#------------------------------------------------------------------------------
#$Date: 2023-07-15 03:47:13 +0200 (Sat, 15 Jul 2023) $
#$Revision: 285218 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022817.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_2022817
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 H5 O -'
_chemical_formula_moiety         'C20 H32 N O +, C7 H5 O -'
_chemical_formula_sum            'C27 H37 N O4'
_chemical_formula_weight         439.57
_chemical_name_common
;
Trihexyphenidylium 4-hydroxybenzoate
;
_chemical_name_systematic
;
1-(3-Cyclohexyl-3-hydroxy-3-phenylpropyl)piperidin-1-ium 4-hydroxybenzoate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                90
_cell_angle_beta                 101.789(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.098(2)
_cell_length_b                   8.5314(5)
_cell_length_c                   12.3516(6)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.43
_cell_volume                     4652.0(4)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_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  0.0619
_diffrn_reflns_av_unetI/netI     2.4891
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5327
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         2.431
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.284
_refine_ls_extinction_coef       0.0030(5)
_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   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0332P)^2^+1.3379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                4543
_reflns_number_total             5327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2286sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2022817
_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   0.980
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_file
;
   6   0   0 2298.92 63.3570  -2
   6   0   0 2298.92 63.3570   1
  12   0   0 7266.52 364.980  -2
  12   0   0 7266.52 364.980   1
  14   0   0 4003.97 73.4493  -2
  14   0   0 4003.97 73.4493   1
  16   0   0 8850.49 445.499  -2
  16   0   0 8850.49 445.499   1
  18   0   0 1714.25 35.7145  -2
  18   0   0 1714.25 35.7145   1
  20   0   0 801.764 18.5264  -2
  20   0   0 801.764 18.5264   1
  22   0   0 1201.98 24.9817  -2
  22   0   0 1201.98 24.9817   1
  24   0   0 3499.76 66.1179  -2
  24   0   0 3499.76 66.1179   1
  26   0   0 638.873 16.2730  -2
  26   0   0 638.873 16.2730   1
  28   0   0 669.263 16.3487  -2
  28   0   0 669.263 16.3487   1
  30   0   0 150.684 6.35510  -2
  30   0   0 150.684 6.35510   1
  32   0   0 82.8513 5.23586  -2
  32   0   0 82.8513 5.23586   1
  34   0   0 1450.57 31.6162  -2
  34   0   0 1450.57 31.6162   1
  36   0   0 313.580 11.2920  -2
  36   0   0 313.580 11.2920   1
  38   0   0 29.4714 5.28769  -2
  38   0   0 29.4714 5.28769   1
  40   0   0 1401.34 39.3504  -2
  40   0   0 1401.34 39.3504   1
  42   0   0 1019.70 34.3829  -2
  42   0   0 1019.70 34.3829   1
  44   0   0 38.0295 6.75608  -2
  44   0   0 38.0295 6.75608   1
  46   0   0 76.9603 8.88383  -2
  46   0   0 76.9603 8.88383   1
  48   0   0 822.346 30.6522  -2
  48   0   0 822.346 30.6522   1
  50   0   0 166.742 12.2784  -2
  50   0   0 166.742 12.2784   1
  52   0   0 170.686 12.7463  -2
  52   0   0 170.686 12.7463   1
  54   0   0 9.97483 7.81655  -2
  54   0   0 9.97483 7.81655   1
  56   0   0 163.080 17.0367  -2
  56   0   0 163.080 17.0367   1
   1   1   0 396.149 9.20402  -2
   1   1   0 396.149 9.20402   1
   3   1   0 2913.42 176.472  -2
   3   1   0 2913.42 176.472   1
   5   1   0 7.02370 1.16878  -2
   5   1   0 7.02370 1.16878   1
   7   1   0 448.437 7.91548  -2
   7   1   0 448.437 7.91548   1
   9   1   0 5250.77 202.284  -2
   9   1   0 5250.77 202.284   1
  11   1   0 4938.48 89.2428  -2
  11   1   0 4938.48 89.2428   1
  13   1   0 1147.07 17.5786  -2
  13   1   0 1147.07 17.5786   1
  15   1   0 6925.66 152.555  -2
  15   1   0 6925.66 152.555   1
  17   1   0 3539.09 51.0657  -2
  17   1   0 3539.09 51.0657   1
  19   1   0 254.813 5.77364  -2
  19   1   0 254.813 5.77364   1
  21   1   0 769.225 13.7609  -2
  21   1   0 769.225 13.7609   1
  23   1   0 4476.65 62.8035  -2
  23   1   0 4476.65 62.8035   1
  25   1   0 280.013 6.40056  -2
  25   1   0 280.013 6.40056   1
  27   1   0 44.2442 2.60635  -2
  27   1   0 44.2442 2.60635   1
  29   1   0 1.55325 1.54448  -2
  29   1   0 1.55325 1.54448   1
  31   1   0 1.32294 1.82449  -2
  31   1   0 1.32294 1.82449   1
  33   1   0 494.926 11.0259  -2
  33   1   0 494.926 11.0259   1
  35   1   0 1.24315 1.93890  -2
  35   1   0 1.24315 1.93890   1
  37   1   0 350.768 9.26395  -2
  37   1   0 350.768 9.26395   1
  39   1   0 442.358 10.9728  -2
  39   1   0 442.358 10.9728   1
  41   1   0 453.966 13.9831  -2
  41   1   0 453.966 13.9831   1
  43   1   0 211.459 8.71488  -2
  43   1   0 211.459 8.71488   1
  45   1   0 326.345 11.1144  -2
  45   1   0 326.345 11.1144   1
  47   1   0 164.467 8.34027  -2
  47   1   0 164.467 8.34027   1
  49   1   0 20.2555 4.52067  -2
  49   1   0 20.2555 4.52067   1
  51   1   0 43.8212 5.74284  -2
  51   1   0 43.8212 5.74284   1
  53   1   0 116.233 8.54533  -2
  53   1   0 116.233 8.54533   1
  55   1   0 88.4627 8.48172  -2
  55   1   0 88.4627 8.48172   1
  57   1   0 219.419 14.0436  -2
  57   1   0 219.419 14.0436   1
   4   2   0 3192.25 69.1268  -2
   4   2   0 3192.25 69.1268   1
   6   2   0 361.688 10.1831  -2
   6   2   0 361.688 10.1831   1
   8   2   0 304.088 8.85185  -2
   8   2   0 304.088 8.85185   1
  10   2   0 294.129 7.65083  -2
  10   2   0 294.129 7.65083   1
  12   2   0 604.986 12.8780  -2
  12   2   0 604.986 12.8780   1
  14   2   0 190.118 5.70905  -2
  14   2   0 190.118 5.70905   1
  16   2   0 94.6319 3.47164  -2
  16   2   0 94.6319 3.47164   1
  18   2   0 3173.25 49.6216  -2
  18   2   0 3173.25 49.6216   1
  20   2   0 159.100 5.34376  -2
  20   2   0 159.100 5.34376   1
  22   2   0 1074.95 17.9276  -2
  22   2   0 1074.95 17.9276   1
  24   2   0 93.9630 3.79979  -2
  24   2   0 93.9630 3.79979   1
  26   2   0 1038.24 18.4258  -2
  26   2   0 1038.24 18.4258   1
  28   2   0 637.900 12.0842  -2
  28   2   0 637.900 12.0842   1
  30   2   0 -1.2182 1.64407  -2
  30   2   0 -1.2182 1.64407   1
  32   2   0 380.581 8.79974  -2
  32   2   0 380.581 8.79974   1
  34   2   0 174.752 5.63045  -2
  34   2   0 174.752 5.63045   1
  36   2   0 128.311 5.11742  -2
  36   2   0 128.311 5.11742   1
  38   2   0 5.11452 2.77455  -2
  38   2   0 5.11452 2.77455   1
  40   2   0 19.0259 3.64739  -2
  40   2   0 19.0259 3.64739   1
  42   2   0 335.790 11.5875  -2
  42   2   0 335.790 11.5875   1
  44   2   0 245.265 11.4137  -2
  44   2   0 245.265 11.4137   1
  46   2   0 419.590 15.7454  -2
  46   2   0 419.590 15.7454   1
  48   2   0 77.0596 7.70990  -2
  48   2   0 77.0596 7.70990   1
  50   2   0 8.08543 4.07039  -2
  50   2   0 8.08543 4.07039   1
  52   2   0 11.2752 5.09381  -2
  52   2   0 11.2752 5.09381   1
  54   2   0 127.320 11.2149  -2
  54   2   0 127.320 11.2149   1
  56   2   0 170.411 14.1013  -2
  56   2   0 170.411 14.1013   1
   1   3   0 2158.83 49.3766  -2
   1   3   0 2158.83 49.3766   1
   3   3   0 736.756 19.3919  -2
   3   3   0 736.756 19.3919   1
   5   3   0 1511.38 35.3049  -2
   5   3   0 1511.38 35.3049   1
   7   3   0 617.556 16.6790  -2
   7   3   0 617.556 16.6790   1
   9   3   0 25.0740 3.33561  -2
   9   3   0 25.0740 3.33561   1
  11   3   0 759.554 18.2715  -2
  11   3   0 759.554 18.2715   1
  13   3   0 21.9388 2.39972  -2
  13   3   0 21.9388 2.39972   1
  15   3   0 1137.95 22.9651  -2
  15   3   0 1137.95 22.9651   1
  17   3   0 367.167 12.1233  -2
  17   3   0 367.167 12.1233   1
  19   3   0 15.1600 2.39923  -2
  19   3   0 15.1600 2.39923   1
  21   3   0 79.0008 4.42047  -2
  21   3   0 79.0008 4.42047   1
  23   3   0 56.5164 3.40553  -2
  23   3   0 56.5164 3.40553   1
  25   3   0 11.9189 2.33313  -2
  25   3   0 11.9189 2.33313   1
  27   3   0 155.829 5.81157  -2
  27   3   0 155.829 5.81157   1
  29   3   0 77.1251 4.25019  -2
  29   3   0 77.1251 4.25019   1
  31   3   0 3.20234 2.16940  -2
  31   3   0 3.20234 2.16940   1
  33   3   0 54.1693 4.08950  -2
  33   3   0 54.1693 4.08950   1
  35   3   0 87.0724 5.15433  -2
  35   3   0 87.0724 5.15433   1
  37   3   0 5.77383 2.64201  -2
  37   3   0 5.77383 2.64201   1
  39   3   0 16.0394 3.24109  -2
  39   3   0 16.0394 3.24109   1
  41   3   0 26.9197 3.69077  -2
  41   3   0 26.9197 3.69077   1
  43   3   0 52.5054 5.78109  -2
  43   3   0 52.5054 5.78109   1
  45   3   0 217.340 10.9953  -2
  45   3   0 217.340 10.9953   1
  47   3   0 213.852 12.7930  -2
  47   3   0 213.852 12.7930   1
  49   3   0 135.217 9.67796  -2
  49   3   0 135.217 9.67796   1
  51   3   0 19.8477 6.62607  -2
  51   3   0 19.8477 6.62607   1
  53   3   0 50.3223 10.4945  -2
  53   3   0 50.3223 10.4945   1
  55   3   0 102.737 11.6060  -2
  55   3   0 102.737 11.6060   1
   0   4   0 -2.5937 3.37247  -2
   0   4   0 -2.5937 3.37247   1
   2   4   0 1810.16 40.3276  -2
   2   4   0 1810.16 40.3276   1
   4   4   0 316.715 11.2583  -2
   4   4   0 316.715 11.2583   1
   6   4   0 674.536 20.4021  -2
   6   4   0 674.536 20.4021   1
   8   4   0 865.448 24.6908  -2
   8   4   0 865.448 24.6908   1
  10   4   0 160.474 9.04313  -2
  10   4   0 160.474 9.04313   1
  12   4   0 -1.0513 3.29184  -2
  12   4   0 -1.0513 3.29184   1
  14   4   0 179.813 7.78991  -2
  14   4   0 179.813 7.78991   1
  16   4   0 187.411 8.08577  -2
  16   4   0 187.411 8.08577   1
  18   4   0 43.7807 3.49615  -2
  18   4   0 43.7807 3.49615   1
  20   4   0 2.10073 2.01794  -2
  20   4   0 2.10073 2.01794   1
  22   4   0 204.987 7.11248  -2
  22   4   0 204.987 7.11248   1
  24   4   0 203.465 7.98357  -2
  24   4   0 203.465 7.98357   1
  26   4   0 1.01334 2.06995  -2
  26   4   0 1.01334 2.06995   1
  28   4   0 40.3610 3.67358  -2
  28   4   0 40.3610 3.67358   1
  30   4   0 2.22177 2.18647  -2
  30   4   0 2.22177 2.18647   1
  32   4   0 258.409 9.56206  -2
  32   4   0 258.409 9.56206   1
  34   4   0 179.439 7.54415  -2
  34   4   0 179.439 7.54415   1
  36   4   0 33.2848 4.51122  -2
  36   4   0 33.2848 4.51122   1
  38   4   0 219.714 11.2094  -2
  38   4   0 219.714 11.2094   1
  40   4   0 18.0548 4.91185  -2
  40   4   0 18.0548 4.91185   1
  42   4   0 240.155 11.9760  -2
  42   4   0 240.155 11.9760   1
  44   4   0 6.60267 4.83229  -2
  44   4   0 6.60267 4.83229   1
  46   4   0 8.40323 4.92438  -2
  46   4   0 8.40323 4.92438   1
  48   4   0 30.0908 6.75596  -2
  48   4   0 30.0908 6.75596   1
  50   4   0 2.24963 6.39444  -2
  50   4   0 2.24963 6.39444   1
  52   4   0 22.3464 7.43096  -2
  52   4   0 22.3464 7.43096   1
   1   5   0 159.628 7.60540  -2
   1   5   0 159.628 7.60540   1
   3   5   0 111.426 6.42987  -2
   3   5   0 111.426 6.42987   1
   5   5   0 8.95354 3.46454  -2
   5   5   0 8.95354 3.46454   1
   7   5   0 307.805 12.9830  -2
   7   5   0 307.805 12.9830   1
   9   5   0 998.707 27.3008  -2
   9   5   0 998.707 27.3008   1
  11   5   0 120.372 7.09022  -2
  11   5   0 120.372 7.09022   1
  13   5   0 483.439 14.5958  -2
  13   5   0 483.439 14.5958   1
  15   5   0 2093.35 42.9277  -2
  15   5   0 2093.35 42.9277   1
  17   5   0 1293.23 28.7109  -2
  17   5   0 1293.23 28.7109   1
  19   5   0 422.387 13.2770  -2
  19   5   0 422.387 13.2770   1
  21   5   0 2.67141 2.50512  -2
  21   5   0 2.67141 2.50512   1
  23   5   0 307.617 10.0492  -2
  23   5   0 307.617 10.0492   1
  25   5   0 126.277 6.04295  -2
  25   5   0 126.277 6.04295   1
  27   5   0 521.760 14.5350  -2
  27   5   0 521.760 14.5350   1
  29   5   0 129.105 6.67408  -2
  29   5   0 129.105 6.67408   1
  31   5   0 417.462 13.8494  -2
  31   5   0 417.462 13.8494   1
  33   5   0 2725.25 64.3126  -2
  33   5   0 2725.25 64.3126   1
  35   5   0 905.748 22.3172  -2
  35   5   0 905.748 22.3172   1
  37   5   0 48.0337 7.00240  -2
  37   5   0 48.0337 7.00240   1
  39   5   0 346.949 16.2821  -2
  39   5   0 346.949 16.2821   1
  41   5   0 496.739 18.5870  -2
  41   5   0 496.739 18.5870   1
  43   5   0 31.2449 5.71779  -2
  43   5   0 31.2449 5.71779   1
  45   5   0 148.297 10.0760  -2
  45   5   0 148.297 10.0760   1
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   3   1  14 40.6858 24.7476   1
 -25   1  14 294.709 46.9084  -2
   5   1  14 294.709 46.9084   1
 -27   1  14 61.9320 28.0181  -2
   7   1  14 61.9320 28.0181   1
 -29   1  14 50.0903 24.5892  -2
   9   1  14 50.0903 24.5892   1
 -35   1  14 88.1256 35.3629  -2
  13   1  14 88.1256 35.3629   1
 -35   1  14 226.572 43.7689  -2
  15   1  14 226.572 43.7689   1
  17   1  14 -4.1543 17.4411   1
 -36   2  14 3.61186 5.74550   1
  14   2  14 -19.900 2000000  -2
 -34   2  14 -19.900 2000000   1
  12   2  14 3.55534 18.4732  -2
 -32   2  14 3.55534 18.4732   1
  10   2  14 16.4066 18.2284  -2
 -30   2  14 16.4066 18.2284   1
   8   2  14 137.990 23.6769  -2
 -28   2  14 137.990 23.6769   1
 -26   2  14 -1.4426 4.80940   1
   4   2  14 82.7378 9.09398  -2
 -24   2  14 82.7378 9.09398   1
   2   2  14 136.297 12.5175  -2
 -22   2  14 136.297 12.5175   1
   0   2  14 -11.706 14.0490  -2
 -20   2  14 -11.706 14.0490   1
 -18   2  14 6.21969 4.96149   1
  -4   2  14 3.96748 11.5500  -2
 -16   2  14 3.96748 11.5500   1
  -6   2  14 31.5872 10.1906  -2
 -14   2  14 31.5872 10.1906   1
  -8   2  14 50.3893 8.63610  -2
 -12   2  14 50.3893 8.63610   1
 -10   2  14 63.2228 8.78489  -2
 -10   2  14 63.2228 8.78489   1
 -12   2  14 52.9619 8.88885  -2
  -8   2  14 52.9619 8.88885   1
 -14   2  14 31.2673 20.7890  -2
  -6   2  14 31.2673 20.7890   1
  -4   2  14 0.11097 7.24216   1
 -18   2  14 61.3407 23.0006  -2
  -2   2  14 61.3407 23.0006   1
 -20   2  14 21.9993 14.3305  -2
   0   2  14 21.9993 14.3305   1
 -22   2  14 157.031 24.3902  -2
   2   2  14 157.031 24.3902   1
 -24   2  14 102.456 28.6769  -2
   4   2  14 102.456 28.6769   1
 -26   2  14 20.3853 20.4266  -2
   6   2  14 20.3853 20.4266   1
 -28   2  14 126.677 22.9682  -2
   8   2  14 126.677 22.9682   1
 -30   2  14 18.3410 25.4036  -2
  10   2  14 18.3410 25.4036   1
 -32   2  14 -6.2888 11.8218  -2
  12   2  14 -6.2888 11.8218   1
 -33   3  14 9.65162 4.50364   1
 -31   3  14 5.65341 3.45811   1
   9   3  14 -17.261 16.8534  -2
 -29   3  14 -17.261 16.8534   1
   7   3  14 5.70250 21.4615  -2
 -27   3  14 5.70250 21.4615   1
   5   3  14 27.2658 19.0588  -2
 -25   3  14 27.2658 19.0588   1
   3   3  14 252.515 30.7880  -2
 -23   3  14 252.515 30.7880   1
   1   3  14 166.839 12.8185  -2
 -21   3  14 166.839 12.8185   1
  -1   3  14 133.082 13.5418  -2
 -19   3  14 133.082 13.5418   1
  -3   3  14 111.877 22.3908  -2
 -17   3  14 111.877 22.3908   1
  -5   3  14 18.9375 17.3554  -2
 -15   3  14 18.9375 17.3554   1
  -7   3  14 29.8151 12.3745  -2
 -13   3  14 29.8151 12.3745   1
  -9   3  14 98.0724 12.6850  -2
 -11   3  14 98.0724 12.6850   1
 -11   3  14 75.3707 13.1089  -2
  -9   3  14 75.3707 13.1089   1
 -13   3  14 29.8346 13.6353  -2
  -7   3  14 29.8346 13.6353   1
 -15   3  14 20.8522 11.9179  -2
  -5   3  14 20.8522 11.9179   1
 -17   3  14 84.3539 10.1924  -2
  -3   3  14 84.3539 10.1924   1
 -19   3  14 129.967 14.4987  -2
  -1   3  14 129.967 14.4987   1
 -21   3  14 162.359 12.5357  -2
   1   3  14 162.359 12.5357   1
 -23   3  14 180.432 24.5263  -2
   3   3  14 180.432 24.5263   1
 -25   3  14 28.7884 17.3729  -2
   5   3  14 28.7884 17.3729   1
 -27   3  14 -5.8028 22.8999  -2
   7   3  14 -5.8028 22.8999   1
 -29   3  14 5.19127 19.5868  -2
   9   3  14 5.19127 19.5868   1
 -31   3  14 26.8067 11.0558  -2
  11   3  14 26.8067 11.0558   1
   8   4  14 111.965 31.4113  -2
 -28   4  14 111.965 31.4113   1
   4   4  14 30.0195 13.0573  -2
 -24   4  14 30.0195 13.0573   1
   2   4  14 67.7523 15.9514  -2
 -22   4  14 67.7523 15.9514   1
   0   4  14 619.811 52.8762  -2
 -20   4  14 619.811 52.8762   1
  -2   4  14 97.8809 16.9754  -2
 -18   4  14 97.8809 16.9754   1
  -4   4  14 17.6995 19.7781  -2
 -16   4  14 17.6995 19.7781   1
  -6   4  14 5.07446 18.4084  -2
 -14   4  14 5.07446 18.4084   1
  -8   4  14 11.4364 19.8703  -2
 -12   4  14 11.4364 19.8703   1
 -10   4  14 -22.426 18.1193  -2
 -10   4  14 -22.426 18.1193   1
 -12   4  14 61.6892 21.8050  -2
  -8   4  14 61.6892 21.8050   1
 -14   4  14 53.8000 24.9205  -2
  -8   4  14 53.8000 24.9205   1
 -16   4  14 15.3574 23.7029  -2
  -6   4  14 15.3574 23.7029   1
 -16   4  14 8.25663 23.8924  -2
  -4   4  14 8.25663 23.8924   1
 -18   4  14 115.800 8.58340  -2
  -2   4  14 115.800 8.58340   1
 -20   4  14 608.690 45.2098  -2
   0   4  14 608.690 45.2098   1
 -22   4  14 28.2954 18.7946  -2
   2   4  14 28.2954 18.7946   1
 -24   4  14 69.5383 20.9038  -2
   4   4  14 69.5383 20.9038   1
 -26   4  14 70.4104 29.5914  -2
   6   4  14 70.4104 29.5914   1
 -28   4  14 44.6842 28.4521  -2
   8   4  14 44.6842 28.4521   1
  -1   5  14 372.107 43.1793  -2
 -21   5  14 372.107 43.1793   1
  -1   5  14 290.787 43.2396  -2
 -19   5  14 290.787 43.2396   1
  -3   5  14 -19.947 21.6082  -2
 -17   5  14 -19.947 21.6082   1
  -5   5  14 14.6286 23.2496  -2
 -15   5  14 14.6286 23.2496   1
  -9   5  14 101.157 30.2530  -2
 -13   5  14 101.157 30.2530   1
  -7   5  14 42.8006 26.7401  -2
 -13   5  14 42.8006 26.7401   1
  -9   5  14 124.961 34.2991  -2
 -11   5  14 124.961 34.2991   1
 -11   5  14 206.627 37.1179  -2
 -11   5  14 206.627 37.1179   1
 -11   5  14 96.8659 30.7510  -2
  -9   5  14 96.8659 30.7510   1
 -13   5  14 9.87052 17.7439  -2
  -7   5  14 9.87052 17.7439   1
 -15   5  14 32.1317 18.8784  -2
  -5   5  14 32.1317 18.8784   1
 -17   5  14 12.3898 18.8692  -2
  -3   5  14 12.3898 18.8692   1
 -19   5  14 393.263 37.2942  -2
  -1   5  14 393.263 37.2942   1
   8   0  15 6.43792 11.0330  -2
 -30   0  15 6.43792 11.0330   1
   4   0  15 15.0438 15.4876  -2
 -26   0  15 15.0438 15.4876   1
   2   0  15 -12.986 12.7515  -2
 -24   0  15 -12.986 12.7515   1
  -4   0  15 28.3439 13.0617  -2
 -18   0  15 28.3439 13.0617   1
  -6   0  15 -7.4091 12.4843  -2
 -16   0  15 -7.4091 12.4843   1
 -12   0  15 3.75829 14.4639  -2
 -10   0  15 3.75829 14.4639   1
 -14   0  15 18.0908 13.3291  -2
  -8   0  15 18.0908 13.3291   1
 -22   0  15 0.03413 16.9896  -2
   0   0  15 0.03413 16.9896   1
 -24   0  15 -8.6058 17.0849  -2
   2   0  15 -8.6058 17.0849   1
 -30   0  15 29.3999 24.4400  -2
   8   0  15 29.3999 24.4400   1
   7   1  15 36.9248 14.7788  -2
 -29   1  15 36.9248 14.7788   1
   5   1  15 80.8129 16.7720  -2
 -27   1  15 80.8129 16.7720   1
   3   1  15 9.20396 9.83412  -2
 -25   1  15 9.20396 9.83412   1
   1   1  15 85.6466 13.5435  -2
 -23   1  15 85.6466 13.5435   1
  -1   1  15 80.5694 14.7650  -2
 -21   1  15 80.5694 14.7650   1
  -3   1  15 96.9843 15.1843  -2
 -19   1  15 96.9843 15.1843   1
  -5   1  15 136.960 18.4530  -2
 -17   1  15 136.960 18.4530   1
  -7   1  15 243.391 20.7761  -2
 -15   1  15 243.391 20.7761   1
  -9   1  15 32.1506 10.0720  -2
 -13   1  15 32.1506 10.0720   1
 -11   1  15 23.1428 10.1567  -2
 -11   1  15 23.1428 10.1567   1
 -13   1  15 10.7867 16.3605  -2
  -9   1  15 10.7867 16.3605   1
 -15   1  15 261.104 39.4527  -2
  -7   1  15 261.104 39.4527   1
 -17   1  15 162.700 15.9229  -2
  -5   1  15 162.700 15.9229   1
 -19   1  15 98.7435 19.0889  -2
  -3   1  15 98.7435 19.0889   1
 -21   1  15 56.2000 15.6990  -2
  -1   1  15 56.2000 15.6990   1
 -23   1  15 80.7660 18.6522  -2
   1   1  15 80.7660 18.6522   1
 -25   1  15 4.81785 22.4951  -2
   3   1  15 4.81785 22.4951   1
 -27   1  15 38.5547 24.3880  -2
   5   1  15 38.5547 24.3880   1
 -29   1  15 64.1320 18.1218  -2
   7   1  15 64.1320 18.1218   1
   6   2  15 9.97069 12.7742  -2
 -28   2  15 9.97069 12.7742   1
   4   2  15 -12.089 11.8101  -2
 -26   2  15 -12.089 11.8101   1
   0   2  15 133.256 25.6340  -2
 -22   2  15 133.256 25.6340   1
  -2   2  15 104.980 24.1412  -2
 -20   2  15 104.980 24.1412   1
  -4   2  15 73.5265 20.4527  -2
 -18   2  15 73.5265 20.4527   1
  -6   2  15 43.6317 9.97202  -2
 -16   2  15 43.6317 9.97202   1
  -8   2  15 115.678 11.9342  -2
 -14   2  15 115.678 11.9342   1
 -10   2  15 55.6567 14.7456  -2
 -12   2  15 55.6567 14.7456   1
 -12   2  15 41.2719 14.9932  -2
 -10   2  15 41.2719 14.9932   1
 -14   2  15 148.794 30.3437  -2
  -8   2  15 148.794 30.3437   1
 -16   2  15 74.2574 17.3860  -2
  -6   2  15 74.2574 17.3860   1
 -18   2  15 87.5862 18.2795  -2
  -4   2  15 87.5862 18.2795   1
 -20   2  15 111.639 20.5737  -2
  -2   2  15 111.639 20.5737   1
 -22   2  15 129.438 22.0861  -2
   0   2  15 129.438 22.0861   1
 -24   2  15 61.2311 26.8081  -2
   2   2  15 61.2311 26.8081   1
 -26   2  15 -15.257 18.3730  -2
   4   2  15 -15.257 18.3730   1
 -28   2  15 22.5484 16.6431  -2
   6   2  15 22.5484 16.6431   1
  -1   3  15 117.771 16.2734  -2
 -21   3  15 117.771 16.2734   1
  -3   3  15 28.2912 13.2815  -2
 -19   3  15 28.2912 13.2815   1
  -5   3  15 12.5476 12.9785  -2
 -17   3  15 12.5476 12.9785   1
  -7   3  15 22.2578 12.8481  -2
 -15   3  15 22.2578 12.8481   1
  -9   3  15 2.86589 11.5128  -2
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 -11   3  15 304.797 41.2896   1
 -13   3  15 15.8262 13.1189  -2
  -9   3  15 15.8262 13.1189   1
 -15   3  15 16.8639 13.3191  -2
  -7   3  15 16.8639 13.3191   1
 -17   3  15 20.1729 13.5179  -2
  -5   3  15 20.1729 13.5179   1
 -19   3  15 60.2856 16.1022  -2
  -3   3  15 60.2856 16.1022   1
 -21   3  15 114.660 20.3858  -2
  -1   3  15 114.660 20.3858   1
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 -14   0  16 91.5378 25.9057   1
 -12   0  16 134.304 30.0548  -2
 -12   0  16 134.304 30.0548   1
 -14   0  16 83.3232 25.2964  -2
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;
_shelx_hkl_checksum              14801
_shelx_res_file
;
TITL m22310 : space group C2/c
    m22310.res
    created by SHELXL-2019/2 at 11:20:31 on 28-Jun-2023
CELL  0.71073  45.0981   8.5314  12.3516   90.000  101.789   90.000
ZERR        8   0.0022   0.0005   0.0006    0.000    0.002    0.000
LATT  7
SYMM -X, Y, 1/2-Z
SFAC C H N O
UNIT 216 296 8 32
TEMP -183
SIZE 0.25 0.20 0.04
REM COLR colourless
REM FORM plate
MERG 0
L.S. 10
BOND $H
LIST 4
ACTA
CONF
REM Instructions for potential hydrogen bonds
HTAB O1 O2
HTAB N1 O3
HTAB C2 O2
EQIV $1 x, -y+1, z+1/2
HTAB C4 O1_$1
HTAB C7 O3
EQIV $2 x, -y, z-1/2
HTAB O4 O3_$2
HTAB C26 O3_$2
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
FMAP 2
PLAN 20
WGHT    0.033200    1.337900
EXTI    0.003026
BASF   0.47023
FVAR       0.45622
O1    4    0.645028    0.476570    0.231971    11.00000    0.02386    0.01894 =
         0.01493   -0.00126    0.00054   -0.00602
H1O   2    0.639424    0.394783    0.266964    11.00000    0.03673
N1    3    0.585097    0.607314    0.406240    11.00000    0.01507    0.01266 =
         0.01533    0.00085    0.00229    0.00006
H1N   2    0.583173    0.498566    0.395496    11.00000    0.02349
C1    1    0.660572    0.581901    0.315817    11.00000    0.01681    0.01776 =
         0.01523   -0.00228    0.00212   -0.00288
C2    1    0.640731    0.599243    0.403159    11.00000    0.01603    0.01822 =
         0.01522    0.00050    0.00222   -0.00160
AFIX  23
H2A   2    0.638047    0.495231    0.435376    11.00000   -1.20000
H2B   2    0.651117    0.668315    0.463538    11.00000   -1.20000
AFIX   0
C3    1    0.609764    0.667911    0.352894    11.00000    0.01773    0.01948 =
         0.01818    0.00458    0.00371   -0.00178
AFIX  23
H3A   2    0.610726    0.783437    0.360334    11.00000   -1.20000
H3B   2    0.604764    0.642710    0.272994    11.00000   -1.20000
AFIX   0
C4    1    0.591043    0.639237    0.527982    11.00000    0.02003    0.01747 =
         0.01289   -0.00136    0.00179   -0.00060
AFIX  23
H4A   2    0.592245    0.753753    0.541102    11.00000   -1.20000
H4B   2    0.610672    0.592309    0.563876    11.00000   -1.20000
AFIX   0
C5    1    0.565834    0.570249    0.577933    11.00000    0.02468    0.01567 =
         0.01555   -0.00111    0.00506   -0.00177
AFIX  23
H5A   2    0.569629    0.595026    0.657884    11.00000   -1.20000
H5B   2    0.565790    0.454786    0.569906    11.00000   -1.20000
AFIX   0
C6    1    0.534953    0.634939    0.521840    11.00000    0.01933    0.02467 =
         0.02203   -0.00445    0.00816    0.00025
AFIX  23
H6A   2    0.518871    0.581952    0.552046    11.00000   -1.20000
H6B   2    0.534062    0.748444    0.537538    11.00000   -1.20000
AFIX   0
C7    1    0.529482    0.609112    0.397284    11.00000    0.01610    0.01874 =
         0.02299   -0.00111    0.00278    0.00227
AFIX  23
H7A   2    0.527524    0.495443    0.381295    11.00000   -1.20000
H7B   2    0.510274    0.660366    0.361565    11.00000   -1.20000
AFIX   0
C8    1    0.555277    0.675515    0.349580    11.00000    0.01747    0.01828 =
         0.01801    0.00236    0.00091    0.00445
AFIX  23
H8A   2    0.551751    0.651862    0.269500    11.00000   -1.20000
H8B   2    0.555856    0.790859    0.358541    11.00000   -1.20000
AFIX   0
C9    1    0.663946    0.737930    0.258656    11.00000    0.01104    0.01874 =
         0.01894    0.00066    0.00372    0.00019
C10   1    0.658617    0.748437    0.143769    11.00000    0.01973    0.02190 =
         0.01973   -0.00091    0.00538   -0.00185
AFIX  43
H10   2    0.652558    0.657720    0.100257    11.00000   -1.20000
AFIX   0
C11   1    0.662051    0.889876    0.092031    11.00000    0.02423    0.03100 =
         0.01797    0.00533    0.00740    0.00013
AFIX  43
H11   2    0.658087    0.895399    0.013573    11.00000   -1.20000
AFIX   0
C12   1    0.671206    1.022719    0.154048    11.00000    0.02181    0.02362 =
         0.03141    0.00936    0.00900    0.00004
AFIX  43
H12   2    0.673865    1.118945    0.118511    11.00000   -1.20000
AFIX   0
C13   1    0.676465    1.014405    0.268274    11.00000    0.01903    0.01894 =
         0.02852   -0.00002    0.00477   -0.00158
AFIX  43
H13   2    0.682632    1.105283    0.311469    11.00000   -1.20000
AFIX   0
C14   1    0.672724    0.873222    0.319698    11.00000    0.01826    0.02084 =
         0.01875    0.00015    0.00423    0.00023
AFIX  43
H14   2    0.676227    0.868889    0.398139    11.00000   -1.20000
AFIX   0
C15   1    0.691585    0.507056    0.368175    11.00000    0.01812    0.01786 =
         0.01722    0.00053    0.00430   -0.00010
AFIX  13
H15   2    0.686969    0.402152    0.396860    11.00000   -1.20000
AFIX   0
C16   1    0.710807    0.475974    0.281970    11.00000    0.02445    0.03002 =
         0.01901    0.00074    0.00534    0.00561
AFIX  23
H16A  2    0.716442    0.577069    0.252371    11.00000   -1.20000
H16B  2    0.698755    0.415569    0.219800    11.00000   -1.20000
AFIX   0
C17   1    0.739573    0.384540    0.331561    11.00000    0.02505    0.03359 =
         0.02693    0.00056    0.00850    0.00924
AFIX  23
H17A  2    0.733941    0.278419    0.352781    11.00000   -1.20000
H17B  2    0.752121    0.372668    0.274999    11.00000   -1.20000
AFIX   0
C18   1    0.758065    0.466483    0.432708    11.00000    0.01851    0.03008 =
         0.03402    0.00308    0.00495    0.00351
AFIX  23
H18A  2    0.775308    0.398936    0.466766    11.00000   -1.20000
H18B  2    0.766361    0.565645    0.409679    11.00000   -1.20000
AFIX   0
C19   1    0.738802    0.501528    0.517299    11.00000    0.01986    0.02953 =
         0.02408   -0.00052   -0.00185    0.00073
AFIX  23
H19A  2    0.750942    0.561859    0.579318    11.00000   -1.20000
H19B  2    0.732701    0.401767    0.547398    11.00000   -1.20000
AFIX   0
C20   1    0.710558    0.594859    0.466375    11.00000    0.01810    0.02424 =
         0.01929   -0.00188    0.00090    0.00117
AFIX  23
H20A  2    0.716603    0.698106    0.441359    11.00000   -1.20000
H20B  2    0.698238    0.613178    0.522950    11.00000   -1.20000
AFIX   0
REM Anion
O2    4    0.617156    0.242253    0.335766    11.00000    0.02098    0.02041 =
         0.02515   -0.00286    0.00421   -0.00348
O3    4    0.572528    0.300065    0.376758    11.00000    0.02411    0.01468 =
         0.01715   -0.00177    0.00743    0.00048
O4    4    0.532728   -0.200041   -0.006359    11.00000    0.01867    0.01973 =
         0.02021   -0.00511    0.00284   -0.00093
H4O   2    0.545490   -0.226611   -0.042036    11.00000    0.04202
C21   1    0.589526    0.218662    0.326163    11.00000    0.02427    0.01136 =
         0.01456    0.00626    0.00471    0.00127
C22   1    0.574563    0.094578    0.247819    11.00000    0.01844    0.01177 =
         0.01364    0.00344    0.00384    0.00063
C23   1    0.543139    0.071629    0.224934    11.00000    0.02022    0.01302 =
         0.01747    0.00240    0.00711    0.00219
AFIX  43
H23   2    0.531016    0.126006    0.267150    11.00000   -1.20000
AFIX   0
C24   1    0.529465   -0.029416    0.141466    11.00000    0.01536    0.01588 =
         0.02012    0.00209    0.00463    0.00017
AFIX  43
H24   2    0.508153   -0.044621    0.127228    11.00000   -1.20000
AFIX   0
C25   1    0.547066   -0.108386    0.078697    11.00000    0.01937    0.01044 =
         0.01413    0.00253    0.00105   -0.00033
C26   1    0.578594   -0.091251    0.103263    11.00000    0.01908    0.01481 =
         0.01630    0.00148    0.00524    0.00368
AFIX  43
H26   2    0.590788   -0.148204    0.062676    11.00000   -1.20000
AFIX   0
C27   1    0.591848    0.009282    0.187114    11.00000    0.01704    0.01457 =
         0.01506    0.00404    0.00136    0.00077
AFIX  43
H27   2    0.613258    0.020403    0.203686    11.00000   -1.20000
AFIX   0
HKLF 5
REM  m22310 : space group C2/c
REM wR2 = 0.0900, GooF = S = 1.030, Restrained GooF = 1.030 for all data
REM R1 = 0.0414 for 4543 Fo > 4sig(Fo) and 0.0531 for all 5327 data
REM 303 parameters refined using 0 restraints
END
WGHT      0.0332      1.3380
REM Instructions for potential hydrogen bonds
HTAB O1 O2
HTAB N1 O3
HTAB C2 O2
HTAB C4 O1_$1
HTAB C7 O3
HTAB O4 O3_$2
HTAB C26 O3_$2
REM Highest difference peak  0.275,  deepest hole -0.284,  1-sigma level  0.049
Q1    1   0.6477  0.6028  0.3571  11.00000  0.05    0.27
Q2    1   0.5709  0.6457  0.3792  11.00000  0.05    0.26
Q3    1   0.5785  0.1802  0.2789  11.00000  0.05    0.25
Q4    1   0.5368 -0.0203  0.0819  11.00000  0.05    0.23
Q5    1   0.5808  0.5937  0.5604  11.00000  0.05    0.23
Q6    1   0.5850 -0.0794  0.1682  11.00000  0.05    0.22
Q7    1   0.6630  0.6636  0.2914  11.00000  0.05    0.22
Q8    1   0.5365  0.0472  0.1589  11.00000  0.05    0.21
Q9    1   0.5802  0.0982  0.1899  11.00000  0.05    0.20
Q10   1   0.5804  0.0852  0.2154  11.00000  0.05    0.20
Q11   1   0.5304  0.5995  0.4689  11.00000  0.05    0.19
Q12   1   0.7007  0.5090  0.3299  11.00000  0.05    0.19
Q13   1   0.5562  0.2689  0.3880  11.00000  0.05    0.19
Q14   1   0.7078  1.1181  0.2389  11.00000  0.05    0.18
Q15   1   0.5114 -0.2301 -0.0277  11.00000  0.05    0.18
Q16   1   0.5400 -0.0081  0.2172  11.00000  0.05    0.18
Q17   1   0.5627  0.0796  0.2473  11.00000  0.05    0.18
Q18   1   0.7751  0.5323  0.6654  11.00000  0.05    0.18
Q19   1   0.6524  0.6826  0.2836  11.00000  0.05    0.17
Q20   1   0.6547  0.3785  0.2084  11.00000  0.05    0.17
;
_shelx_res_checksum              81453
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.64503(3) 0.47657(16) 0.23197(10) 0.0197(3) Uani d 1 . .
H H1O 0.6394(5) 0.395(3) 0.267(2) 0.037(6) Uiso d 1 . .
N N1 0.58510(3) 0.60731(17) 0.40624(11) 0.0145(3) Uani d 1 . .
H H1N 0.5832(4) 0.499(3) 0.3955(17) 0.023(5) Uiso d 1 . .
C C1 0.66057(4) 0.5819(2) 0.31582(14) 0.0168(3) Uani d 1 . .
C C2 0.64073(3) 0.5992(2) 0.40316(14) 0.0166(3) Uani d 1 . .
H H2A 0.638047 0.495231 0.435376 0.020 Uiso calc 1 . .
H H2B 0.651117 0.668315 0.463538 0.020 Uiso calc 1 . .
C C3 0.60976(3) 0.6679(2) 0.35289(14) 0.0185(4) Uani d 1 . .
H H3A 0.610726 0.783437 0.360334 0.022 Uiso calc 1 . .
H H3B 0.604764 0.642710 0.272994 0.022 Uiso calc 1 . .
C C4 0.59104(4) 0.6392(2) 0.52798(13) 0.0170(4) Uani d 1 . .
H H4A 0.592245 0.753753 0.541102 0.020 Uiso calc 1 . .
H H4B 0.610672 0.592309 0.563876 0.020 Uiso calc 1 . .
C C5 0.56583(4) 0.5702(2) 0.57793(14) 0.0185(4) Uani d 1 . .
H H5A 0.569629 0.595026 0.657884 0.022 Uiso calc 1 . .
H H5B 0.565790 0.454786 0.569906 0.022 Uiso calc 1 . .
C C6 0.53495(4) 0.6349(2) 0.52184(14) 0.0215(4) Uani d 1 . .
H H6A 0.518871 0.581952 0.552046 0.026 Uiso calc 1 . .
H H6B 0.534062 0.748444 0.537538 0.026 Uiso calc 1 . .
C C7 0.52948(4) 0.6091(2) 0.39728(15) 0.0194(4) Uani d 1 . .
H H7A 0.527524 0.495443 0.381295 0.023 Uiso calc 1 . .
H H7B 0.510274 0.660366 0.361565 0.023 Uiso calc 1 . .
C C8 0.55528(3) 0.6755(2) 0.34958(14) 0.0183(4) Uani d 1 . .
H H8A 0.551751 0.651862 0.269500 0.022 Uiso calc 1 . .
H H8B 0.555856 0.790859 0.358541 0.022 Uiso calc 1 . .
C C9 0.66395(3) 0.7379(2) 0.25866(14) 0.0161(4) Uani d 1 . .
C C10 0.65862(4) 0.7484(2) 0.14377(15) 0.0203(4) Uani d 1 . .
H H10 0.652558 0.657720 0.100257 0.024 Uiso calc 1 . .
C C11 0.66205(4) 0.8899(2) 0.09203(16) 0.0240(4) Uani d 1 . .
H H11 0.658087 0.895399 0.013573 0.029 Uiso calc 1 . .
C C12 0.67121(4) 1.0227(2) 0.15405(16) 0.0251(4) Uani d 1 . .
H H12 0.673865 1.118945 0.118511 0.030 Uiso calc 1 . .
C C13 0.67646(4) 1.0144(2) 0.26827(16) 0.0222(4) Uani d 1 . .
H H13 0.682632 1.105283 0.311469 0.027 Uiso calc 1 . .
C C14 0.67272(4) 0.8732(2) 0.31970(15) 0.0192(4) Uani d 1 . .
H H14 0.676227 0.868889 0.398139 0.023 Uiso calc 1 . .
C C15 0.69159(4) 0.5071(2) 0.36817(14) 0.0176(4) Uani d 1 . .
H H15 0.686969 0.402152 0.396860 0.021 Uiso calc 1 . .
C C16 0.71081(4) 0.4760(2) 0.28197(16) 0.0244(4) Uani d 1 . .
H H16A 0.716442 0.577069 0.252371 0.029 Uiso calc 1 . .
H H16B 0.698755 0.415569 0.219800 0.029 Uiso calc 1 . .
C C17 0.73957(4) 0.3845(3) 0.33156(16) 0.0281(4) Uani d 1 . .
H H17A 0.733941 0.278419 0.352781 0.034 Uiso calc 1 . .
H H17B 0.752121 0.372668 0.274999 0.034 Uiso calc 1 . .
C C18 0.75806(4) 0.4665(3) 0.43271(17) 0.0276(4) Uani d 1 . .
H H18A 0.775308 0.398936 0.466766 0.033 Uiso calc 1 . .
H H18B 0.766361 0.565645 0.409679 0.033 Uiso calc 1 . .
C C19 0.73880(4) 0.5015(2) 0.51730(16) 0.0254(4) Uani d 1 . .
H H19A 0.750942 0.561859 0.579318 0.030 Uiso calc 1 . .
H H19B 0.732701 0.401767 0.547398 0.030 Uiso calc 1 . .
C C20 0.71056(4) 0.5949(2) 0.46637(15) 0.0210(4) Uani d 1 . .
H H20A 0.716603 0.698106 0.441359 0.025 Uiso calc 1 . .
H H20B 0.698238 0.613178 0.522950 0.025 Uiso calc 1 . .
O O2 0.61716(3) 0.24225(15) 0.33577(10) 0.0223(3) Uani d 1 . .
O O3 0.57253(2) 0.30007(14) 0.37676(10) 0.0182(3) Uani d 1 . .
O O4 0.53273(3) -0.20004(15) -0.00636(10) 0.0197(3) Uani d 1 . .
H H4O 0.5455(5) -0.227(3) -0.042(2) 0.042(7) Uiso d 1 . .
C C21 0.58953(4) 0.2187(2) 0.32616(14) 0.0166(3) Uani d 1 . .
C C22 0.57456(3) 0.0946(2) 0.24782(13) 0.0145(3) Uani d 1 . .
C C23 0.54314(4) 0.0716(2) 0.22493(14) 0.0164(3) Uani d 1 . .
H H23 0.531016 0.126006 0.267150 0.020 Uiso calc 1 . .
C C24 0.52947(4) -0.0294(2) 0.14147(15) 0.0170(4) Uani d 1 . .
H H24 0.508153 -0.044621 0.127228 0.020 Uiso calc 1 . .
C C25 0.54707(4) -0.10839(19) 0.07870(14) 0.0150(3) Uani d 1 . .
C C26 0.57859(4) -0.0913(2) 0.10326(14) 0.0165(3) Uani d 1 . .
H H26 0.590788 -0.148204 0.062676 0.020 Uiso calc 1 . .
C C27 0.59185(3) 0.0093(2) 0.18711(14) 0.0158(3) Uani d 1 . .
H H27 0.613258 0.020403 0.203686 0.019 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 0.0239(6) 0.0189(7) 0.0149(6) -0.0060(5) 0.0005(5) -0.0013(5)
N1 0.0151(6) 0.0127(8) 0.0153(7) 0.0001(5) 0.0023(5) 0.0009(6)
C1 0.0168(7) 0.0178(9) 0.0152(8) -0.0029(7) 0.0021(6) -0.0023(7)
C2 0.0160(8) 0.0182(9) 0.0152(8) -0.0016(7) 0.0022(6) 0.0005(7)
C3 0.0177(8) 0.0195(10) 0.0182(8) -0.0018(7) 0.0037(6) 0.0046(7)
C4 0.0200(8) 0.0175(9) 0.0129(8) -0.0006(7) 0.0018(6) -0.0014(7)
C5 0.0247(8) 0.0157(9) 0.0156(8) -0.0018(7) 0.0051(7) -0.0011(7)
C6 0.0193(8) 0.0247(10) 0.0220(9) 0.0003(7) 0.0082(7) -0.0045(8)
C7 0.0161(7) 0.0187(10) 0.0230(9) 0.0023(7) 0.0028(7) -0.0011(7)
C8 0.0175(8) 0.0183(9) 0.0180(8) 0.0045(7) 0.0009(7) 0.0024(7)
C9 0.0110(7) 0.0187(9) 0.0189(8) 0.0002(6) 0.0037(6) 0.0007(7)
C10 0.0197(8) 0.0219(10) 0.0197(9) -0.0018(7) 0.0054(7) -0.0009(8)
C11 0.0242(9) 0.0310(11) 0.0180(9) 0.0001(8) 0.0074(7) 0.0053(8)
C12 0.0218(8) 0.0236(11) 0.0314(11) 0.0000(7) 0.0090(8) 0.0094(8)
C13 0.0190(8) 0.0189(10) 0.0285(10) -0.0016(7) 0.0048(7) 0.0000(8)
C14 0.0183(8) 0.0208(10) 0.0188(9) 0.0002(7) 0.0042(7) 0.0002(7)
C15 0.0181(7) 0.0179(9) 0.0172(9) -0.0001(7) 0.0043(7) 0.0005(7)
C16 0.0245(9) 0.0300(11) 0.0190(9) 0.0056(8) 0.0053(7) 0.0007(8)
C17 0.0251(9) 0.0336(12) 0.0269(10) 0.0092(8) 0.0085(8) 0.0006(9)
C18 0.0185(8) 0.0301(12) 0.0340(11) 0.0035(7) 0.0049(8) 0.0031(9)
C19 0.0199(8) 0.0295(11) 0.0241(10) 0.0007(8) -0.0018(7) -0.0005(8)
C20 0.0181(8) 0.0242(10) 0.0193(9) 0.0012(7) 0.0009(7) -0.0019(7)
O2 0.0210(6) 0.0204(7) 0.0252(7) -0.0035(5) 0.0042(5) -0.0029(6)
O3 0.0241(6) 0.0147(6) 0.0172(6) 0.0005(5) 0.0074(5) -0.0018(5)
O4 0.0187(6) 0.0197(7) 0.0202(6) -0.0009(5) 0.0028(5) -0.0051(5)
C21 0.0243(8) 0.0114(9) 0.0146(8) 0.0013(7) 0.0047(7) 0.0063(7)
C22 0.0184(8) 0.0118(8) 0.0136(8) 0.0006(6) 0.0038(6) 0.0034(6)
C23 0.0202(8) 0.0130(9) 0.0175(8) 0.0022(7) 0.0071(7) 0.0024(7)
C24 0.0154(7) 0.0159(9) 0.0201(9) 0.0002(6) 0.0046(7) 0.0021(7)
C25 0.0194(8) 0.0104(8) 0.0141(8) -0.0003(6) 0.0010(6) 0.0025(6)
C26 0.0191(8) 0.0148(9) 0.0163(8) 0.0037(6) 0.0052(7) 0.0015(7)
C27 0.0170(7) 0.0146(9) 0.0151(8) 0.0008(7) 0.0014(7) 0.0040(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 . . 106.6(15) ?
C3 N1 C4 . . 112.50(13) ?
C3 N1 C8 . . 109.68(13) ?
C4 N1 C8 . . 110.94(13) ?
C3 N1 H1N . . 109.6(12) ?
C4 N1 H1N . . 108.3(13) ?
C8 N1 H1N . . 105.6(12) ?
O1 C1 C9 . . 106.91(13) ?
O1 C1 C2 . . 107.21(13) ?
C9 C1 C2 . . 111.47(14) ?
O1 C1 C15 . . 107.90(14) ?
C9 C1 C15 . . 112.59(13) ?
C2 C1 C15 . . 110.48(14) ?
C3 C2 C1 . . 111.46(14) ?
C3 C2 H2A . . 109.3 ?
C1 C2 H2A . . 109.3 ?
C3 C2 H2B . . 109.3 ?
C1 C2 H2B . . 109.3 ?
H2A C2 H2B . . 108.0 ?
N1 C3 C2 . . 112.92(14) ?
N1 C3 H3A . . 109.0 ?
C2 C3 H3A . . 109.0 ?
N1 C3 H3B . . 109.0 ?
C2 C3 H3B . . 109.0 ?
H3A C3 H3B . . 107.8 ?
N1 C4 C5 . . 110.01(13) ?
N1 C4 H4A . . 109.7 ?
C5 C4 H4A . . 109.7 ?
N1 C4 H4B . . 109.7 ?
C5 C4 H4B . . 109.7 ?
H4A C4 H4B . . 108.2 ?
C4 C5 C6 . . 111.40(14) ?
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 . . 110.52(14) ?
C7 C6 H6A . . 109.5 ?
C5 C6 H6A . . 109.5 ?
C7 C6 H6B . . 109.5 ?
C5 C6 H6B . . 109.5 ?
H6A C6 H6B . . 108.1 ?
C8 C7 C6 . . 111.06(14) ?
C8 C7 H7A . . 109.4 ?
C6 C7 H7A . . 109.4 ?
C8 C7 H7B . . 109.4 ?
C6 C7 H7B . . 109.4 ?
H7A C7 H7B . . 108.0 ?
N1 C8 C7 . . 111.06(14) ?
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 ?
C14 C9 C10 . . 118.00(16) ?
C14 C9 C1 . . 121.08(15) ?
C10 C9 C1 . . 120.92(16) ?
C11 C10 C9 . . 120.83(17) ?
C11 C10 H10 . . 119.6 ?
C9 C10 H10 . . 119.6 ?
C12 C11 C10 . . 120.39(17) ?
C12 C11 H11 . . 119.8 ?
C10 C11 H11 . . 119.8 ?
C11 C12 C13 . . 119.49(18) ?
C11 C12 H12 . . 120.3 ?
C13 C12 H12 . . 120.3 ?
C12 C13 C14 . . 119.97(18) ?
C12 C13 H13 . . 120.0 ?
C14 C13 H13 . . 120.0 ?
C13 C14 C9 . . 121.31(16) ?
C13 C14 H14 . . 119.3 ?
C9 C14 H14 . . 119.3 ?
C16 C15 C20 . . 109.43(14) ?
C16 C15 C1 . . 111.85(14) ?
C20 C15 C1 . . 116.04(15) ?
C16 C15 H15 . . 106.3 ?
C20 C15 H15 . . 106.3 ?
C1 C15 H15 . . 106.3 ?
C15 C16 C17 . . 111.40(15) ?
C15 C16 H16A . . 109.3 ?
C17 C16 H16A . . 109.3 ?
C15 C16 H16B . . 109.3 ?
C17 C16 H16B . . 109.3 ?
H16A C16 H16B . . 108.0 ?
C18 C17 C16 . . 111.82(17) ?
C18 C17 H17A . . 109.3 ?
C16 C17 H17A . . 109.3 ?
C18 C17 H17B . . 109.3 ?
C16 C17 H17B . . 109.3 ?
H17A C17 H17B . . 107.9 ?
C19 C18 C17 . . 111.13(14) ?
C19 C18 H18A . . 109.4 ?
C17 C18 H18A . . 109.4 ?
C19 C18 H18B . . 109.4 ?
C17 C18 H18B . . 109.4 ?
H18A C18 H18B . . 108.0 ?
C18 C19 C20 . . 111.47(16) ?
C18 C19 H19A . . 109.3 ?
C20 C19 H19A . . 109.3 ?
C18 C19 H19B . . 109.3 ?
C20 C19 H19B . . 109.3 ?
H19A C19 H19B . . 108.0 ?
C19 C20 C15 . . 110.86(15) ?
C19 C20 H20A . . 109.5 ?
C15 C20 H20A . . 109.5 ?
C19 C20 H20B . . 109.5 ?
C15 C20 H20B . . 109.5 ?
H20A C20 H20B . . 108.1 ?
C25 O4 H4O . . 107.3(17) ?
O2 C21 O3 . . 123.43(16) ?
O2 C21 C22 . . 119.08(15) ?
O3 C21 C22 . . 117.42(14) ?
C27 C22 C23 . . 118.22(15) ?
C27 C22 C21 . . 119.29(14) ?
C23 C22 C21 . . 122.17(15) ?
C24 C23 C22 . . 120.95(15) ?
C24 C23 H23 . . 119.5 ?
C22 C23 H23 . . 119.5 ?
C23 C24 C25 . . 119.81(15) ?
C23 C24 H24 . . 120.1 ?
C25 C24 H24 . . 120.1 ?
O4 C25 C24 . . 118.21(14) ?
O4 C25 C26 . . 121.89(15) ?
C24 C25 C26 . . 119.90(15) ?
C27 C26 C25 . . 119.45(16) ?
C27 C26 H26 . . 120.3 ?
C25 C26 H26 . . 120.3 ?
C26 C27 C22 . . 121.58(15) ?
C26 C27 H27 . . 119.2 ?
C22 C27 H27 . . 119.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . 1.440(2) ?
O1 H1O . 0.88(3) ?
N1 C3 . 1.496(2) ?
N1 C4 . 1.497(2) ?
N1 C8 . 1.501(2) ?
N1 H1N . 0.94(2) ?
C1 C9 . 1.529(2) ?
C1 C2 . 1.543(2) ?
C1 C15 . 1.553(2) ?
C2 C3 . 1.525(2) ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C5 . 1.519(2) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.526(2) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 C7 . 1.524(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 ?
C9 C14 . 1.391(2) ?
C9 C10 . 1.393(2) ?
C10 C11 . 1.389(3) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.383(3) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.384(3) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.388(3) ?
C13 H13 . 0.9500 ?
C14 H14 . 0.9500 ?
C15 C16 . 1.527(2) ?
C15 C20 . 1.530(2) ?
C15 H15 . 1.0000 ?
C16 C17 . 1.530(2) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C17 C18 . 1.523(3) ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C18 C19 . 1.519(3) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 C20 . 1.525(2) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
O2 C21 . 1.244(2) ?
O3 C21 . 1.287(2) ?
O4 C25 . 1.362(2) ?
O4 H4O . 0.82(2) ?
C21 C22 . 1.499(2) ?
C22 C27 . 1.392(2) ?
C22 C23 . 1.401(2) ?
C23 C24 . 1.388(2) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.392(2) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.400(2) ?
C26 C27 . 1.383(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 O2 . 0.88(3) 1.94(3) 2.8068(18) 165(2) yes
N1 H1N O3 . 0.94(2) 1.76(2) 2.6908(19) 169.4(17) yes
C2 H2A O2 . 0.99 2.57 3.277(2) 129 yes
C4 H4B O1 6_566 0.99 2.40 3.278(2) 148 yes
C7 H7A O3 . 0.99 2.64 3.314(2) 126 yes
O4 H4O O3 6 0.82(2) 1.84(3) 2.6633(18) 176(3) yes
C26 H26 O3 6 0.95 2.62 3.281(2) 127 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
O1 C1 C2 C3 . . . . -60.92(18) ?
C9 C1 C2 C3 . . . . 55.77(18) ?
C15 C1 C2 C3 . . . . -178.26(14) ?
C4 N1 C3 C2 . . . . 58.13(19) ?
C8 N1 C3 C2 . . . . -177.89(14) ?
C1 C2 C3 N1 . . . . 147.37(15) ?
C3 N1 C4 C5 . . . . -178.06(14) ?
C8 N1 C4 C5 . . . . 58.66(18) ?
N1 C4 C5 C6 . . . . -57.16(18) ?
C4 C5 C6 C7 . . . . 54.9(2) ?
C5 C6 C7 C8 . . . . -53.8(2) ?
C3 N1 C8 C7 . . . . 176.68(14) ?
C4 N1 C8 C7 . . . . -58.44(18) ?
C6 C7 C8 N1 . . . . 55.9(2) ?
O1 C1 C9 C14 . . . . 167.46(14) ?
C2 C1 C9 C14 . . . . 50.6(2) ?
C15 C1 C9 C14 . . . . -74.2(2) ?
O1 C1 C9 C10 . . . . -13.2(2) ?
C2 C1 C9 C10 . . . . -130.08(16) ?
C15 C1 C9 C10 . . . . 105.11(17) ?
C14 C9 C10 C11 . . . . 0.1(2) ?
C1 C9 C10 C11 . . . . -179.21(15) ?
C9 C10 C11 C12 . . . . 0.8(3) ?
C10 C11 C12 C13 . . . . -1.0(3) ?
C11 C12 C13 C14 . . . . 0.4(3) ?
C12 C13 C14 C9 . . . . 0.5(3) ?
C10 C9 C14 C13 . . . . -0.8(2) ?
C1 C9 C14 C13 . . . . 178.57(15) ?
O1 C1 C15 C16 . . . . 58.47(19) ?
C9 C1 C15 C16 . . . . -59.3(2) ?
C2 C1 C15 C16 . . . . 175.39(15) ?
O1 C1 C15 C20 . . . . -175.03(14) ?
C9 C1 C15 C20 . . . . 67.2(2) ?
C2 C1 C15 C20 . . . . -58.1(2) ?
C20 C15 C16 C17 . . . . 56.8(2) ?
C1 C15 C16 C17 . . . . -173.14(16) ?
C15 C16 C17 C18 . . . . -55.2(2) ?
C16 C17 C18 C19 . . . . 53.4(2) ?
C17 C18 C19 C20 . . . . -54.7(2) ?
C18 C19 C20 C15 . . . . 57.6(2) ?
C16 C15 C20 C19 . . . . -58.0(2) ?
C1 C15 C20 C19 . . . . 174.29(16) ?
O2 C21 C22 C27 . . . . -0.4(2) ?
O3 C21 C22 C27 . . . . 176.72(15) ?
O2 C21 C22 C23 . . . . -173.83(16) ?
O3 C21 C22 C23 . . . . 3.3(2) ?
C27 C22 C23 C24 . . . . -2.1(2) ?
C21 C22 C23 C24 . . . . 171.35(16) ?
C22 C23 C24 C25 . . . . -0.6(3) ?
C23 C24 C25 O4 . . . . -176.52(15) ?
C23 C24 C25 C26 . . . . 2.9(3) ?
O4 C25 C26 C27 . . . . 176.85(15) ?
C24 C25 C26 C27 . . . . -2.6(2) ?
C25 C26 C27 C22 . . . . -0.2(3) ?
C23 C22 C27 C26 . . . . 2.5(3) ?
C21 C22 C27 C26 . . . . -171.18(15) ?

_cod_database_fobs_code 2022817