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_4132488
_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         'C58 H30 O16 Zr3'
_chemical_formula_sum            'C58 H30 O16 Zr3'
_chemical_formula_weight         1256.53
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.159(3)
_cell_length_b                   33.299(4)
_cell_length_c                   20.824(2)
_cell_measurement_reflns_used    9635
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      15.58
_cell_measurement_theta_min      2.24
_cell_volume                     16059(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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            189780
_diffrn_reflns_theta_full        15.78
_diffrn_reflns_theta_max         15.78
_diffrn_reflns_theta_min         0.91
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1219 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.9253.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13420
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         5.540
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       0.0035(11)
_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   1.793
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         9734
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.797
_refine_ls_R_factor_all          0.1840
_refine_ls_R_factor_gt           0.1238
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3337
_refine_ls_wR_factor_ref         0.4419
_reflns_number_gt                6114
_reflns_number_total             9734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b04277_si_012.cif
_cod_data_source_block           NPF-300-8
_cod_database_code               4132488
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15-C16 = C17-C16 = C18-C17
 1.38 with sigma of 0.02
 C20-C19 = C21-C20 = C21-C22
 1.38 with sigma of 0.02
 C22-C20
 2.38 with sigma of 0.04
 C21-C19
 2.38 with sigma of 0.04
3. Rigid bond restraints
 C14, C15, C16, C17, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim
C22: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C7(H7), C6(H6), C3(H3), C4(H4), C10(H10), C16(H16), C17(H17),
 C22(H22), C21(H21)
;
_olex2_submission_special_instructions 'No special instructions were received'