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_7129821
_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         'C39 H57 Cl2 N4 Si2 V'
_chemical_formula_sum            'C39 H57 Cl2 N4 Si2 V'
_chemical_formula_weight         759.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.8825(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1641(2)
_cell_length_b                   12.35741(14)
_cell_length_c                   24.0239(3)
_cell_measurement_reflns_used    18924
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.8440
_cell_measurement_theta_min      3.0670
_cell_volume                     4284.32(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(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 0.970
_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     22.00  65.00   0.50    1.00    --   59.87-104.00-139.00   86
  2  \w    -54.00 -21.00   0.50    1.00    --  -62.28 104.00 -39.00   66
  3  \w    -63.00 -28.00   0.50    1.00    --  -71.26 104.00 -39.00   70
  4  \w     35.00  60.00   0.50    2.00    --   71.88-104.00-139.00   50
  5  \w     57.00  91.00   0.50    2.00    --   73.64-104.00-139.00   68
  6  \w    -83.00 -35.00   0.50    2.00    --  -76.11 104.00 -39.00   96
  7  \w     73.00  98.00   0.50    2.00    --   81.22-104.00-139.00   50
  8  \w     11.00  36.00   0.50    1.00    --   59.87 -30.00-180.00   50
  9  \w     11.00  36.00   0.50    1.00    --   59.87 -30.00 -60.00   50
 10  \w     61.00 104.00   0.50    1.00    --   59.87  30.00 120.00   86
 11  \w   -112.00 -63.00   0.50    1.00    --  -62.28 -30.00-150.00   98
 12  \w   -112.00 -69.00   0.50    1.00    --  -62.28 -30.00 -90.00   86
 13  \w   -110.00 -45.00   0.50    1.00    --  -71.26   0.00 -90.00  130
 14  \w   -102.00 -76.00   0.50    1.00    --  -71.26 -30.00 120.00   52
 15  \w   -111.00 -85.00   0.50    1.00    --  -71.26 -30.00-180.00   52
 16  \w   -119.00 -75.00   0.50    1.00    --  -71.26 -30.00-120.00   88
 17  \w     76.00 113.00   0.50    2.00    --   71.88  30.00 -90.00   74
 18  \w     74.00 111.00   0.50    2.00    --   71.88  30.00 150.00   74
 19  \w     35.00  67.00   0.50    2.00    --   73.64 -95.00 -90.00   64
 20  \w     34.00  80.00   0.50    2.00    --   73.64 -95.00 150.00   92
 21  \w     36.00  82.00   0.50    2.00    --   73.64 -95.00  90.00   92
 22  \w   -125.00 -81.00   0.50    2.00    --  -76.11 -30.00   0.00   88
 23  \w   -105.00 -33.00   0.50    2.00    --  -76.11 125.00 -90.00  144
 24  \w   -107.00 -34.00   0.50    2.00    --  -76.11 125.00   0.00  146
 25  \w   -122.00 -97.00   0.50    2.00    --  -76.11-125.00 -60.00   50
 26  \w     84.00 110.00   0.50    2.00    --   81.22-125.00 150.00   52
 27  \w     37.00  80.00   0.50    2.00    --   81.22-125.00 150.00   86
 28  \w     41.00  73.00   0.50    2.00    --   81.22 -95.00  30.00   64
 29  \w     52.00  77.00   0.50    2.00    --   81.22-125.00 -60.00   50
 30  \w    100.00 125.00   0.50    2.00    --   81.22 125.00 150.00   50
 31  \w     97.00 131.00   0.50    2.00    --   81.22  30.00-150.00   68
 32  \w     99.00 126.00   0.50    2.00    --   81.22 125.00-180.00   54
 33  \w     44.00 116.00   0.50    2.00    --   81.22   0.00-180.00  144
 34  \w     80.00 112.00   0.50    2.00    --   81.22-125.00 -60.00   64
 35  \w     87.00 112.00   0.50    2.00    --   81.22-125.00  30.00   50
 36  \w     38.00 111.00   0.50    2.00    --   81.22-125.00-150.00  146
 37  \w     54.00  79.00   0.50    2.00    --   81.22-125.00-180.00   50
 38  \w     87.00 129.00   0.50    2.00    --   81.22  30.00-180.00   84
 39  \w     65.00  90.00   0.50    2.00    --   81.22 -95.00-150.00   50
 40  \w     87.00 112.00   0.50    2.00    --   81.22-125.00-180.00   50
 41  \w     52.00  81.00   0.50    2.00    --   81.22-125.00 -30.00   58
;
_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      0.0850139000
_diffrn_orient_matrix_UB_12      0.0674935000
_diffrn_orient_matrix_UB_13      -0.0008493000
_diffrn_orient_matrix_UB_21      0.0174642000
_diffrn_orient_matrix_UB_22      0.0295626000
_diffrn_orient_matrix_UB_23      0.0648019000
_diffrn_orient_matrix_UB_31      0.0620933000
_diffrn_orient_matrix_UB_32      -0.1005872000
_diffrn_orient_matrix_UB_33      0.0184605000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56762
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.496
_diffrn_reflns_theta_min         3.079
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.842
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (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 dark yellow'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0802P)^2^+1.9346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7129
_reflns_number_total             8625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00768a2.cif
_cod_data_source_block           bk183
_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_database_code               7129821
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C39 H57 Cl2 N4 Si2 V'
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.485
_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:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              80166
_shelx_hkl_checksum              92416
_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 1.825
_oxdiff_exptl_absorpt_empirical_full_min 0.564