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_4126004
_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         'C7.5 H7.4 N4.2 O0.4 Zn'
_chemical_formula_sum            'C7.5 H7.4 N4.2 O0.4 Zn'
_chemical_formula_weight         228.15
_chemical_name_common            ZIF-486
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120
_cell_formula_units_Z            24
_cell_length_a                   27.0807(16)
_cell_length_b                   27.0807(16)
_cell_length_c                   16.7619(16)
_cell_measurement_reflns_used    5520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.863
_cell_measurement_theta_min      2.311
_cell_volume                     10645.7(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15269
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        20.050
_diffrn_reflns_theta_max         20.042
_diffrn_reflns_theta_min         2.311
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1185 before and 0.0719 after correction.
The Ratio of minimum to maximum transmission is 0.7002.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.854
_exptl_crystal_description       Block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1469
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.1153
_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^+75.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3275
_refine_ls_wR_factor_ref         0.3525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1003
_reflns_number_total             1469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_012.cif
_cod_data_source_block           ZIF-486_GME
_cod_depositor_comments
'Adding full bibliography for 4125998--4126004.cif.'
_cod_original_cell_volume        10645.7(16)
_cod_original_formula_sum        'C7.50 H7.40 N4.20 O0.40 Zn'
_cod_database_code               4126004
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.725
_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
 C4_$4-C4
 1.4 with sigma of 0.02
 N2-C5
 1.3 with sigma of 0.02
 O1-N5 = O2-N5
 1.25 with sigma of 0.02
 O2-O1
 2.4 with sigma of 0.02
 C1-C1_$3
 1.4 with sigma of 0.02
 C8-C7
 2.2 with sigma of 0.02
 N2_$4-N2
 2.2 with sigma of 0.02
 C2-C1
 2.2 with sigma of 0.02
 C10-C11
 1.4 with sigma of 0.02
 C11-C12
 1.4 with sigma of 0.02
 C10-C10_$2
 1.4 with sigma of 0.02
 C12-C12_$2
 1.4 with sigma of 0.02
 C10-C12
 2.42 with sigma of 0.02
 C10-C9
 2.2 with sigma of 0.04
 C12-O2
 2.5 with sigma of 0.02
 C12-O1
 2.5 with sigma of 0.02
 N5-C12
 1.5 with sigma of 0.02
 O2-O1
 2.4 with sigma of 0.02
 O1-N5 = O2-N5
 1.25 with sigma of 0.02
 C2-C3
 1.54 with sigma of 0.02
 N2-C5
 1.36 with sigma of 0.02
 N4-C9 \\sim N4-C10
 with sigma of 0.02
 C5-N2 \\sim N4-C10
 with sigma of 0.02
3. Restrained planarity
 N3_$1, N3, C8, C7_$1, C7
 with sigma of 0.1
 N4, N4_$2, C9, C10, C10_$2, C11_$2, C11, C12, C12_$2, N5, N5_$2
 with sigma of 0.1
 C12, O2, N5, O1
 with sigma of 0.1
 N2_$4, N2, C4, C4_$4, C5, C6
 with sigma of 0.1
 N1, N1_$3, C2, C1, C1_$3, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12)
Uanis(C1) = Uanis(C2)
Uanis(C7) = Uanis(C8)
5. Rigid body (RIGU) restrains
 C12, O2, N5, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zn1, N2, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H2(0.3) H10(0.6) C11(0.4) H11(0.4) C12(0.4) O2(0.2) N5(0.2)
 O1(0.2) C3(0.2) H3A(0.2) H3B(0.2) H3C(0.2) H6A(0.5) H6B(0.5) H6C(0.5)
7.a Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C7(H7), C11(H11), C4(H4), C1(H1)
;
_shelx_res_checksum              34759
_shelx_hkl_checksum              54701