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_7716925
_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         'C34 H38 N2 O6 Ti'
_chemical_formula_sum            'C34 H38 N2 O6 Ti'
_chemical_formula_weight         618.56
_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             2023-05-23
_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                 104.270(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8926(2)
_cell_length_b                   14.8890(3)
_cell_length_c                   18.5751(3)
_cell_measurement_reflns_used    39736
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9680
_cell_measurement_theta_min      1.7800
_cell_volume                     3187.59(10)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -26.00 100.00   0.50   25.14    --   10.60  40.00 -97.00  252
  2  \w    -79.00  47.00   0.50   25.14    --   10.60 -40.00 108.00  252
  3  \w   -100.00  25.00   0.50   25.14    --  -10.90 -40.00 108.00  250
  4  \w    -47.00  78.00   0.50   25.14    --  -10.90  40.00 -97.00  250
  5  \w    -20.00 100.00   0.50   25.14    --   10.60  57.00  30.00  240
  6  \w    -79.00  41.00   0.50   25.14    --   10.60 -57.00   0.00  240
  7  \w    -79.00  48.00   0.50   25.14    --   10.60 -38.00 -90.00  254
  8  \w    -17.00 100.00   0.50   25.14    --   10.60  82.00   0.00  234
  9  \w    -79.00  48.00   0.50   25.14    --   10.60 -38.00   0.00  254
 10  \w    -20.00 100.00   0.50   25.14    --   10.60  57.00 -90.00  240
 11  \w    -79.00 -31.00   0.50   25.14    --   10.60 -82.00 -30.00   96
 12  \w    -79.00  38.00   0.50   25.14    --   10.60 -82.00 -90.00  234
 13  \w    -38.00  79.00   0.50   25.14    --  -10.90  82.00 120.00  234
 14  \w   -100.00  17.00   0.50   25.14    --  -10.90 -82.00  60.00  234
;
_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  0.1077
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            79538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.235
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52760
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     1488
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0618P)^2^+1.4263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4692
_reflns_number_total             5595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02282c2.cif
_cod_data_source_block           k11007-hyc-l
_cod_depositor_comments
'Adding full bibliography for 7716924--7716925.cif.'
_cod_database_code               7716925
_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
 O5-C29 \\sim O5-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C29-C31 \\sim C29A-C31A
 with sigma of 0.02
 O5-C30 \\sim O5-C30A
 with sigma of 0.04
 O5-C31 \\sim O5-C31A
 with sigma of 0.04
 C30-C31 \\sim C30A-C31A
 with sigma of 0.04
 O6-C32 \\sim O6-C32A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.02
 C32-C34 \\sim C32A-C34A
 with sigma of 0.02
 O6-C33 \\sim O6-C33A
 with sigma of 0.04
 O6-C34 \\sim O6-C34A
 with sigma of 0.04
 C33-C34 \\sim C33A-C34A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C29A \\sim C30 \\sim C30A \\sim
C31 \\sim C31A \\sim C32 \\sim C32A \\sim C33 \\sim C33A \\sim C34 \\sim C34A
\\sim N1 \\sim N2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim
Ti1: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
4. Others
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(2)
 Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C29(H29), C29A(H29A), C32(H32), C32A(H32A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C23(H23), C24(H24), C26(H26),
  C27(H27)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C30A(H30D,H30E,
 H30F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F), C33(H33A,H33B,H33C),
 C33A(H33D,H33E,H33F), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              7261
_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
;