New V(IV)O-complexes for oxidative desulfurization of refractory sulfur compounds in fuel: synthesis, structure, reactivity trend and mechanistic studies
Tshentu, Zenixole; Dembaremba, Tendai; Correia, Isabel; Pessoa, João Costa; Gerber, Wilhelmus Jacobus; Kuznetsov, Maxim L.; Hosten, Eric Cyriel; Ogunlaja, Adeniyi; Dalton Transactions  (2019) –; doi:10.1039/C9DT02505G

data_7701431
_publ_section_title
;
 New V(IV)O-complexes for oxidative desulfurization of refractory sulfur
 compounds in fuel: synthesis, structure, reactivity trend and mechanistic
 studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02505G
_journal_year                    2019
_chemical_formula_moiety         'C18 H12 Br2 N4 O3 V, 2(C2 H6 O S)'
_chemical_formula_sum            'C22 H24 Br2 N4 O5 S2 V'
_chemical_formula_weight         699.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-06 deposited with the CCDC.    2019-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3157(7)
_cell_length_b                   15.8806(8)
_cell_length_c                   22.1939(13)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.24
_cell_volume                     5398.1(5)
_computing_cell_refinement       'APEX2 v2011.4-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'PLATON (Spek, 2009) and MERCURY (Macrae, 2008)'
_computing_structure_refinement
'SHELXL-2018/3 (Sheldrick, 2015) and ShelXle (H\"ubschle, 2011)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56689
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.301
_diffrn_reflns_theta_min         1.577
_exptl_absorpt_coefficient_mu    3.523
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6424
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'dark blue green'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.486
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 3855 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         13338
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+6.3758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                10145
_reflns_number_total             13338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02505g2.cif
_cod_data_source_block           ha046
_cod_database_code               7701431
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.279
_shelx_estimated_absorpt_t_max   0.635
_shelx_res_checksum              95999