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_4132919
_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(C436 H240 N8 O128 Zr24)'
_chemical_formula_sum            'C109 H64 N2 O32 Zr6'
_chemical_formula_weight         2460.94
_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                   23.2150(8)
_cell_length_b                   30.6351(11)
_cell_length_c                   33.5480(8)
_cell_measurement_reflns_used    6007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      53.9217
_cell_measurement_theta_min      2.3144
_cell_volume                     23859.1(13)
_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 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.1227
_diffrn_reflns_av_unetI/netI     0.1209
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            26608
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        54.134
_diffrn_reflns_theta_max         54.134
_diffrn_reflns_theta_min         2.314
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.685
_exptl_crystal_description       block
_exptl_crystal_F_000             4912
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         7418
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.645
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1532P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2213
_refine_ls_wR_factor_ref         0.2429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4194
_reflns_number_total             7418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07411_si_003.cif
_cod_data_source_block           PCN-609-BDC-BPDC-TPDC
_cod_database_code               4132919
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.797
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C17-C33
 2.2 with sigma of 0.005
 C34-C26
 2.2 with sigma of 0.005
 C32-C34
 2.2 with sigma of 0.005
 C32-C26
 2.2 with sigma of 0.005
 C38-C35
 1.4 with sigma of 0.005
 C38_$1-C38
 1.4 with sigma of 0.005
 C38_$2-C38
 2.2 with sigma of 0.005
 C38_$1-C38_$3
 2.2 with sigma of 0.005
 C12-C34
 1.4 with sigma of 0.0005
 C34-C17 = C32-C17 = C33-C32 = C33-C26 = C26-C12
 1.4 with sigma of 0.0005
 C33-C17
 2.2 with sigma of 0.005
 C26-C34
 2.2 with sigma of 0.005
 C12-C17
 2.2 with sigma of 0.005
 C12-C33
 2.2 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C1) \\sim
Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(C17) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C15) \\sim Ueq: with
sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C11) = Uanis(C25) = Uanis(C28) = Uanis(C21) = Uanis(C27) = Uanis(C24) =
Uanis(C19)
Uanis(C31) = Uanis(C22) = Uanis(C13) = Uanis(C20) = Uanis(C10) = Uanis(C16) =
Uanis(C29)
Uanis(N5) = Uanis(C36) = Uanis(C30) = Uanis(C15) = Uanis(C23) = Uanis(C14) =
Uanis(C18)
Uanis(C9) = Uanis(C34) = Uanis(C17) = Uanis(C32) = Uanis(C33) = Uanis(C26) =
Uanis(C12) = Uanis(C35)
Uanis(C38) = Uanis(C35) = Uanis(C32)
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(O3)
Uanis(C5) = Uanis(C8) = Uanis(C1) = Uanis(C7) = Uanis(C6)
4. Others
 Fixed Sof: C38(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C22(H22), C24(H24), C26(H26), C28(H28), C29(H29), C33(H33), C34(H34),
  N5(H5)
;
_shelx_res_checksum              2837
_shelx_hkl_checksum              1055
_shelx_fab_checksum              47968
_olex2_submission_special_instructions 'No special instructions were received'