Solution and solid state structures and magnetism of a series of linear trinuclear compounds with a hexacoordinate Ln(III) and two terminal Ni(II) centers.
Comba, Peter; Enders, Markus; Großhauser, Michael; Hiller, Markus; Müller, Dennis; Wadepohl, Hubert; Dalton transactions (Cambridge, England : 2003) 46 (2016) 138–149; doi:10.1039/c6dt03488h

data_7041288
_publ_section_title
;
 Solution and solid state structures and magnetism of a series of linear
 trinuclear compounds with a hexacoordinate Ln(III) and two terminal
 Ni(II) centers.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              138
_journal_page_last               149
_journal_paper_doi               10.1039/c6dt03488h
_journal_volume                  46
_journal_year                    2016
_chemical_formula_moiety         'C66 H84 N6 Ni2 O12 Tm, Cl O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H88 Cl5 N6 Ni2 O16 Tm'
_chemical_formula_weight         1709.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mg71
_audit_creation_date
;
'Mon Nov 24 14:27:26 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-04 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.335(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3567(4)
_cell_length_b                   23.5628(3)
_cell_length_c                   18.0810(3)
_cell_measurement_reflns_used    48936
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.5140
_cell_measurement_theta_min      4.4520
_cell_volume                     7772.7(3)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); 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 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -67.00   17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   90.0000 84

  2 omega   42.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000   90.0000 28

  3 omega   39.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 29

  4 omega  -43.00    5.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000   90.0000 48

  5 omega  -15.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -90.0000 67

  6 omega   16.00   41.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000   90.0000 25

  7 omega  -20.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 48

  8 omega   77.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 47

  9 omega   24.00   97.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 73

 10 omega  -17.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000  -90.0000 94

 11 omega  -11.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   30.0000 81

 12 omega   24.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 30

 13 omega   24.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 35

 14 omega   57.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 30

 15 omega   80.00  119.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 39

 16 omega   24.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 35

 17 omega   27.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  150.0000 40

 18 omega   24.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 26

 19 omega   24.00  114.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 90

 20 omega   25.00   70.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 45

 21 omega   73.00  112.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 39

 22 omega   25.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 25

 23 omega   24.00  118.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 94

 24 omega   27.00   64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   73.0000  -59.0078 37

 25 omega   30.00  118.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -135.0000  -37.0000 88

 26 omega   24.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 97

 27 omega   78.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   73.0000  -59.0078 45

 28 omega    1.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000 -180.0000 52

 29 omega   24.00   56.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 32

 30 omega   46.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 65

 31 omega   85.00  164.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 79

 32 omega  108.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 70

 33 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

 34 omega  112.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 46

 35 omega   78.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 32

 36 omega   78.00  142.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -141.2729 64

 37 omega   82.00  114.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -150.0000 32

 38 omega   85.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -150.0000 26

 39 omega   79.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

 40 omega   38.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   30.0000 66

 41 omega   36.00  146.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000   30.0000 110

 42 omega   80.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  139.3336 26

 43 omega   79.00  173.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   45.3599 94

 44 omega   78.00  166.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 88

 45 omega  138.00  165.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   12.5155 27

 46 omega   79.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 27

 47 omega   79.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   12.5155 27

 48 omega   83.00  109.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   69.0000  -74.4128 26

 49 omega   86.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 25

 50 omega  110.00  169.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 59

 51 omega   78.00  106.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 28

 52 omega   85.00  174.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 89

 53 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 26

 54 omega   82.00  108.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  150.0000 26

 55 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

 56 omega  117.00  145.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   76.0675 28

 57 omega   85.00  116.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -60.0000 31

 58 omega   78.00  104.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

 59 omega   78.00  138.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 60

 60 omega   70.00  113.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 43

 61 omega   39.00  102.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -150.0000 63

 62 omega   85.00  175.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 90

 63 omega   36.00  124.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000 -150.0000 88

 64 omega   78.00  176.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 98

 65 omega   81.00  115.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   72.0000   76.0675 34

 66 omega   79.00  156.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -24.8508 77

 67 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   90.0000 90

 68 omega  -44.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000  -90.0000 117

 69 omega  -72.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -38.0000  -60.0000 98

 70 omega  -21.00   69.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

 71 omega  -73.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -19.0000  -30.0000 117

 72 omega  -18.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000  150.0000 98

 73 omega   33.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -60.0000 90

 74 omega    1.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000 -120.0000 95

 75 omega   33.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   90.0000 90

 76 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 100

 77 omega   23.00  111.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000   60.0000 88

 78 omega   23.00  111.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  120.0000 88

 79 omega  -18.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000  -30.0000 98

 80 omega   33.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 90

 81 omega  -15.00   75.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 90

 82 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 100

 83 omega  -18.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   60.0000 98

 84 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 100

 85 omega   33.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 90

 86 omega   26.00  123.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   73.0000  -59.0078 97

 87 omega  -18.00   80.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000 -150.0000 98

 88 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 100

 89 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 100

 90 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 100

 91 omega   24.00  124.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 100

 92 omega   41.00  131.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -64.0000 -150.0000 90

 93 omega  100.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 78

 94 omega  100.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 78

 95 omega   35.00   94.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 59

 96 omega   74.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -30.0000 104

 97 omega  100.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 78

 98 omega   85.00  110.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000   90.0000 25

 99 omega   86.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000 -150.0000 92

100 omega   36.00  116.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  120.0000 80

101 omega   86.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000    0.0000 92

102 omega   78.00  178.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 100

;
_diffrn_measurement_device       'four-circle 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      0.0841708000
_diffrn_orient_matrix_UB_12      -0.0027598000
_diffrn_orient_matrix_UB_13      0.0362641000
_diffrn_orient_matrix_UB_21      -0.0067618000
_diffrn_orient_matrix_UB_22      -0.0359834000
_diffrn_orient_matrix_UB_23      -0.0741878000
_diffrn_orient_matrix_UB_31      -0.0001836000
_diffrn_orient_matrix_UB_32      0.0545105000
_diffrn_orient_matrix_UB_33      -0.0471407000
_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  0.0849
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            210562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.051
_diffrn_reflns_theta_min         3.752
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.739
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   gaussian
_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)
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    1.460
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.044
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         14914
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+24.8211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12731
_reflns_number_total             14914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03488h2.cif
_cod_data_source_block           co_mg71_sq
_cod_depositor_comments
'Adding full bibliography for 7041276--7041289.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7041288
_audit_block_refno               2225
_audit_block_usercomment         'MG428, plate, colourless'
_chemical_oxdiff_formula         'C68 H88 Cl5 N6 O16 Ni2 Tm C6H14'
_chemical_oxdiff_usercomment     'MG428, plate, colourless'
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.547
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 C81-Cl11 \\sim C81-Cl12 \\sim C82-Cl21 \\sim C82-Cl22
 with sigma of 0.01
 Cl11-Cl12 \\sim Cl21-Cl22
 with sigma of 0.02
 Cl1-O11 \\sim Cl1-O12 \\sim Cl1-O13 \\sim Cl1-O14
 with sigma of 0.01
 O11-O12 \\sim O11-O13 \\sim O11-O14 \\sim O12-O13 \\sim O12-O14 \\sim O13-O14
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C116(H11G,H11H), C125(H12G,H12H),
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C207(H20M,H20N), C216(H21G,H21H), C225(H22G,H22H),
 C81(H81A,H81B), C82(H82A,H82B)
3.b Aromatic/amide H refined with riding coordinates:
 C111(H111), C113(H113), C120(H120), C122(H122), C129(H129), C131(H131),
 C211(H211), C213(H213), C220(H220), C222(H222), C229(H229), C231(H231)
3.c Idealised Me refined as rotating group:
 C114(H11A,H11B,H11C), C115(H11D,H11E,H11F), C123(H12A,H12B,H12C), C124(H12D,
 H12E,H12F), C132(H13A,H13B,H13C), C133(H13D,H13E,H13F), C214(H21A,H21B,H21C),
 C215(H21D,H21E,H21F), C223(H22A,H22B,H22C), C224(H22D,H22E,H22F), C232(H23A,
 H23B,H23C), C233(H23D,H23E,H23F)
;
_shelx_res_checksum              16197
_shelx_fab_checksum              10985
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            20.3578(3)
_cell_oxdiff_length_b            23.5652(2)
_cell_oxdiff_length_c            18.07915(19)
_cell_oxdiff_angle_alpha         89.9925(9)
_cell_oxdiff_angle_beta          116.3412(13)
_cell_oxdiff_angle_gamma         90.0125(10)
_cell_oxdiff_volume              7772.66(16)
_cell_oxdiff_measurement_reflns_used 48936