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_7717223
_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         'C145 H129 Co8 Mn6 Mo36 N12 O180'
_chemical_formula_sum            'C145 H129 Co8 Mn6 Mo36 N12 O180'
_chemical_formula_weight         9174.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-07
_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                 102.893(4)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.5098(16)
_cell_length_b                   44.611(3)
_cell_length_c                   26.993(2)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    153.00
_cell_measurement_theta_max      48.062
_cell_measurement_theta_min      2.259
_cell_volume                     21727(3)
_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      153.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            165304
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.379
_diffrn_reflns_theta_max         53.379
_diffrn_reflns_theta_min         1.696
_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    4.248
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.5475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0726 after correction.
The Ratio of minimum to maximum transmission is 0.7295.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.701
_exptl_crystal_description       block
_exptl_crystal_F_000             4401
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         38636
_refine_ls_number_restraints     948
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2495
_refine_ls_wR_factor_ref         0.2988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12148
_reflns_number_total             38636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02609h2.cif
_cod_data_source_block           Co-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_database_code               7717223
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C12-C5 = C21-C20 = C14-C15 = C13-C9
 1.5 with sigma of 0.02
 N1-C5 = N3-C30 = C21-N2
 1.4 with sigma of 0.02
 C34-C31 = C37-C30 = C37A-C30 = C34A-C31A_$2
 1.5 with sigma of 0.02
 C21-C20
 1.5 with sigma of 0.001
 Co2-O6 \\sim Co2-O5 \\sim Co2-O8
 with sigma of 0.02
 Co2-O7 \\sim Co2-O10 \\sim Co2-O9 \\sim Co1-O3 \\sim Co1-O2
 with sigma of 0.02
 C11-C5 \\sim C5-C7
 with sigma of 0.02
 C10-C13 \\sim C13-C8
 with sigma of 0.02
 O1-C13 \\sim O8_$1-C13
 with sigma of 0.02
 O1-C9 \\sim C9-O8_$1
 with sigma of 0.02
 O3-C31A \\sim C31A-O7
 with sigma of 0.02
 C36-C30 \\sim C30-C33
 with sigma of 0.02
 C35-C31 \\sim C31-C32 \\sim C32A-C31A_$2 \\sim C31A_$2-C35A
 with sigma of 0.02
 O7_$2-C31 \\sim C31-O2_$3 \\sim O7_$2-C31A_$2 \\sim C31A_$2-O3_$2
 with sigma of 0.02
 O7_$2-C34A \\sim C34A-O3_$2
 with sigma of 0.02
 O7_$2-C34 \\sim C34-O2_$3
 with sigma of 0.02
3. Restrained planarity
 C7, C12, C11, C5
 with sigma of 0.01
 O4, C14, O5, C15
 with sigma of 0.01
 O2_$3, C31, O7_$2, C34
 with sigma of 0.1
 O7_$2, C31A_$2, O3_$2, C34A
 with sigma of 0.1
 C31, C34, C35, C32
 with sigma of 0.1
 C34A, C35A, C32A, C31A_$2
 with sigma of 0.1
 C36, C37, C33, C36A, C30
 with sigma of 0.1
 C36A, C37A, C33A, C30
 with sigma of 0.1
4. 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
C33 \\sim C32 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C33A \\sim C32A
\\sim C34A \\sim C35A \\sim C36A \\sim C37A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O1 \\sim C13: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
O7 \\sim O3 \\sim C31A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(Co1) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O10) \\sim Ueq,
Uanis(O9) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5) \\sim
Ueq, Uanis(O4) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq,
Uanis(C31A) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C32A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35A) \\sim Ueq,
Uanis(C36A) \\sim Ueq, Uanis(C37A) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O4) \\sim Ueq, Uanis(Co1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(Co1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C31A) = Uanis(C31)
5. Others
 Sof(H30A)=Sof(C33A)=Sof(H33A)=Sof(C32A)=Sof(H32A)=Sof(C34A)=Sof(C35A)=
 Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=1-FVAR(1)
 Sof(C33)=Sof(H33)=Sof(C32)=Sof(H32)=Sof(C34)=Sof(C35)=Sof(H35)=Sof(C36)=
 Sof(H36)=Sof(C37)=Sof(H30)=FVAR(1)
 Fixed Sof: C5(0.25) H5(0.25) O3(0.5) O2(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C23(H23A,H23B), C29(H29A,H29B), C28(H28A,
 H28B), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C26(H26A,H26B)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C16(H16), C17(H17), C21(H21), C8(H8), C7(H7), C11(H11),
 C10(H10), C5(H5), C33(H33), C32(H32), C35(H35), C36(H36), C30(H30), C30(H30A),
 C33A(H33A), C32A(H32A), C35A(H35A), C36A(H36A)
6.c Fitted hexagon refined as free rotating group:
 C18(C20,C19,C16,C15,C17), C9(C8,C7,C12,C11,C10), C33(C32,C34,C35,C36,C37),
 C33A(C32A,C34A,C35A,C36A,C37A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74831
_shelx_hkl_checksum              7346
_shelx_fab_checksum              41082
_olex2_submission_special_instructions 'No special instructions were received'