# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'B Lippert' _publ_contact_author_email BERNHARD.LIPPERT@UNI-DORTMUND.DE _publ_section_title ; Pt(II) Complexes of Unsubstituted Guanine and 7-Methylguanine ; loop_ _publ_author_name 'B Lippert' 'Deepali Gupta' 'Ralf Nowak' # Attachment '2313.CIF' data_2313 _database_code_depnum_ccdc_archive 'CCDC 731729' _audit_creation_method SHELXL-97 _publ_section_title_footnote ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H18 Cl2 N8 O5 Pt' _chemical_formula_sum 'C9 H18 Cl2 N8 O5 Pt' _chemical_formula_weight 584.30 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1800(16) _cell_length_b 19.454(4) _cell_length_c 11.552(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.79(2) _cell_angle_gamma 90.00 _cell_volume 1707.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3913 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needles _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 8.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.424 _exptl_absorpt_process_details 'SADABS, Sheldrick, Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27195 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3913 _reflns_number_gt 2575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0264P)^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 3913 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Pt1 Pt -0.10413(3) -0.373880(13) 0.180253(19) 0.03106(9) Uani 1 1 d . . . N1D N 0.1157(7) -0.3297(4) 0.3077(4) 0.0606(17) Uani 1 1 d . . . H11A H 0.0850 -0.2931 0.3429 0.073 Uiso 1 1 calc R . . H11B H 0.1714 -0.3601 0.3683 0.073 Uiso 1 1 calc R . . C1D C 0.2358(9) -0.3074(4) 0.2433(6) 0.065(2) Uani 1 1 d . . . H1DA H 0.3133 -0.3449 0.2422 0.077 Uiso 1 1 calc R . . H1DB H 0.3076 -0.2690 0.2876 0.077 Uiso 1 1 calc R . . C2D C 0.1260(8) -0.2864(4) 0.1123(6) 0.0490(18) Uani 1 1 d . . . H2DA H 0.0617 -0.2445 0.1123 0.059 Uiso 1 1 calc R . . H2DB H 0.2000 -0.2786 0.0646 0.059 Uiso 1 1 calc R . . N2D N 0.0036(6) -0.3433(3) 0.0586(4) 0.0365(12) Uani 1 1 d . . . H11C H 0.0689 -0.3792 0.0488 0.044 Uiso 1 1 calc R . . C3D C -0.1409(8) -0.3319(4) -0.0641(5) 0.0458(17) Uani 1 1 d . . . H3DA H -0.0938 -0.3282 -0.1295 0.055 Uiso 1 1 calc R . . H3DB H -0.2041 -0.2900 -0.0626 0.055 Uiso 1 1 calc R . . C4D C -0.2609(9) -0.3928(4) -0.0866(5) 0.054(2) Uani 1 1 d . . . H4DA H -0.3663 -0.3850 -0.1599 0.065 Uiso 1 1 calc R . . H4DB H -0.2023 -0.4335 -0.1009 0.065 Uiso 1 1 calc R . . N3D N -0.3091(6) -0.4034(3) 0.0240(4) 0.0412(13) Uani 1 1 d . . . H11D H -0.3340 -0.4480 0.0300 0.049 Uiso 1 1 calc R . . H11E H -0.4053 -0.3784 0.0161 0.049 Uiso 1 1 calc R . . N1 N -0.0208(6) -0.4413(2) 0.6705(4) 0.0314(12) Uani 1 1 d . . . H1A H 0.0224 -0.4488 0.7495 0.038 Uiso 1 1 calc R . . C2 C 0.0847(7) -0.4075(3) 0.6175(6) 0.0351(15) Uani 1 1 d . . . N2 N 0.2426(7) -0.3876(3) 0.6984(5) 0.0582(17) Uani 1 1 d . . . H2A H 0.3138 -0.3659 0.6722 0.070 Uiso 1 1 calc R . . H2B H 0.2727 -0.3965 0.7765 0.070 Uiso 1 1 calc R . . N3 N 0.0353(6) -0.3947(2) 0.4983(4) 0.0351(13) Uani 1 1 d . . . C4 C -0.1282(7) -0.4156(3) 0.4316(5) 0.0284(13) Uani 1 1 d . . . C5 C -0.2418(7) -0.4473(3) 0.4766(5) 0.0323(14) Uani 1 1 d . . . C6 C -0.1923(8) -0.4639(3) 0.6033(5) 0.0349(14) Uani 1 1 d . . . O6 O -0.2743(5) -0.4948(2) 0.6584(4) 0.0477(12) Uani 1 1 d . . . N7 N -0.3977(6) -0.4581(3) 0.3749(4) 0.0382(13) Uani 1 1 d . . . H7A H -0.4920 -0.4769 0.3766 0.046 Uiso 1 1 calc R . . C8 C -0.3740(8) -0.4342(3) 0.2759(5) 0.0392(16) Uani 1 1 d . . . H8A H -0.4592 -0.4355 0.1957 0.047 Uiso 1 1 calc R . . N9 N -0.2134(6) -0.4080(3) 0.3041(4) 0.0335(12) Uani 1 1 d . . . Cl1 Cl -0.4292(2) -0.21330(9) 0.08967(15) 0.0463(4) Uani 1 1 d . . . O11 O -0.4964(7) -0.2661(3) 0.0002(5) 0.0796(17) Uani 1 1 d . . . O12 O -0.2501(6) -0.1994(3) 0.1143(5) 0.0713(15) Uani 1 1 d . . . O13 O -0.4446(8) -0.2351(4) 0.2012(5) 0.100(2) Uani 1 1 d . . . O14 O -0.5335(7) -0.1532(3) 0.0482(5) 0.0783(17) Uani 1 1 d . . . Cl2 Cl 0.2607(2) -0.06617(9) 0.46860(14) 0.0463(4) 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 0.02935(12) 0.03934(14) 0.02539(12) 0.00385(13) 0.01121(8) -0.00191(13) N1D 0.047(3) 0.105(5) 0.031(3) 0.003(3) 0.016(3) -0.028(3) C1D 0.041(4) 0.109(7) 0.040(4) 0.008(4) 0.011(3) -0.027(4) C2D 0.040(4) 0.068(5) 0.041(4) 0.006(4) 0.016(3) -0.019(4) N2D 0.031(3) 0.054(3) 0.029(3) 0.007(2) 0.016(2) -0.003(3) C3D 0.041(4) 0.072(5) 0.026(4) 0.010(3) 0.015(3) 0.001(4) C4D 0.055(4) 0.080(6) 0.023(3) 0.004(3) 0.010(3) -0.009(4) N3D 0.030(3) 0.059(4) 0.031(3) 0.008(3) 0.009(2) -0.003(3) N1 0.034(3) 0.040(3) 0.021(2) 0.005(2) 0.011(2) -0.005(2) C2 0.030(3) 0.039(4) 0.038(4) 0.004(3) 0.014(3) -0.003(3) N2 0.039(3) 0.097(5) 0.033(3) 0.015(3) 0.007(2) -0.023(3) N3 0.035(3) 0.045(4) 0.025(3) 0.006(2) 0.011(2) -0.004(2) C4 0.032(3) 0.030(3) 0.022(3) 0.004(3) 0.009(3) 0.001(3) C5 0.032(3) 0.041(4) 0.028(3) -0.007(3) 0.016(3) -0.010(3) C6 0.037(4) 0.037(4) 0.037(4) 0.002(3) 0.020(3) 0.003(3) O6 0.034(2) 0.080(4) 0.030(2) 0.005(2) 0.0126(19) -0.015(2) N7 0.030(3) 0.056(4) 0.032(3) 0.003(3) 0.015(2) -0.014(2) C8 0.034(4) 0.054(4) 0.028(3) 0.003(3) 0.009(3) -0.006(3) N9 0.033(3) 0.042(3) 0.028(3) 0.004(2) 0.015(2) -0.002(2) Cl1 0.0396(9) 0.0584(12) 0.0430(10) -0.0039(9) 0.0177(7) -0.0022(9) O11 0.082(4) 0.067(4) 0.069(4) -0.019(3) 0.003(3) 0.006(3) O12 0.048(3) 0.074(4) 0.102(4) 0.012(3) 0.039(3) -0.004(3) O13 0.095(5) 0.157(6) 0.054(4) 0.004(4) 0.035(3) -0.038(4) O14 0.064(4) 0.070(4) 0.095(4) -0.016(3) 0.023(3) 0.018(3) Cl2 0.0417(9) 0.0610(11) 0.0367(9) -0.0011(8) 0.0149(7) -0.0006(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 Pt1 N2D 2.006(4) . ? Pt1 N3D 2.037(4) . ? Pt1 N1D 2.043(5) . ? Pt1 N9 2.059(4) . ? N1D C1D 1.500(8) . ? N1D H11A 0.9000 . ? N1D H11B 0.9000 . ? C1D C2D 1.501(8) . ? C1D H1DA 0.9700 . ? C1D H1DB 0.9700 . ? C2D N2D 1.467(7) . ? C2D H2DA 0.9700 . ? C2D H2DB 0.9700 . ? N2D C3D 1.487(7) . ? N2D H11C 0.9100 . ? C3D C4D 1.499(9) . ? C3D H3DA 0.9700 . ? C3D H3DB 0.9700 . ? C4D N3D 1.484(7) . ? C4D H4DA 0.9700 . ? C4D H4DB 0.9700 . ? N3D H11D 0.9000 . ? N3D H11E 0.9000 . ? N1 C2 1.394(7) . ? N1 C6 1.399(7) . ? N1 H1A 0.8600 . ? C2 N3 1.306(7) . ? C2 N2 1.340(7) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C4 1.335(7) . ? C4 C5 1.369(7) . ? C4 N9 1.383(6) . ? C5 N7 1.392(7) . ? C5 C6 1.403(8) . ? C6 O6 1.237(6) . ? N7 C8 1.313(7) . ? N7 H7A 0.8600 . ? C8 N9 1.332(7) . ? C8 H8A 0.9300 . ? Cl1 O13 1.406(5) . ? Cl1 O12 1.411(5) . ? Cl1 O11 1.415(5) . ? Cl1 O14 1.422(5) . ? 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 N2D Pt1 N3D 83.90(18) . . ? N2D Pt1 N1D 83.24(19) . . ? N3D Pt1 N1D 166.29(19) . . ? N2D Pt1 N9 178.4(2) . . ? N3D Pt1 N9 95.63(18) . . ? N1D Pt1 N9 97.35(18) . . ? C1D N1D Pt1 109.1(4) . . ? C1D N1D H11A 109.9 . . ? Pt1 N1D H11A 109.9 . . ? C1D N1D H11B 109.9 . . ? Pt1 N1D H11B 109.9 . . ? H11A N1D H11B 108.3 . . ? N1D C1D C2D 108.8(5) . . ? N1D C1D H1DA 109.9 . . ? C2D C1D H1DA 109.9 . . ? N1D C1D H1DB 109.9 . . ? C2D C1D H1DB 109.9 . . ? H1DA C1D H1DB 108.3 . . ? N2D C2D C1D 106.3(5) . . ? N2D C2D H2DA 110.5 . . ? C1D C2D H2DA 110.5 . . ? N2D C2D H2DB 110.5 . . ? C1D C2D H2DB 110.5 . . ? H2DA C2D H2DB 108.7 . . ? C2D N2D C3D 117.8(5) . . ? C2D N2D Pt1 109.6(4) . . ? C3D N2D Pt1 108.1(3) . . ? C2D N2D H11C 106.9 . . ? C3D N2D H11C 106.9 . . ? Pt1 N2D H11C 106.9 . . ? N2D C3D C4D 106.6(5) . . ? N2D C3D H3DA 110.4 . . ? C4D C3D H3DA 110.4 . . ? N2D C3D H3DB 110.4 . . ? C4D C3D H3DB 110.4 . . ? H3DA C3D H3DB 108.6 . . ? N3D C4D C3D 109.1(5) . . ? N3D C4D H4DA 109.9 . . ? C3D C4D H4DA 109.9 . . ? N3D C4D H4DB 109.9 . . ? C3D C4D H4DB 109.9 . . ? H4DA C4D H4DB 108.3 . . ? C4D N3D Pt1 109.2(4) . . ? C4D N3D H11D 109.8 . . ? Pt1 N3D H11D 109.8 . . ? C4D N3D H11E 109.8 . . ? Pt1 N3D H11E 109.8 . . ? H11D N3D H11E 108.3 . . ? C2 N1 C6 124.2(5) . . ? C2 N1 H1A 117.9 . . ? C6 N1 H1A 117.9 . . ? N3 C2 N2 121.4(5) . . ? N3 C2 N1 123.5(5) . . ? N2 C2 N1 115.1(5) . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C2 N3 C4 113.8(5) . . ? N3 C4 C5 126.4(5) . . ? N3 C4 N9 125.7(5) . . ? C5 C4 N9 107.9(5) . . ? C4 C5 N7 106.6(5) . . ? C4 C5 C6 121.8(5) . . ? N7 C5 C6 131.6(5) . . ? O6 C6 N1 119.4(5) . . ? O6 C6 C5 130.3(6) . . ? N1 C6 C5 110.4(5) . . ? C8 N7 C5 107.3(5) . . ? C8 N7 H7A 126.4 . . ? C5 N7 H7A 126.4 . . ? N7 C8 N9 111.9(5) . . ? N7 C8 H8A 124.0 . . ? N9 C8 H8A 124.0 . . ? C8 N9 C4 106.3(5) . . ? C8 N9 Pt1 126.6(4) . . ? C4 N9 Pt1 126.6(4) . . ? O13 Cl1 O12 108.2(3) . . ? O13 Cl1 O11 107.9(4) . . ? O12 Cl1 O11 112.3(3) . . ? O13 Cl1 O14 108.1(4) . . ? O12 Cl1 O14 111.0(3) . . ? O11 Cl1 O14 109.2(3) . . ? 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 N2D Pt1 N1D C1D -5.7(5) . . . . ? N3D Pt1 N1D C1D -26.1(13) . . . . ? N9 Pt1 N1D C1D 172.8(5) . . . . ? Pt1 N1D C1D C2D 32.5(8) . . . . ? N1D C1D C2D N2D -51.3(8) . . . . ? C1D C2D N2D C3D 170.3(5) . . . . ? C1D C2D N2D Pt1 46.1(6) . . . . ? N3D Pt1 N2D C2D 152.5(4) . . . . ? N1D Pt1 N2D C2D -22.7(4) . . . . ? N3D Pt1 N2D C3D 22.8(4) . . . . ? N1D Pt1 N2D C3D -152.4(5) . . . . ? C2D N2D C3D C4D -171.0(5) . . . . ? Pt1 N2D C3D C4D -46.1(6) . . . . ? N2D C3D C4D N3D 51.6(7) . . . . ? C3D C4D N3D Pt1 -32.3(6) . . . . ? N2D Pt1 N3D C4D 5.2(4) . . . . ? N1D Pt1 N3D C4D 25.6(12) . . . . ? N9 Pt1 N3D C4D -173.2(4) . . . . ? C6 N1 C2 N3 -1.6(9) . . . . ? C6 N1 C2 N2 177.5(5) . . . . ? N2 C2 N3 C4 -177.5(6) . . . . ? N1 C2 N3 C4 1.5(9) . . . . ? C2 N3 C4 C5 0.5(9) . . . . ? C2 N3 C4 N9 179.5(6) . . . . ? N3 C4 C5 N7 178.5(6) . . . . ? N9 C4 C5 N7 -0.6(6) . . . . ? N3 C4 C5 C6 -2.6(10) . . . . ? N9 C4 C5 C6 178.3(5) . . . . ? C2 N1 C6 O6 178.5(5) . . . . ? C2 N1 C6 C5 -0.4(8) . . . . ? C4 C5 C6 O6 -176.5(6) . . . . ? N7 C5 C6 O6 2.2(11) . . . . ? C4 C5 C6 N1 2.2(8) . . . . ? N7 C5 C6 N1 -179.1(6) . . . . ? C4 C5 N7 C8 0.5(7) . . . . ? C6 C5 N7 C8 -178.3(6) . . . . ? C5 N7 C8 N9 -0.2(7) . . . . ? N7 C8 N9 C4 -0.2(7) . . . . ? N7 C8 N9 Pt1 173.1(4) . . . . ? N3 C4 N9 C8 -178.6(6) . . . . ? C5 C4 N9 C8 0.5(7) . . . . ? N3 C4 N9 Pt1 8.1(8) . . . . ? C5 C4 N9 Pt1 -172.8(4) . . . . ? N3D Pt1 N9 C8 -5.0(5) . . . . ? N1D Pt1 N9 C8 170.6(5) . . . . ? N3D Pt1 N9 C4 167.1(5) . . . . ? N1D Pt1 N9 C4 -17.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.439 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.162 # Attachment '2401.CIF' # The compound referred in the manuscript as complex 3. data_2401 _database_code_depnum_ccdc_archive 'CCDC 731730' _audit_creation_method SHELXL-97 _publ_section_title_footnote ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H30 N11 O Pt2, 3(Cl O4)' _chemical_formula_sum 'C13 H30 Cl3 N11 O13 Pt2' _chemical_formula_weight 1045.01 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' 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 7.9300(16) _cell_length_b 14.494(3) _cell_length_c 25.137(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.58(3) _cell_angle_gamma 90.00 _cell_volume 2769.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6272 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needles _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 10.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1998 _exptl_absorpt_correction_T_max 0.351 _exptl_absorpt_process_details 'SADABS, Sheldrick, Bruker, 2000' _exptl_special_details ; The perchlorate anion based on Cl is disordered. Attempts to satisfactorily model this disorder failed. The perchlorate anion was left as an idealised structure. This explains the level 'C' alerts. ; _diffrn_ambient_temperature 153(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37947 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6272 _reflns_number_gt 4661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0001P)^2^+96.0617P] 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 6272 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1029 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.04316(9) 0.47187(5) 0.16419(2) 0.05159(19) Uani 1 1 d . . . Pt2 Pt 0.77880(7) 0.74182(3) -0.01812(2) 0.03637(15) Uani 1 1 d . . . N1 N 0.6272(15) 0.4129(7) -0.0548(4) 0.035(3) Uani 1 1 d . . . H11A H 0.5551 0.3879 -0.0846 0.042 Uiso 1 1 calc R . . C2 C 0.7007(19) 0.3574(9) -0.0104(6) 0.037(3) Uani 1 1 d . . . N2 N 0.6549(17) 0.2703(8) -0.0185(5) 0.047(3) Uani 1 1 d . . . H2A H 0.6937 0.2299 0.0083 0.056 Uiso 1 1 calc R . . H2B H 0.5853 0.2524 -0.0508 0.056 Uiso 1 1 calc R . . N3 N 0.8055(14) 0.3850(7) 0.0381(4) 0.033(2) Uani 1 1 d . . . C4 C 0.8394(17) 0.4754(8) 0.0403(5) 0.031(3) Uani 1 1 d . . . C5 C 0.7723(18) 0.5351(8) -0.0033(5) 0.032(3) Uani 1 1 d . . . C6 C 0.6602(17) 0.5054(8) -0.0554(6) 0.032(3) Uani 1 1 d . . . O6 O 0.5865(12) 0.5479(6) -0.0992(4) 0.038(2) Uani 1 1 d . . . N9 N 0.9437(14) 0.5196(7) 0.0863(4) 0.032(2) Uani 1 1 d . . . C8 C 0.9369(19) 0.6044(9) 0.0696(6) 0.039(3) Uani 1 1 d . . . H8 H 0.9973 0.6527 0.0930 0.046 Uiso 1 1 calc R . . N7 N 0.8388(15) 0.6197(7) 0.0173(4) 0.033(2) Uani 1 1 d . . . N1D N 0.8156(18) 0.4026(9) 0.1593(5) 0.051(3) Uani 1 1 d . . . H1A1 H 0.7213 0.4424 0.1512 0.061 Uiso 1 1 calc R . . H1A2 H 0.7958 0.3578 0.1323 0.061 Uiso 1 1 calc R . . C1D C 0.843(3) 0.3606(16) 0.2151(8) 0.092(7) Uani 1 1 d . . . H1A3 H 0.7344 0.3694 0.2265 0.111 Uiso 1 1 calc R . . H1A4 H 0.8602 0.2933 0.2120 0.111 Uiso 1 1 calc R . . C2D C 0.993(3) 0.3974(15) 0.2595(8) 0.076(6) Uani 1 1 d . . . H2A1 H 0.9499 0.4482 0.2784 0.092 Uiso 1 1 calc R . . H2A2 H 1.0369 0.3480 0.2872 0.092 Uiso 1 1 calc R . . N2D N 1.132(2) 0.4297(14) 0.2430(5) 0.083(5) Uani 1 1 d . . . H22B H 1.1823 0.3739 0.2375 0.100 Uiso 1 1 calc R . . C3D C 1.281(2) 0.4765(17) 0.2718(7) 0.079(6) Uani 1 1 d . . . H3A1 H 1.3557 0.4325 0.2983 0.094 Uiso 1 1 calc R . . H3A2 H 1.2438 0.5247 0.2940 0.094 Uiso 1 1 calc R . . C4D C 1.388(3) 0.519(2) 0.2431(7) 0.114(10) Uani 1 1 d . . . H4A1 H 1.4871 0.4783 0.2428 0.137 Uiso 1 1 calc R . . H4A2 H 1.4365 0.5773 0.2622 0.137 Uiso 1 1 calc R . . N3D N 1.2817(17) 0.5399(11) 0.1849(5) 0.061(4) Uani 1 1 d . . . H3A3 H 1.3443 0.5224 0.1609 0.073 Uiso 1 1 calc R . . H3A4 H 1.2622 0.6024 0.1810 0.073 Uiso 1 1 calc R . . N1DA N 0.8009(16) 0.7080(8) -0.0924(4) 0.041(3) Uani 1 1 d . . . H1B1 H 0.9170 0.6965 -0.0900 0.049 Uiso 1 1 calc R . . H1B2 H 0.7375 0.6552 -0.1048 0.049 Uiso 1 1 calc R . . C1DA C 0.734(2) 0.7846(10) -0.1325(6) 0.049(4) Uani 1 1 d . . . H1B3 H 0.7929 0.7837 -0.1624 0.059 Uiso 1 1 calc R . . H1B4 H 0.6057 0.7788 -0.1495 0.059 Uiso 1 1 calc R . . C2DA C 0.776(2) 0.8708(10) -0.0999(7) 0.054(4) Uani 1 1 d . . . H2B1 H 0.9052 0.8802 -0.0870 0.064 Uiso 1 1 calc R . . H2B2 H 0.7226 0.9243 -0.1231 0.064 Uiso 1 1 calc R . . N2DA N 0.7061(17) 0.8626(8) -0.0527(5) 0.046(3) Uani 1 1 d . . . H22A H 0.5839 0.8643 -0.0655 0.055 Uiso 1 1 calc R . . C3DA C 0.765(2) 0.9309(9) -0.0079(7) 0.053(4) Uani 1 1 d . . . H3B1 H 0.8953 0.9361 0.0034 0.063 Uiso 1 1 calc R . . H3B2 H 0.7143 0.9922 -0.0202 0.063 Uiso 1 1 calc R . . C4DA C 0.704(2) 0.8972(10) 0.0386(7) 0.055(4) Uani 1 1 d . . . H4B1 H 0.7469 0.9384 0.0711 0.066 Uiso 1 1 calc R . . H4B2 H 0.5743 0.8961 0.0279 0.066 Uiso 1 1 calc R . . N3DA N 0.7740(17) 0.8039(8) 0.0526(5) 0.047(3) Uani 1 1 d . . . H3B3 H 0.7034 0.7715 0.0694 0.056 Uiso 1 1 calc R . . H3B4 H 0.8857 0.8066 0.0767 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.7261(6) 0.3490(3) 0.3673(2) 0.0708(14) Uani 1 1 d . . . O11 O 0.5970(17) 0.3718(8) 0.3918(5) 0.069(4) Uani 1 1 d . . . O12 O 0.7645(19) 0.2555(9) 0.3748(6) 0.086(4) Uani 1 1 d . . . O13 O 0.657(2) 0.3680(13) 0.3104(7) 0.124(7) Uani 1 1 d . . . O14 O 0.886(2) 0.3958(13) 0.3923(9) 0.137(8) Uani 1 1 d . . . Cl2 Cl 0.2484(5) 0.1691(3) 0.30940(15) 0.0492(9) Uani 1 1 d . . . O21 O 0.3005(19) 0.2266(9) 0.2735(5) 0.078(4) Uani 1 1 d . . . O22 O 0.302(2) 0.0800(9) 0.3036(7) 0.098(5) Uani 1 1 d . . . O23 O 0.0622(18) 0.1734(10) 0.2989(6) 0.089(4) Uani 1 1 d . . . O24 O 0.3384(17) 0.1923(9) 0.3658(5) 0.073(4) Uani 1 1 d . . . Cl3 Cl 0.7854(6) 0.1380(3) 0.11907(18) 0.0570(10) Uani 1 1 d . . . O31 O 0.709(2) 0.1118(10) 0.0640(6) 0.103(5) Uani 1 1 d . . . O32 O 0.6544(18) 0.1483(11) 0.1437(6) 0.090(4) Uani 1 1 d . . . O33 O 0.9205(18) 0.0756(10) 0.1501(6) 0.088(5) Uani 1 1 d . . . O34 O 0.872(2) 0.2220(9) 0.1199(8) 0.111(6) 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 0.0624(4) 0.0680(4) 0.0277(3) -0.0009(3) 0.0183(3) -0.0135(3) Pt2 0.0473(3) 0.0258(2) 0.0428(3) -0.0028(2) 0.0237(2) -0.0034(2) N1 0.044(7) 0.032(6) 0.032(6) -0.008(5) 0.014(5) -0.010(5) C2 0.048(8) 0.035(7) 0.040(8) 0.006(6) 0.030(7) 0.003(6) N2 0.075(9) 0.032(6) 0.035(6) -0.003(5) 0.019(6) -0.008(6) N3 0.043(7) 0.031(6) 0.034(6) -0.004(5) 0.024(5) -0.004(5) C4 0.037(7) 0.026(6) 0.036(7) 0.000(5) 0.018(6) -0.006(6) C5 0.052(8) 0.019(5) 0.033(7) -0.008(5) 0.025(6) 0.000(6) C6 0.039(7) 0.023(6) 0.043(8) -0.006(5) 0.024(6) -0.005(5) O6 0.051(6) 0.031(5) 0.033(5) 0.000(4) 0.012(4) -0.006(4) N9 0.041(6) 0.028(5) 0.031(6) -0.009(4) 0.016(5) -0.006(5) C8 0.050(9) 0.034(7) 0.038(8) -0.011(6) 0.022(7) -0.007(6) N7 0.047(7) 0.022(5) 0.033(6) -0.001(4) 0.017(5) -0.008(5) N1D 0.069(9) 0.045(7) 0.047(7) -0.007(6) 0.030(7) -0.009(7) C1D 0.15(2) 0.094(16) 0.047(11) 0.014(11) 0.049(13) -0.033(15) C2D 0.079(13) 0.095(15) 0.058(12) 0.034(11) 0.024(10) -0.003(12) N2D 0.098(13) 0.127(15) 0.020(7) 0.008(8) 0.009(8) -0.027(12) C3D 0.063(12) 0.124(19) 0.043(10) 0.011(11) 0.006(9) 0.007(13) C4D 0.081(14) 0.24(3) 0.019(8) 0.008(13) 0.007(9) -0.027(18) N3D 0.064(9) 0.091(11) 0.030(7) -0.004(7) 0.019(6) -0.002(8) N1DA 0.051(7) 0.040(6) 0.038(6) 0.002(5) 0.022(6) -0.002(6) C1DA 0.053(9) 0.051(9) 0.049(9) 0.007(7) 0.022(8) 0.002(7) C2DA 0.076(12) 0.032(7) 0.062(10) 0.010(7) 0.034(9) -0.007(8) N2DA 0.062(8) 0.034(6) 0.051(7) 0.002(5) 0.030(7) 0.011(6) C3DA 0.085(12) 0.023(6) 0.066(11) -0.004(7) 0.047(10) 0.005(7) C4DA 0.078(12) 0.027(7) 0.071(11) -0.002(7) 0.039(10) 0.006(8) N3DA 0.060(8) 0.037(6) 0.054(8) -0.005(6) 0.034(7) -0.004(6) Cl1 0.069(3) 0.078(3) 0.079(3) 0.042(3) 0.044(3) 0.027(3) O11 0.089(9) 0.061(7) 0.075(8) 0.020(6) 0.050(7) 0.026(7) O12 0.108(11) 0.076(9) 0.092(10) 0.035(8) 0.060(9) 0.048(9) O13 0.133(14) 0.167(17) 0.101(12) 0.082(12) 0.081(11) 0.083(13) O14 0.068(11) 0.120(15) 0.22(2) 0.050(15) 0.040(12) -0.002(10) Cl2 0.064(3) 0.047(2) 0.041(2) 0.0053(16) 0.0212(18) 0.0076(19) O21 0.115(11) 0.066(8) 0.065(8) 0.024(7) 0.046(8) 0.018(8) O22 0.141(14) 0.056(8) 0.132(13) 0.016(8) 0.097(11) 0.029(9) O23 0.071(9) 0.089(10) 0.106(11) 0.040(9) 0.021(8) 0.015(8) O24 0.092(10) 0.072(8) 0.065(8) -0.013(7) 0.037(7) -0.003(7) Cl3 0.071(3) 0.045(2) 0.065(3) 0.0075(19) 0.035(2) 0.005(2) O31 0.168(16) 0.070(9) 0.062(9) -0.007(7) 0.017(10) 0.034(10) O32 0.076(9) 0.109(12) 0.097(11) 0.018(9) 0.043(8) 0.022(9) O33 0.084(10) 0.098(11) 0.100(11) 0.038(9) 0.056(8) 0.032(8) O34 0.129(14) 0.048(8) 0.176(17) 0.003(9) 0.076(13) -0.006(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 N2D 1.999(13) . ? Pt1 N9 2.014(10) . ? Pt1 N1D 2.037(12) . ? Pt1 N3D 2.064(14) . ? Pt2 N2DA 1.967(11) . ? Pt2 N7 1.976(10) . ? Pt2 N1DA 1.987(11) . ? Pt2 N3DA 2.004(11) . ? N1 C2 1.365(17) . ? N1 C6 1.367(15) . ? N1 H11A 0.8800 . ? C2 N2 1.314(17) . ? C2 N3 1.326(17) . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? N3 C4 1.336(15) . ? C4 N9 1.373(16) . ? C4 C5 1.378(17) . ? C5 N7 1.376(15) . ? C5 C6 1.423(18) . ? C6 O6 1.252(15) . ? N9 C8 1.294(16) . ? C8 N7 1.343(17) . ? C8 H8 0.9500 . ? N1D C1D 1.49(2) . ? N1D H1A1 0.9200 . ? N1D H1A2 0.9200 . ? C1D C2D 1.48(3) . ? C1D H1A3 0.9900 . ? C1D H1A4 0.9900 . ? C2D N2D 1.36(2) . ? C2D H2A1 0.9900 . ? C2D H2A2 0.9900 . ? N2D C3D 1.38(2) . ? N2D H22B 0.9300 . ? C3D C4D 1.40(3) . ? C3D H3A1 0.9900 . ? C3D H3A2 0.9900 . ? C4D N3D 1.50(2) . ? C4D H4A1 0.9900 . ? C4D H4A2 0.9900 . ? N3D H3A3 0.9200 . ? N3D H3A4 0.9200 . ? N1DA C1DA 1.490(18) . ? N1DA H1B1 0.9200 . ? N1DA H1B2 0.9200 . ? C1DA C2DA 1.48(2) . ? C1DA H1B3 0.9900 . ? C1DA H1B4 0.9900 . ? C2DA N2DA 1.452(18) . ? C2DA H2B1 0.9900 . ? C2DA H2B2 0.9900 . ? N2DA C3DA 1.472(18) . ? N2DA H22A 0.9300 . ? C3DA C4DA 1.47(2) . ? C3DA H3B1 0.9900 . ? C3DA H3B2 0.9900 . ? C4DA N3DA 1.464(18) . ? C4DA H4B1 0.9900 . ? C4DA H4B2 0.9900 . ? N3DA H3B3 0.9200 . ? N3DA H3B4 0.9200 . ? Cl1 O11 1.378(11) . ? Cl1 O12 1.389(13) . ? Cl1 O13 1.404(15) . ? Cl1 O14 1.418(18) . ? Cl2 O21 1.375(12) . ? Cl2 O22 1.380(13) . ? Cl2 O23 1.425(14) . ? Cl2 O24 1.433(13) . ? Cl3 O32 1.360(13) . ? Cl3 O34 1.395(14) . ? Cl3 O31 1.396(14) . ? Cl3 O33 1.448(13) . ? 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 N2D Pt1 N9 176.5(6) . . ? N2D Pt1 N1D 88.0(6) . . ? N9 Pt1 N1D 90.9(5) . . ? N2D Pt1 N3D 81.9(6) . . ? N9 Pt1 N3D 99.1(5) . . ? N1D Pt1 N3D 169.3(5) . . ? N2DA Pt2 N7 176.8(5) . . ? N2DA Pt2 N1DA 84.1(5) . . ? N7 Pt2 N1DA 97.4(4) . . ? N2DA Pt2 N3DA 85.1(5) . . ? N7 Pt2 N3DA 93.8(5) . . ? N1DA Pt2 N3DA 167.0(5) . . ? C2 N1 C6 123.2(12) . . ? C2 N1 H11A 118.4 . . ? C6 N1 H11A 118.4 . . ? N2 C2 N3 120.4(13) . . ? N2 C2 N1 113.9(13) . . ? N3 C2 N1 125.8(12) . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C2 N3 C4 113.5(11) . . ? N3 C4 N9 123.9(12) . . ? N3 C4 C5 123.8(12) . . ? N9 C4 C5 112.3(11) . . ? N7 C5 C4 104.0(11) . . ? N7 C5 C6 133.3(12) . . ? C4 C5 C6 122.7(11) . . ? O6 C6 N1 116.6(12) . . ? O6 C6 C5 132.4(11) . . ? N1 C6 C5 111.0(12) . . ? C8 N9 C4 102.2(11) . . ? C8 N9 Pt1 127.6(9) . . ? C4 N9 Pt1 129.3(8) . . ? N9 C8 N7 115.7(12) . . ? N9 C8 H8 122.2 . . ? N7 C8 H8 122.2 . . ? C8 N7 C5 105.8(10) . . ? C8 N7 Pt2 125.9(9) . . ? C5 N7 Pt2 127.8(9) . . ? C1D N1D Pt1 104.8(12) . . ? C1D N1D H1A1 110.8 . . ? Pt1 N1D H1A1 110.8 . . ? C1D N1D H1A2 110.8 . . ? Pt1 N1D H1A2 110.8 . . ? H1A1 N1D H1A2 108.9 . . ? C2D C1D N1D 115.6(16) . . ? C2D C1D H1A3 108.4 . . ? N1D C1D H1A3 108.4 . . ? C2D C1D H1A4 108.4 . . ? N1D C1D H1A4 108.4 . . ? H1A3 C1D H1A4 107.4 . . ? N2D C2D C1D 116.0(16) . . ? N2D C2D H2A1 108.3 . . ? C1D C2D H2A1 108.3 . . ? N2D C2D H2A2 108.3 . . ? C1D C2D H2A2 108.3 . . ? H2A1 C2D H2A2 107.4 . . ? C2D N2D C3D 130.9(16) . . ? C2D N2D Pt1 108.8(12) . . ? C3D N2D Pt1 112.1(12) . . ? C2D N2D H22B 99.5 . . ? C3D N2D H22B 99.5 . . ? Pt1 N2D H22B 99.5 . . ? N2D C3D C4D 120.2(16) . . ? N2D C3D H3A1 107.3 . . ? C4D C3D H3A1 107.3 . . ? N2D C3D H3A2 107.3 . . ? C4D C3D H3A2 107.3 . . ? H3A1 C3D H3A2 106.9 . . ? C3D C4D N3D 109.7(16) . . ? C3D C4D H4A1 109.7 . . ? N3D C4D H4A1 109.7 . . ? C3D C4D H4A2 109.7 . . ? N3D C4D H4A2 109.7 . . ? H4A1 C4D H4A2 108.2 . . ? C4D N3D Pt1 111.8(12) . . ? C4D N3D H3A3 109.3 . . ? Pt1 N3D H3A3 109.3 . . ? C4D N3D H3A4 109.3 . . ? Pt1 N3D H3A4 109.3 . . ? H3A3 N3D H3A4 107.9 . . ? C1DA N1DA Pt2 110.1(9) . . ? C1DA N1DA H1B1 109.6 . . ? Pt2 N1DA H1B1 109.6 . . ? C1DA N1DA H1B2 109.6 . . ? Pt2 N1DA H1B2 109.6 . . ? H1B1 N1DA H1B2 108.2 . . ? C2DA C1DA N1DA 105.9(12) . . ? C2DA C1DA H1B3 110.6 . . ? N1DA C1DA H1B3 110.6 . . ? C2DA C1DA H1B4 110.6 . . ? N1DA C1DA H1B4 110.6 . . ? H1B3 C1DA H1B4 108.7 . . ? N2DA C2DA C1DA 107.8(12) . . ? N2DA C2DA H2B1 110.1 . . ? C1DA C2DA H2B1 110.1 . . ? N2DA C2DA H2B2 110.1 . . ? C1DA C2DA H2B2 110.1 . . ? H2B1 C2DA H2B2 108.5 . . ? C2DA N2DA C3DA 117.2(12) . . ? C2DA N2DA Pt2 107.6(9) . . ? C3DA N2DA Pt2 105.7(9) . . ? C2DA N2DA H22A 108.7 . . ? C3DA N2DA H22A 108.7 . . ? Pt2 N2DA H22A 108.7 . . ? C4DA C3DA N2DA 106.3(12) . . ? C4DA C3DA H3B1 110.5 . . ? N2DA C3DA H3B1 110.5 . . ? C4DA C3DA H3B2 110.5 . . ? N2DA C3DA H3B2 110.5 . . ? H3B1 C3DA H3B2 108.7 . . ? N3DA C4DA C3DA 108.1(12) . . ? N3DA C4DA H4B1 110.1 . . ? C3DA C4DA H4B1 110.1 . . ? N3DA C4DA H4B2 110.1 . . ? C3DA C4DA H4B2 110.1 . . ? H4B1 C4DA H4B2 108.4 . . ? C4DA N3DA Pt2 107.6(9) . . ? C4DA N3DA H3B3 110.2 . . ? Pt2 N3DA H3B3 110.2 . . ? C4DA N3DA H3B4 110.2 . . ? Pt2 N3DA H3B4 110.2 . . ? H3B3 N3DA H3B4 108.5 . . ? O11 Cl1 O12 109.5(8) . . ? O11 Cl1 O13 106.5(8) . . ? O12 Cl1 O13 109.7(11) . . ? O11 Cl1 O14 111.8(11) . . ? O12 Cl1 O14 105.8(10) . . ? O13 Cl1 O14 113.5(12) . . ? O21 Cl2 O22 109.7(8) . . ? O21 Cl2 O23 110.0(8) . . ? O22 Cl2 O23 110.9(10) . . ? O21 Cl2 O24 110.3(8) . . ? O22 Cl2 O24 104.1(9) . . ? O23 Cl2 O24 111.7(8) . . ? O32 Cl3 O34 109.4(10) . . ? O32 Cl3 O31 108.1(11) . . ? O34 Cl3 O31 108.8(11) . . ? O32 Cl3 O33 111.6(8) . . ? O34 Cl3 O33 104.7(10) . . ? O31 Cl3 O33 114.1(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 C6 N1 C2 N2 -178.8(12) . . . . ? C6 N1 C2 N3 3(2) . . . . ? N2 C2 N3 C4 -179.6(12) . . . . ? N1 C2 N3 C4 -1.5(18) . . . . ? C2 N3 C4 N9 179.6(11) . . . . ? C2 N3 C4 C5 0.3(18) . . . . ? N3 C4 C5 N7 179.3(11) . . . . ? N9 C4 C5 N7 -0.1(14) . . . . ? N3 C4 C5 C6 0(2) . . . . ? N9 C4 C5 C6 -179.9(11) . . . . ? C2 N1 C6 O6 178.8(11) . . . . ? C2 N1 C6 C5 -2.8(17) . . . . ? N7 C5 C6 O6 0(2) . . . . ? C4 C5 C6 O6 179.7(13) . . . . ? N7 C5 C6 N1 -178.1(13) . . . . ? C4 C5 C6 N1 1.7(17) . . . . ? N3 C4 N9 C8 -179.3(12) . . . . ? C5 C4 N9 C8 0.1(14) . . . . ? N3 C4 N9 Pt1 -10.0(18) . . . . ? C5 C4 N9 Pt1 169.4(8) . . . . ? N1D Pt1 N9 C8 127.6(12) . . . . ? N3D Pt1 N9 C8 -48.6(12) . . . . ? N1D Pt1 N9 C4 -39.1(11) . . . . ? N3D Pt1 N9 C4 144.7(11) . . . . ? C4 N9 C8 N7 -0.2(15) . . . . ? Pt1 N9 C8 N7 -169.7(8) . . . . ? N9 C8 N7 C5 0.1(15) . . . . ? N9 C8 N7 Pt2 172.6(9) . . . . ? C4 C5 N7 C8 0.0(13) . . . . ? C6 C5 N7 C8 179.8(13) . . . . ? C4 C5 N7 Pt2 -172.3(8) . . . . ? C6 C5 N7 Pt2 7(2) . . . . ? N1DA Pt2 N7 C8 141.0(11) . . . . ? N3DA Pt2 N7 C8 -32.4(11) . . . . ? N1DA Pt2 N7 C5 -48.1(11) . . . . ? N3DA Pt2 N7 C5 138.5(11) . . . . ? N2D Pt1 N1D C1D -0.3(13) . . . . ? N9 Pt1 N1D C1D -177.0(12) . . . . ? N3D Pt1 N1D C1D -17(4) . . . . ? Pt1 N1D C1D C2D 15(2) . . . . ? N1D C1D C2D N2D -30(3) . . . . ? C1D C2D N2D C3D 172(2) . . . . ? C1D C2D N2D Pt1 27(3) . . . . ? N1D Pt1 N2D C2D -14.7(16) . . . . ? N3D Pt1 N2D C2D 162.2(17) . . . . ? N1D Pt1 N2D C3D -166.8(16) . . . . ? N3D Pt1 N2D C3D 10.1(15) . . . . ? C2D N2D C3D C4D -167(2) . . . . ? Pt1 N2D C3D C4D -23(3) . . . . ? N2D C3D C4D N3D 24(3) . . . . ? C3D C4D N3D Pt1 -13(3) . . . . ? N2D Pt1 N3D C4D 2.0(16) . . . . ? N9 Pt1 N3D C4D 178.6(15) . . . . ? N1D Pt1 N3D C4D 19(4) . . . . ? N2DA Pt2 N1DA C1DA -6.2(10) . . . . ? N7 Pt2 N1DA C1DA 170.9(9) . . . . ? N3DA Pt2 N1DA C1DA -40(3) . . . . ? Pt2 N1DA C1DA C2DA 33.1(14) . . . . ? N1DA C1DA C2DA N2DA -52.9(16) . . . . ? C1DA C2DA N2DA C3DA 166.7(13) . . . . ? C1DA C2DA N2DA Pt2 47.9(15) . . . . ? N1DA Pt2 N2DA C2DA -22.8(11) . . . . ? N3DA Pt2 N2DA C2DA 150.1(11) . . . . ? N1DA Pt2 N2DA C3DA -148.7(10) . . . . ? N3DA Pt2 N2DA C3DA 24.1(10) . . . . ? C2DA N2DA C3DA C4DA -169.2(14) . . . . ? Pt2 N2DA C3DA C4DA -49.4(14) . . . . ? N2DA C3DA C4DA N3DA 56.3(18) . . . . ? C3DA C4DA N3DA Pt2 -34.7(16) . . . . ? N2DA Pt2 N3DA C4DA 5.6(10) . . . . ? N7 Pt2 N3DA C4DA -171.4(10) . . . . ? N1DA Pt2 N3DA C4DA 39(3) . . . . ? 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 N2 H2A O31 0.88 2.19 3.042(19) 162.3 . N2 H2A Cl3 0.88 2.98 3.830(13) 162.0 . N1D H1A2 O34 0.92 2.11 2.877(19) 140.6 . N1D H1A2 N3 0.92 2.42 3.034(15) 124.0 . N1DA H1B2 O6 0.92 1.99 2.854(14) 155.2 . N1D H1A1 O22 0.92 2.33 2.975(18) 127.1 2_655 N1D H1A1 O6 0.92 2.42 3.196(17) 141.8 3_665 N3D H3A3 O6 0.92 2.06 2.938(15) 160.3 3_765 N3D H3A4 O12 0.92 2.60 3.44(2) 152.0 2_755 N1DA H1B1 O34 0.92 2.34 3.044(19) 132.9 3_765 N1DA H1B1 N3 0.92 2.51 3.315(17) 146.4 3_765 N2DA H22A O32 0.93 2.31 3.11(2) 144.0 3_665 N2DA H22A O31 0.93 2.36 3.25(2) 158.7 3_665 N2DA H22A Cl3 0.93 2.85 3.777(14) 172.1 3_665 N3DA H3B3 O24 0.92 2.10 2.943(16) 152.6 2_655 N3DA H3B4 O14 0.92 2.18 2.97(2) 143.6 2_755 N1 H11A O24 0.88 2.15 2.991(17) 158.9 4_565 N2 H2B O11 0.88 2.32 2.990(16) 132.5 4_565 N2 H2B O24 0.88 2.56 3.299(18) 142.7 4_565 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 5.976 _refine_diff_density_min -6.259 _refine_diff_density_rms 0.262 # Attachment '2403.cif' # The compound referred in the manuscript as complex 5. data_2403 _database_code_depnum_ccdc_archive 'CCDC 731731' _audit_creation_method SHELXL-97 _publ_section_title_footnote ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 N12 O2 Pt, 2(H2 O), 2(Cl)' _chemical_formula_sum 'C12 H24 Cl2 N12 O4 Pt' _chemical_formula_weight 666.42 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8340(16) _cell_length_b 11.100(2) _cell_length_c 13.252(3) _cell_angle_alpha 102.69(3) _cell_angle_beta 100.49(3) _cell_angle_gamma 90.02(3) _cell_volume 1104.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5011 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 _exptl_crystal_description Plates _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 6.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.221 _exptl_absorpt_correction_T_max 0.515 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9818 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5011 _reflns_number_gt 4337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0094P)^2^+0.9866P] 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 5011 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 1.15548(2) 0.307391(13) 0.299130(14) 0.02350(6) Uani 1 1 d . . . N11 N 1.2715(4) 0.3054(3) 0.4496(3) 0.0325(8) Uani 1 1 d . . . H11A H 1.2610 0.2296 0.4604 0.049 Uiso 1 1 calc R . . H11B H 1.2206 0.3582 0.4946 0.049 Uiso 1 1 calc R . . H11C H 1.3836 0.3274 0.4594 0.049 Uiso 1 1 calc R . . N12 N 1.3404(5) 0.4356(3) 0.2952(3) 0.0405(10) Uani 1 1 d . . . H12A H 1.3017 0.4749 0.2443 0.061 Uiso 1 1 calc R . . H12B H 1.4372 0.3979 0.2828 0.061 Uiso 1 1 calc R . . H12C H 1.3628 0.4899 0.3568 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.50446(16) 0.74993(12) -0.05470(14) 0.0638(4) Uani 1 1 d . . . Cl2 Cl 1.67821(14) 0.37874(10) 0.46857(10) 0.0428(3) Uani 1 1 d . . . N1A N 0.7190(5) 0.5288(3) 0.0148(3) 0.0385(10) Uani 1 1 d . . . H1AA H 0.6528 0.5786 -0.0139 0.046 Uiso 1 1 calc R . . C2A C 0.7657(5) 0.5583(4) 0.1215(4) 0.0373(11) Uani 1 1 d . . . N2A N 0.6976(5) 0.6608(3) 0.1719(4) 0.0591(13) Uani 1 1 d . . . H2AA H 0.7243 0.6841 0.2394 0.071 Uiso 1 1 calc R . . H2AB H 0.6275 0.7027 0.1367 0.071 Uiso 1 1 calc R . . N3A N 0.8738(4) 0.4944(3) 0.1771(3) 0.0328(8) Uani 1 1 d . . . C4A C 0.9289(5) 0.3939(3) 0.1147(3) 0.0249(9) Uani 1 1 d . . . C5A C 0.8810(5) 0.3561(4) 0.0081(4) 0.0288(10) Uani 1 1 d . . . C6A C 0.7685(6) 0.4257(4) -0.0518(4) 0.0369(11) Uani 1 1 d . . . O6A O 0.7170(5) 0.4039(3) -0.1471(3) 0.0518(9) Uani 1 1 d . . . N7A N 0.9592(5) 0.2446(3) -0.0217(3) 0.0322(8) Uani 1 1 d . . . C7A C 0.9355(7) 0.1654(4) -0.1285(4) 0.0502(13) Uani 1 1 d . . . H7AA H 1.0215 0.1038 -0.1307 0.075 Uiso 1 1 calc R . . H7AB H 0.9478 0.2150 -0.1779 0.075 Uiso 1 1 calc R . . H7AC H 0.8217 0.1258 -0.1467 0.075 Uiso 1 1 calc R . . C8A C 1.0502(6) 0.2205(4) 0.0658(4) 0.0322(10) Uani 1 1 d . . . H8AA H 1.1150 0.1506 0.0679 0.039 Uiso 1 1 calc R . . N9A N 1.0377(4) 0.3081(3) 0.1501(3) 0.0269(8) Uani 1 1 d . . . N1B N 0.9888(5) -0.1390(3) 0.3930(3) 0.0339(9) Uani 1 1 d . . . H1BA H 0.9931 -0.2085 0.4117 0.041 Uiso 1 1 calc R . . C2B C 1.1443(6) -0.0817(4) 0.3930(4) 0.0330(10) Uani 1 1 d . . . N2B N 1.2896(5) -0.1411(3) 0.4195(4) 0.0470(11) Uani 1 1 d . . . H2BA H 1.3896 -0.1087 0.4200 0.056 Uiso 1 1 calc R . . H2BB H 1.2825 -0.2114 0.4360 0.056 Uiso 1 1 calc R . . N3B N 1.1562(4) 0.0268(3) 0.3676(3) 0.0299(8) Uani 1 1 d . . . C4B C 0.9993(5) 0.0721(3) 0.3375(3) 0.0277(9) Uani 1 1 d . . . C5B C 0.8404(5) 0.0187(3) 0.3331(4) 0.0281(9) Uani 1 1 d . . . C6B C 0.8239(6) -0.0939(4) 0.3651(4) 0.0324(10) Uani 1 1 d . . . O6B O 0.6918(4) -0.1512(3) 0.3695(3) 0.0425(8) Uani 1 1 d . . . N7B N 0.7165(4) 0.0937(3) 0.2935(3) 0.0327(9) Uani 1 1 d . . . C7B C 0.5275(6) 0.0747(5) 0.2726(5) 0.0535(15) Uani 1 1 d . . . H7BA H 0.4745 0.1411 0.2443 0.080 Uiso 1 1 calc R . . H7BB H 0.4890 0.0728 0.3371 0.080 Uiso 1 1 calc R . . H7BC H 0.4948 -0.0023 0.2229 0.080 Uiso 1 1 calc R . . C8B C 0.8047(6) 0.1880(4) 0.2766(4) 0.0331(10) Uani 1 1 d . . . H8BA H 0.7525 0.2518 0.2488 0.040 Uiso 1 1 calc R . . N9B N 0.9746(4) 0.1805(3) 0.3038(3) 0.0266(8) Uani 1 1 d . . . O1W O 0.9581(4) -0.3892(3) 0.3965(3) 0.0417(8) Uani 1 1 d . . . H1W H 1.0605 -0.4081 0.4300 0.062 Uiso 1 1 d R . . H2W H 0.9343 -0.4502 0.3386 0.062 Uiso 1 1 d R . . O2W O 1.2645(5) -0.0106(4) -0.0264(4) 0.0887(16) Uani 1 1 d . . . H3W H 1.3470 -0.0650 -0.0154 0.133 Uiso 1 1 d R . . H4W H 1.3282 0.0560 -0.0291 0.133 Uiso 1 1 d 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 0.02591(9) 0.02228(8) 0.02317(10) 0.00887(6) 0.00221(6) 0.00232(5) N11 0.037(2) 0.0332(19) 0.027(2) 0.0127(16) -0.0017(17) -0.0013(15) N12 0.042(2) 0.041(2) 0.041(3) 0.0225(19) -0.0038(19) -0.0089(16) Cl1 0.0448(8) 0.0564(8) 0.1003(14) 0.0464(8) 0.0044(8) 0.0076(6) Cl2 0.0395(7) 0.0401(6) 0.0455(8) 0.0103(5) -0.0013(6) 0.0002(5) N1A 0.037(2) 0.034(2) 0.043(3) 0.0149(19) -0.0049(19) 0.0044(16) C2A 0.029(2) 0.035(2) 0.043(3) 0.007(2) -0.003(2) -0.0006(18) N2A 0.057(3) 0.044(2) 0.063(4) -0.003(2) -0.007(2) 0.024(2) N3A 0.030(2) 0.0343(19) 0.032(2) 0.0058(17) 0.0011(17) 0.0066(14) C4A 0.027(2) 0.026(2) 0.020(2) 0.0070(17) 0.0004(18) -0.0004(15) C5A 0.028(2) 0.031(2) 0.029(3) 0.0120(19) 0.0051(19) -0.0015(16) C6A 0.033(2) 0.039(3) 0.039(3) 0.021(2) -0.007(2) -0.0089(18) O6A 0.062(2) 0.057(2) 0.034(2) 0.0201(18) -0.0091(19) -0.0032(16) N7A 0.042(2) 0.0332(19) 0.020(2) 0.0032(16) 0.0057(17) 0.0002(15) C7A 0.070(4) 0.049(3) 0.022(3) -0.007(2) 0.004(3) 0.004(2) C8A 0.038(3) 0.030(2) 0.030(3) 0.008(2) 0.009(2) 0.0053(17) N9A 0.0286(19) 0.0293(18) 0.024(2) 0.0111(16) 0.0020(16) 0.0050(13) N1B 0.044(2) 0.0240(18) 0.036(2) 0.0110(16) 0.0089(19) 0.0007(15) C2B 0.042(3) 0.028(2) 0.028(3) 0.0060(19) 0.006(2) 0.0028(18) N2B 0.040(2) 0.038(2) 0.069(3) 0.030(2) 0.005(2) 0.0086(17) N3B 0.033(2) 0.0284(18) 0.030(2) 0.0108(16) 0.0049(17) 0.0011(14) C4B 0.031(2) 0.026(2) 0.023(3) 0.0034(17) 0.0031(19) 0.0011(16) C5B 0.029(2) 0.029(2) 0.026(3) 0.0064(18) 0.0050(19) -0.0005(16) C6B 0.043(3) 0.029(2) 0.025(3) 0.0027(18) 0.008(2) -0.0034(18) O6B 0.0413(19) 0.0377(17) 0.051(2) 0.0126(16) 0.0125(17) -0.0076(13) N7B 0.0272(19) 0.0338(19) 0.038(3) 0.0097(17) 0.0075(18) 0.0007(14) C7B 0.030(3) 0.058(3) 0.080(5) 0.031(3) 0.008(3) 0.000(2) C8B 0.038(3) 0.030(2) 0.032(3) 0.0096(19) 0.005(2) 0.0030(17) N9B 0.0241(18) 0.0280(18) 0.027(2) 0.0064(15) 0.0033(16) 0.0033(13) O1W 0.0402(18) 0.0364(17) 0.045(2) 0.0080(15) 0.0009(16) 0.0066(13) O2W 0.056(3) 0.062(3) 0.141(5) 0.002(3) 0.024(3) 0.0089(19) _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 N9B 2.016(3) . ? Pt1 N9A 2.023(3) . ? Pt1 N11 2.040(4) . ? Pt1 N12 2.046(3) . ? N11 H11A 0.8900 . ? N11 H11B 0.8900 . ? N11 H11C 0.8900 . ? N12 H12A 0.8900 . ? N12 H12B 0.8900 . ? N12 H12C 0.8900 . ? N1A C2A 1.359(6) . ? N1A C6A 1.386(6) . ? N1A H1AA 0.8600 . ? C2A N3A 1.329(5) . ? C2A N2A 1.350(6) . ? N2A H2AA 0.8600 . ? N2A H2AB 0.8600 . ? N3A C4A 1.356(5) . ? C4A C5A 1.364(6) . ? C4A N9A 1.381(5) . ? C5A N7A 1.392(5) . ? C5A C6A 1.422(6) . ? C6A O6A 1.223(6) . ? N7A C8A 1.327(6) . ? N7A C7A 1.473(6) . ? C7A H7AA 0.9600 . ? C7A H7AB 0.9600 . ? C7A H7AC 0.9600 . ? C8A N9A 1.329(6) . ? C8A H8AA 0.9300 . ? N1B C2B 1.374(5) . ? N1B C6B 1.402(5) . ? N1B H1BA 0.8600 . ? C2B N3B 1.327(5) . ? C2B N2B 1.345(5) . ? N2B H2BA 0.8600 . ? N2B H2BB 0.8600 . ? N3B C4B 1.354(5) . ? C4B C5B 1.365(5) . ? C4B N9B 1.374(5) . ? C5B N7B 1.385(5) . ? C5B C6B 1.418(5) . ? C6B O6B 1.232(5) . ? N7B C8B 1.334(5) . ? N7B C7B 1.463(5) . ? C7B H7BA 0.9600 . ? C7B H7BB 0.9600 . ? C7B H7BC 0.9600 . ? C8B N9B 1.322(5) . ? C8B H8BA 0.9300 . ? O1W H1W 0.8919 . ? O1W H2W 0.8946 . ? O2W H3W 0.8989 . ? O2W H4W 0.9021 . ? 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 N9B Pt1 N9A 89.09(14) . . ? N9B Pt1 N11 90.17(14) . . ? N9A Pt1 N11 179.25(13) . . ? N9B Pt1 N12 179.56(14) . . ? N9A Pt1 N12 91.29(14) . . ? N11 Pt1 N12 89.45(15) . . ? Pt1 N11 H11A 109.5 . . ? Pt1 N11 H11B 109.5 . . ? H11A N11 H11B 109.5 . . ? Pt1 N11 H11C 109.5 . . ? H11A N11 H11C 109.5 . . ? H11B N11 H11C 109.5 . . ? Pt1 N12 H12A 109.5 . . ? Pt1 N12 H12B 109.5 . . ? H12A N12 H12B 109.5 . . ? Pt1 N12 H12C 109.5 . . ? H12A N12 H12C 109.5 . . ? H12B N12 H12C 109.5 . . ? C2A N1A C6A 125.8(4) . . ? C2A N1A H1AA 117.1 . . ? C6A N1A H1AA 117.1 . . ? N3A C2A N2A 119.3(5) . . ? N3A C2A N1A 124.4(4) . . ? N2A C2A N1A 116.3(4) . . ? C2A N2A H2AA 120.0 . . ? C2A N2A H2AB 120.0 . . ? H2AA N2A H2AB 120.0 . . ? C2A N3A C4A 111.8(4) . . ? N3A C4A C5A 126.8(4) . . ? N3A C4A N9A 125.1(4) . . ? C5A C4A N9A 108.0(4) . . ? C4A C5A N7A 107.1(3) . . ? C4A C5A C6A 121.5(4) . . ? N7A C5A C6A 131.4(4) . . ? O6A C6A N1A 121.9(4) . . ? O6A C6A C5A 128.5(5) . . ? N1A C6A C5A 109.6(4) . . ? C8A N7A C5A 106.5(4) . . ? C8A N7A C7A 127.0(4) . . ? C5A N7A C7A 126.4(4) . . ? N7A C7A H7AA 109.5 . . ? N7A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? N7A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N7A C8A N9A 112.0(4) . . ? N7A C8A H8AA 124.0 . . ? N9A C8A H8AA 124.0 . . ? C8A N9A C4A 106.4(4) . . ? C8A N9A Pt1 124.8(3) . . ? C4A N9A Pt1 128.8(3) . . ? C2B N1B C6B 125.7(3) . . ? C2B N1B H1BA 117.2 . . ? C6B N1B H1BA 117.2 . . ? N3B C2B N2B 119.7(4) . . ? N3B C2B N1B 123.2(4) . . ? N2B C2B N1B 117.1(4) . . ? C2B N2B H2BA 120.0 . . ? C2B N2B H2BB 120.0 . . ? H2BA N2B H2BB 120.0 . . ? C2B N3B C4B 113.0(3) . . ? N3B C4B C5B 126.8(4) . . ? N3B C4B N9B 124.8(3) . . ? C5B C4B N9B 108.4(3) . . ? C4B C5B N7B 107.2(3) . . ? C4B C5B C6B 121.5(4) . . ? N7B C5B C6B 131.4(4) . . ? O6B C6B N1B 120.8(4) . . ? O6B C6B C5B 129.5(4) . . ? N1B C6B C5B 109.8(3) . . ? C8B N7B C5B 105.9(3) . . ? C8B N7B C7B 126.3(3) . . ? C5B N7B C7B 127.8(3) . . ? N7B C7B H7BA 109.5 . . ? N7B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? N7B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N9B C8B N7B 112.5(3) . . ? N9B C8B H8BA 123.8 . . ? N7B C8B H8BA 123.8 . . ? C8B N9B C4B 106.0(3) . . ? C8B N9B Pt1 125.7(3) . . ? C4B N9B Pt1 128.2(3) . . ? H1W O1W H2W 103.8 . . ? H3W O2W H4W 101.9 . . ? 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 C6A N1A C2A N3A 3.5(7) . . . . ? C6A N1A C2A N2A -177.6(4) . . . . ? N2A C2A N3A C4A 179.5(4) . . . . ? N1A C2A N3A C4A -1.6(6) . . . . ? C2A N3A C4A C5A -1.6(6) . . . . ? C2A N3A C4A N9A -178.0(4) . . . . ? N3A C4A C5A N7A -175.8(4) . . . . ? N9A C4A C5A N7A 1.0(4) . . . . ? N3A C4A C5A C6A 3.2(6) . . . . ? N9A C4A C5A C6A -179.9(3) . . . . ? C2A N1A C6A O6A 178.0(4) . . . . ? C2A N1A C6A C5A -1.7(6) . . . . ? C4A C5A C6A O6A 179.0(4) . . . . ? N7A C5A C6A O6A -2.2(8) . . . . ? C4A C5A C6A N1A -1.4(5) . . . . ? N7A C5A C6A N1A 177.5(4) . . . . ? C4A C5A N7A C8A -0.5(4) . . . . ? C6A C5A N7A C8A -179.4(4) . . . . ? C4A C5A N7A C7A 175.8(4) . . . . ? C6A C5A N7A C7A -3.1(7) . . . . ? C5A N7A C8A N9A -0.3(5) . . . . ? C7A N7A C8A N9A -176.6(4) . . . . ? N7A C8A N9A C4A 0.9(5) . . . . ? N7A C8A N9A Pt1 179.8(2) . . . . ? N3A C4A N9A C8A 175.7(4) . . . . ? C5A C4A N9A C8A -1.2(4) . . . . ? N3A C4A N9A Pt1 -3.1(6) . . . . ? C5A C4A N9A Pt1 180.0(3) . . . . ? N9B Pt1 N9A C8A -76.4(3) . . . . ? N12 Pt1 N9A C8A 103.3(3) . . . . ? N9B Pt1 N9A C4A 102.3(3) . . . . ? N12 Pt1 N9A C4A -78.0(3) . . . . ? C6B N1B C2B N3B 1.2(7) . . . . ? C6B N1B C2B N2B -178.2(4) . . . . ? N2B C2B N3B C4B 176.8(4) . . . . ? N1B C2B N3B C4B -2.7(6) . . . . ? C2B N3B C4B C5B 0.9(7) . . . . ? C2B N3B C4B N9B -177.6(4) . . . . ? N3B C4B C5B N7B -177.2(4) . . . . ? N9B C4B C5B N7B 1.5(5) . . . . ? N3B C4B C5B C6B 2.5(7) . . . . ? N9B C4B C5B C6B -178.8(4) . . . . ? C2B N1B C6B O6B -178.7(4) . . . . ? C2B N1B C6B C5B 2.0(6) . . . . ? C4B C5B C6B O6B 177.1(5) . . . . ? N7B C5B C6B O6B -3.3(9) . . . . ? C4B C5B C6B N1B -3.6(6) . . . . ? N7B C5B C6B N1B 176.0(5) . . . . ? C4B C5B N7B C8B -0.3(5) . . . . ? C6B C5B N7B C8B -180.0(5) . . . . ? C4B C5B N7B C7B 179.0(5) . . . . ? C6B C5B N7B C7B -0.6(8) . . . . ? C5B N7B C8B N9B -1.0(5) . . . . ? C7B N7B C8B N9B 179.6(5) . . . . ? N7B C8B N9B C4B 2.0(5) . . . . ? N7B C8B N9B Pt1 -176.4(3) . . . . ? N3B C4B N9B C8B 176.6(4) . . . . ? C5B C4B N9B C8B -2.1(5) . . . . ? N3B C4B N9B Pt1 -5.0(6) . . . . ? C5B C4B N9B Pt1 176.2(3) . . . . ? N9A Pt1 N9B C8B -49.4(4) . . . . ? N11 Pt1 N9B C8B 130.5(4) . . . . ? N9A Pt1 N9B C4B 132.6(4) . . . . ? N11 Pt1 N9B C4B -47.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.114 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.144 # Attachment '2461.CIF' # The compound referred in the manuscript as complex 1a. data_2461 _database_code_depnum_ccdc_archive 'CCDC 731732' _audit_creation_method SHELXL-97 _publ_section_title_footnote ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C9 H18 N8 O Pt),8(Cl O4),9(H2O)' _chemical_formula_sum 'C36 H90 Cl8 N32 O45 Pt4' _chemical_formula_weight 2755.36 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 C2/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.466(8) _cell_length_b 11.210(2) _cell_length_c 27.134(5) _cell_angle_alpha 90.00 _cell_angle_beta 133.49(3) _cell_angle_gamma 90.00 _cell_volume 8488(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9520 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needles _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5352 _exptl_absorpt_coefficient_mu 6.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.351 _exptl_absorpt_correction_T_max 0.500 _exptl_absorpt_process_details 'SADABS, Sheldrick, Bruker, 2000' _exptl_special_details ; One of the perchlorate anions based on Cl is disordered. Further DFIX constraints and SIMU restraints were imposed to maintain reasonable geometries for two out of four perchlorate anions. ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27651 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9520 _reflns_number_gt 5844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0672P)^2^+75.2652P] 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 9520 _refine_ls_number_parameters 537 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1546 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.087 _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 0.118474(16) 0.59183(4) 0.43741(2) 0.03871(14) Uani 1 1 d . . . Pt2 Pt 0.123065(15) 0.30700(4) 0.18958(2) 0.03994(15) Uani 1 1 d . . . N1D N 0.1430(3) 0.4385(9) 0.4296(5) 0.048(3) Uani 1 1 d . . . H77A H 0.1309 0.3747 0.4336 0.058 Uiso 1 1 calc R . . H77B H 0.1337 0.4352 0.3887 0.058 Uiso 1 1 calc R . . C1D C 0.1977(5) 0.4366(14) 0.4859(7) 0.071(4) Uani 1 1 d . . . H6A H 0.2077 0.3973 0.5258 0.085 Uiso 1 1 calc R . . H6B H 0.2107 0.3922 0.4709 0.085 Uiso 1 1 calc R . . C2D C 0.2167(5) 0.5632(13) 0.5035(8) 0.064(4) Uani 1 1 d . . . H5A H 0.2506 0.5644 0.5444 0.077 Uiso 1 1 calc R . . H5B H 0.2121 0.5984 0.4667 0.077 Uiso 1 1 calc R . . N2D N 0.1887(3) 0.6305(10) 0.5144(5) 0.053(3) Uani 1 1 d . . . H44A H 0.1976 0.6005 0.5529 0.064 Uiso 1 1 calc R . . C3D C 0.1945(6) 0.7614(12) 0.5231(9) 0.074(4) Uani 1 1 d . . . H3A H 0.1907 0.7975 0.4871 0.089 Uiso 1 1 calc R . . H3B H 0.2259 0.7818 0.5665 0.089 Uiso 1 1 calc R . . C4D C 0.1559(6) 0.8039(14) 0.5199(10) 0.088(6) Uani 1 1 d . . . H2A H 0.1621 0.7748 0.5590 0.106 Uiso 1 1 calc R . . H2B H 0.1556 0.8904 0.5206 0.106 Uiso 1 1 calc R . . N3D N 0.1085(4) 0.7589(9) 0.4562(6) 0.057(3) Uani 1 1 d . . . H33A H 0.0966 0.8079 0.4213 0.069 Uiso 1 1 calc R . . H33B H 0.0876 0.7561 0.4610 0.069 Uiso 1 1 calc R . . N1A N -0.0279(4) 0.2534(11) 0.2841(5) 0.053(3) Uani 1 1 d . . . H1AA H -0.0435 0.1873 0.2678 0.063 Uiso 1 1 calc R . . C2A C 0.0201(4) 0.2457(13) 0.3353(6) 0.046(3) Uani 1 1 d . . . N2A N 0.0379(4) 0.1344(10) 0.3532(6) 0.058(3) Uani 1 1 d . . . H2AA H 0.0684 0.1234 0.3842 0.070 Uiso 1 1 calc R . . H2AB H 0.0189 0.0742 0.3336 0.070 Uiso 1 1 calc R . . N3A N 0.0492(3) 0.3386(9) 0.3651(4) 0.040(2) Uani 1 1 d . . . C4A C 0.0256(4) 0.4438(11) 0.3392(5) 0.040(3) Uani 1 1 d . . . C5A C -0.0223(4) 0.4595(13) 0.2892(6) 0.049(3) Uani 1 1 d . . . C6A C -0.0545(4) 0.3580(14) 0.2551(6) 0.052(3) Uani 1 1 d . . . O6A O -0.0987(3) 0.3601(10) 0.2067(4) 0.065(3) Uani 1 1 d . . . N7A N -0.0309(4) 0.5787(12) 0.2793(5) 0.062(3) Uani 1 1 d . . . H7AA H -0.0584 0.6129 0.2503 0.074 Uiso 1 1 calc R . . C8A C 0.0116(5) 0.6324(12) 0.3231(6) 0.053(3) Uani 1 1 d . . . H8AA H 0.0159 0.7147 0.3265 0.063 Uiso 1 1 calc R . . N9A N 0.0470(3) 0.5538(9) 0.3611(4) 0.040(2) Uani 1 1 d . . . N1DA N 0.0858(3) 0.1937(8) 0.1094(4) 0.042(2) Uani 1 1 d . . . H71A H 0.0570 0.1784 0.0949 0.050 Uiso 1 1 calc R . . H71B H 0.0810 0.2275 0.0751 0.050 Uiso 1 1 calc R . . C1DA C 0.1131(5) 0.0794(12) 0.1300(6) 0.054(3) Uani 1 1 d . . . H61A H 0.0913 0.0138 0.1025 0.065 Uiso 1 1 calc R . . H61B H 0.1351 0.0854 0.1237 0.065 Uiso 1 1 calc R . . C2DA C 0.1403(5) 0.0589(13) 0.2031(7) 0.061(4) Uani 1 1 d . . . H51A H 0.1183 0.0421 0.2084 0.073 Uiso 1 1 calc R . . H51B H 0.1617 -0.0087 0.2203 0.073 Uiso 1 1 calc R . . N2DA N 0.1680(4) 0.1674(11) 0.2409(5) 0.056(3) Uani 1 1 d . . . H41A H 0.1919 0.1743 0.2418 0.067 Uiso 1 1 calc R . . C3DA C 0.1889(5) 0.1772(17) 0.3118(6) 0.076(5) Uani 1 1 d . . . H31A H 0.1647 0.1590 0.3128 0.092 Uiso 1 1 calc R . . H31B H 0.2151 0.1211 0.3411 0.092 Uiso 1 1 calc R . . C4DA C 0.2063(6) 0.2997(18) 0.3355(8) 0.088(6) Uani 1 1 d . . . H21A H 0.2341 0.3133 0.3418 0.106 Uiso 1 1 calc R . . H21B H 0.2158 0.3118 0.3789 0.106 Uiso 1 1 calc R . . N3DA N 0.1666(4) 0.3869(11) 0.2833(5) 0.060(3) Uani 1 1 d . . . H11A H 0.1793 0.4542 0.2831 0.072 Uiso 1 1 calc R . . H11B H 0.1496 0.4062 0.2936 0.072 Uiso 1 1 calc R . . N1B N -0.0669(3) 0.4468(9) -0.0035(4) 0.044(2) Uani 1 1 d . . . H1BA H -0.0977 0.4470 -0.0330 0.053 Uiso 1 1 calc R . . C2B C -0.0448(4) 0.3382(11) 0.0180(6) 0.044(3) Uani 1 1 d . . . N2B N -0.0717(4) 0.2399(10) -0.0093(5) 0.060(3) Uani 1 1 d . . . H2BA H -0.0583 0.1708 0.0040 0.071 Uiso 1 1 calc R . . H2BB H -0.1024 0.2455 -0.0401 0.071 Uiso 1 1 calc R . . N3B N 0.0022(3) 0.3271(8) 0.0652(4) 0.036(2) Uani 1 1 d . . . C4B C 0.0263(4) 0.4330(10) 0.0894(5) 0.037(3) Uani 1 1 d . . . C5B C 0.0057(4) 0.5433(10) 0.0676(5) 0.038(3) Uani 1 1 d . . . C6B C -0.0439(4) 0.5583(11) 0.0182(6) 0.043(3) Uani 1 1 d . . . O6B O -0.0675(3) 0.6524(8) -0.0058(4) 0.053(2) Uani 1 1 d . . . N7B N 0.0441(4) 0.6233(9) 0.1047(5) 0.051(3) Uani 1 1 d . . . H7BA H 0.0422 0.6998 0.1015 0.062 Uiso 1 1 calc R . . C8B C 0.0839(5) 0.5597(12) 0.1455(7) 0.050(3) Uani 1 1 d . . . H8BA H 0.1144 0.5929 0.1760 0.060 Uiso 1 1 calc R . . N9B N 0.0756(3) 0.4449(9) 0.1384(5) 0.042(2) Uani 1 1 d . . . Cl1 Cl -0.00321(12) 0.9338(3) 0.08099(16) 0.0501(7) Uani 1 1 d . . . O11 O 0.0206(4) 1.0450(9) 0.1116(6) 0.084(3) Uani 1 1 d . . . O12 O 0.0169(4) 0.8705(9) 0.0601(6) 0.084(3) Uani 1 1 d . . . O13 O 0.0011(4) 0.8652(11) 0.1281(5) 0.101(4) Uani 1 1 d . . . O14 O -0.0520(4) 0.9519(12) 0.0244(6) 0.102(4) Uani 1 1 d . . . Cl2 Cl 0.17226(14) 0.0920(3) 0.45972(19) 0.0694(10) Uani 1 1 d . . . O21 O 0.2133(4) 0.0382(12) 0.5188(5) 0.101(4) Uani 1 1 d . . . O22 O 0.1366(5) 0.0038(12) 0.4150(6) 0.130(6) Uani 1 1 d . . . O23 O 0.1531(5) 0.1706(13) 0.4762(8) 0.124(5) Uani 1 1 d . . . O24 O 0.1844(7) 0.1542(15) 0.4283(8) 0.150(6) Uani 1 1 d . . . Cl3 Cl -0.14306(16) 0.7442(4) 0.1883(2) 0.0978(14) Uani 1 1 d DU . . O31 O -0.1840(4) 0.7964(13) 0.1287(6) 0.180(7) Uani 1 1 d DU . . O32 O -0.1024(4) 0.7715(14) 0.1936(8) 0.174(7) Uani 1 1 d DU . . O33 O -0.1442(5) 0.6174(7) 0.1895(7) 0.175(8) Uani 1 1 d DU . . O34 O -0.1300(6) 0.7936(14) 0.2476(6) 0.219(9) Uani 1 1 d DU . . Cl4 Cl 0.2421(3) 0.5802(10) 0.2736(5) 0.217(4) Uani 1 1 d DU . . O41 O 0.2434(8) 0.581(2) 0.3268(9) 0.253(8) Uani 1 1 d DU . . O42 O 0.2734(8) 0.4847(16) 0.2856(13) 0.310(11) Uani 1 1 d DU . . O43 O 0.2586(7) 0.6901(13) 0.2683(11) 0.255(9) Uani 1 1 d DU . . O44 O 0.1943(5) 0.554(2) 0.2083(8) 0.387(17) Uani 1 1 d DU . . O1W O -0.0724(4) 0.0244(11) 0.2307(6) 0.094(3) Uiso 1 1 d . . . H1W H -0.0884 -0.0345 0.2042 0.140 Uiso 1 1 d R . . H2W H -0.0759 0.0259 0.2584 0.140 Uiso 1 1 d R . . O2W O -0.1754(7) 0.4224(15) -0.1050(9) 0.251(12) Uiso 1 1 d . . . H3W H -0.1930 0.4784 -0.1111 0.376 Uiso 1 1 d R . . H4W H -0.1874 0.3993 -0.1438 0.376 Uiso 1 1 d R . . O3W O 0.0000(7) -0.1232(15) 0.2500(9) 0.205(12) Uiso 1 2 d SR . . H5W H -0.0209 -0.0791 0.2395 0.308 Uiso 1 1 d R . . O4W O -0.1713(7) 0.1832(15) -0.1009(9) 0.274(13) Uiso 1 1 d R . . H7W H -0.1832 0.1192 -0.1240 0.411 Uiso 1 1 d R . . H8W H -0.1760 0.1832 -0.0745 0.411 Uiso 1 1 d R . . O5W O 0.2440(11) 0.593(3) 0.6584(15) 0.309(16) Uiso 1 1 d . . . H9W H 0.2413 0.5309 0.6735 0.464 Uiso 1 1 d R . . H10W H 0.2499 0.6514 0.6833 0.464 Uiso 1 1 d 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 0.0412(3) 0.0359(3) 0.0447(3) -0.0001(2) 0.0317(2) 0.0022(2) Pt2 0.0346(2) 0.0506(3) 0.0385(2) -0.0005(2) 0.0266(2) 0.0005(2) N1D 0.040(6) 0.041(6) 0.058(6) -0.009(5) 0.032(5) 0.000(5) C1D 0.040(8) 0.068(11) 0.068(9) -0.013(8) 0.023(7) 0.011(7) C2D 0.048(8) 0.054(9) 0.081(10) -0.013(7) 0.041(8) -0.003(7) N2D 0.038(6) 0.058(7) 0.060(6) -0.018(6) 0.033(5) -0.013(5) C3D 0.076(10) 0.039(9) 0.120(13) -0.024(9) 0.073(11) -0.018(8) C4D 0.104(13) 0.061(11) 0.143(16) -0.055(11) 0.101(13) -0.037(10) N3D 0.076(8) 0.031(6) 0.091(8) -0.003(6) 0.067(7) 0.000(6) N1A 0.046(6) 0.064(8) 0.050(6) -0.011(6) 0.034(6) -0.013(6) C2A 0.029(6) 0.065(9) 0.044(7) -0.002(6) 0.025(6) -0.002(6) N2A 0.048(7) 0.043(7) 0.073(7) -0.002(6) 0.038(6) -0.004(6) N3A 0.038(5) 0.047(6) 0.039(5) 0.002(4) 0.028(5) 0.007(5) C4A 0.034(6) 0.052(8) 0.033(6) -0.004(5) 0.023(5) 0.007(6) C5A 0.042(7) 0.062(9) 0.046(7) 0.002(6) 0.031(6) 0.006(7) C6A 0.045(8) 0.087(11) 0.035(6) -0.005(7) 0.032(6) -0.001(8) O6A 0.029(5) 0.116(8) 0.034(4) -0.007(5) 0.015(4) -0.003(5) N7A 0.038(6) 0.095(10) 0.035(6) 0.010(6) 0.019(5) 0.027(6) C8A 0.065(9) 0.043(8) 0.054(7) 0.014(6) 0.042(8) 0.025(7) N9A 0.033(5) 0.046(6) 0.038(5) 0.001(4) 0.023(4) 0.009(5) N1DA 0.041(5) 0.049(6) 0.042(5) 0.008(5) 0.031(5) 0.011(5) C1DA 0.060(8) 0.057(9) 0.046(7) 0.009(6) 0.037(7) 0.011(7) C2DA 0.053(8) 0.058(10) 0.064(9) 0.012(7) 0.038(7) 0.012(7) N2DA 0.040(6) 0.079(9) 0.048(6) 0.016(6) 0.030(5) 0.018(6) C3DA 0.053(9) 0.113(15) 0.035(7) 0.010(8) 0.019(7) 0.022(9) C4DA 0.063(10) 0.126(17) 0.058(9) -0.019(10) 0.035(9) 0.011(11) N3DA 0.051(7) 0.083(9) 0.052(6) -0.012(6) 0.038(6) -0.002(6) N1B 0.039(6) 0.050(7) 0.038(5) 0.005(5) 0.025(5) 0.009(5) C2B 0.046(7) 0.049(8) 0.042(6) -0.001(6) 0.032(6) 0.000(6) N2B 0.045(6) 0.054(7) 0.052(6) 0.005(6) 0.023(5) 0.002(6) N3B 0.039(5) 0.024(5) 0.043(5) -0.003(4) 0.028(5) 0.001(4) C4B 0.048(7) 0.042(7) 0.034(6) 0.000(5) 0.033(6) 0.005(5) C5B 0.055(7) 0.031(6) 0.043(6) 0.008(5) 0.040(6) 0.005(6) C6B 0.056(8) 0.044(8) 0.042(6) 0.006(6) 0.039(6) 0.008(6) O6B 0.066(6) 0.042(5) 0.064(5) 0.015(4) 0.050(5) 0.021(5) N7B 0.074(8) 0.030(6) 0.066(7) -0.005(5) 0.055(7) -0.002(6) C8B 0.055(8) 0.045(8) 0.057(8) -0.007(6) 0.042(7) -0.004(6) N9B 0.038(6) 0.040(6) 0.048(6) -0.005(4) 0.030(5) 0.000(4) Cl1 0.059(2) 0.0385(18) 0.0579(18) 0.0003(14) 0.0425(17) -0.0035(14) O11 0.097(8) 0.055(7) 0.140(10) -0.036(7) 0.096(8) -0.026(6) O12 0.113(9) 0.050(6) 0.137(10) -0.013(6) 0.104(9) 0.001(6) O13 0.122(10) 0.106(9) 0.069(7) 0.024(7) 0.064(7) -0.021(8) O14 0.077(8) 0.108(10) 0.078(7) -0.007(7) 0.038(7) 0.012(7) Cl2 0.072(2) 0.058(2) 0.064(2) 0.0049(18) 0.041(2) 0.017(2) O21 0.057(7) 0.092(9) 0.079(7) 0.009(7) 0.018(6) 0.006(7) O22 0.093(10) 0.081(10) 0.091(8) -0.013(7) 0.016(8) -0.004(8) O23 0.140(12) 0.105(11) 0.167(13) 0.000(10) 0.121(12) 0.032(9) O24 0.226(19) 0.142(14) 0.145(13) 0.036(11) 0.153(14) 0.025(13) Cl3 0.066(3) 0.073(3) 0.091(3) 0.016(2) 0.030(2) 0.009(2) O31 0.085(9) 0.183(14) 0.155(11) 0.087(10) 0.038(9) 0.034(9) O32 0.092(9) 0.149(13) 0.210(13) 0.018(11) 0.077(10) 0.014(9) O33 0.158(12) 0.097(11) 0.148(11) 0.019(9) 0.059(10) -0.014(10) O34 0.226(15) 0.169(15) 0.151(13) -0.018(11) 0.087(12) 0.046(13) Cl4 0.187(7) 0.293(12) 0.280(10) 0.008(9) 0.203(8) -0.020(7) O41 0.273(15) 0.31(2) 0.288(17) -0.029(16) 0.238(13) -0.066(15) O42 0.236(17) 0.35(2) 0.380(19) -0.020(19) 0.224(15) 0.031(17) O43 0.197(14) 0.280(19) 0.372(18) 0.092(16) 0.227(13) -0.002(13) O44 0.165(16) 0.35(2) 0.34(2) 0.048(19) 0.060(16) -0.074(17) _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 N2D 2.020(10) . ? Pt1 N1D 2.042(9) . ? Pt1 N3D 2.046(10) . ? Pt1 N9A 2.047(9) . ? Pt2 N2DA 2.015(10) . ? Pt2 N1DA 2.027(9) . ? Pt2 N9B 2.040(10) . ? Pt2 N3DA 2.052(10) . ? N1D C1D 1.528(15) . ? N1D H77A 0.9000 . ? N1D H77B 0.9000 . ? C1D C2D 1.51(2) . ? C1D H6A 0.9700 . ? C1D H6B 0.9700 . ? C2D N2D 1.501(16) . ? C2D H5A 0.9700 . ? C2D H5B 0.9700 . ? N2D C3D 1.479(17) . ? N2D H44A 0.9100 . ? C3D C4D 1.504(19) . ? C3D H3A 0.9700 . ? C3D H3B 0.9700 . ? C4D N3D 1.493(19) . ? C4D H2A 0.9700 . ? C4D H2B 0.9700 . ? N3D H33A 0.9000 . ? N3D H33B 0.9000 . ? N1A C2A 1.347(14) . ? N1A C6A 1.390(17) . ? N1A H1AA 0.8600 . ? C2A N3A 1.320(15) . ? C2A N2A 1.343(17) . ? N2A H2AA 0.8600 . ? N2A H2AB 0.8600 . ? N3A C4A 1.352(14) . ? C4A C5A 1.351(16) . ? C4A N9A 1.371(15) . ? C5A N7A 1.358(17) . ? C5A C6A 1.452(19) . ? C6A O6A 1.242(14) . ? N7A C8A 1.330(17) . ? N7A H7AA 0.8600 . ? C8A N9A 1.328(14) . ? C8A H8AA 0.9300 . ? N1DA C1DA 1.499(15) . ? N1DA H71A 0.9000 . ? N1DA H71B 0.9000 . ? C1DA C2DA 1.494(17) . ? C1DA H61A 0.9700 . ? C1DA H61B 0.9700 . ? C2DA N2DA 1.470(18) . ? C2DA H51A 0.9700 . ? C2DA H51B 0.9700 . ? N2DA C3DA 1.493(16) . ? N2DA H41A 0.9100 . ? C3DA C4DA 1.47(2) . ? C3DA H31A 0.9700 . ? C3DA H31B 0.9700 . ? C4DA N3DA 1.522(19) . ? C4DA H21A 0.9700 . ? C4DA H21B 0.9700 . ? N3DA H11A 0.9000 . ? N3DA H11B 0.9000 . ? N1B C2B 1.364(15) . ? N1B C6B 1.405(15) . ? N1B H1BA 0.8600 . ? C2B N3B 1.318(14) . ? C2B N2B 1.333(15) . ? N2B H2BA 0.8600 . ? N2B H2BB 0.8600 . ? N3B C4B 1.365(14) . ? C4B C5B 1.364(15) . ? C4B N9B 1.381(14) . ? C5B C6B 1.394(16) . ? C5B N7B 1.399(15) . ? C6B O6B 1.243(14) . ? N7B C8B 1.320(16) . ? N7B H7BA 0.8600 . ? C8B N9B 1.309(15) . ? C8B H8BA 0.9300 . ? Cl1 O14 1.399(12) . ? Cl1 O13 1.402(9) . ? Cl1 O12 1.424(9) . ? Cl1 O11 1.427(10) . ? Cl2 O21 1.394(11) . ? Cl2 O23 1.407(12) . ? Cl2 O24 1.407(14) . ? Cl2 O22 1.429(13) . ? Cl3 O31 1.390(7) . ? Cl3 O33 1.423(7) . ? Cl3 O34 1.425(8) . ? Cl3 O32 1.499(8) . ? Cl4 O41 1.409(8) . ? Cl4 O43 1.438(8) . ? Cl4 O44 1.457(9) . ? Cl4 O42 1.469(9) . ? O1W H1W 0.8500 . ? O1W H2W 0.8498 . ? O2W H3W 0.8498 . ? O2W H4W 0.8499 . ? O3W H5W 0.8100 . ? O4W H7W 0.8500 . ? O4W H8W 0.8501 . ? O5W H9W 0.8498 . ? O5W H10W 0.8501 . ? 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 N2D Pt1 N1D 84.4(4) . . ? N2D Pt1 N3D 83.9(4) . . ? N1D Pt1 N3D 167.5(4) . . ? N2D Pt1 N9A 178.4(4) . . ? N1D Pt1 N9A 96.6(4) . . ? N3D Pt1 N9A 95.2(4) . . ? N2DA Pt2 N1DA 83.8(4) . . ? N2DA Pt2 N9B 177.1(4) . . ? N1DA Pt2 N9B 96.0(4) . . ? N2DA Pt2 N3DA 84.4(5) . . ? N1DA Pt2 N3DA 167.1(4) . . ? N9B Pt2 N3DA 95.6(4) . . ? C1D N1D Pt1 108.9(7) . . ? C1D N1D H77A 109.9 . . ? Pt1 N1D H77A 109.9 . . ? C1D N1D H77B 109.9 . . ? Pt1 N1D H77B 109.9 . . ? H77A N1D H77B 108.3 . . ? C2D C1D N1D 109.6(11) . . ? C2D C1D H6A 109.8 . . ? N1D C1D H6A 109.8 . . ? C2D C1D H6B 109.8 . . ? N1D C1D H6B 109.8 . . ? H6A C1D H6B 108.2 . . ? N2D C2D C1D 106.1(11) . . ? N2D C2D H5A 110.5 . . ? C1D C2D H5A 110.5 . . ? N2D C2D H5B 110.5 . . ? C1D C2D H5B 110.5 . . ? H5A C2D H5B 108.7 . . ? C3D N2D C2D 118.7(11) . . ? C3D N2D Pt1 108.9(9) . . ? C2D N2D Pt1 108.6(8) . . ? C3D N2D H44A 106.7 . . ? C2D N2D H44A 106.7 . . ? Pt1 N2D H44A 106.7 . . ? N2D C3D C4D 105.7(11) . . ? N2D C3D H3A 110.6 . . ? C4D C3D H3A 110.6 . . ? N2D C3D H3B 110.6 . . ? C4D C3D H3B 110.6 . . ? H3A C3D H3B 108.7 . . ? N3D C4D C3D 109.3(12) . . ? N3D C4D H2A 109.8 . . ? C3D C4D H2A 109.8 . . ? N3D C4D H2B 109.8 . . ? C3D C4D H2B 109.8 . . ? H2A C4D H2B 108.3 . . ? C4D N3D Pt1 108.0(8) . . ? C4D N3D H33A 110.1 . . ? Pt1 N3D H33A 110.1 . . ? C4D N3D H33B 110.1 . . ? Pt1 N3D H33B 110.1 . . ? H33A N3D H33B 108.4 . . ? C2A N1A C6A 126.1(12) . . ? C2A N1A H1AA 116.9 . . ? C6A N1A H1AA 116.9 . . ? N3A C2A N2A 120.3(10) . . ? N3A C2A N1A 124.3(13) . . ? N2A C2A N1A 115.4(12) . . ? C2A N2A H2AA 120.0 . . ? C2A N2A H2AB 120.0 . . ? H2AA N2A H2AB 120.0 . . ? C2A N3A C4A 112.8(10) . . ? C5A C4A N3A 126.8(12) . . ? C5A C4A N9A 108.4(11) . . ? N3A C4A N9A 124.8(10) . . ? C4A C5A N7A 107.7(12) . . ? C4A C5A C6A 120.8(13) . . ? N7A C5A C6A 131.4(12) . . ? O6A C6A N1A 123.6(13) . . ? O6A C6A C5A 127.2(14) . . ? N1A C6A C5A 109.1(11) . . ? C8A N7A C5A 106.7(11) . . ? C8A N7A H7AA 126.6 . . ? C5A N7A H7AA 126.6 . . ? N9A C8A N7A 111.5(12) . . ? N9A C8A H8AA 124.3 . . ? N7A C8A H8AA 124.3 . . ? C8A N9A C4A 105.7(10) . . ? C8A N9A Pt1 126.4(9) . . ? C4A N9A Pt1 127.9(7) . . ? C1DA N1DA Pt2 109.9(7) . . ? C1DA N1DA H71A 109.7 . . ? Pt2 N1DA H71A 109.7 . . ? C1DA N1DA H71B 109.7 . . ? Pt2 N1DA H71B 109.7 . . ? H71A N1DA H71B 108.2 . . ? C2DA C1DA N1DA 107.2(10) . . ? C2DA C1DA H61A 110.3 . . ? N1DA C1DA H61A 110.3 . . ? C2DA C1DA H61B 110.3 . . ? N1DA C1DA H61B 110.3 . . ? H61A C1DA H61B 108.5 . . ? N2DA C2DA C1DA 107.9(11) . . ? N2DA C2DA H51A 110.1 . . ? C1DA C2DA H51A 110.1 . . ? N2DA C2DA H51B 110.1 . . ? C1DA C2DA H51B 110.1 . . ? H51A C2DA H51B 108.4 . . ? C2DA N2DA C3DA 116.7(12) . . ? C2DA N2DA Pt2 107.2(7) . . ? C3DA N2DA Pt2 106.2(9) . . ? C2DA N2DA H41A 108.8 . . ? C3DA N2DA H41A 108.8 . . ? Pt2 N2DA H41A 108.8 . . ? C4DA C3DA N2DA 108.2(14) . . ? C4DA C3DA H31A 110.1 . . ? N2DA C3DA H31A 110.1 . . ? C4DA C3DA H31B 110.1 . . ? N2DA C3DA H31B 110.1 . . ? H31A C3DA H31B 108.4 . . ? C3DA C4DA N3DA 109.2(12) . . ? C3DA C4DA H21A 109.8 . . ? N3DA C4DA H21A 109.8 . . ? C3DA C4DA H21B 109.8 . . ? N3DA C4DA H21B 109.8 . . ? H21A C4DA H21B 108.3 . . ? C4DA N3DA Pt2 108.3(9) . . ? C4DA N3DA H11A 110.0 . . ? Pt2 N3DA H11A 110.0 . . ? C4DA N3DA H11B 110.0 . . ? Pt2 N3DA H11B 110.0 . . ? H11A N3DA H11B 108.4 . . ? C2B N1B C6B 126.0(10) . . ? C2B N1B H1BA 117.0 . . ? C6B N1B H1BA 117.0 . . ? N3B C2B N2B 118.9(11) . . ? N3B C2B N1B 122.2(11) . . ? N2B C2B N1B 119.0(11) . . ? C2B N2B H2BA 120.0 . . ? C2B N2B H2BB 120.0 . . ? H2BA N2B H2BB 120.0 . . ? C2B N3B C4B 114.2(10) . . ? C5B C4B N3B 125.4(11) . . ? C5B C4B N9B 109.5(10) . . ? N3B C4B N9B 125.1(10) . . ? C4B C5B C6B 121.9(11) . . ? C4B C5B N7B 104.9(10) . . ? C6B C5B N7B 133.1(11) . . ? O6B C6B C5B 128.9(12) . . ? O6B C6B N1B 120.9(11) . . ? C5B C6B N1B 110.2(10) . . ? C8B N7B C5B 107.3(10) . . ? C8B N7B H7BA 126.3 . . ? C5B N7B H7BA 126.3 . . ? N9B C8B N7B 112.6(12) . . ? N9B C8B H8BA 123.7 . . ? N7B C8B H8BA 123.7 . . ? C8B N9B C4B 105.7(10) . . ? C8B N9B Pt2 129.2(9) . . ? C4B N9B Pt2 125.1(8) . . ? O14 Cl1 O13 107.9(8) . . ? O14 Cl1 O12 108.8(7) . . ? O13 Cl1 O12 109.6(8) . . ? O14 Cl1 O11 110.6(8) . . ? O13 Cl1 O11 108.9(7) . . ? O12 Cl1 O11 111.0(6) . . ? O21 Cl2 O23 109.4(9) . . ? O21 Cl2 O24 109.1(10) . . ? O23 Cl2 O24 110.4(10) . . ? O21 Cl2 O22 110.1(8) . . ? O23 Cl2 O22 107.2(10) . . ? O24 Cl2 O22 110.7(10) . . ? O31 Cl3 O33 114.7(7) . . ? O31 Cl3 O34 112.9(7) . . ? O33 Cl3 O34 110.7(7) . . ? O31 Cl3 O32 107.2(7) . . ? O33 Cl3 O32 104.4(7) . . ? O34 Cl3 O32 106.1(7) . . ? O41 Cl4 O43 112.8(8) . . ? O41 Cl4 O44 111.9(8) . . ? O43 Cl4 O44 108.9(8) . . ? O41 Cl4 O42 109.4(8) . . ? O43 Cl4 O42 107.2(7) . . ? O44 Cl4 O42 106.2(8) . . ? H1W O1W H2W 107.7 . . ? H3W O2W H4W 107.7 . . ? H7W O4W H8W 107.7 . . ? H9W O5W H10W 107.7 . . ? 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 N2D Pt1 N1D C1D 2.9(9) . . . . ? N3D Pt1 N1D C1D 23(2) . . . . ? N9A Pt1 N1D C1D -175.9(9) . . . . ? Pt1 N1D C1D C2D -29.8(14) . . . . ? N1D C1D C2D N2D 49.9(15) . . . . ? C1D C2D N2D C3D -171.6(12) . . . . ? C1D C2D N2D Pt1 -46.6(13) . . . . ? N1D Pt1 N2D C3D 155.2(9) . . . . ? N3D Pt1 N2D C3D -20.6(9) . . . . ? N1D Pt1 N2D C2D 24.5(9) . . . . ? N3D Pt1 N2D C2D -151.3(10) . . . . ? C2D N2D C3D C4D 169.9(13) . . . . ? Pt1 N2D C3D C4D 45.0(15) . . . . ? N2D C3D C4D N3D -53.6(18) . . . . ? C3D C4D N3D Pt1 36.2(16) . . . . ? N2D Pt1 N3D C4D -8.6(9) . . . . ? N1D Pt1 N3D C4D -29(2) . . . . ? N9A Pt1 N3D C4D 170.1(9) . . . . ? C6A N1A C2A N3A -0.8(18) . . . . ? C6A N1A C2A N2A -177.7(10) . . . . ? N2A C2A N3A C4A 177.4(10) . . . . ? N1A C2A N3A C4A 0.6(15) . . . . ? C2A N3A C4A C5A 1.1(15) . . . . ? C2A N3A C4A N9A 179.6(10) . . . . ? N3A C4A C5A N7A 179.4(10) . . . . ? N9A C4A C5A N7A 0.7(12) . . . . ? N3A C4A C5A C6A -2.6(17) . . . . ? N9A C4A C5A C6A 178.7(9) . . . . ? C2A N1A C6A O6A 178.1(10) . . . . ? C2A N1A C6A C5A -0.6(15) . . . . ? C4A C5A C6A O6A -176.6(11) . . . . ? N7A C5A C6A O6A 1(2) . . . . ? C4A C5A C6A N1A 2.1(14) . . . . ? N7A C5A C6A N1A 179.6(12) . . . . ? C4A C5A N7A C8A -0.1(13) . . . . ? C6A C5A N7A C8A -177.8(11) . . . . ? C5A N7A C8A N9A -0.6(13) . . . . ? N7A C8A N9A C4A 1.1(12) . . . . ? N7A C8A N9A Pt1 -178.2(7) . . . . ? C5A C4A N9A C8A -1.1(12) . . . . ? N3A C4A N9A C8A -179.8(10) . . . . ? C5A C4A N9A Pt1 178.1(7) . . . . ? N3A C4A N9A Pt1 -0.6(15) . . . . ? N1D Pt1 N9A C8A -152.6(9) . . . . ? N3D Pt1 N9A C8A 23.4(9) . . . . ? N1D Pt1 N9A C4A 28.3(9) . . . . ? N3D Pt1 N9A C4A -155.6(9) . . . . ? N2DA Pt2 N1DA C1DA -5.2(7) . . . . ? N9B Pt2 N1DA C1DA 177.7(7) . . . . ? N3DA Pt2 N1DA C1DA -29(2) . . . . ? Pt2 N1DA C1DA C2DA 32.1(12) . . . . ? N1DA C1DA C2DA N2DA -52.6(13) . . . . ? C1DA C2DA N2DA C3DA 166.5(11) . . . . ? C1DA C2DA N2DA Pt2 47.7(11) . . . . ? N1DA Pt2 N2DA C2DA -23.2(8) . . . . ? N3DA Pt2 N2DA C2DA 151.6(8) . . . . ? N1DA Pt2 N2DA C3DA -148.6(10) . . . . ? N3DA Pt2 N2DA C3DA 26.2(9) . . . . ? C2DA N2DA C3DA C4DA -168.7(12) . . . . ? Pt2 N2DA C3DA C4DA -49.3(13) . . . . ? N2DA C3DA C4DA N3DA 51.3(16) . . . . ? C3DA C4DA N3DA Pt2 -27.9(15) . . . . ? N2DA Pt2 N3DA C4DA 0.4(9) . . . . ? N1DA Pt2 N3DA C4DA 24(2) . . . . ? N9B Pt2 N3DA C4DA 177.5(9) . . . . ? C6B N1B C2B N3B 3.1(16) . . . . ? C6B N1B C2B N2B -177.6(10) . . . . ? N2B C2B N3B C4B 179.7(9) . . . . ? N1B C2B N3B C4B -1.0(14) . . . . ? C2B N3B C4B C5B -1.5(14) . . . . ? C2B N3B C4B N9B -179.2(9) . . . . ? N3B C4B C5B C6B 2.1(15) . . . . ? N9B C4B C5B C6B -179.9(9) . . . . ? N3B C4B C5B N7B -177.7(9) . . . . ? N9B C4B C5B N7B 0.4(11) . . . . ? C4B C5B C6B O6B 179.1(10) . . . . ? N7B C5B C6B O6B -1.2(19) . . . . ? C4B C5B C6B N1B -0.1(13) . . . . ? N7B C5B C6B N1B 179.5(10) . . . . ? C2B N1B C6B O6B 178.4(10) . . . . ? C2B N1B C6B C5B -2.3(14) . . . . ? C4B C5B N7B C8B -0.8(11) . . . . ? C6B C5B N7B C8B 179.5(11) . . . . ? C5B N7B C8B N9B 1.0(13) . . . . ? N7B C8B N9B C4B -0.8(13) . . . . ? N7B C8B N9B Pt2 -178.2(7) . . . . ? C5B C4B N9B C8B 0.2(11) . . . . ? N3B C4B N9B C8B 178.3(10) . . . . ? C5B C4B N9B Pt2 177.8(7) . . . . ? N3B C4B N9B Pt2 -4.1(14) . . . . ? N1DA Pt2 N9B C8B -144.9(10) . . . . ? N3DA Pt2 N9B C8B 40.9(10) . . . . ? N1DA Pt2 N9B C4B 38.2(8) . . . . ? N3DA Pt2 N9B C4B -136.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.327 _refine_diff_density_min -1.948 _refine_diff_density_rms 0.213 # Attachment '2500.CIF' # The compound referred in the manuscript as complex 6. data_2500 _database_code_depnum_ccdc_archive 'CCDC 731733' _audit_creation_method SHELXL-97 _publ_section_title_footnote ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H19 Cl2 N9 O Pt2, 3(H2 O), 2(Cl)' _chemical_formula_sum 'C6 H25 Cl4 N9 O4 Pt2' _chemical_formula_weight 819.33 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.525(3) _cell_length_b 17.095(3) _cell_length_c 19.292(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.15(3) _cell_angle_gamma 90.00 _cell_volume 4187.5(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4802 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needles _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 13.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1095 _exptl_absorpt_correction_T_max 0.249 _exptl_absorpt_process_details 'SADABS, Sheldrick, Bruker, 2000' _exptl_special_details ; It was not possible to locate hydrogens on one of the three solvent molecules i.e. O3W. EADP constraint was used to model disordered C2. ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16033 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4802 _reflns_number_gt 2982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0461P)^2^+71.9711P] 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 4802 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1228 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 -0.22297(4) 0.04736(3) -0.47796(3) 0.03975(18) Uani 1 1 d . . . N11 N -0.3436(9) -0.0311(7) -0.5052(7) 0.055(3) Uani 1 1 d . . . H11A H -0.3662 -0.0369 -0.4673 0.066 Uiso 1 1 calc R . . H11B H -0.3211 -0.0770 -0.5159 0.066 Uiso 1 1 calc R . . H11C H -0.3961 -0.0138 -0.5443 0.066 Uiso 1 1 calc R . . N12 N -0.3253(9) 0.1364(6) -0.4794(6) 0.047(3) Uani 1 1 d . . . H11D H -0.3215 0.1472 -0.4335 0.056 Uiso 1 1 calc R . . H11E H -0.3907 0.1218 -0.5058 0.056 Uiso 1 1 calc R . . H11F H -0.3082 0.1787 -0.4997 0.056 Uiso 1 1 calc R . . Pt2 Pt -0.22636(4) 0.10891(3) -0.63322(3) 0.04170(18) Uani 1 1 d . . . N13 N -0.3596(9) 0.0527(8) -0.6949(7) 0.058(3) Uani 1 1 d . . . H11G H -0.3730 0.0632 -0.7424 0.070 Uiso 1 1 calc R . . H11H H -0.4132 0.0688 -0.6818 0.070 Uiso 1 1 calc R . . H11I H -0.3510 0.0014 -0.6875 0.070 Uiso 1 1 calc R . . N14 N -0.1430(10) 0.0095(7) -0.6337(6) 0.052(3) Uani 1 1 d . . . H11J H -0.1635 -0.0101 -0.6792 0.063 Uiso 1 1 calc R . . H11K H -0.1546 -0.0255 -0.6031 0.063 Uiso 1 1 calc R . . H11L H -0.0746 0.0207 -0.6189 0.063 Uiso 1 1 calc R . . N1 N 0.0479(10) 0.2527(7) -0.5585(7) 0.056(3) Uani 1 1 d . . . H1B H 0.0767 0.2827 -0.5819 0.067 Uiso 1 1 d R . . N2 N -0.0619(11) 0.2145(8) -0.6742(7) 0.067(4) Uani 1 1 d . . . H1 H -0.0251 0.2428 -0.6931 0.080 Uiso 1 1 d R . . H2 H -0.1149 0.1885 -0.7024 0.080 Uiso 1 1 d R . . N3 N -0.0938(9) 0.1685(6) -0.5707(6) 0.044(3) Uani 1 1 d . . . C2 C -0.0344(10) 0.2111(8) -0.5972(9) 0.044(3) Uani 1 1 d . . . C4 C -0.0591(11) 0.1664(7) -0.4957(7) 0.038(3) Uani 1 1 d . . . C5 C 0.0294(10) 0.2074(8) -0.4510(9) 0.044(3) Uani 1 1 d . . . C6 C 0.0926(13) 0.2533(8) -0.4834(8) 0.051(4) Uani 1 1 d . . . O6 O 0.1713(8) 0.2911(6) -0.4495(6) 0.060(3) Uani 1 1 d . . . N7 N 0.0397(10) 0.1860(7) -0.3783(6) 0.047(3) Uani 1 1 d . . . C7 C 0.1174(13) 0.2206(9) -0.3127(8) 0.058(4) Uani 1 1 d . . . H3 H 0.1109 0.1972 -0.2692 0.086 Uiso 1 1 calc R . . H4 H 0.1054 0.2759 -0.3122 0.086 Uiso 1 1 calc R . . H5 H 0.1869 0.2113 -0.3137 0.086 Uiso 1 1 calc R . . C8 C -0.0331(9) 0.1422(7) -0.3859(6) 0.027(3) Uani 1 1 d . . . H8B H -0.0426 0.1206 -0.3445 0.032 Uiso 1 1 calc R . . N9 N -0.0987(9) 0.1248(7) -0.4514(7) 0.050(3) Uani 1 1 d . . . Cl1 Cl -0.1100(3) -0.0559(2) -0.4663(2) 0.0614(11) Uani 1 1 d . . . Cl2 Cl -0.3225(3) 0.2197(2) -0.6331(2) 0.0577(10) Uani 1 1 d . . . Cl3 Cl -0.0462(3) 0.4298(3) -0.1205(2) 0.0608(11) Uani 1 1 d . . . Cl4 Cl -0.3646(4) 0.1407(3) -0.1654(3) 0.0885(15) Uani 1 1 d . . . O1W O -0.3624(12) 0.0992(7) -0.3375(8) 0.098(4) Uani 1 1 d . . . H1W H -0.2991 0.0827 -0.3069 0.147 Uiso 1 1 d R . . H2W H -0.4015 0.0554 -0.3433 0.147 Uiso 1 1 d R . . O2W O -0.3134(11) 0.3683(9) -0.1823(7) 0.101(5) Uani 1 1 d . . . H3W H -0.2970 0.3551 -0.1345 0.151 Uiso 1 1 d R . . H4W H -0.3232 0.4167 -0.1923 0.151 Uiso 1 1 d R . . O3W O -0.1516(13) -0.0393(9) -0.7815(8) 0.107(5) 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 0.0316(3) 0.0470(3) 0.0413(3) -0.0008(2) 0.0135(2) 0.0048(3) N11 0.047(8) 0.056(8) 0.059(8) 0.004(6) 0.013(6) -0.004(6) N12 0.042(7) 0.041(7) 0.054(8) 0.000(5) 0.012(6) 0.010(6) Pt2 0.0340(3) 0.0522(4) 0.0369(3) -0.0038(2) 0.0097(2) 0.0064(3) N13 0.041(7) 0.084(10) 0.052(8) -0.012(7) 0.018(6) 0.008(7) N14 0.057(8) 0.045(7) 0.050(7) -0.009(6) 0.013(6) 0.016(6) N1 0.060(9) 0.063(8) 0.046(8) 0.013(6) 0.019(6) 0.004(7) N2 0.067(9) 0.083(10) 0.055(9) -0.008(7) 0.025(7) -0.022(8) N3 0.056(8) 0.041(7) 0.032(6) -0.001(5) 0.013(6) 0.021(6) C2 0.023(5) 0.034(6) 0.078(8) -0.010(5) 0.021(5) -0.002(4) C4 0.043(8) 0.032(7) 0.049(9) 0.013(6) 0.028(7) 0.014(6) C5 0.023(5) 0.034(6) 0.078(8) -0.010(5) 0.021(5) -0.002(4) C6 0.057(10) 0.039(8) 0.058(10) -0.016(7) 0.021(8) 0.016(8) O6 0.045(6) 0.069(7) 0.064(7) -0.013(6) 0.015(6) -0.012(6) N7 0.064(9) 0.047(7) 0.023(6) 0.001(5) 0.007(6) 0.022(7) C7 0.063(10) 0.060(10) 0.044(9) -0.006(7) 0.011(8) -0.001(8) C8 0.012(6) 0.043(8) 0.019(6) -0.017(5) -0.004(5) 0.007(6) N9 0.040(7) 0.046(7) 0.062(8) 0.001(6) 0.016(6) 0.009(6) Cl1 0.043(2) 0.056(2) 0.086(3) -0.005(2) 0.023(2) 0.0094(19) Cl2 0.056(2) 0.058(2) 0.054(2) 0.0029(18) 0.0121(19) 0.019(2) Cl3 0.045(2) 0.082(3) 0.054(2) 0.000(2) 0.0161(19) -0.003(2) Cl4 0.101(4) 0.091(4) 0.090(4) -0.012(3) 0.053(3) -0.008(3) O1W 0.125(12) 0.074(9) 0.114(11) -0.001(8) 0.065(10) 0.000(8) O2W 0.091(10) 0.135(12) 0.059(8) 0.004(8) 0.003(7) -0.006(9) O3W 0.118(13) 0.132(12) 0.078(10) -0.008(8) 0.043(9) 0.009(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 Pt1 N11 2.036(11) . ? Pt1 N12 2.051(10) . ? Pt1 N9 2.060(12) . ? Pt1 Cl1 2.294(4) . ? Pt1 Pt2 3.1601(10) . ? N11 H11A 0.8900 . ? N11 H11B 0.8900 . ? N11 H11C 0.8900 . ? N12 H11D 0.8900 . ? N12 H11E 0.8900 . ? N12 H11F 0.8900 . ? Pt2 N13 2.027(12) . ? Pt2 N14 2.041(11) . ? Pt2 N3 2.054(12) . ? Pt2 Cl2 2.299(4) . ? N13 H11G 0.8900 . ? N13 H11H 0.8900 . ? N13 H11I 0.8900 . ? N14 H11J 0.8900 . ? N14 H11K 0.8900 . ? N14 H11L 0.8900 . ? N1 C2 1.315(17) . ? N1 C6 1.365(18) . ? N1 H1B 0.8600 . ? N2 C2 1.402(19) . ? N2 H1 0.8601 . ? N2 H2 0.8599 . ? N3 C2 1.311(17) . ? N3 C4 1.360(16) . ? C4 N9 1.355(16) . ? C4 C5 1.399(19) . ? C5 N7 1.409(18) . ? C5 C6 1.45(2) . ? C6 O6 1.224(17) . ? N7 C8 1.204(16) . ? N7 C7 1.463(18) . ? C7 H3 0.9600 . ? C7 H4 0.9600 . ? C7 H5 0.9600 . ? C8 N9 1.304(15) . ? C8 H8B 0.9300 . ? O1W H1W 0.9014 . ? O1W H2W 0.9017 . ? O2W H3W 0.9002 . ? O2W H4W 0.8501 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pt1 N12 90.5(5) . . ? N11 Pt1 N9 178.5(5) . . ? N12 Pt1 N9 90.9(5) . . ? N11 Pt1 Cl1 88.0(4) . . ? N12 Pt1 Cl1 174.7(3) . . ? N9 Pt1 Cl1 90.6(3) . . ? N11 Pt1 Pt2 103.1(4) . . ? N12 Pt1 Pt2 87.2(3) . . ? N9 Pt1 Pt2 76.5(3) . . ? Cl1 Pt1 Pt2 98.10(11) . . ? Pt1 N11 H11A 109.5 . . ? Pt1 N11 H11B 109.5 . . ? H11A N11 H11B 109.5 . . ? Pt1 N11 H11C 109.5 . . ? H11A N11 H11C 109.5 . . ? H11B N11 H11C 109.5 . . ? Pt1 N12 H11D 109.5 . . ? Pt1 N12 H11E 109.5 . . ? H11D N12 H11E 109.5 . . ? Pt1 N12 H11F 109.5 . . ? H11D N12 H11F 109.5 . . ? H11E N12 H11F 109.5 . . ? N13 Pt2 N14 89.0(5) . . ? N13 Pt2 N3 178.4(4) . . ? N14 Pt2 N3 92.5(5) . . ? N13 Pt2 Cl2 90.2(4) . . ? N14 Pt2 Cl2 179.1(4) . . ? N3 Pt2 Cl2 88.3(3) . . ? N13 Pt2 Pt1 96.8(4) . . ? N14 Pt2 Pt1 84.2(3) . . ? N3 Pt2 Pt1 83.3(3) . . ? Cl2 Pt2 Pt1 95.55(10) . . ? Pt2 N13 H11G 109.5 . . ? Pt2 N13 H11H 109.5 . . ? H11G N13 H11H 109.5 . . ? Pt2 N13 H11I 109.5 . . ? H11G N13 H11I 109.5 . . ? H11H N13 H11I 109.5 . . ? Pt2 N14 H11J 109.5 . . ? Pt2 N14 H11K 109.5 . . ? H11J N14 H11K 109.5 . . ? Pt2 N14 H11L 109.5 . . ? H11J N14 H11L 109.5 . . ? H11K N14 H11L 109.5 . . ? C2 N1 C6 125.8(14) . . ? C2 N1 H1B 118.1 . . ? C6 N1 H1B 116.0 . . ? C2 N2 H1 119.5 . . ? C2 N2 H2 120.5 . . ? H1 N2 H2 120.0 . . ? C2 N3 C4 113.4(12) . . ? C2 N3 Pt2 125.1(10) . . ? C4 N3 Pt2 121.5(10) . . ? N3 C2 N1 126.2(15) . . ? N3 C2 N2 117.5(13) . . ? N1 C2 N2 116.3(13) . . ? N9 C4 N3 128.2(13) . . ? N9 C4 C5 108.4(12) . . ? N3 C4 C5 123.4(12) . . ? C4 C5 N7 104.6(12) . . ? C4 C5 C6 120.9(14) . . ? N7 C5 C6 134.3(13) . . ? O6 C6 N1 123.7(15) . . ? O6 C6 C5 126.2(14) . . ? N1 C6 C5 110.0(14) . . ? C8 N7 C5 104.2(11) . . ? C8 N7 C7 132.0(12) . . ? C5 N7 C7 123.4(13) . . ? N7 C7 H3 109.5 . . ? N7 C7 H4 109.5 . . ? H3 C7 H4 109.5 . . ? N7 C7 H5 109.5 . . ? H3 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? N7 C8 N9 121.0(13) . . ? N7 C8 H8B 119.5 . . ? N9 C8 H8B 119.5 . . ? C8 N9 C4 101.8(12) . . ? C8 N9 Pt1 127.8(10) . . ? C4 N9 Pt1 130.3(10) . . ? H1W O1W H2W 101.8 . . ? H3W O2W H4W 116.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Pt1 Pt2 N13 6.2(5) . . . . ? N12 Pt1 Pt2 N13 -83.6(5) . . . . ? N9 Pt1 Pt2 N13 -175.3(5) . . . . ? Cl1 Pt1 Pt2 N13 96.0(4) . . . . ? N11 Pt1 Pt2 N14 -82.1(5) . . . . ? N12 Pt1 Pt2 N14 -172.0(5) . . . . ? N9 Pt1 Pt2 N14 96.4(5) . . . . ? Cl1 Pt1 Pt2 N14 7.7(4) . . . . ? N11 Pt1 Pt2 N3 -175.4(5) . . . . ? N12 Pt1 Pt2 N3 94.8(4) . . . . ? N9 Pt1 Pt2 N3 3.2(4) . . . . ? Cl1 Pt1 Pt2 N3 -85.5(3) . . . . ? N11 Pt1 Pt2 Cl2 97.0(4) . . . . ? N12 Pt1 Pt2 Cl2 7.2(3) . . . . ? N9 Pt1 Pt2 Cl2 -84.5(3) . . . . ? Cl1 Pt1 Pt2 Cl2 -173.14(15) . . . . ? N14 Pt2 N3 C2 91.5(11) . . . . ? Cl2 Pt2 N3 C2 -88.8(10) . . . . ? Pt1 Pt2 N3 C2 175.4(10) . . . . ? N14 Pt2 N3 C4 -88.0(10) . . . . ? Cl2 Pt2 N3 C4 91.6(9) . . . . ? Pt1 Pt2 N3 C4 -4.2(9) . . . . ? C4 N3 C2 N1 -3.9(19) . . . . ? Pt2 N3 C2 N1 176.6(10) . . . . ? C4 N3 C2 N2 177.8(11) . . . . ? Pt2 N3 C2 N2 -1.7(17) . . . . ? C6 N1 C2 N3 7(2) . . . . ? C6 N1 C2 N2 -174.9(13) . . . . ? C2 N3 C4 N9 -176.0(12) . . . . ? Pt2 N3 C4 N9 3.5(17) . . . . ? C2 N3 C4 C5 1.9(17) . . . . ? Pt2 N3 C4 C5 -178.6(9) . . . . ? N9 C4 C5 N7 1.0(14) . . . . ? N3 C4 C5 N7 -177.3(11) . . . . ? N9 C4 C5 C6 175.9(11) . . . . ? N3 C4 C5 C6 -2.4(19) . . . . ? C2 N1 C6 O6 177.6(13) . . . . ? C2 N1 C6 C5 -6.2(19) . . . . ? C4 C5 C6 O6 -179.9(13) . . . . ? N7 C5 C6 O6 -7(2) . . . . ? C4 C5 C6 N1 4.1(17) . . . . ? N7 C5 C6 N1 177.2(14) . . . . ? C4 C5 N7 C8 -0.8(13) . . . . ? C6 C5 N7 C8 -174.7(14) . . . . ? C4 C5 N7 C7 -174.6(12) . . . . ? C6 C5 N7 C7 12(2) . . . . ? C5 N7 C8 N9 0.4(16) . . . . ? C7 N7 C8 N9 173.4(13) . . . . ? N7 C8 N9 C4 0.2(15) . . . . ? N7 C8 N9 Pt1 176.4(9) . . . . ? N3 C4 N9 C8 177.4(12) . . . . ? C5 C4 N9 C8 -0.7(13) . . . . ? N3 C4 N9 Pt1 1.4(19) . . . . ? C5 C4 N9 Pt1 -176.8(9) . . . . ? N12 Pt1 N9 C8 94.7(11) . . . . ? Cl1 Pt1 N9 C8 -80.3(11) . . . . ? Pt2 Pt1 N9 C8 -178.4(11) . . . . ? N12 Pt1 N9 C4 -90.2(11) . . . . ? Cl1 Pt1 N9 C4 94.8(11) . . . . ? Pt2 Pt1 N9 C4 -3.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.179 _refine_diff_density_min -1.719 _refine_diff_density_rms 0.260 # Attachment '2600.CIF' # The compound referred in the manuscript as complex 4. data_2600 _database_code_depnum_ccdc_archive 'CCDC 731734' _audit_creation_method SHELXL-97 _publ_section_title_footnote ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H20 Cl N9 O8 Pt' _chemical_formula_sum 'C10 H20 Cl N9 O8 Pt' _chemical_formula_weight 624.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9590(14) _cell_length_b 11.946(2) _cell_length_c 11.964(2) _cell_angle_alpha 97.76(3) _cell_angle_beta 96.47(3) _cell_angle_gamma 92.56(3) _cell_volume 977.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4347 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description Needles _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 7.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1919 _exptl_absorpt_correction_T_max 0.478 _exptl_absorpt_process_details 'SADABS, Sheldrick, Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7550 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4347 _reflns_number_gt 3715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _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^)+(0.0466P)^2^+1.8368P] 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 4347 _refine_ls_number_parameters 256 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.061 _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 0.21863(4) 0.21933(2) 0.78264(2) 0.03787(11) Uani 1 1 d . . . N1D N 0.2628(11) 0.3023(5) 0.9449(5) 0.0504(15) Uani 1 1 d . . . H1FA H 0.1843 0.2711 0.9886 0.060 Uiso 1 1 calc R . . H1FB H 0.3864 0.2980 0.9749 0.060 Uiso 1 1 calc R . . N2D N 0.1959(10) 0.3755(5) 0.7404(5) 0.0471(14) Uani 1 1 d . . . H2FA H 0.0680 0.3894 0.7305 0.057 Uiso 1 1 calc R . . N3D N 0.2037(12) 0.1708(6) 0.6110(5) 0.0554(17) Uani 1 1 d . . . H3FA H 0.3136 0.1391 0.5940 0.066 Uiso 1 1 calc R . . H3FB H 0.1039 0.1193 0.5875 0.066 Uiso 1 1 calc R . . C1D C 0.2193(16) 0.4226(7) 0.9397(7) 0.064(2) Uani 1 1 d . . . H1DA H 0.0808 0.4308 0.9368 0.077 Uiso 1 1 calc R . . H1DB H 0.2832 0.4706 1.0067 0.077 Uiso 1 1 calc R . . C2D C 0.2911(15) 0.4562(7) 0.8355(8) 0.064(2) Uani 1 1 d . . . H2DA H 0.2580 0.5327 0.8263 0.077 Uiso 1 1 calc R . . H2DB H 0.4307 0.4527 0.8401 0.077 Uiso 1 1 calc R . . C3D C 0.2738(16) 0.3745(7) 0.6284(7) 0.063(2) Uani 1 1 d . . . H3DA H 0.2457 0.4436 0.5971 0.076 Uiso 1 1 calc R . . H3DB H 0.4130 0.3683 0.6375 0.076 Uiso 1 1 calc R . . C4D C 0.1756(18) 0.2740(8) 0.5519(7) 0.073(3) Uani 1 1 d . . . H4DA H 0.2311 0.2642 0.4806 0.087 Uiso 1 1 calc R . . H4DB H 0.0385 0.2850 0.5357 0.087 Uiso 1 1 calc R . . N1 N 0.2567(9) -0.0810(5) 1.1063(5) 0.0434(13) Uani 1 1 d . . . H1AA H 0.2581 -0.1107 1.1679 0.052 Uiso 1 1 calc R . . N2 N 0.2024(10) 0.0857(6) 1.2156(6) 0.0556(16) Uani 1 1 d . . . H2AA H 0.1802 0.1564 1.2243 0.067 Uiso 1 1 calc R . . H2AB H 0.2086 0.0491 1.2730 0.067 Uiso 1 1 calc R . . C2 C 0.2270(10) 0.0326(6) 1.1131(6) 0.0427(15) Uani 1 1 d . . . N3 N 0.2174(8) 0.0881(5) 1.0259(5) 0.0401(13) Uani 1 1 d . . . C4 C 0.2457(9) 0.0232(6) 0.9277(6) 0.0363(14) Uani 1 1 d . . . C5 C 0.2754(10) -0.0906(6) 0.9142(6) 0.0386(14) Uani 1 1 d . . . C6 C 0.2845(10) -0.1510(6) 1.0090(7) 0.0468(17) Uani 1 1 d . . . O6 O 0.3168(10) -0.2511(5) 1.0113(5) 0.0638(15) Uani 1 1 d . . . N7 N 0.2937(9) -0.1221(5) 0.8015(5) 0.0419(13) Uani 1 1 d . . . C7 C 0.3285(14) -0.2357(6) 0.7468(8) 0.059(2) Uani 1 1 d . . . H7A H 0.3365 -0.2341 0.6675 0.088 Uiso 1 1 calc R . . H7B H 0.2239 -0.2877 0.7555 0.088 Uiso 1 1 calc R . . H7C H 0.4479 -0.2596 0.7818 0.088 Uiso 1 1 calc R . . C8 C 0.2747(11) -0.0304(6) 0.7509(6) 0.0421(15) Uani 1 1 d . . . H8 H 0.2806 -0.0295 0.6737 0.050 Uiso 1 1 calc R . . N9 N 0.2458(8) 0.0609(5) 0.8241(4) 0.0374(9) Uani 1 1 d . . . Cl1 Cl -0.2013(3) 0.57145(17) 0.71699(18) 0.0559(5) Uani 1 1 d . . . O11 O -0.2096(12) 0.4718(6) 0.7691(7) 0.086(2) Uani 1 1 d . . . O12 O -0.3824(11) 0.5843(8) 0.6539(8) 0.100(3) Uani 1 1 d . . . O13 O -0.1526(16) 0.6665(7) 0.8032(8) 0.115(3) Uani 1 1 d . . . O14 O -0.0531(11) 0.5641(7) 0.6442(7) 0.087(2) Uani 1 1 d . . . N20 N 0.6971(8) 0.1117(6) 0.5777(4) 0.0374(9) Uani 1 1 d D . . O21 O 0.6313(13) 0.1217(9) 0.6662(7) 0.115(3) Uani 1 1 d . . . O22 O 0.8250(13) 0.0391(8) 0.5682(9) 0.124(4) Uani 1 1 d . . . O23 O 0.5900(18) 0.1320(11) 0.4930(9) 0.181(6) Uani 1 1 d 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 0.05069(19) 0.02981(15) 0.03392(16) 0.00636(10) 0.00404(11) 0.00831(10) N1D 0.076(4) 0.038(3) 0.037(3) 0.003(3) 0.003(3) 0.012(3) N2D 0.062(4) 0.041(3) 0.040(3) 0.009(3) 0.006(3) 0.009(3) N3D 0.090(5) 0.038(3) 0.038(3) 0.006(3) 0.003(3) 0.013(3) C1D 0.110(7) 0.036(4) 0.045(5) 0.003(3) 0.004(4) 0.019(4) C2D 0.096(7) 0.032(4) 0.060(5) 0.008(4) -0.007(5) 0.001(4) C3D 0.108(7) 0.043(4) 0.041(4) 0.010(4) 0.019(4) -0.005(4) C4D 0.132(9) 0.051(5) 0.038(4) 0.016(4) 0.006(5) 0.022(5) N1 0.051(3) 0.046(3) 0.035(3) 0.014(3) 0.003(2) 0.007(3) N2 0.077(5) 0.051(4) 0.040(4) 0.006(3) 0.006(3) 0.008(3) C2 0.041(4) 0.046(4) 0.041(4) 0.007(3) 0.004(3) 0.001(3) N3 0.045(3) 0.039(3) 0.037(3) 0.006(2) 0.004(2) 0.010(2) C4 0.038(3) 0.035(3) 0.037(3) 0.009(3) 0.004(3) 0.006(3) C5 0.041(4) 0.042(4) 0.034(3) 0.008(3) 0.003(3) 0.005(3) C6 0.047(4) 0.041(4) 0.054(5) 0.016(3) 0.000(3) 0.005(3) O6 0.097(4) 0.039(3) 0.058(4) 0.017(3) 0.007(3) 0.010(3) N7 0.053(3) 0.033(3) 0.041(3) 0.005(2) 0.008(3) 0.007(2) C7 0.085(6) 0.031(4) 0.064(5) 0.008(4) 0.024(4) 0.009(4) C8 0.057(4) 0.034(4) 0.038(4) 0.012(3) 0.008(3) 0.006(3) N9 0.036(2) 0.060(3) 0.0157(16) -0.0016(16) 0.0064(14) 0.0073(18) Cl1 0.0724(13) 0.0451(10) 0.0530(11) 0.0091(8) 0.0118(9) 0.0170(9) O11 0.115(6) 0.062(4) 0.090(5) 0.032(4) 0.017(4) 0.015(4) O12 0.079(5) 0.111(7) 0.116(7) 0.031(5) 0.006(4) 0.030(4) O13 0.179(9) 0.067(5) 0.090(6) -0.016(4) 0.012(6) 0.020(5) O14 0.093(5) 0.094(6) 0.082(5) 0.024(4) 0.029(4) 0.028(4) N20 0.036(2) 0.060(3) 0.0157(16) -0.0016(16) 0.0064(14) 0.0073(18) O21 0.119(7) 0.180(10) 0.062(5) 0.042(5) 0.023(4) 0.075(7) O22 0.095(6) 0.114(7) 0.140(9) -0.054(6) 0.017(5) -0.016(5) O23 0.280(17) 0.140(10) 0.153(12) 0.035(9) 0.128(12) 0.049(11) _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 N2D 2.006(6) . ? Pt1 N9 2.031(6) . ? Pt1 N1D 2.041(6) . ? Pt1 N3D 2.047(6) . ? N1D C1D 1.490(9) . ? N1D H1FA 0.9000 . ? N1D H1FB 0.9000 . ? N2D C2D 1.463(11) . ? N2D C3D 1.500(10) . ? N2D H2FA 0.9100 . ? N3D C4D 1.512(10) . ? N3D H3FA 0.9000 . ? N3D H3FB 0.9000 . ? C1D C2D 1.491(13) . ? C1D H1DA 0.9700 . ? C1D H1DB 0.9700 . ? C2D H2DA 0.9700 . ? C2D H2DB 0.9700 . ? C3D C4D 1.495(13) . ? C3D H3DA 0.9700 . ? C3D H3DB 0.9700 . ? C4D H4DA 0.9700 . ? C4D H4DB 0.9700 . ? N1 C2 1.374(9) . ? N1 C6 1.376(10) . ? N1 H1AA 0.8600 . ? N2 C2 1.336(9) . ? N2 H2AA 0.8600 . ? N2 H2AB 0.8600 . ? C2 N3 1.307(9) . ? N3 C4 1.356(9) . ? C4 N9 1.375(8) . ? C4 C5 1.374(9) . ? C5 N7 1.371(9) . ? C5 C6 1.421(9) . ? C6 O6 1.231(9) . ? N7 C8 1.326(9) . ? N7 C7 1.467(9) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N9 1.341(9) . ? C8 H8 0.9300 . ? Cl1 O11 1.419(7) . ? Cl1 O14 1.421(7) . ? Cl1 O12 1.420(8) . ? Cl1 O13 1.428(8) . ? N20 O21 1.194(9) . ? N20 O23 1.246(9) . ? N20 O22 1.273(11) . ? 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 N2D Pt1 N9 179.0(2) . . ? N2D Pt1 N1D 84.0(3) . . ? N9 Pt1 N1D 96.5(2) . . ? N2D Pt1 N3D 84.2(3) . . ? N9 Pt1 N3D 95.3(2) . . ? N1D Pt1 N3D 166.4(3) . . ? C1D N1D Pt1 107.3(5) . . ? C1D N1D H1FA 110.3 . . ? Pt1 N1D H1FA 110.3 . . ? C1D N1D H1FB 110.3 . . ? Pt1 N1D H1FB 110.3 . . ? H1FA N1D H1FB 108.5 . . ? C2D N2D C3D 116.9(7) . . ? C2D N2D Pt1 108.0(5) . . ? C3D N2D Pt1 106.8(5) . . ? C2D N2D H2FA 108.3 . . ? C3D N2D H2FA 108.3 . . ? Pt1 N2D H2FA 108.3 . . ? C4D N3D Pt1 108.7(5) . . ? C4D N3D H3FA 109.9 . . ? Pt1 N3D H3FA 109.9 . . ? C4D N3D H3FB 109.9 . . ? Pt1 N3D H3FB 109.9 . . ? H3FA N3D H3FB 108.3 . . ? C2D C1D N1D 107.9(7) . . ? C2D C1D H1DA 110.1 . . ? N1D C1D H1DA 110.1 . . ? C2D C1D H1DB 110.1 . . ? N1D C1D H1DB 110.1 . . ? H1DA C1D H1DB 108.4 . . ? N2D C2D C1D 106.1(7) . . ? N2D C2D H2DA 110.5 . . ? C1D C2D H2DA 110.5 . . ? N2D C2D H2DB 110.5 . . ? C1D C2D H2DB 110.5 . . ? H2DA C2D H2DB 108.7 . . ? C4D C3D N2D 106.4(7) . . ? C4D C3D H3DA 110.4 . . ? N2D C3D H3DA 110.4 . . ? C4D C3D H3DB 110.4 . . ? N2D C3D H3DB 110.4 . . ? H3DA C3D H3DB 108.6 . . ? C3D C4D N3D 108.3(7) . . ? C3D C4D H4DA 110.0 . . ? N3D C4D H4DA 110.0 . . ? C3D C4D H4DB 110.0 . . ? N3D C4D H4DB 110.0 . . ? H4DA C4D H4DB 108.4 . . ? C2 N1 C6 125.4(6) . . ? C2 N1 H1AA 117.3 . . ? C6 N1 H1AA 117.3 . . ? C2 N2 H2AA 120.0 . . ? C2 N2 H2AB 120.0 . . ? H2AA N2 H2AB 120.0 . . ? N3 C2 N2 120.0(7) . . ? N3 C2 N1 123.8(7) . . ? N2 C2 N1 116.2(6) . . ? C2 N3 C4 113.3(6) . . ? N3 C4 N9 125.1(6) . . ? N3 C4 C5 126.2(6) . . ? N9 C4 C5 108.7(6) . . ? N7 C5 C4 106.8(6) . . ? N7 C5 C6 132.8(7) . . ? C4 C5 C6 120.4(6) . . ? O6 C6 N1 121.1(7) . . ? O6 C6 C5 128.0(8) . . ? N1 C6 C5 110.9(6) . . ? C8 N7 C5 107.1(6) . . ? C8 N7 C7 126.2(6) . . ? C5 N7 C7 126.7(6) . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N7 C8 N9 112.0(6) . . ? N7 C8 H8 124.0 . . ? N9 C8 H8 124.0 . . ? C8 N9 C4 105.4(6) . . ? C8 N9 Pt1 124.7(4) . . ? C4 N9 Pt1 129.9(4) . . ? O11 Cl1 O14 108.9(5) . . ? O11 Cl1 O12 110.3(5) . . ? O14 Cl1 O12 110.2(5) . . ? O11 Cl1 O13 108.9(5) . . ? O14 Cl1 O13 108.4(6) . . ? O12 Cl1 O13 110.2(6) . . ? O21 N20 O23 117.0(8) . . ? O21 N20 O22 114.9(8) . . ? O23 N20 O22 121.1(8) . . ? 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 N2D Pt1 N1D C1D 9.6(6) . . . . ? N9 Pt1 N1D C1D -171.3(6) . . . . ? N3D Pt1 N1D C1D 39.2(13) . . . . ? N1D Pt1 N2D C2D 20.8(6) . . . . ? N3D Pt1 N2D C2D -152.5(6) . . . . ? N1D Pt1 N2D C3D 147.3(6) . . . . ? N3D Pt1 N2D C3D -26.0(6) . . . . ? N2D Pt1 N3D C4D -2.6(6) . . . . ? N9 Pt1 N3D C4D 178.3(6) . . . . ? N1D Pt1 N3D C4D -32.2(14) . . . . ? Pt1 N1D C1D C2D -38.0(9) . . . . ? C3D N2D C2D C1D -167.3(7) . . . . ? Pt1 N2D C2D C1D -47.0(8) . . . . ? N1D C1D C2D N2D 56.5(10) . . . . ? C2D N2D C3D C4D 171.0(7) . . . . ? Pt1 N2D C3D C4D 50.0(8) . . . . ? N2D C3D C4D N3D -53.3(10) . . . . ? Pt1 N3D C4D C3D 31.0(10) . . . . ? C6 N1 C2 N3 1.5(11) . . . . ? C6 N1 C2 N2 179.8(7) . . . . ? N2 C2 N3 C4 179.9(7) . . . . ? N1 C2 N3 C4 -1.9(10) . . . . ? C2 N3 C4 N9 -179.1(6) . . . . ? C2 N3 C4 C5 2.2(10) . . . . ? N3 C4 C5 N7 178.9(6) . . . . ? N9 C4 C5 N7 0.0(7) . . . . ? N3 C4 C5 C6 -1.9(11) . . . . ? N9 C4 C5 C6 179.1(6) . . . . ? C2 N1 C6 O6 177.5(7) . . . . ? C2 N1 C6 C5 -0.9(10) . . . . ? N7 C5 C6 O6 1.7(14) . . . . ? C4 C5 C6 O6 -177.1(8) . . . . ? N7 C5 C6 N1 180.0(7) . . . . ? C4 C5 C6 N1 1.1(9) . . . . ? C4 C5 N7 C8 -0.3(8) . . . . ? C6 C5 N7 C8 -179.2(8) . . . . ? C4 C5 N7 C7 179.5(7) . . . . ? C6 C5 N7 C7 0.6(13) . . . . ? C5 N7 C8 N9 0.4(8) . . . . ? C7 N7 C8 N9 -179.4(7) . . . . ? N7 C8 N9 C4 -0.4(8) . . . . ? N7 C8 N9 Pt1 177.8(4) . . . . ? N3 C4 N9 C8 -178.7(7) . . . . ? C5 C4 N9 C8 0.2(7) . . . . ? N3 C4 N9 Pt1 3.2(10) . . . . ? C5 C4 N9 Pt1 -177.9(4) . . . . ? N1D Pt1 N9 C8 -164.0(6) . . . . ? N3D Pt1 N9 C8 9.1(6) . . . . ? N1D Pt1 N9 C4 13.8(6) . . . . ? N3D Pt1 N9 C4 -173.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.150 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.166