#------------------------------------------------------------------------------
#$Date: 2017-02-04 15:47:11 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191582 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/13/7041373.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_7041373
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         'C21 H52 N8 O21 S2 V4, O C H4'
_chemical_formula_sum            'C22 H56 N8 O22 S2 V4'
_chemical_formula_weight         1052.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8617(10)
_cell_length_b                   23.0313(14)
_cell_length_c                   10.4655(6)
_cell_measurement_reflns_used    17008
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.21
_cell_measurement_theta_min      3.31
_cell_volume                     4305.3(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1216
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            82981
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0534P)²+8.6753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3346
_reflns_number_total             4394
_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               7041373
_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+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
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
O3 O 0.95725(12) 0.63402(9) 0.6769(2) 0.0209(5) Uani 1 1 d . .
O2 O 0.94320(12) 0.62803(9) 0.4451(2) 0.0196(5) Uani 1 1 d . .
O4 O 0.84877(12) 0.67641(10) 0.5741(3) 0.0266(6) Uani 1 1 d . .
O1 O 0.97132(12) 0.71883(10) 0.5469(3) 0.0261(6) Uani 1 1 d . .
O7 O 0.88328(11) 0.53597(9) 0.5875(2) 0.0147(5) Uani 1 1 d . .
O9 O 0.90186(13) 0.54612(10) 0.8435(2) 0.0236(5) Uani 1 1 d . .
O8 O 1.13728(12) 0.46338(10) 0.6695(2) 0.0221(5) Uani 1 1 d . .
N2 N 0.73411(16) 0.34580(14) 0.7737(3) 0.0293(7) Uani 1 1 d . .
C1 C 0.92339(17) 0.42288(13) 0.7116(3) 0.0164(7) Uani 1 1 d . .
H1A H 0.8963 0.4267 0.7916 0.020 Uiso 1 1 calc R U
H1B H 0.9446 0.3841 0.7089 0.020 Uiso 1 1 calc R U
N1 N 0.76503(17) 0.39024(13) 0.7341(3) 0.0304(7) Uani 1 1 d . .
C5 C 1.09575(16) 0.58143(13) 0.5299(3) 0.0157(7) Uani 1 1 d . .
H5A H 1.1336 0.5776 0.5958 0.019 Uiso 1 1 calc R U
H5B H 1.0772 0.6210 0.5325 0.019 Uiso 1 1 calc R U
C4 C 0.80766(17) 0.38236(14) 0.6147(3) 0.0208(7) Uani 1 1 d . .
H4A H 0.7738 0.3842 0.5424 0.025 Uiso 1 1 calc R U
H4B H 0.8312 0.3444 0.6149 0.025 Uiso 1 1 calc R U
C3 C 0.83065(16) 0.48951(13) 0.6036(3) 0.0162(7) Uani 1 1 d . .
H3A H 0.7935 0.4915 0.5361 0.019 Uiso 1 1 calc R U
H3B H 0.8049 0.4944 0.6845 0.019 Uiso 1 1 calc R U
N3 N 0.7032(2) 0.30838(15) 0.8223(4) 0.0438(9) Uani 1 1 d . .
C2 C 0.86807(16) 0.42961(13) 0.6008(3) 0.0143(6) Uani 1 1 d . .
V1 V 1.06518(3) 0.45922(2) 0.57966(5) 0.01376(14) Uani 1 1 d . .
V2 V 0.95736(3) 0.54921(2) 0.72361(6) 0.01572(14) Uani 1 1 d . .
S3 S 0.92817(4) 0.66517(3) 0.56139(9) 0.0190(2) Uani 1 1 d . .
O5 O 1.03530(11) 0.54250(8) 0.5575(2) 0.0134(5) Uani 1 1 d . .
O6 O 0.98336(11) 0.46450(9) 0.7097(2) 0.0153(5) Uani 1 1 d . .
O10 O 1.05444(13) 0.56816(10) 0.8201(2) 0.0244(5) Uani 1 1 d . .
H10 H 1.0571 0.6072 0.8450 0.037 Uiso 1 1 d . U
C10 C 1.0834(2) 0.53445(17) 0.9216(4) 0.0340(9) Uani 1 1 d . .
H10A H 1.1291 0.5516 0.9518 0.051 Uiso 1 1 calc R U
H10B H 1.0476 0.5332 0.9899 0.051 Uiso 1 1 calc R U
H10C H 1.0931 0.4957 0.8919 0.051 Uiso 1 1 calc R U
N4 N 0.34188(13) 0.35004(10) 0.4260(3) 0.0132(5) Uani 1 1 d . .
C8 C 0.32048(17) 0.31527(14) 0.3116(3) 0.0194(7) Uani 1 1 d . .
H8A H 0.3309 0.3372 0.2356 0.029 Uiso 1 1 calc R U
H8B H 0.3488 0.2798 0.3102 0.029 Uiso 1 1 calc R U
H8C H 0.2680 0.3064 0.3152 0.029 Uiso 1 1 calc R U
C7 C 0.42399(16) 0.36342(14) 0.4197(3) 0.0189(7) Uani 1 1 d . .
H7A H 0.4382 0.3858 0.4931 0.028 Uiso 1 1 calc R U
H7B H 0.4519 0.3278 0.4183 0.028 Uiso 1 1 calc R U
H7C H 0.4344 0.3852 0.3435 0.028 Uiso 1 1 calc R U
C9 C 0.32605(18) 0.31646(14) 0.5457(3) 0.0205(7) Uani 1 1 d . .
H9A H 0.3400 0.3393 0.6187 0.031 Uiso 1 1 calc R U
H9B H 0.2736 0.3076 0.5500 0.031 Uiso 1 1 calc R U
H9C H 0.3544 0.2810 0.5451 0.031 Uiso 1 1 calc R U
C6 C 0.29705(17) 0.40506(13) 0.4281(3) 0.0189(7) Uani 1 1 d . .
H6A H 0.3107 0.4276 0.5017 0.028 Uiso 1 1 calc R U
H6B H 0.3071 0.4270 0.3521 0.028 Uiso 1 1 calc R U
H6C H 0.2447 0.3958 0.4320 0.028 Uiso 1 1 calc R U
O21 O 1.0869(2) 0.67063(13) 0.8985(3) 0.0584(10) Uani 1 1 d . .
H21 H 1.0664 0.6983 0.8636 0.088 Uiso 1 1 calc R U
C21 C 1.1300(2) 0.6908(2) 1.0034(4) 0.0420(11) Uani 1 1 d . .
H21A H 1.1752 0.7084 0.9725 0.063 Uiso 1 1 calc R U
H21B H 1.1424 0.6586 1.0580 0.063 Uiso 1 1 calc R U
H21C H 1.1016 0.7188 1.0509 0.063 Uiso 1 1 calc R 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'
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
S3 O3 V2 131.34(14) . .
S3 O2 V1 130.48(14) . 5_766
C3 O7 V2 118.13(19) . .
C3 O7 V1 116.76(19) . 5_766
V2 O7 V1 108.56(9) . 5_766
N3 N2 N1 172.2(4) . .
O6 C1 C2 113.7(2) . .
N2 N1 C4 114.4(3) . .
O5 C5 C2 113.2(2) . 5_766
N1 C4 C2 110.8(3) . .
O7 C3 C2 112.5(2) . .
C1 C2 C3 111.0(3) . .
C1 C2 C5 112.8(2) . 5_766
C3 C2 C5 110.5(3) . 5_766
C1 C2 C4 108.0(3) . .
C3 C2 C4 109.2(2) . .
C5 C2 C4 105.2(2) 5_766 .
O8 V1 O7 98.17(11) . 5_766
O8 V1 O6 100.64(11) . .
O7 V1 O6 159.59(9) 5_766 .
O8 V1 O5 103.01(10) . .
O7 V1 O5 88.18(9) 5_766 .
O6 V1 O5 79.97(9) . .
O8 V1 O2 101.18(10) . 5_766
O7 V1 O2 88.68(9) 5_766 5_766
O6 V1 O2 95.33(9) . 5_766
O5 V1 O2 155.81(9) . 5_766
O8 V1 O5 176.49(10) . 5_766
O7 V1 O5 79.16(8) 5_766 5_766
O6 V1 O5 81.70(8) . 5_766
O5 V1 O5 74.72(9) . 5_766
O2 V1 O5 81.13(8) 5_766 5_766
O9 V2 O7 98.27(11) . .
O9 V2 O6 99.01(11) . .
O7 V2 O6 87.28(9) . .
O9 V2 O3 103.46(11) . .
O7 V2 O3 88.51(9) . .
O6 V2 O3 157.52(10) . .
O9 V2 O10 98.47(11) . .
O7 V2 O10 163.06(10) . .
O6 V2 O10 92.68(9) . .
O3 V2 O10 85.07(10) . .
O9 V2 O5 173.47(10) . .
O7 V2 O5 81.09(8) . .
O6 V2 O5 74.49(8) . .
O3 V2 O5 83.04(9) . .
O10 V2 O5 82.58(9) . .
O4 S3 O1 111.98(14) . .
O4 S3 O3 110.56(15) . .
O1 S3 O3 107.77(14) . .
O4 S3 O2 110.42(14) . .
O1 S3 O2 107.49(14) . .
O3 S3 O2 108.49(13) . .
C5 O5 V1 114.93(17) . .
C5 O5 V2 125.71(18) . .
V1 O5 V2 98.18(9) . .
C5 O5 V1 118.24(18) . 5_766
V1 O5 V1 105.28(9) . 5_766
V2 O5 V1 90.03(7) . 5_766
C1 O6 V1 120.87(18) . .
C1 O6 V2 118.29(18) . .
V1 O6 V2 106.07(10) . .
C10 O10 V2 124.2(2) . .
C8 N4 C9 110.2(2) . .
C8 N4 C6 109.2(2) . .
C9 N4 C6 108.8(2) . .
C8 N4 C7 109.0(2) . .
C9 N4 C7 109.1(2) . .
C6 N4 C7 110.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O3 S3 1.499(3) .
O3 V2 2.013(2) .
O2 S3 1.512(2) .
O2 V1 2.031(2) 5_766
O4 S3 1.448(2) .
O1 S3 1.464(2) .
O7 C3 1.434(3) .
O7 V2 1.968(2) .
O7 V1 1.980(2) 5_766
O9 V2 1.600(2) .
O8 V1 1.598(2) .
N2 N3 1.142(4) .
N2 N1 1.235(4) .
C1 O6 1.438(3) .
C1 C2 1.532(4) .
N1 C4 1.474(4) .
C5 O5 1.433(3) .
C5 C2 1.534(4) 5_766
C4 C2 1.539(4) .
C3 C2 1.533(4) .
C2 C5 1.534(4) 5_766
V1 O7 1.980(2) 5_766
V1 O6 2.001(2) .
V1 O5 2.004(2) .
V1 O2 2.032(2) 5_766
V1 O5 2.299(2) 5_766
V2 O6 2.011(2) .
V2 O10 2.053(2) .
V2 O5 2.232(2) .
O5 V1 2.299(2) 5_766
O10 C10 1.413(4) .
N4 C8 1.490(4) .
N4 C9 1.499(4) .
N4 C6 1.499(4) .
N4 C7 1.500(4) .
O21 C21 1.419(5) .
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
O10 H10 O21 0.94 1.65 2.565(4) 163.4
