C1-C5 Photochemical Cyclization of Enediynes
Igor V. Alabugin; Serguei V. Kovalenko; Journal of the American Chemical Society 124 (2002) 9052–9053; doi:10.1021/ja026630d

data_4115007
_publ_section_title
;
 C1-C5 Photochemical Cyclization of Enediynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9052
_journal_page_last               9053
_journal_paper_doi               10.1021/ja026630d
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C22 H12 F8 N2'
_chemical_formula_sum            'C22 H12 F8 N2'
_chemical_formula_weight         456.34
_chemical_melting_point          400(1)
_chemical_name_common            'Indene 3c '
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 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                 107.488(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.133(3)
_cell_length_b                   8.1435(12)
_cell_length_c                   22.136(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3805.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  '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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20382
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       'Flat Plate'
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.8(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9406
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                5421
_reflns_number_total             9406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026630d_s3.cif
_cod_data_source_block           JA026630D
_cod_original_cell_volume        3805.4(10)
_cod_database_code               4115007