Paramagnetic NMR Analysis of Substituted Biscyclooctatetraene Lanthanide Complexes
Hiller, Markus; Maier, Martin; Wadepohl, Hubert; Enders, Markus; Organometallics 35 (2016) 1916–; doi:10.1021/acs.organomet.6b00241

data_4086500
_publ_section_title
;
 Paramagnetic NMR Analysis of Substituted Biscyclooctatetraene Lanthanide
 Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1916
_journal_paper_doi               10.1021/acs.organomet.6b00241
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C40 H58 Li O3 Tb'
_chemical_formula_sum            'C40 H58 Li O3 Tb'
_chemical_formula_weight         752.72
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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                en_mh2
_audit_creation_date
;
'Mon Aug 10 15:57:44 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
'19.08.2015 16:36:38 CEST UTC+02:00  encif 1.32'
_cell_angle_alpha                90
_cell_angle_beta                 94.7190(8)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.93306(18)
_cell_length_b                   11.24577(8)
_cell_length_c                   62.0951(5)
_cell_measurement_reflns_used    69950
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      69.7980
_cell_measurement_theta_min      4.4470
_cell_volume                     13872.2(2)
_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, 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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -18.00   18.00   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.5079  -57.0000  120.0000 48

  2 omega  -76.00  -29.50   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.5079  -57.0000  120.0000 62

  3 omega  -38.00   57.25   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.5079   77.0000 -180.0000 127

  4 omega  -42.00   17.25   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.5079   77.0000  -30.0000 79

  5 phi    165.00  236.25   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
   2.5079    2.5079  -40.0000     -     95

  6 phi    120.00  162.00   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
   2.5079    2.5079  -40.0000     -     56

  7 omega   -9.00   30.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       32.0000   79.0000  -31.2727 52

  8 omega   -2.00   37.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0000   80.0000  169.9188 52

  9 omega    1.00   36.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000   80.0000 -109.0048 47

 10 omega    2.00   30.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0000   80.0000   72.8774 38

 11 omega    7.00   42.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0000   80.0000    3.7359 47

 12 omega  -46.00  -19.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.8793  -77.0000   60.0000 35

 13 omega -137.00  -50.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.8793  -77.0000   60.0000 115

 14 omega  -54.00   18.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.8793   45.0000   60.0000 96

 15 omega  -64.00  -20.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.8793  -77.0000    0.0000 58

 16 omega   21.00   47.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000 -150.0000 35

 17 omega   55.00   81.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000  120.0000 35

 18 omega   35.00   97.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793  -80.0000  176.5409 83

 19 omega   63.00   95.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793  -80.0000  109.0076 43

 20 omega   77.00  136.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000   60.0000 79

 21 omega   50.00   76.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793  -77.0000  -60.0000 35

 22 omega   19.00  114.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000  -60.0000 127

 23 omega  -23.00   52.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793  -80.0000  109.0076 100

 24 omega   21.00   47.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000  120.0000 35

 25 omega   30.00   56.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000   60.0000 35

 26 omega   18.00   44.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000  150.0000 35

 27 omega   18.00   52.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000 -180.0000 46

 28 omega   72.00  121.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793   77.0000 -150.0000 66

 29 omega   18.00   43.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   80.0000 -124.1252 34

 30 omega   19.00   44.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   79.0000   93.4721 34

 31 omega   18.00   43.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   80.0000 -108.7866 34

 32 omega   25.00   61.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000  147.6670 48

 33 omega   83.00  109.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000 -110.5901 35

 34 omega   31.00   56.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       64.0000   77.0000 -110.5901 34

 35 omega  -13.00  110.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000  -80.0000   81.7957 164

 36 omega   98.00  138.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   92.5497 54

 37 omega   33.00  126.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  163.1165 124

 38 omega   29.00   55.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   75.0000  -36.4475 35

 39 omega   28.00  105.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  -95.6193 103

 40 omega   28.00   54.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000   92.5497 35

 41 omega   36.00   70.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   76.0000  112.3114 46

 42 omega   -9.00  114.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000  -80.0000 -112.5458 164

 43 omega   90.00  116.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   64.0000   28.5711 35

 44 omega   39.00   65.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   64.0000   28.5711 35

 45 omega   39.00   87.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   58.0000 -128.2911 64

 46 omega   32.00   58.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   77.0000   45.9952 35

 47 omega   47.00   81.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000  -79.0000  -10.9490 46

 48 omega   40.00  132.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   63.0000  -42.8589 123

 49 omega   38.00   71.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   76.0000  141.9232 44

 50 omega   47.00   73.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000  -79.0000  -52.5132 35

 51 omega    7.00   33.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000  -79.0000  -52.5132 35

 52 omega   45.00   75.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   55.0000   39.5244 40

 53 omega   47.00   73.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   51.0000  179.5580 35

 54 omega   55.00   81.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   59.0000   85.2588 35

 55 omega   41.00   67.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   71.0000  -50.9591 35

 56 omega   72.00   98.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000  -80.0000 -161.9486 35

 57 omega   46.00  116.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   46.0000  141.9088 94

 58 omega   44.00  102.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   77.0000  -33.7439 78

 59 omega   51.00   76.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   65.0000   33.1944 34

 60 omega   51.00   85.50   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   53.0000  -76.5921 46

 61 omega   53.00  110.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   69.0000 -132.7154 76

 62 omega   50.00   76.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       88.0000   77.0000   36.5184 35

 63 omega   56.00  166.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       92.0000   70.0000  131.0160 147

 64 omega   61.00   87.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   51.0000 -165.0549 35

 65 omega   62.00  118.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   66.0000   31.0174 75

 66 omega   62.00  167.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   52.0000  -32.8838 140

 67 omega   62.00  171.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   68.0000  -87.6367 146

 68 omega   59.00   85.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -       96.0000   71.0000 -179.9940 35

 69 omega   61.00   88.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   76.0000  176.5321 36

 70 omega   68.00   94.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   59.0000  -63.7742 35

 71 omega  142.00  168.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   73.0000  -21.3748 35

 72 omega   62.00  108.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   73.0000  -21.3748 62

 73 omega   66.00   92.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      104.0000  -80.0000   -1.8670 35

 74 omega  106.00  157.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   81.9170 68

 75 omega   70.00   97.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   81.9170 36

 76 omega   34.00  153.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000   46.8927 159

 77 omega   74.00  121.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000  -67.0775 63

 78 omega   33.00   58.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000  -67.0775 34

 79 omega   80.00  177.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000 -126.2549 130

 80 omega   80.00  176.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000  120.0000 128

 81 omega   81.00  177.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000  -30.0000 128

 82 omega   72.00   98.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -79.0000  126.5245 35

 83 omega   34.00   61.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -79.0000  126.5245 36

 84 omega   73.00  122.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   43.0000 -180.0000 66

 85 omega   73.00   98.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000  150.0000 34

 86 omega   75.00  101.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000   60.0000 35

 87 omega   80.00  106.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000   30.0000 35

 88 omega  150.00  176.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000 -150.0000 35

 89 omega   80.00  144.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000 -150.0000 86

 90 omega   60.00   92.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000  178.6240 43

 91 omega   58.00   84.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -43.0000  -60.0000 35

 92 omega   39.00  154.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000 -146.0904 154

 93 omega   80.00  176.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000  -90.0000 128

 94 omega  110.50  178.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000    0.0000 90

 95 omega   73.00  100.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000    0.0000 36

 96 omega   73.00   99.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000 -180.0000 35

 97 omega   74.00  100.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000  -30.0000 35

 98 omega   73.00   98.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000 -120.0000 34

 99 omega   80.00  106.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000  150.0000 35

100 omega   73.00  177.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000   30.0000 139

101 omega   73.00   98.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000 -150.0000 34

102 omega  120.00  146.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000  150.0000 35

103 omega   73.00  170.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000   90.0000 130

104 omega   75.00  127.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000  114.2923 70

105 omega   73.00  160.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000  -60.0000 116

106 omega   41.00   68.00   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000  114.2923 36

107 omega   74.00  111.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   43.0000   30.0000 50

108 omega   80.00  171.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000   60.0000 122

109 omega   73.00   99.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   77.0000  120.0000 35

110 omega   80.00  177.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   65.0000 -180.0000 130

111 omega  142.00  167.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   75.0000  -72.7934 34

112 omega   74.00  100.25   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   75.0000  -72.7934 35

113 omega   87.00  163.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507   63.0000  170.2095 102

114 omega   94.00  140.50   0.7500   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.2507  -80.0000  -42.0476 62

115 omega  -77.00   28.75   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.5079  -57.0000    0.0000 141

116 omega  -35.00   70.75   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       -2.5079   57.0000 -180.0000 141

117 omega  -72.00   33.75   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -        2.5079  -57.0000  -90.0000 141

118 omega  -20.00   97.75   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   77.0000   12.7434 157

119 omega  -20.00   97.75   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   77.0000  105.4236 157

120 omega  -13.00  101.00   0.7500    1.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0000   71.0000  -96.3840 152

121 omega  -48.00   21.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.8793   30.0000   30.0000 93

122 omega  -48.00   21.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -57.8793   30.0000 -150.0000 93

123 omega  -22.00   98.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793  -77.0000   60.0000 160

124 omega  -23.00   97.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       57.8793  -80.0000 -119.7538 161

125 omega   20.00   47.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   78.0000  138.0377 37

126 omega   18.00   45.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   80.0000 -124.1252 36

127 omega   19.00   46.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   79.0000   93.4721 36

128 omega   28.00   57.25   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  163.1165 39

129 omega   28.00  145.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       68.0000   77.0000  -95.6193 157

130 omega   30.00  150.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   42.0000 -159.9924 160

131 omega   39.00  144.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   58.0000    7.7359 141

132 omega   -8.00  112.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000  -79.0000  -10.9490 160

133 omega   36.00  147.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       72.0000   50.0000  -95.7693 148

134 omega   43.00  148.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   59.0000   85.2588 141

135 omega   39.00  153.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       76.0000   71.0000  -50.9591 152

136 omega   46.00  154.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   67.0000   52.4813 144

137 omega   41.00  155.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   46.0000  141.9088 153

138 omega    0.00  120.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000  -79.0000  144.3711 160

139 omega   50.00  158.00   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   53.0000  -76.5921 144

140 omega   44.00  161.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   77.0000  -33.7439 157

141 omega   51.00  156.75   0.7500    4.0000
omega____ theta____ kappa____ phi______ frames
    -       84.0000   65.0000   33.1944 141

;
_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      -0.0146625000
_diffrn_orient_matrix_UB_12      0.0225135000
_diffrn_orient_matrix_UB_13      -0.0244032000
_diffrn_orient_matrix_UB_21      -0.0330534000
_diffrn_orient_matrix_UB_22      -0.1235718000
_diffrn_orient_matrix_UB_23      -0.0026117000
_diffrn_orient_matrix_UB_31      -0.0686021000
_diffrn_orient_matrix_UB_32      0.0547098000
_diffrn_orient_matrix_UB_33      0.0041571000
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            167669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.056
_diffrn_reflns_theta_min         4.287
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.294
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.565
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             6240
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         13091
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+42.4518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12463
_reflns_number_total             13091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00241_si_002.cif
_cod_data_source_block           en_mh2
_cod_depositor_comments          'Adding full bibliography for 4086500.cif.'
_cod_original_cell_volume        13872.22(19)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4086500
_audit_block_refno               2499
_audit_block_usercomment         'mh_mm11, block, yellow'
_chemical_oxdiff_formula         'Li Tm C32 H40'
_chemical_oxdiff_usercomment     'mh_mm11, block, yellow'
_shelx_estimated_absorpt_t_max   0.462
_shelx_estimated_absorpt_t_min   0.271
_reflns_odcompleteness_completeness 99.87
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C10A \\sim C9-C10B
 with sigma of 0.005
 C10A-C11A \\sim C10B-C11B
 with sigma of 0.005
 C12-C11A \\sim C12-C11B
 with sigma of 0.005
 C29-C30A \\sim C29-C30B
 with sigma of 0.005
 C30A-C31A \\sim C30B-C31B
 with sigma of 0.005
 C32-C31A \\sim C32-C31B
 with sigma of 0.005
 C64-C65A \\sim C64-C65B
 with sigma of 0.005
 C65A-C66A \\sim C65B-C66B
 with sigma of 0.005
 C56-C66A \\sim C56-C66B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10A \\sim C11A \\sim C10B \\sim C11B \\sim C12 \\sim C13 \\sim C14 \\sim
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30A
\\sim C31A \\sim C30B \\sim C31B \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C51 \\sim C52 \\sim C53 \\sim
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim
C62 \\sim C63 \\sim C64 \\sim C65A \\sim C66A \\sim C65B \\sim C66B \\sim C67
\\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75
\\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83
\\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90: within
0.5A with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C9, C10A, C10B, C11A, C11B, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C30A, C30B, C31A, C31B, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C64, C65A, C65B, C66A, C66B, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H9BC)=Sof(H9BD)=Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=
 Sof(H11D)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31C)=
 Sof(H31D)=Sof(H32C)=Sof(H32D)=1-FVAR(2)
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(C31A)=Sof(H31A)=
 Sof(H31B)=Sof(H32A)=Sof(H32B)=FVAR(2)
 Sof(H64C)=Sof(H64D)=Sof(C65B)=Sof(H65C)=Sof(H65D)=Sof(C66B)=Sof(H66C)=
 Sof(H66D)=1-FVAR(3)
 Sof(H64A)=Sof(H64B)=Sof(C65A)=Sof(H65A)=Sof(H65B)=Sof(C66A)=Sof(H66A)=
 Sof(H66B)=FVAR(3)
6.a Riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C19(H19), C20(H20), C23(H23), C24(H24),
 C53(H53), C54(H54), C57(H57), C58(H58), C69(H69), C70(H70), C73(H73), C74(H74)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9AA,H9AB), C9(H9BC,H9BD), C10A(H10A,H10B), C11A(H11A,H11B), C10B(H10C,
 H10D), C11B(H11C,H11D), C12(H12A,H12B), C12(H12C,H12D), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C29(H29C,H29D), C30A(H30A,
 H30B), C31A(H31A,H31B), C30B(H30C,H30D), C31B(H31C,H31D), C32(H32A,H32B),
 C32(H32C,H32D), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C38(H38A,H38B), C39(H39A,H39B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C64(H64C,H64D),
 C65A(H65A,H65B), C66A(H66A,H66B), C65B(H65C,H65D), C66B(H66C,H66D), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
 C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
  C85(H85A,H85B), C86(H86A,H86B), C88(H88A,H88B), C89(H89A,H89B)
6.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C87(H87A,H87B,H87C), C90(H90A,H90B,
 H90C)
;
_shelx_res_checksum              25673
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            19.93371(17)
_cell_oxdiff_length_b            11.24477(8)
_cell_oxdiff_length_c            62.0990(4)
_cell_oxdiff_angle_alpha         90.0124(5)
_cell_oxdiff_angle_beta          94.7232(6)
_cell_oxdiff_angle_gamma         90.0052(6)
_cell_oxdiff_volume              13872.22(18)
_cell_oxdiff_measurement_reflns_used 69944