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_4135510
_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
'C39 H44 Cl Co N5 O12 Zr3, 2(N O3), C3 H7 N O, C2 H6 O'
_chemical_formula_sum            'C44 H57 Cl Co N8 O20 Zr3'
_chemical_formula_weight         1386.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-24
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.7165(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.71033(8)
_cell_length_b                   19.70013(10)
_cell_length_c                   19.76725(11)
_cell_measurement_reflns_used    41664
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.2720
_cell_measurement_theta_min      3.1870
_cell_volume                     5943.40(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.969
_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    -83.00  -3.00   0.50    0.21    --  -46.87 112.00 106.00  160
  2  \w     25.00  89.00   0.50    0.21    --   46.87-112.00  13.00  128
  3  \w    -82.00 -15.00   0.50    0.85    --  -88.50 112.00 106.00  134
  4  \w   -160.00 -81.00   0.50    0.85    --  -88.50-112.00  13.00  158
  5  \w     34.00 108.00   0.50    0.85    --  106.69-112.00  13.00  148
  6  \w    103.00 178.00   0.50    0.85    --  106.69 112.00 106.00  150
  7  \w   -120.00 -87.00   0.50    0.21    --  -46.87-125.00 -90.00   66
  8  \w   -120.00 -83.00   0.50    0.21    --  -46.87 -57.00 -30.00   74
  9  \w   -120.00 -87.00   0.50    0.21    --  -46.87-125.00  60.00   66
 10  \w   -120.00 -83.00   0.50    0.21    --  -46.87 -57.00  90.00   74
 11  \w   -120.00 -87.00   0.50    0.21    --  -46.87-125.00-120.00   66
 12  \w   -120.00 -83.00   0.50    0.21    --  -46.87 -57.00   0.00   74
 13  \w     83.00 120.00   0.50    0.21    --   46.87  57.00-180.00   74
 14  \w   -164.00 -71.00   0.50    0.85    --  -88.50 -15.00  60.00  186
 15  \w    -51.00 -16.00   0.50    0.85    --  -88.50  45.00 -30.00   70
 16  \w    -51.00 -16.00   0.50    0.85    --  -88.50  45.00 -60.00   70
 17  \w    -51.00 -16.00   0.50    0.85    --  -88.50  45.00  90.00   70
 18  \w     34.00  71.00   0.50    0.85    --  106.69 -61.00  90.00   74
 19  \w     95.00 178.00   0.50    0.85    --  106.69 125.00-180.00  166
 20  \w     89.00 178.00   0.50    0.85    --  106.69  15.00-150.00  178
 21  \w     34.00  71.00   0.50    0.85    --  106.69 -61.00  30.00   74
 22  \w     34.00 105.00   0.50    0.85    --  106.69 -94.00  60.00  142
 23  \w    101.00 178.00   0.50    0.85    --  106.69  77.00  90.00  154
 24  \w     34.00  71.00   0.50    0.85    --  106.69 -61.00 -90.00   74
 25  \w     34.00 101.00   0.50    0.85    --  106.69 -77.00  60.00  134
 26  \w     34.00  71.00   0.50    0.85    --  106.69 -61.00-180.00   74
 27  \w     34.00  71.00   0.50    0.85    --  106.69 -61.00   0.00   74
 28  \w     34.00  71.00   0.50    0.85    --  106.69 -61.00 150.00   74
 29  \w   -121.00 -32.00   0.50    0.21    --  -46.87 -37.00-150.00  178
 30  \w   -121.00 -92.00   0.50    0.21    --  -46.87 -37.00   0.00   58
 31  \w   -121.00 -32.00   0.50    0.21    --  -46.87 -37.00 120.00  178
;
_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      0.0850852000
_diffrn_orient_matrix_UB_12      -0.0380766000
_diffrn_orient_matrix_UB_13      -0.0017291000
_diffrn_orient_matrix_UB_21      -0.0522648000
_diffrn_orient_matrix_UB_22      -0.0665803000
_diffrn_orient_matrix_UB_23      -0.0170011000
_diffrn_orient_matrix_UB_31      -0.0151067000
_diffrn_orient_matrix_UB_32      0.0152070000
_diffrn_orient_matrix_UB_33      -0.0783597000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69187
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.540
_diffrn_reflns_theta_min         3.214
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.403
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.760
_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 light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             2804
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         12099
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+44.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11538
_reflns_number_total             12099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11881_si_003.cif
_cod_data_source_block           Co-MOF
_cod_depositor_comments
'Adding full bibliography for 4135507--4135511.cif.'
_cod_database_code               4135510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Zr Co Cl'
_chemical_oxdiff_usercomment     G-1062
_shelx_estimated_absorpt_t_max   0.622
_shelx_estimated_absorpt_t_min   0.422
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9
 0.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O16B) = Uanis(O17B) = Uanis(O17A) = Uanis(O16A) = Uanis(O15)
Uanis(C23) = Uanis(N5) = Uanis(C24B) = Uanis(C24A) = Uanis(C22)
4. Others
 Fixed Sof: H13B(0.75) H13A(0.25) O17A(0.65) O16A(0.65) C43B(0.75) H43A(0.75)
 H43B(0.75) C44B(0.75) H44A(0.75) H44B(0.75) H44C(0.75) C44A(0.25) H44D(0.25)
 H44E(0.25) H44F(0.25) C43A(0.25) H43C(0.25) H43D(0.25) O17B(0.35) O16B(0.35)
 C24B(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C24A(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C43B(H43A,H43B), C43A(H43C,H43D)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C8(H8), C16(H16), C14(H14), C17(H17), C13(H13), C39(H39), C1(H1),
 C36(H36), C37(H37), C35(H35), C27(H27), C38(H38), C2(H2), C7(H7), C33(H33),
 C19(H19), C25(H25), C4(H4), C32(H32), C10(H10A), C29(H29), C31(H31), C5(H5),
 C28(H28), C11(H11), C34(H34), C30(H30), C22(H22), C40(H40)
5.c Tetrahedral OH refined with riding coordinates:
 O13(H13B), O13(H13A)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C42(H42A,H42B,H42C), C41(H41A,H41B,
 H41C), C23(H23A,H23B,H23C), C44B(H44A,H44B,H44C), C44A(H44D,H44E,H44F),
 C24B(H24A,H24B,H24C), C24A(H24D,H24E,H24F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96037
_shelx_hkl_checksum              8974
_shelx_fab_checksum              64180
_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 1.645
_oxdiff_exptl_absorpt_empirical_full_min 0.779