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_4126003
_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         'C22 H12.25 Br2.25 N9 O2 Zn2, 0.25(Br)'
_chemical_formula_sum            'C22 H13.5 Br2.5 N9 O2 Zn2'
_chemical_formula_weight         766.43
_chemical_name_common            ZIF-725
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m 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                120
_cell_formula_units_Z            24
_cell_length_a                   42.586(3)
_cell_length_b                   42.586(3)
_cell_length_c                   19.8692(13)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.680
_cell_measurement_theta_min      2.409
_cell_volume                     31206(4)
_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 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD diffractometer'
_diffrn_measurement_method       '/w scans with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0332
_diffrn_reflns_av_R_equivalents  0.2655
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            90065
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        21.985
_diffrn_reflns_theta_max         21.965
_diffrn_reflns_theta_min         2.124
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1820 before and 0.1289 after correction.
The Ratio of minimum to maximum transmission is 0.5146.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.979
_exptl_crystal_description       Block
_exptl_crystal_F_000             8928
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         2411
_refine_ls_number_restraints     473
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1996
_refine_ls_R_factor_gt           0.1621
_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^+700.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4143
_refine_ls_wR_factor_ref         0.4377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1548
_reflns_number_total             2411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02272_si_016.cif
_cod_data_source_block           ZIF-725_bam
_cod_depositor_comments
'Adding full bibliography for 4125998--4126004.cif.'
_cod_original_formula_sum        'C22 H13.50 Br2.50 N9 O2 Zn2'
_cod_database_code               4126003
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.737
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Zn2-N10 = Zn2_$1-N10_$1
 2 with sigma of 0.02
 N4-C4
 1.5 with sigma of 0.02
 O2-N4 = O2_$1-N4
 1.25 with sigma of 0.02
 C3-C3_$1
 1.4 with sigma of 0.02
 C1-C1_$2
 1.4 with sigma of 0.02
 C3-C4
 2.3 with sigma of 0.02
 C20-C21
 2.3 with sigma of 0.02
 C17-C16
 2.3 with sigma of 0.02
 C24-C25
 2.2 with sigma of 0.02
 Br5-C27 = Br5_$4-C27_$4
 1.8 with sigma of 0.02
 C9-C10
 2.3 with sigma of 0.02
 C6-C5
 2.3 with sigma of 0.02
 C15-C14
 1.39 with sigma of 0.02
 Br3-C19 = Br4-C23 = Br2'-C13 = Br2-C12 = Br1-C8
 1.8 with sigma of 0.02
 N2-C2
 1.5 with sigma of 0.02
 O1-N2
 1.25 with sigma of 0.02
 Zn1-N3
 2 with sigma of 0.02
 O2_$1-O2 \\sim O2-C4
 with sigma of 0.02
 N10-C20 \\sim N10-C21
 with sigma of 0.02
 N9-C16 \\sim N9-C17
 with sigma of 0.02
 N8-C24 \\sim N8-C25
 with sigma of 0.02
 N6-C9 \\sim N6-C10 \\sim N7-C9 \\sim N7-C15
 with sigma of 0.02
 N3-C4 \\sim N3-C3
 with sigma of 0.02
 C2-O1 \\sim O1-O1_$2
 with sigma of 0.02
3. Restrained planarity
 N8, N8_$4, C25_$4, C25, C24, C27, C27_$4, C26_$4, C26, Br5_$4, Br5
 with sigma of 0.1
 N5_$3, C5, N5, C6, C6_$3, C7_$3, C8_$3, C8, C7
 with sigma of 0.1
 N3, N3_$1, N4, C3, C3_$1, C4, O2_$1, O2
 with sigma of 0.1
 C9, N7, C10, N6, C15, C14, C13, C12, C11, Br2', Br2
 with sigma of 0.1
 O1, O1_$2, N1, N1_$2, N2, C1, C1_$2, C2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim C3 \\sim C4 \\sim O2: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C2 \\sim N2 \\sim O1: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Br1) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br2') \\sim Ueq, Uanis(Br3)
\\sim Ueq, Uanis(Br4) \\sim Ueq, Uanis(Br5) \\sim Ueq: with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C5) = Uanis(C24)
Uanis(N5) = Uanis(N8)
Uanis(C6) = Uanis(C25)
Uanis(C7) = Uanis(C26)
Uanis(C8) = Uanis(C27)
Uanis(Br2') = Uanis(Br2)
Uanis(Zn1) = Uanis(Zn2)
5. Rigid body (RIGU) restrains
 Zn1, Zn2, C1, C5, C6, C7, C8, C3, C4, C9, C15, C14, C13, C12, C11, C10, C16,
 C17, C18, C19, C25, C24, C20, C21, C22, C23, C27, C26, N1, N7, N9, N2, N5, N3,
 N6, N4, N10, N8, Br1, Br4, Br3, Br2', Br2, Br5, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Br1(0.5) H8(0.5) C14(0.75) H14(0.75) H15(0.25) C11(0.75) H11(0.75)
 C12(0.75) H12(0.375) C13(0.75) H13(0.375) H19(0.5) H25(0.5) H23(0.5) C27(0.5)
 H27(0.25) Br4(0.5) Br3(0.5) Br2'(0.375) Br2(0.375) C26(0.5) H26(0.5) Br5(0.25)
7.a Riding coordinates:
 C27(H27)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C3(H3), C9(H9), C14(H14), C15(H15), C11(H11),
 C12(H12), C13(H13), C16(H16), C18(H18), C19(H19), C25(H25), C24(H24), C20(H20),
  C22(H22), C23(H23), C26(H26)
7.c Fitted hexagon refined as free rotating group:
 C14(C15,C10,C11,C12,C13)
;
_shelx_res_checksum              69926
_shelx_hkl_checksum              91809