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_7105513
_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            'C31 H28 Cl3 N2 O Rh'
_chemical_formula_weight         653.81
_chemical_name_common            8
_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                112.1714(17)
_cell_angle_beta                 97.0413(16)
_cell_angle_gamma                100.9423(18)
_cell_formula_units_Z            2
_cell_length_a                   9.1035(5)
_cell_length_b                   12.2818(7)
_cell_length_c                   13.9760(7)
_cell_measurement_reflns_used    6240
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.10
_cell_volume                     1387.98(13)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13659
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.8964
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.664
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0394P)^2^+1.6293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                5626
_reflns_number_total             6240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000747a.txt
_cod_data_source_block           8(CCDC_752604)
_cod_original_cell_volume        1387.97(13)
_cod_database_code               7105513