Toward a Synthesis of Fawcettimine-Type Lycopodium Alkaloids: Stereocontrolled Synthesis of a Functionalized Azaspirocycle Precursor.
Huang, Wen-Yu; Nishikawa, Toshio; Nakazaki, Atsuo; The Journal of organic chemistry 83 (2018) 11108–11117; doi:10.1021/acs.joc.8b01719

data_4035656
_publ_section_title
;
 Toward a Synthesis of Fawcettimine-Type Lycopodium Alkaloids:
 Stereocontrolled Synthesis of a Functionalized Azaspirocycle Precursor.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11108
_journal_page_last               11117
_journal_paper_doi               10.1021/acs.joc.8b01719
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C41 H66 N2 O7 S Si2'
_chemical_formula_weight         787.19
_space_group_crystal_system      orthorhombic
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_space_group_name_Hall           '-P 2ac 2ab'
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_atom_sites_solution_hydrogens   geom
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_cell_volume                     8787.7(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0952
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_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_l_max       46
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_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.21
_diffrn_reflns_theta_min         3.750
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5714
_reflns_number_total             8038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01719_si_002.cif
_cod_data_source_block           NKtes
_cod_database_code               4035656
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.886
_exptl_absorpt_special_details   0.605
_shelx_res_checksum              86786
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