# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' _publ_contact_author_name 'Yurii Yablokov' _publ_contact_author_address ; Solid State Radiospectroscopy Institute of Molecular Physics Smoluchowskiego 17 Poznan 60-179 POLAND ; _publ_contact_author_email YABLOKOV@IFMPAN.POZNAN.PL loop_ _publ_author_name _publ_author_address 'Yurii, Yablokov' ; Solid State Radiospectroscopy Institute of Molecular Physics Smoluchowskiego 17 Poznan 60-179 POLAND ; 'Maria A. Augustyniak-Jablokow' . 'Serguei Borshch' . 'Daniel, Charles' ;Institut f\"ur Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Germany ; 'Hartl, Hans' ;Institut f\"ur Chemie Freie Universit\"at Berlin Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; EPR study of the magnetic states of mixed-valence VIV4 - VV2 alkoxypolyoxovanadium cluster ; data_nc _database_code_depnum_ccdc_archive 'CCDC 274087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; \m6-oxo-dodeca-\m-methoxo-hexakis(oxovanadium) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 O19 V6' _chemical_formula_weight 790.05 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.8343(12) _cell_length_b 10.0830(6) _cell_length_c 13.5064(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2837.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7344 _cell_measurement_theta_min 4.938 _cell_measurement_theta_max 59.462 _exptl_crystal_description octahedron _exptl_crystal_colour dark _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 1.971 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.413253 _exptl_absorpt_correction_T_max 0.647652 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time '20 sec / frame' _diffrn_standards_decay_% ? _diffrn_reflns_number 32332 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8265 _reflns_number_gt 7402 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.483(14) _refine_ls_number_reflns 8265 _refine_ls_number_parameters 348 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 3.431 _refine_ls_shift/su_mean 0.035 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 V1 V 0.399170(19) 0.98550(3) 0.26777(3) 0.02344(8) Uani 1 1 d . . . V2 V 0.41681(2) 1.24498(4) 0.12812(3) 0.02555(9) Uani 1 1 d . . . V3 V 0.276633(18) 1.17305(4) 0.21923(3) 0.02624(9) Uani 1 1 d . . . V4 V 0.33745(2) 1.16785(4) 0.44175(3) 0.02925(10) Uani 1 1 d . . . V5 V 0.47766(2) 1.23901(4) 0.35138(3) 0.02686(9) Uani 1 1 d . . . V6 V 0.35598(2) 1.42352(4) 0.30259(3) 0.02826(9) Uani 1 1 d . . . O1 O 0.41531(9) 0.83260(16) 0.25604(14) 0.0361(4) Uani 1 1 d . . . O2 O 0.44547(10) 1.2682(2) 0.01982(15) 0.0432(5) Uani 1 1 d . . . O3 O 0.20725(9) 1.1506(2) 0.17286(16) 0.0419(5) Uani 1 1 d . . . O4 O 0.30875(12) 1.1405(2) 0.54940(16) 0.0517(6) Uani 1 1 d . . . O5 O 0.54726(10) 1.2618(2) 0.39822(18) 0.0448(5) Uani 1 1 d . . . O6 O 0.34057(10) 1.57602(18) 0.31590(16) 0.0425(5) Uani 1 1 d . . . O12 O 0.42529(8) 1.04658(17) 0.14059(12) 0.0291(4) Uani 1 1 d . . . O13 O 0.31198(8) 0.98615(15) 0.22031(13) 0.0295(4) Uani 1 1 d . . . O14 O 0.36600(8) 0.98509(16) 0.40041(13) 0.0284(4) Uani 1 1 d . . . O15 O 0.47981(8) 1.04374(17) 0.32154(13) 0.0282(4) Uani 1 1 d . . . O23 O 0.32552(8) 1.21022(17) 0.09527(12) 0.0288(3) Uani 1 1 d . . . O25 O 0.49611(8) 1.26512(18) 0.20799(14) 0.0324(4) Uani 1 1 d . . . O26 O 0.39144(9) 1.42917(16) 0.17069(14) 0.0317(4) Uani 1 1 d . . . O34 O 0.25868(8) 1.14426(19) 0.36165(15) 0.0349(4) Uani 1 1 d . . . O36 O 0.27535(8) 1.37061(17) 0.24503(14) 0.0317(4) Uani 1 1 d . . . O45 O 0.42873(9) 1.20059(17) 0.47422(13) 0.0335(4) Uani 1 1 d . . . O46 O 0.32552(10) 1.36426(19) 0.42829(14) 0.0362(4) Uani 1 1 d . . . O56 O 0.44187(9) 1.42465(16) 0.35388(15) 0.0359(4) Uani 1 1 d . . . O123 O 0.37681(7) 1.20916(15) 0.28494(12) 0.0198(3) Uani 1 1 d . . . C36 C 0.21959(17) 1.4499(4) 0.2476(4) 0.0747(13) Uani 1 1 d . . . H36A H 0.2124 1.4804 0.3140 0.112 Uiso 1 1 calc R . . H36B H 0.1834 1.3985 0.2260 0.112 Uiso 1 1 calc R . . H36C H 0.2250 1.5248 0.2045 0.112 Uiso 1 1 calc R . . C12 C 0.41426(16) 0.9672(3) 0.0540(2) 0.0454(7) Uani 1 1 d . . . H12A H 0.4203 0.8753 0.0701 0.068 Uiso 1 1 calc R . . H12B H 0.4440 0.9924 0.0030 0.068 Uiso 1 1 calc R . . H12C H 0.3712 0.9808 0.0310 0.068 Uiso 1 1 calc R . . C13 C 0.27042(14) 0.8799(3) 0.2509(3) 0.0446(7) Uani 1 1 d . . . H13A H 0.2898 0.7964 0.2345 0.067 Uiso 1 1 calc R . . H13B H 0.2299 0.8877 0.2176 0.067 Uiso 1 1 calc R . . H13C H 0.2638 0.8847 0.3212 0.067 Uiso 1 1 calc R . . C14 C 0.39228(14) 0.8957(3) 0.4733(2) 0.0408(6) Uani 1 1 d . . . H14A H 0.3893 0.8062 0.4495 0.061 Uiso 1 1 calc R . . H14B H 0.3686 0.9039 0.5340 0.061 Uiso 1 1 calc R . . H14C H 0.4365 0.9175 0.4850 0.061 Uiso 1 1 calc R . . C15 C 0.53805(13) 0.9858(3) 0.2832(2) 0.0428(7) Uani 1 1 d . . . H15A H 0.5371 0.8915 0.2930 0.064 Uiso 1 1 calc R . . H15B H 0.5743 1.0226 0.3173 0.064 Uiso 1 1 calc R . . H15C H 0.5415 1.0047 0.2137 0.064 Uiso 1 1 calc R . . C23 C 0.29540(16) 1.2766(3) 0.0152(2) 0.0494(8) Uani 1 1 d . . . H23A H 0.2908 1.3690 0.0309 0.074 Uiso 1 1 calc R . . H23B H 0.2538 1.2386 0.0037 0.074 Uiso 1 1 calc R . . H23C H 0.3212 1.2673 -0.0433 0.074 Uiso 1 1 calc R . . C25 C 0.54974(15) 1.3374(4) 0.1735(3) 0.0609(10) Uani 1 1 d . . . H25A H 0.5530 1.3282 0.1029 0.091 Uiso 1 1 calc R . . H25B H 0.5880 1.3038 0.2040 0.091 Uiso 1 1 calc R . . H25C H 0.5446 1.4294 0.1901 0.091 Uiso 1 1 calc R . . C26 C 0.3939(3) 1.5420(3) 0.1134(3) 0.0947(19) Uani 1 1 d . . . H26A H 0.3512 1.5754 0.1035 0.142 Uiso 1 1 calc R . . H26B H 0.4129 1.5214 0.0505 0.142 Uiso 1 1 calc R . . H26C H 0.4194 1.6080 0.1464 0.142 Uiso 1 1 calc R . . C34 C 0.19681(16) 1.1692(5) 0.4013(3) 0.0699(12) Uani 1 1 d . . . H34A H 0.1998 1.1783 0.4719 0.105 Uiso 1 1 calc R . . H34B H 0.1688 1.0967 0.3855 0.105 Uiso 1 1 calc R . . H34C H 0.1800 1.2496 0.3734 0.105 Uiso 1 1 calc R . . C45 C 0.44279(19) 1.2735(3) 0.5635(2) 0.0552(9) Uani 1 1 d . . . H45A H 0.4396 1.3669 0.5505 0.083 Uiso 1 1 calc R . . H45B H 0.4855 1.2527 0.5853 0.083 Uiso 1 1 calc R . . H45C H 0.4126 1.2494 0.6141 0.083 Uiso 1 1 calc R . . C46 C 0.3025(3) 1.4518(4) 0.5041(3) 0.0868(16) Uani 1 1 d . . . H46A H 0.3212 1.5380 0.4953 0.130 Uiso 1 1 calc R . . H46B H 0.3143 1.4175 0.5679 0.130 Uiso 1 1 calc R . . H46C H 0.2566 1.4584 0.4999 0.130 Uiso 1 1 calc R . . C56 C 0.47895(17) 1.5391(3) 0.3692(3) 0.0607(10) Uani 1 1 d . . . H56A H 0.4907 1.5765 0.3064 0.091 Uiso 1 1 calc R . . H56B H 0.5170 1.5163 0.4055 0.091 Uiso 1 1 calc R . . H56C H 0.4545 1.6027 0.4063 0.091 Uiso 1 1 calc R . . 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 V1 0.02799(18) 0.01554(16) 0.02679(18) 0.00049(15) 0.00244(15) 0.00101(13) V2 0.02736(19) 0.02510(19) 0.02420(19) 0.00637(15) 0.00300(16) -0.00093(15) V3 0.02161(17) 0.0245(2) 0.0326(2) -0.00019(16) -0.00155(16) -0.00011(14) V4 0.0396(2) 0.0262(2) 0.02193(19) 0.00288(15) 0.00759(17) 0.00515(17) V5 0.0278(2) 0.02113(19) 0.0316(2) 0.00313(15) -0.00827(16) -0.00146(14) V6 0.0360(2) 0.01620(16) 0.0326(2) 0.00061(15) -0.00525(17) 0.00348(15) O1 0.0455(10) 0.0191(8) 0.0437(11) 0.0001(7) -0.0003(9) 0.0039(7) O2 0.0460(11) 0.0515(13) 0.0321(10) 0.0144(9) 0.0087(9) -0.0013(9) O3 0.0268(9) 0.0448(11) 0.0543(13) -0.0043(9) -0.0077(9) -0.0021(8) O4 0.0730(15) 0.0509(13) 0.0313(10) 0.0052(9) 0.0188(10) 0.0119(11) O5 0.0370(11) 0.0419(11) 0.0554(13) 0.0101(9) -0.0212(10) -0.0088(8) O6 0.0590(12) 0.0213(8) 0.0472(12) -0.0008(8) -0.0073(10) 0.0072(8) O12 0.0330(9) 0.0283(9) 0.0261(8) -0.0042(7) 0.0034(7) 0.0043(7) O13 0.0315(8) 0.0200(8) 0.0370(10) -0.0011(7) -0.0005(7) -0.0062(6) O14 0.0369(9) 0.0199(8) 0.0285(8) 0.0075(6) 0.0038(7) 0.0012(6) O15 0.0280(8) 0.0246(8) 0.0320(9) 0.0042(7) -0.0011(7) 0.0048(6) O23 0.0322(9) 0.0309(9) 0.0233(8) 0.0019(7) -0.0058(7) 0.0039(7) O25 0.0241(8) 0.0333(9) 0.0399(10) 0.0124(8) 0.0013(7) -0.0073(7) O26 0.0398(10) 0.0210(8) 0.0344(9) 0.0080(7) 0.0019(8) -0.0009(7) O34 0.0269(8) 0.0366(10) 0.0411(10) 0.0033(8) 0.0118(8) 0.0024(7) O36 0.0290(8) 0.0261(8) 0.0400(10) -0.0022(7) -0.0021(7) 0.0098(7) O45 0.0500(11) 0.0268(9) 0.0238(8) -0.0028(7) -0.0090(8) 0.0035(8) O46 0.0543(12) 0.0287(9) 0.0257(9) -0.0056(7) 0.0046(8) 0.0134(8) O56 0.0442(11) 0.0185(8) 0.0450(10) -0.0002(8) -0.0161(9) -0.0033(7) O123 0.0233(6) 0.0148(6) 0.0213(7) 0.0016(5) 0.0014(5) 0.0013(5) C36 0.053(2) 0.0424(18) 0.129(4) -0.004(2) -0.029(2) 0.0241(15) C12 0.0589(19) 0.0448(16) 0.0325(14) -0.0152(12) 0.0063(12) 0.0003(13) C13 0.0397(14) 0.0318(14) 0.0622(19) 0.0058(13) -0.0045(13) -0.0146(11) C14 0.0539(16) 0.0310(13) 0.0374(14) 0.0153(11) 0.0037(12) 0.0079(12) C15 0.0330(13) 0.0432(15) 0.0520(17) 0.0006(13) 0.0019(12) 0.0128(11) C23 0.0512(17) 0.0550(19) 0.0421(16) 0.0179(14) -0.0183(14) -0.0077(14) C25 0.0403(16) 0.090(3) 0.0518(19) 0.0036(19) 0.0079(14) -0.0307(17) C26 0.209(6) 0.0240(16) 0.051(2) 0.0132(15) 0.026(3) -0.003(2) C34 0.0370(16) 0.108(3) 0.065(2) 0.014(2) 0.0246(16) 0.0159(18) C45 0.081(3) 0.0510(19) 0.0331(15) -0.0103(13) -0.0184(16) 0.0095(17) C46 0.155(5) 0.055(2) 0.050(2) -0.0065(18) 0.035(3) 0.041(3) C56 0.061(2) 0.0212(13) 0.100(3) -0.0065(16) -0.028(2) -0.0099(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 V1 O1 1.5858(17) . ? V1 O12 1.9042(18) . ? V1 O14 1.9201(17) . ? V1 O15 1.9222(17) . ? V1 O13 1.9264(17) . ? V1 O123 2.3144(15) . ? V2 O2 1.597(2) . ? V2 O25 1.9836(18) . ? V2 O23 1.9842(18) . ? V2 O26 2.0147(18) . ? V2 O12 2.0152(18) . ? V2 O123 2.3046(16) . ? V3 O3 1.5916(19) . ? V3 O34 1.9810(19) . ? V3 O23 1.9953(18) . ? V3 O36 2.0224(18) . ? V3 O13 2.0234(17) . ? V3 O123 2.2970(16) . ? V4 O4 1.596(2) . ? V4 O45 1.979(2) . ? V4 O34 1.980(2) . ? V4 O46 2.0043(19) . ? V4 O14 2.0153(17) . ? V4 O123 2.3090(16) . ? V5 O5 1.5987(19) . ? V5 O45 1.985(2) . ? V5 O25 1.9919(19) . ? V5 O15 2.0102(17) . ? V5 O56 2.0151(18) . ? V5 O123 2.3043(16) . ? V6 O6 1.5811(19) . ? V6 O46 1.908(2) . ? V6 O56 1.9189(18) . ? V6 O36 1.9263(18) . ? V6 O26 1.9296(19) . ? V6 O123 2.2175(16) . ? O12 C12 1.436(3) . ? O13 C13 1.438(3) . ? O14 C14 1.443(3) . ? O15 C15 1.443(3) . ? O23 C23 1.419(3) . ? O25 C25 1.413(3) . ? O26 C26 1.377(4) . ? O34 C34 1.418(3) . ? O36 C36 1.411(3) . ? O45 C45 1.442(3) . ? O46 C46 1.434(4) . ? O56 C56 1.404(3) . ? 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 _geom_angle_publ_flag O1 V1 O12 99.42(9) . . ? O1 V1 O14 99.64(9) . . ? O12 V1 O14 160.94(7) . . ? O1 V1 O15 98.59(9) . . ? O12 V1 O15 89.55(7) . . ? O14 V1 O15 87.86(7) . . ? O1 V1 O13 99.79(8) . . ? O12 V1 O13 88.18(8) . . ? O14 V1 O13 88.35(8) . . ? O15 V1 O13 161.60(7) . . ? O1 V1 O123 179.37(8) . . ? O12 V1 O123 80.37(6) . . ? O14 V1 O123 80.57(6) . . ? O15 V1 O123 80.81(7) . . ? O13 V1 O123 80.81(6) . . ? O2 V2 O25 99.88(10) . . ? O2 V2 O23 100.34(9) . . ? O25 V2 O23 159.73(8) . . ? O2 V2 O26 102.97(10) . . ? O25 V2 O26 88.22(8) . . ? O23 V2 O26 88.58(7) . . ? O2 V2 O12 100.91(9) . . ? O25 V2 O12 89.04(7) . . ? O23 V2 O12 85.84(7) . . ? O26 V2 O12 156.08(7) . . ? O2 V2 O123 179.07(9) . . ? O25 V2 O123 79.48(7) . . ? O23 V2 O123 80.28(6) . . ? O26 V2 O123 77.72(7) . . ? O12 V2 O123 78.42(6) . . ? O3 V3 O34 100.94(10) . . ? O3 V3 O23 99.21(10) . . ? O34 V3 O23 159.84(7) . . ? O3 V3 O36 101.30(9) . . ? O34 V3 O36 88.54(8) . . ? O23 V3 O36 88.07(8) . . ? O3 V3 O13 101.59(9) . . ? O34 V3 O13 85.71(8) . . ? O23 V3 O13 89.72(7) . . ? O36 V3 O13 157.06(7) . . ? O3 V3 O123 178.98(9) . . ? O34 V3 O123 79.61(7) . . ? O23 V3 O123 80.25(6) . . ? O36 V3 O123 77.84(6) . . ? O13 V3 O123 79.29(6) . . ? O4 V4 O45 100.77(11) . . ? O4 V4 O34 99.58(11) . . ? O45 V4 O34 159.63(8) . . ? O4 V4 O46 101.92(10) . . ? O45 V4 O46 88.54(8) . . ? O34 V4 O46 88.07(8) . . ? O4 V4 O14 101.85(10) . . ? O45 V4 O14 86.00(7) . . ? O34 V4 O14 89.05(8) . . ? O46 V4 O14 156.21(7) . . ? O4 V4 O123 178.74(10) . . ? O45 V4 O123 80.33(7) . . ? O34 V4 O123 79.33(7) . . ? O46 V4 O123 77.45(7) . . ? O14 V4 O123 78.81(6) . . ? O5 V5 O45 99.38(10) . . ? O5 V5 O25 100.99(10) . . ? O45 V5 O25 159.62(7) . . ? O5 V5 O15 101.52(9) . . ? O45 V5 O15 89.30(7) . . ? O25 V5 O15 86.00(7) . . ? O5 V5 O56 101.28(9) . . ? O45 V5 O56 88.70(8) . . ? O25 V5 O56 87.99(8) . . ? O15 V5 O56 157.13(7) . . ? O5 V5 O123 179.13(10) . . ? O45 V5 O123 80.32(7) . . ? O25 V5 O123 79.32(7) . . ? O15 V5 O123 79.30(6) . . ? O56 V5 O123 77.91(6) . . ? O6 V6 O46 97.81(10) . . ? O6 V6 O56 98.20(9) . . ? O46 V6 O56 89.48(9) . . ? O6 V6 O36 97.94(9) . . ? O46 V6 O36 88.99(9) . . ? O56 V6 O36 163.85(8) . . ? O6 V6 O26 98.86(10) . . ? O46 V6 O26 163.33(8) . . ? O56 V6 O26 88.62(9) . . ? O36 V6 O26 88.25(8) . . ? O6 V6 O123 179.44(10) . . ? O46 V6 O123 81.70(7) . . ? O56 V6 O123 82.07(7) . . ? O36 V6 O123 81.80(7) . . ? O26 V6 O123 81.63(7) . . ? C12 O12 V1 120.58(17) . . ? C12 O12 V2 118.12(17) . . ? V1 O12 V2 111.81(8) . . ? C13 O13 V1 118.00(16) . . ? C13 O13 V3 118.48(17) . . ? V1 O13 V3 110.41(7) . . ? C14 O14 V1 120.10(15) . . ? C14 O14 V4 119.62(16) . . ? V1 O14 V4 111.27(8) . . ? C15 O15 V1 118.40(17) . . ? C15 O15 V5 119.17(16) . . ? V1 O15 V5 110.82(8) . . ? C23 O23 V2 120.75(17) . . ? C23 O23 V3 120.18(18) . . ? V2 O23 V3 109.56(8) . . ? C25 O25 V2 122.13(19) . . ? C25 O25 V5 122.79(19) . . ? V2 O25 V5 110.76(8) . . ? C26 O26 V6 123.9(2) . . ? C26 O26 V2 126.3(2) . . ? V6 O26 V2 109.68(8) . . ? C34 O34 V4 121.7(2) . . ? C34 O34 V3 120.8(2) . . ? V4 O34 V3 110.88(8) . . ? C36 O36 V6 123.4(2) . . ? C36 O36 V3 125.0(2) . . ? V6 O36 V3 109.32(8) . . ? C45 O45 V4 117.7(2) . . ? C45 O45 V5 119.7(2) . . ? V4 O45 V5 109.91(8) . . ? C46 O46 V6 123.6(2) . . ? C46 O46 V4 125.8(2) . . ? V6 O46 V4 110.41(9) . . ? C56 O56 V6 124.84(18) . . ? C56 O56 V5 124.22(19) . . ? V6 O56 V5 109.48(8) . . ? V6 O123 V3 91.04(6) . . ? V6 O123 V5 90.53(6) . . ? V3 O123 V5 178.39(8) . . ? V6 O123 V2 90.97(6) . . ? V3 O123 V2 89.90(6) . . ? V5 O123 V2 90.44(6) . . ? V6 O123 V4 90.44(6) . . ? V3 O123 V4 90.18(6) . . ? V5 O123 V4 89.44(6) . . ? V2 O123 V4 178.59(8) . . ? V6 O123 V1 179.47(9) . . ? V3 O123 V1 89.41(6) . . ? V5 O123 V1 89.01(5) . . ? V2 O123 V1 89.30(6) . . ? V4 O123 V1 89.29(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.539 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.071