Hydrogen atoms in bridging positions from quantum crystallographic refinements: Influence of hydrogen atom displacement parameters on geometry and electron density
Malaspina, Lorraine Andrade; Hoser, Anna A.; Edwards, Alison; Woinska, Magdalena; Turner, Michael J.; Price, Jason R.; Sugimoto, Kunihisa; Nishibori, Eiji; Burgi, Hans-Beat; Jayatilaka, Dylan; Grabowsky, Simon; CrystEngComm  (2020) –; doi:10.1039/D0CE00378F

data_7240727
_publ_section_title
;
 Hydrogen atoms in bridging positions from quantum crystallographic
 refinements: Influence of hydrogen atom displacement parameters on
 geometry and electron density
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00378F
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C4 H3 O4, C9 H12 N O2'
_chemical_formula_sum            'C13 H15 N O6'
_chemical_formula_weight         281.2676
_chemical_name_common            'L-phenylalaninium hydrogen maleate'
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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   HAR
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-02T17:25:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-03-10 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_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      0.9
_cell_volume                     640.1(2)
_diffrn_ambient_temperature      25
_diffrn_detector                 'SPring-8 BL02B1 Curved Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_device_type  IPDSC-Q
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.354
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_unetI/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         0.9
_diffrn_source                   SPring-8
_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          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.2128
_refine_diff_density_min         -0.2321
_refine_diff_density_rms         0.0355
_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_all   0.8688
_refine_ls_goodness_of_fit_gt    0.8688
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    91
_refine_ls_number_parameters     225
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.0018
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/\s(F)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0213
_refine_ls_wR_factor_gt          0.0213
_reflns_number_gt                7564
_reflns_number_total             7820
_reflns_threshold_expression     'F>0 & F/u(F)>4.0 & |F_calc|>10^-3'
_cod_data_source_file            d0ce00378f2.cif
_cod_data_source_block           PhAla_HAR_neutron
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_Hall     'p 2yb'
_cod_original_sg_symbol_H-M      'p 1 21 1'
_cod_database_code               7240727
_refine_ls_coordinate_system     cartesian
_refine_ls_svd_threshold         0.1E-02