Tris[(3-aminopropyl)dimethylammonium] decavanadate(V) hexahydrate
Zhu, Chun-Yuan; Li, Yan-Tuan; Wu, Jian-Dong; Wu, Zhi-Yong; Wu, Xia; Acta Crystallographica Section E 63 (2007) m1777–m1778; doi:10.1107/S1600536807023306

data_2214002
_publ_section_title
;
 Tris[(3-aminopropyl)dimethylammonium] decavanadate(V) hexahydrate
;
_journal_coeditor_code           XU2250
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1777
_journal_page_last               m1778
_journal_paper_doi               10.1107/S1600536807023306
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '3(C5 H16 N2)2+. [V10 O28]6-. 6H2 O'
_chemical_formula_moiety         '3(C5 H16 N2), O28 V10, 6(H2 O)'
_chemical_formula_sum            'C15 H60 N6 O34 V10'
_chemical_formula_weight         1378.09
_chemical_name_systematic
;
Tris[(3-aminopropyl)dimethylammonium] decavanadate(V) hexahydrate
;
_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
_cell_angle_alpha                90.45(3)
_cell_angle_beta                 94.21(3)
_cell_angle_gamma                117.29(3)
_cell_formula_units_Z            2
_cell_length_a                   11.525(2)
_cell_length_b                   11.743(2)
_cell_length_c                   18.709(4)
_cell_measurement_reflns_used    1736
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      3.5
_cell_volume                     2241.7(10)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12138
_diffrn_reflns_theta_full        25.2
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.045
_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^)+(0.0576P)^2^+1.1434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.109
_refine_ls_wR_factor_ref         0.134
_reflns_number_gt                4858
_reflns_number_total             8110
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu2250.cif
_cod_data_source_block           I
_cod_database_code               2214002
_cod_database_fobs_code          2214002