# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1513 data_wtwong654-Lau082 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Feb 5 18:09:34 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Marresearch Imate Plate' _computing_cell_refinement 'Marresearch Imate Plate' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 20.781(1) _cell_length_b 9.115(1) _cell_length_c 22.989(1) _cell_angle_alpha 90.00(2) _cell_angle_beta 109.62(2) _cell_angle_gamma 90.00(2) _cell_volume 4101.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.260 _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_meas ? _chemical_formula_weight 1065.25 _chemical_formula_analytical ? _chemical_formula_sum 'C37 H35 Cl3 O11 Ru3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2112.00 _exptl_absorpt_coefficient_mu 1.342 _exptl_absorpt_correction_type 'interimage scaling' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 1.000 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'image plate' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 35652 _reflns_number_total 6775 _reflns_number_observed 3076 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 25.52 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 12 -1.259 0.836 'International Tables' C 0 148 0.003 0.002 'International Tables' O 0 44 0.011 0.006 'International Tables' H 0 140 0.000 0.000 'International Tables' Cl 0 12 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.76132(4) -0.01970(9) 0.05833(4) 0.0496(3) Uij ? ? Ru(2) 0.79898(5) 0.0630(1) -0.04445(4) 0.0561(3) Uij ? ? Ru(3) 0.88065(4) 0.14120(10) 0.08277(4) 0.0516(3) Uij ? ? Cl(1) 0.1916(3) 0.1155(9) 0.2513(3) 0.195(3) Uij ? ? Cl(2) 0.0694(3) 0.173(1) 0.2745(4) 0.251(4) Uij ? ? Cl(3) 0.1363(6) -0.1016(8) 0.3053(4) 0.263(4) Uij ? ? O(1) 0.6192(5) -0.1330(9) 0.0377(4) 0.087(3) Uij ? ? O(2) 0.8189(5) -0.2941(10) 0.1302(4) 0.088(3) Uij ? ? O(3) 0.7724(7) -0.260(1) -0.0271(5) 0.130(5) Uij ? ? O(4) 0.8955(5) -0.096(1) -0.0946(4) 0.101(4) Uij ? ? O(5) 0.6860(5) 0.011(1) -0.1635(5) 0.124(4) Uij ? ? O(6) 0.9785(6) -0.111(1) 0.1441(5) 0.118(4) Uij ? ? O(7) 0.9714(4) 0.197(1) 0.0040(4) 0.100(3) Uij ? ? O(8) 0.9378(5) 0.411(1) 0.1585(5) 0.112(4) Uij ? ? O(9) 0.7052(4) 0.3486(7) -0.0518(3) 0.055(2) Uij ? ? O(10) 0.5533(4) 0.3643(8) 0.1560(3) 0.068(3) Uij ? ? O(11) 0.8978(3) 0.0091(8) 0.2243(3) 0.061(2) Uij ? ? C(1) 0.6727(7) -0.089(1) 0.0435(5) 0.061(4) Uij ? ? C(2) 0.7979(6) -0.189(1) 0.1044(5) 0.059(4) Uij ? ? C(3) 0.7751(7) -0.135(2) -0.0134(6) 0.082(5) Uij ? ? C(4) 0.8583(7) -0.038(1) -0.0758(5) 0.074(4) Uij ? ? C(5) 0.7278(7) 0.034(2) -0.1175(6) 0.076(5) Uij ? ? C(6) 0.9423(7) -0.016(2) 0.1250(6) 0.075(5) Uij ? ? C(7) 0.9350(6) 0.170(1) 0.0295(5) 0.060(3) Uij ? ? C(8) 0.9189(6) 0.308(2) 0.1315(6) 0.070(5) Uij ? ? C(9) 0.8413(6) 0.358(1) -0.1066(5) 0.060(4) Uij ? ? C(10) 0.8737(6) 0.292(1) -0.1484(6) 0.072(4) Uij ? ? C(11) 0.9068(9) 0.416(2) -0.1711(8) 0.116(7) Uij ? ? C(12) 0.907(1) 0.541(2) -0.133(1) 0.17(1) Uij ? ? C(13) 0.8552(7) 0.520(1) -0.1040(6) 0.084(5) Uij ? ? C(14) 0.8088(6) 0.290(1) -0.0738(5) 0.056(4) Uij ? ? C(15) 0.7732(6) 0.304(1) -0.0324(5) 0.050(4) Uij ? ? C(16) 0.7944(5) 0.239(1) 0.0256(4) 0.046(3) Uij ? ? C(17) 0.7363(5) 0.236(1) 0.0454(5) 0.045(3) Uij ? ? C(18) 0.6784(5) 0.316(1) -0.0001(5) 0.051(4) Uij ? ? C(19) 0.6092(6) 0.246(1) -0.0291(5) 0.060(4) Uij ? ? C(20) 0.5583(7) 0.369(2) -0.0508(7) 0.095(5) Uij ? ? C(21) 0.5909(9) 0.501(2) -0.016(1) 0.156(8) Uij ? ? C(22) 0.6621(6) 0.469(1) 0.0218(5) 0.063(4) Uij ? ? C(23) 0.7459(5) 0.188(1) 0.1068(5) 0.044(3) Uij ? ? C(24) 0.6898(6) 0.202(1) 0.1298(4) 0.050(4) Uij ? ? C(25) 0.6389(6) 0.212(1) 0.1421(5) 0.050(4) Uij ? ? C(26) 0.5735(5) 0.216(1) 0.1540(4) 0.049(4) Uij ? ? C(27) 0.5160(6) 0.141(1) 0.1020(5) 0.071(4) Uij ? ? C(28) 0.4620(7) 0.111(2) 0.1301(7) 0.101(6) Uij ? ? C(29) 0.4994(8) 0.094(2) 0.1995(8) 0.124(7) Uij ? ? C(30) 0.5739(6) 0.136(1) 0.2118(5) 0.074(4) Uij ? ? C(31) 0.8348(5) 0.090(1) 0.2055(4) 0.049(3) Uij ? ? C(32) 0.8447(6) 0.233(1) 0.2432(5) 0.062(4) Uij ? ? C(33) 0.8405(7) 0.181(1) 0.3051(5) 0.075(4) Uij ? ? C(34) 0.7816(7) 0.075(1) 0.2860(5) 0.073(4) Uij ? ? C(35) 0.7859(5) 0.000(1) 0.2281(4) 0.053(3) Uij ? ? C(36) 0.8115(5) 0.1222(10) 0.1369(4) 0.042(3) Uij ? ? C(37) 0.1459 0.0810 0.3021 0.1242 Uij ? ? H(17) 0.5168 0.4174 0.1567 0.0975 Uij ? ? H(18) 0.9376 -0.0226 0.2220 0.0975 Uij ? ? H(19) 0.9072 0.2216 -0.1276 0.0866 Uij ? ? H(20) 0.8399 0.2468 -0.1822 0.0866 Uij ? ? H(21) 0.9521 0.3906 -0.1677 0.1386 Uij ? ? H(22) 0.8813 0.4376 -0.2130 0.1386 Uij ? ? H(23) 0.9508 0.5495 -0.1022 0.2084 Uij ? ? H(24) 0.8975 0.6267 -0.1579 0.2084 Uij ? ? H(25) 0.8145 0.5718 -0.1265 0.0991 Uij ? ? H(26) 0.8713 0.5555 -0.0627 0.0991 Uij ? ? H(27) 0.6092 0.1861 -0.0632 0.0729 Uij ? ? H(28) 0.5983 0.1868 0.0004 0.0729 Uij ? ? H(29) 0.5478 0.3853 -0.0939 0.1150 Uij ? ? H(30) 0.5174 0.3468 -0.0427 0.1150 Uij ? ? H(31) 0.5906 0.5793 -0.0436 0.1850 Uij ? ? H(32) 0.5667 0.5320 0.0107 0.1850 Uij ? ? H(33) 0.6668 0.4653 0.0644 0.0753 Uij ? ? H(34) 0.6920 0.5411 0.0155 0.0753 Uij ? ? H(35) 0.4991 0.2051 0.0674 0.0859 Uij ? ? H(36) 0.5315 0.0528 0.0893 0.0859 Uij ? ? H(37) 0.4304 0.1901 0.1223 0.1202 Uij ? ? H(38) 0.4382 0.0230 0.1136 0.1202 Uij ? ? H(39) 0.4801 0.1581 0.2220 0.1485 Uij ? ? H(40) 0.4968 -0.0040 0.2121 0.1485 Uij ? ? H(41) 0.6021 0.0507 0.2186 0.0884 Uij ? ? H(42) 0.5904 0.1983 0.2471 0.0884 Uij ? ? H(43) 0.8878 0.2756 0.2485 0.0745 Uij ? ? H(44) 0.8095 0.3010 0.2241 0.0745 Uij ? ? H(45) 0.8814 0.1334 0.3290 0.0909 Uij ? ? H(46) 0.8314 0.2608 0.3278 0.0909 Uij ? ? H(47) 0.7857 0.0060 0.3177 0.0878 Uij ? ? H(48) 0.7395 0.1267 0.2769 0.0878 Uij ? ? H(49) 0.7421 -0.0033 0.1973 0.0633 Uij ? ? H(50) 0.8029 -0.0972 0.2379 0.0633 Uij ? ? H(51) 0.1713 0.1167 0.3421 0.1490 Uij ? ? 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 Ru(1) 0.0513(6) 0.0519(6) 0.0463(5) 0.0004(5) 0.0174(4) -0.0014(4) Ru(2) 0.0594(7) 0.0645(7) 0.0477(5) 0.0035(5) 0.0224(5) -0.0005(5) Ru(3) 0.0427(6) 0.0625(6) 0.0501(5) 0.0043(5) 0.0162(4) 0.0012(5) Cl(1) 0.176(6) 0.294(8) 0.123(4) -0.044(5) 0.058(4) -0.002(4) Cl(2) 0.135(5) 0.39(1) 0.201(7) 0.025(6) 0.018(5) -0.043(7) Cl(3) 0.43(1) 0.176(6) 0.203(7) -0.121(7) 0.139(8) -0.037(5) O(1) 0.072(7) 0.093(7) 0.093(7) -0.024(5) 0.023(5) -0.002(5) O(2) 0.116(8) 0.063(6) 0.073(6) 0.017(5) 0.016(5) 0.012(5) O(3) 0.24(1) 0.076(7) 0.131(9) -0.010(8) 0.132(9) -0.010(7) O(4) 0.101(8) 0.109(8) 0.100(7) 0.032(6) 0.045(6) -0.014(6) O(5) 0.097(8) 0.17(1) 0.084(7) -0.028(7) -0.001(6) -0.027(7) O(6) 0.102(8) 0.149(10) 0.114(8) 0.065(7) 0.048(7) 0.037(7) O(7) 0.069(6) 0.167(9) 0.077(6) -0.002(6) 0.042(5) 0.011(6) O(8) 0.117(8) 0.106(8) 0.124(8) -0.055(7) 0.056(7) -0.043(7) O(9) 0.051(5) 0.069(5) 0.048(4) 0.015(4) 0.019(4) 0.015(4) O(10) 0.053(5) 0.061(5) 0.090(6) 0.015(4) 0.021(4) -0.002(4) O(11) 0.039(4) 0.078(5) 0.062(5) 0.023(4) 0.010(4) 0.014(4) C(1) 0.059(9) 0.067(8) 0.062(7) -0.006(7) 0.026(7) 0.010(6) C(2) 0.068(9) 0.060(8) 0.050(7) 0.011(7) 0.019(6) 0.015(7) C(3) 0.13(1) 0.050(8) 0.085(9) -0.009(8) 0.056(9) -0.014(8) C(4) 0.085(10) 0.076(9) 0.063(8) 0.027(8) 0.030(7) 0.007(7) C(5) 0.077(10) 0.11(1) 0.039(7) -0.009(8) 0.018(7) -0.004(7) C(6) 0.065(9) 0.09(1) 0.071(8) 0.026(8) 0.029(7) 0.021(8) C(8) 0.060(9) 0.072(9) 0.082(9) -0.022(7) 0.027(7) -0.019(8) C(9) 0.074(8) 0.052(8) 0.062(7) 0.013(6) 0.035(7) 0.006(6) C(10) 0.087(10) 0.065(8) 0.085(9) 0.000(7) 0.055(8) 0.005(7) C(11) 0.17(2) 0.08(1) 0.15(1) -0.01(1) 0.12(1) 0.01(1) C(12) 0.27(3) 0.09(1) 0.26(2) -0.03(1) 0.22(2) -0.03(1) C(13) 0.11(1) 0.061(9) 0.098(10) 0.010(8) 0.064(9) -0.004(8) C(14) 0.057(8) 0.063(8) 0.047(7) 0.009(6) 0.014(6) 0.008(6) C(15) 0.052(8) 0.051(7) 0.052(7) 0.001(6) 0.024(6) -0.001(6) C(16) 0.050(7) 0.060(7) 0.035(6) 0.002(5) 0.022(5) 0.013(5) C(17) 0.037(7) 0.045(7) 0.048(7) -0.002(5) 0.010(6) -0.008(5) C(18) 0.048(8) 0.060(7) 0.049(7) 0.006(6) 0.020(6) 0.008(6) C(19) 0.049(8) 0.064(8) 0.065(7) 0.006(7) 0.015(6) 0.006(6) C(20) 0.059(9) 0.11(1) 0.11(1) 0.019(9) 0.017(8) 0.013(10) C(21) 0.08(1) 0.12(1) 0.22(2) 0.04(1) -0.01(1) -0.05(1) C(22) 0.078(9) 0.053(8) 0.066(7) 0.016(6) 0.036(7) 0.007(6) C(23) 0.034(7) 0.052(7) 0.046(7) 0.013(5) 0.013(6) 0.000(5) C(24) 0.050(8) 0.053(7) 0.041(6) 0.005(6) 0.009(6) -0.003(5) C(25) 0.049(8) 0.054(7) 0.049(7) 0.007(6) 0.016(6) -0.003(5) C(26) 0.048(7) 0.060(8) 0.038(6) -0.003(6) 0.014(5) -0.009(6) C(27) 0.057(8) 0.077(8) 0.083(8) -0.016(7) 0.030(7) -0.023(7) C(28) 0.068(10) 0.13(1) 0.10(1) -0.031(9) 0.033(9) -0.037(10) C(29) 0.08(1) 0.17(2) 0.13(1) -0.02(1) 0.04(1) 0.05(1) C(30) 0.066(9) 0.091(9) 0.074(8) 0.008(7) 0.034(7) 0.011(7) C(31) 0.055(8) 0.053(7) 0.040(6) 0.001(6) 0.016(5) 0.006(6) C(32) 0.068(8) 0.062(8) 0.045(7) -0.007(6) 0.005(6) -0.010(6) C(33) 0.09(1) 0.086(9) 0.040(7) 0.021(8) 0.010(7) -0.016(7) C(34) 0.09(1) 0.069(8) 0.064(8) -0.004(8) 0.035(7) -0.002(7) C(35) 0.066(8) 0.055(7) 0.039(6) 0.010(6) 0.019(5) 0.004(5) C(36) 0.047(7) 0.032(6) 0.047(6) -0.004(5) 0.014(5) 0.001(5) C(37) 0.1199 0.1568 0.0939 -0.0228 0.0332 -0.0148 #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 3076 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0440 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0483 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.592 _refine_ls_shift/esd_max 0.0240 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.74 _refine_diff_density_max 0.48 #------------------------------------------------------------------------------ _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 Ru(1) Ru(2) 2.829(1) ? ? yes Ru(1) Ru(3) 2.772(1) ? ? yes Ru(1) C(1) 1.87(1) ? ? yes Ru(1) C(2) 1.88(1) ? ? yes Ru(1) C(3) 2.06(2) ? ? yes Ru(1) C(17) 2.382(10) ? ? yes Ru(1) C(23) 2.27(1) ? ? yes Ru(1) C(36) 2.181(9) ? ? yes Ru(2) Ru(3) 2.934(1) ? ? yes Ru(2) C(3) 2.07(1) ? ? yes Ru(2) C(4) 1.87(2) ? ? yes Ru(2) C(5) 1.85(1) ? ? yes Ru(2) C(14) 2.20(1) ? ? yes Ru(2) C(15) 2.30(1) ? ? yes Ru(2) C(16) 2.30(1) ? ? yes Ru(3) C(6) 1.95(1) ? ? yes Ru(3) C(7) 1.94(1) ? ? yes Ru(3) C(8) 1.90(1) ? ? yes Ru(3) C(16) 2.036(9) ? ? yes Ru(3) C(36) 2.20(1) ? ? yes Cl(1) C(37) 1.764(7) ? ? yes Cl(2) C(37) 1.721(8) ? ? yes Cl(3) C(37) 1.681(8) ? ? yes O(1) C(1) 1.15(2) ? ? yes O(2) C(2) 1.14(1) ? ? yes O(3) C(3) 1.17(2) ? ? yes O(4) C(4) 1.13(2) ? ? yes O(5) C(5) 1.14(1) ? ? yes O(6) C(6) 1.13(2) ? ? yes O(7) C(7) 1.13(2) ? ? yes O(8) C(8) 1.12(2) ? ? yes O(9) C(15) 1.39(1) ? ? yes O(9) C(18) 1.50(1) ? ? yes O(10) C(26) 1.42(1) ? ? yes O(11) C(31) 1.44(1) ? ? yes C(9) C(10) 1.47(2) ? ? yes C(9) C(13) 1.51(2) ? ? yes C(9) C(14) 1.32(2) ? ? yes C(10) C(11) 1.50(2) ? ? yes C(11) C(12) 1.43(3) ? ? yes C(12) C(13) 1.46(3) ? ? yes C(14) C(15) 1.39(2) ? ? yes C(15) C(16) 1.39(1) ? ? yes C(16) C(17) 1.43(2) ? ? yes C(17) C(18) 1.50(1) ? ? yes C(17) C(23) 1.42(2) ? ? yes C(18) C(19) 1.51(1) ? ? yes C(18) C(22) 1.55(2) ? ? yes C(19) C(20) 1.51(2) ? ? yes C(20) C(21) 1.48(2) ? ? yes C(21) C(22) 1.47(2) ? ? yes #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_wtwong578-Lau064 #------------------------------------------------------------------------------ _audit_creation_date 'Wed May 5 11:35:25 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record 'SHELX86' #------------------------------------------------------------------------------ _computing_data_collection 'MARRESEARCH Image Plate' _computing_cell_refinement 'MARRESEARCH Image Plate' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.692(1) _cell_length_b 12.419(1) _cell_length_c 28.419(1) _cell_angle_alpha 90 _cell_angle_beta 97.65(2) _cell_angle_gamma 90 _cell_volume 4089.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.230 _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_meas ? _chemical_formula_weight 1033.05 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H49 O11 Ru3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2084.00 _exptl_absorpt_coefficient_mu 1.154 _exptl_absorpt_correction_type 'interimage scaling' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'MARRESEARCH Image Plate' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 29565 _reflns_number_total 4635 _reflns_number_observed 2630 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 12 -1.259 0.836 'International Tables' C 0 168 0.003 0.002 'International Tables' O 0 44 0.011 0.006 'International Tables' H 0 196 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) -0.03573(9) 0.65770(9) 0.10619(4) 0.0593(4) Uij ? ? Ru(2) 0.13380(9) 0.60150(8) 0.18120(4) 0.0503(4) Uij ? ? Ru(3) 0.07727(9) 0.81582(8) 0.16977(4) 0.0552(4) Uij ? ? O(1) -0.293(1) 0.6837(10) 0.0967(5) 0.118(5) Uij ? ? O(2) -0.054(1) 0.4548(10) 0.0510(4) 0.109(5) Uij ? ? O(3) -0.1129(8) 0.5431(9) 0.1912(4) 0.092(4) Uij ? ? O(4) 0.206(1) 0.3705(10) 0.1697(4) 0.115(5) Uij ? ? O(5) 0.112(1) 0.5576(9) 0.2813(4) 0.108(5) Uij ? ? O(6) 0.201(1) 1.0299(10) 0.1750(4) 0.130(5) Uij ? ? O(7) -0.021(1) 0.8245(9) 0.2618(5) 0.109(5) Uij ? ? O(8) -0.133(1) 0.9252(10) 0.1144(5) 0.115(5) Uij ? ? O(9) 0.1802(8) 0.6691(8) 0.0471(3) 0.072(3) Uij ? ? O(10) 0.4545(7) 0.5739(8) 0.1568(3) 0.090(4) Uij ? ? O(11) 0.3349(7) 0.9587(8) 0.3400(3) 0.071(3) Uij ? ? C(1) -0.198(1) 0.673(1) 0.0999(6) 0.086(6) Uij ? ? C(2) -0.049(1) 0.532(1) 0.0712(6) 0.072(6) Uij ? ? C(3) -0.043(1) 0.582(1) 0.1694(5) 0.067(5) Uij ? ? C(4) 0.175(1) 0.457(2) 0.1721(5) 0.077(6) Uij ? ? C(5) 0.120(1) 0.573(1) 0.2435(6) 0.076(6) Uij ? ? C(6) 0.153(1) 0.948(1) 0.1726(5) 0.075(6) Uij ? ? C(7) 0.013(1) 0.826(1) 0.2269(7) 0.076(6) Uij ? ? C(8) -0.059(1) 0.879(1) 0.1337(6) 0.072(6) Uij ? ? C(9) -0.002(1) 0.751(1) 0.0454(6) 0.070(6) Uij ? ? C(10) -0.053(1) 0.792(1) 0.0055(6) 0.075(6) Uij ? ? C(11) -0.181(2) 0.786(2) -0.0114(6) 0.108(7) Uij ? ? C(12) -0.170(4) 0.844(3) -0.063(2) 0.11(1) Uij ? ? C(13) -0.062(3) 0.850(3) -0.074(1) 0.094(10) Uij ? ? C(14) 0.013(2) 0.854(1) -0.0289(6) 0.096(6) Uij ? ? C(15) 0.109(1) 0.731(1) 0.0692(6) 0.066(6) Uij ? ? C(16) 0.146(1) 0.7401(10) 0.1171(5) 0.049(5) Uij ? ? C(17) 0.249(1) 0.677(1) 0.1286(5) 0.050(5) Uij ? ? C(18) 0.277(1) 0.631(1) 0.0815(5) 0.055(5) Uij ? ? C(19) 0.287(1) 0.512(1) 0.0758(5) 0.073(6) Uij ? ? C(20) 0.349(1) 0.500(1) 0.0315(6) 0.094(6) Uij ? ? C(21) 0.440(1) 0.586(2) 0.0401(5) 0.096(6) Uij ? ? C(22) 0.389(1) 0.677(1) 0.0656(5) 0.083(6) Uij ? ? C(23) 0.305(1) 0.686(1) 0.1743(5) 0.053(5) Uij ? ? C(24) 0.424(1) 0.643(1) 0.1930(5) 0.067(5) Uij ? ? C(25) 0.514(1) 0.737(1) 0.2020(6) 0.091(6) Uij ? ? C(26) 0.607(2) 0.692(2) 0.237(1) 0.15(1) Uij ? ? C(27) 0.560(2) 0.593(2) 0.2594(7) 0.134(9) Uij ? ? C(28) 0.436(1) 0.582(1) 0.2389(5) 0.086(6) Uij ? ? C(29) 0.232(1) 0.745(1) 0.2022(5) 0.052(4) Uij ? ? C(30) 0.273(1) 0.774(1) 0.2501(6) 0.054(5) Uij ? ? C(31) 0.297(1) 0.808(1) 0.2889(6) 0.058(5) Uij ? ? C(32) 0.326(1) 0.843(1) 0.3377(5) 0.058(5) Uij ? ? C(33) 0.442(1) 0.799(1) 0.3606(6) 0.097(7) Uij ? ? C(34) 0.427(3) 0.795(2) 0.4124(9) 0.16(1) Uij ? ? C(35) 0.303(3) 0.788(3) 0.4162(9) 0.21(1) Uij ? ? C(36) 0.238(2) 0.802(1) 0.3682(6) 0.099(7) Uij ? ? C(37) 0.468(4) 0.505(4) 0.525(2) 0.29(3) Uij ? ? C(38) 0.552(4) 0.536(3) 0.564(2) 0.32(3) Uij ? ? C(39) 0.507(7) 0.520(4) 0.612(2) 0.49(4) Uij ? ? C(40) -0.096(4) 0.915(4) -0.060(2) 0.15(1) Uij ? ? C(41) -0.189(4) 0.793(4) -0.062(2) 0.136(9) Uij ? ? H(1) 0.5155 0.5575 0.1669 0.0974 Uij ? ? H(2) 0.3024 1.0181 0.3220 0.0974 Uij ? ? H(3) -0.0080 0.8173 0.0619 0.0835 Uij ? ? H(4) -0.2097 0.7141 -0.0144 0.1290 Uij ? ? H(5) -0.2266 0.8263 0.0078 0.1290 Uij ? ? H(6) -0.2155 0.8040 -0.0874 0.1273 Uij ? ? H(7) -0.1993 0.9151 -0.0624 0.1273 Uij ? ? H(8) -0.0451 0.7879 -0.0919 0.1129 Uij ? ? H(9) -0.0529 0.9126 -0.0926 0.1129 Uij ? ? H(10) 0.0256 0.9266 -0.0188 0.1155 Uij ? ? H(11) 0.0852 0.8208 -0.0314 0.1155 Uij ? ? H(12) 0.3322 0.4813 0.1028 0.0877 Uij ? ? H(13) 0.2134 0.4793 0.0711 0.0877 Uij ? ? H(14) 0.3820 0.4302 0.0300 0.1126 Uij ? ? H(15) 0.2973 0.5126 0.0032 0.1126 Uij ? ? H(16) 0.5063 0.5588 0.0591 0.1157 Uij ? ? H(17) 0.4602 0.6111 0.0107 0.1157 Uij ? ? H(18) 0.3719 0.7368 0.0449 0.0990 Uij ? ? H(19) 0.4413 0.6992 0.0924 0.0990 Uij ? ? H(20) 0.5426 0.7568 0.1735 0.1089 Uij ? ? H(21) 0.4797 0.7987 0.2146 0.1089 Uij ? ? H(22) 0.6714 0.6719 0.2218 0.1840 Uij ? ? H(23) 0.6310 0.7434 0.2612 0.1840 Uij ? ? H(24) 0.6015 0.5306 0.2521 0.1603 Uij ? ? H(25) 0.5662 0.6013 0.2929 0.1603 Uij ? ? H(26) 0.3875 0.6125 0.2598 0.1028 Uij ? ? H(27) 0.4163 0.5087 0.2333 0.1028 Uij ? ? H(28) 0.4562 0.7296 0.3489 0.1163 Uij ? ? H(29) 0.5031 0.8462 0.3553 0.1163 Uij ? ? H(30) 0.4660 0.7343 0.4269 0.1936 Uij ? ? H(31) 0.4582 0.8590 0.4278 0.1936 Uij ? ? H(32) 0.2858 0.7197 0.4286 0.2479 Uij ? ? H(33) 0.2815 0.8431 0.4366 0.2479 Uij ? ? H(34) 0.1774 0.8522 0.3687 0.1185 Uij ? ? H(35) 0.2070 0.7346 0.3564 0.1185 Uij ? ? H(36) 0.4089 0.5582 0.5202 0.3497 Uij ? ? H(37) 0.4350 0.4377 0.5313 0.3497 Uij ? ? H(40) 0.6195 0.4927 0.5638 0.3845 Uij ? ? H(41) 0.5716 0.6094 0.5609 0.3845 Uij ? ? H(44) 0.5643 0.5411 0.6375 0.5881 Uij ? ? H(45) 0.4396 0.5626 0.6132 0.5881 Uij ? ? H(46) 0.4881 0.4462 0.6162 0.5881 Uij ? ? 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 Ru(1) 0.0457(7) 0.0734(9) 0.0565(8) 0.0013(6) -0.0021(6) -0.0054(7) Ru(2) 0.0433(7) 0.0600(8) 0.0475(7) 0.0004(6) 0.0054(5) -0.0033(6) Ru(3) 0.0488(7) 0.0616(8) 0.0540(8) 0.0032(6) 0.0021(6) -0.0059(6) O(1) 0.054(7) 0.13(1) 0.16(1) -0.001(8) -0.004(8) 0.006(8) O(2) 0.132(10) 0.092(9) 0.103(10) -0.031(8) 0.015(8) -0.038(7) O(3) 0.053(6) 0.126(9) 0.101(9) -0.016(7) 0.023(6) 0.017(7) O(4) 0.15(1) 0.083(8) 0.12(1) 0.046(8) 0.049(9) 0.010(8) O(5) 0.14(1) 0.123(10) 0.055(8) -0.042(8) 0.003(8) 0.010(7) O(6) 0.15(1) 0.073(8) 0.15(1) -0.041(8) -0.071(9) 0.029(8) O(7) 0.13(1) 0.119(10) 0.087(9) 0.042(8) 0.055(8) -0.010(7) O(8) 0.084(8) 0.115(10) 0.13(1) 0.036(8) -0.044(8) -0.013(8) O(9) 0.064(6) 0.114(8) 0.036(6) 0.001(6) -0.002(6) 0.003(6) O(10) 0.052(6) 0.135(9) 0.080(7) 0.033(6) -0.007(5) -0.034(7) O(11) 0.063(6) 0.070(7) 0.076(7) -0.006(6) 0.002(5) -0.006(6) C(1) 0.042(9) 0.10(1) 0.11(1) 0.00(1) 0.00(1) 0.01(1) C(2) 0.07(1) 0.07(1) 0.07(1) -0.005(10) 0.007(9) -0.009(9) C(3) 0.042(9) 0.10(1) 0.056(10) 0.013(9) -0.007(8) -0.015(9) C(4) 0.053(10) 0.11(1) 0.07(1) 0.03(1) 0.014(8) 0.01(1) C(5) 0.11(1) 0.07(1) 0.05(1) -0.003(9) -0.017(10) 0.011(9) C(6) 0.08(1) 0.07(1) 0.07(1) 0.00(1) -0.019(9) 0.006(9) C(7) 0.07(1) 0.07(1) 0.09(1) 0.011(9) 0.03(1) -0.02(1) C(8) 0.06(1) 0.08(1) 0.07(1) 0.010(9) -0.006(9) -0.020(9) C(9) 0.06(1) 0.07(1) 0.08(1) 0.012(9) 0.00(1) -0.016(10) C(10) 0.09(1) 0.05(1) 0.07(1) 0.009(9) -0.02(1) -0.011(9) C(11) 0.11(2) 0.16(2) 0.04(1) 0.01(1) -0.03(1) -0.01(1) C(14) 0.13(1) 0.08(1) 0.08(1) 0.00(1) -0.02(1) 0.016(10) C(15) 0.05(1) 0.08(1) 0.08(1) 0.017(9) 0.03(1) -0.003(9) C(16) 0.07(1) 0.049(9) 0.029(9) -0.020(8) 0.001(7) -0.011(6) C(17) 0.034(8) 0.066(10) 0.05(1) 0.016(8) 0.014(8) 0.008(8) C(18) 0.040(9) 0.08(1) 0.049(10) 0.000(8) 0.015(8) -0.013(8) C(19) 0.047(9) 0.14(2) 0.037(9) -0.002(9) 0.007(7) -0.020(9) C(20) 0.08(1) 0.12(1) 0.08(1) -0.01(1) 0.01(1) -0.04(1) C(21) 0.09(1) 0.15(2) 0.06(1) 0.02(1) 0.034(9) -0.04(1) C(22) 0.07(1) 0.12(1) 0.06(1) -0.001(10) 0.005(9) 0.005(10) C(23) 0.041(9) 0.08(1) 0.035(9) -0.001(8) -0.001(8) 0.001(8) C(24) 0.035(9) 0.11(1) 0.06(1) 0.021(9) 0.015(8) -0.009(10) C(25) 0.048(10) 0.13(1) 0.09(1) 0.01(1) 0.01(1) -0.04(1) C(26) 0.08(2) 0.16(2) 0.19(3) -0.01(2) -0.06(2) -0.03(2) C(27) 0.07(1) 0.23(3) 0.09(1) 0.06(2) -0.03(1) -0.03(2) C(28) 0.10(1) 0.10(1) 0.05(1) 0.03(1) -0.004(9) -0.007(10) C(29) 0.040(8) 0.077(10) 0.035(9) -0.001(7) -0.006(7) -0.006(7) C(30) 0.031(8) 0.08(1) 0.06(1) 0.000(7) 0.009(8) 0.005(9) C(31) 0.06(1) 0.056(10) 0.05(1) -0.007(8) 0.001(9) 0.006(9) C(32) 0.042(9) 0.08(1) 0.05(1) -0.019(9) 0.009(8) 0.001(9) C(33) 0.09(1) 0.15(2) 0.04(1) 0.04(1) -0.016(9) -0.03(1) C(34) 0.20(3) 0.16(2) 0.11(2) 0.03(2) -0.02(2) 0.01(2) C(35) 0.17(2) 0.37(4) 0.09(2) 0.07(3) 0.02(2) 0.05(2) C(36) 0.13(1) 0.10(1) 0.07(1) -0.02(1) 0.02(1) -0.02(1) C(37) 0.21(5) 0.25(4) 0.39(9) -0.08(4) -0.04(4) 0.11(6) C(38) 0.25(4) 0.15(3) 0.53(9) -0.07(3) -0.09(5) 0.10(5) C(39) 0.9(1) 0.16(3) 0.41(8) -0.05(5) 0.27(9) 0.12(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 2630 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0545 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0525 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.185 _refine_ls_shift/esd_max 0.2860 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.58 _refine_diff_density_max 0.61 #------------------------------------------------------------------------------ _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 Ru(1) Ru(2) 2.799(2) ? ? yes Ru(1) Ru(3) 2.869(2) ? ? yes Ru(1) C(1) 1.89(2) ? ? yes Ru(1) C(2) 1.84(2) ? ? yes Ru(1) C(3) 2.04(2) ? ? yes Ru(1) C(9) 2.16(2) ? ? yes Ru(1) C(15) 2.30(1) ? ? yes Ru(1) C(16) 2.34(1) ? ? yes Ru(2) Ru(3) 2.751(1) ? ? yes Ru(2) C(3) 2.06(1) ? ? yes Ru(2) C(4) 1.88(2) ? ? yes Ru(2) C(5) 1.83(2) ? ? yes Ru(2) C(17) 2.34(1) ? ? yes Ru(2) C(23) 2.29(1) ? ? yes Ru(2) C(29) 2.15(1) ? ? yes Ru(3) C(6) 1.86(2) ? ? yes Ru(3) C(7) 1.88(2) ? ? yes Ru(3) C(8) 1.95(2) ? ? yes Ru(3) C(16) 2.02(1) ? ? yes Ru(3) C(29) 2.11(1) ? ? yes O(1) C(1) 1.10(1) ? ? yes O(2) C(2) 1.12(1) ? ? yes O(3) C(3) 1.19(1) ? ? yes O(4) C(4) 1.14(2) ? ? yes O(5) C(5) 1.11(1) ? ? yes O(6) C(6) 1.16(1) ? ? yes O(7) C(7) 1.12(2) ? ? yes O(8) C(8) 1.11(1) ? ? yes O(9) C(15) 1.35(1) ? ? yes O(9) C(18) 1.47(1) ? ? yes O(10) C(24) 1.42(1) ? ? yes O(11) C(32) 1.45(2) ? ? yes C(9) C(10) 1.31(2) ? ? yes C(9) C(15) 1.40(2) ? ? yes C(10) C(11) 1.52(2) ? ? yes C(10) C(14) 1.53(2) ? ? yes C(11) C(12) 1.66(5) ? ? yes C(11) C(41) 1.42(5) ? ? yes C(12) C(13) 1.34(5) ? ? yes C(12) C(40) 1.23(5) ? ? yes C(12) C(41) 0.67(6) ? ? yes C(13) C(14) 1.46(4) ? ? yes C(13) C(40) 1.02(5) ? ? yes C(13) C(41) 1.72(6) ? ? yes C(14) C(40) 1.64(5) ? ? yes C(15) C(16) 1.38(2) ? ? yes C(16) C(17) 1.44(2) ? ? yes C(17) C(18) 1.53(2) ? ? yes C(17) C(23) 1.38(2) ? ? yes C(18) C(19) 1.49(2) ? ? yes C(18) C(22) 1.55(2) ? ? yes C(19) C(20) 1.54(2) ? ? yes C(20) C(21) 1.51(2) ? ? yes C(21) C(22) 1.50(2) ? ? yes C(23) C(24) 1.52(2) ? ? yes C(23) C(29) 1.43(2) ? ? yes C(24) C(25) 1.57(2) ? ? yes C(24) C(28) 1.50(2) ? ? yes C(25) C(26) 1.50(3) ? ? yes C(26) C(27) 1.52(3) ? ? yes C(27) C(28) 1.49(2) ? ? yes C(29) C(30) 1.43(2) ? ? yes C(30) C(31) 1.18(2) ? ? yes C(31) C(32) 1.45(2) ? ? yes C(32) C(33) 1.52(2) ? ? yes C(32) C(36) 1.52(2) ? ? yes C(33) C(34) 1.51(3) ? ? yes C(34) C(35) 1.48(3) ? ? yes C(35) C(36) 1.48(3) ? ? yes C(37) C(37) 1.69(10) ? ? yes C(37) C(38) 1.44(7) ? ? yes C(38) C(39) 1.55(8) ? ? 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 Ru(2) Ru(1) Ru(3) 58.06(4) ? ? ? yes Ru(2) Ru(1) C(1) 134.2(5) ? ? ? yes Ru(2) Ru(1) C(2) 101.6(5) ? ? ? yes Ru(2) Ru(1) C(3) 47.3(4) ? ? ? yes Ru(2) Ru(1) C(9) 123.8(4) ? ? ? yes Ru(2) Ru(1) C(15) 87.6(4) ? ? ? yes Ru(2) Ru(1) C(16) 58.0(3) ? ? ? yes Ru(3) Ru(1) C(1) 111.2(5) ? ? ? yes Ru(3) Ru(1) C(2) 156.4(5) ? ? ? yes Ru(3) Ru(1) C(3) 80.3(4) ? ? ? yes Ru(3) Ru(1) C(9) 91.0(4) ? ? ? yes Ru(3) Ru(1) C(15) 73.2(4) ? ? ? yes Ru(3) Ru(1) C(16) 44.2(3) ? ? ? yes C(1) Ru(1) C(2) 91.4(7) ? ? ? yes C(1) Ru(1) C(3) 88.4(6) ? ? ? yes C(1) Ru(1) C(9) 99.0(7) ? ? ? yes C(1) Ru(1) C(15) 134.9(6) ? ? ? yes C(1) Ru(1) C(16) 148.0(6) ? ? ? yes C(2) Ru(1) C(3) 94.2(6) ? ? ? yes C(2) Ru(1) C(9) 92.0(6) ? ? ? yes C(2) Ru(1) C(15) 95.9(6) ? ? ? yes C(2) Ru(1) C(16) 116.8(5) ? ? ? yes C(3) Ru(1) C(9) 170.2(6) ? ? ? yes C(3) Ru(1) C(15) 134.9(6) ? ? ? yes C(3) Ru(1) C(16) 103.2(5) ? ? ? yes C(9) Ru(1) C(15) 36.5(5) ? ? ? yes C(9) Ru(1) C(16) 67.2(5) ? ? ? yes C(15) Ru(1) C(16) 34.5(4) ? ? ? yes Ru(1) Ru(2) Ru(3) 62.24(4) ? ? ? yes Ru(1) Ru(2) C(3) 46.7(4) ? ? ? yes Ru(1) Ru(2) C(4) 107.4(4) ? ? ? yes Ru(1) Ru(2) C(5) 129.7(5) ? ? ? yes Ru(1) Ru(2) C(17) 79.7(3) ? ? ? yes Ru(1) Ru(2) C(23) 111.0(3) ? ? ? yes Ru(1) Ru(2) C(29) 107.6(3) ? ? ? yes Ru(3) Ru(2) C(3) 82.9(4) ? ? ? yes Ru(3) Ru(2) C(4) 165.1(4) ? ? ? yes Ru(3) Ru(2) C(5) 104.4(5) ? ? ? yes Ru(3) Ru(2) C(17) 71.6(3) ? ? ? yes Ru(3) Ru(2) C(23) 75.1(3) ? ? ? yes Ru(3) Ru(2) C(29) 49.1(3) ? ? ? yes C(3) Ru(2) C(4) 97.6(6) ? ? ? yes C(3) Ru(2) C(5) 85.4(6) ? ? ? yes C(3) Ru(2) C(17) 126.3(6) ? ? ? yes C(3) Ru(2) C(23) 155.1(6) ? ? ? yes C(3) Ru(2) C(29) 128.9(5) ? ? ? yes C(4) Ru(2) C(5) 90.5(6) ? ? ? yes C(4) Ru(2) C(17) 96.7(5) ? ? ? yes C(4) Ru(2) C(23) 100.7(5) ? ? ? yes C(4) Ru(2) C(29) 133.4(5) ? ? ? yes C(5) Ru(2) C(17) 145.8(6) ? ? ? yes C(5) Ru(2) C(23) 111.1(6) ? ? ? yes C(5) Ru(2) C(29) 90.1(6) ? ? ? yes C(17) Ru(2) C(23) 34.7(4) ? ? ? yes C(17) Ru(2) C(29) 61.0(5) ? ? ? yes C(23) Ru(2) C(29) 37.5(4) ? ? ? yes Ru(1) Ru(3) Ru(2) 59.70(4) ? ? ? yes Ru(1) Ru(3) C(6) 143.8(4) ? ? ? yes Ru(1) Ru(3) C(7) 112.6(5) ? ? ? yes Ru(1) Ru(3) C(8) 70.7(4) ? ? ? yes Ru(1) Ru(3) C(16) 53.8(3) ? ? ? yes Ru(1) Ru(3) C(29) 106.5(4) ? ? ? yes Ru(2) Ru(3) C(6) 137.7(4) ? ? ? yes Ru(2) Ru(3) C(7) 94.6(4) ? ? ? yes Ru(2) Ru(3) C(8) 128.4(4) ? ? ? yes Ru(2) Ru(3) C(16) 61.6(4) ? ? ? yes Ru(2) Ru(3) C(29) 50.5(4) ? ? ? yes C(6) Ru(3) C(7) 98.6(6) ? ? ? yes C(6) Ru(3) C(8) 91.2(6) ? ? ? yes C(6) Ru(3) C(16) 101.9(6) ? ? ? yes C(6) Ru(3) C(29) 88.5(5) ? ? ? yes C(7) Ru(3) C(8) 91.9(6) ? ? ? yes C(7) Ru(3) C(16) 155.9(6) ? ? ? yes C(7) Ru(3) C(29) 94.0(6) ? ? ? yes C(8) Ru(3) C(16) 100.1(6) ? ? ? yes C(8) Ru(3) C(29) 174.1(6) ? ? ? yes C(16) Ru(3) C(29) 74.3(5) ? ? ? yes C(15) O(9) C(18) 110(1) ? ? ? yes Ru(1) C(1) O(1) 178(1) ? ? ? yes Ru(1) C(2) O(2) 177(1) ? ? ? yes Ru(1) C(3) Ru(2) 86.0(6) ? ? ? yes Ru(1) C(3) O(3) 139(1) ? ? ? yes Ru(2) C(3) O(3) 134(1) ? ? ? yes Ru(2) C(4) O(4) 174(1) ? ? ? yes Ru(2) C(5) O(5) 179(1) ? ? ? yes Ru(3) C(6) O(6) 178(1) ? ? ? yes Ru(3) C(7) O(7) 174(1) ? ? ? yes Ru(3) C(8) O(8) 173(1) ? ? ? yes Ru(1) C(9) C(10) 142(1) ? ? ? yes Ru(1) C(9) C(15) 76(1) ? ? ? yes C(10) C(9) C(15) 140(1) ? ? ? yes C(9) C(10) C(11) 124(1) ? ? ? yes C(9) C(10) C(14) 122(1) ? ? ? yes C(11) C(10) C(14) 112(1) ? ? ? yes C(10) C(11) C(12) 93(1) ? ? ? yes C(10) C(11) C(41) 103(2) ? ? ? yes C(12) C(11) C(41) 23(2) ? ? ? yes C(11) C(12) C(13) 115(3) ? ? ? yes C(11) C(12) C(40) 112(4) ? ? ? yes C(11) C(12) C(41) 57(6) ? ? ? yes C(13) C(12) C(40) 46(2) ? ? ? yes C(13) C(12) C(41) 113(7) ? ? ? yes C(40) C(12) C(41) 155(9) ? ? ? yes C(12) C(13) C(14) 105(3) ? ? ? yes C(12) C(13) C(40) 61(3) ? ? ? yes C(12) C(13) C(41) 20(2) ? ? ? yes C(14) C(13) C(40) 80(3) ? ? ? yes C(14) C(13) C(41) 105(2) ? ? ? yes C(40) C(13) C(41) 80(4) ? ? ? yes C(10) C(14) C(13) 104(1) ? ? ? yes C(10) C(14) C(40) 98(2) ? ? ? yes C(13) C(14) C(40) 37(1) ? ? ? yes Ru(1) C(15) O(9) 121.5(9) ? ? ? yes Ru(1) C(15) C(9) 66.5(9) ? ? ? yes Ru(1) C(15) C(16) 74.4(8) ? ? ? yes O(9) C(15) C(9) 117(1) ? ? ? yes O(9) C(15) C(16) 111(1) ? ? ? yes C(9) C(15) C(16) 127(1) ? ? ? yes Ru(1) C(16) Ru(3) 82.0(4) ? ? ? yes Ru(1) C(16) C(15) 71.1(8) ? ? ? yes Ru(1) C(16) C(17) 120.8(8) ? ? ? yes Ru(3) C(16) C(15) 131(1) ? ? ? yes Ru(3) C(16) C(17) 119.1(10) ? ? ? yes C(15) C(16) C(17) 108(1) ? ? ? yes Ru(2) C(17) C(16) 80.1(7) ? ? ? yes Ru(2) C(17) C(18) 128.2(8) ? ? ? yes Ru(2) C(17) C(23) 70.8(7) ? ? ? yes C(16) C(17) C(18) 106(1) ? ? ? yes C(16) C(17) C(23) 116(1) ? ? ? yes C(18) C(17) C(23) 136(1) ? ? ? yes O(9) C(18) C(17) 102.9(10) ? ? ? yes O(9) C(18) C(19) 108(1) ? ? ? yes O(9) C(18) C(22) 107(1) ? ? ? yes C(17) C(18) C(19) 119(1) ? ? ? yes C(17) C(18) C(22) 114(1) ? ? ? yes C(19) C(18) C(22) 104(1) ? ? ? yes C(18) C(19) C(20) 104(1) ? ? ? yes C(19) C(20) C(21) 100(1) ? ? ? yes C(20) C(21) C(22) 107(1) ? ? ? yes C(18) C(22) C(21) 105(1) ? ? ? yes Ru(2) C(23) C(17) 74.5(7) ? ? ? yes Ru(2) C(23) C(24) 125.4(9) ? ? ? yes Ru(2) C(23) C(29) 66.1(7) ? ? ? yes C(17) C(23) C(24) 126(1) ? ? ? yes C(17) C(23) C(29) 108(1) ? ? ? yes C(24) C(23) C(29) 124(1) ? ? ? yes O(10) C(24) C(23) 105(1) ? ? ? yes O(10) C(24) C(25) 110(1) ? ? ? yes O(10) C(24) C(28) 108(1) ? ? ? yes C(23) C(24) C(25) 110(1) ? ? ? yes C(23) C(24) C(28) 116(1) ? ? ? yes C(25) C(24) C(28) 104(1) ? ? ? yes C(24) C(25) C(26) 103(1) ? ? ? yes C(25) C(26) C(27) 108(1) ? ? ? yes C(26) C(27) C(28) 107(1) ? ? ? yes C(24) C(28) C(27) 105(1) ? ? ? yes Ru(2) C(29) Ru(3) 80.3(4) ? ? ? yes Ru(2) C(29) C(23) 76.4(7) ? ? ? yes Ru(2) C(29) C(30) 125.1(9) ? ? ? yes Ru(3) C(29) C(23) 120.5(9) ? ? ? yes Ru(3) C(29) C(30) 117.8(9) ? ? ? yes C(23) C(29) C(30) 120(1) ? ? ? yes C(29) C(30) C(31) 172(1) ? ? ? yes C(30) C(31) C(32) 176(1) ? ? ? yes O(11) C(32) C(31) 110(1) ? ? ? yes O(11) C(32) C(33) 106(1) ? ? ? yes O(11) C(32) C(36) 111(1) ? ? ? yes C(31) C(32) C(33) 112(1) ? ? ? yes C(31) C(32) C(36) 110(1) ? ? ? yes C(33) C(32) C(36) 105(1) ? ? ? yes C(32) C(33) C(34) 102(1) ? ? ? yes C(33) C(34) C(35) 108(1) ? ? ? yes C(34) C(35) C(36) 108(1) ? ? ? yes C(32) C(36) C(35) 105(1) ? ? ? yes C(37) C(37) C(38) 109(5) ? ? ? yes C(37) C(38) C(39) 111(4) ? ? ? yes C(12) C(40) C(13) 72(4) ? ? ? yes C(12) C(40) C(14) 101(3) ? ? ? yes C(13) C(40) C(14) 61(3) ? ? ? yes C(11) C(41) C(12) 99(8) ? ? ? yes C(11) C(41) C(13) 107(3) ? ? ? yes C(12) C(41) C(13) 45(6) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_WTW256_LAU014_13_JUN_97 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Feb 5 19:14:57 1999' _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 'SIR88' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.328(1) _cell_length_b 20.565(2) _cell_length_c 16.159(1) _cell_angle_alpha 90 _cell_angle_beta 109.09(2) _cell_angle_gamma 90 _cell_volume 3557.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 25.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'dark' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_meas ? _chemical_formula_weight 927.85 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H32 O10 Ru3 ' _chemical_formula_moiety 'C36 H32 O10 Ru3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1840.00 _exptl_absorpt_coefficient_mu 1.314 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.927 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -1 -5 3 1 -5 2 1 4 _diffrn_reflns_number 5096 _reflns_number_total 4880 _reflns_number_observed 3077 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.43 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 22.47 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.02112 _diffrn_orient_matrix_UB_12 0.04691 _diffrn_orient_matrix_UB_13 -0.00350 _diffrn_orient_matrix_UB_21 0.08314 _diffrn_orient_matrix_UB_22 -0.01267 _diffrn_orient_matrix_UB_23 -0.00407 _diffrn_orient_matrix_UB_31 -0.03697 _diffrn_orient_matrix_UB_32 -0.00175 _diffrn_orient_matrix_UB_33 -0.06526 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 12 -1.259 0.836 'International Tables' C 0 144 0.003 0.002 'International Tables' O 0 40 0.011 0.006 'International Tables' H 0 128 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) -0.34184(5) 0.14461(3) 0.66054(4) 0.0478(2) Uij ? ? Ru(2) -0.08359(6) 0.17586(3) 0.70817(4) 0.0489(2) Uij ? ? Ru(3) 0.17254(6) 0.13446(3) 0.82483(4) 0.0446(2) Uij ? ? O(1) -0.4864(7) 0.2705(3) 0.6650(6) 0.124(3) Uij ? ? O(2) -0.5172(6) 0.0567(3) 0.7129(4) 0.089(2) Uij ? ? O(3) -0.4703(6) 0.1313(4) 0.4612(4) 0.106(3) Uij ? ? O(4) -0.0250(7) 0.2087(4) 0.5446(5) 0.136(3) Uij ? ? O(5) -0.0550(7) 0.3199(3) 0.7448(5) 0.112(3) Uij ? ? O(6) 0.4430(6) 0.1085(4) 0.9293(4) 0.096(3) Uij ? ? O(7) 0.2021(7) 0.2755(3) 0.8915(5) 0.112(3) Uij ? ? O(8) 0.2480(6) 0.1641(3) 0.6633(4) 0.086(2) Uij ? ? O(9) -0.0767(4) 0.1776(3) 0.9281(3) 0.054(2) Uij ? ? O(10) -0.0355(4) 0.0173(2) 0.6430(3) 0.049(2) Uij ? ? C(1) -0.4317(8) 0.2243(5) 0.6641(6) 0.074(3) Uij ? ? C(2) -0.4544(7) 0.0900(4) 0.6892(5) 0.058(3) Uij ? ? C(3) -0.4204(8) 0.1377(5) 0.5338(6) 0.073(3) Uij ? ? C(4) -0.0462(8) 0.1956(5) 0.6077(6) 0.082(3) Uij ? ? C(5) -0.0659(8) 0.2649(5) 0.7301(7) 0.078(3) Uij ? ? C(6) 0.3378(8) 0.1143(4) 0.8919(5) 0.063(3) Uij ? ? C(7) 0.1882(8) 0.2247(5) 0.8640(6) 0.070(3) Uij ? ? C(8) 0.2160(8) 0.1530(4) 0.7209(6) 0.059(3) Uij ? ? C(9) -0.2282(8) 0.2665(4) 0.8650(6) 0.071(3) Uij ? ? C(10) -0.302(1) 0.2797(5) 0.9241(10) 0.145(6) Uij ? ? C(11) -0.320(2) 0.2205(6) 0.963(1) 0.189(8) Uij ? ? C(12) -0.2972(7) 0.1649(4) 0.9159(5) 0.061(3) Uij ? ? C(13) -0.2092(7) 0.1918(4) 0.8684(5) 0.050(2) Uij ? ? C(14) -0.2177(6) 0.1549(3) 0.7858(5) 0.045(2) Uij ? ? C(15) -0.1120(6) 0.1135(3) 0.8088(4) 0.037(2) Uij ? ? C(16) -0.1014(6) 0.0740(3) 0.7384(5) 0.039(2) Uij ? ? C(17) -0.2011(6) 0.0824(3) 0.6590(4) 0.041(2) Uij ? ? C(18) -0.1693(6) 0.0370(4) 0.5952(4) 0.047(2) Uij ? ? C(19) -0.2472(7) -0.0250(4) 0.5763(5) 0.058(3) Uij ? ? C(20) -0.239(1) -0.0493(5) 0.4913(6) 0.118(5) Uij ? ? C(21) -0.2296(10) 0.0085(5) 0.4396(6) 0.091(4) Uij ? ? C(22) -0.1713(7) 0.0619(4) 0.5047(5) 0.064(3) Uij ? ? C(23) -0.0264(7) 0.1321(4) 0.8916(5) 0.047(2) Uij ? ? C(24) 0.1008(6) 0.1123(4) 0.9303(4) 0.044(2) Uij ? ? C(25) 0.1464(7) 0.0892(4) 1.0127(5) 0.054(3) Uij ? ? C(26) 0.0726(7) 0.0764(4) 1.0745(5) 0.062(3) Uij ? ? C(27) 0.1708(9) 0.0742(5) 1.1644(5) 0.076(3) Uij ? ? C(28) 0.2798(9) 0.0428(5) 1.1475(6) 0.079(3) Uij ? ? C(29) 0.2815(8) 0.0714(4) 1.0607(5) 0.070(3) Uij ? ? C(30) 0.0010(6) 0.0407(3) 0.7252(5) 0.041(2) Uij ? ? C(31) 0.1260(6) 0.0345(3) 0.7811(4) 0.040(2) Uij ? ? C(32) 0.1874(6) -0.0220(4) 0.7926(5) 0.045(2) Uij ? ? C(33) 0.3222(7) -0.0342(4) 0.8440(6) 0.068(3) Uij ? ? C(34) 0.343(1) -0.1056(6) 0.8347(9) 0.116(5) Uij ? ? C(35) 0.231(1) -0.1351(6) 0.7951(10) 0.140(5) Uij ? ? C(36) 0.1304(8) -0.0876(4) 0.7578(6) 0.070(3) Uij ? ? H(1) -0.2727 0.2801 0.8069 0.0847 Uij ? ? H(2) -0.1499 0.2882 0.8851 0.0847 Uij ? ? H(3) -0.2581 0.3095 0.9686 0.1746 Uij ? ? H(4) -0.3807 0.2979 0.8915 0.1746 Uij ? ? H(5) -0.2651 0.2191 1.0213 0.2255 Uij ? ? H(6) -0.4043 0.2188 0.9626 0.2255 Uij ? ? H(7) -0.2579 0.1310 0.9552 0.0736 Uij ? ? H(8) -0.3727 0.1491 0.8751 0.0736 Uij ? ? H(9) -0.2140 -0.0561 0.6214 0.0696 Uij ? ? H(10) -0.3315 -0.0159 0.5714 0.0696 Uij ? ? H(11) -0.1675 -0.0760 0.5012 0.1421 Uij ? ? H(12) -0.3119 -0.0736 0.4611 0.1421 Uij ? ? H(13) -0.1784 -0.0008 0.4048 0.1095 Uij ? ? H(14) -0.3102 0.0213 0.4027 0.1095 Uij ? ? H(15) -0.2198 0.1005 0.4898 0.0766 Uij ? ? H(16) -0.0887 0.0706 0.5051 0.0766 Uij ? ? H(17) 0.0145 0.1104 1.0712 0.0740 Uij ? ? H(18) 0.0293 0.0362 1.0610 0.0740 Uij ? ? H(19) 0.1915 0.1167 1.1876 0.0913 Uij ? ? H(20) 0.1431 0.0489 1.2037 0.0913 Uij ? ? H(21) 0.3551 0.0527 1.1931 0.0944 Uij ? ? H(22) 0.2691 -0.0031 1.1429 0.0944 Uij ? ? H(23) 0.3104 0.0401 1.0285 0.0841 Uij ? ? H(24) 0.3334 0.1088 1.0705 0.0841 Uij ? ? H(25) 0.3749 -0.0093 0.8210 0.0819 Uij ? ? H(26) 0.3385 -0.0233 0.9039 0.0819 Uij ? ? H(27) 0.3958 -0.1115 0.8000 0.1390 Uij ? ? H(28) 0.3818 -0.1242 0.8909 0.1390 Uij ? ? H(29) 0.2376 -0.1624 0.7495 0.1685 Uij ? ? H(30) 0.2098 -0.1607 0.8373 0.1685 Uij ? ? H(31) 0.0608 -0.0966 0.7764 0.0842 Uij ? ? H(32) 0.1048 -0.0884 0.6956 0.0842 Uij ? ? 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 Ru(1) 0.0350(4) 0.0533(4) 0.0530(4) 0.0014(3) 0.0117(3) 0.0121(3) Ru(2) 0.0396(4) 0.0542(4) 0.0541(4) -0.0071(3) 0.0168(3) 0.0132(3) Ru(3) 0.0351(3) 0.0574(4) 0.0436(4) -0.0092(3) 0.0161(3) -0.0046(3) O(1) 0.097(6) 0.071(5) 0.181(8) 0.040(4) 0.016(5) 0.004(5) O(2) 0.061(4) 0.112(5) 0.088(5) -0.025(4) 0.014(4) 0.036(4) O(3) 0.082(5) 0.169(8) 0.058(4) 0.024(5) 0.010(4) 0.037(5) O(4) 0.135(7) 0.202(9) 0.080(5) -0.074(6) 0.047(5) 0.038(5) O(5) 0.116(6) 0.056(4) 0.179(8) -0.012(4) 0.068(6) 0.017(5) O(6) 0.041(4) 0.158(7) 0.082(5) -0.016(4) 0.010(3) 0.001(4) O(7) 0.120(6) 0.082(5) 0.128(7) -0.033(5) 0.034(5) -0.056(5) O(8) 0.101(5) 0.104(5) 0.077(5) -0.004(4) 0.060(4) 0.010(4) O(9) 0.047(3) 0.068(4) 0.051(3) -0.008(3) 0.024(3) -0.015(3) O(10) 0.046(3) 0.063(3) 0.037(3) 0.006(3) 0.012(2) -0.005(3) C(1) 0.058(6) 0.066(6) 0.090(7) -0.005(5) 0.014(5) 0.016(5) C(2) 0.038(5) 0.077(6) 0.047(5) 0.000(5) -0.001(4) 0.006(4) C(3) 0.047(5) 0.106(8) 0.061(6) 0.015(5) 0.011(5) 0.033(6) C(4) 0.056(6) 0.111(8) 0.079(7) -0.033(5) 0.024(5) 0.020(6) C(5) 0.062(6) 0.062(6) 0.118(8) -0.014(5) 0.042(6) 0.024(6) C(6) 0.046(5) 0.084(7) 0.061(6) -0.008(5) 0.022(5) 0.001(5) C(7) 0.057(6) 0.085(7) 0.068(6) -0.017(5) 0.021(5) -0.015(6) C(8) 0.061(5) 0.056(5) 0.072(6) -0.014(4) 0.038(5) -0.005(4) C(9) 0.074(6) 0.047(5) 0.091(7) -0.011(5) 0.027(5) -0.011(5) C(10) 0.23(2) 0.066(8) 0.20(1) 0.015(9) 0.16(1) -0.013(9) C(11) 0.31(2) 0.069(8) 0.31(2) -0.01(1) 0.26(2) -0.04(1) C(12) 0.054(5) 0.067(6) 0.069(6) -0.003(4) 0.030(5) -0.010(5) C(13) 0.042(5) 0.053(5) 0.058(5) -0.010(4) 0.022(4) -0.009(4) C(14) 0.035(4) 0.047(5) 0.056(5) -0.014(4) 0.020(4) 0.002(4) C(15) 0.035(4) 0.038(4) 0.038(4) -0.005(3) 0.012(3) 0.002(4) C(16) 0.039(4) 0.037(4) 0.046(4) -0.005(3) 0.021(4) 0.005(4) C(17) 0.039(4) 0.048(4) 0.036(4) -0.006(3) 0.014(3) 0.005(3) C(18) 0.037(4) 0.065(5) 0.035(4) -0.008(4) 0.006(3) 0.002(4) C(19) 0.057(5) 0.070(6) 0.045(5) -0.008(4) 0.014(4) -0.013(4) C(20) 0.21(1) 0.085(8) 0.049(6) -0.034(8) 0.020(7) -0.018(6) C(21) 0.113(9) 0.108(9) 0.060(7) -0.003(7) 0.037(6) -0.017(6) C(22) 0.054(5) 0.092(7) 0.048(5) 0.005(5) 0.019(4) 0.012(5) C(23) 0.048(5) 0.055(5) 0.043(5) -0.015(4) 0.022(4) -0.002(4) C(24) 0.032(4) 0.061(5) 0.038(5) -0.004(4) 0.011(4) -0.005(4) C(25) 0.051(5) 0.068(6) 0.045(5) -0.012(4) 0.017(4) -0.013(4) C(26) 0.061(5) 0.077(6) 0.052(5) -0.008(5) 0.025(4) -0.003(4) C(27) 0.093(7) 0.088(7) 0.046(5) -0.005(6) 0.021(5) 0.019(5) C(28) 0.085(7) 0.083(7) 0.058(6) 0.004(6) 0.010(5) 0.014(5) C(29) 0.058(6) 0.096(7) 0.050(5) -0.003(5) 0.010(4) 0.008(5) C(30) 0.044(5) 0.042(4) 0.040(5) -0.004(4) 0.018(4) 0.001(4) C(31) 0.035(4) 0.053(5) 0.034(4) 0.002(4) 0.015(3) 0.001(3) C(32) 0.040(4) 0.055(5) 0.045(5) 0.006(4) 0.019(4) 0.006(4) C(33) 0.049(5) 0.086(7) 0.071(6) 0.020(5) 0.021(5) 0.005(5) C(34) 0.076(8) 0.098(9) 0.16(1) 0.034(7) 0.019(8) 0.006(8) C(35) 0.105(10) 0.087(9) 0.19(1) 0.036(8) -0.010(9) -0.010(9) C(36) 0.071(6) 0.058(6) 0.088(7) 0.005(5) 0.036(5) 0.007(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 3077 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0327 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0340 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.344 _refine_ls_shift/esd_max 0.0300 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.41 _refine_diff_density_max 0.46 #------------------------------------------------------------------------------ _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . 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 # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_wtwong431-LAU034 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Feb 5 18:19:01 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Marresearch Image Plate' _computing_cell_refinement 'Marresearch Image Plate' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR88' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 20.454(1) _cell_length_b 10.328(1) _cell_length_c 26.616(1) _cell_angle_alpha 90.00(2) _cell_angle_beta 104.00(2) _cell_angle_gamma 90.00(2) _cell_volume 5455.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'Brown' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.160 _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_meas ? _chemical_formula_weight 1260.23 _chemical_formula_analytical ? _chemical_formula_sum 'C55 H65 Cl2 O10 Ru3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2564.00 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type 'interimage scaling' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 1.000 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Image plate' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 39627 _reflns_number_total 10259 _reflns_number_observed 7423 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 25.60 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 12 -1.259 0.836 'International Tables' O 0 40 0.011 0.006 'International Tables' C 0 220 0.003 0.002 'International Tables' H 0 260 0.000 0.000 'International Tables' Cl 0 8 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.08109(2) -0.09967(3) 0.81641(1) 0.0328(1) Uij ? ? Ru(2) 0.01977(2) 0.08940(3) 0.86116(1) 0.0337(1) Uij ? ? Ru(3) 0.03765(2) 0.21261(3) 0.77061(1) 0.0356(1) Uij ? ? Cl(1) 0.2670(3) 0.2279(4) 0.4055(2) 0.286(3) Uij ? ? Cl(2) 0.2032(3) 0.1743(3) 0.4852(1) 0.230(2) Uij ? ? O(1) 0.2092(2) -0.1602(4) 0.8997(2) 0.066(1) Uij ? ? O(2) 0.0324(2) -0.3764(4) 0.7886(2) 0.076(1) Uij ? ? O(3) -0.0591(2) 0.2897(4) 0.9039(2) 0.082(2) Uij ? ? O(4) -0.0781(2) 0.4020(4) 0.7657(2) 0.088(2) Uij ? ? O(5) 0.1048(2) 0.4208(3) 0.7222(2) 0.065(1) Uij ? ? O(6) 0.1172(2) 0.1479(3) 0.9620(1) 0.055(1) Uij ? ? O(7) 0.0986(2) -0.0597(3) 0.9505(1) 0.045(1) Uij ? ? O(8) -0.1057(2) 0.0745(3) 0.7209(1) 0.045(1) Uij ? ? O(9) 0.1951(2) 0.2640(3) 0.8416(1) 0.042(1) Uij ? ? O(10) -0.2180(2) -0.0736(3) 0.9495(1) 0.061(1) Uij ? ? C(1) 0.1615(3) -0.1409(4) 0.8684(2) 0.042(2) Uij ? ? C(2) 0.0502(3) -0.2743(5) 0.8003(2) 0.046(2) Uij ? ? C(3) -0.0301(3) 0.2126(5) 0.8871(2) 0.050(2) Uij ? ? C(4) -0.0360(3) 0.3290(5) 0.7664(2) 0.052(2) Uij ? ? C(5) 0.0797(3) 0.3396(5) 0.7401(2) 0.045(2) Uij ? ? C(6) 0.0849(3) 0.0664(4) 0.9339(2) 0.044(2) Uij ? ? C(7) 0.0470(3) -0.1553(4) 0.9278(2) 0.038(1) Uij ? ? C(8) 0.0784(3) -0.2912(5) 0.9327(2) 0.052(2) Uij ? ? C(9) 0.0356(5) -0.3774(7) 0.9552(5) 0.174(5) Uij ? ? C(10) -0.0233(3) -0.3045(5) 0.9630(2) 0.066(2) Uij ? ? C(11) -0.0010(3) -0.1637(5) 0.9647(2) 0.050(2) Uij ? ? C(12) 0.0188(3) -0.1091(4) 0.8727(2) 0.038(1) Uij ? ? C(13) -0.0516(3) -0.0859(4) 0.8499(2) 0.038(1) Uij ? ? C(14) -0.1081(3) -0.1113(4) 0.8721(2) 0.045(2) Uij ? ? C(15) -0.1582(3) -0.1306(5) 0.8862(2) 0.048(2) Uij ? ? C(16) -0.2178(3) -0.1584(5) 0.9071(2) 0.050(2) Uij ? ? C(17) -0.2222(3) -0.2991(5) 0.9227(2) 0.062(2) Uij ? ? C(18) -0.2961(4) -0.3202(8) 0.9201(3) 0.098(3) Uij ? ? C(19) -0.3348(3) -0.2133(7) 0.8894(3) 0.078(2) Uij ? ? C(20) -0.2844(3) -0.1360(6) 0.8674(2) 0.062(2) Uij ? ? C(21) -0.0099(2) -0.0123(4) 0.7761(2) 0.034(1) Uij ? ? C(22) -0.0638(2) -0.0250(4) 0.8004(2) 0.034(1) Uij ? ? C(23) -0.1284(2) 0.0176(4) 0.7649(2) 0.042(1) Uij ? ? C(24) -0.1751(3) -0.0951(4) 0.7430(2) 0.054(2) Uij ? ? C(25) -0.2431(3) -0.0314(6) 0.7197(3) 0.082(2) Uij ? ? C(26) -0.2439(4) 0.0892(7) 0.7495(3) 0.088(3) Uij ? ? C(27) -0.1740(3) 0.1162(5) 0.7823(2) 0.055(2) Uij ? ? C(28) -0.0378(3) 0.0543(4) 0.7280(2) 0.037(1) Uij ? ? C(29) -0.0009(2) 0.1147(4) 0.6972(2) 0.039(1) Uij ? ? C(30) 0.0033(3) 0.1115(5) 0.6484(2) 0.046(2) Uij ? ? C(31) -0.0308(3) 0.0125(6) 0.6094(2) 0.063(2) Uij ? ? C(32) -0.0279(6) 0.068(1) 0.5585(3) 0.144(4) Uij ? ? C(33) 0.0323(4) 0.1505(8) 0.5675(3) 0.099(3) Uij ? ? C(34) 0.0426(3) 0.2041(6) 0.6227(2) 0.063(2) Uij ? ? C(35) 0.0864(2) 0.2338(4) 0.8529(2) 0.036(1) Uij ? ? C(36) 0.1114(3) 0.3581(4) 0.8813(2) 0.043(2) Uij ? ? C(37) 0.1844(3) 0.3729(4) 0.8766(2) 0.042(2) Uij ? ? C(38) 0.2026(3) 0.4993(4) 0.8528(2) 0.051(2) Uij ? ? C(39) 0.2786(3) 0.5184(5) 0.8748(3) 0.069(2) Uij ? ? C(40) 0.3025(3) 0.4092(6) 0.9141(3) 0.071(2) Uij ? ? C(41) 0.2379(3) 0.3587(5) 0.9262(2) 0.055(2) Uij ? ? C(42) 0.1401(2) 0.1887(4) 0.8329(2) 0.033(1) Uij ? ? C(43) 0.1233(2) 0.0851(4) 0.7973(2) 0.034(1) Uij ? ? C(44) 0.1580(2) -0.0109(4) 0.7756(2) 0.034(1) Uij ? ? C(45) 0.2320(3) -0.0461(5) 0.7897(2) 0.045(2) Uij ? ? C(46) 0.2330(3) -0.1882(5) 0.7740(2) 0.055(2) Uij ? ? C(47) 0.1686(3) -0.2079(4) 0.7323(2) 0.051(2) Uij ? ? C(48) 0.1205(2) -0.1043(4) 0.7412(2) 0.038(1) Uij ? ? C(49) 0.2451(6) 0.2843(10) 0.4581(4) 0.148(4) Uij ? ? C(50) 0.353(1) 0.040(2) 0.9680(8) 0.253(8) Uij ? ? C(51) 0.374(2) 0.045(3) 0.928(1) 0.37(1) Uij ? ? C(52) 0.441(1) 0.091(2) 0.9251(10) 0.293(9) Uij ? ? C(53) 0.484(1) 0.131(2) 0.8883(8) 0.228(7) Uij ? ? C(54) 0.538(1) 0.118(2) 0.8738(10) 0.298(10) Uij ? ? C(55) 0.5735(8) 0.167(2) 0.8369(6) 0.213(6) Uij ? ? H(1) -0.1718 -0.0909 0.9800 0.0637 Uij ? ? H(2) 0.0803 -0.3220 0.8994 0.0623 Uij ? ? H(3) 0.1226 -0.2884 0.9546 0.0623 Uij ? ? H(4) 0.0207 -0.4479 0.9323 0.2083 Uij ? ? H(5) 0.0609 -0.4095 0.9875 0.2083 Uij ? ? H(6) -0.0614 -0.3187 0.9351 0.0787 Uij ? ? H(7) -0.0337 -0.3287 0.9946 0.0787 Uij ? ? H(8) 0.0219 -0.1400 0.9989 0.0596 Uij ? ? H(9) -0.0388 -0.1085 0.9530 0.0596 Uij ? ? H(10) -0.2075 -0.3551 0.8993 0.0745 Uij ? ? H(11) -0.1957 -0.3135 0.9568 0.0745 Uij ? ? H(12) -0.3103 -0.4008 0.9039 0.1178 Uij ? ? H(13) -0.3032 -0.3200 0.9541 0.1178 Uij ? ? H(14) -0.3694 -0.2472 0.8621 0.0941 Uij ? ? H(15) -0.3543 -0.1597 0.9110 0.0941 Uij ? ? H(16) -0.2958 -0.0467 0.8649 0.0741 Uij ? ? H(17) -0.2825 -0.1677 0.8343 0.0741 Uij ? ? H(18) -0.1591 -0.1398 0.7172 0.0645 Uij ? ? H(19) -0.1786 -0.1537 0.7698 0.0645 Uij ? ? H(20) -0.2472 -0.0122 0.6842 0.0988 Uij ? ? H(21) -0.2788 -0.0869 0.7230 0.0988 Uij ? ? H(22) -0.2581 0.1592 0.7263 0.1057 Uij ? ? H(23) -0.2742 0.0796 0.7713 0.1057 Uij ? ? H(24) -0.1727 0.1050 0.8180 0.0659 Uij ? ? H(25) -0.1606 0.2018 0.7766 0.0659 Uij ? ? H(26) -0.0075 -0.0678 0.6150 0.0754 Uij ? ? H(27) -0.0762 0.0000 0.6112 0.0754 Uij ? ? H(28) -0.0248 0.0010 0.5349 0.1730 Uij ? ? H(29) -0.0671 0.1185 0.5449 0.1730 Uij ? ? H(30) 0.0703 0.1010 0.5646 0.1182 Uij ? ? H(31) 0.0256 0.2195 0.5432 0.1182 Uij ? ? H(32) 0.0252 0.2895 0.6222 0.0762 Uij ? ? H(33) 0.0890 0.2040 0.6401 0.0762 Uij ? ? H(34) 0.0849 0.4295 0.8656 0.0513 Uij ? ? H(35) 0.1099 0.3521 0.9166 0.0513 Uij ? ? H(36) 0.1927 0.4924 0.8162 0.0609 Uij ? ? H(37) 0.1783 0.5698 0.8623 0.0609 Uij ? ? H(38) 0.3015 0.5136 0.8478 0.0831 Uij ? ? H(39) 0.2870 0.6002 0.8914 0.0831 Uij ? ? H(40) 0.3243 0.3428 0.8995 0.0849 Uij ? ? H(41) 0.3324 0.4416 0.9445 0.0849 Uij ? ? H(42) 0.2268 0.4084 0.9530 0.0665 Uij ? ? H(43) 0.2429 0.2704 0.9364 0.0665 Uij ? ? H(44) 0.2564 0.0058 0.7711 0.0536 Uij ? ? H(45) 0.2505 -0.0359 0.8258 0.0536 Uij ? ? H(46) 0.2713 -0.2055 0.7608 0.0657 Uij ? ? H(47) 0.2337 -0.2431 0.8028 0.0657 Uij ? ? H(48) 0.1771 -0.1986 0.6989 0.0609 Uij ? ? H(49) 0.1505 -0.2915 0.7352 0.0609 Uij ? ? H(50) 0.2849 0.3088 0.4829 0.1778 Uij ? ? H(51) 0.2171 0.3580 0.4484 0.1778 Uij ? ? H(52) 0.3529 0.1245 0.9821 0.3030 Uij ? ? H(53) 0.3087 0.0060 0.9599 0.3030 Uij ? ? H(54) 0.3818 -0.0144 0.9926 0.3030 Uij ? ? H(55) 0.3711 -0.0404 0.9150 0.4449 Uij ? ? H(56) 0.3432 0.0993 0.9050 0.4449 Uij ? ? H(57) 0.4448 0.1672 0.9458 0.3516 Uij ? ? H(58) 0.4686 0.0250 0.9442 0.3516 Uij ? ? H(59) 0.4531 0.1131 0.8563 0.2737 Uij ? ? H(60) 0.4862 0.2212 0.8945 0.2737 Uij ? ? H(61) 0.5708 0.1327 0.9054 0.3569 Uij ? ? H(62) 0.5370 0.0278 0.8659 0.3569 Uij ? ? H(63) 0.6148 0.1217 0.8406 0.2560 Uij ? ? H(64) 0.5464 0.1549 0.8028 0.2560 Uij ? ? H(65) 0.5823 0.2566 0.8430 0.2560 Uij ? ? 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 Ru(1) 0.0372(3) 0.0285(2) 0.0356(2) -0.0003(2) 0.0147(2) 0.0000(2) Ru(2) 0.0386(3) 0.0296(2) 0.0372(2) -0.0012(2) 0.0176(2) -0.0002(2) Ru(3) 0.0402(3) 0.0309(2) 0.0388(2) 0.0007(2) 0.0152(2) 0.0032(2) Cl(1) 0.330(6) 0.246(4) 0.361(7) -0.041(4) 0.234(6) -0.093(4) Cl(2) 0.398(6) 0.146(2) 0.139(3) -0.091(3) 0.048(3) 0.011(2) O(1) 0.053(3) 0.087(3) 0.056(3) 0.007(2) 0.009(2) 0.015(2) O(2) 0.097(4) 0.041(2) 0.089(3) -0.021(2) 0.020(3) -0.013(2) O(3) 0.085(4) 0.078(3) 0.092(3) 0.031(2) 0.041(3) -0.021(2) O(4) 0.062(3) 0.059(3) 0.149(5) 0.017(2) 0.039(3) 0.017(3) O(5) 0.069(3) 0.056(2) 0.076(3) -0.012(2) 0.027(2) 0.025(2) O(6) 0.074(3) 0.047(2) 0.043(2) -0.015(2) 0.011(2) -0.005(2) O(7) 0.052(2) 0.040(2) 0.043(2) -0.005(2) 0.013(2) 0.004(1) O(8) 0.035(2) 0.050(2) 0.051(2) -0.002(2) 0.010(2) 0.009(2) O(9) 0.040(2) 0.037(2) 0.054(2) -0.008(2) 0.021(2) -0.010(1) O(10) 0.050(3) 0.080(3) 0.056(2) -0.003(2) 0.020(2) -0.016(2) C(1) 0.044(4) 0.040(3) 0.048(3) -0.002(2) 0.019(3) 0.005(2) C(2) 0.050(4) 0.044(3) 0.047(3) 0.004(3) 0.018(3) 0.008(2) C(3) 0.052(4) 0.049(3) 0.051(3) -0.008(3) 0.019(3) 0.000(2) C(4) 0.049(4) 0.039(3) 0.070(4) -0.002(3) 0.019(3) 0.006(3) C(5) 0.044(3) 0.046(3) 0.045(3) 0.006(2) 0.011(3) 0.005(2) C(6) 0.052(4) 0.042(3) 0.043(3) -0.003(2) 0.026(3) 0.000(2) C(7) 0.049(3) 0.034(2) 0.035(3) -0.001(2) 0.016(2) 0.003(2) C(8) 0.061(4) 0.050(3) 0.047(3) -0.001(3) 0.018(3) 0.012(2) C(9) 0.21(1) 0.041(4) 0.36(2) 0.002(5) 0.24(1) 0.014(6) C(10) 0.088(5) 0.053(3) 0.067(4) -0.013(3) 0.041(4) 0.007(3) C(11) 0.066(4) 0.050(3) 0.040(3) -0.003(3) 0.027(3) 0.004(2) C(12) 0.050(4) 0.030(2) 0.040(3) -0.001(2) 0.021(2) -0.001(2) C(13) 0.041(3) 0.030(2) 0.047(3) -0.005(2) 0.020(2) -0.003(2) C(14) 0.047(4) 0.042(3) 0.053(3) -0.004(2) 0.022(3) 0.001(2) C(15) 0.047(4) 0.053(3) 0.049(3) -0.005(3) 0.018(3) 0.001(2) C(16) 0.048(4) 0.058(3) 0.050(3) -0.012(3) 0.024(3) -0.003(2) C(17) 0.058(4) 0.062(3) 0.073(4) -0.019(3) 0.027(3) 0.002(3) C(18) 0.075(6) 0.110(6) 0.118(6) -0.036(5) 0.040(5) 0.009(5) C(19) 0.050(4) 0.106(5) 0.078(5) -0.027(4) 0.014(4) -0.012(4) C(20) 0.043(4) 0.090(4) 0.053(4) -0.009(3) 0.013(3) -0.001(3) C(21) 0.039(3) 0.026(2) 0.038(3) -0.006(2) 0.011(2) -0.002(2) C(22) 0.034(3) 0.028(2) 0.043(3) -0.004(2) 0.015(2) -0.002(2) C(23) 0.036(3) 0.041(3) 0.050(3) -0.002(2) 0.013(2) 0.002(2) C(24) 0.044(4) 0.043(3) 0.071(4) -0.009(3) 0.010(3) -0.002(3) C(25) 0.053(5) 0.072(4) 0.111(6) -0.011(3) -0.002(4) 0.009(4) C(26) 0.060(5) 0.083(5) 0.124(6) 0.020(4) 0.025(5) 0.017(4) C(27) 0.050(4) 0.042(3) 0.079(4) 0.005(3) 0.028(3) 0.004(3) C(28) 0.039(3) 0.034(2) 0.037(3) -0.006(2) 0.007(2) -0.005(2) C(29) 0.040(3) 0.042(3) 0.035(3) 0.005(2) 0.009(2) 0.006(2) C(30) 0.041(3) 0.055(3) 0.040(3) 0.009(2) 0.008(2) 0.008(2) C(31) 0.061(4) 0.078(4) 0.048(4) 0.007(3) 0.011(3) -0.015(3) C(32) 0.137(9) 0.24(1) 0.059(5) -0.065(8) 0.038(5) -0.042(6) C(33) 0.098(7) 0.152(7) 0.052(4) 0.006(5) 0.032(4) 0.000(4) C(34) 0.074(5) 0.077(4) 0.047(3) 0.004(3) 0.030(3) 0.009(3) C(35) 0.041(3) 0.031(2) 0.040(3) -0.002(2) 0.017(2) -0.001(2) C(36) 0.052(4) 0.035(2) 0.043(3) -0.004(2) 0.016(3) -0.004(2) C(37) 0.048(4) 0.039(3) 0.042(3) -0.010(2) 0.015(3) -0.006(2) C(38) 0.053(4) 0.033(3) 0.069(4) -0.008(2) 0.020(3) -0.003(2) C(39) 0.061(5) 0.054(3) 0.096(5) -0.016(3) 0.027(4) 0.001(3) C(40) 0.053(4) 0.081(4) 0.073(4) -0.013(3) 0.006(3) -0.011(3) C(41) 0.063(4) 0.051(3) 0.053(4) -0.006(3) 0.014(3) -0.002(2) C(42) 0.034(3) 0.032(2) 0.035(3) -0.003(2) 0.010(2) 0.004(2) C(43) 0.031(3) 0.039(3) 0.036(3) 0.000(2) 0.016(2) 0.001(2) C(44) 0.042(3) 0.030(2) 0.037(3) -0.003(2) 0.020(2) 0.005(2) C(45) 0.040(3) 0.046(3) 0.052(3) -0.001(2) 0.019(3) 0.001(2) C(46) 0.057(4) 0.040(3) 0.076(4) 0.013(3) 0.033(3) -0.002(3) C(47) 0.067(4) 0.037(3) 0.057(3) -0.002(3) 0.032(3) -0.009(2) C(48) 0.048(3) 0.039(3) 0.035(3) -0.001(2) 0.026(2) -0.005(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 7423 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0438 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0470 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.546 _refine_ls_shift/esd_max 0.0070 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.16 _refine_diff_density_max 0.20 #------------------------------------------------------------------------------ _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . 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 # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_wtwong302-LAU023 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Feb 5 18:28:45 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Marresearch Image Plate' _computing_cell_refinement 'Marresearch Image Plate' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR88' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.876(1) _cell_length_b 10.885(1) _cell_length_c 29.792(2) _cell_angle_alpha 90 _cell_angle_beta 94.05(2) _cell_angle_gamma 90 _cell_volume 3841.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'dark' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.180 _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_meas ? _chemical_formula_weight 1084.94 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H32 O12 Ru4 ' _chemical_formula_moiety 'C38 H32 O12 Ru4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2128.00 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type 'interimage scaling' #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Image Plate' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 24583 _reflns_number_total 5555 _reflns_number_observed 2711 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 25.59 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 16 -1.259 0.836 'International Tables' O 0 48 0.011 0.006 'International Tables' C 0 152 0.003 0.002 'International Tables' H 0 128 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) -0.0819(1) 0.1931(1) 0.19699(4) 0.0570(5) Uij ? ? Ru(2) -0.0147(1) 0.1816(1) 0.10916(4) 0.0507(4) Uij ? ? Ru(3) 0.1713(1) 0.2485(1) 0.05134(4) 0.0485(4) Uij ? ? Ru(4) 0.3479(1) 0.3852(1) 0.08729(4) 0.0522(4) Uij ? ? O(1) -0.329(1) 0.289(2) 0.1979(6) 0.135(8) Uij ? ? O(2) -0.024(1) 0.265(2) 0.2934(5) 0.121(7) Uij ? ? O(3) -0.168(1) -0.059(2) 0.2163(6) 0.130(7) Uij ? ? O(4) -0.065(1) -0.081(1) 0.0806(5) 0.109(6) Uij ? ? O(5) -0.215(1) 0.246(1) 0.0458(6) 0.108(6) Uij ? ? O(6) 0.145(1) -0.019(1) 0.0250(5) 0.089(5) Uij ? ? O(7) -0.021(1) 0.338(2) -0.0146(6) 0.131(7) Uij ? ? O(8) 0.440(1) 0.460(1) 0.1807(4) 0.107(6) Uij ? ? O(9) 0.584(1) 0.403(1) 0.0617(5) 0.098(6) Uij ? ? O(10) 0.322(1) 0.291(1) -0.0241(4) 0.087(5) Uij ? ? O(11) 0.0103(10) 0.516(1) 0.1175(4) 0.067(4) Uij ? ? O(12) 0.2455(9) 0.052(1) 0.1564(4) 0.061(4) Uij ? ? C(1) -0.242(2) 0.255(2) 0.1947(6) 0.083(8) Uij ? ? C(2) -0.049(2) 0.236(2) 0.2565(7) 0.087(8) Uij ? ? C(3) -0.139(2) 0.037(2) 0.2118(7) 0.087(8) Uij ? ? C(4) -0.043(2) 0.017(2) 0.0915(6) 0.085(8) Uij ? ? C(5) -0.136(2) 0.220(2) 0.0682(6) 0.070(7) Uij ? ? C(6) 0.152(1) 0.079(2) 0.0357(5) 0.061(6) Uij ? ? C(7) 0.044(2) 0.304(2) 0.0110(7) 0.087(8) Uij ? ? C(8) 0.402(2) 0.432(2) 0.1432(7) 0.090(8) Uij ? ? C(9) 0.498(2) 0.386(2) 0.0696(6) 0.068(7) Uij ? ? C(10) 0.279(1) 0.280(2) 0.0073(6) 0.063(6) Uij ? ? C(11) -0.187(2) 0.490(2) 0.1223(8) 0.102(8) Uij ? ? C(12) -0.244(2) 0.598(3) 0.1410(9) 0.13(1) Uij ? ? C(13) -0.161(3) 0.651(3) 0.174(1) 0.14(1) Uij ? ? C(14) -0.076(2) 0.560(2) 0.1874(6) 0.078(7) Uij ? ? C(15) -0.074(2) 0.467(2) 0.1473(7) 0.076(7) Uij ? ? C(16) -0.032(2) 0.343(2) 0.1629(5) 0.065(7) Uij ? ? C(17) 0.074(1) 0.332(2) 0.1451(5) 0.053(6) Uij ? ? C(18) 0.138(1) 0.220(2) 0.1539(5) 0.048(5) Uij ? ? C(19) 0.071(1) 0.136(1) 0.1799(5) 0.059(6) Uij ? ? C(20) 0.158(2) 0.028(2) 0.1857(7) 0.076(7) Uij ? ? C(21) 0.205(1) 0.023(2) 0.2352(5) 0.076(7) Uij ? ? C(22) 0.242(2) -0.110(2) 0.2398(8) 0.12(1) Uij ? ? C(23) 0.168(4) -0.183(2) 0.214(1) 0.23(2) Uij ? ? C(24) 0.115(2) -0.105(2) 0.1754(7) 0.100(8) Uij ? ? C(25) 0.099(2) 0.432(1) 0.1128(5) 0.060(6) Uij ? ? C(26) 0.235(1) 0.167(2) 0.1371(5) 0.062(6) Uij ? ? C(27) 0.175(1) 0.436(1) 0.0835(5) 0.051(5) Uij ? ? C(28) 0.234(1) 0.546(1) 0.0717(6) 0.058(6) Uij ? ? C(29) 0.235(2) 0.662(2) 0.1015(7) 0.089(7) Uij ? ? C(30) 0.352(2) 0.717(2) 0.0917(8) 0.084(8) Uij ? ? C(31) 0.380(2) 0.677(2) 0.0462(6) 0.083(7) Uij ? ? C(32) 0.313(2) 0.554(2) 0.0414(6) 0.074(7) Uij ? ? C(33) 0.320(1) 0.197(1) 0.1052(5) 0.055(4) Uij ? ? C(34) 0.402(2) 0.099(2) 0.0983(6) 0.071(6) Uij ? ? C(35) 0.457(1) 0.088(1) 0.0561(6) 0.063(6) Uij ? ? C(36) 0.567(2) 0.017(2) 0.067(1) 0.112(10) Uij ? ? C(37) 0.594(2) 0.031(2) 0.1175(6) 0.099(9) Uij ? ? C(38) 0.499(2) 0.099(2) 0.1345(8) 0.104(9) Uij ? ? H(1) -0.2337 0.4198 0.1249 0.1233 Uij ? ? H(2) -0.1762 0.5046 0.0915 0.1233 Uij ? ? H(3) -0.2636 0.6560 0.1179 0.1580 Uij ? ? H(4) -0.3097 0.5736 0.1549 0.1580 Uij ? ? H(5) -0.1255 0.7197 0.1615 0.1715 Uij ? ? H(6) -0.1975 0.6761 0.2000 0.1715 Uij ? ? H(7) -0.0043 0.5976 0.1927 0.0932 Uij ? ? H(8) -0.0953 0.5184 0.2138 0.0932 Uij ? ? H(9) 0.2658 0.0780 0.2409 0.0912 Uij ? ? H(10) 0.1472 0.0408 0.2549 0.0912 Uij ? ? H(11) 0.3164 -0.1180 0.2295 0.1457 Uij ? ? H(12) 0.2439 -0.1343 0.2704 0.1457 Uij ? ? H(13) 0.2063 -0.2505 0.2021 0.2759 Uij ? ? H(14) 0.1101 -0.2122 0.2318 0.2759 Uij ? ? H(15) 0.0348 -0.1074 0.1747 0.1207 Uij ? ? H(16) 0.1388 -0.1321 0.1473 0.1207 Uij ? ? H(17) 0.1752 0.7167 0.0924 0.1072 Uij ? ? H(18) 0.2316 0.6426 0.1324 0.1072 Uij ? ? H(19) 0.3487 0.8038 0.0928 0.1009 Uij ? ? H(20) 0.4078 0.6878 0.1135 0.1009 Uij ? ? H(21) 0.3553 0.7348 0.0238 0.0994 Uij ? ? H(22) 0.4593 0.6640 0.0450 0.0994 Uij ? ? H(23) 0.4100 0.0442 0.0345 0.0758 Uij ? ? H(24) 0.4732 0.1669 0.0447 0.0758 Uij ? ? H(25) 0.5575 -0.0676 0.0592 0.1346 Uij ? ? H(26) 0.6264 0.0502 0.0507 0.1346 Uij ? ? H(27) 0.6007 -0.0470 0.1315 0.1180 Uij ? ? H(28) 0.6621 0.0758 0.1233 0.1180 Uij ? ? H(29) 0.5211 0.1816 0.1411 0.1249 Uij ? ? H(30) 0.4757 0.0611 0.1609 0.1249 Uij ? ? H(31) 0.2867 0.5349 0.0114 0.0887 Uij ? ? H(32) 0.3636 0.0235 0.1019 0.0848 Uij ? ? 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 Ru(1) 0.054(1) 0.0661(10) 0.0521(8) -0.0101(8) 0.0111(7) -0.0096(7) Ru(2) 0.045(1) 0.0579(9) 0.0484(7) -0.0039(8) 0.0012(6) -0.0079(6) Ru(3) 0.0473(10) 0.0520(8) 0.0460(7) 0.0028(7) 0.0024(6) -0.0045(6) Ru(4) 0.052(1) 0.0536(8) 0.0518(7) -0.0026(7) 0.0066(6) -0.0033(6) O(1) 0.04(1) 0.20(2) 0.17(2) 0.00(1) 0.02(1) -0.07(1) O(2) 0.10(1) 0.18(2) 0.08(1) -0.04(1) 0.005(9) -0.018(10) O(3) 0.13(2) 0.13(1) 0.13(1) -0.02(1) 0.08(1) -0.01(1) O(4) 0.15(1) 0.070(10) 0.11(1) -0.027(10) 0.002(10) -0.030(9) O(5) 0.08(1) 0.11(1) 0.12(1) 0.016(9) -0.037(10) -0.011(9) O(6) 0.11(1) 0.053(8) 0.11(1) 0.014(8) 0.004(8) -0.030(8) O(7) 0.11(1) 0.15(2) 0.12(1) 0.06(1) -0.06(1) 0.01(1) O(8) 0.10(1) 0.14(1) 0.072(9) -0.014(10) -0.020(8) -0.024(9) O(9) 0.05(1) 0.13(1) 0.11(1) -0.010(9) 0.035(9) -0.008(9) O(10) 0.09(1) 0.12(1) 0.054(8) -0.032(8) 0.022(8) -0.003(7) O(11) 0.061(9) 0.058(8) 0.082(8) 0.004(7) 0.012(7) -0.006(6) O(12) 0.058(9) 0.058(7) 0.066(7) 0.019(7) 0.011(6) -0.005(6) C(1) 0.07(2) 0.11(2) 0.07(1) -0.04(1) 0.02(1) -0.02(1) C(2) 0.10(2) 0.11(2) 0.05(1) -0.04(1) 0.01(1) 0.00(1) C(3) 0.10(2) 0.07(1) 0.10(2) -0.02(1) 0.06(1) 0.00(1) C(4) 0.08(2) 0.10(2) 0.07(1) 0.03(1) -0.02(1) -0.02(1) C(5) 0.09(2) 0.06(1) 0.06(1) 0.00(1) 0.00(1) -0.003(9) C(6) 0.04(1) 0.09(2) 0.056(10) 0.00(1) 0.019(8) -0.017(10) C(7) 0.10(2) 0.07(1) 0.10(2) -0.02(1) 0.01(1) -0.01(1) C(8) 0.11(2) 0.07(1) 0.09(2) 0.00(1) -0.03(1) 0.01(1) C(9) 0.07(2) 0.039(10) 0.09(1) 0.01(1) 0.03(1) 0.000(9) C(10) 0.07(1) 0.07(1) 0.05(1) 0.000(9) -0.007(9) -0.007(9) C(11) 0.08(2) 0.06(1) 0.16(2) 0.04(1) -0.05(1) -0.02(1) C(12) 0.09(2) 0.20(3) 0.10(2) 0.07(2) 0.02(2) 0.01(2) C(13) 0.13(3) 0.17(3) 0.14(3) 0.02(2) 0.06(2) -0.02(2) C(14) 0.06(1) 0.10(2) 0.08(1) 0.01(1) 0.03(1) -0.02(1) C(15) 0.06(2) 0.05(1) 0.11(2) 0.00(1) 0.01(1) -0.03(1) C(16) 0.06(1) 0.08(1) 0.06(1) -0.02(1) -0.008(9) -0.005(9) C(17) 0.04(1) 0.06(1) 0.058(9) -0.011(9) 0.014(8) 0.003(9) C(18) 0.02(1) 0.07(1) 0.049(8) 0.006(8) 0.008(7) -0.013(8) C(19) 0.08(1) 0.042(9) 0.051(9) 0.017(9) -0.012(9) -0.015(8) C(20) 0.06(2) 0.06(1) 0.11(1) -0.01(1) 0.00(1) 0.00(1) C(21) 0.07(1) 0.12(2) 0.036(9) -0.01(1) 0.001(9) 0.005(10) C(22) 0.16(3) 0.10(2) 0.11(2) 0.05(2) -0.02(2) 0.03(2) C(23) 0.42(5) 0.07(2) 0.17(3) 0.07(3) -0.19(3) -0.06(2) C(24) 0.14(2) 0.04(1) 0.11(2) 0.00(1) -0.05(1) 0.01(1) C(25) 0.08(2) 0.05(1) 0.048(10) -0.01(1) -0.002(9) -0.020(8) C(26) 0.07(1) 0.06(1) 0.055(10) 0.008(10) -0.027(9) 0.003(9) C(27) 0.06(1) 0.05(1) 0.044(9) 0.008(9) 0.006(8) 0.006(8) C(28) 0.07(1) 0.035(9) 0.07(1) 0.010(9) -0.008(9) 0.012(8) C(29) 0.10(2) 0.04(1) 0.12(2) 0.01(1) 0.03(1) -0.02(1) C(30) 0.08(2) 0.04(1) 0.13(2) -0.016(10) 0.00(1) 0.01(1) C(31) 0.10(2) 0.08(1) 0.06(1) -0.04(1) -0.01(1) 0.01(1) C(32) 0.06(1) 0.08(1) 0.08(1) -0.02(1) -0.01(1) 0.01(1) C(34) 0.07(1) 0.05(1) 0.09(1) 0.020(10) -0.01(1) -0.020(9) C(35) 0.06(1) 0.05(1) 0.08(1) 0.007(9) 0.02(1) -0.004(9) C(36) 0.05(2) 0.06(1) 0.22(3) 0.02(1) -0.03(2) 0.00(2) C(37) 0.05(1) 0.18(2) 0.07(1) 0.05(1) 0.03(1) -0.01(1) C(38) 0.05(1) 0.11(2) 0.15(2) 0.02(1) -0.05(1) -0.04(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 2711 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0606 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0676 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.177 _refine_ls_shift/esd_max 0.0440 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.36 _refine_diff_density_max 0.42 #------------------------------------------------------------------------------ _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . 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 # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_wtwong661-Lau #------------------------------------------------------------------------------ _audit_creation_date 'Fri Feb 5 18:32:32 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Marresearch Image Plate' _computing_cell_refinement 'Marresearch Image Plate' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.453(1) _cell_length_b 9.638(1) _cell_length_c 30.759(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2802.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.210 _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_meas ? _chemical_formula_weight 801.61 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H18 O12 Ru3 ' _chemical_formula_moiety 'C24 H18 O12 Ru3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1560.00 _exptl_absorpt_coefficient_mu 1.656 _exptl_absorpt_correction_type 'Interimage scaling' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 1.000 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Image plate' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 11378 _reflns_number_total 2479 _reflns_number_observed 1808 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 4.88 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.62 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru 0 12 -1.259 0.836 'International Tables' C 0 96 0.003 0.002 'International Tables' O 0 48 0.011 0.006 'International Tables' H 0 72 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Ru(1) 0.3633(1) 0.21713(10) 0.18945(3) 0.0424(3) Uij ? ? Ru(2) 0.1302(1) 0.13247(10) 0.14391(4) 0.0451(3) Uij ? ? Ru(3) 0.1712(1) 0.4129(1) 0.16625(4) 0.0499(4) Uij ? ? O(1) 0.623(1) 0.383(1) 0.2129(4) 0.096(5) Uij ? ? O(2) 0.241(1) 0.198(1) 0.2808(4) 0.099(5) Uij ? ? O(3) 0.547(1) -0.043(1) 0.1936(4) 0.074(4) Uij ? ? O(4) -0.134(1) 0.087(2) 0.1986(5) 0.129(6) Uij ? ? O(5) 0.235(1) -0.148(1) 0.1758(4) 0.093(5) Uij ? ? O(6) 0.038(2) 0.006(1) 0.0576(4) 0.120(6) Uij ? ? O(7) -0.069(1) 0.340(1) 0.1011(4) 0.088(5) Uij ? ? O(8) 0.117(2) 0.653(1) 0.1039(5) 0.124(6) Uij ? ? O(9) 0.360(1) 0.5994(9) 0.2203(4) 0.085(4) Uij ? ? O(10) -0.062(2) 0.420(2) 0.2361(5) 0.143(7) Uij ? ? O(11) 0.381(1) -0.0178(8) 0.0876(3) 0.063(3) Uij ? ? O(12) 0.577(2) 0.765(1) 0.1121(4) 0.133(6) Uij ? ? C(1) 0.521(2) 0.321(2) 0.2040(5) 0.060(6) Uij ? ? C(2) 0.290(2) 0.202(1) 0.2476(5) 0.060(5) Uij ? ? C(3) 0.476(2) 0.053(2) 0.1903(5) 0.061(5) Uij ? ? C(4) -0.036(2) 0.096(2) 0.1809(6) 0.075(6) Uij ? ? C(5) 0.205(2) -0.039(1) 0.1655(6) 0.065(5) Uij ? ? C(6) 0.072(2) 0.050(1) 0.0900(6) 0.063(6) Uij ? ? C(7) 0.023(2) 0.309(2) 0.1222(5) 0.052(5) Uij ? ? C(8) 0.129(2) 0.563(2) 0.1278(6) 0.089(7) Uij ? ? C(9) 0.291(2) 0.525(1) 0.2011(6) 0.062(6) Uij ? ? C(10) 0.020(2) 0.417(2) 0.2094(6) 0.078(7) Uij ? ? C(11) 0.383(2) 0.180(1) 0.0396(5) 0.078(6) Uij ? ? C(12) 0.519(2) 0.142(2) 0.0147(6) 0.113(8) Uij ? ? C(13) 0.635(2) 0.158(2) 0.0451(6) 0.094(7) Uij ? ? C(14) 0.572(2) 0.144(1) 0.0902(5) 0.055(5) Uij ? ? C(15) 0.415(1) 0.125(1) 0.0853(4) 0.044(5) Uij ? ? C(16) 0.321(1) 0.204(1) 0.1178(4) 0.039(4) Uij ? ? C(17) 0.336(2) 0.343(1) 0.1280(4) 0.044(4) Uij ? ? C(18) 0.437(1) 0.440(1) 0.1122(5) 0.045(5) Uij ? ? C(19) 0.515(2) 0.529(1) 0.0986(6) 0.062(6) Uij ? ? C(20) 0.602(2) 0.644(1) 0.0840(5) 0.052(5) Uij ? ? C(21) 0.551(2) 0.694(2) 0.0416(6) 0.107(8) Uij ? ? C(22) 0.703(3) 0.739(3) 0.0212(8) 0.16(1) Uij ? ? C(23) 0.816(2) 0.724(3) 0.0537(9) 0.15(1) Uij ? ? C(24) 0.751(2) 0.624(2) 0.083(1) 0.19(1) Uij ? ? H(1) 0.3686 0.2773 0.0399 0.0925 Uij ? ? H(2) 0.3030 0.1352 0.0275 0.0925 Uij ? ? H(3) 0.5146 0.0486 0.0048 0.1352 Uij ? ? H(4) 0.5316 0.2021 -0.0094 0.1352 Uij ? ? H(5) 0.7041 0.0882 0.0404 0.1114 Uij ? ? H(6) 0.6773 0.2469 0.0417 0.1114 Uij ? ? H(7) 0.6114 0.0660 0.1045 0.0666 Uij ? ? H(8) 0.5907 0.2256 0.1066 0.0666 Uij ? ? H(9) 0.5060 0.6234 0.0254 0.1289 Uij ? ? H(10) 0.4888 0.7713 0.0446 0.1289 Uij ? ? H(11) 0.7227 0.6814 -0.0035 0.1875 Uij ? ? H(12) 0.6983 0.8331 0.0115 0.1875 Uij ? ? H(13) 0.9005 0.6880 0.0413 0.1799 Uij ? ? H(14) 0.8353 0.8083 0.0681 0.1799 Uij ? ? H(15) 0.7890 0.6355 0.1105 0.2218 Uij ? ? H(16) 0.7700 0.5338 0.0718 0.2218 Uij ? ? H(17) 0.2972 -0.0085 0.0650 0.0795 Uij ? ? H(18) 0.4832 0.7961 0.1056 0.0795 Uij ? ? 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 Ru(1) 0.0476(8) 0.0442(6) 0.0354(6) 0.0014(6) -0.0071(7) 0.0004(5) Ru(2) 0.0482(8) 0.0414(6) 0.0455(7) -0.0044(6) -0.0025(8) -0.0007(5) Ru(3) 0.0507(9) 0.0421(6) 0.0569(8) 0.0071(5) -0.0057(7) -0.0084(6) O(1) 0.070(9) 0.095(8) 0.12(1) -0.007(8) -0.030(9) -0.029(7) O(2) 0.12(1) 0.113(9) 0.063(9) -0.017(9) 0.022(8) 0.000(8) O(3) 0.090(9) 0.063(7) 0.071(8) 0.025(6) -0.013(7) -0.005(6) O(4) 0.08(1) 0.16(1) 0.15(1) -0.02(1) 0.06(1) 0.03(1) O(5) 0.12(1) 0.038(6) 0.12(1) -0.004(6) -0.010(8) 0.018(6) O(6) 0.14(1) 0.14(1) 0.079(10) -0.05(1) -0.023(10) -0.052(9) O(7) 0.075(10) 0.075(8) 0.11(1) 0.018(6) -0.056(8) -0.012(7) O(8) 0.14(1) 0.065(8) 0.16(1) 0.000(8) -0.08(1) 0.021(8) O(9) 0.107(10) 0.053(6) 0.095(9) 0.007(7) -0.050(9) -0.013(6) O(10) 0.11(1) 0.20(2) 0.12(1) 0.00(1) 0.04(1) -0.06(1) O(11) 0.071(8) 0.033(5) 0.086(7) -0.005(5) 0.000(7) -0.008(4) O(12) 0.22(2) 0.080(9) 0.102(10) -0.040(9) 0.01(1) 0.002(8) C(1) 0.05(1) 0.07(1) 0.06(1) 0.014(9) -0.007(10) 0.018(8) C(2) 0.08(1) 0.047(8) 0.05(1) 0.002(8) -0.01(1) 0.007(8) C(3) 0.07(1) 0.08(1) 0.036(9) -0.013(10) -0.014(9) 0.017(9) C(4) 0.07(1) 0.08(1) 0.07(1) -0.02(1) 0.02(1) -0.003(9) C(5) 0.07(1) 0.046(8) 0.08(1) -0.024(7) 0.01(1) -0.004(9) C(6) 0.05(1) 0.053(9) 0.08(1) 0.004(7) 0.01(1) -0.008(9) C(7) 0.05(1) 0.066(10) 0.035(10) 0.000(9) -0.011(8) -0.009(8) C(8) 0.08(1) 0.06(1) 0.12(2) 0.02(1) -0.06(1) 0.002(10) C(9) 0.06(1) 0.050(9) 0.08(1) 0.004(8) 0.004(10) -0.005(8) C(10) 0.06(1) 0.10(1) 0.07(1) 0.00(1) -0.01(1) -0.04(1) C(11) 0.11(2) 0.073(10) 0.05(1) 0.02(1) 0.02(1) -0.007(8) C(12) 0.11(2) 0.18(2) 0.05(1) 0.00(2) 0.00(1) 0.03(1) C(13) 0.09(1) 0.13(1) 0.07(1) 0.01(1) 0.03(1) 0.00(1) C(14) 0.05(1) 0.056(9) 0.06(1) 0.021(7) -0.008(9) 0.012(8) C(15) 0.05(1) 0.042(8) 0.038(9) -0.007(7) -0.005(8) 0.011(7) C(16) 0.028(9) 0.051(8) 0.036(8) 0.010(7) -0.013(7) 0.013(7) C(17) 0.06(1) 0.029(7) 0.048(9) -0.009(7) 0.006(8) 0.001(6) C(18) 0.04(1) 0.042(8) 0.049(9) 0.007(7) -0.004(8) 0.002(7) C(19) 0.05(1) 0.039(8) 0.10(1) -0.006(8) -0.01(1) 0.016(9) C(20) 0.05(1) 0.030(7) 0.08(1) 0.017(7) 0.011(9) 0.009(7) C(21) 0.13(2) 0.12(1) 0.07(1) -0.08(1) -0.04(1) 0.05(1) C(22) 0.20(3) 0.16(2) 0.11(2) -0.01(2) 0.02(2) 0.04(2) C(23) 0.06(2) 0.22(2) 0.18(2) 0.01(2) -0.02(2) 0.13(2) C(24) 0.06(1) 0.09(1) 0.42(5) 0.01(1) 0.07(2) 0.08(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _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 1808 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0437 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0365 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.143 _refine_ls_shift/esd_max 0.0410 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.39 _refine_diff_density_max 0.48 #------------------------------------------------------------------------------ _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . 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 # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;