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_4126182
_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         'C18.80 H14.10 N9.70 O3.40 Zn2'
_chemical_formula_sum            'C18.8 H14.1 N9.7 O3.4 Zn2'
_chemical_formula_weight         561.04
_chemical_name_common            ZIF-360
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-26
_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            48
_cell_length_a                   35.943(3)
_cell_length_b                   35.943(3)
_cell_length_c                   35.943(3)
_cell_measurement_reflns_used    64698
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.199
_cell_measurement_theta_min      2.421
_cell_volume                     46435(7)
_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_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.2399
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        31.100
_diffrn_reflns_theta_max         31.199
_diffrn_reflns_theta_min         2.421
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    5.520
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1602 before and 0.0672 after correction.
The Ratio of minimum to maximum transmission is 0.7109.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.963
_exptl_crystal_description       Block
_exptl_crystal_F_000             13536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1409
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1553P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1179
_reflns_number_total             1409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_003.cif
_cod_data_source_block           zif-360_KFI
_cod_original_cell_volume        46436(13)
_cod_original_formula_sum        'C18.80 H14.10 N9.70 O3.40 Zn2'
_cod_database_code               4126182
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.557
_shelx_estimated_absorpt_t_min   0.491
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4A-N3
 1.36 with sigma of 0.02
 C4-N3
 1.36 with sigma of 0.02
 C3A-C4A
 2.5 with sigma of 0.04
 C10-C11 = C11-C12 = C12-C12_$1 = C10_$1-C11_$1
 1.39 with sigma of 0.02
 C10-C12
 0.04 with sigma of 2.52
 C11-C10_$1
 0.04 with sigma of 2.52
3. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C4) = Uanis(C4A)
4. Rigid body (RIGU) restrains
 C4, O2, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, N3, C3A, C3A, C13, C13, C14, C14, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, N2, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C4(0.35) H6(0.4) O2(0.7) N4(0.35) H10(0.4) C7(0.7) H7(0.7) C3(0.7)
 H3(0.7) C8(0.7) H8(0.7) C11(0.7) H11(0.7) C12(0.7) H12(0.7) C3A(0.3) C13(0.3)
 H13(0.3) C14(0.3) H14(0.3) C4A(0.15) H4A(0.15)
6.a Riding coordinates:
 C13(H13), C14(H14)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C5(H5), C6(H6), C1(H1), C10(H10), C7(H7), C3(H3), C8(H8), C11(H11),
 C12(H12), C4A(H4A)
;
_shelx_res_checksum              93357
_shelx_hkl_checksum              69600