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_1571094
_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
_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   geom
_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                   28.6081(13)
_cell_length_b                   25.3758(13)
_cell_length_c                   13.7747(7)
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.066
_cell_measurement_theta_min      2.296
_cell_volume                     9999.8(9)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.1139
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43414
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         1.682
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0946 after correction.
The Ratio of minimum to maximum transmission is 0.7870.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.007
_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         0.891
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         11462
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0734
_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^)+(0.0848P)^2^+6.2726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.1972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6966
_reflns_number_total             11462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           a
_cod_database_code               1571094
_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
 O8-C25 = O9-C25
 1.25 with sigma of 0.01
 O4-C17 = O3-C17
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
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 C17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O7 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C18 \\sim C19: 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
O9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O18A) = Uanis(O18B)
4. Others
 Fixed Sof: O3(0.5) O4(0.5) O7(0.5) H7(0.5) O8(0.5) O9(0.5) O13B(0.5)
 O18A(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) O18B(0.5)
 O13A(0.5)
5.a 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)
5.b Fitted hexagon refined as free rotating group:
 C11(C6,C7,C8,C9,C10)
5.c Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12557
_shelx_fab_checksum              72351
_olex2_submission_special_instructions 'No special instructions were received'