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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/01/7050197.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_7050197
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            'C14 H16 Br2 O6'
_chemical_formula_weight         440.09
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.541(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2340(13)
_cell_length_b                   7.4699(11)
_cell_length_c                   20.184(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1682.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2491
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.841
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.797
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.797
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0281
_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)+(0.0380P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                1722
_reflns_number_total             2491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310008a.txt
_cod_data_source_block           tmcg9
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7050197
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Br1 Br 0.40104(4) 0.27462(6) 0.22954(2) 0.04572(15) Uani 1 1 d . . .
Br2 Br -0.09439(4) 0.32019(6) 0.14583(2) 0.05229(15) Uani 1 1 d . . .
C1 C 0.2419(3) 0.2688(4) 0.25040(18) 0.0267(8) Uani 1 1 d . . .
C2 C 0.1497(3) 0.2934(5) 0.20053(18) 0.0322(9) Uani 1 1 d . . .
H2 H 0.1664 0.3144 0.1571 0.039 Uiso 1 1 calc R . .
C3 C 0.0317(3) 0.2871(5) 0.21446(18) 0.0300(9) Uani 1 1 d . . .
C4 C 0.0067(3) 0.2559(5) 0.27975(18) 0.0294(9) Uani 1 1 d . A .
C5 C 0.0994(3) 0.2314(5) 0.32906(18) 0.0337(9) Uani 1 1 d . . .
H5 H 0.0827 0.2097 0.3724 0.040 Uiso 1 1 calc R . .
C6 C 0.2188(3) 0.2383(4) 0.31568(19) 0.0294(9) Uani 1 1 d . . .
C7 C -0.1624(3) 0.3181(5) 0.3444(2) 0.0406(10) Uani 1 1 d . A .
C8 C -0.1107(4) 0.5003(5) 0.3635(2) 0.0546(13) Uani 1 1 d . . .
H8A H -0.0262 0.4893 0.3769 0.082 Uiso 1 1 calc R . .
H8B H -0.1491 0.5476 0.3999 0.082 Uiso 1 1 calc R . .
H8C H -0.1239 0.5796 0.3260 0.082 Uiso 1 1 calc R . .
C9 C -0.2965(4) 0.3288(6) 0.3190(3) 0.0634(14) Uani 1 1 d . . .
H9A H -0.3076 0.4036 0.2801 0.095 Uiso 1 1 calc R . .
H9B H -0.3394 0.3786 0.3532 0.095 Uiso 1 1 calc R . .
H9C H -0.3264 0.2109 0.3079 0.095 Uiso 1 1 calc R . .
C10 C -0.1515(4) 0.1897(5) 0.4024(2) 0.0421(11) Uani 1 1 d . . .
C11 C 0.3187(3) 0.2658(5) 0.42935(19) 0.0356(10) Uani 1 1 d . . .
C12 C 0.4504(4) 0.2435(7) 0.4562(2) 0.0568(13) Uani 1 1 d . . .
H12A H 0.4756 0.1236 0.4480 0.085 Uiso 1 1 calc R . .
H12B H 0.4605 0.2664 0.5033 0.085 Uiso 1 1 calc R . .
H12C H 0.4979 0.3267 0.4342 0.085 Uiso 1 1 calc R . .
C13 C 0.2780(4) 0.4569(5) 0.4353(2) 0.0529(12) Uani 1 1 d . . .
H13A H 0.3232 0.5332 0.4092 0.079 Uiso 1 1 calc R . .
H13B H 0.2904 0.4933 0.4812 0.079 Uiso 1 1 calc R . .
H13C H 0.1944 0.4659 0.4193 0.079 Uiso 1 1 calc R . .
C14 C 0.2474(3) 0.1349(5) 0.46786(18) 0.0333(9) Uani 1 1 d . . .
O1 O -0.1127(2) 0.2393(4) 0.28781(13) 0.0443(7) Uani 1 1 d . . .
O2 O -0.1519(10) 0.2393(8) 0.4625(4) 0.049(3) Uiso 0.53(2) 1 d P A 1
O2' O -0.2103(11) 0.2459(8) 0.4490(4) 0.042(3) Uiso 0.47(2) 1 d P A 2
O3 O -0.1189(3) 0.0307(4) 0.39292(16) 0.0562(9) Uani 1 1 d . A .
H3 H -0.1266 -0.0296 0.4261 0.084 Uiso 1 1 calc R . .
O4 O 0.3164(2) 0.2087(3) 0.36107(12) 0.0373(6) Uani 1 1 d . . .
O5 O 0.1902(3) 0.1884(4) 0.51228(14) 0.0522(8) Uani 1 1 d . . .
O6 O 0.2566(3) -0.0305(4) 0.45251(16) 0.0649(10) Uani 1 1 d . . .
H6 H 0.2214 -0.0920 0.4777 0.097 Uiso 1 1 calc R . .
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'
Br Br -0.2901 2.4595 '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'
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
C2 C1 C6 120.7(3) . . ?
C2 C1 Br1 119.3(2) . . ?
C6 C1 Br1 120.0(3) . . ?
C1 C2 C3 120.4(3) . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 Br2 120.2(3) . . ?
C4 C3 Br2 120.1(3) . . ?
C5 C4 O1 125.0(3) . . ?
C5 C4 C3 119.4(3) . . ?
O1 C4 C3 115.5(3) . . ?
C4 C5 C6 121.4(3) . . ?
O4 C6 C1 116.1(3) . . ?
O4 C6 C5 125.4(3) . . ?
C1 C6 C5 118.4(3) . . ?
O1 C7 C10 110.4(3) . . ?
O1 C7 C8 113.3(3) . . ?
C10 C7 C8 112.3(4) . . ?
O1 C7 C9 102.0(4) . . ?
C10 C7 C9 106.4(3) . . ?
C8 C7 C9 111.8(3) . . ?
O3 C10 O2 116.9(5) . . ?
O3 C10 O2' 127.1(4) . . ?
O2 C10 O2' 31.1(3) . . ?
O3 C10 C7 118.6(3) . . ?
O2 C10 C7 123.2(4) . . ?
O2' C10 C7 111.0(5) . . ?
O4 C11 C13 112.6(3) . . ?
O4 C11 C12 102.6(3) . . ?
C13 C11 C12 111.4(4) . . ?
O4 C11 C14 110.1(3) . . ?
C13 C11 C14 112.5(3) . . ?
C12 C11 C14 107.0(3) . . ?
O5 C14 O6 123.6(3) . . ?
O5 C14 C11 120.7(3) . . ?
O6 C14 C11 115.6(3) . . ?
C4 O1 C7 121.6(3) . . ?
C6 O4 C11 121.3(3) . . ?
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
Br1 C1 1.883(3) . ?
Br2 C3 1.881(4) . ?
C1 C2 1.372(5) . ?
C1 C6 1.390(5) . ?
C2 C3 1.387(5) . ?
C3 C4 1.398(5) . ?
C4 C5 1.368(5) . ?
C4 O1 1.376(4) . ?
C5 C6 1.399(5) . ?
C6 O4 1.364(4) . ?
C7 O1 1.452(4) . ?
C7 C10 1.508(6) . ?
C7 C8 1.512(6) . ?
C7 C9 1.537(6) . ?
C10 O3 1.263(4) . ?
C10 O2 1.269(7) . ?
C10 O2' 1.280(8) . ?
C11 O4 1.440(4) . ?
C11 C13 1.508(5) . ?
C11 C12 1.526(6) . ?
C11 C14 1.531(5) . ?
C14 O5 1.228(4) . ?
C14 O6 1.280(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 O2' 0.82 1.89 2.655(7) 155.0 3_556
O6 H6 O2 0.82 1.87 2.686(6) 175.9 3_556
O3 H3 O5 0.82 1.91 2.708(4) 162.4 3_556
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 C3 -0.4(5) . . . . ?
Br1 C1 C2 C3 179.1(3) . . . . ?
C1 C2 C3 C4 0.1(5) . . . . ?
C1 C2 C3 Br2 -179.8(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
Br2 C3 C4 C5 179.8(3) . . . . ?
C2 C3 C4 O1 -175.5(3) . . . . ?
Br2 C3 C4 O1 4.4(4) . . . . ?
O1 C4 C5 C6 175.4(3) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
C2 C1 C6 O4 177.6(3) . . . . ?
Br1 C1 C6 O4 -1.9(4) . . . . ?
C2 C1 C6 C5 0.7(5) . . . . ?
Br1 C1 C6 C5 -178.8(3) . . . . ?
C4 C5 C6 O4 -177.3(3) . . . . ?
C4 C5 C6 C1 -0.8(5) . . . . ?
O1 C7 C10 O3 -9.5(5) . . . . ?
C8 C7 C10 O3 -136.9(4) . . . . ?
C9 C7 C10 O3 100.5(4) . . . . ?
O1 C7 C10 O2 157.3(7) . . . . ?
C8 C7 C10 O2 29.9(8) . . . . ?
C9 C7 C10 O2 -92.8(7) . . . . ?
O1 C7 C10 O2' -170.4(6) . . . . ?
C8 C7 C10 O2' 62.2(7) . . . . ?
C9 C7 C10 O2' -60.4(7) . . . . ?
O4 C11 C14 O5 -145.6(4) . . . . ?
C13 C11 C14 O5 -19.1(5) . . . . ?
C12 C11 C14 O5 103.7(4) . . . . ?
O4 C11 C14 O6 37.4(5) . . . . ?
C13 C11 C14 O6 163.9(4) . . . . ?
C12 C11 C14 O6 -73.4(4) . . . . ?
C5 C4 O1 C7 45.4(5) . . . . ?
C3 C4 O1 C7 -139.6(3) . . . . ?
C10 C7 O1 C4 -88.0(4) . . . . ?
C8 C7 O1 C4 38.8(5) . . . . ?
C9 C7 O1 C4 159.2(3) . . . . ?
C1 C6 O4 C11 147.2(3) . . . . ?
C5 C6 O4 C11 -36.2(5) . . . . ?
C13 C11 O4 C6 -48.0(4) . . . . ?
C12 C11 O4 C6 -167.9(3) . . . . ?
C14 C11 O4 C6 78.5(4) . . . . ?
