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_4331570
_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            'C21 H20 N3 O5 V'
_chemical_formula_weight         445.34
_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                101.727(10)
_cell_angle_beta                 105.233(10)
_cell_angle_gamma                101.823(10)
_cell_formula_units_Z            4
_cell_length_a                   10.540(12)
_cell_length_b                   13.682(15)
_cell_length_c                   15.952(17)
_cell_measurement_reflns_used    12415
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.37
_cell_volume                     2090(4)
_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 0.908
_diffrn_measured_fraction_theta_max 0.908
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12415
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.512
_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    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0016(7)
_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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0650P)^2^+1.5233P] where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1410
_reflns_number_gt                5920
_reflns_number_total             7350
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051120gsup1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331570