Cu-Induced [H6W12O42]6− polyoxometalate-based bimetallic cluster formation for renewable biomass inulin hydrolysis toward fructose production
Chen, Yongdong; Zhang, Chaolei; Zhang, Jiangwei; Ye, Zhongbin; Zheng, Kai; Fang, Qihua; Li, Gao; Inorganic Chemistry Frontiers 4 (2017) 1917–; doi:10.1039/C7QI00516D

data_4349773
_publ_section_title
;
 Cu-Induced [H6W12O42]6&#x2212; polyoxometalate-based bimetallic cluster
 formation for renewable biomass inulin hydrolysis toward fructose
 production
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1917
_journal_paper_doi               10.1039/C7QI00516D
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'Cu3 H22 O50 W12, 24(H2 O)'
_chemical_formula_sum            'Cu3 H70 O74 W12'
_chemical_formula_weight         3651.29
_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             2017-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-08-13 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                113.737(4)
_cell_angle_beta                 90.433(3)
_cell_angle_gamma                112.560(4)
_cell_formula_units_Z            1
_cell_length_a                   10.6753(5)
_cell_length_b                   12.7814(5)
_cell_length_c                   13.0976(5)
_cell_measurement_reflns_used    6153
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.499
_cell_measurement_theta_min      2.971
_cell_volume                     1482.74(13)
_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_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.971
_exptl_absorpt_coefficient_mu    24.359
_exptl_absorpt_correction_T_max  0.008
_exptl_absorpt_correction_T_min  0.004
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1621
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.096
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+4.6216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5399
_reflns_number_total             6153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00516d2.cif
_cod_data_source_block           exp_4083
_cod_original_cell_volume        1482.73(12)
_cod_database_code               4349773
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H,H) groups
2. Restrained distances
 W6-H2
 2.3 with sigma of 0.02
 O2-H2
 0.8 with sigma of 0.02
 W2-H3
 2.3 with sigma of 0.02
 W5-H3_$1
 2.3 with sigma of 0.02
 W4-H3_$1
 2.3 with sigma of 0.02
 W5-H2
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O11) \\sim
Ueq, Uanis(O15) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O21) \\sim Ueq,
Uanis(O24) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Free rotating group:
 O33(H33A,H33B), O29(H29A,H29B), O32(H32A,H32B), O35(H35A,H35B), O34(H34A,
 H34B), O28(H28A,H28B), O30(H30A,H30B), O36(H36A,H36B), O27(H27A,H27B),
 O25(H25A,H25B), O31(H31A,H31B), O26(H26A,H26B)
4.b Rotating group:
 O24(H24A,H24B), O22(H22A,H22B), O23(H23A,H23B), O1AA(H1AA,H1AB)
4.c Ternary CH refined with riding coordinates:
 O1(H1)
;