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_7024025
_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            'C48 H81 Fe9 N16 Na9 O123 Si3 W28'
_chemical_formula_weight         8791.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.25(3)
_cell_angle_beta                 89.04(3)
_cell_angle_gamma                89.28(3)
_cell_formula_units_Z            2
_cell_length_a                   15.302(3)
_cell_length_b                   23.309(5)
_cell_length_c                   27.828(6)
_cell_measurement_reflns_used    78667
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      3.0
_cell_volume                     9902(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_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  0.1291
_diffrn_reflns_av_sigmaI/netI    0.2116
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61688
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    16.948
_exptl_absorpt_correction_T_max  0.1410
_exptl_absorpt_correction_T_min  0.1119
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.949
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7824
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
;
_refine_diff_density_max         4.618
_refine_diff_density_min         -3.523
_refine_diff_density_rms         0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1601
_refine_ls_number_reflns         31581
_refine_ls_number_restraints     514
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2132
_reflns_number_gt                15065
_reflns_number_total             31581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b905079e.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        9902(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024025