Tris{4-[(2<i>H</i>-tetrazol-5-yl)methyl]morpholinium} dodecatungstophosphate hexahydrate
Feizyzadeh, Babak; Mirzaei, Masoud; Eshtiagh-Hosseini, Hossein; Gholizadeh, Ahmad; Acta Crystallographica Section E 67 (2011) m301–m302; doi:10.1107/S1600536811003734

data_2229535
_publ_section_title
;
 Tris{4-[(2<i>H</i>-tetrazol-5-yl)methyl]morpholinium}
 dodecatungstophosphate hexahydrate
;
_journal_coeditor_code           WM2435
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m301
_journal_page_last               m302
_journal_paper_doi               10.1107/S1600536811003734
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C6 H12 N5 O)3 [W12 (P O4) O36], 6H2 O'
_chemical_formula_moiety         '3(C6 H12 N5 O +), O40 P W12 3-, 6(H2 O)'
_chemical_formula_sum            'C18 H48 N15 O49 P W12'
_chemical_formula_weight         3495.88
_chemical_name_systematic
;
Tris{4-[(2<i>H</i>-tetrazol-5-yl)methyl]morpholinium} dodecatungstophosphate
hexahydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.616(3)
_cell_length_b                   15.213(3)
_cell_length_c                   26.735(6)
_cell_measurement_reflns_used    846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.43
_cell_volume                     5945(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       \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  0.1585
_diffrn_reflns_av_sigmaI/netI    0.1184
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            59635
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    23.265
_exptl_absorpt_correction_T_max  0.246
_exptl_absorpt_correction_T_min  0.078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.801
_refine_diff_density_min         -2.715
_refine_ls_abs_structure_details 'Flack (1983), 5544 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.041(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         12321
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                9617
_reflns_number_total             12321
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2435.cif
_cod_data_source_block           I
_cod_original_cell_volume        5944(2)
_cod_database_code               2229535
_cod_database_fobs_code          2229535