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_7231132
_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         'C48 H42 Si2'
_chemical_formula_sum            'C48 H42 Si2'
_chemical_formula_weight         675.04
_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             2018-01-18
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-11 deposited with the CCDC.
2018-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                81.018(1)
_cell_angle_beta                 82.595(1)
_cell_angle_gamma                71.977(1)
_cell_formula_units_Z            2
_cell_length_a                   10.0656(1)
_cell_length_b                   11.6376(1)
_cell_length_c                   17.0207(1)
_cell_measurement_reflns_used    18829
_cell_measurement_temperature    223
_cell_measurement_theta_max      72.2010
_cell_measurement_theta_min      4.0180
_cell_volume                     1865.81(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 0.9823
_diffrn_measured_fraction_theta_max 0.9813
_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     -6.00  38.00   0.50    2.12    --    8.60 -57.00  -7.00   88
  2  \w    -55.00 -30.00   0.50    2.12    --    8.60 -57.00  -7.00   50
  3  \w     14.00  40.00   0.50    2.12    --    8.60  57.00 133.00   52
  4  \w    146.00 186.00   0.50    8.49    --  100.10  57.00 133.00   80
  5  \w     53.00 106.00   0.50    8.49    --  100.10 -57.00  -7.00  106
  6  \w     70.00  96.00   0.50    8.49    --  100.10  57.00 133.00   52
  7  \w    -18.00   8.00   0.50    2.12    --   -8.60  57.00 133.00   52
  8  \w     23.00  49.00   0.50    2.12    --   -8.60  57.00 133.00   52
  9  \w    -97.00 -57.00   0.50    2.12    --   -8.60 -57.00 120.00   80
 10  \w    -40.00  19.00   0.50    2.12    --   -8.60 -57.00 120.00  118
 11  \w    -62.00 -10.00   0.50    2.12    --   -8.60 -57.00  -7.00  104
 12  \w    -77.00  51.00   0.50    2.12    --    8.60 -82.00 -30.00  256
 13  \w      0.00  66.00   0.50    2.12    --    8.60  82.00 120.00  132
 14  \w     30.00  56.00   0.50    2.12    --    8.60  77.00  90.00   52
 15  \w    -26.00  95.00   0.50    2.12    --    8.60  19.00 -90.00  242
 16  \w    -15.00  97.00   0.50    2.12    --    8.60  38.00 -30.00  224
 17  \w     25.00  51.00   0.50    2.12    --    8.60  57.00  90.00   52
 18  \w    -30.00  21.00   0.50    2.12    --    8.60  77.00  90.00  102
 19  \w    -17.00   9.00   0.50    2.12    --    8.60  57.00  90.00   52
 20  \w    -81.00  45.00   0.50    2.12    --    8.60 -77.00-120.00  252
 21  \w    -55.00  65.00   0.50    2.12    --   32.00 -66.00 108.08  240
 22  \w    112.00 183.00   0.50    8.49    --  100.10  82.00 150.00  142
 23  \w     58.00  83.00   0.50    8.49    --  100.10  82.00 150.00   50
 24  \w     59.00  86.00   0.50    8.49    --  100.10  82.00-180.00   54
 25  \w     54.00 142.00   0.50    8.49    --  100.10 -82.00-150.00  176
 26  \w     17.00 141.00   0.50    8.49    --  100.10 -82.00  90.00  248
 27  \w     58.00  86.00   0.50    8.49    --  100.10  82.00-120.00   56
 28  \w    135.00 189.00   0.50    8.49    --  100.10  82.00  60.00  108
 29  \w     69.00 137.00   0.50    8.49    --  100.10  61.00 -60.00  136
 30  \w     65.00 101.00   0.50    8.49    --  100.10  45.00  90.00   72
 31  \w    126.00 172.00   0.50    8.49    --  100.10  45.00  90.00   92
 32  \w     61.00  87.00   0.50    8.49    --  100.10  77.00  30.00   52
 33  \w     64.00 141.00   0.50    8.49    --  100.10 -82.00 -90.00  154
 34  \w     58.00  90.00   0.50    8.49    --  100.10  82.00  90.00   64
 35  \w     95.00 120.00   0.50    8.49    --  100.10  82.00  90.00   50
 36  \w    144.00 184.00   0.50    8.49    --  100.10  82.00  90.00   80
 37  \w    103.00 185.00   0.50    8.49    --  100.10  82.00 120.00  164
 38  \w     61.00  86.00   0.50    8.49    --  100.10  77.00-150.00   50
 39  \w     58.00  83.00   0.50    8.49    --  100.10  82.00 120.00   50
 40  \w    150.00 176.00   0.50    8.49    --  100.10  82.00 -30.00   52
 41  \w     60.00  86.00   0.50    8.49    --  100.10  82.00 -30.00   52
 42  \w     61.00  87.00   0.50    8.49    --  100.10  77.00   0.00   52
 43  \w     58.00  89.00   0.50    8.49    --  100.10  82.00  60.00   62
 44  \w     65.00 188.00   0.50    8.49    --  100.10  45.00  30.00  246
 45  \w     65.00  98.00   0.50    8.49    --  100.10  45.00 120.00   66
 46  \w    141.00 166.00   0.50    8.49    --  100.10  45.00 120.00   50
 47  \w     58.00  85.00   0.50    8.49    --  100.10  82.00-150.00   54
 48  \w    140.00 187.00   0.50    8.49    --  100.10  45.00 -90.00   94
 49  \w     65.00  91.00   0.50    8.49    --  100.10  45.00 -90.00   52
 50  \w     65.00 100.00   0.50    8.49    --  100.10  45.00 150.00   70
 51  \w     61.00  86.00   0.50    8.49    --  100.10  77.00-180.00   50
 52  \w     61.00  95.00   0.50    8.49    --  100.10  77.00 -30.00   68
 53  \w    115.00 189.00   0.50    8.49    --  100.10  45.00  60.00  148
 54  \w    142.00 189.00   0.50    8.49    --  100.10  61.00 -60.00   94
 55  \w     65.00 188.00   0.50    8.49    --  100.10  45.00 -60.00  246
 56  \w     61.00  91.00   0.50    8.49    --  100.10  77.00 150.00   60
 57  \w     58.00  94.00   0.50    8.49    --  100.10  82.00  30.00   72
 58  \w     58.00  87.00   0.50    8.49    --  100.10  82.00   0.00   58
 59  \w     66.00 189.00   0.50    8.49    --  100.10  45.00-150.00  246
 60  \w    160.00 185.00   0.50    8.49    --  100.10  77.00  30.00   50
 61  \w     39.00  71.00   0.50    8.49    --  100.10 -82.00 120.00   64
 62  \w     74.00 136.00   0.50    8.49    --  100.10 -82.00 120.00  124
 63  \w     65.00  96.00   0.50    8.49    --  100.10  45.00  60.00   62
 64  \w     60.00 142.00   0.50    8.49    --  100.10 -82.00  30.00  164
 65  \w     29.00  54.00   0.50    8.49    --  100.10 -82.00  30.00   50
 66  \w     66.00 170.00   0.50    8.49    --  100.10  45.00-120.00  208
 67  \w     69.00 108.00   0.50    8.49    --  100.10  61.00 150.00   78
 68  \w    130.00 155.00   0.50    8.49    --  100.10  61.00 150.00   50
 69  \w     58.00  84.00   0.50    8.49    --  100.10  82.00 -60.00   52
 70  \w     58.00  84.00   0.50    8.49    --  100.10  82.00 -90.00   52
 71  \w    108.00 133.00   0.50    8.49    --  100.10  82.00-180.00   50
 72  \w     65.00 189.00   0.50    8.49    --  100.10  45.00   0.00  248
;
_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      -0.0169376000
_diffrn_orient_matrix_UB_12      -0.1133535000
_diffrn_orient_matrix_UB_13      -0.0288471000
_diffrn_orient_matrix_UB_21      0.1351647000
_diffrn_orient_matrix_UB_22      -0.0111108000
_diffrn_orient_matrix_UB_23      -0.0560652000
_diffrn_orient_matrix_UB_31      0.0868378000
_diffrn_orient_matrix_UB_32      -0.0818879000
_diffrn_orient_matrix_UB_33      0.0669609000
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0209
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39816
_diffrn_reflns_theta_full        72.6592
_diffrn_reflns_theta_max         72.66
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81658
_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    1.2015
_exptl_crystal_description       block
_exptl_crystal_F_000             718.7782
_exptl_crystal_size_max          0.623
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.4677
_refine_diff_density_min         -0.2963
_refine_diff_density_rms         0.0440
_refine_ls_d_res_high            0.8076
_refine_ls_d_res_low             10.9822
_refine_ls_goodness_of_fit_ref   1.0351
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    84
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7287
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.0261
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0726P)^2^+0.6778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1325
_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              21
_reflns_limit_l_min              0
_reflns_number_gt                6493
_reflns_number_total             7287
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ra05293j2.cif
_cod_data_source_block           yt2_119_180117
_cod_database_code               7231132
_chemical_oxdiff_formula         C48H42Si2
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C6ba \\sim C3ba \\sim C4ba \\sim C5ba: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C48 \\sim C9ba \\sim C45 \\sim C7ba \\sim C47 \\sim C8ba \\sim C30: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6ba) \\sim Ueq, Uanis(C5ba) \\sim Ueq, Uanis(C4ba) \\sim Ueq,
Uanis(C3ba) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9ba) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C7ba) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C8ba) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C30) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: C9ba(0.25) H9ba(0.25) H9bb(0.25) H9bc(0.25) C7ba(0.25) H7ba(0.25)
 H7bb(0.25) H7bc(0.25) C8ba(0.25) H8ba(0.25) H8bb(0.25) H8bc(0.25) C47(0.75)
 H47a(0.75) H47b(0.75) H47c(0.75) C48(0.75) H48a(0.75) H48b(0.75) H48c(0.75)
 C45(0.75) H45a(0.75) H45b(0.75) H45c(0.75) H9ba(0.25) H9bb(0.25) H9bc(0.25)
 H48a(0.75) H48b(0.75) H48c(0.75) H48a(0.75) H48b(0.75) H48c(0.75) H9ba(0.25)
 H9bb(0.25) H9bc(0.25)
4.a Me refined with riding coordinates:
 C48(H48a,H48b,H48c), C9ba(H9ba,H9bb,H9bc)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18), C25(H25), C32(H32), C33(H33), C34(H34), C36(H36),
 C38(H38), C40(H40), C46(H46), C8(H8), C10(H10), C5aa(H5aa), C27(H27), C1(H1),
 C2(H2), C6aa(H6aa), C7aa(H7aa), C9aa(H9aa), C8aa(H8aa), C9(H9), C0ba(H0ba),
 C11(H11), C2ba(H2ba)
4.c Idealised Me refined as rotating group:
 C4ba(H4ba,H4bb,H4bc), C6ba(H6ba,H6bb,H6bc), C5ba(H5ba,H5bb,H5bc), C45(H45a,
 H45b,H45c), C47(H47a,H47b,H47c), C7ba(H7ba,H7bb,H7bc), C8ba(H8ba,H8bb,H8bc)
;
_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 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.678