Highly Specific Coordination-Driven Self-Assembly of 2D Heterometallic Metal-Organic Frameworks with Unprecedented Johnson-type (<i>J</i><sub>51</sub>) Nonanuclear Zr-Oxocarboxylate Clusters.
Gong, Wei; Arman, Hadi; Chen, Zhijie; Xie, Yi; Son, Florencia A.; Cui, Hui; Chen, Xinfa; Shi, Yanshu; Liu, Yan; Chen, Banglin; Farha, Omar K.; Cui, Yong; Journal of the American Chemical Society 143 (2021) 657–663; doi:10.1021/jacs.0c11881

data_4135509
_publ_section_title
;
 Highly Specific Coordination-Driven Self-Assembly of 2D Heterometallic
 Metal-Organic Frameworks with Unprecedented Johnson-type
 (<i>J</i><sub>51</sub>) Nonanuclear Zr-Oxocarboxylate Clusters.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              657
_journal_page_last               663
_journal_paper_doi               10.1021/jacs.0c11881
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety
'C36 H24 I3 N6 O44 Pb1 Zr9, I3 Pb1, 1(I), 3(O)'
_chemical_formula_sum            'C36 H24 I7 N6 O47 Pb2 Zr9'
_chemical_formula_weight         3416.27
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-10-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.3642(7)
_cell_length_b                   18.3642(7)
_cell_length_c                   33.9939(15)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.79
_cell_volume                     9928.3(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57358
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        20.833
_diffrn_reflns_theta_max         20.833
_diffrn_reflns_theta_min         1.754
_exptl_absorpt_coefficient_mu    3.268
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4189
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            light-yellow
_exptl_crystal_colour_primary    light-yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3106
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 2797 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.204(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6864
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1326P)^2^+93.6454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2191
_refine_ls_wR_factor_ref         0.2239
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                6304
_reflns_number_total             6864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11881_si_001.cif
_cod_data_source_block           JMOF-1
_cod_depositor_comments
'Adding full bibliography for 4135507--4135511.cif.'
_cod_original_cell_volume        9928.3(9)
_cod_database_code               4135509
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.736
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C8
 1.5 with sigma of 0.02
 O4-C7
 1.27 with sigma of 0.02
 O5-C7
 1.27 with sigma of 0.02
3. Rigid bond restraints
 C7, C8, C9, C10, N1, C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C6, C5, N2, C4, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4, O5, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zr1, O6, O9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Zr3, O15, O14, Zr2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C7 \\sim O5 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C8 \\sim C9 \\sim C10 \\sim N1 \\sim C11 \\sim C12: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C2 \\sim C6 \\sim C5 \\sim N2 \\sim C4 \\sim C3: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(O15) = Uanis(O14)
Uanis(O6) = Uanis(O9)
Uanis(O11) = Uanis(O9)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C9(H9), C10(H10), C11(H11), C12(H12)
5.b Fitted hexagon refined as free rotating group:
 C2(C6,C5,N2,C4,C3), C8(C9,C10,N1,C11,C12)
;
_shelx_res_checksum              87624
_shelx_hkl_checksum              4695
_olex2_submission_special_instructions 'No special instructions were received'