# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1449 data_1 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Apr 26 14:37:35 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 20.998(1) _cell_length_b 15.341(2) _cell_length_c 21.779(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7015.7(9) _cell_formula_units_Z 8 _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 b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'Block' _exptl_crystal_colour 'Brown' _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 3.343 _exptl_crystal_density_meas ? _chemical_formula_weight 1765.74 _chemical_formula_analytical ? _chemical_formula_sum 'C25 H20 O15 Os6 S2 ' _chemical_formula_moiety 'C25 H20 O15 Os6 S2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 6224.00 _exptl_absorpt_coefficient_mu 21.818 _exptl_absorpt_correction_type 'inter-image 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 59908 _reflns_number_total 7090 _reflns_number_observed 4612 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.134 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.65 _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 Os 0 48 -1.216 7.603 'International Tables' C 0 200 0.003 0.002 'International Tables' O 0 120 0.011 0.006 'International Tables' S 0 16 0.125 0.123 'International Tables' H 0 160 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 Os(1) 0.73239(3) 0.28959(5) 0.40984(4) 0.0457(2) Uij ? ? Os(2) 0.60195(3) 0.29227(4) 0.40666(3) 0.0357(2) Uij ? ? Os(3) 0.66551(3) 0.19608(4) 0.50094(3) 0.0372(2) Uij ? ? Os(4) 0.65678(3) 0.37590(4) 0.50523(3) 0.0380(2) Uij ? ? Os(5) 0.54507(3) 0.27814(4) 0.51632(3) 0.0393(2) Uij ? ? Os(6) 0.62754(3) 0.27705(5) 0.61225(4) 0.0449(2) Uij ? ? S(1) 0.7586(2) 0.4046(3) 0.3419(2) 0.052(2) Uij ? ? S(2) 0.5089(2) 0.2223(3) 0.4260(2) 0.042(1) Uij ? ? O(1) 0.7844(8) 0.1582(10) 0.3220(8) 0.089(6) Uij ? ? O(2) 0.8602(7) 0.297(2) 0.4726(8) 0.134(9) Uij ? ? O(3) 0.6394(6) 0.2027(8) 0.2885(7) 0.064(5) Uij ? ? O(4) 0.5514(7) 0.4474(9) 0.3360(7) 0.084(6) Uij ? ? O(5) 0.6698(7) 0.0621(8) 0.3988(7) 0.078(5) Uij ? ? O(6) 0.5986(8) 0.0482(9) 0.5668(8) 0.088(6) Uij ? ? O(7) 0.7949(7) 0.157(1) 0.5594(8) 0.095(6) Uij ? ? O(8) 0.5909(8) 0.5128(8) 0.5836(7) 0.076(5) Uij ? ? O(9) 0.7861(7) 0.409(1) 0.5633(9) 0.097(6) Uij ? ? O(10) 0.6718(8) 0.5279(9) 0.4164(8) 0.086(6) Uij ? ? O(11) 0.4568(7) 0.428(1) 0.5415(8) 0.089(6) Uij ? ? O(12) 0.4732(7) 0.159(1) 0.6043(8) 0.106(7) Uij ? ? O(13) 0.5852(7) 0.1312(10) 0.6962(7) 0.084(6) Uij ? ? O(14) 0.5506(7) 0.3996(10) 0.6926(7) 0.084(6) Uij ? ? O(15) 0.7548(6) 0.296(1) 0.6767(8) 0.089(6) Uij ? ? C(1) 0.7655(10) 0.208(1) 0.3560(9) 0.062(7) Uij ? ? C(2) 0.811(1) 0.291(2) 0.446(1) 0.082(9) Uij ? ? C(3) 0.6281(7) 0.239(1) 0.3334(10) 0.042(5) Uij ? ? C(4) 0.5693(9) 0.390(1) 0.362(1) 0.060(7) Uij ? ? C(5) 0.6704(9) 0.116(1) 0.4325(9) 0.056(6) Uij ? ? C(6) 0.6210(9) 0.107(1) 0.544(1) 0.058(7) Uij ? ? C(7) 0.7464(10) 0.174(1) 0.5370(9) 0.055(6) Uij ? ? C(8) 0.6147(9) 0.460(1) 0.5553(9) 0.055(7) Uij ? ? C(9) 0.738(1) 0.396(1) 0.542(1) 0.070(8) Uij ? ? C(10) 0.6665(9) 0.472(1) 0.4470(9) 0.053(6) Uij ? ? C(11) 0.4902(10) 0.371(2) 0.5310(10) 0.071(8) Uij ? ? C(12) 0.5006(9) 0.207(1) 0.573(1) 0.076(8) Uij ? ? C(13) 0.6025(9) 0.187(2) 0.6644(9) 0.065(7) Uij ? ? C(14) 0.5811(9) 0.354(1) 0.6619(9) 0.054(6) Uij ? ? C(15) 0.707(1) 0.292(1) 0.652(1) 0.070(8) Uij ? ? C(16) 0.4359(8) 0.259(1) 0.3882(9) 0.050(6) Uij ? ? C(17) 0.4323(9) 0.225(1) 0.322(1) 0.071(7) Uij ? ? C(18) 0.431(1) 0.127(2) 0.320(1) 0.078(8) Uij ? ? C(19) 0.489(1) 0.085(1) 0.349(1) 0.068(7) Uij ? ? C(20) 0.4994(9) 0.106(1) 0.414(1) 0.068(7) Uij ? ? C(21) 0.8366(9) 0.387(1) 0.310(1) 0.074(8) Uij ? ? C(22) 0.852(1) 0.453(1) 0.260(1) 0.074(8) Uij ? ? C(23) 0.807(1) 0.449(1) 0.209(1) 0.085(9) Uij ? ? C(24) 0.740(1) 0.464(1) 0.226(1) 0.077(8) Uij ? ? C(25) 0.7152(9) 0.397(1) 0.270(1) 0.070(7) Uij ? ? H(1) 0.4002 0.2385 0.4106 0.0595 Uij ? ? H(2) 0.4354 0.3213 0.3877 0.0595 Uij ? ? H(3) 0.3946 0.2473 0.3036 0.0851 Uij ? ? H(4) 0.4684 0.2457 0.3002 0.0851 Uij ? ? H(5) 0.3942 0.1080 0.3412 0.0938 Uij ? ? H(6) 0.4287 0.1101 0.2782 0.0938 Uij ? ? H(7) 0.4840 0.0237 0.3453 0.0813 Uij ? ? H(8) 0.5254 0.1031 0.3264 0.0813 Uij ? ? H(9) 0.5368 0.0770 0.4274 0.0809 Uij ? ? H(10) 0.4639 0.0862 0.4369 0.0809 Uij ? ? H(11) 0.8672 0.3913 0.3423 0.0891 Uij ? ? H(12) 0.8382 0.3299 0.2930 0.0891 Uij ? ? H(13) 0.8508 0.5102 0.2777 0.0883 Uij ? ? H(14) 0.8942 0.4423 0.2455 0.0883 Uij ? ? H(15) 0.8193 0.4914 0.1796 0.1024 Uij ? ? H(16) 0.8106 0.3923 0.1912 0.1024 Uij ? ? H(17) 0.7367 0.5195 0.2446 0.0928 Uij ? ? H(18) 0.7149 0.4619 0.1900 0.0928 Uij ? ? H(19) 0.7205 0.3408 0.2531 0.0846 Uij ? ? H(20) 0.6713 0.4078 0.2773 0.0846 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 Os(1) 0.0318(4) 0.0650(5) 0.0404(5) 0.0004(3) 0.0029(3) 0.0056(4) Os(2) 0.0325(3) 0.0388(4) 0.0359(4) 0.0003(3) -0.0008(3) 0.0015(3) Os(3) 0.0357(4) 0.0360(4) 0.0398(4) 0.0035(3) -0.0005(3) 0.0020(3) Os(4) 0.0380(4) 0.0363(4) 0.0398(5) -0.0030(3) 0.0009(3) -0.0005(3) Os(5) 0.0313(4) 0.0470(4) 0.0395(4) 0.0000(3) 0.0019(3) 0.0016(3) Os(6) 0.0455(4) 0.0546(4) 0.0348(4) -0.0015(4) -0.0009(3) 0.0012(4) S(1) 0.051(3) 0.059(3) 0.047(3) -0.012(2) 0.006(2) -0.001(3) S(2) 0.034(2) 0.046(3) 0.045(3) -0.001(2) -0.002(2) 0.004(2) O(1) 0.11(1) 0.08(1) 0.08(1) 0.034(10) 0.02(1) -0.001(10) O(2) 0.038(9) 0.28(3) 0.08(1) -0.02(1) -0.016(9) 0.05(2) O(3) 0.058(9) 0.068(9) 0.07(1) -0.001(7) 0.021(8) -0.011(8) O(4) 0.11(1) 0.067(10) 0.07(1) 0.033(9) -0.007(9) 0.029(9) O(5) 0.10(1) 0.057(9) 0.08(1) 0.014(8) 0.009(9) -0.027(8) O(6) 0.13(1) 0.049(9) 0.09(1) -0.026(9) 0.02(1) 0.006(8) O(7) 0.052(9) 0.13(1) 0.10(1) 0.017(9) -0.033(9) 0.03(1) O(8) 0.11(1) 0.056(9) 0.06(1) 0.007(8) 0.018(9) -0.020(8) O(9) 0.052(9) 0.11(1) 0.13(2) -0.025(9) -0.04(1) 0.01(1) O(10) 0.11(1) 0.058(9) 0.09(1) 0.026(9) 0.04(1) 0.040(9) O(11) 0.09(1) 0.11(1) 0.07(1) 0.040(10) 0.007(9) -0.013(10) O(12) 0.07(1) 0.15(2) 0.10(1) -0.05(1) -0.012(9) 0.06(1) O(13) 0.10(1) 0.09(1) 0.06(1) -0.036(9) 0.000(9) 0.028(9) O(14) 0.08(1) 0.10(1) 0.07(1) 0.023(9) 0.026(9) -0.013(10) O(15) 0.041(8) 0.13(1) 0.10(1) -0.007(9) -0.024(9) 0.01(1) C(1) 0.07(1) 0.09(2) 0.03(1) 0.01(1) 0.009(10) 0.02(1) C(2) 0.05(1) 0.13(2) 0.07(2) 0.01(1) 0.01(1) 0.00(2) C(3) 0.027(9) 0.039(9) 0.06(1) 0.003(8) 0.014(9) -0.003(9) C(4) 0.06(1) 0.07(1) 0.06(2) 0.01(1) 0.01(1) 0.00(1) C(5) 0.08(1) 0.05(1) 0.04(1) 0.03(1) 0.00(1) 0.010(10) C(6) 0.06(1) 0.04(1) 0.08(2) 0.009(10) 0.02(1) 0.00(1) C(7) 0.06(1) 0.07(1) 0.04(1) 0.01(1) 0.01(1) -0.010(10) C(8) 0.08(1) 0.06(1) 0.03(1) -0.02(1) 0.00(1) 0.001(10) C(9) 0.08(2) 0.08(1) 0.06(2) -0.01(1) 0.00(1) 0.03(1) C(10) 0.05(1) 0.07(1) 0.04(1) 0.00(1) 0.009(10) -0.01(1) C(11) 0.06(1) 0.11(2) 0.05(2) 0.02(1) 0.01(1) -0.01(1) C(12) 0.03(1) 0.11(2) 0.09(2) -0.02(1) -0.02(1) 0.04(2) C(13) 0.05(1) 0.11(2) 0.04(1) -0.04(1) -0.008(9) 0.00(1) C(14) 0.05(1) 0.08(1) 0.03(1) -0.01(1) 0.005(9) 0.01(1) C(15) 0.06(1) 0.09(2) 0.06(2) 0.01(1) 0.02(1) 0.03(1) C(16) 0.037(10) 0.06(1) 0.05(1) 0.014(9) 0.009(9) -0.012(9) C(17) 0.05(1) 0.10(2) 0.06(2) -0.01(1) -0.03(1) 0.01(1) C(18) 0.08(2) 0.10(2) 0.06(2) -0.03(1) 0.00(1) -0.01(1) C(19) 0.08(2) 0.05(1) 0.07(2) 0.00(1) -0.01(1) -0.01(1) C(20) 0.06(1) 0.06(1) 0.09(2) -0.04(1) 0.01(1) 0.01(1) C(21) 0.05(1) 0.09(2) 0.08(2) -0.03(1) 0.01(1) 0.01(1) C(22) 0.07(1) 0.08(1) 0.07(2) -0.01(1) 0.04(1) -0.02(1) C(23) 0.10(2) 0.07(1) 0.08(2) -0.04(1) 0.01(2) 0.03(1) C(24) 0.09(2) 0.09(2) 0.05(1) -0.03(1) -0.01(1) 0.02(1) C(25) 0.07(1) 0.09(1) 0.06(2) -0.04(1) -0.01(1) 0.01(1) #------------------------------------------------------------------------------ _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 4612 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0502 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0511 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.495 _refine_ls_shift/esd_max 0.0160 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.17 _refine_diff_density_max 2.57 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.7402(9) ? ? yes Os(1) Os(3) 2.823(1) ? ? yes Os(1) Os(4) 2.931(1) ? ? yes Os(1) S(1) 2.368(5) ? ? yes Os(1) C(1) 1.85(2) ? ? yes Os(1) C(2) 1.83(2) ? ? yes Os(2) Os(3) 2.8591(9) ? ? yes Os(2) Os(4) 2.753(1) ? ? yes Os(2) Os(5) 2.679(1) ? ? yes Os(2) S(2) 2.269(4) ? ? yes Os(2) C(3) 1.88(2) ? ? yes Os(2) C(4) 1.91(2) ? ? yes Os(3) Os(4) 2.766(1) ? ? yes Os(3) Os(5) 2.8447(9) ? ? yes Os(3) Os(6) 2.838(1) ? ? yes Os(3) C(5) 1.93(2) ? ? yes Os(3) C(6) 1.90(2) ? ? yes Os(3) C(7) 1.90(2) ? ? yes Os(4) Os(5) 2.7945(9) ? ? yes Os(4) Os(6) 2.848(1) ? ? yes Os(4) C(8) 1.90(2) ? ? yes Os(4) C(9) 1.91(2) ? ? yes Os(4) C(10) 1.95(2) ? ? yes Os(5) Os(6) 2.714(1) ? ? yes Os(5) S(2) 2.276(5) ? ? yes Os(5) C(11) 1.85(2) ? ? yes Os(5) C(12) 1.89(2) ? ? yes Os(6) C(13) 1.86(2) ? ? yes Os(6) C(14) 1.87(2) ? ? yes Os(6) C(15) 1.89(2) ? ? yes S(1) C(21) 1.80(2) ? ? yes S(1) C(25) 1.81(2) ? ? yes S(2) C(16) 1.83(2) ? ? yes S(2) C(20) 1.82(2) ? ? yes O(1) C(1) 1.14(2) ? ? yes O(2) C(2) 1.19(3) ? ? yes O(3) C(3) 1.15(2) ? ? yes O(4) C(4) 1.12(2) ? ? yes O(5) C(5) 1.11(2) ? ? yes O(6) C(6) 1.14(2) ? ? yes O(7) C(7) 1.16(2) ? ? yes O(8) C(8) 1.14(2) ? ? yes O(9) C(9) 1.13(2) ? ? yes O(10) C(10) 1.09(2) ? ? yes O(11) C(11) 1.15(2) ? ? yes O(12) C(12) 1.16(2) ? ? yes O(13) C(13) 1.16(2) ? ? yes O(14) C(14) 1.16(2) ? ? yes O(15) C(15) 1.14(2) ? ? yes C(16) C(17) 1.53(3) ? ? yes C(17) C(18) 1.50(3) ? ? yes C(18) C(19) 1.51(3) ? ? yes C(19) C(20) 1.47(3) ? ? yes C(21) C(22) 1.53(3) ? ? yes C(22) C(23) 1.47(3) ? ? yes C(23) C(24) 1.48(3) ? ? yes C(24) C(25) 1.49(3) ? ? 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 Os(2) Os(1) Os(3) 61.84(2) ? ? ? yes Os(2) Os(1) Os(4) 57.97(2) ? ? ? yes Os(2) Os(1) S(1) 101.8(1) ? ? ? yes Os(2) Os(1) C(1) 111.7(6) ? ? ? yes Os(2) Os(1) C(2) 155.8(7) ? ? ? yes Os(3) Os(1) Os(4) 57.44(2) ? ? ? yes Os(3) Os(1) S(1) 159.0(1) ? ? ? yes Os(3) Os(1) C(1) 106.8(6) ? ? ? yes Os(3) Os(1) C(2) 98.7(7) ? ? ? yes Os(4) Os(1) S(1) 103.4(1) ? ? ? yes Os(4) Os(1) C(1) 163.4(6) ? ? ? yes Os(4) Os(1) C(2) 100.2(7) ? ? ? yes S(1) Os(1) C(1) 91.1(6) ? ? ? yes S(1) Os(1) C(2) 93.0(7) ? ? ? yes C(1) Os(1) C(2) 86.7(10) ? ? ? yes Os(1) Os(2) Os(3) 60.50(2) ? ? ? yes Os(1) Os(2) Os(4) 64.49(3) ? ? ? yes Os(1) Os(2) Os(5) 114.95(3) ? ? ? yes Os(1) Os(2) S(2) 148.1(1) ? ? ? yes Os(1) Os(2) C(3) 73.9(5) ? ? ? yes Os(1) Os(2) C(4) 112.5(6) ? ? ? yes Os(3) Os(2) Os(4) 59.03(2) ? ? ? yes Os(3) Os(2) Os(5) 61.71(2) ? ? ? yes Os(3) Os(2) S(2) 91.4(1) ? ? ? yes Os(3) Os(2) C(3) 104.3(5) ? ? ? yes Os(3) Os(2) C(4) 159.6(6) ? ? ? yes Os(4) Os(2) Os(5) 61.90(3) ? ? ? yes Os(4) Os(2) S(2) 115.8(1) ? ? ? yes Os(4) Os(2) C(3) 138.1(5) ? ? ? yes Os(4) Os(2) C(4) 100.6(6) ? ? ? yes Os(5) Os(2) S(2) 54.0(1) ? ? ? yes Os(5) Os(2) C(3) 148.5(5) ? ? ? yes Os(5) Os(2) C(4) 111.0(6) ? ? ? yes S(2) Os(2) C(3) 101.7(5) ? ? ? yes S(2) Os(2) C(4) 99.0(6) ? ? ? yes C(3) Os(2) C(4) 90.8(8) ? ? ? yes Os(1) Os(3) Os(2) 57.66(2) ? ? ? yes Os(1) Os(3) Os(4) 63.25(3) ? ? ? yes Os(1) Os(3) Os(5) 107.47(3) ? ? ? yes Os(1) Os(3) Os(6) 121.18(3) ? ? ? yes Os(1) Os(3) C(5) 75.7(6) ? ? ? yes Os(1) Os(3) C(6) 162.9(6) ? ? ? yes Os(1) Os(3) C(7) 86.4(6) ? ? ? yes Os(2) Os(3) Os(4) 58.58(2) ? ? ? yes Os(2) Os(3) Os(5) 56.03(2) ? ? ? yes Os(2) Os(3) Os(6) 104.86(3) ? ? ? yes Os(2) Os(3) C(5) 78.3(5) ? ? ? yes Os(2) Os(3) C(6) 119.6(6) ? ? ? yes Os(2) Os(3) C(7) 143.7(6) ? ? ? yes Os(4) Os(3) Os(5) 59.72(2) ? ? ? yes Os(4) Os(3) Os(6) 61.06(3) ? ? ? yes Os(4) Os(3) C(5) 131.4(5) ? ? ? yes Os(4) Os(3) C(6) 131.8(5) ? ? ? yes Os(4) Os(3) C(7) 103.0(6) ? ? ? yes Os(5) Os(3) Os(6) 57.05(2) ? ? ? yes Os(5) Os(3) C(5) 114.7(6) ? ? ? yes Os(5) Os(3) C(6) 79.8(5) ? ? ? yes Os(5) Os(3) C(7) 145.6(5) ? ? ? yes Os(6) Os(3) C(5) 162.1(6) ? ? ? yes Os(6) Os(3) C(6) 75.8(6) ? ? ? yes Os(6) Os(3) C(7) 88.7(5) ? ? ? yes C(5) Os(3) C(6) 87.2(8) ? ? ? yes C(5) Os(3) C(7) 99.1(8) ? ? ? yes C(6) Os(3) C(7) 96.2(8) ? ? ? yes Os(1) Os(4) Os(2) 57.54(2) ? ? ? yes Os(1) Os(4) Os(3) 59.31(2) ? ? ? yes Os(1) Os(4) Os(5) 105.87(3) ? ? ? yes Os(1) Os(4) Os(6) 117.16(3) ? ? ? yes Os(1) Os(4) C(8) 164.3(5) ? ? ? yes Os(1) Os(4) C(9) 83.1(7) ? ? ? yes Os(1) Os(4) C(10) 79.9(5) ? ? ? yes Os(2) Os(4) Os(3) 62.40(2) ? ? ? yes Os(2) Os(4) Os(5) 57.75(2) ? ? ? yes Os(2) Os(4) Os(6) 107.45(3) ? ? ? yes Os(2) Os(4) C(8) 124.6(6) ? ? ? yes Os(2) Os(4) C(9) 140.5(7) ? ? ? yes Os(2) Os(4) C(10) 83.6(6) ? ? ? yes Os(3) Os(4) Os(5) 61.53(2) ? ? ? yes Os(3) Os(4) Os(6) 60.72(3) ? ? ? yes Os(3) Os(4) C(8) 136.3(5) ? ? ? yes Os(3) Os(4) C(9) 96.5(7) ? ? ? yes Os(3) Os(4) C(10) 136.3(5) ? ? ? yes Os(5) Os(4) Os(6) 57.49(2) ? ? ? yes Os(5) Os(4) C(8) 85.6(5) ? ? ? yes Os(5) Os(4) C(9) 143.3(6) ? ? ? yes Os(5) Os(4) C(10) 123.2(5) ? ? ? yes Os(6) Os(4) C(8) 77.9(6) ? ? ? yes Os(6) Os(4) C(9) 86.5(6) ? ? ? yes Os(6) Os(4) C(10) 162.7(5) ? ? ? yes C(8) Os(4) C(9) 94.1(9) ? ? ? yes C(8) Os(4) C(10) 84.9(8) ? ? ? yes C(9) Os(4) C(10) 93.1(8) ? ? ? yes Os(2) Os(5) Os(3) 62.26(2) ? ? ? yes Os(2) Os(5) Os(4) 60.35(2) ? ? ? yes Os(2) Os(5) Os(6) 113.73(3) ? ? ? yes Os(2) Os(5) S(2) 53.8(1) ? ? ? yes Os(2) Os(5) C(11) 111.6(7) ? ? ? yes Os(2) Os(5) C(12) 147.6(8) ? ? ? yes Os(3) Os(5) Os(4) 58.74(2) ? ? ? yes Os(3) Os(5) Os(6) 61.36(3) ? ? ? yes Os(3) Os(5) S(2) 91.6(1) ? ? ? yes Os(3) Os(5) C(11) 155.6(7) ? ? ? yes Os(3) Os(5) C(12) 105.0(6) ? ? ? yes Os(4) Os(5) Os(6) 62.24(3) ? ? ? yes Os(4) Os(5) S(2) 114.0(1) ? ? ? yes Os(4) Os(5) C(11) 97.3(7) ? ? ? yes Os(4) Os(5) C(12) 141.4(6) ? ? ? yes Os(6) Os(5) S(2) 151.2(1) ? ? ? yes Os(6) Os(5) C(11) 105.6(7) ? ? ? yes Os(6) Os(5) C(12) 79.2(6) ? ? ? yes S(2) Os(5) C(11) 103.3(7) ? ? ? yes S(2) Os(5) C(12) 100.2(7) ? ? ? yes C(11) Os(5) C(12) 91.4(10) ? ? ? yes Os(3) Os(6) Os(4) 58.22(2) ? ? ? yes Os(3) Os(6) Os(5) 61.60(2) ? ? ? yes Os(3) Os(6) C(13) 106.0(7) ? ? ? yes Os(3) Os(6) C(14) 156.2(6) ? ? ? yes Os(3) Os(6) C(15) 101.4(7) ? ? ? yes Os(4) Os(6) Os(5) 60.27(3) ? ? ? yes Os(4) Os(6) C(13) 162.6(6) ? ? ? yes Os(4) Os(6) C(14) 104.4(6) ? ? ? yes Os(4) Os(6) C(15) 97.0(6) ? ? ? yes Os(5) Os(6) C(13) 107.1(6) ? ? ? yes Os(5) Os(6) C(14) 96.2(6) ? ? ? yes Os(5) Os(6) C(15) 156.1(6) ? ? ? yes C(13) Os(6) C(14) 88.2(9) ? ? ? yes C(13) Os(6) C(15) 93.2(8) ? ? ? yes C(14) Os(6) C(15) 96.8(9) ? ? ? yes Os(1) S(1) C(21) 109.7(7) ? ? ? yes Os(1) S(1) C(25) 112.2(6) ? ? ? yes C(21) S(1) C(25) 96(1) ? ? ? yes Os(2) S(2) Os(5) 72.2(1) ? ? ? yes Os(2) S(2) C(16) 119.4(6) ? ? ? yes Os(2) S(2) C(20) 122.2(7) ? ? ? yes Os(5) S(2) C(16) 123.4(6) ? ? ? yes Os(5) S(2) C(20) 122.3(8) ? ? ? yes C(16) S(2) C(20) 98.5(9) ? ? ? yes Os(1) C(1) O(1) 178(2) ? ? ? yes Os(1) C(2) O(2) 174(2) ? ? ? yes Os(2) C(3) O(3) 174(1) ? ? ? yes Os(2) C(4) O(4) 178(1) ? ? ? yes Os(3) C(5) O(5) 169(1) ? ? ? yes Os(3) C(6) O(6) 172(1) ? ? ? yes Os(3) C(7) O(7) 177(1) ? ? ? yes Os(4) C(8) O(8) 176(1) ? ? ? yes Os(4) C(9) O(9) 178(2) ? ? ? yes Os(4) C(10) O(10) 177(1) ? ? ? yes Os(5) C(11) O(11) 178(1) ? ? ? yes Os(5) C(12) O(12) 176(2) ? ? ? yes Os(6) C(13) O(13) 178(1) ? ? ? yes Os(6) C(14) O(14) 177(1) ? ? ? yes Os(6) C(15) O(15) 176(1) ? ? ? yes S(2) C(16) C(17) 110(1) ? ? ? yes C(16) C(17) C(18) 111(1) ? ? ? yes C(17) C(18) C(19) 113(1) ? ? ? yes C(18) C(19) C(20) 115(1) ? ? ? yes S(2) C(20) C(19) 111(1) ? ? ? yes S(1) C(21) C(22) 111(1) ? ? ? yes C(21) C(22) C(23) 111(1) ? ? ? yes C(22) C(23) C(24) 114(2) ? ? ? yes C(23) C(24) C(25) 113(1) ? ? ? yes S(1) C(25) C(24) 109(1) ? ? ? 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_2 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 14:32:52 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.062(1) _cell_length_b 16.484(2) _cell_length_c 18.892(2) _cell_angle_alpha 90 _cell_angle_beta 94.76(1) _cell_angle_gamma 90 _cell_volume 2812.3(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 'Orange' _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 3.479 _exptl_crystal_density_meas ? _chemical_formula_weight 1473.35 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H10 O15 Os5 S ' _chemical_formula_moiety 'C20 H10 O15 Os5 S ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2584.00 _exptl_absorpt_coefficient_mu 22.637 _exptl_absorpt_correction_type 'inter-image 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 23912 _reflns_number_total 5330 _reflns_number_observed 4269 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.55 _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 Os 0 20 -1.216 7.603 'International Tables' C 0 80 0.003 0.002 'International Tables' S 0 4 0.125 0.123 'International Tables' O 0 60 0.011 0.006 'International Tables' H 0 40 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 Os(1) 0.16779(6) 0.03533(4) 0.62651(3) 0.0356(2) Uij ? ? Os(2) 0.23132(6) -0.00102(4) 0.77574(3) 0.0312(2) Uij ? ? Os(3) 0.45446(6) 0.04753(4) 0.68816(3) 0.0357(2) Uij ? ? Os(4) 0.24052(6) 0.15919(4) 0.72268(3) 0.0341(2) Uij ? ? Os(5) 0.46094(6) 0.10623(4) 0.82593(3) 0.0370(2) Uij ? ? S(1) 0.2047(4) -0.0500(2) 0.8953(2) 0.037(1) Uij ? ? O(1) -0.167(1) 0.0394(9) 0.5999(7) 0.071(5) Uij ? ? O(2) 0.167(2) -0.1273(8) 0.5516(8) 0.082(5) Uij ? ? O(3) 0.209(2) 0.1334(9) 0.4943(7) 0.075(5) Uij ? ? O(4) 0.015(1) 0.1121(8) 0.8439(7) 0.070(4) Uij ? ? O(5) 0.001(1) -0.1236(9) 0.7166(7) 0.073(4) Uij ? ? O(6) 0.464(1) -0.1349(8) 0.7701(7) 0.060(4) Uij ? ? O(7) 0.499(2) -0.088(1) 0.5811(8) 0.101(6) Uij ? ? O(8) 0.588(2) 0.1703(9) 0.5930(9) 0.096(6) Uij ? ? O(9) 0.764(1) 0.003(1) 0.7545(7) 0.094(6) Uij ? ? O(10) -0.087(1) 0.2026(9) 0.6876(7) 0.068(4) Uij ? ? O(11) 0.268(2) 0.2935(9) 0.8343(7) 0.085(5) Uij ? ? O(12) 0.334(2) 0.2823(8) 0.6159(7) 0.074(5) Uij ? ? O(13) 0.342(2) 0.1652(9) 0.9624(7) 0.079(5) Uij ? ? O(14) 0.704(1) 0.2342(9) 0.8237(7) 0.076(5) Uij ? ? O(15) 0.649(2) -0.0177(8) 0.9114(8) 0.078(5) Uij ? ? C(1) -0.040(2) 0.0386(10) 0.6129(7) 0.039(4) Uij ? ? C(2) 0.170(2) -0.066(1) 0.5799(8) 0.053(5) Uij ? ? C(3) 0.193(2) 0.0977(10) 0.5451(9) 0.043(5) Uij ? ? C(4) 0.101(2) 0.082(1) 0.8100(8) 0.045(5) Uij ? ? C(5) 0.080(2) -0.0747(10) 0.7354(8) 0.044(5) Uij ? ? C(6) 0.387(2) -0.0798(9) 0.7660(8) 0.040(5) Uij ? ? C(7) 0.474(2) -0.036(1) 0.6195(10) 0.057(6) Uij ? ? C(8) 0.535(2) 0.123(1) 0.628(1) 0.060(6) Uij ? ? C(9) 0.645(2) 0.023(1) 0.7339(8) 0.064(6) Uij ? ? C(10) 0.032(2) 0.184(1) 0.6979(8) 0.053(5) Uij ? ? C(11) 0.264(2) 0.239(1) 0.7965(10) 0.052(5) Uij ? ? C(12) 0.300(2) 0.235(1) 0.6561(8) 0.049(5) Uij ? ? C(13) 0.389(2) 0.144(1) 0.912(1) 0.059(6) Uij ? ? C(14) 0.612(2) 0.188(1) 0.8245(8) 0.044(5) Uij ? ? C(15) 0.580(2) 0.028(1) 0.8787(9) 0.056(6) Uij ? ? C(16) 0.291(2) -0.1472(10) 0.9129(8) 0.047(5) Uij ? ? C(17) 0.255(2) -0.1792(10) 0.9855(9) 0.049(5) Uij ? ? C(18) 0.087(2) -0.194(1) 0.9869(8) 0.061(6) Uij ? ? C(19) -0.004(2) -0.119(1) 0.9712(9) 0.064(6) Uij ? ? C(20) 0.014(2) -0.084(1) 0.8985(9) 0.058(6) Uij ? ? H(1) 0.256 -0.185 0.877 0.056 Uij ? ? H(2) 0.395 -0.142 0.912 0.056 Uij ? ? H(3) 0.306 -0.229 0.995 0.059 Uij ? ? H(4) 0.287 -0.141 1.021 0.059 Uij ? ? H(5) 0.058 -0.234 0.952 0.074 Uij ? ? H(6) 0.069 -0.213 1.033 0.074 Uij ? ? H(7) -0.105 -0.132 0.974 0.076 Uij ? ? H(8) 0.026 -0.079 1.006 0.076 Uij ? ? H(9) -0.051 -0.039 0.890 0.070 Uij ? ? H(10) -0.008 -0.124 0.863 0.070 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 Os(1) 0.0393(3) 0.0441(4) 0.0228(3) -0.0008(3) -0.0015(2) -0.0023(3) Os(2) 0.0351(3) 0.0350(3) 0.0233(3) -0.0003(2) 0.0015(2) 0.0018(2) Os(3) 0.0333(3) 0.0473(4) 0.0267(3) 0.0002(3) 0.0043(2) -0.0001(3) Os(4) 0.0412(3) 0.0340(3) 0.0266(3) 0.0016(2) -0.0009(2) 0.0011(2) Os(5) 0.0391(3) 0.0457(4) 0.0253(3) -0.0046(3) -0.0032(2) 0.0003(3) S(1) 0.045(2) 0.037(2) 0.029(2) -0.002(2) 0.005(2) 0.005(2) O(1) 0.059(8) 0.10(1) 0.054(8) -0.005(7) 0.009(6) -0.001(7) O(2) 0.12(1) 0.050(8) 0.08(1) -0.016(8) 0.001(8) -0.034(8) O(3) 0.089(10) 0.08(1) 0.055(9) -0.001(8) 0.022(7) 0.021(8) O(4) 0.089(9) 0.061(9) 0.069(9) 0.022(7) 0.052(7) 0.018(7) O(5) 0.081(9) 0.077(10) 0.057(8) -0.053(8) -0.016(7) 0.003(7) O(6) 0.073(8) 0.047(8) 0.062(8) 0.009(6) 0.018(6) 0.015(6) O(7) 0.10(1) 0.12(1) 0.09(1) 0.012(10) 0.018(9) -0.07(1) O(8) 0.09(1) 0.09(1) 0.12(1) -0.003(8) 0.054(10) 0.039(10) O(9) 0.048(8) 0.17(2) 0.056(9) 0.025(9) -0.007(6) -0.004(9) O(10) 0.058(8) 0.09(1) 0.060(9) 0.025(7) -0.003(6) 0.009(7) O(11) 0.12(1) 0.067(10) 0.067(10) 0.038(8) -0.025(8) -0.036(8) O(12) 0.10(1) 0.047(8) 0.076(10) -0.012(7) 0.020(8) 0.023(7) O(13) 0.09(1) 0.10(1) 0.043(8) 0.002(8) 0.023(7) -0.020(8) O(14) 0.076(9) 0.072(10) 0.079(10) -0.027(8) -0.004(7) 0.016(8) O(15) 0.10(1) 0.067(9) 0.062(9) 0.020(8) -0.009(8) 0.017(7) C(1) 0.041(9) 0.06(1) 0.016(7) 0.009(7) 0.001(6) -0.002(7) C(2) 0.046(10) 0.08(1) 0.034(9) 0.000(9) -0.009(7) -0.002(9) C(3) 0.045(9) 0.037(9) 0.05(1) -0.009(7) -0.014(7) -0.001(8) C(4) 0.041(9) 0.05(1) 0.044(10) 0.001(7) 0.012(7) 0.011(8) C(5) 0.07(1) 0.035(9) 0.032(9) -0.007(8) 0.000(7) 0.000(7) C(6) 0.053(10) 0.032(9) 0.036(9) 0.004(7) 0.008(7) -0.002(7) C(7) 0.040(10) 0.08(1) 0.05(1) -0.007(9) 0.004(8) -0.01(1) C(8) 0.06(1) 0.06(1) 0.06(1) -0.007(9) 0.007(9) 0.01(1) C(9) 0.05(1) 0.12(2) 0.024(9) 0.01(1) 0.000(7) -0.002(9) C(10) 0.08(1) 0.06(1) 0.022(8) 0.007(10) -0.005(8) 0.008(8) C(11) 0.042(9) 0.05(1) 0.06(1) 0.011(8) -0.007(8) -0.004(9) C(12) 0.07(1) 0.039(10) 0.040(10) 0.001(8) -0.001(8) -0.001(8) C(13) 0.07(1) 0.06(1) 0.05(1) 0.012(9) -0.010(9) 0.003(9) C(14) 0.031(8) 0.05(1) 0.05(1) -0.003(7) -0.001(7) 0.013(8) C(15) 0.08(1) 0.06(1) 0.027(9) 0.000(10) 0.000(8) -0.004(8) C(16) 0.06(1) 0.042(10) 0.041(10) 0.011(8) 0.007(7) 0.002(8) C(17) 0.06(1) 0.041(10) 0.05(1) 0.012(8) 0.000(8) 0.004(8) C(18) 0.10(1) 0.06(1) 0.025(9) 0.00(1) 0.018(9) -0.003(8) C(19) 0.07(1) 0.08(1) 0.05(1) -0.01(1) 0.029(9) 0.007(10) C(20) 0.048(10) 0.08(1) 0.05(1) -0.014(9) 0.011(8) 0.024(10) #------------------------------------------------------------------------------ _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 4269 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0453 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0528 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.489 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min -4.20 _refine_diff_density_max 1.64 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.8928(7) ? ? yes Os(1) Os(3) 2.7647(8) ? ? yes Os(1) Os(4) 2.7759(8) ? ? yes Os(1) C(1) 1.88(1) ? ? yes Os(1) C(2) 1.89(2) ? ? yes Os(1) C(3) 1.88(2) ? ? yes Os(2) Os(3) 2.8322(8) ? ? yes Os(2) Os(4) 2.8284(8) ? ? yes Os(2) Os(5) 2.8332(8) ? ? yes Os(2) S(1) 2.430(4) ? ? yes Os(2) C(4) 1.96(2) ? ? yes Os(2) C(5) 1.94(2) ? ? yes Os(2) C(6) 1.94(2) ? ? yes Os(3) Os(4) 2.7896(8) ? ? yes Os(3) Os(5) 2.7729(8) ? ? yes Os(3) C(7) 1.91(2) ? ? yes Os(3) C(8) 1.87(2) ? ? yes Os(3) C(9) 1.91(2) ? ? yes Os(4) Os(5) 2.8126(8) ? ? yes Os(4) C(10) 1.96(2) ? ? yes Os(4) C(11) 1.92(2) ? ? yes Os(4) C(12) 1.88(2) ? ? yes Os(5) C(13) 1.90(2) ? ? yes Os(5) C(14) 1.92(2) ? ? yes Os(5) C(15) 1.91(2) ? ? yes S(1) C(16) 1.80(2) ? ? yes S(1) C(20) 1.82(2) ? ? yes O(1) C(1) 1.15(2) ? ? yes O(2) C(2) 1.14(2) ? ? yes O(3) C(3) 1.14(2) ? ? yes O(4) C(4) 1.15(2) ? ? yes O(5) C(5) 1.12(2) ? ? yes O(6) C(6) 1.14(2) ? ? yes O(7) C(7) 1.16(2) ? ? yes O(8) C(8) 1.16(2) ? ? yes O(9) C(9) 1.16(2) ? ? yes O(10) C(10) 1.12(2) ? ? yes O(11) C(11) 1.15(2) ? ? yes O(12) C(12) 1.15(2) ? ? yes O(13) C(13) 1.13(2) ? ? yes O(14) C(14) 1.13(2) ? ? yes O(15) C(15) 1.13(2) ? ? yes C(16) C(17) 1.53(2) ? ? yes C(17) C(18) 1.54(2) ? ? yes C(18) C(19) 1.50(3) ? ? yes C(19) C(20) 1.51(2) ? ? 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 Os(2) Os(1) Os(3) 60.03(2) ? ? ? yes Os(2) Os(1) Os(4) 59.82(2) ? ? ? yes Os(2) Os(1) C(1) 104.8(4) ? ? ? yes Os(2) Os(1) C(2) 105.1(5) ? ? ? yes Os(2) Os(1) C(3) 152.0(4) ? ? ? yes Os(3) Os(1) Os(4) 60.46(2) ? ? ? yes Os(3) Os(1) C(1) 162.0(4) ? ? ? yes Os(3) Os(1) C(2) 102.5(5) ? ? ? yes Os(3) Os(1) C(3) 97.5(4) ? ? ? yes Os(4) Os(1) C(1) 104.4(5) ? ? ? yes Os(4) Os(1) C(2) 160.8(5) ? ? ? yes Os(4) Os(1) C(3) 95.4(5) ? ? ? yes C(1) Os(1) C(2) 90.5(7) ? ? ? yes C(1) Os(1) C(3) 93.5(6) ? ? ? yes C(2) Os(1) C(3) 95.6(7) ? ? ? yes Os(1) Os(2) Os(3) 57.74(2) ? ? ? yes Os(1) Os(2) Os(4) 58.04(2) ? ? ? yes Os(1) Os(2) Os(5) 106.15(2) ? ? ? yes Os(1) Os(2) S(1) 161.39(9) ? ? ? yes Os(1) Os(2) C(4) 95.7(5) ? ? ? yes Os(1) Os(2) C(5) 70.7(4) ? ? ? yes Os(1) Os(2) C(6) 97.7(4) ? ? ? yes Os(3) Os(2) Os(4) 59.05(2) ? ? ? yes Os(3) Os(2) Os(5) 58.61(2) ? ? ? yes Os(3) Os(2) S(1) 140.15(9) ? ? ? yes Os(3) Os(2) C(4) 118.3(4) ? ? ? yes Os(3) Os(2) C(5) 117.6(5) ? ? ? yes Os(3) Os(2) C(6) 64.7(4) ? ? ? yes Os(4) Os(2) Os(5) 59.57(2) ? ? ? yes Os(4) Os(2) S(1) 130.40(9) ? ? ? yes Os(4) Os(2) C(4) 59.9(4) ? ? ? yes Os(4) Os(2) C(5) 119.1(5) ? ? ? yes Os(4) Os(2) C(6) 123.3(4) ? ? ? yes Os(5) Os(2) S(1) 91.33(9) ? ? ? yes Os(5) Os(2) C(4) 84.1(5) ? ? ? yes Os(5) Os(2) C(5) 176.2(5) ? ? ? yes Os(5) Os(2) C(6) 85.9(5) ? ? ? yes S(1) Os(2) C(4) 79.4(5) ? ? ? yes S(1) Os(2) C(5) 92.0(4) ? ? ? yes S(1) Os(2) C(6) 89.7(4) ? ? ? yes C(4) Os(2) C(5) 98.2(7) ? ? ? yes C(4) Os(2) C(6) 165.1(6) ? ? ? yes C(5) Os(2) C(6) 92.4(7) ? ? ? yes Os(1) Os(3) Os(2) 62.23(2) ? ? ? yes Os(1) Os(3) Os(4) 59.97(2) ? ? ? yes Os(1) Os(3) Os(5) 111.52(3) ? ? ? yes Os(1) Os(3) C(7) 78.4(5) ? ? ? yes Os(1) Os(3) C(8) 101.0(5) ? ? ? yes Os(1) Os(3) C(9) 163.3(7) ? ? ? yes Os(2) Os(3) Os(4) 60.41(2) ? ? ? yes Os(2) Os(3) Os(5) 60.71(2) ? ? ? yes Os(2) Os(3) C(7) 107.7(5) ? ? ? yes Os(2) Os(3) C(8) 150.9(6) ? ? ? yes Os(2) Os(3) C(9) 109.7(5) ? ? ? yes Os(4) Os(3) Os(5) 60.74(2) ? ? ? yes Os(4) Os(3) C(7) 137.7(5) ? ? ? yes Os(4) Os(3) C(8) 90.8(6) ? ? ? yes Os(4) Os(3) C(9) 130.8(6) ? ? ? yes Os(5) Os(3) C(7) 153.2(6) ? ? ? yes Os(5) Os(3) C(8) 110.9(6) ? ? ? yes Os(5) Os(3) C(9) 72.6(5) ? ? ? yes C(7) Os(3) C(8) 90.4(8) ? ? ? yes C(7) Os(3) C(9) 91.3(8) ? ? ? yes C(8) Os(3) C(9) 92.0(8) ? ? ? yes Os(1) Os(4) Os(2) 62.15(2) ? ? ? yes Os(1) Os(4) Os(3) 59.57(2) ? ? ? yes Os(1) Os(4) Os(5) 110.00(3) ? ? ? yes Os(1) Os(4) C(10) 80.0(5) ? ? ? yes Os(1) Os(4) C(11) 171.0(5) ? ? ? yes Os(1) Os(4) C(12) 96.6(5) ? ? ? yes Os(2) Os(4) Os(3) 60.54(2) ? ? ? yes Os(2) Os(4) Os(5) 60.30(2) ? ? ? yes Os(2) Os(4) C(10) 103.1(5) ? ? ? yes Os(2) Os(4) C(11) 112.8(5) ? ? ? yes Os(2) Os(4) C(12) 151.0(5) ? ? ? yes Os(3) Os(4) Os(5) 59.33(2) ? ? ? yes Os(3) Os(4) C(10) 139.6(5) ? ? ? yes Os(3) Os(4) C(11) 125.8(5) ? ? ? yes Os(3) Os(4) C(12) 92.2(5) ? ? ? yes Os(5) Os(4) C(10) 148.1(5) ? ? ? yes Os(5) Os(4) C(11) 71.2(5) ? ? ? yes Os(5) Os(4) C(12) 116.3(5) ? ? ? yes C(10) Os(4) C(11) 94.4(7) ? ? ? yes C(10) Os(4) C(12) 91.4(7) ? ? ? yes C(11) Os(4) C(12) 90.6(7) ? ? ? yes Os(2) Os(5) Os(3) 60.68(2) ? ? ? yes Os(2) Os(5) Os(4) 60.13(2) ? ? ? yes Os(2) Os(5) C(13) 101.2(6) ? ? ? yes Os(2) Os(5) C(14) 159.5(5) ? ? ? yes Os(2) Os(5) C(15) 96.9(6) ? ? ? yes Os(3) Os(5) Os(4) 59.92(2) ? ? ? yes Os(3) Os(5) C(13) 158.8(5) ? ? ? yes Os(3) Os(5) C(14) 101.0(5) ? ? ? yes Os(3) Os(5) C(15) 102.8(5) ? ? ? yes Os(4) Os(5) C(13) 102.6(5) ? ? ? yes Os(4) Os(5) C(14) 103.9(4) ? ? ? yes Os(4) Os(5) C(15) 155.5(5) ? ? ? yes C(13) Os(5) C(14) 94.6(7) ? ? ? yes C(13) Os(5) C(15) 89.5(7) ? ? ? yes C(14) Os(5) C(15) 96.2(7) ? ? ? yes Os(2) S(1) C(16) 113.1(5) ? ? ? yes Os(2) S(1) C(20) 107.5(6) ? ? ? yes C(16) S(1) C(20) 96.8(8) ? ? ? yes Os(1) C(1) O(1) 175(1) ? ? ? yes Os(1) C(2) O(2) 178(1) ? ? ? yes Os(1) C(3) O(3) 177(1) ? ? ? yes Os(2) C(4) O(4) 158(1) ? ? ? yes Os(2) C(5) O(5) 172(1) ? ? ? yes Os(2) C(6) O(6) 165(1) ? ? ? yes Os(3) C(7) O(7) 173(1) ? ? ? yes Os(3) C(8) O(8) 177(1) ? ? ? yes Os(3) C(9) O(9) 172(1) ? ? ? yes Os(4) C(10) O(10) 174(1) ? ? ? yes Os(4) C(11) O(11) 170(1) ? ? ? yes Os(4) C(12) O(12) 178(1) ? ? ? yes Os(5) C(13) O(13) 178(1) ? ? ? yes Os(5) C(14) O(14) 178(1) ? ? ? yes Os(5) C(15) O(15) 178(1) ? ? ? yes S(1) C(16) C(17) 110(1) ? ? ? yes C(16) C(17) C(18) 110(1) ? ? ? yes C(17) C(18) C(19) 113(1) ? ? ? yes C(18) C(19) C(20) 113(1) ? ? ? yes S(1) C(20) C(19) 108(1) ? ? ? 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_9 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 16:41:04 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 11.976(3) _cell_length_b 13.059(4) _cell_length_c 9.823(2) _cell_angle_alpha 90.43(2) _cell_angle_beta 90.44(2) _cell_angle_gamma 87.36(2) _cell_volume 1534.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 18.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'Brown' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 3.700 _exptl_crystal_density_meas ? _chemical_formula_weight 1709.59 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H8 O16 Os6 S2 ' _chemical_formula_moiety 'C20 H8 O16 Os6 S2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1488.00 _exptl_absorpt_coefficient_mu 24.932 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.449 #------------------------------------------------------------------------------ _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 250 _diffrn_standards_decay_% -4.91 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 3 2 4 2 1 0 4 2 _diffrn_reflns_number 4245 _reflns_number_total 4013 _reflns_number_observed 2535 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 22.50 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00069 _diffrn_orient_matrix_UB_12 -0.04749 _diffrn_orient_matrix_UB_13 0.07941 _diffrn_orient_matrix_UB_21 0.07238 _diffrn_orient_matrix_UB_22 -0.03278 _diffrn_orient_matrix_UB_23 -0.03180 _diffrn_orient_matrix_UB_31 0.04182 _diffrn_orient_matrix_UB_32 0.05046 _diffrn_orient_matrix_UB_33 0.05520 #------------------------------------------------------------------------------ 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 Os 0 12 -1.216 7.603 'International Tables' C 0 40 0.003 0.002 'International Tables' H 0 16 0.000 0.000 'International Tables' S 0 4 0.125 0.123 'International Tables' O 0 32 0.011 0.006 '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 Os(1) 0.9843(1) 0.3314(1) 0.2809(2) 0.0414(6) Uij ? ? Os(2) 0.8927(1) 0.1608(1) 0.1781(2) 0.0399(5) Uij ? ? Os(3) 0.7699(1) 0.2791(1) 0.3785(2) 0.0355(5) Uij ? ? Os(4) 0.7890(1) 0.3489(1) 0.1161(2) 0.0374(5) Uij ? ? Os(5) 0.6709(1) 0.1752(1) 0.1550(2) 0.0368(5) Uij ? ? Os(6) 0.5733(1) 0.3556(1) 0.2414(2) 0.0367(5) Uij ? ? S(1) 0.7747(9) 0.0312(9) 0.205(1) 0.046(3) Uij ? ? S(2) 0.639(1) -0.136(1) 0.101(2) 0.093(6) Uij ? ? O(1) 1.140(3) 0.271(3) 0.516(3) 0.09(2) Uij ? ? O(2) 1.183(4) 0.343(3) 0.094(4) 0.12(2) Uij ? ? O(3) 0.992(3) 0.557(3) 0.362(4) 0.09(1) Uij ? ? O(4) 1.110(3) 0.070(3) 0.300(3) 0.08(1) Uij ? ? O(5) 0.968(3) 0.124(4) -0.103(5) 0.12(2) Uij ? ? O(6) 0.921(3) 0.159(3) 0.582(4) 0.09(1) Uij ? ? O(7) 0.580(3) 0.176(3) 0.523(3) 0.08(1) Uij ? ? O(8) 0.753(3) 0.477(3) 0.543(4) 0.10(2) Uij ? ? O(9) 0.658(3) 0.382(3) -0.147(3) 0.09(1) Uij ? ? O(10) 0.773(2) 0.577(3) 0.198(4) 0.08(1) Uij ? ? O(11) 0.982(3) 0.377(4) -0.084(4) 0.10(2) Uij ? ? O(12) 0.633(3) 0.133(3) -0.146(3) 0.09(1) Uij ? ? O(13) 0.446(4) 0.109(3) 0.236(3) 0.09(2) Uij ? ? O(14) 0.372(3) 0.307(3) 0.402(4) 0.08(1) Uij ? ? O(15) 0.427(3) 0.395(2) 0.000(3) 0.06(1) Uij ? ? O(16) 0.547(3) 0.572(3) 0.349(3) 0.06(1) Uij ? ? C(1) 1.087(5) 0.288(5) 0.434(6) 0.08(2) Uij ? ? C(2) 1.115(4) 0.335(2) 0.180(5) 0.0568 Uij ? ? C(3) 0.992(3) 0.474(4) 0.337(4) 0.05(1) Uij ? ? C(4) 1.030(3) 0.103(3) 0.252(4) 0.04(1) Uij ? ? C(5) 0.939(3) 0.133(4) 0.006(5) 0.06(2) Uij ? ? C(6) 0.877(4) 0.209(4) 0.497(6) 0.07(2) Uij ? ? C(7) 0.649(4) 0.213(5) 0.465(5) 0.12(2) Uij ? ? C(8) 0.761(4) 0.404(4) 0.480(5) 0.06(2) Uij ? ? C(9) 0.701(4) 0.362(3) -0.051(4) 0.05(1) Uij ? ? C(10) 0.771(3) 0.495(4) 0.166(5) 0.05(2) Uij ? ? C(11) 0.914(5) 0.366(3) -0.003(7) 0.0896 Uij ? ? C(12) 0.645(4) 0.146(4) -0.029(5) 0.07(2) Uij ? ? C(13) 0.552(8) 0.145(3) 0.203(3) 0.14(3) Uij ? ? C(14) 0.447(5) 0.328(3) 0.327(6) 0.0762 Uij ? ? C(15) 0.485(3) 0.378(3) 0.096(4) 0.04(1) Uij ? ? C(16) 0.557(4) 0.482(4) 0.302(6) 0.09(2) Uij ? ? C(17) 0.767(4) -0.038(3) 0.363(4) 0.06(2) Uij ? ? C(18) 0.647(3) -0.088(2) 0.387(4) 0.0327 Uij ? ? C(19) 0.652(4) -0.175(3) 0.275(5) 0.07(2) Uij ? ? C(20) 0.768(3) -0.078(3) 0.090(4) 0.05(1) Uij ? ? H(1) 0.8232 -0.0918 0.3619 0.0687 Uij ? ? H(2) 0.7810 0.0079 0.4356 0.0687 Uij ? ? H(3) 0.6412 -0.1147 0.4763 0.0392 Uij ? ? H(4) 0.5862 -0.0392 0.3717 0.0392 Uij ? ? H(5) 0.5933 -0.2194 0.2922 0.0782 Uij ? ? H(6) 0.7219 -0.2117 0.2845 0.0782 Uij ? ? H(7) 0.8257 -0.1268 0.1134 0.0581 Uij ? ? H(8) 0.7778 -0.0552 -0.0002 0.0581 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 Os(1) 0.034(1) 0.046(1) 0.045(1) -0.0081(8) -0.0099(9) 0.0027(9) Os(2) 0.0326(10) 0.040(1) 0.047(1) -0.0005(8) -0.0053(8) -0.0021(9) Os(3) 0.0365(10) 0.039(1) 0.0307(9) -0.0046(8) -0.0075(8) 0.0024(8) Os(4) 0.0344(10) 0.045(1) 0.0328(10) -0.0028(8) -0.0063(8) 0.0083(8) Os(5) 0.0335(10) 0.038(1) 0.039(1) -0.0028(8) -0.0096(8) -0.0010(8) Os(6) 0.0317(10) 0.037(1) 0.041(1) 0.0004(8) -0.0061(8) 0.0046(8) S(1) 0.044(7) 0.033(7) 0.059(8) 0.003(5) -0.005(6) 0.007(6) S(2) 0.09(1) 0.09(1) 0.11(1) -0.027(10) -0.02(1) -0.001(10) O(1) 0.09(3) 0.14(4) 0.04(2) -0.05(3) -0.05(2) 0.01(2) O(2) 0.19(5) 0.09(4) 0.09(3) -0.03(3) 0.07(3) 0.00(3) O(3) 0.11(3) 0.05(3) 0.11(3) -0.02(2) -0.04(3) -0.03(2) O(4) 0.05(2) 0.13(3) 0.06(2) 0.01(2) -0.04(2) -0.03(2) O(5) 0.04(2) 0.17(5) 0.14(4) 0.01(2) 0.06(3) 0.07(3) O(6) 0.11(3) 0.09(3) 0.06(3) 0.00(2) 0.00(2) 0.04(2) O(7) 0.07(2) 0.14(4) 0.04(2) -0.02(2) 0.00(2) 0.02(2) O(8) 0.10(3) 0.07(3) 0.12(3) 0.02(2) 0.00(3) -0.04(3) O(9) 0.11(3) 0.11(3) 0.04(2) -0.02(3) -0.03(2) 0.02(2) O(10) 0.03(2) 0.08(3) 0.12(3) -0.01(2) -0.04(2) 0.03(3) O(11) 0.08(3) 0.17(5) 0.05(2) -0.02(3) 0.04(2) 0.04(2) O(12) 0.09(3) 0.17(4) 0.01(2) -0.01(3) -0.02(2) -0.03(2) O(13) 0.14(4) 0.10(3) 0.03(2) 0.02(3) 0.02(2) 0.01(2) O(14) 0.07(3) 0.08(3) 0.08(3) 0.01(2) -0.01(2) -0.04(2) O(15) 0.06(2) 0.03(2) 0.09(3) 0.01(2) -0.01(2) 0.01(2) O(16) 0.08(2) 0.04(2) 0.07(2) 0.01(2) -0.02(2) 0.00(2) C(1) 0.07(4) 0.12(6) 0.06(4) -0.03(4) 0.00(3) -0.03(4) C(2) 0.12(4) -0.03(2) 0.08(4) -0.01(2) 0.01(3) 0.00(2) C(3) 0.04(3) 0.11(4) 0.00(2) -0.04(3) -0.02(2) 0.00(2) C(4) 0.03(2) 0.03(3) 0.06(3) -0.01(2) 0.01(2) 0.01(2) C(5) 0.00(2) 0.13(5) 0.06(3) 0.04(2) -0.01(2) 0.07(3) C(6) 0.07(4) 0.03(3) 0.11(5) -0.01(3) 0.03(3) 0.02(3) C(7) 0.09(4) 0.24(8) 0.04(3) -0.14(5) 0.07(3) -0.04(4) C(8) 0.03(3) 0.07(4) 0.08(4) 0.04(3) 0.03(3) 0.02(3) C(9) 0.09(4) 0.05(3) 0.01(2) 0.02(3) -0.01(2) 0.03(2) C(10) 0.02(2) 0.07(4) 0.07(3) -0.03(3) 0.01(2) 0.02(3) C(11) 0.11(4) -0.02(2) 0.18(6) 0.03(2) -0.01(4) -0.07(3) C(12) 0.08(4) 0.05(3) 0.07(4) -0.03(3) 0.04(3) -0.01(3) C(13) 0.4(1) 0.01(3) -0.03(2) 0.08(5) 0.08(4) 0.01(2) C(14) 0.11(5) 0.00(2) 0.11(5) 0.06(3) -0.03(4) -0.06(3) C(15) 0.03(3) 0.05(3) 0.05(3) 0.00(2) -0.06(2) -0.01(2) C(16) 0.05(3) 0.06(4) 0.15(5) 0.04(3) 0.01(3) 0.09(4) C(17) 0.08(4) 0.04(3) 0.05(3) -0.03(3) -0.02(3) 0.02(2) C(18) 0.08(3) -0.02(2) 0.04(2) -0.03(2) 0.01(2) 0.02(2) C(19) 0.09(4) 0.03(3) 0.08(4) 0.00(3) -0.03(3) 0.00(3) C(20) 0.05(3) 0.03(3) 0.07(3) -0.03(2) 0.00(2) 0.03(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 2535 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0665 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0665 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.708 _refine_ls_shift/esd_max 0.0140 _refine_ls_shift/esd_mean ? _refine_diff_density_min -3.23 _refine_diff_density_max 3.79 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.713(2) ? ? yes Os(1) Os(3) 2.861(2) ? ? yes Os(1) Os(4) 2.836(2) ? ? yes Os(1) C(1) 2.00(6) ? ? yes Os(1) C(2) 1.86(5) ? ? yes Os(1) C(3) 1.94(5) ? ? yes Os(2) Os(3) 2.865(2) ? ? yes Os(2) Os(4) 2.771(3) ? ? yes Os(2) Os(5) 2.662(2) ? ? yes Os(2) S(1) 2.27(1) ? ? yes Os(2) C(4) 1.92(4) ? ? yes Os(2) C(5) 1.82(5) ? ? yes Os(3) Os(4) 2.755(2) ? ? yes Os(3) Os(5) 2.852(2) ? ? yes Os(3) Os(6) 2.849(2) ? ? yes Os(3) C(6) 1.93(6) ? ? yes Os(3) C(7) 1.93(3) ? ? yes Os(3) C(8) 1.91(6) ? ? yes Os(4) Os(5) 2.759(2) ? ? yes Os(4) Os(6) 2.867(2) ? ? yes Os(4) C(9) 1.95(4) ? ? yes Os(4) C(10) 1.97(6) ? ? yes Os(4) C(11) 1.93(6) ? ? yes Os(5) Os(6) 2.714(2) ? ? yes Os(5) S(1) 2.26(1) ? ? yes Os(5) C(12) 1.87(5) ? ? yes Os(5) C(13) 1.57(9) ? ? yes Os(6) C(14) 1.78(7) ? ? yes Os(6) C(15) 1.79(4) ? ? yes Os(6) C(16) 1.76(6) ? ? yes S(1) C(17) 1.80(4) ? ? yes S(1) C(20) 1.81(4) ? ? yes S(2) C(19) 1.79(5) ? ? yes S(2) C(20) 1.75(4) ? ? yes O(1) C(1) 1.04(6) ? ? yes O(2) C(2) 1.19(5) ? ? yes O(3) C(3) 1.12(6) ? ? yes O(4) C(4) 1.13(5) ? ? yes O(5) C(5) 1.13(5) ? ? yes O(6) C(6) 1.16(6) ? ? yes O(7) C(7) 1.13(4) ? ? yes O(8) C(8) 1.14(5) ? ? yes O(9) C(9) 1.10(4) ? ? yes O(10) C(10) 1.11(5) ? ? yes O(11) C(11) 1.16(6) ? ? yes O(12) C(12) 1.16(5) ? ? yes O(13) C(13) 1.42(9) ? ? yes O(14) C(14) 1.21(6) ? ? yes O(15) C(15) 1.19(4) ? ? yes O(16) C(16) 1.25(6) ? ? yes C(17) C(18) 1.63(5) ? ? yes C(17) H(1) 0.950 ? ? no C(17) H(2) 0.950 ? ? no C(18) C(19) 1.58(5) ? ? yes C(18) H(3) 0.950 ? ? no C(18) H(4) 0.950 ? ? no C(19) H(5) 0.950 ? ? no C(19) H(6) 0.950 ? ? no C(20) H(7) 0.950 ? ? no C(20) H(8) 0.950 ? ? no #------------------------------------------------------------------------------ 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 Os(2) Os(1) Os(3) 61.81(6) ? ? ? yes Os(2) Os(1) Os(4) 59.87(6) ? ? ? yes Os(2) Os(1) C(1) 107(1) ? ? ? yes Os(2) Os(1) C(2) 101(1) ? ? ? yes Os(2) Os(1) C(3) 157(1) ? ? ? yes Os(3) Os(1) Os(4) 57.86(6) ? ? ? yes Os(3) Os(1) C(1) 102(1) ? ? ? yes Os(3) Os(1) C(2) 162(1) ? ? ? yes Os(3) Os(1) C(3) 102(1) ? ? ? yes Os(4) Os(1) C(1) 159(1) ? ? ? yes Os(4) Os(1) C(2) 112(1) ? ? ? yes Os(4) Os(1) C(3) 98(1) ? ? ? yes C(1) Os(1) C(2) 84(2) ? ? ? yes C(1) Os(1) C(3) 90(1) ? ? ? yes C(2) Os(1) C(3) 92(1) ? ? ? yes Os(1) Os(2) Os(3) 61.63(6) ? ? ? yes Os(1) Os(2) Os(4) 62.27(6) ? ? ? yes Os(1) Os(2) Os(5) 114.22(8) ? ? ? yes Os(1) Os(2) S(1) 148.6(3) ? ? ? yes Os(1) Os(2) C(4) 79(1) ? ? ? yes Os(1) Os(2) C(5) 111(1) ? ? ? yes Os(3) Os(2) Os(4) 58.51(6) ? ? ? yes Os(3) Os(2) Os(5) 61.99(6) ? ? ? yes Os(3) Os(2) S(1) 89.6(3) ? ? ? yes Os(3) Os(2) C(4) 111(1) ? ? ? yes Os(3) Os(2) C(5) 153(1) ? ? ? yes Os(4) Os(2) Os(5) 60.99(6) ? ? ? yes Os(4) Os(2) S(1) 114.9(3) ? ? ? yes Os(4) Os(2) C(4) 140(1) ? ? ? yes Os(4) Os(2) C(5) 95(1) ? ? ? yes Os(5) Os(2) S(1) 53.9(3) ? ? ? yes Os(5) Os(2) C(4) 153(1) ? ? ? yes Os(5) Os(2) C(5) 103(1) ? ? ? yes S(1) Os(2) C(4) 102(1) ? ? ? yes S(1) Os(2) C(5) 99(1) ? ? ? yes C(4) Os(2) C(5) 91(1) ? ? ? yes Os(1) Os(3) Os(2) 56.55(6) ? ? ? yes Os(1) Os(3) Os(4) 60.62(6) ? ? ? yes Os(1) Os(3) Os(5) 104.39(7) ? ? ? yes Os(1) Os(3) Os(6) 119.42(8) ? ? ? yes Os(1) Os(3) C(6) 74(1) ? ? ? yes Os(1) Os(3) C(7) 164(2) ? ? ? yes Os(1) Os(3) C(8) 89(1) ? ? ? yes Os(2) Os(3) Os(4) 59.03(6) ? ? ? yes Os(2) Os(3) Os(5) 55.50(6) ? ? ? yes Os(2) Os(3) Os(6) 105.19(7) ? ? ? yes Os(2) Os(3) C(6) 81(1) ? ? ? yes Os(2) Os(3) C(7) 116(1) ? ? ? yes Os(2) Os(3) C(8) 145(1) ? ? ? yes Os(4) Os(3) Os(5) 58.91(6) ? ? ? yes Os(4) Os(3) Os(6) 61.51(6) ? ? ? yes Os(4) Os(3) C(6) 131(1) ? ? ? yes Os(4) Os(3) C(7) 130(1) ? ? ? yes Os(4) Os(3) C(8) 101(1) ? ? ? yes Os(5) Os(3) Os(6) 56.87(6) ? ? ? yes Os(5) Os(3) C(6) 120(1) ? ? ? yes Os(5) Os(3) C(7) 78(1) ? ? ? yes Os(5) Os(3) C(8) 142(1) ? ? ? yes Os(6) Os(3) C(6) 165(1) ? ? ? yes Os(6) Os(3) C(7) 75(2) ? ? ? yes Os(6) Os(3) C(8) 85(1) ? ? ? yes C(6) Os(3) C(7) 90(2) ? ? ? yes C(6) Os(3) C(8) 96(2) ? ? ? yes C(7) Os(3) C(8) 97(2) ? ? ? yes Os(1) Os(4) Os(2) 57.85(6) ? ? ? yes Os(1) Os(4) Os(3) 61.52(6) ? ? ? yes Os(1) Os(4) Os(5) 107.55(8) ? ? ? yes Os(1) Os(4) Os(6) 119.65(7) ? ? ? yes Os(1) Os(4) C(9) 157(1) ? ? ? yes Os(1) Os(4) C(10) 89(1) ? ? ? yes Os(1) Os(4) C(11) 73(1) ? ? ? yes Os(2) Os(4) Os(3) 62.46(6) ? ? ? yes Os(2) Os(4) Os(5) 57.56(6) ? ? ? yes Os(2) Os(4) Os(6) 107.23(7) ? ? ? yes Os(2) Os(4) C(9) 119(1) ? ? ? yes Os(2) Os(4) C(10) 145(1) ? ? ? yes Os(2) Os(4) C(11) 85(1) ? ? ? yes Os(3) Os(4) Os(5) 62.29(6) ? ? ? yes Os(3) Os(4) Os(6) 60.85(6) ? ? ? yes Os(3) Os(4) C(9) 139(1) ? ? ? yes Os(3) Os(4) C(10) 94(1) ? ? ? yes Os(3) Os(4) C(11) 133(1) ? ? ? yes Os(5) Os(4) Os(6) 57.66(6) ? ? ? yes Os(5) Os(4) C(9) 84(1) ? ? ? yes Os(5) Os(4) C(10) 136(1) ? ? ? yes Os(5) Os(4) C(11) 128.2(10) ? ? ? yes Os(6) Os(4) C(9) 83(1) ? ? ? yes Os(6) Os(4) C(10) 78(1) ? ? ? yes Os(6) Os(4) C(11) 165(1) ? ? ? yes C(9) Os(4) C(10) 94(1) ? ? ? yes C(9) Os(4) C(11) 84(2) ? ? ? yes C(10) Os(4) C(11) 94(1) ? ? ? yes Os(2) Os(5) Os(3) 62.51(6) ? ? ? yes Os(2) Os(5) Os(4) 61.45(6) ? ? ? yes Os(2) Os(5) Os(6) 115.17(8) ? ? ? yes Os(2) Os(5) S(1) 54.3(3) ? ? ? yes Os(2) Os(5) C(12) 103(1) ? ? ? yes Os(2) Os(5) C(13) 150(1) ? ? ? yes Os(3) Os(5) Os(4) 58.80(6) ? ? ? yes Os(3) Os(5) Os(6) 61.51(6) ? ? ? yes Os(3) Os(5) S(1) 90.2(3) ? ? ? yes Os(3) Os(5) C(12) 155(1) ? ? ? yes Os(3) Os(5) C(13) 106(1) ? ? ? yes Os(4) Os(5) Os(6) 63.17(6) ? ? ? yes Os(4) Os(5) S(1) 115.7(3) ? ? ? yes Os(4) Os(5) C(12) 96(1) ? ? ? yes Os(4) Os(5) C(13) 139(1) ? ? ? yes Os(6) Os(5) S(1) 148.4(3) ? ? ? yes Os(6) Os(5) C(12) 113(1) ? ? ? yes Os(6) Os(5) C(13) 76(1) ? ? ? yes S(1) Os(5) C(12) 97(1) ? ? ? yes S(1) Os(5) C(13) 101(1) ? ? ? yes C(12) Os(5) C(13) 95(2) ? ? ? yes Os(3) Os(6) Os(4) 57.64(5) ? ? ? yes Os(3) Os(6) Os(5) 61.62(6) ? ? ? yes Os(3) Os(6) C(14) 113(1) ? ? ? yes Os(3) Os(6) C(15) 154(1) ? ? ? yes Os(3) Os(6) C(16) 103(1) ? ? ? yes Os(4) Os(6) Os(5) 59.17(6) ? ? ? yes Os(4) Os(6) C(14) 166(1) ? ? ? yes Os(4) Os(6) C(15) 100(1) ? ? ? yes Os(4) Os(6) C(16) 103(1) ? ? ? yes Os(5) Os(6) C(14) 108(1) ? ? ? yes Os(5) Os(6) C(15) 97(1) ? ? ? yes Os(5) Os(6) C(16) 160(1) ? ? ? yes C(14) Os(6) C(15) 84(2) ? ? ? yes C(14) Os(6) C(16) 88(1) ? ? ? yes C(15) Os(6) C(16) 94(2) ? ? ? yes Os(2) S(1) Os(5) 71.9(3) ? ? ? yes Os(2) S(1) C(17) 122(1) ? ? ? yes Os(2) S(1) C(20) 123(1) ? ? ? yes Os(5) S(1) C(17) 124(1) ? ? ? yes Os(5) S(1) C(20) 118(1) ? ? ? yes C(17) S(1) C(20) 97(1) ? ? ? yes C(19) S(2) C(20) 97(2) ? ? ? yes Os(1) C(1) O(1) 175(5) ? ? ? yes Os(1) C(2) O(2) 166(4) ? ? ? yes Os(1) C(3) O(3) 176(3) ? ? ? yes Os(2) C(4) O(4) 177(3) ? ? ? yes Os(2) C(5) O(5) 174(5) ? ? ? yes Os(3) C(6) O(6) 165(4) ? ? ? yes Os(3) C(7) O(7) 176(4) ? ? ? yes Os(3) C(8) O(8) 177(4) ? ? ? yes Os(4) C(9) O(9) 170(4) ? ? ? yes Os(4) C(10) O(10) 172(4) ? ? ? yes Os(4) C(11) O(11) 173(5) ? ? ? yes Os(5) C(12) O(12) 176(4) ? ? ? yes Os(5) C(13) O(13) 173(3) ? ? ? yes Os(6) C(14) O(14) 170(4) ? ? ? yes Os(6) C(15) O(15) 178(3) ? ? ? yes Os(6) C(16) O(16) 178(4) ? ? ? yes S(1) C(17) C(18) 113(2) ? ? ? yes S(1) C(17) H(1) 108.4 ? ? ? no S(1) C(17) H(2) 108.4 ? ? ? no C(18) C(17) H(1) 108.4 ? ? ? no C(18) C(17) H(2) 108.4 ? ? ? no H(1) C(17) H(2) 109.5 ? ? ? no C(17) C(18) C(19) 99(3) ? ? ? yes C(17) C(18) H(3) 111.9 ? ? ? no C(17) C(18) H(4) 111.8 ? ? ? no C(19) C(18) H(3) 111.9 ? ? ? no C(19) C(18) H(4) 111.8 ? ? ? no H(3) C(18) H(4) 109.5 ? ? ? no S(2) C(19) C(18) 117(2) ? ? ? yes S(2) C(19) H(5) 107.6 ? ? ? no S(2) C(19) H(6) 107.5 ? ? ? no C(18) C(19) H(5) 107.6 ? ? ? no C(18) C(19) H(6) 107.5 ? ? ? no H(5) C(19) H(6) 109.5 ? ? ? no S(1) C(20) S(2) 111(2) ? ? ? yes S(1) C(20) H(7) 108.9 ? ? ? no S(1) C(20) H(8) 108.9 ? ? ? no S(2) C(20) H(7) 108.9 ? ? ? no S(2) C(20) H(8) 108.9 ? ? ? no H(7) C(20) H(8) 109.5 ? ? ? no #------------------------------------------------------------------------------ _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_4 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 14:39:51 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.181(1) _cell_length_b 28.787(1) _cell_length_c 16.533(1) _cell_angle_alpha 90 _cell_angle_beta 102.38(1) _cell_angle_gamma 90 _cell_volume 4268.0(6) _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 'Brown' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 2.919 _exptl_crystal_density_meas ? _chemical_formula_weight 1875.89 _chemical_formula_analytical ? _chemical_formula_sum 'C27.50 H20 O16 Os6 S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3332.00 _exptl_absorpt_coefficient_mu 18.038 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _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 'unknown' _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 17557 _reflns_number_total 6612 _reflns_number_observed 3556 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.115 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.53 _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 Os 0 24 -1.216 7.603 'International Tables' C 0 110 0.003 0.002 'International Tables' O 0 64 0.011 0.006 'International Tables' S 0 16 0.125 0.123 'International Tables' H 0 80 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 Os(1) 0.6687(2) 0.17553(6) 0.4291(1) 0.0575(5) Uij ? ? Os(2) 0.8639(1) 0.09729(5) 0.43386(8) 0.0446(4) Uij ? ? Os(3) 0.5695(1) 0.09221(5) 0.34437(8) 0.0404(4) Uij ? ? Os(4) 0.7752(1) 0.14854(5) 0.28922(9) 0.0437(4) Uij ? ? Os(5) 0.8004(1) 0.05175(5) 0.28377(8) 0.0429(4) Uij ? ? Os(6) 0.5590(2) 0.09854(5) 0.17442(8) 0.0454(4) Uij ? ? S(1) 0.610(1) 0.1713(4) 0.5613(7) 0.081(4) Uij ? ? S(2) 0.415(2) 0.2354(5) 0.6771(9) 0.114(6) Uij ? ? S(3) 0.646(1) 0.1055(3) 0.0484(6) 0.055(3) Uij ? ? S(4) 0.540(2) 0.1476(5) -0.1493(8) 0.112(5) Uij ? ? O(1) 0.868(4) 0.259(1) 0.475(2) 0.14(2) Uij ? ? O(2) 0.408(4) 0.238(1) 0.360(2) 0.11(1) Uij ? ? O(3) 0.971(3) 0.160(1) 0.585(2) 0.10(1) Uij ? ? O(4) 0.850(3) 0.018(1) 0.544(2) 0.09(1) Uij ? ? O(5) 1.199(3) 0.089(1) 0.436(2) 0.08(1) Uij ? ? O(6) 0.274(3) 0.145(1) 0.296(2) 0.09(1) Uij ? ? O(7) 0.521(3) 0.0642(10) 0.514(1) 0.065(9) Uij ? ? O(8) 0.430(3) -0.001(1) 0.299(2) 0.08(1) Uij ? ? O(9) 1.044(3) 0.2051(10) 0.376(2) 0.075(10) Uij ? ? O(10) 0.957(3) 0.138(1) 0.158(1) 0.075(10) Uij ? ? O(11) 0.587(3) 0.230(1) 0.212(2) 0.09(1) Uij ? ? O(12) 0.803(3) -0.0419(10) 0.370(2) 0.07(1) Uij ? ? O(13) 1.116(3) 0.046(1) 0.255(2) 0.09(1) Uij ? ? O(14) 0.721(3) -0.0010(9) 0.118(1) 0.076(10) Uij ? ? O(15) 0.335(3) 0.024(1) 0.106(2) 0.09(1) Uij ? ? O(16) 0.316(3) 0.172(1) 0.123(2) 0.09(1) Uij ? ? C(1) 0.790(5) 0.229(2) 0.461(2) 0.08(2) Uij ? ? C(2) 0.503(5) 0.215(2) 0.385(3) 0.08(2) Uij ? ? C(3) 0.924(3) 0.140(1) 0.527(2) 0.05(1) Uij ? ? C(4) 0.856(4) 0.051(1) 0.503(2) 0.05(1) Uij ? ? C(5) 1.080(5) 0.092(2) 0.436(2) 0.07(1) Uij ? ? C(6) 0.389(5) 0.126(1) 0.317(2) 0.06(1) Uij ? ? C(7) 0.543(3) 0.078(1) 0.448(2) 0.05(1) Uij ? ? C(8) 0.483(5) 0.033(1) 0.310(2) 0.07(1) Uij ? ? C(9) 0.945(4) 0.179(1) 0.343(2) 0.05(1) Uij ? ? C(10) 0.880(3) 0.140(1) 0.204(2) 0.07(1) Uij ? ? C(11) 0.659(4) 0.199(1) 0.246(2) 0.07(1) Uij ? ? C(12) 0.792(4) -0.004(1) 0.336(3) 0.07(1) Uij ? ? C(13) 1.000(5) 0.049(1) 0.267(3) 0.08(2) Uij ? ? C(14) 0.735(4) 0.021(2) 0.178(2) 0.06(1) Uij ? ? C(15) 0.425(3) 0.052(2) 0.132(2) 0.06(1) Uij ? ? C(16) 0.414(5) 0.145(2) 0.142(3) 0.08(2) Uij ? ? C(17) 0.406(5) 0.175(2) 0.552(4) 0.17(3) Uij ? ? C(18) 0.363(5) 0.184(2) 0.626(4) 0.15(2) Uij ? ? C(19) 0.624(7) 0.235(3) 0.693(4) 0.17(3) Uij ? ? C(20) 0.660(4) 0.228(2) 0.612(3) 0.14(2) Uij ? ? C(21) 0.507(5) 0.084(1) -0.035(2) 0.08(1) Uij ? ? C(22) 0.547(6) 0.089(2) -0.124(2) 0.11(2) Uij ? ? C(23) 0.677(5) 0.173(1) -0.065(3) 0.09(2) Uij ? ? C(24) 0.639(5) 0.168(1) 0.022(2) 0.08(2) Uij ? ? C(25) 0.001(7) 0.045(2) 1.011(3) 0.333(10) Uij 0.5 ? C(26) 0.009(4) 0.075(1) 0.936(2) 0.3333 Uij 0.5 ? C(27) -0.060(4) 0.061(1) 0.857(3) 0.3333 Uij 0.5 ? C(28) -0.052(5) 0.089(2) 0.788(2) 0.3333 Uij 0.5 ? C(29) 0.024(5) 0.131(2) 0.800(3) 0.3333 Uij 0.5 ? C(30) 0.093(5) 0.145(1) 0.880(4) 0.3333 Uij 0.5 ? C(31) 0.085(4) 0.118(1) 0.948(3) 0.3333 Uij 0.5 ? H(1) 0.3684 0.1982 0.5136 0.2022 Uij ? ? H(2) 0.3646 0.1455 0.5322 0.2022 Uij ? ? H(3) 0.4007 0.1598 0.6631 0.1818 Uij ? ? H(4) 0.2570 0.1834 0.6137 0.1818 Uij ? ? H(5) 0.6638 0.2631 0.7168 0.2026 Uij ? ? H(6) 0.6634 0.2097 0.7285 0.2026 Uij ? ? H(7) 0.7641 0.2327 0.6183 0.1676 Uij ? ? H(8) 0.6082 0.2517 0.5762 0.1676 Uij ? ? H(9) 0.4924 0.0521 -0.0248 0.0920 Uij ? ? H(10) 0.4176 0.1007 -0.0355 0.0920 Uij ? ? H(11) 0.4762 0.0721 -0.1637 0.1329 Uij ? ? H(12) 0.6439 0.0769 -0.1222 0.1329 Uij ? ? H(13) 0.7701 0.1579 -0.0626 0.1034 Uij ? ? H(14) 0.6862 0.2050 -0.0759 0.1034 Uij ? ? H(15) 0.5417 0.1802 0.0207 0.1014 Uij ? ? H(21) 0.709(4) 0.185(1) 0.062(2) 0.101(10) Uij ? ? H(22) -0.101(4) 0.040(1) 1.014(2) 0.400(10) Uij 0.5 ? H(23) 0.044(4) 0.015(1) 1.005(2) 0.400(10) Uij 0.5 ? H(24) 0.053(4) 0.059(1) 1.060(2) 0.400(10) Uij 0.5 ? H(25) -0.112(4) 0.032(1) 0.849(2) 0.400(10) Uij 0.5 ? H(26) -0.099(4) 0.079(1) 0.734(2) 0.400(10) Uij 0.5 ? H(27) 0.029(4) 0.150(1) 0.754(2) 0.400(10) Uij 0.5 ? H(28) 0.145(4) 0.174(1) 0.888(2) 0.400(10) Uij 0.5 ? H(29) 0.132(4) 0.127(1) 1.002(2) 0.400(10) Uij 0.5 ? 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 Os(1) 0.0433(9) 0.059(1) 0.069(1) 0.0001(8) 0.0079(8) -0.0221(8) Os(2) 0.0336(8) 0.0525(9) 0.0463(8) -0.0005(7) 0.0057(7) -0.0005(7) Os(3) 0.0307(8) 0.0441(8) 0.0457(8) -0.0006(7) 0.0066(6) -0.0019(7) Os(4) 0.0362(8) 0.0421(8) 0.0525(9) -0.0025(7) 0.0086(7) 0.0014(7) Os(5) 0.0355(8) 0.0444(9) 0.0474(9) 0.0050(6) 0.0058(7) -0.0006(7) Os(6) 0.0403(8) 0.0479(9) 0.0453(8) 0.0031(7) 0.0036(7) -0.0010(7) S(1) 0.052(7) 0.105(9) 0.090(8) -0.007(6) 0.023(6) -0.047(7) S(2) 0.11(1) 0.10(1) 0.15(1) 0.001(9) 0.071(10) -0.044(9) S(3) 0.057(6) 0.053(6) 0.055(6) 0.009(5) 0.014(5) 0.004(5) S(4) 0.13(1) 0.14(1) 0.063(8) 0.00(1) 0.007(8) 0.031(8) O(1) 0.14(3) 0.11(3) 0.16(4) -0.09(3) 0.04(3) -0.07(3) O(2) 0.10(3) 0.09(3) 0.12(3) 0.04(2) 0.00(2) 0.00(2) O(3) 0.06(2) 0.16(3) 0.07(2) 0.01(2) -0.01(2) -0.08(2) O(4) 0.06(2) 0.13(3) 0.10(2) -0.01(2) 0.02(2) 0.02(2) O(5) 0.03(2) 0.11(3) 0.11(2) 0.01(2) 0.03(2) 0.00(2) O(6) 0.07(2) 0.10(3) 0.08(2) 0.04(2) 0.03(2) 0.00(2) O(7) 0.05(2) 0.11(2) 0.04(1) -0.01(2) 0.02(1) 0.01(1) O(8) 0.05(2) 0.06(2) 0.12(3) 0.00(2) 0.00(2) 0.01(2) O(9) 0.04(2) 0.09(2) 0.09(2) -0.01(1) -0.01(1) -0.01(2) O(10) 0.07(2) 0.12(2) 0.05(2) -0.03(2) 0.04(1) 0.00(2) O(11) 0.06(2) 0.09(2) 0.13(3) 0.03(2) 0.01(2) 0.03(2) O(12) 0.06(2) 0.10(2) 0.07(2) 0.02(2) 0.02(1) 0.00(2) O(13) 0.05(2) 0.12(3) 0.11(2) -0.01(2) 0.03(2) -0.02(2) O(14) 0.09(2) 0.08(2) 0.05(2) 0.01(2) -0.02(2) -0.02(1) O(15) 0.04(2) 0.11(3) 0.10(2) -0.03(2) -0.02(2) 0.00(2) O(16) 0.05(2) 0.12(3) 0.11(3) 0.04(2) 0.02(2) 0.01(2) C(1) 0.06(3) 0.11(4) 0.06(3) 0.03(3) -0.01(2) -0.05(3) C(2) 0.07(3) 0.08(3) 0.10(4) 0.02(2) 0.05(3) -0.02(3) C(3) 0.03(2) 0.10(3) 0.04(2) 0.01(2) 0.03(2) 0.02(2) C(4) 0.06(2) 0.07(3) 0.04(2) -0.03(2) 0.03(2) 0.04(2) C(5) 0.06(3) 0.12(4) 0.03(2) 0.00(3) 0.01(2) -0.02(2) C(6) 0.08(3) 0.03(2) 0.07(3) -0.01(2) 0.05(3) 0.01(2) C(7) 0.05(2) 0.05(2) 0.05(2) 0.01(2) 0.04(2) 0.00(2) C(8) 0.15(4) 0.04(2) 0.04(2) -0.02(3) 0.04(3) 0.02(2) C(9) 0.05(2) 0.09(3) 0.03(2) 0.00(2) 0.02(2) 0.01(2) C(10) 0.01(2) 0.10(3) 0.08(3) -0.04(2) -0.02(2) 0.00(2) C(11) 0.06(3) 0.08(3) 0.04(2) 0.00(2) -0.02(2) 0.03(2) C(12) 0.05(2) 0.03(2) 0.11(3) -0.04(2) 0.00(2) 0.02(2) C(13) 0.08(3) 0.07(3) 0.09(3) -0.02(3) 0.05(3) -0.03(2) C(14) 0.02(2) 0.11(4) 0.05(2) 0.02(2) 0.00(2) -0.01(2) C(15) 0.02(2) 0.17(4) -0.01(1) 0.00(2) 0.01(1) 0.02(2) C(16) 0.07(3) 0.09(4) 0.07(3) -0.02(3) 0.01(3) -0.03(3) C(17) 0.06(3) 0.15(5) 0.33(9) -0.02(3) 0.11(5) -0.13(6) C(18) 0.03(3) 0.21(6) 0.22(6) -0.04(3) 0.05(3) -0.17(5) C(19) 0.15(6) 0.21(8) 0.17(6) -0.09(5) 0.07(5) 0.00(5) C(20) 0.06(3) 0.24(6) 0.14(4) -0.12(4) 0.07(3) -0.19(5) C(21) 0.09(3) 0.07(3) 0.07(3) -0.02(2) 0.03(3) -0.02(2) C(22) 0.21(6) 0.09(4) 0.06(3) -0.08(4) 0.08(3) -0.02(2) C(23) 0.07(3) 0.05(3) 0.14(4) 0.01(2) 0.04(3) -0.01(3) C(24) 0.14(4) 0.08(3) 0.05(2) 0.02(3) 0.07(3) 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3556 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0651 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0703 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.970 _refine_ls_shift/esd_max 0.0140 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.16 _refine_diff_density_max 1.10 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.869(2) ? ? yes Os(1) Os(3) 2.829(2) ? ? yes Os(1) Os(4) 2.808(2) ? ? yes Os(1) S(1) 2.36(1) ? ? yes Os(1) C(1) 1.92(5) ? ? yes Os(1) C(2) 1.91(4) ? ? yes Os(2) Os(3) 2.794(2) ? ? yes Os(2) Os(4) 2.779(2) ? ? yes Os(2) Os(5) 2.756(2) ? ? yes Os(2) C(3) 1.95(4) ? ? yes Os(2) C(4) 1.77(4) ? ? yes Os(2) C(5) 1.98(4) ? ? yes Os(3) Os(4) 2.787(2) ? ? yes Os(3) Os(5) 2.786(2) ? ? yes Os(3) Os(6) 2.797(2) ? ? yes Os(3) C(6) 1.89(4) ? ? yes Os(3) C(7) 1.84(3) ? ? yes Os(3) C(8) 1.91(4) ? ? yes Os(4) Os(5) 2.799(2) ? ? yes Os(4) Os(6) 2.828(2) ? ? yes Os(4) C(9) 1.85(3) ? ? yes Os(4) C(10) 1.89(4) ? ? yes Os(4) C(11) 1.85(4) ? ? yes Os(5) Os(6) 2.876(2) ? ? yes Os(5) C(12) 1.83(4) ? ? yes Os(5) C(13) 1.91(5) ? ? yes Os(5) C(14) 1.94(4) ? ? yes Os(6) S(3) 2.39(1) ? ? yes Os(6) C(15) 1.85(4) ? ? yes Os(6) C(16) 1.88(5) ? ? yes S(1) C(17) 1.85(5) ? ? yes S(1) C(20) 1.86(6) ? ? yes S(2) C(18) 1.72(6) ? ? yes S(2) C(19) 1.88(6) ? ? yes S(3) C(21) 1.77(4) ? ? yes S(3) C(24) 1.85(4) ? ? yes S(4) C(22) 1.74(5) ? ? yes S(4) C(23) 1.82(4) ? ? yes O(1) C(1) 1.11(6) ? ? yes O(2) C(2) 1.10(5) ? ? yes O(3) C(3) 1.12(4) ? ? yes O(4) C(4) 1.17(5) ? ? yes O(5) C(5) 1.10(5) ? ? yes O(6) C(6) 1.18(5) ? ? yes O(7) C(7) 1.20(4) ? ? yes O(8) C(8) 1.10(5) ? ? yes O(9) C(9) 1.21(4) ? ? yes O(10) C(10) 1.15(5) ? ? yes O(11) C(11) 1.19(5) ? ? yes O(12) C(12) 1.22(5) ? ? yes O(13) C(13) 1.13(6) ? ? yes O(14) C(14) 1.16(5) ? ? yes O(15) C(15) 1.18(5) ? ? yes O(16) C(16) 1.17(6) ? ? yes C(17) C(18) 1.39(10) ? ? yes C(19) C(20) 1.46(8) ? ? yes C(21) C(22) 1.60(6) ? ? yes C(23) C(24) 1.55(7) ? ? yes C(26) C(27) 1.39(6) ? ? yes C(26) C(31) 1.39(5) ? ? yes C(26) C(25) 1.54(7) ? ? yes C(27) C(28) 1.39(7) ? ? yes C(28) C(29) 1.39(8) ? ? yes C(29) C(30) 1.39(8) ? ? yes C(30) C(31) 1.39(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 Os(2) Os(1) Os(3) 58.72(5) ? ? ? yes Os(2) Os(1) Os(4) 58.61(5) ? ? ? yes Os(2) Os(1) S(1) 101.4(3) ? ? ? yes Os(2) Os(1) C(1) 107(1) ? ? ? yes Os(2) Os(1) C(2) 156(1) ? ? ? yes Os(3) Os(1) Os(4) 59.27(5) ? ? ? yes Os(3) Os(1) S(1) 107.6(3) ? ? ? yes Os(3) Os(1) C(1) 158(1) ? ? ? yes Os(3) Os(1) C(2) 99(1) ? ? ? yes Os(4) Os(1) S(1) 159.4(3) ? ? ? yes Os(4) Os(1) C(1) 99(1) ? ? ? yes Os(4) Os(1) C(2) 103(1) ? ? ? yes S(1) Os(1) C(1) 91(1) ? ? ? yes S(1) Os(1) C(2) 93(1) ? ? ? yes C(1) Os(1) C(2) 89(1) ? ? ? yes Os(1) Os(2) Os(3) 59.92(4) ? ? ? yes Os(1) Os(2) Os(4) 59.59(5) ? ? ? yes Os(1) Os(2) Os(5) 109.79(6) ? ? ? yes Os(1) Os(2) C(3) 66.4(10) ? ? ? yes Os(1) Os(2) C(4) 119(1) ? ? ? yes Os(1) Os(2) C(5) 132(1) ? ? ? yes Os(3) Os(2) Os(4) 60.02(5) ? ? ? yes Os(3) Os(2) Os(5) 60.27(5) ? ? ? yes Os(3) Os(2) C(3) 121.9(10) ? ? ? yes Os(3) Os(2) C(4) 97(1) ? ? ? yes Os(3) Os(2) C(5) 148.9(10) ? ? ? yes Os(4) Os(2) Os(5) 60.75(5) ? ? ? yes Os(4) Os(2) C(3) 109(1) ? ? ? yes Os(4) Os(2) C(4) 155.8(10) ? ? ? yes Os(4) Os(2) C(5) 99(1) ? ? ? yes Os(5) Os(2) C(3) 168(1) ? ? ? yes Os(5) Os(2) C(4) 101(1) ? ? ? yes Os(5) Os(2) C(5) 89(1) ? ? ? yes C(3) Os(2) C(4) 90(1) ? ? ? yes C(3) Os(2) C(5) 85(1) ? ? ? yes C(4) Os(2) C(5) 96(1) ? ? ? yes Os(1) Os(3) Os(2) 61.37(4) ? ? ? yes Os(1) Os(3) Os(4) 59.99(5) ? ? ? yes Os(1) Os(3) Os(5) 110.10(5) ? ? ? yes Os(1) Os(3) Os(6) 112.37(6) ? ? ? yes Os(1) Os(3) C(6) 81(1) ? ? ? yes Os(1) Os(3) C(7) 79(1) ? ? ? yes Os(1) Os(3) C(8) 166(1) ? ? ? yes Os(2) Os(3) Os(4) 59.73(5) ? ? ? yes Os(2) Os(3) Os(5) 59.20(5) ? ? ? yes Os(2) Os(3) Os(6) 110.46(6) ? ? ? yes Os(2) Os(3) C(6) 143(1) ? ? ? yes Os(2) Os(3) C(7) 79.9(9) ? ? ? yes Os(2) Os(3) C(8) 119(1) ? ? ? yes Os(4) Os(3) Os(5) 60.29(5) ? ? ? yes Os(4) Os(3) Os(6) 60.86(5) ? ? ? yes Os(4) Os(3) C(6) 104(1) ? ? ? yes Os(4) Os(3) C(7) 132.4(10) ? ? ? yes Os(4) Os(3) C(8) 133(1) ? ? ? yes Os(5) Os(3) Os(6) 62.02(5) ? ? ? yes Os(5) Os(3) C(6) 145(1) ? ? ? yes Os(5) Os(3) C(7) 120(1) ? ? ? yes Os(5) Os(3) C(8) 79(1) ? ? ? yes Os(6) Os(3) C(6) 83(1) ? ? ? yes Os(6) Os(3) C(7) 166.6(10) ? ? ? yes Os(6) Os(3) C(8) 80(1) ? ? ? yes C(6) Os(3) C(7) 93(1) ? ? ? yes C(6) Os(3) C(8) 95(1) ? ? ? yes C(7) Os(3) C(8) 87(1) ? ? ? yes Os(1) Os(4) Os(2) 61.80(5) ? ? ? yes Os(1) Os(4) Os(3) 60.74(5) ? ? ? yes Os(1) Os(4) Os(5) 110.35(7) ? ? ? yes Os(1) Os(4) Os(6) 112.05(6) ? ? ? yes Os(1) Os(4) C(9) 82(1) ? ? ? yes Os(1) Os(4) C(10) 167(1) ? ? ? yes Os(1) Os(4) C(11) 80(1) ? ? ? yes Os(2) Os(4) Os(3) 60.25(5) ? ? ? yes Os(2) Os(4) Os(5) 59.22(5) ? ? ? yes Os(2) Os(4) Os(6) 109.96(6) ? ? ? yes Os(2) Os(4) C(9) 77(1) ? ? ? yes Os(2) Os(4) C(10) 118(1) ? ? ? yes Os(2) Os(4) C(11) 141(1) ? ? ? yes Os(3) Os(4) Os(5) 59.84(5) ? ? ? yes Os(3) Os(4) Os(6) 59.74(5) ? ? ? yes Os(3) Os(4) C(9) 133(1) ? ? ? yes Os(3) Os(4) C(10) 131(1) ? ? ? yes Os(3) Os(4) C(11) 101(1) ? ? ? yes Os(5) Os(4) Os(6) 61.48(5) ? ? ? yes Os(5) Os(4) C(9) 115(1) ? ? ? yes Os(5) Os(4) C(10) 77(1) ? ? ? yes Os(5) Os(4) C(11) 144(1) ? ? ? yes Os(6) Os(4) C(9) 165(1) ? ? ? yes Os(6) Os(4) C(10) 80.2(10) ? ? ? yes Os(6) Os(4) C(11) 82(1) ? ? ? yes C(9) Os(4) C(10) 84(1) ? ? ? yes C(9) Os(4) C(11) 99(1) ? ? ? yes C(10) Os(4) C(11) 98(1) ? ? ? yes Os(2) Os(5) Os(3) 60.53(5) ? ? ? yes Os(2) Os(5) Os(4) 60.03(5) ? ? ? yes Os(2) Os(5) Os(6) 109.21(6) ? ? ? yes Os(2) Os(5) C(12) 90(1) ? ? ? yes Os(2) Os(5) C(13) 97(1) ? ? ? yes Os(2) Os(5) C(14) 174(1) ? ? ? yes Os(3) Os(5) Os(4) 59.87(5) ? ? ? yes Os(3) Os(5) Os(6) 59.16(5) ? ? ? yes Os(3) Os(5) C(12) 94(1) ? ? ? yes Os(3) Os(5) C(13) 153(1) ? ? ? yes Os(3) Os(5) C(14) 113(1) ? ? ? yes Os(4) Os(5) Os(6) 59.76(5) ? ? ? yes Os(4) Os(5) C(12) 147(1) ? ? ? yes Os(4) Os(5) C(13) 97(1) ? ? ? yes Os(4) Os(5) C(14) 118(1) ? ? ? yes Os(6) Os(5) C(12) 127(1) ? ? ? yes Os(6) Os(5) C(13) 124(1) ? ? ? yes Os(6) Os(5) C(14) 66(1) ? ? ? yes C(12) Os(5) C(13) 99(1) ? ? ? yes C(12) Os(5) C(14) 89(1) ? ? ? yes C(13) Os(5) C(14) 88(1) ? ? ? yes Os(3) Os(6) Os(4) 59.40(5) ? ? ? yes Os(3) Os(6) Os(5) 58.82(5) ? ? ? yes Os(3) Os(6) S(3) 159.1(2) ? ? ? yes Os(3) Os(6) C(15) 102.0(9) ? ? ? yes Os(3) Os(6) C(16) 101(1) ? ? ? yes Os(4) Os(6) Os(5) 58.76(5) ? ? ? yes Os(4) Os(6) S(3) 103.0(2) ? ? ? yes Os(4) Os(6) C(15) 159.4(10) ? ? ? yes Os(4) Os(6) C(16) 100(1) ? ? ? yes Os(5) Os(6) S(3) 103.4(2) ? ? ? yes Os(5) Os(6) C(15) 105(1) ? ? ? yes Os(5) Os(6) C(16) 156(1) ? ? ? yes S(3) Os(6) C(15) 93.1(9) ? ? ? yes S(3) Os(6) C(16) 92(1) ? ? ? yes C(15) Os(6) C(16) 91(1) ? ? ? yes Os(1) S(1) C(17) 110(2) ? ? ? yes Os(1) S(1) C(20) 106(1) ? ? ? yes C(17) S(1) C(20) 97(2) ? ? ? yes C(18) S(2) C(19) 103(2) ? ? ? yes Os(6) S(3) C(21) 109(1) ? ? ? yes Os(6) S(3) C(24) 106(1) ? ? ? yes C(21) S(3) C(24) 100(1) ? ? ? yes C(22) S(4) C(23) 102(1) ? ? ? yes Os(1) C(1) O(1) 173(4) ? ? ? yes Os(1) C(2) O(2) 179(3) ? ? ? yes Os(2) C(3) O(3) 171(3) ? ? ? yes Os(2) C(4) O(4) 174(3) ? ? ? yes Os(2) C(5) O(5) 179(3) ? ? ? yes Os(3) C(6) O(6) 175(3) ? ? ? yes Os(3) C(7) O(7) 173(2) ? ? ? yes Os(3) C(8) O(8) 171(3) ? ? ? yes Os(4) C(9) O(9) 171(3) ? ? ? yes Os(4) C(10) O(10) 171(2) ? ? ? yes Os(4) C(11) O(11) 175(3) ? ? ? yes Os(5) C(12) O(12) 172(3) ? ? ? yes Os(5) C(13) O(13) 177(3) ? ? ? yes Os(5) C(14) O(14) 167(2) ? ? ? yes Os(6) C(15) O(15) 177(3) ? ? ? yes Os(6) C(16) O(16) 174(4) ? ? ? yes S(1) C(17) C(18) 114(3) ? ? ? yes S(2) C(18) C(17) 120(4) ? ? ? yes S(2) C(19) C(20) 107(3) ? ? ? yes S(1) C(20) C(19) 116(4) ? ? ? yes S(3) C(21) C(22) 114(3) ? ? ? yes S(4) C(22) C(21) 107(2) ? ? ? yes S(4) C(23) C(24) 114(2) ? ? ? yes S(3) C(24) C(23) 107(2) ? ? ? yes C(27) C(26) C(31) 119(3) ? ? ? yes C(27) C(26) C(25) 119(3) ? ? ? yes C(31) C(26) C(25) 120(3) ? ? ? yes C(26) C(27) C(28) 120(3) ? ? ? yes C(27) C(28) C(29) 120(3) ? ? ? yes C(28) C(29) C(30) 119(4) ? ? ? yes C(29) C(30) C(31) 120(4) ? ? ? yes C(26) C(31) C(30) 120(4) ? ? ? 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_5 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 14:44:45 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.120(1) _cell_length_b 11.170(1) _cell_length_c 29.792(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3367.7(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 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 'brown' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 3.443 _exptl_crystal_density_meas ? _chemical_formula_weight 1745.69 _chemical_formula_analytical ? _chemical_formula_sum 'C21.50 H10 O15 Os6 S3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3052.00 _exptl_absorpt_coefficient_mu 22.784 _exptl_absorpt_correction_type 'inter-image 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 21402 _reflns_number_total 2904 _reflns_number_observed 2159 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.100 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.58 _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 Os 0 24 -1.216 7.603 'International Tables' C 0 86 0.003 0.002 'International Tables' O 0 60 0.011 0.006 'International Tables' S 0 12 0.125 0.123 'International Tables' H 0 40 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 Os(1) 1.0179(2) 0.2600(1) 0.09992(6) 0.0451(6) Uij ? ? Os(2) 1.0496(2) 0.0950(2) 0.16955(6) 0.0461(6) Uij ? ? Os(3) 0.8700(2) 0.0546(2) 0.09768(6) 0.0360(5) Uij ? ? Os(4) 1.1352(2) 0.0343(2) 0.08226(6) 0.0377(5) Uij ? ? Os(5) 1.0078(2) -0.1279(2) 0.14129(6) 0.0454(5) Uij ? ? Os(6) 0.9703(2) -0.1515(2) 0.05187(6) 0.0480(6) Uij ? ? S(1) 1.223(1) 0.360(1) 0.1128(5) 0.058(4) Uij ? ? S(2) 1.256(1) 0.185(1) 0.1931(4) 0.065(5) Uij ? ? S(3) 1.352(1) 0.1167(10) 0.0991(4) 0.044(3) Uij ? ? O(1) 0.866(4) 0.484(3) 0.121(2) 0.11(2) Uij ? ? O(2) 0.981(4) 0.342(3) 0.005(1) 0.08(1) Uij ? ? O(3) 0.977(4) 0.029(3) 0.264(1) 0.08(1) Uij ? ? O(4) 0.885(3) 0.306(3) 0.2034(10) 0.06(1) Uij ? ? O(5) 0.641(4) -0.103(4) 0.121(2) 0.11(2) Uij ? ? O(6) 0.685(4) 0.255(3) 0.129(1) 0.07(1) Uij ? ? O(7) 0.769(4) 0.104(3) 0.005(1) 0.07(1) Uij ? ? O(8) 1.150(3) 0.120(3) -0.014(1) 0.06(1) Uij ? ? O(9) 1.321(4) -0.172(3) 0.061(1) 0.10(2) Uij ? ? O(10) 1.264(4) -0.107(4) 0.193(2) 0.11(2) Uij ? ? O(11) 0.818(3) -0.247(3) 0.206(1) 0.10(2) Uij ? ? O(12) 1.122(5) -0.374(4) 0.131(2) 0.14(2) Uij ? ? O(13) 0.933(3) -0.078(3) -0.045(1) 0.08(1) Uij ? ? O(14) 0.730(3) -0.310(3) 0.052(1) 0.06(1) Uij ? ? O(15) 1.118(4) -0.370(3) 0.023(1) 0.09(1) Uij ? ? C(1) 0.923(4) 0.400(5) 0.117(2) 0.09(2) Uij ? ? C(2) 1.019(5) 0.295(4) 0.042(1) 0.06(2) Uij ? ? C(3) 1.009(5) 0.046(4) 0.229(2) 0.06(2) Uij ? ? C(4) 0.955(4) 0.221(5) 0.188(1) 0.06(2) Uij ? ? C(5) 0.736(6) -0.035(4) 0.116(2) 0.07(2) Uij ? ? C(6) 0.756(9) 0.191(4) 0.123(2) 0.1156 Uij ? ? C(7) 0.804(5) 0.078(3) 0.040(1) 0.04(1) Uij ? ? C(8) 1.116(5) 0.102(6) 0.032(2) 0.19(3) Uij ? ? C(9) 1.235(4) -0.095(4) 0.069(1) 0.05(2) Uij ? ? C(10) 1.168(6) -0.087(4) 0.175(2) 0.08(2) Uij ? ? C(11) 0.893(4) -0.199(4) 0.177(1) 0.05(1) Uij ? ? C(12) 1.072(7) -0.283(5) 0.134(2) 0.09(2) Uij ? ? C(13) 0.959(4) -0.102(4) -0.007(1) 0.04(1) Uij ? ? C(14) 0.816(4) -0.252(3) 0.056(2) 0.0303 Uij ? ? C(15) 1.081(6) -0.302(6) 0.037(2) 0.10(3) Uij ? ? C(16) 1.261(5) 0.332(4) 0.172(2) 0.07(2) Uij ? ? C(17) 1.384(4) 0.124(4) 0.158(1) 0.04(1) Uij ? ? C(18) 1.345(5) 0.277(4) 0.087(1) 0.06(2) Uij ? ? C(19) 0.497(5) 0.169(5) 0.353(1) 0.2701 Uij 0.5 ? C(20) 0.514(3) 0.087(3) 0.312(1) 0.2701 Uij 0.5 ? C(21) 0.433(3) -0.012(3) 0.306(1) 0.2701 Uij 0.5 ? C(22) 0.448(4) -0.086(3) 0.269(2) 0.2701 Uij 0.5 ? C(23) 0.545(5) -0.060(4) 0.237(1) 0.2701 Uij 0.5 ? C(24) 0.626(4) 0.040(4) 0.242(1) 0.2701 Uij 0.5 ? C(25) 0.611(3) 0.113(3) 0.280(1) 0.2701 Uij 0.5 ? H(1) 1.3486 0.3610 0.1772 0.0781 Uij ? ? H(2) 1.2008 0.3781 0.1894 0.0781 Uij ? ? H(3) 1.4604 0.1714 0.1627 0.0510 Uij ? ? H(4) 1.4002 0.0447 0.1686 0.0510 Uij ? ? H(5) 1.3339 0.2863 0.0557 0.0699 Uij ? ? H(6) 1.4273 0.3108 0.0960 0.0699 Uij ? ? H(7) 0.666(4) 0.181(4) 0.284(2) 0.3208 Uij 0.5 ? H(8) 0.692(5) 0.057(6) 0.221(2) 0.3208 Uij 0.5 ? H(9) 0.555(7) -0.110(5) 0.211(2) 0.3208 Uij 0.5 ? H(10) 0.393(5) -0.154(3) 0.265(2) 0.3208 Uij 0.5 ? H(11) 0.367(4) -0.030(5) 0.328(2) 0.3208 Uij 0.5 ? H(12) 0.5844 0.1778 0.3642 0.3355 Uij 0.5 ? H(13) 0.4630 0.2410 0.3430 0.3355 Uij 0.5 ? H(14) 0.4430 0.1309 0.3740 0.3355 Uij 0.5 ? 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 Os(1) 0.041(1) 0.035(1) 0.059(1) -0.002(1) -0.005(1) 0.0007(9) Os(2) 0.050(1) 0.052(1) 0.0364(10) -0.006(1) 0.002(1) -0.0026(9) Os(3) 0.031(1) 0.035(1) 0.0421(9) -0.0022(9) -0.001(1) -0.0008(9) Os(4) 0.039(1) 0.039(1) 0.0358(9) 0.001(1) 0.002(1) -0.0035(8) Os(6) 0.051(1) 0.045(1) 0.048(1) -0.004(1) -0.003(1) -0.0105(9) S(1) 0.072(10) 0.034(7) 0.069(9) -0.010(7) -0.003(8) -0.017(7) S(2) 0.06(1) 0.08(1) 0.049(8) -0.038(8) 0.000(8) -0.017(7) S(3) 0.031(7) 0.048(7) 0.052(7) 0.002(6) 0.008(7) -0.004(6) O(1) 0.09(3) 0.02(2) 0.20(5) 0.05(2) -0.04(3) 0.00(2) O(2) 0.10(3) 0.07(2) 0.08(3) 0.03(2) -0.06(2) 0.00(2) O(3) 0.10(3) 0.10(3) 0.05(2) 0.02(3) 0.04(2) 0.03(2) O(4) 0.04(2) 0.10(3) 0.06(2) 0.05(2) 0.00(2) -0.04(2) O(5) 0.07(3) 0.09(3) 0.17(4) -0.05(3) -0.03(3) 0.07(3) O(6) 0.09(3) 0.02(2) 0.10(3) 0.03(2) -0.01(2) -0.02(2) O(7) 0.11(3) 0.05(2) 0.06(2) 0.06(2) 0.00(2) 0.01(2) O(8) 0.07(2) 0.04(2) 0.06(2) 0.00(2) 0.01(2) -0.02(2) O(9) 0.07(3) 0.08(3) 0.13(4) -0.04(2) 0.07(3) -0.06(3) O(10) 0.09(3) 0.07(3) 0.18(5) -0.01(3) -0.06(3) 0.03(3) O(11) 0.08(3) 0.09(3) 0.14(4) -0.02(3) 0.05(3) 0.06(3) O(12) 0.16(4) 0.06(3) 0.21(6) 0.01(3) 0.12(4) -0.06(3) O(13) 0.09(3) 0.09(3) 0.05(2) 0.03(2) 0.03(2) 0.00(2) O(14) 0.05(3) 0.03(2) 0.10(3) -0.02(2) 0.00(2) 0.00(2) O(15) 0.13(4) 0.02(2) 0.11(3) 0.02(2) -0.02(3) -0.06(2) C(1) 0.01(3) 0.10(5) 0.18(6) -0.05(3) -0.07(4) 0.09(5) C(2) 0.07(4) 0.07(3) 0.04(3) -0.08(3) -0.01(3) 0.00(2) C(3) 0.04(3) 0.04(3) 0.08(4) 0.02(3) 0.01(3) -0.04(3) C(4) 0.02(3) 0.11(4) 0.05(3) 0.06(3) -0.01(2) 0.00(3) C(5) 0.10(5) 0.04(3) 0.09(4) 0.01(3) 0.00(4) 0.05(3) C(6) 0.23(9) 0.00(3) 0.12(6) -0.05(4) 0.01(6) -0.02(3) C(7) 0.11(4) 0.01(2) 0.01(2) -0.01(2) 0.01(2) 0.01(2) C(8) 0.06(4) 0.24(8) 0.28(9) -0.05(5) -0.08(5) 0.31(8) C(9) 0.03(3) 0.07(3) 0.04(3) 0.00(3) 0.01(2) -0.05(3) C(10) 0.12(6) 0.04(3) 0.06(3) 0.05(4) 0.04(4) 0.02(3) C(11) 0.03(3) 0.08(3) 0.03(2) -0.05(2) -0.03(2) 0.05(2) C(12) 0.13(6) 0.09(5) 0.05(3) 0.00(4) 0.01(4) -0.04(3) C(13) 0.02(3) 0.07(3) 0.02(2) 0.04(2) -0.02(2) -0.05(2) C(14) 0.00(2) -0.01(2) 0.09(3) -0.01(2) 0.00(2) -0.01(2) C(15) 0.09(5) 0.12(6) 0.08(4) -0.08(5) 0.00(4) -0.09(4) C(16) 0.09(4) 0.01(3) 0.09(4) 0.00(3) -0.03(3) -0.06(3) C(17) 0.02(3) 0.08(3) 0.02(2) 0.00(3) 0.01(2) 0.02(2) C(18) 0.09(4) 0.05(3) 0.03(3) -0.03(3) 0.02(3) 0.01(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2159 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0620 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0499 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.554 _refine_ls_shift/esd_max 0.0210 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.84 _refine_diff_density_max 3.92 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.793(3) ? ? yes Os(1) Os(3) 2.740(2) ? ? yes Os(1) Os(4) 2.836(2) ? ? yes Os(1) S(1) 2.38(1) ? ? yes Os(1) C(1) 1.91(6) ? ? yes Os(1) C(2) 1.77(4) ? ? yes Os(2) Os(3) 2.845(3) ? ? yes Os(2) Os(4) 2.824(3) ? ? yes Os(2) Os(5) 2.663(3) ? ? yes Os(2) S(2) 2.42(1) ? ? yes Os(2) C(3) 1.91(5) ? ? yes Os(2) C(4) 1.79(5) ? ? yes Os(2) C(10) 2.37(5) ? ? yes Os(3) Os(4) 2.733(3) ? ? yes Os(3) Os(5) 2.791(3) ? ? yes Os(3) Os(6) 2.863(3) ? ? yes Os(3) C(5) 1.77(6) ? ? yes Os(3) C(6) 2.05(7) ? ? yes Os(3) C(7) 1.86(4) ? ? yes Os(4) Os(5) 2.835(3) ? ? yes Os(4) Os(6) 2.812(3) ? ? yes Os(4) S(3) 2.43(1) ? ? yes Os(4) C(8) 1.70(7) ? ? yes Os(4) C(9) 1.81(5) ? ? yes Os(5) Os(6) 2.704(3) ? ? yes Os(5) C(10) 1.96(6) ? ? yes Os(5) C(11) 1.77(4) ? ? yes Os(5) C(12) 1.86(6) ? ? yes Os(6) C(13) 1.84(4) ? ? yes Os(6) C(14) 1.93(4) ? ? yes Os(6) C(15) 2.07(6) ? ? yes S(1) C(16) 1.84(5) ? ? yes S(1) C(18) 1.72(5) ? ? yes S(2) C(16) 1.76(4) ? ? yes S(2) C(17) 1.79(4) ? ? yes S(3) C(17) 1.80(4) ? ? yes S(3) C(18) 1.83(4) ? ? yes O(1) C(1) 1.11(7) ? ? yes O(2) C(2) 1.27(6) ? ? yes O(3) C(3) 1.11(6) ? ? yes O(4) C(4) 1.28(6) ? ? yes O(5) C(5) 1.24(7) ? ? yes O(6) C(6) 1.04(8) ? ? yes O(7) C(7) 1.13(5) ? ? yes O(8) C(8) 1.43(8) ? ? yes O(9) C(9) 1.24(6) ? ? yes O(10) C(10) 1.13(7) ? ? yes O(11) C(11) 1.27(6) ? ? yes O(12) C(12) 1.14(7) ? ? yes O(13) C(13) 1.19(5) ? ? yes O(14) C(14) 1.09(5) ? ? yes O(15) C(15) 0.95(7) ? ? yes C(20) C(21) 1.39(5) ? ? yes C(20) C(25) 1.39(5) ? ? yes C(20) C(19) 1.54(6) ? ? yes C(21) C(22) 1.39(6) ? ? yes C(22) C(23) 1.39(6) ? ? yes C(23) C(24) 1.39(6) ? ? yes C(24) C(25) 1.39(6) ? ? 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 Os(2) Os(1) Os(3) 61.88(6) ? ? ? yes Os(2) Os(1) Os(4) 60.21(6) ? ? ? yes Os(2) Os(1) S(1) 95.0(3) ? ? ? yes Os(2) Os(1) C(1) 113(1) ? ? ? yes Os(2) Os(1) C(2) 150(1) ? ? ? yes Os(3) Os(1) Os(4) 58.66(6) ? ? ? yes Os(3) Os(1) S(1) 150.4(3) ? ? ? yes Os(3) Os(1) C(1) 114(1) ? ? ? yes Os(3) Os(1) C(2) 99(1) ? ? ? yes Os(4) Os(1) S(1) 94.6(3) ? ? ? yes Os(4) Os(1) C(1) 171(1) ? ? ? yes Os(4) Os(1) C(2) 90(1) ? ? ? yes S(1) Os(1) C(1) 90(1) ? ? ? yes S(1) Os(1) C(2) 92(1) ? ? ? yes C(1) Os(1) C(2) 95(2) ? ? ? yes Os(1) Os(2) Os(3) 58.14(6) ? ? ? yes Os(1) Os(2) Os(4) 60.66(6) ? ? ? yes Os(1) Os(2) Os(5) 111.34(8) ? ? ? yes Os(1) Os(2) S(2) 92.3(3) ? ? ? yes Os(1) Os(2) C(3) 149(1) ? ? ? yes Os(1) Os(2) C(4) 69(1) ? ? ? yes Os(1) Os(2) C(10) 132(1) ? ? ? yes Os(3) Os(2) Os(4) 57.64(6) ? ? ? yes Os(3) Os(2) Os(5) 60.79(7) ? ? ? yes Os(3) Os(2) S(2) 146.6(3) ? ? ? yes Os(3) Os(2) C(3) 121(1) ? ? ? yes Os(3) Os(2) C(4) 90(1) ? ? ? yes Os(3) Os(2) C(10) 103(1) ? ? ? yes Os(4) Os(2) Os(5) 62.15(7) ? ? ? yes Os(4) Os(2) S(2) 95.9(3) ? ? ? yes Os(4) Os(2) C(3) 148(1) ? ? ? yes Os(4) Os(2) C(4) 129(1) ? ? ? yes Os(4) Os(2) C(10) 72(1) ? ? ? yes Os(5) Os(2) S(2) 128.2(4) ? ? ? yes Os(5) Os(2) C(3) 89(1) ? ? ? yes Os(5) Os(2) C(4) 138(1) ? ? ? yes Os(5) Os(2) C(10) 45(1) ? ? ? yes S(2) Os(2) C(3) 92(1) ? ? ? yes S(2) Os(2) C(4) 92(1) ? ? ? yes S(2) Os(2) C(10) 84(1) ? ? ? yes C(3) Os(2) C(4) 80(1) ? ? ? yes C(3) Os(2) C(10) 78(1) ? ? ? yes C(4) Os(2) C(10) 158(1) ? ? ? yes Os(1) Os(3) Os(2) 59.98(6) ? ? ? yes Os(1) Os(3) Os(4) 62.43(6) ? ? ? yes Os(1) Os(3) Os(5) 109.11(8) ? ? ? yes Os(1) Os(3) Os(6) 119.42(8) ? ? ? yes Os(1) Os(3) C(5) 151(1) ? ? ? yes Os(1) Os(3) C(6) 71(2) ? ? ? yes Os(1) Os(3) C(7) 95(1) ? ? ? yes Os(2) Os(3) Os(4) 60.79(6) ? ? ? yes Os(2) Os(3) Os(5) 56.38(6) ? ? ? yes Os(2) Os(3) Os(6) 105.06(8) ? ? ? yes Os(2) Os(3) C(5) 110(1) ? ? ? yes Os(2) Os(3) C(6) 88(2) ? ? ? yes Os(2) Os(3) C(7) 154(1) ? ? ? yes Os(4) Os(3) Os(5) 61.75(7) ? ? ? yes Os(4) Os(3) Os(6) 60.29(7) ? ? ? yes Os(4) Os(3) C(5) 139(1) ? ? ? yes Os(4) Os(3) C(6) 132(2) ? ? ? yes Os(4) Os(3) C(7) 102(1) ? ? ? yes Os(5) Os(3) Os(6) 57.12(6) ? ? ? yes Os(5) Os(3) C(5) 79(1) ? ? ? yes Os(5) Os(3) C(6) 130(2) ? ? ? yes Os(5) Os(3) C(7) 135(1) ? ? ? yes Os(6) Os(3) C(5) 88(1) ? ? ? yes Os(6) Os(3) C(6) 166(2) ? ? ? yes Os(6) Os(3) C(7) 78(1) ? ? ? yes C(5) Os(3) C(6) 82(2) ? ? ? yes C(5) Os(3) C(7) 95(2) ? ? ? yes C(6) Os(3) C(7) 91(2) ? ? ? yes Os(1) Os(4) Os(2) 59.14(6) ? ? ? yes Os(1) Os(4) Os(3) 58.91(5) ? ? ? yes Os(1) Os(4) Os(5) 105.22(8) ? ? ? yes Os(1) Os(4) Os(6) 117.85(8) ? ? ? yes Os(1) Os(4) S(3) 90.1(3) ? ? ? yes Os(1) Os(4) C(8) 73(2) ? ? ? yes Os(1) Os(4) C(9) 170(1) ? ? ? yes Os(2) Os(4) Os(3) 61.56(6) ? ? ? yes Os(2) Os(4) Os(5) 56.14(6) ? ? ? yes Os(2) Os(4) Os(6) 106.97(8) ? ? ? yes Os(2) Os(4) S(3) 89.7(3) ? ? ? yes Os(2) Os(4) C(8) 132(2) ? ? ? yes Os(2) Os(4) C(9) 124(1) ? ? ? yes Os(3) Os(4) Os(5) 60.14(7) ? ? ? yes Os(3) Os(4) Os(6) 62.14(7) ? ? ? yes Os(3) Os(4) S(3) 145.1(3) ? ? ? yes Os(3) Os(4) C(8) 89(1) ? ? ? yes Os(3) Os(4) C(9) 130(1) ? ? ? yes Os(5) Os(4) Os(6) 57.21(6) ? ? ? yes Os(5) Os(4) S(3) 121.6(3) ? ? ? yes Os(5) Os(4) C(8) 141(1) ? ? ? yes Os(5) Os(4) C(9) 83(1) ? ? ? yes Os(6) Os(4) S(3) 151.8(3) ? ? ? yes Os(6) Os(4) C(8) 88(2) ? ? ? yes Os(6) Os(4) C(9) 70(1) ? ? ? yes S(3) Os(4) C(8) 96(1) ? ? ? yes S(3) Os(4) C(9) 80(1) ? ? ? yes C(8) Os(4) C(9) 102(2) ? ? ? yes Os(2) Os(5) Os(3) 62.83(7) ? ? ? yes Os(2) Os(5) Os(4) 61.71(7) ? ? ? yes Os(2) Os(5) Os(6) 115.14(8) ? ? ? yes Os(2) Os(5) C(10) 59(1) ? ? ? yes Os(2) Os(5) C(11) 109(1) ? ? ? yes Os(2) Os(5) C(12) 148(1) ? ? ? yes Os(3) Os(5) Os(4) 58.11(6) ? ? ? yes Os(3) Os(5) Os(6) 62.77(7) ? ? ? yes Os(3) Os(5) C(10) 118(1) ? ? ? yes Os(3) Os(5) C(11) 106(1) ? ? ? yes Os(3) Os(5) C(12) 142(1) ? ? ? yes Os(4) Os(5) Os(6) 60.97(7) ? ? ? yes Os(4) Os(5) C(10) 77(1) ? ? ? yes Os(4) Os(5) C(11) 164(1) ? ? ? yes Os(4) Os(5) C(12) 110(1) ? ? ? yes Os(6) Os(5) C(10) 129(1) ? ? ? yes Os(6) Os(5) C(11) 117(1) ? ? ? yes Os(6) Os(5) C(12) 80(1) ? ? ? yes C(10) Os(5) C(11) 110(1) ? ? ? yes C(10) Os(5) C(12) 89(2) ? ? ? yes C(11) Os(5) C(12) 83(2) ? ? ? yes Os(3) Os(6) Os(4) 57.57(6) ? ? ? yes Os(3) Os(6) Os(5) 60.11(7) ? ? ? yes Os(3) Os(6) C(13) 100(1) ? ? ? yes Os(3) Os(6) C(14) 98(1) ? ? ? yes Os(3) Os(6) C(15) 161(1) ? ? ? yes Os(4) Os(6) Os(5) 61.82(7) ? ? ? yes Os(4) Os(6) C(13) 97(1) ? ? ? yes Os(4) Os(6) C(14) 153(1) ? ? ? yes Os(4) Os(6) C(15) 110(1) ? ? ? yes Os(5) Os(6) C(13) 156(1) ? ? ? yes Os(5) Os(6) C(14) 96(1) ? ? ? yes Os(5) Os(6) C(15) 102(1) ? ? ? yes C(13) Os(6) C(14) 100(1) ? ? ? yes C(13) Os(6) C(15) 94(2) ? ? ? yes C(14) Os(6) C(15) 88(2) ? ? ? yes Os(1) S(1) C(16) 105(1) ? ? ? yes Os(1) S(1) C(18) 107(1) ? ? ? yes C(16) S(1) C(18) 100(2) ? ? ? yes Os(2) S(2) C(16) 108(1) ? ? ? yes Os(2) S(2) C(17) 107(1) ? ? ? yes C(16) S(2) C(17) 97(2) ? ? ? yes Os(4) S(3) C(17) 112(1) ? ? ? yes Os(4) S(3) C(18) 107(1) ? ? ? yes C(17) S(3) C(18) 98(1) ? ? ? yes Os(1) C(1) O(1) 169(5) ? ? ? yes Os(1) C(2) O(2) 158(4) ? ? ? yes Os(2) C(3) O(3) 171(3) ? ? ? yes Os(2) C(4) O(4) 175(3) ? ? ? yes Os(3) C(5) O(5) 167(4) ? ? ? yes Os(3) C(6) O(6) 166(6) ? ? ? yes Os(3) C(7) O(7) 173(3) ? ? ? yes Os(4) C(8) O(8) 152(4) ? ? ? yes Os(4) C(9) O(9) 170(3) ? ? ? yes Os(2) C(10) Os(5) 75(1) ? ? ? yes Os(2) C(10) O(10) 129(4) ? ? ? yes Os(5) C(10) O(10) 155(4) ? ? ? yes Os(5) C(11) O(11) 173(3) ? ? ? yes Os(5) C(12) O(12) 173(5) ? ? ? yes Os(6) C(13) O(13) 170(3) ? ? ? yes Os(6) C(14) O(14) 170(4) ? ? ? yes Os(6) C(15) O(15) 163(5) ? ? ? yes S(1) C(16) S(2) 119(2) ? ? ? yes S(2) C(17) S(3) 117(2) ? ? ? yes S(1) C(18) S(3) 117(2) ? ? ? yes C(21) C(20) C(25) 120(3) ? ? ? yes C(21) C(20) C(19) 119(3) ? ? ? yes C(25) C(20) C(19) 120(3) ? ? ? yes C(20) C(21) C(22) 119(3) ? ? ? yes C(21) C(22) C(23) 120(3) ? ? ? yes C(22) C(23) C(24) 120(3) ? ? ? yes C(23) C(24) C(25) 119(3) ? ? ? yes C(20) C(25) C(24) 120(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_6 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 14:50:25 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.314(1) _cell_length_b 12.160(2) _cell_length_c 14.420(2) _cell_angle_alpha 108.01(2) _cell_angle_beta 92.80(1) _cell_angle_gamma 102.84(2) _cell_volume 1663.4(5) _cell_formula_units_Z 2 _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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'Block' _exptl_crystal_colour 'Brown' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.160 _exptl_crystal_density_diffrn 3.533 _exptl_crystal_density_meas ? _chemical_formula_weight 1769.69 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H16 O17 Os6 S2 ' _chemical_formula_moiety 'C23 H16 O17 Os6 S2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1556.00 _exptl_absorpt_coefficient_mu 23.010 _exptl_absorpt_correction_type 'inter-image 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 14561 _reflns_number_total 5736 _reflns_number_observed 5087 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.077 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.54 _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 Os 0 12 -1.216 7.603 'International Tables' S 0 4 0.125 0.123 'International Tables' C 0 46 0.003 0.002 'International Tables' O 0 34 0.011 0.006 'International Tables' H 0 32 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 Os(1) 0.14223(6) 0.17875(5) 0.34700(4) 0.0357(2) Uij ? ? Os(2) 0.10014(5) 0.31998(5) 0.23922(4) 0.0342(2) Uij ? ? Os(3) 0.36422(5) 0.35524(5) 0.33070(4) 0.0316(1) Uij ? ? Os(4) 0.25652(5) 0.16415(5) 0.16327(4) 0.0322(1) Uij ? ? Os(5) 0.30688(5) 0.39359(5) 0.14916(4) 0.0334(2) Uij ? ? Os(6) 0.52069(5) 0.30236(5) 0.17292(4) 0.0362(2) Uij ? ? S(1) -0.0761(4) 0.0463(3) 0.2997(3) 0.042(1) Uij ? ? S(2) 0.1662(4) 0.5043(3) 0.2245(3) 0.044(1) Uij ? ? O(1) 0.081(1) 0.278(1) 0.5545(9) 0.067(4) Uij ? ? O(2) 0.284(2) 0.019(1) 0.409(1) 0.075(5) Uij ? ? O(3) -0.082(1) 0.366(1) 0.400(1) 0.071(5) Uij ? ? O(4) -0.133(1) 0.207(1) 0.077(1) 0.078(5) Uij ? ? O(5) 0.254(1) 0.490(1) 0.5124(9) 0.067(4) Uij ? ? O(6) 0.559(1) 0.5976(10) 0.3656(9) 0.059(4) Uij ? ? O(7) 0.543(1) 0.249(1) 0.4368(9) 0.064(4) Uij ? ? O(8) 0.298(1) 0.082(1) -0.0543(9) 0.076(4) Uij ? ? O(9) 0.402(1) -0.009(1) 0.216(1) 0.072(5) Uij ? ? O(10) 0.000(1) -0.036(1) 0.0936(9) 0.062(3) Uij ? ? O(11) 0.177(1) 0.322(1) -0.0610(9) 0.077(5) Uij ? ? O(12) 0.535(1) 0.582(1) 0.121(1) 0.074(5) Uij ? ? O(13) 0.774(1) 0.505(1) 0.235(1) 0.081(5) Uij ? ? O(14) 0.585(1) 0.232(2) -0.0366(9) 0.083(5) Uij ? ? O(15) 0.680(1) 0.150(1) 0.235(1) 0.083(5) Uij ? ? O(16) 0.186(2) 0.766(1) 0.229(2) 0.096(6) Uij ? ? O(17) -0.290(1) -0.136(1) 0.3607(10) 0.068(4) Uij ? ? C(1) 0.103(2) 0.237(1) 0.475(1) 0.047(5) Uij ? ? C(2) 0.227(1) 0.076(1) 0.386(1) 0.042(4) Uij ? ? C(3) -0.015(2) 0.344(1) 0.341(1) 0.050(5) Uij ? ? C(4) -0.052(2) 0.247(2) 0.141(1) 0.051(5) Uij ? ? C(5) 0.290(2) 0.434(1) 0.445(1) 0.050(5) Uij ? ? C(6) 0.492(2) 0.506(1) 0.348(1) 0.045(5) Uij ? ? C(7) 0.475(2) 0.287(1) 0.397(1) 0.042(4) Uij ? ? C(8) 0.282(2) 0.117(2) 0.026(1) 0.052(5) Uij ? ? C(9) 0.348(1) 0.056(1) 0.196(1) 0.042(4) Uij ? ? C(10) 0.084(2) 0.045(2) 0.123(1) 0.048(5) Uij ? ? C(11) 0.229(2) 0.347(1) 0.016(1) 0.049(5) Uij ? ? C(12) 0.451(2) 0.509(2) 0.131(1) 0.046(5) Uij ? ? C(13) 0.680(2) 0.429(2) 0.213(1) 0.058(6) Uij ? ? C(14) 0.559(2) 0.261(2) 0.042(1) 0.057(6) Uij ? ? C(15) 0.619(1) 0.206(2) 0.213(1) 0.050(5) Uij ? ? C(16) 0.062(2) 0.560(2) 0.152(2) 0.060(6) Uij ? ? C(17) 0.144(2) 0.671(2) 0.135(2) 0.088(9) Uij ? ? C(18) 0.283(3) 0.742(2) 0.287(2) 0.089(8) Uij ? ? C(19) 0.221(2) 0.642(2) 0.324(1) 0.070(6) Uij ? ? C(20) -0.074(2) -0.101(2) 0.299(1) 0.065(6) Uij ? ? C(21) -0.212(2) -0.178(2) 0.285(1) 0.064(6) Uij ? ? C(22) -0.312(2) -0.024(2) 0.369(1) 0.058(6) Uij ? ? C(23) -0.182(2) 0.074(2) 0.398(1) 0.048(5) Uij ? ? H(1) 0.0285 0.4995 0.0903 0.0720 Uij ? ? H(2) -0.0109 0.5784 0.1862 0.0720 Uij ? ? H(3) 0.0903 0.6957 0.0937 0.1061 Uij ? ? H(4) 0.2204 0.6547 0.1055 0.1061 Uij ? ? H(5) 0.3514 0.7192 0.2490 0.1070 Uij ? ? H(6) 0.3217 0.8116 0.3417 0.1070 Uij ? ? H(7) 0.1456 0.6606 0.3560 0.0845 Uij ? ? H(8) 0.2845 0.6346 0.3701 0.0845 Uij ? ? H(9) -0.0270 -0.1364 0.2477 0.0782 Uij ? ? H(10) -0.0294 -0.0960 0.3605 0.0782 Uij ? ? H(11) -0.2069 -0.2560 0.2820 0.0770 Uij ? ? H(12) -0.2566 -0.1815 0.2242 0.0770 Uij ? ? H(13) -0.3532 -0.0275 0.3072 0.0694 Uij ? ? H(14) -0.3699 -0.0051 0.4173 0.0694 Uij ? ? H(15) -0.1365 0.0749 0.4568 0.0574 Uij ? ? H(16) -0.2018 0.1495 0.4075 0.0574 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 Os(1) 0.0402(3) 0.0350(3) 0.0344(3) 0.0099(2) 0.0105(2) 0.0135(2) Os(2) 0.0315(3) 0.0362(3) 0.0384(3) 0.0108(2) 0.0104(2) 0.0144(2) Os(3) 0.0335(3) 0.0292(3) 0.0285(3) 0.0078(2) 0.0046(2) 0.0041(2) Os(4) 0.0334(3) 0.0296(3) 0.0284(3) 0.0055(2) 0.0067(2) 0.0038(2) Os(5) 0.0321(3) 0.0352(3) 0.0350(3) 0.0091(2) 0.0084(2) 0.0132(2) Os(6) 0.0306(3) 0.0377(3) 0.0404(3) 0.0100(2) 0.0103(2) 0.0111(2) S(1) 0.047(2) 0.042(2) 0.039(2) 0.009(2) 0.012(2) 0.018(2) S(2) 0.045(2) 0.041(2) 0.054(2) 0.018(2) 0.016(2) 0.021(2) O(1) 0.092(10) 0.069(9) 0.038(6) 0.030(7) 0.024(6) 0.006(6) O(2) 0.10(1) 0.071(9) 0.071(9) 0.053(8) 0.008(8) 0.024(7) O(3) 0.070(8) 0.086(10) 0.083(9) 0.040(7) 0.052(8) 0.044(8) O(4) 0.043(7) 0.12(1) 0.063(8) 0.009(8) -0.007(6) 0.023(8) O(5) 0.061(7) 0.065(8) 0.053(7) 0.018(6) 0.020(6) -0.012(6) O(6) 0.061(7) 0.036(7) 0.065(8) -0.010(6) 0.005(6) 0.012(6) O(7) 0.071(9) 0.069(9) 0.062(8) 0.038(7) -0.011(6) 0.023(7) O(8) 0.079(9) 0.09(1) 0.034(7) -0.002(8) 0.022(6) -0.004(6) O(9) 0.079(9) 0.052(8) 0.10(1) 0.041(7) 0.023(8) 0.029(7) O(10) 0.039(6) 0.062(8) 0.055(7) -0.018(6) 0.001(5) -0.001(6) O(11) 0.071(9) 0.12(1) 0.040(7) 0.022(8) -0.012(6) 0.023(7) O(12) 0.062(8) 0.069(9) 0.09(1) -0.013(7) 0.009(7) 0.044(8) O(13) 0.036(6) 0.066(9) 0.12(1) -0.013(6) 0.018(7) 0.023(9) O(14) 0.08(1) 0.12(1) 0.042(7) 0.020(9) 0.027(7) 0.023(8) O(15) 0.045(8) 0.10(1) 0.13(1) 0.033(8) 0.020(8) 0.06(1) O(16) 0.09(1) 0.052(9) 0.17(2) 0.033(8) 0.03(1) 0.06(1) O(17) 0.076(9) 0.054(8) 0.068(8) 0.000(7) 0.016(7) 0.022(7) C(1) 0.046(9) 0.041(9) 0.06(1) 0.017(7) 0.011(7) 0.017(8) C(2) 0.036(8) 0.045(9) 0.045(8) 0.010(7) 0.000(6) 0.017(7) C(3) 0.050(9) 0.044(9) 0.06(1) 0.021(8) 0.019(9) 0.017(8) C(4) 0.034(8) 0.07(1) 0.051(9) 0.008(8) 0.001(7) 0.019(8) C(5) 0.049(9) 0.043(9) 0.048(9) 0.007(7) 0.007(8) 0.005(8) C(6) 0.06(1) 0.039(9) 0.040(8) 0.021(8) 0.008(7) 0.017(7) C(7) 0.055(9) 0.032(8) 0.030(7) 0.002(7) 0.000(7) 0.002(6) C(8) 0.044(9) 0.044(9) 0.050(10) -0.009(7) 0.013(7) 0.001(8) C(9) 0.026(7) 0.054(10) 0.036(8) 0.009(6) -0.003(6) 0.004(7) C(10) 0.06(1) 0.052(10) 0.026(7) 0.008(9) 0.009(7) 0.008(7) C(11) 0.042(9) 0.051(10) 0.06(1) 0.013(7) 0.018(8) 0.016(8) C(12) 0.041(8) 0.054(10) 0.044(9) 0.013(8) 0.010(7) 0.019(7) C(13) 0.06(1) 0.06(1) 0.06(1) 0.026(10) 0.025(9) 0.017(9) C(14) 0.049(10) 0.06(1) 0.07(1) 0.008(8) 0.019(8) 0.030(10) C(15) 0.018(7) 0.07(1) 0.06(1) 0.006(7) -0.001(7) 0.028(9) C(16) 0.026(8) 0.07(1) 0.11(2) 0.026(8) 0.015(9) 0.05(1) C(17) 0.08(2) 0.09(2) 0.12(2) 0.01(1) 0.01(1) 0.07(2) C(18) 0.09(2) 0.04(1) 0.13(2) 0.01(1) -0.01(1) 0.02(1) C(19) 0.09(1) 0.05(1) 0.06(1) 0.02(1) 0.02(1) -0.002(9) C(20) 0.09(1) 0.043(10) 0.05(1) 0.014(10) 0.021(10) 0.005(8) C(21) 0.08(1) 0.06(1) 0.041(9) 0.007(10) 0.010(9) 0.010(8) C(22) 0.05(1) 0.06(1) 0.07(1) 0.012(9) 0.023(9) 0.033(10) C(23) 0.044(9) 0.06(1) 0.046(9) 0.014(7) 0.002(7) 0.021(8) #------------------------------------------------------------------------------ _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 5087 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0621 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.397 _refine_ls_shift/esd_max 0.0040 _refine_ls_shift/esd_mean ? _refine_diff_density_min -4.17 _refine_diff_density_max 1.73 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.7330(8) ? ? yes Os(1) Os(3) 2.8432(8) ? ? yes Os(1) Os(4) 2.9236(7) ? ? yes Os(1) S(1) 2.385(4) ? ? yes Os(1) C(1) 1.87(2) ? ? yes Os(1) C(2) 1.87(2) ? ? yes Os(2) Os(3) 2.8501(8) ? ? yes Os(2) Os(4) 2.7639(8) ? ? yes Os(2) Os(5) 2.6787(8) ? ? yes Os(2) S(2) 2.272(4) ? ? yes Os(2) C(3) 1.92(2) ? ? yes Os(2) C(4) 1.91(2) ? ? yes Os(3) Os(4) 2.7539(7) ? ? yes Os(3) Os(5) 2.8542(7) ? ? yes Os(3) Os(6) 2.8477(7) ? ? yes Os(3) C(5) 1.92(2) ? ? yes Os(3) C(6) 1.94(2) ? ? yes Os(3) C(7) 1.92(2) ? ? yes Os(4) Os(5) 2.7951(7) ? ? yes Os(4) Os(6) 2.8374(8) ? ? yes Os(4) C(8) 1.93(2) ? ? yes Os(4) C(9) 1.94(2) ? ? yes Os(4) C(10) 1.96(2) ? ? yes Os(5) Os(6) 2.7313(8) ? ? yes Os(5) S(2) 2.284(4) ? ? yes Os(5) C(11) 1.90(2) ? ? yes Os(5) C(12) 1.90(2) ? ? yes Os(6) C(13) 1.91(2) ? ? yes Os(6) C(14) 1.89(2) ? ? yes Os(6) C(15) 1.90(2) ? ? yes S(1) C(20) 1.80(2) ? ? yes S(1) C(23) 1.82(2) ? ? yes S(2) C(16) 1.83(2) ? ? yes S(2) C(19) 1.79(2) ? ? yes O(1) C(1) 1.15(2) ? ? yes O(2) C(2) 1.13(2) ? ? yes O(3) C(3) 1.13(2) ? ? yes O(4) C(4) 1.12(2) ? ? yes O(5) C(5) 1.14(2) ? ? yes O(6) C(6) 1.12(2) ? ? yes O(7) C(7) 1.15(2) ? ? yes O(8) C(8) 1.14(2) ? ? yes O(9) C(9) 1.15(2) ? ? yes O(10) C(10) 1.10(2) ? ? yes O(11) C(11) 1.13(2) ? ? yes O(12) C(12) 1.15(2) ? ? yes O(13) C(13) 1.14(2) ? ? yes O(14) C(14) 1.14(2) ? ? yes O(15) C(15) 1.13(2) ? ? yes O(16) C(17) 1.44(3) ? ? yes O(16) C(18) 1.42(3) ? ? yes O(17) C(21) 1.42(2) ? ? yes O(17) C(22) 1.40(2) ? ? yes C(16) C(17) 1.53(3) ? ? yes C(18) C(19) 1.50(3) ? ? yes C(20) C(21) 1.49(3) ? ? yes C(22) C(23) 1.52(2) ? ? 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 Os(2) Os(1) Os(3) 61.44(2) ? ? ? yes Os(2) Os(1) Os(4) 58.38(2) ? ? ? yes Os(2) Os(1) S(1) 95.47(9) ? ? ? yes Os(2) Os(1) C(1) 111.6(5) ? ? ? yes Os(2) Os(1) C(2) 156.0(5) ? ? ? yes Os(3) Os(1) Os(4) 57.03(2) ? ? ? yes Os(3) Os(1) S(1) 155.54(9) ? ? ? yes Os(3) Os(1) C(1) 105.3(5) ? ? ? yes Os(3) Os(1) C(2) 102.1(5) ? ? ? yes Os(4) Os(1) S(1) 105.29(9) ? ? ? yes Os(4) Os(1) C(1) 161.9(5) ? ? ? yes Os(4) Os(1) C(2) 98.4(5) ? ? ? yes S(1) Os(1) C(1) 90.2(5) ? ? ? yes S(1) Os(1) C(2) 97.0(5) ? ? ? yes C(1) Os(1) C(2) 88.8(7) ? ? ? yes Os(1) Os(2) Os(3) 61.19(2) ? ? ? yes Os(1) Os(2) Os(4) 64.26(2) ? ? ? yes Os(1) Os(2) Os(5) 115.54(3) ? ? ? yes Os(1) Os(2) S(2) 144.8(1) ? ? ? yes Os(1) Os(2) C(3) 73.7(5) ? ? ? yes Os(1) Os(2) C(4) 113.3(5) ? ? ? yes Os(3) Os(2) Os(4) 58.73(2) ? ? ? yes Os(3) Os(2) Os(5) 62.07(2) ? ? ? yes Os(3) Os(2) S(2) 88.1(1) ? ? ? yes Os(3) Os(2) C(3) 107.7(5) ? ? ? yes Os(3) Os(2) C(4) 156.7(5) ? ? ? yes Os(4) Os(2) Os(5) 61.78(2) ? ? ? yes Os(4) Os(2) S(2) 115.92(10) ? ? ? yes Os(4) Os(2) C(3) 137.2(5) ? ? ? yes Os(4) Os(2) C(4) 98.1(5) ? ? ? yes Os(5) Os(2) S(2) 54.19(10) ? ? ? yes Os(5) Os(2) C(3) 152.9(5) ? ? ? yes Os(5) Os(2) C(4) 106.6(5) ? ? ? yes S(2) Os(2) C(3) 102.8(5) ? ? ? yes S(2) Os(2) C(4) 101.6(6) ? ? ? yes C(3) Os(2) C(4) 90.9(7) ? ? ? yes Os(1) Os(3) Os(2) 57.38(2) ? ? ? yes Os(1) Os(3) Os(4) 62.96(2) ? ? ? yes Os(1) Os(3) Os(5) 106.93(2) ? ? ? yes Os(1) Os(3) Os(6) 120.78(2) ? ? ? yes Os(1) Os(3) C(5) 75.0(5) ? ? ? yes Os(1) Os(3) C(6) 163.1(5) ? ? ? yes Os(1) Os(3) C(7) 86.8(5) ? ? ? yes Os(2) Os(3) Os(4) 59.07(2) ? ? ? yes Os(2) Os(3) Os(5) 56.02(2) ? ? ? yes Os(2) Os(3) Os(6) 105.12(2) ? ? ? yes Os(2) Os(3) C(5) 81.7(5) ? ? ? yes Os(2) Os(3) C(6) 117.7(4) ? ? ? yes Os(2) Os(3) C(7) 143.5(4) ? ? ? yes Os(4) Os(3) Os(5) 59.76(2) ? ? ? yes Os(4) Os(3) Os(6) 60.84(2) ? ? ? yes Os(4) Os(3) C(5) 133.1(5) ? ? ? yes Os(4) Os(3) C(6) 130.7(4) ? ? ? yes Os(4) Os(3) C(7) 100.8(4) ? ? ? yes Os(5) Os(3) Os(6) 57.24(2) ? ? ? yes Os(5) Os(3) C(5) 119.6(5) ? ? ? yes Os(5) Os(3) C(6) 78.2(4) ? ? ? yes Os(5) Os(3) C(7) 143.5(5) ? ? ? yes Os(6) Os(3) C(5) 164.2(5) ? ? ? yes Os(6) Os(3) C(6) 75.8(5) ? ? ? yes Os(6) Os(3) C(7) 86.5(5) ? ? ? yes C(5) Os(3) C(6) 88.4(7) ? ? ? yes C(5) Os(3) C(7) 96.4(7) ? ? ? yes C(6) Os(3) C(7) 98.5(6) ? ? ? yes Os(1) Os(4) Os(2) 57.36(2) ? ? ? yes Os(1) Os(4) Os(3) 60.02(2) ? ? ? yes Os(1) Os(4) Os(5) 106.34(2) ? ? ? yes Os(1) Os(4) Os(6) 118.37(2) ? ? ? yes Os(1) Os(4) C(8) 162.5(4) ? ? ? yes Os(1) Os(4) C(9) 85.0(4) ? ? ? yes Os(1) Os(4) C(10) 75.9(4) ? ? ? yes Os(2) Os(4) Os(3) 62.20(2) ? ? ? yes Os(2) Os(4) Os(5) 57.61(2) ? ? ? yes Os(2) Os(4) Os(6) 107.73(2) ? ? ? yes Os(2) Os(4) C(8) 121.7(6) ? ? ? yes Os(2) Os(4) C(9) 141.9(4) ? ? ? yes Os(2) Os(4) C(10) 83.9(5) ? ? ? yes Os(3) Os(4) Os(5) 61.90(2) ? ? ? yes Os(3) Os(4) Os(6) 61.21(2) ? ? ? yes Os(3) Os(4) C(8) 136.9(5) ? ? ? yes Os(3) Os(4) C(9) 95.6(4) ? ? ? yes Os(3) Os(4) C(10) 133.9(4) ? ? ? yes Os(5) Os(4) Os(6) 58.01(2) ? ? ? yes Os(5) Os(4) C(8) 83.9(5) ? ? ? yes Os(5) Os(4) C(9) 141.1(4) ? ? ? yes Os(5) Os(4) C(10) 125.5(5) ? ? ? yes Os(6) Os(4) C(8) 79.1(4) ? ? ? yes Os(6) Os(4) C(9) 83.6(4) ? ? ? yes Os(6) Os(4) C(10) 164.9(4) ? ? ? yes C(8) Os(4) C(9) 95.9(7) ? ? ? yes C(8) Os(4) C(10) 86.6(6) ? ? ? yes C(9) Os(4) C(10) 93.2(7) ? ? ? yes Os(2) Os(5) Os(3) 61.91(2) ? ? ? yes Os(2) Os(5) Os(4) 60.61(2) ? ? ? yes Os(2) Os(5) Os(6) 113.48(3) ? ? ? yes Os(2) Os(5) S(2) 53.79(10) ? ? ? yes Os(2) Os(5) C(11) 103.0(5) ? ? ? yes Os(2) Os(5) C(12) 154.1(5) ? ? ? yes Os(3) Os(5) Os(4) 58.34(2) ? ? ? yes Os(3) Os(5) Os(6) 61.26(2) ? ? ? yes Os(3) Os(5) S(2) 87.79(10) ? ? ? yes Os(3) Os(5) C(11) 154.5(5) ? ? ? yes Os(3) Os(5) C(12) 109.9(5) ? ? ? yes Os(4) Os(5) Os(6) 61.77(2) ? ? ? yes Os(4) Os(5) S(2) 114.35(10) ? ? ? yes Os(4) Os(5) C(11) 96.7(5) ? ? ? yes Os(4) Os(5) C(12) 138.9(5) ? ? ? yes Os(6) Os(5) S(2) 146.5(1) ? ? ? yes Os(6) Os(5) C(11) 114.0(5) ? ? ? yes Os(6) Os(5) C(12) 77.9(5) ? ? ? yes S(2) Os(5) C(11) 99.5(5) ? ? ? yes S(2) Os(5) C(12) 103.4(5) ? ? ? yes C(11) Os(5) C(12) 92.3(7) ? ? ? yes Os(3) Os(6) Os(4) 57.95(2) ? ? ? yes Os(3) Os(6) Os(5) 61.50(2) ? ? ? yes Os(3) Os(6) C(13) 104.6(5) ? ? ? yes Os(3) Os(6) C(14) 157.5(5) ? ? ? yes Os(3) Os(6) C(15) 100.7(5) ? ? ? yes Os(4) Os(6) Os(5) 60.22(2) ? ? ? yes Os(4) Os(6) C(13) 161.9(5) ? ? ? yes Os(4) Os(6) C(14) 104.9(5) ? ? ? yes Os(4) Os(6) C(15) 99.2(5) ? ? ? yes Os(5) Os(6) C(13) 109.0(5) ? ? ? yes Os(5) Os(6) C(14) 98.1(6) ? ? ? yes Os(5) Os(6) C(15) 157.4(5) ? ? ? yes C(13) Os(6) C(14) 90.6(7) ? ? ? yes C(13) Os(6) C(15) 88.1(7) ? ? ? yes C(14) Os(6) C(15) 96.2(8) ? ? ? yes Os(1) S(1) C(20) 111.5(7) ? ? ? yes Os(1) S(1) C(23) 111.9(6) ? ? ? yes C(20) S(1) C(23) 95.2(8) ? ? ? yes Os(2) S(2) Os(5) 72.0(1) ? ? ? yes Os(2) S(2) C(16) 122.3(6) ? ? ? yes Os(2) S(2) C(19) 125.7(7) ? ? ? yes Os(5) S(2) C(16) 119.6(7) ? ? ? yes Os(5) S(2) C(19) 124.1(7) ? ? ? yes C(16) S(2) C(19) 95.5(10) ? ? ? yes C(17) O(16) C(18) 111(1) ? ? ? yes C(21) O(17) C(22) 113(1) ? ? ? yes Os(1) C(1) O(1) 177(1) ? ? ? yes Os(1) C(2) O(2) 175(1) ? ? ? yes Os(2) C(3) O(3) 175(1) ? ? ? yes Os(2) C(4) O(4) 173(1) ? ? ? yes Os(3) C(5) O(5) 173(1) ? ? ? yes Os(3) C(6) O(6) 173(1) ? ? ? yes Os(3) C(7) O(7) 178(1) ? ? ? yes Os(4) C(8) O(8) 174(1) ? ? ? yes Os(4) C(9) O(9) 179(1) ? ? ? yes Os(4) C(10) O(10) 168(1) ? ? ? yes Os(5) C(11) O(11) 176(1) ? ? ? yes Os(5) C(12) O(12) 177(1) ? ? ? yes Os(6) C(13) O(13) 178(1) ? ? ? yes Os(6) C(14) O(14) 176(1) ? ? ? yes Os(6) C(15) O(15) 177(1) ? ? ? yes S(2) C(16) C(17) 110(1) ? ? ? yes O(16) C(17) C(16) 109(1) ? ? ? yes O(16) C(18) C(19) 110(1) ? ? ? yes S(2) C(19) C(18) 110(1) ? ? ? yes S(1) C(20) C(21) 110(1) ? ? ? yes O(17) C(21) C(20) 113(1) ? ? ? yes O(17) C(22) C(23) 112(1) ? ? ? yes S(1) C(23) C(22) 109(1) ? ? ? 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_8 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 14:52:56 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 ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 15.251(1) _cell_length_b 12.358(1) _cell_length_c 16.422(2) _cell_angle_alpha 90 _cell_angle_beta 102.29(1) _cell_angle_gamma 90 _cell_volume 3024.1(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 'Brown' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.170 _exptl_crystal_density_diffrn 3.719 _exptl_crystal_density_meas ? _chemical_formula_weight 1693.53 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H8 O17 Os6 S ' _chemical_formula_moiety 'C20 H8 O17 Os6 S ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2944.00 _exptl_absorpt_coefficient_mu 25.238 _exptl_absorpt_correction_type 'inter-image 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 20502 _reflns_number_total 5863 _reflns_number_observed 3969 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min ? _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 Os 0 24 -1.216 7.603 'International Tables' C 0 80 0.003 0.002 'International Tables' S 0 4 0.125 0.123 'International Tables' O 0 68 0.011 0.006 'International Tables' H 0 32 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 Os(1) 0.37272(6) 0.13390(8) 0.85772(5) 0.0487(3) Uij ? ? Os(2) 0.19474(5) 0.08947(7) 0.82075(5) 0.0366(2) Uij ? ? Os(3) 0.27600(6) 0.12885(7) 0.68680(5) 0.0426(2) Uij ? ? Os(4) 0.31534(5) -0.06385(7) 0.77279(5) 0.0403(2) Uij ? ? Os(5) 0.13782(5) -0.01733(7) 0.67827(5) 0.0352(2) Uij ? ? Os(6) 0.26892(6) -0.07177(8) 0.59594(5) 0.0456(3) Uij ? ? S(1) 0.0759(3) -0.0265(4) 0.7917(3) 0.037(1) Uij ? ? O(1) 0.441(1) 0.086(2) 1.040(1) 0.086(7) Uij ? ? O(2) 0.352(1) 0.368(2) 0.906(1) 0.099(8) Uij ? ? O(3) 0.565(1) 0.151(2) 0.833(1) 0.093(8) Uij ? ? O(4) 0.098(1) 0.304(1) 0.8203(10) 0.061(5) Uij ? ? O(5) 0.2326(10) 0.069(1) 1.0119(9) 0.059(5) Uij ? ? O(6) 0.258(1) 0.371(2) 0.721(1) 0.082(7) Uij ? ? O(7) 0.459(1) 0.158(2) 0.640(2) 0.106(9) Uij ? ? O(8) 0.171(1) 0.199(2) 0.515(1) 0.081(6) Uij ? ? O(9) 0.364(1) -0.132(2) 0.955(1) 0.073(6) Uij ? ? O(10) 0.508(1) -0.106(2) 0.754(1) 0.080(7) Uij ? ? O(11) 0.246(1) -0.295(2) 0.749(1) 0.087(7) Uij ? ? O(12) 0.063(1) -0.236(1) 0.6037(9) 0.063(5) Uij ? ? O(13) -0.007(1) 0.109(1) 0.561(1) 0.080(6) Uij ? ? O(14) 0.236(1) -0.312(2) 0.556(1) 0.084(7) Uij ? ? O(15) 0.180(1) -0.018(2) 0.417(1) 0.092(8) Uij ? ? O(16) 0.450(1) -0.081(2) 0.553(1) 0.111(10) Uij ? ? O(17) -0.052(1) -0.091(2) 0.907(1) 0.067(6) Uij ? ? C(1) 0.415(1) 0.100(2) 0.971(2) 0.070(9) Uij ? ? C(2) 0.360(2) 0.282(2) 0.886(1) 0.067(8) Uij ? ? C(3) 0.489(2) 0.145(2) 0.842(2) 0.066(8) Uij ? ? C(4) 0.135(1) 0.220(2) 0.821(1) 0.040(6) Uij ? ? C(5) 0.225(1) 0.079(2) 0.940(2) 0.051(7) Uij ? ? C(6) 0.266(2) 0.280(3) 0.711(2) 0.069(9) Uij ? ? C(7) 0.394(2) 0.145(2) 0.660(1) 0.060(8) Uij ? ? C(8) 0.211(2) 0.172(2) 0.579(2) 0.073(9) Uij ? ? C(9) 0.344(1) -0.099(2) 0.888(2) 0.058(8) Uij ? ? C(10) 0.437(2) -0.085(2) 0.760(1) 0.051(7) Uij ? ? C(11) 0.272(2) -0.209(2) 0.752(1) 0.067(8) Uij ? ? C(12) 0.092(1) -0.150(2) 0.629(1) 0.050(7) Uij ? ? C(13) 0.049(2) 0.057(2) 0.604(1) 0.050(7) Uij ? ? C(14) 0.251(2) -0.223(3) 0.571(2) 0.067(9) Uij ? ? C(15) 0.214(1) -0.036(2) 0.484(2) 0.063(8) Uij ? ? C(16) 0.383(2) -0.078(2) 0.575(2) 0.070(9) Uij ? ? C(17) 0.071(1) -0.147(2) 0.849(1) 0.047(6) Uij ? ? C(18) 0.039(2) -0.128(2) 0.928(1) 0.053(7) Uij ? ? C(19) -0.058(2) 0.016(2) 0.876(1) 0.056(7) Uij ? ? C(20) -0.037(1) 0.022(2) 0.790(1) 0.041(6) Uij ? ? H(1) 0.0317 -0.1964 0.8151 0.0566 Uij ? ? H(2) 0.1297 -0.1777 0.8628 0.0566 Uij ? ? H(3) 0.0756 -0.0758 0.9610 0.0633 Uij ? ? H(4) 0.0416 -0.1943 0.9583 0.0633 Uij ? ? H(5) -0.1177 0.0419 0.8725 0.0673 Uij ? ? H(6) -0.0173 0.0609 0.9129 0.0673 Uij ? ? H(7) -0.0415 0.0947 0.7713 0.0493 Uij ? ? H(8) -0.0783 -0.0218 0.7527 0.0493 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 Os(1) 0.0425(5) 0.0561(6) 0.0429(5) -0.0064(4) -0.0011(4) -0.0043(4) Os(2) 0.0402(4) 0.0374(5) 0.0308(4) -0.0012(4) 0.0044(3) -0.0021(3) Os(3) 0.0477(5) 0.0437(5) 0.0360(4) -0.0071(4) 0.0077(3) 0.0037(4) Os(4) 0.0399(4) 0.0440(5) 0.0363(4) 0.0038(4) 0.0064(3) 0.0017(4) Os(5) 0.0384(4) 0.0383(5) 0.0281(4) -0.0012(4) 0.0051(3) -0.0011(3) Os(6) 0.0462(5) 0.0557(6) 0.0368(5) 0.0008(4) 0.0133(4) -0.0048(4) S(1) 0.043(3) 0.038(3) 0.031(2) -0.003(2) 0.009(2) -0.002(2) O(1) 0.07(1) 0.12(2) 0.05(1) -0.01(1) -0.011(10) 0.00(1) O(2) 0.09(2) 0.07(1) 0.12(2) -0.01(1) 0.00(1) -0.05(1) O(3) 0.05(1) 0.16(2) 0.07(1) -0.02(1) 0.016(9) 0.00(1) O(4) 0.08(1) 0.039(10) 0.06(1) 0.019(9) 0.003(8) 0.009(8) O(5) 0.049(9) 0.10(1) 0.030(8) 0.007(9) 0.002(7) -0.014(8) O(6) 0.11(2) 0.05(1) 0.08(1) -0.02(1) 0.00(1) 0.014(10) O(7) 0.06(1) 0.13(2) 0.15(2) -0.03(1) 0.07(1) -0.01(2) O(8) 0.11(1) 0.08(1) 0.045(10) -0.02(1) -0.018(10) 0.028(9) O(9) 0.07(1) 0.10(2) 0.046(10) 0.01(1) 0.001(8) 0.03(1) O(10) 0.042(9) 0.14(2) 0.06(1) 0.02(1) 0.025(8) 0.00(1) O(11) 0.11(2) 0.05(1) 0.09(1) -0.01(1) 0.02(1) 0.01(1) O(12) 0.09(1) 0.05(1) 0.054(10) -0.018(9) 0.021(9) -0.030(8) O(13) 0.09(1) 0.06(1) 0.08(1) 0.01(1) -0.02(1) 0.013(10) O(14) 0.10(2) 0.05(1) 0.12(2) -0.01(1) 0.06(1) -0.03(1) O(15) 0.10(2) 0.12(2) 0.06(1) 0.01(1) 0.01(1) 0.01(1) O(16) 0.04(1) 0.18(3) 0.12(2) 0.00(1) 0.05(1) -0.01(2) O(17) 0.07(1) 0.08(1) 0.07(1) -0.008(10) 0.049(9) -0.002(9) C(1) 0.001(8) 0.12(2) 0.09(2) -0.03(1) -0.001(10) -0.02(2) C(2) 0.06(2) 0.09(2) 0.04(1) 0.01(2) -0.01(1) -0.01(1) C(3) 0.07(2) 0.07(2) 0.05(1) 0.00(1) 0.00(1) 0.01(1) C(4) 0.06(1) 0.03(1) 0.03(1) -0.02(1) 0.009(9) -0.003(9) C(5) 0.03(1) 0.05(1) 0.07(2) 0.00(1) -0.009(10) -0.01(1) C(6) 0.06(2) 0.08(2) 0.06(2) -0.01(2) 0.00(1) 0.03(2) C(7) 0.08(2) 0.06(2) 0.04(1) -0.02(1) 0.03(1) -0.01(1) C(8) 0.11(2) 0.05(2) 0.06(2) -0.03(2) 0.01(2) 0.01(1) C(9) 0.03(1) 0.06(2) 0.08(2) 0.01(1) 0.00(1) 0.00(1) C(10) 0.05(1) 0.07(2) 0.03(1) 0.01(1) 0.001(9) 0.00(1) C(11) 0.10(2) 0.05(2) 0.04(1) 0.00(2) 0.00(1) 0.03(1) C(12) 0.04(1) 0.06(2) 0.05(1) 0.00(1) 0.010(10) -0.02(1) C(13) 0.06(1) 0.04(1) 0.06(1) 0.00(1) 0.02(1) 0.00(1) C(14) 0.04(1) 0.10(2) 0.06(2) 0.03(1) 0.01(1) -0.03(2) C(15) 0.03(1) 0.10(2) 0.06(2) -0.02(1) 0.01(1) -0.02(2) C(16) 0.08(2) 0.07(2) 0.05(1) -0.01(2) 0.00(1) 0.00(1) C(17) 0.05(1) 0.04(1) 0.04(1) -0.02(1) 0.013(10) 0.01(1) C(18) 0.07(2) 0.04(1) 0.05(1) 0.00(1) 0.02(1) 0.02(1) C(19) 0.06(2) 0.06(2) 0.06(1) 0.00(1) 0.03(1) 0.01(1) C(20) 0.04(1) 0.04(1) 0.04(1) 0.000(10) 0.006(9) -0.006(9) #------------------------------------------------------------------------------ _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 3969 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0525 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0633 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.935 _refine_ls_shift/esd_max 0.0070 _refine_ls_shift/esd_mean ? _refine_diff_density_min -4.32 _refine_diff_density_max 2.19 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.708(1) ? ? yes Os(1) Os(3) 2.880(1) ? ? yes Os(1) Os(4) 2.857(1) ? ? yes Os(1) C(1) 1.88(3) ? ? yes Os(1) C(2) 1.90(3) ? ? yes Os(1) C(3) 1.85(3) ? ? yes Os(2) Os(3) 2.788(1) ? ? yes Os(2) Os(4) 2.865(1) ? ? yes Os(2) Os(5) 2.666(1) ? ? yes Os(2) S(1) 2.281(5) ? ? yes Os(2) C(4) 1.86(2) ? ? yes Os(2) C(5) 1.91(3) ? ? yes Os(3) Os(4) 2.769(1) ? ? yes Os(3) Os(5) 2.757(1) ? ? yes Os(3) Os(6) 2.884(1) ? ? yes Os(3) C(6) 1.92(3) ? ? yes Os(3) C(7) 1.94(3) ? ? yes Os(3) C(8) 1.91(3) ? ? yes Os(4) Os(5) 2.878(1) ? ? yes Os(4) Os(6) 2.841(1) ? ? yes Os(4) C(9) 1.90(3) ? ? yes Os(4) C(10) 1.93(2) ? ? yes Os(4) C(11) 1.92(3) ? ? yes Os(5) Os(6) 2.726(1) ? ? yes Os(5) S(1) 2.263(5) ? ? yes Os(5) C(12) 1.90(2) ? ? yes Os(5) C(13) 1.86(2) ? ? yes Os(6) C(14) 1.92(3) ? ? yes Os(6) C(15) 1.90(3) ? ? yes Os(6) C(16) 1.84(3) ? ? yes S(1) C(17) 1.77(2) ? ? yes S(1) C(20) 1.81(2) ? ? yes O(1) C(1) 1.13(3) ? ? yes O(2) C(2) 1.13(3) ? ? yes O(3) C(3) 1.20(3) ? ? yes O(4) C(4) 1.17(2) ? ? yes O(5) C(5) 1.17(3) ? ? yes O(6) C(6) 1.16(3) ? ? yes O(7) C(7) 1.12(3) ? ? yes O(8) C(8) 1.15(3) ? ? yes O(9) C(9) 1.15(3) ? ? yes O(10) C(10) 1.14(3) ? ? yes O(11) C(11) 1.13(3) ? ? yes O(12) C(12) 1.19(3) ? ? yes O(13) C(13) 1.18(3) ? ? yes O(14) C(14) 1.14(3) ? ? yes O(15) C(15) 1.13(3) ? ? yes O(16) C(16) 1.16(3) ? ? yes O(17) C(18) 1.43(3) ? ? yes O(17) C(19) 1.42(3) ? ? yes C(17) C(18) 1.50(3) ? ? yes C(19) C(20) 1.52(3) ? ? 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 Os(2) Os(1) Os(3) 59.76(3) ? ? ? yes Os(2) Os(1) Os(4) 61.91(3) ? ? ? yes Os(2) Os(1) C(1) 107.1(6) ? ? ? yes Os(2) Os(1) C(2) 95.8(8) ? ? ? yes Os(2) Os(1) C(3) 158.2(8) ? ? ? yes Os(3) Os(1) Os(4) 57.70(3) ? ? ? yes Os(3) Os(1) C(1) 162.9(7) ? ? ? yes Os(3) Os(1) C(2) 101.5(6) ? ? ? yes Os(3) Os(1) C(3) 100.0(7) ? ? ? yes Os(4) Os(1) C(1) 107.3(9) ? ? ? yes Os(4) Os(1) C(2) 154.5(6) ? ? ? yes Os(4) Os(1) C(3) 101.4(9) ? ? ? yes C(1) Os(1) C(2) 90(1) ? ? ? yes C(1) Os(1) C(3) 90.8(9) ? ? ? yes C(2) Os(1) C(3) 96(1) ? ? ? yes Os(1) Os(2) Os(3) 63.18(3) ? ? ? yes Os(1) Os(2) Os(4) 61.60(3) ? ? ? yes Os(1) Os(2) Os(5) 114.87(4) ? ? ? yes Os(1) Os(2) S(1) 152.7(1) ? ? ? yes Os(1) Os(2) C(4) 107.1(6) ? ? ? yes Os(1) Os(2) C(5) 76.9(6) ? ? ? yes Os(3) Os(2) Os(4) 58.62(3) ? ? ? yes Os(3) Os(2) Os(5) 60.67(3) ? ? ? yes Os(3) Os(2) S(1) 114.3(1) ? ? ? yes Os(3) Os(2) C(4) 98.9(6) ? ? ? yes Os(3) Os(2) C(5) 140.1(6) ? ? ? yes Os(4) Os(2) Os(5) 62.57(3) ? ? ? yes Os(4) Os(2) S(1) 93.1(1) ? ? ? yes Os(4) Os(2) C(4) 157.3(6) ? ? ? yes Os(4) Os(2) C(5) 102.0(7) ? ? ? yes Os(5) Os(2) S(1) 53.8(1) ? ? ? yes Os(5) Os(2) C(4) 111.5(5) ? ? ? yes Os(5) Os(2) C(5) 145.7(7) ? ? ? yes S(1) Os(2) C(4) 100.2(6) ? ? ? yes S(1) Os(2) C(5) 100.3(7) ? ? ? yes C(4) Os(2) C(5) 93.6(9) ? ? ? yes Os(1) Os(3) Os(2) 57.06(3) ? ? ? yes Os(1) Os(3) Os(4) 60.73(3) ? ? ? yes Os(1) Os(3) Os(5) 106.92(4) ? ? ? yes Os(1) Os(3) Os(6) 118.55(4) ? ? ? yes Os(1) Os(3) C(6) 79.8(7) ? ? ? yes Os(1) Os(3) C(7) 84.8(7) ? ? ? yes Os(1) Os(3) C(8) 162.6(8) ? ? ? yes Os(2) Os(3) Os(4) 62.08(3) ? ? ? yes Os(2) Os(3) Os(5) 57.47(3) ? ? ? yes Os(2) Os(3) Os(6) 106.51(4) ? ? ? yes Os(2) Os(3) C(6) 86.3(8) ? ? ? yes Os(2) Os(3) C(7) 141.3(7) ? ? ? yes Os(2) Os(3) C(8) 123.1(10) ? ? ? yes Os(4) Os(3) Os(5) 62.77(3) ? ? ? yes Os(4) Os(3) Os(6) 60.30(3) ? ? ? yes Os(4) Os(3) C(6) 138.4(7) ? ? ? yes Os(4) Os(3) C(7) 95.2(8) ? ? ? yes Os(4) Os(3) C(8) 136.4(8) ? ? ? yes Os(5) Os(3) Os(6) 57.74(3) ? ? ? yes Os(5) Os(3) C(6) 123.5(8) ? ? ? yes Os(5) Os(3) C(7) 141.9(7) ? ? ? yes Os(5) Os(3) C(8) 83.8(8) ? ? ? yes Os(6) Os(3) C(6) 161.2(7) ? ? ? yes Os(6) Os(3) C(7) 84.6(7) ? ? ? yes Os(6) Os(3) C(8) 78.7(8) ? ? ? yes C(6) Os(3) C(7) 93(1) ? ? ? yes C(6) Os(3) C(8) 82(1) ? ? ? yes C(7) Os(3) C(8) 95(1) ? ? ? yes Os(1) Os(4) Os(2) 56.50(3) ? ? ? yes Os(1) Os(4) Os(3) 61.56(3) ? ? ? yes Os(1) Os(4) Os(5) 104.34(4) ? ? ? yes Os(1) Os(4) Os(6) 120.81(4) ? ? ? yes Os(1) Os(4) C(9) 74.3(7) ? ? ? yes Os(1) Os(4) C(10) 88.1(7) ? ? ? yes Os(1) Os(4) C(11) 160.7(7) ? ? ? yes Os(2) Os(4) Os(3) 59.29(3) ? ? ? yes Os(2) Os(4) Os(5) 55.31(3) ? ? ? yes Os(2) Os(4) Os(6) 105.60(3) ? ? ? yes Os(2) Os(4) C(9) 84.6(7) ? ? ? yes Os(2) Os(4) C(10) 143.9(7) ? ? ? yes Os(2) Os(4) C(11) 116.5(9) ? ? ? yes Os(3) Os(4) Os(5) 58.41(3) ? ? ? yes Os(3) Os(4) Os(6) 61.86(3) ? ? ? yes Os(3) Os(4) C(9) 133.3(7) ? ? ? yes Os(3) Os(4) C(10) 99.8(7) ? ? ? yes Os(3) Os(4) C(11) 133.3(6) ? ? ? yes Os(5) Os(4) Os(6) 56.93(3) ? ? ? yes Os(5) Os(4) C(9) 125.2(7) ? ? ? yes Os(5) Os(4) C(10) 141.7(6) ? ? ? yes Os(5) Os(4) C(11) 80.8(8) ? ? ? yes Os(6) Os(4) C(9) 164.7(7) ? ? ? yes Os(6) Os(4) C(10) 85.4(6) ? ? ? yes Os(6) Os(4) C(11) 77.8(7) ? ? ? yes C(9) Os(4) C(10) 92.9(9) ? ? ? yes C(9) Os(4) C(11) 87.5(10) ? ? ? yes C(10) Os(4) C(11) 99(1) ? ? ? yes Os(2) Os(5) Os(3) 61.86(3) ? ? ? yes Os(2) Os(5) Os(4) 62.11(3) ? ? ? yes Os(2) Os(5) Os(6) 114.93(4) ? ? ? yes Os(2) Os(5) S(1) 54.4(1) ? ? ? yes Os(2) Os(5) C(12) 145.7(7) ? ? ? yes Os(2) Os(5) C(13) 112.9(7) ? ? ? yes Os(3) Os(5) Os(4) 58.82(3) ? ? ? yes Os(3) Os(5) Os(6) 63.47(3) ? ? ? yes Os(3) Os(5) S(1) 116.1(1) ? ? ? yes Os(3) Os(5) C(12) 142.6(7) ? ? ? yes Os(3) Os(5) C(13) 98.7(7) ? ? ? yes Os(4) Os(5) Os(6) 60.86(3) ? ? ? yes Os(4) Os(5) S(1) 93.2(1) ? ? ? yes Os(4) Os(5) C(12) 106.0(7) ? ? ? yes Os(4) Os(5) C(13) 157.2(7) ? ? ? yes Os(6) Os(5) S(1) 151.0(1) ? ? ? yes Os(6) Os(5) C(12) 79.3(7) ? ? ? yes Os(6) Os(5) C(13) 107.5(7) ? ? ? yes S(1) Os(5) C(12) 97.5(7) ? ? ? yes S(1) Os(5) C(13) 101.2(7) ? ? ? yes C(12) Os(5) C(13) 89.7(9) ? ? ? yes Os(3) Os(6) Os(4) 57.84(3) ? ? ? yes Os(3) Os(6) Os(5) 58.79(3) ? ? ? yes Os(3) Os(6) C(14) 159.3(8) ? ? ? yes Os(3) Os(6) C(15) 105.0(9) ? ? ? yes Os(3) Os(6) C(16) 101.4(9) ? ? ? yes Os(4) Os(6) Os(5) 62.21(3) ? ? ? yes Os(4) Os(6) C(14) 104.3(8) ? ? ? yes Os(4) Os(6) C(15) 160.4(8) ? ? ? yes Os(4) Os(6) C(16) 98.7(7) ? ? ? yes Os(5) Os(6) C(14) 105.0(7) ? ? ? yes Os(5) Os(6) C(15) 101.7(7) ? ? ? yes Os(5) Os(6) C(16) 157.3(8) ? ? ? yes C(14) Os(6) C(15) 90(1) ? ? ? yes C(14) Os(6) C(16) 91(1) ? ? ? yes C(15) Os(6) C(16) 93(1) ? ? ? yes Os(2) S(1) Os(5) 71.8(2) ? ? ? yes Os(2) S(1) C(17) 122.5(7) ? ? ? yes Os(2) S(1) C(20) 120.3(7) ? ? ? yes Os(5) S(1) C(17) 123.3(8) ? ? ? yes Os(5) S(1) C(20) 122.1(7) ? ? ? yes C(17) S(1) C(20) 98(1) ? ? ? yes C(18) O(17) C(19) 112(1) ? ? ? yes Os(1) C(1) O(1) 175(2) ? ? ? yes Os(1) C(2) O(2) 177(2) ? ? ? yes Os(1) C(3) O(3) 179(2) ? ? ? yes Os(2) C(4) O(4) 178(1) ? ? ? yes Os(2) C(5) O(5) 171(1) ? ? ? yes Os(3) C(6) O(6) 176(2) ? ? ? yes Os(3) C(7) O(7) 175(2) ? ? ? yes Os(3) C(8) O(8) 178(2) ? ? ? yes Os(4) C(9) O(9) 172(2) ? ? ? yes Os(4) C(10) O(10) 174(2) ? ? ? yes Os(4) C(11) O(11) 172(2) ? ? ? yes Os(5) C(12) O(12) 174(2) ? ? ? yes Os(5) C(13) O(13) 175(2) ? ? ? yes Os(6) C(14) O(14) 176(2) ? ? ? yes Os(6) C(15) O(15) 177(2) ? ? ? yes Os(6) C(16) O(16) 173(2) ? ? ? yes S(1) C(17) C(18) 112(1) ? ? ? yes O(17) C(18) C(17) 109(1) ? ? ? yes O(17) C(19) C(20) 111(1) ? ? ? yes S(1) C(20) C(19) 111(1) ? ? ? 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_9 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Apr 23 14:54:59 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 8.992(1) _cell_length_b 10.348(2) _cell_length_c 18.637(2) _cell_angle_alpha 99.00(2) _cell_angle_beta 94.67(1) _cell_angle_gamma 104.25(1) _cell_volume 1647.0(5) _cell_formula_units_Z 2 _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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'Block' _exptl_crystal_colour 'Brown' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.160 _exptl_crystal_density_diffrn 3.572 _exptl_crystal_density_meas ? _chemical_formula_weight 1771.70 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H18 O17 Os6 S2 ' _chemical_formula_moiety 'C23 H18 O17 Os6 S2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1560.00 _exptl_absorpt_coefficient_mu 23.239 _exptl_absorpt_correction_type 'inter-image 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 10408 _reflns_number_total 5630 _reflns_number_observed 3690 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.68 _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 Os 0 12 -1.216 7.603 'International Tables' C 0 46 0.003 0.002 'International Tables' O 0 34 0.011 0.006 'International Tables' S 0 4 0.125 0.123 'International Tables' H 0 36 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 Os(1) 0.5741(1) 0.3142(1) 0.36475(6) 0.0273(3) Uij ? ? Os(2) 0.3191(1) 0.1131(1) 0.27351(6) 0.0251(3) Uij ? ? Os(3) 0.3819(1) 0.3975(1) 0.26514(6) 0.0266(3) Uij ? ? Os(4) 0.5761(1) 0.2470(1) 0.20962(6) 0.0259(3) Uij ? ? Os(5) 0.3178(1) 0.2564(1) 0.11553(6) 0.0282(3) Uij ? ? Os(6) 0.5792(1) 0.4861(1) 0.15892(7) 0.0332(3) Uij ? ? S(1) 0.7444(9) 0.1932(8) 0.4092(4) 0.040(2) Uij ? ? S(2) 0.1919(7) 0.0665(7) 0.1552(4) 0.025(2) Uij ? ? O(1) 0.830(2) 0.572(2) 0.413(1) 0.066(8) Uij ? ? O(2) 0.443(3) 0.355(2) 0.505(1) 0.062(8) Uij ? ? O(3) 0.029(3) 0.083(3) 0.348(1) 0.077(10) Uij ? ? O(4) 0.312(3) -0.172(2) 0.297(1) 0.057(8) Uij ? ? O(5) 0.188(2) 0.395(3) 0.391(1) 0.055(8) Uij ? ? O(6) 0.141(3) 0.516(2) 0.193(1) 0.059(8) Uij ? ? O(7) 0.564(3) 0.683(2) 0.338(1) 0.056(7) Uij ? ? O(8) 0.685(3) 0.176(3) 0.060(1) 0.065(9) Uij ? ? O(9) 0.909(2) 0.356(3) 0.277(1) 0.065(8) Uij ? ? O(10) 0.618(3) -0.027(2) 0.231(2) 0.065(9) Uij ? ? O(11) 0.027(2) 0.322(2) 0.053(1) 0.053(7) Uij ? ? O(12) 0.362(3) 0.122(3) -0.032(1) 0.069(9) Uij ? ? O(13) 0.453(3) 0.723(3) 0.132(2) 0.078(10) Uij ? ? O(14) 0.758(3) 0.478(3) 0.025(1) 0.076(10) Uij ? ? O(15) 0.870(3) 0.652(2) 0.259(1) 0.055(7) Uij ? ? O(16) -0.070(2) -0.205(2) 0.112(1) 0.050(7) Uij ? ? O(17) 0.788(3) 0.039(3) 0.537(1) 0.060(8) Uij ? ? C(1) 0.736(3) 0.477(3) 0.391(1) 0.030(8) Uij ? ? C(2) 0.497(4) 0.339(3) 0.451(2) 0.05(1) Uij ? ? C(3) 0.140(5) 0.099(2) 0.319(2) 0.0537 Uij ? ? C(4) 0.319(3) -0.061(3) 0.283(2) 0.035(9) Uij ? ? C(5) 0.261(3) 0.390(3) 0.345(2) 0.036(9) Uij ? ? C(6) 0.224(2) 0.459(3) 0.214(1) 0.030(7) Uij ? ? C(7) 0.505(4) 0.575(3) 0.306(2) 0.05(1) Uij ? ? C(8) 0.630(3) 0.202(3) 0.113(1) 0.049(9) Uij ? ? C(9) 0.784(3) 0.323(3) 0.257(2) 0.039(9) Uij ? ? C(10) 0.586(4) 0.069(3) 0.228(2) 0.041(9) Uij ? ? C(11) 0.139(3) 0.294(3) 0.073(1) 0.040(8) Uij ? ? C(12) 0.344(3) 0.168(3) 0.024(2) 0.040(10) Uij ? ? C(13) 0.505(3) 0.636(4) 0.146(2) 0.06(1) Uij ? ? C(14) 0.690(3) 0.485(3) 0.078(2) 0.049(10) Uij ? ? C(15) 0.757(4) 0.592(3) 0.226(2) 0.06(1) Uij ? ? C(16) -0.023(3) 0.033(3) 0.148(2) 0.038(8) Uij ? ? C(17) -0.091(3) -0.100(3) 0.165(2) 0.038(9) Uij ? ? C(18) 0.089(4) -0.213(3) 0.118(2) 0.06(1) Uij ? ? C(19) 0.200(3) -0.090(3) 0.098(2) 0.043(9) Uij ? ? C(20) 0.805(4) 0.256(3) 0.505(2) 0.08(1) Uij ? ? C(21) 0.885(5) 0.161(5) 0.535(3) 0.10(2) Uij ? ? C(22) 0.739(4) -0.034(4) 0.463(2) 0.06(1) Uij ? ? C(23) 0.643(4) 0.031(3) 0.421(2) 0.07(1) Uij ? ? H(1) -0.0491 0.1008 0.1808 0.0450 Uij ? ? H(2) -0.0616 0.0354 0.0990 0.0450 Uij ? ? H(3) -0.1991 -0.1109 0.1663 0.0452 Uij ? ? H(4) -0.0442 -0.1056 0.2114 0.0452 Uij ? ? H(5) 0.1198 -0.2179 0.1675 0.0715 Uij ? ? H(6) 0.0951 -0.2920 0.0867 0.0715 Uij ? ? H(7) 0.1730 -0.0857 0.0483 0.0519 Uij ? ? H(8) 0.3029 -0.0990 0.1045 0.0519 Uij ? ? H(9) 0.8747 0.3437 0.5115 0.0927 Uij ? ? H(10) 0.7178 0.2608 0.5294 0.0927 Uij ? ? H(11) 0.9323 0.2019 0.5829 0.1171 Uij ? ? H(12) 0.9616 0.1466 0.5045 0.1171 Uij ? ? H(13) 0.8275 -0.0379 0.4390 0.0780 Uij ? ? H(14) 0.6803 -0.1233 0.4641 0.0780 Uij ? ? H(15) 0.5571 0.0389 0.4458 0.0854 Uij ? ? H(16) 0.6077 -0.0244 0.3738 0.0854 Uij ? ? H(17) 0.4282 0.1506 0.3671 0.0608 Uij ? ? H(18) 0.4298 0.3998 0.0782 0.0608 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 Os(1) 0.0287(6) 0.0229(6) 0.0298(6) 0.0071(4) -0.0022(5) 0.0055(5) Os(2) 0.0250(5) 0.0196(6) 0.0302(6) 0.0039(4) 0.0022(5) 0.0071(5) Os(3) 0.0305(6) 0.0191(6) 0.0321(6) 0.0091(4) 0.0029(5) 0.0069(5) Os(4) 0.0248(6) 0.0221(6) 0.0313(6) 0.0059(4) 0.0047(5) 0.0058(5) Os(5) 0.0298(6) 0.0227(6) 0.0301(6) 0.0024(5) 0.0003(5) 0.0078(5) Os(6) 0.0346(6) 0.0230(6) 0.0408(7) 0.0008(5) 0.0047(5) 0.0125(5) S(1) 0.042(4) 0.043(5) 0.046(5) 0.022(4) 0.009(4) 0.019(4) S(2) 0.022(3) 0.024(4) 0.030(4) 0.003(3) 0.002(3) 0.010(3) O(1) 0.03(1) 0.03(1) 0.11(2) -0.01(1) -0.01(1) 0.01(1) O(2) 0.11(2) 0.03(1) 0.05(2) 0.02(1) 0.03(1) 0.00(1) O(3) 0.07(2) 0.12(3) 0.05(2) 0.02(2) 0.05(1) 0.03(2) O(4) 0.08(2) 0.05(1) 0.05(2) 0.03(1) 0.02(1) 0.02(1) O(5) 0.04(1) 0.08(2) 0.06(2) 0.02(1) 0.02(1) 0.01(1) O(6) 0.07(2) 0.07(2) 0.05(1) 0.04(1) -0.03(1) 0.02(1) O(7) 0.09(2) 0.02(1) 0.05(1) 0.00(1) 0.00(1) 0.01(1) O(8) 0.10(2) 0.09(2) 0.04(1) 0.05(2) 0.04(1) 0.02(1) O(9) 0.02(1) 0.10(2) 0.09(2) 0.02(1) 0.00(1) 0.02(2) O(10) 0.06(2) 0.03(1) 0.12(2) 0.03(1) 0.01(1) 0.03(1) O(11) 0.03(1) 0.05(1) 0.06(2) 0.01(1) -0.03(1) 0.01(1) O(12) 0.10(2) 0.08(2) 0.02(1) 0.02(2) 0.02(1) -0.01(1) O(13) 0.11(2) 0.05(2) 0.09(2) 0.04(2) -0.01(2) 0.01(1) O(14) 0.08(2) 0.08(2) 0.08(2) 0.02(2) 0.05(2) 0.03(2) O(15) 0.05(1) 0.04(1) 0.06(2) -0.02(1) 0.00(1) 0.02(1) O(16) 0.03(1) 0.05(2) 0.06(2) -0.01(1) 0.01(1) 0.01(1) O(17) 0.07(2) 0.07(2) 0.05(2) 0.03(1) -0.01(1) 0.04(1) C(1) 0.02(1) 0.04(2) 0.04(2) 0.01(1) 0.00(1) 0.02(1) C(2) 0.07(2) 0.00(1) 0.07(2) 0.00(1) 0.02(2) 0.00(1) C(3) 0.13(3) -0.01(1) 0.05(2) 0.03(2) 0.03(2) -0.01(1) C(4) 0.01(1) 0.05(2) 0.05(2) 0.02(1) 0.01(1) 0.04(2) C(5) 0.01(1) 0.03(2) 0.07(2) 0.02(1) -0.03(1) 0.00(2) C(6) 0.00(1) 0.05(2) 0.03(1) -0.02(1) -0.04(1) 0.00(1) C(7) 0.09(2) 0.02(2) 0.05(2) 0.04(2) -0.02(2) 0.00(1) C(8) 0.03(2) 0.07(2) 0.02(2) 0.00(1) -0.07(2) 0.01(1) C(9) 0.01(1) 0.05(2) 0.07(2) 0.03(1) -0.01(1) 0.02(2) C(10) 0.06(2) 0.04(2) 0.02(2) 0.00(2) 0.02(1) 0.00(1) C(11) 0.03(2) 0.05(2) 0.02(1) -0.02(1) -0.04(1) 0.00(1) C(12) 0.03(2) 0.05(2) 0.06(2) 0.01(1) 0.02(2) 0.05(2) C(13) 0.02(1) 0.05(2) 0.08(3) -0.01(1) 0.00(2) -0.01(2) C(14) 0.02(2) 0.04(2) 0.07(3) -0.01(1) -0.04(2) 0.01(2) C(15) 0.04(2) 0.04(2) 0.09(3) 0.00(2) 0.03(2) 0.04(2) C(16) 0.00(1) 0.05(2) 0.05(2) 0.00(1) -0.02(1) 0.00(2) C(17) 0.03(2) 0.05(2) 0.05(2) 0.01(1) 0.01(1) 0.01(2) C(18) 0.07(2) 0.03(2) 0.06(2) 0.01(2) -0.01(2) -0.02(2) C(19) 0.05(2) 0.02(2) 0.06(2) 0.00(1) 0.02(2) -0.01(1) C(20) 0.07(3) 0.03(2) 0.10(3) -0.03(2) -0.02(2) 0.00(2) C(21) 0.09(3) 0.07(3) 0.15(5) 0.03(3) 0.01(3) 0.04(3) C(22) 0.07(2) 0.07(3) 0.09(3) 0.04(2) 0.01(2) 0.07(2) C(23) 0.08(3) 0.03(2) 0.09(3) -0.03(2) -0.01(2) 0.06(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 3690 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0605 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0654 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.979 _refine_ls_shift/esd_max 0.0220 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.77 _refine_diff_density_max 1.08 #------------------------------------------------------------------------------ _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 Os(1) Os(2) 2.896(1) ? ? yes Os(1) Os(3) 2.808(1) ? ? yes Os(1) Os(4) 2.869(2) ? ? yes Os(1) S(1) 2.380(7) ? ? yes Os(1) C(1) 1.90(3) ? ? yes Os(1) C(2) 1.80(4) ? ? yes Os(2) Os(3) 2.888(1) ? ? yes Os(2) Os(4) 2.841(2) ? ? yes Os(2) S(2) 2.321(7) ? ? yes Os(2) C(3) 1.86(4) ? ? yes Os(2) C(4) 1.83(3) ? ? yes Os(3) Os(4) 2.771(2) ? ? yes Os(3) Os(5) 2.879(2) ? ? yes Os(3) Os(6) 2.872(2) ? ? yes Os(3) C(5) 1.91(4) ? ? yes Os(3) C(6) 1.93(2) ? ? yes Os(3) C(7) 1.90(3) ? ? yes Os(4) Os(5) 2.826(1) ? ? yes Os(4) Os(6) 2.778(2) ? ? yes Os(4) C(8) 1.92(3) ? ? yes Os(4) C(9) 1.92(3) ? ? yes Os(4) C(10) 1.94(3) ? ? yes Os(5) Os(6) 2.857(2) ? ? yes Os(5) S(2) 2.278(6) ? ? yes Os(5) C(11) 1.89(3) ? ? yes Os(5) C(12) 1.87(4) ? ? yes Os(6) C(13) 1.87(4) ? ? yes Os(6) C(14) 1.87(4) ? ? yes Os(6) C(15) 1.92(4) ? ? yes S(1) C(20) 1.79(4) ? ? yes S(1) C(23) 1.76(3) ? ? yes S(2) C(16) 1.86(2) ? ? yes S(2) C(19) 1.81(3) ? ? yes O(1) C(1) 1.13(3) ? ? yes O(2) C(2) 1.17(4) ? ? yes O(3) C(3) 1.16(4) ? ? yes O(4) C(4) 1.21(3) ? ? yes O(5) C(5) 1.13(4) ? ? yes O(6) C(6) 1.13(3) ? ? yes O(7) C(7) 1.16(3) ? ? yes O(8) C(8) 1.16(4) ? ? yes O(9) C(9) 1.11(3) ? ? yes O(10) C(10) 1.11(4) ? ? yes O(11) C(11) 1.16(3) ? ? yes O(12) C(12) 1.12(4) ? ? yes O(13) C(13) 1.17(4) ? ? yes O(14) C(14) 1.21(4) ? ? yes O(15) C(15) 1.13(4) ? ? yes O(16) C(17) 1.41(4) ? ? yes O(16) C(18) 1.45(4) ? ? yes O(17) C(21) 1.35(5) ? ? yes O(17) C(22) 1.45(5) ? ? yes C(16) C(17) 1.46(4) ? ? yes C(18) C(19) 1.53(4) ? ? yes C(20) C(21) 1.50(5) ? ? yes C(22) C(23) 1.46(4) ? ? 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 Os(2) Os(1) Os(3) 60.82(4) ? ? ? yes Os(2) Os(1) Os(4) 59.04(4) ? ? ? yes Os(2) Os(1) S(1) 106.3(2) ? ? ? yes Os(2) Os(1) C(1) 157.4(8) ? ? ? yes Os(2) Os(1) C(2) 102.0(10) ? ? ? yes Os(3) Os(1) Os(4) 58.42(4) ? ? ? yes Os(3) Os(1) S(1) 159.2(2) ? ? ? yes Os(3) Os(1) C(1) 99.3(7) ? ? ? yes Os(3) Os(1) C(2) 105(1) ? ? ? yes Os(4) Os(1) S(1) 101.3(2) ? ? ? yes Os(4) Os(1) C(1) 102.4(8) ? ? ? yes Os(4) Os(1) C(2) 158(1) ? ? ? yes S(1) Os(1) C(1) 89.2(8) ? ? ? yes S(1) Os(1) C(2) 93(1) ? ? ? yes C(1) Os(1) C(2) 93(1) ? ? ? yes Os(1) Os(2) Os(3) 58.09(3) ? ? ? yes Os(1) Os(2) Os(4) 60.00(4) ? ? ? yes Os(1) Os(2) S(2) 139.4(2) ? ? ? yes Os(1) Os(2) C(3) 109.8(9) ? ? ? yes Os(1) Os(2) C(4) 112.7(8) ? ? ? yes Os(3) Os(2) Os(4) 57.84(4) ? ? ? yes Os(3) Os(2) S(2) 87.7(2) ? ? ? yes Os(3) Os(2) C(3) 98.0(7) ? ? ? yes Os(3) Os(2) C(4) 169.2(8) ? ? ? yes Os(4) Os(2) S(2) 84.2(2) ? ? ? yes Os(4) Os(2) C(3) 155.9(7) ? ? ? yes Os(4) Os(2) C(4) 113.6(8) ? ? ? yes S(2) Os(2) C(3) 95(1) ? ? ? yes S(2) Os(2) C(4) 98.3(9) ? ? ? yes C(3) Os(2) C(4) 90(1) ? ? ? yes Os(1) Os(3) Os(2) 61.09(4) ? ? ? yes Os(1) Os(3) Os(4) 61.88(4) ? ? ? yes Os(1) Os(3) Os(5) 118.74(5) ? ? ? yes Os(1) Os(3) Os(6) 103.88(5) ? ? ? yes Os(1) Os(3) C(5) 80.0(6) ? ? ? yes Os(1) Os(3) C(6) 167.8(8) ? ? ? yes Os(1) Os(3) C(7) 84.5(8) ? ? ? yes Os(2) Os(3) Os(4) 60.21(4) ? ? ? yes Os(2) Os(3) Os(5) 74.69(4) ? ? ? yes Os(2) Os(3) Os(6) 116.05(5) ? ? ? yes Os(2) Os(3) C(5) 79.0(8) ? ? ? yes Os(2) Os(3) C(6) 118.1(7) ? ? ? yes Os(2) Os(3) C(7) 145.4(8) ? ? ? yes Os(4) Os(3) Os(5) 59.98(4) ? ? ? yes Os(4) Os(3) Os(6) 58.95(4) ? ? ? yes Os(4) Os(3) C(5) 133.5(7) ? ? ? yes Os(4) Os(3) C(6) 129.5(8) ? ? ? yes Os(4) Os(3) C(7) 107(1) ? ? ? yes Os(5) Os(3) Os(6) 59.59(4) ? ? ? yes Os(5) Os(3) C(5) 131.9(7) ? ? ? yes Os(5) Os(3) C(6) 70.8(8) ? ? ? yes Os(5) Os(3) C(7) 130(1) ? ? ? yes Os(6) Os(3) C(5) 164.6(8) ? ? ? yes Os(6) Os(3) C(6) 87.5(8) ? ? ? yes Os(6) Os(3) C(7) 72(1) ? ? ? yes C(5) Os(3) C(6) 87(1) ? ? ? yes C(5) Os(3) C(7) 92(1) ? ? ? yes C(6) Os(3) C(7) 94(1) ? ? ? yes Os(1) Os(4) Os(2) 60.97(4) ? ? ? yes Os(1) Os(4) Os(3) 59.71(4) ? ? ? yes Os(1) Os(4) Os(5) 118.51(5) ? ? ? yes Os(1) Os(4) Os(6) 104.75(5) ? ? ? yes Os(1) Os(4) C(8) 165.7(7) ? ? ? yes Os(1) Os(4) C(9) 70.3(10) ? ? ? yes Os(1) Os(4) C(10) 85.5(8) ? ? ? yes Os(2) Os(4) Os(3) 61.95(4) ? ? ? yes Os(2) Os(4) Os(5) 76.26(4) ? ? ? yes Os(2) Os(4) Os(6) 120.84(5) ? ? ? yes Os(2) Os(4) C(8) 128.7(8) ? ? ? yes Os(2) Os(4) C(9) 126.6(9) ? ? ? yes Os(2) Os(4) C(10) 66.5(9) ? ? ? yes Os(3) Os(4) Os(5) 61.91(4) ? ? ? yes Os(3) Os(4) Os(6) 62.34(4) ? ? ? yes Os(3) Os(4) C(8) 132.5(8) ? ? ? yes Os(3) Os(4) C(9) 110.6(9) ? ? ? yes Os(3) Os(4) C(10) 127.0(9) ? ? ? yes Os(5) Os(4) Os(6) 61.31(4) ? ? ? yes Os(5) Os(4) C(8) 75.6(7) ? ? ? yes Os(5) Os(4) C(9) 151.5(8) ? ? ? yes Os(5) Os(4) C(10) 116.6(9) ? ? ? yes Os(6) Os(4) C(8) 79.7(9) ? ? ? yes Os(6) Os(4) C(9) 90.6(8) ? ? ? yes Os(6) Os(4) C(10) 169.3(8) ? ? ? yes C(8) Os(4) C(9) 96(1) ? ? ? yes C(8) Os(4) C(10) 89(1) ? ? ? yes C(9) Os(4) C(10) 90(1) ? ? ? yes Os(3) Os(5) Os(4) 58.11(4) ? ? ? yes Os(3) Os(5) Os(6) 60.08(4) ? ? ? yes Os(3) Os(5) S(2) 88.8(2) ? ? ? yes Os(3) Os(5) C(11) 107.3(9) ? ? ? yes Os(3) Os(5) C(12) 161.6(8) ? ? ? yes Os(4) Os(5) Os(6) 58.52(4) ? ? ? yes Os(4) Os(5) S(2) 85.3(2) ? ? ? yes Os(4) Os(5) C(11) 165.4(9) ? ? ? yes Os(4) Os(5) C(12) 104.5(8) ? ? ? yes Os(6) Os(5) S(2) 140.6(2) ? ? ? yes Os(6) Os(5) C(11) 115.0(8) ? ? ? yes Os(6) Os(5) C(12) 106.9(8) ? ? ? yes S(2) Os(5) C(11) 96.1(9) ? ? ? yes S(2) Os(5) C(12) 96.3(8) ? ? ? yes C(11) Os(5) C(12) 89(1) ? ? ? yes Os(3) Os(6) Os(4) 58.71(4) ? ? ? yes Os(3) Os(6) Os(5) 60.33(4) ? ? ? yes Os(3) Os(6) C(13) 96(1) ? ? ? yes Os(3) Os(6) C(14) 161.9(9) ? ? ? yes Os(3) Os(6) C(15) 98.1(10) ? ? ? yes Os(4) Os(6) Os(5) 60.16(4) ? ? ? yes Os(4) Os(6) C(13) 155(1) ? ? ? yes Os(4) Os(6) C(14) 106.5(9) ? ? ? yes Os(4) Os(6) C(15) 94.1(10) ? ? ? yes Os(5) Os(6) C(13) 105.1(8) ? ? ? yes Os(5) Os(6) C(14) 104.1(8) ? ? ? yes Os(5) Os(6) C(15) 152.0(9) ? ? ? yes C(13) Os(6) C(14) 96(1) ? ? ? yes C(13) Os(6) C(15) 94(1) ? ? ? yes C(14) Os(6) C(15) 93(1) ? ? ? yes Os(1) S(1) C(20) 109(1) ? ? ? yes Os(1) S(1) C(23) 111(1) ? ? ? yes C(20) S(1) C(23) 94(1) ? ? ? yes Os(2) S(2) Os(5) 99.1(2) ? ? ? yes Os(2) S(2) C(16) 115.6(10) ? ? ? yes Os(2) S(2) C(19) 116(1) ? ? ? yes Os(5) S(2) C(16) 115.5(10) ? ? ? yes Os(5) S(2) C(19) 113.5(10) ? ? ? yes C(16) S(2) C(19) 97(1) ? ? ? yes C(17) O(16) C(18) 111(2) ? ? ? yes C(21) O(17) C(22) 108(3) ? ? ? yes Os(1) C(1) O(1) 173(2) ? ? ? yes Os(1) C(2) O(2) 178(3) ? ? ? yes Os(2) C(3) O(3) 176(2) ? ? ? yes Os(2) C(4) O(4) 172(2) ? ? ? yes Os(3) C(5) O(5) 174(2) ? ? ? yes Os(3) C(6) O(6) 167(2) ? ? ? yes Os(3) C(7) O(7) 170(3) ? ? ? yes Os(4) C(8) O(8) 169(2) ? ? ? yes Os(4) C(9) O(9) 170(2) ? ? ? yes Os(4) C(10) O(10) 165(2) ? ? ? yes Os(5) C(11) O(11) 174(2) ? ? ? yes Os(5) C(12) O(12) 176(2) ? ? ? yes Os(6) C(13) O(13) 174(3) ? ? ? yes Os(6) C(14) O(14) 177(2) ? ? ? yes Os(6) C(15) O(15) 173(3) ? ? ? yes S(2) C(16) C(17) 110(1) ? ? ? yes O(16) C(17) C(16) 111(2) ? ? ? yes O(16) C(18) C(19) 112(2) ? ? ? yes S(2) C(19) C(18) 111(2) ? ? ? yes S(1) C(20) C(21) 108(3) ? ? ? yes O(17) C(21) C(20) 113(3) ? ? ? yes O(17) C(22) C(23) 112(3) ? ? ? yes S(1) C(23) C(22) 112(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 ;