#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:54:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179160 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/21/4312179.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4312179
loop_
_publ_author_name
'Philip L.W. Tregenna-Piggott'
'David Spichiger'
'Graham Carver'
'Beatrice Frey'
'Roland Meier'
'Høgni Weihe'
'John A. Cowan'
'Garry J. McIntyre'
'Gernot Zahn'
'Anne-Laure Barra'
_publ_contact_author
;
Philip L.W. Tregenna-Piggott
Department of Chemistry and Biochemistry
University of Bern 
Freiestrasse 3 
CH-3000 Bern 9
Switzerland
;
_publ_contact_author_email       tregenna@iac.unibe.ch
_publ_contact_author_fax         '+41 31 631 4322'
_publ_contact_author_phone       '+41 31 631 4317'
_publ_section_title
;
 Structure and Bonding of the Vanadium(III) Hexa-Aqua Cation. 1.
 Experimental Characterization and Ligand-Field Analysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8049
_journal_page_last               8060
_journal_paper_doi               10.1021/ic049292l
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C H18 N3 O14 S2 V'
_chemical_formula_weight         411.24
_chemical_name_systematic
; 
Guanidinium Hexaaqua Vanadium Disulphate 
;
_space_group_IT_number           157
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2'
_symmetry_space_group_name_H-M   'P 3 1 m'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.8116(4)
_cell_length_b                   11.8116(4)
_cell_length_c                   9.0311(3)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      33.73
_cell_measurement_theta_min      1.99
_cell_volume                     1091.16(6)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-7 with Mercury CCD'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15473
_diffrn_reflns_theta_full        30.98
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7687
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_coef       0.016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.2500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                2444
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049292lsi20040531_020941.cif
_cod_data_source_block           ghvs
_cod_database_code               4312179
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.0000 0.0000 0.54035(10) 0.01874(13) Uani 1 1 a d S . .
O1 O 0.0000 0.1398(2) 0.4180(3) 0.0308(4) Uani 1 3 c d SD . .
H1O H -0.0672(12) 0.132(3) 0.373(3) 0.056(10) Uiso 1 6 d d D . .
O2 O 0.0000 -0.13915(19) 0.6652(3) 0.0305(4) Uani 1 3 c d SD . .
H2O H -0.0679(12) -0.208(2) 0.691(4) 0.087(14) Uiso 1 6 d d D . .
V2 V 0.3333 0.6667 0.47616(7) 0.02052(12) Uani 1 2 b d S . .
O3 O 0.46875(16) 0.65963(14) 0.35253(19) 0.0318(4) Uani 1 6 d d D . .
H3O H 0.464(2) 0.5913(17) 0.316(3) 0.036(7) Uiso 1 6 d d D . .
H3P H 0.5363(19) 0.7271(16) 0.323(3) 0.032(6) Uiso 1 6 d d D . .
O4 O 0.47606(17) 0.80205(16) 0.59956(18) 0.0313(3) Uani 1 6 d d D . .
H4O H 0.534(2) 0.795(3) 0.644(3) 0.044(8) Uiso 1 6 d d D . .
H4P H 0.472(3) 0.867(2) 0.628(4) 0.053(9) Uiso 1 6 d d D . .
S1 S 0.34947(5) 0.0000 0.78436(3) 0.02238(12) Uani 1 3 c d S . .
O5 O 0.34288(15) 0.11743(16) 0.7457(2) 0.0330(3) Uani 1 6 d d . . .
O6 O 0.45564(18) 0.0000 0.6970(3) 0.0332(5) Uani 1 3 c d S . .
O7 O 0.3751(2) 0.0000 0.9409(3) 0.0467(5) Uani 1 3 c d S . .
S2 S 0.0000 0.68351(5) 0.21564(3) 0.02165(12) Uani 1 3 c d S . .
O8 O -0.11773(16) 0.67528(15) 0.2848(2) 0.0339(3) Uani 1 6 d d . . .
O9 O 0.0000 0.55954(17) 0.2406(2) 0.0288(4) Uani 1 3 c d S . .
O10 O 0.0000 0.70731(19) 0.0576(2) 0.0387(5) Uani 1 3 c d S . .
C1 C 0.0000 1.0000 0.0231(5) 0.0233(7) Uani 1 1 a d S . .
N1 N -0.1120(2) 0.8880(2) 0.0232(3) 0.0321(5) Uani 1 3 c d SD . .
H1N H -0.1828(18) 0.8920(14) 0.015(3) 0.031(7) Uiso 1 6 d d D . .
C2 C 0.3333 0.6667 0.9789(3) 0.0253(5) Uani 1 2 b d SD . .
N2 N 0.4407(2) 0.7817(2) 0.9774(3) 0.0465(5) Uani 1 6 d d D . .
H2N H 0.433(2) 0.8510(18) 0.978(5) 0.094(11) Uiso 1 6 d d D . .
H2M H 0.5148(18) 0.783(2) 0.985(5) 0.094(11) Uiso 1 6 d d D . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O1 92.06(10) 2 . ?
O1 V1 O1 92.06(10) 2 3 ?
O1 V1 O1 92.06(10) . 3 ?
O1 V1 O2 179.33(12) 2 2 ?
O1 V1 O2 88.40(6) . 2 ?
O1 V1 O2 88.40(6) 3 2 ?
O1 V1 O2 88.40(6) 2 3 ?
O1 V1 O2 88.40(6) . 3 ?
O1 V1 O2 179.33(11) 3 3 ?
O2 V1 O2 91.13(10) 2 3 ?
O1 V1 O2 88.40(6) 2 . ?
O1 V1 O2 179.33(11) . . ?
O1 V1 O2 88.40(6) 3 . ?
O2 V1 O2 91.13(10) 2 . ?
O2 V1 O2 91.13(10) 3 . ?
V1 O1 H1O 124.4(15) . . ?
V1 O2 H2O 124.0(16) . . ?
O3 V2 O3 91.49(7) 2_665 3_565 ?
O3 V2 O3 91.49(7) 2_665 . ?
O3 V2 O3 91.49(7) 3_565 . ?
O3 V2 O4 88.40(7) 2_665 2_665 ?
O3 V2 O4 88.52(7) 3_565 2_665 ?
O3 V2 O4 179.88(8) . 2_665 ?
O3 V2 O4 88.52(7) 2_665 . ?
O3 V2 O4 179.88(8) 3_565 . ?
O3 V2 O4 88.40(7) . . ?
O4 V2 O4 91.59(8) 2_665 . ?
O3 V2 O4 179.88(9) 2_665 3_565 ?
O3 V2 O4 88.40(7) 3_565 3_565 ?
O3 V2 O4 88.52(7) . 3_565 ?
O4 V2 O4 91.59(8) 2_665 3_565 ?
O4 V2 O4 91.59(8) . 3_565 ?
V2 O3 H3O 126.3(16) . . ?
V2 O3 H3P 122.6(15) . . ?
H3O O3 H3P 111(2) . . ?
V2 O4 H4O 126.4(18) . . ?
V2 O4 H4P 119.7(19) . . ?
H4O O4 H4P 112(2) . . ?
O7 S1 O5 110.01(10) . 5 ?
O7 S1 O5 110.01(10) . . ?
O5 S1 O5 109.64(13) 5 . ?
O7 S1 O6 110.11(16) . . ?
O5 S1 O6 108.52(9) 5 . ?
O5 S1 O6 108.52(9) . . ?
O10 S2 O9 109.89(13) . . ?
O10 S2 O8 109.61(9) . 6 ?
O9 S2 O8 109.54(8) . 6 ?
O10 S2 O8 109.61(9) . . ?
O9 S2 O8 109.54(8) . . ?
O8 S2 O8 108.62(13) 6 . ?
N1 C1 N1 120.000(2) 3_465 . ?
N1 C1 N1 120.000(2) 3_465 2_675 ?
N1 C1 N1 120.000(1) . 2_675 ?
C1 N1 H1N 117.2(10) . . ?
N2 C2 N2 119.990(7) 2_665 . ?
N2 C2 N2 119.990(9) 2_665 3_565 ?
N2 C2 N2 119.990(8) . 3_565 ?
C2 N2 H2N 118.4(14) . . ?
C2 N2 H2M 117.2(13) . . ?
H2N N2 H2M 124(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.987(2) 2 ?
V1 O1 1.987(2) . ?
V1 O1 1.987(2) 3 ?
V1 O2 1.993(2) 2 ?
V1 O2 1.993(2) 3 ?
V1 O2 1.993(2) . ?
O1 H1O 0.857(16) . ?
O2 H2O 0.839(16) . ?
V2 O3 1.9861(16) 2_665 ?
V2 O3 1.9861(16) 3_565 ?
V2 O3 1.9861(16) . ?
V2 O4 1.9863(16) 2_665 ?
V2 O4 1.9863(16) . ?
V2 O4 1.9863(16) 3_565 ?
O3 H3O 0.850(15) . ?
O3 H3P 0.840(16) . ?
O4 H4O 0.837(16) . ?
O4 H4P 0.836(16) . ?
S1 O7 1.446(3) . ?
S1 O5 1.4696(17) 5 ?
S1 O5 1.4696(17) . ?
S1 O6 1.482(2) . ?
S2 O10 1.455(2) . ?
S2 O9 1.482(2) . ?
S2 O8 1.4829(17) 6 ?
S2 O8 1.4829(17) . ?
C1 N1 1.323(2) 3_465 ?
C1 N1 1.323(2) . ?
C1 N1 1.323(2) 2_675 ?
N1 H1N 0.864(16) . ?
C2 N2 1.316(2) 2_665 ?
C2 N2 1.316(2) . ?
C2 N2 1.316(2) 3_565 ?
N2 H2N 0.866(18) . ?
N2 H2M 0.872(17) . ?
