# 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_alb97sqz(6a) _database_code_depnum_ccdc_archive 'CCDC 904838' #TrackingRef 'alb97pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Br4 N4 Pt, C2 H6 O S, 0.7 (C2 H3 N)' _chemical_formula_sum 'C18.40 H32.1 Br4 N4.70 O Pt S' _chemical_formula_weight 881.94 _chemical_absolute_configuration ad 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' Br Br -0.2901 2.4595 '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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5992(2) _cell_length_b 14.1248(3) _cell_length_c 10.3387(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.272(2) _cell_angle_gamma 90.00 _cell_volume 1401.78(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18633 _cell_measurement_theta_min 3.4866 _cell_measurement_theta_max 29.6712 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2619 _exptl_crystal_size_mid 0.1835 _exptl_crystal_size_min 0.1671 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834.8 _exptl_absorpt_coefficient_mu 10.799 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.305 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24869 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 29.74 _reflns_number_total 6962 _reflns_number_gt 6818 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _computing_publication_material ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _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^)+(0.0612P)^2^+1.8031P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.038(8) _refine_ls_number_reflns 6962 _refine_ls_number_parameters 261 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Pt Pt 0.160578(19) 0.736136(15) 0.409446(17) 0.01508(6) Uani 1 1 d . . . Br1 Br -0.04368(6) 0.76650(4) 0.54524(6) 0.02259(13) Uani 1 1 d . . . Br2 Br 0.36621(6) 0.71007(4) 0.27135(6) 0.02450(14) Uani 1 1 d . . . Br3 Br 0.25316(7) 0.61958(4) 0.57617(6) 0.02441(13) Uani 1 1 d . . . Br4 Br 0.03373(7) 0.60263(4) 0.29410(6) 0.02427(13) Uani 1 1 d . . . C1 C 0.0960(6) 0.8289(4) 0.2755(5) 0.0191(11) Uani 1 1 d . . . C2 C 0.0682(6) 0.8151(5) 0.1483(6) 0.0239(12) Uani 1 1 d . . . H2 H 0.0680 0.7558 0.1049 0.029 Uiso 1 1 calc R . . N1 N 0.0401(6) 0.9020(4) 0.0924(5) 0.0238(11) Uani 1 1 d . . . C8 C 0.0155(9) 0.9176(6) -0.0476(6) 0.0360(17) Uani 1 1 d . . . H8 H -0.0419 0.9760 -0.0593 0.043 Uiso 1 1 calc R . . C9 C -0.0630(13) 0.8335(8) -0.1038(8) 0.064(3) Uani 1 1 d . . . H9A H -0.0082 0.7757 -0.0907 0.097 Uiso 1 1 calc R . . H9B H -0.0784 0.8435 -0.1966 0.097 Uiso 1 1 calc R . . H9C H -0.1530 0.8271 -0.0603 0.097 Uiso 1 1 calc R . . C10 C 0.1519(10) 0.9309(11) -0.1132(9) 0.073(4) Uani 1 1 d . . . H10A H 0.2044 0.9812 -0.0697 0.109 Uiso 1 1 calc R . . H10B H 0.1359 0.9484 -0.2038 0.109 Uiso 1 1 calc R . . H10C H 0.2051 0.8717 -0.1094 0.109 Uiso 1 1 calc R . . C3 C 0.0469(6) 0.9697(4) 0.1822(6) 0.0224(12) Uani 1 1 d . . . C11 C 0.0240(7) 1.0717(5) 0.1646(7) 0.0292(13) Uani 1 1 d . . . H11A H -0.0129 1.0835 0.0776 0.044 Uiso 1 1 calc R . . H11B H 0.1125 1.1054 0.1756 0.044 Uiso 1 1 calc R . . H11C H -0.0429 1.0943 0.2290 0.044 Uiso 1 1 calc R . . N2 N 0.0817(5) 0.9255(4) 0.2961(5) 0.0199(10) Uani 1 1 d . . . C4 C 0.0982(6) 0.9718(4) 0.4212(6) 0.0206(11) Uani 1 1 d . . . H4A H 0.0181 0.9568 0.4775 0.025 Uiso 1 1 calc R . . H4B H 0.1025 1.0414 0.4098 0.025 Uiso 1 1 calc R . . N3 N 0.2270(5) 0.9376(4) 0.4801(5) 0.0199(10) Uani 1 1 d . . . C5 C 0.3255(6) 0.9936(4) 0.5362(6) 0.0184(10) Uani 1 1 d . . . C12 C 0.3252(7) 1.0990(5) 0.5390(7) 0.0292(14) Uani 1 1 d . . . H12A H 0.2390 1.1215 0.5790 0.044 Uiso 1 1 calc R . . H12B H 0.3310 1.1235 0.4504 0.044 Uiso 1 1 calc R . . H12C H 0.4054 1.1216 0.5893 0.044 Uiso 1 1 calc R . . N4 N 0.4206(5) 0.9364(4) 0.5864(5) 0.0188(9) Uani 1 1 d . . . C13 C 0.5476(6) 0.9669(5) 0.6608(7) 0.0282(13) Uani 1 1 d . . . H13 H 0.5736 1.0322 0.6321 0.034 Uiso 1 1 calc R . . C14 C 0.5146(9) 0.9701(7) 0.8034(7) 0.043(2) Uani 1 1 d . . . H14A H 0.4386 1.0151 0.8183 0.065 Uiso 1 1 calc R . . H14B H 0.5974 0.9903 0.8518 0.065 Uiso 1 1 calc R . . H14C H 0.4862 0.9070 0.8325 0.065 Uiso 1 1 calc R . . C15 C 0.6691(7) 0.9015(6) 0.6345(10) 0.046(2) Uani 1 1 d . . . H15A H 0.6574 0.8428 0.6837 0.069 Uiso 1 1 calc R . . H15B H 0.7561 0.9325 0.6610 0.069 Uiso 1 1 calc R . . H15C H 0.6726 0.8869 0.5420 0.069 Uiso 1 1 calc R . . C6 C 0.3832(6) 0.8424(4) 0.5629(6) 0.0209(11) Uani 1 1 d . . . H6 H 0.4344 0.7881 0.5893 0.025 Uiso 1 1 calc R . . C7 C 0.2614(6) 0.8416(4) 0.4957(6) 0.0188(11) Uani 1 1 d . . . S S 0.6208(2) 0.89514(17) 0.1355(2) 0.0432(4) Uani 1 1 d . . . O O 0.7179(7) 0.9690(5) 0.0836(6) 0.0515(16) Uani 1 1 d . . . C16 C 0.4913(10) 0.9570(8) 0.2256(11) 0.059(3) Uani 1 1 d . . . H16A H 0.5361 0.9927 0.2957 0.089 Uiso 1 1 calc R . . H16B H 0.4253 0.9115 0.2623 0.089 Uiso 1 1 calc R . . H16C H 0.4414 1.0008 0.1683 0.089 Uiso 1 1 calc R . . C17 C 0.7142(10) 0.8402(13) 0.2651(13) 0.100(6) Uani 1 1 d . . . H17A H 0.7826 0.7958 0.2298 0.150 Uiso 1 1 calc R . . H17B H 0.6488 0.8059 0.3206 0.150 Uiso 1 1 calc R . . H17C H 0.7623 0.8888 0.3161 0.150 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01866(9) 0.01270(10) 0.01386(9) -0.00022(7) -0.00188(6) 0.00076(7) Br1 0.0220(3) 0.0231(3) 0.0227(3) -0.0047(2) 0.0039(2) -0.0015(2) Br2 0.0252(3) 0.0235(3) 0.0248(3) 0.0016(2) 0.0041(2) 0.0057(2) Br3 0.0329(3) 0.0197(3) 0.0206(3) 0.0029(2) -0.0053(2) 0.0016(2) Br4 0.0337(3) 0.0178(3) 0.0212(3) -0.0041(2) -0.0047(2) -0.0021(2) C1 0.018(2) 0.020(3) 0.019(3) -0.001(2) -0.002(2) 0.000(2) C2 0.030(3) 0.022(3) 0.020(3) 0.002(2) -0.002(2) 0.004(2) N1 0.028(2) 0.023(3) 0.021(2) 0.005(2) -0.0008(19) 0.007(2) C8 0.057(4) 0.034(4) 0.017(3) 0.005(3) 0.002(3) 0.019(3) C9 0.113(9) 0.058(6) 0.021(4) -0.004(4) -0.026(5) 0.004(6) C10 0.065(6) 0.111(11) 0.042(5) 0.039(6) 0.027(5) 0.046(6) C3 0.023(3) 0.021(3) 0.023(3) 0.001(2) 0.000(2) 0.003(2) C11 0.038(3) 0.020(3) 0.029(3) 0.009(3) -0.002(3) 0.004(3) N2 0.019(2) 0.019(3) 0.021(2) -0.0010(19) -0.0041(18) 0.0020(18) C4 0.021(3) 0.016(3) 0.025(3) -0.001(2) -0.008(2) 0.005(2) N3 0.022(2) 0.017(2) 0.021(2) -0.0023(19) -0.0029(18) 0.0032(18) C5 0.020(2) 0.015(3) 0.020(3) -0.002(2) 0.000(2) -0.001(2) C12 0.024(3) 0.021(3) 0.043(4) -0.004(3) -0.002(3) 0.001(2) N4 0.019(2) 0.014(2) 0.023(2) 0.0002(19) -0.0039(18) -0.0027(17) C13 0.021(3) 0.020(3) 0.044(4) -0.002(3) -0.006(3) -0.002(2) C14 0.049(4) 0.051(5) 0.030(4) 0.007(3) -0.015(3) -0.024(4) C15 0.020(3) 0.029(4) 0.088(7) -0.005(4) -0.015(4) 0.003(3) C6 0.024(3) 0.016(3) 0.023(3) 0.003(2) -0.003(2) 0.001(2) C7 0.023(3) 0.017(3) 0.016(3) 0.000(2) -0.003(2) 0.000(2) S 0.0432(10) 0.0450(12) 0.0413(10) 0.0024(9) -0.0046(8) -0.0035(9) O 0.050(3) 0.066(4) 0.039(3) 0.005(3) 0.000(3) -0.011(3) C16 0.054(5) 0.047(6) 0.076(7) -0.020(5) 0.021(5) -0.014(4) C17 0.033(4) 0.178(17) 0.089(9) 0.091(11) -0.017(5) -0.020(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C7 1.985(6) . ? Pt C1 2.003(6) . ? Pt Br1 2.4547(6) . ? Pt Br2 2.4692(6) . ? Pt Br4 2.5391(6) . ? Pt Br3 2.5410(6) . ? C1 C2 1.355(8) . ? C1 N2 1.387(8) . ? C2 N1 1.383(8) . ? C2 H2 0.9500 . ? N1 C3 1.335(8) . ? N1 C8 1.482(8) . ? C8 C10 1.489(12) . ? C8 C9 1.521(13) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C3 N2 1.374(8) . ? C3 C11 1.468(9) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N2 C4 1.458(7) . ? C4 N3 1.458(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N3 C5 1.360(7) . ? N3 C7 1.405(8) . ? C5 N4 1.324(7) . ? C5 C12 1.489(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N4 C6 1.396(8) . ? N4 C13 1.502(8) . ? C13 C14 1.510(11) . ? C13 C15 1.513(10) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C6 C7 1.357(8) . ? C6 H6 0.9500 . ? S O 1.500(7) . ? S C16 1.786(10) . ? S C17 1.787(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 C7 Pt C1 88.2(2) . . ? C7 Pt Br1 90.05(17) . . ? C1 Pt Br1 92.06(17) . . ? C7 Pt Br2 88.99(17) . . ? C1 Pt Br2 86.75(16) . . ? Br1 Pt Br2 178.49(2) . . ? C7 Pt Br4 178.67(17) . . ? C1 Pt Br4 90.87(17) . . ? Br1 Pt Br4 90.91(2) . . ? Br2 Pt Br4 90.03(2) . . ? C7 Pt Br3 90.76(17) . . ? C1 Pt Br3 177.53(16) . . ? Br1 Pt Br3 90.17(2) . . ? Br2 Pt Br3 91.01(2) . . ? Br4 Pt Br3 90.16(2) . . ? C2 C1 N2 105.8(5) . . ? C2 C1 Pt 129.5(5) . . ? N2 C1 Pt 124.6(4) . . ? C1 C2 N1 108.3(6) . . ? C1 C2 H2 125.8 . . ? N1 C2 H2 125.8 . . ? C3 N1 C2 109.7(5) . . ? C3 N1 C8 125.4(6) . . ? C2 N1 C8 124.7(6) . . ? N1 C8 C10 109.1(7) . . ? N1 C8 C9 109.5(6) . . ? C10 C8 C9 111.1(9) . . ? N1 C8 H8 109.0 . . ? C10 C8 H8 109.0 . . ? C9 C8 H8 109.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C3 N2 106.3(5) . . ? N1 C3 C11 127.7(6) . . ? N2 C3 C11 126.0(6) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 N2 C1 109.8(5) . . ? C3 N2 C4 125.5(5) . . ? C1 N2 C4 124.6(5) . . ? N2 C4 N3 108.0(5) . . ? N2 C4 H4A 110.1 . . ? N3 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? N3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C5 N3 C7 110.5(5) . . ? C5 N3 C4 124.8(5) . . ? C7 N3 C4 124.5(5) . . ? N4 C5 N3 106.8(5) . . ? N4 C5 C12 127.2(5) . . ? N3 C5 C12 126.0(5) . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N4 C6 109.6(5) . . ? C5 N4 C13 125.6(5) . . ? C6 N4 C13 124.8(5) . . ? N4 C13 C14 109.5(5) . . ? N4 C13 C15 110.9(6) . . ? C14 C13 C15 111.0(7) . . ? N4 C13 H13 108.4 . . ? C14 C13 H13 108.4 . . ? C15 C13 H13 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C6 N4 108.5(5) . . ? C7 C6 H6 125.7 . . ? N4 C6 H6 125.7 . . ? C6 C7 N3 104.6(5) . . ? C6 C7 Pt 130.8(5) . . ? N3 C7 Pt 124.0(4) . . ? O S C16 106.4(5) . . ? O S C17 105.1(5) . . ? C16 S C17 99.7(7) . . ? S C16 H16A 109.5 . . ? S C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S C17 H17A 109.5 . . ? S C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 C7 Pt C1 C2 148.5(6) . . . . ? Br1 Pt C1 C2 -121.5(6) . . . . ? Br2 Pt C1 C2 59.4(6) . . . . ? Br4 Pt C1 C2 -30.6(6) . . . . ? C7 Pt C1 N2 -25.9(5) . . . . ? Br1 Pt C1 N2 64.0(5) . . . . ? Br2 Pt C1 N2 -115.0(5) . . . . ? Br4 Pt C1 N2 155.0(5) . . . . ? N2 C1 C2 N1 1.1(7) . . . . ? Pt C1 C2 N1 -174.2(4) . . . . ? C1 C2 N1 C3 -1.2(7) . . . . ? C1 C2 N1 C8 175.0(6) . . . . ? C3 N1 C8 C10 89.7(9) . . . . ? C2 N1 C8 C10 -86.0(10) . . . . ? C3 N1 C8 C9 -148.5(7) . . . . ? C2 N1 C8 C9 35.8(10) . . . . ? C2 N1 C3 N2 0.8(7) . . . . ? C8 N1 C3 N2 -175.4(6) . . . . ? C2 N1 C3 C11 -179.9(6) . . . . ? C8 N1 C3 C11 3.9(11) . . . . ? N1 C3 N2 C1 -0.2(7) . . . . ? C11 C3 N2 C1 -179.4(6) . . . . ? N1 C3 N2 C4 -178.8(5) . . . . ? C11 C3 N2 C4 1.9(10) . . . . ? C2 C1 N2 C3 -0.6(7) . . . . ? Pt C1 N2 C3 175.0(4) . . . . ? C2 C1 N2 C4 178.1(5) . . . . ? Pt C1 N2 C4 -6.4(8) . . . . ? C3 N2 C4 N3 -133.4(6) . . . . ? C1 N2 C4 N3 48.2(7) . . . . ? N2 C4 N3 C5 133.3(6) . . . . ? N2 C4 N3 C7 -52.0(7) . . . . ? C7 N3 C5 N4 0.1(7) . . . . ? C4 N3 C5 N4 175.4(5) . . . . ? C7 N3 C5 C12 179.8(6) . . . . ? C4 N3 C5 C12 -4.9(10) . . . . ? N3 C5 N4 C6 -0.1(7) . . . . ? C12 C5 N4 C6 -179.8(6) . . . . ? N3 C5 N4 C13 -178.6(5) . . . . ? C12 C5 N4 C13 1.7(10) . . . . ? C5 N4 C13 C14 91.7(8) . . . . ? C6 N4 C13 C14 -86.5(8) . . . . ? C5 N4 C13 C15 -145.4(7) . . . . ? C6 N4 C13 C15 36.4(9) . . . . ? C5 N4 C6 C7 0.1(7) . . . . ? C13 N4 C6 C7 178.6(5) . . . . ? N4 C6 C7 N3 -0.1(7) . . . . ? N4 C6 C7 Pt 170.7(4) . . . . ? C5 N3 C7 C6 0.0(7) . . . . ? C4 N3 C7 C6 -175.3(5) . . . . ? C5 N3 C7 Pt -171.5(4) . . . . ? C4 N3 C7 Pt 13.1(8) . . . . ? C1 Pt C7 C6 -146.6(6) . . . . ? Br1 Pt C7 C6 121.4(6) . . . . ? Br2 Pt C7 C6 -59.8(6) . . . . ? Br3 Pt C7 C6 31.2(6) . . . . ? C1 Pt C7 N3 22.6(5) . . . . ? Br1 Pt C7 N3 -69.5(5) . . . . ? Br2 Pt C7 N3 109.4(5) . . . . ? Br3 Pt C7 N3 -159.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.453 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.136 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.474 0.186 1.056 100 15 '0.7 (C2 H3 N)' 2 0.525 0.686 0.944 100 15 '0.7 (C2 H3 N)' _platon_squeeze_details ; PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13 PLATON version from 20.02.2011 ; data_alb98(5a) _database_code_depnum_ccdc_archive 'CCDC 904839' #TrackingRef 'alb97pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Cl4 N4 Pt, C2 H6 O S, C2 H3 N' _chemical_formula_sum 'C19 H33 Cl4 N5 O Pt S' _chemical_formula_weight 716.45 _chemical_absolute_configuration ad 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3908(2) _cell_length_b 13.8861(2) _cell_length_c 10.1824(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.069(2) _cell_angle_gamma 90.00 _cell_volume 1327.80(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14519 _cell_measurement_theta_min 3.2874 _cell_measurement_theta_max 32.9462 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2818 _exptl_crystal_size_mid 0.1778 _exptl_crystal_size_min 0.1687 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 5.786 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.377 _exptl_absorpt_correction_T_max 0.495 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; The crystal was refined as an inversion twin. 3404 Friedel pairs were measured. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22108 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7023 _reflns_number_gt 6783 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _computing_publication_material ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _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^)+(0.0288P)^2^+1.2474P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.234(5) _refine_ls_number_reflns 7023 _refine_ls_number_parameters 290 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0604 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Pt Pt 0.160041(13) 0.735592(16) 0.412369(12) 0.01342(4) Uani 1 1 d . . . Cl1 Cl -0.04017(11) 0.76204(7) 0.54012(11) 0.0209(2) Uani 1 1 d . . . Cl2 Cl 0.36071(11) 0.71246(7) 0.28194(11) 0.0228(2) Uani 1 1 d . . . Cl3 Cl 0.24997(12) 0.62306(8) 0.57234(12) 0.0219(2) Uani 1 1 d . . . Cl4 Cl 0.04046(13) 0.60788(8) 0.29681(11) 0.0214(2) Uani 1 1 d . . . C1 C 0.0952(5) 0.8303(3) 0.2776(4) 0.0164(8) Uani 1 1 d . . . C2 C 0.0745(5) 0.8192(3) 0.1469(4) 0.0197(9) Uani 1 1 d . . . H2 H 0.0801 0.7601 0.1003 0.024 Uiso 1 1 calc R . . N1 N 0.0438(4) 0.9082(3) 0.0923(4) 0.0186(7) Uani 1 1 d . . . C8 C 0.0257(6) 0.9285(4) -0.0480(5) 0.0278(10) Uani 1 1 d . . . H8 H -0.0423 0.9834 -0.0579 0.033 Uiso 1 1 calc R . . C9 C -0.0361(8) 0.8414(5) -0.1170(6) 0.0449(15) Uani 1 1 d . . . H9A H 0.0288 0.7867 -0.1068 0.067 Uiso 1 1 calc R . . H9B H -0.0484 0.8558 -0.2105 0.067 Uiso 1 1 calc R . . H9C H -0.1286 0.8255 -0.0782 0.067 Uiso 1 1 calc R . . C10 C 0.1682(6) 0.9580(5) -0.1052(6) 0.0406(15) Uani 1 1 d . . . H10A H 0.2058 1.0131 -0.0560 0.061 Uiso 1 1 calc R . . H10B H 0.1557 0.9761 -0.1975 0.061 Uiso 1 1 calc R . . H10C H 0.2350 0.9040 -0.0989 0.061 Uiso 1 1 calc R . . C3 C 0.0456(5) 0.9747(3) 0.1888(4) 0.0187(8) Uani 1 1 d . . . C11 C 0.0201(5) 1.0803(3) 0.1715(5) 0.0241(9) Uani 1 1 d . . . H11A H -0.0222 1.0920 0.0849 0.036 Uiso 1 1 calc R . . H11B H 0.1107 1.1149 0.1783 0.036 Uiso 1 1 calc R . . H11C H -0.0450 1.1031 0.2399 0.036 Uiso 1 1 calc R . . N2 N 0.0773(4) 0.9285(3) 0.3012(4) 0.0172(7) Uani 1 1 d . . . C4 C 0.0897(4) 0.9733(3) 0.4304(4) 0.0167(8) Uani 1 1 d . . . H4A H 0.0081 0.9546 0.4863 0.020 Uiso 1 1 calc R . . H4B H 0.0902 1.0443 0.4217 0.020 Uiso 1 1 calc R . . N3 N 0.2238(4) 0.9400(3) 0.4892(4) 0.0162(7) Uani 1 1 d . . . C5 C 0.3251(4) 0.9970(3) 0.5427(4) 0.0173(8) Uani 1 1 d . . . C12 C 0.3224(5) 1.1038(3) 0.5449(5) 0.0245(10) Uani 1 1 d . . . H12A H 0.2437 1.1259 0.6003 0.037 Uiso 1 1 calc R . . H12B H 0.3092 1.1282 0.4553 0.037 Uiso 1 1 calc R . . H12C H 0.4127 1.1280 0.5803 0.037 Uiso 1 1 calc R . . N4 N 0.4261(4) 0.9389(3) 0.5905(4) 0.0168(7) Uani 1 1 d . . . C13 C 0.5587(5) 0.9711(3) 0.6582(5) 0.0233(9) Uani 1 1 d . . . H13 H 0.5839 1.0366 0.6249 0.028 Uiso 1 1 calc R . . C14 C 0.5331(7) 0.9779(5) 0.8038(6) 0.0429(16) Uani 1 1 d . . . H14A H 0.4542 1.0225 0.8206 0.064 Uiso 1 1 calc R . . H14B H 0.6194 1.0017 0.8473 0.064 Uiso 1 1 calc R . . H14C H 0.5090 0.9141 0.8383 0.064 Uiso 1 1 calc R . . C15 C 0.6815(5) 0.9036(4) 0.6285(8) 0.0439(17) Uani 1 1 d . . . H15A H 0.6804 0.8497 0.6907 0.066 Uiso 1 1 calc R . . H15B H 0.7717 0.9386 0.6367 0.066 Uiso 1 1 calc R . . H15C H 0.6718 0.8787 0.5388 0.066 Uiso 1 1 calc R . . C6 C 0.3883(4) 0.8438(3) 0.5660(4) 0.0176(8) Uani 1 1 d . . . H6 H 0.4421 0.7887 0.5906 0.021 Uiso 1 1 calc R . . C7 C 0.2619(5) 0.8427(3) 0.5012(5) 0.0168(8) Uani 1 1 d . . . S S 0.61774(16) 0.89475(11) 0.13180(15) 0.0372(3) Uani 1 1 d . . . O O 0.7217(4) 0.9692(3) 0.0827(4) 0.0442(10) Uani 1 1 d . . . C16 C 0.4998(8) 0.9572(6) 0.2382(8) 0.062(2) Uani 1 1 d . . . H16A H 0.5540 0.9863 0.3102 0.092 Uiso 1 1 calc R . . H16B H 0.4299 0.9119 0.2741 0.092 Uiso 1 1 calc R . . H16C H 0.4503 1.0077 0.1889 0.092 Uiso 1 1 calc R . . C17 C 0.7117(8) 0.8247(9) 0.2483(12) 0.118(5) Uani 1 1 d . . . H17A H 0.7774 0.7813 0.2026 0.176 Uiso 1 1 calc R . . H17B H 0.6441 0.7868 0.3001 0.176 Uiso 1 1 calc R . . H17C H 0.7658 0.8673 0.3067 0.176 Uiso 1 1 calc R . . N5 N 0.6313(10) 0.6792(8) 0.8530(19) 0.179(7) Uani 1 1 d . . . C18 C 0.5248(10) 0.6859(7) 0.8913(12) 0.088(3) Uani 1 1 d . . . C19 C 0.3746(7) 0.6943(5) 0.9143(7) 0.0464(15) Uani 1 1 d . . . H19A H 0.3307 0.7307 0.8424 0.070 Uiso 1 1 calc R . . H19B H 0.3584 0.7280 0.9975 0.070 Uiso 1 1 calc R . . H19C H 0.3322 0.6299 0.9186 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01415(6) 0.01233(6) 0.01379(6) -0.00013(7) -0.00216(4) 0.00014(7) Cl1 0.0175(5) 0.0233(6) 0.0219(5) -0.0036(3) 0.0026(4) -0.0008(3) Cl2 0.0212(5) 0.0233(6) 0.0241(5) 0.0013(4) 0.0032(4) 0.0042(4) Cl3 0.0282(6) 0.0177(5) 0.0198(5) 0.0040(4) -0.0047(4) 0.0027(4) Cl4 0.0268(6) 0.0165(5) 0.0207(5) -0.0041(4) -0.0052(4) -0.0020(4) C1 0.013(2) 0.016(2) 0.021(2) -0.0009(16) -0.0029(16) 0.0017(16) C2 0.024(2) 0.018(2) 0.017(2) -0.0002(16) -0.0010(16) 0.0049(17) N1 0.0209(18) 0.0161(17) 0.0188(19) 0.0036(14) -0.0046(14) 0.0049(14) C8 0.036(3) 0.029(2) 0.019(2) 0.0036(18) -0.0004(19) 0.008(2) C9 0.071(5) 0.040(3) 0.023(3) -0.003(2) -0.018(3) 0.003(3) C10 0.034(3) 0.048(4) 0.040(3) 0.015(3) 0.010(3) 0.014(3) C3 0.017(2) 0.018(2) 0.021(2) 0.0032(16) -0.0026(16) 0.0028(16) C11 0.026(2) 0.019(2) 0.027(2) 0.0017(19) -0.0026(19) 0.0051(18) N2 0.0133(16) 0.0183(18) 0.0199(18) 0.0004(14) -0.0042(13) 0.0011(14) C4 0.016(2) 0.0154(19) 0.019(2) -0.0034(16) -0.0074(16) 0.0005(15) N3 0.0154(17) 0.0152(16) 0.0179(18) -0.0029(13) -0.0034(13) 0.0001(13) C5 0.017(2) 0.0157(19) 0.019(2) -0.0004(16) -0.0004(15) -0.0009(15) C12 0.023(2) 0.017(2) 0.034(3) -0.0023(18) -0.0082(19) 0.0014(17) N4 0.0122(16) 0.0163(16) 0.0219(18) -0.0006(14) -0.0052(13) 0.0003(13) C13 0.015(2) 0.024(2) 0.031(3) -0.0004(19) -0.0085(18) -0.0033(17) C14 0.047(4) 0.050(4) 0.031(3) 0.007(3) -0.014(3) -0.019(3) C15 0.015(2) 0.024(3) 0.093(5) -0.003(3) -0.010(3) 0.002(2) C6 0.0128(19) 0.020(2) 0.020(2) 0.0003(16) -0.0024(15) 0.0015(16) C7 0.020(2) 0.015(2) 0.015(2) -0.0001(16) -0.0008(17) -0.0003(16) S 0.0340(7) 0.0395(8) 0.0381(8) 0.0030(6) -0.0016(6) -0.0033(6) O 0.036(2) 0.056(3) 0.040(2) 0.010(2) 0.0006(18) -0.012(2) C16 0.060(5) 0.047(4) 0.077(6) -0.020(4) 0.033(4) -0.014(4) C17 0.035(4) 0.168(11) 0.149(10) 0.132(9) -0.008(5) -0.009(5) N5 0.042(5) 0.081(7) 0.41(2) 0.003(10) 0.016(9) 0.014(5) C18 0.061(6) 0.064(5) 0.139(10) -0.013(6) 0.014(6) -0.018(4) C19 0.060(4) 0.042(3) 0.038(3) 0.001(3) -0.003(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C7 1.986(4) . ? Pt C1 1.996(5) . ? Pt Cl1 2.3168(10) . ? Pt Cl2 2.3290(10) . ? Pt Cl4 2.4058(11) . ? Pt Cl3 2.4094(11) . ? C1 C2 1.353(6) . ? C1 N2 1.394(6) . ? C2 N1 1.385(5) . ? C2 H2 0.9500 . ? N1 C3 1.349(6) . ? N1 C8 1.465(6) . ? C8 C9 1.513(8) . ? C8 C10 1.516(7) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C3 N2 1.345(6) . ? C3 C11 1.497(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N2 C4 1.460(5) . ? C4 N3 1.469(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N3 C5 1.351(5) . ? N3 C7 1.403(5) . ? C5 N4 1.337(6) . ? C5 C12 1.485(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N4 C6 1.390(6) . ? N4 C13 1.491(5) . ? C13 C14 1.505(8) . ? C13 C15 1.517(7) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C6 C7 1.357(6) . ? C6 H6 0.9500 . ? S O 1.507(4) . ? S C17 1.769(8) . ? S C16 1.776(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N5 C18 1.078(12) . ? C18 C19 1.434(12) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 C7 Pt C1 88.07(18) . . ? C7 Pt Cl1 90.94(13) . . ? C1 Pt Cl1 91.97(13) . . ? C7 Pt Cl2 88.47(13) . . ? C1 Pt Cl2 86.87(13) . . ? Cl1 Pt Cl2 178.71(4) . . ? C7 Pt Cl4 177.79(14) . . ? C1 Pt Cl4 90.44(13) . . ? Cl1 Pt Cl4 90.74(4) . . ? Cl2 Pt Cl4 89.83(4) . . ? C7 Pt Cl3 90.53(13) . . ? C1 Pt Cl3 177.26(13) . . ? Cl1 Pt Cl3 90.41(4) . . ? Cl2 Pt Cl3 90.74(4) . . ? Cl4 Pt Cl3 90.89(4) . . ? C2 C1 N2 105.3(4) . . ? C2 C1 Pt 130.1(4) . . ? N2 C1 Pt 124.2(3) . . ? C1 C2 N1 108.8(4) . . ? C1 C2 H2 125.6 . . ? N1 C2 H2 125.6 . . ? C3 N1 C2 108.4(4) . . ? C3 N1 C8 125.4(4) . . ? C2 N1 C8 126.0(4) . . ? N1 C8 C9 110.0(4) . . ? N1 C8 C10 109.0(4) . . ? C9 C8 C10 112.1(5) . . ? N1 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C10 C8 H8 108.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C3 N1 107.2(4) . . ? N2 C3 C11 127.1(4) . . ? N1 C3 C11 125.7(4) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 N2 C1 110.3(4) . . ? C3 N2 C4 125.5(4) . . ? C1 N2 C4 124.3(4) . . ? N2 C4 N3 107.5(3) . . ? N2 C4 H4A 110.2 . . ? N3 C4 H4A 110.2 . . ? N2 C4 H4B 110.2 . . ? N3 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C5 N3 C7 110.4(4) . . ? C5 N3 C4 125.7(3) . . ? C7 N3 C4 123.9(3) . . ? N4 C5 N3 107.0(4) . . ? N4 C5 C12 127.6(4) . . ? N3 C5 C12 125.4(4) . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N4 C6 109.1(3) . . ? C5 N4 C13 125.4(4) . . ? C6 N4 C13 125.5(4) . . ? N4 C13 C14 109.9(4) . . ? N4 C13 C15 110.9(4) . . ? C14 C13 C15 111.0(5) . . ? N4 C13 H13 108.3 . . ? C14 C13 H13 108.3 . . ? C15 C13 H13 108.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C6 N4 108.7(4) . . ? C7 C6 H6 125.6 . . ? N4 C6 H6 125.6 . . ? C6 C7 N3 104.7(4) . . ? C6 C7 Pt 130.6(3) . . ? N3 C7 Pt 124.0(3) . . ? O S C17 106.0(3) . . ? O S C16 105.8(3) . . ? C17 S C16 99.8(5) . . ? S C16 H16A 109.5 . . ? S C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S C17 H17A 109.5 . . ? S C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C19 168.1(16) . . ? 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 . . ? 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 C7 Pt C1 C2 144.7(5) . . . . ? Cl1 Pt C1 C2 -124.5(4) . . . . ? Cl2 Pt C1 C2 56.1(4) . . . . ? Cl4 Pt C1 C2 -33.7(4) . . . . ? C7 Pt C1 N2 -27.4(4) . . . . ? Cl1 Pt C1 N2 63.5(4) . . . . ? Cl2 Pt C1 N2 -116.0(4) . . . . ? Cl4 Pt C1 N2 154.2(4) . . . . ? N2 C1 C2 N1 -0.4(5) . . . . ? Pt C1 C2 N1 -173.6(3) . . . . ? C1 C2 N1 C3 0.1(5) . . . . ? C1 C2 N1 C8 174.8(4) . . . . ? C3 N1 C8 C9 -154.6(5) . . . . ? C2 N1 C8 C9 31.6(7) . . . . ? C3 N1 C8 C10 82.2(6) . . . . ? C2 N1 C8 C10 -91.6(6) . . . . ? C2 N1 C3 N2 0.2(5) . . . . ? C8 N1 C3 N2 -174.5(4) . . . . ? C2 N1 C3 C11 179.0(4) . . . . ? C8 N1 C3 C11 4.3(7) . . . . ? N1 C3 N2 C1 -0.5(5) . . . . ? C11 C3 N2 C1 -179.2(4) . . . . ? N1 C3 N2 C4 -179.7(4) . . . . ? C11 C3 N2 C4 1.5(7) . . . . ? C2 C1 N2 C3 0.6(5) . . . . ? Pt C1 N2 C3 174.3(3) . . . . ? C2 C1 N2 C4 179.8(4) . . . . ? Pt C1 N2 C4 -6.5(6) . . . . ? C3 N2 C4 N3 -131.2(4) . . . . ? C1 N2 C4 N3 49.7(5) . . . . ? N2 C4 N3 C5 129.5(4) . . . . ? N2 C4 N3 C7 -52.7(5) . . . . ? C7 N3 C5 N4 -1.0(5) . . . . ? C4 N3 C5 N4 177.1(4) . . . . ? C7 N3 C5 C12 178.4(4) . . . . ? C4 N3 C5 C12 -3.5(7) . . . . ? N3 C5 N4 C6 0.4(5) . . . . ? C12 C5 N4 C6 -178.9(4) . . . . ? N3 C5 N4 C13 179.9(4) . . . . ? C12 C5 N4 C13 0.5(7) . . . . ? C5 N4 C13 C14 90.8(6) . . . . ? C6 N4 C13 C14 -89.9(6) . . . . ? C5 N4 C13 C15 -146.2(5) . . . . ? C6 N4 C13 C15 33.2(6) . . . . ? C5 N4 C6 C7 0.3(5) . . . . ? C13 N4 C6 C7 -179.2(4) . . . . ? N4 C6 C7 N3 -0.8(5) . . . . ? N4 C6 C7 Pt 169.5(3) . . . . ? C5 N3 C7 C6 1.1(5) . . . . ? C4 N3 C7 C6 -177.0(4) . . . . ? C5 N3 C7 Pt -170.0(3) . . . . ? C4 N3 C7 Pt 11.8(6) . . . . ? C1 Pt C7 C6 -144.1(4) . . . . ? Cl1 Pt C7 C6 124.0(4) . . . . ? Cl2 Pt C7 C6 -57.2(4) . . . . ? Cl3 Pt C7 C6 33.6(4) . . . . ? C1 Pt C7 N3 24.6(4) . . . . ? Cl1 Pt C7 N3 -67.3(4) . . . . ? Cl2 Pt C7 N3 111.6(4) . . . . ? Cl3 Pt C7 N3 -157.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.021 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.105 data_alb99_sqz _database_code_depnum_ccdc_archive 'CCDC 904840' #TrackingRef 'alb97pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Br2 N4 Pt, 2.36 (C H2 Cl2)' _chemical_formula_sum 'C17.36 H28.73 Br2 Cl4.73 N4 Pt ' _chemical_formula_weight 815.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.1521(3) _cell_length_b 17.9528(4) _cell_length_c 22.5774(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5736.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18518 _cell_measurement_theta_min 3.3912 _cell_measurement_theta_max 24.6894 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3114 _exptl_absorpt_coefficient_mu 8.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65303 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Combined with sherical absorption correction, mu*r was assumed to be 0.75 ; _exptl_special_details ; The crystal was selected at low temperature after the method first described by Kottke und Stalke (T, Kottke, D. Stalke, J. Appl. Cryst. 1993 (26), 615). The temperature of the oil was -11 deg. C when the crystals were placed on the slide and was not monitored afterwards. The PLATON "squeeze" procedure was used to treat regions of diffuse solvent(s) which could not be modelled in terms of atomic sites. The number of electrons thus located, 23 per asymmetric unit, is included in the formula, formula weight, calculated density, \m and F(000). This residual electron density was assigned to 0.6 molecules of dichloromethane per asymmetric unit. 0.6 molecules of dichloromethane would give 25 e^-^. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52351 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 24.74 _reflns_number_total 4890 _reflns_number_gt 4276 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _computing_publication_material ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _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^)+(0.0283P)^2^+39.2681P] 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 4890 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Pt Pt 0.636808(15) 0.222990(12) 0.255574(10) 0.01905(9) Uani 1 1 d . . . Br1 Br 0.68145(4) 0.24605(4) 0.36126(3) 0.02782(15) Uani 1 1 d . . . Br2 Br 0.74907(4) 0.11542(3) 0.24982(3) 0.02518(15) Uani 1 1 d . . . C1 C 0.5969(4) 0.2078(3) 0.1730(3) 0.0208(12) Uani 1 1 d . . . C2 C 0.6411(4) 0.1842(3) 0.1231(3) 0.0223(13) Uani 1 1 d . . . H2 H 0.7042 0.1663 0.1212 0.027 Uiso 1 1 calc R . . N1 N 0.5797(4) 0.1902(3) 0.0750(2) 0.0276(12) Uani 1 1 d . . . C8 C 0.6010(5) 0.1683(4) 0.0125(3) 0.0371(17) Uani 1 1 d . . . H8 H 0.5757 0.2080 -0.0143 0.045 Uiso 1 1 calc R . . C9 C 0.7064(5) 0.1634(5) 0.0030(3) 0.0427(18) Uani 1 1 d . . . H9A H 0.7362 0.2098 0.0161 0.064 Uiso 1 1 calc R . . H9B H 0.7196 0.1555 -0.0391 0.064 Uiso 1 1 calc R . . H9C H 0.7318 0.1216 0.0260 0.064 Uiso 1 1 calc R . . C10 C 0.5527(6) 0.0965(5) -0.0027(3) 0.050(2) Uani 1 1 d . . . H10A H 0.5796 0.0561 0.0212 0.075 Uiso 1 1 calc R . . H10B H 0.5619 0.0855 -0.0448 0.075 Uiso 1 1 calc R . . H10C H 0.4850 0.1008 0.0056 0.075 Uiso 1 1 calc R . . C3 C 0.4972(4) 0.2166(3) 0.0940(3) 0.0247(13) Uani 1 1 d . . . C11 C 0.4128(5) 0.2344(4) 0.0577(3) 0.0348(16) Uani 1 1 d . . . H11A H 0.3587 0.2055 0.0721 0.052 Uiso 1 1 calc R . . H11B H 0.4252 0.2217 0.0162 0.052 Uiso 1 1 calc R . . H11C H 0.3988 0.2877 0.0609 0.052 Uiso 1 1 calc R . . N2 N 0.5059(3) 0.2267(3) 0.1529(2) 0.0203(10) Uani 1 1 d . . . C4 C 0.4303(4) 0.2496(3) 0.1932(3) 0.0221(13) Uani 1 1 d . . . H4A H 0.3737 0.2645 0.1704 0.027 Uiso 1 1 calc R . . H4B H 0.4129 0.2077 0.2196 0.027 Uiso 1 1 calc R . . N3 N 0.4643(3) 0.3116(3) 0.2279(2) 0.0222(11) Uani 1 1 d . . . C5 C 0.4203(4) 0.3771(3) 0.2365(3) 0.0249(13) Uani 1 1 d . . . C12 C 0.3257(5) 0.3971(4) 0.2135(3) 0.0350(16) Uani 1 1 d . . . H12A H 0.3244 0.3899 0.1705 0.053 Uiso 1 1 calc R . . H12B H 0.3122 0.4493 0.2227 0.053 Uiso 1 1 calc R . . H12C H 0.2779 0.3652 0.2321 0.053 Uiso 1 1 calc R . . N4 N 0.4767(4) 0.4183(3) 0.2700(2) 0.0265(12) Uani 1 1 d . . . C13 C 0.4621(5) 0.4990(3) 0.2837(3) 0.0322(15) Uani 1 1 d . . . H13 H 0.3927 0.5088 0.2866 0.039 Uiso 1 1 calc R . . C14 C 0.5022(5) 0.5446(4) 0.2320(4) 0.0426(19) Uani 1 1 d . . . H14A H 0.5708 0.5378 0.2301 0.064 Uiso 1 1 calc R . . H14B H 0.4877 0.5974 0.2380 0.064 Uiso 1 1 calc R . . H14C H 0.4736 0.5276 0.1948 0.064 Uiso 1 1 calc R . . C15 C 0.5070(7) 0.5186(4) 0.3415(4) 0.058(2) Uani 1 1 d . . . H15A H 0.4827 0.4857 0.3725 0.087 Uiso 1 1 calc R . . H15B H 0.4922 0.5705 0.3514 0.087 Uiso 1 1 calc R . . H15C H 0.5757 0.5126 0.3384 0.087 Uiso 1 1 calc R . . C6 C 0.5573(4) 0.3777(3) 0.2839(3) 0.0247(13) Uani 1 1 d . . . H6 H 0.6085 0.3947 0.3074 0.030 Uiso 1 1 calc R . . C7 C 0.5505(4) 0.3094(3) 0.2581(3) 0.0226(13) Uani 1 1 d . . . C16 C 0.9228(5) 0.2023(4) 0.1390(3) 0.0397(17) Uani 1 1 d . . . H16A H 0.9853 0.2085 0.1580 0.048 Uiso 1 1 calc R . . H16B H 0.8788 0.1817 0.1689 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.88108(14) 0.29034(12) 0.11532(9) 0.0500(5) Uani 1 1 d . . . Cl2 Cl 0.93288(15) 0.13945(12) 0.08012(10) 0.0544(5) Uani 1 1 d . . . C17 C 0.3274(8) 0.5547(6) 0.0876(5) 0.048(3) Uani 0.763(6) 1 d P . . H17A H 0.3276 0.5624 0.1310 0.058 Uiso 0.763(6) 1 calc PR . . H17B H 0.3532 0.6003 0.0689 0.058 Uiso 0.763(6) 1 calc PR . . Cl3 Cl 0.4018(2) 0.47735(16) 0.06978(14) 0.0640(11) Uani 0.763(6) 1 d P . . Cl4 Cl 0.2154(2) 0.5418(2) 0.06446(19) 0.0880(15) Uani 0.763(6) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01351(12) 0.01725(13) 0.02638(14) 0.00075(9) -0.00185(9) 0.00078(8) Br1 0.0205(3) 0.0331(3) 0.0299(3) -0.0014(3) -0.0034(3) 0.0003(3) Br2 0.0169(3) 0.0216(3) 0.0369(3) -0.0023(2) -0.0041(3) 0.0031(2) C1 0.009(3) 0.024(3) 0.029(3) 0.000(2) -0.004(2) -0.001(2) C2 0.013(3) 0.028(3) 0.026(3) 0.002(3) -0.003(2) 0.002(2) N1 0.021(3) 0.034(3) 0.028(3) 0.003(2) 0.000(2) 0.003(2) C8 0.028(4) 0.058(5) 0.025(3) 0.004(3) -0.001(3) 0.003(3) C9 0.033(4) 0.067(5) 0.028(4) 0.000(3) 0.001(3) 0.003(4) C10 0.045(5) 0.064(5) 0.041(4) -0.017(4) 0.007(4) -0.008(4) C3 0.013(3) 0.029(3) 0.032(3) 0.003(3) 0.000(3) 0.002(2) C11 0.022(3) 0.049(4) 0.033(4) 0.000(3) -0.001(3) 0.007(3) N2 0.018(2) 0.020(2) 0.023(3) 0.000(2) -0.001(2) 0.001(2) C4 0.016(3) 0.020(3) 0.029(3) 0.000(2) 0.000(2) -0.001(2) N3 0.016(3) 0.020(3) 0.030(3) 0.001(2) -0.003(2) 0.002(2) C5 0.017(3) 0.021(3) 0.036(4) -0.001(3) 0.002(3) 0.004(2) C12 0.027(4) 0.028(4) 0.050(4) -0.006(3) -0.010(3) 0.011(3) N4 0.025(3) 0.015(2) 0.039(3) 0.001(2) -0.002(2) 0.001(2) C13 0.026(4) 0.020(3) 0.050(4) -0.008(3) -0.005(3) 0.007(3) C14 0.033(4) 0.023(3) 0.072(6) -0.004(3) 0.010(4) -0.004(3) C15 0.081(7) 0.039(4) 0.054(5) -0.017(4) -0.024(5) 0.028(4) C6 0.015(3) 0.023(3) 0.036(4) -0.004(3) -0.001(3) 0.001(2) C7 0.014(3) 0.022(3) 0.031(3) 0.004(3) 0.001(2) -0.004(2) C16 0.026(4) 0.053(5) 0.040(4) 0.005(3) -0.006(3) -0.008(3) Cl1 0.0469(11) 0.0499(12) 0.0532(12) -0.0037(9) -0.0030(9) 0.0019(9) Cl2 0.0512(12) 0.0513(12) 0.0606(13) -0.0058(10) -0.0156(10) 0.0061(9) C17 0.054(7) 0.041(6) 0.051(6) -0.012(5) 0.002(5) -0.006(5) Cl3 0.077(2) 0.0440(16) 0.071(2) -0.0145(14) 0.0109(16) -0.0006(14) Cl4 0.0474(19) 0.103(3) 0.113(3) -0.053(2) 0.0023(18) -0.0176(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 Pt C1 1.966(6) . ? Pt C7 1.976(6) . ? Pt Br1 2.5027(6) . ? Pt Br2 2.5041(6) . ? C1 C2 1.358(8) . ? C1 N2 1.407(7) . ? C2 N1 1.395(8) . ? C2 H2 0.9500 . ? N1 C3 1.330(8) . ? N1 C8 1.496(8) . ? C8 C10 1.500(11) . ? C8 C9 1.509(10) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C3 N2 1.348(8) . ? C3 C11 1.483(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N2 C4 1.464(7) . ? C4 N3 1.444(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N3 C5 1.345(8) . ? N3 C7 1.398(7) . ? C5 N4 1.325(8) . ? C5 C12 1.480(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N4 C6 1.389(8) . ? N4 C13 1.495(7) . ? C13 C15 1.494(10) . ? C13 C14 1.534(10) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C6 C7 1.359(8) . ? C6 H6 0.9500 . ? C16 Cl2 1.749(8) . ? C16 Cl1 1.770(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 Cl4 1.685(11) . ? C17 Cl3 1.789(11) . ? C17 H17A 0.9900 . ? C17 H17B 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 C1 Pt C7 87.7(2) . . ? C1 Pt Br1 177.47(17) . . ? C7 Pt Br1 89.89(18) . . ? C1 Pt Br2 91.49(17) . . ? C7 Pt Br2 178.21(17) . . ? Br1 Pt Br2 90.97(2) . . ? C2 C1 N2 103.2(5) . . ? C2 C1 Pt 134.3(4) . . ? N2 C1 Pt 122.4(4) . . ? C1 C2 N1 109.6(5) . . ? C1 C2 H2 125.2 . . ? N1 C2 H2 125.2 . . ? C3 N1 C2 108.9(5) . . ? C3 N1 C8 125.1(5) . . ? C2 N1 C8 126.0(5) . . ? N1 C8 C10 110.4(6) . . ? N1 C8 C9 110.4(5) . . ? C10 C8 C9 111.6(7) . . ? N1 C8 H8 108.1 . . ? C10 C8 H8 108.1 . . ? C9 C8 H8 108.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C3 N2 106.6(5) . . ? N1 C3 C11 127.3(6) . . ? N2 C3 C11 126.1(5) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 N2 C1 111.7(5) . . ? C3 N2 C4 125.9(5) . . ? C1 N2 C4 122.3(5) . . ? N3 C4 N2 108.1(4) . . ? N3 C4 H4A 110.1 . . ? N2 C4 H4A 110.1 . . ? N3 C4 H4B 110.1 . . ? N2 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C5 N3 C7 111.0(5) . . ? C5 N3 C4 126.8(5) . . ? C7 N3 C4 122.3(5) . . ? N4 C5 N3 107.0(5) . . ? N4 C5 C12 127.6(5) . . ? N3 C5 C12 125.4(6) . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N4 C6 109.2(5) . . ? C5 N4 C13 125.1(5) . . ? C6 N4 C13 125.2(5) . . ? C15 C13 N4 110.5(5) . . ? C15 C13 C14 112.4(6) . . ? N4 C13 C14 108.0(5) . . ? C15 C13 H13 108.6 . . ? N4 C13 H13 108.6 . . ? C14 C13 H13 108.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C6 N4 108.6(5) . . ? C7 C6 H6 125.7 . . ? N4 C6 H6 125.7 . . ? C6 C7 N3 104.2(5) . . ? C6 C7 Pt 132.6(5) . . ? N3 C7 Pt 123.1(4) . . ? Cl2 C16 Cl1 112.0(4) . . ? Cl2 C16 H16A 109.2 . . ? Cl1 C16 H16A 109.2 . . ? Cl2 C16 H16B 109.2 . . ? Cl1 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? Cl4 C17 Cl3 112.1(6) . . ? Cl4 C17 H17A 109.2 . . ? Cl3 C17 H17A 109.2 . . ? Cl4 C17 H17B 109.2 . . ? Cl3 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? 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 C7 Pt C1 C2 144.6(6) . . . . ? Br2 Pt C1 C2 -33.9(6) . . . . ? C7 Pt C1 N2 -30.9(5) . . . . ? Br2 Pt C1 N2 150.7(4) . . . . ? N2 C1 C2 N1 1.1(6) . . . . ? Pt C1 C2 N1 -174.9(5) . . . . ? C1 C2 N1 C3 -0.5(7) . . . . ? C1 C2 N1 C8 -178.6(6) . . . . ? C3 N1 C8 C10 -73.3(8) . . . . ? C2 N1 C8 C10 104.5(7) . . . . ? C3 N1 C8 C9 162.9(6) . . . . ? C2 N1 C8 C9 -19.3(9) . . . . ? C2 N1 C3 N2 -0.4(7) . . . . ? C8 N1 C3 N2 177.8(6) . . . . ? C2 N1 C3 C11 177.6(6) . . . . ? C8 N1 C3 C11 -4.3(10) . . . . ? N1 C3 N2 C1 1.1(7) . . . . ? C11 C3 N2 C1 -176.9(6) . . . . ? N1 C3 N2 C4 -174.9(5) . . . . ? C11 C3 N2 C4 7.1(10) . . . . ? C2 C1 N2 C3 -1.4(6) . . . . ? Pt C1 N2 C3 175.3(4) . . . . ? C2 C1 N2 C4 174.8(5) . . . . ? Pt C1 N2 C4 -8.5(7) . . . . ? C3 N2 C4 N3 -129.2(6) . . . . ? C1 N2 C4 N3 55.1(7) . . . . ? N2 C4 N3 C5 129.8(6) . . . . ? N2 C4 N3 C7 -51.0(7) . . . . ? C7 N3 C5 N4 1.8(7) . . . . ? C4 N3 C5 N4 -178.9(5) . . . . ? C7 N3 C5 C12 -176.8(6) . . . . ? C4 N3 C5 C12 2.4(10) . . . . ? N3 C5 N4 C6 -1.1(7) . . . . ? C12 C5 N4 C6 177.5(6) . . . . ? N3 C5 N4 C13 171.1(6) . . . . ? C12 C5 N4 C13 -10.2(11) . . . . ? C5 N4 C13 C15 153.4(7) . . . . ? C6 N4 C13 C15 -35.5(9) . . . . ? C5 N4 C13 C14 -83.3(8) . . . . ? C6 N4 C13 C14 87.8(7) . . . . ? C5 N4 C6 C7 0.1(7) . . . . ? C13 N4 C6 C7 -172.2(6) . . . . ? N4 C6 C7 N3 1.0(7) . . . . ? N4 C6 C7 Pt 178.0(5) . . . . ? C5 N3 C7 C6 -1.8(7) . . . . ? C4 N3 C7 C6 178.9(5) . . . . ? C5 N3 C7 Pt -179.1(4) . . . . ? C4 N3 C7 Pt 1.5(8) . . . . ? C1 Pt C7 C6 -141.8(6) . . . . ? Br1 Pt C7 C6 38.9(6) . . . . ? C1 Pt C7 N3 34.7(5) . . . . ? Br1 Pt C7 N3 -144.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.74 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.246 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.136 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.184 0.075 0.900 114 23 '0.6 (C H2 Cl2)' 2 0.184 0.425 0.400 114 23 '0.6 (C H2 Cl2)' 3 0.316 0.575 0.900 114 23 '0.6 (C H2 Cl2)' 4 0.316 0.925 0.400 113 23 '0.6 (C H2 Cl2)' 5 0.684 0.075 0.600 114 23 '0.6 (C H2 Cl2)' 6 0.684 0.425 0.100 114 23 '0.6 (C H2 Cl2)' 7 0.816 0.575 0.600 114 23 '0.6 (C H2 Cl2)' 8 0.816 0.925 0.100 113 23 '0.6 (C H2 Cl2)' _platon_squeeze_details ; PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13 PLATON version from 27.07.2012 ; data_alb158(2a1) _database_code_depnum_ccdc_archive 'CCDC 904841' #TrackingRef 'alb97pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H30 Cl N4 O Pt S, B F4' _chemical_formula_sum 'C17 H30 B Cl F4 N4 O Pt S' _chemical_formula_weight 655.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7668(2) _cell_length_b 21.4564(3) _cell_length_c 10.0029(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.872(2) _cell_angle_gamma 90.00 _cell_volume 2451.80(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 18179 _cell_measurement_theta_min 2.8236 _cell_measurement_theta_max 26.3368 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1122 _exptl_crystal_size_mid 0.0795 _exptl_crystal_size_min 0.0413 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 5.963 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39691 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5027 _reflns_number_gt 4390 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _computing_publication_material ; PLATON (A. L. Spek, J. Appl. Cryst. 2003, 36, 7) ; _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^)+(0.0202P)^2^+4.0871P] 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 5027 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Pt Pt 0.299397(12) 0.201473(6) 0.637579(15) 0.03216(5) Uani 1 1 d . . . Cl Cl 0.31904(9) 0.09210(4) 0.65986(12) 0.0504(3) Uani 1 1 d . . . C1 C 0.2752(3) 0.29310(16) 0.6210(4) 0.0346(8) Uani 1 1 d . . . C2 C 0.3170(4) 0.34118(17) 0.7051(5) 0.0442(9) Uani 1 1 d . . . H2 H 0.3679 0.3375 0.7941 0.053 Uiso 1 1 calc R . . N1 N 0.2749(3) 0.39649(14) 0.6427(3) 0.0406(8) Uani 1 1 d . . . C8 C 0.2978(5) 0.4594(2) 0.7049(6) 0.0710(16) Uani 1 1 d . . . H8 H 0.2848 0.4916 0.6306 0.085 Uiso 1 1 calc R . . C9 C 0.2131(9) 0.4704(3) 0.7971(7) 0.131(3) Uani 1 1 d . . . H9A H 0.2355 0.4440 0.8792 0.196 Uiso 1 1 calc R . . H9B H 0.1334 0.4600 0.7463 0.196 Uiso 1 1 calc R . . H9C H 0.2163 0.5143 0.8250 0.196 Uiso 1 1 calc R . . C10 C 0.4189(8) 0.4634(3) 0.7887(13) 0.203(6) Uani 1 1 d . . . H10A H 0.4339 0.4290 0.8548 0.304 Uiso 1 1 calc R . . H10B H 0.4300 0.5032 0.8384 0.304 Uiso 1 1 calc R . . H10C H 0.4733 0.4608 0.7285 0.304 Uiso 1 1 calc R . . C3 C 0.2018(4) 0.38427(17) 0.5222(4) 0.0415(9) Uani 1 1 d . . . C11 C 0.1386(4) 0.43004(19) 0.4187(5) 0.0554(12) Uani 1 1 d . . . H11A H 0.1315 0.4698 0.4643 0.083 Uiso 1 1 calc R . . H11B H 0.0604 0.4140 0.3756 0.083 Uiso 1 1 calc R . . H11C H 0.1825 0.4364 0.3479 0.083 Uiso 1 1 calc R . . N2 N 0.2004(3) 0.32175(14) 0.5066(3) 0.0353(7) Uani 1 1 d . . . C4 C 0.1382(4) 0.28887(18) 0.3853(4) 0.0445(10) Uani 1 1 d . . . H4A H 0.1938 0.2759 0.3304 0.053 Uiso 1 1 calc R . . H4B H 0.0794 0.3169 0.3278 0.053 Uiso 1 1 calc R . . N3 N 0.0798(3) 0.23408(13) 0.4240(3) 0.0336(7) Uani 1 1 d . . . C5 C -0.0272(3) 0.21470(17) 0.3598(4) 0.0369(8) Uani 1 1 d . . . C12 C -0.1103(4) 0.24809(19) 0.2472(4) 0.0541(12) Uani 1 1 d . . . H12A H -0.1870 0.2276 0.2290 0.081 Uiso 1 1 calc R . . H12B H -0.0807 0.2473 0.1637 0.081 Uiso 1 1 calc R . . H12C H -0.1182 0.2914 0.2748 0.081 Uiso 1 1 calc R . . N4 N -0.0434(3) 0.15956(13) 0.4134(3) 0.0359(7) Uani 1 1 d . . . C13 C -0.1521(3) 0.12165(18) 0.3749(4) 0.0424(9) Uani 1 1 d . . . H13 H -0.1936 0.1329 0.2786 0.051 Uiso 1 1 calc R . . C14 C -0.1224(4) 0.05300(19) 0.3774(5) 0.0599(13) Uani 1 1 d . . . H14A H -0.0659 0.0457 0.3213 0.090 Uiso 1 1 calc R . . H14B H -0.1937 0.0289 0.3399 0.090 Uiso 1 1 calc R . . H14C H -0.0884 0.0399 0.4724 0.090 Uiso 1 1 calc R . . C15 C -0.2321(4) 0.1376(2) 0.4683(5) 0.0571(12) Uani 1 1 d . . . H15A H -0.1928 0.1277 0.5638 0.086 Uiso 1 1 calc R . . H15B H -0.3046 0.1134 0.4408 0.086 Uiso 1 1 calc R . . H15C H -0.2507 0.1822 0.4607 0.086 Uiso 1 1 calc R . . C6 C 0.0568(3) 0.14426(17) 0.5129(4) 0.0353(8) Uani 1 1 d . . . H6 H 0.0677 0.1073 0.5668 0.042 Uiso 1 1 calc R . . C7 C 0.1370(3) 0.19072(16) 0.5208(4) 0.0313(8) Uani 1 1 d . . . S S 0.48649(9) 0.21015(5) 0.77121(12) 0.0438(2) Uani 1 1 d . . . O O 0.5378(3) 0.27180(15) 0.8112(4) 0.0715(10) Uani 1 1 d . . . C16 C 0.5023(4) 0.1663(2) 0.9248(5) 0.0592(12) Uani 1 1 d . . . H16A H 0.5847 0.1664 0.9755 0.089 Uiso 1 1 calc R . . H16B H 0.4767 0.1233 0.9018 0.089 Uiso 1 1 calc R . . H16C H 0.4544 0.1850 0.9820 0.089 Uiso 1 1 calc R . . C17 C 0.5796(4) 0.1694(2) 0.6849(5) 0.0560(11) Uani 1 1 d . . . H17A H 0.5838 0.1921 0.6012 0.084 Uiso 1 1 calc R . . H17B H 0.5482 0.1275 0.6602 0.084 Uiso 1 1 calc R . . H17C H 0.6582 0.1661 0.7458 0.084 Uiso 1 1 calc R . . B B 0.1510(6) 0.6214(2) 0.5142(6) 0.0560(14) Uani 1 1 d . . . F1 F 0.1447(3) 0.60393(14) 0.6462(3) 0.0753(8) Uani 1 1 d . A . F2A F 0.2076(5) 0.67993(18) 0.5284(5) 0.0617(16) Uani 0.734(12) 1 d P A 1 F3A F 0.0485(4) 0.6252(4) 0.4244(6) 0.085(3) Uani 0.734(12) 1 d P A 1 F4A F 0.2276(6) 0.5813(2) 0.4722(7) 0.087(2) Uani 0.734(12) 1 d P A 1 F2B F 0.095(2) 0.5677(7) 0.4403(16) 0.139(11) Uani 0.266(12) 1 d P A 2 F3B F 0.2304(13) 0.637(2) 0.476(2) 0.167(19) Uani 0.266(12) 1 d P A 2 F4B F 0.0445(15) 0.6598(8) 0.481(2) 0.082(5) Uani 0.266(12) 1 d P 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 Pt 0.02935(8) 0.02881(8) 0.03895(9) -0.00141(6) 0.00941(6) 0.00053(5) Cl 0.0471(6) 0.0302(5) 0.0678(7) 0.0002(4) 0.0018(5) 0.0015(4) C1 0.034(2) 0.0334(19) 0.040(2) 0.0035(16) 0.0148(16) 0.0024(15) C2 0.045(2) 0.034(2) 0.050(2) 0.0009(18) 0.0062(19) 0.0003(17) N1 0.055(2) 0.0259(15) 0.0396(18) -0.0009(13) 0.0090(16) -0.0034(14) C8 0.104(4) 0.025(2) 0.075(4) -0.004(2) 0.003(3) 0.001(2) C9 0.266(11) 0.057(4) 0.084(5) -0.007(3) 0.071(6) 0.020(5) C10 0.128(7) 0.050(4) 0.359(16) -0.046(6) -0.080(9) -0.024(4) C3 0.045(2) 0.0322(19) 0.053(3) 0.0096(17) 0.0221(19) -0.0017(16) C11 0.061(3) 0.040(2) 0.067(3) 0.018(2) 0.018(2) 0.001(2) N2 0.0371(17) 0.0332(15) 0.0384(18) 0.0045(13) 0.0149(14) -0.0040(13) C4 0.059(3) 0.043(2) 0.035(2) 0.0087(17) 0.0174(19) -0.0063(19) N3 0.0417(18) 0.0303(15) 0.0282(16) 0.0027(12) 0.0072(13) 0.0005(13) C5 0.045(2) 0.0326(19) 0.0309(19) -0.0027(15) 0.0046(16) 0.0048(16) C12 0.068(3) 0.038(2) 0.045(2) -0.0036(18) -0.009(2) 0.008(2) N4 0.0384(18) 0.0307(16) 0.0350(17) -0.0031(13) 0.0019(13) 0.0017(13) C13 0.038(2) 0.038(2) 0.044(2) -0.0073(17) -0.0036(17) -0.0038(16) C14 0.054(3) 0.039(2) 0.083(4) -0.015(2) 0.008(2) -0.007(2) C15 0.042(3) 0.058(3) 0.071(3) -0.008(2) 0.011(2) -0.002(2) C6 0.038(2) 0.0326(18) 0.0322(19) 0.0002(15) 0.0026(16) -0.0001(15) C7 0.0317(19) 0.0374(19) 0.0260(18) -0.0024(14) 0.0092(14) -0.0018(15) S 0.0294(5) 0.0410(5) 0.0589(7) -0.0052(5) 0.0063(4) 0.0002(4) O 0.0439(18) 0.0443(17) 0.114(3) -0.0135(18) -0.0048(19) -0.0053(14) C16 0.046(3) 0.079(3) 0.049(3) -0.004(2) 0.005(2) 0.006(2) C17 0.038(2) 0.066(3) 0.067(3) 0.002(2) 0.020(2) 0.010(2) B 0.069(4) 0.046(3) 0.049(3) 0.003(2) 0.005(3) 0.002(3) F1 0.095(2) 0.0723(19) 0.0556(17) 0.0157(14) 0.0122(15) -0.0106(17) F2A 0.074(3) 0.044(2) 0.059(3) 0.0094(18) 0.001(2) -0.0117(19) F3A 0.050(3) 0.134(7) 0.063(3) 0.020(3) -0.001(2) -0.028(3) F4A 0.116(5) 0.057(3) 0.094(4) -0.002(3) 0.039(3) 0.006(3) F2B 0.24(3) 0.069(10) 0.093(12) -0.037(8) 0.012(13) 0.013(13) F3B 0.038(8) 0.35(6) 0.109(17) 0.09(3) 0.017(9) -0.018(19) F4B 0.091(10) 0.081(10) 0.080(11) 0.019(8) 0.037(8) 0.035(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 1.988(3) . ? Pt C7 2.000(4) . ? Pt S 2.2928(10) . ? Pt Cl 2.3634(9) . ? C1 C2 1.347(5) . ? C1 N2 1.407(5) . ? C2 N1 1.377(5) . ? C2 H2 0.9500 . ? N1 C3 1.328(5) . ? N1 C8 1.484(5) . ? C8 C10 1.472(9) . ? C8 C9 1.529(10) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C3 N2 1.350(5) . ? C3 C11 1.490(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? N2 C4 1.442(5) . ? C4 N3 1.460(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N3 C5 1.335(5) . ? N3 C7 1.394(4) . ? C5 N4 1.331(5) . ? C5 C12 1.487(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N4 C6 1.387(5) . ? N4 C13 1.487(5) . ? C13 C14 1.513(6) . ? C13 C15 1.516(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C6 C7 1.362(5) . ? C6 H6 0.9500 . ? S O 1.469(3) . ? S C16 1.773(5) . ? S C17 1.779(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? B F3B 1.140(16) . ? B F3A 1.322(7) . ? B F4A 1.382(8) . ? B F1 1.392(6) . ? B F2A 1.412(7) . ? B F2B 1.441(18) . ? B F4B 1.470(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt C7 88.15(15) . . ? C1 Pt S 93.82(11) . . ? C7 Pt S 178.03(10) . . ? C1 Pt Cl 177.18(11) . . ? C7 Pt Cl 89.93(10) . . ? S Pt Cl 88.12(4) . . ? C2 C1 N2 103.7(3) . . ? C2 C1 Pt 133.0(3) . . ? N2 C1 Pt 123.3(3) . . ? C1 C2 N1 109.8(4) . . ? C1 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? C3 N1 C2 109.0(3) . . ? C3 N1 C8 125.0(3) . . ? C2 N1 C8 125.8(4) . . ? C10 C8 N1 110.2(5) . . ? C10 C8 C9 109.2(7) . . ? N1 C8 C9 108.3(5) . . ? C10 C8 H8 109.7 . . ? N1 C8 H8 109.7 . . ? C9 C8 H8 109.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C3 N2 106.8(3) . . ? N1 C3 C11 127.4(4) . . ? N2 C3 C11 125.7(4) . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C3 N2 C1 110.6(3) . . ? C3 N2 C4 125.0(3) . . ? C1 N2 C4 124.2(3) . . ? N2 C4 N3 110.3(3) . . ? N2 C4 H4A 109.6 . . ? N3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? N3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C5 N3 C7 111.6(3) . . ? C5 N3 C4 125.0(3) . . ? C7 N3 C4 122.8(3) . . ? N4 C5 N3 107.0(3) . . ? N4 C5 C12 127.0(4) . . ? N3 C5 C12 126.0(4) . . ? C5 C12 H12A 109.5 . . ? C5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N4 C6 108.7(3) . . ? C5 N4 C13 125.4(3) . . ? C6 N4 C13 125.9(3) . . ? N4 C13 C14 110.3(3) . . ? N4 C13 C15 109.9(3) . . ? C14 C13 C15 112.7(4) . . ? N4 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C6 N4 109.0(3) . . ? C7 C6 H6 125.5 . . ? N4 C6 H6 125.5 . . ? C6 C7 N3 103.7(3) . . ? C6 C7 Pt 132.1(3) . . ? N3 C7 Pt 124.3(2) . . ? O S C16 106.9(2) . . ? O S C17 108.3(2) . . ? C16 S C17 102.1(2) . . ? O S Pt 120.40(14) . . ? C16 S Pt 110.42(16) . . ? C17 S Pt 107.12(16) . . ? S C16 H16A 109.5 . . ? S C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S C17 H17A 109.5 . . ? S C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? F3A B F4A 112.8(6) . . ? F3B B F1 129.2(11) . . ? F3A B F1 114.4(6) . . ? F4A B F1 107.9(5) . . ? F3A B F2A 110.2(5) . . ? F4A B F2A 105.0(6) . . ? F1 B F2A 106.0(4) . . ? F3B B F2B 111(2) . . ? F1 B F2B 98.6(9) . . ? F3B B F4B 119.1(18) . . ? F1 B F4B 97.5(8) . . ? F2B B F4B 94.1(12) . . ? 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 C7 Pt C1 C2 149.4(4) . . . . ? S Pt C1 C2 -30.8(4) . . . . ? C7 Pt C1 N2 -28.9(3) . . . . ? S Pt C1 N2 150.9(3) . . . . ? N2 C1 C2 N1 -2.9(4) . . . . ? Pt C1 C2 N1 178.5(3) . . . . ? C1 C2 N1 C3 3.1(5) . . . . ? C1 C2 N1 C8 177.6(4) . . . . ? C3 N1 C8 C10 -148.9(7) . . . . ? C2 N1 C8 C10 37.6(9) . . . . ? C3 N1 C8 C9 91.7(6) . . . . ? C2 N1 C8 C9 -81.9(6) . . . . ? C2 N1 C3 N2 -1.9(4) . . . . ? C8 N1 C3 N2 -176.3(4) . . . . ? C2 N1 C3 C11 -178.1(4) . . . . ? C8 N1 C3 C11 7.4(7) . . . . ? N1 C3 N2 C1 0.0(4) . . . . ? C11 C3 N2 C1 176.4(4) . . . . ? N1 C3 N2 C4 -175.6(3) . . . . ? C11 C3 N2 C4 0.8(6) . . . . ? C2 C1 N2 C3 1.8(4) . . . . ? Pt C1 N2 C3 -179.4(3) . . . . ? C2 C1 N2 C4 177.5(4) . . . . ? Pt C1 N2 C4 -3.8(5) . . . . ? C3 N2 C4 N3 -137.2(4) . . . . ? C1 N2 C4 N3 47.8(5) . . . . ? N2 C4 N3 C5 139.8(4) . . . . ? N2 C4 N3 C7 -49.7(5) . . . . ? C7 N3 C5 N4 0.9(4) . . . . ? C4 N3 C5 N4 172.2(3) . . . . ? C7 N3 C5 C12 -177.5(4) . . . . ? C4 N3 C5 C12 -6.2(6) . . . . ? N3 C5 N4 C6 -0.3(4) . . . . ? C12 C5 N4 C6 178.0(4) . . . . ? N3 C5 N4 C13 178.2(3) . . . . ? C12 C5 N4 C13 -3.4(6) . . . . ? C5 N4 C13 C14 143.7(4) . . . . ? C6 N4 C13 C14 -37.9(5) . . . . ? C5 N4 C13 C15 -91.5(5) . . . . ? C6 N4 C13 C15 86.9(5) . . . . ? C5 N4 C6 C7 -0.3(4) . . . . ? C13 N4 C6 C7 -178.9(3) . . . . ? N4 C6 C7 N3 0.8(4) . . . . ? N4 C6 C7 Pt -179.7(3) . . . . ? C5 N3 C7 C6 -1.0(4) . . . . ? C4 N3 C7 C6 -172.6(3) . . . . ? C5 N3 C7 Pt 179.4(3) . . . . ? C4 N3 C7 Pt 7.8(5) . . . . ? C1 Pt C7 C6 -152.4(4) . . . . ? Cl Pt C7 C6 25.5(4) . . . . ? C1 Pt C7 N3 27.1(3) . . . . ? Cl Pt C7 N3 -155.0(3) . . . . ? C1 Pt S O 1.2(2) . . . . ? Cl Pt S O -176.7(2) . . . . ? C1 Pt S C16 126.6(2) . . . . ? Cl Pt S C16 -51.36(18) . . . . ? C1 Pt S C17 -122.9(2) . . . . ? Cl Pt S C17 59.10(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.223 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.085 data_compound2a _database_code_depnum_ccdc_archive 'CCDC 904842' #TrackingRef 'alb97pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Cl2 N4 Pt, 1.5 (C2 H6 O S)' _chemical_formula_sum 'C18 H33 Cl2 N4 O1.50 Pt S1.50' _chemical_formula_weight 643.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 7.1071(9) _cell_length_b 14.0822(12) _cell_length_c 28.851(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.917(16) _cell_angle_gamma 90.00 _cell_volume 2872.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 5.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.450 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; The PLATON "squeeze" procedure was used to treat regions of diffuse solvent(s) which could not be modelled in terms of atomic sites. The number of electrons thus located, 223 per unit cell, is included in the formula, formula weight, calculated density, \m and F(000). This residual electron density was assigned to 6 molecules of dimethylsulfoxide per unit cell. 6 molecules of dimethylsulfoxide would give 252 e^-^. ; _diffrn_ambient_temperature 223(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20289 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_sigmaI/netI 0.2304 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4923 _reflns_number_gt 2225 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The bond lengths from the central atoms of the isopropyl groups (C7, C12) to the disordered methyl groups (C8, C8A, C9, C9A, C13, C13A, C14, C14A) were restrained to be 1.5 \%A using DFIX. ; _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^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4923 _refine_ls_number_parameters 149 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 0.568 _refine_ls_restrained_S_all 0.568 _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 C1 C -0.0585(10) 0.2210(7) 0.3518(3) 0.0418(11) Uani 1 1 d . . . C4 C 0.2238(9) 0.2485(7) 0.3076(3) 0.038(2) Uani 1 1 d . . . H4A H 0.3469 0.2804 0.3123 0.045 Uiso 1 1 calc R . . H4B H 0.2446 0.1825 0.2986 0.045 Uiso 1 1 calc R . . C7 C -0.0858(9) 0.2731(6) 0.2601(3) 0.0332(9) Uani 1 1 d . . . C6 C -0.1322(9) 0.3261(7) 0.2196(2) 0.0332(9) Uani 1 1 d . . . H6 H -0.2518 0.3271 0.2023 0.040 Uiso 1 1 calc R . . C5 C 0.1685(10) 0.3587(6) 0.2414(3) 0.0332(9) Uani 1 1 d . . . C10 C 0.3594(11) 0.4023(7) 0.2438(3) 0.045(3) Uani 1 1 d . . . H10A H 0.4467 0.3582 0.2316 0.067 Uiso 1 1 calc R . . H10B H 0.4029 0.4170 0.2760 0.067 Uiso 1 1 calc R . . H10C H 0.3534 0.4603 0.2256 0.067 Uiso 1 1 calc R . . C11 C 0.0269(11) 0.4376(7) 0.1674(3) 0.049(2) Uani 1 1 d D . . H11 H 0.1014 0.4946 0.1778 0.059 Uiso 0.50 1 calc PR A 1 H11A H 0.1376 0.4803 0.1728 0.059 Uiso 0.50 1 d PR A 2 C8 C 0.141(2) 0.3849(16) 0.1339(6) 0.049(2) Uani 0.50 1 d PD B 1 H8A H 0.2750 0.3919 0.1439 0.073 Uiso 0.50 1 calc PR B 1 H8B H 0.1137 0.4111 0.1028 0.073 Uiso 0.50 1 calc PR B 1 H8C H 0.1077 0.3181 0.1335 0.073 Uiso 0.50 1 calc PR B 1 C8A C 0.055(2) 0.3756(15) 0.1257(6) 0.049(2) Uani 0.50 1 d PD B 2 H8D H 0.1801 0.3474 0.1298 0.073 Uiso 0.50 1 calc PR B 2 H8E H 0.0424 0.4141 0.0976 0.073 Uiso 0.50 1 calc PR B 2 H8F H -0.0397 0.3258 0.1230 0.073 Uiso 0.50 1 calc PR B 2 C9 C -0.161(2) 0.4722(17) 0.1474(7) 0.049(2) Uani 0.50 1 d PD B 1 H9A H -0.2145 0.4276 0.1240 0.073 Uiso 0.50 1 calc PR B 1 H9B H -0.1470 0.5338 0.1331 0.073 Uiso 0.50 1 calc PR B 1 H9C H -0.2438 0.4777 0.1719 0.073 Uiso 0.50 1 calc PR B 1 C9A C -0.153(2) 0.4991(16) 0.1638(7) 0.049(2) Uani 0.50 1 d PD B 2 H9D H -0.2589 0.4624 0.1497 0.073 Uiso 0.50 1 calc PR B 2 H9E H -0.1343 0.5545 0.1447 0.073 Uiso 0.50 1 calc PR B 2 H9F H -0.1777 0.5194 0.1947 0.073 Uiso 0.50 1 calc PR B 2 C3 C 0.2162(10) 0.2716(6) 0.3936(3) 0.0418(11) Uani 1 1 d . . . C2 C -0.0793(10) 0.2284(6) 0.3976(3) 0.0418(11) Uani 1 1 d . . . H2 H -0.1919 0.2150 0.4107 0.050 Uiso 1 1 calc R . . C12 C 0.1103(14) 0.2812(8) 0.4744(3) 0.070(3) Uani 1 1 d D . . H12 H 0.2481 0.2770 0.4836 0.083 Uiso 0.50 1 calc PR C 1 H12A H 0.2454 0.2947 0.4839 0.083 Uiso 0.50 1 d PR C 2 C13 C 0.062(3) 0.3840(13) 0.4797(9) 0.070(3) Uani 0.50 1 d PD D 1 H13A H 0.1427 0.4225 0.4620 0.104 Uiso 0.50 1 calc PR D 1 H13B H 0.0821 0.4015 0.5123 0.104 Uiso 0.50 1 calc PR D 1 H13C H -0.0692 0.3945 0.4681 0.104 Uiso 0.50 1 calc PR D 1 C13A C -0.007(3) 0.3690(14) 0.4825(9) 0.070(3) Uani 0.50 1 d PD D 2 H13D H -0.1405 0.3534 0.4770 0.104 Uiso 0.50 1 calc PR D 2 H13E H 0.0226 0.4190 0.4613 0.104 Uiso 0.50 1 calc PR D 2 H13F H 0.0218 0.3904 0.5144 0.104 Uiso 0.50 1 calc PR D 2 C14 C 0.023(5) 0.2111(19) 0.5054(9) 0.070(3) Uani 0.50 1 d PD D 1 H14A H -0.1039 0.1953 0.4919 0.104 Uiso 0.50 1 calc PR D 1 H14B H 0.0170 0.2390 0.5360 0.104 Uiso 0.50 1 calc PR D 1 H14C H 0.0993 0.1539 0.5084 0.104 Uiso 0.50 1 calc PR D 1 C14A C 0.031(5) 0.1939(19) 0.4976(9) 0.070(3) Uani 0.50 1 d PD D 2 H14D H -0.0975 0.2070 0.5044 0.104 Uiso 0.50 1 calc PR D 2 H14E H 0.1091 0.1797 0.5263 0.104 Uiso 0.50 1 calc PR D 2 H14F H 0.0304 0.1400 0.4766 0.104 Uiso 0.50 1 calc PR D 2 C15 C 0.4101(10) 0.3061(10) 0.4048(3) 0.054(3) Uani 1 1 d . . . H15A H 0.4114 0.3749 0.4031 0.081 Uiso 1 1 calc R . . H15B H 0.4904 0.2802 0.3827 0.081 Uiso 1 1 calc R . . H15C H 0.4568 0.2861 0.4361 0.081 Uiso 1 1 calc R . . Cl1 Cl -0.4161(3) 0.09923(17) 0.34501(7) 0.0400(6) Uani 1 1 d . . . Cl2 Cl -0.4554(3) 0.15996(17) 0.23074(7) 0.0443(7) Uani 1 1 d . . . N2 N 0.1321(8) 0.2510(5) 0.3508(2) 0.0418(11) Uani 1 1 d . . . N3 N 0.1044(7) 0.2958(6) 0.2713(2) 0.0332(9) Uani 1 1 d . . . N4 N 0.0227(8) 0.3766(5) 0.2087(2) 0.0332(9) Uani 1 1 d . B . N1 N 0.0864(8) 0.2584(5) 0.4226(2) 0.0418(11) Uani 1 1 d . D . Pt1 Pt -0.23401(4) 0.19206(3) 0.297324(13) 0.03275(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0285(16) 0.058(3) 0.038(2) 0.002(2) 0.0016(16) 0.0051(17) C4 0.022(4) 0.055(7) 0.037(5) 0.014(4) 0.008(4) 0.018(4) C7 0.0286(16) 0.032(3) 0.039(2) -0.0008(18) -0.0004(15) 0.0028(16) C6 0.0286(16) 0.032(3) 0.039(2) -0.0008(18) -0.0004(15) 0.0028(16) C5 0.0286(16) 0.032(3) 0.039(2) -0.0008(18) -0.0004(15) 0.0028(16) C10 0.034(5) 0.051(8) 0.047(6) 0.010(5) -0.007(4) -0.008(5) C11 0.049(4) 0.053(6) 0.043(5) 0.006(4) -0.004(4) -0.008(4) C8 0.049(4) 0.053(6) 0.043(5) 0.006(4) -0.004(4) -0.008(4) C8A 0.049(4) 0.053(6) 0.043(5) 0.006(4) -0.004(4) -0.008(4) C9 0.049(4) 0.053(6) 0.043(5) 0.006(4) -0.004(4) -0.008(4) C9A 0.049(4) 0.053(6) 0.043(5) 0.006(4) -0.004(4) -0.008(4) C3 0.0285(16) 0.058(3) 0.038(2) 0.002(2) 0.0016(16) 0.0051(17) C2 0.0285(16) 0.058(3) 0.038(2) 0.002(2) 0.0016(16) 0.0051(17) C12 0.078(5) 0.096(9) 0.035(4) -0.013(4) 0.005(4) -0.005(5) C13 0.078(5) 0.096(9) 0.035(4) -0.013(4) 0.005(4) -0.005(5) C13A 0.078(5) 0.096(9) 0.035(4) -0.013(4) 0.005(4) -0.005(5) C14 0.078(5) 0.096(9) 0.035(4) -0.013(4) 0.005(4) -0.005(5) C14A 0.078(5) 0.096(9) 0.035(4) -0.013(4) 0.005(4) -0.005(5) C15 0.042(4) 0.067(8) 0.051(6) 0.015(8) -0.009(4) 0.016(7) Cl1 0.0389(11) 0.0375(18) 0.0452(14) 0.0077(11) 0.0118(10) -0.0039(10) Cl2 0.0462(12) 0.045(2) 0.0396(13) -0.0022(11) -0.0044(10) -0.0091(10) N2 0.0285(16) 0.058(3) 0.038(2) 0.002(2) 0.0016(16) 0.0051(17) N3 0.0286(16) 0.032(3) 0.039(2) -0.0008(18) -0.0004(15) 0.0028(16) N4 0.0286(16) 0.032(3) 0.039(2) -0.0008(18) -0.0004(15) 0.0028(16) N1 0.0285(16) 0.058(3) 0.038(2) 0.002(2) 0.0016(16) 0.0051(17) Pt1 0.03052(14) 0.0324(2) 0.03535(16) 0.0017(3) 0.00358(10) 0.0004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.348(10) . ? C1 N2 1.422(9) . ? C1 Pt1 1.946(8) . ? C4 N3 1.439(9) . ? C4 N2 1.465(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C7 N3 1.395(8) . ? C7 C6 1.397(10) . ? C7 Pt1 1.950(8) . ? C6 N4 1.374(9) . ? C6 H6 0.9400 . ? C5 N3 1.350(10) . ? C5 N4 1.352(9) . ? C5 C10 1.484(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 N4 1.470(11) . ? C11 C9 1.480(15) . ? C11 C8A 1.517(15) . ? C11 C8 1.519(15) . ? C11 C9A 1.536(15) . ? C11 H11 0.9900 . ? C11 H11A 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C8A H8D 0.9700 . ? C8A H8E 0.9700 . ? C8A H8F 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C9A H9D 0.9700 . ? C9A H9E 0.9700 . ? C9A H9F 0.9700 . ? C3 N1 1.322(9) . ? C3 N2 1.347(10) . ? C3 C15 1.465(11) . ? C2 N1 1.383(9) . ? C2 H2 0.9400 . ? C12 C13 1.499(17) . ? C12 C14 1.510(17) . ? C12 N1 1.520(11) . ? C12 C13A 1.524(16) . ? C12 C14A 1.534(18) . ? C12 H12 0.9900 . ? C12 H12A 0.9900 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C13A H13D 0.9700 . ? C13A H13E 0.9700 . ? C13A H13F 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C14A H14D 0.9700 . ? C14A H14E 0.9700 . ? C14A H14F 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? Cl1 Pt1 2.376(2) . ? Cl2 Pt1 2.398(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 101.4(7) . . ? C2 C1 Pt1 132.9(6) . . ? N2 C1 Pt1 125.3(6) . . ? N3 C4 N2 109.0(5) . . ? N3 C4 H4A 109.9 . . ? N2 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? N2 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N3 C7 C6 102.3(6) . . ? N3 C7 Pt1 124.8(6) . . ? C6 C7 Pt1 132.8(5) . . ? N4 C6 C7 110.0(6) . . ? N4 C6 H6 125.0 . . ? C7 C6 H6 125.0 . . ? N3 C5 N4 106.5(6) . . ? N3 C5 C10 127.5(7) . . ? N4 C5 C10 126.0(8) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C9 114.5(11) . . ? N4 C11 C8A 108.8(11) . . ? N4 C11 C8 106.7(11) . . ? C9 C11 C8 115.5(12) . . ? N4 C11 C9A 107.3(11) . . ? C8A C11 C9A 116.5(11) . . ? N4 C11 H11 106.5 . . ? C9 C11 H11 106.5 . . ? C8 C11 H11 106.5 . . ? N4 C11 H11A 108.1 . . ? C8A C11 H11A 107.9 . . ? C9A C11 H11A 108.0 . . ? C11 C8 H8A 109.5 . . ? C11 C8 H8B 109.5 . . ? C11 C8 H8C 109.5 . . ? C11 C8A H8D 109.5 . . ? C11 C8A H8E 109.5 . . ? H8D C8A H8E 109.5 . . ? C11 C8A H8F 109.5 . . ? H8D C8A H8F 109.5 . . ? H8E C8A H8F 109.5 . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? C11 C9A H9D 109.5 . . ? C11 C9A H9E 109.5 . . ? H9D C9A H9E 109.5 . . ? C11 C9A H9F 109.5 . . ? H9D C9A H9F 109.5 . . ? H9E C9A H9F 109.5 . . ? N1 C3 N2 106.1(6) . . ? N1 C3 C15 127.5(8) . . ? N2 C3 C15 126.4(7) . . ? C1 C2 N1 111.2(7) . . ? C1 C2 H2 124.4 . . ? N1 C2 H2 124.4 . . ? C13 C12 C14 117.3(16) . . ? C13 C12 N1 107.5(12) . . ? C14 C12 N1 115.8(14) . . ? N1 C12 C13A 108.4(12) . . ? N1 C12 C14A 104.5(12) . . ? C13A C12 C14A 110.5(16) . . ? C13 C12 H12 105.0 . . ? C14 C12 H12 105.0 . . ? N1 C12 H12 105.0 . . ? N1 C12 H12A 108.7 . . ? C13A C12 H12A 109.4 . . ? C14A C12 H12A 115.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? C12 C13A H13D 109.5 . . ? C12 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C12 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C14A H14D 109.5 . . ? C12 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C12 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C3 C15 H15A 109.5 . . ? C3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 N2 C1 112.3(6) . . ? C3 N2 C4 126.2(6) . . ? C1 N2 C4 121.2(7) . . ? C5 N3 C7 112.6(6) . . ? C5 N3 C4 123.8(6) . . ? C7 N3 C4 123.2(7) . . ? C5 N4 C6 108.6(7) . . ? C5 N4 C11 126.6(7) . . ? C6 N4 C11 124.9(6) . . ? C3 N1 C2 108.9(7) . . ? C3 N1 C12 125.3(7) . . ? C2 N1 C12 125.5(7) . . ? C1 Pt1 C7 89.1(3) . . ? C1 Pt1 Cl1 89.4(2) . . ? C7 Pt1 Cl1 177.4(3) . . ? C1 Pt1 Cl2 178.4(3) . . ? C7 Pt1 Cl2 90.9(2) . . ? Cl1 Pt1 Cl2 90.49(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 N3 C7 C6 N4 -0.4(9) . . . . ? Pt1 C7 C6 N4 176.1(6) . . . . ? N2 C1 C2 N1 -1.3(9) . . . . ? Pt1 C1 C2 N1 -175.1(7) . . . . ? N1 C3 N2 C1 -1.4(10) . . . . ? C15 C3 N2 C1 -178.8(10) . . . . ? N1 C3 N2 C4 -175.2(7) . . . . ? C15 C3 N2 C4 7.5(15) . . . . ? C2 C1 N2 C3 1.7(10) . . . . ? Pt1 C1 N2 C3 176.1(7) . . . . ? C2 C1 N2 C4 175.8(7) . . . . ? Pt1 C1 N2 C4 -9.8(11) . . . . ? N3 C4 N2 C3 -135.7(9) . . . . ? N3 C4 N2 C1 51.0(10) . . . . ? N4 C5 N3 C7 -2.0(9) . . . . ? C10 C5 N3 C7 176.7(8) . . . . ? N4 C5 N3 C4 171.1(7) . . . . ? C10 C5 N3 C4 -10.2(14) . . . . ? C6 C7 N3 C5 1.5(9) . . . . ? Pt1 C7 N3 C5 -175.4(6) . . . . ? C6 C7 N3 C4 -171.6(7) . . . . ? Pt1 C7 N3 C4 11.5(11) . . . . ? N2 C4 N3 C5 135.1(8) . . . . ? N2 C4 N3 C7 -52.6(10) . . . . ? N3 C5 N4 C6 1.6(9) . . . . ? C10 C5 N4 C6 -177.1(8) . . . . ? N3 C5 N4 C11 -176.9(8) . . . . ? C10 C5 N4 C11 4.3(13) . . . . ? C7 C6 N4 C5 -0.7(9) . . . . ? C7 C6 N4 C11 177.8(8) . . . . ? C9 C11 N4 C5 -158.9(11) . . . . ? C8A C11 N4 C5 97.6(11) . . . . ? C8 C11 N4 C5 71.9(13) . . . . ? C9A C11 N4 C5 -135.4(11) . . . . ? C9 C11 N4 C6 22.8(15) . . . . ? C8A C11 N4 C6 -80.7(11) . . . . ? C8 C11 N4 C6 -106.4(11) . . . . ? C9A C11 N4 C6 46.2(13) . . . . ? N2 C3 N1 C2 0.5(9) . . . . ? C15 C3 N1 C2 177.9(10) . . . . ? N2 C3 N1 C12 -174.3(8) . . . . ? C15 C3 N1 C12 3.0(14) . . . . ? C1 C2 N1 C3 0.5(10) . . . . ? C1 C2 N1 C12 175.4(8) . . . . ? C13 C12 N1 C3 85.3(13) . . . . ? C14 C12 N1 C3 -141.4(17) . . . . ? C13A C12 N1 C3 107.3(12) . . . . ? C14A C12 N1 C3 -134.8(16) . . . . ? C13 C12 N1 C2 -88.7(13) . . . . ? C14 C12 N1 C2 45(2) . . . . ? C13A C12 N1 C2 -66.7(13) . . . . ? C14A C12 N1 C2 51.2(17) . . . . ? C2 C1 Pt1 C7 148.7(10) . . . . ? N2 C1 Pt1 C7 -23.8(8) . . . . ? C2 C1 Pt1 Cl1 -29.1(9) . . . . ? N2 C1 Pt1 Cl1 158.3(7) . . . . ? N3 C7 Pt1 C1 23.4(7) . . . . ? C6 C7 Pt1 C1 -152.4(9) . . . . ? N3 C7 Pt1 Cl2 -158.1(7) . . . . ? C6 C7 Pt1 Cl2 26.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.998 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.120 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.167 0.479 0.000 725 112 '3 (C2 H6 O S)' 2 0.022 0.608 0.500 725 111 '3 (C2 H6 O S)' _platon_squeeze_details ; PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13 PLATON version from 20.02.2011 ; # start Validation Reply Form _vrf_CHEMW03_mhe1026 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: Disordered solvent molecules were present. Therefore, SQEEZE (PLATON) was used. The pot. solvent was included in calculations. ; _vrf_PLAT043_mhe1026 ; PROBLEM: Check Reported Molecular Weight ................ 643.56 RESPONSE: Disordered solvent molecules were present. Therefore, SQEEZE (PLATON) was used. The pot. solvent was included in calculations. ; _vrf_PLAT044_mhe1026 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: Disordered solvent molecules were present. Therefore, SQEEZE (PLATON) was used. The pot. solvent was included in calculations. ; data_compound4 _database_code_depnum_ccdc_archive 'CCDC 904843' #TrackingRef 'alb97pub.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H20 Cl2 N4 Pt, C2 H6 O S' _chemical_formula_sum 'C15 H26 Cl2 N4 O Pt S' _chemical_formula_weight 576.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.2290(8) _cell_length_b 15.8825(12) _cell_length_c 11.5964(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2068.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.75 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 7.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.133 _exptl_absorpt_correction_T_max 0.215 _exptl_absorpt_process_details 'MULscanABS, (PLATON03, Speck, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15652 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 26.03 _reflns_number_total 2096 _reflns_number_gt 1763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The highest residual electron density peak is 1.06 \%A from Pt1 on the mirror plane. ; _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^)+(0.0461P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2096 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 0.29441(2) -0.2500 0.814638(19) 0.01617(11) Uani 1 2 d S . . Cl1 Cl 0.26613(12) -0.14629(8) 0.95812(10) 0.0263(3) Uani 1 1 d . . . N1 N 0.2745(4) -0.0930(3) 0.6636(4) 0.0245(10) Uani 1 1 d . . . N2 N 0.4182(4) -0.1759(3) 0.6180(3) 0.0222(9) Uani 1 1 d . . . C1 C 0.3267(5) -0.1667(3) 0.6935(4) 0.0200(10) Uani 1 1 d . . . C2 C 0.3332(5) -0.0582(4) 0.5709(5) 0.0328(13) Uani 1 1 d . . . H2A H 0.3139 -0.0066 0.5339 0.039 Uiso 1 1 calc R . . C3 C 0.4223(5) -0.1100(4) 0.5423(4) 0.0330(13) Uani 1 1 d . . . H3A H 0.4776 -0.1025 0.4812 0.040 Uiso 1 1 calc R . . C4 C 0.4925(6) -0.2500 0.6163(6) 0.0239(15) Uani 1 2 d S . . H4A H 0.5459 -0.2500 0.6843 0.029 Uiso 1 2 calc SR . . H4B H 0.5425 -0.2500 0.5459 0.029 Uiso 1 2 calc SR . . C5 C 0.1627(5) -0.0592(4) 0.7130(5) 0.0298(12) Uani 1 1 d . . . H5 H 0.1413 -0.0939 0.7819 0.036 Uiso 1 1 calc R . . C6 C 0.1825(7) 0.0304(4) 0.7524(6) 0.0493(18) Uani 1 1 d . . . H6A H 0.1977 0.0663 0.6852 0.074 Uiso 1 1 calc R . . H6B H 0.2511 0.0325 0.8045 0.074 Uiso 1 1 calc R . . H6C H 0.1114 0.0506 0.7929 0.074 Uiso 1 1 calc R . . C7 C 0.0637(6) -0.0665(5) 0.6264(6) 0.0568(19) Uani 1 1 d . . . H7A H 0.0585 -0.1247 0.5991 0.085 Uiso 1 1 calc R . . H7B H 0.0799 -0.0291 0.5610 0.085 Uiso 1 1 calc R . . H7C H -0.0117 -0.0504 0.6626 0.085 Uiso 1 1 calc R . . S1 S 0.0664(3) -0.2931(3) 0.2466(3) 0.0526(9) Uani 0.50 1 d P . . O1 O -0.0115(7) -0.2500 0.1611(6) 0.081(3) Uani 1 2 d S . . C8 C 0.2056(9) -0.2500 0.2442(9) 0.062(3) Uani 1 2 d S . . H8A H 0.1992 -0.1885 0.2422 0.074 Uiso 0.50 1 d PR . . H8B H 0.2493 -0.2672 0.3134 0.074 Uiso 0.50 1 d PR . . H8C H 0.2482 -0.2696 0.1755 0.074 Uiso 0.50 1 d PR . . C9 C 0.0210(12) -0.2500 0.3832(10) 0.104(6) Uani 1 2 d S . . H9A H 0.0193 -0.1884 0.3782 0.125 Uiso 0.50 1 d PR . . H9B H -0.0586 -0.2709 0.4027 0.125 Uiso 0.50 1 d PR . . H9C H 0.0776 -0.2672 0.4430 0.125 Uiso 0.50 1 d PR . . 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 0.01859(16) 0.01568(15) 0.01424(14) 0.000 0.00033(10) 0.000 Cl1 0.0356(7) 0.0241(6) 0.0193(5) -0.0056(5) 0.0015(5) 0.0003(5) N1 0.028(3) 0.020(2) 0.026(2) 0.0063(18) 0.0021(17) 0.0026(19) N2 0.021(2) 0.022(2) 0.024(2) 0.0020(16) 0.0024(16) 0.0009(18) C1 0.021(2) 0.021(3) 0.018(2) -0.0037(19) -0.0013(18) 0.001(2) C2 0.039(3) 0.029(3) 0.030(3) 0.013(2) 0.007(2) 0.004(2) C3 0.038(3) 0.034(3) 0.027(3) 0.011(2) 0.009(2) -0.002(3) C4 0.026(4) 0.025(4) 0.021(3) 0.000 0.005(3) 0.000 C5 0.026(3) 0.033(3) 0.031(3) 0.007(2) 0.005(2) 0.009(3) C6 0.073(5) 0.031(3) 0.044(4) 0.005(3) 0.016(3) 0.013(3) C7 0.036(4) 0.084(6) 0.050(4) 0.005(4) -0.010(3) 0.009(4) S1 0.042(2) 0.052(2) 0.063(2) -0.0042(17) 0.0009(16) -0.0082(17) O1 0.045(5) 0.159(10) 0.038(4) 0.000 -0.001(3) 0.000 C8 0.047(6) 0.093(9) 0.046(6) 0.000 0.005(5) 0.000 C9 0.057(8) 0.21(2) 0.042(6) 0.000 0.013(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 1.963(5) 8 ? Pt1 C1 1.963(5) . ? Pt1 Cl1 2.3628(12) . ? Pt1 Cl1 2.3628(12) 8 ? N1 C1 1.354(7) . ? N1 C2 1.377(7) . ? N1 C5 1.481(7) . ? N2 C1 1.358(6) . ? N2 C3 1.367(6) . ? N2 C4 1.443(6) . ? C2 C3 1.337(8) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 N2 1.443(6) 8 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C7 1.503(9) . ? C5 C6 1.511(9) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? S1 S1 1.370(8) 8 ? S1 O1 1.489(7) . ? S1 C8 1.707(10) . ? S1 C9 1.799(11) . ? O1 S1 1.489(7) 8 ? C8 S1 1.707(10) 8 ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 S1 1.799(11) 8 ? C9 H9A 0.9799 . ? C9 H9B 0.9800 . ? C9 H9C 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 C1 Pt1 C1 84.7(3) 8 . ? C1 Pt1 Cl1 176.76(15) 8 . ? C1 Pt1 Cl1 93.37(14) . . ? C1 Pt1 Cl1 93.37(14) 8 8 ? C1 Pt1 Cl1 176.76(15) . 8 ? Cl1 Pt1 Cl1 88.40(6) . 8 ? C1 N1 C2 109.9(4) . . ? C1 N1 C5 125.6(4) . . ? C2 N1 C5 124.2(5) . . ? C1 N2 C3 110.9(4) . . ? C1 N2 C4 122.3(4) . . ? C3 N2 C4 126.6(4) . . ? N1 C1 N2 104.8(4) . . ? N1 C1 Pt1 133.3(4) . . ? N2 C1 Pt1 121.9(4) . . ? C3 C2 N1 107.8(5) . . ? C3 C2 H2A 126.1 . . ? N1 C2 H2A 126.1 . . ? C2 C3 N2 106.6(5) . . ? C2 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? N2 C4 N2 109.3(6) . 8 ? N2 C4 H4A 109.8 . . ? N2 C4 H4A 109.8 8 . ? N2 C4 H4B 109.8 . . ? N2 C4 H4B 109.8 8 . ? H4A C4 H4B 108.3 . . ? N1 C5 C7 109.9(5) . . ? N1 C5 C6 109.5(5) . . ? C7 C5 C6 112.5(6) . . ? N1 C5 H5 108.3 . . ? C7 C5 H5 108.3 . . ? C6 C5 H5 108.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 S1 C8 110.0(4) . . ? O1 S1 C9 104.1(5) . . ? C8 S1 C9 97.0(5) . . ? S1 C8 H8A 109.5 . . ? S1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? S1 C9 H9A 109.5 . . ? S1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 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 C2 N1 C1 N2 0.3(6) . . . . ? C5 N1 C1 N2 173.5(5) . . . . ? C2 N1 C1 Pt1 179.6(4) . . . . ? C5 N1 C1 Pt1 -7.2(8) . . . . ? C3 N2 C1 N1 -0.6(6) . . . . ? C4 N2 C1 N1 -176.1(5) . . . . ? C3 N2 C1 Pt1 180.0(4) . . . . ? C4 N2 C1 Pt1 4.5(7) . . . . ? C1 Pt1 C1 N1 138.4(4) 8 . . . ? Cl1 Pt1 C1 N1 -44.2(5) . . . . ? C1 Pt1 C1 N2 -42.3(5) 8 . . . ? Cl1 Pt1 C1 N2 135.0(4) . . . . ? C1 N1 C2 C3 0.1(7) . . . . ? C5 N1 C2 C3 -173.2(5) . . . . ? N1 C2 C3 N2 -0.4(7) . . . . ? C1 N2 C3 C2 0.6(6) . . . . ? C4 N2 C3 C2 175.9(5) . . . . ? C1 N2 C4 N2 47.9(7) . . . 8 ? C3 N2 C4 N2 -127.0(5) . . . 8 ? C1 N1 C5 C7 -107.2(6) . . . . ? C2 N1 C5 C7 65.0(8) . . . . ? C1 N1 C5 C6 128.7(6) . . . . ? C2 N1 C5 C6 -59.1(7) . . . . ? C8 S1 O1 S1 -48.0(4) . . . 8 ? C9 S1 O1 S1 55.0(4) . . . 8 ? O1 S1 C8 S1 46.0(4) . . . 8 ? C9 S1 C8 S1 -61.8(4) . . . 8 ? O1 S1 C9 S1 -51.9(4) . . . 8 ? C8 S1 C9 S1 60.8(4) . . . 8 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.261 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.185