A comparative study of titanium complexes bearing 2-(arylideneamino)phenolates and 2-((arylimino)methyl)phenolates as catalysts for ring-opening polymerization of ε-caprolactone and L-lactide.
Wu, Ling-Jo; Kottalanka, Ravi Kumar; Chu, Yu-Ting; Lin, Zheng-Ian; Chang, Chun-Juei; Ding, Shangwu; Chen, Hsuan-Ying; Wu, Kuo-Hui; Chen, Chih-Kuang; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15660–15673; doi:10.1039/d4dt02282c

data_7716924
_publ_section_title
;
 A comparative study of titanium complexes bearing
 2-(arylideneamino)phenolates and 2-((arylimino)methyl)phenolates as
 catalysts for ring-opening polymerization of &#x3b5;-caprolactone and
 L-lactide.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15660
_journal_page_last               15673
_journal_paper_doi               10.1039/d4dt02282c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C32 H34 N2 O4 Ti)'
_chemical_formula_sum            'C64 H68 N4 O8 Ti2'
_chemical_formula_weight         1117.02
_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
_audit_creation_date             2023-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2024-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.516(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1742(3)
_cell_length_b                   16.9814(4)
_cell_length_c                   27.9303(5)
_cell_measurement_reflns_used    23155
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9310
_cell_measurement_theta_min      1.7400
_cell_volume                     5657.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -15.00 100.00   0.50   62.29    --   10.60  77.00 -90.00  230
  2  \w    -15.00 100.00   0.50   62.29    --   10.60  77.00 150.00  230
  3  \w    -79.00  38.00   0.50   62.29    --   10.60 -82.00-120.00  234
  4  \w     -6.00  91.00   0.50   62.29    --   10.60  77.00  60.00  194
  5  \w    -46.00  36.00   0.50   62.29    --   10.60 -77.00 150.00  164
  6  \w    -36.00  79.00   0.50   62.29    --  -10.90  77.00  90.00  230
  7  \w    -19.00  20.00   0.50   62.29    --  -10.90  77.00  30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60053
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.911
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.068
_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     741
_refine_ls_number_reflns         9916
_refine_ls_number_restraints     2364
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0561P)^2^+8.3723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7877
_reflns_number_total             9916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02282c2.cif
_cod_data_source_block           k11004-hyc-d
_cod_depositor_comments
'Adding full bibliography for 7716924--7716925.cif.'
_cod_database_code               7716924
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 O7-C59 \\sim O7-C62
 with sigma of 0.02
 C61-C59 \\sim C63-C62
 with sigma of 0.02
 C59-C60 \\sim C62-C64
 with sigma of 0.02
 O7-C61 \\sim O7-C63
 with sigma of 0.04
 O7-C60 \\sim O7-C64
 with sigma of 0.04
 C61-C60 \\sim C63-C64
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C40 \\sim C36 \\sim C41 \\sim C37 \\sim C38 \\sim C39 \\sim C45 \\sim C46 \\sim
C47 \\sim C42 \\sim C49 \\sim C43 \\sim C44 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58 \\sim C65 \\sim C66 \\sim C67 \\sim C50 \\sim C51 \\sim C33 \\sim
C34 \\sim C52 \\sim C35 \\sim C53 \\sim C48 \\sim C59 \\sim C61 \\sim C60 \\sim
C64 \\sim C62 \\sim C63 \\sim C1 \\sim C25 \\sim C17 \\sim C13 \\sim C21 \\sim
C3 \\sim C5 \\sim C9 \\sim C7 \\sim C11 \\sim C15 \\sim C19 \\sim C27 \\sim C23
\\sim C29 \\sim C2 \\sim C31 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C12
\\sim C14 \\sim C16 \\sim C18 \\sim C20 \\sim C22 \\sim C32 \\sim C24 \\sim C26
\\sim C28 \\sim C30 \\sim N4 \\sim N3 \\sim N1 \\sim N2 \\sim O5 \\sim O6 \\sim
O7 \\sim O8 \\sim O2 \\sim O4 \\sim O3 \\sim O1 \\sim Ti2 \\sim Ti1: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
4. Others
 Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63A)=
 Sof(H63B)=Sof(H63C)=1-FVAR(1)
 Sof(C59)=Sof(H59)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=Sof(H60C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C65(H65), C59(H59), C62(H62), C27(H27), C30(H30)
5.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C41(H41), C37(H37), C38(H38), C39(H39), C45(H45), C47(H47),
 C42(H42), C49(H49), C43(H43), C44(H44), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C50(H50), C52(H52), C35(H35), C48(H48), C25(H25), C17(H17),
 C13(H13), C3(H3), C5(H5), C9(H9), C7(H7), C11(H11), C15(H15), C23(H23), C4(H4),
  C6(H6), C10(H10), C12(H12), C16(H16), C18(H18), C20(H20), C22(H22), C24(H24),
 C26(H26)
5.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C61(H61A,H61B,H61C), C60(H60A,H60B,
 H60C), C64(H64A,H64B,H64C), C63(H63A,H63B,H63C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              31328
_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
;