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_7129819
_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         'C45 H66 Cl3 N3 P V, 1[C4H8O]'
_chemical_formula_sum            'C45 H66 Cl3 N3 P V'
_chemical_formula_weight         837.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-17 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                84.755(3)
_cell_angle_beta                 81.999(5)
_cell_angle_gamma                67.677(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3015(6)
_cell_length_b                   11.6166(3)
_cell_length_c                   20.8002(9)
_cell_measurement_reflns_used    9104
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      69.2520
_cell_measurement_theta_min      4.0910
_cell_volume                     2499.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     25.00  59.00   0.50    4.00    --   59.56-107.00  39.00   68
  2  \w    -58.00 -22.00   0.50    4.00    --  -62.07 107.00 136.00   72
  3  \w    -84.00 -59.00   0.50    4.00    --  -71.26 107.00 136.00   50
  4  \w     52.00  93.00   0.50    4.00    --   73.45-107.00  39.00   82
  5  \w    -57.00 -32.00   0.50    4.00    --  -75.95 107.00 136.00   50
  6  \w    -95.00 -62.00   0.50    4.00    --  -75.95 107.00 136.00   66
  7  \w     69.00  96.00   0.50    4.00    --   81.22-107.00  39.00   54
  8  \w     11.00  37.00   0.50    4.00    --   59.56 -30.00  30.00   52
  9  \w     10.00  37.00   0.50    4.00    --   59.56 -30.00  90.00   54
 10  \w     10.00  35.00   0.50    4.00    --   59.56 -30.00-120.00   50
 11  \w     10.00  36.00   0.50    4.00    --   59.56 -30.00-150.00   52
 12  \w     10.00  36.00   0.50    4.00    --   59.56 -30.00-180.00   52
 13  \w     22.00  48.00   0.50    4.00    --   59.56 -95.00 -90.00   52
 14  \w   -111.00 -86.00   0.50    4.00    --  -62.07 -30.00-150.00   50
 15  \w   -100.00 -66.00   0.50    4.00    --  -62.07 -30.00  60.00   68
 16  \w   -111.00 -84.00   0.50    4.00    --  -71.26 -30.00 -60.00   54
 17  \w   -109.00 -75.00   0.50    4.00    --  -71.26 -30.00   0.00   68
 18  \w   -116.00 -72.00   0.50    4.00    --  -71.26 -30.00 120.00   88
 19  \w     35.00  74.00   0.50    4.00    --   71.88 -95.00 -90.00   78
 20  \w     34.00  70.00   0.50    4.00    --   71.88 -95.00  90.00   72
 21  \w     36.00  61.00   0.50    4.00    --   71.88-107.00  39.00   50
 22  \w     75.00 122.00   0.50    4.00    --   73.45  30.00  30.00   94
 23  \w     75.00 123.00   0.50    4.00    --   73.45  30.00 -30.00   96
 24  \w     35.00  83.00   0.50    4.00    --   73.45 -95.00 -30.00   96
 25  \w     28.00 104.00   0.50    4.00    --   73.45-125.00-180.00  152
 26  \w   -121.00 -77.00   0.50    4.00    --  -75.95-125.00  30.00   88
 27  \w   -107.00 -32.00   0.50    4.00    --  -75.95 125.00-180.00  150
 28  \w   -125.00-100.00   0.50    4.00    --  -75.95 -30.00  90.00   50
 29  \w   -122.00 -74.00   0.50    4.00    --  -75.95-125.00 120.00   96
 30  \w   -120.00 -74.00   0.50    4.00    --  -75.95-125.00 150.00   92
 31  \w   -125.00 -99.00   0.50    4.00    --  -75.95 -30.00-180.00   52
 32  \w     86.00 112.00   0.50    4.00    --   81.22-125.00 -90.00   52
 33  \w     90.00 131.00   0.50    4.00    --   81.22  30.00   0.00   82
 34  \w     86.00 112.00   0.50    4.00    --   81.22-125.00   0.00   52
 35  \w     38.00  64.00   0.50    4.00    --   81.22-125.00   0.00   52
 36  \w     87.00 128.00   0.50    4.00    --   81.22  30.00 -60.00   82
 37  \w     41.00  78.00   0.50    4.00    --   81.22 -95.00-150.00   74
 38  \w     91.00 122.00   0.50    4.00    --   81.22 125.00 -30.00   62
 39  \w     44.00 110.00   0.50    4.00    --   81.22-125.00  90.00  132
 40  \w     41.00  79.00   0.50    4.00    --   81.22 -95.00 -60.00   76
 41  \w     51.00 112.00   0.50    4.00    --   81.22-125.00 150.00  122
 42  \w     82.00 130.00   0.50    4.00    --   81.22  30.00  60.00   96
;
_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      -0.0883858000
_diffrn_orient_matrix_UB_12      -0.0743124000
_diffrn_orient_matrix_UB_13      0.0032232000
_diffrn_orient_matrix_UB_21      -0.0410337000
_diffrn_orient_matrix_UB_22      0.0266669000
_diffrn_orient_matrix_UB_23      0.0726078000
_diffrn_orient_matrix_UB_31      -0.1118101000
_diffrn_orient_matrix_UB_32      0.1198149000
_diffrn_orient_matrix_UB_33      -0.0179333000
_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  0.0727
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30255
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         4.118
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.658
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (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 yellow'
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       plate
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8894
_refine_ls_number_restraints     1141
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0931
_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^)+(0.1613P)^2^+2.0650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2637
_refine_ls_wR_factor_ref         0.2894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5416
_reflns_number_total             8894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00768a2.cif
_cod_data_source_block           bk212
_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               7129819
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C49 H74 Cl3 N3 OP V'
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45B-C44B
 1.52 with sigma of 0.02
 C35A-C34A = C35B-C34B = C36A-C35A = C35B-C36B = C36A-C37A = C37B-C36B
 1.52 with sigma of 0.02
 C38A-C39A = C38B-C39B = C40A-C39A = C39B-C40B = C40A-C41A = C40B-C41B
 1.52 with sigma of 0.02
 C42A-C43A = C42B-C43B = C44A-C43A = C44B-C43B = C45A-C44A
 1.52 with sigma of 0.02
 V1B-Cl2B = V1B-Cl1B = V1B-Cl3B
 2.3 with sigma of 0.02
 C34A-C36A = C35A-C37A
 2.5 with sigma of 0.04
 C38B-C40B = C39B-C41B
 2.5 with sigma of 0.04
 C38A-C40A = C39A-C41A
 2.5 with sigma of 0.04
 C34B-C36B = C35B-C37B
 2.5 with sigma of 0.04
 C42A-C44A = C43A-C45A
 2.5 with sigma of 0.04
 C42B-C44B = C45B-C43B
 2.5 with sigma of 0.04
 V1A-Cl3A \\sim V1A-Cl2A \\sim V1A-Cl1A
 with sigma of 0.02
 P1-C42A \\sim P1-C42B \\sim P1-C34A \\sim P1-C34B \\sim P1-C38A \\sim P1-C38B
 with sigma of 0.02
 V1A-P1 \\sim V1B-P1
 with sigma of 0.02
 V1A-C3 \\sim V1B-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(V1B)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=Sof(C34B)=Sof(H34C)=Sof(H34D)=
 Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=
 Sof(H39C)=Sof(H39D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41D)=
 Sof(H41E)=Sof(H41F)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=
 Sof(H43D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=1-FVAR(1)
 Sof(V1A)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=
 Sof(H39A)=Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=
 Sof(H41B)=Sof(H41C)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=
 Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(C45A)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C34A(H34A,H34B), C34B(H34C,H34D), C35A(H35A,H35B), C35B(H35C,H35D), C36A(H36A,
 H36B), C36B(H36C,H36D), C38A(H38A,H38B), C38B(H38C,H38D), C39A(H39A,H39B),
 C39B(H39C,H39D), C40A(H40A,H40B), C40B(H40C,H40D), C42A(H42A,H42B), C42B(H42C,
 H42D), C43A(H43A,H43B), C43B(H43C,H43D), C44A(H44A,H44B), C44B(H44C,H44D)
6.c Me refined with riding coordinates:
 C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C41A(H41A,H41B,H41C), C41B(H41D,
 H41E,H41F), C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F)
6.d 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)
6.e 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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7285
_shelx_hkl_checksum              26105
_shelx_fab_checksum              46858
_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 2.909
_oxdiff_exptl_absorpt_empirical_full_min 0.278