# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_V10O18L'4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H122 N6 Na6 O84 P8 V10' _chemical_formula_sum 'C56 H122 N6 Na6 O84 P8 V10' _chemical_formula_weight 3118.69 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' P P 0.1023 0.0942 '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' Na Na 0.0362 0.0249 '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' _space_group_crystal_system tetragonal _space_group_IT_number 128 _space_group_name_H-M_alt 'P 4/m n c' _space_group_name_Hall '-P 4 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 12.4314(6) _cell_length_b 12.4314(6) _cell_length_c 43.467(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6717.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7647 _cell_measurement_theta_min 2.1586 _cell_measurement_theta_max 26.4023 _exptl_crystal_description octahedron _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_F_000 3176 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 0.880 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.875436 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed X-ray tube' _diffrn_measurement_device_type 'Bruker APEX I CCD' _diffrn_measurement_method 'omega or psi scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 86381 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 0.937 _diffrn_reflns_theta_max 28.297 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 4259 _reflns_number_gt 3406 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SMART APEX software' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1807P)^2^+21.3835P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4259 _refine_ls_number_parameters 191 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.2810 _refine_ls_wR_factor_gt 0.2647 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.141 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.59981(6) 0.68394(6) 0.81043(2) 0.0230(3) Uani 1 1 d . . . . . V2 V 0.5000 0.5000 0.77976(3) 0.0186(3) Uani 1 4 d S T P . . P3 P 0.40826(10) 0.80311(10) 0.84814(3) 0.0226(3) Uani 1 1 d . . . . . C1 C 0.4083(5) 0.8211(4) 0.88912(9) 0.0408(15) Uani 1 1 d DG . . . . C2 C 0.5002(5) 0.8528(8) 0.90492(13) 0.034(3) Uiso 0.3333 1 d DG . P A 1 H2 H 0.5643 0.8688 0.8939 0.041 Uiso 0.3333 1 calc R U P A 1 C3 C 0.4984(6) 0.8612(9) 0.93680(13) 0.036(3) Uiso 0.3333 1 d DG . P A 1 H3 H 0.5612 0.8829 0.9476 0.043 Uiso 0.3333 1 calc R U P A 1 C4 C 0.4046(7) 0.8378(6) 0.95289(9) 0.086(4) Uani 1 1 d DG . . A . C5 C 0.3127(6) 0.8060(10) 0.93709(14) 0.038(4) Uiso 0.3333 1 d DG . P A 1 H5 H 0.2486 0.7901 0.9481 0.045 Uiso 0.3333 1 calc R U P A 1 C6 C 0.3146(5) 0.7977(9) 0.90520(13) 0.033(3) Uiso 0.3333 1 d DG . P A 1 H6 H 0.2518 0.7760 0.8944 0.040 Uiso 0.3333 1 calc R U P A 1 C2' C 0.5076(11) 0.7942(12) 0.9052(3) 0.035(3) Uiso 0.3333 1 d D . P A 2 H2' H 0.5706 0.7710 0.8947 0.042 Uiso 0.3333 1 calc R U P A 2 C3' C 0.5031(13) 0.8054(15) 0.9376(4) 0.052(5) Uiso 0.3333 1 d D . P A 2 H3' H 0.5656 0.7913 0.9496 0.063 Uiso 0.3333 1 calc R U P A 2 C5' C 0.3198(14) 0.8665(19) 0.9370(4) 0.058(5) Uiso 0.3333 1 d D . P A 2 H5' H 0.2554 0.8910 0.9465 0.069 Uiso 0.3333 1 calc R U P A 2 C6' C 0.3303(12) 0.8587(14) 0.9061(3) 0.038(4) Uiso 0.3333 1 d D . P A 2 H6' H 0.2705 0.8853 0.8948 0.045 Uiso 0.3333 1 calc R U P A 2 C3" C 0.4456(18) 0.9203(16) 0.9369(4) 0.076(7) Uiso 0.3333 1 d D . P A 3 H3" H 0.4690 0.9857 0.9460 0.092 Uiso 0.3333 1 calc R U P A 3 C2" C 0.4501(14) 0.8998(13) 0.9060(4) 0.054(5) Uiso 0.3333 1 d D . P A 3 H2" H 0.4902 0.9511 0.8946 0.065 Uiso 0.3333 1 calc R U P A 3 C6" C 0.336(2) 0.759(2) 0.9065(5) 0.075(8) Uiso 0.3333 1 d D . P A 3 H6" H 0.2903 0.7091 0.8964 0.090 Uiso 0.3333 1 calc R U P A 3 C5" C 0.332(2) 0.769(3) 0.9381(6) 0.094(10) Uiso 0.3333 1 d D . P A 3 H5" H 0.2807 0.7297 0.9497 0.112 Uiso 0.3333 1 calc R U P A 3 C7 C 0.4025(13) 0.8410(9) 0.98589(16) 0.113(5) Uani 1 1 d . . . . . O1 O 0.6500(3) 0.7651(3) 0.78560(9) 0.0316(8) Uani 1 1 d . . . . . O2 O 0.4602(2) 0.6363(2) 0.79387(7) 0.0199(6) Uani 1 1 d . . . . . O3 O 0.5000 0.5000 0.74267(14) 0.0267(14) Uani 1 4 d S T P . . O4 O 0.7067(3) 0.6668(3) 0.84248(7) 0.0280(8) Uani 1 1 d . . . . . O5 O 0.5247(3) 0.7772(3) 0.83983(8) 0.0287(8) Uani 1 1 d . . . . . O6 O 0.3684(3) 0.9044(3) 0.83285(8) 0.0315(8) Uani 1 1 d . . . . . O7 O 0.5000 1.0000 0.78903(11) 0.0290(10) Uani 1 2 d S T P . . O8 O 0.3457(6) 0.3847(5) 0.6882(2) 0.096(3) Uani 1 1 d . . . . . O9 O 0.3480(7) 0.5492(7) 0.5958(3) 0.136(4) Uani 1 1 d . . . . . O10 O 0.7196(4) 1.0633(4) 0.75558(11) 0.0519(12) Uiso 1 1 d . . . . . O11 O 0.2888(4) 0.0886(3) 0.85621(14) 0.0549(13) Uani 1 1 d . . . . . O12 O 0.175(6) 1.050(6) 1.0000 0.33(4) Uiso 0.5 2 d S . P . . O13 O 0.5000 0.5000 0.6291(18) 0.53(5) Uiso 1 4 d S . P . . Na1 Na 0.59574(17) 0.90426(17) 0.7500 0.0343(7) Uani 1 2 d S T P . . Na2 Na 0.5000 0.5000 0.68522(14) 0.0633(16) Uani 1 4 d S T P . . N1 N 0.5000 0.5000 0.8492(2) 0.066(4) Uani 1 4 d S T P . . N2 N 0.5000 0.5000 0.8749(3) 0.170(13) Uani 1 4 d S T P . . N3 N 0.5000 0.5000 0.9027(3) 0.095(6) Uani 1 4 d S T P . . 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 0.0235(4) 0.0218(4) 0.0238(4) -0.0015(3) -0.0033(3) 0.0001(3) V2 0.0205(5) 0.0205(5) 0.0149(6) 0.000 0.000 0.000 P3 0.0305(6) 0.0220(6) 0.0152(6) -0.0016(4) -0.0001(4) 0.0011(4) C1 0.078(5) 0.027(3) 0.018(2) -0.0007(19) 0.000(2) -0.005(3) C4 0.178(11) 0.055(5) 0.025(3) -0.009(3) 0.007(5) -0.030(6) C7 0.238(15) 0.082(6) 0.017(3) -0.008(4) 0.000(5) -0.027(8) O1 0.0306(18) 0.0289(18) 0.0355(19) 0.0054(15) -0.0068(15) -0.0022(14) O2 0.0216(15) 0.0198(15) 0.0182(14) -0.0002(11) 0.0004(11) -0.0005(11) O3 0.032(2) 0.032(2) 0.016(3) 0.000 0.000 0.000 O4 0.0299(18) 0.0310(18) 0.0231(16) -0.0047(14) -0.0065(13) 0.0039(14) O5 0.0279(17) 0.0258(17) 0.0325(17) -0.0087(14) -0.0041(14) 0.0017(13) O6 0.036(2) 0.0301(18) 0.0286(17) 0.0063(14) 0.0004(15) 0.0077(15) O7 0.041(3) 0.023(2) 0.022(2) 0.000 0.000 0.006(2) O8 0.078(4) 0.050(3) 0.159(7) 0.012(4) -0.050(5) -0.013(3) O9 0.094(6) 0.102(7) 0.212(12) -0.012(7) 0.036(7) 0.008(5) O11 0.053(3) 0.027(2) 0.085(4) -0.003(2) 0.004(3) -0.0071(18) Na1 0.0366(10) 0.0366(10) 0.0296(14) 0.0063(9) 0.0063(9) 0.0121(12) Na2 0.069(3) 0.069(3) 0.051(3) 0.000 0.000 0.000 N1 0.097(6) 0.097(6) 0.005(4) 0.000 0.000 0.000 N2 0.24(2) 0.24(2) 0.023(7) 0.000 0.000 0.000 N3 0.132(10) 0.132(10) 0.022(5) 0.000 0.000 0.000 _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 1.604(4) . ? V1 O4 1.937(3) . ? V1 O5 1.962(4) . ? V1 O2 1.970(3) . ? V1 O2 1.984(3) 4_565 ? V1 V2 2.9232(10) . ? V2 O3 1.612(6) . ? V2 O2 1.868(3) 4_565 ? V2 O2 1.868(3) 3_655 ? V2 O2 1.868(3) 2_665 ? V2 O2 1.868(3) . ? V2 V1 2.9232(10) 4_565 ? V2 V1 2.9232(10) 2_665 ? V2 V1 2.9232(10) 3_655 ? P3 O6 1.508(4) . ? P3 O5 1.527(4) . ? P3 O4 1.538(4) 3_655 ? P3 C1 1.795(4) . ? C1 C6' 1.307(12) . ? C1 C2" 1.330(13) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C6" 1.403(14) . ? C1 C2' 1.456(12) . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5' 1.310(13) . ? C4 C3" 1.340(14) . ? C4 C5 1.3900 . ? C4 C5" 1.397(15) . ? C4 C7 1.435(8) . ? C4 C3' 1.450(13) . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C2' C3' 1.419(13) . ? C2' H2' 0.9500 . ? C3' H3' 0.9500 . ? C5' C6' 1.351(13) . ? C5' H5' 0.9500 . ? C6' H6' 0.9500 . ? C3" C2" 1.366(14) . ? C3" H3" 0.9500 . ? C2" H2" 0.9500 . ? C6" C5" 1.382(14) . ? C6" H6" 0.9500 . ? C5" H5" 0.9500 . ? C7 C7 1.227(14) 10_557 ? O1 Na1 2.417(4) . ? O2 V1 1.984(3) 3_655 ? O3 Na2 2.497(9) . ? O4 P3 1.538(4) 4_565 ? O7 Na1 2.390(4) 2_675 ? O7 Na1 2.390(4) . ? O8 Na2 2.398(7) . ? O10 Na1 2.518(5) . ? O13 Na2 2.44(8) . ? Na1 O7 2.390(4) 7_456 ? Na1 O1 2.417(4) 8_666 ? Na1 O10 2.518(5) 8_666 ? Na1 Na1 3.366(6) 2_675 ? Na2 O8 2.398(7) 2_665 ? Na2 O8 2.398(7) 4_565 ? Na2 O8 2.398(7) 3_655 ? N1 N2 1.116(18) . ? N2 N3 1.212(18) . ? 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 O4 106.62(18) . . ? O1 V1 O5 104.57(18) . . ? O4 V1 O5 85.58(15) . . ? O1 V1 O2 106.63(16) . . ? O4 V1 O2 146.52(15) . . ? O5 V1 O2 89.82(14) . . ? O1 V1 O2 103.62(17) . 4_565 ? O4 V1 O2 90.27(14) . 4_565 ? O5 V1 O2 151.52(15) . 4_565 ? O2 V1 O2 78.28(18) . 4_565 ? O1 V1 V2 110.52(14) . . ? O4 V1 V2 122.21(11) . . ? O5 V1 V2 123.88(11) . . ? O2 V1 V2 39.12(9) . . ? O2 V1 V2 39.18(9) 4_565 . ? O3 V2 O2 109.16(10) . 4_565 ? O3 V2 O2 109.16(10) . 3_655 ? O2 V2 O2 141.68(19) 4_565 3_655 ? O3 V2 O2 109.16(10) . 2_665 ? O2 V2 O2 83.82(6) 4_565 2_665 ? O2 V2 O2 83.82(6) 3_655 2_665 ? O3 V2 O2 109.16(10) . . ? O2 V2 O2 83.82(6) 4_565 . ? O2 V2 O2 83.82(6) 3_655 . ? O2 V2 O2 141.69(19) 2_665 . ? O3 V2 V1 117.13(3) . . ? O2 V2 V1 42.14(9) 4_565 . ? O2 V2 V1 116.24(10) 3_655 . ? O2 V2 V1 116.58(10) 2_665 . ? O2 V2 V1 41.69(10) . . ? O3 V2 V1 117.13(3) . 4_565 ? O2 V2 V1 41.69(9) 4_565 4_565 ? O2 V2 V1 116.58(10) 3_655 4_565 ? O2 V2 V1 42.14(10) 2_665 4_565 ? O2 V2 V1 116.24(10) . 4_565 ? V1 V2 V1 78.00(2) . 4_565 ? O3 V2 V1 117.13(3) . 2_665 ? O2 V2 V1 116.24(10) 4_565 2_665 ? O2 V2 V1 42.14(9) 3_655 2_665 ? O2 V2 V1 41.69(10) 2_665 2_665 ? O2 V2 V1 116.58(10) . 2_665 ? V1 V2 V1 125.74(6) . 2_665 ? V1 V2 V1 78.00(2) 4_565 2_665 ? O3 V2 V1 117.13(3) . 3_655 ? O2 V2 V1 116.58(10) 4_565 3_655 ? O2 V2 V1 41.69(9) 3_655 3_655 ? O2 V2 V1 116.24(10) 2_665 3_655 ? O2 V2 V1 42.14(10) . 3_655 ? V1 V2 V1 78.00(2) . 3_655 ? V1 V2 V1 125.74(6) 4_565 3_655 ? V1 V2 V1 78.00(2) 2_665 3_655 ? O6 P3 O5 112.6(2) . . ? O6 P3 O4 112.4(2) . 3_655 ? O5 P3 O4 111.9(2) . 3_655 ? O6 P3 C1 109.5(2) . . ? O5 P3 C1 105.1(2) . . ? O4 P3 C1 104.8(2) 3_655 . ? C2 C1 C6 120.0 . . ? C2" C1 C6" 110.9(14) . . ? C6' C1 C2' 116.1(10) . . ? C6' C1 P3 127.3(8) . . ? C2" C1 P3 129.8(10) . . ? C2 C1 P3 121.7(4) . . ? C6 C1 P3 118.2(3) . . ? C6" C1 P3 117.7(11) . . ? C2' C1 P3 116.6(7) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C3" C4 C5" 118.3(16) . . ? C5' C4 C7 120.3(12) . . ? C3" C4 C7 120.3(11) . . ? C5 C4 C7 119.1(8) . . ? C3 C4 C7 120.8(8) . . ? C5" C4 C7 117.7(13) . . ? C5' C4 C3' 121.0(11) . . ? C7 C4 C3' 118.7(11) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C3' C2' C1 114.9(13) . . ? C3' C2' H2' 122.6 . . ? C1 C2' H2' 122.6 . . ? C2' C3' C4 121.0(14) . . ? C2' C3' H3' 119.5 . . ? C4 C3' H3' 119.5 . . ? C4 C5' C6' 115.2(16) . . ? C4 C5' H5' 122.4 . . ? C6' C5' H5' 122.4 . . ? C1 C6' C5' 131.3(15) . . ? C1 C6' H6' 114.4 . . ? C5' C6' H6' 114.4 . . ? C4 C3" C2" 112.5(18) . . ? C4 C3" H3" 123.7 . . ? C2" C3" H3" 123.7 . . ? C1 C2" C3" 131.6(19) . . ? C1 C2" H2" 114.2 . . ? C3" C2" H2" 114.2 . . ? C5" C6" C1 121(2) . . ? C5" C6" H6" 119.7 . . ? C1 C6" H6" 119.7 . . ? C6" C5" C4 119(2) . . ? C6" C5" H5" 120.4 . . ? C4 C5" H5" 120.4 . . ? C7 C7 C4 178.1(7) 10_557 . ? V1 O1 Na1 140.6(2) . . ? V2 O2 V1 99.19(14) . . ? V2 O2 V1 98.68(14) . 3_655 ? V1 O2 V1 137.04(16) . 3_655 ? V2 O3 Na2 180.0 . . ? P3 O4 V1 135.7(2) 4_565 . ? P3 O5 V1 136.9(2) . . ? Na1 O7 Na1 89.55(19) 2_675 . ? O7 Na1 O7 90.46(19) . 7_456 ? O7 Na1 O1 92.35(12) . . ? O7 Na1 O1 161.80(9) 7_456 . ? O7 Na1 O1 161.80(9) . 8_666 ? O7 Na1 O1 92.35(12) 7_456 8_666 ? O1 Na1 O1 90.6(2) . 8_666 ? O7 Na1 O10 81.09(12) . . ? O7 Na1 O10 88.97(13) 7_456 . ? O1 Na1 O10 109.23(16) . . ? O1 Na1 O10 80.99(15) 8_666 . ? O7 Na1 O10 88.97(13) . 8_666 ? O7 Na1 O10 81.09(12) 7_456 8_666 ? O1 Na1 O10 80.99(15) . 8_666 ? O1 Na1 O10 109.23(16) 8_666 8_666 ? O10 Na1 O10 165.9(3) . 8_666 ? O7 Na1 Na1 45.23(9) . 2_675 ? O7 Na1 Na1 45.23(9) 7_456 2_675 ? O1 Na1 Na1 134.71(11) . 2_675 ? O1 Na1 Na1 134.71(11) 8_666 2_675 ? O10 Na1 Na1 82.95(13) . 2_675 ? O10 Na1 Na1 82.95(13) 8_666 2_675 ? O8 Na2 O8 173.8(5) . 2_665 ? O8 Na2 O8 89.84(3) . 4_565 ? O8 Na2 O8 89.83(3) 2_665 4_565 ? O8 Na2 O8 89.83(3) . 3_655 ? O8 Na2 O8 89.83(3) 2_665 3_655 ? O8 Na2 O8 173.8(5) 4_565 3_655 ? O8 Na2 O13 93.1(3) . . ? O8 Na2 O13 93.1(3) 2_665 . ? O8 Na2 O13 93.1(3) 4_565 . ? O8 Na2 O13 93.1(3) 3_655 . ? O8 Na2 O3 86.9(3) . . ? O8 Na2 O3 86.9(3) 2_665 . ? O8 Na2 O3 86.9(3) 4_565 . ? O8 Na2 O3 86.9(3) 3_655 . ? O13 Na2 O3 180.0 . . ? N1 N2 N3 180.0 . . ? _refine_diff_density_max 1.872 _refine_diff_density_min -1.349 _refine_diff_density_rms 0.383 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 970548' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_V10O18L"4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H118 N6 Na6 O82 P8 V10' _chemical_formula_sum 'C64 H118 N6 Na6 O82 P8 V10' _chemical_formula_weight 3178.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system tetragonal _space_group_IT_number 128 _space_group_name_H-M_alt 'P 4/m n c' _space_group_name_Hall '-P 4 2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_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' 'y+1/2, x+1/2, -z+1/2' 'y, -x, z' '-y, x, z' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' '-y, x, -z' 'y, -x, -z' 'y-1/2, x-1/2, z-1/2' _cell_length_a 12.144(3) _cell_length_b 12.144(3) _cell_length_c 49.317(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7273(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 476 _cell_measurement_theta_min 2.4779 _cell_measurement_theta_max 18.6595 _exptl_crystal_description Prism _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_F_000 3232 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 0.813 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.467147 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed X-ray tube' _diffrn_measurement_device_type 'Bruker APEX I CCD' _diffrn_measurement_method 'omega or phi scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9094 _diffrn_reflns_av_unetI/netI 0.2131 _diffrn_reflns_av_R_equivalents 0.2219 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 0.826 _diffrn_reflns_theta_max 22.456 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.718 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.718 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.718 _reflns_number_total 2415 _reflns_number_gt 1019 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APRX I software' _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS - 97' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2415 _refine_ls_number_parameters 197 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.2415 _refine_ls_R_factor_gt 0.1287 _refine_ls_wR_factor_ref 0.3677 _refine_ls_wR_factor_gt 0.3085 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.994 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group V1 V -0.5000 0.5000 0.72053(10) 0.0272(16) Uani 1 4 d S T P . . V2 V -0.3969(3) 0.3117(3) 0.69338(5) 0.0342(10) Uani 1 1 d . . . . . P3 P -0.5914(5) 0.1904(5) 0.65994(8) 0.0379(14) Uani 1 1 d . . . . . O1 O -0.2872(10) 0.3298(10) 0.66469(18) 0.033(3) Uani 1 1 d . . . . . O2 O -0.3591(10) 0.4601(9) 0.70829(18) 0.031(3) Uani 1 1 d . . . . . O3 O -0.3471(11) 0.2280(10) 0.7153(2) 0.042(4) Uani 1 1 d . . . . . O4 O -0.5000 0.5000 0.7518(4) 0.031(6) Uani 1 4 d S TU P . . O5 O -0.4741(10) 0.2174(10) 0.6675(2) 0.038(4) Uani 1 1 d . . . . . O6 O -0.6331(12) 0.0849(12) 0.6729(2) 0.056(4) Uani 1 1 d . . . . . O7 O -0.5573(10) 0.2170(10) 0.7537(2) 0.038(3) Uani 1 1 d . . . . . H7A H -0.5695 0.2540 0.7363 0.057 Uiso 0.6667 1 calc R U P . . H7B H -0.5431 0.2722 0.7678 0.057 Uiso 0.6667 1 calc R U P . . H7C H -0.6227 0.1741 0.7585 0.057 Uiso 0.6667 1 calc R U P . . O8 O -0.5000 0.0000 0.7147(3) 0.041(5) Uani 1 2 d S T P . . H8A H -0.4524 -0.0476 0.7034 0.049 Uiso 0.5 1 calc R U P . . H8B H -0.5476 0.0476 0.7034 0.049 Uiso 0.5 1 calc R U P . . O9 O -0.6609(16) 0.6122(14) 0.8004(3) 0.088(6) Uani 1 1 d . . . . . H9A H -0.6500 0.6768 0.8121 0.132 Uiso 0.6667 1 calc R U P . . H9B H -0.7241 0.5698 0.8070 0.132 Uiso 0.6667 1 calc R U P . . H9C H -0.6747 0.6364 0.7818 0.132 Uiso 0.6667 1 calc R U P . . O10 O -0.5000 0.5000 0.8479(16) 0.29(4) Uiso 1 4 d S . P . . H10A H -0.5760 0.5032 0.8545 0.440 Uiso 0.1667 1 calc R U P . . H10B H -0.4592 0.5643 0.8545 0.440 Uiso 0.1667 1 calc R U P . . H10C H -0.4647 0.4326 0.8545 0.440 Uiso 0.1667 1 calc R U P . . O11 O -0.7345(12) -0.0883(11) 0.6490(2) 0.056(4) Uani 1 1 d . . . . . O12 O -0.954(2) 0.157(3) 0.5976(6) 0.238(18) Uani 1 1 d . . . . . O13 O -0.774(9) -0.078(8) 0.5000 0.23(4) Uiso 0.5 2 d S . P . . N1 N -0.5000 0.5000 0.6585(6) 0.048(9) Uani 1 4 d S TU P . . N2 N -0.5000 0.5000 0.6377(11) 0.31(6) Uani 1 4 d S TU P . . N3 N -0.5000 0.5000 0.6128(7) 0.118(19) Uani 1 4 d S TU P . . C1 C -0.5893(14) 0.1705(15) 0.62393(18) 0.051(6) Uani 1 1 d G . . . . C2 C -0.4888(12) 0.156(2) 0.6109(3) 0.21(3) Uani 1 1 d G . . . . H2 H -0.4228 0.1519 0.6212 0.250 Uiso 1 1 calc R U . . . C3 C -0.4850(13) 0.147(2) 0.5828(3) 0.22(3) Uani 1 1 d G . . . . H3 H -0.4163 0.1373 0.5739 0.265 Uiso 1 1 calc R U . . . C4 C -0.5816(16) 0.1531(19) 0.56776(18) 0.109(14) Uani 1 1 d G . . . . C5 C -0.6820(13) 0.168(2) 0.5808(3) 0.128(14) Uani 1 1 d G . . . . H5 H -0.7480 0.1717 0.5705 0.153 Uiso 1 1 calc R U . . . C6 C -0.6859(12) 0.176(2) 0.6089(3) 0.145(17) Uani 1 1 d G . . . . H6 H -0.7545 0.1863 0.6178 0.174 Uiso 1 1 calc R U . . . C7 C -0.583(3) 0.147(3) 0.5376(4) 0.116(13) Uani 1 1 d . . . . . C8 C -0.581(3) 0.146(3) 0.5148(4) 0.113(12) Uani 1 1 d . . . . . Na1 Na -0.4027(6) 0.0973(6) 0.7500 0.037(3) Uani 1 2 d S T P . . Na2 Na -0.5000 0.5000 0.8016(3) 0.074(6) Uani 1 4 d S T P . . 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 0.035(3) 0.035(3) 0.011(3) 0.000 0.000 0.000 V2 0.045(2) 0.040(2) 0.0170(14) 0.0011(14) 0.0053(15) 0.0042(18) P3 0.059(4) 0.041(3) 0.013(2) -0.003(2) 0.002(2) -0.008(3) O1 0.047(9) 0.041(8) 0.012(5) -0.004(5) 0.003(5) 0.008(7) O2 0.047(8) 0.032(8) 0.016(5) 0.007(5) -0.003(5) 0.004(6) O3 0.057(10) 0.050(9) 0.019(6) 0.005(6) 0.002(6) 0.014(7) O4 0.044(10) 0.044(10) 0.004(9) 0.000 0.000 0.000 O5 0.046(9) 0.042(9) 0.024(6) -0.014(5) 0.007(6) 0.000(7) O6 0.077(11) 0.063(11) 0.028(6) -0.012(7) 0.002(7) -0.024(9) O7 0.039(8) 0.033(9) 0.042(7) 0.004(6) 0.007(6) 0.001(6) O8 0.076(15) 0.019(10) 0.027(8) 0.000 0.000 0.002(11) O9 0.148(18) 0.070(13) 0.045(8) 0.003(8) 0.037(10) 0.000(12) O11 0.078(11) 0.051(10) 0.039(7) 0.000(7) -0.009(7) 0.008(9) O12 0.11(2) 0.38(5) 0.22(3) -0.12(3) -0.06(2) 0.06(3) N1 0.053(14) 0.053(14) 0.037(12) 0.000 0.000 0.000 N2 0.44(9) 0.44(9) 0.039(12) 0.000 0.000 0.000 N3 0.16(3) 0.16(3) 0.040(12) 0.000 0.000 0.000 C1 0.073(17) 0.062(16) 0.017(9) -0.007(9) 0.015(11) 0.016(14) C2 0.17(4) 0.43(8) 0.029(13) -0.03(3) 0.009(19) 0.14(5) C3 0.11(3) 0.53(8) 0.019(13) -0.05(3) -0.011(16) 0.13(4) C4 0.12(3) 0.17(3) 0.033(13) 0.005(16) 0.003(15) 0.09(3) C5 0.11(3) 0.23(4) 0.049(15) -0.02(2) -0.025(17) 0.05(3) C6 0.09(2) 0.33(6) 0.018(11) -0.04(2) 0.001(14) -0.01(3) C7 0.20(4) 0.14(3) 0.010(11) -0.001(13) -0.016(15) 0.03(3) C8 0.15(3) 0.15(3) 0.032(12) -0.001(16) -0.007(15) 0.05(3) Na1 0.041(4) 0.041(4) 0.030(5) 0.009(4) -0.009(4) -0.010(6) Na2 0.103(10) 0.103(10) 0.017(7) 0.000 0.000 0.000 _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 O4 1.541(18) . ? V1 O2 1.878(12) . ? V1 O2 1.878(12) 6_455 ? V1 O2 1.878(12) 3_465 ? V1 O2 1.878(12) 7_565 ? V1 V2 2.931(4) . ? V1 V2 2.931(4) 6_455 ? V1 V2 2.931(4) 7_565 ? V1 V2 2.931(4) 3_465 ? V2 O3 1.601(12) . ? V2 O5 1.953(12) . ? V2 O1 1.956(11) . ? V2 O2 1.972(11) 6_455 ? V2 O2 2.000(12) . ? P3 O5 1.509(13) . ? P3 O6 1.520(14) . ? P3 O1 1.533(13) 6_455 ? P3 C1 1.792(9) . ? O1 P3 1.533(13) 7_565 ? O2 V2 1.972(11) 7_565 ? O3 Na1 2.430(13) . ? O4 Na2 2.45(2) . ? O7 Na1 2.381(12) . ? O7 H7A 0.9800 . ? O7 H7B 0.9800 . ? O7 H7C 0.9800 . ? O8 Na1 2.413(12) . ? O8 Na1 2.413(12) 3_455 ? O8 H8A 0.9900 . ? O8 H8B 0.9900 . ? O9 Na2 2.383(18) . ? O9 H9A 0.9800 . ? O9 H9B 0.9800 . ? O9 H9C 0.9800 . ? O10 Na2 2.28(8) . ? O10 H10A 1.3377 . ? O10 H10B 1.3377 . ? O10 H10C 1.3377 . ? N1 N2 1.03(5) . ? N2 N3 1.23(6) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 C7 1.49(2) . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.13(3) . ? C8 C8 1.46(4) 11_556 ? Na1 O7 2.381(12) 5_456 ? Na1 O8 2.413(12) 5_456 ? Na1 O3 2.430(13) 5_456 ? Na1 Na1 3.34(2) 3_455 ? Na2 O9 2.383(18) 7_565 ? Na2 O9 2.383(18) 6_455 ? Na2 O9 2.383(18) 3_465 ? 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 O4 V1 O2 108.8(3) . . ? O4 V1 O2 108.8(3) . 6_455 ? O2 V1 O2 84.07(19) . 6_455 ? O4 V1 O2 108.8(3) . 3_465 ? O2 V1 O2 142.5(6) . 3_465 ? O2 V1 O2 84.07(19) 6_455 3_465 ? O4 V1 O2 108.8(3) . 7_565 ? O2 V1 O2 84.07(19) . 7_565 ? O2 V1 O2 142.5(6) 6_455 7_565 ? O2 V1 O2 84.07(19) 3_465 7_565 ? O4 V1 V2 117.19(10) . . ? O2 V1 V2 42.5(4) . . ? O2 V1 V2 41.6(3) 6_455 . ? O2 V1 V2 116.3(4) 3_465 . ? O2 V1 V2 117.0(4) 7_565 . ? O4 V1 V2 117.19(10) . 6_455 ? O2 V1 V2 117.0(4) . 6_455 ? O2 V1 V2 42.5(4) 6_455 6_455 ? O2 V1 V2 41.6(3) 3_465 6_455 ? O2 V1 V2 116.3(4) 7_565 6_455 ? V2 V1 V2 77.94(8) . 6_455 ? O4 V1 V2 117.19(10) . 7_565 ? O2 V1 V2 41.6(3) . 7_565 ? O2 V1 V2 116.3(4) 6_455 7_565 ? O2 V1 V2 117.0(4) 3_465 7_565 ? O2 V1 V2 42.5(4) 7_565 7_565 ? V2 V1 V2 77.94(8) . 7_565 ? V2 V1 V2 125.6(2) 6_455 7_565 ? O4 V1 V2 117.19(10) . 3_465 ? O2 V1 V2 116.3(4) . 3_465 ? O2 V1 V2 117.0(4) 6_455 3_465 ? O2 V1 V2 42.5(4) 3_465 3_465 ? O2 V1 V2 41.6(3) 7_565 3_465 ? V2 V1 V2 125.6(2) . 3_465 ? V2 V1 V2 77.94(8) 6_455 3_465 ? V2 V1 V2 77.94(8) 7_565 3_465 ? O3 V2 O5 104.4(6) . . ? O3 V2 O1 107.6(6) . . ? O5 V2 O1 85.5(5) . . ? O3 V2 O2 105.4(5) . 6_455 ? O5 V2 O2 89.5(5) . 6_455 ? O1 V2 O2 146.8(5) . 6_455 ? O3 V2 O2 103.8(6) . . ? O5 V2 O2 151.5(5) . . ? O1 V2 O2 90.5(5) . . ? O2 V2 O2 78.6(7) 6_455 . ? O3 V2 V1 110.4(4) . . ? O5 V2 V1 123.4(4) . . ? O1 V2 V1 122.3(4) . . ? O2 V2 V1 39.2(4) 6_455 . ? O2 V2 V1 39.4(3) . . ? O5 P3 O6 113.1(8) . . ? O5 P3 O1 112.6(7) . 6_455 ? O6 P3 O1 111.9(8) . 6_455 ? O5 P3 C1 105.2(7) . . ? O6 P3 C1 108.0(8) . . ? O1 P3 C1 105.3(7) 6_455 . ? P3 O1 V2 134.7(7) 7_565 . ? V1 O2 V2 99.1(5) . 7_565 ? V1 O2 V2 98.1(5) . . ? V2 O2 V2 136.3(5) 7_565 . ? V2 O3 Na1 141.7(8) . . ? V1 O4 Na2 180.0 . . ? P3 O5 V2 138.0(7) . . ? Na1 O7 H7A 109.5 . . ? Na1 O7 H7B 109.5 . . ? H7A O7 H7B 109.5 . . ? Na1 O7 H7C 109.5 . . ? H7A O7 H7C 109.5 . . ? H7B O7 H7C 109.5 . . ? Na1 O8 Na1 87.7(6) . 3_455 ? Na1 O8 H8A 114.0 . . ? Na1 O8 H8A 114.0 3_455 . ? Na1 O8 H8B 114.0 . . ? Na1 O8 H8B 114.0 3_455 . ? H8A O8 H8B 111.2 . . ? Na2 O9 H9A 109.5 . . ? Na2 O9 H9B 109.5 . . ? H9A O9 H9B 109.5 . . ? Na2 O9 H9C 109.5 . . ? H9A O9 H9C 109.5 . . ? H9B O9 H9C 109.5 . . ? Na2 O10 H10A 130.6 . . ? Na2 O10 H10B 130.6 . . ? H10A O10 H10B 82.2 . . ? Na2 O10 H10C 130.6 . . ? H10A O10 H10C 82.2 . . ? H10B O10 H10C 82.2 . . ? N1 N2 N3 180.000(14) . . ? C2 C1 C6 120.0 . . ? C2 C1 P3 119.2(9) . . ? C6 C1 P3 120.7(9) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 C7 117.1(17) . . ? C3 C4 C7 122.8(17) . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C4 177(4) . . ? C7 C8 C8 179(2) . 11_556 ? O7 Na1 O7 165.5(8) 5_456 . ? O7 Na1 O8 88.2(4) 5_456 5_456 ? O7 Na1 O8 81.8(3) . 5_456 ? O7 Na1 O8 81.8(3) 5_456 . ? O7 Na1 O8 88.2(4) . . ? O8 Na1 O8 92.3(6) 5_456 . ? O7 Na1 O3 107.0(4) 5_456 . ? O7 Na1 O3 82.8(4) . . ? O8 Na1 O3 164.6(3) 5_456 . ? O8 Na1 O3 87.0(4) . . ? O7 Na1 O3 82.8(4) 5_456 5_456 ? O7 Na1 O3 107.0(4) . 5_456 ? O8 Na1 O3 87.0(4) 5_456 5_456 ? O8 Na1 O3 164.6(3) . 5_456 ? O3 Na1 O3 97.7(7) . 5_456 ? O7 Na1 Na1 82.8(4) 5_456 3_455 ? O7 Na1 Na1 82.8(4) . 3_455 ? O8 Na1 Na1 46.2(3) 5_456 3_455 ? O8 Na1 Na1 46.2(3) . 3_455 ? O3 Na1 Na1 131.1(4) . 3_455 ? O3 Na1 Na1 131.1(4) 5_456 3_455 ? O10 Na2 O9 91.3(4) . 7_565 ? O10 Na2 O9 91.3(4) . 6_455 ? O9 Na2 O9 177.3(9) 7_565 6_455 ? O10 Na2 O9 91.3(4) . 3_465 ? O9 Na2 O9 89.97(2) 7_565 3_465 ? O9 Na2 O9 89.97(3) 6_455 3_465 ? O10 Na2 O9 91.3(4) . . ? O9 Na2 O9 89.97(3) 7_565 . ? O9 Na2 O9 89.97(2) 6_455 . ? O9 Na2 O9 177.3(9) 3_465 . ? O10 Na2 O4 180.0 . . ? O9 Na2 O4 88.7(4) 7_565 . ? O9 Na2 O4 88.7(4) 6_455 . ? O9 Na2 O4 88.7(4) 3_465 . ? O9 Na2 O4 88.7(4) . . ? _refine_diff_density_max 1.597 _refine_diff_density_min -1.177 _refine_diff_density_rms 0.433 _shelxl_version_number 2013-4 _database_code_depnum_ccdc_archive 'CCDC 970549'