#------------------------------------------------------------------------------
#$Date: 2026-10-30 23:30:59 +0100 (Fri, 30 Oct 2026) $
#$Revision: 307007 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/74/1577495.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_1577495
loop_
_publ_author_name
'Lawley, Hannah K.'
'Archer, Noah K.'
'Baxter, Bailey N.'
'Borchert, Madeline R.'
'Lewis, Grace E.'
'Marmande, Mary Helene'
'Mayeaux, Kathryn N.'
'Orr, Lucy A.'
'Zeller, Matthias'
'Forbes, David C.'
_publ_section_title
;
3-[(2-Chloroethoxy)carbonyl]-7-oxabicyclo[2.2.1]heptane-2-carboxylic acid
;
_journal_coeditor_code BT4210
_journal_issue 10
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314626011211
_journal_volume 11
_journal_year 2026
_chemical_formula_iupac 'C10 H13 Cl O5'
_chemical_formula_moiety 'C10 H13 Cl O5'
_chemical_formula_sum 'C10 H13 Cl O5'
_chemical_formula_weight 248.65
_chemical_name_systematic
;
3-[(2-Chloroethoxy)carbonyl]-7-oxabicyclo[2.2.1]heptane-2-carboxylic acid
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 82.828(2)
_cell_angle_beta 86.801(2)
_cell_angle_gamma 79.872(2)
_cell_formula_units_Z 2
_cell_length_a 4.7953(3)
_cell_length_b 9.8084(6)
_cell_length_c 11.7357(7)
_cell_measurement_reflns_used 9819
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 33.2890
_cell_measurement_theta_min 2.5895
_cell_volume 538.80(6)
_computing_cell_refinement
;
SAINT V8.41 (Bruker, 2025)
;
_computing_data_collection
;
APEX6 v2024.9-1 (Bruker, 2025)
;
_computing_data_reduction
;
SAINT V8.41 (Bruker, 2025)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
Publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (Sheldrick, 2015b),
ShelXle Rev1737 (H\"ubschle et al., 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device 'three circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Quest'
_diffrn_measurement_method 'omega and phi scans'
_diffrn_radiation_monochromator 'Triumph curved graphite crystal'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0404
_diffrn_reflns_av_unetI/netI 0.0260
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 29602
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.299
_diffrn_reflns_theta_min 2.124
_diffrn_source 'fine focus sealed tube X-ray source'
_diffrn_source_current 30
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 0.358
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.6326
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.533
_exptl_crystal_description block
_exptl_crystal_F_000 260
_exptl_crystal_size_max 0.450
_exptl_crystal_size_mid 0.430
_exptl_crystal_size_min 0.280
_refine_diff_density_max 0.443
_refine_diff_density_min -0.493
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.040
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 148
_refine_ls_number_reflns 4150
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.040
_refine_ls_R_factor_all 0.0382
_refine_ls_R_factor_gt 0.0353
_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^)+(0.0484P)^2^+0.1762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0972
_refine_ls_wR_factor_ref 0.0997
_reflns_number_gt 3783
_reflns_number_total 4150
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file bt4210.cif
_cod_data_source_block I
_cod_database_code 1577495
_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 0.856
_shelx_estimated_absorpt_t_max 0.906
_shelx_hkl_file
;
-1 0 0 134.343 7.32220 10
-1 0 0 152.149 7.48403 1
-1 0 0 151.289 7.43362 2
-1 0 0 145.133 7.33431 9
1 0 0 144.950 7.32067 7
1 0 0 154.703 7.35152 8
1 0 0 149.387 7.34314 6
1 0 0 142.044 7.33197 9
1 0 0 139.877 7.43662 1
1 0 0 141.724 7.39980 2
-2 0 0 658.757 32.2036 1
-2 0 0 635.114 32.0840 2
2 0 0 635.029 32.0476 1
2 0 0 617.117 31.9699 2
-3 0 0 994.127 50.6010 2
-3 0 0 1041.24 50.7907 1
3 0 0 979.432 50.3404 1
3 0 0 1004.01 50.2916 2
-4 0 0 26.1840 2.04939 2
-4 0 0 29.4489 1.74428 5
-4 0 0 29.3909 2.27812 1
-4 0 0 23.9829 1.67246 5
-4 0 0 28.2767 1.78244 9
-4 0 0 28.4832 1.76369 10
-4 0 0 27.7078 1.73936 10
4 0 0 27.7195 1.87336 8
4 0 0 26.9216 1.76253 9
4 0 0 25.7966 1.81014 6
-5 0 0 187.701 9.29732 1
-5 0 0 172.473 9.03954 2
-5 0 0 152.168 8.70900 5
-5 0 0 169.355 8.79783 10
-5 0 0 179.224 8.78028 5
5 0 0 168.413 8.80121 9
5 0 0 154.977 8.83426 6
5 0 0 159.416 8.88238 8
-6 0 0 1.40475 0.52206 5
-6 0 0 1.45690 0.54166 5
-6 0 0 0.14098 0.55949 10
6 0 0 0.63525 0.81402 6
6 0 0 1.11582 0.93243 8
-7 0 0 1.78364 0.80197 7
-7 0 0 3.67774 0.83430 10
7 0 0 3.51788 1.26358 8
7 0 0 4.32462 1.15710 6
7 -1 0 8.02341 1.32609 6
7 -1 0 5.64632 1.42574 8
-7 1 0 4.13505 0.85033 10
-7 1 0 4.44808 0.98499 7
6 -1 0 -0.4254 0.64125 9
6 -1 0 -0.0260 0.85340 6
6 -1 0 1.10000 0.98849 8
-6 1 0 0.37109 0.36676 5
-6 1 0 0.71704 1.18202 2
-6 1 0 -0.0762 0.37070 5
-6 1 0 0.26312 0.60483 10
-6 1 0 -0.2128 0.63066 7
5 -1 0 74.7941 4.28960 8
5 -1 0 77.2593 4.17081 9
5 -1 0 70.2712 4.21932 6
-5 1 0 76.6639 4.77501 2
-5 1 0 71.7528 4.10475 10
-5 1 0 66.4335 3.93972 5
-5 1 0 79.0657 5.10485 1
4 -1 0 3.63527 0.78400 1
4 -1 0 2.05133 0.65395 2
4 -1 0 3.96396 0.74347 6
4 -1 0 2.20988 0.58263 9
4 -1 0 2.57878 0.71133 8
-4 1 0 2.78259 0.46956 5
-4 1 0 2.36230 0.92861 2
-4 1 0 2.27689 1.08330 1
-4 1 0 1.66035 0.39231 5
-4 1 0 2.37941 0.52895 10
-4 1 0 2.74490 0.59342 9
3 -1 0 70.1997 3.80550 6
3 -1 0 71.4331 3.82622 8
3 -1 0 71.4097 3.77529 9
3 -1 0 70.0839 4.06100 2
3 -1 0 66.1576 4.19591 1
-3 1 0 64.7374 3.65983 5
-3 1 0 72.8309 3.68863 5
-3 1 0 68.9354 3.77373 9
-3 1 0 73.6610 4.51907 1
-3 1 0 71.2167 3.74567 10
-3 1 0 71.5502 4.28523 2
2 -1 0 50.9775 2.84105 9
2 -1 0 53.5340 2.87193 6
2 -1 0 55.4432 2.88529 8
2 -1 0 51.8168 2.80480 10
2 -1 0 52.5857 3.28973 1
2 -1 0 54.9276 3.18019 2
-2 1 0 54.8120 2.77757 5
-2 1 0 54.9080 2.82716 10
-2 1 0 51.1905 2.76214 5
-2 1 0 54.4017 3.40501 1
-2 1 0 53.5397 3.25782 2
-2 1 0 52.9576 2.85566 9
1 -1 0 11.0399 0.96301 2
1 -1 0 11.7580 0.73858 6
1 -1 0 13.8852 0.75849 8
1 -1 0 11.0940 0.69737 10
1 -1 0 12.6178 0.74447 9
1 -1 0 11.9151 1.07674 1
-1 1 0 11.5984 0.64403 5
-1 1 0 12.0746 1.11059 1
-1 1 0 11.5535 0.73289 9
-1 1 0 12.7865 0.71178 10
-1 1 0 11.7918 1.01799 2
0 -1 0 0.13503 0.06471 9
0 -1 0 0.03661 0.19916 2
0 1 0 -0.0041 0.05774 10
-1 -1 0 2706.97 135.637 3
-1 -1 0 2705.52 135.637 4
-2 -1 0 239.335 11.8634 10
-2 -1 0 230.394 11.8944 5
-2 -1 0 236.540 11.8510 9
-2 -1 0 248.843 11.8616 1
-2 -1 0 241.033 11.8204 2
2 1 0 220.386 11.8423 6
2 1 0 234.367 11.8635 8
2 1 0 232.523 11.8476 9
2 1 0 228.766 11.8256 7
-3 -1 0 3.05653 0.51601 1
-3 -1 0 3.44883 0.52046 5
-3 -1 0 2.40198 0.42719 2
-3 -1 0 3.24140 0.45299 9
3 1 0 3.29138 0.45487 7
3 1 0 4.57334 0.59674 9
3 1 0 3.98156 0.53391 6
-4 -1 0 21.4868 1.40120 2
-4 -1 0 21.6208 1.46565 9
-4 -1 0 23.6961 1.52115 1
-4 -1 0 21.4298 1.48972 5
-4 -1 0 18.2188 1.42723 10
-4 -1 0 21.7107 1.46266 10
-4 -1 0 22.5012 1.50099 5
4 1 0 19.7814 1.40789 7
4 1 0 19.1698 1.50421 8
4 1 0 20.1454 1.49320 6
-5 -1 0 167.465 8.42097 5
-5 -1 0 144.617 8.35031 5
-5 -1 0 165.997 8.39018 10
5 1 0 162.593 8.42377 6
5 1 0 156.192 8.44459 8
-6 -1 0 4.00697 0.73706 5
-6 -1 0 3.97424 0.79495 10
6 1 0 2.76350 0.98661 8
6 1 0 4.03595 0.97972 6
-7 -1 0 3.57208 0.83643 10
-7 -1 0 2.35927 0.65488 5
7 1 0 0.97979 0.91919 6
7 1 0 1.93696 1.03743 8
7 -2 0 0.88473 1.01529 6
-7 2 0 0.16321 0.62337 10
-7 2 0 0.57769 0.94190 7
6 -2 0 18.3880 1.94914 6
6 -2 0 19.3699 1.70356 9
6 -2 0 17.1969 1.96487 8
-6 2 0 12.1236 2.23407 2
-6 2 0 15.3305 1.49537 10
-6 2 0 17.9420 1.60843 7
5 -2 0 66.0602 3.69853 2
5 -2 0 59.6449 3.60319 9
5 -2 0 59.5622 3.79100 1
5 -2 0 55.4854 3.68054 6
5 -2 0 63.4248 3.80210 8
-5 2 0 66.8684 3.58867 7
-5 2 0 67.3124 5.02385 1
-5 2 0 60.6562 3.55558 10
-5 2 0 55.5449 4.40561 2
4 -2 0 1.77396 0.67436 6
4 -2 0 1.95475 0.73883 8
4 -2 0 1.75260 0.86229 2
4 -2 0 2.01220 0.65645 9
4 -2 0 1.42840 0.97660 1
-4 2 0 0.77019 0.97278 2
-4 2 0 1.66516 0.60261 9
-4 2 0 2.23526 0.37476 5
-4 2 0 2.66115 0.37849 5
-4 2 0 3.56878 1.34756 1
-4 2 0 1.95142 0.54527 10
3 -2 0 381.857 19.9608 6
3 -2 0 377.144 20.6873 1
3 -2 0 392.588 20.4717 2
3 -2 0 386.917 19.9309 9
3 -2 0 394.025 19.9768 8
-3 2 0 391.204 20.6699 2
-3 2 0 400.381 19.9540 9
-3 2 0 393.333 19.7765 5
-3 2 0 412.168 19.9126 10
-3 2 0 425.336 21.0344 1
-3 2 0 382.314 19.7695 5
2 -2 0 399.863 20.7730 2
2 -2 0 377.643 20.1826 10
2 -2 0 406.894 20.2427 9
2 -2 0 407.578 20.2562 8
2 -2 0 406.589 20.2573 6
2 -2 0 399.384 20.9778 1
-2 2 0 410.310 20.2457 9
-2 2 0 430.517 21.1469 1
-2 2 0 374.222 20.1736 7
-2 2 0 393.103 20.2031 10
-2 2 0 413.596 20.8815 2
-2 2 0 404.200 20.0995 5
1 -2 0 118.482 6.64756 1
1 -2 0 118.607 6.01893 6
1 -2 0 117.892 6.02239 9
1 -2 0 111.513 5.98349 10
1 -2 0 115.789 5.91987 5
1 -2 0 118.782 6.01171 8
-1 2 0 124.138 6.71906 1
-1 2 0 115.389 5.99239 10
-1 2 0 115.960 6.01760 9
-1 2 0 127.007 6.55988 2
-1 2 0 129.339 5.92439 5
-1 2 0 105.396 5.96932 7
0 -2 0 1784.45 95.0331 4
0 -2 0 1825.92 94.9957 3
0 2 0 1892.51 95.1787 4
0 2 0 1810.12 94.9756 3
-1 -2 0 2.27129 0.28913 9
-1 -2 0 1.74728 0.27309 10
-1 -2 0 1.51418 0.30144 5
-1 -2 0 1.85659 0.38901 2
-1 -2 0 1.49742 0.41628 1
1 2 0 2.27116 0.22939 8
1 2 0 1.58896 0.35725 2
1 2 0 1.54145 0.40541 1
1 2 0 2.06164 0.34343 5
1 2 0 1.76298 0.28387 10
1 2 0 2.59771 0.29213 7
-2 -2 0 415.719 20.5375 10
-2 -2 0 423.190 20.5128 2
-2 -2 0 427.393 20.5710 1
-2 -2 0 414.737 20.5978 5
-2 -2 0 405.857 20.5068 9
2 2 0 398.500 20.4972 8
2 2 0 394.973 20.4854 6
2 2 0 385.440 20.4794 7
-3 -2 0 296.620 14.5482 9
-3 -2 0 292.154 14.6382 5
-3 -2 0 292.800 14.5725 10
3 2 0 274.194 14.5228 6
3 2 0 281.657 14.5058 7
3 2 0 285.276 14.5489 8
-4 -2 0 50.6430 3.02831 10
-4 -2 0 54.9226 3.03317 9
-4 -2 0 54.6817 3.05774 10
-4 -2 0 58.0928 3.14566 5
4 2 0 52.3958 2.98128 7
4 2 0 53.4315 3.05999 8
4 2 0 52.7725 3.02890 6
-5 -2 0 1.15333 0.63028 10
-5 -2 0 0.08931 0.55500 5
-5 -2 0 0.66678 0.60435 5
5 2 0 0.98212 0.70237 8
5 2 0 0.34437 0.62902 6
5 2 0 0.03336 0.52890 7
-6 -2 0 122.604 6.92925 10
-6 -2 0 118.244 6.95624 5
6 2 0 145.779 7.04452 6
-7 -2 0 5.26691 0.97363 5
-7 -2 0 7.38917 1.09384 10
7 2 0 5.55528 1.23546 8
7 2 0 6.86647 1.22518 6
6 -3 0 2.99830 1.04739 6
6 -3 0 4.12271 1.16942 8
6 -3 0 4.64249 1.01190 9
-6 3 0 4.12148 0.98082 7
-6 3 0 3.46327 0.79949 10
-6 3 0 4.77331 2.14212 2
5 -3 0 36.4400 2.61361 6
5 -3 0 37.0989 2.50286 9
5 -3 0 39.0101 3.13894 2
5 -3 0 38.7066 2.71323 8
5 -3 0 35.0070 3.32863 1
-5 3 0 40.5894 2.48327 7
-5 3 0 37.8165 4.22855 1
-5 3 0 28.4217 3.46479 2
4 -3 0 308.985 15.7478 8
4 -3 0 297.336 16.7162 1
4 -3 0 294.958 15.6630 9
4 -3 0 301.490 16.3490 2
4 -3 0 297.215 15.7205 6
-4 3 0 314.570 15.6134 7
-4 3 0 314.939 16.8091 2
-4 3 0 323.539 17.2564 1
-4 3 0 303.927 15.6214 10
3 -3 0 4.43461 0.56939 10
3 -3 0 5.13931 0.68439 9
3 -3 0 4.50659 0.76326 8
3 -3 0 6.39208 0.86299 6
3 -3 0 3.91218 1.08536 2
3 -3 0 6.67269 1.43587 1
-3 3 0 4.09573 1.42044 1
-3 3 0 5.62376 0.72447 7
-3 3 0 5.93000 0.72405 9
-3 3 0 5.97726 0.75027 10
-3 3 0 4.28241 1.25559 2
2 -3 0 44.7047 2.58642 6
2 -3 0 44.3640 2.50384 10
2 -3 0 47.7768 3.54528 1
2 -3 0 44.6335 2.58617 9
2 -3 0 47.4934 2.59577 8
-2 3 0 44.6330 2.51009 7
-2 3 0 50.7661 3.45901 2
-2 3 0 46.7938 2.58906 9
-2 3 0 46.1077 2.53437 10
-2 3 0 52.0113 3.72145 1
1 -3 0 203.742 10.4966 2
1 -3 0 190.832 9.80325 9
1 -3 0 185.117 9.76270 10
1 -3 0 184.113 9.69365 5
1 -3 0 202.626 9.80406 6
1 -3 0 193.035 10.6839 1
1 -3 0 203.145 9.78220 8
-1 3 0 196.261 10.7192 1
-1 3 0 174.015 9.74101 7
-1 3 0 191.621 9.70410 5
-1 3 0 201.774 10.5407 2
-1 3 0 195.911 9.80621 9
-1 3 0 191.714 9.77477 10
0 -3 0 2.39587 0.65724 2
0 -3 0 0.56983 0.24237 9
0 -3 0 1.47949 0.62446 1
0 -3 0 0.65739 0.19947 6
0 -3 0 1.05718 0.22277 5
0 3 0 0.63047 0.22772 10
0 3 0 2.08910 0.67605 1
0 3 0 1.50214 0.24387 7
0 3 0 0.70988 0.23587 5
0 3 0 0.66990 0.49128 2
-1 -3 0 7187.47 350.788 3
-1 -3 0 7022.44 350.789 4
1 3 0 6744.38 350.214 3
1 3 0 6802.87 350.243 4
-2 -3 0 1862.15 90.9381 2
-2 -3 0 1884.67 91.0854 1
2 3 0 1778.65 90.8272 1
2 3 0 1737.08 90.7723 2
-3 -3 0 83.2566 4.31393 9
-3 -3 0 84.5999 4.36996 10
-3 -3 0 83.9054 4.46037 5
3 3 0 77.3548 4.28769 8
3 3 0 78.6676 4.27095 6
3 3 0 82.3594 4.28538 7
-4 -3 0 2.36081 0.50846 9
-4 -3 0 2.53334 0.54618 10
-4 -3 0 2.55485 0.60438 5
4 3 0 1.89760 0.49392 7
4 3 0 1.92482 0.53663 8
4 3 0 2.64515 0.52703 6
-5 -3 0 145.880 7.55680 5
-5 -3 0 138.396 7.40280 10
5 3 0 132.796 7.36624 8
5 3 0 137.852 7.34448 6
5 3 0 141.231 7.31539 7
-6 -3 0 2.42425 0.77651 5
-6 -3 0 0.73885 0.62608 10
6 3 0 1.75400 0.77319 6
6 3 0 2.15582 0.85273 8
6 3 0 1.73900 0.74770 7
-7 -3 0 34.8097 2.51437 10
-7 -3 0 34.0487 2.43515 9
7 3 0 35.9374 2.60168 6
7 3 0 36.1617 2.66085 8
6 -4 0 78.0295 4.62235 6
6 -4 0 78.4512 4.48412 9
6 -4 0 70.7622 6.20295 2
-6 4 0 80.5605 4.45422 7
-6 4 0 66.3603 4.30955 10
-6 4 0 72.5533 6.39733 2
5 -4 0 96.9539 6.90337 1
5 -4 0 103.867 5.73977 6
5 -4 0 97.8412 6.46488 2
5 -4 0 103.320 5.72943 8
5 -4 0 103.222 5.61804 9
-5 4 0 86.6865 5.44880 10
-5 4 0 104.366 5.54979 7
-5 4 0 108.349 7.80077 1
4 -4 0 2.68733 0.74704 9
4 -4 0 3.30322 1.60156 1
4 -4 0 1.07158 1.27637 2
4 -4 0 2.01677 0.83186 6
4 -4 0 2.77685 0.90674 8
4 -4 0 1.33781 0.51191 10
-4 4 0 3.41720 1.83754 1
-4 4 0 1.09560 1.40129 2
-4 4 0 1.41228 0.69211 7
-4 4 0 2.15993 0.68252 10
3 -4 0 60.0123 3.34842 9
3 -4 0 56.1546 3.20298 10
3 -4 0 58.5295 4.61518 1
3 -4 0 51.1803 4.12739 2
3 -4 0 59.2052 3.36637 6
3 -4 0 64.3755 3.40216 8
-3 4 0 51.7633 3.24084 10
-3 4 0 62.3223 3.26673 7
-3 4 0 59.8363 3.33862 9
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0 0 16 4.41960 4.37034 2
0 0 16 0.22339 0.49705 10
0 0 16 -0.3562 0.92128 5
0 0 16 2.31953 3.73889 2
-1 0 -16 159.403 8.53573 8
-1 0 -16 157.973 8.09772 9
-1 0 -16 154.245 13.4008 1
-1 0 -16 126.218 12.4539 1
-1 0 -16 153.384 8.22248 6
1 0 16 167.377 13.5196 2
1 0 16 161.011 8.66260 5
1 0 16 144.560 11.5834 2
1 0 16 149.283 7.82689 10
-2 0 -16 1.28458 0.86287 6
-2 0 -16 -0.8130 0.94912 8
-2 0 -16 0.31540 0.64837 9
2 0 16 0.08441 0.86557 5
-3 0 -16 2.11175 0.91479 6
-3 0 -16 0.56555 1.07369 8
3 0 16 0.47190 0.80543 5
3 -1 -16 -0.5656 1.17650 8
3 -1 -16 0.76833 0.62389 6
-3 1 16 0.92783 1.16388 5
-3 1 16 0.45341 0.79857 10
2 -1 -16 -0.0040 1.04792 8
2 -1 -16 -0.0119 0.59766 6
-2 1 16 0.07048 1.01950 5
-2 1 16 -0.2193 0.66813 10
1 -1 -16 72.4193 4.54419 8
1 -1 -16 68.4596 4.09011 6
1 -1 -16 67.4743 10.0195 1
-1 1 16 69.5232 4.12596 10
-1 1 16 82.3668 9.26628 2
-1 1 16 73.1777 4.68622 5
0 -1 -16 1.28623 4.84840 1
0 -1 -16 0.44351 0.71494 6
0 -1 -16 0.00618 0.42733 9
0 -1 -16 0.47661 0.99392 8
0 -1 -16 2.14358 4.62831 1
0 1 16 -1.8549 3.48167 2
0 1 16 -0.0428 0.48061 10
0 1 16 -2.2201 4.15454 2
0 1 16 0.01477 0.95363 5
-1 -1 -16 0.28163 0.77652 6
-1 -1 -16 -3.5790 4.83953 1
-1 -1 -16 0.21990 1.02594 8
-1 -1 -16 4.07409 4.87234 1
-1 -1 -16 0.74051 0.58840 9
1 1 16 1.98405 3.86291 2
1 1 16 0.33219 0.36496 10
1 1 16 0.49358 1.00345 5
1 1 16 -0.8076 3.81474 2
-2 -1 -16 11.3973 1.58131 8
-2 -1 -16 3.42788 5.76016 1
-2 -1 -16 10.8169 1.35853 9
-2 -1 -16 6.88218 1.17487 6
2 1 16 12.2121 5.46137 2
2 1 16 8.19557 1.39834 5
-3 -1 -16 2.12739 1.09905 8
-3 -1 -16 2.83107 0.87292 9
-3 -1 -16 2.19809 1.07004 6
3 1 16 3.47853 1.07192 5
-3 2 16 15.8913 2.19194 5
-3 2 16 15.0700 1.91748 10
2 -2 -16 4.51378 1.32980 8
2 -2 -16 3.98649 0.90751 6
-2 2 16 3.51921 1.23729 5
-2 2 16 2.90038 0.89939 10
1 -2 -16 12.0857 7.37340 1
1 -2 -16 6.93303 4.94672 1
1 -2 -16 6.91660 1.06841 6
1 -2 -16 8.65041 1.47565 8
-1 2 16 4.54205 4.82610 2
-1 2 16 9.71049 1.25731 10
-1 2 16 7.44082 4.30674 2
-1 2 16 8.99308 1.50561 5
0 -2 -16 1.09189 4.67494 1
0 -2 -16 3.97470 0.91581 6
0 -2 -16 5.43971 1.20061 8
0 -2 -16 4.81119 0.67089 9
0 -2 -16 6.95914 5.13766 1
0 2 16 6.67046 0.94273 10
0 2 16 4.49032 1.23581 5
0 2 16 -1.7784 3.84581 2
0 2 16 4.80189 0.58787 7
-1 -2 -16 0.77792 4.32128 1
-1 -2 -16 -1.2680 4.15423 1
-1 -2 -16 -0.7163 0.83680 6
-1 -2 -16 2.17001 0.65566 9
-1 -2 -16 1.96899 1.06843 8
1 2 16 -1.6361 4.72913 2
1 2 16 1.89776 3.30560 2
-2 -2 -16 104.784 5.76398 9
-2 -2 -16 109.571 5.93654 6
-2 -2 -16 101.733 5.95265 8
2 2 16 88.0533 9.97718 2
2 2 16 101.358 6.14493 5
-3 -2 -16 4.06049 1.23847 8
-3 -2 -16 3.83255 1.12250 6
-3 -2 -16 4.88548 1.09397 9
3 2 16 5.39435 1.23768 5
2 -3 -16 1.02372 1.09831 8
2 -3 -16 0.74196 0.79201 6
-2 3 16 1.20614 1.13907 5
-2 3 16 3.08365 0.90886 10
-2 3 16 1.11140 0.66278 7
1 -3 -16 18.8761 5.69661 1
1 -3 -16 13.0856 1.83383 8
1 -3 -16 22.7556 8.60658 1
1 -3 -16 13.4262 1.56444 6
1 -3 -16 12.7832 0.89259 9
-1 3 16 11.1201 5.12917 2
-1 3 16 17.0438 5.41427 2
-1 3 16 12.6540 1.98462 5
-1 3 16 12.7766 1.12368 7
-1 3 16 13.1660 1.44465 10
0 -3 -16 11.0273 4.86352 1
0 -3 -16 15.5987 5.10877 1
0 -3 -16 12.8066 1.73454 8
0 -3 -16 13.3285 1.63042 6
0 -3 -16 15.7821 1.21788 9
0 3 16 14.8480 4.88098 2
0 3 16 17.0576 2.02724 5
0 3 16 13.6784 0.97810 7
0 3 16 12.8390 1.30692 10
0 3 16 12.4266 4.76480 2
-1 -3 -16 24.8187 2.20994 8
-1 -3 -16 22.9026 1.80208 9
-1 -3 -16 19.8861 5.88205 1
-1 -3 -16 30.9273 6.71138 1
-1 -3 -16 23.3185 2.13637 6
1 3 16 24.7413 1.64673 10
1 3 16 24.6645 2.42102 5
1 3 16 27.8545 4.82978 2
-2 -3 -16 58.6428 3.73027 6
-2 -3 -16 55.0487 3.68634 8
-2 -3 -16 44.3841 9.17002 1
-2 -3 -16 58.2323 3.54308 9
2 3 16 50.6797 8.38877 2
2 3 16 60.9838 3.99522 5
-3 -3 -16 13.5023 1.83877 8
-3 -3 -16 17.0058 1.80753 9
-3 -3 -16 17.6564 1.99975 6
3 3 16 16.5937 2.04643 5
2 -4 -16 1.24951 0.88712 6
2 -4 -16 2.40744 1.11776 8
-2 4 16 0.42791 0.79160 10
-2 4 16 1.72989 1.11874 5
-2 4 16 1.14526 0.66161 7
1 -4 -16 48.6370 7.99895 1
1 -4 -16 44.9165 2.57955 9
1 -4 -16 48.0311 3.12542 6
1 -4 -16 51.5557 3.32337 8
-1 4 16 44.7812 2.70202 7
-1 4 16 47.4725 7.69432 2
-1 4 16 44.6180 2.98613 10
-1 4 16 47.0075 3.59999 5
-1 4 16 41.7762 6.81909 2
0 -4 -16 0.53074 0.51870 9
0 -4 -16 1.25377 0.92892 6
0 -4 -16 2.28226 5.02572 1
0 -4 -16 -5.5395 4.50162 1
0 -4 -16 0.13996 0.83833 8
0 4 16 0.89079 0.35429 7
0 4 16 -2.6636 3.80155 2
0 4 16 0.96603 0.59987 10
0 4 16 2.02844 4.05062 2
0 4 16 1.11748 1.07168 5
-1 -4 -16 3.36052 5.14124 1
-1 -4 -16 1.61441 0.71745 9
-1 -4 -16 5.47666 4.52629 1
-1 -4 -16 1.45463 0.81885 8
-1 -4 -16 1.59767 1.02028 6
1 4 16 1.72570 0.55275 10
1 4 16 0.20106 3.96021 2
1 4 16 2.53212 1.09388 5
-2 -4 -16 57.1415 3.73528 8
-2 -4 -16 62.5392 3.92034 6
-2 -4 -16 65.3931 3.71863 9
2 4 16 59.2149 4.14349 5
2 4 16 56.9573 3.20584 10
-3 -4 -16 0.56031 0.77638 8
-3 -4 -16 1.09738 0.90958 9
-3 -4 -16 1.20441 1.12259 6
3 4 16 0.70689 0.99990 5
2 -5 -16 2.23250 1.00633 6
2 -5 -16 2.96024 1.15257 8
-2 5 16 3.66960 0.84201 7
-2 5 16 3.69175 1.03994 10
-2 5 16 2.22168 1.17529 5
1 -5 -16 9.96672 0.95510 9
1 -5 -16 6.53241 1.21856 6
1 -5 -16 4.56571 6.46694 1
1 -5 -16 8.16794 1.40929 8
-1 5 16 12.4091 5.97386 2
-1 5 16 0.90990 5.57439 2
-1 5 16 9.66145 1.23333 10
-1 5 16 8.39845 1.56575 5
-1 5 16 9.29362 1.04915 7
0 -5 -16 7.57796 1.27653 6
0 -5 -16 5.02448 1.10554 8
0 -5 -16 3.14239 4.87791 1
0 -5 -16 6.02947 5.83804 1
0 -5 -16 6.12742 0.85265 9
0 5 16 7.64441 4.60944 2
0 5 16 3.34685 4.88036 2
0 5 16 6.70597 0.73123 7
0 5 16 6.44655 1.44490 5
0 5 16 7.03167 0.95985 10
-1 -5 -16 17.1649 1.56271 9
-1 -5 -16 16.1489 1.87895 6
-1 -5 -16 18.4808 6.19252 1
-1 -5 -16 10.3726 5.73387 1
-1 -5 -16 12.5239 1.56554 8
1 5 16 17.3585 2.10552 5
1 5 16 17.9193 5.06399 2
1 5 16 15.7671 1.36805 10
-2 -5 -16 25.2258 2.37845 6
-2 -5 -16 26.6366 2.11234 9
2 5 16 24.9112 1.63299 10
2 5 16 24.1427 2.55585 5
-3 -5 -16 59.4987 3.99277 6
-3 -5 -16 59.3253 3.74974 9
3 5 16 54.8734 4.05296 5
1 -6 -16 4.66780 0.72188 9
1 -6 -16 2.67532 1.05157 6
1 -6 -16 4.03047 1.11075 8
-1 6 16 5.36134 0.77055 7
-1 6 16 5.67320 1.36000 5
-1 6 16 3.31698 6.84295 2
-1 6 16 4.37447 0.93615 10
0 -6 -16 1.84149 0.65842 9
0 -6 -16 1.77368 5.53598 1
0 -6 -16 2.15475 1.01784 6
0 -6 -16 1.33941 0.78783 8
0 -6 -16 0.50566 6.05407 1
0 6 16 -1.0460 5.13593 2
0 6 16 1.02872 1.07029 5
0 6 16 1.42019 0.41156 7
0 6 16 1.14340 0.70136 10
-1 -6 -16 29.9035 10.8112 1
-1 -6 -16 41.6612 3.03308 6
-1 -6 -16 41.0250 2.70935 9
1 6 16 39.7265 2.58679 10
1 6 16 41.3430 3.28565 5
-2 -6 -16 2.44966 0.81353 8
-2 -6 -16 3.23262 1.18244 6
-2 -6 -16 3.47473 0.93938 9
2 6 16 2.55512 0.60309 10
2 6 16 3.71776 1.21808 5
-3 -6 -16 62.8416 3.89816 9
-3 -6 -16 54.0200 3.62520 8
-3 -6 -16 66.3043 4.19935 6
3 6 16 60.3263 4.23122 5
1 -7 -16 16.8535 1.48991 9
1 -7 -16 16.4786 2.02986 6
1 -7 -16 16.1548 1.78470 8
-1 7 16 17.6805 2.24668 5
-1 7 16 17.6243 1.46858 7
-1 7 16 19.3001 1.87951 10
0 -7 -16 45.0988 3.26727 6
0 -7 -16 42.7801 2.79497 9
0 7 16 47.4529 3.55813 5
0 7 16 45.0920 2.95786 10
0 7 16 41.3657 2.48964 7
-1 -7 -16 17.9919 1.75596 9
-1 -7 -16 19.3432 2.15127 6
1 7 16 17.4621 1.65177 10
1 7 16 19.8067 2.35451 5
-2 -7 -16 17.6055 2.11899 6
-2 -7 -16 15.2478 1.78313 9
-2 -7 -16 12.7604 1.42286 8
2 7 16 16.9457 1.39989 10
2 7 16 14.7297 2.20950 5
-3 -7 -16 87.4531 5.12382 9
3 7 16 81.1821 5.42048 5
0 -8 -16 0.71865 1.02798 6
0 -8 -16 0.31657 0.65013 9
0 -8 -16 -0.1270 0.65559 8
0 8 16 0.22288 1.04069 5
0 8 16 0.05210 0.80495 10
0 8 16 0.28443 0.43723 7
-1 -8 -16 20.0750 2.26183 6
-1 -8 -16 17.2884 1.79061 9
1 8 16 19.2687 2.28553 5
1 8 16 16.9911 1.70172 10
-2 -8 -16 5.23049 0.83817 8
-2 -8 -16 6.38374 1.09989 9
-2 -8 -16 5.94014 1.40920 6
2 8 16 7.92916 1.57555 5
0 3 -17 36.3526 2.13246 6
0 3 -17 28.9366 2.01090 7
0 3 -17 35.6879 3.04299 8
0 -3 17 37.1067 2.91891 5
1 2 -17 17.4570 2.37529 8
-1 -2 17 19.0024 1.59816 10
-1 -2 17 19.9125 2.37790 5
0 2 -17 1.16991 0.59819 6
0 2 -17 0.31799 1.24044 8
0 -2 17 0.60795 0.46482 10
0 -2 17 0.07950 0.88020 5
-1 2 -17 16.9343 1.55975 6
-1 2 -17 17.4118 1.46028 9
-1 2 -17 19.2205 2.28101 8
1 -2 17 15.1208 1.98344 5
1 1 -17 14.9812 2.15484 8
1 1 -17 14.7520 1.28141 6
-1 -1 17 13.6903 1.40903 10
-1 -1 17 15.3117 2.09205 5
0 1 -17 65.5130 11.5796 1
0 1 -17 56.3116 3.38713 6
0 1 -17 63.5163 4.05911 8
0 -1 17 58.4058 9.61140 2
0 -1 17 53.0036 3.21172 10
0 -1 17 55.3109 3.96907 5
0 -1 17 65.2322 10.4296 2
-1 1 -17 2.70603 0.84508 6
-1 1 -17 1.75672 0.60681 9
-1 1 -17 2.04190 1.25980 8
1 -1 17 2.49130 1.09830 5
-2 1 -17 7.96473 1.56230 8
-2 1 -17 10.2249 1.36050 9
-2 1 -17 11.9672 1.53982 6
2 -1 17 11.0454 1.66389 5
2 0 -17 0.56121 0.54031 6
2 0 -17 -0.7504 1.09917 8
-2 0 17 -0.2896 0.69294 10
-2 0 17 0.70876 1.16736 5
1 0 -17 11.7610 1.69924 8
1 0 -17 10.7368 1.24428 6
-1 0 17 12.3607 1.88979 5
-1 0 17 10.8006 1.30775 10
0 0 -17 29.3593 2.59388 8
0 0 -17 22.4589 1.52400 9
0 0 -17 25.5848 1.91113 6
0 0 -17 15.6408 8.21511 1
0 0 -17 18.7341 7.78921 1
0 0 17 22.3184 1.65668 10
0 0 17 22.7498 2.46271 5
0 0 17 22.8797 6.02309 2
0 0 17 26.8369 6.74361 2
-1 0 -17 -3.1406 11.0550 1
-1 0 -17 7.84724 1.15245 6
-1 0 -17 8.84355 1.59924 8
1 0 17 4.96371 1.24896 5
-2 0 -17 7.22284 1.41828 8
-2 0 -17 6.52663 1.13393 6
-2 0 -17 9.62877 1.19614 9
2 0 17 8.56608 1.48830 5
2 -1 -17 7.68529 1.63361 8
2 -1 -17 8.62316 1.16496 6
-2 1 17 5.34052 1.02196 10
-2 1 17 8.86707 1.65679 5
1 -1 -17 2.99613 1.23157 8
1 -1 -17 1.42844 0.72260 6
-1 1 17 0.26258 0.63189 10
-1 1 17 1.11965 1.14251 5
0 -1 -17 71.3186 4.25246 6
0 -1 -17 77.9492 4.67166 8
0 -1 -17 72.8734 3.89921 9
0 -1 -17 70.4721 10.9816 1
0 1 17 62.8467 3.93168 7
0 1 17 69.7681 4.02994 10
0 1 17 80.0401 4.88000 5
0 1 17 76.1334 10.8627 2
0 1 17 83.6354 9.57447 2
-1 -1 -17 -6.9956 9.60377 1
-1 -1 -17 0.70829 0.84779 6
-1 -1 -17 0.00985 0.53600 9
-1 -1 -17 -0.5347 0.96705 8
1 1 17 0.26147 1.03482 5
1 1 17 0.29871 0.46772 10
-2 -1 -17 0.99043 1.10174 8
-2 -1 -17 1.78336 0.75374 9
-2 -1 -17 0.50590 0.87717 6
2 1 17 2.00013 1.07465 5
2 -2 -17 11.5802 1.40834 6
2 -2 -17 10.7967 1.71072 8
-2 2 17 11.8756 1.57127 10
-2 2 17 13.8887 2.13080 5
1 -2 -17 0.21944 0.73880 6
1 -2 -17 0.89507 1.15354 8
-1 2 17 0.42339 0.45501 7
-1 2 17 0.65174 1.06595 5
-1 2 17 -0.1441 0.62651 10
0 -2 -17 15.5269 1.66195 6
0 -2 -17 9.28486 5.90513 1
0 -2 -17 12.1075 6.62303 1
0 -2 -17 10.2092 1.61562 8
0 -2 -17 12.6830 1.06969 9
0 2 17 12.5803 2.03389 5
0 2 17 11.1988 1.21271 10
0 2 17 14.1175 6.75947 2
0 2 17 13.2647 5.22719 2
-1 -2 -17 0.74403 0.91181 6
-1 -2 -17 -0.3781 0.97927 8
-1 -2 -17 0.78500 0.60415 9
1 2 17 0.86832 1.03601 5
1 2 17 1.60315 0.45444 10
-2 -2 -17 -0.2352 0.63548 9
-2 -2 -17 0.16893 0.89354 6
-2 -2 -17 0.10745 0.97023 8
2 2 17 1.07706 0.97641 5
1 -3 -17 0.15212 1.04058 8
1 -3 -17 1.00017 0.80549 6
-1 3 17 1.31249 0.51473 7
-1 3 17 0.54055 0.62372 10
-1 3 17 0.20735 1.08678 5
0 -3 -17 79.5132 4.68718 6
0 -3 -17 80.7799 4.87280 8
0 -3 -17 74.1618 4.26888 9
0 -3 -17 83.6375 11.3558 1
0 3 17 74.6763 4.39972 10
0 3 17 82.1274 10.6292 2
0 3 17 83.7403 5.17163 5
-1 -3 -17 16.7476 1.91792 6
-1 -3 -17 18.3881 2.01799 8
-1 -3 -17 16.6910 1.51649 9
1 3 17 17.5650 1.30361 10
1 3 17 14.7546 2.18280 5
-2 -3 -17 43.4787 2.83882 9
-2 -3 -17 40.4529 3.07083 8
-2 -3 -17 42.8615 3.07969 6
2 3 17 41.0468 3.30474 5
1 -4 -17 0.24335 0.82872 6
1 -4 -17 -0.4077 0.91263 8
-1 4 17 -0.5741 0.44739 7
-1 4 17 -0.2471 0.64912 10
-1 4 17 0.18680 1.12316 5
0 -4 -17 0.59510 0.97259 8
0 -4 -17 -0.2258 0.88007 6
0 -4 -17 -0.3940 0.48657 9
0 -4 -17 4.34219 6.53697 1
0 -4 -17 -5.1974 5.98296 1
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0 4 17 0.10282 8.26839 2
-1 -4 -17 -0.2428 0.86364 8
-1 -4 -17 0.46887 0.86545 6
-1 -4 -17 0.35403 0.62963 9
1 4 17 -0.0794 0.47317 10
1 4 17 0.66419 1.06534 5
-2 -4 -17 6.60761 1.05795 9
-2 -4 -17 10.2449 1.51477 6
-2 -4 -17 8.27182 1.33010 8
2 4 17 6.96941 1.44685 5
1 -5 -17 2.40973 0.97535 6
1 -5 -17 1.78748 1.01603 8
-1 5 17 1.39568 1.17756 5
-1 5 17 0.57862 0.68194 10
-1 5 17 2.22605 0.59409 7
0 -5 -17 9.32711 1.09642 9
0 -5 -17 7.80948 1.28921 6
0 -5 -17 7.40312 1.32905 8
0 -5 -17 -1.4034 7.50500 1
-1 -5 -17 6.02024 1.17651 8
-1 -5 -17 7.43429 1.38930 6
1 5 17 6.71628 1.57354 5
1 5 17 6.92005 0.90234 10
-2 -5 -17 1.29312 0.80684 9
-2 -5 -17 3.74398 1.23052 6
-2 -5 -17 1.61608 0.89907 8
2 5 17 2.92127 1.24782 5
0 -6 -17 5.11399 1.23156 6
0 -6 -17 5.93283 0.86003 9
0 -6 -17 5.49063 1.09240 8
0 6 17 6.49199 1.02668 10
0 6 17 9.46562 1.72507 5
-1 -6 -17 4.26205 1.20003 6
-1 -6 -17 1.24455 0.81450 8
-1 -6 -17 2.96862 0.78970 9
1 6 17 4.43037 1.35192 5
1 6 17 3.31453 0.74921 10
-2 -6 -17 0.19349 1.05521 6
-2 -6 -17 0.14997 0.69321 8
-2 -6 -17 0.90444 0.86325 9
2 6 17 0.20155 1.11682 5
0 -1 -18 124.313 6.96369 6
0 -1 -18 137.272 7.44643 8
0 1 18 133.115 7.61575 5
0 1 18 115.437 6.71877 10
1 1 18 29.9289 2.81089 5
0 -2 -18 2.16823 1.00832 6
0 -2 -18 2.62468 1.32675 8
0 2 18 2.05326 1.30469 5
0 2 18 1.95443 0.63297 10
-1 -2 -18 39.5991 3.19963 8
-1 -2 -18 42.3272 2.98979 6
-1 -2 -18 42.1726 2.63221 9
1 2 18 40.7454 3.36172 5
0 3 18 32.7287 3.00965 5
0 3 18 30.6351 2.14046 10
1 3 18 121.831 7.32833 5
0 0 0 0.00 0.00 0
_exptl_absorpt_process_details
)
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
J. Appl. Cryst. 48 (2015) 3-10
)
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 0.7465
_exptl_absorpt_correction_T_min 0.6326
_exptl_special_details
)
The following wavelength and cell were deduced by SADABS from the
direction cosines etc. They are given here for emergency use only:
CELL 0.71104 4.801 9.828 11.757 82.843 86.835 79.880
)
;
_shelx_hkl_checksum 53291
_shelx_res_file
;
TITL HKL65L_0m_a.res in P-1
HKL65L_0m.res
created by SHELXL-2019/3 at 08:32:17 on 09-Jul-2025
REM Old TITL HKL65L_0m in P-1
REM SHELXT solution in P-1
REM R1 0.132, Rweak 0.007, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C10 O5 Cl
CELL 0.71073 4.7953 9.8084 11.7357 82.828 86.801 79.872
ZERR 2.000 0.0003 0.0006 0.0007 0.002 0.002 0.002
LATT 1
SFAC C H O CL
UNIT 20 26 10 2
OMIT 0 0 1
TEMP -123.150
SIZE 0.45 0.43 0.28
L.S. 10
BOND $H
ACTA
CONF
HTAB
EQIV $1 -x+1, -y+2, -z
HTAB O1 O2_$1
EQIV $2 x+1, y, z
HTAB C5 O3_$2
HTAB C7 O3_$2
EQIV $3 -x+2, -y+1, -z
HTAB C9 O1_$3
EQIV $4 -x+1, -y+1, -z
HTAB C9 O4_$4
LIST 4
FMAP 2
PLAN 20
WGHT 0.048400 0.176200
FVAR 1.22762
CL1 4 0.802776 0.197752 0.288121 11.00000 0.06047 0.03196 =
0.03627 0.00712 -0.01129 -0.01746
O1 3 0.828494 0.887437 0.048993 11.00000 0.02129 0.02436 =
0.01574 0.00254 0.00034 0.00086
REM AFIX 148
H1 2 0.747126 0.933447 -0.008813 11.00000 -1.50000
O2 3 0.420478 0.975128 0.136574 11.00000 0.02123 0.02352 =
0.01802 0.00004 -0.00272 0.00376
O3 3 0.449549 0.741203 0.368504 11.00000 0.01504 0.02613 =
0.01980 -0.00284 0.00029 -0.00485
O4 3 0.556126 0.640178 0.119281 11.00000 0.02725 0.02191 =
0.02734 -0.00639 -0.01353 -0.00072
O5 3 0.935175 0.475569 0.168255 11.00000 0.02312 0.01494 =
0.02223 -0.00713 -0.00366 -0.00154
C1 1 0.657528 0.903705 0.140069 11.00000 0.01876 0.01309 =
0.01582 -0.00054 -0.00186 -0.00315
C2 1 0.791774 0.835449 0.250959 11.00000 0.01626 0.01265 =
0.01427 -0.00151 -0.00238 -0.00262
AFIX 13
H2 2 0.966906 0.874872 0.259902 11.00000 -1.20000
AFIX 0
C3 1 0.592248 0.860721 0.356317 11.00000 0.01964 0.01743 =
0.01610 -0.00411 -0.00184 0.00022
AFIX 13
H3 2 0.460396 0.952191 0.347524 11.00000 -1.20000
AFIX 0
C4 1 0.765917 0.836607 0.465088 11.00000 0.02692 0.02012 =
0.01553 -0.00515 -0.00354 -0.00267
AFIX 23
H4A 2 0.650998 0.871452 0.531491 11.00000 -1.20000
H4B 2 0.936328 0.881552 0.453301 11.00000 -1.20000
AFIX 0
C5 1 0.846199 0.675562 0.481347 11.00000 0.02389 0.01972 =
0.01372 -0.00050 -0.00288 -0.00392
AFIX 23
H5A 2 1.054113 0.644951 0.476462 11.00000 -1.20000
H5B 2 0.770065 0.634912 0.555576 11.00000 -1.20000
AFIX 0
C6 1 0.701146 0.637451 0.379270 11.00000 0.02046 0.01661 =
0.01551 -0.00029 -0.00145 -0.00602
AFIX 13
H6 2 0.662114 0.539725 0.390068 11.00000 -1.20000
AFIX 0
C7 1 0.869352 0.673514 0.264963 11.00000 0.01545 0.01234 =
0.01375 -0.00204 -0.00243 -0.00227
AFIX 13
H7 2 1.077718 0.642931 0.274643 11.00000 -1.20000
AFIX 0
C8 1 0.765990 0.600088 0.174508 11.00000 0.01887 0.01382 =
0.01502 -0.00224 -0.00171 -0.00369
C9 1 0.844015 0.382388 0.097407 11.00000 0.03289 0.01845 =
0.02192 -0.00884 -0.00311 -0.00468
AFIX 23
H9A 2 1.011379 0.318768 0.070243 11.00000 -1.20000
H9B 2 0.750440 0.437367 0.029199 11.00000 -1.20000
AFIX 0
C10 1 0.641922 0.298279 0.162823 11.00000 0.02923 0.02190 =
0.03506 -0.00526 -0.00687 -0.00772
AFIX 23
H10A 2 0.584360 0.234902 0.112594 11.00000 -1.20000
H10B 2 0.469651 0.361535 0.186272 11.00000 -1.20000
REM
REM HKL65L_0m.hkl
REM
AFIX 0
HKLF 4
REM HKL65L_0m_a.res in P-1
REM wR2 = 0.0997, GooF = S = 1.040, Restrained GooF = 1.040 for all data
REM R1 = 0.0353 for 3783 Fo > 4sig(Fo) and 0.0382 for all 4150 data
REM 148 parameters refined using 0 restraints
END
WGHT 0.0484 0.1787
REM Instructions for potential hydrogen bonds
HTAB O1 O2_$1
HTAB C5 O3_$2
HTAB C7 O3_$2
HTAB C9 O1_$3
HTAB C9 O4_$4
REM Highest difference peak 0.443, deepest hole -0.493, 1-sigma level 0.056
Q1 1 0.8151 0.6411 0.2173 11.00000 0.05 0.44
Q2 1 0.7883 0.6576 0.3191 11.00000 0.05 0.42
Q3 1 0.7223 0.3592 0.1293 11.00000 0.05 0.41
Q4 1 0.7136 0.8618 0.1966 11.00000 0.05 0.40
Q5 1 0.6956 0.8484 0.3027 11.00000 0.05 0.39
Q6 1 0.8877 0.1982 0.2420 11.00000 0.05 0.38
Q7 1 0.7691 0.6548 0.4303 11.00000 0.05 0.37
Q8 1 0.6812 0.8544 0.4062 11.00000 0.05 0.36
Q9 1 0.5383 0.9460 0.1392 11.00000 0.05 0.32
Q10 1 0.8019 0.7572 0.4713 11.00000 0.05 0.32
Q11 1 0.6839 0.2418 0.2797 11.00000 0.05 0.31
Q12 1 0.8481 0.7476 0.2570 11.00000 0.05 0.29
Q13 1 0.7393 0.2578 0.2978 11.00000 0.05 0.29
Q14 1 0.6588 0.6198 0.1460 11.00000 0.05 0.28
Q15 1 0.8495 0.5378 0.1670 11.00000 0.05 0.27
Q16 1 0.8527 0.2388 0.1552 11.00000 0.05 0.26
Q17 1 0.8219 0.4786 0.2009 11.00000 0.05 0.26
Q18 1 0.3818 1.0085 0.0823 11.00000 0.05 0.22
Q19 1 0.7454 0.9003 0.0954 11.00000 0.05 0.21
Q20 1 0.3762 0.9604 0.0993 11.00000 0.05 0.21
;
_shelx_res_checksum 21245
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Cl Cl1 0.80278(8) 0.19775(3) 0.28812(3) 0.04232(9) Uani d 1 . .
O O1 0.82849(14) 0.88744(7) 0.04899(5) 0.02150(13) Uani d 1 . .
H H1 0.747(3) 0.9334(17) -0.0088(14) 0.032 Uiso d 1 . .
O O2 0.42048(14) 0.97513(7) 0.13657(6) 0.02198(13) Uani d 1 . .
O O3 0.44955(13) 0.74120(7) 0.36850(5) 0.02018(12) Uani d 1 . .
O O4 0.55613(15) 0.64018(7) 0.11928(6) 0.02514(14) Uani d 1 . .
O O5 0.93518(14) 0.47557(6) 0.16825(6) 0.01977(12) Uani d 1 . .
C C1 0.65753(16) 0.90371(8) 0.14007(7) 0.01589(13) Uani d 1 . .
C C2 0.79177(16) 0.83545(7) 0.25096(6) 0.01431(12) Uani d 1 . .
H H2 0.966906 0.874872 0.259902 0.017 Uiso calc 1 . .
C C3 0.59225(17) 0.86072(8) 0.35632(7) 0.01790(14) Uani d 1 . .
H H3 0.460396 0.952191 0.347524 0.021 Uiso calc 1 . .
C C4 0.76592(19) 0.83661(9) 0.46509(7) 0.02065(15) Uani d 1 . .
H H4A 0.650998 0.871452 0.531491 0.025 Uiso calc 1 . .
H H4B 0.936328 0.881552 0.453301 0.025 Uiso calc 1 . .
C C5 0.84620(18) 0.67556(9) 0.48135(7) 0.01913(14) Uani d 1 . .
H H5A 1.054113 0.644951 0.476462 0.023 Uiso calc 1 . .
H H5B 0.770065 0.634912 0.555576 0.023 Uiso calc 1 . .
C C6 0.70115(17) 0.63745(8) 0.37927(7) 0.01728(14) Uani d 1 . .
H H6 0.662114 0.539725 0.390068 0.021 Uiso calc 1 . .
C C7 0.86935(15) 0.67351(7) 0.26496(6) 0.01374(12) Uani d 1 . .
H H7 1.077718 0.642931 0.274643 0.016 Uiso calc 1 . .
C C8 0.76599(16) 0.60009(8) 0.17451(7) 0.01570(13) Uani d 1 . .
C C9 0.8440(2) 0.38239(9) 0.09741(8) 0.02375(17) Uani d 1 . .
H H9A 1.011379 0.318768 0.070243 0.028 Uiso calc 1 . .
H H9B 0.750440 0.437367 0.029199 0.028 Uiso calc 1 . .
C C10 0.6419(2) 0.29828(10) 0.16282(10) 0.02793(19) Uani d 1 . .
H H10A 0.584360 0.234902 0.112594 0.034 Uiso calc 1 . .
H H10B 0.469651 0.361535 0.186272 0.034 Uiso calc 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
Cl1 0.0605(2) 0.03196(14) 0.03627(15) -0.01746(13) -0.01129(13) 0.00712(10)
O1 0.0213(3) 0.0244(3) 0.0157(3) 0.0009(2) 0.0003(2) 0.0025(2)
O2 0.0212(3) 0.0235(3) 0.0180(3) 0.0038(2) -0.0027(2) 0.0000(2)
O3 0.0150(2) 0.0261(3) 0.0198(3) -0.0048(2) 0.0003(2) -0.0028(2)
O4 0.0272(3) 0.0219(3) 0.0273(3) -0.0007(2) -0.0135(2) -0.0064(2)
O5 0.0231(3) 0.0149(2) 0.0222(3) -0.0015(2) -0.0037(2) -0.0071(2)
C1 0.0188(3) 0.0131(3) 0.0158(3) -0.0031(2) -0.0019(2) -0.0005(2)
C2 0.0163(3) 0.0127(3) 0.0143(3) -0.0026(2) -0.0024(2) -0.0015(2)
C3 0.0196(3) 0.0174(3) 0.0161(3) 0.0002(2) -0.0018(2) -0.0041(2)
C4 0.0269(4) 0.0201(3) 0.0155(3) -0.0027(3) -0.0035(3) -0.0051(3)
C5 0.0239(3) 0.0197(3) 0.0137(3) -0.0039(3) -0.0029(3) -0.0005(2)
C6 0.0205(3) 0.0166(3) 0.0155(3) -0.0060(2) -0.0015(2) -0.0003(2)
C7 0.0155(3) 0.0123(3) 0.0138(3) -0.0023(2) -0.0024(2) -0.0020(2)
C8 0.0189(3) 0.0138(3) 0.0150(3) -0.0037(2) -0.0017(2) -0.0022(2)
C9 0.0329(4) 0.0184(3) 0.0219(4) -0.0047(3) -0.0031(3) -0.0088(3)
C10 0.0292(4) 0.0219(4) 0.0351(5) -0.0077(3) -0.0069(4) -0.0053(3)
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'
Cl Cl 0.1484 0.1585 '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 O1 H1 . . 108.7(11) ?
C6 O3 C3 . . 96.29(6) ?
C8 O5 C9 . . 116.99(7) ?
O2 C1 O1 . . 123.57(7) ?
O2 C1 C2 . . 122.98(7) ?
O1 C1 C2 . . 113.26(7) ?
C1 C2 C3 . . 112.25(6) ?
C1 C2 C7 . . 116.65(6) ?
C3 C2 C7 . . 101.72(6) ?
C1 C2 H2 . . 108.6 ?
C3 C2 H2 . . 108.6 ?
C7 C2 H2 . . 108.6 ?
O3 C3 C4 . . 102.66(7) ?
O3 C3 C2 . . 102.38(6) ?
C4 C3 C2 . . 109.59(7) ?
O3 C3 H3 . . 113.7 ?
C4 C3 H3 . . 113.7 ?
C2 C3 H3 . . 113.7 ?
C3 C4 C5 . . 101.39(6) ?
C3 C4 H4A . . 111.5 ?
C5 C4 H4A . . 111.5 ?
C3 C4 H4B . . 111.5 ?
C5 C4 H4B . . 111.5 ?
H4A C4 H4B . . 109.3 ?
C6 C5 C4 . . 101.07(6) ?
C6 C5 H5A . . 111.6 ?
C4 C5 H5A . . 111.6 ?
C6 C5 H5B . . 111.6 ?
C4 C5 H5B . . 111.6 ?
H5A C5 H5B . . 109.4 ?
O3 C6 C5 . . 103.23(6) ?
O3 C6 C7 . . 102.00(6) ?
C5 C6 C7 . . 110.15(6) ?
O3 C6 H6 . . 113.5 ?
C5 C6 H6 . . 113.5 ?
C7 C6 H6 . . 113.5 ?
C8 C7 C2 . . 116.50(6) ?
C8 C7 C6 . . 107.32(6) ?
C2 C7 C6 . . 100.23(6) ?
C8 C7 H7 . . 110.7 ?
C2 C7 H7 . . 110.7 ?
C6 C7 H7 . . 110.7 ?
O4 C8 O5 . . 123.81(7) ?
O4 C8 C7 . . 126.48(7) ?
O5 C8 C7 . . 109.59(6) ?
O5 C9 C10 . . 111.17(8) ?
O5 C9 H9A . . 109.4 ?
C10 C9 H9A . . 109.4 ?
O5 C9 H9B . . 109.4 ?
C10 C9 H9B . . 109.4 ?
H9A C9 H9B . . 108.0 ?
C9 C10 Cl1 . . 110.84(7) ?
C9 C10 H10A . . 109.5 ?
Cl1 C10 H10A . . 109.5 ?
C9 C10 H10B . . 109.5 ?
Cl1 C10 H10B . . 109.5 ?
H10A C10 H10B . . 108.1 ?
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
Cl1 C10 . 1.7963(11) ?
O1 C1 . 1.3186(10) ?
O1 H1 . 0.841(16) ?
O2 C1 . 1.2258(10) ?
O3 C6 . 1.4354(10) ?
O3 C3 . 1.4465(11) ?
O4 C8 . 1.2072(10) ?
O5 C8 . 1.3500(10) ?
O5 C9 . 1.4452(10) ?
C1 C2 . 1.5102(11) ?
C2 C3 . 1.5384(11) ?
C2 C7 . 1.5563(10) ?
C2 H2 . 1.0000 ?
C3 C4 . 1.5339(12) ?
C3 H3 . 1.0000 ?
C4 C5 . 1.5488(12) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.5346(11) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.5609(11) ?
C6 H6 . 1.0000 ?
C7 C8 . 1.5055(10) ?
C7 H7 . 1.0000 ?
C9 C10 . 1.4997(14) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
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 2_675 0.841(16) 1.801(17) 2.6413(9) 177.2(16) yes
C5 H5A O3 1_655 0.99 2.48 3.2487(11) 134.1 yes
C7 H7 O3 1_655 1.00 2.53 3.2995(10) 133.3 yes
C9 H9A O1 2_765 0.99 2.58 3.4344(11) 143.9 yes
C9 H9B O4 2_665 0.99 2.61 3.3215(11) 129.3 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O2 C1 C2 C3 . . . . 2.59(11) ?
O1 C1 C2 C3 . . . . 177.78(7) ?
O2 C1 C2 C7 . . . . 119.39(8) ?
O1 C1 C2 C7 . . . . -65.42(9) ?
C6 O3 C3 C4 . . . . -56.25(7) ?
C6 O3 C3 C2 . . . . 57.40(7) ?
C1 C2 C3 O3 . . . . 91.57(7) ?
C7 C2 C3 O3 . . . . -33.87(7) ?
C1 C2 C3 C4 . . . . -159.99(7) ?
C7 C2 C3 C4 . . . . 74.57(7) ?
O3 C3 C4 C5 . . . . 34.64(8) ?
C2 C3 C4 C5 . . . . -73.61(8) ?
C3 C4 C5 C6 . . . . -0.46(8) ?
C3 O3 C6 C5 . . . . 56.17(7) ?
C3 O3 C6 C7 . . . . -58.15(6) ?
C4 C5 C6 O3 . . . . -34.22(8) ?
C4 C5 C6 C7 . . . . 74.07(8) ?
C1 C2 C7 C8 . . . . -8.36(9) ?
C3 C2 C7 C8 . . . . 114.11(7) ?
C1 C2 C7 C6 . . . . -123.70(7) ?
C3 C2 C7 C6 . . . . -1.24(7) ?
O3 C6 C7 C8 . . . . -85.78(7) ?
C5 C6 C7 C8 . . . . 165.12(6) ?
O3 C6 C7 C2 . . . . 36.31(7) ?
C5 C6 C7 C2 . . . . -72.79(7) ?
C9 O5 C8 O4 . . . . -4.82(12) ?
C9 O5 C8 C7 . . . . 171.46(7) ?
C2 C7 C8 O4 . . . . -28.93(12) ?
C6 C7 C8 O4 . . . . 82.38(10) ?
C2 C7 C8 O5 . . . . 154.91(6) ?
C6 C7 C8 O5 . . . . -93.78(7) ?
C8 O5 C9 C10 . . . . -84.98(10) ?
O5 C9 C10 Cl1 . . . . -58.64(9) ?