Phenoxybis(imine) complexes of vanadium: structure, ethylene polymerization, and ring opening polymerization of ε-caprolactone.
Gong, Yi; Shibata, Kaname; Michiue, Kenji; Gbertyo, Joseph; Rais, Zaid; Elsegood, Mark R. J.; Prior, Timothy J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1866–1881; doi:10.1039/d5dt02846a

data_7720468
_publ_section_title
;
 Phenoxybis(imine) complexes of vanadium: structure, ethylene
 polymerization, and ring opening polymerization of &#x3b5;-caprolactone.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1866
_journal_page_last               1881
_journal_paper_doi               10.1039/d5dt02846a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C21 H8 F10 N2 O'
_chemical_formula_sum            'C21 H8 F10 N2 O'
_chemical_formula_weight         494.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.970(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1845(7)
_cell_length_b                   5.03630(10)
_cell_length_c                   19.2407(7)
_cell_measurement_reflns_used    15395
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.6810
_cell_measurement_theta_min      4.6100
_cell_volume                     1829.56(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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     44.00 123.00   0.50    4.50    --   51.51  37.00 116.00  158
  2  \w    -40.00  17.00   0.50    4.50    --  -55.01  37.00 116.00  114
  3  \w   -126.00 -48.00   0.50    4.50    --  -55.01 -37.00 -39.00  156
  4  \w   -151.00 -72.00   0.50   16.00    --  -79.37 -37.00 -39.00  158
  5  \w    -40.00  -8.00   0.50   16.00    --  -79.37  37.00 116.00   64
  6  \w     76.00 155.00   0.50   16.00    --   83.47  37.00 116.00  158
  7  \w     12.00  44.00   0.50   16.00    --   83.47 -37.00 -39.00   64
  8  \w     -8.00  20.00   0.50    4.50    --   20.00  97.00 112.54   56
  9  \w    -18.00  28.00   0.50    4.50    --   51.51 -19.00 150.00   92
 10  \w    -19.00  44.00   0.50    4.50    --   51.51 -37.00 -39.00  126
 11  \w    -24.00  15.00   0.50    4.50    --  -55.01  19.00  60.00   78
 12  \w     12.00  44.00   0.50   16.00    --   83.47 -37.00-150.00   64
 13  \w     12.00  44.00   0.50   16.00    --   83.47 -37.00-180.00   64
 14  \w     16.00  68.00   0.50   16.00    --   83.47 -57.00 150.00  104
 15  \w     12.00  44.00   0.50   16.00    --   83.47 -37.00-120.00   64
 16  \w     30.00  98.00   0.50   16.00    --   92.00 -74.00 -55.54  136
 17  \w     21.00  52.00   0.50   16.00    --   92.00 -44.00   6.87   62
 18  \w     31.00 114.00   0.50   16.00    --   92.00 -85.00-138.04  166
 19  \w     31.00 105.00   0.50   16.00    --   92.00 -93.00 152.45  148
 20  \w     55.00 148.00   0.50   16.00    --   92.00   1.00  -3.96  186
 21  \w     76.00 108.00   0.50   16.00    --   92.00-121.00 146.68   64
 22  \w     40.00  66.00   0.50   16.00    --   92.00-121.00 146.68   52
 23  \w     36.00  82.00   0.50   16.00    --   92.00 -75.00  49.14   92
 24  \w     32.00  57.00   0.50   16.00    --   92.00 -76.00 -11.32   50
 25  \w     68.00  94.00   0.50   16.00    --   92.00 -76.00 -11.32   52
 26  \w     31.00  56.00   0.50   16.00    --   92.00 -74.00   5.48   50
 27  \w     35.00  74.00   0.50    4.50    --   51.51  77.00-180.00   78
 28  \w     13.00  38.00   0.50    4.50    --   36.00  87.00 163.69   50
 29  \w    -11.00  19.00   0.50    4.50    --   51.51 -19.00 -30.00   60
 30  \w    -86.00 -45.00   0.50    4.50    --  -60.00 -74.00-131.73   82
 31  \w    -89.00 -63.00   0.50   16.00    --  -79.37 -77.00 -90.00   52
 32  \w     90.00 116.00   0.50   16.00    --   83.47  57.00-150.00   52
 33  \w     33.00  59.00   0.50   16.00    --   83.47 -57.00  60.00   52
 34  \w     67.00  92.00   0.50   16.00    --   83.47  77.00-120.00   50
 35  \w     13.00  39.00   0.50   16.00    --   83.47 -37.00   0.00   52
 36  \w     67.00  97.00   0.50   16.00    --   83.47  77.00-180.00   60
 37  \w     75.00 101.00   0.50   16.00    --   83.47  77.00 150.00   52
 38  \w    -66.00 -35.00   0.50   16.00    --  -88.00 110.00  84.83   62
 39  \w   -103.00 -77.00   0.50   16.00    --  -88.00 110.00  84.83   52
 40  \w   -145.00 -79.00   0.50   16.00    --  -88.00 -76.00-106.53  132
 41  \w   -112.00 -82.00   0.50   16.00    --  -88.00 -69.00 -95.17   60
 42  \w   -104.00 -78.00   0.50   16.00    --  -88.00 -73.00-133.12   52
 43  \w   -121.00 -89.00   0.50   16.00    --  -88.00 -96.00-129.06   64
 44  \w    119.00 145.00   0.50   16.00    --   92.00  54.00  20.00   52
 45  \w     89.00 151.00   0.50   16.00    --   92.00  91.00 143.54  124
 46  \w     33.00  70.00   0.50   16.00    --   92.00   8.00  35.64   74
 47  \w     86.00 112.00   0.50   16.00    --   92.00  47.00 -15.06   52
 48  \w     98.00 132.00   0.50   16.00    --   92.00 113.00-162.75   68
 49  \w    105.00 131.00   0.50   16.00    --   92.00  13.00-122.87   52
 50  \w      5.00  33.00   0.50    4.50    --   32.00  94.00 -83.61   56
 51  \w     13.00  42.00   0.50    4.50    --   36.00  87.00 -50.99   58
 52  \w     12.00  42.00   0.50    4.50    --   36.00  90.00-178.13   60
 53  \w     16.00  42.00   0.50    4.50    --   40.00  89.00  21.04   52
 54  \w   -126.00 -48.00   0.50    4.50    --  -64.00 -75.00  57.61  156
 55  \w   -127.00 -63.00   0.50    4.50    --  -64.00 -72.00 145.38  128
 56  \w   -134.00 -57.00   0.50    4.50    --  -68.00 -63.00 -64.88  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0151621000
_diffrn_orient_matrix_UB_12      0.1136271000
_diffrn_orient_matrix_UB_13      -0.0803882000
_diffrn_orient_matrix_UB_21      0.0777333000
_diffrn_orient_matrix_UB_22      0.0904199000
_diffrn_orient_matrix_UB_23      0.0328807000
_diffrn_orient_matrix_UB_31      0.0197308000
_diffrn_orient_matrix_UB_32      -0.2692141000
_diffrn_orient_matrix_UB_33      -0.0228572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31527
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.664
_diffrn_reflns_theta_min         4.596
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0784P)^2^+0.4103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3088
_reflns_number_total             3642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02846a2.cif
_cod_data_source_block           pMeL5H
_cod_original_cell_volume        1829.56(11)
_cod_database_code               7720468
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H10 F10 N2 O4 V Al'
_chemical_oxdiff_usercomment     NONC6F5V
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.734
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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, All O(H) groups
2. Restrained distances
 C8-H8 = C3-H3 = C5-H5 = C15-H15
 0.97305 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates and stretchable bonds:
 C3(H3), C5(H5), C8(H8), C15(H15)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
3.c Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O1(H1)
;
_shelx_res_checksum              62716
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.496