Crystal structure of tetraguanidinium [hexahydrogen hexaarsenato(V)tetravanadate(V)] tetrahydrate
Harrison, William T. A.; Acta Crystallographica Section E 70 (2014) m305–m306; doi:10.1107/S1600536814011349

data_2239818
_publ_section_title
;
 Crystal structure of tetraguanidinium [hexahydrogen
 hexaarsenato(V)tetravanadate(V)] tetrahydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m305
_journal_page_last               m306
_journal_paper_doi               10.1107/S1600536814011349
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C H6 N3)4 [H6 V4 As6 O30], 4H2 O'
_chemical_formula_moiety         '4(C H6 N3 +), H6 As6 O30 V4 4-, 4(H2 O)'
_chemical_formula_sum            'C4 H34 As6 N12 O34 V4'
_chemical_formula_weight         1447.71
_chemical_name_systematic
;
Tetraguanidinium [hexahydrogen hexaarsenato(V)tetravanadate(V)] tetrahydrate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.8920(10)
_cell_angle_beta                 94.6960(10)
_cell_angle_gamma                111.7510(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0403(5)
_cell_length_b                   11.0199(6)
_cell_length_c                   11.9806(6)
_cell_measurement_reflns_used    3266
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.28
_cell_volume                     1071.39(10)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Dowty, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70173
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8711
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.556
_exptl_absorpt_correction_T_max  0.4029
_exptl_absorpt_correction_T_min  0.2865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                3655
_reflns_number_total             4909
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm0004sup1.cf
_cod_data_source_block           I
_cod_database_code               2239818
_cod_database_fobs_code          2239818