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_1574692
_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_absolute_configuration ad
_chemical_formula_moiety         'C72 H84 N4 O8 Zn4, C H2 Cl2'
_chemical_formula_sum            'C73 H86 Cl2 N4 O8 Zn4'
_chemical_formula_weight         1479.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-21
_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                90
_cell_angle_beta                 100.8150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6104(3)
_cell_length_b                   17.3943(4)
_cell_length_c                   14.6731(4)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      78.08
_cell_measurement_theta_min      4.80
_cell_volume                     3412.06(14)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            89833
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.276
_diffrn_reflns_theta_min         3.066
_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    2.777
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.5946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1589 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.7884.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         14071
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0288P)^2^+0.9504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0565
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                13709
_reflns_number_total             14071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py01486c2.cif
_cod_data_source_block           cu_240720lu_lgpz160754_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               1574692
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.983(12)
 0.017(12)
2. 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
3. Restrained distances
 Cl1A-C73 \\sim Cl1-C73 \\sim Cl2-C73
 with sigma of 0.02
4. Others
 Sof(H73C)=Sof(H73D)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(H73B)=Sof(H73A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C13(H13), C14(H14), C67(H67), C32(H32), C49(H49), C50(H50), C72(H72)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C33(H33A,H33B), C34(H34A,H34B), C15(H15A,H15B), C36(H36A,
 H36B), C58(H58A,H58B), C35(H35A,H35B), C51(H51A,H51B), C68(H68A,H68B),
 C54(H54A,H54B), C43(H43A,H43B), C17(H17A,H17B), C16(H16A,H16B), C53(H53A,H53B),
  C71(H71A,H71B), C59(H59A,H59B), C69(H69A,H69B), C42(H42A,H42B), C70(H70A,
 H70B), C26(H26A,H26B), C25(H25A,H25B), C8(H8A,H8B), C52(H52A,H52B), C7(H7A,
 H7B), C73(H73B,H73A), C73(H73C,H73D)
5.c Aromatic/amide H refined with riding coordinates:
 C48(H48), C19(H19), C64(H64), C63(H63), C46(H46), C61(H61), C47(H47),
 C62(H62), C22(H22), C24(H24), C23(H23), C4(H4), C45(H45), C5(H5), C1(H1),
 C6(H6)
5.d Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C11(H11A,H11B,H11C), C30(H30A,H30B,H30C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              80041
_shelx_hkl_checksum              53798
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU