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_1566187
_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         'C62 H88 N4 O7 V2'
_chemical_formula_sum            'C62 H88 N4 O7 V2'
_chemical_formula_weight         1103.24
_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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 110.2310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6163(2)
_cell_length_b                   27.57870(10)
_cell_length_c                   20.3189(2)
_cell_measurement_reflns_used    19728
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.8920
_cell_measurement_theta_min      2.1250
_cell_volume                     8211.01(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.710
_diffrn_measured_fraction_theta_max 0.612
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82495
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.710
_diffrn_reflns_Laue_measured_fraction_max 0.612
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43661
_diffrn_reflns_point_group_measured_fraction_full 0.710
_diffrn_reflns_point_group_measured_fraction_max 0.612
_diffrn_reflns_theta_full        29.668
_diffrn_reflns_theta_max         33.003
_diffrn_reflns_theta_min         2.354
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.69662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    0.892
_exptl_crystal_description       brown
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         12119
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1083P)^2^+4.5899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10795
_reflns_number_total             12119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Compound6.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        8211.01(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1566187
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.69662
_shelx_estimated_absorpt_t_max   1.00000
_shelx_res_checksum              29303
_shelx_hkl_checksum              29920
_shelx_fab_checksum              69911