Rhodium-Catalyzed Three-Component Reaction between Silylacetylene and Two Ketenes Leading to 1,3-Enynes Bearing a Carboxylic Ester Group via Double Insertion of Ketenes.
Ogata, Kenichi; Ohashi, Itsuki; Fukuzawa, Shin-Ichi; Organic letters 14 (2012) 4214–4217; doi:10.1021/ol301897h

data_1508352
_publ_section_title
;
 Rhodium-Catalyzed Three-Component Reaction between Silylacetylene and Two
 Ketenes Leading to 1,3-Enynes Bearing a Carboxylic Ester Group via Double
 Insertion of Ketenes.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4214
_journal_page_last               4217
_journal_paper_doi               10.1021/ol301897h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C38 H66 Rh2 Si2'
_chemical_formula_sum            'C38 H66 Rh2 Si2'
_chemical_formula_weight         784.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 111.555(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.8351(9)
_cell_length_b                   11.2002(5)
_cell_length_c                   20.4039(11)
_cell_measurement_reflns_used    11027
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.06
_cell_volume                     3790.8(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0825
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_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
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_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
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_exptl_crystal_size_mid          0.400
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_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_data_source_file            ol301897h_si_004.cif
_cod_data_source_block           20111128ogaf968Rhacetylide
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_cod_database_code               1508352