#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/48/1514846.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_1514846
loop_
_publ_author_name
'Forster, Johannes'
'Rösner, Benedikt'
'Fink, Rainer H.'
'Nye, Leanne C.'
'Ivanovic-Burmazovic, Ivana'
'Kastner, Katharina'
'Tucher, Johannes'
'Streb, Carsten'
_publ_section_title
;
 Oxidation-driven self-assembly gives access to high-nuclearity molecular
 copper vanadium oxide clusters
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              418
_journal_paper_doi               10.1039/c2sc20942j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C10 H30 N2 O12 S5 V'
_chemical_formula_weight         581.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.27(3)
_cell_angle_beta                 77.71(2)
_cell_angle_gamma                89.25(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4145(19)
_cell_length_b                   11.119(2)
_cell_length_c                   13.183(2)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      3.6
_cell_volume                     1240.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Kappa Nonius CCD'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13758
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.85
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Kappa Nonius CCD'
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0276
_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)+(0.0205P)²+1.2451P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                4469
_reflns_number_total             4904
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2sc20942j.txt
_cod_data_source_block           CS1137
_cod_original_cell_volume        1240.0(4)
_cod_database_code               1514846
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4003(2) 0.3993(2) -0.06058(17) 0.0235(4) Uani 1 1 d . . .
H1A H 0.4972 0.3707 -0.0635 0.035 Uiso 1 1 calc R . .
H1B H 0.3957 0.4765 -0.0444 0.035 Uiso 1 1 calc R . .
H1C H 0.3757 0.4185 -0.1320 0.035 Uiso 1 1 calc R . .
C2 C -0.0336(3) 0.3255(2) 0.45031(19) 0.0298(5) Uani 1 1 d . . .
H2A H -0.0961 0.2465 0.4807 0.045 Uiso 1 1 calc R . .
H2B H -0.0912 0.3996 0.4312 0.045 Uiso 1 1 calc R . .
H2C H 0.0177 0.3269 0.5056 0.045 Uiso 1 1 calc R . .
C3 C 0.3762(3) -0.2488(2) 0.30333(19) 0.0271(5) Uani 1 1 d . . .
H3A H 0.3102 -0.2611 0.3736 0.041 Uiso 1 1 calc R . .
H3B H 0.4400 -0.3186 0.3150 0.041 Uiso 1 1 calc R . .
H3C H 0.3217 -0.2488 0.2495 0.041 Uiso 1 1 calc R . .
C4 C 0.1109(2) 0.3538(2) 0.0319(2) 0.0273(5) Uani 1 1 d . . .
H4A H 0.0298 0.2971 0.0859 0.041 Uiso 1 1 calc R . .
H4B H 0.0973 0.3746 -0.0430 0.041 Uiso 1 1 calc R . .
H4C H 0.1174 0.4328 0.0445 0.041 Uiso 1 1 calc R . .
C5 C -0.1632(2) -0.0527(2) 0.32752(19) 0.0278(5) Uani 1 1 d . . .
H5A H -0.1863 -0.0545 0.4026 0.042 Uiso 1 1 calc R . .
H5B H -0.2130 -0.1268 0.3264 0.042 Uiso 1 1 calc R . .
H5C H -0.1935 0.0264 0.2768 0.042 Uiso 1 1 calc R . .
C6 C 0.5028(3) 0.2712(3) 0.4504(2) 0.0357(6) Uani 1 1 d . . .
H6A H 0.4008 0.2660 0.4837 0.054 Uiso 1 1 calc R . .
H6B H 0.5512 0.3453 0.4527 0.054 Uiso 1 1 calc R . .
H6C H 0.5440 0.1928 0.4917 0.054 Uiso 1 1 calc R . .
C7 C 0.5888(2) -0.1006(2) 0.12519(19) 0.0267(5) Uani 1 1 d . . .
H7A H 0.6535 -0.0227 0.0863 0.040 Uiso 1 1 calc R . .
H7B H 0.5265 -0.1056 0.0778 0.040 Uiso 1 1 calc R . .
H7C H 0.6448 -0.1758 0.1431 0.040 Uiso 1 1 calc R . .
C8 C 0.7191(2) 0.2955(2) 0.2713(2) 0.0299(5) Uani 1 1 d . . .
H8A H 0.7508 0.3053 0.1941 0.045 Uiso 1 1 calc R . .
H8B H 0.7519 0.2161 0.3195 0.045 Uiso 1 1 calc R . .
H8C H 0.7593 0.3685 0.2805 0.045 Uiso 1 1 calc R . .
C9 C 0.1909(3) 0.4843(2) 0.2919(2) 0.0346(5) Uani 1 1 d . . .
H9A H 0.2662 0.5025 0.2249 0.052 Uiso 1 1 calc R . .
H9B H 0.2340 0.4799 0.3529 0.052 Uiso 1 1 calc R . .
H9C H 0.1251 0.5526 0.2785 0.052 Uiso 1 1 calc R . .
C10 C 0.0394(3) -0.0540(2) 0.14659(19) 0.0288(5) Uani 1 1 d . . .
H10A H 0.1393 -0.0566 0.1119 0.043 Uiso 1 1 calc R . .
H10B H 0.0022 0.0251 0.1020 0.043 Uiso 1 1 calc R . .
H10C H -0.0171 -0.1281 0.1515 0.043 Uiso 1 1 calc R . .
N2 N 0.7783(3) 0.6118(2) 0.3263(2) 0.0391(5) Uani 1 1 d . . .
N8 N 0.75027(19) 0.24659(17) 0.00108(15) 0.0220(4) Uani 1 1 d . . .
O1 O 0.80467(19) 0.16127(16) 0.07319(14) 0.0344(4) Uani 1 1 d . . .
O2 O 0.19786(15) 0.22882(13) 0.37715(11) 0.0202(3) Uani 1 1 d . . .
O3 O 0.08906(15) 0.07822(13) 0.26604(12) 0.0199(3) Uani 1 1 d . . .
O4 O 0.69239(18) 0.21601(16) -0.06326(14) 0.0326(4) Uani 1 1 d . . .
O5 O 0.47993(15) 0.15339(13) 0.31532(12) 0.0225(3) Uani 1 1 d . . .
O6 O 0.30611(15) 0.27181(13) 0.15699(11) 0.0181(3) Uani 1 1 d . . .
O7 O 0.7533(2) 0.36145(15) -0.00604(16) 0.0383(4) Uani 1 1 d . . .
O8 O 0.24611(16) -0.02895(13) 0.42782(12) 0.0220(3) Uani 1 1 d . . .
O9 O 0.37311(15) 0.00709(13) 0.21000(12) 0.0208(3) Uani 1 1 d . . .
O10 O 0.6534(5) 0.5718(6) 0.3339(7) 0.095(2) Uani 0.665(10) 1 d P A 1
O11 O 0.8319(10) 0.6320(6) 0.3914(6) 0.106(4) Uani 0.665(10) 1 d P A 1
O12 O 0.8572(6) 0.6217(6) 0.2352(4) 0.103(2) Uani 0.665(10) 1 d P A 1
O10A O 0.715(3) 0.629(2) 0.272(2) 0.202(11) Uani 0.335(10) 1 d P A 2
O11A O 0.9018(9) 0.6488(9) 0.3192(15) 0.097(6) Uani 0.335(10) 1 d P A 2
O12A O 0.7191(13) 0.5471(13) 0.4414(8) 0.096(4) Uani 0.335(10) 1 d P A 2
S2 S 0.02800(5) -0.05862(5) 0.28437(4) 0.01967(11) Uani 1 1 d . . .
S3 S 0.52587(5) 0.28907(5) 0.30766(4) 0.01948(11) Uani 1 1 d . . .
S4 S 0.48144(5) -0.09626(5) 0.25111(4) 0.01871(11) Uani 1 1 d . . .
S5 S 0.09362(5) 0.33230(5) 0.32766(4) 0.01883(11) Uani 1 1 d . . .
S6 S 0.27474(5) 0.27356(4) 0.04727(4) 0.01751(11) Uani 1 1 d . . .
V1 V 0.27855(3) 0.09792(3) 0.31134(3) 0.01524(9) Uani 1 1 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
O10A N2 O11 155.7(13)
O10A N2 O11A 134.2(19)
O11 N2 O11A 48.8(7)
O10A N2 O10 46.3(16)
O11 N2 O10 131.4(7)
O11A N2 O10 178.8(5)
O10A N2 O12 73.0(16)
O11 N2 O12 118.4(6)
O11A N2 O12 69.6(8)
O10 N2 O12 110.0(5)
O10A N2 O12A 119.8(17)
O11 N2 O12A 60.4(6)
O11A N2 O12A 105.3(9)
O10 N2 O12A 74.4(6)
O12 N2 O12A 153.8(6)
O7 N8 O4 120.16(18)
O7 N8 O1 120.05(17)
O4 N8 O1 119.79(17)
S5 O2 V1 124.42(8)
S2 O3 V1 119.81(8)
S3 O5 V1 124.55(9)
S6 O6 V1 123.91(8)
S4 O9 V1 118.93(8)
O3 S2 C5 102.99(10)
O3 S2 C10 105.21(10)
C5 S2 C10 100.04(11)
O5 S3 C8 103.02(10)
O5 S3 C6 104.73(11)
C8 S3 C6 98.70(12)
O9 S4 C7 103.88(10)
O9 S4 C3 104.27(10)
C7 S4 C3 99.33(11)
O2 S5 C2 102.33(10)
O2 S5 C9 104.40(10)
C2 S5 C9 99.31(12)
O6 S6 C1 104.10(9)
O6 S6 C4 105.98(10)
C1 S6 C4 98.82(11)
O8 V1 O5 98.03(8)
O8 V1 O9 97.13(7)
O5 V1 O9 88.47(6)
O8 V1 O2 96.96(7)
O5 V1 O2 88.45(6)
O9 V1 O2 165.86(6)
O8 V1 O3 96.63(7)
O5 V1 O3 165.15(6)
O9 V1 O3 87.33(6)
O2 V1 O3 92.16(6)
O8 V1 O6 175.91(6)
O5 V1 O6 85.22(7)
O9 V1 O6 85.40(6)
O2 V1 O6 80.60(6)
O3 V1 O6 80.24(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 S6 1.779(2)
C2 S5 1.772(2)
C3 S4 1.785(2)
C4 S6 1.781(2)
C5 S2 1.777(2)
C6 S3 1.779(2)
C7 S4 1.768(2)
C8 S3 1.775(2)
C9 S5 1.777(2)
C10 S2 1.777(2)
N2 O10A 0.990(12)
N2 O11 1.174(5)
N2 O11A 1.211(10)
N2 O10 1.232(6)
N2 O12 1.235(5)
N2 O12A 1.392(10)
N8 O7 1.244(2)
N8 O4 1.248(2)
N8 O1 1.250(2)
O2 S5 1.5412(15)
O2 V1 2.0284(15)
O3 S2 1.5438(14)
O3 V1 2.0376(14)
O5 S3 1.5343(15)
O5 V1 2.0188(15)
O6 S6 1.5296(14)
O6 V1 2.1665(16)
O8 V1 1.6059(16)
O9 S4 1.5419(15)
O9 V1 2.0275(15)
