Vanadium-Iron-Sulfur Clusters Containing the Cubane-type [VFe3S4] Core Unit: Synthesis of a Cluster with the Topology of the PN Cluster of Nitrogenase
Jing-Lin Zuo; Hong-Cai Zhou; R. H. Holm; Inorganic Chemistry 42 (2003) 4624–4631; doi:10.1021/ic0301369

data_4313902
_publ_section_title
;
 Vanadium-Iron-Sulfur Clusters Containing the Cubane-type [VFe3S4] Core
 Unit: Synthesis of a Cluster with the Topology of the PN Cluster of
 Nitrogenase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4624
_journal_page_last               4631
_journal_paper_doi               10.1021/ic0301369
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         (TpVFe3S4(PBu3)3)(PF6)
_chemical_formula_sum            'C45 H91 B F6 Fe3 N6 P4 S4 V'
_chemical_formula_weight         1311.66
_chemical_melting_point          ?
_chemical_name_common            none
_chemical_name_systematic
;
 (hydrogen tris(pyrazolyl)borato-N,N',N'')-
(tetrakis(mu3-sulfido))-tris(tributylphosphine-
iron-S,S',S'')-vanadium hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.388(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.897(15)
_cell_length_b                   24.33(2)
_cell_length_c                   16.750(16)
_cell_measurement_reflns_used    546
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.6
_cell_volume                     6409(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36315
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2748
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11289
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.098
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                7678
_reflns_number_total             11289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0301369.cif
_cod_data_source_block           (TpVFe3S4(PBu3)3)(PF6)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6409(11)
_cod_database_code               4313902