HAR, TAAM and BODD refinements of model crystal structures using Cu~<i>K</i>α and Mo~<i>K</i>α X-ray diffraction data
Wanat, Monika; Malinska, Maura; Gutmann, Matthias J.; Cooper, Richard I.; Wozniak, Krzysztof; Acta Crystallographica Section B 77 (2021) –; doi:10.1107/S2052520620014936

data_2108760
_publ_section_title
;
 HAR, TAAM and BODD refinements of model crystal structures using
 Cu~<i>K</i>\a and Mo~<i>K</i>\a X-ray diffraction data
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620014936
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C5 H6 N2 O2'
_chemical_formula_moiety         'C5 H6 N2 O2'
_chemical_formula_sum            'C5 H6 N2 O2'
_chemical_formula_weight         126.12
_chemical_name_common            Methyluracil
_chemical_name_systematic
;
1-Methylpyrimidine-2,4(1<i>H</i>,3<i>H</i>)-dione
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.16430(10)
_cell_length_b                   13.1840(2)
_cell_length_c                   6.2067(2)
_cell_measurement_reflns_used    14193
_cell_measurement_temperature    123
_cell_measurement_theta_max      51.9760
_cell_measurement_theta_min      2.1750
_cell_volume                     1077.22(4)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega    6.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000 -132.0000  -24.6169 26

  2 omega   49.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951  160.0000  -30.0000 56

  3 omega   13.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   57.0000 -120.0000 89

  4 omega   13.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   57.0000  -60.0000 89

  5 omega    8.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   37.0000 -150.0000 98

  6 omega  -35.00   55.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951  -57.0000  -30.0000 90

  7 omega   49.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951  160.0000  -90.0000 56

  8 omega    8.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   37.0000   60.0000 98

  9 omega    3.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951 -127.0000 -159.0000 89

 10 omega    4.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   77.0000  -60.0000 100

 11 omega   49.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951  160.0000 -150.0000 56

 12 omega    4.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   77.0000  120.0000 100

 13 omega    8.00  106.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   37.0000  150.0000 98

 14 omega    4.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   77.0000   30.0000 100

 15 omega   21.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951 -160.0000  120.0000 89

 16 omega   13.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951   57.0000 -150.0000 89

 17 omega   21.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6951 -160.0000    0.0000 89

 18 omega   69.00  158.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   76.0000   70.3378 89

 19 omega   73.00  158.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   70.0000   55.8682 85

 20 omega   70.00  158.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   74.0000   -9.7276 88

 21 omega   27.00  115.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342 -111.0000  -90.0000 88

 22 omega   26.00   69.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -30.0000  -60.0000 43

 23 omega   29.00  129.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -77.0000   30.0000 100

 24 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000   30.0000 89

 25 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000 -120.0000 89

 26 omega   27.00  109.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -94.0000  -60.0000 82

 27 omega   72.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   71.0000  -66.0139 86

 28 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   76.0000  108.8212 89

 29 omega   77.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000  -90.0000 81

 30 omega   31.00  121.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -61.0000  150.0000 90

 31 omega   72.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   71.0000  162.5858 86

 32 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000    0.0000 89

 33 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000   90.0000 89

 34 omega   72.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   71.0000 -159.4844 86

 35 omega   74.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   40.0000   49.1326 84

 36 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  150.0000 89

 37 omega   28.00   77.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342  -45.0000   30.0000 49

 38 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  -30.0000 89

 39 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000  120.0000 89

 40 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000   60.0000 89

 41 omega   77.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000 -180.0000 81

 42 omega   77.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000   30.0000 81

 43 omega   77.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000  -30.0000 81

 44 omega   77.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000  150.0000 81

 45 omega   28.00  122.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342 -127.0000 -159.0000 94

 46 omega   75.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   45.0000 -150.0000 83

 47 omega   69.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   77.0000 -150.0000 89

 48 omega   77.00   91.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       98.8342   61.0000   60.0000 14
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova Dual four-circle diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0455760000
_diffrn_orient_matrix_UB_12      -0.0286798000
_diffrn_orient_matrix_UB_13      0.0018678000
_diffrn_orient_matrix_UB_21      -0.0287123000
_diffrn_orient_matrix_UB_22      -0.0454165000
_diffrn_orient_matrix_UB_23      0.0060742000
_diffrn_orient_matrix_UB_31      -0.0007814000
_diffrn_orient_matrix_UB_32      -0.0028671000
_diffrn_orient_matrix_UB_33      -0.1141432000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3266
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         52.155
_diffrn_reflns_theta_min         2.186
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         3266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2580
_reflns_number_total             3266
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {7d115f4e-0e1c-418f-bb17-17e4bb266278}
_cod_data_source_file            px5028sup1.cif
_cod_data_source_block           3Mo
_cod_database_code               2108760
_cod_database_fobs_code          2108760
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C5H6N2O2
_exptl_absorpt_special_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H1), C3(H2), C4(H3)
;
_olex2_date_sample_data_collection 2018-04-10
_olex2_submission_special_instructions 'No special instructions were received'