Butane-1,4-diammonium decavanadate(V) hexahydrate
Rakovský, Erik; Gyepes, Robert; Acta Crystallographica Section E 62 (2006) m2108–m2110; doi:10.1107/S1600536806030480

data_2210239
_publ_section_title
;
 Butane-1,4-diammonium decavanadate(V) hexahydrate
;
_journal_coeditor_code           GK2024
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2108
_journal_page_last               m2110
_journal_paper_doi               10.1107/S1600536806030480
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C4 H14 N2)3 [V10 O28], 6 H2 O'
_chemical_formula_moiety         '3C4 H14 N2 2+, V10 O28 6-, 6H2 O'
_chemical_formula_sum            'C12 H54 N6 O34 V10'
_chemical_formula_weight         1336.01
_chemical_name_systematic
;
butane-1,4-diammonium decavanadate(V) hexahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0375(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6504(4)
_cell_length_b                   17.6351(4)
_cell_length_c                   10.9644(4)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2058.04(12)
_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
'ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material
;
SHELXL97 and publCIF (Westrip, 2006)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD \k-axis'
_diffrn_measurement_method       '\w and \f scans'
_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  0.047
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15546
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[PLATON (Spek, 2003), analytical numeric absorption correction using
a multifaceted crystal model based on de Meulenaar & Tompa (1965)]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.518
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4706
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0319P)^2^+2.7675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                3665
_reflns_number_total             4706
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2210239
_cod_database_fobs_code          2210239