A New Method for the Synthesis of Organopolyoxometalate Hybrid Compounds
Bar-Nahum, Itsik; Ettedgui, Jessica; Konstantinovski, Leonid; Kogan, Vladimir; Neumann, Ronny; Inorganic Chemistry 46 (2007) 5798–5804; doi:10.1021/ic700540g

data_4333292
_publ_section_title
;
 A New Method for the Synthesis of Organopolyoxometalate Hybrid Compounds
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5798
_journal_page_last               5804
_journal_paper_doi               10.1021/ic700540g
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C16 H36 N O14.33 P0.33 Sn0.33 W3.67'
_chemical_formula_weight         1195.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   23.268(3)
_cell_length_b                   23.268(3)
_cell_length_c                   46.969(9)
_cell_measurement_reflns_used    34671
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.82
_cell_measurement_theta_min      1.02
_cell_volume                     22022(6)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.781
_diffrn_measured_fraction_theta_max 0.781
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1431
_diffrn_reflns_theta_full        18.49
_diffrn_reflns_theta_max         18.49
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    8.806
_exptl_absorpt_correction_T_max  0.2719
_exptl_absorpt_correction_T_min  0.2719
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.907
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+4799.7134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2407
_reflns_number_gt                1078
_reflns_number_total             1431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700540gsup1.cif
_cod_data_source_block           n29a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_sg_symbol_H-M      R-3c
_cod_database_code               4333292