Preparation of polyoxometalates in ionic liquids by ionothermal synthesis.
Lin, Shiwei; Liu, Wenli; Li, Yangguang; Wu, Qiong; Wang, Enbo; Zhang, Zhiming; Dalton transactions (Cambridge, England : 2003) 39 (2010) 1740–1744; doi:10.1039/b905079e

data_7024026
_publ_section_title
;
 Preparation of polyoxometalates in ionic liquids by ionothermal
 synthesis.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1740
_journal_page_last               1744
_journal_paper_doi               10.1039/b905079e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C24 H68 Mo12 N8 O52 Si'
_chemical_formula_weight         2480.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.056(3)
_cell_length_b                   16.167(3)
_cell_length_c                   26.572(5)
_cell_measurement_reflns_used    56830
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      3.06
_cell_volume                     6468(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46487
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.379
_exptl_absorpt_correction_T_max  0.7633
_exptl_absorpt_correction_T_min  0.7020
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         1.543
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details 'Flack (1983), 3845 Friedel pairs'
_refine_ls_abs_structure_Flack   0.34(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         6250
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0932P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                5410
_reflns_number_total             6250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905079e.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      p2(1)2(1)2(1)
_cod_database_code               7024026