Ruthenium η4-Trimethylenemethane Complexes Containing Tripodal Phosphanomethylamine Ligands
Scherl, Peter; Kruckenberg, Achim; Mader, Steffen; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 31 (2012) 7024–; doi:10.1021/om300794h

data_4079530
_publ_section_title
;
 Ruthenium \h4-Trimethylenemethane Complexes Containing Tripodal
 Phosphanomethylamine Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              7024
_journal_paper_doi               10.1021/om300794h
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_sum            'C25 H48 N P3 Ru'
_chemical_formula_weight         556.62
_space_group_IT_number           19
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ps13
_audit_creation_date
;
'Wed Jan 11 11:09:39 2012'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_audit_update_record             'Wed Jan 11 11:26:35 CET 2012'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.48059(6)
_cell_length_b                   9.12047(6)
_cell_length_c                   34.1042(3)
_cell_measurement_reflns_used    43845
_cell_measurement_temperature    114.97(11)
_cell_measurement_theta_max      71.8186
_cell_measurement_theta_min      3.8852
_cell_volume                     2637.86(3)
_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_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      114.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -16.00   23.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 39

  2 omega  -69.00   13.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -30.0000 82

  3 omega   -5.00   38.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       22.0000   80.0000  -56.0000 43

  4 omega   10.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -76.0000 25

  5 omega   12.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000  -11.0000 34

  6 omega   10.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   80.0000 -173.0000 25

  7 omega  -65.00   24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000  120.0000 89

  8 omega  -45.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000   90.0000 75

  9 omega  -61.00  -13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 48

 10 omega  -45.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -90.0000 75

 11 omega -113.00  -69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  150.0000 44

 12 omega   15.00   40.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   29.0000 25

 13 omega   18.00   43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -78.0000 25

 14 omega   18.00   43.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -165.0000 25

 15 omega   19.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  106.0000 25

 16 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   68.0000 25

 17 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -143.0000 25

 18 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  142.0000 25

 19 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -39.0000 25

 20 omega   23.00   48.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   38.0000 25

 21 omega   28.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -159.0000 26

 22 omega   31.00   68.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   62.0000 37

 23 omega   65.00  127.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -44.0000 62

 24 omega   28.00   58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -44.0000 30

 25 omega   28.00   55.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  141.0000 27

 26 omega   82.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  141.0000 46

 27 omega   28.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -113.0000 81

 28 omega   36.00   83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000  149.0000 47

 29 omega   97.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  -22.0000 26

 30 omega    0.00   93.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000  -65.0000 93

 31 omega   35.00   61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  -22.0000 26

 32 omega   34.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000 -141.0000 63

 33 omega   90.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000  149.0000 26

 34 omega   33.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000   85.0000 81

 35 omega   38.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000 -149.0000 46

 36 omega   36.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000    0.0000 92

 37 omega   47.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000   94.0000 62

 38 omega   65.00  134.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000  -80.0000 -174.0000 69

 39 omega  113.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000 -122.0000 26

 40 omega   89.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   63.0000    0.0000 26

 41 omega   78.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000 -122.0000 27

 42 omega   39.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000 -122.0000 36

 43 omega   85.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   38.0000  120.0000 93

 44 omega   39.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000  -51.0000 67

 45 omega   80.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  150.0000 27

 46 omega  110.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000 -150.0000 67

 47 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000 -150.0000 26

 48 omega   88.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   63.0000   60.0000 89

 49 omega  119.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000 -120.0000 54

 50 omega   80.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000 -120.0000 25

 51 omega   80.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000   30.0000 97

 52 omega   80.00  174.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  -60.0000 94

 53 omega  153.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   50.0000   90.0000 25

 54 omega  112.00  174.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  150.0000 62

 55 omega   88.00  113.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   50.0000   90.0000 25

 56 omega  151.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  120.0000 26

 57 omega   80.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  120.0000 25

 58 omega  118.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  -30.0000 60

 59 omega   81.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  -30.0000 26

 60 omega  137.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   63.0000    0.0000 38

 61 omega   80.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000   90.0000 26

 62 omega   85.00  156.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   38.0000  -60.0000 71

 63 omega   85.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   38.0000 -150.0000 43

 64 omega  139.00  165.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  -90.0000 26

 65 omega   98.00  156.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   50.0000   30.0000 58

 66 omega   80.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000  -90.0000 25

 67 omega   96.00  122.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   50.0000    0.0000 26

 68 omega   82.00  108.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000    0.0000 26

 69 omega   85.00  155.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   38.0000  150.0000 70

 70 omega   85.00  111.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   38.0000  -90.0000 26

 71 omega   85.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   38.0000 -180.0000 27

 72 omega   88.00  145.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   63.0000 -150.0000 57

 73 omega  130.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000 -180.0000 43

 74 omega   91.00  117.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   50.0000  -90.0000 26

 75 omega   63.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000  143.0000 43

 76 omega   83.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -77.0000   90.0000 26

 77 omega   80.00  105.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   77.0000 -180.0000 25

 78 omega   49.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000   26.0000 93

 79 omega  -30.00   70.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -180.0000 100

 80 omega  -26.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   90.0000 98

 81 omega  -19.00   80.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   76.0000    0.0000 99

 82 omega  -50.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -150.0000 80

 83 omega   15.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -56.0000 32

 84 omega   15.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000 -137.0000 32

 85 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  143.0000 28

 86 omega   19.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  158.0000 28

 87 omega   18.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -78.0000 28

 88 omega   19.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  106.0000 30

 89 omega   18.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -165.0000 28

 90 omega   25.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000 -168.0000 99

 91 omega   23.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   38.0000 26

 92 omega   24.00  124.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -70.0000 100

 93 omega  -17.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000   14.0000 103

 94 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  110.0000 100

 95 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -159.0000 100

 96 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -113.0000 100

 97 omega   29.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   52.0000 99

 98 omega   28.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  -44.0000 100

 99 omega   33.00  132.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000 -141.0000 99

100 omega   34.00  132.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000  -22.0000 98

101 omega   34.00  131.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000    0.0000 97

102 omega   33.00  132.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000   85.0000 99

103 omega   36.00  131.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000  149.0000 95

104 omega   -1.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000  -80.0000  161.0000 103

105 omega    7.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -79.0000 -151.0000 102

106 omega    8.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000 -142.0000 101

107 omega    7.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000   94.0000 103

108 omega    7.00  110.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -80.0000 103

109 omega   39.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -80.0000   26.0000 103

110 omega   88.00  125.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   50.0000 -150.0000 37

111 omega   38.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -38.0000 -120.0000 55

112 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -25.0000  120.0000 57

113 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -25.0000   30.0000 57

114 omega   88.00  178.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580   63.0000   30.0000 90

115 omega   37.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1580  -25.0000  -60.0000 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      -0.1772549000
_diffrn_orient_matrix_UB_12      0.0157528000
_diffrn_orient_matrix_UB_13      -0.0089150000
_diffrn_orient_matrix_UB_21      -0.0069454000
_diffrn_orient_matrix_UB_22      -0.1626475000
_diffrn_orient_matrix_UB_23      -0.0120608000
_diffrn_orient_matrix_UB_31      -0.0390703000
_diffrn_orient_matrix_UB_32      -0.0427478000
_diffrn_orient_matrix_UB_33      0.0426151000
_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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            75987
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         71.8186
_diffrn_reflns_theta_min         3.8852
_diffrn_source                   'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.610
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.1608
_exptl_crystal_size_mid          0.0531
_exptl_crystal_size_min          0.0393
_refine_diff_density_max         1.222
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.5127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0485
_reflns_number_gt                5116
_reflns_number_total             5168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300794h_si_002.cif
_cod_data_source_block           compound_6
_cod_original_cell_volume        2637.85(3)
_cod_database_code               4079530
_audit_block_refno               1409
_audit_block_usercomment         PS306
_cell_oxdiff_length_a            8.48128(15)
_cell_oxdiff_length_b            9.12074(16)
_cell_oxdiff_length_c            34.1003(5)
_cell_oxdiff_angle_alpha         89.9964(14)
_cell_oxdiff_angle_beta          89.9931(13)
_cell_oxdiff_angle_gamma         90.0141(14)
_cell_oxdiff_volume              2637.85(8)
_cell_oxdiff_measurement_reflns_used 43845
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1