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_4132918
_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         '0.13(C424 H216 N8 O128 Zr24)'
_chemical_formula_sum            'C53 H27 N O16 Zr3'
_chemical_formula_weight         1207.41
_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     dual
_audit_creation_date             2018-06-24
_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            8
_cell_length_a                   23.1736(6)
_cell_length_b                   31.6350(9)
_cell_length_c                   32.1726(9)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.37
_cell_measurement_theta_min      2.35
_cell_volume                     23585.6(11)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.02
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            65988
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        62.662
_diffrn_reflns_theta_max         62.662
_diffrn_reflns_theta_min         2.350
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.6317
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    0.680
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.865
_refine_diff_density_min         -2.309
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         9944
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1132P)^2^+130.0655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7515
_reflns_number_total             9944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07411_si_003.cif
_cod_data_source_block           PCN-609-BPDC-TPDC
_cod_database_code               4132918
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C8_$1-C8
 2.2 with sigma of 0.005
 C30-C29
 2.2 with sigma of 0.005
 C34-C33
 1.4 with sigma of 0.005
 C34-C35
 2.2 with sigma of 0.005
 C35-C33 \\sim C34-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3) = Uanis(C1) = Uanis(C2) = Uanis(C6) = Uanis(C8) = Uanis(C4)
Uanis(C3) = Uanis(C11) = Uanis(C31) = Uanis(C30) = Uanis(C24) = Uanis(C29) =
Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35)
4. Others
 Fixed Sof: C34(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), N1(H1), C10(H10), C12(H12), C13(H13), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31)
;
_shelx_res_checksum              58865
_shelx_hkl_checksum              63028
_shelx_fab_checksum              63618
_olex2_submission_special_instructions 'No special instructions were received'