Synthesis of NPN-Coordinated Tantalum Alkyl Complexes and Their Hydrogenolysis: Isolation of a Terminal Tantalum Hydride Incorporating a Doubly Cyclometalated NPN Scaffold
Batke, Sonja; Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00277

data_4345728
_publ_section_title
;
 Synthesis of NPN-Coordinated Tantalum Alkyl Complexes and Their
 Hydrogenolysis: Isolation of a Terminal Tantalum Hydride Incorporating a
 Doubly Cyclometalated NPN Scaffold
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00277
_journal_year                    2017
_chemical_formula_moiety         'C42 H50 N2 P3 Ta'
_chemical_formula_sum            'C42 H50 N2 P3 Ta'
_chemical_formula_weight         856.70
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_jb23
_audit_creation_date             2016-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
'15.02.2016 12:27:23 CET UTC+01:00  encif 1.38'
_cell_angle_alpha                90
_cell_angle_beta                 102.6140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.20187(4)
_cell_length_b                   22.75735(6)
_cell_length_c                   17.01422(5)
_cell_measurement_reflns_used    126604
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6850
_cell_measurement_theta_min      4.4360
_cell_volume                     3854.81(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41p (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      perfluoro
_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 0.996
_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    -30.00  70.00   1.00    1.00    --    0.00  77.00 120.00  100
  2  \w    -21.00  69.00   1.00    1.00    --    0.00  57.00   0.00   90
  3  \w    -69.00  21.00   1.00    1.00    --    0.00 -57.00   0.00   90
  4  \w    -71.00 -13.00   1.00    1.00    --    0.00 147.00 148.00   58
  5  \w    -57.00  -2.00   1.00    1.00    --    0.00 125.00 -17.00   55
  6  \w    -25.00  11.00   1.00    1.00    --   22.00 109.00  61.55   36
  7  \w    -22.00   5.00   1.00    2.00    --   30.00 117.00  -1.12   27
  8  \w    -40.00 -13.00   1.00    2.00    --   30.00 145.00 -34.22   27
  9  \w     -9.00  18.00   1.00    2.00    --   34.00 102.00-173.39   27
 10  \w     -2.00  24.00   1.00    2.00    --   38.00  96.00 135.76   26
 11  \w      6.00  33.00   1.00    2.00    --   42.00  88.00 -70.92   27
 12  \w      6.00  33.00   1.00    2.00    --   42.00  88.00-178.27   27
 13  \w     12.00  38.00   1.00    2.00    --   46.00  84.00 -93.45   26
 14  \w     13.00  40.00   1.00    2.00    --   46.00  83.00 -49.96   27
 15  \w     13.00  40.00   1.00    2.00    --   46.00  83.00-149.51   27
 16  \w     12.00  38.00   1.00    2.00    --   46.00  84.00  83.11   26
 17  \w     12.00  38.00   1.00    2.00    --   46.00  84.00-125.84   26
 18  \w     18.00  46.00   1.00    2.00    --   50.00  81.00  38.94   28
 19  \w     18.00  46.00   1.00    2.00    --   50.00  80.00 -80.41   28
 20  \w     18.00  46.00   1.00    2.00    --   50.00  80.00-171.39   28
 21  \w     17.00  45.00   1.00    2.00    --   50.00  82.00  -0.01   28
 22  \w     18.00  46.00   1.00    2.00    --   50.00  80.00-134.85   28
 23  \w     17.00  45.00   1.00    2.00    --   50.00  82.00 107.16   28
 24  \w    -15.00  75.00   1.00    2.00    --   54.00 -57.00  90.00   90
 25  \w     25.00 124.00   1.00    2.00    --   54.00  75.00  -4.60   99
 26  \w     24.00 124.00   1.00    2.00    --   54.00  77.00-150.00  100
 27  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 150.00  100
 28  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00 -90.00  100
 29  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 120.00  100
 30  \w     23.00 111.00   1.00    2.00    --   54.00-125.00 -95.00   88
 31  \w     24.00 124.00   1.00    2.00    --   54.00  77.00-180.00  100
 32  \w     23.00  49.00   1.00    2.00    --   54.00  78.00 -73.81   26
 33  \w     23.00 111.00   1.00    2.00    --   54.00-125.00  90.00   88
 34  \w     28.00 128.00   1.00    2.00    --   58.00  77.00  31.50  100
 35  \w     28.00 128.00   1.00    2.00    --   58.00  77.00-107.56  100
 36  \w     28.00 119.00   1.00    2.00    --   58.00  77.00 168.05   91
 37  \w     28.00 128.00   1.00    2.00    --   58.00  77.00  69.51  100
 38  \w     35.00 125.00   1.00    2.00    --   58.00  64.00 144.61   90
 39  \w     39.00 130.00   1.00    2.00    --   62.00  65.00-160.83   91
 40  \w     32.00 132.00   1.00    2.00    --   62.00  77.00-135.36  100
 41  \w     33.00 132.00   1.00    2.00    --   62.00  75.00  43.38   99
 42  \w     40.00 135.00   1.00    2.00    --   66.00  70.00-153.02   95
 43  \w     45.00 134.00   1.00    2.00    --   66.00  60.00 -85.45   89
 44  \w     37.00 136.00   1.00    2.00    --   66.00  75.00 142.32   99
 45  \w     45.00 136.00   1.00    2.00    --   66.00  52.00  37.35   91
 46  \w     45.00 135.00   1.00    2.00    --   66.00  58.00-164.40   90
 47  \w     43.00 134.00   1.00    2.00    --   66.00  66.00  77.67   91
 48  \w     47.00 137.00   1.00    2.00    --   70.00  64.00 -86.47   90
 49  \w     43.00 139.00   1.00    2.00    --   70.00  71.00  25.72   96
 50  \w     41.00 140.00   1.00    2.00    --   70.00  75.00 -42.51   99
 51  \w     48.00 138.00   1.00    2.00    --   70.00  63.00 -56.15   90
 52  \w     47.00 138.00   1.00    2.00    --   70.00  65.00 -51.54   91
 53  \w     47.00 137.00   1.00    2.00    --   70.00  64.00 117.78   90
 54  \w     48.00 138.00   1.00    2.00    --   70.00  62.00  85.43   90
 55  \w     50.00 146.00   1.00    2.00    --   74.00  43.00 -80.25   96
 56  \w     53.00 143.00   1.00    2.00    --   74.00  57.00 141.29   90
 57  \w     48.00 143.00   1.00    2.00    --   74.00  70.00 131.88   95
 58  \w     52.00 142.00   1.00    2.00    --   74.00  62.00 105.81   90
 59  \w     57.00 147.00   1.00    2.00    --   78.00  58.00 152.62   90
 60  \w     54.00 146.00   1.00    2.00    --   78.00  67.00 -46.78   92
 61  \w     50.00 148.00   1.00    2.00    --   78.00  74.00-171.27   98
 62  \w     49.00 148.00   1.00    2.00    --   78.00  75.00 124.89   99
 63  \w     51.00 147.00   1.00    2.00    --   78.00  71.00 -84.11   96
 64  \w     53.00 152.00   1.00    4.00    --   82.00  75.00  28.62   99
 65  \w     53.00 152.00   1.00    4.00    --   82.00  75.00 -31.17   99
 66  \w     53.00 152.00   1.00    4.00    --   82.00  75.00 -92.29   99
 67  \w     60.00 152.00   1.00    4.00    --   82.00  49.00 -20.73   92
 68  \w     55.00 151.00   1.00    4.00    --   82.00  72.00-142.73   96
 69  \w     53.00 152.00   1.00    4.00    --   82.00  76.00 157.29   99
 70  \w     65.00 155.00   1.00    4.00    --   86.00  58.00-173.61   90
 71  \w     57.00 156.00   1.00    4.00    --   86.00  76.00 111.43   99
 72  \w     57.00 156.00   1.00    4.00    --   86.00  76.00  69.70   99
 73  \w     62.00 154.00   1.00    4.00    --   86.00  67.00  -0.37   92
 74  \w     68.00 158.00   1.00    4.00    --   90.00  62.00  69.75   90
 75  \w     67.00 158.00   1.00    4.00    --   90.00  66.00  37.60   91
 76  \w     63.00 159.00   1.00    4.00    --   90.00  71.00-166.83   96
 77  \w     71.00 167.00   1.00    4.00    --   98.00  72.00-143.94   96
 78  \w     71.00 167.00   1.00    4.00    --   98.00  72.00-150.73   96
 79  \w     73.00 172.00   1.00    4.00    --  102.00  75.00-159.83   99
 80  \w     79.00 170.00   1.00    4.00    --  102.00  66.00 171.85   91
 81  \w     77.00 170.00   1.00    4.00    --  102.00  69.00 -99.09   93
 82  \w     86.00 176.00   1.00    4.00    --  108.00  63.00 -24.70   90
 83  \w     82.00 178.00   1.00    4.00    --  108.00  38.00  30.00   96
 84  \w     85.00 175.00   1.00    4.00    --  108.00  64.00 -90.00   90
 85  \w     78.00 178.00   1.00    4.00    --  108.00  77.00-180.00  100
 86  \w     82.00 178.00   1.00    4.00    --  108.00  38.00 -90.00   96
 87  \w     85.00 175.00   1.00    4.00    --  108.00  64.00 -60.00   90
 88  \w     85.00 175.00   1.00    4.00    --  108.00  64.00   0.00   90
 89  \w     85.00 175.00   1.00    4.00    --  108.00  64.00 -30.00   90
 90  \w     80.00 178.00   1.00    4.00    --  108.00  74.00 -79.68   98
 91  \w     85.00 175.00   1.00    4.00    --  108.00  64.00  60.00   90
 92  \w     85.00 175.00   1.00    4.00    --  108.00  64.00  30.00   90
 93  \w     85.00 175.00   1.00    4.00    --  108.00  64.00  90.00   90
 94  \w     78.00 178.00   1.00    4.00    --  108.00  77.00-120.00  100
 95  \w     41.00 131.00   1.00    4.00    --  108.00 -64.00-180.00   90
 96  \w     85.00 175.00   1.00    4.00    --  108.00  64.00-180.00   90
 97  \w     78.00 178.00   1.00    4.00    --  108.00  77.00 150.00  100
 98  \w     78.00 178.00   1.00    4.00    --  108.00  77.00 -90.00  100
 99  \w     36.00 116.00   1.00    4.00    --  108.00-111.00-180.00   80
100  \w     78.00 178.00   1.00    4.00    --  108.00  77.00 120.00  100
101  \w     78.00 178.00   1.00    4.00    --  108.00  77.00-150.00  100
102  \w     78.00 178.00   1.00    4.00    --  108.00  77.00 -30.00  100
103  \w     85.00 175.00   1.00    4.00    --  108.00  64.00-120.00   90
104  \w     78.00 178.00   1.00    4.00    --  108.00  77.00 -60.00  100
105  \w     78.00 178.00   1.00    4.00    --  108.00  77.00  90.00  100
106  \w     85.00 175.00   1.00    4.00    --  108.00  64.00 150.00   90
107  \w     78.00 178.00   1.00    4.00    --  108.00  77.00  30.00  100
108  \w     36.00 116.00   1.00    4.00    --  108.00-111.00 -60.00   80
109  \w     36.00 116.00   1.00    4.00    --  108.00-111.00 120.00   80
110  \w     78.00 178.00   1.00    4.00    --  108.00  77.00   0.00  100
111  \w     78.00 178.00   1.00    4.00    --  108.00  77.00  60.00  100
112  \w     85.00 175.00   1.00    4.00    --  108.00  64.00 120.00   90
113  \w     38.00 138.00   1.00    4.00    --  108.00 -77.00   0.00  100
114  \w     38.00 138.00   1.00    4.00    --  108.00 -77.00 150.00  100
115  \w     36.00 116.00   1.00    4.00    --  108.00-111.00   0.00   80
116  \f      0.00 120.00   1.00    1.00   0.00   0.00 -40.00    --   120
117  \f    120.00 240.00   1.00    1.00   0.00   0.00  40.00    --   120
118  \f      0.00 120.00   1.00    1.00   0.00   0.00 -60.00    --   120
119  \f      0.00 120.00   1.00    1.00   0.00   0.00  60.00    --   120
120  \f    120.00 240.00   1.00    1.00   0.00   0.00 -40.00    --   120
121  \f    120.00 240.00   1.00    1.00   0.00   0.00  60.00    --   120
122  \f      0.00 120.00   1.00    1.00   0.00   0.00  40.00    --   120
123  \f    120.00 240.00   1.00    1.00   0.00   0.00 -60.00    --   120
124  \f    120.00 240.00   1.00    2.00  54.00  54.00  40.00    --   120
125  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 -60.00  100
126  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 -90.00  100
127  \f    120.00 240.00   1.00    2.00  54.00  54.00 -40.00    --   120
128  \w     24.00 124.00   1.00    2.00    --   54.00  77.00  30.00  100
129  \f    120.00 240.00   1.00    2.00  54.00  54.00 -60.00    --   120
130  \f      0.00 120.00   1.00    2.00  54.00  54.00  60.00    --   120
131  \f      0.00 120.00   1.00    2.00  54.00  54.00 -60.00    --   120
132  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00  30.00  100
133  \f    240.00 360.00   1.00    2.00  54.00  54.00  60.00    --   120
134  \f      0.00 120.00   1.00    2.00  54.00  54.00  40.00    --   120
135  \w     24.00 124.00   1.00    2.00    --   54.00  77.00-180.00  100
136  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00 150.00  100
137  \w     24.00 124.00   1.00    2.00    --   54.00  77.00-120.00  100
138  \f    240.00 360.00   1.00    2.00  54.00  54.00 -60.00    --   120
139  \f    240.00 360.00   1.00    2.00  54.00  54.00  40.00    --   120
140  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 -30.00  100
141  \w     24.00 124.00   1.00    2.00    --   54.00  77.00   0.00  100
142  \f      0.00 120.00   1.00    2.00  54.00  54.00 -40.00    --   120
143  \w     24.00 124.00   1.00    2.00    --   54.00  77.00  60.00  100
144  \w     24.00 124.00   1.00    2.00    --   54.00  77.00  90.00  100
145  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 120.00  100
146  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00-120.00  100
147  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00-150.00  100
148  \f    240.00 360.00   1.00    2.00  54.00  54.00 -40.00    --   120
149  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00-180.00  100
150  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00 -90.00  100
151  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00 -60.00  100
152  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00 -30.00  100
153  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00   0.00  100
154  \w     24.00 124.00   1.00    2.00    --   54.00  77.00 150.00  100
155  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00  60.00  100
156  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00  90.00  100
157  \w    -16.00  84.00   1.00    2.00    --   54.00 -77.00 120.00  100
158  \f    120.00 240.00   1.00    2.00  54.00  54.00  60.00    --   120
159  \w     24.00 124.00   1.00    2.00    --   54.00  77.00-150.00  100
160  \w     28.00 124.00   1.00    2.00    --   58.00  77.00 168.05   96
161  \w     28.00 128.00   1.00    2.00    --   58.00  77.00-107.56  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0883719000
_diffrn_orient_matrix_UB_12      0.0375504000
_diffrn_orient_matrix_UB_13      0.0664350000
_diffrn_orient_matrix_UB_21      0.0483229000
_diffrn_orient_matrix_UB_22      -0.0561108000
_diffrn_orient_matrix_UB_23      0.0483030000
_diffrn_orient_matrix_UB_31      0.1174204000
_diffrn_orient_matrix_UB_32      -0.0050985000
_diffrn_orient_matrix_UB_33      -0.0431720000
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            239678
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.886
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.672
_exptl_absorpt_correction_T_max  0.754
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41p (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.473
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0166P)^2^+3.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0397
_refine_ls_wR_factor_ref         0.0406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6931
_reflns_number_total             7412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00277_si_002.cif
_cod_data_source_block           ba_jb23
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4345728
_audit_block_refno               2651
_audit_block_usercomment         'jb291, irregular, yellow'
_chemical_oxdiff_formula         'C42 H48 N2 P3 Ta'
_chemical_oxdiff_usercomment     'jb291, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.555
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2014/7
_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.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              60519
_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 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.783
_cell_oxdiff_length_a            10.20481(10)
_cell_oxdiff_length_b            22.75287(17)
_cell_oxdiff_length_c            17.01294(14)
_cell_oxdiff_angle_alpha         90.0314(6)
_cell_oxdiff_angle_beta          102.6178(8)
_cell_oxdiff_angle_gamma         90.0374(7)
_cell_oxdiff_volume              3854.81(6)
_cell_oxdiff_measurement_reflns_used 126604