A flexible copper MOF as a carboxylate-specific crystalline sponge for structure solution using X-ray and electron diffraction.
Main, Russell; Rainer, Daniel N.; Bauzá, Marta; Ettlinger, Romy; Kelly, Nicole L.; Coles, Simon; Ashbrook, Sharon Elizabeth; Morris, Russell; Chemical Science  (2025) –; doi:10.1039/D5SC05651A

data_1576252
_publ_section_title
;
 A flexible copper MOF as a carboxylate-specific crystalline sponge for
 structure solution using X-ray and electron diffraction.
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC05651A
_journal_year                    2025
_chemical_formula_moiety         'C57 H10 Cu12 O48, C'
_chemical_formula_sum            'C58 H10 Cu12 O48'
_chemical_formula_weight         2237.14
_chemical_name_common            SIMOF-5
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-30
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-16 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.83(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.660(4)
_cell_length_b                   15.511(5)
_cell_length_c                   17.028(3)
_cell_measurement_reflns_used    814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.43581043868466
_cell_measurement_theta_min      1.8097284187519582
_cell_volume                     3690.9(18)
_computing_cell_refinement
;
DIALS 3.10.2-1-g02720afcd-release (Winter, G. et al., 2018)
XIA2 3.10.1 (Winter, G., 2010)
;
_computing_data_collection       'GDA 9.20; generic data acquisition software'
_computing_data_reduction
;
DIALS 3.10.2-1-g02720afcd-release (Winter, G. et al., 2018)
dials.scale (Beilsten-Edmands, J. et al., 2020)
XIA2 3.10.1 (Winter, G., 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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  1.4853
_diffrn_reflns_av_unetI/netI     18.9714
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81669
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         36.186
_diffrn_reflns_theta_min         1.423
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9706354068639151
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 3.18.1-gafd9b17f2-release
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       prism
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.264
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.35(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.501
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         33458
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      0.515
_refine_ls_R_factor_all          0.7362
_refine_ls_R_factor_gt           0.1574
_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^)+(0.1500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3384
_refine_ls_wR_factor_ref         0.4470
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.806
_reflns_number_gt                1756
_reflns_number_total             33458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05651a2.cif
_cod_data_source_block           shelxt
_cod_original_cell_volume        3690.5(19)
_cod_database_code               1576252
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C20-O01T
 1.3 with sigma of 0.02
 C57-C58
 1.23 with sigma of 0.02
 O020-C21 = O00D-C11 = O00P-C10
 1.3 with sigma of 0.02
 C57_$1-C50
 1.3 with sigma of 0.02
 C51-C49 = C51-C50 = C49-C48 = C56_$1-C48 = C57-C56 = C57_$1-C50
 1.39 with sigma of 0.001
 C33-C32
 1.39 with sigma of 0.02
 O02I-C37
 1.3 with sigma of 0.02
 C21-C20 = C21-C22 = C21-O020
 1.3 with sigma of 0.02
 C24-C25
 1.39 with sigma of 0.02
 Cu6_$2-O18
 2.1 with sigma of 0.02
 C28-C31
 1.4 with sigma of 0.02
 C39-C38
 1.4 with sigma of 0.02
 C36-O9
 1.2 with sigma of 0.02
 O44-C35
 1.2 with sigma of 0.02
 Cu5-O27
 1.9 with sigma of 0.04
 Cu3A-O7
 1.9 with sigma of 0.02
 O7-C55 = O013-C55
 1.3 with sigma of 0.02
 C1-O18
 1.3 with sigma of 0.02
 C1-O5
 1.14 with sigma of 0.02
 O1_$4-C32_$4
 1.14 with sigma of 0.02
 C56-C58
 1.33 with sigma of 0.01
 C44-C47
 1.33 with sigma of 0.01
 O036-C58
 1.4 with sigma of 0.02
 C58-O01V
 1.4 with sigma of 0.02
 C51_$5-C50_$5 = C57-C50_$5 = C57-C56 = C56-C48_$5 = C49_$5-C48_$5 = C51_$5-
 C49_$5
 1.39 with sigma of 0.02
 O2-C57
 1.5 with sigma of 0.02
 C57-C58
 2.8 with sigma of 0.04
 C56-C51_$5
 2.78 with sigma of 0.04
 C57-C49_$5
 2.78 with sigma of 0.04
 C50_$5-C48_$5
 2.78 with sigma of 0.04
3. Restrained planarity
 C56_$1, C57_$1, C50, C51, C49, C48
 with sigma of 0.1
 O2_$1, C57_$1, C50, C56_$1
 with sigma of 0.1
 C40, C42, C43, C46, C44, C41, C45, C47
 with sigma of 0.1
 C43, C44, C46, C47
 with sigma of 0.1
 C40, C41, C42, C45, C46, C43
 with sigma of 0.1
 C46, C44, C43, O27_$3, O4_$3
 with sigma of 0.1
 O10, C43, C42, C41
 with sigma of 0.1
 O00Z, C64, O00O, C22
 with sigma of 0.1
 C19, C65, O00J, O00K
 with sigma of 0.1
 O02I, C37, C34, C38
 with sigma of 0.1
 O52, C50, C57_$1, C51
 with sigma of 0.1
 C1, O18, C2, C7, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O00O \\sim Cu3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
O02P \\sim Cu3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5. Others
 Fixed Sof: O02I(0.5) O3(0.5) O44(0.5) O9(0.5) O10(0.5) O14(0.5)
 Fixed Uiso: O00J(0.1) O00L(0.06) C3(0.08) C2(0.08) O00O(0.08) O(0.06)
 C20(0.09) C21(0.09) C22(0.08) C59(0.09) C23(0.09) C55(0.08) C51(0.08)
 C50(0.08) O52(0.08) C26(0.08) C25(0.08) C30(0.08) C29(0.08) C28(0.08)
 C38(0.08) C33(0.08) C34(0.08) C37(0.08) C57(0.08) C31(0.08633) O02I(0.05)
 C58(0.08) O02P(0.08) C15(0.08) C12(0.08) O036(0.08) O44(0.05) C1(0.05)
 O18(0.08) O4(0.1) C39(0.08) O9(0.08) O10(0.05) C46(0.08) C45(0.08) C41(0.08)
 C42(0.08) C43(0.08) C44(0.08) C40(0.08) C64(0.05) O62(0.1) O63(0.1) C49(0.08)
 C48(0.08) O14(0.05) O27(0.1) C47(0.08) C61(0.08) C56(0.08) C65(0.05) O2(0.05)
 O5(0.05) O1(0.08)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C59(H59), C23(H23), C30(H30), C29(H29), C14(H14), C15(H15),
 C49(H49), C48(H48)
6.b Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4), C19(C20,C21,C22,C59,C23), C27(C26,C25,C30,C29,C28),
 C38(C36,C35,C33,C34,C37), C14(C15,C12,C11,C10,C16), C46(C45,C41,C42,C43,C44)
;
_shelx_res_checksum              86171
_olex2_submission_special_instructions 'No special instructions were received'