Synthesis of [RhCl(CO)(cyclopentadienone)]2 from [RhCl(cod)]2 and a 1,6-diyne under CO: application to Rh(i)-catalyzed tandem [2+2+1] carbonylative cycloaddition of diynes and Claisen rearrangement
Lee, Sang Ick; Fukumoto, Yoshiya; Chatani, Naoto; Chemical Communications 46 (2010) 3345–3347; doi:10.1039/c000747a

data_7105515
_publ_section_title
;
 Synthesis of [RhCl(CO)(cyclopentadienone)]2 from [RhCl(cod)]2 and a
 1,6-diyne under CO: application to Rh(i)-catalyzed tandem [2+2+1]
 carbonylative cycloaddition of diynes and Claisen rearrangement
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              3345
_journal_page_last               3347
_journal_paper_doi               10.1039/c000747a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C26 H20 O2'
_chemical_formula_weight         364.42
_chemical_name_common            11a
_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                87.5344(12)
_cell_angle_beta                 87.5267(12)
_cell_angle_gamma                89.2463(12)
_cell_formula_units_Z            4
_cell_length_a                   8.6916(2)
_cell_length_b                   8.6917(2)
_cell_length_c                   24.9284(5)
_cell_measurement_reflns_used    7100
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      71.65
_cell_measurement_theta_min      3.55
_cell_volume                     1879.59(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34157
_diffrn_reflns_theta_full        71.65
_diffrn_reflns_theta_max         71.65
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.8897
_exptl_absorpt_correction_T_min  0.8144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+0.2680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1647
_reflns_number_gt                5581
_reflns_number_total             7100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000747a.txt
_cod_data_source_block           11a(CCDC_752606)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7105515