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_2108757
_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          'C10 H11 N O3'
_chemical_formula_moiety         'C10 H11 N O3'
_chemical_formula_sum            'C10 H11 N O3'
_chemical_formula_weight         193.20
_chemical_name_systematic
;
10-Oxa-4-azatricyclo[5.2.1.0^2,6^]dec-8-ene-3,5-dione
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.68960(10)
_cell_length_b                   10.89100(10)
_cell_length_c                   9.59600(10)
_cell_measurement_reflns_used    25673
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      71.4200
_cell_measurement_theta_min      4.5720
_cell_volume                     908.150(16)
_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      99.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -92.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000    0.0000 134

  2 omega  -42.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -30.0000 134

  3 omega    1.00   51.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 50

  4 omega  -49.00   -3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0000  127.0000  176.4400 46

  5 omega    1.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   93.0000 -167.3709 26

  6 omega -146.00  -73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0202 -125.0000  -90.0000 73

  7 omega   11.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202   84.0000  -15.8115 27

  8 omega   94.00  146.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202  125.0000    0.0000 52

  9 omega   11.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202   77.0000  -60.0000 144

 10 omega   23.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202 -125.0000   30.0000 98

 11 omega   11.00   38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202   84.0000   93.6643 27

 12 omega   11.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202   77.0000   60.0000 144

 13 omega   18.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   82.0000  128.6944 27

 14 omega   19.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000   85.2987 139

 15 omega   18.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   82.0000 -163.3698 27

 16 omega   23.00  165.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   74.0000  -45.3897 142

 17 omega   23.00  161.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   67.0000   25.6630 138

 18 omega   27.00  170.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -139.0424 143

 19 omega   27.00  170.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000   55.8475 143

 20 omega   27.00  170.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  151.9117 143

 21 omega   35.00  175.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000  -38.1861 140

 22 omega   46.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   63.0000 -107.5137 132

 23 omega   46.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   65.0000 -156.8402 132

 24 omega   51.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   61.0000   65.4074 127

 25 omega   66.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   63.0000 -180.0000 112

 26 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000  -30.0000 111

 27 omega   18.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405 -111.0000   90.0000 97

 28 omega   57.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  178.0000  120.0000 93

 29 omega   68.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   50.0000   60.0000 110

 30 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000  -90.0000 111

 31 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000   90.0000 111

 32 omega   57.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  178.0000  -90.0000 93

 33 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000  120.0000 111

 34 omega   66.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   63.0000  -90.0000 112

 35 omega   18.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405 -111.0000  -90.0000 97

 36 omega   66.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   63.0000  120.0000 112

 37 omega   68.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   50.0000 -180.0000 110

 38 omega   19.00  152.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  -50.0000 -150.0000 133

 39 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000   60.0000 111

 40 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   70.0000 -130.3790 111

 41 omega   66.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   63.0000 -150.0000 112

 42 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000    0.0000 111

 43 omega   67.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   77.0000  -60.0000 111

 44 omega  100.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  111.0000 -120.0000 78

 45 omega   57.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  178.0000   90.0000 93

 46 omega  100.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  111.0000  -30.0000 78

 47 omega -100.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -180.0000 200

 48 omega  -42.00   92.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 134

 49 omega -100.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -120.0000 200

 50 omega -100.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -150.0000 200

 51 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000    0.0000 200

 52 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000 -180.0000 200

 53 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000  -90.0000 200

 54 omega   10.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202   85.0000  132.9204 26

 55 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000  -60.0000 200

 56 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000 -120.0000 200

 57 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000  -30.0000 200

 58 omega   11.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202   77.0000 -180.0000 144

 59 omega  -45.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0202    0.0000 -150.0000 200

 60 omega   14.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   82.0000 -130.0705 31

 61 omega   15.00  153.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   67.0000    0.8287 138

 62 omega   19.00  161.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   74.0000   38.8007 142

 63 omega   19.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   69.0000  -70.8977 139

 64 omega   23.00  162.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   69.0000   73.3363 139

 65 omega   35.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000  -92.0338 138

 66 omega   35.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   66.0000 -147.6287 138

 67 omega   68.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   50.0000  -30.0000 110

 68 omega  100.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  111.0000 -150.0000 78

 69 omega   66.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   63.0000   90.0000 112

 70 omega   66.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405   63.0000  -30.0000 112

 71 omega  100.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0405  111.0000   60.0000 78
;
_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      0.1388668000
_diffrn_orient_matrix_UB_12      -0.0865851000
_diffrn_orient_matrix_UB_13      -0.0171927000
_diffrn_orient_matrix_UB_21      -0.0327662000
_diffrn_orient_matrix_UB_22      -0.0558759000
_diffrn_orient_matrix_UB_23      0.1444346000
_diffrn_orient_matrix_UB_31      -0.1051918000
_diffrn_orient_matrix_UB_32      -0.0969017000
_diffrn_orient_matrix_UB_33      -0.0679964000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0075
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31209
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.480
_diffrn_reflns_theta_min         5.090
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.5090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1728
_reflns_number_total             1767
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {1e07f431-b684-401e-b284-2a2267f32c98}
_cod_data_source_file            px5028sup1.cif
_cod_data_source_block           1Cu
_cod_database_code               2108757
_cod_database_fobs_code          2108757
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         C10H11NO3
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.779
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1N), C3(H3), C4(H4)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_olex2_date_sample_data_collection 2017-07-11
_olex2_submission_special_instructions 'No special instructions were received'