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_7710665
_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         '3(C35 H43 N3 O),  2(C6 H6)'
_chemical_formula_sum            'C117 H141 N9 O3'
_chemical_formula_weight         1721.38
_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
_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                 97.1360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.67040(10)
_cell_length_b                   40.7623(3)
_cell_length_c                   20.19320(10)
_cell_measurement_reflns_used    47433
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.8140
_cell_measurement_theta_min      2.4900
_cell_volume                     10348.49(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            104829
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         72.129
_diffrn_reflns_theta_min         2.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.433
_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 yellow'
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       plate
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         20288
_refine_ls_number_restraints     510
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0483P)^2^+4.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17916
_reflns_number_total             20288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01250b2.cif
_cod_data_source_block           compound_20
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710665
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              80188
_shelx_hkl_checksum              52726