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#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/01/7050196.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_7050196
loop_
_publ_author_name
'Bickley, Jamie'
'Bonar-Law, Richard'
'McGrath, Thomas'
'Singh, Nirmal'
'Steiner, Alexander'
_publ_section_title
;
 Dirhodium (ii) carboxylate complexes as building blocks. cis-Chelating
 dicarboxylic acids designed to bridge the dinuclear coreElectronic
 supplementary information (ESI) available: Tables S1 and S2. See
 http://www.rsc.org/suppdata/nj/b3/b310008a/
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              425
_journal_paper_doi               10.1039/b310008a
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C12 H12 Br2 O6'
_chemical_formula_weight         412.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.10(3)
_cell_angle_beta                 98.04(3)
_cell_angle_gamma                98.76(3)
_cell_formula_units_Z            2
_cell_length_a                   8.694(2)
_cell_length_b                   9.240(3)
_cell_length_c                   9.899(3)
_cell_measurement_temperature    213(2)
_cell_volume                     722.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4629
_diffrn_reflns_theta_full        24.27
_diffrn_reflns_theta_max         24.27
_diffrn_reflns_theta_min         2.24
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.634
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             404
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0988P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                1587
_reflns_number_total             2155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310008a.txt
_cod_data_source_block           tmcg4
_cod_original_cell_volume        722.0(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050196
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.0192(8) 0.6306(7) 0.2130(7) 0.0327(14) Uani 1 1 d . . .
H1 H 0.0498 0.5820 0.2786 0.039 Uiso 1 1 calc R . .
C2 C -0.1402(9) 0.6400(7) 0.1783(7) 0.0337(15) Uani 1 1 d . . .
C3 C -0.1860(9) 0.7081(7) 0.0764(7) 0.0349(15) Uani 1 1 d . . .
C4 C -0.0730(8) 0.7688(7) 0.0160(7) 0.0364(16) Uani 1 1 d . . .
H4 H -0.1031 0.8161 -0.0509 0.044 Uiso 1 1 calc R . .
C5 C 0.0819(9) 0.7622(7) 0.0505(7) 0.0346(15) Uani 1 1 d . . .
C6 C 0.1298(8) 0.6927(7) 0.1508(6) 0.0311(14) Uani 1 1 d . . .
C7 C 0.3505(10) 0.6292(9) 0.2815(8) 0.0468(18) Uani 1 1 d . . .
H7A H 0.4500 0.5993 0.2589 0.056 Uiso 1 1 calc R . .
H7B H 0.2758 0.5337 0.2720 0.056 Uiso 1 1 calc R . .
C8 C 0.3817(13) 0.7434(15) 0.4347(11) 0.081(3) Uani 1 1 d . B .
C9 C -0.2222(10) 0.5245(8) 0.3481(8) 0.0422(17) Uani 1 1 d . . .
H9A H -0.1487 0.4541 0.3197 0.051 Uiso 1 1 calc R . .
H9B H -0.3200 0.4609 0.3544 0.051 Uiso 1 1 calc R . .
C10 C -0.1492(9) 0.6472(8) 0.4980(8) 0.0431(18) Uani 1 1 d . A .
C11 C -0.030(4) 0.9214(19) 0.6377(18) 0.050(7) Uiso 0.49(6) 1 d P A 1
H11A H -0.0780 0.9244 0.7209 0.075 Uiso 0.49(6) 1 calc PR A 1
H11B H -0.0218 1.0222 0.6262 0.075 Uiso 0.49(6) 1 calc PR A 1
H11C H 0.0759 0.9003 0.6545 0.075 Uiso 0.49(6) 1 calc PR A 1
C11' C -0.105(5) 0.916(2) 0.647(2) 0.067(7) Uiso 0.51(6) 1 d P A 2
H11D H -0.1878 0.8898 0.6963 0.100 Uiso 0.51(6) 1 calc PR A 2
H11E H -0.1082 1.0163 0.6379 0.100 Uiso 0.51(6) 1 calc PR A 2
H11F H -0.0020 0.9217 0.7036 0.100 Uiso 0.51(6) 1 calc PR A 2
O1 O -0.2596(6) 0.5834(5) 0.2343(5) 0.0420(11) Uani 1 1 d . . .
O2 O -0.1170(8) 0.6133(7) 0.6033(6) 0.0633(17) Uani 1 1 d . . .
O3 O -0.1301(8) 0.7933(5) 0.5009(5) 0.0626(17) Uani 1 1 d . . .
O4 O 0.2856(6) 0.6918(6) 0.1770(5) 0.0438(12) Uani 1 1 d . . .
O5 O 0.4712(10) 0.7111(10) 0.5268(7) 0.093(2) Uani 1 1 d . . .
O6 O 0.3216(10) 0.8622(10) 0.4683(7) 0.091(2) Uani 1 1 d . . .
Br1 Br -0.39837(9) 0.72543(9) 0.03252(9) 0.0496(3) Uani 1 1 d . . .
Br2 Br 0.23542(9) 0.85579(9) -0.02906(8) 0.0492(3) Uani 1 1 d . . .
C12 C 0.375(4) 0.945(3) 0.629(3) 0.106(10) Uiso 0.49(2) 1 d P B 1
H12A H 0.3404 0.8746 0.6776 0.159 Uiso 0.49(2) 1 calc PR B 1
H12B H 0.3296 1.0374 0.6609 0.159 Uiso 0.49(2) 1 calc PR B 1
H12C H 0.4901 0.9766 0.6534 0.159 Uiso 0.49(2) 1 calc PR B 1
C12' C 0.509(3) 0.846(2) 0.678(2) 0.084(7) Uiso 0.51(2) 1 d P B 2
H12D H 0.5836 0.9347 0.6768 0.126 Uiso 0.51(2) 1 calc PR B 2
H12E H 0.5559 0.8099 0.7525 0.126 Uiso 0.51(2) 1 calc PR B 2
H12F H 0.4119 0.8784 0.7015 0.126 Uiso 0.51(2) 1 calc PR B 2
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'
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 C1 C2 119.6(6) . . ?
O1 C2 C1 124.6(6) . . ?
O1 C2 C3 115.5(6) . . ?
C1 C2 C3 119.8(6) . . ?
C4 C3 C2 119.1(7) . . ?
C4 C3 Br1 120.6(5) . . ?
C2 C3 Br1 120.1(5) . . ?
C5 C4 C3 121.4(6) . . ?
C4 C5 C6 120.3(6) . . ?
C4 C5 Br2 119.9(5) . . ?
C6 C5 Br2 119.7(6) . . ?
O4 C6 C1 124.8(6) . . ?
O4 C6 C5 115.6(6) . . ?
C1 C6 C5 119.6(7) . . ?
O4 C7 C8 112.4(8) . . ?
O6 C8 O5 123.3(10) . . ?
O6 C8 C7 121.5(10) . . ?
O5 C8 C7 115.1(12) . . ?
O1 C9 C10 115.6(5) . . ?
O2 C10 O3 124.7(7) . . ?
O2 C10 C9 122.1(6) . . ?
O3 C10 C9 113.2(6) . . ?
C2 O1 C9 119.4(6) . . ?
C10 O3 C11' 114.9(9) . . ?
C10 O3 C11 116.8(8) . . ?
C11' O3 C11 26.1(10) . . ?
C6 O4 C7 120.9(5) . . ?
C8 O5 C12' 110.5(13) . . ?
C8 O6 C12 106.2(14) . . ?
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
C1 C6 1.369(9) . ?
C1 C2 1.403(10) . ?
C2 O1 1.362(8) . ?
C2 C3 1.405(9) . ?
C3 C4 1.364(9) . ?
C3 Br1 1.881(7) . ?
C4 C5 1.358(10) . ?
C5 C6 1.406(9) . ?
C5 Br2 1.886(6) . ?
C6 O4 1.345(8) . ?
C7 O4 1.439(8) . ?
C7 C8 1.478(13) . ?
C8 O6 1.249(14) . ?
C8 O5 1.260(14) . ?
C9 O1 1.430(8) . ?
C9 C10 1.500(10) . ?
C10 O2 1.197(8) . ?
C10 O3 1.324(8) . ?
C11 O3 1.500(19) . ?
C11' O3 1.458(19) . ?
O5 C12' 1.54(2) . ?
O6 C12 1.47(3) . ?
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
_geom_torsion_publ_flag
C6 C1 C2 O1 -179.5(5) . . . . ?
C6 C1 C2 C3 2.1(9) . . . . ?
O1 C2 C3 C4 179.5(5) . . . . ?
C1 C2 C3 C4 -2.0(9) . . . . ?
O1 C2 C3 Br1 2.9(8) . . . . ?
C1 C2 C3 Br1 -178.6(4) . . . . ?
C2 C3 C4 C5 1.1(9) . . . . ?
Br1 C3 C4 C5 177.7(5) . . . . ?
C3 C4 C5 C6 -0.3(9) . . . . ?
C3 C4 C5 Br2 -177.2(5) . . . . ?
C2 C1 C6 O4 179.3(5) . . . . ?
C2 C1 C6 C5 -1.3(9) . . . . ?
C4 C5 C6 O4 179.8(6) . . . . ?
Br2 C5 C6 O4 -3.3(7) . . . . ?
C4 C5 C6 C1 0.4(9) . . . . ?
Br2 C5 C6 C1 177.3(5) . . . . ?
O4 C7 C8 O6 16.3(12) . . . . ?
O4 C7 C8 O5 -164.1(8) . . . . ?
O1 C9 C10 O2 177.7(7) . . . . ?
O1 C9 C10 O3 -0.3(10) . . . . ?
C1 C2 O1 C9 7.0(9) . . . . ?
C3 C2 O1 C9 -174.6(6) . . . . ?
C10 C9 O1 C2 75.0(8) . . . . ?
O2 C10 O3 C11' -15(2) . . . . ?
C9 C10 O3 C11' 162.7(19) . . . . ?
O2 C10 O3 C11 13.7(18) . . . . ?
C9 C10 O3 C11 -168.3(15) . . . . ?
C1 C6 O4 C7 -2.9(9) . . . . ?
C5 C6 O4 C7 177.7(6) . . . . ?
C8 C7 O4 C6 -81.2(9) . . . . ?
O6 C8 O5 C12' -6.4(15) . . . . ?
C7 C8 O5 C12' 174.1(11) . . . . ?
O5 C8 O6 C12 -1.1(17) . . . . ?
C7 C8 O6 C12 178.4(13) . . . . ?
