Construction of Unusual and Congested Polycyclic Structures via Benzannulated Enediynyl Alcohols Derived from Truxenone
Yu-Hsuan Wang; Novruz G. Akhmedov; Jeffrey L. Petersen; Kung K. Wang; Journal of Organic Chemistry 72 (2007) 9604–9608; doi:10.1021/jo701736y

data_4023089
_publ_section_title
;
 Construction of Unusual and Congested Polycyclic Structures
 via Benzannulated Enediynyl Alcohols Derived from Truxenone
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9604
_journal_page_last               9608
_journal_paper_doi               10.1021/jo701736y
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C62.5 H38 Cl3 O'
_chemical_formula_weight         911.28
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.152(1)
_cell_angle_beta                 84.070(1)
_cell_angle_gamma                78.997(1)
_cell_formula_units_Z            4
_cell_length_a                   15.8932(11)
_cell_length_b                   16.4553(11)
_cell_length_c                   17.6576(11)
_cell_measurement_reflns_used    7795
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.31
_cell_volume                     4508.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.1575
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32446
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         20170
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.116
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1698
_reflns_number_gt                8171
_reflns_number_total             20170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo701736y-File003.cif
_cod_data_source_block           lw2plt
_cod_original_formula_sum        'C62.50 H38 Cl3 O'
_cod_database_code               4023089