#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:00:41 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180460 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/29/7212992.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7212992
loop_
_publ_author_name
'Sawada, Tsuyoshi'
'Wakabayashi, Masaki'
'Takeo, Hiromi'
'Miyazawa, Akira'
'Tashiro, Masashi'
'Thiemann, Thies'
'Mataka, Shuntaro'
_publ_section_title
;
 Novel, strained 10b,10c-dihydropyrenes bearing bulky TMSCH2 groups at the
 internal positions
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              403
_journal_paper_doi               10.1039/a809561b
_journal_year                    1999
_chemical_formula_moiety         'C32 H48 Si2'
_chemical_formula_sum            'C32 H48 Si2'
_chemical_formula_weight         488.88
_chemical_melting_point          156.5(5)
_chemical_name_common            'dihydropyrene 9a'
_chemical_name_systematic
; 
2,7-di-tert-butyl-10b,10c-bis(trimethylsilylmethyl)-trans-10b,10c-dihydropyrene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                115.500(10)
_cell_angle_beta                 97.540(10)
_cell_angle_gamma                89.190(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5370(10)
_cell_length_b                   9.828(2)
_cell_length_c                   9.0900(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      43
_cell_measurement_theta_min      16
_cell_volume                     761.5(2)
_computing_cell_refinement       'CAD4 Enraf-Nonius software'
_computing_data_collection       'CAD4 Enraf-Nonius software'
_computing_data_reduction        'MolEN  Enraf-Nonius software'
_computing_molecular_graphics    'Xtal_GX (Hall & Boulay, 1995)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
;SIR92 (Altomare, Burla, Camalli, Cascarano, Giacovazzo,
Guagliardi & Polidori, 1994) 
;
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2760
_diffrn_reflns_theta_max         64.94
_diffrn_reflns_theta_min         4.68
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_correction_T_min  0.9455
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep brown'
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .302
_refine_diff_density_min         -.427
_refine_diff_density_rms         .048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.0594P)²+0.5201P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1265
_refine_ls_wR_factor_obs         0.1171
_reflns_number_observed          2165
_reflns_number_total             2592
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809561bsup1.cif
_cod_data_source_block           9a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '156-157' was changed to '156.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0594P)^2^+0.5201P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0594P)^2^+0.5201P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7212992
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
C01 C 0.2654(2) 0.8390(2) 0.8693(2) 0.0292(5) Uani 1 d .
H01 H 0.3544(2) 0.8530(2) 0.8453(2) 0.038 Uiso 1 calc R
C02 C 0.2142(2) 0.6917(2) 0.8225(3) 0.0302(5) Uani 1 d .
C03 C 0.0766(2) 0.6689(2) 0.8507(3) 0.0304(5) Uani 1 d .
H03 H 0.0409(2) 0.5705(2) 0.8141(3) 0.040 Uiso 1 calc R
C03A C -0.0078(2) 0.7864(2) 0.9303(2) 0.0259(4) Uani 1 d .
C09 C 0.1490(2) 1.2339(2) 1.0521(3) 0.0300(5) Uani 1 d .
H09 H 0.1869(2) 1.3312(2) 1.0870(3) 0.039 Uiso 1 calc R
C10B C 0.0556(2) 0.9467(2) 1.0136(2) 0.0230(4) Uani 1 d .
C10 C 0.2336(2) 1.1121(2) 0.9837(3) 0.0291(5) Uani 1 d .
H10 H 0.3218(2) 1.1290(2) 0.9599(3) 0.038 Uiso 1 calc R
C10A C 0.1902(2) 0.9653(2) 0.9497(2) 0.0250(4) Uani 1 d .
C11 C 0.2995(2) 0.5528(2) 0.7342(3) 0.0393(6) Uani 1 d .
C12 C 0.3109(3) 0.4552(3) 0.8282(3) 0.0569(8) Uani 1 d .
H12A H 0.2177(3) 0.4260(3) 0.8365(3) 0.074 Uiso 1 calc R
H12B H 0.3612(3) 0.5117(3) 0.9366(3) 0.074 Uiso 1 calc R
H12C H 0.3610(3) 0.3666(3) 0.7706(3) 0.074 Uiso 1 calc R
C13 C 0.2242(3) 0.4604(3) 0.5595(3) 0.0520(7) Uani 1 d .
H13A H 0.1296(3) 0.4321(3) 0.5642(3) 0.068 Uiso 1 calc R
H13B H 0.2750(3) 0.3713(3) 0.5059(3) 0.068 Uiso 1 calc R
H13C H 0.2208(3) 0.5199(3) 0.4987(3) 0.068 Uiso 1 calc R
C14 C 0.4494(3) 0.5966(3) 0.7239(5) 0.0721(10) Uani 1 d .
H14A H 0.4979(3) 0.6548(3) 0.8329(5) 0.094 Uiso 1 calc R
H14B H 0.4452(3) 0.6557(3) 0.6625(5) 0.094 Uiso 1 calc R
H14C H 0.4994(3) 0.5070(3) 0.6698(5) 0.094 Uiso 1 calc R
C19 C 0.0929(2) 0.9927(2) 1.2029(2) 0.0264(4) Uani 1 d .
H19A H 0.0031(2) 0.9935(2) 1.2426(2) 0.034 Uiso 1 calc R
H19B H 0.1288(2) 1.0968(2) 1.2520(2) 0.034 Uiso 1 calc R
C20 C 0.1486(4) 0.6994(3) 1.2509(4) 0.0672(9) Uani 1 d .
H20A H 0.0530(4) 0.7029(3) 1.2742(4) 0.087 Uiso 1 calc R
H20B H 0.2072(4) 0.6608(3) 1.3172(4) 0.087 Uiso 1 calc R
H20C H 0.1512(4) 0.6347(3) 1.1366(4) 0.087 Uiso 1 calc R
C21 C 0.4006(3) 0.8913(4) 1.2553(3) 0.0619(8) Uani 1 d .
H21A H 0.4032(3) 0.8322(4) 1.1398(3) 0.080 Uiso 1 calc R
H21B H 0.4590(3) 0.8478(4) 1.3168(3) 0.080 Uiso 1 calc R
H21C H 0.4353(3) 0.9926(4) 1.2868(3) 0.080 Uiso 1 calc R
C22 C 0.2167(3) 1.0099(3) 1.5244(3) 0.0463(6) Uani 1 d .
H22A H 0.1220(3) 1.0131(3) 1.5504(3) 0.060 Uiso 1 calc R
H22B H 0.2524(3) 1.1106(3) 1.5545(3) 0.060 Uiso 1 calc R
H22C H 0.2761(3) 0.9658(3) 1.5844(3) 0.060 Uiso 1 calc R
Si01 Si 0.21600(6) 0.89386(7) 1.29894(7) 0.0318(2) Uani 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si .2541 .3302 'International Tables 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_site_symmetry_1
_geom_angle_site_symmetry_3
C10A C01 C02 123.3(2) . .
C01 C02 C03 118.7(2) . .
C01 C02 C11 122.6(2) . .
C03 C02 C11 118.6(2) . .
C03A C03 C02 122.9(2) . .
C03 C03A C09 123.7(2) . 2_577
C03 C03A C10B 119.3(2) . .
C09 C03A C10B 116.8(2) 2_577 .
C10 C09 C03A 121.7(2) . 2_577
C03A C10B C10A 113.2(2) . .
C03A C10B C10B 108.8(2) . 2_577
C10A C10B C10B 109.0(2) . 2_577
C03A C10B C19 108.5(2) . .
C10A C10B C19 108.0(2) . .
C10B C10B C19 109.4(2) 2_577 .
C09 C10 C10A 122.0(2) . .
C01 C10A C10 124.0(2) . .
C01 C10A C10B 119.1(2) . .
C10 C10A C10B 116.8(2) . .
C14 C11 C13 108.6(2) . .
C14 C11 C12 107.8(2) . .
C13 C11 C12 109.3(2) . .
C14 C11 C02 112.1(2) . .
C13 C11 C02 109.4(2) . .
C12 C11 C02 109.6(2) . .
C10B C19 Si01 125.93(14) . .
C21 Si01 C22 107.79(12) . .
C21 Si01 C20 110.6(2) . .
C22 Si01 C20 106.93(14) . .
C21 Si01 C19 114.23(12) . .
C22 Si01 C19 103.55(10) . .
C20 Si01 C19 113.07(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C01 C10A 1.386(3) .
C01 C02 1.396(3) .
C02 C03 1.409(3) .
C02 C11 1.538(3) .
C03 C03A 1.383(3) .
C03A C09 1.404(3) 2_577
C03A C10B 1.517(3) .
C09 C10 1.390(3) .
C09 C03A 1.404(3) 2_577
C10B C10A 1.520(3) .
C10B C10B 1.551(4) 2_577
C10B C19 1.571(3) .
C10 C10A 1.396(3) .
C11 C14 1.525(4) .
C11 C13 1.530(3) .
C11 C12 1.530(4) .
C19 Si01 1.874(2) .
C20 Si01 1.870(3) .
C21 Si01 1.852(3) .
C22 Si01 1.867(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C10A C01 C02 C03 3.2(3) . .
C10A C01 C02 C11 -179.6(2) . .
C01 C02 C03 C03A -3.4(3) . .
C11 C02 C03 C03A 179.4(2) . .
C02 C03 C03A C09 174.7(2) . 2_577
C02 C03 C03A C10B -9.3(3) . .
C03 C03A C10B C10A 20.3(2) . .
C09 C03A C10B C10A -163.4(2) 2_577 .
C03 C03A C10B C10B 141.6(2) . 2_577
C09 C03A C10B C10B -42.1(3) 2_577 2_577
C03 C03A C10B C19 -99.5(2) . .
C09 C03A C10B C19 76.8(2) 2_577 .
C03A C09 C10 C10A -9.0(3) 2_577 .
C02 C01 C10A C10 -173.8(2) . .
C02 C01 C10A C10B 9.5(3) . .
C09 C10 C10A C01 174.4(2) . .
C09 C10 C10A C10B -8.8(3) . .
C03A C10B C10A C01 -20.4(2) . .
C10B C10B C10A C01 -141.6(2) 2_577 .
C19 C10B C10A C01 99.7(2) . .
C03A C10B C10A C10 162.6(2) . .
C10B C10B C10A C10 41.4(3) 2_577 .
C19 C10B C10A C10 -77.3(2) . .
C01 C02 C11 C14 6.8(3) . .
C03 C02 C11 C14 -176.0(2) . .
C01 C02 C11 C13 -113.7(2) . .
C03 C02 C11 C13 63.5(3) . .
C01 C02 C11 C12 126.5(2) . .
C03 C02 C11 C12 -56.4(3) . .
C03A C10B C19 Si01 58.8(2) . .
C10A C10B C19 Si01 -64.2(2) . .
C10B C10B C19 Si01 177.3(2) 2_577 .
C10B C19 Si01 C21 61.0(2) . .
C10B C19 Si01 C22 178.0(2) . .
C10B C19 Si01 C20 -66.7(2) . .
