High-pressure sapphire capillary cell for synchrotron single-crystal X-ray diffraction measurements to 1500 bar
McMonagle, Charles J.; Allan, David R.; Warren, Mark R.; Kamenev, Konstantin V.; Turner, Gemma F.; Moggach, Stephen A.; Journal of Applied Crystallography 53 (2020) 1519–1523; doi:10.1107/S1600576720013710

data_2300672
_publ_section_title
;
 High-pressure sapphire capillary cell for synchrotron single-crystal
 X-ray diffraction measurements to 1500 bar
;
_journal_coeditor_code           KC5114SUP1
_journal_issue                   6
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              1519
_journal_page_last               1523
_journal_paper_doi               10.1107/S1600576720013710
_journal_volume                  53
_journal_year                    2020
_chemical_formula_moiety         'C6 D12 N4'
_chemical_formula_sum            'C6 D12 N4'
_chemical_formula_weight         152.27
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-06-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.01950(10)
_cell_length_b                   7.01950(10)
_cell_length_c                   7.01950(10)
_cell_measurement_reflns_used    1376
_cell_measurement_temperature    297
_cell_measurement_theta_max      29
_cell_measurement_theta_min      4
_cell_volume                     345.874(9)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_unetI/netI     0.0061
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1374
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.190
_diffrn_reflns_theta_min         5.811
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.088
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.023
_refine_ls_abs_structure_details
;
 Flack x determined using 30 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     8
_refine_ls_number_reflns         83
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0436P)^2^+0.0602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.627
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                80
_reflns_number_total             83
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            kc5114sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2300672.cif.'
_cod_original_cell_volume        345.875(15)
_cod_database_code               2300672
_cod_database_fobs_code          2300672
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: D2A(0.25) D2B(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C2(D2A,D2B)
;
_shelx_res_checksum              56334
_shelx_hkl_checksum              5443
_olex2_submission_special_instructions 'No special instructions were received'