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_4135507
_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         'C72 H48 N12 O50 Pb4 Zr9'
_chemical_formula_sum            'C72 H48 N12 O50 Pb4 Zr9'
_chemical_formula_weight         3530.96
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-24
_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            3
_cell_length_a                   18.2062(4)
_cell_length_b                   18.2062(4)
_cell_length_c                   50.5590(19)
_cell_measurement_reflns_used    8910
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.3480
_cell_measurement_theta_min      2.6400
_cell_volume                     14513.4(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -28.00  32.00   0.50    2.35    --   46.37 -10.00   7.00  120
  2  \w     32.00 120.00   0.50    2.35    --   46.37  37.00  60.00  176
  3  \w     83.00 118.00   0.50    2.35    --   46.37  57.00  90.00   70
  4  \w     83.00 118.00   0.50    2.35    --   46.37  57.00 120.00   70
  5  \w     34.00  71.00   0.50    9.40    --  106.69 -61.00 -30.00   74
  6  \w     34.00 105.00   0.50    9.40    --  106.69 -94.00 -60.00  142
  7  \w     34.00 111.00   0.50    9.40    --  106.69-125.00  79.00  154
  8  \w     34.00  71.00   0.50    9.40    --  106.69 -61.00 -60.00   74
  9  \w     34.00 101.00   0.50    9.40    --  106.69 -77.00 -90.00  134
 10  \w     34.00 105.00   0.50    9.40    --  106.69 -94.00-150.00  142
 11  \w     89.00 178.00   0.50    9.40    --  106.69  15.00-180.00  178
 12  \w     32.00 120.00   0.50    2.35    --   46.37  37.00 -30.00  176
 13  \w    -51.00 -16.00   0.50    9.40    --  -88.50  45.00  18.00   70
 14  \w    -51.00 -16.00   0.50    9.40    --  -88.50  45.00 150.00   70
 15  \w    -87.00 -15.00   0.50    9.40    --  -88.50 127.00-113.00  144
 16  \w   -118.00 -83.00   0.50    2.35    --  -46.37 -57.00-120.00   70
 17  \w   -118.00 -87.00   0.50    2.35    --  -46.37-125.00-150.00   62
 18  \w   -118.00 -87.00   0.50    2.35    --  -46.37-125.00-120.00   62
 19  \w   -118.00 -87.00   0.50    2.35    --  -46.37-125.00  30.00   62
 20  \w   -160.00-110.00   0.50    9.40    --  -88.50 -61.00  90.00  100
 21  \w   -160.00-101.00   0.50    9.40    --  -88.50 -77.00  30.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            35763
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.490
_diffrn_reflns_theta_max         67.490
_diffrn_reflns_theta_min         4.858
_exptl_absorpt_coefficient_mu    10.866
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       plate
_exptl_crystal_F_000             4956
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.052
_refine_diff_density_max         3.627
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.183
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.274(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         5792
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1733P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2263
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                4846
_reflns_number_total             5792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11881_si_002.cif
_cod_data_source_block           JMOF-2
_cod_depositor_comments
'Adding full bibliography for 4135507--4135511.cif.'
_cod_original_cell_volume        14513.3(8)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4135507
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.726(17)
 0.274(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 C2, C3, C4, C5, N1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10)
Uanis(O9) = Uanis(Pb1)
Uanis(O8) = Uanis(Zr2)
Uanis(C1) = Uanis(C3)
5. Others
 Fixed Sof: O10(0.5) O9(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,N1)
;
_shelx_res_checksum              7994
_shelx_hkl_checksum              98346
_shelx_fab_checksum              53009
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;