Metal-Mediated Efficient Synthesis, Structural Characterization, and Skeletal Rearrangement of Octasubstituted Semibullvalenes
Chao Wang; Jian Yuan; Guotao Li; Zitao Wang; Shiwei Zhang; Zhenfeng Xi; Journal of the American Chemical Society 128 (2006) 4564–4565; doi:10.1021/ja0579208

data_4110514
_publ_section_title
;
 Metal-Mediated Efficient Synthesis, Structural Characterization, and
 Skeletal Rearrangement of Octasubstituted Semibullvalenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4564
_journal_page_last               4565
_journal_paper_doi               10.1021/ja0579208
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C36 H32'
_chemical_formula_weight         464.62
_chemical_name_systematic
; 
 ? 
;
_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
;
                                  hydrogen atoms are generated by HFIX
                                  instructions
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.66(3)
_cell_angle_beta                 79.32(3)
_cell_angle_gamma                66.81(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7357(19)
_cell_length_b                   10.937(2)
_cell_length_c                   14.409(3)
_cell_measurement_reflns_used    11772
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.09
_cell_volume                     1342.2(6)
_computing_cell_refinement
;
                                   Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   MSC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381 USA.
;
_computing_data_collection
;
                                   Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   SC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381, USA.
;
_computing_data_reduction
;
                                   Sheldrick, G. M. (1998) SHELXS98, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.
;
_computing_molecular_graphics
;
                                   Interactive Molecular Graphics XP, Virsion
                                   4.2 for MSDOS (1990), Siemens Analytical
                                   X-ray Instruments Inc., Madison, Wisconsin,
                                   USA.
;
_computing_publication_material
;
                                   Sheldrick, G. M. (1998) SHELXL98, Program
                                   for the refinement of Crystal Structure,
                                   University of Gottingen, Germany.
;
_computing_structure_refinement
;
                                   Sheldrick, G. M. (1998) SHELXL98, Program
                                   for the Refinement of Crystal Structure,
                                   University of Gottingen, Germany.
;
_computing_structure_solution
;
                                   Sheldrick, G. M. (1998) SHELXS98, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11772
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       Block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.052(5)
_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   1.199
_refine_ls_hydrogen_treatment
;
                                  hydrogen coordinates ride on the coordinates
                                  of the previous atom, the isotropic U values
                                  are 1.2 OR 1.5 time over the U values of the
                                  previous atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                2441
_reflns_number_total             4601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0579208si20051122_050924.cif
_cod_data_source_block           4e
_cod_original_cell_volume        1342.1(5)
_cod_database_code               4110514