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_7249362
_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         'C25.5 H8.5 Fe4.25 O22.667'
_chemical_formula_sum            'C25.5 H8.5 Fe4.25 O22.67'
_chemical_formula_weight         914.85
_chemical_name_systematic        MIL100(Fe)
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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            192
_cell_length_a                   73.27(18)
_cell_length_b                   73.27(15)
_cell_length_c                   73.27(19)
_cell_measurement_temperature    100
_cell_volume                     393349(16)
_computing_cell_refinement       'CrystFEL (White, 2018)'
_computing_data_collection       MXCuBE
_computing_data_reduction        'CrystFEL (White, 2018)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'pixel array detector'
_diffrn_detector_area_resol_mean 0.075
_diffrn_detector_type            'DECTRIS EIGER-9M'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'MD2 microdiffractometer with MK3 mini-kappa'
_diffrn_measurement_method       'omega rotation shutterless scans'
_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     0.72931
_diffrn_reflns_av_R_equivalents  0.3472
_diffrn_reflns_av_unetI/netI     0.2573
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       1
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12742
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.358
_diffrn_reflns_theta_max         19.358
_diffrn_reflns_theta_min         0.494
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    0.825
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.742
_exptl_crystal_description       microcrystals
_exptl_crystal_F_000             87040
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0000016(4)
_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   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7092
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.1381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3477
_refine_ls_wR_factor_ref         0.4214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2723
_reflns_number_total             7092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00735b2.cif
_cod_data_source_block
mil100_gt16_suna20_3_detector_432_unity_3cycles_max321290_xdsconv_a
_cod_depositor_comments
'Adding full bibliography for 7249358--7249364.cif.'
_cod_original_cell_volume        393349(2899)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'C25.50 H8.50 Fe4.25 O22.67'
_cod_database_code               7249362
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C24-C23 = C25-C24 = C26-C25 = C26-C25_$1 = C25_$1-C24_$1 = C24_$1-C23
 1.39 with sigma of 0.02
 C24-C26 = C25_$1-C23
 2.42 with sigma of 0.02
 C25-C25_$1 = C24_$1-C24
 2.42 with sigma of 0.02
 C26-C24_$1 = C23-C25
 2.42 with sigma of 0.02
 C19-C16 = C15-C21
 2.42 with sigma of 0.02
 C21-C18 = C16-C14
 2.42 with sigma of 0.02
 C22-C23 = C22-O15L
 1.39 with sigma of 0.02
 C14-C19 = C18-C15
 2.42 with sigma of 0.02
 C5-C7_$2 = C8-C6
 2.42 with sigma of 0.02
 C6_$2-C8 = C7-C5
 2.42 with sigma of 0.02
 C7_$2-C7 = C6-C6_$2
 2.42 with sigma of 0.02
 C6_$2-C5 = C7_$2-C6_$2 = C8-C7_$2 = C8-C7 = C7-C6 = C6-C5
 1.39 with sigma of 0.02
 C29-C31 = C32-C30_$1
 2.42 with sigma of 0.02
 C30_$1-C30 = C31-C31_$1
 2.42 with sigma of 0.02
 C31_$1-C30_$1 = C30_$1-C29 = C30-C29 = C31-C30 = C32-C31 = C32-C31_$1
 1.39 with sigma of 0.02
 C31_$1-C29 = C30-C32
 2.42 with sigma of 0.02
 C2_$3-C1_$3 = C2_$3-C1_$4 = C2_$4-C1_$4 = C2_$4-C1 = C2-C1 = C2-C1_$3
 1.39 with sigma of 0.02
 C1_$4-C1 = C2-C2_$3
 2.42 with sigma of 0.02
 C1_$3-C1_$4 = C2_$4-C2
 2.42 with sigma of 0.02
 C2_$3-C2_$4 = C1-C1_$3
 2.42 with sigma of 0.02
 C23-C22 \\sim C27_$1-C25_$1 \\sim C27-C25
 with sigma of 0.02
 C20-C19 \\sim C17-C16 \\sim C14-C13
 with sigma of 0.02
3. Restrained planarity
 C22, C23, C24, C25, C27, C26, C25_$1, C27_$1, C24_$1
 with sigma of 0.1
 C4, C5, C6_$2, C7_$2, C9_$2, C8, C7, C9, C6
 with sigma of 0.1
 C33_$1, C31_$1, C30_$1, C29, C28, C30, C31, C33, C32
 with sigma of 0.1
 C3_$3, C2_$3, C1_$4, C2_$4, C3_$4, C1, C2, C3, C1_$3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C27 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C24 \\sim C25 \\sim C27 \\sim
C26: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C33 \\sim C31 \\sim C30 \\sim C29 \\sim C28 \\sim C30 \\sim C31 \\sim C33 \\sim
C32: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim C1 \\sim C2 \\sim C3 \\sim C1 \\sim C2 \\sim C3 \\sim C1:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C22) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C30(H30), C18(H18), C32(H32), C1(H1), C26(H26), C15(H15), C8(H8),
 C21(H21), C24(H24), C6(H6)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67520
_shelx_hkl_checksum              51251
_shelx_fab_checksum              40287
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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;