Immobilization of enzymes on an organic‒inorganic hybrid network consisting of Dawson-type polyoxotungstate and a zinc(ii)-biimidazole complex moiety
Zhu, Haotian; Du, Jing; Lu, Ying; Su, Fang; Li, Yangguang; New Journal of Chemistry 43 (2019) 146–; doi:10.1039/C8NJ03776K

data_7057961
_publ_section_title
;
 Immobilization of enzymes on an organic--inorganic hybrid network
 consisting of Dawson-type polyoxotungstate and a zinc(ii)-biimidazole
 complex moiety
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              146
_journal_paper_doi               10.1039/C8NJ03776K
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C36 H36 N24 O62 P2 W18 Zn3, 6(O)'
_chemical_formula_sum            'C36 H48 N24 O68 P2 W18 Zn3'
_chemical_formula_weight         5472.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-17 deposited with the CCDC.
2018-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                98.5770(10)
_cell_angle_beta                 97.6530(10)
_cell_angle_gamma                118.7610(10)
_cell_formula_units_Z            2
_cell_length_a                   14.6698(9)
_cell_length_b                   14.9855(9)
_cell_length_c                   24.7793(15)
_cell_measurement_reflns_used    8947
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.788
_cell_measurement_theta_min      2.613
_cell_volume                     4588.1(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23345
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.596
_exptl_absorpt_coefficient_mu    23.379
_exptl_absorpt_correction_T_max  0.4703
_exptl_absorpt_correction_T_min  0.2356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.961
_exptl_crystal_description       block
_exptl_crystal_F_000             4856
_exptl_crystal_size_max          0.087
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.038
_refine_diff_density_max         3.680
_refine_diff_density_min         -3.504
_refine_diff_density_rms         0.396
_refine_ls_extinction_coef       0.000046(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1361
_refine_ls_number_reflns         16041
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12404
_reflns_number_total             16041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj03776k2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7057961--7057962.cif.'
_cod_database_code               7057961
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.470
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C35-C36
 1.38 with sigma of 0.01
 C36-N24
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O10) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O39)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O8) \\sim Ueq, Uanis(O47) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N13) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N7(H7), N8(H8), N13(H13), N14(H14), N15(H15), N16(H16),
 N21(H21), N22(H22), N23(H23), N24(H24), C3(H3), C4(H4), C5(H5A), C6(H6A),
 C9(H9), C10(H10), C11(H11), C12(H12), C15(H15A), C16(H16A), C17(H17), C18(H18),
  C21(H21A), C22(H22A), C23(H23A), C24(H24A), C27(H27), C28(H28), C29(H29),
 C30(H30), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              71933
_shelx_hkl_checksum              37232
_shelx_fab_checksum              41582
_olex2_submission_special_instructions 'No special instructions were received'