Vanadium(v) arylimido alkylidene N-heterocyclic carbene complexes containing fluorinated alkoxide or halogenated phenoxide ligands for the syndiospecific ROMP of cyclic olefins
Nomura, Kotohiro; Kuwahara, Shuko; Suthala, Jirapa; Kawamoto, Yuta; Shimoyama, Daisuke; Buchmeiser, Michael R.; New Journal of Chemistry 48 (2024) 14865–14872; doi:10.1039/D4NJ02537G

data_7063350
_publ_section_title
;
 Vanadium(v) arylimido alkylidene N-heterocyclic carbene complexes
 containing fluorinated alkoxide or halogenated phenoxide ligands for the
 syndiospecific ROMP of cyclic olefins
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14865
_journal_page_last               14872
_journal_paper_doi               10.1039/D4NJ02537G
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C33 H33 Cl2 F9 N3 O Si V'
_chemical_formula_sum            'C33 H33 Cl2 F9 N3 O Si V'
_chemical_formula_weight         808.55
_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_date             2024-05-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2024-05-25 deposited with the CCDC.	2024-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.341(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1196(5)
_cell_length_b                   16.0398(5)
_cell_length_c                   15.5170(5)
_cell_measurement_reflns_used    23243
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.6220
_cell_measurement_theta_min      2.4970
_cell_volume                     3676.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00  82.00   0.25   10.00    --   -8.00  44.00 108.00  720
  2  \w    -98.00  82.00   0.25   10.00    --   -8.00  33.00 -36.00  720
  3  \w    -98.00  82.00   0.25   10.00    --   -8.00  55.00-144.00  720
  4  \w    -98.00 -19.25   0.25   10.00    --   -8.00  33.00 -72.00  315
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55266
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.927
_diffrn_reflns_theta_min         1.848
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         8811
_refine_ls_number_restraints     1018
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0818
_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^)+(0.0917P)^2^+9.0994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2234
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6310
_reflns_number_total             8811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02537g2.cif
_cod_data_source_block           20240124_cl2nvcf3ixy
_cod_depositor_comments
'Adding full bibliography for 7063350--7063351.cif.'
_cod_database_code               7063350
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Shared sites
{C11B, Si1A}
{C11A, Si1B}
2. Uiso/Uaniso restraints and constraints
F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim F7A \\sim F8A \\sim
F9A \\sim O1A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim Si1B \\sim C7B
\\sim C8B \\sim C9B \\sim C10B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Si1A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim F1B \\sim F2B \\sim F3B
\\sim F4B \\sim F5B \\sim F6B \\sim F7B \\sim F8B \\sim F9B \\sim O1B \\sim
C11B \\sim C12B \\sim C13B \\sim C14B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Cl1A \\sim Cl2A \\sim N1A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A
\\sim C6A \\sim Cl1B \\sim Cl2B \\sim N1B \\sim C1B \\sim C2B \\sim C3B \\sim
C4B \\sim C5B \\sim C6B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C11B) = Uanis(Si1A)
Uanis(C11A) = Uanis(Si1B)
3. Rigid body (RIGU) restrains
 Si1A, F1A, F2A, F3A, F4A, F5A, F6A, F7A, F8A, F9A, O1A, C7A, C8A, C9A, C10A,
 C11A, C12A, C13A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si1B, F1B, F2B, F3B, F4B, F5B, F6B, F7B, F8B, F9B, O1B, C7B, C8B, C9B, C10B,
 C11B, C12B, C13B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Si1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=
 Sof(F8B)=Sof(F9B)=Sof(O1B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=
 Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=Sof(C11B)=Sof(C12B)=Sof(C13B)=Sof(C14B)=1-FVAR(1)
 Sof(Si1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=
 Sof(F8A)=Sof(F9A)=Sof(O1A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C11A)=Sof(C12A)=Sof(C13A)=Sof(C14A)=FVAR(1)
 Sof(Cl1B)=Sof(Cl2B)=Sof(N1B)=Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=
 Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=1-FVAR(2)
 Sof(Cl1A)=Sof(Cl2A)=Sof(N1A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=FVAR(2)
5.a Me refined with riding coordinates:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C28(H28), C29(H29),
 C30(H30), C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C3B(H3B), C4B(H4B), C5B(H5B),
  C7B(H7B)
5.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C)
;
_shelx_res_checksum              96884
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;