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_7240726
_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, C5 H7 N2'
_chemical_formula_sum            'C9 H10 N2 O4'
_chemical_formula_weight         210.191
_chemical_name_common            '4-aminopyridinium 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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-25T11:21:27-00:00
_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                 96.394(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.85280(10)
_cell_length_b                   5.54510(10)
_cell_length_c                   10.9223(2)
_cell_measurement_reflns_used    109774
_cell_measurement_temperature    16.5(10)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      0.94
_cell_measurement_wavelength     0.3542
_cell_volume                     472.648(15)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction
'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)'
_computing_structure_refinement
'Tonto 18.12.17 github v. 2b3dd9c (Capelli, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      16.5(10)
_diffrn_detector                 'SPring-8 BL02B1 Curved Imaging Plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_device_type  IPDSC-Q
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_UB_11      -0.018979
_diffrn_orient_matrix_UB_12      -0.095374
_diffrn_orient_matrix_UB_13      -0.078031
_diffrn_orient_matrix_UB_21      -0.126383
_diffrn_orient_matrix_UB_22      0.003037
_diffrn_orient_matrix_UB_23      0.00491
_diffrn_orient_matrix_UB_31      -0.009321
_diffrn_orient_matrix_UB_32      0.153024
_diffrn_orient_matrix_UB_33      -0.048731
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3532
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70399
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        12.27
_diffrn_reflns_theta_max         26.277
_diffrn_reflns_theta_min         0.935
_diffrn_source                   SPring-8
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.039
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.3191
_refine_diff_density_min         -0.2819
_refine_diff_density_rms         0.0439
_refine_ls_abs_structure_details
;
 Flack x determined using 6079 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.5401
_refine_ls_goodness_of_fit_gt    2.5401
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    61
_refine_ls_number_parameters     165
_refine_ls_number_reflns         13813
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.0067
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/\s(F)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0171
_refine_ls_wR_factor_gt          0.0171
_reflns_Friedel_coverage         0.84
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.911
_reflns_number_gt                13813
_reflns_number_total             14565
_reflns_threshold_expression     'F>0 & F/u(F)>4.0 & |F_calc|>10^-3'
_cod_data_source_file            d0ce00378f2.cif
_cod_data_source_block           4AP_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_cell_volume        472.648(14)
_cod_original_sg_symbol_Hall     'p 2yb'
_cod_original_sg_symbol_H-M      'p 1 21 1'
_cod_database_code               7240726
_shelx_estimated_absorpt_t_min   0.996
_shelx_estimated_absorpt_t_max   0.997
_refine_ls_coordinate_system     cartesian
_refine_ls_svd_threshold         0.1E-02