# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1272 data_[Ag2(calix[4]resor)(C6H6)2 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 28 09:54:20 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 735.98 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H40 Ag Cl O10.50 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 25.049(8) _cell_length_b 15.247(2) _cell_length_c 17.934(2) _cell_angle_alpha 90 _cell_angle_beta 95.40(2) _cell_angle_gamma 90 _cell_volume 6818(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 14.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040.00 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.40 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 3 1 2 0 4 -4 2 2 _diffrn_reflns_number 8297 _reflns_number_total 8112 _reflns_number_gt 2803 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.150 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00728 _diffrn_orient_matrix_UB_12 0.02187 _diffrn_orient_matrix_UB_13 0.05255 _diffrn_orient_matrix_UB_21 0.02637 _diffrn_orient_matrix_UB_22 0.04318 _diffrn_orient_matrix_UB_23 -0.01694 _diffrn_orient_matrix_UB_31 -0.02932 _diffrn_orient_matrix_UB_32 0.04426 _diffrn_orient_matrix_UB_33 -0.00940 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;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) ; '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) ; #------------------------------------------------------------------------------ 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 Ag(1) Ag 0.85650(3) 0.10608(5) 0.67902(5) 0.0907(3) Uani 1.00 d . . . Cl(1) Cl 1.3743(1) -0.1221(2) 0.8229(2) 0.109(1) Uani 1.00 d . . . O(1) O 0.8855(2) 0.1408(4) 0.8107(4) 0.095(2) Uani 1.00 d . . . O(2) O 1.0706(2) 0.1282(4) 0.9033(4) 0.093(2) Uani 1.00 d . . . O(3) O 1.1760(3) -0.0857(5) 0.9820(3) 0.098(2) Uani 1.00 d . . . O(4) O 1.2349(2) -0.0738(5) 0.7373(4) 0.096(2) Uani 1.00 d . . . O(5) O 1.3293(6) -0.175(1) 0.8331(10) 0.266(8) Uani 1.00 d . . . O(6) O 1.3513(8) -0.074(1) 0.766(1) 0.35(1) Uani 1.00 d . . . O(7) O 1.4113(4) -0.1738(8) 0.8039(9) 0.236(6) Uani 1.00 d . . . O(8) O 1.3853(9) -0.070(1) 0.878(1) 0.34(1) Uani 1.00 d . . . O(9) O 0.4310(4) -0.2063(5) 0.5653(6) 0.139(4) Uani 1.00 d . . . O(10) O 0.2748(4) 0.1058(8) 0.5420(5) 0.165(4) Uani 1.00 d . . . O(11) O 0.0000 0.422(1) 0.2500 0.31(2) Uani 1.00 d S . . C(1) C 0.7953(5) 0.2237(8) 0.633(1) 0.109(5) Uani 1.00 d . . . C(2) C 0.7578(9) 0.196(1) 0.6755(8) 0.136(6) Uani 1.00 d . . . C(3) C 0.7211(7) 0.132(1) 0.650(1) 0.144(7) Uani 1.00 d . . . C(4) C 0.7227(7) 0.098(1) 0.583(1) 0.140(7) Uani 1.00 d . . . C(5) C 0.7603(9) 0.127(1) 0.5383(9) 0.145(7) Uani 1.00 d . . . C(6) C 0.7975(6) 0.189(1) 0.563(1) 0.132(6) Uani 1.00 d . . . C(7) C 0.9293(4) 0.0945(6) 0.8395(5) 0.074(3) Uani 1.00 d . . . C(8) C 0.9233(3) 0.0056(6) 0.8518(4) 0.064(3) Uani 1.00 d . . . C(9) C 0.9687(3) -0.0417(5) 0.8797(4) 0.062(3) Uani 1.00 d . . . C(10) C 1.0190(3) -0.0022(6) 0.8972(4) 0.062(3) Uani 1.00 d . . . C(11) C 1.0224(4) 0.0877(6) 0.8857(5) 0.073(3) Uani 1.00 d . . . C(12) C 0.9783(4) 0.1344(6) 0.8565(5) 0.078(3) Uani 1.00 d . . . C(13) C 0.8687(3) -0.0375(6) 0.8334(4) 0.068(3) Uani 1.00 d . . . C(14) C 0.8637(4) -0.1249(8) 0.8734(5) 0.101(4) Uani 1.00 d . . . C(15) C 1.0685(3) -0.0534(6) 0.9308(4) 0.068(3) Uani 1.00 d . . . C(16) C 1.0550(4) -0.1451(8) 0.9538(5) 0.093(4) Uani 1.00 d . . . C(17) C 1.1127(3) -0.0579(5) 0.8788(4) 0.057(3) Uani 1.00 d . . . C(18) C 1.1648(4) -0.0771(6) 0.9067(5) 0.074(3) Uani 1.00 d . . . C(19) C 1.2060(4) -0.0838(6) 0.8597(6) 0.074(3) Uani 1.00 d . . . C(20) C 1.1948(3) -0.0706(6) 0.7836(6) 0.070(3) Uani 1.00 d . . . C(21) C 1.1425(3) -0.0512(5) 0.7516(5) 0.059(3) Uani 1.00 d . . . C(22) C 1.1037(3) -0.0454(5) 0.8011(5) 0.059(3) Uani 1.00 d . . . C(23) C 0.4408(9) -0.134(1) 0.615(1) 0.202(9) Uani 1.00 d . . . C(24) C 0.449(1) -0.061(1) 0.567(2) 0.26(1) Uani 1.00 d . . . C(25) C 0.450(2) -0.098(2) 0.495(2) 0.36(2) Uani 1.00 d . . . C(26) C 0.4356(9) -0.181(1) 0.4912(10) 0.195(9) Uani 1.00 d . . . C(27) C 0.2736(9) 0.094(2) 0.620(1) 0.34(1) Uani 1.00 d . . . C(28) C 0.322(1) 0.125(2) 0.652(1) 0.28(1) Uani 1.00 d . . . C(29) C 0.3525(8) 0.162(1) 0.599(1) 0.218(10) Uani 1.00 d . . . C(30) C 0.3146(7) 0.164(1) 0.5311(9) 0.196(8) Uani 1.00 d . . . C(31) C 0.0512(8) 0.350(2) 0.229(1) 0.21(1) Uani 1.00 d . . . C(32) C 0.0241(8) 0.266(1) 0.242(1) 0.19(1) Uani 1.00 d . . . H(1) H 0.7564 0.2225 0.7266 0.1673 Uiso 1.00 calc . . . H(2) H 0.6939 0.1117 0.6827 0.1775 Uiso 1.00 calc . . . H(3) H 0.6967 0.0514 0.5667 0.1617 Uiso 1.00 calc . . . H(4) H 0.7615 0.1004 0.4891 0.1734 Uiso 1.00 calc . . . H(5) H 0.8250 0.2100 0.5323 0.1542 Uiso 1.00 calc . . . H(6) H 0.9654 -0.1030 0.8866 0.0739 Uiso 1.00 calc . . . H(7) H 0.9816 0.1953 0.8474 0.0926 Uiso 1.00 calc . . . H(8) H 0.8289 -0.1481 0.8603 0.1204 Uiso 1.00 calc . . . H(9) H 0.8899 -0.1638 0.8577 0.1204 Uiso 1.00 calc . . . H(10) H 0.8691 -0.1157 0.9255 0.1204 Uiso 1.00 calc . . . H(11) H 1.0278 -0.1424 0.9868 0.1113 Uiso 1.00 calc . . . H(12) H 1.0435 -0.1776 0.9107 0.1113 Uiso 1.00 calc . . . H(13) H 1.0864 -0.1711 0.9787 0.1113 Uiso 1.00 calc . . . H(14) H 1.2416 -0.0976 0.8802 0.0891 Uiso 1.00 calc . . . H(15) H 1.0681 -0.0323 0.7811 0.0717 Uiso 1.00 calc . . . H(16) H 1.1839 -0.0922 1.0342 0.1188 Uiso 1.00 calc . . . H(17) H 1.2631 -0.0763 0.7054 0.1165 Uiso 1.00 calc . . . H(18) H 0.8213 0.2702 0.6527 0.1339 Uiso 1.00 calc . . . H(19) H 0.8547 0.1738 0.7901 0.1130 Uiso 1.00 calc . . . H(20) H 1.1047 0.1570 0.9159 0.1086 Uiso 1.00 calc . . . 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 Ag(1) 0.0867(6) 0.0700(5) 0.1085(6) 0.0044(4) -0.0267(4) 0.0127(4) Cl(1) 0.077(2) 0.102(2) 0.147(3) 0.010(2) 0.003(2) -0.018(2) O(1) 0.077(4) 0.091(4) 0.109(5) 0.036(4) -0.032(4) -0.013(4) O(2) 0.070(4) 0.087(4) 0.115(5) 0.002(3) -0.027(3) -0.035(4) O(3) 0.093(4) 0.145(6) 0.054(4) 0.030(4) -0.015(3) 0.006(4) O(4) 0.062(4) 0.138(6) 0.091(5) 0.006(4) 0.022(4) -0.001(4) O(5) 0.21(1) 0.26(2) 0.34(2) -0.11(1) 0.11(1) -0.06(1) O(6) 0.27(2) 0.28(2) 0.46(3) 0.08(2) -0.14(2) 0.09(2) O(7) 0.121(8) 0.17(1) 0.42(2) 0.066(8) 0.033(10) -0.03(1) O(8) 0.43(3) 0.28(2) 0.30(2) -0.06(2) 0.02(2) -0.18(2) O(9) 0.196(9) 0.074(5) 0.145(8) -0.010(5) 0.004(6) 0.032(6) O(10) 0.111(7) 0.26(1) 0.111(7) -0.069(7) -0.028(5) -0.008(7) O(11) 0.53(5) 0.15(2) 0.20(2) 0.0000 -0.18(3) 0.0000 C(1) 0.084(9) 0.078(8) 0.16(1) 0.004(6) -0.025(9) 0.028(9) C(2) 0.17(2) 0.11(1) 0.13(1) 0.01(1) 0.00(1) -0.009(9) C(3) 0.13(1) 0.14(2) 0.17(2) 0.00(1) 0.03(1) 0.03(1) C(4) 0.10(1) 0.12(1) 0.19(2) 0.007(9) -0.03(1) 0.02(1) C(5) 0.15(1) 0.15(1) 0.13(1) 0.02(1) -0.05(1) -0.01(1) C(6) 0.12(1) 0.13(1) 0.15(1) 0.014(10) 0.02(1) 0.04(1) C(7) 0.075(6) 0.073(6) 0.071(6) 0.023(5) -0.010(5) -0.019(5) C(8) 0.064(5) 0.081(6) 0.045(5) 0.012(5) -0.002(4) -0.012(4) C(9) 0.071(6) 0.068(5) 0.045(5) 0.015(5) 0.000(4) -0.015(4) C(10) 0.073(6) 0.075(6) 0.038(4) 0.020(5) 0.000(4) -0.013(4) C(11) 0.075(6) 0.077(7) 0.064(5) 0.012(5) -0.013(4) -0.024(5) C(12) 0.087(7) 0.064(5) 0.079(6) 0.017(5) -0.020(5) -0.017(4) C(13) 0.063(5) 0.090(6) 0.052(5) 0.001(5) 0.005(4) 0.001(5) C(14) 0.084(7) 0.15(1) 0.072(6) -0.011(7) 0.001(5) 0.026(6) C(15) 0.068(6) 0.084(6) 0.049(5) 0.028(5) -0.006(4) -0.001(4) C(16) 0.074(6) 0.130(9) 0.073(6) 0.031(6) 0.003(5) 0.030(6) C(17) 0.060(5) 0.059(5) 0.051(5) 0.009(4) -0.007(4) 0.001(4) C(18) 0.081(7) 0.070(6) 0.067(6) 0.014(5) -0.011(5) -0.003(4) C(19) 0.063(6) 0.074(6) 0.081(7) 0.015(4) -0.009(5) -0.003(5) C(20) 0.052(5) 0.068(5) 0.088(7) 0.013(4) 0.002(5) 0.004(5) C(21) 0.058(5) 0.057(5) 0.061(5) 0.000(4) 0.002(4) -0.005(4) C(22) 0.055(5) 0.059(5) 0.061(5) 0.011(4) -0.011(4) -0.002(4) C(23) 0.33(3) 0.13(1) 0.16(2) -0.05(2) 0.07(2) -0.05(1) C(24) 0.45(4) 0.10(1) 0.24(3) -0.03(2) 0.07(3) -0.05(2) C(25) 0.69(7) 0.18(2) 0.18(2) -0.18(3) -0.01(3) 0.03(2) C(26) 0.34(3) 0.11(1) 0.13(1) -0.01(1) 0.01(1) 0.03(1) C(27) 0.19(2) 0.68(6) 0.12(1) -0.23(3) -0.07(1) 0.11(2) C(28) 0.22(2) 0.47(4) 0.14(2) -0.14(2) -0.04(2) 0.05(2) C(29) 0.21(2) 0.26(2) 0.16(2) -0.14(2) -0.07(1) 0.06(2) C(30) 0.16(1) 0.27(2) 0.16(1) -0.09(2) -0.04(1) 0.05(1) C(31) 0.14(2) 0.35(4) 0.15(2) -0.03(2) -0.02(1) 0.04(2) C(32) 0.27(4) 0.18(1) 0.12(1) 0.09(2) 0.02(2) 0.00(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _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) + 0.00090|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2803 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.689 _refine_ls_shift/su_max 0.5360 _refine_ls_shift/su_mean 0.0240 _refine_diff_density_min -0.46 _refine_diff_density_max 0.58 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Ag(1) O(1) 2.442(6) 1_555 1_555 yes Ag(1) O(2) 2.458(7) 1_555 2_756 yes Ag(1) C(1) 2.45(1) 1_555 1_555 yes Ag(1) C(22) 2.528(8) 1_555 2_756 yes Cl(1) O(5) 1.40(1) 1_555 1_555 yes Cl(1) O(6) 1.33(2) 1_555 1_555 yes Cl(1) O(7) 1.29(1) 1_555 1_555 yes Cl(1) O(8) 1.29(1) 1_555 1_555 yes O(1) C(7) 1.376(9) 1_555 1_555 yes O(2) C(11) 1.38(1) 1_555 1_555 yes O(3) C(18) 1.35(1) 1_555 1_555 yes O(4) C(20) 1.36(1) 1_555 1_555 yes O(9) C(23) 1.44(2) 1_555 1_555 yes O(9) C(26) 1.40(2) 1_555 1_555 yes O(10) C(27) 1.39(2) 1_555 1_555 yes O(10) C(30) 1.36(2) 1_555 1_555 yes O(11) C(31) 1.73(3) 1_555 1_555 yes O(11) C(31) 1.73(3) 1_555 2_555 yes C(1) C(2) 1.33(2) 1_555 1_555 yes C(1) C(6) 1.36(2) 1_555 1_555 yes C(2) C(3) 1.38(2) 1_555 1_555 yes C(3) C(4) 1.32(2) 1_555 1_555 yes C(4) C(5) 1.37(2) 1_555 1_555 yes C(5) C(6) 1.37(2) 1_555 1_555 yes C(7) C(8) 1.38(1) 1_555 1_555 yes C(7) C(12) 1.38(1) 1_555 1_555 yes C(8) C(9) 1.39(1) 1_555 1_555 yes C(8) C(13) 1.53(1) 1_555 1_555 yes C(9) C(10) 1.41(1) 1_555 1_555 yes C(10) C(11) 1.39(1) 1_555 1_555 yes C(10) C(15) 1.54(1) 1_555 1_555 yes C(11) C(12) 1.37(1) 1_555 1_555 yes C(13) C(14) 1.52(1) 1_555 1_555 yes C(13) C(21) 1.54(1) 1_555 2_756 yes C(15) C(16) 1.51(1) 1_555 1_555 yes C(15) C(17) 1.51(1) 1_555 1_555 yes C(17) C(18) 1.38(1) 1_555 1_555 yes C(17) C(22) 1.41(1) 1_555 1_555 yes C(18) C(19) 1.40(1) 1_555 1_555 yes C(19) C(20) 1.39(1) 1_555 1_555 yes C(20) C(21) 1.41(1) 1_555 1_555 yes C(21) C(22) 1.38(1) 1_555 1_555 yes C(23) C(24) 1.41(2) 1_555 1_555 yes C(24) C(25) 1.42(3) 1_555 1_555 yes C(25) C(26) 1.33(2) 1_555 1_555 yes C(27) C(28) 1.40(2) 1_555 1_555 yes C(28) C(29) 1.38(2) 1_555 1_555 yes C(29) C(30) 1.45(2) 1_555 1_555 yes C(31) C(32) 1.47(2) 1_555 1_555 yes C(32) C(32) 1.28(4) 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 O(1) Ag(1) O(2) 111.9(2) 1_555 1_555 2_756 yes O(1) Ag(1) C(1) 106.5(5) 1_555 1_555 1_555 yes O(1) Ag(1) C(22) 89.1(2) 1_555 1_555 2_756 yes O(2) Ag(1) C(1) 100.1(6) 2_756 1_555 1_555 yes O(2) Ag(1) C(22) 84.6(3) 2_756 1_555 2_756 yes C(1) Ag(1) C(22) 160.3(4) 1_555 1_555 2_756 yes O(5) Cl(1) O(6) 97(1) 1_555 1_555 1_555 yes O(5) Cl(1) O(7) 107.6(9) 1_555 1_555 1_555 yes O(5) Cl(1) O(8) 112(1) 1_555 1_555 1_555 yes O(6) Cl(1) O(7) 114(1) 1_555 1_555 1_555 yes O(6) Cl(1) O(8) 106(1) 1_555 1_555 1_555 yes O(7) Cl(1) O(8) 117(1) 1_555 1_555 1_555 yes Ag(1) O(1) C(7) 114.8(5) 1_555 1_555 1_555 yes Ag(1) O(1) H(19) 122.9(4) 1_555 1_555 1_555 no C(7) O(1) H(19) 122.3(7) 1_555 1_555 1_555 no Ag(1) O(2) C(11) 119.6(5) 2_756 1_555 1_555 yes Ag(1) O(2) H(20) 120.4(5) 2_756 1_555 1_555 no C(11) O(2) H(20) 119.9(7) 1_555 1_555 1_555 no C(18) O(3) H(16) 179.6(8) 1_555 1_555 1_555 no C(20) O(4) H(17) 179.9(8) 1_555 1_555 1_555 no C(23) O(9) C(26) 111(1) 1_555 1_555 1_555 yes C(27) O(10) C(30) 108(1) 1_555 1_555 1_555 yes C(31) O(11) C(31) 102(2) 1_555 1_555 2_555 yes Ag(1) C(1) C(2) 92.0(10) 1_555 1_555 1_555 yes Ag(1) C(1) C(6) 87.0(10) 1_555 1_555 1_555 yes Ag(1) C(1) H(18) 91.8(7) 1_555 1_555 1_555 no C(2) C(1) C(6) 119(1) 1_555 1_555 1_555 yes C(2) C(1) H(18) 119(2) 1_555 1_555 1_555 no C(6) C(1) H(18) 120(2) 1_555 1_555 1_555 no C(1) C(2) C(3) 120(1) 1_555 1_555 1_555 yes C(1) C(2) H(1) 118(2) 1_555 1_555 1_555 no C(3) C(2) H(1) 120(2) 1_555 1_555 1_555 no C(2) C(3) C(4) 120(1) 1_555 1_555 1_555 yes C(2) C(3) H(2) 120(2) 1_555 1_555 1_555 no C(4) C(3) H(2) 119(2) 1_555 1_555 1_555 no C(3) C(4) C(5) 119(1) 1_555 1_555 1_555 yes C(3) C(4) H(3) 118(2) 1_555 1_555 1_555 no C(5) C(4) H(3) 122(2) 1_555 1_555 1_555 no C(4) C(5) C(6) 120(1) 1_555 1_555 1_555 yes C(4) C(5) H(4) 118(2) 1_555 1_555 1_555 no C(6) C(5) H(4) 120(2) 1_555 1_555 1_555 no C(1) C(6) C(5) 118(1) 1_555 1_555 1_555 yes C(1) C(6) H(5) 119(2) 1_555 1_555 1_555 no C(5) C(6) H(5) 121(2) 1_555 1_555 1_555 no O(1) C(7) C(8) 118.1(9) 1_555 1_555 1_555 yes O(1) C(7) C(12) 121.1(9) 1_555 1_555 1_555 yes C(8) C(7) C(12) 120.7(8) 1_555 1_555 1_555 yes C(7) C(8) C(9) 117.6(9) 1_555 1_555 1_555 yes C(7) C(8) C(13) 119.3(8) 1_555 1_555 1_555 yes C(9) C(8) C(13) 123.1(9) 1_555 1_555 1_555 yes C(8) C(9) C(10) 123.0(8) 1_555 1_555 1_555 yes C(8) C(9) H(6) 118.5(9) 1_555 1_555 1_555 no C(10) C(9) H(6) 118.5(9) 1_555 1_555 1_555 no C(9) C(10) C(11) 116.6(8) 1_555 1_555 1_555 yes C(9) C(10) C(15) 123.6(8) 1_555 1_555 1_555 yes C(11) C(10) C(15) 119.7(9) 1_555 1_555 1_555 yes O(2) C(11) C(10) 118.0(8) 1_555 1_555 1_555 yes O(2) C(11) C(12) 120.9(9) 1_555 1_555 1_555 yes C(10) C(11) C(12) 121.1(9) 1_555 1_555 1_555 yes C(7) C(12) C(11) 120.9(9) 1_555 1_555 1_555 yes C(7) C(12) H(7) 119.4(9) 1_555 1_555 1_555 no C(11) C(12) H(7) 119.7(10) 1_555 1_555 1_555 no C(8) C(13) C(14) 112.4(7) 1_555 1_555 1_555 yes C(8) C(13) C(21) 110.2(7) 1_555 1_555 2_756 yes C(14) C(13) C(21) 109.0(8) 1_555 1_555 2_756 yes C(13) C(14) H(8) 109.4(9) 1_555 1_555 1_555 no C(13) C(14) H(9) 108.9(9) 1_555 1_555 1_555 no C(13) C(14) H(10) 109(1) 1_555 1_555 1_555 no H(8) C(14) H(9) 109(1) 1_555 1_555 1_555 no H(8) C(14) H(10) 110(1) 1_555 1_555 1_555 no H(9) C(14) H(10) 109(1) 1_555 1_555 1_555 no C(10) C(15) C(16) 112.0(8) 1_555 1_555 1_555 yes C(10) C(15) C(17) 113.0(7) 1_555 1_555 1_555 yes C(16) C(15) C(17) 108.5(7) 1_555 1_555 1_555 yes C(15) C(16) H(11) 109.4(10) 1_555 1_555 1_555 no C(15) C(16) H(12) 109.2(9) 1_555 1_555 1_555 no C(15) C(16) H(13) 108.8(10) 1_555 1_555 1_555 no H(11) C(16) H(12) 110(1) 1_555 1_555 1_555 no H(11) C(16) H(13) 109.9(9) 1_555 1_555 1_555 no H(12) C(16) H(13) 109(1) 1_555 1_555 1_555 no C(15) C(17) C(18) 120.2(8) 1_555 1_555 1_555 yes C(15) C(17) C(22) 123.5(7) 1_555 1_555 1_555 yes C(18) C(17) C(22) 116.3(8) 1_555 1_555 1_555 yes O(3) C(18) C(17) 118.6(9) 1_555 1_555 1_555 yes O(3) C(18) C(19) 120.0(9) 1_555 1_555 1_555 yes C(17) C(18) C(19) 121.3(9) 1_555 1_555 1_555 yes C(18) C(19) C(20) 119.9(9) 1_555 1_555 1_555 yes C(18) C(19) H(14) 119(1) 1_555 1_555 1_555 no C(20) C(19) H(14) 120(1) 1_555 1_555 1_555 no O(4) C(20) C(19) 120.2(8) 1_555 1_555 1_555 yes O(4) C(20) C(21) 118.3(9) 1_555 1_555 1_555 yes C(19) C(20) C(21) 121.5(9) 1_555 1_555 1_555 yes C(13) C(21) C(20) 120.2(9) 2_756 1_555 1_555 yes C(13) C(21) C(22) 124.2(7) 2_756 1_555 1_555 yes C(20) C(21) C(22) 115.7(8) 1_555 1_555 1_555 yes Ag(1) C(22) C(17) 87.5(5) 2_756 1_555 1_555 yes Ag(1) C(22) C(21) 81.7(5) 2_756 1_555 1_555 yes Ag(1) C(22) H(15) 101.6(5) 2_756 1_555 1_555 no C(17) C(22) C(21) 125.4(7) 1_555 1_555 1_555 yes C(17) C(22) H(15) 117.3(9) 1_555 1_555 1_555 no C(21) C(22) H(15) 117.4(9) 1_555 1_555 1_555 no O(9) C(23) C(24) 104(1) 1_555 1_555 1_555 yes C(23) C(24) C(25) 105(1) 1_555 1_555 1_555 yes C(24) C(25) C(26) 113(2) 1_555 1_555 1_555 yes O(9) C(26) C(25) 104(1) 1_555 1_555 1_555 yes O(10) C(27) C(28) 105(1) 1_555 1_555 1_555 yes C(27) C(28) C(29) 111(1) 1_555 1_555 1_555 yes C(28) C(29) C(30) 103(1) 1_555 1_555 1_555 yes O(10) C(30) C(29) 107(1) 1_555 1_555 1_555 yes O(11) C(31) C(32) 99(1) 1_555 1_555 1_555 yes C(31) C(32) C(32) 118(1) 1_555 1_555 2_555 yes #------------------------------------------------------------------------------ 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 Ag(1) O(1) C(7) C(8) -69.1(10) 1_555 1_555 1_555 1_555 yes Ag(1) O(1) C(7) C(12) 109.6(8) 1_555 1_555 1_555 1_555 yes Ag(1) O(2) C(11) C(10) 73.4(9) 1_555 2_756 2_756 2_756 yes Ag(1) O(2) C(11) C(12) -105.4(8) 1_555 2_756 2_756 2_756 yes Ag(1) C(1) C(2) C(3) -86(1) 1_555 1_555 1_555 1_555 yes Ag(1) C(1) C(6) C(5) 90(1) 1_555 1_555 1_555 1_555 yes Ag(1) C(22) C(17) C(15) 103.3(8) 1_555 2_756 2_756 2_756 yes Ag(1) C(22) C(17) C(18) -78.8(7) 1_555 2_756 2_756 2_756 yes Ag(1) C(22) C(21) C(13) -98.5(8) 1_555 2_756 2_756 1_555 yes Ag(1) C(22) C(21) C(20) 81.1(7) 1_555 2_756 2_756 2_756 yes O(1) Ag(1) O(2) C(11) 53.6(7) 1_555 1_555 2_756 2_756 yes O(1) Ag(1) C(1) C(2) -69(1) 1_555 1_555 1_555 1_555 yes O(1) Ag(1) C(1) C(6) 170(1) 1_555 1_555 1_555 1_555 yes O(1) Ag(1) C(22) C(17) -170.4(5) 1_555 1_555 2_756 2_756 yes O(1) Ag(1) C(22) C(21) 63.2(5) 1_555 1_555 2_756 2_756 yes O(1) C(7) C(8) C(9) 177.5(7) 1_555 1_555 1_555 1_555 yes O(1) C(7) C(8) C(13) -1(1) 1_555 1_555 1_555 1_555 yes O(1) C(7) C(12) C(11) -179.3(8) 1_555 1_555 1_555 1_555 yes O(2) Ag(1) O(1) C(7) -56.9(7) 1_555 2_756 2_756 2_756 yes O(2) Ag(1) C(1) C(2) 173(1) 1_555 2_756 2_756 2_756 yes O(2) Ag(1) C(1) C(6) 53(1) 1_555 2_756 2_756 2_756 yes O(2) Ag(1) C(22) C(17) -58.3(5) 1_555 2_756 1_555 1_555 yes O(2) Ag(1) C(22) C(21) 175.4(5) 1_555 2_756 1_555 1_555 yes O(2) C(11) C(10) C(9) 179.8(7) 1_555 1_555 1_555 1_555 yes O(2) C(11) C(10) C(15) 2(1) 1_555 1_555 1_555 1_555 yes O(2) C(11) C(12) C(7) -179.3(8) 1_555 1_555 1_555 1_555 yes O(3) C(18) C(17) C(15) -4(1) 1_555 1_555 1_555 1_555 yes O(3) C(18) C(17) C(22) 177.2(8) 1_555 1_555 1_555 1_555 yes O(3) C(18) C(19) C(20) -176.6(8) 1_555 1_555 1_555 1_555 yes O(4) C(20) C(19) C(18) 177.6(8) 1_555 1_555 1_555 1_555 yes O(4) C(20) C(21) C(13) 1(1) 1_555 1_555 1_555 2_756 yes O(4) C(20) C(21) C(22) -177.7(8) 1_555 1_555 1_555 1_555 yes O(9) C(23) C(24) C(25) -5(3) 1_555 1_555 1_555 1_555 yes O(9) C(26) C(25) C(24) -7(3) 1_555 1_555 1_555 1_555 yes O(10) C(27) C(28) C(29) 4(3) 1_555 1_555 1_555 1_555 yes O(10) C(30) C(29) C(28) -17(2) 1_555 1_555 1_555 1_555 yes O(11) C(31) C(32) C(32) 2(3) 1_555 1_555 1_555 2_555 yes O(11) C(31) C(32) C(32) 2(3) 1_555 2_555 2_555 1_555 yes C(1) Ag(1) O(1) C(7) -165.3(8) 1_555 1_555 1_555 1_555 yes C(1) Ag(1) O(2) C(11) 166.1(7) 1_555 1_555 2_756 2_756 yes C(1) Ag(1) C(22) C(17) 46(2) 1_555 1_555 2_756 2_756 yes C(1) Ag(1) C(22) C(21) -79(1) 1_555 1_555 2_756 2_756 yes C(1) C(2) C(3) C(4) 0(2) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) -1(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) Ag(1) C(22) 71(2) 1_555 1_555 1_555 2_756 yes C(2) C(1) C(6) C(5) 0(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -1(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 0(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 1(2) 1_555 1_555 1_555 1_555 yes C(6) C(1) Ag(1) C(22) -48(2) 1_555 1_555 1_555 2_756 yes C(7) O(1) Ag(1) C(22) 27.0(7) 1_555 1_555 1_555 2_756 yes C(7) C(8) C(9) C(10) 1(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(13) C(14) -160.5(8) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(13) C(21) 77.8(10) 1_555 1_555 1_555 2_756 yes C(7) C(12) C(11) C(10) 1(1) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(11) 0(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 0(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(15) 177.2(8) 1_555 1_555 1_555 1_555 yes C(8) C(13) C(21) C(20) -165.8(8) 1_555 1_555 2_756 2_756 yes C(8) C(13) C(21) C(22) 13(1) 1_555 1_555 2_756 2_756 yes C(9) C(8) C(7) C(12) -1(1) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(14) 20(1) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(13) C(21) -101.4(9) 1_555 1_555 1_555 2_756 yes C(9) C(10) C(11) C(12) -1(1) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(15) C(16) -8(1) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(15) C(17) 114.0(9) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(13) -179.0(7) 1_555 1_555 1_555 1_555 yes C(10) C(15) C(17) C(18) 161.6(8) 1_555 1_555 1_555 1_555 yes C(10) C(15) C(17) C(22) -20(1) 1_555 1_555 1_555 1_555 yes C(11) O(2) Ag(1) C(22) -33.3(6) 1_555 1_555 2_756 1_555 yes C(11) C(10) C(15) C(16) 168.7(8) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(15) C(17) -68(1) 1_555 1_555 1_555 1_555 yes C(12) C(7) C(8) C(13) 179.5(8) 1_555 1_555 1_555 1_555 yes C(12) C(11) C(10) C(15) -179.2(8) 1_555 1_555 1_555 1_555 yes C(13) C(21) C(20) C(19) -180.0(8) 1_555 2_756 2_756 2_756 yes C(13) C(21) C(22) C(17) -179.4(8) 1_555 2_756 2_756 2_756 yes C(14) C(13) C(21) C(20) 70(1) 1_555 1_555 2_756 2_756 yes C(14) C(13) C(21) C(22) -109.9(9) 1_555 1_555 2_756 2_756 yes C(15) C(17) C(18) C(19) 178.7(8) 1_555 1_555 1_555 1_555 yes C(15) C(17) C(22) C(21) -178.7(8) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(17) C(18) -73(1) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(17) C(22) 104.4(9) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 0(1) 1_555 1_555 1_555 1_555 yes C(17) C(22) C(21) C(20) 0(1) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(22) C(21) 0(1) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) 0(1) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(17) C(22) 0(1) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) 0(1) 1_555 1_555 1_555 1_555 yes C(23) O(9) C(26) C(25) 3(2) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 8(4) 1_555 1_555 1_555 1_555 yes C(24) C(23) O(9) C(26) 1(2) 1_555 1_555 1_555 1_555 yes C(27) O(10) C(30) C(29) 21(2) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 7(3) 1_555 1_555 1_555 1_555 yes C(28) C(27) O(10) C(30) -15(3) 1_555 1_555 1_555 1_555 yes C(31) O(11) C(31) C(32) 0(1) 1_555 1_555 2_555 2_555 yes C(31) C(32) C(32) C(31) -3(4) 1_555 1_555 2_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 Ag(1) C(22) 2.528(8) 1_555 2_756 ? O(1) O(7) 2.92(1) 1_555 5_455 ? O(1) O(5) 3.20(2) 1_555 5_455 ? O(2) O(9) 2.592(9) 1_555 6_656 ? O(2) C(26) 3.49(2) 1_555 6_656 ? O(3) O(10) 2.63(1) 1_555 4_655 ? O(3) C(27) 3.31(2) 1_555 4_655 ? O(4) O(6) 2.92(2) 1_555 1_555 ? O(4) O(5) 3.19(2) 1_555 1_555 ? O(4) C(27) 3.52(2) 1_555 1_655 ? O(5) C(19) 3.46(2) 1_555 1_555 ? O(7) C(12) 3.46(1) 1_555 5_545 ? O(7) C(23) 3.58(2) 1_555 1_655 ? O(8) C(25) 3.59(3) 1_555 4_655 ? O(9) C(11) 3.44(1) 1_555 6_646 ? O(9) C(12) 3.53(1) 1_555 6_646 ? O(10) C(18) 3.53(1) 1_555 4_454 ? O(10) C(19) 3.57(1) 1_555 4_454 ? C(5) C(6) 3.58(2) 1_555 7_656 ? C(12) C(16) 3.58(1) 1_555 3_757 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #=END data_[Ag(calix[6]arene)(C6H6)2] #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 28 09:56:17 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _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' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1000.29 _chemical_formula_analytical ? _chemical_formula_sum 'C54 H48 Ag Cl O10 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 21.164(2) _cell_length_b 11.606(2) _cell_length_c 10.146(1) _cell_angle_alpha 71.62(1) _cell_angle_beta 80.302(10) _cell_angle_gamma 79.11(1) _cell_volume 2306.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 6.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032.00 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.972 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.18 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 2 0 1 2 -1 4 2 1 _diffrn_reflns_number 11108 _reflns_number_total 10584 _reflns_number_gt 6731 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_av_sigmaI/netI 0.044 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04139 _diffrn_orient_matrix_UB_12 -0.00320 _diffrn_orient_matrix_UB_13 -0.06385 _diffrn_orient_matrix_UB_21 -0.02518 _diffrn_orient_matrix_UB_22 0.01919 _diffrn_orient_matrix_UB_23 -0.08121 _diffrn_orient_matrix_UB_31 -0.00033 _diffrn_orient_matrix_UB_32 0.08968 _diffrn_orient_matrix_UB_33 -0.01623 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;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) ; '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) ; #------------------------------------------------------------------------------ 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 Ag(1) Ag 0.04444(2) 0.63072(3) -0.59720(4) 0.0839(1) Uani 1.00 d ... Cl(1) Cl 0.07139(5) 0.35970(10) -0.6950(1) 0.0704(3) Uani 1.00 d ... O(1) O 0.2303(1) 0.3142(2) -0.4822(3) 0.0578(7) Uani 1.00 d ... O(2) O 0.3394(1) 0.2836(2) -0.6568(2) 0.0506(7) Uani 1.00 d ... O(3) O 0.3795(1) 0.1207(2) -0.4264(3) 0.0547(7) Uani 1.00 d ... O(4) O 0.3153(1) -0.0670(2) -0.3099(3) 0.0548(7) Uani 1.00 d ... O(5) O 0.2142(1) -0.0835(2) -0.4267(2) 0.0563(7) Uani 1.00 d ... O(6) O 0.1640(1) 0.1274(2) -0.3741(3) 0.0666(8) Uani 1.00 d ... O(7) O 0.0475(2) 0.4201(3) -0.5855(4) 0.093(1) Uani 1.00 d ... O(8) O 0.0446(3) 0.4300(5) -0.8178(5) 0.137(2) Uani 1.00 d ... O(9) O 0.1365(2) 0.3323(7) -0.7063(7) 0.181(3) Uani 1.00 d ... O(10) O 0.0451(3) 0.2484(4) -0.6503(5) 0.126(2) Uani 1.00 d ... C(1) C 0.2099(2) 0.5298(3) -0.5904(4) 0.055(1) Uani 1.00 d ... C(2) C 0.2611(2) 0.5200(3) -0.7095(4) 0.060(1) Uani 1.00 d ... C(3) C 0.3307(2) 0.4959(3) -0.6733(3) 0.0502(9) Uani 1.00 d ... C(4) C 0.3592(2) 0.5902(3) -0.6610(4) 0.060(1) Uani 1.00 d ... C(5) C 0.4234(2) 0.5716(3) -0.6398(4) 0.063(1) Uani 1.00 d ... C(6) C 0.4602(2) 0.4590(3) -0.6314(4) 0.056(1) Uani 1.00 d ... C(7) C 0.4342(2) 0.3601(3) -0.6387(3) 0.0465(9) Uani 1.00 d ... C(8) C 0.4756(2) 0.2378(3) -0.6283(4) 0.0526(10) Uani 1.00 d ... C(9) C 0.4884(2) 0.1610(3) -0.4824(4) 0.0468(9) Uani 1.00 d ... C(10) C 0.5498(2) 0.1423(3) -0.4385(4) 0.059(1) Uani 1.00 d ... C(11) C 0.5611(2) 0.0729(4) -0.3048(5) 0.065(1) Uani 1.00 d ... C(12) C 0.5116(2) 0.0229(3) -0.2108(4) 0.059(1) Uani 1.00 d ... C(13) C 0.4496(2) 0.0384(3) -0.2482(4) 0.0464(9) Uani 1.00 d ... C(14) C 0.3946(2) -0.0108(3) -0.1422(4) 0.0512(9) Uani 1.00 d ... C(15) C 0.3850(2) -0.1408(3) -0.1308(3) 0.0458(8) Uani 1.00 d ... C(16) C 0.4157(2) -0.2406(3) -0.0337(4) 0.057(1) Uani 1.00 d ... C(17) C 0.4070(2) -0.3593(3) -0.0202(4) 0.066(1) Uani 1.00 d ... C(18) C 0.3668(2) -0.3790(3) -0.1019(4) 0.062(1) Uani 1.00 d ... C(19) C 0.3349(2) -0.2830(3) -0.1994(4) 0.0491(9) Uani 1.00 d ... C(20) C 0.2907(2) -0.3054(3) -0.2873(4) 0.056(1) Uani 1.00 d ... C(21) C 0.2187(2) -0.2737(3) -0.2437(4) 0.0511(10) Uani 1.00 d ... C(22) C 0.1867(2) -0.3518(3) -0.1310(4) 0.059(1) Uani 1.00 d ... C(23) C 0.1208(2) -0.3268(4) -0.0947(4) 0.065(1) Uani 1.00 d ... C(24) C 0.0857(2) -0.2218(4) -0.1723(4) 0.063(1) Uani 1.00 d ... C(25) C 0.1155(2) -0.1393(3) -0.2847(4) 0.0521(10) Uani 1.00 d ... C(26) C 0.0753(2) -0.0283(4) -0.3739(4) 0.059(1) Uani 1.00 d ... C(27) C 0.0568(2) 0.0791(3) -0.3132(4) 0.0559(10) Uani 1.00 d ... C(28) C -0.0055(2) 0.1055(4) -0.2529(4) 0.065(1) Uani 1.00 d ... C(29) C -0.0234(2) 0.2011(4) -0.1937(5) 0.070(1) Uani 1.00 d ... C(30) C 0.0234(2) 0.2705(4) -0.1923(4) 0.066(1) Uani 1.00 d ... C(31) C 0.0869(2) 0.2473(3) -0.2541(4) 0.056(1) Uani 1.00 d ... C(32) C 0.1385(2) 0.3193(4) -0.2441(4) 0.061(1) Uani 1.00 d ... C(33) C 0.1497(2) 0.4316(3) -0.3669(4) 0.054(1) Uani 1.00 d ... C(34) C 0.1149(2) 0.5457(4) -0.3652(5) 0.065(1) Uani 1.00 d ... C(35) C 0.1270(2) 0.6504(4) -0.4734(5) 0.072(1) Uani 1.00 d ... C(36) C 0.1740(2) 0.6418(3) -0.5848(5) 0.066(1) Uani 1.00 d ... C(37) C 0.1962(2) 0.4253(3) -0.4799(4) 0.0512(10) Uani 1.00 d ... C(38) C 0.1020(2) 0.1519(3) -0.3136(4) 0.0534(10) Uani 1.00 d ... C(39) C 0.1828(2) -0.1653(3) -0.3174(4) 0.0495(9) Uani 1.00 d ... C(40) C 0.3453(2) -0.1640(3) -0.2124(3) 0.0446(8) Uani 1.00 d ... C(41) C 0.4398(2) 0.1057(3) -0.3848(3) 0.0436(8) Uani 1.00 d ... C(42) C 0.3682(2) 0.3806(3) -0.6559(3) 0.0462(9) Uani 1.00 d ... C(43) C 0.2435(4) -0.0340(9) -0.8004(8) 0.122(3) Uani 1.00 d ... C(44) C 0.1920(4) 0.0558(7) -0.7964(7) 0.109(2) Uani 1.00 d ... C(45) C 0.1456(3) 0.0777(6) -0.8762(7) 0.102(2) Uani 1.00 d ... C(46) C 0.1477(4) 0.0135(8) -0.9652(7) 0.111(2) Uani 1.00 d ... C(47) C 0.1991(6) -0.0796(7) -0.9753(7) 0.129(3) Uani 1.00 d ... C(48) C 0.2488(4) -0.1006(6) -0.8904(10) 0.130(3) Uani 1.00 d ... C(49) C 0.4195(3) 0.3132(5) -0.1335(6) 0.089(2) Uani 1.00 d ... C(50) C 0.3819(3) 0.3439(4) -0.2447(5) 0.089(2) Uani 1.00 d ... C(51) C 0.3160(4) 0.3392(5) -0.2134(6) 0.096(2) Uani 1.00 d ... C(52) C 0.2895(3) 0.3011(6) -0.0773(7) 0.107(2) Uani 1.00 d ... C(53) C 0.3287(4) 0.2702(5) 0.0280(6) 0.098(2) Uani 1.00 d ... C(54) C 0.3917(3) 0.2770(4) -0.0011(6) 0.084(2) Uani 1.00 d ... H(1) H 0.2560 0.5952 -0.7823 0.0714 Uiso 1.00 calc ... H(2) H 0.2549 0.4550 -0.7413 0.0714 Uiso 1.00 calc ... H(3) H 0.3342 0.6683 -0.6682 0.0712 Uiso 1.00 calc ... H(4) H 0.4420 0.6362 -0.6304 0.0745 Uiso 1.00 calc ... H(5) H 0.5049 0.4486 -0.6214 0.0670 Uiso 1.00 calc ... H(6) H 0.5161 0.2517 -0.6825 0.0633 Uiso 1.00 calc ... H(7) H 0.4545 0.1921 -0.6665 0.0633 Uiso 1.00 calc ... H(8) H 0.5841 0.1781 -0.5026 0.0701 Uiso 1.00 calc ... H(9) H 0.6033 0.0596 -0.2779 0.0780 Uiso 1.00 calc ... H(10) H 0.5199 -0.0230 -0.1186 0.0704 Uiso 1.00 calc ... H(11) H 0.4027 -0.0107 -0.0532 0.0621 Uiso 1.00 calc ... H(12) H 0.3557 0.0420 -0.1669 0.0621 Uiso 1.00 calc ... H(13) H 0.4429 -0.2270 0.0231 0.0689 Uiso 1.00 calc ... H(14) H 0.4285 -0.4260 0.0456 0.0783 Uiso 1.00 calc ... H(15) H 0.3609 -0.4604 -0.0912 0.0749 Uiso 1.00 calc ... H(16) H 0.2991 -0.3900 -0.2819 0.0668 Uiso 1.00 calc ... H(17) H 0.3005 -0.2577 -0.3811 0.0668 Uiso 1.00 calc ... H(18) H 0.2102 -0.4242 -0.0772 0.0720 Uiso 1.00 calc ... H(19) H 0.0999 -0.3818 -0.0170 0.0787 Uiso 1.00 calc ... H(20) H 0.0403 -0.2055 -0.1476 0.0751 Uiso 1.00 calc ... H(21) H 0.0367 -0.0524 -0.3852 0.0722 Uiso 1.00 calc ... H(22) H 0.0997 -0.0007 -0.4627 0.0722 Uiso 1.00 calc ... H(23) H -0.0371 0.0562 -0.2516 0.0784 Uiso 1.00 calc ... H(24) H -0.0663 0.2180 -0.1539 0.0841 Uiso 1.00 calc ... H(25) H 0.0117 0.3350 -0.1499 0.0787 Uiso 1.00 calc ... H(26) H 0.1257 0.3461 -0.1626 0.0737 Uiso 1.00 calc ... H(27) H 0.1781 0.2658 -0.2350 0.0737 Uiso 1.00 calc ... H(28) H 0.0828 0.5521 -0.2896 0.0780 Uiso 1.00 calc ... H(29) H 0.1029 0.7275 -0.4709 0.0868 Uiso 1.00 calc ... H(30) H 0.1820 0.7141 -0.6578 0.0787 Uiso 1.00 calc ... H(31) H 0.2542 0.2367 -0.4839 0.0691 Uiso 1.00 calc ... H(32) H 0.3193 0.2170 -0.6564 0.0610 Uiso 1.00 calc ... H(33) H 0.3379 0.1308 -0.4550 0.0660 Uiso 1.00 calc ... H(34) H 0.2945 -0.0003 -0.3776 0.0663 Uiso 1.00 calc ... H(35) H 0.2358 -0.0273 -0.5020 0.0680 Uiso 1.00 calc ... H(36) H 0.2070 0.1104 -0.4161 0.0796 Uiso 1.00 calc ... 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 Ag(1) 0.0701(2) 0.0748(2) 0.1087(3) 0.0115(2) -0.0336(2) -0.0303(2) Cl(1) 0.0642(6) 0.0679(6) 0.0861(7) 0.0026(5) -0.0107(5) -0.0386(5) O(1) 0.047(1) 0.044(1) 0.078(2) 0.003(1) -0.004(1) -0.020(1) O(2) 0.054(1) 0.045(1) 0.058(1) -0.013(1) -0.006(1) -0.019(1) O(3) 0.040(1) 0.058(1) 0.062(1) -0.010(1) -0.013(1) -0.006(1) O(4) 0.054(1) 0.039(1) 0.065(2) -0.005(1) -0.021(1) -0.001(1) O(5) 0.052(1) 0.061(1) 0.051(1) -0.014(1) 0.000(1) -0.008(1) O(6) 0.038(1) 0.061(2) 0.092(2) -0.004(1) 0.011(1) -0.022(1) O(7) 0.093(2) 0.089(2) 0.113(3) -0.012(2) 0.001(2) -0.062(2) O(8) 0.158(4) 0.141(4) 0.089(3) 0.008(3) -0.008(3) -0.022(3) O(9) 0.065(3) 0.294(8) 0.264(7) -0.003(3) -0.009(3) -0.210(7) O(10) 0.171(4) 0.091(3) 0.131(3) -0.040(3) -0.001(3) -0.052(3) C(1) 0.051(2) 0.048(2) 0.070(2) -0.001(1) -0.023(2) -0.018(2) C(2) 0.061(2) 0.051(2) 0.061(2) -0.002(2) -0.021(2) -0.004(2) C(3) 0.056(2) 0.045(2) 0.044(2) -0.007(1) -0.008(1) -0.004(1) C(4) 0.070(2) 0.043(2) 0.063(2) -0.008(2) -0.012(2) -0.008(2) C(5) 0.073(3) 0.050(2) 0.070(2) -0.023(2) -0.014(2) -0.014(2) C(6) 0.053(2) 0.058(2) 0.056(2) -0.017(2) -0.006(2) -0.011(2) C(7) 0.048(2) 0.050(2) 0.039(2) -0.011(1) 0.004(1) -0.011(1) C(8) 0.045(2) 0.057(2) 0.056(2) -0.008(2) 0.009(2) -0.025(2) C(9) 0.041(2) 0.043(2) 0.058(2) -0.002(1) 0.002(1) -0.023(1) C(10) 0.043(2) 0.054(2) 0.081(3) -0.008(2) -0.003(2) -0.026(2) C(11) 0.040(2) 0.064(2) 0.095(3) -0.005(2) -0.017(2) -0.028(2) C(12) 0.059(2) 0.051(2) 0.074(2) 0.001(2) -0.025(2) -0.023(2) C(13) 0.047(2) 0.038(2) 0.059(2) -0.004(1) -0.008(1) -0.022(1) C(14) 0.057(2) 0.050(2) 0.048(2) -0.002(1) -0.008(2) -0.019(1) C(15) 0.045(2) 0.046(2) 0.042(2) -0.003(1) 0.000(1) -0.011(1) C(16) 0.055(2) 0.062(2) 0.049(2) -0.008(2) -0.010(2) -0.006(2) C(17) 0.067(2) 0.051(2) 0.061(2) 0.002(2) -0.014(2) 0.006(2) C(18) 0.064(2) 0.039(2) 0.071(2) 0.000(2) -0.001(2) -0.006(2) C(19) 0.045(2) 0.044(2) 0.054(2) -0.001(1) 0.003(1) -0.016(1) C(20) 0.058(2) 0.043(2) 0.067(2) -0.005(1) -0.003(2) -0.022(2) C(21) 0.053(2) 0.047(2) 0.058(2) -0.008(1) -0.007(2) -0.022(2) C(22) 0.067(2) 0.052(2) 0.061(2) -0.011(2) -0.008(2) -0.017(2) C(23) 0.069(3) 0.063(2) 0.062(2) -0.021(2) 0.006(2) -0.014(2) C(24) 0.055(2) 0.069(2) 0.070(2) -0.015(2) 0.001(2) -0.029(2) C(25) 0.048(2) 0.057(2) 0.059(2) -0.014(2) -0.004(2) -0.023(2) C(26) 0.048(2) 0.069(2) 0.065(2) -0.011(2) -0.014(2) -0.020(2) C(27) 0.041(2) 0.061(2) 0.058(2) -0.006(2) -0.008(2) -0.007(2) C(28) 0.044(2) 0.074(3) 0.072(3) -0.008(2) -0.005(2) -0.016(2) C(29) 0.041(2) 0.077(3) 0.080(3) -0.002(2) 0.006(2) -0.017(2) C(30) 0.050(2) 0.073(3) 0.068(2) 0.001(2) 0.000(2) -0.021(2) C(31) 0.043(2) 0.058(2) 0.061(2) 0.000(2) -0.005(2) -0.012(2) C(32) 0.048(2) 0.076(3) 0.063(2) -0.005(2) -0.005(2) -0.029(2) C(33) 0.045(2) 0.056(2) 0.071(2) -0.003(2) -0.013(2) -0.029(2) C(34) 0.052(2) 0.070(3) 0.091(3) -0.001(2) -0.018(2) -0.048(2) C(35) 0.064(3) 0.057(2) 0.110(4) 0.003(2) -0.029(2) -0.041(2) C(36) 0.062(2) 0.045(2) 0.092(3) -0.003(2) -0.027(2) -0.016(2) C(37) 0.042(2) 0.050(2) 0.067(2) 0.000(1) -0.017(2) -0.022(2) C(38) 0.039(2) 0.056(2) 0.059(2) 0.000(1) -0.006(1) -0.012(2) C(39) 0.051(2) 0.052(2) 0.052(2) -0.011(1) -0.008(1) -0.021(2) C(40) 0.041(2) 0.040(2) 0.046(2) 0.001(1) -0.002(1) -0.008(1) C(41) 0.040(2) 0.039(2) 0.056(2) -0.004(1) -0.006(1) -0.019(1) C(42) 0.054(2) 0.047(2) 0.035(2) -0.012(1) -0.001(1) -0.009(1) C(43) 0.088(4) 0.153(7) 0.102(5) -0.028(5) -0.005(4) -0.004(5) C(44) 0.119(5) 0.120(5) 0.100(4) -0.045(4) 0.009(4) -0.043(4) C(45) 0.096(4) 0.086(4) 0.102(4) -0.014(3) 0.015(4) -0.010(3) C(46) 0.118(5) 0.130(6) 0.077(4) -0.043(5) -0.020(3) 0.000(4) C(47) 0.215(10) 0.100(5) 0.064(3) -0.051(6) 0.046(5) -0.027(3) C(48) 0.112(5) 0.093(4) 0.112(6) 0.016(4) 0.057(5) 0.017(4) C(49) 0.084(3) 0.073(3) 0.109(4) 0.019(2) -0.022(3) -0.037(3) C(50) 0.149(5) 0.054(2) 0.065(3) -0.014(3) 0.005(3) -0.027(2) C(51) 0.131(5) 0.086(3) 0.086(4) -0.019(3) -0.048(4) -0.027(3) C(52) 0.103(4) 0.119(5) 0.116(5) -0.037(4) -0.024(4) -0.043(4) C(53) 0.151(6) 0.080(3) 0.074(3) -0.041(4) -0.009(3) -0.026(3) C(54) 0.104(4) 0.063(3) 0.079(3) -0.006(3) -0.032(3) -0.007(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _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) + 0.00090|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6731 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.812 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.56 _refine_diff_density_max 0.57 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Ag(1) O(7) 2.399(3) 1_555 1_555 yes Ag(1) O(7) 2.469(4) 1_555 2_564 yes Ag(1) C(29) 2.427(4) 1_555 2_564 yes Ag(1) C(35) 2.399(4) 1_555 1_555 yes Cl(1) O(7) 1.466(3) 1_555 1_555 yes Cl(1) O(8) 1.400(5) 1_555 1_555 yes Cl(1) O(9) 1.347(4) 1_555 1_555 yes Cl(1) O(10) 1.414(4) 1_555 1_555 yes O(1) C(37) 1.358(4) 1_555 1_555 yes O(2) C(42) 1.380(4) 1_555 1_555 yes O(3) C(41) 1.373(4) 1_555 1_555 yes O(4) C(40) 1.374(4) 1_555 1_555 yes O(5) C(39) 1.378(4) 1_555 1_555 yes O(6) C(38) 1.370(4) 1_555 1_555 yes C(1) C(2) 1.500(6) 1_555 1_555 yes C(1) C(36) 1.388(5) 1_555 1_555 yes C(1) C(37) 1.406(5) 1_555 1_555 yes C(2) C(3) 1.530(5) 1_555 1_555 yes C(3) C(4) 1.393(5) 1_555 1_555 yes C(3) C(42) 1.397(5) 1_555 1_555 yes C(4) C(5) 1.377(6) 1_555 1_555 yes C(5) C(6) 1.375(6) 1_555 1_555 yes C(6) C(7) 1.389(5) 1_555 1_555 yes C(7) C(8) 1.503(5) 1_555 1_555 yes C(7) C(42) 1.404(5) 1_555 1_555 yes C(8) C(9) 1.507(5) 1_555 1_555 yes C(9) C(10) 1.401(5) 1_555 1_555 yes C(9) C(41) 1.399(5) 1_555 1_555 yes C(10) C(11) 1.376(6) 1_555 1_555 yes C(11) C(12) 1.374(6) 1_555 1_555 yes C(12) C(13) 1.390(5) 1_555 1_555 yes C(13) C(14) 1.510(5) 1_555 1_555 yes C(13) C(41) 1.388(5) 1_555 1_555 yes C(14) C(15) 1.525(5) 1_555 1_555 yes C(15) C(16) 1.395(5) 1_555 1_555 yes C(15) C(40) 1.388(5) 1_555 1_555 yes C(16) C(17) 1.385(6) 1_555 1_555 yes C(17) C(18) 1.376(6) 1_555 1_555 yes C(18) C(19) 1.386(5) 1_555 1_555 yes C(19) C(20) 1.504(5) 1_555 1_555 yes C(19) C(40) 1.401(5) 1_555 1_555 yes C(20) C(21) 1.521(5) 1_555 1_555 yes C(21) C(22) 1.381(5) 1_555 1_555 yes C(21) C(39) 1.400(5) 1_555 1_555 yes C(22) C(23) 1.380(6) 1_555 1_555 yes C(23) C(24) 1.381(6) 1_555 1_555 yes C(24) C(25) 1.383(6) 1_555 1_555 yes C(25) C(26) 1.520(5) 1_555 1_555 yes C(25) C(39) 1.403(5) 1_555 1_555 yes C(26) C(27) 1.519(6) 1_555 1_555 yes C(27) C(28) 1.379(5) 1_555 1_555 yes C(27) C(38) 1.389(5) 1_555 1_555 yes C(28) C(29) 1.386(6) 1_555 1_555 yes C(29) C(30) 1.393(6) 1_555 1_555 yes C(30) C(31) 1.399(5) 1_555 1_555 yes C(31) C(32) 1.528(5) 1_555 1_555 yes C(31) C(38) 1.383(5) 1_555 1_555 yes C(32) C(33) 1.518(6) 1_555 1_555 yes C(33) C(34) 1.392(5) 1_555 1_555 yes C(33) C(37) 1.390(5) 1_555 1_555 yes C(34) C(35) 1.389(6) 1_555 1_555 yes C(35) C(36) 1.390(7) 1_555 1_555 yes C(43) C(44) 1.36(1) 1_555 1_555 yes C(43) C(48) 1.35(1) 1_555 1_555 yes C(44) C(45) 1.315(10) 1_555 1_555 yes C(45) C(46) 1.331(10) 1_555 1_555 yes C(46) C(47) 1.40(1) 1_555 1_555 yes C(47) C(48) 1.41(1) 1_555 1_555 yes C(49) C(50) 1.406(8) 1_555 1_555 yes C(49) C(54) 1.341(8) 1_555 1_555 yes C(50) C(51) 1.383(9) 1_555 1_555 yes C(51) C(52) 1.365(9) 1_555 1_555 yes C(52) C(53) 1.379(9) 1_555 1_555 yes C(53) C(54) 1.329(8) 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 O(7) Ag(1) O(7) 80.7(1) 1_555 1_555 2_564 yes O(7) Ag(1) C(29) 122.7(1) 1_555 1_555 2_564 yes O(7) Ag(1) C(35) 110.5(1) 1_555 1_555 1_555 yes O(7) Ag(1) C(29) 117.8(1) 2_564 1_555 2_564 yes O(7) Ag(1) C(35) 104.2(2) 2_564 1_555 1_555 yes C(29) Ag(1) C(35) 115.1(2) 2_564 1_555 1_555 yes O(7) Cl(1) O(8) 109.0(3) 1_555 1_555 1_555 yes O(7) Cl(1) O(9) 110.9(3) 1_555 1_555 1_555 yes O(7) Cl(1) O(10) 105.8(2) 1_555 1_555 1_555 yes O(8) Cl(1) O(9) 116.2(4) 1_555 1_555 1_555 yes O(8) Cl(1) O(10) 106.3(3) 1_555 1_555 1_555 yes O(9) Cl(1) O(10) 108.1(4) 1_555 1_555 1_555 yes C(37) O(1) H(31) 179.8(3) 1_555 1_555 1_555 no C(42) O(2) H(32) 179.4(3) 1_555 1_555 1_555 no C(41) O(3) H(33) 179.9(3) 1_555 1_555 1_555 no C(40) O(4) H(34) 179.6(3) 1_555 1_555 1_555 no C(39) O(5) H(35) 179.9(3) 1_555 1_555 1_555 no C(38) O(6) H(36) 180.0(3) 1_555 1_555 1_555 no Ag(1) O(7) Ag(1) 99.3(1) 1_555 1_555 2_564 yes Ag(1) O(7) Cl(1) 128.7(2) 1_555 1_555 1_555 yes Ag(1) O(7) Cl(1) 125.7(2) 2_564 1_555 1_555 yes C(2) C(1) C(36) 121.5(4) 1_555 1_555 1_555 yes C(2) C(1) C(37) 121.1(3) 1_555 1_555 1_555 yes C(36) C(1) C(37) 117.4(4) 1_555 1_555 1_555 yes C(1) C(2) C(3) 114.6(3) 1_555 1_555 1_555 yes C(1) C(2) H(1) 107.9(3) 1_555 1_555 1_555 no C(1) C(2) H(2) 108.4(4) 1_555 1_555 1_555 no C(3) C(2) H(1) 108.0(3) 1_555 1_555 1_555 no C(3) C(2) H(2) 108.1(3) 1_555 1_555 1_555 no H(1) C(2) H(2) 109.7(4) 1_555 1_555 1_555 no C(2) C(3) C(4) 120.6(3) 1_555 1_555 1_555 yes C(2) C(3) C(42) 121.5(3) 1_555 1_555 1_555 yes C(4) C(3) C(42) 117.8(3) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.9(3) 1_555 1_555 1_555 yes C(3) C(4) H(3) 119.4(4) 1_555 1_555 1_555 no C(5) C(4) H(3) 119.7(4) 1_555 1_555 1_555 no C(4) C(5) C(6) 119.9(3) 1_555 1_555 1_555 yes C(4) C(5) H(4) 119.9(4) 1_555 1_555 1_555 no C(6) C(5) H(4) 120.2(4) 1_555 1_555 1_555 no C(5) C(6) C(7) 122.1(3) 1_555 1_555 1_555 yes C(5) C(6) H(5) 119.0(4) 1_555 1_555 1_555 no C(7) C(6) H(5) 118.9(4) 1_555 1_555 1_555 no C(6) C(7) C(8) 120.9(3) 1_555 1_555 1_555 yes C(6) C(7) C(42) 116.7(3) 1_555 1_555 1_555 yes C(8) C(7) C(42) 122.4(3) 1_555 1_555 1_555 yes C(7) C(8) C(9) 115.3(3) 1_555 1_555 1_555 yes C(7) C(8) H(6) 108.2(3) 1_555 1_555 1_555 no C(7) C(8) H(7) 108.1(3) 1_555 1_555 1_555 no C(9) C(8) H(6) 108.0(3) 1_555 1_555 1_555 no C(9) C(8) H(7) 107.8(3) 1_555 1_555 1_555 no H(6) C(8) H(7) 109.3(3) 1_555 1_555 1_555 no C(8) C(9) C(10) 121.2(3) 1_555 1_555 1_555 yes C(8) C(9) C(41) 121.8(3) 1_555 1_555 1_555 yes C(10) C(9) C(41) 117.0(3) 1_555 1_555 1_555 yes C(9) C(10) C(11) 120.9(3) 1_555 1_555 1_555 yes C(9) C(10) H(8) 119.1(4) 1_555 1_555 1_555 no C(11) C(10) H(8) 119.9(4) 1_555 1_555 1_555 no C(10) C(11) C(12) 120.3(3) 1_555 1_555 1_555 yes C(10) C(11) H(9) 119.6(4) 1_555 1_555 1_555 no C(12) C(11) H(9) 120.1(4) 1_555 1_555 1_555 no C(11) C(12) C(13) 121.4(4) 1_555 1_555 1_555 yes C(11) C(12) H(10) 119.2(4) 1_555 1_555 1_555 no C(13) C(12) H(10) 119.3(4) 1_555 1_555 1_555 no C(12) C(13) C(14) 121.1(3) 1_555 1_555 1_555 yes C(12) C(13) C(41) 117.3(3) 1_555 1_555 1_555 yes C(14) C(13) C(41) 121.5(3) 1_555 1_555 1_555 yes C(13) C(14) C(15) 115.3(3) 1_555 1_555 1_555 yes C(13) C(14) H(11) 108.0(3) 1_555 1_555 1_555 no C(13) C(14) H(12) 108.1(3) 1_555 1_555 1_555 no C(15) C(14) H(11) 107.7(3) 1_555 1_555 1_555 no C(15) C(14) H(12) 107.8(3) 1_555 1_555 1_555 no H(11) C(14) H(12) 109.9(3) 1_555 1_555 1_555 no C(14) C(15) C(16) 119.8(3) 1_555 1_555 1_555 yes C(14) C(15) C(40) 122.2(3) 1_555 1_555 1_555 yes C(16) C(15) C(40) 118.0(3) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120.8(3) 1_555 1_555 1_555 yes C(15) C(16) H(13) 119.5(4) 1_555 1_555 1_555 no C(17) C(16) H(13) 119.7(4) 1_555 1_555 1_555 no C(16) C(17) C(18) 119.7(3) 1_555 1_555 1_555 yes C(16) C(17) H(14) 119.7(4) 1_555 1_555 1_555 no C(18) C(17) H(14) 120.7(4) 1_555 1_555 1_555 no C(17) C(18) C(19) 121.8(3) 1_555 1_555 1_555 yes C(17) C(18) H(15) 119.0(4) 1_555 1_555 1_555 no C(19) C(18) H(15) 119.3(4) 1_555 1_555 1_555 no C(18) C(19) C(20) 121.3(3) 1_555 1_555 1_555 yes C(18) C(19) C(40) 117.4(3) 1_555 1_555 1_555 yes C(20) C(19) C(40) 121.2(3) 1_555 1_555 1_555 yes C(19) C(20) C(21) 115.0(3) 1_555 1_555 1_555 yes C(19) C(20) H(16) 108.0(3) 1_555 1_555 1_555 no C(19) C(20) H(17) 108.0(3) 1_555 1_555 1_555 no C(21) C(20) H(16) 108.0(3) 1_555 1_555 1_555 no C(21) C(20) H(17) 108.2(3) 1_555 1_555 1_555 no H(16) C(20) H(17) 109.5(4) 1_555 1_555 1_555 no C(20) C(21) C(22) 121.0(3) 1_555 1_555 1_555 yes C(20) C(21) C(39) 121.2(3) 1_555 1_555 1_555 yes C(22) C(21) C(39) 117.9(3) 1_555 1_555 1_555 yes C(21) C(22) C(23) 121.4(4) 1_555 1_555 1_555 yes C(21) C(22) H(18) 119.6(4) 1_555 1_555 1_555 no C(23) C(22) H(18) 119.0(4) 1_555 1_555 1_555 no C(22) C(23) C(24) 119.8(4) 1_555 1_555 1_555 yes C(22) C(23) H(19) 119.9(4) 1_555 1_555 1_555 no C(24) C(23) H(19) 120.3(4) 1_555 1_555 1_555 no C(23) C(24) C(25) 121.2(4) 1_555 1_555 1_555 yes C(23) C(24) H(20) 119.5(4) 1_555 1_555 1_555 no C(25) C(24) H(20) 119.3(4) 1_555 1_555 1_555 no C(24) C(25) C(26) 120.3(3) 1_555 1_555 1_555 yes C(24) C(25) C(39) 117.9(3) 1_555 1_555 1_555 yes C(26) C(25) C(39) 121.7(3) 1_555 1_555 1_555 yes C(25) C(26) C(27) 114.3(3) 1_555 1_555 1_555 yes C(25) C(26) H(21) 108.6(3) 1_555 1_555 1_555 no C(25) C(26) H(22) 108.4(3) 1_555 1_555 1_555 no C(27) C(26) H(21) 108.1(3) 1_555 1_555 1_555 no C(27) C(26) H(22) 107.7(3) 1_555 1_555 1_555 no H(21) C(26) H(22) 109.6(4) 1_555 1_555 1_555 no C(26) C(27) C(28) 120.5(3) 1_555 1_555 1_555 yes C(26) C(27) C(38) 121.4(3) 1_555 1_555 1_555 yes C(28) C(27) C(38) 118.0(4) 1_555 1_555 1_555 yes C(27) C(28) C(29) 121.8(4) 1_555 1_555 1_555 yes C(27) C(28) H(23) 119.1(4) 1_555 1_555 1_555 no C(29) C(28) H(23) 119.2(4) 1_555 1_555 1_555 no Ag(1) C(29) C(28) 99.3(3) 2_564 1_555 1_555 yes Ag(1) C(29) C(30) 81.3(3) 2_564 1_555 1_555 yes Ag(1) C(29) H(24) 90.2(3) 2_564 1_555 1_555 no C(28) C(29) C(30) 119.0(3) 1_555 1_555 1_555 yes C(28) C(29) H(24) 120.4(4) 1_555 1_555 1_555 no C(30) C(29) H(24) 120.6(5) 1_555 1_555 1_555 no C(29) C(30) C(31) 120.7(4) 1_555 1_555 1_555 yes C(29) C(30) H(25) 119.4(4) 1_555 1_555 1_555 no C(31) C(30) H(25) 119.9(4) 1_555 1_555 1_555 no C(30) C(31) C(32) 120.0(4) 1_555 1_555 1_555 yes C(30) C(31) C(38) 118.0(4) 1_555 1_555 1_555 yes C(32) C(31) C(38) 121.8(3) 1_555 1_555 1_555 yes C(31) C(32) C(33) 116.0(3) 1_555 1_555 1_555 yes C(31) C(32) H(26) 107.8(3) 1_555 1_555 1_555 no C(31) C(32) H(27) 108.1(4) 1_555 1_555 1_555 no C(33) C(32) H(26) 107.4(4) 1_555 1_555 1_555 no C(33) C(32) H(27) 107.7(3) 1_555 1_555 1_555 no H(26) C(32) H(27) 109.7(4) 1_555 1_555 1_555 no C(32) C(33) C(34) 119.8(4) 1_555 1_555 1_555 yes C(32) C(33) C(37) 121.8(3) 1_555 1_555 1_555 yes C(34) C(33) C(37) 118.4(4) 1_555 1_555 1_555 yes C(33) C(34) C(35) 120.5(4) 1_555 1_555 1_555 yes C(33) C(34) H(28) 119.8(5) 1_555 1_555 1_555 no C(35) C(34) H(28) 119.7(4) 1_555 1_555 1_555 no Ag(1) C(35) C(34) 91.8(3) 1_555 1_555 1_555 yes Ag(1) C(35) C(36) 91.1(3) 1_555 1_555 1_555 yes Ag(1) C(35) H(29) 86.9(3) 1_555 1_555 1_555 no C(34) C(35) C(36) 120.0(4) 1_555 1_555 1_555 yes C(34) C(35) H(29) 119.6(5) 1_555 1_555 1_555 no C(36) C(35) H(29) 120.4(5) 1_555 1_555 1_555 no C(1) C(36) C(35) 121.2(4) 1_555 1_555 1_555 yes C(1) C(36) H(30) 119.6(5) 1_555 1_555 1_555 no C(35) C(36) H(30) 119.2(4) 1_555 1_555 1_555 no O(1) C(37) C(1) 118.9(3) 1_555 1_555 1_555 yes O(1) C(37) C(33) 118.6(3) 1_555 1_555 1_555 yes C(1) C(37) C(33) 122.4(3) 1_555 1_555 1_555 yes O(6) C(38) C(27) 118.6(3) 1_555 1_555 1_555 yes O(6) C(38) C(31) 118.9(3) 1_555 1_555 1_555 yes C(27) C(38) C(31) 122.4(3) 1_555 1_555 1_555 yes O(5) C(39) C(21) 118.9(3) 1_555 1_555 1_555 yes O(5) C(39) C(25) 119.4(3) 1_555 1_555 1_555 yes C(21) C(39) C(25) 121.7(3) 1_555 1_555 1_555 yes O(4) C(40) C(15) 118.9(3) 1_555 1_555 1_555 yes O(4) C(40) C(19) 118.8(3) 1_555 1_555 1_555 yes C(15) C(40) C(19) 122.3(3) 1_555 1_555 1_555 yes O(3) C(41) C(9) 118.0(3) 1_555 1_555 1_555 yes O(3) C(41) C(13) 119.0(3) 1_555 1_555 1_555 yes C(9) C(41) C(13) 123.0(3) 1_555 1_555 1_555 yes O(2) C(42) C(3) 118.7(3) 1_555 1_555 1_555 yes O(2) C(42) C(7) 118.9(3) 1_555 1_555 1_555 yes C(3) C(42) C(7) 122.3(3) 1_555 1_555 1_555 yes C(44) C(43) C(48) 120.2(7) 1_555 1_555 1_555 yes C(43) C(44) C(45) 121.5(7) 1_555 1_555 1_555 yes C(44) C(45) C(46) 121.0(7) 1_555 1_555 1_555 yes C(45) C(46) C(47) 120.7(7) 1_555 1_555 1_555 yes C(46) C(47) C(48) 117.5(6) 1_555 1_555 1_555 yes C(43) C(48) C(47) 119.1(6) 1_555 1_555 1_555 yes C(50) C(49) C(54) 120.0(5) 1_555 1_555 1_555 yes C(49) C(50) C(51) 118.3(5) 1_555 1_555 1_555 yes C(50) C(51) C(52) 120.0(5) 1_555 1_555 1_555 yes C(51) C(52) C(53) 119.4(6) 1_555 1_555 1_555 yes C(52) C(53) C(54) 120.9(5) 1_555 1_555 1_555 yes C(49) C(54) C(53) 121.3(5) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ 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 Ag(1) O(7) Ag(1) O(7) 0.0 1_555 1_555 2_564 2_564 yes Ag(1) O(7) Ag(1) C(29) -122.2(2) 1_555 1_555 2_564 1_555 yes Ag(1) O(7) Ag(1) C(35) 108.9(1) 1_555 1_555 2_564 2_564 yes Ag(1) O(7) Cl(1) O(8) -49.0(4) 1_555 1_555 1_555 1_555 yes Ag(1) O(7) Cl(1) O(9) 80.1(5) 1_555 1_555 1_555 1_555 yes Ag(1) O(7) Cl(1) O(10) -162.9(3) 1_555 1_555 1_555 1_555 yes Ag(1) O(7) Ag(1) O(7) 0.0 1_555 2_564 2_564 1_555 yes Ag(1) O(7) Ag(1) C(29) 117.1(1) 1_555 2_564 2_564 1_555 yes Ag(1) O(7) Ag(1) C(35) -101.7(2) 1_555 2_564 2_564 2_564 yes Ag(1) O(7) Cl(1) O(8) -97.1(3) 1_555 2_564 2_564 2_564 yes Ag(1) O(7) Cl(1) O(9) 133.7(4) 1_555 2_564 2_564 2_564 yes Ag(1) O(7) Cl(1) O(10) 16.8(4) 1_555 2_564 2_564 2_564 yes Ag(1) C(29) C(28) C(27) -83.6(4) 1_555 2_564 2_564 2_564 yes Ag(1) C(29) C(30) C(31) 93.6(4) 1_555 2_564 2_564 2_564 yes Ag(1) C(35) C(34) C(33) 92.6(3) 1_555 1_555 1_555 1_555 yes Ag(1) C(35) C(36) C(1) -93.0(4) 1_555 1_555 1_555 1_555 yes Cl(1) O(7) Ag(1) O(7) 152.7(4) 1_555 1_555 1_555 2_564 yes Cl(1) O(7) Ag(1) C(29) 35.6(3) 1_555 1_555 1_555 2_564 yes Cl(1) O(7) Ag(1) C(35) -105.5(3) 1_555 1_555 1_555 1_555 yes Cl(1) O(7) Ag(1) O(7) -153.9(4) 1_555 1_555 2_564 2_564 yes Cl(1) O(7) Ag(1) C(29) 83.9(3) 1_555 1_555 2_564 1_555 yes Cl(1) O(7) Ag(1) C(35) -45.0(3) 1_555 1_555 2_564 2_564 yes O(1) C(37) C(1) C(2) 0.1(5) 1_555 1_555 1_555 1_555 yes O(1) C(37) C(1) C(36) 179.9(3) 1_555 1_555 1_555 1_555 yes O(1) C(37) C(33) C(32) 2.8(5) 1_555 1_555 1_555 1_555 yes O(1) C(37) C(33) C(34) -179.9(3) 1_555 1_555 1_555 1_555 yes O(2) C(42) C(3) C(2) -6.9(5) 1_555 1_555 1_555 1_555 yes O(2) C(42) C(3) C(4) 175.0(3) 1_555 1_555 1_555 1_555 yes O(2) C(42) C(7) C(6) -176.9(3) 1_555 1_555 1_555 1_555 yes O(2) C(42) C(7) C(8) 3.1(5) 1_555 1_555 1_555 1_555 yes O(3) C(41) C(9) C(8) 1.5(4) 1_555 1_555 1_555 1_555 yes O(3) C(41) C(9) C(10) -178.7(3) 1_555 1_555 1_555 1_555 yes O(3) C(41) C(13) C(12) 178.6(3) 1_555 1_555 1_555 1_555 yes O(3) C(41) C(13) C(14) -4.4(4) 1_555 1_555 1_555 1_555 yes O(4) C(40) C(15) C(14) 2.1(5) 1_555 1_555 1_555 1_555 yes O(4) C(40) C(15) C(16) -179.2(3) 1_555 1_555 1_555 1_555 yes O(4) C(40) C(19) C(18) 178.9(3) 1_555 1_555 1_555 1_555 yes O(4) C(40) C(19) C(20) -1.4(5) 1_555 1_555 1_555 1_555 yes O(5) C(39) C(21) C(20) -3.4(5) 1_555 1_555 1_555 1_555 yes O(5) C(39) C(21) C(22) 177.4(3) 1_555 1_555 1_555 1_555 yes O(5) C(39) C(25) C(24) -178.4(3) 1_555 1_555 1_555 1_555 yes O(5) C(39) C(25) C(26) 5.0(5) 1_555 1_555 1_555 1_555 yes O(6) C(38) C(27) C(26) 1.9(5) 1_555 1_555 1_555 1_555 yes O(6) C(38) C(27) C(28) -179.5(3) 1_555 1_555 1_555 1_555 yes O(6) C(38) C(31) C(30) -179.7(3) 1_555 1_555 1_555 1_555 yes O(6) C(38) C(31) C(32) -4.8(5) 1_555 1_555 1_555 1_555 yes O(7) Ag(1) O(7) Ag(1) 0.0 1_555 1_555 2_564 2_564 yes O(7) Ag(1) C(29) C(28) 161.0(2) 1_555 1_555 2_564 2_564 yes O(7) Ag(1) C(29) C(30) 42.8(3) 1_555 1_555 2_564 2_564 yes O(7) Ag(1) C(35) C(34) -41.4(3) 1_555 1_555 1_555 1_555 yes O(7) Ag(1) C(35) C(36) 78.7(3) 1_555 1_555 1_555 1_555 yes O(7) Ag(1) O(7) Ag(1) 0.0 1_555 2_564 2_564 1_555 yes O(7) Ag(1) C(29) C(28) -64.0(3) 1_555 2_564 1_555 1_555 yes O(7) Ag(1) C(29) C(30) 54.1(3) 1_555 2_564 1_555 1_555 yes O(7) Ag(1) C(35) C(34) -43.8(3) 1_555 2_564 2_564 2_564 yes O(7) Ag(1) C(35) C(36) -163.9(2) 1_555 2_564 2_564 2_564 yes C(1) C(2) C(3) C(4) -76.8(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(42) 105.2(4) 1_555 1_555 1_555 1_555 yes C(1) C(36) C(35) C(34) -0.3(6) 1_555 1_555 1_555 1_555 yes C(1) C(37) C(33) C(32) -176.0(3) 1_555 1_555 1_555 1_555 yes C(1) C(37) C(33) C(34) 1.2(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(36) C(35) -179.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(37) C(33) 178.9(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -174.6(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(42) C(7) 172.5(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(36) 107.0(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(37) -73.2(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 0.4(6) 1_555 1_555 1_555 1_555 yes C(3) C(42) C(7) C(6) 3.7(5) 1_555 1_555 1_555 1_555 yes C(3) C(42) C(7) C(8) -176.3(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(42) C(7) -5.6(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -2.4(6) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(3) C(42) 3.5(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -179.6(3) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(42) 0.3(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 78.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -108.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(41) 71.0(4) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 179.4(3) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(41) C(13) -177.5(3) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(42) -101.2(4) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) -1.4(6) 1_555 1_555 1_555 1_555 yes C(9) C(41) C(13) C(12) -2.4(5) 1_555 1_555 1_555 1_555 yes C(9) C(41) C(13) C(14) 174.6(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(41) C(13) 2.3(5) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(12) C(13) 1.4(6) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(41) -0.4(5) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) -176.5(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(41) 0.5(5) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -90.9(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 92.0(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(40) -89.4(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 179.2(3) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(40) C(19) -178.2(3) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(41) 92.2(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) -1.2(6) 1_555 1_555 1_555 1_555 yes C(15) C(40) C(19) C(18) -0.9(5) 1_555 1_555 1_555 1_555 yes C(15) C(40) C(19) C(20) 178.8(3) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(40) C(19) 0.5(5) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) 0.8(6) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(15) C(40) 0.5(5) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) -179.5(4) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(40) 0.2(6) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) 104.7(4) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) -78.5(4) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(39) 102.3(4) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) -176.8(3) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(39) C(25) 175.2(3) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(19) C(40) -75.0(4) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 0.2(6) 1_555 1_555 1_555 1_555 yes C(21) C(39) C(25) C(24) 3.0(5) 1_555 1_555 1_555 1_555 yes C(21) C(39) C(25) C(26) -173.5(3) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(39) C(25) -4.1(5) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) -1.3(6) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(39) 2.5(5) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 176.3(4) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(39) -0.3(6) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) 81.7(4) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(28) -105.1(4) 1_555 1_555 1_555 1_555 yes C(25) C(26) C(27) C(38) 73.5(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(28) C(29) 178.4(4) 1_555 1_555 1_555 1_555 yes C(26) C(27) C(38) C(31) -177.5(3) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(39) -101.8(4) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) -1.5(6) 1_555 1_555 1_555 1_555 yes C(27) C(38) C(31) C(30) -0.4(6) 1_555 1_555 1_555 1_555 yes C(27) C(38) C(31) C(32) 174.6(3) 1_555 1_555 1_555 1_555 yes C(28) C(27) C(38) C(31) 1.1(5) 1_555 1_555 1_555 1_555 yes C(28) C(29) Ag(1) C(35) 59.5(3) 1_555 1_555 2_564 2_564 yes C(28) C(29) C(30) C(31) 2.3(6) 1_555 1_555 1_555 1_555 yes C(29) Ag(1) C(35) C(34) -174.3(2) 1_555 2_564 2_564 2_564 yes C(29) Ag(1) C(35) C(36) 65.6(3) 1_555 2_564 2_564 2_564 yes C(29) C(28) C(27) C(38) -0.2(6) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -176.4(4) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(38) -1.4(6) 1_555 1_555 1_555 1_555 yes C(30) C(29) Ag(1) C(35) 177.7(2) 1_555 1_555 2_564 2_564 yes C(30) C(31) C(32) C(33) -95.0(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 91.1(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(37) -91.6(4) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(35) 176.6(3) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(38) 90.2(4) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) 0.3(6) 1_555 1_555 1_555 1_555 yes C(33) C(37) C(1) C(36) -1.3(5) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(33) C(37) -0.7(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(1) C(37) 0.8(6) 1_555 1_555 1_555 1_555 yes C(43) C(44) C(45) C(46) -0.7(10) 1_555 1_555 1_555 1_555 yes C(43) C(48) C(47) C(46) 2.3(9) 1_555 1_555 1_555 1_555 yes C(44) C(43) C(48) C(47) -2.6(10) 1_555 1_555 1_555 1_555 yes C(44) C(45) C(46) C(47) 0.5(9) 1_555 1_555 1_555 1_555 yes C(45) C(44) C(43) C(48) 1(1) 1_555 1_555 1_555 1_555 yes C(45) C(46) C(47) C(48) -1.3(9) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) -2.3(8) 1_555 1_555 1_555 1_555 yes C(49) C(54) C(53) C(52) -0.5(9) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(54) C(53) -0.4(8) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) 1.4(9) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(54) 1.8(7) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) 0.0(9) 1_555 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 O(2) C(53) 3.298(6) 1_555 1_554 ? O(2) C(54) 3.503(6) 1_555 1_554 ? O(9) C(44) 3.547(9) 1_555 1_555 ? C(4) C(17) 3.505(6) 1_555 1_564 ? C(13) C(50) 3.574(6) 1_555 1_555 ? C(15) C(48) 3.510(7) 1_555 1_556 ? C(23) C(34) 3.534(6) 1_555 1_545 ? C(25) C(35) 3.499(5) 1_555 1_545 ? C(31) C(46) 3.542(7) 1_555 1_556 ? C(35) C(39) 3.491(5) 1_555 1_565 ? C(41) C(50) 3.432(5) 1_555 1_555 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #=END data_[Ag(calix[6]arene)](CF3SO3 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 28 09:55:39 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1049.90 _chemical_formula_analytical ? _chemical_formula_sum 'C55 H48 Ag F3 O9 S ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 21.379(4) _cell_length_b 11.788(4) _cell_length_c 10.324(2) _cell_angle_alpha 70.91(2) _cell_angle_beta 80.33(1) _cell_angle_gamma 78.74(2) _cell_volume 2396(1) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.7 _cell_measurement_theta_max 12.3 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080.00 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.90 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -1 0 -3 -1 1 -4 -1 1 _diffrn_reflns_number 11554 _reflns_number_total 11016 _reflns_number_gt 5120 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03794 _diffrn_orient_matrix_UB_12 0.02737 _diffrn_orient_matrix_UB_13 0.05953 _diffrn_orient_matrix_UB_21 -0.02728 _diffrn_orient_matrix_UB_22 0.01976 _diffrn_orient_matrix_UB_23 -0.07653 _diffrn_orient_matrix_UB_31 -0.01093 _diffrn_orient_matrix_UB_32 -0.08430 _diffrn_orient_matrix_UB_33 0.03521 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'AgAg' -0.897 1.101 ;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) ; 'F' 'F' 0.017 0.010 ;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) ; '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) ; #------------------------------------------------------------------------------ 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 Ag(1) Ag 0.04401(4) 0.62213(8) -0.08605(9) 0.0748(3) Uani 1.00 d ... S(1) S 0.0579(2) 0.3554(5) -0.1984(5) 0.140(2) Uani 1.00 d ... F(1) F 0.1434(5) 0.489(1) -0.318(1) 0.161(4) Uiso 1.00 d ... F(2) F 0.1379(5) 0.3460(9) -0.404(1) 0.147(3) Uiso 1.00 d ... F(3) F 0.1679(6) 0.290(1) -0.186(1) 0.175(4) Uiso 1.00 d ... O(1) O 0.2387(3) 0.3168(5) 0.0197(6) 0.057(2) Uani 1.00 d ... O(2) O 0.1700(3) 0.1351(6) 0.1227(7) 0.071(2) Uani 1.00 d ... O(3) O 0.2180(3) -0.0696(6) 0.0593(6) 0.060(2) Uani 1.00 d ... O(4) O 0.3176(3) -0.0633(5) 0.1804(6) 0.061(2) Uani 1.00 d ... O(5) O 0.3831(3) 0.1198(5) 0.0723(6) 0.058(2) Uani 1.00 d ... O(6) O 0.3448(3) 0.2866(5) -0.1539(6) 0.054(2) Uani 1.00 d ... O(7) O 0.0476(3) 0.4166(6) -0.0974(6) 0.076(2) Uani 1.00 d ... O(8) O 0.0199(4) 0.4509(8) -0.3511(9) 0.113(3) Uani 1.00 d ... O(9) O 0.0408(5) 0.2405(7) -0.164(1) 0.114(4) Uani 1.00 d ... C(1) C 0.2170(4) 0.5308(8) -0.0936(9) 0.056(3) Uani 1.00 d ... C(2) C 0.2680(5) 0.5211(8) -0.2085(9) 0.064(3) Uani 1.00 d ... C(3) C 0.3379(4) 0.4964(8) -0.1724(8) 0.053(2) Uani 1.00 d ... C(4) C 0.3676(5) 0.5875(9) -0.1638(10) 0.069(3) Uani 1.00 d ... C(5) C 0.4307(5) 0.5676(9) -0.1421(10) 0.065(3) Uani 1.00 d ... C(6) C 0.4652(4) 0.4550(9) -0.1301(9) 0.060(3) Uani 1.00 d ... C(7) C 0.4390(4) 0.3601(7) -0.1356(8) 0.048(2) Uani 1.00 d ... C(8) C 0.4795(4) 0.2353(8) -0.1206(9) 0.054(3) Uani 1.00 d ... C(9) C 0.4905(4) 0.1582(7) 0.0243(9) 0.052(2) Uani 1.00 d ... C(10) C 0.5509(4) 0.1397(8) 0.068(1) 0.061(3) Uani 1.00 d ... C(11) C 0.5611(4) 0.0681(10) 0.203(1) 0.072(3) Uani 1.00 d ... C(12) C 0.5120(4) 0.0189(8) 0.2918(10) 0.057(3) Uani 1.00 d ... C(13) C 0.4505(4) 0.0345(7) 0.2518(9) 0.051(2) Uani 1.00 d ... C(14) C 0.3944(4) -0.0167(8) 0.3531(8) 0.055(3) Uani 1.00 d ... C(15) C 0.3853(4) -0.1424(7) 0.3620(8) 0.048(2) Uani 1.00 d ... C(16) C 0.4135(4) -0.2444(9) 0.4586(9) 0.061(3) Uani 1.00 d ... C(17) C 0.4039(5) -0.3587(9) 0.471(1) 0.068(3) Uani 1.00 d ... C(18) C 0.3648(5) -0.3751(8) 0.389(1) 0.066(3) Uani 1.00 d ... C(19) C 0.3350(4) -0.2783(8) 0.2903(9) 0.052(2) Uani 1.00 d ... C(20) C 0.2908(4) -0.2967(8) 0.200(1) 0.063(3) Uani 1.00 d ... C(21) C 0.2202(4) -0.2613(8) 0.2367(10) 0.056(3) Uani 1.00 d ... C(22) C 0.1868(5) -0.3386(9) 0.345(1) 0.068(3) Uani 1.00 d ... C(23) C 0.1205(6) -0.312(1) 0.381(1) 0.082(4) Uani 1.00 d ... C(24) C 0.0886(4) -0.204(1) 0.301(1) 0.074(4) Uani 1.00 d ... C(25) C 0.1187(4) -0.1238(8) 0.1940(9) 0.056(3) Uani 1.00 d ... C(26) C 0.0818(4) -0.0104(10) 0.107(1) 0.069(3) Uani 1.00 d ... C(27) C 0.0629(4) 0.0912(8) 0.1725(9) 0.059(3) Uani 1.00 d ... C(28) C 0.0006(4) 0.1186(10) 0.229(1) 0.070(3) Uani 1.00 d ... C(29) C -0.0171(4) 0.210(1) 0.291(1) 0.071(3) Uani 1.00 d ... C(30) C 0.0297(5) 0.2766(9) 0.2974(9) 0.067(3) Uani 1.00 d ... C(31) C 0.0929(4) 0.2529(9) 0.2378(9) 0.057(3) Uani 1.00 d ... C(32) C 0.1432(4) 0.3226(9) 0.2487(9) 0.063(3) Uani 1.00 d ... C(33) C 0.1552(4) 0.4330(8) 0.1273(9) 0.053(3) Uani 1.00 d ... C(34) C 0.1212(4) 0.550(1) 0.123(1) 0.075(4) Uani 1.00 d ... C(35) C 0.1327(5) 0.6522(10) 0.014(1) 0.073(4) Uani 1.00 d ... C(36) C 0.1801(5) 0.6422(9) -0.092(1) 0.068(3) Uani 1.00 d ... C(37) C 0.2036(4) 0.4279(8) 0.0179(9) 0.053(3) Uani 1.00 d ... C(38) C 0.1077(4) 0.1614(8) 0.1768(9) 0.057(3) Uani 1.00 d ... C(39) C 0.1861(4) -0.1507(8) 0.1625(10) 0.057(3) Uani 1.00 d ... C(40) C 0.3473(4) -0.1635(7) 0.2775(8) 0.048(2) Uani 1.00 d ... C(41) C 0.4425(4) 0.1033(7) 0.1156(9) 0.048(2) Uani 1.00 d ... C(42) C 0.3742(4) 0.3805(8) -0.1532(8) 0.050(2) Uani 1.00 d ... C(43) C 0.114(2) 0.393(4) -0.272(4) 0.28(1) Uiso 1.00 d ... C(44) C 0.3303(8) 0.270(1) -0.473(1) 0.099(5) Uani 1.00 d ... C(45) C 0.3928(6) 0.280(1) -0.498(1) 0.085(4) Uani 1.00 d ... C(46) C 0.4201(5) 0.312(1) -0.626(1) 0.086(4) Uani 1.00 d ... C(47) C 0.3879(7) 0.338(1) -0.735(1) 0.083(4) Uani 1.00 d ... C(48) C 0.3244(8) 0.331(1) -0.713(1) 0.103(5) Uani 1.00 d ... C(49) C 0.2946(7) 0.294(2) -0.579(2) 0.127(7) Uani 1.00 d ... C(50) C 0.192(2) 0.023(3) -0.303(2) 0.17(1) Uani 1.00 d ... C(51) C 0.244(1) -0.053(3) -0.322(3) 0.144(9) Uani 1.00 d ... C(52) C 0.247(1) -0.109(2) -0.411(3) 0.156(8) Uani 1.00 d ... C(53) C 0.198(2) -0.090(2) -0.483(2) 0.16(1) Uani 1.00 d ... C(54) C 0.146(1) -0.009(2) -0.470(2) 0.138(8) Uani 1.00 d ... C(55) C 0.143(1) 0.049(1) -0.377(3) 0.130(7) Uani 1.00 d ... H(1) H 0.2626 0.5960 -0.2809 0.0767 Uiso 1.00 calc ... H(2) H 0.2617 0.4573 -0.2389 0.0767 Uiso 1.00 calc ... H(3) H 0.3435 0.6664 -0.1740 0.0831 Uiso 1.00 calc ... H(4) H 0.4502 0.6313 -0.1354 0.0777 Uiso 1.00 calc ... H(5) H 0.5094 0.4423 -0.1169 0.0717 Uiso 1.00 calc ... H(6) H 0.5201 0.2469 -0.1720 0.0651 Uiso 1.00 calc ... H(7) H 0.4584 0.1913 -0.1586 0.0651 Uiso 1.00 calc ... H(8) H 0.5851 0.1751 0.0062 0.0726 Uiso 1.00 calc ... H(9) H 0.6028 0.0543 0.2310 0.0856 Uiso 1.00 calc ... H(10) H 0.5199 -0.0277 0.3832 0.0702 Uiso 1.00 calc ... H(11) H 0.4011 -0.0183 0.4424 0.0666 Uiso 1.00 calc ... H(12) H 0.3562 0.0364 0.3267 0.0666 Uiso 1.00 calc ... H(13) H 0.4401 -0.2340 0.5176 0.0717 Uiso 1.00 calc ... H(14) H 0.4246 -0.4265 0.5360 0.0816 Uiso 1.00 calc ... H(15) H 0.3577 -0.4554 0.3996 0.0793 Uiso 1.00 calc ... H(16) H 0.2982 -0.3809 0.2062 0.0760 Uiso 1.00 calc ... H(17) H 0.3020 -0.2503 0.1076 0.0760 Uiso 1.00 calc ... H(18) H 0.2096 -0.4124 0.3972 0.0821 Uiso 1.00 calc ... H(19) H 0.0981 -0.3658 0.4555 0.0986 Uiso 1.00 calc ... H(20) H 0.0434 -0.1849 0.3224 0.0873 Uiso 1.00 calc ... H(21) H 0.1078 0.0178 0.0230 0.0828 Uiso 1.00 calc ... H(22) H 0.0439 -0.0307 0.0903 0.0828 Uiso 1.00 calc ... H(23) H -0.0311 0.0733 0.2280 0.0842 Uiso 1.00 calc ... H(24) H -0.0604 0.2289 0.3273 0.0852 Uiso 1.00 calc ... H(25) H 0.0184 0.3378 0.3420 0.0803 Uiso 1.00 calc ... H(26) H 0.1826 0.2696 0.2601 0.0762 Uiso 1.00 calc ... H(27) H 0.1299 0.3499 0.3279 0.0762 Uiso 1.00 calc ... H(28) H 0.0890 0.5569 0.1969 0.0891 Uiso 1.00 calc ... H(29) H 0.1082 0.7287 0.0135 0.0880 Uiso 1.00 calc ... H(30) H 0.1875 0.7131 -0.1656 0.0822 Uiso 1.00 calc ... H(31) H 0.2631 0.2397 0.0214 0.0683 Uiso 1.00 calc ... H(32) H 0.2131 0.1170 0.0848 0.0841 Uiso 1.00 calc ... H(33) H 0.2402 -0.0130 -0.0130 0.0715 Uiso 1.00 calc ... H(34) H 0.2975 0.0043 0.1140 0.0731 Uiso 1.00 calc ... H(35) H 0.3421 0.1310 0.0421 0.0693 Uiso 1.00 calc ... H(36) H 0.3245 0.2216 -0.1544 0.0651 Uiso 1.00 calc ... H(37) H 0.3110 0.2448 -0.3778 0.1166 Uiso 1.00 calc ... H(38) H 0.4181 0.2640 -0.4224 0.1001 Uiso 1.00 calc ... H(39) H 0.4656 0.3187 -0.6418 0.1016 Uiso 1.00 calc ... H(40) H 0.4099 0.3616 -0.8272 0.0985 Uiso 1.00 calc ... H(41) H 0.3007 0.3506 -0.7910 0.1224 Uiso 1.00 calc ... H(42) H 0.2489 0.2881 -0.5621 0.1480 Uiso 1.00 calc ... H(43) H 0.1872 0.0661 -0.2351 0.1905 Uiso 1.00 calc ... H(44) H 0.2794 -0.0650 -0.2653 0.1718 Uiso 1.00 calc ... H(45) H 0.2856 -0.1643 -0.4245 0.1832 Uiso 1.00 calc ... H(46) H 0.1993 -0.1394 -0.5438 0.1787 Uiso 1.00 calc ... H(47) H 0.1119 0.0081 -0.5278 0.1650 Uiso 1.00 calc ... H(48) H 0.1042 0.1068 -0.3649 0.1523 Uiso 1.00 calc ... 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 Ag(1) 0.0589(5) 0.0827(6) 0.0794(6) 0.0089(4) -0.0144(4) -0.0283(4) S(1) 0.123(3) 0.165(4) 0.171(4) -0.060(3) 0.074(3) -0.124(4) O(1) 0.047(3) 0.053(3) 0.063(4) 0.008(3) -0.001(3) -0.019(3) O(2) 0.036(3) 0.080(4) 0.095(5) -0.005(3) 0.006(3) -0.033(4) O(3) 0.048(3) 0.077(4) 0.049(3) -0.014(3) 0.003(3) -0.012(3) O(4) 0.056(4) 0.054(4) 0.065(4) 0.001(3) -0.019(3) -0.007(3) O(5) 0.037(3) 0.066(4) 0.065(4) -0.010(3) -0.014(3) -0.008(3) O(6) 0.055(3) 0.057(4) 0.057(3) -0.012(3) -0.009(3) -0.022(3) O(7) 0.088(5) 0.085(5) 0.059(4) -0.002(4) -0.006(3) -0.036(4) O(8) 0.110(7) 0.111(7) 0.113(7) 0.032(5) -0.055(5) -0.034(5) O(9) 0.127(8) 0.076(6) 0.154(9) -0.034(5) -0.028(6) -0.038(5) C(1) 0.047(5) 0.055(5) 0.065(6) 0.002(4) -0.018(4) -0.016(5) C(2) 0.065(6) 0.064(6) 0.053(5) 0.005(4) -0.018(4) -0.009(4) C(3) 0.052(5) 0.058(6) 0.040(5) -0.002(4) -0.002(4) -0.006(4) C(4) 0.085(7) 0.051(6) 0.061(6) -0.005(5) -0.001(5) -0.009(5) C(5) 0.066(6) 0.064(6) 0.064(6) -0.017(5) -0.004(5) -0.016(5) C(6) 0.054(5) 0.060(6) 0.060(6) -0.013(5) 0.001(4) -0.010(5) C(7) 0.049(5) 0.055(5) 0.034(4) -0.007(4) 0.008(3) -0.011(4) C(8) 0.032(4) 0.070(6) 0.058(5) -0.004(4) 0.003(4) -0.024(5) C(9) 0.051(5) 0.047(5) 0.057(5) 0.003(4) 0.003(4) -0.025(4) C(10) 0.025(4) 0.062(6) 0.099(8) 0.000(4) -0.011(4) -0.031(5) C(11) 0.039(5) 0.083(7) 0.100(8) 0.003(5) -0.021(5) -0.037(6) C(12) 0.052(5) 0.056(5) 0.068(6) -0.004(4) -0.020(4) -0.020(4) C(13) 0.054(5) 0.042(5) 0.059(5) -0.009(4) 0.000(4) -0.022(4) C(14) 0.055(5) 0.065(6) 0.045(5) 0.000(4) -0.010(4) -0.020(4) C(15) 0.044(4) 0.050(5) 0.047(5) -0.001(4) 0.000(4) -0.016(4) C(16) 0.054(5) 0.070(7) 0.049(5) -0.001(4) -0.010(4) -0.009(5) C(17) 0.067(6) 0.053(6) 0.067(6) 0.001(5) -0.010(5) 0.002(5) C(18) 0.063(6) 0.042(5) 0.079(7) 0.005(4) -0.001(5) -0.010(5) C(19) 0.045(5) 0.048(5) 0.061(5) -0.002(4) 0.000(4) -0.020(4) C(20) 0.061(6) 0.054(5) 0.077(6) -0.003(4) -0.004(5) -0.029(5) C(21) 0.052(5) 0.058(6) 0.068(6) -0.012(4) -0.003(4) -0.031(5) C(22) 0.068(6) 0.060(6) 0.080(7) -0.014(5) -0.005(5) -0.025(5) C(23) 0.078(8) 0.073(7) 0.097(8) -0.026(6) 0.001(6) -0.024(6) C(24) 0.046(5) 0.083(8) 0.102(8) -0.015(5) -0.008(5) -0.038(7) C(25) 0.048(5) 0.064(6) 0.065(6) -0.012(4) -0.009(4) -0.030(5) C(26) 0.042(5) 0.086(7) 0.084(7) -0.010(5) -0.021(5) -0.026(6) C(27) 0.043(5) 0.068(6) 0.064(6) -0.006(4) -0.010(4) -0.015(5) C(28) 0.043(5) 0.086(7) 0.070(6) -0.007(5) -0.010(4) -0.010(6) C(29) 0.034(5) 0.087(7) 0.073(7) -0.001(5) 0.004(4) -0.008(6) C(30) 0.067(6) 0.072(6) 0.050(5) 0.008(5) -0.002(4) -0.014(5) C(31) 0.043(5) 0.076(6) 0.048(5) -0.005(4) 0.001(4) -0.019(5) C(32) 0.052(5) 0.082(7) 0.058(6) 0.002(5) -0.004(4) -0.033(5) C(33) 0.038(4) 0.071(6) 0.057(5) -0.004(4) -0.005(4) -0.032(5) C(34) 0.043(5) 0.108(9) 0.100(8) 0.001(5) -0.015(5) -0.070(8) C(35) 0.067(6) 0.069(7) 0.090(8) 0.003(5) -0.019(6) -0.037(6) C(36) 0.063(6) 0.067(6) 0.077(7) 0.005(5) -0.028(5) -0.023(5) C(37) 0.045(5) 0.061(6) 0.060(5) 0.001(4) -0.020(4) -0.027(5) C(38) 0.039(5) 0.072(6) 0.049(5) 0.003(4) -0.006(4) -0.010(4) C(39) 0.056(5) 0.065(6) 0.064(6) -0.006(4) -0.013(5) -0.036(5) C(40) 0.036(4) 0.050(5) 0.053(5) -0.001(3) 0.004(4) -0.015(4) C(41) 0.042(5) 0.047(5) 0.058(5) 0.000(4) -0.004(4) -0.024(4) C(42) 0.048(5) 0.064(6) 0.032(4) -0.003(4) -0.001(3) -0.010(4) C(44) 0.13(1) 0.11(1) 0.060(7) -0.035(9) 0.000(7) -0.033(7) C(45) 0.088(9) 0.083(8) 0.084(8) 0.004(6) -0.036(7) -0.020(6) C(46) 0.060(6) 0.103(9) 0.088(9) 0.010(6) -0.001(6) -0.035(7) C(47) 0.111(10) 0.081(8) 0.057(6) -0.010(7) 0.006(7) -0.030(6) C(48) 0.11(1) 0.13(1) 0.092(10) -0.025(9) -0.042(8) -0.045(8) C(49) 0.076(9) 0.21(2) 0.13(1) -0.06(1) 0.004(9) -0.08(1) C(50) 0.29(3) 0.17(2) 0.10(1) -0.13(2) 0.01(2) -0.06(1) C(51) 0.09(1) 0.17(2) 0.15(2) -0.03(1) -0.03(1) 0.00(2) C(52) 0.13(2) 0.11(1) 0.14(2) 0.03(1) 0.08(1) 0.01(1) C(53) 0.30(3) 0.11(2) 0.060(10) -0.06(2) 0.04(1) -0.05(1) C(54) 0.16(2) 0.13(2) 0.11(1) -0.06(1) -0.07(1) 0.03(1) C(55) 0.12(1) 0.09(1) 0.16(2) -0.006(9) 0.03(1) -0.04(1) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _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) + 0.00090|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5120 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.412 _refine_ls_shift/su_max 0.3480 _refine_ls_shift/su_mean 0.0160 _refine_diff_density_min -1.22 _refine_diff_density_max 1.54 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 S(1) O(7) 1.418(7) 1_555 1_555 yes S(1) O(9) 1.389(8) 1_555 1_555 yes S(1) C(43) 1.37(4) 1_555 1_555 yes F(1) C(43) 1.31(4) 1_555 1_555 yes F(2) C(43) 1.61(4) 1_555 1_555 yes O(1) C(37) 1.372(10) 1_555 1_555 yes O(2) C(38) 1.373(10) 1_555 1_555 yes O(3) C(39) 1.36(1) 1_555 1_555 yes O(4) C(40) 1.395(10) 1_555 1_555 yes O(5) C(41) 1.373(9) 1_555 1_555 yes O(6) C(42) 1.38(1) 1_555 1_555 yes C(1) C(2) 1.49(1) 1_555 1_555 yes C(1) C(36) 1.40(1) 1_555 1_555 yes C(1) C(37) 1.41(1) 1_555 1_555 yes C(2) C(3) 1.55(1) 1_555 1_555 yes C(3) C(4) 1.38(1) 1_555 1_555 yes C(3) C(42) 1.40(1) 1_555 1_555 yes C(4) C(5) 1.37(1) 1_555 1_555 yes C(5) C(6) 1.36(1) 1_555 1_555 yes C(6) C(7) 1.37(1) 1_555 1_555 yes C(7) C(8) 1.53(1) 1_555 1_555 yes C(7) C(42) 1.39(1) 1_555 1_555 yes C(8) C(9) 1.51(1) 1_555 1_555 yes C(9) C(10) 1.39(1) 1_555 1_555 yes C(9) C(41) 1.38(1) 1_555 1_555 yes C(10) C(11) 1.40(1) 1_555 1_555 yes C(11) C(12) 1.36(1) 1_555 1_555 yes C(12) C(13) 1.40(1) 1_555 1_555 yes C(13) C(14) 1.53(1) 1_555 1_555 yes C(13) C(41) 1.40(1) 1_555 1_555 yes C(14) C(15) 1.50(1) 1_555 1_555 yes C(15) C(16) 1.39(1) 1_555 1_555 yes C(15) C(40) 1.39(1) 1_555 1_555 yes C(16) C(17) 1.36(1) 1_555 1_555 yes C(17) C(18) 1.36(1) 1_555 1_555 yes C(18) C(19) 1.38(1) 1_555 1_555 yes C(19) C(20) 1.52(1) 1_555 1_555 yes C(19) C(40) 1.39(1) 1_555 1_555 yes C(20) C(21) 1.50(1) 1_555 1_555 yes C(21) C(22) 1.38(1) 1_555 1_555 yes C(21) C(39) 1.41(1) 1_555 1_555 yes C(22) C(23) 1.40(1) 1_555 1_555 yes C(23) C(24) 1.39(1) 1_555 1_555 yes C(24) C(25) 1.35(1) 1_555 1_555 yes C(25) C(26) 1.50(1) 1_555 1_555 yes C(25) C(39) 1.42(1) 1_555 1_555 yes C(26) C(27) 1.52(1) 1_555 1_555 yes C(27) C(28) 1.38(1) 1_555 1_555 yes C(27) C(38) 1.40(1) 1_555 1_555 yes C(28) C(29) 1.39(1) 1_555 1_555 yes C(29) C(30) 1.41(1) 1_555 1_555 yes C(30) C(31) 1.40(1) 1_555 1_555 yes C(31) C(32) 1.51(1) 1_555 1_555 yes C(31) C(38) 1.38(1) 1_555 1_555 yes C(32) C(33) 1.51(1) 1_555 1_555 yes C(33) C(34) 1.42(1) 1_555 1_555 yes C(33) C(37) 1.41(1) 1_555 1_555 yes C(34) C(35) 1.38(2) 1_555 1_555 yes C(35) C(36) 1.38(1) 1_555 1_555 yes C(44) C(45) 1.34(2) 1_555 1_555 yes C(44) C(49) 1.37(2) 1_555 1_555 yes C(45) C(46) 1.32(2) 1_555 1_555 yes C(46) C(47) 1.33(2) 1_555 1_555 yes C(47) C(48) 1.35(2) 1_555 1_555 yes C(48) C(49) 1.39(2) 1_555 1_555 yes C(50) C(51) 1.31(3) 1_555 1_555 yes C(50) C(55) 1.35(3) 1_555 1_555 yes C(51) C(52) 1.28(3) 1_555 1_555 yes C(52) C(53) 1.34(3) 1_555 1_555 yes C(53) C(54) 1.33(3) 1_555 1_555 yes C(54) C(55) 1.33(3) 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 O(7) S(1) O(9) 119.6(6) 1_555 1_555 1_555 yes O(7) S(1) C(43) 101(1) 1_555 1_555 1_555 yes O(9) S(1) C(43) 127(1) 1_555 1_555 1_555 yes C(37) O(1) H(31) 179.8(7) 1_555 1_555 1_555 no C(38) O(2) H(32) 179.7(8) 1_555 1_555 1_555 no C(39) O(3) H(33) 179.9(7) 1_555 1_555 1_555 no C(40) O(4) H(34) 179.6(7) 1_555 1_555 1_555 no C(41) O(5) H(35) 179.8(7) 1_555 1_555 1_555 no C(42) O(6) H(36) 180.0(6) 1_555 1_555 1_555 no C(2) C(1) C(36) 121.4(9) 1_555 1_555 1_555 yes C(2) C(1) C(37) 121.4(8) 1_555 1_555 1_555 yes C(36) C(1) C(37) 117.2(9) 1_555 1_555 1_555 yes C(1) C(2) C(3) 115.6(7) 1_555 1_555 1_555 yes C(1) C(2) H(1) 107.2(8) 1_555 1_555 1_555 no C(1) C(2) H(2) 107.7(9) 1_555 1_555 1_555 no C(3) C(2) H(1) 108.2(9) 1_555 1_555 1_555 no C(3) C(2) H(2) 108.3(8) 1_555 1_555 1_555 no H(1) C(2) H(2) 109.7(9) 1_555 1_555 1_555 no C(2) C(3) C(4) 121.9(8) 1_555 1_555 1_555 yes C(2) C(3) C(42) 120.4(8) 1_555 1_555 1_555 yes C(4) C(3) C(42) 117.7(8) 1_555 1_555 1_555 yes C(3) C(4) C(5) 121.7(9) 1_555 1_555 1_555 yes C(3) C(4) H(3) 119(1) 1_555 1_555 1_555 no C(5) C(4) H(3) 119(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 118.9(9) 1_555 1_555 1_555 yes C(4) C(5) H(4) 120(1) 1_555 1_555 1_555 no C(6) C(5) H(4) 120.6(10) 1_555 1_555 1_555 no C(5) C(6) C(7) 122.7(9) 1_555 1_555 1_555 yes C(5) C(6) H(5) 118.4(9) 1_555 1_555 1_555 no C(7) C(6) H(5) 118.8(9) 1_555 1_555 1_555 no C(6) C(7) C(8) 120.9(8) 1_555 1_555 1_555 yes C(6) C(7) C(42) 117.8(8) 1_555 1_555 1_555 yes C(8) C(7) C(42) 121.3(8) 1_555 1_555 1_555 yes C(7) C(8) C(9) 116.0(7) 1_555 1_555 1_555 yes C(7) C(8) H(6) 108.1(8) 1_555 1_555 1_555 no C(7) C(8) H(7) 107.9(7) 1_555 1_555 1_555 no C(9) C(8) H(6) 107.9(7) 1_555 1_555 1_555 no C(9) C(8) H(7) 107.5(8) 1_555 1_555 1_555 no H(6) C(8) H(7) 109.3(8) 1_555 1_555 1_555 no C(8) C(9) C(10) 119.7(8) 1_555 1_555 1_555 yes C(8) C(9) C(41) 121.8(8) 1_555 1_555 1_555 yes C(10) C(9) C(41) 118.5(8) 1_555 1_555 1_555 yes C(9) C(10) C(11) 119.7(8) 1_555 1_555 1_555 yes C(9) C(10) H(8) 120.0(10) 1_555 1_555 1_555 no C(11) C(10) H(8) 120.4(8) 1_555 1_555 1_555 no C(10) C(11) C(12) 120.3(8) 1_555 1_555 1_555 yes C(10) C(11) H(9) 119(1) 1_555 1_555 1_555 no C(12) C(11) H(9) 120(1) 1_555 1_555 1_555 no C(11) C(12) C(13) 121.9(9) 1_555 1_555 1_555 yes C(11) C(12) H(10) 118.6(9) 1_555 1_555 1_555 no C(13) C(12) H(10) 119.5(9) 1_555 1_555 1_555 no C(12) C(13) C(14) 122.1(8) 1_555 1_555 1_555 yes C(12) C(13) C(41) 116.4(8) 1_555 1_555 1_555 yes C(14) C(13) C(41) 121.4(7) 1_555 1_555 1_555 yes C(13) C(14) C(15) 116.3(7) 1_555 1_555 1_555 yes C(13) C(14) H(11) 107.7(8) 1_555 1_555 1_555 no C(13) C(14) H(12) 107.9(8) 1_555 1_555 1_555 no C(15) C(14) H(11) 107.6(8) 1_555 1_555 1_555 no C(15) C(14) H(12) 107.8(8) 1_555 1_555 1_555 no H(11) C(14) H(12) 109.5(8) 1_555 1_555 1_555 no C(14) C(15) C(16) 121.3(8) 1_555 1_555 1_555 yes C(14) C(15) C(40) 122.3(7) 1_555 1_555 1_555 yes C(16) C(15) C(40) 116.4(8) 1_555 1_555 1_555 yes C(15) C(16) C(17) 121.7(8) 1_555 1_555 1_555 yes C(15) C(16) H(13) 118.9(10) 1_555 1_555 1_555 no C(17) C(16) H(13) 119.3(9) 1_555 1_555 1_555 no C(16) C(17) C(18) 120.0(8) 1_555 1_555 1_555 yes C(16) C(17) H(14) 119(1) 1_555 1_555 1_555 no C(18) C(17) H(14) 120(1) 1_555 1_555 1_555 no C(17) C(18) C(19) 121.7(9) 1_555 1_555 1_555 yes C(17) C(18) H(15) 119.1(9) 1_555 1_555 1_555 no C(19) C(18) H(15) 119(1) 1_555 1_555 1_555 no C(18) C(19) C(20) 121.6(8) 1_555 1_555 1_555 yes C(18) C(19) C(40) 117.0(8) 1_555 1_555 1_555 yes C(20) C(19) C(40) 121.4(8) 1_555 1_555 1_555 yes C(19) C(20) C(21) 115.6(7) 1_555 1_555 1_555 yes C(19) C(20) H(16) 107.7(8) 1_555 1_555 1_555 no C(19) C(20) H(17) 108.1(8) 1_555 1_555 1_555 no C(21) C(20) H(16) 107.9(8) 1_555 1_555 1_555 no C(21) C(20) H(17) 108.1(8) 1_555 1_555 1_555 no H(16) C(20) H(17) 109.3(9) 1_555 1_555 1_555 no C(20) C(21) C(22) 120.1(9) 1_555 1_555 1_555 yes C(20) C(21) C(39) 121.7(8) 1_555 1_555 1_555 yes C(22) C(21) C(39) 118.2(8) 1_555 1_555 1_555 yes C(21) C(22) C(23) 122.4(10) 1_555 1_555 1_555 yes C(21) C(22) H(18) 118.8(10) 1_555 1_555 1_555 no C(23) C(22) H(18) 118(1) 1_555 1_555 1_555 no C(22) C(23) C(24) 117.2(10) 1_555 1_555 1_555 yes C(22) C(23) H(19) 121(1) 1_555 1_555 1_555 no C(24) C(23) H(19) 121(1) 1_555 1_555 1_555 no C(23) C(24) C(25) 123.1(9) 1_555 1_555 1_555 yes C(23) C(24) H(20) 118(1) 1_555 1_555 1_555 no C(25) C(24) H(20) 118(1) 1_555 1_555 1_555 no C(24) C(25) C(26) 121.2(8) 1_555 1_555 1_555 yes C(24) C(25) C(39) 118.7(9) 1_555 1_555 1_555 yes C(26) C(25) C(39) 120.0(9) 1_555 1_555 1_555 yes C(25) C(26) C(27) 114.6(8) 1_555 1_555 1_555 yes C(25) C(26) H(21) 107.8(8) 1_555 1_555 1_555 no C(25) C(26) H(22) 108.0(9) 1_555 1_555 1_555 no C(27) C(26) H(21) 108.4(9) 1_555 1_555 1_555 no C(27) C(26) H(22) 108.2(8) 1_555 1_555 1_555 no H(21) C(26) H(22) 109.7(10) 1_555 1_555 1_555 no C(26) C(27) C(28) 121.4(9) 1_555 1_555 1_555 yes C(26) C(27) C(38) 121.2(8) 1_555 1_555 1_555 yes C(28) C(27) C(38) 117.4(9) 1_555 1_555 1_555 yes C(27) C(28) C(29) 121.9(9) 1_555 1_555 1_555 yes C(27) C(28) H(23) 119(1) 1_555 1_555 1_555 no C(29) C(28) H(23) 118.3(10) 1_555 1_555 1_555 no C(28) C(29) C(30) 119.2(8) 1_555 1_555 1_555 yes C(28) C(29) H(24) 120(1) 1_555 1_555 1_555 no C(30) C(29) H(24) 120(1) 1_555 1_555 1_555 no C(29) C(30) C(31) 120.2(9) 1_555 1_555 1_555 yes C(29) C(30) H(25) 120.0(10) 1_555 1_555 1_555 no C(31) C(30) H(25) 119(1) 1_555 1_555 1_555 no C(30) C(31) C(32) 119.7(8) 1_555 1_555 1_555 yes C(30) C(31) C(38) 118.1(9) 1_555 1_555 1_555 yes C(32) C(31) C(38) 122.1(7) 1_555 1_555 1_555 yes C(31) C(32) C(33) 116.1(7) 1_555 1_555 1_555 yes C(31) C(32) H(26) 108.5(9) 1_555 1_555 1_555 no C(31) C(32) H(27) 108.0(8) 1_555 1_555 1_555 no C(33) C(32) H(26) 107.5(8) 1_555 1_555 1_555 no C(33) C(32) H(27) 107.1(8) 1_555 1_555 1_555 no H(26) C(32) H(27) 109.5(9) 1_555 1_555 1_555 no C(32) C(33) C(34) 121.5(8) 1_555 1_555 1_555 yes C(32) C(33) C(37) 122.4(7) 1_555 1_555 1_555 yes C(34) C(33) C(37) 116.0(9) 1_555 1_555 1_555 yes C(33) C(34) C(35) 122.2(9) 1_555 1_555 1_555 yes C(33) C(34) H(28) 118(1) 1_555 1_555 1_555 no C(35) C(34) H(28) 119(1) 1_555 1_555 1_555 no C(34) C(35) C(36) 119.7(9) 1_555 1_555 1_555 yes C(34) C(35) H(29) 119(1) 1_555 1_555 1_555 no C(36) C(35) H(29) 120(1) 1_555 1_555 1_555 no C(1) C(36) C(35) 121.8(10) 1_555 1_555 1_555 yes C(1) C(36) H(30) 119(1) 1_555 1_555 1_555 no C(35) C(36) H(30) 118.7(10) 1_555 1_555 1_555 no O(1) C(37) C(1) 118.9(8) 1_555 1_555 1_555 yes O(1) C(37) C(33) 118.0(8) 1_555 1_555 1_555 yes C(1) C(37) C(33) 123.1(8) 1_555 1_555 1_555 yes O(2) C(38) C(27) 118.5(8) 1_555 1_555 1_555 yes O(2) C(38) C(31) 118.3(8) 1_555 1_555 1_555 yes C(27) C(38) C(31) 123.1(8) 1_555 1_555 1_555 yes O(3) C(39) C(21) 119.8(8) 1_555 1_555 1_555 yes O(3) C(39) C(25) 119.9(8) 1_555 1_555 1_555 yes C(21) C(39) C(25) 120.2(9) 1_555 1_555 1_555 yes O(4) C(40) C(15) 118.1(7) 1_555 1_555 1_555 yes O(4) C(40) C(19) 118.7(7) 1_555 1_555 1_555 yes C(15) C(40) C(19) 123.1(8) 1_555 1_555 1_555 yes O(5) C(41) C(9) 118.7(7) 1_555 1_555 1_555 yes O(5) C(41) C(13) 118.1(7) 1_555 1_555 1_555 yes C(9) C(41) C(13) 123.2(8) 1_555 1_555 1_555 yes O(6) C(42) C(3) 118.9(7) 1_555 1_555 1_555 yes O(6) C(42) C(7) 120.1(7) 1_555 1_555 1_555 yes C(3) C(42) C(7) 121.0(8) 1_555 1_555 1_555 yes S(1) C(43) F(1) 141(3) 1_555 1_555 1_555 yes S(1) C(43) F(2) 114(2) 1_555 1_555 1_555 yes F(1) C(43) F(2) 95(2) 1_555 1_555 1_555 yes C(45) C(44) C(49) 120(1) 1_555 1_555 1_555 yes C(45) C(44) H(37) 118(1) 1_555 1_555 1_555 no C(49) C(44) H(37) 120(1) 1_555 1_555 1_555 no C(44) C(45) C(46) 119(1) 1_555 1_555 1_555 yes C(44) C(45) H(38) 120(1) 1_555 1_555 1_555 no C(46) C(45) H(38) 119(1) 1_555 1_555 1_555 no C(45) C(46) C(47) 122(1) 1_555 1_555 1_555 yes C(45) C(46) H(39) 118(1) 1_555 1_555 1_555 no C(47) C(46) H(39) 118(1) 1_555 1_555 1_555 no C(46) C(47) C(48) 118(1) 1_555 1_555 1_555 yes C(46) C(47) H(40) 120(1) 1_555 1_555 1_555 no C(48) C(47) H(40) 120(1) 1_555 1_555 1_555 no C(47) C(48) C(49) 119(1) 1_555 1_555 1_555 yes C(47) C(48) H(41) 119(1) 1_555 1_555 1_555 no C(49) C(48) H(41) 121(1) 1_555 1_555 1_555 no C(44) C(49) C(48) 118(1) 1_555 1_555 1_555 yes C(44) C(49) H(42) 121(1) 1_555 1_555 1_555 no C(48) C(49) H(42) 120(1) 1_555 1_555 1_555 no C(51) C(50) C(55) 122(1) 1_555 1_555 1_555 yes C(51) C(50) H(43) 122(4) 1_555 1_555 1_555 no C(55) C(50) H(43) 114(4) 1_555 1_555 1_555 no C(50) C(51) C(52) 119(2) 1_555 1_555 1_555 yes C(50) C(51) H(44) 118(4) 1_555 1_555 1_555 no C(52) C(51) H(44) 122(3) 1_555 1_555 1_555 no C(51) C(52) C(53) 120(1) 1_555 1_555 1_555 yes C(51) C(52) H(45) 118(4) 1_555 1_555 1_555 no C(53) C(52) H(45) 120(4) 1_555 1_555 1_555 no C(52) C(53) C(54) 120(1) 1_555 1_555 1_555 yes C(52) C(53) H(46) 118(4) 1_555 1_555 1_555 no C(54) C(53) H(46) 120(4) 1_555 1_555 1_555 no C(53) C(54) C(55) 119(1) 1_555 1_555 1_555 yes C(53) C(54) H(47) 120(3) 1_555 1_555 1_555 no C(55) C(54) H(47) 120(3) 1_555 1_555 1_555 no C(50) C(55) C(54) 117(1) 1_555 1_555 1_555 yes C(50) C(55) H(48) 122(3) 1_555 1_555 1_555 no C(54) C(55) H(48) 119(3) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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 #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #=END data_[ag2(calix4arene)(clo4)2] #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 28 09:53:49 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 419.57 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H12 Ag Cl O6 ' _chemical_formula_moiety 'C14 H12 Ag Cl O6 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 19.488(6) _cell_length_b 13.359(3) _cell_length_c 10.547(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2745(1) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.6 _cell_measurement_theta_max 15.6 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,1/2-z -x,1/2+y,-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,1/2+z x,1/2-y,z 1/2+x,y,1/2-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664.00 _exptl_absorpt_coefficient_mu 1.686 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.38 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 2 2 -1 -3 2 -2 -2 2 _diffrn_reflns_number 3292 _reflns_number_total 3292 _reflns_number_gt 1636 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.092 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01150 _diffrn_orient_matrix_UB_12 -0.07287 _diffrn_orient_matrix_UB_13 -0.00441 _diffrn_orient_matrix_UB_21 -0.04992 _diffrn_orient_matrix_UB_22 0.01695 _diffrn_orient_matrix_UB_23 -0.00444 _diffrn_orient_matrix_UB_31 0.00288 _diffrn_orient_matrix_UB_32 0.00260 _diffrn_orient_matrix_UB_33 -0.09461 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'Ag' 'Ag' -0.897 1.101 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;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) ; '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) ; #------------------------------------------------------------------------------ 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 Ag1 Ag 0.63712(5) 0.08846(6) 0.63636(9) 0.0713(3) Uani 1.00 d . . . Cl1 Cl 0.7578(3) 0.2500 0.7206(5) 0.088(2) Uani 1.00 d S . . Cl2 Cl 0.5520(2) 0.2500 0.4410(4) 0.071(1) Uani 1.00 d S . . O1 O 0.5679(3) 0.1510(5) 1.1050(5) 0.047(2) Uani 1.00 d . . . O2 O 0.6954(3) 0.1504(5) 1.1900(6) 0.051(2) Uani 1.00 d . . . O3 O 0.7295(6) 0.1589(9) 0.7661(10) 0.122(4) Uani 1.00 d . . . O4 O 0.760(1) 0.2500 0.585(1) 0.140(7) Uani 1.00 d S . . O5 O 0.8310(9) 0.2500 0.761(2) 0.126(6) Uani 1.00 d S . . O6 O 0.599(1) 0.2500 0.570(2) 0.062(7) Uani 0.55 d SP . . O7 O 0.5249(7) 0.3374(10) 0.468(1) 0.175(6) Uani 1.00 d . . . O8 O 0.6050(7) 0.2500 0.361(1) 0.107(5) Uani 1.00 d S . . O9 O 0.492(1) 0.2500 0.324(2) 0.07(1) Uani 0.41 d SP . . C1 C 0.5399(6) 0.0194(9) 0.7560(9) 0.063(3) Uani 1.00 d . . . C2 C 0.5048(5) 0.1093(7) 0.785(1) 0.052(3) Uani 1.00 d . . . C3 C 0.5164(5) 0.1546(7) 0.9022(8) 0.042(3) Uani 1.00 d . . . C4 C 0.5614(5) 0.1108(6) 0.9857(9) 0.043(3) Uani 1.00 d . . . C5 C 0.6002(5) 0.0248(6) 0.9573(8) 0.042(3) Uani 1.00 d . . . C6 C 0.5863(6) -0.0196(7) 0.8406(10) 0.054(3) Uani 1.00 d . . . C7 C 0.4771(7) 0.2500 0.933(1) 0.047(4) Uani 1.00 d S . . C8 C 0.6497(5) -0.0209(7) 1.0470(9) 0.051(3) Uani 1.00 d . . . C9 C 0.7229(5) 0.0270(7) 1.0410(8) 0.043(3) Uani 1.00 d . . . C10 C 0.7406(5) 0.1097 1.1066(8) -0.003(2) Uani 0.50 d P . . C11 C 0.8039(5) 0.1543(7) 1.0936(8) 0.047(3) Uani 1.00 d . . . C12 C 0.8510(5) 0.1084(8) 1.0138(10) 0.055(3) Uani 1.00 d . . . C13 C 0.8363(6) 0.0237(9) 0.9478(9) 0.057(3) Uani 1.00 d . . . C14 C 0.7709(6) -0.0181(7) 0.9621(9) 0.053(3) Uani 1.00 d . . . C15 C 0.8224(7) 0.2500 1.162(1) 0.053(4) Uani 1.00 d S . . H1 H 0.5312 -0.0155 0.6769 0.0748 Uiso 1.00 calc . . . H2 H 0.4733 0.1396 0.7251 0.0633 Uiso 1.00 calc . . . H3 H 0.6111 -0.0796 0.8180 0.0650 Uiso 1.00 calc . . . H4 H 0.4346 0.2500 0.8876 0.0584 Uiso 1.00 calc S . . H5 H 0.4666 0.2500 1.0223 0.0584 Uiso 1.00 calc S . . H6 H 0.6317 -0.0124 1.1314 0.0593 Uiso 1.00 calc . . . H7 H 0.6526 -0.0908 1.0300 0.0593 Uiso 1.00 calc . . . H8 H 0.8965 0.1373 1.0048 0.0667 Uiso 1.00 calc . . . H9 H 0.8698 -0.0070 0.8918 0.0710 Uiso 1.00 calc . . . H10 H 0.7592 -0.0795 0.9154 0.0622 Uiso 1.00 calc . . . H11 H 0.7997 0.2500 1.2431 0.0641 Uiso 1.00 calc S . . H12 H 0.8713 0.2500 1.1789 0.0641 Uiso 1.00 calc S . . H13 H 0.5727 0.1792 1.1881 0.0558 Uiso 1.00 calc . . . H14 H 0.6634 0.1789 1.2497 0.0614 Uiso 1.00 calc . . . 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 Ag1 0.0833(7) 0.0524(5) 0.0783(7) 0.0049(5) 0.0217(5) -0.0031(5) Cl1 0.146(5) 0.053(2) 0.064(3) 0.0000 -0.028(3) 0.0000 Cl2 0.071(3) 0.051(2) 0.090(3) 0.0000 0.043(2) 0.0000 O1 0.059(4) 0.053(4) 0.030(3) -0.001(3) 0.009(3) -0.007(3) O2 0.060(4) 0.053(4) 0.040(3) 0.007(4) 0.007(3) 0.002(3) O3 0.127(9) 0.132(9) 0.109(8) -0.048(7) -0.039(7) 0.056(8) O4 0.26(2) 0.08(1) 0.082(10) 0.0000 -0.04(1) 0.0000 O5 0.09(1) 0.16(2) 0.12(1) 0.0000 0.01(1) 0.0000 O6 0.08(2) 0.05(1) 0.05(1) 0.0000 -0.03(1) 0.0000 O7 0.17(1) 0.16(1) 0.20(1) 0.11(1) -0.05(1) -0.08(1) O8 0.087(9) 0.16(1) 0.074(8) 0.0000 0.047(7) 0.0000 O9 0.05(2) 0.10(2) 0.05(2) 0.0000 0.00(1) 0.0000 C1 0.086(8) 0.064(7) 0.039(6) -0.032(7) 0.011(6) -0.009(5) C2 0.056(6) 0.046(6) 0.053(6) -0.011(5) 0.010(5) 0.004(5) C3 0.039(5) 0.045(5) 0.043(5) -0.011(4) 0.002(4) -0.001(4) C4 0.042(5) 0.039(5) 0.049(5) -0.010(4) 0.012(4) -0.001(4) C5 0.049(6) 0.034(4) 0.043(5) -0.005(4) 0.012(4) 0.008(4) C6 0.064(7) 0.041(5) 0.056(6) -0.014(5) 0.019(5) -0.011(5) C7 0.029(7) 0.062(9) 0.051(8) 0.0000 0.002(6) 0.0000 C8 0.059(7) 0.036(5) 0.057(6) -0.004(5) 0.009(5) 0.003(5) C9 0.046(6) 0.043(5) 0.040(5) 0.009(4) 0.009(4) 0.019(4) C10 0.000(5) 0.000(4) -0.009(4) 0.0119 0.001(3) 0.0129 C11 0.060(6) 0.045(5) 0.035(5) 0.010(5) -0.012(4) 0.007(4) C12 0.045(6) 0.066(7) 0.053(6) 0.008(5) -0.014(5) 0.011(5) C13 0.054(6) 0.072(7) 0.045(6) 0.018(6) -0.003(5) 0.013(6) C14 0.073(8) 0.040(5) 0.045(5) 0.009(5) 0.002(5) 0.005(5) C15 0.031(8) 0.071(10) 0.056(9) 0.0000 -0.010(6) 0.0000 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _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) + 0.00090|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1636 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.948 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.79 _refine_diff_density_max 1.46 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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 Ag(1) O(3) 2.460(9) 1_555 1_555 yes Ag(1) O(6) 2.383(6) 1_555 1_555 yes Ag(1) C(1) 2.457(9) 1_555 1_555 yes Cl(1) O(3) 1.404(9) 1_555 1_555 yes Cl(1) O(3) 1.404(9) 1_555 7_555 yes Cl(1) O(4) 1.41(1) 1_555 1_555 yes Cl(1) O(5) 1.48(1) 1_555 1_555 yes Cl(2) O(6) 1.65(1) 1_555 1_555 yes Cl(2) O(7) 1.322(9) 1_555 1_555 yes Cl(2) O(7) 1.322(9) 1_555 7_555 yes Cl(2) O(8) 1.33(1) 1_555 1_555 yes Cl(2) O(9) 1.73(2) 1_555 1_555 yes O(1) C(4) 1.359(8) 1_555 1_555 yes O(2) C(10) 1.360(9) 1_555 1_555 yes C(1) C(2) 1.41(1) 1_555 1_555 yes C(1) C(6) 1.40(1) 1_555 1_555 yes C(2) C(3) 1.39(1) 1_555 1_555 yes C(3) C(4) 1.39(1) 1_555 1_555 yes C(3) C(7) 1.53(1) 1_555 1_555 yes C(4) C(5) 1.42(1) 1_555 1_555 yes C(5) C(6) 1.40(1) 1_555 1_555 yes C(5) C(8) 1.47(1) 1_555 1_555 yes C(8) C(9) 1.55(1) 1_555 1_555 yes C(9) C(10) 1.383(9) 1_555 1_555 yes C(9) C(14) 1.39(1) 1_555 1_555 yes C(10) C(11) 1.41(1) 1_555 1_555 yes C(11) C(12) 1.39(1) 1_555 1_555 yes C(11) C(15) 1.492(10) 1_555 1_555 yes C(12) C(13) 1.37(1) 1_555 1_555 yes C(13) C(14) 1.39(1) 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 Ag(1) C(13) 2.542(8) 1_555 4_654 ? Ag(1) C(14) 2.731(9) 1_555 4_654 ? Ag(1) C(12) 2.939(9) 1_555 4_654 ? Ag(1) C(9) 3.291(8) 1_555 4_654 ? Ag(1) C(11) 3.480(8) 1_555 4_654 ? Ag(1) C(10) 3.577(6) 1_555 4_654 ? O(1) O(9) 3.04(2) 1_555 1_556 ? O(1) O(8) 3.09(1) 1_555 1_556 ? O(1) C(1) 3.428(10) 1_555 5_657 ? O(1) C(6) 3.54(1) 1_555 5_657 ? O(2) O(8) 2.84(1) 1_555 1_556 ? O(2) C(14) 3.419(10) 1_555 4_655 ? O(3) C(9) 3.58(1) 1_555 4_654 ? O(4) C(14) 3.409(10) 1_555 4_654 ? O(4) C(14) 3.409(10) 1_555 6_654 ? O(4) C(8) 3.55(1) 1_555 4_654 ? O(4) C(8) 3.55(1) 1_555 6_654 ? O(5) C(7) 3.51(2) 1_555 2_556 ? O(7) C(12) 3.45(1) 1_555 2_456 ? O(9) C(15) 3.28(2) 1_555 2_456 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ;