Photoisomerization of Perfluoroaryltetrahedranes to Perfluoroarylcyclobutadienes
Yusuke Inagaki; Masaaki Nakamoto; Akira Sekiguchi; Journal of the American Chemical Society 133 (2011) 16436–16439; doi:10.1021/ja208354x

data_4106979
_publ_section_title
;
 Photoisomerization of Perfluoroaryltetrahedranes to
 Perfluoroarylcyclobutadienes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16436
_journal_page_last               16439
_journal_paper_doi               10.1021/ja208354x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C19 H27 F5 Si3'
_chemical_formula_weight         434.68
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4100(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.2242(15)
_cell_length_b                   10.3105(4)
_cell_length_c                   11.7769(5)
_cell_measurement_reflns_used    7319
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.54
_cell_volume                     4633.2(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11916
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.9060
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7711
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.0620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                7450
_reflns_number_total             7711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208354x_si_001.cif
_cod_data_source_block           cbc6f5_0m
_cod_database_code               4106979