Polyoxotungstates in Molecular Boxes of Purine Bases
Kulikov, Vladislav; Meyer, Gerd; Crystals 4 (2014) 64–; doi:10.3390/cryst4010064

data_1513838
_publ_section_title
;
 Polyoxotungstates in Molecular Boxes of Purine Bases
;
_journal_issue                   1
_journal_name_full               Crystals
_journal_page_first              64
_journal_paper_doi               10.3390/cryst4010064
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'H3 O, 3(C7 H9 N4 O2), W10 O32, 7.5(H2 O)'
_chemical_formula_sum            'C21 H45 N12 O46.5 W10'
_chemical_formula_weight         3048.2
_chemical_melting_point          ?
_chemical_name_common
;
Hydronium tritheobrominium decatungstate trihydrate
;
_chemical_name_systematic
; 
Hydronium tritheobrominium di-mu5-oxo-icosa-mu-oxo-decaoxodecatungstate
hemipentadecahydrate
;
_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                79.594(8)
_cell_angle_beta                 89.386(8)
_cell_angle_gamma                70.001(7)
_cell_formula_units_Z            2
_cell_length_a                   13.4905(12)
_cell_length_b                   15.1707(14)
_cell_length_c                   17.0692(17)
_cell_measurement_reflns_used    41410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      0.86
_cell_volume                     3223.8(6)
_computing_cell_refinement       'X-Area, (Stoe, 2001)'
_computing_data_collection       'X-Area, (Stoe, 2001)'
_computing_data_reduction        'X-Area, (Stoe, 2001)'
_computing_molecular_graphics    'Diamond v3.2 (Crystal Impact 2012)'
_computing_publication_material  'Diamond v3.2 (Crystal Impact 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       '\w and \f 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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.0549
_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       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41410
_diffrn_reflns_theta_full        27.30
_diffrn_reflns_theta_max         27.30
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    17.859
_exptl_absorpt_correction_T_max  0.1890
_exptl_absorpt_correction_T_min  0.0689
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001) 
was performed after optimizing the crystal shape 
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.057
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.046
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.00023(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   0.882
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         14242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                9945
_reflns_number_total             14242
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            THBW10.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3223.8(5)
_cod_database_code               1513838