#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:29:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180041 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/35/7033500.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_7033500
loop_
_publ_author_name
'Dolganov, Alexander V.'
'Belov, Alexander S.'
'Novikov, Valentin V.'
'Vologzhanina, Anna V.'
'Romanenko, Galina V.'
'Budnikova, Yulia G.'
'Zelinskii, Genrikh E.'
'Buzin, Michail I.'
'Voloshin, Yan Z.'
_publ_section_title
;
 First iron and cobalt(ii) hexabromoclathrochelates: structural, magnetic,
 redox, and electrocatalytic behavior.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2476
_journal_page_last               2487
_journal_paper_doi               10.1039/c4dt03082f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Co N6 O6'
_chemical_formula_weight         926.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-11-10 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.919(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.687(3)
_cell_length_b                   8.4103(14)
_cell_length_c                   17.601(3)
_cell_measurement_reflns_used    6181
_cell_measurement_temperature    290
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.32
_cell_volume                     2616.7(8)
_computing_data_collection       'Apex II'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      290
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1109
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.813
_diffrn_reflns_theta_min         2.304
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.861
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_description       prism
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         3254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0140P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1886
_reflns_number_total             3254
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt03082f2.cif
_cod_data_source_block           Co290
_cod_depositor_comments
'Adding full bibliography for 7033492--7033506.cif.'
_cod_database_code               7033500
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2014-3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.243
_shelx_estimated_absorpt_t_min   0.130
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br1 Br 0.27657(2) -0.93476(5) 0.19879(2) 0.05889(16) Uani 1 1 d . . .
Br2 Br 0.39713(2) -0.94300(5) 0.04863(2) 0.05895(17) Uani 1 1 d . . .
Br3 Br 0.43958(2) -0.14708(4) 0.32707(2) 0.05325(16) Uani 1 1 d . . .
Co1 Co 0.5000 -0.65111(7) 0.2500 0.03059(19) Uani 1 2 d S T P
O1 O 0.35349(12) -0.7357(3) 0.32252(11) 0.0366(6) Uani 1 1 d . . .
O2 O 0.53341(12) -0.7524(2) 0.09347(11) 0.0342(6) Uani 1 1 d . . .
O3 O 0.41536(12) -0.4882(2) 0.36697(11) 0.0325(6) Uani 1 1 d . . .
N1 N 0.39500(15) -0.7461(3) 0.25842(15) 0.0309(7) Uani 1 1 d . . .
N2 N 0.48173(16) -0.7560(3) 0.14945(13) 0.0298(7) Uani 1 1 d . . .
N3 N 0.46071(15) -0.4715(3) 0.30656(13) 0.0263(7) Uani 1 1 d . . .
C1 C 0.36863(18) -0.8280(4) 0.20218(18) 0.0289(8) Uani 1 1 d . . .
C2 C 0.4203(2) -0.8316(4) 0.13783(17) 0.0300(9) Uani 1 1 d . . .
C3 C 0.47554(18) -0.3299(4) 0.28275(16) 0.0257(8) Uani 1 1 d . . .
C4 C 0.34647(18) -0.6523(4) 0.46044(15) 0.0293(9) Uani 1 1 d . . .
H4A H 0.3013 -0.5904 0.4487 0.035 Uiso 1 1 calc R . .
H4B H 0.3305 -0.7596 0.4723 0.035 Uiso 1 1 calc R . .
C5 C 0.3867(2) -0.5812(4) 0.53090(17) 0.0444(10) Uani 1 1 d . . .
H5A H 0.4315 -0.6440 0.5430 0.053 Uiso 1 1 calc R . .
H5B H 0.4033 -0.4745 0.5188 0.053 Uiso 1 1 calc R . .
C6 C 0.3385(2) -0.5734(4) 0.60113(19) 0.0477(11) Uani 1 1 d . . .
H6A H 0.3203 -0.6791 0.6127 0.057 Uiso 1 1 calc R . .
H6B H 0.3696 -0.5371 0.6442 0.057 Uiso 1 1 calc R . .
C7 C 0.2724(2) -0.4633(4) 0.5896(2) 0.0636(13) Uani 1 1 d . . .
H7A H 0.2388 -0.5048 0.5505 0.095 Uiso 1 1 calc GR . .
H7B H 0.2901 -0.3603 0.5749 0.095 Uiso 1 1 calc GR . .
H7C H 0.2459 -0.4543 0.6362 0.095 Uiso 1 1 calc GR . .
B1 B 0.3958(2) -0.6580(5) 0.3882(2) 0.0268(10) 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'
B B 0.0013 0.0007 '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
N1 Co1 N1 133.70(15) 2_655 .
N2 Co1 N1 83.26(11) 2_655 .
N2 Co1 N1 76.67(11) 2_655 2_655
N2 Co1 N1 76.67(11) . .
N2 Co1 N1 83.26(11) . 2_655
N2 Co1 N2 127.48(14) 2_655 .
N3 Co1 N1 133.17(11) 2_655 .
N3 Co1 N1 85.70(11) 2_655 2_655
N3 Co1 N1 133.17(11) . 2_655
N3 Co1 N1 85.70(11) . .
N3 Co1 N2 86.54(10) . 2_655
N3 Co1 N2 138.24(10) 2_655 2_655
N3 Co1 N2 138.24(10) . .
N3 Co1 N2 86.54(10) 2_655 .
N3 Co1 N3 78.45(15) . 2_655
N1 O1 B1 113.2(2) . .
N2 O2 B1 115.3(2) . 2_655
N3 O3 B1 115.8(2) . .
O1 N1 Co1 123.5(2) . .
C1 N1 Co1 117.7(2) . .
C1 N1 O1 118.6(3) . .
O2 N2 Co1 122.5(2) . .
C2 N2 Co1 118.5(2) . .
C2 N2 O2 119.0(3) . .
O3 N3 Co1 123.26(18) . .
C3 N3 Co1 117.9(2) . .
C3 N3 O3 118.7(2) . .
N1 C1 Br1 125.5(2) . .
N1 C1 C2 112.6(3) . .
C2 C1 Br1 121.9(2) . .
N2 C2 Br2 123.4(2) . .
N2 C2 C1 114.4(3) . .
C1 C2 Br2 122.1(3) . .
N3 C3 Br3 123.6(2) . .
N3 C3 C3 112.77(16) . 2_655
C3 C3 Br3 123.61(9) 2_655 .
H4A C4 H4B 107.6 . .
C5 C4 H4A 108.7 . .
C5 C4 H4B 108.7 . .
C5 C4 B1 114.4(3) . .
B1 C4 H4A 108.7 . .
B1 C4 H4B 108.7 . .
C4 C5 H5A 108.6 . .
C4 C5 H5B 108.6 . .
H5A C5 H5B 107.6 . .
C6 C5 C4 114.6(3) . .
C6 C5 H5A 108.6 . .
C6 C5 H5B 108.6 . .
C5 C6 H6A 109.3 . .
C5 C6 H6B 109.3 . .
H6A C6 H6B 107.9 . .
C7 C6 C5 111.8(3) . .
C7 C6 H6A 109.3 . .
C7 C6 H6B 109.3 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O1 B1 O2 108.9(3) . 2_655
O1 B1 O3 109.3(3) . .
O1 B1 C4 111.1(3) . .
O2 B1 O3 110.7(3) 2_655 .
O2 B1 C4 108.8(3) 2_655 .
O3 B1 C4 108.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.858(3) .
Br2 C2 1.862(3) .
Br3 C3 1.847(3) .
Co1 N1 2.031(3) 2_655
Co1 N1 2.031(3) .
Co1 N2 1.994(2) 2_655
Co1 N2 1.994(2) .
Co1 N3 1.950(2) .
Co1 N3 1.950(2) 2_655
O1 N1 1.369(3) .
O1 B1 1.505(4) .
O2 N2 1.367(3) .
O2 B1 1.508(4) 2_655
O3 N3 1.360(3) .
O3 B1 1.519(4) .
N1 C1 1.281(4) .
N2 C2 1.269(4) .
N3 C3 1.292(3) .
C1 C2 1.479(4) .
C3 C3 1.464(5) 2_655
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 C5 1.531(4) .
C4 B1 1.567(4) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 C6 1.526(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.500(5) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
B1 O2 1.508(4) 2_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_4
Br1 C1 C2 Br2 0.0(4) . .
Br1 C1 C2 N2 -178.4(2) . .
Co1 N1 C1 Br1 176.63(15) . .
Co1 N1 C1 C2 -2.8(4) . .
Co1 N2 C2 Br2 -177.18(14) . .
Co1 N2 C2 C1 1.2(4) . .
Co1 N3 C3 Br3 177.40(15) . .
Co1 N3 C3 C3 -3.1(4) . 2_655
O1 N1 C1 Br1 0.8(4) . .
O1 N1 C1 C2 -178.6(3) . .
O2 N2 C2 Br2 1.4(4) . .
O2 N2 C2 C1 179.9(3) . .
O3 N3 C3 Br3 0.9(4) . .
O3 N3 C3 C3 -179.6(3) . 2_655
N1 O1 B1 O2 -59.0(3) . 2_655
N1 O1 B1 O3 62.1(3) . .
N1 O1 B1 C4 -178.8(3) . .
N1 C1 C2 Br2 179.5(2) . .
N1 C1 C2 N2 1.0(4) . .
N3 O3 B1 O1 -61.3(3) . .
N3 O3 B1 O2 58.6(3) . 2_655
N3 O3 B1 C4 177.7(2) . .
C4 C5 C6 C7 -64.6(4) . .
C5 C4 B1 O1 177.6(3) . .
C5 C4 B1 O2 57.7(4) . 2_655
C5 C4 B1 O3 -62.5(4) . .
B1 O1 N1 Co1 -4.5(3) . .
B1 O1 N1 C1 171.1(3) . .
B1 O2 N2 Co1 -2.3(3) 2_655 .
B1 O2 N2 C2 179.2(3) 2_655 .
B1 O3 N3 Co1 -0.6(4) . .
B1 O3 N3 C3 175.7(3) . .
B1 C4 C5 C6 179.2(3) . .
