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#$Date: 2016-03-26 22:09:08 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180492 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/61/7216110.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_7216110
loop_
_publ_author_name
'Bourne, Susan A.'
'Moitsheki, Lesego J.'
_publ_section_title
;
 Anion dependent structural diversity in cobalt(ii) complexes of
 4,4′-bipyridine-N,N′-dioxide
;
_journal_issue                   112
_journal_name_full               CrystEngComm
_journal_page_first              674
_journal_paper_doi               10.1039/b510684b
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         '(Co (H2O)6), Br2, 2(C10 H8 N2 O2), 2(H2 O)'
_chemical_formula_sum            'C20 H28 Br2 Co N4 O12'
_chemical_formula_weight         735.21
_chemical_name_common            '(Co(H2O)6)Br2 . 2(bpdo) . 2H2O'
_chemical_name_systematic
;
[Co(H2O)6]Br2 . 2(bpdo) . 2H2O
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.336(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3728(2)
_cell_length_b                   6.6329(1)
_cell_length_c                   20.0945(4)
_cell_measurement_temperature    113(2)
_cell_volume                     1378.58(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22395
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    3.587
_exptl_absorpt_correction_T_max  0.5340
_exptl_absorpt_correction_T_min  0.4333
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.924
_refine_diff_density_min         -3.105
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3295
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+11.0541P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                2882
_reflns_number_total             3295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b510684b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7216110
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Br1A Br 0.39143(4) 0.73924(7) 0.02844(2) 0.01497(15) Uani 0.925(3) 1 d P A 1
O1WA O 1.3435(3) 1.2370(6) 0.05481(18) 0.0241(7) Uani 0.925(3) 1 d P A 1
Br1B Br 1.3909(6) 1.2630(11) 0.0287(3) 0.0241(7) Uani 0.08 1 d P A 2
O1WB O 0.324(4) 0.800(6) 0.058(2) 0.01497(15) Uani 0.08 1 d P A 2
Co1 Co 1.0000 1.0000 0.0000 0.0096(2) Uani 1 2 d S . .
O2 O 1.1075(3) 0.8546(5) 0.08105(16) 0.0192(7) Uani 1 1 d D . .
H21 H 1.076(7) 0.713(8) 0.090(4) 0.06(2) Uiso 1 1 d D . .
H22 H 1.198(4) 0.824(10) 0.074(3) 0.045(19) Uiso 1 1 d D . .
O3 O 0.8490(3) 1.0574(6) 0.05963(17) 0.0244(8) Uani 1 1 d D . .
H31 H 0.840(6) 0.912(6) 0.063(3) 0.05(2) Uiso 1 1 d D . .
H32 H 0.766(5) 1.121(9) 0.044(3) 0.047(19) Uiso 1 1 d D . .
O4 O 1.0866(3) 1.2721(5) 0.02800(16) 0.0197(7) Uani 1 1 d D . .
H41 H 1.181(5) 1.241(12) 0.045(4) 0.07(2) Uiso 1 1 d D . .
H42 H 1.055(6) 1.346(10) 0.065(3) 0.05(2) Uiso 1 1 d D . .
O1 O 1.0265(3) 0.5073(5) 0.13435(15) 0.0151(6) Uani 1 1 d . . .
N2 N 0.9116(3) 0.5054(5) 0.15945(18) 0.0129(7) Uani 1 1 d . . .
C3 C 0.8034(4) 0.5173(7) 0.1179(2) 0.0148(8) Uani 1 1 d . . .
H3 H 0.8102 0.5273 0.0711 0.018 Uiso 1 1 calc R . .
C4 C 0.6832(4) 0.5151(7) 0.1428(2) 0.0137(8) Uani 1 1 d . . .
H4 H 0.6079 0.5234 0.1129 0.016 Uiso 1 1 calc R . .
C5 C 0.6708(4) 0.5006(6) 0.21201(19) 0.0091(7) Uani 1 1 d . . .
C6 C 0.7859(4) 0.4900(7) 0.2529(2) 0.0143(8) Uani 1 1 d . . .
H6 H 0.7825 0.4817 0.2999 0.017 Uiso 1 1 calc R . .
C7 C 0.9042(4) 0.4915(7) 0.2261(2) 0.0146(8) Uani 1 1 d . . .
H7 H 0.9812 0.4827 0.2547 0.017 Uiso 1 1 calc R . .
O8 O 0.1832(3) 0.4910(5) 0.31379(15) 0.0182(7) Uani 1 1 d . . .
N9 N 0.2986(3) 0.4946(5) 0.29060(17) 0.0124(7) Uani 1 1 d . . .
C10 C 0.3084(4) 0.4932(6) 0.2234(2) 0.0127(8) Uani 1 1 d . . .
H10 H 0.2322 0.4904 0.1940 0.015 Uiso 1 1 calc R . .
C11 C 0.4273(4) 0.4956(6) 0.1978(2) 0.0123(8) Uani 1 1 d . . .
H11 H 0.4319 0.4950 0.1508 0.015 Uiso 1 1 calc R . .
C12 C 0.5420(4) 0.4991(6) 0.23926(19) 0.0095(7) Uani 1 1 d . . .
C13 C 0.5284(4) 0.5005(6) 0.3080(2) 0.0126(8) Uani 1 1 d . . .
H13 H 0.6034 0.5030 0.3381 0.015 Uiso 1 1 calc R . .
C14 C 0.4072(4) 0.4981(6) 0.3328(2) 0.0134(8) Uani 1 1 d . . .
H14 H 0.4002 0.4989 0.3796 0.016 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'
N N 0.0061 0.0033 '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'
Co Co 0.3494 0.9721 '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
O4 Co1 O4 180.00(17) 3_775 .
O4 Co1 O3 90.80(14) 3_775 3_775
O4 Co1 O3 89.20(14) . 3_775
O4 Co1 O3 89.20(14) 3_775 .
O4 Co1 O3 90.80(14) . .
O3 Co1 O3 180.0(2) 3_775 .
O4 Co1 O2 89.76(13) 3_775 3_775
O4 Co1 O2 90.24(13) . 3_775
O3 Co1 O2 90.92(13) 3_775 3_775
O3 Co1 O2 89.08(13) . 3_775
O4 Co1 O2 90.24(13) 3_775 .
O4 Co1 O2 89.76(13) . .
O3 Co1 O2 89.08(13) 3_775 .
O3 Co1 O2 90.92(13) . .
O2 Co1 O2 180.00(12) 3_775 .
O1 N2 C7 119.8(3) . .
O1 N2 C3 119.5(3) . .
C7 N2 C3 120.7(3) . .
N2 C3 C4 120.5(4) . .
C3 C4 C5 120.8(4) . .
C6 C5 C4 116.4(4) . .
C6 C5 C12 122.4(4) . .
C4 C5 C12 121.2(3) . .
C7 C6 C5 121.0(4) . .
N2 C7 C6 120.6(4) . .
O8 N9 C14 120.9(3) . .
O8 N9 C10 119.2(3) . .
C14 N9 C10 119.9(3) . .
N9 C10 C11 120.5(4) . .
C10 C11 C12 121.7(4) . .
C13 C12 C11 116.2(3) . .
C13 C12 C5 121.7(3) . .
C11 C12 C5 122.0(4) . .
C14 C13 C12 121.1(4) . .
N9 C14 C13 120.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O4 2.075(3) 3_775
Co1 O4 2.075(3) .
Co1 O3 2.078(3) 3_775
Co1 O3 2.078(3) .
Co1 O2 2.134(3) 3_775
Co1 O2 2.134(3) .
O1 N2 1.329(4) .
N2 C7 1.350(5) .
N2 C3 1.350(5) .
C3 C4 1.378(5) .
C4 C5 1.410(5) .
C5 C6 1.400(5) .
C5 C12 1.481(5) .
C6 C7 1.377(6) .
O8 N9 1.317(4) .
N9 C14 1.358(5) .
N9 C10 1.361(5) .
C10 C11 1.372(5) .
C11 C12 1.400(5) .
C12 C13 1.398(5) .
C13 C14 1.387(5) .
