Topology-Guided Stepwise Insertion of Three Secondary Linkers in Zirconium Metal-Organic Frameworks.
Zhang, Xin; Frey, Brandon L.; Chen, Yu-Sheng; Zhang, Jian; Journal of the American Chemical Society 140 (2018) 7710–7715; doi:10.1021/jacs.8b04277

data_4132491
_publ_section_title
;
 Topology-Guided Stepwise Insertion of Three Secondary Linkers in
 Zirconium Metal-Organic Frameworks.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7710
_journal_page_last               7715
_journal_paper_doi               10.1021/jacs.8b04277
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C125 H60 O32 Zr6'
_chemical_formula_sum            'C125 H60 O32 Zr6'
_chemical_formula_weight         2621.05
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.1544(12)
_cell_length_b                   33.1052(17)
_cell_length_c                   40.833(2)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      12.241
_cell_measurement_theta_min      2.192
_cell_volume                     31300(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12050
_diffrn_reflns_theta_full        13.30
_diffrn_reflns_theta_max         13.30
_diffrn_reflns_theta_min         0.85
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             26070
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.122
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       0.0044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         12050
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1846P)^2^+90.0162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2678
_refine_ls_wR_factor_ref         0.3054
_reflns_number_gt                7800
_reflns_number_total             12050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b04277_si_007.cif
_cod_data_source_block           NPF-300-3
_cod_database_code               4132491
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C38-C37
 1.46 with sigma of 0.02
 C37-C36
 1.38 with sigma of 0.02
 C38-C36
 2.5 with sigma of 0.04
 C38-C33
 3.1 with sigma of 0.04
 C33-C37
 2.5 with sigma of 0.04
3. Restrained planarity
 C33, C36, C37, C38
 with sigma of 0.03
4. Rigid bond restraints
 C29, C30, C35, C34, C33, C32, C31, C36, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, C29, O8, C30, C31, C32, C33, C35, C34, C36, C37, C38
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31 \\sim C37 \\sim
C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O7 \\sim C29 \\sim O8 \\sim C30 \\sim C31 \\sim C32 \\sim C35 \\sim C34 \\sim
C33 \\sim C36 \\sim C37 \\sim C38: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
6. Others
 Fixed Sof: C38(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C41(H41), C16(H16), C18(H18), C15(H15), C3(H3), C42(H42), C6(H6),
 C19(H19), C4(H4), C31(H31), C32(H32), C35(H35), C26(H26), C13(H13), C27(H27),
 C9(H9), C34(H34), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'