Easy Access to Fully Functionalized Chiral Tetrahydro-β-Carboline Alkaloids
Takayoshi Arai; Makiko Wasai; Naota Yokoyama; Journal of Organic Chemistry 76 (2011) 2909–2912; doi:10.1021/jo1025833

data_4026211
_publ_section_title
;
 Easy Access to Fully Functionalized Chiral Tetrahydro-\b-Carboline
 Alkaloids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2909
_journal_page_last               2912
_journal_paper_doi               10.1021/jo1025833
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C30 H25 Br N2 O'
_chemical_formula_weight         509.43
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2659(8)
_cell_length_b                   16.5538(12)
_cell_length_c                   16.9975(12)
_cell_measurement_temperature    296(2)
_cell_volume                     2888.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16054
_diffrn_reflns_theta_full        28.47
_diffrn_reflns_theta_max         28.47
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.445
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_F_000             1048
_refine_diff_density_max         6.065
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.362
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.798
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.798
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.1370
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3728
_refine_ls_wR_factor_ref         0.3800
_reflns_number_gt                5876
_reflns_number_total             6558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1025833_si_001.cif
_cod_data_source_block           pictet_ph_ph_4_br_o
_cod_database_code               4026211