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_1571093
_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 H16 N2 O33 Zr6'
_chemical_formula_sum            'C33 H16 N2 O33 Zr6'
_chemical_formula_weight         1515.80
_chemical_name_systematic        HIAM-4040-OH-323K
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n 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                   28.527(6)
_cell_length_b                   25.427(4)
_cell_length_c                   13.449(3)
_cell_measurement_reflns_used    5480
_cell_measurement_temperature    323
_cell_measurement_theta_max      67.815
_cell_measurement_theta_min      3.553
_cell_volume                     9755(3)
_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      323.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52670
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.667
_diffrn_reflns_theta_min         3.553
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.542
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1414 before and 0.0800 after correction.
The Ratio of minimum to maximum transmission is 0.6286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.032
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9188
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0694
_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^)+(0.1333P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1860
_refine_ls_wR_factor_ref         0.2078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5530
_reflns_number_total             9188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           323k
_cod_original_cell_volume        9756(3)
_cod_database_code               1571093
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.607
_shelx_estimated_absorpt_t_min   0.533
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O9-C25 = O8-C25 = O3-C17 = O4-C17
 1.25 with sigma of 0.01
 O6A-C24 \\sim O6B-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O8 \\sim O9 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O3 \\sim O4 \\sim O7 \\sim N1 \\sim N2 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O10B) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O10B) = Uanis(O10A)
Uanis(O18B) = Uanis(O18A)
Uanis(O6A) = Uanis(O6B)
4. Others
 Fixed Sof: O3(0.5) O4(0.5) O6A(0.5) O6B(0.5) O7(0.5) H7(0.5) O8(0.5) O9(0.5)
 O10A(0.5) O10B(0.5) O13A(0.5) O13B(0.5) O18A(0.5) O18B(0.5) N1(0.5) N2(0.5)
 H2(0.5) C11(0.5) C6(0.5) C7(0.5) H7A(0.5) C8(0.5) H8(0.5) C9(0.5) C10(0.5)
 C12(0.5) C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5) C17(0.5)
 C18(0.5) H18(0.5) C19(0.5) C25(0.5) H25(0.5) H26(0.5) H26A(0.5)
5.a Riding coordinates:
 O7(H7)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C7(H7A), C8(H8), C14(H14), C15(H15), C18(H18),
 C21(H21), C23(H23), C25(H25), C26(H26), C26(H26A)
5.c Fitted hexagon refined as free rotating group:
 C11(C6,C7,C8,C9,C10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69387
_shelx_fab_checksum              93044
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'