Access to unusual polycyclic spiro enones from 2,2'-bis(allyloxy)-1,1'-binaphthyls using Grubbs' catalysts: An unprecedented one-pot RCM/Claisen sequence
Estefania Piedra; Javier Francos; Noel Nebra; Francisco J. Suarez; Josefina Diez; Victorio Cadierno; Chem.Commun. 47 (2011) 7866–; doi:10.1039/c1cc11907a

data_7106580
_publ_section_title
;
 Access to unusual polycyclic spiro enones from
 2,2'-bis(allyloxy)-1,1'-binaphthyls using Grubbs' catalysts: An
 unprecedented one-pot RCM/Claisen sequence
;
_journal_name_full               Chem.Commun.
_journal_page_first              7866
_journal_paper_doi               10.1039/c1cc11907a
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        synthesis
_chemical_formula_moiety         '2 (C48 H36 O4), C4 H8 O2'
_chemical_formula_sum            'C100 H80 O10'
_chemical_formula_weight         1441.64
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 100.798(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3425(2)
_cell_length_b                   34.4213(4)
_cell_length_c                   14.4598(1)
_cell_measurement_reflns_used    14191
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5571
_cell_measurement_theta_min      2.5650
_cell_volume                     7501.14(14)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR 2004'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device
;
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38175
_diffrn_reflns_theta_full        73.82
_diffrn_reflns_theta_max         73.82
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         13996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1527P)^2^+0.4412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2149
_refine_ls_wR_factor_ref         0.2352
_reflns_number_gt                9716
_reflns_number_total             13996
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1cc11907a.txt
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7106580