Silver-Catalyzed Reaction of Enynals with Alkenes: A Tandem 1,3-Dipolar Cycloaddition/Cyclopropanation.
Liang, Renxiao; Ma, Tongmei; Zhu, Shifa; Organic letters 16 (2014) 4412–; doi:10.1021/ol5017299

data_1517395
_publ_section_title
;
 Silver-Catalyzed Reaction of Enynals with Alkenes: A Tandem 1,3-Dipolar
 Cycloaddition/Cyclopropanation.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4412
_journal_paper_doi               10.1021/ol5017299
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C27 H22 Cl2 O3'
_chemical_formula_weight         465.35
_space_group_IT_number           2
_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                97.91(3)
_cell_angle_beta                 101.73(3)
_cell_angle_gamma                98.44(3)
_cell_formula_units_Z            2
_cell_length_a                   9.881(2)
_cell_length_b                   10.831(2)
_cell_length_c                   11.457(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1169.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11276
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.9702
_exptl_absorpt_correction_T_min  0.9417
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0810P)^2^+0.8758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2000
_reflns_number_gt                3925
_reflns_number_total             5289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5017299_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 1517395.cif.'
_cod_database_code               1517395