Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by Carbazolide-Based PNP Pincer Ligands.
Plundrich, Gudrun T.; Wadepohl, Hubert; Gade, Lutz H.; Inorganic chemistry 55 (2015) 353–; doi:10.1021/acs.inorgchem.5b02498

data_4344786
_publ_section_title
;
 Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by
 Carbazolide-Based PNP Pincer Ligands.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              353
_journal_paper_doi               10.1021/acs.inorgchem.5b02498
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C34 H55 N P2'
_chemical_formula_sum            'C34 H55 N P2'
_chemical_formula_weight         539.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_gp34
_audit_creation_date
;
'Fri May 08 05:50:47 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'08.05.2015 10:14:05 CEST UTC+02:00  encif 1.31'
_cell_angle_alpha                90
_cell_angle_beta                 93.6930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2228(3)
_cell_length_b                   12.44798(16)
_cell_length_c                   11.01843(11)
_cell_measurement_reflns_used    24108
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.3760
_cell_measurement_theta_min      5.5710
_cell_volume                     3315.43(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_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 0.993
_diffrn_measurement_details
;
  1 omega  -68.00  -17.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   90.0000 51

  2 omega  -16.00   62.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -90.0000 78

  3 omega  -12.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000   90.0000 38

  4 omega  -67.00  -12.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 55

  5 omega  -11.00   78.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   68.0000  127.7755 89

  6 omega   -6.00   19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000  -79.6640 25

  7 omega    7.00   32.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000   64.9347 25

  8 omega    7.00   32.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -84.2979 25

  9 omega   12.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   77.0000  106.1856 27

 10 omega   11.00   36.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000    5.9176 25

 11 omega   11.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000 -161.1325 32

 12 omega   15.00   40.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  138.3616 25

 13 omega   14.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   10.7860 25

 14 omega   14.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -64.8533 25

 15 omega   21.00   50.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   75.0000 -171.5151 29

 16 omega   20.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -114.3595 27

 17 omega   30.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 27

 18 omega   99.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -127.3320 25

 19 omega   25.00   50.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 25

 20 omega   25.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 30

 21 omega   24.00   51.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 27

 22 omega   27.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 27

 23 omega   29.00   83.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000 -120.0000 54

 24 omega   23.00   48.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -29.4367 25

 25 omega   24.00   50.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -127.3320 26

 26 omega  -16.00   84.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000    0.0000 100

 27 omega   25.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 27

 28 omega   26.00   53.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 27

 29 omega   97.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   13.4474 27

 30 omega   69.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -103.9720 58

 31 omega   30.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -103.9720 27

 32 omega   29.00   58.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   13.4474 29

 33 omega   43.00   70.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000   18.9578 27

 34 omega   34.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  121.3547 27

 35 omega  102.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -76.4662 26

 36 omega   31.00   58.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  167.5346 27

 37 omega   30.00   55.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -76.4662 25

 38 omega   29.00   56.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  103.9713 27

 39 omega   44.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  154.8733 27

 40 omega   38.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -109.6565 30

 41 omega   37.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000   67.0913 60

 42 omega   36.00   92.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000   59.5309 56

 43 omega   -4.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  172.6305 102

 44 omega   38.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000  -33.6855 98

 45 omega   46.00   73.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   65.0000   31.6045 27

 46 omega   39.00   64.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000 -170.9094 25

 47 omega   39.00   64.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000  -67.3624 25

 48 omega   41.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000  107.1284 27

 49 omega   42.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -141.8609 26

 50 omega   45.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000   53.5004 27

 51 omega   54.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   69.0000   34.3882 25

 52 omega   47.00  114.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000  135.3036 67

 53 omega   47.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000   82.2182 29

 54 omega   48.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000   24.4437 27

 55 omega   44.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000 -101.2904 27

 56 omega   56.00   82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   -0.2984 26

 57 omega   61.00  104.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   86.2804 43

 58 omega   66.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000  -52.9843 25

 59 omega   50.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000 -150.8536 92

 60 omega   49.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   37.9828 30

 61 omega   49.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -46.0064 26

 62 omega   55.00  129.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   74.0000   94.1296 74

 63 omega   59.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   48.0000  174.5267 33

 64 omega   54.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   75.0000 -177.6769 25

 65 omega   58.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   68.0000   -3.2474 34

 66 omega   55.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   51.0793 31

 67 omega   67.00  129.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   72.0000   50.6171 62

 68 omega   66.00  131.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   54.0000   30.1546 65

 69 omega   61.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   72.0000  -99.1627 25

 70 omega   65.00   97.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   70.0000  166.1486 32

 71 omega   70.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   58.0000  -81.1071 25

 72 omega   65.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   76.0000  147.6254 26

 73 omega   72.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   71.0000 -140.6672 33

 74 omega   73.00  125.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   70.0000  169.7465 52

 75 omega  138.00  165.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000   78.2662 27

 76 omega   80.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000   78.2662 25

 77 omega   68.00   95.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 27

 78 omega   37.00  102.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  167.8579 65

 79 omega   37.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -84.9175 67

 80 omega   90.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   30.0000 86

 81 omega   87.00  143.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -90.0000 56

 82 omega   88.00  173.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -180.0000 85

 83 omega   38.00  134.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -139.8144 96

 84 omega   87.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000 -120.0000 25

 85 omega  138.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 39

 86 omega   79.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 27

 87 omega   83.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 95

 88 omega   65.00  122.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000  -40.3674 57

 89 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 25

 90 omega   68.00  102.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  119.1927 34

 91 omega   86.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000    0.0000 35

 92 omega   67.00  101.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   60.0000 34

 93 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 25

 94 omega  113.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 65

 95 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 27

 96 omega   79.00  168.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 89

 97 omega  136.00  169.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 33

 98 omega   87.00  112.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -60.0000 25

 99 omega  120.00  171.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 51

100 omega   78.00  116.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 38

101 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

102 omega   82.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 33

103 omega   73.00  138.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -79.0000    9.8147 65

104 omega   86.00  147.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  150.0000 61

105 omega  108.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 70

106 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 27

107 omega  153.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 25

108 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

109 omega  148.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 29

110 omega   78.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 27

111 omega   86.00  175.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000   60.0000 89

112 omega   89.00  120.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 31

113 omega   95.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -30.0000 82

114 omega   81.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   10.9813 77

115 omega  -26.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000 -180.0000 98

116 phi      0.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000  -20.0000     -     120

117 omega  -11.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       14.0000   69.0000 -105.5292 93

118 omega  -11.00   88.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   76.0000  -27.1809 99

119 omega    2.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   67.0000    3.1968 92

120 omega   -6.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   80.0000  -79.6640 52

121 omega   -3.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   75.0000   37.2203 99

122 omega    4.00  104.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   77.0000  130.8116 100

123 omega    7.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000  -84.2979 40

124 omega   14.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -64.8533 32

125 omega   14.00   46.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000   10.7860 32

126 omega   24.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 100

127 omega   24.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 100

128 omega  -19.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000    0.0000    0.0000 146

129 omega   24.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 100

130 omega  -17.00   86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -80.0000  139.1827 103

131 omega   23.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -29.4367 26

132 omega  -15.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 90

133 omega  -15.00   75.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -120.0000 90

134 omega   29.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000   13.4474 99

135 omega   29.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  167.5346 99

136 omega   29.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  -76.4662 99

137 omega   28.00  128.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  103.9713 100

138 omega   34.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000 -109.6565 97

139 omega   33.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  154.8733 99

140 omega   36.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000   67.0913 95

141 omega   -9.00   94.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -80.0000   59.5309 103

142 omega   38.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000 -170.9094 98

143 omega   38.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000  -67.3624 98

144 omega   -5.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000  172.6305 103

145 omega   38.00  136.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000  -33.6855 98

146 omega   46.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000  135.3036 92

147 omega   41.00  140.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000   53.5004 99

148 omega   42.00  139.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   73.0000 -141.8609 97

149 omega   49.00  138.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   60.0000  121.8217 89

150 omega   46.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   73.0000   82.2182 97

151 omega   53.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   55.0000  125.0626 90

152 omega   44.00  144.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000 -101.2904 100

153 omega   47.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   72.0000   24.4437 96

154 omega   53.00  143.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000 -120.1656 90

155 omega    8.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -78.0000  -52.9843 101

156 omega   56.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   86.2804 90

157 omega   56.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   63.0000   -0.2984 90

158 omega   49.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000 -150.8536 99

159 omega   48.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   77.0000   37.9828 100

160 omega   49.00  148.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   75.0000  -46.0064 99

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0632883000
_diffrn_orient_matrix_UB_12      -0.0146273000
_diffrn_orient_matrix_UB_13      -0.0068877000
_diffrn_orient_matrix_UB_21      -0.0030851000
_diffrn_orient_matrix_UB_22      0.0358376000
_diffrn_orient_matrix_UB_23      -0.1340473000
_diffrn_orient_matrix_UB_31      0.0069990000
_diffrn_orient_matrix_UB_32      -0.1175572000
_diffrn_orient_matrix_UB_33      -0.0400046000
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            63368
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.846
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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    1.081
_exptl_crystal_description       needle
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0395P)^2^+3.1374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2962
_reflns_number_total             3177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02498_si_002.cif
_cod_data_source_block           ga_gp34
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4344786
_audit_block_refno               2435
_audit_block_usercomment         'gp916, needle, colourless'
_chemical_oxdiff_formula         'C34 H55 N P2'
_chemical_oxdiff_usercomment     'gp916, needle, colourless'
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.878
_reflns_odcompleteness_completeness 100.00
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group with stretchable bonds:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C), C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              42220
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            24.2156(5)
_cell_oxdiff_length_b            12.4473(2)
_cell_oxdiff_length_c            11.02185(18)
_cell_oxdiff_angle_alpha         90.0018(15)
_cell_oxdiff_angle_beta          93.6577(15)
_cell_oxdiff_angle_gamma         89.9441(16)
_cell_oxdiff_volume              3315.43(11)
_cell_oxdiff_measurement_reflns_used 24123