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_4128885
_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(C384 H240 N12 O96 Zr18)'
_chemical_formula_sum            'C128 H80 N4 O32 Zr6'
_chemical_formula_weight         2733.28
_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             2019-05-10
_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                   27.4034(7)
_cell_length_b                   27.4034(7)
_cell_length_c                   27.4034(7)
_cell_measurement_reflns_used    3075
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.28
_cell_volume                     20578.5(9)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_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  0.1680
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27592
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        40.409
_diffrn_reflns_theta_max         40.409
_diffrn_reflns_theta_min         2.280
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.096
_exptl_absorpt_correction_T_max  30.4230
_exptl_absorpt_correction_T_min  2.2801
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.662
_exptl_crystal_description       block
_exptl_crystal_F_000             4116
_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         0.905
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1324
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1960
_refine_ls_R_factor_gt           0.1119
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3075
_refine_ls_wR_factor_ref         0.3482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                600
_reflns_number_total             1324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05580_si_003.cif
_cod_data_source_block           mm
_cod_original_cell_volume        20578.5(16)
_cod_database_code               4128885
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.818
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C2 = C4-C3 = C5-C4
 1.4 with sigma of 0.005
 C2-C5
 2.8 with sigma of 0.005
 C4-C4_$1 = C11-C15 = C12-C14 = C10-C12 = C10-C14
 2.4 with sigma of 0.005
 C10-C11 = C12-C11 = C13-C12 = C14-C13 = C14-C15 = C15-C10 = C16-C17
 1.4 with sigma of 0.005
 C18-C17 = C5-C6
 1.5 with sigma of 0.005
 Zr1-C9
 3.2 with sigma of 0.005
 C9-C15
 2.5 with sigma of 0.005
 C16-C16_$4 = C16_$4-C16_$3 = C16-C16_$3
 2.4 with sigma of 0.005
 C8_$1-C8_$2 = C8_$1-C7_$1 = N1_$2-C7_$1 = N1_$2-C7_$2 = C8_$2-C7_$2
 1.4 with sigma of 0.005
 C2-C1
 1.5 with sigma of 0.005
 O3-C9 \\sim O2-C9
 with sigma of 0.02
 C9-C15 \\sim C9-C11
 with sigma of 0.02
 C16-C14 \\sim C16-C12
 with sigma of 0.02
3. Restrained planarity
 C18, C17, C16_$3, C18_$3, C17_$3, C16_$4, C16, C17_$4, C18_$4
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4) \\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(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) = Uanis(C14) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10) =
Uanis(C9) = Uanis(C17) = Uanis(C16) = Uanis(C18)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C7) = Uanis(C8) = Uanis(N1)
5. Others
 Fixed Sof: H18A(0.5) H18B(0.5) H18C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C15(H15), C12(H12), C11(H11), C14(H14)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              40150
_shelx_hkl_checksum              63726
_olex2_submission_special_instructions 'No special instructions were received'