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_4132495
_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         'C63 H34 O16 Zr3'
_chemical_formula_sum            'C63 H34 O16 Zr3'
_chemical_formula_weight         1320.56
_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             2017-07-26
_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                   23.2646(12)
_cell_length_b                   32.3320(16)
_cell_length_c                   21.5466(10)
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.842
_cell_measurement_theta_min      4.395
_cell_volume                     16207.2(14)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41325
_diffrn_reflns_av_R_equivalents  0.1169
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            141251
_diffrn_reflns_theta_full        13.45
_diffrn_reflns_theta_max         13.45
_diffrn_reflns_theta_min         0.63
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.291
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13530
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.567
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.0123(12)
_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   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         6363
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1653P)^2^+67.7446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.2640
_reflns_number_gt                5471
_reflns_number_total             6363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8b04277_si_008.cif
_cod_data_source_block           NPF-300-4
_cod_database_code               4132495
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27-C26
 1.46 with sigma of 0.02
 C22-C21 = C23-C22 = C24-C23 = C26-C25
 1.38 with sigma of 0.02
 C16-C15 = C17-C16 = C18-C17
 1.38 with sigma of 0.02
3. Restrained planarity
 C24, C25, C26, C27
 with sigma of 0.1
4. Rigid bond restraints
 C26, C25, C24, C23, C22, C21, C20, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C14, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, C20, C21, C22, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C26 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim O4:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O3 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C27 \\sim C26 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim
O4: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
6. Others
 Fixed Sof: C27(0.25) H27A(0.25) H27B(0.25) H27C(0.25)
7.a Riding coordinates:
 C27(H27A,H27B,H27C)
7.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C6(H6), C22(H22), C9(H9), C4(H4), C16(H16), C10(H10),
 C23(H23), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'