#------------------------------------------------------------------------------
#$Date: 2019-05-25 07:53:46 +0300 (Sat, 25 May 2019) $
#$Revision: 215528 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/29/2242954.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_2242954
loop_
_publ_author_name
'Heger, Dominik'
'Eugene, Alexis J.'
'Parkin, Sean R.'
'Guzman, Marcelo I.'
_publ_section_title
;
Crystal structure of zymonic acid and a redetermination of its precursor,
pyruvic acid
;
_journal_coeditor_code HB7818
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 858
_journal_page_last 862
_journal_paper_doi 10.1107/S2056989019007072
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C3 H4 O3'
_chemical_formula_moiety 'C3 H4 O3'
_chemical_formula_sum 'C3 H4 O3'
_chemical_formula_weight 88.06
_chemical_name_common
;
Pyruvic acid
;
_chemical_name_systematic
;
2-Oxopropanoic acid
;
_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'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 99.0630(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.7486(3)
_cell_length_b 5.1925(2)
_cell_length_c 6.8302(2)
_cell_measurement_reflns_used 6955
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 34.29
_cell_measurement_theta_min 3.84
_cell_volume 376.45(2)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL (Sheldrick, 2008) and CIFFIX (Parkin, 2013)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0248
_diffrn_reflns_av_unetI/netI 0.0198
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 10479
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 34.455
_diffrn_reflns_theta_min 3.839
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.143
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.890
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.554
_exptl_crystal_description 'well-facetted block'
_exptl_crystal_F_000 184
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.220
_exptl_crystal_size_min 0.180
_refine_diff_density_max 0.396
_refine_diff_density_min -0.214
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.076
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 60
_refine_ls_number_reflns 1425
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.076
_refine_ls_R_factor_all 0.0389
_refine_ls_R_factor_gt 0.0313
_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/[\s^2^(Fo^2^)+(0.0299P)^2^+0.1264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0766
_refine_ls_wR_factor_ref 0.0815
_reflns_number_gt 1242
_reflns_number_total 1425
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7818sup1.cif
_cod_data_source_block pyruvic
_cod_database_code 2242954
_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 0.964
_shelx_estimated_absorpt_t_max 0.975
_shelx_hkl_file
;
1 0 0 0.32237 0.18481 1
-1 0 0 0.82638 0.22557 1
2 0 0 1230.68 27.2681 7
2 0 0 1205.03 27.7557 4
-2 0 0 1243.14 28.0537 1
-2 0 0 1231.78 27.8119 4
-3 0 0 0.74003 0.48386 5
-3 0 0 -0.0997 0.31638 4
3 0 0 0.03162 0.23410 7
3 0 0 0.02760 0.26404 7
3 0 0 0.88967 0.52981 5
3 0 0 0.37905 0.37571 1
-3 0 0 0.15880 0.39067 1
3 0 0 0.77534 0.45163 4
-3 0 0 0.84320 0.36198 7
4 0 0 262.165 6.62768 7
4 0 0 264.493 7.80300 4
4 0 0 269.435 6.80233 6
4 0 0 279.178 8.03149 1
-4 0 0 259.983 7.26607 7
-4 0 0 267.202 7.93032 4
-4 0 0 266.900 8.41731 5
4 0 0 269.831 6.57461 7
-4 0 0 266.474 8.22599 1
4 0 0 253.178 8.22196 5
5 0 0 1.47198 0.72586 4
5 0 0 0.12245 0.25531 7
5 0 0 0.37835 0.26746 7
5 0 0 -0.4025 0.66950 5
5 0 0 -0.0959 0.48821 1
-5 0 0 0.81003 0.60020 4
5 0 0 0.46941 0.38056 6
-5 0 0 0.26429 0.50220 1
-5 0 0 1.26708 0.52955 7
-6 0 0 42.4151 3.28438 1
-6 0 0 39.4653 2.60283 7
6 0 0 45.7811 3.54686 5
6 0 0 46.4402 2.10744 6
6 0 0 45.9582 3.06496 1
-7 0 0 1.61547 0.92412 3
7 0 0 0.76360 0.50877 6
7 0 0 0.37031 0.54101 6
7 0 0 1.16870 0.81333 1
-7 0 0 0.46849 0.96480 1
8 0 0 83.5600 2.79593 6
-8 0 0 86.7051 4.95139 3
8 0 0 77.9579 5.26105 5
-9 0 0 2.75646 1.50938 3
-10 0 0 4.05054 1.99915 3
0 -1 0 0.44613 0.39607 1
0 -1 0 0.02910 0.21187 3
0 -1 0 0.13086 0.24786 4
0 -1 0 -0.0373 0.26608 6
0 1 0 0.38348 0.31597 6
0 1 0 0.22572 0.24080 3
0 1 0 0.25047 0.20800 4
-1 -1 0 520.353 11.3848 7
1 -1 0 519.952 11.9446 6
-1 -1 0 500.343 11.4206 3
1 -1 0 497.650 11.9865 5
-1 -1 0 511.586 11.7867 6
1 -1 0 502.592 12.6599 1
1 -1 0 487.147 11.8658 4
-1 -1 0 478.004 11.6257 1
1 -1 0 483.328 11.8506 7
1 1 0 504.927 11.8253 6
-1 1 0 497.612 11.8521 4
-1 1 0 493.866 11.8582 7
-1 1 0 491.738 11.9037 6
-1 1 0 503.397 12.6501 1
-2 -1 0 404.352 9.71226 3
-2 -1 0 420.738 10.2921 5
2 -1 0 413.745 11.2188 1
2 -1 0 415.576 10.2445 7
-2 -1 0 408.172 9.30016 7
-2 -1 0 407.037 9.72314 6
-2 -1 0 406.229 9.64954 1
2 -1 0 415.454 10.2856 7
-2 -1 0 412.373 9.69920 4
2 -1 0 417.479 10.1338 6
2 -1 0 398.124 10.4108 4
2 -1 0 391.083 10.5815 5
2 1 0 392.490 9.74043 3
-2 1 0 418.030 11.2793 1
2 1 0 393.324 10.1060 5
-2 1 0 410.261 10.5747 5
-2 1 0 403.803 10.2568 7
2 1 0 416.991 9.64642 1
-2 1 0 418.130 10.4564 4
2 1 0 407.681 9.78935 6
3 -1 0 6.52054 1.04207 4
3 -1 0 5.35983 1.13604 1
-3 -1 0 5.87740 1.07158 5
3 -1 0 5.67861 1.10721 5
3 -1 0 5.68342 0.78610 6
-3 -1 0 6.07163 0.52454 7
-3 -1 0 5.74279 0.81677 4
-3 -1 0 5.24760 0.67559 1
-3 -1 0 5.64284 0.59254 6
3 -1 0 6.94384 0.91838 7
3 -1 0 5.51219 0.90633 7
-3 -1 0 4.74818 0.73752 3
-3 1 0 5.72994 1.14647 1
3 1 0 5.59599 0.60127 1
3 1 0 4.88440 0.90586 5
3 1 0 4.72947 0.65889 6
-3 1 0 6.37443 1.01660 4
-3 1 0 7.36149 1.01554 7
-3 1 0 5.66397 1.05174 5
4 -1 0 1884.30 41.5290 7
-4 -1 0 1852.97 42.4874 4
4 -1 0 1846.83 43.7562 1
4 -1 0 1813.67 41.8113 6
-4 -1 0 1857.72 41.4970 1
-4 -1 0 1838.43 41.0281 7
-4 -1 0 1856.28 42.3122 3
4 -1 0 1875.50 42.9832 5
4 -1 0 1856.77 41.6413 7
-4 1 0 1755.08 43.2514 5
-4 1 0 1840.14 42.4394 7
4 1 0 1840.88 41.0968 6
4 1 0 1823.21 44.4233 5
4 1 0 1843.02 41.9508 1
-4 1 0 1849.34 43.7481 1
-5 -1 0 32.6851 2.15760 1
-5 -1 0 31.9258 2.23396 4
5 -1 0 29.8567 2.38050 4
5 -1 0 30.1804 2.70352 5
-5 -1 0 31.8101 1.77822 7
5 -1 0 30.9816 1.95842 7
5 -1 0 31.6559 1.96669 7
5 -1 0 32.0210 2.66470 1
5 -1 0 28.1116 1.84432 6
5 1 0 31.0471 2.56565 5
-5 1 0 30.8687 2.80330 1
5 1 0 30.3258 1.87277 1
5 1 0 31.4353 1.63525 6
-5 1 0 32.9225 2.29324 7
-6 -1 0 16.7858 1.81670 3
6 -1 0 17.0176 2.32136 5
6 -1 0 16.7071 2.21461 1
6 -1 0 17.4587 1.51148 7
6 -1 0 18.5002 1.53592 7
-6 -1 0 18.6834 1.85743 1
6 -1 0 16.4882 1.48140 6
6 -1 0 18.3199 2.44852 4
6 1 0 16.0767 1.25397 6
6 1 0 19.3340 2.37636 5
6 1 0 15.5851 1.48304 1
-6 1 0 22.0285 2.52730 1
7 -1 0 110.895 5.88349 1
-7 -1 0 113.438 5.14599 3
7 -1 0 117.310 6.38541 5
7 -1 0 107.659 4.21537 6
7 -1 0 116.442 4.15461 6
7 -1 0 110.839 5.73040 4
7 -1 0 113.571 3.92346 7
7 -1 0 113.143 3.84395 7
-7 -1 0 113.119 5.07771 1
7 1 0 114.402 3.70327 6
7 1 0 117.882 6.09446 5
-7 1 0 114.307 6.48513 1
7 1 0 111.425 4.58090 1
8 -1 0 3.40145 0.85358 6
8 -1 0 0.13485 0.99112 5
8 1 0 3.33745 1.47968 5
-9 -1 0 65.1378 4.47119 3
9 -1 0 58.2085 5.20670 5
-9 1 0 76.5949 5.34599 3
-10 -1 0 2.97195 2.03115 3
0 -2 0 1053.17 26.2885 1
0 -2 0 1195.31 25.5529 6
0 -2 0 1069.10 25.1240 7
0 -2 0 978.652 25.0094 3
0 -2 0 1122.52 25.0975 7
0 -2 0 1103.93 24.9343 4
0 2 0 1046.24 26.3413 1
0 2 0 1097.29 25.7690 6
0 2 0 1152.35 24.4986 4
-1 -2 0 153.115 4.91315 6
1 -2 0 148.957 4.90736 7
1 -2 0 148.041 4.74980 4
1 -2 0 154.004 5.07485 6
1 -2 0 156.619 4.99602 7
-1 -2 0 149.096 4.46771 7
-1 -2 0 153.162 4.05984 4
-1 -2 0 161.092 5.20938 1
1 -2 0 163.113 5.95028 1
-1 -2 0 153.720 4.35573 3
-1 2 0 156.291 4.77529 7
-1 2 0 147.574 4.73973 3
1 2 0 144.667 4.90349 6
-1 2 0 157.636 5.88807 1
-1 2 0 156.076 4.71230 4
1 2 0 152.843 4.52098 3
-1 2 0 150.658 5.08919 6
-2 -2 0 247.498 6.51189 7
2 -2 0 232.098 7.27680 5
-2 -2 0 240.335 6.51139 1
-2 -2 0 248.329 6.83587 1
2 -2 0 245.801 8.31334 1
-2 -2 0 227.243 6.71399 5
2 -2 0 240.503 7.14125 7
2 -2 0 240.968 7.12740 6
-2 -2 0 239.153 6.75246 6
2 -2 0 232.332 7.10431 4
-2 -2 0 242.811 6.19908 3
2 -2 0 238.355 7.13126 7
-2 2 0 236.180 7.13303 6
-2 2 0 230.273 8.24330 1
2 2 0 222.729 6.77191 6
2 2 0 238.273 6.26179 3
-2 2 0 227.740 6.96978 4
-2 2 0 235.404 7.03296 7
3 -2 0 1.41204 0.69997 7
3 -2 0 1.72801 0.69688 4
3 -2 0 -0.2605 0.47365 7
3 -2 0 1.47158 0.75970 5
3 -2 0 1.32259 0.66381 6
-3 -2 0 1.07678 0.65273 5
3 -2 0 1.18310 0.72324 1
-3 -2 0 2.06546 0.49320 1
-3 -2 0 1.02535 0.46529 6
-3 -2 0 1.05274 0.41326 3
3 2 0 0.86949 0.48309 6
-3 2 0 1.17245 0.60412 5
-3 2 0 0.89491 0.68451 4
-3 2 0 0.68989 0.76755 1
3 2 0 0.86289 0.41181 3
-4 -2 0 15.0450 1.63095 5
-4 -2 0 13.6565 1.34766 1
-4 -2 0 15.0849 1.00022 7
-4 -2 0 15.1781 1.25427 3
4 -2 0 12.7708 1.67842 4
4 -2 0 14.2458 1.46638 6
-4 -2 0 13.5864 1.22372 4
4 -2 0 15.2586 1.90256 5
-4 -2 0 15.3727 1.21812 6
4 -2 0 15.1434 2.35395 1
4 -2 0 13.7187 1.54501 7
4 2 0 14.5539 1.35037 6
-4 2 0 13.3252 1.77974 5
-4 2 0 17.3902 2.55497 1
-4 2 0 17.8225 1.75734 4
-4 2 0 11.6161 1.52513 7
4 2 0 13.1497 1.08495 1
5 -2 0 160.603 5.90296 6
5 -2 0 171.220 7.18231 5
-5 -2 0 168.760 5.05925 7
5 -2 0 163.149 6.14536 7
5 -2 0 166.018 6.10348 7
5 -2 0 176.668 6.95600 4
-5 -2 0 173.398 5.80605 4
5 -2 0 179.075 7.75439 1
-5 -2 0 170.715 5.32887 1
-5 2 0 170.961 7.98942 1
5 2 0 170.731 5.14183 1
5 2 0 177.485 5.59065 6
5 2 0 171.587 6.44511 5
-6 -2 0 176.110 5.59532 7
6 -2 0 168.913 6.21487 6
6 -2 0 181.728 7.50919 4
6 -2 0 175.335 7.79074 5
6 -2 0 164.983 8.03177 1
-6 -2 0 179.874 5.70392 1
-6 -2 0 186.837 6.23009 3
-6 -2 0 178.996 6.52700 4
6 -2 0 175.920 6.42645 7
6 2 0 175.931 5.69608 6
-6 2 0 179.437 8.77713 1
6 2 0 179.452 7.13852 5
6 2 0 177.411 5.37898 1
-7 -2 0 0.31624 0.80440 7
7 -2 0 -0.2727 0.73172 7
-7 -2 0 1.12528 0.86832 3
7 -2 0 0.77621 1.05025 6
7 -2 0 -0.1673 1.06539 4
7 -2 0 0.25817 1.05072 5
-7 -2 0 0.13126 0.59504 1
-7 2 0 -0.8857 1.79671 1
7 2 0 -0.4315 0.83550 5
7 2 0 -0.4293 0.61587 6
7 2 0 0.50739 0.48200 1
8 -2 0 3.54190 1.77855 5
8 -2 0 3.41831 1.17823 7
-8 -2 0 2.19874 1.39248 3
8 -2 0 2.07759 1.71530 4
8 2 0 2.96203 1.44124 5
8 2 0 3.92832 0.78810 6
-9 -2 0 200.441 7.96478 3
9 -2 0 204.132 9.94498 5
9 2 0 200.065 9.45621 5
0 -3 0 0.48033 0.47766 6
0 -3 0 -0.5648 0.50960 1
0 -3 0 0.18896 0.52263 7
0 -3 0 0.18942 0.36680 4
0 3 0 0.12966 0.49239 6
0 3 0 0.06422 0.58396 1
0 3 0 0.18986 0.29072 3
0 3 0 1.25497 0.39930 4
1 -3 0 47.9643 2.74281 7
-1 -3 0 46.7429 2.01390 4
1 -3 0 48.3002 2.84677 6
-1 -3 0 47.7412 2.43923 7
-1 -3 0 47.1136 2.31844 3
-1 -3 0 47.2948 2.29373 7
-1 -3 0 49.0180 2.75288 6
1 -3 0 45.2378 3.38254 1
-1 -3 0 47.3380 2.97787 1
1 -3 0 43.2397 2.43043 4
-1 3 0 42.3120 2.34802 7
-1 3 0 49.5489 2.99799 6
-1 3 0 41.1317 2.38424 3
-1 3 0 44.9611 2.31963 4
1 3 0 43.9097 2.76128 6
-1 3 0 45.3305 3.34628 1
1 3 0 49.5870 2.12115 3
-2 -3 0 0.19154 0.40165 3
-2 -3 0 0.06414 0.44850 1
-2 -3 0 0.25745 0.39983 7
2 -3 0 0.29415 0.57798 6
2 -3 0 1.49798 0.88428 1
2 -3 0 0.78664 0.65341 4
2 -3 0 -0.5307 0.52993 7
2 -3 0 0.94955 0.67134 7
2 -3 0 1.16276 0.85112 5
-2 -3 0 1.69469 0.66964 1
-2 -3 0 0.21065 0.46924 6
-2 -3 0 0.39595 0.32851 4
-2 3 0 1.67182 0.62018 3
-2 3 0 0.50185 0.80196 1
2 3 0 0.86807 0.58490 6
2 3 0 0.31060 0.31774 3
-2 3 0 0.84040 0.61574 4
-2 3 0 1.58424 0.59101 7
-2 3 0 -0.3550 0.47490 6
-3 -3 0 20.3104 1.52996 1
3 -3 0 16.0490 1.88033 7
3 -3 0 16.4783 1.87856 4
3 -3 0 15.7328 2.31828 1
3 -3 0 17.1381 1.79678 6
-3 -3 0 18.4792 1.39407 3
3 -3 0 18.1932 2.06523 5
-3 -3 0 16.0393 1.05846 4
-3 -3 0 17.6390 1.35764 7
-3 -3 0 18.0240 1.61838 6
-3 -3 0 17.8320 1.67440 1
-3 -3 0 17.8019 1.71292 5
-3 3 0 16.7842 1.78194 4
3 3 0 14.6468 1.68263 6
-3 3 0 15.7503 2.33510 1
3 3 0 16.5937 1.42101 3
4 -3 0 126.063 5.49001 6
-4 -3 0 134.531 4.40154 7
-4 -3 0 131.461 4.52308 3
4 -3 0 135.027 5.94804 4
4 -3 0 134.938 6.30258 5
-4 -3 0 138.500 5.07504 6
4 -3 0 138.220 5.80895 7
-4 -3 0 140.480 4.88889 1
-4 -3 0 139.697 4.57730 1
-4 -3 0 140.443 4.46639 4
-4 3 0 141.363 7.45636 1
4 3 0 136.100 5.30942 6
4 3 0 131.448 4.74233 3
5 -3 0 547.432 16.0209 4
5 -3 0 524.422 17.7299 1
-5 -3 0 532.884 13.5867 7
-5 -3 0 511.633 15.0203 6
5 -3 0 551.299 16.6146 5
5 -3 0 558.001 15.4635 7
-5 -3 0 546.595 13.3795 1
-5 -3 0 541.214 14.0717 4
-5 -3 0 541.875 13.9745 3
-5 3 0 548.976 18.2440 1
5 3 0 549.118 15.7071 6
-6 -3 0 89.5646 2.71984 1
6 -3 0 87.2475 7.20428 1
6 -3 0 90.0982 5.44050 4
6 -3 0 88.5216 4.75100 7
-6 -3 0 89.2173 3.86540 3
-6 -3 0 87.7545 4.05029 4
6 -3 0 90.2452 5.75491 5
-6 3 0 90.4707 6.64911 1
7 -3 0 100.330 6.00360 4
7 -3 0 104.393 5.20848 7
7 -3 0 90.9163 6.11271 5
-7 -3 0 106.385 4.50133 3
7 3 0 98.0542 4.91444 6
8 -3 0 0.76412 2.23724 5
8 -3 0 1.81446 1.44585 4
-9 -3 0 58.6458 3.71249 3
0 -4 0 7.84808 1.48844 7
0 -4 0 6.56408 1.73233 1
0 -4 0 9.51304 1.31519 4
0 4 0 9.28630 1.11122 3
0 4 0 11.3460 1.07160 4
0 4 0 5.73814 1.60876 1
0 4 0 12.6838 1.97648 6
-1 -4 0 0.48798 0.79556 1
-1 -4 0 -0.0916 0.47955 4
-1 -4 0 1.42935 0.66902 7
-1 -4 0 1.04274 0.74987 7
1 -4 0 1.87428 0.91422 7
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-5 -2 14 18.8308 2.66784 7
5 -2 -14 14.8781 2.60618 7
-5 2 14 13.4009 2.77370 7
-5 2 14 13.9045 2.41013 6
-4 -2 14 29.4019 2.91123 6
4 -2 -14 28.5142 3.30812 7
4 -2 -14 24.8769 4.03058 5
4 -2 -14 36.5385 3.75186 4
-4 -2 14 30.4053 3.15957 7
4 2 -14 24.6488 3.01579 4
-4 2 14 28.6346 3.81706 7
-4 2 14 29.5520 3.31388 6
3 -2 -14 114.994 5.86870 5
3 -2 -14 100.007 7.41219 4
3 -2 -14 104.583 5.88009 3
-3 -2 14 107.496 6.00550 7
-3 -2 14 104.048 5.69978 6
3 -2 -14 97.4010 5.58575 7
-3 2 14 110.250 6.23437 6
3 2 -14 100.806 4.93367 4
2 -2 -14 1.19945 1.51173 5
2 -2 -14 0.61982 1.24408 3
-2 -2 14 0.82332 1.31846 6
-2 -2 14 0.48219 1.24643 7
2 2 -14 0.07589 1.08648 4
-2 2 14 -1.2405 1.37216 6
1 -2 -14 13.7053 2.20224 3
-1 -2 14 14.0685 2.66152 7
-1 -2 14 14.5047 2.45243 6
1 -2 -14 13.0572 2.57029 4
-1 2 14 14.3015 3.23875 7
1 2 -14 15.2155 1.93107 3
-1 2 14 16.6211 2.72411 6
1 2 -14 16.7485 2.11559 4
0 -2 -14 20.9508 2.56273 4
0 -2 -14 18.6508 2.77247 3
0 2 -14 17.6219 2.25396 4
0 2 -14 19.4929 2.12172 3
0 2 14 18.2599 3.04658 7
0 2 14 16.2641 2.95577 6
-1 -2 -14 43.3855 3.90053 4
-1 -2 -14 46.8868 3.85324 3
1 -2 14 46.9000 4.47591 6
1 -2 14 45.2922 4.12275 7
-1 2 -14 45.8150 3.34271 3
1 2 14 45.3965 4.63645 6
2 2 14 49.6737 4.73430 7
-2 2 -14 49.7489 3.44948 3
-3 2 -14 105.773 5.59330 3
-5 -3 14 69.6342 4.74871 7
5 -3 -14 79.1504 5.78692 5
5 -3 -14 69.8531 4.82465 7
-5 3 14 66.4711 5.16146 6
4 -3 -14 -0.0770 2.05786 5
4 -3 -14 -0.7276 2.00615 7
-4 -3 14 1.21361 1.49687 7
-4 -3 14 -1.0171 1.08413 6
-3 -3 14 10.6259 2.06400 6
3 -3 -14 7.49532 2.09261 3
3 -3 -14 6.85305 2.37866 5
-3 -3 14 7.30298 1.98624 7
2 -3 -14 8.38837 2.94681 4
2 -3 -14 7.20706 2.29280 3
2 -3 -14 10.6191 2.44712 7
-2 -3 14 17.4499 2.90233 6
-2 -3 14 12.0923 2.43554 7
-2 3 14 10.4825 2.42255 6
-2 3 14 9.09132 2.35650 7
-1 -3 14 85.5703 6.16216 7
1 -3 -14 84.9379 6.82067 4
1 -3 -14 84.5760 5.63237 3
-1 3 14 85.3134 6.13197 6
1 3 -14 85.8148 4.32273 4
-1 3 14 84.7612 5.93203 7
0 -3 14 0.53431 1.32064 7
0 -3 -14 -0.4957 1.38143 3
0 -3 14 0.91604 1.75029 6
0 3 -14 1.20406 1.31647 4
0 3 14 1.54929 1.86501 7
-1 3 -14 45.7442 3.09078 3
-2 3 -14 6.54561 2.12663 3
4 -4 -14 3.87646 2.74589 5
3 -4 -14 14.8956 3.23966 5
-2 -4 14 7.50968 2.02381 7
-6 0 15 3.56989 2.19043 7
6 0 -15 6.44929 2.92572 4
-5 0 15 -2.3827 1.12786 7
4 0 -15 43.2080 4.06119 4
-4 0 15 49.0629 4.03225 6
-3 0 15 0.05613 1.53533 6
3 0 -15 -0.8277 1.28328 4
-2 0 15 212.045 11.4707 7
2 0 -15 233.619 9.22375 4
-2 0 15 233.639 9.93240 6
2 0 -15 235.065 8.37801 3
-1 0 15 1.56491 1.29732 7
-1 0 15 -0.1496 1.33507 6
1 0 -15 -1.0010 1.07588 4
1 0 -15 -2.2909 0.95053 3
0 0 15 14.2615 2.85541 7
0 0 -15 10.0406 2.33113 3
0 0 -15 9.73852 2.38396 4
0 0 15 9.86291 2.74997 6
-1 0 -15 -0.3461 1.24245 4
-2 0 -15 -0.4045 1.25994 3
-6 -1 15 12.6789 2.59995 7
5 -1 -15 3.86052 1.90816 4
-5 1 15 2.85285 1.97430 7
4 -1 -15 53.0958 4.61426 4
-4 -1 15 47.5774 4.14594 6
-4 1 15 48.9342 4.36176 7
-4 1 15 51.2179 4.25577 6
4 1 -15 46.8785 4.15663 4
-3 -1 15 4.01946 1.60498 6
3 -1 -15 0.25518 1.41200 4
3 -1 -15 3.73461 1.58977 7
3 -1 -15 5.04955 1.90198 3
-3 1 15 5.85355 1.81528 7
3 1 -15 0.37191 1.51732 4
-3 1 15 3.50579 1.69712 6
-2 -1 15 121.862 6.84223 6
2 -1 -15 118.973 6.18084 3
2 1 -15 119.279 5.29424 3
-2 1 15 123.608 7.07543 7
-1 -1 15 41.0814 4.09349 6
-1 -1 15 45.7635 4.26214 7
1 -1 -15 42.3110 3.49554 3
1 -1 -15 44.9611 3.93190 4
-1 1 15 46.1160 4.56427 7
1 1 -15 41.2804 3.21424 3
-1 1 15 42.5365 4.38032 6
1 1 -15 42.4425 3.39301 4
0 -1 15 18.8826 3.32709 7
0 -1 -15 14.4275 2.54844 4
0 -1 15 14.9686 2.85281 6
0 1 15 19.8537 3.22169 7
0 1 -15 19.4305 2.47213 3
0 1 15 17.7587 3.32230 6
-1 -1 -15 5.64495 1.80091 3
-1 1 -15 7.05015 1.73797 4
-1 1 -15 5.42420 1.36500 3
4 -2 -15 -1.9536 1.88604 7
-4 -2 15 -0.3758 1.30406 6
3 -2 -15 0.00162 1.56384 7
3 -2 -15 -0.3601 1.67269 3
-3 -2 15 1.53196 1.91831 7
-3 -2 15 3.33743 1.65133 6
-3 2 15 0.08662 1.57235 6
3 2 -15 2.12087 1.65885 4
-2 -2 15 4.27659 1.51155 7
-2 -2 15 -0.8310 1.55996 6
2 2 -15 1.97729 1.33235 4
-2 2 15 0.42207 1.68924 6
-1 -2 15 32.6441 3.34614 6
-1 -2 15 34.8579 3.63891 7
1 -2 -15 33.0221 3.58753 3
-1 2 15 34.6311 3.62925 6
1 2 -15 33.4410 3.14918 4
0 -2 -15 51.7912 4.17125 3
0 2 -15 50.2411 3.20121 3
0 2 -15 45.5004 3.83381 4
-1 2 -15 2.01578 1.56484 3
-2 2 -15 56.4017 3.82541 3
4 -3 -15 8.41744 2.37738 7
-4 -3 15 3.10268 1.83036 7
-4 3 15 3.39031 1.80234 6
-3 -3 15 3.13612 1.88648 7
3 -3 -15 0.72712 2.11548 7
-3 -3 15 3.63378 1.89650 6
2 -3 -15 4.94004 2.14833 5
-2 -3 15 4.18531 1.81533 7
-2 -3 15 0.15004 1.79572 6
0 3 -15 5.71016 1.62059 4
5 0 -16 -1.2626 2.07797 4
4 0 -16 2.68576 1.92575 4
-3 0 16 -3.8514 1.56071 6
3 0 -16 0.34544 1.62912 4
-2 0 16 150.902 7.79714 6
2 0 -16 151.630 7.01111 3
1 0 -16 -1.1482 1.34557 4
1 0 -16 -1.0406 1.35847 3
0 0 -16 1.41935 1.73115 3
-4 1 16 0.28410 1.92414 6
3 -1 -16 13.2609 2.48458 7
-3 -1 16 21.9428 2.97202 6
3 1 -16 16.4286 2.87594 4
-3 1 16 11.2306 2.47409 6
-2 -1 16 7.73214 2.23744 6
2 -1 -16 9.06319 2.27866 3
2 1 -16 7.57564 2.34449 4
1 -1 -16 10.1240 2.14345 3
1 1 -16 8.68997 2.20998 4
0 -1 -16 15.2347 2.38881 3
0 1 -16 19.3398 2.41173 3
-1 1 -16 -2.2960 1.17903 3
-3 -2 16 81.9032 5.62059 6
3 -2 -16 79.5092 5.65289 3
1 2 -16 1.88278 1.51859 4
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 85465
_shelx_res_file
;
TITL m18187 : space group P21/c
m18187.res
created by SHELXL-2018/3 at 19:01:15 on 14-Sep-2018
CELL 0.71073 10.7486 5.1925 6.8302 90.000 99.063 90.000
ZERR 4 0.0003 0.0002 0.0002 0.000 0.001 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H O
UNIT 12 16 12
TEMP -183
SIZE 0.26 0.22 0.18
REM FORM well-facetted block
REM COLR colourless
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+1, -z+1
HTAB O1 O2_$1
FMAP 2
PLAN 5
REM EXTI 0.010555 not significant.
WGHT 0.029900 0.126400
FVAR 1.37348
O1 3 0.416728 0.303704 0.301913 11.00000 0.01322 0.02180 =
0.02222 -0.00844 -0.00273 0.00411
H1 2 0.490310 0.320298 0.388306 11.00000 -1.50000
C1 1 0.339627 0.484478 0.340051 11.00000 0.01206 0.01378 =
0.01357 0.00033 0.00181 -0.00022
O2 3 0.363173 0.656734 0.461750 11.00000 0.01354 0.01545 =
0.01764 -0.00335 -0.00071 -0.00038
C2 1 0.208529 0.467323 0.210283 11.00000 0.01192 0.01386 =
0.01207 0.00086 0.00098 -0.00107
C3 1 0.114642 0.659488 0.257252 11.00000 0.01402 0.01627 =
0.01481 -0.00129 0.00076 0.00226
AFIX 138
H3A 2 0.149871 0.831418 0.254964 11.00000 -1.50000
H3B 2 0.094007 0.624454 0.388023 11.00000 -1.50000
H3C 2 0.038860 0.647829 0.159379 11.00000 -1.50000
AFIX 0
O3 3 0.188245 0.305077 0.082498 11.00000 0.01672 0.01811 =
0.01725 -0.00490 -0.00081 -0.00020
HKLF 4 1 0 0 1 0 -1 0 1 0 0
REM m18187 : space group P21/c
REM wR2 = 0.0815, GooF = S = 1.076, Restrained GooF = 1.076 for all data
REM R1 = 0.0313 for 1242 Fo > 4sig(Fo) and 0.0389 for all 1425 data
REM 60 parameters refined using 0 restraints
END
WGHT 0.0299 0.1264
REM Highest difference peak 0.396, deepest hole -0.214, 1-sigma level 0.045
Q1 1 0.2748 0.4792 0.2767 11.00000 0.05 0.40
Q2 1 0.1616 0.5576 0.2389 11.00000 0.05 0.36
Q3 1 0.3795 0.3831 0.3359 11.00000 0.05 0.19
Q4 1 0.3581 0.5593 0.4270 11.00000 0.05 0.17
Q5 1 0.4055 0.6588 0.5021 11.00000 0.05 0.17
;
_shelx_res_checksum 71249
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
O O1 0.41673(5) 0.30370(12) 0.30191(9) 0.01968(14) Uani d 1
H H1 0.4903(13) 0.320(3) 0.3883(19) 0.030 Uiso d 1
C C1 0.33963(6) 0.48448(14) 0.34005(11) 0.01316(14) Uani d 1
O O2 0.36317(5) 0.65673(11) 0.46175(8) 0.01589(13) Uani d 1
C C2 0.20853(6) 0.46732(14) 0.21028(10) 0.01271(14) Uani d 1
C C3 0.11464(7) 0.65949(15) 0.25725(11) 0.01520(15) Uani d 1
H H3A 0.1499(3) 0.8314(12) 0.2550(10) 0.023 Uiso calc 1
H H3B 0.0940(5) 0.6245(9) 0.3880(10) 0.023 Uiso calc 1
H H3C 0.0389(6) 0.6478(9) 0.1594(9) 0.023 Uiso calc 1
O O3 0.18824(5) 0.30508(11) 0.08250(9) 0.01774(14) Uani 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
O1 0.0132(2) 0.0218(3) 0.0222(3) 0.0041(2) -0.0027(2) -0.0084(2)
C1 0.0121(3) 0.0138(3) 0.0136(3) -0.0002(2) 0.0018(2) 0.0003(2)
O2 0.0135(2) 0.0155(3) 0.0176(3) -0.00038(19) -0.00071(19) -0.0034(2)
C2 0.0119(3) 0.0139(3) 0.0121(3) -0.0011(2) 0.0010(2) 0.0009(2)
C3 0.0140(3) 0.0163(3) 0.0148(3) 0.0023(2) 0.0008(2) -0.0013(3)
O3 0.0167(3) 0.0181(3) 0.0173(3) -0.0002(2) -0.0008(2) -0.0049(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
C1 O1 H1 108.4(8)
O2 C1 O1 126.37(7)
O2 C1 C2 120.38(6)
O1 C1 C2 113.24(6)
O3 C2 C3 124.85(7)
O3 C2 C1 119.96(7)
C3 C2 C1 115.19(6)
C2 C3 H3A 109.5
C2 C3 H3B 109.5
H3A C3 H3B 109.5
C2 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.3053(9)
O1 H1 0.913(14)
C1 O2 1.2201(9)
C1 C2 1.5446(10)
C2 O3 1.2079(9)
C2 C3 1.4896(10)
C3 H3A 0.971(6)
C3 H3B 0.971(6)
C3 H3C 0.971(6)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O2 3_666 0.913(14) 1.742(14) 2.6536(8) 175.5(12) yes
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
O2 C1 C2 O3 175.81(7)
O1 C1 C2 O3 -3.34(10)
O2 C1 C2 C3 -4.59(10)
O1 C1 C2 C3 176.26(6)
_cod_database_fobs_code 2242954