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_7249361
_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 H12.5 Fe4.25 O22.667'
_chemical_formula_sum            'C25.5 H12.5 Fe4.25 O22.67'
_chemical_formula_weight         918.88
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-20
_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                   73.09(18)
_cell_length_b                   73.09(14)
_cell_length_c                   73.09(18)
_cell_measurement_temperature    100
_cell_volume                     390458(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      100.00
_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  0.1161
_diffrn_reflns_av_unetI/netI     0.0917
_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       46
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12623
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.351
_diffrn_reflns_theta_max         19.351
_diffrn_reflns_theta_min         0.495
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    0.831
_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    0.750
_exptl_crystal_description       microcrystals
_exptl_crystal_F_000             87808
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0000006(3)
_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   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         7027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1816P)^2^+907.4545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2744
_refine_ls_wR_factor_ref         0.2997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4882
_reflns_number_total             7027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00735b2.cif
_cod_data_source_block
mil100_suna20_4_unity_3cycles_xdsconv_a_solventmask
_cod_depositor_comments
'Adding full bibliography for 7249358--7249364.cif.'
_cod_original_cell_volume        390458(2885)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'C25.50 H12.50 Fe4.25 O22.67'
_cod_database_code               7249361
_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 O(H,H) groups
2. Others
 Fixed Sof: H4WA(0.5) H4WB(0.5) H7WA(0.5) H7WB(0.5)
3.a Rotating group:
 O3W(H3WA,H3WB), O4W(H4WA,H4WB), O7W(H7WA,H7WB)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C28(H28), C24(H24), C15(H15), C21(H21), C18(H18), C4(H4), C10(H10),
 C3(H3), C33(H33), C27(H27)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46009
_shelx_hkl_checksum              31082
_shelx_fab_checksum              54623
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;