Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Petr Hermann' _publ_contact_author_address ; Inorganic Chemistry Universita Karlova Hlavova 2030 Prague 2 128 40 CZECH REPUBLIC ; _publ_contact_author_email PETRH@NATUR.CUNI.CZ _publ_section_title ; Thermodynamic study of lanthanide(III) complexes with bifunctional monophosphinic acid analogues of H4dota and comparative kinetic study of yttrium(III) complexes with H4dota-like ligands ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of Gottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; loop_ _publ_author_name 'Petr Hermann' 'Michaela Forsterova' 'Jan Kotek' 'Premysl Lubal' 'Ivan Lukes' 'Ivona Svobodova' ; P.Taborsky ; data_misa-sq _database_code_depnum_ccdc_archive 'CCDC 621031' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H65 N8 Na O20 P2, (H2 O)11.5' ; _chemical_formula_sum 'C36 H88 N8 Na O31.50 P2' _chemical_formula_weight 1222.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.7688(3) _cell_length_b 16.5518(2) _cell_length_c 25.3298(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.5023(8) _cell_angle_gamma 90.00 _cell_volume 11966.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13352 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5224 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25835 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.10 _reflns_number_total 13163 _reflns_number_gt 10506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.353 -0.082 0.468 75.3 11.5 2 0.353 0.082 0.968 75.3 11.3 3 0.647 -0.082 0.032 75.3 12.2 4 0.647 0.082 0.532 75.2 11.8 5 0.500 0.156 0.750 121.3 14.9 6 0.000 0.344 0.250 121.2 15.0 7 0.147 0.418 0.032 75.3 12.2 8 0.853 0.418 0.468 75.3 11.5 9 0.147 0.582 0.532 75.2 11.8 10 0.853 0.582 0.968 75.3 11.3 11 0.000 0.656 0.750 121.2 14.9 12 0.500 0.844 0.250 121.1 15.0 _platon_squeeze_details ; ? ; _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^)+(0.1741P)^2^+37.4445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13163 _refine_ls_number_parameters 727 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.2806 _refine_ls_wR_factor_gt 0.2672 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.047 _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 Na1 Na 0.12631(5) 0.05074(9) 0.60983(6) 0.0388(3) Uani 1 1 d . . . N1A N 0.03690(9) 0.30610(15) 0.61161(11) 0.0273(5) Uani 1 1 d . . . H1A H 0.0501 0.2600 0.6002 0.035 Uiso 1 1 d R . . C2A C 0.06861(11) 0.37894(18) 0.61582(14) 0.0306(6) Uani 1 1 d . . . H2A1 H 0.0517 0.4271 0.6209 0.037 Uiso 1 1 calc R . . H2A2 H 0.0954 0.3730 0.6480 0.037 Uiso 1 1 calc R . . C3A C 0.08558(11) 0.38950(18) 0.56562(14) 0.0303(6) Uani 1 1 d . . . H3A1 H 0.0590 0.4012 0.5341 0.036 Uiso 1 1 calc R . . H3A2 H 0.1067 0.4353 0.5712 0.036 Uiso 1 1 calc R . . N4A N 0.10998(9) 0.31702(15) 0.55378(11) 0.0276(5) Uani 1 1 d . . . C5A C 0.11369(12) 0.3197(2) 0.49705(14) 0.0332(7) Uani 1 1 d . . . H5A1 H 0.1399 0.2865 0.4946 0.040 Uiso 1 1 calc R . . H5A2 H 0.1199 0.3748 0.4880 0.040 Uiso 1 1 calc R . . C6A C 0.06935(12) 0.28986(19) 0.45568(14) 0.0325(7) Uani 1 1 d . . . H6A1 H 0.0431 0.3222 0.4590 0.039 Uiso 1 1 calc R . . H6A2 H 0.0722 0.2974 0.4188 0.039 Uiso 1 1 calc R . . N7A N 0.05939(9) 0.20216(16) 0.46356(11) 0.0301(6) Uani 1 1 d . . . H7A H 0.0622 0.1960 0.4994 0.039 Uiso 1 1 d R . . C8A C 0.00955(12) 0.1805(2) 0.43353(14) 0.0335(7) Uani 1 1 d . . . H8A1 H 0.0066 0.1221 0.4309 0.040 Uiso 1 1 calc R . . H8A2 H 0.0019 0.2020 0.3964 0.040 Uiso 1 1 calc R . . C9A C -0.02490(11) 0.2130(2) 0.46200(14) 0.0332(7) Uani 1 1 d . . . H9A1 H -0.0271 0.2712 0.4575 0.040 Uiso 1 1 calc R . . H9A2 H -0.0556 0.1902 0.4449 0.040 Uiso 1 1 calc R . . N10A N -0.01074(9) 0.19329(16) 0.52095(11) 0.0284(5) Uani 1 1 d . . . C11A C -0.03617(11) 0.2437(2) 0.55077(14) 0.0320(7) Uani 1 1 d . . . H11A H -0.0399 0.2142 0.5823 0.038 Uiso 1 1 calc R . . H11X H -0.0671 0.2561 0.5268 0.038 Uiso 1 1 calc R . . C12 C -0.00992(11) 0.32124(19) 0.56993(14) 0.0313(7) Uani 1 1 d . . . H12A H -0.0287 0.3557 0.5862 0.038 Uiso 1 1 calc R . . H12X H -0.0050 0.3494 0.5384 0.038 Uiso 1 1 calc R . . C20A C 0.03022(11) 0.2850(2) 0.66629(14) 0.0349(7) Uani 1 1 d . . . H20A H 0.0085 0.2401 0.6613 0.042 Uiso 1 1 calc R . . H20X H 0.0159 0.3308 0.6792 0.042 Uiso 1 1 calc R . . P1A P 0.08423(3) 0.25751(5) 0.72039(3) 0.0299(2) Uani 1 1 d . . . O11A O 0.12208(8) 0.23860(16) 0.69358(11) 0.0397(6) Uani 1 1 d . . . O12A O 0.09456(9) 0.32453(16) 0.76232(12) 0.0446(6) Uani 1 1 d . . . C21A C 0.06698(12) 0.1691(2) 0.75079(14) 0.0354(7) Uani 1 1 d . . . H21A H 0.0430 0.1837 0.7682 0.043 Uiso 1 1 calc R . . H21X H 0.0536 0.1300 0.7222 0.043 Uiso 1 1 calc R . . C22A C 0.10831(13) 0.1311(2) 0.79337(16) 0.0419(8) Uani 1 1 d . . . H22A H 0.1231 0.0919 0.7752 0.050 Uiso 1 1 calc R . . H22X H 0.1312 0.1728 0.8088 0.050 Uiso 1 1 calc R . . C23A C 0.09451(14) 0.0899(2) 0.83939(15) 0.0402(8) Uani 1 1 d . . . O23A O 0.12257(11) 0.02763(18) 0.85896(12) 0.0511(7) Uani 1 1 d . . . H23A H 0.1126 0.0154 0.8913 0.066 Uiso 1 1 d R . . O23X O 0.06285(14) 0.1110(2) 0.85681(15) 0.0674(10) Uani 1 1 d . . . C30A C 0.15681(10) 0.31161(19) 0.59278(14) 0.0306(7) Uani 1 1 d . . . H30A H 0.1550 0.3265 0.6291 0.037 Uiso 1 1 calc R . . H30X H 0.1773 0.3501 0.5822 0.037 Uiso 1 1 calc R . . C31A C 0.17807(11) 0.22804(19) 0.59544(14) 0.0308(6) Uani 1 1 d . . . O31A O 0.15624(9) 0.16812(16) 0.57529(13) 0.0507(7) Uani 1 1 d . . . O31X O 0.22175(8) 0.22749(15) 0.62512(11) 0.0370(5) Uani 1 1 d . . . H31X H 0.2302 0.1893 0.6312 0.048 Uiso 1 1 d R . . C40A C 0.09242(12) 0.1467(2) 0.44635(14) 0.0345(7) Uani 1 1 d . . . H40A H 0.1230 0.1722 0.4540 0.041 Uiso 1 1 calc R . . H40X H 0.0810 0.1371 0.4070 0.041 Uiso 1 1 calc R . . C41A C 0.09707(11) 0.06674(19) 0.47671(12) 0.0286(6) Uani 1 1 d . . . O41A O 0.08012(7) 0.05907(14) 0.51528(9) 0.0301(5) Uani 1 1 d . . . O41X O 0.12088(9) 0.01418(14) 0.45944(10) 0.0358(5) Uani 1 1 d . . . C50A C -0.01641(11) 0.10744(19) 0.53167(13) 0.0302(6) Uani 1 1 d . . . H50A H -0.0098 0.0753 0.5027 0.036 Uiso 1 1 calc R . . H50X H -0.0486 0.0973 0.5313 0.036 Uiso 1 1 calc R . . C51A C 0.01603(10) 0.08234(19) 0.58659(13) 0.0279(6) Uani 1 1 d . . . O51A O 0.04711(8) 0.12414(14) 0.61451(9) 0.0325(5) Uani 1 1 d . . . O51X O 0.00685(8) 0.00845(14) 0.59947(10) 0.0344(5) Uani 1 1 d . . . H51X H 0.0223 0.0021 0.6347 0.045 Uiso 1 1 d R . . N1B N 0.28565(9) -0.08245(16) 0.66673(12) 0.0326(6) Uani 1 1 d . . . H1B H 0.2570 -0.0708 0.6680 0.042 Uiso 1 1 d R . . C2B C 0.31831(11) -0.0459(2) 0.71816(16) 0.0379(8) Uani 1 1 d . . . H2B1 H 0.3489 -0.0709 0.7252 0.045 Uiso 1 1 calc R . . H2B2 H 0.3219 0.0113 0.7121 0.045 Uiso 1 1 calc R . . C3B C 0.30063(12) -0.0567(2) 0.76807(15) 0.0391(8) Uani 1 1 d . . . H3B1 H 0.3021 -0.1135 0.7779 0.047 Uiso 1 1 calc R . . H3B2 H 0.3209 -0.0273 0.7989 0.047 Uiso 1 1 calc R . . N4B N 0.25223(9) -0.02780(17) 0.75812(11) 0.0324(6) Uani 1 1 d . . . C5B C 0.23141(12) -0.0601(2) 0.80009(14) 0.0375(8) Uani 1 1 d . . . H5B1 H 0.2073 -0.0234 0.8043 0.045 Uiso 1 1 calc R . . H5B2 H 0.2554 -0.0630 0.8352 0.045 Uiso 1 1 calc R . . C6B C 0.21016(12) -0.1436(2) 0.78541(14) 0.0379(8) Uani 1 1 d . . . H6B1 H 0.2340 -0.1799 0.7798 0.045 Uiso 1 1 calc R . . H6B2 H 0.1998 -0.1642 0.8159 0.045 Uiso 1 1 calc R . . N7B N 0.16928(9) -0.14230(17) 0.73425(11) 0.0309(6) Uani 1 1 d . . . H7B H 0.1757 -0.1164 0.7058 0.040 Uiso 1 1 d R . . C8B C 0.15822(12) -0.2258(2) 0.71022(15) 0.0350(7) Uani 1 1 d . . . H8B1 H 0.1276 -0.2252 0.6834 0.042 Uiso 1 1 calc R . . H8B2 H 0.1570 -0.2631 0.7393 0.042 Uiso 1 1 calc R . . C9B C 0.19451(12) -0.25529(19) 0.68264(14) 0.0343(7) Uani 1 1 d . . . H9B1 H 0.2238 -0.2658 0.7106 0.041 Uiso 1 1 calc R . . H9B2 H 0.1839 -0.3057 0.6637 0.041 Uiso 1 1 calc R . . N10B N 0.20268(9) -0.19647(16) 0.64326(11) 0.0298(6) Uani 1 1 d . . . C11B C 0.24678(11) -0.2137(2) 0.63026(15) 0.0345(7) Uani 1 1 d . . . H11B H 0.2445 -0.1947 0.5934 0.041 Uiso 1 1 calc R . . H11Y H 0.2518 -0.2717 0.6310 0.041 Uiso 1 1 calc R . . C12B C 0.28798(11) -0.1739(2) 0.67038(16) 0.0359(7) Uani 1 1 d . . . H12B H 0.3166 -0.1922 0.6632 0.043 Uiso 1 1 calc R . . H12Y H 0.2890 -0.1903 0.7075 0.043 Uiso 1 1 calc R . . C20B C 0.29637(13) -0.0535(2) 0.61587(17) 0.0406(8) Uani 1 1 d . A . H20B H 0.2751 -0.0799 0.5844 0.049 Uiso 1 1 calc R . . H20Y H 0.3279 -0.0702 0.6174 0.049 Uiso 1 1 calc R . . P1B P 0.29178(4) 0.05621(7) 0.60479(6) 0.0548(3) Uani 1 1 d D . . O11B O 0.25914(10) 0.08821(16) 0.63609(11) 0.0438(6) Uani 1 1 d . A . O12B O 0.33969(15) 0.0902(2) 0.6183(3) 0.111(2) Uani 1 1 d . A . C21B C 0.2546(4) 0.0525(5) 0.5279(3) 0.040(2) Uani 0.521(12) 1 d PD A 1 H21B H 0.2705 0.0205 0.5066 0.048 Uiso 0.521(12) 1 calc PR A 1 H21Y H 0.2243 0.0279 0.5249 0.048 Uiso 0.521(12) 1 calc PR A 1 C22B C 0.2480(3) 0.1388(4) 0.5062(3) 0.041(2) Uani 0.521(12) 1 d P A 1 H22B H 0.2335 0.1728 0.5279 0.049 Uiso 0.521(12) 1 calc PR A 1 H22Y H 0.2774 0.1627 0.5047 0.049 Uiso 0.521(12) 1 calc PR A 1 C21Y C 0.2811(3) 0.0826(5) 0.5400(4) 0.045(2) Uani 0.479(12) 1 d P A 2 H21C H 0.2865 0.1401 0.5377 0.054 Uiso 0.479(12) 1 calc PR A 2 H21Z H 0.3024 0.0543 0.5237 0.054 Uiso 0.479(12) 1 calc PR A 2 C22Y C 0.2291(4) 0.0622(5) 0.5066(4) 0.040(2) Uani 0.479(12) 1 d PD A 2 H22C H 0.2080 0.0727 0.5288 0.048 Uiso 0.479(12) 1 calc PR A 2 H22Z H 0.2263 0.0059 0.4957 0.048 Uiso 0.479(12) 1 calc PR A 2 C23B C 0.2160(2) 0.1233(6) 0.4502(2) 0.111(3) Uani 1 1 d D . . O23B O 0.21099(17) 0.0826(3) 0.41107(14) 0.0816(12) Uani 1 1 d . A . O23Y O 0.19844(15) 0.1983(4) 0.4451(2) 0.120(2) Uani 1 1 d . A . C30B C 0.25092(11) 0.06032(19) 0.75883(14) 0.0325(7) Uani 1 1 d . . . H30B H 0.2730 0.0812 0.7404 0.039 Uiso 1 1 calc R . . H30Y H 0.2608 0.0788 0.7967 0.039 Uiso 1 1 calc R . . C31B C 0.20265(11) 0.0939(2) 0.73095(14) 0.0311(7) Uani 1 1 d . . . O31B O 0.17031(9) 0.05202(15) 0.70486(13) 0.0466(7) Uani 1 1 d . . . O31Y O 0.20024(8) 0.17163(14) 0.73668(10) 0.0330(5) Uani 1 1 d . . . H31Y H 0.1696 0.1970 0.7197 0.043 Uiso 1 1 d R . . C40B C 0.12646(12) -0.1052(2) 0.74408(14) 0.0343(7) Uani 1 1 d . . . H40B H 0.1356 -0.0618 0.7707 0.041 Uiso 1 1 calc R . . H40Y H 0.1099 -0.1455 0.7591 0.041 Uiso 1 1 calc R . . C41B C 0.09399(11) -0.07187(19) 0.68986(14) 0.0312(7) Uani 1 1 d . . . O41B O 0.10640(8) -0.07700(14) 0.64751(9) 0.0322(5) Uani 1 1 d . . . O41Y O 0.05629(8) -0.04099(16) 0.69458(11) 0.0388(6) Uani 1 1 d . . . C50B C 0.16376(11) -0.19398(19) 0.59274(14) 0.0326(7) Uani 1 1 d . . . H50B H 0.1345 -0.2015 0.6017 0.039 Uiso 1 1 calc R . . H50Y H 0.1671 -0.2378 0.5687 0.039 Uiso 1 1 calc R . . C51B C 0.16252(10) -0.11441(19) 0.56313(13) 0.0281(6) Uani 1 1 d . . . O51B O 0.18320(8) -0.05428(14) 0.58446(10) 0.0361(5) Uani 1 1 d . . . O51Y O 0.13477(9) -0.11785(15) 0.51240(10) 0.0379(6) Uani 1 1 d . . . H51Y H 0.1282 -0.0611 0.4948 0.049 Uiso 1 1 d R . . O1W O 0.0000 -0.1100(3) 0.7500 0.0615(12) Uani 1 2 d S . . O2W O 0.1479(2) 0.2513(2) 0.3512(3) 0.1051(19) Uani 1 1 d . . . O3W O 0.05377(19) 0.2232(3) 0.31874(16) 0.0887(13) Uani 1 1 d . . . O4W O 0.0970(2) 0.6638(5) 0.3697(2) 0.147(3) Uani 1 1 d . . . O5W O 0.0774(3) 0.4809(5) 0.3806(4) 0.160(3) Uani 1 1 d . . . O6W O 0.1680(3) 0.7651(8) 0.4386(4) 0.260(7) Uani 1 1 d . . . O7W O 0.0950(2) 0.4028(3) 0.1522(6) 0.249(7) Uani 1 1 d . . . O8W O 0.0445(2) 0.5341(4) 0.2427(5) 0.196(5) Uani 1 1 d . . . O9W O 0.2311(3) 0.9118(3) 0.4031(2) 0.066(2) Uani 0.50 1 d P . . O10W O 0.0106(4) 0.4639(5) 0.4436(3) 0.091(3) Uani 0.50 1 d P . . O11W O -0.0221(4) 0.4371(5) 0.4591(4) 0.098(3) Uani 0.50 1 d P . . O12W O 0.2470(6) 0.8171(7) 0.4986(4) 0.132(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0401(7) 0.0403(8) 0.0332(7) 0.0034(6) 0.0057(6) 0.0003(6) N1A 0.0216(11) 0.0252(12) 0.0328(13) -0.0007(10) 0.0042(10) 0.0036(9) C2A 0.0281(15) 0.0215(14) 0.0392(17) -0.0023(12) 0.0045(13) 0.0025(11) C3A 0.0296(15) 0.0218(14) 0.0379(16) 0.0002(12) 0.0071(13) 0.0014(11) N4A 0.0238(12) 0.0236(12) 0.0338(13) -0.0023(10) 0.0056(10) -0.0005(9) C5A 0.0350(16) 0.0284(15) 0.0370(17) -0.0002(13) 0.0117(13) -0.0021(13) C6A 0.0389(17) 0.0230(14) 0.0334(16) 0.0026(12) 0.0067(13) 0.0007(12) N7A 0.0338(14) 0.0238(12) 0.0314(13) -0.0005(10) 0.0072(11) 0.0014(10) C8A 0.0361(17) 0.0292(15) 0.0297(15) -0.0016(12) 0.0005(13) -0.0016(13) C9A 0.0281(15) 0.0311(16) 0.0332(16) 0.0024(13) -0.0028(12) 0.0018(12) N10A 0.0238(12) 0.0254(12) 0.0321(13) -0.0004(10) 0.0018(10) 0.0016(10) C11A 0.0203(13) 0.0336(16) 0.0393(17) -0.0002(13) 0.0040(12) 0.0042(12) C12 0.0228(14) 0.0297(15) 0.0364(16) 0.0011(12) 0.0007(12) 0.0076(12) C20A 0.0228(14) 0.0459(19) 0.0357(17) 0.0018(14) 0.0079(12) 0.0041(13) P1A 0.0223(4) 0.0320(4) 0.0327(4) 0.0036(3) 0.0033(3) -0.0005(3) O11A 0.0246(11) 0.0517(15) 0.0428(13) 0.0189(11) 0.0094(10) 0.0081(10) O12A 0.0369(13) 0.0364(13) 0.0505(15) -0.0032(11) -0.0040(11) -0.0038(10) C21A 0.0347(17) 0.0356(17) 0.0356(17) -0.0005(13) 0.0093(14) -0.0073(14) C22A 0.0400(19) 0.046(2) 0.044(2) 0.0134(16) 0.0192(16) 0.0059(15) C23A 0.056(2) 0.0335(17) 0.0365(18) 0.0036(14) 0.0219(16) -0.0022(16) O23A 0.0704(19) 0.0461(15) 0.0436(15) 0.0143(12) 0.0271(14) 0.0111(14) O23X 0.091(3) 0.063(2) 0.067(2) 0.0168(16) 0.054(2) 0.0177(18) C30A 0.0233(14) 0.0280(15) 0.0379(17) -0.0058(12) 0.0046(12) -0.0020(11) C31A 0.0243(14) 0.0305(15) 0.0357(16) -0.0069(13) 0.0054(12) -0.0007(12) O31A 0.0344(13) 0.0325(13) 0.0724(19) -0.0146(13) -0.0053(13) 0.0041(10) O31X 0.0258(11) 0.0320(12) 0.0468(14) -0.0062(10) 0.0000(10) 0.0024(9) C40A 0.0393(17) 0.0299(16) 0.0364(17) -0.0030(13) 0.0140(14) 0.0043(13) C41A 0.0290(15) 0.0284(15) 0.0244(14) -0.0058(11) 0.0012(11) -0.0012(12) O41A 0.0262(10) 0.0326(11) 0.0301(11) -0.0049(9) 0.0055(9) -0.0010(9) O41X 0.0442(13) 0.0310(12) 0.0323(12) -0.0033(9) 0.0110(10) 0.0075(10) C50A 0.0247(14) 0.0266(15) 0.0344(16) 0.0004(12) 0.0005(12) -0.0021(11) C51A 0.0230(13) 0.0272(14) 0.0331(15) -0.0003(12) 0.0073(12) 0.0038(11) O51A 0.0282(11) 0.0302(11) 0.0336(12) -0.0019(9) -0.0001(9) -0.0030(9) O51X 0.0333(12) 0.0290(11) 0.0360(12) 0.0035(9) 0.0017(9) -0.0022(9) N1B 0.0227(12) 0.0281(13) 0.0435(15) -0.0007(11) 0.0038(11) 0.0071(10) C2B 0.0222(14) 0.0326(17) 0.052(2) -0.0074(15) -0.0002(14) 0.0053(12) C3B 0.0278(16) 0.0371(18) 0.0415(19) -0.0054(14) -0.0078(14) 0.0086(13) N4B 0.0264(13) 0.0316(14) 0.0338(14) -0.0042(11) -0.0003(11) 0.0062(10) C5B 0.0353(17) 0.0397(18) 0.0314(16) -0.0023(14) -0.0004(13) 0.0051(14) C6B 0.0345(17) 0.0386(18) 0.0339(17) 0.0043(14) -0.0008(14) 0.0049(14) N7B 0.0279(13) 0.0308(13) 0.0312(13) 0.0036(11) 0.0040(11) 0.0042(10) C8B 0.0307(16) 0.0286(15) 0.0416(18) 0.0024(13) 0.0035(14) 0.0003(12) C9B 0.0327(16) 0.0250(15) 0.0396(18) -0.0004(13) 0.0008(13) 0.0050(12) N10B 0.0236(12) 0.0270(13) 0.0345(14) -0.0022(10) 0.0012(10) 0.0033(10) C11B 0.0274(15) 0.0310(16) 0.0417(18) -0.0051(13) 0.0043(13) 0.0065(12) C12B 0.0255(15) 0.0269(15) 0.050(2) -0.0008(14) 0.0028(14) 0.0078(12) C20B 0.0368(18) 0.0356(18) 0.052(2) -0.0027(15) 0.0171(16) 0.0063(14) P1B 0.0599(7) 0.0379(5) 0.0750(8) 0.0150(5) 0.0329(6) 0.0208(5) O11B 0.0484(15) 0.0358(13) 0.0447(14) 0.0015(11) 0.0095(12) 0.0138(11) O12B 0.076(3) 0.0377(18) 0.247(7) 0.009(3) 0.089(4) -0.0006(17) C21B 0.056(6) 0.026(4) 0.041(4) -0.001(3) 0.018(4) 0.005(4) C22B 0.042(4) 0.034(4) 0.048(4) 0.000(3) 0.016(3) 0.000(3) C21Y 0.037(5) 0.035(4) 0.072(6) 0.004(4) 0.029(4) -0.007(4) C22Y 0.052(6) 0.030(4) 0.046(5) 0.001(3) 0.026(4) -0.006(4) C23B 0.052(3) 0.239(10) 0.045(3) -0.038(4) 0.018(2) 0.034(4) O23B 0.127(4) 0.079(3) 0.0442(18) 0.0089(17) 0.034(2) 0.020(2) O23Y 0.064(2) 0.180(5) 0.134(4) -0.118(4) 0.057(3) -0.055(3) C30B 0.0259(14) 0.0286(15) 0.0374(17) -0.0079(13) -0.0004(13) 0.0021(12) C31B 0.0253(14) 0.0305(15) 0.0357(16) -0.0066(13) 0.0056(12) 0.0013(12) O31B 0.0257(11) 0.0351(13) 0.0687(18) -0.0126(12) -0.0033(11) 0.0008(10) O31Y 0.0251(10) 0.0294(11) 0.0398(12) -0.0047(9) 0.0017(9) 0.0027(9) C40B 0.0310(16) 0.0369(17) 0.0348(17) 0.0060(13) 0.0090(13) 0.0054(13) C41B 0.0277(15) 0.0270(15) 0.0379(17) 0.0024(12) 0.0075(13) -0.0008(12) O41B 0.0311(11) 0.0319(11) 0.0331(11) -0.0006(9) 0.0083(9) 0.0000(9) O41Y 0.0303(12) 0.0458(14) 0.0420(13) 0.0099(11) 0.0131(10) 0.0089(10) C50B 0.0275(15) 0.0271(15) 0.0357(17) -0.0034(12) -0.0030(13) 0.0020(12) C51B 0.0208(13) 0.0290(15) 0.0321(15) -0.0041(12) 0.0038(11) 0.0025(11) O51B 0.0337(12) 0.0333(12) 0.0362(12) -0.0011(10) 0.0018(10) -0.0050(9) O51Y 0.0375(13) 0.0318(12) 0.0344(12) -0.0039(9) -0.0059(10) 0.0046(10) O1W 0.054(3) 0.066(3) 0.076(3) 0.000 0.037(2) 0.000 O2W 0.143(4) 0.0356(18) 0.180(5) 0.003(2) 0.117(4) 0.003(2) O3W 0.122(4) 0.083(3) 0.053(2) -0.0057(19) 0.012(2) 0.011(3) O4W 0.145(5) 0.213(7) 0.124(4) 0.098(4) 0.103(4) 0.115(5) O5W 0.143(6) 0.148(6) 0.217(8) 0.079(6) 0.094(6) 0.059(5) O6W 0.141(6) 0.474(19) 0.161(7) -0.147(10) 0.038(5) 0.118(9) O7W 0.124(5) 0.061(3) 0.55(2) 0.104(7) 0.084(8) 0.051(3) O8W 0.108(5) 0.075(4) 0.375(14) 0.035(6) 0.018(6) -0.027(3) O9W 0.137(6) 0.027(3) 0.049(3) 0.006(2) 0.050(4) 0.035(3) O10W 0.135(8) 0.083(6) 0.066(5) 0.038(4) 0.045(5) 0.081(6) O11W 0.150(9) 0.073(5) 0.072(5) 0.029(4) 0.031(6) 0.074(6) O12W 0.254(16) 0.088(7) 0.083(6) 0.000(5) 0.095(9) 0.008(8) _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 Na1 O31B 2.391(3) . ? Na1 O41A 2.403(3) . ? Na1 O31A 2.403(3) . ? Na1 O41B 2.461(3) . ? Na1 O51B 2.631(3) . ? Na1 O51A 2.685(3) . ? N1A C20A 1.495(4) . ? N1A C12 1.511(4) . ? N1A C2A 1.516(4) . ? N1A H1A 0.9405 . ? C2A C3A 1.506(5) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A N4A 1.477(4) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? N4A C30A 1.465(4) . ? N4A C5A 1.473(4) . ? C5A C6A 1.516(5) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A N7A 1.506(4) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? N7A C40A 1.497(4) . ? N7A C8A 1.506(4) . ? N7A H7A 0.8944 . ? C8A C9A 1.510(5) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A N10A 1.468(4) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? N10A C50A 1.465(4) . ? N10A C11A 1.471(4) . ? C11A C12 1.509(5) . ? C11A H11A 0.9700 . ? C11A H11X 0.9700 . ? C12 H12A 0.9700 . ? C12 H12X 0.9700 . ? C20A P1A 1.849(3) . ? C20A H20A 0.9700 . ? C20A H20X 0.9700 . ? P1A O11A 1.505(3) . ? P1A O12A 1.506(3) . ? P1A C21A 1.795(3) . ? C21A C22A 1.523(5) . ? C21A H21A 0.9700 . ? C21A H21X 0.9700 . ? C22A C23A 1.505(5) . ? C22A H22A 0.9700 . ? C22A H22X 0.9700 . ? C23A O23X 1.201(5) . ? C23A O23A 1.330(5) . ? O23A H23A 0.9697 . ? C30A C31A 1.515(4) . ? C30A H30A 0.9700 . ? C30A H30X 0.9700 . ? C31A O31A 1.216(4) . ? C31A O31X 1.304(4) . ? O31X H31X 0.6825 . ? C40A C41A 1.518(5) . ? C40A H40A 0.9700 . ? C40A H40X 0.9700 . ? C41A O41A 1.227(4) . ? C41A O41X 1.275(4) . ? C50A C51A 1.509(4) . ? C50A H50A 0.9700 . ? C50A H50X 0.9700 . ? C51A O51A 1.209(4) . ? C51A O51X 1.314(4) . ? O51X H51X 0.8861 . ? N1B C20B 1.491(5) . ? N1B C2B 1.513(4) . ? N1B C12B 1.516(4) . ? N1B H1B 0.8846 . ? C2B C3B 1.512(6) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B N4B 1.470(4) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? N4B C30B 1.459(4) . ? N4B C5B 1.475(5) . ? C5B C6B 1.521(5) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? C6B N7B 1.505(4) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? N7B C40B 1.498(4) . ? N7B C8B 1.508(4) . ? N7B H7B 0.9040 . ? C8B C9B 1.524(5) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B N10B 1.463(4) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? N10B C50B 1.462(4) . ? N10B C11B 1.469(4) . ? C11B C12B 1.505(5) . ? C11B H11B 0.9700 . ? C11B H11Y 0.9700 . ? C12B H12B 0.9700 . ? C12B H12Y 0.9700 . ? C20B P1B 1.837(4) . ? C20B H20B 0.9700 . ? C20B H20Y 0.9700 . ? P1B O12B 1.480(4) . ? P1B O11B 1.514(3) . ? P1B C21Y 1.640(9) . ? P1B C21B 1.949(9) . ? C21B C22B 1.523(10) . ? C21B H21B 0.9700 . ? C21B H21Y 0.9700 . ? C22B C23B 1.489(9) . ? C22B H22B 0.9700 . ? C22B H22Y 0.9700 . ? C21Y C22Y 1.575(14) . ? C21Y H21C 0.9700 . ? C21Y H21Z 0.9700 . ? C22Y C23B 1.703(11) . ? C22Y H22C 0.9700 . ? C22Y H22Z 0.9700 . ? C23B O23B 1.172(8) . ? C23B O23Y 1.339(11) . ? C30B C31B 1.515(4) . ? C30B H30B 0.9700 . ? C30B H30Y 0.9700 . ? C31B O31B 1.217(4) . ? C31B O31Y 1.299(4) . ? O31Y H31Y 0.9849 . ? C40B C41B 1.540(4) . ? C40B H40B 0.9700 . ? C40B H40Y 0.9700 . ? C41B O41B 1.233(4) . ? C41B O41Y 1.269(4) . ? C50B C51B 1.511(5) . ? C50B H50B 0.9700 . ? C50B H50Y 0.9700 . ? C51B O51B 1.214(4) . ? C51B O51Y 1.317(4) . ? O51Y H51Y 1.0348 . ? O10W O11W 1.229(14) . ? 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 O31B Na1 O41A 175.86(11) . . ? O31B Na1 O31A 101.87(11) . . ? O41A Na1 O31A 75.94(9) . . ? O31B Na1 O41B 74.97(9) . . ? O41A Na1 O41B 107.65(9) . . ? O31A Na1 O41B 172.25(11) . . ? O31B Na1 O51B 92.59(9) . . ? O41A Na1 O51B 91.16(9) . . ? O31A Na1 O51B 96.56(10) . . ? O41B Na1 O51B 76.68(9) . . ? O31B Na1 O51A 100.86(9) . . ? O41A Na1 O51A 75.94(8) . . ? O31A Na1 O51A 94.09(9) . . ? O41B Na1 O51A 93.46(9) . . ? O51B Na1 O51A 160.76(9) . . ? C20A N1A C12 110.3(2) . . ? C20A N1A C2A 111.4(3) . . ? C12 N1A C2A 110.5(2) . . ? C20A N1A H1A 105.7 . . ? C12 N1A H1A 107.6 . . ? C2A N1A H1A 111.2 . . ? C3A C2A N1A 112.6(3) . . ? C3A C2A H2A1 109.1 . . ? N1A C2A H2A1 109.1 . . ? C3A C2A H2A2 109.1 . . ? N1A C2A H2A2 109.1 . . ? H2A1 C2A H2A2 107.8 . . ? N4A C3A C2A 112.3(3) . . ? N4A C3A H3A1 109.1 . . ? C2A C3A H3A1 109.1 . . ? N4A C3A H3A2 109.1 . . ? C2A C3A H3A2 109.1 . . ? H3A1 C3A H3A2 107.9 . . ? C30A N4A C5A 109.8(3) . . ? C30A N4A C3A 110.0(2) . . ? C5A N4A C3A 110.6(2) . . ? N4A C5A C6A 111.9(3) . . ? N4A C5A H5A1 109.2 . . ? C6A C5A H5A1 109.2 . . ? N4A C5A H5A2 109.2 . . ? C6A C5A H5A2 109.2 . . ? H5A1 C5A H5A2 107.9 . . ? N7A C6A C5A 112.8(3) . . ? N7A C6A H6A1 109.0 . . ? C5A C6A H6A1 109.0 . . ? N7A C6A H6A2 109.0 . . ? C5A C6A H6A2 109.0 . . ? H6A1 C6A H6A2 107.8 . . ? C40A N7A C8A 110.0(3) . . ? C40A N7A C6A 112.4(3) . . ? C8A N7A C6A 111.5(2) . . ? C40A N7A H7A 110.2 . . ? C8A N7A H7A 106.3 . . ? C6A N7A H7A 106.2 . . ? N7A C8A C9A 112.3(3) . . ? N7A C8A H8A1 109.1 . . ? C9A C8A H8A1 109.1 . . ? N7A C8A H8A2 109.1 . . ? C9A C8A H8A2 109.1 . . ? H8A1 C8A H8A2 107.9 . . ? N10A C9A C8A 111.7(3) . . ? N10A C9A H9A1 109.3 . . ? C8A C9A H9A1 109.3 . . ? N10A C9A H9A2 109.3 . . ? C8A C9A H9A2 109.3 . . ? H9A1 C9A H9A2 108.0 . . ? C50A N10A C9A 112.9(3) . . ? C50A N10A C11A 110.6(3) . . ? C9A N10A C11A 110.8(2) . . ? N10A C11A C12 110.6(3) . . ? N10A C11A H11A 109.5 . . ? C12 C11A H11A 109.5 . . ? N10A C11A H11X 109.5 . . ? C12 C11A H11X 109.5 . . ? H11A C11A H11X 108.1 . . ? C11A C12 N1A 112.0(2) . . ? C11A C12 H12A 109.2 . . ? N1A C12 H12A 109.2 . . ? C11A C12 H12X 109.2 . . ? N1A C12 H12X 109.2 . . ? H12A C12 H12X 107.9 . . ? N1A C20A P1A 115.3(2) . . ? N1A C20A H20A 108.4 . . ? P1A C20A H20A 108.4 . . ? N1A C20A H20X 108.4 . . ? P1A C20A H20X 108.4 . . ? H20A C20A H20X 107.5 . . ? O11A P1A O12A 116.27(16) . . ? O11A P1A C21A 111.50(16) . . ? O12A P1A C21A 108.89(17) . . ? O11A P1A C20A 108.77(15) . . ? O12A P1A C20A 107.55(16) . . ? C21A P1A C20A 102.96(16) . . ? C22A C21A P1A 111.6(2) . . ? C22A C21A H21A 109.3 . . ? P1A C21A H21A 109.3 . . ? C22A C21A H21X 109.3 . . ? P1A C21A H21X 109.3 . . ? H21A C21A H21X 108.0 . . ? C23A C22A C21A 113.1(3) . . ? C23A C22A H22A 109.0 . . ? C21A C22A H22A 109.0 . . ? C23A C22A H22X 109.0 . . ? C21A C22A H22X 109.0 . . ? H22A C22A H22X 107.8 . . ? O23X C23A O23A 124.4(3) . . ? O23X C23A C22A 124.6(4) . . ? O23A C23A C22A 111.0(3) . . ? C23A O23A H23A 99.5 . . ? N4A C30A C31A 113.0(2) . . ? N4A C30A H30A 109.0 . . ? C31A C30A H30A 109.0 . . ? N4A C30A H30X 109.0 . . ? C31A C30A H30X 109.0 . . ? H30A C30A H30X 107.8 . . ? O31A C31A O31X 124.3(3) . . ? O31A C31A C30A 124.0(3) . . ? O31X C31A C30A 111.6(3) . . ? C31A O31A Na1 135.7(3) . . ? C31A O31X H31X 112.5 . . ? N7A C40A C41A 111.1(3) . . ? N7A C40A H40A 109.4 . . ? C41A C40A H40A 109.4 . . ? N7A C40A H40X 109.4 . . ? C41A C40A H40X 109.4 . . ? H40A C40A H40X 108.0 . . ? O41A C41A O41X 126.6(3) . . ? O41A C41A C40A 119.7(3) . . ? O41X C41A C40A 113.6(3) . . ? C41A O41A Na1 123.5(2) . . ? N10A C50A C51A 111.1(2) . . ? N10A C50A H50A 109.4 . . ? C51A C50A H50A 109.4 . . ? N10A C50A H50X 109.4 . . ? C51A C50A H50X 109.4 . . ? H50A C50A H50X 108.0 . . ? O51A C51A O51X 124.4(3) . . ? O51A C51A C50A 124.4(3) . . ? O51X C51A C50A 111.2(3) . . ? C51A O51A Na1 104.5(2) . . ? C51A O51X H51X 106.0 . . ? C20B N1B C2B 111.9(3) . . ? C20B N1B C12B 110.8(3) . . ? C2B N1B C12B 109.9(3) . . ? C20B N1B H1B 114.0 . . ? C2B N1B H1B 105.8 . . ? C12B N1B H1B 104.1 . . ? C3B C2B N1B 112.4(3) . . ? C3B C2B H2B1 109.1 . . ? N1B C2B H2B1 109.1 . . ? C3B C2B H2B2 109.1 . . ? N1B C2B H2B2 109.1 . . ? H2B1 C2B H2B2 107.8 . . ? N4B C3B C2B 112.0(3) . . ? N4B C3B H3B1 109.2 . . ? C2B C3B H3B1 109.2 . . ? N4B C3B H3B2 109.2 . . ? C2B C3B H3B2 109.2 . . ? H3B1 C3B H3B2 107.9 . . ? C30B N4B C3B 110.6(3) . . ? C30B N4B C5B 109.6(3) . . ? C3B N4B C5B 110.5(3) . . ? N4B C5B C6B 112.6(3) . . ? N4B C5B H5B1 109.1 . . ? C6B C5B H5B1 109.1 . . ? N4B C5B H5B2 109.1 . . ? C6B C5B H5B2 109.1 . . ? H5B1 C5B H5B2 107.8 . . ? N7B C6B C5B 112.1(3) . . ? N7B C6B H6B1 109.2 . . ? C5B C6B H6B1 109.2 . . ? N7B C6B H6B2 109.2 . . ? C5B C6B H6B2 109.2 . . ? H6B1 C6B H6B2 107.9 . . ? C40B N7B C6B 112.4(3) . . ? C40B N7B C8B 110.1(3) . . ? C6B N7B C8B 111.4(3) . . ? C40B N7B H7B 108.6 . . ? C6B N7B H7B 113.1 . . ? C8B N7B H7B 100.6 . . ? N7B C8B C9B 112.2(3) . . ? N7B C8B H8B1 109.2 . . ? C9B C8B H8B1 109.2 . . ? N7B C8B H8B2 109.2 . . ? C9B C8B H8B2 109.2 . . ? H8B1 C8B H8B2 107.9 . . ? N10B C9B C8B 112.1(3) . . ? N10B C9B H9B1 109.2 . . ? C8B C9B H9B1 109.2 . . ? N10B C9B H9B2 109.2 . . ? C8B C9B H9B2 109.2 . . ? H9B1 C9B H9B2 107.9 . . ? C50B N10B C9B 111.8(3) . . ? C50B N10B C11B 110.2(3) . . ? C9B N10B C11B 110.8(3) . . ? N10B C11B C12B 111.8(3) . . ? N10B C11B H11B 109.2 . . ? C12B C11B H11B 109.2 . . ? N10B C11B H11Y 109.2 . . ? C12B C11B H11Y 109.2 . . ? H11B C11B H11Y 107.9 . . ? C11B C12B N1B 112.5(3) . . ? C11B C12B H12B 109.1 . . ? N1B C12B H12B 109.1 . . ? C11B C12B H12Y 109.1 . . ? N1B C12B H12Y 109.1 . . ? H12B C12B H12Y 107.8 . . ? N1B C20B P1B 115.1(2) . . ? N1B C20B H20B 108.5 . . ? P1B C20B H20B 108.5 . . ? N1B C20B H20Y 108.5 . . ? P1B C20B H20Y 108.5 . . ? H20B C20B H20Y 107.5 . . ? O12B P1B O11B 117.8(3) . . ? O12B P1B C21Y 91.8(4) . . ? O11B P1B C21Y 117.4(3) . . ? O12B P1B C20B 108.4(2) . . ? O11B P1B C20B 107.27(17) . . ? C21Y P1B C20B 113.6(4) . . ? O12B P1B C21B 118.7(4) . . ? O11B P1B C21B 105.5(3) . . ? C21Y P1B C21B 27.7(4) . . ? C20B P1B C21B 96.8(3) . . ? C22B C21B P1B 108.0(5) . . ? C22B C21B H21B 110.1 . . ? P1B C21B H21B 110.1 . . ? C22B C21B H21Y 110.1 . . ? P1B C21B H21Y 110.1 . . ? H21B C21B H21Y 108.4 . . ? C23B C22B C21B 99.4(7) . . ? C23B C22B H22B 111.9 . . ? C21B C22B H22B 111.9 . . ? C23B C22B H22Y 111.9 . . ? C21B C22B H22Y 111.9 . . ? H22B C22B H22Y 109.6 . . ? C22Y C21Y P1B 111.2(6) . . ? C22Y C21Y H21C 109.4 . . ? P1B C21Y H21C 109.4 . . ? C22Y C21Y H21Z 109.4 . . ? P1B C21Y H21Z 109.4 . . ? H21C C21Y H21Z 108.0 . . ? C21Y C22Y C23B 106.2(6) . . ? C21Y C22Y H22C 110.5 . . ? C23B C22Y H22C 110.5 . . ? C21Y C22Y H22Z 110.5 . . ? C23B C22Y H22Z 110.5 . . ? H22C C22Y H22Z 108.7 . . ? O23B C23B O23Y 119.9(6) . . ? O23B C23B C22B 142.9(7) . . ? O23Y C23B C22B 93.4(6) . . ? O23B C23B C22Y 108.2(8) . . ? O23Y C23B C22Y 128.4(5) . . ? C22B C23B C22Y 51.0(5) . . ? N4B C30B C31B 112.7(3) . . ? N4B C30B H30B 109.1 . . ? C31B C30B H30B 109.1 . . ? N4B C30B H30Y 109.1 . . ? C31B C30B H30Y 109.1 . . ? H30B C30B H30Y 107.8 . . ? O31B C31B O31Y 124.3(3) . . ? O31B C31B C30B 122.9(3) . . ? O31Y C31B C30B 112.7(3) . . ? C31B O31B Na1 132.4(3) . . ? C31B O31Y H31Y 116.5 . . ? N7B C40B C41B 110.3(3) . . ? N7B C40B H40B 109.6 . . ? C41B C40B H40B 109.6 . . ? N7B C40B H40Y 109.6 . . ? C41B C40B H40Y 109.6 . . ? H40B C40B H40Y 108.1 . . ? O41B C41B O41Y 127.0(3) . . ? O41B C41B C40B 118.9(3) . . ? O41Y C41B C40B 114.1(3) . . ? C41B O41B Na1 116.3(2) . . ? N10B C50B C51B 111.1(3) . . ? N10B C50B H50B 109.4 . . ? C51B C50B H50B 109.4 . . ? N10B C50B H50Y 109.4 . . ? C51B C50B H50Y 109.4 . . ? H50B C50B H50Y 108.0 . . ? O51B C51B O51Y 124.6(3) . . ? O51B C51B C50B 123.8(3) . . ? O51Y C51B C50B 111.5(3) . . ? C51B O51B Na1 111.7(2) . . ? C51B O51Y H51Y 111.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.504 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.104 #===END data_tyc-sqeeze _database_code_depnum_ccdc_archive 'CCDC 621032' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H66 N8 Na O20 P2, Cl, (H2 O)10.5' ; _chemical_formula_sum 'C36 H87 Cl N8 Na O30.50 P2' _chemical_formula_weight 1240.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9291(4) _cell_length_b 16.0112(4) _cell_length_c 17.2340(6) _cell_angle_alpha 96.1631(19) _cell_angle_beta 91.9137(13) _cell_angle_gamma 108.6265(18) _cell_volume 3093.22(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8466 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 22.99 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1322 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16506 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 23.03 _reflns_number_total 8608 _reflns_number_gt 6437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.031 0.000 0.500 487.4 70.4 2 0.208 0.453 0.684 16.9 2.1 3 0.791 0.546 0.316 16.9 2.1 _platon_squeeze_details ; ? ; _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^)+(0.0890P)^2^+1.6393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8608 _refine_ls_number_parameters 678 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1467 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _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 Na1 Na 0.22082(12) 0.22469(8) 0.12542(8) 0.0299(3) Uani 1 1 d . . . Cl1 Cl 0.39430(11) 0.32159(9) 0.61012(7) 0.0637(4) Uani 1 1 d . . . N1A N 0.3972(2) 0.23499(16) -0.14164(15) 0.0213(6) Uani 1 1 d . . . H1A H 0.3489 0.2358 -0.1020 0.028 Uiso 1 1 calc R . . C2A C 0.4459(3) 0.3288(2) -0.1635(2) 0.0248(8) Uani 1 1 d . . . H2A H 0.5070 0.3649 -0.1241 0.030 Uiso 1 1 calc R . . H2X H 0.4819 0.3270 -0.2131 0.030 Uiso 1 1 calc R . . C3A C 0.3502(3) 0.3705(2) -0.17024(19) 0.0252(8) Uani 1 1 d . . . H3A H 0.3860 0.4322 -0.1782 0.030 Uiso 1 1 calc R . . H3X H 0.2969 0.3405 -0.2158 0.030 Uiso 1 1 calc R . . N4A N 0.2809(2) 0.36594(17) -0.10022(15) 0.0235(6) Uani 1 1 d . . . C5A C 0.1677(3) 0.3803(2) -0.1190(2) 0.0280(8) Uani 1 1 d . . . H5A H 0.1801 0.4238 -0.1557 0.034 Uiso 1 1 calc R . . H5X H 0.1411 0.4043 -0.0717 0.034 Uiso 1 1 calc R . . C6A C 0.0725(3) 0.2960(2) -0.1540(2) 0.0275(8) Uani 1 1 d . . . H6A H 0.1004 0.2705 -0.2000 0.033 Uiso 1 1 calc R . . H6X H 0.0027 0.3100 -0.1705 0.033 Uiso 1 1 calc R . . N7A N 0.0388(2) 0.22833(18) -0.09682(16) 0.0264(7) Uani 1 1 d . . . H7A H 0.1070 0.2254 -0.0738 0.034 Uiso 1 1 calc R . . C8A C -0.0285(3) 0.1379(2) -0.1383(2) 0.0311(8) Uani 1 1 d . . . H8A H -0.0908 0.1425 -0.1735 0.037 Uiso 1 1 calc R . . H8X H -0.0658 0.0995 -0.1001 0.037 Uiso 1 1 calc R . . C9A C 0.0501(3) 0.0963(2) -0.1845(2) 0.0290(8) Uani 1 1 d . . . H9A H 0.0053 0.0350 -0.2037 0.035 Uiso 1 1 calc R . . H9X H 0.0747 0.1277 -0.2293 0.035 Uiso 1 1 calc R . . N10A N 0.1553(2) 0.09894(17) -0.13681(16) 0.0253(7) Uani 1 1 d . . . C11A C 0.2471(3) 0.0857(2) -0.1866(2) 0.0278(8) Uani 1 1 d . . . H11A H 0.2098 0.0451 -0.2330 0.033 Uiso 1 1 calc R . . H11X H 0.2960 0.0591 -0.1585 0.033 Uiso 1 1 calc R . . C12A C 0.3240(3) 0.1720(2) -0.21035(19) 0.0254(8) Uani 1 1 d . . . H12A H 0.2741 0.2004 -0.2352 0.031 Uiso 1 1 calc R . . H12X H 0.3767 0.1601 -0.2484 0.031 Uiso 1 1 calc R . . C20A C 0.4943(3) 0.2027(2) -0.1136(2) 0.0267(8) Uani 1 1 d . . . H20A H 0.5434 0.1983 -0.1565 0.032 Uiso 1 1 calc R . . H20X H 0.4589 0.1435 -0.0992 0.032 Uiso 1 1 calc R . . P1A P 0.58967(8) 0.27315(6) -0.02970(5) 0.0257(2) Uani 1 1 d . . . O11A O 0.5142(2) 0.31541(15) 0.01677(13) 0.0295(6) Uani 1 1 d . . . O12A O 0.6981(2) 0.33355(16) -0.06120(14) 0.0327(6) Uani 1 1 d . . . C21A C 0.6353(3) 0.1952(2) 0.0209(2) 0.0308(8) Uani 1 1 d . . . H21A H 0.6462 0.1500 -0.0174 0.037 Uiso 1 1 calc R . . H21X H 0.7112 0.2262 0.0496 0.037 Uiso 1 1 calc R . . C22A C 0.5469(3) 0.1503(2) 0.0777(2) 0.0316(9) Uani 1 1 d . . . H22A H 0.5438 0.1938 0.1206 0.038 Uiso 1 1 calc R . . H22X H 0.4684 0.1251 0.0511 0.038 Uiso 1 1 calc R . . C23A C 0.5835(3) 0.0785(3) 0.1089(2) 0.0359(9) Uani 1 1 d . . . O23A O 0.5577(2) 0.00362(17) 0.06895(16) 0.0425(7) Uani 1 1 d . . . H23A H 0.5209 0.0016 0.0248 0.055 Uiso 1 1 d R . . O23X O 0.6422(3) 0.09299(19) 0.17458(17) 0.0528(8) Uani 1 1 d . . . C30A C 0.3493(3) 0.4311(2) -0.03607(19) 0.0261(8) Uani 1 1 d . . . H30A H 0.3509 0.4899 -0.0462 0.031 Uiso 1 1 calc R . . H30X H 0.4303 0.4304 -0.0336 0.031 Uiso 1 1 calc R . . C31A C 0.2984(3) 0.4130(2) 0.0418(2) 0.0247(8) Uani 1 1 d . . . O31A O 0.2219(2) 0.34448(16) 0.05240(14) 0.0335(6) Uani 1 1 d . . . O31X O 0.3494(2) 0.47879(15) 0.09678(14) 0.0322(6) Uani 1 1 d . . . H31X H 0.3181 0.4728 0.1378 0.042 Uiso 1 1 d R . . C40A C -0.0314(3) 0.2531(2) -0.0337(2) 0.0291(8) Uani 1 1 d . . . H40A H -0.1141 0.2349 -0.0528 0.035 Uiso 1 1 calc R . . H40X H -0.0038 0.3171 -0.0205 0.035 Uiso 1 1 calc R . . C41A C -0.0208(3) 0.2099(2) 0.0394(2) 0.0260(8) Uani 1 1 d . . . O41A O 0.0460(2) 0.16503(15) 0.04115(14) 0.0279(6) Uani 1 1 d . . . O41X O -0.0836(2) 0.22660(16) 0.09303(14) 0.0327(6) Uani 1 1 d . . . C50A C 0.1265(3) 0.0335(2) -0.0804(2) 0.0308(8) Uani 1 1 d . . . H50A H 0.1269 -0.0235 -0.1056 0.037 Uiso 1 1 calc R . . H50X H 0.0475 0.0263 -0.0637 0.037 Uiso 1 1 calc R . . C51A C 0.2139(3) 0.0623(2) -0.0103(2) 0.0250(8) Uani 1 1 d . . . O51A O 0.2831(2) 0.13660(15) 0.00688(14) 0.0285(6) Uani 1 1 d . . . O51X O 0.2041(2) -0.00380(16) 0.03206(14) 0.0360(6) Uani 1 1 d . . . H51X H 0.2695 0.0163 0.0860 0.047 Uiso 1 1 d R . . N1B N 0.2338(2) 0.40187(18) 0.38597(16) 0.0255(7) Uani 1 1 d . . . H1B H 0.2376 0.3615 0.3456 0.033 Uiso 1 1 calc R . . C2B C 0.3544(3) 0.4705(2) 0.4038(2) 0.0274(8) Uani 1 1 d . . . H2B H 0.3533 0.5089 0.4511 0.033 Uiso 1 1 calc R . . H2Y H 0.3719 0.5068 0.3614 0.033 Uiso 1 1 calc R . . C3B C 0.4522(3) 0.4302(2) 0.41474(19) 0.0286(8) Uani 1 1 d . . . H3B H 0.5280 0.4774 0.4235 0.034 Uiso 1 1 calc R . . H3Y H 0.4398 0.3994 0.4608 0.034 Uiso 1 1 calc R . . N4B N 0.4560(3) 0.36802(18) 0.34724(16) 0.0267(7) Uani 1 1 d . . . C5B C 0.5243(3) 0.3111(2) 0.3672(2) 0.0331(9) Uani 1 1 d . . . H5B H 0.5901 0.3452 0.4043 0.040 Uiso 1 1 calc R . . H5Y H 0.5567 0.2917 0.3204 0.040 Uiso 1 1 calc R . . C6B C 0.4496(3) 0.2308(2) 0.4020(2) 0.0338(9) Uani 1 1 d . . . H6B H 0.4156 0.2504 0.4481 0.041 Uiso 1 1 calc R . . H6Y H 0.4999 0.1980 0.4185 0.041 Uiso 1 1 calc R . . N7B N 0.3509(3) 0.17001(18) 0.34521(16) 0.0295(7) Uani 1 1 d . . . H7B H 0.3151 0.2044 0.3221 0.038 Uiso 1 1 calc R . . C8B C 0.2589(3) 0.1061(2) 0.3865(2) 0.0344(9) Uani 1 1 d . . . H8B H 0.2978 0.0784 0.4212 0.041 Uiso 1 1 calc R . . H8Y H 0.2074 0.0597 0.3481 0.041 Uiso 1 1 calc R . . C9B C 0.1849(4) 0.1508(2) 0.4332(2) 0.0351(9) Uani 1 1 d . . . H9B H 0.1205 0.1061 0.4531 0.042 Uiso 1 1 calc R . . H9Y H 0.2334 0.1892 0.4776 0.042 Uiso 1 1 calc R . . N10B N 0.1360(3) 0.20345(18) 0.38567(16) 0.0284(7) Uani 1 1 d . . . C11B C 0.0956(3) 0.2673(2) 0.4347(2) 0.0318(9) Uani 1 1 d . . . H11B H 0.0661 0.2424 0.4818 0.038 Uiso 1 1 calc R . . H11Y H 0.0308 0.2781 0.4066 0.038 Uiso 1 1 calc R . . C12B C 0.1947(3) 0.3541(2) 0.45687(19) 0.0281(8) Uani 1 1 d . . . H12B H 0.2617 0.3426 0.4815 0.034 Uiso 1 1 calc R . . H12Y H 0.1681 0.3919 0.4945 0.034 Uiso 1 1 calc R . . C20B C 0.1460(3) 0.4457(2) 0.3623(2) 0.0288(8) Uani 1 1 d . . . H20B H 0.1496 0.4934 0.4031 0.035 Uiso 1 1 calc R . . H20Y H 0.0671 0.4026 0.3598 0.035 Uiso 1 1 calc R . . P1B P 0.16575(8) 0.49178(6) 0.26860(5) 0.0264(3) Uani 1 1 d . . . O11B O 0.2656(2) 0.46951(16) 0.23122(13) 0.0315(6) Uani 1 1 d . . . O12B O 0.1795(2) 0.58900(15) 0.28770(14) 0.0355(6) Uani 1 1 d . . . C21B C 0.0252(3) 0.4364(2) 0.2152(2) 0.0300(8) Uani 1 1 d . . . H21B H 0.0105 0.3728 0.2108 0.036 Uiso 1 1 calc R . . H21Y H -0.0363 0.4490 0.2450 0.036 Uiso 1 1 calc R . . C22B C 0.0151(3) 0.4621(2) 0.1340(2) 0.0288(8) Uani 1 1 d . . . H22B H 0.0367 0.5263 0.1375 0.035 Uiso 1 1 calc R . . H22Y H 0.0711 0.4441 0.1023 0.035 Uiso 1 1 calc R . . C23B C -0.1071(3) 0.4210(2) 0.0942(2) 0.0261(8) Uani 1 1 d . . . O23B O -0.1099(2) 0.42713(16) 0.01823(14) 0.0318(6) Uani 1 1 d . . . H23B H -0.2004 0.3862 -0.0064 0.041 Uiso 1 1 d R . . O23Y O -0.1958(2) 0.38689(16) 0.12726(14) 0.0339(6) Uani 1 1 d . . . C30B C 0.5070(3) 0.4163(2) 0.2821(2) 0.0310(8) Uani 1 1 d . . . H30B H 0.5920 0.4429 0.2934 0.037 Uiso 1 1 calc R . . H30Y H 0.4742 0.4640 0.2781 0.037 Uiso 1 1 calc R . . C31B C 0.4836(3) 0.3586(2) 0.2055(2) 0.0265(8) Uani 1 1 d . . . O31B O 0.4087(2) 0.28521(16) 0.19363(14) 0.0343(6) Uani 1 1 d . . . O31Y O 0.5503(2) 0.39727(15) 0.15277(14) 0.0325(6) Uani 1 1 d . . . H31Y H 0.5364 0.3605 0.1004 0.042 Uiso 1 1 d R . . C40B C 0.3959(4) 0.1202(2) 0.2818(2) 0.0344(9) Uani 1 1 d . . . H40B H 0.4140 0.0716 0.3024 0.041 Uiso 1 1 calc R . . H40Y H 0.4686 0.1596 0.2650 0.041 Uiso 1 1 calc R . . C41B C 0.3059(3) 0.0836(2) 0.2119(2) 0.0298(9) Uani 1 1 d . . . O41B O 0.2199(2) 0.11103(16) 0.20703(14) 0.0328(6) Uani 1 1 d . . . O41Y O 0.3298(2) 0.02775(16) 0.16303(14) 0.0347(6) Uani 1 1 d . . . C50B C 0.0426(3) 0.1493(2) 0.3274(2) 0.0304(8) Uani 1 1 d . . . H50B H -0.0325 0.1328 0.3514 0.036 Uiso 1 1 calc R . . H50Y H 0.0591 0.0952 0.3093 0.036 Uiso 1 1 calc R . . C51B C 0.0325(3) 0.1975(2) 0.2582(2) 0.0281(8) Uani 1 1 d . . . O51B O 0.1112(2) 0.26449(15) 0.24530(14) 0.0307(6) Uani 1 1 d . . . O51Y O -0.0651(2) 0.15936(16) 0.21484(14) 0.0341(6) Uani 1 1 d . . . H51Y H -0.0659 0.1904 0.1633 0.044 Uiso 1 1 d R . . O1W O 0.7156(2) 0.2674(2) 0.23586(17) 0.0510(8) Uani 1 1 d . . . H1W1 H 0.7548 0.3153 0.2013 0.066 Uiso 1 1 d R . . H1W2 H 0.7680 0.2820 0.2849 0.066 Uiso 1 1 d R . . O2W O 0.7872(2) 0.27920(17) -0.19253(15) 0.0398(7) Uani 1 1 d . . . H2W1 H 0.7628 0.3040 -0.1479 0.052 Uiso 1 1 d R . . H2W2 H 0.7972 0.3235 -0.2243 0.052 Uiso 1 1 d R . . O3W O 0.1365(3) 0.2502(3) -0.3444(2) 0.0852(12) Uani 1 1 d . . . H3W1 H 0.0906 0.2799 -0.3526 0.111 Uiso 1 1 d R . . H3W2 H 0.2238 0.2868 -0.3555 0.111 Uiso 1 1 d R . . O4W O 0.6612(4) 0.1103(2) -0.2499(2) 0.0944(14) Uani 1 1 d . . . O5W O 0.0957(5) 0.5070(3) 0.5559(3) 0.1234(19) Uani 1 1 d . . . O6W O -0.1516(3) 0.3227(3) 0.3759(2) 0.0784(11) Uani 1 1 d . . . O7W O 0.0207(5) 0.6470(3) 0.3721(3) 0.1146(17) 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 Na1 0.0275(8) 0.0288(7) 0.0313(8) 0.0071(6) -0.0040(6) 0.0056(6) Cl1 0.0561(8) 0.0846(9) 0.0475(7) 0.0047(6) -0.0014(6) 0.0205(7) N1A 0.0204(15) 0.0206(14) 0.0187(15) -0.0003(11) 0.0018(12) 0.0015(12) C2A 0.0254(19) 0.0213(18) 0.0226(18) 0.0031(14) 0.0026(15) 0.0002(15) C3A 0.030(2) 0.0195(17) 0.0239(19) 0.0065(14) 0.0049(15) 0.0038(15) N4A 0.0234(16) 0.0224(15) 0.0216(15) 0.0001(12) -0.0018(12) 0.0043(12) C5A 0.029(2) 0.0264(19) 0.030(2) 0.0073(15) 0.0040(16) 0.0099(16) C6A 0.027(2) 0.0300(19) 0.0262(19) 0.0093(15) 0.0023(15) 0.0084(16) N7A 0.0210(16) 0.0317(16) 0.0259(16) 0.0052(13) 0.0008(12) 0.0074(13) C8A 0.024(2) 0.0281(19) 0.033(2) 0.0024(16) -0.0033(16) -0.0024(16) C9A 0.027(2) 0.0238(18) 0.029(2) 0.0027(15) -0.0028(16) -0.0009(15) N10A 0.0249(16) 0.0220(15) 0.0254(16) 0.0058(12) -0.0011(13) 0.0020(12) C11A 0.028(2) 0.0236(18) 0.027(2) -0.0021(15) -0.0044(16) 0.0040(15) C12A 0.028(2) 0.0242(18) 0.0191(18) -0.0007(14) -0.0027(15) 0.0034(15) C20A 0.0242(19) 0.0296(19) 0.027(2) 0.0029(15) 0.0017(15) 0.0099(16) P1A 0.0244(5) 0.0260(5) 0.0235(5) 0.0026(4) -0.0014(4) 0.0043(4) O11A 0.0303(14) 0.0314(13) 0.0253(13) 0.0012(10) -0.0008(11) 0.0088(11) O12A 0.0248(14) 0.0370(14) 0.0293(14) 0.0062(11) -0.0018(11) -0.0003(11) C21A 0.028(2) 0.033(2) 0.029(2) -0.0001(16) -0.0019(16) 0.0088(17) C22A 0.030(2) 0.032(2) 0.034(2) 0.0069(16) 0.0010(17) 0.0119(17) C23A 0.030(2) 0.032(2) 0.044(3) 0.0052(19) -0.0022(19) 0.0086(17) O23A 0.0532(18) 0.0347(16) 0.0427(16) 0.0032(13) -0.0018(13) 0.0196(13) O23X 0.063(2) 0.0459(17) 0.0502(19) 0.0065(14) -0.0187(16) 0.0213(15) C30A 0.026(2) 0.0203(18) 0.028(2) 0.0026(15) 0.0043(16) 0.0013(15) C31A 0.0225(19) 0.0198(19) 0.028(2) -0.0007(16) -0.0014(15) 0.0038(16) O31A 0.0353(15) 0.0276(14) 0.0285(14) 0.0044(11) 0.0018(11) -0.0029(12) O31X 0.0340(15) 0.0279(13) 0.0247(13) -0.0004(11) 0.0073(11) -0.0031(11) C40A 0.0218(19) 0.033(2) 0.034(2) 0.0064(16) 0.0060(16) 0.0100(16) C41A 0.0176(18) 0.0250(18) 0.030(2) 0.0028(15) -0.0034(16) 0.0002(16) O41A 0.0224(13) 0.0262(13) 0.0333(14) 0.0028(10) -0.0006(10) 0.0061(11) O41X 0.0305(14) 0.0433(15) 0.0276(14) 0.0038(11) 0.0020(12) 0.0168(12) C50A 0.034(2) 0.0235(19) 0.030(2) 0.0042(16) 0.0008(17) 0.0012(16) C51A 0.0241(19) 0.023(2) 0.0269(19) 0.0049(16) 0.0047(15) 0.0055(17) O51A 0.0253(14) 0.0201(13) 0.0359(15) 0.0011(11) -0.0015(11) 0.0026(11) O51X 0.0402(16) 0.0290(14) 0.0308(14) 0.0100(11) -0.0022(12) -0.0013(12) N1B 0.0294(17) 0.0263(15) 0.0191(15) 0.0014(12) 0.0001(12) 0.0075(13) C2B 0.029(2) 0.0263(19) 0.0232(19) -0.0035(15) -0.0009(15) 0.0059(16) C3B 0.030(2) 0.0307(19) 0.0204(19) 0.0003(15) 0.0003(15) 0.0045(16) N4B 0.0295(17) 0.0288(16) 0.0208(16) 0.0002(12) 0.0020(13) 0.0091(13) C5B 0.032(2) 0.039(2) 0.027(2) -0.0038(17) -0.0028(16) 0.0132(18) C6B 0.040(2) 0.036(2) 0.028(2) -0.0005(16) -0.0066(17) 0.0172(18) N7B 0.0375(18) 0.0290(16) 0.0242(16) 0.0040(13) -0.0035(14) 0.0141(14) C8B 0.042(2) 0.030(2) 0.032(2) 0.0096(17) -0.0036(17) 0.0106(18) C9B 0.044(2) 0.032(2) 0.028(2) 0.0071(17) -0.0004(17) 0.0099(18) N10B 0.0359(18) 0.0279(16) 0.0223(16) 0.0059(13) -0.0004(13) 0.0110(14) C11B 0.032(2) 0.036(2) 0.027(2) 0.0072(17) 0.0025(16) 0.0101(17) C12B 0.034(2) 0.034(2) 0.0167(18) 0.0025(15) 0.0024(15) 0.0123(17) C20B 0.027(2) 0.036(2) 0.027(2) 0.0049(16) 0.0020(16) 0.0146(17) P1B 0.0290(5) 0.0266(5) 0.0226(5) 0.0029(4) -0.0006(4) 0.0081(4) O11B 0.0304(14) 0.0392(14) 0.0238(13) 0.0036(11) 0.0016(11) 0.0101(12) O12B 0.0474(17) 0.0248(13) 0.0313(14) -0.0001(11) -0.0020(12) 0.0091(12) C21B 0.031(2) 0.0281(19) 0.030(2) 0.0070(16) 0.0000(16) 0.0084(16) C22B 0.0219(19) 0.032(2) 0.029(2) 0.0052(16) -0.0029(15) 0.0030(16) C23B 0.029(2) 0.0159(17) 0.033(2) 0.0011(15) -0.0011(17) 0.0083(16) O23B 0.0251(14) 0.0358(14) 0.0268(14) 0.0066(11) -0.0052(11) -0.0010(11) O23Y 0.0268(15) 0.0398(15) 0.0354(15) 0.0079(12) 0.0042(12) 0.0102(12) C30B 0.031(2) 0.030(2) 0.026(2) -0.0011(16) 0.0048(16) 0.0035(16) C31B 0.027(2) 0.025(2) 0.029(2) 0.0043(16) 0.0030(16) 0.0092(17) O31B 0.0370(15) 0.0299(15) 0.0283(14) 0.0006(11) 0.0038(11) 0.0010(13) O31Y 0.0405(15) 0.0267(13) 0.0253(13) 0.0013(11) 0.0090(12) 0.0038(11) C40B 0.043(2) 0.034(2) 0.031(2) -0.0017(17) -0.0018(18) 0.0205(18) C41B 0.041(2) 0.0189(18) 0.028(2) 0.0069(16) 0.0032(17) 0.0059(17) O41B 0.0351(15) 0.0301(14) 0.0353(15) 0.0091(11) 0.0007(12) 0.0121(12) O41Y 0.0431(16) 0.0318(14) 0.0291(14) 0.0016(12) -0.0018(12) 0.0132(12) C50B 0.031(2) 0.0257(19) 0.029(2) 0.0053(16) -0.0012(16) 0.0013(16) C51B 0.032(2) 0.029(2) 0.024(2) -0.0013(16) 0.0028(17) 0.0125(18) O51B 0.0313(15) 0.0249(13) 0.0318(14) 0.0052(11) 0.0007(11) 0.0033(12) O51Y 0.0317(15) 0.0384(15) 0.0265(14) 0.0052(11) -0.0039(12) 0.0034(12) O1W 0.0413(17) 0.067(2) 0.0446(17) 0.0206(15) 0.0069(14) 0.0127(15) O2W 0.0452(17) 0.0362(15) 0.0418(16) 0.0106(12) 0.0080(13) 0.0159(13) O3W 0.081(3) 0.120(3) 0.053(2) 0.036(2) -0.0068(19) 0.024(2) O4W 0.146(4) 0.048(2) 0.080(3) 0.0032(18) -0.046(3) 0.026(2) O5W 0.164(5) 0.132(4) 0.114(4) 0.032(3) 0.063(4) 0.092(4) O6W 0.062(2) 0.112(3) 0.064(2) 0.006(2) -0.0014(18) 0.034(2) O7W 0.141(4) 0.135(4) 0.116(4) 0.038(3) 0.055(3) 0.099(4) _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 Na1 O31B 2.353(3) . ? Na1 O41A 2.366(3) . ? Na1 O31A 2.401(3) . ? Na1 O41B 2.414(3) . ? Na1 O51B 2.611(3) . ? Na1 O51A 2.621(3) . ? Na1 C41A 3.124(4) . ? N1A C20A 1.496(4) . ? N1A C12A 1.514(4) . ? N1A C2A 1.521(4) . ? N1A H1A 0.9100 . ? C2A C3A 1.503(5) . ? C2A H2A 0.9700 . ? C2A H2X 0.9700 . ? C3A N4A 1.480(4) . ? C3A H3A 0.9700 . ? C3A H3X 0.9700 . ? N4A C30A 1.457(4) . ? N4A C5A 1.473(4) . ? C5A C6A 1.509(5) . ? C5A H5A 0.9700 . ? C5A H5X 0.9700 . ? C6A N7A 1.511(4) . ? C6A H6A 0.9700 . ? C6A H6X 0.9700 . ? N7A C40A 1.490(4) . ? N7A C8A 1.499(4) . ? N7A H7A 0.9100 . ? C8A C9A 1.515(5) . ? C8A H8A 0.9700 . ? C8A H8X 0.9700 . ? C9A N10A 1.463(4) . ? C9A H9A 0.9700 . ? C9A H9X 0.9700 . ? N10A C11A 1.467(4) . ? N10A C50A 1.474(4) . ? C11A C12A 1.503(5) . ? C11A H11A 0.9700 . ? C11A H11X 0.9700 . ? C12A H12A 0.9700 . ? C12A H12X 0.9700 . ? C20A P1A 1.837(3) . ? C20A H20A 0.9700 . ? C20A H20X 0.9700 . ? P1A O11A 1.493(2) . ? P1A O12A 1.505(2) . ? P1A C21A 1.802(4) . ? C21A C22A 1.525(5) . ? C21A H21A 0.9700 . ? C21A H21X 0.9700 . ? C22A C23A 1.496(5) . ? C22A H22A 0.9700 . ? C22A H22X 0.9700 . ? C23A O23A 1.256(5) . ? C23A O23X 1.270(5) . ? O23A H23A 0.8577 . ? C30A C31A 1.509(5) . ? C30A H30A 0.9700 . ? C30A H30X 0.9700 . ? C31A O31A 1.218(4) . ? C31A O31X 1.310(4) . ? O31X H31X 0.8114 . ? C40A C41A 1.522(5) . ? C40A H40A 0.9700 . ? C40A H40X 0.9700 . ? C41A O41A 1.234(4) . ? C41A O41X 1.267(4) . ? O41X H51Y 1.4360 . ? C50A C51A 1.500(5) . ? C50A H50A 0.9700 . ? C50A H50X 0.9700 . ? C51A O51A 1.210(4) . ? C51A O51X 1.326(4) . ? O51X H51X 1.1411 . ? N1B C2B 1.503(4) . ? N1B C20B 1.503(4) . ? N1B C12B 1.519(4) . ? N1B H1B 0.9100 . ? C2B C3B 1.518(5) . ? C2B H2B 0.9700 . ? C2B H2Y 0.9700 . ? C3B N4B 1.459(4) . ? C3B H3B 0.9700 . ? C3B H3Y 0.9700 . ? N4B C5B 1.460(5) . ? N4B C30B 1.469(4) . ? C5B C6B 1.509(5) . ? C5B H5B 0.9700 . ? C5B H5Y 0.9700 . ? C6B N7B 1.510(5) . ? C6B H6B 0.9700 . ? C6B H6Y 0.9700 . ? N7B C40B 1.497(5) . ? N7B C8B 1.499(5) . ? N7B H7B 0.9100 . ? C8B C9B 1.505(5) . ? C8B H8B 0.9700 . ? C8B H8Y 0.9700 . ? C9B N10B 1.467(4) . ? C9B H9B 0.9700 . ? C9B H9Y 0.9700 . ? N10B C50B 1.457(5) . ? N10B C11B 1.466(5) . ? C11B C12B 1.510(5) . ? C11B H11B 0.9700 . ? C11B H11Y 0.9700 . ? C12B H12B 0.9700 . ? C12B H12Y 0.9700 . ? C20B P1B 1.837(3) . ? C20B H20B 0.9700 . ? C20B H20Y 0.9700 . ? P1B O11B 1.494(3) . ? P1B O12B 1.510(2) . ? P1B C21B 1.794(4) . ? C21B C22B 1.512(5) . ? C21B H21B 0.9700 . ? C21B H21Y 0.9700 . ? C22B C23B 1.501(5) . ? C22B H22B 0.9700 . ? C22B H22Y 0.9700 . ? C23B O23Y 1.217(4) . ? C23B O23B 1.323(4) . ? O23B H23B 1.1102 . ? C30B C31B 1.492(5) . ? C30B H30B 0.9700 . ? C30B H30Y 0.9700 . ? C31B O31B 1.219(4) . ? C31B O31Y 1.302(4) . ? O31Y H31Y 1.0014 . ? C40B C41B 1.519(5) . ? C40B H40B 0.9700 . ? C40B H40Y 0.9700 . ? C41B O41B 1.242(4) . ? C41B O41Y 1.267(4) . ? O41Y H51X 1.4539 . ? C50B C51B 1.509(5) . ? C50B H50B 0.9700 . ? C50B H50Y 0.9700 . ? C51B O51B 1.226(4) . ? C51B O51Y 1.296(4) . ? O51Y H51Y 1.0634 . ? O1W H1W1 1.0238 . ? O1W H1W2 0.9945 . ? O2W H2W1 0.9250 . ? O2W H2W2 0.9226 . ? O3W H3W1 0.8501 . ? O3W H3W2 1.0538 . ? 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 O31B Na1 O41A 172.18(10) . . ? O31B Na1 O31A 100.04(9) . . ? O41A Na1 O31A 76.44(9) . . ? O31B Na1 O41B 78.32(9) . . ? O41A Na1 O41B 105.63(9) . . ? O31A Na1 O41B 176.01(10) . . ? O31B Na1 O51B 93.13(9) . . ? O41A Na1 O51B 94.32(9) . . ? O31A Na1 O51B 99.10(9) . . ? O41B Na1 O51B 77.42(9) . . ? O31B Na1 O51A 97.53(9) . . ? O41A Na1 O51A 75.84(8) . . ? O31A Na1 O51A 92.83(9) . . ? O41B Na1 O51A 91.00(9) . . ? O51B Na1 O51A 162.37(9) . . ? O31B Na1 C41A 161.25(10) . . ? O41A Na1 C41A 20.61(8) . . ? O31A Na1 C41A 63.98(9) . . ? O41B Na1 C41A 116.94(10) . . ? O51B Na1 C41A 80.59(9) . . ? O51A Na1 C41A 93.22(9) . . ? C20A N1A C12A 110.4(2) . . ? C20A N1A C2A 111.6(3) . . ? C12A N1A C2A 110.5(2) . . ? C20A N1A H1A 108.1 . . ? C12A N1A H1A 108.1 . . ? C2A N1A H1A 108.1 . . ? C3A C2A N1A 111.6(3) . . ? C3A C2A H2A 109.3 . . ? N1A C2A H2A 109.3 . . ? C3A C2A H2X 109.3 . . ? N1A C2A H2X 109.3 . . ? H2A C2A H2X 108.0 . . ? N4A C3A C2A 112.8(3) . . ? N4A C3A H3A 109.0 . . ? C2A C3A H3A 109.0 . . ? N4A C3A H3X 109.0 . . ? C2A C3A H3X 109.0 . . ? H3A C3A H3X 107.8 . . ? C30A N4A C5A 110.8(3) . . ? C30A N4A C3A 110.4(3) . . ? C5A N4A C3A 110.1(3) . . ? N4A C5A C6A 112.4(3) . . ? N4A C5A H5A 109.1 . . ? C6A C5A H5A 109.1 . . ? N4A C5A H5X 109.1 . . ? C6A C5A H5X 109.1 . . ? H5A C5A H5X 107.8 . . ? C5A C6A N7A 112.2(3) . . ? C5A C6A H6A 109.2 . . ? N7A C6A H6A 109.2 . . ? C5A C6A H6X 109.2 . . ? N7A C6A H6X 109.2 . . ? H6A C6A H6X 107.9 . . ? C40A N7A C8A 109.8(3) . . ? C40A N7A C6A 112.6(3) . . ? C8A N7A C6A 111.0(3) . . ? C40A N7A H7A 107.8 . . ? C8A N7A H7A 107.8 . . ? C6A N7A H7A 107.8 . . ? N7A C8A C9A 112.5(3) . . ? N7A C8A H8A 109.1 . . ? C9A C8A H8A 109.1 . . ? N7A C8A H8X 109.1 . . ? C9A C8A H8X 109.1 . . ? H8A C8A H8X 107.8 . . ? N10A C9A C8A 111.7(3) . . ? N10A C9A H9A 109.3 . . ? C8A C9A H9A 109.3 . . ? N10A C9A H9X 109.3 . . ? C8A C9A H9X 109.3 . . ? H9A C9A H9X 107.9 . . ? C9A N10A C11A 110.7(3) . . ? C9A N10A C50A 111.9(3) . . ? C11A N10A C50A 110.7(3) . . ? N10A C11A C12A 111.3(3) . . ? N10A C11A H11A 109.4 . . ? C12A C11A H11A 109.4 . . ? N10A C11A H11X 109.4 . . ? C12A C11A H11X 109.4 . . ? H11A C11A H11X 108.0 . . ? C11A C12A N1A 112.6(3) . . ? C11A C12A H12A 109.1 . . ? N1A C12A H12A 109.1 . . ? C11A C12A H12X 109.1 . . ? N1A C12A H12X 109.1 . . ? H12A C12A H12X 107.8 . . ? N1A C20A P1A 114.8(2) . . ? N1A C20A H20A 108.6 . . ? P1A C20A H20A 108.6 . . ? N1A C20A H20X 108.6 . . ? P1A C20A H20X 108.6 . . ? H20A C20A H20X 107.5 . . ? O11A P1A O12A 117.59(14) . . ? O11A P1A C21A 113.10(15) . . ? O12A P1A C21A 107.60(15) . . ? O11A P1A C20A 106.63(14) . . ? O12A P1A C20A 107.58(15) . . ? C21A P1A C20A 103.25(16) . . ? C22A C21A P1A 113.5(2) . . ? C22A C21A H21A 108.9 . . ? P1A C21A H21A 108.9 . . ? C22A C21A H21X 108.9 . . ? P1A C21A H21X 108.9 . . ? H21A C21A H21X 107.7 . . ? C23A C22A C21A 109.8(3) . . ? C23A C22A H22A 109.7 . . ? C21A C22A H22A 109.7 . . ? C23A C22A H22X 109.7 . . ? C21A C22A H22X 109.7 . . ? H22A C22A H22X 108.2 . . ? O23A C23A O23X 119.7(3) . . ? O23A C23A C22A 119.6(4) . . ? O23X C23A C22A 120.7(3) . . ? C23A O23A H23A 112.3 . . ? N4A C30A C31A 112.3(3) . . ? N4A C30A H30A 109.1 . . ? C31A C30A H30A 109.1 . . ? N4A C30A H30X 109.1 . . ? C31A C30A H30X 109.1 . . ? H30A C30A H30X 107.9 . . ? O31A C31A O31X 124.4(3) . . ? O31A C31A C30A 124.0(3) . . ? O31X C31A C30A 111.6(3) . . ? C31A O31A Na1 133.4(2) . . ? C31A O31X H31X 112.9 . . ? N7A C40A C41A 112.0(3) . . ? N7A C40A H40A 109.2 . . ? C41A C40A H40A 109.2 . . ? N7A C40A H40X 109.2 . . ? C41A C40A H40X 109.2 . . ? H40A C40A H40X 107.9 . . ? O41A C41A O41X 127.7(3) . . ? O41A C41A C40A 118.8(3) . . ? O41X C41A C40A 113.5(3) . . ? O41A C41A Na1 42.46(16) . . ? O41X C41A Na1 105.1(2) . . ? C40A C41A Na1 123.8(2) . . ? C41A O41A Na1 116.9(2) . . ? C41A O41X H51Y 112.5 . . ? N10A C50A C51A 111.2(3) . . ? N10A C50A H50A 109.4 . . ? C51A C50A H50A 109.4 . . ? N10A C50A H50X 109.4 . . ? C51A C50A H50X 109.4 . . ? H50A C50A H50X 108.0 . . ? O51A C51A O51X 123.9(3) . . ? O51A C51A C50A 124.8(3) . . ? O51X C51A C50A 111.3(3) . . ? C51A O51A Na1 112.7(2) . . ? C51A O51X H51X 112.8 . . ? C2B N1B C20B 109.7(3) . . ? C2B N1B C12B 110.4(3) . . ? C20B N1B C12B 110.2(3) . . ? C2B N1B H1B 108.9 . . ? C20B N1B H1B 108.9 . . ? C12B N1B H1B 108.9 . . ? N1B C2B C3B 113.0(3) . . ? N1B C2B H2B 109.0 . . ? C3B C2B H2B 109.0 . . ? N1B C2B H2Y 109.0 . . ? C3B C2B H2Y 109.0 . . ? H2B C2B H2Y 107.8 . . ? N4B C3B C2B 112.3(3) . . ? N4B C3B H3B 109.1 . . ? C2B C3B H3B 109.1 . . ? N4B C3B H3Y 109.1 . . ? C2B C3B H3Y 109.1 . . ? H3B C3B H3Y 107.9 . . ? C3B N4B C5B 111.2(3) . . ? C3B N4B C30B 110.4(3) . . ? C5B N4B C30B 110.0(3) . . ? N4B C5B C6B 112.0(3) . . ? N4B C5B H5B 109.2 . . ? C6B C5B H5B 109.2 . . ? N4B C5B H5Y 109.2 . . ? C6B C5B H5Y 109.2 . . ? H5B C5B H5Y 107.9 . . ? C5B C6B N7B 112.6(3) . . ? C5B C6B H6B 109.1 . . ? N7B C6B H6B 109.1 . . ? C5B C6B H6Y 109.1 . . ? N7B C6B H6Y 109.1 . . ? H6B C6B H6Y 107.8 . . ? C40B N7B C8B 109.9(3) . . ? C40B N7B C6B 112.3(3) . . ? C8B N7B C6B 111.4(3) . . ? C40B N7B H7B 107.7 . . ? C8B N7B H7B 107.7 . . ? C6B N7B H7B 107.7 . . ? N7B C8B C9B 112.3(3) . . ? N7B C8B H8B 109.2 . . ? C9B C8B H8B 109.2 . . ? N7B C8B H8Y 109.2 . . ? C9B C8B H8Y 109.2 . . ? H8B C8B H8Y 107.9 . . ? N10B C9B C8B 111.6(3) . . ? N10B C9B H9B 109.3 . . ? C8B C9B H9B 109.3 . . ? N10B C9B H9Y 109.3 . . ? C8B C9B H9Y 109.3 . . ? H9B C9B H9Y 108.0 . . ? C50B N10B C11B 111.0(3) . . ? C50B N10B C9B 113.3(3) . . ? C11B N10B C9B 111.5(3) . . ? N10B C11B C12B 111.4(3) . . ? N10B C11B H11B 109.4 . . ? C12B C11B H11B 109.4 . . ? N10B C11B H11Y 109.4 . . ? C12B C11B H11Y 109.4 . . ? H11B C11B H11Y 108.0 . . ? C11B C12B N1B 111.6(3) . . ? C11B C12B H12B 109.3 . . ? N1B C12B H12B 109.3 . . ? C11B C12B H12Y 109.3 . . ? N1B C12B H12Y 109.3 . . ? H12B C12B H12Y 108.0 . . ? N1B C20B P1B 116.3(2) . . ? N1B C20B H20B 108.2 . . ? P1B C20B H20B 108.2 . . ? N1B C20B H20Y 108.2 . . ? P1B C20B H20Y 108.2 . . ? H20B C20B H20Y 107.4 . . ? O11B P1B O12B 117.26(15) . . ? O11B P1B C21B 112.73(16) . . ? O12B P1B C21B 108.75(16) . . ? O11B P1B C20B 108.31(14) . . ? O12B P1B C20B 105.67(15) . . ? C21B P1B C20B 102.91(16) . . ? C22B C21B P1B 114.8(2) . . ? C22B C21B H21B 108.6 . . ? P1B C21B H21B 108.6 . . ? C22B C21B H21Y 108.6 . . ? P1B C21B H21Y 108.6 . . ? H21B C21B H21Y 107.5 . . ? C23B C22B C21B 113.1(3) . . ? C23B C22B H22B 109.0 . . ? C21B C22B H22B 109.0 . . ? C23B C22B H22Y 109.0 . . ? C21B C22B H22Y 109.0 . . ? H22B C22B H22Y 107.8 . . ? O23Y C23B O23B 122.5(3) . . ? O23Y C23B C22B 124.6(3) . . ? O23B C23B C22B 112.9(3) . . ? C23B O23B H23B 106.6 . . ? N4B C30B C31B 113.1(3) . . ? N4B C30B H30B 109.0 . . ? C31B C30B H30B 109.0 . . ? N4B C30B H30Y 109.0 . . ? C31B C30B H30Y 109.0 . . ? H30B C30B H30Y 107.8 . . ? O31B C31B O31Y 124.6(3) . . ? O31B C31B C30B 123.6(3) . . ? O31Y C31B C30B 111.8(3) . . ? C31B O31B Na1 135.4(2) . . ? C31B O31Y H31Y 113.9 . . ? N7B C40B C41B 111.8(3) . . ? N7B C40B H40B 109.2 . . ? C41B C40B H40B 109.2 . . ? N7B C40B H40Y 109.2 . . ? C41B C40B H40Y 109.2 . . ? H40B C40B H40Y 107.9 . . ? O41B C41B O41Y 126.8(3) . . ? O41B C41B C40B 118.8(3) . . ? O41Y C41B C40B 114.3(3) . . ? C41B O41B Na1 120.8(2) . . ? C41B O41Y H51X 113.6 . . ? N10B C50B C51B 112.1(3) . . ? N10B C50B H50B 109.2 . . ? C51B C50B H50B 109.2 . . ? N10B C50B H50Y 109.2 . . ? C51B C50B H50Y 109.2 . . ? H50B C50B H50Y 107.9 . . ? O51B C51B O51Y 125.1(3) . . ? O51B C51B C50B 122.1(3) . . ? O51Y C51B C50B 112.8(3) . . ? C51B O51B Na1 109.0(2) . . ? C51B O51Y H51Y 111.3 . . ? H1W1 O1W H1W2 105.7 . . ? H2W1 O2W H2W2 101.3 . . ? H3W1 O3W H3W2 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.076 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.064