#------------------------------------------------------------------------------
#$Date: 2017-02-04 14:47:11 +0100 (Sat 04 de Feb de 2017) $
#$Revision: 191582 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/13/7041372.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_7041372
loop_
_publ_author_name
'Nachtigall, Olaf'
'Hagenbach, Adelheid'
'Wiecko, Jelena'
'Lentz, Dieter'
'Abram, Ulrich'
'Spandl, Johann'
_publ_section_title
;
 Functional polyoxometalates from solvothermal reactions of VOSO4 with
 tripodal alkoxides - a study on the reactivity of different
 "tris" derivatives.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              509
_journal_page_last               516
_journal_paper_doi               10.1039/c6dt03638d
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C28 H52 N4 O20 S2 V4, 4 (O C H4), 2 (H2 O)'
_chemical_formula_sum            'C32 H72 N4 O26 S2 V4'
_chemical_formula_weight         1196.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-07 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                92.030(10)
_cell_angle_beta                 110.130(10)
_cell_angle_gamma                107.540(10)
_cell_formula_units_Z            1
_cell_length_a                   10.670(2)
_cell_length_b                   11.411(2)
_cell_length_c                   11.905(2)
_cell_measurement_reflns_used    14849
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      3.31
_cell_volume                     1281.9(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2007)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14956
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.291
_diffrn_reflns_theta_min         3.320
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  0.8682
_exptl_absorpt_correction_T_min  0.5892
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0570P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3476
_reflns_number_total             6854
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt03638d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7041370--7041376.cif.'
_cod_database_code               7041372
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
O6 O 0.2209(3) 0.0178(2) 0.4843(2) 0.0414(6) Uani 1 1 d . .
O5 O 0.0904(3) 0.1305(3) 0.2974(2) 0.0488(7) Uani 1 1 d . .
O3 O 0.0530(3) 0.1221(2) 0.5217(2) 0.0411(6) Uani 1 1 d . .
O2 O 0.3347(3) 0.2802(3) 0.5518(3) 0.0500(7) Uani 1 1 d . .
O1 O 0.4324(3) 0.1308(3) 0.7080(2) 0.0517(7) Uani 1 1 d . .
O4 O 0.1697(3) -0.0077(2) 0.6941(2) 0.0406(6) Uani 1 1 d . .
N11 N -0.2288(4) 0.1051(4) -0.0778(3) 0.0533(9) Uani 1 1 d . .
C23 C -0.3372(5) 0.0906(5) -0.0208(4) 0.0695(14) Uani 1 1 d . .
H23A H -0.3074 0.1617 0.0396 0.104 Uiso 1 1 calc R U
H23B H -0.4267 0.0841 -0.0819 0.104 Uiso 1 1 calc R U
H23C H -0.3468 0.0168 0.0163 0.104 Uiso 1 1 calc R U
C20 C -0.2132(5) 0.2208(5) -0.1346(4) 0.0613(12) Uani 1 1 d . .
H20A H -0.1831 0.2915 -0.0737 0.092 Uiso 1 1 calc R U
H20B H -0.1439 0.2302 -0.1710 0.092 Uiso 1 1 calc R U
H20C H -0.3025 0.2150 -0.1956 0.092 Uiso 1 1 calc R U
C22 C -0.2753(6) -0.0048(5) -0.1709(5) 0.0761(15) Uani 1 1 d . .
H22A H -0.3646 -0.0110 -0.2321 0.114 Uiso 1 1 calc R U
H22B H -0.2060 0.0039 -0.2072 0.114 Uiso 1 1 calc R U
H22C H -0.2854 -0.0787 -0.1337 0.114 Uiso 1 1 calc R U
C21 C -0.0901(5) 0.1161(5) 0.0181(4) 0.0720(14) Uani 1 1 d . .
H21A H -0.0610 0.1875 0.0778 0.108 Uiso 1 1 calc R U
H21B H -0.0997 0.0426 0.0558 0.108 Uiso 1 1 calc R U
H21C H -0.0203 0.1252 -0.0177 0.108 Uiso 1 1 calc R U
O30 O 0.5020(4) 0.2615(5) 0.0512(4) 0.0931(13) Uani 1 1 d . .
H30 H 0.4155 0.2421 0.0219 0.140 Uiso 1 1 calc R U
C4 C 0.2024(4) -0.3021(4) 0.5639(4) 0.0468(9) Uani 1 1 d . .
C2 C 0.2453(4) -0.0978(4) 0.4937(4) 0.0471(9) Uani 1 1 d . .
H2A H 0.3459 -0.0819 0.5355 0.056 Uiso 1 1 calc R U
H2B H 0.2179 -0.1411 0.4128 0.056 Uiso 1 1 calc R U
C5 C 0.1648(5) -0.3795(4) 0.4560(4) 0.0528(10) Uani 1 1 d . .
H5 H 0.1137 -0.3601 0.3828 0.063 Uiso 1 1 calc R U
C3 C 0.1633(4) -0.1833(4) 0.5618(3) 0.0444(9) Uani 1 1 d . .
C6 C 0.2027(5) -0.4839(4) 0.4573(4) 0.0564(11) Uani 1 1 d . .
H6 H 0.1751 -0.5346 0.3842 0.068 Uiso 1 1 calc R U
N1 N 0.2783(4) -0.5166(3) 0.5600(3) 0.0539(9) Uani 1 1 d . .
C8 C 0.2803(5) -0.3366(4) 0.6689(4) 0.0563(11) Uani 1 1 d . .
H8 H 0.3099 -0.2877 0.7434 0.068 Uiso 1 1 calc R U
C7 C 0.3139(5) -0.4443(4) 0.6624(4) 0.0605(12) Uani 1 1 d . .
H7 H 0.3643 -0.4666 0.7341 0.073 Uiso 1 1 calc R U
O31 O 0.1676(5) 0.4364(5) 1.0841(4) 0.0989(13) Uani 1 1 d . .
H31 H 0.1601 0.4111 1.0159 0.148 Uiso 1 1 calc R U
C30 C 0.2788(7) 0.4086(8) 1.1709(5) 0.109(2) Uani 1 1 d . .
H30A H 0.3326 0.3820 1.1315 0.163 Uiso 1 1 calc R U
H30B H 0.2403 0.3433 1.2106 0.163 Uiso 1 1 calc R U
H30C H 0.3392 0.4814 1.2296 0.163 Uiso 1 1 calc R U
C31 C 0.5633(6) 0.3578(6) -0.0056(6) 0.102(2) Uani 1 1 d . .
H31A H 0.5559 0.3228 -0.0831 0.153 Uiso 1 1 calc R U
H31B H 0.6613 0.3986 0.0442 0.153 Uiso 1 1 calc R U
H31C H 0.5142 0.4170 -0.0163 0.153 Uiso 1 1 calc R U
C40 C 0.4254(5) 0.2885(5) 0.4864(5) 0.0683(13) Uani 1 1 d . .
H40A H 0.4385 0.3650 0.4538 0.102 Uiso 1 1 calc R U
H40B H 0.5154 0.2864 0.5398 0.102 Uiso 1 1 calc R U
H40C H 0.3835 0.2196 0.4216 0.102 Uiso 1 1 calc R U
C9 C 0.2047(4) -0.1181(4) 0.6915(3) 0.0445(9) Uani 1 1 d . .
H9A H 0.1570 -0.1753 0.7339 0.053 Uiso 1 1 calc R U
H9B H 0.3059 -0.0977 0.7343 0.053 Uiso 1 1 calc R U
H2 H 0.323(4) 0.352(4) 0.559(4) 0.051(13) Uiso 1 1 d . .
V1 V 0.27736(7) 0.13450(7) 0.63643(6) 0.04203(18) Uani 1 1 d . .
V2 V 0.03475(7) 0.02527(7) 0.37065(6) 0.04130(18) Uani 1 1 d . .
S1 S 0.15073(11) 0.22841(10) 0.81908(9) 0.0459(2) Uani 1 1 d . .
O21 O 0.2472(3) 0.2511(3) 0.7494(2) 0.0447(6) Uani 1 1 d . .
O22 O -0.0121(3) -0.1330(3) 0.2579(2) 0.0462(6) Uani 1 1 d . .
O23 O 0.2132(3) 0.1833(3) 0.9306(2) 0.0602(8) Uani 1 1 d . .
O24 O 0.1256(3) 0.3430(3) 0.8424(3) 0.0576(8) Uani 1 1 d . .
C1 C 0.0006(4) -0.2240(4) 0.4969(3) 0.0434(9) Uani 1 1 d . .
H1A H -0.0265 -0.2732 0.4189 0.052 Uiso 1 1 calc R U
H1B H -0.0435 -0.2768 0.5444 0.052 Uiso 1 1 calc R U
O90 O -0.0545(5) 0.4175(4) 0.1683(4) 0.0997(13) Uani 1 1 d . .
H90A H 0.0103 0.4260 0.1382 0.150 Uiso 1 1 d . U
H90B H -0.0593 0.4915 0.1778 0.150 Uiso 1 1 d . U
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'
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 O6 V1 118.8(2) . .
C2 O6 V2 120.3(2) . .
V1 O6 V2 106.98(11) . .
C1 O3 V2 114.8(2) 2_556 .
C1 O3 V1 126.2(2) 2_556 .
V2 O3 V1 98.08(10) . .
C1 O3 V2 117.8(2) 2_556 2_556
V2 O3 V2 105.37(11) . 2_556
V1 O3 V2 90.18(9) . 2_556
C40 O2 V1 123.4(3) . .
C9 O4 V1 116.8(2) . .
C9 O4 V2 117.4(2) . 2_556
V1 O4 V2 109.84(12) . 2_556
C22 N11 C21 110.2(4) . .
C22 N11 C20 110.0(4) . .
C21 N11 C20 109.0(4) . .
C22 N11 C23 109.3(4) . .
C21 N11 C23 109.0(3) . .
C20 N11 C23 109.4(4) . .
C8 C4 C5 116.3(4) . .
C8 C4 C3 123.6(4) . .
C5 C4 C3 120.1(4) . .
O6 C2 C3 113.5(3) . .
C6 C5 C4 120.2(4) . .
C4 C3 C9 111.1(3) . .
C4 C3 C1 106.5(3) . .
C9 C3 C1 108.8(3) . .
C4 C3 C2 106.5(3) . .
C9 C3 C2 110.5(3) . .
C1 C3 C2 113.4(3) . .
N1 C6 C5 122.9(4) . .
C7 N1 C6 117.3(4) . .
C7 C8 C4 119.8(4) . .
N1 C7 C8 123.4(4) . .
O4 C9 C3 113.1(3) . .
O1 V1 O4 98.33(13) . .
O1 V1 O6 100.50(12) . .
O4 V1 O6 87.01(10) . .
O1 V1 O2 97.05(14) . .
O4 V1 O2 164.61(11) . .
O6 V1 O2 89.69(12) . .
O1 V1 O21 104.71(13) . .
O4 V1 O21 88.71(10) . .
O6 V1 O21 154.78(11) . .
O2 V1 O21 87.90(12) . .
O1 V1 O3 174.09(13) . .
O4 V1 O3 80.08(10) . .
O6 V1 O3 73.78(9) . .
O2 V1 O3 84.56(11) . .
O21 V1 O3 81.00(10) . .
O5 V2 O4 99.19(12) . 2_556
O5 V2 O3 103.51(13) . .
O4 V2 O3 87.83(10) 2_556 .
O5 V2 O6 99.81(12) . .
O4 V2 O6 159.35(10) 2_556 .
O3 V2 O6 79.93(10) . .
O5 V2 O22 101.80(12) . .
O4 V2 O22 88.99(10) 2_556 .
O3 V2 O22 154.67(11) . .
O6 V2 O22 94.98(11) . .
O5 V2 O3 177.17(12) . 2_556
O4 V2 O3 78.68(10) 2_556 2_556
O3 V2 O3 74.64(11) . 2_556
O6 V2 O3 82.05(10) . 2_556
O22 V2 O3 80.10(10) . 2_556
O24 S1 O23 111.86(19) . .
O24 S1 O22 108.20(17) . 2_556
O23 S1 O22 109.62(18) . 2_556
O24 S1 O21 108.57(17) . .
O23 S1 O21 110.03(16) . .
O22 S1 O21 108.48(15) 2_556 .
S1 O21 V1 131.84(17) . .
S1 O22 V2 131.46(16) 2_556 .
O3 C1 C3 113.8(3) 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O6 C2 1.421(5) .
O6 V1 2.003(3) .
O6 V2 2.011(3) .
O5 V2 1.599(3) .
O3 C1 1.435(4) 2_556
O3 V2 1.995(3) .
O3 V1 2.269(3) .
O3 V2 2.318(3) 2_556
O2 C40 1.421(5) .
O2 V1 2.020(3) .
O1 V1 1.594(3) .
O4 C9 1.420(5) .
O4 V1 1.980(3) .
O4 V2 1.990(3) 2_556
N11 C22 1.482(6) .
N11 C21 1.492(5) .
N11 C20 1.495(6) .
N11 C23 1.503(5) .
O30 C31 1.420(7) .
C4 C8 1.387(6) .
C4 C5 1.394(6) .
C4 C3 1.533(6) .
C2 C3 1.551(5) .
C5 C6 1.368(6) .
C3 C9 1.544(5) .
C3 C1 1.547(5) .
C6 N1 1.349(5) .
N1 C7 1.316(6) .
C8 C7 1.387(6) .
O31 C30 1.409(7) .
V1 O21 2.027(3) .
V2 O4 1.990(3) 2_556
V2 O22 2.034(3) .
V2 O3 2.318(3) 2_556
S1 O24 1.447(3) .
S1 O23 1.456(3) .
S1 O22 1.496(3) 2_556
S1 O21 1.503(3) .
O22 S1 1.496(3) 2_556
C1 O3 1.435(4) 2_556
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O30 H30 O23 0.82 1.94 2.750(5) 170.9 1_554
O30 H30 S1 0.82 2.97 3.711(4) 150.7 1_554
O31 H31 O24 0.82 2.05 2.867(5) 175.8 .
O2 H2 N1 0.87(5) 1.71(5) 2.571(5) 172(4) 1_565
C23 H23A O30 0.96 2.65 3.223(7) 118.6 1_455
C23 H23B O1 0.96 2.61 3.464(6) 149.0 1_454
C20 H20C O1 0.96 2.51 3.393(5) 153.2 1_454
C22 H22B O5 0.96 2.64 3.438(6) 140.9 2
C22 H22B O22 0.96 2.63 3.513(6) 153.3 2
C21 H21B O23 0.96 2.53 3.429(7) 155.4 2_556
O30 H30 S1 0.82 2.97 3.711(4) 150.7 1_554
O30 H30 O23 0.82 1.94 2.750(5) 170.9 1_554
C2 H2B O22 0.97 2.54 3.088(5) 115.5 .
C8 H8 O30 0.93 2.51 3.241(6) 135.6 2_656
O31 H31 O24 0.82 2.05 2.867(5) 175.8 .
O2 H2 N1 0.87(5) 1.71(5) 2.571(5) 172(4) 1_565
C1 H1A S1 0.97 2.82 3.538(4) 131.1 2_556
C1 H1A O21 0.97 2.60 3.129(5) 114.3 2_556
C1 H1A O22 0.97 2.56 3.037(5) 110.7 .
O90 H90A O31 0.87 1.97 2.830(6) 173.8 1_554
O90 H90B O24 0.87 2.20 3.044(5) 164.2 2_566
