#------------------------------------------------------------------------------ #$Date: 2019-12-09 10:44:45 +0200 (Mon, 09 Dec 2019) $ #$Revision: 244952 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556466.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_1556466 loop_ _publ_author_name 'Delgado-Martinez, P.' 'Elvira-Bravo, A.' 'Gonzalez-Prieto, R.' 'Priego, J.L.' 'Jimenez-Aparicio, R.' 'Torres, M.R.' _publ_section_title ; Synthesis of Ru2Br(mu-O2CC6H4-R)4 (R = o-Me, m-Me, p-Me) Using Microwave Activation: Structural and Magnetic Properties ; _journal_name_full Inorganics _journal_page_first 524 _journal_page_last 536 _journal_paper_doi 10.3390/inorganics2030524 _journal_volume 2 _journal_year 2014 _chemical_formula_sum 'C32 H28 Br O8 Ru2' _chemical_formula_weight 822.59 _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 94.623(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 12.9939(7) _cell_length_b 10.1996(5) _cell_length_c 24.8297(16) _cell_measurement_reflns_used 1598 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.3390 _cell_measurement_theta_min 4.0300 _cell_volume 3280.0(3) _computing_cell_refinement ; 'Mon Mar 03 18:16:02 2014' ; _computing_data_collection ; 'Mon Mar 03 18:16:02 2014' ; _computing_data_reduction ; 'Mon Mar 03 18:16:02 2014' ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.3317 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Xcalibur, Atlas' _diffrn_measurement_method '\w 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 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 8036 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 3.43 _exptl_absorpt_coefficient_mu 2.186 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; 'Mon Mar 03 18:16:02 2014' ; _exptl_crystal_colour 'clear dark brown' _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1628 _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.0900 _exptl_crystal_size_min 0.0700 _refine_diff_density_max 0.700 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 195 _refine_ls_number_reflns 3217 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.997 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0406 _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.0851 _reflns_number_gt 2290 _reflns_number_total 3217 _reflns_threshold_expression >2sigma(I) _cod_data_source_file cif-compound_3.cif _cod_data_source_block aeb16 _cod_database_code 1556466 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -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 Br1 Br 0.7500 0.19466(6) 0.0000 0.0449(2) Uani 1 2 d S . . C1 C 0.3996(3) 0.2095(4) -0.03593(17) 0.0319(10) Uani 1 1 d . . . C2 C 0.3429(3) 0.3246(4) -0.05802(17) 0.0336(11) Uani 1 1 d . . . C3 C 0.3915(4) 0.4444(4) -0.06162(18) 0.0423(12) Uani 1 1 d . . . H3 H 0.4600 0.4540 -0.0482 0.051 Uiso 1 1 calc R . . C4 C 0.3384(4) 0.5502(5) -0.0852(2) 0.0562(15) Uani 1 1 d . . . H4 H 0.3711 0.6310 -0.0868 0.067 Uiso 1 1 calc R . . C5 C 0.2367(4) 0.5367(5) -0.1063(2) 0.0534(14) Uani 1 1 d . . . C6 C 0.1901(4) 0.4189(5) -0.1017(2) 0.0566(15) Uani 1 1 d . . . H6 H 0.1216 0.4096 -0.1150 0.068 Uiso 1 1 calc R . . C7 C 0.2409(4) 0.3116(5) -0.07785(19) 0.0460(13) Uani 1 1 d . . . H7 H 0.2068 0.2319 -0.0752 0.055 Uiso 1 1 calc R . . C8 C 0.1807(5) 0.6525(5) -0.1330(3) 0.089(2) Uani 1 1 d . . . H8A H 0.1461 0.6253 -0.1668 0.134 Uiso 1 1 calc R . . H8B H 0.2296 0.7202 -0.1394 0.134 Uiso 1 1 calc R . . H8C H 0.1310 0.6854 -0.1099 0.134 Uiso 1 1 calc R . . C9 C 0.4781(3) 0.0718(4) 0.10001(18) 0.0348(11) Uani 1 1 d . . . C10 C 0.4628(4) 0.1168(5) 0.15529(18) 0.0407(12) Uani 1 1 d . . . C11 C 0.5322(4) 0.2030(5) 0.1819(2) 0.0578(15) Uani 1 1 d . . . H11 H 0.5910 0.2290 0.1657 0.069 Uiso 1 1 calc R . . C12 C 0.5139(5) 0.2502(6) 0.2323(2) 0.0716(18) Uani 1 1 d . . . H12 H 0.5604 0.3091 0.2494 0.086 Uiso 1 1 calc R . . C13 C 0.4290(5) 0.2126(6) 0.2578(2) 0.0636(17) Uani 1 1 d . . . C14 C 0.3617(5) 0.1252(6) 0.2319(2) 0.0673(17) Uani 1 1 d . . . H14 H 0.3043 0.0975 0.2489 0.081 Uiso 1 1 calc R . . C15 C 0.3774(4) 0.0772(5) 0.1809(2) 0.0553(14) Uani 1 1 d . . . H15 H 0.3305 0.0185 0.1640 0.066 Uiso 1 1 calc R . . C16 C 0.4097(5) 0.2682(8) 0.3127(2) 0.102(3) Uani 1 1 d . . . H16A H 0.4723 0.2649 0.3359 0.153 Uiso 1 1 calc R . . H16B H 0.3574 0.2173 0.3282 0.153 Uiso 1 1 calc R . . H16C H 0.3870 0.3575 0.3086 0.153 Uiso 1 1 calc R . . O1 O 0.4967(2) 0.2179(3) -0.02513(12) 0.0366(7) Uani 1 1 d . . . O2 O 0.3494(2) 0.1044(3) -0.02878(12) 0.0352(7) Uani 1 1 d . . . O3 O 0.5575(2) 0.1110(3) 0.07813(11) 0.0379(7) Uani 1 1 d . . . O4 O 0.4103(2) -0.0020(3) 0.07616(11) 0.0362(7) Uani 1 1 d . . . Ru1 Ru 0.57591(3) 0.05730(3) 0.001175(14) 0.02965(13) 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 Br1 0.0235(3) 0.0335(4) 0.0786(5) 0.000 0.0093(3) 0.000 C1 0.031(3) 0.032(2) 0.033(3) 0.001(2) 0.006(2) 0.001(2) C2 0.031(3) 0.033(2) 0.037(3) 0.001(2) 0.003(2) 0.003(2) C3 0.037(3) 0.039(3) 0.051(3) 0.000(2) 0.003(2) 0.004(2) C4 0.062(4) 0.034(3) 0.072(4) 0.009(3) 0.000(3) 0.002(3) C5 0.059(4) 0.044(3) 0.057(3) 0.010(3) 0.000(3) 0.013(3) C6 0.040(3) 0.062(4) 0.064(4) 0.007(3) -0.014(3) 0.012(3) C7 0.042(3) 0.039(3) 0.057(3) 0.007(2) 0.005(3) 0.001(2) C8 0.091(5) 0.064(4) 0.107(5) 0.027(4) -0.019(4) 0.019(4) C9 0.030(3) 0.032(2) 0.043(3) 0.007(2) 0.005(2) 0.009(2) C10 0.040(3) 0.047(3) 0.036(3) 0.008(2) 0.008(2) 0.008(2) C11 0.046(3) 0.081(4) 0.047(3) -0.006(3) 0.012(3) -0.016(3) C12 0.071(5) 0.097(5) 0.047(4) -0.022(3) 0.006(3) -0.009(4) C13 0.060(4) 0.096(5) 0.035(3) -0.005(3) 0.005(3) 0.020(4) C14 0.059(4) 0.101(5) 0.045(3) 0.001(3) 0.020(3) -0.001(4) C15 0.050(3) 0.070(4) 0.047(3) 0.003(3) 0.011(3) -0.004(3) C16 0.099(6) 0.160(7) 0.046(4) -0.021(4) 0.007(4) 0.024(5) O1 0.0237(17) 0.0326(16) 0.054(2) 0.0070(14) 0.0044(15) 0.0000(14) O2 0.0256(16) 0.0296(15) 0.051(2) 0.0071(15) 0.0039(15) 0.0026(14) O3 0.0317(18) 0.0440(18) 0.0384(18) -0.0011(15) 0.0059(15) -0.0044(15) O4 0.0305(17) 0.0388(17) 0.0403(18) 0.0004(15) 0.0097(15) -0.0045(15) Ru1 0.0207(2) 0.0295(2) 0.0396(2) 0.00232(17) 0.00680(15) -0.00013(15) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 Ru1 Br1 Ru1 116.51(3) 2_655 . O1 C1 O2 122.6(4) . . O1 C1 C2 118.9(4) . . O2 C1 C2 118.5(4) . . C3 C2 C7 119.5(4) . . C3 C2 C1 120.9(4) . . C7 C2 C1 119.6(4) . . C2 C3 C4 120.1(4) . . C3 C4 C5 120.6(5) . . C6 C5 C4 118.3(5) . . C6 C5 C8 121.9(5) . . C4 C5 C8 119.8(5) . . C5 C6 C7 122.4(5) . . C6 C7 C2 119.1(5) . . O3 C9 O4 123.1(4) . . O3 C9 C10 118.3(4) . . O4 C9 C10 118.6(4) . . C15 C10 C11 118.8(5) . . C15 C10 C9 120.7(5) . . C11 C10 C9 120.5(5) . . C10 C11 C12 120.0(5) . . C13 C12 C11 121.7(6) . . C12 C13 C14 118.1(5) . . C12 C13 C16 120.6(6) . . C14 C13 C16 121.2(6) . . C13 C14 C15 121.5(6) . . C10 C15 C14 119.9(5) . . C1 O1 Ru1 119.1(3) . . C1 O2 Ru1 120.0(3) . 5_655 C9 O3 Ru1 118.8(3) . . C9 O4 Ru1 119.8(3) . 5_655 O2 Ru1 O1 178.01(12) 5_655 . O2 Ru1 O3 89.47(12) 5_655 . O1 Ru1 O3 89.41(12) . . O2 Ru1 O4 91.02(11) 5_655 5_655 O1 Ru1 O4 90.05(12) . 5_655 O3 Ru1 O4 178.25(12) . 5_655 O2 Ru1 Ru1 88.92(8) 5_655 5_655 O1 Ru1 Ru1 89.43(8) . 5_655 O3 Ru1 Ru1 89.74(9) . 5_655 O4 Ru1 Ru1 88.60(8) 5_655 5_655 O2 Ru1 Br1 92.77(8) 5_655 . O1 Ru1 Br1 88.92(8) . . O3 Ru1 Br1 91.88(8) . . O4 Ru1 Br1 89.77(8) 5_655 . Ru1 Ru1 Br1 177.67(2) 5_655 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Br1 Ru1 2.6630(5) 2_655 Br1 Ru1 2.6630(5) . C1 O1 1.271(5) . C1 O2 1.275(5) . C1 C2 1.469(6) . C2 C3 1.381(6) . C2 C7 1.383(6) . C3 C4 1.385(6) . C4 C5 1.388(7) . C5 C6 1.354(7) . C5 C8 1.513(7) . C6 C7 1.386(6) . C9 O3 1.270(5) . C9 O4 1.268(5) . C9 C10 1.476(6) . C10 C15 1.383(7) . C10 C11 1.388(7) . C11 C12 1.380(7) . C12 C13 1.370(8) . C13 C14 1.373(8) . C13 C16 1.515(7) . C14 C15 1.387(7) . O1 Ru1 2.016(3) . O2 Ru1 2.007(3) 5_655 O3 Ru1 2.020(3) . O4 Ru1 2.023(3) 5_655 Ru1 O2 2.007(3) 5_655 Ru1 O4 2.023(3) 5_655 Ru1 Ru1 2.2898(7) 5_655 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O1 C1 C2 C3 -7.0(7) . . . . O2 C1 C2 C3 173.6(4) . . . . O1 C1 C2 C7 169.9(4) . . . . O2 C1 C2 C7 -9.5(7) . . . . C7 C2 C3 C4 -0.3(7) . . . . C1 C2 C3 C4 176.6(5) . . . . C2 C3 C4 C5 -1.2(8) . . . . C3 C4 C5 C6 2.1(8) . . . . C3 C4 C5 C8 -178.5(5) . . . . C4 C5 C6 C7 -1.4(9) . . . . C8 C5 C6 C7 179.2(5) . . . . C5 C6 C7 C2 -0.1(8) . . . . C3 C2 C7 C6 1.0(7) . . . . C1 C2 C7 C6 -176.0(4) . . . . O3 C9 C10 C15 179.8(4) . . . . O4 C9 C10 C15 1.3(6) . . . . O3 C9 C10 C11 1.9(6) . . . . O4 C9 C10 C11 -176.7(4) . . . . C15 C10 C11 C12 -1.7(8) . . . . C9 C10 C11 C12 176.3(5) . . . . C10 C11 C12 C13 1.1(9) . . . . C11 C12 C13 C14 0.3(9) . . . . C11 C12 C13 C16 -178.7(6) . . . . C12 C13 C14 C15 -1.1(9) . . . . C16 C13 C14 C15 177.9(5) . . . . C11 C10 C15 C14 0.9(7) . . . . C9 C10 C15 C14 -177.0(5) . . . . C13 C14 C15 C10 0.5(8) . . . . O2 C1 O1 Ru1 2.8(6) . . . . C2 C1 O1 Ru1 -176.5(3) . . . . O1 C1 O2 Ru1 -1.5(6) . . . 5_655 C2 C1 O2 Ru1 177.8(3) . . . 5_655 O4 C9 O3 Ru1 1.4(5) . . . . C10 C9 O3 Ru1 -177.1(3) . . . . O3 C9 O4 Ru1 -2.1(5) . . . 5_655 C10 C9 O4 Ru1 176.4(3) . . . 5_655 C1 O1 Ru1 O2 -36(4) . . . 5_655 C1 O1 Ru1 O3 -92.1(3) . . . . C1 O1 Ru1 O4 86.2(3) . . . 5_655 C1 O1 Ru1 Ru1 -2.4(3) . . . 5_655 C1 O1 Ru1 Br1 176.0(3) . . . . C9 O3 Ru1 O2 -89.1(3) . . . 5_655 C9 O3 Ru1 O1 89.2(3) . . . . C9 O3 Ru1 O4 17(4) . . . 5_655 C9 O3 Ru1 Ru1 -0.2(3) . . . 5_655 C9 O3 Ru1 Br1 178.1(3) . . . . Ru1 Br1 Ru1 O2 20.29(8) 2_655 . . 5_655 Ru1 Br1 Ru1 O1 -160.77(9) 2_655 . . . Ru1 Br1 Ru1 O3 109.85(8) 2_655 . . . Ru1 Br1 Ru1 O4 -70.72(8) 2_655 . . 5_655 Ru1 Br1 Ru1 Ru1 -116.1(7) 2_655 . . 5_655