Vanadium complexes bearing 8-anilide-5,6,7-trihydroquinoline ligands for ethylene (co-)polymerization.
Wu, Ruiyao; Niu, Zhen; Xia, Zhu; He, Jianyun; Bai, Chenxi; Dalton transactions (Cambridge, England : 2003) 52 (2023) 8636–8644; doi:10.1039/d3dt01065a

data_7713284
_publ_section_title
;
 Vanadium complexes bearing 8-anilide-5,6,7-trihydroquinoline ligands for
 ethylene (co-)polymerization.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8636
_journal_page_last               8644
_journal_paper_doi               10.1039/d3dt01065a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C21 H25 Br Cl3 N2 O V'
_chemical_formula_sum            'C21 H25 Br Cl3 N2 O V'
_chemical_formula_weight         558.63
_chemical_name_systematic        1
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-06 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   35.6823(3)
_cell_length_b                   35.6823(3)
_cell_length_c                   13.3003(2)
_cell_measurement_reflns_used    20820
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.8190
_cell_measurement_theta_min      2.4620
_cell_volume                     14665.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.977
_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     85.00 173.00   0.50    0.05    --  111.82  61.00 -30.00  176
  2  \w    133.00 168.00   0.50    0.05    --  111.82  61.00 -90.00   70
  3  \w    131.00 156.00   0.50    0.05    --  111.82  61.00-150.00   50
  4  \w     83.00 119.00   0.50    0.05    --  111.82  61.00-150.00   72
  5  \w     85.00 124.00   0.50    0.05    --  111.82  61.00 -90.00   78
  6  \w    112.00 172.00   0.50    0.05    --  111.82  30.00 -60.00  120
  7  \w    105.00 172.00   0.50    0.05    --  111.82   0.00  90.00  134
  8  \w    125.00 157.00   0.50    0.05    --  111.82  30.00 150.00   64
  9  \w     76.00 102.00   0.50    0.05    --  111.82  30.00 150.00   52
 10  \w     66.00  95.00   0.50    0.05    --  111.82   0.00  90.00   58
 11  \w     28.00  62.00   0.50    0.05    --  111.82   0.00  90.00   68
 12  \w     18.00  98.00   0.50    0.05    --   39.45-125.00  90.00  160
 13  \w     -9.00  20.00   0.50    0.05    --   39.45 -90.00-114.00   58
 14  \w     24.00  50.00   0.50    0.05    --   39.45 -90.00-114.00   52
 15  \w     46.00  95.00   0.50    0.05    --   39.45-125.00-150.00   98
 16  \w     59.00  96.00   0.50    0.05    --  111.82 -90.00-114.00   74
 17  \w     81.00 108.00   0.50    0.05    --  111.82-111.00-150.00   54
 18  \w     57.00 105.00   0.50    0.05    --  111.82-111.00 -30.00   96
 19  \w     78.00 105.00   0.50    0.05    --  111.82-111.00   0.00   54
 20  \w     79.00 105.00   0.50    0.05    --  111.82-111.00 120.00   52
 21  \w     83.00 108.00   0.50    0.05    --  111.82-111.00 150.00   50
 22  \w     32.00  71.00   0.50    0.05    --  111.82-111.00 150.00   78
 23  \w     32.00  58.00   0.50    0.05    --  111.82-111.00 120.00   52
 24  \w     74.00  99.00   0.50    0.05    --  111.82-111.00  60.00   50
 25  \w     61.00  90.00   0.50    0.05    --  111.82 -94.00  60.00   58
 26  \w     33.00  58.00   0.50    0.05    --  111.82 -94.00  60.00   50
 27  \w     36.00 105.00   0.50    0.05    --  111.82 -94.00  90.00  138
 28  \w     74.00 104.00   0.50    0.05    --  111.82 -94.00   0.00   60
 29  \w     35.00  63.00   0.50    0.05    --  111.82 -94.00   0.00   56
 30  \w     75.00 104.00   0.50    0.05    --  111.82 -94.00 -90.00   58
 31  \w     32.00  68.00   0.50    0.05    --  111.82-111.00-150.00   72
 32  \w     37.00 102.00   0.50    0.05    --  111.82 -94.00-180.00  130
 33  \w     55.00  87.00   0.50    0.05    --  111.82 -77.00-120.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0140129000
_diffrn_orient_matrix_UB_12      -0.0285560000
_diffrn_orient_matrix_UB_13      -0.0949931000
_diffrn_orient_matrix_UB_21      -0.0296072000
_diffrn_orient_matrix_UB_22      0.0180663000
_diffrn_orient_matrix_UB_23      -0.0299965000
_diffrn_orient_matrix_UB_31      0.0375643000
_diffrn_orient_matrix_UB_32      0.0366448000
_diffrn_orient_matrix_UB_33      -0.0591712000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31779
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.764
_diffrn_reflns_theta_min         2.477
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             5076
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0484P)^2^+22.2878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5824
_reflns_number_total             6633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01065a2.cif
_cod_data_source_block           ebls-2-100k_auto_sq
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7713284
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.666
_diffrn_oxdiff_digest_frames
;
019541ee55621a0be2b02c49d6513e17d700118576f
;
_diffrn_oxdiff_digest_hkl
;
01192307a2ab40792d6ff8009b7a1834b18eed
;
_reflns_odcompleteness_completeness 98.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C12 \\sim C15 \\sim C11 \\sim C10: within 2.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
3. Others
 Fixed Sof: Br1A(0.25) Br1B(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C12(H12), C14(H14)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              5591
_shelx_fab_checksum              8115
_platon_squeeze_void_probe_radius 1.20
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.677