# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'B Lippert' _publ_contact_author_email BERNHARD.LIPPERT@UNI-DORTMUND.DE _publ_section_title ; On the interrelationship of \m-OH bridged dimers, trimers, and tetramers of (en)PtII and their Ag+ adducts ; loop_ _publ_author_name 'B Lippert' 'Eva Freisinger' 'Ralf-Dieter Schnebeck' 'Wei-Zheng Shen.' data_1 _database_code_depnum_ccdc_archive 'CCDC 678549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H18 Ag N6 O8 Pt2, N O3' _chemical_formula_sum 'C4 H18 Ag N7 O11 Pt2' _chemical_formula_weight 838.30 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' Ag Ag -0.8971 1.1015 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.953(3) _cell_length_b 7.833(2) _cell_length_c 16.874(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.58(3) _cell_angle_gamma 90.00 _cell_volume 1700.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3091 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 25.34 _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 17.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0962 _exptl_absorpt_correction_T_max 0.1720 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf-Nonius-KappaCCD _diffrn_measurement_method 'profile fitted' _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3091 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3091 _reflns_number_gt 2560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _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^)+(0.0442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom; H1, H2 difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00054(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3091 _refine_ls_number_parameters 241 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.01794(2) 0.41648(4) 0.715422(17) 0.03005(12) Uani 1 1 d . . . Pt2 Pt -0.08358(2) 0.52234(4) 0.556056(17) 0.02972(12) Uani 1 1 d D . . Ag1 Ag -0.18904(6) 0.53338(12) 0.69242(4) 0.0644(3) Uani 1 1 d . . . O1 O -0.0262(4) 0.2993(6) 0.6090(3) 0.0322(12) Uani 1 1 d D . . O2 O 0.0383(5) 0.6009(7) 0.6347(3) 0.0381(13) Uani 1 1 d D . . H1 H -0.088(4) 0.271(10) 0.583(5) 0.09(4) Uiso 1 1 d D . . H2 H 0.024(12) 0.681(13) 0.670(7) 0.15(6) Uiso 1 1 d D . . N11 N -0.0027(5) 0.2208(8) 0.7893(3) 0.0388(16) Uani 1 1 d . . . H11A H -0.0706 0.2092 0.7948 0.048(9) Uiso 1 1 calc R . . H11B H 0.0197 0.1230 0.7691 0.048(9) Uiso 1 1 calc R . . N12 N 0.0692(5) 0.5409(8) 0.8175(4) 0.0346(15) Uani 1 1 d . . . H12A H 0.1382 0.5579 0.8199 0.048(9) Uiso 1 1 calc R . . H12B H 0.0381 0.6435 0.8181 0.048(9) Uiso 1 1 calc R . . C11 C 0.0583(8) 0.2571(11) 0.8697(5) 0.052(2) Uani 1 1 d . . . H11C H 0.0327 0.1866 0.9105 0.058(10) Uiso 1 1 calc R . . H11D H 0.1312 0.2312 0.8679 0.058(10) Uiso 1 1 calc R . . C12 C 0.0455(8) 0.4383(11) 0.8883(5) 0.050(2) Uani 1 1 d . . . H12C H 0.0925 0.4697 0.9350 0.058(10) Uiso 1 1 calc R . . H12D H -0.0251 0.4601 0.8995 0.058(10) Uiso 1 1 calc R . . N21 N -0.1319(5) 0.7463(8) 0.5061(4) 0.0369(16) Uani 1 1 d . . . H21A H -0.1264 0.8290 0.5433 0.048(9) Uiso 1 1 calc R . . H21B H -0.0918 0.7749 0.4680 0.048(9) Uiso 1 1 calc R . . N22 N -0.2031(5) 0.4283(8) 0.4788(4) 0.0382(16) Uani 1 1 d . . . H22A H -0.1795 0.3435 0.4497 0.048(9) Uiso 1 1 calc R . . H22B H -0.2523 0.3849 0.5066 0.048(9) Uiso 1 1 calc R . . C21 C -0.2412(7) 0.7305(10) 0.4708(5) 0.043(2) Uani 1 1 d . . . H21C H -0.2602 0.8252 0.4351 0.058(10) Uiso 1 1 calc R . . H21D H -0.2873 0.7294 0.5122 0.058(10) Uiso 1 1 calc R . . C22 C -0.2483(7) 0.5638(11) 0.4255(5) 0.045(2) Uani 1 1 d . . . H22C H -0.3204 0.5377 0.4074 0.058(10) Uiso 1 1 calc R . . H22D H -0.2107 0.5723 0.3791 0.058(10) Uiso 1 1 calc R . . N10 N -0.2810(6) 0.5246(9) 0.8448(4) 0.0425(18) Uani 1 1 d . . . O11 O -0.2780(5) 0.6422(8) 0.7947(3) 0.0526(17) Uani 1 1 d . . . O12 O -0.3321(6) 0.5471(7) 0.9033(4) 0.059(2) Uani 1 1 d . . . O13 O -0.2341(5) 0.3882(8) 0.8372(4) 0.0590(19) Uani 1 1 d . . . N20 N 0.1544(7) 0.9698(9) 0.6765(5) 0.050(2) Uani 1 1 d . . . O21 O 0.2041(6) 1.0819(8) 0.7149(4) 0.065(2) Uani 1 1 d . . . O22 O 0.1877(7) 0.9037(8) 0.6172(5) 0.082(3) Uani 1 1 d . . . O23 O 0.0686(6) 0.9194(8) 0.6976(5) 0.072(2) Uani 1 1 d . . . N30 N -0.4056(7) 0.3745(8) 0.6109(4) 0.058(2) Uani 1 1 d D . . O31 O -0.3514(6) 0.5032(9) 0.6070(5) 0.073(2) Uani 1 1 d D A . O32 O -0.3923(10) 0.2624(11) 0.5621(5) 0.131(4) Uani 1 1 d D A . O33 O -0.4989(9) 0.351(4) 0.614(2) 0.090(10) Uiso 0.27 1 d PD A 1 O33A O -0.4460(11) 0.3493(12) 0.6724(7) 0.096(5) Uani 0.73 1 d PD A 2 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 0.0317(2) 0.02801(18) 0.03143(18) -0.00155(11) 0.00782(13) -0.00035(12) Pt2 0.0337(2) 0.02797(18) 0.02922(17) -0.00186(11) 0.01094(13) -0.00335(13) Ag1 0.0455(5) 0.1086(7) 0.0424(4) 0.0072(4) 0.0196(4) 0.0224(4) O1 0.035(3) 0.029(3) 0.033(3) -0.005(2) 0.008(3) -0.002(2) O2 0.042(4) 0.040(3) 0.033(3) -0.005(2) 0.008(3) -0.003(3) N11 0.048(5) 0.037(4) 0.033(3) -0.006(3) 0.009(3) -0.003(3) N12 0.030(4) 0.034(4) 0.041(4) -0.002(3) 0.009(3) 0.000(3) C11 0.062(7) 0.045(5) 0.046(5) 0.011(4) 0.000(5) -0.003(5) C12 0.059(7) 0.056(6) 0.035(5) -0.003(4) 0.004(4) -0.002(5) N21 0.046(4) 0.033(4) 0.032(3) -0.003(3) 0.008(3) -0.003(3) N22 0.037(4) 0.043(4) 0.035(4) -0.003(3) 0.004(3) 0.000(3) C21 0.046(6) 0.036(5) 0.049(5) 0.010(4) 0.013(4) 0.008(4) C22 0.036(5) 0.061(6) 0.038(5) -0.003(4) 0.000(4) -0.007(4) N10 0.048(5) 0.043(4) 0.038(4) 0.003(3) 0.009(4) -0.001(4) O11 0.064(5) 0.051(4) 0.046(3) 0.012(3) 0.020(3) 0.010(3) O12 0.088(5) 0.048(4) 0.050(4) 0.016(3) 0.041(4) 0.018(4) O13 0.068(5) 0.043(4) 0.071(4) -0.006(3) 0.030(4) 0.017(3) N20 0.062(6) 0.030(4) 0.062(5) 0.000(4) 0.020(4) -0.005(4) O21 0.061(5) 0.056(4) 0.080(5) -0.024(4) 0.017(4) -0.011(4) O22 0.120(7) 0.052(4) 0.089(5) -0.023(4) 0.068(5) -0.025(4) O23 0.070(5) 0.049(4) 0.105(6) -0.024(4) 0.048(5) -0.019(4) N30 0.063(6) 0.043(5) 0.071(6) -0.009(4) 0.022(5) 0.007(4) O31 0.053(5) 0.078(5) 0.089(6) 0.026(4) 0.012(4) -0.017(4) O32 0.242(13) 0.081(6) 0.068(5) -0.013(5) 0.013(7) -0.014(7) O33A 0.148(11) 0.052(6) 0.112(9) -0.024(6) 0.111(10) -0.034(7) _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 2.013(6) . ? Pt1 O2 2.023(5) . ? Pt1 N12 2.024(6) . ? Pt1 O1 2.040(5) . ? Pt1 Ag1 2.8176(10) . ? Pt1 Pt2 2.9729(9) . ? Pt2 N21 2.015(6) . ? Pt2 O2 2.038(6) . ? Pt2 N22 2.043(7) . ? Pt2 O1 2.061(5) . ? Pt2 Ag1 2.8087(10) . ? Pt2 Pt2 3.0542(10) 3_566 ? Pt2 H1 2.02(8) . ? Ag1 O11 2.343(5) . ? Ag1 O31 2.421(8) . ? O1 H1 0.89(2) . ? O2 H2 0.89(2) . ? N11 C11 1.516(10) . ? N11 H11A 0.9000 . ? N11 H11B 0.9000 . ? N12 C12 1.501(10) . ? N12 H12A 0.9000 . ? N12 H12B 0.9000 . ? C11 C12 1.467(11) . ? C11 H11C 0.9700 . ? C11 H11D 0.9700 . ? C12 H12C 0.9700 . ? C12 H12D 0.9700 . ? N21 C21 1.476(10) . ? N21 H21A 0.9000 . ? N21 H21B 0.9000 . ? N22 C22 1.470(11) . ? N22 H22A 0.9000 . ? N22 H22B 0.9000 . ? C21 C22 1.510(11) . ? C21 H21C 0.9700 . ? C21 H21D 0.9700 . ? C22 H22C 0.9700 . ? C22 H22D 0.9700 . ? N10 O13 1.242(9) . ? N10 O11 1.254(8) . ? N10 O12 1.263(8) . ? N20 O21 1.228(10) . ? N20 O22 1.247(9) . ? N20 O23 1.268(9) . ? N30 O32 1.229(5) . ? N30 O33 1.231(6) . ? N30 O33A 1.231(5) . ? N30 O31 1.234(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 N11 Pt1 O2 175.9(2) . . ? N11 Pt1 N12 83.9(2) . . ? O2 Pt1 N12 100.0(2) . . ? N11 Pt1 O1 99.2(2) . . ? O2 Pt1 O1 76.9(2) . . ? N12 Pt1 O1 176.2(2) . . ? N11 Pt1 Ag1 98.1(2) . . ? O2 Pt1 Ag1 82.55(17) . . ? N12 Pt1 Ag1 100.07(19) . . ? O1 Pt1 Ag1 81.86(15) . . ? N11 Pt1 Pt2 134.13(19) . . ? O2 Pt1 Pt2 43.13(17) . . ? N12 Pt1 Pt2 134.72(18) . . ? O1 Pt1 Pt2 43.82(14) . . ? Ag1 Pt1 Pt2 57.96(3) . . ? N21 Pt2 O2 101.0(2) . . ? N21 Pt2 N22 82.6(3) . . ? O2 Pt2 N22 176.4(2) . . ? N21 Pt2 O1 176.9(3) . . ? O2 Pt2 O1 76.1(2) . . ? N22 Pt2 O1 100.3(2) . . ? N21 Pt2 Ag1 99.15(17) . . ? O2 Pt2 Ag1 82.53(14) . . ? N22 Pt2 Ag1 97.45(18) . . ? O1 Pt2 Ag1 81.74(13) . . ? N21 Pt2 Pt1 134.87(18) . . ? O2 Pt2 Pt1 42.74(15) . . ? N22 Pt2 Pt1 134.47(18) . . ? O1 Pt2 Pt1 43.26(14) . . ? Ag1 Pt2 Pt1 58.25(2) . . ? N21 Pt2 Pt2 92.81(17) . 3_566 ? O2 Pt2 Pt2 83.52(15) . 3_566 ? N22 Pt2 Pt2 95.89(18) . 3_566 ? O1 Pt2 Pt2 85.71(13) . 3_566 ? Ag1 Pt2 Pt2 163.11(3) . 3_566 ? Pt1 Pt2 Pt2 104.88(2) . 3_566 ? N21 Pt2 H1 157.9(7) . . ? O2 Pt2 H1 100.8(10) . . ? N22 Pt2 H1 75.7(10) . . ? O1 Pt2 H1 25.2(7) . . ? Ag1 Pt2 H1 80(3) . . ? Pt1 Pt2 H1 63.1(17) . . ? Pt2 Pt2 H1 94(3) 3_566 . ? O11 Ag1 O31 90.4(3) . . ? O11 Ag1 Pt2 160.24(15) . . ? O31 Ag1 Pt2 88.87(18) . . ? O11 Ag1 Pt1 123.88(17) . . ? O31 Ag1 Pt1 142.96(19) . . ? Pt2 Ag1 Pt1 63.79(3) . . ? Pt1 O1 Pt2 92.91(19) . . ? Pt1 O1 H1 134(7) . . ? Pt2 O1 H1 75(5) . . ? Pt1 O2 Pt2 94.1(2) . . ? Pt1 O2 H2 90(9) . . ? Pt2 O2 H2 116(10) . . ? C11 N11 Pt1 108.6(5) . . ? C11 N11 H11A 110.0 . . ? Pt1 N11 H11A 110.0 . . ? C11 N11 H11B 110.0 . . ? Pt1 N11 H11B 110.0 . . ? H11A N11 H11B 108.4 . . ? C12 N12 Pt1 110.1(5) . . ? C12 N12 H12A 109.6 . . ? Pt1 N12 H12A 109.6 . . ? C12 N12 H12B 109.6 . . ? Pt1 N12 H12B 109.6 . . ? H12A N12 H12B 108.2 . . ? C12 C11 N11 108.3(7) . . ? C12 C11 H11C 110.0 . . ? N11 C11 H11C 110.0 . . ? C12 C11 H11D 110.0 . . ? N11 C11 H11D 110.0 . . ? H11C C11 H11D 108.4 . . ? C11 C12 N12 108.0(7) . . ? C11 C12 H12C 110.1 . . ? N12 C12 H12C 110.1 . . ? C11 C12 H12D 110.1 . . ? N12 C12 H12D 110.1 . . ? H12C C12 H12D 108.4 . . ? C21 N21 Pt2 109.5(5) . . ? C21 N21 H21A 109.8 . . ? Pt2 N21 H21A 109.8 . . ? C21 N21 H21B 109.8 . . ? Pt2 N21 H21B 109.8 . . ? H21A N21 H21B 108.2 . . ? C22 N22 Pt2 110.5(5) . . ? C22 N22 H22A 109.6 . . ? Pt2 N22 H22A 109.6 . . ? C22 N22 H22B 109.6 . . ? Pt2 N22 H22B 109.6 . . ? H22A N22 H22B 108.1 . . ? N21 C21 C22 106.1(6) . . ? N21 C21 H21C 110.5 . . ? C22 C21 H21C 110.5 . . ? N21 C21 H21D 110.5 . . ? C22 C21 H21D 110.5 . . ? H21C C21 H21D 108.7 . . ? N22 C22 C21 108.5(7) . . ? N22 C22 H22C 110.0 . . ? C21 C22 H22C 110.0 . . ? N22 C22 H22D 110.0 . . ? C21 C22 H22D 110.0 . . ? H22C C22 H22D 108.4 . . ? O13 N10 O11 120.6(6) . . ? O13 N10 O12 120.5(7) . . ? O11 N10 O12 118.9(7) . . ? N10 O11 Ag1 106.5(5) . . ? O21 N20 O22 120.7(8) . . ? O21 N20 O23 119.9(8) . . ? O22 N20 O23 119.4(8) . . ? O32 N30 O33 98.0(19) . . ? O32 N30 O33A 123.8(8) . . ? O33 N30 O33A 54.5(15) . . ? O32 N30 O31 115.1(8) . . ? O33 N30 O31 133.9(18) . . ? O33A N30 O31 118.3(8) . . ? N30 O31 Ag1 120.6(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 N11 Pt1 Pt2 N21 137.3(4) . . . . ? O2 Pt1 Pt2 N21 -47.0(3) . . . . ? N12 Pt1 Pt2 N21 -1.4(3) . . . . ? O1 Pt1 Pt2 N21 -176.4(3) . . . . ? Ag1 Pt1 Pt2 N21 69.4(3) . . . . ? N11 Pt1 Pt2 O2 -175.7(3) . . . . ? N12 Pt1 Pt2 O2 45.6(3) . . . . ? O1 Pt1 Pt2 O2 -129.3(3) . . . . ? Ag1 Pt1 Pt2 O2 116.4(2) . . . . ? N11 Pt1 Pt2 N22 1.2(4) . . . . ? O2 Pt1 Pt2 N22 176.8(3) . . . . ? N12 Pt1 Pt2 N22 -137.6(4) . . . . ? O1 Pt1 Pt2 N22 47.5(3) . . . . ? Ag1 Pt1 Pt2 N22 -66.8(3) . . . . ? N11 Pt1 Pt2 O1 -46.3(3) . . . . ? O2 Pt1 Pt2 O1 129.3(3) . . . . ? N12 Pt1 Pt2 O1 175.0(3) . . . . ? Ag1 Pt1 Pt2 O1 -114.3(2) . . . . ? N11 Pt1 Pt2 Ag1 68.0(3) . . . . ? O2 Pt1 Pt2 Ag1 -116.4(2) . . . . ? N12 Pt1 Pt2 Ag1 -70.8(2) . . . . ? O1 Pt1 Pt2 Ag1 114.3(2) . . . . ? N11 Pt1 Pt2 Pt2 -113.0(2) . . . 3_566 ? O2 Pt1 Pt2 Pt2 62.6(2) . . . 3_566 ? N12 Pt1 Pt2 Pt2 108.2(2) . . . 3_566 ? O1 Pt1 Pt2 Pt2 -66.7(2) . . . 3_566 ? Ag1 Pt1 Pt2 Pt2 179.02(3) . . . 3_566 ? N21 Pt2 Ag1 O11 -19.9(6) . . . . ? O2 Pt2 Ag1 O11 80.1(5) . . . . ? N22 Pt2 Ag1 O11 -103.5(6) . . . . ? O1 Pt2 Ag1 O11 157.0(5) . . . . ? Pt1 Pt2 Ag1 O11 117.9(5) . . . . ? Pt2 Pt2 Ag1 O11 114.6(5) 3_566 . . . ? N21 Pt2 Ag1 O31 68.1(3) . . . . ? O2 Pt2 Ag1 O31 168.1(2) . . . . ? N22 Pt2 Ag1 O31 -15.5(3) . . . . ? O1 Pt2 Ag1 O31 -115.0(2) . . . . ? Pt1 Pt2 Ag1 O31 -154.11(18) . . . . ? Pt2 Pt2 Ag1 O31 -157.37(19) 3_566 . . . ? N21 Pt2 Ag1 Pt1 -137.79(19) . . . . ? O2 Pt2 Ag1 Pt1 -37.82(16) . . . . ? N22 Pt2 Ag1 Pt1 138.59(19) . . . . ? O1 Pt2 Ag1 Pt1 39.15(16) . . . . ? Pt2 Pt2 Ag1 Pt1 -3.27(9) 3_566 . . . ? N11 Pt1 Ag1 O11 63.3(3) . . . . ? O2 Pt1 Ag1 O11 -120.8(2) . . . . ? N12 Pt1 Ag1 O11 -21.9(3) . . . . ? O1 Pt1 Ag1 O11 161.5(2) . . . . ? Pt2 Pt1 Ag1 O11 -158.91(19) . . . . ? N11 Pt1 Ag1 O31 -91.3(3) . . . . ? O2 Pt1 Ag1 O31 84.6(3) . . . . ? N12 Pt1 Ag1 O31 -176.5(3) . . . . ? O1 Pt1 Ag1 O31 6.8(3) . . . . ? Pt2 Pt1 Ag1 O31 46.5(3) . . . . ? N11 Pt1 Ag1 Pt2 -137.78(17) . . . . ? O2 Pt1 Ag1 Pt2 38.14(15) . . . . ? N12 Pt1 Ag1 Pt2 137.04(17) . . . . ? O1 Pt1 Ag1 Pt2 -39.62(14) . . . . ? N11 Pt1 O1 Pt2 148.3(2) . . . . ? O2 Pt1 O1 Pt2 -32.9(2) . . . . ? N12 Pt1 O1 Pt2 -69(4) . . . . ? Ag1 Pt1 O1 Pt2 51.32(14) . . . . ? N21 Pt2 O1 Pt1 55(4) . . . . ? O2 Pt2 O1 Pt1 32.7(2) . . . . ? N22 Pt2 O1 Pt1 -147.7(2) . . . . ? Ag1 Pt2 O1 Pt1 -51.57(14) . . . . ? Pt2 Pt2 O1 Pt1 117.10(16) 3_566 . . . ? N11 Pt1 O2 Pt2 50(4) . . . . ? N12 Pt1 O2 Pt2 -149.0(2) . . . . ? O1 Pt1 O2 Pt2 33.4(2) . . . . ? Ag1 Pt1 O2 Pt2 -49.98(15) . . . . ? N21 Pt2 O2 Pt1 148.1(2) . . . . ? N22 Pt2 O2 Pt1 -40(4) . . . . ? O1 Pt2 O2 Pt1 -33.09(19) . . . . ? Ag1 Pt2 O2 Pt1 50.20(15) . . . . ? Pt2 Pt2 O2 Pt1 -120.25(18) 3_566 . . . ? O2 Pt1 N11 C11 145(3) . . . . ? N12 Pt1 N11 C11 -16.4(5) . . . . ? O1 Pt1 N11 C11 161.3(5) . . . . ? Ag1 Pt1 N11 C11 -115.7(5) . . . . ? Pt2 Pt1 N11 C11 -168.2(4) . . . . ? N11 Pt1 N12 C12 -10.5(6) . . . . ? O2 Pt1 N12 C12 170.8(5) . . . . ? O1 Pt1 N12 C12 -153(3) . . . . ? Ag1 Pt1 N12 C12 86.6(5) . . . . ? Pt2 Pt1 N12 C12 141.0(5) . . . . ? Pt1 N11 C11 C12 41.2(8) . . . . ? N11 C11 C12 N12 -50.4(10) . . . . ? Pt1 N12 C12 C11 36.3(9) . . . . ? O2 Pt2 N21 C21 -158.3(4) . . . . ? N22 Pt2 N21 C21 22.2(5) . . . . ? O1 Pt2 N21 C21 180(100) . . . . ? Ag1 Pt2 N21 C21 -74.2(4) . . . . ? Pt1 Pt2 N21 C21 -127.9(4) . . . . ? Pt2 Pt2 N21 C21 117.8(4) 3_566 . . . ? N21 Pt2 N22 C22 6.5(5) . . . . ? O2 Pt2 N22 C22 -166(3) . . . . ? O1 Pt2 N22 C22 -172.3(5) . . . . ? Ag1 Pt2 N22 C22 104.8(5) . . . . ? Pt1 Pt2 N22 C22 156.8(4) . . . . ? Pt2 Pt2 N22 C22 -85.6(5) 3_566 . . . ? Pt2 N21 C21 C22 -45.5(7) . . . . ? Pt2 N22 C22 C21 -33.2(8) . . . . ? N21 C21 C22 N22 51.2(8) . . . . ? O13 N10 O11 Ag1 5.5(10) . . . . ? O12 N10 O11 Ag1 -174.7(7) . . . . ? O31 Ag1 O11 N10 104.3(6) . . . . ? Pt2 Ag1 O11 N10 -168.0(4) . . . . ? Pt1 Ag1 O11 N10 -60.8(6) . . . . ? O32 N30 O31 Ag1 -95.4(10) . . . . ? O33 N30 O31 Ag1 133(3) . . . . ? O33A N30 O31 Ag1 66.4(13) . . . . ? O11 Ag1 O31 N30 -84.9(6) . . . . ? Pt2 Ag1 O31 N30 114.8(6) . . . . ? Pt1 Ag1 O31 N30 74.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.563 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.200 data_14 _database_code_depnum_ccdc_archive 'CCDC 678550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H17 N2 O Pt, N O3, H2 O' _chemical_formula_sum 'C6 H19 N3 O5 Pt' _chemical_formula_weight 408.33 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' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.8880(10) _cell_length_b 11.395(2) _cell_length_c 17.896(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.33(3) _cell_angle_gamma 90.00 _cell_volume 1195.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2128 _cell_measurement_theta_min 4.58 _cell_measurement_theta_max 25.67 _exptl_crystal_description needle _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 11.745 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf-Nonius-KappaCCD _diffrn_measurement_method 'profile fitted' _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2128 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.58 _diffrn_reflns_theta_max 25.67 _reflns_number_total 2128 _reflns_number_gt 1674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _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^)+(0.0390P)^2^+0.2896P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, H1w difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0041(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2128 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 0.16124(5) 0.07421(3) 0.056850(16) 0.03253(15) Uani 1 1 d . . . N1 N 0.4043(11) 0.0409(6) 0.1439(4) 0.0361(16) Uani 1 1 d . . . C1 C 0.5375(14) 0.1532(8) 0.1567(5) 0.047(2) Uani 1 1 d . . . H1A H 0.6213 0.1521 0.2060 0.037(11) Uiso 1 1 calc R . . H1B H 0.6461 0.1610 0.1194 0.037(11) Uiso 1 1 calc R . . C11 C 0.5628(16) -0.0555(8) 0.1275(6) 0.056(3) Uani 1 1 d . . . H11A H 0.6531 -0.0314 0.0882 0.062(8) Uiso 1 1 calc R . . H11B H 0.4764 -0.1241 0.1118 0.062(8) Uiso 1 1 calc R . . H11C H 0.6611 -0.0732 0.1719 0.062(8) Uiso 1 1 calc R . . C12 C 0.2940(15) 0.0075(9) 0.2118(5) 0.053(2) Uani 1 1 d . . . H12A H 0.2126 -0.0649 0.2028 0.062(8) Uiso 1 1 calc R . . H12B H 0.1894 0.0680 0.2235 0.062(8) Uiso 1 1 calc R . . H12C H 0.4084 -0.0022 0.2532 0.062(8) Uiso 1 1 calc R . . N2 N 0.2357(11) 0.2480(6) 0.0772(4) 0.0379(15) Uani 1 1 d . . . C2 C 0.3765(16) 0.2532(8) 0.1510(5) 0.053(2) Uani 1 1 d . . . H2A H 0.4604 0.3265 0.1551 0.037(11) Uiso 1 1 calc R . . H2B H 0.2782 0.2496 0.1915 0.037(11) Uiso 1 1 calc R . . C21 C 0.3690(14) 0.2939(8) 0.0170(5) 0.048(2) Uani 1 1 d . . . H21A H 0.5001 0.2450 0.0130 0.062(8) Uiso 1 1 calc R . . H21B H 0.4177 0.3726 0.0291 0.062(8) Uiso 1 1 calc R . . H21C H 0.2754 0.2937 -0.0298 0.062(8) Uiso 1 1 calc R . . C22 C 0.0302(14) 0.3225(7) 0.0809(6) 0.059(3) Uani 1 1 d . . . H22A H -0.0634 0.3178 0.0342 0.062(8) Uiso 1 1 calc R . . H22B H 0.0761 0.4024 0.0902 0.062(8) Uiso 1 1 calc R . . H22C H -0.0548 0.2954 0.1208 0.062(8) Uiso 1 1 calc R . . N20 N 0.5558(13) -0.4150(7) 0.1516(4) 0.0508(19) Uani 1 1 d . . . O21 O 0.7049(13) -0.4885(8) 0.1501(6) 0.096(3) Uani 1 1 d . . . O23 O 0.5980(12) -0.3211(7) 0.1843(4) 0.072(2) Uani 1 1 d . . . O22 O 0.3620(12) -0.4325(6) 0.1195(4) 0.070(2) Uani 1 1 d . . . O1W O 0.0952(10) -0.0959(5) 0.0270(4) 0.0380(14) Uani 1 1 d . . . H1W H 0.053(15) -0.134(9) 0.057(5) 0.04(3) Uiso 1 1 d . . . O2W O 0.4543(10) 0.2497(5) 0.3563(4) 0.0599(17) 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 0.0367(2) 0.0303(2) 0.0306(2) -0.00263(17) 0.00286(11) -0.00517(15) N1 0.044(4) 0.035(4) 0.029(4) -0.005(3) 0.003(3) -0.005(3) C1 0.049(5) 0.049(6) 0.041(5) 0.001(4) -0.010(4) -0.020(4) C11 0.055(6) 0.055(7) 0.057(6) -0.008(5) -0.004(4) 0.010(4) C12 0.068(6) 0.055(6) 0.035(5) 0.005(5) 0.008(4) -0.008(5) N2 0.039(3) 0.033(4) 0.040(4) -0.004(3) 0.002(3) -0.007(3) C2 0.072(6) 0.047(6) 0.039(5) -0.020(4) 0.003(4) -0.012(5) C21 0.052(5) 0.042(5) 0.049(5) 0.002(4) 0.001(4) -0.012(4) C22 0.047(5) 0.033(5) 0.097(8) -0.010(5) 0.004(5) -0.002(4) N20 0.052(5) 0.047(5) 0.054(5) 0.007(4) 0.006(3) -0.007(4) O21 0.071(5) 0.075(6) 0.142(8) -0.013(6) 0.010(5) 0.019(4) O23 0.077(5) 0.053(5) 0.081(5) -0.007(4) -0.014(4) -0.004(3) O22 0.059(4) 0.071(5) 0.079(5) -0.013(4) 0.001(4) -0.014(4) O1W 0.041(3) 0.032(4) 0.039(3) -0.003(3) -0.005(3) -0.007(2) O2W 0.070(4) 0.049(4) 0.059(4) -0.012(3) -0.001(3) 0.005(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 O1W 2.039(6) . ? Pt1 O1W 2.042(6) 3 ? Pt1 N1 2.050(7) . ? Pt1 N2 2.053(7) . ? Pt1 Pt1 3.1445(9) 3 ? N1 C12 1.481(10) . ? N1 C11 1.488(11) . ? N1 C1 1.507(10) . ? C1 C2 1.480(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N2 C21 1.485(10) . ? N2 C22 1.485(10) . ? N2 C2 1.493(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N20 O21 1.216(10) . ? N20 O23 1.234(9) . ? N20 O22 1.245(10) . ? O1W Pt1 2.042(6) 3 ? O1W H1W 0.75(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 O1W Pt1 O1W 79.2(3) . 3 ? O1W Pt1 N1 97.2(2) . . ? O1W Pt1 N1 175.3(2) 3 . ? O1W Pt1 N2 174.8(3) . . ? O1W Pt1 N2 98.3(3) 3 . ? N1 Pt1 N2 85.5(3) . . ? O1W Pt1 Pt1 39.63(16) . 3 ? O1W Pt1 Pt1 39.57(16) 3 3 ? N1 Pt1 Pt1 136.79(18) . 3 ? N2 Pt1 Pt1 137.69(19) . 3 ? C12 N1 C11 107.7(7) . . ? C12 N1 C1 110.8(6) . . ? C11 N1 C1 109.2(7) . . ? C12 N1 Pt1 110.1(5) . . ? C11 N1 Pt1 113.2(5) . . ? C1 N1 Pt1 106.0(5) . . ? C2 C1 N1 108.8(7) . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? N1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 N2 C22 108.6(7) . . ? C21 N2 C2 109.9(6) . . ? C22 N2 C2 109.0(7) . . ? C21 N2 Pt1 109.3(5) . . ? C22 N2 Pt1 113.4(5) . . ? C2 N2 Pt1 106.7(5) . . ? C1 C2 N2 109.2(7) . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? N2 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O21 N20 O23 119.6(8) . . ? O21 N20 O22 120.8(9) . . ? O23 N20 O22 119.6(8) . . ? Pt1 O1W Pt1 100.8(3) . 3 ? Pt1 O1W H1W 115(7) . . ? Pt1 O1W H1W 109(7) 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 O1W Pt1 N1 C12 -80.2(6) . . . . ? O1W Pt1 N1 C12 -40(3) 3 . . . ? N2 Pt1 N1 C12 104.3(6) . . . . ? Pt1 Pt1 N1 C12 -77.3(6) 3 . . . ? O1W Pt1 N1 C11 40.3(6) . . . . ? O1W Pt1 N1 C11 80(3) 3 . . . ? N2 Pt1 N1 C11 -135.2(6) . . . . ? Pt1 Pt1 N1 C11 43.2(7) 3 . . . ? O1W Pt1 N1 C1 160.0(5) . . . . ? O1W Pt1 N1 C1 -160(3) 3 . . . ? N2 Pt1 N1 C1 -15.5(5) . . . . ? Pt1 Pt1 N1 C1 162.8(4) 3 . . . ? C12 N1 C1 C2 -77.8(9) . . . . ? C11 N1 C1 C2 163.8(7) . . . . ? Pt1 N1 C1 C2 41.6(8) . . . . ? O1W Pt1 N2 C21 -15(3) . . . . ? O1W Pt1 N2 C21 -76.5(5) 3 . . . ? N1 Pt1 N2 C21 106.2(5) . . . . ? Pt1 Pt1 N2 C21 -72.1(6) 3 . . . ? O1W Pt1 N2 C22 106(2) . . . . ? O1W Pt1 N2 C22 44.8(6) 3 . . . ? N1 Pt1 N2 C22 -132.4(6) . . . . ? Pt1 Pt1 N2 C22 49.2(7) 3 . . . ? O1W Pt1 N2 C2 -134(2) . . . . ? O1W Pt1 N2 C2 164.8(5) 3 . . . ? N1 Pt1 N2 C2 -12.5(5) . . . . ? Pt1 Pt1 N2 C2 169.2(4) 3 . . . ? N1 C1 C2 N2 -55.0(9) . . . . ? C21 N2 C2 C1 -79.0(8) . . . . ? C22 N2 C2 C1 162.1(7) . . . . ? Pt1 N2 C2 C1 39.3(8) . . . . ? O1W Pt1 O1W Pt1 0.0 3 . . 3 ? N1 Pt1 O1W Pt1 177.0(3) . . . 3 ? N2 Pt1 O1W Pt1 -62(3) . . . 3 ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.67 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 1.598 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.147 data_2947 _database_code_depnum_ccdc_archive 'CCDC 678551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H34 N4 O2 Pt2, 2(Cl O4)' _chemical_formula_sum 'C12 H34 Cl2 N4 O10 Pt2' _chemical_formula_weight 855.51 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' 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' H H 0.0000 0.0000 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.8130(12) _cell_length_b 9.810(2) _cell_length_c 20.361(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.52(3) _cell_angle_gamma 90.00 _cell_volume 1160.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 200 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 12.331 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3719 _exptl_absorpt_correction_T_max 0.3719 _exptl_absorpt_process_details ? _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 Enraf-Nonius-KappaCCD _diffrn_measurement_method 'profile fitted' _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2111 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.37 _reflns_number_total 2111 _reflns_number_gt 1654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _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^)+(0.1144P)^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, H17 difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2111 _refine_ls_number_parameters 135 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.35424(8) 0.07651(5) 0.05244(2) 0.0185(3) Uani 1 1 d . . . Cl4 Cl 0.6362(7) -0.3874(4) 0.15057(19) 0.0313(9) Uani 1 1 d . . . O1 O 0.5931(18) -0.0775(9) 0.0457(5) 0.024(2) Uani 1 1 d D . . H17 H 0.57(3) -0.077(14) 0.088(5) 0.036 Uiso 1 1 d D . . N4 N 0.1340(17) 0.2370(11) 0.0531(5) 0.023(3) Uani 1 1 d . . . C3 C 0.000(2) 0.2253(16) 0.1149(7) 0.029(3) Uani 1 1 d . . . H16 H -0.1221 0.1585 0.1085 0.035 Uiso 1 1 calc R . . H15 H -0.0701 0.3124 0.1247 0.035 Uiso 1 1 calc R . . O41 O 0.4807(18) -0.3344(10) 0.0985(5) 0.035(3) Uani 1 1 d . . . O42 O 0.523(2) -0.4869(12) 0.1868(6) 0.054(3) Uani 1 1 d . . . O43 O 0.707(2) -0.2787(12) 0.1935(6) 0.052(3) Uani 1 1 d . . . C41 C -0.038(2) 0.2402(14) -0.0033(7) 0.028(3) Uani 1 1 d . . . H14 H -0.1346 0.3190 0.0003 0.042 Uiso 1 1 calc R . . H13 H -0.1311 0.1593 -0.0028 0.042 Uiso 1 1 calc R . . H12 H 0.0405 0.2442 -0.0437 0.042 Uiso 1 1 calc R . . O44 O 0.825(3) -0.4467(16) 0.1206(8) 0.081(6) Uani 1 1 d . . . N1 N 0.2897(19) 0.0580(11) 0.1492(6) 0.021(3) Uiso 1 1 d . . . C42 C 0.264(2) 0.3680(14) 0.0546(7) 0.026(3) Uani 1 1 d . . . H11 H 0.1570 0.4428 0.0548 0.038 Uiso 1 1 calc R . . H10 H 0.3541 0.3742 0.0164 0.038 Uiso 1 1 calc R . . H9 H 0.3631 0.3716 0.0934 0.038 Uiso 1 1 calc R . . C11 C 0.500(3) 0.0402(17) 0.1917(8) 0.034(4) Uani 1 1 d . . . H8 H 0.4587 0.0317 0.2367 0.050 Uiso 1 1 calc R . . H7 H 0.5986 0.1180 0.1874 0.050 Uiso 1 1 calc R . . H6 H 0.5797 -0.0405 0.1788 0.050 Uiso 1 1 calc R . . C2 C 0.162(3) 0.1820(15) 0.1723(8) 0.031(3) Uani 1 1 d . . . H5 H 0.2697 0.2547 0.1838 0.037 Uiso 1 1 calc R . . H4 H 0.0758 0.1600 0.2105 0.037 Uiso 1 1 calc R . . C12 C 0.132(3) -0.0667(13) 0.1595(8) 0.025(3) Uani 1 1 d . . . H3 H 0.1021 -0.0751 0.2053 0.037 Uiso 1 1 calc R . . H2 H 0.2072 -0.1477 0.1449 0.037 Uiso 1 1 calc R . . H1 H -0.0105 -0.0545 0.1346 0.037 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 0.0254(4) 0.0214(4) 0.0094(4) -0.0010(2) 0.0067(2) -0.0001(2) Cl4 0.045(2) 0.0261(19) 0.023(2) 0.0029(15) 0.0080(16) 0.0016(15) O1 0.039(6) 0.030(6) 0.004(5) -0.001(4) 0.011(4) 0.004(4) N4 0.031(6) 0.029(7) 0.010(6) 0.005(5) 0.006(5) 0.001(5) C3 0.031(7) 0.040(9) 0.017(8) 0.003(7) 0.014(6) -0.004(6) O41 0.055(6) 0.033(6) 0.018(6) 0.010(4) 0.002(5) -0.004(5) O42 0.093(9) 0.046(8) 0.024(7) 0.013(6) 0.003(6) -0.030(7) O43 0.084(8) 0.032(6) 0.038(8) -0.002(5) -0.013(6) -0.007(6) C41 0.025(7) 0.028(9) 0.031(9) 0.000(6) 0.001(6) -0.005(6) O44 0.090(11) 0.096(12) 0.061(12) 0.033(8) 0.048(9) 0.061(9) C42 0.032(7) 0.025(8) 0.022(9) -0.009(6) 0.011(6) -0.006(6) C11 0.039(9) 0.049(10) 0.013(9) -0.005(7) 0.002(7) 0.002(7) C2 0.043(8) 0.031(9) 0.020(9) -0.004(6) 0.007(7) 0.003(7) C12 0.040(8) 0.018(8) 0.017(9) 0.006(5) 0.016(7) 0.002(6) _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 N4 2.030(11) . ? Pt1 N1 2.030(13) . ? Pt1 O1 2.036(10) 3_655 ? Pt1 O1 2.060(9) . ? Pt1 Pt1 3.1630(12) 3_655 ? Pt1 H17 2.08(14) . ? Cl4 O42 1.405(12) . ? Cl4 O44 1.407(13) . ? Cl4 O43 1.428(12) . ? Cl4 O41 1.458(11) . ? O1 Pt1 2.036(10) 3_655 ? O1 H17 0.87(9) . ? N4 C42 1.489(17) . ? N4 C41 1.490(18) . ? N4 C3 1.514(16) . ? C3 C2 1.53(2) . ? C3 H16 0.9700 . ? C3 H15 0.9700 . ? C41 H14 0.9600 . ? C41 H13 0.9600 . ? C41 H12 0.9600 . ? N1 C11 1.477(18) . ? N1 C2 1.509(18) . ? N1 C12 1.547(17) . ? C42 H11 0.9600 . ? C42 H10 0.9600 . ? C42 H9 0.9600 . ? C11 H8 0.9600 . ? C11 H7 0.9600 . ? C11 H6 0.9600 . ? C2 H5 0.9700 . ? C2 H4 0.9700 . ? C12 H3 0.9600 . ? C12 H2 0.9600 . ? C12 H1 0.9600 . ? 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 N4 Pt1 N1 85.3(4) . . ? N4 Pt1 O1 97.2(4) . 3_655 ? N1 Pt1 O1 174.7(4) . 3_655 ? N4 Pt1 O1 175.1(4) . . ? N1 Pt1 O1 98.8(4) . . ? O1 Pt1 O1 78.9(4) 3_655 . ? N4 Pt1 Pt1 136.9(3) . 3_655 ? N1 Pt1 Pt1 137.8(3) . 3_655 ? O1 Pt1 Pt1 39.7(3) 3_655 3_655 ? O1 Pt1 Pt1 39.2(3) . 3_655 ? N4 Pt1 H17 159(3) . . ? N1 Pt1 H17 75(3) . . ? O1 Pt1 H17 103(3) 3_655 . ? O1 Pt1 H17 24(3) . . ? Pt1 Pt1 H17 64(3) 3_655 . ? O42 Cl4 O44 109.6(9) . . ? O42 Cl4 O43 109.1(8) . . ? O44 Cl4 O43 111.5(10) . . ? O42 Cl4 O41 109.8(7) . . ? O44 Cl4 O41 107.7(9) . . ? O43 Cl4 O41 109.3(7) . . ? Pt1 O1 Pt1 101.1(4) 3_655 . ? Pt1 O1 H17 179(10) 3_655 . ? Pt1 O1 H17 79(10) . . ? C42 N4 C41 108.6(10) . . ? C42 N4 C3 109.2(11) . . ? C41 N4 C3 106.8(10) . . ? C42 N4 Pt1 110.6(8) . . ? C41 N4 Pt1 114.4(8) . . ? C3 N4 Pt1 107.2(8) . . ? N4 C3 C2 109.3(11) . . ? N4 C3 H16 109.8 . . ? C2 C3 H16 109.8 . . ? N4 C3 H15 109.8 . . ? C2 C3 H15 109.8 . . ? H16 C3 H15 108.3 . . ? N4 C41 H14 109.5 . . ? N4 C41 H13 109.5 . . ? H14 C41 H13 109.5 . . ? N4 C41 H12 109.5 . . ? H14 C41 H12 109.5 . . ? H13 C41 H12 109.5 . . ? C11 N1 C2 108.5(11) . . ? C11 N1 C12 107.9(11) . . ? C2 N1 C12 107.1(11) . . ? C11 N1 Pt1 113.3(9) . . ? C2 N1 Pt1 110.1(9) . . ? C12 N1 Pt1 109.7(9) . . ? N4 C42 H11 109.5 . . ? N4 C42 H10 109.5 . . ? H11 C42 H10 109.5 . . ? N4 C42 H9 109.5 . . ? H11 C42 H9 109.5 . . ? H10 C42 H9 109.5 . . ? N1 C11 H8 109.5 . . ? N1 C11 H7 109.5 . . ? H8 C11 H7 109.5 . . ? N1 C11 H6 109.5 . . ? H8 C11 H6 109.5 . . ? H7 C11 H6 109.5 . . ? N1 C2 C3 106.4(12) . . ? N1 C2 H5 110.5 . . ? C3 C2 H5 110.5 . . ? N1 C2 H4 110.5 . . ? C3 C2 H4 110.5 . . ? H5 C2 H4 108.6 . . ? N1 C12 H3 109.5 . . ? N1 C12 H2 109.5 . . ? H3 C12 H2 109.5 . . ? N1 C12 H1 109.5 . . ? H3 C12 H1 109.5 . . ? H2 C12 H1 109.5 . . ? 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 N4 Pt1 O1 Pt1 -38(5) . . . 3_655 ? N1 Pt1 O1 Pt1 175.2(4) . . . 3_655 ? O1 Pt1 O1 Pt1 0.0 3_655 . . 3_655 ? N1 Pt1 N4 C42 102.5(9) . . . . ? O1 Pt1 N4 C42 -82.1(9) 3_655 . . . ? O1 Pt1 N4 C42 -44(5) . . . . ? Pt1 Pt1 N4 C42 -79.3(9) 3_655 . . . ? N1 Pt1 N4 C41 -134.6(9) . . . . ? O1 Pt1 N4 C41 40.8(9) 3_655 . . . ? O1 Pt1 N4 C41 78(5) . . . . ? Pt1 Pt1 N4 C41 43.7(10) 3_655 . . . ? N1 Pt1 N4 C3 -16.4(9) . . . . ? O1 Pt1 N4 C3 159.0(8) 3_655 . . . ? O1 Pt1 N4 C3 -163(5) . . . . ? Pt1 Pt1 N4 C3 161.8(7) 3_655 . . . ? C42 N4 C3 C2 -78.5(14) . . . . ? C41 N4 C3 C2 164.3(11) . . . . ? Pt1 N4 C3 C2 41.3(13) . . . . ? N4 Pt1 N1 C11 -133.1(10) . . . . ? O1 Pt1 N1 C11 108(4) 3_655 . . . ? O1 Pt1 N1 C11 44.2(10) . . . . ? Pt1 Pt1 N1 C11 48.7(11) 3_655 . . . ? N4 Pt1 N1 C2 -11.4(9) . . . . ? O1 Pt1 N1 C2 -131(4) 3_655 . . . ? O1 Pt1 N1 C2 165.9(8) . . . . ? Pt1 Pt1 N1 C2 170.4(7) 3_655 . . . ? N4 Pt1 N1 C12 106.2(9) . . . . ? O1 Pt1 N1 C12 -13(4) 3_655 . . . ? O1 Pt1 N1 C12 -76.5(9) . . . . ? Pt1 Pt1 N1 C12 -72.0(9) 3_655 . . . ? C11 N1 C2 C3 160.6(12) . . . . ? C12 N1 C2 C3 -83.1(14) . . . . ? Pt1 N1 C2 C3 36.1(13) . . . . ? N4 C3 C2 N1 -51.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.214 _refine_diff_density_min -4.105 _refine_diff_density_rms 0.480