Face-Sharing Archimedean Solids Stacking for the Construction of Mixed-Ligand Metal-Organic Frameworks.
Qiu, Yu-Chen; Yuan, Shuai; Li, Xiao-Xin; Du, Dong-Ying; Wang, Cong; Qin, Jun-Sheng; Drake, Hannah F.; Lan, Ya-Qian; Jiang, Lei; Zhou, Hong-Cai; Journal of the American Chemical Society 141 (2019) 13841–13848; doi:10.1021/jacs.9b05580

data_4128884
_publ_section_title
;
 Face-Sharing Archimedean Solids Stacking for the Construction of
 Mixed-Ligand Metal-Organic Frameworks.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13841
_journal_page_last               13848
_journal_paper_doi               10.1021/jacs.9b05580
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.33(C936 H480 N60 O180 Zn63)'
_chemical_formula_sum            'C312 H160 N20 O60 Zn21'
_chemical_formula_weight         6521.36
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-04-24
_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            3
_cell_length_a                   43.4917(16)
_cell_length_b                   43.4917(16)
_cell_length_c                   43.4917(16)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.20
_cell_volume                     82266(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            399034
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.292
_diffrn_reflns_theta_max         23.292
_diffrn_reflns_theta_min         0.662
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0900 before and 0.0709 after correction. The Ratio of minimum to maximum transmission is 0.6706. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.395
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             9846
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.053
_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     136
_refine_ls_number_reflns         11042
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1647
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+23.5881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.2106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7032
_reflns_number_total             11042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05580_si_002.cif
_cod_data_source_block           mo_btbtcppzn_0m
_cod_original_cell_volume        82266(9)
_cod_database_code               4128884
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.954
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.4 with sigma of 0.005
 C23-C24 = C23-C22 = C22-C21
 1.4 with sigma of 0.005
 C27-C26
 1.4 with sigma of 0.005
 C17-C17_$1
 1.4 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(Zn3) \\sim Ueq, Uanis(Zn4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(N3) = Uanis(C26) = Uanis(C27) = Uanis(C24) = Uanis(C25) = Uanis(C23) =
Uanis(C22) = Uanis(C21)
Uanis(N1) = Uanis(C16) = Uanis(N2) = Uanis(C17) = Uanis(C15) = Uanis(C18) =
Uanis(C19) = Uanis(C12) = Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C14) =
Uanis(C13) = Uanis(C8)
Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) =
Uanis(C26) = Uanis(C27) = Uanis(N3)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C7)
4.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C19(H19), C10(H10), C13(H13), C7(H7), C3(H3), C11(H11),
 C4(H4), C22(H22), C27(H27), C23(H23)
;
_shelx_res_checksum              89738
_shelx_hkl_checksum              77770
_olex2_submission_special_instructions 'No special instructions were received'