Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Wing-Tak Wong' 'Yat Li' _publ_contact_author_name 'Prof Wing-Tak Wong' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong CHINA ; _publ_contact_author_email 'WTWONG@HKUCC.HKU.HK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The First Examples of Tetraosmium Carbonyl Clusters Containing m-NH2 Amido Ligand: Syntheses, Crystal Structures and Reactivities ; _publ_section_references ; Bruker AXS Inc. (1997-98) SMART version 5.054, Madison, Wisconsin, USA. Bruker AXS Inc. (1999) SAINT+, version 6.02, Madison, Wisconsin, USA. Molecular Structure Corporation (1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 Sheldrick, G.M. (1990) SHELXS-86, Acta Cryst., A46, 467-473. Sheldrick, G.M. (1998) SADABS, University of G\"ottingen, Germany. ; data_wt0165w_Yat025_compound_1 _database_code_CSD 192358 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 9 11:45:09 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'teXsan (MSC, 1992)' _computing_publication_material 'teXsan (MSC, 1992)' #------------------------------------------------------------------------------ _cell_length_a 15.986(1) _cell_length_b 17.119(1) _cell_length_c 17.981(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4920.8(5) _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 '-P 2ac 2ab' 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 'yellow' _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.090 _exptl_crystal_density_diffrn 3.137 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 1162.08 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H15 N O12 Os4 ' _chemical_formula_moiety 'C15 H15 N O12 Os4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4096.00 _exptl_absorpt_coefficient_mu 20.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_absorpt_correction_T_min 0.101 _exptl_absorpt_correction_T_max 0.156 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 31060 _reflns_number_total 6224 _reflns_number_gt 2743 _reflns_threshold_expression 'I>1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.093 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.5 _diffrn_reflns_theta_full 28.5 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 28.5 _diffrn_measured_fraction_theta_full 28.5 _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 32 -1.216 7.603 'International Tables' C 0 120 0.003 0.002 'International Tables' O 0 96 0.011 0.006 'International Tables' N 0 8 0.006 0.003 'International Tables' H 0 120 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) 0.87900(7) 0.26234(6) 0.49811(7) 0.0395(3) Uij ? ? Os(2) 0.79954(6) 0.11657(6) 0.49132(7) 0.0383(3) Uij ? ? Os(3) 0.79218(7) 0.21004(7) 0.36262(7) 0.0414(3) Uij ? ? Os(4) 0.95748(7) 0.14042(6) 0.40545(7) 0.0350(3) Uij ? ? O(1) 0.736(1) 0.343(1) 0.573(1) 0.088(10) Uij ? ? O(2) 0.983(1) 0.406(1) 0.489(1) 0.084(9) Uij ? ? O(3) 0.950(1) 0.212(1) 0.646(1) 0.078(9) Uij ? ? O(4) 0.642(1) 0.178(1) 0.562(2) 0.089(10) Uij ? ? O(5) 0.862(1) 0.034(1) 0.627(1) 0.068(8) Uij ? ? O(6) 0.717(2) -0.022(1) 0.428(2) 0.09(1) Uij ? ? O(7) 0.720(1) 0.077(2) 0.274(1) 0.10(1) Uij ? ? O(8) 0.797(2) 0.320(2) 0.231(2) 0.12(1) Uij ? ? O(9) 0.619(1) 0.259(1) 0.410(1) 0.078(8) Uij ? ? O(10) 1.082(1) 0.078(1) 0.520(1) 0.070(8) Uij ? ? O(11) 1.086(1) 0.210(1) 0.303(1) 0.075(8) Uij ? ? O(12) 0.926(1) 0.052(1) 0.268(1) 0.054(7) Uij ? ? N(1) 0.956(2) 0.035(1) 0.340(1) 0.059(9) Uij ? ? C(1) 0.789(2) 0.309(2) 0.543(2) 0.06(1) Uij ? ? C(2) 0.943(2) 0.352(2) 0.490(2) 0.06(1) Uij ? ? C(3) 0.921(2) 0.231(2) 0.592(2) 0.06(1) Uij ? ? C(4) 0.703(2) 0.156(2) 0.537(2) 0.05(1) Uij ? ? C(5) 0.837(2) 0.068(2) 0.581(2) 0.050(8) Uij ? ? C(6) 0.749(3) 0.032(2) 0.452(2) 0.09(2) Uij ? ? C(7) 0.747(2) 0.133(2) 0.308(2) 0.06(1) Uij ? ? C(8) 0.800(2) 0.277(2) 0.285(2) 0.07(1) Uij ? ? C(9) 0.686(2) 0.242(2) 0.388(2) 0.07(1) Uij ? ? C(10) 1.035(2) 0.101(2) 0.473(2) 0.050(10) Uij ? ? C(11) 1.039(2) 0.183(1) 0.344(2) 0.040(7) Uij ? ? C(12) 0.932(2) -0.015(2) 0.218(2) 0.060(8) Uij ? ? C(13) 0.885(3) -0.083(2) 0.245(2) 0.11(2) Uij ? ? C(14) 0.891(3) 0.020(2) 0.151(2) 0.11(2) Uij ? ? C(15) 1.018(3) -0.040(3) 0.201(2) 0.16(2) Uij ? ? H(1) 0.8095 0.3015 0.4195 0.0608 Uij ? ? H(2) 0.9884 0.2232 0.4661 0.0608 Uij ? ? H(3) 0.8951 0.1671 0.3208 0.0608 Uij ? ? H(4) 0.9042 0.0642 0.4591 0.0608 Uij ? ? H(5) 1.0052 0.0174 0.3367 0.0709 Uij ? ? H(6) 0.9253 0.0019 0.3603 0.0709 Uij ? ? H(7) 0.8292 -0.0672 0.2559 0.1368 Uij ? ? H(8) 0.8844 -0.1222 0.2081 0.1368 Uij ? ? H(9) 0.9105 -0.1023 0.2890 0.1368 Uij ? ? H(10) 0.9221 0.0640 0.1351 0.1372 Uij ? ? H(11) 0.8899 -0.0179 0.1119 0.1372 Uij ? ? H(12) 0.8357 0.0348 0.1630 0.1372 Uij ? ? H(13) 1.0439 -0.0599 0.2450 0.1941 Uij ? ? H(14) 1.0173 -0.0799 0.1642 0.1941 Uij ? ? H(15) 1.0494 0.0032 0.1832 0.1941 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) 0.0408(6) 0.0351(6) 0.0426(7) 0.0001(5) 0.0052(6) -0.0043(6) Os(2) 0.0357(6) 0.0362(6) 0.0430(8) -0.0028(5) 0.0029(6) 0.0031(6) Os(3) 0.0384(6) 0.0434(7) 0.0424(8) 0.0078(6) -0.0016(6) 0.0037(6) Os(4) 0.0330(5) 0.0346(6) 0.0372(7) 0.0014(5) 0.0005(5) -0.0032(6) O(1) 0.05(1) 0.09(2) 0.12(2) 0.00(1) 0.02(2) -0.03(2) O(2) 0.10(2) 0.06(1) 0.09(2) -0.04(1) 0.03(2) -0.02(1) O(3) 0.08(2) 0.11(2) 0.04(2) -0.04(1) -0.02(1) 0.01(2) O(4) 0.06(2) 0.08(2) 0.13(3) 0.02(1) 0.04(2) 0.01(2) O(5) 0.07(1) 0.08(2) 0.05(2) 0.02(1) 0.00(1) 0.03(1) O(6) 0.11(2) 0.08(2) 0.09(2) -0.04(2) 0.00(2) 0.00(2) O(7) 0.08(2) 0.12(2) 0.08(2) -0.02(2) -0.04(2) 0.00(2) O(8) 0.08(2) 0.16(3) 0.11(2) 0.06(2) 0.01(2) 0.07(2) O(9) 0.08(2) 0.11(2) 0.05(1) 0.05(1) 0.01(1) -0.03(1) O(10) 0.07(2) 0.04(1) 0.10(2) -0.01(1) -0.04(1) -0.01(1) O(11) 0.10(2) 0.07(2) 0.05(2) -0.02(1) 0.04(1) 0.00(1) O(12) 0.08(2) 0.05(1) 0.02(1) 0.00(1) -0.03(1) -0.01(1) N(1) 0.09(2) 0.03(1) 0.06(2) 0.01(1) -0.03(2) 0.00(1) C(1) 0.04(2) 0.07(2) 0.08(3) 0.01(2) 0.00(2) -0.04(2) C(2) 0.06(2) 0.06(2) 0.05(2) -0.01(2) 0.02(2) -0.04(2) C(3) 0.05(2) 0.10(3) 0.03(2) -0.03(2) 0.00(2) -0.01(2) C(4) 0.08(2) 0.03(2) 0.04(2) 0.00(2) 0.02(2) 0.00(1) C(6) 0.10(3) 0.07(3) 0.11(4) 0.02(2) 0.03(3) 0.05(3) C(7) 0.03(2) 0.11(3) 0.05(2) 0.01(2) 0.01(2) 0.02(2) C(8) 0.09(3) 0.06(2) 0.05(2) 0.01(2) 0.02(2) 0.02(2) C(9) 0.06(2) 0.06(2) 0.10(3) 0.03(2) 0.01(2) -0.01(2) C(10) 0.04(2) 0.04(2) 0.07(3) 0.00(1) 0.01(2) -0.04(2) C(13) 0.19(5) 0.05(2) 0.10(4) -0.02(3) -0.04(3) 0.00(3) C(14) 0.23(5) 0.08(3) 0.03(2) 0.04(3) 0.02(3) 0.00(2) C(15) 0.09(3) 0.32(7) 0.07(4) 0.09(4) -0.03(3) -0.02(4) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were attempted to be refined anisotropically, but some atoms [namely: C(5), C(11) and C(12)] were found unsuitable to be refined anisotropically, thus refined isotropic only. All hydride atoms were located from difference fourier map and potential energy calculations but were not refined. Hydrogens attached to organic moieties were refined as riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2743 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0514 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_shift/su_max 0.0122 _refine_ls_shift/su_mean ? _refine_diff_density_min -1.90 _refine_diff_density_max 1.81 #------------------------------------------------------------------------------ _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) 2.803(2) ? ? yes Os(1) Os(3) 2.943(2) ? ? yes Os(1) Os(4) 2.951(2) ? ? yes Os(1) C(1) 1.84(3) ? ? yes Os(1) C(2) 1.85(3) ? ? yes Os(1) C(3) 1.90(3) ? ? yes Os(2) Os(3) 2.816(2) ? ? yes Os(2) Os(4) 2.988(2) ? ? yes Os(2) C(4) 1.88(3) ? ? yes Os(2) C(5) 1.91(3) ? ? yes Os(2) C(6) 1.80(5) ? ? yes Os(3) Os(4) 2.999(2) ? ? yes Os(3) C(7) 1.79(4) ? ? yes Os(3) C(8) 1.81(3) ? ? yes Os(3) C(9) 1.85(3) ? ? yes Os(4) N(1) 2.15(2) ? ? yes Os(4) C(10) 1.86(3) ? ? yes Os(4) C(11) 1.86(3) ? ? yes O(1) C(1) 1.16(3) ? ? yes O(2) C(2) 1.13(3) ? ? yes O(3) C(3) 1.12(3) ? ? yes O(4) C(4) 1.14(3) ? ? yes O(5) C(5) 1.09(3) ? ? yes O(6) C(6) 1.15(4) ? ? yes O(7) C(7) 1.22(4) ? ? yes O(8) C(8) 1.21(3) ? ? yes O(9) C(9) 1.16(3) ? ? yes O(10) C(10) 1.20(3) ? ? yes O(11) C(11) 1.16(3) ? ? yes O(12) N(1) 1.40(3) ? ? yes O(12) C(12) 1.47(3) ? ? yes C(12) C(13) 1.46(5) ? ? yes C(12) C(14) 1.50(4) ? ? yes C(12) C(15) 1.47(5) ? ? yes Os(1) H(1) 1.919 ? ? yes Os(1) H(2) 1.960 ? ? yes Os(2) H(4) 1.985 ? ? yes Os(3) H(1) 1.891 ? ? yes Os(3) H(3) 1.953 ? ? yes Os(4) H(2) 1.855 ? ? yes Os(4) H(3) 1.876 ? ? yes Os(4) H(4) 1.833 ? ? yes N(1) H(5) 0.840 ? ? yes N(1) H(6) 0.840 ? ? yes C(13) H(7) 0.951 ? ? yes C(13) H(8) 0.950 ? ? yes C(13) H(9) 0.950 ? ? yes C(14) H(10) 0.950 ? ? yes C(14) H(11) 0.950 ? ? yes C(14) H(12) 0.951 ? ? yes C(15) H(13) 0.951 ? ? yes C(15) H(14) 0.949 ? ? yes C(15) H(15) 0.952 ? ? 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) 58.63(4) ? ? ? yes Os(2) Os(1) Os(4) 62.51(4) ? ? ? yes Os(2) Os(1) C(1) 93.0(9) ? ? ? yes Os(2) Os(1) C(2) 170.4(8) ? ? ? yes Os(2) Os(1) C(3) 86.9(9) ? ? ? yes Os(3) Os(1) Os(4) 61.18(4) ? ? ? yes Os(3) Os(1) C(1) 97.3(9) ? ? ? yes Os(3) Os(1) C(2) 116(1) ? ? ? yes Os(3) Os(1) C(3) 144.8(9) ? ? ? yes Os(4) Os(1) C(1) 153.0(9) ? ? ? yes Os(4) Os(1) C(2) 108.0(8) ? ? ? yes Os(4) Os(1) C(3) 98(1) ? ? ? yes C(1) Os(1) C(2) 96(1) ? ? ? yes C(1) Os(1) C(3) 90(1) ? ? ? yes C(2) Os(1) C(3) 96(1) ? ? ? yes Os(1) Os(2) Os(3) 63.18(4) ? ? ? yes Os(1) Os(2) Os(4) 61.17(4) ? ? ? yes Os(1) Os(2) C(4) 92.1(8) ? ? ? yes Os(1) Os(2) C(5) 102.2(8) ? ? ? yes Os(1) Os(2) C(6) 159(1) ? ? ? yes Os(3) Os(2) Os(4) 62.15(4) ? ? ? yes Os(3) Os(2) C(4) 97.0(9) ? ? ? yes Os(3) Os(2) C(5) 162.7(8) ? ? ? yes Os(3) Os(2) C(6) 96(1) ? ? ? yes Os(4) Os(2) C(4) 151.0(8) ? ? ? yes Os(4) Os(2) C(5) 103.5(8) ? ? ? yes Os(4) Os(2) C(6) 106(1) ? ? ? yes C(4) Os(2) C(5) 92(1) ? ? ? yes C(4) Os(2) C(6) 94(1) ? ? ? yes C(5) Os(2) C(6) 97(1) ? ? ? yes Os(1) Os(3) Os(2) 58.19(4) ? ? ? yes Os(1) Os(3) Os(4) 59.53(4) ? ? ? yes Os(1) Os(3) C(7) 150.1(10) ? ? ? yes Os(1) Os(3) C(8) 114(1) ? ? ? yes Os(1) Os(3) C(9) 97(1) ? ? ? yes Os(2) Os(3) Os(4) 61.73(4) ? ? ? yes Os(2) Os(3) C(7) 92.9(10) ? ? ? yes Os(2) Os(3) C(8) 172(1) ? ? ? yes Os(2) Os(3) C(9) 90(1) ? ? ? yes Os(4) Os(3) C(7) 101.7(9) ? ? ? yes Os(4) Os(3) C(8) 113(1) ? ? ? yes Os(4) Os(3) C(9) 150(1) ? ? ? yes C(7) Os(3) C(8) 94(1) ? ? ? yes C(7) Os(3) C(9) 89(1) ? ? ? yes C(8) Os(3) C(9) 93(1) ? ? ? yes Os(1) Os(4) Os(2) 56.32(3) ? ? ? yes Os(1) Os(4) Os(3) 59.29(4) ? ? ? yes Os(1) Os(4) N(1) 153.8(7) ? ? ? yes Os(1) Os(4) C(10) 100.0(7) ? ? ? yes Os(1) Os(4) C(11) 111.1(8) ? ? ? yes Os(2) Os(4) Os(3) 56.11(4) ? ? ? yes Os(2) Os(4) N(1) 99.3(7) ? ? ? yes Os(2) Os(4) C(10) 100.4(9) ? ? ? yes Os(2) Os(4) C(11) 162.6(8) ? ? ? yes Os(3) Os(4) N(1) 100.6(7) ? ? ? yes Os(3) Os(4) C(10) 154.1(8) ? ? ? yes Os(3) Os(4) C(11) 108.0(8) ? ? ? yes N(1) Os(4) C(10) 93.4(9) ? ? ? yes N(1) Os(4) C(11) 90(1) ? ? ? yes C(10) Os(4) C(11) 93(1) ? ? ? yes N(1) O(12) C(12) 112(2) ? ? ? yes Os(4) N(1) O(12) 109(1) ? ? ? yes Os(1) C(1) O(1) 175(2) ? ? ? yes Os(1) C(2) O(2) 175(3) ? ? ? yes Os(1) C(3) O(3) 176(2) ? ? ? yes Os(2) C(4) O(4) 176(3) ? ? ? yes Os(2) C(5) O(5) 172(2) ? ? ? yes Os(2) C(6) O(6) 178(3) ? ? ? yes Os(3) C(7) O(7) 175(2) ? ? ? yes Os(3) C(8) O(8) 173(3) ? ? ? yes Os(3) C(9) O(9) 174(3) ? ? ? yes Os(4) C(10) O(10) 175(2) ? ? ? yes Os(4) C(11) O(11) 176(2) ? ? ? yes O(12) C(12) C(13) 112(2) ? ? ? yes O(12) C(12) C(14) 98(2) ? ? ? yes O(12) C(12) C(15) 114(3) ? ? ? yes C(13) C(12) C(14) 111(3) ? ? ? yes C(13) C(12) C(15) 109(3) ? ? ? yes C(14) C(12) C(15) 110(3) ? ? ? yes Os(2) Os(1) H(1) 90.96 ? ? ? yes Os(2) Os(1) H(2) 95.01 ? ? ? yes Os(3) Os(1) H(1) 39.07 ? ? ? yes Os(3) Os(1) H(2) 94.21 ? ? ? yes Os(4) Os(1) H(1) 94.43 ? ? ? yes Os(4) Os(1) H(2) 38.06 ? ? ? yes C(1) Os(1) H(1) 73.62 ? ? ? yes C(1) Os(1) H(2) 168.22 ? ? ? yes C(2) Os(1) H(1) 88.39 ? ? ? yes C(2) Os(1) H(2) 76.61 ? ? ? yes C(3) Os(1) H(1) 163.93 ? ? ? yes C(3) Os(1) H(2) 81.27 ? ? ? yes H(1) Os(1) H(2) 114.80 ? ? ? yes Os(1) Os(2) H(4) 91.90 ? ? ? yes Os(3) Os(2) H(4) 92.97 ? ? ? yes Os(4) Os(2) H(4) 36.72 ? ? ? yes C(4) Os(2) H(4) 170.05 ? ? ? yes C(5) Os(2) H(4) 77.77 ? ? ? yes C(6) Os(2) H(4) 84.41 ? ? ? yes Os(1) Os(3) H(1) 39.75 ? ? ? yes Os(1) Os(3) H(3) 92.06 ? ? ? yes Os(2) Os(3) H(1) 91.14 ? ? ? yes Os(2) Os(3) H(3) 93.86 ? ? ? yes Os(4) Os(3) H(1) 93.49 ? ? ? yes Os(4) Os(3) H(3) 37.52 ? ? ? yes C(7) Os(3) H(1) 164.36 ? ? ? yes C(7) Os(3) H(3) 81.45 ? ? ? yes C(8) Os(3) H(1) 83.10 ? ? ? yes C(8) Os(3) H(3) 83.49 ? ? ? yes C(9) Os(3) H(1) 75.58 ? ? ? yes C(9) Os(3) H(3) 170.05 ? ? ? yes H(1) Os(3) H(3) 113.35 ? ? ? yes Os(1) Os(4) H(2) 40.64 ? ? ? yes Os(1) Os(4) H(3) 93.45 ? ? ? yes Os(1) Os(4) H(4) 90.52 ? ? ? yes Os(2) Os(4) H(2) 91.50 ? ? ? yes Os(2) Os(4) H(3) 90.21 ? ? ? yes Os(2) Os(4) H(4) 40.36 ? ? ? yes Os(3) Os(4) H(2) 94.72 ? ? ? yes Os(3) Os(4) H(3) 39.36 ? ? ? yes Os(3) Os(4) H(4) 90.49 ? ? ? yes N(1) Os(4) H(2) 164.41 ? ? ? yes N(1) Os(4) H(3) 75.81 ? ? ? yes N(1) Os(4) H(4) 71.83 ? ? ? yes C(10) Os(4) H(2) 73.48 ? ? ? yes C(10) Os(4) H(3) 166.05 ? ? ? yes C(10) Os(4) H(4) 73.28 ? ? ? yes C(11) Os(4) H(2) 82.39 ? ? ? yes C(11) Os(4) H(3) 78.00 ? ? ? yes C(11) Os(4) H(4) 156.54 ? ? ? yes H(2) Os(4) H(3) 115.62 ? ? ? yes H(2) Os(4) H(4) 111.04 ? ? ? yes H(3) Os(4) H(4) 110.68 ? ? ? yes Os(4) N(1) H(5) 109.47 ? ? ? yes Os(4) N(1) H(6) 109.46 ? ? ? yes O(12) N(1) H(5) 109.45 ? ? ? yes O(12) N(1) H(6) 109.44 ? ? ? yes H(5) N(1) H(6) 109.51 ? ? ? yes C(12) C(13) H(7) 109.51 ? ? ? yes C(12) C(13) H(8) 109.52 ? ? ? yes C(12) C(13) H(9) 109.52 ? ? ? yes H(7) C(13) H(8) 109.40 ? ? ? yes H(7) C(13) H(9) 109.40 ? ? ? yes H(8) C(13) H(9) 109.49 ? ? ? yes C(12) C(14) H(10) 109.55 ? ? ? yes C(12) C(14) H(11) 109.52 ? ? ? yes C(12) C(14) H(12) 109.49 ? ? ? yes H(10) C(14) H(11) 109.50 ? ? ? yes H(10) C(14) H(12) 109.38 ? ? ? yes H(11) C(14) H(12) 109.38 ? ? ? yes C(12) C(15) H(13) 109.56 ? ? ? yes C(12) C(15) H(14) 109.65 ? ? ? yes C(12) C(15) H(15) 109.50 ? ? ? yes H(13) C(15) H(14) 109.50 ? ? ? yes H(13) C(15) H(15) 109.25 ? ? ? yes H(14) C(15) H(15) 109.37 ? ? ? yes #------------------------------------------------------------------------------ data_wt0406w_YAT084_compound_2 _database_code_CSD 192359 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Oct 9 22:09:10 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'teXsan (MSC, 1992)' _computing_publication_material 'teXsan (MSC, 1992)' #------------------------------------------------------------------------------ _cell_length_a 10.022(1) _cell_length_b 14.121(1) _cell_length_c 15.772(2) _cell_angle_alpha 104.16(1) _cell_angle_beta 96.08(2) _cell_angle_gamma 107.32(1) _cell_volume 2027.2(4) _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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.516 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 1535.92 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H29 Cl N2 O15 Os5 ' _chemical_formula_moiety 'C21 H29 Cl N2 O15 Os5 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1372.00 _exptl_absorpt_coefficient_mu 15.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_absorpt_correction_T_min 0.121 _exptl_absorpt_correction_T_max 0.210 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 12880 _reflns_number_total 8851 _reflns_number_gt 5590 _reflns_threshold_expression 'I>1.5\(I)' _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 27.5 _diffrn_measured_fraction_theta_full 27.5 _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 10 -1.216 7.603 'International Tables' O 0 30 0.011 0.006 'International Tables' C 0 42 0.003 0.002 'International Tables' H 0 58 0.000 0.000 'International Tables' N 0 4 0.006 0.003 'International Tables' Cl 0 2 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.5883(1) 0.12522(9) 0.33589(8) 0.0623(4) Uij ? ? Os(2) 0.8424(1) 0.28919(10) 0.32125(8) 0.0668(4) Uij ? ? Os(3) 0.5998(1) 0.34197(9) 0.35791(8) 0.0635(4) Uij ? ? Os(4) 0.5773(1) 0.19042(8) 0.18415(7) 0.0495(3) Uij ? ? Os(5) 0.6010(1) 0.30184(8) 0.02306(7) 0.0509(3) Uij ? ? Cl(1) 0.5445(9) 0.4503(6) 0.1000(5) 0.077(3) Uij ? ? O(1) 0.652(3) -0.068(2) 0.237(2) 0.13(1) Uij ? ? O(2) 0.269(3) 0.005(3) 0.291(2) 0.13(1) Uij ? ? O(3) 0.626(4) 0.104(3) 0.522(2) 0.14(1) Uij ? ? O(4) 1.002(3) 0.382(2) 0.509(2) 0.15(1) Uij ? ? O(5) 1.049(4) 0.184(3) 0.247(2) 0.18(2) Uij ? ? O(6) 0.969(3) 0.488(2) 0.281(2) 0.13(1) Uij ? ? O(7) 0.737(5) 0.433(3) 0.556(2) 0.16(1) Uij ? ? O(8) 0.705(3) 0.550(2) 0.326(2) 0.15(1) Uij ? ? O(9) 0.318(4) 0.364(3) 0.377(3) 0.20(2) Uij ? ? O(10) 0.260(2) 0.092(2) 0.120(2) 0.087(8) Uij ? ? O(11) 0.645(2) 0.011(2) 0.067(1) 0.086(8) Uij ? ? O(12) 0.918(3) 0.421(2) 0.071(2) 0.13(1) Uij ? ? O(13) 0.673(2) 0.120(2) -0.083(2) 0.087(8) Uij ? ? O(14) 0.672(2) 0.325(2) -0.146(1) 0.085(8) Uij ? ? O(15) 0.307(2) 0.241(2) -0.088(1) 0.086(8) Uij ? ? N(1) 0.588(3) 0.359(2) -0.087(2) 0.09(1) Uij ? ? N(2) 0.369(3) 0.227(2) -0.007(2) 0.10(1) Uij ? ? C(1) 0.630(4) 0.007(3) 0.277(2) 0.08(1) Uij ? ? C(2) 0.389(5) 0.048(3) 0.308(3) 0.10(1) Uij ? ? C(3) 0.608(5) 0.106(4) 0.450(4) 0.14(2) Uij ? ? C(4) 0.941(4) 0.356(3) 0.440(3) 0.09(1) Uij ? ? C(5) 0.954(8) 0.220(5) 0.273(3) 0.22(3) Uij ? ? C(6) 0.917(3) 0.400(3) 0.290(2) 0.09(1) Uij ? ? C(7) 0.685(6) 0.409(3) 0.487(3) 0.14(2) Uij ? ? C(8) 0.667(3) 0.466(3) 0.332(2) 0.07(1) Uij ? ? C(9) 0.414(5) 0.354(3) 0.365(4) 0.12(2) Uij ? ? C(10) 0.382(4) 0.125(2) 0.144(2) 0.08(1) Uij ? ? C(11) 0.613(3) 0.078(2) 0.113(2) 0.055(8) Uij ? ? C(12) 0.793(5) 0.377(2) 0.052(2) 0.09(1) Uij ? ? C(13) 0.642(3) 0.188(2) -0.043(2) 0.060(9) Uij ? ? C(14) 0.670(4) 0.351(2) -0.232(2) 0.07(1) Uij ? ? C(15) 0.728(4) 0.468(3) -0.214(3) 0.11(2) Uij ? ? C(16) 0.770(5) 0.303(3) -0.271(3) 0.12(2) Uij ? ? C(17) 0.519(4) 0.300(4) -0.287(3) 0.13(2) Uij ? ? C(18) 0.149(4) 0.211(4) -0.095(3) 0.13(2) Uij ? ? C(19) 0.123(5) 0.229(5) -0.190(4) 0.19(3) Uij ? ? C(20) 0.085(4) 0.102(4) -0.106(4) 0.16(2) Uij ? ? C(21) 0.110(5) 0.283(5) -0.030(4) 0.29(3) Uij ? ? H(1) 0.7860 0.1742 0.3607 0.0608 Uij ? ? H(2) 0.5298 0.2302 0.3992 0.0608 Uij ? ? H(3) 0.5192 0.3023 0.2395 0.0608 Uij ? ? H(4) 0.7741 0.2432 0.2004 0.0608 Uij ? ? H(5) 0.7113 0.2592 0.1059 0.0608 Uij ? ? H(6) 0.4991 0.1712 0.0729 0.0608 Uij ? ? H(7) 0.5657 0.3154 0.1466 0.0608 Uij ? ? H(8) 0.5025 0.3372 -0.1134 0.1065 Uij ? ? H(9) 0.6172 0.4239 -0.0692 0.1065 Uij ? ? H(10) 0.3495 0.1634 -0.0131 0.1161 Uij ? ? H(11) 0.3348 0.2534 0.0355 0.1161 Uij ? ? H(12) 0.8172 0.4953 -0.1738 0.1300 Uij ? ? H(13) 0.7406 0.4835 -0.2686 0.1300 Uij ? ? H(14) 0.6629 0.4977 -0.1888 0.1300 Uij ? ? H(15) 0.7354 0.2306 -0.2785 0.1494 Uij ? ? H(16) 0.7770 0.3144 -0.3279 0.1494 Uij ? ? H(17) 0.8608 0.3332 -0.2333 0.1494 Uij ? ? H(18) 0.4550 0.3252 -0.2558 0.1536 Uij ? ? H(19) 0.5169 0.3164 -0.3424 0.1536 Uij ? ? H(20) 0.4913 0.2270 -0.2987 0.1536 Uij ? ? H(21) 0.1729 0.2987 -0.1859 0.2304 Uij ? ? H(22) 0.1576 0.1842 -0.2308 0.2304 Uij ? ? H(23) 0.0244 0.2131 -0.2099 0.2304 Uij ? ? H(24) -0.0147 0.0849 -0.1102 0.1963 Uij ? ? H(25) 0.1053 0.0633 -0.1579 0.1963 Uij ? ? H(26) 0.1241 0.0862 -0.0552 0.1963 Uij ? ? H(27) 0.1493 0.2853 0.0277 0.3523 Uij ? ? H(28) 0.1449 0.3503 -0.0382 0.3523 Uij ? ? H(29) 0.0088 0.2622 -0.0377 0.3523 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) 0.0786(8) 0.0499(6) 0.0613(8) 0.0253(6) 0.0157(6) 0.0154(6) Os(2) 0.0553(7) 0.0760(8) 0.0572(8) 0.0178(6) 0.0004(6) 0.0080(6) Os(3) 0.0849(9) 0.0498(6) 0.0587(8) 0.0311(6) 0.0188(7) 0.0082(6) Os(4) 0.0503(6) 0.0446(6) 0.0512(7) 0.0190(5) 0.0063(5) 0.0070(5) Os(5) 0.0530(6) 0.0514(6) 0.0519(7) 0.0263(5) 0.0085(5) 0.0109(5) Cl(1) 0.102(6) 0.074(5) 0.073(5) 0.055(5) 0.019(5) 0.020(4) O(1) 0.21(3) 0.08(2) 0.15(3) 0.10(2) 0.09(2) 0.03(2) O(2) 0.10(2) 0.16(3) 0.15(3) 0.03(2) 0.05(2) 0.08(2) O(3) 0.18(3) 0.19(3) 0.11(3) 0.11(3) 0.02(2) 0.07(2) O(4) 0.15(3) 0.16(3) 0.09(2) 0.04(2) -0.05(2) 0.01(2) O(5) 0.15(3) 0.27(5) 0.14(3) 0.12(3) 0.00(2) 0.02(3) O(6) 0.14(3) 0.12(2) 0.13(3) 0.02(2) 0.06(2) 0.04(2) O(7) 0.31(5) 0.14(3) 0.03(1) 0.10(3) 0.02(2) -0.01(2) O(8) 0.15(3) 0.08(2) 0.16(3) -0.01(2) -0.06(2) 0.04(2) O(9) 0.18(4) 0.14(3) 0.38(6) 0.12(3) 0.17(4) 0.11(3) O(10) 0.04(1) 0.08(1) 0.11(2) 0.01(1) 0.00(1) -0.01(1) O(11) 0.11(2) 0.08(1) 0.08(2) 0.08(1) 0.03(1) 0.00(1) O(12) 0.08(2) 0.12(2) 0.14(3) 0.00(2) 0.02(2) -0.01(2) O(13) 0.10(2) 0.07(1) 0.11(2) 0.05(1) 0.04(1) 0.02(1) O(14) 0.09(2) 0.11(2) 0.09(2) 0.07(1) 0.03(1) 0.03(1) O(15) 0.08(2) 0.09(2) 0.08(2) 0.04(1) -0.01(1) 0.02(1) N(1) 0.10(2) 0.09(2) 0.13(2) 0.06(2) 0.07(2) 0.06(2) N(2) 0.09(2) 0.12(2) 0.07(2) 0.07(2) -0.02(2) -0.02(2) C(1) 0.09(2) 0.07(2) 0.05(2) 0.00(2) 0.01(2) 0.02(2) C(2) 0.12(3) 0.06(2) 0.09(3) 0.01(2) 0.03(3) -0.01(2) C(3) 0.13(4) 0.19(5) 0.21(6) 0.09(4) 0.09(4) 0.17(5) C(4) 0.09(3) 0.10(3) 0.06(2) 0.01(2) 0.00(2) 0.01(2) C(5) 0.39(10) 0.24(6) 0.12(4) 0.26(7) 0.09(5) 0.00(4) C(6) 0.06(2) 0.15(4) 0.04(2) 0.04(2) 0.02(2) 0.00(2) C(7) 0.28(6) 0.04(2) 0.14(4) 0.07(3) 0.13(5) 0.04(2) C(8) 0.07(2) 0.09(2) 0.05(2) 0.02(2) 0.01(2) 0.01(2) C(9) 0.14(4) 0.06(2) 0.23(5) 0.08(2) 0.08(4) 0.06(3) C(10) 0.08(2) 0.07(2) 0.06(2) 0.04(2) 0.00(2) -0.03(2) C(11) 0.05(2) 0.05(2) 0.04(2) 0.00(1) -0.02(1) 0.01(1) C(12) 0.12(3) 0.05(2) 0.08(3) 0.03(2) 0.01(2) -0.01(2) C(13) 0.06(2) 0.06(2) 0.06(2) 0.02(1) 0.00(1) 0.02(1) C(14) 0.09(2) 0.06(2) 0.07(2) 0.04(2) 0.02(2) 0.02(2) C(15) 0.11(3) 0.13(4) 0.10(3) 0.05(3) 0.05(3) 0.04(3) C(16) 0.19(5) 0.12(3) 0.10(3) 0.10(3) 0.08(3) 0.02(3) C(17) 0.09(3) 0.16(4) 0.11(3) 0.01(3) -0.02(2) 0.04(3) C(18) 0.07(3) 0.18(5) 0.15(4) 0.07(3) 0.00(3) 0.04(4) C(19) 0.13(4) 0.22(6) 0.19(6) 0.06(4) -0.08(4) 0.03(5) C(20) 0.05(2) 0.15(4) 0.26(7) 0.03(3) -0.01(3) 0.03(5) C(21) 0.10(3) 0.38(8) 0.27(7) 0.17(5) -0.05(4) -0.22(6) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were refined anisotropically. All hydrides were located from difference fourier map and potential energy calculations but were not refined. Hydrogens attached to organic moieties were introduced on calculated positions and refined riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5590 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0908 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.964 _refine_ls_shift/su_max 0.0163 _refine_ls_shift/su_mean ? _refine_diff_density_min -3.51 _refine_diff_density_max 4.63 #------------------------------------------------------------------------------ _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) 2.962(2) ? ? yes Os(1) Os(3) 2.960(2) ? ? yes Os(1) Os(4) 2.769(2) ? ? yes Os(1) C(1) 1.89(4) ? ? yes Os(1) C(2) 1.91(4) ? ? yes Os(1) C(3) 1.89(5) ? ? yes Os(2) Os(3) 2.822(2) ? ? yes Os(2) Os(4) 2.963(2) ? ? yes Os(2) C(4) 1.88(4) ? ? yes Os(2) C(5) 1.80(5) ? ? yes Os(2) C(6) 1.73(4) ? ? yes Os(3) Os(4) 2.976(2) ? ? yes Os(3) C(7) 1.99(5) ? ? yes Os(3) C(8) 1.84(3) ? ? yes Os(3) C(9) 1.93(4) ? ? yes Os(4) C(10) 1.86(3) ? ? yes Os(4) C(11) 1.86(3) ? ? yes Os(5) Cl(1) 2.407(7) ? ? yes Os(5) N(1) 2.09(3) ? ? yes Os(5) N(2) 2.19(3) ? ? yes Os(5) C(12) 1.84(4) ? ? yes Os(5) C(13) 1.88(3) ? ? yes O(1) C(1) 1.18(4) ? ? yes O(2) C(2) 1.15(4) ? ? yes O(3) C(3) 1.14(5) ? ? yes O(4) C(4) 1.11(4) ? ? yes O(5) C(5) 1.26(5) ? ? yes O(6) C(6) 1.25(4) ? ? yes O(7) C(7) 1.09(6) ? ? yes O(8) C(8) 1.16(3) ? ? yes O(9) C(9) 1.05(4) ? ? yes O(10) C(10) 1.15(3) ? ? yes O(11) C(11) 1.19(3) ? ? yes O(12) C(12) 1.19(4) ? ? yes O(13) C(13) 1.16(3) ? ? yes O(14) N(1) 1.41(3) ? ? yes O(14) C(14) 1.49(3) ? ? yes O(15) N(2) 1.44(3) ? ? yes O(15) C(18) 1.50(4) ? ? yes C(14) C(15) 1.52(5) ? ? yes C(14) C(16) 1.47(4) ? ? yes C(14) C(17) 1.53(5) ? ? yes C(18) C(19) 1.58(7) ? ? yes C(18) C(20) 1.44(6) ? ? yes C(18) C(21) 1.43(6) ? ? yes Os(1) H(1) 1.856 ? ? yes Os(1) H(2) 1.859 ? ? yes Os(2) H(1) 1.834 ? ? yes Os(2) H(4) 1.837 ? ? yes Os(3) H(2) 1.830 ? ? yes Os(3) H(3) 1.832 ? ? yes Os(4) H(3) 1.892 ? ? yes Os(4) H(4) 1.853 ? ? yes Os(4) H(5) 2.106 ? ? yes Os(4) H(6) 1.765 ? ? yes Os(4) H(7) 2.025 ? ? yes Os(5) H(5) 1.940 ? ? yes Os(5) H(6) 2.197 ? ? yes Os(5) H(7) 1.990 ? ? yes N(1) H(8) 0.840 ? ? yes N(1) H(9) 0.840 ? ? yes N(2) H(10) 0.840 ? ? yes N(2) H(11) 0.840 ? ? yes C(15) H(12) 0.950 ? ? yes C(15) H(13) 0.950 ? ? yes C(15) H(14) 0.950 ? ? yes C(16) H(15) 0.950 ? ? yes C(16) H(16) 0.950 ? ? yes C(16) H(17) 0.950 ? ? yes C(17) H(18) 0.950 ? ? yes C(17) H(19) 0.950 ? ? yes C(17) H(20) 0.950 ? ? yes C(19) H(21) 0.950 ? ? yes C(19) H(22) 0.950 ? ? yes C(19) H(23) 0.950 ? ? yes C(20) H(24) 0.950 ? ? yes C(20) H(25) 0.950 ? ? yes C(20) H(26) 0.950 ? ? yes C(21) H(27) 0.950 ? ? yes C(21) H(28) 0.950 ? ? yes C(21) H(29) 0.950 ? ? 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) 56.91(4) ? ? ? yes Os(2) Os(1) Os(4) 62.15(4) ? ? ? yes Os(2) Os(1) C(1) 99.4(9) ? ? ? yes Os(2) Os(1) C(2) 153(1) ? ? ? yes Os(2) Os(1) C(3) 111(1) ? ? ? yes Os(3) Os(1) Os(4) 62.47(4) ? ? ? yes Os(3) Os(1) C(1) 150.6(9) ? ? ? yes Os(3) Os(1) C(2) 103(1) ? ? ? yes Os(3) Os(1) C(3) 107(1) ? ? ? yes Os(4) Os(1) C(1) 92.1(9) ? ? ? yes Os(4) Os(1) C(2) 93(1) ? ? ? yes Os(4) Os(1) C(3) 170(1) ? ? ? yes C(1) Os(1) C(2) 91(1) ? ? ? yes C(1) Os(1) C(3) 96(1) ? ? ? yes C(2) Os(1) C(3) 92(1) ? ? ? yes Os(1) Os(2) Os(3) 61.51(4) ? ? ? yes Os(1) Os(2) Os(4) 55.74(4) ? ? ? yes Os(1) Os(2) C(4) 104(1) ? ? ? yes Os(1) Os(2) C(5) 104(2) ? ? ? yes Os(1) Os(2) C(6) 150(1) ? ? ? yes Os(3) Os(2) Os(4) 61.86(4) ? ? ? yes Os(3) Os(2) C(4) 92(1) ? ? ? yes Os(3) Os(2) C(5) 161(2) ? ? ? yes Os(3) Os(2) C(6) 93.1(10) ? ? ? yes Os(4) Os(2) C(4) 152(1) ? ? ? yes Os(4) Os(2) C(5) 100(2) ? ? ? yes Os(4) Os(2) C(6) 99(1) ? ? ? yes C(4) Os(2) C(5) 103(2) ? ? ? yes C(4) Os(2) C(6) 91(1) ? ? ? yes C(5) Os(2) C(6) 96(2) ? ? ? yes Os(1) Os(3) Os(2) 61.57(4) ? ? ? yes Os(1) Os(3) Os(4) 55.62(4) ? ? ? yes Os(1) Os(3) C(7) 101(1) ? ? ? yes Os(1) Os(3) C(8) 150.9(10) ? ? ? yes Os(1) Os(3) C(9) 110.6(10) ? ? ? yes Os(2) Os(3) Os(4) 61.40(4) ? ? ? yes Os(2) Os(3) C(7) 92(1) ? ? ? yes Os(2) Os(3) C(8) 92.6(10) ? ? ? yes Os(2) Os(3) C(9) 169(1) ? ? ? yes Os(4) Os(3) C(7) 151(1) ? ? ? yes Os(4) Os(3) C(8) 101.5(9) ? ? ? yes Os(4) Os(3) C(9) 108(1) ? ? ? yes C(7) Os(3) C(8) 91(1) ? ? ? yes C(7) Os(3) C(9) 96(2) ? ? ? yes C(8) Os(3) C(9) 92(1) ? ? ? yes Os(1) Os(4) Os(2) 62.12(4) ? ? ? yes Os(1) Os(4) Os(3) 61.91(4) ? ? ? yes Os(1) Os(4) C(10) 95(1) ? ? ? yes Os(1) Os(4) C(11) 94.8(7) ? ? ? yes Os(2) Os(4) Os(3) 56.74(4) ? ? ? yes Os(2) Os(4) C(10) 154.5(9) ? ? ? yes Os(2) Os(4) C(11) 101.8(7) ? ? ? yes Os(3) Os(4) C(10) 103.6(8) ? ? ? yes Os(3) Os(4) C(11) 153.1(7) ? ? ? yes C(10) Os(4) C(11) 91(1) ? ? ? yes Cl(1) Os(5) N(1) 85.0(7) ? ? ? yes Cl(1) Os(5) N(2) 83.1(7) ? ? ? yes Cl(1) Os(5) C(12) 91.3(10) ? ? ? yes Cl(1) Os(5) C(13) 176.7(8) ? ? ? yes N(1) Os(5) N(2) 89(1) ? ? ? yes N(1) Os(5) C(12) 88(1) ? ? ? yes N(1) Os(5) C(13) 91(1) ? ? ? yes N(2) Os(5) C(12) 174(1) ? ? ? yes N(2) Os(5) C(13) 96(1) ? ? ? yes C(12) Os(5) C(13) 89(1) ? ? ? yes N(1) O(14) C(14) 118(2) ? ? ? yes N(2) O(15) C(18) 109(2) ? ? ? yes Os(5) N(1) O(14) 110(1) ? ? ? yes Os(5) N(2) O(15) 111(2) ? ? ? yes Os(1) C(1) O(1) 177(3) ? ? ? yes Os(1) C(2) O(2) 177(4) ? ? ? yes Os(1) C(3) O(3) 173(5) ? ? ? yes Os(2) C(4) O(4) 170(3) ? ? ? yes Os(2) C(5) O(5) 170(6) ? ? ? yes Os(2) C(6) O(6) 170(2) ? ? ? yes Os(3) C(7) O(7) 169(3) ? ? ? yes Os(3) C(8) O(8) 171(3) ? ? ? yes Os(3) C(9) O(9) 173(5) ? ? ? yes Os(4) C(10) O(10) 174(2) ? ? ? yes Os(4) C(11) O(11) 174(2) ? ? ? yes Os(5) C(12) O(12) 176(3) ? ? ? yes Os(5) C(13) O(13) 177(2) ? ? ? yes O(14) C(14) C(15) 110(2) ? ? ? yes O(14) C(14) C(16) 101(2) ? ? ? yes O(14) C(14) C(17) 108(2) ? ? ? yes C(15) C(14) C(16) 110(2) ? ? ? yes C(15) C(14) C(17) 113(3) ? ? ? yes C(16) C(14) C(17) 111(3) ? ? ? yes O(15) C(18) C(19) 93(3) ? ? ? yes O(15) C(18) C(20) 110(3) ? ? ? yes O(15) C(18) C(21) 112(4) ? ? ? yes C(19) C(18) C(20) 107(5) ? ? ? yes C(19) C(18) C(21) 110(5) ? ? ? yes C(20) C(18) C(21) 118(5) ? ? ? yes Os(2) Os(1) H(1) 36.37 ? ? ? yes Os(2) Os(1) H(2) 87.67 ? ? ? yes Os(3) Os(1) H(1) 87.66 ? ? ? yes Os(3) Os(1) H(2) 36.29 ? ? ? yes Os(4) Os(1) H(1) 92.39 ? ? ? yes Os(4) Os(1) H(2) 92.72 ? ? ? yes C(1) Os(1) H(1) 78.41 ? ? ? yes C(1) Os(1) H(2) 172.75 ? ? ? yes C(2) Os(1) H(1) 168.47 ? ? ? yes C(2) Os(1) H(2) 83.14 ? ? ? yes C(3) Os(1) H(1) 84.21 ? ? ? yes C(3) Os(1) H(2) 79.34 ? ? ? yes H(1) Os(1) H(2) 106.77 ? ? ? yes Os(1) Os(2) H(1) 36.88 ? ? ? yes Os(1) Os(2) H(4) 86.81 ? ? ? yes Os(3) Os(2) H(1) 92.40 ? ? ? yes Os(3) Os(2) H(4) 92.78 ? ? ? yes Os(4) Os(2) H(1) 86.85 ? ? ? yes Os(4) Os(2) H(4) 36.78 ? ? ? yes C(4) Os(2) H(1) 83.95 ? ? ? yes C(4) Os(2) H(4) 168.92 ? ? ? yes C(5) Os(2) H(1) 79.82 ? ? ? yes C(5) Os(2) H(4) 73.66 ? ? ? yes C(6) Os(2) H(1) 172.89 ? ? ? yes C(6) Os(2) H(4) 78.53 ? ? ? yes H(1) Os(2) H(4) 105.69 ? ? ? yes Os(1) Os(3) H(2) 36.96 ? ? ? yes Os(1) Os(3) H(3) 87.86 ? ? ? yes Os(2) Os(3) H(2) 92.61 ? ? ? yes Os(2) Os(3) H(3) 92.55 ? ? ? yes Os(4) Os(3) H(2) 86.90 ? ? ? yes Os(4) Os(3) H(3) 37.65 ? ? ? yes C(7) Os(3) H(2) 81.10 ? ? ? yes C(7) Os(3) H(3) 170.13 ? ? ? yes C(8) Os(3) H(2) 171.48 ? ? ? yes C(8) Os(3) H(3) 79.58 ? ? ? yes C(9) Os(3) H(2) 83.09 ? ? ? yes C(9) Os(3) H(3) 79.30 ? ? ? yes H(2) Os(3) H(3) 106.92 ? ? ? yes Os(1) Os(4) H(3) 92.54 ? ? ? yes Os(1) Os(4) H(4) 92.45 ? ? ? yes Os(1) Os(4) H(5) 141.12 ? ? ? yes Os(1) Os(4) H(6) 150.57 ? ? ? yes Os(1) Os(4) H(7) 139.70 ? ? ? yes Os(2) Os(4) H(3) 87.04 ? ? ? yes Os(2) Os(4) H(4) 36.41 ? ? ? yes Os(2) Os(4) H(5) 81.96 ? ? ? yes Os(2) Os(4) H(6) 145.31 ? ? ? yes Os(2) Os(4) H(7) 99.75 ? ? ? yes Os(3) Os(4) H(3) 36.26 ? ? ? yes Os(3) Os(4) H(4) 87.67 ? ? ? yes Os(3) Os(4) H(5) 111.42 ? ? ? yes Os(3) Os(4) H(6) 134.46 ? ? ? yes Os(3) Os(4) H(7) 77.96 ? ? ? yes C(10) Os(4) H(3) 82.19 ? ? ? yes C(10) Os(4) H(4) 168.43 ? ? ? yes C(10) Os(4) H(5) 122.61 ? ? ? yes C(10) Os(4) H(6) 59.60 ? ? ? yes C(10) Os(4) H(7) 90.36 ? ? ? yes C(11) Os(4) H(3) 170.47 ? ? ? yes C(11) Os(4) H(4) 79.74 ? ? ? yes C(11) Os(4) H(5) 77.59 ? ? ? yes C(11) Os(4) H(6) 72.41 ? ? ? yes C(11) Os(4) H(7) 125.07 ? ? ? yes H(3) Os(4) H(4) 106.09 ? ? ? yes H(3) Os(4) H(5) 100.39 ? ? ? yes H(3) Os(4) H(6) 98.29 ? ? ? yes H(3) Os(4) H(7) 48.73 ? ? ? yes H(4) Os(4) H(5) 48.77 ? ? ? yes H(4) Os(4) H(6) 110.43 ? ? ? yes H(4) Os(4) H(7) 89.31 ? ? ? yes H(5) Os(4) H(6) 63.36 ? ? ? yes H(5) Os(4) H(7) 56.36 ? ? ? yes H(6) Os(4) H(7) 61.57 ? ? ? yes Cl(1) Os(5) H(5) 110.68 ? ? ? yes Cl(1) Os(5) H(6) 108.59 ? ? ? yes Cl(1) Os(5) H(7) 60.96 ? ? ? yes N(1) Os(5) H(5) 148.99 ? ? ? yes N(1) Os(5) H(6) 142.75 ? ? ? yes N(1) Os(5) H(7) 145.36 ? ? ? yes N(2) Os(5) H(5) 117.73 ? ? ? yes N(2) Os(5) H(6) 58.96 ? ? ? yes N(2) Os(5) H(7) 80.66 ? ? ? yes C(12) Os(5) H(5) 65.59 ? ? ? yes C(12) Os(5) H(6) 124.71 ? ? ? yes C(12) Os(5) H(7) 97.91 ? ? ? yes C(13) Os(5) H(5) 72.54 ? ? ? yes C(13) Os(5) H(6) 73.67 ? ? ? yes C(13) Os(5) H(7) 122.19 ? ? ? yes H(5) Os(5) H(6) 59.14 ? ? ? yes H(5) Os(5) H(7) 59.54 ? ? ? yes H(6) Os(5) H(7) 55.33 ? ? ? yes Os(5) N(1) H(8) 109.33 ? ? ? yes Os(5) N(1) H(9) 109.32 ? ? ? yes O(14) N(1) H(8) 109.33 ? ? ? yes O(14) N(1) H(9) 109.33 ? ? ? yes H(8) N(1) H(9) 109.46 ? ? ? yes Os(5) N(2) H(10) 109.07 ? ? ? yes Os(5) N(2) H(11) 109.07 ? ? ? yes O(15) N(2) H(10) 109.08 ? ? ? yes O(15) N(2) H(11) 109.07 ? ? ? yes H(10) N(2) H(11) 109.45 ? ? ? yes C(14) C(15) H(12) 109.47 ? ? ? yes C(14) C(15) H(13) 109.47 ? ? ? yes C(14) C(15) H(14) 109.47 ? ? ? yes H(12) C(15) H(13) 109.47 ? ? ? yes H(12) C(15) H(14) 109.47 ? ? ? yes H(13) C(15) H(14) 109.47 ? ? ? yes C(14) C(16) H(15) 109.47 ? ? ? yes C(14) C(16) H(16) 109.47 ? ? ? yes C(14) C(16) H(17) 109.47 ? ? ? yes H(15) C(16) H(16) 109.47 ? ? ? yes H(15) C(16) H(17) 109.47 ? ? ? yes H(16) C(16) H(17) 109.47 ? ? ? yes C(14) C(17) H(18) 109.47 ? ? ? yes C(14) C(17) H(19) 109.47 ? ? ? yes C(14) C(17) H(20) 109.47 ? ? ? yes H(18) C(17) H(19) 109.47 ? ? ? yes H(18) C(17) H(20) 109.47 ? ? ? yes H(19) C(17) H(20) 109.48 ? ? ? yes C(18) C(19) H(21) 109.47 ? ? ? yes C(18) C(19) H(22) 109.47 ? ? ? yes C(18) C(19) H(23) 109.47 ? ? ? yes H(21) C(19) H(22) 109.47 ? ? ? yes H(21) C(19) H(23) 109.47 ? ? ? yes H(22) C(19) H(23) 109.47 ? ? ? yes C(18) C(20) H(24) 109.47 ? ? ? yes C(18) C(20) H(25) 109.47 ? ? ? yes C(18) C(20) H(26) 109.47 ? ? ? yes H(24) C(20) H(25) 109.47 ? ? ? yes H(24) C(20) H(26) 109.47 ? ? ? yes H(25) C(20) H(26) 109.47 ? ? ? yes C(18) C(21) H(27) 109.47 ? ? ? yes C(18) C(21) H(28) 109.47 ? ? ? yes C(18) C(21) H(29) 109.47 ? ? ? yes H(27) C(21) H(28) 109.47 ? ? ? yes H(27) C(21) H(29) 109.47 ? ? ? yes H(28) C(21) H(29) 109.47 ? ? ? yes #----------------------------------------------------------------------------- data_wt0528w_YAT100_compound_3 _database_code_CSD 192360 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Oct 13 11:49:52 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'teXsan (MSC, 1992)' _computing_publication_material 'teXsan (MSC, 1992)' #------------------------------------------------------------------------------ _cell_length_a 9.363(1) _cell_length_b 14.601(1) _cell_length_c 15.911(1) _cell_angle_alpha 64.99(2) _cell_angle_beta 85.13(1) _cell_angle_gamma 82.34(2) _cell_volume 1952.6(4) _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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.110 _exptl_crystal_density_diffrn 3.489 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 2051.61 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H7 Cl2 N O22 Os7' _chemical_formula_moiety 'C22 H5 N O22 Os7, C H2 Cl2' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1788.00 _exptl_absorpt_coefficient_mu 22.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_absorpt_correction_T_min 0.006 _exptl_absorpt_correction_T_max 0.081 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 12297 _reflns_number_total 8497 _reflns_number_gt 5386 _reflns_threshold_expression 'I>\1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 27.5 _diffrn_measured_fraction_theta_full 27.5 _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 14 -1.216 7.603 'International Tables' N 0 2 0.006 0.003 'International Tables' C 0 46 0.003 0.002 'International Tables' H 0 14 0.000 0.000 'International Tables' O 0 44 0.011 0.006 'International Tables' Cl 0 4 0.148 0.159 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.65602(9) 0.13219(7) 0.66908(6) 0.0366(2) Uij ? ? Os(2) 0.45147(8) -0.00256(7) 0.76413(6) 0.0312(2) Uij ? ? Os(3) 0.35213(9) 0.19381(7) 0.61204(6) 0.0397(3) Uij ? ? Os(4) 0.42511(10) 0.17503(7) 0.78527(7) 0.0420(3) Uij ? ? Os(5) 0.33298(9) -0.16965(7) 0.75503(6) 0.0333(2) Uij ? ? Os(6) 0.25671(10) -0.36453(7) 0.78614(6) 0.0408(3) Uij ? ? Os(7) 0.23392(9) -0.31605(7) 0.94716(6) 0.0390(3) Uij ? ? Cl(1) 1.171(2) 0.463(2) 0.292(1) 0.31(1) Uij ? ? Cl(2) 0.936(2) 0.445(2) 0.429(2) 0.40(2) Uij ? ? O(1) 0.710(2) 0.345(1) 0.642(2) 0.103(8) Uij ? ? O(2) 0.855(2) 0.031(2) 0.836(1) 0.074(6) Uij ? ? O(3) 0.895(2) 0.145(1) 0.521(1) 0.071(6) Uij ? ? O(4) 0.616(2) -0.146(1) 0.933(1) 0.067(6) Uij ? ? O(5) 0.176(1) -0.009(1) 0.883(1) 0.054(5) Uij ? ? O(6) 0.285(2) 0.175(2) 0.436(1) 0.101(9) Uij ? ? O(7) 0.039(2) 0.216(2) 0.679(1) 0.084(6) Uij ? ? O(8) 0.368(3) 0.421(1) 0.525(2) 0.107(8) Uij ? ? O(9) 0.451(3) 0.392(1) 0.744(2) 0.103(8) Uij ? ? O(10) 0.604(2) 0.085(2) 0.958(1) 0.076(7) Uij ? ? O(11) 0.142(2) 0.202(2) 0.882(2) 0.101(8) Uij ? ? O(12) 0.383(2) -0.081(1) 0.552(1) 0.067(5) Uij ? ? O(13) 0.650(2) -0.255(1) 0.785(1) 0.055(4) Uij ? ? O(14) 0.041(2) -0.042(1) 0.706(1) 0.070(6) Uij ? ? O(15) 0.567(2) -0.463(1) 0.836(1) 0.069(5) Uij ? ? O(16) 0.338(2) -0.350(2) 0.592(1) 0.094(7) Uij ? ? O(17) 0.143(2) -0.567(1) 0.868(2) 0.098(8) Uij ? ? O(18) -0.039(2) -0.245(2) 0.715(2) 0.085(8) Uij ? ? O(19) 0.555(2) -0.384(1) 0.988(1) 0.068(5) Uij ? ? O(20) 0.140(2) -0.527(1) 1.058(1) 0.072(6) Uij ? ? O(21) -0.076(2) -0.225(2) 0.896(1) 0.083(6) Uij ? ? O(22) 0.207(2) -0.260(2) 1.110(1) 0.086(6) Uij ? ? N(1) 0.617(2) -0.011(1) 0.673(1) 0.036(4) Uij ? ? C(1) 0.682(2) 0.270(2) 0.651(2) 0.049(6) Uij ? ? C(2) 0.786(2) 0.071(2) 0.773(2) 0.042(7) Uij ? ? C(3) 0.807(2) 0.140(2) 0.575(2) 0.045(6) Uij ? ? C(4) 0.553(2) -0.092(1) 0.869(1) 0.033(5) Uij ? ? C(5) 0.278(2) -0.002(2) 0.839(1) 0.037(6) Uij ? ? C(6) 0.320(3) 0.183(2) 0.500(1) 0.060(7) Uij ? ? C(7) 0.159(2) 0.212(2) 0.651(2) 0.057(7) Uij ? ? C(8) 0.362(3) 0.333(2) 0.561(2) 0.072(7) Uij ? ? C(9) 0.439(3) 0.307(2) 0.762(2) 0.059(7) Uij ? ? C(10) 0.536(3) 0.115(2) 0.896(2) 0.060(8) Uij ? ? C(11) 0.247(3) 0.194(2) 0.842(2) 0.075(10) Uij ? ? C(12) 0.364(2) -0.116(1) 0.630(1) 0.037(4) Uij ? ? C(13) 0.533(2) -0.224(2) 0.775(1) 0.057(6) Uij ? ? C(14) 0.143(2) -0.090(2) 0.727(2) 0.049(7) Uij ? ? C(15) 0.451(2) -0.426(2) 0.819(2) 0.044(6) Uij ? ? C(16) 0.308(3) -0.349(2) 0.661(2) 0.060(8) Uij ? ? C(17) 0.185(2) -0.493(2) 0.834(2) 0.063(7) Uij ? ? C(18) 0.066(3) -0.284(2) 0.744(2) 0.063(8) Uij ? ? C(19) 0.438(2) -0.366(2) 0.973(2) 0.062(6) Uij ? ? C(20) 0.178(2) -0.451(2) 1.017(2) 0.046(6) Uij ? ? C(21) 0.038(2) -0.258(2) 0.914(2) 0.058(7) Uij ? ? C(22) 0.213(3) -0.272(2) 1.047(2) 0.057(7) Uij ? ? C(23) 1.039(5) 0.531(2) 0.338(3) 0.207(7) Uij ? ? H(1) 0.3178 0.0606 0.6636 0.0608 Uij ? ? H(2) 0.5421 0.2068 0.5637 0.0608 Uij ? ? H(3) 0.2981 -0.1827 0.8821 0.0608 Uij ? ? H(4) 0.5905 -0.0093 0.6204 0.0431 Uij ? ? H(5) 0.6858 -0.0613 0.6965 0.0431 Uij ? ? H(6) 1.0864 0.5682 0.3622 0.2481 Uij ? ? H(7) 0.9777 0.5764 0.2903 0.2481 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) 0.0296(4) 0.0390(5) 0.0419(5) -0.0067(4) -0.0001(4) -0.0170(4) Os(2) 0.0305(4) 0.0323(5) 0.0337(5) -0.0033(4) -0.0008(4) -0.0168(4) Os(3) 0.0346(5) 0.0375(5) 0.0444(5) -0.0012(4) -0.0069(4) -0.0144(4) Os(4) 0.0400(5) 0.0437(6) 0.0538(6) -0.0040(4) -0.0007(4) -0.0317(5) Os(5) 0.0322(4) 0.0324(5) 0.0366(5) -0.0042(4) -0.0005(4) -0.0156(4) Os(6) 0.0404(5) 0.0369(5) 0.0491(6) -0.0077(4) 0.0004(4) -0.0211(5) Os(7) 0.0351(5) 0.0402(6) 0.0392(5) -0.0053(4) 0.0020(4) -0.0143(4) Cl(1) 0.22(2) 0.48(4) 0.37(3) -0.08(2) 0.06(2) -0.32(3) Cl(2) 0.39(3) 0.68(5) 0.38(3) -0.40(4) 0.20(2) -0.40(3) O(1) 0.07(1) 0.05(1) 0.22(2) -0.04(1) 0.03(1) -0.09(2) O(2) 0.05(1) 0.12(2) 0.047(9) 0.00(1) -0.011(6) -0.03(1) O(3) 0.05(1) 0.10(2) 0.05(1) -0.01(1) 0.023(7) -0.03(1) O(4) 0.06(1) 0.08(1) 0.041(9) 0.021(9) -0.018(7) -0.010(8) O(5) 0.033(7) 0.08(1) 0.07(1) -0.007(8) 0.020(6) -0.06(1) O(6) 0.10(2) 0.18(2) 0.04(1) 0.00(2) -0.03(1) -0.07(1) O(7) 0.037(7) 0.10(2) 0.09(1) 0.00(1) 0.010(9) -0.02(1) O(8) 0.13(2) 0.039(5) 0.14(2) -0.02(1) 0.00(2) -0.03(1) O(9) 0.14(2) 0.051(9) 0.15(2) -0.04(1) 0.04(2) -0.07(1) O(10) 0.07(1) 0.13(2) 0.053(10) -0.02(1) -0.014(7) -0.05(1) O(11) 0.05(1) 0.12(2) 0.15(2) 0.00(1) 0.05(1) -0.09(2) O(12) 0.08(1) 0.08(1) 0.037(3) 0.00(1) 0.001(9) -0.027(9) O(13) 0.038(5) 0.04(1) 0.06(1) 0.002(7) -0.009(8) -0.005(9) O(14) 0.040(8) 0.08(1) 0.07(1) 0.021(7) -0.025(9) -0.02(1) O(15) 0.049(7) 0.06(1) 0.08(1) 0.017(8) -0.016(9) -0.02(1) O(16) 0.11(2) 0.12(2) 0.040(9) -0.02(1) 0.03(1) -0.02(1) O(17) 0.12(2) 0.039(10) 0.13(2) -0.05(1) 0.06(1) -0.03(1) O(18) 0.038(9) 0.11(2) 0.13(2) 0.018(8) -0.030(10) -0.08(2) O(19) 0.045(6) 0.06(1) 0.06(1) 0.011(9) -0.008(9) 0.005(10) O(20) 0.07(1) 0.046(9) 0.09(1) -0.023(9) 0.00(1) -0.007(9) O(21) 0.038(7) 0.11(2) 0.10(1) 0.020(9) -0.007(9) -0.04(1) N(1) 0.033(9) 0.038(8) 0.043(10) 0.007(8) 0.002(5) -0.027(9) C(1) 0.04(1) 0.042(9) 0.08(2) 0.00(1) 0.00(1) -0.03(1) C(2) 0.03(1) 0.05(2) 0.06(1) 0.007(10) -0.017(8) -0.04(1) C(3) 0.03(1) 0.05(1) 0.05(1) 0.01(1) -0.003(6) -0.01(1) C(4) 0.04(1) 0.02(1) 0.04(1) -0.013(8) -0.007(8) -0.006(7) C(5) 0.044(10) 0.05(1) 0.02(1) -0.01(1) 0.004(7) -0.02(1) C(6) 0.06(2) 0.07(2) 0.02(1) 0.02(1) 0.020(10) 0.00(1) C(7) 0.040(8) 0.06(2) 0.06(2) 0.00(1) 0.01(1) -0.02(1) C(8) 0.04(1) 0.038(4) 0.11(2) 0.00(1) -0.01(2) 0.00(2) C(9) 0.06(2) 0.049(10) 0.08(2) -0.03(1) 0.04(1) -0.04(2) C(10) 0.06(2) 0.11(2) 0.04(1) -0.03(1) 0.014(7) -0.05(1) C(11) 0.04(1) 0.07(2) 0.13(3) 0.01(1) 0.02(1) -0.07(2) C(12) 0.05(1) 0.02(1) 0.035(3) -0.012(9) -0.015(9) 0.005(10) C(13) 0.039(7) 0.07(2) 0.03(1) 0.01(1) -0.02(1) 0.01(1) C(14) 0.037(9) 0.04(1) 0.08(2) 0.004(8) -0.01(1) -0.04(1) C(15) 0.042(7) 0.04(1) 0.04(1) -0.006(9) 0.005(10) 0.00(1) C(16) 0.07(2) 0.07(2) 0.044(10) -0.02(2) -0.01(1) -0.02(1) C(17) 0.04(1) 0.04(1) 0.08(2) -0.01(1) 0.02(1) 0.00(1) C(18) 0.04(1) 0.07(2) 0.07(2) -0.005(9) 0.00(1) -0.02(2) C(19) 0.041(6) 0.06(2) 0.04(1) 0.03(1) 0.01(1) 0.02(1) C(20) 0.05(1) 0.037(9) 0.04(1) 0.007(10) 0.00(1) 0.00(1) C(21) 0.036(8) 0.07(2) 0.05(1) 0.00(1) 0.00(1) -0.01(1) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were attempted to be refined anisotropically, but some atoms [namely: C(22) and C(23)] were found unsuitable to be refined anisotropically, thus refined isotropic only. All hydride atoms were located from difference fourier map and potential energy calculations but were not refined. Hydrogens attached to organic moieties were refined as riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5386 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0553 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_shift/su_max 0.0130 _refine_ls_shift/su_mean ? _refine_diff_density_min -2.26 _refine_diff_density_max 2.81 #------------------------------------------------------------------------------ _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) 2.797(1) ? ? yes Os(1) Os(3) 2.966(1) ? ? yes Os(1) Os(4) 2.902(1) ? ? yes Os(1) N(1) 2.15(2) ? ? yes Os(1) C(1) 1.95(3) ? ? yes Os(1) C(2) 1.95(2) ? ? yes Os(1) C(3) 1.95(2) ? ? yes Os(2) Os(3) 2.957(1) ? ? yes Os(2) Os(4) 2.730(1) ? ? yes Os(2) Os(5) 2.872(1) ? ? yes Os(2) N(1) 2.06(2) ? ? yes Os(2) C(4) 1.87(2) ? ? yes Os(2) C(5) 1.93(2) ? ? yes Os(3) Os(4) 2.787(1) ? ? yes Os(3) C(6) 1.92(3) ? ? yes Os(3) C(7) 1.88(2) ? ? yes Os(3) C(8) 1.86(3) ? ? yes Os(4) C(9) 1.82(3) ? ? yes Os(4) C(10) 1.93(3) ? ? yes Os(4) C(11) 1.87(2) ? ? yes Os(5) Os(6) 2.853(1) ? ? yes Os(5) Os(7) 3.049(1) ? ? yes Os(5) C(12) 1.81(2) ? ? yes Os(5) C(13) 1.93(2) ? ? yes Os(5) C(14) 1.97(2) ? ? yes Os(6) Os(7) 2.917(1) ? ? yes Os(6) C(15) 1.93(2) ? ? yes Os(6) C(16) 1.93(3) ? ? yes Os(6) C(17) 1.89(3) ? ? yes Os(6) C(18) 2.00(3) ? ? yes Os(7) C(19) 1.96(2) ? ? yes Os(7) C(20) 1.93(3) ? ? yes Os(7) C(21) 1.93(2) ? ? yes Os(7) C(22) 1.94(3) ? ? yes Cl(1) C(23) 1.78(2) ? ? yes Cl(2) C(23) 1.78(2) ? ? yes O(1) C(1) 1.10(3) ? ? yes O(2) C(2) 1.13(2) ? ? yes O(3) C(3) 1.12(2) ? ? yes O(4) C(4) 1.14(2) ? ? yes O(5) C(5) 1.13(2) ? ? yes O(6) C(6) 1.15(3) ? ? yes O(7) C(7) 1.18(3) ? ? yes O(8) C(8) 1.17(3) ? ? yes O(9) C(9) 1.17(3) ? ? yes O(10) C(10) 1.11(3) ? ? yes O(11) C(11) 1.15(3) ? ? yes O(12) C(12) 1.14(2) ? ? yes O(13) C(13) 1.12(3) ? ? yes O(14) C(14) 1.09(3) ? ? yes O(15) C(15) 1.15(3) ? ? yes O(16) C(16) 1.13(3) ? ? yes O(17) C(17) 1.10(3) ? ? yes O(18) C(18) 1.10(3) ? ? yes O(19) C(19) 1.12(3) ? ? yes O(20) C(20) 1.11(3) ? ? yes O(21) C(21) 1.12(3) ? ? yes O(22) C(22) 1.09(3) ? ? yes Os(1) H(2) 1.893 ? ? yes Os(2) H(1) 1.939 ? ? yes Os(3) H(1) 1.825 ? ? yes Os(3) H(2) 1.877 ? ? yes Os(5) H(3) 1.952 ? ? yes Os(7) H(3) 1.931 ? ? yes N(1) H(4) 0.880 ? ? yes N(1) H(5) 0.880 ? ? yes C(23) H(6) 0.951 ? ? yes C(23) H(7) 0.948 ? ? 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) 61.67(3) ? ? ? yes Os(2) Os(1) Os(4) 57.20(3) ? ? ? yes Os(2) Os(1) N(1) 47.0(4) ? ? ? yes Os(2) Os(1) C(1) 134.6(7) ? ? ? yes Os(2) Os(1) C(2) 92.3(7) ? ? ? yes Os(2) Os(1) C(3) 134.8(8) ? ? ? yes Os(3) Os(1) Os(4) 56.71(3) ? ? ? yes Os(3) Os(1) N(1) 83.8(4) ? ? ? yes Os(3) Os(1) C(1) 91.9(7) ? ? ? yes Os(3) Os(1) C(2) 146.1(7) ? ? ? yes Os(3) Os(1) C(3) 118.9(7) ? ? ? yes Os(4) Os(1) N(1) 104.1(4) ? ? ? yes Os(4) Os(1) C(1) 77.5(7) ? ? ? yes Os(4) Os(1) C(2) 91.7(7) ? ? ? yes Os(4) Os(1) C(3) 166.0(7) ? ? ? yes N(1) Os(1) C(1) 173.3(9) ? ? ? yes N(1) Os(1) C(2) 93.9(9) ? ? ? yes N(1) Os(1) C(3) 87.9(9) ? ? ? yes C(1) Os(1) C(2) 92(1) ? ? ? yes C(1) Os(1) C(3) 89(1) ? ? ? yes C(2) Os(1) C(3) 94.7(9) ? ? ? yes Os(1) Os(2) Os(3) 61.97(3) ? ? ? yes Os(1) Os(2) Os(4) 63.34(3) ? ? ? yes Os(1) Os(2) Os(5) 138.98(4) ? ? ? yes Os(1) Os(2) N(1) 49.7(5) ? ? ? yes Os(1) Os(2) C(4) 100.8(6) ? ? ? yes Os(1) Os(2) C(5) 136.8(7) ? ? ? yes Os(3) Os(2) Os(4) 58.54(3) ? ? ? yes Os(3) Os(2) Os(5) 111.95(4) ? ? ? yes Os(3) Os(2) N(1) 85.4(5) ? ? ? yes Os(3) Os(2) C(4) 157.6(6) ? ? ? yes Os(3) Os(2) C(5) 93.0(7) ? ? ? yes Os(4) Os(2) Os(5) 152.24(4) ? ? ? yes Os(4) Os(2) N(1) 112.9(5) ? ? ? yes Os(4) Os(2) C(4) 101.8(7) ? ? ? yes Os(4) Os(2) C(5) 73.6(7) ? ? ? yes Os(5) Os(2) N(1) 90.6(5) ? ? ? yes Os(5) Os(2) C(4) 90.5(6) ? ? ? yes Os(5) Os(2) C(5) 81.5(7) ? ? ? yes N(1) Os(2) C(4) 93.9(8) ? ? ? yes N(1) Os(2) C(5) 170.8(8) ? ? ? yes C(4) Os(2) C(5) 91.0(9) ? ? ? yes Os(1) Os(3) Os(2) 56.36(3) ? ? ? yes Os(1) Os(3) Os(4) 60.49(3) ? ? ? yes Os(1) Os(3) C(6) 112.7(7) ? ? ? yes Os(1) Os(3) C(7) 146.0(8) ? ? ? yes Os(1) Os(3) C(8) 96.7(8) ? ? ? yes Os(2) Os(3) Os(4) 56.65(3) ? ? ? yes Os(2) Os(3) C(6) 113.4(8) ? ? ? yes Os(2) Os(3) C(7) 100.5(8) ? ? ? yes Os(2) Os(3) C(8) 144.5(10) ? ? ? yes Os(4) Os(3) C(6) 169.7(8) ? ? ? yes Os(4) Os(3) C(7) 86.3(9) ? ? ? yes Os(4) Os(3) C(8) 91(1) ? ? ? yes C(6) Os(3) C(7) 98(1) ? ? ? yes C(6) Os(3) C(8) 97(1) ? ? ? yes C(7) Os(3) C(8) 90(1) ? ? ? yes Os(1) Os(4) Os(2) 59.46(3) ? ? ? yes Os(1) Os(4) Os(3) 62.79(3) ? ? ? yes Os(1) Os(4) C(9) 103.0(8) ? ? ? yes Os(1) Os(4) C(10) 94.3(7) ? ? ? yes Os(1) Os(4) C(11) 165.5(10) ? ? ? yes Os(2) Os(4) Os(3) 64.82(4) ? ? ? yes Os(2) Os(4) C(9) 160.9(8) ? ? ? yes Os(2) Os(4) C(10) 92.8(9) ? ? ? yes Os(2) Os(4) C(11) 110.8(9) ? ? ? yes Os(3) Os(4) C(9) 101.5(9) ? ? ? yes Os(3) Os(4) C(10) 153.5(8) ? ? ? yes Os(3) Os(4) C(11) 103(1) ? ? ? yes C(9) Os(4) C(10) 96(1) ? ? ? yes C(9) Os(4) C(11) 84(1) ? ? ? yes C(10) Os(4) C(11) 97(1) ? ? ? yes Os(2) Os(5) Os(6) 165.66(4) ? ? ? yes Os(2) Os(5) Os(7) 110.87(4) ? ? ? yes Os(2) Os(5) C(12) 90.4(7) ? ? ? yes Os(2) Os(5) C(13) 79.6(9) ? ? ? yes Os(2) Os(5) C(14) 90.7(7) ? ? ? yes Os(6) Os(5) Os(7) 59.13(3) ? ? ? yes Os(6) Os(5) C(12) 100.2(7) ? ? ? yes Os(6) Os(5) C(13) 90.4(9) ? ? ? yes Os(6) Os(5) C(14) 99.8(7) ? ? ? yes Os(7) Os(5) C(12) 158.7(7) ? ? ? yes Os(7) Os(5) C(13) 93.6(7) ? ? ? yes Os(7) Os(5) C(14) 93.2(8) ? ? ? yes C(12) Os(5) C(13) 91.1(10) ? ? ? yes C(12) Os(5) C(14) 85(1) ? ? ? yes C(13) Os(5) C(14) 169(1) ? ? ? yes Os(5) Os(6) Os(7) 63.78(3) ? ? ? yes Os(5) Os(6) C(15) 91.4(8) ? ? ? yes Os(5) Os(6) C(16) 94.0(8) ? ? ? yes Os(5) Os(6) C(17) 165.7(9) ? ? ? yes Os(5) Os(6) C(18) 81.9(9) ? ? ? yes Os(7) Os(6) C(15) 89.0(8) ? ? ? yes Os(7) Os(6) C(16) 157.5(8) ? ? ? yes Os(7) Os(6) C(17) 102.5(9) ? ? ? yes Os(7) Os(6) C(18) 90.1(9) ? ? ? yes C(15) Os(6) C(16) 87(1) ? ? ? yes C(15) Os(6) C(17) 92(1) ? ? ? yes C(15) Os(6) C(18) 172(1) ? ? ? yes C(16) Os(6) C(17) 99(1) ? ? ? yes C(16) Os(6) C(18) 90(1) ? ? ? yes C(17) Os(6) C(18) 94(1) ? ? ? yes Os(5) Os(7) Os(6) 57.09(3) ? ? ? yes Os(5) Os(7) C(19) 87.5(7) ? ? ? yes Os(5) Os(7) C(20) 143.2(8) ? ? ? yes Os(5) Os(7) C(21) 88.2(7) ? ? ? yes Os(5) Os(7) C(22) 118.9(8) ? ? ? yes Os(6) Os(7) C(19) 90.8(9) ? ? ? yes Os(6) Os(7) C(20) 86.1(8) ? ? ? yes Os(6) Os(7) C(21) 88.0(9) ? ? ? yes Os(6) Os(7) C(22) 175.0(8) ? ? ? yes C(19) Os(7) C(20) 91(1) ? ? ? yes C(19) Os(7) C(21) 175(1) ? ? ? yes C(19) Os(7) C(22) 92(1) ? ? ? yes C(20) Os(7) C(21) 93(1) ? ? ? yes C(20) Os(7) C(22) 97(1) ? ? ? yes C(21) Os(7) C(22) 88(1) ? ? ? yes Os(1) N(1) Os(2) 83.3(6) ? ? ? yes Os(1) C(1) O(1) 173(2) ? ? ? yes Os(1) C(2) O(2) 175(2) ? ? ? yes Os(1) C(3) O(3) 178(2) ? ? ? yes Os(2) C(4) O(4) 179(2) ? ? ? yes Os(2) C(5) O(5) 174(2) ? ? ? yes Os(3) C(6) O(6) 172(2) ? ? ? yes Os(3) C(7) O(7) 175(2) ? ? ? yes Os(3) C(8) O(8) 176(3) ? ? ? yes Os(4) C(9) O(9) 177(2) ? ? ? yes Os(4) C(10) O(10) 176(2) ? ? ? yes Os(4) C(11) O(11) 176(3) ? ? ? yes Os(5) C(12) O(12) 178(2) ? ? ? yes Os(5) C(13) O(13) 179(2) ? ? ? yes Os(5) C(14) O(14) 174(2) ? ? ? yes Os(6) C(15) O(15) 177(2) ? ? ? yes Os(6) C(16) O(16) 172(2) ? ? ? yes Os(6) C(17) O(17) 174(3) ? ? ? yes Os(6) C(18) O(18) 173(2) ? ? ? yes Os(7) C(19) O(19) 172(2) ? ? ? yes Os(7) C(20) O(20) 176(2) ? ? ? yes Os(7) C(21) O(21) 178(2) ? ? ? yes Os(7) C(22) O(22) 170(2) ? ? ? yes Cl(1) C(23) Cl(2) 110(1) ? ? ? yes Os(2) Os(1) H(2) 94.41 ? ? ? yes Os(3) Os(1) H(2) 37.95 ? ? ? yes Os(4) Os(1) H(2) 89.63 ? ? ? yes N(1) Os(1) H(2) 92.68 ? ? ? yes C(1) Os(1) H(2) 80.83 ? ? ? yes C(2) Os(1) H(2) 172.73 ? ? ? yes C(3) Os(1) H(2) 82.53 ? ? ? yes Os(1) Os(2) H(1) 92.91 ? ? ? yes Os(3) Os(2) H(1) 36.87 ? ? ? yes Os(4) Os(2) H(1) 89.18 ? ? ? yes Os(5) Os(2) H(1) 75.45 ? ? ? yes N(1) Os(2) H(1) 90.85 ? ? ? yes C(4) Os(2) H(1) 165.21 ? ? ? yes C(5) Os(2) H(1) 82.56 ? ? ? yes Os(1) Os(3) H(1) 90.04 ? ? ? yes Os(1) Os(3) H(2) 38.33 ? ? ? yes Os(2) Os(3) H(1) 39.60 ? ? ? yes Os(2) Os(3) H(2) 89.75 ? ? ? yes Os(4) Os(3) H(1) 89.77 ? ? ? yes Os(4) Os(3) H(2) 93.52 ? ? ? yes C(6) Os(3) H(1) 82.23 ? ? ? yes C(6) Os(3) H(2) 83.26 ? ? ? yes C(7) Os(3) H(1) 82.00 ? ? ? yes C(7) Os(3) H(2) 167.54 ? ? ? yes C(8) Os(3) H(1) 172.74 ? ? ? yes C(8) Os(3) H(2) 76.68 ? ? ? yes H(1) Os(3) H(2) 110.46 ? ? ? yes Os(2) Os(5) H(3) 73.50 ? ? ? yes Os(6) Os(5) H(3) 97.13 ? ? ? yes Os(7) Os(5) H(3) 38.00 ? ? ? yes C(12) Os(5) H(3) 162.04 ? ? ? yes C(13) Os(5) H(3) 93.56 ? ? ? yes C(14) Os(5) H(3) 87.05 ? ? ? yes Os(5) Os(7) H(3) 38.49 ? ? ? yes Os(6) Os(7) H(3) 95.58 ? ? ? yes C(19) Os(7) H(3) 86.10 ? ? ? yes C(20) Os(7) H(3) 176.81 ? ? ? yes C(21) Os(7) H(3) 89.61 ? ? ? yes C(22) Os(7) H(3) 80.48 ? ? ? yes Os(1) N(1) H(4) 115.56 ? ? ? yes Os(1) N(1) H(5) 115.56 ? ? ? yes Os(2) N(1) H(4) 115.56 ? ? ? yes Os(2) N(1) H(5) 115.56 ? ? ? yes H(4) N(1) H(5) 109.46 ? ? ? yes Cl(1) C(23) H(6) 109.22 ? ? ? yes Cl(1) C(23) H(7) 109.36 ? ? ? yes Cl(2) C(23) H(6) 109.22 ? ? ? yes Cl(2) C(23) H(7) 109.39 ? ? ? yes H(6) C(23) H(7) 109.54 ? ? ? yes #------------------------------------------------------------------------------ data_wt0219wYat036_compound_4a _database_code_CSD 192361 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Aug 4 15:24:34 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'teXsan (MSC, 1992)' _computing_publication_material 'teXsan (MSC, 1992)' #------------------------------------------------------------------------------ _cell_length_a 17.842(1) _cell_length_b 15.729(1) _cell_length_c 15.101(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4237.9(5) _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 n ' _symmetry_Int_Tables_number 60 _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2-y,1/2+z' '1/2+x,1/2-y, -z' ' -x, +y,1/2-z' ' -x, -y, -z' '1/2+x,1/2+y,1/2-z' '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.022 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.014 _exptl_crystal_density_diffrn 3.664 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 1168.87 _chemical_formula_analytical ? _chemical_formula_sum 'C11 H6 Br N O11 Os4 ' _chemical_formula_moiety 'C11 H6 Br N O11 Os4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4048.00 _exptl_absorpt_coefficient_mu 25.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.71 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 26281 _reflns_number_total 5335 _reflns_number_gt 3881 _reflns_threshold_expression 'I>\1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 28 _diffrn_measured_fraction_theta_full 28 _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 32 -1.216 7.603 'International Tables' Br 0 8 -0.290 2.459 'International Tables' O 0 88 0.011 0.006 'International Tables' C 0 88 0.003 0.002 'International Tables' N 0 8 0.006 0.003 'International Tables' H 0 48 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) 0.38460(3) 0.15648(3) 0.60431(4) 0.0271(1) Uij ? ? Os(2) 0.24974(3) 0.17174(3) 0.50940(3) 0.0242(1) Uij ? ? Os(3) 0.26937(3) 0.03304(3) 0.63789(4) 0.0241(1) Uij ? ? Os(4) 0.13817(3) 0.16229(3) 0.65718(4) 0.0239(1) Uij ? ? Br(1) 0.19559(10) 0.28291(9) 0.7479(1) 0.0393(4) Uij ? ? O(1) 0.3886(7) 0.2025(8) 0.8004(8) 0.058(4) Uij ? ? O(2) 0.5099(9) 0.0271(9) 0.621(1) 0.089(6) Uij ? ? O(3) 0.4851(8) 0.3060(8) 0.5562(10) 0.072(5) Uij ? ? O(4) 0.2646(9) 0.3490(8) 0.4334(8) 0.070(5) Uij ? ? O(5) 0.1535(7) 0.1067(9) 0.3584(8) 0.063(4) Uij ? ? O(6) 0.1461(7) -0.1067(7) 0.6498(9) 0.058(4) Uij ? ? O(7) 0.3288(8) 0.0029(8) 0.8248(8) 0.062(4) Uij ? ? O(8) 0.3797(7) -0.0849(8) 0.5488(10) 0.061(4) Uij ? ? O(9) 0.0663(7) 0.0326(8) 0.5356(10) 0.070(5) Uij ? ? O(10) 0.0067(7) 0.2799(8) 0.6356(9) 0.059(4) Uij ? ? O(11) 0.0795(8) 0.0888(9) 0.8288(9) 0.068(5) Uij ? ? N(1) 0.3551(7) 0.1332(7) 0.4692(7) 0.029(3) Uij ? ? C(1) 0.3866(9) 0.1854(10) 0.7270(9) 0.033(4) Uij ? ? C(2) 0.4595(10) 0.0739(10) 0.616(1) 0.047(5) Uij ? ? C(3) 0.4489(9) 0.254(1) 0.570(1) 0.041(5) Uij ? ? C(4) 0.2562(9) 0.2825(10) 0.4600(9) 0.037(4) Uij ? ? C(5) 0.1862(9) 0.134(1) 0.414(1) 0.042(5) Uij ? ? C(6) 0.1910(9) -0.0529(10) 0.646(1) 0.044(5) Uij ? ? C(7) 0.3085(9) 0.0126(9) 0.753(1) 0.041(4) Uij ? ? C(8) 0.3401(9) -0.0390(9) 0.584(1) 0.036(4) Uij ? ? C(9) 0.0923(8) 0.081(1) 0.584(1) 0.038(4) Uij ? ? C(10) 0.0575(8) 0.2354(9) 0.641(1) 0.034(4) Uij ? ? C(11) 0.0994(9) 0.1160(10) 0.765(1) 0.037(4) Uij ? ? H(1) 0.2379 0.0525 0.5252 0.0434 Uij ? ? H(2) 0.1946 0.1013 0.7147 0.0434 Uij ? ? H(3) 0.1797 0.2121 0.5730 0.0434 Uij ? ? H(4) 0.2994 0.2162 0.5866 0.0434 Uij ? ? H(5) 0.3770 0.1650 0.4300 0.0348 Uij ? ? H(6) 0.3588 0.0806 0.4515 0.0348 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) 0.0246(3) 0.0222(3) 0.0345(3) -0.0032(2) -0.0002(2) -0.0032(2) Os(2) 0.0302(3) 0.0200(3) 0.0223(3) -0.0009(2) -0.0009(2) 0.0006(2) Os(3) 0.0271(3) 0.0145(2) 0.0308(3) -0.0011(2) -0.0033(2) 0.0016(2) Os(4) 0.0217(3) 0.0206(3) 0.0294(3) -0.0006(2) -0.0014(2) 0.0011(2) Br(1) 0.0504(10) 0.0288(7) 0.0386(8) -0.0030(7) -0.0054(7) -0.0071(7) O(1) 0.063(9) 0.060(8) 0.053(8) -0.002(7) -0.015(7) -0.017(7) O(2) 0.066(10) 0.062(9) 0.14(1) 0.021(8) -0.04(1) -0.011(10) O(3) 0.074(10) 0.048(8) 0.10(1) -0.040(7) 0.028(8) 0.007(8) O(4) 0.14(1) 0.027(7) 0.046(7) 0.001(8) 0.008(8) 0.014(6) O(5) 0.062(9) 0.078(10) 0.048(7) -0.020(7) -0.019(7) -0.007(7) O(6) 0.059(8) 0.027(6) 0.088(10) -0.019(6) -0.009(7) 0.009(6) O(7) 0.081(9) 0.043(7) 0.062(8) -0.015(7) -0.037(7) 0.016(6) O(8) 0.040(7) 0.051(8) 0.090(10) 0.000(6) 0.006(7) -0.014(7) O(9) 0.034(7) 0.066(9) 0.11(1) -0.012(6) -0.025(8) -0.031(8) O(10) 0.043(7) 0.067(9) 0.068(8) 0.017(7) -0.007(7) 0.000(7) O(11) 0.060(9) 0.075(10) 0.070(9) -0.001(8) 0.029(7) 0.027(8) N(1) 0.034(7) 0.033(7) 0.021(6) 0.001(5) 0.009(5) -0.009(5) C(1) 0.039(9) 0.033(8) 0.027(8) -0.002(7) -0.006(6) -0.012(6) C(2) 0.042(10) 0.030(9) 0.07(1) 0.013(8) -0.003(9) -0.011(8) C(3) 0.035(8) 0.041(10) 0.048(10) -0.004(8) 0.007(7) -0.008(8) C(4) 0.06(1) 0.031(8) 0.022(7) 0.005(8) 0.006(7) 0.000(6) C(5) 0.05(1) 0.05(1) 0.029(8) -0.013(8) 0.002(7) 0.014(8) C(6) 0.029(8) 0.027(8) 0.07(1) 0.010(7) -0.005(8) 0.007(8) C(7) 0.038(9) 0.024(8) 0.06(1) -0.003(7) -0.019(8) 0.014(8) C(8) 0.036(9) 0.018(7) 0.055(10) 0.004(6) -0.001(7) -0.001(7) C(9) 0.027(8) 0.038(9) 0.048(10) 0.001(7) -0.006(7) -0.001(7) C(10) 0.028(7) 0.032(8) 0.042(8) 0.001(7) -0.001(7) 0.013(7) C(11) 0.030(8) 0.035(9) 0.048(10) -0.002(7) 0.005(7) 0.009(7) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were refined anisotropically. All hydrogen atoms were located from difference fourier map and potential energy calculations but were not refined. Hydrogens attached to organic moieties were refined as riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3881 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0506 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.560 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean ? _refine_diff_density_min -1.89 _refine_diff_density_max 1.87 #------------------------------------------------------------------------------ _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) 2.8109(8) ? ? yes Os(1) Os(3) 2.8728(7) ? ? yes Os(1) N(1) 2.14(1) ? ? yes Os(1) C(1) 1.91(1) ? ? yes Os(1) C(2) 1.87(2) ? ? yes Os(1) C(3) 1.99(2) ? ? yes Os(2) Os(3) 2.9407(7) ? ? yes Os(2) Os(4) 2.9942(7) ? ? yes Os(2) N(1) 2.07(1) ? ? yes Os(2) C(4) 1.90(2) ? ? yes Os(2) C(5) 1.92(2) ? ? yes Os(3) Os(4) 3.1141(7) ? ? yes Os(3) C(6) 1.95(2) ? ? yes Os(3) C(7) 1.90(2) ? ? yes Os(3) C(8) 1.88(2) ? ? yes Os(4) Br(1) 2.555(2) ? ? yes Os(4) C(9) 1.87(2) ? ? yes Os(4) C(10) 1.86(1) ? ? yes Os(4) C(11) 1.91(2) ? ? yes O(1) C(1) 1.14(2) ? ? yes O(2) C(2) 1.17(2) ? ? yes O(3) C(3) 1.06(2) ? ? yes O(4) C(4) 1.13(2) ? ? yes O(5) C(5) 1.11(2) ? ? yes O(6) C(6) 1.17(2) ? ? yes O(7) C(7) 1.15(2) ? ? yes O(8) C(8) 1.14(2) ? ? yes O(9) C(9) 1.16(2) ? ? yes O(10) C(10) 1.15(2) ? ? yes O(11) C(11) 1.11(2) ? ? yes Os(1) H(4) 1.807 ? ? yes Os(2) H(1) 1.903 ? ? yes Os(2) H(3) 1.699 ? ? yes Os(2) H(4) 1.622 ? ? yes Os(3) H(1) 1.818 ? ? yes Os(3) H(2) 2.068 ? ? yes Os(4) H(2) 1.640 ? ? yes Os(4) H(3) 1.667 ? ? yes N(1) H(5) 0.868 ? ? yes N(1) H(6) 0.871 ? ? 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) 62.30(2) ? ? ? yes Os(2) Os(1) N(1) 47.0(3) ? ? ? yes Os(2) Os(1) C(1) 119.4(5) ? ? ? yes Os(2) Os(1) C(2) 136.0(5) ? ? ? yes Os(2) Os(1) C(3) 107.3(5) ? ? ? yes Os(3) Os(1) N(1) 82.9(3) ? ? ? yes Os(3) Os(1) C(1) 90.2(5) ? ? ? yes Os(3) Os(1) C(2) 91.4(5) ? ? ? yes Os(3) Os(1) C(3) 169.2(5) ? ? ? yes N(1) Os(1) C(1) 166.4(5) ? ? ? yes N(1) Os(1) C(2) 98.5(6) ? ? ? yes N(1) Os(1) C(3) 91.7(6) ? ? ? yes C(1) Os(1) C(2) 93.4(7) ? ? ? yes C(1) Os(1) C(3) 93.2(7) ? ? ? yes C(2) Os(1) C(3) 98.6(7) ? ? ? yes Os(1) Os(2) Os(3) 59.88(2) ? ? ? yes Os(1) Os(2) Os(4) 100.65(2) ? ? ? yes Os(1) Os(2) N(1) 49.2(3) ? ? ? yes Os(1) Os(2) C(4) 103.1(5) ? ? ? yes Os(1) Os(2) C(5) 149.3(5) ? ? ? yes Os(3) Os(2) Os(4) 63.29(2) ? ? ? yes Os(3) Os(2) N(1) 82.4(3) ? ? ? yes Os(3) Os(2) C(4) 158.9(5) ? ? ? yes Os(3) Os(2) C(5) 109.7(5) ? ? ? yes Os(4) Os(2) N(1) 144.0(3) ? ? ? yes Os(4) Os(2) C(4) 112.3(4) ? ? ? yes Os(4) Os(2) C(5) 98.6(5) ? ? ? yes N(1) Os(2) C(4) 95.7(6) ? ? ? yes N(1) Os(2) C(5) 103.1(6) ? ? ? yes C(4) Os(2) C(5) 91.3(7) ? ? ? yes Os(1) Os(3) Os(2) 57.82(2) ? ? ? yes Os(1) Os(3) Os(4) 96.50(2) ? ? ? yes Os(1) Os(3) C(6) 173.4(5) ? ? ? yes Os(1) Os(3) C(7) 90.7(5) ? ? ? yes Os(1) Os(3) C(8) 81.4(5) ? ? ? yes Os(2) Os(3) Os(4) 59.19(2) ? ? ? yes Os(2) Os(3) C(6) 118.0(5) ? ? ? yes Os(2) Os(3) C(7) 140.6(4) ? ? ? yes Os(2) Os(3) C(8) 104.0(5) ? ? ? yes Os(4) Os(3) C(6) 84.7(4) ? ? ? yes Os(4) Os(3) C(7) 107.5(5) ? ? ? yes Os(4) Os(3) C(8) 159.8(5) ? ? ? yes C(6) Os(3) C(7) 95.1(7) ? ? ? yes C(6) Os(3) C(8) 95.2(7) ? ? ? yes C(7) Os(3) C(8) 92.7(7) ? ? ? yes Os(2) Os(4) Os(3) 57.52(2) ? ? ? yes Os(2) Os(4) Br(1) 95.53(4) ? ? ? yes Os(2) Os(4) C(9) 83.3(5) ? ? ? yes Os(2) Os(4) C(10) 112.8(5) ? ? ? yes Os(2) Os(4) C(11) 153.3(5) ? ? ? yes Os(3) Os(4) Br(1) 103.50(4) ? ? ? yes Os(3) Os(4) C(9) 80.2(5) ? ? ? yes Os(3) Os(4) C(10) 166.9(5) ? ? ? yes Os(3) Os(4) C(11) 95.9(5) ? ? ? yes Br(1) Os(4) C(9) 174.8(5) ? ? ? yes Br(1) Os(4) C(10) 85.5(5) ? ? ? yes Br(1) Os(4) C(11) 88.4(5) ? ? ? yes C(9) Os(4) C(10) 90.3(7) ? ? ? yes C(9) Os(4) C(11) 94.9(7) ? ? ? yes C(10) Os(4) C(11) 93.8(6) ? ? ? yes Os(1) N(1) Os(2) 83.9(4) ? ? ? yes Os(1) C(1) O(1) 179(1) ? ? ? yes Os(1) C(2) O(2) 174(1) ? ? ? yes Os(1) C(3) O(3) 176(1) ? ? ? yes Os(2) C(4) O(4) 175(1) ? ? ? yes Os(2) C(5) O(5) 173(1) ? ? ? yes Os(3) C(6) O(6) 177(1) ? ? ? yes Os(3) C(7) O(7) 176(1) ? ? ? yes Os(3) C(8) O(8) 175(1) ? ? ? yes Os(4) C(9) O(9) 176(1) ? ? ? yes Os(4) C(10) O(10) 176(1) ? ? ? yes Os(4) C(11) O(11) 177(1) ? ? ? yes Os(2) Os(1) H(4) 32.84 ? ? ? yes Os(3) Os(1) H(4) 77.02 ? ? ? yes N(1) Os(1) H(4) 74.98 ? ? ? yes C(1) Os(1) H(4) 92.06 ? ? ? yes C(2) Os(1) H(4) 167.26 ? ? ? yes C(3) Os(1) H(4) 92.62 ? ? ? yes Os(1) Os(2) H(1) 86.96 ? ? ? yes Os(1) Os(2) H(3) 111.93 ? ? ? yes Os(1) Os(2) H(4) 37.16 ? ? ? yes Os(3) Os(2) H(1) 36.78 ? ? ? yes Os(3) Os(2) H(3) 89.52 ? ? ? yes Os(3) Os(2) H(4) 77.33 ? ? ? yes Os(4) Os(2) H(1) 77.51 ? ? ? yes Os(4) Os(2) H(3) 26.89 ? ? ? yes Os(4) Os(2) H(4) 81.32 ? ? ? yes N(1) Os(2) H(1) 81.28 ? ? ? yes N(1) Os(2) H(3) 160.89 ? ? ? yes N(1) Os(2) H(4) 80.84 ? ? ? yes C(4) Os(2) H(1) 163.88 ? ? ? yes C(4) Os(2) H(3) 85.65 ? ? ? yes C(4) Os(2) H(4) 81.57 ? ? ? yes C(5) Os(2) H(1) 74.12 ? ? ? yes C(5) Os(2) H(3) 95.93 ? ? ? yes C(5) Os(2) H(4) 172.25 ? ? ? yes H(1) Os(2) H(3) 102.43 ? ? ? yes H(1) Os(2) H(4) 113.29 ? ? ? yes H(3) Os(2) H(4) 80.50 ? ? ? yes Os(1) Os(3) H(1) 86.68 ? ? ? yes Os(1) Os(3) H(2) 102.11 ? ? ? yes Os(2) Os(3) H(1) 38.80 ? ? ? yes Os(2) Os(3) H(2) 84.73 ? ? ? yes Os(4) Os(3) H(1) 75.26 ? ? ? yes Os(4) Os(3) H(2) 28.82 ? ? ? yes C(6) Os(3) H(1) 87.32 ? ? ? yes C(6) Os(3) H(2) 82.10 ? ? ? yes C(7) Os(3) H(1) 176.45 ? ? ? yes C(7) Os(3) H(2) 79.12 ? ? ? yes C(8) Os(3) H(1) 84.51 ? ? ? yes C(8) Os(3) H(2) 171.07 ? ? ? yes H(1) Os(3) H(2) 103.80 ? ? ? yes Os(2) Os(4) H(2) 90.90 ? ? ? yes Os(2) Os(4) H(3) 27.46 ? ? ? yes Os(3) Os(4) H(2) 37.45 ? ? ? yes Os(3) Os(4) H(3) 84.33 ? ? ? yes Br(1) Os(4) H(2) 84.49 ? ? ? yes Br(1) Os(4) H(3) 83.23 ? ? ? yes C(9) Os(4) H(2) 100.59 ? ? ? yes C(9) Os(4) H(3) 93.58 ? ? ? yes C(10) Os(4) H(2) 155.08 ? ? ? yes C(10) Os(4) H(3) 87.35 ? ? ? yes C(11) Os(4) H(2) 63.14 ? ? ? yes C(11) Os(4) H(3) 171.38 ? ? ? yes H(2) Os(4) H(3) 113.96 ? ? ? yes Os(1) N(1) H(5) 116.14 ? ? ? yes Os(1) N(1) H(6) 115.94 ? ? ? yes Os(2) N(1) H(5) 116.13 ? ? ? yes Os(2) N(1) H(6) 115.92 ? ? ? yes H(5) N(1) H(6) 107.71 ? ? ? yes #------------------------------------------------------------------------------ data_wt0390w_Yat080_compound_4b _database_code_CSD 192362 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Oct 13 16:22:22 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SIR88 (Burla, 1989)' _computing_structure_refinement 'teXsan (MSC, 1992)' _computing_publication_material 'teXsan (MSC, 1992)' #------------------------------------------------------------------------------ _cell_length_a 8.5990(8) _cell_length_b 9.6870(8) _cell_length_c 14.047(1) _cell_angle_alpha 91.88(1) _cell_angle_beta 102.76(1) _cell_angle_gamma 113.96(1) _cell_volume 1033.0(2) _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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.070 _exptl_crystal_density_diffrn 3.758 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 1168.87 _chemical_formula_analytical ? _chemical_formula_sum 'C11 H6 Br N O11 Os4 ' _chemical_formula_moiety 'C11 H6 Br N O11 Os4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1012.00 _exptl_absorpt_coefficient_mu 26.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.073 _exptl_absorpt_correction_T_max 0.160 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 6315 _reflns_number_total 4444 _reflns_number_gt 3673 _reflns_threshold_expression 'I>\1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27 _diffrn_reflns_theta_full 27 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 27 _diffrn_measured_fraction_theta_full 27 _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 8 -1.216 7.603 'International Tables' N 0 2 0.006 0.003 'International Tables' C 0 22 0.003 0.002 'International Tables' O 0 22 0.011 0.006 'International Tables' H 0 12 0.000 0.000 'International Tables' Br 0 2 -0.290 2.459 '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) -0.07738(8) 0.23342(7) 0.64229(4) 0.0290(2) Uij ? ? Os(2) 0.14433(7) 0.13929(6) 0.77746(4) 0.0271(2) Uij ? ? Os(3) -0.09530(7) 0.23640(7) 0.85666(4) 0.0279(2) Uij ? ? Os(4) 0.26976(7) 0.47980(6) 0.77113(4) 0.0269(2) Uij ? ? Br(1) -0.2909(2) 0.3723(2) 0.8666(2) 0.0517(6) Uij ? ? O(1) -0.271(2) 0.391(2) 0.520(1) 0.087(5) Uij ? ? O(2) 0.081(2) 0.184(2) 0.479(1) 0.069(4) Uij ? ? O(3) -0.394(2) -0.079(2) 0.585(1) 0.067(4) Uij ? ? O(4) 0.338(2) 0.090(2) 0.632(1) 0.064(4) Uij ? ? O(5) -0.135(2) -0.193(1) 0.725(1) 0.057(3) Uij ? ? O(6) 0.375(2) 0.063(2) 0.9455(10) 0.060(4) Uij ? ? O(7) -0.028(2) 0.229(2) 1.0720(3) 0.071(5) Uij ? ? O(8) -0.393(2) -0.082(1) 0.823(1) 0.076(4) Uij ? ? O(9) 0.597(1) 0.646(2) 0.938(1) 0.058(3) Uij ? ? O(10) 0.238(2) 0.768(2) 0.710(1) 0.064(4) Uij ? ? O(11) 0.484(2) 0.470(2) 0.625(1) 0.066(5) Uij ? ? N(1) 0.112(1) 0.462(1) 0.8722(9) 0.030(3) Uij ? ? C(1) -0.199(2) 0.329(2) 0.566(1) 0.042(4) Uij ? ? C(2) 0.023(2) 0.197(2) 0.541(1) 0.046(5) Uij ? ? C(3) -0.269(2) 0.038(2) 0.607(1) 0.038(4) Uij ? ? C(4) 0.267(2) 0.115(3) 0.687(1) 0.057(6) Uij ? ? C(5) -0.036(2) -0.068(2) 0.740(1) 0.035(3) Uij ? ? C(6) 0.291(2) 0.092(2) 0.884(1) 0.028(3) Uij ? ? C(7) -0.055(2) 0.230(2) 0.9984(7) 0.029(3) Uij ? ? C(8) -0.279(2) 0.038(2) 0.835(1) 0.040(4) Uij ? ? C(9) 0.473(2) 0.583(2) 0.873(1) 0.038(4) Uij ? ? C(10) 0.246(2) 0.657(2) 0.734(1) 0.050(4) Uij ? ? C(11) 0.410(2) 0.482(2) 0.678(1) 0.048(4) Uij ? ? H(1) 0.0669 0.5244 0.8620 0.0357 Uij ? ? H(2) 0.1770 0.4842 0.9299 0.0357 Uij ? ? H(3) -0.2289 0.1986 0.7374 0.0608 Uij ? ? H(4) -0.0099 0.1066 0.8702 0.0608 Uij ? ? H(5) 0.1307 0.4378 0.6536 0.0608 Uij ? ? H(6) 0.3497 0.3458 0.7864 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) 0.0379(3) 0.0318(3) 0.0202(3) 0.0194(3) 0.0037(2) 0.0030(2) Os(2) 0.0379(3) 0.0235(3) 0.0248(3) 0.0183(2) 0.0071(2) 0.0042(2) Os(3) 0.0324(3) 0.0265(3) 0.0256(3) 0.0120(2) 0.0092(2) 0.0035(2) Os(4) 0.0315(3) 0.0235(3) 0.0293(3) 0.0146(2) 0.0084(2) 0.0065(2) Br(1) 0.0505(10) 0.059(1) 0.057(1) 0.0327(9) 0.0157(9) 0.0026(10) O(3) 0.070(8) 0.033(6) 0.07(1) 0.002(3) -0.006(8) -0.009(7) O(5) 0.058(8) 0.032(4) 0.046(8) -0.006(4) -0.006(6) -0.002(6) O(6) 0.061(8) 0.070(9) 0.044(8) 0.036(7) -0.018(6) 0.029(7) O(7) 0.056(8) 0.046(8) 0.09(1) 0.017(7) -0.015(8) -0.022(9) O(8) 0.10(1) 0.027(6) 0.06(1) -0.023(4) 0.030(9) 0.000(6) O(9) 0.034(6) 0.082(10) 0.051(5) 0.033(6) -0.016(3) -0.017(3) O(11) 0.067(9) 0.09(1) 0.066(10) 0.058(9) 0.027(8) 0.013(9) N(1) 0.023(5) 0.033(4) 0.025(6) 0.008(3) -0.002(4) 0.011(6) C(2) 0.06(1) 0.09(1) 0.010(7) 0.05(1) 0.007(6) 0.007(8) C(3) 0.054(8) 0.029(6) 0.031(9) 0.013(3) 0.017(7) 0.007(6) C(4) 0.029(8) 0.13(2) 0.023(8) 0.03(1) 0.018(7) 0.03(1) C(5) 0.063(9) 0.019(4) 0.020(8) 0.022(3) -0.006(7) 0.001(6) C(6) 0.031(7) 0.023(7) 0.032(6) 0.018(6) 0.000(5) -0.007(6) C(8) 0.042(8) 0.031(6) 0.032(9) 0.000(4) 0.011(7) -0.008(7) C(9) 0.021(6) 0.038(9) 0.048(9) 0.012(6) -0.001(4) -0.002(7) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were attempted to be refined anisotropically, but some atoms [namely: C(1), C(7), C(10) C(11), O(1), O(2), O(4) and O(10)] were found unsuitable to be refined anisotropically, thus refined isotropic only. All hydride atoms were located from difference fourier map and potential energy calculations but were not refined. Hydrogens attached to organic moieties were refined as riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3673 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0942 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.577 _refine_ls_shift/su_max 0.0261 _refine_ls_shift/su_mean ? _refine_diff_density_min -4.39 _refine_diff_density_max 4.74 #------------------------------------------------------------------------------ _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) 2.828(1) ? ? yes Os(1) Os(3) 3.049(1) ? ? yes Os(1) Os(4) 3.070(1) ? ? yes Os(1) C(1) 1.86(3) ? ? yes Os(1) C(2) 1.91(2) ? ? yes Os(1) C(3) 1.89(3) ? ? yes Os(2) Os(3) 2.981(1) ? ? yes Os(2) Os(4) 3.037(1) ? ? yes Os(2) C(4) 1.88(3) ? ? yes Os(2) C(5) 1.94(3) ? ? yes Os(2) C(6) 1.93(2) ? ? yes Os(3) Br(1) 2.544(3) ? ? yes Os(3) N(1) 2.15(2) ? ? yes Os(3) C(7) 1.95(1) ? ? yes Os(3) C(8) 1.89(3) ? ? yes Os(4) N(1) 2.13(2) ? ? yes Os(4) C(9) 1.87(3) ? ? yes Os(4) C(10) 1.88(3) ? ? yes Os(4) C(11) 1.96(3) ? ? yes O(1) C(1) 1.15(4) ? ? yes O(2) C(2) 1.12(3) ? ? yes O(3) C(3) 1.17(3) ? ? yes O(4) C(4) 1.16(3) ? ? yes O(5) C(5) 1.14(3) ? ? yes O(6) C(6) 1.13(3) ? ? yes O(7) C(7) 1.01(1) ? ? yes O(8) C(8) 1.15(3) ? ? yes O(9) C(9) 1.16(3) ? ? yes O(10) C(10) 1.16(3) ? ? yes O(11) C(11) 1.12(3) ? ? yes Os(1) H(3) 2.010 ? ? yes Os(1) H(5) 2.031 ? ? yes Os(2) H(4) 2.001 ? ? yes Os(2) H(6) 2.038 ? ? yes Os(3) H(3) 1.741 ? ? yes Os(3) H(4) 1.691 ? ? yes Os(4) H(5) 1.735 ? ? yes Os(4) H(6) 1.697 ? ? yes N(1) H(1) 0.840 ? ? yes N(1) H(2) 0.840 ? ? 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(3) ? ? ? yes Os(2) Os(1) Os(4) 61.82(3) ? ? ? yes Os(2) Os(1) C(1) 170.0(9) ? ? ? yes Os(2) Os(1) C(2) 89.1(7) ? ? ? yes Os(2) Os(1) C(3) 95.4(8) ? ? ? yes Os(3) Os(1) Os(4) 71.23(3) ? ? ? yes Os(3) Os(1) C(1) 115.3(9) ? ? ? yes Os(3) Os(1) C(2) 149.9(7) ? ? ? yes Os(3) Os(1) C(3) 91.1(8) ? ? ? yes Os(4) Os(1) C(1) 108.5(9) ? ? ? yes Os(4) Os(1) C(2) 95.1(9) ? ? ? yes Os(4) Os(1) C(3) 155.8(8) ? ? ? yes C(1) Os(1) C(2) 94(1) ? ? ? yes C(1) Os(1) C(3) 93(1) ? ? ? yes C(2) Os(1) C(3) 92(1) ? ? ? yes Os(1) Os(2) Os(3) 63.25(3) ? ? ? yes Os(1) Os(2) Os(4) 63.01(3) ? ? ? yes Os(1) Os(2) C(4) 95.1(8) ? ? ? yes Os(1) Os(2) C(5) 88.4(7) ? ? ? yes Os(1) Os(2) C(6) 171.9(6) ? ? ? yes Os(3) Os(2) Os(4) 72.61(3) ? ? ? yes Os(3) Os(2) C(4) 157.8(9) ? ? ? yes Os(3) Os(2) C(5) 91.5(8) ? ? ? yes Os(3) Os(2) C(6) 109.3(7) ? ? ? yes Os(4) Os(2) C(4) 93(1) ? ? ? yes Os(4) Os(2) C(5) 151.1(7) ? ? ? yes Os(4) Os(2) C(6) 112.7(7) ? ? ? yes C(4) Os(2) C(5) 92(1) ? ? ? yes C(4) Os(2) C(6) 92(1) ? ? ? yes C(5) Os(2) C(6) 95.1(10) ? ? ? yes Os(1) Os(3) Os(2) 55.93(3) ? ? ? yes Os(1) Os(3) Br(1) 103.53(9) ? ? ? yes Os(1) Os(3) N(1) 82.7(6) ? ? ? yes Os(1) Os(3) C(7) 166.0(6) ? ? ? yes Os(1) Os(3) C(8) 94.2(8) ? ? ? yes Os(2) Os(3) Br(1) 157.95(9) ? ? ? yes Os(2) Os(3) N(1) 84.2(5) ? ? ? yes Os(2) Os(3) C(7) 110.3(6) ? ? ? yes Os(2) Os(3) C(8) 94.5(8) ? ? ? yes Br(1) Os(3) N(1) 85.2(5) ? ? ? yes Br(1) Os(3) C(7) 89.7(7) ? ? ? yes Br(1) Os(3) C(8) 95.1(8) ? ? ? yes N(1) Os(3) C(7) 93.9(9) ? ? ? yes N(1) Os(3) C(8) 176.8(10) ? ? ? yes C(7) Os(3) C(8) 89(1) ? ? ? yes Os(1) Os(4) Os(2) 55.17(3) ? ? ? yes Os(1) Os(4) N(1) 82.5(5) ? ? ? yes Os(1) Os(4) C(9) 162.7(9) ? ? ? yes Os(1) Os(4) C(10) 100.2(9) ? ? ? yes Os(1) Os(4) C(11) 95.4(9) ? ? ? yes Os(2) Os(4) N(1) 83.1(5) ? ? ? yes Os(2) Os(4) C(9) 108.6(8) ? ? ? yes Os(2) Os(4) C(10) 155.0(9) ? ? ? yes Os(2) Os(4) C(11) 93.2(9) ? ? ? yes N(1) Os(4) C(9) 90.0(10) ? ? ? yes N(1) Os(4) C(10) 90(1) ? ? ? yes N(1) Os(4) C(11) 176(1) ? ? ? yes C(9) Os(4) C(10) 95(1) ? ? ? yes C(9) Os(4) C(11) 91(1) ? ? ? yes C(10) Os(4) C(11) 93(1) ? ? ? yes Os(3) N(1) Os(4) 112.3(9) ? ? ? yes Os(1) C(1) O(1) 178(2) ? ? ? yes Os(1) C(2) O(2) 175(2) ? ? ? yes Os(1) C(3) O(3) 176(2) ? ? ? yes Os(2) C(4) O(4) 175(3) ? ? ? yes Os(2) C(5) O(5) 174(2) ? ? ? yes Os(2) C(6) O(6) 178(2) ? ? ? yes Os(3) C(7) O(7) 177(2) ? ? ? yes Os(3) C(8) O(8) 178(2) ? ? ? yes Os(4) C(9) O(9) 178(2) ? ? ? yes Os(4) C(10) O(10) 177(2) ? ? ? yes Os(4) C(11) O(11) 174(2) ? ? ? yes Os(2) Os(1) H(3) 88.16 ? ? ? yes Os(2) Os(1) H(5) 88.99 ? ? ? yes Os(3) Os(1) H(3) 32.77 ? ? ? yes Os(3) Os(1) H(5) 99.46 ? ? ? yes Os(4) Os(1) H(3) 99.80 ? ? ? yes Os(4) Os(1) H(5) 32.30 ? ? ? yes C(1) Os(1) H(3) 91.51 ? ? ? yes C(1) Os(1) H(5) 82.58 ? ? ? yes C(2) Os(1) H(3) 161.45 ? ? ? yes C(2) Os(1) H(5) 77.94 ? ? ? yes C(3) Os(1) H(3) 69.58 ? ? ? yes C(3) Os(1) H(5) 169.37 ? ? ? yes H(3) Os(1) H(5) 120.34 ? ? ? yes Os(1) Os(2) H(4) 90.53 ? ? ? yes Os(1) Os(2) H(6) 89.71 ? ? ? yes Os(3) Os(2) H(4) 32.76 ? ? ? yes Os(3) Os(2) H(6) 100.16 ? ? ? yes Os(4) Os(2) H(4) 100.93 ? ? ? yes Os(4) Os(2) H(6) 32.01 ? ? ? yes C(4) Os(2) H(4) 165.13 ? ? ? yes C(4) Os(2) H(6) 73.49 ? ? ? yes C(5) Os(2) H(4) 73.68 ? ? ? yes C(5) Os(2) H(6) 165.84 ? ? ? yes C(6) Os(2) H(4) 83.49 ? ? ? yes C(6) Os(2) H(6) 88.59 ? ? ? yes H(4) Os(2) H(6) 120.39 ? ? ? yes Os(1) Os(3) H(3) 38.67 ? ? ? yes Os(1) Os(3) H(4) 89.74 ? ? ? yes Os(2) Os(3) H(3) 88.65 ? ? ? yes Os(2) Os(3) H(4) 39.83 ? ? ? yes Br(1) Os(3) H(3) 76.04 ? ? ? yes Br(1) Os(3) H(4) 161.07 ? ? ? yes N(1) Os(3) H(3) 106.92 ? ? ? yes N(1) Os(3) H(4) 110.15 ? ? ? yes C(7) Os(3) H(3) 153.36 ? ? ? yes C(7) Os(3) H(4) 78.65 ? ? ? yes C(8) Os(3) H(3) 70.16 ? ? ? yes C(8) Os(3) H(4) 70.17 ? ? ? yes H(3) Os(3) H(4) 108.34 ? ? ? yes Os(1) Os(4) H(5) 38.71 ? ? ? yes Os(1) Os(4) H(6) 88.83 ? ? ? yes Os(2) Os(4) H(5) 88.29 ? ? ? yes Os(2) Os(4) H(6) 39.53 ? ? ? yes N(1) Os(4) H(5) 106.78 ? ? ? yes N(1) Os(4) H(6) 108.72 ? ? ? yes C(9) Os(4) H(5) 157.78 ? ? ? yes C(9) Os(4) H(6) 78.81 ? ? ? yes C(10) Os(4) H(5) 70.63 ? ? ? yes C(10) Os(4) H(6) 160.09 ? ? ? yes C(11) Os(4) H(5) 72.98 ? ? ? yes C(11) Os(4) H(6) 68.11 ? ? ? yes H(5) Os(4) H(6) 108.30 ? ? ? yes Os(3) N(1) H(1) 108.75 ? ? ? yes Os(3) N(1) H(2) 108.75 ? ? ? yes Os(4) N(1) H(1) 108.76 ? ? ? yes Os(4) N(1) H(2) 108.76 ? ? ? yes H(1) N(1) H(2) 109.46 ? ? ? yes #------------------------------------------------------------------------------ #===End data_wt0421w_YAT087_#1_compound_5 _database_code_CSD 192363 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 27 12:47:15 2002' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1996)' _computing_cell_refinement 'SMART (Bruker, 1996)' _computing_data_reduction 'SAINT+ (Bruker, 1999)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'teXsan (MSC, 1992)' _computing_publication_material 'teXsan (MSC, 1992)' #------------------------------------------------------------------------------ _cell_length_a 13.392(1) _cell_length_b 9.7620(6) _cell_length_c 14.773(1) _cell_angle_alpha 90 _cell_angle_beta 113.96(1) _cell_angle_gamma 90 _cell_volume 1764.9(2) _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 '-P 2ybc' 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 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 3.465 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 920.64 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H4 Br N O9 Os3 ' _chemical_formula_moiety 'C9 H4 Br N O9 Os3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1600.00 _exptl_absorpt_coefficient_mu 23.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.001 _exptl_absorpt_correction_T_max 0.150 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'Bruker SMART 1K CCD Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 10910 _reflns_number_total 4229 _reflns_number_gt 3207 _reflns_threshold_expression 'I>\1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 27.5 _diffrn_measured_fraction_theta_full 27.5 _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 36 0.003 0.002 'International Tables' O 0 36 0.011 0.006 'International Tables' H 0 16 0.000 0.000 'International Tables' N 0 4 0.006 0.003 'International Tables' Br 0 4 -0.290 2.459 '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) 0.82275(4) 0.01731(5) 0.09648(3) 0.0351(1) Uij ? ? Os(2) 0.68692(4) 0.18043(5) 0.15803(4) 0.0356(1) Uij ? ? Os(3) 0.76355(4) -0.06256(5) 0.26761(4) 0.0413(1) Uij ? ? Br(1) 0.6567(1) -0.1092(2) -0.0358(1) 0.0566(4) Uij ? ? O(1) 0.965(1) -0.188(1) 0.045(1) 0.102(5) Uij ? ? O(2) 1.0144(8) 0.167(1) 0.2470(9) 0.070(3) Uij ? ? O(3) 0.8008(9) 0.227(1) -0.0614(8) 0.080(4) Uij ? ? O(4) 0.8453(9) 0.420(1) 0.197(1) 0.087(4) Uij ? ? O(5) 0.5518(9) 0.270(1) -0.0527(8) 0.073(4) Uij ? ? O(6) 0.5446(9) 0.333(1) 0.2425(9) 0.083(4) Uij ? ? O(7) 0.686(1) -0.025(1) 0.4323(10) 0.091(5) Uij ? ? O(8) 0.726(1) -0.369(1) 0.254(1) 0.105(6) Uij ? ? O(9) 0.9988(10) -0.084(1) 0.4154(8) 0.081(4) Uij ? ? N(1) 0.6143(8) -0.010(1) 0.1544(8) 0.044(3) Uij ? ? C(1) 0.915(1) -0.114(2) 0.065(1) 0.056(4) Uij ? ? C(2) 0.942(1) 0.111(1) 0.192(1) 0.045(4) Uij ? ? C(3) 0.811(1) 0.151(1) 0.001(1) 0.049(4) Uij ? ? C(4) 0.785(1) 0.332(1) 0.181(1) 0.049(4) Uij ? ? C(5) 0.605(1) 0.235(1) 0.028(1) 0.050(4) Uij ? ? C(6) 0.598(1) 0.273(2) 0.214(1) 0.052(4) Uij ? ? C(7) 0.714(1) -0.039(1) 0.373(1) 0.062(5) Uij ? ? C(8) 0.741(1) -0.257(2) 0.260(1) 0.063(5) Uij ? ? C(9) 0.914(1) -0.075(2) 0.3611(10) 0.052(4) Uij ? ? H(1) 0.5583 -0.0096 0.1711 0.0534 Uij ? ? H(2) 0.5970 -0.0567 0.0990 0.0534 Uij ? ? H(3) 0.7619 0.1511 0.2900 0.0650 Uij ? ? H(4) 0.8080 -0.1274 0.1600 0.0650 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) 0.0336(2) 0.0410(3) 0.0347(2) 0.0018(2) 0.0179(2) -0.0005(2) Os(2) 0.0346(2) 0.0348(2) 0.0397(3) 0.0003(2) 0.0175(2) -0.0043(2) Os(3) 0.0534(3) 0.0377(3) 0.0419(3) 0.0034(2) 0.0288(2) 0.0011(2) Br(1) 0.0502(8) 0.0689(9) 0.0488(8) -0.0067(7) 0.0180(6) -0.0203(7) O(1) 0.093(9) 0.11(1) 0.13(1) 0.035(8) 0.073(9) -0.018(9) O(2) 0.045(6) 0.060(6) 0.078(7) -0.009(5) -0.001(5) -0.009(6) O(3) 0.081(8) 0.101(9) 0.056(7) 0.008(7) 0.025(6) 0.032(7) O(4) 0.074(8) 0.053(7) 0.14(1) -0.019(6) 0.050(8) -0.011(7) O(5) 0.075(7) 0.085(8) 0.053(6) -0.003(6) 0.019(6) 0.012(6) O(6) 0.067(7) 0.11(1) 0.077(8) 0.033(7) 0.035(6) -0.018(7) O(7) 0.15(1) 0.079(8) 0.095(9) 0.004(8) 0.100(10) 0.003(7) O(8) 0.18(1) 0.043(7) 0.14(1) -0.009(8) 0.11(1) 0.002(7) O(9) 0.066(7) 0.11(1) 0.057(7) 0.018(7) 0.017(6) 0.014(7) N(1) 0.042(6) 0.050(6) 0.050(6) -0.006(5) 0.029(5) -0.009(5) C(1) 0.064(9) 0.059(9) 0.062(9) 0.007(7) 0.043(8) -0.004(7) C(2) 0.046(7) 0.040(7) 0.053(8) 0.012(6) 0.024(6) 0.007(6) C(3) 0.044(7) 0.060(9) 0.050(8) 0.005(6) 0.028(6) 0.006(7) C(4) 0.043(7) 0.047(8) 0.064(9) 0.003(6) 0.029(7) -0.004(7) C(5) 0.059(8) 0.052(8) 0.050(8) -0.011(7) 0.032(7) 0.006(7) C(6) 0.056(8) 0.060(9) 0.045(8) 0.006(7) 0.024(7) -0.004(7) C(7) 0.10(1) 0.046(8) 0.060(9) 0.013(8) 0.056(10) 0.005(7) C(8) 0.10(1) 0.041(8) 0.08(1) -0.004(8) 0.07(1) -0.005(7) C(9) 0.053(8) 0.072(10) 0.032(7) 0.010(7) 0.016(7) 0.006(6) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were refined anisotropically. All hydrogen atoms were located from difference fourier map and potential energy calculations but were not refined. Hydrogens attached to organic moieties were refined as riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3207 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0457 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.303 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean ? _refine_diff_density_min -1.34 _refine_diff_density_max 2.24 #------------------------------------------------------------------------------ _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) 2.8310(6) ? ? yes Os(1) Os(3) 3.0424(6) ? ? yes Os(1) Br(1) 2.600(1) ? ? yes Os(1) C(1) 1.96(1) ? ? yes Os(1) C(2) 1.89(1) ? ? yes Os(1) C(3) 1.88(1) ? ? yes Os(2) Os(3) 2.8198(7) ? ? yes Os(2) N(1) 2.09(1) ? ? yes Os(2) C(4) 1.91(1) ? ? yes Os(2) C(5) 1.87(1) ? ? yes Os(2) C(6) 1.93(1) ? ? yes Os(3) N(1) 2.08(1) ? ? yes Os(3) C(7) 1.94(1) ? ? yes Os(3) C(8) 1.92(2) ? ? yes Os(3) C(9) 1.93(1) ? ? yes O(1) C(1) 1.10(2) ? ? yes O(2) C(2) 1.12(2) ? ? yes O(3) C(3) 1.15(2) ? ? yes O(4) C(4) 1.14(2) ? ? yes O(5) C(5) 1.16(2) ? ? yes O(6) C(6) 1.13(2) ? ? yes O(7) C(7) 1.10(2) ? ? yes O(8) C(8) 1.11(2) ? ? yes O(9) C(9) 1.10(2) ? ? yes Os(1) H(4) 1.751 ? ? yes Os(2) H(3) 1.817 ? ? yes Os(3) H(3) 2.113 ? ? yes Os(3) H(4) 2.013 ? ? yes N(1) H(1) 0.880 ? ? yes N(1) H(2) 0.880 ? ? 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) 57.25(2) ? ? ? yes Os(2) Os(1) Br(1) 92.51(4) ? ? ? yes Os(2) Os(1) C(1) 172.6(4) ? ? ? yes Os(2) Os(1) C(2) 87.0(4) ? ? ? yes Os(2) Os(1) C(3) 88.9(4) ? ? ? yes Os(3) Os(1) Br(1) 94.08(4) ? ? ? yes Os(3) Os(1) C(1) 115.5(4) ? ? ? yes Os(3) Os(1) C(2) 86.0(4) ? ? ? yes Os(3) Os(1) C(3) 146.1(4) ? ? ? yes Br(1) Os(1) C(1) 86.6(5) ? ? ? yes Br(1) Os(1) C(2) 179.4(4) ? ? ? yes Br(1) Os(1) C(3) 88.9(4) ? ? ? yes C(1) Os(1) C(2) 94.0(6) ? ? ? yes C(1) Os(1) C(3) 98.3(6) ? ? ? yes C(2) Os(1) C(3) 90.7(6) ? ? ? yes Os(1) Os(2) Os(3) 65.15(2) ? ? ? yes Os(1) Os(2) N(1) 81.0(3) ? ? ? yes Os(1) Os(2) C(4) 90.3(4) ? ? ? yes Os(1) Os(2) C(5) 90.7(4) ? ? ? yes Os(1) Os(2) C(6) 172.0(4) ? ? ? yes Os(3) Os(2) N(1) 47.4(3) ? ? ? yes Os(3) Os(2) C(4) 119.0(4) ? ? ? yes Os(3) Os(2) C(5) 139.1(4) ? ? ? yes Os(3) Os(2) C(6) 106.8(4) ? ? ? yes N(1) Os(2) C(4) 166.1(5) ? ? ? yes N(1) Os(2) C(5) 98.8(5) ? ? ? yes N(1) Os(2) C(6) 93.7(5) ? ? ? yes C(4) Os(2) C(5) 92.0(6) ? ? ? yes C(4) Os(2) C(6) 93.6(6) ? ? ? yes C(5) Os(2) C(6) 96.1(6) ? ? ? yes Os(1) Os(3) Os(2) 57.60(2) ? ? ? yes Os(1) Os(3) N(1) 76.0(3) ? ? ? yes Os(1) Os(3) C(7) 157.8(4) ? ? ? yes Os(1) Os(3) C(8) 107.2(4) ? ? ? yes Os(1) Os(3) C(9) 93.6(4) ? ? ? yes Os(2) Os(3) N(1) 47.6(3) ? ? ? yes Os(2) Os(3) C(7) 101.3(4) ? ? ? yes Os(2) Os(3) C(8) 141.9(5) ? ? ? yes Os(2) Os(3) C(9) 119.7(5) ? ? ? yes N(1) Os(3) C(7) 95.0(6) ? ? ? yes N(1) Os(3) C(8) 96.7(6) ? ? ? yes N(1) Os(3) C(9) 166.7(5) ? ? ? yes C(7) Os(3) C(8) 93.9(6) ? ? ? yes C(7) Os(3) C(9) 91.6(7) ? ? ? yes C(8) Os(3) C(9) 94.3(7) ? ? ? yes Os(2) N(1) Os(3) 85.0(4) ? ? ? yes Os(1) C(1) O(1) 178(1) ? ? ? yes Os(1) C(2) O(2) 178(1) ? ? ? yes Os(1) C(3) O(3) 176(1) ? ? ? yes Os(2) C(4) O(4) 178(1) ? ? ? yes Os(2) C(5) O(5) 178(1) ? ? ? yes Os(2) C(6) O(6) 175(1) ? ? ? yes Os(3) C(7) O(7) 179(1) ? ? ? yes Os(3) C(8) O(8) 178(1) ? ? ? yes Os(3) C(9) O(9) 178(1) ? ? ? yes Os(2) Os(1) H(4) 93.12 ? ? ? yes Os(3) Os(1) H(4) 39.08 ? ? ? yes Br(1) Os(1) H(4) 76.78 ? ? ? yes C(1) Os(1) H(4) 79.54 ? ? ? yes C(2) Os(1) H(4) 103.62 ? ? ? yes C(3) Os(1) H(4) 165.57 ? ? ? yes Os(1) Os(2) H(3) 96.25 ? ? ? yes Os(3) Os(2) H(3) 48.52 ? ? ? yes N(1) Os(2) H(3) 86.31 ? ? ? yes C(4) Os(2) H(3) 83.86 ? ? ? yes C(5) Os(2) H(3) 171.94 ? ? ? yes C(6) Os(2) H(3) 77.29 ? ? ? yes Os(1) Os(3) H(3) 84.27 ? ? ? yes Os(1) Os(3) H(4) 33.25 ? ? ? yes Os(2) Os(3) H(3) 40.11 ? ? ? yes Os(2) Os(3) H(4) 88.07 ? ? ? yes N(1) Os(3) H(3) 79.44 ? ? ? yes N(1) Os(3) H(4) 86.41 ? ? ? yes C(7) Os(3) H(3) 74.09 ? ? ? yes C(7) Os(3) H(4) 168.49 ? ? ? yes C(8) Os(3) H(3) 166.84 ? ? ? yes C(8) Os(3) H(4) 74.64 ? ? ? yes C(9) Os(3) H(3) 91.41 ? ? ? yes C(9) Os(3) H(4) 89.35 ? ? ? yes H(3) Os(3) H(4) 117.35 ? ? ? yes Os(2) N(1) H(1) 115.20 ? ? ? yes Os(2) N(1) H(2) 115.20 ? ? ? yes Os(3) N(1) H(1) 115.20 ? ? ? yes Os(3) N(1) H(2) 115.20 ? ? ? yes H(1) N(1) H(2) 109.46 ? ? ? yes #------------------------------------------------------------------------------ data_wt0525w_Yat099_compound_6 _database_code_CSD 192364 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Oct 13 16:55:40 2000' _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 SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.985(1) _cell_length_b 9.147(1) _cell_length_c 24.149(2) _cell_angle_alpha 90 _cell_angle_beta 93.12(1) _cell_angle_gamma 90 _cell_volume 1981.8(4) _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 '-P 2ybc' 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 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.090 _exptl_crystal_density_diffrn 3.911 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 1166.86 _chemical_formula_analytical ? _chemical_formula_sum 'C11 H4 Br N O11 Os4 ' _chemical_formula_moiety 'C11 H4 Br N O11 Os4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2016.00 _exptl_absorpt_coefficient_mu 27.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.001 _exptl_absorpt_correction_T_max 0.083 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Bruker SMART 1K CCD Detector' _diffrn_measurement_device 'unknown' _diffrn_measurement_method '\w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 12406 _reflns_number_total 4749 _reflns_number_gt 2800 _reflns_threshold_expression 'I>\1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_reduction_process 'SAINT+ (Bruker, 1999)' _diffrn_measured_fraction_theta_max 27.5 _diffrn_measured_fraction_theta_full 27.5 _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 16 -1.216 7.603 'International Tables' N 0 4 0.006 0.003 'International Tables' O 0 44 0.011 0.006 'International Tables' C 0 44 0.003 0.002 'International Tables' H 0 16 0.000 0.000 'International Tables' Br 0 4 -0.290 2.459 '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) 0.02797(9) 0.7233(1) 0.37888(4) 0.0308(3) Uij ? ? Os(2) 0.30708(10) 0.7710(1) 0.44695(4) 0.0313(3) Uij ? ? Os(3) 0.13286(10) 1.0060(1) 0.38745(4) 0.0292(2) Uij ? ? Os(4) 0.3072(1) 0.8158(1) 0.33274(5) 0.0352(3) Uij ? ? Br(1) 0.0977(3) 1.2317(3) 0.4479(1) 0.0457(7) Uij ? ? O(1) 0.143(2) 0.438(1) 0.3276(7) 0.058(6) Uij ? ? O(2) -0.209(1) 0.559(2) 0.4290(7) 0.079(8) Uij ? ? O(3) -0.164(2) 0.769(2) 0.2727(7) 0.058(6) Uij ? ? O(4) 0.289(2) 0.777(2) 0.5698(8) 0.064(7) Uij ? ? O(5) 0.429(2) 0.465(2) 0.4396(10) 0.083(8) Uij ? ? O(6) 0.617(2) 0.899(2) 0.4569(8) 0.064(7) Uij ? ? O(7) -0.065(2) 1.114(2) 0.2919(9) 0.076(8) Uij ? ? O(8) 0.394(2) 1.186(2) 0.3480(9) 0.082(7) Uij ? ? O(9) 0.612(2) 0.937(2) 0.3316(9) 0.072(7) Uij ? ? O(10) 0.443(2) 0.521(3) 0.294(1) 0.12(1) Uij ? ? O(11) 0.210(2) 0.917(2) 0.2179(8) 0.065(7) Uij ? ? N(1) -0.046(2) 0.921(2) 0.4216(8) 0.040(5) Uij ? ? C(1) 0.113(3) 0.554(2) 0.345(1) 0.061(8) Uij ? ? C(2) -0.113(2) 0.623(3) 0.417(1) 0.067(9) Uij ? ? C(3) -0.093(3) 0.749(3) 0.308(1) 0.046(7) Uij ? ? C(4) 0.290(2) 0.775(3) 0.525(1) 0.032(6) Uij ? ? C(5) 0.394(3) 0.581(3) 0.443(1) 0.037(6) Uij ? ? C(6) 0.499(3) 0.849(3) 0.452(1) 0.041(6) Uij ? ? C(7) 0.016(3) 1.079(3) 0.325(1) 0.037(6) Uij ? ? C(8) 0.295(3) 1.111(3) 0.361(1) 0.057(8) Uij ? ? C(9) 0.499(3) 0.888(3) 0.328(1) 0.046(7) Uij ? ? C(10) 0.396(3) 0.618(4) 0.307(1) 0.065(9) Uij ? ? C(11) 0.245(2) 0.869(3) 0.262(1) 0.041(6) Uij ? ? H(1) 0.2506 0.9582 0.4532 0.0608 Uij ? ? H(2) 0.1392 0.6589 0.4414 0.0608 Uij ? ? H(3) -0.1288 0.9557 0.4103 0.0482 Uij ? ? H(4) -0.0419 0.9176 0.4565 0.0482 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) 0.0303(5) 0.0270(5) 0.0346(6) -0.0013(4) -0.0013(4) -0.0013(5) Os(2) 0.0336(5) 0.0271(5) 0.0325(6) 0.0020(4) -0.0055(4) 0.0003(5) Os(3) 0.0300(4) 0.0255(4) 0.0321(5) 0.0010(4) 0.0020(4) 0.0028(5) Os(4) 0.0343(5) 0.0370(6) 0.0347(6) 0.0022(4) 0.0056(5) -0.0031(5) Br(1) 0.064(2) 0.028(1) 0.046(2) 0.001(1) 0.010(1) -0.0076(10) O(1) 0.06(1) 0.020(9) 0.09(2) 0.018(9) 0.01(1) -0.02(1) O(2) 0.08(1) 0.05(1) 0.11(2) 0.00(1) -0.02(1) -0.03(1) O(3) 0.048(10) 0.08(1) 0.04(1) 0.00(1) -0.039(9) -0.01(1) O(4) 0.07(1) 0.07(1) 0.05(1) 0.01(1) 0.00(1) 0.01(1) O(5) 0.05(1) 0.02(1) 0.18(2) 0.009(9) 0.01(1) -0.01(1) O(6) 0.06(1) 0.06(1) 0.07(2) -0.01(1) -0.01(1) 0.01(1) O(7) 0.05(1) 0.05(1) 0.13(2) -0.008(10) -0.02(1) 0.02(1) O(8) 0.025(9) 0.05(1) 0.17(2) -0.007(9) 0.03(1) 0.02(1) O(9) 0.026(9) 0.06(1) 0.13(2) -0.001(9) 0.01(1) -0.02(1) O(10) 0.06(1) 0.09(2) 0.20(3) 0.04(1) 0.06(2) -0.02(2) O(11) 0.08(1) 0.07(1) 0.05(1) -0.02(1) 0.01(1) 0.00(1) #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were attempted to be refined anisotropically, but all eleven carbon atoms and the nitrogen atom were found unsuitable to be refined anisotropic, thus refined isotropic only. All hydride atoms were located from difference fourier map and potential energys calculation but were not refined. Hydrogens attached to organic moieties were refined as riding on their parent atoms. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2800 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0480 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.537 _refine_ls_shift/su_max 0.0805 _refine_ls_shift/su_mean ? _refine_diff_density_min -2.88 _refine_diff_density_max 3.59 #------------------------------------------------------------------------------ _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) 2.955(2) ? ? yes Os(1) Os(3) 2.756(2) ? ? yes Os(1) Os(4) 2.925(2) ? ? yes Os(1) N(1) 2.21(2) ? ? yes Os(1) C(1) 1.93(1) ? ? yes Os(1) C(2) 1.85(1) ? ? yes Os(1) C(3) 1.99(3) ? ? yes Os(2) Os(3) 2.982(2) ? ? yes Os(2) Os(4) 2.788(2) ? ? yes Os(2) C(4) 1.89(3) ? ? yes Os(2) C(5) 1.91(3) ? ? yes Os(2) C(6) 1.87(3) ? ? yes Os(3) Os(4) 2.730(2) ? ? yes Os(3) Br(1) 2.558(3) ? ? yes Os(3) N(1) 2.00(2) ? ? yes Os(3) C(7) 1.92(3) ? ? yes Os(3) C(8) 1.89(3) ? ? yes Os(4) C(9) 1.85(3) ? ? yes Os(4) C(10) 2.09(4) ? ? yes Os(4) C(11) 1.84(3) ? ? yes O(1) C(1) 1.17(1) ? ? yes O(2) C(2) 1.09(2) ? ? yes O(3) C(3) 1.05(3) ? ? yes O(4) C(4) 1.09(3) ? ? yes O(5) C(5) 1.11(3) ? ? yes O(6) C(6) 1.16(3) ? ? yes O(7) C(7) 1.09(3) ? ? yes O(8) C(8) 1.18(3) ? ? yes O(9) C(9) 1.11(3) ? ? yes O(10) C(10) 1.03(4) ? ? yes O(11) C(11) 1.17(3) ? ? yes Os(1) H(2) 1.861 ? ? yes Os(2) H(1) 1.794 ? ? yes Os(2) H(2) 1.823 ? ? yes Os(3) H(1) 1.909 ? ? yes N(1) H(3) 0.840 ? ? yes N(1) H(4) 0.841 ? ? 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) 62.83(4) ? ? ? yes Os(2) Os(1) Os(4) 56.61(4) ? ? ? yes Os(2) Os(1) N(1) 83.5(5) ? ? ? yes Os(2) Os(1) C(1) 90(1) ? ? ? yes Os(2) Os(1) C(2) 112(1) ? ? ? yes Os(2) Os(1) C(3) 150.2(9) ? ? ? yes Os(3) Os(1) Os(4) 57.35(4) ? ? ? yes Os(3) Os(1) N(1) 45.9(6) ? ? ? yes Os(3) Os(1) C(1) 130.1(10) ? ? ? yes Os(3) Os(1) C(2) 131(1) ? ? ? yes Os(3) Os(1) C(3) 96.9(10) ? ? ? yes Os(4) Os(1) N(1) 103.1(6) ? ? ? yes Os(4) Os(1) C(1) 72.8(10) ? ? ? yes Os(4) Os(1) C(2) 163(1) ? ? ? yes Os(4) Os(1) C(3) 94.5(9) ? ? ? yes N(1) Os(1) C(1) 174(1) ? ? ? yes N(1) Os(1) C(2) 86(1) ? ? ? yes N(1) Os(1) C(3) 97(1) ? ? ? yes C(1) Os(1) C(2) 96(1) ? ? ? yes C(1) Os(1) C(3) 86(1) ? ? ? yes C(2) Os(1) C(3) 97(1) ? ? ? yes Os(1) Os(2) Os(3) 55.32(4) ? ? ? yes Os(1) Os(2) Os(4) 61.14(4) ? ? ? yes Os(1) Os(2) C(4) 116.3(8) ? ? ? yes Os(1) Os(2) C(5) 100.0(8) ? ? ? yes Os(1) Os(2) C(6) 147.6(9) ? ? ? yes Os(3) Os(2) Os(4) 56.35(4) ? ? ? yes Os(3) Os(2) C(4) 113.2(9) ? ? ? yes Os(3) Os(2) C(5) 146.9(9) ? ? ? yes Os(3) Os(2) C(6) 102.4(9) ? ? ? yes Os(4) Os(2) C(4) 169.3(9) ? ? ? yes Os(4) Os(2) C(5) 93.7(9) ? ? ? yes Os(4) Os(2) C(6) 87.3(10) ? ? ? yes C(4) Os(2) C(5) 97(1) ? ? ? yes C(4) Os(2) C(6) 93(1) ? ? ? yes C(5) Os(2) C(6) 88(1) ? ? ? yes Os(1) Os(3) Os(2) 61.85(4) ? ? ? yes Os(1) Os(3) Os(4) 64.43(4) ? ? ? yes Os(1) Os(3) Br(1) 138.39(9) ? ? ? yes Os(1) Os(3) N(1) 52.4(7) ? ? ? yes Os(1) Os(3) C(7) 95.6(9) ? ? ? yes Os(1) Os(3) C(8) 136(1) ? ? ? yes Os(2) Os(3) Os(4) 58.24(4) ? ? ? yes Os(2) Os(3) Br(1) 112.62(9) ? ? ? yes Os(2) Os(3) N(1) 86.3(6) ? ? ? yes Os(2) Os(3) C(7) 152.0(9) ? ? ? yes Os(2) Os(3) C(8) 97.6(10) ? ? ? yes Os(4) Os(3) Br(1) 151.96(9) ? ? ? yes Os(4) Os(3) N(1) 116.6(7) ? ? ? yes Os(4) Os(3) C(7) 98.3(9) ? ? ? yes Os(4) Os(3) C(8) 71(1) ? ? ? yes Br(1) Os(3) N(1) 87.1(7) ? ? ? yes Br(1) Os(3) C(7) 95.2(9) ? ? ? yes Br(1) Os(3) C(8) 84(1) ? ? ? yes N(1) Os(3) C(7) 92(1) ? ? ? yes N(1) Os(3) C(8) 171(1) ? ? ? yes C(7) Os(3) C(8) 87(1) ? ? ? yes Os(1) Os(4) Os(2) 62.24(4) ? ? ? yes Os(1) Os(4) Os(3) 58.22(4) ? ? ? yes Os(1) Os(4) C(9) 161(1) ? ? ? yes Os(1) Os(4) C(10) 102(1) ? ? ? yes Os(1) Os(4) C(11) 102.1(9) ? ? ? yes Os(2) Os(4) Os(3) 65.40(4) ? ? ? yes Os(2) Os(4) C(9) 99.7(10) ? ? ? yes Os(2) Os(4) C(10) 100(1) ? ? ? yes Os(2) Os(4) C(11) 160.9(9) ? ? ? yes Os(3) Os(4) C(9) 111(1) ? ? ? yes Os(3) Os(4) C(10) 159(1) ? ? ? yes Os(3) Os(4) C(11) 97.5(9) ? ? ? yes C(9) Os(4) C(10) 85(1) ? ? ? yes C(9) Os(4) C(11) 94(1) ? ? ? yes C(10) Os(4) C(11) 93(1) ? ? ? yes Os(1) N(1) Os(3) 81.7(8) ? ? ? yes Os(1) C(1) O(1) 168(2) ? ? ? yes Os(1) C(2) O(2) 164(3) ? ? ? yes Os(1) C(3) O(3) 174(3) ? ? ? yes Os(2) C(4) O(4) 175(2) ? ? ? yes Os(2) C(5) O(5) 172(2) ? ? ? yes Os(2) C(6) O(6) 176(3) ? ? ? yes Os(3) C(7) O(7) 171(2) ? ? ? yes Os(3) C(8) O(8) 174(3) ? ? ? yes Os(4) C(9) O(9) 170(3) ? ? ? yes Os(4) C(10) O(10) 178(3) ? ? ? yes Os(4) C(11) O(11) 173(2) ? ? ? yes Os(2) Os(1) H(2) 36.21 ? ? ? yes Os(3) Os(1) H(2) 94.00 ? ? ? yes Os(4) Os(1) H(2) 88.09 ? ? ? yes N(1) Os(1) H(2) 92.43 ? ? ? yes C(1) Os(1) H(2) 83.48 ? ? ? yes C(2) Os(1) H(2) 77.73 ? ? ? yes C(3) Os(1) H(2) 168.37 ? ? ? yes Os(1) Os(2) H(1) 87.24 ? ? ? yes Os(1) Os(2) H(2) 37.09 ? ? ? yes Os(3) Os(2) H(1) 37.71 ? ? ? yes Os(3) Os(2) H(2) 87.68 ? ? ? yes Os(4) Os(2) H(1) 87.58 ? ? ? yes Os(4) Os(2) H(2) 93.13 ? ? ? yes C(4) Os(2) H(1) 81.84 ? ? ? yes C(4) Os(2) H(2) 88.51 ? ? ? yes C(5) Os(2) H(1) 172.33 ? ? ? yes C(5) Os(2) H(2) 79.68 ? ? ? yes C(6) Os(2) H(1) 84.07 ? ? ? yes C(6) Os(2) H(2) 168.10 ? ? ? yes H(1) Os(2) H(2) 107.83 ? ? ? yes Os(1) Os(3) H(1) 91.10 ? ? ? yes Os(2) Os(3) H(1) 35.09 ? ? ? yes Os(4) Os(3) H(1) 87.12 ? ? ? yes Br(1) Os(3) H(1) 77.91 ? ? ? yes N(1) Os(3) H(1) 89.39 ? ? ? yes C(7) Os(3) H(1) 172.77 ? ? ? yes C(8) Os(3) H(1) 89.46 ? ? ? yes Os(1) N(1) H(3) 115.92 ? ? ? yes Os(1) N(1) H(4) 115.89 ? ? ? yes Os(3) N(1) H(3) 115.94 ? ? ? yes Os(3) N(1) H(4) 115.90 ? ? ? yes H(3) N(1) H(4) 109.42 ? ? ? yes #------------------------------------------------------------------------------ #===End