# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bernhard Spingler' _publ_contact_author_email spingler@aci.uzh.ch loop_ _publ_author_name 'Mareike Meyer' 'Bernhard Spingler' 'Wolfgang Meyer-Zaika' 'Arndt Karschin' 'Wolfgang Klui' data_kp020209 _database_code_depnum_ccdc_archive 'CCDC 782185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Na4 O23 P2' _chemical_formula_weight 1098.90 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' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.69271(16) _cell_length_b 16.5739(3) _cell_length_c 19.3218(4) _cell_angle_alpha 84.7890(16) _cell_angle_beta 78.4421(16) _cell_angle_gamma 83.8493(15) _cell_volume 2704.70(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 15783 _cell_measurement_theta_min 2.3966 _cell_measurement_theta_max 32.6396 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8806 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38259 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 30.50 _reflns_number_total 16465 _reflns_number_gt 10954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0516P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16465 _refine_ls_number_parameters 744 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 P1 P 0.46861(4) -0.08681(2) -0.370974(19) 0.01181(7) Uani 1 1 d . . . P41 P -0.04706(4) 0.42003(2) -0.371479(19) 0.01175(7) Uani 1 1 d . . . C1 C 0.39719(15) -0.13132(8) -0.28297(7) 0.0148(3) Uani 1 1 d . . . H1A H 0.3862 -0.0892 -0.2486 0.018 Uiso 1 1 calc R . . H1B H 0.2914 -0.1494 -0.2810 0.018 Uiso 1 1 calc R . . C2 C 0.50676(15) -0.20434(8) -0.26088(7) 0.0150(3) Uani 1 1 d . . . H2A H 0.6172 -0.1942 -0.2819 0.018 Uiso 1 1 calc R . . H2B H 0.4832 -0.2534 -0.2811 0.018 Uiso 1 1 calc R . . C3 C 0.49296(14) -0.22225(8) -0.17969(7) 0.0137(3) Uani 1 1 d . . . C11 C 0.31709(15) -0.23164(8) -0.14932(7) 0.0165(3) Uani 1 1 d . . . C12 C 0.25367(17) -0.30203(9) -0.16101(9) 0.0251(3) Uani 1 1 d . . . H12 H 0.3213 -0.3447 -0.1838 0.030 Uiso 1 1 calc R . . C13 C 0.09443(19) -0.31084(11) -0.14006(10) 0.0352(4) Uani 1 1 d . . . H13 H 0.0545 -0.3599 -0.1473 0.042 Uiso 1 1 calc R . . C14 C -0.00690(19) -0.24888(12) -0.10876(10) 0.0380(4) Uani 1 1 d . . . H14 H -0.1166 -0.2547 -0.0951 0.046 Uiso 1 1 calc R . . C15 C 0.05269(18) -0.17835(11) -0.09740(10) 0.0357(4) Uani 1 1 d . . . H15 H -0.0162 -0.1354 -0.0758 0.043 Uiso 1 1 calc R . . C16 C 0.21416(17) -0.17001(9) -0.11754(9) 0.0257(3) Uani 1 1 d . . . H16 H 0.2540 -0.1213 -0.1093 0.031 Uiso 1 1 calc R . . C21 C 0.59266(15) -0.30279(8) -0.16392(8) 0.0166(3) Uani 1 1 d . . . C22 C 0.72310(16) -0.33171(9) -0.21273(9) 0.0214(3) Uani 1 1 d . . . H22 H 0.7508 -0.3022 -0.2572 0.026 Uiso 1 1 calc R . . C23 C 0.81333(17) -0.40310(9) -0.19740(10) 0.0280(4) Uani 1 1 d . . . H23 H 0.9010 -0.4221 -0.2317 0.034 Uiso 1 1 calc R . . C24 C 0.77675(18) -0.44646(9) -0.13306(10) 0.0299(4) Uani 1 1 d . . . H24 H 0.8394 -0.4949 -0.1226 0.036 Uiso 1 1 calc R . . C25 C 0.6479(2) -0.41883(9) -0.08382(10) 0.0317(4) Uani 1 1 d . . . H25 H 0.6215 -0.4485 -0.0393 0.038 Uiso 1 1 calc R . . C26 C 0.55655(18) -0.34759(9) -0.09936(9) 0.0263(3) Uani 1 1 d . . . H26 H 0.4680 -0.3294 -0.0652 0.032 Uiso 1 1 calc R . . C31 C 0.55770(15) -0.15482(8) -0.14653(8) 0.0164(3) Uani 1 1 d . . . C32 C 0.64596(17) -0.09653(9) -0.18812(8) 0.0228(3) Uani 1 1 d . . . H32 H 0.6640 -0.0970 -0.2382 0.027 Uiso 1 1 calc R . . C33 C 0.70844(18) -0.03747(9) -0.15756(9) 0.0295(4) Uani 1 1 d . . . H33 H 0.7690 0.0015 -0.1870 0.035 Uiso 1 1 calc R . . C34 C 0.68279(19) -0.03533(10) -0.08521(10) 0.0305(4) Uani 1 1 d . . . H34 H 0.7239 0.0054 -0.0645 0.037 Uiso 1 1 calc R . . C35 C 0.5967(2) -0.09294(10) -0.04290(9) 0.0303(4) Uani 1 1 d . . . H35 H 0.5792 -0.0921 0.0072 0.036 Uiso 1 1 calc R . . C36 C 0.53552(18) -0.15211(9) -0.07320(8) 0.0244(3) Uani 1 1 d . . . H36 H 0.4773 -0.1916 -0.0434 0.029 Uiso 1 1 calc R . . C41 C -0.12284(15) 0.37697(8) -0.28304(7) 0.0150(3) Uani 1 1 d . . . H41A H -0.1263 0.4182 -0.2486 0.018 Uiso 1 1 calc R . . H41B H -0.2321 0.3634 -0.2806 0.018 Uiso 1 1 calc R . . C42 C -0.02188(15) 0.29972(8) -0.26196(7) 0.0149(3) Uani 1 1 d . . . H42A H 0.0898 0.3063 -0.2835 0.018 Uiso 1 1 calc R . . H42B H -0.0530 0.2530 -0.2828 0.018 Uiso 1 1 calc R . . C43 C -0.03332(15) 0.27831(8) -0.18134(7) 0.0140(3) Uani 1 1 d . . . C51 C -0.20843(15) 0.26886(8) -0.15025(8) 0.0175(3) Uani 1 1 d . . . C52 C -0.27128(17) 0.19671(9) -0.15777(9) 0.0257(3) Uani 1 1 d . . . H52 H -0.2033 0.1529 -0.1785 0.031 Uiso 1 1 calc R . . C53 C -0.43057(19) 0.18775(11) -0.13568(10) 0.0355(4) Uani 1 1 d . . . H53 H -0.4702 0.1377 -0.1404 0.043 Uiso 1 1 calc R . . C54 C -0.53191(19) 0.25123(13) -0.10690(10) 0.0400(5) Uani 1 1 d . . . H54 H -0.6414 0.2453 -0.0922 0.048 Uiso 1 1 calc R . . C55 C -0.47280(18) 0.32333(12) -0.09970(10) 0.0378(4) Uani 1 1 d . . . H55 H -0.5418 0.3673 -0.0798 0.045 Uiso 1 1 calc R . . C56 C -0.31189(17) 0.33192(10) -0.12150(9) 0.0275(3) Uani 1 1 d . . . H56 H -0.2727 0.3820 -0.1165 0.033 Uiso 1 1 calc R . . C61 C 0.06763(15) 0.19770(8) -0.16785(8) 0.0157(3) Uani 1 1 d . . . C62 C 0.19415(16) 0.16825(8) -0.21838(8) 0.0202(3) Uani 1 1 d . . . H62 H 0.2163 0.1966 -0.2637 0.024 Uiso 1 1 calc R . . C63 C 0.28882(17) 0.09805(9) -0.20372(9) 0.0263(4) Uani 1 1 d . . . H63 H 0.3742 0.0791 -0.2391 0.032 Uiso 1 1 calc R . . C64 C 0.26003(18) 0.05573(9) -0.13841(9) 0.0279(4) Uani 1 1 d . . . H64 H 0.3256 0.0083 -0.1283 0.033 Uiso 1 1 calc R . . C65 C 0.13397(19) 0.08357(9) -0.08781(9) 0.0304(4) Uani 1 1 d . . . H65 H 0.1120 0.0547 -0.0427 0.037 Uiso 1 1 calc R . . C66 C 0.03905(18) 0.15361(9) -0.10256(9) 0.0255(3) Uani 1 1 d . . . H66 H -0.0472 0.1717 -0.0672 0.031 Uiso 1 1 calc R . . C71 C 0.03363(15) 0.34366(8) -0.14627(8) 0.0157(3) Uani 1 1 d . . . C72 C 0.00549(17) 0.34559(9) -0.07264(8) 0.0223(3) Uani 1 1 d . . . H72 H -0.0592 0.3078 -0.0440 0.027 Uiso 1 1 calc R . . C73 C 0.07053(19) 0.40185(9) -0.04046(9) 0.0272(3) Uani 1 1 d . . . H73 H 0.0499 0.4021 0.0097 0.033 Uiso 1 1 calc R . . C74 C 0.16469(18) 0.45728(9) -0.08091(9) 0.0272(4) Uani 1 1 d . . . H74 H 0.2081 0.4960 -0.0589 0.033 Uiso 1 1 calc R . . C75 C 0.19521(18) 0.45607(9) -0.15338(9) 0.0257(3) Uani 1 1 d . . . H75 H 0.2606 0.4939 -0.1815 0.031 Uiso 1 1 calc R . . C76 C 0.13085(16) 0.39956(8) -0.18613(8) 0.0208(3) Uani 1 1 d . . . H76 H 0.1537 0.3992 -0.2363 0.025 Uiso 1 1 calc R . . O1 O 0.50222(10) -0.15576(5) -0.42144(5) 0.0167(2) Uani 1 1 d . . . O2 O 0.61778(10) -0.04699(5) -0.36867(5) 0.0172(2) Uani 1 1 d . . . O3 O 0.33758(10) -0.02371(6) -0.38874(5) 0.0172(2) Uani 1 1 d . . . O41 O -0.03012(10) 0.35197(5) -0.42180(5) 0.0153(2) Uani 1 1 d . . . O42 O 0.11448(10) 0.44793(5) -0.37004(5) 0.0164(2) Uani 1 1 d . . . O43 O -0.16414(10) 0.49101(5) -0.38851(5) 0.0169(2) Uani 1 1 d . . . O81 O -0.18867(11) 0.00234(6) -0.49788(6) 0.0189(2) Uani 1 1 d . . . H81A H -0.254(2) -0.0058(10) -0.4623(10) 0.028 Uiso 1 1 d . . . H81B H -0.237(2) 0.0111(10) -0.5319(10) 0.028 Uiso 1 1 d . . . O82 O -0.08080(12) -0.08868(7) -0.35683(6) 0.0228(2) Uani 1 1 d . . . H82A H -0.172(2) -0.0787(11) -0.3564(9) 0.034 Uiso 1 1 d . . . H82B H -0.052(2) -0.0502(11) -0.3351(10) 0.034 Uiso 1 1 d . . . O83 O -0.17391(12) -0.21078(6) -0.45489(6) 0.0203(2) Uani 1 1 d . . . H83A H -0.152(2) -0.2542(11) -0.4395(10) 0.030 Uiso 1 1 d . . . H83B H -0.266(2) -0.1934(10) -0.4383(9) 0.030 Uiso 1 1 d . . . O84 O 0.22064(12) -0.20024(6) -0.46363(6) 0.0208(2) Uani 1 1 d . . . H84A H 0.294(2) -0.1802(10) -0.4540(9) 0.031 Uiso 1 1 d . . . H84B H 0.2568(19) -0.2259(11) -0.4970(9) 0.031 Uiso 1 1 d . . . O85 O 0.03440(17) -0.23163(9) -0.29783(9) 0.0397(3) Uani 1 1 d . . . H85A H -0.004(3) -0.1879(15) -0.3133(13) 0.072(8) Uiso 1 1 d . . . H85B H 0.024(3) -0.2337(15) -0.2578(14) 0.068(9) Uiso 1 1 d . . . O86 O -0.02239(13) -0.36447(6) -0.43078(6) 0.0218(2) Uani 1 1 d . . . H86A H -0.009(2) -0.3665(11) -0.4715(10) 0.033 Uiso 1 1 d . . . H86B H -0.066(2) -0.4074(11) -0.4162(10) 0.033 Uiso 1 1 d . . . O87 O 0.46243(12) -0.32247(7) -0.41043(6) 0.0228(2) Uani 1 1 d . . . H87A H 0.481(2) -0.2751(11) -0.4093(10) 0.034 Uiso 1 1 d . . . H87B H 0.502(2) -0.3506(11) -0.3826(10) 0.034 Uiso 1 1 d . . . O88 O 0.22740(14) -0.43349(7) -0.31273(7) 0.0292(3) Uani 1 1 d . . . H88A H 0.188(2) -0.4708(12) -0.3260(10) 0.044 Uiso 1 1 d . . . H88B H 0.317(2) -0.4471(12) -0.3119(10) 0.044 Uiso 1 1 d . . . O89 O 0.30695(12) -0.30735(6) -0.56819(6) 0.0210(2) Uani 1 1 d . . . H89A H 0.353(2) -0.2960(11) -0.6088(10) 0.032 Uiso 1 1 d . . . H89B H 0.217(2) -0.3217(10) -0.5701(9) 0.032 Uiso 1 1 d . . . O90 O 0.31224(11) -0.49849(6) -0.49674(6) 0.0201(2) Uani 1 1 d . . . H90A H 0.246(2) -0.5081(11) -0.4621(10) 0.030 Uiso 1 1 d . . . H90B H 0.265(2) -0.4944(10) -0.5306(10) 0.030 Uiso 1 1 d . . . O91 O -0.04525(13) 0.14330(7) -0.39418(6) 0.0244(2) Uani 1 1 d . . . H91A H -0.139(2) 0.1448(11) -0.3844(10) 0.037 Uiso 1 1 d . . . H91B H -0.019(2) 0.1072(11) -0.3721(10) 0.037 Uiso 1 1 d . . . O92 O 0.38346(12) 0.13645(6) -0.43200(6) 0.0222(2) Uani 1 1 d . . . H92A H 0.369(2) 0.0871(11) -0.4199(10) 0.033 Uiso 1 1 d . . . H92B H 0.416(2) 0.1362(11) -0.4751(10) 0.033 Uiso 1 1 d . . . O93 O 0.33072(12) 0.32486(7) -0.39833(6) 0.0231(2) Uani 1 1 d . . . H93A H 0.374(2) 0.3099(11) -0.3655(10) 0.035 Uiso 1 1 d . . . H93B H 0.270(2) 0.3628(11) -0.3876(10) 0.035 Uiso 1 1 d . . . O101 O 0.07387(13) 0.02257(7) -0.30365(7) 0.0268(3) Uani 1 1 d . . . H10A H 0.159(2) 0.0095(11) -0.3283(11) 0.040 Uiso 1 1 d . . . H10B H 0.092(2) 0.0353(11) -0.2673(11) 0.040 Uiso 1 1 d . . . O102 O -0.37804(13) 0.11672(7) -0.35178(7) 0.0268(3) Uani 1 1 d . . . H10C H -0.438(2) 0.1333(11) -0.3792(10) 0.040 Uiso 1 1 d . . . H10D H -0.380(2) 0.0649(12) -0.3483(10) 0.040 Uiso 1 1 d . . . O103 O -0.48097(14) 0.26268(8) -0.29488(7) 0.0314(3) Uani 1 1 d . . . H10E H -0.486(2) 0.2709(12) -0.2548(12) 0.047 Uiso 1 1 d . . . H10F H -0.451(2) 0.2116(12) -0.3006(11) 0.047 Uiso 1 1 d . . . O104 O -0.43261(13) 0.55735(7) -0.31278(7) 0.0301(3) Uani 1 1 d . . . H10G H -0.348(2) 0.5314(12) -0.3356(11) 0.045 Uiso 1 1 d . . . H10H H -0.408(2) 0.5681(12) -0.2747(11) 0.045 Uiso 1 1 d . . . Na1 Na 0.00838(6) -0.10541(3) -0.48191(3) 0.01798(12) Uani 1 1 d . . . Na2 Na 0.16970(6) -0.31545(3) -0.37886(3) 0.02317(14) Uani 1 1 d . . . Na3 Na 0.48620(6) -0.39269(3) -0.51208(3) 0.02014(13) Uani 1 1 d . . . Na4 Na 0.15464(6) 0.23637(3) -0.42679(3) 0.01989(13) 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 P1 0.01107(15) 0.01202(16) 0.01238(19) 0.00139(13) -0.00344(13) -0.00089(12) P41 0.01174(15) 0.01111(16) 0.01268(19) 0.00057(13) -0.00408(13) -0.00022(12) C1 0.0155(6) 0.0156(6) 0.0123(7) 0.0030(5) -0.0027(5) 0.0001(5) C2 0.0175(6) 0.0149(6) 0.0118(7) 0.0008(5) -0.0033(5) 0.0014(5) C3 0.0148(6) 0.0131(6) 0.0128(7) 0.0017(5) -0.0037(5) 0.0005(5) C11 0.0163(6) 0.0194(7) 0.0135(8) 0.0047(5) -0.0050(5) -0.0017(5) C12 0.0249(7) 0.0256(8) 0.0262(9) 0.0019(7) -0.0079(6) -0.0063(6) C13 0.0292(9) 0.0423(10) 0.0381(11) 0.0104(8) -0.0140(8) -0.0179(8) C14 0.0189(8) 0.0618(13) 0.0322(11) 0.0157(9) -0.0066(7) -0.0113(8) C15 0.0221(8) 0.0478(11) 0.0307(11) 0.0036(8) 0.0021(7) 0.0072(7) C16 0.0241(7) 0.0251(8) 0.0252(9) 0.0004(7) -0.0015(6) 0.0014(6) C21 0.0188(6) 0.0139(6) 0.0196(8) -0.0004(5) -0.0099(6) -0.0017(5) C22 0.0194(7) 0.0198(7) 0.0261(9) -0.0020(6) -0.0075(6) -0.0004(5) C23 0.0217(7) 0.0226(8) 0.0419(11) -0.0089(7) -0.0118(7) 0.0042(6) C24 0.0293(8) 0.0164(7) 0.0489(12) -0.0001(7) -0.0228(8) 0.0022(6) C25 0.0398(9) 0.0232(8) 0.0331(11) 0.0087(7) -0.0165(8) 0.0008(7) C26 0.0328(8) 0.0235(8) 0.0217(9) 0.0051(6) -0.0085(7) 0.0023(6) C31 0.0148(6) 0.0153(6) 0.0192(8) -0.0013(6) -0.0050(5) 0.0012(5) C32 0.0256(7) 0.0238(8) 0.0188(9) -0.0006(6) -0.0028(6) -0.0057(6) C33 0.0307(8) 0.0235(8) 0.0352(11) -0.0011(7) -0.0045(7) -0.0113(6) C34 0.0366(9) 0.0239(8) 0.0369(11) -0.0093(7) -0.0166(8) -0.0049(7) C35 0.0427(9) 0.0315(9) 0.0203(9) -0.0071(7) -0.0120(7) -0.0038(7) C36 0.0335(8) 0.0240(8) 0.0167(8) 0.0012(6) -0.0065(6) -0.0061(6) C41 0.0148(6) 0.0162(6) 0.0138(7) 0.0001(5) -0.0039(5) 0.0009(5) C42 0.0182(6) 0.0141(6) 0.0120(7) 0.0014(5) -0.0036(5) -0.0002(5) C43 0.0152(6) 0.0131(6) 0.0135(7) 0.0011(5) -0.0036(5) -0.0006(5) C51 0.0172(6) 0.0220(7) 0.0130(8) 0.0043(6) -0.0049(5) -0.0020(5) C52 0.0253(8) 0.0269(8) 0.0270(10) 0.0026(7) -0.0087(7) -0.0089(6) C53 0.0287(9) 0.0477(11) 0.0335(11) 0.0098(8) -0.0112(7) -0.0193(8) C54 0.0165(7) 0.0729(14) 0.0299(11) 0.0164(9) -0.0070(7) -0.0126(8) C55 0.0211(8) 0.0533(12) 0.0330(11) 0.0026(9) 0.0001(7) 0.0092(8) C56 0.0225(7) 0.0284(8) 0.0290(10) 0.0009(7) -0.0024(6) 0.0022(6) C61 0.0171(6) 0.0128(6) 0.0191(8) 0.0005(5) -0.0083(5) -0.0019(5) C62 0.0197(7) 0.0184(7) 0.0227(9) 0.0001(6) -0.0055(6) -0.0010(5) C63 0.0208(7) 0.0193(7) 0.0393(11) -0.0049(7) -0.0082(7) 0.0027(6) C64 0.0271(8) 0.0141(7) 0.0454(11) 0.0010(7) -0.0168(7) 0.0009(6) C65 0.0394(9) 0.0219(8) 0.0303(10) 0.0093(7) -0.0140(8) -0.0002(7) C66 0.0302(8) 0.0224(8) 0.0222(9) 0.0041(6) -0.0059(6) 0.0022(6) C71 0.0165(6) 0.0143(6) 0.0166(8) -0.0009(5) -0.0055(5) 0.0013(5) C72 0.0286(8) 0.0224(7) 0.0155(8) 0.0003(6) -0.0039(6) -0.0029(6) C73 0.0396(9) 0.0265(8) 0.0179(9) -0.0046(7) -0.0114(7) -0.0006(7) C74 0.0348(9) 0.0219(8) 0.0301(10) -0.0059(7) -0.0173(7) -0.0021(6) C75 0.0292(8) 0.0209(7) 0.0296(10) 0.0010(7) -0.0106(7) -0.0075(6) C76 0.0248(7) 0.0204(7) 0.0181(8) 0.0010(6) -0.0065(6) -0.0036(6) O1 0.0196(5) 0.0153(5) 0.0148(5) -0.0010(4) -0.0027(4) -0.0012(4) O2 0.0135(4) 0.0175(5) 0.0212(6) 0.0018(4) -0.0049(4) -0.0032(4) O3 0.0150(4) 0.0172(5) 0.0188(6) 0.0034(4) -0.0055(4) 0.0012(4) O41 0.0159(4) 0.0159(5) 0.0152(5) -0.0016(4) -0.0052(4) -0.0016(4) O42 0.0148(4) 0.0154(5) 0.0200(6) -0.0005(4) -0.0049(4) -0.0030(4) O43 0.0174(4) 0.0141(5) 0.0187(6) 0.0019(4) -0.0056(4) 0.0022(4) O81 0.0158(5) 0.0233(5) 0.0180(6) 0.0025(4) -0.0055(4) -0.0030(4) O82 0.0178(5) 0.0259(6) 0.0262(7) -0.0032(5) -0.0080(4) 0.0000(4) O83 0.0173(5) 0.0178(5) 0.0245(6) 0.0000(5) -0.0028(4) 0.0012(4) O84 0.0192(5) 0.0196(5) 0.0246(7) -0.0027(4) -0.0070(4) 0.0005(4) O85 0.0546(8) 0.0326(7) 0.0259(9) 0.0052(6) -0.0033(6) 0.0079(6) O86 0.0289(6) 0.0161(5) 0.0207(6) 0.0015(5) -0.0058(5) -0.0040(4) O87 0.0278(6) 0.0175(5) 0.0249(7) 0.0008(5) -0.0107(5) -0.0025(4) O88 0.0334(6) 0.0204(6) 0.0376(8) 0.0005(5) -0.0144(6) -0.0076(5) O89 0.0151(5) 0.0255(6) 0.0233(6) -0.0005(5) -0.0047(4) -0.0052(4) O90 0.0143(5) 0.0255(5) 0.0206(6) 0.0042(5) -0.0056(4) -0.0022(4) O91 0.0210(5) 0.0235(6) 0.0275(7) 0.0019(5) -0.0038(5) -0.0014(5) O92 0.0279(6) 0.0174(5) 0.0207(6) 0.0008(5) -0.0052(5) -0.0007(4) O93 0.0164(5) 0.0208(5) 0.0305(7) 0.0003(5) -0.0043(4) 0.0026(4) O101 0.0190(5) 0.0342(6) 0.0275(7) -0.0085(5) -0.0048(5) 0.0013(5) O102 0.0270(6) 0.0211(6) 0.0341(7) -0.0016(5) -0.0102(5) -0.0028(5) O103 0.0384(7) 0.0330(7) 0.0228(7) 0.0014(5) -0.0070(5) -0.0038(5) O104 0.0216(5) 0.0386(7) 0.0305(7) -0.0073(6) -0.0089(5) 0.0071(5) Na1 0.0170(3) 0.0164(3) 0.0205(3) -0.0004(2) -0.0045(2) -0.0005(2) Na2 0.0219(3) 0.0203(3) 0.0270(4) 0.0026(2) -0.0058(2) -0.0025(2) Na3 0.0183(3) 0.0189(3) 0.0232(3) -0.0010(2) -0.0048(2) -0.0004(2) Na4 0.0198(3) 0.0183(3) 0.0222(3) -0.0036(2) -0.0056(2) 0.0001(2) _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 P1 O2 1.5268(9) . ? P1 O3 1.5314(9) . ? P1 O1 1.5357(9) . ? P1 C1 1.8079(14) . ? P41 O43 1.5281(9) . ? P41 O42 1.5308(9) . ? P41 O41 1.5316(9) . ? P41 C41 1.8142(14) . ? C1 C2 1.5414(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.5529(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C11 1.5429(18) . ? C3 C31 1.5444(18) . ? C3 C21 1.5525(18) . ? C11 C16 1.3853(19) . ? C11 C12 1.3969(19) . ? C12 C13 1.382(2) . ? C12 H12 0.9500 . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 C15 1.380(3) . ? C14 H14 0.9500 . ? C15 C16 1.398(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.389(2) . ? C21 C22 1.3936(19) . ? C22 C23 1.390(2) . ? C22 H22 0.9500 . ? C23 C24 1.375(2) . ? C23 H23 0.9500 . ? C24 C25 1.383(2) . ? C24 H24 0.9500 . ? C25 C26 1.395(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.392(2) . ? C31 C36 1.396(2) . ? C32 C33 1.396(2) . ? C32 H32 0.9500 . ? C33 C34 1.374(2) . ? C33 H33 0.9500 . ? C34 C35 1.381(2) . ? C34 H34 0.9500 . ? C35 C36 1.388(2) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.5436(17) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.5517(19) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C51 1.5395(18) . ? C43 C71 1.5483(18) . ? C43 C61 1.5492(17) . ? C51 C56 1.3833(19) . ? C51 C52 1.397(2) . ? C52 C53 1.385(2) . ? C52 H52 0.9500 . ? C53 C54 1.380(3) . ? C53 H53 0.9500 . ? C54 C55 1.379(3) . ? C54 H54 0.9500 . ? C55 C56 1.396(2) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.390(2) . ? C61 C62 1.3936(19) . ? C62 C63 1.3927(19) . ? C62 H62 0.9500 . ? C63 C64 1.377(2) . ? C63 H63 0.9500 . ? C64 C65 1.383(2) . ? C64 H64 0.9500 . ? C65 C66 1.392(2) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.394(2) . ? C71 C72 1.397(2) . ? C72 C73 1.391(2) . ? C72 H72 0.9500 . ? C73 C74 1.378(2) . ? C73 H73 0.9500 . ? C74 C75 1.374(2) . ? C74 H74 0.9500 . ? C75 C76 1.3972(19) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? O41 Na4 2.3605(10) . ? O81 Na1 2.3822(11) . ? O81 Na1 2.3945(11) 2_554 ? O81 H81A 0.809(18) . ? O81 H81B 0.844(18) . ? O82 Na1 2.4172(13) . ? O82 H82A 0.790(18) . ? O82 H82B 0.878(17) . ? O83 Na4 2.3328(12) 2_554 ? O83 Na1 2.4351(11) . ? O83 H83A 0.773(18) . ? O83 H83B 0.834(17) . ? O84 Na1 2.3534(11) . ? O84 Na2 2.4182(13) . ? O84 H84A 0.813(18) . ? O84 H84B 0.797(17) . ? O85 Na2 2.2520(15) . ? O85 H85A 0.82(3) . ? O85 H85B 0.76(3) . ? O86 Na2 2.3590(12) . ? O86 H86A 0.776(19) . ? O86 H86B 0.840(19) . ? O87 Na3 2.3357(12) . ? O87 Na2 2.4876(12) . ? O87 H87A 0.821(18) . ? O87 H87B 0.785(19) . ? O88 Na2 2.3030(13) . ? O88 H88A 0.823(19) . ? O88 H88B 0.791(19) . ? O89 Na3 2.3516(12) . ? O89 H89A 0.821(19) . ? O89 H89B 0.848(18) . ? O90 Na3 2.3955(11) 2_644 ? O90 Na3 2.3966(12) . ? O90 H90A 0.805(19) . ? O90 H90B 0.835(18) . ? O91 Na4 2.3989(12) . ? O91 Na1 2.4802(13) 2_554 ? O91 H91A 0.793(18) . ? O91 H91B 0.745(19) . ? O92 Na4 2.4399(11) . ? O92 H92A 0.845(19) . ? O92 H92B 0.824(19) . ? O93 Na3 2.3915(13) 2_654 ? O93 Na4 2.4003(11) . ? O93 H93A 0.807(19) . ? O93 H93B 0.789(17) . ? O101 H10A 0.818(19) . ? O101 H10B 0.800(19) . ? O102 H10C 0.826(19) . ? O102 H10D 0.857(19) . ? O103 H10E 0.79(2) . ? O103 H10F 0.869(19) . ? O104 H10G 0.869(19) . ? O104 H10H 0.85(2) . ? Na1 O81 2.3945(11) 2_554 ? Na1 O91 2.4802(13) 2_554 ? Na1 Na4 3.4911(7) 2_554 ? Na1 Na1 3.4937(11) 2_554 ? Na1 Na2 4.1066(8) . ? Na1 H81A 2.648(17) . ? Na1 H82A 2.656(18) . ? Na2 Na3 3.5832(8) . ? Na2 H84B 2.631(18) . ? Na3 O93 2.3915(13) 2_654 ? Na3 O90 2.3955(11) 2_644 ? Na3 Na3 3.5339(11) 2_644 ? Na3 Na4 4.1899(8) 2_654 ? Na4 O83 2.3328(12) 2_554 ? Na4 Na1 3.4911(7) 2_554 ? Na4 Na3 4.1899(8) 2_654 ? Na4 H93B 2.649(17) . ? 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 O2 P1 O3 111.39(5) . . ? O2 P1 O1 111.80(5) . . ? O3 P1 O1 111.86(5) . . ? O2 P1 C1 107.44(6) . . ? O3 P1 C1 106.55(6) . . ? O1 P1 C1 107.48(6) . . ? O43 P41 O42 112.02(5) . . ? O43 P41 O41 112.53(5) . . ? O42 P41 O41 110.49(5) . . ? O43 P41 C41 107.59(6) . . ? O42 P41 C41 106.75(6) . . ? O41 P41 C41 107.12(6) . . ? C2 C1 P1 112.99(9) . . ? C2 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C3 114.82(10) . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? C11 C3 C31 112.98(11) . . ? C11 C3 C21 109.54(11) . . ? C31 C3 C21 106.64(10) . . ? C11 C3 C2 106.19(10) . . ? C31 C3 C2 111.45(11) . . ? C21 C3 C2 110.05(10) . . ? C16 C11 C12 117.68(13) . . ? C16 C11 C3 123.16(12) . . ? C12 C11 C3 118.78(12) . . ? C13 C12 C11 121.26(15) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.47(16) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.32(15) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 120.17(16) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 121.07(15) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C26 C21 C22 117.65(13) . . ? C26 C21 C3 120.69(13) . . ? C22 C21 C3 121.64(13) . . ? C23 C22 C21 121.08(15) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 120.58(15) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.30(14) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.18(16) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 121.21(15) . . ? C21 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C32 C31 C36 117.24(13) . . ? C32 C31 C3 121.69(13) . . ? C36 C31 C3 121.01(13) . . ? C31 C32 C33 121.25(15) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 120.36(15) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.39(14) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 120.32(15) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 121.42(15) . . ? C35 C36 H36 119.3 . . ? C31 C36 H36 119.3 . . ? C42 C41 P41 112.61(9) . . ? C42 C41 H41A 109.1 . . ? P41 C41 H41A 109.1 . . ? C42 C41 H41B 109.1 . . ? P41 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C41 C42 C43 116.09(11) . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42B 108.3 . . ? C43 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C51 C43 C71 112.76(11) . . ? C51 C43 C61 110.04(11) . . ? C71 C43 C61 105.68(10) . . ? C51 C43 C42 106.38(10) . . ? C71 C43 C42 111.46(11) . . ? C61 C43 C42 110.58(11) . . ? C56 C51 C52 117.55(13) . . ? C56 C51 C43 122.84(13) . . ? C52 C51 C43 119.25(12) . . ? C53 C52 C51 121.37(15) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C54 C53 C52 120.26(16) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C53 119.38(15) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 120.21(16) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 121.22(15) . . ? C51 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C66 C61 C62 117.20(13) . . ? C66 C61 C43 120.48(12) . . ? C62 C61 C43 122.25(13) . . ? C63 C62 C61 121.31(15) . . ? C63 C62 H62 119.3 . . ? C61 C62 H62 119.3 . . ? C64 C63 C62 120.70(15) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 118.84(14) . . ? C63 C64 H64 120.6 . . ? C65 C64 H64 120.6 . . ? C64 C65 C66 120.44(16) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C61 C66 C65 121.51(15) . . ? C61 C66 H66 119.2 . . ? C65 C66 H66 119.2 . . ? C76 C71 C72 117.46(13) . . ? C76 C71 C43 121.75(13) . . ? C72 C71 C43 120.69(13) . . ? C73 C72 C71 121.19(15) . . ? C73 C72 H72 119.4 . . ? C71 C72 H72 119.4 . . ? C74 C73 C72 120.40(15) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C75 C74 C73 119.46(14) . . ? C75 C74 H74 120.3 . . ? C73 C74 H74 120.3 . . ? C74 C75 C76 120.51(15) . . ? C74 C75 H75 119.7 . . ? C76 C75 H75 119.7 . . ? C71 C76 C75 120.97(14) . . ? C71 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? P41 O41 Na4 126.11(5) . . ? Na1 O81 Na1 94.01(4) . 2_554 ? Na1 O81 H81A 100.3(12) . . ? Na1 O81 H81A 126.0(12) 2_554 . ? Na1 O81 H81B 127.3(11) . . ? Na1 O81 H81B 104.0(12) 2_554 . ? H81A O81 H81B 107.4(16) . . ? Na1 O82 H82A 98.9(13) . . ? Na1 O82 H82B 123.1(12) . . ? H82A O82 H82B 106.6(16) . . ? Na4 O83 Na1 94.12(4) 2_554 . ? Na4 O83 H83A 99.7(13) 2_554 . ? Na1 O83 H83A 123.4(13) . . ? Na4 O83 H83B 109.2(12) 2_554 . ? Na1 O83 H83B 113.7(12) . . ? H83A O83 H83B 112.6(18) . . ? Na1 O84 Na2 118.77(5) . . ? Na1 O84 H84A 114.1(12) . . ? Na2 O84 H84A 106.2(13) . . ? Na1 O84 H84B 113.4(12) . . ? Na2 O84 H84B 96.6(13) . . ? H84A O84 H84B 105.7(16) . . ? Na2 O85 H85A 116.4(17) . . ? Na2 O85 H85B 131.9(19) . . ? H85A O85 H85B 111(2) . . ? Na2 O86 H86A 120.1(13) . . ? Na2 O86 H86B 124.1(12) . . ? H86A O86 H86B 101.9(17) . . ? Na3 O87 Na2 95.90(4) . . ? Na3 O87 H87A 126.1(13) . . ? Na2 O87 H87A 102.9(12) . . ? Na3 O87 H87B 108.4(13) . . ? Na2 O87 H87B 111.4(14) . . ? H87A O87 H87B 110.5(17) . . ? Na2 O88 H88A 108.7(14) . . ? Na2 O88 H88B 117.9(15) . . ? H88A O88 H88B 109.2(19) . . ? Na3 O89 H89A 107.1(12) . . ? Na3 O89 H89B 121.4(12) . . ? H89A O89 H89B 108.0(17) . . ? Na3 O90 Na3 95.03(4) 2_644 . ? Na3 O90 H90A 102.5(13) 2_644 . ? Na3 O90 H90A 125.9(12) . . ? Na3 O90 H90B 120.0(12) 2_644 . ? Na3 O90 H90B 109.1(12) . . ? H90A O90 H90B 105.3(17) . . ? Na4 O91 Na1 91.36(4) . 2_554 ? Na4 O91 H91A 138.5(13) . . ? Na1 O91 H91A 98.4(13) 2_554 . ? Na4 O91 H91B 111.8(15) . . ? Na1 O91 H91B 108.5(15) 2_554 . ? H91A O91 H91B 103.1(19) . . ? Na4 O92 H92A 119.0(12) . . ? Na4 O92 H92B 101.0(12) . . ? H92A O92 H92B 102.8(16) . . ? Na3 O93 Na4 121.94(5) 2_654 . ? Na3 O93 H93A 108.1(13) 2_654 . ? Na4 O93 H93A 117.2(13) . . ? Na3 O93 H93B 98.3(14) 2_654 . ? Na4 O93 H93B 99.6(12) . . ? H93A O93 H93B 108.6(18) . . ? H10A O101 H10B 106.5(18) . . ? H10C O102 H10D 104.4(17) . . ? H10E O103 H10F 109(2) . . ? H10G O104 H10H 104.6(17) . . ? O84 Na1 O81 173.39(4) . . ? O84 Na1 O81 87.76(4) . 2_554 ? O81 Na1 O81 85.99(4) . 2_554 ? O84 Na1 O82 93.27(4) . . ? O81 Na1 O82 85.21(4) . . ? O81 Na1 O82 95.91(4) 2_554 . ? O84 Na1 O83 91.23(4) . . ? O81 Na1 O83 94.90(4) . . ? O81 Na1 O83 177.02(5) 2_554 . ? O82 Na1 O83 81.35(4) . . ? O84 Na1 O91 89.86(4) . 2_554 ? O81 Na1 O91 93.14(4) . 2_554 ? O81 Na1 O91 97.83(4) 2_554 2_554 ? O82 Na1 O91 166.02(4) . 2_554 ? O83 Na1 O91 84.97(4) . 2_554 ? O84 Na1 Na4 94.09(3) . 2_554 ? O81 Na1 Na4 92.13(3) . 2_554 ? O81 Na1 Na4 141.08(4) 2_554 2_554 ? O82 Na1 Na4 122.72(3) . 2_554 ? O83 Na1 Na4 41.80(3) . 2_554 ? O91 Na1 Na4 43.39(3) 2_554 2_554 ? O84 Na1 Na1 130.58(4) . 2_554 ? O81 Na1 Na1 43.13(3) . 2_554 ? O81 Na1 Na1 42.86(3) 2_554 2_554 ? O82 Na1 Na1 90.78(3) . 2_554 ? O83 Na1 Na1 137.97(4) . 2_554 ? O91 Na1 Na1 97.51(4) 2_554 2_554 ? Na4 Na1 Na1 123.96(3) 2_554 2_554 ? O84 Na1 Na2 31.08(3) . . ? O81 Na1 Na2 152.48(3) . . ? O81 Na1 Na2 113.41(3) 2_554 . ? O82 Na1 Na2 73.94(3) . . ? O83 Na1 Na2 64.79(3) . . ? O91 Na1 Na2 102.74(3) 2_554 . ? Na4 Na1 Na2 84.542(16) 2_554 . ? Na1 Na1 Na2 151.28(3) 2_554 . ? O84 Na1 H81A 163.4(4) . . ? O81 Na1 H81A 17.5(4) . . ? O81 Na1 H81A 96.7(4) 2_554 . ? O82 Na1 H81A 70.4(4) . . ? O83 Na1 H81A 83.5(4) . . ? O91 Na1 H81A 105.3(4) 2_554 . ? Na4 Na1 H81A 92.4(4) 2_554 . ? Na1 Na1 H81A 55.2(4) 2_554 . ? Na2 Na1 H81A 135.1(4) . . ? O84 Na1 H82A 107.9(4) . . ? O81 Na1 H82A 71.7(4) . . ? O81 Na1 H82A 104.7(4) 2_554 . ? O82 Na1 H82A 17.1(4) . . ? O83 Na1 H82A 72.9(4) . . ? O91 Na1 H82A 151.5(4) 2_554 . ? Na4 Na1 H82A 111.5(4) 2_554 . ? Na1 Na1 H82A 87.7(4) 2_554 . ? Na2 Na1 H82A 84.2(4) . . ? H81A Na1 H82A 55.5(6) . . ? O85 Na2 O88 103.91(6) . . ? O85 Na2 O86 105.40(5) . . ? O88 Na2 O86 97.07(4) . . ? O85 Na2 O84 90.18(5) . . ? O88 Na2 O84 157.23(5) . . ? O86 Na2 O84 96.26(4) . . ? O85 Na2 O87 120.79(5) . . ? O88 Na2 O87 81.27(4) . . ? O86 Na2 O87 132.91(4) . . ? O84 Na2 O87 76.14(4) . . ? O85 Na2 Na3 158.55(4) . . ? O88 Na2 Na3 85.10(4) . . ? O86 Na2 Na3 92.49(3) . . ? O84 Na2 Na3 75.94(3) . . ? O87 Na2 Na3 40.42(3) . . ? O85 Na2 Na1 71.11(4) . . ? O88 Na2 Na1 172.58(4) . . ? O86 Na2 Na1 79.36(3) . . ? O84 Na2 Na1 30.16(3) . . ? O87 Na2 Na1 105.95(3) . . ? Na3 Na2 Na1 101.477(19) . . ? O85 Na2 H84B 107.5(4) . . ? O88 Na2 H84B 145.3(4) . . ? O86 Na2 H84B 88.8(4) . . ? O84 Na2 H84B 17.5(4) . . ? O87 Na2 H84B 70.1(3) . . ? Na3 Na2 H84B 60.4(4) . . ? Na1 Na2 H84B 41.7(4) . . ? O87 Na3 O89 98.56(4) . . ? O87 Na3 O93 105.91(4) . 2_654 ? O89 Na3 O93 80.77(4) . 2_654 ? O87 Na3 O90 105.44(4) . 2_644 ? O89 Na3 O90 155.68(5) . 2_644 ? O93 Na3 O90 88.83(4) 2_654 2_644 ? O87 Na3 O90 112.97(5) . . ? O89 Na3 O90 89.34(4) . . ? O93 Na3 O90 140.89(5) 2_654 . ? O90 Na3 O90 84.97(4) 2_644 . ? O87 Na3 Na3 116.43(4) . 2_644 ? O89 Na3 Na3 127.59(4) . 2_644 ? O93 Na3 Na3 120.82(4) 2_654 2_644 ? O90 Na3 Na3 42.50(3) 2_644 2_644 ? O90 Na3 Na3 42.47(3) . 2_644 ? O87 Na3 Na2 43.67(3) . . ? O89 Na3 Na2 71.49(3) . . ? O93 Na3 Na2 131.44(3) 2_654 . ? O90 Na3 Na2 129.94(4) 2_644 . ? O90 Na3 Na2 78.79(3) . . ? Na3 Na3 Na2 107.66(3) 2_644 . ? O87 Na3 Na4 78.22(3) . 2_654 ? O89 Na3 Na4 93.46(3) . 2_654 ? O93 Na3 Na4 29.09(3) 2_654 2_654 ? O90 Na3 Na4 87.69(3) 2_644 2_654 ? O90 Na3 Na4 167.94(3) . 2_654 ? Na3 Na3 Na4 129.48(2) 2_644 2_654 ? Na2 Na3 Na4 113.220(17) . 2_654 ? O83 Na4 O41 98.96(4) 2_554 . ? O83 Na4 O91 89.11(4) 2_554 . ? O41 Na4 O91 93.40(4) . . ? O83 Na4 O93 118.53(4) 2_554 . ? O41 Na4 O93 85.67(4) . . ? O91 Na4 O93 152.19(5) . . ? O83 Na4 O92 84.17(4) 2_554 . ? O41 Na4 O92 168.57(4) . . ? O91 Na4 O92 97.66(4) . . ? O93 Na4 O92 83.20(4) . . ? O83 Na4 Na1 44.09(3) 2_554 2_554 ? O41 Na4 Na1 102.30(3) . 2_554 ? O91 Na4 Na1 45.26(3) . 2_554 ? O93 Na4 Na1 161.40(4) . 2_554 ? O92 Na4 Na1 87.63(3) . 2_554 ? O83 Na4 Na3 89.61(3) 2_554 2_654 ? O41 Na4 Na3 88.33(3) . 2_654 ? O91 Na4 Na3 177.99(3) . 2_654 ? O93 Na4 Na3 28.97(3) . 2_654 ? O92 Na4 Na3 80.67(3) . 2_654 ? Na1 Na4 Na3 133.31(2) 2_554 2_654 ? O83 Na4 H93B 122.9(4) 2_554 . ? O41 Na4 H93B 69.0(4) . . ? O91 Na4 H93B 144.6(4) . . ? O93 Na4 H93B 17.1(4) . . ? O92 Na4 H93B 100.1(4) . . ? Na1 Na4 H93B 164.6(4) 2_554 . ? Na3 Na4 H93B 37.2(4) 2_654 . ? 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 O2 P1 C1 C2 -68.13(10) . . . . ? O3 P1 C1 C2 172.39(9) . . . . ? O1 P1 C1 C2 52.33(10) . . . . ? P1 C1 C2 C3 156.02(9) . . . . ? C1 C2 C3 C11 54.54(14) . . . . ? C1 C2 C3 C31 -68.89(14) . . . . ? C1 C2 C3 C21 173.01(10) . . . . ? C31 C3 C11 C16 22.89(19) . . . . ? C21 C3 C11 C16 141.62(14) . . . . ? C2 C3 C11 C16 -99.57(15) . . . . ? C31 C3 C11 C12 -164.37(13) . . . . ? C21 C3 C11 C12 -45.64(17) . . . . ? C2 C3 C11 C12 73.17(15) . . . . ? C16 C11 C12 C13 -1.6(2) . . . . ? C3 C11 C12 C13 -174.72(14) . . . . ? C11 C12 C13 C14 1.9(3) . . . . ? C12 C13 C14 C15 -1.1(3) . . . . ? C13 C14 C15 C16 0.0(3) . . . . ? C12 C11 C16 C15 0.5(2) . . . . ? C3 C11 C16 C15 173.32(14) . . . . ? C14 C15 C16 C11 0.2(3) . . . . ? C11 C3 C21 C26 -39.33(16) . . . . ? C31 C3 C21 C26 83.26(15) . . . . ? C2 C3 C21 C26 -155.72(13) . . . . ? C11 C3 C21 C22 142.32(12) . . . . ? C31 C3 C21 C22 -95.10(14) . . . . ? C2 C3 C21 C22 25.92(16) . . . . ? C26 C21 C22 C23 0.3(2) . . . . ? C3 C21 C22 C23 178.69(12) . . . . ? C21 C22 C23 C24 -0.8(2) . . . . ? C22 C23 C24 C25 0.7(2) . . . . ? C23 C24 C25 C26 -0.2(2) . . . . ? C22 C21 C26 C25 0.2(2) . . . . ? C3 C21 C26 C25 -178.19(13) . . . . ? C24 C25 C26 C21 -0.3(2) . . . . ? C11 C3 C31 C32 -132.00(13) . . . . ? C21 C3 C31 C32 107.60(14) . . . . ? C2 C3 C31 C32 -12.52(17) . . . . ? C11 C3 C31 C36 50.79(16) . . . . ? C21 C3 C31 C36 -69.60(15) . . . . ? C2 C3 C31 C36 170.27(12) . . . . ? C36 C31 C32 C33 -0.5(2) . . . . ? C3 C31 C32 C33 -177.83(12) . . . . ? C31 C32 C33 C34 -0.5(2) . . . . ? C32 C33 C34 C35 1.0(2) . . . . ? C33 C34 C35 C36 -0.5(2) . . . . ? C34 C35 C36 C31 -0.5(2) . . . . ? C32 C31 C36 C35 1.0(2) . . . . ? C3 C31 C36 C35 178.36(13) . . . . ? O43 P41 C41 C42 175.04(9) . . . . ? O42 P41 C41 C42 -64.55(10) . . . . ? O41 P41 C41 C42 53.83(10) . . . . ? P41 C41 C42 C43 156.58(9) . . . . ? C41 C42 C43 C51 57.99(14) . . . . ? C41 C42 C43 C71 -65.30(14) . . . . ? C41 C42 C43 C61 177.45(10) . . . . ? C71 C43 C51 C56 28.60(19) . . . . ? C61 C43 C51 C56 146.32(14) . . . . ? C42 C43 C51 C56 -93.87(16) . . . . ? C71 C43 C51 C52 -158.48(13) . . . . ? C61 C43 C51 C52 -40.76(17) . . . . ? C42 C43 C51 C52 79.05(15) . . . . ? C56 C51 C52 C53 -1.6(2) . . . . ? C43 C51 C52 C53 -174.87(14) . . . . ? C51 C52 C53 C54 1.4(3) . . . . ? C52 C53 C54 C55 -0.7(3) . . . . ? C53 C54 C55 C56 0.1(3) . . . . ? C52 C51 C56 C55 1.1(2) . . . . ? C43 C51 C56 C55 174.09(15) . . . . ? C54 C55 C56 C51 -0.4(3) . . . . ? C51 C43 C61 C66 -42.72(16) . . . . ? C71 C43 C61 C66 79.30(15) . . . . ? C42 C43 C61 C66 -159.94(12) . . . . ? C51 C43 C61 C62 140.39(13) . . . . ? C71 C43 C61 C62 -97.59(14) . . . . ? C42 C43 C61 C62 23.16(16) . . . . ? C66 C61 C62 C63 -0.6(2) . . . . ? C43 C61 C62 C63 176.35(12) . . . . ? C61 C62 C63 C64 -0.2(2) . . . . ? C62 C63 C64 C65 0.8(2) . . . . ? C63 C64 C65 C66 -0.6(2) . . . . ? C62 C61 C66 C65 0.9(2) . . . . ? C43 C61 C66 C65 -176.19(13) . . . . ? C64 C65 C66 C61 -0.2(2) . . . . ? C51 C43 C71 C76 -136.69(13) . . . . ? C61 C43 C71 C76 103.06(14) . . . . ? C42 C43 C71 C76 -17.12(16) . . . . ? C51 C43 C71 C72 46.97(16) . . . . ? C61 C43 C71 C72 -73.28(15) . . . . ? C42 C43 C71 C72 166.54(12) . . . . ? C76 C71 C72 C73 0.8(2) . . . . ? C43 C71 C72 C73 177.26(13) . . . . ? C71 C72 C73 C74 0.0(2) . . . . ? C72 C73 C74 C75 -0.6(2) . . . . ? C73 C74 C75 C76 0.4(2) . . . . ? C72 C71 C76 C75 -1.0(2) . . . . ? C43 C71 C76 C75 -177.47(12) . . . . ? C74 C75 C76 C71 0.5(2) . . . . ? O43 P41 O41 Na4 172.71(6) . . . . ? O42 P41 O41 Na4 46.68(8) . . . . ? C41 P41 O41 Na4 -69.24(8) . . . . ? Na2 O84 Na1 O81 127.4(4) . . . . ? Na2 O84 Na1 O81 146.61(6) . . . 2_554 ? Na2 O84 Na1 O82 50.82(6) . . . . ? Na2 O84 Na1 O83 -30.58(6) . . . . ? Na2 O84 Na1 O91 -115.55(6) . . . 2_554 ? Na2 O84 Na1 Na4 -72.33(5) . . . 2_554 ? Na2 O84 Na1 Na1 144.66(5) . . . 2_554 ? Na1 O81 Na1 O84 19.3(4) 2_554 . . . ? Na1 O81 Na1 O81 0.0 2_554 . . 2_554 ? Na1 O81 Na1 O82 96.28(4) 2_554 . . . ? Na1 O81 Na1 O83 177.15(5) 2_554 . . . ? Na1 O81 Na1 O91 -97.63(4) 2_554 . . 2_554 ? Na1 O81 Na1 Na4 -141.06(4) 2_554 . . 2_554 ? Na1 O81 Na1 Na2 136.67(6) 2_554 . . . ? Na4 O83 Na1 O84 -94.77(4) 2_554 . . . ? Na4 O83 Na1 O81 87.71(4) 2_554 . . . ? Na4 O83 Na1 O81 -164.9(8) 2_554 . . 2_554 ? Na4 O83 Na1 O82 172.10(4) 2_554 . . . ? Na4 O83 Na1 O91 -5.02(4) 2_554 . . 2_554 ? Na4 O83 Na1 Na1 90.62(6) 2_554 . . 2_554 ? Na4 O83 Na1 Na2 -111.65(4) 2_554 . . . ? Na1 O84 Na2 O85 -49.46(7) . . . . ? Na1 O84 Na2 O88 -178.42(10) . . . . ? Na1 O84 Na2 O86 56.06(6) . . . . ? Na1 O84 Na2 O87 -171.22(6) . . . . ? Na1 O84 Na2 Na3 147.07(5) . . . . ? Na3 O87 Na2 O85 -166.25(6) . . . . ? Na3 O87 Na2 O88 92.71(5) . . . . ? Na3 O87 Na2 O86 1.15(8) . . . . ? Na3 O87 Na2 O84 -84.48(5) . . . . ? Na3 O87 Na2 Na1 -89.06(4) . . . . ? O84 Na1 Na2 O85 126.56(7) . . . . ? O81 Na1 Na2 O85 -42.01(8) . . . . ? O81 Na1 Na2 O85 89.75(5) 2_554 . . . ? O82 Na1 Na2 O85 0.21(5) . . . . ? O83 Na1 Na2 O85 -87.65(5) . . . . ? O91 Na1 Na2 O85 -165.77(5) 2_554 . . . ? Na4 Na1 Na2 O85 -126.13(4) 2_554 . . . ? Na1 Na1 Na2 O85 60.48(7) 2_554 . . . ? O84 Na1 Na2 O88 175.2(3) . . . . ? O81 Na1 Na2 O88 6.7(3) . . . . ? O81 Na1 Na2 O88 138.4(3) 2_554 . . . ? O82 Na1 Na2 O88 48.9(3) . . . . ? O83 Na1 Na2 O88 -39.0(3) . . . . ? O91 Na1 Na2 O88 -117.1(3) 2_554 . . . ? Na4 Na1 Na2 O88 -77.4(3) 2_554 . . . ? Na1 Na1 Na2 O88 109.2(3) 2_554 . . . ? O84 Na1 Na2 O86 -122.96(7) . . . . ? O81 Na1 Na2 O86 68.47(8) . . . . ? O81 Na1 Na2 O86 -159.77(4) 2_554 . . . ? O82 Na1 Na2 O86 110.69(4) . . . . ? O83 Na1 Na2 O86 22.83(4) . . . . ? O91 Na1 Na2 O86 -55.29(4) 2_554 . . . ? Na4 Na1 Na2 O86 -15.65(3) 2_554 . . . ? Na1 Na1 Na2 O86 170.96(6) 2_554 . . . ? O81 Na1 Na2 O84 -168.58(9) . . . . ? O81 Na1 Na2 O84 -36.81(6) 2_554 . . . ? O82 Na1 Na2 O84 -126.36(6) . . . . ? O83 Na1 Na2 O84 145.79(7) . . . . ? O91 Na1 Na2 O84 67.67(6) 2_554 . . . ? Na4 Na1 Na2 O84 107.31(6) 2_554 . . . ? Na1 Na1 Na2 O84 -66.09(8) 2_554 . . . ? O84 Na1 Na2 O87 8.86(6) . . . . ? O81 Na1 Na2 O87 -159.71(7) . . . . ? O81 Na1 Na2 O87 -27.95(5) 2_554 . . . ? O82 Na1 Na2 O87 -117.49(4) . . . . ? O83 Na1 Na2 O87 154.65(4) . . . . ? O91 Na1 Na2 O87 76.53(4) 2_554 . . . ? Na4 Na1 Na2 O87 116.17(3) 2_554 . . . ? Na1 Na1 Na2 O87 -57.22(6) 2_554 . . . ? O84 Na1 Na2 Na3 -32.56(6) . . . . ? O81 Na1 Na2 Na3 158.87(7) . . . . ? O81 Na1 Na2 Na3 -69.37(4) 2_554 . . . ? O82 Na1 Na2 Na3 -158.91(3) . . . . ? O83 Na1 Na2 Na3 113.24(3) . . . . ? O91 Na1 Na2 Na3 35.11(3) 2_554 . . . ? Na4 Na1 Na2 Na3 74.752(18) 2_554 . . . ? Na1 Na1 Na2 Na3 -98.64(5) 2_554 . . . ? Na2 O87 Na3 O89 51.50(5) . . . . ? Na2 O87 Na3 O93 134.28(4) . . . 2_654 ? Na2 O87 Na3 O90 -132.48(4) . . . 2_644 ? Na2 O87 Na3 O90 -41.43(5) . . . . ? Na2 O87 Na3 Na3 -88.28(4) . . . 2_644 ? Na2 O87 Na3 Na4 143.28(4) . . . 2_654 ? Na3 O90 Na3 O87 -104.65(5) 2_644 . . . ? Na3 O90 Na3 O89 156.33(5) 2_644 . . . ? Na3 O90 Na3 O93 81.91(7) 2_644 . . 2_654 ? Na3 O90 Na3 O90 0.0 2_644 . . 2_644 ? Na3 O90 Na3 Na2 -132.41(4) 2_644 . . . ? Na3 O90 Na3 Na4 52.72(17) 2_644 . . 2_654 ? O85 Na2 Na3 O87 33.94(14) . . . . ? O88 Na2 Na3 O87 -82.27(5) . . . . ? O86 Na2 Na3 O87 -179.16(6) . . . . ? O84 Na2 Na3 O87 85.01(5) . . . . ? Na1 Na2 Na3 O87 101.19(5) . . . . ? O85 Na2 Na3 O89 -91.36(14) . . . . ? O88 Na2 Na3 O89 152.43(4) . . . . ? O86 Na2 Na3 O89 55.54(4) . . . . ? O84 Na2 Na3 O89 -40.29(4) . . . . ? O87 Na2 Na3 O89 -125.30(5) . . . . ? Na1 Na2 Na3 O89 -24.10(3) . . . . ? O85 Na2 Na3 O93 -32.78(15) . . . 2_654 ? O88 Na2 Na3 O93 -148.99(5) . . . 2_654 ? O86 Na2 Na3 O93 114.12(5) . . . 2_654 ? O84 Na2 Na3 O93 18.29(5) . . . 2_654 ? O87 Na2 Na3 O93 -66.72(6) . . . 2_654 ? Na1 Na2 Na3 O93 34.48(5) . . . 2_654 ? O85 Na2 Na3 O90 101.95(14) . . . 2_644 ? O88 Na2 Na3 O90 -14.26(5) . . . 2_644 ? O86 Na2 Na3 O90 -111.14(5) . . . 2_644 ? O84 Na2 Na3 O90 153.03(5) . . . 2_644 ? O87 Na2 Na3 O90 68.01(6) . . . 2_644 ? Na1 Na2 Na3 O90 169.21(4) . . . 2_644 ? O85 Na2 Na3 O90 175.54(13) . . . . ? O88 Na2 Na3 O90 59.33(4) . . . . ? O86 Na2 Na3 O90 -37.55(4) . . . . ? O84 Na2 Na3 O90 -133.38(4) . . . . ? O87 Na2 Na3 O90 141.61(6) . . . . ? Na1 Na2 Na3 O90 -117.20(3) . . . . ? O85 Na2 Na3 Na3 144.00(13) . . . 2_644 ? O88 Na2 Na3 Na3 27.79(4) . . . 2_644 ? O86 Na2 Na3 Na3 -69.10(4) . . . 2_644 ? O84 Na2 Na3 Na3 -164.93(4) . . . 2_644 ? O87 Na2 Na3 Na3 110.06(5) . . . 2_644 ? Na1 Na2 Na3 Na3 -148.75(2) . . . 2_644 ? O85 Na2 Na3 Na4 -5.62(14) . . . 2_654 ? O88 Na2 Na3 Na4 -121.83(3) . . . 2_654 ? O86 Na2 Na3 Na4 141.28(3) . . . 2_654 ? O84 Na2 Na3 Na4 45.45(3) . . . 2_654 ? O87 Na2 Na3 Na4 -39.56(5) . . . 2_654 ? Na1 Na2 Na3 Na4 61.63(2) . . . 2_654 ? P41 O41 Na4 O83 -153.09(7) . . . 2_554 ? P41 O41 Na4 O91 117.27(7) . . . . ? P41 O41 Na4 O93 -34.87(7) . . . . ? P41 O41 Na4 O92 -48.0(3) . . . . ? P41 O41 Na4 Na1 162.13(6) . . . 2_554 ? P41 O41 Na4 Na3 -63.76(7) . . . 2_654 ? Na1 O91 Na4 O83 5.07(4) 2_554 . . 2_554 ? Na1 O91 Na4 O41 103.99(4) 2_554 . . . ? Na1 O91 Na4 O93 -168.86(8) 2_554 . . . ? Na1 O91 Na4 O92 -78.92(4) 2_554 . . . ? Na1 O91 Na4 Na3 -45.2(11) 2_554 . . 2_654 ? Na3 O93 Na4 O83 3.46(7) 2_654 . . 2_554 ? Na3 O93 Na4 O41 -94.38(6) 2_654 . . . ? Na3 O93 Na4 O91 176.55(7) 2_654 . . . ? Na3 O93 Na4 O92 83.01(6) 2_654 . . . ? Na3 O93 Na4 Na1 22.03(15) 2_654 . . 2_554 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O81 H81A O2 0.809(18) 2.029(19) 2.8237(15) 167.5(17) 1_455 O81 H81B O3 0.844(18) 1.896(18) 2.7381(14) 175.7(16) 2_554 O82 H82A O2 0.790(18) 1.903(18) 2.6867(13) 171.6(19) 1_455 O83 H83B O1 0.834(17) 2.012(17) 2.8289(13) 166.4(16) 1_455 O84 H84A O1 0.813(18) 2.117(19) 2.9146(14) 166.8(17) . O86 H86A O41 0.776(19) 2.017(19) 2.7850(15) 170.6(19) 2_554 O86 H86B O43 0.840(19) 1.953(19) 2.7923(15) 176.3(17) 1_545 O87 H87A O1 0.821(18) 1.994(19) 2.8050(14) 169.2(17) . O88 H88A O42 0.823(19) 1.89(2) 2.7012(14) 171(2) 1_545 O89 H89B O41 0.848(18) 1.793(18) 2.6399(13) 177.5(17) 2_554 O90 H90A O42 0.805(19) 2.034(19) 2.8253(15) 167.7(18) 1_545 O90 H90B O43 0.835(18) 1.932(18) 2.7656(14) 176.2(17) 2_554 O92 H92A O3 0.845(19) 1.911(19) 2.7558(15) 177.8(18) . O93 H93B O42 0.789(17) 1.854(18) 2.6385(13) 173.1(18) . O101 H10A O3 0.818(19) 1.81(2) 2.6245(14) 174.2(19) . O102 H10D O2 0.857(19) 1.933(19) 2.7671(14) 163.9(18) 1_455 O104 H10G O43 0.869(19) 1.81(2) 2.6777(15) 172.1(19) . O92 H92B O1 0.824(19) 1.99(2) 2.8081(15) 170.1(18) 2_654 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.425 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.057 #===END data_kp020310 _database_code_depnum_ccdc_archive 'CCDC 782186' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 Na2 O7 P2' _chemical_formula_weight 438.29 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' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.4328(3) _cell_length_b 8.63377(13) _cell_length_c 12.2755(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.6314(15) _cell_angle_gamma 90.00 _cell_volume 2158.48(6) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 11667 _cell_measurement_theta_min 2.5571 _cell_measurement_theta_max 32.6597 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9273 _exptl_absorpt_correction_T_max 0.9918 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26469 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 30.51 _reflns_number_total 6589 _reflns_number_gt 4795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0489P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6589 _refine_ls_number_parameters 264 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 C1 C 0.17744(6) 0.08226(14) -0.37022(11) 0.0224(3) Uani 1 1 d . . . H1A H 0.1715 0.1334 -0.4425 0.027 Uiso 1 1 calc R . . H1B H 0.1917 0.1619 -0.3153 0.027 Uiso 1 1 calc R . . C2 C 0.23046(6) -0.04202(15) -0.37272(11) 0.0239(3) Uani 1 1 d . . . H2A H 0.2107 -0.1358 -0.4083 0.029 Uiso 1 1 calc R . . H2B H 0.2455 -0.0699 -0.2966 0.029 Uiso 1 1 calc R . . C5 C 0.17904(9) -0.4499(2) -0.21469(18) 0.0546(5) Uani 1 1 d . . . H5A H 0.2068 -0.4076 -0.2690 0.082 Uiso 1 1 calc R . . H5B H 0.1788 -0.5632 -0.2193 0.082 Uiso 1 1 calc R . . H5C H 0.1965 -0.4181 -0.1414 0.082 Uiso 1 1 calc R . . C6 C 0.21483(8) -0.5228(2) -0.51113(15) 0.0459(4) Uani 1 1 d . . . H6C H 0.2253 -0.6133 -0.5547 0.069 Uiso 1 1 calc R . . H6B H 0.2279 -0.5429 -0.4339 0.069 Uiso 1 1 calc R . . H6A H 0.2386 -0.4323 -0.5355 0.069 Uiso 1 1 calc R . . C11 C 0.35821(7) 0.10571(15) -0.33916(11) 0.0240(3) Uani 1 1 d . . . C12 C 0.33784(7) 0.17691(18) -0.24595(12) 0.0328(3) Uani 1 1 d . . . H12 H 0.2925 0.1769 -0.2335 0.039 Uiso 1 1 calc R . . C13 C 0.38250(9) 0.24785(18) -0.17100(14) 0.0410(4) Uani 1 1 d . . . H13 H 0.3675 0.2956 -0.1079 0.049 Uiso 1 1 calc R . . C14 C 0.44821(9) 0.24992(18) -0.18692(15) 0.0433(4) Uani 1 1 d . . . H14 H 0.4787 0.2974 -0.1347 0.052 Uiso 1 1 calc R . . C15 C 0.46947(8) 0.1826(2) -0.27922(15) 0.0457(4) Uani 1 1 d . . . H15 H 0.5148 0.1845 -0.2912 0.055 Uiso 1 1 calc R . . C16 C 0.42507(7) 0.11211(18) -0.35490(14) 0.0360(4) Uani 1 1 d . . . H16 H 0.4404 0.0672 -0.4187 0.043 Uiso 1 1 calc R . . C21 C 0.34359(6) -0.17385(16) -0.45308(11) 0.0242(3) Uani 1 1 d . . . C22 C 0.35056(7) -0.27683(18) -0.36523(12) 0.0326(3) Uani 1 1 d . . . H22 H 0.3345 -0.2486 -0.2975 0.039 Uiso 1 1 calc R . . C23 C 0.38034(8) -0.41851(19) -0.37506(14) 0.0388(4) Uani 1 1 d . . . H23 H 0.3838 -0.4880 -0.3149 0.047 Uiso 1 1 calc R . . C24 C 0.40520(9) -0.45991(19) -0.47246(15) 0.0431(4) Uani 1 1 d . . . H24 H 0.4268 -0.5566 -0.4788 0.052 Uiso 1 1 calc R . . C25 C 0.39853(10) -0.3608(2) -0.55968(15) 0.0482(5) Uani 1 1 d . . . H25 H 0.4149 -0.3898 -0.6270 0.058 Uiso 1 1 calc R . . C26 C 0.36802(8) -0.21810(18) -0.55055(13) 0.0360(4) Uani 1 1 d . . . H26 H 0.3639 -0.1502 -0.6116 0.043 Uiso 1 1 calc R . . O1 O 0.11378(4) -0.09228(10) -0.23039(7) 0.01960(19) Uani 1 1 d . . . O2 O 0.05284(4) 0.13311(10) -0.31865(7) 0.0219(2) Uani 1 1 d . . . O3 O 0.07444(4) -0.10154(10) -0.43113(7) 0.02041(19) Uani 1 1 d . . . O5 O 0.11431(5) -0.39350(11) -0.23536(8) 0.0266(2) Uani 1 1 d . . . H5D H 0.1161(8) -0.301(2) -0.2320(14) 0.040 Uiso 1 1 d . . . O6 O 0.14620(5) -0.49387(12) -0.52453(8) 0.0304(2) Uani 1 1 d D . . H6D H 0.1391(9) -0.473(2) -0.5870(12) 0.046 Uiso 1 1 d D . . O7 O 0.00220(5) -0.39661(10) -0.60538(7) 0.02069(19) Uani 1 1 d . . . H7A H -0.0223(8) -0.321(2) -0.6225(12) 0.031 Uiso 1 1 d . . . H7B H 0.0319(8) -0.4037(18) -0.6496(13) 0.031 Uiso 1 1 d . . . O8 O -0.06380(6) -0.25050(11) -0.38559(9) 0.0307(2) Uani 1 1 d D . . H8A H -0.0631(8) -0.282(2) -0.3192(15) 0.046 Uiso 1 1 d . . . H8B H -0.0893(8) -0.304(2) -0.4205(14) 0.046 Uiso 1 1 d D . . Na1 Na 0.05386(3) -0.36793(5) -0.42395(4) 0.02232(12) Uani 1 1 d . . . Na2 Na -0.04523(3) 0.01233(5) -0.39567(4) 0.02077(12) Uani 1 1 d . . . P1 P 0.099919(15) 0.00012(3) -0.33667(2) 0.01437(7) Uani 1 1 d . . . P2 P 0.302713(17) 0.01477(4) -0.44494(3) 0.02307(9) 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 C1 0.0190(6) 0.0179(6) 0.0304(7) 0.0027(5) 0.0019(5) -0.0016(5) C2 0.0176(6) 0.0235(6) 0.0312(7) 0.0026(5) 0.0046(5) -0.0006(5) C5 0.0424(11) 0.0448(10) 0.0778(14) 0.0113(10) 0.0127(10) 0.0149(9) C6 0.0323(9) 0.0583(11) 0.0456(10) 0.0116(8) -0.0058(8) -0.0014(8) C11 0.0207(7) 0.0234(6) 0.0281(7) 0.0043(5) 0.0020(5) -0.0017(5) C12 0.0265(8) 0.0365(8) 0.0353(8) -0.0048(6) 0.0024(6) 0.0009(6) C13 0.0483(11) 0.0351(9) 0.0385(9) -0.0094(7) -0.0038(8) 0.0022(7) C14 0.0414(10) 0.0349(9) 0.0507(10) -0.0009(7) -0.0141(8) -0.0103(7) C15 0.0268(9) 0.0533(11) 0.0560(11) 0.0034(9) -0.0020(8) -0.0104(7) C16 0.0243(8) 0.0451(9) 0.0391(9) 0.0004(7) 0.0053(7) -0.0039(7) C21 0.0196(7) 0.0279(7) 0.0251(7) -0.0021(5) 0.0022(5) -0.0022(5) C22 0.0311(8) 0.0409(8) 0.0257(7) 0.0003(6) 0.0017(6) 0.0077(6) C23 0.0389(9) 0.0363(8) 0.0400(9) 0.0053(7) -0.0040(7) 0.0054(7) C24 0.0429(10) 0.0319(8) 0.0543(11) -0.0100(8) 0.0035(8) 0.0066(7) C25 0.0600(12) 0.0418(10) 0.0456(10) -0.0120(8) 0.0223(9) 0.0045(8) C26 0.0453(10) 0.0350(8) 0.0293(8) -0.0020(6) 0.0124(7) -0.0024(7) O1 0.0239(5) 0.0192(4) 0.0154(4) 0.0015(3) -0.0004(4) 0.0031(3) O2 0.0224(5) 0.0190(4) 0.0241(5) 0.0009(3) 0.0009(4) 0.0060(3) O3 0.0254(5) 0.0182(4) 0.0170(4) -0.0003(3) -0.0024(4) -0.0033(3) O5 0.0326(6) 0.0193(4) 0.0279(5) 0.0018(4) 0.0029(4) 0.0011(4) O6 0.0290(6) 0.0410(6) 0.0206(5) 0.0051(4) -0.0016(4) -0.0011(4) O7 0.0239(5) 0.0176(4) 0.0210(5) 0.0037(4) 0.0044(4) 0.0046(4) O8 0.0444(7) 0.0234(5) 0.0240(5) 0.0022(4) 0.0009(5) -0.0096(4) Na1 0.0304(3) 0.0170(2) 0.0190(2) 0.00072(19) -0.0016(2) -0.0042(2) Na2 0.0232(3) 0.0210(2) 0.0176(2) 0.00057(19) -0.0012(2) -0.0005(2) P1 0.01463(14) 0.01363(14) 0.01463(14) 0.00061(11) -0.00010(11) 0.00082(11) P2 0.01940(17) 0.02764(18) 0.02247(17) 0.00268(13) 0.00361(14) -0.00051(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 C1 C2 1.5269(18) . ? C1 P1 1.8129(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 P2 1.8486(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 O5 1.413(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O6 1.4207(19) . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C6 H6A 0.9800 . ? C11 C12 1.392(2) . ? C11 C16 1.3962(19) . ? C11 P2 1.8305(14) . ? C12 C13 1.385(2) . ? C12 H12 0.9500 . ? C13 C14 1.372(2) . ? C13 H13 0.9500 . ? C14 C15 1.375(3) . ? C14 H14 0.9500 . ? C15 C16 1.386(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.3867(19) . ? C21 C22 1.396(2) . ? C21 P2 1.8366(14) . ? C22 C23 1.376(2) . ? C22 H22 0.9500 . ? C23 C24 1.383(2) . ? C23 H23 0.9500 . ? C24 C25 1.369(3) . ? C24 H24 0.9500 . ? C25 C26 1.389(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O1 P1 1.5360(9) . ? O2 P1 1.5255(9) . ? O2 Na2 2.3855(11) . ? O3 P1 1.5127(9) . ? O3 Na2 2.2946(10) 3_554 ? O3 Na1 2.3410(10) . ? O3 Na2 2.7030(10) . ? O5 Na2 2.3680(11) 2_544 ? O5 Na1 2.5441(11) . ? O5 H5D 0.797(18) . ? O6 Na1 2.5775(12) . ? O6 H6D 0.789(14) . ? O7 Na1 2.3751(10) 3_544 ? O7 Na1 2.3992(10) . ? O7 H7A 0.838(17) . ? O7 H7B 0.849(17) . ? O8 Na2 2.3057(11) . ? O8 Na1 2.6854(13) . ? O8 H8A 0.860(19) . ? O8 H8B 0.795(14) . ? Na1 O7 2.3750(10) 3_544 ? Na1 P1 3.4595(6) . ? Na1 Na1 3.5872(10) 3_544 ? Na1 Na2 3.7811(7) 3_554 ? Na1 Na2 3.8873(7) . ? Na1 Na2 4.0749(7) 2_544 ? Na1 H5D 2.649(17) . ? Na2 O3 2.2946(10) 3_554 ? Na2 O5 2.3680(11) 2_554 ? 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 C2 C1 P1 111.35(9) . . ? C2 C1 H1A 109.4 . . ? P1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 P2 114.75(9) . . ? C1 C2 H2A 108.6 . . ? P2 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? P2 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O6 C6 H6C 109.5 . . ? O6 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? O6 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? C12 C11 C16 117.21(14) . . ? C12 C11 P2 124.29(11) . . ? C16 C11 P2 118.41(11) . . ? C13 C12 C11 121.10(15) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.72(16) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.33(16) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 120.32(16) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 121.30(15) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? C26 C21 C22 118.01(13) . . ? C26 C21 P2 119.22(11) . . ? C22 C21 P2 122.76(10) . . ? C23 C22 C21 121.11(14) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 120.10(15) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 119.62(15) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.55(15) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C21 C26 C25 120.60(15) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? P1 O2 Na2 97.63(4) . . ? P1 O3 Na2 124.27(5) . 3_554 ? P1 O3 Na1 126.37(5) . . ? Na2 O3 Na1 109.30(4) 3_554 . ? P1 O3 Na2 85.72(4) . . ? Na2 O3 Na2 81.73(3) 3_554 . ? Na1 O3 Na2 100.58(3) . . ? C5 O5 Na2 111.12(10) . 2_544 ? C5 O5 Na1 124.89(11) . . ? Na2 O5 Na1 112.06(4) 2_544 . ? C5 O5 H5D 107.2(13) . . ? Na2 O5 H5D 109.6(12) 2_544 . ? Na1 O5 H5D 88.7(13) . . ? C6 O6 Na1 140.59(10) . . ? C6 O6 H6D 104.7(14) . . ? Na1 O6 H6D 106.7(14) . . ? Na1 O7 Na1 97.41(4) 3_544 . ? Na1 O7 H7A 114.8(11) 3_544 . ? Na1 O7 H7A 111.2(11) . . ? Na1 O7 H7B 114.5(11) 3_544 . ? Na1 O7 H7B 108.5(11) . . ? H7A O7 H7B 109.8(14) . . ? Na2 O8 Na1 102.04(4) . . ? Na2 O8 H8A 112.1(12) . . ? Na1 O8 H8A 95.7(12) . . ? Na2 O8 H8B 130.3(14) . . ? Na1 O8 H8B 104.0(13) . . ? H8A O8 H8B 106.5(17) . . ? O3 Na1 O7 159.54(4) . 3_544 ? O3 Na1 O7 97.66(3) . . ? O7 Na1 O7 82.58(4) 3_544 . ? O3 Na1 O5 92.52(3) . . ? O7 Na1 O5 89.57(3) 3_544 . ? O7 Na1 O5 168.72(4) . . ? O3 Na1 O6 104.82(4) . . ? O7 Na1 O6 95.29(4) 3_544 . ? O7 Na1 O6 78.23(4) . . ? O5 Na1 O6 94.52(4) . . ? O3 Na1 O8 78.57(3) . . ? O7 Na1 O8 81.20(4) 3_544 . ? O7 Na1 O8 82.46(4) . . ? O5 Na1 O8 104.42(4) . . ? O6 Na1 O8 160.66(4) . . ? O3 Na1 P1 20.62(2) . . ? O7 Na1 P1 149.52(3) 3_544 . ? O7 Na1 P1 118.07(3) . . ? O5 Na1 P1 72.42(2) . . ? O6 Na1 P1 110.15(3) . . ? O8 Na1 P1 79.86(3) . . ? O3 Na1 Na1 135.20(3) . 3_544 ? O7 Na1 Na1 41.55(2) 3_544 3_544 ? O7 Na1 Na1 41.04(2) . 3_544 ? O5 Na1 Na1 130.61(3) . 3_544 ? O6 Na1 Na1 85.67(3) . 3_544 ? O8 Na1 Na1 79.10(3) . 3_544 ? P1 Na1 Na1 152.29(2) . 3_544 ? O3 Na1 Na2 34.94(2) . 3_554 ? O7 Na1 Na2 141.58(3) 3_544 3_554 ? O7 Na1 Na2 62.87(2) . 3_554 ? O5 Na1 Na2 126.84(3) . 3_554 ? O6 Na1 Na2 93.63(3) . 3_554 ? O8 Na1 Na2 78.23(3) . 3_554 ? P1 Na1 Na2 55.543(11) . 3_554 ? Na1 Na1 Na2 102.34(2) 3_544 3_554 ? O3 Na1 Na2 43.12(3) . . ? O7 Na1 Na2 116.64(3) 3_544 . ? O7 Na1 Na2 88.67(3) . . ? O5 Na1 Na2 102.13(3) . . ? O6 Na1 Na2 143.68(3) . . ? O8 Na1 Na2 35.46(2) . . ? P1 Na1 Na2 47.719(11) . . ? Na1 Na1 Na2 106.34(2) 3_544 . ? Na2 Na1 Na2 50.695(15) 3_554 . ? O3 Na1 Na2 107.90(3) . 2_544 ? O7 Na1 Na2 65.04(3) 3_544 2_544 ? O7 Na1 Na2 144.84(3) . 2_544 ? O5 Na1 Na2 32.59(2) . 2_544 ? O6 Na1 Na2 116.39(3) . 2_544 ? O8 Na1 Na2 79.52(3) . 2_544 ? P1 Na1 Na2 88.093(13) . 2_544 ? Na1 Na1 Na2 105.51(2) 3_544 2_544 ? Na2 Na1 Na2 140.020(15) 3_554 2_544 ? Na2 Na1 Na2 93.725(13) . 2_544 ? O3 Na1 H5D 75.3(4) . . ? O7 Na1 H5D 104.7(4) 3_544 . ? O7 Na1 H5D 172.7(4) . . ? O5 Na1 H5D 17.5(4) . . ? O6 Na1 H5D 101.5(4) . . ? O8 Na1 H5D 97.8(4) . . ? P1 Na1 H5D 55.0(4) . . ? Na1 Na1 H5D 146.2(4) 3_544 . ? Na2 Na1 H5D 110.0(4) 3_554 . ? Na2 Na1 H5D 87.4(4) . . ? Na2 Na1 H5D 41.7(4) 2_544 . ? O3 Na2 O8 110.39(4) 3_554 . ? O3 Na2 O5 112.92(4) 3_554 2_554 ? O8 Na2 O5 101.05(4) . 2_554 ? O3 Na2 O2 111.58(4) 3_554 . ? O8 Na2 O2 123.06(4) . . ? O5 Na2 O2 96.22(4) 2_554 . ? O3 Na2 O3 98.27(3) 3_554 . ? O8 Na2 O3 78.79(4) . . ? O5 Na2 O3 146.19(4) 2_554 . ? O2 Na2 O3 58.74(3) . . ? O3 Na2 P1 114.45(3) 3_554 . ? O8 Na2 P1 96.68(3) . . ? O5 Na2 P1 118.71(3) 2_554 . ? O2 Na2 P1 30.29(2) . . ? O3 Na2 P1 30.216(19) . . ? O3 Na2 Na2 54.53(3) 3_554 3_554 ? O8 Na2 Na2 94.79(3) . 3_554 ? O5 Na2 Na2 162.91(4) 2_554 3_554 ? O2 Na2 Na2 80.21(3) . 3_554 ? O3 Na2 Na2 43.74(2) . 3_554 ? P1 Na2 Na2 65.041(17) . 3_554 ? O3 Na2 P1 21.67(2) 3_554 3_554 ? O8 Na2 P1 88.74(3) . 3_554 ? O5 Na2 P1 120.13(3) 2_554 3_554 ? O2 Na2 P1 126.83(3) . 3_554 ? O3 Na2 P1 93.68(2) . 3_554 ? P1 Na2 P1 118.424(16) . 3_554 ? Na2 Na2 P1 53.383(15) 3_554 3_554 ? O3 Na2 Na1 35.75(2) 3_554 3_554 ? O8 Na2 Na1 146.14(3) . 3_554 ? O5 Na2 Na1 96.71(3) 2_554 3_554 ? O2 Na2 Na1 82.83(3) . 3_554 ? O3 Na2 Na1 101.60(2) . 3_554 ? P1 Na2 Na1 99.701(16) . 3_554 ? Na2 Na2 Na1 66.327(17) 3_554 3_554 ? P1 Na2 Na1 57.408(12) 3_554 3_554 ? O3 Na2 Na1 107.40(3) 3_554 . ? O8 Na2 Na1 42.50(3) . . ? O5 Na2 Na1 133.94(3) 2_554 . ? O2 Na2 Na1 88.72(3) . . ? O3 Na2 Na1 36.30(2) . . ? P1 Na2 Na1 58.640(13) . . ? Na2 Na2 Na1 62.978(16) 3_554 . ? P1 Na2 Na1 91.146(14) 3_554 . ? Na1 Na2 Na1 129.305(15) 3_554 . ? O3 Na2 Na1 141.15(3) 3_554 2_554 ? O8 Na2 Na1 100.25(3) . 2_554 ? O5 Na2 Na1 35.35(3) 2_554 2_554 ? O2 Na2 Na1 66.91(2) . 2_554 ? O3 Na2 Na1 110.94(2) . 2_554 ? P1 Na2 Na1 83.984(15) . 2_554 ? Na2 Na2 Na1 146.95(3) 3_554 2_554 ? P1 Na2 Na1 154.941(17) 3_554 2_554 ? Na1 Na2 Na1 110.749(12) 3_554 2_554 ? Na1 Na2 Na1 111.320(14) . 2_554 ? O3 P1 O2 111.46(5) . . ? O3 P1 O1 112.22(5) . . ? O2 P1 O1 110.06(5) . . ? O3 P1 C1 107.81(6) . . ? O2 P1 C1 108.14(5) . . ? O1 P1 C1 106.95(6) . . ? O3 P1 Na2 64.06(4) . . ? O2 P1 Na2 52.07(4) . . ? O1 P1 Na2 109.54(4) . . ? C1 P1 Na2 142.84(4) . . ? O3 P1 Na2 34.06(3) . 3_554 ? O2 P1 Na2 90.12(4) . 3_554 ? O1 P1 Na2 146.27(4) . 3_554 ? C1 P1 Na2 91.03(5) . 3_554 ? Na2 P1 Na2 61.577(16) . 3_554 ? O3 P1 Na1 33.02(3) . . ? O2 P1 Na1 125.26(4) . . ? O1 P1 Na1 79.22(3) . . ? C1 P1 Na1 120.65(4) . . ? Na2 P1 Na1 73.641(14) . . ? Na2 P1 Na1 67.050(13) 3_554 . ? C11 P2 C21 99.24(6) . . ? C11 P2 C2 104.27(6) . . ? C21 P2 C2 100.09(6) . . ? 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 P1 C1 C2 P2 162.46(7) . . . . ? C16 C11 C12 C13 -1.4(2) . . . . ? P2 C11 C12 C13 -177.89(12) . . . . ? C11 C12 C13 C14 0.1(2) . . . . ? C12 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C11 -0.8(3) . . . . ? C12 C11 C16 C15 1.8(2) . . . . ? P2 C11 C16 C15 178.44(13) . . . . ? C26 C21 C22 C23 -0.5(2) . . . . ? P2 C21 C22 C23 178.69(12) . . . . ? C21 C22 C23 C24 1.3(2) . . . . ? C22 C23 C24 C25 -1.6(3) . . . . ? C23 C24 C25 C26 1.1(3) . . . . ? C22 C21 C26 C25 -0.1(2) . . . . ? P2 C21 C26 C25 -179.26(13) . . . . ? C24 C25 C26 C21 -0.2(3) . . . . ? P1 O3 Na1 O7 82.91(13) . . . 3_544 ? Na2 O3 Na1 O7 -94.43(11) 3_554 . . 3_544 ? Na2 O3 Na1 O7 -9.57(12) . . . 3_544 ? P1 O3 Na1 O7 172.23(6) . . . . ? Na2 O3 Na1 O7 -5.11(5) 3_554 . . . ? Na2 O3 Na1 O7 79.75(4) . . . . ? P1 O3 Na1 O5 -12.63(7) . . . . ? Na2 O3 Na1 O5 170.03(4) 3_554 . . . ? Na2 O3 Na1 O5 -105.11(3) . . . . ? P1 O3 Na1 O6 -107.98(6) . . . . ? Na2 O3 Na1 O6 74.68(5) 3_554 . . . ? Na2 O3 Na1 O6 159.54(3) . . . . ? P1 O3 Na1 O8 91.58(7) . . . . ? Na2 O3 Na1 O8 -85.77(4) 3_554 . . . ? Na2 O3 Na1 O8 -0.91(3) . . . . ? Na2 O3 Na1 P1 -177.34(9) 3_554 . . . ? Na2 O3 Na1 P1 -92.48(7) . . . . ? P1 O3 Na1 Na1 153.06(5) . . . 3_544 ? Na2 O3 Na1 Na1 -24.28(7) 3_554 . . 3_544 ? Na2 O3 Na1 Na1 60.58(5) . . . 3_544 ? P1 O3 Na1 Na2 177.34(9) . . . 3_554 ? Na2 O3 Na1 Na2 84.86(4) . . . 3_554 ? P1 O3 Na1 Na2 92.48(7) . . . . ? Na2 O3 Na1 Na2 -84.86(4) 3_554 . . . ? P1 O3 Na1 Na2 16.67(7) . . . 2_544 ? Na2 O3 Na1 Na2 -160.67(3) 3_554 . . 2_544 ? Na2 O3 Na1 Na2 -75.81(3) . . . 2_544 ? Na1 O7 Na1 O3 -159.37(4) 3_544 . . . ? Na1 O7 Na1 O7 0.0 3_544 . . 3_544 ? Na1 O7 Na1 O5 46.3(2) 3_544 . . . ? Na1 O7 Na1 O6 97.01(4) 3_544 . . . ? Na1 O7 Na1 O8 -82.05(4) 3_544 . . . ? Na1 O7 Na1 P1 -156.27(3) 3_544 . . . ? Na1 O7 Na1 Na2 -162.65(4) 3_544 . . 3_554 ? Na1 O7 Na1 Na2 -117.08(3) 3_544 . . . ? Na1 O7 Na1 Na2 -22.50(6) 3_544 . . 2_544 ? C5 O5 Na1 O3 -100.68(12) . . . . ? Na2 O5 Na1 O3 120.16(4) 2_544 . . . ? C5 O5 Na1 O7 99.67(12) . . . 3_544 ? Na2 O5 Na1 O7 -39.49(5) 2_544 . . 3_544 ? C5 O5 Na1 O7 53.9(2) . . . . ? Na2 O5 Na1 O7 -85.3(2) 2_544 . . . ? C5 O5 Na1 O6 4.40(12) . . . . ? Na2 O5 Na1 O6 -134.76(4) 2_544 . . . ? C5 O5 Na1 O8 -179.52(12) . . . . ? Na2 O5 Na1 O8 41.32(5) 2_544 . . . ? C5 O5 Na1 P1 -105.31(12) . . . . ? Na2 O5 Na1 P1 115.52(4) 2_544 . . . ? C5 O5 Na1 Na1 92.58(12) . . . 3_544 ? Na2 O5 Na1 Na1 -46.58(6) 2_544 . . 3_544 ? C5 O5 Na1 Na2 -93.57(12) . . . 3_554 ? Na2 O5 Na1 Na2 127.27(3) 2_544 . . 3_554 ? C5 O5 Na1 Na2 -143.13(12) . . . . ? Na2 O5 Na1 Na2 77.71(4) 2_544 . . . ? C5 O5 Na1 Na2 139.16(14) . . . 2_544 ? C6 O6 Na1 O3 71.09(15) . . . . ? C6 O6 Na1 O7 -112.72(15) . . . 3_544 ? C6 O6 Na1 O7 166.01(15) . . . . ? C6 O6 Na1 O5 -22.73(15) . . . . ? C6 O6 Na1 O8 168.83(14) . . . . ? C6 O6 Na1 P1 50.19(15) . . . . ? C6 O6 Na1 Na1 -153.18(15) . . . 3_544 ? C6 O6 Na1 Na2 104.70(15) . . . 3_554 ? C6 O6 Na1 Na2 94.88(15) . . . . ? C6 O6 Na1 Na2 -48.00(15) . . . 2_544 ? Na2 O8 Na1 O3 1.07(4) . . . . ? Na2 O8 Na1 O7 178.02(5) . . . 3_544 ? Na2 O8 Na1 O7 -98.37(4) . . . . ? Na2 O8 Na1 O5 90.75(4) . . . . ? Na2 O8 Na1 O6 -101.15(11) . . . . ? Na2 O8 Na1 P1 22.02(3) . . . . ? Na2 O8 Na1 Na1 -139.84(4) . . . 3_544 ? Na2 O8 Na1 Na2 -34.62(4) . . . 3_554 ? Na2 O8 Na1 Na2 111.95(4) . . . 2_544 ? Na1 O8 Na2 O3 93.82(5) . . . 3_554 ? Na1 O8 Na2 O5 -146.44(4) . . . 2_554 ? Na1 O8 Na2 O2 -41.43(6) . . . . ? Na1 O8 Na2 O3 -0.93(3) . . . . ? Na1 O8 Na2 P1 -25.40(4) . . . . ? Na1 O8 Na2 Na2 39.99(4) . . . 3_554 ? Na1 O8 Na2 P1 93.08(3) . . . 3_554 ? Na1 O8 Na2 Na1 93.23(7) . . . 3_554 ? Na1 O8 Na2 Na1 -110.46(3) . . . 2_554 ? P1 O2 Na2 O3 -101.85(5) . . . 3_554 ? P1 O2 Na2 O8 32.95(6) . . . . ? P1 O2 Na2 O5 140.48(5) . . . 2_554 ? P1 O2 Na2 O3 -15.24(3) . . . . ? P1 O2 Na2 Na2 -56.40(4) . . . 3_554 ? P1 O2 Na2 P1 -84.09(5) . . . 3_554 ? P1 O2 Na2 Na1 -123.51(4) . . . 3_554 ? P1 O2 Na2 Na1 6.39(4) . . . . ? P1 O2 Na2 Na1 120.27(4) . . . 2_554 ? P1 O3 Na2 O3 125.56(5) . . . 3_554 ? Na2 O3 Na2 O3 0.0 3_554 . . 3_554 ? Na1 O3 Na2 O3 -108.22(4) . . . 3_554 ? P1 O3 Na2 O8 -125.16(5) . . . . ? Na2 O3 Na2 O8 109.28(4) 3_554 . . . ? Na1 O3 Na2 O8 1.06(4) . . . . ? P1 O3 Na2 O5 -31.99(8) . . . 2_554 ? Na2 O3 Na2 O5 -157.55(6) 3_554 . . 2_554 ? Na1 O3 Na2 O5 94.23(7) . . . 2_554 ? P1 O3 Na2 O2 15.28(3) . . . . ? Na2 O3 Na2 O2 -110.28(4) 3_554 . . . ? Na1 O3 Na2 O2 141.50(4) . . . . ? Na2 O3 Na2 P1 -125.56(5) 3_554 . . . ? Na1 O3 Na2 P1 126.22(5) . . . . ? P1 O3 Na2 Na2 125.56(5) . . . 3_554 ? Na1 O3 Na2 Na2 -108.22(4) . . . 3_554 ? P1 O3 Na2 P1 146.86(3) . . . 3_554 ? Na2 O3 Na2 P1 21.30(2) 3_554 . . 3_554 ? Na1 O3 Na2 P1 -86.92(3) . . . 3_554 ? P1 O3 Na2 Na1 89.39(3) . . . 3_554 ? Na2 O3 Na2 Na1 -36.17(2) 3_554 . . 3_554 ? Na1 O3 Na2 Na1 -144.39(2) . . . 3_554 ? P1 O3 Na2 Na1 -126.22(5) . . . . ? Na2 O3 Na2 Na1 108.22(4) 3_554 . . . ? P1 O3 Na2 Na1 -28.37(4) . . . 2_554 ? Na2 O3 Na2 Na1 -153.93(3) 3_554 . . 2_554 ? Na1 O3 Na2 Na1 97.86(3) . . . 2_554 ? O3 Na1 Na2 O3 80.09(5) . . . 3_554 ? O7 Na1 Na2 O3 -103.64(4) 3_544 . . 3_554 ? O7 Na1 Na2 O3 -22.62(4) . . . 3_554 ? O5 Na1 Na2 O3 160.67(4) . . . 3_554 ? O6 Na1 Na2 O3 45.29(6) . . . 3_554 ? O8 Na1 Na2 O3 -101.45(5) . . . 3_554 ? P1 Na1 Na2 O3 108.48(3) . . . 3_554 ? Na1 Na1 Na2 O3 -60.15(3) 3_544 . . 3_554 ? Na2 Na1 Na2 O3 32.60(3) 3_554 . . 3_554 ? Na2 Na1 Na2 O3 -167.51(3) 2_544 . . 3_554 ? O3 Na1 Na2 O8 -178.46(6) . . . . ? O7 Na1 Na2 O8 -2.19(5) 3_544 . . . ? O7 Na1 Na2 O8 78.83(5) . . . . ? O5 Na1 Na2 O8 -97.89(5) . . . . ? O6 Na1 Na2 O8 146.74(7) . . . . ? P1 Na1 Na2 O8 -150.08(5) . . . . ? Na1 Na1 Na2 O8 41.30(4) 3_544 . . . ? Na2 Na1 Na2 O8 134.04(5) 3_554 . . . ? Na2 Na1 Na2 O8 -66.06(4) 2_544 . . . ? O3 Na1 Na2 O5 -129.58(5) . . . 2_554 ? O7 Na1 Na2 O5 46.70(6) 3_544 . . 2_554 ? O7 Na1 Na2 O5 127.72(5) . . . 2_554 ? O5 Na1 Na2 O5 -49.00(6) . . . 2_554 ? O6 Na1 Na2 O5 -164.38(6) . . . 2_554 ? O8 Na1 Na2 O5 48.89(6) . . . 2_554 ? P1 Na1 Na2 O5 -101.19(4) . . . 2_554 ? Na1 Na1 Na2 O5 90.19(5) 3_544 . . 2_554 ? Na2 Na1 Na2 O5 -177.07(5) 3_554 . . 2_554 ? Na2 Na1 Na2 O5 -17.17(4) 2_544 . . 2_554 ? O3 Na1 Na2 O2 -32.16(4) . . . . ? O7 Na1 Na2 O2 144.12(4) 3_544 . . . ? O7 Na1 Na2 O2 -134.86(3) . . . . ? O5 Na1 Na2 O2 48.42(4) . . . . ? O6 Na1 Na2 O2 -66.96(6) . . . . ? O8 Na1 Na2 O2 146.31(5) . . . . ? P1 Na1 Na2 O2 -3.77(2) . . . . ? Na1 Na1 Na2 O2 -172.39(3) 3_544 . . . ? Na2 Na1 Na2 O2 -79.65(3) 3_554 . . . ? Na2 Na1 Na2 O2 80.25(3) 2_544 . . . ? O7 Na1 Na2 O3 176.27(5) 3_544 . . . ? O7 Na1 Na2 O3 -102.71(4) . . . . ? O5 Na1 Na2 O3 80.58(4) . . . . ? O6 Na1 Na2 O3 -34.80(6) . . . . ? O8 Na1 Na2 O3 178.46(6) . . . . ? P1 Na1 Na2 O3 28.39(3) . . . . ? Na1 Na1 Na2 O3 -140.24(4) 3_544 . . . ? Na2 Na1 Na2 O3 -47.49(3) 3_554 . . . ? Na2 Na1 Na2 O3 112.40(4) 2_544 . . . ? O3 Na1 Na2 P1 -28.39(3) . . . . ? O7 Na1 Na2 P1 147.88(3) 3_544 . . . ? O7 Na1 Na2 P1 -131.10(3) . . . . ? O5 Na1 Na2 P1 52.19(3) . . . . ? O6 Na1 Na2 P1 -63.19(5) . . . . ? O8 Na1 Na2 P1 150.08(5) . . . . ? Na1 Na1 Na2 P1 -168.63(2) 3_544 . . . ? Na2 Na1 Na2 P1 -75.883(18) 3_554 . . . ? Na2 Na1 Na2 P1 84.015(15) 2_544 . . . ? O3 Na1 Na2 Na2 47.49(3) . . . 3_554 ? O7 Na1 Na2 Na2 -136.23(3) 3_544 . . 3_554 ? O7 Na1 Na2 Na2 -55.21(3) . . . 3_554 ? O5 Na1 Na2 Na2 128.07(3) . . . 3_554 ? O6 Na1 Na2 Na2 12.70(5) . . . 3_554 ? O8 Na1 Na2 Na2 -134.04(5) . . . 3_554 ? P1 Na1 Na2 Na2 75.883(18) . . . 3_554 ? Na1 Na1 Na2 Na2 -92.74(2) 3_544 . . 3_554 ? Na2 Na1 Na2 Na2 159.90(2) 2_544 . . 3_554 ? O3 Na1 Na2 P1 94.66(3) . . . 3_554 ? O7 Na1 Na2 P1 -89.07(3) 3_544 . . 3_554 ? O7 Na1 Na2 P1 -8.05(3) . . . 3_554 ? O5 Na1 Na2 P1 175.24(3) . . . 3_554 ? O6 Na1 Na2 P1 59.86(5) . . . 3_554 ? O8 Na1 Na2 P1 -86.88(4) . . . 3_554 ? P1 Na1 Na2 P1 123.048(15) . . . 3_554 ? Na1 Na1 Na2 P1 -45.58(2) 3_544 . . 3_554 ? Na2 Na1 Na2 P1 47.164(14) 3_554 . . 3_554 ? Na2 Na1 Na2 P1 -152.937(16) 2_544 . . 3_554 ? O3 Na1 Na2 Na1 47.49(3) . . . 3_554 ? O7 Na1 Na2 Na1 -136.23(3) 3_544 . . 3_554 ? O7 Na1 Na2 Na1 -55.21(3) . . . 3_554 ? O5 Na1 Na2 Na1 128.07(3) . . . 3_554 ? O6 Na1 Na2 Na1 12.69(5) . . . 3_554 ? O8 Na1 Na2 Na1 -134.04(5) . . . 3_554 ? P1 Na1 Na2 Na1 75.883(18) . . . 3_554 ? Na1 Na1 Na2 Na1 -92.74(2) 3_544 . . 3_554 ? Na2 Na1 Na2 Na1 0.0 3_554 . . 3_554 ? Na2 Na1 Na2 Na1 159.90(2) 2_544 . . 3_554 ? O3 Na1 Na2 Na1 -96.70(4) . . . 2_554 ? O7 Na1 Na2 Na1 79.57(3) 3_544 . . 2_554 ? O7 Na1 Na2 Na1 160.60(3) . . . 2_554 ? O5 Na1 Na2 Na1 -16.12(3) . . . 2_554 ? O6 Na1 Na2 Na1 -131.50(5) . . . 2_554 ? O8 Na1 Na2 Na1 81.77(4) . . . 2_554 ? P1 Na1 Na2 Na1 -68.309(15) . . . 2_554 ? Na1 Na1 Na2 Na1 123.07(2) 3_544 . . 2_554 ? Na2 Na1 Na2 Na1 -144.19(3) 3_554 . . 2_554 ? Na2 Na1 Na2 Na1 15.707(13) 2_544 . . 2_554 ? Na2 O3 P1 O2 54.73(7) 3_554 . . . ? Na1 O3 P1 O2 -122.24(6) . . . . ? Na2 O3 P1 O2 -22.24(5) . . . . ? Na2 O3 P1 O1 178.69(5) 3_554 . . . ? Na1 O3 P1 O1 1.72(8) . . . . ? Na2 O3 P1 O1 101.72(4) . . . . ? Na2 O3 P1 C1 -63.80(7) 3_554 . . . ? Na1 O3 P1 C1 119.24(7) . . . . ? Na2 O3 P1 C1 -140.76(5) . . . . ? Na2 O3 P1 Na2 76.96(5) 3_554 . . . ? Na1 O3 P1 Na2 -100.00(6) . . . . ? Na1 O3 P1 Na2 -176.96(11) . . . 3_554 ? Na2 O3 P1 Na2 -76.96(5) . . . 3_554 ? Na2 O3 P1 Na1 176.96(11) 3_554 . . . ? Na2 O3 P1 Na1 100.00(6) . . . . ? Na2 O2 P1 O3 25.56(6) . . . . ? Na2 O2 P1 O1 -99.61(5) . . . . ? Na2 O2 P1 C1 143.89(5) . . . . ? Na2 O2 P1 Na2 52.77(3) . . . 3_554 ? Na2 O2 P1 Na1 -8.80(5) . . . . ? C2 C1 P1 O3 -67.90(11) . . . . ? C2 C1 P1 O2 171.46(9) . . . . ? C2 C1 P1 O1 52.97(11) . . . . ? C2 C1 P1 Na2 -138.23(8) . . . . ? C2 C1 P1 Na2 -98.07(9) . . . 3_554 ? C2 C1 P1 Na1 -34.35(11) . . . . ? O3 Na2 P1 O3 -62.18(5) 3_554 . . . ? O8 Na2 P1 O3 53.84(5) . . . . ? O5 Na2 P1 O3 160.36(5) 2_554 . . . ? O2 Na2 P1 O3 -153.48(6) . . . . ? Na2 Na2 P1 O3 -38.34(4) 3_554 . . . ? P1 Na2 P1 O3 -38.34(4) 3_554 . . . ? Na1 Na2 P1 O3 -96.42(4) 3_554 . . . ? Na1 Na2 P1 O3 34.01(4) . . . . ? Na1 Na2 P1 O3 153.50(4) 2_554 . . . ? O3 Na2 P1 O2 91.30(5) 3_554 . . . ? O8 Na2 P1 O2 -152.68(5) . . . . ? O5 Na2 P1 O2 -46.16(5) 2_554 . . . ? O3 Na2 P1 O2 153.48(6) . . . . ? Na2 Na2 P1 O2 115.13(5) 3_554 . . . ? P1 Na2 P1 O2 115.13(5) 3_554 . . . ? Na1 Na2 P1 O2 57.06(4) 3_554 . . . ? Na1 Na2 P1 O2 -172.52(5) . . . . ? Na1 Na2 P1 O2 -53.02(4) 2_554 . . . ? O3 Na2 P1 O1 -168.05(4) 3_554 . . . ? O8 Na2 P1 O1 -52.04(5) . . . . ? O5 Na2 P1 O1 54.48(5) 2_554 . . . ? O2 Na2 P1 O1 100.64(6) . . . . ? O3 Na2 P1 O1 -105.88(5) . . . . ? Na2 Na2 P1 O1 -144.22(4) 3_554 . . . ? P1 Na2 P1 O1 -144.22(4) 3_554 . . . ? Na1 Na2 P1 O1 157.71(4) 3_554 . . . ? Na1 Na2 P1 O1 -71.87(4) . . . . ? Na1 Na2 P1 O1 47.62(4) 2_554 . . . ? O3 Na2 P1 C1 23.31(8) 3_554 . . . ? O8 Na2 P1 C1 139.33(8) . . . . ? O5 Na2 P1 C1 -114.15(8) 2_554 . . . ? O2 Na2 P1 C1 -67.99(9) . . . . ? O3 Na2 P1 C1 85.49(8) . . . . ? Na2 Na2 P1 C1 47.14(8) 3_554 . . . ? P1 Na2 P1 C1 47.14(8) 3_554 . . . ? Na1 Na2 P1 C1 -10.93(8) 3_554 . . . ? Na1 Na2 P1 C1 119.49(7) . . . . ? Na1 Na2 P1 C1 -121.01(7) 2_554 . . . ? O3 Na2 P1 Na2 -23.83(2) 3_554 . . 3_554 ? O8 Na2 P1 Na2 92.19(3) . . . 3_554 ? O5 Na2 P1 Na2 -161.30(4) 2_554 . . 3_554 ? O2 Na2 P1 Na2 -115.13(5) . . . 3_554 ? O3 Na2 P1 Na2 38.34(4) . . . 3_554 ? P1 Na2 P1 Na2 0.0 3_554 . . 3_554 ? Na1 Na2 P1 Na2 -58.071(14) 3_554 . . 3_554 ? Na1 Na2 P1 Na2 72.350(16) . . . 3_554 ? Na1 Na2 P1 Na2 -168.15(2) 2_554 . . 3_554 ? O3 Na2 P1 Na1 -96.18(3) 3_554 . . . ? O8 Na2 P1 Na1 19.84(3) . . . . ? O5 Na2 P1 Na1 126.35(3) 2_554 . . . ? O2 Na2 P1 Na1 172.52(5) . . . . ? O3 Na2 P1 Na1 -34.01(4) . . . . ? Na2 Na2 P1 Na1 -72.350(16) 3_554 . . . ? P1 Na2 P1 Na1 -72.349(16) 3_554 . . . ? Na1 Na2 P1 Na1 -130.421(13) 3_554 . . . ? Na1 Na2 P1 Na1 119.496(13) 2_554 . . . ? O7 Na1 P1 O3 -136.87(10) 3_544 . . . ? O7 Na1 P1 O3 -8.73(7) . . . . ? O5 Na1 P1 O3 166.76(7) . . . . ? O6 Na1 P1 O3 78.37(7) . . . . ? O8 Na1 P1 O3 -84.46(7) . . . . ? Na1 Na1 P1 O3 -43.35(8) 3_544 . . . ? Na2 Na1 P1 O3 -1.85(7) 3_554 . . . ? Na2 Na1 P1 O3 -67.36(7) . . . . ? Na2 Na1 P1 O3 -164.15(7) 2_544 . . . ? O3 Na1 P1 O2 74.59(8) . . . . ? O7 Na1 P1 O2 -62.28(8) 3_544 . . . ? O7 Na1 P1 O2 65.86(6) . . . . ? O5 Na1 P1 O2 -118.65(5) . . . . ? O6 Na1 P1 O2 152.96(5) . . . . ? O8 Na1 P1 O2 -9.87(5) . . . . ? Na1 Na1 P1 O2 31.24(7) 3_544 . . . ? Na2 Na1 P1 O2 72.75(5) 3_554 . . . ? Na2 Na1 P1 O2 7.23(4) . . . . ? Na2 Na1 P1 O2 -89.56(5) 2_544 . . . ? O3 Na1 P1 O1 -178.38(8) . . . . ? O7 Na1 P1 O1 44.75(7) 3_544 . . . ? O7 Na1 P1 O1 172.89(5) . . . . ? O5 Na1 P1 O1 -11.62(4) . . . . ? O6 Na1 P1 O1 -100.01(4) . . . . ? O8 Na1 P1 O1 97.16(4) . . . . ? Na1 Na1 P1 O1 138.27(6) 3_544 . . . ? Na2 Na1 P1 O1 179.78(4) 3_554 . . . ? Na2 Na1 P1 O1 114.26(4) . . . . ? Na2 Na1 P1 O1 17.47(4) 2_544 . . . ? O3 Na1 P1 C1 -74.96(8) . . . . ? O7 Na1 P1 C1 148.17(8) 3_544 . . . ? O7 Na1 P1 C1 -83.69(6) . . . . ? O5 Na1 P1 C1 91.80(6) . . . . ? O6 Na1 P1 C1 3.41(6) . . . . ? O8 Na1 P1 C1 -159.42(6) . . . . ? Na1 Na1 P1 C1 -118.31(7) 3_544 . . . ? Na2 Na1 P1 C1 -76.81(5) 3_554 . . . ? Na2 Na1 P1 C1 -142.32(5) . . . . ? Na2 Na1 P1 C1 120.89(5) 2_544 . . . ? O3 Na1 P1 Na2 67.36(7) . . . . ? O7 Na1 P1 Na2 -69.51(6) 3_544 . . . ? O7 Na1 P1 Na2 58.63(3) . . . . ? O5 Na1 P1 Na2 -125.88(3) . . . . ? O6 Na1 P1 Na2 145.73(3) . . . . ? O8 Na1 P1 Na2 -17.10(3) . . . . ? Na1 Na1 P1 Na2 24.02(5) 3_544 . . . ? Na2 Na1 P1 Na2 65.519(17) 3_554 . . . ? Na2 Na1 P1 Na2 -96.784(14) 2_544 . . . ? O3 Na1 P1 Na2 1.85(7) . . . 3_554 ? O7 Na1 P1 Na2 -135.03(6) 3_544 . . 3_554 ? O7 Na1 P1 Na2 -6.88(3) . . . 3_554 ? O5 Na1 P1 Na2 168.60(3) . . . 3_554 ? O6 Na1 P1 Na2 80.22(3) . . . 3_554 ? O8 Na1 P1 Na2 -82.61(3) . . . 3_554 ? Na1 Na1 P1 Na2 -41.50(5) 3_544 . . 3_554 ? Na2 Na1 P1 Na2 -65.519(17) . . . 3_554 ? Na2 Na1 P1 Na2 -162.302(19) 2_544 . . 3_554 ? C12 C11 P2 C21 -129.02(13) . . . . ? C16 C11 P2 C21 54.58(12) . . . . ? C12 C11 P2 C2 -26.04(14) . . . . ? C16 C11 P2 C2 157.55(11) . . . . ? C26 C21 P2 C11 -118.14(12) . . . . ? C22 C21 P2 C11 62.72(13) . . . . ? C26 C21 P2 C2 135.44(12) . . . . ? C22 C21 P2 C2 -43.70(14) . . . . ? C1 C2 P2 C11 88.77(11) . . . . ? C1 C2 P2 C21 -168.91(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5D O1 0.797(18) 1.807(18) 2.6014(13) 175.4(18) . O6 H6D O1 0.789(14) 1.881(14) 2.6661(13) 172.7(19) 4 O7 H7A O2 0.838(17) 1.863(18) 2.6722(12) 161.7(15) 3_554 O7 H7B O1 0.849(17) 2.013(17) 2.8509(13) 169.3(15) 4 O8 H8A O2 0.860(19) 1.839(19) 2.6935(14) 172.6(18) 2_544 O8 H8B O6 0.795(14) 2.174(15) 2.9366(15) 160.9(19) 3_544 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.427 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.049 data_kp140809 _database_code_depnum_ccdc_archive 'CCDC 782187' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H22 Na2 O8 P2' _chemical_formula_weight 426.24 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' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.3578(18) _cell_length_b 8.7338(7) _cell_length_c 12.0390(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.306(10) _cell_angle_gamma 90.00 _cell_volume 1928.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 3067 _cell_measurement_theta_min 2.5773 _cell_measurement_theta_max 32.6449 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9189 _exptl_absorpt_correction_T_max 0.9908 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur Ruby CCD' _diffrn_measurement_method '\o oscillation scan' _diffrn_detector_area_resol_mean 10.4498 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14105 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1141 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.28 _reflns_number_total 14105 _reflns_number_gt 9318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis^Pro^ (Oxford, 2007)' _computing_cell_refinement 'CrysAlis^Pro^ (Oxford, 2007)' _computing_data_reduction 'CrysAlis^Pro^ (Oxford, 2007)' _computing_structure_solution 'SIR-97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0621P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14105 _refine_ls_number_parameters 257 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.992 _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 P1 P 0.61432(4) 0.00446(7) 0.35924(6) 0.01382(16) Uani 1 1 d . . . P2 P 0.79857(4) 0.33470(8) 0.37809(7) 0.01663(17) Uani 1 1 d . . . C1 C 0.69844(16) 0.1011(3) 0.4027(2) 0.0182(7) Uani 1 1 d . . . H1A H 0.6931 0.1432 0.4782 0.022 Uiso 1 1 calc R . . H1B H 0.7385 0.0251 0.4067 0.022 Uiso 1 1 calc R . . C2 C 0.71951(15) 0.2313(3) 0.3248(2) 0.0181(7) Uani 1 1 d . . . H2A H 0.6780 0.3031 0.3152 0.022 Uiso 1 1 calc R . . H2B H 0.7298 0.1884 0.2510 0.022 Uiso 1 1 calc R . . C11 C 0.87889(16) 0.2259(3) 0.3467(2) 0.0194(7) Uani 1 1 d . . . C12 C 0.88938(19) 0.1621(3) 0.2435(3) 0.0265(8) Uani 1 1 d . . . H12 H 0.8523 0.1710 0.1865 0.032 Uiso 1 1 calc R . . C13 C 0.9534(2) 0.0852(3) 0.2223(3) 0.0391(10) Uani 1 1 d . . . H13 H 0.9596 0.0389 0.1519 0.047 Uiso 1 1 calc R . . C14 C 1.0078(2) 0.0766(4) 0.3040(3) 0.0460(11) Uani 1 1 d . . . H14 H 1.0520 0.0251 0.2894 0.055 Uiso 1 1 calc R . . C15 C 0.9990(2) 0.1415(4) 0.4061(3) 0.0490(11) Uani 1 1 d . . . H15 H 1.0371 0.1362 0.4617 0.059 Uiso 1 1 calc R . . C16 C 0.93390(19) 0.2153(3) 0.4280(3) 0.0350(9) Uani 1 1 d . . . H16 H 0.9273 0.2585 0.4993 0.042 Uiso 1 1 calc R . . C21 C 0.80401(15) 0.5080(3) 0.2959(2) 0.0171(6) Uani 1 1 d . . . C22 C 0.78667(17) 0.5132(3) 0.1823(2) 0.0270(8) Uani 1 1 d . . . H22 H 0.7728 0.4224 0.1435 0.032 Uiso 1 1 calc R . . C23 C 0.78976(19) 0.6514(3) 0.1259(2) 0.0336(9) Uani 1 1 d . . . H23 H 0.7767 0.6554 0.0488 0.040 Uiso 1 1 calc R . . C24 C 0.81172(18) 0.7834(3) 0.1812(3) 0.0312(9) Uani 1 1 d . . . H24 H 0.8136 0.8777 0.1422 0.037 Uiso 1 1 calc R . . C25 C 0.83078(18) 0.7777(3) 0.2924(3) 0.0322(9) Uani 1 1 d . . . H25 H 0.8474 0.8675 0.3300 0.039 Uiso 1 1 calc R . . C26 C 0.82574(17) 0.6404(3) 0.3500(2) 0.0268(8) Uani 1 1 d . . . H26 H 0.8374 0.6379 0.4276 0.032 Uiso 1 1 calc R . . O1 O 0.59395(11) -0.10061(18) 0.45265(15) 0.0214(5) Uani 1 1 d . . . O2 O 0.62973(10) -0.08131(18) 0.25178(14) 0.0166(5) Uani 1 1 d . . . O3 O 0.55760(10) 0.12900(18) 0.33518(15) 0.0195(5) Uani 1 1 d . . . O4 O 0.79614(12) 0.3708(2) 0.49899(15) 0.0251(5) Uani 1 1 d . . . O11 O 0.43697(13) -0.2482(2) 0.37083(18) 0.0270(6) Uani 1 1 d . . . H11A H 0.4172(19) -0.301(3) 0.408(3) 0.041 Uiso 1 1 d . . . H11B H 0.4370(17) -0.293(3) 0.301(2) 0.041 Uiso 1 1 d . . . O12 O 0.37608(12) 0.1209(2) 0.23561(19) 0.0239(6) Uani 1 1 d D . . H12A H 0.3746(16) 0.218(3) 0.241(2) 0.036 Uiso 1 1 d . . . H12B H 0.3369(11) 0.091(3) 0.226(3) 0.036 Uiso 1 1 d D . . O13 O 0.50178(12) -0.1006(2) 0.10953(17) 0.0210(6) Uani 1 1 d . . . H13A H 0.5320(17) -0.091(3) 0.161(2) 0.031 Uiso 1 1 d . . . H13B H 0.4812(17) -0.179(3) 0.120(2) 0.031 Uiso 1 1 d . . . O14 O 0.34307(12) -0.0133(2) -0.04253(15) 0.0250(5) Uani 1 1 d D . . H14A H 0.3401(19) 0.017(3) -0.1007(16) 0.038 Uiso 1 1 d D . . Na11 Na 0.44697(6) 0.01494(11) 0.38184(9) 0.0226(3) Uani 1 1 d . . . Na12 Na 0.43864(6) 0.13512(10) 0.06196(9) 0.0208(3) 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 P1 0.0149(4) 0.0121(3) 0.0145(4) -0.0005(3) 0.0027(4) -0.0022(3) P2 0.0137(4) 0.0172(3) 0.0191(4) 0.0013(3) 0.0025(4) -0.0016(3) C1 0.0172(18) 0.0194(14) 0.0177(18) 0.0064(12) -0.0035(13) -0.0019(13) C2 0.0116(17) 0.0241(15) 0.0184(17) 0.0011(12) -0.0002(14) -0.0026(13) C11 0.0163(18) 0.0175(14) 0.0250(19) 0.0026(13) 0.0073(15) -0.0002(13) C12 0.030(2) 0.0239(16) 0.026(2) -0.0003(14) 0.0042(16) 0.0024(16) C13 0.050(3) 0.0279(18) 0.040(3) 0.0005(16) 0.021(2) 0.0071(18) C14 0.032(3) 0.043(2) 0.064(3) 0.013(2) 0.024(2) 0.0150(19) C15 0.024(2) 0.068(3) 0.055(3) 0.013(2) -0.002(2) 0.015(2) C16 0.028(2) 0.044(2) 0.033(2) -0.0041(16) 0.0048(18) 0.0057(17) C21 0.0096(16) 0.0180(13) 0.0241(17) 0.0023(12) 0.0052(13) -0.0008(14) C22 0.031(2) 0.0227(15) 0.027(2) 0.0006(14) -0.0007(16) -0.0108(15) C23 0.046(3) 0.0324(18) 0.0220(19) 0.0074(14) -0.0045(17) -0.0031(17) C24 0.034(2) 0.0207(16) 0.039(2) 0.0111(15) 0.0088(18) 0.0002(15) C25 0.044(3) 0.0139(15) 0.039(2) -0.0032(14) 0.0091(19) -0.0065(16) C26 0.032(2) 0.0248(16) 0.0240(19) -0.0036(13) 0.0063(16) 0.0021(16) O1 0.0283(14) 0.0179(10) 0.0184(12) -0.0010(8) 0.0062(10) -0.0046(9) O2 0.0189(13) 0.0160(9) 0.0154(11) -0.0004(8) 0.0060(9) -0.0019(9) O3 0.0164(12) 0.0157(10) 0.0267(13) -0.0015(8) 0.0032(10) 0.0017(9) O4 0.0244(14) 0.0286(11) 0.0223(13) 0.0002(9) 0.0009(10) -0.0006(11) O11 0.0379(16) 0.0232(12) 0.0203(14) -0.0004(9) 0.0044(12) -0.0060(11) O12 0.0249(15) 0.0143(10) 0.0326(14) -0.0018(9) 0.0036(12) -0.0012(11) O13 0.0231(14) 0.0162(10) 0.0233(14) 0.0038(10) -0.0012(10) -0.0058(10) O14 0.0259(14) 0.0341(12) 0.0149(13) 0.0031(10) -0.0007(11) -0.0032(11) Na11 0.0233(7) 0.0211(6) 0.0238(7) -0.0013(5) 0.0062(5) -0.0034(5) Na12 0.0269(8) 0.0148(5) 0.0208(7) 0.0004(5) 0.0035(6) 0.0017(5) _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 P1 O1 1.5102(18) . ? P1 O3 1.5254(19) . ? P1 O2 1.5311(17) . ? P1 C1 1.818(3) . ? P1 Na11 3.0964(14) . ? P1 Na11 3.3605(13) 3_656 ? P2 O4 1.4916(19) . ? P2 C2 1.805(3) . ? P2 C11 1.807(3) . ? P2 C21 1.814(3) . ? C1 C2 1.533(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C11 C16 1.381(4) . ? C11 C12 1.382(4) . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C15 1.369(5) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.378(4) . ? C21 C22 1.392(4) . ? C22 C23 1.387(4) . ? C22 H22 0.9500 . ? C23 C24 1.383(4) . ? C23 H23 0.9500 . ? C24 C25 1.371(4) . ? C24 H24 0.9500 . ? C25 C26 1.390(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? O1 Na11 2.284(2) 3_656 ? O1 Na12 2.3890(19) 2_645 ? O1 Na11 2.973(2) . ? O3 Na11 2.351(2) . ? O11 Na11 2.309(2) . ? O11 Na12 2.600(3) 2_645 ? O11 H11A 0.75(3) . ? O11 H11B 0.93(3) . ? O12 Na11 2.338(3) . ? O12 Na12 2.429(3) . ? O12 H12A 0.85(3) . ? O12 H12B 0.768(17) . ? O13 Na12 2.394(2) 3_655 ? O13 Na12 2.420(2) . ? O13 H13A 0.82(3) . ? O13 H13B 0.79(3) . ? O14 Na12 2.483(2) . ? O14 H14A 0.747(16) . ? Na11 O1 2.284(2) 3_656 ? Na11 P1 3.3605(13) 3_656 ? Na11 Na11 3.392(2) 3_656 ? Na11 Na12 3.7541(14) 4_566 ? Na11 Na12 3.9696(15) 2_645 ? Na11 Na12 3.9885(16) . ? Na12 O1 2.3890(19) 2_655 ? Na12 O13 2.394(2) 3_655 ? Na12 O11 2.600(3) 2_655 ? Na12 Na12 3.625(2) 3_655 ? Na12 Na11 3.7542(14) 4_565 ? Na12 Na11 3.9695(15) 2_655 ? Na12 H12A 2.60(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 P1 O3 112.78(11) . . ? O1 P1 O2 113.06(10) . . ? O3 P1 O2 109.65(11) . . ? O1 P1 C1 107.52(12) . . ? O3 P1 C1 106.79(11) . . ? O2 P1 C1 106.64(12) . . ? O1 P1 Na11 71.11(8) . . ? O3 P1 Na11 47.44(7) . . ? O2 P1 Na11 107.84(8) . . ? C1 P1 Na11 142.68(10) . . ? O1 P1 Na11 34.56(7) . 3_656 ? O3 P1 Na11 87.75(8) . 3_656 ? O2 P1 Na11 147.06(7) . 3_656 ? C1 P1 Na11 93.96(9) . 3_656 ? Na11 P1 Na11 63.23(4) . 3_656 ? O4 P2 C2 113.39(12) . . ? O4 P2 C11 111.84(13) . . ? C2 P2 C11 108.29(13) . . ? O4 P2 C21 111.15(12) . . ? C2 P2 C21 106.54(13) . . ? C11 P2 C21 105.15(13) . . ? C2 C1 P1 113.65(18) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 P2 111.91(18) . . ? C1 C2 H2A 109.2 . . ? P2 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? P2 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C16 C11 C12 119.1(3) . . ? C16 C11 P2 117.8(2) . . ? C12 C11 P2 123.0(3) . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 119.4(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.7(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.3(3) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C26 C21 C22 119.2(3) . . ? C26 C21 P2 117.6(2) . . ? C22 C21 P2 123.2(2) . . ? C23 C22 C21 119.8(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 119.9(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.8(3) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? P1 O1 Na11 123.41(10) . 3_656 ? P1 O1 Na12 126.94(10) . 2_645 ? Na11 O1 Na12 106.90(8) 3_656 2_645 ? P1 O1 Na11 80.17(8) . . ? Na11 O1 Na11 79.19(7) 3_656 . ? Na12 O1 Na11 94.89(7) 2_645 . ? P1 O3 Na11 104.01(9) . . ? Na11 O11 Na12 107.78(9) . 2_645 ? Na11 O11 H11A 128(2) . . ? Na12 O11 H11A 91(3) 2_645 . ? Na11 O11 H11B 117.8(18) . . ? Na12 O11 H11B 95.0(19) 2_645 . ? H11A O11 H11B 108(3) . . ? Na11 O12 Na12 113.60(10) . . ? Na11 O12 H12A 110.6(19) . . ? Na12 O12 H12A 92.1(19) . . ? Na11 O12 H12B 118(2) . . ? Na12 O12 H12B 111(2) . . ? H12A O12 H12B 108(3) . . ? Na12 O13 Na12 97.71(8) 3_655 . ? Na12 O13 H13A 110(2) 3_655 . ? Na12 O13 H13A 113(2) . . ? Na12 O13 H13B 106(2) 3_655 . ? Na12 O13 H13B 123(2) . . ? H13A O13 H13B 106(3) . . ? Na12 O14 H14A 108(3) . . ? O1 Na11 O11 110.37(8) 3_656 . ? O1 Na11 O12 109.55(9) 3_656 . ? O11 Na11 O12 108.08(9) . . ? O1 Na11 O3 112.79(8) 3_656 . ? O11 Na11 O3 118.40(8) . . ? O12 Na11 O3 96.45(8) . . ? O1 Na11 O1 100.81(7) 3_656 . ? O11 Na11 O1 75.39(7) . . ? O12 Na11 O1 145.24(8) . . ? O3 Na11 O1 55.22(6) . . ? O1 Na11 P1 116.66(7) 3_656 . ? O11 Na11 P1 92.43(7) . . ? O12 Na11 P1 118.02(7) . . ? O3 Na11 P1 28.55(4) . . ? O1 Na11 P1 28.72(4) . . ? O1 Na11 P1 22.03(4) 3_656 3_656 ? O11 Na11 P1 88.53(6) . 3_656 ? O12 Na11 P1 121.43(7) . 3_656 ? O3 Na11 P1 124.60(6) . 3_656 ? O1 Na11 P1 92.91(5) . 3_656 ? P1 Na11 P1 116.77(4) . 3_656 ? O1 Na11 Na11 59.42(6) 3_656 3_656 ? O11 Na11 Na11 90.76(7) . 3_656 ? O12 Na11 Na11 160.97(8) . 3_656 ? O3 Na11 Na11 76.16(6) . 3_656 ? O1 Na11 Na11 41.39(4) . 3_656 ? P1 Na11 Na11 62.19(4) . 3_656 ? P1 Na11 Na11 54.58(3) 3_656 3_656 ? O1 Na11 Na12 37.51(5) 3_656 4_566 ? O11 Na11 Na12 146.99(7) . 4_566 ? O12 Na11 Na12 94.49(6) . 4_566 ? O3 Na11 Na12 81.30(5) . 4_566 ? O1 Na11 Na12 99.69(5) . 4_566 ? P1 Na11 Na12 97.96(4) . 4_566 ? P1 Na11 Na12 58.82(3) 3_656 4_566 ? Na11 Na11 Na12 67.27(4) 3_656 4_566 ? O1 Na11 Na12 108.39(6) 3_656 2_645 ? O11 Na11 Na12 38.58(6) . 2_645 ? O12 Na11 Na12 137.21(6) . 2_645 ? O3 Na11 Na12 86.48(5) . 2_645 ? O1 Na11 Na12 36.84(4) . 2_645 ? P1 Na11 Na12 58.02(3) . 2_645 ? P1 Na11 Na12 89.68(3) 3_656 2_645 ? Na11 Na11 Na12 60.72(3) 3_656 2_645 ? Na12 Na11 Na12 127.99(3) 4_566 2_645 ? O1 Na11 Na12 139.03(6) 3_656 . ? O11 Na11 Na12 101.92(6) . . ? O12 Na11 Na12 33.92(6) . . ? O3 Na11 Na12 69.98(5) . . ? O1 Na11 Na12 111.42(5) . . ? P1 Na11 Na12 85.56(3) . . ? P1 Na11 Na12 155.18(4) 3_656 . ? Na11 Na11 Na12 145.94(5) 3_656 . ? Na12 Na11 Na12 110.03(3) 4_566 . ? Na12 Na11 Na12 112.58(3) 2_645 . ? O1 Na12 O13 100.36(7) 2_655 3_655 ? O1 Na12 O13 162.83(9) 2_655 . ? O13 Na12 O13 82.29(8) 3_655 . ? O1 Na12 O12 89.26(7) 2_655 . ? O13 Na12 O12 169.81(8) 3_655 . ? O13 Na12 O12 89.51(8) . . ? O1 Na12 O14 107.30(8) 2_655 . ? O13 Na12 O14 80.53(7) 3_655 . ? O13 Na12 O14 89.87(7) . . ? O12 Na12 O14 93.47(8) . . ? O1 Na12 O11 81.86(7) 2_655 2_655 ? O13 Na12 O11 83.78(8) 3_655 2_655 ? O13 Na12 O11 81.57(8) . 2_655 ? O12 Na12 O11 101.07(8) . 2_655 ? O14 Na12 O11 163.00(8) . 2_655 ? O1 Na12 Na12 139.16(7) 2_655 3_655 ? O13 Na12 Na12 41.42(5) 3_655 3_655 ? O13 Na12 Na12 40.87(5) . 3_655 ? O12 Na12 Na12 130.11(7) . 3_655 ? O14 Na12 Na12 83.67(6) . 3_655 ? O11 Na12 Na12 80.24(6) 2_655 3_655 ? O1 Na12 Na11 35.59(5) 2_655 4_565 ? O13 Na12 Na11 64.77(5) 3_655 4_565 ? O13 Na12 Na11 143.04(7) . 4_565 ? O12 Na12 Na11 124.79(6) . 4_565 ? O14 Na12 Na11 100.18(6) . 4_565 ? O11 Na12 Na11 78.76(6) 2_655 4_565 ? Na12 Na12 Na11 104.59(4) 3_655 4_565 ? O1 Na12 Na11 48.27(5) 2_655 2_655 ? O13 Na12 Na11 89.72(6) 3_655 2_655 ? O13 Na12 Na11 115.18(7) . 2_655 ? O12 Na12 Na11 99.28(6) . 2_655 ? O14 Na12 Na11 151.75(6) . 2_655 ? O11 Na12 Na11 33.64(5) 2_655 2_655 ? Na12 Na12 Na11 106.31(5) 3_655 2_655 ? Na11 Na12 Na11 52.01(3) 4_565 2_655 ? O1 Na12 Na11 108.97(5) 2_655 . ? O13 Na12 Na11 142.98(6) 3_655 . ? O13 Na12 Na11 63.14(6) . . ? O12 Na12 Na11 32.49(6) . . ? O14 Na12 Na11 110.53(6) . . ? O11 Na12 Na11 78.67(6) 2_655 . ? Na12 Na12 Na11 103.04(4) 3_655 . ? Na11 Na12 Na11 140.45(3) 4_565 . ? Na11 Na12 Na11 93.20(3) 2_655 . ? O1 Na12 H12A 70.9(6) 2_655 . ? O13 Na12 H12A 171.1(6) 3_655 . ? O13 Na12 H12A 105.6(6) . . ? O12 Na12 H12A 19.1(6) . . ? O14 Na12 H12A 103.4(6) . . ? O11 Na12 H12A 93.0(6) 2_655 . ? Na12 Na12 H12A 146.2(6) 3_655 . ? Na11 Na12 H12A 106.5(6) 4_565 . ? Na11 Na12 H12A 83.1(6) 2_655 . ? Na11 Na12 H12A 43.4(6) . . ? 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 O1 P1 C1 C2 -170.41(19) . . . . ? O3 P1 C1 C2 -49.1(2) . . . . ? O2 P1 C1 C2 68.1(2) . . . . ? Na11 P1 C1 C2 -88.8(2) . . . . ? Na11 P1 C1 C2 -137.96(19) 3_656 . . . ? P1 C1 C2 P2 174.71(14) . . . . ? O4 P2 C2 C1 -44.6(2) . . . . ? C11 P2 C2 C1 80.1(2) . . . . ? C21 P2 C2 C1 -167.22(19) . . . . ? O4 P2 C11 C16 -12.6(3) . . . . ? C2 P2 C11 C16 -138.2(2) . . . . ? C21 P2 C11 C16 108.2(2) . . . . ? O4 P2 C11 C12 171.7(2) . . . . ? C2 P2 C11 C12 46.0(3) . . . . ? C21 P2 C11 C12 -67.6(3) . . . . ? C16 C11 C12 C13 1.5(4) . . . . ? P2 C11 C12 C13 177.2(2) . . . . ? C11 C12 C13 C14 -2.0(5) . . . . ? C12 C13 C14 C15 0.8(5) . . . . ? C13 C14 C15 C16 0.8(5) . . . . ? C12 C11 C16 C15 0.1(5) . . . . ? P2 C11 C16 C15 -175.8(3) . . . . ? C14 C15 C16 C11 -1.3(5) . . . . ? O4 P2 C21 C26 18.0(3) . . . . ? C2 P2 C21 C26 141.9(2) . . . . ? C11 P2 C21 C26 -103.2(2) . . . . ? O4 P2 C21 C22 -161.3(2) . . . . ? C2 P2 C21 C22 -37.4(3) . . . . ? C11 P2 C21 C22 77.4(3) . . . . ? C26 C21 C22 C23 -1.6(4) . . . . ? P2 C21 C22 C23 177.7(2) . . . . ? C21 C22 C23 C24 1.6(5) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C23 C24 C25 C26 -2.1(5) . . . . ? C22 C21 C26 C25 -0.3(5) . . . . ? P2 C21 C26 C25 -179.7(2) . . . . ? C24 C25 C26 C21 2.2(5) . . . . ? O3 P1 O1 Na11 -46.77(17) . . . 3_656 ? O2 P1 O1 Na11 -171.88(12) . . . 3_656 ? C1 P1 O1 Na11 70.68(16) . . . 3_656 ? Na11 P1 O1 Na11 -69.98(12) . . . 3_656 ? O3 P1 O1 Na12 111.94(14) . . . 2_645 ? O2 P1 O1 Na12 -13.17(19) . . . 2_645 ? C1 P1 O1 Na12 -130.61(15) . . . 2_645 ? Na11 P1 O1 Na12 88.73(13) . . . 2_645 ? Na11 P1 O1 Na12 158.7(2) 3_656 . . 2_645 ? O3 P1 O1 Na11 23.20(10) . . . . ? O2 P1 O1 Na11 -101.91(10) . . . . ? C1 P1 O1 Na11 140.66(10) . . . . ? Na11 P1 O1 Na11 69.98(12) 3_656 . . . ? O1 P1 O3 Na11 -30.41(13) . . . . ? O2 P1 O3 Na11 96.54(11) . . . . ? C1 P1 O3 Na11 -148.29(11) . . . . ? Na11 P1 O3 Na11 -54.84(7) 3_656 . . . ? Na12 O11 Na11 O1 -94.25(10) 2_645 . . 3_656 ? Na12 O11 Na11 O12 145.97(9) 2_645 . . . ? Na12 O11 Na11 O3 37.86(11) 2_645 . . . ? Na12 O11 Na11 O1 2.06(7) 2_645 . . . ? Na12 O11 Na11 P1 25.41(8) 2_645 . . . ? Na12 O11 Na11 P1 -91.33(8) 2_645 . . 3_656 ? Na12 O11 Na11 Na11 -36.79(8) 2_645 . . 3_656 ? Na12 O11 Na11 Na12 -83.23(15) 2_645 . . 4_566 ? Na12 O11 Na11 Na12 111.38(7) 2_645 . . . ? Na12 O12 Na11 O1 155.20(8) . . . 3_656 ? Na12 O12 Na11 O11 -84.50(10) . . . . ? Na12 O12 Na11 O3 38.21(9) . . . . ? Na12 O12 Na11 O1 5.78(17) . . . . ? Na12 O12 Na11 P1 18.45(11) . . . . ? Na12 O12 Na11 P1 175.84(5) . . . 3_656 ? Na12 O12 Na11 Na11 104.0(3) . . . 3_656 ? Na12 O12 Na11 Na12 119.94(8) . . . 4_566 ? Na12 O12 Na11 Na12 -53.58(13) . . . 2_645 ? P1 O3 Na11 O1 104.25(10) . . . 3_656 ? P1 O3 Na11 O11 -26.78(13) . . . . ? P1 O3 Na11 O12 -141.37(10) . . . . ? P1 O3 Na11 O1 16.77(7) . . . . ? P1 O3 Na11 P1 82.94(10) . . . 3_656 ? P1 O3 Na11 Na11 56.46(9) . . . 3_656 ? P1 O3 Na11 Na12 125.05(9) . . . 4_566 ? P1 O3 Na11 Na12 -4.23(8) . . . 2_645 ? P1 O3 Na11 Na12 -119.82(9) . . . . ? P1 O1 Na11 O1 -127.02(10) . . . 3_656 ? Na11 O1 Na11 O1 0.0 3_656 . . 3_656 ? Na12 O1 Na11 O1 106.30(8) 2_645 . . 3_656 ? P1 O1 Na11 O11 124.53(9) . . . . ? Na11 O1 Na11 O11 -108.45(8) 3_656 . . . ? Na12 O1 Na11 O11 -2.15(7) 2_645 . . . ? P1 O1 Na11 O12 23.77(15) . . . . ? Na11 O1 Na11 O12 150.79(13) 3_656 . . . ? Na12 O1 Na11 O12 -102.91(13) 2_645 . . . ? P1 O1 Na11 O3 -16.68(7) . . . . ? Na11 O1 Na11 O3 110.34(8) 3_656 . . . ? Na12 O1 Na11 O3 -143.36(8) 2_645 . . . ? Na11 O1 Na11 P1 127.02(10) 3_656 . . . ? Na12 O1 Na11 P1 -126.68(10) 2_645 . . . ? P1 O1 Na11 P1 -147.75(6) . . . 3_656 ? Na11 O1 Na11 P1 -20.73(4) 3_656 . . 3_656 ? Na12 O1 Na11 P1 85.57(6) 2_645 . . 3_656 ? P1 O1 Na11 Na11 -127.02(10) . . . 3_656 ? Na12 O1 Na11 Na11 106.30(8) 2_645 . . 3_656 ? P1 O1 Na11 Na12 -88.89(7) . . . 4_566 ? Na11 O1 Na11 Na12 38.12(5) 3_656 . . 4_566 ? Na12 O1 Na11 Na12 144.43(5) 2_645 . . 4_566 ? P1 O1 Na11 Na12 126.68(10) . . . 2_645 ? Na11 O1 Na11 Na12 -106.30(8) 3_656 . . 2_645 ? P1 O1 Na11 Na12 27.23(8) . . . . ? Na11 O1 Na11 Na12 154.25(6) 3_656 . . . ? Na12 O1 Na11 Na12 -99.45(6) 2_645 . . . ? O1 P1 Na11 O1 61.35(10) . . . 3_656 ? O3 P1 Na11 O1 -89.10(11) . . . 3_656 ? O2 P1 Na11 O1 170.30(9) . . . 3_656 ? C1 P1 Na11 O1 -33.00(16) . . . 3_656 ? Na11 P1 Na11 O1 24.70(5) 3_656 . . 3_656 ? O1 P1 Na11 O11 -52.93(9) . . . . ? O3 P1 Na11 O11 156.63(11) . . . . ? O2 P1 Na11 O11 56.02(9) . . . . ? C1 P1 Na11 O11 -147.27(15) . . . . ? Na11 P1 Na11 O11 -89.57(7) 3_656 . . . ? O1 P1 Na11 O12 -164.91(10) . . . . ? O3 P1 Na11 O12 44.64(11) . . . . ? O2 P1 Na11 O12 -55.96(10) . . . . ? C1 P1 Na11 O12 100.74(16) . . . . ? Na11 P1 Na11 O12 158.44(9) 3_656 . . . ? O1 P1 Na11 O3 150.45(12) . . . . ? O2 P1 Na11 O3 -100.61(12) . . . . ? C1 P1 Na11 O3 56.10(17) . . . . ? Na11 P1 Na11 O3 113.80(10) 3_656 . . . ? O3 P1 Na11 O1 -150.45(12) . . . . ? O2 P1 Na11 O1 108.95(10) . . . . ? C1 P1 Na11 O1 -94.35(16) . . . . ? Na11 P1 Na11 O1 -36.65(7) 3_656 . . . ? O1 P1 Na11 P1 36.65(7) . . . 3_656 ? O3 P1 Na11 P1 -113.80(10) . . . 3_656 ? O2 P1 Na11 P1 145.60(8) . . . 3_656 ? C1 P1 Na11 P1 -57.70(15) . . . 3_656 ? Na11 P1 Na11 P1 0.0 3_656 . . 3_656 ? O1 P1 Na11 Na11 36.65(7) . . . 3_656 ? O3 P1 Na11 Na11 -113.80(10) . . . 3_656 ? O2 P1 Na11 Na11 145.60(8) . . . 3_656 ? C1 P1 Na11 Na11 -57.70(15) . . . 3_656 ? O1 P1 Na11 Na12 95.66(8) . . . 4_566 ? O3 P1 Na11 Na12 -54.79(10) . . . 4_566 ? O2 P1 Na11 Na12 -155.40(7) . . . 4_566 ? C1 P1 Na11 Na12 1.31(15) . . . 4_566 ? Na11 P1 Na11 Na12 59.01(3) 3_656 . . 4_566 ? O1 P1 Na11 Na12 -34.54(7) . . . 2_645 ? O3 P1 Na11 Na12 175.02(10) . . . 2_645 ? O2 P1 Na11 Na12 74.41(7) . . . 2_645 ? C1 P1 Na11 Na12 -128.89(15) . . . 2_645 ? Na11 P1 Na11 Na12 -71.19(3) 3_656 . . 2_645 ? O1 P1 Na11 Na12 -154.71(8) . . . . ? O3 P1 Na11 Na12 54.85(9) . . . . ? O2 P1 Na11 Na12 -45.76(8) . . . . ? C1 P1 Na11 Na12 110.95(14) . . . . ? Na11 P1 Na11 Na12 168.65(4) 3_656 . . . ? Na12 O13 Na12 O1 -100.2(3) 3_655 . . 2_655 ? Na12 O13 Na12 O13 0.0 3_655 . . 3_655 ? Na12 O13 Na12 O12 173.92(9) 3_655 . . . ? Na12 O13 Na12 O14 80.46(8) 3_655 . . . ? Na12 O13 Na12 O11 -84.81(8) 3_655 . . 2_655 ? Na12 O13 Na12 Na11 -26.46(13) 3_655 . . 4_565 ? Na12 O13 Na12 Na11 -86.04(7) 3_655 . . 2_655 ? Na12 O13 Na12 Na11 -166.32(9) 3_655 . . . ? Na11 O12 Na12 O1 -128.72(9) . . . 2_655 ? Na11 O12 Na12 O13 70.5(5) . . . 3_655 ? Na11 O12 Na12 O13 34.15(10) . . . . ? Na11 O12 Na12 O14 123.99(9) . . . . ? Na11 O12 Na12 O11 -47.16(10) . . . 2_655 ? Na11 O12 Na12 Na12 39.34(13) . . . 3_655 ? Na11 O12 Na12 Na11 -131.08(8) . . . 4_565 ? Na11 O12 Na12 Na11 -81.30(8) . . . 2_655 ? O1 Na11 Na12 O1 18.51(10) 3_656 . . 2_655 ? O11 Na11 Na12 O1 160.31(9) . . . 2_655 ? O12 Na11 Na12 O1 55.58(11) . . . 2_655 ? O3 Na11 Na12 O1 -83.56(8) . . . 2_655 ? O1 Na11 Na12 O1 -120.89(7) . . . 2_655 ? P1 Na11 Na12 O1 -108.14(7) . . . 2_655 ? P1 Na11 Na12 O1 47.11(11) 3_656 . . 2_655 ? Na11 Na11 Na12 O1 -90.03(11) 3_656 . . 2_655 ? Na12 Na11 Na12 O1 -11.28(9) 4_566 . . 2_655 ? Na12 Na11 Na12 O1 -160.72(7) 2_645 . . 2_655 ? O1 Na11 Na12 O13 159.01(12) 3_656 . . 3_655 ? O11 Na11 Na12 O13 -59.19(13) . . . 3_655 ? O12 Na11 Na12 O13 -163.91(14) . . . 3_655 ? O3 Na11 Na12 O13 56.94(11) . . . 3_655 ? O1 Na11 Na12 O13 19.62(12) . . . 3_655 ? P1 Na11 Na12 O13 32.36(11) . . . 3_655 ? P1 Na11 Na12 O13 -172.39(10) 3_656 . . 3_655 ? Na11 Na11 Na12 O13 50.48(14) 3_656 . . 3_655 ? Na12 Na11 Na12 O13 129.23(9) 4_566 . . 3_655 ? Na12 Na11 Na12 O13 -20.22(11) 2_645 . . 3_655 ? O1 Na11 Na12 O13 -178.08(12) 3_656 . . . ? O11 Na11 Na12 O13 -36.28(9) . . . . ? O12 Na11 Na12 O13 -141.01(11) . . . . ? O3 Na11 Na12 O13 79.84(8) . . . . ? O1 Na11 Na12 O13 42.52(7) . . . . ? P1 Na11 Na12 O13 55.27(6) . . . . ? P1 Na11 Na12 O13 -149.48(10) 3_656 . . . ? Na11 Na11 Na12 O13 73.38(10) 3_656 . . . ? Na12 Na11 Na12 O13 152.13(7) 4_566 . . . ? Na12 Na11 Na12 O13 2.69(6) 2_645 . . . ? O1 Na11 Na12 O12 -37.07(13) 3_656 . . . ? O11 Na11 Na12 O12 104.73(11) . . . . ? O3 Na11 Na12 O12 -139.15(10) . . . . ? O1 Na11 Na12 O12 -176.47(11) . . . . ? P1 Na11 Na12 O12 -163.72(10) . . . . ? P1 Na11 Na12 O12 -8.47(11) 3_656 . . . ? Na11 Na11 Na12 O12 -145.61(13) 3_656 . . . ? Na12 Na11 Na12 O12 -66.86(10) 4_566 . . . ? Na12 Na11 Na12 O12 143.70(10) 2_645 . . . ? O1 Na11 Na12 O14 -99.17(11) 3_656 . . . ? O11 Na11 Na12 O14 42.63(9) . . . . ? O12 Na11 Na12 O14 -62.10(11) . . . . ? O3 Na11 Na12 O14 158.75(8) . . . . ? O1 Na11 Na12 O14 121.43(7) . . . . ? P1 Na11 Na12 O14 134.18(7) . . . . ? P1 Na11 Na12 O14 -70.58(11) 3_656 . . . ? Na11 Na11 Na12 O14 152.29(9) 3_656 . . . ? Na12 Na11 Na12 O14 -128.96(6) 4_566 . . . ? Na12 Na11 Na12 O14 81.60(6) 2_645 . . . ? O1 Na11 Na12 O11 95.71(11) 3_656 . . 2_655 ? O11 Na11 Na12 O11 -122.49(7) . . . 2_655 ? O12 Na11 Na12 O11 132.78(11) . . . 2_655 ? O3 Na11 Na12 O11 -6.36(6) . . . 2_655 ? O1 Na11 Na12 O11 -43.68(7) . . . 2_655 ? P1 Na11 Na12 O11 -30.94(5) . . . 2_655 ? P1 Na11 Na12 O11 124.31(9) 3_656 . . 2_655 ? Na11 Na11 Na12 O11 -12.83(10) 3_656 . . 2_655 ? Na12 Na11 Na12 O11 65.92(6) 4_566 . . 2_655 ? Na12 Na11 Na12 O11 -83.52(6) 2_645 . . 2_655 ? O1 Na11 Na12 Na12 172.78(10) 3_656 . . 3_655 ? O11 Na11 Na12 Na12 -45.42(8) . . . 3_655 ? O12 Na11 Na12 Na12 -150.15(10) . . . 3_655 ? O3 Na11 Na12 Na12 70.71(6) . . . 3_655 ? O1 Na11 Na12 Na12 33.38(6) . . . 3_655 ? P1 Na11 Na12 Na12 46.13(4) . . . 3_655 ? P1 Na11 Na12 Na12 -158.62(8) 3_656 . . 3_655 ? Na11 Na11 Na12 Na12 64.24(10) 3_656 . . 3_655 ? Na12 Na11 Na12 Na12 142.99(3) 4_566 . . 3_655 ? Na12 Na11 Na12 Na12 -6.45(5) 2_645 . . 3_655 ? O1 Na11 Na12 Na11 39.42(15) 3_656 . . 4_565 ? O11 Na11 Na12 Na11 -178.78(8) . . . 4_565 ? O12 Na11 Na12 Na11 76.49(11) . . . 4_565 ? O3 Na11 Na12 Na11 -62.66(9) . . . 4_565 ? O1 Na11 Na12 Na11 -99.98(8) . . . 4_565 ? P1 Na11 Na12 Na11 -87.24(7) . . . 4_565 ? P1 Na11 Na12 Na11 68.01(13) 3_656 . . 4_565 ? Na11 Na11 Na12 Na11 -69.12(12) 3_656 . . 4_565 ? Na12 Na11 Na12 Na11 9.63(10) 4_566 . . 4_565 ? Na12 Na11 Na12 Na11 -139.81(7) 2_645 . . 4_565 ? O1 Na11 Na12 Na11 65.22(9) 3_656 . . 2_655 ? O11 Na11 Na12 Na11 -152.98(8) . . . 2_655 ? O12 Na11 Na12 Na11 102.29(9) . . . 2_655 ? O3 Na11 Na12 Na11 -36.86(5) . . . 2_655 ? O1 Na11 Na12 Na11 -74.18(5) . . . 2_655 ? P1 Na11 Na12 Na11 -61.44(4) . . . 2_655 ? P1 Na11 Na12 Na11 93.81(8) 3_656 . . 2_655 ? Na11 Na11 Na12 Na11 -43.32(9) 3_656 . . 2_655 ? Na12 Na11 Na12 Na11 35.43(4) 4_566 . . 2_655 ? Na12 Na11 Na12 Na11 -114.02(5) 2_645 . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11A O14 0.75(3) 2.21(3) 2.923(3) 159(3) 4_556 O11 H11B O3 0.93(3) 1.78(3) 2.707(3) 176(3) 2_645 O12 H12A O2 0.85(3) 1.76(3) 2.608(3) 178(3) 2_655 O13 H13A O2 0.82(3) 2.07(3) 2.856(3) 162(3) . O13 H13B O3 0.79(3) 1.91(3) 2.696(3) 171(3) 2_645 O14 H14A O2 0.747(16) 2.00(2) 2.717(2) 160(4) 3_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.874 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.107