#------------------------------------------------------------------------------
#$Date: 2025-07-01 14:34:05 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1294 $
#$URL: svn://crystallography.net/testcod/cif/1/00/00/1000024.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1000024
loop_
_publ_author_name
'Guidoni, Leonardo'
'Gontrani, Lorenzo'
'Bencivenni, Luigi'
'Sadun, Claudia'
'Ballirano, Paolo'
_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
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_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.
 #1(GU)   = 1171.620 #2(GV)   = -488.418 #3(GW)   =   81.222
 #4(GP)   =    0.000 #5(LX)   =   12.659 #6(LY)   =    0.000
 #7(S/L)  =   0.0120 #8(H/L)  =   0.0114
 #9(trns) =     0.00 #10(shft)=  -5.7664
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.000 #15(L22) =    0.000 #16(L33) =    0.000
 #17(L12) =    0.000 #18(L13) =    0.000 #19(L23) =    0.000
 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               1000024
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x+1/2,+y+1/2,-z
-1 -x,-y,-z
-2 +x+1/2,-y+1/2,+z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
O O1 0.38658(10) 0.07428(23) 0.7016(4) 1.0 Uiso 0.03159(14) 4
C C2 0.43669(16) 0.15834(33) 0.6038(5) 1.0 Uiso 0.03159(14) 4
N N3 0.39441(12) 0.24462(27) 0.3519(5) 1.0 Uiso 0.03159(14) 4
H H4 0.3361(5) 0.1876(12) 0.1965(20) 1.0 Uiso 0.05 4
C C5 0.43816(16) 0.34616(32) 0.2205(5) 1.0 Uiso 0.03159(14) 4
O O6 0.39931(11) 0.41857(26) -0.0051(4) 1.0 Uiso 0.03159(14) 4
N N7 0.53437(14) 0.34445(28) 0.3482(4) 1.0 Uiso 0.03159(14) 4
H H8 0.5649(4) 0.4253(11) 0.2521(15) 1.0 Uiso 0.05 4
C C9 0.57808(15) 0.26454(33) 0.6031(6) 1.0 Uiso 0.03159(14) 4
C C10 0.53356(17) 0.16972(31) 0.7319(5) 1.0 Uiso 0.03159(14) 4
H H11 0.5626(5) 0.1505(13) 0.9646(11) 1.0 Uiso 0.05 4
C C12 0.68079(16) 0.27062(32) 0.7149(5) 1.0 Uiso 0.03159(14) 4
O O13 0.29725(11) 0.58833(24) 0.41008(33) 1.0 Uiso 0.03159(14) 4
H H14 0.2303(4) 0.5956(14) 0.3851(24) 1.0 Uiso 0.05 4
O O15 0.29001(12) 0.70770(21) 0.9826(4) 1.0 Uiso 0.03159(14) 4
H H16 0.3097(7) 0.5984(9) 0.9455(18) 1.0 Uiso 0.05 4
H H17 0.2110(5) 0.3429(8) 0.6692(18) 1.0 Uiso 0.05 4
loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
O 16.0 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
C 20.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
N 8.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
H 24.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081
57.7997 0.00304 International_Tables_Vol_C
I 0.0 0.000 0.000 20.1472 4.34700 18.9949 0.38140 7.51380 27.7660 2.27350
66.8776 4.07120 International_Tables_Vol_C
loop_
_diffrn_radiation_wavelength
_diffrn_radiation_wavelength_wt
_diffrn_radiation_type
_diffrn_radiation_wavelength_id
1.540598 1.000 K\a~1~ 1
1.544390 0.500 K\a~2~ 2
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C2 N3 117.30(20) 1_555 . 1_555 n
O1 C2 C10 125.08(22) 1_555 . 1_555 n
N3 C2 C10 117.62(24) 1_555 . 1_555 n
C2 N3 H4 116.9(6) 1_555 . 1_555 n
C2 N3 C5 124.96(19) 1_555 . 1_555 n
H4 N3 C5 110.7(6) 1_555 . 1_555 n
N3 C5 O6 123.60(21) 1_555 . 1_555 n
N3 C5 N7 114.55(20) 1_555 . 1_555 n
O6 C5 N7 121.40(25) 1_555 . 1_555 n
C5 N7 H8 112.8(4) 1_555 . 1_555 n
C5 N7 C9 121.46(23) 1_555 . 1_555 n
H8 N7 C9 124.7(4) 1_555 . 1_555 n
N7 C9 C10 122.46(20) 1_555 . 1_555 n
N7 C9 C12 116.25(24) 1_555 . 1_555 n
C10 C9 C12 120.86(22) 1_555 . 1_555 n
C2 C10 C9 118.47(21) 1_555 . 1_555 n
C2 C10 H11 115.9(5) 1_555 . 1_555 n
C9 C10 H11 119.8(5) 1_555 . 1_555 n
C9 C12 O13 105.32(19) 1_555 . -1_666 n
C9 C12 O15 106.99(23) 1_555 . -1_667 n
C9 C12 H17 112.6(4) 1_555 . -2_665 n
O13 C12 O15 109.69(19) -1_666 . -1_667 n
O13 C12 H17 113.0(5) -1_666 . -2_665 n
O15 C12 H17 109.0(5) -1_667 . -2_665 n
C12 O13 H14 108.0(7) -1_666 . 1_555 n
C12 O15 H16 108.0(5) -1_667 . 1_555 n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.2663(35) . 1_555 n
O1 H14 1.744(6) . 2_546 n
C2 O1 1.2663(35) . 1_555 n
C2 N3 1.3852(33) . 1_555 n
C2 C10 1.4326(33) . 1_555 n
N3 C2 1.3852(33) . 1_555 n
N3 H4 1.072(8) . 1_555 n
N3 C5 1.381(4) . 1_555 n
H4 N3 1.072(8) . 1_555 n
H4 C5 2.026(10) . 1_555 n
H4 O15 1.873(8) . 2_546 n
C5 N3 1.381(4) . 1_555 n
C5 H4 2.026(10) . 1_555 n
C5 O6 1.2239(28) . 1_555 n
C5 N7 1.4201(30) . 1_555 n
C5 H8 2.050(8) . 1_555 n
O6 C5 1.2239(28) . 1_555 n
O6 H8 1.985(9) . -1_665 n
O6 H16 1.979(9) . 1_554 n
N7 C5 1.4201(30) . 1_555 n
N7 H8 1.028(9) . 1_555 n
N7 C9 1.3751(32) . 1_555 n
H8 C5 2.050(8) . 1_555 n
H8 O6 1.985(9) . -1_665 n
H8 N7 1.028(9) . 1_555 n
C9 N7 1.3751(32) . 1_555 n
C9 C10 1.349(4) . 1_555 n
C9 C12 1.5134(32) . 1_555 n
C10 C2 1.4326(33) . 1_555 n
C10 C9 1.349(4) . 1_555 n
C10 H11 1.100(6) . 1_555 n
H11 C10 1.100(6) . 1_555 n
C12 C9 1.5134(32) . 1_555 n
C12 O13 1.4019(33) . -1_666 n
C12 H14 1.972(10) . -1_666 n
C12 O15 1.4275(30) . -1_667 n
C12 H16 1.962(9) . -1_667 n
C12 H17 1.095(8) . -2_555 n
O13 C12 1.4019(33) . -1_666 n
O13 H14 1.020(7) . 1_555 n
H14 O1 1.744(6) . 2_556 n
H14 C12 1.972(10) . -1_666 n
H14 O13 1.020(7) . 1_555 n
O15 H4 1.873(8) . 2_556 n
O15 C12 1.4275(30) . -1_667 n
O15 H16 0.975(8) . 1_555 n
O15 H17 2.063(9) . 2_557 n
H16 O6 1.979(9) . 1_556 n
H16 C12 1.962(9) . -1_667 n
H16 O15 0.975(8) . 1_555 n
H17 C12 1.095(8) . -2_455 n
H17 O15 2.063(9) . 2_547 n
loop_
_pd_meas_counts_total
_pd_proc_ls_weight
_pd_proc_intensity_bkg_calc
_pd_calc_intensity_total
8159.0 0.0 1323691.87500 .
8087.0 0.0 1288801.50000 .
8061.0 0.0 1254743.50000 .
8005.0 0.0 1221500.87500 .
7996.0 0.0 1189054.12500 .
7963.0 0.0 1157386.37500 .
7917.0 0.0 1126483.62500 .
7890.0 0.0 1096327.87500 .
7917.0 0.0 1066901.50000 .
7943.0 0.0 1038189.62500 .
8049.0 0.0 1010176.68750 .
7928.0 0.0 982849.62500 .
7769.0 0.0 956189.50000 .
7718.0 0.0 930184.18750 .
7900.0 0.0 904818.37500 .
7801.0 0.0 880079.75000 .
7790.0 0.0 855952.43750 .
7733.0 0.0 832423.68750 .
7617.0 0.0 809479.81250 .
7566.0 0.0 787108.62500 .
7602.0 0.0 765296.62500 .
7570.0 0.0 744031.93750 .
7653.0 0.0 723301.56250 .
7678.0 0.0 703094.12500 .
7423.0 0.0 683397.87500 .
7572.0 0.0 664200.93750 .
7465.0 0.0 645492.06250 .
7468.0 0.0 627260.43750 .
7481.0 0.0 609494.81250 .
7595.0 0.0 592185.43750 .
7493.0 0.0 575320.81250 .
7454.0 0.0 558891.12500 .
7729.0 0.0 542886.56250 .
7495.0 0.0 527297.75000 .
7487.0 0.0 512113.81250 .
7501.0 0.0 497326.59375 .
7560.0 0.0 482926.21875 .
7446.0 0.0 468904.31250 .
7455.0 0.0 455251.59375 .
7623.0 0.0 441959.21875 .
7526.0 0.0 429019.12500 .
7524.0 0.0 416422.71875 .
7741.0 0.0 404162.65625 .
7587.0 0.0 392230.09375 .
7309.0 0.0 380617.15625 .
7633.0 0.0 369317.09375 .
7544.0 0.0 358321.96875 .
7630.0 0.0 347625.09375 .
7491.0 0.0 337217.96875 .
7553.0 0.0 327094.53125 .
7537.0 0.0 317247.84375 .
7581.0 0.0 307671.68750 .
7514.0 0.0 298358.37500 .
7549.0 0.0 289302.28125 .
7383.0 0.0 280496.93750 .
7613.0 0.0 271936.34375 .
7640.0 0.0 263614.46875 .
7681.0 0.0 255525.31250 .
7606.0 0.0 247663.10938 .
7600.0 0.0 240022.20313 .
7434.0 0.0 232597.43750 .
7486.0 0.0 225383.25000 .
7476.0 0.0 218373.92188 .
7633.0 0.0 211565.00000 .
7572.0 0.0 204951.26563 .
7383.0 0.0 198527.39063 .
7511.0 0.0 192288.92188 .
7606.0 0.0 186231.10938 .
7506.0 0.0 180349.59375 .
7664.0 0.0 174639.07813 .
7559.0 0.0 169096.15625 .
7438.0 0.0 163715.82813 .
7489.0 0.0 158494.23438 .
7657.0 0.0 153427.10938 .
7461.0 0.0 148510.53125 .
7622.0 0.0 143740.43750 .
7598.0 0.0 139113.34375 .
7529.0 0.0 134625.04688 .
7546.0 0.0 130272.13281 .
7685.0 0.0 126050.96094 .
7538.0 0.0 121958.07813 .
7634.0 0.0 117990.21875 .
7692.0 0.0 114143.75781 .
7576.0 0.0 110415.53906 .
7635.0 0.0 106802.50781 .
7665.0 0.0 103301.42188 .
7529.0 0.0 99909.33594 .
7657.0 0.0 96623.22656 .
7536.0 0.0 93440.20313 .
7617.0 0.0 90357.51563 .
7635.0 0.0 87372.27344 .
7560.0 0.0 84481.82031 .
7538.0 0.0 81683.72656 .
7674.0 0.0 78975.42188 .
7706.0 0.0 76353.96094 .
7667.0 0.0 73817.35156 .
7533.0 0.0 71363.08594 .
7612.0 0.0 68988.78906 .
7778.0 0.0 66692.23438 .
7746.0 0.0 64471.15625 .
7804.0 0.0 62323.55469 .
7719.0 0.0 60247.13281 .
7542.0 0.0 58239.96875 .
7695.0 0.0 56299.99609 .
7701.0 0.0 54425.30859 .
7729.0 0.0 52613.95313 .
7765.0 0.0 50864.16016 .
7807.0 0.0 49174.01563 .
7804.0 0.0 47541.80078 .
7792.0 0.0 45965.83594 .
7857.0 0.0 44444.41797 .
7685.0 0.0 42975.87500 .
7584.0 0.0 41558.68750 .
7631.0 0.0 40191.29688 .
7606.0 0.0 38872.12500 .
7573.0 0.0 37599.76953 .
7619.0 0.0 36372.80078 .
7612.0 0.0 35189.83203 .
7698.0 0.0 34049.40234 .
7589.0 0.0 32950.32031 .
7769.0 0.0 31891.22656 .
7742.0 0.0 30870.90625 .
7608.0 0.0 29888.08594 .
7738.0 0.0 28941.63672 .
7869.0 0.0 28030.36914 .
7881.0 0.0 27153.20898 .
7833.0 0.0 26308.97852 .
7954.0 0.0 25496.69336 .
7845.0 0.0 24715.25977 .
7816.0 0.0 23963.71680 .
7855.0 0.0 23241.06250 .
7735.0 0.0 22546.34961 .
7861.0 0.0 21878.64258 .
7841.0 0.0 21237.05859 .
7802.0 0.0 20620.72852 .
7738.0 0.0 20028.77930 .
7720.0 0.0 19460.42188 .
7817.0 0.0 18914.79297 .
7769.0 0.0 18391.18555 .
7931.0 0.0 17888.78320 .
7886.0 0.0 17406.87109 .
7908.0 0.0 16944.74609 .
7685.0 0.0 16501.71875 .
7876.0 0.0 16077.10059 .
7838.0 0.0 15670.23145 .
7911.0 0.0 15280.48535 .
7971.0 0.0 14907.26270 .
7799.0 0.0 14549.95215 .
7821.0 0.0 14207.97363 .
7820.0 0.0 13880.75684 .
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7855.0 0.0 13268.49902 .
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