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_7249363
_publ_section_title
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 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             2022-06-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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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                   73.2(6)
_cell_length_b                   73.2(6)
_cell_length_c                   73.2(6)
_cell_measurement_temperature    100
_cell_volume                     392223(6)
_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    'olex2.solve 1.5 (Bourhis et al., 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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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     0.729
_diffrn_reflns_av_R_equivalents  0.7031
_diffrn_reflns_av_unetI/netI     0.1592
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            142408
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        16.282
_diffrn_reflns_theta_max         16.282
_diffrn_reflns_theta_min         0.494
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    0.827
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    0.743
_exptl_crystal_description       microcrystals
_exptl_crystal_F_000             87040
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0000054(5)
_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   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2250
_reflns_number_total             4287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00735b2.cif
_cod_data_source_block
mil100gt16_sample7_mc_sg225_unmerged_a_solventmask
_cod_depositor_comments
'Adding full bibliography for 7249358--7249364.cif.'
_cod_original_cell_volume        392384(9036)
_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               7249363
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C20-C18 = C16-C18 = C16-C15 = C15-C14 = C19-C14 = C19-C20
 1.39 with sigma of 0.02
 C11-C10_$2 = C10_$2-C8_$2 = C9-C8_$2 = C9-C8 = C10-C8 = C11-C10
 1.39 with sigma of 0.02
 C20-C16 = C15-C19
 2.42 with sigma of 0.02
 C10_$2-C9 = C8-C11
 2.42 with sigma of 0.02
 C18-C15 = C14-C20
 2.42 with sigma of 0.02
 C16-C14 = C19-C18
 2.42 with sigma of 0.02
 C11-C8_$2 = C9-C10
 2.42 with sigma of 0.02
 C28_$1-C29 = C28-C29 = C26-C28 = C26-C27 = C26_$1-C27 = C26_$1-C28_$1
 1.39 with sigma of 0.02
 C10-C10_$2 = C8_$2-C8
 2.42 with sigma of 0.02
 C28_$1-C28 = C26-C26_$1
 2.42 with sigma of 0.02
 C29-C26 = C27-C28_$1
 2.42 with sigma of 0.02
 C28-C27 = C26_$1-C29
 2.42 with sigma of 0.02
 C33-C33_$3 = C32_$3-C32_$4
 2.42 with sigma of 0.02
 C33_$3-C33_$4 = C32_$4-C32
 2.42 with sigma of 0.02
 C33_$3-C32 = C33_$3-C32_$3 = C33_$4-C32_$4 = C33-C32_$4 = C33-C32 = C33_$4-
 C32_$3
 1.39 with sigma of 0.02
 C32-C32_$3 = C33_$4-C33
 2.42 with sigma of 0.02
 C23_$5-C23_$6 = C24-C24_$5
 2.42 with sigma of 0.02
 C24_$5-C24_$6 = C23_$6-C23
 2.42 with sigma of 0.02
 C23-C23_$5 = C24_$6-C24
 2.42 with sigma of 0.02
 C23-C24_$5 = C23_$5-C24_$5 = C23_$5-C24_$6 = C23_$6-C24_$6 = C23_$6-C24 = C23-
 C24
 1.39 with sigma of 0.02
 C5-C2 = C3_$7-C4
 2.42 with sigma of 0.02
 C5-C3 = C3-C2 = C3_$7-C2 = C5_$7-C3_$7 = C5_$7-C4 = C5-C4
 1.39 with sigma of 0.02
 C3-C3_$7 = C5_$7-C5
 2.42 with sigma of 0.02
 C2-C5_$7 = C4-C3
 2.42 with sigma of 0.02
 C14-C13 \\sim C32-C31 \\sim C30-C29 \\sim C26-C25 \\sim C23-C22 \\sim C21-C20
\\sim C17-C16 \\sim C12-C11
 \\sim C8-C7 \\sim C6-C5 \\sim C2-C1
 with sigma of 0.02
3. Restrained planarity
 C17, C16, C15, C14, C13, C19, C20, C21, C18
 with sigma of 0.1
 C12, C11, C10_$2, C8_$2, C7_$2, C9, C8, C7, C10
 with sigma of 0.1
 C30, C29, C28, C26, C25, C27, C26_$1, C25_$1, C28_$1
 with sigma of 0.1
 C31, C32, C33_$3, C31_$3, C33_$4, C32_$4, C31_$4, C33
 with sigma of 0.1
 C22, C23, C24_$5, C23_$5, C22_$5, C24_$6, C23_$6, C22_$6, C24
 with sigma of 0.1
 C6, C5, C3, C2, C1, C3_$7, C5_$7, C4, C6_$7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C17 \\sim C20 \\sim C18 \\sim C16 \\sim C15 \\sim C14 \\sim C19 \\sim C13 \\sim
C21: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C30 \\sim C29 \\sim C28 \\sim C26 \\sim C25 \\sim C27 \\sim C25 \\sim C28:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C12 \\sim C10 \\sim C8 \\sim C7 \\sim C9 \\sim C7 \\sim C8 \\sim C10 \\sim C11:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C1 \\sim C2 \\sim C3 \\sim C5 \\sim C6 \\sim C4 \\sim C5 \\sim C6 \\sim C3:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C31 \\sim C32 \\sim C33 \\sim C32 \\sim C31 \\sim C33 \\sim C31 \\sim C32 \\sim
C33: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C22 \\sim C23 \\sim C24 \\sim C23 \\sim C22 \\sim C24 \\sim C23 \\sim C22 \\sim
C24: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Fe05 \\sim Fe05 \\sim Fe07 \\sim O2B: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O15L \\sim C25 \\sim O14L: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
O1B \\sim Fe04 \\sim Fe06: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
Uanis(C27) \\sim Ueq, Uanis(O9L) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C8) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.04
Uanis(C32) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms of 0.1
5.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C18(H18), C19(H19), C15(H15), C27(H27), C28(H28), C10(H10),
 C33(H33), C9(H9), C3(H3), C4(H4)
5.b Fitted hexagon refined as free rotating group:
 C18(C20,C19,C14,C15,C16)
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_shelx_res_checksum              73602
_shelx_hkl_checksum              26580
_shelx_fab_checksum              6194
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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