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_1569210
_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 H24 Cl2 N4 O4 Zn2, 2(N O3)'
_chemical_formula_sum            'C22 H24 Cl2 N6 O10 Zn2'
_chemical_formula_weight         734.11
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-02-26
_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                 105.3664(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.37106(7)
_cell_length_b                   17.24574(11)
_cell_length_c                   9.47691(8)
_cell_measurement_reflns_used    13998
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      66.5340
_cell_measurement_theta_min      4.7740
_cell_volume                     1319.226(18)
_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      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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     75.00 133.00   0.50    0.50    --   43.60  55.00 -90.00  116
  2  \w     69.00 133.00   0.50    0.50    --   43.60  37.00  60.00  128
  3  \w     19.00  51.00   0.50    0.50    --   43.60  37.00  60.00   64
  4  \w      4.00  70.00   0.50    0.50    --   43.60  55.00 -90.00  132
  5  \w    102.00 133.00   0.50    0.50    --   43.60  55.00 -60.00   62
  6  \w    -44.00 133.00   0.50    0.50    --   43.60  55.00   0.00  354
  7  \w     35.00  61.00   0.50    0.50    --   90.00  46.00   0.00   52
  8  \w     75.00 110.00   0.50    0.50    --   90.00  46.00-150.00   70
  9  \w     54.00  80.00   0.50    0.50    --   90.00  37.00-180.00   52
 10  \w    138.00 164.00   0.50    0.50    --   90.00  46.00  60.00   52
 11  \w      1.00  69.00   0.50    0.50    --   90.00   9.00-150.00  136
 12  \w    118.00 172.00   0.50    0.50    --   90.00  46.00-150.00  108
 13  \w    142.00 178.00   0.50    0.50    --   90.00  28.00-120.00   72
 14  \w     36.00 101.00   0.50    0.50    --   90.00  18.00 150.00  130
 15  \w     74.00 122.00   0.50    0.50    --   90.00  46.00  60.00   96
 16  \w    100.00 172.00   0.50    0.50    --   90.00  46.00 -90.00  144
 17  \w     76.00 118.00   0.50    0.50    --   90.00  46.00  90.00   84
 18  \w     15.00  40.00   0.50    0.50    --   90.00  46.00  90.00   50
 19  \w    114.00 174.00   0.50    0.50    --   90.00  46.00 -30.00  120
 20  \w     15.00  41.00   0.50    0.50    --   90.00  37.00  30.00   52
 21  \w     81.00 106.00   0.50    0.50    --   90.00  37.00  30.00   50
 22  \w    133.00 163.00   0.50    0.50    --   90.00  37.00  30.00   60
 23  \w      3.00  64.00   0.50    0.50    --   90.00  46.00  60.00  122
 24  \w    125.00 178.00   0.50    0.50    --   90.00   9.00-150.00  106
 25  \w    102.00 130.00   0.50    0.50    --   90.00  28.00   0.00   56
 26  \w      1.00 112.00   0.50    0.50    --   90.00  28.00-120.00  222
 27  \w    123.00 179.00   0.50    0.50    --   90.00  46.00 -60.00  112
 28  \w     83.00 179.00   0.50    0.50    --   90.00  46.00 120.00  192
 29  \w     17.00  42.00   0.50    0.50    --   90.00  37.00   0.00   50
 30  \w    106.00 131.00   0.50    0.50    --   90.00  18.00 150.00   50
 31  \w     12.00  37.00   0.50    0.50    --   90.00  46.00 -60.00   50
 32  \w    101.00 172.00   0.50    0.50    --   90.00  46.00   0.00  142
 33  \w    139.00 164.00   0.50    0.50    --   90.00  37.00   0.00   50
 34  \w    134.00 159.00   0.50    0.50    --   90.00  46.00  30.00   50
 35  \w     54.00  80.00   0.50    0.50    --   90.00  46.00-180.00   52
 36  \w    118.00 161.00   0.50    0.50    --   90.00  46.00-180.00   86
 37  \w     32.00  61.00   0.50    0.50    --   90.00  46.00 -90.00   58
 38  \w      1.00  43.00   0.50    0.50    --   90.00  37.00-180.00   84
 39  \w      4.00 173.00   0.50    0.50    --   90.00  53.00 119.66  338
;
_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      0.0785379000
_diffrn_orient_matrix_UB_12      -0.0784491000
_diffrn_orient_matrix_UB_13      0.0579526000
_diffrn_orient_matrix_UB_21      -0.0845098000
_diffrn_orient_matrix_UB_22      -0.0380546000
_diffrn_orient_matrix_UB_23      -0.1480222000
_diffrn_orient_matrix_UB_31      0.1521061000
_diffrn_orient_matrix_UB_32      0.0193831000
_diffrn_orient_matrix_UB_33      -0.0560775000
_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  0.0166
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17264
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         6.787
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71258
_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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       prism
_exptl_crystal_F_000             744
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol and water'
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0242P)^2^+1.0798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2257
_reflns_number_total             2299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01161e2.cif
_cod_data_source_block           cl-zn2-(no3)
_cod_depositor_comments
'Adding full bibliography for 1569205--1569212.cif.'
_cod_database_code               1569210
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H O N Zn Cl'
_reflns_odcompleteness_completeness 98.03
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10A) = Uanis(C10)
Uanis(C9A) = Uanis(C9)
3. Others
 Sof(H11C)=Sof(H11D)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(H11A)=Sof(H11B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(2)
4.a Rotating group:
 O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C11(H11C,H11D), C10(H10A,H10B), C10A(H10C,H10D),
 C9A(H9AA,H9AB)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C6(H6), C8(H8)
;
_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 2.021
_oxdiff_exptl_absorpt_empirical_full_min 0.760