#Electronic Supplementary Information for Dalton Transactions #This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bai, Shi' _publ_contact_author_email andyhor@nus.edu.sg loop_ _publ_author_name J.J.Hu S.Bai H.H.Yeh D.Young Yu.Chi A.Hor data_9242 _database_code_depnum_ccdc_archive 'CCDC 787469' #TrackingRef '- Dalton-CIF-13Oct2010.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H18 Br2 N4 O3 Pt S' _chemical_formula_weight 641.26 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 P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 8.0003(19) _cell_length_b 8.957(2) _cell_length_c 12.129(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.276(5) _cell_angle_gamma 90.00 _cell_volume 849.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2768 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.28 _exptl_crystal_description PLATE _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 2.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 13.104 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0650 _exptl_absorpt_correction_T_max 0.3541 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5774 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0606 _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 -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.42 _reflns_number_total 2055 _reflns_number_gt 1718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1068P)^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_number_reflns 2055 _refine_ls_number_parameters 98 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.015 _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 0.17379(4) 0.2500 0.08820(3) 0.0324(2) Uani 1 2 d S . . Br1 Br 0.39608(16) 0.2500 -0.02255(12) 0.0522(4) Uani 1 2 d S . . Br2 Br -0.05381(14) 0.2500 -0.08391(10) 0.0411(3) Uani 1 2 d S . . S1 S -0.0199(3) 0.2500 0.1937(3) 0.0323(6) Uani 1 2 d S . . C10 C -0.1601(11) 0.0979(11) 0.1587(9) 0.050(2) Uani 1 1 d . . . H10A H -0.0952 0.0045 0.1720 0.075 Uiso 1 1 calc R A . H10B H -0.2175 0.1044 0.0790 0.075 Uiso 1 1 calc R . . H10C H -0.2459 0.1001 0.2056 0.075 Uiso 1 1 calc R . . O3 O 0.0436(12) 0.2500 0.3163(8) 0.057(3) Uani 1 2 d S . . N1 N 0.4380(10) 0.1471(10) 0.2802(7) 0.0279(18) Uiso 0.50 1 d PD A -1 N2 N 0.7990(9) 0.1995(10) 0.5246(6) 0.025(2) Uiso 0.50 1 d PD A -1 N3 N 0.6881(10) 0.4277(10) 0.4385(7) 0.0231(18) Uiso 0.50 1 d PD A -1 N4 N 0.4438(10) 0.3966(10) 0.2727(7) 0.0279(18) Uiso 0.50 1 d PD A -1 O1 O 0.6835(15) -0.0237(11) 0.4560(10) 0.041(2) Uiso 0.50 1 d PD A -1 O2 O 0.9139(11) 0.4193(13) 0.5931(8) 0.036(2) Uiso 0.50 1 d PD A -1 C1 C 0.3643(6) 0.2715(11) 0.2241(6) 0.025(3) Uiso 0.50 1 d PD A -1 C2 C 0.5683(8) 0.1978(13) 0.3670(6) 0.022(2) Uiso 0.50 1 d PD A -1 C3 C 0.6819(12) 0.1165(10) 0.4484(8) 0.0231(18) Uiso 0.50 1 d PD A -1 C4 C 0.8036(11) 0.3540(10) 0.5207(7) 0.025(2) Uiso 0.50 1 d PD A -1 C5 C 0.5695(8) 0.3512(13) 0.3608(6) 0.022(2) Uiso 0.50 1 d PD A -1 C6 C 0.3878(19) -0.0017(13) 0.2527(14) 0.034(2) Uiso 0.50 1 d PD A -1 H6A H 0.2873 -0.0022 0.1903 0.051 Uiso 0.50 1 calc PR A -1 H6B H 0.3594 -0.0507 0.3186 0.051 Uiso 0.50 1 calc PR A -1 H6C H 0.4818 -0.0554 0.2300 0.051 Uiso 0.50 1 calc PR A -1 C7 C 0.9208(14) 0.134(2) 0.6109(9) 0.036(2) Uiso 0.50 1 d PD A -1 H7A H 0.8808 0.0349 0.6283 0.054 Uiso 0.50 1 calc PR A -1 H7B H 0.9377 0.1968 0.6785 0.054 Uiso 0.50 1 calc PR A -1 H7C H 1.0294 0.1237 0.5864 0.054 Uiso 0.50 1 calc PR A -1 C8 C 0.696(2) 0.5848(12) 0.4368(14) 0.041(2) Uiso 0.50 1 d PD A -1 H8A H 0.8023 0.6183 0.4871 0.062 Uiso 0.50 1 calc PR A -1 H8B H 0.5979 0.6266 0.4624 0.062 Uiso 0.50 1 calc PR A -1 H8C H 0.6946 0.6189 0.3598 0.062 Uiso 0.50 1 calc PR A -1 C9 C 0.3987(18) 0.5420(11) 0.2352(13) 0.034(2) Uiso 0.50 1 d PD A -1 H9A H 0.2906 0.5696 0.2555 0.051 Uiso 0.50 1 calc PR A -1 H9B H 0.3852 0.5464 0.1530 0.051 Uiso 0.50 1 calc PR A -1 H9C H 0.4886 0.6115 0.2707 0.051 Uiso 0.50 1 calc PR A -1 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 0.0146(3) 0.0578(4) 0.0246(3) 0.000 0.00340(17) 0.000 Br1 0.0254(6) 0.0949(11) 0.0400(8) 0.000 0.0149(5) 0.000 Br2 0.0269(6) 0.0649(8) 0.0284(6) 0.000 -0.0016(5) 0.000 S1 0.0203(12) 0.0491(16) 0.0290(15) 0.000 0.0086(10) 0.000 C10 0.038(5) 0.052(5) 0.066(7) -0.006(5) 0.023(5) -0.009(4) O3 0.045(5) 0.095(8) 0.032(5) 0.000 0.010(4) 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 2.002(7) 4_565 ? Pt1 C1 2.002(7) . ? Pt1 S1 2.210(3) . ? Pt1 Br1 2.4459(13) . ? Pt1 Br2 2.4611(13) . ? S1 O3 1.466(10) . ? S1 C10 1.758(9) . ? S1 C10 1.758(9) 4_565 ? N1 C1 1.372(9) . ? N1 C2 1.391(9) . ? N1 C6 1.411(9) . ? N2 C3 1.385(9) . ? N2 C4 1.386(9) . ? N2 C7 1.399(9) . ? N3 C5 1.370(8) . ? N3 C4 1.376(8) . ? N3 C8 1.410(9) . ? N4 C1 1.359(8) . ? N4 C5 1.364(8) . ? N4 C9 1.402(8) . ? O1 C3 1.259(9) . ? O2 C4 1.250(9) . ? C2 C5 1.376(18) . ? C2 C3 1.396(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 Pt1 C1 11.1(5) 4_565 . ? C1 Pt1 S1 91.60(15) 4_565 . ? C1 Pt1 S1 91.60(15) . . ? C1 Pt1 Br1 86.40(14) 4_565 . ? C1 Pt1 Br1 86.40(14) . . ? S1 Pt1 Br1 177.99(8) . . ? C1 Pt1 Br2 174.1(3) 4_565 . ? C1 Pt1 Br2 174.1(3) . . ? S1 Pt1 Br2 90.44(8) . . ? Br1 Pt1 Br2 91.57(5) . . ? O3 S1 C10 108.1(4) . . ? O3 S1 C10 108.1(4) . 4_565 ? C10 S1 C10 101.6(7) . 4_565 ? O3 S1 Pt1 116.9(4) . . ? C10 S1 Pt1 110.5(3) . . ? C10 S1 Pt1 110.5(3) 4_565 . ? C1 N1 C2 106.5(7) . . ? C1 N1 C6 125.4(11) . . ? C2 N1 C6 128.1(11) . . ? C3 N2 C4 122.2(8) . . ? C3 N2 C7 122.6(11) . . ? C4 N2 C7 115.2(11) . . ? C5 N3 C4 121.3(8) . . ? C5 N3 C8 121.1(12) . . ? C4 N3 C8 117.6(11) . . ? C1 N4 C5 107.1(7) . . ? C1 N4 C9 124.1(9) . . ? C5 N4 C9 128.9(10) . . ? N4 C1 N1 110.0(7) . . ? N4 C1 Pt1 129.9(7) . . ? N1 C1 Pt1 120.1(7) . . ? C5 C2 N1 107.3(6) . . ? C5 C2 C3 123.3(9) . . ? N1 C2 C3 129.4(10) . . ? O1 C3 N2 119.4(11) . . ? O1 C3 C2 124.6(11) . . ? N2 C3 C2 116.0(8) . . ? O2 C4 N3 123.4(10) . . ? O2 C4 N2 117.6(11) . . ? N3 C4 N2 119.0(10) . . ? N4 C5 N3 132.6(10) . . ? N4 C5 C2 109.1(6) . . ? N3 C5 C2 118.2(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.478 _refine_diff_density_min -2.383 _refine_diff_density_rms 0.323 #===end data_9419 _database_code_depnum_ccdc_archive 'CCDC 787470' #TrackingRef '- Dalton-CIF-13Oct2010.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H23 Cl N6 O2 Pt' _chemical_formula_weight 634.00 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca 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 10.6151(6) _cell_length_b 17.5119(10) _cell_length_c 23.4857(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4365.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6028 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description BLOCK _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 6.584 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.0909 _exptl_absorpt_correction_T_max 0.3527 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29483 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5013 _reflns_number_gt 4461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0322P)^2^+9.5044P] 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 5013 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.710289(12) 0.508674(8) 0.656565(6) 0.01711(6) Uani 1 1 d . . . Cl1 Cl 0.88002(9) 0.46094(5) 0.71213(4) 0.0284(2) Uani 1 1 d . . . O1 O 0.8638(3) 0.24851(17) 0.50264(12) 0.0308(6) Uani 1 1 d . . . O2 O 0.5344(3) 0.10257(16) 0.56647(13) 0.0329(7) Uani 1 1 d . . . N1 N 0.5978(3) 0.35465(17) 0.63421(13) 0.0189(6) Uani 1 1 d . . . N2 N 0.7669(3) 0.37285(17) 0.58326(13) 0.0194(6) Uani 1 1 d . . . N3 N 0.5501(3) 0.22260(18) 0.60295(14) 0.0226(6) Uani 1 1 d . . . N4 N 0.6993(3) 0.17532(19) 0.53585(14) 0.0263(7) Uani 1 1 d . . . N5 N 0.7205(3) 0.61780(18) 0.69019(13) 0.0192(6) Uani 1 1 d . . . C1 C 0.6916(3) 0.4069(2) 0.62240(15) 0.0181(7) Uani 1 1 d . . . C2 C 0.6163(3) 0.28894(19) 0.60319(15) 0.0191(7) Uani 1 1 d . . . C3 C 0.5907(4) 0.1626(2) 0.56835(16) 0.0236(8) Uani 1 1 d . . . C4 C 0.7711(4) 0.2426(2) 0.53388(17) 0.0245(8) Uani 1 1 d . . . C5 C 0.7227(3) 0.2996(2) 0.57120(16) 0.0198(7) Uani 1 1 d . . . C6 C 0.5030(4) 0.3705(2) 0.67816(18) 0.0254(8) Uani 1 1 d . . . H6A H 0.4186 0.3624 0.6624 0.038 Uiso 1 1 calc R . . H6B H 0.5111 0.4236 0.6909 0.038 Uiso 1 1 calc R . . H6C H 0.5160 0.3361 0.7106 0.038 Uiso 1 1 calc R . . C7 C 0.8820(3) 0.4066(2) 0.55989(17) 0.0250(8) Uani 1 1 d . . . H7A H 0.8896 0.4596 0.5729 0.038 Uiso 1 1 calc R . . H7B H 0.8783 0.4056 0.5182 0.038 Uiso 1 1 calc R . . H7C H 0.9552 0.3773 0.5729 0.038 Uiso 1 1 calc R . . C8 C 0.4309(4) 0.2119(2) 0.63320(19) 0.0303(9) Uani 1 1 d . . . H8A H 0.4463 0.2126 0.6743 0.045 Uiso 1 1 calc R . . H8B H 0.3940 0.1627 0.6224 0.045 Uiso 1 1 calc R . . H8C H 0.3727 0.2532 0.6231 0.045 Uiso 1 1 calc R . . C9 C 0.7397(5) 0.1118(2) 0.50060(18) 0.0346(10) Uani 1 1 d . . . H9A H 0.7699 0.0702 0.5250 0.052 Uiso 1 1 calc R . . H9B H 0.8078 0.1285 0.4754 0.052 Uiso 1 1 calc R . . H9C H 0.6685 0.0937 0.4777 0.052 Uiso 1 1 calc R . . C10 C 0.5665(3) 0.5550(2) 0.61544(14) 0.0175(7) Uani 1 1 d . . . C11 C 0.4846(4) 0.5218(2) 0.57628(16) 0.0228(8) Uani 1 1 d . . . H11 H 0.4970 0.4699 0.5657 0.027 Uiso 1 1 calc R . . C12 C 0.3852(4) 0.5623(2) 0.55216(17) 0.0255(8) Uani 1 1 d . . . H12 H 0.3313 0.5380 0.5255 0.031 Uiso 1 1 calc R . . C13 C 0.3642(4) 0.6377(2) 0.56676(16) 0.0260(8) Uani 1 1 d . . . H13 H 0.2960 0.6648 0.5502 0.031 Uiso 1 1 calc R . . C14 C 0.4424(3) 0.6735(2) 0.60532(16) 0.0223(7) Uani 1 1 d . . . H14 H 0.4284 0.7253 0.6155 0.027 Uiso 1 1 calc R . . C15 C 0.5431(3) 0.6325(2) 0.62946(15) 0.0193(7) Uani 1 1 d . . . C16 C 0.6310(3) 0.6670(2) 0.67036(15) 0.0191(7) Uani 1 1 d . . . C17 C 0.6297(3) 0.7428(2) 0.68893(16) 0.0206(7) Uani 1 1 d . . . H17 H 0.5686 0.7774 0.6745 0.025 Uiso 1 1 calc R . . C18 C 0.7169(4) 0.7672(2) 0.72814(17) 0.0244(8) Uani 1 1 d . . . H18 H 0.7161 0.8185 0.7411 0.029 Uiso 1 1 calc R . . C19 C 0.8064(4) 0.7162(2) 0.74860(17) 0.0251(8) Uani 1 1 d . . . H19 H 0.8670 0.7322 0.7759 0.030 Uiso 1 1 calc R . . C20 C 0.8058(3) 0.6421(2) 0.72878(17) 0.0231(8) Uani 1 1 d . . . H20 H 0.8671 0.6072 0.7426 0.028 Uiso 1 1 calc R . . N1SA N 0.1658(4) 0.3584(2) 0.65214(17) 0.0358(9) Uani 1 1 d . . . C2SA C 0.1737(5) 0.5044(2) 0.6671(2) 0.0375(11) Uani 1 1 d . . . H2SA H 0.1150 0.5293 0.6409 0.056 Uiso 1 1 calc R . . H2SB H 0.2595 0.5225 0.6596 0.056 Uiso 1 1 calc R . . H2SC H 0.1504 0.5167 0.7064 0.056 Uiso 1 1 calc R . . C1SA C 0.1685(4) 0.4224(3) 0.65893(17) 0.0279(9) 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 Pt1 0.01577(9) 0.01664(8) 0.01892(9) -0.00061(5) -0.00093(5) 0.00153(4) Cl1 0.0251(5) 0.0274(5) 0.0326(5) 0.0028(4) -0.0082(4) 0.0044(4) O1 0.0357(16) 0.0336(15) 0.0232(14) 0.0001(11) 0.0069(13) 0.0102(13) O2 0.0440(17) 0.0206(14) 0.0341(16) -0.0036(12) -0.0090(14) 0.0003(13) N1 0.0184(15) 0.0172(14) 0.0209(15) -0.0014(12) 0.0020(12) 0.0035(11) N2 0.0204(15) 0.0206(15) 0.0174(15) 0.0000(12) 0.0015(12) 0.0040(12) N3 0.0233(16) 0.0197(15) 0.0248(16) -0.0028(12) -0.0027(14) 0.0011(12) N4 0.0353(19) 0.0220(16) 0.0217(17) -0.0045(13) -0.0036(14) 0.0107(13) N5 0.0204(15) 0.0212(15) 0.0161(15) 0.0000(12) 0.0011(12) -0.0033(12) C1 0.0190(17) 0.0177(16) 0.0175(17) 0.0015(13) -0.0001(14) 0.0035(13) C2 0.0232(18) 0.0181(16) 0.0160(16) -0.0008(13) -0.0035(15) 0.0042(14) C3 0.029(2) 0.0193(18) 0.0221(19) -0.0021(14) -0.0096(16) 0.0060(15) C4 0.030(2) 0.0249(19) 0.0186(18) 0.0003(14) -0.0044(16) 0.0110(16) C5 0.0215(18) 0.0207(17) 0.0172(17) 0.0005(13) -0.0029(14) 0.0045(14) C6 0.0219(19) 0.0240(19) 0.030(2) -0.0019(16) 0.0089(16) 0.0003(15) C7 0.0198(18) 0.031(2) 0.025(2) 0.0012(15) 0.0055(16) 0.0016(15) C8 0.028(2) 0.026(2) 0.037(2) -0.0039(17) 0.0035(18) -0.0067(16) C9 0.050(3) 0.026(2) 0.027(2) -0.0108(17) -0.002(2) 0.0110(19) C10 0.0146(16) 0.0244(18) 0.0135(16) 0.0020(13) -0.0009(13) -0.0020(13) C11 0.0239(19) 0.0208(17) 0.0236(19) -0.0015(14) -0.0012(15) 0.0006(14) C12 0.0221(19) 0.032(2) 0.0221(19) -0.0016(15) -0.0059(16) 0.0002(16) C13 0.0252(19) 0.032(2) 0.0209(19) 0.0048(15) -0.0035(16) 0.0065(16) C14 0.0218(19) 0.0225(18) 0.0225(18) 0.0018(14) 0.0016(15) 0.0048(14) C15 0.0180(17) 0.0229(18) 0.0170(17) 0.0024(13) 0.0024(14) 0.0006(14) C16 0.0195(17) 0.0220(17) 0.0158(17) 0.0021(13) 0.0038(14) -0.0010(14) C17 0.0236(18) 0.0195(17) 0.0188(18) 0.0015(13) 0.0055(15) 0.0001(14) C18 0.029(2) 0.0223(18) 0.0215(19) -0.0038(15) 0.0054(16) -0.0037(15) C19 0.0255(19) 0.029(2) 0.0209(19) -0.0044(16) -0.0015(16) -0.0061(15) C20 0.0218(18) 0.0242(18) 0.0232(19) 0.0020(15) -0.0030(15) -0.0004(14) N1SA 0.033(2) 0.032(2) 0.041(2) -0.0005(16) -0.0074(17) 0.0028(16) C2SA 0.038(3) 0.029(2) 0.046(3) 0.0024(19) 0.000(2) -0.0049(18) C1SA 0.0208(19) 0.033(2) 0.030(2) 0.0053(17) -0.0055(16) 0.0006(16) _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 1.964(4) . ? Pt1 C10 1.980(3) . ? Pt1 N5 2.071(3) . ? Pt1 Cl1 2.3766(9) . ? O1 C4 1.232(5) . ? O2 C3 1.210(5) . ? N1 C2 1.376(4) . ? N1 C1 1.381(5) . ? N1 C6 1.468(5) . ? N2 C1 1.356(5) . ? N2 C5 1.394(5) . ? N2 C7 1.464(5) . ? N3 C2 1.358(5) . ? N3 C3 1.397(5) . ? N3 C8 1.463(5) . ? N4 C3 1.400(5) . ? N4 C4 1.404(5) . ? N4 C9 1.452(5) . ? N5 C20 1.350(5) . ? N5 C16 1.365(5) . ? C2 C5 1.370(5) . ? C4 C5 1.424(5) . ? C10 C11 1.393(5) . ? C10 C15 1.418(5) . ? C11 C12 1.393(5) . ? C12 C13 1.382(6) . ? C13 C14 1.379(5) . ? C14 C15 1.407(5) . ? C15 C16 1.469(5) . ? C16 C17 1.396(5) . ? C17 C18 1.374(5) . ? C18 C19 1.388(6) . ? C19 C20 1.379(5) . ? N1SA C1SA 1.132(6) . ? C2SA C1SA 1.450(6) . ? 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 C10 95.43(14) . . ? C1 Pt1 N5 176.69(13) . . ? C10 Pt1 N5 81.27(13) . . ? C1 Pt1 Cl1 88.95(10) . . ? C10 Pt1 Cl1 175.11(11) . . ? N5 Pt1 Cl1 94.33(9) . . ? C2 N1 C1 110.2(3) . . ? C2 N1 C6 128.9(3) . . ? C1 N1 C6 120.7(3) . . ? C1 N2 C5 110.2(3) . . ? C1 N2 C7 124.6(3) . . ? C5 N2 C7 125.1(3) . . ? C2 N3 C3 119.1(3) . . ? C2 N3 C8 123.7(3) . . ? C3 N3 C8 116.9(3) . . ? C3 N4 C4 126.8(3) . . ? C3 N4 C9 115.6(4) . . ? C4 N4 C9 117.7(4) . . ? C20 N5 C16 119.8(3) . . ? C20 N5 Pt1 125.6(3) . . ? C16 N5 Pt1 114.6(2) . . ? N2 C1 N1 105.6(3) . . ? N2 C1 Pt1 128.1(3) . . ? N1 C1 Pt1 126.3(3) . . ? N3 C2 C5 122.8(3) . . ? N3 C2 N1 130.1(3) . . ? C5 C2 N1 107.1(3) . . ? O2 C3 N3 121.5(4) . . ? O2 C3 N4 121.7(4) . . ? N3 C3 N4 116.8(3) . . ? O1 C4 N4 121.6(4) . . ? O1 C4 C5 126.6(4) . . ? N4 C4 C5 111.9(3) . . ? C2 C5 N2 106.9(3) . . ? C2 C5 C4 122.6(3) . . ? N2 C5 C4 130.4(3) . . ? C11 C10 C15 116.4(3) . . ? C11 C10 Pt1 129.2(3) . . ? C15 C10 Pt1 114.4(3) . . ? C12 C11 C10 121.9(4) . . ? C13 C12 C11 120.5(4) . . ? C14 C13 C12 120.0(4) . . ? C13 C14 C15 119.3(4) . . ? C14 C15 C10 121.8(3) . . ? C14 C15 C16 122.4(3) . . ? C10 C15 C16 115.8(3) . . ? N5 C16 C17 120.0(3) . . ? N5 C16 C15 113.9(3) . . ? C17 C16 C15 126.1(3) . . ? C18 C17 C16 119.9(3) . . ? C17 C18 C19 119.5(4) . . ? C20 C19 C18 119.0(4) . . ? N5 C20 C19 121.8(4) . . ? N1SA C1SA C2SA 179.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.960 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.134