A 2,2′-diphosphinotolane as a versatile precursor for the synthesis of P-ylidic mesoionic carbenes via reversible C‒P bond formation
Wagner, Hannah K.; Wadepohl, Hubert; Ballmann, Joachim; Chemical Science 12 (2021) 3693–3701; doi:10.1039/D0SC06128J

data_1560218
_publ_section_title
;
 A 2,2&#x2032;-diphosphinotolane as a versatile precursor for the
 synthesis of P-ylidic mesoionic carbenes via reversible C--P bond
 formation
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3693
_journal_page_last               3701
_journal_paper_doi               10.1039/D0SC06128J
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C46 H66 P2 Y, C24 H20 B'
_chemical_formula_sum            'C70 H86 B P2 Y'
_chemical_formula_weight         1089.04
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_hw34
_audit_creation_date             2020-06-04
_audit_creation_method
;
encif (version 1.113)

encifer (version_id = 274361.64)

Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a3 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1824(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.84621(17)
_cell_length_b                   15.33735(10)
_cell_length_c                   19.6362(2)
_cell_measurement_reflns_used    40139
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.9180
_cell_measurement_theta_min      3.6360
_cell_volume                     5975.76(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_publication_material
'encif (Wadepohl, 2009-19); encifer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -72.00  26.00   1.00    4.00    --    0.00 -38.00-180.00   98
  2  \w    -69.00  21.00   1.00    4.00    --    0.00 -57.00 120.00   90
  3  \w    -69.00  21.00   1.00    4.00    --    0.00 -57.00 -60.00   90
  4  \w    -34.00  11.00   1.00    4.00    --   14.00 110.00 130.22   45
  5  \w    -36.00   7.00   1.00    4.00    --   14.00 114.00  13.69   43
  6  \w    -26.00  17.00   1.00    4.00    --   18.00 104.00-108.05   43
  7  \w    -31.00   4.00   1.00    4.00    --   22.00 118.00 112.22   35
  8  \w    -29.00   1.00   1.00    4.00    --   26.00 121.00 101.15   30
  9  \w    -22.00   5.00   1.00   16.00    --   30.00 117.00 -18.50   27
 10  \w    -31.00  59.00   1.00   16.00    --   38.00 -57.00-129.33   90
 11  \w      6.00  33.00   1.00   16.00    --   42.00  88.00  61.62   27
 12  \w      5.00  32.00   1.00   16.00    --   42.00  90.00 -40.48   27
 13  \w     12.00  38.00   1.00   16.00    --   46.00  84.00-113.04   26
 14  \w     13.00  40.00   1.00   16.00    --   46.00  83.00-152.84   27
 15  \w     12.00  38.00   1.00   16.00    --   46.00  84.00  75.87   26
 16  \w     12.00  38.00   1.00   16.00    --   46.00  84.00 145.61   26
 17  \w     13.00  40.00   1.00   16.00    --   46.00  83.00  -1.15   27
 18  \w     17.00  45.00   1.00   16.00    --   50.00  82.00-145.87   28
 19  \w     17.00  45.00   1.00   16.00    --   50.00  82.00 -75.01   28
 20  \w     17.00  45.00   1.00   16.00    --   50.00  82.00 169.32   28
 21  \w     18.00  45.00   1.00   16.00    --   50.00  81.00  98.39   27
 22  \w     18.00  45.00   1.00   16.00    --   50.00  80.00 -44.07   27
 23  \w     19.00  45.00   1.00   16.00    --   50.00  79.00  15.20   26
 24  \w     19.00  45.00   1.00   16.00    --   50.00  79.00  46.34   26
 25  \w     24.00 124.00   1.00   16.00    --   54.00  77.00-150.00  100
 26  \w    -15.00  75.00   1.00   16.00    --   54.00 -57.00  60.00   90
 27  \w     24.00 124.00   1.00   16.00    --   54.00  77.00 -30.00  100
 28  \w     23.00 111.00   1.00   16.00    --   54.00-125.00  60.00   88
 29  \w     24.00 124.00   1.00   16.00    --   54.00  77.00   0.00  100
 30  \w     25.00 124.00   1.00   16.00    --   54.00  76.00 116.09   99
 31  \w     23.00 111.00   1.00   16.00    --   54.00-125.00 -30.00   88
 32  \w     24.00 124.00   1.00   16.00    --   54.00  77.00  60.00  100
 33  \w    -15.00  75.00   1.00   16.00    --   54.00 -57.00 150.00   90
 34  \w     28.00 128.00   1.00   16.00    --   58.00  77.00 -52.76  100
 35  \w     28.00 128.00   1.00   16.00    --   58.00  77.00 165.02  100
 36  \w     29.00 128.00   1.00   16.00    --   58.00  75.00-115.41   99
 37  \w     29.00 128.00   1.00   16.00    --   58.00  76.00  31.36   99
 38  \w     30.00 128.00   1.00   16.00    --   58.00  74.00 130.55   98
 39  \w     29.00 128.00   1.00   16.00    --   58.00  76.00-171.44   99
 40  \w     28.00 128.00   1.00   16.00    --   58.00  77.00 108.85  100
 41  \w     28.00 128.00   1.00   16.00    --   58.00  77.00 -81.63  100
 42  \w     29.00 128.00   1.00   16.00    --   58.00  75.00 -95.87   99
 43  \w     28.00 128.00   1.00   16.00    --   58.00  77.00  71.42  100
 44  \w     28.00 128.00   1.00   16.00    --   58.00  77.00  18.49  100
 45  \w     28.00 128.00   1.00   16.00    --   58.00  77.00 149.43  100
 46  \w     30.00 128.00   1.00   16.00    --   58.00  74.00  12.80   98
 47  \w     32.00 132.00   1.00   16.00    --   62.00  77.00-101.43  100
 48  \w     34.00 132.00   1.00   16.00    --   62.00  74.00-124.45   98
 49  \w     32.00 132.00   1.00   16.00    --   62.00  77.00  44.81  100
 50  \w     33.00 132.00   1.00   16.00    --   62.00  75.00 172.09   99
 51  \w     32.00 132.00   1.00   16.00    --   62.00  77.00 -32.54  100
 52  \w     34.00 132.00   1.00   16.00    --   62.00  74.00 135.56   98
 53  \w     35.00 131.00   1.00   16.00    --   62.00  71.00 -70.58   96
 54  \w     34.00 131.00   1.00   16.00    --   62.00  73.00  82.24   97
 55  \w     32.00 132.00   1.00   16.00    --   62.00  77.00  83.77  100
 56  \w     32.00 132.00   1.00   16.00    --   62.00  77.00 149.11  100
 57  \w     35.00 110.00   1.00   16.00    --   62.00  72.00  70.95   75
 58  \w     39.00  66.00   1.00   16.00    --   62.00  70.00  28.30   27
 59  \w     35.00  62.00   1.00   16.00    --   62.00  74.00-158.85   27
 60  \w     38.00  65.00   1.00   16.00    --   66.00  77.00 134.44   27
 61  \w     39.00  66.00   1.00   16.00    --   66.00  77.00 171.34   27
 62  \w     42.00  70.00   1.00   16.00    --   66.00  67.00 124.27   28
 63  \w     37.00  64.00   1.00   16.00    --   66.00  76.00  80.47   27
 64  \w     40.00  65.00   1.00   16.00    --   66.00  72.00 170.95   25
 65  \w     37.00  64.00   1.00   16.00    --   66.00  75.00 -54.95   27
 66  \w     39.00  64.00   1.00   16.00    --   66.00  73.00  55.53   25
 67  \w     48.00  75.00   1.00   16.00    --   66.00  72.00 -27.15   27
 68  \w     41.00  68.00   1.00   16.00    --   70.00  77.00-105.72   27
 69  \w     44.00  75.00   1.00   16.00    --   70.00  70.00 138.94   31
 70  \w     41.00  73.00   1.00   16.00    --   70.00  77.00-163.89   32
 71  \w     47.00  74.00   1.00   16.00    --   70.00  74.00 147.95   27
 72  \w     42.00  68.00   1.00   16.00    --   70.00  75.00  63.93   26
 73  \w     42.00  69.00   1.00   16.00    --   70.00  75.00-150.50   27
 74  \w     47.00  74.00   1.00   16.00    --   70.00  69.00 125.55   27
 75  \w     42.00  69.00   1.00   16.00    --   70.00  76.00  -0.60   27
 76  \w     51.00  86.00   1.00   16.00    --   74.00  67.00-142.91   35
 77  \w     45.00  80.00   1.00   16.00    --   74.00  75.00-129.36   35
 78  \w     52.00 141.00   1.00   16.00    --   74.00  68.00 151.23   89
 79  \w     47.00  79.00   1.00   16.00    --   74.00  74.00 177.41   32
 80  \w     46.00  71.00   1.00   16.00    --   74.00  76.00 -72.89   25
 81  \w     52.00  79.00   1.00   16.00    --   74.00  72.00-168.19   27
 82  \w     54.00  81.00   1.00   16.00    --   74.00  64.00 101.14   27
 83  \w     48.00  75.00   1.00   16.00    --   74.00  74.00 -41.22   27
 84  \w     44.00  70.00   1.00   16.00    --   74.00  77.00  20.09   26
 85  \w     45.00  70.00   1.00   16.00    --   74.00  77.00-142.45   25
 86  \w     53.00 114.00   1.00   16.00    --   74.00  63.00 138.32   61
 87  \w     47.00  90.00   1.00   16.00    --   74.00  71.00 -16.65   43
 88  \w     54.00  81.00   1.00   16.00    --   78.00  69.00-174.40   27
 89  \w     49.00  79.00   1.00   16.00    --   78.00  77.00 156.08   30
 90  \w     59.00 113.00   1.00   16.00    --   78.00  66.00-132.29   54
 91  \w     60.00  88.00   1.00   16.00    --   78.00  74.00 -42.28   28
 92  \w     50.00  76.00   1.00   16.00    --   78.00  73.00  51.36   26
 93  \w     49.00  76.00   1.00   16.00    --   78.00  77.00 -64.86   27
 94  \w     48.00  85.00   1.00   16.00    --   78.00  77.00 -12.78   37
 95  \w     53.00  80.00   1.00   16.00    --   78.00  70.00  74.14   27
 96  \w     53.00  79.00   1.00   24.00    --   82.00  76.00 124.24   26
 97  \w     52.00  79.00   1.00   24.00    --   82.00  77.00  95.74   27
 98  \w     54.00  79.00   1.00   24.00    --   82.00  75.00 -55.76   25
 99  \w     61.00  88.00   1.00   24.00    --   82.00  65.00 -67.16   27
100  \w     56.00  83.00   1.00   24.00    --   82.00  70.00-156.66   27
101  \w     55.00  80.00   1.00   24.00    --   82.00  73.00 145.75   25
102  \w     56.00  82.00   1.00   24.00    --   82.00  72.00  14.32   26
103  \w     57.00  94.00   1.00   24.00    --   86.00  76.00 -93.93   37
104  \w     63.00 153.00   1.00   24.00    --   86.00  66.00 148.66   90
105  \w     63.00 105.00   1.00   24.00    --   86.00  74.00  12.50   42
106  \w     57.00  87.00   1.00   24.00    --   86.00  76.00  39.23   30
107  \w     73.00 100.00   1.00   24.00    --   86.00  52.00-109.53   27
108  \w     62.00 105.00   1.00   24.00    --   90.00  74.00  75.15   43
109  \w     69.00  94.00   1.00   24.00    --   90.00  61.00-154.93   25
110  \w     78.00 105.00   1.00   24.00    --   90.00  64.00-138.26   27
111  \w     69.00 155.00   1.00   24.00    --   90.00  63.00 101.27   86
112  \w     69.00 103.00   1.00   24.00    --   90.00  62.00-177.37   34
113  \w     70.00 107.00   1.00   24.00    --   94.00  68.00 117.57   37
114  \w     67.00 122.00   1.00   24.00    --   94.00  71.00 -73.99   55
115  \w     65.00  91.00   1.00   24.00    --   94.00  76.00  -9.97   26
116  \w     65.00  91.00   1.00   24.00    --   94.00  76.00  47.04   26
117  \w     67.00  92.00   1.00   24.00    --   94.00  73.00 148.47   25
118  \w     82.00 149.00   1.00   24.00    --   98.00  56.00 128.79   67
119  \w     71.00  99.00   1.00   24.00    --   98.00  74.00 146.82   28
120  \w     71.00 122.00   1.00   24.00    --   98.00  71.00-154.09   51
121  \w     77.00 103.00   1.00   24.00    --   98.00  57.00 -17.14   26
122  \w     78.00 105.00   1.00   24.00    --  108.00  77.00 120.00   27
123  \w     79.00 104.00   1.00   24.00    --  108.00  77.00  90.00   25
124  \w     78.00 105.00   1.00   24.00    --  108.00  77.00 -90.00   27
125  \w     78.00 105.00   1.00   24.00    --  108.00  77.00-120.00   27
126  \w     78.00 177.00   1.00   24.00    --  108.00  77.00  30.00   99
127  \w     78.00 104.00   1.00   24.00    --  108.00  77.00   0.00   26
128  \w     78.00 177.00   1.00   24.00    --  108.00  77.00 150.00   99
129  \w     78.00 177.00   1.00   24.00    --  108.00  77.00-150.00   99
130  \w     44.00  72.00   1.00   24.00    --  108.00-111.00  30.00   28
131  \w     79.00 178.00   1.00   24.00    --  108.00  77.00 -30.00   99
132  \w     41.00 130.00   1.00   24.00    --  108.00 -64.00  30.00   89
133  \w     85.00 167.00   1.00   24.00    --  108.00  64.00  90.00   82
134  \w     86.00 113.00   1.00   24.00    --  108.00  64.00-180.00   27
135  \w     86.00 174.00   1.00   24.00    --  108.00  64.00 120.00   88
136  \w     78.00 104.00   1.00   24.00    --  108.00  77.00 -60.00   26
137  \w    144.00 175.00   1.00   24.00    --  108.00  64.00-120.00   31
138  \w     85.00 111.00   1.00   24.00    --  108.00  64.00-120.00   26
139  \w     79.00 148.00   1.00   24.00    --  108.00  77.00  60.00   69
140  \w     36.00  81.00   1.00   24.00    --  108.00 -92.00-120.00   45
141  \w     81.00 109.00   1.00   24.00    --  108.00 -92.00  90.00   28
142  \w     36.00  92.00   1.00   24.00    --  108.00 -92.00 -30.00   56
143  \w     37.00 112.00   1.00   24.00    --  108.00-111.00-150.00   75
144  \w     81.00 166.00   1.00   24.00    --  108.00  72.00 -96.02   85
145  \w     83.00 146.00   1.00   24.00    --  108.00  38.00 -60.00   63
146  \w    115.00 156.00   1.00   24.00    --  108.00  38.00 -90.00   41
147  \w     83.00 110.00   1.00   24.00    --  108.00  38.00 -90.00   27
148  \w     86.00 111.00   1.00   24.00    --  108.00  64.00 -30.00   25
149  \w     36.00 110.00   1.00   24.00    --  108.00-115.00 -42.00   74
150  \w     78.00 163.00   1.00   24.00    --  108.00  77.00-180.00   85
151  \w     85.00 112.00   1.00   24.00    --  108.00  38.00  60.00   27
152  \w     86.00 111.00   1.00   24.00    --  108.00  64.00  60.00   25
153  \w     85.00 148.00   1.00   24.00    --  108.00  64.00  30.00   63
154  \w     53.00 112.00   1.00   24.00    --  108.00-111.00  60.00   59
155  \w    119.00 166.00   1.00   24.00    --  108.00  64.00   0.00   47
156  \w     85.00 118.00   1.00   24.00    --  108.00  64.00   0.00   33
157  \w     85.00 174.00   1.00   24.00    --  108.00  64.00 -60.00   89
;
_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      -0.0764336000
_diffrn_orient_matrix_UB_12      0.0000295000
_diffrn_orient_matrix_UB_13      0.0121127000
_diffrn_orient_matrix_UB_21      -0.0031937000
_diffrn_orient_matrix_UB_22      -0.0976692000
_diffrn_orient_matrix_UB_23      -0.0181069000
_diffrn_orient_matrix_UB_31      0.0132354000
_diffrn_orient_matrix_UB_32      -0.0234584000
_diffrn_orient_matrix_UB_33      0.0753923000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            223988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.152
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         11524
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0416P)^2^+11.6249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9272
_reflns_number_total             11524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06128j2.cif
_cod_data_source_block           ba_hw34
_cod_depositor_comments
'Adding full bibliography for 1560218--1560233.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1560218
_audit_block_refno               3571
_audit_block_usercomment         'HW327, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.812
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2018/3
_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
 C24-C25A \\sim C24-C25B \\sim C24-C26
 with sigma of 0.02
 C25A-C26 \\sim C25B-C26
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H24A)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(H24)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C21(H21), C24(H24), C24(H24A)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71),
  C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80),
 C81(H81), C82(H82), C83(H83), C84(H84)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25A(H25A,H25B,H25C),
 C25B(H25D,H25E,H25F), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.837
_shelx_res_checksum              23389
_cell_oxdiff_length_a            19.8477(4)
_cell_oxdiff_length_b            15.33707(19)
_cell_oxdiff_length_c            19.6354(4)
_cell_oxdiff_angle_alpha         90.0017(13)
_cell_oxdiff_angle_beta          91.2223(16)
_cell_oxdiff_angle_gamma         89.9933(12)
_cell_oxdiff_volume              5975.76(19)
_cell_oxdiff_measurement_reflns_used 40143