#------------------------------------------------------------------------------
#$Date: 2019-11-26 13:22:32 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243421 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/37/4133700.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_4133700
loop_
_publ_author_name
'Joo, Wontae'
'Wang, Wade'
'Mesch, Ryan'
'Matsuzawa, Kensuke'
'Liu, Di'
'Willson, C. Grant'
_publ_section_title
;
 Synthesis of Unzipping Polyester and a Study of its Photochemistry.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14736
_journal_page_last               14741
_journal_paper_doi               10.1021/jacs.9b06285
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C32 H32 O8'
_chemical_formula_sum            'C32 H32 O8'
_chemical_formula_weight         544.57
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2082(7)
_cell_length_b                   16.2082(7)
_cell_length_c                   5.7910(5)
_cell_measurement_reflns_used    4033
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8
_cell_measurement_theta_min      1.77
_cell_volume                     1521.33(16)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction
'CrysAlisPro V 1.171.38.43, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;

Sir2004.  Burla M.C., Caliandro, R., Camalli M., Carrozzini, B., Cascarano G.L., 
De Caro, L., Giacovazzo C., Polidori G., Spagna R. 
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            21548
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.079
_diffrn_reflns_theta_min         1.777
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       needles
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.1110
_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)+(0.0707P)²+1.4460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1678
_reflns_number_total             2343
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b06285_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1521.33(19)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4133700
_shelx_shelxl_version_number     2016/6
_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.
;
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.997
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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
O1 O -0.04070(15) 0.36969(14) 0.4675(5) 0.0514(7) Uani 1 1 d . .
C1 C -0.00600(17) 0.33740(17) 0.3082(5) 0.0299(6) Uani 1 1 d . .
O2 O 0.05664(12) 0.37164(12) 0.1941(4) 0.0322(5) Uani 1 1 d . .
C2 C -0.02975(16) 0.25179(16) 0.2150(5) 0.0276(6) Uani 1 1 d . .
C3 C -0.03181(16) 0.19471(17) 0.4197(5) 0.0299(6) Uani 1 1 d . .
H3 H -0.059913 0.212585 0.554749 0.036 Uiso 1 1 calc R U
C4 C 0.00335(17) 0.12091(18) 0.4224(5) 0.0305(6) Uani 1 1 d . .
H4 H 0.000088 0.089016 0.559752 0.037 Uiso 1 1 calc R U
C5 C 0.04753(17) 0.08583(17) 0.2210(5) 0.0291(6) Uani 1 1 d . .
C6 C 0.06155(17) 0.14716(17) 0.0319(5) 0.0283(6) Uani 1 1 d . .
H6 H 0.095959 0.131778 -0.093690 0.034 Uiso 1 1 calc R U
C7 C 0.02859(17) 0.22128(17) 0.0310(5) 0.0293(6) Uani 1 1 d . .
H7 H 0.042257 0.257544 -0.092054 0.035 Uiso 1 1 calc R U
C8 C -0.11710(18) 0.25937(19) 0.1120(6) 0.0389(8) Uani 1 1 d . .
H8A H -0.115651 0.296221 -0.022105 0.058 Uiso 1 1 calc R U
H8B H -0.154635 0.281969 0.228638 0.058 Uiso 1 1 calc R U
H8C H -0.136556 0.204758 0.063994 0.058 Uiso 1 1 calc R U
H5 H 0.0176(16) 0.0384(17) 0.166(5) 0.019(7) Uiso 1 1 d . .
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
O1 C1 O2 123.8(2) . .
O1 C1 C2 123.1(3) . .
O2 C1 C2 113.1(2) . .
C1 O2 C5 116.7(2) . 7_566
C3 C2 C7 111.7(2) . .
C3 C2 C1 106.5(2) . .
C7 C2 C1 112.8(2) . .
C3 C2 C8 109.5(2) . .
C7 C2 C8 109.2(2) . .
C1 C2 C8 107.1(2) . .
C4 C3 C2 123.7(3) . .
C4 C3 H3 118.2 . .
C2 C3 H3 118.2 . .
C3 C4 C5 123.0(3) . .
C3 C4 H4 118.5 . .
C5 C4 H4 118.5 . .
O2 C5 C4 106.8(2) 8_656 .
O2 C5 C6 108.8(2) 8_656 .
C4 C5 C6 113.2(2) . .
O2 C5 H5 107.5(16) 8_656 .
C4 C5 H5 108.7(17) . .
C6 C5 H5 111.5(17) . .
C7 C6 C5 123.2(3) . .
C7 C6 H6 118.4 . .
C5 C6 H6 118.4 . .
C6 C7 C2 123.5(3) . .
C6 C7 H7 118.3 . .
C2 C7 H7 118.3 . .
C2 C8 H8A 109.5 . .
C2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.201(3) .
C1 O2 1.332(3) .
C1 C2 1.538(4) .
O2 C5 1.477(3) 7_566
C2 C3 1.504(4) .
C2 C7 1.508(4) .
C2 C8 1.541(4) .
C3 C4 1.325(4) .
C3 H3 0.9500 .
C4 C5 1.482(4) .
C4 H4 0.9500 .
C5 C6 1.496(4) .
C5 H5 0.96(3) .
C6 C7 1.315(4) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
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_4
O1 C1 O2 C5 2.6(4) . 7_566
C2 C1 O2 C5 -177.4(2) . 7_566
O1 C1 C2 C3 -51.2(4) . .
O2 C1 C2 C3 128.8(3) . .
O1 C1 C2 C7 -174.0(3) . .
O2 C1 C2 C7 6.0(3) . .
O1 C1 C2 C8 65.9(4) . .
O2 C1 C2 C8 -114.1(3) . .
C7 C2 C3 C4 -9.6(4) . .
C1 C2 C3 C4 -133.1(3) . .
C8 C2 C3 C4 111.4(3) . .
C2 C3 C4 C5 -1.1(4) . .
C3 C4 C5 O2 130.1(3) . 8_656
C3 C4 C5 C6 10.4(4) . .
O2 C5 C6 C7 -127.1(3) 8_656 .
C4 C5 C6 C7 -8.5(4) . .
C5 C6 C7 C2 -2.6(4) . .
C3 C2 C7 C6 11.5(4) . .
C1 C2 C7 C6 131.4(3) . .
C8 C2 C7 C6 -109.8(3) . .
