Convenient one-step construction of yne-functionalized aryl halides through domino cyclization from tetraynes
Hao Zhang; Qiong Hu; Lidong Li; Yimin Hu; Pingping Zhou; Xiaorong Zhang; Haifeng Xie; Fei Yin; Yadong Hu; Shaowu Wang; Chem.Commun. 50 (2014) 3335–; doi:10.1039/c3cc47707j

data_7112095
_publ_section_title
;
 Convenient one-step construction of yne-functionalized aryl halides
 through domino cyclization from tetraynes
;
_journal_name_full               Chem.Commun.
_journal_page_first              3335
_journal_paper_doi               10.1039/c3cc47707j
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C29 H25 Cl O4'
_chemical_formula_weight         472.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.902(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4930(12)
_cell_length_b                   32.264(4)
_cell_length_c                   7.8878(10)
_cell_measurement_reflns_used    7275
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.24
_cell_volume                     2415.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20851
_diffrn_reflns_theta_full        27.64
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+0.5210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                4079
_reflns_number_total             5582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47707j2.cif
_cod_data_source_block           111222a
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7112095