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_4125999
_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         'C31.6 H22.95 N13.85 O3.7 Zn3'
_chemical_formula_sum            'C31.6 H22.95 N13.85 O3.7 Zn3'
_chemical_formula_weight         852.00
_chemical_name_common            ZIF-412
_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                   72.205(2)
_cell_length_b                   72.205(2)
_cell_length_c                   72.205(2)
_cell_measurement_reflns_used    270972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.303
_cell_measurement_theta_min      1.704
_cell_volume                     376445(18)
_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
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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '/w scans with narrow frames'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8265
_diffrn_reflns_av_R_equivalents  0.1418
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            270972
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.305
_diffrn_reflns_theta_max         19.303
_diffrn_reflns_theta_min         1.704
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker,2014/5)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.722
_exptl_crystal_description       Block
_exptl_crystal_F_000             82387
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         4845
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0434
_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^)+(0.1168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3983
_reflns_number_total             4845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_009.cif
_cod_data_source_block           ZIF-412_ucb
_cod_depositor_comments
'Adding full bibliography for 4125998--4126004.cif.'
_cod_original_cell_volume        376445(31)
_cod_original_formula_sum        'C31.60 H22.95 N13.85 O3.70 Zn3'
_cod_database_code               4125999
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, H5 of C5, H7 of C7, H8 of C8, H9 of C9, H11 of C11, H30 of C30,
  H29 of C29, H32 of C32, H33 of C33, H34 of C34, H35 of C35, H36 of C36, H37
  of C37, H18A of C18A, H20 of C20, H18B of C18B, H19B of C19B, H17 of C17, H16
  of C16, H14 of C14, H13 of C13, H1 of C1, H3 of C3, H31 of C31, H27 of C27,
  H26 of C26, H25 of C25, H24 of C24, H23 of C23, H22 of C22, H21 of C21
 At 1.5 times of:
  H38 of C38
2. Restrained distances
 N9-C19A \\sim N9-C19B \\sim N9-C18A \\sim N9-C18B
 with sigma of 0.02
3. Restrained planarity
 N9, C19B, N9_$1, C18B, C18B_$1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C19A) \\sim Ueq, Uanis(C19B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18B) = Uanis(C18A)
Uanis(C19A) = Uanis(C19B)
5. Rigid body (RIGU) restrains
 C36, C38, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, N12, N11, C21, C26, C25, C24, C23, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, N14, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O4(0.7) N10(0.35) C19B(0.15) H19B(0.15) C18B(0.3) H18B(0.3)
 H21(0.1) C22(0.9) H22(0.9) C23(0.9) H23(0.9) C24(0.9) H24(0.9) C25(0.9)
 H25(0.9) H26(0.1) H32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5) H36(0.5)
 C37(0.5) H37(0.5) C38(0.5) H38(0.5) C18A(0.7) H18A(0.7) C19A(0.35)
7.a Riding coordinates:
 C19B(H19B), C18B(H18B), C38(H38)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C18A(H18A)
;
_shelx_res_checksum              95902
_shelx_hkl_checksum              47549