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_4135508
_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         'C42 H42 Mo4 N2 O26 Zr6, 5(C6 H14 N2 O2)'
_chemical_formula_sum            'C72 H112 Mo4 N12 O36 Zr6'
_chemical_formula_weight         2652.81
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                88.9510(10)
_cell_angle_beta                 78.2580(10)
_cell_angle_gamma                87.9520(10)
_cell_formula_units_Z            1
_cell_length_a                   9.87790(10)
_cell_length_b                   12.4026(2)
_cell_length_c                   19.6503(4)
_cell_measurement_reflns_used    31564
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9640
_cell_measurement_theta_min      2.3270
_cell_volume                     2355.36(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 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 n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.965
_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   -119.00 -57.00   0.50    0.05    --  -46.75-148.00 152.00  124
  2  \w    -84.00 -11.00   0.50    0.05    --  -46.75 123.00  37.00  146
  3  \w   -102.00 -25.00   0.50    0.05    --  -46.75 148.00-158.00  154
  4  \w     33.00  95.00   0.50    0.05    --   46.75-123.00 -42.00  124
  5  \w     47.00 110.00   0.50    0.05    --   46.75-148.00 152.00  126
  6  \w   -150.00 -57.00   0.50    0.13    --  -88.50-148.00 152.00  186
  7  \w   -102.00 -25.00   0.50    0.13    --  -88.50 148.00-158.00  154
  8  \w   -160.00 -75.00   0.50    0.13    --  -88.50-123.00 -42.00  170
  9  \w    -84.00 -15.00   0.50    0.13    --  -88.50 123.00  37.00  138
 10  \w     79.00 167.00   0.50    0.13    --  106.69 148.00-158.00  176
 11  \w     47.00 128.00   0.50    0.13    --  106.69-148.00 152.00  162
 12  \w     34.00 110.00   0.50    0.13    --  106.69-123.00 -42.00  152
 13  \w     96.00 178.00   0.50    0.13    --  106.69 123.00  37.00  164
 14  \w   -119.00 -87.00   0.50    0.05    --  -46.75-125.00 150.00   64
 15  \w   -119.00 -83.00   0.50    0.05    --  -46.75 -57.00-180.00   72
 16  \w   -119.00 -83.00   0.50    0.05    --  -46.75 -57.00  90.00   72
 17  \w   -119.00 -83.00   0.50    0.05    --  -46.75 -57.00-150.00   72
 18  \w   -119.00 -87.00   0.50    0.05    --  -46.75-125.00-150.00   64
 19  \w   -119.00 -83.00   0.50    0.05    --  -46.75 -57.00-120.00   72
 20  \w    -30.00  29.00   0.50    0.05    --  -46.75  19.00 -30.00  118
 21  \w     83.00 119.00   0.50    0.05    --   46.75  57.00  90.00   72
 22  \w   -160.00-101.00   0.50    0.13    --  -88.50 -77.00 -30.00  118
 23  \w   -160.00 -91.00   0.50    0.13    --  -88.50 -61.00   0.00  138
 24  \w    -51.00 -16.00   0.50    0.13    --  -88.50  45.00 -90.00   70
 25  \w    -51.00 -16.00   0.50    0.13    --  -88.50  45.00 150.00   70
 26  \w   -160.00 -73.00   0.50    0.13    --  -88.50 -53.00  16.16  174
 27  \w   -160.00 -91.00   0.50    0.13    --  -88.50 -61.00  60.00  138
 28  \w     34.00 111.00   0.50    0.13    --  106.69-125.00   0.00  154
 29  \w     91.00 178.00   0.50    0.13    --  106.69  30.00-150.00  174
 30  \w     34.00  71.00   0.50    0.13    --  106.69 -61.00 120.00   74
 31  \w     92.00 178.00   0.50    0.13    --  106.69  45.00 120.00  172
 32  \w     34.00 111.00   0.50    0.13    --  106.69-125.00  60.00  154
 33  \w     34.00 111.00   0.50    0.13    --  106.69-125.00-150.00  154
 34  \w     95.00 178.00   0.50    0.13    --  106.69 125.00  60.00  166
 35  \w     34.00 105.00   0.50    0.13    --  106.69 -94.00 150.00  142
 36  \w     34.00 101.00   0.50    0.13    --  106.69 -77.00 -60.00  134
 37  \w     34.00 101.00   0.50    0.13    --  106.69 -77.00   0.00  134
 38  \w     42.00 122.00   0.50    0.13    --  106.69-139.00 -36.66  160
 39  \w     34.00 105.00   0.50    0.13    --  106.69 -94.00-180.00  142
 40  \w     34.00 106.00   0.50    0.13    --  106.69 -99.00-138.95  144
 41  \w     92.00 178.00   0.50    0.13    --  106.69  45.00  60.00  172
 42  \w     34.00  71.00   0.50    0.13    --  106.69 -61.00-150.00   74
 43  \w     34.00  71.00   0.50    0.13    --  106.69 -61.00-180.00   74
 44  \w   -119.00 -32.00   0.50    0.05    --  -46.75 -45.00-171.80  174
 45  \w   -119.00 -31.00   0.50    0.05    --  -46.75 -53.00 126.65  176
 46  \w   -119.00 -31.00   0.50    0.05    --  -46.75 -52.00 -20.91  176
 47  \w   -119.00 -30.00   0.50    0.05    --  -46.75 -54.00 -73.11  178
 48  \w   -119.00 -32.00   0.50    0.05    --  -46.75 -48.00-115.57  174
 49  \w   -119.00 -31.00   0.50    0.05    --  -46.75 -46.00  28.55  176
 50  \w     31.00 119.00   0.50    0.05    --   46.75  54.00 135.60  176
 51  \w     31.00 119.00   0.50    0.05    --   46.75  55.00-108.16  176
 52  \w     31.00 119.00   0.50    0.05    --   46.75  55.00  82.03  176
 53  \w   -160.00-120.00   0.50    0.13    --  -88.50 -51.00 -28.64   80
 54  \w   -160.00 -72.00   0.50    0.13    --  -88.50 -51.00-123.63  176
 55  \w   -160.00 -72.00   0.50    0.13    --  -88.50 -54.00 -72.60  176
 56  \w     92.00 178.00   0.50    0.13    --  106.69  45.00 150.00  172
;
_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      -0.0169090000
_diffrn_orient_matrix_UB_12      0.0011235000
_diffrn_orient_matrix_UB_13      0.0796721000
_diffrn_orient_matrix_UB_21      0.1057378000
_diffrn_orient_matrix_UB_22      -0.0951846000
_diffrn_orient_matrix_UB_23      -0.0038406000
_diffrn_orient_matrix_UB_31      0.1180481000
_diffrn_orient_matrix_UB_32      0.0799319000
_diffrn_orient_matrix_UB_33      -0.0070976000
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62537
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.778
_diffrn_reflns_theta_min         2.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.180
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_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    1.870
_exptl_crystal_description       plate
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         9602
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0500P)^2^+4.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9106
_reflns_number_total             9602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11881_si_004.cif
_cod_data_source_block           Mo-cage
_cod_depositor_comments
'Adding full bibliography for 4135507--4135511.cif.'
_cod_database_code               4135508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Zn Mo'
_chemical_oxdiff_usercomment     G-MeOH
_shelx_estimated_absorpt_t_max   0.544
_shelx_estimated_absorpt_t_min   0.275
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All C(H,H,H,H,H) groups
2. Restrained distances
 H12-O12
 0.82 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C3(H3), C14(H14), C7(H7A), C5(H5), C4(H4), C18(H18),
 C6(H6), C11(H11), C13(H13), C28(H28), C12(H12A), C16(H16), C21(H21), C17(H17),
 C10(H10), C15(H15), C9(H9), C8(H8), C22(H22), C34(H34), C31(H31), C25(H25)
3.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C24(H24A,
 H24B,H24C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C)
;
_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 2.298
_oxdiff_exptl_absorpt_empirical_full_min 0.586