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_1571092
_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 H20 N2 O27 Zr6'
_chemical_formula_sum            'C33 H20 N2 O27 Zr6'
_chemical_formula_weight         1423.83
_chemical_name_systematic        HIAM-4040-OH-EtOH
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-23 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                   25.437(2)
_cell_length_b                   28.850(2)
_cell_length_c                   12.9217(11)
_cell_measurement_reflns_used    5402
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      24.806
_cell_measurement_theta_min      2.263
_cell_volume                     9482.7(13)
_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 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1322
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         1.768
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0834 after correction.
The Ratio of minimum to maximum transmission is 0.6635.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.997
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5072
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.1030
_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^)+(0.1909P)^2^+40.1696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.3269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3125
_reflns_number_total             5072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           etoh
_cod_original_cell_volume        9482.6(13)
_cod_database_code               1571092
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.917
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C13-C16
 1.5 with sigma of 0.01
 O5-C11
 1.4 with sigma of 0.01
 O3-C16 = O4-C16
 1.25 with sigma of 0.01
 O9-C17 = O8-C17
 1.25 with sigma of 0.01
 O12-C18 = O13-C18
 1.25 with sigma of 0.01
 N1-C7 = N2-C8
 1.45 with sigma of 0.01
 O8-O9
 2.2 with sigma of 0.01
 O12-O12_$1
 2.2 with sigma of 0.01
 O12-O13
 2.2 with sigma of 0.01
 Zr1-O6A \\sim Zr1-O6
 with sigma of 0.02
 Zr2-O6A \\sim Zr2-O6
 with sigma of 0.02
3. Restrained planarity
 O3, O4, C13, C16
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O5 \\sim N1 \\sim N2 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12
\\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O6 \\sim O6A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O8 \\sim O9 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O3 \\sim O4 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O12 \\sim O13 \\sim C18: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(O11) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(O12) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O3(0.25) O4(0.25) O5(0.25) H5(0.25) O6(0.25) O6A(0.25) O8(0.25)
 O9(0.25) O11(0.5) O12(0.5) O13(0.5) N1(0.25) N2(0.25) H2(0.25) C7(0.5)
 H7(0.75) C8(0.5) H8(0.75) C9(0.25) C10(0.25) C11(0.25) C12(0.25) H12(0.25)
 C13(0.25) C14(0.25) H14(0.25) C15(0.25) H15(0.25) C16(0.25) C17(0.25)
 H17(0.25) C18(0.5) H18(0.5)
6.a Riding coordinates:
 O5(H5), C7(H7), C8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18)
6.c Fitted hexagon refined as free rotating group:
 C10(C11,C12,C13,C14,C15)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75742
_shelx_fab_checksum              72418
_olex2_submission_special_instructions 'No special instructions were received'