# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1a _chemical_melting_point 165 _chemical_formula_moiety 'C21 H28 Cl1 N O2 Pt S, C H2 Cl2' _chemical_formula_sum 'C22 H30 Cl3 N O2 Pt S' _chemical_formula_weight 673.97 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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1719(3) _cell_length_b 11.1215(2) _cell_length_c 14.2096(4) _cell_angle_alpha 110.883(2) _cell_angle_beta 108.6750(10) _cell_angle_gamma 91.334(2) _cell_volume 1267.38(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10198 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.41 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 5.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5040 _exptl_absorpt_correction_T_max 0.6473 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; Half sphere of data collected using COLLECT strategy (Nonius, 2000). Crystal to detector distance = 30mm; combination of \f and \w scans of 1.2\%, 90s per \%, 2 iterations. ; _diffrn_ambient_temperature 173(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 Kappa CCD diffractometer' _diffrn_measurement_method '1.2\% \f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10198 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.41 _reflns_number_total 5197 _reflns_number_gt 4574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT program (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2001)' _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^)+(0.0069P)^2^+2.4764P] 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 SHELXL _refine_ls_extinction_coef 0.00257(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5197 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0437 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Pt1 Pt 0.169350(16) 0.432789(13) 0.152669(11) 0.01808(6) Uani 1 1 d . . . Cl1 Cl 0.26711(11) 0.46264(8) 0.03012(7) 0.0279(2) Uani 1 1 d . . . Cl2 Cl 0.53759(13) 0.85050(11) 0.18240(9) 0.0462(3) Uani 1 1 d . . . Cl3 Cl 0.78604(15) 0.74026(12) 0.29316(13) 0.0700(4) Uani 1 1 d . . . S1 S 0.04696(10) 0.23889(8) 0.02904(7) 0.02085(18) Uani 1 1 d . . . O1 O 0.2889(3) 0.6124(2) 0.24955(18) 0.0233(5) Uani 1 1 d . . . O2 O -0.0622(3) 0.1622(2) 0.0490(2) 0.0323(6) Uani 1 1 d . . . N1 N 0.0980(3) 0.4235(2) 0.2723(2) 0.0159(6) Uani 1 1 d . . . C1 C 0.2594(4) 0.6946(3) 0.3311(3) 0.0184(7) Uani 1 1 d . . . C2 C 0.3259(4) 0.8270(3) 0.3710(3) 0.0239(8) Uani 1 1 d . . . H2 H 0.3897 0.8530 0.3384 0.029 Uiso 1 1 calc R . . C3 C 0.2992(4) 0.9180(3) 0.4564(3) 0.0271(8) Uani 1 1 d . . . H3 H 0.3434 1.0066 0.4810 0.032 Uiso 1 1 calc R . . C4 C 0.2088(5) 0.8834(3) 0.5077(3) 0.0298(9) Uani 1 1 d . . . H4 H 0.1904 0.9476 0.5663 0.036 Uiso 1 1 calc R . . C5 C 0.1469(4) 0.7553(3) 0.4724(3) 0.0272(8) Uani 1 1 d . . . H5 H 0.0873 0.7307 0.5081 0.033 Uiso 1 1 calc R . . C6 C 0.1698(4) 0.6591(3) 0.3838(3) 0.0202(7) Uani 1 1 d . . . C7 C 0.1082(4) 0.5269(3) 0.3557(3) 0.0191(7) Uani 1 1 d . . . H7 H 0.0686 0.5124 0.4055 0.023 Uiso 1 1 calc R . . C8 C 0.0381(4) 0.3023(3) 0.2734(3) 0.0181(7) Uani 1 1 d . . . C9 C 0.1445(4) 0.2218(3) 0.3015(3) 0.0205(7) Uani 1 1 d . . . C10 C 0.0846(4) 0.1060(3) 0.3028(3) 0.0251(8) Uani 1 1 d . . . H10 H 0.1535 0.0492 0.3218 0.030 Uiso 1 1 calc R . . C11 C -0.0730(4) 0.0730(3) 0.2769(3) 0.0271(8) Uani 1 1 d . . . H11 H -0.1119 -0.0068 0.2772 0.033 Uiso 1 1 calc R . . C12 C -0.1746(4) 0.1553(3) 0.2506(3) 0.0261(8) Uani 1 1 d . . . H12 H -0.2828 0.1318 0.2341 0.031 Uiso 1 1 calc R . . C13 C -0.1223(4) 0.2721(3) 0.2477(3) 0.0199(7) Uani 1 1 d . . . C14 C 0.3192(4) 0.2597(4) 0.3354(3) 0.0282(8) Uani 1 1 d . . . H14 H 0.3376 0.3200 0.3008 0.034 Uiso 1 1 calc R . . C15 C 0.4015(5) 0.1423(4) 0.3007(4) 0.0401(10) Uani 1 1 d . . . H15A H 0.5133 0.1720 0.3236 0.060 Uiso 1 1 calc R . . H15B H 0.3586 0.0975 0.2222 0.060 Uiso 1 1 calc R . . H15C H 0.3854 0.0822 0.3341 0.060 Uiso 1 1 calc R . . C16 C 0.3883(5) 0.3328(4) 0.4573(3) 0.0470(12) Uani 1 1 d . . . H16A H 0.5010 0.3575 0.4792 0.070 Uiso 1 1 calc R . . H16B H 0.3680 0.2764 0.4927 0.070 Uiso 1 1 calc R . . H16C H 0.3404 0.4113 0.4782 0.070 Uiso 1 1 calc R . . C17 C -0.2378(4) 0.3583(4) 0.2163(3) 0.0304(9) Uani 1 1 d . . . H17 H -0.1820 0.4266 0.2042 0.036 Uiso 1 1 calc R . . C18 C -0.3733(5) 0.2824(5) 0.1122(4) 0.0558(13) Uani 1 1 d . . . H18A H -0.4457 0.3414 0.0951 0.084 Uiso 1 1 calc R . . H18B H -0.4279 0.2127 0.1212 0.084 Uiso 1 1 calc R . . H18C H -0.3334 0.2443 0.0534 0.084 Uiso 1 1 calc R . . C19 C -0.2992(5) 0.4272(4) 0.3067(4) 0.0439(11) Uani 1 1 d . . . H19A H -0.3738 0.4822 0.2844 0.066 Uiso 1 1 calc R . . H19B H -0.2122 0.4814 0.3715 0.066 Uiso 1 1 calc R . . H19C H -0.3512 0.3621 0.3220 0.066 Uiso 1 1 calc R . . C20 C -0.0548(5) 0.2521(4) -0.0951(3) 0.0324(9) Uani 1 1 d . . . H20A H -0.1377 0.3046 -0.0872 0.049 Uiso 1 1 calc R . . H20B H -0.1004 0.1650 -0.1506 0.049 Uiso 1 1 calc R . . H20C H 0.0177 0.2942 -0.1161 0.049 Uiso 1 1 calc R . . C21 C 0.1886(4) 0.1417(3) -0.0024(3) 0.0315(9) Uani 1 1 d . . . H21A H 0.2529 0.1277 0.0616 0.047 Uiso 1 1 calc R . . H21B H 0.2549 0.1862 -0.0259 0.047 Uiso 1 1 calc R . . H21C H 0.1363 0.0575 -0.0602 0.047 Uiso 1 1 calc R . . C22 C 0.5985(5) 0.7061(4) 0.1958(3) 0.0399(10) Uani 1 1 d . . . H22A H 0.5243 0.6649 0.2170 0.048 Uiso 1 1 calc R . . H22B H 0.5991 0.6441 0.1257 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02056(8) 0.01476(8) 0.01959(8) 0.00615(5) 0.00851(5) 0.00178(5) Cl1 0.0376(5) 0.0239(5) 0.0272(5) 0.0082(4) 0.0197(4) 0.0012(4) Cl2 0.0439(6) 0.0481(7) 0.0530(7) 0.0259(6) 0.0177(5) 0.0085(5) Cl3 0.0458(7) 0.0494(7) 0.1020(11) 0.0433(8) -0.0057(7) -0.0052(6) S1 0.0250(5) 0.0153(4) 0.0206(4) 0.0048(3) 0.0086(4) 0.0008(3) O1 0.0269(13) 0.0172(12) 0.0256(13) 0.0043(10) 0.0138(11) -0.0025(10) O2 0.0383(16) 0.0237(14) 0.0302(14) 0.0031(11) 0.0153(12) -0.0117(12) N1 0.0151(14) 0.0143(14) 0.0169(14) 0.0055(12) 0.0044(11) 0.0038(11) C1 0.0193(17) 0.0184(17) 0.0158(16) 0.0062(14) 0.0044(14) 0.0025(14) C2 0.028(2) 0.0213(18) 0.0214(18) 0.0078(15) 0.0080(15) -0.0029(15) C3 0.035(2) 0.0162(18) 0.0237(19) 0.0060(15) 0.0041(16) -0.0020(16) C4 0.042(2) 0.0187(19) 0.026(2) 0.0036(16) 0.0149(18) 0.0031(17) C5 0.033(2) 0.027(2) 0.0222(19) 0.0065(16) 0.0134(16) 0.0032(16) C6 0.0216(18) 0.0188(17) 0.0181(17) 0.0064(14) 0.0048(14) 0.0037(14) C7 0.0170(17) 0.0226(18) 0.0208(17) 0.0111(15) 0.0075(14) 0.0027(14) C8 0.0252(18) 0.0116(16) 0.0192(17) 0.0052(14) 0.0111(14) -0.0010(14) C9 0.0238(18) 0.0195(18) 0.0169(17) 0.0061(14) 0.0067(14) 0.0019(14) C10 0.036(2) 0.0172(18) 0.0275(19) 0.0110(15) 0.0147(17) 0.0074(16) C11 0.039(2) 0.0186(18) 0.028(2) 0.0078(16) 0.0196(17) 0.0002(16) C12 0.0235(19) 0.0258(19) 0.028(2) 0.0041(16) 0.0156(16) -0.0033(16) C13 0.0217(18) 0.0175(17) 0.0210(17) 0.0058(14) 0.0101(15) -0.0001(14) C14 0.0214(19) 0.030(2) 0.040(2) 0.0217(18) 0.0101(17) 0.0085(16) C15 0.037(2) 0.043(3) 0.055(3) 0.028(2) 0.023(2) 0.019(2) C16 0.025(2) 0.048(3) 0.051(3) 0.013(2) -0.001(2) 0.006(2) C17 0.0207(19) 0.030(2) 0.043(2) 0.0186(18) 0.0104(17) 0.0021(16) C18 0.030(2) 0.063(3) 0.055(3) 0.016(3) -0.004(2) 0.012(2) C19 0.044(3) 0.038(2) 0.067(3) 0.025(2) 0.035(2) 0.018(2) C20 0.038(2) 0.027(2) 0.024(2) 0.0081(17) 0.0020(17) 0.0043(18) C21 0.036(2) 0.0218(19) 0.032(2) 0.0049(17) 0.0129(18) 0.0085(17) C22 0.036(2) 0.030(2) 0.049(3) 0.007(2) 0.019(2) 0.0000(18) _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 O1 2.015(2) . ? Pt1 N1 2.040(3) . ? Pt1 S1 2.2181(8) . ? Pt1 Cl1 2.3118(8) . ? Cl2 C22 1.766(4) . ? Cl3 C22 1.758(4) . ? S1 O2 1.457(2) . ? S1 C20 1.772(4) . ? S1 C21 1.774(4) . ? O1 C1 1.307(4) . ? N1 C7 1.300(4) . ? N1 C8 1.451(4) . ? C1 C6 1.408(5) . ? C1 C2 1.415(5) . ? C2 C3 1.372(5) . ? C2 H2 0.9500 . ? C3 C4 1.394(5) . ? C3 H3 0.9500 . ? C4 C5 1.368(5) . ? C4 H4 0.9500 . ? C5 C6 1.412(5) . ? C5 H5 0.9500 . ? C6 C7 1.427(5) . ? C7 H7 0.9500 . ? C8 C13 1.398(5) . ? C8 C9 1.399(5) . ? C9 C10 1.397(5) . ? C9 C14 1.519(5) . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 C12 1.382(5) . ? C11 H11 0.9500 . ? C12 C13 1.393(5) . ? C12 H12 0.9500 . ? C13 C17 1.513(5) . ? C14 C16 1.527(6) . ? C14 C15 1.531(5) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.526(5) . ? C17 C19 1.528(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? 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 Pt1 N1 90.26(10) . . ? O1 Pt1 S1 172.36(7) . . ? N1 Pt1 S1 97.35(7) . . ? O1 Pt1 Cl1 83.94(7) . . ? N1 Pt1 Cl1 174.13(8) . . ? S1 Pt1 Cl1 88.46(3) . . ? O2 S1 C20 106.60(17) . . ? O2 S1 C21 107.85(17) . . ? C20 S1 C21 102.25(19) . . ? O2 S1 Pt1 119.97(10) . . ? C20 S1 Pt1 110.28(13) . . ? C21 S1 Pt1 108.43(13) . . ? C1 O1 Pt1 126.1(2) . . ? C7 N1 C8 114.9(3) . . ? C7 N1 Pt1 121.8(2) . . ? C8 N1 Pt1 123.3(2) . . ? O1 C1 C6 124.1(3) . . ? O1 C1 C2 117.8(3) . . ? C6 C1 C2 118.0(3) . . ? C3 C2 C1 120.6(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 121.5(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.7(3) . . ? C1 C6 C7 122.5(3) . . ? C5 C6 C7 117.7(3) . . ? N1 C7 C6 129.8(3) . . ? N1 C7 H7 115.1 . . ? C6 C7 H7 115.1 . . ? C13 C8 C9 123.2(3) . . ? C13 C8 N1 118.7(3) . . ? C9 C8 N1 118.1(3) . . ? C10 C9 C8 117.2(3) . . ? C10 C9 C14 120.2(3) . . ? C8 C9 C14 122.5(3) . . ? C11 C10 C9 121.0(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 121.6(3) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C8 116.8(3) . . ? C12 C13 C17 119.9(3) . . ? C8 C13 C17 123.3(3) . . ? C9 C14 C16 109.4(3) . . ? C9 C14 C15 112.7(3) . . ? C16 C14 C15 110.0(3) . . ? C9 C14 H14 108.2 . . ? C16 C14 H14 108.2 . . ? C15 C14 H14 108.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C18 112.1(3) . . ? C13 C17 C19 111.0(3) . . ? C18 C17 C19 110.0(3) . . ? C13 C17 H17 107.9 . . ? C18 C17 H17 107.9 . . ? C19 C17 H17 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S1 C20 H20A 109.5 . . ? S1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S1 C21 H21A 109.5 . . ? S1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Cl3 C22 Cl2 110.5(2) . . ? Cl3 C22 H22A 109.5 . . ? Cl2 C22 H22A 109.5 . . ? Cl3 C22 H22B 109.5 . . ? Cl2 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? 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 O1 Pt1 S1 O2 -167.7(6) . . . . ? N1 Pt1 S1 O2 7.80(15) . . . . ? Cl1 Pt1 S1 O2 -173.08(14) . . . . ? O1 Pt1 S1 C20 -43.3(6) . . . . ? N1 Pt1 S1 C20 132.19(16) . . . . ? Cl1 Pt1 S1 C20 -48.69(15) . . . . ? O1 Pt1 S1 C21 67.9(6) . . . . ? N1 Pt1 S1 C21 -116.61(16) . . . . ? Cl1 Pt1 S1 C21 62.51(14) . . . . ? N1 Pt1 O1 C1 -25.0(3) . . . . ? S1 Pt1 O1 C1 150.5(4) . . . . ? Cl1 Pt1 O1 C1 155.9(3) . . . . ? O1 Pt1 N1 C7 16.1(3) . . . . ? S1 Pt1 N1 C7 -163.4(2) . . . . ? Cl1 Pt1 N1 C7 25.2(9) . . . . ? O1 Pt1 N1 C8 -161.6(2) . . . . ? S1 Pt1 N1 C8 19.0(2) . . . . ? Cl1 Pt1 N1 C8 -152.4(6) . . . . ? Pt1 O1 C1 C6 19.2(5) . . . . ? Pt1 O1 C1 C2 -162.8(2) . . . . ? O1 C1 C2 C3 179.9(3) . . . . ? C6 C1 C2 C3 -2.0(5) . . . . ? C1 C2 C3 C4 1.2(5) . . . . ? C2 C3 C4 C5 0.6(6) . . . . ? C3 C4 C5 C6 -1.6(6) . . . . ? O1 C1 C6 C5 179.0(3) . . . . ? C2 C1 C6 C5 1.1(5) . . . . ? O1 C1 C6 C7 3.1(5) . . . . ? C2 C1 C6 C7 -174.8(3) . . . . ? C4 C5 C6 C1 0.7(5) . . . . ? C4 C5 C6 C7 176.8(3) . . . . ? C8 N1 C7 C6 175.8(3) . . . . ? Pt1 N1 C7 C6 -2.0(5) . . . . ? C1 C6 C7 N1 -12.5(6) . . . . ? C5 C6 C7 N1 171.5(3) . . . . ? C7 N1 C8 C13 77.5(4) . . . . ? Pt1 N1 C8 C13 -104.7(3) . . . . ? C7 N1 C8 C9 -101.7(3) . . . . ? Pt1 N1 C8 C9 76.1(3) . . . . ? C13 C8 C9 C10 0.3(5) . . . . ? N1 C8 C9 C10 179.6(3) . . . . ? C13 C8 C9 C14 -176.4(3) . . . . ? N1 C8 C9 C14 2.8(5) . . . . ? C8 C9 C10 C11 0.3(5) . . . . ? C14 C9 C10 C11 177.1(3) . . . . ? C9 C10 C11 C12 -0.9(5) . . . . ? C10 C11 C12 C13 1.0(5) . . . . ? C11 C12 C13 C8 -0.4(5) . . . . ? C11 C12 C13 C17 178.8(3) . . . . ? C9 C8 C13 C12 -0.2(5) . . . . ? N1 C8 C13 C12 -179.5(3) . . . . ? C9 C8 C13 C17 -179.4(3) . . . . ? N1 C8 C13 C17 1.4(5) . . . . ? C10 C9 C14 C16 -86.3(4) . . . . ? C8 C9 C14 C16 90.4(4) . . . . ? C10 C9 C14 C15 36.5(5) . . . . ? C8 C9 C14 C15 -146.9(3) . . . . ? C12 C13 C17 C18 -49.9(5) . . . . ? C8 C13 C17 C18 129.2(4) . . . . ? C12 C13 C17 C19 73.5(4) . . . . ? C8 C13 C17 C19 -107.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.272 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.122 _database_code_depnum_ccdc_archive 'CCDC 931185' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1b _chemical_melting_point 194 _chemical_formula_moiety 'C21 H28 Cl N O2 Pt S' _chemical_formula_sum 'C21 H28 Cl N O2 Pt S' _chemical_formula_weight 589.04 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' S S 0.1246 0.1234 '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 _symmetry_space_group_name_Hall -P2ybc 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 16.4013(18) _cell_length_b 19.269(2) _cell_length_c 14.4597(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.062(2) _cell_angle_gamma 90.00 _cell_volume 4569.0(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 106417 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 28.35 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 6.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6411 _exptl_absorpt_correction_T_max 0.7813 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; Half sphere of data collected using SAINT strategy (Bruker, 2006). Crystal to detector distance = 50mm; combination of \f and \w scans of 0.5\%, 20s per \%, 2 iterations. ; _diffrn_ambient_temperature 173(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 'Bruker Kappa Duo Apex II Diffractometer' _diffrn_measurement_method '0.5\% \f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 106417 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.35 _reflns_number_total 11388 _reflns_number_gt 9108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT program (Bruker, 2006)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2001)' _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^)+(0.0152P)^2^+4.9542P] 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 11388 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0504 _refine_ls_wR_factor_gt 0.0460 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1A Pt 0.279124(7) 0.345491(7) 0.041971(8) 0.02350(4) Uani 1 1 d . . . Cl1A Cl 0.34329(6) 0.26816(6) 0.13973(7) 0.0511(3) Uani 1 1 d . . . S1A S 0.39114(5) 0.34642(5) -0.04245(6) 0.0334(2) Uani 1 1 d . . . O1A O 0.23423(13) 0.41822(12) -0.04246(16) 0.0283(5) Uani 1 1 d . . . N1A N 0.17272(16) 0.33961(14) 0.11071(18) 0.0212(5) Uani 1 1 d . . . C1A C 0.1562(2) 0.42991(16) -0.0586(2) 0.0224(7) Uani 1 1 d . . . O2A O 0.46642(16) 0.37319(19) -0.0006(2) 0.0573(9) Uani 1 1 d . . . C2A C 0.1363(2) 0.47432(17) -0.1328(2) 0.0268(7) Uani 1 1 d . . . H2A H 0.1785 0.4975 -0.1646 0.032 Uiso 1 1 calc R . . C3A C 0.0568(2) 0.48446(18) -0.1596(3) 0.0324(8) Uani 1 1 d . . . H3A H 0.0448 0.5140 -0.2107 0.039 Uiso 1 1 calc R . . C4A C -0.0070(2) 0.4524(2) -0.1136(3) 0.0354(9) Uani 1 1 d . . . H4A H -0.0618 0.4579 -0.1349 0.042 Uiso 1 1 calc R . . C5A C 0.0108(2) 0.41279(18) -0.0370(2) 0.0300(8) Uani 1 1 d . . . H5A H -0.0325 0.3929 -0.0032 0.036 Uiso 1 1 calc R . . C6A C 0.09220(19) 0.40103(16) -0.0075(2) 0.0208(7) Uani 1 1 d . . . C7A C 0.1048(2) 0.36267(16) 0.0771(2) 0.0219(7) Uani 1 1 d . . . H7A H 0.0575 0.3534 0.1121 0.026 Uiso 1 1 calc R . . C8A C 0.16747(19) 0.30581(17) 0.2007(2) 0.0223(7) Uani 1 1 d . . . C9A C 0.1481(2) 0.23485(17) 0.2042(2) 0.0234(7) Uani 1 1 d . . . C10A C 0.1363(2) 0.20582(18) 0.2901(2) 0.0291(8) Uani 1 1 d . . . H10A H 0.1200 0.1586 0.2946 0.035 Uiso 1 1 calc R . . C11A C 0.1478(2) 0.24444(19) 0.3697(2) 0.0327(8) Uani 1 1 d . . . H11A H 0.1397 0.2236 0.4283 0.039 Uiso 1 1 calc R . . C12A C 0.1709(2) 0.31273(19) 0.3646(2) 0.0317(8) Uani 1 1 d . . . H12A H 0.1798 0.3384 0.4200 0.038 Uiso 1 1 calc R . . C13A C 0.1814(2) 0.34506(17) 0.2794(2) 0.0276(7) Uani 1 1 d . . . C14A C 0.1387(2) 0.19045(18) 0.1179(2) 0.0291(8) Uani 1 1 d . . . H14A H 0.1612 0.2174 0.0651 0.035 Uiso 1 1 calc R . . C15A C 0.1876(3) 0.1232(2) 0.1263(3) 0.0458(11) Uani 1 1 d . . . H15A H 0.1802 0.0958 0.0697 0.069 Uiso 1 1 calc R . . H15B H 0.1684 0.0964 0.1793 0.069 Uiso 1 1 calc R . . H15C H 0.2455 0.1342 0.1354 0.069 Uiso 1 1 calc R . . C16A C 0.0501(3) 0.1749(2) 0.0949(3) 0.0529(12) Uani 1 1 d . . . H16A H 0.0467 0.1463 0.0389 0.079 Uiso 1 1 calc R . . H16B H 0.0206 0.2185 0.0844 0.079 Uiso 1 1 calc R . . H16C H 0.0258 0.1498 0.1464 0.079 Uiso 1 1 calc R . . C17A C 0.2080(3) 0.42040(19) 0.2764(3) 0.0370(9) Uani 1 1 d . . . H17A H 0.2110 0.4344 0.2099 0.044 Uiso 1 1 calc R . . C18A C 0.1470(3) 0.4682(2) 0.3228(3) 0.0529(12) Uani 1 1 d . . . H18A H 0.1660 0.5163 0.3188 0.079 Uiso 1 1 calc R . . H18B H 0.1422 0.4550 0.3880 0.079 Uiso 1 1 calc R . . H18C H 0.0937 0.4639 0.2916 0.079 Uiso 1 1 calc R . . C19A C 0.2931(3) 0.4284(2) 0.3196(4) 0.0622(14) Uani 1 1 d . . . H19A H 0.3097 0.4772 0.3170 0.093 Uiso 1 1 calc R . . H19B H 0.3318 0.3999 0.2854 0.093 Uiso 1 1 calc R . . H19C H 0.2923 0.4131 0.3843 0.093 Uiso 1 1 calc R . . C20A C 0.4089(3) 0.2616(3) -0.0839(3) 0.0610(14) Uani 1 1 d . . . H20A H 0.4199 0.2305 -0.0316 0.092 Uiso 1 1 calc R . . H20B H 0.4560 0.2620 -0.1246 0.092 Uiso 1 1 calc R . . H20C H 0.3607 0.2453 -0.1185 0.092 Uiso 1 1 calc R . . C21A C 0.3738(3) 0.3903(3) -0.1482(3) 0.0538(13) Uani 1 1 d . . . H21A H 0.3629 0.4395 -0.1359 0.081 Uiso 1 1 calc R . . H21B H 0.3267 0.3697 -0.1806 0.081 Uiso 1 1 calc R . . H21C H 0.4221 0.3862 -0.1867 0.081 Uiso 1 1 calc R . . Pt1B Pt 0.218393(7) 0.662183(6) -0.192135(8) 0.02016(3) Uani 1 1 d . . . Cl1B Cl 0.15915(6) 0.73463(6) -0.08670(7) 0.0433(2) Uani 1 1 d . . . S1B S 0.10598(5) 0.67364(5) -0.27997(6) 0.02828(19) Uani 1 1 d . . . O1B O 0.25661(13) 0.59243(12) -0.28336(16) 0.0268(5) Uani 1 1 d . . . N1B N 0.32558(15) 0.65865(13) -0.11992(17) 0.0191(5) Uani 1 1 d . . . C1B C 0.3307(2) 0.56744(15) -0.2901(2) 0.0210(7) Uani 1 1 d . . . O2B O 0.02896(15) 0.64665(15) -0.2459(2) 0.0434(7) Uani 1 1 d . . . C2B C 0.3451(2) 0.52149(18) -0.3633(2) 0.0315(8) Uani 1 1 d . . . H2B H 0.3012 0.5088 -0.4036 0.038 Uiso 1 1 calc R . . C3B C 0.4211(2) 0.49453(19) -0.3779(3) 0.0373(9) Uani 1 1 d . . . H3B H 0.4292 0.4636 -0.4281 0.045 Uiso 1 1 calc R . . C4B C 0.4865(2) 0.5119(2) -0.3199(3) 0.0419(10) Uani 1 1 d . . . H4B H 0.5393 0.4938 -0.3309 0.050 Uiso 1 1 calc R . . C5B C 0.4739(2) 0.5557(2) -0.2467(3) 0.0340(8) Uani 1 1 d . . . H5B H 0.5184 0.5672 -0.2066 0.041 Uiso 1 1 calc R . . C6B C 0.3963(2) 0.58391(17) -0.2296(2) 0.0228(7) Uani 1 1 d . . . C7B C 0.38927(19) 0.62632(16) -0.1487(2) 0.0212(7) Uani 1 1 d . . . H7B H 0.4374 0.6313 -0.1117 0.025 Uiso 1 1 calc R . . C8B C 0.33649(18) 0.69374(16) -0.0311(2) 0.0184(6) Uani 1 1 d . . . C9B C 0.32756(19) 0.65427(16) 0.0493(2) 0.0226(7) Uani 1 1 d . . . C10B C 0.3409(2) 0.68779(18) 0.1334(2) 0.0274(7) Uani 1 1 d . . . H10B H 0.3356 0.6625 0.1893 0.033 Uiso 1 1 calc R . . C11B C 0.3617(2) 0.75739(18) 0.1370(2) 0.0288(8) Uani 1 1 d . . . H11B H 0.3708 0.7794 0.1951 0.035 Uiso 1 1 calc R . . C12B C 0.3692(2) 0.79474(18) 0.0565(2) 0.0275(7) Uani 1 1 d . . . H12B H 0.3841 0.8423 0.0597 0.033 Uiso 1 1 calc R . . C13B C 0.3554(2) 0.76420(17) -0.0291(2) 0.0230(7) Uani 1 1 d . . . C14B C 0.3043(2) 0.57838(17) 0.0482(2) 0.0256(7) Uani 1 1 d . . . H14B H 0.2990 0.5633 -0.0178 0.031 Uiso 1 1 calc R . . C15B C 0.3689(2) 0.53359(18) 0.0950(3) 0.0387(9) Uani 1 1 d . . . H15D H 0.3519 0.4849 0.0925 0.058 Uiso 1 1 calc R . . H15E H 0.3759 0.5479 0.1597 0.058 Uiso 1 1 calc R . . H15F H 0.4207 0.5390 0.0630 0.058 Uiso 1 1 calc R . . C16B C 0.2216(2) 0.5684(2) 0.0933(3) 0.0370(9) Uani 1 1 d . . . H16D H 0.2068 0.5191 0.0917 0.055 Uiso 1 1 calc R . . H16E H 0.1801 0.5954 0.0594 0.055 Uiso 1 1 calc R . . H16F H 0.2247 0.5843 0.1576 0.055 Uiso 1 1 calc R . . C17B C 0.3637(2) 0.80647(17) -0.1173(2) 0.0254(7) Uani 1 1 d . . . H17B H 0.3364 0.7800 -0.1687 0.031 Uiso 1 1 calc R . . C18B C 0.3216(3) 0.8768(2) -0.1103(3) 0.0452(11) Uani 1 1 d . . . H18D H 0.3282 0.9024 -0.1682 0.068 Uiso 1 1 calc R . . H18E H 0.3461 0.9033 -0.0590 0.068 Uiso 1 1 calc R . . H18F H 0.2634 0.8699 -0.0991 0.068 Uiso 1 1 calc R . . C19B C 0.4530(2) 0.8155(2) -0.1417(3) 0.0424(10) Uani 1 1 d . . . H19D H 0.4568 0.8427 -0.1988 0.064 Uiso 1 1 calc R . . H19E H 0.4779 0.7698 -0.1509 0.064 Uiso 1 1 calc R . . H19F H 0.4817 0.8398 -0.0913 0.064 Uiso 1 1 calc R . . C20B C 0.0933(3) 0.7626(2) -0.3089(3) 0.0498(11) Uani 1 1 d . . . H20D H 0.0839 0.7895 -0.2525 0.075 Uiso 1 1 calc R . . H20E H 0.0465 0.7678 -0.3514 0.075 Uiso 1 1 calc R . . H20F H 0.1426 0.7797 -0.3387 0.075 Uiso 1 1 calc R . . C21B C 0.1219(3) 0.6392(3) -0.3915(3) 0.0539(12) Uani 1 1 d . . . H21D H 0.1300 0.5889 -0.3870 0.081 Uiso 1 1 calc R . . H21E H 0.1703 0.6606 -0.4180 0.081 Uiso 1 1 calc R . . H21F H 0.0742 0.6489 -0.4312 0.081 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 Pt1A 0.02027(6) 0.03231(7) 0.01791(6) 0.00379(6) -0.00022(5) 0.00059(5) Cl1A 0.0334(5) 0.0772(8) 0.0429(6) 0.0302(6) 0.0055(4) 0.0207(5) S1A 0.0215(4) 0.0528(6) 0.0260(4) 0.0044(4) 0.0013(3) 0.0007(4) O1A 0.0257(12) 0.0309(13) 0.0283(13) 0.0110(11) 0.0002(10) -0.0026(10) N1A 0.0237(13) 0.0233(14) 0.0168(13) 0.0012(11) 0.0016(10) 0.0020(11) C1A 0.0273(17) 0.0195(16) 0.0204(17) -0.0016(13) 0.0010(13) 0.0003(13) O2A 0.0236(14) 0.098(3) 0.0497(19) 0.0030(18) -0.0041(13) -0.0131(15) C2A 0.0329(18) 0.0211(17) 0.0265(18) 0.0045(14) 0.0001(14) -0.0014(14) C3A 0.040(2) 0.0281(19) 0.0293(19) 0.0104(16) -0.0028(16) 0.0060(16) C4A 0.0270(18) 0.040(2) 0.039(2) 0.0063(18) -0.0070(16) 0.0082(16) C5A 0.0262(17) 0.0325(19) 0.031(2) 0.0049(16) 0.0013(15) 0.0054(15) C6A 0.0248(16) 0.0206(16) 0.0169(16) 0.0013(13) 0.0022(12) 0.0037(13) C7A 0.0257(16) 0.0218(16) 0.0185(16) 0.0006(13) 0.0039(13) 0.0011(13) C8A 0.0243(16) 0.0264(17) 0.0164(16) 0.0064(13) 0.0009(13) 0.0015(13) C9A 0.0276(17) 0.0271(18) 0.0154(16) 0.0023(13) -0.0031(13) 0.0006(14) C10A 0.041(2) 0.0212(17) 0.0250(18) 0.0039(14) -0.0029(15) -0.0025(15) C11A 0.047(2) 0.035(2) 0.0164(17) 0.0059(15) -0.0023(15) -0.0088(17) C12A 0.045(2) 0.0317(19) 0.0179(17) -0.0004(15) -0.0017(15) -0.0102(17) C13A 0.0368(19) 0.0262(18) 0.0198(17) 0.0016(14) 0.0018(14) -0.0076(15) C14A 0.042(2) 0.0253(18) 0.0202(17) -0.0022(14) -0.0006(15) 0.0064(16) C15A 0.070(3) 0.035(2) 0.031(2) -0.0034(18) -0.003(2) 0.019(2) C16A 0.045(2) 0.062(3) 0.051(3) -0.024(2) -0.014(2) 0.005(2) C17A 0.060(3) 0.0278(19) 0.0231(19) 0.0006(16) 0.0004(17) -0.0112(18) C18A 0.068(3) 0.032(2) 0.058(3) 0.004(2) -0.008(2) -0.001(2) C19A 0.051(3) 0.045(3) 0.091(4) -0.004(3) 0.003(3) -0.024(2) C20A 0.057(3) 0.065(3) 0.062(3) -0.005(3) 0.019(2) 0.017(3) C21A 0.042(2) 0.088(4) 0.032(2) 0.023(2) 0.0135(19) 0.005(2) Pt1B 0.01941(6) 0.02365(6) 0.01741(6) 0.00111(5) -0.00006(4) 0.00181(5) Cl1B 0.0329(5) 0.0591(6) 0.0378(5) -0.0171(5) -0.0012(4) 0.0196(5) S1B 0.0214(4) 0.0356(5) 0.0277(4) 0.0075(4) -0.0029(3) 0.0005(3) O1B 0.0243(12) 0.0304(13) 0.0254(13) -0.0107(10) -0.0034(10) 0.0007(10) N1B 0.0241(13) 0.0187(13) 0.0144(12) -0.0005(11) -0.0008(10) 0.0008(11) C1B 0.0304(17) 0.0142(15) 0.0184(16) 0.0027(12) 0.0018(13) 0.0005(13) O2B 0.0241(13) 0.0537(18) 0.0523(18) 0.0164(14) -0.0007(12) -0.0041(12) C2B 0.040(2) 0.0271(18) 0.0274(19) -0.0081(16) -0.0019(15) -0.0018(16) C3B 0.049(2) 0.031(2) 0.032(2) -0.0118(17) 0.0030(18) 0.0091(18) C4B 0.035(2) 0.046(2) 0.046(2) -0.014(2) 0.0036(18) 0.0144(18) C5B 0.0300(19) 0.041(2) 0.031(2) -0.0075(17) -0.0008(15) 0.0082(16) C6B 0.0278(17) 0.0209(16) 0.0199(16) 0.0011(13) 0.0027(13) -0.0003(13) C7B 0.0232(16) 0.0213(16) 0.0188(16) -0.0007(13) -0.0042(12) 0.0000(13) C8B 0.0197(15) 0.0212(16) 0.0142(15) -0.0032(12) 0.0000(12) 0.0020(12) C9B 0.0228(15) 0.0231(17) 0.0220(16) 0.0007(14) 0.0002(12) -0.0014(13) C10B 0.0353(19) 0.0293(18) 0.0176(17) 0.0025(14) 0.0006(14) -0.0041(15) C11B 0.039(2) 0.0300(19) 0.0173(17) -0.0044(14) 0.0013(15) -0.0021(16) C12B 0.0374(19) 0.0216(17) 0.0235(18) -0.0017(14) 0.0009(15) -0.0018(15) C13B 0.0265(17) 0.0234(17) 0.0193(16) 0.0001(13) 0.0005(13) 0.0019(13) C14B 0.0351(18) 0.0228(17) 0.0189(17) -0.0021(14) -0.0010(14) -0.0057(14) C15B 0.038(2) 0.0223(18) 0.056(3) 0.0062(18) -0.0021(19) -0.0023(16) C16B 0.035(2) 0.034(2) 0.043(2) 0.0040(18) 0.0042(17) -0.0077(17) C17B 0.0377(19) 0.0190(16) 0.0197(17) 0.0031(13) 0.0011(14) 0.0015(14) C18B 0.077(3) 0.028(2) 0.030(2) 0.0087(17) 0.005(2) 0.016(2) C19B 0.044(2) 0.047(2) 0.036(2) 0.0114(19) 0.0071(18) -0.0050(19) C20B 0.048(3) 0.042(2) 0.059(3) 0.023(2) -0.009(2) 0.004(2) C21B 0.042(2) 0.086(4) 0.032(2) -0.011(2) -0.0165(19) 0.010(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 Pt1A O1A 1.991(2) . ? Pt1A N1A 2.028(3) . ? Pt1A S1A 2.2247(9) . ? Pt1A Cl1A 2.2959(10) . ? S1A O2A 1.459(3) . ? S1A C21A 1.766(4) . ? S1A C20A 1.767(5) . ? O1A C1A 1.315(4) . ? N1A C7A 1.286(4) . ? N1A C8A 1.459(4) . ? C1A C2A 1.405(4) . ? C1A C6A 1.410(4) . ? C2A C3A 1.368(5) . ? C2A H2A 0.9500 . ? C3A C4A 1.394(5) . ? C3A H3A 0.9500 . ? C4A C5A 1.372(5) . ? C4A H4A 0.9500 . ? C5A C6A 1.413(4) . ? C5A H5A 0.9500 . ? C6A C7A 1.441(4) . ? C7A H7A 0.9500 . ? C8A C13A 1.382(5) . ? C8A C9A 1.405(5) . ? C9A C10A 1.379(4) . ? C9A C14A 1.519(4) . ? C10A C11A 1.380(5) . ? C10A H10A 0.9500 . ? C11A C12A 1.371(5) . ? C11A H11A 0.9500 . ? C12A C13A 1.394(5) . ? C12A H12A 0.9500 . ? C13A C17A 1.516(5) . ? C14A C16A 1.514(5) . ? C14A C15A 1.527(5) . ? C14A H14A 1.0000 . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A C18A 1.524(6) . ? C17A C19A 1.527(6) . ? C17A H17A 1.0000 . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? Pt1B O1B 1.992(2) . ? Pt1B N1B 2.029(3) . ? Pt1B S1B 2.2304(8) . ? Pt1B Cl1B 2.2961(9) . ? S1B O2B 1.460(3) . ? S1B C21B 1.768(4) . ? S1B C20B 1.776(4) . ? O1B C1B 1.312(4) . ? N1B C7B 1.292(4) . ? N1B C8B 1.459(4) . ? C1B C2B 1.403(4) . ? C1B C6B 1.410(4) . ? C2B C3B 1.371(5) . ? C2B H2B 0.9500 . ? C3B C4B 1.390(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.372(5) . ? C4B H4B 0.9500 . ? C5B C6B 1.411(5) . ? C5B H5B 0.9500 . ? C6B C7B 1.433(4) . ? C7B H7B 0.9500 . ? C8B C13B 1.393(4) . ? C8B C9B 1.399(4) . ? C9B C10B 1.391(4) . ? C9B C14B 1.511(4) . ? C10B C11B 1.384(5) . ? C10B H10B 0.9500 . ? C11B C12B 1.376(5) . ? C11B H11B 0.9500 . ? C12B C13B 1.386(4) . ? C12B H12B 0.9500 . ? C13B C17B 1.522(4) . ? C14B C15B 1.515(5) . ? C14B C16B 1.529(5) . ? C14B H14B 1.0000 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B C19B 1.523(5) . ? C17B C18B 1.525(5) . ? C17B H17B 1.0000 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? 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 O1A Pt1A N1A 91.61(10) . . ? O1A Pt1A S1A 87.58(7) . . ? N1A Pt1A S1A 175.25(8) . . ? O1A Pt1A Cl1A 174.03(7) . . ? N1A Pt1A Cl1A 92.91(8) . . ? S1A Pt1A Cl1A 88.24(4) . . ? O2A S1A C21A 108.1(2) . . ? O2A S1A C20A 108.9(2) . . ? C21A S1A C20A 100.0(2) . . ? O2A S1A Pt1A 118.44(13) . . ? C21A S1A Pt1A 110.93(14) . . ? C20A S1A Pt1A 108.78(16) . . ? C1A O1A Pt1A 125.2(2) . . ? C7A N1A C8A 115.2(3) . . ? C7A N1A Pt1A 122.9(2) . . ? C8A N1A Pt1A 121.9(2) . . ? O1A C1A C2A 116.8(3) . . ? O1A C1A C6A 124.8(3) . . ? C2A C1A C6A 118.4(3) . . ? C3A C2A C1A 120.7(3) . . ? C3A C2A H2A 119.7 . . ? C1A C2A H2A 119.7 . . ? C2A C3A C4A 121.4(3) . . ? C2A C3A H3A 119.3 . . ? C4A C3A H3A 119.3 . . ? C5A C4A C3A 118.8(3) . . ? C5A C4A H4A 120.6 . . ? C3A C4A H4A 120.6 . . ? C4A C5A C6A 121.3(3) . . ? C4A C5A H5A 119.4 . . ? C6A C5A H5A 119.4 . . ? C1A C6A C5A 119.2(3) . . ? C1A C6A C7A 123.4(3) . . ? C5A C6A C7A 117.3(3) . . ? N1A C7A C6A 127.4(3) . . ? N1A C7A H7A 116.3 . . ? C6A C7A H7A 116.3 . . ? C13A C8A C9A 122.5(3) . . ? C13A C8A N1A 118.6(3) . . ? C9A C8A N1A 118.9(3) . . ? C10A C9A C8A 117.6(3) . . ? C10A C9A C14A 119.8(3) . . ? C8A C9A C14A 122.6(3) . . ? C9A C10A C11A 120.8(3) . . ? C9A C10A H10A 119.6 . . ? C11A C10A H10A 119.6 . . ? C12A C11A C10A 120.4(3) . . ? C12A C11A H11A 119.8 . . ? C10A C11A H11A 119.8 . . ? C11A C12A C13A 121.0(3) . . ? C11A C12A H12A 119.5 . . ? C13A C12A H12A 119.5 . . ? C8A C13A C12A 117.5(3) . . ? C8A C13A C17A 122.9(3) . . ? C12A C13A C17A 119.6(3) . . ? C16A C14A C9A 112.1(3) . . ? C16A C14A C15A 110.4(3) . . ? C9A C14A C15A 111.5(3) . . ? C16A C14A H14A 107.5 . . ? C9A C14A H14A 107.5 . . ? C15A C14A H14A 107.5 . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14A C16A H16A 109.5 . . ? C14A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C14A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C13A C17A C18A 112.0(3) . . ? C13A C17A C19A 110.2(3) . . ? C18A C17A C19A 111.1(3) . . ? C13A C17A H17A 107.8 . . ? C18A C17A H17A 107.8 . . ? C19A C17A H17A 107.8 . . ? C17A C18A H18A 109.5 . . ? C17A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5 . . ? C17A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? S1A C20A H20A 109.5 . . ? S1A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? S1A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? S1A C21A H21A 109.5 . . ? S1A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? S1A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? O1B Pt1B N1B 92.17(9) . . ? O1B Pt1B S1B 87.52(7) . . ? N1B Pt1B S1B 174.58(7) . . ? O1B Pt1B Cl1B 172.70(7) . . ? N1B Pt1B Cl1B 92.98(7) . . ? S1B Pt1B Cl1B 87.85(3) . . ? O2B S1B C21B 108.5(2) . . ? O2B S1B C20B 108.99(19) . . ? C21B S1B C20B 99.6(2) . . ? O2B S1B Pt1B 118.92(12) . . ? C21B S1B Pt1B 110.35(14) . . ? C20B S1B Pt1B 108.74(15) . . ? C1B O1B Pt1B 126.8(2) . . ? C7B N1B C8B 114.8(3) . . ? C7B N1B Pt1B 123.3(2) . . ? C8B N1B Pt1B 121.88(19) . . ? O1B C1B C2B 117.2(3) . . ? O1B C1B C6B 124.6(3) . . ? C2B C1B C6B 118.2(3) . . ? C3B C2B C1B 121.5(3) . . ? C3B C2B H2B 119.3 . . ? C1B C2B H2B 119.3 . . ? C2B C3B C4B 120.6(3) . . ? C2B C3B H3B 119.7 . . ? C4B C3B H3B 119.7 . . ? C5B C4B C3B 119.2(3) . . ? C5B C4B H4B 120.4 . . ? C3B C4B H4B 120.4 . . ? C4B C5B C6B 121.5(3) . . ? C4B C5B H5B 119.3 . . ? C6B C5B H5B 119.3 . . ? C1B C6B C5B 119.0(3) . . ? C1B C6B C7B 124.2(3) . . ? C5B C6B C7B 116.7(3) . . ? N1B C7B C6B 128.0(3) . . ? N1B C7B H7B 116.0 . . ? C6B C7B H7B 116.0 . . ? C13B C8B C9B 122.6(3) . . ? C13B C8B N1B 119.6(3) . . ? C9B C8B N1B 117.8(3) . . ? C10B C9B C8B 117.2(3) . . ? C10B C9B C14B 119.6(3) . . ? C8B C9B C14B 123.2(3) . . ? C11B C10B C9B 121.2(3) . . ? C11B C10B H10B 119.4 . . ? C9B C10B H10B 119.4 . . ? C12B C11B C10B 120.0(3) . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C11B C12B C13B 121.2(3) . . ? C11B C12B H12B 119.4 . . ? C13B C12B H12B 119.4 . . ? C12B C13B C8B 117.7(3) . . ? C12B C13B C17B 120.4(3) . . ? C8B C13B C17B 121.8(3) . . ? C9B C14B C15B 111.9(3) . . ? C9B C14B C16B 110.1(3) . . ? C15B C14B C16B 110.9(3) . . ? C9B C14B H14B 107.9 . . ? C15B C14B H14B 107.9 . . ? C16B C14B H14B 107.9 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14B C16B H16D 109.5 . . ? C14B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C14B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C13B C17B C19B 110.9(3) . . ? C13B C17B C18B 111.8(3) . . ? C19B C17B C18B 110.6(3) . . ? C13B C17B H17B 107.8 . . ? C19B C17B H17B 107.8 . . ? C18B C17B H17B 107.8 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? S1B C20B H20D 109.5 . . ? S1B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? S1B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? S1B C21B H21D 109.5 . . ? S1B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? S1B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? 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 O1A Pt1A S1A O2A 111.79(19) . . . . ? N1A Pt1A S1A O2A -168.0(9) . . . . ? Cl1A Pt1A S1A O2A -63.95(17) . . . . ? O1A Pt1A S1A C21A -14.1(2) . . . . ? N1A Pt1A S1A C21A 66.1(10) . . . . ? Cl1A Pt1A S1A C21A 170.15(19) . . . . ? O1A Pt1A S1A C20A -123.2(2) . . . . ? N1A Pt1A S1A C20A -43.0(10) . . . . ? Cl1A Pt1A S1A C20A 61.04(19) . . . . ? N1A Pt1A O1A C1A -21.0(3) . . . . ? S1A Pt1A O1A C1A 154.3(3) . . . . ? Cl1A Pt1A O1A C1A -160.1(6) . . . . ? O1A Pt1A N1A C7A 18.1(3) . . . . ? S1A Pt1A N1A C7A -61.9(11) . . . . ? Cl1A Pt1A N1A C7A -165.8(3) . . . . ? O1A Pt1A N1A C8A -164.7(2) . . . . ? S1A Pt1A N1A C8A 115.3(9) . . . . ? Cl1A Pt1A N1A C8A 11.4(2) . . . . ? Pt1A O1A C1A C2A -168.4(2) . . . . ? Pt1A O1A C1A C6A 11.3(5) . . . . ? O1A C1A C2A C3A 174.2(3) . . . . ? C6A C1A C2A C3A -5.6(5) . . . . ? C1A C2A C3A C4A 1.3(6) . . . . ? C2A C3A C4A C5A 3.3(6) . . . . ? C3A C4A C5A C6A -3.5(6) . . . . ? O1A C1A C6A C5A -174.4(3) . . . . ? C2A C1A C6A C5A 5.3(5) . . . . ? O1A C1A C6A C7A 9.0(5) . . . . ? C2A C1A C6A C7A -171.2(3) . . . . ? C4A C5A C6A C1A -0.8(5) . . . . ? C4A C5A C6A C7A 175.9(3) . . . . ? C8A N1A C7A C6A 176.6(3) . . . . ? Pt1A N1A C7A C6A -6.0(5) . . . . ? C1A C6A C7A N1A -11.9(5) . . . . ? C5A C6A C7A N1A 171.5(3) . . . . ? C7A N1A C8A C13A -93.4(4) . . . . ? Pt1A N1A C8A C13A 89.2(3) . . . . ? C7A N1A C8A C9A 86.3(4) . . . . ? Pt1A N1A C8A C9A -91.1(3) . . . . ? C13A C8A C9A C10A 5.5(5) . . . . ? N1A C8A C9A C10A -174.2(3) . . . . ? C13A C8A C9A C14A -175.5(3) . . . . ? N1A C8A C9A C14A 4.7(5) . . . . ? C8A C9A C10A C11A -3.7(5) . . . . ? C14A C9A C10A C11A 177.3(3) . . . . ? C9A C10A C11A C12A 0.4(6) . . . . ? C10A C11A C12A C13A 1.4(6) . . . . ? C9A C8A C13A C12A -3.8(5) . . . . ? N1A C8A C13A C12A 175.9(3) . . . . ? C9A C8A C13A C17A 175.7(3) . . . . ? N1A C8A C13A C17A -4.6(5) . . . . ? C11A C12A C13A C8A 0.3(6) . . . . ? C11A C12A C13A C17A -179.3(4) . . . . ? C10A C9A C14A C16A 74.2(4) . . . . ? C8A C9A C14A C16A -104.8(4) . . . . ? C10A C9A C14A C15A -50.2(5) . . . . ? C8A C9A C14A C15A 130.8(4) . . . . ? C8A C13A C17A C18A 120.1(4) . . . . ? C12A C13A C17A C18A -60.4(5) . . . . ? C8A C13A C17A C19A -115.7(4) . . . . ? C12A C13A C17A C19A 63.8(5) . . . . ? O1B Pt1B S1B O2B 109.30(16) . . . . ? N1B Pt1B S1B O2B -163.9(8) . . . . ? Cl1B Pt1B S1B O2B -65.05(15) . . . . ? O1B Pt1B S1B C21B -17.0(2) . . . . ? N1B Pt1B S1B C21B 69.8(8) . . . . ? Cl1B Pt1B S1B C21B 168.65(19) . . . . ? O1B Pt1B S1B C20B -125.24(18) . . . . ? N1B Pt1B S1B C20B -38.5(8) . . . . ? Cl1B Pt1B S1B C20B 60.40(17) . . . . ? N1B Pt1B O1B C1B -8.2(3) . . . . ? S1B Pt1B O1B C1B 166.4(3) . . . . ? Cl1B Pt1B O1B C1B -143.0(5) . . . . ? O1B Pt1B N1B C7B 8.9(3) . . . . ? S1B Pt1B N1B C7B -77.7(9) . . . . ? Cl1B Pt1B N1B C7B -176.3(2) . . . . ? O1B Pt1B N1B C8B -171.9(2) . . . . ? S1B Pt1B N1B C8B 101.5(8) . . . . ? Cl1B Pt1B N1B C8B 2.9(2) . . . . ? Pt1B O1B C1B C2B -176.4(2) . . . . ? Pt1B O1B C1B C6B 3.1(4) . . . . ? O1B C1B C2B C3B 177.7(3) . . . . ? C6B C1B C2B C3B -1.8(5) . . . . ? C1B C2B C3B C4B 0.2(6) . . . . ? C2B C3B C4B C5B 1.1(6) . . . . ? C3B C4B C5B C6B -0.7(6) . . . . ? O1B C1B C6B C5B -177.4(3) . . . . ? C2B C1B C6B C5B 2.1(5) . . . . ? O1B C1B C6B C7B 4.7(5) . . . . ? C2B C1B C6B C7B -175.8(3) . . . . ? C4B C5B C6B C1B -0.9(5) . . . . ? C4B C5B C6B C7B 177.1(4) . . . . ? C8B N1B C7B C6B 175.8(3) . . . . ? Pt1B N1B C7B C6B -4.9(5) . . . . ? C1B C6B C7B N1B -3.6(5) . . . . ? C5B C6B C7B N1B 178.4(3) . . . . ? C7B N1B C8B C13B 96.4(3) . . . . ? Pt1B N1B C8B C13B -82.8(3) . . . . ? C7B N1B C8B C9B -83.4(4) . . . . ? Pt1B N1B C8B C9B 97.4(3) . . . . ? C13B C8B C9B C10B -1.9(5) . . . . ? N1B C8B C9B C10B 177.8(3) . . . . ? C13B C8B C9B C14B 177.9(3) . . . . ? N1B C8B C9B C14B -2.3(4) . . . . ? C8B C9B C10B C11B 0.3(5) . . . . ? C14B C9B C10B C11B -179.6(3) . . . . ? C9B C10B C11B C12B 0.3(5) . . . . ? C10B C11B C12B C13B 0.7(5) . . . . ? C11B C12B C13B C8B -2.2(5) . . . . ? C11B C12B C13B C17B 179.8(3) . . . . ? C9B C8B C13B C12B 2.9(5) . . . . ? N1B C8B C13B C12B -176.9(3) . . . . ? C9B C8B C13B C17B -179.1(3) . . . . ? N1B C8B C13B C17B 1.1(5) . . . . ? C10B C9B C14B C15B -59.7(4) . . . . ? C8B C9B C14B C15B 120.4(4) . . . . ? C10B C9B C14B C16B 64.1(4) . . . . ? C8B C9B C14B C16B -115.8(3) . . . . ? C12B C13B C17B C19B 78.3(4) . . . . ? C8B C13B C17B C19B -99.7(4) . . . . ? C12B C13B C17B C18B -45.7(4) . . . . ? C8B C13B C17B C18B 136.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.888 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 931186' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2 _chemical_melting_point 173 _chemical_formula_moiety 'C15 H16 Cl N O2 Pt S' _chemical_formula_sum 'C15 H16 Cl N O2 Pt S' _chemical_formula_weight 504.89 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' S S 0.1246 0.1234 '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' 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' _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 8.8183(2) _cell_length_b 10.1831(2) _cell_length_c 10.4630(2) _cell_angle_alpha 111.9260(10) _cell_angle_beta 93.0980(10) _cell_angle_gamma 111.1600(10) _cell_volume 793.23(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6569 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.73 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 9.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4332 _exptl_absorpt_correction_T_max 0.5282 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Kappa CCD diffractometer' _diffrn_measurement_method '1.2\% \f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6569 _diffrn_reflns_av_R_equivalents 0.0095 _diffrn_reflns_av_unetI/netI 0.0159 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.73 _reflns_number_total 3359 _reflns_number_gt 3223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT program (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2001)' _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^)+(0.0117P)^2^+1.1092P] 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 SHELXL _refine_ls_extinction_coef 0.00229(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3359 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0162 _refine_ls_R_factor_gt 0.0144 _refine_ls_wR_factor_ref 0.0330 _refine_ls_wR_factor_gt 0.0325 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.265699(12) 0.311595(10) 0.223653(10) 0.01880(5) Uani 1 1 d . . . Cl1 Cl 0.25503(9) 0.25267(8) 0.41559(7) 0.02850(14) Uani 1 1 d . . . S1 S 0.47776(8) 0.24635(7) 0.18748(6) 0.01920(12) Uani 1 1 d . . . O1 O 0.0904(2) 0.3922(2) 0.2815(2) 0.0284(4) Uani 1 1 d . . . O2 O 0.5653(2) 0.2770(2) 0.0796(2) 0.0271(4) Uani 1 1 d . . . N1 N 0.2481(3) 0.3524(2) 0.0490(2) 0.0193(4) Uani 1 1 d . . . C1 C 0.2095(3) 0.4640(3) 0.0495(3) 0.0220(5) Uani 1 1 d . . . H1 H 0.2136 0.4824 -0.0331 0.026 Uiso 1 1 calc R . . C2 C 0.1614(3) 0.5623(3) 0.1623(3) 0.0209(5) Uani 1 1 d . . . C3 C 0.1602(3) 0.6979(3) 0.1555(3) 0.0245(5) Uani 1 1 d . . . H3 H 0.2015 0.7257 0.0831 0.029 Uiso 1 1 calc R . . C4 C 0.1004(3) 0.7901(3) 0.2518(3) 0.0266(6) Uani 1 1 d . . . H4 H 0.1036 0.8829 0.2482 0.032 Uiso 1 1 calc R . . C5 C 0.0349(3) 0.7457(3) 0.3547(3) 0.0257(6) Uani 1 1 d . . . H5 H -0.0095 0.8077 0.4198 0.031 Uiso 1 1 calc R . . C6 C 0.0331(3) 0.6138(3) 0.3642(3) 0.0253(6) Uani 1 1 d . . . H6 H -0.0125 0.5862 0.4353 0.030 Uiso 1 1 calc R . . C7 C 0.0985(3) 0.5190(3) 0.2690(3) 0.0220(5) Uani 1 1 d . . . C8 C 0.2685(3) 0.2516(3) -0.0821(3) 0.0208(5) Uani 1 1 d . . . C9 C 0.3670(3) 0.3134(3) -0.1618(3) 0.0253(5) Uani 1 1 d . . . H9 H 0.4221 0.4227 -0.1304 0.030 Uiso 1 1 calc R . . C10 C 0.3842(4) 0.2139(4) -0.2878(3) 0.0327(7) Uani 1 1 d . . . H10 H 0.4538 0.2552 -0.3418 0.039 Uiso 1 1 calc R . . C11 C 0.3004(4) 0.0548(4) -0.3352(3) 0.0362(7) Uani 1 1 d . . . H11 H 0.3122 -0.0127 -0.4219 0.043 Uiso 1 1 calc R . . C12 C 0.1995(4) -0.0064(3) -0.2568(3) 0.0323(6) Uani 1 1 d . . . H12 H 0.1404 -0.1156 -0.2905 0.039 Uiso 1 1 calc R . . C13 C 0.1847(3) 0.0922(3) -0.1288(3) 0.0254(6) Uani 1 1 d . . . H13 H 0.1176 0.0507 -0.0736 0.031 Uiso 1 1 calc R . . C14 C 0.4172(4) 0.0488(3) 0.1542(3) 0.0281(6) Uani 1 1 d . . . H14A H 0.3322 -0.0171 0.0663 0.042 Uiso 1 1 calc R . . H14B H 0.3715 0.0308 0.2325 0.042 Uiso 1 1 calc R . . H14C H 0.5144 0.0234 0.1456 0.042 Uiso 1 1 calc R . . C15 C 0.6296(4) 0.3404(4) 0.3478(3) 0.0326(6) Uani 1 1 d . . . H15A H 0.6739 0.4531 0.3787 0.049 Uiso 1 1 calc R . . H15B H 0.7205 0.3064 0.3328 0.049 Uiso 1 1 calc R . . H15C H 0.5782 0.3135 0.4204 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02236(6) 0.01758(6) 0.02133(6) 0.01029(4) 0.00958(4) 0.01058(4) Cl1 0.0403(4) 0.0335(3) 0.0253(3) 0.0188(3) 0.0167(3) 0.0218(3) S1 0.0216(3) 0.0174(3) 0.0223(3) 0.0096(2) 0.0079(2) 0.0103(2) O1 0.0340(10) 0.0308(10) 0.0415(11) 0.0256(9) 0.0253(9) 0.0227(9) O2 0.0267(10) 0.0330(10) 0.0333(11) 0.0204(9) 0.0160(8) 0.0167(8) N1 0.0196(10) 0.0173(10) 0.0212(10) 0.0077(9) 0.0055(8) 0.0082(8) C1 0.0230(12) 0.0215(12) 0.0239(13) 0.0126(11) 0.0074(10) 0.0083(10) C2 0.0190(12) 0.0191(12) 0.0258(13) 0.0094(10) 0.0060(10) 0.0089(10) C3 0.0243(13) 0.0210(13) 0.0295(14) 0.0122(11) 0.0065(11) 0.0091(11) C4 0.0232(13) 0.0199(13) 0.0373(15) 0.0115(12) 0.0057(11) 0.0104(11) C5 0.0211(13) 0.0243(13) 0.0293(14) 0.0061(11) 0.0052(11) 0.0123(11) C6 0.0218(13) 0.0287(14) 0.0299(14) 0.0138(12) 0.0105(11) 0.0129(11) C7 0.0183(12) 0.0221(12) 0.0287(13) 0.0126(11) 0.0065(10) 0.0094(10) C8 0.0218(12) 0.0233(13) 0.0194(12) 0.0086(10) 0.0040(10) 0.0119(10) C9 0.0248(13) 0.0286(14) 0.0228(13) 0.0118(11) 0.0039(10) 0.0107(11) C10 0.0299(15) 0.0520(19) 0.0196(13) 0.0156(13) 0.0064(11) 0.0200(14) C11 0.0363(16) 0.0475(19) 0.0207(14) 0.0027(13) 0.0017(12) 0.0255(15) C12 0.0304(15) 0.0291(15) 0.0308(15) 0.0030(12) -0.0016(12) 0.0163(12) C13 0.0241(13) 0.0244(13) 0.0279(14) 0.0102(11) 0.0039(11) 0.0112(11) C14 0.0352(15) 0.0224(13) 0.0344(15) 0.0143(12) 0.0126(12) 0.0168(12) C15 0.0268(14) 0.0345(16) 0.0302(15) 0.0079(13) 0.0008(12) 0.0127(13) _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 O1 2.0191(18) . ? Pt1 N1 2.029(2) . ? Pt1 S1 2.2062(6) . ? Pt1 Cl1 2.2981(6) . ? S1 O2 1.4666(19) . ? S1 C14 1.770(3) . ? S1 C15 1.777(3) . ? O1 C7 1.323(3) . ? N1 C1 1.297(3) . ? N1 C8 1.441(3) . ? C1 C2 1.433(4) . ? C1 H1 0.9500 . ? C2 C3 1.413(4) . ? C2 C7 1.416(4) . ? C3 C4 1.372(4) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.377(4) . ? C5 H5 0.9500 . ? C6 C7 1.415(4) . ? C6 H6 0.9500 . ? C8 C9 1.386(4) . ? C8 C13 1.386(4) . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 C11 1.383(5) . ? C10 H10 0.9500 . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 Pt1 N1 89.01(8) . . ? O1 Pt1 S1 172.56(6) . . ? N1 Pt1 S1 95.19(6) . . ? O1 Pt1 Cl1 86.87(6) . . ? N1 Pt1 Cl1 173.87(6) . . ? S1 Pt1 Cl1 89.39(2) . . ? O2 S1 C14 109.15(13) . . ? O2 S1 C15 106.95(13) . . ? C14 S1 C15 101.18(14) . . ? O2 S1 Pt1 118.26(8) . . ? C14 S1 Pt1 110.27(10) . . ? C15 S1 Pt1 109.64(10) . . ? C7 O1 Pt1 119.21(16) . . ? C1 N1 C8 117.9(2) . . ? C1 N1 Pt1 121.41(18) . . ? C8 N1 Pt1 120.57(16) . . ? N1 C1 C2 126.4(2) . . ? N1 C1 H1 116.8 . . ? C2 C1 H1 116.8 . . ? C3 C2 C7 119.9(2) . . ? C3 C2 C1 117.5(2) . . ? C7 C2 C1 122.2(2) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.1(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? O1 C7 C6 117.9(2) . . ? O1 C7 C2 124.2(2) . . ? C6 C7 C2 117.8(2) . . ? C9 C8 C13 120.6(2) . . ? C9 C8 N1 120.4(2) . . ? C13 C8 N1 118.9(2) . . ? C8 C9 C10 119.3(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 119.6(3) . . ? C8 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? S1 C14 H14A 109.5 . . ? S1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S1 C15 H15A 109.5 . . ? S1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 O1 Pt1 S1 O2 -112.6(4) . . . . ? N1 Pt1 S1 O2 11.67(11) . . . . ? Cl1 Pt1 S1 O2 -172.40(10) . . . . ? O1 Pt1 S1 C14 120.9(4) . . . . ? N1 Pt1 S1 C14 -114.87(12) . . . . ? Cl1 Pt1 S1 C14 61.06(11) . . . . ? O1 Pt1 S1 C15 10.3(4) . . . . ? N1 Pt1 S1 C15 134.57(13) . . . . ? Cl1 Pt1 S1 C15 -49.50(12) . . . . ? N1 Pt1 O1 C7 -43.1(2) . . . . ? S1 Pt1 O1 C7 81.5(5) . . . . ? Cl1 Pt1 O1 C7 141.5(2) . . . . ? O1 Pt1 N1 C1 30.5(2) . . . . ? S1 Pt1 N1 C1 -143.38(19) . . . . ? Cl1 Pt1 N1 C1 78.3(6) . . . . ? O1 Pt1 N1 C8 -145.76(18) . . . . ? S1 Pt1 N1 C8 40.38(18) . . . . ? Cl1 Pt1 N1 C8 -97.9(6) . . . . ? C8 N1 C1 C2 170.7(2) . . . . ? Pt1 N1 C1 C2 -5.6(4) . . . . ? N1 C1 C2 C3 166.3(3) . . . . ? N1 C1 C2 C7 -21.0(4) . . . . ? C7 C2 C3 C4 0.7(4) . . . . ? C1 C2 C3 C4 173.6(2) . . . . ? C2 C3 C4 C5 -2.2(4) . . . . ? C3 C4 C5 C6 1.8(4) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? Pt1 O1 C7 C6 -150.74(19) . . . . ? Pt1 O1 C7 C2 32.3(3) . . . . ? C5 C6 C7 O1 -178.7(2) . . . . ? C5 C6 C7 C2 -1.6(4) . . . . ? C3 C2 C7 O1 178.1(2) . . . . ? C1 C2 C7 O1 5.5(4) . . . . ? C3 C2 C7 C6 1.2(4) . . . . ? C1 C2 C7 C6 -171.4(2) . . . . ? C1 N1 C8 C9 49.0(3) . . . . ? Pt1 N1 C8 C9 -134.7(2) . . . . ? C1 N1 C8 C13 -129.4(3) . . . . ? Pt1 N1 C8 C13 46.9(3) . . . . ? C13 C8 C9 C10 -1.4(4) . . . . ? N1 C8 C9 C10 -179.8(2) . . . . ? C8 C9 C10 C11 1.7(4) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C10 C11 C12 C13 -1.2(4) . . . . ? C9 C8 C13 C12 -0.1(4) . . . . ? N1 C8 C13 C12 178.3(2) . . . . ? C11 C12 C13 C8 1.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.292 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 931187' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3a _chemical_melting_point 213 _chemical_formula_moiety 'C37 H37 Cl1 N O P Pt, 2(C H2 Cl2)' _chemical_formula_sum 'C39 H41 Cl5 N O P Pt' _chemical_formula_weight 943.04 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' 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 P21/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 10.3272(9) _cell_length_b 18.7983(17) _cell_length_c 20.8684(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.185(2) _cell_angle_gamma 90.00 _cell_volume 3987.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7573 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.68 _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 3.925 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3155 _exptl_absorpt_correction_T_max 0.5551 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker Kappa Duo Apex II Diffractometer' _diffrn_measurement_method '0.5\% \f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 63670 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_unetI/netI 0.0125 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7573 _reflns_number_gt 7001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT program (Bruker, 2006)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2001)' _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^)+(0.0307P)^2^+13.2989P] 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 7573 _refine_ls_number_parameters 431 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.047 _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 Cl1 Cl 0.07713(8) 0.64932(5) 0.33678(5) 0.0320(2) Uani 1 1 d . . . Pt2 Pt 0.252183(12) 0.722249(7) 0.324789(6) 0.02201(5) Uani 1 1 d . . . Cl3A Cl 0.14244(19) 0.62192(12) 0.13321(10) 0.1004(6) Uani 1 1 d D A . O3 O 0.1060(3) 0.77944(14) 0.26893(15) 0.0361(7) Uani 1 1 d . . . Cl1A Cl -0.1024(3) 0.7004(2) 0.10943(13) 0.0819(11) Uiso 0.722(11) 1 d PD A 1 C4 C 0.1121(4) 0.8451(2) 0.24903(19) 0.0314(8) Uani 1 1 d . . . C5 C -0.0057(4) 0.8796(3) 0.2204(2) 0.0442(11) Uani 1 1 d . . . H5 H -0.0868 0.8547 0.2156 0.053 Uiso 1 1 calc R . . C6 C -0.0042(5) 0.9493(3) 0.1993(2) 0.0495(13) Uani 1 1 d . . . H6 H -0.0846 0.9716 0.1809 0.059 Uiso 1 1 calc R . . C7 C 0.1131(5) 0.9874(2) 0.2046(2) 0.0485(12) Uani 1 1 d . . . H7 H 0.1127 1.0355 0.1904 0.058 Uiso 1 1 calc R . . C8 C 0.2282(5) 0.9547(2) 0.2304(2) 0.0415(10) Uani 1 1 d . . . H8 H 0.3086 0.9800 0.2334 0.050 Uiso 1 1 calc R . . C9 C 0.2305(4) 0.8834(2) 0.25306(19) 0.0298(8) Uani 1 1 d . . . C10 C 0.3566(4) 0.85287(19) 0.27636(19) 0.0283(8) Uani 1 1 d . . . H10 H 0.4292 0.8816 0.2703 0.034 Uiso 1 1 calc R . . N11 N 0.3882(3) 0.79209(15) 0.30460(15) 0.0238(6) Uani 1 1 d . . . C12 C 0.5308(3) 0.78126(18) 0.31715(19) 0.0257(8) Uani 1 1 d . . . C13 C 0.6065(4) 0.8203(2) 0.3678(2) 0.0315(8) Uani 1 1 d . . . C14 C 0.7433(4) 0.8157(2) 0.3732(2) 0.0425(10) Uani 1 1 d . . . H14 H 0.7979 0.8407 0.4073 0.051 Uiso 1 1 calc R . . C15 C 0.8008(4) 0.7758(2) 0.3302(3) 0.0449(11) Uani 1 1 d . . . H15 H 0.8939 0.7747 0.3342 0.054 Uiso 1 1 calc R . . C16 C 0.7231(4) 0.7375(2) 0.2813(2) 0.0379(10) Uani 1 1 d . . . H16 H 0.7639 0.7099 0.2523 0.046 Uiso 1 1 calc R . . C17 C 0.5864(4) 0.73852(19) 0.2737(2) 0.0288(8) Uani 1 1 d . . . C18 C 0.5011(4) 0.6977(2) 0.21853(19) 0.0312(8) Uani 1 1 d . . . H18 H 0.4149 0.6881 0.2323 0.037 Uiso 1 1 calc R . . C19 C 0.4729(5) 0.7421(3) 0.1564(2) 0.0473(11) Uani 1 1 d . . . H19A H 0.4177 0.7148 0.1220 0.071 Uiso 1 1 calc R . . H19B H 0.5560 0.7544 0.1426 0.071 Uiso 1 1 calc R . . H19C H 0.4269 0.7858 0.1648 0.071 Uiso 1 1 calc R . . C20 C 0.5586(5) 0.6260(2) 0.2039(2) 0.0501(12) Uani 1 1 d . . . H20A H 0.4988 0.6025 0.1685 0.075 Uiso 1 1 calc R . . H20B H 0.5697 0.5961 0.2429 0.075 Uiso 1 1 calc R . . H20C H 0.6442 0.6334 0.1908 0.075 Uiso 1 1 calc R . . C21 C 0.5458(5) 0.8677(2) 0.4135(2) 0.0398(10) Uani 1 1 d . . . H21 H 0.4499 0.8563 0.4077 0.048 Uiso 1 1 calc R . . C22 C 0.6055(7) 0.8566(3) 0.4852(3) 0.0706(17) Uani 1 1 d . . . H22A H 0.5623 0.8883 0.5122 0.106 Uiso 1 1 calc R . . H22B H 0.6998 0.8672 0.4921 0.106 Uiso 1 1 calc R . . H22C H 0.5925 0.8070 0.4973 0.106 Uiso 1 1 calc R . . C23 C 0.5593(6) 0.9468(3) 0.3975(3) 0.0595(14) Uani 1 1 d . . . H23A H 0.5188 0.9758 0.4277 0.089 Uiso 1 1 calc R . . H23B H 0.5150 0.9560 0.3528 0.089 Uiso 1 1 calc R . . H23C H 0.6527 0.9591 0.4019 0.089 Uiso 1 1 calc R . . P24 P 0.37201(9) 0.64280(5) 0.39171(4) 0.02177(18) Uani 1 1 d . . . C25 C 0.2882(3) 0.6316(2) 0.46130(17) 0.0252(7) Uani 1 1 d . . . C26 C 0.2529(4) 0.6934(2) 0.4909(2) 0.0337(9) Uani 1 1 d . . . H26 H 0.2714 0.7384 0.4739 0.040 Uiso 1 1 calc R . . C27 C 0.1916(4) 0.6900(3) 0.5444(2) 0.0398(10) Uani 1 1 d . . . H27 H 0.1684 0.7326 0.5641 0.048 Uiso 1 1 calc R . . C28 C 0.1638(4) 0.6248(3) 0.5693(2) 0.0413(10) Uani 1 1 d . . . H28 H 0.1222 0.6224 0.6064 0.050 Uiso 1 1 calc R . . C29 C 0.1969(4) 0.5632(3) 0.5400(2) 0.0439(11) Uani 1 1 d . . . H29 H 0.1767 0.5183 0.5567 0.053 Uiso 1 1 calc R . . C30 C 0.2596(4) 0.5661(2) 0.4861(2) 0.0337(9) Uani 1 1 d . . . H30 H 0.2827 0.5234 0.4665 0.040 Uiso 1 1 calc R . . C31 C 0.3763(3) 0.55635(19) 0.35237(18) 0.0251(7) Uani 1 1 d . . . C32 C 0.3082(4) 0.5457(2) 0.28956(19) 0.0301(8) Uani 1 1 d . . . H32 H 0.2619 0.5841 0.2664 0.036 Uiso 1 1 calc R . . C33 C 0.3074(4) 0.4792(2) 0.2603(2) 0.0381(10) Uani 1 1 d . . . H33 H 0.2602 0.4723 0.2174 0.046 Uiso 1 1 calc R . . C34 C 0.3751(4) 0.4231(2) 0.2935(2) 0.0407(10) Uani 1 1 d . . . H34 H 0.3721 0.3773 0.2741 0.049 Uiso 1 1 calc R . . C35 C 0.4473(5) 0.4339(2) 0.3551(2) 0.0426(10) Uani 1 1 d . . . H35 H 0.4964 0.3958 0.3773 0.051 Uiso 1 1 calc R . . C36 C 0.4486(4) 0.5001(2) 0.3848(2) 0.0344(9) Uani 1 1 d . . . H36 H 0.4986 0.5071 0.4271 0.041 Uiso 1 1 calc R . . C37 C 0.5441(4) 0.65111(19) 0.43238(19) 0.0274(8) Uani 1 1 d . . . C38 C 0.5762(4) 0.6669(2) 0.4985(2) 0.0379(9) Uani 1 1 d . . . H38 H 0.5086 0.6783 0.5222 0.046 Uiso 1 1 calc R . . C39 C 0.7072(5) 0.6659(3) 0.5299(2) 0.0507(12) Uani 1 1 d . . . H39 H 0.7282 0.6751 0.5753 0.061 Uiso 1 1 calc R . . C40 C 0.8065(4) 0.6515(3) 0.4952(3) 0.0502(12) Uani 1 1 d . . . H40 H 0.8958 0.6520 0.5165 0.060 Uiso 1 1 calc R . . Cl3B Cl 0.0077(6) 0.9545(3) 0.4126(3) 0.165(3) Uiso 0.535(5) 1 d PD B 1 C41 C 0.7758(4) 0.6363(2) 0.4297(2) 0.0425(10) Uani 1 1 d . . . H41 H 0.8441 0.6266 0.4058 0.051 Uiso 1 1 calc R . . C42 C 0.6456(4) 0.6351(2) 0.3984(2) 0.0327(8) Uani 1 1 d . . . H42 H 0.6253 0.6234 0.3535 0.039 Uiso 1 1 calc R . . Cl1B Cl 0.2533(4) 0.9048(3) 0.4800(2) 0.1172(17) Uiso 0.535(5) 1 d PD B 1 C2B C 0.1143(7) 0.8693(4) 0.4212(4) 0.0363(18) Uiso 0.535(5) 1 d PD B 1 H2B1 H 0.0706 0.8290 0.4391 0.044 Uiso 0.535(5) 1 calc PR B 1 H2B2 H 0.1406 0.8553 0.3796 0.044 Uiso 0.535(5) 1 calc PR B 1 C2A C 0.0058(6) 0.6477(4) 0.1666(3) 0.0778(19) Uani 1 1 d D . . H2A1 H 0.0352 0.6754 0.2068 0.093 Uiso 1 1 calc R A 1 H2A2 H -0.0412 0.6049 0.1780 0.093 Uiso 1 1 calc R A 1 Cl1C Cl 0.2066(7) 1.0013(3) 0.4111(3) 0.142(3) Uiso 0.465(5) 1 d PD B 2 Cl3C Cl 0.0938(10) 0.8744(5) 0.4495(5) 0.215(5) Uiso 0.465(5) 1 d PD B 2 C2C C 0.0794(13) 0.9395(7) 0.3890(6) 0.085(4) Uiso 0.465(5) 1 d PD B 2 H2C1 H -0.0070 0.9635 0.3849 0.102 Uiso 0.465(5) 1 calc PR B 2 H2C2 H 0.0862 0.9175 0.3466 0.102 Uiso 0.465(5) 1 calc PR B 2 Cl1D Cl -0.1283(6) 0.6652(6) 0.1104(3) 0.082(3) Uiso 0.278(11) 1 d PD A 2 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 Cl1 0.0204(4) 0.0318(5) 0.0439(5) 0.0082(4) 0.0056(4) -0.0035(3) Pt2 0.01780(8) 0.01994(8) 0.02875(8) 0.00404(5) 0.00537(5) 0.00137(5) Cl3A 0.0825(12) 0.1190(16) 0.0949(13) 0.0368(12) 0.0024(10) 0.0147(11) O3 0.0225(13) 0.0354(15) 0.0492(17) 0.0179(13) 0.0035(12) 0.0034(11) C4 0.0288(19) 0.034(2) 0.034(2) 0.0101(16) 0.0124(16) 0.0102(16) C5 0.029(2) 0.054(3) 0.054(3) 0.024(2) 0.0164(19) 0.0151(19) C6 0.044(3) 0.056(3) 0.055(3) 0.026(2) 0.024(2) 0.032(2) C7 0.058(3) 0.033(2) 0.059(3) 0.018(2) 0.024(2) 0.023(2) C8 0.047(3) 0.027(2) 0.052(3) 0.0088(19) 0.016(2) 0.0081(18) C9 0.032(2) 0.0243(18) 0.035(2) 0.0054(15) 0.0111(16) 0.0083(15) C10 0.0286(19) 0.0220(18) 0.036(2) 0.0025(15) 0.0105(16) -0.0002(14) N11 0.0219(15) 0.0194(14) 0.0315(16) 0.0010(12) 0.0081(12) 0.0015(11) C12 0.0208(17) 0.0196(17) 0.038(2) 0.0083(14) 0.0072(15) 0.0006(13) C13 0.0289(19) 0.0234(18) 0.041(2) 0.0050(16) 0.0025(16) -0.0033(15) C14 0.030(2) 0.035(2) 0.058(3) 0.006(2) -0.0041(19) -0.0063(18) C15 0.023(2) 0.037(2) 0.074(3) 0.017(2) 0.007(2) 0.0012(17) C16 0.030(2) 0.029(2) 0.060(3) 0.0117(19) 0.019(2) 0.0064(16) C17 0.0288(19) 0.0194(17) 0.040(2) 0.0082(15) 0.0110(16) 0.0015(14) C18 0.036(2) 0.0221(18) 0.039(2) 0.0013(16) 0.0151(17) 0.0019(16) C19 0.058(3) 0.037(2) 0.044(3) 0.005(2) 0.001(2) -0.003(2) C20 0.070(3) 0.034(2) 0.047(3) -0.005(2) 0.014(2) 0.014(2) C21 0.044(2) 0.034(2) 0.039(2) -0.0022(18) 0.0020(19) -0.0046(18) C22 0.104(5) 0.056(3) 0.044(3) -0.005(2) -0.007(3) 0.003(3) C23 0.086(4) 0.033(2) 0.062(3) -0.003(2) 0.019(3) 0.007(3) P24 0.0209(4) 0.0189(4) 0.0260(4) 0.0021(3) 0.0057(3) 0.0015(3) C25 0.0201(17) 0.0289(19) 0.0269(18) 0.0012(14) 0.0045(14) 0.0009(14) C26 0.034(2) 0.030(2) 0.040(2) -0.0027(17) 0.0125(17) -0.0016(16) C27 0.033(2) 0.051(3) 0.036(2) -0.0096(19) 0.0084(18) 0.0047(19) C28 0.030(2) 0.066(3) 0.030(2) 0.005(2) 0.0111(17) 0.005(2) C29 0.045(2) 0.046(3) 0.044(2) 0.016(2) 0.018(2) 0.002(2) C30 0.036(2) 0.031(2) 0.037(2) 0.0072(16) 0.0130(17) 0.0049(16) C31 0.0242(17) 0.0219(17) 0.0316(19) 0.0001(14) 0.0113(15) 0.0005(14) C32 0.0253(18) 0.0300(19) 0.036(2) -0.0022(16) 0.0086(16) -0.0006(15) C33 0.031(2) 0.041(2) 0.045(2) -0.0145(19) 0.0134(18) -0.0064(18) C34 0.038(2) 0.029(2) 0.061(3) -0.0139(19) 0.025(2) -0.0035(17) C35 0.050(3) 0.025(2) 0.058(3) 0.0015(19) 0.024(2) 0.0100(18) C36 0.040(2) 0.028(2) 0.036(2) 0.0017(16) 0.0112(18) 0.0065(17) C37 0.0233(17) 0.0242(18) 0.034(2) 0.0074(15) 0.0041(15) 0.0011(14) C38 0.027(2) 0.050(3) 0.036(2) -0.0006(19) 0.0033(17) -0.0032(18) C39 0.036(2) 0.069(3) 0.043(3) 0.003(2) -0.005(2) -0.007(2) C40 0.028(2) 0.057(3) 0.061(3) 0.014(2) -0.006(2) 0.000(2) C41 0.026(2) 0.040(2) 0.063(3) 0.012(2) 0.012(2) 0.0050(17) C42 0.0283(19) 0.031(2) 0.041(2) 0.0079(17) 0.0108(17) 0.0035(16) C2A 0.083(4) 0.089(5) 0.055(3) 0.008(3) -0.006(3) -0.006(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 Cl1 Pt2 2.3174(9) . ? Pt2 N11 2.021(3) . ? Pt2 O3 2.043(3) . ? Pt2 P24 2.2585(9) . ? Cl3A C2A 1.748(7) . ? O3 C4 1.307(5) . ? Cl1A C2A 1.784(5) . ? C4 C9 1.409(6) . ? C4 C5 1.414(5) . ? C5 C6 1.382(6) . ? C5 H5 0.9500 . ? C6 C7 1.395(7) . ? C6 H6 0.9500 . ? C7 C8 1.363(6) . ? C7 H7 0.9500 . ? C8 C9 1.419(5) . ? C8 H8 0.9500 . ? C9 C10 1.428(5) . ? C10 N11 1.300(5) . ? C10 H10 0.9500 . ? N11 C12 1.463(5) . ? C12 C13 1.404(5) . ? C12 C17 1.408(5) . ? C13 C14 1.400(6) . ? C13 C21 1.521(6) . ? C14 C15 1.383(7) . ? C14 H14 0.9500 . ? C15 C16 1.383(7) . ? C15 H15 0.9500 . ? C16 C17 1.392(6) . ? C16 H16 0.9500 . ? C17 C18 1.528(6) . ? C18 C20 1.524(5) . ? C18 C19 1.526(6) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.529(7) . ? C21 C23 1.535(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? P24 C31 1.825(4) . ? P24 C25 1.830(4) . ? P24 C37 1.836(4) . ? C25 C30 1.387(5) . ? C25 C26 1.394(5) . ? C26 C27 1.379(6) . ? C26 H26 0.9500 . ? C27 C28 1.381(7) . ? C27 H27 0.9500 . ? C28 C29 1.382(7) . ? C28 H28 0.9500 . ? C29 C30 1.394(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.388(5) . ? C31 C36 1.399(5) . ? C32 C33 1.391(6) . ? C32 H32 0.9500 . ? C33 C34 1.383(6) . ? C33 H33 0.9500 . ? C34 C35 1.382(7) . ? C34 H34 0.9500 . ? C35 C36 1.388(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.392(6) . ? C37 C42 1.399(5) . ? C38 C39 1.395(6) . ? C38 H38 0.9500 . ? C39 C40 1.384(7) . ? C39 H39 0.9500 . ? C40 C41 1.378(7) . ? C40 H40 0.9500 . ? Cl3B C2B 1.932(7) . ? C41 C42 1.387(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? Cl1B C2B 1.840(6) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C2A Cl1D 1.681(6) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? Cl1C C2C 1.753(8) . ? Cl3C C2C 1.745(8) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? 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 N11 Pt2 O3 90.58(11) . . ? N11 Pt2 P24 103.50(9) . . ? O3 Pt2 P24 165.89(8) . . ? N11 Pt2 Cl1 172.38(9) . . ? O3 Pt2 Cl1 82.00(8) . . ? P24 Pt2 Cl1 83.95(3) . . ? C4 O3 Pt2 127.3(3) . . ? O3 C4 C9 123.6(3) . . ? O3 C4 C5 118.8(4) . . ? C9 C4 C5 117.6(4) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 121.4(4) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C8 C7 C6 118.9(4) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 121.4(4) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C4 C9 C8 120.0(4) . . ? C4 C9 C10 123.0(3) . . ? C8 C9 C10 116.9(4) . . ? N11 C10 C9 130.4(4) . . ? N11 C10 H10 114.8 . . ? C9 C10 H10 114.8 . . ? C10 N11 C12 111.5(3) . . ? C10 N11 Pt2 122.5(3) . . ? C12 N11 Pt2 125.9(2) . . ? C13 C12 C17 123.1(3) . . ? C13 C12 N11 118.1(3) . . ? C17 C12 N11 118.5(3) . . ? C14 C13 C12 116.7(4) . . ? C14 C13 C21 120.4(4) . . ? C12 C13 C21 122.8(4) . . ? C15 C14 C13 121.6(4) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 117.1(4) . . ? C16 C17 C18 121.1(4) . . ? C12 C17 C18 121.7(3) . . ? C20 C18 C19 109.7(4) . . ? C20 C18 C17 113.7(4) . . ? C19 C18 C17 111.3(3) . . ? C20 C18 H18 107.3 . . ? C19 C18 H18 107.3 . . ? C17 C18 H18 107.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 C22 113.2(4) . . ? C13 C21 C23 111.6(4) . . ? C22 C21 C23 108.0(4) . . ? C13 C21 H21 107.9 . . ? C22 C21 H21 107.9 . . ? C23 C21 H21 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C31 P24 C25 107.87(17) . . ? C31 P24 C37 100.67(17) . . ? C25 P24 C37 101.42(17) . . ? C31 P24 Pt2 111.41(12) . . ? C25 P24 Pt2 106.43(12) . . ? C37 P24 Pt2 127.55(12) . . ? C30 C25 C26 119.0(3) . . ? C30 C25 P24 124.1(3) . . ? C26 C25 P24 116.9(3) . . ? C27 C26 C25 120.9(4) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 119.5(4) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C28 C29 C30 120.7(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 119.7(4) . . ? C25 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C36 119.1(3) . . ? C32 C31 P24 120.3(3) . . ? C36 C31 P24 120.6(3) . . ? C31 C32 C33 120.5(4) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.6(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C38 C37 C42 118.7(4) . . ? C38 C37 P24 121.2(3) . . ? C42 C37 P24 119.9(3) . . ? C37 C38 C39 120.3(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 120.2(4) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 119.9(4) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 120.6(4) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? Cl1B C2B Cl3B 97.3(4) . . ? Cl1B C2B H2B1 112.3 . . ? Cl3B C2B H2B1 112.3 . . ? Cl1B C2B H2B2 112.3 . . ? Cl3B C2B H2B2 112.3 . . ? H2B1 C2B H2B2 109.9 . . ? Cl1D C2A Cl3A 113.6(4) . . ? Cl3A C2A Cl1A 110.0(3) . . ? Cl1D C2A H2A1 125.4 . . ? Cl3A C2A H2A1 109.7 . . ? Cl1A C2A H2A1 109.7 . . ? Cl1D C2A H2A2 87.1 . . ? Cl3A C2A H2A2 109.7 . . ? Cl1A C2A H2A2 109.7 . . ? H2A1 C2A H2A2 108.2 . . ? Cl3C C2C Cl1C 108.2(6) . . ? Cl3C C2C H2C1 110.1 . . ? Cl1C C2C H2C1 110.1 . . ? Cl3C C2C H2C2 110.1 . . ? Cl1C C2C H2C2 110.1 . . ? H2C1 C2C H2C2 108.4 . . ? 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 N11 Pt2 O3 C4 -17.2(3) . . . . ? P24 Pt2 O3 C4 159.1(3) . . . . ? Cl1 Pt2 O3 C4 164.6(3) . . . . ? Pt2 O3 C4 C9 12.4(6) . . . . ? Pt2 O3 C4 C5 -169.1(3) . . . . ? O3 C4 C5 C6 179.3(4) . . . . ? C9 C4 C5 C6 -2.1(7) . . . . ? C4 C5 C6 C7 1.0(8) . . . . ? C5 C6 C7 C8 0.7(8) . . . . ? C6 C7 C8 C9 -1.2(7) . . . . ? O3 C4 C9 C8 -179.8(4) . . . . ? C5 C4 C9 C8 1.7(6) . . . . ? O3 C4 C9 C10 3.3(6) . . . . ? C5 C4 C9 C10 -175.2(4) . . . . ? C7 C8 C9 C4 0.0(7) . . . . ? C7 C8 C9 C10 177.0(4) . . . . ? C4 C9 C10 N11 -9.6(7) . . . . ? C8 C9 C10 N11 173.5(4) . . . . ? C9 C10 N11 C12 177.0(4) . . . . ? C9 C10 N11 Pt2 -1.3(6) . . . . ? O3 Pt2 N11 C10 11.2(3) . . . . ? P24 Pt2 N11 C10 -167.9(3) . . . . ? Cl1 Pt2 N11 C10 24.4(9) . . . . ? O3 Pt2 N11 C12 -166.8(3) . . . . ? P24 Pt2 N11 C12 14.1(3) . . . . ? Cl1 Pt2 N11 C12 -153.6(5) . . . . ? C10 N11 C12 C13 73.8(4) . . . . ? Pt2 N11 C12 C13 -108.0(3) . . . . ? C10 N11 C12 C17 -99.4(4) . . . . ? Pt2 N11 C12 C17 78.8(4) . . . . ? C17 C12 C13 C14 0.8(5) . . . . ? N11 C12 C13 C14 -172.0(3) . . . . ? C17 C12 C13 C21 178.5(4) . . . . ? N11 C12 C13 C21 5.7(5) . . . . ? C12 C13 C14 C15 1.1(6) . . . . ? C21 C13 C14 C15 -176.6(4) . . . . ? C13 C14 C15 C16 -1.8(7) . . . . ? C14 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C12 1.2(6) . . . . ? C15 C16 C17 C18 178.3(4) . . . . ? C13 C12 C17 C16 -1.9(5) . . . . ? N11 C12 C17 C16 170.9(3) . . . . ? C13 C12 C17 C18 -179.1(3) . . . . ? N11 C12 C17 C18 -6.3(5) . . . . ? C16 C17 C18 C20 37.7(5) . . . . ? C12 C17 C18 C20 -145.2(4) . . . . ? C16 C17 C18 C19 -86.7(5) . . . . ? C12 C17 C18 C19 90.3(4) . . . . ? C14 C13 C21 C22 -49.5(6) . . . . ? C12 C13 C21 C22 132.8(5) . . . . ? C14 C13 C21 C23 72.6(5) . . . . ? C12 C13 C21 C23 -105.0(5) . . . . ? N11 Pt2 P24 C31 -111.13(15) . . . . ? O3 Pt2 P24 C31 72.7(4) . . . . ? Cl1 Pt2 P24 C31 67.24(12) . . . . ? N11 Pt2 P24 C25 131.53(15) . . . . ? O3 Pt2 P24 C25 -44.7(4) . . . . ? Cl1 Pt2 P24 C25 -50.10(13) . . . . ? N11 Pt2 P24 C37 12.38(19) . . . . ? O3 Pt2 P24 C37 -163.8(4) . . . . ? Cl1 Pt2 P24 C37 -169.25(16) . . . . ? C31 P24 C25 C30 12.2(4) . . . . ? C37 P24 C25 C30 -93.1(3) . . . . ? Pt2 P24 C25 C30 131.8(3) . . . . ? C31 P24 C25 C26 -168.5(3) . . . . ? C37 P24 C25 C26 86.2(3) . . . . ? Pt2 P24 C25 C26 -48.8(3) . . . . ? C30 C25 C26 C27 0.6(6) . . . . ? P24 C25 C26 C27 -178.8(3) . . . . ? C25 C26 C27 C28 -0.2(6) . . . . ? C26 C27 C28 C29 -0.5(7) . . . . ? C27 C28 C29 C30 0.9(7) . . . . ? C26 C25 C30 C29 -0.2(6) . . . . ? P24 C25 C30 C29 179.1(3) . . . . ? C28 C29 C30 C25 -0.6(7) . . . . ? C25 P24 C31 C32 114.9(3) . . . . ? C37 P24 C31 C32 -139.3(3) . . . . ? Pt2 P24 C31 C32 -1.5(3) . . . . ? C25 P24 C31 C36 -65.4(3) . . . . ? C37 P24 C31 C36 40.4(3) . . . . ? Pt2 P24 C31 C36 178.1(3) . . . . ? C36 C31 C32 C33 2.6(6) . . . . ? P24 C31 C32 C33 -177.7(3) . . . . ? C31 C32 C33 C34 -0.3(6) . . . . ? C32 C33 C34 C35 -2.2(6) . . . . ? C33 C34 C35 C36 2.3(6) . . . . ? C34 C35 C36 C31 0.1(6) . . . . ? C32 C31 C36 C35 -2.5(6) . . . . ? P24 C31 C36 C35 177.8(3) . . . . ? C31 P24 C37 C38 -128.1(3) . . . . ? C25 P24 C37 C38 -17.2(4) . . . . ? Pt2 P24 C37 C38 104.1(3) . . . . ? C31 P24 C37 C42 46.0(3) . . . . ? C25 P24 C37 C42 156.9(3) . . . . ? Pt2 P24 C37 C42 -81.8(3) . . . . ? C42 C37 C38 C39 -0.7(6) . . . . ? P24 C37 C38 C39 173.5(4) . . . . ? C37 C38 C39 C40 2.1(7) . . . . ? C38 C39 C40 C41 -1.6(8) . . . . ? C39 C40 C41 C42 -0.3(7) . . . . ? C40 C41 C42 C37 1.7(6) . . . . ? C38 C37 C42 C41 -1.2(6) . . . . ? P24 C37 C42 C41 -175.4(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.604 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.091 _iucr_refine_instructions_details ; TITL 3a in P2(1)/c CELL 0.71073 10.3272 18.7983 20.8684 90.000 100.185 90.000 ZERR 4.0000 0.0009 0.0017 0.0018 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O P CL PT UNIT 156 164 4 4 4 20 4 MERG 2 FMAP 2 GRID PLAN 20 TEMP -100 SIZE 0.17 0.202 0.382 BOND $H HTAB CONF DFIX 1.73 0.008 Cl1C C2C DFIX 1.73 0.008 C2C Cl3C DFIX 1.79 0.008 C2B Cl1B DFIX 1.80 0.008 Cl3B C2B DFIX 1.73 0.008 C2A Cl1D DFIX 1.73 0.008 C2A CL1A DFIX 2.87 0.01 CL1A CL3A DFIX 2.87 0.01 CL3A CL1D DFIX 2.87 0.01 CL3B CL1B DFIX 2.87 0.01 CL1C CL3C L.S. 20 ACTA WGHT 0.030700 13.298901 FVAR 0.07159 0.53530 0.72237 CL1 6 0.077129 0.649319 0.336784 11.00000 0.02039 0.03178 = 0.04394 0.00817 0.00563 -0.00348 PT2 7 0.252183 0.722249 0.324789 11.00000 0.01780 0.01994 = 0.02875 0.00404 0.00537 0.00137 CL3A 6 0.142442 0.621915 0.133210 11.00000 0.08247 0.11902 = 0.09488 0.03679 0.00243 0.01472 O3 4 0.105966 0.779438 0.268931 11.00000 0.02252 0.03539 = 0.04924 0.01786 0.00347 0.00336 PART 1 CL1A 6 -0.102384 0.700383 0.109435 31.00000 0.08189 PART 0 C4 1 0.112053 0.845055 0.249027 11.00000 0.02884 0.03413 = 0.03367 0.01012 0.01239 0.01022 C5 1 -0.005691 0.879620 0.220400 11.00000 0.02876 0.05368 = 0.05356 0.02413 0.01636 0.01510 AFIX 43 H5 2 -0.086819 0.854657 0.215603 11.00000 -1.20000 AFIX 0 C6 1 -0.004157 0.949273 0.199320 11.00000 0.04368 0.05588 = 0.05462 0.02646 0.02401 0.03242 AFIX 43 H6 2 -0.084648 0.971619 0.180867 11.00000 -1.20000 AFIX 0 C7 1 0.113055 0.987444 0.204565 11.00000 0.05786 0.03344 = 0.05917 0.01804 0.02396 0.02307 AFIX 43 H7 2 0.112658 1.035466 0.190351 11.00000 -1.20000 AFIX 0 C8 1 0.228211 0.954654 0.230442 11.00000 0.04736 0.02746 = 0.05218 0.00880 0.01565 0.00812 AFIX 43 H8 2 0.308594 0.980037 0.233393 11.00000 -1.20000 AFIX 0 C9 1 0.230493 0.883389 0.253062 11.00000 0.03223 0.02426 = 0.03464 0.00536 0.01105 0.00830 C10 1 0.356644 0.852866 0.276364 11.00000 0.02857 0.02196 = 0.03608 0.00254 0.01048 -0.00018 AFIX 43 H10 2 0.429178 0.881582 0.270259 11.00000 -1.20000 AFIX 0 N11 3 0.388212 0.792090 0.304597 11.00000 0.02188 0.01941 = 0.03148 0.00102 0.00806 0.00147 C12 1 0.530766 0.781259 0.317145 11.00000 0.02081 0.01959 = 0.03755 0.00831 0.00719 0.00057 C13 1 0.606489 0.820253 0.367763 11.00000 0.02891 0.02337 = 0.04076 0.00499 0.00253 -0.00332 C14 1 0.743278 0.815732 0.373227 11.00000 0.03034 0.03459 = 0.05807 0.00604 -0.00415 -0.00627 AFIX 43 H14 2 0.797899 0.840673 0.407329 11.00000 -1.20000 AFIX 0 C15 1 0.800802 0.775828 0.330173 11.00000 0.02271 0.03717 = 0.07419 0.01692 0.00719 0.00120 AFIX 43 H15 2 0.893852 0.774722 0.334159 11.00000 -1.20000 AFIX 0 C16 1 0.723098 0.737519 0.281312 11.00000 0.02964 0.02871 = 0.05955 0.01166 0.01912 0.00636 AFIX 43 H16 2 0.763851 0.709932 0.252308 11.00000 -1.20000 AFIX 0 C17 1 0.586414 0.738520 0.273721 11.00000 0.02881 0.01944 = 0.04008 0.00817 0.01101 0.00148 C18 1 0.501134 0.697668 0.218525 11.00000 0.03584 0.02215 = 0.03858 0.00130 0.01507 0.00189 AFIX 13 H18 2 0.414867 0.688102 0.232342 11.00000 -1.20000 AFIX 0 C19 1 0.472930 0.742133 0.156446 11.00000 0.05848 0.03672 = 0.04389 0.00527 0.00117 -0.00252 AFIX 33 H19A 2 0.417749 0.714757 0.122040 11.00000 -1.50000 H19B 2 0.556017 0.754377 0.142600 11.00000 -1.50000 H19C 2 0.426909 0.785823 0.164828 11.00000 -1.50000 AFIX 0 C20 1 0.558608 0.626020 0.203876 11.00000 0.07040 0.03390 = 0.04745 -0.00521 0.01423 0.01418 AFIX 33 H20A 2 0.498825 0.602542 0.168476 11.00000 -1.50000 H20B 2 0.569711 0.596073 0.242905 11.00000 -1.50000 H20C 2 0.644234 0.633385 0.190829 11.00000 -1.50000 AFIX 0 C21 1 0.545800 0.867737 0.413499 11.00000 0.04375 0.03440 = 0.03922 -0.00224 0.00202 -0.00460 AFIX 13 H21 2 0.449863 0.856313 0.407716 11.00000 -1.20000 AFIX 0 C22 1 0.605453 0.856571 0.485233 11.00000 0.10439 0.05627 = 0.04401 -0.00539 -0.00655 0.00259 AFIX 33 H22A 2 0.562251 0.888292 0.512211 11.00000 -1.50000 H22B 2 0.699792 0.867222 0.492112 11.00000 -1.50000 H22C 2 0.592547 0.807045 0.497348 11.00000 -1.50000 AFIX 0 C23 1 0.559278 0.946788 0.397509 11.00000 0.08573 0.03325 = 0.06167 -0.00345 0.01858 0.00682 AFIX 33 H23A 2 0.518823 0.975772 0.427665 11.00000 -1.50000 H23B 2 0.514961 0.956005 0.352760 11.00000 -1.50000 H23C 2 0.652657 0.959067 0.401892 11.00000 -1.50000 AFIX 0 P24 5 0.372015 0.642803 0.391711 11.00000 0.02095 0.01893 = 0.02599 0.00210 0.00569 0.00155 C25 1 0.288203 0.631565 0.461300 11.00000 0.02006 0.02890 = 0.02690 0.00118 0.00450 0.00094 C26 1 0.252920 0.693375 0.490869 11.00000 0.03373 0.02995 = 0.03975 -0.00269 0.01252 -0.00162 AFIX 43 H26 2 0.271377 0.738436 0.473938 11.00000 -1.20000 AFIX 0 C27 1 0.191597 0.689998 0.544355 11.00000 0.03310 0.05086 = 0.03635 -0.00959 0.00836 0.00469 AFIX 43 H27 2 0.168420 0.732584 0.564082 11.00000 -1.20000 AFIX 0 C28 1 0.163805 0.624842 0.569304 11.00000 0.02982 0.06568 = 0.03045 0.00494 0.01109 0.00523 AFIX 43 H28 2 0.122217 0.622433 0.606375 11.00000 -1.20000 AFIX 0 C29 1 0.196893 0.563168 0.539983 11.00000 0.04453 0.04643 = 0.04432 0.01551 0.01781 0.00231 AFIX 43 H29 2 0.176672 0.518303 0.556709 11.00000 -1.20000 AFIX 0 C30 1 0.259645 0.566066 0.486108 11.00000 0.03609 0.03057 = 0.03677 0.00724 0.01305 0.00485 AFIX 43 H30 2 0.282731 0.523394 0.466485 11.00000 -1.20000 AFIX 0 C31 1 0.376331 0.556354 0.352366 11.00000 0.02422 0.02194 = 0.03157 0.00008 0.01135 0.00045 C32 1 0.308229 0.545727 0.289557 11.00000 0.02531 0.02996 = 0.03609 -0.00216 0.00864 -0.00062 AFIX 43 H32 2 0.261868 0.584146 0.266402 11.00000 -1.20000 AFIX 0 C33 1 0.307394 0.479209 0.260281 11.00000 0.03129 0.04057 = 0.04493 -0.01446 0.01343 -0.00643 AFIX 43 H33 2 0.260183 0.472326 0.217353 11.00000 -1.20000 AFIX 0 C34 1 0.375139 0.423073 0.293526 11.00000 0.03845 0.02865 = 0.06094 -0.01391 0.02496 -0.00355 AFIX 43 H34 2 0.372097 0.377255 0.274111 11.00000 -1.20000 AFIX 0 C35 1 0.447258 0.433921 0.355098 11.00000 0.05002 0.02481 = 0.05819 0.00146 0.02391 0.01004 AFIX 43 H35 2 0.496355 0.395788 0.377299 11.00000 -1.20000 AFIX 0 C36 1 0.448606 0.500057 0.384806 11.00000 0.04016 0.02822 = 0.03639 0.00168 0.01123 0.00653 AFIX 43 H36 2 0.498568 0.507076 0.427128 11.00000 -1.20000 AFIX 0 C37 1 0.544102 0.651114 0.432381 11.00000 0.02330 0.02417 = 0.03431 0.00736 0.00406 0.00109 C38 1 0.576188 0.666861 0.498457 11.00000 0.02742 0.04973 = 0.03579 -0.00058 0.00327 -0.00319 AFIX 43 H38 2 0.508602 0.678327 0.522242 11.00000 -1.20000 AFIX 0 C39 1 0.707152 0.665885 0.529927 11.00000 0.03597 0.06914 = 0.04260 0.00273 -0.00536 -0.00675 AFIX 43 H39 2 0.728157 0.675145 0.575333 11.00000 -1.20000 AFIX 0 C40 1 0.806531 0.651473 0.495211 11.00000 0.02763 0.05651 = 0.06124 0.01358 -0.00611 -0.00001 AFIX 43 H40 2 0.895782 0.652029 0.516524 11.00000 -1.20000 PART 1 AFIX 0 CL3B 6 0.007720 0.954451 0.412613 21.00000 0.16493 PART 0 C41 1 0.775846 0.636316 0.429686 11.00000 0.02641 0.03983 = 0.06265 0.01169 0.01182 0.00502 AFIX 43 H41 2 0.844143 0.626628 0.405836 11.00000 -1.20000 AFIX 0 C42 1 0.645650 0.635140 0.398386 11.00000 0.02829 0.03089 = 0.04062 0.00793 0.01075 0.00351 AFIX 43 H42 2 0.625276 0.623380 0.353456 11.00000 -1.20000 PART 1 AFIX 0 CL1B 6 0.253269 0.904809 0.480023 21.00000 0.11716 C2B 1 0.114333 0.869350 0.421196 21.00000 0.03631 AFIX 23 H2B1 2 0.070617 0.828953 0.439119 21.00000 -1.20000 H2B2 2 0.140572 0.855286 0.379597 21.00000 -1.20000 PART 0 AFIX 0 C2A 1 0.005845 0.647655 0.166563 11.00000 0.08288 0.08867 = 0.05506 0.00790 -0.00646 -0.00609 AFIX 23 H2A1 2 0.035187 0.675385 0.206844 11.00000 -1.20000 H2A2 2 -0.041181 0.604903 0.178030 11.00000 -1.20000 PART 2 AFIX 0 CL1C 6 0.206572 1.001314 0.411071 -21.00000 0.14153 CL3C 6 0.093763 0.874372 0.449496 -21.00000 0.21533 C2C 1 0.079423 0.939500 0.389039 -21.00000 0.08538 AFIX 23 H2C1 2 -0.007010 0.963485 0.384854 -21.00000 -1.20000 H2C2 2 0.086158 0.917537 0.346636 -21.00000 -1.20000 AFIX 0 CL1D 6 -0.128339 0.665237 0.110450 -31.00000 0.08183 HKLF 4 ; _database_code_depnum_ccdc_archive 'CCDC 931188' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3b _chemical_melting_point 237 _chemical_formula_moiety 'C37 H37 Cl N O P Pt' _chemical_formula_sum 'C37 H37 Cl N O P Pt' _chemical_formula_weight 773.19 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.498(4) _cell_length_b 10.2831(11) _cell_length_c 23.873(3) _cell_angle_alpha 90.00 _cell_angle_beta 130.634(2) _cell_angle_gamma 90.00 _cell_volume 6613.3(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9659 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.06 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 4.402 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4443 _exptl_absorpt_correction_T_max 0.7781 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker Kappa Duo Apex II Diffractometer' _diffrn_measurement_method '0.5\% \f scans and \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 61047 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.06 _reflns_number_total 9659 _reflns_number_gt 8221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SAINT program (Bruker, 2006)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2001)' _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^)+(0.0182P)^2^+8.2178P] 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 9659 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0444 _refine_ls_wR_factor_gt 0.0406 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.004 _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 0.892491(3) 0.767955(7) 0.470384(4) 0.02003(2) Uani 1 1 d . . . Cl2 Cl 0.813858(18) 0.83897(5) 0.41586(3) 0.02916(11) Uani 1 1 d . . . P24 P 0.883342(18) 0.84840(5) 0.37419(3) 0.02113(10) Uani 1 1 d . . . O3 O 0.96104(6) 0.71337(16) 0.51469(9) 0.0360(4) Uani 1 1 d . . . N11 N 0.90108(6) 0.69062(17) 0.55820(9) 0.0222(3) Uani 1 1 d . . . C4 C 0.99483(8) 0.6603(2) 0.57954(13) 0.0300(5) Uani 1 1 d . . . C5 C 1.04262(9) 0.6413(2) 0.60240(16) 0.0442(6) Uani 1 1 d . . . H5 H 1.0486 0.6662 0.5705 0.053 Uiso 1 1 calc R . . C6 C 1.08055(9) 0.5873(2) 0.66996(17) 0.0482(7) Uani 1 1 d . . . H6 H 1.1123 0.5766 0.6840 0.058 Uiso 1 1 calc R . . C7 C 1.07335(9) 0.5483(3) 0.71782(15) 0.0471(7) Uani 1 1 d . . . H7 H 1.0998 0.5113 0.7644 0.057 Uiso 1 1 calc R . . C8 C 1.02770(9) 0.5639(3) 0.69701(13) 0.0431(6) Uani 1 1 d . . . H8 H 1.0225 0.5355 0.7294 0.052 Uiso 1 1 calc R . . C9 C 0.98749(8) 0.6214(2) 0.62829(11) 0.0292(4) Uani 1 1 d . . . C10 C 0.94208(8) 0.6365(2) 0.61431(11) 0.0293(4) Uani 1 1 d . . . H10 H 0.9418 0.6024 0.6510 0.035 Uiso 1 1 calc R . . C12 C 0.86214(7) 0.6896(2) 0.56267(10) 0.0230(4) Uani 1 1 d . . . C13 C 0.86048(8) 0.7905(2) 0.60058(12) 0.0281(4) Uani 1 1 d . . . C14 C 0.82533(9) 0.7806(2) 0.60940(14) 0.0353(5) Uani 1 1 d . . . H14 H 0.8237 0.8467 0.6355 0.042 Uiso 1 1 calc R . . C15 C 0.79306(9) 0.6771(2) 0.58105(14) 0.0372(5) Uani 1 1 d . . . H15 H 0.7697 0.6720 0.5881 0.045 Uiso 1 1 calc R . . C16 C 0.79462(9) 0.5806(2) 0.54222(13) 0.0331(5) Uani 1 1 d . . . H16 H 0.7718 0.5102 0.5222 0.040 Uiso 1 1 calc R . . C17 C 0.82906(8) 0.5846(2) 0.53198(11) 0.0257(4) Uani 1 1 d . . . C18 C 0.83004(9) 0.4771(2) 0.48921(12) 0.0305(5) Uani 1 1 d . . . H18 H 0.8549 0.5023 0.4840 0.037 Uiso 1 1 calc R . . C19 C 0.77973(11) 0.4639(3) 0.41161(16) 0.0585(8) Uani 1 1 d . . . H19A H 0.7548 0.4354 0.4148 0.088 Uiso 1 1 calc R . . H19B H 0.7821 0.3997 0.3837 0.088 Uiso 1 1 calc R . . H19C H 0.7699 0.5482 0.3865 0.088 Uiso 1 1 calc R . . C20 C 0.84684(16) 0.3487(3) 0.5306(2) 0.0756(12) Uani 1 1 d . . . H20A H 0.8798 0.3595 0.5793 0.113 Uiso 1 1 calc R . . H20B H 0.8484 0.2825 0.5027 0.113 Uiso 1 1 calc R . . H20C H 0.8232 0.3214 0.5366 0.113 Uiso 1 1 calc R . . C21 C 0.89456(9) 0.9071(2) 0.63103(14) 0.0364(5) Uani 1 1 d . . . H21 H 0.9141 0.9012 0.6145 0.044 Uiso 1 1 calc R . . C22 C 0.86522(12) 1.0335(3) 0.60113(19) 0.0574(8) Uani 1 1 d . . . H22A H 0.8436 1.0342 0.5472 0.086 Uiso 1 1 calc R . . H22B H 0.8882 1.1072 0.6215 0.086 Uiso 1 1 calc R . . H22C H 0.8449 1.0405 0.6154 0.086 Uiso 1 1 calc R . . C23 C 0.93105(14) 0.9085(3) 0.71489(17) 0.0770(11) Uani 1 1 d . . . H23A H 0.9127 0.9104 0.7326 0.115 Uiso 1 1 calc R . . H23B H 0.9522 0.9859 0.7327 0.115 Uiso 1 1 calc R . . H23C H 0.9518 0.8303 0.7335 0.115 Uiso 1 1 calc R . . C25 C 0.85789(7) 1.0120(2) 0.34754(11) 0.0236(4) Uani 1 1 d . . . C26 C 0.82671(8) 1.0547(2) 0.27450(12) 0.0316(5) Uani 1 1 d . . . H26 H 0.8171 0.9964 0.2363 0.038 Uiso 1 1 calc R . . C27 C 0.80961(9) 1.1827(3) 0.25737(14) 0.0386(5) Uani 1 1 d . . . H27 H 0.7884 1.2115 0.2075 0.046 Uiso 1 1 calc R . . C28 C 0.82351(10) 1.2673(2) 0.31254(16) 0.0394(6) Uani 1 1 d . . . H28 H 0.8114 1.3541 0.3006 0.047 Uiso 1 1 calc R . . C29 C 0.85494(10) 1.2268(2) 0.38525(15) 0.0375(5) Uani 1 1 d . . . H29 H 0.8651 1.2863 0.4233 0.045 Uiso 1 1 calc R . . C30 C 0.87157(8) 1.0994(2) 0.40258(13) 0.0314(5) Uani 1 1 d . . . H30 H 0.8925 1.0713 0.4525 0.038 Uiso 1 1 calc R . . C31 C 0.94060(7) 0.8600(2) 0.38903(11) 0.0235(4) Uani 1 1 d . . . C32 C 0.96111(8) 0.9780(2) 0.39313(12) 0.0296(4) Uani 1 1 d . . . H32 H 0.9462 1.0571 0.3906 0.036 Uiso 1 1 calc R . . C33 C 1.00353(8) 0.9808(2) 0.40100(14) 0.0371(5) Uani 1 1 d . . . H33 H 1.0174 1.0620 0.4038 0.045 Uiso 1 1 calc R . . C34 C 1.02549(8) 0.8671(3) 0.40483(13) 0.0373(5) Uani 1 1 d . . . H34 H 1.0540 0.8699 0.4090 0.045 Uiso 1 1 calc R . . C35 C 1.00618(9) 0.7493(2) 0.40267(15) 0.0400(6) Uani 1 1 d . . . H35 H 1.0217 0.6707 0.4062 0.048 Uiso 1 1 calc R . . C36 C 0.96397(9) 0.7450(2) 0.39532(14) 0.0349(5) Uani 1 1 d . . . H36 H 0.9510 0.6636 0.3946 0.042 Uiso 1 1 calc R . . C37 C 0.84324(8) 0.75070(19) 0.29053(11) 0.0245(4) Uani 1 1 d . . . C38 C 0.84791(9) 0.7555(2) 0.23674(13) 0.0322(5) Uani 1 1 d . . . H38 H 0.8731 0.8074 0.2446 0.039 Uiso 1 1 calc R . . C39 C 0.81571(9) 0.6842(3) 0.17167(13) 0.0376(5) Uani 1 1 d . . . H39 H 0.8191 0.6877 0.1354 0.045 Uiso 1 1 calc R . . C40 C 0.77883(8) 0.6085(2) 0.15980(13) 0.0356(5) Uani 1 1 d . . . H40 H 0.7568 0.5606 0.1152 0.043 Uiso 1 1 calc R . . C41 C 0.77416(8) 0.6028(2) 0.21303(13) 0.0333(5) Uani 1 1 d . . . H41 H 0.7489 0.5506 0.2050 0.040 Uiso 1 1 calc R . . C42 C 0.80624(8) 0.6731(2) 0.27814(12) 0.0292(4) Uani 1 1 d . . . H42 H 0.8029 0.6683 0.3145 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01882(4) 0.02230(4) 0.02151(4) 0.00234(3) 0.01426(3) 0.00179(3) Cl2 0.0223(2) 0.0419(3) 0.0265(2) 0.0102(2) 0.0174(2) 0.0085(2) P24 0.0211(2) 0.0231(2) 0.0223(2) 0.00004(18) 0.0155(2) -0.00046(18) O3 0.0272(8) 0.0446(10) 0.0444(9) 0.0191(8) 0.0269(8) 0.0131(7) N11 0.0214(8) 0.0251(8) 0.0221(8) 0.0016(6) 0.0149(7) 0.0021(6) C4 0.0243(10) 0.0213(10) 0.0404(12) 0.0036(9) 0.0193(10) 0.0033(8) C5 0.0293(12) 0.0402(14) 0.0656(17) 0.0192(12) 0.0321(13) 0.0097(10) C6 0.0211(11) 0.0347(13) 0.0697(19) 0.0060(12) 0.0210(12) 0.0058(9) C7 0.0273(12) 0.0468(15) 0.0387(14) -0.0003(11) 0.0089(11) 0.0127(10) C8 0.0328(13) 0.0548(16) 0.0281(12) 0.0030(11) 0.0138(11) 0.0159(11) C9 0.0230(10) 0.0305(11) 0.0249(10) -0.0009(8) 0.0115(9) 0.0065(8) C10 0.0296(11) 0.0352(12) 0.0235(10) 0.0043(8) 0.0175(9) 0.0081(9) C12 0.0260(10) 0.0259(9) 0.0213(9) 0.0071(7) 0.0173(8) 0.0058(8) C13 0.0344(11) 0.0282(11) 0.0294(10) 0.0048(8) 0.0242(10) 0.0045(8) C14 0.0491(14) 0.0341(12) 0.0422(13) 0.0026(10) 0.0384(12) 0.0054(10) C15 0.0432(13) 0.0412(13) 0.0488(14) 0.0072(11) 0.0395(12) 0.0042(10) C16 0.0377(12) 0.0330(12) 0.0388(12) 0.0053(9) 0.0294(11) -0.0003(9) C17 0.0284(10) 0.0268(10) 0.0252(10) 0.0054(8) 0.0189(9) 0.0041(8) C18 0.0366(12) 0.0296(11) 0.0315(11) 0.0012(9) 0.0249(10) 0.0005(9) C19 0.0459(16) 0.065(2) 0.0513(17) -0.0256(15) 0.0259(15) -0.0075(14) C20 0.145(4) 0.0419(17) 0.082(2) 0.0222(16) 0.092(3) 0.038(2) C21 0.0472(14) 0.0291(12) 0.0445(14) -0.0045(10) 0.0350(12) -0.0023(10) C22 0.067(2) 0.0317(14) 0.083(2) 0.0046(14) 0.0528(19) 0.0032(13) C23 0.080(2) 0.055(2) 0.0499(19) -0.0083(15) 0.0217(18) -0.0235(18) C25 0.0226(9) 0.0272(10) 0.0256(10) 0.0038(8) 0.0177(9) 0.0025(7) C26 0.0326(12) 0.0363(12) 0.0281(11) 0.0053(9) 0.0207(10) 0.0046(9) C27 0.0369(13) 0.0433(14) 0.0388(13) 0.0168(11) 0.0261(11) 0.0118(10) C28 0.0423(13) 0.0284(11) 0.0600(16) 0.0117(11) 0.0389(13) 0.0085(10) C29 0.0443(14) 0.0293(11) 0.0481(14) -0.0033(10) 0.0342(12) 0.0015(10) C30 0.0338(12) 0.0316(12) 0.0311(11) 0.0002(9) 0.0221(10) 0.0021(9) C31 0.0222(9) 0.0292(10) 0.0216(9) -0.0012(8) 0.0154(8) -0.0019(8) C32 0.0260(10) 0.0316(11) 0.0312(11) -0.0012(9) 0.0185(9) -0.0025(8) C33 0.0288(11) 0.0411(13) 0.0422(13) -0.0038(10) 0.0235(11) -0.0107(10) C34 0.0250(11) 0.0567(16) 0.0346(12) -0.0072(11) 0.0213(10) -0.0059(10) C35 0.0340(12) 0.0428(14) 0.0494(15) -0.0092(11) 0.0298(12) 0.0018(10) C36 0.0339(12) 0.0306(12) 0.0475(14) -0.0044(10) 0.0297(11) -0.0030(9) C37 0.0236(9) 0.0276(11) 0.0242(9) -0.0019(7) 0.0164(8) -0.0008(7) C38 0.0336(11) 0.0381(13) 0.0321(11) -0.0060(9) 0.0245(10) -0.0063(9) C39 0.0414(13) 0.0489(14) 0.0312(12) -0.0095(10) 0.0274(11) -0.0053(11) C40 0.0311(12) 0.0385(13) 0.0313(12) -0.0115(10) 0.0178(10) -0.0027(9) C41 0.0285(11) 0.0327(12) 0.0381(12) -0.0082(9) 0.0214(10) -0.0065(9) C42 0.0289(11) 0.0333(12) 0.0312(11) -0.0044(9) 0.0220(9) -0.0047(9) _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 O3 2.0008(15) . ? Pt1 N11 2.0707(16) . ? Pt1 P24 2.2567(6) . ? Pt1 Cl2 2.2993(5) . ? P24 C25 1.818(2) . ? P24 C37 1.823(2) . ? P24 C31 1.826(2) . ? O3 C4 1.309(3) . ? N11 C10 1.297(3) . ? N11 C12 1.454(2) . ? C4 C9 1.406(3) . ? C4 C5 1.417(3) . ? C5 C6 1.376(4) . ? C5 H5 0.9500 . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.360(4) . ? C7 H7 0.9500 . ? C8 C9 1.424(3) . ? C8 H8 0.9500 . ? C9 C10 1.426(3) . ? C10 H10 0.9500 . ? C12 C17 1.400(3) . ? C12 C13 1.403(3) . ? C13 C14 1.398(3) . ? C13 C21 1.512(3) . ? C14 C15 1.375(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.395(3) . ? C16 H16 0.9500 . ? C17 C18 1.521(3) . ? C18 C20 1.519(3) . ? C18 C19 1.527(3) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.519(4) . ? C21 C22 1.522(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 C30 1.392(3) . ? C25 C26 1.395(3) . ? C26 C27 1.395(3) . ? C26 H26 0.9500 . ? C27 C28 1.374(4) . ? C27 H27 0.9500 . ? C28 C29 1.382(4) . ? C28 H28 0.9500 . ? C29 C30 1.385(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.386(3) . ? C31 C36 1.395(3) . ? C32 C33 1.391(3) . ? C32 H32 0.9500 . ? C33 C34 1.375(4) . ? C33 H33 0.9500 . ? C34 C35 1.377(4) . ? C34 H34 0.9500 . ? C35 C36 1.391(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.394(3) . ? C37 C38 1.398(3) . ? C38 C39 1.394(3) . ? C38 H38 0.9500 . ? C39 C40 1.385(3) . ? C39 H39 0.9500 . ? C40 C41 1.386(3) . ? C40 H40 0.9500 . ? C41 C42 1.389(3) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? 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 O3 Pt1 N11 91.75(6) . . ? O3 Pt1 P24 87.72(5) . . ? N11 Pt1 P24 178.90(5) . . ? O3 Pt1 Cl2 176.92(5) . . ? N11 Pt1 Cl2 91.10(5) . . ? P24 Pt1 Cl2 89.446(18) . . ? C25 P24 C37 105.75(9) . . ? C25 P24 C31 104.14(9) . . ? C37 P24 C31 103.00(9) . . ? C25 P24 Pt1 113.88(7) . . ? C37 P24 Pt1 113.91(7) . . ? C31 P24 Pt1 114.97(7) . . ? C4 O3 Pt1 127.17(14) . . ? C10 N11 C12 113.70(17) . . ? C10 N11 Pt1 122.46(14) . . ? C12 N11 Pt1 123.83(12) . . ? O3 C4 C9 125.20(19) . . ? O3 C4 C5 117.3(2) . . ? C9 C4 C5 117.5(2) . . ? C6 C5 C4 121.3(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 121.3(2) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 118.8(2) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 122.1(3) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C4 C9 C8 119.0(2) . . ? C4 C9 C10 124.44(19) . . ? C8 C9 C10 116.6(2) . . ? N11 C10 C9 128.7(2) . . ? N11 C10 H10 115.6 . . ? C9 C10 H10 115.6 . . ? C17 C12 C13 122.30(19) . . ? C17 C12 N11 118.73(18) . . ? C13 C12 N11 118.89(18) . . ? C14 C13 C12 117.4(2) . . ? C14 C13 C21 119.9(2) . . ? C12 C13 C21 122.72(19) . . ? C15 C14 C13 121.4(2) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 120.0(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.2(2) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 117.6(2) . . ? C16 C17 C18 120.1(2) . . ? C12 C17 C18 122.27(19) . . ? C20 C18 C17 111.44(19) . . ? C20 C18 C19 111.5(3) . . ? C17 C18 C19 111.1(2) . . ? C20 C18 H18 107.6 . . ? C17 C18 H18 107.6 . . ? C19 C18 H18 107.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 C23 111.7(2) . . ? C13 C21 C22 111.3(2) . . ? C23 C21 C22 110.2(2) . . ? C13 C21 H21 107.8 . . ? C23 C21 H21 107.8 . . ? C22 C21 H21 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C30 C25 C26 118.8(2) . . ? C30 C25 P24 118.60(16) . . ? C26 C25 P24 122.53(16) . . ? C25 C26 C27 120.2(2) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.0(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.4(2) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C30 119.9(2) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.6(2) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C32 C31 C36 119.10(19) . . ? C32 C31 P24 122.56(16) . . ? C36 C31 P24 118.33(16) . . ? C31 C32 C33 120.0(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.6(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.9(2) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.1(2) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.2(2) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C42 C37 C38 118.94(19) . . ? C42 C37 P24 120.23(16) . . ? C38 C37 P24 120.79(16) . . ? C39 C38 C37 120.2(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C38 120.2(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 119.9(2) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C42 120.2(2) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 120.5(2) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? 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 O3 Pt1 P24 C25 -132.48(9) . . . . ? N11 Pt1 P24 C25 166(4) . . . . ? Cl2 Pt1 P24 C25 46.30(7) . . . . ? O3 Pt1 P24 C37 106.13(9) . . . . ? N11 Pt1 P24 C37 45(3) . . . . ? Cl2 Pt1 P24 C37 -75.09(8) . . . . ? O3 Pt1 P24 C31 -12.42(9) . . . . ? N11 Pt1 P24 C31 -74(3) . . . . ? Cl2 Pt1 P24 C31 166.36(8) . . . . ? N11 Pt1 O3 C4 -5.31(19) . . . . ? P24 Pt1 O3 C4 175.65(18) . . . . ? Cl2 Pt1 O3 C4 152.3(9) . . . . ? O3 Pt1 N11 C10 1.84(18) . . . . ? P24 Pt1 N11 C10 63(3) . . . . ? Cl2 Pt1 N11 C10 -176.99(17) . . . . ? O3 Pt1 N11 C12 -177.16(16) . . . . ? P24 Pt1 N11 C12 -116(3) . . . . ? Cl2 Pt1 N11 C12 4.02(15) . . . . ? Pt1 O3 C4 C9 5.7(3) . . . . ? Pt1 O3 C4 C5 -173.99(17) . . . . ? O3 C4 C5 C6 179.4(2) . . . . ? C9 C4 C5 C6 -0.3(4) . . . . ? C4 C5 C6 C7 0.7(4) . . . . ? C5 C6 C7 C8 0.1(4) . . . . ? C6 C7 C8 C9 -1.3(4) . . . . ? O3 C4 C9 C8 179.5(2) . . . . ? C5 C4 C9 C8 -0.8(3) . . . . ? O3 C4 C9 C10 -1.2(4) . . . . ? C5 C4 C9 C10 178.5(2) . . . . ? C7 C8 C9 C4 1.6(4) . . . . ? C7 C8 C9 C10 -177.7(2) . . . . ? C12 N11 C10 C9 -179.5(2) . . . . ? Pt1 N11 C10 C9 1.4(3) . . . . ? C4 C9 C10 N11 -2.7(4) . . . . ? C8 C9 C10 N11 176.6(2) . . . . ? C10 N11 C12 C17 -90.8(2) . . . . ? Pt1 N11 C12 C17 88.3(2) . . . . ? C10 N11 C12 C13 86.2(2) . . . . ? Pt1 N11 C12 C13 -94.7(2) . . . . ? C17 C12 C13 C14 2.4(3) . . . . ? N11 C12 C13 C14 -174.52(18) . . . . ? C17 C12 C13 C21 -177.3(2) . . . . ? N11 C12 C13 C21 5.9(3) . . . . ? C12 C13 C14 C15 -1.0(3) . . . . ? C21 C13 C14 C15 178.6(2) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? C15 C16 C17 C12 0.3(3) . . . . ? C15 C16 C17 C18 179.9(2) . . . . ? C13 C12 C17 C16 -2.0(3) . . . . ? N11 C12 C17 C16 174.89(18) . . . . ? C13 C12 C17 C18 178.41(19) . . . . ? N11 C12 C17 C18 -4.7(3) . . . . ? C16 C17 C18 C20 -67.7(3) . . . . ? C12 C17 C18 C20 111.9(3) . . . . ? C16 C17 C18 C19 57.3(3) . . . . ? C12 C17 C18 C19 -123.1(2) . . . . ? C14 C13 C21 C23 67.9(3) . . . . ? C12 C13 C21 C23 -112.5(3) . . . . ? C14 C13 C21 C22 -55.8(3) . . . . ? C12 C13 C21 C22 123.8(2) . . . . ? C37 P24 C25 C30 161.96(17) . . . . ? C31 P24 C25 C30 -89.85(18) . . . . ? Pt1 P24 C25 C30 36.14(19) . . . . ? C37 P24 C25 C26 -20.5(2) . . . . ? C31 P24 C25 C26 87.73(19) . . . . ? Pt1 P24 C25 C26 -146.28(16) . . . . ? C30 C25 C26 C27 -0.1(3) . . . . ? P24 C25 C26 C27 -177.72(18) . . . . ? C25 C26 C27 C28 0.1(4) . . . . ? C26 C27 C28 C29 0.9(4) . . . . ? C27 C28 C29 C30 -1.7(4) . . . . ? C28 C29 C30 C25 1.6(4) . . . . ? C26 C25 C30 C29 -0.7(3) . . . . ? P24 C25 C30 C29 177.00(18) . . . . ? C25 P24 C31 C32 12.1(2) . . . . ? C37 P24 C31 C32 122.28(18) . . . . ? Pt1 P24 C31 C32 -113.22(17) . . . . ? C25 P24 C31 C36 -166.92(18) . . . . ? C37 P24 C31 C36 -56.71(19) . . . . ? Pt1 P24 C31 C36 67.78(19) . . . . ? C36 C31 C32 C33 2.1(3) . . . . ? P24 C31 C32 C33 -176.93(17) . . . . ? C31 C32 C33 C34 0.0(4) . . . . ? C32 C33 C34 C35 -1.6(4) . . . . ? C33 C34 C35 C36 1.1(4) . . . . ? C34 C35 C36 C31 0.9(4) . . . . ? C32 C31 C36 C35 -2.5(3) . . . . ? P24 C31 C36 C35 176.5(2) . . . . ? C25 P24 C37 C42 -99.27(18) . . . . ? C31 P24 C37 C42 151.73(17) . . . . ? Pt1 P24 C37 C42 26.54(19) . . . . ? C25 P24 C37 C38 78.58(19) . . . . ? C31 P24 C37 C38 -30.4(2) . . . . ? Pt1 P24 C37 C38 -155.61(16) . . . . ? C42 C37 C38 C39 0.4(3) . . . . ? P24 C37 C38 C39 -177.44(18) . . . . ? C37 C38 C39 C40 0.1(4) . . . . ? C38 C39 C40 C41 -0.5(4) . . . . ? C39 C40 C41 C42 0.2(4) . . . . ? C40 C41 C42 C37 0.4(3) . . . . ? C38 C37 C42 C41 -0.7(3) . . . . ? P24 C37 C42 C41 177.19(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.263 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 931189'