Elucidating metal–organic framework structures using synchrotron serial crystallography
De Zitter, Elke; Perl, David; Savko, Martin; Paley, Daniel W.; Thom, Alexander J.; Jeangerard, Damien; Brewster, Aaron S.; Tissot, Antoine; Serre, Christian; Shepard, William; CrystEngComm 26 (2024) 5644–5654; doi:10.1039/D4CE00735B

data_7249359
_publ_section_title
;
 Elucidating metal--organic framework structures using synchrotron serial
 crystallography
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5644
_journal_page_last               5654
_journal_paper_doi               10.1039/D4CE00735B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C8 H10 N4 Zn'
_chemical_formula_sum            'C8 H10 N4 Zn'
_chemical_formula_weight         227.57
_chemical_name_common            ZIF-8
_chemical_name_systematic        Zn(mim)2
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-05-06 deposited with the CCDC.	2024-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   16.902
_cell_length_b                   16.902
_cell_length_c                   16.902
_cell_measurement_reflns_used    19
_cell_measurement_temperature    100
_cell_measurement_theta_max      7.647
_cell_measurement_theta_min      1.747
_cell_volume                     4828.523
_computing_data_collection       MXCuBE
_computing_data_reduction
;
CCTBX: Grosse-Kunstleve RW, Sauter NK, Moriarty NW, Adams PD: The Computational
Crystallography Toolbox: crystallographic algorithms in a reusable software
framework. J Appl Crystallogr. 2002, 35: 126-136. 10.1107/S0021889801017824.

DIALS: Waterman DG, Winter G, Parkhurst JM, Fuentes-Montero L, Hattne J,
Brewster A, Sauter NK, Evans G. CCP4 Newsletter on Protein Crystallography 49,
16-19 (2013).

cctbx.small_cell: Brewster AS, Sawaya MR, Rodriguez J, Hattne J, Echols N,
McFarlane HT, Cascio D, Adams PD, Eisenberg DS, Sauter NK. Acta Cryst. D71,
357-366 (2015). 10.1107/S1399004714026145.
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_type            'DECTRIS EIGER-9M'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'MD2 microdiffractometer with MK3 mini-kappa'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation
'0.010 mm x 0.005 mm (H*V, FWHM) KB focusing mirrors'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.730
_diffrn_reflns_av_unetI/netI     0.1242
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_number            431
_diffrn_reflns_point_group_measured_fraction_full 0.541
_diffrn_reflns_point_group_measured_fraction_max 0.541
_diffrn_reflns_theta_full        25.383
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_min         1.750
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    1.602
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_density_diffrn    0.939
_exptl_crystal_description       microcrystals
_exptl_crystal_F_000             1392
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.11(10)
_refine_ls_extinction_coef       0.0038(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0929
_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^)+(0.1548P)^2^+5.4305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2456
_refine_ls_wR_factor_ref         0.2672
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                361
_reflns_number_total             431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00735b2.cif
_cod_data_source_block           zif8_dwp_edz
_cod_depositor_comments
'Adding full bibliography for 7249358--7249364.cif.'
_cod_original_cell_volume        4828.2
_cod_database_code               7249359
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              88040
_shelx_hkl_checksum              663
_shelx_fab_checksum              18734
_olex2_submission_special_instructions 'No special instructions were received'