Thermally stable vanadium(v) complexes bearing bidentate phenoxy-phosphine ligands: synthesis, characterization, and catalytic properties for alkene polymerization
Li, Biao; Ding, Yingli; Gao, Huan; Pan, Li; Li, Yuesheng; Polymer Chemistry 16 (2025) 4889–4898; doi:10.1039/D5PY00730E

data_1576097
_publ_section_title
;
 Thermally stable vanadium(v) complexes bearing bidentate
 phenoxy-phosphine ligands: synthesis, characterization, and catalytic
 properties for alkene polymerization
;
_journal_issue                   45
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4889
_journal_page_last               4898
_journal_paper_doi               10.1039/D5PY00730E
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C39 H41 Cl2 N O P V, C6 H6'
_chemical_formula_sum            'C45 H47 Cl2 N O P V'
_chemical_formula_weight         770.64
_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_block_doi                 10.5517/ccdc.csd.cc2nxt8p
_audit_creation_date             2024-10-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.7275(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.5327(4)
_cell_length_b                   12.96804(16)
_cell_length_c                   26.1924(4)
_cell_measurement_reflns_used    13524
_cell_measurement_temperature    100.3(7)
_cell_measurement_theta_max      75.5860
_cell_measurement_theta_min      3.6120
_cell_volume                     8056.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.3(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.960
_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    -22.00  58.00   0.50    0.10    --   47.66 -72.00 161.00  160
  2  \w     33.00  92.00   0.50    0.40    --  105.91 -72.00 161.00  118
  3  \w     38.00  86.00   0.50    0.40    --  105.91-125.00 120.00   96
  4  \w     40.00  73.00   0.50    0.40    --  105.91 -61.00 -30.00   66
  5  \w     42.00  68.00   0.50    0.40    --  105.91 -61.00-150.00   52
  6  \w    102.00 171.00   0.50    0.40    --  105.91  15.00-120.00  138
  7  \w     95.00 154.00   0.50    0.40    --  105.91  15.00 -90.00  118
  8  \w    105.00 131.00   0.50    0.40    --  105.91  72.00 -68.00   52
  9  \w     94.00 176.00   0.50    0.40    --  105.91  30.00   0.00  164
 10  \w     28.00 109.00   0.50    0.10    --   47.66  72.00 -68.00  162
 11  \w    -35.00  21.00   0.50    0.10    --  -47.66  72.00 -68.00  112
 12  \w    -22.00  16.00   0.50    0.10    --  -47.66  19.00 -60.00   76
 13  \w    -68.00 -36.00   0.50    0.40    -- -104.50  61.00 -90.00   64
 14  \w    -76.00 -32.00   0.50    0.40    -- -104.50  72.00 -68.00   88
 15  \w    -66.00 -40.00   0.50    0.40    -- -104.50  61.00 -30.00   52
 16  \w    -66.00 -32.00   0.50    0.40    -- -104.50  61.00  60.00   68
 17  \w    -20.00  28.00   0.50    0.10    --  -47.66  19.00  90.00   96
 18  \w    -97.00 -72.00   0.50    0.10    --  -47.66 -72.00 161.00   50
 19  \w   -149.00-119.00   0.50    0.40    -- -104.50 -72.00 161.00   60
 20  \w   -173.00 -91.00   0.50    0.40    -- -104.50 -15.00 150.00  164
 21  \w   -173.00-119.00   0.50    0.40    -- -104.50 -45.00  60.00  108
 22  \w   -121.00 -93.00   0.50    0.40    -- -104.50 -30.00 -60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0507698000
_diffrn_orient_matrix_UB_12      0.0655870000
_diffrn_orient_matrix_UB_13      0.0353902000
_diffrn_orient_matrix_UB_21      -0.0073846000
_diffrn_orient_matrix_UB_22      0.0693051000
_diffrn_orient_matrix_UB_23      -0.0499608000
_diffrn_orient_matrix_UB_31      -0.0397832000
_diffrn_orient_matrix_UB_32      0.0708472000
_diffrn_orient_matrix_UB_33      0.0161632000
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28044
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.513
_diffrn_reflns_theta_min         3.633
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67063
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0623P)^2^+10.4834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7020
_reflns_number_total             8112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py00730e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1576095--1576097.cif.'
_cod_database_code               1576097
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         VPClCHON
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.799
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              25453
_shelx_hkl_checksum              34285
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.731