Isolation of arylhalodiphosphenes: periodic trends in R–PP–X bonding (X = Cl, Br, I)
Wenger, John S.; Gaschik, Nina; Rowe, William J.; Crumpton, Agamemnon E.; van IJzendoorn, Bono; Mehta, Meera; Chemical Science  (2026) –; doi:10.1039/D6SC00723F

data_1576682
_publ_section_title
;
 Isolation of arylhalodiphosphenes: periodic trends in R-P[double bond,
 length as m-dash]P-X bonding (X = Cl, Br, I).
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              7475
_journal_page_last               7485
_journal_paper_doi               10.1039/d6sc00723f
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C72 H91 P, C6 H14'
_chemical_formula_sum            'C78 H105 P'
_chemical_formula_weight         1073.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-04 deposited with the CCDC.	2026-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0641(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.46887(5)
_cell_length_b                   26.12266(10)
_cell_length_c                   20.84307(9)
_cell_measurement_reflns_used    108493
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2220
_cell_measurement_theta_min      1.6770
_cell_volume                     6639.07(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.92a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_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-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     28.00  54.00   0.50    0.92    --   60.11 -97.00-114.00   52
  2  \w     42.00  68.00   0.50    0.92    --   73.66 -97.00-114.00   52
  3  \w     41.00  66.00   0.50    0.92    --   79.84 -97.00-114.00   50
  4  \w     12.00  37.00   0.50    0.92    --   60.11 -30.00  90.00   50
  5  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00  30.00   50
  6  \w     27.00  66.00   0.50    0.92    --   60.11 -95.00 150.00   78
  7  \w     11.00  37.00   0.50    0.92    --   60.11 -30.00   0.00   52
  8  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00-120.00   50
  9  \w     19.00  85.00   0.50    0.92    --   60.11-125.00-120.00  132
 10  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00-180.00   50
 11  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00  60.00   50
 12  \w     64.00  95.00   0.50    0.92    --   60.11  30.00  60.00   62
 13  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00 -60.00   50
 14  \w     61.00  92.00   0.50    0.92    --   60.11  30.00-150.00   62
 15  \w     20.00  63.00   0.50    0.92    --   60.11 -95.00 -60.00   86
 16  \w     76.00 123.00   0.50    0.92    --   73.66  30.00 -90.00   94
 17  \w     37.00  73.00   0.50    0.92    --   73.66 -95.00  90.00   72
 18  \w     35.00  84.00   0.50    0.92    --   73.66 -95.00  60.00   98
 19  \w     92.00 118.00   0.50    0.92    --   73.66  30.00 120.00   52
 20  \w     87.00 121.00   0.50    0.92    --   73.66  30.00  90.00   68
 21  \w     77.00 103.00   0.50    0.92    --   73.66-125.00-120.00   52
 22  \w     85.00 115.00   0.50    0.92    --   73.66  15.00  30.00   60
 23  \w     87.00 115.00   0.50    0.92    --   73.66  30.00 -30.00   56
 24  \w     55.00  84.00   0.50    0.92    --   73.66 -95.00 -30.00   58
 25  \w     35.00  74.00   0.50    0.92    --   73.66 -95.00   0.00   78
 26  \w     43.00 103.00   0.50    0.92    --   73.66-125.00 -30.00  120
 27  \w     82.00 122.00   0.50    0.92    --   73.66  30.00  60.00   80
 28  \w     41.00  80.00   0.50    0.92    --   73.66  15.00  30.00   78
 29  \w     44.00  76.00   0.50    0.92    --   79.84 -95.00 150.00   64
 30  \w     42.00  75.00   0.50    0.92    --   79.84 -95.00   0.00   66
 31  \w     40.00  65.00   0.50    0.92    --   79.84 -95.00-150.00   50
 32  \w     62.00  88.00   0.50    0.92    --   79.84-125.00-150.00   52
 33  \w     41.00  90.00   0.50    0.92    --   79.84 -95.00  90.00   98
 34  \w     64.00  98.00   0.50    0.92    --   79.84-125.00  30.00   68
 35  \w     90.00 118.00   0.50    0.92    --   79.84  30.00  90.00   56
 36  \w     81.00 106.00   0.50    0.92    --   79.84  30.00  30.00   50
 37  \w     44.00  95.00   0.50    0.92    --   79.84-125.00-180.00  102
 38  \w     52.00 109.00   0.50    0.92    --   79.84-125.00 150.00  114
 39  \w     61.00  86.00   0.50    0.92    --   79.84-125.00 -90.00   50
 40  \w     40.00  66.00   0.50    0.92    --   79.84-125.00 120.00   52
 41  \w     43.00  69.00   0.50    0.92    --   79.84 -95.00 -90.00   52
 42  \w     81.00 106.00   0.50    0.92    --   79.84  30.00-120.00   50
 43  \w     82.00 108.00   0.50    0.92    --   79.84  30.00 -30.00   52
 44  \w     75.00 100.00   0.50    0.92    --   79.84-125.00 -60.00   50
 45  \w    102.00 129.00   0.50    0.92    --   79.84  30.00 150.00   54
 46  \w     46.00  72.00   0.50    0.92    --   79.84 -95.00 120.00   52
 47  \w     57.00  83.00   0.50    0.92    --   79.84 -95.00  60.00   52
 48  \w     50.00  76.00   0.50    0.92    --   79.84 -95.00 -60.00   52
 49  \w     40.00  65.00   0.50    0.92    --   79.84-125.00  90.00   50
 50  \w     80.00 125.00   0.50    0.92    --   83.00   4.00 -22.00   90
 51  \w     52.00  79.00   0.50    0.92    --   83.00   4.00 -22.00   54
 52  \w     45.00 110.00   0.50    0.92    --   83.00-120.00  82.29  130
 53  \w     77.00 122.00   0.50    0.92    --   83.00  15.00  99.09   90
 54  \w     61.00  92.00   0.50    0.92    --   83.00  20.00-118.61   62
 55  \w     68.00 125.00   0.50    0.92    --   83.00   3.00-174.00  114
 56  \w     48.00 124.00   0.50    0.92    --   83.00   6.00-101.57  152
 57  \w     93.00 118.00   0.50    0.92    --   83.00  59.00-100.82   50
 58  \w     59.00 100.00   0.50    0.92    --   83.00-111.00 173.53   82
 59  \w     39.00 110.00   0.50    0.92    --   83.00-122.00   0.79  142
 60  \w     91.00 120.00   0.50    0.92    --   83.00  57.00 143.10   58
 61  \w     44.00 117.00   0.50    0.92    --   83.00-132.00  64.30  146
 62  \w     66.00 128.00   0.50    0.92    --   83.00  21.00 -46.65  124
 63  \w     54.00 107.00   0.50    0.92    --   83.00-116.00-147.92  106
 64  \w     47.00 116.00   0.50    0.92    --   83.00-131.00-100.19  138
 65  \w     45.00  85.00   0.50    0.92    --   83.00-101.00 -36.93   80
 66  \w     59.00 104.00   0.50    0.92    --   83.00-112.00 -49.97   90
 67  \w     55.00  80.00   0.50    0.92    --   83.00  20.00 -97.04   50
 68  \w     65.00  99.00   0.50    0.92    --   83.00  22.00 -79.79   68
 69  \w     85.00 111.00   0.50    0.92    --   83.00  22.00  54.84   52
 70  \w     65.00 108.00   0.50    0.92    --   83.00  22.00 160.46   86
 71  \w     46.00  88.00   0.50    0.92    --   83.00 -87.00-113.75   84
 72  \w     90.00 115.00   0.50    0.92    --   83.00  64.00 -78.99   50
 73  \w     50.00  96.00   0.50    0.92    --   83.00  14.00  44.72   92
 74  \w     35.00  60.00   0.50    0.92    --   73.66 -97.00-114.00   50
 75  \w    -50.00 -12.00   0.50    0.92    --   -3.00 -44.00 133.32   76
 76  \w    -15.00  10.00   0.50    0.92    --   -3.00-100.00 -28.79   50
 77  \w    -16.00  10.00   0.50    0.92    --   -3.00-100.00  -3.48   52
 78  \w    -16.00  10.00   0.50    0.92    --   -3.00 -99.00  61.10   52
 79  \w    -39.00 -12.00   0.50    0.92    --   -3.00 -46.00 -26.04   54
 80  \w     -8.00  17.00   0.50    0.92    --    6.00 101.00 112.81   50
 81  \w     -3.00  22.00   0.50    0.92    --   10.00  99.00  63.40   50
 82  \w      8.00  33.00   0.50    0.92    --   18.00  94.00-152.47   50
 83  \w     16.00  41.00   0.50    0.92    --   22.00  88.00  58.82   50
 84  \w     14.00  41.00   0.50    0.92    --   22.00  91.00 -24.31   54
 85  \w     15.00  40.00   0.50    0.92    --   22.00  89.00-107.52   50
 86  \w     13.00  38.00   0.50    0.92    --   22.00  92.00 131.38   50
 87  \w     31.00  56.00   0.50    0.92    --   30.00  77.00-146.34   50
 88  \w     32.00  57.00   0.50    0.92    --   30.00  75.00 -81.95   50
 89  \w     31.00  56.00   0.50    0.92    --   30.00  77.00  77.99   50
 90  \w     31.00  56.00   0.50    0.92    --   30.00  77.00 159.85   50
 91  \w     35.00  60.00   0.50    0.92    --   34.00  77.00 -57.69   50
 92  \w     35.00  60.00   0.50    0.92    --   34.00  77.00 105.33   50
 93  \w     37.00  62.00   0.50    0.92    --   34.00  73.00-105.98   50
 94  \w     39.00  64.00   0.50    0.92    --   38.00  77.00  12.75   50
 95  \w     40.00  65.00   0.50    0.92    --   38.00  76.00 144.36   50
 96  \w     44.00  69.00   0.50    0.92    --   42.00  76.00 -15.99   50
 97  \w     45.00  70.00   0.50    0.92    --   42.00  73.00  45.38   50
 98  \w     43.00  68.00   0.50    0.92    --   42.00  77.00 176.64   50
 99  \w     44.00  69.00   0.50    0.92    --   42.00  76.00 -41.01   50
100  \w     47.00  72.00   0.50    0.92    --   46.00  77.00 104.38   50
101  \w     47.00  72.00   0.50    0.92    --   46.00  77.00-109.50   50
102  \w     47.00  72.00   0.50    0.92    --   46.00  77.00 -82.25   50
103  \w     48.00  73.00   0.50    0.92    --   46.00  76.00 143.75   50
104  \w     48.00  73.00   0.50    0.92    --   46.00  76.00  63.44   50
105  \w     47.00  72.00   0.50    0.92    --   46.00  77.00 -95.19   50
106  \w     48.00  73.00   0.50    0.92    --   46.00  75.00-150.90   50
107  \w     53.00  78.00   0.50    0.92    --   50.00  73.00 -16.48   50
108  \w     53.00  78.00   0.50    0.92    --   50.00  73.00 119.50   50
109  \w     52.00  77.00   0.50    0.92    --   50.00  76.00  72.65   50
110  \w     55.00  80.00   0.50    0.92    --   54.00  77.00 -47.22   50
111  \w     55.00  80.00   0.50    0.92    --   54.00  77.00 -19.40   50
112  \w     55.00  80.00   0.50    0.92    --   54.00  77.00-161.70   50
113  \w     55.00  80.00   0.50    0.92    --   54.00  77.00 159.19   50
114  \w     55.00  80.00   0.50    0.92    --   54.00  77.00  -2.05   50
115  \w     55.00  80.00   0.50    0.92    --   54.00  77.00 -69.35   50
116  \w     55.00  80.00   0.50    0.92    --   54.00  77.00 172.06   50
117  \w     55.00  80.00   0.50    0.92    --   54.00  77.00  25.24   50
118  \w     55.00  80.00   0.50    0.92    --   54.00  77.00   6.90   50
119  \w     63.00  88.00   0.50    0.92    --   58.00  69.00  52.90   50
120  \w     64.00  89.00   0.50    0.92    --   58.00  68.00 105.94   50
121  \w     63.00  88.00   0.50    0.92    --   58.00  71.00 -45.62   50
122  \w     64.00  89.00   0.50    0.92    --   58.00  67.00-122.23   50
123  \w     62.00  87.00   0.50    0.92    --   58.00  72.00-136.01   50
124  \w     63.00  88.00   0.50    0.92    --   58.00  71.00 124.66   50
125  \w     61.00  86.00   0.50    0.92    --   58.00  73.00 144.03   50
126  \w     64.00  89.00   0.50    0.92    --   58.00  68.00  89.45   50
127  \w     63.00  88.00   0.50    0.92    --   58.00  71.00 112.34   50
128  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00 -90.00   50
129  \w     22.00  48.00   0.50    0.92    --   60.11-125.00 -60.00   52
130  \w     11.00  37.00   0.50    0.92    --   60.11 -30.00 -30.00   52
131  \w     11.00  36.00   0.50    0.92    --   60.11 -30.00 120.00   50
132  \w     66.00  91.00   0.50    0.92    --   62.00  72.00 -41.75   50
133  \w     67.00  99.00   0.50    0.92    --   62.00  71.00 -17.86   64
134  \w     67.00  96.00   0.50    0.92    --   62.00  70.00-162.16   58
135  \w     66.00  91.00   0.50    0.92    --   62.00  72.00  56.94   50
136  \w     67.00  92.00   0.50    0.92    --   62.00  71.00 129.12   50
137  \w     68.00  93.00   0.50    0.92    --   66.00  75.00 -92.66   50
138  \w     68.00  93.00   0.50    0.92    --   66.00  75.00-107.82   50
139  \w     69.00  94.00   0.50    0.92    --   66.00  73.00  -5.90   50
140  \w     69.00  94.00   0.50    0.92    --   66.00  73.00 164.91   50
141  \w     69.00  94.00   0.50    0.92    --   66.00  74.00-151.66   50
142  \w     69.00  94.00   0.50    0.92    --   66.00  74.00  58.12   50
143  \w     69.00  98.00   0.50    0.92    --   66.00  73.00 141.87   58
144  \w     69.00  94.00   0.50    0.92    --   66.00  74.00  -2.11   50
145  \w     72.00 105.00   0.50    0.92    --   70.00  75.00 -79.75   66
146  \w     77.00 104.00   0.50    0.92    --   73.66  30.00 150.00   54
147  \w     72.00 113.00   0.50    0.92    --   73.66   0.00-120.00   82
148  \w     42.00  68.00   0.50    0.92    --   73.66   0.00-120.00   52
149  \w     32.00  57.00   0.50    0.92    --   73.66-125.00 120.00   50
150  \w     81.00 106.00   0.50    0.92    --   74.00  62.00 176.38   50
151  \w     85.00 111.00   0.50    0.92    --   78.00  60.00  22.75   52
152  \w     81.00 125.00   0.50    0.92    --   79.84  30.00 -90.00   88
153  \w     49.00  77.00   0.50    0.92    --   79.84   0.00 -60.00   56
154  \w     36.00  63.00   0.50    0.92    --   79.84-125.00  30.00   54
155  \w     36.00  62.00   0.50    0.92    --   79.84-125.00 150.00   52
156  \w     81.00 106.00   0.50    0.92    --   79.84  30.00 120.00   50
157  \w     81.00 110.00   0.50    0.92    --   79.84  30.00   0.00   58
158  \w     38.00  64.00   0.50    0.92    --   79.84-125.00-150.00   52
159  \w     41.00  67.00   0.50    0.92    --   79.84-125.00-120.00   52
160  \w     37.00  63.00   0.50    0.92    --   79.84-125.00 -60.00   52
161  \w     36.00  62.00   0.50    0.92    --   79.84-125.00 -90.00   52
162  \w     80.00 112.00   0.50    0.92    --   79.84   0.00 -60.00   64
163  \w     77.00 103.00   0.50    0.92    --   83.00  27.00  79.78   52
164  \w     42.00  76.00   0.50    0.92    --   83.00-100.00  80.97   68
165  \w     92.00 117.00   0.50    0.92    --   83.00  46.00-143.69   50
166  \w     40.00  66.00   0.50    0.92    --   83.00-116.00 -31.51   52
167  \w     85.00 110.00   0.50    0.92    --   83.00-120.00 -54.45   50
168  \w     41.00  67.00   0.50    0.92    --   83.00-120.00 -54.45   52
169  \w     63.00 123.00   0.50    0.92    --   83.00   2.00 102.46  120
170  \w     68.00 113.00   0.50    0.92    --   83.00   3.00 156.00   90
171  \w     42.00  86.00   0.50    0.92    --   83.00-100.00 136.39   88
172  \w     94.00 119.00   0.50    0.92    --   83.00  39.00 142.97   50
173  \w     93.00 118.00   0.50    0.92    --   83.00  38.00 110.44   50
174  \w     49.00  81.00   0.50    0.92    --   83.00  -1.00  44.80   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0136270000
_diffrn_orient_matrix_UB_12      0.0275118000
_diffrn_orient_matrix_UB_13      0.0665897000
_diffrn_orient_matrix_UB_21      -0.0424383000
_diffrn_orient_matrix_UB_22      -0.0479986000
_diffrn_orient_matrix_UB_23      0.0297020000
_diffrn_orient_matrix_UB_31      0.1182409000
_diffrn_orient_matrix_UB_32      -0.0204181000
_diffrn_orient_matrix_UB_33      0.0198857000
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            300587
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         2.750
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.98789
_exptl_absorpt_correction_T_min  0.98789
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.92a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.046
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13589
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0435P)^2^+2.9085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12215
_reflns_number_total             13589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00723f3.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
'Adding full bibliography for 1576673--1576682.cif.'
_cod_original_cell_volume        6639.06(5)
_cod_database_code               1576682
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C78 H103 P1'
_cell_oxdiff_angle_alpha         90.0080(5)
_cell_oxdiff_angle_beta          102.0775(5)
_cell_oxdiff_angle_gamma         89.9805(5)
_cell_oxdiff_length_a            12.46753(8)
_cell_oxdiff_length_b            26.12374(15)
_cell_oxdiff_length_c            20.84548(13)
_cell_oxdiff_measurement_reflns_used 108493
_cell_oxdiff_volume              6639.06(7)
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-C1 \\sim P1A-C1
 with sigma of 0.02
 P1-H1A \\sim P1A-H1AA
 with sigma of 0.01
 P1-H1B \\sim P1A-H1AB
 with sigma of 0.01
 H1B-H1A \\sim H1AB-H1AA
 with sigma of 0.01
3. Others
 Sof(P1A)=Sof(H1AA)=Sof(H1AB)=1-FVAR(1)
 Sof(P1)=Sof(H1A)=Sof(H1B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C21(H21A,H21B), C22(H22A,H22B), C31(H31A,H31B),
 C32(H32A,H32B), C49(H49A,H49B), C50(H50A,H50B), C59(H59A,H59B), C60(H60A,H60B),
  C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C18(H18), C25(H25), C28(H28), C35(H35), C46(H46), C53(H53), C56(H56),
 C63(H63)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              22818
_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_exptl_absorpt_empirical_full_max 1.750
_oxdiff_exptl_absorpt_empirical_full_min 0.529