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_1559142
_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
'2(C11 H13 Co0.5 Mo3 N O12), 3(C16 H36 N), 2(C2 H3 N)'
_chemical_formula_sum            'C74 H140 Co Mo6 N7 O24'
_chemical_formula_weight         2146.50
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-22
_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                90.00
_cell_angle_beta                 106.497(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0770(3)
_cell_length_b                   20.9593(2)
_cell_length_c                   25.0897(3)
_cell_measurement_reflns_used    13665
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7770
_cell_measurement_theta_min      3.2340
_cell_volume                     9114.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37368
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.047
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         16047
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+3.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                12388
_reflns_number_total             16047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0nr05662f2.cif
_cod_data_source_block           p190707a2_sqd
_cod_depositor_comments
'Adding full bibliography for 1559142--1559143.cif.'
_cod_database_code               1559142
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5EA,H5EB,H5EC} of C5EA, All C(H,H) groups, All C(H,H,H,
  H) groups, All N(H) groups
 At 1.5 times of:
  {H17C,H17D,H17E} of C175, {H6AA,H6AB,H6AC} of C6AA, {H1DA,H1DB,H1DC} of
  C1DA, {H2DA,H2DB,H2DC} of C2DA, {H3A,H3B,H3C} of C3, {H21A,H21B,H21C} of C216,
   {H9CA,H9CB,H9CC} of C9CA, {H20A,H20B,H20C} of C200, {H1EA,H1EB,H1EC} of C1EA,
   {H4BA,H4BB,H4BC} of C4BA, {H4DA,H4DB,H4DC} of C4DA, {H9BA,H9BB,H9BC} of C9BA,
   {H2EA,H2EB,H2EC} of C2EA, {H17F,H17G,H17H} of C17
2. Rigid bond restraints
 C128, C101, C175, C147
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4BA, C76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C128 \\sim C101 \\sim C175: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C147 \\sim C128 \\sim C101 \\sim C175: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C4DA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C5EA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(N6DA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C101) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C175) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
4. Others
 Sof(H10C)=Sof(H10D)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C175)=Sof(H17C)=Sof(H17D)=Sof(H17E)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C65(H65A,H65B), C146(H14I,H14J), C10(H10G,H10H), C26(H26A,
 H26B), C62(H62A,H62B), C1(H1A,H1B), C13(H13A,H13B), C3DA(H3DA,H3DB), C19(H19A,
 H19B), C106(H10E,H10F), C134(H13C,H13D), C139(H13E,H13F), C143(H14C,H14D),
 C145(H14E,H14F), C148(H14G,H14H), C192(H19C,H19D), C226(H22A,H22B), C8BA(H8BA,
 H8BB), C0CA(H0CA,H0CB), C6DA(H6DA,H6DB), C7DA(H7DA,H7DB), C76(H76A,H76B),
 C95(H95A,H95B), C96(H96A,H96B), C101(H10A,H10B), C101(H10C,H10D), C115(H11A,
 H11B), C128(H12A,H12B), C147(H14A,H14B), C172(H17A,H17B), C2(H2A,H2B), C5(H5A,
 H5B), C11(H11C,H11D), C15(H15A,H15B), C7BA(H7BA,H7BB), C77(H77A,H77B),
 C130(H13G,H13H), C161(H16A,H16B), C165(H16C,H16D), C181(H18A,H18B), C203(H20D,
 H20E), C223(H22C,H22D)
5.b Aromatic/amide H refined with riding coordinates:
 N74(H74), C7CA(H7CA), C2BA(H2BA), C1BA(H1BA), C6CA(H6CA), C9(H9), C140(H140),
 N69(H69), C0AA(H0AA), C3BA(H3BA), C3CA(H3CA), C4CA(H4CA), C43(H43), C188(H188)
5.c Idealised Me refined as rotating group:
 C9BA(H9BA,H9BB,H9BC), C2EA(H2EA,H2EB,H2EC), C17(H17F,H17G,H17H), C200(H20A,
 H20B,H20C), C4DA(H4DA,H4DB,H4DC), C4BA(H4BA,H4BB,H4BC), C1EA(H1EA,H1EB,H1EC),
 C175(H17C,H17D,H17E), C6AA(H6AA,H6AB,H6AC), C1DA(H1DA,H1DB,H1DC), C2DA(H2DA,
 H2DB,H2DC), C216(H21A,H21B,H21C), C9CA(H9CA,H9CB,H9CC), C5EA(H5EA,H5EB,H5EC),
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'