High-pressure single-crystal diffraction at the Australian Synchrotron.
Boer, Stephanie A.; Price, Jason R.; Riboldi-Tunnicliffe, Alan; Williamson, Rachel; Summers, Aston; Turner, Gemma F.; Jones, Isabelle; Bond, Charles; Vrielink, Alice; Marshall, Andrew C.; Hitchings, John; Moggach, Stephen A.; Journal of synchrotron radiation 30 (2023) 841–846; doi:10.1107/S160057752300406X

data_1569375
_publ_section_title
;
 High-pressure single-crystal diffraction at the Australian Synchrotron.
;
_journal_issue                   4
_journal_name_full               'Journal of synchrotron radiation'
_journal_page_first              841
_journal_page_last               846
_journal_paper_doi               10.1107/S160057752300406X
_journal_volume                  30
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C4 H9 N O3'
_chemical_formula_sum            'C4 H9 N O3'
_chemical_formula_weight         119.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1419(2)
_cell_length_b                   7.7217(4)
_cell_length_c                   13.613(5)
_cell_measurement_reflns_used    4402
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5260
_cell_measurement_theta_min      3.9800
_cell_volume                     540.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.512
_diffrn_measured_fraction_theta_max 0.501
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -2.00  69.00   0.50    3.00    --   24.20 -82.00-151.00  142
  2  \w     -8.00  63.00   0.50    3.00    --   24.20 -67.00  23.00  142
  3  \w    -48.00  -5.00   0.50    3.00    --   24.20 114.00 -45.00   86
  4  \w    -43.00  16.00   0.50    3.00    --   24.20  38.00-180.00  118
  5  \w    -29.00  -9.00   0.50    3.00    --   24.20  77.00 -30.00   40
  6  \w     68.00 106.00   0.50    3.00    --   24.20 178.00  90.00   76
  7  \w    -23.00  16.00   0.50    3.00    --   24.20  67.00 157.00   78
  8  \w    -48.00  -5.00   0.50    3.00    --   24.20 114.00 135.00   86
  9  \w    -30.00  39.00   0.50    3.00    --   24.20   0.00   0.00  138
 10  \w    -22.00  27.00   0.50    3.00    --   24.20 -19.00-180.00   98
 11  \w    -26.00  53.00   0.50    3.00    --  -24.59 -40.00-167.00  158
 12  \w    -27.00  27.00   0.50    3.00    --  -24.59  19.00-180.00  108
 13  \w     -4.00  18.00   0.50    3.00    --  -24.59 -57.00  30.00   44
 14  \w    -57.00  22.00   0.50    3.00    --  -24.59  53.00 -17.00  158
 15  \w    -29.00  -9.00   0.50    3.00    --   24.20  77.00   0.00   40
 16  \w     60.00 106.00   0.50    3.00    --   24.20 178.00 -90.00   92
 17  \w    -36.00 -16.00   0.50    3.00    --   24.20  38.00   0.00   40
 18  \w    -29.00  -9.00   0.50    3.00    --   24.20  77.00 150.00   40
 19  \w     30.00  71.00   0.50    3.00    --   24.20 -99.00-150.00   82
 20  \w    -36.00 -16.00   0.50    3.00    --  -24.59  38.00 -30.00   40
 21  \w    -35.00  44.00   0.50    3.00    --  -24.59 -13.00   3.00  158
 22  \w    -26.00  53.00   0.50    3.00    --  -24.59 -40.00  12.00  158
 23  \w    -32.00  47.00   0.50    3.00    --  -24.59 -26.00   8.00  158
 24  \w    -27.00  27.00   0.50    3.00    --  -24.59 -19.00-180.00  108
 25  \w    -38.00  -9.00   0.50    3.00    --  -24.59  77.00 -30.00   58
 26  \w    -36.00 -16.00   0.50    3.00    --  -24.59  38.00 150.00   40
 27  \w    -53.00  26.00   0.50    3.00    --  -24.59  40.00 -12.00  158
 28  \w    -57.00  22.00   0.50    3.00    --  -24.59  53.00 -17.00  158
 29  \w    -63.00  16.00   0.50    3.00    --  -24.59  67.00 -23.00  158
 30  \w    -69.00 -44.00   0.50    3.00    --  -24.59  82.00 -29.00   50
 31  \w    -44.00  35.00   0.50    3.00    --  -24.59  13.00  -3.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0012468000
_diffrn_orient_matrix_UB_12      -0.0239489000
_diffrn_orient_matrix_UB_13      0.0502806000
_diffrn_orient_matrix_UB_21      0.1028521000
_diffrn_orient_matrix_UB_22      0.0589588000
_diffrn_orient_matrix_UB_23      0.0094255000
_diffrn_orient_matrix_UB_31      -0.0919561000
_diffrn_orient_matrix_UB_32      0.0662543000
_diffrn_orient_matrix_UB_33      0.0098185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.512
_diffrn_reflns_Laue_measured_fraction_max 0.501
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7737
_diffrn_reflns_point_group_measured_fraction_full 0.517
_diffrn_reflns_point_group_measured_fraction_max 0.507
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         3.991
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         567
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0652P)^2^+0.2675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.653
_reflns_Friedel_fraction_full    0.524
_reflns_Friedel_fraction_max     0.515
_reflns_number_gt                482
_reflns_number_total             567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vy5009sup1.cif
_cod_data_source_block           threonine_150000kPa_lab
_cod_original_cell_volume        540.49(19)
_cod_database_code               1569375
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         'C4 H7 O3 N'
_chemical_oxdiff_usercomment     'L-threonine in tiny DAC'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 C3, O3, C2, C4, N1, C1, O1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C3(H3A), C2(H2)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
3.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              80465
_shelx_hkl_checksum              22538
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.504
_oxdiff_exptl_absorpt_empirical_full_min 0.703
_cod_database_fobs_code 1569375