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_7112096
_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            'C33 H33 Cl O4'
_chemical_formula_weight         529.04
_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            8
_cell_length_a                   12.1117(9)
_cell_length_b                   15.1500(12)
_cell_length_c                   31.225(2)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    293(2)
_cell_volume                     5729.5(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            47424
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9800
_exptl_absorpt_correction_T_min  0.9703
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0835P)^2^+1.6385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1801
_reflns_number_gt                4184
_reflns_number_total             6659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47707j2.cif
_cod_data_source_block           120109a_0m
_cod_original_cell_volume        5729.6(8)
_cod_original_sg_symbol_H-M      'Pbca '
_cod_database_code               7112096