Crystal structures of natural amino acid perhydrates
Prikhodchenko, Petr V.; Medvedev, Alexander G.; Tripol'skaya, Tatiana A.; Churakov, Andrei V.; Wolanov, Yitzhak; Howard, Judith A. K.; Lev, Ovadia; CrystEngComm 13 (2011) 2399–; doi:10.1039/c0ce00481b

data_7205610
_publ_section_title
;
 Crystal structures of natural amino acid perhydrates
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              2399
_journal_paper_doi               10.1039/c0ce00481b
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C9 H11 N O2, H2 O2, 0.5(H2 O)'
_chemical_formula_sum            'C9 H14 N O4.5'
_chemical_formula_weight         208.21
_chemical_name_common
;(S)-2-Amino-3-phenylpropionic acid hydrogen peroxide solvate
hemihydrate
;
_chemical_name_systematic
;
(S)-2-Amino-3-phenylpropionic acid
hydrogen peroxide solvate hemihydrate
;
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.780(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0268(16)
_cell_length_b                   7.2283(12)
_cell_length_c                   14.150(2)
_cell_measurement_reflns_used    2427
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.981
_cell_measurement_theta_min      2.882
_cell_volume                     1024.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1K'
_diffrn_measurement_method       \W
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3278
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_correction_T_min  0.9630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1307
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.2195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                1205
_reflns_number_total             1307
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0ce00481b.txt
_cod_data_source_block           Phe50
_cod_depositor_comments
;

2018-06-26
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_moiety     '2(C9 H11 N O2), 2(H2 O2), H2 O'
_cod_original_formula_sum        'C18 H28 N2 O9'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     416.42
_cod_database_code               7205610