#------------------------------------------------------------------------------
#$Date: 2023-04-05 13:15:34 +0200 (Wed, 05 Apr 2023) $
#$Revision: 282400 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022715.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_2022715
loop_
_publ_author_name
Vinaya,
'Basavaraju, Yeriyur B.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Syntheses and crystal structures of four
4-(4-methoxyphenyl)piperazin-1-ium salts: trifluoroacetate,
2,3,4,5,6-pentafluorobenzoate, 4-iodobenzoate, and a polymorph with
4-methylbenzoate
;
_journal_coeditor_code VM2279
_journal_issue 4
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 380
_journal_page_last 385
_journal_paper_doi 10.1107/S2056989023002529
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C11 H17 N2 O +, C7 H4 I O2 -, H2 O'
_chemical_formula_moiety 'C11 H17 N2 O +, C7 H4 I O2 -, H2 O'
_chemical_formula_sum 'C18 H23 I N2 O4'
_chemical_formula_weight 458.28
_chemical_name_systematic
;
4-(4-Methoxyphenyl)piperazin-1-ium 4-iodobenzoate 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-2019/2 and CIFFIX'
_cell_angle_alpha 90
_cell_angle_beta 92.970(3)
_cell_angle_gamma 90
_cell_formula_units_Z 12
_cell_length_a 20.4117(18)
_cell_length_b 7.4255(6)
_cell_length_c 36.796(3)
_cell_measurement_reflns_used 9052
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.49
_cell_measurement_theta_min 2.33
_cell_volume 5569.6(8)
_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),
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and publCIF (Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2019/2 (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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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 0.0556
_diffrn_reflns_av_unetI/netI 0.0489
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 47
_diffrn_reflns_limit_l_min -47
_diffrn_reflns_number 72181
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.658
_diffrn_reflns_theta_min 1.998
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 1.750
_exptl_absorpt_correction_T_max 0.862
_exptl_absorpt_correction_T_min 0.726
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.640
_exptl_crystal_description plate
_exptl_crystal_F_000 2760
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.839
_refine_diff_density_min -0.805
_refine_ls_extinction_coef 0.00017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 729
_refine_ls_number_reflns 12876
_refine_ls_number_restraints 12
_refine_ls_restrained_S_all 1.029
_refine_ls_R_factor_all 0.0507
_refine_ls_R_factor_gt 0.0328
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+1.7628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0637
_refine_ls_wR_factor_ref 0.0687
_reflns_number_gt 10003
_reflns_number_total 12876
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2279sup1.cif
_cod_data_source_block III
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2022715
_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 0.622
_shelx_estimated_absorpt_t_max 0.949
_shelx_hkl_file
;
-2 0 0 186.064 10.0627 2
-2 0 0 190.756 10.2333 3
-2 0 0 188.601 10.6511 4
2 0 0 190.103 10.1330 2
2 0 0 180.447 10.5225 3
2 0 0 212.977 10.9713 4
3 0 0 16.4716 2.19118 4
3 0 0 15.0024 1.77366 2
-3 0 0 13.9758 1.58840 2
-3 0 0 14.4533 1.79019 2
-3 0 0 15.5741 1.78824 3
-3 0 0 15.2679 2.08208 4
3 0 0 13.2476 1.61173 2
3 0 0 15.3237 1.95923 3
-4 0 0 1133.97 57.8131 2
-4 0 0 1151.24 58.2196 3
4 0 0 1159.40 57.8093 2
4 0 0 1141.54 58.0897 2
4 0 0 1213.34 58.3523 3
4 0 0 1187.51 58.8225 4
-4 0 0 1178.00 58.1722 2
5 0 0 313.219 17.0508 2
-5 0 0 324.643 18.1539 4
-5 0 0 311.310 17.4040 2
-5 0 0 296.318 16.9266 2
5 0 0 332.606 18.2899 4
5 0 0 327.178 17.6565 3
5 0 0 326.473 18.0700 2
6 0 0 5638.91 270.950 3
-6 0 0 5314.76 270.734 3
6 0 0 5650.83 271.742 4
7 0 0 2211.08 108.996 2
7 0 0 2261.03 109.869 3
7 0 0 2236.75 110.753 4
-7 0 0 2211.15 109.965 3
-7 0 0 2152.05 109.581 2
7 0 0 2146.38 110.339 2
8 0 0 3033.50 152.734 3
8 0 0 2932.74 149.915 2
8 0 0 3148.13 152.099 4
-8 0 0 3057.74 150.769 2
9 0 0 185.133 12.2355 3
9 0 0 181.243 11.4290 2
-9 0 0 172.822 11.9282 2
9 0 0 181.616 13.1961 4
10 0 0 15.8536 3.05938 2
10 0 0 11.7746 3.04941 3
10 0 0 10.9213 4.03509 4
-10 0 0 8.54356 2.99435 2
11 0 0 336.810 20.4189 2
11 0 0 372.708 21.8555 3
-11 0 0 358.403 21.4758 2
11 0 0 361.892 23.0017 4
12 0 0 838.039 45.9220 4
12 0 0 826.689 44.4744 3
-12 0 0 788.000 43.9949 2
12 0 0 788.321 42.9260 2
13 0 0 1659.09 84.7652 2
13 0 0 1694.03 86.3753 3
-13 0 0 1631.68 85.7223 2
14 0 0 531.227 30.6949 2
-14 0 0 567.420 38.0601 2
14 0 0 535.302 32.1134 3
15 0 0 246.176 23.4842 3
15 0 0 228.718 16.0265 2
-15 0 0 253.888 18.2707 2
-16 0 0 35.3697 6.34491 2
16 0 0 25.2742 5.90061 3
16 0 0 26.0515 4.78625 2
17 0 0 79.1614 8.51812 2
-17 0 0 74.7599 9.48988 2
17 0 0 89.3578 9.66906 3
18 0 0 265.185 19.3612 2
18 0 0 268.383 20.6597 3
-18 0 0 294.135 22.2457 2
19 0 0 166.141 13.7824 2
19 0 0 186.628 15.5894 3
-19 0 0 139.780 16.3138 2
-20 0 0 315.806 28.8048 2
20 0 0 423.263 26.1124 2
20 0 0 402.571 27.2119 3
21 0 0 152.420 15.4076 3
21 0 0 156.226 17.3083 2
-22 0 0 43.6949 10.5002 2
22 0 0 26.4350 7.38222 3
22 0 0 24.3897 7.19959 2
23 0 0 4.84242 4.73095 2
23 0 0 3.72139 4.70158 3
24 0 0 25.5081 7.87471 2
-24 0 0 37.2340 12.9073 2
24 0 0 38.7038 9.22000 3
-25 0 0 14.7003 10.7346 2
25 0 0 6.29465 6.34572 3
25 0 0 8.24762 5.93298 2
26 0 0 23.9139 8.68744 3
26 0 0 14.7865 6.94661 2
0 -1 0 -0.0620 0.47461 4
0 1 0 -0.0698 0.46850 4
1 -1 0 114.505 6.71687 2
1 -1 0 124.545 6.96008 4
-1 -1 0 124.035 6.40032 5
1 -1 0 122.708 7.24352 3
1 -1 0 119.795 6.25704 2
-1 -1 0 128.192 6.98122 4
1 1 0 122.648 6.40775 5
-1 1 0 119.844 7.19977 3
-1 1 0 121.981 6.94676 4
-2 -1 0 643.255 31.9165 5
2 -1 0 627.898 32.1230 2
2 -1 0 666.659 32.6047 4
-2 -1 0 662.566 31.8935 2
-2 -1 0 625.499 32.4008 3
2 -1 0 651.327 32.1086 2
2 -1 0 645.160 32.8729 3
-2 1 0 640.287 31.9809 2
2 1 0 626.607 31.9306 5
-2 1 0 637.395 31.9990 2
-2 1 0 650.252 32.9014 3
-2 1 0 670.441 32.6055 4
-3 -1 0 854.950 41.7773 2
-3 -1 0 858.834 41.6647 5
3 -1 0 886.868 42.6604 3
-3 -1 0 821.141 41.9675 3
3 -1 0 802.863 41.7803 2
3 -1 0 824.062 42.0151 2
3 -1 0 864.593 42.3513 4
-3 -1 0 831.167 41.4701 2
-3 1 0 836.960 41.8923 2
-3 1 0 855.245 42.3326 4
3 1 0 820.285 42.0687 3
3 1 0 847.919 41.5186 2
-3 1 0 822.615 41.7714 2
-3 1 0 853.238 42.6551 3
3 1 0 832.051 41.6510 5
3 1 0 838.283 41.4085 2
4 -1 0 1071.17 54.1959 2
4 -1 0 1106.41 55.0027 3
4 -1 0 1103.98 54.8600 4
-4 -1 0 1072.83 54.3399 3
4 -1 0 1100.79 54.6399 2
-4 -1 0 1077.79 53.8522 2
-4 -1 0 1100.57 54.3397 2
4 1 0 1107.96 53.8385 2
-4 1 0 1059.00 54.1789 2
4 1 0 1079.26 54.0738 5
4 1 0 1088.00 54.0630 2
-4 1 0 1110.19 54.8426 4
4 1 0 1097.30 54.4857 3
-4 1 0 1107.04 55.1070 3
-4 1 0 1076.81 54.4099 2
5 -1 0 1196.37 58.7043 4
-5 -1 0 1158.12 58.0549 2
5 -1 0 1105.76 58.1997 2
-5 -1 0 1169.04 58.7879 3
5 -1 0 1184.04 58.6358 3
-5 -1 0 1191.92 57.8581 2
5 -1 0 1147.38 57.8041 2
5 1 0 1174.00 58.1035 3
-5 1 0 1165.80 58.5263 4
-5 1 0 1168.08 58.7500 3
5 1 0 1125.42 57.7137 2
-5 1 0 1114.35 58.0492 2
5 1 0 1126.69 57.7280 5
-5 1 0 1147.91 58.3799 2
5 1 0 1201.21 57.4534 2
6 -1 0 141.297 9.40482 4
6 -1 0 127.001 8.77587 2
6 -1 0 150.742 9.34543 3
-6 -1 0 136.633 8.73800 2
6 -1 0 144.805 8.57046 2
-6 -1 0 129.481 9.42213 4
-6 -1 0 137.933 8.12383 2
-6 -1 0 136.255 8.59740 3
6 1 0 132.385 8.29490 5
-6 1 0 128.343 8.93546 4
6 1 0 139.820 8.76035 3
-6 1 0 130.762 8.71817 2
-6 1 0 130.307 9.21468 3
6 1 0 141.090 8.10962 2
-6 1 0 127.038 8.30079 2
7 -1 0 357.758 20.0077 4
-7 -1 0 340.499 18.9727 2
-7 -1 0 328.922 18.7646 3
7 1 0 352.529 19.0362 3
7 1 0 326.835 18.5254 2
7 1 0 349.683 18.2024 2
7 1 0 299.015 18.2174 5
8 -1 0 134.672 9.23846 2
-8 -1 0 138.496 9.66341 2
8 -1 0 146.574 10.1976 3
8 -1 0 141.882 10.5335 4
-8 1 0 146.682 9.74883 2
8 1 0 131.870 9.27962 2
-9 -1 0 3381.24 169.513 2
9 -1 0 3359.04 169.044 2
9 -1 0 3557.32 170.256 3
9 -1 0 3487.52 171.148 4
9 1 0 3390.65 168.445 2
-9 1 0 3394.20 169.499 2
9 1 0 3391.42 169.458 3
-10 -1 0 3045.26 150.608 2
10 -1 0 3119.74 151.571 3
10 -1 0 3180.76 150.413 2
-10 1 0 2965.46 150.463 2
10 1 0 2882.38 149.306 2
10 1 0 2943.53 150.473 3
-11 -1 0 136.295 10.5564 2
11 -1 0 140.438 11.7592 4
11 -1 0 136.053 10.3211 2
11 -1 0 147.498 11.3497 3
11 1 0 140.841 10.5966 3
11 1 0 144.866 9.83549 2
-11 1 0 144.241 10.6888 2
12 -1 0 156.943 11.4188 2
12 -1 0 166.931 13.6933 4
12 -1 0 167.253 12.7032 3
-12 -1 0 161.611 11.9969 2
12 1 0 148.068 11.6661 3
12 1 0 156.552 10.8843 2
-12 1 0 165.275 12.0026 2
-13 -1 0 13.7902 3.84430 2
13 -1 0 16.2773 4.43658 3
13 -1 0 11.9372 4.44409 4
13 -1 0 18.6506 3.87935 2
13 1 0 6.34388 2.61139 2
13 1 0 12.1926 3.36390 3
-13 1 0 11.5188 3.85087 2
14 -1 0 141.940 13.1118 3
14 -1 0 160.605 15.0160 4
-14 -1 0 159.842 13.0647 2
14 -1 0 168.220 13.7506 2
14 1 0 157.812 11.6008 2
14 1 0 168.161 12.7963 3
15 -1 0 330.493 22.3567 3
-15 -1 0 345.467 21.7122 2
15 -1 0 313.678 20.6409 2
15 -1 0 313.598 23.2154 4
15 1 0 359.843 22.4001 3
15 1 0 309.938 21.3653 2
-15 1 0 317.610 21.6672 2
16 -1 0 387.359 29.0417 4
16 -1 0 427.034 27.1392 3
16 -1 0 405.314 25.6275 2
-16 -1 0 398.091 27.1324 2
-16 1 0 436.318 27.1848 2
16 1 0 423.368 25.4588 2
16 1 0 437.780 26.8364 3
-17 -1 0 466.392 31.9027 2
17 -1 0 493.168 30.5213 2
17 -1 0 508.733 33.5709 4
17 -1 0 447.469 31.1857 3
17 1 0 539.125 31.6582 3
-17 1 0 496.264 32.1725 2
17 1 0 514.884 29.7857 2
18 -1 0 258.070 19.0665 2
18 -1 0 256.054 22.0530 4
18 -1 0 238.546 19.6233 3
-18 -1 0 254.982 20.3364 2
18 1 0 276.833 19.7346 3
18 1 0 250.499 17.9142 2
-18 1 0 224.149 21.6445 2
19 -1 0 111.564 12.7580 3
-19 -1 0 140.702 13.8364 2
19 -1 0 102.220 11.1871 2
19 1 0 111.689 11.0531 2
-19 1 0 110.898 13.7381 2
19 1 0 131.249 12.3900 3
20 -1 0 17.1447 6.20971 3
20 -1 0 20.6917 6.09994 2
20 1 0 28.4711 6.26801 3
-20 1 0 35.0489 8.59917 2
20 1 0 18.5584 5.49752 2
-21 -1 0 18.4738 8.32900 2
21 -1 0 24.5887 7.21209 2
21 1 0 14.6351 5.18420 2
21 1 0 19.5770 6.56094 3
-21 1 0 26.6861 9.72275 2
22 -1 0 63.9700 10.2044 3
-22 -1 0 91.1572 14.5849 2
22 -1 0 60.6098 9.81243 2
22 1 0 71.3764 11.5716 3
-22 1 0 84.7883 15.3375 2
23 -1 0 139.394 16.8046 3
23 -1 0 181.097 16.7590 2
23 1 0 192.877 17.3777 3
23 1 0 185.269 16.3725 2
24 -1 0 23.9479 8.54353 3
-24 -1 0 37.0985 11.4583 2
24 -1 0 30.4056 8.17518 2
24 1 0 25.1153 8.40086 3
-24 1 0 27.9992 11.7140 2
24 1 0 26.7405 7.47884 2
25 -1 0 139.463 16.5206 3
-25 -1 0 189.302 24.9034 2
25 -1 0 139.023 16.0431 2
25 1 0 148.879 15.7116 2
25 1 0 144.676 16.0597 3
26 -1 0 31.3667 10.7922 3
26 1 0 51.9652 10.3690 3
26 1 0 40.7436 9.66662 2
0 -2 0 9999.99 485.909 4
0 -2 0 9996.14 486.463 3
0 2 0 9950.43 485.792 4
1 -2 0 13.1327 2.40042 3
-1 -2 0 10.6919 1.40625 5
1 -2 0 17.9764 2.27521 4
-1 -2 0 13.7232 2.16793 4
1 2 0 12.1835 2.02950 4
-2 -2 0 122.614 6.80941 5
-2 -2 0 123.091 7.88993 4
2 -2 0 126.588 8.46444 3
2 -2 0 119.253 6.79466 2
2 -2 0 124.358 7.87831 4
2 -2 0 116.507 6.74594 2
-2 2 0 119.371 8.30148 3
-2 2 0 125.380 8.43575 4
2 2 0 122.601 6.86172 5
3 -2 0 225.219 12.4052 2
3 -2 0 233.321 13.8635 3
-3 -2 0 222.458 11.7459 2
3 -2 0 230.536 13.2828 4
3 -2 0 224.065 12.3806 2
-3 -2 0 240.347 11.8393 2
-3 -2 0 229.454 12.0842 5
3 2 0 231.143 12.2063 5
-3 2 0 222.743 11.6557 2
-3 2 0 220.182 13.7803 3
-3 2 0 233.765 11.7558 2
-4 -2 0 1.04134 0.72459 2
-4 -2 0 0.71256 0.84251 3
4 -2 0 1.05568 1.03394 2
4 -2 0 1.00631 1.19521 4
-4 -2 0 0.69665 0.71507 5
4 -2 0 -0.4422 0.95220 2
4 -2 0 0.98761 1.31563 3
-4 -2 0 0.87382 0.84968 2
4 2 0 0.00358 0.72533 5
-4 2 0 -0.3325 0.94102 4
-4 2 0 0.69666 0.90207 2
-4 2 0 1.14346 0.85433 2
5 -2 0 6.81884 1.80057 2
5 -2 0 5.75056 1.91443 2
-5 -2 0 8.58254 1.48803 5
-5 -2 0 6.83940 1.68985 2
-5 -2 0 6.58839 1.68812 3
5 -2 0 5.79424 2.12556 4
-5 2 0 6.50997 1.62450 2
5 2 0 7.09121 1.37961 5
-5 2 0 8.24321 1.62723 2
5 2 0 7.12980 1.45779 2
-5 2 0 6.01741 1.97008 4
-6 -2 0 142.820 8.83030 2
6 -2 0 140.635 9.98260 3
-6 -2 0 132.076 8.94994 3
-6 -2 0 134.268 8.13508 2
6 -2 0 155.654 9.87738 4
6 -2 0 137.225 8.81336 2
-6 2 0 139.991 8.76124 2
6 2 0 132.420 8.39942 5
6 2 0 140.414 9.31322 3
-6 2 0 139.142 8.64399 2
6 2 0 140.319 7.90194 2
-7 -2 0 72.5868 5.78152 2
7 -2 0 67.3377 6.46334 3
7 -2 0 72.2009 6.55564 4
7 -2 0 77.0149 6.07901 2
-7 2 0 69.6829 6.25349 2
7 2 0 80.9349 6.68696 3
7 2 0 67.3109 4.93962 2
-7 2 0 66.1628 5.40276 2
7 2 0 75.1614 4.95292 2
7 2 0 72.7614 5.37749 5
8 -2 0 547.099 30.5075 3
-8 -2 0 556.973 33.1890 2
8 -2 0 538.856 30.4327 4
8 -2 0 528.920 29.1962 2
8 2 0 555.982 29.8852 3
8 2 0 568.422 28.4230 2
-8 2 0 523.511 29.2667 2
9 -2 0 311.669 18.8958 3
9 -2 0 303.942 19.0257 4
9 -2 0 316.877 17.8510 2
-9 -2 0 300.557 17.8329 2
9 2 0 309.166 18.2040 3
9 2 0 288.598 16.8513 2
-9 2 0 296.958 17.7036 2
9 2 0 270.903 16.9541 2
10 -2 0 435.501 26.3573 4
-10 -2 0 443.827 25.2411 2
10 -2 0 432.386 24.9037 2
10 -2 0 444.459 26.3372 3
-10 2 0 421.177 24.9516 2
10 2 0 459.203 24.0868 2
10 2 0 456.728 25.5894 3
11 -2 0 39.3349 5.70194 3
11 -2 0 40.3512 6.04676 4
-11 -2 0 40.0000 5.16122 2
11 -2 0 39.1287 4.97670 2
11 2 0 41.0147 4.31481 2
11 2 0 41.4910 5.15656 3
-11 2 0 43.4349 5.15040 2
12 -2 0 12.7389 4.72240 4
12 -2 0 6.58431 3.18751 3
-12 -2 0 13.0079 3.44198 2
12 -2 0 7.17623 3.08840 2
12 2 0 8.16586 3.02257 3
12 2 0 11.0497 2.66500 2
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-1 2 45 9.79234 5.23044 5
0 -2 -45 14.9675 7.07642 4
0 -2 45 9.64984 7.75730 2
0 -2 -45 12.9105 8.65015 2
0 2 45 7.15830 5.11833 5
-1 -2 -45 13.1394 7.46875 2
1 -2 45 12.8636 7.86717 2
-1 -2 -45 25.9065 10.6175 4
1 -2 45 4.78740 6.17588 5
1 2 45 16.9764 6.76899 5
2 -2 45 2.84921 4.79362 2
-2 -2 -45 -2.6330 5.84624 2
2 -2 45 1.76143 5.34224 5
2 2 45 4.19038 5.00989 5
3 -2 45 4.64291 6.04176 2
3 2 45 4.95713 5.08807 2
3 2 45 4.74438 5.43838 5
4 -2 45 22.8142 10.4240 2
-4 -2 -45 7.03589 7.47779 4
-4 -2 -45 4.86343 7.44754 2
4 2 45 20.6922 8.79485 2
4 2 45 10.6702 7.13646 5
5 -2 45 26.7486 11.2590 2
-5 -2 -45 21.7949 10.5808 2
5 -2 45 13.4069 8.45821 5
5 2 45 14.2918 7.20230 5
5 2 45 3.98964 7.40100 2
6 -2 45 2.13602 6.88148 5
6 2 45 -3.7788 4.37425 5
-5 -3 45 6.84666 6.35925 5
5 -3 -45 5.26754 7.19147 4
5 -3 -45 5.62807 5.76824 3
-5 3 45 -0.9105 3.75302 5
-4 -3 45 2.03847 5.05470 2
4 -3 -45 0.58081 5.35423 3
4 -3 -45 -2.0160 5.42703 4
-4 -3 45 8.40689 5.76014 5
-4 3 45 1.22202 5.13442 2
-4 3 45 -4.4202 3.48817 5
-3 -3 45 0.42867 5.27988 2
3 -3 -45 -2.4613 5.28287 3
3 -3 -45 -0.2747 4.86962 4
-3 -3 45 -1.1483 4.88934 5
-3 3 45 2.23948 3.86860 5
-3 3 45 -2.9885 5.09291 2
2 -3 -45 13.9205 7.60185 4
2 -3 -45 19.5017 8.35852 3
-2 -3 45 17.9259 8.41593 2
-2 -3 45 15.1290 6.39129 5
-2 3 45 19.5597 5.91022 5
-2 3 45 17.6118 7.67297 2
-1 -3 45 3.80412 6.52082 5
-1 -3 45 6.28513 6.13651 2
1 -3 -45 6.81293 6.85621 4
-1 3 45 5.96483 5.59412 2
-1 3 45 9.50987 4.64384 5
0 -3 45 -5.1585 5.12650 5
0 -3 45 -0.4090 6.13144 2
0 -3 -45 4.18837 6.47074 4
0 3 45 -0.0393 3.82338 5
0 3 45 0.40217 4.87224 2
1 -3 45 1.95204 6.23663 2
1 -3 45 -2.5031 5.92483 5
-1 -3 -45 7.63801 7.37144 4
1 3 45 5.77012 4.74426 5
1 3 45 3.39675 5.18533 2
2 -3 45 6.32068 6.06939 5
-2 -3 -45 -0.2693 6.53530 2
-2 -3 -45 1.84785 6.53014 4
2 3 45 -0.2985 4.05936 5
-8 0 46 42.1738 10.7132 2
8 0 -46 18.4133 10.5278 4
7 0 -46 3.46873 7.04146 4
-7 0 46 4.85490 4.83941 5
-6 0 46 34.5024 8.26421 5
-6 0 46 37.9458 13.7177 2
6 0 -46 21.2681 9.30995 4
5 0 -46 -0.4957 6.31525 4
-5 0 46 -2.0923 4.95138 2
-5 0 46 -0.3708 3.85915 5
-4 0 46 -5.7163 3.78244 2
-4 0 46 6.32736 5.12413 5
4 0 -46 -1.1705 6.35020 4
-3 0 46 24.1282 8.57170 5
3 0 -46 18.1789 8.58843 4
-3 0 46 21.4115 8.17482 2
-2 0 46 7.11386 5.69572 5
-2 0 46 5.76224 6.43384 2
-1 0 46 35.7563 9.42905 2
-1 0 46 41.6039 9.62575 5
0 0 46 14.5941 6.93668 5
0 0 46 16.4005 7.49581 2
1 0 46 2.30994 5.70623 5
1 0 46 4.34171 4.95402 2
2 0 46 2.50954 5.60590 2
2 0 46 7.75645 6.57998 5
-2 0 -46 2.11420 5.21621 2
3 0 46 5.73190 6.32301 5
4 0 46 -3.3286 6.65103 5
-4 0 -46 9.23523 6.84522 2
5 0 46 15.0623 8.98381 5
5 0 46 24.9934 10.3202 2
6 0 46 -0.3923 6.59563 5
8 -1 -46 -3.9851 6.30936 4
8 -1 -46 -0.8815 5.43388 2
-8 -1 46 -0.7549 3.70571 5
-8 1 46 2.50671 4.18770 5
7 -1 -46 1.18484 5.34592 2
-7 -1 46 -2.2418 4.90154 5
-7 -1 46 0.12379 5.03591 2
7 -1 -46 6.23673 7.28006 4
-7 1 46 -0.0152 5.46766 2
-7 1 46 3.82588 4.10347 5
6 -1 -46 20.0200 8.06234 4
6 -1 -46 23.7135 8.43872 2
-6 -1 46 14.7763 7.00186 2
-6 1 46 7.29091 5.75753 5
-6 1 46 27.4763 8.92743 2
5 -1 -46 19.8656 9.05246 4
-5 -1 46 27.7013 9.70456 2
-5 -1 46 18.3231 7.48176 5
5 -1 -46 15.0495 7.85537 2
-5 1 46 19.4480 6.30038 5
-5 1 46 16.0306 10.0596 2
-4 -1 46 12.2784 6.31209 5
-4 -1 46 1.07886 5.20729 2
4 -1 -46 14.7328 8.44084 4
4 -1 -46 6.01375 5.91360 2
-4 1 46 14.4215 6.35323 5
-3 -1 46 9.44598 5.94588 5
3 -1 -46 3.71534 6.19968 2
-3 -1 46 18.9527 7.90528 2
-3 1 46 8.42631 5.16562 5
-2 -1 46 9.77438 6.81401 2
2 -1 -46 8.66748 6.67183 2
2 -1 -46 -2.6206 6.06161 3
2 -1 -46 2.60508 6.58700 4
-2 -1 46 8.35686 6.15232 5
-2 1 46 -3.9829 3.99568 5
1 -1 -46 -6.3338 4.60510 2
-1 -1 46 2.33153 5.18253 5
-1 -1 46 1.26519 4.77581 2
1 -1 -46 -1.0806 6.51114 4
-1 1 46 4.61488 4.89085 5
0 -1 -46 7.64732 6.10061 2
0 -1 46 19.0490 7.09829 2
0 -1 -46 2.20276 5.95941 4
0 -1 46 24.0620 8.10276 5
0 1 46 13.7769 6.58071 5
-1 -1 -46 2.91641 5.20210 4
-1 -1 -46 8.57003 6.87539 2
1 -1 46 9.84075 6.41209 2
1 -1 46 9.80443 6.80880 5
1 1 46 15.2171 6.68660 5
-2 -1 -46 1.72035 5.43863 2
2 -1 46 0.33673 4.71390 5
2 1 46 2.60448 6.59279 2
2 1 46 2.89290 5.00263 5
3 -1 46 2.78692 5.34975 5
3 -1 46 -7.2641 5.13126 2
-3 -1 -46 0.96476 6.28076 2
3 1 46 -3.5060 4.61790 2
3 1 46 -1.2667 4.73371 5
-4 -1 -46 2.08910 6.86031 2
4 -1 46 6.66876 7.12959 5
4 1 46 4.35628 6.36509 2
4 1 46 -4.3167 4.62936 5
5 -1 46 1.52696 7.82776 5
5 1 46 3.58886 6.18194 2
5 1 46 -4.0936 5.21644 5
6 -2 -46 5.06814 5.75620 2
-6 -2 46 0.86331 5.22753 5
6 -2 -46 -1.0703 5.57470 4
-6 2 46 -0.0177 3.57492 5
5 -2 -46 -0.6754 5.51379 3
5 -2 -46 -0.8704 5.69728 4
5 -2 -46 9.18530 6.19977 2
-5 -2 46 3.58948 5.96533 2
-5 -2 46 0.29149 5.31242 5
-5 2 46 2.30275 4.31760 5
4 -2 -46 -1.8193 5.59061 4
4 -2 -46 -2.4611 5.00169 2
-4 -2 46 -0.7326 4.90139 2
4 -2 -46 -0.9356 5.19457 3
-4 -2 46 3.33475 4.78426 5
-4 2 46 1.23804 4.12941 5
-4 2 46 -4.6301 4.74950 2
-3 -2 46 23.1001 8.66444 2
3 -2 -46 14.8096 8.65641 2
-3 -2 46 5.78313 5.67267 5
3 -2 -46 16.0809 8.58696 4
3 -2 -46 12.4848 6.35741 3
-3 2 46 15.8522 6.95732 2
-3 2 46 12.3539 5.49032 5
2 -2 -46 4.31879 5.85029 2
-2 -2 46 10.5131 9.71713 5
-2 -2 46 14.0914 7.47609 2
2 -2 -46 14.0501 7.01476 4
-2 2 46 12.4108 6.19501 5
-2 2 46 17.7155 7.99015 2
1 -2 -46 3.21382 5.48038 2
1 -2 -46 -0.6933 5.69241 4
-1 -2 46 4.27514 5.91804 2
-1 2 46 1.81691 3.86615 5
-1 2 46 6.00750 5.67189 2
0 -2 -46 -0.1201 6.19318 2
0 -2 -46 -2.4225 4.46034 4
0 -2 46 1.91964 6.85832 2
0 2 46 5.23766 4.45119 5
0 2 46 -1.3634 4.91938 2
1 -2 46 9.29299 8.00150 2
-1 -2 -46 2.89516 5.09317 2
1 -2 46 4.72031 6.59039 5
-1 -2 -46 -0.0240 5.78608 4
1 2 46 0.34438 5.19389 2
1 2 46 5.13552 4.44030 5
-2 -2 -46 5.23922 6.53507 2
2 -2 46 7.58069 6.72392 5
2 -2 46 18.5937 8.82259 2
-2 -2 -46 -1.8548 6.04638 4
2 2 46 2.92614 5.67738 2
2 2 46 3.31902 5.11867 5
3 -2 46 5.99636 10.1909 5
3 -2 46 20.7485 10.5737 2
3 2 46 18.4011 6.83529 5
3 2 46 8.85402 7.64567 2
-6 0 47 -1.7352 4.72099 2
-5 0 47 1.15401 4.44310 5
-5 0 47 0.19836 4.64480 2
-4 0 47 -5.4844 3.69519 5
-3 0 47 0.93822 4.46652 5
-2 0 47 -3.7538 4.30211 5
-1 0 47 6.71279 5.61531 5
0 0 47 7.80033 5.86031 5
1 0 47 3.36386 5.85851 2
1 0 47 -2.0718 4.11161 5
-1 0 -47 0.95291 4.82499 2
-2 0 -47 4.41915 5.28479 2
2 0 47 0.68652 4.53079 5
3 0 47 -2.9062 5.79644 2
-3 0 -47 1.71637 5.14929 2
3 0 47 3.26712 5.46141 5
-6 -1 47 6.52178 5.50172 5
-6 1 47 0.59339 4.25521 5
-5 -1 47 3.64568 4.99230 5
5 -1 -47 0.04084 5.86677 4
5 -1 -47 1.43552 5.42388 2
-5 1 47 1.30368 5.11097 2
-5 1 47 0.38920 3.70597 5
4 -1 -47 -3.3831 6.02880 4
4 -1 -47 1.73658 5.60915 2
-4 1 47 -1.9917 4.91069 2
-4 1 47 0.83388 3.91200 5
3 -1 -47 9.11220 7.21837 2
-3 -1 47 -0.5467 6.19613 2
3 -1 -47 12.9504 7.89004 4
-3 1 47 10.5808 7.14622 2
-3 1 47 9.33181 5.51502 5
2 -1 -47 10.4414 7.90816 4
2 -1 -47 20.3544 8.66223 2
-2 -1 47 0.19077 5.16145 2
-2 1 47 6.02586 5.29102 5
-2 1 47 15.8082 7.37181 2
-1 -1 47 9.08945 7.68974 2
1 -1 -47 11.7714 6.67010 2
-1 1 47 2.24595 4.39231 5
-1 1 47 19.5254 7.36241 2
0 -1 -47 17.4800 8.08254 2
0 1 47 1.90758 5.01465 2
0 1 47 3.68781 5.44409 5
-1 -1 -47 7.88965 7.50380 2
1 1 47 3.98061 4.87773 2
1 1 47 -1.9461 4.43809 5
-2 -1 -47 4.40673 6.84934 2
2 1 47 5.75030 6.28729 5
2 1 47 18.1629 8.17729 2
3 1 47 2.15297 5.45078 5
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 25557
_shelx_res_file
;
TITL m22268 : space group P21/c
m22268.res
created by SHELXL-2019/2 at 16:59:11 on 27-Feb-2023
CELL 0.71073 20.4117 7.4255 36.796 90.000 92.970 90.000
ZERR 12 0.0018 0.0006 0.003 0.000 0.003 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H I N O
UNIT 216 276 12 24 48
TEMP -183
SIZE 0.30 0.13 0.03
REM FORM plate
REM COLR colourless
L.S. 10
BOND $H
CONF
REM Instructions for potential hydrogen bonds
EQIV $1 x, -y+1/2, z+1/2
HTAB O1W O3C_$1
HTAB O1W O2A
HTAB O2W O3A
HTAB O2W O2B
HTAB O3W O3B
HTAB O3W O2C
EQIV $2 -x+1, -y+1, -z+1
HTAB N1A O3W_$2
HTAB N1A O2A
HTAB C1A O2W
HTAB C2A O3B_$2
EQIV $3 -x+1, -y, -z+1
HTAB C4A O2C_$3
HTAB C7A I1B_$3
EQIV $4 -x+2, -y+1, -z+1
HTAB C11A O1B_$4
HTAB N1B O2B
HTAB N1B O2W_$2
HTAB C1B O3W
HTAB C2B O3A_$2
HTAB C4B O2B_$3
HTAB C4B O2W
HTAB C9B I1B_$2
HTAB N1C O2C
HTAB N1C O3C
HTAB N1C O1W_$2
EQIV $5 x, -y+1/2, z-1/2
HTAB C1C O1W_$5
HTAB C4C O2A_$3
HTAB C9C I1A_$2
HTAB
REM Relative twist of benzene and piperazinium rings:
MPLA C1A C2A C3A C4A
MPLA C5A C6A C7A C8A C9A C10A
MPLA C1B C2B C3B C4B
MPLA C5B C6B C7B C8B C9B C10B
MPLA C1C C2C C3C C4C
MPLA C5C C6C C7C C8C C9C C10C
REM Out of planarity of methoxy group:
RTAB tors C9A C8A O1A C11A
MPLA 7 C5A C6A C7A C8A C9A C10A O1A C11A
RTAB tors C9B C8B O1B C11B
MPLA 7 C5B C6B C7B C8B C9B C10B O1B C11B
RTAB tors C9C C8C O1C C11C
MPLA 7 C5C C6C C7C C8C C9C C10C O1C C11C
REM Out of planarity of N2:
RTAB angl C2A N2A C3A
RTAB angl C3A N2A C5A
RTAB angl C5A N2A C2A
RTAB angl C2B N2B C3B
RTAB angl C3B N2B C5B
RTAB angl C5B N2B C2B
RTAB angl C2C N2C C3C
RTAB angl C3C N2C C5C
RTAB angl C5C N2C C2C
REM Planarity of anion:
MPLA C12A O2A O3A
MPLA C13A C14A C15A C16A C17A C18A
MPLA C12B O2B O3B
MPLA C13B C14B C15B C16B C17B C18B
MPLA C12C O2C O3C
MPLA C13C C14C C15C C16C C17C C18C
REM Iodine...iodine close contacts:
EQIV $6 -x, -y, 1-z
RTAB dist I1A I1C_$6
RTAB dist I1B I1B_$6
RTAB dist I1C I1A_$6
LIST 4
ACTA
FMAP 2
PLAN 20
REM waters
DFIX 21.000 0.010 O1W H1W1 O1W H2W1 O2W H1W2 O2W H2W2 O3W H1W3 O3W H2W3
DFIX 21.581 0.020 H1W1 H2W1 H1W2 H2W2 H1W3 H2W3
SIMU 0.020 H1W1 H2W1
SIMU 0.020 H1W2 H2W2
SIMU 0.020 H1W3 H2W3
WGHT 0.021600 1.762800
EXTI 0.000169
FVAR 0.12555 0.77198
O1W 5 0.439688 0.220461 0.707116 11.00000 0.02650 0.02294 =
0.01671 -0.00037 -0.00088 -0.00404
H1W1 2 0.423605 0.181485 0.723843 11.00000 0.04298
H2W1 2 0.426018 0.166208 0.690646 11.00000 0.04328
O2W 5 0.465211 0.341878 0.542254 11.00000 0.02140 0.02347 =
0.01651 0.00102 0.00524 -0.00309
H1W2 2 0.445955 0.310058 0.558524 11.00000 0.02429
H2W2 2 0.446899 0.300175 0.525347 11.00000 0.04617
O3W 5 0.471528 0.463731 0.385242 11.00000 0.02026 0.02057 =
0.01623 -0.00032 0.00459 -0.00030
H1W3 2 0.449288 0.438858 0.400787 11.00000 0.03928
H2W3 2 0.455188 0.417043 0.368251 11.00000 0.03134
REM cation-anion pair A
N1A 4 0.537278 0.170081 0.625815 11.00000 0.01586 0.01710 =
0.01814 0.00049 0.00391 -0.00107
H1AA 2 0.497901 0.122562 0.630318 11.00000 0.03885
H1AB 2 0.530496 0.293096 0.621228 11.00000 0.03586
N2A 4 0.677219 0.157817 0.619696 11.00000 0.01314 0.01809 =
0.01492 -0.00076 0.00229 -0.00040
C1A 1 0.566523 0.080160 0.594235 11.00000 0.01510 0.01538 =
0.01947 -0.00218 0.00230 0.00041
AFIX 23
H1AC 2 0.536526 0.091693 0.572342 11.00000 -1.20000
H1AD 2 0.573059 -0.049571 0.599461 11.00000 -1.20000
AFIX 0
C2A 1 0.631714 0.167778 0.587407 11.00000 0.01429 0.01745 =
0.01478 -0.00028 0.00210 -0.00010
AFIX 23
H2AA 2 0.651615 0.106930 0.566729 11.00000 -1.20000
H2AB 2 0.624385 0.295573 0.580691 11.00000 -1.20000
AFIX 0
C3A 1 0.648550 0.235067 0.651861 11.00000 0.01761 0.02257 =
0.01177 -0.00084 0.00266 0.00105
AFIX 23
H3A1 2 0.643210 0.366608 0.648468 11.00000 -1.20000
H3A2 2 0.678752 0.215151 0.673412 11.00000 -1.20000
AFIX 0
C4A 1 0.582402 0.151569 0.658592 11.00000 0.01715 0.02340 =
0.01690 0.00355 0.00454 0.00072
AFIX 23
H4AA 2 0.588228 0.022477 0.664660 11.00000 -1.20000
H4AB 2 0.563121 0.211922 0.679520 11.00000 -1.20000
AFIX 0
C5A 1 0.741573 0.219318 0.613438 11.00000 0.01442 0.01560 =
0.01512 0.00202 0.00202 0.00214
C6A 1 0.774153 0.153289 0.583738 11.00000 0.01693 0.01763 =
0.01783 -0.00414 0.00054 -0.00175
AFIX 43
H6A 2 0.752173 0.070253 0.567695 11.00000 -1.20000
AFIX 0
C7A 1 0.837270 0.205084 0.577023 11.00000 0.01900 0.01863 =
0.01845 -0.00440 0.00373 -0.00031
AFIX 43
H7A 2 0.857901 0.158525 0.556458 11.00000 -1.20000
AFIX 0
C8A 1 0.870771 0.324961 0.600190 11.00000 0.01346 0.01543 =
0.02274 0.00194 0.00228 0.00112
C9A 1 0.839018 0.391582 0.629850 11.00000 0.01881 0.01865 =
0.01842 -0.00457 -0.00217 -0.00135
AFIX 43
H9A 2 0.861272 0.473954 0.645926 11.00000 -1.20000
AFIX 0
C10A 1 0.775866 0.340382 0.636371 11.00000 0.01924 0.02091 =
0.01444 -0.00480 0.00231 0.00225
AFIX 43
H10A 2 0.755274 0.388262 0.656829 11.00000 -1.20000
AFIX 0
O1A 5 0.933244 0.386454 0.596119 11.00000 0.01576 0.02883 =
0.02980 -0.00994 0.00711 -0.00644
C11A 1 0.967906 0.308468 0.567151 11.00000 0.02019 0.03538 =
0.02848 -0.00566 0.01059 -0.00357
AFIX 137
H11A 2 1.012352 0.358505 0.567375 11.00000 -1.50000
H11B 2 0.944723 0.335895 0.543819 11.00000 -1.50000
H11C 2 0.970366 0.177628 0.570434 11.00000 -1.50000
AFIX 0
I1A 3 0.070540 0.224139 0.659854 11.00000 0.01674 0.02892 =
0.05171 -0.01156 0.00330 0.00099
O2A 5 0.410188 0.074138 0.641099 11.00000 0.01752 0.02032 =
0.01718 -0.00222 0.00374 -0.00230
O3A 5 0.387287 0.256273 0.594159 11.00000 0.03427 0.03809 =
0.02724 0.01149 0.01534 -0.00185
C12A 1 0.371154 0.170771 0.621355 11.00000 0.02188 0.01566 =
0.01611 -0.00502 0.00492 -0.00481
C13A 1 0.300618 0.183851 0.631104 11.00000 0.01869 0.01173 =
0.01635 -0.00332 0.00359 -0.00492
C14A 1 0.255984 0.279782 0.608712 11.00000 0.03089 0.01329 =
0.01651 0.00175 0.00163 -0.00426
AFIX 43
H14A 2 0.270779 0.337633 0.587618 11.00000 -1.20000
AFIX 0
C15A 1 0.190675 0.292707 0.616486 11.00000 0.02397 0.01693 =
0.02886 -0.00093 -0.00632 0.00125
AFIX 43
H15A 2 0.160641 0.357675 0.600863 11.00000 -1.20000
AFIX 0
C16A 1 0.169656 0.208595 0.647699 11.00000 0.01440 0.01573 =
0.02662 -0.00775 0.00084 -0.00334
C17A 1 0.213082 0.113053 0.670424 11.00000 0.01943 0.01628 =
0.02021 0.00006 0.00543 -0.00206
AFIX 43
H17A 2 0.198222 0.056099 0.691601 11.00000 -1.20000
AFIX 0
C18A 1 0.278422 0.100790 0.662150 11.00000 0.01826 0.01177 =
0.01504 -0.00032 0.00145 -0.00169
AFIX 43
H18A 2 0.308316 0.035272 0.677757 11.00000 -1.20000
AFIX 0
REM cation-anion pair B
N1B 4 0.545284 0.287196 0.462790 11.00000 0.01492 0.01503 =
0.01728 -0.00060 0.00260 -0.00086
H1BA 2 0.504695 0.246842 0.467782 11.00000 0.03178
H1BB 2 0.541311 0.409959 0.459934 11.00000 0.01901
N2B 4 0.683408 0.238967 0.453571 11.00000 0.01529 0.01599 =
0.01220 -0.00214 0.00121 -0.00092
C1B 1 0.570088 0.194821 0.430216 11.00000 0.01461 0.01685 =
0.01557 -0.00113 0.00176 -0.00027
AFIX 23
H1BC 2 0.539379 0.215359 0.408906 11.00000 -1.20000
H1BD 2 0.572919 0.063524 0.434700 11.00000 -1.20000
AFIX 0
C2B 1 0.636909 0.267454 0.422524 11.00000 0.01597 0.01814 =
0.01117 -0.00177 0.00165 0.00067
AFIX 23
H2BA 2 0.653183 0.206538 0.400822 11.00000 -1.20000
H2BB 2 0.633515 0.397882 0.417175 11.00000 -1.20000
AFIX 0
C3B 1 0.659996 0.326541 0.486210 11.00000 0.01717 0.01999 =
0.01128 -0.00203 0.00154 -0.00131
AFIX 23
H3B1 2 0.658596 0.458500 0.482408 11.00000 -1.20000
H3B2 2 0.691065 0.301479 0.507155 11.00000 -1.20000
AFIX 0
C4B 1 0.592362 0.260251 0.494767 11.00000 0.01857 0.01971 =
0.01375 0.00035 0.00180 -0.00055
AFIX 23
H4BA 2 0.594522 0.130750 0.501113 11.00000 -1.20000
H4BB 2 0.576808 0.326780 0.515985 11.00000 -1.20000
AFIX 0
C5B 1 0.750175 0.269910 0.446376 11.00000 0.01642 0.00984 =
0.01365 0.00146 -0.00134 0.00063
C6B 1 0.776270 0.196880 0.415115 11.00000 0.01868 0.01449 =
0.01635 -0.00293 -0.00049 -0.00232
AFIX 43
H6B 2 0.747807 0.135704 0.398002 11.00000 -1.20000
AFIX 0
C7B 1 0.841917 0.210923 0.408384 11.00000 0.02006 0.01578 =
0.01862 -0.00440 0.00260 -0.00145
AFIX 43
H7B 2 0.857875 0.160425 0.386830 11.00000 -1.20000
AFIX 0
C8B 1 0.884687 0.298488 0.432970 11.00000 0.01411 0.01691 =
0.02470 -0.00004 0.00199 0.00060
C9B 1 0.859538 0.374392 0.464038 11.00000 0.02056 0.02216 =
0.01929 -0.00653 -0.00321 -0.00401
AFIX 43
H9B 2 0.888096 0.435936 0.481045 11.00000 -1.20000
AFIX 0
C10B 1 0.793552 0.360981 0.470321 11.00000 0.02181 0.01822 =
0.01465 -0.00315 0.00188 0.00236
AFIX 43
H10B 2 0.777431 0.415177 0.491472 11.00000 -1.20000
AFIX 0
O1B 5 0.950517 0.319519 0.429362 11.00000 0.01366 0.03542 =
0.03512 -0.01241 0.00425 -0.00358
C11B 1 0.978114 0.242132 0.398055 11.00000 0.02091 0.03575 =
0.03520 -0.00988 0.01049 -0.00383
AFIX 137
H11D 2 1.025183 0.268615 0.398486 11.00000 -1.50000
H11E 2 0.956558 0.293296 0.375985 11.00000 -1.50000
H11F 2 0.971528 0.111410 0.398221 11.00000 -1.50000
AFIX 0
I1B 3 0.074779 0.154532 0.494366 11.00000 0.01675 0.02811 =
0.04205 -0.00998 0.00875 -0.00272
O2B 5 0.418367 0.189379 0.478495 11.00000 0.01719 0.02253 =
0.02008 -0.00324 0.00460 -0.00129
O3B 5 0.385734 0.374291 0.433237 11.00000 0.02881 0.03018 =
0.03183 0.01181 0.01377 -0.00169
C12B 1 0.374718 0.273936 0.459379 11.00000 0.02274 0.01428 =
0.01680 -0.00689 0.00608 -0.00433
C13B 1 0.304025 0.249895 0.468340 11.00000 0.01955 0.00993 =
0.01423 -0.00347 0.00420 -0.00226
C14B 1 0.253890 0.321557 0.445798 11.00000 0.02437 0.01552 =
0.01387 -0.00010 0.00026 -0.00506
AFIX 43
H14B 2 0.264596 0.389536 0.425054 11.00000 -1.20000
AFIX 0
C15B 1 0.188604 0.295826 0.452979 11.00000 0.02117 0.01747 =
0.02125 -0.00156 -0.00355 -0.00010
AFIX 43
H15B 2 0.154697 0.343937 0.437190 11.00000 -1.20000
AFIX 0
C16B 1 0.173628 0.198501 0.483654 11.00000 0.01508 0.01588 =
0.02536 -0.00537 0.00626 -0.00057
C17B 1 0.222459 0.128920 0.506924 11.00000 0.02255 0.01385 =
0.01995 0.00172 0.00781 -0.00044
AFIX 43
H17B 2 0.211464 0.064335 0.528047 11.00000 -1.20000
AFIX 0
C18B 1 0.287552 0.153797 0.499304 11.00000 0.01929 0.01530 =
0.01432 0.00103 0.00201 0.00168
AFIX 43
H18B 2 0.321254 0.105354 0.515187 11.00000 -1.20000
AFIX 0
REM cation-anion pair C
N1C 4 0.547316 0.409604 0.301881 11.00000 0.01619 0.01447 =
0.01467 0.00024 0.00007 -0.00142
H1CA 2 0.503948 0.382375 0.309247 11.00000 0.03633
H1CB 2 0.548686 0.518891 0.297576 11.00000 0.01175
N2C 4 0.677886 0.290307 0.289524 11.00000 0.01433 0.01657 =
0.01108 -0.00147 0.00103 0.00056
C1C 1 0.562033 0.302270 0.269137 11.00000 0.01716 0.02089 =
0.01689 -0.00398 0.00052 0.00009
AFIX 23
H1CC 2 0.531549 0.337052 0.248527 11.00000 -1.20000
H1CD 2 0.555525 0.172679 0.274144 11.00000 -1.20000
AFIX 0
C2C 1 0.631866 0.334093 0.259077 11.00000 0.01582 0.02122 =
0.01318 -0.00021 -0.00045 0.00097
AFIX 23
H2CA 2 0.641494 0.258599 0.237828 11.00000 -1.20000
H2CB 2 0.637343 0.461852 0.252166 11.00000 -1.20000
AFIX 0
C3C 1 0.664874 0.399214 0.321465 11.00000 0.01773 0.01976 =
0.01157 -0.00124 0.00033 0.00001
AFIX 23
H3C1 2 0.671354 0.528155 0.315826 11.00000 -1.20000
H3C2 2 0.696146 0.366146 0.341838 11.00000 -1.20000
AFIX 0
C4C 1 0.595498 0.369705 0.332639 11.00000 0.01951 0.01810 =
0.01159 0.00085 0.00019 0.00156
AFIX 23
H4CA 2 0.590283 0.243214 0.340487 11.00000 -1.20000
H4CB 2 0.586798 0.448762 0.353511 11.00000 -1.20000
AFIX 0
C5C 1 0.744725 0.275822 0.280622 11.00000 0.01490 0.01266 =
0.01461 0.00266 0.00007 -0.00187
C6C 1 0.760690 0.170614 0.250952 11.00000 0.01632 0.02005 =
0.01660 -0.00239 -0.00148 -0.00254
AFIX 43
H6C 2 0.726496 0.118494 0.235930 11.00000 -1.20000
AFIX 0
C7C 1 0.825497 0.140401 0.242895 11.00000 0.01729 0.02076 =
0.01817 -0.00272 0.00381 0.00010
AFIX 43
H7C 2 0.835037 0.070293 0.222230 11.00000 -1.20000
AFIX 0
C8C 1 0.876559 0.212083 0.264875 11.00000 0.01812 0.01646 =
0.02453 0.00567 0.00452 -0.00090
C9C 1 0.860897 0.318438 0.294221 11.00000 0.01899 0.01969 =
0.02223 -0.00141 -0.00307 -0.00474
AFIX 43
H9C 2 0.895187 0.369408 0.309346 11.00000 -1.20000
AFIX 0
C10C 1 0.796329 0.351707 0.301888 11.00000 0.02135 0.01345 =
0.01830 -0.00126 0.00056 -0.00121
AFIX 43
H10C 2 0.786977 0.427006 0.321839 11.00000 -1.20000
AFIX 0
O1C 5 0.941802 0.186146 0.260048 11.00000 0.01426 0.02821 =
0.03304 -0.00367 0.00541 -0.00036
C11C 1 0.958386 0.059850 0.233037 11.00000 0.02213 0.03757 =
0.03522 -0.00428 0.00833 0.00485
AFIX 137
H11G 2 1.006183 0.046967 0.233207 11.00000 -1.50000
H11H 2 0.941860 0.102414 0.209073 11.00000 -1.50000
H11I 2 0.938558 -0.056985 0.238193 11.00000 -1.50000
AFIX 0
I1C 3 0.090418 0.067807 0.319099 11.00000 0.01743 0.02945 =
0.04390 -0.00136 0.00347 -0.00327
O2C 5 0.427068 0.301589 0.322896 11.00000 0.01646 0.02485 =
0.01935 0.00135 0.00174 -0.00225
O3C 5 0.393996 0.414130 0.268962 11.00000 0.02655 0.02385 =
0.02080 0.00703 0.00750 0.00091
C12C 1 0.383272 0.331526 0.297579 11.00000 0.02038 0.01189 =
0.01843 -0.00430 0.00607 0.00159
C13C 1 0.315253 0.262709 0.302859 11.00000 0.02027 0.00900 =
0.01749 -0.00118 0.00261 0.00257
C14C 1 0.272019 0.232512 0.273010 11.00000 0.02006 0.02060 =
0.01722 -0.00185 0.00297 0.00415
AFIX 43
H14C 2 0.286224 0.254050 0.249216 11.00000 -1.20000
AFIX 0
C15C 1 0.208842 0.171854 0.277215 11.00000 0.02165 0.02005 =
0.02152 -0.00600 -0.00301 0.00328
AFIX 43
H15C 2 0.180102 0.148483 0.256620 11.00000 -1.20000
AFIX 0
C16C 1 0.188361 0.145886 0.312181 11.00000 0.01344 0.01492 =
0.03112 -0.00100 0.00310 0.00273
C17C 1 0.230038 0.173664 0.342274 11.00000 0.02237 0.01792 =
0.02133 0.00331 0.00500 0.00263
AFIX 43
H17C 2 0.215262 0.154375 0.366023 11.00000 -1.20000
AFIX 0
C18C 1 0.293592 0.229894 0.337594 11.00000 0.01876 0.01603 =
0.01679 0.00126 0.00012 0.00089
AFIX 43
H18C 2 0.322853 0.246385 0.358253 11.00000 -1.20000
AFIX 0
HKLF 4
REM m22268 : space group P21/c
REM wR2 = 0.0687, GooF = S = 1.029, Restrained GooF = 1.029 for all data
REM R1 = 0.0328 for 10003 Fo > 4sig(Fo) and 0.0507 for all 12876 data
REM 729 parameters refined using 12 restraints
END
WGHT 0.0216 1.7564
REM Instructions for potential hydrogen bonds
HTAB O1W O3C_$1
HTAB O1W O2A
HTAB O2W O3A
HTAB O2W O2B
HTAB O3W O3B
HTAB O3W O2C
HTAB N1A O2A
HTAB N1A O3W_$2
HTAB C1A O2W
HTAB C2A O3B_$2
HTAB C4A O2C_$3
HTAB C7A I1B_$3
HTAB C11A O1B_$4
HTAB N1B O2B
HTAB N1B O2W_$2
HTAB C1B O3W
HTAB C2B O3A_$2
HTAB C4B O2B_$3
HTAB C4B O2W
HTAB C9B I1B_$2
HTAB N1C O2C
HTAB N1C O3C
HTAB N1C O1W_$2
HTAB C1C O1W_$5
HTAB C4C O2A_$3
HTAB C9C I1A_$2
REM Highest difference peak 0.839, deepest hole -0.805, 1-sigma level 0.096
Q1 1 0.0795 0.2844 0.6416 11.00000 0.05 0.84
Q2 1 0.0790 0.2354 0.4809 11.00000 0.05 0.74
Q3 1 0.0932 0.1614 0.3095 11.00000 0.05 0.66
Q4 1 0.0887 -0.0671 0.3203 11.00000 0.05 0.58
Q5 1 0.6715 0.2812 0.4692 11.00000 0.05 0.54
Q6 1 0.0645 0.0623 0.3176 11.00000 0.05 0.53
Q7 1 0.0683 0.3579 0.6646 11.00000 0.05 0.53
Q8 1 0.0718 0.2781 0.5002 11.00000 0.05 0.51
Q9 1 0.0536 0.1947 0.3049 11.00000 0.05 0.50
Q10 1 0.0477 0.2170 0.6585 11.00000 0.05 0.50
Q11 1 0.0721 0.1408 0.6575 11.00000 0.05 0.48
Q12 1 0.0318 0.1063 0.6451 11.00000 0.05 0.47
Q13 1 0.0488 0.1554 0.4927 11.00000 0.05 0.45
Q14 1 0.7647 0.2722 0.6233 11.00000 0.05 0.45
Q15 1 0.0460 -0.0694 0.3084 11.00000 0.05 0.43
Q16 1 0.2936 0.2328 0.4856 11.00000 0.05 0.43
Q17 1 0.7140 0.1618 0.6193 11.00000 0.05 0.42
Q18 1 0.7575 0.1509 0.6089 11.00000 0.05 0.41
Q19 1 0.2888 0.1419 0.6469 11.00000 0.05 0.40
Q20 1 0.8778 0.3344 0.4467 11.00000 0.05 0.40
;
_shelx_res_checksum 95612
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
O O1W 0.43969(10) 0.2205(3) 0.70712(5) 0.0221(4) Uani d 1 . .
H H1W1 0.4236(15) 0.181(4) 0.7238(6) 0.043(10) Uiso d 1 . .
H H2W1 0.4260(15) 0.166(4) 0.6906(6) 0.043(10) Uiso d 1 . .
O O2W 0.46521(10) 0.3419(3) 0.54225(5) 0.0203(4) Uani d 1 . .
H H1W2 0.4460(12) 0.310(4) 0.5585(5) 0.024(8) Uiso d 1 . .
H H2W2 0.4469(14) 0.300(4) 0.5253(5) 0.046(10) Uiso d 1 . .
O O3W 0.47153(9) 0.4637(3) 0.38524(5) 0.0189(4) Uani d 1 . .
H H1W3 0.4493(13) 0.439(4) 0.4008(6) 0.039(9) Uiso d 1 . .
H H2W3 0.4552(13) 0.417(4) 0.3683(5) 0.031(9) Uiso d 1 . .
N N1A 0.53728(11) 0.1701(3) 0.62582(6) 0.0169(5) Uani d 1 . .
H H1AA 0.4979(16) 0.123(4) 0.6303(8) 0.039(9) Uiso d 1 . .
H H1AB 0.5305(15) 0.293(4) 0.6212(8) 0.036(9) Uiso d 1 . .
N N2A 0.67722(10) 0.1578(3) 0.61970(5) 0.0153(5) Uani d 1 . .
C C1A 0.56652(12) 0.0802(3) 0.59424(7) 0.0166(6) Uani d 1 . .
H H1AC 0.536526 0.091693 0.572342 0.020 Uiso calc 1 . .
H H1AD 0.573059 -0.049571 0.599461 0.020 Uiso calc 1 . .
C C2A 0.63171(12) 0.1678(3) 0.58741(6) 0.0155(5) Uani d 1 . .
H H2AA 0.651615 0.106930 0.566729 0.019 Uiso calc 1 . .
H H2AB 0.624385 0.295573 0.580691 0.019 Uiso calc 1 . .
C C3A 0.64855(13) 0.2351(4) 0.65186(6) 0.0173(6) Uani d 1 . .
H H3A1 0.643210 0.366608 0.648468 0.021 Uiso calc 1 . .
H H3A2 0.678752 0.215151 0.673412 0.021 Uiso calc 1 . .
C C4A 0.58240(13) 0.1516(4) 0.65859(7) 0.0190(6) Uani d 1 . .
H H4AA 0.588228 0.022477 0.664660 0.023 Uiso calc 1 . .
H H4AB 0.563121 0.211922 0.679520 0.023 Uiso calc 1 . .
C C5A 0.74157(13) 0.2193(3) 0.61344(6) 0.0150(5) Uani d 1 . .
C C6A 0.77415(13) 0.1533(3) 0.58374(7) 0.0175(6) Uani d 1 . .
H H6A 0.752173 0.070253 0.567695 0.021 Uiso calc 1 . .
C C7A 0.83727(13) 0.2051(3) 0.57702(7) 0.0186(6) Uani d 1 . .
H H7A 0.857901 0.158525 0.556458 0.022 Uiso calc 1 . .
C C8A 0.87077(13) 0.3250(3) 0.60019(7) 0.0172(6) Uani d 1 . .
C C9A 0.83902(13) 0.3916(4) 0.62985(7) 0.0187(6) Uani d 1 . .
H H9A 0.861272 0.473954 0.645926 0.022 Uiso calc 1 . .
C C10A 0.77587(13) 0.3404(3) 0.63637(7) 0.0181(6) Uani d 1 . .
H H10A 0.755274 0.388262 0.656829 0.022 Uiso calc 1 . .
O O1A 0.93324(9) 0.3865(3) 0.59612(5) 0.0246(5) Uani d 1 . .
C C11A 0.96791(14) 0.3085(4) 0.56715(7) 0.0277(7) Uani d 1 . .
H H11A 1.012352 0.358505 0.567375 0.042 Uiso calc 1 . .
H H11B 0.944723 0.335895 0.543819 0.042 Uiso calc 1 . .
H H11C 0.970366 0.177628 0.570434 0.042 Uiso calc 1 . .
I I1A 0.07054(2) 0.22414(3) 0.65985(2) 0.03241(6) Uani d 1 . .
O O2A 0.41019(9) 0.0741(2) 0.64110(4) 0.0182(4) Uani d 1 . .
O O3A 0.38729(10) 0.2563(3) 0.59416(5) 0.0327(5) Uani d 1 . .
C C12A 0.37115(13) 0.1708(3) 0.62136(7) 0.0177(6) Uani d 1 . .
C C13A 0.30062(13) 0.1839(3) 0.63110(6) 0.0155(6) Uani d 1 . .
C C14A 0.25598(14) 0.2798(3) 0.60871(7) 0.0202(6) Uani d 1 . .
H H14A 0.270779 0.337633 0.587618 0.024 Uiso calc 1 . .
C C15A 0.19067(14) 0.2927(4) 0.61649(7) 0.0235(6) Uani d 1 . .
H H15A 0.160641 0.357675 0.600863 0.028 Uiso calc 1 . .
C C16A 0.16966(13) 0.2086(3) 0.64770(7) 0.0189(6) Uani d 1 . .
C C17A 0.21308(13) 0.1131(3) 0.67042(7) 0.0185(6) Uani d 1 . .
H H17A 0.198222 0.056099 0.691601 0.022 Uiso calc 1 . .
C C18A 0.27842(13) 0.1008(3) 0.66215(6) 0.0150(5) Uani d 1 . .
H H18A 0.308316 0.035272 0.677757 0.018 Uiso calc 1 . .
N N1B 0.54528(11) 0.2872(3) 0.46279(6) 0.0157(5) Uani d 1 . .
H H1BA 0.5047(15) 0.247(4) 0.4678(8) 0.032(9) Uiso d 1 . .
H H1BB 0.5413(13) 0.410(4) 0.4599(7) 0.019(7) Uiso d 1 . .
N N2B 0.68341(10) 0.2390(3) 0.45357(5) 0.0145(5) Uani d 1 . .
C C1B 0.57009(12) 0.1948(3) 0.43022(6) 0.0156(6) Uani d 1 . .
H H1BC 0.539379 0.215359 0.408906 0.019 Uiso calc 1 . .
H H1BD 0.572919 0.063524 0.434700 0.019 Uiso calc 1 . .
C C2B 0.63691(12) 0.2675(3) 0.42252(6) 0.0151(5) Uani d 1 . .
H H2BA 0.653183 0.206538 0.400822 0.018 Uiso calc 1 . .
H H2BB 0.633515 0.397882 0.417175 0.018 Uiso calc 1 . .
C C3B 0.66000(12) 0.3265(3) 0.48621(6) 0.0161(6) Uani d 1 . .
H H3B1 0.658596 0.458500 0.482408 0.019 Uiso calc 1 . .
H H3B2 0.691065 0.301479 0.507155 0.019 Uiso calc 1 . .
C C4B 0.59236(13) 0.2603(4) 0.49477(6) 0.0173(6) Uani d 1 . .
H H4BA 0.594522 0.130750 0.501113 0.021 Uiso calc 1 . .
H H4BB 0.576808 0.326780 0.515985 0.021 Uiso calc 1 . .
C C5B 0.75017(12) 0.2699(3) 0.44638(6) 0.0134(5) Uani d 1 . .
C C6B 0.77627(13) 0.1969(3) 0.41512(7) 0.0166(6) Uani d 1 . .
H H6B 0.747807 0.135704 0.398002 0.020 Uiso calc 1 . .
C C7B 0.84192(13) 0.2109(3) 0.40838(7) 0.0181(6) Uani d 1 . .
H H7B 0.857875 0.160425 0.386830 0.022 Uiso calc 1 . .
C C8B 0.88469(13) 0.2985(3) 0.43297(7) 0.0185(6) Uani d 1 . .
C C9B 0.85954(13) 0.3744(4) 0.46404(7) 0.0208(6) Uani d 1 . .
H H9B 0.888096 0.435936 0.481045 0.025 Uiso calc 1 . .
C C10B 0.79355(13) 0.3610(3) 0.47032(7) 0.0182(6) Uani d 1 . .
H H10B 0.777431 0.415177 0.491472 0.022 Uiso calc 1 . .
O O1B 0.95052(9) 0.3195(3) 0.42936(5) 0.0280(5) Uani d 1 . .
C C11B 0.97811(14) 0.2421(4) 0.39805(8) 0.0303(7) Uani d 1 . .
H H11D 1.025183 0.268615 0.398486 0.045 Uiso calc 1 . .
H H11E 0.956558 0.293296 0.375985 0.045 Uiso calc 1 . .
H H11F 0.971528 0.111410 0.398221 0.045 Uiso calc 1 . .
I I1B 0.07478(2) 0.15453(3) 0.49437(2) 0.02872(6) Uani d 1 . .
O O2B 0.41837(9) 0.1894(2) 0.47849(5) 0.0198(4) Uani d 1 . .
O O3B 0.38573(10) 0.3743(3) 0.43324(5) 0.0298(5) Uani d 1 . .
C C12B 0.37472(13) 0.2739(3) 0.45938(7) 0.0178(6) Uani d 1 . .
C C13B 0.30402(13) 0.2499(3) 0.46834(6) 0.0145(5) Uani d 1 . .
C C14B 0.25389(13) 0.3216(3) 0.44580(7) 0.0179(6) Uani d 1 . .
H H14B 0.264596 0.389536 0.425054 0.022 Uiso calc 1 . .
C C15B 0.18860(14) 0.2958(4) 0.45298(7) 0.0201(6) Uani d 1 . .
H H15B 0.154697 0.343937 0.437190 0.024 Uiso calc 1 . .
C C16B 0.17363(13) 0.1985(3) 0.48365(7) 0.0186(6) Uani d 1 . .
C C17B 0.22246(13) 0.1289(3) 0.50692(7) 0.0186(6) Uani d 1 . .
H H17B 0.211464 0.064335 0.528047 0.022 Uiso calc 1 . .
C C18B 0.28755(13) 0.1538(3) 0.49930(6) 0.0163(6) Uani d 1 . .
H H18B 0.321254 0.105354 0.515187 0.020 Uiso calc 1 . .
N N1C 0.54732(11) 0.4096(3) 0.30188(6) 0.0151(5) Uani d 1 . .
H H1CA 0.5039(15) 0.382(4) 0.3092(8) 0.036(9) Uiso d 1 . .
H H1CB 0.5487(13) 0.519(4) 0.2976(7) 0.012(7) Uiso d 1 . .
N N2C 0.67789(10) 0.2903(3) 0.28952(5) 0.0140(5) Uani d 1 . .
C C1C 0.56203(13) 0.3023(4) 0.26914(7) 0.0183(6) Uani d 1 . .
H H1CC 0.531549 0.337052 0.248527 0.022 Uiso calc 1 . .
H H1CD 0.555525 0.172679 0.274144 0.022 Uiso calc 1 . .
C C2C 0.63187(12) 0.3341(4) 0.25908(6) 0.0168(6) Uani d 1 . .
H H2CA 0.641494 0.258599 0.237828 0.020 Uiso calc 1 . .
H H2CB 0.637343 0.461852 0.252166 0.020 Uiso calc 1 . .
C C3C 0.66487(13) 0.3992(4) 0.32146(6) 0.0164(6) Uani d 1 . .
H H3C1 0.671354 0.528155 0.315826 0.020 Uiso calc 1 . .
H H3C2 0.696146 0.366146 0.341838 0.020 Uiso calc 1 . .
C C4C 0.59550(12) 0.3697(4) 0.33264(6) 0.0164(6) Uani d 1 . .
H H4CA 0.590283 0.243214 0.340487 0.020 Uiso calc 1 . .
H H4CB 0.586798 0.448762 0.353511 0.020 Uiso calc 1 . .
C C5C 0.74472(12) 0.2758(3) 0.28062(6) 0.0141(5) Uani d 1 . .
C C6C 0.76069(13) 0.1706(3) 0.25095(7) 0.0177(6) Uani d 1 . .
H H6C 0.726496 0.118494 0.235930 0.021 Uiso calc 1 . .
C C7C 0.82550(13) 0.1404(4) 0.24290(7) 0.0186(6) Uani d 1 . .
H H7C 0.835037 0.070293 0.222230 0.022 Uiso calc 1 . .
C C8C 0.87656(13) 0.2121(4) 0.26487(7) 0.0196(6) Uani d 1 . .
C C9C 0.86090(13) 0.3184(4) 0.29422(7) 0.0204(6) Uani d 1 . .
H H9C 0.895187 0.369408 0.309346 0.025 Uiso calc 1 . .
C C10C 0.79633(13) 0.3517(3) 0.30189(7) 0.0177(6) Uani d 1 . .
H H10C 0.786977 0.427006 0.321839 0.021 Uiso calc 1 . .
O O1C 0.94180(9) 0.1861(3) 0.26005(5) 0.0250(4) Uani d 1 . .
C C11C 0.95839(14) 0.0599(4) 0.23304(8) 0.0314(7) Uani d 1 . .
H H11G 1.006183 0.046967 0.233207 0.047 Uiso calc 1 . .
H H11H 0.941860 0.102414 0.209073 0.047 Uiso calc 1 . .
H H11I 0.938558 -0.056985 0.238193 0.047 Uiso calc 1 . .
I I1C 0.09042(2) 0.06781(3) 0.31910(2) 0.03020(6) Uani d 1 . .
O O2C 0.42707(9) 0.3016(2) 0.32290(5) 0.0202(4) Uani d 1 . .
O O3C 0.39400(9) 0.4141(2) 0.26896(5) 0.0235(4) Uani d 1 . .
C C12C 0.38327(13) 0.3315(3) 0.29758(7) 0.0167(6) Uani d 1 . .
C C13C 0.31525(13) 0.2627(3) 0.30286(7) 0.0155(6) Uani d 1 . .
C C14C 0.27202(13) 0.2325(4) 0.27301(7) 0.0192(6) Uani d 1 . .
H H14C 0.286224 0.254050 0.249216 0.023 Uiso calc 1 . .
C C15C 0.20884(14) 0.1719(4) 0.27722(7) 0.0212(6) Uani d 1 . .
H H15C 0.180102 0.148483 0.256620 0.025 Uiso calc 1 . .
C C16C 0.18836(13) 0.1459(3) 0.31218(7) 0.0198(6) Uani d 1 . .
C C17C 0.23004(13) 0.1737(3) 0.34227(7) 0.0204(6) Uani d 1 . .
H H17C 0.215262 0.154375 0.366023 0.024 Uiso calc 1 . .
C C18C 0.29359(13) 0.2299(3) 0.33759(7) 0.0172(6) Uani d 1 . .
H H18C 0.322853 0.246385 0.358253 0.021 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1W 0.0265(12) 0.0229(11) 0.0167(10) -0.0040(9) -0.0009(9) -0.0004(9)
O2W 0.0214(11) 0.0235(11) 0.0165(10) -0.0031(9) 0.0052(9) 0.0010(9)
O3W 0.0203(11) 0.0206(11) 0.0162(10) -0.0003(9) 0.0046(9) -0.0003(9)
N1A 0.0159(13) 0.0171(12) 0.0181(11) -0.0011(10) 0.0039(9) 0.0005(10)
N2A 0.0131(11) 0.0181(11) 0.0149(10) -0.0004(9) 0.0023(9) -0.0008(9)
C1A 0.0151(14) 0.0154(13) 0.0195(13) 0.0004(11) 0.0023(11) -0.0022(11)
C2A 0.0143(14) 0.0174(13) 0.0148(12) -0.0001(11) 0.0021(10) -0.0003(11)
C3A 0.0176(14) 0.0226(14) 0.0118(12) 0.0011(12) 0.0027(10) -0.0008(11)
C4A 0.0172(14) 0.0234(15) 0.0169(13) 0.0007(12) 0.0045(11) 0.0036(11)
C5A 0.0144(14) 0.0156(13) 0.0151(12) 0.0021(11) 0.0020(10) 0.0020(10)
C6A 0.0169(14) 0.0176(14) 0.0178(13) -0.0018(11) 0.0005(11) -0.0041(11)
C7A 0.0190(15) 0.0186(14) 0.0184(13) -0.0003(12) 0.0037(11) -0.0044(11)
C8A 0.0135(14) 0.0154(13) 0.0227(13) 0.0011(11) 0.0023(11) 0.0019(11)
C9A 0.0188(15) 0.0187(14) 0.0184(13) -0.0014(12) -0.0022(11) -0.0046(11)
C10A 0.0192(15) 0.0209(14) 0.0144(12) 0.0023(12) 0.0023(11) -0.0048(11)
O1A 0.0158(10) 0.0288(11) 0.0298(11) -0.0064(9) 0.0071(8) -0.0099(9)
C11A 0.0202(16) 0.0354(18) 0.0285(15) -0.0036(14) 0.0106(13) -0.0057(13)
I1A 0.01674(11) 0.02892(11) 0.05171(13) 0.00099(9) 0.00330(9) -0.01156(10)
O2A 0.0175(10) 0.0203(10) 0.0172(9) -0.0023(8) 0.0037(8) -0.0022(8)
O3A 0.0343(13) 0.0381(13) 0.0272(11) -0.0018(10) 0.0153(10) 0.0115(9)
C12A 0.0219(15) 0.0157(13) 0.0161(13) -0.0048(12) 0.0049(11) -0.0050(11)
C13A 0.0187(14) 0.0117(13) 0.0163(12) -0.0049(11) 0.0036(11) -0.0033(10)
C14A 0.0309(17) 0.0133(13) 0.0165(13) -0.0043(12) 0.0016(12) 0.0018(11)
C15A 0.0240(16) 0.0169(14) 0.0289(15) 0.0013(12) -0.0063(13) -0.0009(12)
C16A 0.0144(14) 0.0157(13) 0.0266(14) -0.0033(11) 0.0008(11) -0.0078(11)
C17A 0.0194(15) 0.0163(13) 0.0202(13) -0.0021(12) 0.0054(11) 0.0001(11)
C18A 0.0183(14) 0.0118(12) 0.0150(12) -0.0017(11) 0.0014(10) -0.0003(10)
N1B 0.0149(12) 0.0150(12) 0.0173(11) -0.0009(10) 0.0026(9) -0.0006(9)
N2B 0.0153(12) 0.0160(11) 0.0122(10) -0.0009(9) 0.0012(9) -0.0021(9)
C1B 0.0146(14) 0.0169(13) 0.0156(12) -0.0003(11) 0.0018(10) -0.0011(10)
C2B 0.0160(14) 0.0181(13) 0.0112(12) 0.0007(11) 0.0017(10) -0.0018(10)
C3B 0.0172(14) 0.0200(14) 0.0113(12) -0.0013(11) 0.0015(10) -0.0020(10)
C4B 0.0186(14) 0.0197(14) 0.0137(12) -0.0005(12) 0.0018(11) 0.0003(11)
C5B 0.0164(14) 0.0098(12) 0.0137(12) 0.0006(11) -0.0013(10) 0.0015(10)
C6B 0.0187(14) 0.0145(13) 0.0163(13) -0.0023(11) -0.0005(11) -0.0029(10)
C7B 0.0201(15) 0.0158(13) 0.0186(13) -0.0015(12) 0.0026(11) -0.0044(11)
C8B 0.0141(14) 0.0169(14) 0.0247(14) 0.0006(11) 0.0020(11) 0.0000(11)
C9B 0.0206(15) 0.0222(15) 0.0193(13) -0.0040(12) -0.0032(11) -0.0065(11)
C10B 0.0218(15) 0.0182(14) 0.0147(12) 0.0024(12) 0.0019(11) -0.0032(11)
O1B 0.0137(10) 0.0354(12) 0.0351(11) -0.0036(9) 0.0042(9) -0.0124(9)
C11B 0.0209(16) 0.0357(18) 0.0352(17) -0.0038(14) 0.0105(13) -0.0099(14)
I1B 0.01675(10) 0.02811(11) 0.04205(12) -0.00272(8) 0.00875(8) -0.00998(9)
O2B 0.0172(10) 0.0225(10) 0.0201(9) -0.0013(8) 0.0046(8) -0.0032(8)
O3B 0.0288(12) 0.0302(12) 0.0318(11) -0.0017(10) 0.0138(9) 0.0118(9)
C12B 0.0227(15) 0.0143(13) 0.0168(13) -0.0043(12) 0.0061(11) -0.0069(11)
C13B 0.0195(14) 0.0099(12) 0.0142(12) -0.0023(11) 0.0042(11) -0.0035(10)
C14B 0.0244(15) 0.0155(13) 0.0139(12) -0.0051(12) 0.0003(11) -0.0001(10)
C15B 0.0212(15) 0.0175(14) 0.0212(14) -0.0001(12) -0.0036(11) -0.0016(11)
C16B 0.0151(14) 0.0159(13) 0.0254(14) -0.0006(11) 0.0063(11) -0.0054(11)
C17B 0.0226(15) 0.0139(13) 0.0200(13) -0.0004(12) 0.0078(11) 0.0017(11)
C18B 0.0193(14) 0.0153(13) 0.0143(12) 0.0017(11) 0.0020(11) 0.0010(11)
N1C 0.0162(13) 0.0145(12) 0.0147(11) -0.0014(10) 0.0001(9) 0.0002(9)
N2C 0.0143(11) 0.0166(11) 0.0111(10) 0.0006(9) 0.0010(9) -0.0015(8)
C1C 0.0172(14) 0.0209(14) 0.0169(13) 0.0001(12) 0.0005(11) -0.0040(11)
C2C 0.0158(14) 0.0212(14) 0.0132(12) 0.0010(11) -0.0005(10) -0.0002(11)
C3C 0.0177(14) 0.0198(14) 0.0116(12) 0.0000(11) 0.0003(10) -0.0012(10)
C4C 0.0195(14) 0.0181(14) 0.0116(12) 0.0016(12) 0.0002(10) 0.0009(10)
C5C 0.0149(14) 0.0127(12) 0.0146(12) -0.0019(11) 0.0001(10) 0.0027(10)
C6C 0.0163(14) 0.0201(14) 0.0166(13) -0.0025(12) -0.0015(11) -0.0024(11)
C7C 0.0173(14) 0.0208(14) 0.0182(13) 0.0001(12) 0.0038(11) -0.0027(11)
C8C 0.0181(15) 0.0165(13) 0.0245(14) -0.0009(12) 0.0045(12) 0.0057(11)
C9C 0.0190(15) 0.0197(14) 0.0222(14) -0.0047(12) -0.0031(11) -0.0014(11)
C10C 0.0213(15) 0.0135(13) 0.0183(13) -0.0012(12) 0.0006(11) -0.0013(11)
O1C 0.0143(10) 0.0282(11) 0.0330(11) -0.0004(9) 0.0054(8) -0.0037(9)
C11C 0.0221(17) 0.0376(18) 0.0352(17) 0.0049(14) 0.0083(13) -0.0043(15)
I1C 0.01743(10) 0.02945(11) 0.04390(12) -0.00327(8) 0.00347(8) -0.00136(9)
O2C 0.0165(10) 0.0249(11) 0.0194(9) -0.0022(8) 0.0017(8) 0.0013(8)
O3C 0.0266(11) 0.0239(10) 0.0208(10) 0.0009(9) 0.0075(8) 0.0070(8)
C12C 0.0204(15) 0.0119(13) 0.0184(13) 0.0016(11) 0.0061(11) -0.0043(11)
C13C 0.0203(15) 0.0090(12) 0.0175(13) 0.0026(11) 0.0026(11) -0.0012(10)
C14C 0.0201(15) 0.0206(14) 0.0172(13) 0.0042(12) 0.0030(11) -0.0018(11)
C15C 0.0216(15) 0.0200(14) 0.0215(14) 0.0033(12) -0.0030(12) -0.0060(12)
C16C 0.0134(14) 0.0149(13) 0.0311(15) 0.0027(11) 0.0031(12) -0.0010(12)
C17C 0.0224(15) 0.0179(14) 0.0213(13) 0.0026(12) 0.0050(12) 0.0033(11)
C18C 0.0188(15) 0.0160(13) 0.0168(13) 0.0009(11) 0.0001(11) 0.0013(11)
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'
I I -0.4742 1.8119 '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_
_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
H1W1 O1W H2W1 . . 106(2) ?
H1W2 O2W H2W2 . . 105(2) ?
H1W3 O3W H2W3 . . 104(2) ?
C4A N1A C1A . . 109.6(2) ?
C4A N1A H1AA . . 110(2) ?
C1A N1A H1AA . . 111(2) ?
C4A N1A H1AB . . 108.4(19) ?
C1A N1A H1AB . . 110.9(18) ?
H1AA N1A H1AB . . 107(3) ?
C5A N2A C3A . . 114.6(2) ?
C5A N2A C2A . . 113.78(19) ?
C3A N2A C2A . . 111.8(2) ?
N1A C1A C2A . . 109.1(2) ?
N1A C1A H1AC . . 109.9 ?
C2A C1A H1AC . . 109.9 ?
N1A C1A H1AD . . 109.9 ?
C2A C1A H1AD . . 109.9 ?
H1AC C1A H1AD . . 108.3 ?
N2A C2A C1A . . 111.6(2) ?
N2A C2A H2AA . . 109.3 ?
C1A C2A H2AA . . 109.3 ?
N2A C2A H2AB . . 109.3 ?
C1A C2A H2AB . . 109.3 ?
H2AA C2A H2AB . . 108.0 ?
N2A C3A C4A . . 111.6(2) ?
N2A C3A H3A1 . . 109.3 ?
C4A C3A H3A1 . . 109.3 ?
N2A C3A H3A2 . . 109.3 ?
C4A C3A H3A2 . . 109.3 ?
H3A1 C3A H3A2 . . 108.0 ?
N1A C4A C3A . . 110.4(2) ?
N1A C4A H4AA . . 109.6 ?
C3A C4A H4AA . . 109.6 ?
N1A C4A H4AB . . 109.6 ?
C3A C4A H4AB . . 109.6 ?
H4AA C4A H4AB . . 108.1 ?
C10A C5A C6A . . 117.0(2) ?
C10A C5A N2A . . 123.2(2) ?
C6A C5A N2A . . 119.7(2) ?
C7A C6A C5A . . 122.0(2) ?
C7A C6A H6A . . 119.0 ?
C5A C6A H6A . . 119.0 ?
C6A C7A C8A . . 120.3(2) ?
C6A C7A H7A . . 119.9 ?
C8A C7A H7A . . 119.9 ?
O1A C8A C7A . . 125.3(2) ?
O1A C8A C9A . . 116.2(2) ?
C7A C8A C9A . . 118.4(2) ?
C10A C9A C8A . . 121.2(2) ?
C10A C9A H9A . . 119.4 ?
C8A C9A H9A . . 119.4 ?
C9A C10A C5A . . 121.1(2) ?
C9A C10A H10A . . 119.4 ?
C5A C10A H10A . . 119.4 ?
C8A O1A C11A . . 116.4(2) ?
O1A C11A H11A . . 109.5 ?
O1A C11A H11B . . 109.5 ?
H11A C11A H11B . . 109.5 ?
O1A C11A H11C . . 109.5 ?
H11A C11A H11C . . 109.5 ?
H11B C11A H11C . . 109.5 ?
O3A C12A O2A . . 124.3(2) ?
O3A C12A C13A . . 117.1(2) ?
O2A C12A C13A . . 118.6(2) ?
C14A C13A C18A . . 118.7(2) ?
C14A C13A C12A . . 119.8(2) ?
C18A C13A C12A . . 121.5(2) ?
C15A C14A C13A . . 121.5(2) ?
C15A C14A H14A . . 119.3 ?
C13A C14A H14A . . 119.3 ?
C14A C15A C16A . . 118.7(3) ?
C14A C15A H15A . . 120.6 ?
C16A C15A H15A . . 120.6 ?
C17A C16A C15A . . 120.9(2) ?
C17A C16A I1A . . 119.64(19) ?
C15A C16A I1A . . 119.5(2) ?
C16A C17A C18A . . 119.7(2) ?
C16A C17A H17A . . 120.2 ?
C18A C17A H17A . . 120.2 ?
C17A C18A C13A . . 120.5(2) ?
C17A C18A H18A . . 119.7 ?
C13A C18A H18A . . 119.7 ?
C1B N1B C4B . . 109.9(2) ?
C1B N1B H1BA . . 111.2(18) ?
C4B N1B H1BA . . 110.7(18) ?
C1B N1B H1BB . . 113.3(16) ?
C4B N1B H1BB . . 105.8(17) ?
H1BA N1B H1BB . . 106(2) ?
C5B N2B C2B . . 114.91(19) ?
C5B N2B C3B . . 115.9(2) ?
C2B N2B C3B . . 110.5(2) ?
N1B C1B C2B . . 109.5(2) ?
N1B C1B H1BC . . 109.8 ?
C2B C1B H1BC . . 109.8 ?
N1B C1B H1BD . . 109.8 ?
C2B C1B H1BD . . 109.8 ?
H1BC C1B H1BD . . 108.2 ?
N2B C2B C1B . . 111.0(2) ?
N2B C2B H2BA . . 109.4 ?
C1B C2B H2BA . . 109.4 ?
N2B C2B H2BB . . 109.4 ?
C1B C2B H2BB . . 109.4 ?
H2BA C2B H2BB . . 108.0 ?
N2B C3B C4B . . 111.4(2) ?
N2B C3B H3B1 . . 109.3 ?
C4B C3B H3B1 . . 109.3 ?
N2B C3B H3B2 . . 109.3 ?
C4B C3B H3B2 . . 109.3 ?
H3B1 C3B H3B2 . . 108.0 ?
N1B C4B C3B . . 110.4(2) ?
N1B C4B H4BA . . 109.6 ?
C3B C4B H4BA . . 109.6 ?
N1B C4B H4BB . . 109.6 ?
C3B C4B H4BB . . 109.6 ?
H4BA C4B H4BB . . 108.1 ?
C10B C5B C6B . . 116.8(2) ?
C10B C5B N2B . . 123.1(2) ?
C6B C5B N2B . . 120.0(2) ?
C7B C6B C5B . . 122.2(2) ?
C7B C6B H6B . . 118.9 ?
C5B C6B H6B . . 118.9 ?
C6B C7B C8B . . 120.2(2) ?
C6B C7B H7B . . 119.9 ?
C8B C7B H7B . . 119.9 ?
O1B C8B C7B . . 125.4(2) ?
O1B C8B C9B . . 116.0(2) ?
C7B C8B C9B . . 118.6(2) ?
C10B C9B C8B . . 120.7(2) ?
C10B C9B H9B . . 119.6 ?
C8B C9B H9B . . 119.6 ?
C9B C10B C5B . . 121.5(2) ?
C9B C10B H10B . . 119.2 ?
C5B C10B H10B . . 119.2 ?
C8B O1B C11B . . 117.6(2) ?
O1B C11B H11D . . 109.5 ?
O1B C11B H11E . . 109.5 ?
H11D C11B H11E . . 109.5 ?
O1B C11B H11F . . 109.5 ?
H11D C11B H11F . . 109.5 ?
H11E C11B H11F . . 109.5 ?
O3B C12B O2B . . 124.9(2) ?
O3B C12B C13B . . 116.9(2) ?
O2B C12B C13B . . 118.1(2) ?
C14B C13B C18B . . 118.7(2) ?
C14B C13B C12B . . 120.5(2) ?
C18B C13B C12B . . 120.8(2) ?
C15B C14B C13B . . 121.3(2) ?
C15B C14B H14B . . 119.4 ?
C13B C14B H14B . . 119.4 ?
C14B C15B C16B . . 118.8(3) ?
C14B C15B H15B . . 120.6 ?
C16B C15B H15B . . 120.6 ?
C17B C16B C15B . . 121.1(2) ?
C17B C16B I1B . . 119.67(18) ?
C15B C16B I1B . . 119.2(2) ?
C16B C17B C18B . . 119.6(2) ?
C16B C17B H17B . . 120.2 ?
C18B C17B H17B . . 120.2 ?
C17B C18B C13B . . 120.4(3) ?
C17B C18B H18B . . 119.8 ?
C13B C18B H18B . . 119.8 ?
C1C N1C C4C . . 110.8(2) ?
C1C N1C H1CA . . 110.1(18) ?
C4C N1C H1CA . . 109.0(18) ?
C1C N1C H1CB . . 111.1(17) ?
C4C N1C H1CB . . 108.2(19) ?
H1CA N1C H1CB . . 108(3) ?
C5C N2C C2C . . 115.22(19) ?
C5C N2C C3C . . 116.3(2) ?
C2C N2C C3C . . 110.9(2) ?
N1C C1C C2C . . 110.3(2) ?
N1C C1C H1CC . . 109.6 ?
C2C C1C H1CC . . 109.6 ?
N1C C1C H1CD . . 109.6 ?
C2C C1C H1CD . . 109.6 ?
H1CC C1C H1CD . . 108.1 ?
N2C C2C C1C . . 110.8(2) ?
N2C C2C H2CA . . 109.5 ?
C1C C2C H2CA . . 109.5 ?
N2C C2C H2CB . . 109.5 ?
C1C C2C H2CB . . 109.5 ?
H2CA C2C H2CB . . 108.1 ?
N2C C3C C4C . . 110.5(2) ?
N2C C3C H3C1 . . 109.5 ?
C4C C3C H3C1 . . 109.5 ?
N2C C3C H3C2 . . 109.5 ?
C4C C3C H3C2 . . 109.5 ?
H3C1 C3C H3C2 . . 108.1 ?
N1C C4C C3C . . 110.8(2) ?
N1C C4C H4CA . . 109.5 ?
C3C C4C H4CA . . 109.5 ?
N1C C4C H4CB . . 109.5 ?
C3C C4C H4CB . . 109.5 ?
H4CA C4C H4CB . . 108.1 ?
C6C C5C C10C . . 117.7(2) ?
C6C C5C N2C . . 119.2(2) ?
C10C C5C N2C . . 123.0(2) ?
C7C C6C C5C . . 121.4(2) ?
C7C C6C H6C . . 119.3 ?
C5C C6C H6C . . 119.3 ?
C6C C7C C8C . . 120.5(2) ?
C6C C7C H7C . . 119.8 ?
C8C C7C H7C . . 119.8 ?
O1C C8C C9C . . 116.5(2) ?
O1C C8C C7C . . 125.2(2) ?
C9C C8C C7C . . 118.3(2) ?
C10C C9C C8C . . 121.3(3) ?
C10C C9C H9C . . 119.3 ?
C8C C9C H9C . . 119.3 ?
C9C C10C C5C . . 120.8(2) ?
C9C C10C H10C . . 119.6 ?
C5C C10C H10C . . 119.6 ?
C8C O1C C11C . . 117.0(2) ?
O1C C11C H11G . . 109.5 ?
O1C C11C H11H . . 109.5 ?
H11G C11C H11H . . 109.5 ?
O1C C11C H11I . . 109.5 ?
H11G C11C H11I . . 109.5 ?
H11H C11C H11I . . 109.5 ?
O3C C12C O2C . . 123.7(2) ?
O3C C12C C13C . . 118.7(2) ?
O2C C12C C13C . . 117.6(2) ?
C14C C13C C18C . . 118.5(2) ?
C14C C13C C12C . . 120.4(2) ?
C18C C13C C12C . . 121.1(2) ?
C15C C14C C13C . . 121.4(2) ?
C15C C14C H14C . . 119.3 ?
C13C C14C H14C . . 119.3 ?
C14C C15C C16C . . 118.5(3) ?
C14C C15C H15C . . 120.8 ?
C16C C15C H15C . . 120.8 ?
C17C C16C C15C . . 121.5(3) ?
C17C C16C I1C . . 119.61(19) ?
C15C C16C I1C . . 118.9(2) ?
C16C C17C C18C . . 119.3(2) ?
C16C C17C H17C . . 120.3 ?
C18C C17C H17C . . 120.3 ?
C17C C18C C13C . . 120.7(3) ?
C17C C18C H18C . . 119.6 ?
C13C C18C H18C . . 119.6 ?
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
O1W H1W1 . 0.769(15) ?
O1W H2W1 . 0.768(15) ?
O2W H1W2 . 0.770(14) ?
O2W H2W2 . 0.774(15) ?
O3W H1W3 . 0.771(15) ?
O3W H2W3 . 0.775(14) ?
N1A C4A . 1.486(3) ?
N1A C1A . 1.491(3) ?
N1A H1AA . 0.90(3) ?
N1A H1AB . 0.94(3) ?
N2A C5A . 1.421(3) ?
N2A C3A . 1.464(3) ?
N2A C2A . 1.472(3) ?
C1A C2A . 1.514(3) ?
C1A H1AC . 0.9900 ?
C1A H1AD . 0.9900 ?
C2A H2AA . 0.9900 ?
C2A H2AB . 0.9900 ?
C3A C4A . 1.518(3) ?
C3A H3A1 . 0.9900 ?
C3A H3A2 . 0.9900 ?
C4A H4AA . 0.9900 ?
C4A H4AB . 0.9900 ?
C5A C10A . 1.396(4) ?
C5A C6A . 1.397(3) ?
C6A C7A . 1.379(3) ?
C6A H6A . 0.9500 ?
C7A C8A . 1.388(4) ?
C7A H7A . 0.9500 ?
C8A O1A . 1.370(3) ?
C8A C9A . 1.389(3) ?
C9A C10A . 1.377(4) ?
C9A H9A . 0.9500 ?
C10A H10A . 0.9500 ?
O1A C11A . 1.432(3) ?
C11A H11A . 0.9800 ?
C11A H11B . 0.9800 ?
C11A H11C . 0.9800 ?
I1A C16A . 2.098(3) ?
O2A C12A . 1.272(3) ?
O3A C12A . 1.244(3) ?
C12A C13A . 1.505(3) ?
C13A C14A . 1.392(4) ?
C13A C18A . 1.394(3) ?
C14A C15A . 1.381(4) ?
C14A H14A . 0.9500 ?
C15A C16A . 1.394(4) ?
C15A H15A . 0.9500 ?
C16A C17A . 1.383(4) ?
C17A C18A . 1.386(3) ?
C17A H17A . 0.9500 ?
C18A H18A . 0.9500 ?
N1B C1B . 1.492(3) ?
N1B C4B . 1.494(3) ?
N1B H1BA . 0.91(3) ?
N1B H1BB . 0.92(3) ?
N2B C5B . 1.420(3) ?
N2B C2B . 1.462(3) ?
N2B C3B . 1.467(3) ?
C1B C2B . 1.507(3) ?
C1B H1BC . 0.9900 ?
C1B H1BD . 0.9900 ?
C2B H2BA . 0.9900 ?
C2B H2BB . 0.9900 ?
C3B C4B . 1.514(3) ?
C3B H3B1 . 0.9900 ?
C3B H3B2 . 0.9900 ?
C4B H4BA . 0.9900 ?
C4B H4BB . 0.9900 ?
C5B C10B . 1.392(4) ?
C5B C6B . 1.402(3) ?
C6B C7B . 1.379(3) ?
C6B H6B . 0.9500 ?
C7B C8B . 1.386(4) ?
C7B H7B . 0.9500 ?
C8B O1B . 1.366(3) ?
C8B C9B . 1.396(3) ?
C9B C10B . 1.382(4) ?
C9B H9B . 0.9500 ?
C10B H10B . 0.9500 ?
O1B C11B . 1.429(3) ?
C11B H11D . 0.9800 ?
C11B H11E . 0.9800 ?
C11B H11F . 0.9800 ?
I1B C16B . 2.101(3) ?
O2B C12B . 1.272(3) ?
O3B C12B . 1.246(3) ?
C12B C13B . 1.507(3) ?
C13B C14B . 1.389(4) ?
C13B C18B . 1.400(3) ?
C14B C15B . 1.385(4) ?
C14B H14B . 0.9500 ?
C15B C16B . 1.388(4) ?
C15B H15B . 0.9500 ?
C16B C17B . 1.380(4) ?
C17B C18B . 1.384(3) ?
C17B H17B . 0.9500 ?
C18B H18B . 0.9500 ?
N1C C1C . 1.488(3) ?
N1C C4C . 1.490(3) ?
N1C H1CA . 0.96(3) ?
N1C H1CB . 0.83(3) ?
N2C C5C . 1.424(3) ?
N2C C2C . 1.461(3) ?
N2C C3C . 1.462(3) ?
C1C C2C . 1.510(3) ?
C1C H1CC . 0.9900 ?
C1C H1CD . 0.9900 ?
C2C H2CA . 0.9900 ?
C2C H2CB . 0.9900 ?
C3C C4C . 1.511(3) ?
C3C H3C1 . 0.9900 ?
C3C H3C2 . 0.9900 ?
C4C H4CA . 0.9900 ?
C4C H4CB . 0.9900 ?
C5C C6C . 1.395(3) ?
C5C C10C . 1.398(4) ?
C6C C7C . 1.389(3) ?
C6C H6C . 0.9500 ?
C7C C8C . 1.392(4) ?
C7C H7C . 0.9500 ?
C8C O1C . 1.366(3) ?
C8C C9C . 1.388(4) ?
C9C C10C . 1.384(4) ?
C9C H9C . 0.9500 ?
C10C H10C . 0.9500 ?
O1C C11C . 1.420(3) ?
C11C H11G . 0.9800 ?
C11C H11H . 0.9800 ?
C11C H11I . 0.9800 ?
I1C C16C . 2.110(3) ?
O2C C12C . 1.277(3) ?
O3C C12C . 1.248(3) ?
C12C C13C . 1.501(4) ?
C13C C14C . 1.391(4) ?
C13C C18C . 1.395(3) ?
C14C C15C . 1.382(4) ?
C14C H14C . 0.9500 ?
C15C C16C . 1.387(3) ?
C15C H15C . 0.9500 ?
C16C C17C . 1.376(4) ?
C17C C18C . 1.382(4) ?
C17C H17C . 0.9500 ?
C18C H18C . 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
_geom_hbond_publ_flag
O1W H1W1 O3C 4_566 0.769(15) 1.931(15) 2.696(3) 173(3) yes
O1W H2W1 O2A . 0.768(15) 1.958(16) 2.700(3) 162(3) yes
O2W H1W2 O3A . 0.770(14) 1.864(15) 2.626(2) 170(3) yes
O2W H2W2 O2B . 0.774(15) 1.971(16) 2.733(3) 168(3) yes
O3W H1W3 O3B . 0.771(15) 1.871(16) 2.636(2) 172(3) yes
O3W H2W3 O2C . 0.775(14) 1.937(15) 2.706(3) 172(3) yes
N1A H1AB O3W 3_666 0.94(3) 1.82(3) 2.754(3) 172(3) yes
N1A H1AA O2A . 0.90(3) 1.89(3) 2.776(3) 168(3) yes
C1A H1AC O2W . 0.99 2.57 3.362(3) 136 yes
C2A H2AB O3B 3_666 0.99 2.51 3.498(3) 175 yes
C4A H4AA O2C 3_656 0.99 2.47 3.441(3) 166 yes
C7A H7A I1B 3_656 0.95 3.32 4.212(2) 156 yes
C11A H11A O1B 3_766 0.98 2.51 3.225(4) 130 yes
N1B H1BA O2B . 0.91(3) 1.87(3) 2.780(3) 174(3) yes
N1B H1BB O2W 3_666 0.92(3) 1.85(3) 2.768(3) 176(2) yes
C1B H1BC O3W . 0.99 2.44 3.229(3) 136 yes
C2B H2BB O3A 3_666 0.99 2.63 3.619(3) 174 yes
C4B H4BA O2B 3_656 0.99 2.51 3.491(3) 170 yes
C4B H4BB O2W . 0.99 2.52 3.260(3) 131 yes
C9B H9B I1B 3_666 0.95 3.25 4.020(3) 139 yes
N1C H1CA O2C . 0.96(3) 1.78(3) 2.732(3) 172(3) yes
N1C H1CA O3C . 0.96(3) 2.64(3) 3.297(3) 126(2) yes
N1C H1CB O1W 3_666 0.83(3) 1.96(3) 2.781(3) 172(3) yes
C1C H1CC O1W 4_565 0.99 2.39 3.299(3) 152 yes
C4C H4CA O2A 3_656 0.99 2.45 3.438(3) 174 yes
C9C H9C I1A 3_666 0.95 3.29 4.013(3) 135 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
C4A N1A C1A C2A . . . . -59.7(3) ?
C5A N2A C2A C1A . . . . 173.1(2) ?
C3A N2A C2A C1A . . . . -55.1(3) ?
N1A C1A C2A N2A . . . . 58.0(3) ?
C5A N2A C3A C4A . . . . -175.2(2) ?
C2A N2A C3A C4A . . . . 53.5(3) ?
C1A N1A C4A C3A . . . . 58.9(3) ?
N2A C3A C4A N1A . . . . -55.7(3) ?
C3A N2A C5A C10A . . . . 1.4(3) ?
C2A N2A C5A C10A . . . . 131.8(3) ?
C3A N2A C5A C6A . . . . 179.3(2) ?
C2A N2A C5A C6A . . . . -50.3(3) ?
C10A C5A C6A C7A . . . . -0.3(4) ?
N2A C5A C6A C7A . . . . -178.3(2) ?
C5A C6A C7A C8A . . . . 0.6(4) ?
C6A C7A C8A O1A . . . . -179.6(2) ?
C6A C7A C8A C9A . . . . -0.5(4) ?
O1A C8A C9A C10A . . . . 179.3(2) ?
C7A C8A C9A C10A . . . . 0.1(4) ?
C8A C9A C10A C5A . . . . 0.2(4) ?
C6A C5A C10A C9A . . . . -0.1(4) ?
N2A C5A C10A C9A . . . . 177.8(2) ?
C7A C8A O1A C11A . . . . -5.2(4) ?
C9A C8A O1A C11A . . . . 175.6(2) ?
O3A C12A C13A C14A . . . . 3.8(4) ?
O2A C12A C13A C14A . . . . -176.1(2) ?
O3A C12A C13A C18A . . . . -176.6(2) ?
O2A C12A C13A C18A . . . . 3.5(4) ?
C18A C13A C14A C15A . . . . -0.5(4) ?
C12A C13A C14A C15A . . . . 179.1(2) ?
C13A C14A C15A C16A . . . . 0.6(4) ?
C14A C15A C16A C17A . . . . -0.4(4) ?
C14A C15A C16A I1A . . . . -179.42(19) ?
C15A C16A C17A C18A . . . . 0.1(4) ?
I1A C16A C17A C18A . . . . 179.17(19) ?
C16A C17A C18A C13A . . . . -0.1(4) ?
C14A C13A C18A C17A . . . . 0.3(4) ?
C12A C13A C18A C17A . . . . -179.3(2) ?
C4B N1B C1B C2B . . . . -58.0(3) ?
C5B N2B C2B C1B . . . . 168.0(2) ?
C3B N2B C2B C1B . . . . -58.5(3) ?
N1B C1B C2B N2B . . . . 59.4(3) ?
C5B N2B C3B C4B . . . . -170.5(2) ?
C2B N2B C3B C4B . . . . 56.6(3) ?
C1B N1B C4B C3B . . . . 56.4(3) ?
N2B C3B C4B N1B . . . . -55.9(3) ?
C2B N2B C5B C10B . . . . 137.5(2) ?
C3B N2B C5B C10B . . . . 6.6(3) ?
C2B N2B C5B C6B . . . . -46.9(3) ?
C3B N2B C5B C6B . . . . -177.8(2) ?
C10B C5B C6B C7B . . . . 1.1(4) ?
N2B C5B C6B C7B . . . . -174.8(2) ?
C5B C6B C7B C8B . . . . 0.4(4) ?
C6B C7B C8B O1B . . . . 179.5(2) ?
C6B C7B C8B C9B . . . . -1.3(4) ?
O1B C8B C9B C10B . . . . 180.0(2) ?
C7B C8B C9B C10B . . . . 0.6(4) ?
C8B C9B C10B C5B . . . . 0.9(4) ?
C6B C5B C10B C9B . . . . -1.7(4) ?
N2B C5B C10B C9B . . . . 174.0(2) ?
C7B C8B O1B C11B . . . . -1.3(4) ?
C9B C8B O1B C11B . . . . 179.4(2) ?
O3B C12B C13B C14B . . . . 6.7(4) ?
O2B C12B C13B C14B . . . . -172.3(2) ?
O3B C12B C13B C18B . . . . -173.8(2) ?
O2B C12B C13B C18B . . . . 7.1(3) ?
C18B C13B C14B C15B . . . . -1.6(4) ?
C12B C13B C14B C15B . . . . 177.9(2) ?
C13B C14B C15B C16B . . . . 0.9(4) ?
C14B C15B C16B C17B . . . . 0.4(4) ?
C14B C15B C16B I1B . . . . -178.92(18) ?
C15B C16B C17B C18B . . . . -1.1(4) ?
I1B C16B C17B C18B . . . . 178.25(19) ?
C16B C17B C18B C13B . . . . 0.4(4) ?
C14B C13B C18B C17B . . . . 0.9(4) ?
C12B C13B C18B C17B . . . . -178.6(2) ?
C4C N1C C1C C2C . . . . -55.2(3) ?
C5C N2C C2C C1C . . . . 166.3(2) ?
C3C N2C C2C C1C . . . . -59.0(3) ?
N1C C1C C2C N2C . . . . 57.1(3) ?
C5C N2C C3C C4C . . . . -167.4(2) ?
C2C N2C C3C C4C . . . . 58.4(3) ?
C1C N1C C4C C3C . . . . 55.1(3) ?
N2C C3C C4C N1C . . . . -56.4(3) ?
C2C N2C C5C C6C . . . . -49.1(3) ?
C3C N2C C5C C6C . . . . 178.6(2) ?
C2C N2C C5C C10C . . . . 135.7(2) ?
C3C N2C C5C C10C . . . . 3.5(3) ?
C10C C5C C6C C7C . . . . 0.6(4) ?
N2C C5C C6C C7C . . . . -174.8(2) ?
C5C C6C C7C C8C . . . . 1.3(4) ?
C6C C7C C8C O1C . . . . 177.9(2) ?
C6C C7C C8C C9C . . . . -1.9(4) ?
O1C C8C C9C C10C . . . . -179.2(2) ?
C7C C8C C9C C10C . . . . 0.6(4) ?
C8C C9C C10C C5C . . . . 1.3(4) ?
C6C C5C C10C C9C . . . . -1.9(4) ?
N2C C5C C10C C9C . . . . 173.3(2) ?
C9C C8C O1C C11C . . . . 172.3(2) ?
C7C C8C O1C C11C . . . . -7.6(4) ?
O3C C12C C13C C14C . . . . 22.7(4) ?
O2C C12C C13C C14C . . . . -157.3(2) ?
O3C C12C C13C C18C . . . . -156.5(2) ?
O2C C12C C13C C18C . . . . 23.6(3) ?
C18C C13C C14C C15C . . . . 0.2(4) ?
C12C C13C C14C C15C . . . . -179.0(2) ?
C13C C14C C15C C16C . . . . 1.8(4) ?
C14C C15C C16C C17C . . . . -2.1(4) ?
C14C C15C C16C I1C . . . . 176.51(19) ?
C15C C16C C17C C18C . . . . 0.5(4) ?
I1C C16C C17C C18C . . . . -178.12(19) ?
C16C C17C C18C C13C . . . . 1.5(4) ?
C14C C13C C18C C17C . . . . -1.8(4) ?
C12C C13C C18C C17C . . . . 177.3(2) ?
_cod_database_fobs_code 2022715