Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Dr Celine Marmion ' _publ_contact_author_address ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; _publ_contact_author_phone ' 353 1 402 2161 ' _publ_contact_author_fax ' 353 1 402 2168 ' _publ_contact_author_email ' cmarmion@rcsi.ie ' loop_ _publ_author_name _publ_author_address ' Celine Marmiom' ; Centre for Synthesis and Chemical Biology, Department of Pharmaceutical and Medicinal Chemistry, Royal College of Surgeons in Ireland, 123 St. Stephen's Green, Dublin 2, Ireland ; ' Darren Griffith' ; Centre for Synthesis and Chemical Biology, Department of Pharmaceutical and Medicinal Chemistry, Royal College of Surgeons in Ireland, 123 St. Stephen's Green, Dublin 2, Ireland ; ' Paul E. Kruger ' ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; ' Paul Jensen ' ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; ' Konstantin Lyssenko ' ; X-ray Structural Centre of the Russian Academy of Sciences, Institute of Organoelement Compounds, 28 Vavilov St., Moscow 117813, Russia ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Novel platinum(II) ammine hydroxamate and hydroximate complexes and the platinum-assisted hydrolysis of hydroxamic acids ; data_1 _database_code_depnum_ccdc_archive 'CCDC 260887' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Cl4 N O2 Pt -1, C6 H6 N O2 +1, H2 O' _chemical_formula_sum 'C12 H12 Cl4 N2 O5 Pt' _chemical_formula_weight 601.13 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 7.760(2) _cell_length_b 8.530(2) _cell_length_c 14.599(4) _cell_angle_alpha 96.943(6) _cell_angle_beta 102.772(6) _cell_angle_gamma 111.955(5) _cell_volume 851.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 8.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.531 _exptl_absorpt_correction_T_max 0.842 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8678 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 28.07 _reflns_number_total 4008 _reflns_number_gt 3336 _reflns_threshold_expression I>2s(I) _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0320P)^2^+0.0500P] 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 4008 _refine_ls_number_parameters 219 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0727 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.42152(3) 0.65140(3) 0.273775(15) 0.02449(8) Uani 1 1 d . . . Cl1 Cl 0.4133(2) 0.45933(19) 0.37085(10) 0.0321(3) Uani 1 1 d . . . Cl2 Cl 0.5261(2) 0.86765(18) 0.40959(10) 0.0292(3) Uani 1 1 d . . . Cl3 Cl 0.09997(19) 0.59515(18) 0.25898(10) 0.0280(3) Uani 1 1 d . . . Cl4 Cl 0.7373(2) 0.7032(2) 0.27889(10) 0.0309(3) Uani 1 1 d . . . O1 O 0.4256(5) 0.8209(5) 0.1851(2) 0.0226(8) Uani 1 1 d . . . O2 O 0.3494(7) 0.8300(6) 0.0334(3) 0.0419(11) Uani 1 1 d . . . O3 O 0.1059(6) 0.9098(6) -0.1616(3) 0.0398(11) Uani 1 1 d D . . O4 O 0.3235(6) 0.7925(5) -0.1514(3) 0.0337(9) Uani 1 1 d D . . H4O H 0.3044 0.7958 -0.0962 0.05(2) Uiso 1 1 d R . . N1 N 0.3297(6) 0.4761(6) 0.1452(3) 0.0201(9) Uani 1 1 d . . . N2 N 0.0221(7) 0.8421(6) -0.3564(3) 0.0275(10) Uani 1 1 d . . . H2N H -0.0361 0.8895 -0.3169 0.004(11) Uiso 1 1 d R . . C1 C 0.3092(8) 0.5550(7) 0.0697(4) 0.0266(12) Uani 1 1 d . . . C2 C 0.2448(9) 0.4596(8) -0.0234(4) 0.0344(14) Uani 1 1 d . . . H2A H 0.2269 0.5109 -0.0753 0.041 Uiso 1 1 calc R . . C3 C 0.2066(9) 0.2813(8) -0.0382(4) 0.0326(13) Uani 1 1 d . . . H3A H 0.1633 0.2134 -0.1003 0.039 Uiso 1 1 calc R . . C4 C 0.2341(9) 0.2091(8) 0.0403(4) 0.0320(13) Uani 1 1 d . . . H4A H 0.2122 0.0927 0.0313 0.038 Uiso 1 1 calc R . . C5 C 0.2944(8) 0.3104(7) 0.1327(4) 0.0287(12) Uani 1 1 d . . . H5A H 0.3099 0.2613 0.1858 0.034 Uiso 1 1 calc R . . C6 C 0.3615(9) 0.7467(8) 0.0953(4) 0.0290(12) Uani 1 1 d . . . C7 C 0.1622(8) 0.8037(7) -0.3041(4) 0.0239(11) Uani 1 1 d D . . C8 C 0.2542(9) 0.7236(7) -0.3501(4) 0.0291(12) Uani 1 1 d . . . H8A H 0.3455 0.6911 -0.3148 0.035 Uiso 1 1 calc R . . C9 C 0.2091(9) 0.6920(7) -0.4499(4) 0.0316(13) Uani 1 1 d . . . H9A H 0.2728 0.6416 -0.4822 0.038 Uiso 1 1 calc R . . C10 C 0.0682(9) 0.7366(7) -0.5004(4) 0.0310(13) Uani 1 1 d . . . H10A H 0.0380 0.7173 -0.5672 0.037 Uiso 1 1 calc R . . C11 C -0.0268(9) 0.8084(8) -0.4534(5) 0.0341(14) Uani 1 1 d . . . H11A H -0.1249 0.8341 -0.4880 0.041 Uiso 1 1 calc R . . C12 C 0.1920(7) 0.8432(5) -0.1963(4) 0.054(2) Uani 1 1 d D . . O1W O 0.2161(7) 1.0201(6) 0.3040(4) 0.0501(13) Uani 1 1 d . . . H1WB H 0.3282 1.0427 0.3405 0.080 Uiso 1 1 d R . . H1WA H 0.1761 0.9103 0.2925 0.080 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 0.02719(12) 0.02617(12) 0.02137(12) 0.00474(8) 0.00716(8) 0.01251(9) Cl1 0.0393(8) 0.0342(8) 0.0281(7) 0.0102(6) 0.0112(6) 0.0191(6) Cl2 0.0333(7) 0.0300(7) 0.0231(6) 0.0018(6) 0.0081(6) 0.0130(6) Cl3 0.0249(6) 0.0300(7) 0.0290(7) 0.0022(6) 0.0078(5) 0.0127(6) Cl4 0.0250(7) 0.0414(8) 0.0282(7) 0.0056(6) 0.0087(5) 0.0156(6) O1 0.0283(19) 0.0230(19) 0.0158(17) 0.0023(15) 0.0059(15) 0.0108(16) O2 0.069(3) 0.035(2) 0.024(2) 0.0078(19) 0.009(2) 0.027(2) O3 0.042(3) 0.040(3) 0.039(3) 0.010(2) 0.019(2) 0.014(2) O4 0.047(3) 0.036(2) 0.023(2) 0.0092(18) 0.0134(19) 0.021(2) N1 0.015(2) 0.033(3) 0.014(2) 0.0080(18) 0.0032(16) 0.0118(19) N2 0.027(2) 0.022(2) 0.028(3) 0.011(2) 0.007(2) 0.003(2) C1 0.029(3) 0.024(3) 0.027(3) 0.005(2) 0.010(2) 0.011(2) C2 0.034(3) 0.040(4) 0.027(3) 0.003(3) 0.007(3) 0.016(3) C3 0.038(3) 0.031(3) 0.025(3) 0.001(2) 0.008(3) 0.012(3) C4 0.036(3) 0.027(3) 0.030(3) 0.000(2) 0.008(3) 0.014(3) C5 0.030(3) 0.025(3) 0.032(3) 0.005(2) 0.010(2) 0.012(2) C6 0.038(3) 0.027(3) 0.023(3) 0.004(2) 0.006(2) 0.017(3) C7 0.034(3) 0.015(3) 0.024(3) 0.005(2) 0.011(2) 0.010(2) C8 0.035(3) 0.027(3) 0.030(3) 0.007(2) 0.012(2) 0.016(3) C9 0.041(3) 0.023(3) 0.030(3) 0.001(2) 0.014(3) 0.011(3) C10 0.036(3) 0.025(3) 0.024(3) 0.006(2) 0.006(2) 0.005(3) C11 0.033(3) 0.028(3) 0.035(3) 0.009(3) 0.005(3) 0.009(3) C12 0.059(4) 0.132(8) 0.020(3) 0.039(4) 0.026(3) 0.076(5) O1W 0.047(3) 0.036(3) 0.066(3) 0.006(2) 0.008(2) 0.023(2) _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 N1 2.050(4) . ? Pt1 O1 2.050(4) . ? Pt1 Cl1 2.2848(15) . ? Pt1 Cl2 2.2974(14) . ? Pt1 Cl4 2.3035(15) . ? Pt1 Cl3 2.3118(15) . ? O1 C6 1.282(6) . ? O2 C6 1.223(7) . ? O3 C12 1.179(7) . ? O4 C12 1.326(7) . ? N1 C5 1.317(7) . ? N1 C1 1.369(7) . ? N2 C11 1.347(8) . ? N2 C7 1.354(7) . ? C1 C2 1.374(8) . ? C1 C6 1.506(8) . ? C2 C3 1.415(9) . ? C3 C4 1.378(8) . ? C4 C5 1.386(8) . ? C7 C8 1.376(8) . ? C7 C12 1.515(8) . ? C8 C9 1.388(8) . ? C9 C10 1.380(8) . ? C10 C11 1.360(9) . ? 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 Pt1 O1 82.45(16) . . ? N1 Pt1 Cl1 96.83(13) . . ? O1 Pt1 Cl1 179.16(11) . . ? N1 Pt1 Cl2 174.57(13) . . ? O1 Pt1 Cl2 92.12(11) . . ? Cl1 Pt1 Cl2 88.61(6) . . ? N1 Pt1 Cl4 88.99(12) . . ? O1 Pt1 Cl4 89.42(11) . . ? Cl1 Pt1 Cl4 90.98(5) . . ? Cl2 Pt1 Cl4 90.88(5) . . ? N1 Pt1 Cl3 88.06(12) . . ? O1 Pt1 Cl3 88.66(11) . . ? Cl1 Pt1 Cl3 90.90(5) . . ? Cl2 Pt1 Cl3 91.91(5) . . ? Cl4 Pt1 Cl3 176.67(5) . . ? C6 O1 Pt1 113.3(3) . . ? C5 N1 C1 122.5(5) . . ? C5 N1 Pt1 127.0(4) . . ? C1 N1 Pt1 110.4(4) . . ? C11 N2 C7 121.6(5) . . ? N1 C1 C2 120.0(5) . . ? N1 C1 C6 116.5(5) . . ? C2 C1 C6 123.6(5) . . ? C1 C2 C3 118.3(6) . . ? C4 C3 C2 119.5(6) . . ? C3 C4 C5 119.8(6) . . ? N1 C5 C4 119.9(5) . . ? O2 C6 O1 121.0(5) . . ? O2 C6 C1 121.8(5) . . ? O1 C6 C1 117.1(5) . . ? N2 C7 C8 119.9(5) . . ? N2 C7 C12 114.4(5) . . ? C8 C7 C12 125.5(5) . . ? C7 C8 C9 119.2(6) . . ? C10 C9 C8 119.0(5) . . ? C11 C10 C9 120.6(6) . . ? N2 C11 C10 119.6(6) . . ? O3 C12 O4 127.7(5) . . ? O3 C12 C7 122.1(5) . . ? O4 C12 C7 110.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 O1 C6 4.2(4) . . . . ? Cl1 Pt1 O1 C6 -26(8) . . . . ? Cl2 Pt1 O1 C6 -175.9(4) . . . . ? Cl4 Pt1 O1 C6 93.2(4) . . . . ? Cl3 Pt1 O1 C6 -84.0(4) . . . . ? O1 Pt1 N1 C5 176.6(5) . . . . ? Cl1 Pt1 N1 C5 -3.8(4) . . . . ? Cl2 Pt1 N1 C5 175.7(10) . . . . ? Cl4 Pt1 N1 C5 87.1(4) . . . . ? Cl3 Pt1 N1 C5 -94.5(4) . . . . ? O1 Pt1 N1 C1 -3.0(3) . . . . ? Cl1 Pt1 N1 C1 176.6(3) . . . . ? Cl2 Pt1 N1 C1 -3.9(15) . . . . ? Cl4 Pt1 N1 C1 -92.6(3) . . . . ? Cl3 Pt1 N1 C1 85.9(3) . . . . ? C5 N1 C1 C2 1.7(8) . . . . ? Pt1 N1 C1 C2 -178.6(4) . . . . ? C5 N1 C1 C6 -178.0(5) . . . . ? Pt1 N1 C1 C6 1.7(6) . . . . ? N1 C1 C2 C3 -1.8(8) . . . . ? C6 C1 C2 C3 177.9(5) . . . . ? C1 C2 C3 C4 0.2(9) . . . . ? C2 C3 C4 C5 1.5(9) . . . . ? C1 N1 C5 C4 0.0(8) . . . . ? Pt1 N1 C5 C4 -179.5(4) . . . . ? C3 C4 C5 N1 -1.6(9) . . . . ? Pt1 O1 C6 O2 177.8(5) . . . . ? Pt1 O1 C6 C1 -4.4(6) . . . . ? N1 C1 C6 O2 179.6(5) . . . . ? C2 C1 C6 O2 0.0(9) . . . . ? N1 C1 C6 O1 1.9(8) . . . . ? C2 C1 C6 O1 -177.8(5) . . . . ? C11 N2 C7 C8 -1.9(8) . . . . ? C11 N2 C7 C12 -177.5(4) . . . . ? N2 C7 C8 C9 3.5(8) . . . . ? C12 C7 C8 C9 178.5(4) . . . . ? C7 C8 C9 C10 -2.2(9) . . . . ? C8 C9 C10 C11 -0.8(9) . . . . ? C7 N2 C11 C10 -1.1(8) . . . . ? C9 C10 C11 N2 2.4(9) . . . . ? N2 C7 C12 O3 -3.5(4) . . . . ? C8 C7 C12 O3 -178.8(5) . . . . ? N2 C7 C12 O4 176.4(4) . . . . ? C8 C7 C12 O4 1.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.628 _refine_diff_density_min -1.893 _refine_diff_density_rms 0.172 _publ_section_references ; Bruker (1998a) SAINTPlus Data Reduction and Correction Program v. 6.01, Bruker AXS, Madison, Wisconsin, USA. Bruker (1998b) SMART. Bruker Molecular Analysis Research Tool, v. 5.059. Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998b). SHELXTL v. 5.10, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; There is a high positive residual density of 1.68 e\%A^-3^ near the O3 center due to considerable absorption effects which could not be completely corrected ; data_3 _database_code_depnum_ccdc_archive 'CCDC 260888' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pt2(NH3)4(C6H4N2O2)](ClO4)2.H2O' _chemical_formula_sum 'C6 H18 Cl2 N6 O11 Pt2' _chemical_formula_weight 811.34 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 22.6328(10) _cell_length_b 11.1671(5) _cell_length_c 14.4022(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.0070(10) _cell_angle_gamma 90.00 _cell_volume 3595.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 15.913 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.217 _exptl_absorpt_correction_T_max 0.626 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _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 'Bruker SMART APEX CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22557 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4129 _reflns_number_gt 3416 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+33.1808P] 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 4129 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.442567(17) 0.64203(3) 0.56617(2) 0.02124(12) Uani 1 1 d . . . Pt2 Pt 0.630322(17) 0.57227(4) 0.74163(3) 0.02391(12) Uani 1 1 d . . . Cl1 Cl 0.59846(13) 1.0110(2) 0.6682(2) 0.0345(6) Uani 1 1 d . . . Cl2 Cl 0.72191(13) 1.0448(2) 0.4621(2) 0.0339(6) Uani 1 1 d . . . O1 O 0.5597(3) 0.6682(6) 0.6887(5) 0.0242(15) Uani 1 1 d . . . O2 O 0.5775(3) 0.4315(6) 0.6976(5) 0.0237(15) Uani 1 1 d . . . O3 O 0.6081(5) 1.1322(8) 0.6984(10) 0.080(4) Uani 1 1 d . . . O4 O 0.6540(5) 0.9556(10) 0.6595(9) 0.070(3) Uani 1 1 d . . . O5 O 0.5715(5) 0.9436(11) 0.7312(7) 0.071(3) Uani 1 1 d . . . O6 O 0.5606(4) 1.0103(9) 0.5789(6) 0.054(2) Uani 1 1 d . . . O7 O 0.7530(5) 1.0720(9) 0.3851(7) 0.055(3) Uani 1 1 d . . . O8 O 0.7462(5) 1.1169(8) 0.5408(7) 0.054(3) Uani 1 1 d . . . O9 O 0.6615(4) 1.0720(10) 0.4353(7) 0.057(3) Uani 1 1 d . . . O10 O 0.7307(5) 0.9207(8) 0.4841(7) 0.053(3) Uani 1 1 d . . . O11 O 0.7113(4) 0.7914(8) 0.3076(7) 0.047(2) Uani 1 1 d . . . N1 N 0.5149(4) 0.5896(8) 0.6490(5) 0.0218(17) Uani 1 1 d . . . N3 N 0.4633(4) 0.8197(8) 0.5938(7) 0.030(2) Uani 1 1 d . . . N4 N 0.3705(4) 0.6912(9) 0.4667(7) 0.035(2) Uani 1 1 d . . . N5 N 0.7037(4) 0.4707(8) 0.7926(7) 0.034(2) Uani 1 1 d . . . N6 N 0.6798(4) 0.7226(8) 0.7769(7) 0.034(2) Uani 1 1 d . . . C1 C 0.5264(5) 0.4763(9) 0.6553(7) 0.023(2) Uani 1 1 d . . . N2 N 0.4324(3) 0.4615(4) 0.5562(5) 0.0323(10) Uani 1 1 d G . . C2 C 0.4786(3) 0.3997(6) 0.6108(4) 0.0323(10) Uani 1 1 d G . . C3 C 0.4762(3) 0.2757(6) 0.6176(4) 0.0323(10) Uani 1 1 d G . . H3 H 0.5077 0.2334 0.6549 0.039 Uiso 1 1 calc R . . C4 C 0.4275(3) 0.2135(4) 0.5698(5) 0.0323(10) Uani 1 1 d G . . H4 H 0.4258 0.1287 0.5744 0.039 Uiso 1 1 calc R . . C5 C 0.3813(3) 0.2753(6) 0.5151(5) 0.0323(10) Uani 1 1 d G . . H5 H 0.3480 0.2328 0.4825 0.039 Uiso 1 1 calc R . . C6 C 0.3837(3) 0.3993(6) 0.5084(4) 0.0323(10) Uani 1 1 d G . . H6 H 0.3521 0.4416 0.4710 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0195(2) 0.0256(2) 0.01939(19) -0.00050(14) 0.00548(14) 0.00276(15) Pt2 0.0222(2) 0.0261(2) 0.0236(2) 0.00094(15) 0.00395(15) 0.00151(15) Cl1 0.0346(15) 0.0282(13) 0.0395(15) 0.0082(11) 0.0024(12) -0.0007(11) Cl2 0.0306(14) 0.0358(14) 0.0345(14) 0.0023(11) 0.0028(11) 0.0007(11) O1 0.021(4) 0.022(3) 0.030(4) -0.001(3) 0.003(3) -0.001(3) O2 0.022(4) 0.021(3) 0.029(4) 0.004(3) 0.005(3) 0.003(3) O3 0.059(7) 0.034(5) 0.134(11) -0.015(6) -0.027(7) -0.004(5) O4 0.051(7) 0.078(8) 0.079(8) 0.014(6) 0.010(6) 0.020(6) O5 0.074(8) 0.097(9) 0.039(5) 0.022(6) 0.005(5) -0.035(7) O6 0.055(6) 0.061(6) 0.041(5) 0.011(5) -0.005(4) -0.003(5) O7 0.051(6) 0.064(6) 0.051(6) 0.008(5) 0.008(5) -0.003(5) O8 0.073(7) 0.037(5) 0.049(6) -0.006(4) 0.001(5) -0.013(5) O9 0.031(5) 0.089(8) 0.050(6) 0.011(5) 0.000(4) 0.016(5) O10 0.067(7) 0.037(5) 0.053(6) 0.004(4) 0.000(5) 0.015(5) O11 0.042(5) 0.037(5) 0.065(6) -0.004(4) 0.014(4) -0.004(4) N1 0.012(4) 0.034(5) 0.019(4) -0.003(3) -0.001(3) -0.002(3) N3 0.026(5) 0.029(5) 0.034(5) -0.003(4) -0.001(4) 0.000(4) N4 0.028(5) 0.041(5) 0.032(5) -0.003(4) -0.005(4) 0.002(4) N5 0.033(5) 0.029(5) 0.041(5) -0.002(4) 0.006(4) 0.007(4) N6 0.030(5) 0.025(5) 0.043(5) -0.002(4) -0.002(4) -0.003(4) C1 0.025(5) 0.027(5) 0.020(5) -0.006(4) 0.010(4) 0.001(4) N2 0.039(3) 0.034(2) 0.029(2) -0.0053(18) 0.0206(19) -0.008(2) C2 0.039(3) 0.034(2) 0.029(2) -0.0053(18) 0.0206(19) -0.008(2) C3 0.039(3) 0.034(2) 0.029(2) -0.0053(18) 0.0206(19) -0.008(2) C4 0.039(3) 0.034(2) 0.029(2) -0.0053(18) 0.0206(19) -0.008(2) C5 0.039(3) 0.034(2) 0.029(2) -0.0053(18) 0.0206(19) -0.008(2) C6 0.039(3) 0.034(2) 0.029(2) -0.0053(18) 0.0206(19) -0.008(2) _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 N1 1.959(8) . ? Pt1 N2 2.032(5) . ? Pt1 N3 2.063(9) . ? Pt1 N4 2.070(9) . ? Pt2 O1 1.976(7) . ? Pt2 O2 2.016(7) . ? Pt2 N6 2.037(9) . ? Pt2 N5 2.050(9) . ? Cl1 O5 1.391(10) . ? Cl1 O4 1.424(11) . ? Cl1 O3 1.428(10) . ? Cl1 O6 1.430(9) . ? Cl2 O9 1.395(9) . ? Cl2 O8 1.428(9) . ? Cl2 O10 1.429(9) . ? Cl2 O7 1.436(10) . ? O1 N1 1.393(10) . ? O2 C1 1.319(12) . ? N1 C1 1.292(13) . ? C1 C2 1.448(11) . ? N2 C2 1.3900 . ? N2 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? 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 Pt1 N2 79.7(3) . . ? N1 Pt1 N3 91.5(4) . . ? N2 Pt1 N3 171.0(3) . . ? N1 Pt1 N4 173.8(4) . . ? N2 Pt1 N4 98.4(3) . . ? N3 Pt1 N4 90.5(4) . . ? O1 Pt2 O2 84.1(3) . . ? O1 Pt2 N6 91.7(3) . . ? O2 Pt2 N6 175.1(3) . . ? O1 Pt2 N5 178.3(3) . . ? O2 Pt2 N5 95.1(3) . . ? N6 Pt2 N5 89.1(4) . . ? O5 Cl1 O4 107.8(8) . . ? O5 Cl1 O3 112.1(8) . . ? O4 Cl1 O3 110.1(7) . . ? O5 Cl1 O6 108.8(6) . . ? O4 Cl1 O6 109.3(7) . . ? O3 Cl1 O6 108.7(7) . . ? O9 Cl2 O8 109.6(7) . . ? O9 Cl2 O10 111.7(7) . . ? O8 Cl2 O10 110.4(6) . . ? O9 Cl2 O7 108.6(6) . . ? O8 Cl2 O7 108.6(6) . . ? O10 Cl2 O7 108.0(6) . . ? N1 O1 Pt2 108.0(5) . . ? C1 O2 Pt2 106.4(6) . . ? C1 N1 O1 117.6(8) . . ? C1 N1 Pt1 118.3(7) . . ? O1 N1 Pt1 123.1(6) . . ? N1 C1 O2 123.8(9) . . ? N1 C1 C2 114.8(9) . . ? O2 C1 C2 121.4(8) . . ? C2 N2 C6 120.0 . . ? C2 N2 Pt1 112.7(4) . . ? C6 N2 Pt1 127.1(4) . . ? N2 C2 C3 120.0 . . ? N2 C2 C1 113.6(6) . . ? C3 C2 C1 126.4(6) . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 N2 120.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 6.589 _refine_diff_density_min -1.157 _refine_diff_density_rms 0.322