#------------------------------------------------------------------------------
#$Date: 2021-05-15 07:50:02 +0300 (Sat, 15 May 2021) $
#$Revision: 265246 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243832.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_2243832
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 'C6 H5 N O4'
_chemical_formula_moiety 'C6 H5 N O4'
_chemical_formula_sum 'C6 H5 N O4'
_chemical_formula_weight 155.11
_chemical_name_common
;
3,6-Dihydroxypicolinic acid
;
_chemical_name_systematic
;
3-Hydroxy-6-oxo-1,6-dihydropyridine-2-carboxylic acid
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 39
_space_group_name_Hall 'A 2 -2b'
_space_group_name_H-M_alt 'A e m 2'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.2045(6)
_cell_length_b 6.1282(4)
_cell_length_c 9.7293(6)
_cell_measurement_reflns_used 3820
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 78.48
_cell_measurement_theta_min 4.33
_cell_volume 608.42(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0246
_diffrn_reflns_av_unetI/netI 0.0201
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 4025
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 77.820
_diffrn_reflns_theta_min 4.332
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 1.270
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.799
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.693
_exptl_crystal_description plate
_exptl_crystal_F_000 320
_exptl_crystal_size_max 0.140
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.020
_refine_diff_density_max 0.202
_refine_diff_density_min -0.251
_refine_ls_abs_structure_details
;
Refined as a perfect inversion twin
;
_refine_ls_abs_structure_Flack 0.5
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.109
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 74
_refine_ls_number_reflns 700
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.105
_refine_ls_R_factor_all 0.0246
_refine_ls_R_factor_gt 0.0243
_refine_ls_shift/su_max 0.024
_refine_ls_shift/su_mean 0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0669
_refine_ls_wR_factor_ref 0.0675
_reflns_number_gt 690
_reflns_number_total 700
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7975sup1.cif
_cod_data_source_block II
_cod_original_sg_symbol_Hall 'A 2 -2c'
_cod_original_sg_symbol_H-M 'A b m 2'
_cod_database_code 2243832
_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 0.842
_shelx_estimated_absorpt_t_max 0.975
_shelx_hkl_file
;
2 0 0 1368.44 44.8697 1
-2 0 0 1344.44 44.1667 1
4 0 0 635.518 19.3463 4
4 0 0 606.671 19.9500 10
-4 0 0 676.825 21.0432 4
-6 0 0 1874.75 61.2252 16
-6 0 0 1994.08 59.7502 4
6 0 0 1812.45 58.3491 16
6 0 0 1872.78 57.1852 4
6 0 0 1873.53 57.8151 10
-8 0 0 193.498 8.06690 3
-8 0 0 193.546 6.81748 4
-8 0 0 197.538 7.81069 7
8 0 0 188.814 8.02361 3
-8 0 0 204.985 8.78860 16
8 0 0 186.290 7.58268 10
8 0 0 204.900 8.32296 16
10 0 0 55.2102 3.56009 16
-10 0 0 55.3966 3.19532 7
-10 0 0 55.6875 4.03663 16
10 0 0 55.3906 3.49587 3
-10 0 0 55.9279 3.35070 3
12 0 0 3.21270 0.83527 3
1 1 0 0.39650 0.24222 4
1 -1 0 0.09341 0.23883 10
1 -1 0 0.17248 0.18231 4
-1 -1 0 0.17910 0.17318 4
-1 -1 0 0.05630 0.20662 10
-1 1 0 0.20065 0.20825 4
3 -1 0 0.07380 0.40385 10
3 1 0 -0.3814 0.37033 10
3 -1 0 -0.1894 0.32114 4
-3 1 0 -0.0348 0.30980 4
3 1 0 0.57617 0.43109 4
-3 -1 0 -0.2478 0.24634 4
5 1 0 1.35414 0.89625 16
5 1 0 -0.0320 0.40599 10
-5 -1 0 0.34176 0.36318 4
5 1 0 -0.0757 0.52035 4
-5 1 0 1.33570 0.46001 4
5 -1 0 0.03408 0.38841 4
5 -1 0 -0.0376 0.49057 10
5 -1 0 -0.2172 0.70714 16
-5 1 0 1.02572 0.94857 16
7 -1 0 0.09630 0.79618 16
-7 -1 0 -1.1271 0.48299 4
7 -1 0 0.83553 0.91285 10
-7 -1 0 -1.4302 1.00101 7
7 1 0 -0.2148 0.54739 4
7 1 0 0.43602 0.66554 10
-7 1 0 1.21657 1.19418 7
-7 1 0 -0.0841 1.09419 16
7 -1 0 3.01565 1.38377 3
7 1 0 0.54425 0.92275 16
9 -1 0 -0.4611 1.13883 3
-9 1 0 1.05628 1.22242 3
-9 -1 0 -0.8618 0.91757 7
9 1 0 0.38381 0.98539 16
-9 1 0 1.12887 1.83337 16
-9 -1 0 1.88235 1.63068 16
9 -1 0 0.14931 0.86639 16
-9 1 0 0.64733 1.33110 7
-9 -1 0 0.65088 1.32079 3
-11 1 0 -0.8448 0.60818 7
11 -1 0 -0.5989 0.83630 3
-11 -1 0 0.37188 0.75211 3
11 1 0 0.74753 0.85705 3
-11 -1 0 -0.0379 0.73628 7
11 1 0 0.20789 0.80460 16
-11 -1 0 -0.9103 1.04718 16
-2 2 0 794.158 25.0632 4
2 -2 0 783.054 25.0027 10
-2 -2 0 802.180 24.1464 4
2 2 0 794.327 24.1086 4
-2 -2 0 782.055 24.3933 10
4 -2 0 376.847 12.6137 10
-4 -2 0 390.435 12.6382 10
4 2 0 387.744 12.1177 4
-4 -2 0 389.538 12.2931 4
-4 2 0 408.536 12.8084 4
-6 -2 0 1301.03 40.3050 10
-6 2 0 1308.82 40.5020 4
6 2 0 1287.00 38.9724 4
6 -2 0 1207.25 39.8214 10
-6 -2 0 1260.90 39.6631 4
6 2 0 1261.47 40.5267 16
8 2 0 168.639 7.54832 16
-8 -2 0 186.301 8.28234 16
8 2 0 153.504 5.81909 4
-8 2 0 171.719 8.11409 16
10 -2 0 48.3608 2.95488 3
-10 2 0 50.7620 3.56062 16
10 2 0 54.9269 3.85918 16
-10 2 0 50.9851 2.88839 7
-10 -2 0 54.0058 4.07253 16
10 2 0 42.3797 3.02210 3
-10 -2 0 48.8650 3.11573 3
1 -3 0 0.16791 0.44436 10
-1 -3 0 0.38752 0.32740 10
-1 3 0 0.32507 0.34989 4
1 3 0 0.06810 0.39712 4
-3 -3 0 0.56477 0.46263 10
-3 3 0 -0.0449 0.45347 4
3 -3 0 -1.1125 0.57698 10
3 3 0 0.43136 0.47929 4
5 3 0 -0.8414 1.10477 16
-5 3 0 1.48195 0.66943 4
-5 -3 0 1.64415 0.74933 10
5 3 0 0.20577 0.64968 4
-7 -3 0 -0.2585 1.25587 7
7 -3 0 3.22855 1.23461 6
-7 3 0 2.58218 1.12846 4
-7 3 0 6.01519 1.95975 16
7 3 0 0.57433 0.75063 4
7 3 0 7.18761 2.25693 16
7 3 0 1.65751 1.73696 3
9 -3 0 0.08332 0.94113 3
-9 3 0 0.90809 0.96009 7
9 3 0 -1.3569 1.02521 16
-9 3 0 0.62832 1.58907 16
-9 -3 0 -0.5801 0.98460 3
-9 -3 0 0.54412 1.23389 16
9 3 0 0.81518 1.26659 3
11 -3 0 0.38055 0.48732 13
11 -3 0 0.15950 0.45440 3
-11 3 0 -0.3397 0.56509 7
-11 -3 0 -0.5933 0.52183 3
0 4 0 9999.99 306.422 4
2 4 0 217.154 7.46049 4
-2 4 0 216.749 7.37522 4
4 -4 0 160.945 7.72384 12
4 4 0 138.480 5.26227 4
4 4 0 133.430 6.70834 16
-4 -4 0 155.338 6.71049 6
-4 -4 0 142.705 7.20546 12
4 -4 0 135.797 5.59320 13
-4 4 0 163.916 6.15964 4
4 -4 0 147.008 9.76326 14
6 -4 0 453.854 16.1425 15
6 -4 0 479.586 16.3223 3
-6 4 0 525.279 17.3651 7
6 4 0 510.819 17.6664 16
-6 -4 0 514.488 17.4942 3
-6 -4 0 479.435 18.1185 12
-8 -4 0 106.265 5.21589 16
-8 4 0 113.512 4.83178 7
-8 -4 0 111.149 5.46320 11
8 -4 0 105.673 4.43026 3
-8 -4 0 102.805 4.88919 3
8 -4 0 102.248 5.24265 12
10 -4 0 37.5929 1.91044 13
10 -4 0 39.5225 1.72757 3
10 -4 0 41.5508 2.23369 12
-1 5 0 -0.0278 0.78221 4
1 5 0 0.93628 0.96858 7
-1 -5 0 0.80442 1.95864 14
-1 5 0 -0.2316 1.17971 7
-1 -5 0 -0.0144 1.36223 13
1 5 0 0.30250 0.76434 4
1 -5 0 1.30478 0.83801 6
1 -5 0 0.22513 1.19132 15
-1 -5 0 -1.5422 1.15113 3
-1 -5 0 -0.6946 0.99943 6
1 -5 0 0.40665 1.86126 14
1 -5 0 -0.5772 0.87572 3
1 -5 0 0.27119 0.89584 13
-1 -5 0 0.16545 1.16263 5
1 -5 0 1.53791 0.93554 5
3 -5 0 0.67241 0.99890 6
-3 -5 0 0.12792 1.73549 14
3 5 0 -0.2833 1.09052 4
3 -5 0 0.05569 1.67420 15
3 -5 0 -0.6557 1.53251 14
3 -5 0 1.40436 1.02913 13
5 -5 0 -0.1645 1.42693 14
5 -5 0 0.77383 0.83061 3
-5 5 0 0.39183 0.98229 7
5 -5 0 -0.5727 0.93898 15
5 -5 0 0.66465 0.73881 13
-5 -5 0 0.96328 1.00493 3
-7 5 0 -0.4658 0.74908 7
7 -5 0 -0.3841 0.71815 3
-7 -5 0 0.00233 0.90983 16
-7 -5 0 1.37780 1.00014 11
7 -5 0 0.04749 1.11948 13
9 -5 0 -0.0081 0.52827 5
-9 5 0 0.36368 0.46978 7
-9 -5 0 0.86570 0.54941 3
0 -6 0 2767.86 87.3292 5
0 6 0 2777.78 87.1294 7
0 -6 0 2748.63 85.6562 3
0 -6 0 2754.28 87.1123 6
0 -6 0 2830.06 90.7745 14
2 -6 0 40.7119 2.33147 6
2 -6 0 46.6540 3.09341 12
-2 -6 0 47.0192 2.49055 5
4 -6 0 65.2074 3.02017 3
-4 -6 0 70.6358 3.40179 3
4 -6 0 63.3173 3.25300 5
4 -6 0 63.1252 5.36059 14
-4 6 0 68.9556 3.54675 7
4 -6 0 66.0194 3.80742 12
-6 -6 0 168.655 7.08513 11
-6 6 0 184.406 6.58021 7
6 -6 0 173.879 6.19545 5
6 -6 0 167.580 6.21754 12
-6 -6 0 187.121 6.35894 3
1 -7 0 0.50568 0.65283 5
-1 -7 0 1.04783 0.95553 11
-1 7 0 0.16812 0.64576 7
-3 -7 0 -0.5957 0.89040 11
3 -7 0 0.16766 0.71353 5
5 -7 0 -0.9072 0.56960 5
-5 -7 0 0.54105 0.47555 11
0 0 -1 1444.30 44.0326 1
0 0 1 1387.55 43.9646 1
-2 0 1 715.042 21.7462 4
2 0 -1 702.768 21.8808 10
2 0 1 731.135 22.2110 4
2 0 1 714.674 22.3860 10
-2 0 -1 714.817 22.2943 4
-4 0 -1 145.081 4.86574 4
-4 0 1 146.073 4.76374 4
4 0 -1 134.130 4.49299 4
4 0 -1 132.591 4.71393 10
4 0 1 133.257 4.74427 10
4 0 1 135.834 4.42247 4
6 0 1 394.981 12.5565 4
6 0 -1 386.719 13.7968 16
-6 0 1 438.408 13.4986 4
-6 0 -1 432.634 13.6941 4
6 0 -1 404.906 12.7285 4
6 0 1 387.282 14.0754 16
6 0 -1 401.028 13.2370 10
6 0 1 404.741 13.2732 10
-6 0 1 401.976 14.8643 16
-8 0 -1 27.8631 2.52770 7
8 0 -1 23.7118 2.30190 10
-8 0 1 25.9295 2.28577 7
8 0 -1 27.6110 1.67189 4
-8 0 1 25.2801 1.54884 4
8 0 1 27.7631 2.59417 3
-8 0 1 25.3641 2.50349 3
8 0 1 26.5004 2.62250 16
-8 0 -1 26.2351 3.17595 3
8 0 -1 26.2882 2.62261 16
-8 0 -1 28.6482 2.98947 16
8 0 -1 27.9853 2.58057 3
-8 0 1 27.5172 2.97984 16
-8 0 -1 27.9402 1.66461 4
-10 0 1 118.230 4.97288 7
10 0 -1 107.079 5.23914 3
10 0 1 114.776 5.39131 3
-10 0 1 118.834 5.15759 3
-10 0 -1 108.212 5.27519 3
-10 0 -1 118.147 5.22032 7
10 0 1 122.971 5.34959 16
10 0 -1 114.093 5.57192 16
-10 0 1 119.356 5.87416 16
-10 0 -1 113.536 6.07548 16
12 0 1 36.4343 1.76565 3
12 0 -1 35.3498 1.79607 3
1 -1 1 2359.77 72.3766 10
3 1 -1 324.647 9.91067 4
3 1 -1 330.029 10.1131 10
3 -1 1 328.814 10.4742 10
-3 1 -1 335.200 10.7375 4
3 -1 -1 326.891 10.1846 10
3 1 1 282.019 10.7495 4
-3 -1 1 333.544 10.1625 4
-5 1 1 2039.75 67.9837 16
5 1 -1 1982.92 67.5601 16
-5 -1 -1 2209.51 66.3805 4
-5 1 1 2203.19 66.8838 4
5 1 -1 2124.69 64.0741 4
5 -1 1 2102.52 65.9090 10
5 1 -1 2150.85 64.4775 10
5 -1 1 2071.30 66.3080 16
5 1 1 1998.16 65.2642 16
5 -1 -1 2057.34 65.3595 16
-5 1 -1 2216.46 68.0567 4
5 -1 -1 2175.55 64.4665 4
5 1 1 2161.17 64.0219 4
-5 -1 1 2190.38 66.2006 4
5 -1 -1 2101.15 64.9338 10
5 1 1 2138.83 64.4667 10
-7 1 1 478.662 16.6180 7
7 -1 1 449.759 15.7182 10
-7 -1 -1 493.017 16.9000 7
7 1 -1 463.074 15.5551 10
7 -1 1 474.093 16.0190 16
7 -1 1 495.432 16.5112 3
-7 1 1 482.215 17.0960 16
7 1 -1 469.161 16.4520 16
7 -1 1 449.382 15.9611 8
7 -1 -1 438.163 16.1881 3
7 1 1 449.216 14.7683 4
-7 -1 1 485.069 17.1423 16
-7 1 -1 499.421 16.9127 7
-7 1 -1 460.587 17.1283 16
7 -1 -1 452.576 14.6045 4
7 -1 -1 450.847 15.7981 10
7 -1 -1 463.711 16.0766 16
7 1 1 492.421 17.0149 3
-7 -1 1 459.388 16.4431 3
7 1 1 476.092 16.4131 16
-7 -1 1 466.101 14.9817 4
-9 -1 -1 896.325 28.6382 7
-9 -1 -1 885.673 29.0240 3
-9 -1 -1 773.793 30.6457 16
-9 1 1 886.182 30.9376 16
9 -1 1 897.094 28.0503 16
-9 1 1 886.614 28.5181 7
9 1 -1 726.750 28.8435 16
9 1 -1 833.419 28.0148 3
9 -1 1 865.973 27.9848 3
-9 1 1 867.397 28.6528 3
-9 -1 1 851.975 28.1477 7
9 1 1 868.375 28.4923 16
9 1 1 854.058 28.2105 3
9 -1 -1 857.907 28.0323 3
-9 -1 1 889.571 28.8174 3
-9 -1 1 902.428 29.7160 16
-9 1 -1 889.123 28.7700 7
11 1 -1 14.7952 1.68248 3
11 -1 1 19.6324 1.62172 3
-11 -1 -1 16.2191 1.64178 3
11 -1 1 14.4609 2.11543 6
-11 -1 -1 15.3674 1.39070 7
11 1 -1 15.1397 2.02537 16
-11 1 1 16.3297 1.60562 3
-11 1 1 16.1601 1.49992 7
11 1 1 14.9924 1.72205 3
11 -1 -1 14.3993 1.66395 3
11 1 1 14.5924 1.58694 16
-11 1 -1 17.2842 1.67293 7
-11 -1 1 17.5163 1.58734 3
-11 -1 1 16.7892 1.87223 16
0 2 -1 785.025 24.4888 4
0 -2 -1 795.971 23.9780 4
0 -2 -1 785.666 24.6850 10
0 -2 1 780.118 24.5456 10
0 2 1 790.896 24.0577 4
-2 2 1 377.504 11.8791 4
-2 -2 -1 379.309 12.0979 10
2 -2 1 384.143 12.5721 10
-2 -2 -1 380.986 11.4896 4
2 2 -1 379.604 11.7790 4
2 2 1 377.688 11.7669 4
-2 2 -1 373.134 12.0968 4
2 -2 -1 379.089 12.1239 10
4 2 -1 89.6947 3.29818 4
-4 -2 -1 90.9025 3.15200 4
4 2 -1 90.0849 3.51677 10
-4 2 1 94.4187 3.35552 4
-4 -2 -1 89.7471 3.42898 10
4 -2 1 85.7000 3.47181 10
-4 2 1 88.9468 4.25711 16
4 2 1 90.8436 3.25880 4
-4 2 -1 92.3849 3.34230 4
4 -2 -1 89.5942 3.15745 4
4 -2 -1 89.1790 3.62071 10
-4 -2 1 89.7394 3.38063 10
-6 2 1 296.675 9.51588 4
-6 -2 -1 287.724 9.74592 10
-6 -2 -1 282.291 9.22236 4
6 2 -1 276.818 9.12157 4
6 2 -1 248.141 10.8961 16
-6 2 1 291.809 10.9984 16
6 2 1 280.542 9.00051 4
-6 2 -1 292.064 9.64326 4
6 2 1 273.881 10.4791 16
6 -2 -1 272.837 9.64919 10
-6 2 -1 264.404 10.8887 16
-6 -2 1 283.403 9.61316 10
-8 -2 -1 23.6625 3.01344 3
8 -2 1 24.9447 2.51609 3
8 2 -1 21.8908 2.56312 16
-8 -2 -1 21.4405 2.03195 10
-8 2 1 23.3877 2.36198 7
-8 2 1 22.0115 2.67546 16
-8 -2 -1 15.7570 2.93549 7
-8 2 -1 24.6203 2.53670 7
-8 2 -1 20.2926 2.90389 16
8 -2 -1 24.1148 2.65420 3
8 2 1 20.0469 2.56517 16
-8 -2 1 22.0744 2.88623 16
-8 -2 1 24.7702 2.56057 3
8 2 1 22.1450 2.74974 3
10 -2 1 96.5281 4.26300 3
-10 -2 -1 93.5317 4.11997 7
10 -2 1 88.3038 4.05518 6
-10 2 1 97.8248 4.31458 7
-10 -2 -1 96.9259 4.53236 3
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-2 2 9 27.4291 2.43483 9
-2 2 9 29.1410 2.84085 2
2 2 9 24.0265 2.28982 8
-2 -2 9 26.0906 2.45451 8
2 -2 -9 28.1434 2.51438 7
-2 -2 9 28.3327 2.27057 2
2 2 9 30.4429 2.68170 9
2 2 9 30.1376 2.43486 2
2 2 9 26.0111 2.77539 11
-2 -2 9 27.0524 2.39592 9
-2 -2 9 28.1473 2.64824 11
-2 -2 9 27.3009 2.30166 5
-4 2 9 116.040 4.83806 8
4 -2 9 99.1419 4.73582 15
4 -2 9 108.423 4.90814 8
4 -2 9 106.510 4.62307 9
4 -2 9 110.754 4.91089 2
4 -2 9 103.582 4.20766 6
4 -2 9 110.417 8.16886 14
-4 -2 -9 112.765 5.55505 7
-4 2 9 107.582 5.19588 11
-4 -2 9 107.419 4.89673 9
-4 -2 9 112.315 5.33956 11
-4 -2 9 113.153 4.80934 8
4 2 9 111.053 4.85018 15
4 2 9 111.302 5.09254 9
-4 -2 9 116.242 4.83648 2
-4 -2 9 107.733 4.65832 5
4 2 9 103.055 4.67794 2
4 -2 -9 111.086 5.14722 7
6 -2 9 125.048 4.57220 6
6 -2 9 128.969 7.91482 14
6 -2 9 126.851 4.99610 8
6 -2 9 123.786 5.05851 15
-6 -2 -9 132.527 5.87442 7
-6 2 9 116.224 5.65951 8
-6 -2 9 129.434 4.95822 2
-6 -2 9 126.590 5.17559 11
6 2 9 124.279 4.75213 15
-6 -2 9 120.829 4.65152 8
6 2 9 119.425 8.28506 14
6 2 9 116.508 4.42864 3
8 -2 9 74.5800 4.13156 14
-8 2 9 75.0470 2.73338 8
8 -2 9 75.0651 2.77774 8
8 -2 -9 72.3881 2.80912 7
-8 -2 9 74.1374 2.76140 2
-1 3 9 257.672 9.48365 16
1 -3 9 261.475 9.34906 2
1 -3 9 258.128 9.10468 15
1 -3 9 253.987 9.60787 11
1 -3 9 254.018 8.88626 5
1 -3 9 260.190 9.31980 9
1 -3 9 259.062 9.34625 8
1 -3 9 262.321 12.5624 14
1 -3 9 249.019 8.81860 13
1 -3 9 264.506 9.71480 12
1 -3 9 247.317 8.80356 6
1 3 9 261.680 9.32408 16
-1 -3 9 250.730 9.77252 9
-1 -3 9 261.448 9.45768 5
-1 -3 9 263.694 9.45731 2
-1 -3 9 265.767 9.89489 12
1 3 9 261.412 9.43258 9
-1 -3 9 264.762 9.33924 8
-1 -3 9 267.001 8.95792 13
3 -3 9 28.5724 2.30870 9
3 -3 9 27.9573 1.76303 6
-3 -3 -9 31.5508 2.75872 7
-3 3 9 28.8297 1.99640 8
3 -3 9 28.2754 2.45534 8
3 -3 9 25.3148 1.76047 13
3 -3 9 27.0959 2.07402 2
3 -3 9 28.5889 2.11162 15
3 -3 9 29.8448 4.09660 14
-3 -3 9 29.5841 2.58497 12
3 -3 -9 32.5968 2.58270 7
-3 -3 9 28.8983 2.04766 8
-3 -3 9 29.4250 2.21382 9
-3 -3 9 33.8443 2.40696 5
-3 -3 9 29.8531 2.54415 11
-3 -3 9 30.6425 2.12670 2
-5 3 9 74.0351 3.10410 8
5 -3 9 76.9210 3.31952 6
5 -3 9 80.2618 3.90831 8
5 -3 9 73.8607 3.33199 2
5 -3 9 72.8517 8.14954 14
-5 -3 9 77.5216 3.42356 2
5 3 9 77.0574 3.45300 15
-5 -3 9 75.7226 4.78009 11
7 -3 9 4.72036 0.74270 8
7 -3 9 2.86277 1.03621 14
7 -3 9 3.18296 0.78326 6
-7 -3 -9 3.71128 0.79442 7
7 -3 9 2.89547 0.67779 15
7 3 9 2.83272 1.05505 14
-7 -3 9 3.15494 0.67429 2
-7 -3 9 3.62052 0.64990 9
0 -4 -9 1265.16 38.2968 7
0 -4 9 1198.81 36.7542 6
0 4 9 1199.86 38.0864 16
0 -4 9 1215.45 37.6783 2
0 -4 9 1117.19 39.8045 12
0 -4 9 1176.69 37.9302 9
2 -4 9 19.8767 1.37737 13
2 -4 9 16.7925 2.73478 14
2 -4 9 14.3128 1.63287 8
2 -4 9 18.3107 1.38789 6
-2 4 9 18.1903 1.77545 16
-2 -4 -9 21.2118 2.16789 7
2 -4 9 17.4748 1.89256 12
2 -4 9 17.1262 1.42229 15
-2 -4 9 18.0903 2.10947 11
-2 -4 9 16.7722 1.54382 2
-2 -4 9 15.2066 2.03008 9
2 4 9 14.3152 1.58537 16
2 -4 -9 18.9016 2.12132 7
-2 -4 9 16.6793 1.81085 12
4 -4 9 90.6439 3.34155 6
4 -4 9 89.4672 5.74698 14
4 -4 9 85.8473 4.02620 8
4 -4 9 86.8292 3.51106 15
-4 -4 -9 92.6449 4.11505 7
-4 -4 9 91.1707 3.59876 5
-4 -4 9 84.7002 3.63939 2
-4 -4 9 89.3991 4.79639 12
-4 -4 9 80.6972 3.89048 11
4 -4 -9 85.5131 3.86061 7
-4 -4 9 88.8954 3.61885 9
4 4 9 89.0371 3.59279 15
6 -4 9 47.0691 2.97924 14
-6 -4 -9 76.8618 3.13237 7
-6 -4 9 80.6889 2.87872 5
-6 -4 9 66.7847 3.35964 11
-6 -4 9 74.2699 2.99190 9
1 -5 9 140.841 4.70686 13
1 -5 9 134.480 4.98338 6
-1 -5 -9 133.725 5.13750 7
1 -5 9 135.713 5.08831 12
-1 -5 9 124.467 5.09041 11
-1 -5 9 135.934 4.94429 12
3 -5 9 7.93251 1.71722 14
-3 -5 -9 7.51301 1.03558 7
3 5 9 8.63060 0.90119 15
-3 -5 9 9.31126 1.01176 11
-3 -5 9 8.75971 0.99134 5
0 0 10 29.6156 2.58612 2
0 0 10 26.1509 2.35485 9
0 0 10 28.6068 2.67189 11
0 0 10 25.9186 2.19741 8
0 0 10 24.9311 2.20424 15
2 0 10 60.0117 3.90736 8
-2 0 10 68.7579 4.82189 11
2 0 10 65.2238 4.24834 9
-2 0 10 61.3096 3.96834 8
2 0 10 60.0802 3.83836 15
2 0 10 59.4403 5.66804 14
-4 0 10 1.43422 0.72959 8
-4 0 10 1.26910 0.87431 11
-4 0 10 1.25499 0.61392 9
4 0 10 1.40677 0.91336 15
4 0 10 0.83204 1.29028 14
4 0 10 1.29985 0.55372 2
4 0 10 1.46436 0.86526 9
-4 0 10 0.83959 0.39563 2
4 0 10 1.00432 0.89959 8
-6 0 10 1.79748 1.21603 11
6 0 10 1.92982 0.68141 8
6 0 10 -0.1400 0.63393 15
6 0 10 0.63283 0.43114 2
6 0 10 1.35278 1.08516 14
-6 0 10 0.72303 0.58154 8
-1 -1 -10 120.149 5.62852 7
-1 1 10 115.265 5.70604 15
1 -1 10 130.294 5.50372 8
1 -1 10 131.310 5.81202 2
1 -1 10 133.499 7.83981 11
-1 1 10 127.894 6.14701 11
-1 -1 10 130.452 5.40807 2
1 -1 -10 119.798 5.62071 7
1 1 10 130.981 6.44691 9
1 1 10 132.913 6.07593 11
1 1 10 129.349 6.84349 15
-1 -1 10 124.530 6.04533 11
-1 -1 10 127.996 5.66736 9
-3 1 10 3.20714 0.75517 9
-3 1 10 5.23263 1.63494 11
3 -1 10 3.47155 0.94851 9
3 -1 10 2.28194 0.88262 8
3 -1 10 1.90804 0.60270 2
3 -1 10 4.42539 1.14372 15
-3 1 10 5.39934 1.46730 2
-3 1 10 2.34060 0.83720 8
3 1 10 3.33191 1.17536 15
-3 -1 10 5.60717 1.45882 5
-3 -1 10 2.71847 0.86310 9
3 1 10 1.53796 0.76911 8
-3 -1 10 5.39561 1.41029 8
3 1 10 1.87001 0.55571 2
3 -1 -10 2.50305 1.10876 7
3 1 10 1.98584 0.94044 9
-3 -1 10 3.39778 1.06899 11
-3 -1 10 1.73146 0.49533 2
5 -1 10 72.8536 6.67895 14
-5 1 10 66.1281 3.23802 11
5 -1 10 63.1249 3.12340 9
5 -1 10 66.0978 3.18728 15
-5 1 10 64.0610 2.92058 2
5 -1 10 69.7308 3.40058 2
-5 -1 -10 62.7342 3.45305 7
-5 1 10 70.5359 3.15169 8
5 -1 10 66.2917 3.24418 8
-5 -1 10 67.4564 3.16720 2
-5 -1 10 61.3236 4.07536 8
5 -1 -10 60.7750 3.10295 7
5 1 10 70.6127 3.18395 15
5 1 10 64.7398 2.89527 8
-5 -1 10 73.5418 4.03930 9
-7 1 10 12.0175 1.29343 8
7 -1 10 11.9548 0.99365 15
7 -1 10 13.3804 2.04266 14
7 -1 10 12.5895 1.10451 8
-7 -1 10 12.8127 1.06229 2
-7 -1 10 12.1058 1.08231 8
7 1 10 12.9193 1.13125 15
7 -1 -10 11.9760 1.27722 7
7 1 10 13.0575 1.96144 14
0 -2 10 19.4415 2.14462 8
0 -2 10 19.8449 2.00993 2
0 2 10 15.6163 1.95598 2
0 2 10 22.1167 1.63911 8
0 -2 10 21.2259 2.17189 11
0 -2 10 19.6830 1.94020 9
0 2 10 18.4220 2.32216 11
0 -2 -10 18.3660 2.39814 7
0 -2 10 16.8088 1.80886 15
0 2 10 18.5481 2.16904 9
2 -2 10 49.1364 2.76231 8
-2 2 10 46.0605 2.73258 9
-2 -2 -10 46.3614 3.33256 7
2 -2 10 46.5025 2.60722 15
2 -2 10 45.9498 2.85760 11
2 -2 10 45.7010 2.76206 9
-2 2 10 48.6265 2.53995 8
2 -2 10 44.3708 4.39308 14
-2 2 10 46.9148 3.17853 11
2 -2 10 45.5364 2.84795 2
-2 -2 10 47.2770 2.82909 9
-2 -2 10 46.2978 2.44985 5
2 2 10 43.6544 2.53600 8
2 2 10 46.0512 2.88535 9
-2 -2 10 43.4711 2.78688 2
-2 -2 10 48.6713 3.13302 11
2 2 10 40.8635 2.64872 2
-2 -2 10 47.6983 2.64420 8
2 -2 -10 46.2518 3.07750 7
2 2 10 45.7372 2.83261 15
4 -2 10 1.47760 0.72369 9
4 -2 10 0.16486 0.52082 2
-4 2 10 1.19661 0.69288 8
4 -2 10 2.79334 0.95828 15
4 -2 10 0.18755 1.62170 14
4 -2 10 1.38033 0.72824 8
-4 2 10 0.49765 0.75372 11
4 2 10 1.06793 1.21934 14
-4 -2 10 1.29187 0.59238 9
4 2 10 0.14613 0.42251 2
-4 -2 10 0.69193 0.79439 11
-4 -2 10 0.87529 0.38430 2
4 2 10 0.98783 0.81445 15
-4 -2 10 1.21913 0.88140 8
6 -2 10 1.21273 0.58132 15
6 -2 10 0.69167 0.99888 14
6 -2 10 0.25659 0.48139 2
-6 -2 -10 1.72318 0.88797 7
6 -2 10 0.68998 0.58347 8
-6 2 10 -0.3293 0.60759 8
6 2 10 0.92187 1.13627 14
6 2 10 1.24076 0.51361 15
-6 -2 10 0.30321 0.29101 2
-6 -2 10 -0.0721 0.46526 9
-6 -2 10 -0.1378 0.54631 11
6 -2 -10 1.02195 0.71929 7
1 -3 10 91.8686 3.75529 15
1 -3 10 97.8198 4.53093 2
1 -3 10 96.9093 5.10898 11
-1 -3 -10 99.7119 4.62086 7
1 -3 10 94.1459 4.01799 8
-1 -3 10 100.736 4.42872 11
-1 -3 10 91.0864 4.02722 9
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1 -3 -10 99.0146 4.57606 7
3 -3 10 3.66914 0.74101 8
-3 -3 -10 2.73813 1.21510 7
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3 -3 10 5.30423 1.11021 2
3 -3 10 3.00232 1.72204 14
3 -3 10 4.28532 1.00797 15
-3 -3 10 4.08233 1.27264 2
-3 -3 10 2.70336 1.25769 11
-3 -3 10 2.84451 1.02425 8
-3 -3 10 2.90553 0.85328 9
3 3 10 2.04639 1.95403 14
3 3 10 5.98255 1.40625 15
-3 -3 10 3.25489 1.22094 5
5 -3 10 50.8627 2.27061 15
5 -3 10 47.7008 4.30918 14
5 -3 10 49.0025 2.95179 8
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5 3 10 42.9794 2.36007 15
5 -3 -10 47.7007 2.60214 7
-5 -3 10 50.0876 2.36639 9
-5 -3 10 55.9431 2.99168 2
0 -4 10 7.98534 1.18508 11
0 -4 10 5.44517 0.98878 9
0 -4 -10 8.99453 1.52916 7
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2 -4 10 20.3363 1.59334 15
-2 -4 10 25.5367 1.94876 9
-2 -4 10 25.5356 1.71627 5
2 -4 -10 24.4629 1.86133 7
-2 -4 10 25.5650 1.73436 11
4 -4 10 0.56575 0.70958 15
-4 -4 -10 2.22141 0.77041 7
-4 -4 10 1.27599 0.40181 9
4 -4 -10 0.97755 0.70755 7
4 4 10 1.32709 0.62744 15
-4 -4 10 1.36751 0.46842 11
0 0 11 61.4474 3.19019 8
0 0 11 67.3875 3.24231 15
0 0 11 65.7503 3.40824 9
0 0 11 63.3605 3.58017 11
0 0 11 63.9583 3.25600 2
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2 0 11 34.4252 2.44575 2
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2 0 11 38.2534 2.63498 11
2 0 11 35.3248 2.19592 15
2 0 11 34.6040 2.26396 8
-2 0 11 35.5732 2.21255 8
2 0 11 35.4108 2.38426 9
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4 0 11 26.3850 1.87897 9
-4 0 11 24.7137 1.71015 2
4 0 11 28.6754 1.99160 2
4 0 11 25.1991 1.68568 8
4 0 11 21.7969 2.67064 14
-4 0 11 25.0794 1.62561 9
4 0 11 27.5503 1.77838 15
-4 0 11 27.2674 1.79507 8
6 0 11 92.7346 3.18919 15
6 0 11 74.2962 5.49880 14
-6 0 11 95.5201 3.50737 8
6 0 11 90.0670 3.30497 2
1 -1 11 25.6315 2.97685 15
-1 1 11 28.3259 1.83041 15
-1 1 11 26.5976 2.04336 9
1 -1 11 25.6415 2.11510 2
1 -1 11 27.1685 2.10793 11
1 -1 11 28.2635 2.14517 9
1 -1 11 26.8233 2.05061 8
-1 -1 -11 25.4201 2.46496 7
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1 1 11 27.2887 2.49353 11
-1 -1 11 26.6954 2.07189 9
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1 1 11 27.7320 2.10209 15
1 1 11 27.6293 2.13770 9
1 1 11 26.9148 1.95777 2
1 1 11 26.8027 1.85480 8
-1 -1 11 29.8292 1.98265 8
-1 -1 11 28.9115 2.09522 2
3 -1 11 66.2460 3.30035 15
3 -1 11 60.1606 4.66591 14
3 -1 11 65.5980 3.77804 8
-3 1 11 65.1500 2.83948 9
3 -1 11 54.8660 3.85057 9
-3 1 11 63.6670 4.33437 11
-3 1 11 64.3786 2.80757 2
-3 -1 11 53.9185 3.77397 8
-3 -1 11 70.9736 3.56206 9
3 1 11 61.5023 2.92519 2
3 -1 -11 59.9519 2.99062 7
-3 -1 11 55.5298 4.09816 11
-3 -1 11 69.6103 4.11300 2
3 1 11 61.1602 2.77176 8
5 -1 11 0.70125 0.58723 15
-5 1 11 0.49173 0.45114 8
5 -1 11 0.59551 0.51310 8
5 -1 11 -0.1438 0.30929 2
5 -1 11 0.36751 0.75504 14
5 1 11 0.05838 0.38320 2
5 1 11 0.01259 0.54489 15
-5 -1 11 -0.3484 0.55828 11
-5 -1 11 0.30498 0.46818 9
-5 -1 11 0.48963 0.26731 2
-5 -1 11 0.41727 0.75853 8
5 -1 -11 1.05061 0.60721 7
0 2 11 57.6162 2.64680 15
0 -2 11 51.4830 3.57854 8
0 -2 11 57.7575 3.20538 9
0 -2 11 50.8962 2.79089 2
0 -2 -11 46.6724 3.00382 7
0 2 11 49.8788 2.39810 8
0 -2 11 48.3374 3.70333 11
0 2 11 48.3424 2.51806 9
2 -2 11 32.2677 2.06452 2
-2 2 11 30.9572 1.80315 8
2 -2 11 30.7171 3.09323 11
2 -2 11 31.4931 1.92113 9
2 -2 11 32.1752 1.89234 15
2 -2 11 31.6346 1.95489 8
-2 -2 -11 29.6314 2.34341 7
2 2 11 30.6800 1.95848 9
-2 -2 11 30.8219 2.00838 9
-2 -2 11 31.7896 2.37113 11
2 -2 -11 30.5745 2.15903 7
-2 -2 11 30.8110 1.96136 8
-2 -2 11 34.4513 2.11282 2
2 2 11 31.8506 1.93218 15
4 -2 11 16.7112 1.99679 14
4 -2 11 20.6063 1.35973 15
-4 2 11 19.0560 1.40595 8
4 -2 11 21.5139 1.54059 2
-4 -2 -11 21.5430 1.66933 7
4 -2 11 20.0487 1.48277 8
-4 -2 11 20.2906 1.43853 9
4 2 11 20.2547 1.40612 15
-4 -2 11 20.9466 1.37294 8
-4 -2 11 19.9203 1.60372 11
-4 -2 11 21.0039 1.52635 2
1 -3 11 19.0501 1.99639 2
1 -3 11 18.4161 1.39926 9
1 -3 11 19.2668 1.97959 8
-1 3 11 20.4611 1.38168 15
-1 -3 -11 21.1710 1.82211 7
-1 -3 11 20.1103 1.61799 11
1 3 11 19.5017 1.36222 15
1 -3 -11 20.0502 1.62149 7
-1 -3 11 19.2712 1.31779 8
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3 -3 11 44.3082 2.04449 15
3 -3 11 42.2923 1.94635 8
-3 -3 11 48.4533 2.98415 11
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3 -3 -11 44.3966 2.17220 7
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3 3 11 43.1104 2.22397 15
0 0 12 17.2853 1.58841 11
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-2 0 12 82.1452 3.71071 9
2 0 12 87.6292 3.48211 8
2 0 12 95.1577 4.30543 15
2 0 12 89.0163 3.63662 9
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-4 0 12 42.9046 1.80122 8
4 0 12 44.7954 1.87073 15
1 -1 12 178.608 6.23973 8
-1 1 12 184.642 6.59308 11
-1 1 12 178.312 6.28027 8
1 -1 12 176.335 6.56755 2
1 -1 12 178.073 7.20087 11
-1 1 12 181.004 6.40631 2
1 -1 12 176.510 6.28814 15
-1 1 12 181.631 7.30638 9
1 -1 12 179.887 6.60756 9
-1 -1 12 181.864 6.22845 8
-1 -1 12 178.601 6.26772 2
1 1 12 177.990 6.54313 8
-1 -1 12 184.318 6.75495 9
-1 -1 12 182.069 6.65962 11
1 1 12 181.247 6.35477 2
1 1 12 179.325 6.31855 15
1 1 12 182.842 6.55783 9
3 -1 12 215.379 8.00173 2
-3 1 12 244.818 7.94490 8
3 -1 12 230.997 7.58586 15
3 -1 12 233.460 7.69756 9
3 -1 12 245.017 7.73943 8
3 1 12 236.294 7.64461 15
3 1 12 229.187 7.95524 2
-3 -1 12 244.531 8.06826 2
-3 -1 12 241.974 8.02070 8
-3 -1 12 236.541 8.04204 9
-3 -1 12 244.817 8.28565 11
0 -2 12 16.1012 1.73187 2
0 -2 12 14.6385 1.09618 8
0 -2 12 13.8433 1.29726 9
0 -2 12 14.8321 1.17868 11
2 -2 12 68.7961 3.04027 9
2 -2 12 72.1181 2.78894 8
2 -2 12 70.2495 2.77277 2
-2 -2 12 69.9063 2.85638 11
-2 -2 12 71.0386 2.74603 9
-2 -2 12 66.5538 3.00401 8
-2 -2 12 70.2878 2.71471 2
2 2 12 71.8456 2.68965 15
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 17703
_shelx_res_file
;
TITL c21005 : space group Abm2
c21005.res
created by SHELXL-2018/3 at 10:16:43 on 29-Apr-2021
CELL 1.54178 10.2045 6.1282 9.7293 90.000 90.000 90.000
ZERR 4 0.0006 0.0004 0.0006 0.000 0.000 0.000
LATT -5
SYMM -X, -Y, Z
SYMM X, 1/2-Y, Z
SYMM -X, 1/2+Y, Z
SFAC C H N O
UNIT 24 20 4 16
TEMP -183
SIZE 0.14 0.10 0.02
REM COLR colourless
REM FORM plate
L.S. 10
BOND $H
TWIN -1 0 0 0 -1 0 0 0 -1
LIST 4
MORE 3
ACTA
EADP N1 C2'
EADP C2 N1'
EADP C3 C6'
EADP O1 O2'
EADP C4 C5'
EADP C5 C4'
EADP C6 C3'
EADP O2 O1'
EADP C7 C7'
EADP O3 O3'
EADP O4 O4'
SADI 0.010 N1 H1N N1' H1'N
SADI 0.010 O1 H1O O1' H1'O
SADI 0.010 O2 H2O O2' H2'O
CONF
HTAB
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+1/2, z-1/2
HTAB N1 O4_$1
HTAB O1 O4
EQIV $2 -x, -y+1/2, z-1/2
HTAB C5 O1_$2
HTAB O2 O3_$1
HTAB O2 O4_$1
EQIV $3 -x+1, -y+1/2, z+1/2
HTAB N1' O4'_$3
HTAB O1' O4'
EQIV $4 -x, -y+1/2, z+1/2
HTAB C5' O1'_$4
HTAB O2' O3'_$3
HTAB O2' O4'_$3
FMAP 2
PLAN 5
REM EXTI 0.000000 : removed as not needed.
REM BASF 0.53198, SU = 0.3 : removed so twin fraction fixed at 0.5 each.
REM Hooft and Parsons parameters were more definitive than Flack's parameter.
WGHT 0.050000 0.051200
FVAR 0.90842 0.95306 0.33274 0.32596 0.20327 0.19022 0.09194
FVAR 0.10115 0.22795 0.23688 0.44881 0.55590 0.43850 0.44103
FVAR 0.58275 0.64582 0.78305 0.56262 0.42262 0.35916 0.22580
FVAR 0.66165 0.59684 0.79057
PART 1
N1 3 31.000000 0.250000 141.000000 20.50000 0.01424 0.01902 =
0.01047 0.00000 -0.00003 0.00000
AFIX 44
H1N 2 0.420670 0.250000 0.397586 20.50000 -1.20000
AFIX 0
C2 1 41.000000 0.250000 151.000000 20.50000 0.01265 0.01553 =
0.01119 0.00000 -0.00156 0.00000
C3 1 51.000000 0.250000 161.000000 20.50000 0.01512 0.01797 =
0.01128 0.00000 0.00398 0.00000
O1 4 61.000000 0.250000 171.000000 20.50000 0.01670 0.02742 =
0.01231 0.00000 0.00409 0.00000
AFIX 84
H1O 2 0.269050 0.250000 0.821896 20.50000 -1.50000
AFIX 0
C4 1 71.000000 0.250000 181.000000 20.50000 0.01588 0.02218 =
0.02016 0.00000 0.00255 0.00000
AFIX 43
H4 2 0.007769 0.250000 0.604343 20.50000 -1.20000
AFIX 0
C5 1 81.000000 0.250000 191.000000 20.50000 0.01499 0.02588 =
0.01657 0.00000 -0.00173 0.00000
AFIX 43
H5 2 0.024166 0.250000 0.367711 20.50000 -1.20000
AFIX 0
C6 1 91.000000 0.250000 201.000000 20.50000 0.01496 0.01700 =
0.01414 0.00000 -0.00310 0.00000
O2 4 101.000000 0.250000 211.000000 20.50000 0.01627 0.02949 =
0.01005 0.00000 0.00028 0.00000
AFIX 84
H2O 2 0.325989 0.250000 0.199960 20.50000 -1.50000
AFIX 0
C7 1 111.000000 0.250000 221.000000 20.50000 0.01669 0.01963 =
0.01116 0.00000 -0.00020 0.00000
O3 4 121.000000 0.250000 231.000000 20.50000 0.01409 0.02681 =
0.01365 0.00000 -0.00083 0.00000
O4 4 131.000000 0.250000 241.000000 20.50000 0.01477 0.03679 =
0.01573 0.00000 -0.00135 0.00000
PART 2
N1' 3 31.000000 0.250000 -141.000000 -20.50000 0.01265 0.01553 =
0.01119 0.00000 -0.00156 0.00000
AFIX 44
H1'N 2 0.420644 0.250000 0.602401 -20.50000 -1.20000
AFIX 0
C2' 1 41.000000 0.250000 -151.000000 -20.50000 0.01424 0.01902 =
0.01047 0.00000 -0.00003 0.00000
C3' 1 51.000000 0.250000 -161.000000 -20.50000 0.01496 0.01700 =
0.01414 0.00000 -0.00310 0.00000
O1' 4 61.000000 0.250000 -171.000000 -20.50000 0.01627 0.02949 =
0.01005 0.00000 0.00028 0.00000
AFIX 84
H1'O 2 0.269046 0.250000 0.178106 -20.50000 -1.50000
AFIX 0
C4' 1 71.000000 0.250000 -181.000000 -20.50000 0.01499 0.02588 =
0.01657 0.00000 -0.00173 0.00000
AFIX 43
H4' 2 0.007769 0.250000 0.395657 -20.50000 -1.20000
AFIX 0
C5' 1 81.000000 0.250000 -191.000000 -20.50000 0.01588 0.02218 =
0.02016 0.00000 0.00255 0.00000
AFIX 43
H5' 2 0.024166 0.250000 0.632289 -20.50000 -1.20000
AFIX 0
C6' 1 91.000000 0.250000 -201.000000 -20.50000 0.01512 0.01797 =
0.01128 0.00000 0.00398 0.00000
O2' 4 101.000000 0.250000 -211.000000 -20.50000 0.01670 0.02742 =
0.01231 0.00000 0.00409 0.00000
AFIX 84
H2'O 2 0.326029 0.250000 0.800052 -20.50000 -1.50000
AFIX 0
C7' 1 111.000000 0.250000 -221.000000 -20.50000 0.01669 0.01963 =
0.01116 0.00000 -0.00020 0.00000
O3' 4 121.000000 0.250000 -231.000000 -20.50000 0.01409 0.02681 =
0.01365 0.00000 -0.00083 0.00000
O4' 4 131.000000 0.250000 -241.000000 -20.50000 0.01477 0.03679 =
0.01573 0.00000 -0.00135 0.00000
PART 0
HKLF 4 1 0 0 1 0 -1 0 1 0 0
REM c21005 : space group Abm2
REM wR2 = 0.0675, GooF = S = 1.109, Restrained GooF = 1.105 for all data
REM R1 = 0.0243 for 690 Fo > 4sig(Fo) and 0.0246 for all 700 data
REM 74 parameters refined using 4 restraints
END
WGHT 0.0500 0.0512
REM Instructions for potential hydrogen bonds
HTAB N1 O4_$1
HTAB O1 O4
HTAB C5 O1_$2
HTAB O2 O3_$1
HTAB O2 O4_$1
HTAB N1' O4'_$3
HTAB O1' O4'
HTAB C5' O1'_$4
HTAB O2' O3'_$3
HTAB O2' O4'_$3
REM Highest difference peak 0.202, deepest hole -0.251, 1-sigma level 0.050
Q1 1 0.2452 0.2500 0.9466 10.50000 0.05 0.20
Q2 1 0.6021 0.2500 0.4401 10.50000 0.05 0.19
Q3 1 0.1699 0.2500 0.0606 10.50000 0.05 0.19
Q4 1 0.3645 0.2500 0.1341 10.50000 0.05 0.17
Q5 1 0.6943 0.2500 0.4961 10.50000 0.05 0.16
;
_shelx_res_checksum 41291
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y+1/2, z'
'-x, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1, z+1/2'
'-x, y+1, 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
N N1 0.3327(2) 0.250000 0.44103(19) 0.0146(4) Uani d 0.953(3) A 1
H H1N 0.421(3) 0.25000(2) 0.3976(15) 0.017 Uiso calc 0.953(3) A 1
C C2 0.3260(2) 0.250000 0.5827(2) 0.0131(5) Uani d 0.953(3) A 1
C C3 0.2033(3) 0.250000 0.6458(3) 0.0148(5) Uani d 0.953(3) A 1
O O1 0.19022(19) 0.250000 0.7831(2) 0.0188(4) Uani d 0.953(3) A 1
H H1O 0.269(4) 0.25000(2) 0.8219(19) 0.028 Uiso calc 0.953(3) A 1
C C4 0.0919(3) 0.250000 0.5626(3) 0.0194(6) Uani d 0.953(3) A 1
H H4 0.007769 0.250000 0.604343 0.023 Uiso calc 0.953(3) A 1
C C5 0.1011(2) 0.250000 0.4226(3) 0.0191(5) Uani d 0.953(3) A 1
H H5 0.024166 0.250000 0.367711 0.023 Uiso calc 0.953(3) A 1
C C6 0.2280(2) 0.250000 0.3592(3) 0.0154(5) Uani d 0.953(3) A 1
O O2 0.2369(2) 0.250000 0.22580(18) 0.0186(4) Uani d 0.953(3) A 1
H H2O 0.326(3) 0.25000(2) 0.2000(10) 0.028 Uiso calc 0.953(3) A 1
C C7 0.4488(2) 0.250000 0.6616(2) 0.0158(5) Uani d 0.953(3) A 1
O O3 0.55590(18) 0.250000 0.59684(19) 0.0182(4) Uani d 0.953(3) A 1
O O4 0.43850(17) 0.250000 0.7906(2) 0.0224(5) Uani d 0.953(3) A 1
N N1' 0.3327(2) 0.250000 0.55897(19) 0.0131(5) Uani d 0.047(3) A 2
H H1'N 0.421(3) 0.25000(2) 0.6024(16) 0.016 Uiso calc 0.047(3) A 2
C C2' 0.3260(2) 0.250000 0.4173(2) 0.0146(4) Uani d 0.047(3) A 2
C C3' 0.2033(3) 0.250000 0.3542(3) 0.0154(5) Uani d 0.047(3) A 2
O O1' 0.19022(19) 0.250000 0.2169(2) 0.0186(4) Uani d 0.047(3) A 2
H H1'O 0.269(4) 0.25000(2) 0.178(2) 0.028 Uiso calc 0.047(3) A 2
C C4' 0.0919(3) 0.250000 0.4374(3) 0.0191(5) Uani d 0.047(3) A 2
H H4' 0.007769 0.250000 0.395657 0.023 Uiso calc 0.047(3) A 2
C C5' 0.1011(2) 0.250000 0.5774(3) 0.0194(6) Uani d 0.047(3) A 2
H H5' 0.024166 0.250000 0.632289 0.023 Uiso calc 0.047(3) A 2
C C6' 0.2280(2) 0.250000 0.6408(3) 0.0148(5) Uani d 0.047(3) A 2
O O2' 0.2369(2) 0.250000 0.77420(18) 0.0188(4) Uani d 0.047(3) A 2
H H2'O 0.326(4) 0.25000(2) 0.8001(11) 0.028 Uiso calc 0.047(3) A 2
C C7' 0.4488(2) 0.250000 0.3384(2) 0.0158(5) Uani d 0.047(3) A 2
O O3' 0.55590(18) 0.250000 0.40316(19) 0.0182(4) Uani d 0.047(3) A 2
O O4' 0.43850(17) 0.250000 0.2094(2) 0.0224(5) Uani d 0.047(3) A 2
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
N1 0.0142(9) 0.0190(8) 0.0105(11) 0.000 0.0000(9) 0.000
C2 0.0127(12) 0.0155(9) 0.0112(10) 0.000 -0.0016(9) 0.000
C3 0.0151(10) 0.0180(11) 0.0113(11) 0.000 0.0040(8) 0.000
O1 0.0167(9) 0.0274(9) 0.0123(8) 0.000 0.0041(7) 0.000
C4 0.0159(12) 0.0222(10) 0.0202(13) 0.000 0.0025(10) 0.000
C5 0.0150(11) 0.0259(10) 0.0166(10) 0.000 -0.0017(9) 0.000
C6 0.0150(12) 0.0170(10) 0.0141(12) 0.000 -0.0031(9) 0.000
O2 0.0163(9) 0.0295(8) 0.0101(8) 0.000 0.0003(6) 0.000
C7 0.0167(10) 0.0196(12) 0.0112(14) 0.000 -0.0002(9) 0.000
O3 0.0141(8) 0.0268(7) 0.0137(8) 0.000 -0.0008(6) 0.000
O4 0.0148(12) 0.0368(11) 0.0157(9) 0.000 -0.0014(7) 0.000
N1' 0.0127(12) 0.0155(9) 0.0112(10) 0.000 -0.0016(9) 0.000
C2' 0.0142(9) 0.0190(8) 0.0105(11) 0.000 0.0000(9) 0.000
C3' 0.0150(12) 0.0170(10) 0.0141(12) 0.000 -0.0031(9) 0.000
O1' 0.0163(9) 0.0295(8) 0.0101(8) 0.000 0.0003(6) 0.000
C4' 0.0150(11) 0.0259(10) 0.0166(10) 0.000 -0.0017(9) 0.000
C5' 0.0159(12) 0.0222(10) 0.0202(13) 0.000 0.0025(10) 0.000
C6' 0.0151(10) 0.0180(11) 0.0113(11) 0.000 0.0040(8) 0.000
O2' 0.0167(9) 0.0274(9) 0.0123(8) 0.000 0.0041(7) 0.000
C7' 0.0167(10) 0.0196(12) 0.0112(14) 0.000 -0.0002(9) 0.000
O3' 0.0141(8) 0.0268(7) 0.0137(8) 0.000 -0.0008(6) 0.000
O4' 0.0148(12) 0.0368(11) 0.0157(9) 0.000 -0.0014(7) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C6 N1 C2 . . 123.81(19) ?
C6 N1 H1N . . 118.1 ?
C2 N1 H1N . . 118.1 ?
N1 C2 C3 . . 119.0(2) ?
N1 C2 C7 . . 118.6(2) ?
C3 C2 C7 . . 122.41(19) ?
O1 C3 C2 . . 121.8(2) ?
O1 C3 C4 . . 119.8(2) ?
C2 C3 C4 . . 118.4(2) ?
C3 O1 H1O . . 109.5 ?
C5 C4 C3 . . 121.5(2) ?
C5 C4 H4 . . 119.2 ?
C3 C4 H4 . . 119.2 ?
C4 C5 C6 . . 119.5(2) ?
C4 C5 H5 . . 120.3 ?
C6 C5 H5 . . 120.3 ?
O2 C6 N1 . . 122.7(2) ?
O2 C6 C5 . . 119.5(2) ?
N1 C6 C5 . . 117.8(2) ?
C6 O2 H2O . . 109.5 ?
O4 C7 O3 . . 124.8(2) ?
O4 C7 C2 . . 116.7(2) ?
O3 C7 C2 . . 118.53(19) ?
C6' N1' C2' . . 123.81(19) ?
C6' N1' H1'N . . 118.1 ?
C2' N1' H1'N . . 118.1 ?
N1' C2' C3' . . 119.0(2) ?
N1' C2' C7' . . 118.6(2) ?
C3' C2' C7' . . 122.41(19) ?
O1' C3' C2' . . 121.8(2) ?
O1' C3' C4' . . 119.8(2) ?
C2' C3' C4' . . 118.4(2) ?
C3' O1' H1'O . . 109.5 ?
C5' C4' C3' . . 121.5(2) ?
C5' C4' H4' . . 119.2 ?
C3' C4' H4' . . 119.2 ?
C4' C5' C6' . . 119.5(2) ?
C4' C5' H5' . . 120.3 ?
C6' C5' H5' . . 120.3 ?
O2' C6' N1' . . 122.7(2) ?
O2' C6' C5' . . 119.5(2) ?
N1' C6' C5' . . 117.8(2) ?
C6' O2' H2'O . . 109.5 ?
O4' C7' O3' . . 124.8(2) ?
O4' C7' C2' . . 116.7(2) ?
O3' C7' C2' . . 118.53(19) ?
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
N1 C6 . 1.333(3) ?
N1 C2 . 1.381(3) ?
N1 H1N . 0.99(3) ?
C2 C3 . 1.394(3) ?
C2 C7 . 1.470(3) ?
C3 O1 . 1.342(3) ?
C3 C4 . 1.395(4) ?
O1 H1O . 0.89(4) ?
C4 C5 . 1.365(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.434(3) ?
C5 H5 . 0.9500 ?
C6 O2 . 1.301(3) ?
O2 H2O . 0.94(4) ?
C7 O4 . 1.259(3) ?
C7 O3 . 1.262(3) ?
N1' C6' . 1.333(3) ?
N1' C2' . 1.381(3) ?
N1' H1'N . 0.99(4) ?
C2' C3' . 1.394(3) ?
C2' C7' . 1.470(3) ?
C3' O1' . 1.342(3) ?
C3' C4' . 1.395(4) ?
O1' H1'O . 0.89(4) ?
C4' C5' . 1.365(3) ?
C4' H4' . 0.9500 ?
C5' C6' . 1.434(3) ?
C5' H5' . 0.9500 ?
C6' O2' . 1.301(3) ?
O2' H2'O . 0.94(4) ?
C7' O4' . 1.259(3) ?
C7' O3' . 1.262(3) ?
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
N1 H1N O4 6_654 0.99 1.77 2.755(3) 169 yes
O1 H1O O4 . 0.89 1.76 2.535(3) 145 yes
C5 H5 O1 6_554 0.95 2.34 3.269(3) 166 yes
C4 H4 O2 6 0.95 2.76 3.712(4) 180 yes
O2 H2O O3 6_654 0.94 1.57 2.459(3) 156 yes
O2 H2O O4 6_654 0.94 2.56 3.372(3) 144 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
C6 N1 C2 C3 . . . . 0.0000(10) ?
C6 N1 C2 C7 . . . . 180.000000 ?
N1 C2 C3 O1 . . . . 180.000000 ?
C7 C2 C3 O1 . . . . 0.0000(10) ?
N1 C2 C3 C4 . . . . 0.0000(10) ?
C7 C2 C3 C4 . . . . 180.0000(10) ?
O1 C3 C4 C5 . . . . 180.0000(10) ?
C2 C3 C4 C5 . . . . 0.0000(10) ?
C3 C4 C5 C6 . . . . 0.0000(10) ?
C2 N1 C6 O2 . . . . 180.000000 ?
C2 N1 C6 C5 . . . . 0.000000 ?
C4 C5 C6 O2 . . . . 180.000000 ?
C4 C5 C6 N1 . . . . 0.000000 ?
N1 C2 C7 O4 . . . . 180.000000 ?
C3 C2 C7 O4 . . . . 0.0000(10) ?
N1 C2 C7 O3 . . . . 0.000000 ?
C3 C2 C7 O3 . . . . 180.000000 ?
C6' N1' C2' C3' . . . . 0.000000 ?
C6' N1' C2' C7' . . . . 180.000000 ?
N1' C2' C3' O1' . . . . 180.000000 ?
C7' C2' C3' O1' . . . . 0.000000 ?
N1' C2' C3' C4' . . . . 0.000000 ?
C7' C2' C3' C4' . . . . 180.000000 ?
O1' C3' C4' C5' . . . . 180.000000 ?
C2' C3' C4' C5' . . . . 0.000000 ?
C3' C4' C5' C6' . . . . 0.000000 ?
C2' N1' C6' O2' . . . . 180.000000 ?
C2' N1' C6' C5' . . . . 0.0000(10) ?
C4' C5' C6' O2' . . . . 180.000000 ?
C4' C5' C6' N1' . . . . 0.0000(10) ?
N1' C2' C7' O4' . . . . 180.000000 ?
C3' C2' C7' O4' . . . . 0.000000 ?
N1' C2' C7' O3' . . . . 0.000000 ?
C3' C2' C7' O3' . . . . 180.000000 ?
_cod_database_fobs_code 2243832