Closely Related Benzylene-Linked Diamidophosphine Scaffolds and Their Zirconium and Hafnium Complexes: How Small Changes of the Ligand Result in Different Complex Stabilities and Reactivities
Batke, Sonja; Sietzen, Malte; Merz, Lukas; Wadepohl, Hubert; Ballmann, Joachim; Organometallics 35 (2016) 2294–; doi:10.1021/acs.organomet.6b00384

data_4086562
_publ_section_title
;
 Closely Related Benzylene-Linked Diamidophosphine Scaffolds and Their
 Zirconium and Hafnium Complexes: How Small Changes of the Ligand Result
 in Different Complex Stabilities and Reactivities
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2294
_journal_paper_doi               10.1021/acs.organomet.6b00384
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C40 H49 N2 P Si2 Zr'
_chemical_formula_sum            'C40 H49 N2 P Si2 Zr'
_chemical_formula_weight         736.18
_chemical_properties_physical    'air-sensitive, moisture-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_sb37
_audit_creation_date
;
'Tue Oct 13 11:56:42 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
'13.10.2015 11:58:41 CEST UTC+02:00  encif 1.35'
_cell_angle_alpha                73.997(2)
_cell_angle_beta                 89.0580(18)
_cell_angle_gamma                74.023(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3850(2)
_cell_length_b                   10.8151(3)
_cell_length_c                   18.4097(5)
_cell_measurement_reflns_used    15450
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.1650
_cell_measurement_theta_min      4.4280
_cell_volume                     1906.82(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -29.00   -3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -90.0000 26

  2 omega  -23.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -150.0000 37

  3 omega  -62.00  -28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -150.0000 34

  4 omega   32.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 32

  5 omega  -15.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 27

  6 omega  -15.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 80

  7 omega    4.00   68.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -90.0000 64

  8 omega  -20.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000   91.0000  141.2349 49

  9 omega  -12.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.0000  105.0000  179.3620 27

 10 omega    7.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   79.0000 -122.9823 25

 11 omega    6.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   88.0000   98.0174 25

 12 omega    9.00   34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   83.0000   15.5226 25

 13 omega    5.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   89.0000  -60.0433 25

 14 omega    5.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   89.0000   50.4440 25

 15 omega   12.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   84.0000 -165.0883 25

 16 omega   15.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   81.0000  -20.0794 29

 17 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000   -5.5885 25

 18 omega   17.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   82.0000  161.2225 28

 19 omega   18.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   81.0000  148.6779 25

 20 omega   19.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000   23.9711 25

 21 omega   18.00   43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000 -109.6920 25

 22 omega   29.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 27

 23 omega   25.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 25

 24 omega   27.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   62.1537 27

 25 omega   25.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 25

 26 omega   25.00   52.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 27

 27 omega   99.00  124.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   62.1537 25

 28 omega   25.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 25

 29 omega   25.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 25

 30 omega  -15.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000    0.0000 99

 31 omega   24.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 48

 32 omega   28.00   55.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 27

 33 omega   29.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 25

 34 omega    2.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000 -120.0000 89

 35 omega   23.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   43.1769 25

 36 omega   28.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000 -159.3356 41

 37 omega   30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000    0.1857 27

 38 omega   33.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -55.6464 27

 39 omega   31.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000   -7.9824 25

 40 omega   99.00  124.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  -55.6464 25

 41 omega   30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   76.0000  178.7502 27

 42 omega   36.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   64.0000  102.5950 43

 43 omega   84.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   73.0000    0.1857 27

 44 omega   34.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000   -3.7515 27

 45 omega   45.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  158.1163 27

 46 omega   46.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   65.0000   49.6061 81

 47 omega   33.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  115.1069 35

 48 omega   33.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   75.0000  152.3248 35

 49 omega   36.00  125.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   70.0000 -109.3963 89

 50 omega   39.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   71.0000  -86.7368 27

 51 omega   47.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000   20.0446 32

 52 omega   49.00  138.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   54.0000  -76.4879 89

 53 omega   85.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  115.7383 26

 54 omega   45.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  115.7383 32

 55 omega   84.00  115.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   68.0000   20.0446 31

 56 omega   44.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   61.2512 31

 57 omega   58.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   50.0000   13.0131 27

 58 omega   45.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  143.4442 63

 59 omega   45.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  -37.0377 30

 60 omega   51.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  115.8507 45

 61 omega   59.00   84.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000 -173.5589 25

 62 omega   56.00   86.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   49.0000  -48.5366 30

 63 omega   54.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   73.0000 -178.8610 56

 64 omega   74.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   53.0000   72.4257 25

 65 omega   58.00   85.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   71.0000  -47.7224 27

 66 omega   52.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   77.0000   27.7528 52

 67 omega   58.00  150.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   76.0000  -56.7894 92

 68 omega   56.00  155.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000   77.4499 99

 69 omega   70.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   59.0000  170.4495 26

 70 omega   70.00  142.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   59.0000   54.6198 72

 71 omega   61.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   76.0000  128.0675 30

 72 omega   62.00  118.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.0000 -167.4439 56

 73 omega   69.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   73.0000 -170.4955 94

 74 omega   71.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   71.0000  -11.0197 35

 75 omega   37.00   79.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 42

 76 omega   86.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   30.0000 88

 77 omega   39.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -30.0000 64

 78 omega   38.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  120.0000 36

 79 omega   80.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 27

 80 omega  136.00  162.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 26

 81 omega   85.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 35

 82 omega   83.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -30.0000 64

 83 omega   85.00  112.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -60.0000 27

 84 omega  115.00  140.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000  -90.0000 25

 85 omega   37.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000  -90.0000 55

 86 omega   86.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 49

 87 omega   37.00   75.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 38

 88 omega   78.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 27

 89 omega   87.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   56.0000  102.7772 30

 90 omega   85.00  129.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 44

 91 omega   86.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 89

 92 omega   87.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 27

 93 omega   86.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -180.0000 89

 94 omega   85.00  162.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 77

 95 omega   82.00  156.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  -90.0000 74

 96 omega   78.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 27

 97 omega   78.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 26

 98 omega   86.00  174.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 88

 99 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 25

100 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 25

101 omega  137.00  163.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   60.0000 26

102 omega   83.00  151.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 68

103 omega   63.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000   60.0000 72

104 omega   85.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 26

105 omega   79.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

106 omega   78.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 27

107 omega   37.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 78

108 omega   78.00  105.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 27

109 omega   87.00  118.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  120.0000 31

110 omega   85.00  145.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 60

111 omega   86.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 89

112 omega   97.00  140.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -30.0000 43

113 omega   78.00  169.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 91

114 omega   37.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 70

115 omega   80.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 27

116 omega   78.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 26

117 omega  109.00  162.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 53

118 omega  -26.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000   30.0000 98

119 omega  -30.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  150.0000 100

120 phi      0.00  120.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000   20.0000     -     120

121 omega  -21.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 90

122 omega  -13.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000   66.0000  -35.6390 91

123 omega  -21.00   12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000  108.0000   90.8392 33

124 omega    2.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   67.0000   20.1700 92

125 omega   23.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -150.0000 88

126 omega  -15.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -120.0000 90

127 omega  -18.00   80.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   30.0000 98

128 omega   52.00  144.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   50.0000   13.0131 92

129 omega   45.00  144.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   75.0000  143.4442 99

130 omega   45.00  144.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  -37.0377 99

131 omega   44.00  123.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   61.2512 79

132 omega   57.00  147.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   54.0000 -173.5589 90

133 omega   50.00  148.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000  115.8507 98

;
_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      -0.0200862000
_diffrn_orient_matrix_UB_12      0.0019662000
_diffrn_orient_matrix_UB_13      -0.0830791000
_diffrn_orient_matrix_UB_21      -0.1530860000
_diffrn_orient_matrix_UB_22      0.0516468000
_diffrn_orient_matrix_UB_23      0.0037912000
_diffrn_orient_matrix_UB_31      0.0083799000
_diffrn_orient_matrix_UB_32      0.1455367000
_diffrn_orient_matrix_UB_33      -0.0263381000
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.864
_diffrn_reflns_theta_min         4.433
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.282
_exptl_crystal_description       irregular
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0326
_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^+1.1689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6064
_reflns_number_total             7252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00384_si_002.cif
_cod_data_source_block           ba_sb37
_cod_depositor_comments
'Adding full bibliography for 4086549--4086572.cif.'
_cod_original_cell_volume        1906.82(8)
_cod_database_code               4086562
_audit_block_refno               2550
_audit_block_usercomment         'sb390, irregular, colourless'
_chemical_oxdiff_formula         'C40 H49 N2 P Si2 Zr'
_chemical_oxdiff_usercomment     'sb390, irregular, colourless'
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.716
_reflns_odcompleteness_completeness 99.97
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B), C33(H33A,H33B), C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              72572
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            10.3850(2)
_cell_oxdiff_length_b            10.8151(3)
_cell_oxdiff_length_c            18.4097(4)
_cell_oxdiff_angle_alpha         73.997(2)
_cell_oxdiff_angle_beta          89.0580(18)
_cell_oxdiff_angle_gamma         74.023(2)
_cell_oxdiff_volume              1906.82(8)
_cell_oxdiff_measurement_reflns_used 15450