New Fischer Carbene Complexes of Rhodium(I): Preparation and 2-Cyclopentenone Ring Synthesis by Annelation to Alkynes
José Barluenga; Rubén Vicente; Luis A. López; Eduardo Rubio; Miguel Tomás; Carmen Álvarez-Rúa; Journal of the American Chemical Society 126 (2004) 470–471; doi:10.1021/ja038817q

data_4112143
_publ_contact_author
;     Carmen Alvarez-R\'ua
      Departamento de Qu\'imica F\'isica y Anal\'itica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33071 Oviedo
      Spain
;
_publ_contact_author_email       mcara@sauron.quimica.uniovi.es
_publ_contact_author_fax         '0034 98 5103125'
_publ_contact_author_phone       '0034 98 5102968'
_publ_section_title
;
 New Fischer Carbene Complexes of Rhodium(I): Preparation and
 2-Cyclopentenone Ring Synthesis by Annelation to Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              470
_journal_page_last               471
_journal_paper_doi               10.1021/ja038817q
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C20 H24 F6 O3 Rh Sb'
_chemical_formula_weight         651.05
_chemical_name_systematic
; 
(carbonyl)(\h^4^-1,5-cycloctadiene)
[1-methoxy-3-(4-methoxyphenyl)-2-propenylidene]rhodium(I)
hexafluoroantimonate 
;
_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                100.643(2)
_cell_angle_beta                 96.326(2)
_cell_angle_gamma                100.073(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7212(3)
_cell_length_b                   9.4995(4)
_cell_length_c                   15.4033(6)
_cell_measurement_reflns_used    4063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.90
_cell_measurement_theta_min      2.95
_cell_volume                     1221.37(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8270
_diffrn_reflns_theta_full        62.90
_diffrn_reflns_theta_max         62.90
_diffrn_reflns_theta_min         2.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.822
_exptl_absorpt_correction_T_max  0.411
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       prism
_exptl_crystal_F_000             636
_exptl_crystal_preparation
;
 Crystallization solvents: dichloromethane / diethyl ether 
;
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0868P)^2^+1.7657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1455
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                2879
_reflns_number_total             3698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038817qsi20031001_012002.cif
_cod_data_source_block           lop2m
_cod_database_code               4112143