Titanium complexes of pyrrolylaldiminate ligands and their exploitation for the ring-opening polymerization of cyclic esters.
Upitak, Kanokon; Wattanathana, Worawat; Nanok, Tanin; Chuawong, Pitak; Hormnirun, Pimpa; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10964–10981; doi:10.1039/d1dt01470f

data_7707814
_publ_section_title
;
 Titanium complexes of pyrrolylaldiminate ligands and their exploitation
 for the ring-opening polymerization of cyclic esters.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10964
_journal_page_last               10981
_journal_paper_doi               10.1039/d1dt01470f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C26 H40 N4 O2 Ti'
_chemical_formula_sum            'C26 H40 N4 O2 Ti'
_chemical_formula_weight         488.52
_chemical_properties_physical    Air-sensitive
_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             2021-06-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-02 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 75.196(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9560(9)
_cell_length_b                   16.7630(17)
_cell_length_c                   18.1781(19)
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.678
_cell_measurement_theta_min      3.644
_cell_volume                     2638.5(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42047
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.645
_diffrn_reflns_theta_min         3.644
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_T_max  0.7106
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1610 before and 0.1020 after correction.
The Ratio of minimum to maximum transmission is 0.8995.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4688
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.1454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+31.7454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3409
_refine_ls_wR_factor_ref         0.3410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4639
_reflns_number_total             4688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01470f2.cif
_cod_data_source_block           kuc4_lt_0m
_cod_depositor_comments          'Adding full bibliography for 7707814.cif.'
_cod_database_code               7707814
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.891
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 C25, C26A, C22, C23, C24, C26, C23A, C24A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5, C5A, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C24 \\sim C26A \\sim C23 \\sim C22 \\sim C25 \\sim C26 \\sim C24A \\sim C23A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C6 \\sim C5 \\sim C5A \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4. Others
 Fixed Sof: H22(0.7) H22A(0.3) H6BD(0.75) H6BE(0.75) H6BF(0.75) H6AA(0.25)
 H6AB(0.25) H6AC(0.25) C5(0.75) H5(0.75) H4BD(0.75) H4BE(0.75) H4BF(0.75)
 H4AA(0.25) H4AB(0.25) H4AC(0.25) C24(0.7) H24A(0.7) H24B(0.7) H25A(0.7)
 H25B(0.7) H25C(0.3) H25D(0.3) C26(0.7) H26A(0.7) H26B(0.7) C23(0.7) H23A(0.7)
 H23B(0.7) H1AA(0.6) H1AB(0.6) H1AC(0.6) H1BD(0.4) H1BE(0.4) H1BF(0.4) C2(0.6)
 H2(0.6) C3(0.6) H3A(0.6) H3B(0.6) H3C(0.6) C2A(0.4) H2A(0.4) C3A(0.4)
 H3AA(0.4) H3AB(0.4) H3AC(0.4) C26A(0.3) H26C(0.3) H26D(0.3) C23A(0.3)
 H23C(0.3) H23D(0.3) C24A(0.3) H24C(0.3) H24D(0.3) C5A(0.25) H5A(0.25)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C22(H22), C22(H22A), C5(H5), C2(H2), C2A(H2A), C5A(H5A)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C24(H24A,
 H24B), C25(H25A,H25B), C25(H25C,H25D), C26(H26A,H26B), C23(H23A,H23B),
 C26A(H26C,H26D), C23A(H23C,H23D), C24A(H24C,H24D)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21), C17(H17), C7(H7), C19(H19), C18(H18), C9(H9), C8(H8)
5.d Idealised Me refined as rotating group:
 C6(H6BD,H6BE,H6BF), C6(H6AA,H6AB,H6AC), C4(H4BD,H4BE,H4BF), C4(H4AA,H4AB,
 H4AC), C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,
 H3AC)
;
_shelx_res_checksum              74217
_shelx_hkl_checksum              87557
_olex2_submission_special_instructions 'No special instructions were received'