Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Trevor Hambley' 'Timothy W. Failes' 'Matthew D. Hall' _publ_contact_author_name 'Prof Trevor Hambley' _publ_contact_author_address ; School of Chemistry University of Sydney Centre for Heavy Metals Research Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_email T.HAMBLEY@CHEM.USYD.EDU.AU _publ_section_title ; The first examples of platinum amine hydroxamate complexes: structures and biological activity ; data_twf18 _database_code_CSD 200413 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [{Pt(en)}2-u-(bha-H)]ClO4 _chemical_formula_sum 'C11 H22 Cl N5 O7 Pt2' _chemical_formula_weight 761.95 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' Ho Ho -0.2175 4.6783 '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 24.038(5) _cell_length_b 9.838(2) _cell_length_c 17.166(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.438(3) _cell_angle_gamma 90.00 _cell_volume 3948.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 14.334 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.0991 _exptl_absorpt_correction_T_max 0.3282 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _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 17757 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4626 _reflns_number_gt 4047 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-86 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.0709P)^2^+14.6094P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4626 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1134 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 C1 C -0.0069(3) 0.1694(8) 0.0717(5) 0.0473(16) Uani 1 1 d . . . C2 C -0.0591(3) 0.2116(8) 0.0981(5) 0.0468(16) Uani 1 1 d . . . C3 C -0.0854(3) 0.3288(8) 0.0587(4) 0.0445(15) Uani 1 1 d . . . C4 C -0.1332(3) 0.3792(9) 0.0843(5) 0.0522(18) Uani 1 1 d . . . H4 H -0.1518 0.4569 0.0606 0.063 Uiso 1 1 calc R . . C5 C -0.1525(4) 0.3144(9) 0.1437(5) 0.058(2) Uani 1 1 d . . . H5 H -0.1840 0.3496 0.1598 0.069 Uiso 1 1 calc R . . C6 C -0.1265(4) 0.1988(11) 0.1801(5) 0.065(2) Uani 1 1 d . . . H6 H -0.1410 0.1554 0.2193 0.078 Uiso 1 1 calc R . . C7 C -0.0787(3) 0.1471(9) 0.1583(5) 0.0541(18) Uani 1 1 d . . . H7 H -0.0602 0.0705 0.1836 0.065 Uiso 1 1 calc R . . C8 C 0.1921(4) -0.1056(11) 0.1083(8) 0.080(3) Uani 1 1 d . . . H8C H 0.2162 -0.0454 0.1466 0.096 Uiso 1 1 calc R . . H8D H 0.2064 -0.1975 0.1194 0.096 Uiso 1 1 calc R . . C9 C 0.1957(5) -0.0676(11) 0.0278(7) 0.076(3) Uani 1 1 d . . . H9C H 0.1789 -0.1380 -0.0099 0.091 Uiso 1 1 calc R . . H9D H 0.2353 -0.0561 0.0255 0.091 Uiso 1 1 calc R . . C10 C -0.1170(5) 0.5448(13) -0.1681(6) 0.077(3) Uani 1 1 d . . . H10A H -0.1369 0.6283 -0.1876 0.093 Uiso 1 1 calc R . . H10B H -0.1388 0.4689 -0.1956 0.093 Uiso 1 1 calc R . . C11 C -0.0577(5) 0.5457(11) -0.1833(6) 0.071(3) Uani 1 1 d . . . H11A H -0.0601 0.5348 -0.2402 0.086 Uiso 1 1 calc R . . H11B H -0.0394 0.6322 -0.1666 0.086 Uiso 1 1 calc R . . N1 N 0.0030(3) 0.2451(7) 0.0148(4) 0.0487(14) Uani 1 1 d . . . N2 N 0.1334(3) -0.0981(8) 0.1179(5) 0.0622(19) Uani 1 1 d . . . H2A H 0.1334 -0.0897 0.1701 0.075 Uiso 1 1 calc R . . H2B H 0.1145 -0.1747 0.0992 0.075 Uiso 1 1 calc R . . N3 N 0.1642(3) 0.0614(8) 0.0072(5) 0.0604(18) Uani 1 1 d . . . H3A H 0.1528 0.0695 -0.0464 0.072 Uiso 1 1 calc R . . H3B H 0.1873 0.1319 0.0259 0.072 Uiso 1 1 calc R . . N4 N -0.1113(3) 0.5325(7) -0.0815(4) 0.0542(15) Uani 1 1 d . . . H4A H -0.1453 0.5101 -0.0719 0.065 Uiso 1 1 calc R . . H4B H -0.1007 0.6132 -0.0581 0.065 Uiso 1 1 calc R . . N5 N -0.0232(3) 0.4345(7) -0.1388(4) 0.0559(16) Uani 1 1 d . . . H5A H 0.0138 0.4592 -0.1253 0.067 Uiso 1 1 calc R . . H5B H -0.0263 0.3601 -0.1700 0.067 Uiso 1 1 calc R . . O1 O 0.0550(2) 0.2212(5) -0.0073(3) 0.0518(13) Uani 1 1 d . . . O2 O 0.0271(2) 0.0726(5) 0.1062(3) 0.0533(13) Uani 1 1 d . . . O1W O 0.0764(9) 0.256(3) -0.1531(14) 0.134(8) Uani 0.50 1 d P . . O3 O 0.3126(6) 0.3764(17) 0.1884(9) 0.185(6) Uani 1 1 d . . . O2W O -0.0309(13) 0.1605(14) -0.1994(10) 0.138(9) Uani 0.50 1 d P . . O4 O 0.2417(7) 0.250(2) 0.2074(10) 0.208(8) Uani 1 1 d . . . O5 O 0.2316(6) 0.354(3) 0.0880(10) 0.288(14) Uani 1 1 d . . . O6 O 0.2994(8) 0.2013(19) 0.1186(11) 0.218(8) Uani 1 1 d . . . Cl1 Cl 0.27035(14) 0.2963(4) 0.15295(19) 0.0996(10) Uani 1 1 d . . . Pt1 Pt -0.052255(12) 0.38881(3) -0.032911(17) 0.04402(12) Uani 1 1 d . . . Pt2 Pt 0.094610(12) 0.06419(3) 0.056397(19) 0.04829(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(4) 0.049(4) 0.061(4) 0.003(3) 0.014(3) 0.006(3) C2 0.033(4) 0.047(4) 0.058(4) -0.002(3) 0.007(3) -0.003(3) C3 0.030(3) 0.050(4) 0.053(4) -0.003(3) 0.008(3) 0.002(3) C4 0.034(4) 0.064(5) 0.056(4) -0.006(3) 0.005(3) 0.008(3) C5 0.044(4) 0.078(6) 0.048(4) -0.009(4) 0.005(3) 0.003(4) C6 0.059(5) 0.084(6) 0.054(5) -0.003(4) 0.019(4) -0.014(5) C7 0.043(4) 0.061(5) 0.058(4) 0.006(4) 0.011(3) 0.001(4) C8 0.039(5) 0.076(7) 0.114(10) 0.006(6) 0.000(5) 0.018(4) C9 0.053(6) 0.073(6) 0.098(8) -0.008(5) 0.011(5) 0.015(5) C10 0.065(6) 0.109(8) 0.058(5) 0.024(5) 0.015(5) 0.031(6) C11 0.065(6) 0.087(7) 0.062(5) 0.020(5) 0.013(5) 0.008(5) N1 0.040(3) 0.048(3) 0.060(4) 0.004(3) 0.014(3) 0.005(3) N2 0.042(4) 0.055(4) 0.084(5) 0.001(4) 0.003(4) 0.007(3) N3 0.037(4) 0.069(5) 0.076(5) -0.003(4) 0.015(3) 0.001(3) N4 0.041(4) 0.052(4) 0.065(4) 0.007(3) 0.002(3) -0.001(3) N5 0.046(4) 0.059(4) 0.060(4) 0.001(3) 0.008(3) 0.004(3) O1 0.049(3) 0.044(3) 0.068(3) 0.006(2) 0.024(3) 0.007(2) O2 0.041(3) 0.050(3) 0.066(3) 0.013(2) 0.009(3) 0.006(2) O1W 0.077(13) 0.18(2) 0.140(17) -0.025(16) 0.016(12) 0.005(13) O3 0.161(13) 0.196(13) 0.173(12) -0.039(10) -0.013(10) -0.083(11) O2W 0.31(3) 0.052(8) 0.074(10) -0.009(7) 0.081(14) -0.003(13) O4 0.169(13) 0.29(2) 0.207(14) 0.021(14) 0.128(12) -0.028(13) O5 0.114(11) 0.58(4) 0.171(14) 0.132(19) 0.042(10) 0.138(18) O6 0.198(16) 0.223(17) 0.255(18) -0.083(15) 0.097(14) 0.033(14) Cl1 0.0730(19) 0.145(3) 0.0814(18) -0.0248(19) 0.0193(15) -0.0277(19) Pt1 0.03526(19) 0.04320(19) 0.0516(2) 0.00287(10) 0.00609(13) 0.00186(10) Pt2 0.0350(2) 0.0451(2) 0.0616(2) -0.00224(12) 0.00502(14) 0.00268(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 C1 N1 1.292(10) . ? C1 O2 1.305(9) . ? C1 C2 1.490(10) . ? C2 C7 1.385(11) . ? C2 C3 1.410(10) . ? C3 C4 1.411(10) . ? C3 Pt1 2.010(7) . ? C4 C5 1.373(12) . ? C5 C6 1.376(13) . ? C6 C7 1.384(12) . ? C8 C9 1.453(16) . ? C8 N2 1.460(12) . ? C9 N3 1.477(12) . ? C10 N4 1.465(11) . ? C10 C11 1.508(14) . ? C11 N5 1.474(12) . ? N1 O1 1.408(8) . ? N1 Pt1 1.982(7) . ? N2 Pt2 2.019(7) . ? N3 Pt2 2.042(7) . ? N4 Pt1 2.039(7) . ? N5 Pt1 2.140(7) . ? O1 Pt2 2.001(5) . ? O2 Pt2 2.003(6) . ? O3 Cl1 1.318(12) . ? O4 Cl1 1.361(12) . ? O5 Cl1 1.398(14) . ? O6 Cl1 1.378(14) . ? 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 N1 C1 O2 123.8(7) . . ? N1 C1 C2 112.7(7) . . ? O2 C1 C2 123.3(7) . . ? C7 C2 C3 122.7(7) . . ? C7 C2 C1 123.8(7) . . ? C3 C2 C1 113.4(7) . . ? C2 C3 C4 116.4(7) . . ? C2 C3 Pt1 113.6(5) . . ? C4 C3 Pt1 129.8(6) . . ? C5 C4 C3 120.6(8) . . ? C4 C5 C6 121.6(8) . . ? C5 C6 C7 120.0(8) . . ? C6 C7 C2 118.7(8) . . ? C9 C8 N2 111.5(9) . . ? C8 C9 N3 108.0(8) . . ? N4 C10 C11 107.8(8) . . ? N5 C11 C10 110.2(8) . . ? C1 N1 O1 116.0(6) . . ? C1 N1 Pt1 120.0(5) . . ? O1 N1 Pt1 124.0(5) . . ? C8 N2 Pt2 108.8(6) . . ? C9 N3 Pt2 109.6(6) . . ? C10 N4 Pt1 111.4(6) . . ? C11 N5 Pt1 110.0(5) . . ? N1 O1 Pt2 108.8(4) . . ? C1 O2 Pt2 108.8(5) . . ? O3 Cl1 O4 109.9(11) . . ? O3 Cl1 O6 100.9(11) . . ? O4 Cl1 O6 117.2(13) . . ? O3 Cl1 O5 115.1(15) . . ? O4 Cl1 O5 109.5(10) . . ? O6 Cl1 O5 104.2(13) . . ? N1 Pt1 C3 79.4(3) . . ? N1 Pt1 N4 178.1(3) . . ? C3 Pt1 N4 99.2(3) . . ? N1 Pt1 N5 100.5(3) . . ? C3 Pt1 N5 173.2(3) . . ? N4 Pt1 N5 80.8(3) . . ? O1 Pt2 O2 82.6(2) . . ? O1 Pt2 N2 178.2(3) . . ? O2 Pt2 N2 97.6(3) . . ? O1 Pt2 N3 96.7(3) . . ? O2 Pt2 N3 178.2(3) . . ? N2 Pt2 N3 83.2(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 N1 C1 C2 C7 -179.7(8) . . . . ? O2 C1 C2 C7 -4.3(12) . . . . ? N1 C1 C2 C3 -2.9(10) . . . . ? O2 C1 C2 C3 172.6(7) . . . . ? C7 C2 C3 C4 0.5(11) . . . . ? C1 C2 C3 C4 -176.4(7) . . . . ? C7 C2 C3 Pt1 -174.4(6) . . . . ? C1 C2 C3 Pt1 8.7(8) . . . . ? C2 C3 C4 C5 -0.8(11) . . . . ? Pt1 C3 C4 C5 173.2(6) . . . . ? C3 C4 C5 C6 -0.3(13) . . . . ? C4 C5 C6 C7 1.7(13) . . . . ? C5 C6 C7 C2 -1.9(13) . . . . ? C3 C2 C7 C6 0.8(13) . . . . ? C1 C2 C7 C6 177.4(8) . . . . ? N2 C8 C9 N3 48.7(12) . . . . ? N4 C10 C11 N5 47.6(12) . . . . ? O2 C1 N1 O1 -2.3(11) . . . . ? C2 C1 N1 O1 173.2(6) . . . . ? O2 C1 N1 Pt1 179.9(6) . . . . ? C2 C1 N1 Pt1 -4.7(9) . . . . ? C9 C8 N2 Pt2 -37.7(11) . . . . ? C8 C9 N3 Pt2 -35.6(10) . . . . ? C11 C10 N4 Pt1 -44.4(11) . . . . ? C10 C11 N5 Pt1 -28.6(10) . . . . ? C1 N1 O1 Pt2 3.2(8) . . . . ? Pt1 N1 O1 Pt2 -179.0(3) . . . . ? N1 C1 O2 Pt2 0.0(10) . . . . ? C2 C1 O2 Pt2 -175.0(6) . . . . ? C1 N1 Pt1 C3 7.5(6) . . . . ? O1 N1 Pt1 C3 -170.1(6) . . . . ? C1 N1 Pt1 N4 -35(8) . . . . ? O1 N1 Pt1 N4 147(8) . . . . ? C1 N1 Pt1 N5 -165.5(6) . . . . ? O1 N1 Pt1 N5 16.8(6) . . . . ? C2 C3 Pt1 N1 -8.5(5) . . . . ? C4 C3 Pt1 N1 177.4(8) . . . . ? C2 C3 Pt1 N4 170.2(5) . . . . ? C4 C3 Pt1 N4 -3.9(8) . . . . ? C2 C3 Pt1 N5 81(2) . . . . ? C4 C3 Pt1 N5 -93(2) . . . . ? C10 N4 Pt1 N1 -108(8) . . . . ? C10 N4 Pt1 C3 -150.4(7) . . . . ? C10 N4 Pt1 N5 22.7(7) . . . . ? C11 N5 Pt1 N1 -177.8(6) . . . . ? C11 N5 Pt1 C3 94(2) . . . . ? C11 N5 Pt1 N4 3.7(6) . . . . ? N1 O1 Pt2 O2 -2.5(5) . . . . ? N1 O1 Pt2 N2 92(9) . . . . ? N1 O1 Pt2 N3 179.2(5) . . . . ? C1 O2 Pt2 O1 1.5(5) . . . . ? C1 O2 Pt2 N2 -176.8(5) . . . . ? C1 O2 Pt2 N3 67(9) . . . . ? C8 N2 Pt2 O1 100(9) . . . . ? C8 N2 Pt2 O2 -165.3(7) . . . . ? C8 N2 Pt2 N3 13.1(7) . . . . ? C9 N3 Pt2 O1 -165.8(6) . . . . ? C9 N3 Pt2 O2 129(8) . . . . ? C9 N3 Pt2 N2 12.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.070 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.249 data_twf32 _database_code_CSD 203671 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [{Pt(R,R-chxn)}2-u-(bha-H)]NO3 _chemical_formula_sum 'C38 H72 N12 O14 Pt4' _chemical_formula_weight 1701.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.704(3) _cell_length_b 23.505(8) _cell_length_c 15.251(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.141(6) _cell_angle_gamma 90.00 _cell_volume 2726.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 10.296 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.1045 _exptl_absorpt_correction_T_max 0.2326 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 24663 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6601 _reflns_number_gt 5062 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.0808P)^2^+21.2894P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(6) _refine_ls_number_reflns 6601 _refine_ls_number_parameters 614 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.277(3) 0.1626(10) 0.0794(15) 0.040(5) Uani 1 1 d . . . C2 C 0.247(3) 0.1077(10) 0.029(2) 0.052(6) Uani 1 1 d . . . C3 C 0.256(3) 0.0606(11) 0.0843(15) 0.044(5) Uani 1 1 d U . . C4 C 0.230(4) 0.0080(11) 0.0392(17) 0.057(6) Uani 1 1 d . . . H4 H 0.2315 -0.0252 0.0727 0.068 Uiso 1 1 calc R . . C5 C 0.203(5) 0.0035(11) -0.0504(19) 0.072(9) Uani 1 1 d . . . H5 H 0.1972 -0.0323 -0.0767 0.086 Uiso 1 1 calc R . . C6 C 0.184(4) 0.0514(13) -0.103(2) 0.066(7) Uani 1 1 d . . . H6 H 0.1521 0.0482 -0.1645 0.079 Uiso 1 1 calc R . . C7 C 0.213(3) 0.1061(10) -0.0622(15) 0.044(5) Uani 1 1 d . . . H7 H 0.2091 0.1392 -0.0959 0.053 Uiso 1 1 calc R . . C8 C 0.367(4) 0.3916(10) 0.1038(19) 0.057(7) Uani 1 1 d . . . H8 H 0.4951 0.3898 0.1178 0.069 Uiso 1 1 calc R . . C9 C 0.292(4) 0.3893(10) 0.186(2) 0.062(7) Uani 1 1 d . . . H9 H 0.1635 0.3915 0.1730 0.075 Uiso 1 1 calc R . . C10 C 0.367(7) 0.4384(18) 0.259(3) 0.121(15) Uani 1 1 d U . . H10A H 0.4936 0.4369 0.2744 0.145 Uiso 1 1 calc R . . H10B H 0.3137 0.4357 0.3123 0.145 Uiso 1 1 calc R . . C11 C 0.301(5) 0.4959(13) 0.201(3) 0.097(12) Uani 1 1 d . . . H11A H 0.1744 0.4955 0.1854 0.117 Uiso 1 1 calc R . . H11B H 0.3343 0.5294 0.2370 0.117 Uiso 1 1 calc R . . C12 C 0.384(6) 0.4990(14) 0.117(3) 0.099(12) Uani 1 1 d U . . H12A H 0.5110 0.4965 0.1309 0.119 Uiso 1 1 calc R . . H12B H 0.3536 0.5346 0.0859 0.119 Uiso 1 1 calc R . . C13 C 0.311(5) 0.4485(14) 0.058(3) 0.088(10) Uani 1 1 d . . . H13A H 0.3545 0.4505 0.0016 0.106 Uiso 1 1 calc R . . H13B H 0.1837 0.4508 0.0457 0.106 Uiso 1 1 calc R . . C14 C 0.251(3) -0.0053(12) 0.3541(17) 0.056(7) Uani 1 1 d . . . H14 H 0.1277 0.0053 0.3540 0.068 Uiso 1 1 calc R . . C15 C 0.365(3) 0.0379(12) 0.4029(17) 0.056(7) Uani 1 1 d . . . H15 H 0.4873 0.0268 0.4012 0.067 Uiso 1 1 calc R . . C16 C 0.342(3) 0.0415(14) 0.4966(18) 0.066(8) Uani 1 1 d . . . H16A H 0.2238 0.0541 0.5003 0.079 Uiso 1 1 calc R . . H16B H 0.4237 0.0693 0.5269 0.079 Uiso 1 1 calc R . . C17 C 0.375(4) -0.0169(17) 0.543(2) 0.079(9) Uani 1 1 d U . . H17A H 0.3490 -0.0146 0.6025 0.095 Uiso 1 1 calc R . . H17B H 0.4984 -0.0271 0.5461 0.095 Uiso 1 1 calc R . . C18 C 0.257(5) -0.0640(13) 0.489(2) 0.079(10) Uani 1 1 d . . . H18A H 0.2865 -0.1008 0.5165 0.095 Uiso 1 1 calc R . . H18B H 0.1348 -0.0562 0.4921 0.095 Uiso 1 1 calc R . . C19 C 0.284(4) -0.0657(12) 0.395(2) 0.068(8) Uani 1 1 d . . . H19A H 0.2032 -0.0927 0.3622 0.082 Uiso 1 1 calc R . . H19B H 0.4030 -0.0778 0.3913 0.082 Uiso 1 1 calc R . . C20 C 0.209(3) 0.4662(9) 0.5818(16) 0.040(5) Uani 1 1 d . . . C21 C 0.163(3) 0.5153(9) 0.5218(14) 0.038(4) Uani 1 1 d . . . C22 C 0.174(3) 0.5691(13) 0.5675(19) 0.062(7) Uani 1 1 d . . . C23 C 0.139(4) 0.6172(13) 0.511(3) 0.077(9) Uani 1 1 d . . . H23 H 0.1425 0.6533 0.5364 0.092 Uiso 1 1 calc R . . C24 C 0.099(4) 0.6119(12) 0.422(2) 0.062(7) Uani 1 1 d . . . H24 H 0.0749 0.6443 0.3867 0.074 Uiso 1 1 calc R . . C25 C 0.096(4) 0.5588(15) 0.381(2) 0.076(8) Uani 1 1 d . . . H25 H 0.0721 0.5570 0.3194 0.092 Uiso 1 1 calc R . . C26 C 0.125(4) 0.5088(13) 0.428(2) 0.070(8) Uani 1 1 d . . . H26 H 0.1198 0.4735 0.4005 0.084 Uiso 1 1 calc R . . C27 C 0.315(5) 0.2394(17) 0.661(2) 0.085(10) Uani 1 1 d U . . H27 H 0.2010 0.2315 0.6797 0.102 Uiso 1 1 calc R . . C28 C 0.443(5) 0.2604(11) 0.7372(17) 0.081(10) Uani 1 1 d U . . H28 H 0.5537 0.2672 0.7154 0.097 Uiso 1 1 calc R . . C29 C 0.475(6) 0.2158(12) 0.806(2) 0.086(10) Uani 1 1 d . . . H29A H 0.3756 0.2146 0.8381 0.104 Uiso 1 1 calc R . . H29B H 0.5777 0.2265 0.8486 0.104 Uiso 1 1 calc R . . C30 C 0.505(7) 0.157(2) 0.772(3) 0.123(15) Uani 1 1 d U . . H30A H 0.6179 0.1559 0.7518 0.148 Uiso 1 1 calc R . . H30B H 0.5098 0.1299 0.8207 0.148 Uiso 1 1 calc R . . C31 C 0.371(6) 0.1370(16) 0.699(3) 0.101(12) Uani 1 1 d U . . H31A H 0.2552 0.1368 0.7165 0.121 Uiso 1 1 calc R . . H31B H 0.3979 0.0992 0.6797 0.121 Uiso 1 1 calc R . . C32 C 0.385(7) 0.1863(15) 0.619(3) 0.103(12) Uani 1 1 d U . . H32A H 0.5053 0.1916 0.6094 0.124 Uiso 1 1 calc R . . H32B H 0.3119 0.1763 0.5636 0.124 Uiso 1 1 calc R . . C33 C 0.252(3) 0.6599(12) 0.820(2) 0.063(7) Uani 1 1 d . . . H33 H 0.3807 0.6578 0.8281 0.075 Uiso 1 1 calc R . . C34 C 0.180(3) 0.6075(12) 0.871(2) 0.059(7) Uani 1 1 d . . . H34 H 0.0517 0.6067 0.8568 0.070 Uiso 1 1 calc R . . C35 C 0.235(4) 0.6173(16) 0.975(3) 0.085(11) Uani 1 1 d . . . H35A H 0.1786 0.5885 1.0062 0.102 Uiso 1 1 calc R . . H35B H 0.3608 0.6126 0.9903 0.102 Uiso 1 1 calc R . . C36 C 0.182(4) 0.6774(15) 1.005(3) 0.084(11) Uani 1 1 d . . . H36A H 0.0554 0.6791 1.0019 0.101 Uiso 1 1 calc R . . H36B H 0.2346 0.6831 1.0667 0.101 Uiso 1 1 calc R . . C37 C 0.241(5) 0.7254(14) 0.949(3) 0.094(11) Uani 1 1 d U . . H37A H 0.3663 0.7310 0.9667 0.113 Uiso 1 1 calc R . . H37B H 0.1828 0.7601 0.9624 0.113 Uiso 1 1 calc R . . C38 C 0.203(4) 0.7160(15) 0.842(2) 0.083(10) Uani 1 1 d . . . H38A H 0.0790 0.7219 0.8206 0.099 Uiso 1 1 calc R . . H38B H 0.2691 0.7437 0.8138 0.099 Uiso 1 1 calc R . . N1 N 0.290(3) 0.1552(8) 0.1645(13) 0.046(5) Uani 1 1 d . . . N2 N 0.301(3) 0.3414(9) 0.0531(15) 0.053(5) Uani 1 1 d . . . H2A H 0.3685 0.3346 0.0110 0.064 Uiso 1 1 calc R . . H2B H 0.1906 0.3477 0.0258 0.064 Uiso 1 1 calc R . . N3 N 0.345(4) 0.3342(12) 0.2307(19) 0.078(8) Uani 1 1 d . . . H3A H 0.2800 0.3268 0.2732 0.094 Uiso 1 1 calc R . . H3B H 0.4594 0.3353 0.2557 0.094 Uiso 1 1 calc R . . N4 N 0.288(3) -0.0052(9) 0.2592(16) 0.059(6) Uani 1 1 d . . . H4A H 0.2039 -0.0247 0.2240 0.070 Uiso 1 1 calc R . . H4B H 0.3921 -0.0224 0.2571 0.070 Uiso 1 1 calc R . . N5 N 0.332(3) 0.0929(10) 0.3545(12) 0.054(5) Uani 1 1 d . . . H5A H 0.4238 0.1165 0.3700 0.064 Uiso 1 1 calc R . . H5B H 0.2354 0.1095 0.3691 0.064 Uiso 1 1 calc R . . N6 N 0.767(3) 0.3560(12) 0.938(3) 0.106(13) Uani 1 1 d . . . N7 N 0.243(2) 0.4797(8) 0.6651(13) 0.040(4) Uani 1 1 d . . . N8 N 0.301(5) 0.2909(11) 0.5954(17) 0.101(11) Uani 1 1 d U . . H8A H 0.2015 0.2878 0.5556 0.121 Uiso 1 1 calc R . . H8B H 0.3926 0.2905 0.5657 0.121 Uiso 1 1 calc R . . N9 N 0.383(4) 0.3160(9) 0.7688(15) 0.075(8) Uani 1 1 d . . . H9A H 0.4719 0.3335 0.8038 0.090 Uiso 1 1 calc R . . H9B H 0.2949 0.3105 0.8005 0.090 Uiso 1 1 calc R . . N10 N 0.186(4) 0.6486(10) 0.729(2) 0.085(9) Uani 1 1 d . . . H10C H 0.2426 0.6706 0.6941 0.102 Uiso 1 1 calc R . . H10D H 0.0708 0.6577 0.7175 0.102 Uiso 1 1 calc R . . N11 N 0.247(3) 0.5571(10) 0.8386(15) 0.060(6) Uani 1 1 d . . . H11C H 0.1883 0.5268 0.8545 0.072 Uiso 1 1 calc R . . H11D H 0.3616 0.5531 0.8617 0.072 Uiso 1 1 calc R . . N12 N 0.163(8) 0.7771(16) 0.490(4) 0.167(19) Uani 1 1 d U . . O1 O 0.318(3) 0.2062(8) 0.2165(11) 0.056(5) Uani 1 1 d . . . O2 O 0.2760(19) 0.2120(7) 0.0396(10) 0.042(3) Uani 1 1 d . . . O1W O 0.046(3) 0.4431(10) 0.8348(13) 0.069(5) Uani 1 1 d . . . O3 O 0.613(3) 0.3625(11) 0.9598(18) 0.093(7) Uani 1 1 d . . . O2W O 0.118(3) 0.2788(10) 0.8797(14) 0.078(6) Uani 1 1 d . . . O4 O 0.783(4) 0.334(2) 0.8571(19) 0.149(17) Uani 1 1 d . . . O3W O 0.127(4) 0.2047(11) 0.3610(19) 0.105(9) Uani 1 1 d . . . O5 O 0.896(3) 0.3658(10) 0.992(2) 0.119(11) Uani 1 1 d . . . O4W O 0.545(7) 0.2052(18) 0.360(2) 0.21(3) Uani 1 1 d . . . O6 O 0.300(2) 0.4392(7) 0.7263(10) 0.046(4) Uani 1 1 d . . . O7 O 0.219(2) 0.4130(8) 0.5556(11) 0.052(4) Uani 1 1 d . . . O10 O 0.376(4) 0.7817(13) 0.503(2) 0.131(11) Uani 1 1 d U . . O11 O 0.093(8) 0.793(5) 0.536(6) 0.36(5) Uani 1 1 d U . . O12 O 0.160(6) 0.772(2) 0.398(4) 0.184(17) Uani 1 1 d U . . Pt1 Pt 0.29609(12) 0.07730(3) 0.21441(6) 0.0462(2) Uani 1 1 d . . . Pt2 Pt 0.30578(12) 0.27314(4) 0.13292(6) 0.0476(2) Uani 1 1 d . . . Pt3 Pt 0.21812(11) 0.56233(3) 0.69723(6) 0.0486(2) Uani 1 1 d . . . Pt4 Pt 0.29772(14) 0.36445(4) 0.66173(6) 0.0538(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(10) 0.034(11) 0.047(12) 0.008(9) -0.004(9) 0.004(8) C2 0.039(12) 0.030(11) 0.087(19) -0.016(11) 0.005(12) -0.004(9) C3 0.031(7) 0.039(8) 0.062(9) -0.005(7) 0.001(7) -0.002(7) C4 0.079(18) 0.042(13) 0.055(15) 0.007(11) 0.029(13) 0.004(12) C5 0.13(3) 0.024(11) 0.065(17) 0.009(11) 0.033(17) 0.002(14) C6 0.069(17) 0.061(18) 0.067(17) -0.002(14) 0.010(13) -0.006(13) C7 0.048(13) 0.036(11) 0.049(13) -0.008(9) 0.005(10) -0.013(9) C8 0.062(15) 0.031(11) 0.082(18) -0.022(12) 0.019(13) -0.014(10) C9 0.09(2) 0.022(11) 0.078(18) -0.013(11) 0.013(15) 0.011(11) C10 0.13(3) 0.08(2) 0.15(3) -0.05(2) 0.02(2) 0.020(19) C11 0.12(3) 0.033(15) 0.14(3) -0.044(18) 0.00(2) -0.026(16) C12 0.12(3) 0.039(15) 0.15(3) -0.028(18) 0.04(2) -0.001(16) C13 0.11(3) 0.046(17) 0.11(3) -0.009(17) 0.03(2) 0.002(17) C14 0.047(13) 0.064(17) 0.065(15) 0.023(13) 0.031(12) 0.025(12) C15 0.048(13) 0.064(16) 0.059(15) 0.019(12) 0.018(11) 0.028(12) C16 0.043(13) 0.09(2) 0.061(16) 0.024(15) 0.007(11) 0.019(13) C17 0.059(16) 0.11(2) 0.072(17) 0.025(17) 0.029(14) 0.027(17) C18 0.12(3) 0.049(16) 0.08(2) 0.030(15) 0.05(2) 0.014(17) C19 0.058(16) 0.053(16) 0.10(2) 0.043(15) 0.028(15) 0.011(12) C20 0.027(10) 0.030(10) 0.067(15) -0.002(9) 0.021(9) -0.002(7) C21 0.027(9) 0.039(11) 0.047(12) 0.008(9) 0.005(8) -0.006(8) C22 0.036(11) 0.059(17) 0.094(19) 0.021(15) 0.018(11) 0.015(12) C23 0.08(2) 0.039(15) 0.12(3) 0.020(16) 0.016(19) 0.003(13) C24 0.066(17) 0.048(15) 0.069(18) 0.019(13) 0.002(14) 0.015(12) C25 0.09(2) 0.069(19) 0.066(17) 0.006(16) 0.010(15) -0.007(18) C26 0.061(16) 0.051(16) 0.10(2) 0.013(15) 0.023(16) 0.023(13) C27 0.095(13) 0.077(13) 0.079(12) 0.001(9) 0.003(9) 0.009(9) C28 0.16(3) 0.030(13) 0.048(14) 0.003(10) 0.014(16) 0.012(15) C29 0.14(3) 0.032(14) 0.09(2) 0.001(14) 0.02(2) 0.025(17) C30 0.18(4) 0.09(3) 0.09(2) 0.01(2) 0.02(3) 0.06(3) C31 0.15(3) 0.054(16) 0.09(2) -0.015(16) -0.016(19) 0.010(18) C32 0.16(3) 0.052(16) 0.091(19) -0.020(15) -0.018(19) 0.028(17) C33 0.034(11) 0.047(14) 0.10(2) -0.018(15) -0.002(12) -0.014(10) C34 0.025(10) 0.059(15) 0.09(2) -0.027(14) 0.016(11) -0.006(10) C35 0.042(15) 0.09(2) 0.12(3) -0.04(2) 0.016(16) -0.008(15) C36 0.034(13) 0.08(2) 0.14(3) -0.03(2) 0.022(17) -0.005(13) C37 0.070(19) 0.047(16) 0.16(3) 0.000(19) 0.00(2) -0.005(14) C38 0.063(18) 0.059(19) 0.11(3) -0.012(18) -0.029(17) -0.022(14) N1 0.063(12) 0.026(9) 0.049(11) -0.008(8) 0.006(9) 0.004(9) N2 0.049(11) 0.046(12) 0.066(14) 0.001(10) 0.017(10) -0.003(9) N3 0.086(19) 0.070(18) 0.078(18) -0.008(14) 0.013(14) 0.012(14) N4 0.059(12) 0.031(10) 0.096(16) 0.027(11) 0.041(12) 0.010(9) N5 0.060(12) 0.061(14) 0.039(10) 0.009(9) 0.005(9) 0.011(10) N6 0.044(13) 0.062(17) 0.21(4) 0.08(2) 0.014(19) -0.003(12) N7 0.034(9) 0.028(9) 0.061(12) 0.000(8) 0.015(8) -0.003(7) N8 0.19(3) 0.051(16) 0.058(15) -0.030(12) 0.007(17) -0.005(18) N9 0.15(3) 0.029(11) 0.051(12) -0.004(9) 0.023(14) -0.009(13) N10 0.10(2) 0.027(11) 0.12(2) -0.014(13) -0.009(17) -0.003(12) N11 0.041(10) 0.053(12) 0.092(15) -0.013(11) 0.029(10) -0.021(9) N12 0.22(4) 0.041(15) 0.18(3) 0.02(2) -0.13(3) 0.00(2) O1 0.086(13) 0.034(9) 0.047(9) 0.000(7) 0.003(9) 0.002(8) O2 0.038(8) 0.036(8) 0.053(9) 0.003(7) 0.011(7) -0.007(6) O1W 0.084(14) 0.065(12) 0.066(11) -0.002(9) 0.032(10) 0.005(10) O3 0.066(12) 0.057(12) 0.17(2) 0.008(15) 0.052(14) 0.014(11) O2W 0.096(15) 0.062(13) 0.081(13) 0.007(11) 0.025(11) -0.001(12) O4 0.13(2) 0.25(5) 0.077(17) 0.07(2) 0.054(17) 0.01(3) O3W 0.14(2) 0.054(14) 0.11(2) 0.006(13) 0.006(17) 0.023(15) O5 0.076(14) 0.037(11) 0.22(3) -0.015(17) -0.049(17) -0.004(11) O4W 0.35(6) 0.18(4) 0.082(19) -0.01(2) -0.01(3) 0.20(4) O6 0.061(10) 0.036(8) 0.043(8) 0.000(6) 0.017(7) 0.003(7) O7 0.045(9) 0.054(10) 0.061(10) -0.019(8) 0.022(8) 0.000(7) O10 0.14(2) 0.079(17) 0.16(2) 0.045(17) -0.010(19) -0.048(17) O11 0.25(6) 0.45(9) 0.47(9) 0.01(7) 0.28(6) 0.04(5) O12 0.16(3) 0.19(4) 0.21(4) -0.03(4) 0.03(3) -0.02(3) Pt1 0.0481(4) 0.0387(5) 0.0548(5) 0.0124(4) 0.0173(4) 0.0087(4) Pt2 0.0549(5) 0.0376(4) 0.0500(5) 0.0017(4) 0.0076(4) 0.0036(4) Pt3 0.0459(4) 0.0320(4) 0.0690(6) 0.0010(4) 0.0123(4) -0.0010(3) Pt4 0.0807(6) 0.0324(4) 0.0527(5) 0.0024(4) 0.0239(5) 0.0077(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.30(3) . ? C1 O2 1.31(3) . ? C1 C2 1.51(3) . ? C2 C7 1.37(4) . ? C2 C3 1.39(4) . ? C3 C4 1.41(4) . ? C3 Pt1 2.00(2) . ? C4 C5 1.35(4) . ? C5 C6 1.38(4) . ? C6 C7 1.43(4) . ? C8 N2 1.46(3) . ? C8 C9 1.47(4) . ? C8 C13 1.54(4) . ? C9 N3 1.49(4) . ? C9 C10 1.64(5) . ? C10 C11 1.65(6) . ? C11 C12 1.53(5) . ? C12 C13 1.54(5) . ? C14 C15 1.47(4) . ? C14 N4 1.52(3) . ? C14 C19 1.56(3) . ? C15 C16 1.47(4) . ? C15 N5 1.49(3) . ? C16 C17 1.54(4) . ? C17 C18 1.57(5) . ? C18 C19 1.49(4) . ? C20 N7 1.30(3) . ? C20 O7 1.32(3) . ? C20 C21 1.48(3) . ? C21 C26 1.42(4) . ? C21 C22 1.44(4) . ? C22 C23 1.42(4) . ? C22 Pt3 1.96(3) . ? C23 C24 1.36(5) . ? C24 C25 1.39(4) . ? C25 C26 1.38(4) . ? C27 C28 1.48(5) . ? C27 C32 1.54(5) . ? C27 N8 1.57(5) . ? C28 C29 1.48(4) . ? C28 N9 1.49(3) . ? C29 C30 1.52(5) . ? C30 C31 1.46(6) . ? C31 C32 1.70(6) . ? C33 N10 1.43(4) . ? C33 C38 1.43(4) . ? C33 C34 1.60(4) . ? C34 N11 1.41(3) . ? C34 C35 1.59(5) . ? C35 C36 1.56(4) . ? C36 C37 1.53(5) . ? C37 C38 1.62(6) . ? N1 O1 1.43(3) . ? N1 Pt1 1.98(2) . ? N2 Pt2 2.01(2) . ? N3 Pt2 2.06(3) . ? N4 Pt1 2.06(2) . ? N5 Pt1 2.142(19) . ? N6 O5 1.21(4) . ? N6 O3 1.29(3) . ? N6 O4 1.36(5) . ? N7 O6 1.36(2) . ? N7 Pt3 2.020(19) . ? N8 Pt4 2.00(2) . ? N9 Pt4 2.01(2) . ? N10 Pt3 2.11(2) . ? N11 Pt3 2.14(2) . ? N12 O11 1.02(8) . ? N12 O12 1.40(7) . ? N12 O10 1.62(7) . ? O1 Pt2 2.018(18) . ? O2 Pt2 2.010(16) . ? O6 Pt4 2.014(17) . ? O7 Pt4 1.994(19) . ? 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 N1 C1 O2 125(2) . . ? N1 C1 C2 112(2) . . ? O2 C1 C2 122(2) . . ? C7 C2 C3 126(2) . . ? C7 C2 C1 122(2) . . ? C3 C2 C1 112(2) . . ? C2 C3 C4 114(2) . . ? C2 C3 Pt1 115.8(17) . . ? C4 C3 Pt1 130.0(19) . . ? C5 C4 C3 123(2) . . ? C4 C5 C6 121(3) . . ? C5 C6 C7 119(3) . . ? C2 C7 C6 117(2) . . ? N2 C8 C9 106(2) . . ? N2 C8 C13 114(2) . . ? C9 C8 C13 108(2) . . ? C8 C9 N3 108(2) . . ? C8 C9 C10 114(3) . . ? N3 C9 C10 105(3) . . ? C9 C10 C11 100(3) . . ? C12 C11 C10 111(3) . . ? C11 C12 C13 107(3) . . ? C12 C13 C8 111(3) . . ? C15 C14 N4 107(2) . . ? C15 C14 C19 112(2) . . ? N4 C14 C19 110(2) . . ? C14 C15 C16 112(2) . . ? C14 C15 N5 108(2) . . ? C16 C15 N5 113(2) . . ? C15 C16 C17 111(3) . . ? C16 C17 C18 111(2) . . ? C19 C18 C17 111(3) . . ? C18 C19 C14 109(3) . . ? N7 C20 O7 121(2) . . ? N7 C20 C21 114.0(19) . . ? O7 C20 C21 125(2) . . ? C26 C21 C22 124(2) . . ? C26 C21 C20 122(2) . . ? C22 C21 C20 113(2) . . ? C23 C22 C21 115(3) . . ? C23 C22 Pt3 131(3) . . ? C21 C22 Pt3 113.8(18) . . ? C24 C23 C22 122(3) . . ? C23 C24 C25 121(3) . . ? C26 C25 C24 123(3) . . ? C25 C26 C21 115(3) . . ? C28 C27 C32 111(3) . . ? C28 C27 N8 102(3) . . ? C32 C27 N8 111(3) . . ? C27 C28 C29 110(3) . . ? C27 C28 N9 110(3) . . ? C29 C28 N9 115(2) . . ? C28 C29 C30 115(3) . . ? C31 C30 C29 115(4) . . ? C30 C31 C32 102(3) . . ? C27 C32 C31 101(3) . . ? N10 C33 C38 110(3) . . ? N10 C33 C34 104(2) . . ? C38 C33 C34 118(3) . . ? N11 C34 C35 115(3) . . ? N11 C34 C33 107(2) . . ? C35 C34 C33 108(2) . . ? C36 C35 C34 113(3) . . ? C37 C36 C35 113(3) . . ? C36 C37 C38 116(3) . . ? C33 C38 C37 111(3) . . ? C1 N1 O1 114.9(18) . . ? C1 N1 Pt1 120.2(15) . . ? O1 N1 Pt1 124.6(14) . . ? C8 N2 Pt2 110.7(17) . . ? C9 N3 Pt2 106.3(18) . . ? C14 N4 Pt1 109.7(16) . . ? C15 N5 Pt1 109.3(16) . . ? O5 N6 O3 119(4) . . ? O5 N6 O4 121(3) . . ? O3 N6 O4 120(3) . . ? C20 N7 O6 119.8(18) . . ? C20 N7 Pt3 117.5(15) . . ? O6 N7 Pt3 122.7(14) . . ? C27 N8 Pt4 110.4(19) . . ? C28 N9 Pt4 108.1(16) . . ? C33 N10 Pt3 111.3(19) . . ? C34 N11 Pt3 109(2) . . ? O11 N12 O12 142(7) . . ? O11 N12 O10 122(6) . . ? O12 N12 O10 89(5) . . ? N1 O1 Pt2 108.4(12) . . ? C1 O2 Pt2 108.2(14) . . ? N7 O6 Pt4 107.4(12) . . ? C20 O7 Pt4 108.8(14) . . ? N1 Pt1 C3 79.0(9) . . ? N1 Pt1 N4 176.0(10) . . ? C3 Pt1 N4 97.8(10) . . ? N1 Pt1 N5 102.5(8) . . ? C3 Pt1 N5 177.9(9) . . ? N4 Pt1 N5 80.6(9) . . ? O2 Pt2 N2 98.8(7) . . ? O2 Pt2 O1 83.0(7) . . ? N2 Pt2 O1 177.8(9) . . ? O2 Pt2 N3 177.7(10) . . ? N2 Pt2 N3 82.4(11) . . ? O1 Pt2 N3 95.8(9) . . ? C22 Pt3 N7 80.9(10) . . ? C22 Pt3 N10 98.2(12) . . ? N7 Pt3 N10 178.6(9) . . ? C22 Pt3 N11 175.8(9) . . ? N7 Pt3 N11 101.0(9) . . ? N10 Pt3 N11 79.8(11) . . ? O7 Pt4 N8 96.3(10) . . ? O7 Pt4 N9 178.7(10) . . ? N8 Pt4 N9 83.9(11) . . ? O7 Pt4 O6 82.8(7) . . ? N8 Pt4 O6 178.4(12) . . ? N9 Pt4 O6 96.9(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 N1 C1 C2 C7 174(2) . . . . ? O2 C1 C2 C7 -2(3) . . . . ? N1 C1 C2 C3 -5(3) . . . . ? O2 C1 C2 C3 179(2) . . . . ? C7 C2 C3 C4 1(3) . . . . ? C1 C2 C3 C4 -180(2) . . . . ? C7 C2 C3 Pt1 -177.1(19) . . . . ? C1 C2 C3 Pt1 2(2) . . . . ? C2 C3 C4 C5 2(4) . . . . ? Pt1 C3 C4 C5 179(2) . . . . ? C3 C4 C5 C6 -6(5) . . . . ? C4 C5 C6 C7 7(5) . . . . ? C3 C2 C7 C6 0(4) . . . . ? C1 C2 C7 C6 -179(2) . . . . ? C5 C6 C7 C2 -4(4) . . . . ? N2 C8 C9 N3 57(3) . . . . ? C13 C8 C9 N3 180(3) . . . . ? N2 C8 C9 C10 173(3) . . . . ? C13 C8 C9 C10 -63(4) . . . . ? C8 C9 C10 C11 61(4) . . . . ? N3 C9 C10 C11 179(3) . . . . ? C9 C10 C11 C12 -61(4) . . . . ? C10 C11 C12 C13 65(4) . . . . ? C11 C12 C13 C8 -63(4) . . . . ? N2 C8 C13 C12 179(3) . . . . ? C9 C8 C13 C12 62(4) . . . . ? N4 C14 C15 C16 -179.4(19) . . . . ? C19 C14 C15 C16 -59(3) . . . . ? N4 C14 C15 N5 55(2) . . . . ? C19 C14 C15 N5 175.8(19) . . . . ? C14 C15 C16 C17 57(3) . . . . ? N5 C15 C16 C17 179(2) . . . . ? C15 C16 C17 C18 -54(3) . . . . ? C16 C17 C18 C19 55(3) . . . . ? C17 C18 C19 C14 -55(3) . . . . ? C15 C14 C19 C18 58(3) . . . . ? N4 C14 C19 C18 176(3) . . . . ? N7 C20 C21 C26 179(2) . . . . ? O7 C20 C21 C26 0(3) . . . . ? N7 C20 C21 C22 3(3) . . . . ? O7 C20 C21 C22 -176.0(19) . . . . ? C26 C21 C22 C23 1(3) . . . . ? C20 C21 C22 C23 177(2) . . . . ? C26 C21 C22 Pt3 177.2(19) . . . . ? C20 C21 C22 Pt3 -7(2) . . . . ? C21 C22 C23 C24 0(4) . . . . ? Pt3 C22 C23 C24 -175(2) . . . . ? C22 C23 C24 C25 -1(5) . . . . ? C23 C24 C25 C26 2(5) . . . . ? C24 C25 C26 C21 -1(4) . . . . ? C22 C21 C26 C25 0(4) . . . . ? C20 C21 C26 C25 -176(2) . . . . ? C32 C27 C28 C29 -61(4) . . . . ? N8 C27 C28 C29 -179(3) . . . . ? C32 C27 C28 N9 172(3) . . . . ? N8 C27 C28 N9 54(3) . . . . ? C27 C28 C29 C30 45(5) . . . . ? N9 C28 C29 C30 170(4) . . . . ? C28 C29 C30 C31 -51(6) . . . . ? C29 C30 C31 C32 60(5) . . . . ? C28 C27 C32 C31 71(4) . . . . ? N8 C27 C32 C31 -176(3) . . . . ? C30 C31 C32 C27 -68(4) . . . . ? N10 C33 C34 N11 59(3) . . . . ? C38 C33 C34 N11 -179(2) . . . . ? N10 C33 C34 C35 -176(2) . . . . ? C38 C33 C34 C35 -55(3) . . . . ? N11 C34 C35 C36 171(2) . . . . ? C33 C34 C35 C36 51(3) . . . . ? C34 C35 C36 C37 -50(3) . . . . ? C35 C36 C37 C38 46(4) . . . . ? N10 C33 C38 C37 168(3) . . . . ? C34 C33 C38 C37 50(3) . . . . ? C36 C37 C38 C33 -45(4) . . . . ? O2 C1 N1 O1 -4(3) . . . . ? C2 C1 N1 O1 -179.5(18) . . . . ? O2 C1 N1 Pt1 -178.2(16) . . . . ? C2 C1 N1 Pt1 6(2) . . . . ? C9 C8 N2 Pt2 -41(3) . . . . ? C13 C8 N2 Pt2 -160(2) . . . . ? C8 C9 N3 Pt2 -45(3) . . . . ? C10 C9 N3 Pt2 -167(2) . . . . ? C15 C14 N4 Pt1 -46(2) . . . . ? C19 C14 N4 Pt1 -168.0(18) . . . . ? C14 C15 N5 Pt1 -39(2) . . . . ? C16 C15 N5 Pt1 -163.8(18) . . . . ? O7 C20 N7 O6 4(3) . . . . ? C21 C20 N7 O6 -175.1(16) . . . . ? O7 C20 N7 Pt3 -178.7(14) . . . . ? C21 C20 N7 Pt3 3(2) . . . . ? C28 C27 N8 Pt4 -40(3) . . . . ? C32 C27 N8 Pt4 -159(3) . . . . ? C27 C28 N9 Pt4 -44(3) . . . . ? C29 C28 N9 Pt4 -168(3) . . . . ? C38 C33 N10 Pt3 -171(2) . . . . ? C34 C33 N10 Pt3 -44(3) . . . . ? C35 C34 N11 Pt3 -165.3(18) . . . . ? C33 C34 N11 Pt3 -45(2) . . . . ? C1 N1 O1 Pt2 4(2) . . . . ? Pt1 N1 O1 Pt2 178.1(11) . . . . ? N1 C1 O2 Pt2 2(3) . . . . ? C2 C1 O2 Pt2 176.4(16) . . . . ? C20 N7 O6 Pt4 -4(2) . . . . ? Pt3 N7 O6 Pt4 179.0(8) . . . . ? N7 C20 O7 Pt4 -2(2) . . . . ? C21 C20 O7 Pt4 177.0(15) . . . . ? C1 N1 Pt1 C3 -4.2(17) . . . . ? O1 N1 Pt1 C3 -177.6(19) . . . . ? C1 N1 Pt1 N4 -42(13) . . . . ? O1 N1 Pt1 N4 144(11) . . . . ? C1 N1 Pt1 N5 177.3(17) . . . . ? O1 N1 Pt1 N5 3.8(19) . . . . ? C2 C3 Pt1 N1 0.6(17) . . . . ? C4 C3 Pt1 N1 -177(2) . . . . ? C2 C3 Pt1 N4 178.1(17) . . . . ? C4 C3 Pt1 N4 0(2) . . . . ? C2 C3 Pt1 N5 139(25) . . . . ? C4 C3 Pt1 N5 -39(26) . . . . ? C14 N4 Pt1 N1 -122(12) . . . . ? C14 N4 Pt1 C3 -160.0(17) . . . . ? C14 N4 Pt1 N5 18.6(16) . . . . ? C15 N5 Pt1 N1 -171.9(16) . . . . ? C15 N5 Pt1 C3 50(26) . . . . ? C15 N5 Pt1 N4 10.7(16) . . . . ? C1 O2 Pt2 N2 179.6(14) . . . . ? C1 O2 Pt2 O1 1.0(13) . . . . ? C1 O2 Pt2 N3 58(26) . . . . ? C8 N2 Pt2 O2 -165.0(17) . . . . ? C8 N2 Pt2 O1 -24(23) . . . . ? C8 N2 Pt2 N3 13.1(18) . . . . ? N1 O1 Pt2 O2 -2.8(13) . . . . ? N1 O1 Pt2 N2 -144(22) . . . . ? N1 O1 Pt2 N3 179.1(16) . . . . ? C9 N3 Pt2 O2 139(24) . . . . ? C9 N3 Pt2 N2 17(2) . . . . ? C9 N3 Pt2 O1 -164(2) . . . . ? C23 C22 Pt3 N7 -179(3) . . . . ? C21 C22 Pt3 N7 6.3(15) . . . . ? C23 C22 Pt3 N10 3(3) . . . . ? C21 C22 Pt3 N10 -172.6(16) . . . . ? C23 C22 Pt3 N11 64(16) . . . . ? C21 C22 Pt3 N11 -111(15) . . . . ? C20 N7 Pt3 C22 -5.1(15) . . . . ? O6 N7 Pt3 C22 172.4(16) . . . . ? C20 N7 Pt3 N10 47(46) . . . . ? O6 N7 Pt3 N10 -135(45) . . . . ? C20 N7 Pt3 N11 171.1(14) . . . . ? O6 N7 Pt3 N11 -11.4(15) . . . . ? C33 N10 Pt3 C22 -166(2) . . . . ? C33 N10 Pt3 N7 142(44) . . . . ? C33 N10 Pt3 N11 18(2) . . . . ? C34 N11 Pt3 C22 -45(16) . . . . ? C34 N11 Pt3 N7 -162.0(14) . . . . ? C34 N11 Pt3 N10 16.8(15) . . . . ? C20 O7 Pt4 N8 -178.9(17) . . . . ? C20 O7 Pt4 N9 -79(37) . . . . ? C20 O7 Pt4 O6 -0.3(13) . . . . ? C27 N8 Pt4 O7 -167(2) . . . . ? C27 N8 Pt4 N9 15(3) . . . . ? C27 N8 Pt4 O6 134(38) . . . . ? C28 N9 Pt4 O7 -85(37) . . . . ? C28 N9 Pt4 N8 15(3) . . . . ? C28 N9 Pt4 O6 -164(2) . . . . ? N7 O6 Pt4 O7 2.0(12) . . . . ? N7 O6 Pt4 N8 61(40) . . . . ? N7 O6 Pt4 N9 -179.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 4.890 _refine_diff_density_min -1.452 _refine_diff_density_rms 0.265