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_1569376
_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
_chemical_name_common            L-threonine
_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                   5.1489(5)
_cell_length_b                   7.7304(5)
_cell_length_c                   13.602(6)
_cell_measurement_reflns_used    4230
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      3.0
_cell_volume                     541.4(2)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_pressure         150000
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.447
_diffrn_measured_fraction_theta_max 0.373
_diffrn_measurement_device_type  MX1
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0134
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.447
_diffrn_reflns_Laue_measured_fraction_max 0.373
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_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            1209
_diffrn_reflns_point_group_measured_fraction_full 0.450
_diffrn_reflns_point_group_measured_fraction_max 0.369
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.710
_diffrn_reflns_theta_min         3.031
_diffrn_source_type              'MX1 Beamline Australian Synchrotron'
_diffrn_standards_decay_%        0.0(1)
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction.'
_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    1.461
_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         0.217
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 157 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         468
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0507
_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^)+(0.0720P)^2^+0.4786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.631
_reflns_Friedel_fraction_full    0.454
_reflns_Friedel_fraction_max     0.362
_reflns_number_gt                428
_reflns_number_total             468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vy5009sup1.cif
_cod_data_source_block           threonine_150000kPa
_cod_original_cell_volume        541.4(3)
_cod_database_code               1569376
_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. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C2)
3. Rigid body (RIGU) restrains
 C3, O3, C2, C4, N1, C1, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C3(H3A), C2(H2)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              97250
_shelx_hkl_checksum              93938
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 1569376