New oxidovanadium(iv) complex with a BIAN ligand: synthesis, structure, redox properties and catalytic activity
Fomenko, Iakov S.; Gushchin, Artem L.; Shul’pina, Lidia S.; Ikonnikov, Nikolay S.; Abramov, Pavel A.; Romashev, Nikolay F.; Poryvaev, Artem S.; Sheveleva, Alena M.; Bogomyakov, Artem S.; Shmelev, Nikita Y.; Fedin, Matvey V.; Shul’pin, Georgiy B.; Sokolov, Maxim N.; New Journal of Chemistry 42 (2018) 16200–; doi:10.1039/C8NJ03358G

data_7057686
_publ_section_title
;
 New oxidovanadium(iv) complex with a BIAN ligand: synthesis, structure,
 redox properties and catalytic activity
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16200
_journal_paper_doi               10.1039/C8NJ03358G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C37.7 H43.4 Cl5.4 N2 O V'
_chemical_formula_weight         782.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.714(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5919(2)
_cell_length_b                   29.7642(5)
_cell_length_c                   12.0184(2)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.4540
_cell_measurement_theta_min      3.6920
_cell_volume                     3991.65(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25845
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.965
_diffrn_reflns_theta_min         3.291
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.97600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            greenish-yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1626
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.356
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         14630
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0715
_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^)+(0.1417P)^2^+6.6061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2307
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                11553
_reflns_number_total             14630
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8nj03358g2.cif
_cod_data_source_block           c
_cod_depositor_comments          'Adding full bibliography for 7057686.cif.'
_cod_original_formula_sum        'C37.70 H43.40 Cl5.40 N2 O V'
_cod_database_code               7057686
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              67912