Novel, strained 10b,10c-dihydropyrenes bearing bulky TMSCH2 groups at the internal positions
Sawada, Tsuyoshi; Wakabayashi, Masaki; Takeo, Hiromi; Miyazawa, Akira; Tashiro, Masashi; Thiemann, Thies; Mataka, Shuntaro; Journal of the Chemical Society, Perkin Transactions 1  (1999) 403–; doi:10.1039/a809561b

data_7212993
_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         'C29 H40 Si1'
_chemical_formula_sum            'C29 H40 Si'
_chemical_formula_weight         416.70
_chemical_melting_point          146.0(10)
_chemical_name_common            'dihydropyrene 9b'
_chemical_name_systematic
; 
2,7-di-tert-butyl-10b-methyl-10c-trimethylsilylmethyl-trans-10b,
10c-dihydropyrene  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.23(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.586(18)
_cell_length_b                   13.153(6)
_cell_length_c                   19.186(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      38
_cell_measurement_theta_min      21
_cell_volume                     5187(6)
_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      296(2)
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuKa
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1637
_diffrn_reflns_av_sigmaI/netI    0.3486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6077
_diffrn_reflns_theta_max         52.38
_diffrn_reflns_theta_min         3.99
_diffrn_standards_decay_%        -0.01
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep brown'
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         .341
_refine_diff_density_min         -.336
_refine_diff_density_rms         .071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.002
_refine_ls_goodness_of_fit_obs   1.271
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         5873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_restrained_S_obs      1.271
_refine_ls_R_factor_all          0.3566
_refine_ls_R_factor_obs          0.0917
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3669
_refine_ls_wR_factor_obs         0.2042
_reflns_number_observed          1491
_reflns_number_total             5876
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809561bsup1.cif
_cod_data_source_block           9b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '145-147' was changed to '146.0(10)'
- 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:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1311P)^2^+0.0000P] 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^)+( 0.1311P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5186.7(56)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C29 H40 Si1'
_cod_database_code               7212993