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_4126184
_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         '0.03(C270 H144 Cl18 N153 O18 Zn36)'
_chemical_formula_sum            'C7.5 H4 Cl0.5 N4.25 O0.5 Zn'
_chemical_formula_weight         244.74
_chemical_name_common            ZIF-303
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-16
_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            36
_cell_length_a                   26.9457(15)
_cell_length_b                   26.9457(15)
_cell_length_c                   26.763(2)
_cell_measurement_reflns_used    2560
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.337
_cell_measurement_theta_min      2.076
_cell_volume                     16828.5(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      298(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2560
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        18.360
_diffrn_reflns_theta_max         18.337
_diffrn_reflns_theta_min         2.076
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.869
_exptl_crystal_description       Block
_exptl_crystal_F_000             4365
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         2560
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.2176
_refine_ls_R_factor_gt           0.1247
_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^+400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3101
_refine_ls_wR_factor_ref         0.4031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1427
_reflns_number_total             2560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_002.cif
_cod_data_source_block           ZIF-303_CHA
_cod_original_cell_volume        16828(2)
_cod_original_formula_sum        'C7.50 H4 Cl0.50 N4.25 O0.50 Zn'
_cod_database_code               4126184
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.782
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.563(10) 0.437(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C8-Cl2
 1.7 with sigma of 0.02
 C7-Cl1
 1.7 with sigma of 0.02
 C17-Cl3
 1.7 with sigma of 0.02
 C18-Cl4
 1.7 with sigma of 0.02
 C15-N6
 2.52 with sigma of 0.04
 N10-O2
 1.25 with sigma of 0.02
 N10-O1
 1.25 with sigma of 0.02
 N5-C15
 1.36 with sigma of 0.02
 C20-N5
 2.5 with sigma of 0.04
 C14-C20
 2.52 with sigma of 0.04
 C14-N6
 1.36 with sigma of 0.02
 N10-C1
 1.5 with sigma of 0.02
 C20-N6
 1.36 with sigma of 0.02
 C10-C8 \\sim C8-C6 \\sim C6-C10 \\sim C5-C9 \\sim C9-C7 \\sim C7-C5
 with sigma of 0.02
 C5-C10 \\sim C6-C5 \\sim C7-C6 \\sim C8-C7 \\sim C8-C9 \\sim C9-C10
 with sigma of 0.02
4. Restrained planarity
 C14, C5, C6, C7, Cl1, C8, Cl2, C9, C10
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C14 \\sim N5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C11 \\sim N7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim N2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N10) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl1) = Uanis(Cl2)
Uanis(O1) = Uanis(O2)
6. Rigid body (RIGU) restrains
 N7, C13, C12, N8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C16, C19, C17, C15, C18, Cl4, N5, Cl3, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C2, N1, C1, N2, Zn1, N10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C7, C6, C5, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C10, N3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C12(0.5) H12(0.5) C13(0.5) H13(0.5) O2(0.5) O1(0.5) N10(0.5)
 C6(0.5) H6(0.5) C9(0.5) H9(0.5) C7(0.5) C8(0.5) Cl1(0.25) Cl2(0.25) C17(0.5)
 C18(0.5) C19(0.5) H19(0.5) C16(0.5) H16(0.5) Cl4(0.25) Cl3(0.25)
8.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C4(H4), C2(H2), C3(H3), C6(H6),
 C9(H9), C19(H19), C16(H16)
8.b Fitted pentagon refined as free rotating group:
 N7(C11,N8,C12,C13), C5(C10,N4,C4,N3), N2(C1,N1,C2,C3)
8.c Fitted hexagon refined as free rotating group:
 C17(C18,C19,C20,C15,C16)
;
_shelx_res_checksum              38201
_shelx_hkl_checksum              10884
_shelx_fab_checksum              41218