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_1569209
_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 Br2 N4 O4 Zn2, 2(N O3)'
_chemical_formula_sum            'C24 H23.84 Br2 N4 O10 Zn2'
_chemical_formula_weight         818.87
_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                 104.2460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.50810(10)
_cell_length_b                   17.08160(10)
_cell_length_c                   9.70880(10)
_cell_measurement_reflns_used    8823
_cell_measurement_temperature    271.26(13)
_cell_measurement_theta_max      66.4440
_cell_measurement_theta_min      6.1710
_cell_volume                     1367.61(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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      271.26(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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     88.00 131.00   0.50    0.50    --   43.60  53.00  66.00   86
  2  \w    -46.00  84.00   0.50    0.50    --   43.60  53.00  66.00  260
  3  \w     28.00  54.00   0.50    0.50    --   43.60   9.00-180.00   52
  4  \w    -43.00  15.00   0.50    0.50    --   43.60   9.00-180.00  116
  5  \w    124.00 150.00   0.50    0.50    --   90.00  53.00  66.00   52
  6  \w    106.00 132.00   0.50    0.50    --   90.00  18.00 -60.00   52
  7  \w     43.00 179.00   0.50    0.50    --   90.00  46.00 150.00  272
  8  \w     78.00 179.00   0.50    0.50    --   90.00  28.00   0.00  202
  9  \w     23.00  64.00   0.50    0.50    --   90.00   9.00 -30.00   82
 10  \w     97.00 146.00   0.50    0.50    --   90.00  18.00 -90.00   98
 11  \w      1.00  79.00   0.50    0.50    --   90.00  18.00-180.00  156
 12  \w     83.00 109.00   0.50    0.50    --   90.00  18.00-180.00   52
 13  \w    137.00 163.00   0.50    0.50    --   90.00  18.00-180.00   52
 14  \w      1.00  79.00   0.50    0.50    --   90.00  46.00-150.00  156
 15  \w    149.00 176.00   0.50    0.50    --   90.00  46.00-150.00   54
 16  \w     79.00 128.00   0.50    0.50    --   90.00  37.00  90.00   98
 17  \w    141.00 167.00   0.50    0.50    --   90.00  37.00  90.00   52
 18  \w      3.00  38.00   0.50    0.50    --   90.00  18.00 -60.00   70
 19  \w     83.00 108.00   0.50    0.50    --   90.00  53.00  66.00   50
 20  \w    114.00 165.00   0.50    0.50    --   90.00  37.00 -60.00  102
 21  \w      2.00  32.00   0.50    0.50    --   90.00  37.00  30.00   60
 22  \w    151.00 176.00   0.50    0.50    --   90.00  37.00  30.00   50
 23  \w     33.00  67.00   0.50    0.50    --   90.00  46.00  60.00   68
 24  \w    150.00 175.00   0.50    0.50    --   90.00  46.00  60.00   50
 25  \w      1.00  26.00   0.50    0.50    --   90.00  18.00  30.00   50
 26  \w     39.00  65.00   0.50    0.50    --   90.00  53.00  66.00   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      0.0771366000
_diffrn_orient_matrix_UB_12      -0.0662905000
_diffrn_orient_matrix_UB_13      -0.0687448000
_diffrn_orient_matrix_UB_21      -0.0933239000
_diffrn_orient_matrix_UB_22      0.0280937000
_diffrn_orient_matrix_UB_23      -0.1484215000
_diffrn_orient_matrix_UB_31      0.1422969000
_diffrn_orient_matrix_UB_32      0.0542980000
_diffrn_orient_matrix_UB_33      -0.0071204000
_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  0.0209
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_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            10694
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.465
_diffrn_reflns_theta_max         66.465
_diffrn_reflns_theta_min         5.367
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34348
_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 orangish yellow'
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0477P)^2^+1.2012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2283
_reflns_number_total             2372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01161e2.cif
_cod_data_source_block           br-zn2l2new
_cod_depositor_comments
'Adding full bibliography for 1569205--1569212.cif.'
_cod_database_code               1569209
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zn Br'
_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(O00I) = Uanis(O00J)
Uanis(C00M) = Uanis(C00L)
Uanis(C1) = Uanis(C00K)
3. Others
 Sof(O00J)=1-FVAR(1)
 Sof(O00I)=FVAR(1)
 Sof(H00F)=Sof(H00I)=Sof(C00M)=Sof(H00N)=Sof(H00O)=1-FVAR(2)
 Sof(H00D)=Sof(H00E)=Sof(C00L)=Sof(H00L)=Sof(H00M)=FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=1-FVAR(3)
 Sof(C00K)=Sof(H00J)=Sof(H00K)=FVAR(3)
4.a Rotating group:
 O004(H00A,H00B)
4.b Secondary CH2 refined with riding coordinates:
 C00J(H00D,H00E), C00J(H00F,H00I), C00K(H00J,H00K), C00L(H00L,H00M), C00M(H00N,
 H00O), C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00C(H00C), C00G(H00G), C00H(H00H)
;
_shelx_res_checksum              87732
_shelx_hkl_checksum              90553
_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 3.010
_oxdiff_exptl_absorpt_empirical_full_min 0.688