#------------------------------------------------------------------------------
#$Date: 2023-06-06 07:33:28 +0200 (Tue, 06 Jun 2023) $
#$Revision: 284381 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022746.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_2022746
loop_
_publ_author_name
'Vinaya, ?'
'Anil Kumar, Haleyur G.'
'Mohan Kumar, Thaluru M.'
'Lakshmana, Beliyaiah'
'Basavaraju, Yeriyur B.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Syntheses, crystal structures and Hirshfeld surface analyses of four
mol-ecular salts of amitriptynol.
;
_journal_coeditor_code HB8061
_journal_issue 'Pt 5'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 451
_journal_page_last 457
_journal_paper_doi 10.1107/S2056989023003225
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C20 H26 N O +, C5 H3 O2 S -, H2 O'
_chemical_formula_moiety 'C20 H26 N O +, C5 H3 O2 S -, H2 O'
_chemical_formula_sum 'C25 H31 N O4 S'
_chemical_formula_weight 441.57
_chemical_name_common
;
Amitriptynolium thiophene-2-carboxylate monohydrate
;
_chemical_name_systematic
'(3-{2-Hydroxytricyclo[9.4.0.0^3,8^]pentadeca-1(11),3,5,7,12,14-hexaen-2-yl}propyl)dimethylazanium thiophene-2-carboxylate monohydrate'
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_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 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.1659(5)
_cell_length_b 13.1299(12)
_cell_length_c 27.698(2)
_cell_measurement_reflns_used 9921
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.51
_cell_measurement_theta_min 2.70
_cell_volume 2242.4(3)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELX (Sheldrick, 2008) and 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 0.998
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0424
_diffrn_reflns_av_unetI/netI 0.0273
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 36
_diffrn_reflns_limit_l_min -36
_diffrn_reflns_number 43123
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.526
_diffrn_reflns_theta_min 2.137
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.176
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.852
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.308
_exptl_crystal_description tablet
_exptl_crystal_F_000 944
_exptl_crystal_size_max 0.270
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.188
_refine_diff_density_min -0.186
_refine_ls_abs_structure_details
;
Twinned by inversion.
;
_refine_ls_abs_structure_Flack 0.30(7)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 315
_refine_ls_number_reflns 5133
_refine_ls_number_restraints 10
_refine_ls_restrained_S_all 1.056
_refine_ls_R_factor_all 0.0331
_refine_ls_R_factor_gt 0.0284
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+0.4590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0594
_refine_ls_wR_factor_ref 0.0616
_reflns_number_gt 4772
_reflns_number_total 5133
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8061sup1.cif
_cod_data_source_block IV
_cod_depositor_comments
'Adding full bibliography for 2022743--2022746.cif.'
_cod_original_cell_volume 2242.3(3)
_cod_database_code 2022746
_cod_database_fobs_code 2022746
_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 0.954
_shelx_estimated_absorpt_t_max 0.993
_shelx_hkl_file
;
-1 0 0 1.21631 1.62150 9
1 0 0 0.55487 1.26797 3
1 0 0 -0.2126 1.21539 8
-2 0 0 3783.23 61.5070 9
-2 0 0 3785.41 61.4209 6
3 0 0 0.83710 1.96972 8
-3 0 0 -1.6667 1.69194 8
3 0 0 0.12673 1.87936 3
-3 0 0 -1.9328 1.60979 9
-3 0 0 1.19114 1.83353 7
-3 0 0 0.11792 1.77791 3
-4 0 0 6.98637 3.60247 6
-4 0 0 4.43962 3.01831 3
-4 0 0 5.62826 1.02981 2
-4 0 0 12.5452 4.17950 8
-4 0 0 9.50374 4.06186 9
4 0 0 5.19760 2.79392 3
4 0 0 11.7855 3.81591 8
-4 0 0 5.88933 3.13057 7
-5 0 0 0.78466 1.39704 2
-5 0 0 -1.7737 3.58714 9
-5 0 0 1.57456 1.58092 2
-5 0 0 4.18087 3.26179 3
-5 0 0 -2.5071 2.68318 6
-5 0 0 1.44685 3.73833 7
-5 0 0 -3.7550 3.47302 8
-6 0 0 81.2594 6.00256 2
-6 0 0 78.5479 11.1665 8
-6 0 0 74.6333 11.1267 6
-6 0 0 95.5258 11.6059 3
-6 0 0 83.4939 6.83077 2
-7 0 0 1.31049 2.64132 2
-7 0 0 -0.4685 3.45589 8
-7 0 0 -0.0865 4.75681 5
-7 0 0 -0.2230 3.29848 2
-7 0 0 1.84769 4.90905 6
-7 0 0 13.5807 4.92487 3
-8 0 0 20.1808 4.46521 2
-8 0 0 25.6276 6.59528 8
-8 0 0 23.8093 6.24950 3
1 -1 0 1874.91 29.3406 9
1 -1 0 1835.50 29.1555 6
1 1 0 1835.95 30.7053 8
-1 1 0 1856.41 28.6796 7
-1 1 0 1849.05 28.4387 6
-1 -1 0 1840.88 28.1796 2
-1 1 0 1864.31 28.3448 9
-1 -1 0 1845.98 30.6151 8
1 1 0 1811.70 26.5972 2
1 -1 0 1866.21 29.4572 7
1 1 0 1871.76 30.6953 3
-1 -1 0 1868.35 30.6712 3
-2 1 0 0.34638 1.80439 8
-2 -1 0 0.78055 1.80848 3
-2 -1 0 0.22459 1.68125 8
2 -1 0 2.44443 1.74209 9
-2 -1 0 1.54028 0.90165 2
2 1 0 0.78314 1.71176 3
-2 1 0 2.02266 2.02625 3
-2 -1 0 0.97978 0.92548 2
-2 1 0 -2.2882 1.51818 9
-2 1 0 2.50636 1.67513 6
-2 1 0 3.53159 1.80599 7
2 1 0 2.23688 1.84735 8
-3 1 0 0.71009 2.12974 3
-3 -1 0 -0.5957 1.96737 9
-3 -1 0 2.22255 1.19318 2
-3 -1 0 0.67228 2.00261 8
3 1 0 0.07147 2.38432 8
-3 1 0 1.24017 1.96323 9
-3 -1 0 3.86104 2.40112 3
-3 -1 0 4.03698 1.32078 2
3 1 0 4.85295 2.53967 3
-3 1 0 1.03318 2.00414 6
-3 1 0 2.79665 3.05998 8
-3 1 0 0.95206 2.06657 7
4 1 0 22.1884 5.46969 8
-4 1 0 33.8030 5.82051 8
4 1 0 34.9061 5.55572 3
-4 1 0 22.2584 4.86787 6
-4 -1 0 25.8292 5.66222 9
-4 1 0 27.4672 5.00375 9
-4 -1 0 31.1235 3.19927 2
-4 1 0 27.0360 4.54881 7
-4 -1 0 25.3251 5.58477 8
-4 -1 0 30.8177 5.75930 3
-4 -1 0 27.0128 2.94808 2
-4 -1 0 29.0345 6.06577 6
-4 1 0 34.6765 5.47544 3
-5 -1 0 446.958 21.0061 8
-5 1 0 487.140 21.2471 9
-5 -1 0 478.989 22.5601 6
-5 1 0 449.891 10.0173 2
-5 1 0 490.914 21.1431 6
-5 1 0 495.804 20.6831 7
-5 1 0 469.078 21.1206 3
-5 -1 0 448.542 22.5018 9
5 1 0 454.821 21.0163 8
-5 -1 0 459.132 13.5757 2
-5 -1 0 456.216 20.5269 3
-5 -1 0 469.852 21.4250 7
5 1 0 397.235 22.2924 3
-5 1 0 480.718 21.9784 8
-6 1 0 108.604 11.6490 8
-6 -1 0 89.1731 12.0735 6
-6 1 0 99.7605 6.04803 2
-6 -1 0 102.641 11.2710 3
-6 1 0 108.010 7.53887 2
-6 -1 0 101.553 7.50339 2
-6 -1 0 105.074 8.31696 2
-6 1 0 113.190 11.4901 3
-6 -1 0 104.979 12.1889 8
-6 1 0 85.5750 10.8345 6
-7 1 0 -0.9430 4.29702 3
-7 -1 0 2.06029 4.72501 3
-7 -1 0 2.33983 2.66069 2
-7 1 0 6.39265 2.64194 2
-7 1 0 5.28594 4.19240 5
-7 1 0 -9.4610 4.47203 8
-7 -1 0 4.30301 4.37288 8
-7 1 0 -8.7806 4.38902 6
-7 -1 0 4.22600 3.63810 2
0 2 0 28.1276 3.07779 2
0 -2 0 26.8674 2.94660 2
-1 2 0 75.1867 3.50626 9
-1 2 0 73.4214 3.68733 4
-1 2 0 80.4001 4.18668 7
1 2 0 81.1111 5.20683 8
1 -2 0 81.6689 4.16546 7
-1 -2 0 76.8766 5.13145 3
1 -2 0 83.1889 4.64954 4
1 2 0 82.0607 4.75565 2
1 2 0 73.1868 5.11165 3
-1 -2 0 88.1130 5.27816 2
1 -2 0 81.1049 2.33997 5
1 -2 0 83.2240 3.84356 6
-1 2 0 78.9580 3.37788 2
1 -2 0 75.3759 4.23537 9
-1 -2 0 84.5735 5.29985 8
-2 2 0 8.68652 2.20104 9
-2 2 0 12.5922 2.55664 6
2 -2 0 6.82329 2.37377 6
2 -2 0 10.8041 2.74939 7
2 -2 0 11.7949 2.70613 9
-2 2 0 11.4801 1.16434 5
2 2 0 12.9054 3.25899 8
-2 2 0 16.0788 2.94162 7
-2 -2 0 11.1085 3.06848 3
2 2 0 16.0535 3.58430 3
-2 -2 0 14.2047 3.17282 8
-2 -2 0 10.0900 2.37310 2
-3 2 0 150.718 8.37146 9
-3 2 0 168.300 8.84240 7
-3 2 0 151.058 9.36111 3
3 -2 0 174.556 9.55515 9
3 2 0 145.406 9.55294 3
-3 -2 0 158.104 6.97040 2
-3 2 0 146.711 10.1761 8
3 2 0 147.848 9.64383 8
-3 2 0 150.536 8.47585 6
-3 -2 0 146.782 9.39437 3
-3 -2 0 152.559 9.45311 8
-3 -2 0 137.502 7.00610 2
-4 2 0 -2.0019 1.98608 6
-4 -2 0 -0.4382 2.30502 8
4 2 0 -3.1931 2.72567 8
-4 -2 0 0.22049 1.62238 2
-4 -2 0 3.20349 2.91771 3
-4 2 0 0.79581 2.54328 7
-4 2 0 0.37635 3.30436 8
-4 2 0 -0.3107 2.02424 9
4 2 0 2.61886 2.58609 3
-4 2 0 3.22504 2.80825 3
-4 -2 0 2.87026 3.96198 9
-5 -2 0 89.8419 9.98272 3
5 2 0 91.5580 10.8109 3
-5 -2 0 84.5241 6.72411 2
-5 2 0 84.4791 9.30980 7
-5 2 0 78.0006 9.82939 8
-5 2 0 96.5119 9.59813 9
-5 -2 0 85.7412 10.2448 6
-5 -2 0 76.2572 10.0508 8
-5 2 0 83.6857 8.94602 6
-5 -2 0 95.2069 7.47957 2
-5 2 0 94.4261 9.90779 3
5 2 0 99.2375 10.1227 8
-6 -2 0 311.420 19.1793 8
-6 -2 0 333.434 21.5498 6
-6 2 0 342.134 18.6985 6
-6 2 0 324.464 20.0039 3
-6 -2 0 315.288 15.3865 2
-6 -2 0 319.576 19.1209 3
-6 2 0 331.550 13.3252 5
-6 2 0 316.934 10.2987 2
-6 2 0 323.783 20.8142 8
-6 2 0 332.463 12.3285 5
-7 2 0 50.9031 5.51085 5
-7 2 0 50.2500 10.3540 8
-7 -2 0 42.5055 8.68451 8
-7 2 0 52.4405 8.91357 3
-7 -2 0 50.0558 8.70813 3
-7 2 0 47.4108 5.34148 2
-7 -2 0 41.1396 7.62291 2
-7 2 0 51.0765 9.06460 6
-7 2 0 45.1763 5.12222 5
0 -3 0 -1.4716 2.14763 2
0 3 0 -0.7269 1.85519 2
-1 -3 0 441.902 13.7636 2
1 3 0 454.302 14.1126 8
-1 3 0 449.456 11.8889 2
1 3 0 478.989 13.7716 2
-1 3 0 421.290 10.5494 6
1 -3 0 449.936 10.8198 6
1 -3 0 428.348 10.5874 4
1 3 0 440.792 13.8923 3
1 -3 0 420.723 11.2751 7
1 -3 0 432.259 10.2814 9
2 -3 0 2837.68 47.8692 7
-2 -3 0 2746.99 50.9912 8
2 3 0 2845.30 44.7652 2
2 3 0 2860.05 51.6214 8
2 3 0 2891.71 45.4453 2
-2 -3 0 2746.24 51.0597 3
-2 3 0 2920.86 45.6262 6
-2 3 0 2859.57 44.8925 9
2 -3 0 2913.14 46.4772 9
2 -3 0 2859.87 46.7548 6
2 3 0 2863.59 51.3384 3
-2 3 0 2849.91 45.7546 4
-3 3 0 803.010 19.8415 9
3 -3 0 834.080 22.2443 6
-3 3 0 803.179 20.9139 7
-3 3 0 760.578 20.3832 4
-3 3 0 775.978 20.0137 6
-3 3 0 825.218 25.4177 8
3 3 0 831.828 24.4641 8
-3 -3 0 785.351 23.7139 8
3 -3 0 793.810 22.2591 7
-3 -3 0 768.375 20.7610 2
3 -3 0 800.273 21.6462 9
-3 -3 0 812.754 24.0787 3
-3 3 0 767.989 23.2376 3
3 3 0 820.215 24.0166 3
-4 3 0 510.729 17.9842 7
-4 3 0 515.360 17.9524 6
-4 3 0 503.043 21.9150 8
-4 -3 0 478.891 19.9199 8
4 3 0 479.234 20.0846 8
-4 3 0 491.425 17.2319 9
-4 3 0 490.386 10.6730 5
-4 -3 0 484.543 20.0672 3
-4 -3 0 461.396 16.6087 2
-4 3 0 496.470 20.2784 3
4 3 0 512.612 20.3591 3
-5 3 0 50.6867 6.98567 9
-5 -3 0 64.6143 8.92214 3
-5 3 0 50.7523 3.62834 5
5 3 0 46.8449 7.83150 3
-5 3 0 46.2679 7.41398 7
-5 3 0 50.9848 3.62041 5
-5 3 0 49.1069 6.76588 6
-5 -3 0 57.1828 8.22037 8
-5 3 0 49.0632 8.01850 3
-5 -3 0 42.8002 8.96943 6
-5 3 0 56.0541 8.49498 8
5 3 0 66.7313 9.78989 8
-5 -3 0 54.1198 6.47964 2
-6 -3 0 187.739 15.2326 3
-6 3 0 171.618 15.1120 3
-6 3 0 181.921 13.3628 6
-6 -3 0 173.073 12.4548 2
-6 3 0 180.406 7.78851 2
-6 3 0 173.707 6.61409 5
-6 3 0 181.946 16.5860 8
-6 3 0 162.608 12.6542 9
-6 3 0 189.409 6.41068 5
-6 -3 0 151.894 15.6570 6
-6 -3 0 192.243 14.9692 8
-7 3 0 21.8897 7.78365 3
-7 -3 0 36.6160 8.21486 8
-7 -3 0 29.7254 7.36663 3
-7 3 0 29.7028 9.16875 8
-7 3 0 38.2434 8.66629 6
-7 3 0 33.8862 4.92412 2
0 4 0 422.598 14.5285 2
1 4 0 254.418 11.3542 3
1 -4 0 253.203 8.81626 2
-1 -4 0 240.501 11.0586 2
1 -4 0 238.762 8.33761 6
1 4 0 243.101 10.8432 2
-1 4 0 236.077 9.95095 2
1 -4 0 237.445 8.00037 9
1 -4 0 244.190 8.38808 4
1 4 0 240.355 11.2823 8
2 4 0 167.071 10.0570 3
-2 -4 0 174.690 9.74275 2
2 -4 0 180.293 7.69161 9
2 4 0 182.884 8.96194 2
2 -4 0 173.389 3.88091 5
2 4 0 185.145 10.4876 8
-2 4 0 179.407 7.42585 4
2 -4 0 175.241 7.92657 6
-2 4 0 178.238 7.15745 9
-2 4 0 181.129 7.74826 2
2 -4 0 179.676 8.62525 7
-2 4 0 180.368 7.60641 6
-2 -4 0 177.401 10.4940 8
-3 4 0 705.023 15.2905 2
3 4 0 707.397 14.4493 2
-3 -4 0 739.239 23.6080 3
3 4 0 687.493 22.8543 3
3 -4 0 684.135 19.8369 6
-3 -4 0 695.806 22.9991 8
-3 4 0 675.818 18.0875 6
3 4 0 697.935 23.3678 8
-3 4 0 691.378 18.6167 4
3 -4 0 690.928 19.5718 9
3 4 0 691.139 14.1691 2
-3 4 0 684.146 19.2329 7
-3 -4 0 723.090 21.7522 2
3 -4 0 706.935 20.8423 7
-3 4 0 666.368 18.0415 9
-4 4 0 0.74061 3.04252 8
-4 4 0 3.03872 2.13514 9
4 4 0 4.78106 3.87844 8
-4 4 0 4.42314 3.49144 3
4 -4 0 8.29407 3.39722 6
-4 -4 0 2.48261 3.59861 8
-4 -4 0 2.34523 2.64474 2
-4 4 0 2.01869 1.27582 2
-4 4 0 -0.3026 1.82309 6
-4 4 0 2.38702 2.17995 7
4 -4 0 2.15873 2.57978 9
4 -4 0 4.14941 3.43112 7
-4 4 0 -1.0325 2.21423 4
-5 4 0 23.6278 5.30329 4
-5 4 0 22.6214 5.55315 7
-5 4 0 20.2003 2.86856 2
-5 -4 0 22.3251 6.23753 8
-5 4 0 12.4132 5.42618 8
-5 -4 0 14.6356 5.56927 3
-5 4 0 18.0094 6.08869 3
5 4 0 30.6295 7.37277 3
-5 4 0 26.6556 5.37864 9
-5 -4 0 25.5592 5.78243 2
5 4 0 14.6065 5.68844 8
-5 4 0 18.0709 4.93475 6
-6 4 0 60.7317 8.14669 6
-6 4 0 66.7665 10.1501 8
-6 -4 0 59.7074 9.16940 3
-6 4 0 53.8957 8.68646 4
-6 4 0 57.2335 5.22797 2
-6 4 0 45.0227 8.48450 3
-6 4 0 61.5434 7.86677 9
-6 -4 0 52.1543 12.0800 6
-6 -4 0 72.3337 9.32363 2
-6 -4 0 55.3591 9.32248 8
-7 -4 0 14.8057 6.32385 3
-7 -4 0 4.71641 4.95022 8
-7 4 0 3.48507 3.00988 2
-7 4 0 -0.9164 5.30195 8
-7 4 0 -1.5705 4.19727 6
-7 4 0 3.33302 5.10809 3
0 -5 0 0.63683 2.53096 2
0 5 0 -1.6137 2.39342 2
1 -5 0 456.965 13.4460 6
1 5 0 476.607 17.2842 2
-1 5 0 470.289 16.2627 2
-1 -5 0 474.387 17.3131 2
1 -5 0 453.936 16.0916 2
1 5 0 499.616 18.0162 8
2 -5 0 156.387 5.33569 5
2 -5 0 157.103 7.91527 4
-2 5 0 161.645 8.69941 2
2 -5 0 156.849 8.44806 7
2 5 0 147.399 10.4731 8
2 5 0 142.450 10.1796 3
-2 -5 0 147.214 10.0196 2
-2 5 0 163.804 7.72454 6
2 5 0 146.060 9.28036 2
2 -5 0 151.479 7.37312 9
2 -5 0 158.687 9.21812 6
-3 -5 0 6.04405 3.33762 2
-3 5 0 2.75108 1.77300 9
3 5 0 2.35763 2.90292 8
-3 5 0 3.75549 2.11903 2
-3 -5 0 7.00285 3.62998 8
3 5 0 3.26636 2.50352 2
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;
_shelx_hkl_checksum 10633
_shelx_res_file
;
TITL m22284 : space group P212121
m22284.res
created by SHELXL-2019/2 at 13:03:10 on 28-Mar-2023
CELL 0.71073 6.1659 13.1299 27.6977 90.000 90.000 90.000
ZERR 4 0.0005 0.0012 0.0022 0.000 0.000 0.000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H N O S
UNIT 100 124 4 16 4
TEMP -183
SIZE 0.27 0.13 0.04
REM FORM tablet
REM COLR colourless
TWIN -1 0 0 0 -1 0 0 0 -1
L.S. 10
BOND $H
ACTA
LIST 4
CONF
REM Instructions for potential hydrogen bonds
EQIV $1 x-1, y, z
HTAB O1 O1W_$1
HTAB N1 O2
EQIV $2 -x+1, y-1/2, -z+3/2
HTAB C18 S1'_$2
HTAB C18 O1W
HTAB C19 O3_$2
EQIV $3 x+1, y, z
HTAB C25' S1'_$3
HTAB O1W O3
HTAB O1W O2_$3
HTAB
REM Conformation-defining torsion angles:
RTAB tors C6 C7 C8 C9
RTAB tors C15 C16 C17 C18
RTAB tors C16 C17 C18 N1
REM
REM Anion geometry:
MPLA O2 O3 C21 C22 S1 C23 C24 C25
MPLA O2 O3 C21 C22' S1' C23' C24' C25'
MPLA C22 S1 C23 C24 C25
MPLA C22 C21 O2 O3
MPLA C22' S1' C23' C24' C25'
MPLA C22' C21 O2 O3
REM
FMAP 2
PLAN 20
REM EXTI 0.001410 : SU = 0.0009 - not significant.
WGHT 0.023400 0.459000
BASF 0.30167
FVAR 0.59727 0.89944
O1 4 0.012570 0.587777 0.639416 11.00000 0.01630 0.01876 =
0.01477 -0.00230 0.00360 -0.00306
H1O 2 0.003789 0.603087 0.668061 11.00000 0.02948
N1 3 0.445905 0.424005 0.735563 11.00000 0.02682 0.01286 =
0.01474 -0.00090 -0.00317 0.00336
H1N 2 0.414049 0.487597 0.750024 11.00000 0.02770
C1 1 0.191104 0.747880 0.617577 11.00000 0.01630 0.01446 =
0.01285 -0.00082 -0.00361 0.00218
C2 1 0.014918 0.794753 0.640744 11.00000 0.01964 0.01875 =
0.01579 -0.00154 -0.00090 0.00193
AFIX 43
H2 2 -0.091994 0.753200 0.655643 11.00000 -1.20000
AFIX 0
C3 1 -0.008094 0.899554 0.642586 11.00000 0.02501 0.02142 =
0.01805 -0.00405 -0.00366 0.00852
AFIX 43
H3 2 -0.131587 0.928973 0.657624 11.00000 -1.20000
AFIX 0
C4 1 0.149422 0.961153 0.622445 11.00000 0.03517 0.01261 =
0.01777 -0.00146 -0.00730 0.00282
AFIX 43
H4 2 0.138751 1.033189 0.624603 11.00000 -1.20000
AFIX 0
C5 1 0.322391 0.916243 0.599157 11.00000 0.02620 0.01634 =
0.01717 0.00168 -0.00562 -0.00393
AFIX 43
H5 2 0.430753 0.958886 0.585524 11.00000 -1.20000
AFIX 0
C6 1 0.345388 0.810535 0.594714 11.00000 0.01891 0.01624 =
0.01465 0.00007 -0.00549 0.00095
C7 1 0.532700 0.779123 0.562259 11.00000 0.01754 0.02043 =
0.01983 0.00368 -0.00015 -0.00297
AFIX 23
H7A 2 0.661250 0.818537 0.572726 11.00000 -1.20000
H7B 2 0.496813 0.802372 0.529210 11.00000 -1.20000
AFIX 0
C8 1 0.602761 0.668278 0.558392 11.00000 0.01633 0.02112 =
0.01689 0.00186 0.00321 0.00039
AFIX 23
H8A 2 0.723454 0.663333 0.534937 11.00000 -1.20000
H8B 2 0.658328 0.645680 0.590169 11.00000 -1.20000
AFIX 0
C9 1 0.424342 0.597538 0.542886 11.00000 0.01921 0.01635 =
0.01580 0.00181 0.00116 0.00406
C10 1 0.446828 0.545760 0.499021 11.00000 0.02648 0.02205 =
0.01499 0.00167 0.00384 0.00429
AFIX 43
H10 2 0.573560 0.556479 0.480189 11.00000 -1.20000
AFIX 0
C11 1 0.289457 0.479337 0.482311 11.00000 0.03580 0.01842 =
0.01450 -0.00304 0.00141 0.00372
AFIX 43
H11 2 0.308467 0.444647 0.452511 11.00000 -1.20000
AFIX 0
C12 1 0.104266 0.464094 0.509521 11.00000 0.02782 0.01568 =
0.01783 -0.00027 -0.00363 -0.00239
AFIX 43
H12 2 -0.005380 0.418995 0.498405 11.00000 -1.20000
AFIX 0
C13 1 0.078936 0.514926 0.553178 11.00000 0.02048 0.01424 =
0.01643 0.00179 0.00108 0.00070
AFIX 43
H13 2 -0.048939 0.504153 0.571617 11.00000 -1.20000
AFIX 0
C14 1 0.237105 0.581336 0.570467 11.00000 0.01791 0.01249 =
0.01398 0.00073 0.00068 0.00449
C15 1 0.208285 0.630350 0.620482 11.00000 0.01411 0.01477 =
0.01350 0.00016 0.00124 -0.00072
C16 1 0.392399 0.599931 0.656238 11.00000 0.01674 0.01384 =
0.01517 0.00051 0.00086 -0.00028
AFIX 23
H16A 2 0.518832 0.645177 0.651203 11.00000 -1.20000
H16B 2 0.340931 0.609543 0.689787 11.00000 -1.20000
AFIX 0
C17 1 0.462323 0.489452 0.649287 11.00000 0.02280 0.01564 =
0.01424 -0.00037 0.00171 0.00279
AFIX 23
H17A 2 0.331425 0.448170 0.642543 11.00000 -1.20000
H17B 2 0.556508 0.485789 0.620391 11.00000 -1.20000
AFIX 0
C18 1 0.582259 0.441306 0.691305 11.00000 0.01714 0.01517 =
0.02080 -0.00091 -0.00055 0.00288
AFIX 23
H18A 2 0.642223 0.375076 0.680643 11.00000 -1.20000
H18B 2 0.705992 0.485638 0.700092 11.00000 -1.20000
AFIX 0
C19 1 0.236312 0.372533 0.725151 11.00000 0.02956 0.01989 =
0.02616 -0.00048 0.00556 -0.00555
AFIX 137
H19A 2 0.143055 0.418364 0.706473 11.00000 -1.50000
H19B 2 0.164428 0.354959 0.755588 11.00000 -1.50000
H19C 2 0.263284 0.310346 0.706529 11.00000 -1.50000
AFIX 0
C20 1 0.573639 0.365125 0.771556 11.00000 0.05428 0.02873 =
0.01817 0.00252 -0.01052 0.01429
AFIX 137
H20A 2 0.489898 0.358568 0.801467 11.00000 -1.50000
H20B 2 0.709976 0.400774 0.778277 11.00000 -1.50000
H20C 2 0.605215 0.297237 0.758641 11.00000 -1.50000
AFIX 0
O2 4 0.311643 0.583136 0.787198 11.00000 0.02395 0.02336 =
0.02062 -0.00629 -0.00171 0.00403
O3 4 0.646826 0.630273 0.807972 11.00000 0.01985 0.02962 =
0.02304 0.00112 0.00579 0.00251
C21 1 0.447090 0.627593 0.814404 11.00000 0.02124 0.01309 =
0.01666 0.00343 0.00316 0.00303
SAME 0.010 C22' S1' C23' C24' C25'
EADP C22 C22'
EADP S1 C25'
EADP C23 C24'
EADP C24 C23'
EADP C25 S1'
REM SIMU 0.010 C22 > C25'
PART 1
C22 1 0.355673 0.682391 0.857176 21.00000 0.01746 0.01101 =
0.01754 0.00195 0.00225 -0.00075
S1 5 0.534025 0.728811 0.899928 21.00000 0.01957 0.01926 =
0.01912 -0.00194 -0.00141 -0.00066
C23 1 0.326102 0.784748 0.931325 21.00000 0.02413 0.01926 =
0.02129 -0.00661 0.00568 -0.00030
AFIX 43
H23 2 0.345230 0.822272 0.960340 21.00000 -1.20000
AFIX 0
C24 1 0.129862 0.769065 0.909761 21.00000 0.02017 0.01902 =
0.02516 -0.00345 0.00375 0.00058
AFIX 43
H24 2 -0.003283 0.795199 0.921778 21.00000 -1.20000
AFIX 0
C25 1 0.147698 0.709858 0.867783 21.00000 0.02844 0.01638 =
0.02465 -0.00148 0.00188 -0.00233
AFIX 43
H25 2 0.026638 0.690741 0.848600 21.00000 -1.20000
AFIX 0
PART 2
C22' 1 0.387585 0.677973 0.856738 -21.00000 0.01746 0.01101 =
0.01754 0.00195 0.00225 -0.00075
S1' 5 0.117670 0.707046 0.864158 -21.00000 0.02844 0.01638 =
0.02465 -0.00148 0.00188 -0.00233
C23' 1 0.171373 0.770490 0.916971 -21.00000 0.02017 0.01902 =
0.02516 -0.00345 0.00375 0.00058
AFIX 43
H23' 2 0.062801 0.799212 0.937142 -21.00000 -1.20000
AFIX 0
C24' 1 0.387340 0.774879 0.926596 -21.00000 0.02413 0.01926 =
0.02129 -0.00661 0.00568 -0.00030
AFIX 43
H24' 2 0.447583 0.807427 0.954137 -21.00000 -1.20000
AFIX 0
C25' 1 0.510552 0.725660 0.891046 -21.00000 0.01957 0.01926 =
0.01912 -0.00194 -0.00141 -0.00066
AFIX 43
H25' 2 0.664620 0.725448 0.890806 -21.00000 -1.20000
AFIX 0
PART 0
O1W 4 0.944052 0.622704 0.736512 11.00000 0.01967 0.05320 =
0.01821 -0.00393 0.00290 0.00239
H1W 2 0.834173 0.618973 0.755897 11.00000 0.05759
H2W 2 1.053096 0.614070 0.753327 11.00000 0.05598
HKLF 4
REM m22284 : space group P212121
REM wR2 = 0.0616, GooF = S = 1.057, Restrained GooF = 1.056 for all data
REM R1 = 0.0284 for 4772 Fo > 4sig(Fo) and 0.0331 for all 5133 data
REM 315 parameters refined using 10 restraints
END
WGHT 0.0234 0.4589
REM Instructions for potential hydrogen bonds
HTAB O1 O1W_$1
HTAB N1 O2
HTAB C18 S1'_$2
HTAB C18 O1W
HTAB C19 O3_$2
HTAB C25' S1'_$3
HTAB O1W O3
HTAB O1W O2_$3
REM Highest difference peak 0.188, deepest hole -0.186, 1-sigma level 0.034
Q1 1 0.2371 0.6046 0.5947 11.00000 0.05 0.19
Q2 1 0.3571 0.5825 0.5628 11.00000 0.05 0.17
Q3 1 0.4081 0.6553 0.8368 11.00000 0.05 0.15
Q4 1 0.1032 0.7730 0.6277 11.00000 0.05 0.14
Q5 1 0.3119 0.6199 0.6350 11.00000 0.05 0.14
Q6 1 0.1952 0.4796 0.4985 11.00000 0.05 0.14
Q7 1 0.6373 0.9198 0.9411 11.00000 0.05 0.13
Q8 1 0.5153 0.6255 0.5522 11.00000 0.05 0.13
Q9 1 0.6504 0.8021 0.9069 11.00000 0.05 0.12
Q10 1 0.4922 0.7285 0.9320 11.00000 0.05 0.12
Q11 1 0.2784 0.9371 0.6251 11.00000 0.05 0.12
Q12 1 0.2151 0.6926 0.6206 11.00000 0.05 0.12
Q13 1 0.3780 0.7975 0.9742 11.00000 0.05 0.12
Q14 1 0.2403 0.6627 0.8645 11.00000 0.05 0.12
Q15 1 0.0189 0.8446 0.6335 11.00000 0.05 0.11
Q16 1 0.4307 0.7838 0.5761 11.00000 0.05 0.11
Q17 1 0.3230 0.8603 0.5924 11.00000 0.05 0.11
Q18 1 0.2875 0.7780 0.6134 11.00000 0.05 0.11
Q19 1 0.4744 0.6394 0.6631 11.00000 0.05 0.11
Q20 1 0.5513 0.7213 0.5610 11.00000 0.05 0.11
;
_shelx_res_checksum 9730
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.0126(2) 0.58778(10) 0.63942(4) 0.0166(3) Uani d 1 . .
H H1O 0.004(4) 0.6031(17) 0.6681(8) 0.029(6) Uiso d 1 . .
N N1 0.4459(3) 0.42400(12) 0.73556(5) 0.0181(3) Uani d 1 . .
H H1N 0.414(3) 0.4876(19) 0.7500(7) 0.028(6) Uiso d 1 . .
C C1 0.1911(3) 0.74788(14) 0.61758(6) 0.0145(4) Uani d 1 . .
C C2 0.0149(3) 0.79475(14) 0.64074(6) 0.0181(4) Uani d 1 . .
H H2 -0.091994 0.753200 0.655643 0.022 Uiso calc 1 . .
C C3 -0.0081(3) 0.89955(15) 0.64259(6) 0.0215(4) Uani d 1 . .
H H3 -0.131587 0.928973 0.657624 0.026 Uiso calc 1 . .
C C4 0.1494(3) 0.96115(15) 0.62245(6) 0.0219(4) Uani d 1 . .
H H4 0.138751 1.033189 0.624603 0.026 Uiso calc 1 . .
C C5 0.3224(3) 0.91624(15) 0.59916(6) 0.0199(4) Uani d 1 . .
H H5 0.430753 0.958886 0.585524 0.024 Uiso calc 1 . .
C C6 0.3454(3) 0.81054(14) 0.59471(6) 0.0166(4) Uani d 1 . .
C C7 0.5327(3) 0.77912(15) 0.56226(6) 0.0193(4) Uani d 1 . .
H H7A 0.661250 0.818537 0.572726 0.023 Uiso calc 1 . .
H H7B 0.496813 0.802372 0.529210 0.023 Uiso calc 1 . .
C C8 0.6028(3) 0.66828(15) 0.55839(6) 0.0181(4) Uani d 1 . .
H H8A 0.723454 0.663333 0.534937 0.022 Uiso calc 1 . .
H H8B 0.658328 0.645680 0.590169 0.022 Uiso calc 1 . .
C C9 0.4243(3) 0.59754(14) 0.54289(6) 0.0171(4) Uani d 1 . .
C C10 0.4468(3) 0.54576(15) 0.49902(6) 0.0212(4) Uani d 1 . .
H H10 0.573560 0.556479 0.480189 0.025 Uiso calc 1 . .
C C11 0.2895(3) 0.47934(15) 0.48231(6) 0.0229(4) Uani d 1 . .
H H11 0.308467 0.444647 0.452511 0.027 Uiso calc 1 . .
C C12 0.1043(3) 0.46409(15) 0.50952(6) 0.0204(4) Uani d 1 . .
H H12 -0.005380 0.418995 0.498405 0.025 Uiso calc 1 . .
C C13 0.0789(3) 0.51493(14) 0.55318(6) 0.0170(4) Uani d 1 . .
H H13 -0.048939 0.504153 0.571617 0.020 Uiso calc 1 . .
C C14 0.2371(3) 0.58134(14) 0.57047(6) 0.0148(4) Uani d 1 . .
C C15 0.2083(3) 0.63035(14) 0.62048(6) 0.0141(3) Uani d 1 . .
C C16 0.3924(3) 0.59993(14) 0.65624(6) 0.0153(4) Uani d 1 . .
H H16A 0.518832 0.645177 0.651203 0.018 Uiso calc 1 . .
H H16B 0.340931 0.609543 0.689787 0.018 Uiso calc 1 . .
C C17 0.4623(3) 0.48945(14) 0.64929(6) 0.0176(4) Uani d 1 . .
H H17A 0.331425 0.448170 0.642543 0.021 Uiso calc 1 . .
H H17B 0.556508 0.485789 0.620391 0.021 Uiso calc 1 . .
C C18 0.5823(3) 0.44131(15) 0.69130(6) 0.0177(4) Uani d 1 . .
H H18A 0.642223 0.375076 0.680643 0.021 Uiso calc 1 . .
H H18B 0.705992 0.485638 0.700092 0.021 Uiso calc 1 . .
C C19 0.2363(3) 0.37253(17) 0.72515(7) 0.0252(4) Uani d 1 . .
H H19A 0.143055 0.418364 0.706473 0.038 Uiso calc 1 . .
H H19B 0.164428 0.354959 0.755588 0.038 Uiso calc 1 . .
H H19C 0.263284 0.310346 0.706529 0.038 Uiso calc 1 . .
C C20 0.5736(4) 0.36513(18) 0.77156(7) 0.0337(5) Uani d 1 . .
H H20A 0.489898 0.358568 0.801467 0.051 Uiso calc 1 . .
H H20B 0.709976 0.400774 0.778277 0.051 Uiso calc 1 . .
H H20C 0.605215 0.297237 0.758641 0.051 Uiso calc 1 . .
O O2 0.3116(2) 0.58314(11) 0.78720(5) 0.0226(3) Uani d 1 . .
O O3 0.6468(2) 0.63027(12) 0.80797(5) 0.0242(3) Uani d 1 . .
C C21 0.4471(3) 0.62759(14) 0.81440(6) 0.0170(4) Uani d 1 . .
C C22 0.3557(6) 0.6824(7) 0.8572(3) 0.0153(5) Uani d 0.899(3) A 1
S S1 0.53403(11) 0.72881(9) 0.89993(2) 0.01932(17) Uani d 0.899(3) A 1
C C23 0.3261(4) 0.7847(2) 0.93133(10) 0.0216(6) Uani d 0.899(3) A 1
H H23 0.345230 0.822272 0.960340 0.026 Uiso calc 0.899(3) A 1
C C24 0.1299(4) 0.7691(4) 0.90976(12) 0.0214(6) Uani d 0.899(3) A 1
H H24 -0.003283 0.795199 0.921778 0.026 Uiso calc 0.899(3) A 1
C C25 0.1477(15) 0.7099(11) 0.8678(4) 0.0232(11) Uani d 0.899(3) A 1
H H25 0.026638 0.690741 0.848600 0.028 Uiso calc 0.899(3) A 1
C C22' 0.388(5) 0.678(7) 0.857(2) 0.0153(5) Uani d 0.101(3) A 2
S S1' 0.118(4) 0.707(3) 0.8642(10) 0.0232(11) Uani d 0.101(3) A 2
C C23' 0.171(4) 0.770(4) 0.9170(13) 0.0214(6) Uani d 0.101(3) A 2
H H23' 0.062801 0.799212 0.937142 0.026 Uiso calc 0.101(3) A 2
C C24' 0.387(4) 0.775(3) 0.9266(10) 0.0216(6) Uani d 0.101(3) A 2
H H24' 0.447583 0.807427 0.954137 0.026 Uiso calc 0.101(3) A 2
C C25' 0.511(4) 0.726(4) 0.8910(12) 0.01932(17) Uani d 0.101(3) A 2
H H25' 0.664620 0.725448 0.890806 0.023 Uiso calc 0.101(3) A 2
O O1W 0.9441(3) 0.62270(13) 0.73651(5) 0.0304(4) Uani d 1 . .
H H1W 0.834(5) 0.619(2) 0.7559(10) 0.058(9) Uiso d 1 . .
H H2W 1.053(5) 0.614(2) 0.7533(11) 0.056(9) 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
O1 0.0163(6) 0.0188(7) 0.0148(6) -0.0031(5) 0.0036(5) -0.0023(5)
N1 0.0268(8) 0.0129(8) 0.0147(7) 0.0034(7) -0.0032(6) -0.0009(6)
C1 0.0163(8) 0.0145(10) 0.0128(7) 0.0022(7) -0.0036(6) -0.0008(6)
C2 0.0196(9) 0.0187(10) 0.0158(8) 0.0019(7) -0.0009(7) -0.0015(6)
C3 0.0250(10) 0.0214(10) 0.0180(8) 0.0085(8) -0.0037(7) -0.0040(7)
C4 0.0352(11) 0.0126(10) 0.0178(8) 0.0028(8) -0.0073(8) -0.0015(7)
C5 0.0262(9) 0.0163(10) 0.0172(8) -0.0039(8) -0.0056(8) 0.0017(7)
C6 0.0189(9) 0.0162(9) 0.0147(8) 0.0010(7) -0.0055(7) 0.0001(7)
C7 0.0175(8) 0.0204(10) 0.0198(8) -0.0030(8) -0.0001(7) 0.0037(7)
C8 0.0163(9) 0.0211(11) 0.0169(8) 0.0004(7) 0.0032(7) 0.0019(7)
C9 0.0192(9) 0.0164(10) 0.0158(8) 0.0041(7) 0.0012(7) 0.0018(7)
C10 0.0265(10) 0.0220(10) 0.0150(8) 0.0043(9) 0.0038(8) 0.0017(7)
C11 0.0358(11) 0.0184(10) 0.0145(8) 0.0037(8) 0.0014(8) -0.0030(7)
C12 0.0278(10) 0.0157(10) 0.0178(8) -0.0024(8) -0.0036(7) -0.0003(7)
C13 0.0205(9) 0.0142(9) 0.0164(8) 0.0007(7) 0.0011(7) 0.0018(7)
C14 0.0179(8) 0.0125(9) 0.0140(8) 0.0045(7) 0.0007(7) 0.0007(6)
C15 0.0141(8) 0.0148(9) 0.0135(7) -0.0007(7) 0.0012(6) 0.0002(7)
C16 0.0167(8) 0.0138(9) 0.0152(8) -0.0003(7) 0.0009(6) 0.0005(7)
C17 0.0228(9) 0.0156(9) 0.0142(7) 0.0028(8) 0.0017(7) -0.0004(7)
C18 0.0171(9) 0.0152(9) 0.0208(8) 0.0029(7) -0.0006(7) -0.0009(7)
C19 0.0296(11) 0.0199(11) 0.0262(9) -0.0055(9) 0.0056(8) -0.0005(8)
C20 0.0543(15) 0.0287(12) 0.0182(9) 0.0143(11) -0.0105(10) 0.0025(8)
O2 0.0240(7) 0.0234(8) 0.0206(6) 0.0040(6) -0.0017(5) -0.0063(6)
O3 0.0198(7) 0.0296(8) 0.0230(7) 0.0025(6) 0.0058(5) 0.0011(6)
C21 0.0212(9) 0.0131(9) 0.0167(8) 0.0030(8) 0.0032(7) 0.0034(7)
C22 0.0175(14) 0.0110(14) 0.0175(8) -0.0007(18) 0.0022(14) 0.0020(7)
S1 0.0196(3) 0.0193(3) 0.0191(4) -0.0007(3) -0.0014(2) -0.0019(3)
C23 0.0241(15) 0.0193(13) 0.0213(10) -0.0003(12) 0.0057(11) -0.0066(8)
C24 0.0202(13) 0.0190(10) 0.0252(15) 0.0006(14) 0.0037(10) -0.0035(12)
C25 0.028(3) 0.0164(12) 0.0247(19) -0.002(2) 0.0019(17) -0.0015(12)
C22' 0.0175(14) 0.0110(14) 0.0175(8) -0.0007(18) 0.0022(14) 0.0020(7)
S1' 0.028(3) 0.0164(12) 0.0247(19) -0.002(2) 0.0019(17) -0.0015(12)
C23' 0.0202(13) 0.0190(10) 0.0252(15) 0.0006(14) 0.0037(10) -0.0035(12)
C24' 0.0241(15) 0.0193(13) 0.0213(10) -0.0003(12) 0.0057(11) -0.0066(8)
C25' 0.0196(3) 0.0193(3) 0.0191(4) -0.0007(3) -0.0014(2) -0.0019(3)
O1W 0.0197(7) 0.0532(11) 0.0182(6) 0.0024(8) 0.0029(6) -0.0039(7)
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C15 O1 H1O . . 108.3(17) ?
C19 N1 C20 . . 110.74(17) ?
C19 N1 C18 . . 113.36(14) ?
C20 N1 C18 . . 109.20(15) ?
C19 N1 H1N . . 107.6(13) ?
C20 N1 H1N . . 106.5(13) ?
C18 N1 H1N . . 109.1(13) ?
C2 C1 C6 . . 118.18(17) ?
C2 C1 C15 . . 117.77(16) ?
C6 C1 C15 . . 124.00(15) ?
C3 C2 C1 . . 122.14(17) ?
C3 C2 H2 . . 118.9 ?
C1 C2 H2 . . 118.9 ?
C4 C3 C2 . . 119.67(18) ?
C4 C3 H3 . . 120.2 ?
C2 C3 H3 . . 120.2 ?
C5 C4 C3 . . 118.84(19) ?
C5 C4 H4 . . 120.6 ?
C3 C4 H4 . . 120.6 ?
C4 C5 C6 . . 122.90(18) ?
C4 C5 H5 . . 118.5 ?
C6 C5 H5 . . 118.5 ?
C5 C6 C1 . . 118.10(17) ?
C5 C6 C7 . . 113.43(16) ?
C1 C6 C7 . . 128.36(17) ?
C6 C7 C8 . . 121.10(15) ?
C6 C7 H7A . . 107.1 ?
C8 C7 H7A . . 107.1 ?
C6 C7 H7B . . 107.1 ?
C8 C7 H7B . . 107.1 ?
H7A C7 H7B . . 106.8 ?
C9 C8 C7 . . 113.79(15) ?
C9 C8 H8A . . 108.8 ?
C7 C8 H8A . . 108.8 ?
C9 C8 H8B . . 108.8 ?
C7 C8 H8B . . 108.8 ?
H8A C8 H8B . . 107.7 ?
C10 C9 C14 . . 118.78(18) ?
C10 C9 C8 . . 118.43(17) ?
C14 C9 C8 . . 122.79(15) ?
C11 C10 C9 . . 121.80(18) ?
C11 C10 H10 . . 119.1 ?
C9 C10 H10 . . 119.1 ?
C12 C11 C10 . . 119.20(17) ?
C12 C11 H11 . . 120.4 ?
C10 C11 H11 . . 120.4 ?
C11 C12 C13 . . 119.83(18) ?
C11 C12 H12 . . 120.1 ?
C13 C12 H12 . . 120.1 ?
C12 C13 C14 . . 121.39(17) ?
C12 C13 H13 . . 119.3 ?
C14 C13 H13 . . 119.3 ?
C13 C14 C9 . . 118.99(15) ?
C13 C14 C15 . . 119.39(15) ?
C9 C14 C15 . . 121.54(16) ?
O1 C15 C14 . . 105.33(14) ?
O1 C15 C1 . . 110.54(14) ?
C14 C15 C1 . . 112.21(14) ?
O1 C15 C16 . . 106.35(13) ?
C14 C15 C16 . . 112.40(14) ?
C1 C15 C16 . . 109.76(14) ?
C17 C16 C15 . . 111.67(14) ?
C17 C16 H16A . . 109.3 ?
C15 C16 H16A . . 109.3 ?
C17 C16 H16B . . 109.3 ?
C15 C16 H16B . . 109.3 ?
H16A C16 H16B . . 107.9 ?
C18 C17 C16 . . 115.93(14) ?
C18 C17 H17A . . 108.3 ?
C16 C17 H17A . . 108.3 ?
C18 C17 H17B . . 108.3 ?
C16 C17 H17B . . 108.3 ?
H17A C17 H17B . . 107.4 ?
N1 C18 C17 . . 114.57(15) ?
N1 C18 H18A . . 108.6 ?
C17 C18 H18A . . 108.6 ?
N1 C18 H18B . . 108.6 ?
C17 C18 H18B . . 108.6 ?
H18A C18 H18B . . 107.6 ?
N1 C19 H19A . . 109.5 ?
N1 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
N1 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
N1 C20 H20A . . 109.5 ?
N1 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
N1 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
O3 C21 O2 . . 125.44(17) ?
O3 C21 C22' . . 111.5(15) ?
O2 C21 C22' . . 123.0(16) ?
O3 C21 C22 . . 118.2(2) ?
O2 C21 C22 . . 116.4(2) ?
C25 C22 C21 . . 130.7(5) ?
C25 C22 S1 . . 111.0(4) ?
C21 C22 S1 . . 118.2(2) ?
C23 S1 C22 . . 91.31(12) ?
C24 C23 S1 . . 112.10(19) ?
C24 C23 H23 . . 123.9 ?
S1 C23 H23 . . 123.9 ?
C23 C24 C25 . . 112.1(4) ?
C23 C24 H24 . . 123.9 ?
C25 C24 H24 . . 123.9 ?
C22 C25 C24 . . 113.5(5) ?
C22 C25 H25 . . 123.3 ?
C24 C25 H25 . . 123.3 ?
C25' C22' C21 . . 131(3) ?
C25' C22' S1' . . 110.6(12) ?
C21 C22' S1' . . 117(2) ?
C23' S1' C22' . . 91.3(9) ?
C24' C23' S1' . . 112.1(13) ?
C24' C23' H23' . . 123.9 ?
S1' C23' H23' . . 123.9 ?
C23' C24' C25' . . 111.9(14) ?
C23' C24' H24' . . 124.0 ?
C25' C24' H24' . . 124.0 ?
C22' C25' C24' . . 113.5(15) ?
C22' C25' H25' . . 123.2 ?
C24' C25' H25' . . 123.2 ?
H1W O1W H2W . . 106(2) ?
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 C15 . 1.430(2) ?
O1 H1O . 0.82(2) ?
N1 C19 . 1.487(3) ?
N1 C20 . 1.487(2) ?
N1 C18 . 1.504(2) ?
N1 H1N . 0.95(2) ?
C1 C2 . 1.404(2) ?
C1 C6 . 1.408(3) ?
C1 C15 . 1.549(2) ?
C2 C3 . 1.384(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.382(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.379(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.401(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.521(3) ?
C7 C8 . 1.522(3) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.502(3) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.399(2) ?
C9 C14 . 1.401(2) ?
C10 C11 . 1.384(3) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.383(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.390(2) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.393(3) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.538(2) ?
C15 C16 . 1.559(2) ?
C16 C17 . 1.525(2) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 C18 . 1.517(2) ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 H19A . 0.9800 ?
C19 H19B . 0.9800 ?
C19 H19C . 0.9800 ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
O2 C21 . 1.267(2) ?
O3 C21 . 1.245(2) ?
C21 C22' . 1.40(3) ?
C21 C22 . 1.496(3) ?
C22 C25 . 1.364(9) ?
C22 S1 . 1.727(3) ?
S1 C23 . 1.714(2) ?
C23 C24 . 1.365(3) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.403(10) ?
C24 H24 . 0.9500 ?
C25 H25 . 0.9500 ?
C22' C25' . 1.367(16) ?
C22' S1' . 1.720(14) ?
S1' C23' . 1.716(13) ?
C23' C24' . 1.359(13) ?
C23' H23' . 0.9500 ?
C24' C25' . 1.402(16) ?
C24' H24' . 0.9500 ?
C25' H25' . 0.9500 ?
O1W H1W . 0.87(3) ?
O1W H2W . 0.83(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1O O1W 1_455 0.82(2) 1.95(2) 2.7607(18) 170(2) yes
N1 H1N O2 . 0.95(2) 1.74(2) 2.664(2) 164(2) yes
C18 H18A S1'b 3_646 0.99 2.93 3.90(3) 167.3 yes
C18 H18B O1W . 0.99 2.53 3.495(3) 164.3 yes
C19 H19C O3 3_646 0.98 2.46 3.388(3) 157.6 yes
C25'b H25'b S1'b 1_655 0.95 2.90 3.82(3) 164.9 yes
O1W H1W O3 . 0.87(3) 1.85(3) 2.6993(19) 165(3) yes
O1W H2W O2 1_655 0.83(3) 1.89(3) 2.716(2) 174(3) yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . -1.5(2) ?
C15 C1 C2 C3 . . . . 176.23(16) ?
C1 C2 C3 C4 . . . . -2.1(3) ?
C2 C3 C4 C5 . . . . 2.6(3) ?
C3 C4 C5 C6 . . . . 0.4(3) ?
C4 C5 C6 C1 . . . . -3.8(3) ?
C4 C5 C6 C7 . . . . 172.66(16) ?
C2 C1 C6 C5 . . . . 4.2(2) ?
C15 C1 C6 C5 . . . . -173.28(15) ?
C2 C1 C6 C7 . . . . -171.65(16) ?
C15 C1 C6 C7 . . . . 10.8(3) ?
C5 C6 C7 C8 . . . . 171.58(16) ?
C1 C6 C7 C8 . . . . -12.4(3) ?
C6 C7 C8 C9 . . . . 56.9(2) ?
C7 C8 C9 C10 . . . . 116.72(18) ?
C7 C8 C9 C14 . . . . -63.3(2) ?
C14 C9 C10 C11 . . . . 0.0(3) ?
C8 C9 C10 C11 . . . . 180.00(18) ?
C9 C10 C11 C12 . . . . 0.4(3) ?
C10 C11 C12 C13 . . . . -0.3(3) ?
C11 C12 C13 C14 . . . . -0.1(3) ?
C12 C13 C14 C9 . . . . 0.6(3) ?
C12 C13 C14 C15 . . . . -176.05(16) ?
C10 C9 C14 C13 . . . . -0.5(3) ?
C8 C9 C14 C13 . . . . 179.54(17) ?
C10 C9 C14 C15 . . . . 176.04(16) ?
C8 C9 C14 C15 . . . . -3.9(3) ?
C13 C14 C15 O1 . . . . 2.8(2) ?
C9 C14 C15 O1 . . . . -173.68(15) ?
C13 C14 C15 C1 . . . . -117.49(18) ?
C9 C14 C15 C1 . . . . 66.0(2) ?
C13 C14 C15 C16 . . . . 118.22(18) ?
C9 C14 C15 C16 . . . . -58.3(2) ?
C2 C1 C15 O1 . . . . 11.1(2) ?
C6 C1 C15 O1 . . . . -171.35(15) ?
C2 C1 C15 C14 . . . . 128.37(16) ?
C6 C1 C15 C14 . . . . -54.1(2) ?
C2 C1 C15 C16 . . . . -105.89(17) ?
C6 C1 C15 C16 . . . . 71.6(2) ?
O1 C15 C16 C17 . . . . 77.64(17) ?
C14 C15 C16 C17 . . . . -37.1(2) ?
C1 C15 C16 C17 . . . . -162.76(14) ?
C15 C16 C17 C18 . . . . -160.52(15) ?
C19 N1 C18 C17 . . . . 49.0(2) ?
C20 N1 C18 C17 . . . . 172.95(16) ?
C16 C17 C18 N1 . . . . 68.6(2) ?
O3 C21 C22 C25 . . . . 164.9(11) ?
O2 C21 C22 C25 . . . . -14.1(14) ?
O3 C21 C22 S1 . . . . -9.9(9) ?
O2 C21 C22 S1 . . . . 171.0(5) ?
C25 C22 S1 C23 . . . . -0.2(9) ?
C21 C22 S1 C23 . . . . 175.7(7) ?
C22 S1 C23 C24 . . . . -0.4(5) ?
S1 C23 C24 C25 . . . . 0.9(8) ?
C21 C22 C25 C24 . . . . -174.5(9) ?
S1 C22 C25 C24 . . . . 0.7(14) ?
C23 C24 C25 C22 . . . . -1.0(13) ?
O3 C21 C22' C25' . . . . -2(12) ?
O2 C21 C22' C25' . . . . 177(8) ?
O3 C21 C22' S1' . . . . 165(5) ?
O2 C21 C22' S1' . . . . -16(10) ?
C25' C22' S1' C23' . . . . -6(7) ?
C21 C22' S1' C23' . . . . -176(7) ?
C22' S1' C23' C24' . . . . 4(6) ?
S1' C23' C24' C25' . . . . 0(6) ?
C21 C22' C25' C24' . . . . 175(8) ?
S1' C22' C25' C24' . . . . 7(9) ?
C23' C24' C25' C22' . . . . -5(8) ?