Synthesis and structure of titanium complexes with phosphonium-bisphenolate ligands "{P<sup>+</sup>[O<sub>2</sub>]}H<sub>2</sub>" and their catalytic trimerization of 1-octene.
Toda, Tomoyuki; Cheng, Yu; Takenaka, Katsuhiko; Chemical communications (Cambridge, England) 61 (2025) 15594–15597; doi:10.1039/d5cc04541j

data_7134933
_publ_section_title
;
 Synthesis and structure of titanium complexes with
 phosphonium-bisphenolate ligands
 "{P<sup>+</sup>[O<sub>2</sub>]}H<sub>2</sub>" and their catalytic
 trimerization of 1-octene.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15594
_journal_page_last               15597
_journal_paper_doi               10.1039/d5cc04541j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C42 H52 Cl3 O2 P Ti, 1(C7 H8)'
_chemical_formula_sum            'C49 H60 Cl3 O2 P Ti'
_chemical_formula_weight         866.19
_chemical_name_systematic        'Titanium complex'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-22
_audit_creation_method
;
Olex2 1.5-ac7-016
(compiled 2025.05.29 svn.r8cd99b3d for Rigaku Oxford Diffraction, GUI svn.r7254)
;
_audit_update_record
;
2025-08-22 deposited with the CCDC.	2025-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.631(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7820(3)
_cell_length_b                   24.6362(5)
_cell_length_c                   12.3944(3)
_cell_measurement_reflns_used    21436
_cell_measurement_temperature    103
_cell_measurement_theta_max      28.1470
_cell_measurement_theta_min      2.0440
_cell_volume                     4617.46(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac7-016 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-016 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      103
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.941
_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    -36.00   3.00   0.50  200.00    --   12.07 -75.00-173.00   78
  2  \w     10.00  80.00   0.50  200.00    --   12.07  75.00 -45.00  140
  3  \w    -79.00 -18.00   0.50  200.00    --  -12.15 -75.00-173.00  122
  4  \w      9.00  48.00   0.50  200.00    --  -12.15  75.00 -45.00   78
  5  \w    -54.00  23.00   0.50  200.00    --   12.07 -37.00   0.00  154
  6  \w    -57.00  13.00   0.50  200.00    --   12.07 -19.00 -90.00  140
  7  \w     31.00  59.00   0.50  200.00    --   12.07-125.00-180.00   56
  8  \w      2.00  27.00   0.50  200.00    --   12.07  37.00 -30.00   50
  9  \w     -2.00  50.00   0.50  200.00    --   12.07  19.00 -30.00  104
 10  \w    -56.00 -21.00   0.50  200.00    --  -12.15 125.00-180.00   70
 11  \w    -57.00 -13.00   0.50  200.00    --  -12.15 125.00  60.00   88
 12  \w    -51.00 -18.00   0.50  200.00    --  -12.15 125.00 -90.00   66
 13  \w    -50.00 -13.00   0.50  200.00    --  -12.15 125.00   0.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449004000
_diffrn_orient_matrix_UB_12      0.0081253000
_diffrn_orient_matrix_UB_13      0.0122153000
_diffrn_orient_matrix_UB_21      -0.0128064000
_diffrn_orient_matrix_UB_22      0.0223545000
_diffrn_orient_matrix_UB_23      -0.0371661000
_diffrn_orient_matrix_UB_31      -0.0048657000
_diffrn_orient_matrix_UB_32      0.0162032000
_diffrn_orient_matrix_UB_33      0.0451190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51657
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.285
_diffrn_reflns_theta_min         1.653
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         10786
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+2.6161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8107
_reflns_number_total             10786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04541j2.cif
_cod_data_source_block           sei005_auto
_cod_depositor_comments          'Adding full bibliography for 7134933.cif.'
_cod_database_code               7134933
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C42H52P1O2Ti1Cl3
_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
C49A \\sim C46 \\sim C45 \\sim C47 \\sim C44 \\sim C48 \\sim C47A \\sim C46A
\\sim C43 \\sim C44A \\sim C45A \\sim C48A \\sim C49 \\sim C43A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C43A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49D)=Sof(H49E)=Sof(H49F)=
 Sof(C44A)=Sof(H44A)=Sof(C47A)=Sof(H47A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46A)=1-FVAR(1)
 Sof(C46)=Sof(H46)=Sof(C45)=Sof(H45)=Sof(C44)=Sof(H44)=Sof(C43)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(H47)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C28(H28A,H28B)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C9(H9), C34(H34), C6(H6), C17(H17), C32(H32), C12(H12), C10(H10),
 C11(H11), C5(H5), C3(H3), C4(H4), C46(H46), C48A(H48A), C45(H45), C44(H44),
 C48(H48), C44A(H44A), C47A(H47A), C45A(H45A), C46A(H46A), C47(H47)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C38(H38A,H38B,
 H38C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C27(H27A,H27B,H27C), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C49A(H49D,H49E,H49F)
;
_shelx_res_checksum              13260
_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 1.947
_oxdiff_exptl_absorpt_empirical_full_min 0.525