# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Jan Reedijk' 'Francisco R. Fortea-Perez' 'M. Amparo Gamiz-Gonzalez' 'Bojan Kozlevear' 'Martin Lutz' 'Patricia Marques-Gallego' 'Andrej Pevek' 'A Spek' _publ_contact_author_name 'Jan Reedijk' _publ_contact_author_email REEDIJK@CHEM.LEIDENUNIV.NL _publ_section_title ; Quinoxaline-2-carboxamide as a carrier ligand in two new platinum(II) compounds: Synthesis, crystal structure, cytotoxic activity and DNA interaction ; # Attachment 'marques_deposit_2files.cif' data_k1331 _database_code_depnum_ccdc_archive 'CCDC 762648' #TrackingRef 'marques_deposit_2files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H10 Cl2 N4 O Pt' _chemical_formula_sum 'C11 H10 Cl2 N4 O Pt' _chemical_formula_weight 480.22 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' 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 8.2756(2) _cell_length_b 8.8185(2) _cell_length_c 19.8387(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.4107(8) _cell_angle_gamma 90.00 _cell_volume 1428.31(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3382 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 10.194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1127 _exptl_absorpt_correction_T_max 0.3508 _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; 357 frames in 3 sets of \w and \f scans. Rotation/frame = 1.100 \%. Crystal-detector distance = 33.0 mm. Measuring time = 35 s/\%. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Nonius KappaCCD area-detector diffractometer ; _diffrn_measurement_method '\w scans and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6124 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3255 _reflns_number_gt 2639 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'WinGX (Farrugia, 1999)' _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^ > 2\s(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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3255 _refine_ls_number_parameters 180 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.0001 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 0.38013(2) 0.34987(2) 0.280203(11) 0.03536(12) Uani 1 1 d . . . Cl1 Cl 0.15888(19) 0.33920(19) 0.33466(9) 0.0562(4) Uani 1 1 d . . . Cl2 Cl 0.23115(15) 0.25860(17) 0.18084(7) 0.0513(4) Uani 1 1 d . . . N1 N 0.7081(5) 0.5583(4) 0.4824(2) 0.0356(9) Uani 1 1 d . . . N2 N 0.5162(4) 0.4293(4) 0.3675(2) 0.0332(9) Uani 1 1 d . . . N3 N 0.6435(6) 0.8411(5) 0.5227(3) 0.0425(12) Uani 1 1 d D . . H3N1 H 0.622(7) 0.927(4) 0.539(3) 0.051 Uiso 1 1 d D . . H3N2 H 0.711(6) 0.782(6) 0.548(3) 0.051 Uiso 1 1 d D . . O1 O 0.4339(5) 0.8598(4) 0.4337(2) 0.0437(10) Uani 1 1 d . . . C1 C 0.5844(7) 0.6297(5) 0.4473(3) 0.0334(12) Uani 1 1 d . . . C2 C 0.4855(6) 0.5662(5) 0.3898(3) 0.0343(11) Uani 1 1 d . . . H2 H 0.3972 0.6211 0.3670 0.041 Uiso 1 1 calc R . . C3 C 0.6469(6) 0.3502(5) 0.4027(3) 0.0347(12) Uani 1 1 d . . . C4 C 0.6878(6) 0.2024(6) 0.3828(3) 0.0440(13) Uani 1 1 d . . . H4 H 0.6276 0.1572 0.3444 0.053 Uiso 1 1 calc R . . C5 C 0.8158(8) 0.1268(6) 0.4203(4) 0.0516(16) Uani 1 1 d . . . H5 H 0.8399 0.0285 0.4081 0.062 Uiso 1 1 calc R . . C6 C 0.9113(7) 0.1956(6) 0.4768(4) 0.0531(16) Uani 1 1 d . . . H6 H 1.0020 0.1444 0.4999 0.064 Uiso 1 1 calc R . . C7 C 0.8744(7) 0.3355(6) 0.4988(4) 0.0450(14) Uani 1 1 d . . . H7 H 0.9355 0.3775 0.5378 0.054 Uiso 1 1 calc R . . C8 C 0.7407(6) 0.4166(5) 0.4609(3) 0.0347(11) Uani 1 1 d . . . C9 C 0.5475(6) 0.7889(5) 0.4677(3) 0.0314(10) Uani 1 1 d . . . N4 N 0.5769(6) 0.3737(6) 0.2353(3) 0.0453(12) Uani 1 1 d . . . C10 C 0.6920(7) 0.3979(8) 0.2156(3) 0.0478(14) Uani 1 1 d . . . C11 C 0.8453(7) 0.4217(10) 0.1897(4) 0.0664(19) Uani 1 1 d . . . H11A H 0.9281 0.3559 0.2134 0.100 Uiso 1 1 calc R . . H11B H 0.8793 0.5253 0.1971 0.100 Uiso 1 1 calc R . . H11C H 0.8294 0.3996 0.1417 0.100 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 0.03664(16) 0.03708(15) 0.03152(16) -0.00272(8) 0.00305(9) 0.00507(8) Cl1 0.0378(7) 0.0928(12) 0.0374(9) 0.0024(8) 0.0045(6) 0.0054(7) Cl2 0.0460(7) 0.0676(9) 0.0379(8) -0.0129(7) -0.0006(6) 0.0049(7) N1 0.035(2) 0.036(2) 0.036(3) 0.004(2) 0.0046(18) -0.0002(18) N2 0.034(2) 0.0292(19) 0.036(3) 0.0027(18) 0.0049(17) 0.0031(17) N3 0.052(3) 0.036(2) 0.036(3) -0.003(2) -0.003(2) 0.007(2) O1 0.049(2) 0.040(2) 0.038(2) -0.0051(16) -0.0040(18) 0.0153(16) C1 0.037(3) 0.030(2) 0.035(3) 0.004(2) 0.011(2) 0.003(2) C2 0.038(2) 0.033(2) 0.032(3) -0.002(2) 0.004(2) 0.006(2) C3 0.035(3) 0.034(3) 0.035(3) 0.000(2) 0.005(2) -0.002(2) C4 0.045(3) 0.036(3) 0.050(4) -0.001(3) 0.005(3) 0.010(2) C5 0.054(3) 0.032(3) 0.067(5) 0.000(3) 0.006(3) 0.014(3) C6 0.044(3) 0.038(3) 0.072(5) 0.011(3) -0.005(3) 0.011(3) C7 0.039(3) 0.043(3) 0.049(4) 0.011(3) -0.004(3) 0.002(2) C8 0.034(2) 0.034(2) 0.036(3) 0.006(2) 0.005(2) 0.000(2) C9 0.034(2) 0.034(2) 0.027(3) 0.001(2) 0.007(2) 0.005(2) N4 0.042(3) 0.060(3) 0.032(3) -0.012(2) 0.001(2) 0.000(2) C10 0.039(3) 0.066(4) 0.036(4) -0.001(3) -0.002(3) -0.003(3) C11 0.036(3) 0.109(6) 0.053(4) 0.016(4) 0.003(3) 0.001(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N4 1.991(6) . ? Pt1 N2 2.029(4) . ? Pt1 Cl1 2.2749(16) . ? Pt1 Cl2 2.2933(14) . ? N1 C1 1.303(6) . ? N1 C8 1.361(6) . ? N2 C2 1.324(6) . ? N2 C3 1.377(6) . ? N3 C9 1.323(7) . ? N3 H3N1 0.86(2) . ? N3 H3N2 0.86(2) . ? O1 C9 1.234(6) . ? C1 C2 1.408(7) . ? C1 C9 1.506(6) . ? C2 H2 0.9300 . ? C3 C8 1.410(7) . ? C3 C4 1.418(7) . ? C4 C5 1.364(8) . ? C4 H4 0.9300 . ? C5 C6 1.400(9) . ? C5 H5 0.9300 . ? C6 C7 1.359(8) . ? C6 H6 0.9300 . ? C7 C8 1.424(7) . ? C7 H7 0.9300 . ? N4 C10 1.108(9) . ? C10 C11 1.459(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? 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 N4 Pt1 N2 87.97(18) . . ? N4 Pt1 Cl1 175.98(15) . . ? N2 Pt1 Cl1 89.24(12) . . ? N4 Pt1 Cl2 90.95(15) . . ? N2 Pt1 Cl2 178.83(11) . . ? Cl1 Pt1 Cl2 91.85(6) . . ? C1 N1 C8 117.0(4) . . ? C2 N2 C3 118.0(4) . . ? C2 N2 Pt1 119.3(3) . . ? C3 N2 Pt1 122.6(3) . . ? C9 N3 H3N1 119(4) . . ? C9 N3 H3N2 121(4) . . ? H3N1 N3 H3N2 118(6) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 C9 118.9(5) . . ? C2 C1 C9 118.2(4) . . ? N2 C2 C1 121.1(4) . . ? N2 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? N2 C3 C8 119.1(4) . . ? N2 C3 C4 121.9(5) . . ? C8 C3 C4 119.0(5) . . ? C5 C4 C3 119.8(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.7(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 121.5(5) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 118.9(6) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? N1 C8 C3 121.8(4) . . ? N1 C8 C7 118.2(5) . . ? C3 C8 C7 120.0(5) . . ? O1 C9 N3 125.1(5) . . ? O1 C9 C1 119.7(5) . . ? N3 C9 C1 115.2(4) . . ? C10 N4 Pt1 172.5(5) . . ? N4 C10 C11 177.1(7) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 N4 Pt1 N2 C2 109.2(4) . . . . ? Cl1 Pt1 N2 C2 -67.9(4) . . . . ? N4 Pt1 N2 C3 -66.7(4) . . . . ? Cl1 Pt1 N2 C3 116.1(4) . . . . ? C8 N1 C1 C2 0.5(7) . . . . ? C8 N1 C1 C9 -177.8(4) . . . . ? C3 N2 C2 C1 0.7(7) . . . . ? Pt1 N2 C2 C1 -175.4(4) . . . . ? N1 C1 C2 N2 -1.4(8) . . . . ? C9 C1 C2 N2 177.0(4) . . . . ? C2 N2 C3 C8 0.7(7) . . . . ? Pt1 N2 C3 C8 176.7(4) . . . . ? C2 N2 C3 C4 179.4(5) . . . . ? Pt1 N2 C3 C4 -4.6(7) . . . . ? N2 C3 C4 C5 -178.3(5) . . . . ? C8 C3 C4 C5 0.3(8) . . . . ? C3 C4 C5 C6 -2.3(9) . . . . ? C4 C5 C6 C7 4.0(10) . . . . ? C5 C6 C7 C8 -3.4(10) . . . . ? C1 N1 C8 C3 1.0(7) . . . . ? C1 N1 C8 C7 -179.5(5) . . . . ? N2 C3 C8 N1 -1.6(7) . . . . ? C4 C3 C8 N1 179.7(5) . . . . ? N2 C3 C8 C7 178.9(5) . . . . ? C4 C3 C8 C7 0.2(8) . . . . ? C6 C7 C8 N1 -178.2(5) . . . . ? C6 C7 C8 C3 1.4(8) . . . . ? N1 C1 C9 O1 177.8(5) . . . . ? C2 C1 C9 O1 -0.6(7) . . . . ? N1 C1 C9 N3 -2.4(7) . . . . ? C2 C1 C9 N3 179.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.254 _refine_diff_density_min -1.434 _refine_diff_density_rms 0.169 #===END data_s3822a _database_code_depnum_ccdc_archive 'CCDC 762649' #TrackingRef 'marques_deposit_2files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H12 Cl N3 O2 Pt S' _chemical_formula_sum 'C11 H12 Cl N3 O2 Pt S' _chemical_formula_weight 480.84 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 10.3211(3) _cell_length_b 18.9564(7) _cell_length_c 7.0183(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.0280(10) _cell_angle_gamma 90.00 _cell_volume 1326.18(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11742 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.49 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 10.939 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.1253 _exptl_absorpt_correction_T_max 0.5954 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20861 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2484 _reflns_number_gt 2116 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'EvalCCD, Sadabs' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0454P)^2^+3.1315P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2484 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.63318(2) 0.149123(12) 0.30502(4) 0.02265(12) Uani 1 1 d . . . Cl1 Cl 0.48969(18) 0.05232(9) 0.2464(3) 0.0383(4) Uani 1 1 d . . . S1 S 0.79924(17) 0.07227(8) 0.3566(3) 0.0259(4) Uani 1 1 d . . . O1 O 0.7896(6) 0.3481(2) 0.3437(8) 0.0371(13) Uani 1 1 d . . . O2 O 0.9336(5) 0.1039(2) 0.4082(7) 0.0337(12) Uani 1 1 d . . . N1 N 0.5014(6) 0.2374(3) 0.2711(7) 0.0235(12) Uani 1 1 d . . . N2 N 0.3763(7) 0.3708(4) 0.2353(10) 0.0451(18) Uani 1 1 d . . . N3 N 0.7617(7) 0.2281(3) 0.3473(9) 0.0283(14) Uani 1 1 d . . . H3N H 0.834(9) 0.219(4) 0.365(12) 0.04(3) Uiso 1 1 d . . . C1 C 0.5710(7) 0.2977(3) 0.2837(10) 0.0265(15) Uani 1 1 d . . . C2 C 0.5054(8) 0.3634(4) 0.2634(12) 0.0359(18) Uani 1 1 d . . . H2 H 0.5584 0.4048 0.2705 0.043 Uiso 1 1 calc R . . C3 C 0.3031(8) 0.3098(4) 0.2295(11) 0.0341(17) Uani 1 1 d . . . C4 C 0.1672(8) 0.3149(5) 0.2103(12) 0.046(2) Uani 1 1 d . . . H4 H 0.1264 0.3601 0.2020 0.055 Uiso 1 1 calc R . . C5 C 0.0910(9) 0.2565(5) 0.2029(11) 0.045(2) Uani 1 1 d . . . H5 H -0.0029 0.2608 0.1877 0.054 Uiso 1 1 calc R . . C6 C 0.1509(8) 0.1895(5) 0.2179(13) 0.046(2) Uani 1 1 d . . . H6 H 0.0968 0.1487 0.2134 0.055 Uiso 1 1 calc R . . C7 C 0.2858(8) 0.1818(4) 0.2387(13) 0.0418(19) Uani 1 1 d . . . H7 H 0.3246 0.1361 0.2485 0.050 Uiso 1 1 calc R . . C8 C 0.3659(7) 0.2413(4) 0.2455(10) 0.0274(15) Uani 1 1 d . . . C9 C 0.7210(7) 0.2938(3) 0.3275(10) 0.0273(15) Uani 1 1 d . . . C10 C 0.7899(7) 0.0125(3) 0.5460(10) 0.0305(16) Uani 1 1 d . . . H10A H 0.8622 -0.0223 0.5629 0.046 Uiso 1 1 calc R . . H10B H 0.7031 -0.0118 0.5104 0.046 Uiso 1 1 calc R . . H10C H 0.7991 0.0383 0.6697 0.046 Uiso 1 1 calc R . . C11 C 0.7873(8) 0.0177(4) 0.1459(11) 0.0335(17) Uani 1 1 d . . . H11A H 0.7893 0.0473 0.0321 0.050 Uiso 1 1 calc R . . H11B H 0.7029 -0.0088 0.1175 0.050 Uiso 1 1 calc R . . H11C H 0.8630 -0.0152 0.1722 0.050 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 0.01255(17) 0.01969(17) 0.03548(18) 0.00036(11) 0.00579(11) -0.00083(10) Cl1 0.0175(9) 0.0274(9) 0.0676(12) -0.0044(9) 0.0069(8) -0.0062(7) S1 0.0126(8) 0.0202(8) 0.0443(10) -0.0009(7) 0.0062(7) -0.0003(6) O1 0.033(3) 0.021(3) 0.056(3) 0.000(2) 0.010(3) -0.004(2) O2 0.014(3) 0.030(3) 0.056(3) -0.005(2) 0.006(2) 0.0003(19) N1 0.022(3) 0.023(3) 0.024(3) 0.001(2) 0.004(2) 0.006(2) N2 0.039(5) 0.035(4) 0.055(4) -0.004(3) 0.000(3) 0.018(3) N3 0.020(4) 0.023(3) 0.041(4) 0.000(2) 0.007(3) 0.001(3) C1 0.028(4) 0.023(3) 0.029(3) 0.001(3) 0.008(3) 0.006(3) C2 0.025(4) 0.031(4) 0.050(5) 0.003(3) 0.006(4) 0.004(3) C3 0.029(4) 0.039(4) 0.036(4) 0.005(3) 0.013(3) 0.011(3) C4 0.029(5) 0.063(6) 0.043(5) 0.004(4) 0.005(4) 0.021(4) C5 0.030(5) 0.069(6) 0.036(4) 0.009(4) 0.008(4) 0.016(4) C6 0.020(4) 0.058(5) 0.060(5) 0.015(4) 0.009(4) -0.001(4) C7 0.024(4) 0.041(4) 0.062(5) 0.014(4) 0.015(4) 0.005(3) C8 0.017(4) 0.034(4) 0.031(3) 0.003(3) 0.005(3) 0.008(3) C9 0.020(4) 0.026(4) 0.036(4) 0.000(3) 0.009(3) -0.002(3) C10 0.025(4) 0.024(3) 0.039(4) 0.006(3) 0.003(3) 0.002(3) C11 0.025(4) 0.029(4) 0.047(4) -0.006(3) 0.012(3) 0.006(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 Pt1 N3 1.971(6) . ? Pt1 N1 2.131(5) . ? Pt1 S1 2.2066(16) . ? Pt1 Cl1 2.3267(17) . ? S1 O2 1.467(5) . ? S1 C10 1.769(7) . ? S1 C11 1.782(7) . ? O1 C9 1.238(8) . ? N1 C1 1.340(9) . ? N1 C8 1.365(8) . ? N2 C2 1.303(10) . ? N2 C3 1.377(11) . ? N3 C9 1.310(9) . ? N3 H3N 0.75(9) . ? C1 C2 1.407(10) . ? C1 C9 1.500(11) . ? C2 H2 0.9500 . ? C3 C4 1.377(11) . ? C3 C8 1.443(10) . ? C4 C5 1.351(12) . ? C4 H4 0.9500 . ? C5 C6 1.405(12) . ? C5 H5 0.9500 . ? C6 C7 1.370(11) . ? C6 H6 0.9500 . ? C7 C8 1.391(10) . ? C7 H7 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 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 N3 Pt1 N1 78.8(3) . . ? N3 Pt1 S1 90.8(2) . . ? N1 Pt1 S1 169.43(16) . . ? N3 Pt1 Cl1 176.68(19) . . ? N1 Pt1 Cl1 103.97(17) . . ? S1 Pt1 Cl1 86.56(6) . . ? O2 S1 C10 108.0(3) . . ? O2 S1 C11 107.4(3) . . ? C10 S1 C11 104.3(3) . . ? O2 S1 Pt1 114.5(2) . . ? C10 S1 Pt1 110.8(2) . . ? C11 S1 Pt1 111.3(3) . . ? C1 N1 C8 118.4(6) . . ? C1 N1 Pt1 110.3(5) . . ? C8 N1 Pt1 131.2(5) . . ? C2 N2 C3 116.4(7) . . ? C9 N3 Pt1 121.4(5) . . ? C9 N3 H3N 121(7) . . ? Pt1 N3 H3N 117(7) . . ? N1 C1 C2 120.8(7) . . ? N1 C1 C9 118.6(6) . . ? C2 C1 C9 120.6(6) . . ? N2 C2 C1 123.9(7) . . ? N2 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? C4 C3 N2 118.7(7) . . ? C4 C3 C8 119.8(8) . . ? N2 C3 C8 121.5(7) . . ? C5 C4 C3 120.9(8) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.8(8) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 121.3(8) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 119.8(8) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N1 C8 C7 122.8(6) . . ? N1 C8 C3 118.9(6) . . ? C7 C8 C3 118.4(6) . . ? O1 C9 N3 128.3(7) . . ? O1 C9 C1 120.9(6) . . ? N3 C9 C1 110.8(6) . . ? S1 C10 H10A 109.5 . . ? S1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 N3 Pt1 S1 O2 2.5(3) . . . . ? N1 Pt1 S1 O2 -4.2(8) . . . . ? Cl1 Pt1 S1 O2 -179.5(2) . . . . ? N3 Pt1 S1 C10 124.9(3) . . . . ? N1 Pt1 S1 C10 118.2(8) . . . . ? Cl1 Pt1 S1 C10 -57.1(3) . . . . ? N3 Pt1 S1 C11 -119.6(3) . . . . ? N1 Pt1 S1 C11 -126.3(8) . . . . ? Cl1 Pt1 S1 C11 58.5(3) . . . . ? N3 Pt1 N1 C1 3.6(4) . . . . ? S1 Pt1 N1 C1 10.4(11) . . . . ? Cl1 Pt1 N1 C1 -174.5(4) . . . . ? N3 Pt1 N1 C8 -174.4(6) . . . . ? S1 Pt1 N1 C8 -167.6(6) . . . . ? Cl1 Pt1 N1 C8 7.5(6) . . . . ? N1 Pt1 N3 C9 -4.1(6) . . . . ? S1 Pt1 N3 C9 177.1(6) . . . . ? C8 N1 C1 C2 -2.5(10) . . . . ? Pt1 N1 C1 C2 179.2(5) . . . . ? C8 N1 C1 C9 175.3(6) . . . . ? Pt1 N1 C1 C9 -3.0(7) . . . . ? C3 N2 C2 C1 1.2(12) . . . . ? N1 C1 C2 N2 1.3(12) . . . . ? C9 C1 C2 N2 -176.4(7) . . . . ? C2 N2 C3 C4 176.7(8) . . . . ? C2 N2 C3 C8 -2.5(11) . . . . ? N2 C3 C4 C5 179.7(7) . . . . ? C8 C3 C4 C5 -1.1(12) . . . . ? C3 C4 C5 C6 0.9(12) . . . . ? C4 C5 C6 C7 -0.4(13) . . . . ? C5 C6 C7 C8 0.0(13) . . . . ? C1 N1 C8 C7 -177.3(7) . . . . ? Pt1 N1 C8 C7 0.5(10) . . . . ? C1 N1 C8 C3 1.2(9) . . . . ? Pt1 N1 C8 C3 179.0(5) . . . . ? C6 C7 C8 N1 178.3(7) . . . . ? C6 C7 C8 C3 -0.2(11) . . . . ? C4 C3 C8 N1 -177.9(6) . . . . ? N2 C3 C8 N1 1.4(10) . . . . ? C4 C3 C8 C7 0.7(11) . . . . ? N2 C3 C8 C7 179.9(7) . . . . ? Pt1 N3 C9 O1 -177.7(6) . . . . ? Pt1 N3 C9 C1 3.5(8) . . . . ? N1 C1 C9 O1 -178.8(6) . . . . ? C2 C1 C9 O1 -1.1(11) . . . . ? N1 C1 C9 N3 0.0(9) . . . . ? C2 C1 C9 N3 177.8(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N O2 0.75(9) 2.39(8) 2.912(8) 128(8) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.178 _refine_diff_density_min -1.466 _refine_diff_density_rms 0.190 #===END