Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Celine Marmion' _publ_contact_author_address ; Department of Pharmaceutical & Medicinal Chemistry Royal College of Surgeons in Ireland 123 St Stephens Green Dublin 2 REPUBLIC OF IRELAND ; _publ_contact_author_email CMARMION@RCSI.IE _publ_section_title ; Synthesis, characterisation and speciation studies of heterobimetallic pyridinehydroxamate-bridged Pt(II)/M(II) complexes (M = Cu, Ni, Zn). Crystal structure of a novel heterobimetallic 3-pyridinehydroxamate-bridged Pt(II)/Cu(II) wave-like coordination polymer. ; _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 2.23 e\%A^-3^ near the Pt1 center due to considerable absorption effects which could not be completely corrected ; loop_ _publ_author_name 'Celine Marmion' 'F. M. Dolgushin' 'Darren Griffith' 'Krystyna Krot' 'Clodagh Mulcahy' data_cp15 _database_code_depnum_ccdc_archive 'CCDC 246167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 Cu N6 O4 Pt +2, O4 S -2, 8(H2 O)' _chemical_formula_sum 'C12 H32 Cu N6 O16 Pt S' _chemical_formula_weight 807.13 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 8.268(2) _cell_length_b 10.003(2) _cell_length_c 17.156(4) _cell_angle_alpha 80.524(5) _cell_angle_beta 81.164(5) _cell_angle_gamma 72.404(5) _cell_volume 1325.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1669 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 22.7 _exptl_crystal_description prism _exptl_crystal_colour chlorine _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 6.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.318 _exptl_absorpt_correction_T_max 0.694 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-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 9679 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.1742 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.10 _reflns_number_total 5093 _reflns_number_gt 2777 _reflns_threshold_expression I>2\s(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^)+(0.0642P)^2^+2.3100P] 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 5093 _refine_ls_number_parameters 337 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1402 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.003 _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 0.68000(8) 0.88839(8) 0.27951(3) 0.0374(2) Uani 1 1 d . . . Cu1 Cu 1.5000 0.5000 0.5000 0.0718(12) Uani 1 2 d S . . Cu2 Cu 1.5000 1.0000 0.0000 0.1073(19) Uani 1 2 d S . . O1 O 1.4083(11) 0.6889(10) 0.4518(8) 0.051(3) Uani 1 1 d . . . O2 O 1.3069(14) 0.4660(13) 0.4643(11) 0.091(5) Uani 1 1 d . . . O3 O 1.3777(15) 1.0789(18) 0.0914(6) 0.085(5) Uani 1 1 d . . . O4 O 1.3319(17) 0.899(2) 0.0098(7) 0.113(7) Uani 1 1 d . . . N1 N 0.8259(13) 0.6971(14) 0.3275(8) 0.045(4) Uani 1 1 d . . . C1 C 0.9610(17) 0.7014(18) 0.3588(9) 0.042(4) Uani 1 1 d . . . H1A H 0.9828 0.7895 0.3584 0.051 Uiso 1 1 calc R . . C2 C 1.0708(18) 0.5779(17) 0.3920(14) 0.066(6) Uani 1 1 d . . . C3 C 1.034(2) 0.448(2) 0.3948(19) 0.110(11) Uani 1 1 d . . . H3A H 1.1027 0.3625 0.4200 0.132 Uiso 1 1 calc R . . C4 C 0.892(2) 0.451(2) 0.3588(19) 0.112(11) Uani 1 1 d U . . H4A H 0.8685 0.3656 0.3540 0.135 Uiso 1 1 calc R . . C5 C 0.788(2) 0.576(2) 0.3310(14) 0.073(7) Uani 1 1 d . . . H5A H 0.6842 0.5785 0.3133 0.087 Uiso 1 1 calc R . . N3 N 0.8262(17) 0.8501(19) 0.1766(7) 0.066(5) Uani 1 1 d . . . C7 C 0.958(2) 0.905(3) 0.1563(9) 0.089(9) Uani 1 1 d . . . H7A H 0.9764 0.9619 0.1914 0.107 Uiso 1 1 calc R . . C8 C 1.068(3) 0.884(3) 0.0891(9) 0.098(10) Uani 1 1 d . . . C9 C 1.040(3) 0.799(3) 0.0356(11) 0.125(12) Uani 1 1 d . . . H9A H 1.1190 0.7728 -0.0095 0.150 Uiso 1 1 calc R . . C10 C 0.897(3) 0.758(3) 0.0522(13) 0.133(13) Uani 1 1 d . . . H10A H 0.8684 0.7097 0.0152 0.160 Uiso 1 1 calc R . . C11 C 0.788(2) 0.784(3) 0.1237(10) 0.091(9) Uani 1 1 d . . . H11A H 0.6878 0.7540 0.1340 0.109 Uiso 1 1 calc R . . N2 N 1.2664(14) 0.6932(13) 0.4199(9) 0.045(4) Uani 1 1 d . . . H2A H 1.2080 0.7727 0.3945 0.054 Uiso 1 1 calc R . . N4 N 1.234(2) 1.024(2) 0.1120(8) 0.098(8) Uani 1 1 d . . . H4B H 1.1609 1.0482 0.1537 0.117 Uiso 1 1 calc R . . N5 N 0.5473(13) 0.9214(12) 0.3862(6) 0.027(3) Uani 1 1 d . . . H5B H 0.5013 0.8489 0.4051 0.040 Uiso 1 1 d R . . H5C H 0.4623 1.0040 0.3813 0.040 Uiso 1 1 d R . . H5D H 0.6183 0.9264 0.4206 0.040 Uiso 1 1 d R . . N6 N 0.5432(15) 1.0785(14) 0.2306(7) 0.043(4) Uani 1 1 d . . . H6A H 0.4830 1.0665 0.1934 0.065 Uiso 1 1 d R . . H6B H 0.6153 1.1302 0.2071 0.065 Uiso 1 1 d R . . H6C H 0.4698 1.1249 0.2691 0.065 Uiso 1 1 d R . . C6 C 1.218(2) 0.5834(19) 0.4266(14) 0.068(6) Uani 1 1 d . . . C12 C 1.216(3) 0.942(3) 0.0690(9) 0.096(9) Uani 1 1 d . . . S1 S 1.1051(4) 1.0730(4) 0.3187(2) 0.0310(9) Uani 1 1 d . . . O1S O 1.2213(12) 1.1321(10) 0.3490(5) 0.034(2) Uani 1 1 d . . . O2S O 0.9494(12) 1.0845(12) 0.3729(5) 0.044(3) Uani 1 1 d . . . O3S O 1.1884(12) 0.9238(11) 0.3062(5) 0.037(2) Uani 1 1 d . . . O4S O 1.0656(13) 1.1540(13) 0.2392(6) 0.049(3) Uani 1 1 d . . . O1W O 0.8073(13) 0.9082(12) 0.4850(6) 0.049(3) Uani 1 1 d . . . O2W O 0.3994(15) 0.7755(12) 0.6180(8) 0.066(4) Uani 1 1 d . . . O3W O 0.5730(15) 0.2777(16) 0.7920(8) 0.076(4) Uani 1 1 d . . . O4W O 0.2307(15) 0.7442(15) 0.8368(7) 0.071(4) Uani 1 1 d . . . O5W O 0.571(2) 0.5493(16) 0.7248(12) 0.117(7) Uani 1 1 d . . . O6W O 0.338(4) 0.400(2) 1.0549(12) 0.185(11) Uani 1 1 d . . . O7W O 0.422(3) 0.479(2) 0.9024(9) 0.134(7) Uani 1 1 d . . . O8W O 0.828(4) 0.589(3) 0.7950(16) 0.253(18) 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 0.0385(4) 0.0619(5) 0.0246(3) -0.0176(3) 0.0098(2) -0.0333(3) Cu1 0.0195(14) 0.0255(19) 0.164(4) 0.002(2) -0.0038(18) -0.0078(13) Cu2 0.074(2) 0.275(6) 0.0239(16) -0.044(2) 0.0232(15) -0.125(3) O1 0.018(5) 0.018(6) 0.112(10) -0.008(6) 0.004(6) -0.003(5) O2 0.034(7) 0.028(8) 0.214(18) -0.007(9) -0.019(9) -0.017(6) O3 0.069(8) 0.209(17) 0.021(6) -0.021(8) 0.009(5) -0.107(10) O4 0.086(9) 0.28(2) 0.035(7) -0.058(10) 0.033(7) -0.140(13) N1 0.014(6) 0.043(9) 0.083(10) -0.044(8) 0.023(6) -0.010(6) C1 0.018(7) 0.047(12) 0.069(11) -0.039(9) 0.018(7) -0.015(8) C2 0.015(8) 0.017(10) 0.16(2) -0.026(11) 0.015(10) -0.006(7) C3 0.029(10) 0.022(12) 0.27(3) -0.025(16) -0.016(15) 0.004(9) C4 0.041(12) 0.016(12) 0.28(3) -0.056(16) -0.003(16) 0.004(9) C5 0.031(9) 0.057(14) 0.15(2) -0.063(14) 0.020(11) -0.028(10) N3 0.068(9) 0.156(17) 0.016(6) -0.038(8) 0.020(6) -0.091(11) C7 0.080(13) 0.22(3) 0.020(9) -0.046(12) 0.033(8) -0.117(17) C8 0.084(14) 0.24(3) 0.028(9) -0.063(14) 0.033(9) -0.128(18) C9 0.097(16) 0.30(4) 0.048(12) -0.101(18) 0.054(11) -0.15(2) C10 0.095(16) 0.30(4) 0.078(15) -0.14(2) 0.063(12) -0.13(2) C11 0.080(14) 0.21(3) 0.037(10) -0.055(14) 0.024(9) -0.112(17) N2 0.013(6) 0.015(8) 0.098(11) -0.003(7) 0.004(6) 0.001(5) N4 0.070(11) 0.24(2) 0.027(8) -0.033(11) 0.014(7) -0.110(14) N5 0.021(6) 0.039(8) 0.028(6) -0.004(6) 0.005(5) -0.025(6) N6 0.045(8) 0.073(11) 0.023(7) 0.018(7) -0.016(6) -0.041(8) C6 0.028(9) 0.016(11) 0.15(2) -0.001(11) -0.005(11) 0.000(8) C12 0.096(15) 0.23(3) 0.015(9) -0.034(13) 0.019(9) -0.126(18) S1 0.036(2) 0.045(3) 0.0203(18) -0.0017(17) -0.0008(15) -0.0251(19) O1S 0.043(6) 0.031(6) 0.037(6) -0.001(5) -0.006(5) -0.023(5) O2S 0.042(6) 0.058(8) 0.026(5) 0.022(5) -0.002(5) -0.021(6) O3S 0.047(6) 0.042(7) 0.032(5) -0.014(5) 0.001(5) -0.024(5) O4S 0.057(7) 0.068(9) 0.032(6) 0.007(6) -0.011(5) -0.037(6) O1W 0.051(7) 0.065(8) 0.039(6) -0.007(6) -0.012(5) -0.026(6) O2W 0.060(8) 0.040(8) 0.107(11) -0.013(7) -0.027(8) -0.018(6) O3W 0.053(7) 0.111(12) 0.084(9) -0.056(9) 0.029(7) -0.049(8) O4W 0.072(8) 0.114(12) 0.049(7) 0.022(7) -0.018(6) -0.068(8) O5W 0.122(13) 0.050(11) 0.201(19) 0.002(11) -0.083(14) -0.031(9) O6W 0.32(3) 0.18(2) 0.108(15) 0.071(15) -0.121(19) -0.16(2) O7W 0.22(2) 0.128(17) 0.071(11) -0.020(11) 0.040(12) -0.089(15) O8W 0.39(4) 0.30(3) 0.20(2) 0.15(2) -0.16(3) -0.32(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N3 2.004(11) . ? Pt1 N5 2.007(10) . ? Pt1 N6 2.017(12) . ? Pt1 N1 2.046(14) . ? Cu1 O1 1.908(10) . ? Cu1 O1 1.908(10) 2_866 ? Cu1 O2 1.933(12) 2_866 ? Cu1 O2 1.933(12) . ? Cu2 O3 1.882(12) 2_875 ? Cu2 O3 1.882(12) . ? Cu2 O4 1.924(12) 2_875 ? Cu2 O4 1.924(12) . ? O1 N2 1.356(15) . ? O2 C6 1.31(2) . ? O3 N4 1.422(17) . ? O4 C12 1.31(2) . ? N1 C5 1.32(2) . ? N1 C1 1.326(17) . ? C1 C2 1.39(2) . ? C2 C3 1.41(2) . ? C2 C6 1.45(2) . ? C3 C4 1.40(3) . ? C4 C5 1.34(3) . ? N3 C11 1.329(19) . ? N3 C7 1.341(19) . ? C7 C8 1.36(2) . ? C8 C9 1.44(2) . ? C8 C12 1.48(2) . ? C9 C10 1.34(2) . ? C10 C11 1.42(2) . ? N2 C6 1.26(2) . ? N4 C12 1.25(3) . ? S1 O2S 1.453(10) . ? S1 O1S 1.464(9) . ? S1 O3S 1.479(11) . ? S1 O4S 1.494(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pt1 N5 176.3(5) . . ? N3 Pt1 N6 91.9(6) . . ? N5 Pt1 N6 90.9(5) . . ? N3 Pt1 N1 86.8(6) . . ? N5 Pt1 N1 90.3(5) . . ? N6 Pt1 N1 178.1(5) . . ? O1 Cu1 O1 180.000(2) . 2_866 ? O1 Cu1 O2 95.8(5) . 2_866 ? O1 Cu1 O2 84.2(5) 2_866 2_866 ? O1 Cu1 O2 84.2(5) . . ? O1 Cu1 O2 95.8(5) 2_866 . ? O2 Cu1 O2 180.000(1) 2_866 . ? O3 Cu2 O3 180.000(2) 2_875 . ? O3 Cu2 O4 86.1(5) 2_875 2_875 ? O3 Cu2 O4 93.9(5) . 2_875 ? O3 Cu2 O4 93.9(5) 2_875 . ? O3 Cu2 O4 86.1(5) . . ? O4 Cu2 O4 180.000(2) 2_875 . ? N2 O1 Cu1 107.6(8) . . ? C6 O2 Cu1 109.1(11) . . ? N4 O3 Cu2 106.7(10) . . ? C12 O4 Cu2 108.0(12) . . ? C5 N1 C1 120.8(16) . . ? C5 N1 Pt1 123.9(12) . . ? C1 N1 Pt1 115.2(11) . . ? N1 C1 C2 120.3(15) . . ? C1 C2 C3 119.4(16) . . ? C1 C2 C6 120.1(15) . . ? C3 C2 C6 120.5(17) . . ? C4 C3 C2 117.1(19) . . ? C5 C4 C3 119.3(18) . . ? N1 C5 C4 122.6(17) . . ? C11 N3 C7 118.1(13) . . ? C11 N3 Pt1 122.7(10) . . ? C7 N3 Pt1 118.9(10) . . ? N3 C7 C8 124.4(16) . . ? C7 C8 C9 117.8(15) . . ? C7 C8 C12 123.6(16) . . ? C9 C8 C12 118.6(15) . . ? C10 C9 C8 117.1(16) . . ? C9 C10 C11 121.3(16) . . ? N3 C11 C10 120.6(15) . . ? C6 N2 O1 120.1(14) . . ? C12 N4 O3 118.0(15) . . ? N2 C6 O2 119.1(16) . . ? N2 C6 C2 123.5(17) . . ? O2 C6 C2 117.4(16) . . ? N4 C12 O4 121.0(16) . . ? N4 C12 C8 118.9(16) . . ? O4 C12 C8 120.0(18) . . ? O2S S1 O1S 110.5(6) . . ? O2S S1 O3S 110.3(6) . . ? O1S S1 O3S 110.7(6) . . ? O2S S1 O4S 110.5(6) . . ? O1S S1 O4S 107.5(6) . . ? O3S S1 O4S 107.2(6) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.10 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.234 _refine_diff_density_min -1.863 _refine_diff_density_rms 0.256