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_7720471
_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         'C52 H42 F12 N4 O3 V, C7 H8'
_chemical_formula_sum            'C59 H50 F12 N4 O3 V'
_chemical_formula_weight         1141.97
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-22
_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                 109.452(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.8959(7)
_cell_length_b                   10.6717(3)
_cell_length_c                   30.5882(7)
_cell_measurement_reflns_used    5745
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5220
_cell_measurement_theta_min      2.6720
_cell_volume                     10740.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.961
_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    -66.00 -33.00   0.50    0.05    -- -103.00  61.00 -90.00   66
  2  \w   -103.00 -57.00   0.50    0.05    -- -103.00  77.00  30.00   92
  3  \w    -58.00 -32.00   0.50    0.05    -- -103.00  61.00  60.00   52
  4  \w    -21.00  29.00   0.50    0.05    --  -46.61  19.00  90.00  100
  5  \w    -22.00  28.00   0.50    0.05    --  -46.61  19.00-180.00  100
  6  \w   -118.00 -64.00   0.50    0.05    --  -46.61-143.00  21.00  108
  7  \w   -162.00 -85.00   0.50    0.05    -- -103.00-143.00  21.00  154
  8  \w   -125.00 -79.00   0.50    0.05    -- -103.00-127.00-168.00   92
  9  \w   -106.00 -81.00   0.50    0.05    -- -103.00 -74.00 -75.57   50
 10  \w   -174.00 -86.00   0.50    0.05    -- -103.00 -61.00-157.37  176
 11  \w   -155.00-128.00   0.50    0.05    -- -103.00 -74.00 -75.57   54
 12  \w   -125.00 -63.00   0.50    0.05    -- -103.00 143.00  77.00  124
 13  \w     32.00 105.00   0.50    0.05    --   46.61-143.00  21.00  146
 14  \w     32.00 125.00   0.50    0.05    --  101.75-143.00  21.00  186
 15  \w     39.00  78.00   0.50    0.05    --  101.75-125.00-120.00   78
 16  \w     31.00 113.00   0.50    0.05    --  101.75-127.00-168.00  164
 17  \w     84.00 112.00   0.50    0.05    --  101.75-125.00-120.00   56
 18  \w     25.00  94.00   0.50    0.05    --   46.61-127.00-168.00  138
 19  \w     29.00 106.00   0.50    0.05    --  101.75 -94.00-180.00  154
 20  \w    -24.00  28.00   0.50    0.05    --   46.61 -19.00-120.00  104
 21  \w     53.00 105.00   0.50    0.05    --  101.75-101.00  36.70  104
 22  \w     95.00 170.00   0.50    0.05    --  101.75  61.00   0.00  150
 23  \w     70.00 118.00   0.50    0.05    --   46.61 143.00  77.00   96
 24  \w     70.00 171.00   0.50    0.05    --  101.75 143.00  77.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0010398000
_diffrn_orient_matrix_UB_12      -0.0937661000
_diffrn_orient_matrix_UB_13      -0.0387005000
_diffrn_orient_matrix_UB_21      0.0045881000
_diffrn_orient_matrix_UB_22      -0.1093857000
_diffrn_orient_matrix_UB_23      0.0342030000
_diffrn_orient_matrix_UB_31      -0.0465855000
_diffrn_orient_matrix_UB_32      -0.0086170000
_diffrn_orient_matrix_UB_33      -0.0136500000
_diffrn_radiation_collimation    'Arc)Sec VHF Varimax focusing mirrors'
_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  0.0669
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            50560
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.326
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       prism
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0880P)^2^+7.8994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9036
_reflns_number_total             10685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02846a2.cif
_cod_data_source_block           12
_cod_database_code               7720471
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C59 H50 F12 N4 O3 V'
_chemical_oxdiff_usercomment     VCF3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.503
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18),
 C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C31(H31), C33(H33), C40(H40),
  C41(H41), C42(H42), C43(H43), C45(H45), C48(H48), C49(H49), C50(H50),
 C51(H51), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              30720
_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 2.420
_oxdiff_exptl_absorpt_empirical_full_min 0.392