#------------------------------------------------------------------------------
#$Date: 2023-05-06 11:45:32 +0100 (Sat, 06 May 2023) $
#$Revision: 283580 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/42/2244224.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_2244224
loop_
_publ_author_name
'Herbig, Marcus'
'Böhme, Uwe'
_publ_section_title
;
 Two polymorphs of
 <i>N</i>,<i>N</i>'-diphenyl-2-[1-(propyl-amino)-ethyl-idene]propanedi-amide.
;
_journal_coeditor_code           PK2679
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              308
_journal_page_last               312
_journal_paper_doi               10.1107/S2056989023002141
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C20 H23 N3 O2'
_chemical_formula_moiety         'C20 H23 N3 O2'
_chemical_formula_sum            'C20 H23 N3 O2'
_chemical_formula_weight         337.41
_chemical_name_systematic
;
<i>N</i>,<i>N</i>'-Diphenyl-2-[1-(propylamino)ethylidene]propanediamide
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   27.7071(11)
_cell_length_b                   27.7071(11)
_cell_length_c                   9.4575(4)
_cell_measurement_reflns_used    23893
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.71
_cell_volume                     7260.4(5)
_computing_cell_refinement
;
X-AREA (Stoe, 2009)
;
_computing_data_collection
;
X-AREA (Stoe, 2009)
;
_computing_data_reduction
;
X-RED (Stoe, 2009)
;
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.911
_diffrn_reflns_theta_min         2.709
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.8437
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED; Stoe, 2009)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3884
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0409P)^2^+6.4556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                2635
_reflns_number_total             3884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2679sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2244223--2244224.cif.'
_cod_original_cell_volume        7260.4(7)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2244224
_cod_database_fobs_code          2244224
_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   0.961
_shelx_estimated_absorpt_t_max   0.980
_shelx_hkl_file
;
  -4  -2   0  812.40    8.95   0
   2  -4   0  824.28    8.28   0
  -2   4   0  781.49    8.37   0
   4   2   0  802.09    9.04   0
   4   0   0  150.58    5.18   0
   0   4   0  166.52    5.03   0
   0  -4   0  160.48    4.61   0
  -4   0   0  154.37    4.96   0
  -4   2   0  994.60   10.04   0
  -2  -4   0  990.76    9.80   0
   2   4   0  973.89    9.62   0
  -4  -4   0 3622.00   15.29   0
  -4   4   0 3580.24   15.07   0
   4  -4   0 3539.95   14.81   0
  -4  -4   0 3702.20   17.90   0
  -4   6   0  460.86    5.88   0
  -6  -4   0  453.04    6.17   0
  -6  -2   0 5607.08   19.49   0
  -2   6   0 5580.91   17.07   0
   6   2   0 5409.18   19.10   0
   2  -6   0 5192.57   16.57   0
  -6   0   0 3088.08   14.61   0
   0  -6   0 3156.29   13.64   0
   0   6   0 3066.99   13.42   0
   6   0   0 2991.43   14.44   0
  -6   2   0 3792.37   13.69   0
  -6   2   0 3818.32   16.54   0
   6  -2   0 3700.96   14.72   0
  -2  -6   0 3651.49   14.94   0
   2   6   0 3700.76   14.97   0
   6  -4   0 9980.24   22.79   0
  -6   4   0 9999.99   21.83   0
  -6  -6   0   46.46    3.75   0
   6  -6   0   44.23    3.74   0
  -6  -6   0   44.40    3.06   0
  -6   6   0   45.82    3.57   0
  -8  -6   0   30.98    2.67   0
  -6   8   0   29.53    3.42   0
   8   4   0  584.34    5.87   0
  -8  -4   0  589.48    5.90   0
  -4   8   0  604.66    5.56   0
  -2   8   0 1185.93   13.06   0
  -2   8   0 1210.22    7.84   0
   8   2   0 1208.56    8.38   0
  -8  -2   0 1239.43    8.77   0
   2  -8   0 1197.85    7.68   0
  -8   0   0   18.06    3.07   0
  -8   0   0   18.64    4.11   0
   0  -8   0   19.49    3.29   0
   8   0   0   14.96    3.80   0
   0   8   0   18.37    3.31   0
  -2  -8   0 2680.33   11.41   0
  -8   2   0 2700.47   13.01   0
  -8   2   0 2696.19   10.20   0
   8  -2   0 2653.25   11.32   0
   2   8   0 2688.78   11.31   0
  -4  -8   0 2082.18   10.14   0
  -8   4   0 2067.78    9.10   0
   4   8   0 2010.06    9.88   0
   8  -4   0 2049.23    9.45   0
   8  -6   0   71.50    3.42   0
  -6  -8   0   72.25    3.28   0
  -8   8   0   -0.08    2.36   0
   8  -8   0   -0.45    2.86   0
  -8  -8   0    0.27    2.76   0
  -8  -8   0    0.89    2.24   0
  -8   8   0    0.27    2.95   0
  -8  10   0    2.85    2.83   0
 -10  -8   0    6.24    2.65   0
   8 -10   0    8.68    2.71   0
  -6  10   0  327.22    4.27   0
 -10  -6   0  324.56    4.35   0
 -10  -4   0   57.95    3.17   0
  -4  10   0   58.42    4.20   0
  -4  10   0   53.32    3.33   0
  10   4   0   57.45    3.07   0
  10   2   0  123.09    3.60   0
  -2  10   0  120.90    6.71   0
   2 -10   0  127.05    3.42   0
 -10  -2   0  130.93    2.95   0
  -2  10   0  122.37    3.64   0
 -10  -2   0  123.84    3.71   0
  10   0   0   20.94    3.05   0
 -10   0   0   23.62    3.17   0
 -10   0   0   27.61    2.67   0
   0  10   0   20.38    3.09   0
  10  -2   0  702.79    5.83   0
 -10   2   0  689.75    6.67   0
   2  10   0  717.43    5.72   0
  -2 -10   0  704.31    5.75   0
  10  -4   0 3518.45   11.23   0
 -10   4   0 3695.62   10.86   0
  -4 -10   0 3679.27   11.95   0
 -10   6   0   57.32    2.82   0
  -6 -10   0   57.97    3.33   0
  10  -8   0  790.38    5.68   0
 -10   8   0  823.29    5.78   0
  -8 -10   0  817.89    6.34   0
 -10 -10   0  150.78    3.11   0
 -10  10   0  143.77    3.45   0
  10 -10   0  152.18    3.40   0
 -10 -10   0  155.28    3.76   0
 -12 -10   0    3.27    2.18   0
 -10  12   0    3.15    2.58   0
 -12 -10   0   -0.54    2.30   0
   8 -12   0   26.70    2.46   0
 -12  -8   0   27.08    2.47   0
  -8  12   0   29.28    2.78   0
 -12  -8   0   33.48    2.49   0
  -6  12   0  314.27    5.06   0
   6 -12   0  311.00    3.92   0
  -6  12   0  318.28    3.72   0
 -12  -6   0  319.25    4.27   0
 -12  -6   0  331.06    3.78   0
 -12  -4   0   86.55    3.01   0
 -12  -4   0   85.71    2.49   0
  12   4   0   83.03    3.10   0
  -4  12   0   84.90    3.08   0
  -4  12   0   84.00    4.41   0
  -2  12   0   31.22    2.53   0
 -12  -2   0   35.90    2.17   0
  12   2   0   35.55    2.83   0
 -12  -2   0   35.37    2.76   0
 -12   0   0  800.91    5.10   0
 -12   0   0  785.13    5.99   0
   0  12   0  795.59    5.37   0
  12   0   0  772.23    5.96   0
   0 -12   0  780.13    5.37   0
 -12   2   0  442.01    3.96   0
  -2 -12   0  425.62    4.28   0
 -12   2   0  430.44    5.35   0
  12  -2   0  429.52    4.59   0
 -12   4   0  172.25    3.20   0
  12  -4   0  173.27    3.59   0
  -4 -12   0  174.80    3.56   0
  12  -6   0   53.82    3.01   0
  -6 -12   0   49.16    3.27   0
 -12   8   0   75.44    2.85   0
  -8 -12   0   75.94    3.34   0
 -10 -12   0   82.37    3.17   0
 -12  10   0   79.56    2.74   0
 -12  10   0   83.48    2.79   0
  12 -10   0   86.02    3.05   0
 -10 -12   0   78.84    3.28   0
 -12 -12   0   91.02    3.03   0
 -12  12   0   88.43    2.73   0
 -12 -12   0   87.51    3.16   0
 -12  12   0   94.11    2.92   0
 -12 -12   0   88.77    2.81   0
  12 -12   0   84.59    2.91   0
 -12  14   0   26.44    2.54   0
 -14 -12   0   18.32    2.43   0
 -14 -12   0   17.75    2.31   0
 -14 -12   0   16.39    2.67   0
 -12  14   0   21.66    2.48   0
  12 -14   0   19.52    2.64   0
 -10  14   0   66.06    2.78   0
 -14 -10   0   73.10    2.68   0
 -14 -10   0   75.91    2.61   0
 -14  -8   0   48.03    2.56   0
  -8  14   0   48.46    2.66   0
 -14  -8   0   47.96    2.45   0
  -8  14   0   46.96    3.12   0
 -14  -6   0    3.30    2.39   0
 -14  -6   0    1.94    2.18   0
  -6  14   0    0.35    3.23   0
  -6  14   0    3.12    2.14   0
  -4  14   0   13.20    4.12   0
  -4  14   0   13.56    2.53   0
 -14  -4   0   11.17    2.27   0
  14   4   0   12.38    2.68   0
 -14  -4   0   11.17    2.93   0
 -14  -2   0  685.86    4.61   0
 -14  -2   0  662.88    5.38   0
  14   2   0  656.93    5.43   0
  -2  14   0  647.14    4.61   0
  14   0   0   13.30    2.85   0
 -14   0   0   12.07    3.19   0
 -14   0   0   14.04    2.23   0
  14  -2   0   69.70    3.20   0
 -14   2   0   75.73    2.52   0
  14  -4   0  107.19    3.30   0
  -4 -14   0  109.50    3.06   0
 -14   4   0  110.52    2.71   0
 -14   6   0   21.35    2.24   0
  14  -6   0   18.43    2.66   0
  -6 -14   0   16.82    2.70   0
 -14   8   0  135.31    2.89   0
  -8 -14   0  140.05    3.93   0
  14  -8   0  128.88    3.12   0
  -8 -14   0  125.50    3.17   0
 -14  10   0   37.96    2.71   0
 -10 -14   0   37.98    2.79   0
 -10 -14   0   43.28    2.80   0
 -12 -14   0   71.01    3.07   0
 -14  12   0   68.83    2.57   0
 -12 -14   0   65.68    2.45   0
 -14  12   0   67.27    2.81   0
  14 -12   0   63.19    2.53   0
 -12 -14   0   66.02    3.00   0
  14 -14   0   86.62    2.71   0
 -14  14   0   94.64    2.80   0
 -14 -14   0   89.03    2.87   0
 -14 -14   0  102.20    3.05   0
 -14  14   0   93.83    2.94   0
 -14 -14   0   88.12    3.35   0
 -14  16   0  156.45    3.40   0
 -14  16   0  146.51    3.26   0
 -16 -14   0  158.25    3.28   0
 -16 -14   0  152.73    3.16   0
  14 -16   0  146.65    3.23   0
 -16 -14   0  143.91    3.78   0
  12 -16   0  203.65    3.09   0
 -16 -12   0  201.61    3.18   0
 -12  16   0  196.69    3.27   0
 -16 -12   0  210.89    3.46   0
 -16 -10   0    3.43    2.49   0
 -10  16   0   14.27    2.50   0
 -16 -10   0    4.63    2.56   0
 -16  -8   0   95.08    2.73   0
  -8  16   0   94.16    3.50   0
  -8  16   0   81.88    2.86   0
 -16  -8   0   93.89    3.00   0
  -6  16   0   41.67    2.31   0
   6 -16   0   37.75    2.42   0
  -6  16   0   37.42    3.74   0
 -16  -6   0   35.80    2.85   0
 -16  -6   0   37.76    2.40   0
   4 -16   0 1125.35    5.64   0
 -16  -4   0 1118.79    6.61   0
 -16  -4   0 1176.61    5.59   0
  16   4   0 1115.37    6.53   0
  -4  16   0 1116.83   11.36   0
  -4  16   0 1122.44    5.72   0
 -16  -2   0  601.95    4.08   0
  -2  16   0  580.69    4.47   0
 -16  -2   0  615.47    5.30   0
  16   2   0  593.23    5.14   0
 -16   0   0  232.74    3.99   0
 -16   0   0  238.01    3.09   0
  16   0   0  223.56    3.78   0
 -16   2   0  484.63    3.90   0
  -2 -16   0  464.74    4.33   0
  16  -2   0  456.43    4.38   0
  -4 -16   0  127.06    5.49   0
  16  -4   0  120.86    3.25   0
 -16   4   0  123.44    2.69   0
  -4 -16   0  117.49    3.05   0
 -16   6   0   -0.04    2.18   0
  -6 -16   0    4.89    3.08   0
  -6 -16   0    2.88    2.38   0
  16  -6   0    1.52    2.43   0
  -8 -16   0  121.23    3.33   0
  16  -8   0  125.50    3.08   0
 -16   8   0  129.65    2.74   0
  -8 -16   0  129.62    3.84   0
  16 -10   0   11.64    2.56   0
 -16  10   0    6.63    2.64   0
 -10 -16   0    8.65    2.86   0
 -10 -16   0    8.47    2.47   0
 -16  10   0    5.04    2.28   0
 -16  12   0   15.05    2.61   0
 -12 -16   0   14.52    2.21   0
 -12 -16   0   16.60    2.46   0
 -16  12   0   10.95    2.52   0
 -12 -16   0   15.01    2.50   0
 -14 -16   0   60.13    3.20   0
 -14 -16   0   62.93    2.89   0
 -16  14   0   60.43    2.76   0
 -16  14   0   62.93    2.59   0
 -14 -16   0   57.04    2.47   0
 -16 -16   0  280.17    4.05   0
 -16 -16   0  258.59    4.26   0
 -16  16   0  270.89    3.81   0
 -16  16   0  272.95    3.75   0
 -16 -16   0  266.96    3.49   0
 -18 -16   0  384.89    3.95   0
  16 -18   0  370.95    3.96   0
 -18 -16   0  369.44    4.79   0
 -18 -16   0  407.75    4.34   0
 -16  18   0  373.73    4.33   0
 -16  18   0  380.43    4.02   0
 -18 -14   0  139.95    3.25   0
 -14  18   0  137.98    2.92   0
  14 -18   0  145.58    3.01   0
 -18 -14   0  154.02    3.10   0
 -12  18   0   30.09    2.42   0
  12 -18   0   36.05    2.83   0
 -18 -12   0   30.50    2.60   0
 -18 -12   0   35.21    2.48   0
 -10  18   0   53.03    3.47   0
 -18 -10   0   54.77    2.84   0
 -18 -10   0   57.61    2.60   0
 -10  18   0   51.41    2.90   0
  -8  18   0    0.37    2.17   0
   8 -18   0    5.21    2.56   0
  -8  18   0    5.93    3.38   0
 -18  -8   0    4.26    2.68   0
 -18  -8   0    4.31    2.24   0
  -6  18   0    7.19    4.18   0
 -18  -6   0    9.24    2.46   0
  -6  18   0    5.99    2.43   0
 -18  -6   0    8.47    1.91   0
 -18  -4   0    9.30    2.16   0
  18   4   0    8.49    2.51   0
  -4  18   0    8.81    2.11   0
   4 -18   0   11.31    2.31   0
 -18  -4   0    9.21    2.82   0
 -18  -2   0  382.56    3.37   0
 -18  -2   0  371.73    4.39   0
  18   2   0  357.48    4.20   0
 -18   0   0  323.22    4.29   0
  18   0   0  317.29    4.06   0
 -18   0   0  339.55    3.46   0
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   9  14   5   29.92    3.31   0
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 -15 -14   5   33.35    4.37   0
 -14  15   5   26.79    2.73   0
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   6 -15   5   25.71    2.56   0
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   6 -15   5   26.51    2.53   0
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   4 -15  -5    7.62    2.54   0
 -15  -4   5    7.00    2.50   0
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   2 -15  -5   61.36    2.95   0
   2 -15   5   53.70    2.93   0
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   2 -15   5   59.55    2.69   0
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  15   0   5  175.99    6.11   0
   0 -15   5  180.35    3.23   0
   0 -15  -5  171.55    3.81   0
   0 -15   5  178.80    3.49   0
   0  15   5  179.77    3.52   0
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   0   4  -8    6.09    2.68   0
   0  -4  -8    3.53    2.36   0
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   4  -2  -8   71.21    2.80   0
   4  -2   8   66.11    2.60   0
   2   4  -8   63.96    2.63   0
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  -4   2  -8   66.34    3.07   0
  -4   2  -8   70.38    3.08   0
   4   4   8  136.39    2.95   0
  -4  -4   8  145.61    3.86   0
   4   4  -8  135.55    3.08   0
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   4  -4  -8  133.37    3.12   0
   4  -4   8  139.34    2.98   0
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  -4   4  -8  141.61    3.27   0
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   5   3  -8    4.33    2.62   0
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  -5  -3  -8    5.18    2.45   0
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  -3   5  -8    7.32    2.88   0
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   5   1   8   65.99    2.55   0
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   5  -1  -8   25.10    2.53   0
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  -3  -5   8    8.98    2.82   0
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   5   5   8   29.54    2.28   0
  -5   5  -8   29.06    3.04   0
  -5  -5   8   27.77    3.36   0
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   5  -5  -8   26.49    2.51   0
   5  -5   8   32.88    2.59   0
   5  -5   8   29.62    2.68   0
  -5   5  -8   20.99    2.50   0
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   6   0  -8   25.39    2.28   0
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   6  -6   8    7.55    2.27   0
   6  -6   8    7.89    2.57   0
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   7  -3   8  166.81    3.09   0
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   7  -7   8   34.07    2.57   0
   7  -7   8   31.77    2.49   0
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   6  -8   8  102.54    2.87   0
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  11  -7   8   15.64    2.04   0
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   8 -12  -8   37.67    2.58   0
   8 -12   8   35.79    2.43   0
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  12   2   8    4.39    2.51   0
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  12  -2   8   12.58    2.55   0
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  -7   4  -9   51.34    2.74   0
  -6  -7   9   22.29    3.37   0
   7  -6  -9   23.45    2.90   0
   7  -6  -9   23.58    2.31   0
  -6  -7  -9   22.64    2.42   0
   7  -6   9   19.37    2.37   0
  -6  -7  -9   23.48    2.60   0
  -7   6  -9   22.83    2.53   0
   7  -8  -9    6.95    2.04   0
  -8  -7  -9   10.09    2.17   0
   7  -8   9    6.09    2.13   0
   7  -8   9    9.46    2.23   0
  -7   8  -9    9.82    2.41   0
  -8  -7  -9   10.96    2.41   0
   8   5   9   28.03    2.09   0
   5  -8  -9   27.76    2.42   0
   5  -8   9   30.42    2.31   0
  -8  -5  -9   33.04    2.35   0
  -5   8  -9   31.39    2.24   0
   5  -8   9   30.70    2.50   0
  -8  -5  -9   32.67    2.66   0
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   8   3   9   -2.98    2.16   0
   8   3  -9   -1.51    1.95   0
   3  -8  -9    3.79    2.37   0
  -3   8  -9    3.56    2.45   0
   3  -8   9    2.87    2.20   0
  -8  -3  -9   -0.73    2.09   0
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  -8  -1  -9    3.03    2.37   0
   8   1   9    8.13    2.22   0
   8   1  -9    5.37    2.38   0
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  -1   8  -9   -4.76    2.49   0
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   8  -1  -9   18.28    2.12   0
   8  -1   9   18.94    2.38   0
  -1  -8  -9   17.37    2.29   0
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   8  -3  -9   -3.19    2.29   0
  -8   3  -9   -0.94    2.48   0
   8  -3   9    5.56    2.28   0
  -3  -8   9    3.96    2.78   0
  -3  -8  -9    1.95    2.24   0
  -8   3  -9    8.09    2.34   0
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  -5  -8   9   24.14    3.16   0
   8  -5  -9   26.59    3.03   0
   8  -5   9   20.93    2.40   0
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  -8   5  -9   29.90    2.57   0
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   8  -9  -9    2.70    2.29   0
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   8  -9   9    3.77    2.12   0
   8  -9   9    7.11    2.28   0
  -8   9  -9    3.79    2.46   0
  -9  -8  -9    7.51    2.19   0
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  -9  -6  -9   14.98    2.28   0
  -6   9  -9   17.77    2.57   0
   6  -9   9   22.41    2.34   0
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   9   4   9    3.57    2.39   0
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  -4   9  -9    9.15    2.45   0
   4  -9   9   10.77    2.29   0
  -9  -4  -9    8.62    2.24   0
   4  -9  -9    8.95    2.53   0
   2  -9  -9   25.07    2.55   0
   9   2   9   18.17    2.30   0
   9   2  -9   28.31    2.17   0
   2  -9  -9   27.60    2.57   0
  -2   9  -9   24.24    2.56   0
   2  -9   9   28.05    2.68   0
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   9   0  -9   37.53    2.51   0
   9   0   9   36.21    2.45   0
  -9   0  -9   42.69    2.58   0
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   0  -9  -9   32.78    2.62   0
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   9  -2  -9   14.75    2.05   0
   9  -2   9   -1.17    2.25   0
   9  -2   9   12.06    2.43   0
  -2  -9  -9    5.64    2.59   0
  -2  -9   9    7.08    2.70   0
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  -4  -9   9    4.14    2.85   0
   9  -4   9    0.56    2.20   0
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   9  -4  -9    4.24    3.04   0
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   9  -6  -9    1.40    2.79   0
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   9  -6   9   -0.47    2.26   0
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   9  -8  -9   13.84    2.65   0
  -8  -9   9   14.56    3.59   0
  -8  -9  -9   14.47    2.18   0
   9  -8  -9    3.01    2.35   0
   9  -8   9   13.64    2.36   0
  -8  -9  -9   16.03    2.24   0
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   5 -10  -9    2.01    2.53   0
   5 -10   9    4.43    2.46   0
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  10  -1   9   14.86    2.25   0
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  -1 -10   9   17.18    2.76   0
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  10  -3  -9   13.17    3.34   0
  10  -3   9   25.45    2.24   0
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  -3 -10   9   19.23    2.76   0
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   6 -11  -9    0.63    2.42   0
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   4 -11  -9   14.99    2.52   0
   4 -11   9   14.67    2.30   0
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   0 -11   9   12.95    2.61   0
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  -2 -11   9    1.67    2.57   0
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  11  -4  -9    0.70    2.10   0
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  -6 -13   9   18.67    3.12   0
  -6 -13  -9   19.90    2.21   0
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   5 -14  -9   24.76    2.59   0
  -5  14  -9   29.43    2.77   0
  -5  14   9   27.78    2.60   0
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   3 -14  -9    8.37    2.21   0
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  14  -3   9   12.54    2.17   0
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  14  -5  -9   19.27    4.30   0
  14  -5   9   20.55    2.07   0
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  -5 -14  -9   20.24    2.31   0
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  -7 -12 -11   -3.88    2.41   0
  -7 -12 -11   -0.96    2.32   0
  13   4  11    0.50    2.12   0
   4 -13 -11   -1.39    2.70   0
   4 -13 -11    2.76    2.38   0
 -13  -4 -11    1.51    2.33   0
  -4  13 -11    5.12    2.48   0
 -13  -4 -11   -2.14    2.23   0
  13   2  11    2.08    2.39   0
   2 -13 -11   -1.08    2.59   0
   2 -13 -11   -2.47    2.28   0
  -2  13 -11   -2.61    2.42   0
   2 -13  11    0.69    2.94   0
 -13  -2 -11    1.22    2.42   0
 -13  -2 -11    5.02    2.46   0
   0 -13 -11    0.55    2.37   0
  13   0  11    0.93    2.29   0
 -13   0 -11    1.87    2.34   0
   0  13 -11    1.81    2.34   0
   0 -13 -11   -0.70    2.34   0
   0 -13  11   -2.68    2.96   0
   0  13  11   -1.53    2.73   0
 -13   0 -11    1.22    2.55   0
  -2 -13 -11    1.71    2.38   0
  13  -2 -11    5.70    2.27   0
 -13   2 -11   -1.56    2.48   0
  13  -2  11    4.80    2.42   0
   2  13 -11    0.74    2.44   0
  -2 -13 -11    2.56    2.04   0
  -2 -13  11    1.45    3.01   0
 -13   2 -11   -3.51    2.49   0
  13  -4  11   -0.59    2.44   0
 -13   4 -11   -1.71    2.49   0
  -4 -13  11    1.15    3.24   0
  -4 -13 -11   -3.03    2.32   0
   4  13  11   -1.79    2.83   0
   3 -14 -11    0.08    2.12   0
   1 -14 -11   -0.63    2.40   0
   1 -14 -11    5.03    2.43   0
  14  -1 -11    1.25    2.28   0
  -1  -1 -12    3.59    2.78   0
;
_shelx_hkl_checksum              22041
_shelx_res_file
;
TITL MH271_3   I -4         R = 0.05  New: I41/a
    MH271_35.res
    created by SHELXL-2018/3 at 13:33:40 on 16-Jan-2023
CELL  0.71073   27.7071  27.7071   9.4575   90.000   90.000   90.000
ZERR    16    0.0011   0.0011   0.0004    0.000    0.000    0.000
LATT 2
SYMM     0.75000 - Y ,    0.25000 + X ,    0.25000 + Z
SYMM     0.50000 - X ,            - Y ,    0.50000 + Z
SYMM     0.75000 + Y ,    0.75000 - X ,    0.75000 + Z
SFAC C  H  N  O
UNIT 320  368 48  32
LIST 4
OMIT -3 55
FMAP 2
PLAN 5
L.S. 20
ACTA
BOND $H
CONF
MPLA  4  O2 C14 N3 C5  H3N C15
MPLA  6 C15 > C20  N3
MPLA  3  O2 C14 N3 H3N C15
MPLA  4  N1 C4 C5 C6   C7 C14
MPLA  3  O1 C7 N2  H2N C8
MPLA  6 C8 > C13  N2
MPLA  4  O1 C7  N2 C5  H2N C8
MPLA  3 C6 C4 N1
MPLA  3 C14 C5 C7
MPLA  4  O1 C7  N2 C5  H2N C8
MPLA  3  N1 C4 C5  C6
MPLA  4  O2 C14 N3 C5  H3N C15
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+1, -z+2
HTAB N1 O2
HTAB N2 O2_$1
HTAB N3 O1
HTAB C6 N2
HTAB C9 O2_$1
HTAB C13 O1
HTAB C20 O2
TEMP  -80
SIZE  0.25  0.35  0.49
SADI  C1A C2A C1B C2B
SADI  C2A C3A C2B C3B
SADI  C3A N1  C3B  N1
ISOR  0.002 C1A C2A C3A C1B C2B C3B
SIMU  C1A C2A C3A
DELU  C1A C2A C3A
SIMU  C1B C2B C3B
DELU  C1B C2B C3B
WGHT    0.040900    6.455600
FVAR       0.22645   0.79386
PART 1
C1A   1    0.330339    0.450943    1.007278    21.00000    0.09236    0.11775 =
         0.09260   -0.00228    0.00886   -0.05532
AFIX 137
H1A   2    0.345612    0.480495    1.042488    21.00000   -1.50000
H1B   2    0.315992    0.433244    1.086538    21.00000   -1.50000
H1C   2    0.305092    0.459356    0.939020    21.00000   -1.50000
AFIX   0
C2A   1    0.366125    0.421124    0.939281    21.00000    0.09025    0.06839 =
         0.07896    0.00548   -0.01283   -0.03051
AFIX  23
H2A   2    0.349729    0.392523    0.898911    21.00000   -1.20000
H2B   2    0.388915    0.409434    1.012267    21.00000   -1.20000
AFIX   0
C3A   1    0.394747    0.445132    0.823623    21.00000    0.05780    0.05129 =
         0.05799   -0.00706   -0.00937   -0.00493
AFIX  23
H3A   2    0.416173    0.421327    0.777213    21.00000   -1.20000
H3B   2    0.372703    0.458651    0.751383    21.00000   -1.20000
AFIX   0
PART 2
C1B   1    0.314162    0.468920    0.965234   -21.00000    0.05962    0.06048 =
         0.07062    0.00284    0.00544   -0.00130
AFIX 137
H1D   2    0.335316    0.489802    1.021394   -21.00000   -1.50000
H1E   2    0.294887    0.448625    1.028587   -21.00000   -1.50000
H1F   2    0.292641    0.488873    0.907398   -21.00000   -1.50000
AFIX   0
C2B   1    0.342917    0.438850    0.874949   -21.00000    0.08067    0.08167 =
         0.08391   -0.00383    0.00024   -0.00060
AFIX  23
H2C   2    0.334739    0.448684    0.777208   -21.00000   -1.20000
H2D   2    0.329972    0.405792    0.886790   -21.00000   -1.20000
AFIX   0
C3B   1    0.395955    0.433665    0.877331   -21.00000    0.05973    0.06053 =
         0.05861   -0.00208   -0.00193   -0.00058
AFIX  23
H3C   2    0.406400    0.416664    0.790496   -21.00000   -1.20000
H3D   2    0.405204    0.413461    0.959305   -21.00000   -1.20000
AFIX   0
PART 0
N1    3    0.423347    0.483562    0.887122    11.00000    0.05181    0.05244 =
         0.06196   -0.01233   -0.00850   -0.00284
H1N   2    0.420259    0.489858    0.981166    11.00000    0.06245
C4    1    0.453707    0.511413    0.814771    11.00000    0.04601    0.04992 =
         0.05081   -0.00369   -0.00662    0.00966
C5    1    0.477279    0.550378    0.877421    11.00000    0.04708    0.04113 =
         0.04399    0.00010   -0.00261    0.00585
C6    1    0.457773    0.500233    0.659175    11.00000    0.06740    0.08050 =
         0.05391   -0.01851   -0.00865    0.00789
AFIX 137
H6A   2    0.474937    0.469611    0.646512    11.00000   -1.50000
H6B   2    0.475621    0.526138    0.611807    11.00000   -1.50000
H6C   2    0.425402    0.497686    0.618089    11.00000   -1.50000
AFIX   0
C7    1    0.515948    0.576537    0.800248    11.00000    0.06501    0.04305 =
         0.04279    0.00272    0.00474    0.00691
O1    4    0.519264    0.620927    0.798179    11.00000    0.11088    0.04129 =
         0.06493    0.00503    0.03162    0.00497
N2    3    0.549967    0.547612    0.738374    11.00000    0.05572    0.04024 =
         0.05280    0.00394    0.00924    0.00324
H2N   2    0.549594    0.517012    0.764138    11.00000    0.05550
C8    1    0.590198    0.561769    0.656320    11.00000    0.05530    0.04741 =
         0.04315   -0.00178    0.00255   -0.00782
C9    1    0.627180    0.528796    0.639678    11.00000    0.05661    0.06560 =
         0.05983    0.00785    0.00437    0.00296
AFIX  43
H9    2    0.625036    0.497964    0.683170    11.00000   -1.20000
AFIX   0
C10   1    0.667522    0.540637    0.559432    11.00000    0.05737    0.09410 =
         0.07263    0.00226    0.01211    0.00232
AFIX  43
H10   2    0.692931    0.517901    0.548843    11.00000   -1.20000
AFIX   0
C11   1    0.670879    0.585081    0.495250    11.00000    0.06975    0.08874 =
         0.06706   -0.00599    0.01511   -0.02827
AFIX  43
H11   2    0.698696    0.593338    0.441738    11.00000   -1.20000
AFIX   0
C12   1    0.633736    0.617242    0.509324    11.00000    0.10013    0.05819 =
         0.06911   -0.00359    0.02565   -0.02492
AFIX  43
H12   2    0.635694    0.647678    0.463431    11.00000   -1.20000
AFIX   0
C13   1    0.593362    0.606254    0.589184    11.00000    0.08371    0.04968 =
         0.06464    0.00220    0.01863   -0.00418
AFIX  43
H13   2    0.567914    0.629032    0.598067    11.00000   -1.20000
AFIX   0
C14   1    0.465647    0.565802    1.021362    11.00000    0.03979    0.03691 =
         0.04588    0.00172   -0.00058    0.00477
O2    4    0.439009    0.541850    1.102898    11.00000    0.04580    0.04114 =
         0.05206   -0.00126    0.00635   -0.00169
N3    3    0.485658    0.608337    1.065017    11.00000    0.05809    0.03972 =
         0.04616   -0.00110    0.00791   -0.00634
H3N   2    0.501378    0.623977    0.995996    11.00000    0.06868
C15   1    0.486746    0.629076    1.201072    11.00000    0.04528    0.03693 =
         0.05013   -0.00271    0.00335    0.00605
C16   1    0.518795    0.667372    1.220192    11.00000    0.05584    0.04145 =
         0.06447   -0.00759    0.00746   -0.00250
AFIX  43
H16   2    0.538506    0.677647    1.143708    11.00000   -1.20000
AFIX   0
C17   1    0.522146    0.690478    1.349142    11.00000    0.06642    0.05039 =
         0.07890   -0.01920    0.00219   -0.00215
AFIX  43
H17   2    0.543793    0.716791    1.360352    11.00000   -1.20000
AFIX   0
C18   1    0.494443    0.675694    1.461053    11.00000    0.08429    0.06416 =
         0.06940   -0.02635    0.00520    0.00264
AFIX  43
H18   2    0.496925    0.691430    1.550003    11.00000   -1.20000
AFIX   0
C19   1    0.463049    0.637849    1.443027    11.00000    0.07946    0.07488 =
         0.05983   -0.01508    0.02210   -0.00139
AFIX  43
H19   2    0.443956    0.627485    1.520741    11.00000   -1.20000
AFIX   0
C20   1    0.458522    0.614406    1.314361    11.00000    0.05652    0.05221 =
         0.05805   -0.00994    0.01331   -0.00430
AFIX  43
H20   2    0.436309    0.588537    1.303791    11.00000   -1.20000
AFIX   0
HKLF 4
REM  MH271_3   I -4         R = 0.05  New: I41/a
REM wR2 = 0.1321, GooF = S = 1.067, Restrained GooF = 1.147 for all data
REM R1 = 0.0516 for 2635 Fo > 4sig(Fo) and 0.0851 for all 3884 data
REM 269 parameters refined using 69 restraints
END
WGHT      0.0408      6.4555
REM Highest difference peak  0.245,  deepest hole -0.185,  1-sigma level  0.033
Q1    1   0.3456  0.4302  0.9634  11.00000  0.05    0.24
Q2    1   0.3077  0.4687  0.8778  11.00000  0.05    0.18
Q3    1   0.3890  0.4093  0.9284  11.00000  0.05    0.14
Q4    1   0.3261  0.5022  0.9879  11.00000  0.05    0.13
Q5    1   0.3271  0.4682  1.0067  11.00000  0.05    0.13
;
_shelx_res_checksum              89719
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
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
C C1A 0.33034(19) 0.4509(2) 1.0073(5) 0.1009(15) Uani d 0.794(7) A 1
H H1A 0.345612 0.480495 1.042488 0.151 Uiso calc 0.794(7) A 1
H H1B 0.315992 0.433244 1.086538 0.151 Uiso calc 0.794(7) A 1
H H1C 0.305092 0.459356 0.939020 0.151 Uiso calc 0.794(7) A 1
C C2A 0.36613(16) 0.42112(13) 0.9393(4) 0.0792(12) Uani d 0.794(7) A 1
H H2A 0.349729 0.392523 0.898911 0.095 Uiso calc 0.794(7) A 1
H H2B 0.388915 0.409434 1.012267 0.095 Uiso calc 0.794(7) A 1
C C3A 0.39475(11) 0.44513(12) 0.8236(4) 0.0557(9) Uani d 0.794(7) A 1
H H3A 0.416173 0.421327 0.777213 0.067 Uiso calc 0.794(7) A 1
H H3B 0.372703 0.458651 0.751383 0.067 Uiso calc 0.794(7) A 1
C C1B 0.3142(5) 0.4689(5) 0.9652(16) 0.064(4) Uani d 0.206(7) A 2
H H1D 0.335316 0.489802 1.021394 0.095 Uiso calc 0.206(7) A 2
H H1E 0.294887 0.448625 1.028587 0.095 Uiso calc 0.206(7) A 2
H H1F 0.292641 0.488873 0.907398 0.095 Uiso calc 0.206(7) A 2
C C2B 0.3429(5) 0.4388(5) 0.8749(18) 0.082(4) Uani d 0.206(7) A 2
H H2C 0.334739 0.448684 0.777208 0.098 Uiso calc 0.206(7) A 2
H H2D 0.329972 0.405792 0.886790 0.098 Uiso calc 0.206(7) A 2
C C3B 0.3960(4) 0.4337(4) 0.8773(17) 0.060(4) Uani d 0.206(7) A 2
H H3C 0.406400 0.416664 0.790496 0.072 Uiso calc 0.206(7) A 2
H H3D 0.405204 0.413461 0.959305 0.072 Uiso calc 0.206(7) A 2
N N1 0.42335(7) 0.48356(7) 0.8871(2) 0.0554(5) Uani d 1 . .
H H1N 0.4203(8) 0.4899(8) 0.981(3) 0.062(7) Uiso d 1 . .
C C4 0.45371(7) 0.51141(7) 0.8148(2) 0.0489(5) Uani d 1 . .
C C5 0.47728(7) 0.55038(7) 0.8774(2) 0.0441(4) Uani d 1 . .
C C6 0.45777(9) 0.50023(10) 0.6592(2) 0.0673(6) Uani d 1 . .
H H6A 0.474937 0.469611 0.646512 0.101 Uiso calc 1 . .
H H6B 0.475621 0.526138 0.611807 0.101 Uiso calc 1 . .
H H6C 0.425402 0.497686 0.618089 0.101 Uiso calc 1 . .
C C7 0.51595(8) 0.57654(7) 0.8002(2) 0.0503(5) Uani d 1 . .
O O1 0.51926(7) 0.62093(5) 0.79818(17) 0.0724(5) Uani d 1 . .
N N2 0.54997(6) 0.54761(6) 0.73837(19) 0.0496(4) Uani d 1 . .
H H2N 0.5496(8) 0.5170(8) 0.764(2) 0.055(6) Uiso d 1 . .
C C8 0.59020(8) 0.56177(7) 0.6563(2) 0.0486(5) Uani d 1 . .
C C9 0.62718(8) 0.52880(9) 0.6397(2) 0.0607(6) Uani d 1 . .
H H9 0.625036 0.497964 0.683170 0.073 Uiso calc 1 . .
C C10 0.66752(9) 0.54064(11) 0.5594(3) 0.0747(7) Uani d 1 . .
H H10 0.692931 0.517901 0.548843 0.090 Uiso calc 1 . .
C C11 0.67088(10) 0.58508(11) 0.4952(3) 0.0752(7) Uani d 1 . .
H H11 0.698696 0.593338 0.441738 0.090 Uiso calc 1 . .
C C12 0.63374(11) 0.61724(9) 0.5093(3) 0.0758(8) Uani d 1 . .
H H12 0.635694 0.647678 0.463431 0.091 Uiso calc 1 . .
C C13 0.59336(10) 0.60625(8) 0.5892(3) 0.0660(6) Uani d 1 . .
H H13 0.567914 0.629032 0.598067 0.079 Uiso calc 1 . .
C C14 0.46565(7) 0.56580(6) 1.0214(2) 0.0409(4) Uani d 1 . .
O O2 0.43901(5) 0.54185(4) 1.10290(14) 0.0463(3) Uani d 1 . .
N N3 0.48566(6) 0.60834(6) 1.06502(18) 0.0480(4) Uani d 1 . .
H H3N 0.5014(9) 0.6240(9) 0.996(3) 0.069(7) Uiso d 1 . .
C C15 0.48675(7) 0.62908(7) 1.2011(2) 0.0441(4) Uani d 1 . .
C C16 0.51880(8) 0.66737(7) 1.2202(2) 0.0539(5) Uani d 1 . .
H H16 0.538506 0.677647 1.143708 0.065 Uiso calc 1 . .
C C17 0.52215(9) 0.69048(8) 1.3491(3) 0.0652(6) Uani d 1 . .
H H17 0.543793 0.716791 1.360352 0.078 Uiso calc 1 . .
C C18 0.49444(10) 0.67569(9) 1.4611(3) 0.0726(7) Uani d 1 . .
H H18 0.496925 0.691430 1.550003 0.087 Uiso calc 1 . .
C C19 0.46305(10) 0.63785(9) 1.4430(3) 0.0714(7) Uani d 1 . .
H H19 0.443956 0.627485 1.520741 0.086 Uiso calc 1 . .
C C20 0.45852(8) 0.61441(8) 1.3144(2) 0.0556(5) Uani d 1 . .
H H20 0.436309 0.588537 1.303791 0.067 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
C1A 0.092(3) 0.118(3) 0.093(3) -0.055(2) 0.009(2) -0.002(2)
C2A 0.0903(19) 0.0684(16) 0.0790(18) -0.0305(14) -0.0128(15) 0.0055(13)
C3A 0.0578(14) 0.0513(14) 0.0580(15) -0.0049(11) -0.0094(12) -0.0071(12)
C1B 0.060(4) 0.060(5) 0.071(5) -0.001(3) 0.005(3) 0.003(3)
C2B 0.081(5) 0.082(5) 0.084(5) -0.001(2) 0.000(2) -0.004(2)
C3B 0.060(4) 0.061(4) 0.059(4) -0.001(2) -0.002(2) -0.002(2)
N1 0.0518(10) 0.0524(10) 0.0620(12) -0.0028(8) -0.0085(9) -0.0123(9)
C4 0.0460(11) 0.0499(11) 0.0508(11) 0.0097(9) -0.0066(9) -0.0037(9)
C5 0.0471(11) 0.0411(10) 0.0440(10) 0.0058(8) -0.0026(9) 0.0001(8)
C6 0.0674(15) 0.0805(16) 0.0539(13) 0.0079(12) -0.0086(11) -0.0185(12)
C7 0.0650(13) 0.0431(11) 0.0428(10) 0.0069(9) 0.0047(10) 0.0027(9)
O1 0.1109(14) 0.0413(8) 0.0649(10) 0.0050(8) 0.0316(10) 0.0050(7)
N2 0.0557(10) 0.0402(9) 0.0528(10) 0.0032(7) 0.0092(8) 0.0039(8)
C8 0.0553(12) 0.0474(11) 0.0432(10) -0.0078(9) 0.0026(9) -0.0018(9)
C9 0.0566(13) 0.0656(14) 0.0598(13) 0.0030(11) 0.0044(11) 0.0078(11)
C10 0.0574(14) 0.094(2) 0.0726(16) 0.0023(13) 0.0121(13) 0.0023(15)
C11 0.0698(17) 0.0887(19) 0.0671(15) -0.0283(15) 0.0151(13) -0.0060(14)
C12 0.100(2) 0.0582(14) 0.0691(16) -0.0249(14) 0.0257(15) -0.0036(12)
C13 0.0837(17) 0.0497(12) 0.0646(14) -0.0042(11) 0.0186(13) 0.0022(11)
C14 0.0398(10) 0.0369(9) 0.0459(10) 0.0048(7) -0.0006(8) 0.0017(8)
O2 0.0458(7) 0.0411(7) 0.0521(8) -0.0017(6) 0.0064(6) -0.0013(6)
N3 0.0581(10) 0.0397(9) 0.0462(9) -0.0063(7) 0.0079(8) -0.0011(7)
C15 0.0453(10) 0.0369(10) 0.0501(11) 0.0060(8) 0.0033(9) -0.0027(8)
C16 0.0558(12) 0.0415(11) 0.0645(13) -0.0025(9) 0.0075(10) -0.0076(10)
C17 0.0664(15) 0.0504(12) 0.0789(16) -0.0022(11) 0.0022(13) -0.0192(12)
C18 0.0843(18) 0.0642(15) 0.0694(16) 0.0026(13) 0.0052(14) -0.0263(13)
C19 0.0795(17) 0.0749(16) 0.0598(14) -0.0014(13) 0.0221(13) -0.0151(13)
C20 0.0565(12) 0.0522(12) 0.0580(13) -0.0043(9) 0.0133(10) -0.0099(10)
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
30 23 7 0.2217
30 -1 2 0.3561
30 22 4 0.3512
28 -18 30 0.9806
-30 -14 -6 0.2011
-30 8 -2 0.4506
10 -30 -1 0.7079
-30 -9 -10 0.3841
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
C2A C1A H1A . . 109.5 ?
C2A C1A H1B . . 109.5 ?
H1A C1A H1B . . 109.5 ?
C2A C1A H1C . . 109.5 ?
H1A C1A H1C . . 109.5 ?
H1B C1A H1C . . 109.5 ?
C1A C2A C3A . . 115.7(3) ?
C1A C2A H2A . . 108.4 ?
C3A C2A H2A . . 108.4 ?
C1A C2A H2B . . 108.4 ?
C3A C2A H2B . . 108.4 ?
H2A C2A H2B . . 107.4 ?
N1 C3A C2A . . 108.1(3) ?
N1 C3A H3A . . 110.1 ?
C2A C3A H3A . . 110.1 ?
N1 C3A H3B . . 110.1 ?
C2A C3A H3B . . 110.1 ?
H3A C3A H3B . . 108.4 ?
C2B C1B H1D . . 109.5 ?
C2B C1B H1E . . 109.5 ?
H1D C1B H1E . . 109.5 ?
C2B C1B H1F . . 109.5 ?
H1D C1B H1F . . 109.5 ?
H1E C1B H1F . . 109.5 ?
C1B C2B C3B . . 126.9(13) ?
C1B C2B H2C . . 105.6 ?
C3B C2B H2C . . 105.6 ?
C1B C2B H2D . . 105.6 ?
C3B C2B H2D . . 105.6 ?
H2C C2B H2D . . 106.1 ?
C2B C3B N1 . . 113.2(10) ?
C2B C3B H3C . . 108.9 ?
N1 C3B H3C . . 108.9 ?
C2B C3B H3D . . 108.9 ?
N1 C3B H3D . . 108.9 ?
H3C C3B H3D . . 107.8 ?
C4 N1 C3A . . 123.8(2) ?
C4 N1 C3B . . 141.3(6) ?
C4 N1 H1N . . 116.8(15) ?
C3A N1 H1N . . 119.5(15) ?
C3B N1 H1N . . 100.4(16) ?
N1 C4 C5 . . 121.78(19) ?
N1 C4 C6 . . 115.5(2) ?
C5 C4 C6 . . 122.6(2) ?
C4 C5 C14 . . 121.24(18) ?
C4 C5 C7 . . 120.47(18) ?
C14 C5 C7 . . 118.27(17) ?
C4 C6 H6A . . 109.5 ?
C4 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
C4 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
O1 C7 N2 . . 121.7(2) ?
O1 C7 C5 . . 123.24(19) ?
N2 C7 C5 . . 114.91(17) ?
C7 N2 C8 . . 127.97(18) ?
C7 N2 H2N . . 115.9(14) ?
C8 N2 H2N . . 115.3(14) ?
C9 C8 C13 . . 119.2(2) ?
C9 C8 N2 . . 117.63(18) ?
C13 C8 N2 . . 123.1(2) ?
C8 C9 C10 . . 120.2(2) ?
C8 C9 H9 . . 119.9 ?
C10 C9 H9 . . 119.9 ?
C11 C10 C9 . . 120.4(3) ?
C11 C10 H10 . . 119.8 ?
C9 C10 H10 . . 119.8 ?
C12 C11 C10 . . 119.3(2) ?
C12 C11 H11 . . 120.4 ?
C10 C11 H11 . . 120.4 ?
C11 C12 C13 . . 121.2(2) ?
C11 C12 H12 . . 119.4 ?
C13 C12 H12 . . 119.4 ?
C12 C13 C8 . . 119.7(2) ?
C12 C13 H13 . . 120.1 ?
C8 C13 H13 . . 120.1 ?
O2 C14 N3 . . 120.55(18) ?
O2 C14 C5 . . 123.10(17) ?
N3 C14 C5 . . 116.35(17) ?
C14 N3 C15 . . 129.51(17) ?
C14 N3 H3N . . 113.2(16) ?
C15 N3 H3N . . 117.2(16) ?
C20 C15 C16 . . 118.78(19) ?
C20 C15 N3 . . 125.00(18) ?
C16 C15 N3 . . 116.23(18) ?
C17 C16 C15 . . 120.7(2) ?
C17 C16 H16 . . 119.7 ?
C15 C16 H16 . . 119.7 ?
C18 C17 C16 . . 120.4(2) ?
C18 C17 H17 . . 119.8 ?
C16 C17 H17 . . 119.8 ?
C17 C18 C19 . . 119.2(2) ?
C17 C18 H18 . . 120.4 ?
C19 C18 H18 . . 120.4 ?
C18 C19 C20 . . 121.6(2) ?
C18 C19 H19 . . 119.2 ?
C20 C19 H19 . . 119.2 ?
C19 C20 C15 . . 119.3(2) ?
C19 C20 H20 . . 120.3 ?
C15 C20 H20 . . 120.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1A C2A . 1.442(6) ?
C1A H1A . 0.9800 ?
C1A H1B . 0.9800 ?
C1A H1C . 0.9800 ?
C2A C3A . 1.506(5) ?
C2A H2A . 0.9900 ?
C2A H2B . 0.9900 ?
C3A N1 . 1.457(3) ?
C3A H3A . 0.9900 ?
C3A H3B . 0.9900 ?
C1B C2B . 1.435(14) ?
C1B H1D . 0.9800 ?
C1B H1E . 0.9800 ?
C1B H1F . 0.9800 ?
C2B C3B . 1.477(14) ?
C2B H2C . 0.9900 ?
C2B H2D . 0.9900 ?
C3B N1 . 1.580(12) ?
C3B H3C . 0.9900 ?
C3B H3D . 0.9900 ?
N1 C4 . 1.331(3) y
N1 H1N . 0.91(2) ?
C4 C5 . 1.394(3) y
C4 C6 . 1.508(3) ?
C5 C14 . 1.463(3) ?
C5 C7 . 1.485(3) ?
C6 H6A . 0.9800 ?
C6 H6B . 0.9800 ?
C6 H6C . 0.9800 ?
C7 O1 . 1.234(2) y
C7 N2 . 1.369(3) y
N2 C8 . 1.414(3) ?
N2 H2N . 0.88(2) ?
C8 C9 . 1.382(3) ?
C8 C13 . 1.389(3) ?
C9 C10 . 1.390(3) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.376(4) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.368(4) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.384(3) ?
C12 H12 . 0.9500 ?
C13 H13 . 0.9500 ?
C14 O2 . 1.257(2) y
C14 N3 . 1.366(2) y
N3 C15 . 1.410(3) ?
N3 H3N . 0.90(3) ?
C15 C20 . 1.387(3) ?
C15 C16 . 1.395(3) ?
C16 C17 . 1.380(3) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.370(4) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.373(4) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.385(3) ?
C19 H19 . 0.9500 ?
C20 H20 . 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
N1 H1N O2 . 0.91(2) 1.92(2) 2.638(2) 135(2) yes
N3 H3N O1 . 0.90(3) 1.94(3) 2.712(2) 144(2) yes
C6 H6B N2 . 0.98 2.46 2.968(3) 112.2 yes
C13 H13 O1 . 0.95 2.33 2.879(3) 115.9 yes
C20 H20 O2 . 0.95 2.30 2.887(3) 119.4 yes
N2 H2N O2 9_667 0.88(2) 2.08(2) 2.914(2) 157(2) yes
C9 H9 O2 9_667 0.95 2.91 3.622(3) 132.9 yes
C13 H13 Cg2 1_554 0.95 3.37 3.960(3) 122.2 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
C1A C2A C3A N1 . . . . 65.0(4) y
C1B C2B C3B N1 . . . . -46(2) y
C2A C3A N1 C4 . . . . 178.5(3) ?
C2B C3B N1 C4 . . . . -116.6(12) ?
C3A N1 C4 C5 . . . . 174.5(2) ?
C3B N1 C4 C5 . . . . -166.6(8) ?
C3A N1 C4 C6 . . . . -1.1(3) ?
C3B N1 C4 C6 . . . . 17.9(9) ?
N1 C4 C5 C14 . . . . -7.0(3) ?
C6 C4 C5 C14 . . . . 168.25(18) ?
N1 C4 C5 C7 . . . . 171.42(18) ?
C6 C4 C5 C7 . . . . -13.4(3) ?
C4 C5 C7 O1 . . . . 136.4(2) ?
C14 C5 C7 O1 . . . . -45.1(3) ?
C4 C5 C7 N2 . . . . -47.7(3) ?
C14 C5 C7 N2 . . . . 130.73(19) ?
O1 C7 N2 C8 . . . . -5.4(3) ?
C5 C7 N2 C8 . . . . 178.67(19) ?
C7 N2 C8 C9 . . . . 161.2(2) ?
C7 N2 C8 C13 . . . . -20.8(3) ?
C13 C8 C9 C10 . . . . 1.6(3) ?
N2 C8 C9 C10 . . . . 179.6(2) ?
C8 C9 C10 C11 . . . . -0.4(4) ?
C9 C10 C11 C12 . . . . -1.0(4) ?
C10 C11 C12 C13 . . . . 1.3(4) ?
C11 C12 C13 C8 . . . . -0.2(4) ?
C9 C8 C13 C12 . . . . -1.3(4) ?
N2 C8 C13 C12 . . . . -179.3(2) ?
C4 C5 C14 O2 . . . . 9.5(3) ?
C7 C5 C14 O2 . . . . -168.94(17) ?
C4 C5 C14 N3 . . . . -170.85(17) ?
C7 C5 C14 N3 . . . . 10.7(2) ?
O2 C14 N3 C15 . . . . 9.3(3) ?
C5 C14 N3 C15 . . . . -170.35(18) ?
C14 N3 C15 C20 . . . . -14.1(3) ?
C14 N3 C15 C16 . . . . 166.21(19) ?
C20 C15 C16 C17 . . . . -0.4(3) ?
N3 C15 C16 C17 . . . . 179.2(2) ?
C15 C16 C17 C18 . . . . 0.9(4) ?
C16 C17 C18 C19 . . . . -0.5(4) ?
C17 C18 C19 C20 . . . . -0.3(4) ?
C18 C19 C20 C15 . . . . 0.7(4) ?
C16 C15 C20 C19 . . . . -0.3(3) ?
N3 C15 C20 C19 . . . . 180.0(2) ?