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_7717221
_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 Fe2 Mn1.5 Mo9 N3 O43'
_chemical_formula_sum            'C36 H33 Fe2 Mn1.5 Mo9 N3 O43'
_chemical_formula_weight         2253.22
_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
_audit_creation_date             2024-07-21
_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                   45.266(18)
_cell_length_b                   45.266(18)
_cell_length_c                   18.250(7)
_cell_measurement_reflns_used    5666
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      21.624
_cell_measurement_theta_min      2.180
_cell_volume                     32385(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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)'
_diffrn_ambient_temperature      173.00
_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 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  0.1548
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57376
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.498
_diffrn_reflns_theta_max         22.498
_diffrn_reflns_theta_min         1.770
_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    0.749
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0648 after correction.
The Ratio of minimum to maximum transmission is 0.7105.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.693
_exptl_crystal_description       block
_exptl_crystal_F_000             6489
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4934
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1849
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1829P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2849
_refine_ls_wR_factor_ref         0.3151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1517
_reflns_number_total             4934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02609h2.cif
_cod_data_source_block           Fe-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        32385(28)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'C36 H33 Fe2 Mn1.50 Mo9 N3 O43'
_cod_database_code               7717221
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Restrained distances
 C4-C5
 1.5 with sigma of 0.02
 C8-C11
 1.5 with sigma of 0.02
 O2-O3
 2.4 with sigma of 0.04
 C6-C4 \\sim C4-C10
 with sigma of 0.02
 C9-C11 \\sim C11-C7
 with sigma of 0.02
 O2-C11 \\sim C11-O3
 with sigma of 0.02
 O3-C8 \\sim C8-O2
 with sigma of 0.02
2. Restrained planarity
 C8, C11, O2, O3
 with sigma of 0.1
 C7, C9, C8, C11
 with sigma of 0.1
 C6, C5, C10, C4
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C10 \\sim C9 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C4 \\sim C11: within 2A
with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
O5 \\sim C1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(O5) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) Fe2(0.16665) O2(0.5) C11(0.5) C7(0.5) H7(0.5)
 C6(0.5) H6(0.5) C5(0.25) C10(0.5) H10(0.5) C9(0.5) H9(0.5) C8(0.5) C4(0.5)
 H4(0.5) O1(0.16665)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C10(H10), C9(H9), C4(H4)
5.c Fitted hexagon refined as free rotating group:
 C7(C6,C5,C10,C9,C8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51338
_shelx_hkl_checksum              54455
_shelx_fab_checksum              95860
_olex2_submission_special_instructions 'No special instructions were received'