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_7129822
_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         'C66 H78 Cl4 N6 V2, 2(C6 H6)'
_chemical_formula_sum            'C78 H90 Cl4 N6 V2'
_chemical_formula_weight         1355.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-10-08 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8968(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.2710(5)
_cell_length_b                   23.7721(4)
_cell_length_c                   13.68963(17)
_cell_measurement_reflns_used    17787
_cell_measurement_temperature    229.99(10)
_cell_measurement_theta_max      75.8710
_cell_measurement_theta_min      3.8260
_cell_volume                     7482.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (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      229.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -95.00 -52.00   1.00    4.00    --  -40.91-162.00 -17.00   43
  2  \w    -93.00 -68.00   1.00    4.00    --  -40.91 162.00  11.00   25
  3  \w    -66.00 -41.00   1.00    4.00    --  -40.91 117.00-139.00   25
  4  \w     32.00  57.00   1.00    4.00    --   40.91-117.00 133.00   25
  5  \w     70.00  95.00   1.00    4.00    --   40.91-162.00 -17.00   25
  6  \w     92.00 117.00   1.00   16.00    --  112.00-162.00 -17.00   25
  7  \w     54.00  80.00   1.00   16.00    --  112.00-117.00 133.00   26
  8  \w    115.00 140.00   1.00   16.00    --  112.00 117.00-139.00   25
  9  \w     91.00 116.00   1.00   16.00    --  112.00 162.00  11.00   25
 10  \w   -113.00 -17.00   1.00    4.00    --  -40.91 -57.00-120.00   96
 11  \w    -86.00  -6.00   1.00    4.00    --  -40.91 125.00 120.00   80
 12  \w   -104.00 -14.00   1.00    4.00    --  -40.91 -57.00 -60.00   90
 13  \w   -105.00 -16.00   1.00    4.00    --  -40.91 -38.00 -30.00   89
 14  \w     28.00  96.00   1.00    4.00    --   40.91-125.00 150.00   68
 15  \w    142.00 168.00   1.00   16.00    --  112.00  61.00  60.00   26
 16  \w    107.00 175.00   1.00   16.00    --  112.00 111.00-150.00   68
 17  \w    103.00 176.00   1.00   16.00    --  112.00  77.00 -90.00   73
 18  \w     57.00  84.00   1.00   16.00    --  112.00 -94.00 150.00   27
 19  \w     70.00 109.00   1.00   16.00    --  112.00-111.00-150.00   39
 20  \w     87.00 154.00   1.00   16.00    --  112.00  45.00-180.00   67
 21  \w    107.00 157.00   1.00   16.00    --  112.00  77.00-150.00   50
 22  \w     54.00 109.00   1.00   16.00    --  112.00-111.00 -30.00   55
 23  \w    108.00 139.00   1.00   16.00    --  112.00 111.00 120.00   31
 24  \w     54.00 138.00   1.00   16.00    --  112.00 -45.00 120.00   84
 25  \w    108.00 165.00   1.00   16.00    --  112.00 111.00-180.00   57
 26  \w     42.00 109.00   1.00   16.00    --  112.00-111.00 150.00   67
 27  \w     77.00 104.00   1.00   16.00    --  112.00 -94.00  30.00   27
 28  \w     59.00 108.00   1.00   16.00    --  112.00-111.00  30.00   49
 29  \w     43.00 109.00   1.00   16.00    --  112.00-111.00 -60.00   66
 30  \w    119.00 150.00   1.00   16.00    --  112.00 111.00  90.00   31
 31  \w     36.00  84.00   1.00   16.00    --  112.00-111.00  60.00   48
 32  \w    104.00 165.00   1.00   16.00    --  112.00  77.00-180.00   61
 33  \w     72.00 109.00   1.00   16.00    --  112.00-111.00-120.00   37
 34  \w     46.00 104.00   1.00   16.00    --  112.00-111.00 -90.00   58
 35  \w    104.00 133.00   1.00   16.00    --  112.00 111.00  60.00   29
 36  \w     45.00  72.00   1.00   16.00    --  112.00 -77.00 -30.00   27
 37  \w    103.00 129.00   1.00   16.00    --  112.00  77.00-120.00   26
 38  \w    142.00 167.00   1.00   16.00    --  112.00  77.00-120.00   25
 39  \w     71.00 109.00   1.00   16.00    --  112.00-111.00-180.00   38
 40  \w     30.00  70.00   1.00   16.00    --  112.00 -94.00  30.00   40
 41  \w     31.00 102.00   1.00   16.00    --  112.00 -94.00 -30.00   71
 42  \w    140.00 177.00   1.00   16.00    --  112.00  77.00 120.00   37
 43  \w     53.00 109.00   1.00   16.00    --  112.00-111.00  90.00   56
 44  \w     49.00  75.00   1.00   16.00    --  112.00 -94.00 -60.00   26
 45  \w    103.00 135.00   1.00   16.00    --  112.00  77.00 120.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073294000
_diffrn_orient_matrix_UB_12      0.0640178000
_diffrn_orient_matrix_UB_13      -0.0144526000
_diffrn_orient_matrix_UB_21      -0.0609982000
_diffrn_orient_matrix_UB_22      -0.0033469000
_diffrn_orient_matrix_UB_23      0.0301027000
_diffrn_orient_matrix_UB_31      0.0267250000
_diffrn_orient_matrix_UB_32      0.0094857000
_diffrn_orient_matrix_UB_33      0.1089227000
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.061
_diffrn_reflns_theta_min         3.719
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.746
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (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    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7784
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0700P)^2^+1.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6691
_reflns_number_total             7784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00768a2.cif
_cod_data_source_block           bk142
_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               7129822
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C78 H90 Cl4 N6 V2'
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.507
_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. Restrained distances
 C37-C36_$1 = C36-C35 = C34-C35_$1 = C34-C35 = C36-C35 = C37-C36
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C42(0.5) H42(0.5) C41(0.5) H41(0.5) C40(0.5) H40(0.5) C39(0.5)
 H39(0.5) C38(0.5) H38(0.5) C43(0.5) H43(0.5)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
5.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), C34(H34), C35(H35), C36(H36), C37(H37), C42(H42),
  C41(H41), C40(H40), C39(H39), C38(H38), C43(H43)
5.c Fitted hexagon refined as free rotating group:
 C42(C41,C40,C39,C38,C43)
5.d 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              47677
_shelx_hkl_checksum              14690
_olex2_date_sample_data_collection 2021-10-07
_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 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.664