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_7720466
_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         'C29 H34 N2 O'
_chemical_formula_sum            'C29 H34 N2 O'
_chemical_formula_weight         426.58
_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
_audit_creation_date             2023-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                74.785(2)
_cell_angle_beta                 81.0860(10)
_cell_angle_gamma                80.4970(10)
_cell_formula_units_Z            4
_cell_length_a                   10.4654(2)
_cell_length_b                   14.8091(2)
_cell_length_c                   16.8078(3)
_cell_measurement_reflns_used    23242
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.6000
_cell_measurement_theta_min      3.0910
_cell_volume                     2462.01(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_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, 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 0.996
_diffrn_measured_fraction_theta_max 0.954
_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    -82.00  -9.00   0.50    1.00    --  -45.18 114.00  92.00  146
  2  \w      4.00  82.00   0.50    1.00    --   45.18-114.00   2.00  156
  3  \w    -97.00 -27.00   0.50    4.00    --  -97.00 114.00  92.00  140
  4  \w   -166.00-100.00   0.50    4.00    --  -97.00-114.00   2.00  132
  5  \w     94.00 175.00   0.50    4.00    --  109.75 114.00  92.00  162
  6  \w     40.00  97.00   0.50    4.00    --  109.75-114.00   2.00  114
  7  \w    -65.00  18.00   0.50    1.00    --  -45.18  77.00  30.00  166
  8  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00 150.00   90
  9  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00 -90.00   90
 10  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00  30.00   90
 11  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00-150.00   90
 12  \w     39.00 120.00   0.50    1.00    --   45.18  38.00 150.00  162
 13  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00-120.00   90
 14  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00 -60.00   90
 15  \w    -30.00  15.00   0.50    1.00    --   45.18 -38.00   0.00   90
 16  \w    -93.00 -23.00   0.50    4.00    --  -97.00  93.00-105.70  140
 17  \w   -167.00 -94.00   0.50    4.00    --  -97.00-125.00-180.00  146
 18  \w   -140.00 -90.00   0.50    4.00    --  -97.00 -15.00 -30.00  100
 19  \w    -97.00 -27.00   0.50    4.00    --  -97.00 114.00   2.75  140
 20  \w    -93.00 -23.00   0.50    4.00    --  -97.00  93.00 154.40  140
 21  \w   -140.00 -90.00   0.50    4.00    --  -97.00 -15.00-120.00  100
 22  \w    -55.00 -23.00   0.50    4.00    --  -97.00  61.00 120.00   64
 23  \w    -55.00 -23.00   0.50    4.00    --  -97.00  61.00 -30.00   64
 24  \w    -92.00 -23.00   0.50    4.00    --  -97.00  94.00  32.40  138
 25  \w    -93.00 -25.00   0.50    4.00    --  -97.00  97.00 -22.41  136
 26  \w    -93.00 -23.00   0.50    4.00    --  -97.00  93.00-154.69  140
 27  \w    -93.00 -25.00   0.50    4.00    --  -97.00  97.00 108.97  136
 28  \w    -93.00 -23.00   0.50    4.00    --  -97.00  93.00-170.26  140
 29  \w    -55.00 -23.00   0.50    4.00    --  -97.00  61.00 -60.00   64
 30  \w    -55.00 -23.00   0.50    4.00    --  -97.00  61.00-120.00   64
 31  \w   -170.00 -90.00   0.50    4.00    --  -97.00 -30.00-120.00  160
 32  \w    -93.00 -25.00   0.50    4.00    --  -97.00  97.00 -37.78  136
 33  \w    -93.00 -23.00   0.50    4.00    --  -97.00  93.00  89.64  140
 34  \w     39.00 100.00   0.50    4.00    --  109.75-125.00 120.00  122
 35  \w     39.00 100.00   0.50    4.00    --  109.75-125.00-150.00  122
 36  \w    102.00 175.00   0.50    4.00    --  109.75  45.00   0.00  146
 37  \w    104.00 162.00   0.50    4.00    --  109.75  30.00 -30.00  116
 38  \w     37.00  93.00   0.50    4.00    --  109.75 -95.00 -60.00  112
 39  \w     37.00  93.00   0.50    4.00    --  109.75 -95.00-180.00  112
 40  \w    104.00 162.00   0.50    4.00    --  109.75  30.00  90.00  116
 41  \w     37.00  93.00   0.50    4.00    --  109.75 -95.00   0.00  112
 42  \w     37.00  71.00   0.50    4.00    --  109.75 -77.00 120.00   68
 43  \w    104.00 132.00   0.50    4.00    --  109.75  15.00 120.00   56
 44  \w     37.00  93.00   0.50    4.00    --  109.75 -95.00-150.00  112
 45  \w    104.00 132.00   0.50    4.00    --  109.75  15.00-150.00   56
 46  \w     37.00  93.00   0.50    4.00    --  109.75 -95.00  30.00  112
 47  \w     45.00  85.00   0.50    4.00    --  109.75 -95.00  90.00   80
 48  \w     43.00  92.00   0.50    4.00    --  109.75 -95.00 -90.00   98
 49  \w     38.00  65.00   0.50    4.00    --  109.75 -77.00  30.00   54
 50  \w     52.00  92.00   0.50    4.00    --  109.75 -95.00-120.00   80
 51  \w    105.00 131.00   0.50    4.00    --  109.75  15.00  90.00   52
 52  \w     37.00  62.00   0.50    4.00    --  109.75 -77.00  60.00   50
;
_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      0.0214660000
_diffrn_orient_matrix_UB_12      0.0939029000
_diffrn_orient_matrix_UB_13      -0.0635039000
_diffrn_orient_matrix_UB_21      -0.0311021000
_diffrn_orient_matrix_UB_22      -0.0403268000
_diffrn_orient_matrix_UB_23      -0.0694566000
_diffrn_orient_matrix_UB_31      -0.1454618000
_diffrn_orient_matrix_UB_32      0.0371454000
_diffrn_orient_matrix_UB_33      0.0170700000
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47699
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.010
_diffrn_reflns_theta_min         2.743
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.533
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0763P)^2^+0.3374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8356
_reflns_number_total             9932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02846a2.cif
_cod_data_source_block           pMeL3H
_cod_database_code               7720466
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C63O3N4H64
_chemical_oxdiff_usercomment     'Me o-tBuV'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.897
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14), C19(H19),
 C22(H22), C23(H23), C24(H24), C25(H25), C33(H33), C35(H35), C38(H38), C41(H41),
  C42(H42), C43(H43), C44(H44), C49(H49), C52(H52), C53(H53), C54(H54), C55(H55)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,
 H37B,H37C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              82270
_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 3.286
_oxdiff_exptl_absorpt_empirical_full_min 0.542