Cyanide-bridged decanuclear cobalt-iron cage.
Shiga, Takuya; Tetsuka, Tamaki; Sakai, Kanae; Sekine, Yoshihiro; Nihei, Masayuki; Newton, Graham N.; Oshio, Hiroki; Inorganic chemistry 53 (2014) 5899–5901; doi:10.1021/ic500964m

data_4338720
_publ_section_title
;
 Cyanide-bridged decanuclear cobalt-iron cage.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5899
_journal_page_last               5901
_journal_paper_doi               10.1021/ic500964m
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C192 H168 Co6 Fe4 N48, 2(C8 H20 N), B F4, 9(C O), 7(O)'
_chemical_formula_sum            'C217 H260 B Co6 F4 Fe4 N50 O17'
_chemical_formula_weight         4504.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.959(12)
_cell_length_b                   29.150(15)
_cell_length_c                   34.113(18)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.25
_cell_volume                     22830(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2100
_diffrn_reflns_av_unetI/netI     0.3203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            108751
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.069
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.9294
_exptl_absorpt_correction_T_min  0.8656
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             9420
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5736
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 4461 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.176(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2240
_refine_ls_number_reflns         42389
_refine_ls_number_restraints     2086
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.3009
_refine_ls_R_factor_gt           0.1352
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2993
_refine_ls_wR_factor_ref         0.3468
_reflns_Friedel_coverage         0.873
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                14480
_reflns_number_total             42389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500964m_si_002.cif
_cod_data_source_block           Comp1_291K
_cod_depositor_comments
'Adding full bibliography for 4338719--4338720.cif.'
_cod_original_cell_volume        22831(20)
_cod_database_code               4338720
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.929
_shelxl_version_number           2013-4
_shelx_res_checksum              37525
_shelx_hkl_checksum              48408