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_1576253
_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         'C16.5 H9.443 Cu3 N0.5 O14, 0.5(O)'
_chemical_formula_sum            'C16.5 H9.45 Cu3 N0.5 O14.5'
_chemical_formula_weight         637.31
_chemical_name_common            SIMOF-5
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2024-11-21 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.245(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.071(3)
_cell_length_b                   20.985(4)
_cell_length_c                   16.560(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.27
_cell_volume                     5365.8(17)
_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      100.15
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type
'Fluid Film Devices diffractometer with Pilatus 2M detector'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1461
_diffrn_reflns_av_unetI/netI     0.1276
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64208
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         24.630
_diffrn_reflns_theta_min         1.278
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9892722514174753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CCP4 8.0.010: AIMLESS, version 0.7.9 : 10/06/22
Scaling & analysis of unmerged intensities, absorption correction using
 spherical harmonics
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       needle
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         2.981
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         9870
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1616
_refine_ls_R_factor_gt           0.1196
_refine_ls_shift/su_max          0.000
_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          0.3228
_refine_ls_wR_factor_ref         0.3488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5370
_reflns_number_total             9870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05651a2.cif
_cod_data_source_block           rmm9b
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        5365.8(15)
_cod_original_formula_sum        'C16.50 H9.45 Cu3 N0.50 O14.50'
_cod_database_code               1576253
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 C01K-C01T \\sim C01K-C01U
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O01V \\sim C01O: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C01T \\sim C01U \\sim C01K: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
C3 \\sim N4 \\sim C7 \\sim O01P: within 2.7A with sigma of 0.02 and sigma for
terminal atoms of 0.08 within 2.7A
C19 \\sim N4 \\sim C7 \\sim O01P \\sim C3: within 2.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2.7A
4. Others
 Sof(C01U)=Sof(H01A)=Sof(H01D)=Sof(H01G)=1-FVAR(1)
 Sof(C01T)=FVAR(1)
 Fixed Sof: H01O(0.5) H01R(0.5) O01S(0.5) O01V(0.5) H01S(0.5) H01V(0.5)
 Fixed X: H01S(0.11069) H01V(0.13111)
 Fixed Y: H01S(0.4667) H01V(0.41384)
 Fixed Z: H01S(0.395081) H01V(0.651561)
5.a Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00T(H00T), C01B(H01B), C01C(H01C), C01E(H01E), C01F(H01F),
 C01O(H01O), C01R(H01R), C7(H7)
5.b Idealised Me refined as rotating group:
 C01U(H01A,H01D,H01G), C3(H3A,H3B,H3C), C19(H19A,H19B,H19C)
5.c Idealised tetrahedral OH refined as rotating group:
 O011(H011), O01I(H01I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77567
_shelx_fab_checksum              16782
_olex2_submission_special_instructions 'No special instructions were received'