Tetrakis{<i>trans</i>-4-[(<i>N</i>,<i>N</i>-diethylamino)styryl]-1-methylpyridinium} dodecatungstosilicate tetradecahydrate
Xue-Jie Tan; Dian-Xiang Xing; Yun Liu; Acta Crystallographica Section E 62 (2006) m2613–m2615; doi:10.1107/S1600536806036609

data_2210753
_publ_section_title
;Tetrakis{<i>trans</i>-4-[(<i>N</i>,<i>N</i>-diethylamino)styryl]-1-methylpyridinium}
 dodecatungstosilicate tetradecahydrate
;
_journal_coeditor_code           OB3019
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2613
_journal_page_last               m2615
_journal_paper_doi               10.1107/S1600536806036609
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C18 H23 N2)4 [W12 O40 Si W12], 14H2 O'
_chemical_formula_moiety         '4C18 H23 N2 +, O40 Si W12 4-, 14H2 O'
_chemical_formula_sum            'C72 H120 N8 O54 Si W12'
_chemical_formula_weight         4195.91
_chemical_name_systematic
;
Tetrakis{trans-4-[(N,N-diethylamino)styryl]-1-methylpyridinium}
dodecatungstosilicate tetradecahydrate
;
_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                64.393(3)
_cell_angle_beta                 79.436(4)
_cell_angle_gamma                65.578(3)
_cell_formula_units_Z            1
_cell_length_a                   15.019(4)
_cell_length_b                   15.056(4)
_cell_length_c                   16.080(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.74
_cell_volume                     2985.5(14)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.1152
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16302
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    11.598
_exptl_absorpt_correction_T_max  0.311
_exptl_absorpt_correction_T_min  0.065
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Parkin <i>et al.</i>,  1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1914.0
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.182
_refine_diff_density_min         -1.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         10904
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                5387
_reflns_number_total             10904
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob3019.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2210753
_cod_database_fobs_code          2210753