Bis(phenolate)-functionalized N-heterocyclic carbene complexes of oxo- and imido-vanadium(V)
Suresh, Lakshmi; Finnstad, Jone; Törnroos, Karl W.; Le Roux, Erwan; Inorganica Chimica Acta 521 (2021) 120301–; doi:10.1016/j.ica.2021.120301

data_1566186
_publ_section_title
;
 Bis(phenolate)-functionalized N-heterocyclic carbene complexes of oxo-
 and imido-vanadium(V)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120301
_journal_paper_doi               10.1016/j.ica.2021.120301
_journal_volume                  521
_journal_year                    2021
_chemical_formula_moiety         'C33 H44 F3 N2 O5 V'
_chemical_formula_sum            'C33 H44 F3 N2 O5 V'
_chemical_formula_weight         656.64
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.0480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3728(7)
_cell_length_b                   17.2974(7)
_cell_length_c                   12.1482(5)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.35
_cell_volume                     3230.3(2)
_computing_cell_refinement       'Bruker AXS Inc. SAINT V6.45A'
_computing_data_collection       'Bruker AXS Inc. APEX2 v2008.1-0'
_computing_data_reduction        'Bruker AXS Inc. SAINT V6.45A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS APEXII Pt135 CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.974
_diffrn_reflns_theta_min         1.772
_diffrn_source                   'Bruker AXS TXS Ultra Rotating Anode'
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_exptl_transmission_factor_max   0.8622
_exptl_transmission_factor_min   0.5379
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.002
_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^+1.4731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7358
_reflns_number_total             9396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Compound5.cif
_cod_data_source_block           Compound5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566186
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              52428
_shelx_hkl_checksum              53561