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_1569212
_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         'C25 H28 N6 O9 Zn2'
_chemical_formula_sum            'C25 H28 N6 O9 Zn2'
_chemical_formula_weight         687.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-05-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-08 deposited with the CCDC.	2023-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.808(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9701(3)
_cell_length_b                   17.0535(3)
_cell_length_c                   8.0230(2)
_cell_measurement_reflns_used    7985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.0020
_cell_measurement_theta_min      5.1470
_cell_volume                     2706.98(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_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   -114.00 -20.00   1.00    1.00    --  -42.06 -57.00-150.00   94
  2  \w    -76.00 -22.00   1.00    1.00    --  -42.06 125.00 -30.00   54
  3  \w    -69.00  25.00   1.00    1.00    --  -42.06  57.00   0.00   94
  4  \w     14.00  51.00   1.00    1.00    --   42.06  57.00 150.00   37
  5  \w    131.00 165.00   1.00    1.00    --   89.04  77.00  60.00   34
  6  \w     31.00  97.00   1.00    1.00    --   89.04-125.00-120.00   66
  7  \w    113.00 154.00   1.00    1.00    --   89.04  77.00-180.00   41
  8  \w     21.00  55.00   1.00    1.00    --   89.04 -45.00  30.00   34
  9  \w     23.00 121.00   1.00    1.00    --   89.04 -77.00   0.00   98
 10  \w     60.00 104.00   1.00    1.00    --   89.04 -45.00  30.00   44
 11  \w    105.00 132.00   1.00    1.00    --   89.04  77.00   0.00   27
 12  \w     60.00 145.00   1.00    1.00    --   89.04  61.00 -30.00   85
 13  \w     32.00 112.00   1.00    1.00    --   89.04-125.00-150.00   80
 14  \w     64.00 112.00   1.00    1.00    --   89.04-125.00  30.00   48
 15  \w     66.00 160.00   1.00    1.00    --   89.04  61.00-120.00   94
 16  \w    103.00 143.00   1.00    1.00    --   89.04  45.00 120.00   40
 17  \w     41.00  84.00   1.00    1.00    --   89.04 -95.00 -90.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0268050000
_diffrn_orient_matrix_UB_12      -0.0672105000
_diffrn_orient_matrix_UB_13      -0.1009353000
_diffrn_orient_matrix_UB_21      0.0341914000
_diffrn_orient_matrix_UB_22      0.0602251000
_diffrn_orient_matrix_UB_23      -0.1041202000
_diffrn_orient_matrix_UB_31      0.0646104000
_diffrn_orient_matrix_UB_32      -0.0040096000
_diffrn_orient_matrix_UB_33      0.1286038000
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17712
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        65.115
_diffrn_reflns_theta_max         65.115
_diffrn_reflns_theta_min         4.470
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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    1.686
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         4551
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0648P)^2^+3.1194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3935
_reflns_number_total             4551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01161e2.cif
_cod_data_source_block           zn2l2(no3)
_cod_depositor_comments
'Adding full bibliography for 1569205--1569212.cif.'
_cod_database_code               1569212
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H O N Zn'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5A-N5
 1.3 with sigma of 0.02
 C24-C23A
 1.5 with sigma of 0.02
 C23A-C22
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20) = Uanis(C20A)
Uanis(C23) = Uanis(C23A)
4. Others
 Sof(Zn2)=1-FVAR(1)
 Sof(Zn2A)=FVAR(1)
 Sof(Zn1A)=1-FVAR(2)
 Sof(Zn1)=FVAR(2)
 Sof(H19C)=Sof(H19D)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H21C)=Sof(H21D)=1-FVAR(3)
 Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(H21A)=Sof(H21B)=FVAR(3)
 Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(4)
 Sof(C23)=Sof(H23A)=Sof(H23B)=FVAR(4)
 Fixed Sof: O4(0.5) O5(0.5) O9(0.5) H9(0.5) O10(0.5) H10(0.5) O5A(0.5)
 O4A(0.5) H22A(0.5) H22B(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C19(H19C,H19D), C20(H20A,H20B), C20A(H20C,H20D), C21(H21A,
 H21B), C21(H21C,H21D), C22(H22A,H22B), C23(H23A,H23B), C23A(H23C,H23D),
 C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9A), C12(H12), C16(H16), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
5.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10)
;
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.913