Revisit of the Dessy-White Intramolecular Acetylene-Acetylene [2 + 2] Cycloadditions
Chung-Chieh Lee; Man-kit Leung; Gene-Hsiang Lee; Yi-Hung Liu; Shie-Ming Peng; Journal of Organic Chemistry 71 (2006) 8417–8423; doi:10.1021/jo061334v

data_4022037
_publ_section_title
;
 Revisit of the Dessy-White Intramolecular
 Acetylene-Acetylene [2 + 2] Cycloadditions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8417
_journal_page_last               8423
_journal_paper_doi               10.1021/jo061334v
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C60 H42 O4'
_chemical_formula_weight         826.94
_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                94.876(3)
_cell_angle_beta                 100.979(2)
_cell_angle_gamma                91.852(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6082(6)
_cell_length_b                   11.9869(5)
_cell_length_c                   16.3251(8)
_cell_measurement_temperature    295(2)
_cell_volume                     2219.20(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.1029
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13562
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0040(11)
_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   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         7792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1549
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0719P)^2^+0.2840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1830
_reflns_number_gt                3848
_reflns_number_total             7792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061334vsi20060628_063858.cif
_cod_database_code               4022037