Principles of Designing Extra-Large Pore Openings and Cages in Zeolitic Imidazolate Frameworks.
Yang, Jingjing; Zhang, Yue-Biao; Liu, Qi; Trickett, Christopher A.; Gutiérrez-Puebla, Enrique; Monge, M Ángeles; Cong, Hengjiang; Aldossary, Abdulrahman; Deng, Hexiang; Yaghi, Omar M.; Journal of the American Chemical Society 139 (2017) 6448–6455; doi:10.1021/jacs.7b02272

data_4126002
_publ_section_title
;
 Principles of Designing Extra-Large Pore Openings and Cages in Zeolitic
 Imidazolate Frameworks.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6448
_journal_page_last               6455
_journal_paper_doi               10.1021/jacs.7b02272
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C33.5 H26.49 N13.81 O3.63 Zn3'
_chemical_formula_sum            'C33.5 H26.49 N13.81 O3.63 Zn3'
_chemical_formula_weight         876.70
_chemical_name_common            ZIF-413
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            192
_cell_length_a                   72.3673(14)
_cell_length_b                   72.3673(14)
_cell_length_c                   72.3673(14)
_cell_measurement_reflns_used    168049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.064
_cell_measurement_theta_min      1.964
_cell_volume                     378989(13)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '/w scans with narrow frames'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.2399
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            168049
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        31.105
_diffrn_reflns_theta_max         31.064
_diffrn_reflns_theta_min         1.964
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    4.056
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0501 before and 0.0424 after correction.
The Ratio of minimum to maximum transmission is 0.9103.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    0.737
_exptl_crystal_description       Block
_exptl_crystal_F_000             85094
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     362
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.1032
_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^)+(0.2500P)^2^+2000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3171
_refine_ls_wR_factor_ref         0.3434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4190
_reflns_number_total             5478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_010.cif
_cod_data_source_block           zif-413_ucb
_cod_depositor_comments
'Adding full bibliography for 4125998--4126004.cif.'
_cod_original_cell_volume        378989(22)
_cod_original_formula_sum        'C33.50 H26.49 N13.81 O3.63 Zn3'
_cod_database_code               4126002
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.687
_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
2. Restrained distances
 C9-C10
 1.54 with sigma of 0.02
 N13-C32
 1.36 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C46) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C36) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C12B) = Uanis(C12A)
Uanis(C31) = Uanis(C30)
Uanis(C11A) = Uanis(C11)
4. Rigid body (RIGU) restrains
 O3, O2, N5, N6, C13, N4, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N9, O4, C17, N10, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, N13, N13, C34, C34, C33, C33, C35, C35, C36, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N12, N12, C38, C38, C37, C39, C39, C41, C41, C40, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, N1, C1, C2, C2, C4, C4, C3, C3, C5, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, C19, C18, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, C42, C43, C44, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11, N8, C23, C24, C29, C28, C27, C26, C25, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, N2, C6, C7, C7, C8, C8, C9, C9, C10, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12B, C12B, C11, O1, O1, N23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11A, C12A, C12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H4(0.5) H43(0.5) H7(0.5) C39(0.75) H39(0.75) C34(0.75) H34(0.75)
 H33(0.5) C35(0.75) H35(0.75) H21(0.5) C12B(0.8) H12B(0.8) C11(0.3125)
 O1(0.625) H24(0.15) H29(0.15) C28(0.85) H28(0.85) C27(0.85) C26(0.85)
 C25(0.85) H25(0.85) C8(0.5) H8(0.5) C9(0.5) H9(0.25) C10(0.25) H10A(0.25)
 H10B(0.25) H10C(0.25) C36(0.375) H36A(0.375) H36B(0.375) H36C(0.375)
 C31(0.425) H31A(0.425) H31B(0.425) H31C(0.425) C41(0.375) H41A(0.375)
 H41B(0.375) H41C(0.375) C40(0.75) N23(0.3125) C5(0.5) H5A(0.5) H5B(0.5)
 H5C(0.5) C44(0.5) H44(0.5) C45(0.5) C46(0.25) H46A(0.25) H46B(0.25) H46C(0.25)
 C30(0.425) H30A(0.425) H30B(0.425) H30C(0.425) C22(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C11A(0.1875) H11A(0.1875) C12A(0.2) H12A(0.2)
6.a Riding coordinates:
 C1(H1), C6(H6), C18(H18), C42(H42), C4(H4), C43(H43), C3(H3), C7(H7),
 C32(H32), C20(H20), C34(H34), C33(H33), C35(H35), C21(H21), C24(H24), C29(H29),
  C8(H8), C9(H9), C10(H10A,H10B,H10C), C36(H36A,H36B,H36C), C31(H31A,H31B,H31C),
  C41(H41A,H41B,H41C), C5(H5A,H5B,H5C), C44(H44), C46(H46A,H46B,H46C), C30(H30A,
 H30B,H30C), C22(H22A,H22B,H22C)
6.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C14(H14), C15(H15), C37(H37), C39(H39), C12B(H12B), C28(H28),
 C25(H25), C11A(H11A), C12A(H12A)
6.c Fitted pentagon refined as free rotating group:
 N6(C13,N4,C14,C15)
6.d Fitted hexagon refined as free rotating group:
 C24(C29,C28,C27,C26,C25)
;
_shelx_res_checksum              46627
_shelx_hkl_checksum              49478