Structural studies on C-amidated amino acids and peptides: structures of hydrochloride salts of C-amidated Ile, Val, Thr, Ser, Met, Trp, Gln and Arg, and comparison with their C-unamidated counterparts
In, Yasuko; Fujii, Mayumi; Sasada, Yasuhiro; Ishida, Toshimasa; Acta Crystallographica Section B 57 (2001) 72–81; doi:10.1107/S0108768100013975

data_2103564
_publ_section_title
;
 Structural studies on C-amidated amino acids and peptides: structures
 of hydrochloride salts of C-amidated Ile, Val, Thr, Ser, Met, Trp, Gln
 and Arg, and comparison with their C-unamidated counterparts
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              72
_journal_page_last               81
_journal_paper_doi               10.1107/S0108768100013975
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C4 H11 N2 O2 +,Cl -'
_chemical_formula_sum            'C4 H11 Cl N2 O2'
_chemical_formula_weight         154.60
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1624(15)
_cell_length_b                   10.5673(17)
_cell_length_c                   6.749(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.10
_cell_measurement_theta_min      .3
_cell_volume                     724.8(4)
_computing_cell_refinement       'MSC/AFC (Molecular Structure Corp. 1991)'
_computing_data_collection       'MSC/AFC (Molecular Structure Corp. 1991)'
_computing_data_reduction        'MSC/AFC (Molecular Structure Corp. 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0079
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            710
_diffrn_reflns_theta_full        63.10
_diffrn_reflns_theta_max         63.10
_diffrn_reflns_theta_min         6.04
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.173
_exptl_absorpt_correction_T_max  .999
_exptl_absorpt_correction_T_min  .782
_exptl_absorpt_correction_type   \y-scan
_exptl_absorpt_process_details   'North, et al., 1990'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_meas      1.402(5)
_exptl_crystal_density_method    measured
_exptl_crystal_description       cubic
_exptl_crystal_F_000             328
_exptl_crystal_size_max          .8
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .6
_refine_diff_density_max         .496
_refine_diff_density_min         -.589
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   .06(3)
_refine_ls_extinction_coef       .34(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          .0471
_refine_ls_R_factor_gt           .0471
_refine_ls_shift/su_max          .049
_refine_ls_shift/su_mean         .008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+0.4071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1210
_reflns_number_gt                710
_reflns_number_total             710
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            oa0030.cif
_cod_data_source_block           thrNH2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+0.4071P] 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^)+(0.0986P)^2^+0.4071P] 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        724.8(3)
_cod_original_sg_symbol_H-M      'P 212121'
_cod_database_code               2103564
_cod_database_fobs_code          2103564