Vanadium complexes with N-heterocyclic vinylidene ligands
Kooij, Bastiaan; Dong, Zhaowen; Varava, Paul; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Piveteau, Laura; Severin, Kay; Chemical Communications  (2022) –; doi:10.1039/D2CC00768A

data_7129818
_publ_section_title
;
 Vanadium complexes with N-heterocyclic vinylidene ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00768A
_journal_year                    2022
_chemical_formula_moiety         'C33 H39 Cl3 N3 V'
_chemical_formula_sum            'C33 H39 Cl3 N3 V'
_chemical_formula_weight         634.96
_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_date             2021-08-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-03 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.2322(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.08899(15)
_cell_length_b                   19.34274(17)
_cell_length_c                   14.78739(17)
_cell_measurement_reflns_used    31694
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      75.0050
_cell_measurement_theta_min      3.8450
_cell_volume                     3302.58(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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     42.00  68.00   0.50    1.00    --   65.75-125.00-150.00   52
  2  \w     39.00  68.00   0.50    1.00    --   65.75-125.00 150.00   58
  3  \w     26.00  86.00   0.50    1.00    --   65.75-125.00   0.00  120
  4  \w     36.00  62.00   0.50    1.00    --   65.75-125.00 -30.00   52
  5  \w    -60.00 -33.00   0.50    1.00    --  -67.30 125.00-150.00   54
  6  \w    -78.00 -52.00   0.50    1.00    --  -67.30 -15.00 -60.00   52
  7  \w    -97.00 -46.00   0.50    1.00    --  -67.30   0.00 150.00  102
  8  \w    -92.00 -67.00   0.50    1.00    --  -67.30 125.00  30.00   50
  9  \w    -93.00 -36.00   0.50    1.00    --  -67.30   0.00 -90.00  114
 10  \w    -92.00 -32.00   0.50    1.00    --  -67.30 125.00 -60.00  120
 11  \w    -77.00 -40.00   0.50    1.00    --  -67.30   0.00-180.00   74
 12  \w    -73.00 -41.00   0.50    1.00    --  -67.30   0.00  30.00   64
 13  \w   -109.00 -54.00   0.50    1.00    --  -67.30 -15.00  90.00  110
 14  \w    -74.00 -35.00   0.50    1.00    --  -67.30 125.00   0.00   78
 15  \w     58.00  84.00   0.50    1.00    --   72.75  15.00 -60.00   52
 16  \w     51.00 110.00   0.50    1.00    --   72.75  15.00 120.00  118
 17  \w     36.00  98.00   0.50    1.00    --   72.75-125.00 120.00  124
 18  \w     50.00 112.00   0.50    1.00    --   72.75  15.00  60.00  124
 19  \w     64.00  97.00   0.50    1.00    --   72.75-125.00  30.00   66
 20  \w    -97.00 -36.00   0.50    1.00    --  -73.25 122.00-156.57  122
 21  \w    -97.00 -36.00   0.50    1.00    --  -73.25 123.00 165.23  122
 22  \w   -113.00 -45.00   0.50    1.00    --  -73.25 149.00 115.09  136
 23  \w   -111.00 -46.00   0.50    1.00    --  -73.25 146.00  53.23  130
 24  \w     74.00  99.00   0.50    4.00    --   76.90-118.00  -1.76   50
 25  \w     37.00  69.00   0.50    4.00    --   76.90-118.00  -1.76   64
 26  \w     38.00  99.00   0.50    4.00    --   76.90-118.00 -40.03  122
 27  \w     45.00 101.00   0.50    4.00    --   76.97-125.00  60.00  112
 28  \w     77.00 102.00   0.50    4.00    --   76.97-125.00 120.00   50
 29  \w     77.00 102.00   0.50    4.00    --   76.97-125.00  30.00   50
 30  \w     50.00 119.00   0.50    4.00    --   76.97  15.00-120.00  138
 31  \w     55.00 115.00   0.50    4.00    --   76.97  15.00 -30.00  120
 32  \w     72.00 102.00   0.50    4.00    --   76.97-125.00  90.00   60
 33  \w     49.00 111.00   0.50    4.00    --   76.97  15.00-180.00  124
 34  \w     54.00 101.00   0.50    4.00    --   76.97-125.00-150.00   94
 35  \w     77.00 102.00   0.50    4.00    --   76.97-125.00 150.00   50
 36  \w     38.00  63.00   0.50    4.00    --   76.97-125.00 150.00   50
 37  \w     77.00 102.00   0.50    4.00    --   76.97-125.00 -30.00   50
 38  \w     59.00 102.00   0.50    4.00    --   76.97-125.00 -60.00   86
 39  \w     69.00 102.00   0.50    4.00    --   76.97-125.00-120.00   66
 40  \w     41.00 102.00   0.50    4.00    --   76.97-125.00 -90.00  122
 41  \w     57.00 101.00   0.50    4.00    --   76.97-125.00-180.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0810140000
_diffrn_orient_matrix_UB_12      -0.0246464000
_diffrn_orient_matrix_UB_13      -0.0958635000
_diffrn_orient_matrix_UB_21      -0.0980040000
_diffrn_orient_matrix_UB_22      0.0455186000
_diffrn_orient_matrix_UB_23      0.0145905000
_diffrn_orient_matrix_UB_31      0.0406531000
_diffrn_orient_matrix_UB_32      0.0604776000
_diffrn_orient_matrix_UB_33      -0.0499162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54724
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.658
_diffrn_reflns_theta_min         3.875
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.933
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense green'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0599P)^2^+1.4839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6266
_reflns_number_total             6754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00768a2.cif
_cod_data_source_block           bk100-2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3302.59(7)
_cod_database_code               7129818
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C33 H39 Cl3 N3 V'
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.638
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C)
;
_shelx_res_checksum              51322
_shelx_hkl_checksum              57604
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.810