N-Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Complexes of Vanadium(III) and Vanadium(V)
Horrer, Günther; Mann, Sophie; Krummenacher, Ivo; Braunschweig, Holger; Radius, Udo; Dalton Transactions  (2022) –; doi:10.1039/D2DT01250B

data_7710651
_publ_section_title
;
 N-Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Complexes of
 Vanadium(III) and Vanadium(V)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01250B
_journal_year                    2022
_chemical_formula_moiety         'C24 H39 Cl3 N O V'
_chemical_formula_sum            'C24 H39 Cl3 N O V'
_chemical_formula_weight         514.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-21 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1141(2)
_cell_length_b                   14.5456(3)
_cell_length_c                   16.2000(3)
_cell_measurement_reflns_used    14588
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.5730
_cell_measurement_theta_min      4.9720
_cell_volume                     2611.48(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22237
_diffrn_reflns_point_group_measured_fraction_full 0.780
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         5.017
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.108
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense purple'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       needle
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.014(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4017
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0976P)^2^+5.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.562
_reflns_Friedel_fraction_full    0.563
_reflns_Friedel_fraction_max     0.562
_reflns_number_gt                3939
_reflns_number_total             4017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01250b2.cif
_cod_data_source_block           compound_1(thf)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7710651
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              54840
_shelx_hkl_checksum              43036