Diarylrhodates as promising active catalysts for the arylation of vinyl ethers with grignard reagents.
Iwasaki, Takanori; Miyata, Yoshinori; Akimoto, Ryo; Fujii, Yuuki; Kuniyasu, Hitoshi; Kambe, Nobuaki; Journal of the American Chemical Society 136 (2014) 9260–9263; doi:10.1021/ja5043534

data_4122093
_publ_section_title
;
 Diarylrhodates as promising active catalysts for the arylation of vinyl
 ethers with grignard reagents.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9260
_journal_page_last               9263
_journal_paper_doi               10.1021/ja5043534
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C32 H52 Li O6 Rh'
_chemical_formula_sum            'C32 H52 Li O6 Rh'
_chemical_formula_weight         642.61
_chemical_melting_point          368
_chemical_name_common            'RhPh2(cod) Li(dme)3'
_chemical_name_systematic
'tris(1,2-dimethoxyethane)lithium (h4-1,5-cyclooctadiene)diphenylrhodate(I)'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 109.64(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.564(4)
_cell_length_b                   16.3801(16)
_cell_length_c                   13.740(8)
_cell_measurement_reflns_used    13304
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      3.13
_cell_volume                     3299(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 5.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1160
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25899
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1360.00
_exptl_crystal_recrystallization_method
'dietnhyl ether/1,2-dimethoxyethane/pentane at 248 K'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3789
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0772P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                2714
_reflns_number_total             3789
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja5043534_si_002.cif
_cod_data_source_block           RhPh2(cod)Li(dme)3
_cod_depositor_comments
'Adding full bibliography for 4122092--4122093.cif.'
_cod_original_cell_volume        3299(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4122093