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_7033498
_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 Fe N6 O6'
_chemical_formula_sum            'C14 H18 B2 Br6 Fe N6 O6'
_chemical_formula_weight         923.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 119.409(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.216(2)
_cell_length_b                   24.294(6)
_cell_length_c                   8.219(3)
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    265
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.85
_cell_volume                     1429.1(7)
_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      265
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1549
_diffrn_reflns_av_unetI/netI     0.1690
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13686
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.824
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.955
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_description       plate
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1843
_refine_ls_R_factor_gt           0.0609
_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          0.1078
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1727
_reflns_number_total             4147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03082f2.cif
_cod_data_source_block           265
_cod_depositor_comments
'Adding full bibliography for 7033492--7033506.cif.'
_cod_original_cell_volume        1429.0(7)
_cod_database_code               7033498
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim N2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N1 \\sim N1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N3 \\sim N3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O1A) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
: with sigma of 0.008 and sigma for terminal atoms of 0.008
3. Others
 Fixed Sof: N1(0.5) N2(0.5) N3(0.5) H4BC(0.5) H4BD(0.5) H4AA(0.5) H4AB(0.5)
 O1A(0.5) O2A(0.5) O3A(0.5) O1B(0.5) O2B(0.5) O3B(0.5) C5B(0.5) H5BA(0.5)
 H5BB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5)
 C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) N2A(0.5) N1A(0.5) N3A(0.5)
 Fixed Uiso: C7A(0.09) C7B(0.09) C6A(0.08) C6B(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C5B(H5BA,H5BB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C6B(H6BA,H6BB)
4.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,H7BC)
;