PET recycling under mild conditions <i>via</i> substituent-modulated intramolecular hydrolysis.
Zhang, Shengbo; Xue, Yingying; Wu, Yanfen; Zhang, Yu-Xiao; Tan, Ting; Niu, Zhiqiang; Chemical science 14 (2023) 6558–6563; doi:10.1039/d3sc01161e

data_1569206
_publ_section_title
;
 PET recycling under mild conditions <i>via</i> substituent-modulated
 intramolecular hydrolysis.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6558
_journal_page_last               6563
_journal_paper_doi               10.1039/d3sc01161e
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C22 H22 N6 O8 Zn2'
_chemical_formula_sum            'C22 H22 N6 O8 Zn2'
_chemical_formula_weight         629.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-11-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-06 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5336(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.00730(5)
_cell_length_b                   13.58036(7)
_cell_length_c                   19.66015(10)
_cell_measurement_reflns_used    17319
_cell_measurement_temperature    300.51(10)
_cell_measurement_theta_max      66.3820
_cell_measurement_theta_min      3.9240
_cell_volume                     2371.66(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.78a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.51(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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    -46.00 -12.00   0.50    0.50    --   43.60   9.00  60.00   68
  2  \w     84.00 132.00   0.50    0.50    --   43.60  55.00  60.00   96
  3  \w     30.00  58.00   0.50    0.50    --   43.60  55.00  60.00   56
  4  \w     -8.00 132.00   0.50    0.50    --   43.60   9.00  60.00  280
  5  \w     35.00  80.00   0.50    0.50    --   90.00  46.00 -90.00   90
  6  \w    104.00 170.00   0.50    0.50    --   90.00  46.00 -90.00  132
  7  \w    140.00 174.00   0.50    0.50    --   90.00  46.00   0.00   68
  8  \w     62.00  88.00   0.50    0.50    --   90.00  46.00 -30.00   52
  9  \w     24.00  50.00   0.50    0.50    --   90.00  46.00 -60.00   52
 10  \w    126.00 178.00   0.50    0.50    --   90.00  46.00 -60.00  104
 11  \w     10.00  36.00   0.50    0.50    --   90.00   9.00-180.00   52
 12  \w    119.00 144.00   0.50    0.50    --   90.00   9.00-180.00   50
 13  \w    151.00 177.00   0.50    0.50    --   90.00  46.00 120.00   52
 14  \w    114.00 166.00   0.50    0.50    --   90.00  46.00  60.00  104
 15  \w    129.00 178.00   0.50    0.50    --   90.00  37.00 -30.00   98
 16  \w     48.00  91.00   0.50    0.50    --   90.00  37.00 -30.00   86
 17  \w     26.00  63.00   0.50    0.50    --   90.00  28.00-120.00   74
 18  \w     33.00  59.00   0.50    0.50    --   90.00  46.00 -30.00   52
 19  \w      7.00  32.00   0.50    0.50    --   90.00  46.00  60.00   50
 20  \w    132.00 164.00   0.50    0.50    --   90.00  46.00 -30.00   64
 21  \w     71.00 111.00   0.50    0.50    --   90.00  46.00  30.00   80
 22  \w    147.00 172.00   0.50    0.50    --   90.00  46.00  30.00   50
 23  \w     72.00  98.00   0.50    0.50    --   90.00  18.00  30.00   52
 24  \w    144.00 176.00   0.50    0.50    --   90.00  18.00  30.00   64
 25  \w      2.00 151.00   0.50    0.50    --   90.00  37.00 -60.00  298
 26  \w     38.00 176.00   0.50    0.50    --   90.00  46.00-150.00  276
 27  \w     25.00  51.00   0.50    0.50    --   90.00  46.00   0.00   52
 28  \w      2.00  81.00   0.50    0.50    --   90.00  18.00   0.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1318174000
_diffrn_orient_matrix_UB_12      -0.0348618000
_diffrn_orient_matrix_UB_13      -0.0548916000
_diffrn_orient_matrix_UB_21      0.0675560000
_diffrn_orient_matrix_UB_22      -0.1044607000
_diffrn_orient_matrix_UB_23      0.0033437000
_diffrn_orient_matrix_UB_31      -0.0901771000
_diffrn_orient_matrix_UB_32      -0.0272075000
_diffrn_orient_matrix_UB_33      0.0573747000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20522
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        66.440
_diffrn_reflns_theta_max         66.440
_diffrn_reflns_theta_min         3.974
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.78a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4036
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0413P)^2^+1.2393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3956
_reflns_number_total             4036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01161e2.cif
_cod_data_source_block           h-zn2l2
_cod_depositor_comments
'Adding full bibliography for 1569205--1569212.cif.'
_cod_database_code               1569206
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         CHONZn
_reflns_odcompleteness_completeness 95.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O7) = Uanis(O7A)
3. Others
 Sof(O7A)=1-FVAR(1)
 Sof(O7)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C9(H9A,H9B), C11(H11A,H11B), C14(H14A,H14B),
 C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C2(H2), C8(H8), C6(H6), C16(H16), C22(H22), C21(H21),
 C15(H15), C20(H20)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.743