Stereoselective Construction of Spiro-Fused Tricyclic Frameworks by Sequential Reaction of Enynes, Imines, and Diazoalkenes with Rh(I) and Rh(II) Catalysts.
Hato, Yoshio; Oonishi, Yoshihiro; Yamamoto, Yasunori; Nakajima, Kiyohiko; Sato, Yoshihiro; The Journal of organic chemistry 81 (2016) 7847–7854; doi:10.1021/acs.joc.6b01502

data_4037104
_publ_section_title
;
 Stereoselective Construction of Spiro-Fused Tricyclic Frameworks by
 Sequential Reaction of Enynes, Imines, and Diazoalkenes with Rh(I) and
 Rh(II) Catalysts.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              7847
_journal_page_last               7854
_journal_paper_doi               10.1021/acs.joc.6b01502
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C31 H42 N2 O4.67 S'
_chemical_formula_sum            'C31 H42 N2 O4.67 S'
_chemical_formula_weight         549.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-25
_audit_creation_method           'by CrystalStructure 4.1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.149(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            12
_cell_length_a                   22.508(3)
_cell_length_b                   15.8459(17)
_cell_length_c                   26.254(4)
_cell_measurement_reflns_used    4718
_cell_measurement_temperature    100
_cell_measurement_theta_max      75.20
_cell_measurement_theta_min      25.70
_cell_volume                     9350(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0859
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_diffrn_reflns_limit_h_min       -28
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
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_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.226
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             3544.32
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_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  8323 Friedel Pairs'
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_refine_ls_number_restraints     0
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_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0058Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                13212
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