Synthesis of 1,4-Dichloro-1,3-butadienes by Rhodium Complex Catalyzed Reaction of Terminal Alkynes with Trichloroacetyl Chloride
Taigo Kashiwabara; Kouichirou Fuse; Takeshi Muramatsu; Masato Tanaka; Journal of Organic Chemistry 74 (2009) 9433–9439; doi:10.1021/jo902088p

data_4025111
_publ_contact_author_address
'4259-R1-13 Nagatsuta, Midori-ku, Yokohama 226-8503 JAPAN'
_publ_contact_author_email       m.tanaka@res.titech.ac.jp
_publ_contact_author_fax         +81-45-924-5279
_publ_contact_author_name        'Masato TANAKA'
_publ_contact_author_phone       +81-45-924-5245
_publ_section_title
;
Synthesis of 1,4-Dichloro-1,3-butadienes by Rhodium Complex Catalyzed
Reaction of Terminal Alkynes with Trichloroacetyl Chloride
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9433
_journal_page_last               9439
_journal_paper_doi               10.1021/jo902088p
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C12 H30 Cl6 P4 Rh2 '
_chemical_formula_sum            'C12 H30 Cl6 P4 Rh2'
_chemical_formula_weight         716.79
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_audit_creation_date             2008-10-01
_audit_creation_method           'by CrystalStructure 3.7.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.217(5)
_cell_length_b                   13.036(6)
_cell_length_c                   17.985(9)
_cell_measurement_reflns_used    6161
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2630(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18882
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    2.102
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.07
_refine_diff_density_min         -0.83
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1327
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0023Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                1327
_reflns_number_total             3062
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo902088p_si_001_2.cif
_cod_data_source_block           '__6'
_cod_original_formula_sum        'C12 H30 Cl6 P4 Rh2 '
_cod_database_code               4025111