Synthesis of V/Fe/S Clusters Using Vanadium(III) Thiolate Complexes Bearing a Phenoxide-Based Tridentate Ligand.
Taniyama, Nobuhiro; Ohki, Yasuhiro; Tatsumi, Kazuyuki; Inorganic chemistry 53 (2014) 5438–5446; doi:10.1021/ic4030603

data_4338455
_publ_section_title
;
 Synthesis of V/Fe/S Clusters Using Vanadium(III) Thiolate Complexes
 Bearing a Phenoxide-Based Tridentate Ligand.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5438
_journal_page_last               5446
_journal_paper_doi               10.1021/ic4030603
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C107 H106 Fe4 O3 P S7 V'
_chemical_formula_sum            'C107 H106 Fe4 O3 P S7 V'
_chemical_formula_weight         1969.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                87.810(6)
_cell_angle_beta                 82.923(5)
_cell_angle_gamma                79.975(5)
_cell_formula_units_Z            2
_cell_length_a                   15.978(3)
_cell_length_b                   16.111(3)
_cell_length_c                   22.370(4)
_cell_measurement_reflns_used    15549
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.01
_cell_volume                     5626.6(18)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            69808
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             2052.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.710
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         25680
_refine_ls_number_restraints     14
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                16196
_reflns_number_total             25680
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic4030603_si_002.cif
_cod_data_source_block           '[VFe3S4-Fe]'
_cod_depositor_comments
'Adding full bibliography for 4338450--4338455.cif.'
_cod_original_cell_volume        5626.8(16)
_cod_database_code               4338455