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_7231130
_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         'C40 H26 Si2'
_chemical_formula_sum            'C40 H26 Si2'
_chemical_formula_weight         562.82
_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     iterative
_audit_creation_date             2017-07-05
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-07 deposited with the CCDC.
2018-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                78.2801(9)
_cell_angle_beta                 76.5644(9)
_cell_angle_gamma                78.9663(9)
_cell_formula_units_Z            2
_cell_length_a                   10.09473(11)
_cell_length_b                   10.11978(11)
_cell_length_c                   16.43719(17)
_cell_measurement_reflns_used    17653
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.2280
_cell_measurement_theta_min      4.5020
_cell_volume                     1580.73(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9795
_diffrn_measured_fraction_theta_max 0.9795
_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     61.00  94.00   0.50    1.12    --    8.60  41.00  69.00   66
  2  \w     96.00 136.00   0.50    4.48    --  100.10  41.00  69.00   80
  3  \w    140.00 166.00   0.50    4.48    --  100.10  41.00  69.00   52
  4  \w     52.00  78.00   0.50    4.48    --  100.10 -41.00 -83.00   52
  5  \w    110.00 136.00   0.50    4.48    --  100.10 -41.00 -83.00   52
  6  \w     62.00  87.00   0.50    4.48    --  100.10  41.00  69.00   50
  7  \w    -96.00 -23.00   0.50    1.12    --   -8.60 -38.00-120.00  146
  8  \w    -15.00  30.00   0.50    1.12    --   -8.60 -38.00-120.00   90
  9  \w    -97.00 -71.00   0.50    1.12    --   -8.60 -41.00 -83.00   52
 10  \w    -58.00 -33.00   0.50    1.12    --   -8.60 -41.00 -83.00   50
 11  \w     18.00  44.00   0.50    1.12    --   -8.60  41.00  69.00   52
 12  \w    -27.00  -1.00   0.50    1.12    --   -8.60  41.00  69.00   52
 13  \w    -28.00  34.00   0.50    1.12    --    8.60  38.00-180.00  124
 14  \w    -31.00  26.00   0.50    1.12    --    8.60  77.00 -30.00  114
 15  \w    -21.00  37.00   0.50    1.12    --    8.60  57.00  30.00  116
 16  \w     61.00  87.00   0.50    1.12    --    8.60  57.00  30.00   52
 17  \w    -31.00  31.00   0.50    1.12    --    8.60  77.00-180.00  124
 18  \w     44.00  98.00   0.50    1.12    --    8.60  38.00-180.00  108
 19  \w     38.00  94.00   0.50    1.12    --    8.60  77.00-180.00  112
 20  \w    -41.00 -16.00   0.50    1.12    --    8.60 -41.00 -83.00   50
 21  \w    -52.00  45.00   0.50    1.12    --    8.60 -38.00-180.00  194
 22  \w     57.00  82.00   0.50    1.12    --    8.60  77.00 -30.00   50
 23  \w    -55.00   6.00   0.50    1.12    --   28.00 -64.00 -64.99  122
 24  \w      9.00  59.00   0.50    1.12    --   28.00 -64.00 -64.99  100
 25  \w    -15.00  66.00   0.50    1.12    --   32.00 -68.00  -2.17  162
 26  \w    -56.00  63.00   0.50    1.12    --   32.00 -61.00 115.47  238
 27  \w    -56.00 -21.00   0.50    1.12    --   32.00 -68.00  -2.17   70
 28  \w     58.00  83.00   0.50    4.48    --  100.10  82.00 -60.00   50
 29  \w     58.00  87.00   0.50    4.48    --  100.10  82.00  60.00   58
 30  \w     58.00  83.00   0.50    4.48    --  100.10  82.00 -30.00   50
 31  \w     70.00 186.00   0.50    4.48    --  100.10  61.00 -30.00  232
 32  \w     70.00 138.00   0.50    4.48    --  100.10 -82.00 -90.00  136
 33  \w     60.00  91.00   0.50    4.48    --  100.10  82.00   0.00   62
 34  \w    164.00 189.00   0.50    4.48    --  100.10  82.00   0.00   50
 35  \w     65.00 189.00   0.50    4.48    --  100.10  45.00 150.00  248
 36  \w     61.00  89.00   0.50    4.48    --  100.10  77.00  90.00   56
 37  \w     59.00  85.00   0.50    4.48    --  100.10  82.00-180.00   52
 38  \w     66.00 189.00   0.50    4.48    --  100.10  45.00-180.00  246
 39  \w     11.00  46.00   0.50    4.48    --  100.10 -82.00-180.00   70
 40  \w     15.00 141.00   0.50    4.48    --  100.10 -82.00 -30.00  252
 41  \w    137.00 182.00   0.50    4.48    --  100.10  82.00 120.00   90
 42  \w     59.00  87.00   0.50    4.48    --  100.10  82.00 -90.00   56
 43  \w    106.00 131.00   0.50    4.48    --  100.10  82.00  30.00   50
 44  \w     58.00  83.00   0.50    4.48    --  100.10  82.00  30.00   50
 45  \w     58.00  88.00   0.50    4.48    --  100.10  82.00 120.00   60
 46  \w     61.00  86.00   0.50    4.48    --  100.10  77.00-180.00   50
 47  \w     66.00 188.00   0.50    4.48    --  100.10  45.00 -90.00  244
 48  \w    125.00 189.00   0.50    4.48    --  100.10  77.00-150.00  128
 49  \w     61.00  86.00   0.50    4.48    --  100.10  77.00 -90.00   50
 50  \w     61.00  86.00   0.50    4.48    --  100.10  77.00 -30.00   50
 51  \w    161.00 188.00   0.50    4.48    --  100.10  77.00 -30.00   54
 52  \w     59.00  86.00   0.50    4.48    --  100.10  82.00-150.00   54
 53  \w     58.00  83.00   0.50    4.48    --  100.10  82.00  90.00   50
 54  \w     43.00 141.00   0.50    4.48    --  100.10 -82.00  30.00  196
 55  \w     58.00 140.00   0.50    4.48    --  100.10 -82.00-180.00  164
 56  \w     11.00  56.00   0.50    4.48    --  100.10 -82.00 -90.00   90
 57  \w     65.00 173.00   0.50    4.48    --  100.10  45.00  90.00  216
 58  \w     66.00 141.00   0.50    4.48    --  100.10  45.00 120.00  150
 59  \w     61.00  87.00   0.50    4.48    --  100.10  77.00 120.00   52
 60  \w     55.00 111.00   0.50    4.48    --  100.10  30.00-120.00  112
 61  \w    120.00 189.00   0.50    4.48    --  100.10  30.00-120.00  138
 62  \w     54.00  96.00   0.50    4.48    --  100.10  30.00   0.00   84
 63  \w    144.00 188.00   0.50    4.48    --  100.10  30.00   0.00   88
 64  \w     66.00  98.00   0.50    4.48    --  100.10  45.00 -60.00   64
 65  \w    132.00 179.00   0.50    4.48    --  100.10  45.00 -60.00   94
 66  \w     61.00  94.00   0.50    4.48    --  100.10  77.00  30.00   66
 67  \w     58.00  83.00   0.50    4.48    --  100.10  82.00 150.00   50
 68  \w     61.00 117.00   0.50    4.48    --  100.10  77.00-150.00  112
 69  \w     65.00 112.00   0.50    4.48    --  100.10 -82.00  60.00   94
 70  \w    138.00 181.00   0.50    4.48    --  100.10  61.00   0.00   86
 71  \w     69.00 106.00   0.50    4.48    --  100.10  61.00   0.00   74
 72  \w    155.00 181.00   0.50    4.48    --  100.10  82.00-120.00   52
 73  \w     61.00  86.00   0.50    4.48    --  100.10  77.00   0.00   50
 74  \w     61.00  99.00   0.50    4.48    --  100.10  77.00 -60.00   76
 75  \w     58.00  84.00   0.50    4.48    --  100.10  82.00-120.00   52
 76  \w     41.00 140.00   0.50    4.48    --  100.10 -82.00 150.00  198
 77  \w    123.00 148.00   0.50    4.48    --  100.10  82.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0321896000
_diffrn_orient_matrix_UB_12      -0.0980966000
_diffrn_orient_matrix_UB_13      -0.0507644000
_diffrn_orient_matrix_UB_21      0.1397568000
_diffrn_orient_matrix_UB_22      -0.0902739000
_diffrn_orient_matrix_UB_23      0.0064882000
_diffrn_orient_matrix_UB_31      -0.0680335000
_diffrn_orient_matrix_UB_32      -0.0834682000
_diffrn_orient_matrix_UB_33      0.0832476000
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34297
_diffrn_reflns_theta_full        72.6396
_diffrn_reflns_theta_max         72.64
_diffrn_reflns_theta_min         4.51
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77014
_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            'translucent yellow'
_exptl_crystal_density_diffrn    1.1824
_exptl_crystal_description       block
_exptl_crystal_F_000             590.4854
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.3293
_refine_diff_density_min         -0.3350
_refine_diff_density_rms         0.0367
_refine_ls_d_res_high            0.8077
_refine_ls_d_res_low             9.7946
_refine_ls_goodness_of_fit_ref   0.9496
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.9437
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0759P)^2^+0.3895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5481
_reflns_number_total             6162
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra05293j2.cif
_cod_data_source_block           yt2_063_170703
_cod_database_code               7231130
_chemical_oxdiff_formula         C46H40Si2
_diffrn_oxdiff_ac3_digest_frames
;
01ce367fdd5a8e43f6d6157b2130457dc007486e9ca
;
_diffrn_oxdiff_ac3_digest_hkl
;
0174e7ef32a1ad8d43b20300081ef990e486f7
;
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C23 \\sim C31 \\sim C37 \\sim C36 \\sim C35 \\sim C32 \\sim C34: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: C6bb(0.5) C8bb(0.5) C6ba(0.5) C8ba(0.5) H8ba(0.5) H6ba(0.5)
 Fixed U22: C8bb(3.829623)
4.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C4(H4), C5(H5), C6(H6), C37(H37), C36(H36), C35(H35), C34(H34),
 C32(H32), C8(H8), C18(H18), C19(H19), C20(H20), C39(H39), C40(H40), C41(H41),
 C42(H42), C43(H43), C27(H27), C24(H24), C25(H25), C26(H26), C13(H13), C12(H12),
  C11(H11), C10(H10)
;
_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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.842