#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:06:21 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178680 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/91/4079179.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4079179
loop_
_publ_author_name
'Tanabe, Makoto'
'Yumoto, Ryouhei'
'Osakada, Kohtaro'
'Sanji, Takanobu'
'Tanaka, Masato'
_publ_section_title
;
 Preparation and Properties of Perarylated 3,4-Disila-1,5-hexadienes. A
 Fluorescent Disilane Accommodated in the Crystal Lattice
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6787
_journal_paper_doi               10.1021/om300551t
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C70 H54 N4 Si2'
_chemical_formula_sum            'C70 H54 N4 Si2'
_chemical_formula_weight         1007.39
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                103.954(5)
_cell_angle_beta                 94.733(4)
_cell_angle_gamma                105.892(5)
_cell_formula_units_Z            1
_cell_length_a                   9.504(4)
_cell_length_b                   12.433(5)
_cell_length_c                   12.806(5)
_cell_measurement_reflns_used    3852
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.26
_cell_volume                     1394.4(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11139
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             530.00
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.52
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.550
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.343
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6063
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1023P)²+0.1592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2392
_reflns_number_gt                4185
_reflns_number_total             6063
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            om300551t_si_001.cif
_cod_data_source_block           compound4f
_cod_database_code               4079179
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.12394(7) 0.00094(6) 0.48812(5) 0.0280(3) Uani 1.0 2 d .
N1 N -0.3669(4) -0.0832(3) -0.0738(3) 0.0771(12) Uani 1.0 2 d .
N2 N 0.4535(6) -0.4270(4) -0.1206(3) 0.0950(14) Uani 1.0 2 d .
C1 C 0.1311(3) -0.0846(3) 0.3453(2) 0.0316(6) Uani 1.0 2 d .
C2 C 0.2309(3) -0.1442(3) 0.3325(2) 0.0327(6) Uani 1.0 2 d .
C3 C 0.0284(3) -0.0831(3) 0.2515(2) 0.0308(6) Uani 1.0 2 d .
C4 C 0.0257(3) 0.0212(3) 0.2301(2) 0.0349(7) Uani 1.0 2 d .
C5 C -0.0731(3) 0.0222(3) 0.1450(3) 0.0390(7) Uani 1.0 2 d .
C6 C -0.1747(4) -0.0815(3) 0.0819(3) 0.0402(7) Uani 1.0 2 d .
C7 C -0.1747(4) -0.1868(3) 0.1017(3) 0.0428(7) Uani 1.0 2 d .
C8 C -0.0723(4) -0.1868(3) 0.1854(3) 0.0380(7) Uani 1.0 2 d .
C9 C -0.2828(4) -0.0812(4) -0.0046(3) 0.0531(9) Uani 1.0 2 d .
C10 C 0.2738(3) -0.2038(3) 0.2319(2) 0.0296(6) Uani 1.0 2 d .
C11 C 0.2615(3) -0.1739(3) 0.1342(3) 0.0359(7) Uani 1.0 2 d .
C12 C 0.3101(4) -0.2302(3) 0.0441(3) 0.0438(8) Uani 1.0 2 d .
C13 C 0.3706(4) -0.3185(3) 0.0498(3) 0.0429(7) Uani 1.0 2 d .
C14 C 0.3860(4) -0.3489(3) 0.1466(3) 0.0457(8) Uani 1.0 2 d .
C15 C 0.3393(3) -0.2906(3) 0.2371(3) 0.0393(7) Uani 1.0 2 d .
C16 C 0.4180(5) -0.3785(4) -0.0458(3) 0.0626(11) Uani 1.0 2 d .
C17 C 0.2042(3) -0.0648(3) 0.5875(2) 0.0299(6) Uani 1.0 2 d .
C18 C 0.1382(3) -0.1799(3) 0.5884(3) 0.0360(7) Uani 1.0 2 d .
C19 C 0.1978(3) -0.2297(3) 0.6610(3) 0.0388(7) Uani 1.0 2 d .
C20 C 0.3274(3) -0.1636(3) 0.7332(3) 0.0367(7) Uani 1.0 2 d .
C21 C 0.3918(3) -0.0503(3) 0.7342(3) 0.0391(7) Uani 1.0 2 d .
C22 C 0.3322(3) -0.0006(3) 0.6625(3) 0.0338(6) Uani 1.0 2 d .
C23 C 0.2478(3) 0.1545(3) 0.5107(2) 0.0316(6) Uani 1.0 2 d .
C24 C 0.3729(4) 0.1786(3) 0.4602(3) 0.0465(8) Uani 1.0 2 d .
C25 C 0.4709(4) 0.2898(4) 0.4860(4) 0.0548(9) Uani 1.0 2 d .
C26 C 0.4505(4) 0.3783(3) 0.5622(3) 0.0494(9) Uani 1.0 2 d .
C27 C 0.3277(4) 0.3593(3) 0.6140(3) 0.0473(8) Uani 1.0 2 d .
C28 C 0.2267(4) 0.2476(3) 0.5868(3) 0.0399(7) Uani 1.0 2 d .
C29 C -0.0485(15) 0.5021(13) 0.1126(12) 0.322(9) Uani 1.0 2 d .
C30 C 0.0167(9) 0.4692(6) 0.1931(7) 0.120(3) Uani 1.0 2 d .
C31 C 0.0748(7) 0.3894(6) 0.1641(5) 0.1028(18) Uani 1.0 2 d .
C32 C 0.1603(6) 0.3686(7) 0.2407(6) 0.124(3) Uani 1.0 2 d .
C33 C 0.1710(7) 0.4175(10) 0.3477(8) 0.160(4) Uani 1.0 2 d .
C34 C 0.1057(14) 0.5022(9) 0.3805(8) 0.185(5) Uani 1.0 2 d .
C35 C 0.0225(9) 0.5270(6) 0.2993(9) 0.139(3) Uani 1.0 2 d .
H1 H 0.2807 -0.1482 0.3982 0.0392 Uiso 1.0 2 calc R
H2 H 0.0927 0.0925 0.2745 0.0419 Uiso 1.0 2 calc R
H3 H -0.0716 0.0935 0.1297 0.0468 Uiso 1.0 2 calc R
H4 H -0.2439 -0.2577 0.0585 0.0513 Uiso 1.0 2 calc R
H5 H -0.0705 -0.2586 0.1981 0.0456 Uiso 1.0 2 calc R
H6 H 0.2191 -0.1140 0.1295 0.0430 Uiso 1.0 2 calc R
H7 H 0.3021 -0.2084 -0.0218 0.0525 Uiso 1.0 2 calc R
H8 H 0.4282 -0.4091 0.1508 0.0548 Uiso 1.0 2 calc R
H9 H 0.3520 -0.3100 0.3039 0.0471 Uiso 1.0 2 calc R
H10 H 0.0507 -0.2254 0.5383 0.0432 Uiso 1.0 2 calc R
H11 H 0.1505 -0.3076 0.6610 0.0466 Uiso 1.0 2 calc R
H12 H 0.3709 -0.1969 0.7817 0.0440 Uiso 1.0 2 calc R
H13 H 0.4788 -0.0049 0.7849 0.0470 Uiso 1.0 2 calc R
H14 H 0.3790 0.0781 0.6646 0.0406 Uiso 1.0 2 calc R
H15 H 0.3911 0.1178 0.4075 0.0558 Uiso 1.0 2 calc R
H16 H 0.5543 0.3044 0.4495 0.0658 Uiso 1.0 2 calc R
H17 H 0.5206 0.4536 0.5800 0.0593 Uiso 1.0 2 calc R
H18 H 0.3121 0.4210 0.6672 0.0568 Uiso 1.0 2 calc R
H19 H 0.1412 0.2347 0.6211 0.0479 Uiso 1.0 2 calc R
H20 H -0.0772 0.4381 0.0454 0.3864 Uiso 1.0 2 calc R
H21 H 0.0216 0.5702 0.0999 0.3864 Uiso 1.0 2 calc R
H22 H -0.1368 0.5219 0.1344 0.3864 Uiso 1.0 2 calc R
H23 H 0.0586 0.3452 0.0901 0.1234 Uiso 1.0 2 calc R
H24 H 0.2160 0.3168 0.2182 0.1488 Uiso 1.0 2 calc R
H25 H 0.2231 0.3934 0.3998 0.1914 Uiso 1.0 2 calc R
H26 H 0.1164 0.5426 0.4552 0.2225 Uiso 1.0 2 calc R
H27 H -0.0289 0.5829 0.3176 0.1666 Uiso 1.0 2 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Si Si 0.0817 0.0704
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
Si1 Si1 C1 111.53(9) yes 2_556
Si1 Si1 C17 111.00(9) yes 2_556
Si1 Si1 C23 110.76(10) yes 2_556
C1 Si1 C17 107.83(14) yes .
C1 Si1 C23 107.53(13) yes .
C17 Si1 C23 108.03(12) yes .
Si1 C1 C2 118.3(2) yes .
Si1 C1 C3 119.3(3) yes .
C2 C1 C3 122.4(3) yes .
C1 C2 C10 129.6(3) yes .
C1 C3 C4 121.2(2) yes .
C1 C3 C8 120.4(3) yes .
C4 C3 C8 118.4(3) yes .
C3 C4 C5 120.9(3) yes .
C4 C5 C6 119.8(4) yes .
C5 C6 C7 120.5(3) yes .
C5 C6 C9 120.4(4) yes .
C7 C6 C9 119.1(3) yes .
C6 C7 C8 119.1(3) yes .
C3 C8 C7 121.3(4) yes .
N1 C9 C6 178.4(5) yes .
C2 C10 C11 123.9(3) yes .
C2 C10 C15 117.7(3) yes .
C11 C10 C15 118.3(3) yes .
C10 C11 C12 120.8(4) yes .
C11 C12 C13 120.0(4) yes .
C12 C13 C14 120.3(3) yes .
C12 C13 C16 119.4(4) yes .
C14 C13 C16 120.3(4) yes .
C13 C14 C15 119.3(4) yes .
C10 C15 C14 121.2(4) yes .
N2 C16 C13 179.0(5) yes .
Si1 C17 C18 121.33(19) yes .
Si1 C17 C22 121.1(3) yes .
C18 C17 C22 117.5(3) yes .
C17 C18 C19 121.7(3) yes .
C18 C19 C20 119.1(3) yes .
C19 C20 C21 119.7(3) yes .
C20 C21 C22 121.2(3) yes .
C17 C22 C21 120.7(3) yes .
Si1 C23 C24 121.5(3) yes .
Si1 C23 C28 121.3(3) yes .
C24 C23 C28 116.8(3) yes .
C23 C24 C25 120.9(3) yes .
C24 C25 C26 121.4(4) yes .
C25 C26 C27 120.0(3) yes .
C26 C27 C28 118.9(3) yes .
C23 C28 C27 122.0(3) yes .
C29 C30 C31 117.0(9) yes .
C29 C30 C35 119.2(10) yes .
C31 C30 C35 123.7(9) yes .
C30 C31 C32 118.0(7) yes .
C31 C32 C33 123.2(8) yes .
C32 C33 C34 118.9(10) yes .
C33 C34 C35 117.0(9) yes .
C30 C35 C34 118.5(9) yes .
C1 C2 H1 115.187 no .
C10 C2 H1 115.185 no .
C3 C4 H2 119.566 no .
C5 C4 H2 119.558 no .
C4 C5 H3 120.093 no .
C6 C5 H3 120.093 no .
C6 C7 H4 120.465 no .
C8 C7 H4 120.454 no .
C3 C8 H5 119.349 no .
C7 C8 H5 119.339 no .
C10 C11 H6 119.574 no .
C12 C11 H6 119.586 no .
C11 C12 H7 119.986 no .
C13 C12 H7 119.989 no .
C13 C14 H8 120.341 no .
C15 C14 H8 120.351 no .
C10 C15 H9 119.386 no .
C14 C15 H9 119.382 no .
C17 C18 H10 119.146 no .
C19 C18 H10 119.138 no .
C18 C19 H11 120.445 no .
C20 C19 H11 120.439 no .
C19 C20 H12 120.157 no .
C21 C20 H12 120.156 no .
C20 C21 H13 119.406 no .
C22 C21 H13 119.411 no .
C17 C22 H14 119.636 no .
C21 C22 H14 119.630 no .
C23 C24 H15 119.566 no .
C25 C24 H15 119.567 no .
C24 C25 H16 119.320 no .
C26 C25 H16 119.321 no .
C25 C26 H17 119.997 no .
C27 C26 H17 119.982 no .
C26 C27 H18 120.559 no .
C28 C27 H18 120.552 no .
C23 C28 H19 119.014 no .
C27 C28 H19 119.009 no .
C30 C29 H20 109.470 no .
C30 C29 H21 109.473 no .
C30 C29 H22 109.476 no .
H20 C29 H21 109.466 no .
H20 C29 H22 109.472 no .
H21 C29 H22 109.470 no .
C30 C31 H23 120.998 no .
C32 C31 H23 120.999 no .
C31 C32 H24 118.382 no .
C33 C32 H24 118.378 no .
C32 C33 H25 120.563 no .
C34 C33 H25 120.569 no .
C33 C34 H26 121.478 no .
C35 C34 H26 121.476 no .
C30 C35 H27 120.734 no .
C34 C35 H27 120.734 no .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Si1 Si1 2.3946(14) yes 2_556
Si1 C1 1.899(3) yes .
Si1 C17 1.885(4) yes .
Si1 C23 1.888(3) yes .
N1 C9 1.135(6) yes .
N2 C16 1.133(6) yes .
C1 C2 1.351(5) yes .
C1 C3 1.490(4) yes .
C2 C10 1.472(4) yes .
C3 C4 1.395(5) yes .
C3 C8 1.400(4) yes .
C4 C5 1.384(5) yes .
C5 C6 1.391(4) yes .
C6 C7 1.392(6) yes .
C6 C9 1.449(5) yes .
C7 C8 1.388(5) yes .
C10 C11 1.394(5) yes .
C10 C15 1.397(5) yes .
C11 C12 1.383(5) yes .
C12 C13 1.385(6) yes .
C13 C14 1.388(5) yes .
C13 C16 1.447(6) yes .
C14 C15 1.386(5) yes .
C17 C18 1.400(4) yes .
C17 C22 1.395(4) yes .
C18 C19 1.396(5) yes .
C19 C20 1.393(4) yes .
C20 C21 1.371(5) yes .
C21 C22 1.388(5) yes .
C23 C24 1.395(5) yes .
C23 C28 1.394(4) yes .
C24 C25 1.383(5) yes .
C25 C26 1.353(6) yes .
C26 C27 1.382(5) yes .
C27 C28 1.397(4) yes .
C29 C30 1.361(19) yes .
C30 C31 1.259(11) yes .
C30 C35 1.365(13) yes .
C31 C32 1.339(11) yes .
C32 C33 1.341(12) yes .
C33 C34 1.363(17) yes .
C34 C35 1.399(16) yes .
C2 H1 0.950 no .
C4 H2 0.950 no .
C5 H3 0.950 no .
C7 H4 0.950 no .
C8 H5 0.950 no .
C11 H6 0.950 no .
C12 H7 0.950 no .
C14 H8 0.950 no .
C15 H9 0.950 no .
C18 H10 0.950 no .
C19 H11 0.950 no .
C20 H12 0.950 no .
C21 H13 0.950 no .
C22 H14 0.950 no .
C24 H15 0.950 no .
C25 H16 0.950 no .
C26 H17 0.950 no .
C27 H18 0.950 no .
C28 H19 0.950 no .
C29 H20 0.980 no .
C29 H21 0.980 no .
C29 H22 0.980 no .
C31 H23 0.950 no .
C32 H24 0.950 no .
C33 H25 0.950 no .
C34 H26 0.950 no .
C35 H27 0.950 no .
