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_1569211
_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 F2 N4 O4 Zn2, 2(N O3)'
_chemical_formula_sum            'C22 H24 F2 N6 O10 Zn2'
_chemical_formula_weight         701.21
_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     dual
_audit_creation_date             2022-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-06 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.14410(10)
_cell_length_b                   17.9862(2)
_cell_length_c                   9.44930(10)
_cell_measurement_reflns_used    7229
_cell_measurement_temperature    272.1(8)
_cell_measurement_theta_max      66.4540
_cell_measurement_theta_min      4.9280
_cell_volume                     1307.07(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      272.1(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_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     33.00  69.00   0.50    0.50    --   43.60   0.00-180.00   72
  2  \w     57.00 133.00   0.50    0.50    --   43.60  46.00  90.00  152
  3  \w     78.00 104.00   0.50    0.50    --   43.60   0.00-180.00   52
  4  \w    -32.00  -6.00   0.50    0.50    --   43.60   0.00-180.00   52
  5  \w    -45.00  51.00   0.50    0.50    --   43.60  46.00  90.00  192
  6  \w    141.00 170.00   0.50    0.50    --   90.00  18.00  60.00   58
  7  \w    112.00 138.00   0.50    0.50    --   90.00  18.00  60.00   52
  8  \w    118.00 170.00   0.50    0.50    --   90.00  46.00 120.00  104
  9  \w      1.00  27.00   0.50    0.50    --   90.00  37.00 120.00   52
 10  \w      3.00 177.00   0.50    0.50    --   90.00  46.00  30.00  348
 11  \w     77.00 103.00   0.50    0.50    --   90.00  37.00 120.00   52
 12  \w    143.00 169.00   0.50    0.50    --   90.00  37.00 120.00   52
 13  \w     68.00  94.00   0.50    0.50    --   90.00  28.00-120.00   52
 14  \w     27.00  53.00   0.50    0.50    --   90.00  28.00-120.00   52
 15  \w     63.00 132.00   0.50    0.50    --   90.00   9.00-120.00  138
 16  \w    105.00 178.00   0.50    0.50    --   90.00  46.00-180.00  146
 17  \w     22.00  47.00   0.50    0.50    --   90.00  18.00-180.00   50
 18  \w    147.00 178.00   0.50    0.50    --   90.00  18.00-180.00   62
 19  \w     79.00 173.00   0.50    0.50    --   90.00  37.00-150.00  188
 20  \w      2.00  59.00   0.50    0.50    --   90.00  37.00-180.00  114
 21  \w    116.00 141.00   0.50    0.50    --   90.00  46.00  90.00   50
 22  \w    147.00 173.00   0.50    0.50    --   90.00  46.00 150.00   52
 23  \w     15.00  41.00   0.50    0.50    --   90.00  37.00-150.00   52
;
_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      0.1293611000
_diffrn_orient_matrix_UB_12      0.0414934000
_diffrn_orient_matrix_UB_13      -0.0596612000
_diffrn_orient_matrix_UB_21      -0.0355830000
_diffrn_orient_matrix_UB_22      0.0725854000
_diffrn_orient_matrix_UB_23      0.0714482000
_diffrn_orient_matrix_UB_31      0.1486742000
_diffrn_orient_matrix_UB_32      -0.0187118000
_diffrn_orient_matrix_UB_33      0.1453581000
_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  0.0096
_diffrn_reflns_av_unetI/netI     0.0070
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8116
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        66.442
_diffrn_reflns_theta_max         66.442
_diffrn_reflns_theta_min         6.709
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.006
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61213
_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 colourless'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0308P)^2^+0.7772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2063
_reflns_number_total             2092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01161e2.cif
_cod_data_source_block           f-zn2l22
_cod_depositor_comments
'Adding full bibliography for 1569205--1569212.cif.'
_cod_database_code               1569211
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H O N Zn F'
_reflns_odcompleteness_completeness 89.56
_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(C9) = Uanis(C9A)
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:
 O2(H2a,H2b)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C11(H11c,H11d), C10(H10a,H10b), C10A(H10c,H10d), C9(H9a,H9b),
 C9A(H9Aa,H9Ab)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C7(H7), C6(H6)
;
_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.742