#------------------------------------------------------------------------------
#$Date: 2023-07-15 03:47:13 +0200 (Sat, 15 Jul 2023) $
#$Revision: 285218 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022816.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_2022816
loop_
_publ_author_name
Vinaya,
'Basavaraju, Yeriyur B.'
'Yathirajan, Hemmige S.'
'Parkin, Sean'
_publ_section_title
;
Crystal structures of four organic salts of trihexyphenidyl at
90 K
;
_journal_coeditor_code VM2286
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023005960
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C20 H32 N O +, C7 H4 N O4 -'
_chemical_formula_moiety 'C20 H32 N O +, C7 H4 N O4 -'
_chemical_formula_sum 'C27 H36 N2 O5'
_chemical_formula_weight 468.58
_chemical_name_common
;
Trihexyphenidylium 4-nitrobenzoate
;
_chemical_name_systematic
;
1-(3-Cyclohexyl-3-hydroxy-3-phenylpropyl)piperidin-1-ium 4-nitrobenzoate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -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 85.329(3)
_cell_angle_beta 79.534(4)
_cell_angle_gamma 87.785(3)
_cell_formula_units_Z 2
_cell_length_a 6.2568(5)
_cell_length_b 11.7542(14)
_cell_length_c 16.9162(19)
_cell_measurement_reflns_used 9957
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 27.54
_cell_measurement_theta_min 2.20
_cell_volume 1219.0(2)
_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) and
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 0.996
_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 0.0411
_diffrn_reflns_av_unetI/netI 0.0273
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 35646
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.557
_diffrn_reflns_theta_min 2.051
_diffrn_source microsource
_exptl_absorpt_coefficient_mu 0.088
_exptl_absorpt_correction_T_max 0.959
_exptl_absorpt_correction_T_min 0.907
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.277
_exptl_crystal_description plate
_exptl_crystal_F_000 504
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.303
_refine_diff_density_min -0.193
_refine_ls_extinction_coef 0.0101(18)
_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 2008)
;
_refine_ls_goodness_of_fit_ref 1.114
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 355
_refine_ls_number_reflns 5590
_refine_ls_number_restraints 68
_refine_ls_restrained_S_all 1.109
_refine_ls_R_factor_all 0.0555
_refine_ls_R_factor_gt 0.0465
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.7788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1028
_refine_ls_wR_factor_ref 0.1074
_reflns_number_gt 4825
_reflns_number_total 5590
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2286sup1.cif
_cod_data_source_block I
_cod_database_code 2022816
_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 0.974
_shelx_estimated_absorpt_t_max 0.996
_shelx_hkl_file
;
-1 0 0 319.934 9.01045 3
-1 0 0 317.495 9.01819 3
1 0 0 305.708 9.00549 3
1 0 0 320.334 8.97611 3
-2 0 0 260.137 8.02854 3
-2 0 0 254.529 7.89631 3
2 0 0 265.403 7.86042 3
2 0 0 266.925 7.99746 3
-3 0 0 3.88053 0.79691 3
3 0 0 5.07266 0.74135 3
3 0 0 4.51133 0.79161 3
-4 0 0 39.9526 3.50149 5
-4 0 0 41.6146 2.24566 3
-4 0 0 42.4480 2.44864 3
-5 0 0 179.993 8.87433 5
-6 0 0 1.92374 0.91727 6
-6 0 0 0.52728 0.77170 6
-6 0 0 4.08338 1.66036 5
-6 0 0 -1.7635 2.27782 4
-7 0 0 15.5069 2.96965 5
-7 0 0 14.8857 2.15492 6
-7 0 0 12.7490 2.24464 6
-7 0 0 15.2216 3.71420 5
-8 0 0 119.914 11.9293 4
-7 1 0 1.89817 2.07432 5
-7 1 0 2.28012 3.34280 4
-7 1 0 2.63357 1.34427 6
-7 1 0 0.40359 1.06224 6
-7 1 0 1.23190 2.66171 5
-6 1 0 31.1539 5.66831 4
-6 1 0 34.4473 4.27840 5
-6 1 0 31.3880 2.17577 6
-6 1 0 30.6560 2.30396 6
-5 1 0 396.312 16.2753 5
-5 1 0 403.507 18.7453 4
-4 1 0 3.45508 0.69747 3
3 -1 0 15.5125 1.22186 3
3 -1 0 15.0704 1.03979 3
-3 1 0 16.9758 1.26304 3
-3 1 0 16.3497 1.51245 3
2 -1 0 40.5851 1.84080 3
2 -1 0 39.9809 2.16216 3
-2 1 0 36.2014 2.13741 3
-2 1 0 41.6266 2.04473 3
1 -1 0 1159.07 33.0297 3
-1 1 0 1147.33 33.1795 3
-1 1 0 1225.72 34.5109 4
-1 -1 0 147.353 4.85901 6
-1 -1 0 150.820 5.56051 3
-1 -1 0 149.351 5.48909 3
-1 -1 0 145.111 4.63798 6
-1 -1 0 153.794 5.25854 4
-1 -1 0 150.298 4.49799 5
1 1 0 146.945 5.53577 3
1 1 0 151.172 4.52866 5
-2 -1 0 1291.27 37.1365 3
-2 -1 0 1310.86 37.5048 3
-2 -1 0 1319.42 36.8175 5
2 1 0 1288.21 37.4435 3
2 1 0 1333.96 36.9689 3
-3 -1 0 269.236 9.48755 5
-3 -1 0 275.884 9.10467 3
-3 -1 0 278.418 9.72458 3
3 1 0 268.228 9.42478 3
3 1 0 273.900 8.76315 3
-4 -1 0 675.997 20.8213 3
-4 -1 0 645.582 20.9307 5
4 1 0 665.557 19.2300 3
4 1 0 666.582 19.7334 3
-5 -1 0 213.949 7.34805 3
-5 -1 0 206.948 7.00154 6
-5 -1 0 218.725 8.11754 3
-5 -1 0 204.671 7.35969 6
-5 -1 0 211.928 8.92666 5
-6 -1 0 2.75636 1.15878 6
-6 -1 0 1.38172 1.24183 5
-6 -1 0 -0.6300 0.79989 6
-7 -1 0 54.8593 5.31738 5
-7 -1 0 62.2196 3.93460 6
-7 -1 0 63.4787 7.79480 4
-7 -1 0 54.8956 4.64015 6
-7 -1 0 56.1972 4.33955 5
-7 2 0 12.6550 1.90446 6
-7 2 0 9.24217 4.25273 4
-7 2 0 17.0643 2.54691 6
-7 2 0 5.65785 3.49614 5
-6 2 0 3.44056 0.97141 6
-6 2 0 4.99044 1.31556 6
-6 2 0 7.00418 3.11439 4
-6 2 0 1.67303 2.01370 5
-5 2 0 3.67631 0.87147 3
-5 2 0 5.12296 2.75390 4
-5 2 0 3.73732 0.79731 3
4 -2 0 50.0955 2.21300 3
-4 2 0 52.4638 5.90492 4
-4 2 0 49.7718 2.68615 3
3 -2 0 251.860 8.80344 3
3 -2 0 242.671 8.01825 3
-3 2 0 237.358 8.40443 3
-3 2 0 241.065 9.05631 3
-3 2 0 236.616 11.7611 4
2 -2 0 818.102 24.4125 3
2 -2 0 831.069 25.0231 3
-2 2 0 809.103 22.9812 6
-2 2 0 807.848 23.2102 6
-2 2 0 830.207 24.8163 3
-2 2 0 814.527 25.0613 3
-2 2 0 887.802 27.5780 4
1 -2 0 1888.45 53.1272 4
1 -2 0 1858.09 52.3940 3
1 -2 0 1759.22 52.0653 3
1 -2 0 1834.41 50.6250 6
-1 2 0 1843.17 52.3315 3
-1 2 0 1854.30 53.1137 4
-1 2 0 1828.69 52.3764 3
-1 2 0 1783.36 51.2928 6
0 -2 0 560.149 17.3526 6
0 -2 0 559.365 17.9991 3
0 -2 0 578.569 17.4245 6
0 -2 0 583.102 17.3423 4
0 -2 0 572.374 18.0230 3
0 2 0 542.599 17.3477 6
0 2 0 540.893 17.9099 3
0 2 0 567.333 17.2264 4
0 2 0 556.703 17.3995 6
0 2 0 578.701 18.0734 3
-1 -2 0 192.609 7.81491 3
-1 -2 0 207.032 6.52510 4
-1 -2 0 175.870 7.68903 3
-1 -2 0 198.543 7.29921 6
-1 -2 0 196.386 6.50833 5
-1 -2 0 185.157 6.97407 6
1 2 0 195.077 6.50029 4
1 2 0 188.117 6.64560 6
1 2 0 188.979 6.92054 6
1 2 0 194.642 7.89574 3
1 2 0 188.764 7.70939 3
1 2 0 195.115 6.29815 5
-2 -2 0 780.863 21.2937 5
-2 -2 0 791.597 23.7987 3
-2 -2 0 723.350 22.6323 4
-2 -2 0 743.923 21.9262 6
-2 -2 0 739.768 23.2854 3
-2 -2 0 761.421 22.4923 6
2 2 0 727.801 23.5054 3
2 2 0 744.233 21.3170 5
-3 -2 0 37.9734 2.82354 3
-3 -2 0 36.4046 2.42957 6
-3 -2 0 30.3242 2.91838 4
-3 -2 0 35.8836 1.99199 5
-3 -2 0 36.7713 3.13360 3
-3 -2 0 34.9311 2.03680 6
3 2 0 36.5685 2.61369 3
3 2 0 36.2744 3.06462 3
-4 -2 0 200.177 9.52197 4
-4 -2 0 202.791 7.89935 3
-4 -2 0 197.149 7.22583 5
-4 -2 0 198.327 6.98855 6
-4 -2 0 203.128 8.83385 3
-4 -2 0 196.806 7.61968 6
4 2 0 202.351 7.37653 3
4 2 0 196.721 8.29176 3
-5 -2 0 405.309 14.5114 3
-5 -2 0 381.251 16.2186 4
-5 -2 0 401.453 13.1803 3
-5 -2 0 385.791 12.8012 6
-5 -2 0 389.330 13.7562 6
-5 -2 0 395.041 13.1233 5
5 2 0 390.783 12.1943 3
5 2 0 401.615 12.7069 3
-6 -2 0 638.242 18.5802 3
-6 -2 0 596.302 20.0338 3
-6 -2 0 586.224 20.5003 5
-6 -2 0 618.993 20.6728 6
-6 -2 0 618.899 19.6074 6
-6 -2 0 604.928 23.7350 4
-6 -2 0 623.612 19.4101 5
-7 -2 0 49.6563 6.74216 4
-7 -2 0 54.3791 4.15717 6
-7 -2 0 51.4908 3.36464 5
-7 -2 0 51.8976 3.94476 5
-7 -2 0 56.5026 4.74804 6
-7 3 0 5.74773 3.66702 4
-7 3 0 4.19267 1.99717 6
-7 3 0 0.24353 2.77373 5
-6 3 0 898.245 25.9011 6
-6 3 0 869.401 38.5506 4
-6 3 0 867.770 27.2615 6
-6 3 0 841.022 32.1894 5
-5 3 0 70.7322 3.58138 3
-5 3 0 73.3285 4.09798 6
-5 3 0 72.9773 3.42394 6
-5 3 0 76.5705 8.37697 4
-5 3 0 66.6698 4.15379 3
4 -3 0 380.942 12.9659 3
4 -3 0 393.670 12.1313 3
-4 3 0 376.819 11.6789 6
-4 3 0 381.936 12.8318 3
-4 3 0 356.148 17.5732 4
-4 3 0 373.294 12.4265 6
-4 3 0 401.220 14.0595 3
3 -3 0 345.914 12.1159 3
3 -3 0 357.891 13.0850 3
-3 3 0 375.765 13.5375 3
-3 3 0 360.125 12.7633 3
-3 3 0 353.446 11.7567 6
-3 3 0 355.795 16.0065 4
-3 3 0 351.435 11.0933 6
2 -3 0 9.27235 1.80268 3
-2 3 0 8.48357 1.91844 3
-2 3 0 13.2821 2.74050 4
-2 3 0 9.98956 1.55025 6
-2 3 0 6.67272 1.65354 3
1 -3 0 2.54846 1.36184 3
1 -3 0 2.59621 0.88335 6
1 -3 0 1.01976 1.10940 3
1 -3 0 6.08414 1.60585 4
1 -3 0 2.07814 0.90596 6
-1 3 0 2.19678 1.23592 3
-1 3 0 3.29906 1.21448 6
-1 3 0 0.58887 1.04098 3
-1 3 0 0.29988 0.94494 6
-1 3 0 3.35732 1.66952 4
0 -3 0 9999.99 290.761 2
0 3 0 9956.90 290.250 2
-1 -3 0 2388.66 70.1060 6
-1 -3 0 2385.46 69.9227 6
-1 -3 0 2484.55 71.2145 3
-1 -3 0 2475.78 71.0938 3
1 3 0 2413.53 71.0878 3
1 3 0 2617.60 71.2619 3
-2 -3 0 273.820 10.6801 6
-2 -3 0 283.334 11.6307 3
-2 -3 0 282.137 9.65851 4
-2 -3 0 275.492 9.06743 5
-2 -3 0 268.186 11.2411 3
-2 -3 0 279.833 10.3236 6
2 3 0 292.074 8.62097 5
2 3 0 282.091 10.1093 4
2 3 0 281.351 9.17555 6
2 3 0 280.170 8.85477 6
2 3 0 268.481 11.5493 3
2 3 0 293.903 11.3057 3
-3 -3 0 15.6101 1.86418 6
-3 -3 0 16.4072 2.32249 6
-3 -3 0 15.5996 1.22361 5
-3 -3 0 15.3109 2.52043 3
-3 -3 0 15.2936 1.96039 4
3 3 0 16.6495 2.60843 3
-4 -3 0 12.9325 2.28192 4
-4 -3 0 12.3971 2.56371 3
-4 -3 0 10.8558 1.13313 5
-4 -3 0 11.8016 2.17253 6
-4 -3 0 9.28833 1.73928 6
-4 -3 0 14.9942 2.22569 3
4 3 0 13.0361 2.45110 3
4 3 0 11.2684 1.84683 3
-5 -3 0 8.05790 2.07856 6
-5 -3 0 6.86772 2.05797 3
-5 -3 0 6.43009 1.01741 5
-5 -3 0 6.34794 1.19761 5
-5 -3 0 7.86883 2.39309 4
-5 -3 0 7.80053 1.71491 3
-5 -3 0 10.9828 1.89463 6
5 3 0 6.91127 1.89329 3
5 3 0 5.96491 1.46386 3
-6 -3 0 16.0387 2.63278 3
-6 -3 0 12.0721 2.05012 3
-6 -3 0 9.46266 2.81480 6
-6 -3 0 10.1891 2.29424 6
-6 -3 0 10.6888 2.99218 4
-7 -3 0 0.99662 2.30920 4
-7 -3 0 0.50125 2.16086 6
-7 -3 0 2.03729 2.13997 4
-7 -3 0 4.61061 2.09652 6
-7 4 0 34.8198 3.46692 6
-7 4 0 36.4580 4.22445 6
-7 4 0 39.8069 6.29740 5
-7 4 0 48.5831 8.30330 4
-6 4 0 4.78879 1.13655 3
-6 4 0 -2.3991 2.40704 4
-6 4 0 3.25554 2.13034 6
-6 4 0 3.37451 1.56115 6
5 -4 0 25.3385 1.96029 3
-5 4 0 26.1287 2.50194 6
-5 4 0 29.8008 3.24760 6
-5 4 0 27.9961 5.88131 4
-5 4 0 28.4026 3.22578 3
-5 4 0 26.3554 2.58511 3
4 -4 0 6.09193 1.37726 3
4 -4 0 8.18304 1.86885 3
-4 4 0 5.60231 1.86434 3
-4 4 0 1.28065 2.34874 4
-4 4 0 5.30338 1.74647 6
-4 4 0 9.48386 1.66158 6
-4 4 0 7.09385 1.72338 3
3 -4 0 318.325 12.1541 3
-3 4 0 311.013 13.1840 3
-3 4 0 308.779 15.2179 4
-3 4 0 323.885 11.3622 6
-3 4 0 323.454 11.9690 6
-3 4 0 319.288 12.7939 3
2 -4 0 101.028 3.37989 6
2 -4 0 94.2868 6.17025 3
2 -4 0 99.4597 3.47227 6
2 -4 0 94.4048 5.83695 3
-2 4 0 103.450 7.14087 4
-2 4 0 98.7483 6.39908 3
-2 4 0 99.5197 5.52326 6
-2 4 0 104.333 6.32952 3
-2 4 0 101.160 5.36819 6
1 -4 0 63.2267 5.03618 3
1 -4 0 60.9839 3.78557 6
1 -4 0 61.9739 4.02428 6
1 -4 0 62.9860 4.90030 4
1 -4 0 64.6388 4.89212 3
-1 4 0 67.7740 4.60204 6
-1 4 0 56.4076 4.22857 6
-1 4 0 62.3815 4.97222 3
-1 4 0 68.4305 5.13940 4
-1 4 0 65.8259 5.08293 3
0 -4 0 203.683 9.01443 6
0 -4 0 213.594 10.1546 3
0 -4 0 193.797 9.69716 3
0 -4 0 202.783 8.93786 4
0 -4 0 206.819 9.03130 6
0 4 0 204.462 9.15870 6
0 4 0 190.982 9.80535 3
0 4 0 202.620 9.89668 3
0 4 0 204.657 8.75317 4
0 4 0 214.014 9.27471 6
-1 -4 0 875.461 28.7452 3
-1 -4 0 856.416 27.5456 6
-1 -4 0 832.068 27.5279 6
-1 -4 0 880.410 28.9079 3
-1 -4 0 892.513 26.3564 4
1 4 0 832.700 27.1530 6
1 4 0 854.115 27.0110 6
1 4 0 853.393 25.7651 4
1 4 0 802.091 26.3660 5
1 4 0 890.038 28.9048 3
1 4 0 859.674 28.5998 3
-2 -4 0 468.272 17.6140 3
-2 -4 0 452.338 14.9216 4
-2 -4 0 473.179 16.5253 6
-2 -4 0 448.535 17.7266 3
-2 -4 0 455.956 16.7600 6
2 4 0 463.763 14.8764 6
2 4 0 430.739 17.4644 3
2 4 0 464.212 14.1767 5
2 4 0 463.525 15.1210 4
2 4 0 464.958 15.4116 6
2 4 0 431.612 17.1011 3
-3 -4 0 2.29037 1.26375 6
-3 -4 0 5.45429 1.71826 6
-3 -4 0 2.51566 1.76061 3
-3 -4 0 2.15053 1.53544 3
-3 -4 0 3.30781 1.13073 4
3 4 0 1.37371 1.39356 3
3 4 0 1.78917 1.26005 3
3 4 0 3.25513 0.62886 5
-4 -4 0 34.3710 3.75642 6
-4 -4 0 37.4644 3.33825 4
-4 -4 0 37.5030 4.22059 3
-4 -4 0 31.7885 3.59274 3
4 4 0 33.0756 3.93985 3
-5 -4 0 4.96956 2.32261 6
-5 -4 0 8.93413 2.48370 3
-5 -4 0 9.96331 2.12925 6
-5 -4 0 8.90553 2.40143 4
-5 -4 0 3.62688 1.71188 3
5 4 0 8.12830 1.77282 3
5 4 0 6.60479 2.21566 3
-6 -4 0 16.5997 3.11358 4
-6 -4 0 17.0195 3.40683 6
-6 -4 0 16.9893 3.23260 6
-6 -4 0 13.2480 2.97472 3
-6 -4 0 19.8589 2.64297 3
6 4 0 14.1861 2.51590 3
-7 -4 0 5.32932 2.74068 4
-7 -4 0 6.64968 3.01608 6
-7 -4 0 10.0074 3.16758 6
-7 -4 0 11.5650 1.97600 3
-7 5 0 1.40428 2.03544 6
-7 5 0 -3.6144 2.80840 5
-7 5 0 11.8551 5.02639 4
-6 5 0 27.4234 3.17978 3
-6 5 0 15.7700 3.31499 6
-6 5 0 24.1832 3.42999 6
-6 5 0 19.2312 5.59822 4
-6 5 0 24.3445 2.43953 3
5 -5 0 8.64445 2.08144 3
5 -5 0 14.7973 1.89425 3
-5 5 0 14.5366 2.76695 3
-5 5 0 12.5146 2.65634 6
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0 -1 20 61.6225 7.52442 6
-1 1 -20 1.99660 2.95016 6
-1 1 -20 -0.9764 2.41175 3
-1 1 -20 -0.6701 2.72341 5
1 -1 20 3.06414 3.64764 3
1 -1 20 4.05545 2.83512 6
-2 1 -20 4.82031 3.40011 3
-2 1 -20 1.04435 2.91899 5
-2 1 -20 3.62668 2.76510 6
-2 1 -20 10.5005 4.14105 4
2 -1 20 9.96773 4.30258 3
-3 1 -20 74.0321 8.24205 4
-3 1 -20 80.6024 10.4621 5
-3 1 -20 81.1392 8.67716 6
-3 1 -20 83.7393 10.1595 3
3 -1 20 90.8103 7.21220 6
3 -1 20 84.1839 9.73033 3
-4 1 -20 6.01833 3.74326 3
-4 1 -20 7.27940 3.66787 4
-4 1 -20 14.1806 4.70186 5
4 -1 20 -1.1632 4.15001 3
1 0 -20 1.33697 4.35239 3
1 0 -20 3.84530 3.55402 6
1 0 -20 3.64740 3.84623 5
-1 0 20 3.91204 3.17704 6
-1 0 20 8.95168 4.34577 3
0 0 -20 17.8838 5.73975 3
0 0 -20 11.3202 3.94332 6
0 0 -20 15.3038 5.07299 5
0 0 20 19.0258 4.42893 6
0 0 20 12.9550 5.11327 3
-1 0 -20 -4.0765 3.02039 5
-1 0 -20 0.29392 2.69659 6
-1 0 -20 1.80956 3.12005 3
1 0 20 0.56571 3.37282 3
-2 0 -20 -0.4097 2.40125 6
-2 0 -20 0.28758 3.42763 5
-2 0 -20 1.00679 2.63622 3
2 0 20 -2.3917 2.76475 3
-3 0 -20 -0.2947 3.02907 6
-3 0 -20 -5.8551 3.22169 3
-3 0 -20 -0.8820 2.83523 3
-3 0 -20 0.37402 2.67040 5
-3 0 -20 -0.3159 2.96951 4
3 0 20 -4.6598 2.89277 6
3 0 20 5.47182 4.29767 3
-4 0 -20 43.8455 6.64501 3
-4 0 -20 42.6686 7.77198 5
-4 0 -20 45.2551 6.62654 4
-4 0 -20 42.9904 6.34953 6
1 -1 -20 10.1584 4.39168 5
1 -1 -20 -1.6734 3.55026 6
1 -1 -20 -0.5124 3.25301 3
-1 1 20 1.54062 3.66707 6
-1 1 20 6.40889 4.03211 3
0 -1 -20 93.3471 9.50257 6
0 -1 -20 58.7343 8.94070 3
0 -1 -20 70.6885 8.82188 5
0 1 20 70.8145 9.54273 3
-1 -1 -20 2.67243 3.56036 3
-1 -1 -20 4.54594 3.73413 5
-1 -1 -20 0.47407 3.16378 6
1 1 20 5.97954 3.93617 6
1 1 20 5.85555 4.03571 3
-2 -1 -20 4.45090 3.56569 5
-2 -1 -20 9.09498 4.00084 3
-2 -1 -20 2.15599 3.00284 6
2 1 20 13.6694 4.88747 3
-3 -1 -20 44.3494 7.99080 3
-3 -1 -20 39.7205 7.11388 3
-3 -1 -20 51.0444 7.73632 5
-3 -1 -20 51.0453 6.79694 6
3 1 20 60.0633 7.22342 6
3 1 20 49.4222 8.46255 3
3 1 20 46.9527 6.08812 6
-4 -1 -20 51.4720 7.77326 5
-4 -1 -20 55.4901 8.13795 3
-4 -1 -20 62.4312 7.69486 6
1 -2 -20 12.1237 4.66637 3
1 -2 -20 7.01167 4.16102 5
1 -2 -20 7.04498 4.46844 6
-1 2 20 3.45894 3.55169 3
0 -2 -20 9.56313 4.78203 3
0 -2 -20 6.15086 3.79198 5
0 -2 -20 6.84418 4.52267 6
0 2 20 8.24495 4.26183 6
0 2 20 6.56480 4.20700 3
-1 -2 -20 2.71917 3.45830 3
-1 -2 -20 -1.2087 2.49876 5
-1 -2 -20 1.10475 2.60888 6
1 2 20 2.24025 3.66510 3
1 2 20 -1.1757 2.66743 6
-2 -2 -20 3.65827 3.90552 5
-2 -2 -20 6.95321 3.78214 6
-2 -2 -20 9.48477 4.34782 3
2 2 20 6.82660 4.29685 6
2 2 20 2.58688 4.42416 3
-3 -2 -20 -0.2338 2.46130 6
-3 -2 -20 4.62715 3.99277 3
-3 -2 -20 4.88888 3.84145 5
-3 -2 -20 2.29306 2.70472 3
3 2 20 11.9772 4.37865 6
3 2 20 4.41879 3.37016 6
3 2 20 0.62333 3.91417 3
-4 -2 -20 -0.5222 3.01072 6
-4 -2 -20 8.01945 3.61387 5
-4 -2 -20 2.16635 2.99306 3
4 2 20 -3.0608 4.54089 3
1 -3 -20 -0.6540 3.68153 5
1 -3 -20 3.33900 3.41443 6
1 -3 -20 -0.2602 4.11648 3
-1 3 20 4.42614 3.94738 3
0 -3 -20 42.4884 7.01500 6
0 -3 -20 50.6065 8.28661 3
0 -3 -20 47.0641 8.72403 5
0 3 20 50.1530 8.74707 3
0 3 20 52.9817 7.57354 6
-1 -3 -20 14.3880 5.03373 3
-1 -3 -20 16.4396 5.25324 6
-1 -3 -20 10.0472 4.54322 5
1 3 20 14.8262 5.86453 3
1 3 20 33.5428 5.98579 6
-2 -3 -20 10.0466 3.89517 6
-2 -3 -20 5.09100 3.73975 3
-2 -3 -20 0.59391 3.10433 5
2 3 20 7.52972 4.14331 6
2 3 20 6.85653 4.38438 3
-3 -3 -20 63.5032 10.2977 3
-3 -3 -20 61.3433 9.95208 5
-3 -3 -20 56.4101 8.74025 3
-3 -3 -20 75.0359 9.13365 6
3 3 20 69.7889 7.45101 6
3 3 20 72.3894 10.3661 3
-4 -3 -20 2.51647 3.74474 3
-4 -3 -20 0.66762 3.48256 5
4 3 20 -2.7439 4.77397 3
1 -4 -20 10.3029 5.08302 6
1 -4 -20 11.4103 6.50636 3
1 -4 -20 27.7999 6.82527 5
-1 4 20 9.46770 5.48473 3
-1 4 20 16.9194 5.51104 6
0 -4 -20 56.4523 7.93990 6
0 -4 -20 29.6483 6.93381 5
0 -4 -20 44.5967 8.11763 3
0 4 20 36.5752 8.39427 3
0 4 20 50.3107 7.68137 6
-1 -4 -20 48.8065 9.15107 3
-1 -4 -20 46.8333 8.67418 5
-1 -4 -20 59.7528 8.61971 6
1 4 20 64.0570 8.10982 6
1 4 20 52.4718 8.87489 3
-2 -4 -20 -2.1692 2.35697 6
-2 -4 -20 2.11199 3.28605 5
-2 -4 -20 1.75892 3.76203 3
2 4 20 1.90806 4.09337 3
2 4 20 1.92850 3.82974 6
-3 -4 -20 41.3457 7.49917 3
-3 -4 -20 48.0470 8.79482 6
3 4 20 57.0197 7.42598 6
3 4 20 52.8659 9.09292 3
3 4 20 48.9034 7.64021 4
-4 -4 -20 35.1360 7.28431 3
-4 -4 -20 18.5118 5.42049 5
4 4 20 14.2469 5.47404 3
1 -5 -20 3.44106 3.79876 6
1 -5 -20 7.41932 4.72990 3
-1 5 20 8.32847 4.65242 6
-1 5 20 1.78887 3.79556 3
0 -5 -20 105.051 12.5541 3
0 -5 -20 66.2897 10.8928 6
0 5 20 84.7711 10.1898 6
0 5 20 94.7390 11.7296 3
-1 -5 -20 4.10857 3.95893 6
-1 -5 -20 3.43807 3.76331 3
-1 -5 -20 -7.0395 3.18318 5
1 5 20 0.08437 3.78487 3
1 5 20 -1.1513 3.18061 6
-2 -5 -20 121.670 13.2536 3
2 5 20 137.910 11.7509 6
-3 -5 -20 27.3718 6.94630 5
-3 -5 -20 36.0224 7.93036 3
3 5 20 28.6960 6.64842 3
3 5 20 42.0452 7.04854 6
0 -6 -20 -0.3746 5.21762 5
0 -6 -20 0.96279 3.46753 6
0 -6 -20 1.91029 4.29807 3
0 6 20 5.44205 4.91154 3
-1 -6 -20 22.5931 6.70167 3
-1 -6 -20 30.6236 7.83478 5
-1 -6 -20 41.7225 7.69215 6
1 6 20 23.5159 5.82177 6
1 6 20 23.3085 7.18309 3
-2 -6 -20 -0.0216 3.35754 6
2 6 20 -0.2004 4.08306 6
2 6 20 -1.9503 4.09369 3
-3 -6 -20 26.7501 6.23418 6
-3 -6 -20 15.3718 5.33502 5
-3 -6 -20 20.2623 5.75213 3
3 6 20 10.3262 6.22163 3
3 6 20 10.8059 4.91775 6
-1 -7 -20 15.3284 6.01581 5
-1 -7 -20 27.4803 6.64899 6
1 7 20 15.2268 5.28224 6
1 7 20 17.3523 7.73544 3
-2 -7 -20 21.6178 6.65795 6
-2 -7 -20 15.5481 6.18397 5
-2 -7 -20 23.0810 6.74694 3
2 7 20 23.2925 7.19047 3
2 7 20 26.9595 6.58422 6
-1 3 -21 2.45674 4.19197 3
-1 3 -21 2.51381 3.42531 6
1 -3 21 10.5908 4.75660 3
1 -3 21 0.11997 3.11467 6
-2 3 -21 5.43845 4.14601 3
-2 3 -21 3.57147 4.19974 4
-2 3 -21 10.0944 4.79206 5
2 -3 21 6.06828 4.84076 3
0 2 -21 121.125 11.3946 6
0 2 -21 78.0946 9.74410 3
0 2 -21 118.200 11.2501 5
0 -2 21 118.440 12.6722 3
0 -2 21 117.696 10.2954 6
-1 2 -21 23.5490 5.43667 5
-1 2 -21 13.3360 5.21426 6
1 -2 21 16.6158 5.42129 3
1 -2 21 19.6052 4.97268 6
-2 2 -21 4.43155 4.16091 4
-2 2 -21 0.78859 4.47323 5
-2 2 -21 2.69411 2.98779 3
-2 2 -21 2.84052 3.59419 6
2 -2 21 -0.9014 3.19175 6
-3 2 -21 2.23052 3.50620 4
-3 2 -21 -2.4636 3.44819 5
3 -2 21 2.30075 4.26565 3
0 1 -21 39.9307 7.04918 6
0 1 -21 42.5415 7.25827 5
0 -1 21 37.9411 7.73190 3
0 -1 21 45.6879 7.02930 6
-1 1 -21 0.67867 3.60555 3
-1 1 -21 6.54807 3.50308 6
-1 1 -21 3.48037 3.16776 5
1 -1 21 6.05341 5.22881 3
-2 1 -21 2.22625 3.14447 6
-2 1 -21 6.21269 4.78827 3
2 -1 21 7.36317 5.59460 3
2 -1 21 3.15438 3.94767 6
-3 1 -21 115.414 11.3417 5
-3 1 -21 94.1503 9.95907 4
-3 1 -21 104.621 10.9281 3
3 -1 21 107.468 8.45391 6
3 -1 21 100.046 11.7444 3
0 0 -21 159.838 13.6044 3
0 0 -21 130.406 13.7913 6
0 0 -21 143.383 12.7105 5
0 0 21 153.149 11.9244 6
-1 0 -21 5.50268 3.66410 6
-1 0 -21 0.94545 3.24510 5
-1 0 -21 -1.3660 3.41104 3
1 0 21 6.84274 4.62429 3
1 0 21 5.29177 3.61335 6
-2 0 -21 2.82603 2.77524 6
2 0 21 1.86325 3.81769 3
2 0 21 3.06502 3.25818 6
-3 0 -21 48.4068 7.69502 6
-3 0 -21 41.7297 7.45121 3
-3 0 -21 44.9825 7.64989 5
3 0 21 45.0099 8.71139 3
3 0 21 42.2479 6.26326 6
0 -1 -21 14.5877 4.42961 5
0 -1 -21 24.9921 5.96337 3
0 1 21 5.66027 4.26149 3
-1 -1 -21 20.1087 5.51865 5
-1 -1 -21 25.5900 6.64680 3
1 1 21 24.1469 5.80138 6
1 1 21 25.2531 6.22759 3
-2 -1 -21 -5.1818 3.19133 6
2 1 21 1.21190 3.99762 3
2 1 21 0.07637 3.45248 6
-3 -1 -21 4.85623 4.41679 3
-3 -1 -21 6.70544 3.66796 6
-3 -1 -21 10.0328 4.65886 5
3 1 21 10.4133 3.96472 6
3 1 21 5.19507 5.07908 3
0 -2 -21 14.4162 5.38548 5
0 -2 -21 26.4185 6.60199 6
0 -2 -21 26.1861 6.82743 3
0 2 21 16.0867 5.12024 6
0 2 21 15.8965 5.68604 3
-1 -2 -21 21.4772 6.45460 6
-1 -2 -21 48.9587 9.12067 5
1 2 21 42.5818 7.83325 3
1 2 21 40.4561 7.16059 6
-2 -2 -21 5.57590 3.68629 6
2 2 21 1.09700 3.43816 6
2 2 21 1.60907 4.15680 3
-3 -2 -21 88.2923 9.68682 6
-3 -2 -21 64.2166 9.26071 5
-3 -2 -21 82.1032 10.1220 3
3 2 21 77.7905 7.87256 6
3 2 21 71.2430 10.5303 3
0 -3 -21 0.05140 3.62801 6
0 -3 -21 1.35708 5.20645 3
0 3 21 -2.3853 3.76209 3
0 3 21 -0.4023 3.73159 6
-1 -3 -21 7.69472 4.69624 6
-1 -3 -21 -0.9133 3.16566 3
1 3 21 -1.3740 2.99420 6
1 3 21 1.34188 4.05839 3
-2 -3 -21 73.0446 10.3932 5
-2 -3 -21 71.4772 9.74033 6
2 3 21 65.4431 8.49431 6
-3 -3 -21 6.35588 4.14148 6
-3 -3 -21 3.26707 3.59427 3
-3 -3 -21 8.59193 4.85234 5
3 3 21 2.02879 4.66552 3
3 3 21 3.01229 3.86107 6
0 -4 -21 -6.3322 4.23527 6
0 -4 -21 0.52174 3.94289 3
0 -4 -21 17.1101 5.66780 5
0 4 21 6.12190 4.60295 3
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-1 -4 -21 3.92611 4.02033 5
-1 -4 -21 -2.0283 2.63540 6
1 4 21 1.84972 4.24426 3
1 4 21 3.81445 4.11523 6
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-2 -4 -21 31.5264 6.77606 6
-2 -4 -21 21.8374 5.78100 5
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2 4 21 35.7099 8.07388 3
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-3 -4 -21 17.3622 6.09060 5
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3 4 21 2.09287 4.34843 6
3 4 21 3.20479 5.14542 3
-1 -5 -21 13.6786 5.58536 5
-1 -5 -21 14.9604 5.07268 6
1 5 21 20.3043 7.15835 3
1 5 21 11.3488 5.11680 6
-2 -5 -21 13.2037 5.22410 6
-2 -5 -21 11.1439 5.79672 5
-2 -5 -21 8.20812 5.01803 3
2 5 21 2.90500 4.66802 6
2 5 21 13.4256 6.87437 3
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 21725
_shelx_res_file
;
TITL m22282 : space group P1bar
m22282.res
created by SHELXL-2019/2 at 11:20:17 on 28-Jun-2023
CELL 0.71073 6.2568 11.7542 16.9162 85.329 79.534 87.785
ZERR 2 0.0005 0.0014 0.0019 0.003 0.004 0.003
LATT 1
SFAC C H N O
UNIT 54 72 4 10
TEMP -183
SIZE 0.30 0.21 0.04
REM COLR colourless
REM FORM plate
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds:
HTAB O1 O3
HTAB N1 O2
EQIV $1 x-1, y, z
HTAB C4 O1_$1
HTAB
REM Conformation-defining torsion angles:
RTAB tors O1 C1 C2 C3
RTAB tors C1 C2 C3 N1
RTAB tors C2 C3 N1 C4
RTAB tors O1 C1 C9 C10
RTAB tors O1 C1 C15 C16
RTAB tors O1 C1 C9' C10'
RTAB tors O1 C1 C15' C16'
FMAP 2
PLAN 20
WGHT 0.027400 0.778800
EXTI 0.010138
FVAR 0.91774 0.50318 1.52375 1.40123
O1 4 0.824216 0.322815 0.667700 11.00000 0.02309 0.01799 =
0.02311 -0.00464 -0.00998 -0.00367
H1O 2 0.780635 0.390744 0.683106 11.00000 0.03709
N1 3 0.288797 0.321800 0.839349 11.00000 0.01606 0.01553 =
0.01355 -0.00177 -0.00299 -0.00126
H1N 2 0.342727 0.402860 0.833072 11.00000 0.03950
C2 1 0.435062 0.305086 0.691685 11.00000 0.02109 0.01676 =
0.01491 -0.00256 -0.00487 0.00120
AFIX 23
H2A 2 0.415565 0.389099 0.691340 11.00000 -1.20000
H2B 2 0.312841 0.274844 0.670545 11.00000 -1.20000
AFIX 0
C3 1 0.431105 0.254913 0.777849 11.00000 0.02022 0.01918 =
0.01573 -0.00312 -0.00220 0.00439
AFIX 23
H3A 2 0.379240 0.175688 0.782916 11.00000 -1.20000
H3B 2 0.581117 0.251798 0.789138 11.00000 -1.20000
AFIX 0
C4 1 0.056972 0.330017 0.827096 11.00000 0.01707 0.01875 =
0.02286 -0.00350 -0.00629 -0.00185
AFIX 23
H4A 2 -0.000299 0.252326 0.828888 11.00000 -1.20000
H4B 2 0.049986 0.368697 0.773374 11.00000 -1.20000
AFIX 0
C5 1 -0.082424 0.396446 0.892007 11.00000 0.01857 0.01847 =
0.02811 -0.00062 0.00010 0.00080
AFIX 23
H5A 2 -0.235727 0.397598 0.884423 11.00000 -1.20000
H5B 2 -0.033901 0.476326 0.886619 11.00000 -1.20000
AFIX 0
C6 1 -0.067497 0.343503 0.976074 11.00000 0.03061 0.01811 =
0.02399 0.00084 0.00802 0.00120
AFIX 23
H6A 2 -0.153718 0.390390 1.017119 11.00000 -1.20000
H6B 2 -0.127707 0.265915 0.983520 11.00000 -1.20000
AFIX 0
C7 1 0.168557 0.337086 0.986652 11.00000 0.03700 0.01778 =
0.01367 0.00025 -0.00099 -0.00039
AFIX 23
H7A 2 0.224705 0.415231 0.983490 11.00000 -1.20000
H7B 2 0.179046 0.299809 1.040486 11.00000 -1.20000
AFIX 0
C8 1 0.305508 0.269969 0.921959 11.00000 0.02329 0.01828 =
0.01450 0.00086 -0.00426 -0.00080
AFIX 23
H8A 2 0.459291 0.268557 0.928976 11.00000 -1.20000
H8B 2 0.256145 0.190218 0.927814 11.00000 -1.20000
AFIX 0
SADI 0.020 C1 C9 C1 C9'
SADI 0.020 C1 C15 C1 C15'
C1 1 0.650918 0.275405 0.636728 11.00000 0.01774 0.01711 =
0.01551 -0.00281 -0.00453 -0.00386
SAME 0.010 C9' > C14'
DFIX 31.000 0.010 C15 C16 C16 C17 C17 C18 C18 C19 C19 C20 C20 C15
DFIX 31.000 0.010 C15' C16' C16' C17' C17' C18' C18' C19' C19' C20' C20' C15'
DFIX 31.633 0.020 C15 C17 C16 C18 C17 C19 C18 C20 C19 C15 C20 C16
DFIX 31.633 0.020 C15' C17' C16' C18' C17' C19' C18' C20' C19' C15' C20' C16'
DFIX 41.000 0.010 C9 C10 C10 C11 C11 C12 C12 C13 C13 C14 C14 C9
DFIX 41.000 0.010 C9' C10' C10' C11' C11' C12' C12' C13' C13' C14' C14' C9'
DFIX 41.732 0.020 C9 C11 C10 C12 C11 C13 C12 C14 C13 C9 C14 C10
DFIX 41.732 0.020 C9' C11' C10' C12' C11' C13' C12' C14' C13' C9' C14' C10'
EADP C9 C15'
EADP C10 C16'
EADP C11 C17'
EADP C12 C18'
EADP C13 C19'
EADP C14 C20'
EADP C9' C15
EADP C10' C16
EADP C11' C17
EADP C12' C18
EADP C13' C19
EADP C14' C20
PART 1
FLAT 0.010 C9 > C14
C9 1 0.691264 0.149737 0.635170 21.00000 0.01551 0.01618 =
0.01465 -0.00191 -0.00399 -0.00025
C10 1 0.906096 0.109135 0.630220 21.00000 0.01879 0.01938 =
0.02205 -0.00179 -0.00388 -0.00325
AFIX 43
H10 2 1.017442 0.161637 0.630723 21.00000 -1.20000
AFIX 0
C11 1 0.961115 -0.006627 0.624555 21.00000 0.02171 0.01684 =
0.02361 -0.00123 -0.00808 -0.00027
AFIX 43
H11 2 1.107859 -0.032621 0.621441 21.00000 -1.20000
AFIX 0
C12 1 0.795963 -0.084141 0.623529 21.00000 0.02375 0.01629 =
0.01977 -0.00171 -0.00314 0.00060
AFIX 43
H12 2 0.830948 -0.163027 0.619228 21.00000 -1.20000
AFIX 0
C13 1 0.580191 -0.044945 0.628847 21.00000 0.02104 0.02091 =
0.02466 -0.00452 -0.00692 -0.00086
AFIX 43
H13 2 0.468533 -0.097386 0.628653 21.00000 -1.20000
AFIX 0
C14 1 0.528603 0.071253 0.634447 21.00000 0.01344 0.01679 =
0.02428 -0.00429 0.00037 0.00064
AFIX 43
H14 2 0.381829 0.097303 0.637796 21.00000 -1.20000
AFIX 0
C15 1 0.639436 0.336406 0.551059 21.00000 0.01658 0.01288 =
0.01741 -0.00066 -0.00354 -0.00054
AFIX 13
H15 2 0.595441 0.417765 0.559790 21.00000 -1.20000
AFIX 0
C16 1 0.863241 0.338402 0.497779 21.00000 0.01583 0.01843 =
0.01773 -0.00421 -0.00271 -0.00197
AFIX 23
H16A 2 0.914545 0.259178 0.488027 21.00000 -1.20000
H16B 2 0.967116 0.373263 0.525847 21.00000 -1.20000
AFIX 0
C17 1 0.858017 0.405929 0.417405 21.00000 0.01773 0.01858 =
0.01923 -0.00046 0.00087 -0.00108
AFIX 23
H17A 2 0.818716 0.486717 0.426845 21.00000 -1.20000
H17B 2 1.004414 0.403480 0.383390 21.00000 -1.20000
AFIX 0
C18 1 0.695455 0.357868 0.373700 21.00000 0.02474 0.01926 =
0.01547 0.00127 -0.00243 0.00091
AFIX 23
H18A 2 0.740979 0.279132 0.360210 21.00000 -1.20000
H18B 2 0.690913 0.404932 0.322736 21.00000 -1.20000
AFIX 0
C19 1 0.471464 0.356911 0.425974 21.00000 0.02051 0.01791 =
0.01849 -0.00082 -0.00553 0.00105
AFIX 23
H19A 2 0.368218 0.321764 0.397780 21.00000 -1.20000
H19B 2 0.420477 0.436353 0.435100 21.00000 -1.20000
AFIX 0
C20 1 0.475069 0.290532 0.506459 21.00000 0.01671 0.02356 =
0.01729 -0.00193 -0.00328 -0.00284
AFIX 23
H20A 2 0.511136 0.209320 0.497424 21.00000 -1.20000
H20B 2 0.328551 0.294531 0.540256 21.00000 -1.20000
AFIX 0
PART 2
FLAT 0.010 C9' > C14'
C9' 1 0.661901 0.316378 0.548726 -21.00000 0.01658 0.01288 =
0.01741 -0.00066 -0.00354 -0.00054
C10' 1 0.851029 0.363501 0.502057 -21.00000 0.01583 0.01843 =
0.01773 -0.00421 -0.00271 -0.00197
AFIX 43
H10' 2 0.973969 0.372373 0.526510 -21.00000 -1.20000
AFIX 0
C11' 1 0.862170 0.397717 0.420138 -21.00000 0.01773 0.01858 =
0.01923 -0.00046 0.00087 -0.00108
AFIX 43
H11' 2 0.991624 0.429451 0.389556 -21.00000 -1.20000
AFIX 0
C12' 1 0.681743 0.384988 0.383440 -21.00000 0.02474 0.01926 =
0.01547 0.00127 -0.00243 0.00091
AFIX 43
H12' 2 0.688241 0.407963 0.327914 -21.00000 -1.20000
AFIX 0
C13' 1 0.491937 0.338185 0.429192 -21.00000 0.02051 0.01791 =
0.01849 -0.00082 -0.00553 0.00105
AFIX 43
H13' 2 0.369144 0.329390 0.404641 -21.00000 -1.20000
AFIX 0
C14' 1 0.482433 0.304276 0.511041 -21.00000 0.01671 0.02356 =
0.01729 -0.00193 -0.00328 -0.00284
AFIX 43
H14' 2 0.352773 0.272635 0.541527 -21.00000 -1.20000
AFIX 0
C15' 1 0.710005 0.142453 0.643155 -21.00000 0.01551 0.01618 =
0.01465 -0.00191 -0.00399 -0.00025
AFIX 13
H15' 2 0.730895 0.122954 0.699947 -21.00000 -1.20000
AFIX 0
C16' 1 0.529564 0.066499 0.629690 -21.00000 0.01879 0.01938 =
0.02205 -0.00179 -0.00388 -0.00325
AFIX 23
H16C 2 0.391453 0.087722 0.664630 -21.00000 -1.20000
H16D 2 0.509202 0.078531 0.572899 -21.00000 -1.20000
AFIX 0
C17' 1 0.585167 -0.058423 0.648715 -21.00000 0.02171 0.01684 =
0.02361 -0.00123 -0.00808 -0.00027
AFIX 23
H17C 2 0.467720 -0.106094 0.638287 -21.00000 -1.20000
H17D 2 0.594430 -0.071330 0.706574 -21.00000 -1.20000
AFIX 0
C18' 1 0.799909 -0.094655 0.598083 -21.00000 0.02375 0.01629 =
0.01977 -0.00171 -0.00314 0.00060
AFIX 23
H18C 2 0.838653 -0.173790 0.616098 -21.00000 -1.20000
H18D 2 0.783465 -0.093545 0.540911 -21.00000 -1.20000
AFIX 0
C19' 1 0.979373 -0.016853 0.605106 -21.00000 0.02104 0.02091 =
0.02466 -0.00452 -0.00692 -0.00086
AFIX 23
H19C 2 1.110868 -0.036668 0.566067 -21.00000 -1.20000
H19D 2 1.014763 -0.029729 0.659896 -21.00000 -1.20000
AFIX 0
C20' 1 0.921673 0.108407 0.589655 -21.00000 0.01344 0.01679 =
0.02428 -0.00429 0.00037 0.00064
AFIX 23
H20C 2 0.907689 0.124037 0.532398 -21.00000 -1.20000
H20D 2 1.040472 0.155317 0.599858 -21.00000 -1.20000
AFIX 0
PART 0
REM anion
O2 4 0.408089 0.537661 0.833708 11.00000 0.02529 0.01844 =
0.02428 -0.00107 -0.00218 -0.00736
O3 4 0.713575 0.522003 0.741977 11.00000 0.03239 0.02534 =
0.02352 -0.01030 0.00023 -0.00787
O4 4 1.054616 1.022087 0.858787 11.00000 0.03334 0.02728 =
0.10278 -0.01708 -0.01988 -0.00857
O5 4 0.721768 1.071630 0.903941 11.00000 0.04254 0.02136 =
0.09753 -0.02496 -0.01535 0.00287
N2 3 0.859067 1.003867 0.872716 11.00000 0.03366 0.01584 =
0.06392 -0.00705 -0.01711 -0.00196
C21 1 0.586876 0.573180 0.793419 11.00000 0.02402 0.01629 =
0.01463 0.00074 -0.00692 -0.00390
C22 1 0.654504 0.689611 0.811745 11.00000 0.02226 0.01512 =
0.01454 0.00216 -0.00646 -0.00393
C23 1 0.870596 0.721318 0.787792 11.00000 0.02194 0.01923 =
0.01580 -0.00054 -0.00235 -0.00262
AFIX 43
H23 2 0.972057 0.671709 0.757832 11.00000 -1.20000
AFIX 0
C24 1 0.938372 0.824657 0.807376 11.00000 0.02156 0.01949 =
0.02378 0.00340 -0.00705 -0.00569
AFIX 43
H24 2 1.085757 0.846162 0.791836 11.00000 -1.20000
AFIX 0
C25 1 0.786338 0.895624 0.850052 11.00000 0.02773 0.01181 =
0.03683 -0.00063 -0.01269 -0.00273
C26 1 0.569426 0.867972 0.873554 11.00000 0.02398 0.01608 =
0.04728 -0.00673 -0.00872 0.00394
AFIX 43
H26 2 0.467630 0.918967 0.901992 11.00000 -1.20000
AFIX 0
C27 1 0.505735 0.763429 0.854216 11.00000 0.01781 0.01816 =
0.03169 0.00002 -0.00684 -0.00093
AFIX 43
H27 2 0.358403 0.742036 0.870235 11.00000 -1.20000
AFIX 0
HKLF 4
REM m22282 : space group P1bar
REM wR2 = 0.1074, GooF = S = 1.114, Restrained GooF = 1.109 for all data
REM R1 = 0.0465 for 4825 Fo > 4sig(Fo) and 0.0555 for all 5590 data
REM 355 parameters refined using 68 restraints
END
WGHT 0.0274 0.7788
REM Instructions for potential hydrogen bonds
HTAB O1 O3
HTAB N1 O2
HTAB C4 O1_$1
REM Highest difference peak 0.303, deepest hole -0.193, 1-sigma level 0.042
Q1 1 0.6473 0.3025 0.5932 11.00000 0.05 0.30
Q2 1 0.6679 0.2060 0.6411 11.00000 0.05 0.29
Q3 1 0.6202 0.6371 0.8023 11.00000 0.05 0.28
Q4 1 0.8721 -0.0445 0.6064 11.00000 0.05 0.26
Q5 1 0.7672 0.6963 0.8131 11.00000 0.05 0.26
Q6 1 0.5439 0.2883 0.6632 11.00000 0.05 0.26
Q7 1 0.6629 0.8938 0.8410 11.00000 0.05 0.25
Q8 1 0.6193 0.1044 0.6387 11.00000 0.05 0.25
Q9 1 0.7744 0.3820 0.4021 11.00000 0.05 0.24
Q10 1 0.5609 0.3170 0.5284 11.00000 0.05 0.24
Q11 1 -0.0681 0.3651 0.9326 11.00000 0.05 0.23
Q12 1 0.0654 0.3464 0.9714 11.00000 0.05 0.22
Q13 1 0.4394 0.2871 0.7326 11.00000 0.05 0.22
Q14 1 0.2284 0.3017 0.9555 11.00000 0.05 0.21
Q15 1 0.6956 -0.0636 0.6230 11.00000 0.05 0.21
Q16 1 0.7468 0.7168 0.7845 11.00000 0.05 0.20
Q17 1 0.7808 1.0447 0.9344 11.00000 0.05 0.20
Q18 1 0.5906 0.7160 0.8391 11.00000 0.05 0.20
Q19 1 0.8481 0.8782 0.8109 11.00000 0.05 0.19
Q20 1 0.7708 1.0612 0.8690 11.00000 0.05 0.19
;
_shelx_res_checksum 29072
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.82422(17) 0.32282(9) 0.66770(6) 0.0204(2) Uani d 1 . .
H H1O 0.781(3) 0.3907(18) 0.6831(12) 0.037(5) Uiso d 1 . .
N N1 0.28880(18) 0.32180(10) 0.83935(7) 0.0149(2) Uani d 1 . .
H H1N 0.343(3) 0.4029(18) 0.8331(12) 0.040(5) Uiso d 1 . .
C C2 0.4351(2) 0.30509(12) 0.69168(8) 0.0173(3) Uani d 1 . .
H H2A 0.415565 0.389099 0.691340 0.021 Uiso calc 1 . .
H H2B 0.312841 0.274844 0.670545 0.021 Uiso calc 1 . .
C C3 0.4311(2) 0.25491(12) 0.77785(8) 0.0185(3) Uani d 1 . .
H H3A 0.379240 0.175688 0.782916 0.022 Uiso calc 1 . .
H H3B 0.581117 0.251798 0.789138 0.022 Uiso calc 1 . .
C C4 0.0570(2) 0.33002(12) 0.82710(9) 0.0191(3) Uani d 1 . .
H H4A -0.000299 0.252326 0.828888 0.023 Uiso calc 1 . .
H H4B 0.049986 0.368697 0.773374 0.023 Uiso calc 1 . .
C C5 -0.0824(2) 0.39645(12) 0.89201(9) 0.0223(3) Uani d 1 . .
H H5A -0.235727 0.397598 0.884423 0.027 Uiso calc 1 . .
H H5B -0.033901 0.476326 0.886619 0.027 Uiso calc 1 . .
C C6 -0.0675(3) 0.34350(13) 0.97607(9) 0.0260(3) Uani d 1 . .
H H6A -0.153718 0.390390 1.017119 0.031 Uiso calc 1 . .
H H6B -0.127707 0.265915 0.983520 0.031 Uiso calc 1 . .
C C7 0.1686(3) 0.33709(13) 0.98665(8) 0.0233(3) Uani d 1 . .
H H7A 0.224705 0.415231 0.983490 0.028 Uiso calc 1 . .
H H7B 0.179046 0.299809 1.040486 0.028 Uiso calc 1 . .
C C8 0.3055(2) 0.26997(12) 0.92196(8) 0.0187(3) Uani d 1 . .
H H8A 0.459291 0.268557 0.928976 0.022 Uiso calc 1 . .
H H8B 0.256145 0.190218 0.927814 0.022 Uiso calc 1 . .
C C1 0.6509(2) 0.27540(12) 0.63673(8) 0.0164(3) Uani d 1 . .
C C9 0.6913(11) 0.1497(8) 0.6352(4) 0.0153(7) Uani d 0.503(4) A 1
C C10 0.9061(5) 0.1091(3) 0.6302(2) 0.0200(6) Uani d 0.503(4) A 1
H H10 1.017442 0.161637 0.630723 0.024 Uiso calc 0.503(4) A 1
C C11 0.9611(8) -0.0066(3) 0.6246(3) 0.0202(8) Uani d 0.503(4) A 1
H H11 1.107859 -0.032621 0.621441 0.024 Uiso calc 0.503(4) A 1
C C12 0.7960(9) -0.0841(6) 0.6235(3) 0.0200(8) Uani d 0.503(4) A 1
H H12 0.830948 -0.163027 0.619228 0.024 Uiso calc 0.503(4) A 1
C C13 0.5802(7) -0.0449(4) 0.6288(3) 0.0217(8) Uani d 0.503(4) A 1
H H13 0.468533 -0.097386 0.628653 0.026 Uiso calc 0.503(4) A 1
C C14 0.5286(14) 0.0713(6) 0.6344(5) 0.0185(6) Uani d 0.503(4) A 1
H H14 0.381829 0.097303 0.637796 0.022 Uiso calc 0.503(4) A 1
C C15 0.639(2) 0.3364(10) 0.5511(7) 0.0156(12) Uani d 0.503(4) A 1
H H15 0.595441 0.417765 0.559790 0.019 Uiso calc 0.503(4) A 1
C C16 0.863(2) 0.3384(9) 0.4978(8) 0.0172(13) Uani d 0.503(4) A 1
H H16A 0.914545 0.259178 0.488027 0.021 Uiso calc 0.503(4) A 1
H H16B 0.967116 0.373263 0.525847 0.021 Uiso calc 0.503(4) A 1
C C17 0.858(2) 0.4059(9) 0.4174(7) 0.0191(5) Uani d 0.503(4) A 1
H H17A 0.818716 0.486717 0.426845 0.023 Uiso calc 0.503(4) A 1
H H17B 1.004414 0.403480 0.383390 0.023 Uiso calc 0.503(4) A 1
C C18 0.695(2) 0.3579(7) 0.3737(6) 0.0202(12) Uani d 0.503(4) A 1
H H18A 0.740979 0.279132 0.360210 0.024 Uiso calc 0.503(4) A 1
H H18B 0.690913 0.404932 0.322736 0.024 Uiso calc 0.503(4) A 1
C C19 0.471(2) 0.3569(10) 0.4260(8) 0.0188(12) Uani d 0.503(4) A 1
H H19A 0.368218 0.321764 0.397780 0.023 Uiso calc 0.503(4) A 1
H H19B 0.420477 0.436353 0.435100 0.023 Uiso calc 0.503(4) A 1
C C20 0.475(2) 0.2905(11) 0.5065(8) 0.0191(10) Uani d 0.503(4) A 1
H H20A 0.511136 0.209320 0.497424 0.023 Uiso calc 0.503(4) A 1
H H20B 0.328551 0.294531 0.540256 0.023 Uiso calc 0.503(4) A 1
C C9' 0.662(2) 0.3164(9) 0.5487(7) 0.0156(12) Uani d 0.497(4) A 2
C C10' 0.851(2) 0.3635(8) 0.5021(8) 0.0172(13) Uani d 0.497(4) A 2
H H10' 0.973969 0.372373 0.526510 0.021 Uiso calc 0.497(4) A 2
C C11' 0.862(2) 0.3977(9) 0.4201(7) 0.0191(5) Uani d 0.497(4) A 2
H H11' 0.991624 0.429451 0.389556 0.023 Uiso calc 0.497(4) A 2
C C12' 0.682(2) 0.3850(7) 0.3834(6) 0.0202(12) Uani d 0.497(4) A 2
H H12' 0.688241 0.407963 0.327914 0.024 Uiso calc 0.497(4) A 2
C C13' 0.492(2) 0.3382(10) 0.4292(8) 0.0188(12) Uani d 0.497(4) A 2
H H13' 0.369144 0.329390 0.404641 0.023 Uiso calc 0.497(4) A 2
C C14' 0.482(2) 0.3043(11) 0.5110(8) 0.0191(10) Uani d 0.497(4) A 2
H H14' 0.352773 0.272635 0.541527 0.023 Uiso calc 0.497(4) A 2
C C15' 0.7100(12) 0.1425(8) 0.6432(4) 0.0153(7) Uani d 0.497(4) A 2
H H15' 0.730895 0.122954 0.699947 0.018 Uiso calc 0.497(4) A 2
C C16' 0.5296(15) 0.0665(6) 0.6297(6) 0.0200(6) Uani d 0.497(4) A 2
H H16C 0.391453 0.087722 0.664630 0.024 Uiso calc 0.497(4) A 2
H H16D 0.509202 0.078531 0.572899 0.024 Uiso calc 0.497(4) A 2
C C17' 0.5852(7) -0.0584(4) 0.6487(3) 0.0202(8) Uani d 0.497(4) A 2
H H17C 0.467720 -0.106094 0.638287 0.024 Uiso calc 0.497(4) A 2
H H17D 0.594430 -0.071330 0.706574 0.024 Uiso calc 0.497(4) A 2
C C18' 0.7999(9) -0.0947(6) 0.5981(3) 0.0200(8) Uani d 0.497(4) A 2
H H18C 0.838653 -0.173790 0.616098 0.024 Uiso calc 0.497(4) A 2
H H18D 0.783465 -0.093545 0.540911 0.024 Uiso calc 0.497(4) A 2
C C19' 0.9794(8) -0.0169(4) 0.6051(4) 0.0217(8) Uani d 0.497(4) A 2
H H19C 1.110868 -0.036668 0.566067 0.026 Uiso calc 0.497(4) A 2
H H19D 1.014763 -0.029729 0.659896 0.026 Uiso calc 0.497(4) A 2
C C20' 0.9217(5) 0.1084(2) 0.5897(3) 0.0185(6) Uani d 0.497(4) A 2
H H20C 0.907689 0.124037 0.532398 0.022 Uiso calc 0.497(4) A 2
H H20D 1.040472 0.155317 0.599858 0.022 Uiso calc 0.497(4) A 2
O O2 0.40809(17) 0.53766(9) 0.83371(6) 0.0228(2) Uani d 1 . .
O O3 0.71358(18) 0.52200(9) 0.74198(6) 0.0271(3) Uani d 1 . .
O O4 1.0546(2) 1.02209(11) 0.85879(11) 0.0526(4) Uani d 1 . .
O O5 0.7218(2) 1.07163(11) 0.90394(11) 0.0524(4) Uani d 1 . .
N N2 0.8591(2) 1.00387(12) 0.87272(10) 0.0365(4) Uani d 1 . .
C C21 0.5869(2) 0.57318(12) 0.79342(8) 0.0179(3) Uani d 1 . .
C C22 0.6545(2) 0.68961(11) 0.81174(8) 0.0170(3) Uani d 1 . .
C C23 0.8706(2) 0.72132(12) 0.78779(8) 0.0191(3) Uani d 1 . .
H H23 0.972057 0.671709 0.757832 0.023 Uiso calc 1 . .
C C24 0.9384(2) 0.82466(12) 0.80738(9) 0.0214(3) Uani d 1 . .
H H24 1.085757 0.846162 0.791836 0.026 Uiso calc 1 . .
C C25 0.7863(3) 0.89562(12) 0.85005(10) 0.0246(3) Uani d 1 . .
C C26 0.5694(3) 0.86797(13) 0.87355(11) 0.0287(4) Uani d 1 . .
H H26 0.467630 0.918967 0.901992 0.034 Uiso calc 1 . .
C C27 0.5057(2) 0.76343(12) 0.85422(9) 0.0223(3) Uani d 1 . .
H H27 0.358403 0.742036 0.870235 0.027 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
O1 0.0231(5) 0.0180(5) 0.0231(5) -0.0037(4) -0.0100(4) -0.0046(4)
N1 0.0161(6) 0.0155(6) 0.0135(5) -0.0013(4) -0.0030(4) -0.0018(4)
C2 0.0211(7) 0.0168(7) 0.0149(6) 0.0012(5) -0.0049(5) -0.0026(5)
C3 0.0202(7) 0.0192(7) 0.0157(7) 0.0044(5) -0.0022(5) -0.0031(5)
C4 0.0171(7) 0.0188(7) 0.0229(7) -0.0018(5) -0.0063(5) -0.0035(5)
C5 0.0186(7) 0.0185(7) 0.0281(8) 0.0008(5) 0.0001(6) -0.0006(6)
C6 0.0306(8) 0.0181(7) 0.0240(8) 0.0012(6) 0.0080(6) 0.0008(6)
C7 0.0370(9) 0.0178(7) 0.0137(7) -0.0004(6) -0.0010(6) 0.0003(5)
C8 0.0233(7) 0.0183(7) 0.0145(6) -0.0008(5) -0.0043(5) 0.0009(5)
C1 0.0177(6) 0.0171(7) 0.0155(6) -0.0039(5) -0.0045(5) -0.0028(5)
C9 0.0155(11) 0.0162(11) 0.0147(12) -0.0003(9) -0.0040(9) -0.0019(9)
C10 0.0188(13) 0.0194(14) 0.0221(14) -0.0033(10) -0.0039(9) -0.0018(9)
C11 0.0217(15) 0.0168(13) 0.024(2) -0.0003(10) -0.0081(11) -0.0012(9)
C12 0.0237(9) 0.0163(13) 0.020(3) 0.0006(8) -0.0031(17) -0.0017(19)
C13 0.0210(15) 0.0209(14) 0.025(2) -0.0009(10) -0.0069(11) -0.0045(10)
C14 0.0134(12) 0.0168(13) 0.0243(15) 0.0006(9) 0.0004(9) -0.0043(9)
C15 0.017(2) 0.013(3) 0.0174(8) -0.001(2) -0.0035(11) -0.0007(16)
C16 0.0158(13) 0.018(4) 0.0177(12) -0.002(2) -0.0027(10) -0.004(2)
C17 0.0177(8) 0.0186(12) 0.0192(9) -0.0011(8) 0.0009(6) -0.0005(9)
C18 0.0247(15) 0.019(4) 0.015(2) 0.001(3) -0.0024(15) 0.001(2)
C19 0.0205(19) 0.018(3) 0.0185(10) 0.0010(18) -0.0055(11) -0.0008(18)
C20 0.0167(9) 0.024(2) 0.0173(13) -0.0028(13) -0.0033(8) -0.0019(15)
C9' 0.017(2) 0.013(3) 0.0174(8) -0.001(2) -0.0035(11) -0.0007(16)
C10' 0.0158(13) 0.018(4) 0.0177(12) -0.002(2) -0.0027(10) -0.004(2)
C11' 0.0177(8) 0.0186(12) 0.0192(9) -0.0011(8) 0.0009(6) -0.0005(9)
C12' 0.0247(15) 0.019(4) 0.015(2) 0.001(3) -0.0024(15) 0.001(2)
C13' 0.0205(19) 0.018(3) 0.0185(10) 0.0010(18) -0.0055(11) -0.0008(18)
C14' 0.0167(9) 0.024(2) 0.0173(13) -0.0028(13) -0.0033(8) -0.0019(15)
C15' 0.0155(11) 0.0162(11) 0.0147(12) -0.0003(9) -0.0040(9) -0.0019(9)
C16' 0.0188(13) 0.0194(14) 0.0221(14) -0.0033(10) -0.0039(9) -0.0018(9)
C17' 0.0217(15) 0.0168(13) 0.024(2) -0.0003(10) -0.0081(11) -0.0012(9)
C18' 0.0237(9) 0.0163(13) 0.020(3) 0.0006(8) -0.0031(17) -0.0017(19)
C19' 0.0210(15) 0.0209(14) 0.025(2) -0.0009(10) -0.0069(11) -0.0045(10)
C20' 0.0134(12) 0.0168(13) 0.0243(15) 0.0006(9) 0.0004(9) -0.0043(9)
O2 0.0253(5) 0.0184(5) 0.0243(5) -0.0074(4) -0.0022(4) -0.0011(4)
O3 0.0324(6) 0.0253(6) 0.0235(6) -0.0079(5) 0.0002(5) -0.0103(4)
O4 0.0333(7) 0.0273(7) 0.1028(13) -0.0086(6) -0.0199(8) -0.0171(7)
O5 0.0425(8) 0.0214(6) 0.0975(12) 0.0029(6) -0.0154(8) -0.0250(7)
N2 0.0337(8) 0.0158(7) 0.0639(11) -0.0020(6) -0.0171(7) -0.0070(7)
C21 0.0240(7) 0.0163(7) 0.0146(6) -0.0039(5) -0.0069(5) 0.0007(5)
C22 0.0223(7) 0.0151(6) 0.0145(6) -0.0039(5) -0.0065(5) 0.0022(5)
C23 0.0219(7) 0.0192(7) 0.0158(6) -0.0026(5) -0.0024(5) -0.0005(5)
C24 0.0216(7) 0.0195(7) 0.0238(7) -0.0057(6) -0.0071(6) 0.0034(6)
C25 0.0277(8) 0.0118(7) 0.0368(9) -0.0027(6) -0.0127(7) -0.0006(6)
C26 0.0240(8) 0.0161(7) 0.0473(10) 0.0039(6) -0.0087(7) -0.0067(7)
C27 0.0178(7) 0.0182(7) 0.0317(8) -0.0009(5) -0.0068(6) 0.0000(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
C1 O1 H1O . . 107.8(13) ?
C3 N1 C8 . . 109.22(10) ?
C3 N1 C4 . . 112.50(11) ?
C8 N1 C4 . . 111.30(11) ?
C3 N1 H1N . . 108.1(11) ?
C8 N1 H1N . . 109.2(11) ?
C4 N1 H1N . . 106.4(11) ?
C3 C2 C1 . . 111.20(11) ?
C3 C2 H2A . . 109.4 ?
C1 C2 H2A . . 109.4 ?
C3 C2 H2B . . 109.4 ?
C1 C2 H2B . . 109.4 ?
H2A C2 H2B . . 108.0 ?
N1 C3 C2 . . 113.20(11) ?
N1 C3 H3A . . 108.9 ?
C2 C3 H3A . . 108.9 ?
N1 C3 H3B . . 108.9 ?
C2 C3 H3B . . 108.9 ?
H3A C3 H3B . . 107.8 ?
N1 C4 C5 . . 110.64(11) ?
N1 C4 H4A . . 109.5 ?
C5 C4 H4A . . 109.5 ?
N1 C4 H4B . . 109.5 ?
C5 C4 H4B . . 109.5 ?
H4A C4 H4B . . 108.1 ?
C4 C5 C6 . . 111.42(12) ?
C4 C5 H5A . . 109.3 ?
C6 C5 H5A . . 109.3 ?
C4 C5 H5B . . 109.3 ?
C6 C5 H5B . . 109.3 ?
H5A C5 H5B . . 108.0 ?
C7 C6 C5 . . 109.47(12) ?
C7 C6 H6A . . 109.8 ?
C5 C6 H6A . . 109.8 ?
C7 C6 H6B . . 109.8 ?
C5 C6 H6B . . 109.8 ?
H6A C6 H6B . . 108.2 ?
C8 C7 C6 . . 110.62(12) ?
C8 C7 H7A . . 109.5 ?
C6 C7 H7A . . 109.5 ?
C8 C7 H7B . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 108.1 ?
N1 C8 C7 . . 111.18(11) ?
N1 C8 H8A . . 109.4 ?
C7 C8 H8A . . 109.4 ?
N1 C8 H8B . . 109.4 ?
C7 C8 H8B . . 109.4 ?
H8A C8 H8B . . 108.0 ?
O1 C1 C9 . . 108.1(3) ?
O1 C1 C9' . . 110.1(6) ?
O1 C1 C2 . . 108.07(11) ?
C9 C1 C2 . . 112.1(3) ?
C9' C1 C2 . . 114.3(5) ?
O1 C1 C15 . . 109.0(5) ?
C9 C1 C15 . . 113.1(5) ?
C2 C1 C15 . . 106.3(5) ?
O1 C1 C15' . . 102.0(3) ?
C9' C1 C15' . . 109.1(5) ?
C2 C1 C15' . . 112.5(3) ?
C10 C9 C14 . . 118.5(6) ?
C10 C9 C1 . . 117.6(5) ?
C14 C9 C1 . . 123.8(5) ?
C11 C10 C9 . . 121.7(5) ?
C11 C10 H10 . . 119.1 ?
C9 C10 H10 . . 119.1 ?
C10 C11 C12 . . 119.0(4) ?
C10 C11 H11 . . 120.5 ?
C12 C11 H11 . . 120.5 ?
C13 C12 C11 . . 119.9(5) ?
C13 C12 H12 . . 120.0 ?
C11 C12 H12 . . 120.0 ?
C14 C13 C12 . . 120.1(5) ?
C14 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
C13 C14 C9 . . 120.7(6) ?
C13 C14 H14 . . 119.7 ?
C9 C14 H14 . . 119.7 ?
C20 C15 C16 . . 109.9(6) ?
C20 C15 C1 . . 116.1(9) ?
C16 C15 C1 . . 110.7(8) ?
C20 C15 H15 . . 106.5 ?
C16 C15 H15 . . 106.5 ?
C1 C15 H15 . . 106.5 ?
C15 C16 C17 . . 111.3(6) ?
C15 C16 H16A . . 109.4 ?
C17 C16 H16A . . 109.4 ?
C15 C16 H16B . . 109.4 ?
C17 C16 H16B . . 109.4 ?
H16A C16 H16B . . 108.0 ?
C18 C17 C16 . . 111.1(6) ?
C18 C17 H17A . . 109.4 ?
C16 C17 H17A . . 109.4 ?
C18 C17 H17B . . 109.4 ?
C16 C17 H17B . . 109.4 ?
H17A C17 H17B . . 108.0 ?
C17 C18 C19 . . 110.3(6) ?
C17 C18 H18A . . 109.6 ?
C19 C18 H18A . . 109.6 ?
C17 C18 H18B . . 109.6 ?
C19 C18 H18B . . 109.6 ?
H18A C18 H18B . . 108.1 ?
C18 C19 C20 . . 111.0(6) ?
C18 C19 H19A . . 109.4 ?
C20 C19 H19A . . 109.4 ?
C18 C19 H19B . . 109.4 ?
C20 C19 H19B . . 109.4 ?
H19A C19 H19B . . 108.0 ?
C19 C20 C15 . . 112.1(7) ?
C19 C20 H20A . . 109.2 ?
C15 C20 H20A . . 109.2 ?
C19 C20 H20B . . 109.2 ?
C15 C20 H20B . . 109.2 ?
H20A C20 H20B . . 107.9 ?
C10' C9' C14' . . 118.1(7) ?
C10' C9' C1 . . 121.7(10) ?
C14' C9' C1 . . 120.1(10) ?
C11' C10' C9' . . 121.3(7) ?
C11' C10' H10' . . 119.3 ?
C9' C10' H10' . . 119.3 ?
C10' C11' C12' . . 119.8(7) ?
C10' C11' H11' . . 120.1 ?
C12' C11' H11' . . 120.1 ?
C13' C12' C11' . . 119.5(7) ?
C13' C12' H12' . . 120.2 ?
C11' C12' H12' . . 120.2 ?
C12' C13' C14' . . 120.2(7) ?
C12' C13' H13' . . 119.9 ?
C14' C13' H13' . . 119.9 ?
C13' C14' C9' . . 121.0(7) ?
C13' C14' H14' . . 119.5 ?
C9' C14' H14' . . 119.5 ?
C20' C15' C16' . . 109.0(6) ?
C20' C15' C1 . . 114.6(5) ?
C16' C15' C1 . . 114.1(5) ?
C20' C15' H15' . . 106.1 ?
C16' C15' H15' . . 106.1 ?
C1 C15' H15' . . 106.1 ?
C17' C16' C15' . . 110.7(6) ?
C17' C16' H16C . . 109.5 ?
C15' C16' H16C . . 109.5 ?
C17' C16' H16D . . 109.5 ?
C15' C16' H16D . . 109.5 ?
H16C C16' H16D . . 108.1 ?
C16' C17' C18' . . 111.6(5) ?
C16' C17' H17C . . 109.3 ?
C18' C17' H17C . . 109.3 ?
C16' C17' H17D . . 109.3 ?
C18' C17' H17D . . 109.3 ?
H17C C17' H17D . . 108.0 ?
C19' C18' C17' . . 111.4(4) ?
C19' C18' H18C . . 109.4 ?
C17' C18' H18C . . 109.4 ?
C19' C18' H18D . . 109.4 ?
C17' C18' H18D . . 109.4 ?
H18C C18' H18D . . 108.0 ?
C18' C19' C20' . . 113.1(4) ?
C18' C19' H19C . . 109.0 ?
C20' C19' H19C . . 109.0 ?
C18' C19' H19D . . 109.0 ?
C20' C19' H19D . . 109.0 ?
H19C C19' H19D . . 107.8 ?
C19' C20' C15' . . 111.7(4) ?
C19' C20' H20C . . 109.3 ?
C15' C20' H20C . . 109.3 ?
C19' C20' H20D . . 109.3 ?
C15' C20' H20D . . 109.3 ?
H20C C20' H20D . . 107.9 ?
O5 N2 O4 . . 123.33(14) ?
O5 N2 C25 . . 118.52(14) ?
O4 N2 C25 . . 118.15(14) ?
O3 C21 O2 . . 126.87(13) ?
O3 C21 C22 . . 117.08(12) ?
O2 C21 C22 . . 116.04(12) ?
C27 C22 C23 . . 119.55(13) ?
C27 C22 C21 . . 120.94(13) ?
C23 C22 C21 . . 119.48(13) ?
C24 C23 C22 . . 120.50(14) ?
C24 C23 H23 . . 119.8 ?
C22 C23 H23 . . 119.7 ?
C25 C24 C23 . . 118.38(14) ?
C25 C24 H24 . . 120.8 ?
C23 C24 H24 . . 120.8 ?
C24 C25 C26 . . 122.75(14) ?
C24 C25 N2 . . 118.45(14) ?
C26 C25 N2 . . 118.80(14) ?
C25 C26 C27 . . 117.89(15) ?
C25 C26 H26 . . 121.1 ?
C27 C26 H26 . . 121.1 ?
C26 C27 C22 . . 120.92(14) ?
C26 C27 H27 . . 119.5 ?
C22 C27 H27 . . 119.5 ?
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 C1 . 1.4358(16) ?
O1 H1O . 0.88(2) ?
N1 C3 . 1.4953(17) ?
N1 C8 . 1.4982(17) ?
N1 C4 . 1.5004(17) ?
N1 H1N . 1.01(2) ?
C2 C3 . 1.5235(18) ?
C2 C1 . 1.5396(19) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C5 . 1.522(2) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.522(2) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.518(2) ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.517(2) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C1 C9 . 1.490(9) ?
C1 C9' . 1.517(11) ?
C1 C15 . 1.576(11) ?
C1 C15' . 1.592(10) ?
C9 C10 . 1.399(7) ?
C9 C14 . 1.402(7) ?
C10 C11 . 1.397(5) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.407(6) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.399(6) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.398(6) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C15 C20 . 1.519(7) ?
C15 C16 . 1.521(7) ?
C15 H15 . 1.0000 ?
C16 C17 . 1.523(7) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 C18 . 1.512(7) ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C18 C19 . 1.515(7) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 C20 . 1.516(7) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C9' C10' . 1.404(7) ?
C9' C14' . 1.405(7) ?
C10' C11' . 1.401(6) ?
C10' H10' . 0.9500 ?
C11' C12' . 1.402(7) ?
C11' H11' . 0.9500 ?
C12' C13' . 1.400(7) ?
C12' H12' . 0.9500 ?
C13' C14' . 1.401(7) ?
C13' H13' . 0.9500 ?
C14' H14' . 0.9500 ?
C15' C20' . 1.522(7) ?
C15' C16' . 1.526(7) ?
C15' H15' . 1.0000 ?
C16' C17' . 1.518(7) ?
C16' H16C . 0.9900 ?
C16' H16D . 0.9900 ?
C17' C18' . 1.522(6) ?
C17' H17C . 0.9900 ?
C17' H17D . 0.9900 ?
C18' C19' . 1.502(6) ?
C18' H18C . 0.9900 ?
C18' H18D . 0.9900 ?
C19' C20' . 1.516(5) ?
C19' H19C . 0.9900 ?
C19' H19D . 0.9900 ?
C20' H20C . 0.9900 ?
C20' H20D . 0.9900 ?
O2 C21 . 1.2661(17) ?
O3 C21 . 1.2431(18) ?
O4 N2 . 1.227(2) ?
O5 N2 . 1.226(2) ?
N2 C25 . 1.4698(19) ?
C21 C22 . 1.5197(19) ?
C22 C27 . 1.390(2) ?
C22 C23 . 1.395(2) ?
C23 C24 . 1.386(2) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.382(2) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.387(2) ?
C26 C27 . 1.388(2) ?
C26 H26 . 0.9500 ?
C27 H27 . 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
O1 H1O O3 . 0.88(2) 1.90(2) 2.7527(15) 164.5(19) yes
N1 H1N O2 . 1.01(2) 1.65(2) 2.6618(15) 172.6(18) yes
C4 H4B O1 1_455 0.99 2.57 3.2972(17) 130 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
C8 N1 C3 C2 . . . . -176.78(11) ?
C4 N1 C3 C2 . . . . 59.11(15) ?
C1 C2 C3 N1 . . . . 152.29(11) ?
C3 N1 C4 C5 . . . . 178.76(11) ?
C8 N1 C4 C5 . . . . 55.81(14) ?
N1 C4 C5 C6 . . . . -56.25(16) ?
C4 C5 C6 C7 . . . . 56.67(16) ?
C5 C6 C7 C8 . . . . -56.90(16) ?
C3 N1 C8 C7 . . . . 178.38(12) ?
C4 N1 C8 C7 . . . . -56.81(15) ?
C6 C7 C8 N1 . . . . 57.53(15) ?
C3 C2 C1 O1 . . . . -60.52(14) ?
C3 C2 C1 C9 . . . . 58.5(3) ?
C3 C2 C1 C9' . . . . 176.5(5) ?
C3 C2 C1 C15 . . . . -177.4(5) ?
C3 C2 C1 C15' . . . . 51.3(3) ?
O1 C1 C9 C10 . . . . -25.0(5) ?
C2 C1 C9 C10 . . . . -144.1(3) ?
C15 C1 C9 C10 . . . . 95.7(7) ?
O1 C1 C9 C14 . . . . 158.2(4) ?
C2 C1 C9 C14 . . . . 39.1(5) ?
C15 C1 C9 C14 . . . . -81.1(7) ?
C14 C9 C10 C11 . . . . 0.1(3) ?
C1 C9 C10 C11 . . . . -176.9(5) ?
C9 C10 C11 C12 . . . . 0.2(2) ?
C10 C11 C12 C13 . . . . -0.5(5) ?
C11 C12 C13 C14 . . . . 0.6(6) ?
C12 C13 C14 C9 . . . . -0.3(7) ?
C10 C9 C14 C13 . . . . 0.0(6) ?
C1 C9 C14 C13 . . . . 176.7(6) ?
O1 C1 C15 C20 . . . . 175.6(5) ?
C9 C1 C15 C20 . . . . 55.4(8) ?
C2 C1 C15 C20 . . . . -68.1(6) ?
O1 C1 C15 C16 . . . . 49.4(7) ?
C9 C1 C15 C16 . . . . -70.9(7) ?
C2 C1 C15 C16 . . . . 165.6(5) ?
C20 C15 C16 C17 . . . . 55.2(7) ?
C1 C15 C16 C17 . . . . -175.1(8) ?
C15 C16 C17 C18 . . . . -57.1(6) ?
C16 C17 C18 C19 . . . . 57.1(7) ?
C17 C18 C19 C20 . . . . -56.3(8) ?
C18 C19 C20 C15 . . . . 56.1(8) ?
C16 C15 C20 C19 . . . . -55.1(7) ?
C1 C15 C20 C19 . . . . 178.3(8) ?
O1 C1 C9' C10' . . . . 17.5(8) ?
C2 C1 C9' C10' . . . . 139.3(6) ?
C15' C1 C9' C10' . . . . -93.7(7) ?
O1 C1 C9' C14' . . . . -164.6(5) ?
C2 C1 C9' C14' . . . . -42.8(7) ?
C15' C1 C9' C14' . . . . 84.1(7) ?
C14' C9' C10' C11' . . . . 0.0(3) ?
C1 C9' C10' C11' . . . . 177.9(8) ?
C9' C10' C11' C12' . . . . 0.0(3) ?
C10' C11' C12' C13' . . . . 0.0(6) ?
C11' C12' C13' C14' . . . . 0.0(8) ?
C12' C13' C14' C9' . . . . 0.0(8) ?
C10' C9' C14' C13' . . . . 0.0(6) ?
C1 C9' C14' C13' . . . . -177.9(9) ?
O1 C1 C15' C20' . . . . -64.7(6) ?
C9' C1 C15' C20' . . . . 51.8(8) ?
C2 C1 C15' C20' . . . . 179.7(4) ?
O1 C1 C15' C16' . . . . 168.6(4) ?
C9' C1 C15' C16' . . . . -74.9(7) ?
C2 C1 C15' C16' . . . . 53.1(5) ?
C20' C15' C16' C17' . . . . 58.7(7) ?
C1 C15' C16' C17' . . . . -171.8(5) ?
C15' C16' C17' C18' . . . . -57.6(7) ?
C16' C17' C18' C19' . . . . 53.0(6) ?
C17' C18' C19' C20' . . . . -51.2(6) ?
C18' C19' C20' C15' . . . . 54.0(6) ?
C16' C15' C20' C19' . . . . -56.6(6) ?
C1 C15' C20' C19' . . . . 174.1(5) ?
O3 C21 C22 C27 . . . . 165.70(13) ?
O2 C21 C22 C27 . . . . -15.63(19) ?
O3 C21 C22 C23 . . . . -16.34(19) ?
O2 C21 C22 C23 . . . . 162.33(13) ?
C27 C22 C23 C24 . . . . 1.2(2) ?
C21 C22 C23 C24 . . . . -176.75(13) ?
C22 C23 C24 C25 . . . . -0.9(2) ?
C23 C24 C25 C26 . . . . -0.4(2) ?
C23 C24 C25 N2 . . . . 178.42(14) ?
O5 N2 C25 C24 . . . . 173.37(16) ?
O4 N2 C25 C24 . . . . -6.1(2) ?
O5 N2 C25 C26 . . . . -7.8(2) ?
O4 N2 C25 C26 . . . . 172.74(17) ?
C24 C25 C26 C27 . . . . 1.2(2) ?
N2 C25 C26 C27 . . . . -177.59(15) ?
C25 C26 C27 C22 . . . . -0.8(2) ?
C23 C22 C27 C26 . . . . -0.4(2) ?
C21 C22 C27 C26 . . . . 177.57(14) ?
_cod_database_fobs_code 2022816