A Zr-hydroxamate metal-organic framework with intrinsic chelating sites for postsynthetic Pd metalation and Suzuki-Miyaura catalysis.
Shao, Zhen-Wu; Xiong, Chaozhi; Yang, Jiajie; Mei, Zhewei; Xiong, Li; Wu, Wenjing; Liu, Chong; Chemical communications (Cambridge, England) 60 (2024) 11100–11103; doi:10.1039/d4cc03895a

data_7133707
_publ_section_title
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 A Zr-hydroxamate metal-organic framework with intrinsic chelating sites
 for postsynthetic Pd metalation and Suzuki-Miyaura catalysis.
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_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11100
_journal_page_last               11103
_journal_paper_doi               10.1039/d4cc03895a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C12 H8 N8 O8 Zr, 7[C3H7NO]'
_chemical_formula_sum            'C33 H57 N15 O15 Zr'
_chemical_formula_weight         995.136
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_symmetry_Int_Tables_number      192
_audit_creation_date             2024-08-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
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_audit_update_record
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2024-08-30 deposited with the CCDC.	2024-09-09 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.8945(4)
_cell_length_b                   22.8945(4)
_cell_length_c                   16.5284(5)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      60.37
_cell_measurement_theta_min      3.36
_cell_volume                     7502.8(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.9899
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.9958
_diffrn_reflns_Laue_measured_fraction_max 0.9899
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55736
_diffrn_reflns_point_group_measured_fraction_full 0.9958
_diffrn_reflns_point_group_measured_fraction_max 0.9899
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         60.38
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1343 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.8819.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             3126.372
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.6047
_refine_diff_density_min         -0.7097
_refine_diff_density_rms         0.0873
_refine_ls_d_res_high            0.7715
_refine_ls_d_res_low             19.8272
_refine_ls_goodness_of_fit_ref   1.0037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    4
_refine_ls_number_parameters     67
_refine_ls_number_reflns         2947
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.9996
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+2.3173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              25
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2166
_reflns_number_total             2947
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc03895a2.cif
_cod_data_source_block           SUM-1-pz
_cod_depositor_comments          'Adding full bibliography for 7133707.cif.'
_cod_original_formula_sum        'C33 H57 N15 O15 Zr1'
_cod_database_code               7133707
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
N2 \\sim C2 \\sim C3: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
Uanis(C3) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3)
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_smtbx_masks_special_details
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A solvent mask was calculated and 1662 electrons were 
found in a volume of 5578\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 7[C3H7NO] per Formula Unit 
which account for 1680 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'