Chemistry of Monomeric and Dinuclear Non-Oxido Vanadium(IV) and Oxidovanadium(V) Aroylazine Complexes: Exploring Solution Behavior.
Dash, Subhashree P.; Majumder, Sudarshana; Banerjee, Atanu; Carvalho, M Fernanda N N; Adão, Pedro; Pessoa, João Costa; Brzezinski, Krzysztof; Garribba, Eugenio; Reuter, Hans; Dinda, Rupam; Inorganic chemistry 55 (2016) 1165–1182; doi:10.1021/acs.inorgchem.5b02346

data_4344716
_publ_section_title
;
 Chemistry of Monomeric and Dinuclear Non-Oxido Vanadium(IV) and
 Oxidovanadium(V) Aroylazine Complexes: Exploring Solution Behavior.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1165
_journal_page_last               1182
_journal_paper_doi               10.1021/acs.inorgchem.5b02346
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C47.63 H34.63 Cl0.74 N4.63 O4 V'
_chemical_formula_weight         812.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.8290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.81820(10)
_cell_length_b                   19.0878(2)
_cell_length_c                   16.5463(2)
_cell_measurement_reflns_used    9566
_cell_measurement_temperature    406(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      3.44
_cell_volume                     3697.78(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      406(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            130709
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.638
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       prism
_exptl_crystal_F_000             1682
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8929
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.0608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7548
_reflns_number_total             8929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02346_si_003.cif
_cod_data_source_block           RuSD67_0m
_cod_database_code               4344716
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              59996
_shelx_hkl_checksum              52812