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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/1/57/04/1570471.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_1570471
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            'C6 H8 O4'
_chemical_formula_weight         144.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.6336(3)
_cell_length_b                   10.5499(6)
_cell_length_c                   18.8351(15)
_cell_measurement_reflns_used    1228
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.3560
_cell_measurement_theta_min      3.7520
_cell_volume                     1318.15(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4711
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_min         3.757
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53509
_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    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0426
_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/[σ²(Fo²)+(0.0525P)²+0.4317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1103
_reflns_number_total             1503
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3py01250f2.cif
_cod_data_source_block           3_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1570470--1570474.cif.'
_cod_database_code               1570471
_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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 0.79548(17) 0.31765(13) 0.41363(7) 0.0499(4) Uani 1 1 d . . . . .
O2 O 0.48302(16) 0.25173(10) 0.43180(7) 0.0385(3) Uani 1 1 d . . . . .
O3 O 0.39306(17) 0.50636(10) 0.40878(7) 0.0417(3) Uani 1 1 d . . . . .
O4 O 0.40706(17) 0.37968(12) 0.30757(6) 0.0444(3) Uani 1 1 d . . . . .
C1 C 0.6669(3) 0.52907(17) 0.32891(10) 0.0458(5) Uani 1 1 d . . . . .
H1A H 0.5945 0.5944 0.3042 0.069 Uiso 1 1 calc R U . . .
H1B H 0.7512 0.4842 0.2960 0.069 Uiso 1 1 calc R U . . .
H1C H 0.7490 0.5665 0.3653 0.069 Uiso 1 1 calc R U . . .
C2 C 0.5201(2) 0.43869(14) 0.36204(8) 0.0308(4) Uani 1 1 d . . . . .
C3 C 0.6187(2) 0.33280(15) 0.40438(9) 0.0325(4) Uani 1 1 d . . . . .
C4 C 0.2777(2) 0.29249(16) 0.41542(9) 0.0336(4) Uani 1 1 d . . . . .
H4 H 0.1792 0.2344 0.4365 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2527(3) 0.42329(15) 0.44484(10) 0.0385(4) Uani 1 1 d . . . . .
H5A H 0.1157 0.4525 0.4374 0.046 Uiso 1 1 calc R U . . .
H5B H 0.2797 0.4232 0.4955 0.046 Uiso 1 1 calc R U . . .
C6 C 0.2587(3) 0.29357(19) 0.33615(9) 0.0438(5) Uani 1 1 d . . . . .
H6A H 0.2807 0.2090 0.3175 0.053 Uiso 1 1 calc R U . . .
H6B H 0.1245 0.3208 0.3226 0.053 Uiso 1 1 calc R U . . .
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
C3 O2 C4 110.82(12) . . ?
C2 O3 C5 111.72(11) . . ?
C2 O4 C6 111.58(12) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 O4 111.00(12) . . ?
O3 C2 C1 109.00(13) . . ?
O4 C2 C1 108.80(13) . . ?
O3 C2 C3 107.52(12) . . ?
O4 C2 C3 106.55(12) . . ?
C1 C2 C3 113.97(14) . . ?
O1 C3 O2 121.01(15) . . ?
O1 C3 C2 126.59(15) . . ?
O2 C3 C2 112.39(13) . . ?
O2 C4 C5 107.25(13) . . ?
O2 C4 C6 106.92(13) . . ?
C5 C4 C6 110.65(15) . . ?
O2 C4 H4 110.6 . . ?
C5 C4 H4 110.6 . . ?
C6 C4 H4 110.6 . . ?
O3 C5 C4 108.25(13) . . ?
O3 C5 H5A 110.0 . . ?
C4 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
C4 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
O4 C6 C4 108.60(13) . . ?
O4 C6 H6A 110.0 . . ?
C4 C6 H6A 110.0 . . ?
O4 C6 H6B 110.0 . . ?
C4 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
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 C3 1.1965(19) . ?
O2 C3 1.3446(19) . ?
O2 C4 1.4610(19) . ?
O3 C2 1.4122(18) . ?
O3 C5 1.4477(19) . ?
O4 C2 1.4149(19) . ?
O4 C6 1.443(2) . ?
C1 C2 1.499(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.521(2) . ?
C4 C5 1.496(2) . ?
C4 C6 1.499(2) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 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
C5 O3 C2 O4 62.57(17) . . . . ?
C5 O3 C2 C1 -177.62(14) . . . . ?
C5 O3 C2 C3 -53.61(17) . . . . ?
C6 O4 C2 O3 -58.56(17) . . . . ?
C6 O4 C2 C1 -178.49(15) . . . . ?
C6 O4 C2 C3 58.21(16) . . . . ?
C4 O2 C3 O1 178.04(15) . . . . ?
C4 O2 C3 C2 -2.54(18) . . . . ?
O3 C2 C3 O1 -119.94(18) . . . . ?
O4 C2 C3 O1 120.99(17) . . . . ?
C1 C2 C3 O1 1.0(2) . . . . ?
O3 C2 C3 O2 60.68(16) . . . . ?
O4 C2 C3 O2 -58.39(16) . . . . ?
C1 C2 C3 O2 -178.39(14) . . . . ?
C3 O2 C4 C5 -57.80(17) . . . . ?
C3 O2 C4 C6 60.92(17) . . . . ?
C2 O3 C5 C4 -4.83(19) . . . . ?
O2 C4 C5 O3 62.76(17) . . . . ?
C6 C4 C5 O3 -53.51(18) . . . . ?
C2 O4 C6 C4 -1.57(19) . . . . ?
O2 C4 C6 O4 -59.20(18) . . . . ?
C5 C4 C6 O4 57.29(18) . . . . ?
