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_4116462
_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            'C17 H19 N O4'
_chemical_formula_weight         301.33
_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                74.383(7)
_cell_angle_beta                 88.256(7)
_cell_angle_gamma                73.228(6)
_cell_formula_units_Z            2
_cell_length_a                   6.1423(4)
_cell_length_b                   9.9509(8)
_cell_length_c                   13.630(1)
_cell_measurement_temperature    183(2)
_cell_volume                     767.19(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(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  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5145
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.093
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             320
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0292(36)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.995
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_obs          0.0495
_refine_ls_shift/esd_max         0.042
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.3269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1193
_refine_ls_wR_factor_obs         0.0996
_reflns_number_observed          2798
_reflns_number_total             4350
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja990077r_7.cif
_cod_data_source_block           11b
_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^)+(0.0384P)^2^+0.3269P] 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^)+(0.0384P)^2^+0.3269P] 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               4116462