#------------------------------------------------------------------------------
#$Date: 2023-04-15 03:51:25 +0200 (Sat, 15 Apr 2023) $
#$Revision: 282651 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022743.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_2022743
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
molecular salts of amitriptynol
;
_journal_coeditor_code HB8061
_journal_issue 5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023003225
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C20 H26 N O +, C8 H7 O3 -, H2 O'
_chemical_formula_moiety 'C20 H26 N O +, C8 H7 O3 -, H2 O'
_chemical_formula_sum 'C28 H35 N O5'
_chemical_formula_weight 465.57
_chemical_name_common
;
Amitriptynolium 4-methoxybenzoate 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 4-methoxybenzoate monohydrate'
_space_group_crystal_system monoclinic
_space_group_IT_number 7
_space_group_name_Hall 'P -2yac'
_space_group_name_H-M_alt 'P 1 n 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 94.2290(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.2398(2)
_cell_length_b 14.7216(4)
_cell_length_c 13.5383(4)
_cell_measurement_reflns_used 9880
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 74.38
_cell_measurement_theta_min 3.00
_cell_volume 1240.24(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0223
_diffrn_reflns_av_unetI/netI 0.0264
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 15326
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 74.377
_diffrn_reflns_theta_min 3.002
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.683
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.893
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.247
_exptl_crystal_description 'cut block'
_exptl_crystal_F_000 500
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.240
_exptl_crystal_size_min 0.180
_refine_diff_density_max 0.163
_refine_diff_density_min -0.138
_refine_ls_abs_structure_details
;
Flack x obtained from 1479 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.08(7)
_refine_ls_extinction_coef 0.0035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2019/2 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.023
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 327
_refine_ls_number_reflns 4078
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0249
_refine_ls_R_factor_gt 0.0241
_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^)+(0.0320P)^2^+0.2099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0632
_refine_ls_wR_factor_ref 0.0637
_reflns_number_gt 3995
_reflns_number_total 4078
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8061sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P n'
_cod_database_code 2022743
_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 0.821
_shelx_estimated_absorpt_t_max 0.887
_shelx_hkl_file
;
1 0 0 0.26198 0.17594 13
1 0 0 0.75958 0.27823 10
-1 0 0 0.17314 0.44020 1
-1 0 0 0.64838 0.11912 6
1 0 0 0.65297 0.47861 1
-2 0 0 2601.06 83.4846 1
2 0 0 2525.25 81.0001 1
3 0 0 0.00201 0.66767 13
-3 0 0 0.35699 2.13837 1
-3 0 0 0.01078 0.56372 6
-3 0 0 0.68075 0.33589 6
-3 0 0 4.13192 2.07170 1
3 0 0 1.25194 0.92386 10
4 0 0 816.947 28.0167 10
-4 0 0 812.576 26.3884 6
5 0 0 2.18432 2.40571 4
5 0 0 -0.0160 2.83738 9
5 0 0 0.27098 1.92036 10
5 0 0 0.86599 2.71001 14
-5 0 0 0.18222 0.85468 6
5 0 0 -1.2854 2.53136 16
6 0 0 406.127 15.7462 14
6 0 0 396.618 15.4768 16
6 0 0 398.777 15.7104 9
6 0 0 410.060 15.3811 4
7 0 0 0.53946 1.64174 14
7 0 0 1.75943 1.36124 4
0 -1 0 25.3737 1.05597 1
0 -1 0 21.9157 0.80133 6
0 1 0 19.9484 0.78915 6
0 1 0 21.0451 1.06282 1
-1 -1 0 1293.68 41.0769 1
-1 -1 0 1233.35 40.7215 6
1 1 0 1332.12 42.9875 1
-1 1 0 1251.86 40.7723 1
-1 1 0 1308.68 40.7191 1
-2 -1 0 499.836 16.4223 6
2 -1 0 502.050 16.5187 13
2 -1 0 510.124 16.8639 10
-2 -1 0 507.929 17.0916 1
-2 1 0 518.310 16.3099 1
-2 1 0 510.496 16.3228 1
2 1 0 497.692 16.9119 1
2 1 0 498.578 16.8622 10
-2 1 0 494.418 16.2647 6
-3 -1 0 950.778 31.0878 6
-3 -1 0 951.580 32.3108 1
-3 -1 0 976.823 30.9720 6
3 -1 0 951.523 31.4698 13
3 -1 0 969.456 32.0152 10
3 1 0 964.518 32.0237 10
-3 1 0 964.838 30.8089 6
4 -1 0 182.372 7.77776 10
-4 -1 0 182.943 6.40276 6
-4 1 0 181.776 6.20292 6
4 1 0 187.452 7.81512 10
5 -1 0 125.814 6.97631 16
5 -1 0 125.184 6.54546 10
5 -1 0 123.139 7.09043 14
-5 -1 0 124.145 4.75079 6
5 -1 0 125.404 7.27268 9
5 -1 0 118.543 6.74528 4
5 1 0 123.204 7.31803 14
5 1 0 131.483 6.82282 4
5 1 0 125.081 7.18685 9
5 1 0 121.789 6.62608 10
5 1 0 117.845 6.93924 16
-5 1 0 125.937 4.51938 6
6 -1 0 173.594 8.10554 16
6 -1 0 164.046 7.88076 4
6 -1 0 162.836 8.17788 14
6 -1 0 163.531 8.25019 9
6 1 0 165.427 8.28986 9
6 1 0 164.111 8.34240 14
6 1 0 160.942 8.03331 16
6 1 0 167.401 7.76450 4
7 -1 0 31.4232 3.31788 14
7 -1 0 36.2154 2.75039 4
7 -1 0 37.1891 3.55719 9
7 1 0 31.6623 2.60035 14
7 1 0 31.7414 2.36593 4
7 1 0 28.0828 3.32386 9
0 -2 0 489.134 15.8460 6
0 -2 0 492.140 16.2225 1
0 2 0 481.859 15.8385 6
0 2 0 501.808 16.2551 1
1 -2 0 1819.75 58.0595 1
-1 -2 0 1837.06 59.1784 1
1 2 0 1798.73 58.4642 1
-1 2 0 1825.30 58.7692 1
-2 -2 0 340.391 12.3619 1
2 -2 0 335.066 11.5459 13
-2 -2 0 342.089 11.1021 6
2 -2 0 347.233 11.5511 10
2 2 0 344.146 12.2424 1
2 2 0 343.476 11.8474 10
-2 2 0 338.384 11.0808 6
-3 -2 0 173.789 6.01781 6
3 -2 0 170.769 6.38214 13
-3 -2 0 176.887 9.14319 1
3 -2 0 175.864 6.84320 10
3 2 0 176.851 6.91499 10
3 2 0 175.281 8.70388 1
-3 2 0 169.292 5.68970 6
-4 -2 0 144.244 5.17904 6
4 -2 0 135.471 5.56639 13
4 -2 0 134.017 6.09949 10
-4 2 0 135.523 4.96167 6
4 2 0 132.860 6.19718 10
-4 2 0 140.252 4.77442 6
5 -2 0 113.544 6.38775 10
5 -2 0 116.006 6.44664 4
5 -2 0 114.065 6.67400 16
5 -2 0 117.831 6.98644 9
-5 -2 0 114.493 4.57303 6
5 -2 0 112.124 6.90232 14
5 2 0 121.482 7.01438 9
5 2 0 107.498 6.91038 2
5 2 0 113.764 6.37051 4
5 2 0 113.820 7.05101 14
-5 2 0 112.896 3.89229 6
5 2 0 120.088 6.63203 16
5 2 0 112.446 6.34938 10
6 -2 0 170.696 8.22317 9
6 -2 0 172.672 8.21624 14
6 -2 0 170.637 7.98971 4
6 -2 0 176.737 8.38171 16
6 2 0 165.503 8.33447 9
6 2 0 178.358 8.62118 14
6 2 0 171.078 8.15961 16
6 2 0 168.707 7.89455 4
7 -2 0 62.7740 3.84008 9
7 2 0 63.6582 3.96435 14
0 -3 0 754.349 24.7607 6
0 -3 0 774.455 25.3901 1
0 3 0 759.752 24.7626 6
0 3 0 784.298 25.3687 1
1 -3 0 2460.91 79.7152 1
-1 -3 0 2460.17 79.1246 1
1 3 0 2497.51 80.1113 1
-1 3 0 2402.78 78.3705 6
-1 3 0 2484.08 78.7653 1
-2 -3 0 1086.82 34.6994 6
2 -3 0 1097.72 35.4154 13
2 -3 0 1117.31 35.6568 10
-2 -3 0 1085.64 36.0511 1
-2 3 0 1064.98 35.1202 6
2 3 0 1085.28 37.1166 1
2 3 0 1088.13 35.8064 10
-2 3 0 1087.17 34.4981 6
3 -3 0 172.534 6.84397 10
3 -3 0 181.191 6.51191 13
-3 -3 0 175.778 6.24506 6
-3 -3 0 170.464 10.9284 1
3 3 0 176.810 6.96610 10
-3 3 0 178.421 5.81900 6
3 3 0 165.526 10.3040 1
4 -3 0 197.666 8.21632 10
4 -3 0 193.865 8.20248 13
-4 -3 0 205.487 7.25617 6
4 3 0 202.860 8.38108 10
-4 3 0 196.620 6.65649 6
5 -3 0 118.890 6.96420 9
5 -3 0 111.376 6.50183 4
5 -3 0 116.498 6.75708 16
-5 -3 0 117.174 4.86917 6
5 -3 0 110.993 7.13795 14
5 -3 0 109.515 6.93237 7
5 -3 0 116.533 6.35954 10
5 3 0 117.196 6.56120 16
5 3 0 116.405 6.44606 10
5 3 0 120.022 6.92978 9
5 3 0 121.426 6.41515 2
5 3 0 100.598 4.98238 5
5 3 0 119.054 6.39253 4
5 3 0 117.871 7.11081 14
6 -3 0 39.2819 4.62316 9
6 -3 0 34.6607 3.77730 4
6 -3 0 33.9807 4.14402 16
6 3 0 30.1931 4.19941 14
6 3 0 31.8002 3.01125 4
6 3 0 30.7168 3.79977 16
6 3 0 33.0291 4.14518 9
7 -3 0 76.1806 4.20360 16
7 -3 0 73.0190 3.96166 9
7 -3 0 72.7159 3.69168 4
7 3 0 75.3138 3.87091 4
7 3 0 77.4894 3.89423 16
7 3 0 73.8010 4.25161 14
0 -4 0 6105.22 193.402 1
0 4 0 5950.28 193.398 1
1 -4 0 2360.44 74.4292 1
-1 -4 0 2312.80 73.5876 1
1 4 0 2277.27 74.5107 10
-1 4 0 2218.56 72.7671 6
1 4 0 2291.84 74.4553 6
1 4 0 2337.60 75.4622 1
2 -4 0 745.558 24.1997 1
2 -4 0 745.368 24.4930 10
-2 -4 0 744.519 23.7697 6
-2 -4 0 741.526 25.9762 1
-2 4 0 734.720 24.1077 1
-2 4 0 710.060 23.8198 6
2 4 0 743.663 26.0564 1
-2 4 0 744.629 23.7873 6
2 4 0 745.609 24.9066 10
3 -4 0 2203.46 71.0959 10
-3 -4 0 2157.64 69.1058 6
3 -4 0 2143.73 70.7331 13
-3 4 0 2138.18 68.9213 6
3 4 0 2204.16 70.9377 10
4 -4 0 70.8299 3.86724 13
-4 -4 0 72.7578 3.26856 6
4 -4 0 69.1541 4.09231 10
-4 4 0 72.9712 2.61211 6
4 4 0 74.8636 4.30043 10
5 -4 0 311.600 13.0588 16
5 -4 0 315.459 12.8366 4
-5 -4 0 321.596 11.4721 6
5 -4 0 320.444 12.6673 15
5 -4 0 318.667 12.6713 7
5 -4 0 321.432 13.2895 9
5 -4 0 290.290 14.2578 14
5 4 0 315.145 11.5428 5
5 4 0 331.691 13.2104 9
5 4 0 314.273 12.8348 16
5 4 0 325.171 12.4999 4
5 4 0 324.320 12.8920 10
6 -4 0 76.6949 5.29893 4
6 -4 0 78.7889 5.76168 16
6 -4 0 63.7164 4.64594 7
6 4 0 78.6640 5.67517 9
6 4 0 59.2822 5.59039 14
6 4 0 78.8406 5.04324 16
6 4 0 68.8318 5.19732 2
7 -4 0 6.23373 1.32932 16
7 -4 0 8.11446 1.47991 4
7 4 0 6.60920 1.43641 16
7 4 0 7.13751 1.12275 4
7 4 0 8.43576 1.37852 9
7 4 0 6.78182 1.33329 14
0 -5 0 1321.89 42.9001 1
0 -5 0 1265.49 41.7627 6
0 5 0 1307.04 41.8028 6
0 5 0 1316.13 42.9298 1
0 5 0 1269.01 41.5294 10
-1 -5 0 1921.27 63.0415 1
1 -5 0 1927.89 61.8028 1
-1 -5 0 1905.67 61.7117 6
1 5 0 1893.07 61.8152 10
1 5 0 1918.73 62.9970 1
-1 5 0 1920.41 62.2818 1
1 5 0 1916.51 61.7978 6
-2 -5 0 560.341 21.2688 1
-2 -5 0 576.480 18.7090 6
2 -5 0 559.034 18.6749 13
-2 5 0 547.175 18.4759 6
2 5 0 563.194 18.8483 10
-2 5 0 576.291 19.5725 1
-2 5 0 563.454 18.3817 6
-3 -5 0 196.665 7.14135 6
3 -5 0 175.118 6.64114 13
3 -5 0 171.388 6.75679 10
-3 5 0 171.160 6.16400 6
3 5 0 169.297 6.92033 10
4 -5 0 46.7604 3.43034 13
-4 -5 0 49.9783 2.63450 6
4 5 0 48.1882 3.63333 10
-4 5 0 44.7579 1.88347 6
5 -5 0 106.166 6.67336 9
5 -5 0 131.770 7.06044 4
5 -5 0 116.043 7.10810 15
5 -5 0 129.686 7.11434 7
-5 -5 0 116.736 5.35167 6
5 -5 0 92.3739 7.39314 11
5 5 0 116.084 5.45989 5
5 5 0 132.083 6.94816 4
6 -5 0 277.459 11.0393 4
6 -5 0 277.386 10.9753 9
6 -5 0 296.549 11.6236 16
6 -5 0 283.020 10.8560 7
6 5 0 287.426 11.6492 9
6 5 0 281.159 12.0211 14
6 5 0 289.468 10.9578 4
6 5 0 285.595 10.6517 2
6 5 0 250.647 11.8760 16
7 -5 0 149.661 5.91479 4
7 -5 0 149.583 6.16467 16
7 5 0 139.447 6.20324 14
7 5 0 156.684 6.12002 16
7 5 0 149.648 5.82169 4
7 5 0 141.922 6.10749 9
0 -6 0 202.122 7.18400 6
0 -6 0 207.414 10.3637 1
0 6 0 213.589 7.16619 6
0 6 0 203.136 9.64717 1
0 6 0 204.638 6.73118 10
1 -6 0 413.897 15.2070 1
-1 -6 0 411.080 13.7760 6
1 -6 0 409.346 13.7884 13
-1 -6 0 411.991 16.4917 1
1 6 0 410.897 16.4442 1
-1 6 0 398.047 15.7140 1
1 6 0 409.379 13.7728 6
1 6 0 407.556 13.6044 10
-1 6 0 419.358 13.6304 6
-2 -6 0 1103.34 38.6423 1
-2 -6 0 1073.07 35.4016 6
2 -6 0 1077.61 35.0518 13
2 6 0 1079.69 35.3074 10
-2 6 0 1082.95 35.2120 6
2 6 0 1043.55 37.7107 1
-3 -6 0 13.8335 1.47391 6
3 6 0 12.6829 1.83505 10
-3 6 0 11.6074 1.01882 6
-4 -6 0 75.8401 3.65048 6
4 -6 0 75.2873 6.06180 15
-4 -6 0 74.6809 6.15285 12
4 -6 0 73.5841 4.82625 13
4 -6 0 77.0064 5.83124 16
4 -6 0 72.3963 5.57144 4
-4 6 0 72.1685 2.82604 6
4 6 0 73.9749 4.65539 10
4 6 0 73.4579 5.09427 4
5 -6 0 123.036 6.72281 15
5 -6 0 118.380 8.06913 11
5 -6 0 131.933 6.42341 7
5 -6 0 127.387 7.13217 16
5 -6 0 108.570 7.92774 9
5 -6 0 129.175 6.85833 4
5 6 0 127.905 5.92025 5
5 6 0 102.514 8.21755 10
5 6 0 132.335 6.79272 16
5 6 0 124.966 6.37962 4
5 6 0 131.430 7.16850 9
6 -6 0 246.821 9.57782 7
6 -6 0 242.754 9.78929 4
6 -6 0 245.163 10.1618 16
6 -6 0 231.466 9.95902 15
6 6 0 232.126 9.32543 2
6 6 0 239.759 9.44999 4
6 6 0 253.231 10.7446 14
6 6 0 255.713 10.2885 9
6 6 0 236.899 9.63229 16
7 -6 0 116.163 4.81315 4
7 6 0 120.242 5.36052 14
7 6 0 119.831 5.06061 9
7 6 0 125.151 4.95323 16
7 6 0 118.326 4.74010 4
0 -7 0 1891.10 63.2735 6
0 -7 0 1981.74 64.5439 1
0 7 0 1981.59 62.6816 6
0 7 0 1943.49 64.8580 1
1 -7 0 601.242 22.2579 1
-1 -7 0 612.784 20.3223 6
1 -7 0 608.838 20.3102 13
-1 -7 0 612.318 23.9050 1
-1 7 0 633.764 20.2315 6
1 7 0 611.746 23.7718 1
-1 7 0 587.818 23.1299 1
1 7 0 614.657 20.2387 6
-2 -7 0 2131.70 69.4681 6
-2 -7 0 2150.48 72.3983 1
2 -7 0 2118.18 68.6238 13
-2 7 0 2143.45 69.4619 6
3 -7 0 101.360 4.73235 13
-3 -7 0 92.6904 4.21882 6
3 7 0 96.5320 4.90254 10
-3 7 0 95.7546 3.66095 6
4 -7 0 255.455 10.7458 11
4 -7 0 256.096 10.8759 16
4 -7 0 255.546 10.5581 7
4 -7 0 251.125 10.6645 15
4 -7 0 255.655 10.1889 13
-4 -7 0 260.781 9.70079 6
4 7 0 290.827 10.9936 3
-4 7 0 258.681 8.79066 6
4 7 0 258.213 10.5916 16
4 7 0 245.083 10.3692 5
4 7 0 215.263 10.8914 4
5 -7 0 156.250 8.09920 11
5 -7 0 158.572 8.11026 16
5 -7 0 158.074 7.69381 4
5 -7 0 160.047 7.42353 7
5 -7 0 154.602 7.65037 15
5 7 0 170.194 7.64305 16
5 7 0 142.925 10.3171 9
5 7 0 158.593 7.61854 4
5 7 0 165.856 7.15898 5
6 -7 0 119.942 6.02664 16
6 -7 0 114.128 5.62620 4
6 -7 0 103.901 5.94175 15
6 -7 0 113.340 5.50439 7
6 7 0 111.611 5.19594 4
6 7 0 118.402 6.34929 14
6 7 0 117.188 5.56119 16
6 7 0 111.513 5.91448 9
7 -7 0 8.38174 1.27653 16
7 7 0 5.74649 1.26879 14
7 7 0 11.9005 1.69271 9
0 -8 0 542.798 23.8560 1
0 8 0 568.002 18.2524 6
0 8 0 518.650 22.8269 1
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1 2 15 101.338 5.68382 5
-1 2 -15 97.1560 4.79736 8
-1 2 -15 96.3041 5.03092 5
-2 -2 -15 27.3266 3.76558 5
2 -2 15 23.2392 2.18329 5
-2 2 -15 20.6285 2.37709 12
-2 2 -15 20.1518 2.14418 8
2 2 15 26.9260 2.85446 5
3 -3 -15 220.913 8.32692 7
3 -3 -15 230.458 8.67909 15
3 3 -15 239.663 8.72863 15
3 3 -15 226.263 8.42740 11
2 -3 -15 54.0895 2.78971 5
2 -3 -15 53.5378 3.45707 15
2 3 -15 52.7076 5.05650 8
2 3 -15 53.1297 2.91893 5
1 -3 -15 41.2974 3.30940 15
1 -3 -15 39.4786 2.65767 5
1 3 -15 38.4749 2.99514 8
0 -3 15 5.54320 2.72006 5
0 3 -15 7.12462 1.86713 8
0 3 -15 5.31514 1.52084 5
1 -3 15 148.889 6.31767 5
-1 -3 -15 149.658 6.51493 5
-1 3 -15 127.734 6.26323 5
1 3 15 108.821 6.03578 12
1 3 15 127.281 6.04797 5
-2 -3 -15 77.5705 4.76322 5
2 -3 15 84.3226 4.21118 5
3 -4 -15 116.754 4.60413 7
3 4 -15 113.033 4.07571 5
2 -4 -15 79.5322 4.12440 15
2 -4 -15 76.9085 3.97926 7
2 -4 -15 77.0804 3.37846 5
2 4 -15 84.9298 3.97661 5
1 -4 -15 77.3150 4.23677 15
1 -4 -15 75.8843 4.46397 5
1 4 -15 85.9957 4.42856 5
1 4 -15 83.9180 4.53516 8
0 -4 -15 115.596 5.41875 5
0 -4 15 103.231 5.95702 5
0 4 -15 107.501 5.62246 5
-1 -4 -15 2.30212 1.25210 5
1 -4 15 0.16949 1.78713 5
-1 4 -15 0.53368 1.58529 8
1 4 15 3.69765 1.83173 5
1 4 15 -0.2840 1.66178 12
-2 -4 -15 12.4528 2.19818 5
-2 4 -15 10.6994 1.77829 8
2 4 15 9.05961 1.51765 5
3 -5 -15 3.54050 1.11702 15
3 -5 -15 2.60485 1.38940 7
3 5 -15 4.67905 1.39008 15
2 -5 -15 51.1540 3.09565 7
2 5 -15 50.9390 2.73022 5
1 -5 -15 4.73775 1.24253 5
-1 -5 15 0.15351 2.42190 5
1 5 -15 3.99911 1.16089 5
1 5 -15 5.71960 1.76730 8
0 -5 -15 312.395 11.2923 5
0 -5 15 314.054 11.7808 5
0 5 15 312.757 11.3261 12
0 5 -15 311.108 11.5262 8
0 5 -15 298.275 11.4033 5
-1 -5 -15 282.095 10.7670 5
1 -5 15 282.992 10.7775 5
1 5 15 285.683 11.0360 5
-1 5 -15 289.336 10.8839 5
-1 5 -15 290.910 10.6800 8
-2 -5 -15 37.9389 3.06508 5
2 -5 15 36.9689 2.26399 5
2 5 15 43.1398 3.04888 5
2 -6 -15 55.3283 3.00304 7
2 -6 -15 56.5177 3.03465 15
-2 6 15 54.4374 3.04396 12
2 6 -15 49.9539 2.67322 5
1 -6 -15 23.9979 1.90614 5
-1 6 15 24.5731 2.36106 12
1 6 -15 23.8349 2.50937 5
0 -6 15 141.933 6.19337 5
0 -6 -15 141.247 5.84537 5
0 6 15 146.023 5.82050 12
0 6 -15 144.735 6.89626 5
0 6 -15 147.948 6.08421 8
-1 -6 -15 28.6911 3.04071 5
-2 -6 -15 33.1394 2.63418 5
2 -6 15 36.9078 2.19585 5
2 -7 -15 42.8121 2.46238 7
-2 7 15 42.8823 2.61266 12
2 7 -15 43.0902 2.36984 5
1 -7 -15 198.547 7.41746 7
1 -7 -15 193.405 7.10072 5
-1 7 15 198.109 7.50183 12
0 -7 15 40.8457 2.77065 5
0 -7 -15 42.8210 2.52131 5
0 7 -15 40.7446 2.76167 5
1 -7 15 13.6902 2.00067 5
-1 -7 -15 12.8273 1.92483 5
-1 7 -15 10.8345 1.96497 8
1 -8 -15 12.5560 1.66854 7
-1 8 15 8.43772 1.57518 12
1 8 -15 10.3873 1.85843 5
0 -8 15 5.17290 1.34113 5
0 -8 -15 3.08064 0.90343 5
0 -8 -15 3.92918 1.10065 7
0 8 -15 6.71854 1.88037 5
0 8 15 3.26400 1.17837 12
3 0 -16 -0.8260 0.94775 15
2 0 -16 60.6237 3.21881 15
1 0 -16 1.98503 1.35520 15
1 0 -16 0.16657 0.83589 5
0 0 -16 7.66926 1.77306 15
0 0 16 7.81805 3.51006 5
0 0 -16 6.09207 1.63613 5
0 0 -16 4.95498 1.28893 8
-1 0 -16 0.70105 1.17015 5
-1 0 -16 2.91109 1.95999 8
1 0 16 1.40047 1.81743 5
3 -1 -16 6.71057 1.14232 15
3 1 -16 7.43357 1.15605 15
2 -1 -16 58.3525 2.57823 5
2 1 -16 59.2897 3.19612 15
1 -1 -16 41.3632 2.64840 5
1 1 -16 43.1590 2.77756 5
1 1 -16 35.8511 2.66550 8
0 -1 -16 13.4321 1.79805 5
0 -1 -16 14.8308 1.91564 8
0 1 -16 18.1190 2.43242 5
0 1 16 16.2893 2.00249 12
0 1 -16 14.4994 1.95943 8
1 -1 16 58.6686 3.67650 5
-1 -1 -16 53.2176 3.11524 5
1 1 16 55.0905 3.84745 5
-1 1 -16 51.9410 3.47234 5
2 -2 -16 115.914 4.73277 7
2 -2 -16 116.863 4.79547 15
2 2 -16 113.940 5.41722 15
1 -2 -16 20.8950 2.18228 15
1 -2 -16 15.9618 1.58624 5
1 2 -16 17.6702 2.63425 8
1 2 -16 18.7143 2.11774 5
0 -2 16 29.1701 3.90445 5
0 -2 -16 24.0211 2.48697 5
0 2 -16 25.2027 2.73096 8
0 2 16 23.7848 2.55672 12
0 2 -16 21.7981 2.15420 5
-1 -2 -16 9.65957 1.71473 5
1 -2 16 12.0364 1.91628 5
-1 2 -16 14.5948 2.16869 8
-1 2 -16 9.80851 1.86786 5
2 -3 -16 16.0801 1.78281 15
2 -3 -16 16.5774 1.80903 7
2 3 -16 14.0103 1.68531 5
1 -3 -16 26.2029 2.03703 5
1 3 -16 29.5520 2.41118 5
1 3 -16 30.9742 2.91314 8
0 -3 -16 101.168 4.48957 5
0 3 -16 104.053 4.91034 8
0 3 16 102.115 4.31749 12
-1 -3 -16 132.289 5.51796 5
1 -3 16 137.595 5.65389 5
-1 3 -16 139.489 6.35402 8
2 -4 -16 9.57531 1.46683 7
2 4 -16 12.1734 1.27780 5
1 -4 -16 30.8548 2.75800 5
0 4 -16 73.1224 3.88479 8
0 4 -16 69.7118 3.55250 5
0 4 16 70.7080 3.43368 12
1 -4 16 152.651 5.98216 5
-1 -4 -16 168.171 6.52870 5
1 -5 -16 131.766 4.99745 7
1 -5 -16 127.596 4.50935 5
1 5 -16 124.630 5.18587 5
-1 5 16 129.445 5.06141 12
0 -5 -16 97.5617 4.08109 5
0 5 -16 100.135 4.54310 5
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 71919
_shelx_res_file
;
TITL c22013 : space group Pn
c22013.res
created by SHELXL-2019/2 at 12:05:23 on 28-Mar-2023
CELL 1.54178 6.2398 14.7216 13.5383 90.000 94.229 90.000
ZERR 2 0.0002 0.0004 0.0004 0.000 0.001 0.000
LATT -1
SYMM 1/2+X, -Y, 1/2+Z
SFAC C H N O
UNIT 56 70 2 10
TEMP -183
SIZE 0.30 0.24 0.18
REM FORM cut block
REM COLR colourless
L.S. 10
BOND $H
LIST 4
ACTA
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, z
HTAB C18 O1_$2
HTAB C18 O1W
EQIV $3 x-1/2, -y+1, z+1/2
HTAB C19 O3_$3
HTAB C20 O1W
HTAB O1W O3
HTAB O1W O2_$2
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 C23 C24 C25 C26 C27 O4 C28
RTAB tors C24 C25 O4 C28
REM
REM Anti-bumping restraint here has little effect as these two H atoms really
REM do seem to be close together, about 1.8\%A
DFIX -2.000 0.020 H16A H7A
FMAP 2
PLAN 5
WGHT 0.032000 0.209900
EXTI 0.003508
FVAR 1.10259
O1 4 0.055519 0.724395 0.571070 11.00000 0.01842 0.01682 =
0.02748 -0.00236 0.00552 -0.00322
H1O 2 0.052878 0.667203 0.560717 11.00000 0.03864
N1 3 0.593624 0.549094 0.726624 11.00000 0.01902 0.01554 =
0.01603 0.00036 -0.00022 -0.00288
H1N 2 0.536964 0.523924 0.666558 11.00000 0.02119
C1 1 0.257069 0.859820 0.571917 11.00000 0.01802 0.01805 =
0.01405 0.00137 -0.00237 0.00070
C2 1 0.097112 0.892569 0.628516 11.00000 0.02209 0.01996 =
0.01624 0.00158 0.00050 -0.00063
AFIX 43
H2 2 -0.017827 0.853518 0.642767 11.00000 -1.20000
AFIX 0
C3 1 0.100481 0.980708 0.664824 11.00000 0.02896 0.02264 =
0.01589 -0.00155 0.00269 0.00285
AFIX 43
H3 2 -0.012447 1.001724 0.702307 11.00000 -1.20000
AFIX 0
C4 1 0.269467 1.038153 0.646213 11.00000 0.03675 0.01640 =
0.01823 -0.00304 -0.00154 -0.00042
AFIX 43
H4 2 0.273384 1.098709 0.670526 11.00000 -1.20000
AFIX 0
C5 1 0.431580 1.005680 0.591765 11.00000 0.02745 0.02063 =
0.02067 0.00052 -0.00147 -0.00535
AFIX 43
H5 2 0.548457 1.044559 0.579907 11.00000 -1.20000
AFIX 0
C6 1 0.429441 0.917544 0.553532 11.00000 0.02066 0.01965 =
0.01840 0.00102 -0.00109 -0.00209
C7 1 0.609516 0.886494 0.494234 11.00000 0.02014 0.02113 =
0.02460 0.00363 0.00041 -0.00429
AFIX 23
H7A 2 0.670947 0.829778 0.523644 11.00000 -1.20000
H7B 2 0.724160 0.933119 0.498402 11.00000 -1.20000
AFIX 0
C8 1 0.539027 0.869467 0.385625 11.00000 0.02561 0.02735 =
0.02018 0.00277 0.00629 -0.00106
AFIX 23
H8A 2 0.511844 0.929638 0.354531 11.00000 -1.20000
H8B 2 0.663866 0.843058 0.354795 11.00000 -1.20000
AFIX 0
C9 1 0.346065 0.810080 0.355036 11.00000 0.02736 0.01745 =
0.01705 -0.00024 0.00057 0.00543
C10 1 0.301544 0.805174 0.252056 11.00000 0.04307 0.02091 =
0.01935 0.00155 0.00076 0.00323
AFIX 43
H10 2 0.399634 0.832237 0.210388 11.00000 -1.20000
AFIX 0
C11 1 0.121077 0.762641 0.208795 11.00000 0.05503 0.02017 =
0.01819 -0.00260 -0.01073 0.00590
AFIX 43
H11 2 0.095222 0.761135 0.138778 11.00000 -1.20000
AFIX 0
C12 1 -0.020662 0.722504 0.268461 11.00000 0.03510 0.02073 =
0.03120 -0.00658 -0.01483 0.00342
AFIX 43
H12 2 -0.147085 0.693966 0.239991 11.00000 -1.20000
AFIX 0
C13 1 0.022003 0.723897 0.370742 11.00000 0.02410 0.01877 =
0.02740 -0.00379 -0.00633 0.00259
AFIX 43
H13 2 -0.076086 0.695359 0.411320 11.00000 -1.20000
AFIX 0
C14 1 0.206057 0.766299 0.415904 11.00000 0.02073 0.01388 =
0.01904 -0.00151 -0.00295 0.00450
C15 1 0.239400 0.762628 0.530066 11.00000 0.01608 0.01648 =
0.01858 -0.00004 0.00158 -0.00177
C16 1 0.432543 0.700397 0.563095 11.00000 0.01832 0.01589 =
0.01533 0.00095 0.00092 -0.00103
AFIX 23
H16B 2 0.391728 0.636220 0.550513 11.00000 -1.20000
H16A 2 0.554670 0.714706 0.523040 11.00000 -1.20000
AFIX 0
C17 1 0.503492 0.712353 0.673108 11.00000 0.02649 0.01704 =
0.01500 0.00083 -0.00001 -0.00109
AFIX 23
H17A 2 0.561491 0.774523 0.683229 11.00000 -1.20000
H17B 2 0.375332 0.707074 0.711697 11.00000 -1.20000
AFIX 0
C18 1 0.671272 0.645098 0.714302 11.00000 0.02257 0.01644 =
0.01929 0.00148 -0.00367 -0.00473
AFIX 23
H18A 2 0.790325 0.644083 0.669854 11.00000 -1.20000
H18B 2 0.730746 0.667431 0.779651 11.00000 -1.20000
AFIX 0
C19 1 0.413610 0.543631 0.791941 11.00000 0.03253 0.02300 =
0.02836 0.00037 0.01348 -0.00397
AFIX 137
H19A 2 0.376582 0.479798 0.802175 11.00000 -1.50000
H19B 2 0.288444 0.575669 0.760923 11.00000 -1.50000
H19C 2 0.456773 0.571815 0.855914 11.00000 -1.50000
AFIX 0
C20 1 0.776853 0.491303 0.766082 11.00000 0.02840 0.01957 =
0.02839 0.00285 -0.00628 0.00000
AFIX 137
H20A 2 0.728457 0.428261 0.771203 11.00000 -1.50000
H20B 2 0.829547 0.513304 0.831755 11.00000 -1.50000
H20C 2 0.892900 0.494386 0.721206 11.00000 -1.50000
AFIX 0
O2 4 0.403445 0.451943 0.578296 11.00000 0.02462 0.02008 =
0.02469 -0.00664 -0.00316 0.00062
O3 4 0.698371 0.435184 0.497336 11.00000 0.03310 0.04859 =
0.04806 -0.02376 0.01552 -0.02438
O4 4 0.234924 0.075436 0.350223 11.00000 0.02830 0.01769 =
0.02754 -0.00466 0.00238 -0.00190
C21 1 0.517546 0.410338 0.519216 11.00000 0.02128 0.02093 =
0.01663 -0.00001 -0.00309 -0.00173
C22 1 0.430557 0.323480 0.473544 11.00000 0.01893 0.01698 =
0.01432 0.00246 -0.00256 0.00107
C23 1 0.228400 0.289823 0.491199 11.00000 0.01880 0.01870 =
0.01637 -0.00118 0.00062 0.00220
AFIX 43
H23 2 0.138870 0.323687 0.531451 11.00000 -1.20000
AFIX 0
C24 1 0.154912 0.207514 0.451016 11.00000 0.01679 0.01862 =
0.02012 0.00103 -0.00047 -0.00133
AFIX 43
H24 2 0.015986 0.185752 0.463216 11.00000 -1.20000
AFIX 0
C25 1 0.286779 0.157313 0.392761 11.00000 0.02213 0.01541 =
0.01722 0.00096 -0.00228 0.00148
C26 1 0.488873 0.190913 0.373834 11.00000 0.02196 0.02109 =
0.01832 -0.00113 0.00265 0.00512
AFIX 43
H26 2 0.578018 0.157350 0.333126 11.00000 -1.20000
AFIX 0
C27 1 0.559524 0.272389 0.413850 11.00000 0.01703 0.02284 =
0.01667 0.00336 0.00067 0.00121
AFIX 43
H27 2 0.697803 0.294343 0.400821 11.00000 -1.20000
AFIX 0
C28 1 0.041426 0.032667 0.376097 11.00000 0.02557 0.01984 =
0.03470 -0.00455 -0.00488 -0.00275
AFIX 137
H28A 2 0.028544 -0.027200 0.344564 11.00000 -1.50000
H28B 2 -0.082092 0.070258 0.353305 11.00000 -1.50000
H28C 2 0.045039 0.025594 0.448178 11.00000 -1.50000
AFIX 0
O1W 4 1.023452 0.542570 0.555702 11.00000 0.02136 0.01922 =
0.06866 -0.00968 -0.00116 -0.00404
H1W1 2 0.913108 0.511471 0.538803 11.00000 0.05206
H2W1 2 1.140828 0.507793 0.553161 11.00000 0.05105
HKLF 4
REM c22013 : space group Pn
REM wR2 = 0.0637, GooF = S = 1.023, Restrained GooF = 1.030 for all data
REM R1 = 0.0241 for 3995 Fo > 4sig(Fo) and 0.0249 for all 4078 data
REM 327 parameters refined using 3 restraints
END
WGHT 0.0320 0.2099
REM Instructions for potential hydrogen bonds
HTAB O1 O1W_$1
HTAB N1 O2
HTAB C18 O1_$2
HTAB C18 O1W
HTAB C19 O3_$3
HTAB C20 O1W
HTAB O1W O3
HTAB O1W O2_$2
REM Highest difference peak 0.163, deepest hole -0.138, 1-sigma level 0.028
Q1 1 0.5786 0.9218 0.4423 11.00000 0.05 0.16
Q2 1 0.3427 0.7343 0.5451 11.00000 0.05 0.16
Q3 1 0.4670 0.3625 0.4999 11.00000 0.05 0.14
Q4 1 0.2401 0.8137 0.5482 11.00000 0.05 0.14
Q5 1 0.3870 0.9635 0.5429 11.00000 0.05 0.14
;
_shelx_res_checksum 32819
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, 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 O1 0.05552(19) 0.72439(8) 0.57107(10) 0.0207(3) Uani d 1 . .
H H1O 0.053(4) 0.6672(19) 0.561(2) 0.039(7) Uiso d 1 . .
N N1 0.5936(2) 0.54909(9) 0.72662(11) 0.0169(3) Uani d 1 . .
H H1N 0.537(3) 0.5239(15) 0.6666(18) 0.021(5) Uiso d 1 . .
C C1 0.2571(3) 0.85982(11) 0.57192(12) 0.0169(3) Uani d 1 . .
C C2 0.0971(3) 0.89257(12) 0.62852(13) 0.0195(3) Uani d 1 . .
H H2 -0.017827 0.853518 0.642767 0.023 Uiso calc 1 . .
C C3 0.1005(3) 0.98071(12) 0.66482(13) 0.0224(4) Uani d 1 . .
H H3 -0.012447 1.001724 0.702307 0.027 Uiso calc 1 . .
C C4 0.2695(3) 1.03815(12) 0.64621(13) 0.0240(4) Uani d 1 . .
H H4 0.273384 1.098709 0.670526 0.029 Uiso calc 1 . .
C C5 0.4316(3) 1.00568(12) 0.59177(14) 0.0231(4) Uani d 1 . .
H H5 0.548457 1.044559 0.579907 0.028 Uiso calc 1 . .
C C6 0.4294(3) 0.91754(12) 0.55353(13) 0.0197(3) Uani d 1 . .
C C7 0.6095(3) 0.88649(12) 0.49423(14) 0.0220(4) Uani d 1 . .
H H7A 0.670947 0.829778 0.523644 0.026 Uiso calc 1 . .
H H7B 0.724160 0.933119 0.498402 0.026 Uiso calc 1 . .
C C8 0.5390(3) 0.86947(13) 0.38562(14) 0.0242(4) Uani d 1 . .
H H8A 0.511844 0.929638 0.354531 0.029 Uiso calc 1 . .
H H8B 0.663866 0.843058 0.354795 0.029 Uiso calc 1 . .
C C9 0.3461(3) 0.81008(11) 0.35504(13) 0.0207(4) Uani d 1 . .
C C10 0.3015(4) 0.80517(12) 0.25206(14) 0.0279(4) Uani d 1 . .
H H10 0.399634 0.832237 0.210388 0.033 Uiso calc 1 . .
C C11 0.1211(4) 0.76264(12) 0.20880(14) 0.0318(5) Uani d 1 . .
H H11 0.095222 0.761135 0.138778 0.038 Uiso calc 1 . .
C C12 -0.0207(3) 0.72250(12) 0.26846(16) 0.0299(5) Uani d 1 . .
H H12 -0.147085 0.693966 0.239991 0.036 Uiso calc 1 . .
C C13 0.0220(3) 0.72390(11) 0.37074(15) 0.0238(4) Uani d 1 . .
H H13 -0.076086 0.695359 0.411320 0.029 Uiso calc 1 . .
C C14 0.2061(3) 0.76630(10) 0.41590(13) 0.0181(3) Uani d 1 . .
C C15 0.2394(3) 0.76263(11) 0.53007(13) 0.0170(3) Uani d 1 . .
C C16 0.4325(3) 0.70040(11) 0.56309(12) 0.0165(3) Uani d 1 . .
H H16B 0.391728 0.636220 0.550513 0.020 Uiso calc 1 . .
H H16A 0.554670 0.714706 0.523040 0.020 Uiso calc 1 . .
C C17 0.5035(3) 0.71235(11) 0.67311(12) 0.0196(4) Uani d 1 . .
H H17A 0.561491 0.774523 0.683229 0.024 Uiso calc 1 . .
H H17B 0.375332 0.707074 0.711697 0.024 Uiso calc 1 . .
C C18 0.6713(3) 0.64510(11) 0.71430(13) 0.0197(3) Uani d 1 . .
H H18A 0.790325 0.644083 0.669854 0.024 Uiso calc 1 . .
H H18B 0.730746 0.667431 0.779651 0.024 Uiso calc 1 . .
C C19 0.4136(3) 0.54363(13) 0.79194(15) 0.0274(4) Uani d 1 . .
H H19A 0.376582 0.479798 0.802175 0.041 Uiso calc 1 . .
H H19B 0.288444 0.575669 0.760923 0.041 Uiso calc 1 . .
H H19C 0.456773 0.571815 0.855914 0.041 Uiso calc 1 . .
C C20 0.7769(3) 0.49130(12) 0.76608(15) 0.0259(4) Uani d 1 . .
H H20A 0.728457 0.428261 0.771203 0.039 Uiso calc 1 . .
H H20B 0.829547 0.513304 0.831755 0.039 Uiso calc 1 . .
H H20C 0.892900 0.494386 0.721206 0.039 Uiso calc 1 . .
O O2 0.4034(2) 0.45194(8) 0.57830(10) 0.0234(3) Uani d 1 . .
O O3 0.6984(2) 0.43518(11) 0.49734(13) 0.0426(4) Uani d 1 . .
O O4 0.2349(2) 0.07544(8) 0.35022(10) 0.0245(3) Uani d 1 . .
C C21 0.5175(3) 0.41034(11) 0.51922(13) 0.0198(3) Uani d 1 . .
C C22 0.4306(3) 0.32348(11) 0.47354(12) 0.0169(3) Uani d 1 . .
C C23 0.2284(3) 0.28982(11) 0.49120(12) 0.0180(3) Uani d 1 . .
H H23 0.138870 0.323687 0.531451 0.022 Uiso calc 1 . .
C C24 0.1549(3) 0.20751(11) 0.45102(13) 0.0186(3) Uani d 1 . .
H H24 0.015986 0.185752 0.463216 0.022 Uiso calc 1 . .
C C25 0.2868(3) 0.15731(11) 0.39276(13) 0.0184(3) Uani d 1 . .
C C26 0.4889(3) 0.19091(11) 0.37383(13) 0.0204(4) Uani d 1 . .
H H26 0.578018 0.157350 0.333126 0.024 Uiso calc 1 . .
C C27 0.5595(3) 0.27239(11) 0.41385(13) 0.0189(3) Uani d 1 . .
H H27 0.697803 0.294343 0.400821 0.023 Uiso calc 1 . .
C C28 0.0414(3) 0.03267(12) 0.37610(16) 0.0271(4) Uani d 1 . .
H H28A 0.028544 -0.027200 0.344564 0.041 Uiso calc 1 . .
H H28B -0.082092 0.070258 0.353305 0.041 Uiso calc 1 . .
H H28C 0.045039 0.025594 0.448178 0.041 Uiso calc 1 . .
O O1W 1.0235(3) 0.54257(9) 0.55570(14) 0.0366(4) Uani d 1 . .
H H1W1 0.913(5) 0.511(2) 0.539(2) 0.052(8) Uiso d 1 . .
H H2W1 1.141(5) 0.508(2) 0.553(2) 0.051(8) 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 0.0184(6) 0.0168(6) 0.0275(7) -0.0032(5) 0.0055(5) -0.0024(5)
N1 0.0190(7) 0.0155(6) 0.0160(7) -0.0029(5) -0.0002(6) 0.0004(5)
C1 0.0180(8) 0.0181(8) 0.0140(7) 0.0007(6) -0.0024(6) 0.0014(6)
C2 0.0221(9) 0.0200(8) 0.0162(8) -0.0006(7) 0.0005(6) 0.0016(6)
C3 0.0290(9) 0.0226(8) 0.0159(8) 0.0028(7) 0.0027(7) -0.0016(6)
C4 0.0368(11) 0.0164(7) 0.0182(8) -0.0004(7) -0.0015(7) -0.0030(6)
C5 0.0274(10) 0.0206(8) 0.0207(9) -0.0054(7) -0.0015(7) 0.0005(6)
C6 0.0207(8) 0.0197(8) 0.0184(8) -0.0021(7) -0.0011(6) 0.0010(6)
C7 0.0201(8) 0.0211(8) 0.0246(9) -0.0043(7) 0.0004(7) 0.0036(7)
C8 0.0256(9) 0.0273(9) 0.0202(9) -0.0011(8) 0.0063(7) 0.0028(7)
C9 0.0274(9) 0.0174(8) 0.0170(9) 0.0054(7) 0.0006(7) -0.0002(6)
C10 0.0431(12) 0.0209(8) 0.0193(9) 0.0032(8) 0.0008(8) 0.0016(7)
C11 0.0550(14) 0.0202(8) 0.0182(9) 0.0059(9) -0.0107(9) -0.0026(7)
C12 0.0351(11) 0.0207(8) 0.0312(10) 0.0034(8) -0.0148(8) -0.0066(7)
C13 0.0241(9) 0.0188(8) 0.0274(9) 0.0026(7) -0.0063(7) -0.0038(7)
C14 0.0207(8) 0.0139(7) 0.0190(8) 0.0045(6) -0.0030(6) -0.0015(6)
C15 0.0161(8) 0.0165(8) 0.0186(8) -0.0018(6) 0.0016(6) 0.0000(6)
C16 0.0183(8) 0.0159(7) 0.0153(8) -0.0010(6) 0.0009(6) 0.0009(6)
C17 0.0265(9) 0.0170(8) 0.0150(8) -0.0011(7) 0.0000(7) 0.0008(6)
C18 0.0226(8) 0.0164(8) 0.0193(8) -0.0047(7) -0.0037(6) 0.0015(6)
C19 0.0325(11) 0.0230(9) 0.0284(10) -0.0040(7) 0.0135(8) 0.0004(7)
C20 0.0284(9) 0.0196(8) 0.0284(10) 0.0000(7) -0.0063(8) 0.0029(7)
O2 0.0246(7) 0.0201(6) 0.0247(7) 0.0006(5) -0.0032(5) -0.0066(5)
O3 0.0331(8) 0.0486(9) 0.0481(10) -0.0244(7) 0.0155(7) -0.0238(8)
O4 0.0283(7) 0.0177(6) 0.0275(7) -0.0019(5) 0.0024(5) -0.0047(5)
C21 0.0213(8) 0.0209(8) 0.0166(8) -0.0017(7) -0.0031(6) 0.0000(6)
C22 0.0189(8) 0.0170(7) 0.0143(7) 0.0011(6) -0.0026(6) 0.0025(6)
C23 0.0188(8) 0.0187(8) 0.0164(8) 0.0022(6) 0.0006(6) -0.0012(6)
C24 0.0168(8) 0.0186(8) 0.0201(8) -0.0013(7) -0.0005(6) 0.0010(6)
C25 0.0221(8) 0.0154(7) 0.0172(8) 0.0015(7) -0.0023(6) 0.0010(6)
C26 0.0220(9) 0.0211(8) 0.0183(8) 0.0051(7) 0.0027(7) -0.0011(6)
C27 0.0170(8) 0.0228(8) 0.0167(8) 0.0012(7) 0.0007(6) 0.0034(6)
C28 0.0256(9) 0.0198(8) 0.0347(10) -0.0028(8) -0.0049(8) -0.0046(7)
O1W 0.0214(7) 0.0192(6) 0.0687(11) -0.0040(6) -0.0012(7) -0.0097(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C15 O1 H1O . . 109.4(18) ?
C19 N1 C20 . . 110.48(14) ?
C19 N1 C18 . . 112.39(14) ?
C20 N1 C18 . . 109.28(13) ?
C19 N1 H1N . . 104.0(13) ?
C20 N1 H1N . . 108.3(13) ?
C18 N1 H1N . . 112.2(13) ?
C2 C1 C6 . . 118.54(15) ?
C2 C1 C15 . . 119.39(15) ?
C6 C1 C15 . . 122.07(15) ?
C3 C2 C1 . . 121.84(16) ?
C3 C2 H2 . . 119.1 ?
C1 C2 H2 . . 119.1 ?
C2 C3 C4 . . 119.81(17) ?
C2 C3 H3 . . 120.1 ?
C4 C3 H3 . . 120.1 ?
C5 C4 C3 . . 118.82(16) ?
C5 C4 H4 . . 120.6 ?
C3 C4 H4 . . 120.6 ?
C4 C5 C6 . . 122.16(17) ?
C4 C5 H5 . . 118.9 ?
C6 C5 H5 . . 118.9 ?
C5 C6 C1 . . 118.81(16) ?
C5 C6 C7 . . 119.64(15) ?
C1 C6 C7 . . 121.55(15) ?
C6 C7 C8 . . 113.10(15) ?
C6 C7 H7A . . 109.0 ?
C8 C7 H7A . . 109.0 ?
C6 C7 H7B . . 109.0 ?
C8 C7 H7B . . 109.0 ?
H7A C7 H7B . . 107.8 ?
C9 C8 C7 . . 121.58(15) ?
C9 C8 H8A . . 106.9 ?
C7 C8 H8A . . 106.9 ?
C9 C8 H8B . . 106.9 ?
C7 C8 H8B . . 106.9 ?
H8A C8 H8B . . 106.7 ?
C14 C9 C10 . . 118.31(17) ?
C14 C9 C8 . . 128.30(16) ?
C10 C9 C8 . . 113.26(16) ?
C11 C10 C9 . . 122.71(19) ?
C11 C10 H10 . . 118.6 ?
C9 C10 H10 . . 118.6 ?
C12 C11 C10 . . 119.06(18) ?
C12 C11 H11 . . 120.5 ?
C10 C11 H11 . . 120.5 ?
C11 C12 C13 . . 119.64(18) ?
C11 C12 H12 . . 120.2 ?
C13 C12 H12 . . 120.2 ?
C12 C13 C14 . . 121.97(19) ?
C12 C13 H13 . . 119.0 ?
C14 C13 H13 . . 119.0 ?
C9 C14 C13 . . 118.22(16) ?
C9 C14 C15 . . 124.09(15) ?
C13 C14 C15 . . 117.69(16) ?
O1 C15 C1 . . 105.14(13) ?
O1 C15 C14 . . 110.50(13) ?
C1 C15 C14 . . 109.65(13) ?
O1 C15 C16 . . 106.53(13) ?
C1 C15 C16 . . 114.15(13) ?
C14 C15 C16 . . 110.67(13) ?
C17 C16 C15 . . 111.99(14) ?
C17 C16 H16B . . 109.2 ?
C15 C16 H16B . . 109.2 ?
C17 C16 H16A . . 109.2 ?
C15 C16 H16A . . 109.2 ?
H16B C16 H16A . . 107.9 ?
C18 C17 C16 . . 115.12(14) ?
C18 C17 H17A . . 108.5 ?
C16 C17 H17A . . 108.5 ?
C18 C17 H17B . . 108.5 ?
C16 C17 H17B . . 108.5 ?
H17A C17 H17B . . 107.5 ?
N1 C18 C17 . . 115.72(14) ?
N1 C18 H18A . . 108.4 ?
C17 C18 H18A . . 108.4 ?
N1 C18 H18B . . 108.4 ?
C17 C18 H18B . . 108.4 ?
H18A C18 H18B . . 107.4 ?
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 ?
C25 O4 C28 . . 117.67(14) ?
O3 C21 O2 . . 124.79(16) ?
O3 C21 C22 . . 117.31(16) ?
O2 C21 C22 . . 117.89(15) ?
C23 C22 C27 . . 118.31(15) ?
C23 C22 C21 . . 122.41(15) ?
C27 C22 C21 . . 119.23(15) ?
C24 C23 C22 . . 121.28(16) ?
C24 C23 H23 . . 119.4 ?
C22 C23 H23 . . 119.4 ?
C23 C24 C25 . . 119.45(15) ?
C23 C24 H24 . . 120.3 ?
C25 C24 H24 . . 120.3 ?
O4 C25 C24 . . 125.17(15) ?
O4 C25 C26 . . 115.15(15) ?
C24 C25 C26 . . 119.69(15) ?
C27 C26 C25 . . 120.30(16) ?
C27 C26 H26 . . 119.9 ?
C25 C26 H26 . . 119.9 ?
C26 C27 C22 . . 120.96(16) ?
C26 C27 H27 . . 119.5 ?
C22 C27 H27 . . 119.5 ?
O4 C28 H28A . . 109.5 ?
O4 C28 H28B . . 109.5 ?
H28A C28 H28B . . 109.5 ?
O4 C28 H28C . . 109.5 ?
H28A C28 H28C . . 109.5 ?
H28B C28 H28C . . 109.5 ?
H1W1 O1W H2W1 . . 109(3) ?
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 . 1.427(2) ?
O1 H1O . 0.85(3) ?
N1 C19 . 1.482(2) ?
N1 C20 . 1.492(2) ?
N1 C18 . 1.507(2) ?
N1 H1N . 0.94(2) ?
C1 C2 . 1.389(2) ?
C1 C6 . 1.407(2) ?
C1 C15 . 1.540(2) ?
C2 C3 . 1.387(2) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.389(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.380(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.397(2) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.500(3) ?
C7 C8 . 1.524(3) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 C9 . 1.521(3) ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C14 . 1.401(3) ?
C9 C10 . 1.403(3) ?
C10 C11 . 1.381(3) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.374(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.391(3) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.407(2) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.545(2) ?
C15 C16 . 1.553(2) ?
C16 C17 . 1.532(2) ?
C16 H16B . 0.9900 ?
C16 H16A . 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 . 1.243(2) ?
O4 C25 . 1.364(2) ?
O4 C28 . 1.428(2) ?
C21 C22 . 1.504(2) ?
C22 C23 . 1.392(2) ?
C22 C27 . 1.401(2) ?
C23 C24 . 1.392(2) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.393(2) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.396(3) ?
C26 C27 . 1.375(2) ?
C26 H26 . 0.9500 ?
C27 H27 . 0.9500 ?
C28 H28A . 0.9800 ?
C28 H28B . 0.9800 ?
C28 H28C . 0.9800 ?
O1W H1W1 . 0.84(3) ?
O1W H2W1 . 0.90(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 0.85(3) 1.84(3) 2.6911(18) 171(3) yes
N1 H1N O2 . 0.94(2) 1.76(2) 2.6711(18) 163(2) yes
C18 H18A O1 1_655 0.99 2.50 3.400(2) 150.9 yes
C18 H18A O1W . 0.99 2.66 3.523(3) 146.0 yes
C19 H19C O3 2_465 0.98 2.59 3.191(3) 119.3 yes
C20 H20C O1W . 0.98 2.54 3.420(3) 149.2 yes
O1W H1W1 O3 . 0.84(3) 1.81(3) 2.646(2) 173(3) yes
O1W H2W1 O2 1_655 0.90(3) 1.84(3) 2.718(2) 165(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 . . . . 1.7(2) ?
C15 C1 C2 C3 . . . . -177.45(15) ?
C1 C2 C3 C4 . . . . -1.2(3) ?
C2 C3 C4 C5 . . . . -0.2(3) ?
C3 C4 C5 C6 . . . . 1.0(3) ?
C4 C5 C6 C1 . . . . -0.5(3) ?
C4 C5 C6 C7 . . . . 179.51(17) ?
C2 C1 C6 C5 . . . . -0.8(2) ?
C15 C1 C6 C5 . . . . 178.29(15) ?
C2 C1 C6 C7 . . . . 179.15(15) ?
C15 C1 C6 C7 . . . . -1.8(2) ?
C5 C6 C7 C8 . . . . -112.86(18) ?
C1 C6 C7 C8 . . . . 67.2(2) ?
C6 C7 C8 C9 . . . . -50.9(2) ?
C7 C8 C9 C14 . . . . 2.0(3) ?
C7 C8 C9 C10 . . . . 177.79(17) ?
C14 C9 C10 C11 . . . . 3.0(3) ?
C8 C9 C10 C11 . . . . -173.25(17) ?
C9 C10 C11 C12 . . . . -0.6(3) ?
C10 C11 C12 C13 . . . . -1.2(3) ?
C11 C12 C13 C14 . . . . 0.7(3) ?
C10 C9 C14 C13 . . . . -3.4(2) ?
C8 C9 C14 C13 . . . . 172.22(17) ?
C10 C9 C14 C15 . . . . 177.46(16) ?
C8 C9 C14 C15 . . . . -6.9(3) ?
C12 C13 C14 C9 . . . . 1.6(2) ?
C12 C13 C14 C15 . . . . -179.15(16) ?
C2 C1 C15 O1 . . . . -5.43(19) ?
C6 C1 C15 O1 . . . . 175.48(15) ?
C2 C1 C15 C14 . . . . 113.37(16) ?
C6 C1 C15 C14 . . . . -65.71(19) ?
C2 C1 C15 C16 . . . . -121.82(16) ?
C6 C1 C15 C16 . . . . 59.1(2) ?
C9 C14 C15 O1 . . . . 171.96(14) ?
C13 C14 C15 O1 . . . . -7.22(19) ?
C9 C14 C15 C1 . . . . 56.5(2) ?
C13 C14 C15 C1 . . . . -122.66(16) ?
C9 C14 C15 C16 . . . . -70.29(19) ?
C13 C14 C15 C16 . . . . 110.54(16) ?
O1 C15 C16 C17 . . . . -73.23(16) ?
C1 C15 C16 C17 . . . . 42.34(19) ?
C14 C15 C16 C17 . . . . 166.61(13) ?
C15 C16 C17 C18 . . . . 172.16(14) ?
C19 N1 C18 C17 . . . . -57.8(2) ?
C20 N1 C18 C17 . . . . 179.13(15) ?
C16 C17 C18 N1 . . . . -71.7(2) ?
O3 C21 C22 C23 . . . . -178.82(18) ?
O2 C21 C22 C23 . . . . 2.4(2) ?
O3 C21 C22 C27 . . . . 3.6(2) ?
O2 C21 C22 C27 . . . . -175.24(15) ?
C27 C22 C23 C24 . . . . 0.1(2) ?
C21 C22 C23 C24 . . . . -177.54(16) ?
C22 C23 C24 C25 . . . . 0.6(2) ?
C28 O4 C25 C24 . . . . -7.5(2) ?
C28 O4 C25 C26 . . . . 172.93(15) ?
C23 C24 C25 O4 . . . . 179.18(16) ?
C23 C24 C25 C26 . . . . -1.2(2) ?
O4 C25 C26 C27 . . . . -179.22(15) ?
C24 C25 C26 C27 . . . . 1.2(3) ?
C25 C26 C27 C22 . . . . -0.4(3) ?
C23 C22 C27 C26 . . . . -0.2(2) ?
C21 C22 C27 C26 . . . . 177.53(15) ?
_cod_database_fobs_code 2022743