#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/35/2003528.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003528 loop_ _publ_author_name 'Capparelli, M. V.' 'De Sanctis, Y.' 'Arce, A. J.' _publ_section_title ;Hexacarbonyl-1\k^4^C,2\k^2^C-[\m-1\kC^6^:2(\h^5^)-6-methylfulvene]diruthenium(Ru---Ru), [Ru~2~(C~5~H~4~CHCH~3~)(CO)~6~] ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1118 _journal_page_last 1120 _journal_paper_doi 10.1107/S0108270194012928 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C13 H8 O6 Ru2' _chemical_formula_weight 462.34 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 103.23(1) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.256(2) _cell_length_b 8.644(3) _cell_length_c 13.484(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295(1) _cell_measurement_theta_max 38.4 _cell_measurement_theta_min 32.4 _cell_volume 1504.1(6) _diffrn_ambient_temperature 295.0(10) _diffrn_measurement_device AFC7S _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 3848 _diffrn_reflns_theta_max 27.5 _diffrn_standards_decay_% -8.25 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.030 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.042 _exptl_crystal_description prism _exptl_crystal_F_000 888.00 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.67 _refine_diff_density_min -0.64 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.962 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 198 _refine_ls_number_reflns 2061 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0368 _refine_ls_shift/esd_max 0.0005 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_obs 0.0367 _reflns_number_observed 2061 _reflns_number_total 3696 _reflns_observed_criterion '[I > 2\s(I)]' _cod_data_source_file bk1081.cif _cod_data_source_block Ru2 _cod_original_cell_volume 1504.0(7) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2003528 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' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ru(1) 0.0346(3) 0.0053(3) 0.0115(3) 0.0488(4) -0.0034(3) 0.0456(3) Ru(2) 0.0489(4) 0.0061(3) 0.0174(3) 0.0417(3) 0.0017(3) 0.0370(3) O(11) 0.074(5) 0.010(4) 0.050(4) 0.110(6) -0.041(5) 0.132(6) O(12) 0.083(5) 0.004(5) -0.035(5) 0.167(8) -0.018(6) 0.100(6) O(13) 0.064(4) -0.007(4) -0.002(3) 0.102(5) -0.001(4) 0.067(4) O(14) 0.082(5) -0.001(3) 0.036(4) 0.055(4) -0.003(3) 0.093(5) O(21) 0.131(6) -0.024(4) 0.002(4) 0.069(4) -0.010(4) 0.070(4) O(22) 0.067(4) 0.016(3) 0.017(3) 0.068(4) 0.021(3) 0.070(4) C(1) 0.061(5) -0.003(4) 0.020(4) 0.034(4) 0.010(3) 0.046(5) C(2) 0.076(6) 0.007(4) 0.009(4) 0.060(5) 0.008(4) 0.036(4) C(3) 0.097(7) 0.004(6) 0.038(5) 0.072(6) 0.006(5) 0.047(5) C(4) 0.071(6) 0.012(5) 0.046(5) 0.078(6) 0.024(5) 0.077(6) C(5) 0.062(5) -0.009(4) 0.024(4) 0.047(4) 0.002(4) 0.047(4) C(6) 0.058(5) 0.009(4) 0.015(4) 0.051(5) -0.005(4) 0.053(5) C(7) 0.117(9) 0.005(5) 0.037(6) 0.047(5) -0.007(5) 0.077(6) C(11) 0.061(6) 0.009(5) 0.027(5) 0.058(5) -0.011(5) 0.082(6) C(12) 0.055(5) -0.004(5) -0.004(5) 0.089(7) -0.006(6) 0.064(6) C(13) 0.044(4) -0.004(4) 0.015(4) 0.062(5) -0.006(4) 0.052(5) C(14) 0.040(4) 0.001(4) 0.020(4) 0.051(5) -0.006(4) 0.065(5) C(21) 0.086(7) 0.006(5) 0.009(4) 0.051(5) 0.005(4) 0.040(5) C(22) 0.046(5) 0.004(4) 0.028(4) 0.042(4) 0.002(4) 0.055(5) 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 Ru(1) 0.18259(5) 0.01135(7) -0.11478(4) 0.0426(2) Uani ? Ru(2) 0.32005(5) -0.11145(7) -0.22340(4) 0.0413(2) Uani ? O(11) 0.0543(5) 0.1981(8) 0.0019(5) 0.101(3) Uani ? O(12) 0.0133(6) -0.0323(10) -0.3099(6) 0.126(3) Uani ? O(13) 0.3751(5) 0.0444(7) 0.0590(4) 0.080(2) Uani ? O(14) 0.1528(5) -0.3192(7) -0.0403(5) 0.074(2) Uani ? O(21) 0.1845(6) -0.3778(7) -0.3179(5) 0.093(3) Uani ? O(22) 0.4429(4) -0.3056(6) -0.0524(4) 0.068(2) Uani ? C(1) 0.2999(6) 0.1464(8) -0.2432(5) 0.046(2) Uani ? C(2) 0.2731(7) 0.0726(9) -0.3396(6) 0.058(3) Uani ? C(3) 0.3623(8) -0.003(1) -0.3585(6) 0.068(3) Uani ? C(4) 0.4449(7) 0.020(1) -0.2742(7) 0.070(3) Uani ? C(5) 0.4082(6) 0.1116(9) -0.2013(5) 0.050(2) Uani ? C(6) 0.2287(6) 0.2216(9) -0.1899(6) 0.053(3) Uani ? C(7) 0.2752(8) 0.3528(9) -0.1197(7) 0.078(3) Uani ? C(11) 0.1010(7) 0.1309(10) -0.0448(7) 0.066(3) Uani ? C(12) 0.0758(7) -0.018(1) -0.2389(7) 0.072(3) Uani ? C(13) 0.3044(6) 0.0346(9) -0.0061(6) 0.052(3) Uani ? C(14) 0.1619(6) -0.1992(9) -0.0686(6) 0.051(3) Uani ? C(21) 0.2368(7) -0.2774(9) -0.2796(6) 0.060(3) Uani ? C(22) 0.3953(6) -0.2336(8) -0.1166(6) 0.045(2) Uani ? H(2) 0.2057 0.0735 -0.3848 0.05(2) Uiso calc H(3) 0.3653 -0.0601 -0.4188 0.07(2) Uiso calc H(4) 0.5142 -0.0184 -0.2666 0.06(2) Uiso calc H(5) 0.4483 0.1442 -0.1360 0.05(2) Uiso calc H(6) 0.1697 0.2594 -0.2391 0.05(2) Uiso calc H(71) 0.2935 0.4361 -0.1593 0.12(1) Uiso calc H(72) 0.3359 0.3168 -0.0721 0.242(8) Uiso calc H(73) 0.2253 0.3888 -0.0833 0.17(1) Uiso calc loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'International Tables for X-ray Crystallography (1974, Vol. IV)' 0.003 0.0 H 'International Tables for X-ray Crystallography (1974, Vol. IV)' 0.000 0.0 O 'International Tables for X-ray Crystallography (1974, Vol. IV)' 0.011 0.0 Ru 'International Tables for X-ray Crystallography (1974, Vol. IV)' -1.259 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 1 -1 0 1 -1 -1 1 -1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Ru(2) Ru(1) C(6) 78.0(2) yes Ru(2) Ru(1) C(11) 169.2(3) yes Ru(2) Ru(1) C(12) 86.2(3) yes Ru(2) Ru(1) C(13) 84.5(2) yes Ru(2) Ru(1) C(14) 88.2(2) yes C(6) Ru(1) C(11) 91.7(3) yes C(6) Ru(1) C(12) 86.3(3) yes C(6) Ru(1) C(13) 89.5(3) yes C(6) Ru(1) C(14) 166.2(3) yes C(11) Ru(1) C(12) 96.5(4) yes C(11) Ru(1) C(13) 92.2(3) yes C(11) Ru(1) C(14) 102.1(3) yes C(12) Ru(1) C(13) 170.4(3) yes C(12) Ru(1) C(14) 91.5(4) yes C(13) Ru(1) C(14) 90.5(3) yes Ru(1) Ru(2) C(1) 67.2(2) yes Ru(1) Ru(2) C(2) 89.2(2) no Ru(1) Ru(2) C(3) 125.7(2) no Ru(1) Ru(2) C(4) 125.7(2) no Ru(1) Ru(2) C(5) 89.2(2) no Ru(1) Ru(2) C(21) 96.3(3) yes Ru(1) Ru(2) C(22) 96.2(2) yes C(1) Ru(2) C(2) 36.9(2) no C(1) Ru(2) C(3) 62.1(3) no C(1) Ru(2) C(4) 62.4(3) no C(1) Ru(2) C(5) 37.6(3) no C(1) Ru(2) C(21) 132.1(3) no C(1) Ru(2) C(22) 132.4(3) no C(2) Ru(2) C(3) 37.3(3) no C(2) Ru(2) C(4) 61.8(3) no C(2) Ru(2) C(5) 62.0(3) no C(2) Ru(2) C(21) 102.8(3) no C(2) Ru(2) C(22) 163.4(3) no C(3) Ru(2) C(4) 36.5(3) no C(3) Ru(2) C(5) 61.7(3) no C(3) Ru(2) C(21) 103.2(3) no C(3) Ru(2) C(22) 132.3(3) no C(4) Ru(2) C(5) 37.2(3) no C(4) Ru(2) C(21) 132.6(3) no C(4) Ru(2) C(22) 102.7(3) no C(5) Ru(2) C(21) 163.8(3) no C(5) Ru(2) C(22) 102.3(3) no C(21) Ru(2) C(22) 92.3(3) yes Ru(2) C(1) C(2) 70.2(4) no Ru(2) C(1) C(5) 70.6(4) no Ru(2) C(1) C(6) 116.9(5) yes C(2) C(1) C(5) 106.4(7) no C(2) C(1) C(6) 126.5(7) no C(5) C(1) C(6) 126.4(7) no Ru(2) C(2) C(1) 72.8(4) no Ru(2) C(2) C(3) 71.8(4) no C(1) C(2) C(3) 109.0(7) no Ru(2) C(3) C(2) 70.9(4) no Ru(2) C(3) C(4) 72.2(4) no C(2) C(3) C(4) 108.4(7) no Ru(2) C(4) C(3) 71.4(5) no Ru(2) C(4) C(5) 71.3(4) no C(3) C(4) C(5) 108.1(8) no Ru(2) C(5) C(1) 71.7(4) no Ru(2) C(5) C(4) 71.5(5) no C(1) C(5) C(4) 108.0(7) no Ru(1) C(6) C(1) 97.8(4) yes Ru(1) C(6) C(7) 116.1(5) no C(1) C(6) C(7) 115.1(7) no Ru(1) C(11) O(11) 176.3(9) no Ru(1) C(12) O(12) 178.7(9) no Ru(1) C(13) O(13) 178.0(7) no Ru(1) C(14) O(14) 177.9(8) no Ru(2) C(21) O(21) 177.5(7) no Ru(2) C(22) O(22) 178.3(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ru(1) Ru(2) 2.7954(8) yes Ru(1) C(6) 2.232(8) yes Ru(1) C(11) 1.896(8) no Ru(1) C(12) 1.945(9) no Ru(1) C(13) 1.926(8) no Ru(1) C(14) 1.963(8) no Ru(2) C(1) 2.253(7) yes Ru(2) C(2) 2.219(7) yes Ru(2) C(3) 2.231(7) yes Ru(2) C(4) 2.241(8) yes Ru(2) C(5) 2.239(7) yes Ru(2) C(21) 1.862(9) no Ru(2) C(22) 1.878(8) no O(11) C(11) 1.139(9) no O(12) C(12) 1.120(9) no O(13) C(13) 1.131(8) no O(14) C(14) 1.121(8) no O(21) C(21) 1.157(9) no O(22) C(22) 1.134(8) no C(1) C(2) 1.417(9) yes C(1) C(5) 1.449(9) yes C(1) C(6) 1.464(9) yes C(2) C(3) 1.420(10) yes C(3) C(4) 1.400(10) yes C(4) C(5) 1.430(10) yes C(6) C(7) 1.520(10) no