Mechanistic Investigation of Rh<sup>I</sup>-Catalyzed Cycloisomerization of Benzylallene-Internal Alkynes via C-H Activation.
Kawaguchi, Yasuaki; Yasuda, Shigeo; Mukai, Chisato; The Journal of organic chemistry 82 (2017) 7666–7674; doi:10.1021/acs.joc.7b01048

data_4037503
_publ_section_title
;
 Mechanistic Investigation of Rh<sup>I</sup>-Catalyzed Cycloisomerization
 of Benzylallene-Internal Alkynes via C-H Activation.
;
_journal_issue                   14
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              7666
_journal_page_last               7674
_journal_paper_doi               10.1021/acs.joc.7b01048
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C31 H36 O6 S'
_chemical_formula_sum            'C31 H36 O6 S'
_chemical_formula_weight         536.68
_chemical_name_systematic
;(2R*,12S*)-2-Butyl-14,14-bis(methoxycarbonyl)-9,9-dimethyl-12-
phenylsulfonyltricyclo[9.4.0.03,8]tetradeca-1(15),3,5,7,10-tetraene
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 99.530(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.711(3)
_cell_length_b                   9.334(2)
_cell_length_c                   25.458(6)
_cell_measurement_reflns_used    7590
_cell_measurement_temperature    103
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.00
_cell_volume                     2744.4(11)
_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    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      103
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.1154
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19472
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'R-AXIS RAPID'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144.00
_exptl_crystal_recrystallization_method Chloroform
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.850
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6102
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1268P)^2^+3.0561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3107
_reflns_number_gt                3455
_reflns_number_total             6102
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo7b01048_si_002.cif
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_cod_original_cell_volume        2744.3(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4037503