Polycyclic alkaloids via transannular Mannich reactions.
Vital, Paulo; Hosseini, Masood; Shanmugham, M Sundaram; Gotfredsen, Charlotte H; Harris, Pernille; Tanner, David; Chemical communications (Cambridge, England) 34 (2009) 1888–1890; doi:10.1039/b822955d

data_7104307
_publ_section_title
;
 Polycyclic alkaloids via transannular Mannich reactions.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1888
_journal_page_last               1890
_journal_paper_doi               10.1039/b822955d
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C17 H29 N O4'
_chemical_formula_weight         311.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.957(2)
_cell_angle_beta                 91.847(2)
_cell_angle_gamma                96.174(2)
_cell_formula_units_Z            2
_cell_length_a                   5.6851(7)
_cell_length_b                   10.6061(12)
_cell_length_c                   14.1542(16)
_cell_measurement_reflns_used    2216
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.207
_cell_measurement_theta_min      2.887
_cell_volume                     845.80(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART platform ccd'
_diffrn_measurement_method       'profile data from \w/2\q scans'
_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  0.1283
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11580
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1024P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                2593
_reflns_number_total             4082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b822955d.txt
_cod_data_source_block           mscy02m
_cod_original_formula_sum        'C17 H29 N1 O4'
_cod_database_code               7104307