Hirshfeld atom refinement for modelling strong hydrogen bonds
Woińska, Magdalena; Jayatilaka, Dylan; Spackman, Mark A.; Edwards, Alison J.; Dominiak, Paulina M.; Woźniak, Krzysztof; Nishibori, Eiji; Sugimoto, Kunihisa; Grabowsky, Simon; Acta Crystallographica Section A 70 (2014) 483–498; doi:10.1107/S2053273314012443

data_2310143
_publ_section_title
;
 Hirshfeld atom refinement for modelling strong hydrogen bonds
;
_journal_coeditor_code           KX5029
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              483
_journal_page_last               498
_journal_paper_doi               10.1107/S2053273314012443
_journal_volume                  70
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H12 N O2, C4 H3 O4'
_chemical_formula_sum            'C13 H15 N O6'
_chemical_formula_weight         281.27
_chemical_name_common            'L-phenylalaninium hydrogen maleate'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.905(2)
_cell_length_b                   5.2338(10)
_cell_length_c                   11.439(2)
_cell_measurement_reflns_used    124185
_cell_measurement_temperature    25
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      0.90
_cell_volume                     640.1(2)
_diffrn_ambient_temperature      25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SPring-8 BL02B1 Imaging plate camera'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3540
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.063
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            124185
_diffrn_reflns_theta_full        23.16
_diffrn_reflns_theta_max         23.16
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    0.039
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.20
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.86
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    211
_refine_ls_number_parameters     105
_refine_ls_number_reflns         7370
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/\s(F)
_refine_ls_wR_factor_gt          0.0211
_reflns_number_gt                7370
_reflns_number_total             7820
_reflns_threshold_expression     >2sigma(I)
_iucr_refine_instructions_details 'Hirshfeld Atom Refinement'
_cod_data_source_file            kx5029sup1.cif
_cod_data_source_block           xray
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C13 H15 N1 O6'
_cod_database_code               2310143
_cod_database_fobs_code          2310143