Tetrakis{4-[(2<i>H</i>-tetrazol-5-yl)methyl]morpholin-4-ium} dodecatungstosilicate hexahydrate
Yousefi, Mohammad; Eshtiagh-Hosseini, Hossein; Mirzaei, Masoud; Gholizadeh, Ahmad; Nikpour, Mohsen; Acta Crystallographica Section E 67 (2011) m271–m272; doi:10.1107/S1600536811001772

data_2229269
_publ_section_title
;
 Tetrakis{4-[(2<i>H</i>-tetrazol-5-yl)methyl]morpholin-4-ium}
 dodecatungstosilicate hexahydrate
;
_journal_coeditor_code           XU5096
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m271
_journal_page_last               m272
_journal_paper_doi               10.1107/S1600536811001772
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C6 H12 N5 O)4 [W12 (Si O4) O36], 6H2 O'
_chemical_formula_moiety         '4(C6 H12 N5 O +), O40 Si W12 4-, 6(H2 O)'
_chemical_formula_sum            'C24 H60 N20 O50 Si W12'
_chemical_formula_weight         3663.21
_chemical_name_systematic
;
Tetrakis{4-[(2<i>H</i>-tetrazol-5-yl)methyl]morpholin-4-ium}
dodecatungstosilicate hexahydrate
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.8560(10)
_cell_angle_beta                 116.3310(10)
_cell_angle_gamma                116.4500(10)
_cell_formula_units_Z            1
_cell_length_a                   12.4512(5)
_cell_length_b                   13.1805(5)
_cell_length_c                   13.4065(6)
_cell_measurement_reflns_used    7382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.91
_cell_measurement_theta_min      2.26
_cell_volume                     1666.58(12)
_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  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33857
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.752
_exptl_absorpt_correction_T_max  0.164
_exptl_absorpt_correction_T_min  0.024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1646
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.911
_refine_diff_density_min         -3.377
_refine_ls_abs_structure_details 'Flack (1983), 8497 Friedel pairs'
_refine_ls_abs_structure_Flack   0.377(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         17355
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0033P)^2^+14.9946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                16382
_reflns_number_total             17355
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5096.cif
_cod_data_source_block           I
_cod_database_code               2229269
_cod_database_fobs_code          2229269