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_4338454
_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_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C71 H88 Fe3 N O3 P S5 V'
_chemical_formula_sum            'C71 H88 Fe3 N O3 P S5 V'
_chemical_formula_weight         1413.24
_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                102.80(2)
_cell_angle_beta                 93.233(9)
_cell_angle_gamma                114.945(15)
_cell_formula_units_Z            2
_cell_length_a                   14.50(3)
_cell_length_b                   16.41(3)
_cell_length_c                   17.69(3)
_cell_measurement_reflns_used    6827
_cell_measurement_temperature    273
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      3.00
_cell_volume                     3668(12)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.3041
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32174
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1482.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.300
_refine_diff_density_min         -1.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     709
_refine_ls_number_reflns         13319
_refine_ls_number_restraints     30
_refine_ls_R_factor_gt           0.1629
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.4614
_reflns_number_gt                6119
_reflns_number_total             13319
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic4030603_si_002.cif
_cod_data_source_block           (OPO)VFe3S4(SDmp)(HNMe2)
_cod_depositor_comments
'Adding full bibliography for 4338450--4338455.cif.'
_cod_original_cell_volume        3667(10)
_cod_database_code               4338454