Rhodium-catalyzed tandem nucleophilic addition/bicyclization of diyne-enones with alcohols: a modular entry to 2,3-fused bicyclic furans
Zhao, Wanxiang; Zhang, Junliang; Chemical Communications 46 (2010) 4384–4386; doi:10.1039/c000883d

data_7111591
_publ_section_title
;
 Rhodium-catalyzed tandem nucleophilic addition/bicyclization of
 diyne-enones with alcohols: a modular entry to 2,3-fused bicyclic furans
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              4384
_journal_page_last               4386
_journal_paper_doi               10.1039/c000883d
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C33 H29 N O8'
_chemical_formula_weight         567.57
_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                80.8370(10)
_cell_angle_beta                 73.1060(10)
_cell_angle_gamma                63.5430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1741(4)
_cell_length_b                   10.9686(4)
_cell_length_c                   14.9749(6)
_cell_measurement_temperature    296(2)
_cell_volume                     1430.68(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16771
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9685
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yello
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0682P)^2^+0.4315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1528
_reflns_number_gt                3333
_reflns_number_total             5003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000883dsup1.cif
_cod_data_source_block           z
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111591