#------------------------------------------------------------------------------
#$Date: 2019-10-28 09:23:29 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/20/15/2201513.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_2201513
loop_
_publ_author_name
'Bremner, Colin A.'
'Harrison, William T. A.'
_publ_section_title
;
 Bis(dabconium) vanadium arsenate octahydrate,
 (N₂C₆H₁₄)₂[V₄As₆O₃₀H₆]·8H₂O
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m319
_journal_page_last               m321
_journal_paper_doi               10.1107/S1600536802009546
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C6 H14 N2)2 [V4 As6 O30 H6], 8H2 O'
_chemical_formula_moiety         '(C6 H14 N2)2, V4 As6 O30 H6, 8H2 O'
_chemical_formula_sum            'C12 H50 As6 N4 O38 V4'
_chemical_formula_weight         1511.82
_chemical_melting_point          'decomposes before melting'
_chemical_name_systematic        ?
_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                94.546(2)
_cell_angle_beta                 101.557(2)
_cell_angle_gamma                114.193(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6824(5)
_cell_length_b                   11.0733(7)
_cell_length_c                   11.8967(7)
_cell_measurement_reflns_used    3766
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.05
_cell_volume                     1121.17(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SMART
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7764
_diffrn_reflns_theta_full        30.21
_diffrn_reflns_theta_max         30.21
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.316
_exptl_absorpt_correction_T_max  0.225
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.818
_refine_ls_extinction_coef       0.0025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         6021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0277
_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/[σ²(Fo²)+(0.0410P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                4987
_reflns_number_total             6021
_reflns_threshold_expression     I>2σ()'
_cod_data_source_file            mg6010.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

2019-10-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H25 As3 N2 O19 V2'
_cod_original_formula_weight         755.91
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1121.16(11)
_cod_database_code               2201513
_cod_database_fobs_code          2201513
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
V1 0.65452(5) 0.77980(4) 0.61404(4) 0.02073(10) Uani d . 1 . . V
V2 0.58641(5) 0.54350(4) 0.76000(4) 0.02084(10) Uani d . 1 . . V
As1 0.58581(3) 0.78147(2) 0.33273(2) 0.01968(7) Uani d . 1 . . As
As2 0.66837(3) 0.48861(2) 0.47031(2) 0.01778(7) Uani d . 1 . . As
As3 0.94147(3) 0.73424(3) 0.76272(2) 0.02442(8) Uani d . 1 . . As
O1 0.6256(2) 0.53455(17) 0.34055(15) 0.0209(4) Uani d . 1 . . O
O2 0.5701(2) 0.31980(17) 0.45954(16) 0.0211(4) Uani d . 1 . . O
O3 0.4199(2) 0.63745(17) 0.28393(17) 0.0235(4) Uani d . 1 . . O
O4 0.6037(2) 0.70664(17) 0.74747(16) 0.0230(4) Uani d . 1 . . O
O5 0.6480(2) 0.57482(17) 0.58194(15) 0.0196(3) Uani d . 1 . . O
O6 0.8654(2) 0.83099(18) 0.69252(17) 0.0263(4) Uani d . 1 . . O
O7 0.6980(2) 0.8180(2) 0.24049(18) 0.0290(4) Uani d . 1 . . O
O8 0.6959(2) 0.78996(18) 0.46561(16) 0.0244(4) Uani d . 1 . . O
O9 0.8594(2) 0.5176(2) 0.49243(18) 0.0294(4) Uani d . 1 . . O
H9 0.9168 0.5761 0.5676 0.035 Uiso d R 1 . . H
O10 1.0341(2) 0.6813(2) 0.68360(19) 0.0335(5) Uani d . 1 . . O
O11 0.5100(2) 0.89555(19) 0.34370(19) 0.0310(5) Uani d . 1 . . O
H11 0.5748 0.9812 0.3498 0.037 Uiso d R 1 . . H
O12 0.5439(2) 0.5250(2) 0.88139(17) 0.0332(5) Uani d . 1 . . O
O13 0.8100(2) 0.60699(19) 0.81023(17) 0.0279(4) Uani d . 1 . . O
O14 0.6484(2) 0.91935(18) 0.64181(19) 0.0314(4) Uani d . 1 . . O
O15 1.0627(3) 0.8341(2) 0.89093(18) 0.0403(5) Uani d . 1 . . O
H15 1.1588 0.8800 0.8801 0.048 Uiso d R 1 . . H
O20 0.3350(3) 0.0102(2) 0.8958(2) 0.0419(6) Uani d . 1 . . O
H20 0.3254 0.0615 0.8419 0.050 Uiso d R 1 . . H
H21 0.3912 0.0609 0.9697 0.050 Uiso d R 1 . . H
O21 0.7046(3) 1.1523(2) 0.3799(3) 0.0637(9) Uani d . 1 . . O
H22 0.7948 1.1896 0.3628 0.063(13) Uiso d R 1 . . H
H23 0.6614 1.1983 0.4117 0.24(4) Uiso d R 1 . . H
O22 0.6954(3) 0.3441(3) 0.9789(2) 0.0537(7) Uani d . 1 . . O
H24 0.6056 0.3634 0.9487 0.064 Uiso d R 1 . . H
H25 0.6410 0.2866 1.0320 0.064 Uiso d R 1 . . H
O23 0.5113(3) 0.1620(3) 0.1110(2) 0.0545(7) Uani d . 1 . . O
H26 0.4721 0.2064 0.1586 0.065 Uiso d R 1 . . H
H27 0.5648 0.1337 0.1512 0.065 Uiso d R 1 . . H
N1 1.0736(3) 0.2422(2) 0.7741(2) 0.0288(5) Uani d . 1 . . N
H1 1.1529 0.2198 0.7688 0.035 Uiso calc R 1 . . H
N2 0.8561(3) 0.3017(3) 0.7871(3) 0.0387(6) Uani d . 1 . . N
H2 0.7766 0.3240 0.7923 0.046 Uiso calc R 1 . . H
C1 0.9750(4) 0.2232(4) 0.6545(3) 0.0415(8) Uani d . 1 . . C
H1A 0.9229 0.1285 0.6194 0.050 Uiso calc R 1 . . H
H1B 1.0401 0.2720 0.6059 0.050 Uiso calc R 1 . . H
C2 1.1409(4) 0.3838(3) 0.8336(3) 0.0425(8) Uani d . 1 . . C
H2A 1.1953 0.4434 0.7852 0.051 Uiso calc R 1 . . H
H2B 1.2153 0.3976 0.9069 0.051 Uiso calc R 1 . . H
C3 0.9752(4) 0.1522(3) 0.8428(3) 0.0386(7) Uani d . 1 . . C
H3A 1.0355 0.1692 0.9228 0.046 Uiso calc R 1 . . H
H3B 0.9418 0.0587 0.8096 0.046 Uiso calc R 1 . . H
C4 0.8543(4) 0.2755(5) 0.6636(3) 0.0559(11) Uani d . 1 . . C
H4A 0.8790 0.3578 0.6319 0.067 Uiso calc R 1 . . H
H4B 0.7511 0.2094 0.6193 0.067 Uiso calc R 1 . . H
C5 1.0080(4) 0.4143(4) 0.8557(5) 0.0620(13) Uani d . 1 . . C
H5A 1.0118 0.4225 0.9382 0.074 Uiso calc R 1 . . H
H5B 1.0179 0.4986 0.8317 0.074 Uiso calc R 1 . . H
C6 0.8341(4) 0.1795(3) 0.8397(3) 0.0342(7) Uani d . 1 . . C
H6A 0.7401 0.1030 0.7936 0.041 Uiso calc R 1 . . H
H6B 0.8225 0.1937 0.9181 0.041 Uiso calc R 1 . . H
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'
C C 0.0033 0.0016 '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'
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
_geom_angle_publ_flag
O14 V1 O6 . . 99.03(10) ?
O14 V1 O8 . . 99.98(10) ?
O6 V1 O8 . . 93.80(8) ?
O14 V1 O4 . . 100.12(10) ?
O6 V1 O4 . . 86.14(8) ?
O8 V1 O4 . . 159.65(8) ?
O14 V1 O2 . 2_666 94.53(9) ?
O6 V1 O2 . 2_666 164.97(8) ?
O8 V1 O2 . 2_666 90.22(8) ?
O4 V1 O2 . 2_666 85.09(8) ?
O14 V1 O5 . . 175.43(9) ?
O6 V1 O5 . . 83.30(7) ?
O8 V1 O5 . . 83.73(7) ?
O4 V1 O5 . . 76.04(7) ?
O2 V1 O5 2_666 . 82.74(7) ?
O12 V2 O4 . . 102.49(10) ?
O12 V2 O13 . . 99.81(10) ?
O4 V2 O13 . . 92.37(8) ?
O12 V2 O1 . 2_666 98.36(10) ?
O4 V2 O1 . 2_666 90.12(8) ?
O13 V2 O1 . 2_666 160.67(8) ?
O12 V2 O3 . 2_666 98.45(10) ?
O4 V2 O3 . 2_666 159.01(8) ?
O13 V2 O3 . 2_666 85.55(8) ?
O1 V2 O3 2_666 2_666 85.29(7) ?
O12 V2 O5 . . 178.77(9) ?
O4 V2 O5 . . 76.31(7) ?
O13 V2 O5 . . 80.52(7) ?
O1 V2 O5 2_666 . 81.46(7) ?
O3 V2 O5 2_666 . 82.75(7) ?
O7 As1 O3 . . 113.76(10) ?
O7 As1 O8 . . 108.98(10) ?
O3 As1 O8 . . 114.53(9) ?
O7 As1 O11 . . 109.71(10) ?
O3 As1 O11 . . 100.58(9) ?
O8 As1 O11 . . 108.86(10) ?
O5 As2 O1 . . 114.52(8) ?
O5 As2 O2 . . 112.76(8) ?
O1 As2 O2 . . 110.59(9) ?
O5 As2 O9 . . 109.41(9) ?
O1 As2 O9 . . 104.43(9) ?
O2 As2 O9 . . 104.27(9) ?
O10 As3 O13 . . 112.23(10) ?
O10 As3 O15 . . 112.17(11) ?
O13 As3 O15 . . 101.20(10) ?
O10 As3 O6 . . 111.22(10) ?
O13 As3 O6 . . 114.03(9) ?
O15 As3 O6 . . 105.38(11) ?
As2 O1 V2 . 2_666 122.07(9) yes
As2 O2 V1 . 2_666 122.51(10) yes
As1 O3 V2 . 2_666 124.36(10) yes
V2 O4 V1 . . 119.80(10) yes
As2 O5 V1 . . 133.04(9) yes
As2 O5 V2 . . 138.98(9) yes
V1 O5 V2 . . 87.86(6) yes
As3 O6 V1 . . 127.43(10) yes
As1 O8 V1 . . 132.74(11) yes
As2 O9 H9 . . 108.0 ?
As1 O11 H11 . . 117.0 ?
As3 O13 V2 . . 124.54(10) yes
As3 O15 H15 . . 108.6 ?
H20 O20 H21 . . 112.7 ?
H22 O21 H23 . . 123.9 ?
H24 O22 H25 . . 92.5 ?
H26 O23 H27 . . 109.8 ?
C2 N1 C1 . . 110.7(3) ?
C2 N1 C3 . . 109.7(2) ?
C1 N1 C3 . . 109.1(2) ?
C2 N1 H1 . . 109.1 ?
C1 N1 H1 . . 109.1 ?
C3 N1 H1 . . 109.1 ?
C4 N2 C6 . . 110.3(3) ?
C4 N2 C5 . . 111.4(3) ?
C6 N2 C5 . . 108.0(3) ?
C4 N2 H2 . . 109.0 ?
C6 N2 H2 . . 109.0 ?
C5 N2 H2 . . 109.0 ?
N1 C1 C4 . . 108.6(3) ?
N1 C1 H1A . . 110.0 ?
C4 C1 H1A . . 110.0 ?
N1 C1 H1B . . 110.0 ?
C4 C1 H1B . . 110.0 ?
H1A C1 H1B . . 108.4 ?
N1 C2 C5 . . 108.4(3) ?
N1 C2 H2A . . 110.0 ?
C5 C2 H2A . . 110.0 ?
N1 C2 H2B . . 110.0 ?
C5 C2 H2B . . 110.0 ?
H2A C2 H2B . . 108.4 ?
N1 C3 C6 . . 108.7(2) ?
N1 C3 H3A . . 110.0 ?
C6 C3 H3A . . 110.0 ?
N1 C3 H3B . . 110.0 ?
C6 C3 H3B . . 110.0 ?
H3A C3 H3B . . 108.3 ?
N2 C4 C1 . . 108.7(3) ?
N2 C4 H4A . . 110.0 ?
C1 C4 H4A . . 110.0 ?
N2 C4 H4B . . 110.0 ?
C1 C4 H4B . . 110.0 ?
H4A C4 H4B . . 108.3 ?
N2 C5 C2 . . 108.3(3) ?
N2 C5 H5A . . 110.0 ?
C2 C5 H5A . . 110.0 ?
N2 C5 H5B . . 110.0 ?
C2 C5 H5B . . 110.0 ?
H5A C5 H5B . . 108.4 ?
N2 C6 C3 . . 108.7(2) ?
N2 C6 H6A . . 109.9 ?
C3 C6 H6A . . 109.9 ?
N2 C6 H6B . . 109.9 ?
C3 C6 H6B . . 109.9 ?
H6A C6 H6B . . 108.3 ?
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 O14 . 1.5819(19) yes
V1 O6 . 1.8879(19) yes
V1 O8 . 1.8892(19) yes
V1 O4 . 1.8996(18) yes
V1 O2 2_666 1.9576(18) yes
V1 O5 . 2.2443(17) yes
V2 O12 . 1.585(2) yes
V2 O4 . 1.7661(18) yes
V2 O13 . 1.9252(19) yes
V2 O1 2_666 1.9469(18) yes
V2 O3 2_666 2.0029(19) yes
V2 O5 . 2.3272(18) yes
As1 O7 . 1.6539(18) yes
As1 O3 . 1.6852(18) yes
As1 O8 . 1.6920(18) yes
As1 O11 . 1.7098(19) yes
As2 O5 . 1.6651(17) yes
As2 O1 . 1.6894(17) yes
As2 O2 . 1.6945(17) yes
As2 O9 . 1.7027(18) yes
As3 O10 . 1.648(2) yes
As3 O13 . 1.6939(18) yes
As3 O15 . 1.696(2) yes
As3 O6 . 1.7120(19) yes
O9 H9 . 0.9702 ?
O11 H11 . 0.8835 ?
O15 H15 . 0.9009 ?
O20 H20 . 0.9059 ?
O20 H21 . 0.9298 ?
O21 H22 . 0.8739 ?
O21 H23 . 0.8855 ?
O22 H24 . 0.9850 ?
O22 H25 . 1.0018 ?
O23 H26 . 0.9503 ?
O23 H27 . 0.8070 ?
N1 C2 . 1.478(4) yes
N1 C1 . 1.491(4) yes
N1 C3 . 1.495(4) yes
N1 H1 . 0.9100 ?
N2 C4 . 1.470(5) yes
N2 C6 . 1.490(4) yes
N2 C5 . 1.496(5) yes
N2 H2 . 0.9100 ?
C1 C4 . 1.519(5) yes
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 C5 . 1.522(5) yes
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C6 . 1.510(5) yes
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
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
_geom_hbond_publ_flag
O9 H9 O10 . 0.97 1.61 2.571(3) 171.4 yes
O11 H11 O21 . 0.88 1.75 2.629(3) 173.1 yes
O15 H15 O20 1_665 0.90 1.68 2.542(3) 158.1 yes
O20 H20 O7 2_666 0.91 1.78 2.670(3) 168.4 yes
O20 H21 O23 1_556 0.93 1.81 2.740(4) 176.6 yes
O21 H22 O10 2_776 0.87 1.91 2.745(3) 159.5 yes
O21 H23 O2 1_565 0.89 1.99 2.868(3) 169.7 yes
O21 H23 O14 2_676 0.89 2.65 3.125(3) 115.1 yes
O22 H24 O12 . 0.99 2.26 3.100(3) 142.3 yes
O22 H25 O23 1_556 1.00 1.90 2.897(4) 170.8 yes
O23 H26 O4 2_666 0.95 1.86 2.808(3) 179.6 yes
O23 H27 O20 2_656 0.81 2.27 2.864(3) 131.3 yes
N1 H1 O7 2_766 0.91 1.68 2.591(3) 178.7 yes
N2 H2 O3 2_666 0.91 2.16 2.995(3) 152.2 yes
N2 H2 O22 . 0.91 2.52 3.114(4) 123.1 yes
