Bis(diisopropylphosphinomethyl)amine Nickel(II) and Nickel(0) Complexes: Coordination Chemistry, Reactivity, and Catalytic Decarbonylative C‒H Arylation of Benzoxazole
Kruckenberg, Achim; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 32 (2013) 5153–; doi:10.1021/om400711d

data_4081432
_publ_section_title
;
 Bis(diisopropylphosphinomethyl)amine Nickel(II) and Nickel(0) Complexes:
 Coordination Chemistry, Reactivity, and Catalytic Decarbonylative C--H
 Arylation of Benzoxazole
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5153
_journal_paper_doi               10.1021/om400711d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C17 H41 N Ni P2'
_chemical_formula_sum            'C17 H41 N Ni P2'
_chemical_formula_weight         380.16
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ak23
_audit_creation_date
;
'Thu Dec 01 13:47:03 2011'
;
_audit_update_record             'Thu Jul  4 09:22:02 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 90.076(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7071(6)
_cell_length_b                   14.5014(8)
_cell_length_c                   14.8907(11)
_cell_measurement_reflns_used    11280
_cell_measurement_temperature    115(1)
_cell_measurement_theta_max      72.0979
_cell_measurement_theta_min      4.2414
_cell_volume                     2096.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      115(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega  -70.00  -20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -150.0000 50

  2 omega  -25.00   65.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 90

  3 omega  -19.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -150.0000 40

  4 omega  -11.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   77.0000  173.0000 44

  5 omega   47.00   74.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   77.0000  173.0000 27

  6 omega  -24.00    1.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  -80.0000  125.0000 25

  7 omega   10.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -64.0000 25

  8 omega -105.00  -77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000    0.0000 28

  9 omega  -41.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000    0.0000 29

 10 omega  -52.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000 -120.0000 77

 11 omega  -50.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000   90.0000 76

 12 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -31.0000 25

 13 omega   14.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -117.0000 30

 14 omega   15.00   40.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000 -136.0000 25

 15 omega   21.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   76.0000   39.0000 26

 16 omega   20.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   -8.0000 28

 17 omega   80.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   76.0000   39.0000 27

 18 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  145.0000 25

 19 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -114.0000 25

 20 omega   73.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  123.0000 45

 21 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -62.0000 25

 22 omega   45.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  123.0000 27

 23 omega   23.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  171.0000 25

 24 omega   25.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   58.0000 27

 25 omega   74.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -29.0000 50

 26 omega   25.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -29.0000 27

 27 omega   64.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   58.0000 59

 28 omega   90.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   86.0000 34

 29 omega   25.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   86.0000 27

 30 omega   45.00   80.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -38.0000  -30.0000 35

 31 omega  -14.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       55.4296  -38.0000  -30.0000 30

 32 omega   28.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000    8.0000 73

 33 omega   28.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  102.0000 59

 34 omega   35.00   73.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -69.0000 38

 35 omega   32.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000  -94.0000 94

 36 omega   31.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000 -174.0000 96

 37 omega   76.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -69.0000 47

 38 omega   -5.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -36.0000 88

 39 omega   18.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000   90.0000 77

 40 omega   11.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000 -131.0000 76

 41 omega   79.00  125.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000  -80.0000   31.0000 46

 42 omega   41.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  -26.0000 67

 43 omega   40.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  139.0000 63

 44 omega   41.00  142.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000 -179.0000 101

 45 omega  153.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   30.0000 25

 46 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   30.0000 27

 47 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -60.0000 26

 48 omega  113.00  176.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   90.0000 63

 49 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   90.0000 26

 50 omega  119.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -120.0000 59

 51 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -120.0000 27

 52 omega   81.00  172.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -30.0000 91

 53 omega  140.00  167.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   60.0000 27

 54 omega  134.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -60.0000 29

 55 omega   82.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000   60.0000 25

 56 omega  120.00  168.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  120.0000 48

 57 omega   81.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -150.0000 94

 58 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  120.0000 27

 59 omega   89.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  -30.0000 26

 60 omega   90.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000   60.0000 26

 61 omega  120.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000    0.0000 58

 62 omega   86.00  148.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  -30.0000 62

 63 omega   90.00  161.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  150.0000 71

 64 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000    0.0000 26

 65 omega   92.00  118.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  120.0000 26

 66 omega   94.00  122.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000   30.0000 28

 67 omega   81.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  150.0000 92

 68 omega   81.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -180.0000 27

 69 omega  120.00  164.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -90.0000 44

 70 omega   85.00  148.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   90.0000 63

 71 omega   85.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -120.0000 30

 72 omega   81.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000  -90.0000 26

 73 omega   88.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000   30.0000 89

 74 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   30.0000 26

 75 omega  116.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000   52.0000 27

 76 omega  112.00  170.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   77.0000 -180.0000 58

 77 omega   91.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  -60.0000 86

 78 omega   93.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000  -90.0000 27

 79 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000  120.0000 26

 80 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000 -120.0000 27

 81 omega   45.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000   52.0000 65

 82 omega   89.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000 -180.0000 27

 83 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  -90.0000 27

 84 omega   85.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -150.0000 30

 85 omega   85.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000    0.0000 30

 86 omega   74.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -79.0000 -103.0000 29

 87 omega   85.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000 -180.0000 27

 88 omega   88.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  120.0000 26

 89 omega  -51.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000 -150.0000 31

 90 omega   -2.00   30.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000 -150.0000 32

 91 omega  -38.00  -12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000   60.0000 26

 92 omega   14.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -172.0000 25

 93 omega   19.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -136.0000 25

 94 omega   32.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   71.0000   92.0000 25

 95 omega   89.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  150.0000 25

 96 omega   91.00  118.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000 -150.0000 27

 97 omega  153.00  178.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  -60.0000 25

 98 omega   89.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000  -60.0000 25

 99 omega   88.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   63.0000 -180.0000 27

100 omega   86.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   38.0000   60.0000 25

101 omega   93.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592   50.0000    0.0000 27

102 omega   44.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.8592  -80.0000  103.0000 52

;
_diffrn_measurement_device       '\k-geometry 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_UB_11      -0.0109257000
_diffrn_orient_matrix_UB_12      -0.1057759000
_diffrn_orient_matrix_UB_13      -0.0067282000
_diffrn_orient_matrix_UB_21      0.1570134000
_diffrn_orient_matrix_UB_22      -0.0061631000
_diffrn_orient_matrix_UB_23      -0.0138744000
_diffrn_orient_matrix_UB_31      0.0203617000
_diffrn_orient_matrix_UB_32      -0.0077069000
_diffrn_orient_matrix_UB_33      0.1023027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1360
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33698
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.163
_diffrn_reflns_theta_min         4.256
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0907P)^2^+1.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3486
_reflns_number_total             4037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400711d_si_002.cif
_cod_data_source_block           ga_ak23_4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4081432
_audit_block_refno               1384
_audit_block_usercomment         'AK293 plate yellow'
_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 Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.496
_shelx_res_checksum              93139
_shelxl_version_number           2013-3
_cell_oxdiff_length_a            9.7071(6)
_cell_oxdiff_length_b            14.5015(8)
_cell_oxdiff_length_c            14.8907(11)
_cell_oxdiff_angle_alpha         90.046(5)
_cell_oxdiff_angle_beta          89.923(5)
_cell_oxdiff_angle_gamma         90.106(5)
_cell_oxdiff_volume              2096.1(2)
_cell_oxdiff_measurement_reflns_used 11280
_cell_oxdiff_twin_number         2