Polyoxometalates-based heterometallic organic-inorganic hybrid materials for rapid adsorption and selective separation of methylene blue from aqueous solutions
Fei-Yan Yi; Wei Zhu; Song Dang; Jian-Ping Li; Dai Wu; Yun-hui Li; Zhong-Ming Sun; Chem.Commun. 51 (2015) 3336–; doi:10.1039/C4cc09569C

data_7116528
_publ_section_title
;
 Polyoxometalates-based heterometallic organic-inorganic hybrid materials
 for rapid adsorption and selective separation of methylene blue from
 aqueous solutions
;
_journal_name_full               Chem.Commun.
_journal_page_first              3336
_journal_paper_doi               10.1039/C4cc09569C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C16 H111 Cu4 Dy2 K2 N16 O101.5 Si2 W22'
_chemical_formula_weight         6910.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-23 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.9730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.5847(11)
_cell_length_b                   13.4613(7)
_cell_length_c                   22.9069(13)
_cell_measurement_reflns_used    4214
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      1.82
_cell_volume                     6209.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19627
_diffrn_reflns_theta_full        26.09
_diffrn_reflns_theta_max         26.09
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    22.331
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS was used for absorption correction. wR2(int) was 0.0672 before and 0.0527 after correction. The Ratio of minimum to maximum transmission is 0.8148. The  Lambda/2 correction factor is 0.0015.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    3.696
_exptl_crystal_density_meas      3.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6146
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_platon_squeeze_details
;
;
_refine_diff_density_max         2.515
_refine_diff_density_min         -2.311
_refine_diff_density_rms         0.336
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.000037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         8892
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+59.1303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                7796
_reflns_number_total             8892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc09569c2.cif
_cod_data_source_block           Dy-1
_cod_original_sg_symbol_H-M      Cm
_cod_original_formula_sum        'C16 H111 Cu4 Dy2 K2 N16 O101.50 Si2 W22'
_cod_database_code               7116528