Synthesis, Structure, and Isomerization of Decapentynylcorannulene: Enediyne Cyclization/Interconversion of C40R10 Isomers
Tomoharu Hayama; Yao-Ting Wu; Anthony Linden; Kim K. Baldridge; Jay S. Siegel; Journal of the American Chemical Society 129 (2007) 12612–12613; doi:10.1021/ja074403b

data_4110038
_publ_contact_author_address
; Institute of Organic Chemistry
   University of Z\"urich
   Winterthurerstrasse 190
   CH-8057 Z\"urich
   Switzerland
;
_publ_contact_author_email       alinden@oci.uzh.ch
_publ_contact_author_fax         '41 44 635 6812'
_publ_contact_author_name        'Dr. Anthony Linden'
_publ_contact_author_phone       '41 44 635 4228'
_publ_section_title
;
 Synthesis, Structure, and Isomerization of Decapentynylcorannulene:
 Enediyne Cyclization/Interconversion of C40R10 Isomers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12612
_journal_page_last               12613
_journal_paper_doi               10.1021/ja074403b
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C70 H70'
_chemical_formula_sum            'C70 H70'
_chemical_formula_weight         911.32
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-06-11
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.436(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   35.385(1)
_cell_length_b                   19.860(1)
_cell_length_c                   22.686(1)
_cell_measurement_reflns_used    177867
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      1.28
_cell_volume                     15842.0(12)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Swiss Light Source PX6 beamline software'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD detector'
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'MarResearch 225 CCD detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.775
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            177867
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.28
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0642
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             5880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0113(14)
_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   2.031
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5049
_refine_ls_number_reflns         26090
_refine_ls_number_restraints     28418
_refine_ls_restrained_S_all      1.899
_refine_ls_R_factor_all          0.1493
_refine_ls_R_factor_gt           0.1242
_refine_ls_shift/su_max          0.508
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.16P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3547
_refine_ls_wR_factor_ref         0.3785
_reflns_number_gt                18177
_reflns_number_total             26090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja074403brom20070617_020300.cif
_cod_data_source_block           6
_cod_database_code               4110038