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_4135511
_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         'C66 H54 Br6 N6 O20 Pd3 Zr6, Br6 Pd2'
_chemical_formula_sum            'C66 H54 Br12 N6 O20 Pd5 Zr6'
_chemical_formula_weight         3289.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                76.234(2)
_cell_angle_beta                 79.8840(10)
_cell_angle_gamma                68.246(2)
_cell_formula_units_Z            2
_cell_length_a                   15.1229(3)
_cell_length_b                   20.0995(4)
_cell_length_c                   25.5356(4)
_cell_measurement_reflns_used    32283
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.2780
_cell_measurement_theta_min      2.7220
_cell_volume                     6969.0(2)
_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 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -30.00  29.00   0.50    0.85    --  -46.37  19.00   0.00  118
  2  \w    -30.00  29.00   0.50    0.85    --  -46.37  19.00-120.00  118
  3  \w    -51.00 -16.00   0.50    3.40    --  -88.50  45.00  30.00   70
  4  \w    -51.00 -16.00   0.50    3.40    --  -88.50  45.00 -30.00   70
  5  \w    -51.00 -16.00   0.50    3.40    --  -88.50  45.00   0.00   70
  6  \w    -51.00 -16.00   0.50    3.40    --  -88.50  45.00  60.00   70
  7  \w    -51.00 -16.00   0.50    3.40    --  -88.50  45.00 150.00   70
  8  \w    -85.00 -12.00   0.50    0.85    --  -46.37 124.00  39.00  146
  9  \w     83.00 118.00   0.50    0.85    --   46.37  57.00  30.00   70
 10  \w     96.00 178.00   0.50    3.40    --  106.69 124.00  39.00  164
 11  \w     89.00 178.00   0.50    3.40    --  106.69  15.00 -30.00  178
 12  \w     95.00 178.00   0.50    3.40    --  106.69 125.00-180.00  166
 13  \w     91.00 178.00   0.50    3.40    --  106.69  30.00 -30.00  174
 14  \w     92.00 178.00   0.50    3.40    --  106.69  45.00-150.00  172
 15  \w     92.00 178.00   0.50    3.40    --  106.69  45.00-180.00  172
 16  \w     80.00 168.00   0.50    3.40    --  106.69 147.00-155.00  176
 17  \w     34.00  71.00   0.50    3.40    --  106.69 -61.00-150.00   74
 18  \w     34.00  71.00   0.50    3.40    --  106.69 -61.00-180.00   74
 19  \w     34.00 111.00   0.50    3.40    --  106.69-125.00 -90.00  154
 20  \w     45.00 126.00   0.50    3.40    --  106.69-144.00  48.58  162
 21  \w     46.00 107.00   0.50    0.85    --   46.37-147.00 155.00  122
 22  \w     46.00 128.00   0.50    3.40    --  106.69-147.00 155.00  164
 23  \w     34.00  71.00   0.50    3.40    --  106.69 -61.00 150.00   74
 24  \w     34.00 109.00   0.50    3.40    --  106.69-117.00 170.41  150
 25  \w     34.00  71.00   0.50    3.40    --  106.69 -61.00 120.00   74
 26  \w   -102.00 -24.00   0.50    0.85    --  -46.37 147.00-155.00  156
 27  \w   -101.00 -24.00   0.50    3.40    --  -88.50 147.00-155.00  154
 28  \w    -51.00 -16.00   0.50    3.40    --  -88.50  45.00-180.00   70
 29  \w   -118.00 -83.00   0.50    0.85    --  -46.37 -57.00-120.00   70
 30  \w   -118.00 -83.00   0.50    0.85    --  -46.37 -57.00-150.00   70
 31  \w   -118.00 -32.00   0.50    0.85    --  -46.37 -49.00-102.78  172
 32  \w   -118.00 -87.00   0.50    0.85    --  -46.37-125.00   0.00   62
 33  \w   -118.00 -87.00   0.50    0.85    --  -46.37-125.00  90.00   62
 34  \w   -118.00 -58.00   0.50    0.85    --  -46.37-147.00 155.00  120
 35  \w   -118.00 -83.00   0.50    0.85    --  -46.37 -57.00  90.00   70
 36  \w   -118.00 -83.00   0.50    0.85    --  -46.37 -57.00 120.00   70
 37  \w   -151.00 -58.00   0.50    3.40    --  -88.50-147.00 155.00  186
 38  \w   -160.00 -74.00   0.50    3.40    --  -88.50-124.00 -40.00  172
 39  \w   -118.00 -87.00   0.50    0.85    --  -46.37-125.00-150.00   62
 40  \w   -118.00 -87.00   0.50    0.85    --  -46.37-125.00-180.00   62
 41  \w   -160.00 -91.00   0.50    3.40    --  -88.50 -61.00-120.00  138
 42  \w   -161.00 -74.00   0.50    3.40    --  -88.50 -45.00  20.59  174
 43  \w   -160.00-101.00   0.50    3.40    --  -88.50 -77.00 -30.00  118
 44  \w   -160.00-101.00   0.50    3.40    --  -88.50 -77.00 -90.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112417000
_diffrn_orient_matrix_UB_12      -0.0089664000
_diffrn_orient_matrix_UB_13      0.0621688000
_diffrn_orient_matrix_UB_21      0.1082820000
_diffrn_orient_matrix_UB_22      -0.0174373000
_diffrn_orient_matrix_UB_23      -0.0005608000
_diffrn_orient_matrix_UB_31      -0.0170999000
_diffrn_orient_matrix_UB_32      0.0817198000
_diffrn_orient_matrix_UB_33      -0.0054321000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            112667
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        64.994
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_min         2.717
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.986
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
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    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             3084
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.043
_refine_diff_density_max         3.068
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         23450
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0867
_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^)+(0.0100P)^2^+160.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19500
_reflns_number_total             23450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11881_si_005.cif
_cod_data_source_block           Pd-cage
_cod_depositor_comments
'Adding full bibliography for 4135507--4135511.cif.'
_cod_database_code               4135511
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pd C  H O N Zr Br Cl'
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15-C18
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C61) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C10(H10), C28(H28), C1(H1), C47(H47), C20(H20), C5(H5),
 C25(H25), C44(H44), C17(H17), C26(H26), C65(H65), C4(H4), C35(H35), C51(H51),
 C48(H48), C34(H34), C19(H19), C7(H7), C23(H23), C29(H29), C38(H38), C16(H16),
 C11(H11), C32(H32), C45(H45), C14(H14), C64(H64), C50(H50), C56(H56), C46(H46),
  C13(H13), C31(H31), C52(H52), C49(H49), C22(H22), C63(H63), C42(H42),
 C43(H43), C40(H40), C39(H39), C66(H66), C62(H62), C37(H37), C53(H53), C54(H54),
  C55(H55), C41(H41), C61(H61), C60(H60), C59(H59), C58(H58), C57(H57)
4.b Fitted pentagon refined as free rotating group:
 C61(C60,C59,C58,C57)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76060
_shelx_hkl_checksum              93873
_shelx_fab_checksum              91048
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.467
_oxdiff_exptl_absorpt_empirical_full_min 0.677