data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H58 P2 Pt' _chemical_formula_weight 867.95 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' 'P' 'P' 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.515(2) _cell_length_b 25.187(3) _cell_length_c 14.685(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4628.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.7 _cell_measurement_theta_max 12.4 _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 3.127 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details ? _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 'Nonius CAD-4 serial diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4199 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.1133 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4064 _reflns_number_gt 1675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4/PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'CAD4/PC (Enraf-Nonius, 1993)' _computing_data_reduction 'TEXSAN (Molecular Structure Corp., 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'SHELXTL' _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^)+(0.0855P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4064 _refine_ls_number_parameters 191 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1806 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2185 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.49709(7) 0.2500 0.7500 0.0567(3) Uani 1 2 d S . . P1 P 0.4849(4) 0.3172(2) 0.8547(3) 0.0775(13) Uani 1 1 d D . . C1 C 0.5101(11) 0.1957(5) 0.8488(11) 0.060(4) Uani 1 1 d . . . C2 C 0.5334(10) 0.1667(6) 0.9094(10) 0.051(4) Uani 1 1 d . . . C3 C 0.5807(11) 0.1377(5) 0.9835(8) 0.045(3) Uani 1 1 d . . . C4 C 0.5184(11) 0.1055(5) 1.0409(9) 0.055(4) Uani 1 1 d . . . H4 H 0.4455 0.1025 1.0298 0.066 Uiso 1 1 calc R . . C5 C 0.5619(13) 0.0785(6) 1.1125(12) 0.067(4) Uani 1 1 d . . . C6 C 0.6709(14) 0.0872(7) 1.1314(13) 0.091(6) Uani 1 1 d . . . H6 H 0.7017 0.0712 1.1820 0.109 Uiso 1 1 calc R . . C7 C 0.7311(13) 0.1182(9) 1.0775(13) 0.108(8) Uani 1 1 d . . . H7 H 0.8029 0.1229 1.0919 0.129 Uiso 1 1 calc R . . C8 C 0.6905(12) 0.1433(6) 1.0017(11) 0.070(5) Uani 1 1 d . . . C9 C 0.7598(13) 0.1747(7) 0.9423(10) 0.069(5) Uani 1 1 d . . . C10 C 0.8091(11) 0.1960(7) 0.8886(10) 0.065(5) Uani 1 1 d . . . c12 C 0.8150(14) 0.2500 0.7500 0.058(5) Uani 1 2 d S . . H11 H 0.7407 0.2500 0.7500 0.069 Uiso 1 2 calc SR . . c11 C 0.8679(11) 0.2238(6) 0.8205(10) 0.056(4) Uani 1 1 d . . . C13 C 0.9792(11) 0.2232(6) 0.8179(11) 0.064(4) Uani 1 1 d . . . H13 H 1.0175 0.2047 0.8620 0.077 Uiso 1 1 calc R . . C14 C 1.0319(15) 0.2500 0.7500 0.072(7) Uani 1 2 d S . . H14 H 1.1062 0.2500 0.7500 0.086 Uiso 1 2 calc SR . . C15 C 0.4911(17) 0.0425(6) 1.1757(12) 0.089(6) Uani 1 1 d . . . C16 C 0.378(3) 0.0305(14) 1.130(2) 0.084(10) Uiso 0.50 1 d P . . C17 C 0.479(3) 0.0679(14) 1.272(2) 0.083(11) Uiso 0.50 1 d P . . C18 C 0.547(3) -0.0127(13) 1.187(2) 0.074(10) Uiso 0.50 1 d P . . C16B C 0.383(5) 0.073(2) 1.209(4) 0.17(2) Uiso 0.50 1 d P . . C17B C 0.555(4) 0.0225(18) 1.269(3) 0.117(15) Uiso 0.50 1 d P . . C18B C 0.471(4) -0.0100(18) 1.132(3) 0.118(15) Uiso 0.50 1 d P . . C19 C 0.558(2) 0.3794(11) 0.824(3) 0.252(17) Uiso 1 1 d D . . C20 C 0.6809(19) 0.3667(10) 0.846(2) 0.177(11) Uiso 1 1 d D . . C21 C 0.357(2) 0.3548(11) 0.832(2) 0.242(16) Uiso 1 1 d D . . C22 C 0.267(2) 0.3107(15) 0.865(3) 0.30(2) Uiso 1 1 d D . . C23 C 0.495(2) 0.2942(10) 0.9748(15) 0.156(10) Uiso 1 1 d D . . C24 C 0.483(2) 0.3462(10) 1.0380(15) 0.163(11) Uiso 1 1 d 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 Pt1 0.0436(4) 0.0711(5) 0.0556(4) 0.0141(5) 0.000 0.000 P1 0.085(3) 0.086(3) 0.062(2) -0.005(2) 0.002(3) 0.012(3) C1 0.050(9) 0.047(8) 0.084(10) 0.015(7) 0.023(10) -0.004(8) C2 0.047(8) 0.061(9) 0.046(8) 0.001(7) 0.019(7) -0.007(7) C3 0.060(9) 0.043(7) 0.032(8) -0.003(6) 0.011(7) -0.004(7) C4 0.052(10) 0.056(8) 0.057(8) 0.004(7) 0.004(8) 0.007(8) C5 0.074(11) 0.051(9) 0.075(12) 0.005(8) 0.017(10) 0.012(8) C6 0.072(12) 0.117(16) 0.084(14) 0.054(12) -0.005(11) -0.001(11) C7 0.047(10) 0.17(2) 0.108(16) 0.075(16) -0.002(11) -0.013(12) C8 0.054(10) 0.088(12) 0.067(11) 0.029(10) 0.003(9) -0.003(9) C9 0.060(10) 0.099(13) 0.048(9) 0.025(10) -0.004(8) 0.015(10) C10 0.044(8) 0.106(14) 0.046(9) 0.026(9) -0.003(8) -0.001(9) c12 0.036(9) 0.086(14) 0.051(11) 0.016(13) 0.000 0.000 c11 0.050(9) 0.061(9) 0.056(9) 0.020(8) 0.010(8) -0.006(8) C13 0.049(10) 0.077(9) 0.066(10) 0.018(9) 0.007(8) 0.007(8) C14 0.036(10) 0.103(17) 0.075(16) 0.014(15) 0.000 0.000 C15 0.116(16) 0.074(10) 0.076(11) 0.027(9) 0.005(14) -0.024(14) _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 C1 2.001(15) . ? Pt1 C1 2.001(15) 3_556 ? Pt1 P1 2.291(5) 3_556 ? Pt1 P1 2.291(5) . ? P1 C23 1.86(2) . ? P1 C19 1.87(2) . ? P1 C21 1.89(2) . ? C1 C2 1.188(19) . ? C2 C3 1.438(19) . ? C3 C4 1.405(17) . ? C3 C8 1.408(19) . ? C4 C5 1.365(19) . ? C5 C6 1.41(2) . ? C5 C15 1.57(2) . ? C6 C7 1.34(2) . ? C7 C8 1.38(2) . ? C8 C9 1.46(2) . ? C9 C10 1.136(18) . ? C10 c11 1.425(18) . ? c12 c11 1.395(16) . ? c12 c11 1.395(16) 3_556 ? c11 C13 1.393(18) . ? C13 C14 1.374(17) . ? C14 C13 1.374(17) 3_556 ? C15 C18B 1.49(5) . ? C15 C18 1.57(4) . ? C15 C17 1.56(4) . ? C15 C16 1.59(4) . ? C15 C16B 1.63(6) . ? C15 C17B 1.66(5) . ? C16 C18B 1.54(5) . ? C16 C16B 1.58(6) . ? C17 C17B 1.49(6) . ? C17 C16B 1.53(7) . ? C18 C18B 1.24(5) . ? C18 C17B 1.50(5) . ? C19 C20 1.61(2) . ? C21 C22 1.65(2) . ? C23 C24 1.61(2) . ? 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 Pt1 C1 170.7(8) . 3_556 ? C1 Pt1 P1 89.3(5) . 3_556 ? C1 Pt1 P1 91.4(4) 3_556 3_556 ? C1 Pt1 P1 91.4(4) . . ? C1 Pt1 P1 89.3(5) 3_556 . ? P1 Pt1 P1 172.4(3) 3_556 . ? C23 P1 C19 117.4(15) . . ? C23 P1 C21 112.2(13) . . ? C19 P1 C21 87.1(14) . . ? C23 P1 Pt1 113.7(8) . . ? C19 P1 Pt1 115.0(13) . . ? C21 P1 Pt1 108.1(11) . . ? C2 C1 Pt1 169.8(14) . . ? C1 C2 C3 168.6(16) . . ? C4 C3 C8 119.1(13) . . ? C4 C3 C2 121.2(13) . . ? C8 C3 C2 119.6(13) . . ? C5 C4 C3 121.8(14) . . ? C4 C5 C6 117.4(16) . . ? C4 C5 C15 121.1(15) . . ? C6 C5 C15 121.3(16) . . ? C7 C6 C5 121.2(17) . . ? C6 C7 C8 122.4(16) . . ? C7 C8 C3 117.9(14) . . ? C7 C8 C9 120.8(14) . . ? C3 C8 C9 121.4(14) . . ? C10 C9 C8 173(2) . . ? C9 C10 c11 178.1(18) . . ? c11 c12 c11 123.3(17) . 3_556 ? C13 c11 c12 117.4(14) . . ? C13 c11 C10 122.0(14) . . ? c12 c11 C10 120.6(13) . . ? C14 C13 c11 119.6(15) . . ? C13 C14 C13 122.6(19) . 3_556 ? C18B C15 C18 48(2) . . ? C18B C15 C17 137(2) . . ? C18 C15 C17 108(2) . . ? C18B C15 C5 111(2) . . ? C18 C15 C5 108.7(19) . . ? C17 C15 C5 110.6(18) . . ? C18B C15 C16 60(2) . . ? C18 C15 C16 106(2) . . ? C17 C15 C16 112(2) . . ? C5 C15 C16 111.3(18) . . ? C18B C15 C16B 114(3) . . ? C18 C15 C16B 139(3) . . ? C17 C15 C16B 57(2) . . ? C5 C15 C16B 112(2) . . ? C16 C15 C16B 59(2) . . ? C18B C15 C17B 99(3) . . ? C18 C15 C17B 55(2) . . ? C17 C15 C17B 54.9(19) . . ? C5 C15 C17B 113(2) . . ? C16 C15 C17B 136(2) . . ? C16B C15 C17B 107(3) . . ? C18B C16 C16B 114(4) . . ? C18B C16 C15 57(2) . . ? C16B C16 C15 62(3) . . ? C17B C17 C16B 123(4) . . ? C17B C17 C15 66(2) . . ? C16B C17 C15 64(3) . . ? C18B C18 C17B 122(4) . . ? C18B C18 C15 63(3) . . ? C17B C18 C15 66(2) . . ? C17 C16B C16 115(5) . . ? C17 C16B C15 59(3) . . ? C16 C16B C15 59(3) . . ? C17 C17B C18 116(4) . . ? C17 C17B C15 59(2) . . ? C18 C17B C15 59(2) . . ? C18 C18B C15 69(3) . . ? C18 C18B C16 129(4) . . ? C15 C18B C16 63(2) . . ? C20 C19 P1 104.5(16) . . ? C22 C21 P1 100.8(15) . . ? C24 C23 P1 106.7(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.872 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.122