#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:36:45 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178787 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/41/4104153.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_4104153
loop_
_publ_author_name
'Charles Daniel'
'Hans Hartl'
_publ_section_title
;
 A Mixed-Valence VIV/VV Alkoxo-polyoxovanadium Cluster Series
 [V6O8(OCH3)11]n+/-: Exploring the Influence of a μ-Oxo Ligand in a Spin
 Frustrated Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5101
_journal_page_last               5114
_journal_paper_doi               10.1021/ja8073648
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         '(CH3O)11 V6O8'
_chemical_formula_sum            'C11 H33 O19 V6'
_chemical_formula_weight         775.01
_chemical_name_systematic
;
 undeca-methoxo-octa-oxo-hexavanadium 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.720(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1160(19)
_cell_length_b                   13.004(3)
_cell_length_c                   10.385(2)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.52
_cell_volume                     1353.7(5)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    DIAMOND
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans with 0.3 deg in omega'
_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  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0101
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27410
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       SHELXL
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0461P)²+2.0588P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                3615
_reflns_number_total             4137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8073648_si_001.cif
_cod_data_source_block           onc
_cod_original_cell_volume        1353.8(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4104153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C12 C 0.8116(3) 0.0548(3) 0.8012(3) 0.0584(8) Uani 1 1 d . A .
H12A H 0.8929 0.0832 0.8453 0.088 Uiso 1 1 calc R . .
H12B H 0.7895 0.0883 0.7188 0.088 Uiso 1 1 calc R . .
H12C H 0.8231 -0.0175 0.7878 0.088 Uiso 1 1 calc R . .
C13A C 0.5550(5) 0.2816(3) 0.8658(6) 0.0537(13) Uani 0.588(6) 1 d P A 1
H13A H 0.5523 0.2884 0.7735 0.081 Uiso 0.588(6) 1 calc PR A 1
H13B H 0.6460 0.2756 0.9055 0.081 Uiso 0.588(6) 1 calc PR A 1
H13C H 0.5152 0.3410 0.8996 0.081 Uiso 0.588(6) 1 calc PR A 1
C13B C 0.4510(9) 0.2944(5) 0.8304(7) 0.055(2) Uani 0.412(6) 1 d P A 2
H13D H 0.4483 0.3462 0.8960 0.082 Uiso 0.412(6) 1 calc PR A 2
H13E H 0.3654 0.2899 0.7783 0.082 Uiso 0.412(6) 1 calc PR A 2
H13F H 0.5173 0.3124 0.7763 0.082 Uiso 0.412(6) 1 calc PR A 2
C21A C 0.2525(5) -0.0148(4) 0.6628(4) 0.0444(11) Uani 0.588(6) 1 d P A 1
H21A H 0.1577 -0.0068 0.6589 0.067 Uiso 0.588(6) 1 calc PR A 1
H21B H 0.2745 -0.0867 0.6649 0.067 Uiso 0.588(6) 1 calc PR A 1
H21C H 0.2816 0.0163 0.5876 0.067 Uiso 0.588(6) 1 calc PR A 1
C21B C 0.2311(7) 0.0734(10) 0.6771(8) 0.082(4) Uani 0.412(6) 1 d P A 2
H21D H 0.2442 0.0377 0.5989 0.123 Uiso 0.412(6) 1 calc PR A 2
H21E H 0.2470 0.1455 0.6667 0.123 Uiso 0.412(6) 1 calc PR A 2
H21F H 0.1411 0.0632 0.6943 0.123 Uiso 0.412(6) 1 calc PR A 2
C23 C 0.7392(6) 0.2514(4) 1.0921(6) 0.0548(14) Uani 0.50 1 d P . .
H23A H 0.8315 0.2382 1.1221 0.082 Uiso 0.50 1 calc PR . .
H23B H 0.7076 0.3056 1.1429 0.082 Uiso 0.50 1 calc PR . .
H23C H 0.7294 0.2718 1.0024 0.082 Uiso 0.50 1 calc PR . .
C31A C 0.5919(6) -0.1342(5) 0.6629(5) 0.0508(13) Uani 0.588(6) 1 d P A 1
H31A H 0.5921 -0.2074 0.6744 0.076 Uiso 0.588(6) 1 calc PR A 1
H31B H 0.6811 -0.1109 0.6580 0.076 Uiso 0.588(6) 1 calc PR A 1
H31C H 0.5357 -0.1167 0.5839 0.076 Uiso 0.588(6) 1 calc PR A 1
C31B C 0.5179(14) -0.1188(8) 0.6405(7) 0.076(3) Uani 0.412(6) 1 d P A 2
H31D H 0.5741 -0.0813 0.5894 0.114 Uiso 0.412(6) 1 calc PR A 2
H31E H 0.4261 -0.1064 0.6074 0.114 Uiso 0.412(6) 1 calc PR A 2
H31F H 0.5366 -0.1910 0.6358 0.114 Uiso 0.412(6) 1 calc PR A 2
C32A C 0.8196(8) -0.1897(6) 1.0299(5) 0.0387(12) Uani 0.588(6) 1 d P A 1
H32A H 0.8064 -0.2519 0.9800 0.058 Uiso 0.588(6) 1 calc PR A 1
H32B H 0.8192 -0.2050 1.1202 0.058 Uiso 0.588(6) 1 calc PR A 1
H32C H 0.9038 -0.1596 1.0177 0.058 Uiso 0.588(6) 1 calc PR A 1
C32B C 0.8203(14) -0.1828(14) 0.992(2) 0.158(10) Uani 0.412(6) 1 d P A 2
H32D H 0.8666 -0.1850 1.0789 0.237 Uiso 0.412(6) 1 calc PR A 2
H32E H 0.8796 -0.1581 0.9340 0.237 Uiso 0.412(6) 1 calc PR A 2
H32F H 0.7899 -0.2505 0.9660 0.237 Uiso 0.412(6) 1 calc PR A 2
V1 V 0.51595(3) 0.06471(3) 0.79672(3) 0.03016(9) Uani 1 1 d . A .
V2 V 0.72331(3) 0.02525(3) 1.05768(3) 0.03065(9) Uani 1 1 d . . .
V3 V 0.46816(3) 0.16078(3) 1.07217(3) 0.03003(9) Uani 1 1 d . . .
O123 O 0.5000 0.0000 1.0000 0.0238(3) Uani 1 2 d S . .
O21 O 0.31965(14) 0.03536(12) 0.78086(14) 0.0327(3) Uani 1 1 d . . .
O23 O 0.65782(15) 0.15394(12) 1.10593(15) 0.0360(3) Uani 1 1 d . . .
O32 O 0.71509(13) -0.11919(11) 0.98779(15) 0.0321(3) Uani 1 1 d . . .
O12 O 0.70726(14) 0.07021(13) 0.87763(15) 0.0352(3) Uani 1 1 d . . .
O31 O 0.54276(16) -0.08633(13) 0.76943(13) 0.0362(3) Uani 1 1 d . . .
O13 O 0.48496(15) 0.19423(11) 0.89316(15) 0.0341(3) Uani 1 1 d . . .
O2 O 0.87985(16) 0.03863(15) 1.09641(18) 0.0462(4) Uani 1 1 d . . .
O1 O 0.52802(19) 0.11081(16) 0.65653(16) 0.0497(4) Uani 1 1 d . . .
O3 O 0.4430(2) 0.27386(13) 1.1214(2) 0.0502(4) 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'
O O 0.0106 0.0060 '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
O1 V1 O12 100.44(8) . .
O1 V1 O13 100.17(9) . .
O12 V1 O13 88.14(6) . .
O1 V1 O21 101.12(8) . .
O12 V1 O21 158.42(6) . .
O13 V1 O21 88.94(6) . .
O1 V1 O31 102.16(9) . .
O12 V1 O31 87.30(7) . .
O13 V1 O31 157.67(6) . .
O21 V1 O31 87.32(7) . .
O1 V1 O123 179.28(8) . .
O12 V1 O123 79.11(4) . .
O13 V1 O123 79.27(4) . .
O21 V1 O123 79.34(4) . .
O31 V1 O123 78.40(4) . .
O2 V2 O23 102.03(9) . .
O2 V2 O12 99.32(8) . .
O23 V2 O12 90.10(7) . .
O2 V2 O21 98.96(8) . 3_657
O23 V2 O21 90.19(7) . 3_657
O12 V2 O21 161.24(6) . 3_657
O2 V2 O32 100.65(8) . .
O23 V2 O32 157.31(6) . .
O12 V2 O32 86.54(7) . .
O21 V2 O32 85.97(7) 3_657 .
O2 V2 O123 177.91(7) . .
O23 V2 O123 80.06(5) . .
O12 V2 O123 80.74(4) . .
O21 V2 O123 80.84(4) 3_657 .
O32 V2 O123 77.25(4) . .
O3 V3 O23 100.66(9) . .
O3 V3 O31 99.23(9) . 3_657
O23 V3 O31 89.50(7) . 3_657
O3 V3 O13 98.02(9) . .
O23 V3 O13 88.34(7) . .
O31 V3 O13 162.72(7) 3_657 .
O3 V3 O32 99.95(9) . 3_657
O23 V3 O32 159.35(6) . 3_657
O31 V3 O32 88.41(7) 3_657 3_657
O13 V3 O32 87.60(7) . 3_657
O3 V3 O123 178.91(8) . .
O23 V3 O123 80.38(5) . .
O31 V3 O123 81.09(5) 3_657 .
O13 V3 O123 81.65(5) . .
O32 V3 O123 79.00(4) 3_657 .
V3 O123 V3 180.0 3_657 .
V3 O123 V2 92.295(14) 3_657 .
V3 O123 V2 87.705(14) . .
V3 O123 V2 87.705(14) 3_657 3_657
V3 O123 V2 92.295(14) . 3_657
V2 O123 V2 180.0 . 3_657
V3 O123 V1 89.807(17) 3_657 3_657
V3 O123 V1 90.193(17) . 3_657
V2 O123 V1 90.041(14) . 3_657
V2 O123 V1 89.959(14) 3_657 3_657
V3 O123 V1 90.193(16) 3_657 .
V3 O123 V1 89.807(17) . .
V2 O123 V1 89.959(14) . .
V2 O123 V1 90.041(14) 3_657 .
V1 O123 V1 180.0 3_657 .
C21B O21 C21A 48.6(5) . .
C21B O21 V2 127.7(4) . 3_657
C21A O21 V2 113.9(2) . 3_657
C21B O21 V1 121.4(4) . .
C21A O21 V1 119.6(2) . .
V2 O21 V1 109.75(6) 3_657 .
C23 O23 V2 119.8(3) . .
C23 O23 V3 119.0(3) . .
V2 O23 V3 111.86(8) . .
C32B O32 C32A 16.5(12) . .
C32B O32 V3 123.7(8) . 3_657
C32A O32 V3 123.7(4) . 3_657
C32B O32 V2 124.7(8) . .
C32A O32 V2 119.8(4) . .
V3 O32 V2 111.44(6) 3_657 .
C12 O12 V2 121.57(16) . .
C12 O12 V1 120.66(16) . .
V2 O12 V1 110.08(7) . .
C31B O31 C31A 32.2(5) . .
C31B O31 V3 130.2(5) . 3_657
C31A O31 V3 120.9(3) . 3_657
C31B O31 V1 114.9(4) . .
C31A O31 V1 127.4(3) . .
V3 O31 V1 110.31(7) 3_657 .
C13A O13 C13B 44.2(4) . .
C13A O13 V3 119.5(3) . .
C13B O13 V3 125.2(3) . .
C13A O13 V1 117.8(3) . .
C13B O13 V1 124.3(3) . .
V3 O13 V1 109.28(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C12 O12 1.418(3) .
C13A O13 1.388(4) .
C13B O13 1.477(5) .
C21A O21 1.472(4) .
C21B O21 1.397(6) .
C23 O23 1.529(5) .
C31A O31 1.416(5) .
C31B O31 1.394(7) .
C32A O32 1.423(6) .
C32B O32 1.344(13) .
V1 O1 1.5944(16) .
V1 O12 2.0050(16) .
V1 O13 2.0057(16) .
V1 O21 2.0070(16) .
V1 O31 2.0082(17) .
V1 O123 2.2984(5) .
V2 O2 1.5902(16) .
V2 O23 1.8920(16) .
V2 O12 1.9450(16) .
V2 O21 1.9539(15) 3_657
V2 O32 2.0115(16) .
V2 O123 2.2817(5) .
V3 O3 1.5886(17) .
V3 O23 1.9056(16) .
V3 O31 1.9246(16) 3_657
V3 O13 1.9390(16) .
V3 O32 1.9510(15) 3_657
V3 O123 2.2588(5) .
O123 V3 2.2588(5) 3_657
O123 V2 2.2817(5) 3_657
O123 V1 2.2984(5) 3_657
O21 V2 1.9539(15) 3_657
O32 V3 1.9510(15) 3_657
O31 V3 1.9246(16) 3_657
