Vinylogous Mannich Reactions. The Asymmetric Total Synthesis of (+)-Croomine
Stephen F. Martin; Kenneth J. Barr; Journal of the American Chemical Society 118 (1996) 3299–3300; doi:10.1021/ja9542146

data_4117119
_publ_section_title
;
 Vinylogous Mannich Reactions. The Asymmetric Total Synthesis of
 (+)-Croomine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3299
_journal_page_last               3300
_journal_paper_doi               10.1021/ja9542146
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C20 H30 Br N O6'
_chemical_formula_weight         460.36
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3430(10)
_cell_length_b                   10.1240(10)
_cell_length_c                   22.733(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2150.3(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0882
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4018
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.946
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_F_000             960
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(11)
_refine_ls_extinction_coef       0.0066(5)
_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   1.031
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.0728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0872
_refine_ls_wR_factor_obs         0.0725
_reflns_number_observed          2488
_reflns_number_total             3885
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9542146_2.cif
_cod_data_source_block           11
_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^)+(0.0281P)^2^+0.0728P] 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^)+(0.0281P)^2^+0.0728P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4117119