A Novel Trisamidophosphine Ligand and Its Group(IV) Metal Complexes
Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Organometallics 33 (2014) 612–; doi:10.1021/om401018f

data_4082454
_publ_section_title
;
 A Novel Trisamidophosphine Ligand and Its Group(IV) Metal Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              612
_journal_paper_doi               10.1021/om401018f
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C45 H45 Cl N3 P Zr, 2(C7 H8)'
_chemical_formula_sum            'C62.5 H65 Cl N3 P Zr'
_chemical_formula_weight         1015.81
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_ms1
_audit_creation_date
;
'Tue Dec 18 11:32:33 2012'
;
_audit_update_record             'Wed Oct  2 16:04:24 CEST 2013'
_cell_angle_alpha                69.1157(12)
_cell_angle_beta                 80.0360(12)
_cell_angle_gamma                80.8870(12)
_cell_formula_units_Z            2
_cell_length_a                   10.53327(16)
_cell_length_b                   15.8299(2)
_cell_length_c                   16.9562(2)
_cell_measurement_reflns_used    53571
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      71.7130
_cell_measurement_theta_min      4.7120
_cell_volume                     2587.29(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.9850
_diffrn_measured_fraction_theta_max 0.9699
_diffrn_measurement_details
;
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  2 omega  -54.00   20.00   1.0000    1.0000
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  3 omega  -18.00   47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega    6.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega    3.00   28.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   78.0000  116.7839 25

  6 omega  -47.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -34.0000  -66.0000  -44.8578 36

  7 omega    8.00   37.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000    5.0591 29

  8 omega    6.00   31.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000 -157.6986 25

  9 omega   11.00   36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   79.0000   -9.7542 25

 10 omega  -64.00   24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   64.0000  -90.0000 88

 11 omega  -42.00  -13.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 29

 12 omega  -43.00  -14.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 29

 13 omega -113.00  -78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000 -150.0000 35

 14 omega -112.00  -86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 26

 15 omega  -45.00  -19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
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 16 omega   15.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  -38.7402 25

 17 omega   15.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000   40.7454 25

 18 omega   19.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  130.3797 26

 19 omega   15.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  108.5665 25

 20 omega   15.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   79.0000  162.3759 25

 21 omega   19.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   77.0000  -60.4210 26

 22 omega   14.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -90.6943 25

 23 omega   20.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -138.3841 28

 24 omega   19.00   44.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -124.4071 25

 25 omega   20.00   45.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -18.5970 25

 26 omega   22.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  148.9451 26

 27 omega   26.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.3879 26

 28 omega   27.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   75.0000 -101.4268 42

 29 omega   23.00   48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   59.6688 25

 30 omega   88.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -163.4270 27

 31 omega   25.00   51.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -163.4270 26

 32 omega   26.00   52.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   76.0000   33.5306 26

 33 omega   29.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000   -2.7375 26

 34 omega   32.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   90.1250 26

 35 omega   29.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -132.9580 30

 36 omega   29.00   57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -64.2233 28

 37 omega   29.00   55.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  156.3327 26

 38 omega   30.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   75.0000  179.6043 26

 39 omega   36.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000  163.1529 28

 40 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   76.0000   55.3833 26

 41 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000   -2.9300 26

 42 omega   37.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000   47.6118 26

 43 omega   65.00   96.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   89.6231 31

 44 omega   43.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000    0.0876 26

 45 omega   43.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
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 46 omega   78.00  110.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
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 47 omega   39.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000 -102.2575 34

 48 omega   40.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000 -130.0579 26

 49 omega    2.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   35.5159 95

 50 omega  107.00  132.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   49.0000  -18.2221 25

 51 omega   54.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   49.0000  -18.2221 50

 52 omega   37.00   68.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000   98.9454 31

 53 omega   48.00   73.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   66.0000   32.5726 25

 54 omega   49.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   53.0000 -175.2818 31

 55 omega   40.00   67.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   48.5136 27

 56 omega   48.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   62.0000  -60.0729 29

 57 omega   55.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   61.0000 -124.0208 25

 58 omega   40.00  138.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  113.8869 98

 59 omega   57.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  170.7351 25

 60 omega   54.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000  -64.3919 87

 61 omega   13.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  170.7351 26

 62 omega   50.00  132.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   41.0000   14.2333 82

 63 omega   53.00   79.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   58.0000 -144.5583 26

 64 omega   64.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000   45.5504 27

 65 omega   57.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   50.0000    8.8580 26

 66 omega    8.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000  -72.1544 101

 67 omega   59.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  -76.8833 35

 68 omega   55.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   64.0000  171.5959 26

 69 omega   57.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   56.0000  109.7825 32

 70 omega   60.00   97.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   62.0000   74.3327 37

 71 omega   64.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   58.0000 -179.1253 80

 72 omega   60.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   62.0000   -6.9027 26

 73 omega   57.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000 -168.0591 26

 74 omega   63.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   72.0000  -18.2557 28

 75 omega   63.00  159.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   72.0000 -135.9158 96

 76 omega   69.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   49.0000  120.2965 33

 77 omega   69.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   52.0000   39.1610 50

 78 omega   73.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   61.0000 -134.8559 26

 79 omega   68.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   70.0000   23.6378 26

 80 omega   75.00  169.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   47.0000  127.1584 94

 81 omega   87.00  136.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000   30.0000 49

 82 omega   85.00  133.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000    0.0000 48

 83 omega   88.00  159.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -30.0000 71

 84 omega   59.00  141.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  172.7581 82

 85 omega   98.00  125.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000   60.0000 27

 86 omega   88.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   30.0000 89

 87 omega  149.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 27

 88 omega   69.00  142.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000    6.7379 73

 89 omega   89.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -180.0000 25

 90 omega   40.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000    6.7379 26

 91 omega   85.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  -60.0000 30

 92 omega   89.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  120.0000 28

 93 omega   88.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -60.0000 26

 94 omega   88.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000 -120.0000 28

 95 omega   88.00  139.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -77.0000   60.0000 51

 96 omega   81.00  107.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 26

 97 omega   85.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -150.0000 91

 98 omega   88.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  150.0000 90

 99 omega   88.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -90.0000 27

100 omega   81.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   60.0000 27

101 omega   85.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000  150.0000 65

102 omega  152.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 26

103 omega   81.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -150.0000 27

104 omega   88.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000   60.0000 26

105 omega  139.00  165.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

106 omega  133.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000    0.0000 39

107 omega   80.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -60.0000 26

108 omega  146.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 26

109 omega   81.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -180.0000 25

110 omega  139.00  165.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

111 omega   80.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000 -120.0000 26

112 omega  111.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 66

113 omega   80.00  105.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -90.0000 25

114 omega   80.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  150.0000 26

115 omega   81.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  -30.0000 27

116 omega   88.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   64.0000  -30.0000 90

117 omega   80.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   90.0000 97

118 omega  101.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000 -120.0000 27

119 omega   60.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  113.0770 80

120 omega  153.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 25

121 omega   82.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000   30.0000 26

122 omega   94.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   50.0000  -90.0000 27

123 omega  134.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 38

124 omega   81.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   77.0000  120.0000 27

125 omega   89.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   38.0000 -120.0000 88

126 omega   84.00  171.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   70.0000   64.1152 87

127 omega   55.00  142.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000  -46.0481 87

128 omega   87.00  113.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342   42.0000  -40.4444 26

129 omega   69.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -126.2416 43

130 omega   66.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.2342  -80.0000 -112.9948 27

131 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   30.0000 90

132 omega  -26.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   60.0000 98

133 omega  -73.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000 -120.0000 117

134 omega  -69.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 90

135 omega    3.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   66.0000  -22.7257 91

136 omega    6.00   46.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   80.0000    5.0591 40

137 omega  -50.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  150.0000 80

138 omega  -63.00   26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   57.0000    0.0000 89

139 omega   15.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000  108.5665 34

140 omega   19.00   47.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000 -124.4071 28

141 omega   19.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000  -18.5970 30

142 omega   29.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000 -132.9580 99

143 omega   -9.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -86.8318 102

144 omega   -9.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -38.8862 102

145 omega   36.00  131.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000  -91.4691 95

146 omega   -5.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000  -80.0000   89.6231 25

147 omega   36.00  136.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000 -130.0579 100

148 omega   40.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  113.8869 100

149 omega   40.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   48.5136 100

150 omega    3.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -80.0000  170.7351 103

151 omega    3.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000  -79.0000   45.5504 102

152 omega   50.00  142.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   68.0000  -64.3919 92

153 omega   57.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   56.0000  109.7825 90

154 omega   57.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000  -76.8833 90

155 omega   61.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   58.0000 -179.1253 90

156 omega   60.00  150.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   62.0000   -6.9027 90

157 omega   60.00  150.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   62.0000   74.3327 90

;
_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      -0.0650476000
_diffrn_orient_matrix_UB_12      -0.0140228000
_diffrn_orient_matrix_UB_13      0.0917768000
_diffrn_orient_matrix_UB_21      -0.0430251000
_diffrn_orient_matrix_UB_22      -0.0905882000
_diffrn_orient_matrix_UB_23      0.0050864000
_diffrn_orient_matrix_UB_31      0.1273385000
_diffrn_orient_matrix_UB_32      -0.0506784000
_diffrn_orient_matrix_UB_33      0.0340745000
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            85054
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.107
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.2205
_exptl_crystal_size_mid          0.1110
_exptl_crystal_size_min          0.0644
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         9867
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0314P)^2^+1.5028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9413
_reflns_number_total             9867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401018f_si_001.cif
_cod_data_source_block           ba_ms1_sq
_cod_original_cell_volume        2587.28(7)
_cod_original_formula_sum        'C62.50 H65 Cl N3 P Zr'
_cod_database_code               4082454
_audit_block_refno               1669
_audit_block_usercomment         'MSSB25, irregular, yellow'
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C62.5 H65 Cl1 N3 P1 Zr1'
_chemical_oxdiff_usercomment     'MSSB25, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.765
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained planarity
 C81A, C82A, C83A, C84A, C85A, C86A, C87A
 with sigma of 0.1
 C81B, C82B, C83B, C84B, C85B, C86B, C87B
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C81A \\sim C81B: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
C82A \\sim C82B: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
C83A \\sim C83B: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
C84A \\sim C84B: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
C85A \\sim C85B: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
C86A \\sim C86B: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
C87A \\sim C87B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
4. Same fragment restrains
{C81A, C82A, C83A, C84A, C85A, C86A, C87A}
as
{C81B, C82B, C83B, C84B, C85B, C86B, C87B}
5. Others
 Sof(C81B)=Sof(C82B)=Sof(H82B)=Sof(C83B)=Sof(H83B)=Sof(C84B)=Sof(H84B)=
 Sof(C85B)=Sof(H85B)=Sof(C86B)=Sof(H86B)=Sof(C87B)=Sof(H87D)=Sof(H87E)=
 Sof(H87F)=1-FVAR(1)
 Sof(C81A)=Sof(C82A)=Sof(H82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=Sof(H84A)=
 Sof(C85A)=Sof(H85A)=Sof(C86A)=Sof(H86A)=Sof(C87A)=Sof(H87A)=Sof(H87B)=
 Sof(H87C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B), C37(H37A,H37B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), C39(H39), C41(H41), C43(H43), C82A(H82A), C83A(H83A),
 C84A(H84A), C85A(H85A), C86A(H86A), C82B(H82B), C83B(H83B), C84B(H84B),
 C85B(H85B), C86B(H86B), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C87A(H87A,H87B,H87C),
 C87B(H87D,H87E,H87F), C97(H97A,H97B,H97C)
;
_shelx_res_checksum              52845
_cell_oxdiff_length_a            10.53327(15)
_cell_oxdiff_length_b            15.8299(2)
_cell_oxdiff_length_c            16.9562(2)
_cell_oxdiff_angle_alpha         69.1157(12)
_cell_oxdiff_angle_beta          80.0360(12)
_cell_oxdiff_angle_gamma         80.8870(12)
_cell_oxdiff_volume              2587.28(6)
_cell_oxdiff_measurement_reflns_used 53571