Triflic imide-catalyzed cascade cycloaddition and Friedel–Crafts reaction of diarylvinylidenecyclopropanes with ethyl 5,5-diarylpenta-2,3,4-trienoate
Li, Wei; Shi, Min; Organic & Biomolecular Chemistry 7 (2009) 1775–1777; doi:10.1039/b903965a

data_7150676
_publ_section_title
;
 Triflic imide-catalyzed cascade cycloaddition and Friedel--Crafts
 reaction of diarylvinylidenecyclopropanes with ethyl
 5,5-diarylpenta-2,3,4-trienoate
;
_journal_issue                   9
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              1775
_journal_page_last               1777
_journal_paper_doi               10.1039/b903965a
_journal_volume                  7
_journal_year                    2009
_chemical_formula_sum            'C42 H40 Cl2 O3'
_chemical_formula_weight         663.64
_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                90.102(2)
_cell_angle_beta                 93.697(3)
_cell_angle_gamma                100.409(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7469(12)
_cell_length_b                   11.6130(14)
_cell_length_c                   15.7201(18)
_cell_measurement_reflns_used    2201
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.201
_cell_measurement_theta_min      4.383
_cell_volume                     1746.3(4)
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9974
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75452
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.425
_exptl_crystal_size_min          0.360
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7077
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                4011
_reflns_number_total             7077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903965a.txt
_cod_data_source_block           cd2931
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7150676