C(7) C(8) H(8) 119.8 . . . no C(9) C(8) H(8) 119.8 . . . no C(8) C(9) C(10) 120.3(7) . . . yes C(8) C(9) H(9) 119.9 . . . no C(10) C(9) H(9) 119.8 . . . no C(9) C(10) C(11) 120.4(6) . . . yes C(9) C(10) H(10) 119.8 . . . no C(11) C(10) H(10) 119.8 . . . no C(10) C(11) C(12) 119.9(6) . . . yes C(10) C(11) H(11) 119.9 . . . no C(12) C(11) H(11) 120.2 . . . no C(7) C(12) C(11) 120.0(6) . . . yes C(7) C(12) H(12) 120.0 . . . no C(11) C(12) H(12) 120.0 . . . no P(1) C(13) N(14) 114.4(4) . . . yes P(1) C(13) H(13a) 108.2(5) . . . yes P(1) C(13) H(13b) 108.1(5) . . . yes N(14) C(13) H(13a) 108.3(6) . . . yes N(14) C(13) H(13b) 108.2(5) . . . yes H(13a) C(13) H(13b) 109.5(6) . . . yes N(14) C(15) N(16) 118.0(5) . . . yes N(14) C(15) C(20) 120.9(6) . . . yes N(16) C(15) C(20) 121.1(6) . . . yes N(16) C(17) C(18) 123.3(7) . . . yes N(16) C(17) H(17) 118.4 . . . no C(18) C(17) H(17) 118.3 . . . no Cl(18) C(18) C(17) 120.7(6) . . . yes Cl(18) C(18) C(19) 120.5(5) . . . yes C(17) C(18) C(19) 118.8(7) . . . yes C(18) C(19) C(20) 118.2(6) . . . yes C(18) C(19) H(19) 120.9 . . . no C(20) C(19) H(19) 120.9 . . . no C(15) C(20) C(19) 120.2(6) . . . yes C(15) C(20) H(20) 119.9 . . . no C(19) C(20) H(20) 119.9 . . . no Pd(1) C(21) C(21a) 112.3(4) . . . yes Pd(1) C(21) C(22) 130.4(5) . . . yes C(21a) C(21) C(22) 117.3(5) . . . yes C(21) C(21a) C(24a) 121.8(5) . . . yes C(21) C(21a) C(28) 120.2(5) . . . yes C(24a) C(21a) C(28) 118.0(5) . . . yes C(21) C(22) C(23) 121.0(6) . . . yes C(21) C(22) H(22) 119.5 . . . no C(23) C(22) H(22) 119.5 . . . no C(22) C(23) C(24) 121.9(6) . . . yes C(22) C(23) H(23) 119.1 . . . no C(24) C(23) H(23) 119.0 . . . no C(23) C(24) C(24a) 119.3(6) . . . yes C(23) C(24) H(24) 120.4 . . . no C(24a) C(24) H(24) 120.3 . . . no C(21a) C(24a) C(24) 118.7(6) . . . yes C(21a) C(24a) C(25) 119.2(6) . . . yes C(24) C(24a) C(25) 122.1(6) . . . yes C(24a) C(25) C(26) 120.3(7) . . . yes C(24a) C(25) H(25) 119.9 . . . no C(26) C(25) H(25) 119.8 . . . no C(25) C(26) C(27) 120.4(7) . . . yes C(25) C(26) H(26) 119.9 . . . no C(27) C(26) H(26) 119.7 . . . no C(26) C(27) C(28) 120.7(6) . . . yes C(26) C(27) H(27) 119.7 . . . no C(28) C(27) H(27) 119.6 . . . no N(28) C(28) C(21a) 115.2(5) . . . yes N(28) C(28) C(27) 123.5(6) . . . yes C(21a) C(28) C(27) 121.3(6) . . . yes N(28) C(29) H(29a) 109.4(6) . . . yes N(28) C(29) H(29b) 109.4(7) . . . yes N(28) C(29) H(29c) 109.4(7) . . . yes H(29a) C(29) H(29b) 109.6(8) . . . yes H(29a) C(29) H(29c) 109.6(8) . . . yes H(29b) C(29) H(29c) 109.5(7) . . . yes N(28) C(30) H(30a) 109.4(7) . . . yes N(28) C(30) H(30b) 109.4(7) . . . yes N(28) C(30) H(30c) 109.3(6) . . . yes H(30a) C(30) H(30b) 109.6(7) . . . yes H(30a) C(30) H(30c) 109.6(8) . . . yes H(30b) C(30) H(30c) 109.5(8) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(19) 3.516(7) . 3_576 no N(14) C(26) 3.400(9) . 2_556 no C(4) C(10) 3.59(1) . 2_656 no C(9) C(17) 3.44(1) . 3_676 no C(10) C(18) 3.55(1) . 3_676 no C(13) C(24) 3.517(9) . 4_564 no C(20) C(27) 3.54(1) . 2_556 no C(30) C(30) 3.18(1) . 3_566 no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(14)' 'H(14n)' 'Cl(1)' '0.96' '2.60' '3.179(6)' '119.4' '.' #---end data_2 _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 9.226(2) _cell_length_b 12.365(6) _cell_length_c 8.559(4) _cell_angle_alpha 98.90(4) _cell_angle_beta 107.85(2) _cell_angle_gamma 106.17(3) _cell_volume 861.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.3 _cell_measurement_theta_max 18.1 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 342.76 _chemical_formula_analytical 'C18 H16 Cl N2 O P ' _chemical_formula_sum 'C18 H16 Cl N2 O P ' _chemical_formula_moiety 'C18 H16 Cl N2 O P ' _chemical_formula_structural 'C18 H16 Cl N2 O P ' _chemical_compound_source - _exptl_crystal_F_000 356.00 _exptl_absorpt_coefficient_mu 0.316 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.959 _exptl_special_details ; The scan width was (1.05+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 12). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; - ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.14 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -4 2 -1 -3 2 1 -3 2 _diffrn_reflns_number 3229 _reflns_number_total 3025 _reflns_number_gt 2160 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01543 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04317 _diffrn_orient_matrix_UB_12 -0.03208 _diffrn_orient_matrix_UB_13 0.08343 _diffrn_orient_matrix_UB_21 -0.10771 _diffrn_orient_matrix_UB_22 0.00558 _diffrn_orient_matrix_UB_23 -0.06199 _diffrn_orient_matrix_UB_31 -0.03566 _diffrn_orient_matrix_UB_32 -0.08096 _diffrn_orient_matrix_UB_33 -0.07333 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 36 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 32 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 2 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 2 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Cl(18) 0.91524(7) 0.06400(5) 1.36221(8) 0.0974(2) 1.00000 . Uani d ? P(1) 0.23159(5) 0.34435(3) 0.99127(5) 0.0395(1) 1.00000 . Uani d ? O(1) 0.2734(1) 0.45739(8) 0.9456(1) 0.0498(3) 1.00000 . Uani d ? N(14) 0.5164(1) 0.3126(1) 1.0287(2) 0.0544(4) 1.00000 . Uani d ? N(16) 0.5403(1) 0.1488(1) 1.1184(2) 0.0519(4) 1.00000 . Uani d ? C(1) 0.0210(2) 0.2560(1) 0.8788(2) 0.0413(4) 1.00000 . Uani d ? C(2) -0.0729(2) 0.2924(2) 0.7534(2) 0.0623(6) 1.00000 . Uani d ? C(3) -0.2358(2) 0.2281(2) 0.6661(3) 0.0815(7) 1.00000 . Uani d ? C(4) -0.3047(2) 0.1271(2) 0.7028(3) 0.0767(7) 1.00000 . Uani d ? C(5) -0.2144(2) 0.0894(2) 0.8262(3) 0.0727(6) 1.00000 . Uani d ? C(6) -0.0502(2) 0.1536(1) 0.9150(2) 0.0599(6) 1.00000 . Uani d ? C(7) 0.2707(2) 0.3636(1) 1.2140(2) 0.0432(4) 1.00000 . Uani d ? C(8) 0.2594(2) 0.4642(1) 1.3003(2) 0.0567(5) 1.00000 . Uani d ? C(9) 0.2837(2) 0.4836(2) 1.4714(3) 0.0746(7) 1.00000 . Uani d ? C(10) 0.3211(2) 0.4049(2) 1.5582(2) 0.0791(7) 1.00000 . Uani d ? C(11) 0.3343(2) 0.3059(2) 1.4754(2) 0.0727(7) 1.00000 . Uani d ? C(12) 0.3093(2) 0.2849(1) 1.3041(2) 0.0575(6) 1.00000 . Uani d ? C(13) 0.3440(2) 0.2552(1) 0.9373(2) 0.0477(5) 1.00000 . Uani d ? C(15) 0.6119(2) 0.2572(1) 1.1124(2) 0.0446(5) 1.00000 . Uani d ? C(17) 0.6364(2) 0.0941(1) 1.1964(2) 0.0571(6) 1.00000 . Uani d ? C(18) 0.8002(2) 0.1435(1) 1.2701(2) 0.0566(6) 1.00000 . Uani d ? C(19) 0.8748(2) 0.2572(1) 1.2688(2) 0.0595(6) 1.00000 . Uani d ? C(20) 0.7805(2) 0.3146(1) 1.1896(2) 0.0534(5) 1.00000 . Uani d ? H(2) -0.025300 0.362400 0.726700 0.07470 1.00000 . Uiso c ? H(3) -0.300000 0.254200 0.580600 0.09770 1.00000 . Uiso c ? H(4) -0.416500 0.082800 0.641800 0.09210 1.00000 . Uiso c ? H(5) -0.263500 0.019200 0.851500 0.08710 1.00000 . Uiso c ? H(6) 0.013100 0.126900 1.000600 0.07180 1.00000 . Uiso c ? H(8) 0.235000 0.520100 1.241300 0.06780 1.00000 . Uiso c ? H(9) 0.274400 0.552000 1.529100 0.08950 1.00000 . Uiso c ? H(10) 0.337800 0.418800 1.675800 0.09470 1.00000 . Uiso c ? H(11) 0.360900 0.251500 1.536100 0.08730 1.00000 . Uiso c ? H(12) 0.318500 0.215900 1.247600 0.06880 1.00000 . Uiso c ? H(13) 0.310100 0.183400 0.965500 0.05710 1.00000 . Uiso c ? H(13) 0.322200 0.240500 0.818700 0.05710 1.00000 . Uiso c ? H(14) 0.564800 0.390400 1.000600 0.08300 1.00000 . Uiso c ? H(17) 0.586900 0.016400 1.200100 0.06860 1.00000 . Uiso c ? H(19) 0.989300 0.294200 1.321800 0.07140 1.00000 . Uiso c ? H(20) 0.828300 0.392800 1.186800 0.06400 1.00000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(18) 0.0790(4) 0.0834(4) 0.1318(5) 0.0439(3) 0.0162(4) 0.0507(4) P(1) 0.0365(2) 0.0359(2) 0.0457(2) 0.0101(2) 0.0158(2) 0.0125(2) O(1) 0.0489(7) 0.0395(6) 0.0636(7) 0.0117(5) 0.0231(6) 0.0220(5) N(14) 0.0398(8) 0.0434(8) 0.088(1) 0.0163(7) 0.0267(8) 0.0300(8) N(16) 0.0436(8) 0.0396(8) 0.072(1) 0.0124(6) 0.0196(7) 0.0201(7) C(1) 0.0365(9) 0.0406(9) 0.0427(9) 0.0106(7) 0.0135(7) 0.0074(7) C(2) 0.048(1) 0.065(1) 0.064(1) 0.0118(9) 0.0099(9) 0.023(1) C(3) 0.051(1) 0.093(2) 0.078(1) 0.015(1) 0.002(1) 0.027(1) C(4) 0.045(1) 0.079(1) 0.074(1) -0.001(1) 0.007(1) 0.000(1) C(5) 0.058(1) 0.052(1) 0.087(2) -0.0019(9) 0.022(1) 0.011(1) C(6) 0.049(1) 0.050(1) 0.070(1) 0.0079(9) 0.0145(9) 0.0193(9) C(7) 0.0331(8) 0.0433(9) 0.0453(9) 0.0049(7) 0.0135(7) 0.0079(7) C(8) 0.054(1) 0.051(1) 0.058(1) 0.0081(9) 0.0239(9) 0.0075(9) C(9) 0.075(1) 0.066(1) 0.066(1) 0.002(1) 0.036(1) -0.008(1) C(10) 0.065(1) 0.106(2) 0.046(1) 0.003(1) 0.021(1) 0.010(1) C(11) 0.058(1) 0.103(2) 0.057(1) 0.023(1) 0.019(1) 0.036(1) C(12) 0.053(1) 0.067(1) 0.053(1) 0.0187(9) 0.0192(9) 0.0206(9) C(13) 0.048(1) 0.0433(9) 0.055(1) 0.0175(8) 0.0219(8) 0.0135(8) C(15) 0.0434(9) 0.0395(9) 0.058(1) 0.0159(7) 0.0260(8) 0.0138(8) C(17) 0.059(1) 0.042(1) 0.073(1) 0.0166(9) 0.024(1) 0.0221(9) C(18) 0.052(1) 0.056(1) 0.068(1) 0.0261(9) 0.0195(9) 0.0248(9) C(19) 0.040(1) 0.057(1) 0.080(1) 0.0156(9) 0.0204(9) 0.018(1) C(20) 0.044(1) 0.0415(9) 0.079(1) 0.0120(8) 0.0286(9) 0.0191(9) #------------------------------------------------------------------------------ _refine_special_details ; - ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 2160 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_all 0.0332 _refine_ls_wR_factor_ref 0.0332 _refine_ls_goodness_of_fit_all 2.399 _refine_ls_goodness_of_fit_ref 2.399 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean 0.0550 _refine_diff_density_min -0.23 _refine_diff_density_max 0.21 #------------------------------------------------------------------------------ _geom_special_details ; - ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(18) C(18) 1.738(2) . . yes P(1) O(1) 1.489(2) . . yes P(1) C(1) 1.800(2) . . yes P(1) C(7) 1.792(2) . . yes P(1) C(13) 1.811(2) . . yes N(14) C(13) 1.443(3) . . yes N(14) C(15) 1.364(3) . . yes N(14) H(14n) 1.040(2) . . yes N(16) C(15) 1.336(3) . . yes N(16) C(17) 1.342(3) . . yes C(1) C(2) 1.379(3) . . yes C(1) C(6) 1.385(3) . . yes C(2) C(3) 1.383(4) . . yes C(2) H(2) 0.95 . . no C(3) C(4) 1.365(4) . . yes C(3) H(3) 0.95 . . no C(4) C(5) 1.362(4) . . yes C(4) H(4) 0.95 . . no C(5) C(6) 1.393(4) . . yes C(5) H(5) 0.95 . . no C(6) H(6) 0.95 . . no C(7) C(8) 1.393(3) . . yes C(7) C(12) 1.388(3) . . yes C(8) C(9) 1.383(4) . . yes C(8) H(8) 0.95 . . no C(9) C(10) 1.367(4) . . yes C(9) H(9) 0.95 . . no C(10) C(11) 1.373(4) . . yes C(10) H(10) 0.95 . . no C(11) C(12) 1.383(4) . . yes C(11) H(11) 0.95 . . no C(12) H(12) 0.95 . . no C(13) H(13a) 0.950(2) . . yes C(13) H(13b) 0.950(2) . . yes C(15) C(20) 1.404(3) . . yes C(17) C(18) 1.355(3) . . yes C(17) H(17) 0.95 . . no C(18) C(19) 1.386(3) . . yes C(19) C(20) 1.361(3) . . yes C(19) H(19) 0.95 . . no C(20) H(20) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) P(1) C(1) 112.0(1) . . . yes O(1) P(1) C(7) 112.4(1) . . . yes O(1) P(1) C(13) 112.6(1) . . . yes C(1) P(1) C(7) 107.3(1) . . . yes C(1) P(1) C(13) 105.3(1) . . . yes C(7) P(1) C(13) 106.8(1) . . . yes C(13) N(14) C(15) 122.2(2) . . . yes C(13) N(14) H(14n) 114.0(2) . . . yes C(15) N(14) H(14n) 122.1(2) . . . yes C(15) N(16) C(17) 117.5(2) . . . yes P(1) C(1) C(2) 118.8(2) . . . yes P(1) C(1) C(6) 122.3(2) . . . yes C(2) C(1) C(6) 118.9(2) . . . yes C(1) C(2) C(3) 120.6(3) . . . yes C(1) C(2) H(2) 119.7 . . . no C(3) C(2) H(2) 119.6 . . . no C(2) C(3) C(4) 120.0(3) . . . yes C(2) C(3) H(3) 120.1 . . . no C(4) C(3) H(3) 119.9 . . . no C(3) C(4) C(5) 120.5(3) . . . yes C(3) C(4) H(4) 119.7 . . . no C(5) C(4) H(4) 119.8 . . . no C(4) C(5) C(6) 120.0(3) . . . yes C(4) C(5) H(5) 120.0 . . . no C(6) C(5) H(5) 120.0 . . . no C(1) C(6) C(5) 120.0(2) . . . yes C(1) C(6) H(6) 120.0 . . . no C(5) C(6) H(6) 120.0 . . . no P(1) C(7) C(8) 117.0(2) . . . yes P(1) C(7) C(12) 124.4(2) . . . yes C(8) C(7) C(12) 118.5(2) . . . yes C(7) C(8) C(9) 120.3(3) . . . yes C(7) C(8) H(8) 119.9 . . . no C(9) C(8) H(8) 119.8 . . . no C(8) C(9) C(10) 120.4(3) . . . yes C(8) C(9) H(9) 119.8 . . . no C(10) C(9) H(9) 119.8 . . . no C(9) C(10) C(11) 120.0(3) . . . yes C(9) C(10) H(10) 120.0 . . . no C(11) C(10) H(10) 120.0 . . . no C(10) C(11) C(12) 120.3(3) . . . yes C(10) C(11) H(11) 119.8 . . . no C(12) C(11) H(11) 119.9 . . . no C(7) C(12) C(11) 120.4(3) . . . yes C(7) C(12) H(12) 119.8 . . . no C(11) C(12) H(12) 119.7 . . . no P(1) C(13) N(14) 111.3(2) . . . yes P(1) C(13) H(13a) 109.0(2) . . . yes P(1) C(13) H(13b) 109.0(2) . . . yes N(14) C(13) H(13a) 109.0(2) . . . yes N(14) C(13) H(13b) 109.0(2) . . . yes H(13a) C(13) H(13b) 109.5(2) . . . yes N(14) C(15) N(16) 118.2(2) . . . yes N(14) C(15) C(20) 119.8(2) . . . yes N(16) C(15) C(20) 122.0(2) . . . yes N(16) C(17) C(18) 123.5(2) . . . yes N(16) C(17) H(17) 118.2 . . . no C(18) C(17) H(17) 118.3 . . . no Cl(18) C(18) C(17) 120.2(2) . . . yes Cl(18) C(18) C(19) 120.5(2) . . . yes C(17) C(18) C(19) 119.3(2) . . . yes C(18) C(19) C(20) 118.5(2) . . . yes C(18) C(19) H(19) 120.8 . . . no C(20) C(19) H(19) 120.7 . . . no C(15) C(20) C(19) 119.1(2) . . . yes C(15) C(20) H(20) 120.4 . . . no C(19) C(20) H(20) 120.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(18) Cl(18) 3.284(2) . 2_758 no O(1) N(14) 2.894(2) . 2_667 no O(1) C(20) 3.312(3) . 2_667 no O(1) C(10) 3.464(3) . 1_554 no O(1) C(15) 3.551(3) . 2_667 no N(16) C(17) 3.318(3) . 2_657 no C(3) C(18) 3.533(4) . 1_454 no C(6) C(19) 3.445(4) . 1_455 no C(8) C(10) 3.478(4) . 2_668 no C(9) C(11) 3.598(4) . 2_668 no C(17) C(17) 3.490(5) . 2_657 no #------------------------------------------------------------------------------ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(14)' 'H(14n)' 'O(1)' '1.04' '1.93' '2.894(2)' '152.5' '2_667' #---end data_s92 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 B2 Cl2 F8 N4 P2 Pt' _chemical_formula_weight 1022.21 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.82140(10) _cell_length_b 18.0482(2) _cell_length_c 17.5951(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.9540(5) _cell_angle_gamma 90.00 _cell_volume 4061.87(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 45264 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.49 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 3.734 _exptl_absorpt_correction_type 'Semi empirical from equivalents' _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'Phi + omega scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45264 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9139 _reflns_number_gt 7859 _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^)+(0.1000P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9139 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1251 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.004 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 Pt1 Pt 0.742265(11) 0.927609(9) 0.209721(8) 0.02132(8) Uani 1 1 d . . . P1 P 0.60631(8) 0.87377(6) 0.25964(6) 0.0243(2) Uani 1 1 d . . . P2 P 0.83071(8) 0.96250(6) 0.31751(6) 0.0244(2) Uani 1 1 d . . . Cl1 Cl 0.67596(11) 1.05990(8) -0.07405(8) 0.0472(3) Uani 1 1 d . . . Cl2 Cl 1.00986(12) 0.83464(12) -0.00473(10) 0.0755(6) Uani 1 1 d . . . F1 F 0.6497(4) 1.2149(3) 0.1066(2) 0.0987(17) Uani 1 1 d . . . F2 F 0.6741(4) 1.1031(2) 0.1662(3) 0.0925(14) Uani 1 1 d . . . F3 F 0.5655(5) 1.1836(3) 0.2052(4) 0.141(3) Uani 1 1 d . . . F4 F 0.7348(3) 1.2108(3) 0.2185(2) 0.0830(15) Uani 1 1 d . . . F5 F -0.0978(3) 0.6294(2) 0.1312(2) 0.0702(10) Uani 1 1 d . . . F6 F -0.1648(6) 0.7439(3) 0.1615(3) 0.091(2) Uani 0.70 1 d P . . F6' F -0.2501(5) 0.6596(4) 0.1726(4) 0.0216(16) Uani 0.30 1 d P . . F7 F -0.0179(7) 0.7263(4) 0.1706(4) 0.160(3) Uani 1 1 d . . . F8 F -0.1083(3) 0.66386(18) 0.25364(18) 0.0578(9) Uani 1 1 d . . . N1 N 0.5454(3) 0.8198(2) 0.1178(2) 0.0329(8) Uani 1 1 d . . . H1 H 0.4928 0.7958 0.0973 0.039 Uiso 1 1 calc R . . N2 N 0.6595(3) 0.92088(19) 0.1001(2) 0.0231(8) Uani 1 1 d . . . N3 N 0.9476(3) 1.0534(2) 0.2312(2) 0.0379(9) Uani 1 1 d . . . H3 H 0.9925 1.0889 0.2327 0.045 Uiso 1 1 calc R . . N4 N 0.8830(3) 0.9515(2) 0.1572(2) 0.0280(7) Uani 1 1 d . . . B1 B 0.6587(5) 1.1766(3) 0.1731(4) 0.0427(14) Uani 1 1 d . . . B2 B -0.1257(7) 0.6825(4) 0.1787(4) 0.065(2) Uani 1 1 d . . . C1 C 0.4853(4) 0.9250(2) 0.2633(3) 0.0274(10) Uani 1 1 d . . . C2 C 0.3921(4) 0.8869(3) 0.2747(3) 0.0375(11) Uani 1 1 d . . . H2 H 0.3922 0.8357 0.2809 0.045 Uiso 1 1 calc R . . C3 C 0.3013(4) 0.9261(3) 0.2767(3) 0.0472(15) Uani 1 1 d . . . H3 H 0.2393 0.9014 0.2846 0.057 Uiso 1 1 calc R . . C4 C 0.3006(4) 1.0027(4) 0.2668(3) 0.0463(14) Uani 1 1 d . . . H4 H 0.2381 1.0288 0.2678 0.056 Uiso 1 1 calc R . . C5 C 0.3912(4) 1.0397(3) 0.2557(3) 0.0405(12) Uani 1 1 d . . . H5 H 0.3907 1.0910 0.2502 0.049 Uiso 1 1 calc R . . C6 C 0.4847(3) 1.0004(3) 0.2526(2) 0.0318(10) Uani 1 1 d . . . H6 H 0.5462 1.0251 0.2434 0.038 Uiso 1 1 calc R . . C7 C 0.6355(3) 0.8272(2) 0.3493(2) 0.0284(9) Uani 1 1 d . . . C8 C 0.5805(4) 0.8386(3) 0.4127(3) 0.0347(10) Uani 1 1 d . . . H8 H 0.5210 0.8683 0.4093 0.042 Uiso 1 1 calc R . . C9 C 0.6132(4) 0.8060(3) 0.4814(3) 0.0448(13) Uani 1 1 d . . . H9 H 0.5768 0.8148 0.5245 0.054 Uiso 1 1 calc R . . C10 C 0.7001(4) 0.7602(3) 0.4860(3) 0.0451(13) Uani 1 1 d . . . H10 H 0.7231 0.7393 0.5325 0.054 Uiso 1 1 calc R . . C11 C 0.7528(4) 0.7456(3) 0.4219(3) 0.0449(13) Uani 1 1 d . . . H11 H 0.8095 0.7132 0.4247 0.054 Uiso 1 1 calc R . . C12 C 0.7214(3) 0.7790(3) 0.3540(3) 0.0350(10) Uani 1 1 d . . . H12 H 0.7572 0.7695 0.3108 0.042 Uiso 1 1 calc R . . C13 C 0.5805(4) 0.7963(2) 0.1936(3) 0.0316(10) Uani 1 1 d . . . H13A H 0.6439 0.7673 0.1911 0.038 Uiso 1 1 calc R . . H13B H 0.5277 0.7644 0.2134 0.038 Uiso 1 1 calc R . . C14 C 0.5827(3) 0.8734(2) 0.0748(2) 0.0283(9) Uani 1 1 d . . . C15 C 0.5369(4) 0.8798(3) -0.0016(3) 0.0361(11) Uani 1 1 d . . . H15 H 0.4862 0.8461 -0.0195 0.043 Uiso 1 1 calc R . . C16 C 0.5667(4) 0.9341(3) -0.0479(3) 0.0380(12) Uani 1 1 d . . . H16 H 0.5378 0.9379 -0.0977 0.046 Uiso 1 1 calc R . . C17 C 0.6418(3) 0.9844(3) -0.0194(2) 0.0335(10) Uani 1 1 d . . . C18 C 0.6860(3) 0.9763(3) 0.0521(2) 0.0301(9) Uani 1 1 d . . . H18 H 0.7369 1.0101 0.0696 0.036 Uiso 1 1 calc R . . C19 C 0.9455(3) 0.9101(3) 0.3477(3) 0.0286(9) Uani 1 1 d . . . C20 C 1.0140(4) 0.9347(3) 0.4066(3) 0.0372(12) Uani 1 1 d . . . H20 H 1.0023 0.9803 0.4290 0.045 Uiso 1 1 calc R . . C21 C 1.0988(4) 0.8930(3) 0.4324(3) 0.0416(12) Uani 1 1 d . . . H21 H 1.1438 0.9101 0.4723 0.050 Uiso 1 1 calc R . . C22 C 1.1172(4) 0.8239(3) 0.3981(3) 0.0407(12) Uani 1 1 d . . . H22 H 1.1730 0.7944 0.4160 0.049 Uiso 1 1 calc R . . C23 C 1.0511(4) 0.8011(3) 0.3377(3) 0.0379(11) Uani 1 1 d . . . H23 H 1.0646 0.7566 0.3134 0.045 Uiso 1 1 calc R . . C24 C 0.9659(3) 0.8423(3) 0.3124(3) 0.0304(9) Uani 1 1 d . . . H24 H 0.9217 0.8254 0.2720 0.036 Uiso 1 1 calc R . . C25 C 0.7606(3) 0.9825(2) 0.4002(2) 0.0263(9) Uani 1 1 d . . . C26 C 0.7797(4) 0.9460(3) 0.4692(3) 0.0325(10) Uani 1 1 d . . . H26 H 0.8323 0.9105 0.4743 0.039 Uiso 1 1 calc R . . C27 C 0.7211(4) 0.9617(3) 0.5307(3) 0.0404(11) Uani 1 1 d . . . H27 H 0.7335 0.9359 0.5761 0.048 Uiso 1 1 calc R . . C28 C 0.6450(4) 1.0153(3) 0.5244(3) 0.0425(12) Uani 1 1 d . . . H28 H 0.6063 1.0261 0.5658 0.051 Uiso 1 1 calc R . . C29 C 0.6258(4) 1.0536(3) 0.4562(3) 0.0414(12) Uani 1 1 d . . . H29 H 0.5749 1.0904 0.4522 0.050 Uiso 1 1 calc R . . C30 C 0.6825(4) 1.0369(3) 0.3944(3) 0.0376(11) Uani 1 1 d . . . H30 H 0.6686 1.0619 0.3486 0.045 Uiso 1 1 calc R . . C31 C 0.8756(4) 1.0540(3) 0.2909(3) 0.0330(10) Uani 1 1 d . . . H31A H 0.8154 1.0838 0.2742 0.040 Uiso 1 1 calc R . . H31B H 0.9094 1.0776 0.3356 0.040 Uiso 1 1 calc R . . C32 C 0.9542(4) 1.0046(3) 0.1735(3) 0.0340(10) Uani 1 1 d . . . C33 C 1.0429(4) 1.0117(4) 0.1287(3) 0.0541(16) Uani 1 1 d . . . H33 H 1.0892 1.0509 0.1375 0.065 Uiso 1 1 calc R . . C34 C 1.0595(4) 0.9621(4) 0.0744(3) 0.0627(18) Uani 1 1 d . . . H34 H 1.1165 0.9669 0.0449 0.075 Uiso 1 1 calc R . . C35 C 0.9880(4) 0.9015(4) 0.0622(3) 0.0510(14) Uani 1 1 d . . . C36 C 0.9031(4) 0.8998(3) 0.1024(3) 0.0376(11) Uani 1 1 d . . . H36 H 0.8551 0.8617 0.0929 0.045 Uiso 1 1 calc R . . 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 Pt1 0.02167(12) 0.02314(12) 0.01886(12) -0.00060(5) -0.00071(7) -0.00086(5) P1 0.0261(5) 0.0248(6) 0.0220(5) 0.0011(4) 0.0013(4) -0.0004(4) P2 0.0255(5) 0.0272(6) 0.0200(5) -0.0019(4) -0.0016(4) 0.0000(4) Cl1 0.0391(7) 0.0678(9) 0.0352(7) 0.0231(6) 0.0057(5) 0.0073(6) Cl2 0.0428(8) 0.1227(16) 0.0626(10) -0.0445(10) 0.0141(7) 0.0081(9) F1 0.117(4) 0.104(4) 0.068(3) 0.034(2) -0.038(3) -0.042(3) F2 0.118(4) 0.045(2) 0.115(4) -0.017(2) 0.012(3) 0.012(2) F3 0.117(4) 0.099(4) 0.219(7) -0.015(4) 0.093(5) -0.002(3) F4 0.085(3) 0.076(3) 0.081(3) -0.007(2) -0.041(3) -0.022(2) F5 0.073(2) 0.067(2) 0.070(2) -0.0273(19) -0.0026(19) 0.0108(19) F6 0.167(6) 0.070(4) 0.034(2) 0.016(2) 0.001(3) 0.085(4) F6' 0.014(3) 0.020(4) 0.030(4) -0.004(3) 0.001(3) -0.003(3) F7 0.215(8) 0.143(6) 0.125(5) -0.028(4) 0.032(5) -0.054(6) F8 0.072(2) 0.055(2) 0.0459(18) 0.0091(15) -0.0038(16) 0.0272(17) N1 0.039(2) 0.031(2) 0.028(2) -0.0051(16) -0.0045(16) -0.0050(17) N2 0.0216(18) 0.027(2) 0.0201(18) -0.0005(13) 0.0007(14) 0.0037(13) N3 0.041(2) 0.040(2) 0.033(2) -0.0030(18) -0.0001(18) -0.0155(19) N4 0.0218(17) 0.038(2) 0.0239(18) -0.0009(16) -0.0021(14) -0.0011(16) B1 0.043(3) 0.038(3) 0.045(3) -0.007(3) -0.005(3) -0.003(3) B2 0.100(6) 0.051(4) 0.040(4) -0.013(3) -0.010(4) 0.021(4) C1 0.024(2) 0.036(3) 0.021(2) 0.0028(16) 0.0009(18) 0.0037(16) C2 0.035(2) 0.049(3) 0.029(2) 0.007(2) 0.0013(19) -0.003(2) C3 0.028(3) 0.081(5) 0.033(3) 0.001(2) 0.007(2) -0.003(2) C4 0.034(3) 0.081(4) 0.024(2) 0.000(2) 0.002(2) 0.019(3) C5 0.045(3) 0.046(3) 0.030(2) -0.001(2) 0.001(2) 0.020(2) C6 0.029(2) 0.039(3) 0.028(2) -0.0012(19) 0.0005(18) 0.0005(19) C7 0.027(2) 0.027(2) 0.030(2) 0.0059(17) 0.0008(17) -0.0061(17) C8 0.040(3) 0.036(3) 0.027(2) 0.0062(19) 0.0012(19) 0.000(2) C9 0.055(3) 0.052(3) 0.028(3) 0.013(2) 0.005(2) -0.003(3) C10 0.045(3) 0.051(3) 0.038(3) 0.022(2) -0.005(2) -0.005(2) C11 0.034(3) 0.042(3) 0.058(3) 0.018(3) -0.005(2) -0.001(2) C12 0.033(2) 0.036(3) 0.036(3) 0.008(2) 0.0018(19) 0.002(2) C13 0.035(2) 0.027(2) 0.033(2) 0.0003(18) -0.0001(19) -0.0031(19) C14 0.027(2) 0.031(2) 0.027(2) -0.0061(17) -0.0032(17) 0.0033(18) C15 0.034(2) 0.048(3) 0.026(2) -0.010(2) -0.0076(19) 0.003(2) C16 0.033(3) 0.059(4) 0.022(2) -0.003(2) 0.000(2) 0.011(2) C17 0.026(2) 0.050(3) 0.025(2) 0.0073(19) 0.0036(17) 0.013(2) C18 0.027(2) 0.036(2) 0.027(2) 0.0042(18) 0.0029(17) 0.0033(18) C19 0.024(2) 0.038(2) 0.024(2) -0.0004(18) -0.0001(17) -0.0029(19) C20 0.035(3) 0.042(3) 0.034(3) -0.0095(19) -0.008(2) -0.0005(19) C21 0.034(2) 0.051(3) 0.038(3) -0.005(2) -0.012(2) -0.002(2) C22 0.028(2) 0.048(3) 0.045(3) 0.008(2) -0.004(2) 0.005(2) C23 0.032(2) 0.037(3) 0.045(3) -0.008(2) 0.000(2) 0.002(2) C24 0.027(2) 0.035(2) 0.030(2) -0.0047(18) 0.0034(17) 0.0002(18) C25 0.029(2) 0.025(2) 0.024(2) -0.0042(16) -0.0004(16) 0.0005(17) C26 0.031(2) 0.035(2) 0.031(2) 0.0008(19) -0.0016(19) 0.005(2) C27 0.046(3) 0.050(3) 0.025(2) 0.003(2) -0.001(2) 0.003(2) C28 0.040(3) 0.060(3) 0.028(2) -0.010(2) 0.005(2) 0.009(2) C29 0.037(3) 0.045(3) 0.041(3) -0.006(2) 0.000(2) 0.021(2) C30 0.040(3) 0.046(3) 0.026(2) -0.002(2) -0.0046(19) 0.008(2) C31 0.033(2) 0.029(2) 0.036(3) -0.004(2) -0.002(2) -0.006(2) C32 0.032(2) 0.041(3) 0.028(2) 0.004(2) -0.0036(18) -0.008(2) C33 0.035(3) 0.090(5) 0.038(3) -0.003(3) 0.004(2) -0.025(3) C34 0.027(3) 0.116(6) 0.046(3) -0.018(4) 0.013(2) -0.017(3) C35 0.030(3) 0.089(4) 0.034(3) -0.017(3) 0.005(2) -0.001(3) C36 0.030(2) 0.046(3) 0.036(3) -0.005(2) -0.001(2) 0.004(2) _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 Pt1 N4 2.127(4) . ? Pt1 N2 2.140(4) . ? Pt1 P1 2.2283(11) . ? Pt1 P2 2.2321(10) . ? P1 C7 1.804(4) . ? P1 C1 1.810(5) . ? P1 C13 1.834(4) . ? P2 C25 1.799(4) . ? P2 C19 1.799(5) . ? P2 C31 1.822(5) . ? Cl1 C17 1.740(5) . ? Cl2 C35 1.722(6) . ? F1 B1 1.356(7) . ? F2 B1 1.349(7) . ? F3 B1 1.363(8) . ? F4 B1 1.364(6) . ? F5 B2 1.336(8) . ? F6 B2 1.246(8) . ? F6' B2 1.645(12) . ? F7 B2 1.606(12) . ? F8 B2 1.364(8) . ? N1 C14 1.337(6) . ? N1 C13 1.441(6) . ? N2 C14 1.358(6) . ? N2 C18 1.366(6) . ? N3 C32 1.351(6) . ? N3 C31 1.445(7) . ? N4 C32 1.342(6) . ? N4 C36 1.379(6) . ? C1 C6 1.373(6) . ? C1 C2 1.406(7) . ? C2 C3 1.364(8) . ? C3 C4 1.394(8) . ? C4 C5 1.366(8) . ? C5 C6 1.398(7) . ? C7 C8 1.375(6) . ? C7 C12 1.402(6) . ? C8 C9 1.384(6) . ? C9 C10 1.385(8) . ? C10 C11 1.379(8) . ? C11 C12 1.375(7) . ? C14 C15 1.435(6) . ? C15 C16 1.345(7) . ? C16 C17 1.392(7) . ? C17 C18 1.352(6) . ? C19 C20 1.384(7) . ? C19 C24 1.405(7) . ? C20 C21 1.374(7) . ? C21 C22 1.412(7) . ? C22 C23 1.376(7) . ? C23 C24 1.370(6) . ? C25 C26 1.389(6) . ? C25 C30 1.400(6) . ? C26 C27 1.388(7) . ? C27 C28 1.374(7) . ? C28 C29 1.391(8) . ? C29 C30 1.383(7) . ? C32 C33 1.433(7) . ? C33 C34 1.336(9) . ? C34 C35 1.435(9) . ? C35 C36 1.339(7) . ? 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 N4 Pt1 N2 90.15(14) . . ? N4 Pt1 P1 165.83(11) . . ? N2 Pt1 P1 88.74(11) . . ? N4 Pt1 P2 85.14(10) . . ? N2 Pt1 P2 166.69(9) . . ? P1 Pt1 P2 98.83(4) . . ? C7 P1 C1 109.5(2) . . ? C7 P1 C13 102.5(2) . . ? C1 P1 C13 107.1(2) . . ? C7 P1 Pt1 115.29(14) . . ? C1 P1 Pt1 119.12(15) . . ? C13 P1 Pt1 101.25(15) . . ? C25 P2 C19 108.2(2) . . ? C25 P2 C31 102.1(2) . . ? C19 P2 C31 106.6(2) . . ? C25 P2 Pt1 119.38(14) . . ? C19 P2 Pt1 117.38(16) . . ? C31 P2 Pt1 100.85(16) . . ? C14 N1 C13 129.5(4) . . ? C14 N2 C18 117.7(4) . . ? C14 N2 Pt1 129.4(3) . . ? C18 N2 Pt1 112.7(3) . . ? C32 N3 C31 128.9(4) . . ? C32 N4 C36 118.4(4) . . ? C32 N4 Pt1 129.6(3) . . ? C36 N4 Pt1 111.8(3) . . ? F2 B1 F1 115.3(5) . . ? F2 B1 F3 105.4(5) . . ? F1 B1 F3 106.6(6) . . ? F2 B1 F4 113.3(5) . . ? F1 B1 F4 106.8(5) . . ? F3 B1 F4 109.1(6) . . ? F6 B2 F5 127.4(6) . . ? F6 B2 F8 119.3(6) . . ? F5 B2 F8 113.3(6) . . ? F6 B2 F7 82.8(7) . . ? F5 B2 F7 91.7(6) . . ? F8 B2 F7 97.1(6) . . ? F6 B2 F6' 80.4(7) . . ? F5 B2 F6' 94.6(6) . . ? F8 B2 F6' 95.4(6) . . ? F7 B2 F6' 162.6(7) . . ? C6 C1 C2 120.5(4) . . ? C6 C1 P1 119.9(4) . . ? C2 C1 P1 119.6(3) . . ? C3 C2 C1 119.1(5) . . ? C2 C3 C4 120.6(5) . . ? C5 C4 C3 120.3(5) . . ? C4 C5 C6 119.8(5) . . ? C1 C6 C5 119.7(5) . . ? C8 C7 C12 119.4(4) . . ? C8 C7 P1 123.6(3) . . ? C12 C7 P1 117.0(3) . . ? C7 C8 C9 120.2(5) . . ? C8 C9 C10 119.9(5) . . ? C11 C10 C9 120.3(5) . . ? C12 C11 C10 119.7(5) . . ? C11 C12 C7 120.3(5) . . ? N1 C13 P1 113.1(3) . . ? N1 C14 N2 123.5(4) . . ? N1 C14 C15 116.8(4) . . ? N2 C14 C15 119.8(4) . . ? C16 C15 C14 120.8(4) . . ? C15 C16 C17 118.4(4) . . ? C18 C17 C16 119.9(5) . . ? C18 C17 Cl1 119.6(4) . . ? C16 C17 Cl1 120.4(3) . . ? C17 C18 N2 123.3(4) . . ? C20 C19 C24 118.8(4) . . ? C20 C19 P2 121.1(4) . . ? C24 C19 P2 120.1(3) . . ? C21 C20 C19 121.3(5) . . ? C20 C21 C22 119.6(4) . . ? C23 C22 C21 118.9(4) . . ? C24 C23 C22 121.5(5) . . ? C23 C24 C19 119.9(4) . . ? C26 C25 C30 118.6(4) . . ? C26 C25 P2 122.9(3) . . ? C30 C25 P2 118.5(3) . . ? C25 C26 C27 120.8(4) . . ? C28 C27 C26 120.1(5) . . ? C27 C28 C29 120.1(5) . . ? C30 C29 C28 119.8(5) . . ? C29 C30 C25 120.6(4) . . ? N3 C31 P2 114.1(3) . . ? N4 C32 N3 123.3(4) . . ? N4 C32 C33 120.0(5) . . ? N3 C32 C33 116.7(4) . . ? C34 C33 C32 120.3(5) . . ? C33 C34 C35 119.1(5) . . ? C36 C35 C34 118.2(5) . . ? C36 C35 Cl2 121.5(5) . . ? C34 C35 Cl2 120.3(4) . . ? C35 C36 N4 123.5(5) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.694 _refine_diff_density_min -2.118 _refine_diff_density_rms 0.158