Solution Study of a Structurally Characterized Monoalkoxo-Bound Monooxo-Vanadium(V) Complex: Spontaneous Generation of the Corresponding Oxobridged Divanadium(V,V) Complex and its Electroreduction to a Mixed-Valence Species in Solution
Rupam Dinda; Parbati Sengupta; Manas Sutradhar; Thomas C. W. Mak; Saktiprosad Ghosh; Inorganic Chemistry 47 (2008) 5634–5640; doi:10.1021/ic702172p

data_4305169
_publ_section_title
;
Solution Study of a Structurally Characterized Monoalkoxo-Bound
Monooxo-Vanadium(V) Complex: Spontaneous Generation of the Corresponding
Oxobridged Divanadium(V,V) Complex and its Electroreduction to a
Mixed-Valence Species in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5634
_journal_page_last               5640
_journal_paper_doi               10.1021/ic702172p
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C16 H15 N2 O5 V'
_chemical_formula_weight         366.24
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   10.136(3)
_cell_length_b                   8.868(3)
_cell_length_c                   35.640(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3203.5(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            20112
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0600P)^2^+1.0750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                3002
_reflns_number_total             3889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702172p-file002.cif
_cod_data_source_block           d13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3203.7(16)
_cod_database_code               4305169