A Porous Anderson-Type Polyoxometalate-based Metal-Organic Framework as Multifunctional Platform for Selective Oxidative Coupling with Amines
Tan, Hong-Ru; Zhou, Xiang; You, Hanqi; Zheng, Qi; Zhao, Sheng-yin; Xuan, Weimin; Dalton Transactions  (2023) –; doi:10.1039/D3DT02620E

data_7714309
_publ_section_title
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 A Porous Anderson-Type Polyoxometalate-based Metal-Organic Framework as
 Multifunctional Platform for Selective Oxidative Coupling with Amines
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02620E
_journal_year                    2023
_chemical_formula_moiety
'C5 H8 Cr0.5 Mo3 O13, C5 H9 Cr0.5 Mo3 O13, C52 H44 N4 O10 Y, 13[H2O]'
_chemical_formula_sum            'C62 H87 Cr Mo6 N4 O49 Y'
_chemical_formula_weight         2388.90
_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
_audit_creation_date             2023-07-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-31 deposited with the CCDC.	2023-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                104.555(7)
_cell_angle_beta                 104.167(7)
_cell_angle_gamma                90.510(6)
_cell_formula_units_Z            2
_cell_length_a                   13.262(2)
_cell_length_b                   13.818(3)
_cell_length_c                   24.319(4)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.309
_cell_measurement_theta_min      2.288
_cell_volume                     4170.6(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1096
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            78679
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.355
_diffrn_reflns_theta_min         1.961
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1774 before and 0.0815 after correction.
The Ratio of minimum to maximum transmission is 0.7877.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       plate
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.980
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         15210
_refine_ls_number_restraints     1638
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0640P)^2^+9.9903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10738
_reflns_number_total             15210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02620e2.cif
_cod_data_source_block           mo_shy1146_0m_a_sq
_cod_original_cell_volume        4170.5(13)
_cod_database_code               7714309
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H10A)=Sof(O26')=Sof(H26')=1-FVAR(1)
 Sof(H10)=Sof(O26)=Sof(H26A)=FVAR(1)
5.a Rotating group:
 O31(H31A,H31B), O32(H32A,H32B)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C44(H44A,H44B), C55(H55A,H55B), C18(H18A,H18B), C5(H5A,H5B),
 C8(H8A,H8B), C6(H6A,H6B), C3(H3A,H3B), C2(H2A,H2B), C7(H7A,H7B), C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C31(H31), C32(H32), C19(H19), C48(H48), C53(H53), C22(H22),
 C45(H45), C51(H51), C17(H17), C16(H16), C42(H42), C54(H54), C40(H40), C52(H52),
  C35(H35), C28(H28), C43(H43), C20(H20), C26(H26), C49(H49), C58(H58),
 C46(H46), C39(H39), C57(H57), C34(H34), C23(H23), C27(H27), C61(H61), C60(H60),
  C14(H14), C13(H13), C10(H10), C10(H10A)
5.d Idealised tetrahedral OH refined as rotating group:
 O25(H25A), O26(H26A), O26'(H26')
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61871
_shelx_fab_checksum              63711
_olex2_submission_special_instructions 'No special instructions were received'