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_1576096
_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         'C44 H49 Cl2 N O P V'
_chemical_formula_sum            'C44 H49 Cl2 N O P V'
_chemical_formula_weight         760.65
_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.cc2nxt7n
_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                84.0364(14)
_cell_angle_beta                 89.5297(12)
_cell_angle_gamma                65.930(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1205(2)
_cell_length_b                   13.2561(3)
_cell_length_c                   15.58115(20)
_cell_measurement_reflns_used    24938
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.5170
_cell_measurement_theta_min      2.8670
_cell_volume                     2459.21(8)
_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      100.01(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     33.00  90.00   0.50    0.05    --   47.65-125.00  60.00  114
  2  \w     47.00 110.00   0.50    0.05    --  106.54-125.00 -30.00  126
  3  \w     48.00  74.00   0.50    0.05    --  106.54-125.00 -60.00   52
  4  \w     65.00 109.00   0.50    0.05    --  106.54-125.00-120.00   88
  5  \w     83.00 108.00   0.50    0.05    --  106.54-125.00-150.00   50
  6  \w     51.00 102.00   0.50    0.05    --  106.54 -95.00-120.00  102
  7  \w     35.00  85.00   0.50    0.05    --  106.54 -95.00 -30.00  100
  8  \w     69.00 105.00   0.50    0.05    --  106.54 -95.00   0.00   72
  9  \w     38.00 111.00   0.50    0.05    --  106.54-125.00  90.00  146
 10  \w     34.00 106.00   0.50    0.05    --  106.54 -77.00  90.00  144
 11  \w     34.00  75.00   0.50    0.05    --  106.54 -61.00 150.00   82
 12  \w     -3.00  27.00   0.50    0.05    --   47.65 -10.00 157.00   60
 13  \w     34.00  63.00   0.50    0.05    --  106.54 -61.00   0.00   58
 14  \w     34.00  74.00   0.50    0.05    --  106.54 -61.00-180.00   80
 15  \w    -19.00  44.00   0.50    0.05    --   47.65 -57.00-180.00  126
 16  \w     36.00 119.00   0.50    0.05    --   47.65  57.00 -30.00  166
 17  \w     92.00 176.00   0.50    0.05    --  106.54  10.00 -29.00  168
 18  \w     31.00 122.00   0.50    0.05    --   47.65  10.00 -29.00  182
 19  \w    -69.00 -26.00   0.50    0.05    --  -47.65  77.00 -90.00   86
 20  \w    -18.00  14.00   0.50    0.05    --  -47.65  77.00 -90.00   64
 21  \w    -21.00   4.00   0.50    0.05    --  -47.65  10.00 -29.00   50
 22  \w    -20.00  22.00   0.50    0.05    --  -47.65  19.00 150.00   84
 23  \w   -108.00 -50.00   0.50    0.05    -- -104.50 110.00 117.97  116
 24  \w   -124.00 -91.00   0.50    0.05    -- -104.50 143.00 122.81   66
 25  \w   -102.00 -61.00   0.50    0.05    -- -104.50 125.00  60.00   82
 26  \w   -125.00 -93.00   0.50    0.05    -- -104.50 143.00 -48.15   64
 27  \w    -82.00 -39.00   0.50    0.05    -- -104.50 143.00 -48.15   86
 28  \w    -66.00 -41.00   0.50    0.05    -- -104.50  77.00   0.00   50
 29  \w    -67.00 -41.00   0.50    0.05    -- -104.50  61.00  60.00   52
 30  \w    -67.00 -42.00   0.50    0.05    -- -104.50  61.00 120.00   50
 31  \w    -67.00 -38.00   0.50    0.05    -- -104.50  61.00 150.00   58
 32  \w    -98.00 -72.00   0.50    0.05    -- -104.50  77.00   0.00   52
 33  \w    -60.00 -34.00   0.50    0.05    -- -104.50  61.00   0.00   52
 34  \w    -67.00 -32.00   0.50    0.05    -- -104.50  61.00-180.00   70
 35  \w   -167.00-132.00   0.50    0.05    -- -104.50 -77.00 -60.00   70
 36  \w   -128.00 -82.00   0.50    0.05    -- -104.50 -77.00 -60.00   92
 37  \w   -172.00 -96.00   0.50    0.05    -- -104.50 -15.00-120.00  152
 38  \w   -169.00-107.00   0.50    0.05    -- -104.50 -15.00-150.00  124
 39  \w   -153.00 -92.00   0.50    0.05    -- -104.50 -15.00  90.00  122
 40  \w   -163.00 -95.00   0.50    0.05    -- -104.50 -10.00 157.00  136
 41  \w   -107.00 -54.00   0.50    0.05    --  -47.65 -10.00 157.00  106
;
_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      0.0382857000
_diffrn_orient_matrix_UB_12      0.0959175000
_diffrn_orient_matrix_UB_13      -0.0059664000
_diffrn_orient_matrix_UB_21      0.1209097000
_diffrn_orient_matrix_UB_22      -0.0828235000
_diffrn_orient_matrix_UB_23      -0.0119179000
_diffrn_orient_matrix_UB_31      -0.0218196000
_diffrn_orient_matrix_UB_32      0.0184391000
_diffrn_orient_matrix_UB_33      -0.0985850000
_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  0.0286
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31869
_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         76.848
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63835
_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    1.027
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9995
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0517P)^2^+1.1833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9592
_reflns_number_total             9995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5py00730e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1576095--1576097.cif.'
_cod_original_cell_volume        2459.20(9)
_cod_database_code               1576096
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         VPClCHON
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.831
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
3.a Ternary CH refined with riding coordinates:
 C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C20(H20A,H20B), C17(H17A,H17B), C19(H19A,H19B), C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C10(H10), C4(H4), C3(H3), C38(H38), C5(H5), C42(H42),
 C14(H14), C11(H11), C12(H12), C39(H39), C41(H41), C13(H13), C29(H29), C33(H33),
  C40(H40), C31(H31), C32(H32), C30(H30)
3.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C),
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              68319
_shelx_hkl_checksum              64739
_shelx_fab_checksum              58347
_platon_squeeze_void_probe_radius 1.20
_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 1.903
_oxdiff_exptl_absorpt_empirical_full_min 0.569