Zipping up Tetraazaperylene: Synthesis of Tetraazacoronenes via Double Coupling in the Bay Positions
Eichelmann, Robert; Rippel, Daniel; Ballmann, Joachim; Gade, Lutz H.; Chemical Communications  (2023) –; doi:10.1039/D3CC04113A

data_7132141
_publ_section_title
;
 Zipping up Tetraazaperylene: Synthesis of Tetraazacoronenes via Double
 Coupling in the Bay Positions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04113A
_journal_year                    2023
_chemical_formula_moiety         'C74 H80 N8 O6, 1[CH2Cl2], 1[CH3OH], 0.5[OH2]'
_chemical_formula_sum            'C76 H87 Cl2 N8 O7.5'
_chemical_formula_weight         1303.43
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-23 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.6270(10)
_cell_angle_beta                 96.5330(10)
_cell_angle_gamma                91.8250(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3834(2)
_cell_length_b                   15.0836(2)
_cell_length_c                   17.5480(2)
_cell_measurement_reflns_used    30195
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.8230
_cell_measurement_theta_min      3.9720
_cell_volume                     3364.53(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_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    -22.00  54.00   1.00    4.00    --    0.00  46.00-120.00   76
  2  \w    -59.00 -22.00   1.00    4.00    --    0.00 -46.00  90.00   37
  3  \w     54.00  79.00   1.00    8.00    --   54.49  46.00-120.00   25
  4  \w    -16.00  78.00   1.00    8.00    --   54.49 -46.00  90.00   94
  5  \w    108.00 133.00   1.00   16.00    --  108.98  46.00-120.00   25
  6  \w     46.00 132.00   1.00   16.00    --  108.98 -46.00  90.00   86
  7  \w    -19.00  23.00   1.00    4.00    --    0.00 -46.00  90.00   42
  8  \w    -17.00  13.00   1.00    4.00    --    0.00  57.00 120.00   30
  9  \w     17.00  68.00   1.00    4.00    --    0.00  57.00 120.00   51
 10  \w    -40.00  -1.00   1.00    4.00    --    0.00 -77.00  60.00   39
 11  \w    -19.00  29.00   1.00    4.00    --    0.00  57.00 -90.00   48
 12  \w     33.00  66.00   1.00    4.00    --    0.00  57.00 -90.00   33
 13  \w    -24.00   8.00   1.00    4.00    --   18.00 104.00  84.13   32
 14  \w     -8.00  17.00   1.00    8.00    --   34.00 102.00 -96.28   25
 15  \w      6.00  31.00   1.00    8.00    --   42.00  88.00-147.12   25
 16  \w      6.00  31.00   1.00    8.00    --   42.00  88.00   7.05   25
 17  \w      6.00  31.00   1.00    8.00    --   42.00  88.00 121.09   25
 18  \w     13.00  38.00   1.00    8.00    --   46.00  83.00 -80.95   25
 19  \w     15.00  43.00   1.00    8.00    --   46.00  82.00 133.44   28
 20  \w     12.00  37.00   1.00    8.00    --   46.00  84.00 -44.64   25
 21  \w     13.00  38.00   1.00    8.00    --   46.00  83.00   9.86   25
 22  \w     17.00  44.00   1.00    8.00    --   46.00  79.00 178.07   27
 23  \w     14.00  39.00   1.00    8.00    --   46.00  81.00 104.51   25
 24  \w     18.00  43.00   1.00    8.00    --   50.00  80.00-118.04   25
 25  \w     19.00  44.00   1.00    8.00    --   50.00  79.00 159.41   25
 26  \w     17.00  42.00   1.00    8.00    --   50.00  82.00 -45.67   25
 27  \w     18.00  43.00   1.00    8.00    --   50.00  81.00  57.07   25
 28  \w     18.00  43.00   1.00    8.00    --   50.00  80.00-152.97   25
 29  \w     61.00 110.00   1.00    8.00    --   54.49-125.00  90.00   49
 30  \w     24.00  51.00   1.00    8.00    --   54.49  77.00 120.00   27
 31  \w     24.00  51.00   1.00    8.00    --   54.49  77.00-150.00   27
 32  \w    -15.00  84.00   1.00    8.00    --   54.49 -77.00-120.00   99
 33  \w     29.00  56.00   1.00    8.00    --   54.49  77.00-180.00   27
 34  \w     25.00  51.00   1.00    8.00    --   54.49  77.00   0.00   26
 35  \w    -14.00  76.00   1.00    8.00    --   54.49 -57.00   0.00   90
 36  \w     27.00  54.00   1.00    8.00    --   54.49  77.00 -30.00   27
 37  \w     43.00  70.00   1.00    8.00    --   54.49-125.00 -90.00   27
 38  \w     29.00  56.00   1.00    8.00    --   58.00  77.00  19.28   27
 39  \w     28.00  57.00   1.00    8.00    --   58.00  77.00  55.96   29
 40  \w     30.00  55.00   1.00    8.00    --   58.00  76.00-118.86   25
 41  \w     30.00  57.00   1.00    8.00    --   58.00  77.00 -93.77   27
 42  \w     28.00  55.00   1.00    8.00    --   58.00  77.00 -70.76   27
 43  \w     31.00  56.00   1.00    8.00    --   58.00  73.00-158.93   25
 44  \w     30.00  55.00   1.00    8.00    --   58.00  76.00  78.27   25
 45  \w     79.00 107.00   1.00    8.00    --   58.00  77.00  19.28   28
 46  \w     28.00  55.00   1.00    8.00    --   58.00  77.00  90.62   27
 47  \w     30.00  57.00   1.00    8.00    --   58.00  77.00-107.97   27
 48  \w     30.00  55.00   1.00    8.00    --   58.00  75.00  91.04   25
 49  \w     33.00  69.00   1.00    8.00    --   62.00  75.00 -57.80   36
 50  \w     34.00  59.00   1.00    8.00    --   62.00  76.00 109.37   25
 51  \w     34.00  64.00   1.00    8.00    --   62.00  75.00 -16.06   30
 52  \w     36.00  63.00   1.00    8.00    --   62.00  76.00 -38.29   27
 53  \w     33.00  59.00   1.00    8.00    --   62.00  76.00-157.65   26
 54  \w     33.00  59.00   1.00    8.00    --   62.00  76.00 160.77   26
 55  \w     34.00  61.00   1.00    8.00    --   62.00  77.00  21.69   27
 56  \w     35.00  62.00   1.00    8.00    --   62.00  77.00  -3.94   27
 57  \w     33.00  60.00   1.00    8.00    --   62.00  77.00-148.38   27
 58  \w     41.00  68.00   1.00    8.00    --   62.00  70.00 -78.30   27
 59  \w     38.00  65.00   1.00    8.00    --   66.00  76.00  62.52   27
 60  \w     43.00  75.00   1.00    8.00    --   66.00  67.00   2.52   32
 61  \w     36.00  63.00   1.00    8.00    --   66.00  77.00   6.66   27
 62  \w     37.00  62.00   1.00    8.00    --   66.00  77.00 163.87   25
 63  \w     43.00  70.00   1.00    8.00    --   66.00  76.00-144.44   27
 64  \w     37.00  81.00   1.00    8.00    --   66.00  76.00 125.96   44
 65  \w     40.00  67.00   1.00    8.00    --   66.00  74.00-114.67   27
 66  \w     43.00  70.00   1.00    8.00    --   70.00  71.00  81.30   27
 67  \w     40.00  67.00   1.00    8.00    --   70.00  77.00 133.99   27
 68  \w     45.00  77.00   1.00    8.00    --   70.00  72.00 -66.88   32
 69  \w     47.00  72.00   1.00    8.00    --   70.00  67.00-113.69   25
 70  \w     48.00  73.00   1.00    8.00    --   70.00  64.00-117.32   25
 71  \w    111.00 139.00   1.00    8.00    --   70.00  75.00  41.97   28
 72  \w     46.00  73.00   1.00    8.00    --   70.00  73.00-105.45   27
 73  \w     44.00  70.00   1.00    8.00    --   70.00  71.00 -37.24   26
 74  \w     43.00  70.00   1.00    8.00    --   70.00  73.00 -52.37   27
 75  \w     42.00 100.00   1.00    8.00    --   70.00  75.00  41.97   58
 76  \w     47.00  74.00   1.00    8.00    --   74.00  75.00 -15.13   27
 77  \w     47.00  78.00   1.00    8.00    --   74.00  73.00-173.14   31
 78  \w     44.00 128.00   1.00    8.00    --   74.00  77.00 126.48   84
 79  \w     46.00  73.00   1.00    8.00    --   74.00  77.00 -41.52   27
 80  \w     47.00 103.00   1.00    8.00    --   74.00  73.00  26.19   56
 81  \w     44.00  71.00   1.00    8.00    --   74.00  77.00  75.11   27
 82  \w     45.00  79.00   1.00    8.00    --   74.00  76.00  -2.19   34
 83  \w     52.00  78.00   1.00    8.00    --   74.00  48.00-107.15   26
 84  \w     50.00  79.00   1.00    8.00    --   74.00  67.00 179.41   29
 85  \w     50.00  75.00   1.00    8.00    --   74.00  69.00 -90.68   25
 86  \w     56.00  85.00   1.00    8.00    --   74.00  56.00  66.77   29
 87  \w     45.00  71.00   1.00    8.00    --   74.00  76.00-126.45   26
 88  \w     57.00  90.00   1.00    8.00    --   78.00  68.00  95.60   33
 89  \w     57.00 102.00   1.00    8.00    --   78.00  66.00-169.62   45
 90  \w     50.00  77.00   1.00    8.00    --   78.00  76.00 -61.68   27
 91  \w     54.00 117.00   1.00    8.00    --   78.00  68.00-114.54   63
 92  \w     49.00  76.00   1.00    8.00    --   78.00  76.00   7.23   27
 93  \w     53.00  82.00   1.00   16.00    --   82.00  77.00 -38.63   29
 94  \w     61.00  87.00   1.00   16.00    --   82.00  43.00 -75.98   26
 95  \w     52.00  78.00   1.00   16.00    --   82.00  77.00 -89.59   26
 96  \w     59.00 149.00   1.00   16.00    --   82.00  68.00 -66.30   90
 97  \w     61.00  88.00   1.00   16.00    --   82.00  61.00  26.63   27
 98  \w     65.00  92.00   1.00   16.00    --   86.00  57.00  62.48   27
 99  \w     58.00 130.00   1.00   16.00    --   86.00  73.00  93.86   72
100  \w     59.00  95.00   1.00   16.00    --   86.00  74.00 -36.43   36
101  \w     64.00 105.00   1.00   16.00    --   86.00  62.00-127.42   41
102  \w     62.00  89.00   1.00   16.00    --   86.00  72.00 155.48   27
103  \w     60.00 116.00   1.00   16.00    --   86.00  75.00  -2.38   56
104  \w     58.00  87.00   1.00   16.00    --   86.00  73.00 -16.61   29
105  \w     64.00  90.00   1.00   16.00    --   86.00  48.00  74.10   26
106  \w     62.00  96.00   1.00   16.00    --   90.00  73.00 112.60   34
107  \w     61.00  87.00   1.00   16.00    --   90.00  75.00 -18.93   26
108  \w     64.00  90.00   1.00   16.00    --   90.00  73.00 135.31   26
109  \w     61.00  91.00   1.00   16.00    --   90.00  75.00 179.14   30
110  \w     61.00  86.00   1.00   16.00    --   90.00  77.00 -50.07   25
111  \w     62.00  90.00   1.00   16.00    --   90.00  76.00 -67.19   28
112  \w     61.00  88.00   1.00   16.00    --   90.00  75.00 -91.34   27
113  \w     67.00 151.00   1.00   16.00    --   90.00  67.00 -93.24   84
114  \w     63.00  98.00   1.00   16.00    --   90.00  72.00 151.32   35
115  \w     64.00  96.00   1.00   16.00    --   90.00  72.00  69.30   32
116  \w     69.00 105.00   1.00   16.00    --   98.00  75.00 -85.05   36
117  \w    143.00 168.00   1.00   16.00    --   98.00  76.00  -8.91   25
118  \w     69.00 123.00   1.00   16.00    --   98.00  76.00  -8.91   54
119  \w     72.00 100.00   1.00   16.00    --   98.00  71.00 -62.00   28
120  \w     77.00 110.00   1.00   16.00    --   98.00  56.00 108.78   33
121  \w     74.00 109.00   1.00   16.00    --   98.00  69.00  56.88   35
122  \w     71.00 166.00   1.00   16.00    --   98.00  73.00 115.55   95
123  \w     78.00 111.00   1.00   16.00    --   98.00  54.00 -19.32   33
124  \w     80.00 122.00   1.00   16.00    --   98.00  63.00  72.73   42
125  \w     73.00 108.00   1.00   16.00    --  102.00  77.00 -65.63   35
126  \w     82.00 168.00   1.00   16.00    --  102.00  64.00 -27.36   86
127  \w     80.00 170.00   1.00   16.00    --  102.00  49.00 111.35   90
128  \w     86.00 171.00   1.00   16.00    --  106.00  57.00-164.64   85
129  \w     87.00 112.00   1.00   16.00    --  108.98  64.00-180.00   25
130  \w     80.00 105.00   1.00   16.00    --  108.98  77.00   0.00   25
131  \w     80.00 159.00   1.00   16.00    --  108.98  77.00-120.00   79
132  \w     87.00 112.00   1.00   16.00    --  108.98  64.00  90.00   25
133  \w     86.00 175.00   1.00   16.00    --  108.98  64.00  60.00   89
134  \w     37.00  96.00   1.00   16.00    --  108.98 -92.00 120.00   59
135  \w    100.00 168.00   1.00   16.00    --  108.98  64.00 -90.00   68
136  \w     79.00 105.00   1.00   16.00    --  108.98  77.00-150.00   26
137  \w    148.00 175.00   1.00   16.00    --  108.98  77.00  30.00   27
138  \w     79.00 105.00   1.00   16.00    --  108.98  77.00  30.00   26
139  \w    139.00 166.00   1.00   16.00    --  108.98  76.00 133.45   27
140  \w     90.00 132.00   1.00   16.00    --  108.98 -64.00 -30.00   42
141  \w     86.00 175.00   1.00   16.00    --  108.98  64.00  30.00   89
142  \w     86.00 112.00   1.00   16.00    --  108.98  64.00-120.00   26
143  \w     80.00 105.00   1.00   16.00    --  108.98  76.00 133.45   25
144  \w     42.00  68.00   1.00   16.00    --  108.98 -64.00 -30.00   26
145  \w    125.00 159.00   1.00   16.00    --  108.98 111.00  90.00   34
146  \w     61.00 106.00   1.00   16.00    --  108.98-111.00-150.00   45
147  \w     79.00 105.00   1.00   16.00    --  108.98  77.00 -30.00   26
148  \w     84.00 113.00   1.00   16.00    --  108.98-111.00  90.00   29
149  \w     82.00 164.00   1.00   16.00    --  108.98  77.00 -60.00   82
150  \w     87.00 154.00   1.00   16.00    --  108.98  63.00  22.41   67
151  \w     82.00 109.00   1.00   16.00    --  108.98  77.00 120.00   27
152  \w     86.00 176.00   1.00   16.00    --  108.98  64.00-150.00   90
153  \w    137.00 167.00   1.00   16.00    --  108.98  77.00  60.00   30
154  \w     37.00 100.00   1.00   16.00    --  108.98 -92.00-120.00   63
155  \w    126.00 153.00   1.00   16.00    --  108.98  77.00  90.00   27
156  \w     79.00 105.00   1.00   16.00    --  108.98  77.00  60.00   26
157  \w     79.00 105.00   1.00   16.00    --  108.98  77.00  90.00   26
158  \w     83.00 135.00   1.00   16.00    --  108.98  38.00-120.00   52
159  \w    145.00 173.00   1.00   16.00    --  108.98  77.00-180.00   28
160  \w     83.00 110.00   1.00   16.00    --  108.98  77.00 150.00   27
161  \w     38.00 109.00   1.00   16.00    --  108.98 -92.00 -60.00   71
162  \w     78.00 112.00   1.00   16.00    --  108.98-111.00 -60.00   34
163  \w     89.00 175.00   1.00   16.00    --  108.98  64.00 150.00   86
164  \w     87.00 128.00   1.00   16.00    --  108.98  64.00 120.00   41
165  \w     88.00 147.00   1.00   16.00    --  108.98  64.00   0.00   59
166  \w     79.00 106.00   1.00   16.00    --  108.98  77.00-180.00   27
167  \w     41.00  91.00   1.00   16.00    --  108.98-111.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0194145000
_diffrn_orient_matrix_UB_12      -0.0672617000
_diffrn_orient_matrix_UB_13      0.0508047000
_diffrn_orient_matrix_UB_21      0.1116555000
_diffrn_orient_matrix_UB_22      0.0003767000
_diffrn_orient_matrix_UB_23      -0.0137343000
_diffrn_orient_matrix_UB_31      0.0253366000
_diffrn_orient_matrix_UB_32      0.0830050000
_diffrn_orient_matrix_UB_33      0.0759304000
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            97860
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.228
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.369
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       needle
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00176(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         12847
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0730P)^2^+2.0668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10532
_reflns_number_total             12847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04113a2.cif
_cod_data_source_block           compd_2c_ga_re39
_cod_original_formula_sum        'C76 H87 Cl2 N8 O7.50'
_cod_database_code               7132141
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C74 H80 N8 O6 (CH2Cl2)(OH2)(CH3OH)'
_chemical_oxdiff_usercomment     're615, needle, red'
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.753
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H,
  H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-C25A \\sim C24-C25B
 with sigma of 0.02
 C27A-C27C \\sim C27B-C27C
 with sigma of 0.02
 C27A-C28C \\sim C27B-C28C
 with sigma of 0.02
 C28A-C27C \\sim C28B-C27C
 with sigma of 0.02
 C28A-C28C \\sim C28B-C28C
 with sigma of 0.02
 C25A-C26A \\sim C25B-C26B
 with sigma of 0.02
 C27A-C26A \\sim C27A-C26B
 with sigma of 0.02
 C24-C26A \\sim C24-C26B
 with sigma of 0.02
 C25A-C27A \\sim C25B-C27A
 with sigma of 0.02
 C27A-C26A \\sim C27B-C26A
 with sigma of 0.02
 C27A-C28A \\sim C27B-C28A
 with sigma of 0.02
 C27A-C26B \\sim C27B-C26B
 with sigma of 0.02
 C27A-C28A \\sim C27A-C28B
 with sigma of 0.02
 C28A-C27B \\sim C28B-C27B
 with sigma of 0.02
 C25A-C24 \\sim C24-C25C
 with sigma of 0.02
 C25C-C24 \\sim C24-C25B
 with sigma of 0.02
 C25B-C26B \\sim C25C-C26C \\sim C25A-C26A
 with sigma of 0.02
 C26A-C27A \\sim C26B-C27B \\sim C26C-C27C
 with sigma of 0.02
 C27A-C28A \\sim C27C-C28C \\sim C27B-C28B
 with sigma of 0.02
 C32-C33 \\sim C33-C34
 with sigma of 0.02
 C29-C30 \\sim C29-C30A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 C29-C31 \\sim C29-C31A
 with sigma of 0.02
 C30-C32 \\sim C30A-C32A
 with sigma of 0.02
 C31-C33 \\sim C31A-C33A
 with sigma of 0.02
 C32-C34 \\sim C32A-C34A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C25A \\sim C25C \\sim C25B \\sim C26B \\sim C26C \\sim C26A \\sim C27A \\sim
C27B \\sim C27C \\sim C28B \\sim C28C \\sim C28A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C23 \\sim C24 \\sim C25A \\sim C25C \\sim C25B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C30A \\sim C30 \\sim C29 \\sim C31A \\sim C32A \\sim C32 \\sim C34A \\sim C33A
\\sim C33 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
4. Others
 1*[Sof(H24A)+Sof(H24B)+Sof(C25A)+Sof(H25A)+Sof(H25B)+Sof(C26A)+Sof(H26E)+
 Sof(H26F)+Sof(C27A)+Sof(H27A)+Sof(H27B)+Sof(C28A)+Sof(H28G)+Sof(H28H)+
 Sof(H28I)]+1*[Sof(H24C)+Sof(H24D)+Sof(C25B)+Sof(H25E)+Sof(H25F)+Sof(C26B)+
 Sof(H26A)+Sof(H26B)+Sof(C27B)+Sof(H27C)+Sof(H27D)+Sof(C28B)+Sof(H28A)+
 Sof(H28B)+Sof(H28C)]+1*[Sof(H24E)+Sof(H24F)+Sof(C25C)+Sof(H25C)+Sof(H25D)+
 Sof(C26C)+Sof(H26C)+Sof(H26D)+Sof(C27C)+Sof(H27E)+Sof(H27F)+Sof(C28C)+
 Sof(H28D)+Sof(H28E)+Sof(H28F)]=1 with esd of 0.0001
 Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26E)=
 Sof(H26F)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28G)=Sof(H28H)=
 Sof(H28I)=FVAR(1)
 Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25E)=Sof(H25F)=Sof(C26B)=Sof(H26A)=
 Sof(H26B)=Sof(C27B)=Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=FVAR(2)
 Sof(H24E)=Sof(H24F)=Sof(C25C)=Sof(H25C)=Sof(H25D)=Sof(C26C)=Sof(H26C)=
 Sof(H26D)=Sof(C27C)=Sof(H27E)=Sof(H27F)=Sof(C28C)=Sof(H28D)=Sof(H28E)=
 Sof(H28F)=FVAR(3)
 Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=
 Sof(H31D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(4)
 Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C24(H24E,H24F), C24(H24C,H24D), C25A(H25A,
 H25B), C25C(H25C,H25D), C25B(H25E,H25F), C26B(H26A,H26B), C26C(H26C,H26D),
 C26A(H26E,H26F), C27A(H27A,H27B), C27B(H27C,H27D), C27C(H27E,H27F), C29(H29A,
 H29B), C29(H29C,H29D), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,H32D),
 C33A(H33C,H33D)
5.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C49(H49), C51(H51), C52(H52), C55(H55), C56(H56), C58(H58),
 C59(H59), C62(H62), C63(H63), C65(H65), C66(H66), C69(H69), C70(H70), C72(H72),
  C73(H73)
5.c Idealised Me refined as rotating group:
 C28B(H28A,H28B,H28C), C28C(H28D,H28E,H28F), C28A(H28G,H28H,H28I), C34(H34A,
 H34B,H34C), C40(H40A,H40B,H40C), C46(H46A,H46B,H46C), C53(H53A,H53B,H53C),
 C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C74(H74A,H74B,H74C), C34A(H34D,H34E,
 H34F)
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_smtbx_masks_special_details
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A solvent mask was calculated and 131 electrons were 
found in a volume of 698\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2], 1[CH3OH], 0.5[OH2] per Asymmetric Unit 
which account for 130 electrons 
per unit cell.
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_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 3.0
_shelx_res_checksum              83904
_shelx_hkl_checksum              72715
_shelx_fab_checksum              63296
_olex2_date_sample_data_collection 2023-06-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
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Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
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