Triclinic modification of tetrakis(triethylammonium) dihydrogenodecavanadate(V)
Ng, Seik Weng; Acta Crystallographica Section E 67 (2011) m811–m812; doi:10.1107/S1600536811019696

data_2230563
_publ_section_title
;
 Triclinic modification of tetrakis(triethylammonium)
 dihydrogenodecavanadate(V)
;
_journal_coeditor_code           ZS2113
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m811
_journal_page_last               m812
_journal_paper_doi               10.1107/S1600536811019696
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C6 H16 N)4 [H2 V10 O28]'
_chemical_formula_moiety         '4(C6 H16 N +), H2 O28 V10 4-'
_chemical_formula_sum            'C24 H66 N4 O28 V10'
_chemical_formula_weight         1368.21
_chemical_name_systematic
;
tetrakis(triethylammonium) dihydrogenodecavanadate(V)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.669(3)
_cell_angle_beta                 86.263(3)
_cell_angle_gamma                76.979(3)
_cell_formula_units_Z            4
_cell_length_a                   13.1735(4)
_cell_length_b                   20.0061(7)
_cell_length_c                   20.2427(7)
_cell_measurement_reflns_used    9283
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3491
_cell_measurement_theta_min      2.2627
_cell_volume                     4613.0(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38533
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  0.8235
_exptl_absorpt_correction_T_min  0.6880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.470
_refine_diff_density_min         -0.786
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         20465
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+4.3210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                13087
_reflns_number_total             20465
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2113.cif
_cod_data_source_block           I
_cod_database_code               2230563
_cod_database_fobs_code          2230563