b Turns, water cage formation and hydrogen bonding in the structures of L-Valyl-L-phenylalanine
Görbitz, Carl Henrik; Acta Crystallographica, Section B 58 (2002) 512–518; doi:10.1107/S010876810200277X

data_2103138
_publ_section_title
;
b Turns, water cage formation and hydrogen bonding in the structures of
L-Valyl-L-phenylalanine
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica, Section B'
_journal_page_first              512
_journal_page_last               518
_journal_paper_doi               10.1107/S010876810200277X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C14 H26 N2 O6'
_chemical_formula_weight         318.37
_chemical_name_systematic
;
 L-Val-L-Phe trihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.1710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   10.3137(3)
_cell_length_b                   45.2095(12)
_cell_length_c                   15.5891(4)
_cell_measurement_reflns_used    49294
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      1.43
_cell_volume                     7015.5(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method
'Sets of exposures each taken over 0.3\% \w rotation'
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       62
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            72689
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          1.10
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.417
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1475
_refine_ls_number_reflns         19842
_refine_ls_number_restraints     1703
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+9.9786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2081
_reflns_number_gt                18611
_reflns_number_total             19842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            os0088.cif
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2103138