Synthesis, Reactivity, and X-ray Crystal Structure of Some Mixed-Ligand Oxovanadium(V) Complexes: First Report of Binuclear Oxovanadium(V) Complexes Containing 4,4‘-Bipyridine Type Bridge
Sutradhar, Manas; Mukherjee, Gurunath; Drew, Michael G. B.; Ghosh, Saktiprosad; Inorganic Chemistry 45 (2006) 5150–5161; doi:10.1021/ic051120g

data_4331573
_publ_section_title
;
 Synthesis, Reactivity, and X-ray Crystal Structure of Some Mixed-Ligand
 Oxovanadium(V) Complexes:&#x00A0; First Report of Binuclear
 Oxovanadium(V) Complexes Containing 4,4&#x2018;-Bipyridine Type Bridge
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5150
_journal_page_last               5161
_journal_paper_doi               10.1021/ic051120g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C19 H17 N4 O5 V'
_chemical_formula_weight         432.31
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.400(10)
_cell_angle_beta                 63.540(10)
_cell_angle_gamma                88.400(10)
_cell_formula_units_Z            2
_cell_length_a                   9.662(12)
_cell_length_b                   10.443(12)
_cell_length_c                   10.640(12)
_cell_measurement_reflns_used    5733
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.36
_cell_volume                     961(2)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1988)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5733
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Walker et al., Acta Cryst 1983 A39 158'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0044(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.8756P] where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                2850
_reflns_number_total             3364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051120gsup6.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331573