Synthesis of Bi-, Ter-, and Quaterpyridinecarboxylates via Propargylisoxazole-Pyridine Rearrangement.
Galenko, Ekaterina E.; Kryukova, Mariya A.; Novikov, Mikhail S.; Khlebnikov, Alexander F.; The Journal of organic chemistry 85 (2020) 6109–6122; doi:10.1021/acs.joc.0c00611

data_4038261
_publ_section_title
;
 Synthesis of Bi-, Ter-, and Quaterpyridinecarboxylates via
 Propargylisoxazole-Pyridine Rearrangement.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6109
_journal_page_last               6122
_journal_paper_doi               10.1021/acs.joc.0c00611
_journal_volume                  85
_journal_year                    2020
_chemical_formula_moiety         'C27 H19 N3 O4 S'
_chemical_formula_sum            'C27 H19 N3 O4 S'
_chemical_formula_weight         481.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                107.6500(10)
_cell_angle_beta                 107.1590(10)
_cell_angle_gamma                93.5990(10)
_cell_formula_units_Z            2
_cell_length_a                   8.87440(10)
_cell_length_b                   11.65640(10)
_cell_length_c                   11.83170(10)
_cell_measurement_reflns_used    26193
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      76.6110
_cell_measurement_theta_min      4.0380
_cell_volume                     1098.70(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -14.00  11.00   0.50    0.11    --   47.20 -21.00 -81.00   50
  2  \w     36.00  79.00   0.50    0.42    --  107.75 -77.00   0.00   86
  3  \w     57.00  97.00   0.50    0.42    --  107.75 -77.00  30.00   80
  4  \w     71.00 102.00   0.50    0.42    --  107.75-125.00 -60.00   62
  5  \w     81.00 106.00   0.50    0.42    --  107.75 -94.00-120.00   50
  6  \w     56.00 112.00   0.50    0.42    --  107.75-125.00-150.00  112
  7  \w     35.00  60.00   0.50    0.42    --  107.75 -61.00-180.00   50
  8  \w    106.00 177.00   0.50    0.42    --  107.75  30.00-150.00  142
  9  \w     95.00 175.00   0.50    0.42    --  107.75  30.00   0.00  160
 10  \w     96.00 178.00   0.50    0.42    --  107.75  21.00  84.00  164
 11  \w    105.00 146.00   0.50    0.42    --  107.75  45.00 150.00   82
 12  \w     44.00  69.00   0.50    0.42    --  107.75 -61.00   0.00   50
 13  \w     39.00  64.00   0.50    0.42    --  107.75 -61.00  60.00   50
 14  \w     46.00  71.00   0.50    0.42    --  107.75 -61.00  90.00   50
 15  \w     37.00  69.00   0.50    0.42    --  107.75 -94.00 120.00   64
 16  \w     36.00  71.00   0.50    0.42    --  107.75 -61.00 150.00   70
 17  \w     36.00 112.00   0.50    0.11    --   47.20  21.00  84.00  152
 18  \w     50.00  95.00   0.50    0.11    --   47.20-125.00 120.00   90
 19  \w     39.00 111.00   0.50    0.42    --  107.75-125.00  30.00  144
 20  \w     36.00  61.00   0.50    0.42    --  107.75-125.00 -60.00   50
 21  \w      1.00  32.00   0.50    0.11    --   47.20 -37.00  60.00   62
 22  \w    -19.00  23.00   0.50    0.11    --  -47.20  21.00  84.00   84
 23  \w    -67.00  24.00   0.50    0.11    --  -47.20  77.00 -60.00  182
 24  \w    -25.00   1.00   0.50    0.11    --  -47.20  37.00-150.00   52
 25  \w    -40.00  26.00   0.50    0.11    --  -47.20  37.00-120.00  132
 26  \w    -68.00 -34.00   0.50    0.42    -- -106.00  61.00-120.00   68
 27  \w    -61.00 -35.00   0.50    0.42    -- -106.00  77.00-120.00   52
 28  \w    -71.00 -45.00   0.50    0.42    -- -106.00 135.00 -45.56   52
 29  \w    -88.00 -37.00   0.50    0.42    -- -106.00 125.00   0.00  102
 30  \w    -63.00 -38.00   0.50    0.42    -- -106.00 139.00  61.92   50
 31  \w    -84.00 -58.00   0.50    0.42    -- -106.00  77.00 150.00   52
 32  \w   -108.00 -83.00   0.50    0.42    -- -106.00 112.00 106.58   50
 33  \w   -108.00 -64.00   0.50    0.42    -- -106.00 112.00 133.44   88
 34  \w   -112.00 -49.00   0.50    0.42    -- -106.00 125.00  30.00  126
 35  \w    -69.00 -40.00   0.50    0.42    -- -106.00  61.00 -60.00   58
 36  \w    -71.00 -41.00   0.50    0.42    -- -106.00  61.00 -30.00   60
 37  \w    -84.00 -35.00   0.50    0.11    --  -47.20 -21.00 -81.00   98
 38  \w   -119.00 -93.00   0.50    0.11    --  -47.20 -21.00 -81.00   52
 39  \w   -125.00 -99.00   0.50    0.42    -- -106.00 -94.00 -30.00   52
 40  \w   -174.00-117.00   0.50    0.42    -- -106.00 -21.00 -81.00  114
 41  \w   -173.00-148.00   0.50    0.42    -- -106.00 -94.00 -30.00   50
 42  \w   -177.00-113.00   0.50    0.42    -- -106.00 -15.00 150.00  128
 43  \w   -119.00 -87.00   0.50    0.42    -- -106.00 135.00 -45.56   64
 44  \w   -108.00 -57.00   0.50    0.42    -- -106.00 115.00-107.64  102
 45  \w   -104.00 -64.00   0.50    0.42    -- -106.00  77.00-120.00   80
 46  \w   -107.00 -38.00   0.50    0.42    -- -106.00 106.00-132.70  138
 47  \w   -118.00 -33.00   0.50    0.42    -- -106.00 134.00 -86.78  170
 48  \w   -122.00 -97.00   0.50    0.42    -- -106.00 139.00  61.92   50
 49  \w   -125.00-100.00   0.50    0.42    -- -106.00 143.00 -13.85   50
 50  \w   -120.00 -94.00   0.50    0.42    -- -106.00 136.00-151.32   52
 51  \w   -103.00 -78.00   0.50    0.11    --  -47.20 -21.00 -81.00   50
 52  \w    -17.00  12.00   0.50    0.11    --   18.00 102.00 164.39   58
 53  \w    -41.00 -15.00   0.50    0.11    --  -42.00 -87.00-135.09   52
 54  \w     17.00  42.00   0.50    0.11    --   46.00  90.00  -0.84   50
 55  \w     17.00  42.00   0.50    0.11    --   46.00  90.00  74.81   50
 56  \w    -60.00 -35.00   0.50    0.11    --  -47.20 -37.00  30.00   50
 57  \w     39.00  75.00   0.50    0.11    --   47.20  37.00 -30.00   72
 58  \w     32.00  58.00   0.50    0.11    --   47.20  57.00   0.00   52
 59  \w     38.00  65.00   0.50    0.11    --   47.20  19.00-180.00   54
 60  \w     27.00  53.00   0.50    0.11    --   50.00  78.00  40.44   52
 61  \w     27.00  53.00   0.50    0.11    --   50.00  77.00  99.26   52
 62  \w     31.00  57.00   0.50    0.11    --   54.00  79.00-165.17   52
 63  \w     30.00  56.00   0.50    0.11    --   54.00  79.00 -49.60   52
 64  \w     81.00 126.00   0.50    0.11    --   54.00  79.00-165.17   90
 65  \w     32.00  58.00   0.50    0.11    --   54.00  78.00-119.11   52
 66  \w     32.00  58.00   0.50    0.11    --   54.00  77.00 113.02   52
 67  \w     87.00 113.00   0.50    0.11    --   54.00  78.00-119.11   52
 68  \w     32.00  58.00   0.50    0.11    --   54.00  78.00 140.07   52
 69  \w     31.00  56.00   0.50    0.11    --   54.00  77.00 -77.15   50
 70  \w     31.00  57.00   0.50    0.11    --   54.00  77.00   6.71   52
 71  \w     35.00  61.00   0.50    0.11    --   54.00  75.00 171.52   52
 72  \w     38.00  64.00   0.50    0.11    --   58.00  74.00-101.93   52
 73  \w    -63.00 -38.00   0.50    0.11    --  -62.00 -79.00 121.71   50
 74  \w   -129.00-103.00   0.50    0.11    --  -62.00 -79.00 121.71   52
 75  \w    -73.00 -48.00   0.50    0.11    --  -66.00 -66.00  92.27   50
 76  \w    -73.00 -48.00   0.50    0.11    --  -66.00 -66.00-107.80   50
 77  \w    -72.00 -47.00   0.50    0.11    --  -66.00 -67.00-120.59   50
 78  \w    -73.00 -48.00   0.50    0.11    --  -66.00 -64.00  69.75   50
 79  \w   -139.00 -96.00   0.50    0.11    --  -66.00 -66.00-107.80   86
 80  \w     43.00  69.00   0.50    0.11    --   66.00  78.00  25.29   52
 81  \w     42.00  68.00   0.50    0.11    --   66.00  80.00 -36.83   52
 82  \w    -71.00 -46.00   0.50    0.11    --  -70.00 -79.00 152.06   50
 83  \w    -77.00 -51.00   0.50    0.11    --  -70.00 -68.00-170.12   52
 84  \w    -79.00 -53.00   0.50    0.11    --  -70.00 -66.00 104.61   52
 85  \w    -74.00 -47.00   0.50    0.11    --  -70.00 -78.00-118.19   54
 86  \w    -79.00 -53.00   0.50    0.11    --  -70.00 -67.00 174.04   52
 87  \w     48.00  73.00   0.50    0.11    --   70.00  76.00  62.89   50
 88  \w     47.00  72.00   0.50    0.11    --   70.00  77.00  91.25   50
 89  \w    117.00 143.00   0.50    0.11    --   70.00  77.00  91.25   52
 90  \w     82.00 108.00   0.50    0.11    --   70.00  76.00 -11.03   52
 91  \w     49.00  75.00   0.50    0.11    --   70.00  76.00 -11.03   52
 92  \w    -84.00 -58.00   0.50    0.11    --  -74.00 -65.00 115.72   52
 93  \w   -133.00-107.00   0.50    0.11    --  -74.00 -74.00-131.83   52
 94  \w    -77.00 -52.00   0.50    0.11    --  -74.00 -74.00-131.83   50
 95  \w    -84.00 -58.00   0.50    0.11    --  -74.00 -64.00-110.14   52
 96  \w    -80.00 -54.00   0.50    0.11    --  -74.00 -75.00  50.12   52
 97  \w     55.00  81.00   0.50    0.11    --   74.00  74.00-144.88   52
 98  \w    -86.00 -60.00   0.50    0.42    --  -78.00 -70.00 175.75   52
 99  \w    -83.00 -57.00   0.50    0.42    --  -78.00 -73.00  12.61   52
100  \w    -87.00 -62.00   0.50    0.42    --  -78.00 -63.00  96.19   50
101  \w    -96.00 -67.00   0.50    0.42    --  -82.00 -63.00-102.05   58
102  \w    -90.00 -65.00   0.50    0.42    --  -82.00 -61.00  63.31   50
103  \w    -92.00 -66.00   0.50    0.42    --  -82.00 -66.00-138.63   52
104  \w    -87.00 -61.00   0.50    0.42    --  -82.00 -74.00 -44.35   52
105  \w    -87.00 -61.00   0.50    0.42    --  -82.00 -72.00 -77.23   52
106  \w    -85.00 -60.00   0.50    0.42    --  -82.00 -74.00  64.63   50
107  \w    -90.00 -64.00   0.50    0.42    --  -82.00 -66.00 157.17   52
108  \w    -90.00 -65.00   0.50    0.42    --  -86.00 -73.00 -23.67   50
109  \w    -90.00 -65.00   0.50    0.42    --  -86.00 -73.00 -10.27   50
110  \w   -101.00 -72.00   0.50    0.42    --  -90.00 -65.00-126.74   58
111  \w   -100.00 -74.00   0.50    0.42    --  -90.00 -63.00  98.25   52
112  \w   -100.00 -74.00   0.50    0.42    --  -90.00 -62.00  89.61   52
113  \w    -98.00 -72.00   0.50    0.42    --  -90.00 -66.00 151.28   52
114  \w    -97.00 -72.00   0.50    0.42    --  -90.00 -66.00 140.20   50
115  \w    -95.00 -69.00   0.50    0.42    --  -90.00 -76.00 -47.88   52
116  \w    -93.00 -68.00   0.50    0.42    --  -90.00 -74.00   9.29   50
117  \w   -150.00-124.00   0.50    0.42    --  -90.00 -74.00   9.29   52
118  \w    -97.00 -71.00   0.50    0.42    --  -90.00 -67.00 162.98   52
119  \w    -96.00 -70.00   0.50    0.42    --  -90.00 -71.00 130.78   52
120  \w   -100.00 -72.00   0.50    0.42    --  -90.00 -64.00-103.25   56
121  \w    -93.00 -68.00   0.50    0.42    --  -90.00 -74.00  51.10   50
122  \w   -105.00 -75.00   0.50    0.42    --  -94.00 -68.00-135.42   60
123  \w   -105.00 -75.00   0.50    0.42    --  -94.00 -68.00-169.28   60
124  \w   -101.00 -76.00   0.50    0.42    --  -94.00 -64.00  88.35   50
125  \w    -97.00 -71.00   0.50    0.42    --  -94.00 -76.00  74.94   52
126  \w   -164.00-138.00   0.50    0.42    --  -94.00 -76.00  74.94   52
127  \w   -102.00 -76.00   0.50    0.42    --  -94.00 -66.00 114.43   52
128  \w   -113.00 -74.00   0.50    0.42    --  -98.00 -79.00 -32.50   78
129  \w   -156.00-130.00   0.50    0.42    --  -98.00 -79.00 -32.50   52
130  \w   -104.00 -79.00   0.50    0.42    --  -98.00 -69.00-124.39   50
131  \w   -101.00 -75.00   0.50    0.42    --  -98.00 -76.00  69.20   52
132  \w   -104.00 -78.00   0.50    0.42    --  -98.00 -69.00-177.89   52
133  \w   -105.00 -79.00   0.50    0.42    -- -102.00 -78.00  41.05   52
134  \w   -158.00-132.00   0.50    0.42    -- -102.00 -78.00  41.05   52
135  \w    -62.00 -36.00   0.50    0.42    -- -106.00  61.00   0.00   52
136  \w   -118.00 -79.00   0.50    0.42    -- -106.00 -85.00  31.95   78
137  \w   -127.00 -88.00   0.50    0.42    -- -106.00 -66.00  51.60   78
138  \w   -167.00-126.00   0.50    0.42    -- -106.00 -85.00  31.95   82
139  \w   -130.00 -83.00   0.50    0.42    -- -106.00 -77.00  30.00   94
140  \w   -174.00-142.00   0.50    0.42    -- -106.00 -66.00  51.60   64
141  \w   -153.00 -86.00   0.50    0.42    -- -106.00 -74.00-140.42  134
142  \w   -118.00 -82.00   0.50    0.42    -- -106.00 -81.00 159.86   72
143  \w   -132.00 -84.00   0.50    0.42    -- -106.00 -77.00 125.43   96
144  \w   -111.00 -83.00   0.50    0.42    -- -106.00 -77.00-120.00   56
145  \w   -119.00 -82.00   0.50    0.42    -- -106.00 -80.00 -44.17   74
146  \w   -170.00-129.00   0.50    0.42    -- -106.00 -80.00 -44.17   82
147  \w   -114.00 -88.00   0.50    0.42    -- -106.00 -65.00-118.12   52
148  \w   -167.00-104.00   0.50    0.42    -- -106.00 -72.00  70.23  126
149  \w   -109.00 -81.00   0.50    0.42    -- -106.00 -81.00-126.75   56
150  \w   -147.00-115.00   0.50    0.42    -- -106.00 -81.00-126.75   64
151  \w   -134.00 -85.00   0.50    0.42    -- -106.00 -73.00 137.87   98
152  \w   -108.00 -83.00   0.50    0.42    -- -106.00 109.00-169.51   50
153  \w   -105.00 -80.00   0.50    0.42    -- -106.00 -83.00-153.62   50
154  \w   -119.00 -82.00   0.50    0.42    -- -106.00 -80.00 -87.29   74
155  \w   -113.00 -81.00   0.50    0.42    -- -106.00 -82.00  11.70   64
156  \w   -165.00-129.00   0.50    0.42    -- -106.00 -80.00 -87.29   72
157  \w   -109.00 -83.00   0.50    0.42    -- -106.00 -78.00  -8.86   52
158  \w   -169.00-116.00   0.50    0.42    -- -106.00 -78.00  -8.86  106
159  \w   -110.00 -84.00   0.50    0.42    -- -106.00 -74.00 163.87   52
160  \w   -112.00 -87.00   0.50    0.42    -- -106.00 -70.00 103.63   50
161  \w   -115.00 -86.00   0.50    0.42    -- -106.00 -70.00 -65.75   58
162  \w   -163.00-135.00   0.50    0.42    -- -106.00 -70.00 103.63   56
163  \w   -113.00 -84.00   0.50    0.42    -- -106.00 -75.00 172.32   58
164  \w   -123.00 -91.00   0.50    0.42    -- -106.00 -61.00-120.00   64
165  \w   -173.00-147.00   0.50    0.42    -- -106.00 -75.00 172.32   52
166  \w   -132.00 -90.00   0.50    0.42    -- -106.00 -66.00-166.44   84
167  \w   -127.00-102.00   0.50    0.42    -- -106.00 -15.00 -90.00   50
168  \w   -175.00-150.00   0.50    0.42    -- -106.00 -15.00 -90.00   50
169  \w   -109.00 -84.00   0.50    0.42    -- -106.00 -74.00  48.73   50
170  \w   -104.00 -79.00   0.50    0.42    -- -106.00 -88.00 117.94   50
171  \w   -164.00-138.00   0.50    0.42    -- -106.00 -66.00-166.44   52
172  \w   -141.00-115.00   0.50    0.42    -- -106.00 -88.00 117.94   52
173  \w    153.00 178.00   0.50    0.42    --  107.75  77.00 -90.00   50
174  \w     85.00 112.00   0.50    0.42    --  107.75  77.00 -90.00   54
175  \w    145.00 175.00   0.50    0.42    --  107.75  77.00  60.00   60
176  \w     85.00 131.00   0.50    0.42    --  107.75  77.00  60.00   92
177  \w    141.00 166.00   0.50    0.42    --  107.75  61.00  90.00   50
178  \w     98.00 124.00   0.50    0.42    --  107.75  61.00  90.00   52
179  \w    140.00 175.00   0.50    0.42    --  107.75  45.00 -60.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1028027000
_diffrn_orient_matrix_UB_12      0.0400455000
_diffrn_orient_matrix_UB_13      0.1397745000
_diffrn_orient_matrix_UB_21      -0.1529083000
_diffrn_orient_matrix_UB_22      0.0011842000
_diffrn_orient_matrix_UB_23      0.0365397000
_diffrn_orient_matrix_UB_31      -0.0029530000
_diffrn_orient_matrix_UB_32      -0.1348472000
_diffrn_orient_matrix_UB_33      -0.0091176000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44689
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.778
_diffrn_reflns_theta_min         4.037
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       plate
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.6268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4280
_reflns_number_total             4591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c00611_si_003.cif
_cod_data_source_block           15444_14.11
_cod_depositor_comments
'Adding full bibliography for 4038260--4038261.cif.'
_cod_database_code               4038261
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C27 H19 N3 O4 S '
_diffrn_oxdiff_digest_frames
;
01bbdc61ec36debb5bbf67b598d3b70ba10005008bb
;
_diffrn_oxdiff_digest_hkl
;
0115f997b2e852181a83f5863d0a8d333077d8
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C26(H26), C16(H16), C17(H17), C5(H5), C25(H25), C20(H20),
 C23(H23), C27(H27), C6(H6), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              90968
_shelx_hkl_checksum              48579
_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 1.519
_oxdiff_exptl_absorpt_empirical_full_min 0.391