Reaction of cyclotrisilene with phenylacetylene: an unusual product with a bicyclo[3.2.0]hepta-3,6-diene skeleton
Ichinohe, Masaaki; Matsuno, Tadahiro; Sekiguchi, Akira; Chemical Communications  (2001) 183–; doi:10.1039/b008375p

data_7111171
_publ_section_title
;
 Reaction of cyclotrisilene with phenylacetylene: an unusual product with
 a bicyclo[3.2.0]hepta-3,6-diene skeleton
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              183
_journal_paper_doi               10.1039/b008375p
_journal_year                    2001
_chemical_formula_sum            'C52 H96 Si7'
_chemical_formula_weight         917.92
_chemical_name_systematic
;
  1,2,2,5-tetrakis[di-tert-butyl(methyl)silyl]-4,7-diphenyl-
  1,2,5-trisilabicyclo[4.2.0]hepta-3,6-diene
;
_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-97
_cell_angle_alpha                99.765(3)
_cell_angle_beta                 114.847(3)
_cell_angle_gamma                92.241(3)
_cell_formula_units_Z            2
_cell_length_a                   13.7380(8)
_cell_length_b                   14.6250(9)
_cell_length_c                   15.751(1)
_cell_measurement_reflns_used    26823
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.12
_cell_volume                     2808.5(3)
_computing_cell_refinement       Scalepack
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device       'Mac Science DIP2030 Image plate'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.04762
_diffrn_orient_matrix_UB_12      0.04807
_diffrn_orient_matrix_UB_13      0.04390
_diffrn_orient_matrix_UB_21      -0.01647
_diffrn_orient_matrix_UB_22      -0.02639
_diffrn_orient_matrix_UB_23      0.06238
_diffrn_orient_matrix_UB_31      0.06207
_diffrn_orient_matrix_UB_32      -0.02849
_diffrn_orient_matrix_UB_33      0.02066
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26823
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Cube
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.578
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0211(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         12169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+4.4780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1851
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                10097
_reflns_number_total             12169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008375psup1.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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 
;
_cod_original_sg_symbol_H-M      'P -1          '
_cod_database_code               7111171