Enhancing Pore-Environment Complexity Using a Trapezoidal Linker: Toward Stepwise Assembly of Multivariate Quinary Metal-Organic Frameworks.
Pang, Jiandong; Yuan, Shuai; Qin, Junsheng; Wu, Mingyan; Lollar, Christina T.; Li, Jialuo; Huang, Ning; Li, Bao; Zhang, Peng; Zhou, Hong-Cai; Journal of the American Chemical Society 140 (2018) 12328–12332; doi:10.1021/jacs.8b07411

data_4132920
_publ_section_title
;
 Enhancing Pore-Environment Complexity Using a Trapezoidal Linker: Toward
 Stepwise Assembly of Multivariate Quinary Metal-Organic Frameworks.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12328
_journal_page_last               12332
_journal_paper_doi               10.1021/jacs.8b07411
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.25(C420 H216 N16 O128 Zr24)'
_chemical_formula_sum            'C105 H54 N4 O32 Zr6'
_chemical_formula_weight         2430.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-19
_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            4
_cell_length_a                   20.8534(9)
_cell_length_b                   32.2081(14)
_cell_length_c                   33.4473(16)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.8142
_cell_measurement_theta_min      3.6553
_cell_volume                     22464.8(17)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            39867
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        51.869
_diffrn_reflns_theta_max         51.869
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.523
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.719
_exptl_crystal_description       block
_exptl_crystal_F_000             4832
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.988
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.292
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0859P)^2^+68.9378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5392
_reflns_number_total             6716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07411_si_003.cif
_cod_data_source_block           PCN-609-BDC-BPDC-AZDC
_cod_database_code               4132920
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C27-C22 = C27-C26 = C26-C25 = C25-C24 = C24-C23 = C23-C22
 1.4 with sigma of 0.005
 C24-C26 = C22-C26 = C25-C27
 2.2 with sigma of 0.005
 C25-C23
 2.2 with sigma of 0.005
 C27-C23
 2.2 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) =
Uanis(C27) = Uanis(N3) = Uanis(N2)
Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13)
Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19)
Uanis(C4) = Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C2) = Uanis(C3)
Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C13(H13), C15(H15), C16(H16),
 C18(H18), C19(H19), C23(H23), C24(H24), C26(H26), C27(H27), C30(H30), C31(H31),
  C35(H35)
;
_shelx_res_checksum              88096
_shelx_hkl_checksum              55740
_shelx_fab_checksum              50745
_olex2_submission_special_instructions 'No special instructions were received'