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_1571095
_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-pH2
_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                   28.822(3)
_cell_length_b                   25.209(2)
_cell_length_c                   13.8069(13)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      26.160
_cell_measurement_theta_min      2.299
_cell_volume                     10031.7(16)
_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 0.998
_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  0.1338
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            82826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.374
_diffrn_reflns_theta_min         1.824
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0968 before and 0.0861 after correction.
The Ratio of minimum to maximum transmission is 0.7824.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.004
_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         0.603
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         10477
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6545
_reflns_number_total             10477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           ph2
_cod_original_cell_volume        10031.9(15)
_cod_database_code               1571095
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.920
_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
 O9-C25 = O8-C25 = O3-C17 = O4-C17
 1.25 with sigma of 0.01
 O10B-C26 = C26-O11B
 1.25 with sigma of 0.02
 O10A-C26A = C26A-O11A
 1.25 with sigma of 0.02
 O10B-O11B
 2.165 with sigma of 0.04
 O10A-O11A
 2.165 with sigma of 0.04
 Zr3-O10B \\sim Zr3-O10A
 with sigma of 0.02
 O11B-C26 \\sim O11A-C26A
 with sigma of 0.02
 Zr2-O11B \\sim Zr2-O11A
 with sigma of 0.02
 O10B-C26 \\sim O10A-C26A
 with sigma of 0.02
 Zr2-C26 \\sim Zr2-C26A
 with sigma of 0.04
 Zr3-C26 \\sim Zr3-C26A
 with sigma of 0.04
 O10B-O11B \\sim O10A-O11A
 with sigma of 0.04
3. Rigid bond restraints
 O10A, O10B, O11A, O11B, C26, C26A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. 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
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11: 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 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
: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O10A \\sim O11A \\sim C26A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O10B \\sim O11B \\sim C26: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
O10A \\sim O10B \\sim O11A \\sim O11B \\sim C26 \\sim C26A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O18B) = Uanis(O18A)
Uanis(O8) = Uanis(O4)
Uanis(O9) = Uanis(O3)
5. Others
 Fixed Sof: O3(0.5) O4(0.5) O7(0.5) H7(0.5) O8(0.5) O9(0.5) O10A(0.5)
 O10B(0.5) O11A(0.5) O11B(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) C26(0.5) H26(0.5)
 C26A(0.5) H26A(0.5)
6.a Riding coordinates:
 O7(H7)
6.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), C26A(H26A)
6.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              15932
_shelx_fab_checksum              55906
_olex2_submission_special_instructions 'No special instructions were received'