#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/07/1100761.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_1100761 loop_ _publ_author_name 'Sergey M. Dibrov' 'Bin Deng' 'Donald E. Ellis' 'James A. Ibers' _publ_contact_author_name 'James A. Ibers' _publ_section_title ; Synthesis and Structural Characterization of Some Selenoruthenates and Telluroruthenates ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3441 _journal_page_last 3448 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C20 H20 Ru4 Se6' _chemical_formula_weight 1138.40 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 110.628(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.401(3) _cell_length_b 13.607(3) _cell_length_c 14.801(3) _cell_measurement_reflns_used 5839 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 28.94 _cell_measurement_theta_min 2.31 _cell_volume 2337.4(9) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.930 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_device_type 'Bruker 1000-CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13716 _diffrn_reflns_theta_full 28.94 _diffrn_reflns_theta_max 28.94 _diffrn_reflns_theta_min 2.31 _exptl_absorpt_coefficient_mu 11.886 _exptl_absorpt_correction_T_max 0.68343 _exptl_absorpt_correction_T_min 0.13242 _exptl_absorpt_correction_type numerical _exptl_crystal_colour brown _exptl_crystal_density_diffrn 3.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.176 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.038 _refine_diff_density_max 1.325 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.259 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2878 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.116 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0347 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+13.1919P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.0860 _reflns_number_gt 2237 _reflns_number_total 2878 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic0483646si20041124_025321_3.cif _[local]_cod_data_source_block Ru4Se6 _cod_original_cell_volume 2337.5(8) _cod_database_code 1100761 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.99668(4) 0.21122(4) 0.61636(3) 0.01353(12) Uani 1 1 d . . . Ru2 Ru 1.17818(4) 0.08056(4) 0.71171(3) 0.01555(13) Uani 1 1 d . . . Se1 Se 0.87219(5) 0.22395(4) 0.71571(4) 0.01384(14) Uani 1 1 d . . . Se2 Se 0.98380(5) 0.03600(5) 0.60385(4) 0.01773(15) Uani 1 1 d . . . Se3 Se 1.14903(6) -0.03018(5) 0.83160(5) 0.02213(16) Uani 1 1 d . . . C1 C 0.9802(6) 0.3646(5) 0.5611(4) 0.0204(14) Uani 1 1 d . . . H1 H 0.9819 0.4199 0.6007 0.024 Uiso 1 1 calc R . . C2 C 0.8808(6) 0.3124(5) 0.5046(4) 0.0229(14) Uani 1 1 d . . . H2 H 0.8039 0.3258 0.5004 0.027 Uiso 1 1 calc R . . C3 C 0.9158(6) 0.2366(5) 0.4554(4) 0.0197(13) Uani 1 1 d . . . H3 H 0.8662 0.1909 0.4118 0.024 Uiso 1 1 calc R . . C4 C 1.0377(6) 0.2405(5) 0.4823(4) 0.0232(14) Uani 1 1 d . . . H4 H 1.0840 0.1979 0.4604 0.028 Uiso 1 1 calc R . . C5 C 1.0774(6) 0.3198(5) 0.5480(4) 0.0241(15) Uani 1 1 d . . . H5 H 1.1553 0.3395 0.5782 0.029 Uiso 1 1 calc R . . C6 C 1.3370(6) 0.1563(5) 0.7117(6) 0.0291(16) Uani 1 1 d . . . H6 H 1.3521 0.2234 0.7297 0.035 Uiso 1 1 calc R . . C7 C 1.2820(6) 0.1214(6) 0.6175(5) 0.0339(18) Uani 1 1 d . . . H7 H 1.2540 0.1604 0.5607 0.041 Uiso 1 1 calc R . . C8 C 1.2756(6) 0.0181(6) 0.6218(5) 0.0314(17) Uani 1 1 d . . . H8 H 1.2427 -0.0245 0.5683 0.038 Uiso 1 1 calc R . . C9 C 1.3263(6) -0.0108(5) 0.7187(5) 0.0265(15) Uani 1 1 d . . . H9 H 1.3329 -0.0762 0.7424 0.032 Uiso 1 1 calc R . . C10 C 1.3660(6) 0.0757(5) 0.7752(5) 0.0250(15) Uani 1 1 d . . . H10 H 1.4049 0.0782 0.8431 0.030 Uiso 1 1 calc R . . 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 Ru1 0.0135(2) 0.0182(3) 0.0098(2) 0.00076(17) 0.00507(18) -0.00099(18) Ru2 0.0158(3) 0.0189(3) 0.0146(2) 0.00028(19) 0.00853(19) 0.0019(2) Se1 0.0133(3) 0.0176(3) 0.0112(3) 0.0007(2) 0.0051(2) 0.0009(2) Se2 0.0200(3) 0.0203(3) 0.0159(3) -0.0044(2) 0.0100(2) -0.0038(2) Se3 0.0263(4) 0.0221(3) 0.0236(3) 0.0073(3) 0.0157(3) 0.0089(3) C1 0.030(4) 0.016(3) 0.018(3) 0.003(2) 0.011(3) -0.001(3) C2 0.021(3) 0.028(4) 0.018(3) 0.014(3) 0.005(3) 0.004(3) C3 0.028(4) 0.022(3) 0.008(3) 0.002(2) 0.006(2) -0.008(3) C4 0.028(4) 0.031(4) 0.015(3) 0.009(3) 0.013(3) 0.003(3) C5 0.025(4) 0.031(4) 0.018(3) -0.001(3) 0.010(3) -0.013(3) C6 0.022(4) 0.029(4) 0.048(4) 0.007(3) 0.026(3) 0.007(3) C7 0.027(4) 0.056(5) 0.029(4) 0.019(4) 0.022(3) 0.010(4) C8 0.022(4) 0.048(5) 0.027(4) -0.011(3) 0.012(3) 0.006(3) C9 0.021(3) 0.032(4) 0.032(4) 0.002(3) 0.016(3) 0.010(3) C10 0.016(3) 0.038(4) 0.023(3) -0.007(3) 0.010(3) 0.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 C5 Ru1 C1 37.4(2) . . ? C5 Ru1 C2 61.9(3) . . ? C1 Ru1 C2 36.9(2) . . ? C5 Ru1 C4 37.0(2) . . ? C1 Ru1 C4 61.9(2) . . ? C2 Ru1 C4 61.7(2) . . ? C5 Ru1 C3 61.4(2) . . ? C1 Ru1 C3 61.3(2) . . ? C2 Ru1 C3 36.7(2) . . ? C4 Ru1 C3 36.7(2) . . ? C5 Ru1 Se2 131.08(18) . . ? C1 Ru1 Se2 155.71(16) . . ? C2 Ru1 Se2 123.18(18) . . ? C4 Ru1 Se2 97.92(18) . . ? C3 Ru1 Se2 94.47(16) . . ? C5 Ru1 Se1 99.83(17) . 2_756 ? C1 Ru1 Se1 104.42(17) . 2_756 ? C2 Ru1 Se1 136.81(18) . 2_756 ? C4 Ru1 Se1 127.33(18) . 2_756 ? C3 Ru1 Se1 161.26(16) . 2_756 ? Se2 Ru1 Se1 98.70(3) . 2_756 ? C5 Ru1 Se1 134.23(19) . . ? C1 Ru1 Se1 99.01(17) . . ? C2 Ru1 Se1 91.33(18) . . ? C4 Ru1 Se1 152.86(18) . . ? C3 Ru1 Se1 118.37(17) . . ? Se2 Ru1 Se1 94.40(3) . . ? Se1 Ru1 Se1 73.95(3) 2_756 . ? C5 Ru1 Ru2 103.83(19) . . ? C1 Ru1 Ru2 136.72(17) . . ? C2 Ru1 Ru2 161.15(18) . . ? C4 Ru1 Ru2 99.44(18) . . ? C3 Ru1 Ru2 127.00(17) . . ? Se2 Ru1 Ru2 55.33(2) . . ? Se1 Ru1 Ru2 53.88(2) 2_756 . ? Se1 Ru1 Ru2 107.46(3) . . ? C10 Ru2 C9 38.1(3) . . ? C10 Ru2 C6 37.2(3) . . ? C9 Ru2 C6 62.3(3) . . ? C10 Ru2 C8 62.0(3) . . ? C9 Ru2 C8 36.8(3) . . ? C6 Ru2 C8 61.1(3) . . ? C10 Ru2 C7 61.5(3) . . ? C9 Ru2 C7 61.4(3) . . ? C6 Ru2 C7 36.3(3) . . ? C8 Ru2 C7 36.2(3) . . ? C10 Ru2 Se1 103.73(18) . 2_756 ? C9 Ru2 Se1 141.47(19) . 2_756 ? C6 Ru2 Se1 89.60(19) . 2_756 ? C8 Ru2 Se1 147.5(2) . 2_756 ? C7 Ru2 Se1 111.5(2) . 2_756 ? C10 Ru2 Se3 94.41(19) . . ? C9 Ru2 Se3 87.25(19) . . ? C6 Ru2 Se3 129.94(19) . . ? C8 Ru2 Se3 116.3(2) . . ? C7 Ru2 Se3 148.6(2) . . ? Se1 Ru2 Se3 92.72(3) 2_756 . ? C10 Ru2 Se2 157.98(17) . . ? C9 Ru2 Se2 120.4(2) . . ? C6 Ru2 Se2 141.5(2) . . ? C8 Ru2 Se2 97.52(19) . . ? C7 Ru2 Se2 107.5(2) . . ? Se1 Ru2 Se2 98.07(3) 2_756 . ? Se3 Ru2 Se2 87.56(3) . . ? C10 Ru2 Ru1 140.8(2) . . ? C9 Ru2 Ru1 152.65(18) . . ? C6 Ru2 Ru1 104.95(18) . . ? C8 Ru2 Ru1 116.1(2) . . ? C7 Ru2 Ru1 93.64(19) . . ? Se1 Ru2 Ru1 55.10(2) 2_756 . ? Se3 Ru2 Ru1 117.00(3) . . ? Se2 Ru2 Ru1 53.35(2) . . ? Ru2 Se1 Ru1 71.01(2) 2_756 2_756 ? Ru2 Se1 Ru1 121.28(3) 2_756 . ? Ru1 Se1 Ru1 105.46(3) 2_756 . ? Se3 Se2 Ru1 112.76(3) 2_756 . ? Se3 Se2 Ru2 119.87(3) 2_756 . ? Ru1 Se2 Ru2 71.32(2) . . ? Se2 Se3 Ru2 111.19(3) 2_756 . ? C2 C1 C5 108.0(6) . . ? C2 C1 Ru1 72.2(4) . . ? C5 C1 Ru1 71.0(4) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Ru1 C1 H1 122.4 . . ? C1 C2 C3 107.9(6) . . ? C1 C2 Ru1 70.9(3) . . ? C3 C2 Ru1 72.5(3) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Ru1 C2 H2 122.3 . . ? C2 C3 C4 108.5(6) . . ? C2 C3 Ru1 70.9(3) . . ? C4 C3 Ru1 71.2(3) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Ru1 C3 H3 123.8 . . ? C5 C4 C3 107.3(6) . . ? C5 C4 Ru1 70.2(3) . . ? C3 C4 Ru1 72.1(3) . . ? C5 C4 H4 126.3 . . ? C3 C4 H4 126.3 . . ? Ru1 C4 H4 123.0 . . ? C4 C5 C1 108.3(6) . . ? C4 C5 Ru1 72.7(4) . . ? C1 C5 Ru1 71.6(4) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Ru1 C5 H5 121.5 . . ? C7 C6 C10 108.6(7) . . ? C7 C6 Ru2 73.9(4) . . ? C10 C6 Ru2 69.9(4) . . ? C7 C6 H6 125.7 . . ? C10 C6 H6 125.7 . . ? Ru2 C6 H6 122.2 . . ? C6 C7 C8 108.0(6) . . ? C6 C7 Ru2 69.8(4) . . ? C8 C7 Ru2 71.1(4) . . ? C6 C7 H7 126.0 . . ? C8 C7 H7 126.0 . . ? Ru2 C7 H7 124.6 . . ? C9 C8 C7 108.3(7) . . ? C9 C8 Ru2 69.1(4) . . ? C7 C8 Ru2 72.6(4) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Ru2 C8 H8 124.0 . . ? C8 C9 C10 107.8(7) . . ? C8 C9 Ru2 74.2(4) . . ? C10 C9 Ru2 70.7(4) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Ru2 C9 H9 120.8 . . ? C6 C10 C9 107.4(6) . . ? C6 C10 Ru2 72.9(4) . . ? C9 C10 Ru2 71.2(4) . . ? C6 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Ru2 C10 H10 121.4 . . ? 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 Ru1 C5 2.218(6) . ? Ru1 C1 2.225(6) . ? Ru1 C2 2.241(6) . ? Ru1 C4 2.250(6) . ? Ru1 C3 2.262(6) . ? Ru1 Se2 2.3924(9) . ? Ru1 Se1 2.4503(8) 2_756 ? Ru1 Se1 2.4851(8) . ? Ru1 Ru2 2.8250(8) . ? Ru2 C10 2.184(7) . ? Ru2 C9 2.190(7) . ? Ru2 C6 2.223(7) . ? Ru2 C8 2.256(7) . ? Ru2 C7 2.275(7) . ? Ru2 Se1 2.4133(8) 2_756 ? Ru2 Se3 2.4500(9) . ? Ru2 Se2 2.4526(9) . ? Se1 Ru2 2.4133(8) 2_756 ? Se1 Ru1 2.4503(8) 2_756 ? Se2 Se3 2.3550(9) 2_756 ? Se3 Se2 2.3550(9) 2_756 ? C1 C2 1.413(9) . ? C1 C5 1.423(10) . ? C1 H1 0.9500 . ? C2 C3 1.417(9) . ? C2 H2 0.9500 . ? C3 C4 1.422(9) . ? C3 H3 0.9500 . ? C4 C5 1.420(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.403(11) . ? C6 C10 1.406(10) . ? C6 H6 0.9500 . ? C7 C8 1.409(11) . ? C7 H7 0.9500 . ? C8 C9 1.404(10) . ? C8 H8 0.9500 . ? C9 C10 1.427(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ?