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_1576095
_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         'C42 H47 Cl2 N O P V'
_chemical_formula_sum            'C42 H47 Cl2 N O P V'
_chemical_formula_weight         734.61
_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_block_doi                 10.5517/ccdc.csd.cc2nxt6m
_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                88.807(2)
_cell_angle_beta                 69.449(2)
_cell_angle_gamma                76.892(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5612(3)
_cell_length_b                   12.6489(3)
_cell_length_c                   14.3413(4)
_cell_measurement_reflns_used    19806
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4180
_cell_measurement_theta_min      3.3180
_cell_volume                     1908.61(9)
_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 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 0.999
_diffrn_measured_fraction_theta_max 0.962
_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     56.00  94.00   0.50    0.05    --   47.90-125.00  30.00   76
  2  \w     42.00 111.00   0.50    0.05    --  106.54-125.00 -30.00  138
  3  \w     38.00  82.00   0.50    0.05    --  106.54-125.00   0.00   88
  4  \w     53.00 111.00   0.50    0.05    --  106.54-125.00 120.00  116
  5  \w     37.00 110.00   0.50    0.05    --  106.54-125.00  90.00  146
  6  \w     43.00 108.00   0.50    0.05    --  106.54-107.00  28.46  130
  7  \w     69.00  99.00   0.50    0.05    --  106.54 -95.00 -30.00   60
  8  \w     74.00 111.00   0.50    0.05    --  106.54-125.00-120.00   74
  9  \w     80.00 105.00   0.50    0.05    --  106.54 -95.00-120.00   50
 10  \w     -8.00  79.00   0.50    0.05    --   47.90 -99.00-150.00  174
 11  \w    -26.00  25.00   0.50    0.05    --   47.90 -19.00  60.00  102
 12  \w     48.00  73.00   0.50    0.05    --  106.54 -61.00 150.00   50
 13  \w     43.00  72.00   0.50    0.05    --  106.54 -61.00  90.00   58
 14  \w     39.00  65.00   0.50    0.05    --  106.54 -61.00   0.00   52
 15  \w     14.00  48.00   0.50    0.05    --   47.90 -41.00-154.00   68
 16  \w     74.00 119.00   0.50    0.05    --   47.90  41.00  -1.00   90
 17  \w    103.00 175.00   0.50    0.05    --  106.54  30.00 120.00  144
 18  \w     99.00 176.00   0.50    0.05    --  106.54  30.00  90.00  154
 19  \w     95.00 177.00   0.50    0.05    --  106.54  41.00  -1.00  164
 20  \w     36.00  70.00   0.50    0.05    --   47.90  41.00  -1.00   68
 21  \w    -22.00  21.00   0.50    0.05    --  -47.90  41.00  -1.00   86
 22  \w    -37.00  -1.00   0.50    0.05    --  -47.90  38.00  60.00   72
 23  \w    -23.00  16.00   0.50    0.05    --  -47.90  19.00 -30.00   78
 24  \w   -101.00 -33.00   0.50    0.05    -- -104.50  77.00 -90.00  136
 25  \w   -100.00 -75.00   0.50    0.05    -- -104.50  77.00-180.00   50
 26  \w    -57.00 -32.00   0.50    0.05    -- -104.50  77.00-180.00   50
 27  \w    -66.00 -40.00   0.50    0.05    -- -104.50  61.00-180.00   52
 28  \w   -174.00 -91.00   0.50    0.05    -- -104.50 -15.00-120.00  166
 29  \w   -106.00 -39.00   0.50    0.05    --  -47.90 -41.00-154.00  134
 30  \w   -122.00 -96.00   0.50    0.05    -- -104.50 -61.00   0.00   52
 31  \w   -166.00-125.00   0.50    0.05    -- -104.50 -61.00   0.00   82
 32  \w   -171.00-126.00   0.50    0.05    -- -104.50 -45.00  90.00   90
 33  \w   -117.00 -92.00   0.50    0.05    -- -104.50 -45.00  90.00   50
 34  \w   -174.00 -92.00   0.50    0.05    -- -104.50 -41.00-154.00  164
 35  \w   -108.00 -54.00   0.50    0.05    -- -104.50 110.00-101.41  108
 36  \w    -75.00 -35.00   0.50    0.05    -- -104.50 125.00 120.00   80
 37  \w   -102.00 -76.00   0.50    0.05    -- -104.50 125.00 120.00   52
 38  \w   -102.00 -45.00   0.50    0.05    -- -104.50 125.00 150.00  114
;
_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      0.0807372000
_diffrn_orient_matrix_UB_12      -0.1173955000
_diffrn_orient_matrix_UB_13      -0.0125025000
_diffrn_orient_matrix_UB_21      0.0757729000
_diffrn_orient_matrix_UB_22      0.0350409000
_diffrn_orient_matrix_UB_23      0.0584397000
_diffrn_orient_matrix_UB_31      -0.0957579000
_diffrn_orient_matrix_UB_32      -0.0263411000
_diffrn_orient_matrix_UB_33      0.0982069000
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23604
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.946
_diffrn_reflns_theta_min         3.298
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47144
_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            'dark orange'
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0536P)^2^+0.5731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7556
_reflns_number_total             7745
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py00730e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1576095--1576097.cif.'
_cod_database_code               1576095
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         VPClCHON
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.791
_reflns_odcompleteness_completeness 99.97
_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)
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), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              99404
_shelx_hkl_checksum              10190
_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 1.802
_oxdiff_exptl_absorpt_empirical_full_min 0.622