Cu(I)-Catalyzed Domino Reaction of 3-Cyclopropylideneprop-2-en-1-ones
Maozhong Miao; Jian Cao; Jingjing Zhang; Xian Huang; Luling Wu; Journal of Organic Chemistry 78 (2013) 2687–2692; doi:10.1021/jo302312y

data_4028015
_publ_section_title
;
 Cu(I)-Catalyzed Domino Reaction of 3-Cyclopropylideneprop-2-en-1-ones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2687
_journal_page_last               2692
_journal_paper_doi               10.1021/jo302312y
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C36 H26 F2 O2'
_chemical_formula_weight         528.57
_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                87.010(2)
_cell_angle_beta                 88.663(2)
_cell_angle_gamma                76.653(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8825(8)
_cell_length_b                   10.8228(11)
_cell_length_c                   15.9897(17)
_cell_measurement_reflns_used    3336
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.132
_cell_measurement_theta_min      4.534
_cell_volume                     1325.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1084
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7036
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8146
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.217
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.089(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0908P)^2^+0.0313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                3909
_reflns_number_total             4871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo302312y_si_001.cif
_cod_data_source_block           cd29627
_cod_database_code               4028015