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_7710661
_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         'C28 H31 Cl3 N3 V'
_chemical_formula_sum            'C28 H31 Cl3 N3 V'
_chemical_formula_weight         566.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                92.430(2)
_cell_angle_beta                 99.959(2)
_cell_angle_gamma                94.631(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2007(2)
_cell_length_b                   10.9533(2)
_cell_length_c                   15.7167(4)
_cell_measurement_reflns_used    18205
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2300
_cell_measurement_theta_min      2.8470
_cell_volume                     1383.65(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'PhotonJet R (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27628
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    5.822
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.96a (Rigaku Oxford Diffraction, 2021) 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 red'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0461P)^2^+0.5804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4931
_reflns_number_total             5418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01250b2.cif
_cod_data_source_block           compound_19
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H62 Cl6 N6 V2'
_cod_original_formula_weight         1133.69
_cod_original_formula_moiety         'C56 H62 Cl6 N6 V2'
_cod_original_formula_units_Z            1
_cod_database_code               7710661
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.475
_shelx_estimated_absorpt_t_max   0.801
_shelx_res_checksum              77333
_shelx_hkl_checksum              93174