Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_vo94 _database_code_CSD 187826 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Pessoa, Joao Costa' 'Calhorda, Maria' 'Cavaco, Isabel' 'Correia, Isabel' 'Duarte, M. Teresa' 'Felix, Vitor' 'Henriques, Rui T.' 'Piedale, Maria F. M.' 'Tomaz, Isabel' _publ_contact_author_name 'Dr Joao Costa Pessoa' _publ_contact_author_address ; Centro Quimica Estrutural Instituto Superior Tecnico Av Rovisco Pais Lisboa 1049-001 PORTUGAL ; _publ_contact_author_email 'PCJPESSOA@POPSRV.IST.UTL.PT' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Molecular modelling studies of N-Salicylideneamino acidato complexes of Oxovanadium (IV). Molecular and crystal structure of a new dinuclear LOVIV-O-VvOL mixed valence complex ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 N2 Na O12 V2' _chemical_formula_weight 717.46 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' 'Na' 'Na' 0.0362 0.0249 '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 ? _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.518(5) _cell_length_b 6.425(3) _cell_length_c 18.913(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.523(2) _cell_angle_gamma 90.00 _cell_volume 1574.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 16.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7851 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3938 _reflns_number_gt 3111 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0592P)^2^+0.4188P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 3938 _refine_ls_number_parameters 414 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 H7A H 0.464(6) 0.134(12) 0.087(4) 0.07(3) Uiso 1 1 d D . . H7B H 0.444(14) -0.107(18) 0.093(8) 0.30(11) Uiso 1 1 d D . . O6 O 0.3597(3) -0.0046(9) 0.2076(2) 0.0381(10) Uani 1 1 d . . . O7 O 0.4594(4) 0.0062(9) 0.0627(3) 0.0473(13) Uani 1 1 d D . . VA V 0.45083(7) 0.18122(15) 0.26203(5) 0.0269(2) Uani 1 1 d . . . N1A N 0.4977(3) 0.4893(8) 0.2866(2) 0.0243(11) Uani 1 1 d . . . O1A O 0.5490(3) 0.0575(8) 0.3095(2) 0.0425(11) Uani 1 1 d . . . 02A O 0.4893(3) 0.2757(8) 0.1751(2) 0.0373(11) Uani 1 1 d . . . O3A O 0.5725(3) 0.4894(8) 0.1209(2) 0.0395(11) Uani 1 1 d . . . O4A O 0.3651(3) 0.2249(8) 0.3226(2) 0.0402(11) Uani 1 1 d . . . O5A O 0.2626(4) 0.3814(9) 0.5361(2) 0.0483(14) Uani 1 1 d . . . C1A C 0.5394(4) 0.4472(11) 0.1719(3) 0.0285(13) Uani 1 1 d . . . C2A C 0.5540(4) 0.5866(10) 0.2388(3) 0.0263(12) Uani 1 1 d . . . H2A H 0.5212 0.7207 0.2220 0.032 Uiso 1 1 calc R . . C3A C 0.4822(4) 0.5996(10) 0.3392(3) 0.0294(13) Uani 1 1 d . . . H3A H 0.5086 0.7342 0.3445 0.035 Uiso 1 1 calc R . . C4A C 0.4279(4) 0.5338(10) 0.3904(3) 0.0275(12) Uani 1 1 d . . . C5A C 0.3715(4) 0.3490(10) 0.3793(3) 0.0277(14) Uani 1 1 d . . . C6A C 0.3163(4) 0.2933(11) 0.4289(3) 0.0309(13) Uani 1 1 d . . . H6A H 0.2796 0.1690 0.4221 0.037 Uiso 1 1 calc R . . C7A C 0.3154(4) 0.4177(12) 0.4867(3) 0.0334(14) Uani 1 1 d . . . C8A C 0.3709(4) 0.6081(12) 0.4974(3) 0.0388(17) Uani 1 1 d . . . H8A H 0.3705 0.6936 0.5370 0.047 Uiso 1 1 calc R . . C9A C 0.4247(5) 0.6658(12) 0.4495(3) 0.0379(14) Uani 1 1 d . . . H9A H 0.4595 0.7925 0.4557 0.045 Uiso 1 1 calc R . . C10A C 0.6691(4) 0.6272(10) 0.2774(3) 0.0324(14) Uani 1 1 d . . . H10A H 0.6722 0.6948 0.3245 0.039 Uiso 1 1 calc R . . C11A C 0.7158(5) 0.7818(13) 0.2340(3) 0.0422(16) Uani 1 1 d . . . H11A H 0.7259 0.7114 0.1912 0.051 Uiso 1 1 calc R . . H11B H 0.6671 0.8942 0.2164 0.051 Uiso 1 1 calc R . . C12A C 0.8171(5) 0.8728(16) 0.2781(4) 0.068(3) Uani 1 1 d . . . H12A H 0.8419 0.9678 0.2478 0.103 Uiso 1 1 calc R . . H12B H 0.8665 0.7630 0.2946 0.103 Uiso 1 1 calc R . . H12C H 0.8077 0.9457 0.3200 0.103 Uiso 1 1 calc R . . C13A C 0.7291(5) 0.4283(13) 0.2962(4) 0.0501(19) Uani 1 1 d . . . H13A H 0.6961 0.3390 0.3233 0.075 Uiso 1 1 calc R . . H13B H 0.7980 0.4588 0.3257 0.075 Uiso 1 1 calc R . . H13C H 0.7316 0.3600 0.2516 0.075 Uiso 1 1 calc R . . C14A C 0.2029(5) 0.1978(15) 0.5255(4) 0.053(2) Uani 1 1 d . . . H14A H 0.1689 0.1867 0.5635 0.080 Uiso 1 1 calc R . . H14B H 0.2470 0.0794 0.5276 0.080 Uiso 1 1 calc R . . H14C H 0.1523 0.2025 0.4782 0.080 Uiso 1 1 calc R . . VB V 0.25848(7) -0.19324(15) 0.16472(5) 0.0264(2) Uani 1 1 d . . . N1B N 0.2149(3) -0.5012(8) 0.1391(2) 0.0259(11) Uani 1 1 d . . . O1B O 0.1638(3) -0.0682(8) 0.1143(2) 0.0427(12) Uani 1 1 d . . . O2B O 0.3398(3) -0.2772(8) 0.0983(2) 0.0388(12) Uani 1 1 d . . . O3B O 0.3660(3) -0.4841(8) 0.0126(2) 0.0383(11) Uani 1 1 d . . . O4B O 0.2284(3) -0.2407(7) 0.2549(2) 0.0347(11) Uani 1 1 d . . . O5B O 0.0321(3) -0.4298(10) 0.4176(2) 0.0500(13) Uani 1 1 d . . . C1B C 0.3218(4) -0.4487(10) 0.0587(3) 0.0284(13) Uani 1 1 d . . . C2B C 0.2442(4) -0.5898(10) 0.0757(3) 0.0260(13) Uani 1 1 d . . . H2B H 0.2774 -0.7246 0.0909 0.031 Uiso 1 1 calc R . . C3B C 0.1654(4) -0.6148(10) 0.1731(3) 0.0298(13) Uani 1 1 d . . . H3B H 0.1484 -0.7484 0.1546 0.036 Uiso 1 1 calc R . . C4B C 0.1338(4) -0.5600(9) 0.2352(3) 0.0265(12) Uani 1 1 d . . . C5B C 0.1653(4) -0.3713(10) 0.2735(3) 0.0305(15) Uani 1 1 d . . . C6B C 0.1308(4) -0.3246(12) 0.3345(3) 0.0348(14) Uani 1 1 d D . . H6B H 0.1505 -0.2001 0.3597 0.042 Uiso 1 1 calc RD . . C7B C 0.0679(4) -0.4604(13) 0.3580(3) 0.0382(16) Uani 1 1 d . . . C8B C 0.0370(5) -0.6470(10) 0.3202(3) 0.0371(16) Uani 1 1 d . . . H8B H -0.0065 -0.7376 0.3355 0.045 Uiso 1 1 calc R . . C9B C 0.0708(5) -0.6954(12) 0.2616(3) 0.0381(14) Uani 1 1 d . . . H9B H 0.0518 -0.8223 0.2380 0.046 Uiso 1 1 calc R . . C10B C 0.1507(4) -0.6259(10) 0.0075(3) 0.0296(13) Uani 1 1 d . . . H10B H 0.0971 -0.6934 0.0251 0.036 Uiso 1 1 calc R . . C11B C 0.1776(5) -0.7746(13) -0.0469(3) 0.0477(19) Uani 1 1 d . . . H11C H 0.2227 -0.7033 -0.0707 0.057 Uiso 1 1 calc R . . H11D H 0.2156 -0.8913 -0.0197 0.057 Uiso 1 1 calc R . . C12B C 0.0859(6) -0.8575(16) -0.1057(4) 0.068(3) Uani 1 1 d . . . H12D H 0.1092 -0.9496 -0.1376 0.103 Uiso 1 1 calc R . . H12E H 0.0486 -0.7437 -0.1340 0.103 Uiso 1 1 calc R . . H12F H 0.0415 -0.9320 -0.0829 0.103 Uiso 1 1 calc R . . C13B C 0.1060(5) -0.4258(14) -0.0285(4) 0.0523(19) Uani 1 1 d . . . H13D H 0.0899 -0.3365 0.0074 0.078 Uiso 1 1 calc R . . H13E H 0.0442 -0.4546 -0.0673 0.078 Uiso 1 1 calc R . . H13F H 0.1552 -0.3582 -0.0488 0.078 Uiso 1 1 calc R . . C14B C 0.0678(6) -0.2550(15) 0.4626(4) 0.061(2) Uani 1 1 d . . . H14D H 0.0365 -0.2526 0.5023 0.091 Uiso 1 1 calc R . . H14E H 0.0497 -0.1304 0.4337 0.091 Uiso 1 1 calc R . . H14F H 0.1414 -0.2627 0.4824 0.091 Uiso 1 1 calc R . . Na Na 0.5439(2) 0.7389(5) 0.02647(16) 0.0587(8) 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 O6 0.045(2) 0.032(3) 0.040(2) -0.010(2) 0.0188(18) -0.017(2) O7 0.074(3) 0.032(3) 0.046(3) -0.019(2) 0.034(2) -0.019(3) VA 0.0383(5) 0.0128(5) 0.0309(5) -0.0033(4) 0.0120(4) -0.0042(5) N1A 0.028(2) 0.015(3) 0.031(2) -0.004(2) 0.010(2) -0.002(2) O1A 0.045(2) 0.016(2) 0.061(3) 0.005(2) 0.005(2) -0.001(2) 02A 0.056(3) 0.025(3) 0.035(2) -0.006(2) 0.020(2) -0.017(2) O3A 0.050(3) 0.034(3) 0.038(2) 0.003(2) 0.019(2) -0.008(2) O4A 0.050(2) 0.029(3) 0.049(2) -0.014(2) 0.026(2) -0.016(2) O5A 0.053(3) 0.059(4) 0.040(2) -0.008(3) 0.025(2) -0.014(3) C1A 0.026(3) 0.024(3) 0.032(3) 0.005(3) 0.003(2) -0.002(3) C2A 0.031(3) 0.012(3) 0.034(3) 0.004(3) 0.007(2) 0.000(3) C3A 0.033(3) 0.009(3) 0.044(3) 0.006(3) 0.007(3) 0.001(3) C4A 0.031(3) 0.018(3) 0.035(3) -0.002(3) 0.012(2) -0.002(3) C5A 0.027(3) 0.018(4) 0.035(3) 0.001(3) 0.006(2) 0.003(3) C6A 0.039(3) 0.019(3) 0.038(3) -0.003(3) 0.016(3) -0.001(3) C7A 0.033(3) 0.035(4) 0.033(3) -0.001(3) 0.010(3) -0.003(3) C8A 0.043(3) 0.042(4) 0.034(3) -0.014(3) 0.015(3) -0.002(3) C9A 0.048(3) 0.025(3) 0.039(3) -0.011(3) 0.010(3) -0.001(3) C10A 0.031(3) 0.021(4) 0.042(3) -0.004(3) 0.006(3) -0.008(3) C11A 0.042(3) 0.032(4) 0.055(4) 0.004(4) 0.019(3) -0.009(3) C12A 0.048(4) 0.067(7) 0.088(6) 0.007(5) 0.015(4) -0.020(5) C13A 0.041(4) 0.035(4) 0.068(5) 0.001(4) 0.004(3) 0.005(4) C14A 0.063(4) 0.056(5) 0.047(4) -0.011(4) 0.028(3) -0.020(5) VB 0.0334(5) 0.0127(5) 0.0358(5) -0.0040(5) 0.0140(4) -0.0044(5) N1B 0.029(2) 0.013(3) 0.034(3) -0.007(2) 0.006(2) -0.004(2) O1B 0.049(3) 0.017(3) 0.054(3) -0.004(2) 0.002(2) 0.008(2) O2B 0.045(2) 0.033(3) 0.047(2) -0.020(2) 0.028(2) -0.015(2) O3B 0.044(2) 0.030(3) 0.045(2) -0.015(2) 0.020(2) -0.008(2) O4B 0.047(2) 0.025(3) 0.038(2) -0.008(2) 0.0229(19) -0.015(2) O5B 0.057(3) 0.053(4) 0.050(3) -0.007(3) 0.032(2) -0.013(3) C1B 0.036(3) 0.016(3) 0.034(3) -0.011(3) 0.011(3) -0.009(3) C2B 0.036(3) 0.018(3) 0.027(3) -0.010(3) 0.014(2) 0.001(3) C3B 0.029(3) 0.016(3) 0.044(3) -0.001(3) 0.011(3) 0.000(3) C4B 0.032(3) 0.009(3) 0.040(3) 0.003(3) 0.013(2) -0.002(3) C5B 0.034(3) 0.024(4) 0.037(3) 0.001(3) 0.015(3) -0.001(3) C6B 0.039(3) 0.025(3) 0.042(3) -0.006(3) 0.015(3) -0.006(3) C7B 0.032(3) 0.041(4) 0.045(3) 0.005(3) 0.017(3) -0.003(3) C8B 0.037(3) 0.027(4) 0.048(4) 0.000(3) 0.014(3) -0.017(3) C9B 0.048(3) 0.022(3) 0.046(3) -0.005(3) 0.016(3) -0.007(4) C10B 0.031(3) 0.020(3) 0.038(3) -0.010(3) 0.011(2) -0.007(3) C11B 0.048(4) 0.046(5) 0.049(4) -0.025(4) 0.013(3) -0.010(4) C12B 0.074(5) 0.064(7) 0.064(5) -0.039(5) 0.015(4) -0.014(5) C13B 0.043(4) 0.048(5) 0.054(4) -0.003(4) -0.004(3) 0.008(4) C14B 0.076(5) 0.056(6) 0.062(4) -0.019(4) 0.038(4) -0.016(5) Na 0.100(2) 0.0207(15) 0.0739(19) 0.0008(14) 0.0550(18) 0.0003(16) _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 O6 VA 1.811(5) . ? O6 VB 1.836(5) . ? O7 Na 2.245(6) 2_645 ? O7 Na 2.274(6) 1_545 ? O7 H7A 0.94(7) . ? O7 H7B 0.98(8) . ? VA O1A 1.588(4) . ? VA O4A 1.868(4) . ? VA 02A 1.957(4) . ? VA N1A 2.090(5) . ? N1A C3A 1.286(7) . ? N1A C2A 1.476(7) . ? 02A C1A 1.304(8) . ? O3A C1A 1.203(7) . ? O3A Na 2.349(5) . ? O4A C5A 1.320(7) . ? O5A C7A 1.347(7) . ? O5A C14A 1.411(10) . ? C1A C2A 1.518(8) . ? C2A C10A 1.542(7) . ? C2A H2A 0.9800 . ? C3A C4A 1.436(7) . ? C3A H3A 0.9300 . ? C4A C5A 1.395(8) . ? C4A C9A 1.413(8) . ? C5A C6A 1.401(8) . ? C6A C7A 1.356(8) . ? C6A H6A 0.9300 . ? C7A C8A 1.419(10) . ? C8A C9A 1.366(8) . ? C8A H8A 0.9300 . ? C9A H9A 0.9300 . ? C10A C13A 1.501(9) . ? C10A C11A 1.535(9) . ? C10A H10A 0.9800 . ? C11A C12A 1.505(9) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? VB O1B 1.581(4) . ? VB O4B 1.886(4) . ? VB O2B 1.966(4) . ? VB N1B 2.082(5) . ? N1B C3B 1.281(7) . ? N1B C2B 1.478(6) . ? O2B C1B 1.316(7) . ? O3B C1B 1.212(6) . ? O3B Na 2.388(5) 2_635 ? O3B Na 2.747(5) 1_545 ? O4B C5B 1.314(7) . ? O5B C7B 1.362(7) . ? O5B C14B 1.409(9) . ? C1B C2B 1.489(8) . ? C2B C10B 1.545(7) . ? C2B H2B 0.9800 . ? C3B C4B 1.404(8) . ? C3B H3B 0.9300 . ? C4B C9B 1.405(8) . ? C4B C5B 1.414(8) . ? C5B C6B 1.395(7) . ? C6B C7B 1.377(9) . ? C6B H6B 0.9300 . ? C7B C8B 1.397(10) . ? C8B C9B 1.350(8) . ? C8B H8B 0.9300 . ? C9B H9B 0.9300 . ? C10B C13B 1.500(10) . ? C10B C11B 1.522(8) . ? C10B H10B 0.9800 . ? C11B C12B 1.507(9) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? Na O7 2.245(6) 2_655 ? Na O7 2.274(6) 1_565 ? Na O3B 2.388(5) 2_665 ? Na O3B 2.747(5) 1_565 ? Na Na 3.472(3) 2_645 ? Na Na 3.472(3) 2_655 ? 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 VA O6 VB 170.9(3) . . ? Na O7 Na 100.43(17) 2_645 1_545 ? Na O7 H7A 77(5) 2_645 . ? Na O7 H7A 148(5) 1_545 . ? Na O7 H7B 165(10) 2_645 . ? Na O7 H7B 80(10) 1_545 . ? H7A O7 H7B 111(8) . . ? O1A VA O6 108.4(3) . . ? O1A VA O4A 107.0(2) . . ? O6 VA O4A 90.43(19) . . ? O1A VA 02A 104.6(2) . . ? O6 VA 02A 91.55(19) . . ? O4A VA 02A 145.9(2) . . ? O1A VA N1A 101.3(2) . . ? O6 VA N1A 149.9(2) . . ? O4A VA N1A 85.59(19) . . ? 02A VA N1A 75.93(18) . . ? C3A N1A C2A 117.7(5) . . ? C3A N1A VA 126.0(4) . . ? C2A N1A VA 116.2(3) . . ? C1A 02A VA 124.5(4) . . ? C1A O3A Na 138.1(5) . . ? C5A O4A VA 132.9(4) . . ? C7A O5A C14A 116.2(5) . . ? O3A C1A 02A 123.0(6) . . ? O3A C1A C2A 123.1(6) . . ? 02A C1A C2A 114.0(5) . . ? N1A C2A C1A 107.1(5) . . ? N1A C2A C10A 114.1(4) . . ? C1A C2A C10A 111.7(4) . . ? N1A C2A H2A 107.9 . . ? C1A C2A H2A 107.9 . . ? C10A C2A H2A 107.9 . . ? N1A C3A C4A 125.9(6) . . ? N1A C3A H3A 117.0 . . ? C4A C3A H3A 117.0 . . ? C5A C4A C9A 119.4(5) . . ? C5A C4A C3A 120.8(5) . . ? C9A C4A C3A 119.5(6) . . ? O4A C5A C4A 122.9(5) . . ? O4A C5A C6A 117.8(6) . . ? C4A C5A C6A 119.3(6) . . ? C7A C6A C5A 121.2(6) . . ? C7A C6A H6A 119.4 . . ? C5A C6A H6A 119.4 . . ? O5A C7A C6A 125.7(6) . . ? O5A C7A C8A 114.4(6) . . ? C6A C7A C8A 119.9(5) . . ? C9A C8A C7A 119.9(6) . . ? C9A C8A H8A 120.0 . . ? C7A C8A H8A 120.0 . . ? C8A C9A C4A 120.2(7) . . ? C8A C9A H9A 119.9 . . ? C4A C9A H9A 119.9 . . ? C13A C10A C11A 113.6(5) . . ? C13A C10A C2A 111.9(5) . . ? C11A C10A C2A 111.7(5) . . ? C13A C10A H10A 106.4 . . ? C11A C10A H10A 106.4 . . ? C2A C10A H10A 106.4 . . ? C12A C11A C10A 113.8(6) . . ? C12A C11A H11A 108.8 . . ? C10A C11A H11A 108.8 . . ? C12A C11A H11B 108.8 . . ? C10A C11A H11B 108.8 . . ? H11A C11A H11B 107.7 . . ? C11A C12A H12A 109.5 . . ? C11A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C11A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C10A C13A H13A 109.5 . . ? C10A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C10A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? O5A C14A H14A 109.5 . . ? O5A C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? O5A C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? O1B VB O6 107.8(3) . . ? O1B VB O4B 106.4(2) . . ? O6 VB O4B 91.87(18) . . ? O1B VB O2B 104.9(2) . . ? O6 VB O2B 88.93(19) . . ? O4B VB O2B 146.8(2) . . ? O1B VB N1B 102.5(2) . . ? O6 VB N1B 148.9(2) . . ? O4B VB N1B 86.42(18) . . ? O2B VB N1B 76.28(19) . . ? C3B N1B C2B 119.1(5) . . ? C3B N1B VB 125.3(4) . . ? C2B N1B VB 115.6(4) . . ? C1B O2B VB 123.1(4) . . ? C1B O3B Na 139.6(5) . 2_635 ? C1B O3B Na 115.6(4) . 1_545 ? Na O3B Na 84.79(13) 2_635 1_545 ? C5B O4B VB 132.0(4) . . ? C7B O5B C14B 118.3(6) . . ? O3B C1B O2B 121.2(6) . . ? O3B C1B C2B 124.3(6) . . ? O2B C1B C2B 114.5(5) . . ? N1B C2B C1B 108.0(5) . . ? N1B C2B C10B 113.0(4) . . ? C1B C2B C10B 111.7(5) . . ? N1B C2B H2B 108.0 . . ? C1B C2B H2B 108.0 . . ? C10B C2B H2B 108.0 . . ? N1B C3B C4B 127.2(6) . . ? N1B C3B H3B 116.4 . . ? C4B C3B H3B 116.4 . . ? C3B C4B C9B 120.1(6) . . ? C3B C4B C5B 121.6(5) . . ? C9B C4B C5B 118.3(5) . . ? O4B C5B C6B 118.7(6) . . ? O4B C5B C4B 122.3(5) . . ? C6B C5B C4B 119.0(6) . . ? C7B C6B C5B 120.9(7) . . ? C7B C6B H6B 119.6 . . ? C5B C6B H6B 119.6 . . ? O5B C7B C6B 124.9(7) . . ? O5B C7B C8B 115.0(6) . . ? C6B C7B C8B 120.1(6) . . ? C9B C8B C7B 119.7(6) . . ? C9B C8B H8B 120.1 . . ? C7B C8B H8B 120.1 . . ? C8B C9B C4B 122.0(6) . . ? C8B C9B H9B 119.0 . . ? C4B C9B H9B 119.0 . . ? C13B C10B C11B 111.9(5) . . ? C13B C10B C2B 112.3(5) . . ? C11B C10B C2B 111.3(5) . . ? C13B C10B H10B 107.0 . . ? C11B C10B H10B 107.0 . . ? C2B C10B H10B 107.0 . . ? C12B C11B C10B 114.6(6) . . ? C12B C11B H11C 108.6 . . ? C10B C11B H11C 108.6 . . ? C12B C11B H11D 108.6 . . ? C10B C11B H11D 108.6 . . ? H11C C11B H11D 107.6 . . ? C11B C12B H12D 109.5 . . ? C11B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C10B C13B H13D 109.5 . . ? C10B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C10B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? O5B C14B H14D 109.5 . . ? O5B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? O5B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? O7 Na O7 145.60(17) 2_655 1_565 ? O7 Na O3A 94.6(2) 2_655 . ? O7 Na O3A 105.9(2) 1_565 . ? O7 Na O3B 99.6(2) 2_655 2_665 ? O7 Na O3B 82.8(2) 1_565 2_665 ? O3A Na O3B 139.1(2) . 2_665 ? O7 Na O3B 75.57(18) 2_655 1_565 ? O7 Na O3B 85.49(19) 1_565 1_565 ? O3A Na O3B 70.53(16) . 1_565 ? O3B Na O3B 150.26(17) 2_665 1_565 ? O7 Na Na 40.10(14) 2_655 2_645 ? O7 Na Na 128.7(2) 1_565 2_645 ? O3A Na Na 63.67(13) . 2_645 ? O3B Na Na 139.72(18) 2_665 2_645 ? O3B Na Na 43.23(12) 1_565 2_645 ? O7 Na Na 117.9(2) 2_655 2_655 ? O7 Na Na 39.47(14) 1_565 2_655 ? O3A Na Na 145.04(18) . 2_655 ? O3B Na Na 51.98(12) 2_665 2_655 ? O3B Na Na 103.69(18) 1_565 2_655 ? Na Na Na 135.4(2) 2_645 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag VB O6 VA O1A 92(2) . . . . ? VB O6 VA O4A -16(2) . . . . ? VB O6 VA 02A -162(2) . . . . ? VB O6 VA N1A -98(2) . . . . ? O1A VA N1A C3A -91.2(5) . . . . ? O6 VA N1A C3A 98.5(6) . . . . ? O4A VA N1A C3A 15.3(5) . . . . ? 02A VA N1A C3A 166.4(5) . . . . ? O1A VA N1A C2A 88.5(4) . . . . ? O6 VA N1A C2A -81.7(5) . . . . ? O4A VA N1A C2A -165.0(4) . . . . ? 02A VA N1A C2A -13.8(4) . . . . ? O1A VA 02A C1A -86.0(5) . . . . ? O6 VA 02A C1A 164.5(5) . . . . ? O4A VA 02A C1A 71.5(6) . . . . ? N1A VA 02A C1A 12.3(5) . . . . ? O1A VA O4A C5A 72.7(6) . . . . ? O6 VA O4A C5A -177.9(6) . . . . ? 02A VA O4A C5A -84.5(6) . . . . ? N1A VA O4A C5A -27.8(6) . . . . ? Na O3A C1A 02A 114.5(7) . . . . ? Na O3A C1A C2A -66.8(8) . . . . ? VA 02A C1A O3A 171.0(4) . . . . ? VA 02A C1A C2A -7.8(7) . . . . ? C3A N1A C2A C1A -166.6(5) . . . . ? VA N1A C2A C1A 13.7(5) . . . . ? C3A N1A C2A C10A 69.3(7) . . . . ? VA N1A C2A C10A -110.5(5) . . . . ? O3A C1A C2A N1A 176.6(5) . . . . ? 02A C1A C2A N1A -4.5(7) . . . . ? O3A C1A C2A C10A -57.8(8) . . . . ? 02A C1A C2A C10A 121.1(5) . . . . ? C2A N1A C3A C4A 179.0(5) . . . . ? VA N1A C3A C4A -1.3(8) . . . . ? N1A C3A C4A C5A -10.7(9) . . . . ? N1A C3A C4A C9A 174.4(6) . . . . ? VA O4A C5A C4A 24.9(9) . . . . ? VA O4A C5A C6A -157.0(4) . . . . ? C9A C4A C5A O4A 175.4(5) . . . . ? C3A C4A C5A O4A 0.4(9) . . . . ? C9A C4A C5A C6A -2.7(9) . . . . ? C3A C4A C5A C6A -177.6(5) . . . . ? O4A C5A C6A C7A -177.1(5) . . . . ? C4A C5A C6A C7A 1.1(9) . . . . ? C14A O5A C7A C6A -0.5(9) . . . . ? C14A O5A C7A C8A 177.4(6) . . . . ? C5A C6A C7A O5A 178.0(6) . . . . ? C5A C6A C7A C8A 0.2(9) . . . . ? O5A C7A C8A C9A -177.9(6) . . . . ? C6A C7A C8A C9A 0.1(9) . . . . ? C7A C8A C9A C4A -1.8(9) . . . . ? C5A C4A C9A C8A 3.1(9) . . . . ? C3A C4A C9A C8A 178.1(6) . . . . ? N1A C2A C10A C13A 67.8(7) . . . . ? C1A C2A C10A C13A -53.8(7) . . . . ? N1A C2A C10A C11A -163.6(5) . . . . ? C1A C2A C10A C11A 74.8(7) . . . . ? C13A C10A C11A C12A -68.5(8) . . . . ? C2A C10A C11A C12A 163.8(6) . . . . ? VA O6 VB O1B 94(2) . . . . ? VA O6 VB O4B -14(2) . . . . ? VA O6 VB O2B -161(2) . . . . ? VA O6 VB N1B -100(2) . . . . ? O1B VB N1B C3B -91.3(5) . . . . ? O6 VB N1B C3B 102.3(6) . . . . ? O4B VB N1B C3B 14.7(5) . . . . ? O2B VB N1B C3B 166.1(5) . . . . ? O1B VB N1B C2B 88.1(4) . . . . ? O6 VB N1B C2B -78.2(5) . . . . ? O4B VB N1B C2B -165.9(4) . . . . ? O2B VB N1B C2B -14.5(4) . . . . ? O1B VB O2B C1B -86.7(5) . . . . ? O6 VB O2B C1B 165.2(5) . . . . ? O4B VB O2B C1B 73.4(6) . . . . ? N1B VB O2B C1B 12.7(5) . . . . ? O1B VB O4B C5B 75.5(6) . . . . ? O6 VB O4B C5B -175.3(6) . . . . ? O2B VB O4B C5B -84.4(6) . . . . ? N1B VB O4B C5B -26.4(5) . . . . ? Na O3B C1B O2B 132.9(6) 2_635 . . . ? Na O3B C1B O2B 18.9(8) 1_545 . . . ? Na O3B C1B C2B -47.0(9) 2_635 . . . ? Na O3B C1B C2B -161.1(5) 1_545 . . . ? VB O2B C1B O3B 172.0(4) . . . . ? VB O2B C1B C2B -8.1(7) . . . . ? C3B N1B C2B C1B -166.1(5) . . . . ? VB N1B C2B C1B 14.4(6) . . . . ? C3B N1B C2B C10B 69.9(7) . . . . ? VB N1B C2B C10B -109.6(5) . . . . ? O3B C1B C2B N1B 175.2(6) . . . . ? O2B C1B C2B N1B -4.8(7) . . . . ? O3B C1B C2B C10B -60.0(8) . . . . ? O2B C1B C2B C10B 120.0(5) . . . . ? C2B N1B C3B C4B 178.1(5) . . . . ? VB N1B C3B C4B -2.5(9) . . . . ? N1B C3B C4B C9B 173.6(6) . . . . ? N1B C3B C4B C5B -7.6(10) . . . . ? VB O4B C5B C6B -157.0(4) . . . . ? VB O4B C5B C4B 24.9(9) . . . . ? C3B C4B C5B O4B -2.4(9) . . . . ? C9B C4B C5B O4B 176.4(6) . . . . ? C3B C4B C5B C6B 179.5(6) . . . . ? C9B C4B C5B C6B -1.6(9) . . . . ? O4B C5B C6B C7B -177.4(6) . . . . ? C4B C5B C6B C7B 0.7(9) . . . . ? C14B O5B C7B C6B -5.2(10) . . . . ? C14B O5B C7B C8B 174.0(6) . . . . ? C5B C6B C7B O5B 178.7(6) . . . . ? C5B C6B C7B C8B -0.5(10) . . . . ? O5B C7B C8B C9B -178.0(6) . . . . ? C6B C7B C8B C9B 1.3(10) . . . . ? C7B C8B C9B C4B -2.3(10) . . . . ? C3B C4B C9B C8B -178.7(6) . . . . ? C5B C4B C9B C8B 2.5(9) . . . . ? N1B C2B C10B C13B 71.1(7) . . . . ? C1B C2B C10B C13B -50.8(7) . . . . ? N1B C2B C10B C11B -162.5(5) . . . . ? C1B C2B C10B C11B 75.5(7) . . . . ? C13B C10B C11B C12B -67.0(9) . . . . ? C2B C10B C11B C12B 166.4(7) . . . . ? C1A O3A Na O7 -133.7(6) . . . 2_655 ? C1A O3A Na O7 18.4(7) . . . 1_565 ? C1A O3A Na O3B 115.9(6) . . . 2_665 ? C1A O3A Na O3B -60.8(6) . . . 1_565 ? C1A O3A Na Na -107.3(6) . . . 2_645 ? C1A O3A Na Na 25.4(8) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.815 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.081