Conformation of (<i>S</i>,<i>S</i>)-Methyl (2-Methyl-4-phenylbutanamido)(phenyl)acetate
Yoshinobu Inouye; Tetsuya Yabuuti; Takenori Kusumi; Acta Crystallographica Section C 53 (1997) IUC9700017–; doi:10.1107/S0108270197099393

data_2006617
_publ_section_title
;
 Conformation of (<i>S</i>,<i>S</i>)-Methyl
 (2-Methyl-4-phenylbutanamido)(phenyl)acetate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9700017
_journal_paper_doi               10.1107/S0108270197099393
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C20 H23 N O3'
_chemical_formula_weight         325.39
_chemical_melting_point          135.5(5)
_chemical_name_systematic
' (S,S)-2-methyl-4-phenyl-N-[(methoxycarbonyl)phenylmethyl]butanamide'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 122.870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.874(6)
_cell_length_b                   5.1010(10)
_cell_length_c                   18.261(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.86
_cell_measurement_theta_min      10.06
_cell_volume                     1789.6(7)
_computing_cell_refinement       'CAD4 Software(Enraf-Nonius, 1989)'
_computing_data_collection       'CAD4 Software(Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEM(Fair, 1990)'
_computing_molecular_graphics    'ORTEPII(Johnson, 1976)'
_computing_publication_material  'MS-WORD (Microsoft, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0102
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2957
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.140
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_obs          .0466
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.3196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1330
_refine_ls_wR_factor_obs         .1107
_reflns_number_observed          1910
_reflns_number_total             2876
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            qb0020.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '135--136' was changed to '135.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '135--136' was changed to '135.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.3196P] 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^)+(0.0629P)^2^+0.3196P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C20 H23 N1 O3'
_cod_database_code               2006617