Borohydride intermediates pave the way for magnesium-catalysed enantioselective ketone reduction.
Vasilenko, Vladislav; Blasius, Clemens K.; Wadepohl, Hubert; Gade, Lutz H.; Chemical communications (Cambridge, England) 56 (2020) 1203–1206; doi:10.1039/c9cc09111d

data_7125679
_publ_section_title
;
 Borohydride intermediates pave the way for magnesium-catalysed
 enantioselective ketone reduction.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1203
_journal_page_last               1206
_journal_paper_doi               10.1039/c9cc09111d
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H41 Mg N3 O3 Si, 0.5(C4 H10 O)'
_chemical_formula_sum            'C38 H46 Mg N3 O3.5 Si'
_chemical_formula_weight         653.18
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_vv34
_audit_creation_date             2018-10-09
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-29 deposited with the CCDC.	2019-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                94.6517(18)
_cell_angle_beta                 98.1677(18)
_cell_angle_gamma                90.4055(18)
_cell_formula_units_Z            2
_cell_length_a                   9.7605(2)
_cell_length_b                   10.6398(3)
_cell_length_c                   17.7151(4)
_cell_measurement_reflns_used    21132
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.0130
_cell_measurement_theta_min      4.1640
_cell_volume                     1814.73(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_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     -7.00  18.00   1.00    4.00    --    0.00 -57.00 150.00   25
  2  \w    -21.00  69.00   1.00    4.00    --    0.00  57.00 -90.00   90
  3  \w    -68.00 -40.00   1.00    4.00    --    0.00 -57.00  60.00   28
  4  \w    -14.00  34.00   1.00    4.00    --    0.00  57.00-150.00   48
  5  \w    -14.00  52.00   1.00    4.00    --    0.00  77.00   0.00   66
  6  \w    -63.00 -20.00   1.00    4.00    --    0.00 138.00  32.00   43
  7  \w     36.00  63.00   1.00    4.00    --    0.00  57.00-150.00   27
  8  \w    -26.00  13.00   1.00    4.00    --    0.00 -57.00  60.00   39
  9  \w    -40.00   4.00   1.00    4.00    --   12.00 116.00  36.97   44
 10  \w    -31.00  -6.00   1.00    8.00    --   28.00 126.00  66.54   25
 11  \w    -21.00   4.00   1.00    8.00    --   32.00 117.00 -45.16   25
 12  \w     -9.00  16.00   1.00    8.00    --   36.00 101.00 146.79   25
 13  \w      0.00  25.00   1.00    8.00    --   40.00  93.00-107.96   25
 14  \w     -2.00  23.00   1.00    8.00    --   40.00  96.00  19.02   25
 15  \w      6.00  31.00   1.00    8.00    --   44.00  89.00 -62.27   25
 16  \w      5.00  30.00   1.00    8.00    --   44.00  90.00 131.84   25
 17  \w      5.00  30.00   1.00    8.00    --   44.00  90.00 -32.75   25
 18  \w     13.00  38.00   1.00    8.00    --   48.00  83.00-117.99   25
 19  \w     13.00  38.00   1.00    8.00    --   48.00  83.00-165.89   25
 20  \w     13.00  38.00   1.00    8.00    --   48.00  83.00  24.58   25
 21  \w     18.00  43.00   1.00    8.00    --   52.00  81.00 137.69   25
 22  \w     18.00  43.00   1.00    8.00    --   52.00  82.00 -42.69   25
 23  \w     19.00  44.00   1.00    8.00    --   52.00  80.00 170.25   25
 24  \w     18.00  43.00   1.00    8.00    --   52.00  82.00 -59.09   25
 25  \w     18.00  43.00   1.00    8.00    --   52.00  81.00 -97.41   25
 26  \w     21.00  48.00   1.00    8.00    --   52.00  76.00-154.27   27
 27  \w     18.00  43.00   1.00    8.00    --   52.00  81.00 -27.16   25
 28  \w     19.00  44.00   1.00    8.00    --   52.00  80.00 -14.24   25
 29  \w     19.00  44.00   1.00    8.00    --   52.00  80.00 150.51   25
 30  \w     18.00  43.00   1.00    8.00    --   52.00  81.00 -73.89   25
 31  \w     18.00  43.00   1.00    8.00    --   52.00  81.00  61.32   25
 32  \w    -14.00  75.00   1.00    8.00    --   54.00 -57.00  30.00   89
 33  \w      2.00  98.00   1.00    8.00    --   54.00 -99.00   0.00   96
 34  \w     23.00  98.00   1.00    8.00    --   54.00-125.00-150.00   75
 35  \w     22.00  49.00   1.00    8.00    --   54.00  77.00-180.00   27
 36  \w    -15.00  75.00   1.00    8.00    --   54.00 -57.00-150.00   90
 37  \w     26.00  73.00   1.00    8.00    --   56.00  76.00   1.28   47
 38  \w     83.00 113.00   1.00    8.00    --   56.00  76.00   1.28   30
 39  \w     24.00  51.00   1.00    8.00    --   56.00  77.00  76.59   27
 40  \w     24.00  51.00   1.00    8.00    --   56.00  77.00-172.93   27
 41  \w     25.00  52.00   1.00    8.00    --   56.00  77.00-134.15   27
 42  \w     30.00  57.00   1.00    8.00    --   60.00  75.00 149.46   27
 43  \w     29.00  54.00   1.00    8.00    --   60.00  77.00-159.37   25
 44  \w     99.00 126.00   1.00    8.00    --   60.00  77.00 -81.87   27
 45  \w     32.00  59.00   1.00    8.00    --   60.00  76.00 -51.97   27
 46  \w     28.00  55.00   1.00    8.00    --   60.00  77.00 -81.87   27
 47  \w     30.00  59.00   1.00    8.00    --   60.00  76.00 133.89   29
 48  \w     29.00  56.00   1.00    8.00    --   60.00  77.00 -26.99   27
 49  \w     31.00  58.00   1.00    8.00    --   60.00  74.00 -94.77   27
 50  \w     33.00  60.00   1.00    8.00    --   60.00  71.00   7.94   27
 51  \w     29.00  57.00   1.00    8.00    --   60.00  77.00  24.77   28
 52  \w     34.00  61.00   1.00    8.00    --   60.00  73.00  56.22   27
 53  \w     30.00  55.00   1.00    8.00    --   60.00  76.00 125.26   25
 54  \w     30.00  57.00   1.00    8.00    --   60.00  74.00-121.22   27
 55  \w     28.00  54.00   1.00    8.00    --   60.00  77.00 109.25   26
 56  \w     39.00  66.00   1.00    8.00    --   60.00  75.00 164.59   27
 57  \w     28.00 106.00   1.00    8.00    --   60.00  77.00 -35.03   78
 58  \w     28.00  55.00   1.00    8.00    --   60.00  77.00  92.83   27
 59  \w     38.00  65.00   1.00    8.00    --   64.00  70.00  76.17   27
 60  \w     32.00  58.00   1.00    8.00    --   64.00  77.00-126.25   26
 61  \w     33.00  60.00   1.00    8.00    --   64.00  75.00 -71.22   27
 62  \w     83.00 111.00   1.00    8.00    --   68.00  76.00  49.00   28
 63  \w     47.00  83.00   1.00    8.00    --   68.00  65.00-134.54   36
 64  \w     97.00 126.00   1.00    8.00    --   68.00  77.00  97.57   29
 65  \w     36.00  63.00   1.00    8.00    --   68.00  77.00  97.57   27
 66  \w     48.00  75.00   1.00    8.00    --   68.00  66.00 -75.18   27
 67  \w     39.00  66.00   1.00    8.00    --   68.00  76.00  49.00   27
 68  \w     36.00  63.00   1.00    8.00    --   68.00  77.00 177.27   27
 69  \w     44.00 121.00   1.00    8.00    --   68.00  62.00   1.80   77
 70  \w     39.00  66.00   1.00    8.00    --   68.00  75.00  40.41   27
 71  \w     37.00  64.00   1.00    8.00    --   68.00  76.00  22.33   27
 72  \w     40.00  67.00   1.00    8.00    --   68.00  70.00 -99.51   27
 73  \w     96.00 126.00   1.00    8.00    --   68.00  71.00 148.59   30
 74  \w     42.00  86.00   1.00    8.00    --   68.00  71.00 148.59   44
 75  \w     41.00 126.00   1.00    8.00    --   72.00  75.00 -40.96   85
 76  \w     45.00  71.00   1.00    8.00    --   72.00  69.00 -68.10   26
 77  \w     51.00 141.00   1.00    8.00    --   72.00  54.00-113.39   90
 78  \w     47.00  72.00   1.00    8.00    --   72.00  67.00  64.63   25
 79  \w     80.00 108.00   1.00    8.00    --   72.00  73.00 145.14   28
 80  \w     44.00  75.00   1.00    8.00    --   72.00  73.00 145.14   31
 81  \w     48.00  73.00   1.00    8.00    --   72.00  67.00  78.59   25
 82  \w     46.00  71.00   1.00    8.00    --   76.00  76.00  16.80   25
 83  \w     54.00  79.00   1.00    8.00    --   76.00  66.00-154.74   25
 84  \w     47.00 145.00   1.00    8.00    --   76.00  73.00 158.76   98
 85  \w     58.00  97.00   1.00    8.00    --   80.00  59.00  87.03   39
 86  \w     53.00  84.00   1.00    8.00    --   80.00  70.00   6.71   31
 87  \w     53.00  97.00   1.00    8.00    --   80.00  68.00  52.86   44
 88  \w     49.00  75.00   1.00    8.00    --   80.00  75.00 -67.56   26
 89  \w     50.00 118.00   1.00    8.00    --   80.00  75.00 114.48   68
 90  \w     52.00  83.00   1.00    8.00    --   80.00  71.00 134.45   31
 91  \w     49.00  75.00   1.00    8.00    --   80.00  76.00 104.08   26
 92  \w     50.00  77.00   1.00    8.00    --   80.00  77.00-121.55   27
 93  \w     51.00 121.00   1.00    8.00    --   80.00  73.00 -35.59   70
 94  \w     50.00  75.00   1.00    8.00    --   80.00  75.00 -16.35   25
 95  \w     50.00  76.00   1.00    8.00    --   80.00  74.00-136.91   26
 96  \w     72.00 125.00   1.00   16.00    --   84.00  52.00 128.00   53
 97  \w     53.00  83.00   1.00   16.00    --   84.00  76.00 143.22   30
 98  \w     52.00  78.00   1.00   16.00    --   84.00  77.00  77.03   26
 99  \w     54.00  79.00   1.00   16.00    --   84.00  75.00 -83.00   25
100  \w     52.00  80.00   1.00   16.00    --   84.00  77.00 178.09   28
101  \w     67.00 121.00   1.00   16.00    --   88.00  59.00   2.68   54
102  \w     60.00  85.00   1.00   16.00    --   88.00  73.00 -95.40   25
103  \w     56.00  86.00   1.00   16.00    --   88.00  77.00  14.68   30
104  \w     57.00  85.00   1.00   16.00    --   88.00  77.00 160.47   28
105  \w     69.00 135.00   1.00   16.00    --   88.00  59.00 -63.50   66
106  \w     63.00 149.00   1.00   16.00    --   92.00  73.00 -47.32   86
107  \w     70.00  95.00   1.00   16.00    --   92.00  52.00-131.11   25
108  \w     63.00 103.00   1.00   16.00    --   92.00  73.00 127.41   40
109  \w     61.00  88.00   1.00   16.00    --   92.00  76.00 148.12   27
110  \w     61.00 148.00   1.00   16.00    --   92.00  76.00  76.60   87
111  \w     72.00 127.00   1.00   16.00    --   92.00  65.00 -29.79   55
112  \w     73.00 127.00   1.00   16.00    --   96.00  50.00-171.62   54
113  \w     75.00 102.00   1.00   16.00    --   96.00  65.00  14.21   27
114  \w     72.00 115.00   1.00   16.00    --  100.00  70.00 130.36   43
115  \w     73.00 173.00   1.00   16.00    --  104.00  75.00-116.40  100
116  \w     83.00 176.00   1.00   16.00    --  108.00  64.00  90.00   93
117  \w     83.00 120.00   1.00   16.00    --  108.00  64.00  30.00   37
118  \w     83.00 139.00   1.00   16.00    --  108.00  64.00 150.00   56
119  \w     51.00 112.00   1.00   16.00    --  108.00-111.00 150.00   61
120  \w     79.00 106.00   1.00   16.00    --  108.00  77.00  60.00   27
121  \w     77.00 102.00   1.00   16.00    --  108.00  77.00 -30.00   25
122  \w     76.00 103.00   1.00   16.00    --  108.00  77.00 120.00   27
123  \w     77.00 102.00   1.00   16.00    --  108.00  77.00 -60.00   25
124  \w     36.00 108.00   1.00   16.00    --  108.00 -92.00 -60.00   72
125  \w    105.00 148.00   1.00   16.00    --  108.00  77.00 -90.00   43
126  \w     76.00 103.00   1.00   16.00    --  108.00  77.00 -90.00   27
127  \w    116.00 178.00   1.00   16.00    --  108.00  77.00-180.00   62
128  \w     76.00 102.00   1.00   16.00    --  108.00  77.00-180.00   26
129  \w     76.00 176.00   1.00   16.00    --  108.00  77.00-150.00  100
130  \w     36.00 112.00   1.00   16.00    --  108.00-111.00-150.00   76
131  \w     86.00 112.00   1.00   16.00    --  108.00-111.00  30.00   26
132  \w     40.00  74.00   1.00   16.00    --  108.00-111.00  30.00   34
133  \w    106.00 177.00   1.00   16.00    --  108.00  77.00  30.00   71
134  \w     76.00 103.00   1.00   16.00    --  108.00  77.00  30.00   27
135  \w     76.00 102.00   1.00   16.00    --  108.00  77.00  90.00   26
136  \w     76.00 102.00   1.00   16.00    --  108.00  77.00   0.00   26
137  \w     84.00 176.00   1.00   16.00    --  108.00  64.00 -30.00   92
138  \w    126.00 167.00   1.00   16.00    --  108.00  64.00  60.00   41
139  \w     84.00 122.00   1.00   16.00    --  108.00  64.00  60.00   38
140  \w     50.00  77.00   1.00   16.00    --  108.00 -92.00  90.00   27
141  \w    141.00 175.00   1.00   16.00    --  108.00 111.00  90.00   34
142  \w    103.00 176.00   1.00   16.00    --  108.00 111.00 -90.00   73
143  \w     83.00 110.00   1.00   16.00    --  108.00  38.00  60.00   27
144  \w    121.00 148.00   1.00   16.00    --  108.00 111.00-150.00   27
145  \w     36.00 107.00   1.00   16.00    --  108.00 -92.00  30.00   71
146  \w     47.00  74.00   1.00   16.00    --  108.00 -92.00-150.00   27
147  \w     36.00 103.00   1.00   16.00    --  108.00 -92.00-120.00   67
148  \w    136.00 163.00   1.00   16.00    --  108.00  64.00 -60.00   27
149  \w     84.00 132.00   1.00   16.00    --  108.00  64.00 -60.00   48
150  \w     84.00 113.00   1.00   16.00    --  108.00  63.00-154.41   29
151  \w     83.00 167.00   1.00   16.00    --  108.00  64.00   0.00   84
152  \w     84.00 109.00   1.00   16.00    --  108.00  64.00-150.00   25
153  \w     78.00 155.00   1.00   16.00    --  108.00  76.00 159.01   77
154  \w     77.00 104.00   1.00   16.00    --  108.00  77.00 150.00   27
155  \w     83.00 175.00   1.00   16.00    --  108.00  64.00 120.00   92
156  \w     83.00 110.00   1.00   16.00    --  108.00  64.00 -90.00   27
157  \w     83.00 133.00   1.00   16.00    --  108.00  64.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0160555000
_diffrn_orient_matrix_UB_12      -0.0144257000
_diffrn_orient_matrix_UB_13      -0.0880651000
_diffrn_orient_matrix_UB_21      -0.1261192000
_diffrn_orient_matrix_UB_22      -0.0887564000
_diffrn_orient_matrix_UB_23      -0.0021034000
_diffrn_orient_matrix_UB_31      -0.0962835000
_diffrn_orient_matrix_UB_32      0.1141290000
_diffrn_orient_matrix_UB_33      -0.0034572000
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60236
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.715
_diffrn_reflns_theta_min         4.170
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       needle
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.028(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         18074
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0690P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.876
_reflns_Friedel_fraction_max     0.845
_reflns_number_gt                15882
_reflns_number_total             18074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09111d2.cif
_cod_data_source_block           ga_vv34_5
_cod_depositor_comments
'Adding full bibliography for 7125679--7125681.cif.'
_cod_original_cell_volume        1814.72(7)
_cod_original_formula_sum        'C38 H46 Mg N3 O3.50 Si'
_cod_database_code               7125679
_audit_block_refno               3180
_audit_block_usercomment         'VVPE6, needle, red'
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.901
_shelxl_version_number           2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6605(8)
 0.3395(8)
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
 C35-C34A \\sim C35-C34B
 with sigma of 0.02
 C33-C34A \\sim C33-C34B
 with sigma of 0.02
 C36-C34A \\sim C36-C34B
 with sigma of 0.04
 O3-C34A \\sim O3-C34B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34A \\sim C34B \\sim C35 \\sim C36 \\sim C51 \\sim C52 \\sim C53 \\sim
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim
C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim
C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim
C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim
C86 \\sim C91 \\sim C92 \\sim C93 \\sim C94: within 1A with sigma of 0.01 and
sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C33, C34A, C34B, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(H35C)=Sof(H35D)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H35A)=Sof(H35B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16), C51(H51), C66(H66)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B), C29(H29A,H29B), C33(H33A,H33B), C33(H33C,H33D),
 C34A(H34A,H34B), C34B(H34C,H34D), C35(H35A,H35B), C35(H35C,H35D), C36(H36A,
 H36B), C52(H52A,H52B), C65(H65A,H65B), C79(H79A,H79B), C83(H83A,H83B),
 C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C91(H91A,H91B), C93(H93A,H93B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C63(H63), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78)
7.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C80(H80A,H80B,
 H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C92(H92A,H92B,H92C), C94(H94A,
 H94B,H94C)
;
_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
- Detector area scaling
;
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 179.9760\%
 around [0.97 -0.00 -0.25] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_shelx_res_checksum              25442
_cell_oxdiff_length_a            9.7605(2)
_cell_oxdiff_length_b            10.6398(2)
_cell_oxdiff_length_c            17.7151(4)
_cell_oxdiff_angle_alpha         94.6517(18)
_cell_oxdiff_angle_beta          98.1677(18)
_cell_oxdiff_angle_gamma         90.4055(18)
_cell_oxdiff_volume              1814.72(7)
_cell_oxdiff_measurement_reflns_used 20729