#------------------------------------------------------------------------------
#$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       'ω 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/[σ²(Fo²)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/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_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
