# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Athanasia Dervisi' _publ_contact_author_email DervisiA@cardiff.ac.uk loop_ _publ_author_name 'Paul Marshall' W.Clegg 'Ross W. Harrington' 'Samantha Callear' 'Simon J. Coles' 'Ian A. Fallis' 'Athanasia Dervisi' data_2009src0239 _database_code_depnum_ccdc_archive 'CCDC 893546' #TrackingRef '12832_web_deposit_cif_file_0_BillClegg_1343162816.dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H28 N4 O2 2+,2 I -' _chemical_formula_sum 'C18 H28 I2 N4 O2' _chemical_formula_weight 586.24 _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' I I -0.4742 1.8119 '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 21 21 21' 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' _cell_length_a 8.9301(2) _cell_length_b 10.8793(2) _cell_length_c 23.2605(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2259.83(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12375 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 2.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD diffractometer' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 19225 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5180 _reflns_number_gt 4674 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL97 _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0272P)^2^+1.0155P] 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 -0.01(2) _refine_ls_number_reflns 5180 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 N1 N 0.3799(4) 0.9869(3) 0.21892(15) 0.0175(8) Uani 1 1 d . . . C2 C 0.3074(5) 0.9088(4) 0.18471(17) 0.0192(9) Uani 1 1 d . . . H2 H 0.3386 0.8848 0.1473 0.023 Uiso 1 1 calc R . . N3 N 0.1832(4) 0.8694(3) 0.21138(14) 0.0147(7) Uani 1 1 d . . . C4 C 0.1765(5) 0.9271(4) 0.26436(18) 0.0205(10) Uani 1 1 d . . . H4 H 0.1007 0.9169 0.2926 0.025 Uiso 1 1 calc R . . C5 C 0.2968(5) 1.0000(4) 0.26835(18) 0.0212(9) Uani 1 1 d . . . H5 H 0.3207 1.0518 0.2999 0.025 Uiso 1 1 calc R . . C6 C 0.5241(5) 1.0459(4) 0.2045(2) 0.0282(11) Uani 1 1 d . . . H6 H 0.5414 1.0371 0.1622 0.034 Uiso 1 1 calc R . . C7 C 0.6500(5) 0.9817(5) 0.2359(2) 0.0393(14) Uani 1 1 d . . . H7A H 0.6339 0.9883 0.2775 0.059 Uiso 1 1 calc R . . H7B H 0.7456 1.0203 0.2258 0.059 Uiso 1 1 calc R . . H7C H 0.6521 0.8948 0.2248 0.059 Uiso 1 1 calc R . . C8 C 0.5163(6) 1.1830(4) 0.2189(2) 0.0339(12) Uani 1 1 d . . . H8A H 0.4247 1.2182 0.2025 0.051 Uiso 1 1 calc R . . H8B H 0.6038 1.2250 0.2027 0.051 Uiso 1 1 calc R . . H8C H 0.5155 1.1937 0.2607 0.051 Uiso 1 1 calc R . . C9 C 0.0701(4) 0.7824(3) 0.19014(16) 0.0146(8) Uani 1 1 d . . . H9 H 0.0131 0.7457 0.2229 0.018 Uiso 1 1 calc R . . C10 C 0.1435(4) 0.6810(3) 0.15390(17) 0.0137(8) Uani 1 1 d . . . H10 H 0.2485 0.6640 0.1666 0.016 Uiso 1 1 calc R . . O11 O 0.0362(3) 0.8307(2) 0.09167(12) 0.0200(7) Uani 1 1 d . . . C12 C -0.0365(4) 0.8417(4) 0.14734(18) 0.0180(9) Uani 1 1 d . . . H12A H -0.1342 0.7986 0.1472 0.022 Uiso 1 1 calc R . . H12B H -0.0534 0.9291 0.1571 0.022 Uiso 1 1 calc R . . C13 C -0.0241(4) 0.5578(4) 0.10125(19) 0.0179(9) Uani 1 1 d . . . H13A H -0.1237 0.5976 0.1024 0.022 Uiso 1 1 calc R . . H13B H -0.0371 0.4697 0.0919 0.022 Uiso 1 1 calc R . . O14 O 0.0524(3) 0.5723(2) 0.15527(11) 0.0172(6) Uani 1 1 d . . . C15 C 0.1376(4) 0.7290(3) 0.09201(17) 0.0129(8) Uani 1 1 d . . . H15 H 0.2392 0.7540 0.0782 0.015 Uiso 1 1 calc R . . C16 C 0.0769(4) 0.6203(3) 0.05738(16) 0.0137(8) Uani 1 1 d . . . H16 H 0.0189 0.6487 0.0231 0.016 Uiso 1 1 calc R . . N17 N 0.2035(3) 0.5397(3) 0.04041(13) 0.0136(7) Uani 1 1 d . . . C18 C 0.2618(4) 0.4492(4) 0.07172(17) 0.0148(8) Uani 1 1 d . . . H18 H 0.2272 0.4243 0.1085 0.018 Uiso 1 1 calc R . . N19 N 0.3760(4) 0.3992(3) 0.04352(15) 0.0181(8) Uani 1 1 d . . . C20 C 0.3910(5) 0.4621(4) -0.00854(19) 0.0246(10) Uani 1 1 d . . . H20 H 0.4638 0.4467 -0.0375 0.030 Uiso 1 1 calc R . . C21 C 0.2827(5) 0.5490(4) -0.01013(17) 0.0189(9) Uani 1 1 d . . . H21 H 0.2648 0.6057 -0.0404 0.023 Uiso 1 1 calc R . . C22 C 0.4695(5) 0.2977(4) 0.0658(2) 0.0267(10) Uani 1 1 d . . . H22 H 0.4260 0.2708 0.1033 0.032 Uiso 1 1 calc R . . C23 C 0.4674(8) 0.1901(5) 0.0260(3) 0.0602(19) Uani 1 1 d . . . H23A H 0.3645 0.1603 0.0218 0.090 Uiso 1 1 calc R . . H23B H 0.5303 0.1244 0.0418 0.090 Uiso 1 1 calc R . . H23C H 0.5062 0.2149 -0.0116 0.090 Uiso 1 1 calc R . . C24 C 0.6283(6) 0.3448(6) 0.0773(3) 0.0541(18) Uani 1 1 d . . . H24A H 0.6709 0.3775 0.0416 0.081 Uiso 1 1 calc R . . H24B H 0.6907 0.2770 0.0912 0.081 Uiso 1 1 calc R . . H24C H 0.6249 0.4099 0.1063 0.081 Uiso 1 1 calc R . . I1 I 0.56467(3) 0.71043(2) 0.100494(11) 0.01982(8) Uani 1 1 d . . . I2 I -0.07227(3) 0.69460(2) 0.351234(12) 0.02396(8) 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 N1 0.0189(18) 0.0178(18) 0.0158(18) -0.0051(15) 0.0028(14) -0.0037(15) C2 0.024(2) 0.022(2) 0.012(2) -0.0048(17) 0.0015(18) -0.0023(19) N3 0.0150(17) 0.0142(17) 0.0148(17) -0.0045(14) -0.0021(15) -0.0013(14) C4 0.027(2) 0.025(2) 0.010(2) -0.0074(18) 0.0048(19) 0.001(2) C5 0.028(2) 0.018(2) 0.017(2) -0.0034(18) 0.0038(19) -0.002(2) C6 0.027(2) 0.040(3) 0.018(2) -0.008(2) 0.0058(19) -0.022(2) C7 0.017(2) 0.040(3) 0.061(4) -0.022(3) 0.004(2) -0.007(2) C8 0.043(3) 0.028(3) 0.030(3) 0.007(2) -0.008(2) -0.019(2) C9 0.0122(17) 0.0161(18) 0.0155(18) -0.0013(15) -0.0022(17) 0.000(2) C10 0.0139(18) 0.0126(19) 0.0144(19) -0.0003(16) 0.0018(16) -0.0030(16) O11 0.0246(16) 0.0140(14) 0.0213(15) 0.0008(12) -0.0050(13) 0.0068(12) C12 0.017(2) 0.0174(19) 0.020(2) -0.0053(17) 0.0004(18) 0.0020(16) C13 0.0122(19) 0.017(2) 0.024(2) -0.0023(18) 0.0010(18) -0.0001(16) O14 0.0252(15) 0.0134(13) 0.0131(14) -0.0025(11) 0.0020(14) -0.0070(13) C15 0.0101(17) 0.0105(19) 0.018(2) -0.0003(16) 0.0016(16) -0.0007(15) C16 0.0106(18) 0.0142(18) 0.0164(19) -0.0017(15) -0.0035(18) 0.0041(18) N17 0.0121(16) 0.0181(17) 0.0107(16) -0.0031(14) 0.0013(14) -0.0001(14) C18 0.0120(19) 0.017(2) 0.016(2) 0.0007(16) 0.0019(16) -0.0002(17) N19 0.0184(17) 0.0167(18) 0.0190(19) -0.0023(15) 0.0011(15) 0.0062(15) C20 0.026(2) 0.033(3) 0.015(2) -0.0045(19) 0.0059(18) 0.005(2) C21 0.020(2) 0.025(2) 0.012(2) -0.0001(18) -0.0005(17) 0.0002(19) C22 0.028(2) 0.030(3) 0.022(2) 0.000(2) 0.0001(19) 0.013(2) C23 0.092(5) 0.025(3) 0.064(4) -0.012(3) -0.029(4) 0.029(3) C24 0.029(3) 0.045(4) 0.088(5) 0.013(3) -0.014(3) 0.010(3) I1 0.01221(12) 0.02702(15) 0.02021(14) 0.00251(11) -0.00032(12) -0.00065(13) I2 0.03353(16) 0.01678(13) 0.02158(14) -0.00092(11) 0.00047(14) 0.00039(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.333(5) . ? N1 C5 1.376(5) . ? N1 C6 1.478(5) . ? C2 H2 0.950 . ? C2 N3 1.341(5) . ? N3 C4 1.384(5) . ? N3 C9 1.470(5) . ? C4 H4 0.950 . ? C4 C5 1.338(6) . ? C5 H5 0.950 . ? C6 H6 1.000 . ? C6 C7 1.512(7) . ? C6 C8 1.530(7) . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9 1.000 . ? C9 C10 1.535(5) . ? C9 C12 1.521(5) . ? C10 H10 1.000 . ? C10 O14 1.436(4) . ? C10 C15 1.532(5) . ? O11 C12 1.454(5) . ? O11 C15 1.430(4) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 O14 1.439(5) . ? C13 C16 1.523(5) . ? C15 H15 1.000 . ? C15 C16 1.529(5) . ? C16 H16 1.000 . ? C16 N17 1.484(5) . ? N17 C18 1.331(5) . ? N17 C21 1.376(5) . ? C18 H18 0.950 . ? C18 N19 1.329(5) . ? N19 C20 1.397(6) . ? N19 C22 1.478(5) . ? C20 H20 0.950 . ? C20 C21 1.353(6) . ? C21 H21 0.950 . ? C22 H22 1.000 . ? C22 C23 1.492(7) . ? C22 C24 1.531(7) . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? 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 N1 C5 107.6(3) . . ? C2 N1 C6 124.4(4) . . ? C5 N1 C6 128.0(4) . . ? N1 C2 H2 125.4 . . ? N1 C2 N3 109.3(4) . . ? H2 C2 N3 125.4 . . ? C2 N3 C4 107.6(3) . . ? C2 N3 C9 128.2(3) . . ? C4 N3 C9 124.2(3) . . ? N3 C4 H4 126.4 . . ? N3 C4 C5 107.2(4) . . ? H4 C4 C5 126.4 . . ? N1 C5 C4 108.3(4) . . ? N1 C5 H5 125.9 . . ? C4 C5 H5 125.9 . . ? N1 C6 H6 108.4 . . ? N1 C6 C7 109.7(4) . . ? N1 C6 C8 109.5(4) . . ? H6 C6 C7 108.4 . . ? H6 C6 C8 108.4 . . ? C7 C6 C8 112.3(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9 110.5 . . ? N3 C9 C10 110.7(3) . . ? N3 C9 C12 112.1(3) . . ? H9 C9 C10 110.5 . . ? H9 C9 C12 110.5 . . ? C10 C9 C12 102.3(3) . . ? C9 C10 H10 111.8 . . ? C9 C10 O14 109.7(3) . . ? C9 C10 C15 104.9(3) . . ? H10 C10 O14 111.8 . . ? H10 C10 C15 111.8 . . ? O14 C10 C15 106.4(3) . . ? C12 O11 C15 110.0(3) . . ? C9 C12 O11 105.6(3) . . ? C9 C12 H12A 110.6 . . ? C9 C12 H12B 110.6 . . ? O11 C12 H12A 110.6 . . ? O11 C12 H12B 110.6 . . ? H12A C12 H12B 108.8 . . ? H13A C13 H13B 108.9 . . ? H13A C13 O14 110.8 . . ? H13A C13 C16 110.8 . . ? H13B C13 O14 110.8 . . ? H13B C13 C16 110.8 . . ? O14 C13 C16 104.8(3) . . ? C10 O14 C13 109.9(3) . . ? C10 C15 O11 106.9(3) . . ? C10 C15 H15 111.3 . . ? C10 C15 C16 104.1(3) . . ? O11 C15 H15 111.3 . . ? O11 C15 C16 111.8(3) . . ? H15 C15 C16 111.3 . . ? C13 C16 C15 101.7(3) . . ? C13 C16 H16 111.4 . . ? C13 C16 N17 111.4(3) . . ? C15 C16 H16 111.4 . . ? C15 C16 N17 109.1(3) . . ? H16 C16 N17 111.4 . . ? C16 N17 C18 126.2(3) . . ? C16 N17 C21 125.2(3) . . ? C18 N17 C21 108.7(3) . . ? N17 C18 H18 125.3 . . ? N17 C18 N19 109.5(3) . . ? H18 C18 N19 125.3 . . ? C18 N19 C20 107.5(3) . . ? C18 N19 C22 124.5(4) . . ? C20 N19 C22 128.0(4) . . ? N19 C20 H20 126.3 . . ? N19 C20 C21 107.3(4) . . ? H20 C20 C21 126.3 . . ? N17 C21 C20 107.1(4) . . ? N17 C21 H21 126.5 . . ? C20 C21 H21 126.5 . . ? N19 C22 H22 107.8 . . ? N19 C22 C23 111.2(4) . . ? N19 C22 C24 109.6(4) . . ? H22 C22 C23 107.8 . . ? H22 C22 C24 107.8 . . ? C23 C22 C24 112.4(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.061 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.132 data_ssi1369 _database_code_depnum_ccdc_archive 'CCDC 893547' #TrackingRef '12832_web_deposit_cif_file_0_BillClegg_1343162816.dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Cl4 N4 O4 Pt2 S2,C H2 Cl2' _chemical_formula_sum 'C19 H32 Cl6 N4 O4 Pt2 S2' _chemical_formula_weight 1047.49 _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 0.1002 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1182 0.1501 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7143 8.0079 '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 21 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 15.032(12) _cell_length_b 15.651(13) _cell_length_c 6.587(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1550(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1574 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 22.89 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.001 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 8.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Crystal Logic diffractometer and Rigaku Saturn 724+ detector' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10347 _diffrn_reflns_av_R_equivalents 0.1691 _diffrn_reflns_av_sigmaI/netI 0.1228 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.38 _reflns_number_total 2790 _reflns_number_gt 1873 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0967P)^2^+6.8405P] 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 0.05(4) _refine_ls_number_reflns 2790 _refine_ls_number_parameters 173 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2144 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.32339(6) 0.71444(7) 0.26327(16) 0.0584(4) Uani 1 1 d . . . Cl1 Cl 0.3551(6) 0.8610(5) 0.3071(12) 0.081(2) Uani 1 1 d . . . Cl2 Cl 0.2081(6) 0.7252(6) 0.4927(14) 0.094(3) Uani 1 1 d . . . S S 0.4318(5) 0.7036(5) 0.0393(11) 0.0633(16) Uani 1 1 d . . . C1 C 0.2993(12) 0.5903(14) 0.246(4) 0.047(4) Uani 1 1 d U . . C2 C 0.2495(18) 0.4648(19) 0.132(4) 0.063(5) Uani 1 1 d U . . H2 H 0.2184 0.4244 0.0514 0.075 Uiso 1 1 calc R . . C3 C 0.2947(14) 0.4475(16) 0.291(4) 0.051(5) Uani 1 1 d U . . H3 H 0.3049 0.3931 0.3506 0.061 Uiso 1 1 calc R . . C4 C 0.2079(18) 0.595(2) -0.069(4) 0.069(7) Uani 1 1 d U . . H4A H 0.2207 0.6560 -0.0645 0.104 Uiso 1 1 calc R . . H4B H 0.1437 0.5855 -0.0556 0.104 Uiso 1 1 calc R . . H4C H 0.2285 0.5710 -0.1982 0.104 Uiso 1 1 calc R . . C5 C 0.3878(16) 0.5401(16) 0.514(4) 0.054(4) Uani 1 1 d U . . H5 H 0.3735 0.5925 0.5949 0.065 Uiso 1 1 calc R . . C6 C 0.4828(15) 0.5434(16) 0.433(4) 0.050(5) Uani 1 1 d U . . H6 H 0.4823 0.5660 0.2906 0.060 Uiso 1 1 calc R . . C7 C 0.3969(17) 0.4600(17) 0.655(4) 0.057(5) Uani 1 1 d U . . H7A H 0.4198 0.4767 0.7906 0.068 Uiso 1 1 calc R . . H7B H 0.3385 0.4316 0.6730 0.068 Uiso 1 1 calc R . . C8 C 0.416(2) 0.772(2) -0.173(3) 0.074(8) Uani 1 1 d . . . H8A H 0.4657 0.7654 -0.2684 0.111 Uiso 1 1 calc R . . H8B H 0.4138 0.8318 -0.1269 0.111 Uiso 1 1 calc R . . H8C H 0.3602 0.7578 -0.2416 0.111 Uiso 1 1 calc R . . C9 C 0.536(2) 0.744(2) 0.149(4) 0.080(9) Uani 1 1 d . . . H9A H 0.5840 0.7386 0.0483 0.120 Uiso 1 1 calc R . . H9B H 0.5514 0.7100 0.2694 0.120 Uiso 1 1 calc R . . H9C H 0.5290 0.8037 0.1872 0.120 Uiso 1 1 calc R . . N1 N 0.2533(14) 0.5526(14) 0.096(3) 0.058(5) Uani 1 1 d U . . N2 N 0.3260(15) 0.5276(14) 0.359(3) 0.058(4) Uani 1 1 d U . . O1 O 0.4573(12) 0.4053(11) 0.556(3) 0.063(4) Uani 1 1 d U . . O2 O 0.4476(12) 0.6188(13) -0.053(4) 0.082(6) Uani 1 1 d . . . C10 C 0.0000 0.5000 0.381(4) 0.16(3) Uani 1 2 d SD . . H10A H 0.0186 0.4459 0.4350 0.187 Uiso 0.50 1 d PR . . H10B H -0.0573 0.5147 0.4350 0.187 Uiso 0.50 1 d PR . . Cl3 Cl 0.0000 0.5000 0.120(2) 0.128(7) Uani 1 2 d SD . . Cl4 Cl 0.0745(12) 0.5765(13) 0.454(3) 0.103(6) Uani 0.50 1 d PD . . 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 0.0581(6) 0.0692(6) 0.0479(5) 0.0023(7) 0.0016(6) 0.0091(5) Cl1 0.096(5) 0.064(4) 0.084(6) -0.002(4) -0.006(4) 0.010(4) Cl2 0.086(6) 0.103(6) 0.095(6) 0.017(5) 0.038(4) 0.035(5) S 0.053(4) 0.072(4) 0.065(4) 0.001(4) 0.001(3) -0.005(4) C1 0.042(10) 0.073(8) 0.028(8) -0.014(8) 0.008(8) 0.013(7) C2 0.060(15) 0.077(10) 0.051(13) -0.002(9) -0.004(9) -0.012(11) C3 0.032(10) 0.071(9) 0.051(13) -0.001(8) 0.000(8) -0.013(8) C4 0.054(16) 0.103(18) 0.050(14) 0.017(13) -0.006(10) -0.016(14) C5 0.048(10) 0.058(10) 0.056(12) -0.005(8) -0.008(7) -0.011(8) C6 0.042(9) 0.063(13) 0.046(12) -0.005(10) -0.014(9) 0.003(10) C7 0.052(13) 0.068(13) 0.051(12) -0.008(8) -0.007(8) -0.002(9) C8 0.10(2) 0.09(2) 0.034(12) -0.004(12) 0.001(13) -0.004(18) C9 0.07(2) 0.11(2) 0.061(16) -0.004(15) 0.006(14) 0.002(17) N1 0.049(11) 0.077(10) 0.048(10) 0.005(8) -0.003(7) -0.013(9) N2 0.041(9) 0.067(10) 0.067(10) -0.003(7) -0.008(7) -0.009(9) O1 0.062(11) 0.059(9) 0.068(11) -0.010(8) -0.003(9) 0.001(7) O2 0.045(11) 0.083(14) 0.118(18) -0.009(12) 0.019(11) -0.005(10) C10 0.16(8) 0.09(5) 0.22(10) 0.000 0.000 0.00(5) Cl3 0.115(14) 0.182(19) 0.086(11) 0.000 0.000 0.069(13) Cl4 0.069(11) 0.121(14) 0.118(15) -0.039(12) -0.001(10) 0.006(10) _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 Cl1 2.361(8) . ? Pt Cl2 2.305(8) . ? Pt S 2.205(7) . ? Pt C1 1.98(2) . ? S C8 1.78(3) . ? S C9 1.84(3) . ? S O2 1.48(2) . ? C1 N1 1.34(3) . ? C1 N2 1.29(3) . ? C2 C3 1.28(4) . ? C2 N1 1.40(4) . ? C3 N2 1.41(3) . ? C4 N1 1.44(3) . ? C5 C6 1.53(4) . ? C5 C7 1.57(4) . ? C5 N2 1.40(3) . ? C6 C6 1.45(5) 2_665 ? C6 O1 1.46(3) 2_665 ? C7 O1 1.41(3) . ? O1 C6 1.46(3) 2_665 ? C10 Cl3 1.72(2) . ? C10 Cl4 1.709(16) . ? C10 Cl4 1.709(16) 2_565 ? 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 Cl1 Pt Cl2 90.0(3) . . ? Cl1 Pt S 90.4(3) . . ? Cl1 Pt C1 176.1(8) . . ? Cl2 Pt S 178.9(3) . . ? Cl2 Pt C1 88.4(6) . . ? S Pt C1 91.2(6) . . ? Pt S C8 112.4(11) . . ? Pt S C9 110.0(10) . . ? Pt S O2 117.6(8) . . ? C8 S C9 102.4(14) . . ? C8 S O2 103.9(14) . . ? C9 S O2 109.3(13) . . ? Pt C1 N1 124.6(18) . . ? Pt C1 N2 130.8(18) . . ? N1 C1 N2 104(2) . . ? C3 C2 N1 109(3) . . ? C2 C3 N2 104(2) . . ? C6 C5 C7 99(2) . . ? C6 C5 N2 112(2) . . ? C7 C5 N2 112(2) . . ? C5 C6 C6 108(3) . 2_665 ? C5 C6 O1 113(2) . 2_665 ? C6 C6 O1 107(2) 2_665 2_665 ? C5 C7 O1 106(2) . . ? C1 N1 C2 109(2) . . ? C1 N1 C4 127(2) . . ? C2 N1 C4 124(2) . . ? C1 N2 C3 113(2) . . ? C1 N2 C5 121(2) . . ? C3 N2 C5 125(2) . . ? C6 O1 C7 108.8(18) 2_665 . ? Cl3 C10 Cl4 106.3(12) . . ? Cl3 C10 Cl4 106.3(12) . 2_565 ? Cl4 C10 Cl4 147(2) . 2_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.222 _refine_diff_density_min -1.554 _refine_diff_density_rms 0.290 #===END data_ssi0980 _database_code_depnum_ccdc_archive 'CCDC 893548' #TrackingRef '12832_web_deposit_cif_file_0_BillClegg_1343162816.dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H38 Cl4 N4 O4 Pt2 S2' _chemical_formula_sum 'C22 H38 Cl4 N4 O4 Pt2 S2' _chemical_formula_weight 1018.66 _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 0.1002 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1182 0.1501 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7143 8.0079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 19.248(6) _cell_length_b 19.248(6) _cell_length_c 23.080(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8551(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 967 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 19.82 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 6.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Crystal Logic diffractometer and Rigaku Saturn 724+ detector' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67854 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 24.25 _reflns_number_total 7575 _reflns_number_gt 5716 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0958P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.037(13) _refine_ls_number_reflns 7575 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.07287(3) 0.68883(3) 0.29666(2) 0.06238(16) Uani 1 1 d . . . Pt2 Pt 0.27117(3) 0.33821(3) 0.31349(3) 0.0740(2) Uani 1 1 d . . . Cl1 Cl -0.0614(2) 0.80954(18) 0.29934(17) 0.0771(9) Uani 1 1 d . . . Cl2 Cl -0.15174(19) 0.69204(18) 0.37310(15) 0.0717(9) Uani 1 1 d . . . Cl3 Cl 0.2863(3) 0.2338(3) 0.3638(2) 0.1138(16) Uani 1 1 d . . . Cl4 Cl 0.3753(2) 0.3794(3) 0.3490(2) 0.0975(13) Uani 1 1 d . . . S1 S -0.0053(2) 0.68310(19) 0.22053(16) 0.0705(9) Uani 1 1 d . . . S2 S 0.1709(2) 0.3027(2) 0.27983(18) 0.0791(10) Uani 1 1 d . . . O1 O 0.0067(5) 0.6152(5) 0.1958(4) 0.076(2) Uani 1 1 d . . . O2 O 0.1328(6) 0.3468(6) 0.2411(5) 0.092(3) Uani 1 1 d . . . O3 O 0.0837(5) 0.4619(5) 0.3841(4) 0.071(2) Uani 1 1 d . . . O4 O 0.1422(5) 0.6044(5) 0.3351(4) 0.077(3) Uani 1 1 d . . . N1 N -0.1293(5) 0.5445(5) 0.2736(5) 0.061(3) Uani 1 1 d . . . N2 N -0.0342(5) 0.5425(5) 0.3264(5) 0.055(2) Uani 1 1 d . . . N3 N 0.2856(6) 0.4351(6) 0.2128(5) 0.070(3) Uani 1 1 d . . . N4 N 0.2309(6) 0.4856(6) 0.2869(6) 0.077(3) Uani 1 1 d . . . C1 C 0.0755(14) 0.7247(12) 0.2338(14) 0.23(2) Uani 1 1 d . . . H1A H 0.1009 0.6991 0.2638 0.340 Uiso 1 1 calc R . . H1B H 0.0672 0.7724 0.2469 0.340 Uiso 1 1 calc R . . H1C H 0.1029 0.7254 0.1980 0.340 Uiso 1 1 calc R . . C2 C -0.0460(8) 0.7367(7) 0.1673(6) 0.078(4) Uani 1 1 d . . . H2A H -0.0915 0.7173 0.1574 0.117 Uiso 1 1 calc R . . H2B H -0.0168 0.7385 0.1325 0.117 Uiso 1 1 calc R . . H2C H -0.0519 0.7837 0.1828 0.117 Uiso 1 1 calc R . . C3 C 0.1153(10) 0.2822(11) 0.3410(8) 0.116(6) Uani 1 1 d . . . H3A H 0.1044 0.3249 0.3623 0.174 Uiso 1 1 calc R . . H3B H 0.1392 0.2496 0.3668 0.174 Uiso 1 1 calc R . . H3C H 0.0721 0.2611 0.3270 0.174 Uiso 1 1 calc R . . C4 C 0.1832(9) 0.2211(8) 0.2485(9) 0.105(6) Uani 1 1 d . . . H4A H 0.2158 0.2250 0.2161 0.158 Uiso 1 1 calc R . . H4B H 0.1386 0.2033 0.2344 0.158 Uiso 1 1 calc R . . H4C H 0.2021 0.1891 0.2775 0.158 Uiso 1 1 calc R . . C5 C -0.0797(6) 0.5879(7) 0.2981(5) 0.060(3) Uani 1 1 d . . . C6 C -0.1080(10) 0.4767(7) 0.2814(7) 0.094(6) Uani 1 1 d . . . H6 H -0.1286 0.4374 0.2633 0.113 Uiso 1 1 calc R . . C7 C -0.0550(7) 0.4744(8) 0.3175(6) 0.072(4) Uani 1 1 d . . . H7 H -0.0350 0.4339 0.3342 0.086 Uiso 1 1 calc R . . C8 C 0.0289(6) 0.5670(6) 0.3576(6) 0.065(3) Uani 1 1 d . . . H8 H 0.0231 0.6164 0.3701 0.078 Uiso 1 1 calc R . . C9 C 0.0431(7) 0.5226(6) 0.4070(6) 0.066(3) Uani 1 1 d . . . H9A H -0.0008 0.5067 0.4250 0.079 Uiso 1 1 calc R . . H9B H 0.0705 0.5481 0.4365 0.079 Uiso 1 1 calc R . . C10 C 0.1158(7) 0.4827(6) 0.3321(6) 0.067(3) Uani 1 1 d . . . H10 H 0.1057 0.4506 0.2990 0.080 Uiso 1 1 calc R . . C11 C 0.0897(7) 0.5596(7) 0.3209(6) 0.070(4) Uani 1 1 d . . . H11 H 0.0766 0.5655 0.2793 0.084 Uiso 1 1 calc R . . C12 C 0.1980(7) 0.5643(8) 0.3630(7) 0.080(4) Uani 1 1 d . . . H12A H 0.2437 0.5856 0.3545 0.096 Uiso 1 1 calc R . . H12B H 0.1914 0.5638 0.4056 0.096 Uiso 1 1 calc R . . C13 C 0.1953(7) 0.4961(9) 0.3409(6) 0.076(4) Uani 1 1 d . . . H13 H 0.2139 0.4630 0.3705 0.092 Uiso 1 1 calc R . . C14 C 0.2323(9) 0.5308(7) 0.2423(6) 0.076(4) Uani 1 1 d . . . H14 H 0.2121 0.5758 0.2420 0.092 Uiso 1 1 calc R . . C15 C 0.2664(8) 0.5017(8) 0.1992(7) 0.081(4) Uani 1 1 d . . . H15 H 0.2763 0.5240 0.1634 0.097 Uiso 1 1 calc R . . C16 C 0.2637(8) 0.4199(10) 0.2694(6) 0.088(5) Uani 1 1 d . . . C17 C -0.1824(7) 0.5716(10) 0.2369(6) 0.080(4) Uani 1 1 d . . . H17 H -0.1782 0.6231 0.2328 0.096 Uiso 1 1 calc R . . C18 C -0.1824(9) 0.5398(11) 0.1840(9) 0.133(9) Uani 1 1 d . . . H18A H -0.1400 0.5525 0.1629 0.199 Uiso 1 1 calc R . . H18B H -0.2231 0.5549 0.1618 0.199 Uiso 1 1 calc R . . H18C H -0.1840 0.4893 0.1892 0.199 Uiso 1 1 calc R . . C19 C -0.2539(10) 0.5509(14) 0.2669(9) 0.138(9) Uani 1 1 d . . . H19A H -0.2565 0.5722 0.3054 0.208 Uiso 1 1 calc R . . H19B H -0.2566 0.5002 0.2707 0.208 Uiso 1 1 calc R . . H19C H -0.2927 0.5674 0.2431 0.208 Uiso 1 1 calc R . . C20 C 0.3188(8) 0.3832(8) 0.1806(6) 0.076(4) Uani 1 1 d . . . H20 H 0.3233 0.3399 0.2041 0.092 Uiso 1 1 calc R . . C21 C 0.2828(11) 0.3689(9) 0.1273(7) 0.104(6) Uani 1 1 d . . . H21A H 0.2376 0.3479 0.1359 0.157 Uiso 1 1 calc R . . H21B H 0.3104 0.3367 0.1038 0.157 Uiso 1 1 calc R . . H21C H 0.2759 0.4123 0.1058 0.157 Uiso 1 1 calc R . . C22 C 0.3891(8) 0.4114(9) 0.1657(7) 0.094(6) Uani 1 1 d . . . H22A H 0.4153 0.4199 0.2013 0.140 Uiso 1 1 calc R . . H22B H 0.3838 0.4550 0.1442 0.140 Uiso 1 1 calc R . . H22C H 0.4140 0.3776 0.1416 0.140 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0640(3) 0.0592(3) 0.0639(3) -0.0072(2) -0.0017(2) 0.0035(2) Pt2 0.0721(4) 0.0815(4) 0.0685(4) 0.0082(3) 0.0008(3) 0.0163(3) Cl1 0.090(2) 0.0649(18) 0.076(2) -0.0106(17) -0.0079(19) -0.0002(18) Cl2 0.076(2) 0.0669(19) 0.072(2) -0.0051(17) 0.0133(17) 0.0028(17) Cl3 0.120(4) 0.106(3) 0.116(4) 0.042(3) -0.015(3) 0.020(3) Cl4 0.086(3) 0.118(3) 0.088(3) 0.005(2) -0.021(2) 0.003(2) S1 0.078(2) 0.066(2) 0.068(2) -0.0072(17) 0.0053(17) 0.0027(17) S2 0.082(2) 0.074(2) 0.081(3) -0.0064(19) 0.0068(19) 0.0117(19) O1 0.087(6) 0.074(6) 0.066(6) -0.002(5) 0.006(5) 0.008(5) O2 0.101(8) 0.085(7) 0.092(8) -0.017(6) -0.029(6) 0.016(6) O3 0.061(5) 0.083(6) 0.069(6) 0.001(5) 0.016(5) 0.000(4) O4 0.082(6) 0.058(5) 0.092(7) -0.009(5) -0.034(5) -0.013(5) N1 0.057(6) 0.062(6) 0.066(7) -0.012(5) 0.011(5) -0.008(5) N2 0.055(5) 0.049(5) 0.060(6) -0.002(5) 0.002(5) -0.006(4) N3 0.077(7) 0.069(7) 0.065(8) 0.005(6) -0.011(6) -0.004(6) N4 0.069(7) 0.070(7) 0.091(9) -0.023(7) -0.006(6) 0.030(6) C1 0.22(3) 0.140(18) 0.32(4) -0.16(2) 0.22(3) -0.13(2) C2 0.081(9) 0.067(9) 0.087(11) -0.004(7) -0.014(8) 0.016(7) C3 0.105(14) 0.140(17) 0.102(14) -0.018(12) 0.036(11) -0.005(12) C4 0.101(12) 0.079(10) 0.137(15) -0.044(10) 0.009(12) 0.019(9) C5 0.050(6) 0.085(9) 0.045(7) -0.014(6) 0.001(6) 0.005(6) C6 0.134(15) 0.054(8) 0.095(12) -0.025(8) 0.057(11) -0.044(9) C7 0.062(8) 0.092(10) 0.060(9) -0.011(7) -0.036(7) 0.016(7) C8 0.065(8) 0.051(7) 0.080(9) -0.012(7) -0.015(7) 0.003(6) C9 0.079(9) 0.057(7) 0.062(9) -0.013(6) 0.000(7) -0.017(6) C10 0.073(8) 0.058(7) 0.069(9) -0.008(6) -0.007(7) 0.019(6) C11 0.066(8) 0.082(9) 0.062(8) 0.029(7) -0.015(6) 0.014(7) C12 0.059(8) 0.104(12) 0.077(10) -0.018(9) 0.000(7) -0.023(8) C13 0.064(8) 0.107(12) 0.059(9) -0.001(8) 0.018(7) 0.010(8) C14 0.114(12) 0.048(7) 0.068(9) 0.012(7) 0.028(9) 0.001(7) C15 0.085(10) 0.078(9) 0.081(11) 0.026(8) 0.016(9) 0.006(8) C16 0.074(9) 0.138(15) 0.051(9) -0.027(9) -0.012(7) -0.014(10) C17 0.060(8) 0.127(13) 0.052(8) -0.013(8) -0.012(6) 0.031(8) C18 0.096(13) 0.160(19) 0.142(18) -0.078(15) -0.054(12) 0.069(13) C19 0.098(14) 0.20(3) 0.121(17) 0.041(16) -0.019(12) 0.046(15) C20 0.078(9) 0.079(9) 0.072(9) -0.007(7) -0.003(8) 0.044(8) C21 0.147(17) 0.091(11) 0.075(11) -0.029(9) -0.022(11) -0.004(11) C22 0.094(11) 0.095(11) 0.091(12) 0.021(9) 0.054(9) 0.044(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Cl1 2.335(4) . ? Pt1 Cl2 2.328(4) . ? Pt1 S1 2.189(4) . ? Pt1 C5 1.948(14) . ? Pt2 Cl3 2.338(4) . ? Pt2 Cl4 2.306(4) . ? Pt2 S2 2.190(4) . ? Pt2 C16 1.88(2) . ? S1 O1 1.445(10) . ? S1 C1 1.77(2) . ? S1 C2 1.784(14) . ? S2 O2 1.435(11) . ? S2 C3 1.815(17) . ? S2 C4 1.745(14) . ? O3 C9 1.502(16) . ? O3 C10 1.408(16) . ? O4 C11 1.369(16) . ? O4 C12 1.472(18) . ? N1 C5 1.389(16) . ? N1 C6 1.380(19) . ? N1 C17 1.426(16) . ? N2 C5 1.399(16) . ? N2 C7 1.386(17) . ? N2 C8 1.488(16) . ? N3 C15 1.372(18) . ? N3 C16 1.404(19) . ? N3 C20 1.398(17) . ? N4 C13 1.436(18) . ? N4 C14 1.349(18) . ? N4 C16 1.47(2) . ? C6 C7 1.32(2) . ? C8 C9 1.452(19) . ? C8 C11 1.452(19) . ? C10 C11 1.584(17) . ? C10 C13 1.566(19) . ? C12 C13 1.41(2) . ? C14 C15 1.32(2) . ? C17 C18 1.37(2) . ? C17 C19 1.59(3) . ? C20 C21 1.44(2) . ? C20 C22 1.50(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 Cl1 Pt1 Cl2 90.86(13) . . ? Cl1 Pt1 S1 90.88(14) . . ? Cl1 Pt1 C5 177.1(4) . . ? Cl2 Pt1 S1 175.60(14) . . ? Cl2 Pt1 C5 88.3(4) . . ? S1 Pt1 C5 90.2(4) . . ? Cl3 Pt2 Cl4 90.62(18) . . ? Cl3 Pt2 S2 91.02(18) . . ? Cl3 Pt2 C16 176.0(5) . . ? Cl4 Pt2 S2 178.04(16) . . ? Cl4 Pt2 C16 88.3(5) . . ? S2 Pt2 C16 90.1(5) . . ? Pt1 S1 O1 117.2(4) . . ? Pt1 S1 C1 111.1(7) . . ? Pt1 S1 C2 105.2(5) . . ? O1 S1 C1 109.6(9) . . ? O1 S1 C2 108.7(6) . . ? C1 S1 C2 104.0(14) . . ? Pt2 S2 O2 119.1(5) . . ? Pt2 S2 C3 108.2(7) . . ? Pt2 S2 C4 108.0(6) . . ? O2 S2 C3 108.2(9) . . ? O2 S2 C4 110.1(9) . . ? C3 S2 C4 101.9(10) . . ? C9 O3 C10 107.9(9) . . ? C11 O4 C12 108.2(9) . . ? C5 N1 C6 108.2(12) . . ? C5 N1 C17 121.0(12) . . ? C6 N1 C17 129.5(13) . . ? C5 N2 C7 109.9(10) . . ? C5 N2 C8 122.5(10) . . ? C7 N2 C8 127.4(10) . . ? C15 N3 C16 109.0(13) . . ? C15 N3 C20 132.0(13) . . ? C16 N3 C20 118.9(13) . . ? C13 N4 C14 125.5(12) . . ? C13 N4 C16 124.4(14) . . ? C14 N4 C16 109.6(12) . . ? Pt1 C5 N1 129.7(9) . . ? Pt1 C5 N2 126.1(9) . . ? N1 C5 N2 104.2(11) . . ? N1 C6 C7 110.1(12) . . ? N2 C7 C6 106.6(12) . . ? N2 C8 C9 110.3(11) . . ? N2 C8 C11 110.2(11) . . ? C9 C8 C11 104.3(11) . . ? O3 C9 C8 106.2(10) . . ? O3 C10 C11 105.3(10) . . ? O3 C10 C13 111.4(11) . . ? C11 C10 C13 100.2(11) . . ? O4 C11 C8 113.2(13) . . ? O4 C11 C10 108.4(10) . . ? C8 C11 C10 104.7(11) . . ? O4 C12 C13 107.6(11) . . ? N4 C13 C10 109.2(12) . . ? N4 C13 C12 115.3(14) . . ? C10 C13 C12 103.7(11) . . ? N4 C14 C15 108.2(12) . . ? N3 C15 C14 111.1(13) . . ? Pt2 C16 N3 130.9(13) . . ? Pt2 C16 N4 127.2(11) . . ? N3 C16 N4 101.9(15) . . ? N1 C17 C18 111.5(12) . . ? N1 C17 C19 105.7(12) . . ? C18 C17 C19 106.1(17) . . ? N3 C20 C21 111.9(13) . . ? N3 C20 C22 106.0(13) . . ? C21 C20 C22 107.9(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.016 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.154 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.098 -0.097 0.022 2760.6 1933.3 _platon_squeeze_details ; ; #===END