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_7129820
_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         'C28 H36 Cl3 N2 V, C6 H6'
_chemical_formula_sum            'C34 H42 Cl3 N2 V'
_chemical_formula_weight         635.98
_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             2021-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-27 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.312(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7785(3)
_cell_length_b                   9.29150(18)
_cell_length_c                   22.4036(4)
_cell_measurement_reflns_used    7502
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5500
_cell_measurement_theta_min      3.6830
_cell_volume                     3398.82(11)
_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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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    -16.00  30.00   1.00   12.50    --  -43.50  81.00-130.00   46
  2  \w      3.00  28.00   1.00   12.50    --   43.68 -81.00 106.00   25
  3  \w     52.00 101.00   1.00   50.00    --  103.26 -81.00 106.00   49
  4  \w    106.00 178.00   1.00   50.00    --  103.26  81.00-130.00   72
  5  \w    -59.00  -6.00   1.00   12.50    --  -43.50 125.00 -60.00   53
  6  \w   -103.00 -18.00   1.00   12.50    --  -43.50 -57.00  60.00   85
  7  \w      7.00  84.00   1.00   12.50    --   43.68 -99.00 -90.00   77
  8  \w    103.00 175.00   1.00   50.00    --  103.26  77.00  90.00   72
  9  \w    116.00 148.00   1.00   50.00    --  103.26 125.00 -90.00   32
 10  \w     34.00  84.00   1.00   50.00    --  103.26 -61.00 -30.00   50
 11  \w    115.00 176.00   1.00   50.00    --  103.26  77.00 -60.00   61
 12  \w    116.00 143.00   1.00   50.00    --  103.26 125.00  30.00   27
 13  \w     86.00 166.00   1.00   50.00    --  103.26  45.00-150.00   80
 14  \w    134.00 159.00   1.00   50.00    --  103.26  77.00 120.00   25
 15  \w     40.00  67.00   1.00   50.00    --  103.26-125.00  90.00   27
 16  \w     99.00 125.00   1.00   50.00    --  103.26 -77.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356587000
_diffrn_orient_matrix_UB_12      -0.0837573000
_diffrn_orient_matrix_UB_13      -0.0594811000
_diffrn_orient_matrix_UB_21      -0.0862235000
_diffrn_orient_matrix_UB_22      0.0112881000
_diffrn_orient_matrix_UB_23      0.0126685000
_diffrn_orient_matrix_UB_31      -0.0140823000
_diffrn_orient_matrix_UB_32      0.1425767000
_diffrn_orient_matrix_UB_33      -0.0360194000
_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     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.529
_diffrn_reflns_theta_min         3.737
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.784
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.712
_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 light green'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.9668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5506
_reflns_number_total             6581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00768a2.cif
_cod_data_source_block           bk122
_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        3398.82(12)
_cod_database_code               7129820
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C34 H42 Cl3 N2 V'
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.621
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
C31A \\sim C31B \\sim C32A \\sim C32B \\sim C33A \\sim C33B \\sim C34A \\sim
C34B \\sim C35A \\sim C35B \\sim C36A \\sim C36B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33B)=Sof(C34B)=
 Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=
 Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
 C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B)
4.c Fitted hexagon refined as free rotating group:
 C31A(C32A,C33A,C34A,C35A,C36A), C31B(C32B,C33B,C34B,C35B,C36B)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              12858
_shelx_hkl_checksum              38094
_olex2_date_sample_data_collection 2021-08-26
_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 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.891