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_1576256
_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         'C30 H23.333 Cu6 O27.667'
_chemical_formula_sum            'C30 H23.333 Cu6 O27.667'
_chemical_formula_weight         1207.777
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-07
_audit_creation_method
;
Olex2 1.5-ac7-013
(compiled 2025.01.02 svn.rf662f148 for Rigaku Oxford Diffraction, GUI svn.r7109)
;
_audit_update_record
;
2025-01-07 deposited with the CCDC.	2025-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.48(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.715(6)
_cell_length_b                   20.514(3)
_cell_length_c                   16.066(4)
_cell_measurement_reflns_used    2924
_cell_measurement_temperature    175(5)
_cell_measurement_theta_max      0.8830
_cell_measurement_theta_min      0.0620
_cell_volume                     4842(3)
_computing_cell_refinement       'CrysAlisPro 1.171.44.71a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.67a 64-bit (release 23-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.71a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac7-013 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-013 (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.5-ac7-013 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      175(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.8302
_diffrn_measured_fraction_theta_max 0.8302
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -57.25  55.50   0.25    0.75    --    0.00   0.00   0.00  451
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_measurement_specimen_support 'lacey carbon copper grid, 200 mesh'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0014625000
_diffrn_orient_matrix_UB_12      0.0005864000
_diffrn_orient_matrix_UB_13      -0.0004159000
_diffrn_orient_matrix_UB_21      0.0000618000
_diffrn_orient_matrix_UB_22      0.0005389000
_diffrn_orient_matrix_UB_23      -0.0013706000
_diffrn_orient_matrix_UB_31      -0.0008846000
_diffrn_orient_matrix_UB_32      -0.0009281000
_diffrn_orient_matrix_UB_33      -0.0010539000
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.2930
_diffrn_reflns_av_unetI/netI     0.3251
_diffrn_reflns_Laue_measured_fraction_full 0.8302
_diffrn_reflns_Laue_measured_fraction_max 0.8302
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12079
_diffrn_reflns_point_group_measured_fraction_full 0.8302
_diffrn_reflns_point_group_measured_fraction_max 0.8302
_diffrn_reflns_theta_full        0.7190
_diffrn_reflns_theta_max         0.72
_diffrn_reflns_theta_min         0.06
_diffrn_source                   LaB6
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_diffrn_source_voltage           200
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.71a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellow-orange (bulk)'
_exptl_crystal_colour_primary    'yellow-orange (bulk)'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             704.064
_exptl_crystal_preparation
;
sample ground between glass slides, grid tapped
;
_exptl_crystal_size_max          0.0024
_exptl_crystal_size_mid          0.0013
_refine_diff_density_max         1.4989
_refine_diff_density_min         -1.2497
_refine_diff_density_rms         0.2931
_refine_ls_d_res_high            1.0000
_refine_ls_d_res_low             11.6320
_refine_ls_extinction_coef       5522(451)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.4760
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    46
_refine_ls_number_parameters     606
_refine_ls_number_reflns         4215
_refine_ls_number_restraints     811
_refine_ls_restrained_S_all      1.3338
_refine_ls_R_factor_all          0.3063
_refine_ls_R_factor_gt           0.2338
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4855
_refine_ls_wR_factor_ref         0.5219
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2437
_reflns_number_total             4215
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5sc05651a2.cif
_cod_data_source_block           exp_1454_mP_s20e470
_cod_database_code               1576256
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment
;
'repeat of exp_1452, Agar holey carbon gold grid, orange-yellow solid, ground
between glass slides, grid tapped, cryo transfer @ 175 K, coll @ 175 K'
;
_diffrn_oxdiff_scatteringfactors_ed
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_diffrn_oxdiff_digest_creation
;
CAP 1.171.44.71a, AC 1.5-ac7-008
;
_diffrn_oxdiff_digest_dyn_ed
;
61441b0e2a6df6ddaead44e46243d36ca33ff9
;
_diffrn_oxdiff_digest_hkl
;
43bcc58f69e405203308b38f18e33856eeb61e
;
_diffrn_oxdiff_digest_hkl_ed
;
530e8d00540fe293ad33582521bd3407f901e4
;
_diffrn_oxdiff_digest_od_ed
;
6226db7819d4ea2144402d28ec8fe38e4c5daf
;
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 C14-C15 = C15-C16 = C16-C17 = C17-C18 = C18-C19 = C19-C14
 1.39 with sigma of 0.01
 C4-C3 = C3-C2 = C2-C7 = C7-C6 = C6-C5 = C5-C4
 1.39 with sigma of 0.01
 O29-C29 = O30-C29
 1.25 with sigma of 0.02
 C23-C24 = C24-C25 = C25-C26 = C26-C27 = C27-C22 = C22-C23
 1.39 with sigma of 0.01
 C10-C12 = C12-C11_$1 = C11-C10 = C10-C12 = C12_$1-C11 = C11-C10
 1.39 with sigma of 0.01
 C11-O10
 1.35 with sigma of 0.02
 C4-C2 \\sim C3-C7 \\sim C2-C6 \\sim C7-C5 \\sim C6-C4 \\sim C5-C3
 with sigma of 0.02
 C14-C16 \\sim C15-C17 \\sim C16-C18 \\sim C17-C19 \\sim C18-C14 \\sim C19-C15
 with sigma of 0.02
 C23-C25 \\sim C24-C26 \\sim C25-C27 \\sim C26-C22 \\sim C27-C23 \\sim C22-C24
 with sigma of 0.02
 C10-C11_$1 \\sim C12-C10_$1 \\sim C11-C12 \\sim C10_$1-C11 \\sim C12_$1-C10
\\sim C11-C12
 with sigma of 0.02
3. Restrained planarity
 C2, C3, C4, C5, C6, C7
 with sigma of 0.1
 C14, C15, C16, C17, C18, C19
 with sigma of 0.1
 C22, C23, C24, C25, C26, C27
 with sigma of 0.1
 C10, C10_$1, C11, C11_$1, C12_$1, C12
 with sigma of 0.1
 O15, O16, H16, C15
 with sigma of 0.1
 O12, C12, O13, H13
 with sigma of 0.1
 O17, H17, O18, C16
 with sigma of 0.1
 O12, C9, C12, O13, H13
 with sigma of 0.1
 O11, C9, C11, O10, H10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
O11 \\sim O12 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim O10 \\sim O13:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C29 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C30) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O9(0.5) H9a(0.5) H9b(0.5) O20(0.75) H20a(0.75) H20b(0.75) O7(0.75)
 H7a(0.75) H7b(0.75) O22(0.66667) H22a(0.66667) H22b(0.66667) O10(0.5) H10(0.5)
 O13(0.5) H13(0.5)
7.a Rotating group:
 O21(H21a,H21b), O9(H9a,H9b), O20(H20a,H20b), O8(H8a,H8b), O7(H7a,H7b),
 O22(H22a,H22b)
7.b Me refined with riding coordinates:
 C30(H30a,H30b,H30c)
7.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C7(H7), C27(H27), C12(H12), C6(H6), C19(H19), C18(H18), C11(H11)
7.d Idealised tetrahedral OH refined as rotating group:
 O10(H10), O16(H16), O17(H17), O13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.137
_oxdiff_exptl_absorpt_empirical_full_min 0.273
_oxdiff_exptl_crystal_thickness  1000.0