# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/185 data_S1 #*complex 1* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 Cl4 N O3 P2 Pd' _chemical_formula_weight 923.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.628(19) _cell_length_b 11.548(13) _cell_length_c 19.43(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.100(10) _cell_angle_gamma 90.00 _cell_volume 4174(8) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11573 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.94 _reflns_number_total 7263 _reflns_number_gt 5299 _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 w=1/[\s^2^(Fo^2^)+(0.1248P)^2^+23.3956P] 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 SHELXL _refine_ls_extinction_coef 0.0011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7263 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.47143(2) 0.14903(3) 0.32405(2) 0.03207(17) Uani 1 d . . . P1 P 0.36225(8) 0.22660(12) 0.35588(7) 0.0336(3) Uani 1 d . . . P2 P 0.58479(7) 0.09016(12) 0.29309(7) 0.0346(3) Uani 1 d . . . Cl Cl 0.51943(8) 0.18207(14) 0.43419(7) 0.0477(4) Uani 1 d . . . O71 O 0.4777(2) 0.3167(4) 0.2252(2) 0.0522(11) Uani 1 d . . . N1 N 0.4239(2) 0.0914(4) 0.2308(2) 0.0351(10) Uani 1 d . . . C6 C 0.4171(3) 0.1550(5) 0.1724(3) 0.0388(13) Uani 1 d . . . O72 O 0.4409(3) 0.3276(5) 0.1146(3) 0.0697(14) Uani 1 d . . . C21 C 0.3122(3) 0.1375(5) 0.4137(3) 0.0371(12) Uani 1 d . . . C11 C 0.3771(3) 0.3684(5) 0.3953(3) 0.0441(14) Uani 1 d . . . C61 C 0.6153(3) -0.0476(5) 0.3286(3) 0.0427(13) Uani 1 d . . . C46 C 0.6084(4) 0.1642(6) 0.1594(3) 0.0550(17) Uani 1 d . . . H46 H 0.6236 0.2337 0.1794 0.066 Uiso 1 calc R . . C35 C 0.2644(4) 0.3574(5) 0.1791(3) 0.0485(15) Uani 1 d . . . H35 H 0.2678 0.4235 0.1522 0.058 Uiso 1 calc R . . C36 C 0.3054(3) 0.3487(5) 0.2406(3) 0.0418(13) Uani 1 d . . . H36 H 0.3364 0.4083 0.2546 0.050 Uiso 1 calc R . . O25 O 0.3731(3) 0.1690(5) 0.0559(2) 0.0736(15) Uani 1 d . . . HO25 H 0.3945 0.2308 0.0605 0.088 Uiso 1 calc R . . C62 C 0.5789(4) -0.1002(5) 0.3817(3) 0.0478(14) Uani 1 d . . . H62 H 0.5393 -0.0639 0.3993 0.057 Uiso 1 calc R . . C41 C 0.5901(3) 0.0730(5) 0.2001(3) 0.0407(13) Uani 1 d . . . C5 C 0.3813(3) 0.1081(6) 0.1139(3) 0.0501(15) Uani 1 d . . . C22 C 0.3458(3) 0.0443(5) 0.4476(3) 0.0444(14) Uani 1 d . . . H22 H 0.3941 0.0295 0.4417 0.053 Uiso 1 calc R . . C23 C 0.3079(4) -0.0264(6) 0.4898(3) 0.0563(17) Uani 1 d . . . H23 H 0.3310 -0.0877 0.5127 0.068 Uiso 1 calc R . . C26 C 0.2392(4) 0.1569(6) 0.4238(3) 0.0533(16) Uani 1 d . . . H26 H 0.2159 0.2192 0.4021 0.064 Uiso 1 calc R . . C56 C 0.7190(3) 0.1744(7) 0.3477(3) 0.0541(17) Uani 1 d . . . H56 H 0.7337 0.0976 0.3519 0.065 Uiso 1 calc R . . C2 C 0.3974(3) -0.0154(5) 0.2336(3) 0.0471(14) Uani 1 d . . . H2 H 0.4039 -0.0579 0.2741 0.057 Uiso 1 calc R . . C31 C 0.2997(3) 0.2496(5) 0.2813(3) 0.0375(12) Uani 1 d . . . C32 C 0.2530(3) 0.1621(5) 0.2587(3) 0.0433(14) Uani 1 d . . . H32 H 0.2483 0.0963 0.2857 0.052 Uiso 1 calc R . . C51 C 0.6508(3) 0.1997(6) 0.3199(3) 0.0428(13) Uani 1 d . . . C7 C 0.4475(3) 0.2756(5) 0.1724(3) 0.0445(14) Uani 1 d . . . C3 C 0.3605(4) -0.0641(6) 0.1775(4) 0.0577(18) Uani 1 d . . . H3 H 0.3414 -0.1383 0.1801 0.069 Uiso 1 calc R . . C66 C 0.6737(4) -0.1050(7) 0.3032(4) 0.0592(18) Uani 1 d . . . H66 H 0.6981 -0.0722 0.2675 0.071 Uiso 1 calc R . . C4 C 0.3523(4) -0.0010(7) 0.1173(4) 0.0621(19) Uani 1 d . . . H4 H 0.3272 -0.0323 0.0791 0.074 Uiso 1 calc R . . C34 C 0.2188(4) 0.2701(6) 0.1574(3) 0.0588(18) Uani 1 d . . . H34 H 0.1914 0.2774 0.1162 0.071 Uiso 1 calc R . . C45 C 0.6040(4) 0.1521(8) 0.0873(4) 0.071(2) Uani 1 d . . . H45 H 0.6173 0.2131 0.0594 0.085 Uiso 1 calc R . . C63 C 0.6020(5) -0.2061(6) 0.4078(4) 0.0620(19) Uani 1 d . . . H63 H 0.5776 -0.2403 0.4431 0.074 Uiso 1 calc R . . C12 C 0.3355(5) 0.4087(6) 0.4474(4) 0.066(2) Uani 1 d . . . H12 H 0.2980 0.3640 0.4627 0.080 Uiso 1 calc R . . C43 C 0.5630(4) -0.0390(7) 0.0981(4) 0.0615(19) Uani 1 d . . . H43 H 0.5486 -0.1085 0.0776 0.074 Uiso 1 calc R . . C24 C 0.2361(4) -0.0067(7) 0.4982(4) 0.0631(19) Uani 1 d . . . H24 H 0.2107 -0.0555 0.5261 0.076 Uiso 1 calc R . . C52 C 0.6317(4) 0.3151(6) 0.3128(4) 0.0551(17) Uani 1 d . . . H52 H 0.5864 0.3341 0.2937 0.066 Uiso 1 calc R . . C33 C 0.2135(4) 0.1716(6) 0.1969(4) 0.0573(17) Uani 1 d . . . H33 H 0.1833 0.1115 0.1818 0.069 Uiso 1 calc R . . C44 C 0.5804(4) 0.0514(9) 0.0586(4) 0.073(2) Uani 1 d . . . H44 H 0.5761 0.0446 0.0109 0.088 Uiso 1 calc R . . C42 C 0.5663(3) -0.0290(6) 0.1687(3) 0.0478(15) Uani 1 d . . . H42 H 0.5525 -0.0909 0.1956 0.057 Uiso 1 calc R . . C54 C 0.7457(4) 0.3759(8) 0.3631(4) 0.064(2) Uani 1 d . . . H54 H 0.7770 0.4341 0.3786 0.077 Uiso 1 calc R . . C64 C 0.6599(5) -0.2610(7) 0.3827(4) 0.072(2) Uani 1 d . . . H64 H 0.6749 -0.3322 0.4007 0.086 Uiso 1 calc R . . C25 C 0.2016(4) 0.0855(8) 0.4652(4) 0.065(2) Uani 1 d . . . H25 H 0.1531 0.0990 0.4712 0.078 Uiso 1 calc R . . C53 C 0.6790(4) 0.4034(6) 0.3335(4) 0.0607(18) Uani 1 d . . . H53 H 0.6656 0.4804 0.3275 0.073 Uiso 1 calc R . . C16 C 0.4331(4) 0.4347(6) 0.3741(4) 0.066(2) Uani 1 d . . . H16 H 0.4614 0.4076 0.3395 0.079 Uiso 1 calc R . . C13 C 0.3504(7) 0.5161(8) 0.4764(4) 0.092(3) Uani 1 d . . . H13 H 0.3219 0.5448 0.5103 0.110 Uiso 1 calc R . . C55 C 0.7656(4) 0.2624(8) 0.3693(4) 0.070(2) Uani 1 d . . . H55 H 0.8110 0.2438 0.3883 0.084 Uiso 1 calc R . . C15 C 0.4478(5) 0.5427(7) 0.4043(6) 0.089(3) Uani 1 d . . . H15 H 0.4851 0.5882 0.3894 0.107 Uiso 1 calc R . . C65 C 0.6961(5) -0.2103(7) 0.3303(4) 0.078(2) Uani 1 d . . . H65 H 0.7358 -0.2472 0.3133 0.094 Uiso 1 calc R . . C14 C 0.4069(7) 0.5802(7) 0.4555(5) 0.098(4) Uani 1 d . . . H14 H 0.4175 0.6507 0.4767 0.117 Uiso 1 calc R . . C99 C 0.4841(6) 0.4376(10) -0.1460(8) 0.125(4) Uani 1 d . . . H99 H 0.5029 0.5165 -0.1405 0.151 Uiso 1 calc R . . Cl2 Cl 0.4814(3) 0.3749(4) -0.0645(3) 0.189(2) Uani 1 d . . . Cl3 Cl 0.5436(7) 0.3583(5) -0.1891(4) 0.326(6) Uani 1 d . . . Cl4 Cl 0.4051(4) 0.4447(9) -0.1815(6) 0.464(10) Uani 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 Pd 0.0331(3) 0.0317(3) 0.0313(3) -0.00504(15) 0.00026(16) 0.00060(16) P1 0.0357(7) 0.0338(7) 0.0310(7) -0.0054(5) -0.0006(5) 0.0056(6) P2 0.0333(7) 0.0390(8) 0.0315(7) -0.0033(6) 0.0025(5) 0.0018(6) Cl 0.0461(8) 0.0602(9) 0.0358(7) -0.0136(6) -0.0063(6) 0.0041(7) O71 0.060(3) 0.043(2) 0.053(3) 0.000(2) -0.006(2) -0.013(2) N1 0.033(2) 0.038(2) 0.035(2) -0.0096(19) 0.0045(18) -0.002(2) C6 0.039(3) 0.043(3) 0.034(3) -0.005(2) 0.003(2) -0.001(2) O72 0.091(4) 0.069(3) 0.049(3) 0.021(2) -0.006(3) -0.015(3) C21 0.039(3) 0.046(3) 0.026(3) -0.003(2) 0.000(2) 0.006(2) C11 0.051(4) 0.038(3) 0.042(3) -0.013(2) -0.009(3) 0.014(3) C61 0.044(3) 0.046(3) 0.038(3) -0.005(2) 0.002(2) 0.005(3) C46 0.062(4) 0.060(4) 0.044(4) -0.002(3) 0.016(3) -0.005(3) C35 0.071(4) 0.034(3) 0.039(3) 0.006(2) -0.003(3) 0.009(3) C36 0.050(3) 0.029(3) 0.047(3) -0.002(2) -0.003(3) 0.006(2) O25 0.096(4) 0.090(4) 0.034(3) -0.002(2) -0.006(2) -0.008(3) C62 0.057(4) 0.044(3) 0.042(3) -0.007(3) 0.004(3) -0.002(3) C41 0.031(3) 0.057(4) 0.033(3) -0.001(3) 0.001(2) 0.001(3) C5 0.050(4) 0.067(4) 0.034(3) -0.011(3) 0.004(3) -0.004(3) C22 0.043(3) 0.046(3) 0.043(3) 0.001(3) 0.000(3) 0.003(3) C23 0.069(5) 0.059(4) 0.040(3) 0.012(3) -0.003(3) 0.000(3) C26 0.048(4) 0.068(4) 0.045(4) 0.006(3) 0.010(3) 0.015(3) C56 0.036(3) 0.071(4) 0.055(4) 0.009(3) -0.007(3) -0.003(3) C2 0.049(4) 0.043(3) 0.050(4) -0.013(3) 0.007(3) -0.007(3) C31 0.039(3) 0.033(3) 0.041(3) -0.004(2) 0.004(2) 0.009(2) C32 0.049(3) 0.039(3) 0.041(3) 0.004(2) -0.001(3) -0.004(3) C51 0.039(3) 0.054(4) 0.036(3) -0.006(3) 0.003(2) -0.006(3) C7 0.041(3) 0.048(3) 0.044(3) 0.003(3) -0.002(3) 0.000(3) C3 0.060(4) 0.051(4) 0.063(4) -0.020(3) 0.009(3) -0.021(3) C66 0.054(4) 0.066(4) 0.058(4) 0.002(3) 0.008(3) 0.023(4) C4 0.065(4) 0.074(5) 0.047(4) -0.024(4) -0.001(3) -0.016(4) C34 0.070(5) 0.058(4) 0.045(4) -0.003(3) -0.019(3) 0.002(4) C45 0.070(5) 0.098(7) 0.045(4) 0.019(4) 0.009(4) -0.003(4) C63 0.100(6) 0.040(4) 0.045(4) 0.001(3) 0.006(4) 0.001(4) C12 0.097(6) 0.053(4) 0.049(4) -0.014(3) 0.006(4) 0.008(4) C43 0.057(4) 0.078(5) 0.049(4) -0.024(4) -0.001(3) 0.004(4) C24 0.057(4) 0.088(5) 0.045(4) 0.019(4) 0.006(3) -0.007(4) C52 0.040(3) 0.059(4) 0.066(4) -0.013(3) -0.004(3) 0.004(3) C33 0.061(4) 0.056(4) 0.053(4) 0.001(3) -0.017(3) -0.009(3) C44 0.075(5) 0.106(7) 0.038(4) -0.007(4) 0.005(4) 0.016(5) C42 0.042(3) 0.055(4) 0.047(4) -0.012(3) 0.003(3) 0.006(3) C54 0.054(4) 0.088(6) 0.051(4) -0.013(4) 0.006(3) -0.030(4) C64 0.112(7) 0.050(4) 0.052(4) -0.002(3) -0.009(4) 0.024(4) C25 0.048(4) 0.095(6) 0.055(4) 0.005(4) 0.016(3) 0.004(4) C53 0.062(4) 0.048(4) 0.072(5) -0.013(3) 0.002(4) -0.016(3) C16 0.058(4) 0.045(4) 0.093(6) -0.022(4) -0.011(4) 0.002(3) C13 0.148(10) 0.069(6) 0.059(5) -0.030(4) 0.002(6) 0.017(6) C55 0.035(4) 0.101(7) 0.073(5) 0.008(4) -0.009(3) -0.021(4) C15 0.086(6) 0.042(4) 0.133(8) -0.024(5) -0.046(6) -0.003(4) C65 0.091(6) 0.075(5) 0.069(5) -0.005(4) 0.010(4) 0.040(5) C14 0.156(10) 0.046(5) 0.083(6) -0.033(5) -0.067(7) 0.017(6) C99 0.105(8) 0.075(7) 0.194(13) 0.030(8) -0.013(8) -0.030(6) Cl2 0.192(4) 0.172(4) 0.198(5) 0.061(3) -0.040(4) -0.079(3) Cl3 0.553(17) 0.144(5) 0.294(9) -0.041(5) 0.153(10) 0.046(7) Cl4 0.194(5) 0.562(14) 0.607(15) 0.478(14) -0.231(8) -0.240(8) _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 Pd N1 2.081(5) . ? Pd Cl 2.306(3) . ? Pd P2 2.328(2) . ? Pd P1 2.336(2) . ? P1 C21 1.818(6) . ? P1 C11 1.822(6) . ? P1 C31 1.829(6) . ? P2 C61 1.812(6) . ? P2 C51 1.821(6) . ? P2 C41 1.827(6) . ? O71 C7 1.238(7) . ? N1 C2 1.332(8) . ? N1 C6 1.352(7) . ? C6 C5 1.396(8) . ? C6 C7 1.503(8) . ? O72 C7 1.274(7) . ? C21 C22 1.392(8) . ? C21 C26 1.403(9) . ? C11 C16 1.375(10) . ? C11 C12 1.388(9) . ? C61 C66 1.389(9) . ? C61 C62 1.403(9) . ? C46 C41 1.370(9) . ? C46 C45 1.407(10) . ? C35 C34 1.369(9) . ? C35 C36 1.386(9) . ? C36 C31 1.398(8) . ? O25 C5 1.332(8) . ? C62 C63 1.384(9) . ? C41 C42 1.388(9) . ? C5 C4 1.374(10) . ? C22 C23 1.378(9) . ? C23 C24 1.374(10) . ? C26 C25 1.370(10) . ? C56 C51 1.385(9) . ? C56 C55 1.386(10) . ? C2 C3 1.376(9) . ? C31 C32 1.389(8) . ? C32 C33 1.380(9) . ? C51 C52 1.384(10) . ? C3 C4 1.378(10) . ? C66 C65 1.381(11) . ? C34 C33 1.379(10) . ? C45 C44 1.352(12) . ? C63 C64 1.365(11) . ? C12 C13 1.384(12) . ? C43 C44 1.346(12) . ? C43 C42 1.374(9) . ? C24 C25 1.383(11) . ? C52 C53 1.392(9) . ? C54 C55 1.365(12) . ? C54 C53 1.378(11) . ? C64 C65 1.382(12) . ? C16 C15 1.398(10) . ? C13 C14 1.366(15) . ? C15 C14 1.356(15) . ? C99 Cl4 1.593(13) . ? C99 Cl3 1.694(15) . ? C99 Cl2 1.745(14) . ? 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 Pd Cl 170.28(13) . . ? N1 Pd P2 91.75(13) . . ? Cl Pd P2 88.66(7) . . ? N1 Pd P1 91.02(13) . . ? Cl Pd P1 89.44(7) . . ? P2 Pd P1 174.36(5) . . ? C21 P1 C11 108.7(3) . . ? C21 P1 C31 104.3(3) . . ? C11 P1 C31 106.1(3) . . ? C21 P1 Pd 115.41(19) . . ? C11 P1 Pd 109.9(2) . . ? C31 P1 Pd 111.83(19) . . ? C61 P2 C51 108.0(3) . . ? C61 P2 C41 104.4(3) . . ? C51 P2 C41 106.7(3) . . ? C61 P2 Pd 115.3(2) . . ? C51 P2 Pd 109.3(2) . . ? C41 P2 Pd 112.69(19) . . ? C2 N1 C6 121.2(5) . . ? C2 N1 Pd 113.8(4) . . ? C6 N1 Pd 125.0(4) . . ? N1 C6 C5 119.5(5) . . ? N1 C6 C7 119.1(5) . . ? C5 C6 C7 121.5(6) . . ? C22 C21 C26 118.1(6) . . ? C22 C21 P1 119.9(4) . . ? C26 C21 P1 122.0(5) . . ? C16 C11 C12 119.6(6) . . ? C16 C11 P1 118.4(5) . . ? C12 C11 P1 122.0(6) . . ? C66 C61 C62 118.3(6) . . ? C66 C61 P2 121.3(5) . . ? C62 C61 P2 120.4(5) . . ? C41 C46 C45 119.7(7) . . ? C34 C35 C36 121.1(6) . . ? C35 C36 C31 119.4(6) . . ? C63 C62 C61 120.1(6) . . ? C46 C41 C42 118.9(6) . . ? C46 C41 P2 121.0(5) . . ? C42 C41 P2 119.6(5) . . ? O25 C5 C4 119.8(6) . . ? O25 C5 C6 120.8(6) . . ? C4 C5 C6 119.3(6) . . ? C23 C22 C21 120.5(6) . . ? C24 C23 C22 120.4(6) . . ? C25 C26 C21 121.1(6) . . ? C51 C56 C55 120.6(7) . . ? N1 C2 C3 121.2(6) . . ? C32 C31 C36 118.8(5) . . ? C32 C31 P1 120.3(4) . . ? C36 C31 P1 120.2(4) . . ? C33 C32 C31 120.9(6) . . ? C52 C51 C56 117.9(6) . . ? C52 C51 P2 118.4(5) . . ? C56 C51 P2 123.8(5) . . ? O71 C7 O72 124.6(6) . . ? O71 C7 C6 120.5(5) . . ? O72 C7 C6 114.8(5) . . ? C2 C3 C4 118.9(6) . . ? C65 C66 C61 120.8(7) . . ? C5 C4 C3 119.9(6) . . ? C35 C34 C33 119.8(6) . . ? C44 C45 C46 119.7(7) . . ? C64 C63 C62 121.0(7) . . ? C13 C12 C11 119.4(9) . . ? C44 C43 C42 120.3(7) . . ? C23 C24 C25 120.2(7) . . ? C51 C52 C53 121.4(6) . . ? C34 C33 C32 119.9(6) . . ? C43 C44 C45 121.0(7) . . ? C43 C42 C41 120.4(7) . . ? C55 C54 C53 119.5(7) . . ? C63 C64 C65 119.6(7) . . ? C26 C25 C24 119.7(7) . . ? C54 C53 C52 119.6(7) . . ? C11 C16 C15 120.4(8) . . ? C14 C13 C12 120.3(9) . . ? C54 C55 C56 121.0(7) . . ? C14 C15 C16 119.2(10) . . ? C64 C65 C66 120.3(7) . . ? C15 C14 C13 121.2(7) . . ? Cl4 C99 Cl3 115.3(11) . . ? Cl4 C99 Cl2 110.1(8) . . ? Cl3 C99 Cl2 106.0(7) . . ? _diffrn_measured_fraction_theta_max 0.848 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.848 _refine_diff_density_max 1.256 _refine_diff_density_min -1.087 _refine_diff_density_rms 0.113 #=END data_S2 #*complex 2* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 Cl4 N O3 P2 Pt' _chemical_formula_weight 1012.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.002(14) _cell_length_b 12.641(14) _cell_length_c 16.825(18) _cell_angle_alpha 112.240(10) _cell_angle_beta 93.520(10) _cell_angle_gamma 104.510(10) _cell_volume 2065(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 3.774 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7297 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.99 _reflns_number_total 7297 _reflns_number_gt 5985 _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 w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+10.3009P] 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_number_reflns 7297 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.37083(2) 0.49346(2) 0.166348(17) 0.03740(9) Uani 1 d . . . Cl Cl 0.33027(17) 0.50244(16) 0.03047(11) 0.0479(4) Uani 1 d . . . P1 P 0.42241(16) 0.49505(15) 0.29922(11) 0.0380(4) Uani 1 d . . . P2 P 0.24318(17) 0.30246(15) 0.09969(12) 0.0419(4) Uani 1 d . . . O71 O 0.2617(5) 0.6734(4) 0.2467(4) 0.0529(13) Uani 1 d . . . N1 N 0.5033(5) 0.6676(4) 0.2068(4) 0.0379(12) Uani 1 d . . . O72 O 0.3290(6) 0.8724(5) 0.3007(4) 0.0710(17) Uani 1 d . . . O25 O 0.5521(6) 0.9851(5) 0.3107(4) 0.0766(18) Uani 1 d . . . H25 H 0.4782 0.9736 0.3191 0.092 Uiso 1 calc R . . C21 C 0.2862(7) 0.4414(6) 0.3458(5) 0.0471(17) Uani 1 d . . . C11 C 0.5016(6) 0.6455(6) 0.3831(4) 0.0403(15) Uani 1 d . . . C31 C 0.5404(7) 0.4166(6) 0.3006(4) 0.0422(15) Uani 1 d . . . C6 C 0.4776(6) 0.7707(6) 0.2467(4) 0.0397(14) Uani 1 d . . . C26 C 0.1798(7) 0.4806(7) 0.3347(5) 0.0531(18) Uani 1 d . . . H26 H 0.1795 0.5251 0.3016 0.064 Uiso 1 calc R . . C12 C 0.6312(7) 0.6956(7) 0.3927(5) 0.0506(18) Uani 1 d . . . H12 H 0.6787 0.6509 0.3583 0.061 Uiso 1 calc R . . C2 C 0.6191(6) 0.6654(7) 0.1847(5) 0.0489(17) Uani 1 d . . . H2 H 0.6336 0.5921 0.1554 0.059 Uiso 1 calc R . . C51 C 0.3149(7) 0.2054(6) 0.0191(5) 0.0486(17) Uani 1 d . . . C52 C 0.4309(7) 0.2515(7) -0.0029(5) 0.0541(19) Uani 1 d . . . H52 H 0.4676 0.3339 0.0181 0.065 Uiso 1 calc R . . C22 C 0.2848(8) 0.3715(7) 0.3925(5) 0.060(2) Uani 1 d . . . H22 H 0.3537 0.3433 0.3984 0.072 Uiso 1 calc R . . C16 C 0.4326(7) 0.7150(7) 0.4335(5) 0.0548(19) Uani 1 d . . . H16 H 0.3448 0.6836 0.4270 0.066 Uiso 1 calc R . . C7 C 0.3452(7) 0.7704(6) 0.2655(5) 0.0465(16) Uani 1 d . . . C36 C 0.5895(8) 0.3701(7) 0.2252(5) 0.059(2) Uani 1 d . . . H36 H 0.5590 0.3764 0.1749 0.071 Uiso 1 calc R . . C61 C 0.0936(7) 0.3008(7) 0.0462(6) 0.058(2) Uani 1 d . . . C41 C 0.1970(9) 0.2120(6) 0.1613(5) 0.060(2) Uani 1 d . . . C5 C 0.5743(8) 0.8802(7) 0.2706(5) 0.0532(18) Uani 1 d . . . C13 C 0.6916(8) 0.8113(7) 0.4525(6) 0.062(2) Uani 1 d . . . H13 H 0.7791 0.8436 0.4579 0.074 Uiso 1 calc R . . C3 C 0.7164(7) 0.7697(8) 0.2048(6) 0.060(2) Uani 1 d . . . H3 H 0.7949 0.7671 0.1879 0.073 Uiso 1 calc R . . C25 C 0.0758(8) 0.4528(8) 0.3731(6) 0.067(2) Uani 1 d . . . H25 H 0.0055 0.4788 0.3663 0.081 Uiso 1 calc R . . C33 C 0.6836(10) 0.3538(10) 0.3741(8) 0.086(3) Uani 1 d . . . H33 H 0.7151 0.3476 0.4242 0.103 Uiso 1 calc R . . C4 C 0.6949(8) 0.8783(7) 0.2504(6) 0.064(2) Uani 1 d . . . H4 H 0.7604 0.9494 0.2674 0.076 Uiso 1 calc R . . C42 C 0.0756(12) 0.1861(9) 0.1803(7) 0.092(4) Uani 1 d . . . H42 H 0.0154 0.2179 0.1643 0.110 Uiso 1 calc R . . C15 C 0.4935(8) 0.8310(7) 0.4938(6) 0.066(2) Uani 1 d . . . H15 H 0.4463 0.8767 0.5275 0.080 Uiso 1 calc R . . C32 C 0.5922(8) 0.4115(8) 0.3761(6) 0.065(2) Uani 1 d . . . H32 H 0.5650 0.4473 0.4283 0.078 Uiso 1 calc R . . C14 C 0.6234(9) 0.8788(7) 0.5039(6) 0.069(2) Uani 1 d . . . H14 H 0.6643 0.9559 0.5452 0.083 Uiso 1 calc R . . C66 C 0.0441(8) 0.3937(8) 0.0884(6) 0.071(3) Uani 1 d . . . H66 H 0.0850 0.4525 0.1431 0.086 Uiso 1 calc R . . C35 C 0.6842(10) 0.3139(9) 0.2238(7) 0.081(3) Uani 1 d . . . H35 H 0.7169 0.2828 0.1731 0.097 Uiso 1 calc R . . C53 C 0.4910(10) 0.1745(9) -0.0559(6) 0.075(3) Uani 1 d . . . H53 H 0.5688 0.2053 -0.0698 0.090 Uiso 1 calc R . . C65 C -0.0680(9) 0.3979(10) 0.0477(8) 0.088(3) Uani 1 d . . . H65 H -0.1034 0.4585 0.0765 0.106 Uiso 1 calc R . . C54 C 0.4360(11) 0.0522(10) -0.0882(7) 0.085(3) Uani 1 d . . . H54 H 0.4775 0.0009 -0.1229 0.102 Uiso 1 calc R . . C56 C 0.2591(9) 0.0809(7) -0.0157(6) 0.068(2) Uani 1 d . . . H56 H 0.1810 0.0489 -0.0027 0.081 Uiso 1 calc R . . C23 C 0.1788(9) 0.3439(9) 0.4308(6) 0.075(3) Uani 1 d . . . H23 H 0.1769 0.2972 0.4624 0.089 Uiso 1 calc R . . C24 C 0.0772(9) 0.3859(9) 0.4216(6) 0.078(3) Uani 1 d . . . H24 H 0.0081 0.3690 0.4486 0.094 Uiso 1 calc R . . C46 C 0.2865(11) 0.1637(7) 0.1866(6) 0.079(3) Uani 1 d . . . H46 H 0.3677 0.1802 0.1728 0.095 Uiso 1 calc R . . C34 C 0.7281(10) 0.3054(9) 0.2982(9) 0.091(3) Uani 1 d . . . H34 H 0.7893 0.2661 0.2974 0.109 Uiso 1 calc R . . C55 C 0.3202(11) 0.0062(8) -0.0691(6) 0.080(3) Uani 1 d . . . H55 H 0.2825 -0.0762 -0.0925 0.095 Uiso 1 calc R . . C62 C 0.0322(10) 0.2137(9) -0.0344(8) 0.098(4) Uani 1 d . . . H62 H 0.0628 0.1491 -0.0620 0.117 Uiso 1 calc R . . C64 C -0.1268(11) 0.3133(11) -0.0346(10) 0.130(6) Uani 1 d . . . H64 H -0.1998 0.3186 -0.0619 0.156 Uiso 1 calc R . . C63 C -0.0790(12) 0.2241(11) -0.0747(11) 0.151(7) Uani 1 d . . . H63 H -0.1190 0.1676 -0.1303 0.181 Uiso 1 calc R . . C43 C 0.0449(18) 0.1108(12) 0.2242(10) 0.139(7) Uani 1 d . . . H43 H -0.0376 0.0897 0.2351 0.167 Uiso 1 calc R . . C45 C 0.256(2) 0.0920(10) 0.2316(9) 0.133(6) Uani 1 d . . . H45 H 0.3162 0.0608 0.2482 0.160 Uiso 1 calc R . . C44 C 0.136(3) 0.0673(14) 0.2516(11) 0.176(12) Uani 1 d . . . H44 H 0.1151 0.0213 0.2836 0.211 Uiso 1 calc R . . C99 C 0.0678(10) 0.7883(10) 0.3692(8) 0.092(3) Uani 1 d . . . H99 H 0.1374 0.7895 0.3356 0.110 Uiso 1 calc R . . Cl2 Cl 0.1264(4) 0.7986(4) 0.4714(3) 0.1314(13) Uani 1 d . . . Cl3 Cl -0.0555(3) 0.6550(3) 0.3119(4) 0.1452(16) Uani 1 d . . . Cl4 Cl 0.0141(3) 0.9121(3) 0.3822(3) 0.1176(12) Uani 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 Pt 0.03734(14) 0.03686(14) 0.03729(15) 0.01447(10) 0.00653(9) 0.01080(10) Cl 0.0503(10) 0.0551(10) 0.0405(9) 0.0217(8) 0.0068(7) 0.0163(8) P1 0.0364(9) 0.0384(9) 0.0362(9) 0.0118(7) 0.0063(7) 0.0118(7) P2 0.0402(9) 0.0343(9) 0.0454(10) 0.0129(7) 0.0040(7) 0.0074(7) O71 0.049(3) 0.052(3) 0.067(3) 0.031(3) 0.016(2) 0.019(2) N1 0.032(3) 0.035(3) 0.045(3) 0.017(2) 0.005(2) 0.006(2) O72 0.080(4) 0.049(3) 0.087(4) 0.021(3) 0.028(3) 0.032(3) O25 0.092(5) 0.037(3) 0.088(5) 0.015(3) 0.028(4) 0.012(3) C21 0.053(4) 0.041(4) 0.044(4) 0.018(3) 0.013(3) 0.007(3) C11 0.043(4) 0.044(4) 0.032(3) 0.015(3) 0.004(3) 0.013(3) C31 0.050(4) 0.045(4) 0.037(4) 0.021(3) -0.001(3) 0.018(3) C6 0.045(4) 0.038(3) 0.037(4) 0.016(3) 0.009(3) 0.015(3) C26 0.046(4) 0.053(4) 0.064(5) 0.028(4) 0.016(4) 0.012(3) C12 0.044(4) 0.058(4) 0.047(4) 0.019(4) 0.011(3) 0.014(3) C2 0.041(4) 0.054(4) 0.054(4) 0.020(3) 0.018(3) 0.018(3) C51 0.057(4) 0.041(4) 0.046(4) 0.013(3) 0.005(3) 0.021(3) C52 0.060(5) 0.058(5) 0.049(4) 0.021(4) 0.011(4) 0.026(4) C22 0.058(5) 0.070(5) 0.063(5) 0.040(4) 0.009(4) 0.014(4) C16 0.046(4) 0.052(4) 0.051(4) 0.006(4) 0.006(3) 0.011(3) C7 0.052(4) 0.041(4) 0.049(4) 0.019(3) 0.011(3) 0.017(3) C36 0.062(5) 0.058(5) 0.054(5) 0.015(4) 0.010(4) 0.026(4) C61 0.038(4) 0.045(4) 0.079(6) 0.018(4) -0.005(4) 0.007(3) C41 0.079(6) 0.037(4) 0.047(4) 0.007(3) 0.012(4) 0.003(4) C5 0.064(5) 0.046(4) 0.044(4) 0.017(3) 0.008(4) 0.010(4) C13 0.044(4) 0.057(5) 0.069(5) 0.018(4) 0.002(4) 0.002(4) C3 0.041(4) 0.069(5) 0.066(5) 0.027(4) 0.014(4) 0.009(4) C25 0.047(5) 0.088(6) 0.070(6) 0.036(5) 0.021(4) 0.016(4) C33 0.075(7) 0.104(8) 0.094(8) 0.052(7) -0.003(6) 0.039(6) C4 0.048(4) 0.056(5) 0.076(6) 0.029(4) 0.005(4) -0.005(4) C42 0.112(9) 0.068(6) 0.070(6) 0.021(5) 0.030(6) -0.009(6) C15 0.061(5) 0.052(5) 0.063(5) 0.000(4) 0.015(4) 0.016(4) C32 0.060(5) 0.072(6) 0.067(6) 0.027(5) 0.010(4) 0.027(4) C14 0.073(6) 0.040(4) 0.064(5) 0.001(4) 0.000(4) 0.002(4) C66 0.051(5) 0.071(6) 0.077(6) 0.013(5) 0.004(4) 0.023(4) C35 0.081(7) 0.076(6) 0.079(7) 0.013(5) 0.012(5) 0.041(5) C53 0.080(6) 0.093(7) 0.068(6) 0.033(5) 0.025(5) 0.052(6) C65 0.056(5) 0.087(7) 0.121(9) 0.037(7) 0.002(6) 0.032(5) C54 0.115(9) 0.082(7) 0.068(6) 0.016(5) 0.026(6) 0.067(7) C56 0.080(6) 0.045(4) 0.069(6) 0.012(4) 0.011(5) 0.022(4) C23 0.075(6) 0.092(7) 0.080(6) 0.066(6) 0.025(5) 0.012(5) C24 0.065(6) 0.089(7) 0.069(6) 0.028(5) 0.032(5) 0.004(5) C46 0.122(8) 0.044(5) 0.069(6) 0.030(4) 0.005(6) 0.011(5) C34 0.078(7) 0.085(7) 0.116(10) 0.030(7) 0.005(6) 0.053(6) C55 0.118(9) 0.052(5) 0.065(6) 0.014(4) 0.014(6) 0.036(6) C62 0.074(6) 0.065(6) 0.114(9) -0.002(6) -0.035(6) 0.027(5) C64 0.077(8) 0.093(9) 0.167(14) 0.001(9) -0.052(8) 0.037(7) C63 0.098(9) 0.086(8) 0.182(15) -0.019(9) -0.086(10) 0.025(7) C43 0.183(16) 0.090(10) 0.109(12) 0.046(8) 0.060(12) -0.036(10) C45 0.24(2) 0.057(7) 0.099(10) 0.038(7) 0.014(12) 0.039(10) C44 0.34(3) 0.084(10) 0.083(10) 0.059(8) 0.033(16) -0.015(14) C99 0.070(6) 0.112(9) 0.123(10) 0.071(8) 0.040(6) 0.035(6) Cl2 0.128(3) 0.168(4) 0.156(4) 0.108(3) 0.052(3) 0.067(3) Cl3 0.087(2) 0.113(3) 0.238(5) 0.070(3) 0.017(3) 0.039(2) Cl4 0.105(2) 0.117(2) 0.176(4) 0.095(3) 0.054(2) 0.0459(19) _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 Pt N1 2.137(5) . ? Pt P2 2.262(3) . ? Pt P1 2.264(3) . ? Pt Cl 2.353(3) . ? P1 C31 1.824(7) . ? P1 C11 1.831(7) . ? P1 C21 1.832(7) . ? P2 C61 1.817(8) . ? P2 C41 1.819(9) . ? P2 C51 1.823(7) . ? O71 C7 1.246(8) . ? N1 C6 1.332(8) . ? N1 C2 1.353(8) . ? O72 C7 1.263(8) . ? O25 C5 1.334(9) . ? C21 C22 1.385(11) . ? C21 C26 1.410(11) . ? C11 C12 1.380(10) . ? C11 C16 1.384(9) . ? C31 C36 1.388(10) . ? C31 C32 1.391(11) . ? C6 C5 1.413(10) . ? C6 C7 1.510(10) . ? C26 C25 1.382(10) . ? C12 C13 1.382(10) . ? C2 C3 1.382(10) . ? C51 C52 1.398(11) . ? C51 C56 1.403(11) . ? C52 C53 1.386(11) . ? C22 C23 1.398(11) . ? C16 C15 1.388(10) . ? C36 C35 1.397(12) . ? C61 C62 1.376(12) . ? C61 C66 1.385(11) . ? C41 C42 1.381(13) . ? C41 C46 1.404(13) . ? C5 C4 1.393(11) . ? C13 C14 1.372(11) . ? C3 C4 1.384(12) . ? C25 C24 1.381(13) . ? C33 C34 1.371(15) . ? C33 C32 1.378(13) . ? C42 C43 1.403(17) . ? C15 C14 1.376(12) . ? C66 C65 1.396(13) . ? C35 C34 1.365(15) . ? C53 C54 1.381(14) . ? C65 C64 1.379(16) . ? C54 C55 1.373(15) . ? C56 C55 1.379(12) . ? C23 C24 1.376(14) . ? C46 C45 1.380(16) . ? C62 C63 1.422(14) . ? C64 C63 1.330(16) . ? C43 C44 1.39(3) . ? C45 C44 1.37(3) . ? C99 Cl2 1.744(13) . ? C99 Cl4 1.751(11) . ? C99 Cl3 1.753(12) . ? 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 Pt P2 169.41(15) . . ? N1 Pt P1 90.23(16) . . ? P2 Pt P1 98.07(8) . . ? N1 Pt Cl 86.04(16) . . ? P2 Pt Cl 85.50(8) . . ? P1 Pt Cl 176.08(6) . . ? C31 P1 C11 102.5(3) . . ? C31 P1 C21 110.4(3) . . ? C11 P1 C21 102.8(3) . . ? C31 P1 Pt 112.2(2) . . ? C11 P1 Pt 113.1(2) . . ? C21 P1 Pt 114.8(3) . . ? C61 P2 C41 104.9(4) . . ? C61 P2 C51 108.9(4) . . ? C41 P2 C51 99.2(4) . . ? C61 P2 Pt 109.1(3) . . ? C41 P2 Pt 121.0(3) . . ? C51 P2 Pt 112.8(3) . . ? C6 N1 C2 121.1(6) . . ? C6 N1 Pt 125.4(4) . . ? C2 N1 Pt 113.4(4) . . ? C22 C21 C26 120.0(7) . . ? C22 C21 P1 124.6(6) . . ? C26 C21 P1 115.3(6) . . ? C12 C11 C16 118.3(6) . . ? C12 C11 P1 120.2(5) . . ? C16 C11 P1 121.3(5) . . ? C36 C31 C32 118.4(7) . . ? C36 C31 P1 118.6(6) . . ? C32 C31 P1 122.7(6) . . ? N1 C6 C5 119.9(6) . . ? N1 C6 C7 120.0(6) . . ? C5 C6 C7 120.1(6) . . ? C25 C26 C21 119.9(8) . . ? C11 C12 C13 121.0(7) . . ? N1 C2 C3 121.5(7) . . ? C52 C51 C56 119.0(7) . . ? C52 C51 P2 121.2(5) . . ? C56 C51 P2 119.5(6) . . ? C53 C52 C51 119.9(8) . . ? C21 C22 C23 119.4(8) . . ? C11 C16 C15 120.5(7) . . ? O71 C7 O72 125.0(7) . . ? O71 C7 C6 119.7(6) . . ? O72 C7 C6 115.3(6) . . ? C31 C36 C35 120.9(9) . . ? C62 C61 C66 120.2(8) . . ? C62 C61 P2 122.3(7) . . ? C66 C61 P2 117.5(6) . . ? C42 C41 C46 119.7(9) . . ? C42 C41 P2 121.8(8) . . ? C46 C41 P2 118.5(7) . . ? O25 C5 C4 119.4(7) . . ? O25 C5 C6 121.5(7) . . ? C4 C5 C6 119.1(7) . . ? C14 C13 C12 120.4(7) . . ? C2 C3 C4 118.8(7) . . ? C24 C25 C26 119.4(9) . . ? C34 C33 C32 120.0(10) . . ? C3 C4 C5 119.5(7) . . ? C41 C42 C43 118.6(14) . . ? C14 C15 C16 120.5(7) . . ? C33 C32 C31 120.4(9) . . ? C13 C14 C15 119.2(7) . . ? C61 C66 C65 119.0(9) . . ? C34 C35 C36 118.8(9) . . ? C54 C53 C52 120.3(9) . . ? C64 C65 C66 120.9(10) . . ? C55 C54 C53 120.1(8) . . ? C55 C56 C51 119.9(9) . . ? C24 C23 C22 119.9(9) . . ? C23 C24 C25 121.4(8) . . ? C45 C46 C41 121.1(13) . . ? C35 C34 C33 121.3(9) . . ? C54 C55 C56 120.7(9) . . ? C61 C62 C63 118.8(10) . . ? C63 C64 C65 119.8(10) . . ? C64 C63 C62 121.3(11) . . ? C44 C43 C42 121.1(15) . . ? C44 C45 C46 119.3(16) . . ? C45 C44 C43 120.2(13) . . ? Cl2 C99 Cl4 109.3(7) . . ? Cl2 C99 Cl3 111.3(6) . . ? Cl4 C99 Cl3 110.4(6) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 3.441 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.123 #=END data_S3 #*complex 3* _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H19 I2 N O4 P Re' _chemical_formula_weight 856.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.116(9) _cell_length_b 15.241(17) _cell_length_c 21.061(24) _cell_angle_alpha 90.00 _cell_angle_beta 100.170(10) _cell_angle_gamma 90.00 _cell_volume 2564(5) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 7.239 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7366 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4188 _reflns_number_gt 3271 _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 w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+10.8735P] 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_number_reflns 4188 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.28287(4) 0.35153(2) 0.162289(16) 0.03333(14) Uani 1 d . . . I1 I 0.58048(9) 0.37406(5) 0.23764(4) 0.0558(2) Uani 1 d . . . I2 I 0.38835(10) 0.44682(6) 0.06689(4) 0.0656(3) Uani 1 d . . . P1 P 0.2102(3) 0.23836(14) 0.23888(10) 0.0297(5) Uani 1 d . . . C11 C 0.3814(11) 0.1703(6) 0.2807(4) 0.0334(19) Uani 1 d . . . C12 C 0.4000(14) 0.1565(7) 0.3461(5) 0.051(3) Uani 1 d . . . H12 H 0.3223 0.1798 0.3691 0.061 Uiso 1 calc R . . C13 C 0.5364(17) 0.1073(8) 0.3786(6) 0.066(3) Uani 1 d . . . H13 H 0.5495 0.0985 0.4229 0.079 Uiso 1 calc R . . C14 C 0.6477(14) 0.0732(7) 0.3448(6) 0.055(3) Uani 1 d . . . H14 H 0.7385 0.0413 0.3663 0.066 Uiso 1 calc R . . C15 C 0.6293(14) 0.0846(8) 0.2799(6) 0.059(3) Uani 1 d . . . H15 H 0.7063 0.0598 0.2572 0.071 Uiso 1 calc R . . C16 C 0.4964(14) 0.1331(7) 0.2473(6) 0.053(3) Uani 1 d . . . H16 H 0.4843 0.1408 0.2029 0.063 Uiso 1 calc R . . C21 C 0.1116(11) 0.2859(6) 0.3015(4) 0.0340(19) Uani 1 d . . . C22 C -0.0072(13) 0.2393(7) 0.3295(5) 0.048(2) Uani 1 d . . . H22 H -0.0370 0.1826 0.3157 0.058 Uiso 1 calc R . . C26 C 0.1554(15) 0.3699(7) 0.3256(5) 0.048(2) Uani 1 d . . . H26 H 0.2372 0.4016 0.3097 0.058 Uiso 1 calc R . . C23 C -0.0790(13) 0.2766(10) 0.3770(5) 0.063(3) Uani 1 d . . . H23 H -0.1580 0.2449 0.3945 0.076 Uiso 1 calc R . . C24 C -0.0376(16) 0.3597(8) 0.3994(6) 0.061(3) Uani 1 d . . . H24 H -0.0871 0.3839 0.4320 0.074 Uiso 1 calc R . . C25 C 0.0773(17) 0.4063(9) 0.3731(6) 0.066(3) Uani 1 d . . . H25 H 0.1039 0.4632 0.3872 0.079 Uiso 1 calc R . . C31 C 0.0555(11) 0.1658(6) 0.1953(4) 0.0346(19) Uani 1 d . . . C32 C 0.0947(14) 0.0829(7) 0.1737(5) 0.052(3) Uani 1 d . . . H32 H 0.2017 0.0605 0.1873 0.062 Uiso 1 calc R . . C33 C -0.0212(18) 0.0329(7) 0.1325(5) 0.065(3) Uani 1 d . . . H33 H 0.0052 -0.0230 0.1197 0.078 Uiso 1 calc R . . C34 C -0.1768(17) 0.0693(9) 0.1112(5) 0.067(4) Uani 1 d . . . H34 H -0.2529 0.0382 0.0813 0.081 Uiso 1 calc R . . C35 C -0.2246(14) 0.1489(8) 0.1321(5) 0.052(3) Uani 1 d . . . H35 H -0.3326 0.1700 0.1186 0.063 Uiso 1 calc R . . C36 C -0.1089(11) 0.1967(6) 0.1734(4) 0.039(2) Uani 1 d . . . H36 H -0.1396 0.2512 0.1874 0.047 Uiso 1 calc R . . N1 N 0.0769(9) 0.3134(5) 0.0879(3) 0.0377(17) Uani 1 d . . . C2 C -0.0677(14) 0.3564(7) 0.0745(5) 0.052(3) Uani 1 d . . . H2 H -0.0866 0.4061 0.0978 0.063 Uiso 1 calc R . . C3 C -0.1916(15) 0.3251(8) 0.0242(6) 0.062(3) Uani 1 d . . . H3 H -0.2918 0.3558 0.0138 0.075 Uiso 1 calc R . . C4 C -0.1689(14) 0.2510(9) -0.0096(5) 0.062(3) Uani 1 d . . . H4 H -0.2536 0.2297 -0.0414 0.074 Uiso 1 calc R . . C5 C -0.0191(15) 0.2091(8) 0.0045(5) 0.057(3) Uani 1 d . . . C6 C 0.1046(12) 0.2407(6) 0.0532(4) 0.040(2) Uani 1 d . . . C7 C 0.2706(12) 0.1991(7) 0.0732(4) 0.041(2) Uani 1 d . . . O72 O 0.3116(11) 0.1339(5) 0.0452(4) 0.064(2) Uani 1 d . . . O71 O 0.3643(8) 0.2396(4) 0.1210(3) 0.0401(15) Uani 1 d . . . O25 O 0.0116(15) 0.1347(8) -0.0280(5) 0.089(3) Uani 1 d . . . H25 H 0.09(2) 0.109(12) -0.009(8) 0.107 Uiso 1 d . . . O1 O 0.1584(9) 0.4257(4) 0.1880(3) 0.0480(17) Uani 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 Re 0.0347(3) 0.0329(2) 0.0325(2) 0.00092(14) 0.00598(14) 0.00063(13) I1 0.0444(5) 0.0582(5) 0.0607(5) -0.0036(3) -0.0021(3) -0.0106(3) I2 0.0683(6) 0.0714(5) 0.0603(5) 0.0237(4) 0.0202(4) -0.0091(4) P1 0.0297(12) 0.0290(11) 0.0293(11) -0.0012(8) 0.0024(8) 0.0010(8) C11 0.037(5) 0.024(4) 0.036(5) 0.002(3) -0.002(3) 0.002(3) C12 0.059(7) 0.055(7) 0.034(5) 0.002(5) -0.003(4) 0.016(5) C13 0.078(9) 0.059(8) 0.054(7) 0.017(6) -0.007(6) 0.008(6) C14 0.040(7) 0.046(6) 0.073(8) 0.017(5) -0.004(5) 0.001(5) C15 0.039(7) 0.059(7) 0.079(8) 0.018(6) 0.011(5) 0.017(5) C16 0.051(7) 0.056(7) 0.052(6) 0.018(5) 0.013(5) 0.014(5) C21 0.042(5) 0.033(5) 0.027(4) -0.002(3) 0.005(3) 0.001(4) C22 0.050(6) 0.060(7) 0.039(5) -0.011(5) 0.019(4) -0.013(5) C26 0.068(7) 0.040(6) 0.036(5) -0.001(4) 0.009(5) 0.001(5) C23 0.033(7) 0.110(11) 0.051(6) 0.005(7) 0.019(5) -0.006(6) C24 0.067(8) 0.075(9) 0.044(6) -0.011(6) 0.015(5) 0.023(6) C25 0.086(10) 0.063(8) 0.053(7) -0.009(6) 0.025(6) 0.014(6) C31 0.027(5) 0.043(5) 0.034(5) 0.000(4) 0.004(3) -0.005(4) C32 0.057(7) 0.045(6) 0.050(6) -0.005(5) 0.001(5) -0.007(5) C33 0.104(11) 0.030(6) 0.052(7) -0.006(5) -0.009(6) -0.008(6) C34 0.078(9) 0.074(9) 0.043(6) 0.001(6) -0.008(5) -0.034(7) C35 0.039(6) 0.080(9) 0.038(6) 0.004(5) 0.008(4) -0.014(5) C36 0.039(6) 0.038(5) 0.042(5) -0.005(4) 0.010(4) 0.004(4) N1 0.035(4) 0.041(4) 0.035(4) 0.008(3) 0.001(3) 0.005(3) C2 0.056(7) 0.051(7) 0.051(6) 0.028(5) 0.013(5) 0.021(5) C3 0.050(8) 0.065(8) 0.062(7) 0.015(6) -0.015(5) 0.005(6) C4 0.050(8) 0.087(9) 0.041(6) 0.015(6) -0.016(5) -0.013(6) C5 0.064(8) 0.079(8) 0.029(5) -0.013(5) 0.005(4) -0.010(6) C6 0.044(6) 0.046(6) 0.028(5) 0.004(4) 0.005(4) -0.001(4) C7 0.043(6) 0.054(6) 0.028(5) -0.005(4) 0.011(4) 0.000(4) O72 0.066(6) 0.070(6) 0.056(5) -0.023(4) 0.017(4) 0.011(4) O71 0.047(4) 0.046(4) 0.030(3) 0.001(3) 0.015(3) 0.004(3) O25 0.095(9) 0.107(9) 0.059(6) -0.039(6) -0.005(5) -0.004(6) O1 0.057(5) 0.036(4) 0.051(4) -0.003(3) 0.010(3) 0.011(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 Re O1 1.669(6) . ? Re O71 2.074(6) . ? Re N1 2.159(8) . ? Re P1 2.502(3) . ? Re I1 2.668(2) . ? Re I2 2.736(2) . ? P1 C31 1.799(9) . ? P1 C21 1.810(9) . ? P1 C11 1.831(9) . ? C11 C12 1.375(13) . ? C11 C16 1.385(14) . ? C12 C13 1.410(15) . ? C12 H12 0.9300 . ? C13 C14 1.349(17) . ? C13 H13 0.9300 . ? C14 C15 1.361(16) . ? C14 H14 0.9300 . ? C15 C16 1.386(14) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C26 1.400(13) . ? C21 C22 1.409(13) . ? C22 C23 1.366(14) . ? C22 H22 0.9300 . ? C26 C25 1.390(15) . ? C26 H26 0.9300 . ? C23 C24 1.373(17) . ? C23 H23 0.9300 . ? C24 C25 1.365(18) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 C32 1.399(14) . ? C31 C36 1.413(13) . ? C32 C33 1.389(15) . ? C32 H32 0.9300 . ? C33 C34 1.380(18) . ? C33 H33 0.9300 . ? C34 C35 1.371(17) . ? C34 H34 0.9300 . ? C35 C36 1.371(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N1 C2 1.331(13) . ? N1 C6 1.368(12) . ? C2 C3 1.408(16) . ? C2 H2 0.9300 . ? C3 C4 1.365(17) . ? C3 H3 0.9300 . ? C4 C5 1.358(17) . ? C4 H4 0.9300 . ? C5 O25 1.370(15) . ? C5 C6 1.389(14) . ? C6 C7 1.481(14) . ? C7 O72 1.232(11) . ? C7 O71 1.305(11) . ? O25 H25 0.78(17) . ? 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 O1 Re O71 161.6(3) . . ? O1 Re N1 89.0(3) . . ? O71 Re N1 74.8(3) . . ? O1 Re P1 91.9(3) . . ? O71 Re P1 80.34(19) . . ? N1 Re P1 92.4(2) . . ? O1 Re I1 104.8(3) . . ? O71 Re I1 91.89(19) . . ? N1 Re I1 165.9(2) . . ? P1 Re I1 89.82(8) . . ? O1 Re I2 99.5(2) . . ? O71 Re I2 87.97(18) . . ? N1 Re I2 85.0(2) . . ? P1 Re I2 168.29(6) . . ? I1 Re I2 90.04(7) . . ? C31 P1 C21 105.0(4) . . ? C31 P1 C11 107.4(4) . . ? C21 P1 C11 105.8(4) . . ? C31 P1 Re 108.5(3) . . ? C21 P1 Re 112.2(3) . . ? C11 P1 Re 117.1(3) . . ? C12 C11 C16 118.8(9) . . ? C12 C11 P1 120.5(7) . . ? C16 C11 P1 120.6(7) . . ? C11 C12 C13 120.3(10) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.4(11) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.0(10) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 120.3(11) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.1(10) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C26 C21 C22 117.3(8) . . ? C26 C21 P1 120.9(7) . . ? C22 C21 P1 121.8(7) . . ? C23 C22 C21 120.6(10) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C25 C26 C21 120.4(11) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C22 C23 C24 121.7(11) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 118.9(10) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 121.1(12) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C32 C31 C36 116.8(8) . . ? C32 C31 P1 122.9(7) . . ? C36 C31 P1 119.7(7) . . ? C33 C32 C31 122.1(11) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C34 C33 C32 117.5(11) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 121.2 . . ? C35 C34 C33 123.1(10) . . ? C35 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? C34 C35 C36 118.3(11) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C35 C36 C31 122.1(9) . . ? C35 C36 H36 119.0 . . ? C31 C36 H36 119.0 . . ? C2 N1 C6 120.5(9) . . ? C2 N1 Re 124.2(7) . . ? C6 N1 Re 115.2(6) . . ? N1 C2 C3 118.6(11) . . ? N1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 121.9(11) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C5 C4 C3 118.2(10) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 O25 120.9(10) . . ? C4 C5 C6 120.1(11) . . ? O25 C5 C6 119.0(11) . . ? N1 C6 C5 120.6(9) . . ? N1 C6 C7 115.0(8) . . ? C5 C6 C7 124.4(10) . . ? O72 C7 O71 125.6(9) . . ? O72 C7 C6 121.2(9) . . ? O71 C7 C6 113.2(8) . . ? C7 O71 Re 121.8(6) . . ? C5 O25 H25 110(10) . . ? _diffrn_measured_fraction_theta_max 0.807 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.807 _refine_diff_density_max 1.683 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.183