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_4125998
_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         'C29.08 H24.28 N14.3 O4.6 Zn3'
_chemical_formula_sum            'C29.08 H24.45 N14.3 O4.6 Zn3'
_chemical_formula_weight         843.95
_chemical_name_common            ZIF-414
_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             2015-10-15
_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                   72.2609(18)
_cell_length_b                   72.2609(18)
_cell_length_c                   72.2609(18)
_cell_measurement_reflns_used    9138
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.413
_cell_measurement_theta_min      2.300
_cell_volume                     377320(16)
_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_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.7749
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            285177
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        16.935
_diffrn_reflns_theta_max         16.925
_diffrn_reflns_theta_min         2.038
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1375 before and 0.0711 after correction.
The Ratio of minimum to maximum transmission is 0.8390.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.713
_exptl_crystal_description       Block
_exptl_crystal_F_000             81760
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     500
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1414P)^2^+4002.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2280
_refine_ls_wR_factor_ref         0.2491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3185
_reflns_number_total             4062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_011.cif
_cod_data_source_block           zif-414_ucb
_cod_depositor_comments
'Adding full bibliography for 4125998--4126004.cif.'
_cod_original_cell_volume        377320(28)
_cod_original_formula_sum        'C29.08 H24.45 N14.30 O4.60 Zn3'
_cod_database_code               4125998
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.901
_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
 C2'-C1' = C2-C1
 2.1 with sigma of 0.02
 C8-C7
 2.5 with sigma of 0.04
 O6'-N15'
 1.25 with sigma of 0.02
 O1-O2
 2.2 with sigma of 0.02
 N6-C23
 1.36 with sigma of 0.02
 C24-C23
 2.5 with sigma of 0.04
 C14-C15 \\sim C14-C13 \\sim C12-C13 \\sim C17-C12 \\sim C16-C17 \\sim C15-C16
 with sigma of 0.02
 C8-C8_$2 \\sim C9_$2-C8_$2 \\sim C9_$2-C10_$2 \\sim C10-C10_$2 \\sim C9-C10
\\sim C9-C8
 with sigma of 0.02
 N1'-C1' \\sim N1'-C2' \\sim N1'_$1-C2'_$1 \\sim N1'_$1-C1' \\sim N1-C1 \\sim
N1-C2 \\sim N1_$1-C2_$1
 \\sim N1_$1-C1
 with sigma of 0.02
 O1-O2 \\sim O3-O4 \\sim O5-O6 \\sim O7-O8 \\sim O9-O10 \\sim O11-O12
 with sigma of 0.02
 C29-C30 \\sim C3-C4 \\sim C26-C27 \\sim C27-C25
 with sigma of 0.02
 O12-N18 \\sim O11-N18 \\sim O10-N17 \\sim O9-N17 \\sim O3-N14 \\sim O4-N14
\\sim O5'-N15' \\sim O6'-N15'
 \\sim O6-N15 \\sim O5-N15 \\sim O7-N16 \\sim O1-N13 \\sim O2-N13 \\sim O8-N16
 with sigma of 0.02
3. Restrained planarity
 O4, N14, O3, C10, C9
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C38 \\sim N18 \\sim O12 \\sim O11: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C27 \\sim N9 \\sim Zn3: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N5 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C12 \\sim C13: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N12 \\sim C29: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C28 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C33 \\sim C34: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N17) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C39) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N14) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N1') = Uanis(N1)
Uanis(C1) = Uanis(C1')
Uanis(C2') = Uanis(C2)
Uanis(N1') = Uanis(N10)
Uanis(O7) = Uanis(O1) = Uanis(O8) = Uanis(O2)
Uanis(O5') = Uanis(O6') = Uanis(O6) = Uanis(O5)
Uanis(O3) = Uanis(O4)
5. Rigid body (RIGU) restrains
 N2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zn3, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zn2, N8, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zn2, N7, N8, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, N14, N16, N17, N13, N18, N15', N15, N1, C23, C4, C8, C24, C37, C9, C29,
 C5, C10, C20, C25, C26, C27, C35, C2', C30, C7, C33, C34, C21, C6, C13, C16,
 C15, C14, C39, C38, C2, C1', O3, O4, O8, O7, O9, O10, O2, O1, O12, O11, O5',
 O6', O6, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N1')=1-FVAR(1)
 Sof(O5')=Sof(N15')=Sof(O6')=0.5*(1-FVAR(2))
 Sof(O6)=Sof(N15)=Sof(O5)=0.5*FVAR(2)
 Sof(N1)=FVAR(1)
 Sof(C2')=Sof(H2')=1-FVAR(2)
 Sof(C1)=Sof(H1)=0.5*(1-FVAR(3))
 Sof(C1')=Sof(H1')=0.5*FVAR(3)
 Sof(C2)=Sof(H2)=FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(3)
 Fixed Sof: H12(0.5) H17(0.5) H19(0.2) H4(0.2) H8(0.2) H37(0.5) C9(0.5)
 H9(0.5) C5(0.8) H5(0.8) C10(0.5) H10(0.4) C20(0.8) H20(0.8) H35(0.5)
 C31(0.375) H31A(0.75) H31B(0.75) H31C(0.75) C21(0.8) H21(0.4) C6(0.8) H6(0.4)
 O3(0.25) N14(0.25) O4(0.25) C13(0.5) H13(0.5) C16(0.5) H16(0.5) C15(0.5)
 H15(0.25) C14(0.5) H14(0.25) C39(0.5) H39(0.25) C38(0.5) H38(0.5) O8(0.4)
 N16(0.4) O7(0.4) O9(0.5) N17(0.5) O10(0.5) N13(0.4) O2(0.4) O1(0.4) N18(0.25)
 O12(0.25) O11(0.25)
7.a Riding coordinates:
 C28(H28A,H28B,H28C), C32(H32), C11(H11), C12(H12), C17(H17), C19(H19), C1(H1),
  C3(H3), C4(H4), C8(H8), C18(H18), C22(H22A,H22B,H22C), C36(H36), C24(H24),
 C37(H37), C9(H9), C29(H29), C5(H5), C10(H10), C20(H20), C25(H25), C26(H26),
 C35(H35), C2'(H2'), C31(H31A,H31B,H31C), C7(H7), C34(H34), C21(H21), C6(H6),
 C13(H13), C16(H16), C15(H15), C14(H14), C39(H39), C38(H38), C2(H2), C1'(H1')
7.b Fitted pentagon refined as free rotating group:
 C25(C26,N9,C27,N8)
;
_shelx_res_checksum              55187
_shelx_hkl_checksum              19829