Carboxyl Position Directed Structure Diversity in Zirconium-Tricarboxylate Frameworks
Xia, Jun; Si, Jincheng; Zhou, Kang; Xia, Hai-Lun; Zhang, Jian; Xu, Yingqian; Wang, Lei; Liu, Xiao-Yuan; Dalton Transactions  (2023) –; doi:10.1039/D3DT03348A

data_7714460
_publ_section_title
;
 Carboxyl Position Directed Structure Diversity in
 Zirconium-Tricarboxylate Frameworks
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03348A
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C79 H50 N6 O32 S3 Zr6'
_chemical_formula_sum            'C79 H50 N6 O32 S3 Zr6'
_chemical_formula_weight         2238.75
_chemical_name_systematic        HIAM-4033
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-11 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.3248(9)
_cell_length_b                   23.3248(9)
_cell_length_c                   32.710(2)
_cell_measurement_reflns_used    9119
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      56.76
_cell_measurement_theta_min      2.24
_cell_volume                     15411.6(13)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            116666
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.980
_diffrn_reflns_theta_max         52.980
_diffrn_reflns_theta_min         1.903
_diffrn_source                   MetalJet
_diffrn_source_current           2.23
_diffrn_source_power             0.1554533
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0840 after correction.
The Ratio of minimum to maximum transmission is 0.6338.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.724
_exptl_crystal_description       block
_exptl_crystal_F_000             3330
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.338
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         18131
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1251P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                12604
_reflns_number_total             18131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03348a2.cif
_cod_data_source_block           221114lu_lgpz119885_2_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        15411.6(15)
_cod_database_code               7714460
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(2)
 0.47(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 C30-C31 = C29-C28
 1.35 with sigma of 0.005
 O7-C27 = O8-C27
 1.25 with sigma of 0.005
 O12-C47 = O13-C47
 1.25 with sigma of 0.005
 O10-C39 = O9-C39
 1.25 with sigma of 0.005
 C30-C29
 1.4 with sigma of 0.005
 O4-C26 = O3-C26
 1.25 with sigma of 0.005
 O6-C20 = O5-C20
 1.25 with sigma of 0.005
 C41-C40 = C40-C33
 1.39 with sigma of 0.005
 C32-C40
 2.15 with sigma of 0.005
 C32-C33
 2.15 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
C27 \\sim C47: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
O10 \\sim O9 \\sim C39: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
O8 \\sim O13: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O12) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C47) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: S2(0.5) O9(0.5) O12(0.5) O13(0.5) N4(0.5) H4(0.5) N3(0.5) C47(0.5)
 H47(0.5) C29(0.5) H29(0.5) H33(0.5) H40(0.5) C32(0.5) C30(0.5) H30(0.5)
 C28(0.5) C31(0.5) O7(0.5) C27(0.5) O8(0.5) O10(0.5)
6.a Riding coordinates:
 O18(H18A,H18B), O19(H19A,H19B), N2(H2), C3(H3), C44(H44), C43(H43), C4(H4A),
 C23(H23)
6.b Ternary CH refined with riding coordinates:
 O17(H17)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C47(H47), C18(H18), C19(H19), C15(H15), C16(H16), C7(H7), C6(H6),
 C29(H29), C37(H37), C36(H36), C33(H33), C40(H40), C9(H9), C10(H10), C24(H24),
 C30(H30)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1752
_shelx_fab_checksum              64972
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU