#------------------------------------------------------------------------------
#$Date: 2024-12-10 04:51:12 +0200 (Tue, 10 Dec 2024) $
#$Revision: 296811 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312730.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312730
loop_
_publ_author_name
'Hollenwäger, Dirk'
'Bockmair, Valentin'
'Kornath, Andreas J.'
_publ_section_title
;
 The crystal structures of methyl prop-2-ynoate, dimethyl fumarate and
 their protonated species.
;
_journal_coeditor_code           OJ3025
_journal_issue                   1
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624011653
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          'C4 H4 O2'
_chemical_formula_moiety         'C4 H4 O2'
_chemical_formula_sum            'C4 H4 O2'
_chemical_formula_weight         84.07
_chemical_name_systematic
;
Methyl prop-2-ynoate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 99.910(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.8409(5)
_cell_length_b                   15.593(2)
_cell_length_c                   7.6149(10)
_cell_measurement_reflns_used    1269
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      31.4840
_cell_measurement_theta_min      3.0100
_cell_volume                     449.26(10)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      111(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Rigaku Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.878
_diffrn_reflns_theta_min         3.013
_diffrn_source_current           40
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2020)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             176
_exptl_crystal_size_max          0.997
_exptl_crystal_size_mid          0.557
_exptl_crystal_size_min          0.306
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0475P)^2^+0.0483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                891
_reflns_number_total             1060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oj3025.cif
_cod_data_source_block           I
_cod_original_cell_volume        449.27(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2312730
_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   0.906
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_file
;
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   0   0  -3-32.6414 98.4431   8
   0   0  -4 140034. 2524.22   8
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   0   1  -3 154435. 2199.91   8
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   0   1  -4 251.036 147.742   8
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   0  -1  -7 155.900 194.589   8
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   0   3  -7 569.815 247.215   8
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   0   5   8 344.182 319.534   4
   0   5  -8 377.359 211.931   8
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   0   5   9 1766.51 578.131   4
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   2   1  -7 34448.0 1714.80   8
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   2  -1  -7 34563.5 1684.94   8
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   2   1  -3 100207. 1828.29   8
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   2   1   3 32817.7 1013.18   3
   2   1   3 33966.4 1586.48   4
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   2   1   4 10360.2 970.568   4
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   2   1   5 26511.9 1692.67   4
   2   1   6 245.679 252.314   4
   2  -1   6 2.59429 302.602   4
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   2   1   7 5280.59 893.795   4
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   2   2  -9 1108.50 351.487   8
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   2  -2  -8 6439.81 787.152   8
   2   2  -8 6276.07 808.681   8
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   2  -2  -7 19693.2 1255.35   8
   2   2  -7 19935.9 1285.52   8
   2   2  -6 11890.7 921.943   8
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   2  -2  -6 12936.6 917.907   8
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   2   6   6 11872.8 1394.09   4
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   2   6   7 11326.6 1451.18   4
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   2   6   8 15009.6 1762.89   4
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   2   7  -9-30.4791 127.124   8
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   2   7  -8 239.525 232.781   8
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   2   7  -7 463.722 215.336   8
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   2   7  -6 52260.7 2136.54   8
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   2   7  -5 11580.5 934.718   8
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   2   7  -4 39264.0 1640.89   8
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   2   7  -3 3762.44 479.574   8
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   2   7  -2 119679. 1505.06   2
   2   7  -2 127797. 3100.19   5
   2   7  -2 127009. 2683.70   8
   2  -7  -2 121267. 1266.45   5
   2  -7  -2 125229. 1754.87   4
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   2   7   0 136310. 3887.41   5
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   2  12   1 65821.4 1914.92   1
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   2  12   4-374.890 452.492   5
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   2  12   5 992.076 326.212   5
   2  12   5 1790.57 588.242   4
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   2  12   6 535.996 351.330   4
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   2  12   6-265.510 468.984   5
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   2  12   7-525.631 574.742   5
   2  12   7 497.277 470.326   4
   2  12   8-780.590 728.676   5
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   2  13  -7 853.399 398.589   8
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   2  13  -4 2275.91 506.137   8
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   2  13  -2 8455.08 889.335   8
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   2  13  -1 808.414 235.380   2
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   2  13   0 1509.09 471.405   5
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   2  14   2 43311.1 2662.30   5
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   3   0  -8-12.8684 170.131   8
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   3   0  -7 36875.8 1705.29   8
   3   0  -6 84.6003 132.259   8
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   3   0  -5 23861.4 1096.05   8
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   3   0   2 85.5145 95.6264   4
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   3   0   3 196611. 4138.79   4
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   3   0   5 3983.16 730.994   4
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   3   1 -10 11455.6 1205.26   8
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   3  -1  -9 3054.70 591.807   8
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   3   1  -9 3421.18 614.998   8
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   3  -1  -8 1709.97 414.921   8
   3   1  -8 1827.37 451.002   8
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   3  -1  -7 13908.5 1035.29   8
   3   1  -7 13007.5 1033.75   8
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   3  -1  -6 30990.7 1386.67   8
   3   1  -6 30730.0 1422.54   8
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   3  -1  -4 2.33825 69.0767   8
   3   1  -4-62.4435 62.7670   8
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   3  -1  -3 4422.05 448.239   5
   3   1  -3 4971.33 544.157   5
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   3   1  -3 4343.54 402.357   8
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   3   1  -2 39014.3 1145.04   8
   3   1  -2 38092.4 1825.28   5
   3  -1  -2 39238.3 1723.60   5
   3  -1  -2 36823.5 864.123   8
   3  -1  -1 187.777 60.5065   8
   3   1  -1 126.749 87.3014   8
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   3   1  -1-60.0310 239.823   5
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   3   1   2 4223.86 566.965   4
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   3  -1   3 686.084 352.419   4
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   3   1   3 957.894 369.633   4
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   3   1   4 16059.2 1340.49   4
   3  -1   4 16522.5 1328.59   4
   3   1   5 3739.00 726.027   4
   3  -1   5 3497.70 691.924   4
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   3   1   6 7891.14 1135.00   4
   3  -1   6 9140.45 1211.97   4
   3   1   7-79.9262 174.787   4
   3  -1   7 177.373 321.768   4
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   3   1   8 999.470 453.636   4
   3  -1   8 1297.27 516.987   4
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   3   2 -10 46.8874 158.140   8
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   3  -2  -9 888.904 310.274   8
   3   2  -9 833.067 346.389   8
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   3  -2  -8 1272.06 359.350   8
   3   2  -8 1840.95 470.841   8
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   3  -2  -7 4840.23 603.706   8
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   3   2  -7 5013.65 661.128   8
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   3  -2  -6 13930.5 917.728   8
   3   2  -6 13810.4 985.468   8
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   3  -2  -5 8168.86 620.684   8
   3   2  -5 7949.20 679.477   8
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   3  -2  -4 2493.37 303.078   8
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   3   2  -4 2739.88 357.967   8
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   3  -2  -3 2760.79 327.175   5
   3   2  -3 2685.37 431.760   5
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   3  -2  -3 2584.16 244.562   8
   3   2  -3 2484.77 321.909   8
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   3   2  -2 23338.2 1482.43   5
   3  -2  -2 22712.3 1256.44   5
   3  -2  -2 22266.7 531.245   8
   3   2  -2 22394.3 927.976   8
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   3   2  -1 16254.7 1329.79   5
   3  -2  -1 16919.9 455.077   8
   3  -2  -1 15815.7 374.959   8
   3   2  -1 17999.0 834.522   8
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  -3   2   0 423.334 183.741   3
  -3  -2   0 376.547 185.177   3
   3  -2   0 506.209 117.971   4
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   3   8  -4 93730.4 2733.74   8
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   3   8  -2 46720.5 2307.38   5
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   3   8   3-11.0496 348.583   5
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   3   8   4 3165.58 714.312   4
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   3  12   2 24539.5 2302.53   5
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   3  13  -7 7356.25 995.553   8
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   3  13  -5 4388.36 717.798   8
   3  13  -4 988.671 356.949   8
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   3  13   3 4184.40 1078.00   5
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   3  13   4 324.943 341.466   5
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   3  13   5 4647.39 1189.76   5
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   3  14  -7 3748.88 729.569   8
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   3  14  -6 2884.65 637.002   8
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   3  14  -5 2730.02 567.042   8
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   3  14   0 709.306 424.244   5
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   3  14   1 9781.07 1386.74   5
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   3  14   2 20934.7 2154.02   5
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   3  14   4 8188.23 1510.91   5
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   3  14   5 696.553 652.603   5
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   3  15  -5 727.266 260.159   8
   3  15  -4 341.406 265.279   8
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   3  15   3 1563.56 731.251   5
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   3  15   4 3303.40 979.480   5
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   4   0  -3 13.8846 132.465   5
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   4   0  -2 1754.17 454.960   5
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   4   1  -3 331.098 201.397   5
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   4   1  -2 1201.42 411.343   5
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   4   1  -1 5017.81 847.933   5
   4  -1  -1 5431.94 809.078   5
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   4   1   0 205.845 170.218   5
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   4   5   1 8838.73 1300.70   5
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   4   5   6-25.0994 156.118   4
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   4   6  -5 13914.9 1088.02   8
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   4   6  -4 15263.0 1102.96   8
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   4   6  -3 25147.7 1695.13   5
   4   6  -3 25949.7 1408.84   8
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   4   6  -2 42194.2 2503.84   5
   4   6  -2 46514.5 1874.76   8
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   4   6  -1 8010.69 1190.03   5
   4   6  -1 8614.00 799.331   8
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   4   6   5 664.179 384.787   4
   4   6   6 628.390 368.388   4
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   4   7  -5-71.8002 129.837   8
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   4   7  -4 15319.4 1152.63   8
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   4   7  -3 1313.83 349.000   8
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   4   7  -3 987.591 409.967   5
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   4   7  -2 758.905 295.595   8
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   4   7  -2 1176.45 501.354   5
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   4   7  -1 2335.72 433.615   8
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   4   7  -1 2846.00 781.482   5
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   4   7   0 20706.8 2040.19   5
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   4   7   1 2869.34 760.019   5
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   4   7   2 5862.14 1130.16   5
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   4   7   5 377.060 367.559   4
   4   8  -8 332.231 223.865   8
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   4   8  -7 584.502 257.248   8
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   4   8  -6 2299.28 497.909   8
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   4   8  -5 4674.08 701.914   8
   4   8  -4 1736.67 445.186   8
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   4   8  -3 42598.2 2352.24   5
   4   8  -3 43681.2 1985.18   8
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   4   8  -2 245.263 102.823   8
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   4   8  -2 333.882 237.460   5
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   4   8  -1 18599.5 1851.21   5
   4   8  -1 20258.5 1344.34   8
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   4   8   2 527.709 293.509   5
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   4   8   3-341.825 479.929   5
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   4   8   4-660.412 771.041   5
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   4   8   5 784.598 378.731   4
   4   9  -8 452.420 208.348   8
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   4   9  -7 1399.73 424.358   8
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   4   9  -6 1333.73 399.389   8
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   4   9  -5 181.114 147.642   8
   4   9  -4 330.648 202.227   8
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   4   9  -3 12909.7 1115.74   8
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   4   9  -2 15.8538 173.036   8
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   4   9  -1 38.3203 148.083   8
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   4   9  -1 478.176 291.137   5
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   4   9   0 712.087 425.002   5
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   4   9   1 798.105 425.065   5
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   4   9   2 1849.07 717.837   5
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   4  10  -7 243.112 241.202   8
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   4  10  -6-74.9689 214.492   8
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   4  10  -5 3113.74 596.804   8
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   4  10  -4 4218.23 682.434   8
   4  10  -3 669.975 297.324   8
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   4  10  -2 92.3507 175.351   8
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   4  10  -2 120.145 230.685   5
   4  10  -1 327.333 230.914   8
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   4  10  -1 417.339 441.115   5
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   4  10   0-31.9242 122.667   8
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   4  10   0-48.4967 277.826   5
   4  10   1 635.364 596.189   5
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   4  10   2-70.9303 437.797   5
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   4  10   3-125.312 385.178   5
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   4  11  -7 97.5626 154.495   8
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   4  11  -6 785.489 245.418   8
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  -4  11   5 592.909 321.831   2
   4  11  -5 902.863 380.562   8
   4  11  -4 415.761 222.114   8
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   4  11  -3 1090.55 311.952   8
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   4  11  -2 2255.34 505.315   8
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   4  11  -2 2579.66 712.865   5
  -4  11   2 1961.89 474.958   2
  -4  11   1 2809.63 506.692   3
  -4  11   1 3200.23 605.334   2
   4  11  -1 3188.54 816.935   5
   4  11  -1 3675.05 641.511   8
  -4 -11   1 3105.66 664.769   3
   4  11   0 724.026 281.830   8
  -4  11   0 826.854 332.324   2
   4  11   0 1623.92 657.217   5
   4  11   1 865.226 493.627   5
  -4  11  -2 445.663 273.206   7
  -4  11  -2 1689.42 555.613   6
   4  11   2 1756.86 686.030   5
  -4  11  -3-25.2534 173.016   7
  -4  11  -3 608.476 407.652   6
   4  11   3 275.830 581.611   5
  -4  11  -4 504.388 430.973   6
  -4  12   6-103.333 189.539   3
   4  12  -6 207.934 171.950   8
  -4  12   5 9860.70 1118.39   2
  -4  12   5 9742.80 1054.10   3
   4  12  -5 11536.9 1192.50   8
   4  12  -4 203.932 215.072   8
  -4  12   4 176.128 218.884   3
  -4  12   4 287.415 232.482   2
   4  12  -3 460.351 267.462   8
  -4  12   3 300.381 235.439   3
  -4  12   3 470.995 211.274   2
   4  12  -2 200.696 230.409   8
  -4  12   2-63.0299 152.227   3
  -4  12   2 234.252 109.278   2
   4  12  -1 81.1584 126.257   8
  -4  12   1-58.2392 151.375   3
  -4  12   1 439.449 292.568   2
   4  12  -1 140.901 286.735   5
   4  12   0 1198.61 386.263   8
  -4  12   0 1491.26 449.569   2
   4  12   0 1278.52 621.102   5
  -4  12  -1 6515.56 913.042   7
   4  12   1 8835.45 1488.17   5
  -4  12  -2-108.212 219.258   7
   4  12   2 1534.77 852.480   5
  -4  12  -3 6492.47 988.621   7
  -4  12  -3 8581.23 1151.59   6
   4  12   3 7522.39 1520.88   5
  -4  12  -4 1250.24 523.133   6
   4  13  -6 5721.07 902.403   8
  -4  13   5 203.282 286.196   3
  -4  13   5 83.9552 235.212   2
   4  13  -5 136.769 203.666   8
   4  13  -4 3238.73 641.979   8
  -4  13   4 2646.53 571.969   3
  -4  13   4 2436.95 584.024   2
   4  13  -3 427.856 230.913   8
  -4  13   3 606.230 269.547   3
  -4  13   3 235.970 157.915   2
   4  13  -2 91.9334 136.399   8
  -4  13   2 343.979 187.676   3
  -4  13   2 60.0613 178.321   2
   4  13  -1 1242.34 385.651   8
  -4  13   1 1499.69 462.390   2
   4  13  -1 1408.55 508.038   5
   4  13   0 1267.95 412.678   8
  -4  13   0 971.342 347.163   2
   4  13   0 1441.21 580.442   5
  -4  13  -1 314.577 271.697   7
   4  13   1 979.080 647.202   5
  -4  13  -2-41.4625 142.230   7
   4  13   2 399.168 491.137   5
  -4  13  -3 1152.29 513.462   6
  -4  14   5 1479.40 484.759   2
   4  14  -5 1607.77 479.118   8
   4  14  -4 738.970 335.381   8
  -4  14   4 795.178 327.653   3
  -4  14   4 808.509 362.815   2
   4  14  -3 2331.56 559.664   8
  -4  14   3 3040.35 576.537   3
  -4  14   3 1868.15 497.742   2
   4  14  -2 295.640 201.681   8
  -4  14   2 392.885 269.973   2
   4  14  -1 1239.43 394.753   8
  -4  14   1 1248.23 440.840   2
   4  14  -1 1148.66 514.194   5
   4  14   0 71.5999 189.804   8
  -4  14   0 152.142 160.788   2
   4  14   0 91.4607 261.618   5
  -4  14  -1 985.565 430.650   7
   4  14   1 841.819 565.968   5
  -4  14  -2 4591.40 837.175   7
  -4  15   5 3015.24 698.939   2
   4  15  -4 588.902 259.905   8
  -4  15   4 288.340 192.972   2
   4  15  -3 109.417 139.951   8
  -4  15   3 87.1729 186.349   2
   4  15  -2-157.533 135.786   8
  -4  15   2 176.033 200.535   2
   4  15  -1 1466.07 459.373   8
   4  15  -1 1196.99 580.472   5
  -4  15   1 929.466 372.537   2
   4  15   0 289.217 244.688   8
  -4  15   0 371.400 256.327   2
   4  15   0 36.7996 296.958   5
  -4  15  -1 2118.45 583.934   7
   4  16  -2-91.0001 228.648   8
  -4  16   2-23.8049 151.428   2
   4  16  -1 789.823 388.702   8
  -4  16  -1 1179.51 444.566   7
  -5   0   6 372.759 341.979   3
  -5   0   5 9939.40 1228.68   3
  -5   0   4-346.498 331.058   3
  -5   0   3 1866.23 510.396   3
  -5   0   2 25.0562 145.389   3
  -5   0   1 619.505 275.783   3
  -5   0   0-95.1887 192.464   6
  -5   0   0-22.4122 132.827   3
   5   0   0-264.006 320.451   5
  -5   0  -1 852.652 447.667   6
   5   0   1 161.728 352.945   5
  -5   0  -2 236.359 252.308   6
  -5   1   6 1256.65 462.141   3
  -5  -1   6 1562.51 586.733   3
  -5   1   5 2695.07 659.805   3
  -5  -1   5 2579.56 683.132   3
  -5   1   4 5562.91 837.118   3
  -5  -1   4 6086.78 937.311   3
  -5   1   3-364.870 288.809   3
  -5  -1   3 275.966 160.225   3
  -5   1   2 51.2525 168.080   3
  -5  -1   2-106.258 164.583   3
  -5   1   1-14.8799 137.979   3
  -5  -1   1-107.014 130.320   3
  -5   1   0 501.879 333.346   6
  -5  -1   0 505.474 339.061   6
  -5   1   0 538.501 225.577   3
  -5  -1   0 702.274 269.096   3
   5   1   0 516.501 336.038   5
  -5   1  -1 903.450 450.993   6
  -5  -1  -1 510.434 300.482   6
   5   1   1 147.351 320.107   5
  -5   1  -2-111.137 180.723   6
  -5  -1  -2 259.393 286.285   6
  -5  -2   6 1848.97 578.795   3
  -5   2   5 750.768 378.865   3
  -5  -2   5 966.429 385.221   3
  -5   2   4 2204.71 512.297   3
  -5  -2   4 2728.59 641.742   3
  -5   2   3 226.973 197.856   3
  -5  -2   3 269.283 261.725   3
  -5   2   2-65.7124 157.606   3
  -5  -2   2 257.150 208.662   3
  -5   2   1-13.3085 144.757   3
  -5  -2   1-68.1349 173.701   3
   5   2  -1-333.541 307.639   5
  -5  -2   0 354.192 302.839   6
  -5   2   0 325.500 231.707   3
   5   2   0 97.0142 274.771   5
  -5   2  -1 2987.98 712.224   6
  -5  -2  -1 3232.85 664.148   6
   5   2   1 1118.79 457.623   5
  -5   2  -2 522.355 350.644   6
  -5  -2  -2 791.879 387.703   6
   5   2   2 173.621 260.621   5
  -5   3   5-47.3223 184.018   3
  -5  -3   5 43.0187 205.579   3
  -5   3   4 157.978 206.630   3
  -5  -3   4 122.014 235.812   3
  -5   3   3 338.112 171.875   3
  -5  -3   3 286.752 243.121   3
  -5   3   2-100.313 126.458   3
  -5  -3   2-55.1263 199.888   3
  -5   3   1 1735.36 412.700   3
   5   3  -1 1993.69 647.608   5
  -5  -3   1 1571.54 395.563   3
  -5  -3   0 131.866 220.854   6
  -5   3   0-110.507 169.420   3
   5   3   0-272.261 423.507   5
  -5   3  -1 2065.49 585.747   6
  -5  -3  -1 1669.76 482.716   6
  -5   3  -1 2137.69 422.037   3
   5   3   1 777.740 404.313   5
  -5   3  -2 837.715 459.813   6
  -5  -3  -2 342.324 290.404   6
  -5   4   5 1141.96 410.188   3
  -5  -4   5 1574.69 522.658   3
  -5   4   4-245.895 327.112   3
  -5  -4   4 169.899 262.960   3
  -5   4   3 6602.98 903.417   3
  -5  -4   3 7760.10 1031.00   3
  -5   4   2 227.799 132.749   3
  -5  -4   2-112.452 198.268   3
  -5   4   1 715.275 287.438   3
   5   4  -1 1045.00 545.162   5
  -5  -4   1 597.800 284.923   3
  -5  -4   0 418.020 332.335   6
  -5   4   0 377.400 239.158   3
   5   4   0-287.312 356.530   5
  -5   4  -1 728.031 439.389   6
  -5  -4  -1 533.467 338.171   6
  -5   4  -1 389.711 198.194   3
   5   4   1-419.961 444.569   5
  -5   4  -2 520.411 357.415   6
  -5  -4  -2 826.033 386.578   6
   5   4   2-265.789 492.798   5
   5   4   3-1385.30 658.130   5
  -5   5   5 952.254 380.316   3
  -5  -5   5 849.552 447.984   3
  -5   5   4 723.593 279.156   3
  -5  -5   4 1210.27 440.317   3
  -5   5   3 1178.10 409.541   3
  -5  -5   3 865.583 353.909   3
  -5   5   2 236.901 227.985   3
   5   5  -2 435.614 309.770   5
  -5  -5   2 602.412 317.674   3
  -5   5   1 1123.90 353.454   3
   5   5  -1 1820.13 624.509   5
  -5  -5   1 872.450 316.890   3
  -5  -5   0 568.888 290.044   6
  -5   5   0 97.1807 117.770   3
   5   5   0-87.8664 325.289   5
  -5   5  -1 356.772 403.512   6
  -5  -5  -1 205.320 246.191   6
  -5   5  -1 363.987 221.304   3
   5   5   1-292.613 410.077   5
  -5  -5  -2 2316.49 578.365   6
   5   5   2 2226.80 760.501   5
  -5  -6   5 155.072 224.968   3
  -5   6   4 5453.24 853.716   3
  -5  -6   4 5714.72 989.815   3
  -5   6   3 5179.71 797.946   3
  -5  -6   3 4928.36 829.876   3
  -5   6   2 7476.66 938.716   3
  -5  -6   2 7268.03 963.017   3
   5   6  -2 7367.01 1112.04   5
  -5   6   1 13882.6 1197.48   3
   5   6  -1 12306.0 1558.67   5
  -5  -6   0 2554.96 584.175   6
  -5   6   0 2435.77 495.848   3
   5   6   0 2750.35 828.562   5
  -5   6  -1 1404.50 556.165   6
  -5  -6  -1 1287.92 429.246   6
  -5   6  -1 1082.18 324.749   3
   5   6   1 912.321 485.158   5
  -5  -6  -2 462.196 299.692   6
   5   6   2 412.538 308.076   5
  -5  -7   5-465.228 343.802   3
  -5   7   4-247.174 278.588   3
  -5  -7   4-21.8137 210.956   3
  -5   7   3 4247.74 714.521   3
   5   7  -3 4006.19 786.837   5
  -5  -7   3 3347.13 722.579   3
  -5   7   2 162.214 238.902   3
   5   7  -2 451.797 357.375   5
  -5  -7   2 3.50569 184.159   3
  -5   7   1 351.972 289.739   3
   5   7  -1 958.745 543.872   5
  -5  -7   0 1791.58 501.710   6
  -5   7   0 1429.27 384.388   3
   5   7   0 1645.39 696.901   5
  -5   7  -1 6486.83 745.989   3
  -5  -7  -1 6261.92 892.624   6
   5   7   1 5955.95 1269.33   5
  -5  -7  -2 867.989 374.281   6
  -5  -8   4 2762.15 712.695   3
  -5   8   3 316.152 234.183   3
  -5  -8   3 560.885 363.807   3
  -5   8   2 13123.8 1228.28   3
  -5  -8   2 12811.9 1285.26   3
   5   8  -2 11651.2 1442.87   5
  -5   8   1 334.750 225.210   3
   5   8  -1 218.880 212.459   5
  -5   8   0 6028.98 764.957   3
   5   8   0 5346.11 1124.28   5
   5   8   1 438.071 421.886   5
  -5  -8  -2 663.339 317.329   6
  -5  -9   4 51.3142 188.427   3
  -5  -9   3 594.224 399.644   3
  -5   9   2 3897.11 674.310   3
   5   9  -2 3915.69 863.707   5
  -5   9   1 89.1799 108.736   3
   5   9  -1 477.269 390.608   5
  -5   9   0 42.3832 128.350   3
   5   9   0 450.103 492.244   5
  -5 -10   4 1372.90 545.666   3
  -5 -10   3 1042.75 451.815   3
   5  10  -2 369.055 320.674   5
   5  10  -1 284.600 269.241   5
  -5 -11   3 98.0566 202.717   3
   5  11  -2 161.656 243.092   5
   0   0   0    0.00    0.00   0
TITL xl021 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073   3.840883  15.593207   7.614937  90.0000  99.9097  90.0000
ZERR    1.00   0.000504   0.001981   0.001040   0.0000   0.0120   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H O
UNIT 16.00 16.00 8.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum              95384
_shelx_res_file
;
TITL shelxt_a.res in P2(1)/n
    shelx.res
    created by SHELXL-2019/3 at 09:15:37 on 24-Sep-2024
CELL  0.71073   3.8409  15.5932   7.6149   90.000   99.910   90.000
ZERR     4.00   0.0005   0.0020   0.0010    0.000    0.012    0.000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    O
UNIT  16 16 8
MERG   2
OMIT     0   2   0
SHEL1000 0.76
FMAP   2
PLAN   20
SIZE     0.306   0.557   0.997
ACTA
BOND
CONF
LIST   4
L.S.  10
TEMP  -162.00
WGHT    0.047500    0.048300
FVAR      20.49327
O2    3    0.313416    0.527417    0.658906    11.00000    0.03821    0.03684 =
         0.02952   -0.00299    0.00969   -0.00010
O1    3    0.127573    0.599897    0.878035    11.00000    0.06351    0.04269 =
         0.03398    0.00416    0.02294    0.01227
C1    1    0.247861    0.597987    0.743116    11.00000    0.02653    0.03610 =
         0.02493    0.00066    0.00309    0.00366
C2    1    0.339261    0.673469    0.650387    11.00000    0.03279    0.04163 =
         0.03084   -0.00101    0.00636    0.00173
C4    1    0.227599    0.447728    0.738788    11.00000    0.03902    0.03564 =
         0.03978    0.00140    0.00560    0.00066
C3    1    0.412947    0.735342    0.575921    11.00000    0.04649    0.04086 =
         0.04625    0.00414    0.01240   -0.00217
H1    2    0.470245    0.783644    0.516938    11.00000    0.05803
H2B   2    0.295108    0.405301    0.664113    11.00000    0.06082
H2A   2    0.362670    0.441354    0.853068    11.00000    0.05750
H2C   2   -0.012968    0.444426    0.741398    11.00000    0.06066
HKLF 4
REM  shelxt_a.res in P2(1)/n
REM wR2 = 0.0986, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0358 for 891 Fo > 4sig(Fo) and 0.0431 for all 1060 data
REM 71 parameters refined using 0 restraints
END
WGHT      0.0490      0.0397
REM Highest difference peak  0.175,  deepest hole -0.148,  1-sigma level  0.033
Q1    1   0.2417  0.7007  0.6338  11.00000  0.05    0.17
Q2    1   0.2328  0.6427  0.6851  11.00000  0.05    0.17
Q3    1   0.4453  0.7052  0.6758  11.00000  0.05    0.15
Q4    1   0.2199  0.5597  0.6780  11.00000  0.05    0.13
Q5    1   0.0730  0.4572  0.8530  11.00000  0.05    0.12
Q6    1   0.0873  0.4038  0.6578  11.00000  0.05    0.12
Q7    1   0.3385  0.4940  0.7025  11.00000  0.05    0.11
Q8    1   0.0933  0.6044  0.7807  11.00000  0.05    0.11
Q9    1   0.2294  0.6255  0.9121  11.00000  0.05    0.10
Q10   1   0.1102  0.5446  0.9426  11.00000  0.05    0.10
Q11   1  -0.0753  0.4376  0.6506  11.00000  0.05    0.09
Q12   1   0.0052  0.6569  0.8765  11.00000  0.05    0.09
Q13   1   0.5035  0.5274  0.5710  11.00000  0.05    0.08
Q14   1  -0.0316  0.6347  0.9195  11.00000  0.05    0.08
Q15   1   0.2953  0.6001  0.8077  11.00000  0.05    0.07
Q16   1   0.5951  0.7416  0.3471  11.00000  0.05    0.06
Q17   1   0.4605  0.6550  0.4750  11.00000  0.05    0.06
Q18   1   0.4405  0.4009  0.7673  11.00000  0.05    0.06
Q19   1   0.5064  0.4444  0.8245  11.00000  0.05    0.06
Q20   1   0.2465  0.6187  1.0695  11.00000  0.05    0.06
;
_shelx_res_checksum              96683
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O2 0.31342(18) 0.52742(5) 0.65891(10) 0.0344(2) Uani d 1 . .
O O1 0.1276(2) 0.59990(5) 0.87804(11) 0.0450(3) Uani d 1 . .
C C1 0.2479(3) 0.59799(6) 0.74312(14) 0.0293(3) Uani d 1 . .
C C2 0.3393(3) 0.67347(7) 0.65039(14) 0.0350(3) Uani d 1 . .
C C4 0.2276(3) 0.44773(8) 0.73879(18) 0.0383(3) Uani d 1 . .
C C3 0.4129(3) 0.73534(8) 0.57592(18) 0.0440(3) Uani d 1 . .
H H1 0.470(4) 0.7836(9) 0.517(2) 0.058(4) Uiso d 1 . .
H H2B 0.295(4) 0.4053(9) 0.664(2) 0.061(5) Uiso d 1 . .
H H2A 0.363(4) 0.4414(9) 0.853(2) 0.057(4) Uiso d 1 . .
H H2C -0.013(4) 0.4444(9) 0.741(2) 0.061(4) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O2 0.0382(4) 0.0368(4) 0.0295(4) -0.0001(3) 0.0097(3) -0.0030(3)
O1 0.0635(6) 0.0427(5) 0.0340(5) 0.0123(4) 0.0229(4) 0.0042(3)
C1 0.0265(5) 0.0361(6) 0.0249(5) 0.0037(4) 0.0031(4) 0.0007(4)
C2 0.0328(5) 0.0416(6) 0.0308(6) 0.0017(4) 0.0064(4) -0.0010(4)
C4 0.0390(6) 0.0356(6) 0.0398(7) 0.0007(4) 0.0056(5) 0.0014(5)
C3 0.0465(7) 0.0409(6) 0.0462(7) -0.0022(5) 0.0124(5) 0.0041(5)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 O2 C4 . . 115.83(9) ?
O1 C1 O2 . . 124.88(10) ?
O1 C1 C2 . . 124.10(10) ?
O2 C1 C2 . . 111.02(9) ?
C3 C2 C1 . . 179.47(11) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O2 C1 . 1.3195(12) ?
O2 C4 . 1.4463(13) ?
O1 C1 . 1.1972(14) ?
C1 C2 . 1.4466(15) ?
C2 C3 . 1.1780(16) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C4 O2 C1 O1 . . . . 0.50(16) ?
C4 O2 C1 C2 . . . . -179.25(9) ?