#------------------------------------------------------------------------------ #$Date: 2019-10-09 17:54:25 +0300 (Wed, 09 Oct 2019) $ #$Revision: 219223 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/10/02/4100290.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_4100290 loop_ _publ_author_name 'Daniel, Charles' 'Hartl, Hans' _publ_section_title ; Neutral and Cationic V^IV^/V^V^ Mixed-Valence Alkoxo-polyoxovanadium Clusters [V~6~O~7~(OR)~12~]^n+^(R = --CH~3~, --C~2~H~5~): Structural, Cyclovoltammetric and IR-Spectroscopic Investigations on Mixed Valency in a Hexanuclear Core ; _journal_coden_ASTM JACSAT _journal_issue 40 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 13978 _journal_page_last 13987 _journal_paper_doi 10.1021/ja052902b _journal_volume 127 _journal_year 2005 _chemical_formula_sum 'C26 H64 Cl16 O19 Sb2 V6' _chemical_formula_weight 1797.11 _space_group_IT_number 2 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 109.445(3) _cell_angle_beta 102.351(4) _cell_angle_gamma 93.771(4) _cell_formula_units_Z 1 _cell_length_a 11.1503(19) _cell_length_b 11.584(2) _cell_length_c 12.829(2) _cell_measurement_temperature 173(2) _cell_volume 1509.3(5) _diffrn_ambient_temperature 173(2) _exptl_crystal_density_diffrn 1.977 _cod_depositor_comments ; Updated bibliographic information. Antanas Vaitkus, 2019-10-09 ; _cod_database_code 4100290 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 Sb1 Sb 0.860538(8) 0.917433(8) 0.692137(8) 0.01402(2) Uani 1 1 d . . . V2 V 0.66183(2) 0.444858(19) -0.078019(18) 0.01047(4) Uani 1 1 d . . . V1 V 0.62615(2) 0.667145(19) 0.137374(18) 0.01021(4) Uani 1 1 d . . . V3 V 0.45219(2) 0.614651(19) -0.113332(18) 0.01014(4) Uani 1 1 d . . . Cl6 Cl 1.07543(3) 0.99459(3) 0.75127(3) 0.02462(7) Uani 1 1 d . . . Cl4 Cl 0.86230(4) 0.88360(4) 0.50071(3) 0.02550(8) Uani 1 1 d . . . Cl3 Cl 0.81747(3) 1.12087(3) 0.71644(3) 0.02162(7) Uani 1 1 d . . . Cl1 Cl 0.64546(3) 0.83980(3) 0.63259(4) 0.02855(8) Uani 1 1 d . . . Cl2 Cl 0.85621(4) 0.95001(4) 0.88339(3) 0.02962(8) Uani 1 1 d . . . Cl5 Cl 0.90852(3) 0.71544(3) 0.67097(3) 0.02186(7) Uani 1 1 d . . . Cl1L Cl 0.68128(4) 0.20529(4) 0.43732(4) 0.03616(10) Uani 1 1 d . . . Cl2L Cl 0.88930(4) 0.37402(4) 0.61368(4) 0.03553(10) Uani 1 1 d . . . C321 C 0.72629(12) 0.23688(12) 0.00497(12) 0.0153(2) Uani 1 1 d . . . H21A H 0.7596 0.2217 -0.0616 0.018 Uiso 1 1 calc R . . H21B H 0.6614 0.1687 -0.0113 0.018 Uiso 1 1 calc R . . C322 C 0.82818(13) 0.24318(14) 0.10648(13) 0.0203(3) Uani 1 1 d . . . H22A H 0.8906 0.3129 0.1247 0.030 Uiso 1 1 calc R . . H22B H 0.8648 0.1685 0.0884 0.030 Uiso 1 1 calc R . . H22C H 0.7939 0.2521 0.1708 0.030 Uiso 1 1 calc R . . C121 C 0.88001(12) 0.62946(14) 0.09537(12) 0.0186(3) Uani 1 1 d . . . H31A H 0.9159 0.5569 0.1006 0.022 Uiso 1 1 calc R . . H31B H 0.9010 0.6923 0.1712 0.022 Uiso 1 1 calc R . . C122 C 0.93485(14) 0.67690(15) 0.01739(14) 0.0246(3) Uani 1 1 d . . . H32A H 0.9183 0.6132 -0.0567 0.037 Uiso 1 1 calc R . . H32B H 1.0229 0.7001 0.0483 0.037 Uiso 1 1 calc R . . H32C H 0.8983 0.7477 0.0108 0.037 Uiso 1 1 calc R . . C311 C 0.77267(13) 0.54862(13) 0.28745(12) 0.0180(3) Uani 1 1 d . . . H41A H 0.8174 0.6321 0.3152 0.022 Uiso 1 1 calc R . . H41B H 0.8206 0.4935 0.2439 0.022 Uiso 1 1 calc R . . C312 C 0.76097(17) 0.51296(18) 0.38673(14) 0.0328(4) Uani 1 1 d . . . H42A H 0.7164 0.5694 0.4318 0.049 Uiso 1 1 calc R . . H42B H 0.8422 0.5161 0.4327 0.049 Uiso 1 1 calc R . . H42C H 0.7167 0.4304 0.3596 0.049 Uiso 1 1 calc R . . C211 C 0.47737(13) 0.74572(12) 0.30720(11) 0.0165(3) Uani 1 1 d . . . H61A H 0.5351 0.7118 0.3531 0.020 Uiso 1 1 calc R . . H61B H 0.3952 0.7269 0.3166 0.020 Uiso 1 1 calc R . . C212 C 0.51323(15) 0.88363(13) 0.34887(14) 0.0240(3) Uani 1 1 d . . . H62A H 0.5986 0.9028 0.3496 0.036 Uiso 1 1 calc R . . H62B H 0.5025 0.9197 0.4247 0.036 Uiso 1 1 calc R . . H62C H 0.4616 0.9166 0.2989 0.036 Uiso 1 1 calc R . . C131 C 0.63445(13) 0.85331(12) 0.02532(12) 0.0173(3) Uani 1 1 d . . . H71A H 0.6077 0.8593 -0.0495 0.021 Uiso 1 1 calc R . . H71B H 0.7228 0.8491 0.0402 0.021 Uiso 1 1 calc R . . C132 C 0.61080(14) 0.96711(12) 0.11450(13) 0.0222(3) Uani 1 1 d . . . H72A H 0.5234 0.9715 0.0997 0.033 Uiso 1 1 calc R . . H72B H 0.6545 1.0397 0.1115 0.033 Uiso 1 1 calc R . . H72C H 0.6395 0.9624 0.1888 0.033 Uiso 1 1 calc R . . C231 C 0.65906(14) 0.59637(14) -0.23248(12) 0.0194(3) Uani 1 1 d . . . H91A H 0.7422 0.5747 -0.2228 0.023 Uiso 1 1 calc R . . H91B H 0.6663 0.6858 -0.2082 0.023 Uiso 1 1 calc R . . C232 C 0.59144(16) 0.54062(15) -0.35571(13) 0.0251(3) Uani 1 1 d . . . H92A H 0.5831 0.4520 -0.3798 0.038 Uiso 1 1 calc R . . H92B H 0.6372 0.5686 -0.4004 0.038 Uiso 1 1 calc R . . H92C H 0.5106 0.5654 -0.3662 0.038 Uiso 1 1 calc R . . C1L C 0.84401(15) 0.23411(15) 0.49399(15) 0.0273(3) Uani 1 1 d . . . H1L1 H 0.8847 0.2391 0.4356 0.033 Uiso 1 1 calc R . . H1L2 H 0.8704 0.1660 0.5166 0.033 Uiso 1 1 calc R . . O2 O 0.77499(9) 0.40549(9) -0.13160(8) 0.01673(19) Uani 1 1 d . . . O32 O 0.67391(8) 0.35256(8) 0.02775(8) 0.01249(17) Uani 1 1 d . . . O12 O 0.74486(8) 0.59714(8) 0.05474(8) 0.01296(17) Uani 1 1 d . . . O31 O 0.65127(8) 0.54312(8) 0.21251(8) 0.01219(17) Uani 1 1 d . . . O1 O 0.71973(9) 0.77848(8) 0.23336(8) 0.01484(18) Uani 1 1 d . . . O21 O 0.47753(8) 0.68692(8) 0.18684(8) 0.01231(17) Uani 1 1 d . . . O13 O 0.56792(9) 0.74044(8) 0.02611(8) 0.01279(17) Uani 1 1 d . . . O123 O 0.5000 0.5000 0.0000 0.0101(2) Uani 1 2 d S . . O23 O 0.59523(9) 0.55343(9) -0.16034(8) 0.01480(18) Uani 1 1 d . . . O3 O 0.42472(9) 0.70301(9) -0.18404(8) 0.01523(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.01373(4) 0.01248(4) 0.01486(4) 0.00479(3) 0.00189(3) 0.00118(3) V2 0.01100(10) 0.01092(9) 0.01010(10) 0.00384(8) 0.00354(7) 0.00228(7) V1 0.01131(10) 0.00923(9) 0.00935(9) 0.00294(7) 0.00181(7) 0.00105(7) V3 0.01152(10) 0.01013(9) 0.00932(9) 0.00434(8) 0.00230(7) 0.00170(7) Cl6 0.01521(15) 0.02307(16) 0.03078(19) 0.00841(15) -0.00063(14) -0.00244(13) Cl4 0.0333(2) 0.02718(17) 0.01470(16) 0.00627(14) 0.00441(14) 0.00735(15) Cl3 0.02657(18) 0.01454(14) 0.02511(17) 0.00775(13) 0.00737(14) 0.00563(12) Cl1 0.01432(16) 0.02309(17) 0.0485(2) 0.01680(17) 0.00228(15) 0.00110(13) Cl2 0.0453(2) 0.02857(18) 0.02033(18) 0.01154(15) 0.01380(16) 0.00810(17) Cl5 0.02125(16) 0.01487(14) 0.02759(18) 0.00755(13) 0.00190(13) 0.00400(12) Cl1L 0.0294(2) 0.0325(2) 0.0408(2) 0.01107(18) 0.00184(18) -0.00100(17) Cl2L 0.0343(2) 0.0306(2) 0.0346(2) 0.00823(18) 0.00058(18) 0.00125(17) C321 0.0165(6) 0.0122(5) 0.0177(6) 0.0050(5) 0.0044(5) 0.0063(5) C322 0.0190(7) 0.0230(7) 0.0214(7) 0.0106(6) 0.0042(5) 0.0095(5) C121 0.0098(6) 0.0251(7) 0.0187(7) 0.0072(6) 0.0008(5) 0.0007(5) C122 0.0157(7) 0.0311(8) 0.0258(8) 0.0091(6) 0.0061(6) -0.0036(6) C311 0.0165(6) 0.0185(6) 0.0160(6) 0.0073(5) -0.0032(5) 0.0006(5) C312 0.0336(9) 0.0415(9) 0.0205(8) 0.0187(7) -0.0070(7) -0.0089(7) C211 0.0221(7) 0.0168(6) 0.0096(6) 0.0016(5) 0.0062(5) 0.0038(5) C212 0.0279(8) 0.0159(6) 0.0224(7) -0.0023(6) 0.0090(6) 0.0027(6) C131 0.0194(6) 0.0135(6) 0.0190(7) 0.0081(5) 0.0028(5) -0.0028(5) C132 0.0253(7) 0.0122(6) 0.0250(7) 0.0059(5) -0.0002(6) 0.0006(5) C231 0.0203(7) 0.0260(7) 0.0149(6) 0.0107(6) 0.0070(5) -0.0029(5) C232 0.0356(9) 0.0259(7) 0.0146(7) 0.0072(6) 0.0098(6) -0.0027(6) C1L 0.0253(8) 0.0292(8) 0.0296(8) 0.0103(7) 0.0106(7) 0.0075(6) O2 0.0167(5) 0.0178(4) 0.0172(5) 0.0057(4) 0.0077(4) 0.0044(4) O32 0.0128(4) 0.0111(4) 0.0138(4) 0.0045(3) 0.0030(3) 0.0039(3) O12 0.0099(4) 0.0149(4) 0.0136(4) 0.0055(4) 0.0020(3) -0.0001(3) O31 0.0119(4) 0.0135(4) 0.0099(4) 0.0039(3) 0.0006(3) 0.0013(3) O1 0.0158(4) 0.0129(4) 0.0136(4) 0.0039(3) 0.0010(4) 0.0006(3) O21 0.0151(4) 0.0113(4) 0.0092(4) 0.0016(3) 0.0037(3) 0.0014(3) O13 0.0151(4) 0.0101(4) 0.0130(4) 0.0051(3) 0.0024(3) -0.0006(3) O123 0.0112(6) 0.0096(5) 0.0099(6) 0.0037(5) 0.0030(5) 0.0016(4) O23 0.0152(4) 0.0198(4) 0.0111(4) 0.0077(4) 0.0043(3) -0.0009(4) O3 0.0173(5) 0.0149(4) 0.0144(4) 0.0071(4) 0.0029(4) 0.0024(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 Cl4 2.3591(6) . ? Sb1 Cl2 2.3667(6) . ? Sb1 Cl6 2.3675(5) . ? Sb1 Cl3 2.3675(5) . ? Sb1 Cl1 2.3703(5) . ? Sb1 Cl5 2.3745(5) . ? V2 O2 1.5844(10) . ? V2 O32 1.9771(9) . ? V2 O23 1.9800(9) . ? V2 O12 1.9949(10) . ? V2 O21 2.0087(9) 2_665 ? V2 O123 2.2726(4) . ? V1 O1 1.5761(10) . ? V1 O21 1.8985(10) . ? V1 O13 1.9138(9) . ? V1 O12 1.9241(10) . ? V1 O31 1.9827(9) . ? V1 O123 2.2677(3) . ? V3 O3 1.5827(9) . ? V3 O23 1.9199(10) . ? V3 O32 1.9441(10) 2_665 ? V3 O31 1.9586(9) 2_665 ? V3 O13 2.0045(10) . ? V3 O123 2.2823(3) . ? Cl1L C1L 1.7683(17) . ? Cl2L C1L 1.7729(18) . ? C321 O32 1.4620(15) . ? C321 C322 1.5116(18) . ? C121 O12 1.4638(16) . ? C121 C122 1.503(2) . ? C311 O31 1.4669(15) . ? C311 C312 1.491(2) . ? C211 O21 1.4660(16) . ? C211 C212 1.5012(19) . ? C131 O13 1.4644(15) . ? C131 C132 1.512(2) . ? C231 O23 1.4670(16) . ? C231 C232 1.494(2) . ? O32 V3 1.9441(10) 2_665 ? O31 V3 1.9586(9) 2_665 ? O21 V2 2.0087(10) 2_665 ? O123 V1 2.2677(3) 2_665 ? O123 V2 2.2726(4) 2_665 ? O123 V3 2.2823(3) 2_665 ?