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_4132485
_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         'C117 H62 O32 Zr6'
_chemical_formula_sum            'C117 H62 O32 Zr6'
_chemical_formula_weight         2526.99
_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   mixed
_audit_creation_date             2017-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.2664(8)
_cell_length_b                   32.9221(12)
_cell_length_c                   41.4807(13)
_cell_measurement_reflns_used    9283
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      15.29
_cell_measurement_theta_min      2.23
_cell_volume                     31773.3(19)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1278
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            411608
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.602
_diffrn_reflns_theta_min         0.623
_diffrn_source                   synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1941 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.8822.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    0.528
_exptl_crystal_description       block
_exptl_crystal_F_000             26510
_refine_diff_density_max         3.447
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       0.0067(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         18695
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0906
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1738P)^2^+121.1084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2848
_refine_ls_wR_factor_ref         0.3042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13570
_reflns_number_total             18695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04277_si_006.cif
_cod_data_source_block           NPF-300-2
_cod_database_code               4132485
_shelx_shelxl_version_number     2014/7
_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
 C9-C10
 1.508 with sigma of 0.02
 C9-C8
 1.38 with sigma of 0.02
 C13-C12 = C14-C13 = C14-C15
 1.38 with sigma of 0.02
 C8-C10
 2.52 with sigma of 0.01
3. Restrained planarity
 C5, C9, C8, C10
 with sigma of 0.1
4. Rigid bond restraints
 O2, O1, C1, C2, C3, C5, C4, C9, C7, C6, C8, C10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C11, C12, C15, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O2 \\sim O1 \\sim C1 \\sim C2 \\sim C3 \\sim C5 \\sim C4 \\sim C9 \\sim C7
\\sim C6 \\sim C8 \\sim C10: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O3 \\sim C11 \\sim C12 \\sim C15 \\sim C13 \\sim C14: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
6. Others
 Fixed Sof: C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
7.a Riding coordinates:
 C10(H10A,H10B,H10C)
7.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C18(H18), C19(H19), C33(H33), C31(H31), C21(H21), C34(H34),
 C30(H30), C26(H26), C3(H3), C28(H28), C4(H4), C13(H13), C7(H7), C14(H14),
 C24(H24), C6(H6)
;
_shelx_res_checksum              17647
_shelx_hkl_checksum              87517
_olex2_submission_special_instructions 'No special instructions were received'