Zirconium-Based Metal‒Organic Framework with 9-Connected Nodes for Ammonia Capture
Chen, Yongwei; Zhang, Xuan; Ma, Kaikai; Chen, Zhijie; Wang, Xingjie; Knapp, Julia; Alayoglu, Selim; Wang, Fenfen; Xia, Qibin; Li, Zhong; Islamoglu, Timur; Farha, Omar K.; ACS Applied Nano Materials 2 (2019) 6098–; doi:10.1021/acsanm.9b01534

data_4516657
_publ_section_title
;
 Zirconium-Based Metal--Organic Framework with 9-Connected Nodes for
 Ammonia Capture
;
_journal_issue                   10
_journal_name_full               'ACS Applied Nano Materials'
_journal_page_first              6098
_journal_paper_doi               10.1021/acsanm.9b01534
_journal_volume                  2
_journal_year                    2019
_chemical_formula_moiety         'C91 H46 N2 O38 Zr6'
_chemical_formula_sum            'C91 H46 N2 O38 Zr6'
_chemical_formula_weight         2322.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7051(6)
_cell_length_b                   24.9288(8)
_cell_length_c                   63.4039(16)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.16
_cell_measurement_theta_min      3.11
_cell_volume                     32726.1(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.875
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            54719
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.382
_diffrn_reflns_theta_min         2.774
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.469
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0487 before and 0.0419 after correction. The Ratio of minimum to maximum transmission is 0.9058. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_description       block
_exptl_crystal_F_000             9200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.417(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         24137
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+31.3390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.873
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                23511
_reflns_number_total             24137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            an9b01534_si_002.cif
_cod_data_source_block           xz93_0m_a
_cod_database_code               4516657
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.723
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.583(7)
 0.417(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C90A-C93A
 1.51 with sigma of 0.02
 C90B-C93B
 1.51 with sigma of 0.02
 N4-C9
 1.5 with sigma of 0.04
 O37-C93A
 1.3 with sigma of 0.04
 C93A-O38B
 1.3 with sigma of 0.04
 C93B-O38A
 1.3 with sigma of 0.04
 C93A-O37
 1.3 with sigma of 0.04
 C93B-O37
 1.3 with sigma of 0.04
 N8-C4
 1.5 with sigma of 0.04
 N4-C10
 1.5 with sigma of 0.04
 C53-C54A \\sim C53-C54B
 with sigma of 0.02
 C53-C58A \\sim C53-C58B
 with sigma of 0.02
 C56-C55A \\sim C56-C55B
 with sigma of 0.02
 C56-C57A \\sim C56-C57B
 with sigma of 0.02
 C54A-C55A \\sim C54B-C55B
 with sigma of 0.02
 C57A-C58A \\sim C57B-C58B
 with sigma of 0.02
 C53-C55A \\sim C53-C55B
 with sigma of 0.04
 C53-C57A \\sim C53-C57B
 with sigma of 0.04
 C56-C54A \\sim C56-C54B
 with sigma of 0.04
 C56-C58A \\sim C56-C58B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C93B) \\sim Ueq, Uanis(C93A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C57B) = Uanis(C57A) = Uanis(C58B) = Uanis(C58A) = Uanis(C54B) =
Uanis(C54A) = Uanis(C55B) = Uanis(C55A)
Uanis(C5) = Uanis(C2) = Uanis(C8)
Uanis(C88A) = Uanis(C92A) = Uanis(C92B) = Uanis(C91B) = Uanis(C89A) =
Uanis(C91A) = Uanis(C89B) = Uanis(C88B)
Uanis(C93A) = Uanis(C93B)
Uanis(C90A) = Uanis(C90B)
Uanis(O37) = Uanis(O38B)
Uanis(N027) = Uanis(N8) = Uanis(N4)
Uanis(C6) = Uanis(C7) = Uanis(C9) = Uanis(C10)
5. Others
 Sof(C88A)=Sof(H88A)=Sof(C89A)=Sof(H89A)=Sof(C91A)=Sof(H91A)=Sof(C92A)=
 Sof(H92A)=1-FVAR(1)
 Sof(C89B)=Sof(H89B)=Sof(C88B)=Sof(H88B)=Sof(C92B)=Sof(H92B)=Sof(C91B)=
 Sof(H91B)=FVAR(1)
 Sof(O38A)=1-FVAR(2)
 Sof(O38B)=FVAR(2)
 Sof(C90B)=1-FVAR(3)
 Sof(C90A)=FVAR(3)
 Sof(C93B)=1-FVAR(4)
 Sof(C93A)=FVAR(4)
 Sof(C54B)=Sof(C55B)=Sof(C57B)=Sof(C58B)=1-FVAR(5)
 Sof(C57A)=Sof(C55A)=Sof(C54A)=Sof(C58A)=FVAR(5)
 Fixed Sof: C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) N8(0.5) C8(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) H4C(0.5) N4(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C2(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C75(H75), C21(H21), C79(H79), C19(H19), C41(H41), C78(H78), C76(H76),
 C39(H39), C81(H81), C46(H46), C43(H43), C47(H47), C28(H28), C29(H29), C20(H20),
  C50(H50), C33(H33), C22(H22), C37(H37), C49(H49), C85(H85), C34(H34), C1(H1),
 C36(H36), C83(H83), C13(H13), C17(H17), C25(H25), C15(H15), C26(H26),
 C89B(H89B), C88B(H88B), C92B(H92B), C91B(H91B), C88A(H88A), C89A(H89A),
 C91A(H91A), C92A(H92A)
6.b Fitted hexagon refined as free rotating group:
 C90B(C89B,C88B,C87,C92B,C91B)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'