A cyanide and hydroxo-bridged nanocage: a new generation of coordination clusters.
Mondal, Abhishake; Durdevic, Sonja; Chamoreau, Lise-Marie; Journaux, Yves; Julve, Miguel; Lisnard, Laurent; Lescouëzec, Rodrigue; Chemical communications (Cambridge, England) 49 (2013) 1181–1183; doi:10.1039/c2cc38404c

data_7112396
_publ_section_title
;
 A cyanide and hydroxo-bridged nanocage: a new generation of coordination
 clusters.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1181
_journal_page_last               1183
_journal_paper_doi               10.1039/c2cc38404c
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety
'C150 H231 B4 Co12 Fe4 N37 O44, C12 H18 N6 Co, 9 (C2 H3 N), 1.5 (H2 O)'
_chemical_formula_sum            'C180 H279 B4 Co13 Fe4 N52 O45.5'
_chemical_formula_weight         4932.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.4290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6791(7)
_cell_length_b                   36.3243(13)
_cell_length_c                   34.1575(12)
_cell_measurement_reflns_used    9552
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.32
_cell_volume                     25656.8(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND. Crystal Impact GbR, Bonn, Germany'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            152231
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison,
Wisconsin, USA.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             10248
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.016
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2576
_refine_ls_number_reflns         55987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+16.0182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                48048
_reflns_number_total             55987
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             7108822
_cod_data_source_file            c2cc38404c.txt
_cod_data_source_block           sd110_0m
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C180 H279 B4 Co13 Fe4 N52 O45.50'
_cod_database_code               7112396