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_4132492
_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         'C60 H30 O24 Zr3'
_chemical_formula_sum            'C60 H30 O24 Zr3'
_chemical_formula_weight         1280.50
_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             2017-07-27
_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                   21.1374(11)
_cell_length_b                   33.1766(18)
_cell_length_c                   21.4671(10)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      12.809
_cell_measurement_theta_min      2.212
_cell_volume                     15054.2(13)
_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      273.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0193
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9978
_diffrn_reflns_theta_full        12.86
_diffrn_reflns_theta_max         12.86
_diffrn_reflns_theta_min         0.86
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.9498.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12540
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.278
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.020(3)
_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   1.483
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.493
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.1027
_refine_ls_shift/su_max          0.001
_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          0.3260
_refine_ls_wR_factor_ref         0.3457
_reflns_number_gt                4175
_reflns_number_total             5324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b04277_si_009.cif
_cod_data_source_block           NPF-300-5
_cod_database_code               4132492
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15-C16 = C17-C18
 1.38 with sigma of 0.02
 C16-C17
 1.38 with sigma of 0.02
3. Rigid bond restraints
 C19, C18, C17, C16, C15, C14, O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C12, C10, C9, C11, C8, C5, C4, C3, C2, C7, C6, C1, O4, O006
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C24, C23, C22, C21, C20, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C19 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim O3: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C13 \\sim C12 \\sim C10 \\sim C9 \\sim C8 \\sim C11 \\sim C5 \\sim C4 \\sim C3
\\sim C2 \\sim C7 \\sim C6 \\sim C1 \\sim O4 \\sim O006: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim O5: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C7(H7), C3(H3), C6(H6), C4(H4), C16(H16), C11(H11),
 C9(H9), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'