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_4126000
_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         '0.08(C480 H276 Cl48 N240 O96 Zn48)'
_chemical_formula_sum            'C40 H23 Cl4 N20 O8 Zn4'
_chemical_formula_weight         1315.06
_chemical_name_common            ZIF-615
_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   'rigid body and difmap'
_audit_creation_date             2016-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   31.731(6)
_cell_length_b                   31.731(6)
_cell_length_c                   28.412(6)
_cell_measurement_reflns_used    10270
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.737
_cell_measurement_theta_min      1.625
_cell_volume                     24774(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd., Version 171.37.33
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd., Version 171.37.33
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd., 171.37.33
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  SHELXL-2014/6
_computing_structure_solution    'SHELXT 2014/4'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'PILATUS3 6M'
_diffrn_measurement_method       '\f shutterless scans'
_diffrn_radiation_monochromator  'double crystal, Si(111)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8999
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4924
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        18.750
_diffrn_reflns_theta_max         18.737
_diffrn_reflns_theta_min         1.625
_diffrn_source
;
Advanced Light Source, Station 5.0.2
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   absscale
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_description       Rod
_exptl_crystal_F_000             7860
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.2577
_refine_ls_R_factor_gt           0.1933
_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^)+(0.2500P)^2^+250.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4933
_refine_ls_wR_factor_ref         0.5500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2548
_reflns_number_total             4924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_015.cif
_cod_data_source_block           ZIF-615
_cod_depositor_comments
'Adding full bibliography for 4125998--4126004.cif.'
_cod_original_cell_volume        24774(11)
_cod_database_code               4126000
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.911(4) 0.089(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Cl(H) groups
3. Uiso/Uaniso restraints and constraints
Cl51 \\sim C28 \\sim C27 \\sim Cl52: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C14 \\sim N10 \\sim N9 \\sim C12 \\sim C13 \\sim N15 \\sim O59 \\sim O60:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Cl52 \\sim C27 \\sim C26 \\sim C25 \\sim C21 \\sim C29 \\sim C28 \\sim Cl51:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
N31 \\sim H8 \\sim O43 \\sim O44 \\sim C8: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O59 \\sim N15 \\sim O60 \\sim C12 \\sim N9 \\sim C14 \\sim N10 \\sim C13:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C18 \\sim C19 \\sim C20 \\sim Cl56: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C33 \\sim N17 \\sim C18 \\sim C19 \\sim C20 \\sim Cl56: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: H6(0.5) Cl41(0.5) H13(0.5) H30(0.5) N32(0.5) O34(0.5) O35(0.5)
 H20(0.5) Cl56(0.5) H27(0.5) H28(0.5) Cl52(0.5) H8(0.5) N31(0.5) O43(0.5)
 O44(0.5)
 Fixed X: N3(0.52492)
 Fixed Y: N3(0.54458)
 Fixed Z: N3(0.654181)
5.a Free rotating group:
 N3(C4,C5,H5,C6,H6,C63,H63,Cl41), N9(N10,C12,C13,H13,C14,N15,O59,O60), N16(C30,
 H30,N32,O34,O35,C64,H64), N17(C18,C19,H19,C20,H20,C33,H33,Cl56), C21(N22,C24,
 H24,C25,C26,C27,H27,C28,H28,Cl52,H26,N23,C29,H29,Cl51), C65(H65,N7,C8,H8,N31,
 O43,O44)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14)
;
_shelx_fab_checksum              48689
_olex2_submission_special_instructions 'No special instructions were received'