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_7717220
_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
'C12 H11.5 Mn0.5 Mo3 N O14, C12 H10.5 Mn0.5 Mo3 N O14, C16 H35 N, 2(C2 H6 O S), 3(C16 H36 N), 1.4[C2H6SO], 0.1[C2H6SO]'
_chemical_formula_sum            'C95 H186 Mn Mo6 N6 O31.5 S3.5'
_chemical_formula_weight         2659.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90.450(4)
_cell_angle_beta                 106.263(4)
_cell_angle_gamma                95.652(4)
_cell_formula_units_Z            2
_cell_length_a                   16.5890(17)
_cell_length_b                   17.1075(18)
_cell_length_c                   22.616(2)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      60.14
_cell_measurement_theta_min      4.13
_cell_volume                     6127.3(11)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62217
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        52.982
_diffrn_reflns_theta_max         52.982
_diffrn_reflns_theta_min         1.772
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.588
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1197 before and 0.0846 after correction.
The Ratio of minimum to maximum transmission is 0.7517.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             2766
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.148
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         21332
_refine_ls_number_restraints     864
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0833
_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^)+(0.0414P)^2^+123.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2149
_refine_ls_wR_factor_ref         0.2173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19230
_reflns_number_total             21332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02609h2.cif
_cod_data_source_block           POM-COOH
_cod_depositor_comments
'Adding full bibliography for 7717220--7717223.cif.'
_cod_original_cell_volume        6127.2(11)
_cod_original_formula_sum        'C95 H186 Mn Mo6 N6 O31.50 S3.50'
_cod_database_code               7717220
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.418
_olex2_refinement_description
;
1. Restrained distances
 C36-C35 = C35-C34 = C34-C33 = C30-C29 = C31-C30 = C32-C31 = C38-C37 = C39-C38
 = C40-C39 = C26-C25 = C28-C27 = C27-C26
 1.53 with sigma of 0.01
 C88-C87 = C87-C86 = C86-C85 = C78-C77 = C79-C78 = C80-C79 = C82-C81 = C83-C82
 = C84-C83 = C75-C74 = C74-C73 = C76-C75
 1.53 with sigma of 0.01
 C62-C61 = C63-C62 = C64-C63 = C70-C69 = C71-C70 = C72A-C71 = C58-C57 = C59-
 C58 = C60-C59 = C66-C65 = C67-C66 = C68-C67
 1.53 with sigma of 0.01
 C46-C45 = C47-C46 = C48-C47 = C42-C41 = C43-C42 = C44-C43 = C54-C53 = C55-C54
 = C56-C55 = C50-C49 = C51-C50 = C52-C51
 1.53 with sigma of 0.01
2. 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
3. Others
 Sof(H71A)=Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=1-FVAR(1)
 Sof(H71)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=FVAR(1)
 Sof(H91D)=Sof(H91E)=Sof(H91F)=Sof(H92D)=Sof(H92E)=Sof(H92F)=Sof(S2A)=1-FVAR(2)
 Sof(H91A)=Sof(H91B)=Sof(H91C)=Sof(H92A)=Sof(H92B)=Sof(H92C)=Sof(S2)=FVAR(2)
 Fixed Sof: H1(0.5) H15A(0.5)
4.a Riding coordinates:
 C91(H91A,H91B,H91C), C91(H91D,H91E,H91F), C92(H92A,H92B,H92C), C92(H92D,H92E,
 H92F)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C11(H11A,H11B), C12(H12A,
 H12B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C61(H61A,H61B),
 C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B),
  C69(H69A,H69B), C70(H70A,H70B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C73(H73A,H73B), C74(H74A,H74B),
  C75(H75A,H75B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C85(H85A,H85B), C86(H86A,H86B),
 C87(H87A,H87B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C3(H3), C4(H4), C6(H6),
 C7(H7), C8(H8), C10(H10), C71(H71), C71(H71A)
4.d Tetrahedral OH refined with riding coordinates:
 O1(H1), O15(H15A)
4.e Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C72(H72A,H72B,
 H72C), C72A(H72D,H72E,H72F), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C),
 C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C56(H56A,
 H56B,H56C), C76(H76A,H76B,H76C), C80(H80A,H80B,H80C), C84(H84A,H84B,H84C),
 C88(H88A,H88B,H88C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 120 electrons were 
found in a volume of 484\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1.4[C2H6SO], 0.1[C2H6SO] per formula unit 
which account for 126 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27341
_shelx_hkl_checksum              92498
_shelx_fab_checksum              99878
_olex2_submission_special_instructions 'No special instructions were received'