Efficient synthesis of polylactide and copolymers under industrial conditions by multinuclear β-ketoimide zinc complexes
Cheng, Yu; Zhao, Zihe; Xu, Xiaowei; Ren, Chunxiao; Wei, Xiaohui; Yang, Yanxiang; Li, Jin; Jiang, Daqiang; Zhang, Kunyu; Wang, Bin; Luo, Yi; Polymer Chemistry 16 (2025) 3030–3040; doi:10.1039/D4PY01486C

data_1574693
_publ_section_title
;
 Efficient synthesis of polylactide and copolymers under industrial
 conditions by multinuclear \b-ketoimide zinc complexes
;
_journal_issue                   26
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3030
_journal_page_last               3040
_journal_paper_doi               10.1039/D4PY01486C
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(C41 H41 N3 O5 Zn2), C1 H2 Cl2'
_chemical_formula_sum            'C83 H84 Cl2 N6 O10 Zn4'
_chemical_formula_weight         1657.94
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-31 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                76.404(2)
_cell_angle_beta                 85.521(2)
_cell_angle_gamma                84.815(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3644(6)
_cell_length_b                   16.4964(7)
_cell_length_c                   17.4218(7)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      79.51
_cell_measurement_theta_min      2.61
_cell_volume                     3711.6(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 V2023.9-2 (Bruker, 2023)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            170060
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.665
_diffrn_reflns_theta_min         2.614
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.653
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8056.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         15857
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+2.3320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14054
_reflns_number_total             15857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py01486c2.cif
_cod_data_source_block           cu_240824lulgpz192038_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1574691--1574693.cif.
;
_cod_database_code               1574693
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.741
_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. Restrained distances
 Cl1A-C80A \\sim Cl2A-C80A \\sim Cl2-C80 \\sim Cl1-C80
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C80 \\sim Cl1A \\sim Cl2A \\sim C80A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C31 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Cl1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O9) = Uanis(C81)
4. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(C80A)=Sof(H80C)=Sof(H80D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C80)=Sof(H80A)=Sof(H80B)=FVAR(1)
5.a Riding coordinates:
 C20(H20A,H20B,H20C)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C30(H30A,H30B), C31(H31A,H31B), C52(H52A,
 H52B), C53(H53A,H53B), C71(H71A,H71B), C72(H72A,H72B), C80(H80A,H80B),
 C80A(H80C,H80D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C17(H17), C22(H22),
 C25(H25), C26(H26), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C44(H44),
  C47(H47), C48(H48), C55(H55), C56(H56), C57(H57), C58(H58), C63(H63),
 C66(H66), C67(H67), C74(H74), C75(H75), C76(H76), C77(H77), C81(H81)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C27(H27A,H27B,H27C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C61(H61A,H61B,
 H61C), C68(H68A,H68B,H68C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C)
;
_shelx_res_checksum              10226
_shelx_hkl_checksum              63700
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU