# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1301 data_Ag2[Pt(ox)2] #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 622.90 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H4 Ag2 O10 Pt ' _chemical_formula_moiety 'C4 H4 Ag2 O10 Pt ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.745(2) _cell_length_b 7.913(1) _cell_length_c 6.954(1) _cell_angle_alpha 90 _cell_angle_beta 117.050(10) _cell_angle_gamma 90 _cell_volume 477.6(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 14.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m ' _symmetry_Int_Tables_number 12 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,z -x,-y,-z -x,y,-z 1/2+x,1/2+y,z 1/2+x,1/2-y,z 1/2-x,1/2-y,-z 1/2-x,1/2+y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 4.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560.00 _exptl_absorpt_coefficient_mu 18.645 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -13.68 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 1 -2 3 -1 -2 1 -1 -1 _diffrn_reflns_number 625 _reflns_number_total 591 _reflns_number_observed 585 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06327 _diffrn_orient_matrix_UB_12 -0.05107 _diffrn_orient_matrix_UB_13 -0.14551 _diffrn_orient_matrix_UB_21 -0.05828 _diffrn_orient_matrix_UB_22 0.10836 _diffrn_orient_matrix_UB_23 -0.05066 _diffrn_orient_matrix_UB_31 0.07665 _diffrn_orient_matrix_UB_32 0.04023 _diffrn_orient_matrix_UB_33 -0.04826 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Pt' ' Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.0000 0.0000 0.0000 0.0122(1) Uani 1.00 d S . . Ag Ag -0.28217(9) 0.0000 0.5856(1) 0.0266(2) Uani 1.00 d S . . O(1) O -0.0861(6) 0.1667(6) 0.1334(7) 0.023(1) Uani 1.00 d . . . O(2) O -0.1942(6) 0.1753(6) 0.3526(9) 0.033(1) Uani 1.00 d . . . O(3) O -0.4604(10) 0.0000 0.7404(14) 0.036(2) Uani 1.00 d S . . C(1) C -0.1424(7) 0.0970(8) 0.2494(11) 0.021(2) Uani 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt 0.0134(3) 0.0110(3) 0.0129(3) 0.0000 0.0066(2) 0.0000 Ag 0.0232(5) 0.0299(4) 0.0279(4) 0.0000 0.0127(4) 0.0000 O(1) 0.033(3) 0.017(2) 0.026(2) 0.001(2) 0.021(2) 0.001(2) O(2) 0.049(3) 0.025(2) 0.041(3) -0.001(2) 0.036(3) -0.007(2) O(3) 0.044(5) 0.020(3) 0.042(5) 0.0000 0.019(4) 0.0000 C(1) 0.023(3) 0.020(3) 0.026(3) -0.004(3) 0.015(3) -0.004(3) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0059(7) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 585 _refine_ls_number_parameters 45 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0241 _refine_ls_wR_factor_obs 0.0302 _refine_ls_goodness_of_fit_obs 2.335 _refine_ls_shift/su_max 0.0030 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -1.29 _refine_diff_density_max 1.47 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt Ag 2.9425(8) 1_555 1_554 yes Pt Ag 2.9425(8) 1_555 3_556 yes Pt O(1) 2.003(4) 1_555 1_555 yes Pt O(1) 2.003(4) 1_555 2_555 yes Pt O(1) 2.003(4) 1_555 3_555 yes Pt O(1) 2.003(4) 1_555 4_555 yes Ag O(2) 2.559(5) 1_555 1_555 yes Ag O(2) 2.559(5) 1_555 2_555 yes Ag O(2) 2.632(5) 1_555 8_446 yes Ag O(2) 2.632(5) 1_555 7_456 yes Ag O(3) 2.424(8) 1_555 1_555 yes Ag O(3) 2.502(9) 1_555 3_456 yes O(1) C(1) 1.288(7) 1_555 1_555 yes O(2) C(1) 1.218(7) 1_555 1_555 yes C(1) C(1) 1.54(1) 1_555 2_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag Pt Ag 180.0 1_554 1_555 3_556 yes Ag Pt O(1) 93.0(1) 1_554 1_555 1_555 yes Ag Pt O(1) 93.0(1) 1_554 1_555 2_555 yes Ag Pt O(1) 87.0(1) 1_554 1_555 3_555 yes Ag Pt O(1) 87.0(1) 1_554 1_555 4_555 yes Ag Pt O(1) 87.0(1) 3_556 1_555 1_555 yes Ag Pt O(1) 87.0(1) 3_556 1_555 2_555 yes Ag Pt O(1) 93.0(1) 3_556 1_555 3_555 yes Ag Pt O(1) 93.0(1) 3_556 1_555 4_555 yes O(1) Pt O(1) 82.4(2) 1_555 1_555 2_555 yes O(1) Pt O(1) 180.0 1_555 1_555 3_555 yes O(1) Pt O(1) 97.6(2) 1_555 1_555 4_555 yes O(1) Pt O(1) 97.6(2) 2_555 1_555 3_555 yes O(1) Pt O(1) 180.0 2_555 1_555 4_555 yes O(1) Pt O(1) 82.4(2) 3_555 1_555 4_555 yes Pt Ag O(2) 100.8(1) 1_556 1_555 1_555 yes Pt Ag O(2) 100.8(1) 1_556 1_555 2_555 yes Pt Ag O(2) 87.3(1) 1_556 1_555 8_446 yes Pt Ag O(2) 87.3(1) 1_556 1_555 7_456 yes Pt Ag O(3) 96.0(2) 1_556 1_555 1_555 yes Pt Ag O(3) 173.1(2) 1_556 1_555 3_456 yes O(2) Ag O(2) 65.7(2) 1_555 1_555 2_555 yes O(2) Ag O(2) 135.4(1) 1_555 1_555 8_446 yes O(2) Ag O(2) 69.7(2) 1_555 1_555 7_456 yes O(2) Ag O(3) 142.7(1) 1_555 1_555 1_555 yes O(2) Ag O(3) 85.0(2) 1_555 1_555 3_456 yes O(2) Ag O(2) 69.7(2) 2_555 1_555 8_446 yes O(2) Ag O(2) 135.4(1) 2_555 1_555 7_456 yes O(2) Ag O(3) 142.7(1) 2_555 1_555 1_555 yes O(2) Ag O(3) 85.0(2) 2_555 1_555 3_456 yes O(2) Ag O(2) 154.9(2) 8_446 1_555 7_456 yes O(2) Ag O(3) 78.11(10) 8_446 1_555 1_555 yes O(2) Ag O(3) 91.2(1) 8_446 1_555 3_456 yes O(2) Ag O(3) 78.11(10) 7_456 1_555 1_555 yes O(2) Ag O(3) 91.2(1) 7_456 1_555 3_456 yes O(3) Ag O(3) 77.1(3) 1_555 1_555 3_456 yes Pt O(1) C(1) 113.3(4) 1_555 1_555 1_555 yes Ag O(2) Ag 110.3(2) 1_555 1_555 7_456 yes Ag O(2) C(1) 116.4(4) 1_555 1_555 1_555 yes Ag O(2) C(1) 133.1(4) 7_456 1_555 1_555 yes Ag O(3) Ag 102.9(3) 1_555 1_555 3_456 yes O(1) C(1) O(2) 124.1(6) 1_555 1_555 1_555 yes O(1) C(1) C(1) 115.3(4) 1_555 1_555 2_555 yes O(2) C(1) C(1) 120.6(4) 1_555 1_555 2_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt Ag 2.9425(8) 1_555 1_554 ? Pt Ag 2.9425(8) 1_555 3_556 ? Ag O(2) 2.559(5) 1_555 1_555 ? Ag O(2) 2.559(5) 1_555 2_555 ? Ag O(2) 2.632(5) 1_555 8_446 ? Ag O(2) 2.632(5) 1_555 7_456 ? Ag O(3) 2.502(9) 1_555 3_456 ? Ag O(1) 3.472(5) 1_555 4_556 ? O(1) O(1) 3.162(10) 1_555 7_455 ? O(1) O(2) 3.315(7) 1_555 7_455 ? O(1) C(1) 3.343(8) 1_555 7_455 ? O(1) O(2) 3.370(7) 1_555 4_556 ? O(2) C(1) 3.248(9) 1_555 4_556 ? O(2) O(2) 3.39(1) 1_555 4_556 ? O(3) C(1) 3.57(1) 1_555 1_556 ? O(3) C(1) 3.57(1) 1_555 2_556 ? C(1) C(1) 3.33(1) 1_555 4_556 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' Tasuku ITO' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, Tohoku University,Sendai 980-8578, JAPAN ; _publ_contact_author_email ' Ito@agnus.chem.tohoku.ac.jp ' _publ_contact_author_fax ' +81 22 217 6548 ' _publ_contact_author_phone ' +81 22 217 6544 ' _publ_requested_journal ' J.C.S.,Dalton Trans. ' #------------------------------------------------------------------------------ #=END data_2 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution DIRDIF91_PATTY _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1850.38 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H32 Ag4 F12 O22 Pt2 S4 ' _chemical_formula_moiety 'C24 H32 Ag4 F12 O22 Pt2 S4 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.039(7) _cell_length_b 12.287(3) _cell_length_c 15.000(3) _cell_angle_alpha 90 _cell_angle_beta 102.90(2) _cell_angle_gamma 90 _cell_volume 2342(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 14.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736.00 _exptl_absorpt_coefficient_mu 7.860 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 1.000 #------------------------------------------------------------------------------ _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.86 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 4 -3 0 3 -2 0 2 _diffrn_reflns_number 5872 _reflns_number_total 5635 _reflns_number_observed 2985 _reflns_observed_expression >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.112 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03233 _diffrn_orient_matrix_UB_12 -0.00321 _diffrn_orient_matrix_UB_13 0.05445 _diffrn_orient_matrix_UB_21 0.07153 _diffrn_orient_matrix_UB_22 -0.00749 _diffrn_orient_matrix_UB_23 0.04096 _diffrn_orient_matrix_UB_31 0.00534 _diffrn_orient_matrix_UB_32 0.08098 _diffrn_orient_matrix_UB_33 0.00595 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Pt' 'Pt' -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags Pt Pt -0.02852(4) -0.36292(5) -0.00396(4) 0.0453(1) Uani 1.00 d Ag(1) Ag -0.01459(8) -0.13448(9) -0.00825(7) 0.0488(3) Uani 1.00 d Ag(2) Ag 0.2728(1) -0.1545(1) 0.28365(8) 0.0841(5) Uani 1.00 d S(1) S 0.0281(3) -0.0027(4) 0.2130(3) 0.061(1) Uani 1.00 d S(2) S 0.2390(3) -0.0269(4) 0.0650(3) 0.056(1) Uani 1.00 d F(1) F -0.092(2) -0.076(1) 0.313(1) 0.23(1) Uani 1.00 d F(2) F -0.154(1) 0.057(2) 0.2332(9) 0.228(9) Uani 1.00 d F(3) F -0.0391(9) 0.077(1) 0.3488(7) 0.134(5) Uani 1.00 d F(4) F 0.4167(8) 0.0403(9) 0.0407(7) 0.109(4) Uani 1.00 d F(5) F 0.3083(10) 0.007(1) -0.0802(7) 0.165(6) Uani 1.00 d F(6) F 0.3877(9) -0.1219(9) 0.0040(9) 0.132(5) Uani 1.00 d O(1) O -0.1823(7) -0.3463(8) -0.0414(6) 0.057(3) Uani 1.00 d O(2) O -0.0261(8) -0.3602(9) 0.1288(6) 0.065(3) Uani 1.00 d O(3) O 0.1267(7) -0.3750(8) 0.0340(6) 0.059(3) Uani 1.00 d O(4) O -0.0314(7) -0.3619(8) -0.1362(6) 0.058(3) Uani 1.00 d O(5) O -0.016(1) -0.079(1) 0.1454(8) 0.148(7) Uani 1.00 d O(6) O 0.1136(8) -0.037(1) 0.2782(7) 0.114(5) Uani 1.00 d O(7) O 0.038(1) 0.101(1) 0.1772(9) 0.135(7) Uani 1.00 d O(8) O 0.1729(8) -0.111(1) 0.0253(10) 0.118(6) Uani 1.00 d O(9) O 0.1935(8) 0.0775(9) 0.0495(8) 0.087(4) Uani 1.00 d O(10) O 0.3006(8) -0.042(1) 0.1551(7) 0.121(5) Uani 1.00 d O(11) O 0.195(1) -0.3191(10) 0.2437(9) 0.148(6) Uani 1.00 d C(1) C -0.359(1) -0.306(1) -0.0360(10) 0.063(5) Uani 1.00 d C(2) C -0.245(1) -0.326(1) 0.0137(10) 0.061(5) Uani 1.00 d C(3) C -0.210(1) -0.319(1) 0.1084(9) 0.061(5) Uani 1.00 d C(4) C -0.108(1) -0.339(1) 0.1584(10) 0.062(5) Uani 1.00 d C(5) C -0.081(1) -0.334(2) 0.2650(10) 0.091(7) Uani 1.00 d C(6) C 0.305(1) -0.374(1) 0.027(1) 0.078(6) Uani 1.00 d C(7) C 0.188(1) -0.369(1) -0.023(1) 0.063(5) Uani 1.00 d C(8) C 0.156(1) -0.364(1) -0.114(1) 0.064(5) Uani 1.00 d C(9) C 0.051(1) -0.361(1) -0.169(1) 0.063(5) Uani 1.00 d C(10) C 0.027(1) -0.353(2) -0.2721(9) 0.083(6) Uani 1.00 d C(11) C -0.070(2) 0.017(2) 0.280(2) 0.100(9) Uani 1.00 d C(12) C 0.339(1) -0.030(2) 0.001(1) 0.078(7) Uani 1.00 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt 0.0476(3) 0.0406(2) 0.0463(3) -0.0047(3) 0.0074(2) 0.0000(3) Ag(1) 0.0448(6) 0.0487(5) 0.0552(6) -0.0026(6) 0.0161(5) -0.0010(6) Ag(2) 0.0725(9) 0.120(1) 0.0587(8) -0.0100(9) 0.0121(7) 0.0054(8) S(1) 0.055(3) 0.093(3) 0.041(2) 0.018(2) 0.026(2) 0.000(2) S(2) 0.034(2) 0.085(3) 0.056(2) 0.000(2) 0.020(2) 0.009(2) F(1) 0.27(2) 0.20(2) 0.32(2) -0.07(2) 0.25(2) -0.04(2) F(2) 0.073(9) 0.50(4) 0.12(1) 0.09(2) 0.026(8) -0.05(2) F(3) 0.119(10) 0.22(2) 0.072(7) 0.013(10) 0.042(7) -0.051(9) F(4) 0.071(7) 0.127(9) 0.144(10) -0.021(7) 0.058(7) -0.014(8) F(5) 0.14(1) 0.31(2) 0.060(7) 0.05(1) 0.061(7) 0.026(10) F(6) 0.116(9) 0.087(8) 0.23(1) 0.006(8) 0.117(10) -0.025(9) O(1) 0.057(6) 0.058(6) 0.055(6) -0.001(5) 0.011(5) -0.006(5) O(2) 0.073(7) 0.078(7) 0.040(5) -0.004(7) 0.005(5) 0.008(6) O(3) 0.049(6) 0.054(6) 0.070(7) -0.004(5) 0.004(5) 0.014(5) O(4) 0.052(6) 0.073(7) 0.052(6) -0.006(6) 0.016(5) -0.007(6) O(5) 0.14(1) 0.23(2) 0.088(10) -0.02(1) 0.055(9) -0.08(1) O(6) 0.061(8) 0.22(2) 0.064(7) 0.056(9) 0.021(6) 0.012(9) O(7) 0.17(1) 0.12(1) 0.16(1) 0.03(1) 0.12(1) 0.04(1) O(8) 0.046(7) 0.10(1) 0.22(2) -0.005(7) 0.054(9) 0.00(1) O(9) 0.058(7) 0.093(9) 0.118(10) 0.019(7) 0.040(7) 0.000(8) O(10) 0.068(8) 0.25(2) 0.059(7) 0.03(1) 0.034(6) 0.048(9) O(11) 0.15(1) 0.09(1) 0.16(1) 0.008(9) -0.08(1) 0.003(9) C(1) 0.023(7) 0.09(1) 0.08(1) -0.006(8) 0.014(7) -0.009(9) C(2) 0.09(1) 0.043(8) 0.07(1) -0.026(8) 0.055(10) -0.016(7) C(3) 0.06(1) 0.07(1) 0.046(9) -0.008(9) 0.010(8) 0.007(8) C(4) 0.09(1) 0.05(1) 0.046(9) -0.012(9) 0.029(9) 0.005(7) C(5) 0.12(2) 0.12(2) 0.038(9) -0.01(1) 0.023(9) 0.008(10) C(6) 0.038(9) 0.08(1) 0.12(1) -0.002(9) 0.014(9) 0.00(1) C(7) 0.06(1) 0.041(8) 0.09(1) 0.004(8) 0.028(9) -0.006(9) C(8) 0.054(10) 0.070(10) 0.068(10) 0.001(9) 0.013(8) -0.004(10) C(9) 0.06(1) 0.052(8) 0.08(1) 0.002(9) 0.028(9) -0.022(9) C(10) 0.09(1) 0.13(2) 0.039(8) -0.01(1) 0.035(8) -0.02(1) C(11) 0.07(1) 0.15(2) 0.09(2) -0.02(1) 0.03(1) 0.00(2) C(12) 0.04(1) 0.12(2) 0.08(1) 0.00(1) 0.025(10) 0.01(1) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2985 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0455 _refine_ls_wR_factor_obs 0.0370 _refine_ls_goodness_of_fit_obs 1.926 _refine_ls_shift/su_max 0.1746 _refine_ls_shift/su_mean 0.0225 _refine_diff_density_min -1.07 _refine_diff_density_max 1.29 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt Ag(1) 2.814(1) 1_555 1_555 yes Pt O(1) 1.968(9) 1_555 1_555 yes Pt O(2) 1.985(9) 1_555 1_555 yes Pt O(3) 1.982(9) 1_555 1_555 yes Pt O(4) 1.976(8) 1_555 1_555 yes Ag(1) Ag(1) 3.329(2) 1_555 3_555 yes Ag(1) O(5) 2.41(1) 1_555 1_555 yes Ag(1) O(7) 2.52(1) 1_555 3_555 yes Ag(1) O(8) 2.40(1) 1_555 1_555 yes Ag(1) O(9) 2.38(1) 1_555 3_555 yes Ag(2) O(1) 2.557(9) 1_555 4_545 yes Ag(2) O(4) 2.575(9) 1_555 4_545 yes Ag(2) O(6) 2.52(1) 1_555 1_555 yes Ag(2) O(10) 2.47(1) 1_555 1_555 yes Ag(2) O(11) 2.28(1) 1_555 1_555 yes S(1) O(5) 1.41(1) 1_555 1_555 yes S(1) O(6) 1.37(1) 1_555 1_555 yes S(1) O(7) 1.40(1) 1_555 1_555 yes S(1) C(11) 1.80(2) 1_555 1_555 yes S(2) O(8) 1.39(1) 1_555 1_555 yes S(2) O(9) 1.41(1) 1_555 1_555 yes S(2) O(10) 1.42(1) 1_555 1_555 yes S(2) C(12) 1.78(2) 1_555 1_555 yes F(1) C(11) 1.31(3) 1_555 1_555 yes F(2) C(11) 1.26(3) 1_555 1_555 yes F(3) C(11) 1.27(2) 1_555 1_555 yes F(4) C(12) 1.37(2) 1_555 1_555 yes F(5) C(12) 1.28(2) 1_555 1_555 yes F(6) C(12) 1.29(2) 1_555 1_555 yes O(1) C(2) 1.31(1) 1_555 1_555 yes O(2) C(4) 1.27(2) 1_555 1_555 yes O(3) C(7) 1.30(2) 1_555 1_555 yes O(4) C(9) 1.28(1) 1_555 1_555 yes C(1) C(2) 1.52(2) 1_555 1_555 yes C(2) C(3) 1.40(2) 1_555 1_555 yes C(3) C(4) 1.39(2) 1_555 1_555 yes C(4) C(5) 1.56(2) 1_555 1_555 yes C(6) C(7) 1.54(2) 1_555 1_555 yes C(7) C(8) 1.34(2) 1_555 1_555 yes C(8) C(9) 1.43(2) 1_555 1_555 yes C(9) C(10) 1.51(2) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ag(1) Pt O(1) 87.5(3) 1_555 1_555 1_555 yes Ag(1) Pt O(2) 91.1(3) 1_555 1_555 1_555 yes Ag(1) Pt O(3) 90.8(3) 1_555 1_555 1_555 yes Ag(1) Pt O(4) 87.6(3) 1_555 1_555 1_555 yes O(1) Pt O(2) 94.1(4) 1_555 1_555 1_555 yes O(1) Pt O(3) 178.3(4) 1_555 1_555 1_555 yes O(1) Pt O(4) 85.6(4) 1_555 1_555 1_555 yes O(2) Pt O(3) 85.8(4) 1_555 1_555 1_555 yes O(2) Pt O(4) 178.6(4) 1_555 1_555 1_555 yes O(3) Pt O(4) 94.5(4) 1_555 1_555 1_555 yes Pt Ag(1) Ag(1) 174.33(6) 1_555 1_555 3_555 yes Pt Ag(1) O(5) 104.2(4) 1_555 1_555 1_555 yes Pt Ag(1) O(7) 101.2(3) 1_555 1_555 3_555 yes Pt Ag(1) O(8) 100.5(3) 1_555 1_555 1_555 yes Pt Ag(1) O(9) 103.6(3) 1_555 1_555 3_555 yes Ag(1) Ag(1) O(5) 70.9(4) 3_555 1_555 1_555 yes Ag(1) Ag(1) O(7) 84.1(3) 3_555 1_555 3_555 yes Ag(1) Ag(1) O(8) 76.8(3) 3_555 1_555 1_555 yes Ag(1) Ag(1) O(9) 79.4(3) 3_555 1_555 3_555 yes O(5) Ag(1) O(7) 153.0(5) 1_555 1_555 3_555 yes O(5) Ag(1) O(8) 89.5(5) 1_555 1_555 1_555 yes O(5) Ag(1) O(9) 87.1(4) 1_555 1_555 3_555 yes O(7) Ag(1) O(8) 94.7(5) 3_555 1_555 1_555 yes O(7) Ag(1) O(9) 78.3(4) 3_555 1_555 3_555 yes O(8) Ag(1) O(9) 155.8(4) 1_555 1_555 3_555 yes O(1) Ag(2) O(4) 62.9(3) 4_545 1_555 4_545 yes O(1) Ag(2) O(6) 91.7(3) 4_545 1_555 1_555 yes O(1) Ag(2) O(10) 139.5(4) 4_545 1_555 1_555 yes O(1) Ag(2) O(11) 105.0(4) 4_545 1_555 1_555 yes O(4) Ag(2) O(6) 134.0(4) 4_545 1_555 1_555 yes O(4) Ag(2) O(10) 91.0(3) 4_545 1_555 1_555 yes O(4) Ag(2) O(11) 122.0(4) 4_545 1_555 1_555 yes O(6) Ag(2) O(10) 85.2(4) 1_555 1_555 1_555 yes O(6) Ag(2) O(11) 100.6(5) 1_555 1_555 1_555 yes O(10) Ag(2) O(11) 115.3(5) 1_555 1_555 1_555 yes O(5) S(1) O(6) 116.6(9) 1_555 1_555 1_555 yes O(5) S(1) O(7) 112.8(9) 1_555 1_555 1_555 yes O(5) S(1) C(11) 105.3(10) 1_555 1_555 1_555 yes O(6) S(1) O(7) 114.7(10) 1_555 1_555 1_555 yes O(6) S(1) C(11) 101.9(9) 1_555 1_555 1_555 yes O(7) S(1) C(11) 103(1) 1_555 1_555 1_555 yes O(8) S(2) O(9) 114.1(7) 1_555 1_555 1_555 yes O(8) S(2) O(10) 118.4(9) 1_555 1_555 1_555 yes O(8) S(2) C(12) 102.1(9) 1_555 1_555 1_555 yes O(9) S(2) O(10) 113.6(8) 1_555 1_555 1_555 yes O(9) S(2) C(12) 105.3(8) 1_555 1_555 1_555 yes O(10) S(2) C(12) 100.5(7) 1_555 1_555 1_555 yes Pt O(1) Ag(2) 106.2(4) 1_555 1_555 4_444 yes Pt O(1) C(2) 125.4(9) 1_555 1_555 1_555 yes Ag(2) O(1) C(2) 127.9(9) 4_444 1_555 1_555 yes Pt O(2) C(4) 121.8(9) 1_555 1_555 1_555 yes Pt O(3) C(7) 123.0(9) 1_555 1_555 1_555 yes Pt O(4) Ag(2) 105.3(4) 1_555 1_555 4_444 yes Pt O(4) C(9) 123.9(9) 1_555 1_555 1_555 yes Ag(2) O(4) C(9) 130.6(9) 4_444 1_555 1_555 yes Ag(1) O(5) S(1) 142.1(9) 1_555 1_555 1_555 yes Ag(2) O(6) S(1) 136.9(7) 1_555 1_555 1_555 yes Ag(1) O(7) S(1) 122.5(9) 3_555 1_555 1_555 yes Ag(1) O(8) S(2) 133.1(7) 1_555 1_555 1_555 yes Ag(1) O(9) S(2) 131.4(7) 3_555 1_555 1_555 yes Ag(2) O(10) S(2) 131.7(8) 1_555 1_555 1_555 yes O(1) C(2) C(1) 113(1) 1_555 1_555 1_555 yes O(1) C(2) C(3) 123(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 123(1) 1_555 1_555 1_555 yes C(2) C(3) C(4) 126(1) 1_555 1_555 1_555 yes O(2) C(4) C(3) 128(1) 1_555 1_555 1_555 yes O(2) C(4) C(5) 110(1) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120(1) 1_555 1_555 1_555 yes O(3) C(7) C(6) 111(1) 1_555 1_555 1_555 yes O(3) C(7) C(8) 125(1) 1_555 1_555 1_555 yes C(6) C(7) C(8) 123(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 129(1) 1_555 1_555 1_555 yes O(4) C(9) C(8) 123(1) 1_555 1_555 1_555 yes O(4) C(9) C(10) 113(1) 1_555 1_555 1_555 yes C(8) C(9) C(10) 122(1) 1_555 1_555 1_555 yes S(1) C(11) F(1) 109(1) 1_555 1_555 1_555 yes S(1) C(11) F(2) 112(1) 1_555 1_555 1_555 yes S(1) C(11) F(3) 113(1) 1_555 1_555 1_555 yes F(1) C(11) F(2) 108(2) 1_555 1_555 1_555 yes F(1) C(11) F(3) 104(2) 1_555 1_555 1_555 yes F(2) C(11) F(3) 107(2) 1_555 1_555 1_555 yes S(2) C(12) F(4) 108(1) 1_555 1_555 1_555 yes S(2) C(12) F(5) 113(1) 1_555 1_555 1_555 yes S(2) C(12) F(6) 114(1) 1_555 1_555 1_555 yes F(4) C(12) F(5) 103(1) 1_555 1_555 1_555 yes F(4) C(12) F(6) 103(1) 1_555 1_555 1_555 yes F(5) C(12) F(6) 112(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt Ag(1) 2.814(1) 1_555 1_555 ? Ag(1) Ag(1) 3.329(2) 1_555 3_555 ? Ag(1) O(7) 2.52(1) 1_555 3_555 ? Ag(2) O(1) 2.557(9) 1_555 4_545 ? Ag(2) O(4) 2.575(9) 1_555 4_545 ? Ag(2) O(6) 2.52(1) 1_555 1_555 ? Pt Pt 3.446(1) 1_555 3_545 ? Pt O(3) 3.458(10) 1_555 3_545 ? F(3) C(6) 3.26(2) 1_555 2_555 ? F(4) F(4) 2.89(2) 1_555 3_655 ? F(4) F(6) 2.95(1) 1_555 3_655 ? F(4) C(12) 3.39(2) 1_555 3_655 ? F(4) F(5) 3.55(2) 1_555 3_655 ? F(4) C(5) 3.56(2) 1_555 2_555 ? O(1) O(3) 3.50(1) 1_555 3_545 ? O(2) O(4) 3.49(1) 1_555 3_545 ? O(2) C(9) 3.50(2) 1_555 3_545 ? O(4) O(10) 3.60(1) 1_555 4_444 ? O(6) C(6) 3.50(2) 1_555 2_555 ? O(7) O(11) 3.56(2) 1_555 2_555 ? O(9) O(11) 3.37(2) 1_555 2_555 ? O(10) O(11) 3.12(2) 1_555 2_555 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' Tasuku ITO' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, Tohoku University,Sendai 980-8578, JAPAN ; _publ_contact_author_email ' Ito@agnus.chem.tohoku.ac.jp ' _publ_contact_author_fax ' +81 22 217 6548 ' _publ_contact_author_phone ' +81 22 217 6544 ' _publ_requested_journal ' J.C.S.,Dalton Trans. '