Two inorganic‒organic hybrid materials based on polyoxometalate anions and methylene blue: Preparations, crystal structures and properties
Nie, Shanshan; Zhang, Yaobin; Liu, Bin; Li, Zuoxi; Hu, Huaiming; Xue, Ganglin; Fu, Feng; Wang, Jiwu; Journal of Solid State Chemistry 183 (2010) 2957–2962; doi:10.1016/j.jssc.2010.08.023

data_1563391
_publ_section_title
;
 Two inorganic--organic hybrid materials based on polyoxometalate anions
 and methylene blue: Preparations, crystal structures and properties
;
_journal_issue                   12
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              2957
_journal_page_last               2962
_journal_paper_doi               10.1016/j.jssc.2010.08.023
_journal_volume                  183
_journal_year                    2010
_chemical_formula_sum            'C38 H50 N8 O21 S2 W6'
_chemical_formula_weight         2122.08
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.777(2)
_cell_angle_beta                 65.197(2)
_cell_angle_gamma                79.206(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3680(18)
_cell_length_b                   11.703(2)
_cell_length_c                   12.164(2)
_cell_measurement_temperature    296(2)
_cell_volume                     1311.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6527
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    13.266
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadbas
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.782
_refine_diff_density_min         -2.128
_refine_diff_density_rms         0.324
_refine_ls_extinction_coef       0.0000(2)
_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   0.988
_refine_ls_hydrogen_treatment    constrn
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          2.177
_refine_ls_shift/su_mean         0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+1.6511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                3660
_reflns_number_total             4569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-2957.cif
_cod_data_source_block           xb3515_0m
_cod_original_cell_volume        1311.4(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1563391