Highly diastereoselective additions of methoxyallene and acetylenes to chiral α-keto amides
Youn, So Won; Kim, Yong Hae; Hwang, Jeong-Wook; Do, Youngkyu; Chemical Communications  (2001) 996–; doi:10.1039/b100355k

data_7114936
_publ_contact_author             'Prof Yong Hae Kim'
_publ_section_title
;
 Highly diastereoselective additions of methoxyallene and acetylenes to
 chiral \a-keto amides
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              996
_journal_paper_doi               10.1039/b100355k
_journal_year                    2001
_chemical_formula_sum            'C15 H17 N O3'
_chemical_formula_weight         259.30
_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            8
_cell_length_a                   10.300(2)
_cell_length_b                   10.536(2)
_cell_length_c                   25.810(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     2800.9(10)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART 1K CCD'
_diffrn_measurement_method       scanning
_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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32006
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7411
_exptl_absorpt_correction_type
'SADABS-Bruker area detector absortion corrections'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          '0.22 mm'
_exptl_crystal_size_mid          '0.15 mm'
_exptl_crystal_size_min          '0.12 mm'
_refine_diff_density_max         0.097
_refine_diff_density_min         -0.094
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.43(76)
_refine_ls_extinction_coef       0.0062(2)
_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   0.713
_refine_ls_goodness_of_fit_obs   0.956
_refine_ls_hydrogen_treatment    'refined isotropically'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6530
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      0.956
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_obs          0.0333
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w==1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0502
_refine_ls_wR_factor_obs         0.0404
_reflns_number_observed          2661
_reflns_number_total             6530
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b100355k.txt
_cod_data_source_block           5g
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w==1/[\s^2^(Fo^2^)+(0.0126P)^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^)+(0.0126P)^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_original_cell_volume        2800.9(11)
_cod_original_sg_symbol_H-M      'P212121 (No. 19)'
_cod_database_code               7114936