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_4335774
_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            'C25 H28 N2 O12 V3'
_chemical_formula_weight         701.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.779(5)
_cell_length_b                   14.807(4)
_cell_length_c                   11.232(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2790.6(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1051
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21422
_diffrn_reflns_theta_full        23.12
_diffrn_reflns_theta_max         23.12
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.9206
_exptl_absorpt_correction_T_min  0.8667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0430
_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^)+(0.1000P)^2^+0.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                1421
_reflns_number_total             2061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4013203_si_001_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2790.5(13)
_cod_database_code               4335774