Construction of the Fused Pentacycle of Talatisamine via a Combination of Radical and Cationic Cyclizations.
Tabuchi, Toshiki; Urabe, Daisuke; Inoue, Masayuki; The Journal of organic chemistry 81 (2016) 10204–10213; doi:10.1021/acs.joc.6b01011

data_4036938
_publ_section_title
;
 Construction of the Fused Pentacycle of Talatisamine via a Combination of
 Radical and Cationic Cyclizations.
;
_journal_issue                   21
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10204
_journal_page_last               10213
_journal_paper_doi               10.1021/acs.joc.6b01011
_journal_volume                  81
_journal_year                    2016
_chemical_formula_sum            'C35 H51 N O8 Se Si'
_chemical_formula_weight         720.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 114.015(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0171(11)
_cell_length_b                   8.3446(5)
_cell_length_c                   21.3332(12)
_cell_measurement_reflns_used    444
_cell_measurement_temperature    93.0(2)
_cell_measurement_theta_max      69.4265
_cell_measurement_theta_min      4.6144
_cell_volume                     3417.5(3)
_computing_cell_refinement       'APEX2 v2013.10 (Bruker AXS)'
_computing_data_collection       'APEX II ULTRA (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT v8.34A (Bruker AXS Inc.)'
_computing_molecular_graphics    'XSHELL v6.3.1 (Bruker AXS Inc.)'
_computing_publication_material  'Generate Report (Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'D8 goniometer (Bruker AXS Inc.)'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22973
_diffrn_reflns_theta_full        66.74
_diffrn_reflns_theta_max         66.74
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Tourbo X-ray Source'
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.749
_refine_ls_extinction_coef       0.00024(9)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6026
_refine_ls_number_restraints     473
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+1.0676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                4721
_reflns_number_total             6026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b01011_si_002.cif
_cod_data_source_block           I
_cod_database_code               4036938