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_4132923
_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         '0.5(C176 H88 O72 Zr12)'
_chemical_formula_sum            'C88 H44 O36 Zr6'
_chemical_formula_weight         2224.55
_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            2
_cell_length_a                   21.531(3)
_cell_length_b                   35.053(4)
_cell_length_c                   15.0898(17)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.7741
_cell_measurement_theta_min      2.2201
_cell_volume                     11389(2)
_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
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69179
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        22.833
_diffrn_reflns_theta_max         22.833
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.299
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.649
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.232
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1334P)^2^+67.5614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3078
_reflns_number_total             4243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07411_si_002.cif
_cod_data_source_block           PCN-606-BDC
_cod_database_code               4132923
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5-C20
 1.5 with sigma of 0.005
 C1AA-C1AA_$1
 2.2 with sigma of 0.005
 C1AA_$2-C1AA_$3
 2.2 with sigma of 0.005
 C5-C1AA_$2
 2.2 with sigma of 0.005
 C5_$3-C1AA_$1
 2.2 with sigma of 0.005
 C1AA_$3-C5
 2.2 with sigma of 0.005
 O7-C20 \\sim O7_$1-C20
 with sigma of 0.02
 C5-C1AA \\sim C1AA-C1AA_$2 \\sim C5_$3-C1AA_$2 \\sim C5_$3-C1AA_$3 \\sim
C1AA_$1-C1AA_$3 \\sim C5-
 C1AA_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(O7) = Uanis(C5) = Uanis(C1AA)
4.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C21(H21), C23(H23), C24(H24), C1AA(H1AA)
;
_shelx_res_checksum              79901
_shelx_hkl_checksum              10133
_shelx_fab_checksum              33051
_olex2_submission_special_instructions 'No special instructions were received'