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_7720470
_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         'C50 H50 N4 O3 V'
_chemical_formula_sum            'C50 H50 N4 O3 V'
_chemical_formula_weight         805.88
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2023-05-18
_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                 96.2020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.39860(10)
_cell_length_b                   22.0578(3)
_cell_length_c                   11.60800(10)
_cell_measurement_reflns_used    16465
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      74.9460
_cell_measurement_theta_min      4.0030
_cell_volume                     2137.85(4)
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_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   -119.00 -52.00   0.50    1.50    --  -48.43-160.00-152.00  134
  2  \w     39.00 117.00   0.50    1.50    --   48.43-160.00-152.00  156
  3  \w     19.00  87.00   0.50    1.50    --   48.43-117.00  -1.00  136
  4  \w     58.00 119.00   0.50    1.50    --   48.43 160.00-122.00  122
  5  \w     32.00 109.00   0.50    6.00    --  100.00-117.00  -1.00  154
  6  \w     39.00 135.00   0.50    6.00    --  100.00-160.00-152.00  192
  7  \w     58.00 158.00   0.50    6.00    --  100.00 160.00-122.00  200
  8  \w   -170.00 -81.00   0.50    6.00    -- -102.00-117.00  -1.00  178
  9  \w    -95.00 -52.00   0.50    6.00    -- -102.00 160.00-122.00   86
 10  \w   -106.00 -70.00   0.50    6.00    -- -102.00 117.00  86.00   72
 11  \w    -22.00  19.00   0.50    1.50    --  -48.43  19.00  30.00   82
 12  \w    -24.00   2.00   0.50    1.50    --  -48.43  19.00   0.00   52
 13  \w    -17.00  20.00   0.50    1.50    --  -48.43  19.00-120.00   74
 14  \w    -23.00  27.00   0.50    1.50    --   48.43 -19.00 150.00  100
 15  \w     94.00 172.00   0.50    6.00    --  100.00  30.00  90.00  156
 16  \w     58.00 112.00   0.50    6.00    --  100.00-125.00  60.00  108
 17  \w    133.00 171.00   0.50    6.00    --  100.00  45.00  60.00   76
 18  \w     28.00 102.00   0.50    6.00    --  100.00 -94.00-180.00  148
 19  \w     98.00 124.00   0.50    6.00    --  100.00  45.00  60.00   52
 20  \w     28.00  86.00   0.50    6.00    --  100.00 -94.00   0.00  116
 21  \w     39.00  66.00   0.50    6.00    --  100.00 -61.00   0.00   54
 22  \w    -68.00 -31.00   0.50    6.00    -- -102.00  61.00  90.00   74
 23  \w   -174.00-140.00   0.50    6.00    -- -102.00 -15.00-120.00   68
 24  \w    -69.00 -32.00   0.50    6.00    -- -102.00  61.00 -60.00   74
 25  \w    -68.00 -33.00   0.50    6.00    -- -102.00  61.00 -90.00   70
 26  \w     54.00  79.00   0.50    1.50    --   48.43-160.00-152.00   50
 27  \w   -119.00 -28.00   0.50    1.50    --  -48.43 -77.00 -90.00  182
 28  \w   -119.00 -28.00   0.50    1.50    --  -48.43 -77.00 150.00  182
 29  \w     36.00 119.00   0.50    1.50    --   48.43  57.00  30.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0543604000
_diffrn_orient_matrix_UB_12      -0.0508211000
_diffrn_orient_matrix_UB_13      0.0779356000
_diffrn_orient_matrix_UB_21      0.0920146000
_diffrn_orient_matrix_UB_22      -0.0468256000
_diffrn_orient_matrix_UB_23      -0.0659565000
_diffrn_orient_matrix_UB_31      0.1504013000
_diffrn_orient_matrix_UB_32      0.0100957000
_diffrn_orient_matrix_UB_33      0.0859940000
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25035
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.121
_diffrn_reflns_theta_min         4.008
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77972
_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            'dark green'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       blade
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4275
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0584P)^2^+0.4104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3931
_reflns_number_total             4275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02846a2.cif
_cod_data_source_block           1
_cod_database_code               7720470
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H40 N4 O4 V Al'
_chemical_oxdiff_usercomment     'NONMe V'
_reflns_odcompleteness_completeness 99.48
_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
2. Restrained distances
 C18-C23 \\sim C18A-C23A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C23-C22 \\sim C23A-C22A
 with sigma of 0.02
 C23-C25 \\sim C23A-C25A
 with sigma of 0.02
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C19-C24 \\sim C19A-C24A
 with sigma of 0.02
 C23-C19 \\sim C23A-C19A
 with sigma of 0.04
 C20-C24 \\sim C20A-C24A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C18-C22 \\sim C18A-C22A
 with sigma of 0.04
 C18-C24 \\sim C18A-C24A
 with sigma of 0.04
 C18-C25 \\sim C18A-C25A
 with sigma of 0.04
 C22-C25 \\sim C22A-C25A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C21-C19 \\sim C21A-C19A
 with sigma of 0.04
 N2-C18A \\sim N2-C18
 with sigma of 0.02
3. Others
 Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=FVAR(1)
 Fixed Sof: V1(0.5) O2(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C17(H17), C20(H20),
 C20A(H20A), C21(H21), C21A(H21A), C22(H22), C22A(H22A)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C24A(H24D,H24E,H24F), C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              8171
_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 2.169
_oxdiff_exptl_absorpt_empirical_full_min 0.722