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#$Date: 2024-02-04 14:33:14 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289650 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/04/1570470.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570470
loop_
_publ_author_name
'Zhou, Tong'
'Guo, Yu-Ting'
'Yang, Chun'
'Meng, Xian-Bin'
'Du, Fu-Sheng'
'Li, Zi-Chen'
_publ_section_title
;
 High-Tg PLA copolymers via base-catalyzed transesterification of PLA with
 2,5,7-trioxabicyclo[2.2.2]octan-6-one
;
_journal_issue                   3
_journal_name_full               'Polymer Chemistry'
_journal_page_first              156
_journal_page_last               165
_journal_paper_doi               10.1039/D3PY01250F
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C5 H6 O4'
_chemical_formula_weight         130.10
_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     dual
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-10-31 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.851(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5342(9)
_cell_length_b                   6.5619(4)
_cell_length_c                   9.7191(10)
_cell_measurement_reflns_used    1326
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      29.6470
_cell_measurement_theta_min      2.4780
_cell_volume                     547.20(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3541
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.562
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1381
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0634
_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/[σ²(Fo²)+(0.0596P)²+0.4400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                994
_reflns_number_total             1381
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3py01250f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1570470--1570474.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1570470
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.3969(2) 0.2299(3) 0.1782(3) 0.0655(6) Uani 1 1 d . . . . .
O2 O 0.32693(17) 0.5556(2) 0.16347(17) 0.0368(4) Uani 1 1 d D . . . .
O3A O 0.5970(7) 0.5753(9) 0.4356(6) 0.0534(12) Uani 0.533(4) 1 d D U P A 1
O3B O 0.6278(8) 0.6097(11) 0.3921(7) 0.0534(12) Uani 0.467(4) 1 d D U P A 2
O4A O 0.6391(6) 0.6061(8) 0.2161(6) 0.0468(11) Uani 0.533(4) 1 d D U P A 1
O4B O 0.6035(8) 0.6286(9) 0.1429(7) 0.0468(11) Uani 0.467(4) 1 d D U P A 2
C1 C 0.4332(3) 0.4054(3) 0.2045(3) 0.0426(6) Uani 1 1 d D U . . .
C2A C 0.5998(9) 0.4756(11) 0.3093(7) 0.0398(13) Uani 0.533(4) 1 d D U P A 1
H2A H 0.6708 0.3586 0.3426 0.048 Uiso 0.533(4) 1 calc R U P A 1
C2B C 0.5911(11) 0.5030(13) 0.2538(8) 0.0398(13) Uani 0.467(4) 1 d D U P A 2
H2B H 0.6676 0.3930 0.2763 0.048 Uiso 0.467(4) 1 calc R U P A 2
C3A C 0.5237(10) 0.7673(14) 0.1552(8) 0.0411(14) Uani 0.533(4) 1 d D U P A 1
H3AA H 0.4736 0.7585 0.0445 0.049 Uiso 0.533(4) 1 calc R U P A 1
H3AB H 0.5757 0.8983 0.1829 0.049 Uiso 0.533(4) 1 calc R U P A 1
C3B C 0.4867(12) 0.7869(17) 0.0998(10) 0.0411(14) Uani 0.467(4) 1 d D U P A 2
H3BA H 0.4135 0.7748 -0.0071 0.049 Uiso 0.467(4) 1 calc R U P A 2
H3BB H 0.5345 0.9207 0.1170 0.049 Uiso 0.467(4) 1 calc R U P A 2
C4A C 0.401(2) 0.755(3) 0.2137(18) 0.0324(10) Uani 0.533(4) 1 d D U P A 1
H4A H 0.3266 0.8685 0.1784 0.039 Uiso 0.533(4) 1 calc R U P A 1
C4B C 0.406(3) 0.753(3) 0.202(2) 0.0324(10) Uani 0.467(4) 1 d D U P A 2
H4B H 0.3263 0.8585 0.1776 0.039 Uiso 0.467(4) 1 calc R U P A 2
C5A C 0.4786(9) 0.7335(12) 0.3851(12) 0.0413(15) Uani 0.533(4) 1 d D U P A 1
H5AA H 0.5261 0.8623 0.4307 0.050 Uiso 0.533(4) 1 calc R U P A 1
H5AB H 0.4003 0.7012 0.4203 0.050 Uiso 0.533(4) 1 calc R U P A 1
C5B C 0.5165(11) 0.7723(14) 0.3679(14) 0.0413(15) Uani 0.467(4) 1 d D . P A 2
H5BA H 0.5675 0.9043 0.3896 0.050 Uiso 0.467(4) 1 calc R U P A 2
H5BB H 0.4626 0.7541 0.4317 0.050 Uiso 0.467(4) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O2 C4A 111.4(10) . . ?
C1 O2 C4B 109.6(11) . . ?
C2A O3A C5A 110.3(6) . . ?
C2B O3B C5B 110.5(7) . . ?
C2A O4A C3A 109.8(6) . . ?
C2B O4B C3B 109.5(7) . . ?
O1 C1 O2 122.1(2) . . ?
O1 C1 C2B 129.1(4) . . ?
O2 C1 C2B 107.6(4) . . ?
O1 C1 C2A 123.3(3) . . ?
O2 C1 C2A 113.9(3) . . ?
O3A C2A O4A 113.0(6) . . ?
O3A C2A C1 108.1(6) . . ?
O4A C2A C1 104.1(4) . . ?
O3A C2A H2A 110.5 . . ?
O4A C2A H2A 110.5 . . ?
C1 C2A H2A 110.5 . . ?
O4B C2B O3B 111.7(7) . . ?
O4B C2B C1 114.3(5) . . ?
O3B C2B C1 108.1(6) . . ?
O4B C2B H2B 107.5 . . ?
O3B C2B H2B 107.5 . . ?
C1 C2B H2B 107.5 . . ?
O4A C3A C4A 112.4(11) . . ?
O4A C3A H3AA 109.1 . . ?
C4A C3A H3AA 109.1 . . ?
O4A C3A H3AB 109.1 . . ?
C4A C3A H3AB 109.1 . . ?
H3AA C3A H3AB 107.8 . . ?
O4B C3B C4B 104.6(13) . . ?
O4B C3B H3BA 110.8 . . ?
C4B C3B H3BA 110.8 . . ?
O4B C3B H3BB 110.8 . . ?
C4B C3B H3BB 110.8 . . ?
H3BA C3B H3BB 108.9 . . ?
O2 C4A C3A 105.1(12) . . ?
O2 C4A C5A 102.5(11) . . ?
C3A C4A C5A 109.5(13) . . ?
O2 C4A H4A 113.0 . . ?
C3A C4A H4A 113.0 . . ?
C5A C4A H4A 113.0 . . ?
O2 C4B C5B 113.0(14) . . ?
O2 C4B C3B 108.6(13) . . ?
C5B C4B C3B 112.0(14) . . ?
O2 C4B H4B 107.7 . . ?
C5B C4B H4B 107.7 . . ?
C3B C4B H4B 107.7 . . ?
O3A C5A C4A 112.1(12) . . ?
O3A C5A H5AA 109.2 . . ?
C4A C5A H5AA 109.2 . . ?
O3A C5A H5AB 109.2 . . ?
C4A C5A H5AB 109.2 . . ?
H5AA C5A H5AB 107.9 . . ?
O3B C5B C4B 103.4(13) . . ?
O3B C5B H5BA 111.1 . . ?
C4B C5B H5BA 111.1 . . ?
O3B C5B H5BB 111.1 . . ?
C4B C5B H5BB 111.1 . . ?
H5BA C5B H5BB 109.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.198(3) . ?
O2 C1 1.343(3) . ?
O2 C4A 1.468(14) . ?
O2 C4B 1.463(15) . ?
O3A C2A 1.402(8) . ?
O3A C5A 1.453(9) . ?
O3B C2B 1.418(10) . ?
O3B C5B 1.450(11) . ?
O4A C2A 1.410(6) . ?
O4A C3A 1.454(7) . ?
O4B C2B 1.402(7) . ?
O4B C3B 1.445(10) . ?
C1 C2B 1.509(10) . ?
C1 C2A 1.537(8) . ?
C2A H2A 0.9800 . ?
C2B H2B 0.9800 . ?
C3A C4A 1.509(15) . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C3B C4B 1.511(15) . ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C4A C5A 1.507(14) . ?
C4A H4A 0.9800 . ?
C4B C5B 1.501(15) . ?
C4B H4B 0.9800 . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C5B H5BA 0.9700 . ?
C5B H5BB 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4A O2 C1 O1 177.9(6) . . . . ?
C4B O2 C1 O1 -176.3(7) . . . . ?
C4B O2 C1 C2B -7.6(8) . . . . ?
C4A O2 C1 C2A 7.4(7) . . . . ?
C5A O3A C2A O4A 62.3(7) . . . . ?
C5A O3A C2A C1 -52.4(6) . . . . ?
C3A O4A C2A O3A -61.4(8) . . . . ?
C3A O4A C2A C1 55.7(7) . . . . ?
O1 C1 C2A O3A -116.2(5) . . . . ?
O2 C1 C2A O3A 54.2(5) . . . . ?
O1 C1 C2A O4A 123.4(4) . . . . ?
O2 C1 C2A O4A -66.2(5) . . . . ?
C3B O4B C2B O3B -65.5(9) . . . . ?
C3B O4B C2B C1 57.6(9) . . . . ?
C5B O3B C2B O4B 63.7(9) . . . . ?
C5B O3B C2B C1 -62.9(6) . . . . ?
O1 C1 C2B O4B 111.1(6) . . . . ?
O2 C1 C2B O4B -56.6(7) . . . . ?
O1 C1 C2B O3B -123.8(5) . . . . ?
O2 C1 C2B O3B 68.5(5) . . . . ?
C2A O4A C3A C4A 2.6(10) . . . . ?
C2B O4B C3B C4B 2.9(10) . . . . ?
C1 O2 C4A C3A 52.0(12) . . . . ?
C1 O2 C4A C5A -62.5(12) . . . . ?
O4A C3A C4A O2 -60.1(13) . . . . ?
O4A C3A C4A C5A 49.4(13) . . . . ?
C1 O2 C4B C5B -57.1(16) . . . . ?
C1 O2 C4B C3B 67.9(15) . . . . ?
O4B C3B C4B O2 -64.5(16) . . . . ?
O4B C3B C4B C5B 61.0(17) . . . . ?
C2A O3A C5A C4A -4.0(9) . . . . ?
O2 C4A C5A O3A 62.6(13) . . . . ?
C3A C4A C5A O3A -48.6(13) . . . . ?
C2B O3B C5B C4B 0.9(9) . . . . ?
O2 C4B C5B O3B 60.6(17) . . . . ?
C3B C4B C5B O3B -62.4(15) . . . . ?
