Isolation and structural characterization of a titanacyclopropane as key intermediate in the double aryl Grignard addition to 2-(arylethynyl)pyridine derivatives.
Foschi, Francesco; Roth, Torsten; Enders, Markus; Wadepohl, Hubert; Clot, Eric; Gade, Lutz H.; Chemical communications (Cambridge, England) 54 (2018) 2228–2231; doi:10.1039/c8cc00478a

data_7121236
_publ_section_title
;
 Isolation and structural characterization of a titanacyclopropane as key
 intermediate in the double aryl Grignard addition to
 2-(arylethynyl)pyridine derivatives.
;
_journal_issue                   18
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2228
_journal_page_last               2231
_journal_paper_doi               10.1039/c8cc00478a
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C24 H18 F2 N2'
_chemical_formula_sum            'C24 H18 F2 N2'
_chemical_formula_weight         372.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_tro59
_audit_creation_date             2018-01-15
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:44:14 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-17 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1238(3)
_cell_length_b                   8.54517(18)
_cell_length_c                   15.8226(3)
_cell_measurement_reflns_used    15217
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      66.9260
_cell_measurement_theta_min      5.5790
_cell_volume                     1909.63(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -12.00  20.00   1.00    5.00    --    0.00 -38.00 -30.00   32
  2  \w    -43.00 -17.00   1.00    5.00    --    0.00  19.00-180.00   26
  3  \w    -40.00 -14.00   1.00    5.00    --    0.00 -38.00 -30.00   26
  4  \w    -69.00 -16.00   1.00    5.00    --    0.00 -38.00-120.00   53
  5  \w     12.00  70.00   1.00    5.00    --    0.00  19.00-180.00   58
  6  \w    -26.00  24.00   1.00    5.00    --    0.00  77.00-120.00   50
  7  \w     28.00  70.00   1.00    5.00    --    0.00  77.00-120.00   42
  8  \w     -9.00  42.00   1.00    5.00    --   14.00  80.00 -41.72   51
  9  \w     -6.00  19.00   1.00    5.00    --   26.00  80.00 125.49   25
 10  \w     -1.00  34.00   1.00   15.00    --   30.00  78.00-156.59   35
 11  \w      2.00  27.00   1.00   15.00    --   34.00  80.00 -62.41   25
 12  \w      6.00  31.00   1.00   15.00    --   38.00  80.00 166.44   25
 13  \w     11.00  37.00   1.00   15.00    --   42.00  80.00  -3.51   26
 14  \w     11.00  36.00   1.00   15.00    --   42.00  79.00 152.46   25
 15  \w     10.00  46.00   1.00   15.00    --   42.00  80.00  68.67   36
 16  \w     17.00  44.00   1.00   15.00    --   46.00  77.00 -72.62   27
 17  \w     90.00 116.00   1.00   15.00    --   46.00  75.00 -19.91   26
 18  \w     19.00  45.00   1.00   15.00    --   46.00  75.00 -19.91   26
 19  \w     19.00  44.00   1.00   15.00    --   50.00  78.00 154.71   25
 20  \w     19.00  44.00   1.00   15.00    --   50.00  79.00  55.32   25
 21  \w     19.00  44.00   1.00   15.00    --   50.00  79.00 113.58   25
 22  \w     24.00  50.00   1.00   15.00    --   54.00  77.00-180.00   26
 23  \w     26.00  53.00   1.00   15.00    --   54.00  77.00-150.00   27
 24  \w     24.00  50.00   1.00   15.00    --   54.00  77.00-123.76   26
 25  \w     24.00  51.00   1.00   15.00    --   54.00  77.00  90.00   27
 26  \w     23.00  48.00   1.00   15.00    --   54.00  78.00-162.46   25
 27  \w     31.00  57.00   1.00   15.00    --   54.00  77.00 -30.00   26
 28  \w     18.00  83.00   1.00   15.00    --   54.00 -77.00 -60.00   65
 29  \w     24.00  53.00   1.00   15.00    --   54.00  77.00  30.00   29
 30  \w     24.00  52.00   1.00   15.00    --   54.00  77.00   0.00   28
 31  \w     55.00  82.00   1.00   15.00    --   54.00  77.00-123.76   27
 32  \w    -16.00  82.00   1.00   15.00    --   54.00 -78.00 -90.26   98
 33  \w     29.00  56.00   1.00   15.00    --   54.00  77.00  60.00   27
 34  \w    -17.00  84.00   1.00   15.00    --   54.00 -79.00  53.20  101
 35  \w     23.00  48.00   1.00   15.00    --   54.00  78.00 -75.57   25
 36  \w     73.00 123.00   1.00   15.00    --   54.00  77.00  90.00   50
 37  \w     35.00  62.00   1.00   15.00    --   58.00  71.00 156.00   27
 38  \w     37.00  64.00   1.00   15.00    --   58.00  77.00 -74.03   27
 39  \w     40.00  67.00   1.00   15.00    --   58.00  59.00 124.85   27
 40  \w     31.00  57.00   1.00   15.00    --   58.00  75.00   8.55   26
 41  \w     78.00 104.00   1.00   15.00    --   58.00  74.00 133.05   26
 42  \w     34.00  61.00   1.00   15.00    --   58.00  70.00  37.82   27
 43  \w     31.00  56.00   1.00   15.00    --   58.00  74.00 133.05   25
 44  \w     35.00  61.00   1.00   15.00    --   62.00  76.00-110.63   26
 45  \w     40.00  67.00   1.00   15.00    --   62.00  71.00  43.26   27
 46  \w     33.00  58.00   1.00   15.00    --   62.00  77.00 -90.53   25
 47  \w     39.00  65.00   1.00   15.00    --   66.00  73.00-140.41   26
 48  \w     43.00 120.00   1.00   15.00    --   66.00  69.00 -41.74   77
 49  \w     43.00  69.00   1.00   15.00    --   66.00  64.00 134.09   26
 50  \w     38.00  65.00   1.00   15.00    --   66.00  75.00  48.33   27
 51  \w     40.00  67.00   1.00   15.00    --   66.00  77.00 143.92   27
 52  \w     42.00 103.00   1.00   15.00    --   70.00  73.00-162.67   61
 53  \w     44.00  85.00   1.00   15.00    --   70.00  70.00 172.27   41
 54  \w     52.00  78.00   1.00   15.00    --   70.00  59.00 -94.61   26
 55  \w     41.00  66.00   1.00   15.00    --   70.00  75.00  14.79   25
 56  \w     45.00  91.00   1.00   15.00    --   70.00  75.00 -80.55   46
 57  \w     53.00  80.00   1.00   15.00    --   74.00 -80.00  96.46   27
 58  \w     52.00  83.00   1.00   15.00    --   74.00  66.00  24.43   31
 59  \w     49.00 108.00   1.00   15.00    --   74.00  72.00  34.24   59
 60  \w     49.00  75.00   1.00   15.00    --   74.00  70.00 135.48   26
 61  \w     57.00  86.00   1.00   15.00    --   74.00  66.00  78.67   29
 62  \w     45.00  80.00   1.00   15.00    --   74.00  76.00  59.16   35
 63  \w     47.00  90.00   1.00   15.00    --   74.00  73.00-145.41   43
 64  \w      4.00 106.00   1.00   15.00    --   74.00 -80.00 150.50  102
 65  \w     53.00  80.00   1.00   15.00    --   78.00  76.00 -28.96   27
 66  \w     57.00  85.00   1.00   15.00    --   78.00  63.00  46.48   28
 67  \w     51.00  77.00   1.00   15.00    --   78.00  72.00 -93.87   26
 68  \w     54.00  80.00   1.00   15.00    --   78.00  72.00 141.28   26
 69  \w     53.00  81.00   1.00   15.00    --   78.00  69.00 -32.50   28
 70  \w     52.00 145.00   1.00   15.00    --   78.00  72.00  -9.95   93
 71  \w     57.00  83.00   1.00   15.00    --   78.00  65.00 103.45   26
 72  \w     60.00 109.00   1.00   30.00    --   82.00  63.00 150.96   49
 73  \w     63.00  88.00   1.00   30.00    --   82.00  47.00 135.07   25
 74  \w     57.00 145.00   1.00   30.00    --   82.00  70.00 -94.14   88
 75  \w     57.00  83.00   1.00   30.00    --   82.00  70.00  59.71   26
 76  \w     55.00 107.00   1.00   30.00    --   82.00  71.00-174.97   52
 77  \w     57.00  84.00   1.00   30.00    --   82.00  70.00 -27.20   27
 78  \w     67.00  94.00   1.00   30.00    --   86.00 -80.00  31.85   27
 79  \w     87.00 120.00   1.00   30.00    --   86.00  77.00 151.06   33
 80  \w     57.00  82.00   1.00   30.00    --   86.00  77.00 151.06   25
 81  \w     62.00  99.00   1.00   30.00    --   86.00  69.00-153.15   37
 82  \w     65.00 103.00   1.00   30.00    --   94.00  75.00  56.99   38
 83  \w     73.00 123.00   1.00   30.00    --   94.00  58.00-120.08   50
 84  \w     69.00 103.00   1.00   30.00    --   98.00  76.00 -58.52   34
 85  \w     79.00 106.00   1.00   30.00    --   98.00  57.00  94.57   27
 86  \w     72.00  98.00   1.00   30.00    --   98.00  72.00 115.04   26
 87  \w     73.00 101.00   1.00   30.00    --   98.00  72.00  20.58   28
 88  \w     75.00 148.00   1.00   30.00    --  102.00  75.00 150.13   73
 89  \w     84.00 157.00   1.00   30.00    --  108.00  38.00 -60.00   73
 90  \w     82.00 142.00   1.00   30.00    --  108.00  38.00-150.00   60
 91  \w     85.00 174.00   1.00   30.00    --  108.00  64.00 -60.00   89
 92  \w     59.00  85.00   1.00   30.00    --  108.00 -38.00 -60.00   26
 93  \w    109.00 170.00   1.00   30.00    --  108.00  77.00   0.00   61
 94  \w     79.00 104.00   1.00   30.00    --  108.00  77.00   0.00   25
 95  \w     83.00 110.00   1.00   30.00    --  108.00  77.00 150.00   27
 96  \w     38.00 140.00   1.00   30.00    --  108.00 -80.00 -69.56  102
 97  \w     85.00 137.00   1.00   30.00    --  108.00  64.00-150.00   52
 98  \w     78.00 104.00   1.00   30.00    --  108.00  77.00  60.00   26
 99  \w     81.00 106.00   1.00   30.00    --  108.00  77.00  30.00   25
100  \w    115.00 140.00   1.00   30.00    --  108.00 -80.00  28.26   25
101  \w     65.00 108.00   1.00   30.00    --  108.00 -80.00  28.26   43
102  \w     78.00 105.00   1.00   30.00    --  108.00  77.00-180.00   27
103  \w     84.00 134.00   1.00   30.00    --  108.00 -77.00 150.00   50
104  \w    115.00 140.00   1.00   30.00    --  108.00 -80.00-126.13   25
105  \w    136.00 166.00   1.00   30.00    --  108.00  77.00 -90.00   30
106  \w     78.00 104.00   1.00   30.00    --  108.00  77.00 -90.00   26
107  \w     79.00 178.00   1.00   30.00    --  108.00  77.00  90.00   99
108  \w    112.00 176.00   1.00   30.00    --  108.00  77.00-150.00   64
109  \w     79.00 104.00   1.00   30.00    --  108.00  77.00-150.00   25
110  \w     86.00 113.00   1.00   30.00    --  108.00  64.00-120.00   27
111  \w     76.00 107.00   1.00   30.00    --  108.00 -79.00-153.19   31
112  \w     86.00 175.00   1.00   30.00    --  108.00  64.00-180.00   89
113  \w     71.00 100.00   1.00   30.00    --  108.00 -80.00-126.13   29
114  \w    151.00 177.00   1.00   30.00    --  108.00  77.00 -60.00   26
115  \w     78.00 104.00   1.00   30.00    --  108.00  77.00 -60.00   26
116  \w     86.00 174.00   1.00   30.00    --  108.00  64.00  60.00   88
117  \w     85.00 111.00   1.00   30.00    --  108.00  64.00   0.00   26
118  \w     79.00 177.00   1.00   30.00    --  108.00  77.00 120.00   98
119  \w    112.00 177.00   1.00   30.00    --  108.00  77.00-120.00   65
120  \w     47.00 139.00   1.00   30.00    --  108.00 -80.00  91.34   92
121  \w     78.00 104.00   1.00   30.00    --  108.00  77.00-120.00   26
122  \w     78.00 177.00   1.00   30.00    --  108.00  77.00 -30.00   99
123  \w     85.00 114.00   1.00   30.00    --  108.00  64.00 -90.00   29
124  \w     84.00 111.00   1.00   30.00    --  108.00 -80.00 -37.07   27
125  \w     80.00 178.00   1.00   30.00    --  108.00  76.00  18.92   98
126  \w     79.00 104.00   1.00   30.00    --  108.00  77.00  74.92   25
127  \w    -70.00  30.00   1.00    5.00    --    0.00 -77.00 120.00  100
128  \w    -21.00  69.00   1.00    5.00    --    0.00  57.00   0.00   90
129  \w    -26.00  72.00   1.00    5.00    --    0.00  38.00  90.00   98
130  \w    -21.00  69.00   1.00    5.00    --    0.00  57.00 150.00   90
131  \w     -6.00  91.00   1.00    5.00    --   22.00  73.00-166.69   97
132  \w     -9.00  47.00   1.00    5.00    --   22.00  79.00-132.18   56
133  \w     -6.00  46.00   1.00    5.00    --   26.00  80.00 125.49   52
134  \w      7.00  49.00   1.00   15.00    --   38.00  78.00 -54.74   42
135  \w     11.00  47.00   1.00   15.00    --   42.00  79.00 152.46   36
136  \w     19.00  47.00   1.00   15.00    --   50.00  79.00  55.32   28
137  \w     19.00  49.00   1.00   15.00    --   50.00  78.00 154.71   30
138  \w     23.00  49.00   1.00   15.00    --   54.00  78.00 -75.57   26
139  \w     23.00  49.00   1.00   15.00    --   54.00  78.00-162.46   26
140  \w    -15.00  75.00   1.00   15.00    --   54.00 -57.00-180.00   90
141  \w    -18.00  80.00   1.00   15.00    --   54.00 -38.00  30.00   98
142  \w     30.00 128.00   1.00   15.00    --   58.00  74.00 133.05   98
143  \w     -5.00  98.00   1.00   15.00    --   66.00 -80.00  57.13  103
144  \w     41.00 134.00   1.00   15.00    --   66.00  69.00 -41.74   93
145  \w     42.00 139.00   1.00   15.00    --   70.00  73.00-162.67   97
146  \w     44.00 139.00   1.00   15.00    --   70.00  70.00 172.27   95
147  \w     41.00 140.00   1.00   15.00    --   70.00  75.00 -80.55   99
148  \w      4.00 105.00   1.00   15.00    --   74.00 -78.00 -82.57  101
149  \w     47.00 143.00   1.00   15.00    --   74.00  72.00  34.24   96
150  \w      3.00 106.00   1.00   15.00    --   74.00 -80.00  96.46  103
151  \w     48.00 143.00   1.00   15.00    --   74.00  70.00 135.48   95
152  \w      3.00 106.00   1.00   15.00    --   74.00 -80.00 150.50  103
153  \w     45.00 135.00   1.00   15.00    --   74.00  76.00  59.16   90
154  \w     46.00 143.00   1.00   15.00    --   74.00  73.00-145.41   97
155  \w     56.00 148.00   1.00   15.00    --   78.00  50.00 -82.22   92
156  \w     51.00 147.00   1.00   15.00    --   78.00  72.00 141.28   96
157  \w     56.00 146.00   1.00   15.00    --   78.00  63.00  46.48   90
158  \w     51.00 147.00   1.00   15.00    --   78.00  72.00  -9.95   96
159  \w     53.00 146.00   1.00   15.00    --   78.00  69.00 -32.50   93
160  \w     55.00 146.00   1.00   15.00    --   78.00  65.00 103.45   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, 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      -0.0551686000
_diffrn_orient_matrix_UB_12      0.1553099000
_diffrn_orient_matrix_UB_13      0.0043282000
_diffrn_orient_matrix_UB_21      0.0085647000
_diffrn_orient_matrix_UB_22      -0.0009746000
_diffrn_orient_matrix_UB_23      0.0970682000
_diffrn_orient_matrix_UB_31      0.0937449000
_diffrn_orient_matrix_UB_32      0.0914091000
_diffrn_orient_matrix_UB_33      -0.0063390000
_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  0.1686
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56245
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.373
_diffrn_reflns_theta_max         67.373
_diffrn_reflns_theta_min         5.592
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 981 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3420
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0928
_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^)+(0.1589P)^2^+1.2955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2666
_refine_ls_wR_factor_ref         0.3170
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2778
_reflns_number_total             3420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00478a2.cif
_cod_data_source_block           ga_tro59
_cod_depositor_comments
'Adding full bibliography for 7121234--7121240.cif.'
_cod_original_cell_volume        1909.64(7)
_cod_database_code               7121236
_audit_block_refno               1961
_audit_block_usercomment         'tr1209, needle, colourless'
_chemical_oxdiff_formula         'C24 H18 F2 N2'
_chemical_oxdiff_usercomment     'tr1209, needle, colourless'
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.837
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24)
;
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 14.959
_oxdiff_exptl_absorpt_empirical_full_min 0.092
_shelx_res_checksum              21118
_cell_oxdiff_length_a            14.1194(3)
_cell_oxdiff_length_b            8.5484(2)
_cell_oxdiff_length_c            15.8215(3)
_cell_oxdiff_angle_alpha         89.9940(16)
_cell_oxdiff_angle_beta          89.9910(15)
_cell_oxdiff_angle_gamma         89.9786(18)
_cell_oxdiff_volume              1909.64(7)
_cell_oxdiff_measurement_reflns_used 15217