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_4132925
_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(C216 H112 O72 Zr12)'
_chemical_formula_sum            'C54 H30 O18 Zr3'
_chemical_formula_weight         1240.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C 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                   23.1663(6)
_cell_length_b                   34.0796(8)
_cell_length_c                   14.9174(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.632
_cell_measurement_theta_min      3.756
_cell_volume                     11777.3(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      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29355
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.767
_diffrn_reflns_theta_max         66.767
_diffrn_reflns_theta_min         3.755
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6279
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.700
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.232
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1499P)^2^+30.3834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4561
_reflns_number_total             5564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07411_si_002.cif
_cod_data_source_block           PCN-606-BDC-TPDC
_cod_database_code               4132925
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.794
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C20-C21_$2
 1.39 with sigma of 0.02
 C20-C21_$1
 2.4 with sigma of 0.02
 C20-C20_$1
 2.8 with sigma of 0.02
 C19-C17 \\sim C17-C17_$3 \\sim C19_$3-C17_$3 \\sim C19_$3-C17_$4 \\sim
C17_$5-C17_$4 \\sim C19-
 C17_$5
 with sigma of 0.02
3. Restrained planarity
 C21, C21, C20, C21, C21, C20
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C21) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C21) = Uanis(C20) = Uanis(C10) = Uanis(C11) = Uanis(C8) = Uanis(C15)
5. Others
 Fixed Sof: H3(0.5) C21(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3a), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17)
6.b Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              66418
_shelx_hkl_checksum              99413
_shelx_fab_checksum              23059
_olex2_submission_special_instructions 'No special instructions were received'