First iron and cobalt(ii) hexabromoclathrochelates: structural, magnetic, redox, and electrocatalytic behavior.
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.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2476–2487; doi:10.1039/c4dt03082f

data_7033506
_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
_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             2014-11-07
_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                 91.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.455(4)
_cell_length_b                   8.2599(17)
_cell_length_c                   17.455(4)
_cell_measurement_reflns_used    3751
_cell_measurement_temperature    60(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.33
_cell_volume                     2515.7(10)
_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      60(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.788
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10951
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.788
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         32.280
_diffrn_reflns_theta_min         2.334
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.257
_exptl_absorpt_correction_T_max  0.130
_exptl_absorpt_correction_T_min  0.099
_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    2.446
_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         1.605
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0445
_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/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2290
_reflns_number_total             3531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03082f2.cif
_cod_data_source_block           Co60
_cod_depositor_comments
'Adding full bibliography for 7033492--7033506.cif.'
_cod_original_cell_volume        2515.8(9)
_cod_database_code               7033506
_shelxl_version_number           2014-3
_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(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim
Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
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)
;