Homo- and Heterometal Complexes of Oxido-Metal Ions with a Triangular [V(V)O-MO-V(V)O] [M = V(IV) and Re(V)] Core: Reporting Mixed-Oxidation Oxido-Vanadium(V/IV/V) Compounds with Valence Trapped Structures
Kisholoy Bhattacharya; Manoranjan Maity; Sk Md Towsif Abtab; Mithun Chandra Majee; Muktimoy Chaudhury; Inorganic Chemistry 52 (2013) 9597–9605; doi:10.1021/ic4013203

data_4335773
_publ_section_title
;
 Homo- and Heterometal Complexes of Oxido-Metal Ions with a Triangular
 [V(V)O-MO-V(V)O] [M = V(IV) and Re(V)] Core: Reporting Mixed-Oxidation
 Oxido-Vanadium(V/IV/V) Compounds with Valence Trapped Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9597
_journal_page_last               9605
_journal_paper_doi               10.1021/ic4013203
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C22 H32 N2 O13 V3'
_chemical_formula_weight         685.32
_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                 97.921(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.094(4)
_cell_length_b                   9.921(3)
_cell_length_c                   18.717(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2776.1(13)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1309
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14588
_diffrn_reflns_theta_full        18.21
_diffrn_reflns_theta_max         18.21
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.9491
_exptl_absorpt_correction_T_min  0.8837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       FLAKES
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         1962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.641
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                1323
_reflns_number_total             1962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4013203_si_001_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2776.0(12)
_cod_database_code               4335773