A comparison of microcrystal electron diffraction and X-ray powder diffraction for the structural analysis of metal-organic frameworks.
Biehler, Erik; Pagola, Silvina; Stam, Daniel; Merkelbach, Johannes; Jandl, Christian; Abdel-Fattah, Tarek M; Journal of applied crystallography 58 (2025) 398–411; doi:10.1107/S1600576724012068

data_2300755
_publ_section_title
;
 A comparison of microcrystal electron diffraction and X-ray powder
 diffraction for the structural analysis of metal-organic frameworks.
;
_journal_coeditor_code           TE5145SUP1
_journal_issue                   'Pt 2'
_journal_name_full               'Journal of applied crystallography'
_journal_page_first              398
_journal_page_last               411
_journal_paper_doi               10.1107/S1600576724012068
_journal_volume                  58
_journal_year                    2025
_chemical_compound_source        'synthesized from aqueous solution'
_chemical_formula_moiety         'C8 H8 Co O6'
_chemical_formula_sum            'C8 H8 Co O6'
_chemical_formula_weight         259.07
_chemical_name_common            'cobalt terephthalate dihydrate'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     XD
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.867(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.22(11)
_cell_length_b                   6.54(4)
_cell_length_c                   7.28(4)
_cell_measurement_reflns_used    1331
_cell_measurement_temperature    293
_cell_measurement_theta_max      1.1643
_cell_measurement_theta_min      0.2570
_cell_volume                     857(9)
_computing_cell_refinement       'SAINT (Bruker 2019)'
_computing_data_collection       'Eldix (ELDICO 2023)'
_computing_data_reduction        'SAINT (Bruker 2019)'
_computing_molecular_graphics    'Mercury (Macrae 2008)'
_computing_publication_material  'EnCIFer (Allen 2004), PLATON (Spek 2009)'
_computing_structure_refinement
'SHELXL (Sheldrick 2015), ShelXle (Huebschle 2011)'
_computing_structure_solution    'SHELXD (Sheldrick 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Dectris QUADRO'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.772
_diffrn_measurement_device       'ELDICO ED-1'
_diffrn_measurement_device_type  'electron diffractometer'
_diffrn_measurement_method       'continuous rotation 3D ED'
_diffrn_radiation_source         LaB~6~
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02851
_diffrn_reflns_av_R_equivalents  0.0841
_diffrn_reflns_av_unetI/netI     0.1026
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2750
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        0.98
_diffrn_reflns_theta_max         1.20
_diffrn_reflns_theta_min         0.13
_exptl_absorpt_coefficient_mu    0
_exptl_absorpt_correction_T_max  0.7431
_exptl_absorpt_correction_T_min  0.1161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker 2016)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             0
_exptl_crystal_size_max          0.002
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0002
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       20113
_refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^
_refine_ls_extinction_method     'shelxl-2019/1 (sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1096
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.2313
_refine_ls_R_factor_gt           0.2044
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.3411P)^2^+4.1400P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4977
_refine_ls_wR_factor_ref         0.5242
_reflns_number_gt                839
_reflns_number_total             1096
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            te5145.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2300754--2300756.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2300755
_shelx_res_checksum              97098
_shelx_hkl_checksum              33699