Overcoming the inadequacy of X-ray powder diffraction in reliable hydrogen location with the aid of first principles calculations: crystal structure determination of orotaldehyde monohydrate.
Guidoni, Leonardo; Gontrani, Lorenzo; Bencivenni, Luigi; Sadun, Claudia; Ballirano, Paolo; The journal of physical chemistry. A 113 (2009) 353–359; doi:10.1021/jp809076t

data_1516384
_publ_section_title
;
 Overcoming the inadequacy of X-ray powder diffraction in reliable
 hydrogen location with the aid of first principles calculations: crystal
 structure determination of orotaldehyde monohydrate.
;
_journal_issue                   1
_journal_name_full               'The journal of physical chemistry. A'
_journal_page_first              353
_journal_page_last               359
_journal_paper_doi               10.1021/jp809076t
_journal_volume                  113
_journal_year                    2009
_chemical_formula_sum            'C5 H6 N2 O4'
_chemical_formula_weight         158.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_date             2008-10-22T10:11
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
;
2008-10-22T10:11  Initial CIF as created by GSAS2CIF

2008-10-22 # Formatted by publCIF
;
_cell_angle_alpha                90.0
_cell_angle_beta                 111.0090(12)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   15.77423(27)
_cell_length_b                   8.07596(8)
_cell_length_c                   5.00886(8)
_cell_measurement_pressure       101.325
_cell_measurement_temperature    296(1)
_cell_volume                     595.671(16)
_computing_cell_refinement       GSAS
_computing_data_collection       DiffracPlus
_computing_structure_refinement  GSAS
_computing_structure_solution    'EXPO 2004'
_diffrn_ambient_pressure         101.325
_diffrn_ambient_temperature      296(1)
_diffrn_detector                 Vantec-1
_diffrn_detector_type            PSD
_diffrn_measurement_device_type  'AXS Bruker D8 Advance'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Sealed tube'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_meas      1.7(1)
_exptl_crystal_density_method    flotation
_pd_block_id
2008-10-22T10:11|4FURA_BIS_DIOLO_ADVA|p|Siemens_D5005
_pd_calc_method                  'Rietveld Refinement'
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.02151
_pd_meas_2theta_range_max        140.69606
_pd_meas_2theta_range_min        4.0
_pd_meas_number_of_points        6356
_pd_meas_scan_method             step
_pd_phase_name                   'Orotaldehyde Monohydrate'
_pd_proc_2theta_range_inc        0.02151
_pd_proc_2theta_range_max        140.69606
_pd_proc_2theta_range_min        4.0
_pd_proc_info_datetime           2008-10-22T10:11:41
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 32 terms.
 Shifted Chebyshev function of 1st kind
      1:    4214.26     2:   -2426.57     3:    1355.78     4:    105.371    
      5:   -309.214     6:    423.378     7:   -257.972     8:   -104.017    
      9:    444.303    10:   -553.109    11:    465.599    12:   -268.599    
     13:   -5.39316    14:    247.891    15:   -297.504    16:    215.760    
     17:   -84.8993    18:   -49.5779    19:    174.561    20:   -183.669    
     21:    104.167    22:   -14.1060    23:   -29.4390    24:    87.7132    
     25:   -94.9654    26:    71.2255    27:    5.82393    28:   -54.1032    
     29:    77.3530    30:   -47.9593    31:    22.5246    32:    6.96448    
;
_pd_proc_ls_peak_cutoff          0.00040
_pd_proc_ls_pref_orient_corr     'spherical harmonics'
_pd_proc_ls_profile_function
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 Peak tails are ignored  where the intensity is below 0.0004 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0234
_pd_proc_ls_prof_wR_expected     0.0133
_pd_proc_ls_prof_wR_factor       0.0308
_pd_proc_number_of_points        6356
_pd_proc_wavelength              1.540598
_pd_spec_mounting                Capillary
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.40
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     110
_refine_ls_number_restraints     85
_refine_ls_R_Fsqd_factor         0.04826
_refine_ls_R_I_factor            0.0357
_refine_ls_shift/su_max          0.08
_refine_ls_shift/su_mean         0.00
_refine_ls_weighting_scheme      sigma
_reflns_d_resolution_high        0.820
_reflns_d_resolution_low         7.363
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              6
_reflns_limit_l_min              -6
_reflns_number_total             2253
_cod_data_source_file            jp809076t_si_001.cif
_cod_data_source_block           4FURA_BIS_DIOLO_ADVA_publ
_cod_original_cell_volume        595.671(15)
_cod_database_code               1516384
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000