Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Otto, Stefanus' ; Inorganic Chemistry Chemical Center Lund University P.O. Box 124 SE-221 00 Lund Sweden ; 'Elding, Lars I.' ; Inorganic Chemistry Chemical Center Lund University P.O. Box 124 SE-221 00 Lund Sweden ; _publ_contact_author_name 'Prof Lars Elding' _publ_contact_author_address ; Inorganic Chemistry 1 Chemical Center Lund University PO Box 124 Lund S 221 00 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 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_section_title ; Low temperature kinetic study of very fast substitution reactions at platinum(II) trans to olefins. ; _publ_contact_letter ; Please consider this CIF file as supplementary material to our submission for publication as a regular paper in J. Chem. Soc. Dalton Trans.. The cif file passed the Chester checkcif routine indicating no serious problems. ; _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 Gottingen, Germany. Sheldrick, G.M. (1997a). SHELXS-97. Program for Crystal Structure Solution. University of Gottingen, Germany. Sheldrick, G.M. (1997b). SHELXL-97. Program for Crystal Structure Refinement. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #======================================================================= data_Bu4N[PtCl3(C8H14)] _database_code_CSD 176914 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrabutylammoniumtrichloro(cyclooctene)platinum(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H50 Cl3 N Pt' _chemical_formula_sum 'C24 H50 Cl3 N Pt' _chemical_formula_weight 654.09 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' '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 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 14.731(3) _cell_length_b 9.4487(19) _cell_length_c 21.021(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.94(3) _cell_angle_gamma 90.00 _cell_volume 2924.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5604 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.70 _exptl_crystal_description 'Rectangle' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 5.083 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.335 _exptl_absorpt_correction_T_max 0.827 _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 10 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 the 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 'fine-focus sealed tube' _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 29582 _diffrn_reflns_av_R_equivalents 0.0802 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 31.83 _reflns_number_total 9167 _reflns_number_gt 6441 _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^)+(0.0653P)^2^] 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 0.0057(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9167 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1202 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.002 _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 0.019839(11) 0.616057(16) 0.182195(7) 0.04604(8) Uani 1 1 d . . . Cl1 Cl 0.14113(11) 0.61939(13) 0.11435(8) 0.0730(4) Uani 1 1 d . . . Cl2 Cl 0.09987(9) 0.45261(13) 0.24271(6) 0.0641(3) Uani 1 1 d . . . Cl3 Cl -0.05532(9) 0.77998(15) 0.11803(6) 0.0719(3) Uani 1 1 d . . . C1 C -0.0695(3) 0.6736(5) 0.2565(2) 0.0515(10) Uani 1 1 d . . . H1 H -0.081(3) 0.771(5) 0.245(2) 0.057(13) Uiso 1 1 d . . . C2 C -0.1083(3) 0.5638(6) 0.2209(2) 0.0536(10) Uani 1 1 d . . . H2 H -0.143(3) 0.597(4) 0.186(2) 0.049(12) Uiso 1 1 d . . . C3 C -0.1231(4) 0.4175(6) 0.2478(3) 0.0688(14) Uani 1 1 d . . . H3A H -0.0779 0.3981 0.2813 0.112(3) Uiso 1 1 calc R . . H3B H -0.1169 0.3472 0.2146 0.112(3) Uiso 1 1 calc R . . C4 C -0.2181(5) 0.4096(7) 0.2744(4) 0.097(2) Uani 1 1 d . . . H4A H -0.2620 0.4126 0.2390 0.112(3) Uiso 1 1 calc R . . H4B H -0.2245 0.3187 0.2952 0.112(3) Uiso 1 1 calc R . . C5 C -0.2421(6) 0.5228(10) 0.3207(5) 0.134(3) Uani 1 1 d . . . H5A H -0.2503 0.6099 0.2968 0.112(3) Uiso 1 1 calc R . . H5B H -0.3008 0.4985 0.3372 0.112(3) Uiso 1 1 calc R . . C6 C -0.1836(5) 0.5532(12) 0.3733(4) 0.120(3) Uani 1 1 d . . . H6A H -0.1484 0.4684 0.3825 0.112(3) Uiso 1 1 calc R . . H6B H -0.2213 0.5693 0.4096 0.112(3) Uiso 1 1 calc R . . C7 C -0.1158(5) 0.6779(7) 0.3708(3) 0.0844(17) Uani 1 1 d . . . H7A H -0.0902 0.6941 0.4133 0.112(3) Uiso 1 1 calc R . . H7B H -0.1489 0.7626 0.3580 0.112(3) Uiso 1 1 calc R . . C8 C -0.0365(4) 0.6558(6) 0.3246(2) 0.0648(13) Uani 1 1 d . . . H8A H 0.0112 0.7239 0.3343 0.112(3) Uiso 1 1 calc R . . H8B H -0.0114 0.5616 0.3305 0.112(3) Uiso 1 1 calc R . . N N 0.1862(3) 0.1184(3) 0.09634(18) 0.0499(8) Uani 1 1 d . . . C11 C 0.1854(4) 0.1103(5) 0.1691(2) 0.0672(15) Uani 1 1 d . . . H11A H 0.2475 0.1178 0.1856 0.112(3) Uiso 1 1 calc R . . H11B H 0.1525 0.1917 0.1845 0.112(3) Uiso 1 1 calc R . . C12 C 0.1434(5) -0.0229(9) 0.1968(3) 0.103(2) Uani 1 1 d . . . H12A H 0.0833 -0.0366 0.1775 0.112(3) Uiso 1 1 calc R . . H12B H 0.1802 -0.1041 0.1859 0.112(3) Uiso 1 1 calc R . . C13 C 0.1361(6) -0.0161(13) 0.2684(4) 0.136(4) Uani 1 1 d . . . H13A H 0.1423 -0.1117 0.2849 0.112(3) Uiso 1 1 calc R . . H13B H 0.1875 0.0377 0.2853 0.112(3) Uiso 1 1 calc R . . C14 C 0.0616(10) 0.0391(14) 0.2914(7) 0.232(8) Uani 1 1 d . . . H14A H 0.0612 0.1395 0.2842 0.112(3) Uiso 1 1 calc R . . H14B H 0.0603 0.0209 0.3363 0.112(3) Uiso 1 1 calc R . . H14C H 0.0093 -0.0028 0.2705 0.112(3) Uiso 1 1 calc R . . C21 C 0.2276(3) -0.0149(5) 0.0692(2) 0.0537(10) Uani 1 1 d . . . H21A H 0.1947 -0.0958 0.0850 0.112(3) Uiso 1 1 calc R . . H21B H 0.2184 -0.0130 0.0233 0.112(3) Uiso 1 1 calc R . . C22 C 0.3279(3) -0.0370(5) 0.0844(2) 0.0620(12) Uani 1 1 d . . . H22A H 0.3396 -0.0306 0.1300 0.112(3) Uiso 1 1 calc R . . H22B H 0.3630 0.0358 0.0639 0.112(3) Uiso 1 1 calc R . . C23 C 0.3560(4) -0.1832(6) 0.0604(3) 0.0725(14) Uani 1 1 d . . . H23A H 0.3251 -0.2554 0.0844 0.112(3) Uiso 1 1 calc R . . H23B H 0.3367 -0.1928 0.0160 0.112(3) Uiso 1 1 calc R . . C24 C 0.4569(4) -0.2073(8) 0.0667(3) 0.100(2) Uani 1 1 d . . . H24A H 0.4882 -0.1286 0.0486 0.112(3) Uiso 1 1 calc R . . H24B H 0.4723 -0.2925 0.0446 0.112(3) Uiso 1 1 calc R . . H24C H 0.4747 -0.2162 0.1109 0.112(3) Uiso 1 1 calc R . . C31 C 0.2392(3) 0.2478(5) 0.0795(3) 0.0633(13) Uani 1 1 d . . . H31A H 0.2992 0.2403 0.0998 0.112(3) Uiso 1 1 calc R . . H31B H 0.2098 0.3294 0.0977 0.112(3) Uiso 1 1 calc R . . C32 C 0.2504(4) 0.2754(6) 0.0098(3) 0.0743(14) Uani 1 1 d . . . H32A H 0.1918 0.2992 -0.0098 0.112(3) Uiso 1 1 calc R . . H32B H 0.2721 0.1900 -0.0103 0.112(3) Uiso 1 1 calc R . . C33 C 0.3163(6) 0.3942(6) -0.0011(5) 0.096(2) Uani 1 1 d . . . H33A H 0.2947 0.4788 0.0197 0.112(3) Uiso 1 1 calc R . . H33B H 0.3747 0.3697 0.0186 0.112(3) Uiso 1 1 calc R . . C34 C 0.3290(6) 0.4263(9) -0.0695(5) 0.121(3) Uani 1 1 d . . . H34A H 0.3510 0.3435 -0.0905 0.112(3) Uiso 1 1 calc R . . H34B H 0.3722 0.5017 -0.0731 0.112(3) Uiso 1 1 calc R . . H34C H 0.2720 0.4545 -0.0890 0.112(3) Uiso 1 1 calc R . . C41 C 0.0893(3) 0.1223(5) 0.0677(2) 0.0583(12) Uani 1 1 d . . . H41A H 0.0928 0.1213 0.0217 0.112(3) Uiso 1 1 calc R . . H41B H 0.0586 0.0363 0.0801 0.112(3) Uiso 1 1 calc R . . C42 C 0.0317(4) 0.2463(7) 0.0860(3) 0.0804(16) Uani 1 1 d . . . H42A H 0.0598 0.3343 0.0734 0.112(3) Uiso 1 1 calc R . . H42B H 0.0244 0.2479 0.1317 0.112(3) Uiso 1 1 calc R . . C43 C -0.0618(4) 0.2276(7) 0.0509(3) 0.0802(16) Uani 1 1 d . . . H43A H -0.0527 0.2186 0.0056 0.112(3) Uiso 1 1 calc R . . H43B H -0.0898 0.1409 0.0652 0.112(3) Uiso 1 1 calc R . . C44 C -0.1246(5) 0.3488(8) 0.0619(4) 0.100(2) Uani 1 1 d . . . H44A H -0.1443 0.3459 0.1049 0.112(3) Uiso 1 1 calc R . . H44B H -0.1763 0.3420 0.0330 0.112(3) Uiso 1 1 calc R . . H44C H -0.0933 0.4362 0.0548 0.112(3) 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 0.04675(12) 0.05009(12) 0.04167(10) 0.00014(6) 0.00720(7) -0.00086(6) Cl1 0.0698(8) 0.0736(9) 0.0776(9) 0.0100(6) 0.0332(7) 0.0069(6) Cl2 0.0692(7) 0.0657(7) 0.0575(6) 0.0039(5) 0.0024(5) 0.0142(6) Cl3 0.0689(8) 0.0871(9) 0.0600(7) 0.0217(6) 0.0079(5) 0.0126(6) C1 0.055(3) 0.051(2) 0.049(2) -0.001(2) 0.0158(19) 0.002(2) C2 0.044(2) 0.068(3) 0.049(2) 0.000(2) 0.0071(18) -0.004(2) C3 0.073(3) 0.065(3) 0.069(3) -0.013(3) 0.015(3) -0.024(3) C4 0.096(5) 0.088(4) 0.107(6) 0.000(4) 0.031(4) -0.035(4) C5 0.115(6) 0.145(8) 0.148(8) -0.011(6) 0.073(6) -0.044(6) C6 0.093(5) 0.198(9) 0.071(4) -0.006(5) 0.042(4) -0.015(6) C7 0.116(5) 0.082(4) 0.057(3) -0.014(3) 0.034(3) 0.002(4) C8 0.082(4) 0.067(3) 0.046(2) -0.012(2) 0.008(2) -0.013(3) N 0.048(2) 0.054(2) 0.0471(19) -0.0124(14) 0.0002(16) 0.0058(14) C11 0.065(3) 0.091(4) 0.046(2) -0.021(2) -0.005(2) 0.015(2) C12 0.098(5) 0.154(7) 0.059(3) 0.009(4) 0.017(3) -0.020(5) C13 0.098(6) 0.240(12) 0.070(4) 0.021(6) 0.021(4) 0.015(7) C14 0.290(18) 0.212(13) 0.203(13) -0.088(11) 0.156(13) -0.143(13) C21 0.060(3) 0.056(2) 0.045(2) -0.0094(18) 0.0047(19) 0.007(2) C22 0.057(3) 0.069(3) 0.060(3) -0.009(2) -0.003(2) 0.011(2) C23 0.067(3) 0.076(3) 0.075(3) -0.011(3) 0.012(3) 0.015(3) C24 0.079(4) 0.118(6) 0.105(5) -0.013(4) 0.011(4) 0.039(4) C31 0.057(3) 0.056(3) 0.077(3) -0.012(2) -0.003(2) 0.003(2) C32 0.068(3) 0.065(3) 0.090(4) 0.007(3) 0.004(3) -0.005(3) C33 0.085(5) 0.075(4) 0.129(7) 0.018(4) 0.019(4) 0.002(3) C34 0.101(6) 0.103(5) 0.161(9) 0.041(6) 0.036(5) 0.016(4) C41 0.047(2) 0.073(3) 0.054(3) -0.010(2) -0.006(2) 0.008(2) C42 0.064(3) 0.097(4) 0.080(4) -0.015(3) -0.006(3) 0.024(3) C43 0.071(3) 0.104(4) 0.065(3) -0.010(3) -0.005(3) 0.022(3) C44 0.076(4) 0.139(6) 0.083(4) -0.009(4) -0.013(4) 0.035(4) _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 2.139(4) . ? Pt C1 2.147(4) . ? Pt Cl2 2.3003(12) . ? Pt Cl3 2.3115(13) . ? Pt Cl1 2.3238(16) . ? C1 C2 1.391(7) . ? C1 C8 1.504(6) . ? C2 C3 1.512(7) . ? C3 C4 1.527(9) . ? C4 C5 1.497(11) . ? C5 C6 1.409(11) . ? C6 C7 1.546(11) . ? C7 C8 1.558(8) . ? N C31 1.499(6) . ? N C21 1.519(5) . ? N C41 1.530(6) . ? N C11 1.532(6) . ? C11 C12 1.526(9) . ? C12 C13 1.515(9) . ? C13 C14 1.322(14) . ? C21 C22 1.515(6) . ? C22 C23 1.532(7) . ? C23 C24 1.506(8) . ? C31 C32 1.503(7) . ? C32 C33 1.507(8) . ? C33 C34 1.486(12) . ? C41 C42 1.504(7) . ? C42 C43 1.551(7) . ? C43 C44 1.494(8) . ? 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 37.87(19) . . ? C2 Pt Cl2 94.42(14) . . ? C1 Pt Cl2 94.75(13) . . ? C2 Pt Cl3 88.00(14) . . ? C1 Pt Cl3 87.81(13) . . ? Cl2 Pt Cl3 177.36(5) . . ? C2 Pt Cl1 160.67(14) . . ? C1 Pt Cl1 161.16(13) . . ? Cl2 Pt Cl1 87.61(5) . . ? Cl3 Pt Cl1 89.76(5) . . ? C2 C1 C8 122.8(4) . . ? C2 C1 Pt 70.8(3) . . ? C8 C1 Pt 118.5(3) . . ? C1 C2 C3 122.8(5) . . ? C1 C2 Pt 71.4(3) . . ? C3 C2 Pt 119.6(4) . . ? C2 C3 C4 109.1(5) . . ? C5 C4 C3 116.3(6) . . ? C6 C5 C4 120.3(9) . . ? C5 C6 C7 120.4(7) . . ? C6 C7 C8 114.7(5) . . ? C1 C8 C7 110.7(5) . . ? C31 N C21 111.6(4) . . ? C31 N C41 112.0(3) . . ? C21 N C41 104.7(3) . . ? C31 N C11 107.3(4) . . ? C21 N C11 110.5(3) . . ? C41 N C11 110.8(4) . . ? C12 C11 N 116.0(4) . . ? C13 C12 C11 112.8(7) . . ? C14 C13 C12 117.9(10) . . ? C22 C21 N 115.9(4) . . ? C21 C22 C23 109.1(4) . . ? C24 C23 C22 112.6(5) . . ? N C31 C32 116.5(4) . . ? C31 C32 C33 111.7(5) . . ? C34 C33 C32 113.7(7) . . ? C42 C41 N 116.5(4) . . ? C41 C42 C43 106.8(5) . . ? C44 C43 C42 112.5(5) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 31.83 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 2.323 _refine_diff_density_min -1.883 _refine_diff_density_rms 0.136 #===================================================================== data_Bu4N[PtCl3(CH2CHSiMe3)] _database_code_CSD 176915 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrabutylammoniumtrichloro(vinyltrimethylsilyl)platinum(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H48 Cl3 N Pt Si' _chemical_formula_sum 'C21 H48 Cl3 N Pt Si' _chemical_formula_weight 644.13 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' 'Si' 'Si' 0.0817 0.0704 '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 9.0980(18) _cell_length_b 13.448(3) _cell_length_c 13.449(3) _cell_angle_alpha 99.16(3) _cell_angle_beta 104.48(3) _cell_angle_gamma 109.64(3) _cell_volume 1446.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3606 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.60 _exptl_crystal_description 'Rectangle' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 5.177 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.150 _exptl_absorpt_correction_T_max 0.422 _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 15 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 the 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 'fine-focus sealed tube' _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 10481 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6628 _reflns_number_gt 4873 _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^)+(0.0864P)^2^] 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 6628 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.032 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.14417(3) 0.33173(2) 0.20967(2) 0.04831(13) Uani 1 1 d . . . Cl1 Cl 0.2149(3) 0.51874(18) 0.2407(2) 0.0711(6) Uani 1 1 d . . . Cl2 Cl 0.0620(4) 0.3360(2) 0.35694(19) 0.0874(8) Uani 1 1 d . . . Cl3 Cl 0.2316(3) 0.3322(2) 0.0638(2) 0.0798(7) Uani 1 1 d . . . Si Si -0.1702(4) 0.0785(2) 0.1811(2) 0.0791(8) Uani 1 1 d . . . C1 C 0.1851(13) 0.1880(7) 0.2195(9) 0.079(3) Uani 1 1 d . . . C2 C 0.0192(11) 0.1557(7) 0.1501(7) 0.063(2) Uani 1 1 d . . . C3 C -0.2574(17) -0.0564(9) 0.0826(12) 0.129(6) Uani 1 1 d . . . H3A H -0.3146 -0.0509 0.0145 0.099(5) Uiso 1 1 calc R . . H3B H -0.3331 -0.1093 0.1054 0.099(5) Uiso 1 1 calc R . . H3C H -0.1698 -0.0790 0.0765 0.099(5) Uiso 1 1 calc R . . C4 C -0.3261(15) 0.1427(11) 0.1613(12) 0.107(4) Uani 1 1 d . . . H4A H -0.3485 0.1547 0.0916 0.099(5) Uiso 1 1 calc R . . H4B H -0.2831 0.2115 0.2142 0.099(5) Uiso 1 1 calc R . . H4C H -0.4263 0.0947 0.1682 0.099(5) Uiso 1 1 calc R . . C5 C -0.1226(18) 0.0535(10) 0.3158(11) 0.125(5) Uani 1 1 d . . . H5A H -0.1812 0.0814 0.3554 0.099(5) Uiso 1 1 calc R . . H5B H -0.0061 0.0900 0.3528 0.099(5) Uiso 1 1 calc R . . H5C H -0.1561 -0.0238 0.3083 0.099(5) Uiso 1 1 calc R . . N N 0.7670(7) 0.5980(5) 0.2740(5) 0.0445(13) Uani 1 1 d . . . C11 C 0.7636(10) 0.5279(6) 0.3525(6) 0.0494(17) Uani 1 1 d . . . H11A H 0.8346 0.4891 0.3448 0.099(5) Uiso 1 1 calc R . . H11B H 0.8109 0.5762 0.4241 0.099(5) Uiso 1 1 calc R . . C12 C 0.5960(11) 0.4448(8) 0.3416(7) 0.067(2) Uani 1 1 d . . . H12A H 0.5179 0.4798 0.3353 0.099(5) Uiso 1 1 calc R . . H12B H 0.5579 0.3865 0.2770 0.099(5) Uiso 1 1 calc R . . C13 C 0.6001(13) 0.3965(9) 0.4353(8) 0.074(3) Uani 1 1 d . . . H13A H 0.6363 0.4556 0.4990 0.099(5) Uiso 1 1 calc R . . H13B H 0.4882 0.3482 0.4261 0.099(5) Uiso 1 1 calc R . . C14 C 0.704(2) 0.3360(13) 0.4529(13) 0.135(6) Uani 1 1 d . . . H14A H 0.6598 0.2705 0.3955 0.099(5) Uiso 1 1 calc R . . H14B H 0.7083 0.3168 0.5190 0.099(5) Uiso 1 1 calc R . . H14C H 0.8135 0.3803 0.4558 0.099(5) Uiso 1 1 calc R . . C21 C 0.6638(9) 0.6644(6) 0.2852(6) 0.0512(17) Uani 1 1 d . . . H21A H 0.5510 0.6137 0.2701 0.099(5) Uiso 1 1 calc R . . H21B H 0.6635 0.7038 0.2306 0.099(5) Uiso 1 1 calc R . . C22 C 0.7153(11) 0.7468(7) 0.3920(6) 0.059(2) Uani 1 1 d . . . H22A H 0.7168 0.7096 0.4481 0.099(5) Uiso 1 1 calc R . . H22B H 0.8257 0.8012 0.4072 0.099(5) Uiso 1 1 calc R . . C23 C 0.5968(13) 0.8018(8) 0.3889(7) 0.067(2) Uani 1 1 d . . . H23A H 0.4883 0.7469 0.3774 0.099(5) Uiso 1 1 calc R . . H23B H 0.5895 0.8331 0.3285 0.099(5) Uiso 1 1 calc R . . C24 C 0.6426(15) 0.8907(8) 0.4881(8) 0.083(3) Uani 1 1 d . . . H24A H 0.6653 0.8633 0.5494 0.099(5) Uiso 1 1 calc R . . H24B H 0.5527 0.9135 0.4853 0.099(5) Uiso 1 1 calc R . . H24C H 0.7389 0.9519 0.4928 0.099(5) Uiso 1 1 calc R . . C31 C 0.6928(9) 0.5269(6) 0.1584(5) 0.0474(16) Uani 1 1 d . . . H31A H 0.5791 0.4802 0.1469 0.099(5) Uiso 1 1 calc R . . H31B H 0.6907 0.5750 0.1119 0.099(5) Uiso 1 1 calc R . . C32 C 0.7743(11) 0.4572(7) 0.1244(6) 0.061(2) Uani 1 1 d . . . H32A H 0.7834 0.4106 0.1718 0.099(5) Uiso 1 1 calc R . . H32B H 0.8847 0.5023 0.1274 0.099(5) Uiso 1 1 calc R . . C33 C 0.6734(13) 0.3866(8) 0.0104(7) 0.071(2) Uani 1 1 d . . . H33A H 0.5669 0.3376 0.0101 0.099(5) Uiso 1 1 calc R . . H33B H 0.6538 0.4340 -0.0341 0.099(5) Uiso 1 1 calc R . . C34 C 0.7513(17) 0.3210(9) -0.0370(8) 0.096(4) Uani 1 1 d . . . H34A H 0.8551 0.3688 -0.0397 0.099(5) Uiso 1 1 calc R . . H34B H 0.6803 0.2788 -0.1079 0.099(5) Uiso 1 1 calc R . . H34C H 0.7694 0.2726 0.0055 0.099(5) Uiso 1 1 calc R . . C41 C 0.9482(9) 0.6705(6) 0.3004(6) 0.0511(18) Uani 1 1 d . . . H41A H 0.9918 0.7095 0.3754 0.099(5) Uiso 1 1 calc R . . H41B H 1.0073 0.6239 0.2895 0.099(5) Uiso 1 1 calc R . . C42 C 0.9840(11) 0.7531(7) 0.2367(7) 0.061(2) Uani 1 1 d . . . H42A H 0.9233 0.7993 0.2447 0.099(5) Uiso 1 1 calc R . . H42B H 0.9489 0.7156 0.1618 0.099(5) Uiso 1 1 calc R . . C43 C 1.1695(12) 0.8236(8) 0.2763(8) 0.075(3) Uani 1 1 d . . . H43A H 1.2037 0.8586 0.3518 0.099(5) Uiso 1 1 calc R . . H43B H 1.2286 0.7766 0.2673 0.099(5) Uiso 1 1 calc R . . C44 C 1.2161(15) 0.9101(9) 0.2188(11) 0.100(4) Uani 1 1 d . . . H44A H 1.2284 0.8790 0.1536 0.099(5) Uiso 1 1 calc R . . H44B H 1.3184 0.9687 0.2630 0.099(5) Uiso 1 1 calc R . . H44C H 1.1311 0.9381 0.2031 0.099(5) 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 0.04031(17) 0.05467(19) 0.03802(17) 0.01158(12) 0.00500(12) 0.01033(12) Cl1 0.0545(12) 0.0585(12) 0.0918(17) 0.0181(11) 0.0148(12) 0.0196(10) Cl2 0.0917(19) 0.0885(16) 0.0508(12) 0.0026(11) 0.0298(13) 0.0005(14) Cl3 0.0782(16) 0.0942(17) 0.0581(13) 0.0199(11) 0.0310(12) 0.0169(13) Si 0.0638(16) 0.0614(15) 0.0824(18) 0.0244(13) 0.0063(14) -0.0007(12) C1 0.077(7) 0.055(5) 0.094(7) 0.026(5) 0.011(6) 0.023(5) C2 0.062(5) 0.051(4) 0.061(5) 0.006(4) 0.014(4) 0.013(4) C3 0.091(9) 0.077(8) 0.144(13) 0.009(8) -0.015(9) -0.008(7) C4 0.070(7) 0.112(9) 0.125(11) 0.043(8) 0.020(7) 0.021(7) C5 0.110(10) 0.106(9) 0.136(12) 0.074(9) 0.037(9) 0.000(8) N 0.040(3) 0.056(3) 0.038(3) 0.017(3) 0.009(2) 0.020(3) C11 0.052(4) 0.058(4) 0.037(4) 0.014(3) 0.005(3) 0.027(4) C12 0.059(5) 0.067(5) 0.063(5) 0.028(4) 0.010(4) 0.014(4) C13 0.066(6) 0.089(7) 0.068(6) 0.029(5) 0.027(5) 0.026(5) C14 0.155(14) 0.187(15) 0.183(15) 0.145(14) 0.119(13) 0.123(13) C21 0.040(4) 0.062(4) 0.048(4) 0.014(3) 0.008(3) 0.020(3) C22 0.062(5) 0.070(5) 0.044(4) 0.010(4) 0.015(4) 0.028(4) C23 0.077(6) 0.075(6) 0.057(5) 0.014(4) 0.022(5) 0.041(5) C24 0.107(9) 0.080(7) 0.074(7) 0.011(5) 0.032(6) 0.053(7) C31 0.042(4) 0.055(4) 0.032(3) 0.006(3) 0.001(3) 0.012(3) C32 0.057(5) 0.071(5) 0.050(4) 0.011(4) 0.010(4) 0.026(4) C33 0.082(7) 0.070(6) 0.050(5) 0.007(4) 0.011(5) 0.028(5) C34 0.141(12) 0.093(8) 0.057(6) 0.007(5) 0.032(7) 0.056(8) C41 0.044(4) 0.057(4) 0.048(4) 0.010(3) 0.010(3) 0.021(4) C42 0.061(5) 0.061(5) 0.059(5) 0.015(4) 0.018(4) 0.022(4) C43 0.061(6) 0.072(6) 0.077(6) 0.014(5) 0.018(5) 0.014(5) C44 0.080(8) 0.074(7) 0.143(12) 0.029(7) 0.051(8) 0.016(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 2.105(9) . ? Pt C2 2.161(8) . ? Pt Cl2 2.285(2) . ? Pt Cl3 2.294(2) . ? Pt Cl1 2.314(2) . ? Si C3 1.849(13) . ? Si C5 1.866(12) . ? Si C2 1.874(10) . ? Si C4 1.880(13) . ? C1 C2 1.437(13) . ? N C21 1.514(9) . ? N C41 1.520(10) . ? N C11 1.523(9) . ? N C31 1.535(9) . ? C11 C12 1.512(11) . ? C12 C13 1.504(12) . ? C13 C14 1.443(15) . ? C21 C22 1.523(11) . ? C22 C23 1.494(12) . ? C23 C24 1.504(12) . ? C31 C32 1.462(11) . ? C32 C33 1.531(12) . ? C33 C34 1.467(14) . ? C41 C42 1.507(11) . ? C42 C43 1.531(12) . ? C43 C44 1.500(15) . ? 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 39.3(4) . . ? C1 Pt Cl2 92.0(3) . . ? C2 Pt Cl2 93.2(3) . . ? C1 Pt Cl3 88.9(3) . . ? C2 Pt Cl3 88.2(3) . . ? Cl2 Pt Cl3 178.49(9) . . ? C1 Pt Cl1 155.9(3) . . ? C2 Pt Cl1 164.6(3) . . ? Cl2 Pt Cl1 89.24(10) . . ? Cl3 Pt Cl1 89.43(10) . . ? C3 Si C5 106.9(6) . . ? C3 Si C2 103.1(6) . . ? C5 Si C2 113.1(5) . . ? C3 Si C4 109.1(7) . . ? C5 Si C4 111.1(7) . . ? C2 Si C4 113.0(5) . . ? C2 C1 Pt 72.4(5) . . ? C1 C2 Si 124.2(7) . . ? C1 C2 Pt 68.2(5) . . ? Si C2 Pt 121.4(5) . . ? C21 N C41 112.1(5) . . ? C21 N C11 110.9(6) . . ? C41 N C11 105.2(5) . . ? C21 N C31 106.2(5) . . ? C41 N C31 111.4(6) . . ? C11 N C31 111.3(6) . . ? C12 C11 N 116.2(6) . . ? C13 C12 C11 112.1(7) . . ? C14 C13 C12 116.5(9) . . ? N C21 C22 117.4(6) . . ? C23 C22 C21 109.8(7) . . ? C22 C23 C24 114.3(8) . . ? C32 C31 N 117.7(6) . . ? C31 C32 C33 109.3(7) . . ? C34 C33 C32 114.5(9) . . ? C42 C41 N 115.5(6) . . ? C41 C42 C43 109.4(7) . . ? C44 C43 C42 113.1(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.701 _refine_diff_density_min -2.304 _refine_diff_density_rms 0.175