Applications of Vinylogous Mannich Reactions. Concise Enantiospecific Total Syntheses of (+)-Croomine
Stephen F. Martin; Kenneth J. Barr; Dudley W. Smith; Scott K. Bur; Journal of the American Chemical Society 121 (1999) 6990–6997; doi:10.1021/ja990077r

data_4116458
_publ_section_title
;
 Applications of Vinylogous Mannich Reactions. Concise Enantiospecific
 Total Syntheses of (+)-Croomine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6990
_journal_page_last               6997
_journal_paper_doi               10.1021/ja990077r
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C18 H21 N O4'
_chemical_formula_weight         315.36
_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
_cell_angle_alpha                96.24(9)
_cell_angle_beta                 102.65(6)
_cell_angle_gamma                97.01(8)
_cell_formula_units_Z            2
_cell_length_a                   6.154(4)
_cell_length_b                   11.495(15)
_cell_length_c                   12.322(10)
_cell_measurement_temperature    298(2)
_cell_volume                     835.9(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_av_sigmaI/netI    0.2223
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2380
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.088
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_F_000             336
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.768
_refine_ls_goodness_of_fit_obs   2.827
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.768
_refine_ls_restrained_S_obs      2.827
_refine_ls_R_factor_all          0.3303
_refine_ls_R_factor_obs          0.1338
_refine_ls_shift/esd_max         0.037
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2479
_refine_ls_wR_factor_obs         0.2020
_reflns_number_observed          705
_reflns_number_total             2149
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990077r_3.cif
_cod_data_source_block           11d
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116458