Beam-sensitive metal-organic framework structure determination by microcrystal electron diffraction.
Banihashemi, Fateme; Bu, Guanhong; Thaker, Amar; Williams, Dewight; Lin, Jerry Y S; Nannenga, Brent L; Ultramicroscopy 216 (2020) 113048–; doi:10.1016/j.ultramic.2020.113048

data_1560435
_publ_section_title
;
 Beam-sensitive metal-organic framework structure determination by
 microcrystal electron diffraction.
;
_journal_name_full               Ultramicroscopy
_journal_page_first              113048
_journal_paper_doi               10.1016/j.ultramic.2020.113048
_journal_volume                  216
_journal_year                    2020
_chemical_formula_sum            'C96 H120 N48 Zn12'
_chemical_formula_weight         2730.91
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            1
_cell_length_a                   16.880(3)
_cell_length_b                   16.880(3)
_cell_length_c                   16.880(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4809.7(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.3206
_diffrn_reflns_av_unetI/netI     0.2108
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7484
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        34.949
_diffrn_reflns_theta_max         34.949
_diffrn_reflns_theta_min         3.396
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_F_000             483
_refine_diff_density_max         0.105
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef       0.07(3)
_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   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1779
_refine_ls_R_factor_gt           0.1348
_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^)+(0.1649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3253
_refine_ls_wR_factor_ref         0.3411
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                342
_reflns_number_total             738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            02-211_a.cif
_cod_data_source_block           02-211_a
_cod_original_cell_volume        4810(3)
_cod_database_code               1560435
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              958
_shelx_hkl_checksum              85672