Methylene-bridged, intramolecular donor-acceptor systems based on rare-earth metals and phosphinomethanides.
Pieper, Martin; Lamm, Jan-Hendrik; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5326–5336; doi:10.1039/c7dt00554g

data_7042569
_publ_section_title
;
 Methylene-bridged, intramolecular donor-acceptor systems based on
 rare-earth metals and phosphinomethanides.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5326
_journal_page_last               5336
_journal_paper_doi               10.1039/c7dt00554g
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C56 H38 Ho2, 2(C6 H6)'
_chemical_formula_sum            'C68 H50 Ho2'
_chemical_formula_weight         1196.94
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-06
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2017-02-10 deposited with the CCDC.
2017-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.7876(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.59946(11)
_cell_length_b                   14.44030(17)
_cell_length_c                   15.36988(11)
_cell_measurement_reflns_used    79548
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2320
_cell_measurement_theta_min      2.8730
_cell_volume                     2556.41(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
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_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9949
_diffrn_measurement_details
;
  1 omega  -84.00   37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -30.0000 121

  2 omega  -84.00   37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 121

  3 omega  -95.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   60.0000 61

  4 omega  -39.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000  -60.0000 131

  5 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000 -180.0000 131

  6 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000  -90.0000 131

  7 omega  -96.00   -2.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  125.0000  -90.0000 94

  8 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000  -60.0000 131

  9 omega  -96.00   -2.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  125.0000 -150.0000 94

 10 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000    0.0000 131

 11 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000   60.0000 131

 12 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000 -150.0000 131

 13 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000  120.0000 131

 14 omega   19.00   45.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   82.0000   91.5094 26

 15 omega   23.00  122.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000 -125.0000   60.0000 99

 16 omega   94.00  143.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000  125.0000 -150.0000 49

 17 omega   19.00   45.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   82.0000   15.6094 26

 18 omega   94.00  143.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000  125.0000  -60.0000 49

 19 omega   19.00   46.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   81.0000  -92.7748 27

 20 omega   20.00   47.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   79.0000 -118.4434 27

 21 omega   94.00  143.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000  125.0000 -120.0000 49

 22 omega   19.00   46.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   81.0000   43.5675 27

 23 omega   20.00   46.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   80.0000  129.5388 26

 24 omega   27.00  163.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000  -91.0000  -60.0000 136

 25 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   69.0000  -87.1690 97

 26 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000  120.0000 96

 27 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   64.0000  124.5415 96

 28 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   65.0000  105.3914 97

 29 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000 -180.0000 98

 30 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000    0.0000 83

 31 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000  -60.0000 98

 32 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000  120.0000 83

 33 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000 -120.0000 98

 34 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   47.0000   27.9859 95

 35 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000   90.0000 96

 36 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000  -90.0000 83

 37 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000 -150.0000 98

 38 omega   34.00  156.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000  -63.0000   90.0000 122

 39 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   73.0000   46.9885 98

 40 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   75.0000  175.0432 98

 41 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000    0.0000 96

 42 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000  150.0000 98

 43 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000   60.0000 98

 44 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000  -90.0000 98

 45 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   76.0000    1.0053 98

 46 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000 -150.0000 96

 47 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   73.0000  -22.0054 98

 48 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000  -60.0000 83

 49 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000  150.0000 95

 50 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000  -30.0000 96

 51 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000   30.0000 96

 52 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000 -120.0000 96

 53 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   57.0000  -17.0115 96

 54 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000   30.0000 98

 55 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   69.0000  169.9417 97

 56 omega   35.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000  -50.0000  -60.0000 69

 57 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   68.0000  -98.3069 97

 58 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   74.0000  143.2037 98

 59 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000  150.0000 96

 60 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000  -60.0000 96

 61 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   75.0000  127.1049 98

 62 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000 -150.0000 83

 63 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   74.0000 -154.9863 98

 64 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   64.0000   96.8399 96

 65 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -150.0000 192

 66 omega  -92.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  150.0000 131

 67 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -180.0000 192

 68 omega    1.00   47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -30.0000 46

 69 omega  -37.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 121

 70 omega  -37.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 121

 71 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000   90.0000 131

 72 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000 -120.0000 131

 73 omega -151.00  -20.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -77.0000  150.0000 131

 74 omega -144.00  -23.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -57.0000   30.0000 121

 75 omega -144.00  -23.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -57.0000  -30.0000 121

 76 omega -146.00  -22.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -66.0000  138.0209 124

 77 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000  -90.0000 121

 78 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000   60.0000 121

 79 omega   20.00  151.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   77.0000  120.0000 131

 80 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000 -150.0000 121

 81 omega   20.00  151.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   77.0000  -60.0000 131

 82 omega   20.00  151.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   77.0000  150.0000 131

 83 omega   94.00  143.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000  125.0000  -30.0000 49

 84 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000  -60.0000 121

 85 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000 -120.0000 121

 86 omega   20.00  151.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   77.0000   90.0000 131

 87 omega   20.00  151.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   77.0000  -30.0000 131

 88 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000   30.0000 121

 89 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000   30.0000 95

 90 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000 -120.0000 95

 91 omega   64.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   25.0000 -180.0000 114

 92 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   37.0000   86.9650 96

 93 omega   64.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   25.0000   60.0000 114

 94 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000   60.0000 95

 95 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   45.0000  -90.4856 95

 96 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   46.0000  -28.1425 95

 97 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   67.0000  143.4910 97

 98 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000  -30.0000 95

 99 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   38.0000   60.0000 96

100 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   46.0000   87.1332 95

101 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   38.0000  -90.0000 96

102 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000  120.0000 95

103 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000 -150.0000 95

104 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000   90.0000 98

105 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000  -30.0000 98

106 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000 -180.0000 95

107 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000   60.0000 83

108 omega   33.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000 -111.0000 -180.0000 83

109 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000  120.0000 98

110 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000    0.0000 95

111 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000  -90.0000 96

112 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   49.0000 -136.7248 95

113 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000   90.0000 95

114 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   62.0000 -116.1305 96

115 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000  -60.0000 95

116 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   38.0000  -30.0000 96

117 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   38.0000    0.0000 96

118 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   38.0000  120.0000 96

119 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   50.0000  -90.0000 95

120 omega   80.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   77.0000   14.2091 98

121 omega   64.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   25.0000  -60.0000 114

122 omega   64.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   25.0000    0.0000 114

123 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   70.0000  -34.1065 97

124 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      119.0000   63.0000 -180.0000 96

125 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  -30.0000 192

126 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000    0.0000 192

127 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -120.0000 192

128 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  -90.0000 192

129 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000   30.0000 192

130 omega  -96.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000  -60.0000 192

131 omega -144.00  -23.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -57.0000  -60.0000 121

132 omega -144.00  -23.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -      -59.5000  -57.0000 -180.0000 121

133 omega   23.00  144.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   57.0000  150.0000 121

134 omega   22.00  129.00   1.0000    4.4850
omega____ theta____ kappa____ phi______ frames
    -       59.5000   63.0000  -96.2259 107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0754642000
_diffrn_orient_matrix_UB_12      0.0455946000
_diffrn_orient_matrix_UB_13      0.0776577000
_diffrn_orient_matrix_UB_21      0.0343953000
_diffrn_orient_matrix_UB_22      0.0771939000
_diffrn_orient_matrix_UB_23      -0.0611359000
_diffrn_orient_matrix_UB_31      -0.1048452000
_diffrn_orient_matrix_UB_32      0.0577521000
_diffrn_orient_matrix_UB_33      0.0208505000
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0064
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            147476
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.997
_diffrn_reflns_theta_min         4.215
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2755
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.0865
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00068(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0419P)^2^+6.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4853
_reflns_number_total             5012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00554g2.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 7042559--7042570.cif.'
_cod_database_code               7042569
_chemical_oxdiff_formula         'C68 H50 Ho2'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_res_checksum              48184
_shelxl_version_number           2014-3