COF-inspired fabrication of two-dimensional polyoxometalate based open frameworks for biomimetic catalysis.
Zhao, Yu; Wang, Zhifang; Gao, Jia; Zhao, Zhengfeng; Li, Xia; Wang, Ting; Cheng, Peng; Ma, Shengqian; Chen, Yao; Zhang, Zhenjie; Nanoscale 12 (2020) 21218–21224; doi:10.1039/d0nr05662f

data_1559143
_publ_section_title
;
 COF-inspired fabrication of two-dimensional polyoxometalate based open
 frameworks for biomimetic catalysis.
;
_journal_issue                   41
_journal_name_full               Nanoscale
_journal_page_first              21218
_journal_page_last               21224
_journal_paper_doi               10.1039/d0nr05662f
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety
'0.05(C22 H24 Mn Mo6 N2 O24), 0.1(C16 H36 N), 0.05(C22 H26 Mn Mo6 N2 O24), 0.1(C2 H3 N)'
_chemical_formula_sum            'C4 H6.3 Mn0.1 Mo0.6 N0.4 O2.4'
_chemical_formula_weight         161.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-16 deposited with the CCDC.	2020-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.116(3)
_cell_angle_gamma                90
_cell_formula_units_Z            40
_cell_length_a                   15.4385(5)
_cell_length_b                   24.0709(8)
_cell_length_c                   25.3004(8)
_cell_measurement_reflns_used    10492
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1400
_cell_measurement_theta_min      3.4410
_cell_volume                     9255.9(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36809
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.981
_exptl_absorpt_coefficient_mu    0.967
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         16296
_refine_ls_number_restraints     591
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+1.7723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11519
_reflns_number_total             16296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr05662f2.cif
_cod_data_source_block           p190617c_sqd_sqd_sq
_cod_depositor_comments
'Adding full bibliography for 1559142--1559143.cif.'
_cod_original_formula_sum        'C4 H6.30 Mn0.10 Mo0.60 N0.40 O2.40'
_cod_database_code               1559143
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8AA-C7AA
 1.45 with sigma of 0.01
3. Rigid bond restraints
 N22, C7AA
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C8AA, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C26 \\sim C29 \\sim C30 \\sim C47 \\sim C50 \\sim C16 \\sim C32 \\sim C44 \\sim
C6 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim
C15 \\sim C0AA \\sim C18 \\sim C8AA \\sim C1AA \\sim C9AA \\sim C6AA \\sim C2AA
\\sim C3AA \\sim C4AA \\sim C7AA \\sim C17 \\sim C5AA \\sim C19 \\sim C20 \\sim
C3BA \\sim C1BA \\sim C2BA \\sim C4BA \\sim C0BA \\sim C0DA \\sim C5DA \\sim C7
\\sim C3EA: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C30(H30A,H30B), C47(H47A,H47B), C50(H50A,H50B), C16(H16A,
 H16B), C44(H44A,H44B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,
 H12B), C13(H13A,H13B), C15(H15A,H15B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB),
 C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C17(H17A,H17B), C0BA(H0BA,H0BB)
5.b Aromatic/amide H refined with riding coordinates:
 N37(H37), C8(H8), C14(H14), C18(H18), C9AA(H9AA), C4AA(H4AA), C7AA(H7AA),
 C5AA(H5AA), C20(H20), C3BA(H3BA), C1BA(H1BA), C2BA(H2BA), C4BA(H4BA)
5.c Idealised Me refined as rotating group:
 C6AA(H6AA,H6AB,H6AC), C19(H19A,H19B,H19C), C0DA(H0DA,H0DB,H0DC), C5DA(H5DA,
 H5DB,H5DC), C3EA(H3EA,H3EB,H3EC)
;
_shelx_res_checksum              62534
_shelx_fab_checksum              56704
_olex2_submission_special_instructions 'No special instructions were received'