Versatile Reactivity and Theoretical Evaluation of Mono- and Dinuclear Oxidovanadium(V) Compounds of Aroylazines: Electrogeneration of Mixed-Valence Divanadium(IV,V) Complexes.
Dash, Subhashree P.; Roy, Satabdi; Mohanty, Monalisa; Carvalho, M Fernanda N N; Kuznetsov, Maxim L.; Pessoa, João Costa; Kumar, Amit; Patil, Yogesh P.; Crochet, Aurélien; Dinda, Rupam; Inorganic chemistry 55 (2016) 8407–8421; doi:10.1021/acs.inorgchem.6b01001

data_4348131
_publ_section_title
;
 Versatile Reactivity and Theoretical Evaluation of Mono- and Dinuclear
 Oxidovanadium(V) Compounds of Aroylazines: Electrogeneration of
 Mixed-Valence Divanadium(IV,V) Complexes.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8407
_journal_page_last               8421
_journal_paper_doi               10.1021/acs.inorgchem.6b01001
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C21 H20 N3 O4 V'
_chemical_formula_weight         429.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.716(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.305(2)
_cell_length_b                   10.502(2)
_cell_length_c                   18.603(3)
_cell_measurement_reflns_used    6846
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.71
_cell_measurement_theta_min      2.19
_cell_volume                     2011.0(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25250
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.192
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.8610
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0070(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1625
_reflns_number_total             3549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01001_si_004.cif
_cod_data_source_block           SD-45
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4348131
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              92949
_shelx_hkl_checksum              95114