#------------------------------------------------------------------------------ #$Date: 2014-07-11 21:33:45 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120075 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/07/51/4075160.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4075160 loop_ _publ_author_name 'Zhang, Jie' 'Huang, Kuo-Wei' 'Szalda, David J.' 'Bullock, R. Morris' _publ_section_title ; Efficient Synthesis of the Os−Os Dimers [Cp(CO)2Os]2, [Cp*(CO)2Os]2, and [(iPr4C5H)(CO)2Os]2and Computational Studies on the Relative Stabilities of Their Geometrical Isomers ; _journal_issue 9 _journal_name_full Organometallics _journal_page_first 2209 _journal_volume 25 _journal_year 2006 _chemical_formula_moiety 'C24 H30 O4 Os2' _chemical_formula_sum 'C24 H30 O4 Os2' _chemical_formula_weight 762.88 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.83(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.792(2) _cell_length_b 8.3580(17) _cell_length_c 14.374(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32 _cell_measurement_theta_min 15 _cell_volume 1159.1(4) _computing_cell_refinement 'CAD-4 (Enraf-Nonius, 1977)' _computing_data_collection 'CAD-4 (Enraf-Nonius, 1977)' _computing_data_reduction 'XCAD4VAX (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Enraf Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2382 _diffrn_reflns_theta_full 75.16 _diffrn_reflns_theta_max 75.16 _diffrn_reflns_theta_min 6.15 _diffrn_standards_decay_% <2% _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 20.601 _exptl_absorpt_correction_T_max 1.834 _exptl_absorpt_correction_T_min .548 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Parkin, S., Moezzi, B., and Hope, H., J. Appl. Cryst., 1995, 28, 53-56. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _refine_diff_density_max 2.184 _refine_diff_density_min -5.115 _refine_diff_density_rms 0.263 _refine_ls_extinction_coef 0.00130(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 143 _refine_ls_number_reflns 2382 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0416 _refine_ls_shift/su_max 0.077 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+6.3428P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.1067 _reflns_number_gt 1975 _reflns_number_total 2382 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file om060075xsi20060124_111107.cif _[local]_cod_data_source_block osco719 _[local]_cod_cif_authors_sg_H-M P21/n _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_hydrogen_treatment' value 'refu' changed to 'refU' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4075160 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Os1 Os 0.00776(3) 0.89151(4) 0.07339(2) 0.01649(17) Uani 1 1 d . C1 C -0.2127(8) 0.8345(12) 0.1002(6) 0.0273(18) Uani 1 1 d . C2 C -0.1304(8) 0.6933(12) 0.1136(6) 0.0248(17) Uani 1 1 d . C3 C -0.0197(9) 0.7251(11) 0.1898(6) 0.0261(18) Uani 1 1 d . C4 C -0.0325(9) 0.8846(10) 0.2239(6) 0.0249(17) Uani 1 1 d . C5 C -0.1542(9) 0.9511(11) 0.1663(6) 0.0257(17) Uani 1 1 d . C11 C -0.3473(10) 0.8510(16) 0.0321(8) 0.043(3) Uani 1 1 d . H111 H -0.3372 0.8058 -0.0278 0.068(12) Uiso 1 1 calc R H112 H -0.3711 0.9621 0.0241 0.068(12) Uiso 1 1 calc R H113 H -0.4194 0.7954 0.0565 0.068(12) Uiso 1 1 calc R C21 C -0.1637(11) 0.5393(13) 0.0619(8) 0.040(2) Uani 1 1 d . H211 H -0.0803 0.4784 0.0632 0.068(12) Uiso 1 1 calc R H212 H -0.2045 0.5613 -0.0024 0.068(12) Uiso 1 1 calc R H213 H -0.2279 0.4792 0.0917 0.068(12) Uiso 1 1 calc R C31 C 0.0836(11) 0.6002(13) 0.2348(8) 0.040(2) Uani 1 1 d . H311 H 0.1667 0.6524 0.2653 0.068(12) Uiso 1 1 calc R H312 H 0.1054 0.5292 0.1869 0.068(12) Uiso 1 1 calc R H313 H 0.0441 0.5402 0.2806 0.068(12) Uiso 1 1 calc R C41 C 0.0534(12) 0.9569(18) 0.3072(7) 0.048(3) Uani 1 1 d . H411 H 0.0594 1.0703 0.2980 0.068(12) Uiso 1 1 calc R H412 H 0.1446 0.9112 0.3160 0.068(12) Uiso 1 1 calc R H413 H 0.0122 0.9365 0.3620 0.068(12) Uiso 1 1 calc R C51 C -0.2128(13) 1.1135(13) 0.1829(9) 0.045(3) Uani 1 1 d . H511 H -0.1391 1.1904 0.1941 0.068(12) Uiso 1 1 calc R H512 H -0.2585 1.1087 0.2369 0.068(12) Uiso 1 1 calc R H513 H -0.2783 1.1446 0.1284 0.068(12) Uiso 1 1 calc R C6 C 0.1877(9) 0.8294(12) 0.0684(6) 0.0300(18) Uani 1 1 d . O6 O 0.2996(6) 0.7848(10) 0.0704(6) 0.047(2) Uani 1 1 d . C7 C 0.0571(8) 1.1301(10) 0.0688(6) 0.0207(16) Uani 1 1 d . O7 O 0.1009(7) 1.2304(8) 0.1230(5) 0.0344(14) Uani 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0161(2) 0.0168(2) 0.0166(2) 0.00185(12) 0.00272(12) 0.00137(12) C1 0.026(4) 0.031(5) 0.026(4) 0.013(4) 0.009(3) 0.004(4) C2 0.023(3) 0.032(5) 0.021(4) -0.001(4) 0.007(3) -0.002(3) C3 0.031(4) 0.026(5) 0.021(4) 0.009(3) 0.004(3) -0.001(3) C4 0.033(4) 0.018(4) 0.025(4) -0.001(3) 0.007(3) -0.001(3) C5 0.033(4) 0.024(4) 0.024(4) -0.001(4) 0.017(3) -0.004(4) C11 0.028(4) 0.057(7) 0.044(6) 0.010(5) 0.006(4) 0.000(5) C21 0.045(5) 0.022(5) 0.052(6) -0.005(5) 0.003(5) -0.010(4) C31 0.040(5) 0.031(5) 0.046(6) 0.017(5) -0.001(4) 0.005(4) C41 0.055(6) 0.061(8) 0.026(5) -0.009(5) 0.003(4) -0.016(6) C51 0.055(6) 0.033(6) 0.057(7) -0.002(5) 0.036(6) 0.011(5) C6 0.037(4) 0.023(4) 0.031(4) 0.005(4) 0.008(3) -0.005(4) O6 0.019(3) 0.055(5) 0.068(5) 0.015(4) 0.008(3) 0.018(3) C7 0.021(3) 0.020(4) 0.023(4) 0.006(3) 0.008(3) 0.002(3) O7 0.046(4) 0.025(3) 0.029(3) -0.008(3) -0.003(3) -0.009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -4.9801 6.2216 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 _geom_angle_publ_flag C6 Os1 C7 94.1(4) . 3_575 y C6 Os1 C7 92.3(4) . . y C7 Os1 C7 95.1(3) 3_575 . y C6 Os1 C3 95.3(4) . . ? C7 Os1 C3 129.8(3) 3_575 . ? C7 Os1 C3 133.6(3) . . ? C6 Os1 C4 110.6(4) . . ? C7 Os1 C4 151.5(3) 3_575 . ? C7 Os1 C4 97.8(3) . . ? C3 Os1 C4 37.2(3) . . ? C6 Os1 C2 114.6(4) . . ? C7 Os1 C2 95.3(3) 3_575 . ? C7 Os1 C2 150.2(3) . . ? C3 Os1 C2 37.0(3) . . ? C4 Os1 C2 62.0(3) . . ? C6 Os1 C5 147.2(4) . . ? C7 Os1 C5 118.3(3) 3_575 . ? C7 Os1 C5 89.9(3) . . ? C3 Os1 C5 60.9(3) . . ? C4 Os1 C5 36.8(3) . . ? C2 Os1 C5 60.7(3) . . ? C6 Os1 C1 150.8(4) . . ? C7 Os1 C1 90.5(3) 3_575 . ? C7 Os1 C1 115.9(3) . . ? C3 Os1 C1 60.6(3) . . ? C4 Os1 C1 61.0(3) . . ? C2 Os1 C1 36.2(3) . . ? C5 Os1 C1 35.7(3) . . ? C6 Os1 Os1 94.8(3) . 3_575 y C7 Os1 Os1 47.8(2) 3_575 3_575 ? C7 Os1 Os1 47.3(2) . 3_575 y C3 Os1 Os1 169.8(2) . 3_575 ? C4 Os1 Os1 138.5(2) . 3_575 ? C2 Os1 Os1 135.5(2) . 3_575 ? C5 Os1 Os1 110.4(2) . 3_575 ? C1 Os1 Os1 109.4(2) . 3_575 ? C5 C1 C2 109.0(8) . . ? C5 C1 C11 125.7(9) . . ? C2 C1 C11 125.1(9) . . ? C5 C1 Os1 71.7(4) . . ? C2 C1 Os1 70.7(4) . . ? C11 C1 Os1 127.7(6) . . ? C1 C2 C3 106.7(8) . . ? C1 C2 C21 125.2(8) . . ? C3 C2 C21 127.9(9) . . ? C1 C2 Os1 73.1(5) . . ? C3 C2 Os1 69.7(5) . . ? C21 C2 Os1 126.2(6) . . ? C2 C3 C4 109.6(8) . . ? C2 C3 C31 124.2(9) . . ? C4 C3 C31 125.8(9) . . ? C2 C3 Os1 73.3(5) . . ? C4 C3 Os1 72.8(5) . . ? C31 C3 Os1 126.2(6) . . ? C3 C4 C5 105.9(8) . . ? C3 C4 C41 126.1(10) . . ? C5 C4 C41 127.7(9) . . ? C3 C4 Os1 70.0(5) . . ? C5 C4 Os1 72.7(5) . . ? C41 C4 Os1 126.8(6) . . ? C1 C5 C4 108.7(8) . . ? C1 C5 C51 127.3(9) . . ? C4 C5 C51 123.7(9) . . ? C1 C5 Os1 72.6(4) . . ? C4 C5 Os1 70.4(4) . . ? C51 C5 Os1 127.4(6) . . ? C1 C11 H111 109.5 . . ? C1 C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? C1 C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? C2 C21 H211 109.5 . . ? C2 C21 H212 109.5 . . ? H211 C21 H212 109.5 . . ? C2 C21 H213 109.5 . . ? H211 C21 H213 109.5 . . ? H212 C21 H213 109.5 . . ? C3 C31 H311 109.5 . . ? C3 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C3 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C4 C41 H411 109.5 . . ? C4 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? C4 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? C5 C51 H511 109.5 . . ? C5 C51 H512 109.5 . . ? H511 C51 H512 109.5 . . ? C5 C51 H513 109.5 . . ? H511 C51 H513 109.5 . . ? H512 C51 H513 109.5 . . ? O6 C6 Os1 175.6(9) . . y O7 C7 Os1 138.0(7) . 3_575 y O7 C7 Os1 137.0(7) . . y Os1 C7 Os1 84.9(3) 3_575 . y loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C6 1.850(9) . y Os1 C7 2.041(8) 3_575 y Os1 C7 2.056(8) . y Os1 C3 2.228(8) . ? Os1 C4 2.265(8) . ? Os1 C2 2.275(9) . ? Os1 C5 2.295(7) . ? Os1 C1 2.307(8) . ? Os1 Os1 2.7664(7) 3_575 y C1 C5 1.412(14) . ? C1 C2 1.424(13) . ? C1 C11 1.508(13) . ? C2 C3 1.428(12) . ? C2 C21 1.494(13) . ? C3 C4 1.433(12) . ? C3 C31 1.519(13) . ? C4 C5 1.441(13) . ? C4 C41 1.471(13) . ? C5 C51 1.508(13) . ? C11 H111 0.9600 . ? C11 H112 0.9600 . ? C11 H113 0.9600 . ? C21 H211 0.9600 . ? C21 H212 0.9600 . ? C21 H213 0.9600 . ? C31 H311 0.9600 . ? C31 H312 0.9600 . ? C31 H313 0.9600 . ? C41 H411 0.9600 . ? C41 H412 0.9600 . ? C41 H413 0.9600 . ? C51 H511 0.9600 . ? C51 H512 0.9600 . ? C51 H513 0.9600 . ? C6 O6 1.153(11) . y C7 O7 1.175(11) . y C7 Os1 2.041(8) 3_575 ? _journal_paper_doi 10.1021/om060075x