Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global # 1. SUBMISSION DETAILS _publ_contact_author 'Lars I. Elding' _publ_contact_author_address ; Professor Lars I. Elding Inorganic Chemistry Department of Chemistry Lund University P.O. Box 124 SE-221 00 Lund Sweden ; _publ_contact_author_phone 'Intl-46-46-222 8105' _publ_contact_author_fax 'Intl-46-46-222 4439' _publ_contact_author_email LarsI.Elding@inorg.lu.se _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF file as supplementary material to our submission for publication as a regular paper in Dalton Transactions. The cif file passed the Chester checkcif routine indicating no serious problems. ; #========================================================================= # 2. PROCESSING SUMMARY (Office Use Only) _journal_coden_Cambridge 222 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #========================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Bridge-splitting kinetics, equilibria and structures of trans-bis cyclooctene complexes of platinum(II) ; loop_ _publ_author_name _publ_author_address 'Otto, Stefanus' ; Inorganic Chemistry Department of Chemistry Lund University P.O. Box 124 SE-221 00 Lund Sweden ; 'Roodt, Andreas' ; Department of Chemistry and Biochemistry Rand Afrikaans University P. O. Box 524, Auckland Park 2006 Johannesburg South Africa ; 'Elding, Lars I.' ; Inorganic Chemistry Department of chemistry University of Lund P.O. Box 124 SE-221 00 Lund Sweden ; #========================================================================= # 4. TEXT _publ_section_abstract ; See text ; _publ_section_comment ; See text ; _publ_section_exptl_prep ; See text ; _publ_section_exptl_refinement ; See text ; _publ_section_references ; See text Brandenburg, K. & Berndt, M. (1999). DIAMOND. Release 2.1c. Crystal Impact GbR, Bonn, Germany. Sheldrick, G.M. (1996). SADABS. Program for Absorption Correction of Area Detector Data. University of G\"ottingen, Germany. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of G\"ottingen, Germany. Siemens (1995). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _publ_section_figure_captions ; See text ; _publ_section_acknowledgements ; See text ; #========================================================================= data_sad2xp _database_code_CSD 205486 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-mu-dichloro(cyclooctene)diplatinum(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Cl4 Pt2' _chemical_formula_sum 'C16 H28 Cl4 Pt2' _chemical_formula_weight 752.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 8.2310(16) _cell_length_b 5.9600(12) _cell_length_c 20.991(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.68(3) _cell_angle_gamma 90.00 _cell_volume 1015.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4324 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 31.50 _exptl_crystal_description Rectangle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 14.287 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.054 _exptl_absorpt_correction_T_max 0.158 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The intensity data were collected on a Siemens SMART CCD diffractometer using an exposure time of 33 seconds/frame. A total of 2300 frames with a frame width of 0.20\% were collected. The first 50 frames were recollected at the end of each data collection to check for decay; no decay was observed. Both the minimum and maximum residual electron density are located within 1.5 \%A of the Pt atom. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'First 50 frames repeated after data collection.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 7730 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2168 _reflns_number_gt 1887 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0938P)^2^+17.4700P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2168 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Pt Pt 0.15508(6) 0.20458(9) 0.01286(2) 0.0341(2) Uani 1 1 d . . . Cl1 Cl 0.0589(4) -0.0885(6) 0.07076(16) 0.0458(9) Uani 1 1 d . . . Cl2 Cl 0.2237(5) 0.4814(8) -0.0516(2) 0.0589(11) Uani 1 1 d . . . C1 C 0.3976(17) 0.215(2) 0.0678(7) 0.039(3) Uani 1 1 d . . . H1 H 0.4771 0.2886 0.0448 0.064(15) Uiso 1 1 calc R . . C2 C 0.2978(18) 0.369(2) 0.0944(7) 0.040(3) Uani 1 1 d . . . H2 H 0.3229 0.5255 0.0858 0.064(15) Uiso 1 1 calc R . . C3 C 0.242(2) 0.337(3) 0.1581(8) 0.052(4) Uani 1 1 d . . . H3A H 0.2128 0.1807 0.1621 0.064(15) Uiso 1 1 calc R . . H3B H 0.1438 0.4259 0.1585 0.064(15) Uiso 1 1 calc R . . C4 C 0.371(3) 0.402(5) 0.2171(10) 0.080(7) Uani 1 1 d . . . H4A H 0.4134 0.5491 0.2094 0.064(15) Uiso 1 1 calc R . . H4B H 0.3149 0.4142 0.2542 0.064(15) Uiso 1 1 calc R . . C5 C 0.517(3) 0.241(4) 0.2348(10) 0.073(6) Uani 1 1 d . . . H5A H 0.5741 0.2801 0.2777 0.064(15) Uiso 1 1 calc R . . H5B H 0.4744 0.0903 0.2372 0.064(15) Uiso 1 1 calc R . . C6 C 0.643(3) 0.238(4) 0.1895(11) 0.078(6) Uani 1 1 d . . . H6A H 0.6305 0.3741 0.1640 0.064(15) Uiso 1 1 calc R . . H6B H 0.7523 0.2402 0.2154 0.064(15) Uiso 1 1 calc R . . C7 C 0.633(2) 0.039(4) 0.1438(9) 0.062(5) Uani 1 1 d . . . H7A H 0.6634 -0.0949 0.1692 0.064(15) Uiso 1 1 calc R . . H7B H 0.7140 0.0601 0.1157 0.064(15) Uiso 1 1 calc R . . C8 C 0.4638(16) -0.003(3) 0.1008(7) 0.040(3) Uani 1 1 d . . . H8A H 0.4755 -0.1152 0.0683 0.064(15) Uiso 1 1 calc R . . H8B H 0.3866 -0.0600 0.1271 0.064(15) 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 Pt 0.0358(3) 0.0347(3) 0.0311(3) 0.00614(19) 0.0029(2) -0.00694(19) Cl1 0.050(2) 0.049(2) 0.0341(16) 0.0145(15) -0.0066(14) -0.0135(15) Cl2 0.061(2) 0.061(2) 0.051(2) 0.024(2) -0.0009(17) -0.024(2) C1 0.033(7) 0.049(8) 0.032(6) 0.003(6) -0.002(5) -0.011(6) C2 0.054(8) 0.030(6) 0.035(7) -0.008(6) 0.005(6) -0.012(6) C3 0.056(10) 0.064(10) 0.039(8) -0.012(8) 0.014(7) 0.002(8) C4 0.080(14) 0.108(18) 0.052(10) -0.034(12) 0.017(9) -0.026(13) C5 0.061(12) 0.104(16) 0.047(10) -0.004(10) -0.004(8) -0.021(11) C6 0.072(14) 0.101(17) 0.056(12) 0.007(12) -0.002(10) -0.010(12) C7 0.047(9) 0.083(13) 0.054(10) 0.018(10) 0.000(7) 0.003(9) C8 0.034(7) 0.048(8) 0.038(7) 0.002(6) 0.002(5) 0.001(6) _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 C1 2.132(13) . ? Pt C2 2.143(13) . ? Pt Cl2 2.265(4) . ? Pt Cl1 2.340(3) . ? Pt Cl1 2.371(3) 3 ? Cl1 Pt 2.371(3) 3 ? C1 C2 1.41(2) . ? C1 C8 1.53(2) . ? C2 C3 1.50(2) . ? C3 C4 1.54(2) . ? C4 C5 1.54(3) . ? C5 C6 1.52(3) . ? C6 C7 1.52(3) . ? C7 C8 1.55(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 Pt C2 38.4(6) . . ? C1 Pt Cl2 89.8(4) . . ? C2 Pt Cl2 89.2(4) . . ? C1 Pt Cl1 96.2(4) . . ? C2 Pt Cl1 96.5(4) . . ? Cl2 Pt Cl1 173.74(12) . . ? C1 Pt Cl1 157.0(4) . 3 ? C2 Pt Cl1 164.5(4) . 3 ? Cl2 Pt Cl1 89.97(13) . 3 ? Cl1 Pt Cl1 83.84(12) . 3 ? Pt Cl1 Pt 96.16(12) . 3 ? C2 C1 C8 124.2(13) . . ? C2 C1 Pt 71.2(8) . . ? C8 C1 Pt 116.7(9) . . ? C1 C2 C3 123.9(14) . . ? C1 C2 Pt 70.4(8) . . ? C3 C2 Pt 116.6(10) . . ? C2 C3 C4 114.7(15) . . ? C5 C4 C3 116.4(18) . . ? C6 C5 C4 116.6(19) . . ? C7 C6 C5 116(2) . . ? C6 C7 C8 116.4(16) . . ? C1 C8 C7 110.0(13) . . ? 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 C1 C2 Pt Cl1 91.8(8) . . . . ? C1 C2 Pt Cl2 -90.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 5.253 _refine_diff_density_min -4.242 _refine_diff_density_rms 0.394 #===================================================== data_[PtCl2(C8H14)2] _database_code_CSD 205487 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-dichlorobis(cyclooctene)platinum(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Cl2 Pt' _chemical_formula_sum 'C16 H28 Cl2 Pt' _chemical_formula_weight 486.37 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8407(12) _cell_length_b 7.4886(15) _cell_length_c 10.069(2) _cell_angle_alpha 84.01(3) _cell_angle_beta 88.45(3) _cell_angle_gamma 73.59(3) _cell_volume 420.17(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3387 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 30.85 _exptl_crystal_description Prism _exptl_crystal_colour Orange-yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 236 _exptl_absorpt_coefficient_mu 8.653 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.043 _exptl_absorpt_correction_T_max 0.124 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The intensity data were collected on a Siemens SMART CCD diffractometer using an exposure time of 20 seconds/frame. A total of 2300 frames with a frame width of 0.20\% were collected. The first 50 frames were recollected at the end of each data collection to check for decay; no decay was observed. Both the minimum and maximum residual electron density are located within 1 \%A of the Pt atom. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'First 50 frames repeated after data collection.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 4315 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 31.89 _reflns_number_total 2547 _reflns_number_gt 2542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0815P)^2^+0.3400P] 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 2547 _refine_ls_number_parameters 90 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Pt Pt 0.5000 0.5000 0.5000 0.03430(12) Uani 1 2 d S . . Cl1 Cl 0.1773(3) 0.6333(2) 0.36007(18) 0.0461(3) Uani 1 1 d . . . C1 C 0.3775(11) 0.7624(8) 0.6055(6) 0.0360(10) Uani 1 1 d . . . H1 H 0.2700 0.8661 0.5502 0.053(19) Uiso 1 1 calc R . . C2 C 0.2618(11) 0.6390(9) 0.6659(7) 0.0376(11) Uani 1 1 d . . . H2 H 0.0917 0.6746 0.6432 0.053(19) Uiso 1 1 calc R . . C3 C 0.3146(14) 0.5384(9) 0.8043(7) 0.0437(13) Uani 1 1 d . . . H3A H 0.4856 0.5011 0.8196 0.049(7) Uiso 1 1 calc R . . H3B H 0.2621 0.4260 0.8106 0.049(7) Uiso 1 1 calc R . . C4 C 0.1884(15) 0.6630(11) 0.9139(7) 0.0481(14) Uani 1 1 d . . . H4A H 0.0229 0.7194 0.8879 0.049(7) Uiso 1 1 calc R . . H4B H 0.1895 0.5830 0.9963 0.049(7) Uiso 1 1 calc R . . C5 C 0.2967(15) 0.8198(12) 0.9425(7) 0.0503(15) Uani 1 1 d . . . H5A H 0.4681 0.7671 0.9521 0.049(7) Uiso 1 1 calc R . . H5B H 0.2356 0.8633 1.0274 0.049(7) Uiso 1 1 calc R . . C6 C 0.2482(17) 0.9910(12) 0.8360(8) 0.0538(16) Uani 1 1 d . . . H6A H 0.1112 0.9916 0.7833 0.049(7) Uiso 1 1 calc R . . H6B H 0.2044 1.1034 0.8819 0.049(7) Uiso 1 1 calc R . . C7 C 0.4529(16) 1.0023(10) 0.7400(8) 0.0494(15) Uani 1 1 d . . . H7A H 0.5760 1.0318 0.7890 0.049(7) Uiso 1 1 calc R . . H7B H 0.3933 1.1047 0.6711 0.049(7) Uiso 1 1 calc R . . C8 C 0.5682(12) 0.8210(9) 0.6713(7) 0.0400(12) Uani 1 1 d . . . H8A H 0.6830 0.8440 0.6051 0.049(7) Uiso 1 1 calc R . . H8B H 0.6517 0.7218 0.7373 0.049(7) 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 Pt 0.03382(16) 0.02987(16) 0.03903(17) -0.00139(10) -0.00933(10) -0.00853(10) Cl1 0.0406(7) 0.0439(8) 0.0502(8) -0.0043(6) -0.0164(6) -0.0045(6) C1 0.041(3) 0.026(2) 0.041(3) -0.0025(19) -0.003(2) -0.0087(19) C2 0.035(2) 0.035(3) 0.046(3) -0.009(2) 0.001(2) -0.014(2) C3 0.056(4) 0.036(3) 0.043(3) 0.000(2) -0.001(3) -0.020(3) C4 0.056(4) 0.048(3) 0.044(3) -0.003(3) 0.004(3) -0.020(3) C5 0.057(4) 0.054(4) 0.042(3) -0.009(3) 0.000(3) -0.018(3) C6 0.064(4) 0.044(4) 0.052(4) -0.008(3) 0.004(3) -0.014(3) C7 0.069(4) 0.036(3) 0.052(3) -0.013(3) -0.001(3) -0.026(3) C8 0.044(3) 0.036(3) 0.046(3) -0.007(2) -0.001(2) -0.020(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 Pt C1 2.259(6) 2_666 ? Pt C1 2.259(6) . ? Pt C2 2.287(6) 2_666 ? Pt C2 2.287(6) . ? Pt Cl1 2.3068(18) . ? Pt Cl1 2.3068(18) 2_666 ? C1 C2 1.375(8) . ? C1 C8 1.500(8) . ? C2 C3 1.509(9) . ? C3 C4 1.554(10) . ? C4 C5 1.536(11) . ? C5 C6 1.549(12) . ? C6 C7 1.533(11) . ? C7 C8 1.559(10) . ? 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 Pt C1 180.0(3) 2_666 . ? C1 Pt C2 35.2(2) 2_666 2_666 ? C1 Pt C2 144.8(2) . 2_666 ? C1 Pt C2 144.8(2) 2_666 . ? C1 Pt C2 35.2(2) . . ? C2 Pt C2 180.000(1) 2_666 . ? C1 Pt Cl1 93.96(17) 2_666 . ? C1 Pt Cl1 86.04(17) . . ? C2 Pt Cl1 93.81(18) 2_666 . ? C2 Pt Cl1 86.19(18) . . ? C1 Pt Cl1 86.04(17) 2_666 2_666 ? C1 Pt Cl1 93.96(17) . 2_666 ? C2 Pt Cl1 86.19(18) 2_666 2_666 ? C2 Pt Cl1 93.81(18) . 2_666 ? Cl1 Pt Cl1 180.0 . 2_666 ? C2 C1 C8 124.2(6) . . ? C2 C1 Pt 73.5(3) . . ? C8 C1 Pt 116.3(4) . . ? C1 C2 C3 125.2(6) . . ? C1 C2 Pt 71.3(3) . . ? C3 C2 Pt 115.5(4) . . ? C2 C3 C4 112.0(6) . . ? C5 C4 C3 116.0(6) . . ? C4 C5 C6 115.9(7) . . ? C7 C6 C5 116.7(7) . . ? C6 C7 C8 114.9(6) . . ? C1 C8 C7 109.5(6) . . ? 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 C1 C2 Pt Cl1 -88.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 31.89 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 2.303 _refine_diff_density_min -2.377 _refine_diff_density_rms 0.217 #==================================================================== data_sadxp _database_code_CSD 205488 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetraphenylphosphoniumtrichlorocycloocteneplatinum(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Cl3 P Pt' _chemical_formula_sum 'C32 H34 Cl3 P Pt' _chemical_formula_weight 751.00 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' 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 11.227(2) _cell_length_b 14.746(3) _cell_length_c 18.901(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.18(3) _cell_angle_gamma 90.00 _cell_volume 2989.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7090 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.60 _exptl_crystal_description Yellow _exptl_crystal_colour Rectangle _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 5.035 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The intensity data were collected on a Siemens SMART CCD diffractometer using an exposure time of 25 seconds/frame. A total of 1940 frames with a frame width of 0.25\% were collected. The first 50 frames were recollected at the end of each data collection to check for decay; no decay was observed. Both the minimum and maximum residual electron density are located within 1 \%A of the Pt atom. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'First 50 frames repeated after data collection.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 31554 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 31.82 _reflns_number_total 9316 _reflns_number_gt 5336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0320P)^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 9316 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.003 _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 Pt Pt 0.053470(14) 0.707771(11) 0.191178(9) 0.03465(6) Uani 1 1 d . . . P P 0.37028(10) 1.02407(7) 0.32659(6) 0.0329(2) Uani 1 1 d . . . Cl1 Cl -0.06066(10) 0.75617(8) 0.07109(6) 0.0460(3) Uani 1 1 d . . . Cl2 Cl -0.07805(12) 0.78736(9) 0.24165(7) 0.0624(3) Uani 1 1 d . . . Cl3 Cl 0.17636(11) 0.62783(10) 0.13565(7) 0.0629(4) Uani 1 1 d . . . C1 C 0.1896(4) 0.7051(3) 0.2992(2) 0.0389(10) Uani 1 1 d . . . H1 H 0.165(5) 0.766(3) 0.324(3) 0.075(16) Uiso 1 1 d . . . C2 C 0.1104(4) 0.6303(3) 0.2927(2) 0.0384(10) Uani 1 1 d . . . H2 H 0.046(4) 0.635(3) 0.309(2) 0.039(12) Uiso 1 1 d . . . C3 C 0.1543(5) 0.5345(3) 0.2896(3) 0.0533(13) Uani 1 1 d . . . H3A H 0.2221 0.5335 0.2676 0.057(2) Uiso 1 1 calc R . . H3B H 0.0867 0.4978 0.2591 0.057(2) Uiso 1 1 calc R . . C4 C 0.1987(5) 0.4952(3) 0.3685(3) 0.0703(16) Uani 1 1 d . . . H4A H 0.1272 0.4896 0.3870 0.057(2) Uiso 1 1 calc R . . H4B H 0.2309 0.4347 0.3659 0.057(2) Uiso 1 1 calc R . . C5 C 0.2995(5) 0.5507(4) 0.4246(3) 0.0685(16) Uani 1 1 d . . . H5A H 0.2607 0.6052 0.4362 0.057(2) Uiso 1 1 calc R . . H5B H 0.3282 0.5156 0.4698 0.057(2) Uiso 1 1 calc R . . C6 C 0.4113(4) 0.5784(3) 0.4019(3) 0.0566(14) Uani 1 1 d . . . H6A H 0.4167 0.5396 0.3616 0.057(2) Uiso 1 1 calc R . . H6B H 0.4852 0.5676 0.4433 0.057(2) Uiso 1 1 calc R . . C7 C 0.4131(4) 0.6770(3) 0.3775(3) 0.0549(13) Uani 1 1 d . . . H7A H 0.4971 0.6917 0.3772 0.057(2) Uiso 1 1 calc R . . H7B H 0.3937 0.7154 0.4143 0.057(2) Uiso 1 1 calc R . . C8 C 0.3236(4) 0.7007(3) 0.3018(3) 0.0510(12) Uani 1 1 d . . . H8A H 0.3477 0.7590 0.2865 0.057(2) Uiso 1 1 calc R . . H8B H 0.3328 0.6558 0.2662 0.057(2) Uiso 1 1 calc R . . C11 C 0.2856(4) 1.0321(3) 0.2303(2) 0.0372(10) Uani 1 1 d . . . C12 C 0.2136(4) 0.9586(3) 0.1954(3) 0.0506(12) Uani 1 1 d . . . H12 H 0.2074 0.9072 0.2227 0.057(2) Uiso 1 1 calc R . . C13 C 0.1516(5) 0.9615(4) 0.1207(3) 0.0632(14) Uani 1 1 d . . . H13 H 0.1043 0.9123 0.0975 0.057(2) Uiso 1 1 calc R . . C14 C 0.1600(5) 1.0375(4) 0.0810(3) 0.0635(15) Uani 1 1 d . . . H14 H 0.1190 1.0395 0.0305 0.057(2) Uiso 1 1 calc R . . C15 C 0.2289(5) 1.1111(4) 0.1153(3) 0.0683(16) Uani 1 1 d . . . H15 H 0.2329 1.1630 0.0881 0.057(2) Uiso 1 1 calc R . . C16 C 0.2916(4) 1.1078(3) 0.1897(3) 0.0527(12) Uani 1 1 d . . . H16 H 0.3385 1.1574 0.2125 0.057(2) Uiso 1 1 calc R . . C21 C 0.4165(4) 1.1355(3) 0.3636(2) 0.0331(9) Uani 1 1 d . . . C22 C 0.3454(4) 1.1845(3) 0.3982(2) 0.0430(11) Uani 1 1 d . . . H22 H 0.2727 1.1602 0.4043 0.057(2) Uiso 1 1 calc R . . C23 C 0.3845(5) 1.2714(3) 0.4237(3) 0.0553(13) Uani 1 1 d . . . H23 H 0.3379 1.3047 0.4479 0.057(2) Uiso 1 1 calc R . . C24 C 0.4895(5) 1.3085(3) 0.4140(3) 0.0534(13) Uani 1 1 d . . . H24 H 0.5133 1.3669 0.4309 0.057(2) Uiso 1 1 calc R . . C25 C 0.5612(4) 1.2593(3) 0.3792(3) 0.0496(12) Uani 1 1 d . . . H25 H 0.6339 1.2838 0.3730 0.057(2) Uiso 1 1 calc R . . C26 C 0.5225(4) 1.1732(3) 0.3536(3) 0.0431(11) Uani 1 1 d . . . H26 H 0.5690 1.1401 0.3293 0.057(2) Uiso 1 1 calc R . . C31 C 0.5108(4) 0.9596(3) 0.3373(2) 0.0346(9) Uani 1 1 d . . . C32 C 0.5360(4) 0.9176(3) 0.2783(2) 0.0420(10) Uani 1 1 d . . . H32 H 0.4783 0.9206 0.2315 0.057(2) Uiso 1 1 calc R . . C33 C 0.6463(4) 0.8709(3) 0.2881(3) 0.0504(12) Uani 1 1 d . . . H33 H 0.6627 0.8429 0.2478 0.057(2) Uiso 1 1 calc R . . C34 C 0.7316(4) 0.8655(3) 0.3566(3) 0.0483(12) Uani 1 1 d . . . H34 H 0.8057 0.8340 0.3628 0.057(2) Uiso 1 1 calc R . . C35 C 0.7079(4) 0.9063(3) 0.4161(3) 0.0539(13) Uani 1 1 d . . . H35 H 0.7651 0.9016 0.4629 0.057(2) Uiso 1 1 calc R . . C36 C 0.5983(4) 0.9549(3) 0.4063(3) 0.0459(11) Uani 1 1 d . . . H36 H 0.5835 0.9844 0.4464 0.057(2) Uiso 1 1 calc R . . C41 C 0.2729(4) 0.9713(3) 0.3741(2) 0.0352(9) Uani 1 1 d . . . C42 C 0.3144(4) 0.9011(3) 0.4246(2) 0.0397(10) Uani 1 1 d . . . H42 H 0.3953 0.8793 0.4343 0.057(2) Uiso 1 1 calc R . . C43 C 0.2352(5) 0.8643(3) 0.4601(2) 0.0515(12) Uani 1 1 d . . . H43 H 0.2632 0.8175 0.4939 0.057(2) Uiso 1 1 calc R . . C44 C 0.1149(4) 0.8956(3) 0.4463(3) 0.0530(12) Uani 1 1 d . . . H44 H 0.0621 0.8697 0.4704 0.057(2) Uiso 1 1 calc R . . C45 C 0.0735(4) 0.9642(4) 0.3974(3) 0.0560(13) Uani 1 1 d . . . H45 H -0.0076 0.9855 0.3883 0.057(2) Uiso 1 1 calc R . . C46 C 0.1511(4) 1.0028(3) 0.3609(2) 0.0467(11) Uani 1 1 d . . . H46 H 0.1221 1.0498 0.3275 0.057(2) 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 Pt 0.03398(9) 0.03638(9) 0.03197(9) 0.00022(9) 0.00725(6) -0.00272(8) P 0.0331(5) 0.0321(5) 0.0319(6) -0.0018(5) 0.0073(5) 0.0016(4) Cl1 0.0447(6) 0.0547(6) 0.0314(6) 0.0116(5) 0.0002(5) -0.0048(5) Cl2 0.0619(8) 0.0671(8) 0.0539(8) -0.0077(7) 0.0107(6) 0.0316(7) Cl3 0.0441(7) 0.1063(11) 0.0408(7) -0.0156(7) 0.0164(5) 0.0050(7) C1 0.046(2) 0.036(2) 0.030(2) -0.004(2) 0.0034(19) 0.004(2) C2 0.037(2) 0.048(3) 0.029(2) 0.004(2) 0.009(2) 0.002(2) C3 0.060(3) 0.031(2) 0.055(3) 0.004(2) -0.004(2) -0.003(2) C4 0.078(4) 0.044(3) 0.073(4) 0.021(3) -0.004(3) 0.002(3) C5 0.072(4) 0.061(3) 0.058(4) 0.023(3) -0.003(3) 0.003(3) C6 0.045(3) 0.065(3) 0.045(3) -0.004(3) -0.008(2) 0.014(2) C7 0.044(3) 0.057(3) 0.053(3) -0.004(3) -0.003(2) 0.002(2) C8 0.044(3) 0.053(3) 0.051(3) 0.000(2) 0.006(2) -0.011(2) C11 0.035(2) 0.044(2) 0.029(2) 0.001(2) 0.0023(18) 0.0038(19) C12 0.054(3) 0.044(3) 0.046(3) 0.005(2) 0.002(2) -0.011(2) C13 0.066(3) 0.062(3) 0.048(3) -0.004(3) -0.004(3) -0.019(3) C14 0.062(3) 0.087(4) 0.031(3) -0.003(3) -0.003(2) -0.012(3) C15 0.088(4) 0.064(3) 0.044(3) 0.009(3) 0.005(3) -0.018(3) C16 0.066(3) 0.048(3) 0.036(3) 0.003(2) 0.004(2) -0.015(2) C21 0.034(2) 0.030(2) 0.031(2) 0.0004(18) 0.0027(18) 0.0019(17) C22 0.046(3) 0.039(2) 0.042(3) -0.002(2) 0.011(2) 0.0061(19) C23 0.068(3) 0.044(3) 0.052(3) -0.009(2) 0.014(3) 0.011(2) C24 0.066(3) 0.033(3) 0.050(3) -0.001(2) -0.002(3) -0.002(2) C25 0.046(3) 0.042(3) 0.053(3) 0.006(2) 0.003(2) -0.008(2) C26 0.040(2) 0.039(2) 0.049(3) -0.002(2) 0.011(2) 0.001(2) C31 0.037(2) 0.030(2) 0.036(2) -0.0025(19) 0.0085(19) 0.0000(17) C32 0.043(3) 0.043(2) 0.039(3) -0.004(2) 0.011(2) 0.002(2) C33 0.046(3) 0.053(3) 0.056(3) -0.008(3) 0.022(2) 0.008(2) C34 0.040(3) 0.046(3) 0.062(3) -0.004(3) 0.019(2) 0.008(2) C35 0.039(3) 0.061(3) 0.053(3) 0.005(3) 0.001(2) 0.005(2) C36 0.042(3) 0.051(3) 0.041(3) -0.012(2) 0.008(2) 0.005(2) C41 0.034(2) 0.038(2) 0.032(2) -0.0020(19) 0.0067(18) 0.0023(18) C42 0.046(3) 0.038(2) 0.030(2) 0.000(2) 0.004(2) 0.000(2) C43 0.063(3) 0.058(3) 0.032(3) 0.013(2) 0.010(2) -0.006(3) C44 0.054(3) 0.066(3) 0.040(3) 0.009(3) 0.014(2) -0.010(3) C45 0.034(3) 0.080(4) 0.055(3) 0.006(3) 0.015(2) 0.007(2) C46 0.040(3) 0.054(3) 0.043(3) 0.014(2) 0.008(2) 0.002(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 Pt C2 2.161(4) . ? Pt C1 2.160(4) . ? Pt Cl3 2.2913(12) . ? Pt Cl2 2.3022(12) . ? Pt Cl1 2.3632(12) . ? P C41 1.785(4) . ? P C11 1.790(4) . ? P C31 1.801(4) . ? P C21 1.802(4) . ? C1 C2 1.399(6) . ? C1 C8 1.492(6) . ? C2 C3 1.504(6) . ? C3 C4 1.539(7) . ? C4 C5 1.537(7) . ? C5 C6 1.498(7) . ? C6 C7 1.527(6) . ? C7 C8 1.527(6) . ? C11 C16 1.368(6) . ? C11 C12 1.398(6) . ? C12 C13 1.377(6) . ? C13 C14 1.367(7) . ? C14 C15 1.378(7) . ? C15 C16 1.375(6) . ? C21 C26 1.376(6) . ? C21 C22 1.376(5) . ? C22 C23 1.393(6) . ? C23 C24 1.361(7) . ? C24 C25 1.386(7) . ? C25 C26 1.382(6) . ? C31 C32 1.378(5) . ? C31 C36 1.383(6) . ? C32 C33 1.381(6) . ? C33 C34 1.366(6) . ? C34 C35 1.370(6) . ? C35 C36 1.388(6) . ? C41 C42 1.391(5) . ? C41 C46 1.395(5) . ? C42 C43 1.374(6) . ? C43 C44 1.377(6) . ? C44 C45 1.357(6) . ? C45 C46 1.383(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 C2 Pt C1 37.77(16) . . ? C2 Pt Cl3 94.30(13) . . ? C1 Pt Cl3 94.00(12) . . ? C2 Pt Cl2 87.64(13) . . ? C1 Pt Cl2 88.80(12) . . ? Cl3 Pt Cl2 177.16(4) . . ? C2 Pt Cl1 161.19(12) . . ? C1 Pt Cl1 160.96(12) . . ? Cl3 Pt Cl1 86.81(5) . . ? Cl2 Pt Cl1 90.68(5) . . ? C41 P C11 108.7(2) . . ? C41 P C31 111.05(19) . . ? C11 P C31 109.53(19) . . ? C41 P C21 110.57(19) . . ? C11 P C21 109.87(19) . . ? C31 P C21 107.15(18) . . ? C2 C1 C8 125.3(4) . . ? C2 C1 Pt 71.2(2) . . ? C8 C1 Pt 117.2(3) . . ? C1 C2 C3 122.4(4) . . ? C1 C2 Pt 71.0(2) . . ? C3 C2 Pt 118.4(3) . . ? C2 C3 C4 109.3(4) . . ? C5 C4 C3 115.5(4) . . ? C6 C5 C4 117.1(5) . . ? C5 C6 C7 115.6(4) . . ? C6 C7 C8 116.0(4) . . ? C1 C8 C7 114.7(4) . . ? C16 C11 C12 119.0(4) . . ? C16 C11 P 121.7(3) . . ? C12 C11 P 119.2(3) . . ? C13 C12 C11 120.4(4) . . ? C14 C13 C12 119.5(5) . . ? C13 C14 C15 120.5(5) . . ? C16 C15 C14 120.0(5) . . ? C11 C16 C15 120.6(4) . . ? C26 C21 C22 120.0(4) . . ? C26 C21 P 118.5(3) . . ? C22 C21 P 121.5(3) . . ? C21 C22 C23 118.7(4) . . ? C24 C23 C22 121.3(5) . . ? C23 C24 C25 120.1(4) . . ? C26 C25 C24 118.7(4) . . ? C21 C26 C25 121.2(4) . . ? C32 C31 C36 118.9(4) . . ? C32 C31 P 121.9(3) . . ? C36 C31 P 119.2(3) . . ? C31 C32 C33 120.4(4) . . ? C34 C33 C32 120.4(4) . . ? C33 C34 C35 120.0(4) . . ? C34 C35 C36 119.8(4) . . ? C31 C36 C35 120.4(4) . . ? C42 C41 C46 118.8(4) . . ? C42 C41 P 122.6(3) . . ? C46 C41 P 118.6(3) . . ? C43 C42 C41 119.7(4) . . ? C42 C43 C44 121.0(4) . . ? C45 C44 C43 119.9(4) . . ? C44 C45 C46 120.4(4) . . ? C45 C46 C41 120.2(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 C1 C2 Pt Cl2 -91.1(3) . . . . ? C1 C2 Pt Cl3 91.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 31.82 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.103 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.124