#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/98/2239818.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2239818
loop_
_publ_author_name
'Harrison, William T. A.'
_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       ω
_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/[σ²(Fo²)+(0.0766P)²] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            wm0004sup1.cf
_cod_data_source_block           I
_cod_database_code               2239818
_cod_database_fobs_code          2239818
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
V V1 0.26837(10) 0.46285(10) 0.57607(9) 0.0176(2) Uani d . 1 1
V V2 0.05032(10) 0.50770(11) 0.74922(9) 0.0193(2) Uani d . 1 1
As As1 0.26156(6) 0.46227(6) 0.30244(6) 0.02044(15) Uani d . 1 1
As As2 -0.08161(6) 0.30204(6) 0.44111(5) 0.01626(14) Uani d . 1 1
As As3 0.39072(6) 0.77706(6) 0.84192(5) 0.01955(15) Uani d . 1 1
O O1 0.3661(5) 0.3738(5) 0.5506(4) 0.0282(10) Uani d . 1 1
O O2 0.1882(4) 0.4284(4) 0.6880(4) 0.0192(8) Uani d . 1 1
O O3 0.1265(4) 0.6002(4) 0.6171(4) 0.0194(8) Uani d . 1 1
O O4 0.4243(4) 0.6617(4) 0.7138(4) 0.0202(8) Uani d . 1 1
O O5 0.0880(4) 0.3108(4) 0.4329(4) 0.0198(8) Uani d . 1 1
O O6 0.3215(4) 0.5543(4) 0.4605(4) 0.0211(8) Uani d . 1 1
O O7 -0.0827(4) 0.6107(5) 0.7760(4) 0.0254(9) Uani d . 1 1
O O8 0.0098(5) 0.4435(5) 0.8461(4) 0.0328(10) Uani d . 1 1
O O9 -0.1059(4) 0.3374(4) 0.5863(4) 0.0216(8) Uani d . 1 1
O O10 0.2301(4) 0.7032(4) 0.8748(4) 0.0253(9) Uani d . 1 1
O O11 0.3741(5) 0.5860(6) 0.2582(5) 0.0389(12) Uani d . 1 1
O O12 0.2976(5) 0.3108(5) 0.2403(4) 0.0299(10) Uani d . 1 1
H H12 0.4043 0.3389 0.2643 0.036 Uiso d R 1 1
O O13 0.4138(4) 0.9295(4) 0.8315(4) 0.0260(9) Uani d . 1 1
O O14 0.5335(5) 0.8266(5) 0.9655(4) 0.0319(10) Uani d . 1 1
H H14 0.5560 0.9049 1.0518 0.038 Uiso d R 1 1
O O15 -0.2016(5) 0.1152(4) 0.3450(4) 0.0290(10) Uani d . 1 1
H H15 -0.2710 0.1031 0.2766 0.035 Uiso d R 1 1
C C1 0.6359(8) -0.0343(7) 0.5654(7) 0.0336(15) Uani d . 1 1
N N1 0.5480(7) -0.1219(6) 0.6055(6) 0.0441(16) Uani d . 1 1
H H1A 0.5002 -0.2169 0.5551 0.053 Uiso calc R 1 1
H H1B 0.5389 -0.0834 0.6818 0.053 Uiso calc R 1 1
N N2 0.6494(8) -0.0929(7) 0.4497(7) 0.0530(19) Uani d . 1 1
H H2A 0.7044 -0.0363 0.4229 0.064 Uiso calc R 1 1
H H2B 0.6033 -0.1882 0.4001 0.064 Uiso calc R 1 1
N N3 0.7054(8) 0.1105(7) 0.6418(7) 0.0510(18) Uani d . 1 1
H H3A 0.7607 0.1680 0.6159 0.061 Uiso calc R 1 1
H H3B 0.6959 0.1482 0.7180 0.061 Uiso calc R 1 1
C C2 0.9422(9) 0.0768(8) 0.8896(7) 0.0406(17) Uani d . 1 1
N N4 0.8450(8) 0.0292(9) 0.9471(8) 0.069(2) Uani d . 1 1
H H4A 0.7854 -0.0646 0.9131 0.082 Uiso calc R 1 1
H H4B 0.8411 0.0919 1.0186 0.082 Uiso calc R 1 1
N N5 1.0309(9) 0.2208(7) 0.9432(7) 0.061(2) Uani d . 1 1
H H5A 1.0945 0.2540 0.9067 0.073 Uiso calc R 1 1
H H5B 1.0254 0.2818 1.0147 0.073 Uiso calc R 1 1
N N6 0.9483(9) -0.0180(8) 0.7813(7) 0.064(2) Uani d . 1 1
H H6A 1.0112 0.0134 0.7435 0.076 Uiso calc R 1 1
H H6B 0.8894 -0.1120 0.7475 0.076 Uiso calc R 1 1
O O1W 0.7341(7) 0.3408(9) 0.9023(6) 0.074(2) Uani d . 1 1
O O2WA 0.2417(12) 0.2587(12) 0.7880(10) 0.082(4) Uiso d P 0.703(17) 1
O O2WB 0.063(5) 0.108(5) 0.631(5) 0.18(2) Uiso d P 0.297(17) 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 V1 O2 . . 102.7(2)
O1 V1 O5 . . 99.0(2)
O2 V1 O5 . . 93.43(17)
O1 V1 O4 . . 98.6(2)
O2 V1 O4 . . 90.70(17)
O5 V1 O4 . . 160.49(18)
O1 V1 O6 . . 99.5(2)
O2 V1 O6 . . 157.65(18)
O5 V1 O6 . . 84.99(16)
O4 V1 O6 . . 83.98(16)
O1 V1 O3 . . 178.9(2)
O2 V1 O3 . . 77.34(16)
O5 V1 O3 . . 82.06(15)
O4 V1 O3 . . 80.26(15)
O6 V1 O3 . . 80.37(15)
O8 V2 O2 . . 99.5(2)
O8 V2 O9 . . 100.3(2)
O2 V2 O9 . . 87.28(16)
O8 V2 O7 . . 96.9(2)
O2 V2 O7 . . 163.55(18)
O9 V2 O7 . . 88.82(16)
O8 V2 O10 . . 97.8(2)
O2 V2 O10 . . 87.81(16)
O9 V2 O10 . . 161.83(17)
O7 V2 O10 . . 90.97(17)
O8 V2 O3 . . 175.3(2)
O2 V2 O3 . . 76.60(15)
O9 V2 O3 . . 82.29(15)
O7 V2 O3 . . 87.04(16)
O10 V2 O3 . . 79.55(16)
O6 As1 O7 . 2_566 122.0(2)
O6 As1 O12 . . 111.2(2)
O7 As1 O12 2_566 . 102.3(2)
O6 As1 O11 . . 103.8(2)
O7 As1 O11 2_566 . 110.7(2)
O12 As1 O11 . . 106.1(2)
O3 As2 O9 2_566 . 114.15(19)
O3 As2 O5 2_566 . 112.86(19)
O9 As2 O5 . . 112.62(19)
O3 As2 O15 2_566 . 108.9(2)
O9 As2 O15 . . 103.6(2)
O5 As2 O15 . . 103.63(19)
O13 As3 O10 . . 112.3(2)
O13 As3 O4 . . 109.0(2)
O10 As3 O4 . . 117.33(19)
O13 As3 O14 . . 108.5(2)
O10 As3 O14 . . 107.1(2)
O4 As3 O14 . . 101.8(2)
V1 O2 V2 . . 119.8(2)
As2 O3 V2 2_566 . 136.2(2)
As2 O3 V1 2_566 . 137.1(2)
V2 O3 V1 . . 86.10(14)
As3 O4 V1 . . 124.0(2)
As2 O5 V1 . . 121.6(2)
As1 O6 V1 . . 125.2(2)
As1 O7 V2 2_566 . 127.5(2)
As2 O9 V2 . . 122.6(2)
As3 O10 V2 . . 124.8(2)
As1 O12 H12 . . 112.3
As3 O14 H14 . . 122.9
As2 O15 H15 . . 109.3
N2 C1 N3 . . 120.6(6)
N2 C1 N1 . . 119.8(6)
N3 C1 N1 . . 119.5(7)
C1 N1 H1A . . 120.0
C1 N1 H1B . . 120.0
H1A N1 H1B . . 120.0
C1 N2 H2A . . 120.0
C1 N2 H2B . . 120.0
H2A N2 H2B . . 120.0
C1 N3 H3A . . 120.0
C1 N3 H3B . . 120.0
H3A N3 H3B . . 120.0
N6 C2 N5 . . 121.2(8)
N6 C2 N4 . . 120.1(7)
N5 C2 N4 . . 118.7(7)
C2 N4 H4A . . 120.0
C2 N4 H4B . . 120.0
H4A N4 H4B . . 120.0
C2 N5 H5A . . 120.0
C2 N5 H5B . . 120.0
H5A N5 H5B . . 120.0
C2 N6 H6A . . 120.0
C2 N6 H6B . . 120.0
H6A N6 H6B . . 120.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O1 . 1.591(4) y
V1 O2 . 1.723(4) y
V1 O5 . 1.963(4) y
V1 O4 . 1.992(4) y
V1 O6 . 2.029(4) y
V1 O3 . 2.376(4) y
V2 O8 . 1.603(5) y
V2 O2 . 1.934(4) y
V2 O9 . 2.006(4) y
V2 O7 . 2.015(4) y
V2 O10 . 2.027(4) y
V2 O3 . 2.260(4) y
As1 O6 . 1.649(4) ?
As1 O7 2_566 1.665(4) ?
As1 O12 . 1.708(4) ?
As1 O11 . 1.726(5) ?
As2 O3 2_566 1.671(4) ?
As2 O9 . 1.675(4) ?
As2 O5 . 1.683(4) ?
As2 O15 . 1.719(4) ?
As3 O13 . 1.669(4) ?
As3 O10 . 1.679(4) ?
As3 O4 . 1.687(4) ?
As3 O14 . 1.714(4) ?
O3 As2 2_566 1.671(4) ?
O7 As1 2_566 1.665(4) ?
O12 H12 . 0.9769 ?
O14 H14 . 0.9637 ?
O15 H15 . 0.9600 ?
C1 N2 . 1.304(9) ?
C1 N3 . 1.309(9) ?
C1 N1 . 1.330(8) ?
N1 H1A . 0.8600 ?
N1 H1B . 0.8600 ?
N2 H2A . 0.8600 ?
N2 H2B . 0.8600 ?
N3 H3A . 0.8600 ?
N3 H3B . 0.8600 ?
C2 N6 . 1.304(9) ?
C2 N5 . 1.313(9) ?
C2 N4 . 1.318(10) ?
N4 H4A . 0.8600 ?
N4 H4B . 0.8600 ?
N5 H5A . 0.8600 ?
N5 H5B . 0.8600 ?
N6 H6A . 0.8600 ?
N6 H6B . 0.8600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O12 H12 O4 2_666 0.98 1.72 2.678(5) 165
O14 H14 O13 2_677 0.96 1.66 2.579(6) 158
O15 H15 O13 2_566 0.96 1.67 2.619(6) 170
N1 H1B O13 1_545 0.86 2.26 3.056(8) 154
N1 H1A O6 1_545 0.86 2.18 3.007(7) 160
N2 H2A O15 1_655 0.86 2.20 3.042(8) 167
N2 H2B O11 1_545 0.86 2.44 3.210(8) 150
N2 H2B O1 2_656 0.86 2.47 3.040(8) 125
N3 H3A O9 1_655 0.86 2.05 2.895(7) 169
N3 H3B O1W . 0.86 2.20 2.984(10) 152
N4 H4A O12 2_656 0.86 2.30 3.089(9) 152
N4 H4B O10 2_667 0.86 2.48 3.230(9) 146
N5 H5A O2WA 1_655 0.86 2.14 2.959(13) 160
N5 H5B O7 2_667 0.86 2.19 2.963(8) 150
N6 H6B O12 2_656 0.86 2.37 3.140(9) 150
N6 H6B O5 2_656 0.86 2.45 3.022(7) 125
N6 H6A O2WB 1_655 0.86 2.01 2.78(5) 148
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O1 V1 O2 V2 . . -178.0(2)
O5 V1 O2 V2 . . -77.9(2)
O4 V1 O2 V2 . . 83.0(2)
O6 V1 O2 V2 . . 7.3(6)
O3 V1 O2 V2 . . 3.14(19)
O8 V2 O2 V1 . . 179.4(2)
O9 V2 O2 V1 . . 79.4(2)
O7 V2 O2 V1 . . 2.9(7)
O10 V2 O2 V1 . . -83.1(2)
O3 V2 O2 V1 . . -3.3(2)
O8 V2 O3 As2 . 2_566 -152(2)
O2 V2 O3 As2 . 2_566 173.8(3)
O9 V2 O3 As2 . 2_566 84.8(3)
O7 V2 O3 As2 . 2_566 -4.4(3)
O10 V2 O3 As2 . 2_566 -95.9(3)
O8 V2 O3 V1 . . 37(3)
O2 V2 O3 V1 . . 2.09(13)
O9 V2 O3 V1 . . -86.94(14)
O7 V2 O3 V1 . . -176.15(14)
O10 V2 O3 V1 . . 92.32(15)
O1 V1 O3 As2 . 2_566 91(11)
O2 V1 O3 As2 . 2_566 -174.0(3)
O5 V1 O3 As2 . 2_566 -78.6(3)
O4 V1 O3 As2 . 2_566 93.1(3)
O6 V1 O3 As2 . 2_566 7.6(3)
O1 V1 O3 V2 . . -97(10)
O2 V1 O3 V2 . . -2.33(14)
O5 V1 O3 V2 . . 93.02(15)
O4 V1 O3 V2 . . -95.27(15)
O6 V1 O3 V2 . . 179.25(15)
O13 As3 O4 V1 . . -112.7(3)
O10 As3 O4 V1 . . 16.3(4)
O14 As3 O4 V1 . . 132.8(3)
O1 V1 O4 As3 . . -142.3(3)
O2 V1 O4 As3 . . -39.3(3)
O5 V1 O4 As3 . . 63.0(6)
O6 V1 O4 As3 . . 118.9(3)
O3 V1 O4 As3 . . 37.7(3)
O3 As2 O5 V1 2_566 . 92.3(3)
O9 As2 O5 V1 . . -38.8(3)
O15 As2 O5 V1 . . -150.1(3)
O1 V1 O5 As2 . . 152.3(3)
O2 V1 O5 As2 . . 48.8(3)
O4 V1 O5 As2 . . -53.1(6)
O6 V1 O5 As2 . . -108.9(3)
O3 V1 O5 As2 . . -27.9(2)
O7 As1 O6 V1 2_566 . 67.3(3)
O12 As1 O6 V1 . . -53.5(3)
O11 As1 O6 V1 . . -167.1(3)
O1 V1 O6 As1 . . 73.3(3)
O2 V1 O6 As1 . . -111.9(4)
O5 V1 O6 As1 . . -25.0(3)
O4 V1 O6 As1 . . 171.1(3)
O3 V1 O6 As1 . . -107.8(3)
O8 V2 O7 As1 . 2_566 -88.3(3)
O2 V2 O7 As1 . 2_566 88.2(6)
O9 V2 O7 As1 . 2_566 12.0(3)
O10 V2 O7 As1 . 2_566 173.8(3)
O3 V2 O7 As1 . 2_566 94.3(3)
O3 As2 O9 V2 2_566 . -85.4(3)
O5 As2 O9 V2 . . 45.0(3)
O15 As2 O9 V2 . . 156.3(2)
O8 V2 O9 As2 . . -153.2(3)
O2 V2 O9 As2 . . -54.0(3)
O7 V2 O9 As2 . . 110.0(3)
O10 V2 O9 As2 . . 20.5(7)
O3 V2 O9 As2 . . 22.8(2)
O13 As3 O10 V2 . . 109.2(3)
O4 As3 O10 V2 . . -18.1(4)
O14 As3 O10 V2 . . -131.8(3)
O8 V2 O10 As3 . . 137.6(3)
O2 V2 O10 As3 . . 38.3(3)
O9 V2 O10 As3 . . -36.1(7)
O7 V2 O10 As3 . . -125.3(3)
O3 V2 O10 As3 . . -38.5(3)
