Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Joyce L.C. Chim ' 'Man-Kit Lau' 'Wa-Hung Leung' 'Wing-tak Wong' ' Qian-Feng Zhang' _publ_contact_author_name 'Dr Wa-Hung Leung' _publ_contact_author_address ;Department of Chemistry The Hong Kong University of Science & Technology Clear Water Bay Kowloon HONG KONG ; _publ_contact_author_email CHLEUNG@UST.HK data_Wong880_WHL257_17_Dec_1999 compound 2 _database_code_CSD 164948 #------------------------------------------------------------------- _audit_creation_date 'Sat May 24 11:45:14 1997' _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 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------ _cell_length_a 12.424(2) _cell_length_b 17.168(3) _cell_length_c 9.184(2) _cell_angle_alpha 91.71(2) _cell_angle_beta 106.76(1) _cell_angle_gamma 95.82(2) _cell_volume 1862.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.4 _cell_measurement_theta_max 16.6 #---------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _exptl_crystal_description 'rod' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_meas ? _chemical_formula_weight 779.03 _chemical_formula_analytical ? _chemical_formula_sum 'C41 H48 O3 Os' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 788.00 _exptl_absorpt_coefficient_mu 3.456 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.905 #--------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_decay_% -3.20 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 1 0 2 2 -3 3 -3 -2 _diffrn_reflns_number 5289 _reflns_number_total 5016 _reflns_number_observed 3843 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 3.32 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00116 _diffrn_orient_matrix_UB_12 0.05246 _diffrn_orient_matrix_UB_13 -0.04438 _diffrn_orient_matrix_UB_21 0.08371 _diffrn_orient_matrix_UB_22 0.00968 _diffrn_orient_matrix_UB_23 0.04807 _diffrn_orient_matrix_UB_31 0.01231 _diffrn_orient_matrix_UB_32 -0.02441 _diffrn_orient_matrix_UB_33 -0.09328 #------------------------------------------------------------------ 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 2 -1.216 7.603 'International Tables' O 0 6 0.011 0.006 'International Tables' C 0 82 0.003 0.002 'International Tables' H 0 96 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) 0.19203(3) 0.27379(2) 0.31973(4) 0.0582(1) Uij ? ? O(1) -0.2334(8) 0.2397(5) -0.3772(10) 0.126(4) Uij ? ? O(2) 0.619(2) 0.292(1) -0.030(2) 0.215(8) Uij ? ? O(3) 0.1242(10) -0.0300(5) 0.793(1) 0.156(5) Uij ? ? O(4) 0.191(5) 0.563(3) 0.834(6) 0.21(1) Uij ? ? C(1) 0.0630(8) 0.2833(5) 0.1321(9) 0.059(3) Uij ? ? C(2) 0.0551(8) 0.3529(6) 0.054(1) 0.068(3) Uij ? ? C(3) -0.0325(9) 0.3523(6) -0.077(1) 0.074(3) Uij ? ? C(4) -0.1103(8) 0.2886(6) -0.137(1) 0.065(3) Uij ? ? C(5) -0.1036(8) 0.2201(6) -0.061(1) 0.063(3) Uij ? ? C(6) -0.0173(8) 0.2203(5) 0.074(1) 0.066(3) Uij ? ? C(7) 0.1342(10) 0.4274(6) 0.110(1) 0.107(4) Uij ? ? C(8) -0.1855(10) 0.1467(6) -0.116(1) 0.099(4) Uij ? ? C(9) -0.2013(10) 0.2945(7) -0.283(1) 0.086(4) Uij ? ? C(10) -0.251(1) 0.3703(8) -0.316(2) 0.129(5) Uij ? ? C(11) 0.3308(8) 0.2707(5) 0.2567(9) 0.056(3) Uij ? ? C(12) 0.4343(8) 0.2542(5) 0.3502(10) 0.062(3) Uij ? ? C(13) 0.5253(8) 0.2558(6) 0.293(1) 0.071(3) Uij ? ? C(14) 0.5174(9) 0.2735(7) 0.142(1) 0.082(4) Uij ? ? C(15) 0.4156(9) 0.2888(6) 0.046(1) 0.077(4) Uij ? ? C(16) 0.3254(8) 0.2872(5) 0.1036(10) 0.066(3) Uij ? ? C(17) 0.4488(9) 0.2332(7) 0.516(1) 0.088(4) Uij ? ? C(18) 0.396(1) 0.3062(9) -0.119(1) 0.129(6) Uij ? ? C(19) 0.621(2) 0.276(1) 0.095(2) 0.119(6) Uij ? ? C(20) 0.729(2) 0.270(1) 0.196(2) 0.144(7) Uij ? ? C(21) 0.1677(7) 0.1754(5) 0.4212(9) 0.055(3) Uij ? ? C(22) 0.1685(8) 0.1012(5) 0.3563(10) 0.062(3) Uij ? ? C(23) 0.1603(8) 0.0355(5) 0.441(1) 0.069(3) Uij ? ? C(24) 0.1486(8) 0.0430(6) 0.589(1) 0.068(3) Uij ? ? C(25) 0.1464(8) 0.1165(7) 0.653(1) 0.073(3) Uij ? ? C(26) 0.1586(8) 0.1802(5) 0.5688(10) 0.064(3) Uij ? ? C(27) 0.181(1) 0.0866(6) 0.199(1) 0.087(4) Uij ? ? C(28) 0.133(1) 0.1311(7) 0.811(1) 0.111(5) Uij ? ? C(29) 0.139(1) -0.0315(8) 0.668(1) 0.098(5) Uij ? ? C(30) 0.145(1) -0.1072(8) 0.595(2) 0.127(6) Uij ? ? C(31) 0.2112(8) 0.3642(6) 0.468(1) 0.067(3) Uij ? ? C(32) 0.1239(10) 0.3845(7) 0.524(1) 0.085(4) Uij ? ? C(33) 0.148(1) 0.4473(8) 0.632(2) 0.102(5) Uij ? ? C(34) 0.254(1) 0.4872(7) 0.695(2) 0.104(5) Uij ? ? C(35) 0.340(1) 0.4686(6) 0.639(1) 0.087(4) Uij ? ? C(36) 0.3183(9) 0.4074(6) 0.528(1) 0.071(3) Uij ? ? C(37) 0.005(1) 0.3436(8) 0.462(2) 0.122(6) Uij ? ? C(38) 0.459(1) 0.5110(8) 0.702(2) 0.143(6) Uij ? ? C(39) 0.275(4) 0.545(3) 0.827(5) 0.08(1) Uij ? ? C(40) 0.360(5) 0.548(3) 0.942(6) 0.12(1) Uij ? ? C(41) 0.483(3) 0.031(2) 0.057(5) 0.34(1) Uij ? ? C(42) 0.516(3) -0.035(2) 0.151(4) 0.33(1) Uij ? ? C(43) 0.504(3) -0.001(2) 0.335(4) 0.37(1) Uij ? ? H(1) -0.0398 0.3991 -0.1296 0.0887 Uij ? ? H(2) -0.0134 0.1744 0.1299 0.0793 Uij ? ? H(3) 0.5960 0.2445 0.3575 0.0848 Uij ? ? H(4) 0.2548 0.2978 0.0376 0.0798 Uij ? ? H(5) 0.1628 -0.0151 0.3984 0.0826 Uij ? ? H(6) 0.1610 0.2309 0.6147 0.0768 Uij ? ? H(7) 0.0871 0.4638 0.6641 0.1228 Uij ? ? H(8) 0.3786 0.3941 0.4914 0.0852 Uij ? ? H(9) 0.1901 0.4189 0.2013 0.1288 Uij ? ? H(10) 0.1698 0.4421 0.0343 0.1288 Uij ? ? H(11) 0.0925 0.4681 0.1282 0.1288 Uij ? ? H(12) -0.2231 0.1339 -0.0416 0.1193 Uij ? ? H(13) -0.2396 0.1554 -0.2089 0.1193 Uij ? ? H(14) -0.1452 0.1046 -0.1315 0.1193 Uij ? ? H(15) -0.2178 0.4075 -0.2324 0.1548 Uij ? ? H(16) -0.2375 0.3899 -0.4053 0.1548 Uij ? ? H(17) -0.3307 0.3617 -0.3309 0.1548 Uij ? ? H(18) 0.3792 0.2352 0.5390 0.1055 Uij ? ? H(19) 0.4706 0.1818 0.5290 0.1055 Uij ? ? H(20) 0.5055 0.2696 0.5830 0.1055 Uij ? ? H(21) 0.3704 0.3564 -0.1349 0.1546 Uij ? ? H(22) 0.4646 0.3055 -0.1449 0.1546 Uij ? ? H(23) 0.3403 0.2675 -0.1816 0.1546 Uij ? ? H(24) 0.7222 0.2578 0.2934 0.1735 Uij ? ? H(25) 0.7634 0.2302 0.1583 0.1735 Uij ? ? H(26) 0.7756 0.3189 0.2057 0.1735 Uij ? ? H(27) 0.1173 0.0530 0.1382 0.1042 Uij ? ? H(28) 0.1857 0.1350 0.1525 0.1042 Uij ? ? H(29) 0.2479 0.0625 0.2068 0.1042 Uij ? ? H(30) 0.1975 0.1640 0.8728 0.1329 Uij ? ? H(31) 0.0670 0.1559 0.8033 0.1329 Uij ? ? H(32) 0.1272 0.0825 0.8569 0.1329 Uij ? ? H(33) 0.0764 -0.1400 0.5825 0.1532 Uij ? ? H(34) 0.1565 -0.0995 0.4985 0.1532 Uij ? ? H(35) 0.2063 -0.1313 0.6574 0.1532 Uij ? ? H(36) -0.0430 0.3653 0.5127 0.1470 Uij ? ? H(37) -0.0228 0.3505 0.3557 0.1470 Uij ? ? H(38) 0.0049 0.2892 0.4779 0.1470 Uij ? ? H(39) 0.5094 0.4747 0.7479 0.1720 Uij ? ? H(40) 0.4824 0.5339 0.6218 0.1720 Uij ? ? H(41) 0.4593 0.5509 0.7762 0.1720 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) 0.0619(3) 0.0622(2) 0.0473(2) -0.0015(2) 0.0138(2) 0.0073(2) O(1) 0.130(8) 0.115(7) 0.102(7) 0.022(6) -0.014(6) -0.006(6) O(3) 0.25(1) 0.135(8) 0.094(7) -0.002(8) 0.073(8) 0.054(6) C(1) 0.063(6) 0.057(6) 0.049(5) -0.005(5) 0.009(5) 0.003(4) C(2) 0.070(7) 0.068(7) 0.062(6) 0.000(5) 0.014(5) 0.008(5) C(3) 0.075(7) 0.064(6) 0.074(7) 0.001(6) 0.008(6) 0.012(5) C(4) 0.058(6) 0.077(7) 0.050(6) 0.002(5) 0.004(5) 0.005(5) C(5) 0.060(6) 0.070(7) 0.058(6) -0.006(5) 0.021(5) 0.000(5) C(6) 0.069(7) 0.066(6) 0.063(6) 0.001(5) 0.020(5) 0.012(5) C(7) 0.105(9) 0.063(7) 0.116(10) -0.015(6) -0.020(7) 0.032(7) C(8) 0.104(9) 0.081(8) 0.089(8) -0.021(7) 0.001(7) 0.009(6) C(9) 0.091(9) 0.082(8) 0.080(8) 0.004(7) 0.019(7) 0.000(7) C(10) 0.12(1) 0.11(1) 0.12(1) 0.028(9) -0.020(9) 0.008(9) C(11) 0.065(6) 0.058(6) 0.039(5) -0.002(5) 0.010(5) 0.000(4) C(12) 0.068(7) 0.065(6) 0.052(6) 0.004(5) 0.016(5) 0.002(5) C(13) 0.058(7) 0.088(7) 0.061(6) 0.008(5) 0.009(5) 0.000(5) C(14) 0.068(8) 0.122(9) 0.068(7) 0.004(7) 0.041(6) 0.005(6) C(15) 0.063(7) 0.112(9) 0.050(6) -0.008(6) 0.015(5) 0.008(6) C(16) 0.069(7) 0.078(7) 0.043(5) -0.010(5) 0.009(5) 0.010(5) C(17) 0.078(8) 0.127(10) 0.055(6) 0.015(7) 0.011(5) 0.026(6) C(18) 0.12(1) 0.21(2) 0.060(7) -0.01(1) 0.041(7) 0.040(9) C(21) 0.055(6) 0.070(6) 0.037(5) 0.002(5) 0.008(4) 0.010(4) C(22) 0.074(7) 0.069(6) 0.047(5) 0.009(5) 0.024(5) 0.012(5) C(23) 0.079(7) 0.056(6) 0.063(6) 0.001(5) 0.009(5) 0.007(5) C(24) 0.070(7) 0.082(7) 0.048(6) -0.005(6) 0.016(5) 0.020(5) C(25) 0.080(7) 0.095(8) 0.041(5) -0.009(6) 0.020(5) 0.006(6) C(26) 0.070(7) 0.073(7) 0.046(6) -0.007(5) 0.018(5) -0.003(5) C(27) 0.15(1) 0.073(7) 0.051(6) 0.012(7) 0.044(7) 0.006(5) C(28) 0.16(1) 0.117(10) 0.064(7) -0.022(9) 0.057(8) 0.007(7) C(29) 0.111(10) 0.100(10) 0.080(9) -0.007(8) 0.026(7) 0.032(8) C(30) 0.15(1) 0.085(9) 0.15(1) 0.003(9) 0.04(1) 0.056(9) C(31) 0.068(7) 0.077(7) 0.058(6) 0.009(6) 0.023(5) 0.013(5) C(32) 0.085(9) 0.087(8) 0.085(8) 0.010(7) 0.026(7) 0.014(7) C(33) 0.14(1) 0.090(9) 0.10(1) 0.039(9) 0.062(9) 0.009(8) C(34) 0.14(1) 0.078(9) 0.10(1) 0.001(9) 0.046(10) -0.005(7) C(35) 0.113(10) 0.066(7) 0.068(7) -0.020(7) 0.017(7) 0.009(6) C(36) 0.085(8) 0.069(7) 0.056(6) -0.005(6) 0.020(6) 0.009(5) C(37) 0.10(1) 0.14(1) 0.14(1) 0.019(9) 0.055(9) -0.008(10) C(38) 0.18(2) 0.11(1) 0.12(1) -0.06(1) 0.03(1) -0.019(9) #-------------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3843 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0418 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0442 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.564 _refine_ls_shift/esd_max 0.0640 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.57 _refine_diff_density_max 1.01 #---------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE # e.g. C1 C2 1.541(1) . . yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # --ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------- _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER' _publ_contact_author_fax ' ENTER FAX NUMBER' _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #====================end of compound2================================= data_wong892_WHL263 compound4 _database_code_CSD 164949 #------------------------------------------------------------------------- _audit_creation_date 'Fri May 23 16:01:25 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------ _cell_length_a 37.556(8) _cell_length_b 9.256(6) _cell_length_c 18.856(7) _cell_angle_alpha 90 _cell_angle_beta 97.13(3) _cell_angle_gamma 90 _cell_volume 6503(4) _cell_formula_units_Z 8 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.3 _cell_measurement_theta_max 16.7 #---------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? #loop_ #_symmetry_equiv_pos_as_xyz #' +x, +y, +z' #' +x, +y, +z' #' -x, +y, 1/2-z' #' -x, +y, 1/2-z' #' -x, -y, -z' #' -x, -y, -z' #' +x, -y, 1/2+z' #' +x, -y, 1/2+z' #----------------------------------------------------------------- _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_meas ? _chemical_formula_weight 926.42 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H32 Br4 Os' _chemical_formula_moiety 'C32 H32 Br4 Os' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3520.00 _exptl_absorpt_coefficient_mu 8.867 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.281 #--------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_decay_% 0.57 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 -1 -5 11 -1 -3 3 3 -4 _diffrn_reflns_number 6205 _reflns_number_total 6101 _reflns_number_observed 117 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 7.13 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00968 _diffrn_orient_matrix_UB_12 -0.01578 _diffrn_orient_matrix_UB_13 -0.05125 _diffrn_orient_matrix_UB_21 -0.02493 _diffrn_orient_matrix_UB_22 0.01580 _diffrn_orient_matrix_UB_23 0.01189 _diffrn_orient_matrix_UB_31 0.00228 _diffrn_orient_matrix_UB_32 0.10571 _diffrn_orient_matrix_UB_33 -0.00943 #------------------------------------------------------------------ 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' Br 0 32 -0.290 2.459 'International Tables' C 0 256 0.003 0.002 'International Tables' H 0 256 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) 0.12667(2) 0.21705(7) 0.71352(3) 0.0407(2) Uij ? ? Br(1) 0.04250(7) 0.6655(2) 0.4717(1) 0.0932(9) Uij ? ? Br(2) 0.00431(6) -0.1477(2) 0.8703(1) 0.0804(8) Uij ? ? Br(3) 0.23266(7) -0.2723(3) 0.5864(1) 0.0952(9) Uij ? ? Br(4) 0.22329(8) 0.6665(3) 0.9366(1) 0.112(1) Uij ? ? C(1) 0.1017(4) 0.337(2) 0.6361(8) 0.042(4) Uij ? ? C(2) 0.0760(4) 0.293(2) 0.5816(8) 0.046(4) Uij ? ? C(3) 0.0590(5) 0.393(2) 0.5339(8) 0.056(5) Uij ? ? C(4) 0.0672(5) 0.538(2) 0.5398(8) 0.048(5) Uij ? ? C(5) 0.0906(5) 0.591(2) 0.5921(8) 0.049(5) Uij ? ? C(6) 0.1089(4) 0.492(2) 0.6412(8) 0.047(4) Uij ? ? C(7) 0.0657(6) 0.140(2) 0.5729(10) 0.078(6) Uij ? ? C(8) 0.1001(5) 0.747(2) 0.6014(9) 0.072(6) Uij ? ? C(9) 0.0889(4) 0.116(2) 0.7613(7) 0.042(4) Uij ? ? C(10) 0.0592(5) 0.182(2) 0.7840(8) 0.046(5) Uij ? ? C(11) 0.0345(5) 0.100(2) 0.8162(8) 0.045(4) Uij ? ? C(12) 0.0393(5) -0.047(2) 0.8264(8) 0.048(5) Uij ? ? C(13) 0.0683(5) -0.117(2) 0.8042(9) 0.057(5) Uij ? ? C(14) 0.0922(5) -0.034(2) 0.7728(8) 0.051(5) Uij ? ? C(15) 0.0517(5) 0.343(2) 0.7720(8) 0.058(5) Uij ? ? C(16) 0.0730(6) -0.279(2) 0.812(1) 0.098(7) Uij ? ? C(17) 0.1601(4) 0.072(2) 0.6754(8) 0.042(4) Uij ? ? C(18) 0.1820(5) -0.018(2) 0.7239(8) 0.047(5) Uij ? ? C(19) 0.2031(5) -0.120(2) 0.6939(8) 0.053(5) Uij ? ? C(20) 0.2022(5) -0.131(2) 0.6218(9) 0.060(5) Uij ? ? C(21) 0.1824(5) -0.044(2) 0.5734(8) 0.051(5) Uij ? ? C(22) 0.1603(4) 0.056(2) 0.6032(8) 0.046(4) Uij ? ? C(23) 0.1859(5) -0.007(2) 0.8034(9) 0.072(6) Uij ? ? C(24) 0.1814(5) -0.051(2) 0.4937(9) 0.071(6) Uij ? ? C(25) 0.1563(4) 0.343(2) 0.7829(7) 0.041(4) Uij ? ? C(26) 0.1878(5) 0.416(2) 0.7616(8) 0.051(5) Uij ? ? C(27) 0.2061(5) 0.511(2) 0.8097(9) 0.060(5) Uij ? ? C(28) 0.1952(5) 0.537(2) 0.8729(9) 0.061(5) Uij ? ? C(29) 0.1657(5) 0.470(2) 0.8968(8) 0.050(5) Uij ? ? C(30) 0.1465(4) 0.376(2) 0.8482(8) 0.047(4) Uij ? ? C(31) 0.2015(6) 0.389(2) 0.6913(10) 0.078(6) Uij ? ? C(32) 0.1531(6) 0.493(2) 0.9680(10) 0.086(7) Uij ? ? H(1) 0.0415 0.3602 0.4966 0.0662 Uij ? ? H(2) 0.1259 0.5276 0.6784 0.0568 Uij ? ? H(3) 0.0140 0.1461 0.8312 0.0542 Uij ? ? H(4) 0.1125 -0.0807 0.7577 0.0613 Uij ? ? H(5) 0.2181 -0.1828 0.7244 0.0640 Uij ? ? H(6) 0.1445 0.1151 0.5719 0.0544 Uij ? ? H(7) 0.2269 0.5576 0.7970 0.0718 Uij ? ? H(8) 0.1253 0.3324 0.8614 0.0565 Uij ? ? H(9) 0.0409 0.1304 0.5773 0.0930 Uij ? ? H(10) 0.0703 0.1071 0.5275 0.0930 Uij ? ? H(11) 0.0793 0.0847 0.6094 0.0930 Uij ? ? H(12) 0.1247 0.7613 0.5962 0.0864 Uij ? ? H(13) 0.0857 0.8034 0.5667 0.0864 Uij ? ? H(14) 0.0960 0.7782 0.6480 0.0864 Uij ? ? H(15) 0.0504 0.3893 0.8166 0.0702 Uij ? ? H(16) 0.0705 0.3856 0.7495 0.0702 Uij ? ? H(17) 0.0295 0.3555 0.7423 0.0702 Uij ? ? H(18) 0.0528 -0.3271 0.7861 0.1175 Uij ? ? H(19) 0.0942 -0.3087 0.7935 0.1175 Uij ? ? H(20) 0.0744 -0.3055 0.8610 0.1175 Uij ? ? H(21) 0.1794 -0.0960 0.8229 0.0861 Uij ? ? H(22) 0.2101 0.0153 0.8208 0.0861 Uij ? ? H(23) 0.1706 0.0677 0.8168 0.0861 Uij ? ? H(24) 0.1578 -0.0748 0.4728 0.0841 Uij ? ? H(25) 0.1880 0.0401 0.4762 0.0841 Uij ? ? H(26) 0.1977 -0.1229 0.4818 0.0841 Uij ? ? H(27) 0.1864 0.3213 0.6648 0.0930 Uij ? ? H(28) 0.2015 0.4774 0.6658 0.0930 Uij ? ? H(29) 0.2252 0.3523 0.7000 0.0930 Uij ? ? H(30) 0.1693 0.5568 0.9954 0.1020 Uij ? ? H(31) 0.1299 0.5344 0.9614 0.1020 Uij ? ? H(32) 0.1526 0.4032 0.9917 0.1020 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) 0.0444(4) 0.0336(3) 0.0440(3) -0.0052(5) 0.0047(3) -0.0002(4) Br(1) 0.101(2) 0.081(2) 0.092(2) 0.023(2) -0.010(1) 0.030(1) Br(2) 0.068(2) 0.070(1) 0.108(2) -0.011(1) 0.029(1) 0.031(1) Br(3) 0.100(2) 0.076(2) 0.120(2) 0.019(2) 0.058(2) -0.015(1) Br(4) 0.106(2) 0.083(2) 0.132(2) -0.012(2) -0.045(2) -0.044(2) #-------------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3117 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0673 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0507 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.962 _refine_ls_shift/esd_max 0.0620 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.14 _refine_diff_density_max 1.97 #---------------------------------------------------------------------- _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) C(1) 1.98(2) ? ? yes Os(1) C(9) 2.01(2) ? ? yes Os(1) C(17) 2.03(2) ? ? yes Os(1) C(25) 1.98(1) ? ? yes Br(1) C(4) 1.90(2) ? ? yes Br(2) C(12) 1.88(2) ? ? yes Br(3) C(20) 1.91(2) ? ? yes Br(4) C(28) 1.92(2) ? ? yes C(1) C(2) 1.38(2) ? ? yes C(1) C(6) 1.46(2) ? ? yes C(2) C(3) 1.39(2) ? ? yes C(2) C(7) 1.47(2) ? ? yes C(3) C(4) 1.38(2) ? ? yes C(4) C(5) 1.33(2) ? ? yes C(5) C(6) 1.41(2) ? ? yes C(5) C(8) 1.50(2) ? ? yes C(9) C(10) 1.38(2) ? ? yes C(9) C(14) 1.40(2) ? ? yes C(10) C(11) 1.39(2) ? ? yes C(10) C(15) 1.53(2) ? ? yes C(11) C(12) 1.38(2) ? ? yes C(12) C(13) 1.38(2) ? ? yes C(13) C(14) 1.37(2) ? ? yes C(13) C(16) 1.52(2) ? ? yes C(17) C(18) 1.42(2) ? ? yes C(17) C(22) 1.37(2) ? ? yes C(18) C(19) 1.40(2) ? ? yes C(18) C(23) 1.49(2) ? ? yes C(19) C(20) 1.36(2) ? ? yes C(20) C(21) 1.37(2) ? ? yes C(21) C(22) 1.41(2) ? ? yes C(21) C(24) 1.50(2) ? ? yes C(25) C(26) 1.46(2) ? ? yes C(25) C(30) 1.36(2) ? ? yes C(26) C(27) 1.38(2) ? ? yes C(26) C(31) 1.50(2) ? ? yes C(27) C(28) 1.33(2) ? ? yes C(28) C(29) 1.39(2) ? ? yes C(29) C(30) 1.40(2) ? ? yes C(29) C(32) 1.49(2) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) Os(1) C(9) 107.3(6) ? ? ? yes C(1) Os(1) C(17) 111.6(6) ? ? ? yes C(1) Os(1) C(25) 109.5(6) ? ? ? yes C(9) Os(1) C(17) 110.8(6) ? ? ? yes C(9) Os(1) C(25) 110.3(6) ? ? ? yes C(17) Os(1) C(25) 107.4(6) ? ? ? yes Os(1) C(1) C(2) 127(1) ? ? ? yes Os(1) C(1) C(6) 115(1) ? ? ? yes C(2) C(1) C(6) 116(1) ? ? ? yes C(1) C(2) C(3) 120(1) ? ? ? yes C(1) C(2) C(7) 121(1) ? ? ? yes C(3) C(2) C(7) 118(1) ? ? ? yes C(2) C(3) C(4) 121(1) ? ? ? yes Br(1) C(4) C(3) 117(1) ? ? ? yes Br(1) C(4) C(5) 119(1) ? ? ? yes C(3) C(4) C(5) 122(1) ? ? ? yes C(4) C(5) C(6) 118(1) ? ? ? yes C(4) C(5) C(8) 124(1) ? ? ? yes C(6) C(5) C(8) 117(1) ? ? ? yes C(1) C(6) C(5) 121(1) ? ? ? yes Os(1) C(9) C(10) 125(1) ? ? ? yes Os(1) C(9) C(14) 118(1) ? ? ? yes C(10) C(9) C(14) 116(1) ? ? ? yes C(9) C(10) C(11) 120(1) ? ? ? yes C(9) C(10) C(15) 121(1) ? ? ? yes C(11) C(10) C(15) 118(1) ? ? ? yes C(10) C(11) C(12) 120(1) ? ? ? yes Br(2) C(12) C(11) 117(1) ? ? ? yes Br(2) C(12) C(13) 121(1) ? ? ? yes C(11) C(12) C(13) 121(1) ? ? ? yes C(12) C(13) C(14) 116(1) ? ? ? yes C(12) C(13) C(16) 121(1) ? ? ? yes C(14) C(13) C(16) 121(1) ? ? ? yes C(9) C(14) C(13) 124(1) ? ? ? yes Os(1) C(17) C(18) 119(1) ? ? ? yes Os(1) C(17) C(22) 120(1) ? ? ? yes C(18) C(17) C(22) 120(1) ? ? ? yes C(17) C(18) C(19) 116(1) ? ? ? yes C(17) C(18) C(23) 125(1) ? ? ? yes C(19) C(18) C(23) 117(1) ? ? ? yes C(18) C(19) C(20) 120(1) ? ? ? yes Br(3) C(20) C(19) 117(1) ? ? ? yes Br(3) C(20) C(21) 118(1) ? ? ? yes C(19) C(20) C(21) 124(1) ? ? ? yes C(20) C(21) C(22) 114(1) ? ? ? yes C(20) C(21) C(24) 125(1) ? ? ? yes C(22) C(21) C(24) 119(1) ? ? ? yes C(17) C(22) C(21) 122(1) ? ? ? yes Os(1) C(25) C(26) 119(1) ? ? ? yes Os(1) C(25) C(30) 122(1) ? ? ? yes C(26) C(25) C(30) 117(1) ? ? ? yes C(25) C(26) C(27) 117(1) ? ? ? yes C(25) C(26) C(31) 122(1) ? ? ? yes C(27) C(26) C(31) 119(1) ? ? ? yes C(26) C(27) C(28) 121(1) ? ? ? yes Br(4) C(28) C(27) 118(1) ? ? ? yes Br(4) C(28) C(29) 118(1) ? ? ? yes C(27) C(28) C(29) 123(1) ? ? ? yes C(28) C(29) C(30) 115(1) ? ? ? yes C(28) C(29) C(32) 125(1) ? ? ? yes C(30) C(29) C(32) 118(1) ? ? ? yes C(25) C(30) C(29) 123(1) ? ? ? yes #----------------------------------------------------------------------- _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER' _publ_contact_author_fax ' ENTER FAX NUMBER' _publ_contact_author_email ' ENTER EMAIL ADDRESS' _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=================end of compound 4================================ #=======================end of file==================================