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_4081435
_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_absolute_configuration ad
_chemical_formula_moiety         'C31 H53 N Ni P2'
_chemical_formula_sum            'C31 H53 N Ni P2'
_chemical_formula_weight         560.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ak22
_audit_creation_date
;
'Fri Nov 18 17:04:01 2011'
;
_audit_update_record             'Fri Apr  5 16:53:57 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1007(4)
_cell_length_b                   14.7680(5)
_cell_length_c                   20.7811(6)
_cell_measurement_reflns_used    22672
_cell_measurement_temperature    115(1)
_cell_measurement_theta_max      71.8547
_cell_measurement_theta_min      3.6687
_cell_volume                     3099.86(18)
_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 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   31.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 37

  2 omega   28.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 36

  3 omega  -21.00    6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 27

  4 omega  -20.00   15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 35

  5 omega  -50.00   -1.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0000  -76.0000  -51.0000 49

  6 omega  -91.00  -54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.0000  -76.0000  -51.0000 37

  7 omega  -24.00    2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  -80.0000    4.0000 26

  8 omega  -27.00    0.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000  -78.0000  116.0000 27

  9 omega   10.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  118.0000 25

 10 omega   13.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000  166.0000 31

 11 omega  -49.00   -2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -150.0000 47

 12 omega  -37.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -30.0000 67

 13 omega  -58.00  -28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000   60.0000 30

 14 omega  -15.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000   60.0000 39

 15 omega  -39.00   25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -90.0000 64

 16 omega   14.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000 -121.0000 25

 17 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -146.0000 25

 18 omega   14.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   85.0000 25

 19 omega   14.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -80.0000 25

 20 omega   15.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   30.0000 25

 21 omega   18.00   43.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -29.0000 25

 22 omega   18.00   43.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -143.0000 25

 23 omega   19.00   44.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -60.0000 25

 24 omega   19.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000    5.0000 30

 25 omega   24.00  112.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -109.0000 88

 26 omega   35.00   61.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -77.0000 26

 27 omega   23.00   48.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  151.0000 25

 28 omega   25.00   51.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  108.0000 26

 29 omega   74.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000  -77.0000 50

 30 omega   95.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -92.0000 26

 31 omega   29.00   78.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -92.0000 49

 32 omega   29.00  113.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  151.0000 84

 33 omega   28.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   47.0000 59

 34 omega   32.00  100.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000   94.0000 68

 35 omega   28.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -19.0000 100

 36 omega   29.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  175.0000 99

 37 omega    4.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   68.0000 77

 38 omega   41.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000  -84.0000 58

 39 omega   30.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  166.0000 69

 40 omega   39.00   65.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  117.0000 26

 41 omega   85.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 28

 42 omega   78.00  103.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -51.0000 25

 43 omega   49.00   75.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -51.0000 26

 44 omega   40.00  140.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -79.0000   29.0000 100

 45 omega   80.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 98

 46 omega   80.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 96

 47 omega   88.00  118.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -150.0000 30

 48 omega  124.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 54

 49 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 26

 50 omega  151.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 27

 51 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

 52 omega  140.00  166.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 53 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

 54 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

 55 omega   80.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 25

 56 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 26

 57 omega  111.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 67

 58 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 26

 59 omega   80.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 25

 60 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 26

 61 omega   90.00  121.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   90.0000 31

 62 omega   88.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -90.0000 89

 63 omega  143.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 34

 64 omega   93.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 26

 65 omega   88.00  161.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  -60.0000 73

 66 omega   88.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -120.0000 26

 67 omega  117.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 60

 68 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   60.0000 26

 69 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 26

 70 omega   88.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000  150.0000 90

 71 omega   88.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000   90.0000 89

 72 omega   45.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -165.0000 59

 73 omega   92.00  118.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -150.0000 26

 74 omega   88.00  150.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 62

 75 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   90.0000 26

 76 omega   89.00  116.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  150.0000 27

 77 omega   88.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000    0.0000 26

 78 omega  111.00  177.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 66

 79 omega   70.00  142.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -126.0000 72

 80 omega   80.00  105.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 25

 81 omega   88.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   63.0000 -180.0000 88

 82 omega   69.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  117.0000 50

 83 omega  -73.00   44.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -30.0000 117

 84 omega  -26.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 98

 85 omega   10.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -153.0000 36

 86 omega -115.00  -17.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -38.0000    0.0000 98

 87 omega -115.00  -17.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -38.0000  150.0000 98

 88 omega   14.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -33.0000 32

 89 omega   18.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -29.0000 28

 90 omega   18.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -143.0000 28

 91 omega   19.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -78.0000 30

 92 omega   19.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   52.0000 28

 93 omega   23.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   99.0000 26

 94 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -109.0000 100

 95 omega   28.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -92.0000 100

 96 omega   32.00  127.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   70.0000   94.0000 95

 97 omega  -13.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000   69.0000 103

 98 omega   31.00  127.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   72.0000  178.0000 96

 99 omega   29.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -98.0000 99

100 omega   28.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -19.0000 100

101 omega   28.00  128.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   47.0000 100

102 omega   -5.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  123.0000 103

103 omega   -5.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   68.0000 103

104 omega   -1.00  102.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  -58.0000 103

105 omega    7.00  110.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  166.0000 103

106 omega    8.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000  -84.0000 101

107 omega    7.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -147.0000 102

108 omega   11.00  114.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  -10.0000 103

109 omega   37.00   62.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000 -120.0000 25

110 omega   37.00   94.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -25.0000  -30.0000 57

;
_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      -0.0002336000
_diffrn_orient_matrix_UB_12      0.0140214000
_diffrn_orient_matrix_UB_13      0.0734917000
_diffrn_orient_matrix_UB_21      0.0200622000
_diffrn_orient_matrix_UB_22      -0.1024471000
_diffrn_orient_matrix_UB_23      0.0098360000
_diffrn_orient_matrix_UB_31      0.1512116000
_diffrn_orient_matrix_UB_32      0.0135101000
_diffrn_orient_matrix_UB_33      -0.0008105000
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77120
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.000
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68056
_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            red
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 2236 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.019(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0321P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                5493
_reflns_number_total             5994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400711d_si_002.cif
_cod_data_source_block           ga_ak22
_cod_original_cell_volume        3099.88(18)
_cod_database_code               4081435
_audit_block_refno               1374
_audit_block_usercomment         AK334
_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 Idealised Me refined as rotating group with stretchable bonds:
 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),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.795
_shelx_hkl_checksum              61820
_cell_oxdiff_length_a            10.0997(7)
_cell_oxdiff_length_b            14.7732(6)
_cell_oxdiff_length_c            20.7762(9)
_cell_oxdiff_angle_alpha         90.088(4)
_cell_oxdiff_angle_beta          90.292(4)
_cell_oxdiff_angle_gamma         89.943(4)
_cell_oxdiff_volume              3099.9(3)
_cell_oxdiff_measurement_reflns_used 22672
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1