Diamidophosphines with six-membered chelates and their coordination chemistry with group 4 metals: development of a trimethylene-methane-tethered [PN2]-type "molecular claw".
Batke, S.; Kothe, T.; Haas, M.; Wadepohl, H.; Ballmann, J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 3528–3540; doi:10.1039/c5dt04911c

data_7038127
_publ_section_title
;
 Diamidophosphines with six-membered chelates and their coordination
 chemistry with group 4 metals: development of a
 trimethylene-methane-tethered [PN2]-type &quot;molecular claw&quot;.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3528
_journal_page_last               3540
_journal_paper_doi               10.1039/c5dt04911c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C24 H35 Cl2 N2 P Ti'
_chemical_formula_sum            'C24 H35 Cl2 N2 P Ti'
_chemical_formula_weight         501.31
_chemical_properties_physical    moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_tk4
_audit_creation_date
;
'Mon Mar 02 18:39:36 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-07 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8960(3)
_cell_length_b                   20.0990(4)
_cell_length_c                   9.01231(14)
_cell_measurement_reflns_used    18276
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.6330
_cell_measurement_theta_min      5.3660
_cell_volume                     2517.10(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_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 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
  1 omega   10.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 28

  2 omega  -20.00   66.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -180.0000 86

  3 omega  -59.00    1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000   60.0000 60

  4 omega   41.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 31

  5 omega  -25.00    7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -30.0000 32

  6 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -180.0000 90

  7 omega   24.00   54.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 30

  8 omega    3.00   73.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -90.0000 70

  9 omega   24.00   50.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 26

 10 omega   -9.00   74.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 83

 11 omega   24.00   67.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   60.0000 43

 12 omega   24.00   50.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 26

 13 omega   75.00  119.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 44

 14 omega   62.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 60

 15 omega   24.00   62.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 38

 16 omega   81.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 43

 17 omega   23.00   94.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000  120.0000 71

 18 omega   25.00   68.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -180.0000 43

 19 omega   24.00   56.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 32

 20 omega   24.00  120.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 96

 21 omega   87.00  122.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 35

 22 omega  -14.00   72.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  120.0000 86

 23 omega   55.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -30.0000 53

 24 omega   24.00   58.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 34

 25 omega   26.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   90.0000 98

 26 omega   57.00  112.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  150.0000 55

 27 omega   24.00   51.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  120.0000 27

 28 omega   24.00   53.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 29

 29 omega   80.00  118.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -90.0000 38

 30 omega   82.00  157.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000  120.0000 75

 31 omega   45.00   72.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 27

 32 omega   78.00  162.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 84

 33 omega   85.00  133.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -30.0000 48

 34 omega   85.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  -90.0000 26

 35 omega   80.00  106.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  135.2122 26

 36 omega  117.00  144.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -76.5469 27

 37 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 26

 38 omega   78.00  123.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 45

 39 omega   80.00  177.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000   14.0621 97

 40 omega   36.00  125.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000 -180.0000 89

 41 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

 42 omega  117.00  144.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000 -137.3822 27

 43 omega   79.00  105.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  -76.5469 26

 44 omega   80.00  156.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   74.0000  -50.0831 76

 45 omega   78.00  176.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 98

 46 omega   80.00  107.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   73.0000 -137.3822 27

 47 omega   78.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 100

 48 omega   78.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 100

 49 omega   78.00  139.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 61

 50 omega   37.00  120.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000    0.0000 83

 51 omega  118.00  175.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   58.0000   86.1952 57

 52 omega   79.00  172.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000 -162.6481 93

 53 omega   78.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 33

 54 omega   79.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 25

 55 omega   79.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 99

 56 omega   88.00  113.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   58.0000   86.1952 25

 57 omega   57.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 54

 58 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 26

 59 omega   85.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000    0.0000 26

 60 omega   85.00  111.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000  150.0000 26

 61 omega   79.00  105.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   75.0000  166.7059 26

 62 omega   85.00  118.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   64.0000 -120.0000 33

 63 omega   79.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000   40.2016 99

 64 omega  151.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  106.6256 27

 65 omega   39.00  103.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000    0.0000 64

 66 omega   37.00  116.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 79

 67 omega   78.00  104.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  106.6256 26

 68 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  120.0000 90

 69 omega  -70.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -120.0000 100

 70 omega  -54.00    2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  120.0000 -138.0000 56

 71 omega  -21.00   69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  120.0000 90

 72 omega  -69.00   21.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 90

 73 omega    1.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  120.0000 95

 74 omega   28.00  126.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000   60.0000 98

 75 omega  -18.00   80.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000  120.0000 98

 76 omega  -16.00   84.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -77.0000  -90.0000 100

 77 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -150.0000 90

 78 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -30.0000 90

 79 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -90.0000 90

 80 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  150.0000 90

 81 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  120.0000 90

 82 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000  -60.0000 100

 83 omega    1.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000  -60.0000 95

 84 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 90

 85 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 100

 86 omega    1.00   96.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 95

 87 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000   30.0000 100

 88 omega   19.00  108.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -120.0000  137.0000 89

 89 omega   33.00  123.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -60.0000 90

 90 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 100

 91 omega   28.00  126.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000 -180.0000 98

 92 omega   24.00  124.00   1.0000    9.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -120.0000 100

 93 omega   36.00   93.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -30.0000 57

 94 omega  100.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 78

 95 omega   36.00   93.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 57

 96 omega   35.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   90.0000 59

 97 omega   36.00  116.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 80

 98 omega   35.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  150.0000 59

 99 omega  100.00  145.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 45

100 omega   36.00  146.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000  150.0000 110

101 omega   78.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

102 omega   86.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000  -90.0000 92

103 omega   86.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   50.0000   60.0000 92

104 omega   79.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   76.0000 -162.6481 99

105 omega   35.00   94.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -90.0000 59

;
_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      0.0134927000
_diffrn_orient_matrix_UB_12      -0.0760591000
_diffrn_orient_matrix_UB_13      -0.0017524000
_diffrn_orient_matrix_UB_21      0.0123083000
_diffrn_orient_matrix_UB_22      0.0002962000
_diffrn_orient_matrix_UB_23      0.1699014000
_diffrn_orient_matrix_UB_31      -0.1093605000
_diffrn_orient_matrix_UB_32      -0.0093537000
_diffrn_orient_matrix_UB_33      0.0189036000
_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  0.1029
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            39026
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.048
_diffrn_reflns_theta_min         5.852
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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            'dark red'
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+16.1905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.1932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2144
_reflns_number_total             2452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04911c2.cif
_cod_data_source_block           ba_tk4_4
_cod_depositor_comments
'Adding full bibliography for 7038121--7038129.cif.'
_cod_database_code               7038127
_audit_block_refno               2354
_audit_block_usercomment         'TK102, plate, red'
_chemical_oxdiff_formula         'C24 H35 Cl2 N2 P Ti'
_chemical_oxdiff_usercomment     'TK102, plate, red'
_shelx_estimated_absorpt_t_max   0.608
_shelx_estimated_absorpt_t_min   0.072
_diffrn_oxdiff_twin_integration_method simultaneous
_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. Others
 Fixed Sof: H1A(0.5) H1B(0.5)
3.a Ternary CH refined with riding coordinates:
 C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              92968
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            13.8946(4)
_cell_oxdiff_length_b            20.1031(4)
_cell_oxdiff_length_c            9.01134(16)
_cell_oxdiff_angle_alpha         90.0295(16)
_cell_oxdiff_angle_beta          90.0004(19)
_cell_oxdiff_angle_gamma         90.002(2)
_cell_oxdiff_volume              2517.10(10)
_cell_oxdiff_measurement_reflns_used 17913
_cell_oxdiff_twin_number         2