Intra- and intermolecular interaction of anthracene moieties in 7,8-disilabicyclo[3.3.0]octadienyl-bridged bisanthracenes
Tokoro, Yuichiro; Ohtsuka, Nobuhiko; Fukuzawa, Shin-ichi; Oyama, Toshiyuki; RSC Advances 8 (2018) 25177–; doi:10.1039/C8RA05293J

data_7231131
_publ_section_title
;
 Intra- and intermolecular interaction of anthracene moieties in
 7,8-disilabicyclo[3.3.0]octadienyl-bridged bisanthracenes
;
_journal_issue                   44
_journal_name_full               'RSC Advances'
_journal_page_first              25177
_journal_paper_doi               10.1039/C8RA05293J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C H2 Cl2, C40 H26 O Si2'
_chemical_formula_sum            'C41 H28 Cl2 O Si2'
_chemical_formula_weight         663.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-07
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-07 deposited with the CCDC.
2018-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                98.550(1)
_cell_angle_beta                 97.125(1)
_cell_angle_gamma                107.149(1)
_cell_formula_units_Z            2
_cell_length_a                   10.3826(2)
_cell_length_b                   11.6392(2)
_cell_length_c                   14.3255(2)
_cell_measurement_reflns_used    19691
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.2830
_cell_measurement_theta_min      3.1670
_cell_volume                     1609.80(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9807
_diffrn_measured_fraction_theta_max 0.9807
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     20.00  80.00   0.50    0.63    --   -8.60  77.00  60.00  120
  2  \w    -51.00  32.00   0.50    0.63    --   -8.60  82.00 -30.00  166
  3  \w    -48.00  -5.00   0.50    0.63    --   -8.60  77.00  60.00   86
  4  \w    -83.00 -34.00   0.50    0.63    --   -8.60 -57.00  90.00   98
  5  \w    -75.00 -49.00   0.50    0.63    --    8.60 -57.00 -30.00   52
  6  \w    -29.00  48.00   0.50    0.63    --    8.60 -38.00-150.00  154
  7  \w     34.00  66.00   0.50    0.63    --    8.60  57.00  30.00   64
  8  \w    -33.00  98.00   0.50    0.63    --    8.60  82.00-120.00  262
  9  \w    -34.00  19.00   0.50    0.63    --    8.60 -57.00  90.00  106
 10  \w     32.00  58.00   0.50    0.63    --    8.60  82.00 120.00   52
 11  \w     32.00  88.00   0.50    0.63    --    8.60  38.00-120.00  112
 12  \w    -80.00 -34.00   0.50    0.63    --    8.60 -38.00-150.00   92
 13  \w    -16.00   9.00   0.50    0.63    --    8.60  57.00  30.00   50
 14  \w    -17.00  35.00   0.50    0.63    --    8.60  38.00  60.00  104
 15  \w    -20.00  14.00   0.50    0.63    --    8.60 -57.00 -30.00   68
 16  \w    -13.00  65.00   0.50    0.63    --    8.60  82.00   0.00  156
 17  \w    -29.00   0.00   0.50    0.63    --    8.60  38.00-120.00   58
 18  \w    -24.00  11.00   0.50    0.63    --    8.60  82.00 120.00   70
 19  \w    -34.00  64.00   0.50    0.63    --   32.00 -65.00 172.07  196
 20  \w    153.00 188.00   0.50    2.51    --  100.10  82.00 120.00   70
 21  \w     65.00 105.00   0.50    2.51    --  100.10  45.00   0.00   80
 22  \w     58.00  89.00   0.50    2.51    --  100.10  82.00 120.00   62
 23  \w     65.00 107.00   0.50    2.51    --  100.10  45.00 -30.00   84
 24  \w    140.00 166.00   0.50    2.51    --  100.10  82.00-150.00   52
 25  \w    135.00 189.00   0.50    2.51    --  100.10  45.00 -60.00  108
 26  \w    128.00 185.00   0.50    2.51    --  100.10  45.00 -30.00  114
 27  \w    136.00 188.00   0.50    2.51    --  100.10  45.00  90.00  104
 28  \w    124.00 188.00   0.50    2.51    --  100.10  45.00   0.00  128
 29  \w     65.00 102.00   0.50    2.51    --  100.10  45.00 150.00   74
 30  \w    132.00 189.00   0.50    2.51    --  100.10  45.00 150.00  114
 31  \w     59.00  85.00   0.50    2.51    --  100.10  82.00-150.00   52
 32  \w    148.00 174.00   0.50    2.51    --  100.10  82.00 -60.00   52
 33  \w     98.00 124.00   0.50    2.51    --  100.10  82.00  30.00   52
 34  \w     66.00 104.00   0.50    2.51    --  100.10  45.00  90.00   76
 35  \w    157.00 189.00   0.50    2.51    --  100.10  82.00-180.00   64
 36  \w     58.00  91.00   0.50    2.51    --  100.10  82.00  60.00   66
 37  \w     58.00  92.00   0.50    2.51    --  100.10  82.00-180.00   68
 38  \w     58.00  90.00   0.50    2.51    --  100.10  82.00 -30.00   64
 39  \w    131.00 187.00   0.50    2.51    --  100.10  45.00-180.00  112
 40  \w    141.00 167.00   0.50    2.51    --  100.10  82.00-120.00   52
 41  \w    156.00 188.00   0.50    2.51    --  100.10  82.00 -30.00   64
 42  \w     58.00  83.00   0.50    2.51    --  100.10  82.00 -60.00   50
 43  \w     67.00 110.00   0.50    2.51    --  100.10  45.00-150.00   86
 44  \w    124.00 189.00   0.50    2.51    --  100.10  45.00-150.00  130
 45  \w     65.00  97.00   0.50    2.51    --  100.10  45.00 -90.00   64
 46  \w    135.00 189.00   0.50    2.51    --  100.10  45.00 -90.00  108
 47  \w     61.00  89.00   0.50    2.51    --  100.10  77.00 -60.00   56
 48  \w     66.00 117.00   0.50    2.51    --  100.10  45.00 -60.00  102
 49  \w     65.00 108.00   0.50    2.51    --  100.10  45.00-180.00   86
 50  \w     65.00 108.00   0.50    2.51    --  100.10  45.00 120.00   86
 51  \w    126.00 181.00   0.50    2.51    --  100.10  45.00 120.00  110
 52  \w     62.00 131.00   0.50    2.51    --  100.10 -82.00 120.00  138
 53  \w     58.00  91.00   0.50    2.51    --  100.10  82.00   0.00   66
 54  \w     58.00  90.00   0.50    2.51    --  100.10  82.00  90.00   64
 55  \w     78.00 126.00   0.50    2.51    --  100.10 -82.00-120.00   96
 56  \w    132.00 189.00   0.50    2.51    --  100.10  45.00  60.00  114
 57  \w     57.00 128.00   0.50    2.51    --  100.10 -82.00  30.00  142
 58  \w     58.00  84.00   0.50    2.51    --  100.10  82.00-120.00   52
 59  \w     61.00  92.00   0.50    2.51    --  100.10  77.00-150.00   62
 60  \w     61.00  91.00   0.50    2.51    --  100.10  77.00-120.00   60
 61  \w     65.00 104.00   0.50    2.51    --  100.10  45.00  60.00   78
 62  \w    124.00 178.00   0.50    2.51    --  100.10  45.00-120.00  108
 63  \w    164.00 189.00   0.50    2.51    --  100.10  77.00 -90.00   50
 64  \w     61.00  89.00   0.50    2.51    --  100.10  77.00  30.00   56
 65  \w    128.00 189.00   0.50    2.51    --  100.10  45.00  30.00  122
 66  \w     66.00 101.00   0.50    2.51    --  100.10  45.00-120.00   70
 67  \w     61.00  86.00   0.50    2.51    --  100.10  77.00 120.00   50
 68  \w     37.00 118.00   0.50    2.51    --  100.10 -82.00 -30.00  162
 69  \w     66.00  97.00   0.50    2.51    --  100.10  45.00  30.00   62
 70  \w     61.00  91.00   0.50    2.51    --  100.10  77.00 -90.00   60
 71  \w     60.00 137.00   0.50    2.51    --  100.10 -82.00-180.00  154
 72  \w     42.00  72.00   0.50    2.51    --  100.10 -82.00-120.00   60
 73  \w     58.00  92.00   0.50    2.51    --  100.10  82.00 150.00   68
 74  \w     33.00  58.00   0.50    2.51    --  100.10 -82.00 120.00   50
 75  \w    160.00 186.00   0.50    2.51    --  100.10  82.00  30.00   52
 76  \w     59.00  84.00   0.50    2.51    --  100.10  82.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1006811000
_diffrn_orient_matrix_UB_12      0.0477693000
_diffrn_orient_matrix_UB_13      -0.0587295000
_diffrn_orient_matrix_UB_21      -0.0544398000
_diffrn_orient_matrix_UB_22      0.0361507000
_diffrn_orient_matrix_UB_23      0.0914637000
_diffrn_orient_matrix_UB_31      0.1086204000
_diffrn_orient_matrix_UB_32      0.1279061000
_diffrn_orient_matrix_UB_33      0.0199241000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30926
_diffrn_reflns_theta_full        72.8200
_diffrn_reflns_theta_max         72.82
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.3692
_exptl_crystal_description       block
_exptl_crystal_F_000             692.1154
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.2608
_refine_diff_density_min         -0.5640
_refine_diff_density_rms         0.0760
_refine_ls_d_res_high            0.8069
_refine_ls_d_res_low             13.9409
_refine_ls_goodness_of_fit_ref   1.0346
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    55
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0346
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.6189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5829
_reflns_number_total             6285
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra05293j2.cif
_cod_data_source_block           yt3_077_180322
_cod_database_code               7231131
_chemical_oxdiff_formula         C36H24OSi2
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C44(H44a,H44b)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C27(H27), C20(H20), C18(H18), C4(H4), C13(H13), C22(H22), C32(H32),
 C38(H38), C36(H36), C19(H19), C26(H26), C25(H25), C40(H40), C41(H41), C24(H24),
  C8(H8), C12(H12), C6(H6), C10(H10), C5(H5), C33(H33), C39(H39), C11(H11),
 C34(H34), C35(H35)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.165
_oxdiff_exptl_absorpt_empirical_full_min 0.428