Butane-1,4-diammonium dihydrogendecavanadate(V)
Rakovský, Erik; Gyepes, Robert; Acta Crystallographica Section E 62 (2006) m1820–m1822; doi:10.1107/S1600536806026249

data_2209881
_publ_section_title
;
 Butane-1,4-diammonium dihydrogendecavanadate(V)
;
_journal_coeditor_code           HK2073
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1820
_journal_page_last               m1822
_journal_paper_doi               10.1107/S1600536806026249
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C4 H14 N2)2 H2 V10 O28'
_chemical_formula_moiety         'H2 O28 V10, 2(C4 H14 N2)'
_chemical_formula_sum            'C8 H30 N4 O28 V10'
_chemical_formula_weight         1139.76
_chemical_name_systematic
;
1,4-butanediamminium dihydrogendecavanadate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   10.22680(10)
_cell_length_b                   16.7196(2)
_cell_length_c                   18.2311(2)
_cell_measurement_reflns_used    32381
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      1.00
_cell_volume                     3117.30(6)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material
;
publCIF (Westrip, 2006)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius KappaCCD \k-axis'
_diffrn_measurement_method       '\w-scans to fill Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.092
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            59189
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    2.964
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
PLATON (Spek, 2003), analytical numeric absorption correction using a
multifaceted crystal model based on de Meulenaer Tompa (1965).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.374
_refine_ls_abs_structure_details
;
?
;
_refine_ls_extinction_coef       0.00128(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0180P)^2^+3.0702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                4375
_reflns_number_total             4555
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2073.cif
_cod_data_source_block           I
_cod_database_code               2209881
_cod_database_fobs_code          2209881