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_4126183
_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         '0.04(C174 H138 N102 O12 Zn24)'
_chemical_formula_sum            'C7.25 H5.75 N4.25 O0.5 Zn'
_chemical_formula_weight         225.78
_chemical_name_common            ZIF-376
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-11
_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            24
_cell_length_a                   22.688(3)
_cell_length_b                   22.688(3)
_cell_length_c                   22.688(3)
_cell_measurement_reflns_used    7779
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.940
_cell_measurement_theta_min      3.374
_cell_volume                     11679(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7779
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        39.970
_diffrn_reflns_theta_max         39.940
_diffrn_reflns_theta_min         3.374
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1113 before and 0.0838 after correction.
The Ratio of minimum to maximum transmission is 0.6651.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.770
_exptl_crystal_description       Block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         765
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.1189
_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^)+(0.2000P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3241
_refine_ls_wR_factor_ref         0.3415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                599
_reflns_number_total             765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_005.cif
_cod_data_source_block           ZIF-376_LTA
_cod_original_cell_volume        11679(4)
_cod_original_formula_sum        'C7.25 H5.75 N4.25 O0.50 Zn'
_cod_database_code               4126183
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.856
_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
 N4-C9
 1.5 with sigma of 0.02
 O1-N4 = O2-N4
 1.25 with sigma of 0.02
 C9-O1
 2.5 with sigma of 0.02
 C9-O2
 2.5 with sigma of 0.02
 O1-O2
 2.5 with sigma of 0.02
 N4-C8
 2.5 with sigma of 0.02
 C1'-C2'
 2.2 with sigma of 0.02
 C2-C1
 2.2 with sigma of 0.02
 C2_$2-C2 = C2'_$2-C2'
 1.25 with sigma of 0.02
 C4-C3
 1.54 with sigma of 0.02
 C8-C7_$1 \\sim C7_$1-C9_$1 \\sim C9_$1-C8 \\sim C7-C8_$1 \\sim C8_$1-C9 \\sim
C9-C7
 with sigma of 0.02
 C7-C7_$1 \\sim C8_$1-C7_$1 \\sim C9_$1-C8_$1 \\sim C9-C9_$1 \\sim C9-C8 \\sim
C8-C7
 with sigma of 0.02
 N3_$1-C6 \\sim N3_$1-C7_$1 \\sim N3-C6 \\sim N3-C7
 with sigma of 0.02
3. Restrained planarity
 C6, N3, C7, C7_$1, N3_$1, C8_$1, C9_$1, C9, C8, N4, N4_$1
 with sigma of 0.1
 N4, C9, C8, O1, O2
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(N4) \\sim
Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C1') = Uanis(C1)
Uanis(C4) = Uanis(C7)
5. Rigid body (RIGU) restrains
 C6, C1, N1, C2, C7, C8, C9, C1', C2', N3, N1', N4, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zn1, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C4
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: H6(0.25) C1(0.25) H1(0.25) N3(0.5) N1(0.5) C3(0.125) H3A(0.125)
 H3B(0.125) H3C(0.125) C2(0.5) H2(0.5) C7(0.5) C8(0.25) H8(0.25) C9(0.25)
 C1'(0.25) H1'(0.25) N1'(0.5) O1(0.125) O2(0.125) N4(0.125) C2'(0.5) H2'(0.5)
7.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1), C5(H5), C2(H2), C8(H8), C1'(H1'), C2'(H2')
;
_shelx_res_checksum              86759
_shelx_hkl_checksum              54091