#------------------------------------------------------------------------------
#$Date: 2026-09-11 22:14:58 +0100 (Fri, 11 Sep 2026) $
#$Revision: 306876 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/35/2023563.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_2023563
loop_
_publ_author_name
'Vassilyeva, Olga Yu.'
'Kokozay, Vladimir N.'
'Goreshnik, Evgeny'
_publ_section_title
;
2,2′-(Ethane-1,2-diyl)bis[3-(pyridin-2-yl)imidazo[1,5-a]pyridin-2-ium]
dichloride hexahydrate
;
_journal_coeditor_code JY2076
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989026009229
_journal_volume 82
_journal_year 2026
_chemical_formula_iupac 'C26 H22 N6 2+, 2(Cl -), 6(H2 O)'
_chemical_formula_moiety 'C26 H22 N6 2+, 2(Cl -), 6(H2 O)'
_chemical_formula_sum 'C26 H34 Cl2 N6 O6'
_chemical_formula_weight 597.49
_chemical_name_systematic
;
2,2'-(Ethane-1,2-diyl)bis[3-(pyridin-2-yl)imidazo[1,5-a]pyridin-2-ium]
dichloride hexahydrate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2026.05.24 svn.rec792b02 for OlexSys, GUI svn.r7575)
;
_cell_angle_alpha 90
_cell_angle_beta 96.752(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.0061(7)
_cell_length_b 15.1053(10)
_cell_length_c 21.2487(14)
_cell_measurement_reflns_used 3978
_cell_measurement_temperature 150.00(10)
_cell_measurement_theta_max 27.2780
_cell_measurement_theta_min 2.8550
_cell_volume 2870.6(4)
_computing_cell_refinement
;
CrysAlisPro 1.171.xx.xx (Rigaku OD, 2026)
;
_computing_data_collection
;
CrysAlisPro 1.171.xx.xx (Rigaku OD, 2026)
;
_computing_data_reduction
;
CrysAlisPro 1.171.xx.xx (Rigaku OD, 2026)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Mercury (Macrae et al., 2020)
;
_computing_structure_refinement
;
SHELXL2016/6 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 150.00(10)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.6426
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'New Gemini, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_unetI/netI 0.1581
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 6542
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 28.786
_diffrn_reflns_theta_min 2.355
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.277
_exptl_absorpt_correction_T_max 0.980
_exptl_absorpt_correction_T_min 0.933
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2026)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.382
_exptl_crystal_description needle
_exptl_crystal_F_000 1256
_exptl_crystal_size_max 0.382
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.054
_refine_diff_density_max 0.265
_refine_diff_density_min -0.338
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.860
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 380
_refine_ls_number_reflns 6542
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.860
_refine_ls_R_factor_all 0.1215
_refine_ls_R_factor_gt 0.0509
_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^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0808
_refine_ls_wR_factor_ref 0.0910
_reflns_number_gt 3396
_reflns_number_total 6542
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jy2076.cif
_cod_data_source_block I
_cod_original_cell_volume 2870.6(3)
_cod_database_code 2023563
_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 0.902
_shelx_estimated_absorpt_t_max 0.985
_shelx_hkl_file
;
1 0 3 1383.94 17.7191 -2
0 0 -4 1383.94 17.7191 1
0 0 6 152.265 13.3905 1
-2 0 -6 16755.5 59.5009 -2
0 0 8 16755.5 59.5009 1
0 0 10 977.260 19.6924 1
-3 0 -9 21.2144 23.5034 -2
0 0 12 21.2144 23.5034 1
0 0 -14 19.1943 17.8413 1
-4 0 -12 593.711 31.9574 -2
0 0 16 593.711 31.9574 1
0 0 18 87.8895 23.8483 1
-5 0 -15 7.35804 48.9177 -2
0 0 20 7.35804 48.9177 1
0 0 22 182.147 41.3943 1
-6 0 -18 36.0945 60.4224 -2
0 0 24 36.0945 60.4224 1
0 1 2 235.981 6.15501 1
0 -1 3 337.926 6.41748 1
-1 -1 -3 54.0120 10.4449 -2
0 1 4 54.0120 10.4449 1
0 1 5 72.7123 8.16420 1
0 1 -6 446.102 9.78167 1
0 -1 7 431.762 10.3141 1
-2 1 -6 31.9217 13.6782 -2
0 -1 8 31.9217 13.6782 1
0 1 -9 535.215 14.2932 1
-2 1 -7 1147.51 32.2305 -2
0 -1 9 1147.51 32.2305 1
0 -1 -10 1323.69 14.9509 1
0 -1 -11 112.461 11.6809 1
3 1 9 79.4801 16.5854 -2
0 -1 -12 79.4801 16.5854 1
-3 1 -10 1510.68 21.6060 -2
0 -1 13 1510.68 21.6060 1
0 1 14 11.7948 12.4512 1
0 -1 15 45.3656 13.5083 1
4 1 12 147.987 20.8510 -2
0 -1 -16 147.987 20.8510 1
4 -1 13 243.568 22.7562 -2
0 1 -17 243.568 22.7562 1
0 1 -18 176.457 17.0435 1
0 -1 19 79.3160 19.5027 1
-5 -1 -15 15.0118 33.8702 -2
0 1 20 15.0118 33.8702 1
-5 -1 -16 297.803 38.8890 -2
0 1 21 297.803 38.8890 1
-5 -1 -17 9.56034 38.0301 -2
0 1 22 9.56034 38.0301 1
0 1 23 34.4913 44.5749 1
-6 -1 -18 42.2067 64.6843 -2
0 1 24 42.2067 64.6843 1
6 -1 19 94.9026 40.1364 -2
0 1 -25 94.9026 40.1364 1
-6 -1 -20 101.813 73.9129 -2
0 1 26 101.813 73.9129 1
0 1 27 125.528 56.5066 1
0 -2 0-2.90659 13.8753 -2
0 2 0-2.90659 13.8753 1
0 2 1 370.473 12.5560 1
0 2 -2 58.7693 5.42118 1
0 2 -3-0.25384 5.55201 1
-1 -2 -3 191.475 10.1323 -2
0 2 4 191.475 10.1323 1
0 2 -5 484.960 12.0256 1
0 2 6 2094.65 18.3213 1
0 2 7 470.434 11.8847 1
-2 2 -6 13.1338 12.3540 -2
0 -2 8 13.1338 12.3540 1
0 2 9 102.631 9.87962 1
0 -2 10 1244.10 14.3005 1
0 -2 11 112.513 11.1144 1
-3 -2 -9 276.531 16.6673 -2
0 2 12 276.531 16.6673 1
3 2 10 167.185 16.7172 -2
0 -2 -13 167.185 16.7172 1
0 2 -14 410.903 14.2601 1
0 -2 -15 585.590 15.6497 1
4 -2 12 439.085 22.1584 -2
0 2 -16 439.085 22.1584 1
4 -2 13 151.273 22.2693 -2
0 2 -17 151.273 22.2693 1
0 2 -18 5.26383 18.3830 1
0 2 19 1179.30 31.3955 1
-5 -2 -15 369.159 57.4977 -2
0 2 20 369.159 57.4977 1
-5 -2 -16 211.619 59.9092 -2
0 2 21 211.619 59.9092 1
0 2 22 76.0955 43.6703 1
0 2 -23 3.46188 27.0697 1
6 -2 18 63.5827 39.9130 -2
0 2 -24 63.5827 39.9130 1
-6 -2 -19 14.7923 41.8915 -2
0 2 25 14.7923 41.8915 1
-6 -2 -20 16.3531 74.6875 -2
0 2 26 16.3531 74.6875 1
0 2 27 13.9424 57.2880 1
0 -3 -1 31.7416 11.4225 1
0 -3 2 14.0866 5.92281 1
0 -3 3 298.766 5.51849 1
-1 -3 -3 219.119 9.07461 -2
0 3 4 219.119 9.07461 1
0 3 -5 27.3269 7.42641 1
0 3 -6 245.595 7.60166 1
0 3 -7 735.923 9.54993 1
2 -3 6 848.585 16.4408 -2
0 3 -8 848.585 16.4408 1
0 3 9 11.9834 12.2580 1
0 3 -10 547.253 16.0937 1
0 3 -11 142.228 12.7404 1
-3 -3 -9 62.5628 18.5044 -2
0 3 12 62.5628 18.5044 1
3 3 10 194.583 19.1560 -2
0 -3 -13 194.583 19.1560 1
0 3 -14 26.8792 14.2822 1
0 3 -15 329.963 17.6770 1
4 3 12 79.6003 24.5706 -2
0 -3 -16 79.6003 24.5706 1
4 3 13 47.4640 26.1780 -2
0 -3 -17 47.4640 26.1780 1
0 3 -18 844.501 21.4593 1
0 3 19 141.599 18.8257 1
-5 -3 -15 19.7246 32.1128 -2
0 3 20 19.7246 32.1128 1
-5 -3 -16 78.4223 33.7264 -2
0 3 21 78.4223 33.7264 1
0 3 22 52.6476 47.1627 1
5 -3 17 40.4570 41.8828 -2
0 3 -22 40.4570 41.8828 1
0 3 -23 47.9793 27.2271 1
6 -3 18 25.2630 39.5168 -2
0 3 -24 25.2630 39.5168 1
6 -3 19 15.6741 39.8828 -2
0 3 -25 15.6741 39.8828 1
-6 -3 -20-5.14018 79.6348 -2
0 3 26-5.14018 79.6348 1
0 -4 0 980.044 22.1019 -2
0 4 0 980.044 22.1019 1
0 4 1 8869.99 46.3488 1
0 4 2 512.250 10.2667 1
0 -4 3 845.469 8.60495 1
-1 4 -3 1980.77 12.8494 -2
0 -4 4 1980.77 12.8494 1
0 4 -5 650.177 7.80690 1
1 -4 4 787.413 20.8788 -2
0 4 -5 787.413 20.8788 1
0 4 -6 389.190 9.23673 1
0 4 -7 50.6750 7.32725 1
2 -4 6 402.581 12.5552 -2
0 4 -8 402.581 12.5552 1
0 4 9 178.580 28.7005 1
2 -4 7 230.248 12.5456 -2
0 4 -9 230.248 12.5456 1
0 4 -10 1645.22 17.2302 1
0 4 11 31.5924 8.27642 1
-3 -4 -9 703.766 13.9399 -2
0 4 12 703.766 13.9399 1
3 -4 10 1207.27 16.0020 -2
0 4 -13 1207.27 16.0020 1
0 4 -14 35.5257 9.29098 1
0 4 -15 75.7066 10.3264 1
4 4 12 16.5962 15.4431 -2
0 -4 -16 16.5962 15.4431 1
4 -4 13 895.921 22.8058 -2
0 4 -17 895.921 22.8058 1
0 4 18-8.79976 13.5262 1
0 4 -19 338.638 16.2662 1
5 -4 15 774.219 25.5266 -2
0 4 -20 774.219 25.5266 1
5 -4 16 7.18089 21.3841 -2
0 4 -21 7.18089 21.3841 1
0 4 22 16.9148 45.9868 1
5 -4 17-55.3748 39.2989 -2
0 4 -22-55.3748 39.2989 1
0 4 -23 15.2869 26.5960 1
6 -4 18 42.9429 38.2725 -2
0 4 -24 42.9429 38.2725 1
-6 -4 -19 26.7265 39.3368 -2
0 4 25 26.7265 39.3368 1
0 5 1 2998.99 34.0455 1
0 -5 2 1.58225 9.31796 1
0 -5 3 9.39357 7.30112 1
1 5 3 1808.06 15.7782 -2
0 -5 -4 1808.06 15.7782 1
0 -5 -5 812.558 9.78733 1
1 -5 4 1026.99 20.5999 -2
0 5 -5 1026.99 20.5999 1
0 5 -6 6.33444 10.0812 1
0 5 -7 492.986 10.4668 1
-2 -5 -6 1886.14 17.8507 -2
0 5 8 1886.14 17.8507 1
0 5 9 197.852 29.0202 1
2 -5 7 663.820 13.8451 -2
0 5 -9 663.820 13.8451 1
0 5 10 151.184 8.95474 1
0 5 -11-2.07932 8.96775 1
3 -5 9 134.205 12.7533 -2
0 5 -12 134.205 12.7533 1
3 -5 10 265.015 13.6557 -2
0 5 -13 265.015 13.6557 1
0 5 -14 92.5898 9.74916 1
0 5 -15 67.3461 10.2839 1
-4 -5 -12 14.3551 15.4004 -2
0 5 16 14.3551 15.4004 1
4 -5 13 30.3166 16.0120 -2
0 5 -17 30.3166 16.0120 1
0 5 -18 108.389 13.3591 1
0 5 19 20.0811 13.7830 1
5 -5 15 4.24560 19.8265 -2
0 5 -20 4.24560 19.8265 1
5 -5 16 44.0793 21.7310 -2
0 5 -21 44.0793 21.7310 1
0 5 22 215.298 49.2500 1
5 -5 17 147.885 36.2134 -2
0 5 -22 147.885 36.2134 1
0 5 -23 4.69446 24.8360 1
6 -5 18 27.2457 36.1507 -2
0 5 -24 27.2457 36.1507 1
6 -5 19-4.42450 37.1781 -2
0 5 -25-4.42450 37.1781 1
0 -6 0 1006.96 27.4975 -2
0 6 0 1006.96 27.4975 1
0 6 -1 444.791 16.1886 1
0 6 2 2669.49 36.4286 1
0 6 3 160.937 10.1459 1
-1 6 -3 275.555 11.6518 -2
0 -6 4 275.555 11.6518 1
0 6 5 2124.18 13.3714 1
0 -6 6 0.18640 6.69363 1
0 6 -7 1.51696 12.1544 1
2 -6 6 4.03999 13.2747 -2
0 6 -8 4.03999 13.2747 1
2 -6 7 279.722 12.0393 -2
0 6 -9 279.722 12.0393 1
0 6 -10 77.2231 8.76939 1
0 6 -11 175.918 9.18188 1
3 -6 9 291.707 13.7077 -2
0 6 -12 291.707 13.7077 1
3 6 10 1086.44 17.0861 -2
0 -6 -13 1086.44 17.0861 1
0 6 14 86.0580 10.5639 1
0 6 -15 74.5392 11.6597 1
4 -6 12 369.760 18.1595 -2
0 6 -16 369.760 18.1595 1
-4 -6 -13 546.925 20.7952 -2
0 6 17 546.925 20.7952 1
0 6 18 10.5865 12.6262 1
0 6 -19 229.866 14.8437 1
5 -6 15-19.8680 19.6387 -2
0 6 -20-19.8680 19.6387 1
5 -6 16 138.009 32.2993 -2
0 6 -21 138.009 32.2993 1
0 6 22-5.30288 53.7581 1
5 -6 17 20.4061 36.0654 -2
0 6 -22 20.4061 36.0654 1
0 6 23 9.73789 24.0665 1
6 -6 18 0.51050 35.8994 -2
0 6 -24 0.51050 35.8994 1
6 -6 19-30.1358 41.1927 -2
0 6 -25-30.1358 41.1927 1
0 7 -1 16.2979 15.1706 1
0 7 2 88.0765 23.8220 1
0 -7 3 172.308 11.3039 1
-1 7 -3 10.7280 11.1123 -2
0 -7 4 10.7280 11.1123 1
0 -7 -5 330.146 11.2702 1
-1 7 -4 438.796 20.0780 -2
0 -7 5 438.796 20.0780 1
0 7 6 1.02625 8.06853 1
0 -7 7 4.78924 8.30492 1
2 -7 6 545.312 18.1735 -2
0 7 -8 545.312 18.1735 1
0 -7 -9-0.19510 19.0649 1
2 -7 7-5.64529 19.8003 -2
0 7 -9-5.64529 19.8003 1
0 7 10-7.62965 8.63073 1
0 7 11 307.038 9.83546 1
3 -7 9 27.6459 12.0491 -2
0 7 -12 27.6459 12.0491 1
3 7 10 26.3301 13.7281 -2
0 -7 -13 26.3301 13.7281 1
0 7 -14 607.325 13.9122 1
0 7 -15 83.5837 11.9588 1
4 -7 12 126.825 17.7780 -2
0 7 -16 126.825 17.7780 1
4 -7 13 87.5756 18.4066 -2
0 7 -17 87.5756 18.4066 1
0 7 18 132.341 13.9604 1
0 7 -19 136.406 14.8290 1
5 -7 15 32.8575 24.4947 -2
0 7 -20 32.8575 24.4947 1
-5 -7 -16 18.6991 26.7914 -2
0 7 21 18.6991 26.7914 1
-5 -7 -17-6.70106 33.6707 -2
0 7 22-6.70106 33.6707 1
0 7 -23 192.012 27.9398 1
6 -7 18 10.7660 40.9805 -2
0 7 -24 10.7660 40.9805 1
6 -7 19 36.0122 43.0496 -2
0 7 -25 36.0122 43.0496 1
0 -8 0 763.653 29.0004 -2
0 8 0 763.653 29.0004 1
0 8 -1 128.246 16.7835 1
0 8 2 567.074 18.7331 1
0 -8 3 1368.35 19.0406 1
-1 -8 -3 874.507 16.8983 -2
0 8 4 874.507 16.8983 1
0 -8 5 71.2256 11.2689 1
-1 8 -4 95.2479 18.4275 -2
0 -8 5 95.2479 18.4275 1
0 -8 6 254.272 9.43516 1
0 -8 7 4.55003 7.87834 1
-2 -8 -6 57.1775 24.5064 -2
0 8 8 57.1775 24.5064 1
0 8 9 33.9200 32.5492 1
2 -8 7 165.016 18.1549 -2
0 8 -9 165.016 18.1549 1
0 8 10 391.325 14.0924 1
0 8 11 19.4495 10.7937 1
-3 -8 -9 473.997 18.4619 -2
0 8 12 473.997 18.4619 1
3 -8 10 32.9182 15.5199 -2
0 8 -13 32.9182 15.5199 1
0 8 14 376.782 13.2690 1
0 8 -15 142.399 12.6723 1
-4 -8 -12 4.62651 18.0172 -2
0 8 16 4.62651 18.0172 1
4 -8 13 32.0033 18.7760 -2
0 8 -17 32.0033 18.7760 1
0 8 -18 65.9151 14.3821 1
0 8 19 127.941 19.1552 1
5 -8 15 245.866 37.3706 -2
0 8 -20 245.866 37.3706 1
-5 -8 -16 57.6461 37.2806 -2
0 8 21 57.6461 37.2806 1
5 -8 17 36.8696 37.8936 -2
0 8 -22 36.8696 37.8936 1
0 8 -23-15.9905 31.6730 1
6 -8 18 47.8882 45.4166 -2
0 8 -24 47.8882 45.4166 1
6 -8 19 18.3517 35.6769 -2
0 8 -25 18.3517 35.6769 1
0 9 1 1516.10 24.3363 1
0 9 2 111.607 16.9777 1
0 -9 3 183.501 12.2552 1
-1 -9 -3 141.236 13.5927 -2
0 9 4 141.236 13.5927 1
0 -9 -5 807.419 15.0676 1
-1 9 -4 1185.53 24.1605 -2
0 -9 5 1185.53 24.1605 1
0 -9 6 53.0287 8.40160 1
0 9 7 625.756 10.8946 1
-2 -9 -6 85.7366 31.1670 -2
0 9 8 85.7366 31.1670 1
-2 -9 -7 15.3491 31.4775 -2
0 9 9 15.3491 31.4775 1
0 -9 -10 62.9869 23.2726 1
0 -9 -11 332.064 14.6130 1
-3 -9 -9 241.300 18.2834 -2
0 9 12 241.300 18.2834 1
3 -9 10 140.715 18.9961 -2
0 9 -13 140.715 18.9961 1
0 9 -14-8.41813 14.0912 1
0 9 -15 103.012 15.3459 1
4 -9 12-7.11515 19.0483 -2
0 9 -16-7.11515 19.0483 1
4 -9 13 381.860 27.3329 -2
0 9 -17 381.860 27.3329 1
0 9 18 46.3864 25.5269 1
0 9 -19 33.1012 25.7873 1
-5 -9 -15 67.9923 37.8665 -2
0 9 20 67.9923 37.8665 1
-5 -9 -16 37.1233 38.4876 -2
0 9 21 37.1233 38.4876 1
5 -9 17-19.4971 39.9364 -2
0 9 -22-19.4971 39.9364 1
0 9 -23 26.9522 33.8470 1
6 -9 18-31.6537 47.3355 -2
0 9 -24-31.6537 47.3355 1
6 -9 19-31.0403 47.9355 -2
0 9 -25-31.0403 47.9355 1
0 -10 0 134.361 26.0360 -2
0 10 0 134.361 26.0360 1
0 10 1 78.2992 18.3087 1
0 10 -2 27.4922 12.3886 1
0 10 3 542.699 14.7695 1
-1 10 -3 41.0143 13.7928 -2
0 -10 4 41.0143 13.7928 1
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9 -8 -5 81.6924 74.0512 1
8 8 -13 41.1269 74.1456 -2
9 -8 -4 41.1269 74.1456 1
9 -8 -3 13.7687 54.8167 1
9 -8 -2-13.9970 55.5521 1
7 8 -15 154.086 77.8820 -2
9 -8 -1 154.086 77.8820 1
7 8 -16 112.731 70.9084 -2
9 -8 0 112.731 70.9084 1
9 -8 1-7.89294 50.0677 1
9 -8 2 63.9343 55.0236 1
6 8 -18 174.994 79.3093 -2
9 -8 3 174.994 79.3093 1
6 8 -19 38.7368 52.1507 -2
9 -8 4 38.7368 52.1507 1
9 -8 5 41.3484 42.3611 1
9 -8 6 11.1809 42.7954 1
5 8 -21 131.270 58.3025 -2
9 -8 7 131.270 58.3025 1
5 -8 -22 125.481 94.1489 -2
9 8 8 125.481 94.1489 1
9 8 9 13.8851 66.4644 1
9 -9 -8-4.86573 62.2365 1
9 -9 -7-7.90859 55.0959 1
9 -9 -6 245.354 55.3581 1
8 9 -12 165.996 79.4179 -2
9 -9 -5 165.996 79.4179 1
8 9 -13 107.558 73.9258 -2
9 -9 -4 107.558 73.9258 1
9 -9 -3 49.5588 57.3215 1
9 -9 -2 24.5011 54.6958 1
7 9 -15 26.4715 62.0171 -2
9 -9 -1 26.4715 62.0171 1
7 9 -16 75.9105 73.5262 -2
9 -9 0 75.9105 73.5262 1
9 -9 1-18.9807 55.7492 1
9 -9 2 25.1332 58.0850 1
6 9 -18-20.3371 78.7872 -2
9 -9 3-20.3371 78.7872 1
6 9 -19 68.9825 55.4132 -2
9 -9 4 68.9825 55.4132 1
9 -9 5 64.5650 45.7849 1
9 9 6 8.82345 66.1516 1
9 -10 -4 33.2492 58.1728 1
9 -10 -3 30.0484 57.3063 1
9 -10 -2-3.84818 57.7891 1
7 10 -15 7.59856 64.5742 -2
9 -10 -1 7.59856 64.5742 1
9 -10 1 18.6329 59.3733 1
10 0 -16 27.5402 56.5570 1
11 0 -7 1.18374 72.9663 -2
10 0 -14 1.18374 72.9663 1
10 0 -12 409.312 55.4569 1
10 0 -10 54.4726 70.8505 -2
10 0 -10 54.4726 70.8505 1
10 0 -8 1.19227 49.4887 1
9 0 -13 74.9880 69.5916 -2
10 0 -6 74.9880 69.5916 1
10 0 -4 229.282 53.2932 1
8 0 -16 50.9096 69.2294 -2
10 0 -2 50.9096 69.2294 1
10 0 0 102.785 53.1289 1
7 0 -19 78.2120 71.8476 -2
10 0 2 78.2120 71.8476 1
10 0 4 46.9320 55.9888 1
6 0 -22 87.9396 65.0419 -2
10 0 6 87.9396 65.0419 1
12 1 -4-32.2215 84.2298 -2
10 -1 -18-32.2215 84.2298 1
10 -1 -17 16.6073 59.1387 1
10 1 -16 88.4298 39.6970 1
11 -1 -6 182.606 53.2478 -2
10 1 -15 182.606 53.2478 1
11 -1 -7-2.95876 53.1303 -2
10 1 -14-2.95876 53.1303 1
10 1 -13 7.23198 37.1522 1
10 1 -12 6.27216 37.0744 1
10 -1 -9 65.4496 49.1651 -2
10 1 -11 65.4496 49.1651 1
10 -1 -10 23.5774 49.3028 -2
10 1 -10 23.5774 49.3028 1
10 -1 -11 124.948 50.3971 -2
10 1 -9 124.948 50.3971 1
10 1 -8-8.91013 35.7549 1
10 1 -7-5.42508 35.6757 1
9 -1 -13 57.5663 48.5612 -2
10 1 -6 57.5663 48.5612 1
9 -1 -14 131.426 50.0904 -2
10 1 -5 131.426 50.0904 1
10 1 -4-13.9639 34.1020 1
10 1 -3 235.307 36.6758 1
8 -1 -16 64.5560 48.4964 -2
10 1 -2 64.5560 48.4964 1
8 -1 -17 25.5691 46.9726 -2
10 1 -1 25.5691 46.9726 1
10 1 0 75.8007 35.3953 1
10 1 1 49.5438 35.4410 1
7 -1 -19 0.56599 48.5576 -2
10 1 2 0.56599 48.5576 1
7 -1 -20 65.6980 50.4506 -2
10 1 3 65.6980 50.4506 1
10 1 4 4.02756 36.9768 1
10 -1 5-17.9622 53.7651 1
6 1 -22 40.0198 37.1339 -2
10 -1 6 40.0198 37.1339 1
6 -1 -23-17.3727 68.5039 -2
10 1 7-17.3727 68.5039 1
10 1 8-5.91126 49.3755 1
10 1 9 177.526 49.5130 1
10 -2 -17 12.6902 64.2370 1
10 -2 -16 27.2074 61.7873 1
11 -2 -6 185.542 54.2309 -2
10 2 -15 185.542 54.2309 1
11 -2 -7 123.921 52.5878 -2
10 2 -14 123.921 52.5878 1
10 2 -13 161.610 38.8276 1
10 2 -12 43.3043 36.7455 1
10 -2 -9 36.8782 50.1650 -2
10 2 -11 36.8782 50.1650 1
10 -2 -10 22.4242 39.7301 -2
10 2 -10 22.4242 39.7301 1
10 -2 -11-18.3221 49.2370 -2
10 2 -9-18.3221 49.2370 1
10 2 -8 71.8373 36.6015 1
10 2 -7 195.086 36.0954 1
9 -2 -13 60.8153 48.5964 -2
10 2 -6 60.8153 48.5964 1
9 -2 -14 91.0629 48.9850 -2
10 2 -5 91.0629 48.9850 1
10 2 -4 45.3959 35.4037 1
10 2 -3 11.1737 35.2628 1
8 -2 -16 31.2328 49.4277 -2
10 2 -2 31.2328 49.4277 1
8 -2 -17-3.62753 48.7046 -2
10 2 -1-3.62753 48.7046 1
10 2 0 2.36899 35.4514 1
10 2 1 35.6077 35.9379 1
7 -2 -19 139.823 52.0492 -2
10 2 2 139.823 52.0492 1
7 2 -20 766.186 78.1777 -2
10 -2 3 766.186 78.1777 1
10 -2 4 72.6591 51.5662 1
10 -2 5-27.7575 53.1893 1
6 2 -22 178.329 52.0650 -2
10 -2 6 178.329 52.0650 1
6 -2 -23-18.1103 71.1560 -2
10 2 7-18.1103 71.1560 1
6 -2 -24 108.731 71.0838 -2
10 2 8 108.731 71.0838 1
10 2 9 29.2319 52.8209 1
5 -2 -25 67.6117 71.0597 -2
10 2 10 67.6117 71.0597 1
11 3 -6 115.389 83.6869 -2
10 -3 -15 115.389 83.6869 1
11 3 -7 89.0374 84.2623 -2
10 -3 -14 89.0374 84.2623 1
10 3 -13 7.33164 36.8056 1
10 3 -12 16.1490 37.2430 1
10 -3 -9 56.4693 49.5349 -2
10 3 -11 56.4693 49.5349 1
10 -3 -10 202.047 42.7170 -2
10 3 -10 202.047 42.7170 1
10 -3 -11 23.8192 50.5721 -2
10 3 -9 23.8192 50.5721 1
10 3 -8 11.1100 35.9352 1
10 3 -7 12.2999 35.0721 1
9 -3 -13 200.466 50.2218 -2
10 3 -6 200.466 50.2218 1
9 -3 -14 93.4173 49.4154 -2
10 3 -5 93.4173 49.4154 1
10 3 -4 3.75498 34.7817 1
10 3 -3 40.2409 35.2201 1
8 -3 -16 62.3309 49.3850 -2
10 3 -2 62.3309 49.3850 1
8 -3 -17 75.9315 48.2867 -2
10 3 -1 75.9315 48.2867 1
10 3 0-6.08504 35.5003 1
10 3 1-6.33206 36.0687 1
7 3 -19 8.00642 70.2647 -2
10 -3 2 8.00642 70.2647 1
7 3 -20 46.4350 71.7872 -2
10 -3 3 46.4350 71.7872 1
10 -3 4 14.4845 55.3527 1
10 -3 5 1.47134 39.7663 1
6 -3 -22-22.6754 75.0140 -2
10 3 6-22.6754 75.0140 1
6 -3 -23 2.12645 64.4985 -2
10 3 7 2.12645 64.4985 1
6 -3 -24 22.2738 79.7510 -2
10 3 8 22.2738 79.7510 1
10 3 9-20.7057 54.0188 1
5 -3 -25 50.3153 78.8605 -2
10 3 10 50.3153 78.8605 1
5 -3 -26 196.588 82.8170 -2
10 3 11 196.588 82.8170 1
10 -4 -13-4.95405 58.6751 1
10 -4 -12 7.90598 61.4272 1
10 -4 -11-22.6914 54.8895 1
10 -4 -9 90.0341 64.0626 -2
10 4 -11 90.0341 64.0626 1
10 -4 -10 149.091 42.8601 -2
10 4 -10 149.091 42.8601 1
10 -4 -11 34.3891 49.9126 -2
10 4 -9 34.3891 49.9126 1
10 4 -8 36.2418 34.0800 1
10 4 -7 27.0945 36.0910 1
9 -4 -13-2.68069 48.6459 -2
10 4 -6-2.68069 48.6459 1
9 -4 -14 45.6694 49.3311 -2
10 4 -5 45.6694 49.3311 1
10 4 -4 2.44845 34.1334 1
10 4 -3 4.07342 35.1923 1
8 -4 -16 401.020 51.8458 -2
10 4 -2 401.020 51.8458 1
8 -4 -17 68.4363 51.3963 -2
10 4 -1 68.4363 51.3963 1
10 -4 0 18.7351 52.0145 1
10 -4 1 16.6064 53.7312 1
7 4 -19 392.491 78.9964 -2
10 -4 2 392.491 78.9964 1
7 4 -20 158.529 82.9288 -2
10 -4 3 158.529 82.9288 1
10 -4 4 3.25761 58.6176 1
10 4 5 97.7918 58.5578 1
6 -4 -22 32.6376 82.5676 -2
10 4 6 32.6376 82.5676 1
6 -4 -23 53.7183 83.5922 -2
10 4 7 53.7183 83.5922 1
6 -4 -24 102.171 85.2740 -2
10 4 8 102.171 85.2740 1
10 4 9 44.7310 60.6975 1
5 -4 -25 113.386 82.4815 -2
10 4 10 113.386 82.4815 1
5 -4 -26 153.880 85.5285 -2
10 4 11 153.880 85.5285 1
10 4 12-36.6754 59.8139 1
10 5 -9 235.793 81.9309 -2
10 -5 -11 235.793 81.9309 1
10 5 -10-1.42220 77.7305 -2
10 -5 -10-1.42220 77.7305 1
10 5 -11 91.1820 80.5358 -2
10 -5 -9 91.1820 80.5358 1
10 5 -8 540.980 40.6371 1
10 5 -7 9.11121 33.7976 1
9 -5 -13 255.864 50.5720 -2
10 5 -6 255.864 50.5720 1
9 -5 -14 17.3124 49.5416 -2
10 5 -5 17.3124 49.5416 1
10 5 -4 99.0987 37.1223 1
10 -5 -3-1.29357 57.3291 1
8 5 -16 74.4414 78.4414 -2
10 -5 -2 74.4414 78.4414 1
8 5 -17 28.8025 76.4903 -2
10 -5 -1 28.8025 76.4903 1
10 -5 0 20.5184 57.6417 1
10 -5 1-4.78754 56.4276 1
7 5 -19 112.040 79.2753 -2
10 -5 2 112.040 79.2753 1
10 5 5 21.5707 61.3299 1
6 -5 -22-62.4179 85.6823 -2
10 5 6-62.4179 85.6823 1
6 -5 -23 53.3156 89.4529 -2
10 5 7 53.3156 89.4529 1
6 -5 -24 184.873 89.4780 -2
10 5 8 184.873 89.4780 1
10 5 9 36.8251 63.0850 1
5 -5 -25 233.109 89.6537 -2
10 5 10 233.109 89.6537 1
5 -5 -26 127.509 94.0429 -2
10 5 11 127.509 94.0429 1
10 5 12 76.6989 66.7589 1
10 -6 -9 11.9755 59.4202 1
10 -6 -8 142.481 60.0549 1
10 6 -7 62.5893 34.9524 1
9 6 -13 79.6479 80.2071 -2
10 -6 -6 79.6479 80.2071 1
9 6 -14 131.123 78.6218 -2
10 -6 -5 131.123 78.6218 1
10 -6 -4 39.9788 59.9513 1
10 -6 -3 121.457 59.0583 1
8 6 -16 284.670 78.8940 -2
10 -6 -2 284.670 78.8940 1
8 6 -17 218.140 82.3101 -2
10 -6 -1 218.140 82.3101 1
10 -6 0 573.653 64.7613 1
10 -6 1 30.4341 60.1585 1
10 6 5-29.8704 64.8157 1
6 -6 -22-90.1426 90.5911 -2
10 6 6-90.1426 90.5911 1
6 -6 -23 86.1044 93.2150 -2
10 6 7 86.1044 93.2150 1
6 -6 -24-25.1656 97.6255 -2
10 6 8-25.1656 97.6255 1
10 6 9 126.202 70.8428 1
5 -6 -25 172.384 93.8179 -2
10 6 10 172.384 93.8179 1
10 7 4 138.391 70.4025 1
10 7 5 23.8695 68.0165 1
6 -7 -22 46.1799 97.7197 -2
10 7 6 46.1799 97.7197 1
11 0 -13 112.567 62.5384 1
11 0 -11 81.0675 82.5989 -2
11 0 -11 81.0675 82.5989 1
11 0 -9-20.6276 58.0657 1
10 0 -14 15.6625 79.7751 -2
11 0 -7 15.6625 79.7751 1
11 0 -5 109.051 57.8304 1
9 0 -17 488.728 87.9722 -2
11 0 -3 488.728 87.9722 1
11 0 -1 22.1733 57.7795 1
11 1 -14 43.7530 59.2029 1
11 1 -13 52.7458 42.7769 1
11 -1 -12 67.6271 62.6860 1
11 -1 -10 31.2967 81.9433 -2
11 1 -12 31.2967 81.9433 1
11 -1 -11 41.2205 57.6422 -2
11 1 -11 41.2205 57.6422 1
11 -1 -12 44.2288 82.3028 -2
11 1 -10 44.2288 82.3028 1
11 1 -9 4.76271 41.7845 1
11 1 -8 297.064 43.1276 1
10 -1 -14-10.9542 57.0178 -2
11 1 -7-10.9542 57.0178 1
10 -1 -15 57.7242 57.7582 -2
11 1 -6 57.7242 57.7582 1
11 1 -5 29.2352 40.6800 1
11 1 -4 1.35811 42.1425 1
9 -1 -17-11.0184 55.1502 -2
11 1 -3-11.0184 55.1502 1
9 -1 -18-4.47167 78.1853 -2
11 1 -2-4.47167 78.1853 1
11 1 -1-9.23027 40.3740 1
11 1 0 28.8818 60.2468 1
8 -1 -20 67.7727 80.7652 -2
11 1 1 67.7727 80.7652 1
7 -1 -23-127.496 79.2149 -2
11 1 5-127.496 79.2149 1
11 -2 -10 47.5748 79.3346 -2
11 2 -12 47.5748 79.3346 1
11 -2 -11-14.3893 77.6451 -2
11 2 -11-14.3893 77.6451 1
11 -2 -12 101.330 80.8369 -2
11 2 -10 101.330 80.8369 1
11 2 -9 26.6031 41.3542 1
11 2 -8 88.9146 41.6189 1
10 -2 -14 27.5121 49.8919 -2
11 2 -7 27.5121 49.8919 1
10 -2 -15 213.211 80.0085 -2
11 2 -6 213.211 80.0085 1
11 2 -5 0.05716 40.1057 1
11 2 -4 52.1021 41.9150 1
9 -2 -17 52.2687 56.5109 -2
11 2 -3 52.2687 56.5109 1
9 -2 -18 313.110 80.3611 -2
11 2 -2 313.110 80.3611 1
11 2 -1 200.663 60.4763 1
11 2 0 43.0154 57.4613 1
8 -2 -20 226.684 85.0853 -2
11 2 1 226.684 85.0853 1
7 -2 -23 56.5547 83.9177 -2
11 2 5 56.5547 83.9177 1
7 -2 -24 37.7911 84.3582 -2
11 2 6 37.7911 84.3582 1
11 3 -9 11.4332 56.3989 1
11 3 -8 27.7844 56.8764 1
10 -3 -14 52.9477 59.1216 -2
11 3 -7 52.9477 59.1216 1
10 -3 -15 173.101 77.2700 -2
11 3 -6 173.101 77.2700 1
11 3 -5 121.039 58.1929 1
11 3 -4-17.7311 55.5639 1
9 -3 -17-5.94272 76.8314 -2
11 3 -3-5.94272 76.8314 1
9 -3 -18 252.824 81.2210 -2
11 3 -2 252.824 81.2210 1
11 3 -1 37.7606 59.3215 1
7 -3 -23-26.8034 86.9451 -2
11 3 5-26.8034 86.9451 1
7 -3 -24 0.66579 74.9031 -2
11 3 6 0.66579 74.9031 1
11 3 7 72.2093 62.0845 1
11 4 -8 25.6276 55.4899 1
10 -4 -14 241.980 77.6332 -2
11 4 -7 241.980 77.6332 1
10 -4 -15 58.5044 77.8085 -2
11 4 -6 58.5044 77.8085 1
11 4 -5-4.78660 53.3168 1
11 4 -4 49.3291 57.4618 1
9 -4 -17 17.9357 78.6372 -2
11 4 -3 17.9357 78.6372 1
7 -4 -23 42.1969 89.5017 -2
11 4 5 42.1969 89.5017 1
7 -4 -24 24.0196 76.9022 -2
11 4 6 24.0196 76.9022 1
11 4 8 96.7277 67.2844 1
11 5 -5 33.4318 58.3348 1
11 5 4-89.9456 71.1882 1
7 -5 -23 154.490 97.6975 -2
11 5 5 154.490 97.6975 1
11 5 6-26.3246 69.4979 1
0 0 0 0.00000 0.00000 0
TITL UM3_twin1_hklf4 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073 9.006118 15.105283 21.248714 90.0000 96.7520 90.0000
ZERR 8.00 0.000656 0.001042 0.001438 0.0000 0.0067 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N Cl
UNIT 128.00 160.00 32.00 16.00
REM CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
TREF
HKLF 5
BASF 0.31486
END
;
_shelx_hkl_checksum 82734
_shelx_res_file
;
TITL um3_twin1_hklf4_a.res in P2(1)/n
(i).res
created by SHELXL-2016/6 at 21:58:05 on 10-Jun-2026
REM Old TITL UM3_twin1_hklf4 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.202, Rweak 0.021, Alpha 0.049, Orientation as input
REM Formula found by SHELXT: C27 N11 Cl2
CELL 0.71073 9.006118 15.105283 21.248714 90 96.752 90
ZERR 4 0.000656 0.001042 0.001438 0 0.0067 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl N O
UNIT 104 136 8 24 24
EQIV $1 1-X,1-Y,1-Z
EQIV $2 0.5-X,0.5+Y,0.5-Z
L.S. 12 0 0
PLAN 2
SIZE 0.054 0.09 0.382
TEMP -123
CONF
HTAB O1 O5
HTAB O2 O1
HTAB O2 O6
HTAB O3 Cl2_$1
HTAB O3 O2
HTAB O5 Cl1_$2
HTAB O5 O4
HTAB O6 Cl1
HTAB O6 O3_$1
BOND $H
list 4
fmap 2 53
acta 52
MORE -1
OMIT -5 -11 -1
OMIT 2 -1 -11
REM
REM
REM
WGHT 0.035400
BASF 0.29222
FVAR 0.57044
CL1 3 0.341590 0.449246 0.278637 11.00000 0.01743 0.02269 =
0.02090 -0.00436 0.00296 -0.00043
CL2 3 0.342295 0.124878 0.454453 11.00000 0.02625 0.02834 =
0.02128 -0.00172 0.00588 -0.00601
AFIX 6
O1 5 0.396883 0.693670 0.309243 11.00000 0.02341 0.02681 =
0.06674 0.01010 -0.00404 0.00020
H1A 2 0.391339 0.751196 0.309624 11.00000 -1.50000
AFIX 6
O2 5 0.344080 0.652004 0.437519 11.00000 0.05862 0.03388 =
0.05417 0.00688 -0.00432 -0.00391
H2A 2 0.378637 0.665517 0.402141 11.00000 -1.50000
H2B 2 0.341652 0.594725 0.441537 11.00000 -1.50000
AFIX 6
O3 5 0.611285 0.675442 0.511388 11.00000 0.04431 0.02800 =
0.03261 -0.00059 0.00607 0.00086
H3A 2 0.631277 0.728534 0.525820 11.00000 -1.50000
H3B 2 0.522942 0.674898 0.489763 11.00000 -1.50000
AFIX 6
O4 5 0.369487 0.915685 0.443297 11.00000 0.04714 0.03398 =
0.03510 -0.00822 -0.00999 0.00095
H4A 2 0.445418 0.902545 0.470926 11.00000 -1.50000
H4B 2 0.361142 0.972962 0.445853 11.00000 -1.50000
AFIX 6
O5 5 0.411391 0.875225 0.320041 11.00000 0.01954 0.02865 =
0.02692 -0.00174 -0.00207 0.00430
H5A 2 0.393442 0.894352 0.357044 11.00000 -1.50000
H5B 2 0.341090 0.898619 0.293589 11.00000 -1.50000
AFIX 6
O6 5 0.314080 0.472813 0.420803 11.00000 0.03367 0.03093 =
0.01836 0.00350 0.00591 -0.00233
H6A 2 0.343403 0.426310 0.443087 11.00000 -1.50000
H6B 2 0.326415 0.463805 0.381280 11.00000 -1.50000
AFIX 0
N1 4 0.750976 0.755807 0.318692 11.00000 0.01446 0.01561 =
0.01267 0.00108 0.00813 0.00170
N2 4 0.725184 0.799111 0.184632 11.00000 0.01086 0.01116 =
0.01389 0.00119 0.00525 0.00235
N3 4 0.951322 0.752222 0.183908 11.00000 0.01043 0.01378 =
0.01758 0.00176 0.00614 0.00284
N4 4 1.008032 0.585188 0.255508 11.00000 0.00873 0.01472 =
0.01142 0.00107 0.00225 0.00338
N5 4 0.829842 0.551060 0.310921 11.00000 0.00789 0.01271 =
0.01032 -0.00002 0.00196 -0.00161
N6 4 0.622886 0.597149 0.197620 11.00000 0.00881 0.01686 =
0.02077 -0.00026 0.00253 0.00055
C1 1 0.761172 0.759611 0.382131 11.00000 0.01931 0.02213 =
0.02248 0.00019 0.00889 0.00142
AFIX 43
H1 2 0.677703 0.740553 0.402076 11.00000 -1.20000
AFIX 0
C2 1 0.885871 0.789602 0.420094 11.00000 0.02560 0.02139 =
0.01737 -0.00095 0.00666 0.00231
AFIX 43
H2 2 0.888213 0.789370 0.464908 11.00000 -1.20000
AFIX 0
C3 1 1.005907 0.819628 0.392543 11.00000 0.02201 0.02036 =
0.02190 -0.00253 0.00204 -0.00444
AFIX 43
H3 2 1.093105 0.840312 0.417761 11.00000 -1.20000
AFIX 0
C4 1 0.997666 0.819260 0.326537 11.00000 0.01528 0.01974 =
0.01833 0.00121 0.00754 -0.00314
AFIX 43
H4 2 1.077720 0.841562 0.305784 11.00000 -1.20000
AFIX 0
C5 1 0.870714 0.785796 0.292148 11.00000 0.01033 0.00915 =
0.01609 -0.00058 0.00444 0.00477
C6 1 0.851475 0.780328 0.222281 11.00000 0.01238 0.00760 =
0.01707 0.00156 0.00494 -0.00150
C7 1 0.589305 0.831282 0.200134 11.00000 0.01066 0.01484 =
0.02485 0.00234 0.01102 0.00216
AFIX 43
H7 2 0.575635 0.843549 0.242923 11.00000 -1.20000
AFIX 0
C8 1 0.478212 0.844565 0.153370 11.00000 0.01514 0.01771 =
0.03090 0.00537 0.00385 0.00504
AFIX 43
H8 2 0.385170 0.866297 0.163785 11.00000 -1.20000
AFIX 0
C9 1 0.494357 0.827339 0.088664 11.00000 0.01996 0.02224 =
0.02638 0.00646 -0.00386 0.00524
AFIX 43
H9 2 0.413001 0.837278 0.056747 11.00000 -1.20000
AFIX 0
C10 1 0.626423 0.796687 0.072857 11.00000 0.02797 0.02094 =
0.01594 0.00644 0.00589 0.00399
AFIX 43
H10 2 0.638820 0.785341 0.029810 11.00000 -1.20000
AFIX 0
C11 1 0.745346 0.781824 0.121151 11.00000 0.01736 0.01466 =
0.01432 0.00396 0.00747 0.00172
C12 1 0.888533 0.752730 0.122429 11.00000 0.01400 0.01695 =
0.01464 0.00157 0.00431 0.00046
AFIX 43
H12 2 0.936291 0.735764 0.086739 11.00000 -1.20000
AFIX 0
C13 1 1.101128 0.713858 0.202664 11.00000 0.00692 0.02402 =
0.01787 0.00359 0.00258 0.00131
AFIX 23
H13A 2 1.141404 0.736686 0.244920 11.00000 -1.20000
H13B 2 1.169780 0.732209 0.171945 11.00000 -1.20000
AFIX 0
C14 1 1.093641 0.614357 0.204811 11.00000 0.00489 0.02364 =
0.01204 -0.00014 0.00208 -0.00061
AFIX 23
H14A 2 1.045755 0.591735 0.163619 11.00000 -1.20000
H14B 2 1.196154 0.589822 0.212102 11.00000 -1.20000
AFIX 0
C15 1 0.861987 0.562564 0.251231 11.00000 0.00830 0.00771 =
0.01481 0.00047 0.00351 0.00219
C16 1 0.696393 0.523659 0.332127 11.00000 0.00916 0.01495 =
0.02147 0.00446 0.00517 0.00138
AFIX 43
H16 2 0.610915 0.510540 0.303019 11.00000 -1.20000
AFIX 0
C17 1 0.692284 0.516378 0.394769 11.00000 0.01753 0.02108 =
0.02835 0.01088 0.01695 0.00678
AFIX 43
H17 2 0.601920 0.498198 0.409892 11.00000 -1.20000
AFIX 0
C18 1 0.819200 0.535052 0.439374 11.00000 0.02337 0.02272 =
0.01517 0.00604 0.00757 0.00962
AFIX 43
H18 2 0.811986 0.530007 0.483475 11.00000 -1.20000
AFIX 0
C19 1 0.948861 0.559732 0.419372 11.00000 0.02027 0.02066 =
0.00946 -0.00003 0.00066 0.00594
AFIX 43
H19 2 1.033991 0.571571 0.448994 11.00000 -1.20000
AFIX 0
C20 1 0.957020 0.567884 0.353466 11.00000 0.01116 0.01279 =
0.01460 0.00094 0.00125 0.00513
C21 1 1.067615 0.589042 0.317519 11.00000 0.00798 0.01566 =
0.01444 0.00179 -0.00453 0.00093
AFIX 43
H21 2 1.167919 0.603788 0.332841 11.00000 -1.20000
AFIX 0
C22 1 0.754252 0.556307 0.193463 11.00000 0.01069 0.00865 =
0.01512 0.00149 0.00084 -0.00238
C23 1 0.788326 0.513038 0.139975 11.00000 0.01022 0.01594 =
0.02153 -0.00259 0.00203 0.00150
AFIX 43
H23 2 0.881120 0.483198 0.139762 11.00000 -1.20000
AFIX 0
C24 1 0.684652 0.513947 0.086612 11.00000 0.02714 0.02529 =
0.01585 -0.00934 -0.00022 -0.00562
AFIX 43
H24 2 0.705556 0.486108 0.048541 11.00000 -1.20000
AFIX 0
C25 1 0.551199 0.555890 0.089911 11.00000 0.02302 0.03140 =
0.01849 -0.00111 -0.01013 -0.00321
AFIX 43
H25 2 0.478077 0.558064 0.053876 11.00000 -1.20000
AFIX 0
C26 1 0.523934 0.594800 0.145766 11.00000 0.00766 0.02325 =
0.02641 0.00349 -0.00549 -0.00351
AFIX 43
H26 2 0.429119 0.621606 0.147604 11.00000 -1.20000
AFIX 0
H1B 2 10.494800 10.679000 10.299700 11.00000 -1.50000
HKLF 5
REM um3_twin1_hklf4_a.res in P2(1)/n
REM R1 = 0.0509 for 3396 Fo > 4sig(Fo) and 0.1215 for all 6542 data
REM 380 parameters refined using 0 restraints
END
WGHT 0.0354 0.0000
REM Highest difference peak 0.265, deepest hole -0.338, 1-sigma level 0.067
Q1 1 0.3421 0.9834 0.2604 11.00000 0.05 0.26
Q2 1 0.5990 0.7577 0.5785 11.00000 0.05 0.26
;
_shelx_res_checksum 23311
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1 0.34159(8) 0.44925(5) 0.27864(3) 0.02028(19) Uani d 1 . .
Cl Cl2 0.34229(8) 0.12488(5) 0.45445(4) 0.02505(19) Uani d 1 . .
O O1 0.3969(2) 0.69367(14) 0.30924(12) 0.0397(7) Uani d 1 . .
H H1A 0.391339 0.751196 0.309624 0.060 Uiso d 1 . .
O O2 0.3441(3) 0.65200(15) 0.43752(12) 0.0498(7) Uani d 1 . .
H H2A 0.378637 0.665517 0.402141 0.075 Uiso d 1 . .
H H2B 0.341652 0.594725 0.441537 0.075 Uiso d 1 . .
O O3 0.6113(3) 0.67544(13) 0.51139(11) 0.0349(6) Uani d 1 . .
H H3A 0.631277 0.728534 0.525820 0.052 Uiso d 1 . .
H H3B 0.522942 0.674898 0.489763 0.052 Uiso d 1 . .
O O4 0.3695(3) 0.91568(14) 0.44330(11) 0.0399(6) Uani d 1 . .
H H4A 0.445418 0.902545 0.470926 0.060 Uiso d 1 . .
H H4B 0.361142 0.972962 0.445853 0.060 Uiso d 1 . .
O O5 0.4114(2) 0.87522(14) 0.32004(10) 0.0254(5) Uani d 1 . .
H H5A 0.393442 0.894352 0.357044 0.038 Uiso d 1 . .
H H5B 0.341090 0.898619 0.293589 0.038 Uiso d 1 . .
O O6 0.3141(2) 0.47281(13) 0.42080(10) 0.0274(5) Uani d 1 . .
H H6A 0.343403 0.426310 0.443087 0.041 Uiso d 1 . .
H H6B 0.326415 0.463805 0.381280 0.041 Uiso d 1 . .
N N1 0.7510(2) 0.75581(14) 0.31869(11) 0.0137(6) Uani d 1 . .
N N2 0.7252(2) 0.79911(14) 0.18463(11) 0.0117(5) Uani d 1 . .
N N3 0.9513(2) 0.75222(14) 0.18391(11) 0.0136(6) Uani d 1 . .
N N4 1.0080(2) 0.58519(14) 0.25551(10) 0.0115(5) Uani d 1 . .
N N5 0.8298(2) 0.55106(14) 0.31092(10) 0.0102(5) Uani d 1 . .
N N6 0.6229(2) 0.59715(14) 0.19762(11) 0.0154(6) Uani d 1 . .
C C1 0.7612(3) 0.75961(18) 0.38213(15) 0.0208(7) Uani d 1 . .
H H1 0.677703 0.740553 0.402076 0.025 Uiso calc 1 . .
C C2 0.8859(3) 0.78960(19) 0.42009(14) 0.0211(8) Uani d 1 . .
H H2 0.888213 0.789370 0.464908 0.025 Uiso calc 1 . .
C C3 1.0059(3) 0.81963(18) 0.39254(14) 0.0215(8) Uani d 1 . .
H H3 1.093105 0.840312 0.417761 0.026 Uiso calc 1 . .
C C4 0.9977(3) 0.81926(18) 0.32654(13) 0.0173(7) Uani d 1 . .
H H4 1.077720 0.841562 0.305784 0.021 Uiso calc 1 . .
C C5 0.8707(3) 0.78580(17) 0.29215(13) 0.0116(7) Uani d 1 . .
C C6 0.8515(3) 0.78033(17) 0.22228(13) 0.0121(7) Uani d 1 . .
C C7 0.5893(3) 0.83128(17) 0.20013(14) 0.0161(7) Uani d 1 . .
H H7 0.575635 0.843549 0.242923 0.019 Uiso calc 1 . .
C C8 0.4782(3) 0.84457(18) 0.15337(14) 0.0212(7) Uani d 1 . .
H H8 0.385170 0.866297 0.163785 0.025 Uiso calc 1 . .
C C9 0.4944(3) 0.82734(19) 0.08866(15) 0.0234(8) Uani d 1 . .
H H9 0.413001 0.837278 0.056747 0.028 Uiso calc 1 . .
C C10 0.6264(3) 0.79669(19) 0.07286(14) 0.0214(8) Uani d 1 . .
H H10 0.638820 0.785341 0.029810 0.026 Uiso calc 1 . .
C C11 0.7453(3) 0.78182(18) 0.12115(13) 0.0150(7) Uani d 1 . .
C C12 0.8885(3) 0.75273(17) 0.12243(14) 0.0150(7) Uani d 1 . .
H H12 0.936291 0.735764 0.086739 0.018 Uiso calc 1 . .
C C13 1.1011(3) 0.71386(18) 0.20266(14) 0.0162(7) Uani d 1 . .
H H13A 1.141404 0.736686 0.244920 0.019 Uiso calc 1 . .
H H13B 1.169780 0.732209 0.171945 0.019 Uiso calc 1 . .
C C14 1.0936(3) 0.61436(17) 0.20481(13) 0.0134(6) Uani d 1 . .
H H14A 1.045755 0.591735 0.163619 0.016 Uiso calc 1 . .
H H14B 1.196154 0.589822 0.212102 0.016 Uiso calc 1 . .
C C15 0.8620(3) 0.56256(16) 0.25123(13) 0.0101(6) Uani d 1 . .
C C16 0.6964(3) 0.52366(17) 0.33213(14) 0.0149(7) Uani d 1 . .
H H16 0.610915 0.510540 0.303019 0.018 Uiso calc 1 . .
C C17 0.6923(3) 0.51638(18) 0.39477(14) 0.0212(7) Uani d 1 . .
H H17 0.601920 0.498198 0.409892 0.025 Uiso calc 1 . .
C C18 0.8192(3) 0.53505(18) 0.43937(14) 0.0200(7) Uani d 1 . .
H H18 0.811986 0.530007 0.483475 0.024 Uiso calc 1 . .
C C19 0.9489(3) 0.55973(18) 0.41937(13) 0.0169(7) Uani d 1 . .
H H19 1.033991 0.571571 0.448994 0.020 Uiso calc 1 . .
C C20 0.9570(3) 0.56788(17) 0.35347(13) 0.0129(7) Uani d 1 . .
C C21 1.0676(3) 0.58904(17) 0.31752(13) 0.0132(7) Uani d 1 . .
H H21 1.167919 0.603788 0.332841 0.016 Uiso calc 1 . .
C C22 0.7543(3) 0.55631(17) 0.19346(12) 0.0115(6) Uani d 1 . .
C C23 0.7883(3) 0.51304(17) 0.13998(13) 0.0159(7) Uani d 1 . .
H H23 0.881120 0.483198 0.139762 0.019 Uiso calc 1 . .
C C24 0.6847(3) 0.51395(19) 0.08661(14) 0.0230(8) Uani d 1 . .
H H24 0.705556 0.486108 0.048541 0.028 Uiso calc 1 . .
C C25 0.5512(3) 0.5559(2) 0.08991(14) 0.0253(8) Uani d 1 . .
H H25 0.478077 0.558064 0.053876 0.030 Uiso calc 1 . .
C C26 0.5239(3) 0.59480(18) 0.14577(14) 0.0197(7) Uani d 1 . .
H H26 0.429119 0.621606 0.147604 0.024 Uiso calc 1 . .
H H1B 0.494800 0.679000 0.299700 0.030 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
Cl1 0.0174(4) 0.0227(4) 0.0209(4) -0.0004(3) 0.0030(3) -0.0044(3)
Cl2 0.0263(5) 0.0283(4) 0.0213(4) -0.0060(4) 0.0059(4) -0.0017(4)
O1 0.0234(14) 0.0268(13) 0.0667(18) 0.0002(11) -0.0040(13) 0.0101(13)
O2 0.0586(18) 0.0339(15) 0.0542(18) -0.0039(14) -0.0043(15) 0.0069(12)
O3 0.0443(17) 0.0280(13) 0.0326(15) 0.0009(12) 0.0061(12) -0.0006(11)
O4 0.0471(18) 0.0340(14) 0.0351(15) 0.0009(12) -0.0100(13) -0.0082(11)
O5 0.0195(13) 0.0286(12) 0.0269(13) 0.0043(10) -0.0021(10) -0.0017(11)
O6 0.0337(14) 0.0309(13) 0.0184(12) -0.0023(11) 0.0059(11) 0.0035(10)
N1 0.0145(15) 0.0156(13) 0.0127(14) 0.0017(10) 0.0081(12) 0.0011(11)
N2 0.0109(14) 0.0112(13) 0.0139(14) 0.0023(10) 0.0052(12) 0.0012(11)
N3 0.0104(14) 0.0138(13) 0.0176(15) 0.0028(10) 0.0061(12) 0.0018(11)
N4 0.0087(14) 0.0147(13) 0.0114(13) 0.0034(10) 0.0023(11) 0.0011(10)
N5 0.0079(13) 0.0127(12) 0.0103(13) -0.0016(11) 0.0020(11) 0.0000(11)
N6 0.0088(14) 0.0169(13) 0.0208(14) 0.0005(11) 0.0025(11) -0.0003(11)
C1 0.0193(19) 0.0221(18) 0.0225(19) 0.0014(14) 0.0089(16) 0.0002(14)
C2 0.026(2) 0.0214(18) 0.0174(18) 0.0023(15) 0.0067(16) -0.0010(14)
C3 0.0220(19) 0.0204(18) 0.0219(19) -0.0044(14) 0.0020(15) -0.0025(14)
C4 0.0153(18) 0.0197(17) 0.0183(18) -0.0031(13) 0.0075(14) 0.0012(14)
C5 0.0103(17) 0.0092(14) 0.0161(17) 0.0048(12) 0.0044(13) -0.0006(13)
C6 0.0124(17) 0.0076(14) 0.0171(17) -0.0015(12) 0.0049(14) 0.0016(13)
C7 0.0107(17) 0.0148(16) 0.0248(18) 0.0022(13) 0.0110(15) 0.0023(14)
C8 0.0151(18) 0.0177(17) 0.0309(19) 0.0050(13) 0.0038(16) 0.0054(14)
C9 0.0200(19) 0.0222(18) 0.0264(19) 0.0052(14) -0.0039(15) 0.0065(15)
C10 0.028(2) 0.0209(18) 0.0159(18) 0.0040(15) 0.0059(16) 0.0064(14)
C11 0.0174(18) 0.0147(16) 0.0143(17) 0.0017(13) 0.0075(14) 0.0040(13)
C12 0.0140(18) 0.0169(17) 0.0146(18) 0.0005(13) 0.0043(14) 0.0016(13)
C13 0.0069(17) 0.0240(17) 0.0179(17) 0.0013(13) 0.0026(13) 0.0036(14)
C14 0.0049(15) 0.0236(17) 0.0120(15) -0.0006(13) 0.0021(12) -0.0001(14)
C15 0.0083(16) 0.0077(14) 0.0148(16) 0.0022(12) 0.0035(13) 0.0005(13)
C16 0.0092(16) 0.0150(15) 0.0215(18) 0.0014(13) 0.0052(14) 0.0045(13)
C17 0.0175(18) 0.0211(17) 0.028(2) 0.0068(14) 0.0169(16) 0.0109(15)
C18 0.0234(19) 0.0227(18) 0.0152(17) 0.0096(14) 0.0076(15) 0.0060(14)
C19 0.0203(19) 0.0207(17) 0.0095(16) 0.0059(14) 0.0007(14) 0.0000(13)
C20 0.0112(17) 0.0128(16) 0.0146(16) 0.0051(12) 0.0013(13) 0.0009(13)
C21 0.0080(16) 0.0157(16) 0.0144(16) 0.0009(12) -0.0045(14) 0.0018(12)
C22 0.0107(16) 0.0087(14) 0.0151(16) -0.0024(13) 0.0008(13) 0.0015(13)
C23 0.0102(16) 0.0159(16) 0.0215(18) 0.0015(13) 0.0020(14) -0.0026(14)
C24 0.027(2) 0.0253(18) 0.0159(18) -0.0056(15) -0.0002(15) -0.0093(14)
C25 0.023(2) 0.0314(19) 0.0185(18) -0.0032(16) -0.0101(15) -0.0011(16)
C26 0.0077(16) 0.0232(18) 0.0264(19) -0.0035(13) -0.0055(14) 0.0035(14)
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'
Cl Cl 0.1484 0.1585 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 29 0.0499
-1 -14 -22 0.1167
0 -19 14 0.2015
0 21 -3 0.1650
-1 -3 -29 0.0395
-13 -1 3 0.0271
13 1 -3 0.0271
-8 1 25 0.0332
-10 -9 15 0.0815
5 -1 -29 0.0270
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
H1A O1 H1B . . 106.8 ?
H2A O2 H2B . . 109.5 ?
H3A O3 H3B . . 109.5 ?
H4A O4 H4B . . 104.6 ?
H5A O5 H5B . . 104.5 ?
H6A O6 H6B . . 109.5 ?
C1 N1 C5 . . 116.2(2) ?
C6 N2 C7 . . 129.8(2) ?
C6 N2 C11 . . 109.7(2) ?
C7 N2 C11 . . 120.5(2) ?
C6 N3 C12 . . 110.3(2) ?
C6 N3 C13 . . 127.7(2) ?
C12 N3 C13 . . 121.6(2) ?
C15 N4 C14 . . 128.2(2) ?
C15 N4 C21 . . 110.2(2) ?
C21 N4 C14 . . 121.1(2) ?
C15 N5 C16 . . 129.2(2) ?
C15 N5 C20 . . 109.6(2) ?
C16 N5 C20 . . 121.1(2) ?
C26 N6 C22 . . 116.1(2) ?
N1 C1 H1 . . 118.1 ?
N1 C1 C2 . . 123.8(3) ?
C2 C1 H1 . . 118.1 ?
C1 C2 H2 . . 120.4 ?
C3 C2 C1 . . 119.3(3) ?
C3 C2 H2 . . 120.4 ?
C2 C3 H3 . . 120.7 ?
C2 C3 C4 . . 118.6(3) ?
C4 C3 H3 . . 120.7 ?
C3 C4 H4 . . 120.8 ?
C5 C4 C3 . . 118.5(3) ?
C5 C4 H4 . . 120.8 ?
N1 C5 C4 . . 123.6(3) ?
N1 C5 C6 . . 113.3(2) ?
C4 C5 C6 . . 123.1(3) ?
N2 C6 N3 . . 106.5(2) ?
N2 C6 C5 . . 125.4(2) ?
N3 C6 C5 . . 128.1(3) ?
N2 C7 H7 . . 120.7 ?
C8 C7 N2 . . 118.5(3) ?
C8 C7 H7 . . 120.7 ?
C7 C8 H8 . . 118.8 ?
C7 C8 C9 . . 122.5(3) ?
C9 C8 H8 . . 118.8 ?
C8 C9 H9 . . 120.2 ?
C10 C9 C8 . . 119.6(3) ?
C10 C9 H9 . . 120.2 ?
C9 C10 H10 . . 120.4 ?
C9 C10 C11 . . 119.2(3) ?
C11 C10 H10 . . 120.4 ?
N2 C11 C10 . . 119.7(2) ?
C12 C11 N2 . . 105.7(2) ?
C12 C11 C10 . . 134.7(3) ?
N3 C12 H12 . . 126.1 ?
C11 C12 N3 . . 107.9(3) ?
C11 C12 H12 . . 126.1 ?
N3 C13 H13A . . 109.5 ?
N3 C13 H13B . . 109.5 ?
N3 C13 C14 . . 110.9(2) ?
H13A C13 H13B . . 108.0 ?
C14 C13 H13A . . 109.5 ?
C14 C13 H13B . . 109.5 ?
N4 C14 C13 . . 110.6(2) ?
N4 C14 H14A . . 109.5 ?
N4 C14 H14B . . 109.5 ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 108.1 ?
N4 C15 C22 . . 127.7(2) ?
N5 C15 N4 . . 106.6(2) ?
N5 C15 C22 . . 125.7(2) ?
N5 C16 H16 . . 121.0 ?
C17 C16 N5 . . 118.1(3) ?
C17 C16 H16 . . 121.0 ?
C16 C17 H17 . . 119.0 ?
C16 C17 C18 . . 122.1(3) ?
C18 C17 H17 . . 119.0 ?
C17 C18 H18 . . 119.9 ?
C19 C18 C17 . . 120.3(3) ?
C19 C18 H18 . . 119.9 ?
C18 C19 H19 . . 120.5 ?
C18 C19 C20 . . 119.1(3) ?
C20 C19 H19 . . 120.5 ?
N5 C20 C19 . . 119.4(2) ?
C21 C20 N5 . . 106.1(2) ?
C21 C20 C19 . . 134.5(3) ?
N4 C21 H21 . . 126.2 ?
C20 C21 N4 . . 107.5(2) ?
C20 C21 H21 . . 126.2 ?
N6 C22 C15 . . 114.4(2) ?
N6 C22 C23 . . 123.7(3) ?
C23 C22 C15 . . 121.9(2) ?
C22 C23 H23 . . 120.7 ?
C22 C23 C24 . . 118.6(3) ?
C24 C23 H23 . . 120.7 ?
C23 C24 H24 . . 120.8 ?
C25 C24 C23 . . 118.4(3) ?
C25 C24 H24 . . 120.8 ?
C24 C25 H25 . . 120.3 ?
C24 C25 C26 . . 119.4(3) ?
C26 C25 H25 . . 120.3 ?
N6 C26 C25 . . 123.8(3) ?
N6 C26 H26 . . 118.1 ?
C25 C26 H26 . . 118.1 ?
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
O1 H1A . 0.8705 ?
O1 H1B . 0.954(2) ?
O2 H2A . 0.8710 ?
O2 H2B . 0.8699 ?
O3 H3A . 0.8698 ?
O3 H3B . 0.8708 ?
O4 H4A . 0.8702 ?
O4 H4B . 0.8707 ?
O5 H5A . 0.8705 ?
O5 H5B . 0.8706 ?
O6 H6A . 0.8706 ?
O6 H6B . 0.8707 ?
N1 C1 . 1.342(4) y
N1 C5 . 1.352(3) y
N2 C6 . 1.342(3) y
N2 C7 . 1.392(3) y
N2 C11 . 1.407(3) y
N3 C6 . 1.351(3) y
N3 C12 . 1.361(3) y
N3 C13 . 1.479(3) y
N4 C14 . 1.464(3) y
N4 C15 . 1.352(3) y
N4 C21 . 1.364(3) y
N5 C15 . 1.345(3) y
N5 C16 . 1.395(3) y
N5 C20 . 1.397(3) y
N6 C22 . 1.346(3) y
N6 C26 . 1.334(3) y
C1 H1 . 0.9500 ?
C1 C2 . 1.380(4) y
C2 H2 . 0.9500 ?
C2 C3 . 1.366(4) y
C3 H3 . 0.9500 ?
C3 C4 . 1.396(4) y
C4 H4 . 0.9500 ?
C4 C5 . 1.378(4) y
C5 C6 . 1.477(4) y
C7 H7 . 0.9500 ?
C7 C8 . 1.340(4) y
C8 H8 . 0.9500 ?
C8 C9 . 1.423(4) y
C9 H9 . 0.9500 ?
C9 C10 . 1.355(4) y
C10 H10 . 0.9500 ?
C10 C11 . 1.411(4) y
C11 C12 . 1.360(4) y
C12 H12 . 0.9500 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C13 C14 . 1.505(4) y
C14 H14A . 0.9900 ?
C14 H14B . 0.9900 ?
C15 C22 . 1.475(4) y
C16 H16 . 0.9500 ?
C16 C17 . 1.340(4) y
C17 H17 . 0.9500 ?
C17 C18 . 1.425(4) y
C18 H18 . 0.9500 ?
C18 C19 . 1.342(4) y
C19 H19 . 0.9500 ?
C19 C20 . 1.416(4) y
C20 C21 . 1.363(4) y
C21 H21 . 0.9500 ?
C22 C23 . 1.377(4) y
C23 H23 . 0.9500 ?
C23 C24 . 1.382(4) y
C24 H24 . 0.9500 ?
C24 C25 . 1.368(4) y
C25 H25 . 0.9500 ?
C25 C26 . 1.372(4) y
C26 H26 . 0.9500 ?
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
O1 H1A O5 . 0.87 1.89 2.754(3) 169.9
O2 H2A O1 . 0.87 2.04 2.891(4) 163.6
O2 H2B O6 . 0.87 1.90 2.739(3) 160.7
O3 H3A Cl2 3_666 0.87 2.26 3.119(2) 168.9
O3 H3B O2 . 0.87 1.88 2.737(4) 168.7
O5 H5A O4 . 0.87 1.90 2.758(3) 169.4
O5 H5B Cl1 2 0.87 2.25 3.117(2) 175.7
O6 H6A O3 3_666 0.87 1.84 2.705(3) 175.1
O6 H6B Cl1 . 0.87 2.21 3.081(2) 175.0
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
N1 C1 C2 C3 . . . . 1.8(4) ?
N1 C5 C6 N2 . . . . 40.3(4) ?
N1 C5 C6 N3 . . . . -136.2(3) ?
N2 C7 C8 C9 . . . . -0.2(4) ?
N2 C11 C12 N3 . . . . 0.2(3) ?
N3 C13 C14 N4 . . . . -66.3(3) ?
N4 C15 C22 N6 . . . . -132.1(3) ?
N4 C15 C22 C23 . . . . 47.1(4) ?
N5 C15 C22 N6 . . . . 44.1(4) ?
N5 C15 C22 C23 . . . . -136.8(3) ?
N5 C16 C17 C18 . . . . -0.5(4) ?
N5 C20 C21 N4 . . . . 0.2(3) ?
N6 C22 C23 C24 . . . . 2.4(4) ?
C1 N1 C5 C4 . . . . -0.3(4) ?
C1 N1 C5 C6 . . . . -179.6(2) ?
C1 C2 C3 C4 . . . . 0.3(4) ?
C2 C3 C4 C5 . . . . -2.2(4) ?
C3 C4 C5 N1 . . . . 2.3(4) ?
C3 C4 C5 C6 . . . . -178.6(3) ?
C4 C5 C6 N2 . . . . -138.9(3) ?
C4 C5 C6 N3 . . . . 44.5(4) ?
C5 N1 C1 C2 . . . . -1.7(4) ?
C6 N2 C7 C8 . . . . -179.8(3) ?
C6 N2 C11 C10 . . . . 179.9(2) ?
C6 N2 C11 C12 . . . . -0.4(3) ?
C6 N3 C12 C11 . . . . 0.1(3) ?
C6 N3 C13 C14 . . . . 93.3(3) ?
C7 N2 C6 N3 . . . . -179.2(2) ?
C7 N2 C6 C5 . . . . 3.6(4) ?
C7 N2 C11 C10 . . . . -0.4(4) ?
C7 N2 C11 C12 . . . . 179.3(2) ?
C7 C8 C9 C10 . . . . -0.3(4) ?
C8 C9 C10 C11 . . . . 0.5(4) ?
C9 C10 C11 N2 . . . . -0.1(4) ?
C9 C10 C11 C12 . . . . -179.7(3) ?
C10 C11 C12 N3 . . . . 179.8(3) ?
C11 N2 C6 N3 . . . . 0.5(3) ?
C11 N2 C6 C5 . . . . -176.7(3) ?
C11 N2 C7 C8 . . . . 0.6(4) ?
C12 N3 C6 N2 . . . . -0.3(3) ?
C12 N3 C6 C5 . . . . 176.8(3) ?
C12 N3 C13 C14 . . . . -77.9(3) ?
C13 N3 C6 N2 . . . . -172.3(2) ?
C13 N3 C6 C5 . . . . 4.8(4) ?
C13 N3 C12 C11 . . . . 172.6(2) ?
C14 N4 C15 N5 . . . . -172.6(2) ?
C14 N4 C15 C22 . . . . 4.2(4) ?
C14 N4 C21 C20 . . . . 172.9(2) ?
C15 N4 C14 C13 . . . . 96.2(3) ?
C15 N4 C21 C20 . . . . 0.3(3) ?
C15 N5 C16 C17 . . . . 179.4(3) ?
C15 N5 C20 C19 . . . . -180.0(2) ?
C15 N5 C20 C21 . . . . -0.6(3) ?
C15 C22 C23 C24 . . . . -176.6(3) ?
C16 N5 C15 N4 . . . . -176.9(2) ?
C16 N5 C15 C22 . . . . 6.3(4) ?
C16 N5 C20 C19 . . . . -2.1(4) ?
C16 N5 C20 C21 . . . . 177.3(2) ?
C16 C17 C18 C19 . . . . -0.9(4) ?
C17 C18 C19 C20 . . . . 0.7(4) ?
C18 C19 C20 N5 . . . . 0.7(4) ?
C18 C19 C20 C21 . . . . -178.4(3) ?
C19 C20 C21 N4 . . . . 179.4(3) ?
C20 N5 C15 N4 . . . . 0.8(3) ?
C20 N5 C15 C22 . . . . -176.0(2) ?
C20 N5 C16 C17 . . . . 1.9(4) ?
C21 N4 C14 C13 . . . . -74.9(3) ?
C21 N4 C15 N5 . . . . -0.7(3) ?
C21 N4 C15 C22 . . . . 176.0(2) ?
C22 N6 C26 C25 . . . . -1.7(4) ?
C22 C23 C24 C25 . . . . -1.7(4) ?
C23 C24 C25 C26 . . . . -0.6(4) ?
C24 C25 C26 N6 . . . . 2.4(5) ?
C26 N6 C22 C15 . . . . 178.4(2) ?
C26 N6 C22 C23 . . . . -0.7(4) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7078(12)
2 0.2922(12)