#------------------------------------------------------------------------------
#$Date: 2021-05-15 07:50:02 +0300 (Sat, 15 May 2021) $
#$Revision: 265246 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243831.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_2243831
loop_
_publ_author_name
'Behrman, Edward J.'
'Parkin, Sean'
_publ_section_title
;
Synthesis and crystal structures of 3,6-dihydroxypicolinic acid and its
labile intermediate dipotassium
3-hydroxy-6-(sulfonatooxy)pyridine-2-carboxylate monohydrate
;
_journal_coeditor_code HB7975
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 623
_journal_page_last 628
_journal_paper_doi 10.1107/S2056989021004904
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac '2K +, C6 H3 N O7 S 2-, H2 O1'
_chemical_formula_moiety '2(K +), C6 H3 N O7 S 2-, H2 O1'
_chemical_formula_sum 'C6 H5 K2 N O8 S'
_chemical_formula_weight 329.37
_chemical_name_systematic
;
Dipotassium 3-hydroxy-6-(sulfonatooxy)pyridine-2-carboxylate monohydrate
;
_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'
_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 103.5530(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 13.3366(4)
_cell_length_b 11.5467(3)
_cell_length_c 7.3078(2)
_cell_measurement_reflns_used 9459
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.49
_cell_measurement_theta_min 3.14
_cell_volume 1094.02(5)
_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
;
SHELX (Sheldrick, 2008) and CIFFIX (Parkin, 2013)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 0.0362
_diffrn_reflns_av_unetI/netI 0.0216
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 22347
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.493
_diffrn_reflns_theta_min 1.571
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 1.091
_exptl_absorpt_correction_T_max 0.862
_exptl_absorpt_correction_T_min 0.793
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.000
_exptl_crystal_description block
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.160
_exptl_crystal_size_min 0.130
_refine_diff_density_max 0.398
_refine_diff_density_min -0.437
_refine_ls_extinction_coef 0.0116(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.078
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 174
_refine_ls_number_reflns 2505
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.078
_refine_ls_R_factor_all 0.0212
_refine_ls_R_factor_gt 0.0204
_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^)+(0.0254P)^2^+0.7213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0548
_refine_ls_wR_factor_ref 0.0555
_reflns_number_gt 2423
_reflns_number_total 2505
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7975sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2243831
_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 0.828
_shelx_estimated_absorpt_t_max 0.871
_shelx_hkl_file
;
-1 0 0 0.53895 0.15747 5
1 0 0 0.50412 0.42259 1
1 0 0 0.52858 0.15944 3
1 0 0 0.75043 0.17650 3
1 0 0 1.07564 0.19262 4
1 0 0 0.49271 0.15009 5
-1 0 0 0.66892 0.17383 3
-1 0 0 0.40613 0.13831 3
-1 0 0 1.45463 0.55790 1
-2 0 0 341.257 13.2642 5
2 0 0 292.008 15.0422 1
2 0 0 357.482 13.1731 3
2 0 0 355.989 13.1902 4
2 0 0 365.068 13.2680 5
-2 0 0 380.230 13.2636 4
-2 0 0 348.220 13.1813 3
-2 0 0 321.257 15.4274 1
-2 0 0 367.078 13.2472 3
3 0 0 0.51209 0.28956 5
3 0 0 0.66013 0.31389 4
-3 0 0 -0.1208 1.30221 1
3 0 0 -0.1976 1.05519 1
3 0 0 -0.0457 0.22515 3
3 0 0 0.43579 0.27710 3
-3 0 0 -0.1224 0.21415 4
-3 0 0 0.28696 0.30114 5
-3 0 0 0.37288 0.29831 3
-3 0 0 1.57242 0.40323 3
-4 0 0 366.230 15.6331 3
-4 0 0 399.271 15.5925 3
4 0 0 399.642 15.5143 3
4 0 0 403.668 15.6392 3
4 0 0 423.930 15.6177 4
4 0 0 391.587 15.6834 5
-4 0 0 426.637 15.9139 5
-4 0 0 406.004 20.4727 1
-4 0 0 387.927 15.6450 4
4 0 0 396.379 19.8720 1
5 0 0 1.54255 0.70064 3
5 0 0 4.11925 2.70054 1
-5 0 0 3.45273 2.98029 1
-6 0 0 268.966 11.6407 3
6 0 0 269.070 11.4320 3
6 0 0 271.122 11.2677 4
6 0 0 273.248 17.4273 1
-6 0 0 261.692 18.0786 1
-6 0 0 258.903 11.4850 4
6 0 0 256.194 11.4771 5
-6 0 0 275.804 11.8228 5
7 0 0 -0.1488 4.08821 1
7 0 0 0.09374 0.73370 3
7 0 0 0.33990 0.52412 4
-7 0 0 -0.0376 0.68106 5
-7 0 0 0.02869 0.85822 3
-7 0 0 1.11992 4.62729 1
-8 0 0 1130.08 55.7585 1
-8 0 0 1134.82 43.8697 3
8 0 0 1099.13 43.1400 4
-8 0 0 1156.47 44.1047 5
9 0 0 0.02019 0.94373 3
-9 0 0 -1.2541 0.86603 3
-9 0 0 0.44342 1.05976 5
-9 0 0 -9.0644 9.55291 1
0 1 0 0.31437 0.08765 4
-1 -1 0 507.447 19.7247 1
1 1 0 511.971 19.6821 1
-1 1 0 473.274 19.3802 1
-2 -1 0 255.326 10.2225 4
-2 -1 0 265.337 10.0775 5
2 -1 0 251.931 9.93289 3
2 -1 0 274.090 12.2454 1
-2 -1 0 254.689 10.0394 3
2 -1 0 261.220 9.99603 3
2 -1 0 254.532 9.87762 4
-2 -1 0 267.466 10.1241 3
2 -1 0 268.834 10.1978 5
-2 1 0 265.045 9.92406 4
2 1 0 276.078 10.1234 3
2 1 0 269.765 10.1146 3
-2 1 0 281.859 10.0758 3
2 1 0 243.451 12.1750 1
-2 1 0 249.296 10.0033 3
2 1 0 258.372 10.0284 5
-2 1 0 275.947 10.2662 5
2 1 0 265.550 10.2080 4
-2 1 0 244.756 12.1564 1
3 -1 0 6.18743 0.76927 5
3 -1 0 5.50401 0.64656 3
3 -1 0 5.21464 0.66954 3
-3 -1 0 7.34854 0.88371 3
3 -1 0 6.17346 0.61309 4
-3 -1 0 4.25194 1.72605 1
3 -1 0 4.46267 1.67953 1
-3 -1 0 7.25109 0.77003 3
-3 -1 0 5.63950 0.77900 4
-3 -1 0 4.92394 0.70341 5
-3 1 0 7.47972 0.87624 5
-3 1 0 5.29789 1.66309 1
3 1 0 5.40112 0.72935 3
3 1 0 8.00341 2.09304 1
3 1 0 7.41595 0.82789 3
-3 1 0 5.88027 0.71535 3
-3 1 0 4.95479 0.63138 4
3 1 0 5.19258 0.71963 4
-3 1 0 5.10047 0.70769 3
-4 1 0 3982.91 150.717 1
5 -1 0 297.226 11.2564 4
-5 -1 0 272.587 11.3574 3
5 -1 0 258.549 11.5003 5
-5 -1 0 297.375 11.6831 3
5 -1 0 256.603 11.0805 3
-5 -1 0 269.787 17.0791 1
5 -1 0 275.351 11.3316 3
5 -1 0 261.470 15.9808 1
-5 -1 0 277.708 11.6744 4
-5 -1 0 277.174 11.5940 5
-5 1 0 270.182 11.3014 4
5 1 0 274.001 11.4771 3
-5 1 0 276.889 11.5635 3
5 1 0 291.541 11.4086 3
5 1 0 289.736 16.7453 1
5 1 0 283.615 11.4575 5
5 1 0 264.034 11.4095 4
-5 1 0 289.167 11.8699 5
-5 1 0 267.783 11.3457 3
-5 1 0 257.462 16.5924 1
6 -1 0 249.414 12.6171 5
-6 -1 0 284.583 12.3508 3
6 -1 0 307.469 18.3976 1
6 -1 0 284.642 12.0516 3
-6 -1 0 252.502 18.4287 1
6 -1 0 295.992 11.8573 4
-6 -1 0 283.116 12.4241 4
-6 -1 0 293.827 12.4435 5
6 -1 0 292.331 12.3185 3
-6 1 0 305.756 12.4929 3
-6 1 0 272.348 18.6075 1
-6 1 0 299.413 12.1502 4
-6 1 0 285.664 12.5860 5
6 1 0 299.441 18.5049 1
6 1 0 290.024 12.2601 3
6 1 0 308.467 12.2802 4
6 1 0 277.168 12.1469 5
7 -1 0 5.16199 4.39078 1
7 -1 0 3.50059 0.89765 4
-7 -1 0 3.15918 1.08344 5
-7 -1 0 4.08763 1.21543 3
7 -1 0 4.92565 1.16346 3
-7 1 0 5.19574 5.08556 1
7 1 0 6.36431 4.69512 1
-7 1 0 4.20752 1.13811 3
7 1 0 5.11089 1.26664 3
-7 1 0 2.95593 1.16534 5
7 1 0 3.39757 1.01211 4
-8 -1 0 102.503 14.6041 1
8 -1 0 95.3177 5.30916 4
-8 -1 0 97.3333 6.00980 5
-8 -1 0 100.513 5.95851 3
8 -1 0 104.097 13.0399 1
-8 1 0 95.2635 6.11102 5
8 1 0 98.2623 5.76124 3
-8 1 0 103.089 6.12147 3
8 1 0 101.874 13.2080 1
-8 1 0 85.8586 13.3842 1
9 -1 0 24.6374 2.64805 3
-9 -1 0 16.8369 2.78108 5
-9 -1 0 18.6036 2.81257 3
-9 -1 0 21.1793 11.4464 1
9 1 0 25.5087 2.72097 3
-9 1 0 12.1865 10.2168 1
-9 1 0 24.0111 3.17112 3
-9 1 0 22.3177 2.95372 5
-1 -2 0 295.581 12.9409 1
1 -2 0 311.621 12.4518 1
-1 -2 0 325.434 11.8631 4
-1 2 0 299.749 11.6985 5
1 2 0 304.216 11.8079 4
1 2 0 313.811 12.9283 1
-1 2 0 320.302 12.5642 1
-2 -2 0 2829.39 101.102 2
-2 2 0 2460.77 99.3941 2
2 2 0 2521.14 100.172 2
-3 -2 0 69.7895 3.27755 3
3 -2 0 64.1053 2.93518 3
-3 -2 0 68.2320 3.17102 5
3 -2 0 66.5329 3.03272 3
3 -2 0 64.5520 2.85502 4
3 -2 0 81.4341 5.74636 1
-3 -2 0 56.7677 5.33744 1
-3 -2 0 67.4033 3.49259 4
3 -2 0 64.0616 3.33591 5
-3 -2 0 66.2720 3.15300 3
3 2 0 64.6761 3.23440 3
3 2 0 62.9444 3.22946 3
3 2 0 69.3450 3.44396 4
-3 2 0 71.5112 3.83822 5
-3 2 0 70.8746 5.67526 1
-3 2 0 65.5533 3.15764 3
-3 2 0 65.9610 3.13583 3
-3 2 0 60.2972 2.88808 4
3 2 0 70.3677 3.14127 5
3 2 0 73.0601 5.85269 1
-4 -2 0 693.381 27.4777 4
-4 -2 0 709.460 27.0534 3
-4 -2 0 765.582 32.8603 1
4 -2 0 685.897 26.7378 3
-4 -2 0 794.256 27.3586 3
4 -2 0 718.248 26.6932 4
4 -2 0 729.165 31.5319 1
4 -2 0 710.201 27.3508 5
4 -2 0 709.434 26.9025 3
-4 2 0 700.060 26.7955 4
-4 2 0 692.247 27.1279 3
-4 2 0 627.673 31.3644 1
4 2 0 746.079 27.4366 4
4 2 0 736.463 27.2654 3
-4 2 0 711.371 27.0684 3
4 2 0 716.599 31.9571 1
4 2 0 758.783 27.2275 3
4 2 0 711.333 27.0149 5
-4 2 0 711.049 27.5017 5
5 -2 0 4.44934 2.68667 1
-5 -2 0 6.67028 3.08688 1
-5 -2 0 3.86355 0.99486 4
5 -2 0 2.63001 0.60525 4
-5 -2 0 3.95339 0.82541 3
5 -2 0 3.15409 0.74900 3
-5 -2 0 4.17728 0.88808 5
5 -2 0 3.61823 0.70388 3
-5 2 0 2.89335 2.64736 1
-5 2 0 3.49845 0.95291 5
5 2 0 4.60225 1.01618 3
-5 2 0 5.30862 1.01968 3
5 2 0 4.05745 0.81833 5
-5 2 0 3.81053 0.72078 4
5 2 0 3.20315 0.84592 3
5 2 0 3.55393 2.82612 1
-5 2 0 6.02544 1.03800 3
5 2 0 4.68664 0.94659 4
-6 -2 0 259.159 18.3002 1
-6 -2 0 261.941 11.6786 5
6 -2 0 266.834 11.3357 3
6 -2 0 263.196 11.0271 4
-6 -2 0 263.692 11.6906 3
6 -2 0 268.102 17.2200 1
6 -2 0 262.409 11.0756 3
6 2 0 289.393 12.3827 5
6 2 0 276.220 11.7935 4
-6 2 0 296.216 11.9666 3
6 2 0 304.567 18.3180 1
-6 2 0 262.055 17.9970 1
6 2 0 271.277 11.7477 3
-7 -2 0 2.43057 1.03755 4
7 -2 0 4.33940 1.06962 3
-7 -2 0 5.80377 1.38076 3
-7 -2 0 -4.2313 4.65276 1
7 -2 0 2.68183 4.14523 1
7 -2 0 4.67440 0.93283 4
-7 -2 0 2.63019 1.10942 5
-7 2 0 2.95730 1.08331 3
7 2 0 1.90553 4.95363 1
7 2 0 3.47193 1.02727 4
-7 2 0 1.23482 4.76967 1
-7 2 0 2.51176 1.04933 5
7 2 0 2.92824 1.06538 3
-8 -2 0 195.274 18.8498 1
8 -2 0 176.447 8.08113 4
8 -2 0 165.500 8.76695 3
-8 -2 0 171.894 8.92339 5
-8 -2 0 174.343 8.97370 3
8 2 0 175.758 8.85544 3
8 2 0 183.550 17.1678 1
-8 2 0 179.051 9.41224 5
-8 2 0 191.523 18.5178 1
-8 2 0 184.192 9.16078 3
-9 -2 0 31.3775 3.26976 3
9 -2 0 36.3606 3.00192 3
-9 -2 0 26.9770 3.82318 5
-9 2 0 32.1218 3.57436 5
9 2 0 31.1394 3.32594 3
0 -3 0 0.28572 0.17948 4
0 3 0 0.59356 0.20899 4
-1 -3 0 102.857 4.39451 4
-1 -3 0 91.3244 5.21882 1
1 -3 0 99.1723 4.63134 1
1 3 0 99.8315 3.87187 3
1 3 0 99.6457 3.79856 5
-1 3 0 101.154 4.75298 1
1 3 0 101.047 3.88698 3
1 3 0 102.716 4.37375 4
1 3 0 97.8970 5.18986 1
-1 3 0 97.8664 3.82796 4
-1 3 0 110.758 4.25859 5
-2 -3 0 648.712 26.2451 1
2 -3 0 583.887 25.0104 1
2 3 0 627.639 25.9310 1
-2 3 0 644.503 25.4890 1
3 -3 0 950.620 35.1029 1
3 -3 0 814.761 31.7925 5
-3 -3 0 829.677 35.6824 1
-3 -3 0 886.688 32.1258 4
-3 -3 0 830.800 31.3996 3
3 3 0 898.069 35.6543 1
3 3 0 824.821 31.5838 3
-3 3 0 825.400 31.8979 5
-3 3 0 762.902 34.6801 1
-4 -3 0 2483.03 90.0103 1
-4 3 0 2098.67 88.1722 1
4 3 0 2240.75 88.6315 1
-5 -3 0 2312.09 85.2485 1
-5 -3 0 1950.05 76.3851 3
5 -3 0 2111.56 82.4208 1
5 3 0 2094.65 77.0200 4
-5 3 0 2006.91 83.1489 1
5 3 0 2150.66 83.5602 1
5 3 0 1933.93 76.5657 3
-6 -3 0 463.604 25.9449 1
6 -3 0 445.684 17.2205 4
6 -3 0 440.665 17.4817 3
6 -3 0 438.047 17.2751 3
-6 -3 0 459.780 18.0709 5
-6 -3 0 445.657 18.1106 3
6 -3 0 436.749 23.9121 1
-6 -3 0 439.556 18.6258 4
6 3 0 416.723 24.3526 1
-6 3 0 477.098 18.2978 3
-6 3 0 423.612 18.5710 5
6 3 0 472.564 18.4554 4
-6 3 0 458.586 25.4036 1
6 3 0 436.660 17.7998 5
7 -3 0 44.9972 3.03563 3
7 -3 0 36.1907 2.46976 4
7 -3 0 28.6830 6.84923 1
-7 -3 0 41.7222 3.29300 3
-7 -3 0 40.4776 8.47551 1
-7 -3 0 38.3301 3.04191 5
7 -3 0 42.1444 2.77973 3
-7 -3 0 38.1349 3.35617 4
7 3 0 42.2035 8.21026 1
7 3 0 38.9126 3.18435 3
-7 3 0 38.5588 8.30421 1
-7 3 0 43.1256 3.43046 3
-7 3 0 40.3928 3.49200 5
-8 -3 0 99.3813 15.1167 1
-8 -3 0 112.416 6.56775 3
8 -3 0 117.189 5.70862 4
8 -3 0 123.817 6.00072 3
-8 -3 0 125.687 6.83719 5
8 3 0 120.853 13.4227 1
-8 3 0 111.071 7.04433 5
8 3 0 128.361 6.90293 3
-8 3 0 123.377 6.96179 3
-8 3 0 111.730 15.0305 1
9 -3 0 1.74336 1.11656 3
-9 -3 0 -10.998 10.3235 1
-9 -3 0 3.76811 1.48521 5
-9 -3 0 -0.9396 10.6490 1
9 3 0 -0.6505 1.05011 3
-1 -4 0 5349.68 194.003 2
-1 4 0 5503.71 191.981 2
-1 4 0 5015.21 191.664 2
1 4 0 5136.12 193.503 2
-2 -4 0 85.4037 3.37422 3
-2 -4 0 85.5823 4.25405 4
-2 -4 0 91.3882 6.05861 1
-2 -4 0 89.5419 3.37421 3
2 -4 0 81.8128 5.00514 1
-2 -4 0 86.1755 3.47544 5
-2 4 0 84.8281 4.05570 5
2 4 0 86.7172 3.73480 3
2 4 0 84.7550 3.45005 5
2 4 0 91.9807 5.88036 1
-2 4 0 85.6748 3.39798 3
-2 4 0 83.7842 5.32496 1
2 4 0 91.7356 4.25929 4
2 4 0 87.3010 3.76784 3
-2 4 0 85.8467 3.42721 3
-3 -4 0 1093.79 44.7459 1
3 -4 0 1162.02 43.5142 1
3 4 0 1053.82 40.7973 4
3 4 0 1088.93 40.3747 3
-3 4 0 1088.54 40.7504 5
-3 4 0 1044.67 43.6061 1
3 4 0 1084.47 44.2887 1
4 -4 0 320.451 12.1783 4
-4 -4 0 315.605 17.9496 1
-4 -4 0 325.686 12.8339 3
4 -4 0 324.543 12.1228 3
-4 -4 0 325.288 12.8363 5
-4 -4 0 342.516 13.8250 4
-4 -4 0 317.200 12.9369 3
4 -4 0 348.984 16.9320 1
4 -4 0 332.655 12.1553 3
-4 4 0 328.652 12.9256 3
-4 4 0 334.197 13.6115 5
4 4 0 316.768 13.1160 3
-4 4 0 325.217 17.2585 1
4 4 0 349.259 13.6683 4
4 4 0 334.413 13.2165 3
-4 4 0 335.663 12.9795 3
4 4 0 324.041 12.7410 5
4 4 0 288.090 17.0487 1
-5 -4 0 87.4615 9.26197 1
-5 -4 0 79.9421 5.35586 4
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5 5 -15 8.55463 2.02309 3
4 -5 -15 212.830 10.4879 4
-4 5 15 207.607 10.9873 5
4 5 -15 220.756 10.5908 3
-4 5 15 215.424 10.8498 3
-3 -5 15 106.819 5.31372 3
3 -5 -15 93.5438 6.01073 4
3 -5 -15 95.5162 16.6886 1
3 -5 -15 100.351 5.03732 3
-3 5 15 82.6896 13.8764 1
-3 5 15 108.303 6.43012 3
3 5 -15 103.214 6.04388 3
2 -5 -15 614.038 25.4084 4
2 -5 -15 607.552 23.8704 3
-2 -5 15 616.748 23.9182 3
2 -5 -15 608.699 38.0387 1
-2 5 15 619.221 25.5544 3
2 5 -15 635.430 25.1932 3
-2 5 15 608.620 37.2495 1
1 -5 -15 193.792 21.1860 1
-1 -5 15 188.245 8.21381 3
-1 5 15 165.943 19.0701 1
1 5 -15 183.538 9.19926 3
-1 5 15 189.376 9.52810 3
0 5 -15 271.891 12.4401 3
0 5 15 280.245 12.8711 3
0 5 15 249.394 24.0303 1
-1 -5 -15 120.280 6.05457 3
1 5 15 117.674 6.95454 3
-1 5 -15 108.714 6.54892 3
-4 -6 15 4.29828 1.14966 3
4 -6 -15 7.79622 1.80557 4
-4 6 15 3.43695 1.49124 3
-4 6 15 6.55302 1.60121 5
4 6 -15 4.90568 1.51956 3
3 -6 -15 1.49317 1.14291 4
3 -6 -15 -0.5560 0.93051 3
-3 -6 15 -0.0682 0.73418 3
-3 6 15 -0.8701 0.89611 3
3 6 -15 2.28802 1.12439 3
2 -6 -15 638.193 25.1985 3
2 -6 -15 672.756 27.2870 4
-2 6 15 660.386 27.2794 3
2 6 -15 691.181 27.0048 3
1 6 -15 323.564 14.5231 3
-1 6 15 332.630 14.9321 3
0 -6 -15 4.27702 1.26333 3
0 6 -15 6.81756 1.68408 3
0 6 15 6.20007 1.80337 3
3 -7 -15 9.43379 1.97554 4
-3 7 15 10.8074 2.23513 3
3 7 -15 6.75988 1.52183 3
-2 7 15 213.785 10.6963 3
2 7 -15 209.400 10.3004 3
1 7 -15 414.846 17.3517 3
-1 7 15 385.656 17.6430 3
5 0 -16 -7.2412 10.4218 1
-5 0 16 -1.0439 0.90766 3
-5 0 16 -3.4201 9.85462 1
4 0 -16 24.8763 2.77232 3
-4 0 16 30.8863 10.1010 1
4 0 -16 27.0214 11.3276 1
3 0 -16 0.93184 0.97726 3
3 0 -16 -19.904 8.82715 1
-3 0 16 3.68829 8.27169 1
2 0 -16 225.362 10.5501 3
-2 0 16 238.695 10.9854 3
-2 0 16 201.835 20.7179 1
2 0 -16 233.160 23.6049 1
-1 0 16 -9.3809 7.77857 1
1 0 -16 -0.3516 0.88519 3
-1 0 16 1.37804 0.93418 3
1 0 -16 16.6417 10.2107 1
0 0 16 159.447 21.1714 1
0 0 -16 129.135 20.5333 1
0 0 16 162.009 8.17659 3
-1 0 -16 -0.0915 1.08517 3
1 0 16 3.94617 9.24889 1
-1 0 -16 -8.1781 11.4325 1
-5 -1 16 0.17833 1.24143 3
5 -1 -16 -6.4756 11.1615 1
-5 -1 16 -7.9245 9.99710 1
5 1 -16 1.82072 1.17745 3
-5 1 16 1.07937 1.36370 3
-5 1 16 19.9371 10.3296 1
5 1 -16 3.58756 11.3230 1
4 -1 -16 19.1079 2.20515 3
4 -1 -16 24.8339 11.8357 1
-4 -1 16 20.7733 2.76175 3
-4 1 16 13.6770 9.49474 1
4 1 -16 22.1303 2.95286 3
4 1 -16 29.5026 13.1148 1
-4 1 16 23.2304 2.84003 3
3 -1 -16 4.25352 1.19271 3
-3 -1 16 -4.3502 9.23651 1
-3 -1 16 4.84101 1.51269 3
3 -1 -16 1.61898 9.79618 1
3 1 -16 14.5486 9.94982 1
3 1 -16 5.03605 1.55203 3
-3 1 16 6.67190 8.35788 1
2 -1 -16 52.8001 3.93862 3
2 -1 -16 71.6705 14.3631 1
-2 -1 16 57.6727 4.27804 3
-2 1 16 52.4268 4.28899 3
2 1 -16 38.2665 13.3924 1
2 1 -16 64.3666 4.30829 3
-2 1 16 63.2251 11.9749 1
-1 -1 16 4.91130 1.43475 3
1 -1 -16 8.94844 9.42917 1
1 -1 -16 4.64677 1.36490 3
-1 -1 16 5.69946 7.83220 1
-1 1 16 6.41180 1.53304 3
-1 1 16 3.40274 8.26033 1
1 1 -16 -4.1673 11.8085 1
0 -1 16 22.8891 9.78317 1
0 -1 16 12.9795 2.12792 3
0 -1 -16 21.1291 2.33095 3
0 -1 -16 0.64717 10.4110 1
0 1 16 16.2686 9.09349 1
0 1 -16 14.3391 10.5724 1
-1 -1 -16 36.3377 3.41768 3
-1 -1 -16 30.0157 14.0297 1
1 -1 16 38.3761 3.50308 3
1 1 16 47.1271 3.76882 3
1 1 16 58.1008 13.0445 1
-1 1 -16 42.9859 3.49142 3
-5 -2 16 4.43739 1.38070 3
5 -2 -16 0.71626 1.12812 3
-5 -2 16 4.06405 10.1468 1
-5 2 16 11.6974 10.8306 1
5 2 -16 22.5048 11.8421 1
-4 -2 16 72.2571 13.8117 1
4 -2 -16 109.168 17.2155 1
4 -2 -16 94.3185 5.27144 3
4 2 -16 90.9462 15.7310 1
-4 2 16 94.3189 6.00023 3
4 2 -16 88.3421 5.61424 3
-4 2 16 70.8970 13.7026 1
3 -2 -16 416.236 32.0761 1
-3 -2 16 421.745 18.3554 3
3 -2 -16 425.644 18.0384 3
3 2 -16 406.576 31.5144 1
-3 2 16 496.933 32.2544 1
-3 2 16 462.713 19.1397 3
3 2 -16 448.270 18.7174 3
2 -2 -16 1.79643 1.07847 3
2 -2 -16 4.69188 7.02494 1
-2 -2 16 4.09345 1.34945 3
-2 -2 16 -0.9557 7.74538 1
-2 2 16 1.85606 1.26833 3
-2 2 16 -0.1679 8.31806 1
2 2 -16 0.42976 9.69523 1
2 2 -16 2.11485 1.21104 3
-1 -2 16 140.341 7.41552 3
1 -2 -16 168.495 20.5058 1
-1 -2 16 121.342 16.7378 1
1 2 -16 140.781 7.58131 3
-1 2 16 152.836 8.07172 3
1 2 -16 148.910 19.8704 1
-1 2 16 153.656 18.2539 1
0 -2 -16 21.7074 2.48546 3
0 -2 -16 22.5618 11.8774 1
0 -2 16 20.5525 2.52477 3
0 2 16 27.0643 2.90219 3
0 2 -16 22.3004 2.56274 3
0 2 16 42.3150 10.8256 1
-1 -2 -16 58.5110 16.2362 1
-1 -2 -16 50.5305 4.38347 3
1 -2 16 66.9995 4.27627 3
-1 2 -16 58.0424 4.37323 3
1 2 16 61.7209 13.0748 1
1 2 16 62.8271 4.55430 3
5 -3 -16 62.5745 4.13829 3
4 -3 -16 51.7720 3.57485 3
-4 -3 16 41.5238 3.71661 3
-4 3 16 54.4121 4.40266 3
4 3 -16 57.0655 4.27849 3
-3 -3 16 214.456 10.3225 3
3 -3 -16 211.544 9.96065 3
3 -3 -16 216.332 23.5302 1
-3 3 16 229.272 11.1347 3
3 3 -16 238.224 10.8535 3
-2 -3 16 1.28296 0.85177 3
2 -3 -16 2.70368 1.03939 3
2 3 -16 3.00254 1.21949 3
-2 3 16 13.5259 9.27179 1
-2 3 16 2.86334 1.22018 3
-1 -3 16 48.2709 3.52252 3
1 -3 -16 44.4909 3.41694 3
1 -3 -16 42.9421 12.9799 1
-1 3 16 58.0861 12.5560 1
1 3 -16 51.7107 3.99972 3
-1 3 16 50.3127 4.07695 3
0 -3 -16 4.82198 12.1177 1
0 -3 -16 4.86289 1.27330 3
0 -3 16 4.40521 1.26983 3
0 3 -16 2.76049 1.24879 3
0 3 16 3.79923 1.40230 3
0 3 16 4.42272 9.05971 1
4 -4 -16 7.32243 1.48688 3
-4 -4 16 10.6644 1.82379 3
4 4 -16 5.83621 1.51898 3
-4 4 16 7.49859 1.89921 3
3 -4 -16 143.280 7.13522 3
-3 -4 16 151.843 7.42612 3
3 4 -16 156.728 8.07807 3
-3 4 16 149.961 8.35095 3
-3 4 16 141.587 26.1685 1
2 -4 -16 187.686 8.71249 3
-2 -4 16 181.694 8.76962 3
2 4 -16 203.909 9.64495 3
-2 4 16 181.059 20.4163 1
-2 4 16 192.867 9.85840 3
1 -4 -16 23.8916 2.27283 3
-1 -4 16 24.6011 2.32569 3
1 4 -16 21.9943 2.53248 3
-1 4 16 15.5243 11.9823 1
-1 4 16 20.1536 2.90913 3
0 -4 16 255.729 11.2303 3
0 -4 -16 217.678 10.4081 3
0 4 -16 222.040 11.7201 3
0 4 16 239.150 11.5093 3
3 -5 -16 37.3465 2.67059 3
-3 -5 16 36.3837 2.84264 3
3 5 -16 33.5702 3.63850 3
-3 5 16 28.7464 3.71334 3
2 -5 -16 27.6252 2.36561 3
2 5 -16 26.1815 2.91106 3
-2 5 16 25.0616 3.11777 3
-1 -5 16 75.5546 4.67995 3
1 5 -16 85.0055 5.95638 3
-1 5 16 92.2519 6.45002 3
3 0 -17 0.76489 0.93479 3
-3 0 17 1.50640 1.34818 3
-2 0 17 363.722 33.3527 1
-2 0 17 351.452 15.7549 3
-1 0 17 -0.2661 0.96511 3
1 0 -17 0.78631 12.0333 1
-1 0 17 -0.1416 9.66074 1
1 0 -17 -0.4080 0.82882 3
-3 -1 17 31.4194 12.2339 1
3 -1 -17 37.5720 13.7118 1
3 1 -17 55.2942 14.7616 1
-3 1 17 35.8725 12.4019 1
-3 1 17 50.3429 4.14985 3
3 1 -17 53.4611 3.97139 3
-2 -1 17 75.5246 14.2309 1
2 -1 -17 76.9302 17.8276 1
-2 -1 17 63.3034 4.69936 3
2 1 -17 66.5249 4.64980 3
-2 1 17 69.0043 4.84215 3
2 1 -17 44.3146 14.8503 1
-2 1 17 70.4464 13.8508 1
-1 -1 17 21.1940 11.2253 1
-1 -1 17 6.02704 1.49008 3
1 -1 -17 6.25656 12.6186 1
1 -1 -17 5.56983 1.42887 3
1 1 -17 4.04549 1.37421 3
1 1 -17 -4.6045 13.3371 1
-1 1 17 1.50928 10.0272 1
-1 1 17 4.16634 1.36657 3
3 -2 -17 2.23447 1.21842 3
-3 -2 17 0.52535 1.21282 3
3 2 -17 1.60077 1.04073 3
-3 2 17 0.61435 1.11616 3
-3 2 17 7.88601 10.5591 1
2 -2 -17 280.223 12.2247 3
-2 2 17 226.661 24.4961 1
-2 2 17 262.252 12.8505 3
2 2 -17 290.087 12.7477 3
-1 -2 17 1.91920 1.12365 3
1 2 -17 1.88045 1.39842 3
-1 2 17 3.33985 1.26267 3
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 33744
_shelx_res_file
;
TITL m21051 : P21/c
m21051.res
created by SHELXL-2018/3 at 09:29:10 on 20-Apr-2021
CELL 0.71073 13.3366 11.5467 7.3078 90.000 103.553 90.000
ZERR 4 0.0004 0.0003 0.0002 0.000 0.001 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H K N O S
UNIT 24 20 8 4 32 4
TEMP -183
SIZE 0.18 0.16 0.13
REM COLR colourless
REM FORM block
ACTA
L.S. 10
BOND $H
LIST 4
CONF
HTAB
REM Instructions for potential hydrogen bonds
HTAB O1 O4
EQIV $12 x, -y+1/2, z-1/2
HTAB C4 O5_$12
EQIV $7 -x+1, -y+1, -z+1
HTAB C5 O6_$7
EQIV $14 x+1, y, z
HTAB O1W O3_$14
EQIV $5 x+1, -y+1/2, z+1/2
HTAB O1W O4_$5
FMAP 2
PLAN 10
WGHT 0.025400 0.721300
EXTI 0.011581
FVAR 0.57621 0.82833
K1 3 -0.113027 0.441956 0.298171 11.00000 0.00957 0.00968 =
0.01288 -0.00086 0.00285 0.00117
K2 3 0.658509 0.372541 0.807221 11.00000 0.00967 0.01126 =
0.01074 0.00146 0.00281 0.00044
S1 6 0.394464 0.564023 0.684968 11.00000 0.00738 0.00825 =
0.00966 -0.00085 0.00215 -0.00042
O1 5 0.186893 0.055976 0.563504 11.00000 0.01167 0.00751 =
0.01686 -0.00001 0.00538 -0.00046
H1O 2 0.127786 0.066207 0.583642 11.00000 -1.50000
O2 5 0.326410 0.494480 0.503016 11.00000 0.01211 0.00885 =
0.00866 -0.00016 0.00186 -0.00273
O3 5 0.010004 0.345627 0.615466 11.00000 0.00956 0.01226 =
0.01423 0.00016 0.00376 0.00102
O4 5 0.024113 0.152419 0.614126 11.00000 0.01092 0.01118 =
0.01537 0.00088 0.00442 -0.00172
O5 5 0.326625 0.580234 0.811362 11.00000 0.01234 0.01643 =
0.01109 -0.00193 0.00478 -0.00038
O6 5 0.415000 0.669291 0.593028 11.00000 0.01469 0.00925 =
0.01601 -0.00023 0.00586 -0.00278
O7 5 0.482509 0.492414 0.760268 11.00000 0.01083 0.01386 =
0.01801 -0.00166 -0.00054 0.00330
N1 4 0.202757 0.371076 0.559029 11.00000 0.00964 0.00931 =
0.00716 -0.00060 0.00149 -0.00022
C2 1 0.166126 0.263183 0.571695 11.00000 0.00860 0.01011 =
0.00760 0.00049 0.00179 -0.00083
C3 1 0.223928 0.164677 0.552841 11.00000 0.01123 0.00824 =
0.00778 0.00002 0.00082 -0.00096
C4 1 0.322893 0.178835 0.521499 11.00000 0.01040 0.01095 =
0.01013 -0.00144 0.00226 0.00208
AFIX 43
H4 2 0.363874 0.113328 0.509029 11.00000 -1.20000
AFIX 0
C5 1 0.359838 0.289305 0.509047 11.00000 0.00872 0.01322 =
0.00957 -0.00140 0.00257 -0.00021
AFIX 43
H5 2 0.426568 0.302283 0.487955 11.00000 -1.20000
AFIX 0
C6 1 0.295426 0.381258 0.528624 11.00000 0.01085 0.00818 =
0.00701 -0.00012 0.00101 -0.00211
C7 1 0.058955 0.254535 0.604039 11.00000 0.00907 0.01288 =
0.00654 0.00019 0.00108 -0.00075
DFIX 21.000 0.010 O1W H1W O1W H2W
DFIX 21.581 0.020 H1W H2W
O1W 5 0.852624 0.302178 0.798321 11.00000 0.01129 0.01646 =
0.01814 0.00034 0.00442 0.00050
H1W 2 0.890860 0.316722 0.726202 11.00000 -1.50000
H2W 2 0.891438 0.314536 0.903347 11.00000 -1.50000
HKLF 4 1 0 0 1 0 -1 0 1 0 0
REM m21051 : P21/c
REM wR2 = 0.0555, GooF = S = 1.078, Restrained GooF = 1.078 for all data
REM R1 = 0.0204 for 2423 Fo > 4sig(Fo) and 0.0212 for all 2505 data
REM 174 parameters refined using 3 restraints
END
WGHT 0.0254 0.7213
REM Instructions for potential hydrogen bonds
HTAB O1 O4
HTAB C4 O5_$12
HTAB C5 O6_$7
HTAB O1W O3_$14
HTAB O1W O4_$5
REM Highest difference peak 0.398, deepest hole -0.437, 1-sigma level 0.061
Q1 1 0.3225 0.3336 0.5065 11.00000 0.05 0.40
Q2 1 0.1964 0.2108 0.5855 11.00000 0.05 0.40
Q3 1 0.1167 0.2574 0.5858 11.00000 0.05 0.40
Q4 1 0.3436 0.2375 0.5250 11.00000 0.05 0.37
Q5 1 0.2024 0.1163 0.5546 11.00000 0.05 0.34
Q6 1 0.2710 0.1688 0.5396 11.00000 0.05 0.31
Q7 1 0.1651 0.4189 0.5637 11.00000 0.05 0.28
Q8 1 0.4159 0.6226 0.6288 11.00000 0.05 0.28
Q9 1 0.3563 0.5191 0.5833 11.00000 0.05 0.27
Q10 1 0.1847 0.3085 0.5492 11.00000 0.05 0.26
;
_shelx_res_checksum 79416
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
_atom_site_disorder_assembly
_atom_site_disorder_group
K K1 -0.11303(2) 0.44196(2) 0.29817(4) 0.01068(9) Uani d 1 . .
K K2 0.65851(2) 0.37254(2) 0.80722(4) 0.01048(9) Uani d 1 . .
S S1 0.39446(2) 0.56402(3) 0.68497(4) 0.00841(9) Uani d 1 . .
O O1 0.18689(8) 0.05598(7) 0.56350(13) 0.01168(19) Uani d 1 . .
H H1O 0.1278(15) 0.0662(15) 0.584(3) 0.018 Uiso d 1 . .
O O2 0.32641(7) 0.49448(8) 0.50302(12) 0.00997(18) Uani d 1 . .
O O3 0.01000(7) 0.34563(8) 0.61547(13) 0.01185(19) Uani d 1 . .
O O4 0.02411(7) 0.15242(8) 0.61413(13) 0.01227(19) Uani d 1 . .
O O5 0.32663(7) 0.58023(8) 0.81136(13) 0.01295(19) Uani d 1 . .
O O6 0.41500(7) 0.66929(8) 0.59303(13) 0.01295(19) Uani d 1 . .
O O7 0.48251(7) 0.49241(8) 0.76027(14) 0.0149(2) Uani d 1 . .
N N1 0.20276(8) 0.37108(9) 0.55903(14) 0.0088(2) Uani d 1 . .
C C2 0.16613(9) 0.26318(11) 0.57169(17) 0.0088(2) Uani d 1 . .
C C3 0.22393(10) 0.16468(11) 0.55284(17) 0.0093(2) Uani d 1 . .
C C4 0.32289(10) 0.17884(11) 0.52150(17) 0.0105(2) Uani d 1 . .
H H4 0.363874 0.113328 0.509029 0.013 Uiso calc 1 . .
C C5 0.35984(9) 0.28931(11) 0.50905(17) 0.0104(2) Uani d 1 . .
H H5 0.426568 0.302283 0.487955 0.013 Uiso calc 1 . .
C C6 0.29543(10) 0.38126(10) 0.52862(17) 0.0089(2) Uani d 1 . .
C C7 0.05895(9) 0.25453(11) 0.60404(17) 0.0096(2) Uani d 1 . .
O O1W 0.85262(7) 0.30218(9) 0.79832(14) 0.0151(2) Uani d 1 . .
H H1W 0.8909(13) 0.3167(17) 0.726(2) 0.023 Uiso d 1 . .
H H2W 0.8914(13) 0.3145(17) 0.903(2) 0.023 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
K1 0.00957(14) 0.00968(14) 0.01288(14) 0.00117(9) 0.00285(10) -0.00086(9)
K2 0.00967(14) 0.01126(14) 0.01074(14) 0.00044(9) 0.00281(10) 0.00146(9)
S1 0.00738(15) 0.00825(15) 0.00966(15) -0.00042(10) 0.00215(11) -0.00085(10)
O1 0.0117(5) 0.0075(4) 0.0169(5) -0.0005(3) 0.0054(4) 0.0000(3)
O2 0.0121(4) 0.0089(4) 0.0087(4) -0.0027(3) 0.0019(3) -0.0002(3)
O3 0.0096(4) 0.0123(4) 0.0142(4) 0.0010(3) 0.0038(3) 0.0002(3)
O4 0.0109(4) 0.0112(4) 0.0154(4) -0.0017(3) 0.0044(3) 0.0009(3)
O5 0.0123(4) 0.0164(5) 0.0111(4) -0.0004(4) 0.0048(3) -0.0019(4)
O6 0.0147(5) 0.0093(4) 0.0160(4) -0.0028(3) 0.0059(4) -0.0002(3)
O7 0.0108(4) 0.0139(4) 0.0180(5) 0.0033(3) -0.0005(4) -0.0017(4)
N1 0.0096(5) 0.0093(5) 0.0072(5) -0.0002(4) 0.0015(4) -0.0006(4)
C2 0.0086(5) 0.0101(6) 0.0076(5) -0.0008(4) 0.0018(4) 0.0005(4)
C3 0.0112(6) 0.0082(6) 0.0078(5) -0.0010(4) 0.0008(4) 0.0000(4)
C4 0.0104(6) 0.0109(6) 0.0101(6) 0.0021(4) 0.0023(4) -0.0014(4)
C5 0.0087(5) 0.0132(6) 0.0096(5) -0.0002(5) 0.0026(4) -0.0014(4)
C6 0.0108(6) 0.0082(5) 0.0070(5) -0.0021(4) 0.0010(4) -0.0001(4)
C7 0.0091(6) 0.0129(6) 0.0065(5) -0.0007(4) 0.0011(4) 0.0002(4)
O1W 0.0113(5) 0.0165(5) 0.0181(5) 0.0005(4) 0.0044(4) 0.0003(4)
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
O4 K1 O3 4_565 . 85.28(3) ?
O4 K1 O5 4_565 3_566 125.34(3) ?
O3 K1 O5 . 3_566 125.08(3) ?
O4 K1 N1 4_565 3_566 152.53(3) ?
O3 K1 N1 . 3_566 102.82(3) ?
O5 K1 N1 3_566 3_566 71.26(3) ?
O4 K1 O3 4_565 3_566 96.31(3) ?
O3 K1 O3 . 3_566 90.00(3) ?
O5 K1 O3 3_566 3_566 123.94(3) ?
N1 K1 O3 3_566 3_566 58.00(3) ?
O4 K1 O1W 4_565 4_465 74.51(3) ?
O3 K1 O1W . 4_465 70.34(3) ?
O5 K1 O1W 3_566 4_465 75.87(3) ?
N1 K1 O1W 3_566 4_465 132.96(3) ?
O3 K1 O1W 3_566 4_465 158.67(3) ?
O4 K1 O1 4_565 2 81.77(3) ?
O3 K1 O1 . 2 163.61(3) ?
O5 K1 O1 3_566 2 71.02(3) ?
N1 K1 O1 3_566 2 84.60(3) ?
O3 K1 O1 3_566 2 81.53(3) ?
O1W K1 O1 4_465 2 115.26(3) ?
O4 K1 S1 4_565 3_566 142.24(2) ?
O3 K1 S1 . 3_566 111.50(2) ?
O5 K1 S1 3_566 3_566 18.571(19) ?
N1 K1 S1 3_566 3_566 59.06(2) ?
O3 K1 S1 3_566 3_566 116.43(2) ?
O1W K1 S1 4_465 3_566 79.72(2) ?
O1 K1 S1 2 3_566 84.87(2) ?
O4 K1 K1 4_565 3_566 91.22(2) ?
O3 K1 K1 . 3_566 45.69(2) ?
O5 K1 K1 3_566 3_566 143.23(2) ?
N1 K1 K1 3_566 3_566 77.04(2) ?
O3 K1 K1 3_566 3_566 44.305(19) ?
O1W K1 K1 4_465 3_566 115.57(2) ?
O1 K1 K1 2 3_566 124.38(2) ?
S1 K1 K1 3_566 3_566 125.061(11) ?
O4 K1 K2 4_565 1_454 86.50(2) ?
O3 K1 K2 . 1_454 144.54(2) ?
O5 K1 K2 3_566 1_454 41.328(19) ?
N1 K1 K2 3_566 1_454 100.27(2) ?
O3 K1 K2 3_566 1_454 125.21(2) ?
O1W K1 K2 4_465 1_454 74.21(2) ?
O1 K1 K2 2 1_454 44.587(19) ?
S1 K1 K2 3_566 1_454 59.892(7) ?
K1 K1 K2 3_566 1_454 168.952(12) ?
O4 K1 K2 4_565 4_465 101.95(2) ?
O3 K1 K2 . 4_465 86.38(2) ?
O5 K1 K2 3_566 4_465 46.95(2) ?
N1 K1 K2 3_566 4_465 104.70(2) ?
O3 K1 K2 3_566 4_465 161.00(2) ?
O1W K1 K2 4_465 4_465 30.91(2) ?
O1 K1 K2 2 4_465 106.07(2) ?
S1 K1 K2 3_566 4_465 48.809(6) ?
K1 K1 K2 3_566 4_465 129.234(11) ?
K2 K1 K2 1_454 4_465 61.786(6) ?
O7 K2 O6 . 2_646 96.93(3) ?
O7 K2 O1W . . 163.59(3) ?
O6 K2 O1W 2_646 . 98.84(3) ?
O7 K2 O2 . 3_666 80.73(3) ?
O6 K2 O2 2_646 3_666 142.83(3) ?
O1W K2 O2 . 3_666 83.96(3) ?
O7 K2 O5 . 3_667 83.24(3) ?
O6 K2 O5 2_646 3_667 81.17(3) ?
O1W K2 O5 . 3_667 103.61(3) ?
O2 K2 O5 3_666 3_667 134.52(3) ?
O7 K2 O6 . 3_666 82.98(3) ?
O6 K2 O6 2_646 3_666 93.96(2) ?
O1W K2 O6 . 3_666 91.42(3) ?
O2 K2 O6 3_666 3_666 48.87(3) ?
O5 K2 O6 3_667 3_666 164.72(3) ?
O7 K2 O1 . 2_656 101.29(3) ?
O6 K2 O1 2_646 2_656 143.63(3) ?
O1W K2 O1 . 2_656 68.03(3) ?
O2 K2 O1 3_666 2_656 71.74(3) ?
O5 K2 O1 3_667 2_656 70.16(3) ?
O6 K2 O1 3_666 2_656 119.21(3) ?
O7 K2 S1 . 3_666 78.73(2) ?
O6 K2 S1 2_646 3_666 116.72(2) ?
O1W K2 S1 . 3_666 90.11(2) ?
O2 K2 S1 3_666 3_666 26.201(18) ?
O5 K2 S1 3_667 3_666 155.84(2) ?
O6 K2 S1 3_666 3_666 22.895(18) ?
O1 K2 S1 2_656 3_666 97.67(2) ?
O7 K2 S1 . 2_646 109.94(2) ?
O6 K2 S1 2_646 2_646 20.38(2) ?
O1W K2 S1 . 2_646 84.12(2) ?
O2 K2 S1 3_666 2_646 127.21(2) ?
O5 K2 S1 3_667 2_646 98.27(2) ?
O6 K2 S1 3_666 2_646 80.302(19) ?
O1 K2 S1 2_656 2_646 145.27(2) ?
S1 K2 S1 3_666 2_646 102.902(10) ?
O7 K2 K1 . 1_656 116.69(2) ?
O6 K2 K1 2_646 1_656 99.86(2) ?
O1W K2 K1 . 1_656 64.86(2) ?
O2 K2 K1 3_666 1_656 114.43(2) ?
O5 K2 K1 3_667 1_656 41.02(2) ?
O6 K2 K1 3_666 1_656 154.00(2) ?
O1 K2 K1 2_656 1_656 43.784(19) ?
S1 K2 K1 3_666 1_656 138.793(10) ?
S1 K2 K1 2_646 1_656 106.147(8) ?
O7 K2 K2 . 4_565 112.19(2) ?
O6 K2 K2 2_646 4_565 75.48(2) ?
O1W K2 K2 . 4_565 67.86(2) ?
O2 K2 K2 3_666 4_565 71.370(18) ?
O5 K2 K2 3_667 4_565 153.22(2) ?
O6 K2 K2 3_666 4_565 33.178(19) ?
O1 K2 K2 2_656 4_565 124.254(19) ?
S1 K2 K2 3_666 4_565 50.703(5) ?
S1 K2 K2 2_646 4_565 56.517(8) ?
K1 K2 K2 1_656 4_565 131.084(6) ?
O7 K2 K2 . 4_566 104.80(2) ?
O6 K2 K2 2_646 4_566 35.86(2) ?
O1W K2 K2 . 4_566 90.71(2) ?
O2 K2 K2 3_666 4_566 174.19(2) ?
O5 K2 K2 3_667 4_566 49.13(2) ?
O6 K2 K2 3_666 4_566 129.27(2) ?
O1 K2 K2 2_656 4_566 108.403(19) ?
S1 K2 K2 3_666 4_566 152.157(10) ?
S1 K2 K2 2_646 4_566 49.568(8) ?
K1 K2 K2 1_656 4_566 64.932(5) ?
K2 K2 K2 4_565 4_566 104.485(11) ?
O7 S1 O6 . . 115.80(6) ?
O7 S1 O5 . . 114.01(6) ?
O6 S1 O5 . . 113.72(6) ?
O7 S1 O2 . . 106.09(5) ?
O6 S1 O2 . . 99.47(5) ?
O5 S1 O2 . . 105.75(5) ?
O7 S1 K2 . 3_666 117.03(4) ?
O6 S1 K2 . 3_666 51.28(4) ?
O5 S1 K2 . 3_666 127.54(4) ?
O2 S1 K2 . 3_666 48.78(3) ?
O7 S1 K2 . 2_656 134.65(4) ?
O6 S1 K2 . 2_656 40.71(4) ?
O5 S1 K2 . 2_656 73.18(4) ?
O2 S1 K2 . 2_656 114.92(3) ?
K2 S1 K2 3_666 2_656 79.729(8) ?
O7 S1 K1 . 3_566 134.83(4) ?
O6 S1 K1 . 3_566 109.13(4) ?
O5 S1 K1 . 3_566 37.75(4) ?
O2 S1 K1 . 3_566 69.61(3) ?
K2 S1 K1 3_666 3_566 94.176(9) ?
K2 S1 K1 2_656 3_566 79.600(8) ?
C3 O1 K1 . 2_545 114.60(7) ?
C3 O1 K2 . 2_646 116.45(7) ?
K1 O1 K2 2_545 2_646 91.63(3) ?
C3 O1 H1O . . 104.4(12) ?
K1 O1 H1O 2_545 . 95.2(12) ?
K2 O1 H1O 2_646 . 131.0(12) ?
C6 O2 S1 . . 118.44(7) ?
C6 O2 K2 . 3_666 134.86(7) ?
S1 O2 K2 . 3_666 105.02(4) ?
C7 O3 K1 . . 120.18(8) ?
C7 O3 K1 . 3_566 120.90(8) ?
K1 O3 K1 . 3_566 90.00(3) ?
C7 O4 K1 . 4_566 133.68(8) ?
S1 O5 K1 . 3_566 123.68(5) ?
S1 O5 K2 . 3_667 138.63(5) ?
K1 O5 K2 3_566 3_667 97.65(3) ?
S1 O6 K2 . 2_656 118.92(5) ?
S1 O6 K2 . 3_666 105.82(5) ?
K2 O6 K2 2_656 3_666 110.96(3) ?
S1 O7 K2 . . 163.84(6) ?
C6 N1 C2 . . 117.72(11) ?
C6 N1 K1 . 3_566 119.90(8) ?
C2 N1 K1 . 3_566 119.70(8) ?
N1 C2 C3 . . 121.82(11) ?
N1 C2 C7 . . 116.38(11) ?
C3 C2 C7 . . 121.79(11) ?
O1 C3 C2 . . 121.99(11) ?
O1 C3 C4 . . 119.11(11) ?
C2 C3 C4 . . 118.90(11) ?
C5 C4 C3 . . 118.94(11) ?
C5 C4 H4 . . 120.5 ?
C3 C4 H4 . . 120.5 ?
C4 C5 C6 . . 117.37(11) ?
C4 C5 H5 . . 121.3 ?
C6 C5 H5 . . 121.3 ?
N1 C6 C5 . . 125.24(11) ?
N1 C6 O2 . . 115.26(11) ?
C5 C6 O2 . . 119.36(11) ?
O3 C7 O4 . . 124.78(11) ?
O3 C7 C2 . . 118.96(11) ?
O4 C7 C2 . . 116.25(11) ?
K2 O1W K1 . 4_666 116.56(4) ?
K2 O1W H1W . . 132.9(13) ?
K1 O1W H1W 4_666 . 94.4(14) ?
K2 O1W H2W . . 108.4(13) ?
K1 O1W H2W 4_666 . 96.0(14) ?
H1W O1W H2W . . 102.0(15) ?
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
K1 O4 4_565 2.7376(9) ?
K1 O3 . 2.7428(10) ?
K1 O5 3_566 2.7843(10) ?
K1 N1 3_566 2.7869(11) ?
K1 O3 3_566 2.8099(10) ?
K1 O1W 4_465 2.8560(10) ?
K1 O1 2 2.9102(10) ?
K1 S1 3_566 3.7848(4) ?
K1 K1 3_566 3.9268(5) ?
K1 K2 1_454 4.2041(4) ?
K1 K2 4_465 4.7508(4) ?
K2 O7 . 2.6769(9) ?
K2 O6 2_646 2.7084(10) ?
K2 O1W . 2.7286(10) ?
K2 O2 3_666 2.7842(9) ?
K2 O5 3_667 2.8012(9) ?
K2 O6 3_666 2.8993(10) ?
K2 O1 2_656 2.9525(10) ?
K2 S1 3_666 3.5751(4) ?
K2 S1 2_646 3.6348(4) ?
K2 K2 4_565 4.6216(3) ?
K2 K2 4_566 4.6216(3) ?
S1 O7 . 1.4361(9) ?
S1 O6 . 1.4457(9) ?
S1 O5 . 1.4486(9) ?
S1 O2 . 1.6343(9) ?
O1 C3 . 1.3577(15) ?
O1 H1O . 0.843(19) ?
O2 C6 . 1.3968(14) ?
O3 C7 . 1.2510(16) ?
O4 C7 . 1.2758(16) ?
N1 C6 . 1.3112(16) ?
N1 C2 . 1.3492(16) ?
C2 C3 . 1.3988(17) ?
C2 C7 . 1.5057(17) ?
C3 C4 . 1.4010(17) ?
C4 C5 . 1.3781(18) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.3940(17) ?
C5 H5 . 0.9500 ?
O1W H1W . 0.832(15) ?
O1W H2W . 0.831(15) ?
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 H1O O4 . 0.843(19) 1.760(19) 2.5429(13) 153.6(17) yes
C4 H4 O5 4_565 0.95 2.64 3.3682(16) 133 yes
C5 H5 O6 3_666 0.95 2.35 3.2943(15) 175 yes
O1W H1W O3 1_655 0.832(15) 1.973(15) 2.7852(13) 165.0(17) yes
O1W H2W O4 4_666 0.831(15) 2.091(15) 2.8910(14) 161.4(17) 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
O7 S1 O2 C6 . . . . 55.28(10) ?
O6 S1 O2 C6 . . . . 175.77(9) ?
O5 S1 O2 C6 . . . . -66.14(10) ?
K2 S1 O2 C6 3_666 . . . 167.38(11) ?
K2 S1 O2 C6 2_656 . . . -144.57(8) ?
K1 S1 O2 C6 3_566 . . . -77.22(8) ?
O7 S1 O2 K2 . . . 3_666 -112.10(5) ?
O6 S1 O2 K2 . . . 3_666 8.39(5) ?
O5 S1 O2 K2 . . . 3_666 126.48(5) ?
K2 S1 O2 K2 2_656 . . 3_666 48.05(4) ?
K1 S1 O2 K2 3_566 . . 3_666 115.40(3) ?
O7 S1 O5 K1 . . . 3_566 -133.28(6) ?
O6 S1 O5 K1 . . . 3_566 90.99(7) ?
O2 S1 O5 K1 . . . 3_566 -17.12(7) ?
K2 S1 O5 K1 3_666 . . 3_566 32.58(8) ?
K2 S1 O5 K1 2_656 . . 3_566 94.73(5) ?
O7 S1 O5 K2 . . . 3_667 43.85(10) ?
O6 S1 O5 K2 . . . 3_667 -91.88(9) ?
O2 S1 O5 K2 . . . 3_667 160.01(7) ?
K2 S1 O5 K2 3_666 . . 3_667 -150.29(5) ?
K2 S1 O5 K2 2_656 . . 3_667 -88.14(7) ?
K1 S1 O5 K2 3_566 . . 3_667 177.13(12) ?
O7 S1 O6 K2 . . . 2_656 -129.41(6) ?
O5 S1 O6 K2 . . . 2_656 5.50(8) ?
O2 S1 O6 K2 . . . 2_656 117.46(5) ?
K2 S1 O6 K2 3_666 . . 2_656 125.55(7) ?
K1 S1 O6 K2 3_566 . . 2_656 45.88(6) ?
O7 S1 O6 K2 . . . 3_666 105.04(6) ?
O5 S1 O6 K2 . . . 3_666 -120.05(5) ?
O2 S1 O6 K2 . . . 3_666 -8.09(5) ?
K2 S1 O6 K2 2_656 . . 3_666 -125.55(7) ?
K1 S1 O6 K2 3_566 . . 3_666 -79.67(4) ?
O6 S1 O7 K2 . . . . -44.2(2) ?
O5 S1 O7 K2 . . . . -179.00(19) ?
O2 S1 O7 K2 . . . . 65.0(2) ?
K2 S1 O7 K2 3_666 . . . 13.6(2) ?
K2 S1 O7 K2 2_656 . . . -89.3(2) ?
K1 S1 O7 K2 3_566 . . . 142.06(18) ?
C6 N1 C2 C3 . . . . -0.18(17) ?
K1 N1 C2 C3 3_566 . . . -161.62(9) ?
C6 N1 C2 C7 . . . . -179.20(10) ?
K1 N1 C2 C7 3_566 . . . 19.36(14) ?
K1 O1 C3 C2 2_545 . . . 101.95(11) ?
K2 O1 C3 C2 2_646 . . . -152.82(9) ?
K1 O1 C3 C4 2_545 . . . -77.87(12) ?
K2 O1 C3 C4 2_646 . . . 27.36(14) ?
N1 C2 C3 O1 . . . . -179.28(11) ?
C7 C2 C3 O1 . . . . -0.31(18) ?
N1 C2 C3 C4 . . . . 0.54(18) ?
C7 C2 C3 C4 . . . . 179.51(11) ?
O1 C3 C4 C5 . . . . 179.41(11) ?
C2 C3 C4 C5 . . . . -0.41(18) ?
C3 C4 C5 C6 . . . . -0.03(18) ?
C2 N1 C6 C5 . . . . -0.32(18) ?
K1 N1 C6 C5 3_566 . . . 161.09(9) ?
C2 N1 C6 O2 . . . . 175.49(10) ?
K1 N1 C6 O2 3_566 . . . -23.10(13) ?
C4 C5 C6 N1 . . . . 0.42(19) ?
C4 C5 C6 O2 . . . . -175.23(11) ?
S1 O2 C6 N1 . . . . 94.96(11) ?
K2 O2 C6 N1 3_666 . . . -102.36(12) ?
S1 O2 C6 C5 . . . . -88.96(12) ?
K2 O2 C6 C5 3_666 . . . 73.72(14) ?
K1 O3 C7 O4 . . . . -88.64(13) ?
K1 O3 C7 O4 3_566 . . . 160.99(9) ?
K1 O3 C7 C2 . . . . 89.91(11) ?
K1 O3 C7 C2 3_566 . . . -20.46(14) ?
K1 O4 C7 O3 4_566 . . . -30.63(18) ?
K1 O4 C7 C2 4_566 . . . 150.78(8) ?
N1 C2 C7 O3 . . . . 0.67(17) ?
C3 C2 C7 O3 . . . . -178.36(11) ?
N1 C2 C7 O4 . . . . 179.34(10) ?
C3 C2 C7 O4 . . . . 0.31(17) ?
_cod_database_fobs_code 2243831