Understanding of Mirabegron Edisylate Hydrate Conversion and Solvate Characterisation
Balogh, Margareta Cristina; Claybourn, Boe M.; Bonnaud, Thierry; Pitak, Mateusz B.; CrystEngComm  (2026) –; doi:10.1039/D5CE00592B

data_7251880
_publ_section_title
;
 Understanding of Mirabegron Edisylate Hydrate Conversion and Solvate
 Characterisation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00592B
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C21 H26 N4 O2 S), 2(C2 H4 O6 S2), C4 H8 O2,  0.65(H2 O)'
_chemical_formula_sum            'C50 H69.3 N8 O18.65 S6'
_chemical_formula_weight         1273.19
_chemical_name_common
;
'Mirabegron Edysilate 1,4-dioxane, partial water hydrate'
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-10-07 deposited with the CCDC.	2026-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                85.1410(10)
_cell_angle_beta                 72.053(2)
_cell_angle_gamma                71.7410(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7367(2)
_cell_length_b                   11.3761(2)
_cell_length_c                   14.6395(3)
_cell_measurement_reflns_used    40664
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.6260
_cell_measurement_theta_min      4.0810
_cell_volume                     1464.85(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.122a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.144a 64-bit (release 23-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.122a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.999
_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    -83.00  -4.00   0.50    0.70    --  -49.38 113.00-134.00  158
  2  \w     26.00  86.00   0.50    0.70    --   49.38-113.00 133.00  120
  3  \w   -158.00 -81.00   0.50    2.80    --  -90.00-113.00 133.00  154
  4  \w    -82.00 -22.00   0.50    2.80    --  -90.00 113.00-134.00  120
  5  \w     44.00 108.00   0.50    2.80    --  111.50-113.00 133.00  128
  6  \w    102.00 178.00   0.50    2.80    --  111.50 113.00-134.00  152
  7  \w    -21.00   9.00   0.50    0.70    --   10.00 101.00 179.10   60
  8  \w    -18.00   8.00   0.50    0.70    --   14.00 102.00  26.37   52
  9  \w      0.00  26.00   0.50    0.70    --   22.00  80.00 121.60   52
 10  \w      8.00  37.00   0.50    0.70    --   26.00  71.00  50.15   58
 11  \w     14.00  45.00   0.50    0.70    --   30.00  66.00-113.32   62
 12  \w     12.00  38.00   0.50    0.70    --   30.00  70.00 -58.71   52
 13  \w     14.00  43.00   0.50    0.70    --   30.00  67.00-170.17   58
 14  \w     23.00  54.00   0.50    0.70    --   38.00  62.00 -61.35   62
 15  \w     23.00  49.00   0.50    0.70    --   38.00  64.00 161.42   52
 16  \w     23.00  49.00   0.50    0.70    --   38.00  64.00 130.94   52
 17  \w     33.00 117.00   0.50    0.70    --   46.00  59.00 127.10  168
 18  \w   -118.00 -93.00   0.50    0.70    --  -49.38-125.00   0.00   50
 19  \w    -25.00  16.00   0.50    0.70    --  -49.38  19.00 120.00   82
 20  \w    -96.00 -69.00   0.50    0.70    --  -49.38 -57.00 -30.00   54
 21  \w    -62.00 -37.00   0.50    0.70    --  -49.38 -57.00 -30.00   50
 22  \w    -62.00  20.00   0.50    0.70    --  -49.38  57.00-150.00  164
 23  \w    -62.00 -37.00   0.50    0.70    --  -49.38 -57.00  30.00   50
 24  \w     40.00  67.00   0.50    0.70    --   49.38  58.00 -10.40   54
 25  \w     37.00  64.00   0.50    0.70    --   49.38  57.00 -90.00   54
 26  \w     38.00  65.00   0.50    0.70    --   49.38  57.00 120.00   54
 27  \w     39.00  66.00   0.50    0.70    --   49.38  57.00 -60.00   54
 28  \w     42.00  72.00   0.50    0.70    --   49.38  19.00  30.00   60
 29  \w     77.00 105.00   0.50    0.70    --   49.38  57.00 120.00   56
 30  \w     40.00  67.00   0.50    0.70    --   49.38  57.00-150.00   54
 31  \w     37.00  64.00   0.50    0.70    --   49.38  57.00  60.00   54
 32  \w     40.00  67.00   0.50    0.70    --   49.38  57.00-180.00   54
 33  \w     38.00  63.00   0.50    0.70    --   49.38  57.00 -30.00   50
 34  \w     39.00  74.00   0.50    0.70    --   49.38  57.00  15.89   70
 35  \w     42.00  71.00   0.50    0.70    --   49.38  37.00-120.00   58
 36  \w     72.00  97.00   0.50    0.70    --   49.38  19.00 120.00   50
 37  \w     42.00  67.00   0.50    0.70    --   49.38  57.00  90.00   50
 38  \w     41.00  86.00   0.50    0.70    --   54.00  60.00 -41.31   90
 39  \w     40.00  76.00   0.50    0.70    --   54.00  60.00-129.89   72
 40  \w     50.00  75.00   0.50    0.70    --   62.00  59.00-163.61   50
 41  \w    -78.00 -52.00   0.50    0.70    --  -66.00 -60.00-132.28   52
 42  \w    -77.00 -52.00   0.50    0.70    --  -66.00 -59.00 -84.34   50
 43  \w    -79.00 -52.00   0.50    0.70    --  -66.00 -59.00 104.31   54
 44  \w   -101.00 -52.00   0.50    0.70    --  -66.00 -60.00-161.73   98
 45  \w    -78.00 -52.00   0.50    0.70    --  -66.00 -59.00 118.70   52
 46  \w    -78.00 -52.00   0.50    0.70    --  -66.00 -60.00 -62.95   52
 47  \w    -79.00 -52.00   0.50    0.70    --  -66.00 -60.00  26.54   54
 48  \w    -83.00 -56.00   0.50    0.70    --  -66.00 -60.00  21.32   54
 49  \w    -80.00 -53.00   0.50    0.70    --  -66.00 -60.00 -70.14   54
 50  \w    -88.00 -52.00   0.50    0.70    --  -66.00 -60.00  89.91   72
 51  \w     54.00  79.00   0.50    0.70    --   66.00  59.00 -24.87   50
 52  \w    -82.00 -57.00   0.50    0.70    --  -70.00 -57.00-152.03   50
 53  \w    -86.00 -57.00   0.50    0.70    --  -70.00 -58.00  40.99   58
 54  \w    -87.00 -60.00   0.50    0.70    --  -74.00 -59.00-139.11   54
 55  \w    -86.00 -61.00   0.50    0.70    --  -74.00 -56.00  55.46   50
 56  \w    -87.00 -62.00   0.50    0.70    --  -74.00 -55.00 -96.83   50
 57  \w    -89.00 -64.00   0.50    0.70    --  -74.00 -54.00 168.35   50
 58  \w    -89.00 -62.00   0.50    0.70    --  -74.00 -53.00 -13.70   54
 59  \w   -139.00-113.00   0.50    0.70    --  -74.00 -56.00  55.46   52
 60  \w    -92.00 -67.00   0.50    0.70    --  -78.00 -52.00 -34.76   50
 61  \w    -94.00 -67.00   0.50    0.70    --  -78.00 -53.00 -26.38   54
 62  \w    -93.00 -66.00   0.50    0.70    --  -78.00 -54.00  75.85   54
 63  \w    -97.00 -70.00   0.50    2.80    --  -82.00 -54.00  68.84   54
 64  \w    -98.00 -71.00   0.50    2.80    --  -82.00 -52.00  84.07   54
 65  \w    -96.00 -70.00   0.50    2.80    --  -82.00 -54.00-173.02   52
 66  \w    -97.00 -70.00   0.50    2.80    --  -82.00 -53.00   5.28   54
 67  \w    -96.00 -69.00   0.50    2.80    --  -82.00 -58.00 104.98   54
 68  \w    -95.00 -68.00   0.50    2.80    --  -82.00 -59.00-120.44   54
 69  \w    -95.00 -68.00   0.50    2.80    --  -82.00 -59.00 -60.82   54
 70  \w    -99.00 -72.00   0.50    2.80    --  -82.00 -51.00-116.17   54
 71  \w    -96.00 -69.00   0.50    2.80    --  -82.00 -59.00  37.77   54
 72  \w    -93.00 -68.00   0.50    2.80    --  -82.00 -59.00  82.97   50
 73  \w    -96.00 -71.00   0.50    2.80    --  -82.00 -52.00 -42.13   50
 74  \w   -100.00 -73.00   0.50    2.80    --  -86.00 -59.00 -64.76   54
 75  \w   -104.00 -74.00   0.50    2.80    --  -86.00 -53.00 -13.58   60
 76  \w    -99.00 -74.00   0.50    2.80    --  -86.00 -54.00-152.12   50
 77  \w   -157.00-130.00   0.50    2.80    --  -86.00 -54.00-152.12   54
 78  \w   -105.00 -79.00   0.50    2.80    --  -90.00 -51.00-110.50   52
 79  \w   -102.00 -76.00   0.50    2.80    --  -90.00 -59.00 152.66   52
 80  \w    -64.00 -18.00   0.50    2.80    --  -90.00  57.00 -30.00   92
 81  \w   -155.00-119.00   0.50    2.80    --  -90.00 -59.00 152.66   72
 82  \w   -103.00 -78.00   0.50    2.80    --  -90.00 -60.00 -68.94   50
 83  \w   -158.00-113.00   0.50    2.80    --  -90.00 -57.00  13.49   90
 84  \w   -140.00-113.00   0.50    2.80    --  -90.00 -60.00 -68.94   54
 85  \w    -84.00 -22.00   0.50    2.80    --  -90.00 125.00-180.00  124
 86  \w   -103.00 -77.00   0.50    2.80    --  -90.00 -60.00 174.17   52
 87  \w   -110.00 -81.00   0.50    2.80    --  -90.00 -61.00 166.84   58
 88  \w   -160.00-133.00   0.50    2.80    --  -90.00 -60.00 174.17   54
 89  \w   -110.00 -79.00   0.50    2.80    --  -90.00 -57.00   0.00   62
 90  \w   -161.00-128.00   0.50    2.80    --  -90.00 -57.00   0.00   66
 91  \w   -105.00 -78.00   0.50    2.80    --  -90.00 -60.00  97.64   54
 92  \w   -106.00 -79.00   0.50    2.80    --  -90.00 -54.00 -42.21   54
 93  \w   -122.00 -81.00   0.50    2.80    --  -90.00 -59.00-126.89   82
 94  \w   -160.00-116.00   0.50    2.80    --  -90.00 -54.00 -42.21   88
 95  \w   -131.50-131.00   0.50    2.80    --  -90.00 -56.00 -50.10    1
 96  \w   -104.00 -79.00   0.50    2.80    --  -90.00 -58.00  71.75   50
 97  \w    -85.00 -23.00   0.50    2.80    --  -90.00 125.00  30.00  124
 98  \w   -103.00 -77.00   0.50    2.80    --  -90.00 -60.00  88.79   52
 99  \w   -160.00-115.00   0.50    2.80    --  -90.00 -60.00  88.79   90
100  \w   -149.00-120.00   0.50    2.80    --  -90.00 -58.00  71.75   58
101  \w   -107.00 -76.00   0.50    2.80    --  -90.00 -59.00 -20.22   62
102  \w   -110.00 -81.00   0.50    2.80    --  -90.00 -57.00 -79.77   58
103  \w   -116.00 -77.00   0.50    2.80    --  -90.00 -57.00  60.00   78
104  \w   -160.00-132.00   0.50    2.80    --  -90.00 -57.00 -79.77   56
105  \w   -101.00 -76.00   0.50    2.80    --  -90.00 -59.00 121.53   50
106  \w   -101.00 -76.00   0.50    2.80    --  -90.00 -60.00-169.84   50
107  \w   -154.00-127.00   0.50    2.80    --  -90.00 -59.00 121.53   54
108  \w   -103.00 -77.00   0.50    2.80    --  -90.00 -57.00-150.00   52
109  \w   -105.00 -78.00   0.50    2.80    --  -90.00 -60.00  41.80   54
110  \w   -112.00 -81.00   0.50    2.80    --  -90.00 -49.00 121.54   62
111  \w    -48.00 -21.00   0.50    2.80    --  -90.00  57.00-150.00   54
112  \w   -102.00 -76.00   0.50    2.80    --  -90.00 -59.00 -84.62   52
113  \w   -103.00 -76.00   0.50    2.80    --  -90.00 -59.00 -66.76   54
114  \w   -101.00 -76.00   0.50    2.80    --  -90.00 -60.00-118.78   50
115  \w   -155.00-123.00   0.50    2.80    --  -90.00 -60.00-118.78   64
116  \w   -159.00 -78.00   0.50    2.80    --  -90.00 -53.00 101.15  162
117  \w   -108.00 -81.00   0.50    2.80    --  -90.00 -57.00 -90.00   54
118  \w   -109.00 -80.00   0.50    2.80    --  -90.00 -57.00  13.49   58
119  \w   -161.00-111.00   0.50    2.80    --  -90.00 -60.00  41.80  100
120  \w   -159.00-110.00   0.50    2.80    --  -90.00 -99.00   0.00   98
121  \w   -160.00-112.00   0.50    2.80    --  -90.00 -57.00 -90.00   96
122  \w   -108.00 -78.00   0.50    2.80    --  -90.00 -58.00-163.15   60
123  \w   -158.00-103.00   0.50    2.80    --  -90.00 -99.00-120.00  110
124  \w   -103.00 -76.00   0.50    2.80    --  -90.00 -60.00 145.52   54
125  \w    -64.00 -19.00   0.50    2.80    --  -90.00  57.00-180.00   90
126  \w   -116.00 -83.00   0.50    2.80    --  -90.00 -50.00-115.06   66
127  \w   -159.00-111.00   0.50    2.80    --  -90.00 -60.00 145.52   96
128  \w   -113.00 -78.00   0.50    2.80    --  -90.00 -55.00  49.38   70
129  \w   -160.00-114.00   0.50    2.80    --  -90.00 -58.00-163.15   92
130  \w   -106.00 -76.00   0.50    2.80    --  -90.00 -60.00  82.81   60
131  \w   -160.00-133.00   0.50    2.80    --  -90.00 -55.00  49.38   54
132  \w   -102.00 -77.00   0.50    2.80    --  -90.00 -57.00  48.80   50
133  \w   -104.00 -78.00   0.50    2.80    --  -90.00 -55.00  22.72   52
134  \w   -159.00-132.00   0.50    2.80    --  -90.00 -55.00  22.72   54
135  \w   -107.00 -77.00   0.50    2.80    --  -90.00 -57.00-180.00   60
136  \w   -160.00-116.00   0.50    2.80    --  -90.00 -57.00-180.00   88
137  \w   -153.00-123.00   0.50    2.80    --  -90.00 -50.00-115.06   60
138  \w     44.00  98.00   0.50    2.80    --  111.50 -99.00 150.00  108
139  \w     83.00 110.00   0.50    2.80    --  111.50-125.00-150.00   54
140  \w     43.00  81.00   0.50    2.80    --  111.50-125.00   0.00   76
141  \w     47.00  81.00   0.50    2.80    --  111.50-125.00-150.00   68
142  \w     65.00 104.00   0.50    2.80    --  111.50 -99.00 -90.00   78
143  \w     43.00  84.00   0.50    2.80    --  111.50-125.00  60.00   82
144  \w     74.00 106.00   0.50    2.80    --  111.50 -99.00  60.00   64
145  \w     43.00  81.00   0.50    2.80    --  111.50-125.00  90.00   76
146  \w     45.00 105.00   0.50    2.80    --  111.50 -99.00-120.00  120
147  \w     45.00  72.00   0.50    2.80    --  111.50 -99.00-150.00   54
148  \w     71.00 105.00   0.50    2.80    --  111.50 -99.00 -30.00   68
149  \w     42.00 106.00   0.50    2.80    --  111.50 -99.00   0.00  128
150  \w     44.00  93.00   0.50    2.80    --  111.50-125.00 -30.00   98
151  \w     82.00 107.00   0.50    2.80    --  111.50-178.00  -2.00   50
152  \w     62.00  88.00   0.50    2.80    --  111.50 -99.00  30.00   52
153  \w     80.00 106.00   0.50    2.80    --  111.50 -99.00 -90.00   52
154  \w     32.00  57.00   0.50    0.70    --   49.63-113.00 133.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0224540000
_diffrn_orient_matrix_UB_12      -0.0005377000
_diffrn_orient_matrix_UB_13      -0.1088524000
_diffrn_orient_matrix_UB_21      -0.0554152000
_diffrn_orient_matrix_UB_22      0.1425950000
_diffrn_orient_matrix_UB_23      0.0013539000
_diffrn_orient_matrix_UB_31      0.1639569000
_diffrn_orient_matrix_UB_32      0.0022728000
_diffrn_orient_matrix_UB_33      -0.0196773000
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            53310
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.230
_diffrn_reflns_theta_min         4.092
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.122a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 4583 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         10194
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0802P)^2^+0.4132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.906
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                9926
_reflns_number_total             10194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00592b2.cif
_cod_data_source_block           p25074_1_r1
_cod_original_formula_sum        'C50 H69.30 N8 O18.65 S6'
_cod_database_code               7251880
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C46 H54 N10 O16 S6 '
_chemical_oxdiff_usercomment     'TB-2260-26a, P4335, MP, 15SEP25P, Cu 100K'
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
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 N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C13C-C12B
 1.53 with sigma of 0.02
 C14B-N4C
 1.47 with sigma of 0.01
 O101-C104
 1.45 with sigma of 0.01
 H13D-H8B
 2.1 with sigma of 0.01
 O102-C102 \\sim O202-C202
 with sigma of 0.02
 O102-C103 \\sim O202-C203
 with sigma of 0.02
 C103-O101 \\sim C203-O201
 with sigma of 0.04
 C103-C104 \\sim C203-C204
 with sigma of 0.02
 C102-O101 \\sim C202-O201
 with sigma of 0.04
 O101-C104 \\sim O201-C204
 with sigma of 0.02
 C102-C101 \\sim C202-C201
 with sigma of 0.02
 C103-C102 \\sim C203-C202
 with sigma of 0.04
 O102-C104 \\sim O202-C204
 with sigma of 0.04
 O102-C101 \\sim O202-C201
 with sigma of 0.04
 C104-C101 \\sim C204-C201
 with sigma of 0.04
 O101-C101 \\sim O201-C201
 with sigma of 0.02
 C13B-C14B \\sim C13C-C14B
 with sigma of 0.04
 C13B-N4B \\sim C13C-N4C
 with sigma of 0.02
 N4B-C12B \\sim N4C-C12B
 with sigma of 0.04
 N4B-C14B \\sim N4C-C14B
 with sigma of 0.02
 C13B-C12B \\sim C13C-C12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O101 \\sim O102 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O101 \\sim O102 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim O201 \\sim
O202 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O2A \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
N4B \\sim N4C \\sim C12B \\sim C13B \\sim C13C \\sim C14B: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N4C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C201) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O101, O102, C101, C102, C103, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O101, O102, C101, C102, C103, C104, O201, O202, C201, C202, C203, C204
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, C15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4B, N4C, C12B, C13B, C13C, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O201)=Sof(O202)=Sof(C201)=Sof(H20C)=Sof(H20D)=Sof(C202)=Sof(H20E)=
 Sof(H20F)=Sof(C203)=Sof(H20G)=Sof(H20H)=Sof(C204)=Sof(H20I)=Sof(H20J)=1-FVAR(1)
 Sof(O101)=Sof(O102)=Sof(C101)=Sof(H10C)=Sof(H10D)=Sof(C102)=Sof(H10E)=
 Sof(H10F)=Sof(C103)=Sof(H10G)=Sof(H10H)=Sof(C104)=Sof(H10I)=Sof(H10J)=FVAR(1)
 Sof(N4C)=Sof(H4CA)=Sof(H4CB)=Sof(H12C)=Sof(H12D)=Sof(C13C)=Sof(H13C)=
 Sof(H13D)=Sof(H14C)=Sof(H14D)=1-FVAR(2)
 Sof(N4B)=Sof(H4BA)=Sof(H4BB)=Sof(H12A)=Sof(H12B)=Sof(C13B)=Sof(H13A)=
 Sof(H13B)=Sof(H14A)=Sof(H14B)=FVAR(2)
 Fixed Sof: O1W(0.65) H1WA(0.65) H1WB(0.65)
6.a Free rotating group:
 O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 C15A(H15A), C15B(H15B)
6.c Secondary CH2 refined with riding coordinates:
 N4A(H4AA,H4AB), C4A(H4AC,H4AD), C12A(H12E,H12F), C13A(H13E,H13F), C14A(H14E,
 H14F), N4B(H4BA,H4BB), N4C(H4CA,H4CB), C4B(H4BC,H4BD), C12B(H12A,H12B),
 C12B(H12C,H12D), C13B(H13A,H13B), C13C(H13C,H13D), C14B(H14A,H14B), C14B(H14C,
 H14D), C22A(H22A,H22B), C23A(H23A,H23B), C22B(H22C,H22D), C23B(H23C,H23D),
 C101(H10C,H10D), C102(H10E,H10F), C103(H10G,H10H), C104(H10I,H10J), C201(H20C,
 H20D), C202(H20E,H20F), C203(H20G,H20H), C204(H20I,H20J)
6.d Aromatic/amide H refined with riding coordinates:
 N2A(H2AA), N3A(H3A), C2A(H2AB), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A),
 C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A), C21A(H21A), N3B(H3B),
 C2B(H2BB), C7B(H7B), C8B(H8B), C10B(H10B), C11B(H11B), C17B(H17B), C18B(H18B),
 C19B(H19B), C20B(H20B), C21B(H21B)
6.e X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N1B(H1BA,H1BB)
6.f Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O2B(H2B)
;
_shelx_res_checksum              15338
_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 1.740
_oxdiff_exptl_absorpt_empirical_full_min 0.545