#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:50:31 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/96/1559638.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1559638
loop_
_publ_author_name
'Guarnieri-Ibáñez, Alejandro'
'de Aguirre, Adiran'
'Besnard, Céline'
'Poblador-Bahamonde, Amalia I'
'Lacour, Jérôme'
_publ_section_title
;
 Regiodivergent synthesis of pyrazino-indolines vs. triazocines
 via α-imino carbenes addition to imidazolidines.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1479
_journal_page_last               1485
_journal_paper_doi               10.1039/d0sc05725h
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C26 H25 N3 O2'
_chemical_formula_sum            'C26 H25 N3 O2'
_chemical_formula_weight         411.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-05
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-07-09 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.50216(12)
_cell_length_b                   21.27952(14)
_cell_length_c                   10.92519(7)
_cell_measurement_reflns_used    53948
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      74.2240
_cell_measurement_theta_min      3.1410
_cell_volume                     4301.43(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -91.00 -66.00   0.50    1.00    --  -57.24 154.00-128.00   50
  2  ω    -53.00 -20.00   0.50    1.00    --  -57.24  93.00-179.00   66
  3  ω    -51.00 -13.00   0.50    1.00    --  -57.24 120.00  74.00   76
  4  ω   -106.00 -62.00   0.50    1.00    --  -57.24 -31.00-154.00   88
  5  ω    -33.00  -8.00   0.50    1.00    --  -57.24  31.00   5.00   50
  6  ω     24.00  49.00   0.50    1.00    --   60.61 -93.00  68.00   50
  7  ω     63.00  88.00   0.50    1.00    --   60.61  31.00   5.00   50
  8  ω     55.00  80.00   0.50    1.00    --   60.61-154.00-167.00   50
  9  ω     36.00  61.00   0.50    1.00    --   75.13 -93.00  68.00   50
 10  ω     54.00  80.00   0.50    1.00    --   75.13-120.00 -10.00   52
 11  ω     38.00  63.00   0.50    1.00    --   77.04 -93.00  68.00   50
 12  ω     63.00  89.00   0.50    1.00    --   77.04-154.00-167.00   52
 13  ω     80.00 105.00   0.50    1.00    --   77.04  31.00   5.00   50
 14  ω    -35.00 -10.00   0.50    1.00    --  -57.24  30.00   0.00   50
 15  ω     41.00  79.00   0.50    1.00    --   75.13 -94.00-120.00   76
 16  ω     37.00  79.00   0.50    1.00    --   75.13 -94.00  90.00   84
 17  ω     93.00 118.00   0.50    1.00    --   77.04  30.00  60.00   50
 18  ω     92.00 127.00   0.50    1.00    --   77.04  30.00  90.00   70
 19  ω     84.00 110.00   0.50    1.00    --   81.25-152.00 135.67   52
 20  ω     40.00 101.00   0.50    1.00    --   81.25-108.00 164.97  122
 21  ω     43.00  76.00   0.50    1.00    --   81.25 -73.00 -49.66   66
 22  ω    101.00 126.00   0.50    1.00    --   81.25   8.00  11.67   50
 23  ω     43.00  68.00   0.50    1.00    --   81.25-113.00  85.23   50
 24  ω     49.00  75.00   0.50    1.00    --   81.25   0.00 175.68   52
 25  ω     45.00  71.00   0.50    1.00    --   81.25   0.00  -4.18   52
 26  ω     72.00 115.00   0.50    1.00    --   81.25  -1.00  73.92   86
 27  ω     92.00 117.00   0.50    1.00    --   81.25  58.00 -99.83   50
 28  ω     37.00  62.00   0.50    1.00    --   81.25 -54.00 -86.77   50
 29  ω     89.00 114.00   0.50    1.00    --   81.25  36.00 -48.98   50
 30  ω     55.00 106.00   0.50    1.00    --   81.25-115.00 -98.49  102
 31  ω     53.00 105.00   0.50    1.00    --   81.25  14.00 171.17  104
 32  ω     42.00 115.00   0.50    1.00    --   81.25-138.00 166.72  146
 33  ω     47.00  83.00   0.50    1.00    --   81.25   8.00  11.67   72
 34  ω     48.00  74.00   0.50    1.00    --   81.25 -80.00 162.42   52
 35  ω     57.00  92.00   0.50    1.00    --   81.25-122.00  47.57   70
 36  ω     71.00 103.00   0.50    1.00    --   81.25 163.00-166.54   64
 37  ω     56.00 102.00   0.50    1.00    --   81.25   5.00 116.37   92
 38  ω     57.00  83.00   0.50    1.00    --   75.13-154.00-167.00   52
 39  ω    -14.00  14.00   0.50    1.00    --    0.00 102.00 -54.87   56
 40  ω     -4.00  21.00   0.50    1.00    --    8.00  97.00 131.50   50
 41  ω      5.00  30.00   0.50    1.00    --   16.00  95.00-117.12   50
 42  ω     12.00  38.00   0.50    1.00    --   20.00  92.00 -97.54   52
 43  ω     12.00  37.00   0.50    1.00    --   20.00  91.00 -13.12   50
 44  ω     12.00  37.00   0.50    1.00    --   20.00  91.00 116.16   50
 45  ω     16.00  41.00   0.50    1.00    --   24.00  91.00  46.18   50
 46  ω    -41.00  -8.00   0.50    1.00    --  -24.00 104.00 119.35   66
 47  ω     16.00  41.00   0.50    1.00    --   24.00  91.00-178.77   50
 48  ω     30.00  55.00   0.50    1.00    --   28.00  75.00 121.30   50
 49  ω     29.00  54.00   0.50    1.00    --   28.00  77.00 -41.52   50
 50  ω     34.00  59.00   0.50    1.00    --   28.00  67.00  73.59   50
 51  ω    -60.00 -35.00   0.50    1.00    --  -32.00 -74.00 160.82   50
 52  ω     31.00  56.00   0.50    1.00    --   32.00  80.00 141.99   50
 53  ω     35.00  60.00   0.50    1.00    --   36.00  80.00 157.40   50
 54  ω     36.00  61.00   0.50    1.00    --   36.00  79.00-117.02   50
 55  ω     36.00  61.00   0.50    1.00    --   36.00  78.00  19.56   50
 56  ω     37.00  62.00   0.50    1.00    --   36.00  77.00  79.41   50
 57  ω     38.00  63.00   0.50    1.00    --   36.00  75.00-126.95   50
 58  ω     38.00  63.00   0.50    1.00    --   36.00  76.00 -29.75   50
 59  ω     41.00  66.00   0.50    1.00    --   36.00  69.00  11.30   50
 60  ω    -67.00 -41.00   0.50    1.00    --  -40.00 -76.00 -26.98   52
 61  ω     46.00  71.00   0.50    1.00    --   40.00  65.00  41.21   50
 62  ω     42.00  67.00   0.50    1.00    --   40.00  75.00 -73.12   50
 63  ω     45.00  71.00   0.50    1.00    --   44.00  79.00  43.11   52
 64  ω    -69.00 -43.00   0.50    1.00    --  -44.00 -80.00 168.67   52
 65  ω     43.00  68.00   0.50    1.00    --   44.00  80.00 118.00   50
 66  ω     46.00  71.00   0.50    1.00    --   44.00  76.00-105.86   50
 67  ω     43.00  68.00   0.50    1.00    --   44.00  80.00-127.95   50
 68  ω    -71.00 -46.00   0.50    1.00    --  -44.00 -75.00 -84.86   50
 69  ω     43.00  68.00   0.50    1.00    --   44.00  80.00  98.39   50
 70  ω     47.00  72.00   0.50    1.00    --   48.00  80.00-159.58   50
 71  ω     54.00  79.00   0.50    1.00    --   48.00  65.00 157.95   50
 72  ω     47.00  72.00   0.50    1.00    --   48.00  80.00 -87.35   50
 73  ω     57.00  82.00   0.50    1.00    --   52.00  71.00  15.55   50
 74  ω     55.00  80.00   0.50    1.00    --   52.00  73.00 -40.78   50
 75  ω     51.00  76.00   0.50    1.00    --   52.00  80.00 152.01   50
 76  ω     58.00  83.00   0.50    1.00    --   52.00  66.00  87.42   50
 77  ω     56.00  81.00   0.50    1.00    --   52.00  72.00 -28.48   50
 78  ω     57.00  82.00   0.50    1.00    --   52.00  70.00  -0.66   50
 79  ω     59.00  84.00   0.50    1.00    --   52.00  63.00-160.34   50
 80  ω     57.00  82.00   0.50    1.00    --   52.00  70.00 -55.74   50
 81  ω     51.00  76.00   0.50    1.00    --   52.00  80.00  22.17   50
 82  ω     60.00  85.00   0.50    1.00    --   56.00  72.00  38.63   50
 83  ω    -87.00 -61.00   0.50    1.00    --  -56.00 -71.00-135.04   52
 84  ω     61.00  86.00   0.50    1.00    --   56.00  71.00-138.13   50
 85  ω    -34.00  -8.00   0.50    1.00    --  -57.24  30.00 -60.00   52
 86  ω    -35.00  -8.00   0.50    1.00    --  -57.24  30.00  60.00   54
 87  ω    -35.00 -10.00   0.50    1.00    --  -57.24  30.00  30.00   50
 88  ω    -35.00 -10.00   0.50    1.00    --  -57.24  30.00 120.00   50
 89  ω    -35.00 -10.00   0.50    1.00    --  -57.24  30.00-150.00   50
 90  ω    -35.00  -9.00   0.50    1.00    --  -57.24  30.00-180.00   52
 91  ω    -35.00 -10.00   0.50    1.00    --  -57.24  30.00  90.00   50
 92  ω     64.00  89.00   0.50    1.00    --   60.00  72.00 -17.69   50
 93  ω     65.00  90.00   0.50    1.00    --   60.00  70.00  68.82   50
 94  ω     67.00  92.00   0.50    1.00    --   64.00  73.00   1.58   50
 95  ω     67.00  92.00   0.50    1.00    --   64.00  73.00 100.96   50
 96  ω    -90.00 -64.00   0.50    1.00    --  -64.50 -80.00 -98.53   52
 97  ω    -99.00 -73.00   0.50    1.00    --  -64.50 -76.00  71.25   52
 98  ω    -93.00 -67.00   0.50    1.00    --  -64.50 -75.00  27.01   52
 99  ω    -92.00 -66.00   0.50    1.00    --  -64.50 -79.00 124.34   52
100  ω    -94.00 -65.00   0.50    1.00    --  -64.50 -78.00 -60.54   58
101  ω    -92.00 -66.00   0.50    1.00    --  -64.50 -78.00-154.59   52
102  ω    -92.00 -66.00   0.50    1.00    --  -64.50 -78.00-168.59   52
103  ω    -92.00 -66.00   0.50    1.00    --  -64.50 -80.00-174.43   52
104  ω    -90.00 -64.00   0.50    1.00    --  -64.50 -79.00 -30.94   52
105  ω    -93.00 -67.00   0.50    1.00    --  -64.50 -75.00  49.09   52
106  ω   -100.00 -64.00   0.50    1.00    --  -64.50 -80.00 171.02   72
107  ω    -91.00 -65.00   0.50    1.00    --  -64.50 -77.00 107.80   52
108  ω    -91.00 -65.00   0.50    1.00    --  -64.50 -78.00 148.49   52
109  ω   -113.00 -76.00   0.50    1.00    --  -64.50 -36.00 176.94   74
110  ω    -90.00 -65.00   0.50    1.00    --  -64.50 -78.00 126.59   50
111  ω    -94.00 -68.00   0.50    1.00    --  -64.50 -72.00 -88.97   52
112  ω    -91.00 -65.00   0.50    1.00    --  -64.50 -79.00  95.30   52
113  ω    -89.00 -64.00   0.50    1.00    --  -64.50 -79.00-123.47   50
114  ω   -104.00 -79.00   0.50    1.00    --  -64.50 -71.00  96.47   50
115  ω     68.00  98.00   0.50    1.00    --   68.00  79.00   9.35   60
116  ω     71.00  96.00   0.50    1.00    --   68.00  74.00-119.59   50
117  ω     71.00  96.00   0.50    1.00    --   68.00  74.00 124.66   50
118  ω     36.00 107.00   0.50    1.00    --   75.13   0.00 120.00  142
119  ω     36.00  62.00   0.50    1.00    --   75.13   0.00-150.00   52
120  ω     34.00  60.00   0.50    1.00    --   75.13-125.00 -90.00   52
121  ω     99.00 124.00   0.50    1.00    --   75.13-154.00-167.00   50
122  ω     82.00 107.00   0.50    1.00    --   76.00  68.00 -35.09   50
123  ω     44.00  74.00   0.50    1.00    --   77.04-125.00 -60.00   60
124  ω     79.00 111.00   0.50    1.00    --   77.04  30.00-180.00   64
125  ω     73.00 105.00   0.50    1.00    --   77.04-125.00  60.00   64
126  ω     41.00  67.00   0.50    1.00    --   77.04-125.00  60.00   52
127  ω     38.00  63.00   0.50    1.00    --   77.04 -94.00 -60.00   50
128  ω     38.00  73.00   0.50    1.00    --   77.04-125.00-150.00   70
129  ω     48.00  81.00   0.50    1.00    --   77.04-125.00  30.00   66
130  ω     37.00  81.00   0.50    1.00    --   77.04-125.00 -30.00   88
131  ω     77.00 102.00   0.50    1.00    --   77.04-125.00 -60.00   50
132  ω     45.00  90.00   0.50    1.00    --   77.04   0.00  60.00   90
133  ω     90.00 116.00   0.50    1.00    --   77.04  30.00 -60.00   52
134  ω     37.00  66.00   0.50    1.00    --   77.04 -94.00-150.00   58
135  ω     51.00  77.00   0.50    1.00    --   77.04-125.00 150.00   52
136  ω     79.00 107.00   0.50    1.00    --   80.00  80.00 -68.87   56
137  ω     83.00 108.00   0.50    1.00    --   81.25  76.00 -93.25   50
138  ω     91.00 119.00   0.50    1.00    --   81.25  59.00   7.58   56
139  ω     62.00 120.00   0.50    1.00    --   81.25  -2.00-161.63  116
140  ω     83.00 110.00   0.50    1.00    --   81.25-125.00-138.29   54
141  ω     67.00 105.00   0.50    1.00    --   81.25-118.00-117.96   76
142  ω     35.00  61.00   0.50    1.00    --   81.25-118.00-117.96   52
143  ω     42.00  68.00   0.50    1.00    --   81.25-125.00-138.29   52
144  ω     90.00 115.00   0.50    1.00    --   81.25  54.00  94.00   50
145  ω     65.00  91.00   0.50    1.00    --   81.25-174.00  37.70   52
146  ω    105.00 130.00   0.50    1.00    --   81.25  19.00 -31.45   50
147  ω     59.00  85.00   0.50    1.00    --   81.25  19.00 -31.45   52
148  ω     92.00 118.00   0.50    1.00    --   81.25  22.00  34.17   52
149  ω     62.00  88.00   0.50    1.00    --   81.25  22.00  34.17   52
150  ω     83.00 109.00   0.50    1.00    --   81.25-120.00  84.46   52
151  ω     76.00 111.00   0.50    1.00    --   81.25-125.00 163.80   70
152  ω     36.00  62.00   0.50    1.00    --   81.25-120.00  84.46   52
153  ω     51.00 106.00   0.50    1.00    --   81.25-152.00 -46.25  110
154  ω     42.00  76.00   0.50    1.00    --   81.25 -67.00-141.95   68
155  ω     95.00 121.00   0.50    1.00    --   81.25  55.00-125.23   52
156  ω     84.00 109.00   0.50    1.00    --   81.25  74.00  22.86   50
157  ω     90.00 125.00   0.50    1.00    --   81.25  47.00-148.61   70
158  ω     87.00 114.00   0.50    1.00    --   81.25  76.00  32.95   54
159  ω     44.00  73.00   0.50    1.00    --   81.25 -69.00  12.95   58
160  ω     82.00 116.00   0.50    1.00    --   81.25  78.00 141.48   68
161  ω     41.00 120.00   0.50    1.00    --   81.25  -2.00 -76.76  158
162  ω     89.00 115.00   0.50    1.00    --   81.25  60.00 -14.95   52
163  ω     89.00 130.00   0.50    1.00    --   81.25-155.00   9.85   82
164  ω     51.00  76.00   0.50    1.00    --   81.25-155.00   9.85   50
165  ω     58.00  84.00   0.50    1.00    --   81.25-154.00 134.21   52
166  ω     90.00 116.00   0.50    1.00    --   81.25-132.00  26.70   52
167  ω     38.00  82.00   0.50    1.00    --   81.25-132.00  26.70   88
168  ω     84.00 119.00   0.50    1.00    --   81.25  75.00  95.30   70
169  ω     81.00 118.00   0.50    1.00    --   81.25  79.00   2.00   74
170  ω     89.00 122.00   0.50    1.00    --   81.25  58.00-133.33   66
171  ω     61.00 121.00   0.50    1.00    --   81.25  22.00-145.39  120
172  ω     55.00  80.00   0.50    1.00    --   60.61-154.00-167.00   50
173  ω     82.00 107.00   0.50    1.00    --   81.25  77.00 110.58   50
174  ω     51.00  77.00   0.50    1.00    --   81.25 -73.00-110.12   52
175  ω     37.00  63.00   0.50    1.00    --   81.25-112.00  30.60   52
176  ω     72.00  98.00   0.50    1.00    --   81.25-112.00  30.60   52
177  ω     81.00 106.00   0.50    1.00    --   81.25  79.00 154.27   50
178  ω     80.00 105.00   0.50    1.00    --   77.04-120.00 -10.00   50
179  ω     51.00 102.00   0.50    1.00    --   81.25-146.00  82.66  102
180  ω     82.00 107.00   0.50    1.00    --   81.25  77.00  81.03   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0443184000
_diffrn_orient_matrix_UB_12      0.0608389000
_diffrn_orient_matrix_UB_13      0.0150123000
_diffrn_orient_matrix_UB_21      0.0629204000
_diffrn_orient_matrix_UB_22      0.0381882000
_diffrn_orient_matrix_UB_23      -0.0545154000
_diffrn_orient_matrix_UB_31      -0.0316931000
_diffrn_orient_matrix_UB_32      -0.0090402000
_diffrn_orient_matrix_UB_33      -0.1292336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            89610
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.897
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       plate
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.652
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.112
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
 Flack parameter: the space groupÃ? contains symmetry element of the second kind.
 The NO2 group is disordered and was refined using 2 components with the following restraints:
SADI N29A C28 N29B C28
SADI O30A N29A O30B N29B O31A N29A O31B N29B
RIGU O30B O31B N29B C28
RIGU O30A O31A N29A C28
;
_refine_ls_abs_structure_Flack   -0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0280
_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/[σ²(Fo²)+(0.0443P)²+0.9442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                4241
_reflns_number_total             4355
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc05725h2.cif
_cod_data_source_block           ajgi879b
_cod_depositor_comments
;Adding full bibliography for 1559635--1559639.cif.

 Adding full bibliography for 1559635--1559639.cif.
;
_cod_database_code               1559638
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H25 N3 O2'
_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.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.1(3)
 -0.1(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N29A-C28 \\sim N29B-C28
 with sigma of 0.02
 O30A-N29A \\sim O30B-N29B \\sim O31A-N29A \\sim O31B-N29B
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 O30B, O31B, N29B, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O30A, O31A, N29A, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O30B)=Sof(O31B)=Sof(N29B)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(O30A)=Sof(O31A)=Sof(N29A)=Sof(H28A)=Sof(H28B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C28(H28C,H28D), C28(H28A,H28B)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C26(H26), C27(H27)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.060
_oxdiff_exptl_absorpt_empirical_full_min 0.654
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1, z+1/2'
'-x+1, y+1, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O30A O 0.5491(6) 0.6666(9) 0.9008(7) 0.075(3) Uani 0.48(3) 1 d D . P A 1
O30B O 0.5343(5) 0.6350(9) 0.8902(8) 0.070(3) Uani 0.52(3) 1 d D . P A 2
O31A O 0.5022(7) 0.5765(7) 0.8464(16) 0.087(4) Uani 0.48(3) 1 d D . P A 1
O31B O 0.4766(8) 0.5606(4) 0.7948(14) 0.079(3) Uani 0.52(3) 1 d D . P A 2
N1 N 0.64541(8) 0.63118(6) 0.43545(13) 0.0297(3) Uani 1 1 d . . . . .
N4 N 0.63487(7) 0.57586(6) 0.66475(13) 0.0295(3) Uani 1 1 d . . . . .
N29A N 0.5268(7) 0.6294(8) 0.8246(11) 0.054(3) Uani 0.48(3) 1 d D . P A 1
N29B N 0.5102(6) 0.6103(5) 0.7977(11) 0.0499(19) Uani 0.52(3) 1 d D . P A 2
C2 C 0.65802(10) 0.56355(8) 0.44311(16) 0.0347(4) Uani 1 1 d . . . . .
H2A H 0.710417 0.554893 0.450398 0.042 Uiso 1 1 calc R U . . .
H2B H 0.639743 0.542484 0.368472 0.042 Uiso 1 1 calc R U . . .
C3 C 0.61843(9) 0.53918(7) 0.55506(16) 0.0330(4) Uani 1 1 d . . . . .
H3A H 0.565726 0.540571 0.539650 0.040 Uiso 1 1 calc R U . . .
H3B H 0.632117 0.494793 0.569188 0.040 Uiso 1 1 calc R U . . .
C5 C 0.60915(9) 0.64093(7) 0.65572(15) 0.0300(3) Uani 1 1 d . . . . .
H5 H 0.635855 0.666643 0.717568 0.036 Uiso 1 1 calc R U . . .
C6 C 0.62321(8) 0.66881(7) 0.53078(14) 0.0275(3) Uani 1 1 d . . . . .
C7 C 0.61611(8) 0.73001(7) 0.49134(15) 0.0273(3) Uani 1 1 d . . . . .
C8 C 0.63659(8) 0.73050(7) 0.36456(14) 0.0272(3) Uani 1 1 d . . . . .
C9 C 0.64449(8) 0.77781(8) 0.27577(15) 0.0295(3) Uani 1 1 d . . . . .
H9 H 0.632650 0.820106 0.295099 0.035 Uiso 1 1 calc R U . . .
C10 C 0.66959(9) 0.76262(8) 0.15992(15) 0.0321(3) Uani 1 1 d . . . . .
C11 C 0.68049(10) 0.81201(10) 0.06268(18) 0.0407(4) Uani 1 1 d . . . . .
H11A H 0.678388 0.853818 0.100117 0.061 Uiso 1 1 calc R U . . .
H11B H 0.642407 0.808262 0.000770 0.061 Uiso 1 1 calc R U . . .
H11C H 0.727774 0.806042 0.023944 0.061 Uiso 1 1 calc R U . . .
C12 C 0.68572(10) 0.69934(9) 0.13215(16) 0.0357(4) Uani 1 1 d . . . . .
H12 H 0.701678 0.689246 0.051881 0.043 Uiso 1 1 calc R U . . .
C13 C 0.67926(9) 0.65181(8) 0.21645(16) 0.0339(4) Uani 1 1 d . . . . .
H13 H 0.690849 0.609587 0.196156 0.041 Uiso 1 1 calc R U . . .
C14 C 0.65497(9) 0.66809(8) 0.33327(15) 0.0291(3) Uani 1 1 d . . . . .
C15 C 0.58880(8) 0.78362(7) 0.56432(15) 0.0273(3) Uani 1 1 d . . . . .
C16 C 0.62076(9) 0.80131(7) 0.67446(16) 0.0329(3) Uani 1 1 d . . . . .
H16 H 0.662597 0.779864 0.702671 0.040 Uiso 1 1 calc R U . . .
C17 C 0.59186(12) 0.85017(8) 0.74348(17) 0.0409(4) Uani 1 1 d . . . . .
H17 H 0.613904 0.861632 0.818772 0.049 Uiso 1 1 calc R U . . .
C18 C 0.53170(11) 0.88197(8) 0.70362(19) 0.0427(4) Uani 1 1 d . . . . .
H18 H 0.511907 0.915084 0.751357 0.051 Uiso 1 1 calc R U . . .
C19 C 0.50009(11) 0.86540(8) 0.5932(2) 0.0437(4) Uani 1 1 d . . . . .
H19 H 0.458801 0.887605 0.564909 0.052 Uiso 1 1 calc R U . . .
C20 C 0.52825(9) 0.81668(8) 0.52384(18) 0.0367(4) Uani 1 1 d . . . . .
H20 H 0.506182 0.805744 0.448275 0.044 Uiso 1 1 calc R U . . .
C21 C 0.69951(9) 0.56354(7) 0.72880(14) 0.0270(3) Uani 1 1 d . . . . .
C22 C 0.71385(9) 0.59352(7) 0.84080(15) 0.0309(3) Uani 1 1 d . . . . .
H22 H 0.680776 0.623825 0.871457 0.037 Uiso 1 1 calc R U . . .
C23 C 0.77571(9) 0.57941(8) 0.90719(15) 0.0322(3) Uani 1 1 d . . . . .
H23 H 0.784600 0.600935 0.981867 0.039 Uiso 1 1 calc R U . . .
C24 C 0.82505(9) 0.53452(8) 0.86715(16) 0.0321(3) Uani 1 1 d . . . . .
C25 C 0.89062(10) 0.51717(10) 0.9414(2) 0.0448(4) Uani 1 1 d . . . . .
H25A H 0.879022 0.481517 0.994640 0.067 Uiso 1 1 calc R U . . .
H25B H 0.905309 0.553147 0.991546 0.067 Uiso 1 1 calc R U . . .
H25C H 0.930211 0.505560 0.886250 0.067 Uiso 1 1 calc R U . . .
C26 C 0.81034(9) 0.50485(8) 0.75678(15) 0.0329(3) Uani 1 1 d . . . . .
H26 H 0.842903 0.473801 0.727430 0.039 Uiso 1 1 calc R U . . .
C27 C 0.74963(9) 0.51918(7) 0.68821(15) 0.0302(3) Uani 1 1 d . . . . .
H27 H 0.741955 0.498469 0.612281 0.036 Uiso 1 1 calc R U . . .
C28 C 0.52800(10) 0.64483(9) 0.68538(19) 0.0430(4) Uani 1 1 d D . . . .
H28C H 0.513959 0.689436 0.695199 0.052 Uiso 0.52(3) 1 calc R U P A 2
H28D H 0.499954 0.627209 0.616251 0.052 Uiso 0.52(3) 1 calc R U P A 2
H28A H 0.499985 0.613587 0.637850 0.052 Uiso 0.48(3) 1 calc R U P A 1
H28B H 0.508628 0.687367 0.668962 0.052 Uiso 0.48(3) 1 calc R U P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 0 0.0409
1 1 0 0.0085
1 0 -1 0.2544
1 1 2 0.2818
-1 1 0 0.0559
1 -1 0 0.0481
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 N1 C2 125.28(14) . . ?
C14 N1 C2 126.03(14) . . ?
C14 N1 C6 108.67(13) . . ?
C3 N4 C5 112.41(13) . . ?
C21 N4 C3 118.94(12) . . ?
C21 N4 C5 118.93(13) . . ?
O30A N29A O31A 125.7(8) . . ?
O30A N29A C28 121.7(7) . . ?
O31A N29A C28 112.6(8) . . ?
O30B N29B O31B 125.3(7) . . ?
O30B N29B C28 113.1(6) . . ?
O31B N29B C28 121.6(7) . . ?
N1 C2 H2A 110.1 . . ?
N1 C2 H2B 110.1 . . ?
N1 C2 C3 107.81(14) . . ?
H2A C2 H2B 108.5 . . ?
C3 C2 H2A 110.1 . . ?
C3 C2 H2B 110.1 . . ?
N4 C3 C2 112.21(13) . . ?
N4 C3 H3A 109.2 . . ?
N4 C3 H3B 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N4 C5 H5 108.1 . . ?
N4 C5 C6 112.04(13) . . ?
N4 C5 C28 110.68(14) . . ?
C6 C5 H5 108.1 . . ?
C6 C5 C28 109.71(13) . . ?
C28 C5 H5 108.1 . . ?
N1 C6 C5 120.44(13) . . ?
N1 C6 C7 109.97(14) . . ?
C7 C6 C5 129.58(14) . . ?
C6 C7 C8 106.46(13) . . ?
C6 C7 C15 126.31(14) . . ?
C8 C7 C15 127.14(14) . . ?
C9 C8 C7 134.29(15) . . ?
C9 C8 C14 118.77(14) . . ?
C14 C8 C7 106.86(13) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.85(15) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 C11 121.70(16) . . ?
C9 C10 C12 119.29(15) . . ?
C12 C10 C11 119.01(16) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12 118.7 . . ?
C13 C12 C10 122.68(16) . . ?
C13 C12 H12 118.7 . . ?
C12 C13 H13 121.4 . . ?
C12 C13 C14 117.27(15) . . ?
C14 C13 H13 121.4 . . ?
N1 C14 C8 108.01(13) . . ?
N1 C14 C13 129.86(15) . . ?
C13 C14 C8 122.12(15) . . ?
C16 C15 C7 121.91(14) . . ?
C16 C15 C20 118.60(15) . . ?
C20 C15 C7 119.47(15) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.47(16) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.52(18) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 120.2 . . ?
C17 C18 C19 119.51(17) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.51(18) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 H20 119.8 . . ?
C19 C20 C15 120.39(17) . . ?
C19 C20 H20 119.8 . . ?
C22 C21 N4 120.51(14) . . ?
C27 C21 N4 122.11(14) . . ?
C27 C21 C22 117.28(15) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.83(14) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 119.2 . . ?
C22 C23 C24 121.68(16) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 C25 121.85(16) . . ?
C26 C24 C23 117.17(16) . . ?
C26 C24 C25 120.96(16) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26 119.0 . . ?
C27 C26 C24 121.95(16) . . ?
C27 C26 H26 119.0 . . ?
C21 C27 H27 119.5 . . ?
C26 C27 C21 121.08(15) . . ?
C26 C27 H27 119.5 . . ?
N29A C28 H28A 111.4 . . ?
N29A C28 H28B 111.4 . . ?
N29B C28 C5 111.6(5) . . ?
N29B C28 H28C 109.3 . . ?
N29B C28 H28D 109.3 . . ?
C5 C28 N29A 102.0(5) . . ?
C5 C28 H28C 109.3 . . ?
C5 C28 H28D 109.3 . . ?
C5 C28 H28A 111.4 . . ?
C5 C28 H28B 111.4 . . ?
H28C C28 H28D 108.0 . . ?
H28A C28 H28B 109.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O30A N29A 1.220(10) . ?
O30B N29B 1.224(9) . ?
O31A N29A 1.239(10) . ?
O31B N29B 1.227(8) . ?
N1 C2 1.460(2) . ?
N1 C6 1.376(2) . ?
N1 C14 1.376(2) . ?
N4 C3 1.462(2) . ?
N4 C5 1.468(2) . ?
N4 C21 1.410(2) . ?
N29A C28 1.556(10) . ?
N29B C28 1.468(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.517(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 H5 1.0000 . ?
C5 C6 1.511(2) . ?
C5 C28 1.538(2) . ?
C6 C7 1.378(2) . ?
C7 C8 1.436(2) . ?
C7 C15 1.481(2) . ?
C8 C9 1.406(2) . ?
C8 C14 1.413(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(2) . ?
C10 C11 1.508(2) . ?
C10 C12 1.412(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 0.9500 . ?
C12 C13 1.373(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.397(2) . ?
C15 C16 1.393(2) . ?
C15 C20 1.395(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.391(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.373(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.386(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.405(2) . ?
C21 C27 1.396(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.392(2) . ?
C24 C25 1.505(2) . ?
C24 C26 1.388(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?
C26 C27 1.384(2) . ?
C27 H27 0.9500 . ?
C28 H28C 0.9900 . ?
C28 H28D 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O30A N29A C28 C5 71.8(9) . . . . ?
O30B N29B C28 C5 69.2(8) . . . . ?
O31A N29A C28 C5 -107.4(7) . . . . ?
O31B N29B C28 C5 -108.3(8) . . . . ?
N1 C2 C3 N4 -50.43(18) . . . . ?
N1 C6 C7 C8 -1.23(18) . . . . ?
N1 C6 C7 C15 175.70(14) . . . . ?
N4 C5 C6 N1 10.8(2) . . . . ?
N4 C5 C6 C7 -170.45(16) . . . . ?
N4 C5 C28 N29A 68.7(7) . . . . ?
N4 C5 C28 N29B 47.7(7) . . . . ?
N4 C21 C22 C23 176.91(15) . . . . ?
N4 C21 C27 C26 -175.63(15) . . . . ?
C2 N1 C6 C5 -0.5(2) . . . . ?
C2 N1 C6 C7 -179.50(15) . . . . ?
C2 N1 C14 C8 179.77(15) . . . . ?
C2 N1 C14 C13 -1.3(3) . . . . ?
C3 N4 C5 C6 -41.86(18) . . . . ?
C3 N4 C5 C28 80.94(17) . . . . ?
C3 N4 C21 C22 -173.88(14) . . . . ?
C3 N4 C21 C27 2.5(2) . . . . ?
C5 N4 C3 C2 64.82(17) . . . . ?
C5 N4 C21 C22 42.7(2) . . . . ?
C5 N4 C21 C27 -140.89(15) . . . . ?
C5 C6 C7 C8 179.93(15) . . . . ?
C5 C6 C7 C15 -3.1(3) . . . . ?
C6 N1 C2 C3 19.6(2) . . . . ?
C6 N1 C14 C8 -1.41(17) . . . . ?
C6 N1 C14 C13 177.56(17) . . . . ?
C6 C5 C28 N29A -167.2(7) . . . . ?
C6 C5 C28 N29B 171.8(6) . . . . ?
C6 C7 C8 C9 -176.09(17) . . . . ?
C6 C7 C8 C14 0.34(17) . . . . ?
C6 C7 C15 C16 57.4(2) . . . . ?
C6 C7 C15 C20 -120.96(19) . . . . ?
C7 C8 C9 C10 176.41(17) . . . . ?
C7 C8 C14 N1 0.65(17) . . . . ?
C7 C8 C14 C13 -178.42(15) . . . . ?
C7 C15 C16 C17 -177.18(16) . . . . ?
C7 C15 C20 C19 177.42(16) . . . . ?
C8 C7 C15 C16 -126.26(18) . . . . ?
C8 C7 C15 C20 55.3(2) . . . . ?
C8 C9 C10 C11 -178.61(15) . . . . ?
C8 C9 C10 C12 1.1(2) . . . . ?
C9 C8 C14 N1 177.74(14) . . . . ?
C9 C8 C14 C13 -1.3(2) . . . . ?
C9 C10 C12 C13 -1.6(3) . . . . ?
C10 C12 C13 C14 0.6(3) . . . . ?
C11 C10 C12 C13 178.10(17) . . . . ?
C12 C13 C14 N1 -177.99(16) . . . . ?
C12 C13 C14 C8 0.9(2) . . . . ?
C14 N1 C2 C3 -161.74(15) . . . . ?
C14 N1 C6 C5 -179.37(14) . . . . ?
C14 N1 C6 C7 1.67(18) . . . . ?
C14 C8 C9 C10 0.3(2) . . . . ?
C15 C7 C8 C9 7.0(3) . . . . ?
C15 C7 C8 C14 -176.55(15) . . . . ?
C15 C16 C17 C18 -0.5(3) . . . . ?
C16 C15 C20 C19 -1.0(3) . . . . ?
C16 C17 C18 C19 -0.5(3) . . . . ?
C17 C18 C19 C20 0.7(3) . . . . ?
C18 C19 C20 C15 0.1(3) . . . . ?
C20 C15 C16 C17 1.2(2) . . . . ?
C21 N4 C3 C2 -80.85(17) . . . . ?
C21 N4 C5 C6 103.81(16) . . . . ?
C21 N4 C5 C28 -133.39(16) . . . . ?
C21 C22 C23 C24 -1.2(2) . . . . ?
C22 C21 C27 C26 0.9(2) . . . . ?
C22 C23 C24 C25 -177.45(16) . . . . ?
C22 C23 C24 C26 0.8(2) . . . . ?
C23 C24 C26 C27 0.4(2) . . . . ?
C24 C26 C27 C21 -1.3(3) . . . . ?
C25 C24 C26 C27 178.71(16) . . . . ?
C27 C21 C22 C23 0.3(2) . . . . ?
C28 C5 C6 N1 -112.54(17) . . . . ?
C28 C5 C6 C7 66.2(2) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.1(3)
2 -0.1(3)
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9995 -1.0001 0.0000 -0.0166 -0.1011 0.0407
0.9995 1.0001 -0.0000 0.0166 0.1011 -0.0407
0.9998 -0.0005 -0.9999 -0.0594 0.1174 0.0975
0.9989 1.0012 1.9997 0.0467 -0.0079 -0.2991
-0.9996 1.0001 -0.0000 0.1051 -0.0247 0.0226
0.9996 -1.0001 0.0000 -0.1051 0.0247 -0.0226
