Reticular chemistry guided precise construction of zirconium-pentacarboxylate frameworks with 5-connected Zr<sub>6</sub> clusters.
Peng, Tianyou; Han, Chao-Qin; Xia, Hai-Lun; Zhou, Kang; Zhang, Jian; Si, Jincheng; Wang, Lei; Miao, Jiafeng; Guo, Fu-An; Wang, Hao; Qu, Lu-Lu; Xu, Guozhong; Li, Jing; Liu, Xiao-Yuan; Chemical science 15 (2024) 3174–3181; doi:10.1039/d3sc05410a

data_1571091
_publ_section_title
;
 Reticular chemistry guided precise construction of
 zirconium-pentacarboxylate frameworks with 5-connected Zr<sub>6</sub>
 clusters.
;
_journal_issue                   9
_journal_name_full               'Chemical science'
_journal_page_first              3174
_journal_page_last               3181
_journal_paper_doi               10.1039/d3sc05410a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C33 H15 N2 O32 Zr6'
_chemical_formula_sum            'C33 H15 N2 O32 Zr6'
_chemical_formula_weight         1498.79
_chemical_name_systematic        HIAM-4040
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-26 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5866(8)
_cell_length_b                   25.3514(14)
_cell_length_c                   28.7868(15)
_cell_measurement_reflns_used    9024
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      59.92
_cell_measurement_theta_min      3.21
_cell_volume                     9915.3(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76214
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.319
_diffrn_reflns_theta_min         2.020
_diffrn_source_current           2.85
_diffrn_source_power             0.1986735
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.645
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1448 before and 0.0975 after correction.
The Ratio of minimum to maximum transmission is 0.7902.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_description       block
_exptl_crystal_F_000             2892
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.515(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         20916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0390P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                15820
_reflns_number_total             20916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           230223li_lidz213717_1_0m
_cod_database_code               1571091
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.485(10)
 0.515(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C17(H17), C18(H18), C20(H20),
 C21(H21), C24(H24), C26(H26), C28(H28), C31(H31), C32(H32), C33(H33)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              73132
_shelx_fab_checksum              14823
_olex2_submission_special_instructions 'No special instructions were received'