trans-RhCl(CO)(PPh3)2-Catalyzed Monomeric and Dimeric Cycloisomerization of Propargylic 2,3-Dienoates. Establishment of α,β-Unsaturated δ-Lactone Rings by Cyclometallation
Xuefeng Jiang; Shengming Ma; Journal of the American Chemical Society 129 (2007) 11600–11607; doi:10.1021/ja073582u

data_4109931
_publ_section_title
;
 trans-RhCl(CO)(PPh3)2-Catalyzed Monomeric and Dimeric Cycloisomerization
 of Propargylic 2,3-Dienoates. Establishment of \a,\b-Unsaturated
 \d-Lactone Rings by Cyclometallation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11600
_journal_page_last               11607
_journal_paper_doi               10.1021/ja073582u
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C34 H36 O4'
_chemical_formula_weight         508.63
_chemical_name_systematic
; 
 ? 
;
_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                93.347(4)
_cell_angle_beta                 92.725(4)
_cell_angle_gamma                94.441(3)
_cell_formula_units_Z            4
_cell_length_a                   8.6809(14)
_cell_length_b                   15.504(2)
_cell_length_c                   21.838(3)
_cell_measurement_reflns_used    1151
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      37.733
_cell_measurement_theta_min      4.443
_cell_volume                     2921.3(7)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1336
_diffrn_reflns_av_sigmaI/netI    0.2344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15521
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62678
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0012(8)
_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   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         10707
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.2184
_refine_ls_R_factor_gt           0.0900
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2722
_reflns_number_gt                3481
_reflns_number_total             10707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073582usi20070518_113906.cif
_cod_data_source_block           cd27126
_cod_original_cell_volume        2921.4(8)
_cod_database_code               4109931