#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:29:08 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180041 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/35/7033504.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_7033504
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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-07
_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                 91.575(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4640(15)
_cell_length_b                   8.2746(8)
_cell_length_c                   17.4676(15)
_cell_measurement_reflns_used    3210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.33
_cell_volume                     2523.2(4)
_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)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.830
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10962
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.631
_diffrn_reflns_theta_min         2.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.226
_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    2.439
_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         2.268
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3526
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0350P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2164
_reflns_number_total             3526
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt03082f2.cif
_cod_data_source_block           Co100
_cod_depositor_comments
'Adding full bibliography for 7033492--7033506.cif.'
_cod_database_code               7033504
#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   0.234
_shelx_estimated_absorpt_t_min   0.124
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.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 0.22368(3) -0.44394(7) -0.20024(3) 0.01840(15) Uani 1 1 d . . .
Br2 Br 0.10030(3) -0.45048(7) -0.04913(3) 0.02063(16) Uani 1 1 d . . .
Br3 Br 0.06197(3) 0.35758(6) -0.32830(3) 0.01901(15) Uani 1 1 d . . .
Co4 Co 0.0000 -0.14429(12) -0.2500 0.0159(3) Uani 1 2 d S T P
O1 O 0.15118(17) -0.2254(4) -0.32122(19) 0.0123(8) Uani 1 1 d . . .
O2 O -0.03782(18) -0.2647(4) -0.09572(19) 0.0118(8) Uani 1 1 d . . .
O3 O 0.08092(18) 0.0111(4) -0.37040(19) 0.0104(8) Uani 1 1 d . . .
N1 N 0.1086(2) -0.2375(5) -0.2565(2) 0.0100(9) Uani 1 1 d . . .
N2 N 0.0147(2) -0.2647(5) -0.1519(2) 0.0103(9) Uani 1 1 d . . .
N3 N 0.0359(2) 0.0280(5) -0.3093(2) 0.0102(9) Uani 1 1 d . . .
C1 C 0.1323(3) -0.3280(6) -0.2021(3) 0.0075(10) Uani 1 1 d . U .
C2 C 0.0790(3) -0.3382(6) -0.1397(3) 0.0122(11) Uani 1 1 d . . .
C3 C 0.0230(2) 0.1729(6) -0.2833(3) 0.0098(11) Uani 1 1 d . . .
C4 C 0.1557(3) -0.1493(6) -0.4618(3) 0.0123(11) Uani 1 1 d . . .
H4A H 0.2003 -0.0785 -0.4505 0.015 Uiso 1 1 calc R . .
H4B H 0.1755 -0.2585 -0.4733 0.015 Uiso 1 1 calc R . .
C5 C 0.1127(3) -0.0850(6) -0.5323(3) 0.0125(11) Uani 1 1 d . . .
H5A H 0.0918 0.0231 -0.5203 0.015 Uiso 1 1 calc R . .
H5B H 0.0688 -0.1573 -0.5443 0.015 Uiso 1 1 calc R . .
C6 C 0.1621(3) -0.0714(6) -0.6032(3) 0.0167(12) Uani 1 1 d . . .
H6A H 0.1296 -0.0364 -0.6474 0.020 Uiso 1 1 calc R . .
H6B H 0.1832 -0.1792 -0.6153 0.020 Uiso 1 1 calc R . .
C7 C 0.2286(3) 0.0493(6) -0.5915(3) 0.0195(13) Uani 1 1 d . . .
H7A H 0.2551 0.0632 -0.6398 0.029 Uiso 1 1 calc GR . .
H7B H 0.2648 0.0077 -0.5523 0.029 Uiso 1 1 calc GR . .
H7C H 0.2084 0.1536 -0.5749 0.029 Uiso 1 1 calc GR . .
B1 B 0.1054(3) -0.1593(7) -0.3888(3) 0.0112(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'
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 Co4 N1 135.9(2) . 2_554
N2 Co4 N1 76.27(16) . .
N2 Co4 N1 82.06(16) . 2_554
N2 Co4 N1 76.27(16) 2_554 2_554
N2 Co4 N1 82.06(16) 2_554 .
N2 Co4 N2 120.0(2) . 2_554
N3 Co4 N1 129.63(17) 2_554 .
N3 Co4 N1 129.63(17) . 2_554
N3 Co4 N1 86.09(16) . .
N3 Co4 N1 86.09(16) 2_554 2_554
N3 Co4 N2 86.70(17) . 2_554
N3 Co4 N2 86.70(17) 2_554 .
N3 Co4 N2 144.67(17) 2_554 2_554
N3 Co4 N2 144.68(17) . .
N3 Co4 N3 81.3(2) . 2_554
N1 O1 B1 112.5(3) . .
N2 O2 B1 114.6(4) . 2_554
N3 O3 B1 116.1(3) . .
O1 N1 Co4 122.7(3) . .
C1 N1 Co4 117.5(3) . .
C1 N1 O1 119.1(4) . .
O2 N2 Co4 123.1(3) . .
C2 N2 Co4 117.9(3) . .
C2 N2 O2 118.8(4) . .
O3 N3 Co4 124.6(3) . .
C3 N3 Co4 116.2(3) . .
C3 N3 O3 118.7(4) . .
N1 C1 Br1 125.3(4) . .
N1 C1 C2 113.1(4) . .
C2 C1 Br1 121.6(4) . .
N2 C2 Br2 121.8(4) . .
N2 C2 C1 114.9(4) . .
C1 C2 Br2 123.2(4) . .
N3 C3 Br3 122.7(3) . .
N3 C3 C3 112.9(3) . 2_554
C3 C3 Br3 124.39(15) 2_554 .
C5 C4 B1 113.6(4) . .
C4 C5 C6 113.7(4) . .
C5 C6 C7 112.3(4) . .
O1 B1 C4 111.0(4) . .
O2 B1 O1 109.3(4) 2_554 .
O2 B1 O3 111.0(4) 2_554 .
O2 B1 C4 110.1(4) 2_554 .
O3 B1 O1 108.5(4) . .
O3 B1 C4 107.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C1 1.862(4) .
Br2 C2 1.864(5) .
Br3 C3 1.857(5) .
Co4 N1 2.053(4) 2_554
Co4 N1 2.053(4) .
Co4 N2 1.993(4) .
Co4 N2 1.993(4) 2_554
Co4 N3 1.879(4) 2_554
Co4 N3 1.879(4) .
O1 N1 1.373(5) .
O1 B1 1.511(7) .
O2 N2 1.362(4) .
O2 B1 1.486(6) 2_554
O3 N3 1.351(5) .
O3 B1 1.511(7) .
N1 C1 1.272(6) .
N2 C2 1.290(6) .
N3 C3 1.304(6) .
C1 C2 1.454(6) .
C3 C3 1.430(9) 2_554
C4 C5 1.521(7) .
C4 B1 1.570(7) .
C5 C6 1.533(6) .
C6 C7 1.541(7) .
B1 O2 1.486(6) 2_554
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 5.9(6) . .
Br1 C1 C2 N2 -173.4(4) . .
Co4 N1 C1 Br1 172.9(2) . .
Co4 N1 C1 C2 -5.2(6) . .
Co4 N2 C2 Br2 178.5(2) . .
Co4 N2 C2 C1 -2.2(6) . .
Co4 N3 C3 Br3 173.9(2) . .
Co4 N3 C3 C3 -5.4(7) . 2_554
O1 N1 C1 Br1 2.3(7) . .
O1 N1 C1 C2 -175.9(4) . .
O2 N2 C2 Br2 2.3(6) . .
O2 N2 C2 C1 -178.4(4) . .
O3 N3 C3 Br3 1.6(6) . .
O3 N3 C3 C3 -177.7(5) . 2_554
N1 Co4 N3 O3 -108.6(4) 2_554 .
N1 Co4 N3 O3 42.8(4) . .
N1 Co4 N3 C3 79.6(4) 2_554 .
N1 Co4 N3 C3 -129.0(4) . .
N1 O1 B1 O2 -57.8(5) . 2_554
N1 O1 B1 O3 63.4(5) . .
N1 O1 B1 C4 -179.3(4) . .
N1 C1 C2 Br2 -175.9(4) . .
N1 C1 C2 N2 4.9(7) . .
N2 Co4 N3 O3 -39.5(4) 2_554 .
N2 Co4 N3 O3 102.3(4) . .
N2 Co4 N3 C3 -69.5(5) . .
N2 Co4 N3 C3 148.7(4) 2_554 .
N3 Co4 N3 O3 173.9(5) 2_554 .
N3 Co4 N3 C3 2.1(3) 2_554 .
N3 O3 B1 O1 -61.0(5) . .
N3 O3 B1 O2 59.1(5) . 2_554
N3 O3 B1 C4 179.2(4) . .
C4 C5 C6 C7 -62.8(6) . .
C5 C4 B1 O1 179.5(4) . .
C5 C4 B1 O2 58.4(6) . 2_554
C5 C4 B1 O3 -62.3(5) . .
B1 O1 N1 Co4 -8.3(5) . .
B1 O1 N1 C1 161.8(4) . .
B1 O2 N2 Co4 -3.6(5) 2_554 .
B1 O2 N2 C2 172.4(5) 2_554 .
B1 O3 N3 Co4 -2.4(5) . .
B1 O3 N3 C3 169.2(4) . .
B1 C4 C5 C6 178.7(4) . .
