Heterobimetallic μ-Oxido Complexes Containing Discrete V(V)-O-M(III) (M = Mn, Fe) Cores: Targeted Synthesis, Structural Characterization, and Redox Studies.
Bhattacharya, Kisholoy; Abtab, Sk Md Towsif; Majee, Mithun Chandra; Endo, Akira; Chaudhury, Muktimoy; Inorganic chemistry 53 (2014) 8287–8297; doi:10.1021/ic501563r

data_4340774
_publ_section_title
;
 Heterobimetallic \m-Oxido Complexes Containing Discrete V(V)-O-M(III) (M
 = Mn, Fe) Cores: Targeted Synthesis, Structural Characterization, and
 Redox Studies.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8287
_journal_page_last               8297
_journal_paper_doi               10.1021/ic501563r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C31 H29 Br Mn N4 O5 S2 V'
_chemical_formula_weight         787.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.565(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6244(18)
_cell_length_b                   12.4882(18)
_cell_length_c                   23.283(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3479.7(8)
_computing_cell_refinement       'BRUKER APEX-II'
_computing_data_collection       'BRUKER APEX-II'
_computing_data_reduction        'BRUKER APEX-II'
_computing_molecular_graphics    'MERCURY 2.2, PLATON-97'
_computing_publication_material  'MERCURY 2.2, PLATON-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_measurement_method       OMEGA-SCAN
_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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9233
_diffrn_reflns_theta_full        18.54
_diffrn_reflns_theta_max         18.54
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.943
_exptl_absorpt_correction_T_max  0.7593
_exptl_absorpt_correction_T_min  0.6423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.284
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         2597
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.1800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                1477
_reflns_number_total             2597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501563r_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4340774--4340778.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4340774