A multicentre synergistic polyoxometalate-based metal‒organic framework for one-step selective oxidative cleavage of β-O-4 lignin model compounds
Tian, Hong-Rui; Liu, Yi-Wei; Zhang, Zhong; Liu, Shu-Mei; Dang, Tian-Yi; Li, Xiao-Hui; Sun, Xiu-Wei; Lu, Ying; Liu, Shu-Xia; Green Chemistry 22 (2020) 248–255; doi:10.1039/C9GC03626A

data_7239605
_publ_section_title
;
 A multicentre synergistic polyoxometalate-based metal--organic framework
 for one-step selective oxidative cleavage of \b-O-4 lignin model
 compounds
;
_journal_issue                   1
_journal_name_full               'Green Chemistry'
_journal_page_first              248
_journal_page_last               255
_journal_paper_doi               10.1039/C9GC03626A
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'O13 V5, 2(C10 H14 Cu N4), H2 O'
_chemical_formula_sum            'C20 H30 Cu2 N8 O14 V5'
_chemical_formula_weight         988.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.02.02 svn.r3481 for OlexSys, GUI svn.r5480)
;
_audit_update_record
;
2019-04-28 deposited with the CCDC.	2019-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.796(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7662(11)
_cell_length_b                   12.1453(5)
_cell_length_c                   24.9282(11)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.26
_cell_volume                     6811.6(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      294.9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34966
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.742
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    2.610
_exptl_absorpt_correction_T_max  0.593
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       plate
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         6490
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0210P)^2^+59.9715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5329
_reflns_number_total             6490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9gc03626a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7239605.cif.

 Adding full bibliography for 7239605.cif.
;
_cod_database_code               7239605
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.598
_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,H) groups
2. Restrained distances
 C18A-C19A
 1.5 with sigma of 0.02
 C18B-N5A
 2.5 with sigma of 0.02
 C19B-C18B = C18B-C17A
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C16A, Cu2, N6, C14, C16, N5, C15, C17, C18A, C19A, C20, N8, C12, C11, C13,
 N8A, C13A, N7, C20A, C11A, N7A, C19B, C18B, C17A, N5A, C15A, C14A, N6A, Cu3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cu3)=Sof(H12A)=Sof(C15A)=Sof(H15A)=Sof(N6A)=Sof(C14A)=Sof(H14A)=Sof(C16A)=
 Sof(H16A)=Sof(N5A)=Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=
 Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(N8A)=Sof(C11A)=
 Sof(H11A)=Sof(C13A)=Sof(H13A)=Sof(N7A)=1-FVAR(1)
 Sof(Cu2)=Sof(N6)=Sof(C14)=Sof(H14)=Sof(N5)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16)=Sof(N7)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(N8)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C19A)=
 Sof(H19A)=Sof(H19B)=Sof(C11)=Sof(H11)=FVAR(1)
5.a Free rotating group:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C9(H9A,H9B), C20(H20A,H20B), C8(H8A,H8B), C17(H17A,H17B),
 C7(H7A,H7B), C18A(H18A,H18B), C19A(H19A,H19B), C17A(H17C,H17D), C18B(H18C,
 H18D), C19B(H19C,H19D), C20A(H20C,H20D)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C12(H12), C12(H12A), C13(H13), C6(H6), C1A(H1A),
  C2A(H2A), C4A(H4A), C5A(H5A), C3A(H3A), C11(H11), C15A(H15A), C14A(H14A),
 C16A(H16A), C11A(H11A), C13A(H13A)
;
_shelx_res_checksum              91214
_olex2_submission_special_instructions 'No special instructions were received'