Imine bond-directed assembly of polyoxometalate-based metal-organic frameworks.
Yu, Xiang; Xu, Xinyu; Gao, Lei; Luo, Rengan; Liu, Yi-Fan; Gu, Yu-Hao; Yuan, Shuai; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17902–17908; doi:10.1039/d4dt02609h

data_7717222
_publ_section_title
;
 Imine bond-directed assembly of polyoxometalate-based metal-organic
 frameworks.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17902
_journal_page_last               17908
_journal_paper_doi               10.1039/d4dt02609h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H33 Mn1.5 Mo9 N3 O43 Zn2'
_chemical_formula_sum            'C36 H33 Mn1.5 Mo9 N3 O43 Zn2'
_chemical_formula_weight         2272.26
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-09-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-03 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   45.047(2)
_cell_length_b                   45.047
_cell_length_c                   18.7659(10)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      24.852
_cell_measurement_theta_min      2.232
_cell_volume                     32979(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo_Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84385
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.057
_diffrn_reflns_theta_max         25.057
_diffrn_reflns_theta_min         1.756
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms DIAMOND'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.8666.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.686
_exptl_crystal_description       block
_exptl_crystal_F_000             6537
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         6767
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1797P)^2^+70.8178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2815
_refine_ls_wR_factor_ref         0.3582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2840
_reflns_number_total             6767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02609h2.cif
_cod_data_source_block           Zn-POMOF
_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 

 Adding full bibliography for 7717220--7717223.cif.
;
_cod_original_cell_volume        32979(4)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'C36 H33 Mn1.50 Mo9 N3 O43 Zn2'
_cod_database_code               7717222
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Restrained distances
 C8-C11
 1.5 with sigma of 0.02
 C5-C4
 1.5 with sigma of 0.02
 C9-C11 \\sim C11-C7
 with sigma of 0.02
 C10-C4 \\sim C4-C6
 with sigma of 0.02
 O2-C11 \\sim C11-O3
 with sigma of 0.02
 C9-C10 \\sim C5-C6 \\sim C7-C8
 with sigma of 0.02
2. Restrained planarity
 O2, O3, C8, C11
 with sigma of 0.1
 C6, C5, C10, C4
 with sigma of 0.01
 C9, C8, C7, C11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C3 \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C9 \\sim C10 \\sim C6 \\sim C7 \\sim C8 \\sim C5 \\sim C11 \\sim C4: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C9, C8, C7, C6, C5, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Zn2(0.16665) H3A(0.5) H3B(0.5) O3(0.5) O1(0.16665) C9(0.5) H9(0.5)
 C10(0.25) H10(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) C4(0.5)
 H4(0.5) C11(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C6(H6), C7(H7), C4(H4)
6.c Fitted hexagon refined as free rotating group:
 C9(C10,C5,C6,C7,C8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99776
_shelx_hkl_checksum              44354
_shelx_fab_checksum              56924
_olex2_submission_special_instructions 'No special instructions were received'