Tris(propane-1,3-diammonium) decavanadate 5.5-hydrate
Chun-Yuan Zhu; Yan-Tuan Li; Zhi-Yong Wu; Man Jiang; Acta Crystallographica Section E 62 (2006) m3092–m3095; doi:10.1107/S1600536806042553

data_2211122
_publ_section_title
;
 Tris(propane-1,3-diammonium) decavanadate 5.5-hydrate
;
_journal_coeditor_code           LN3021
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3092
_journal_page_last               m3095
_journal_paper_doi               10.1107/S1600536806042553
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C3 H12 N2)3 [V10 O28], 5.5H2 O'
_chemical_formula_moiety         '3C3 H12 N2 3+, O28 V10 6-, 5.5H2 O'
_chemical_formula_sum            'C9 H47 N6 O33.5 V10'
_chemical_formula_weight         1284.93
_chemical_name_systematic
;
Tris(propane-1,3-diammonium) decavanadate 5.5-hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.6090(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1206(16)
_cell_length_b                   14.4900(16)
_cell_length_c                   18.733(2)
_cell_measurement_reflns_used    3320
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.116
_cell_measurement_theta_min      2.372
_cell_volume                     3814.6(7)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'CAMERON (Watkin <i>et al.</i>,  1993) and 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX 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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15786
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.447
_exptl_absorpt_correction_T_max  0.5843
_exptl_absorpt_correction_T_min  0.4740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.533
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         6903
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                5600
_reflns_number_total             6911
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ln3021.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2211122
_cod_database_fobs_code          2211122