Tris{<i>trans</i>-4-[<i>p</i>-(<i>N</i>,<i>N</i>-diethylamino)styryl]-<i>N</i>-methylpyridinium} dodecatungstophosphate
Xuejie Tan; Sixiu Sun; Shu-Lian Liu; Jian-Ping Ma; Dian-Xiang Xing; Acta Crystallographica Section E 61 (2005) m437–m440; doi:10.1107/S1600536805002928

data_2205326
_publ_section_title
;Tris{<i>trans</i>-4-[<i>p</i>-(<i>N</i>,<i>N</i>-diethylamino)styryl]-<i>N</i>-methylpyridinium}
 dodecatungstophosphate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m437
_journal_page_last               m440
_journal_paper_doi               10.1107/S1600536805002928
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C18 H23 N2)3 [P W12 O40]'
_chemical_formula_moiety         '3(C18 H23 N2 +), O40 P W12 3-'
_chemical_formula_sum            'C54 H69 N6 O40 P W12'
_chemical_formula_weight         3679.32
_chemical_name_systematic
;
Tris{trans-4-[p-(N,N-diethylamino)styryl]-N-methylpyridinium}
dodecatungstophosphate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.467(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.394(4)
_cell_length_b                   21.167(3)
_cell_length_c                   13.0130(15)
_cell_measurement_reflns_used    380
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      7.5
_cell_volume                     8906(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      288(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26688
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    15.526
_exptl_absorpt_correction_T_max  0.158
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6632
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.785
_refine_diff_density_min         -1.672
_refine_ls_abs_structure_details 'Flack (1983), 7126 Friedel pairs'
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         16777
_refine_ls_number_restraints     583
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1095P)^2^+138.0939P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2137
_reflns_number_gt                12364
_reflns_number_total             16779
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6472.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 (45 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 (45 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        8907(2)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2205326
_cod_database_fobs_code          2205326