A Family of Octahedral Magnetic Molecules Based on [Nb(IV)(CN)8](4).
Arczyński, Mirosław; Rams, Michał; Stanek, Jan; Fitta, Magdalena; Sieklucka, Barbara; Dunbar, Kim R.; Pinkowicz, Dawid; Inorganic chemistry 56 (2017) 4021–4027; doi:10.1021/acs.inorgchem.6b03134

data_4345609
_publ_section_title
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 A Family of Octahedral Magnetic Molecules Based on [Nb(IV)(CN)8](4).
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4021
_journal_page_last               4027
_journal_paper_doi               10.1021/acs.inorgchem.6b03134
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C144 H128 Fe4 N32 Nb2'
_chemical_formula_weight         2715.99
_space_group_crystal_system      tetragonal
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_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.91690(10)
_cell_length_b                   22.91690(10)
_cell_length_c                   62.7877(8)
_cell_measurement_reflns_used    36733
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      70.963
_cell_measurement_theta_min      2.815
_cell_volume                     32975.1(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'SuperNova Atlas CCD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            74541
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.963
_diffrn_reflns_theta_min         2.815
_exptl_absorpt_coefficient_mu    4.250
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysalisPro
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       block
_exptl_crystal_F_000             11216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.498(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1640
_refine_ls_number_reflns         27952
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                14699
_reflns_number_total             27952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03134_si_003.cif
_cod_data_source_block           Fe4Nb2
_cod_depositor_comments
;

2021-04-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C288 H256 Fe8 Mo0 N64 Nb4'
_cod_original_formula_weight         5431.99
_cod_original_formula_units_Z            4
_cod_database_code               4345609
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              94798
_shelx_hkl_checksum              74791