EMM-25: The Structure of Two-Dimensional 11 ×10 Medium-Pore Borosilicate Zeolite Unraveled Using 3D Electron Diffraction
Cho, Jung; Yun, Yifeng; Xu, Hongyi; Sun, Junliang; Burton, Allen W.; Strohmaier, Karl G.; Terefenko, Gene; Vroman, Hilda; Afeworki, Mobae; Cao, Guang; Wang, Hao; Zou, Xiaodong; Willhammar, Tom; Chemistry of Materials  (2021) –; doi:10.1021/acs.chemmater.1c00892

data_4003943
_publ_section_title
;
 EMM-25: The Structure of Two-Dimensional 11 \\times 10 Medium-Pore
 Borosilicate Zeolite Unraveled Using 3D Electron Diffraction
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.1c00892
_journal_year                    2021
_chemical_formula_moiety         'O232 Si116, 0.25(C208 N16)'
_chemical_formula_sum            'C52 N4 O232 Si116'
_chemical_formula_weight         7650.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_audit_creation_date             2021-02-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.055(2)
_cell_length_b                   22.912(5)
_cell_length_c                   24.914(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6311(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  JEOL-2100
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.1803
_diffrn_reflns_av_unetI/netI     0.1724
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14434
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.919
_diffrn_reflns_theta_min         0.058
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       'needle-like nanocrystal'
_exptl_crystal_F_000             1274
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.380
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3698
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.379
_refine_ls_R_factor_all          0.2375
_refine_ls_R_factor_gt           0.2017
_refine_ls_shift/su_max          2.585
_refine_ls_shift/su_mean         0.022
_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          0.4364
_refine_ls_wR_factor_ref         0.4636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2278
_reflns_number_total             3698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c00892_si_003.cif
_cod_data_source_block           cmc21-cmcm-osda
_cod_database_code               4003943
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C2-C2_$1
 1.52 with sigma of 0.02
 C3-C3_$2
 1.92 with sigma of 0.02
2. Others
 Fixed Sof: Si1(0.25) Si2(0.25) Si3(0.25) Si4(0.25) Si5(0.25) Si6(0.5)
 Si7(0.5) Si8(0.5) Si9(0.5) Si10(0.5) Si11(0.5) Si12(0.5) Si13(0.5) Si14(0.5)
 Si15(0.5) O1(0.25) O2(0.25) O3(0.25) O4(0.25) O5(0.25) O6(0.5) O7(0.5) O8(0.5)
 O9(0.5) O10(0.5) O11(0.5) O12(0.5) O13(0.5) O14(0.5) O15(0.5) O16(0.5)
 O17(0.5) O18(0.5) O19(0.5) O20(0.5) O21(0.5) O22(0.5) O23(0.5) O24(0.5)
 O25(0.5) O26(0.5) O28(0.5) O29(0.25) O30(0.25) O31(0.25) O32(0.25) O33(0.25)
 O34(0.25) O35(0.25) N1(0.25) C1(0.25) C2(0.25) C3(0.25) C4(0.25) C5(0.25)
 C6(0.25) C7(0.25) C8(0.25) C9(0.25) C10(0.25) C11(0.25) C12(0.25) C13(0.25)
3.a Free rotating group:
 N1(C1,C2,C3,C4,C5,C6,C7,C8,C9,C10,C11,C12,C13)
;
_shelx_res_checksum              67220
_shelx_hkl_checksum              986
_olex2_submission_special_instructions 'No special instructions were received'