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_7249364
_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             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            192
_cell_length_a                   72.89(16)
_cell_length_b                   72.89(16)
_cell_length_c                   72.89(16)
_cell_measurement_temperature    100
_cell_volume                     387261(15)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       MXCuBE
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.826
_diffrn_reflns_av_R_equivalents  0.3623
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -67
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            665282
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.878
_diffrn_reflns_theta_max         22.878
_diffrn_reflns_theta_min         0.562
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    1.189
_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    0.753
_exptl_crystal_description       microcrystals
_exptl_crystal_F_000             87040
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0000005(1)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7717
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1143P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5779
_reflns_number_total             7717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00735b2.cif
_cod_data_source_block
mil100_sample3_mc_mc2_sg225_unmerged_a_solventmask
_cod_depositor_comments
'Adding full bibliography for 7249358--7249364.cif.'
_cod_original_cell_volume        387261(2534)
_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               7249364
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Fe02-O3W \\sim Fe03-O1W \\sim Fe04-O4W \\sim Fe05-O5W \\sim Fe06-O2W \\sim
Fe07-O6W \\sim Fe01-O7W
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Fe01) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C18(H18), C5(H5), C26(H26), C14(H14), C19(H19), C33(H33), C3(H3),
 C24(H24), C7(H7), C12(H12)
;
_shelx_res_checksum              44913
_shelx_hkl_checksum              58508
_shelx_fab_checksum              19897
_olex2_submission_special_instructions 'No special instructions were received'