Diaceno[a,e]pentalenes from Homoannulations of o-Alkynylaryliodides Utilizing a Unique Pd(OAc)2/n-Bu4NOAc Catalytic Combination.
Shen, Junjian; Yuan, Dafei; Qiao, Yan; Shen, Xingxing; Zhang, Zhongbo; Zhong, Yuwu; Yi, Yuanping; Zhu, Xiaozhang; Organic letters 16 (2014) 4924–4927; doi:10.1021/ol502440d

data_1517559
_publ_section_title
;
 Diaceno[a,e]pentalenes from Homoannulations of o-Alkynylaryliodides
 Utilizing a Unique Pd(OAc)2/n-Bu4NOAc Catalytic Combination.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4924
_journal_page_last               4927
_journal_paper_doi               10.1021/ol502440d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C28 H16 F2'
_chemical_formula_sum            'C28 H16 F2'
_chemical_formula_weight         390.41
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.498(3)
_cell_length_b                   7.559(4)
_cell_length_c                   23.466(10)
_cell_measurement_reflns_used    5488
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.74
_cell_volume                     1862.1(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 ver 1.1'
_computing_publication_material  'SHELX97 (Sheldrick, 2008)'
_computing_structure_refinement  'Olex2 ver 1.1'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11455
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.367
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.367
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0821
_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^)+(0.0177P)^2^+1.4531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                2032
_reflns_number_total             2118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol502440d_si_003.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1517557--1517560.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1517559