Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Charles T O'Hara" _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email CHARLIE.OHARA@STRATH.AC.UK _publ_section_title ; Synthetic and Structural Investigations of Alkali Metal Diamine Bis(phenolate) Complexes ; loop_ _publ_author_name "Charles T O'Hara" W.Clegg 'Matthew G. Davidson' 'David V. Graham' 'Gemma Griffen' ; M.D.Jones ; 'Alan R Kennedy' 'Luca Russo' 'Calum M. Thomson' # Attachment 'dalton2.cif' data_coh2 _database_code_depnum_ccdc_archive 'CCDC 669061' #--------------------------------------------------------------- #----------------COMPOUND 1------------------------------------ #--------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H124 Li4 N4 O4' _chemical_formula_sum 'C82 H124 Li4 N4 O4' _chemical_formula_weight 1257.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 15.1350(6) _cell_length_b 16.7141(6) _cell_length_c 18.3935(7) _cell_angle_alpha 88.527(2) _cell_angle_beta 66.122(2) _cell_angle_gamma 69.106(2) _cell_volume 3936.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14561 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description bar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.063 _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 123(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' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26003 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13822 _reflns_number_gt 7928 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1.9658P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13822 _refine_ls_number_parameters 896 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1311 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Li1 Li -0.1734(3) 0.4546(3) 0.7168(3) 0.0305(10) Uani 1 1 d . . . Li2 Li -0.0041(3) 0.4201(3) 0.7051(3) 0.0303(10) Uani 1 1 d . . . Li3 Li 0.0599(3) 0.2499(3) 0.6836(3) 0.0301(11) Uani 1 1 d . . . Li4 Li 0.1545(3) 0.2174(3) 0.7628(3) 0.0319(11) Uani 1 1 d . . . O1 O -0.10902(12) 0.52845(10) 0.72346(10) 0.0243(4) Uani 1 1 d . . . O2 O -0.05505(12) 0.34191(10) 0.67419(10) 0.0247(4) Uani 1 1 d . . . O3 O 0.13299(13) 0.14399(10) 0.70381(10) 0.0262(4) Uani 1 1 d . . . O4 O 0.10143(13) 0.32895(10) 0.72533(10) 0.0254(4) Uani 1 1 d . . . N1 N -0.29222(15) 0.52634(13) 0.69170(12) 0.0240(5) Uani 1 1 d . . . N2 N -0.27397(15) 0.42658(13) 0.81904(12) 0.0254(5) Uani 1 1 d . . . N3 N 0.28538(16) 0.14562(13) 0.77366(12) 0.0272(5) Uani 1 1 d . . . N4 N 0.07585(16) 0.25167(13) 0.88464(12) 0.0265(5) Uani 1 1 d . . . C1 C -0.16530(19) 0.61394(16) 0.74154(15) 0.0232(6) Uani 1 1 d . . . C2 C -0.15205(19) 0.67028(16) 0.78966(15) 0.0239(6) Uani 1 1 d . . . C3 C -0.2136(2) 0.75819(16) 0.80409(15) 0.0279(6) Uani 1 1 d . . . H3 H -0.2031 0.7952 0.8354 0.033 Uiso 1 1 calc R . . C4 C -0.2892(2) 0.79539(17) 0.77584(16) 0.0290(6) Uani 1 1 d . A . C5 C -0.3022(2) 0.73971(17) 0.73015(15) 0.0284(6) Uani 1 1 d . . . H5 H -0.3539 0.7627 0.7103 0.034 Uiso 1 1 calc R . . C6 C -0.24252(19) 0.65135(16) 0.71211(15) 0.0235(6) Uani 1 1 d . . . C7 C -0.0719(2) 0.63627(16) 0.82531(15) 0.0273(6) Uani 1 1 d . . . C8 C -0.0975(2) 0.56960(18) 0.88058(16) 0.0358(7) Uani 1 1 d . . . H8A H -0.1671 0.5971 0.9246 0.054 Uiso 1 1 calc R . . H8B H -0.0457 0.5473 0.9027 0.054 Uiso 1 1 calc R . . H8C H -0.0960 0.5218 0.8498 0.054 Uiso 1 1 calc R . . C9 C 0.0386(2) 0.59625(17) 0.75825(16) 0.0320(7) Uani 1 1 d . . . H9A H 0.0416 0.5522 0.7222 0.048 Uiso 1 1 calc R . . H9B H 0.0881 0.5695 0.7817 0.048 Uiso 1 1 calc R . . H9C H 0.0568 0.6414 0.7279 0.048 Uiso 1 1 calc R . . C10 C -0.0719(2) 0.70774(18) 0.87610(18) 0.0431(8) Uani 1 1 d . . . H10A H -0.0532 0.7507 0.8423 0.065 Uiso 1 1 calc R . . H10B H -0.0209 0.6824 0.8985 0.065 Uiso 1 1 calc R . . H10C H -0.1415 0.7358 0.9199 0.065 Uiso 1 1 calc R . . C11 C -0.3545(2) 0.89325(18) 0.79269(19) 0.0415(8) Uani 1 1 d . . . C12 C -0.4712(3) 0.9092(3) 0.8324(4) 0.0655(17) Uani 0.787(6) 1 d P A 1 H12A H -0.5123 0.9715 0.8421 0.098 Uiso 0.787(6) 1 calc PR A 1 H12B H -0.4878 0.8859 0.8835 0.098 Uiso 0.787(6) 1 calc PR A 1 H12C H -0.4880 0.8805 0.7969 0.098 Uiso 0.787(6) 1 calc PR A 1 C13 C -0.3326(4) 0.9287(3) 0.7113(3) 0.080(2) Uani 0.787(6) 1 d P A 1 H13A H -0.3525 0.8995 0.6784 0.120 Uiso 0.787(6) 1 calc PR A 1 H13B H -0.2580 0.9180 0.6832 0.120 Uiso 0.787(6) 1 calc PR A 1 H13C H -0.3734 0.9910 0.7207 0.120 Uiso 0.787(6) 1 calc PR A 1 C14 C -0.3294(5) 0.9417(3) 0.8437(4) 0.091(2) Uani 0.787(6) 1 d P A 1 H14A H -0.3723 1.0035 0.8519 0.136 Uiso 0.787(6) 1 calc PR A 1 H14B H -0.2554 0.9332 0.8169 0.136 Uiso 0.787(6) 1 calc PR A 1 H14C H -0.3440 0.9204 0.8957 0.136 Uiso 0.787(6) 1 calc PR A 1 C15 C -0.2612(2) 0.59901(16) 0.65822(15) 0.0268(6) Uani 1 1 d . . . H15A H -0.3164 0.6386 0.6439 0.032 Uiso 1 1 calc R . . H15B H -0.1965 0.5752 0.6079 0.032 Uiso 1 1 calc R . . C16 C -0.3216(2) 0.49091(17) 0.63671(16) 0.0302(6) Uani 1 1 d . . . H16A H -0.3359 0.4395 0.6555 0.045 Uiso 1 1 calc R . . H16B H -0.2642 0.4750 0.5828 0.045 Uiso 1 1 calc R . . H16C H -0.3842 0.5345 0.6351 0.045 Uiso 1 1 calc R . . C17 C -0.37571(19) 0.55067(16) 0.77364(15) 0.0259(6) Uani 1 1 d . . . H17A H -0.4441 0.5806 0.7719 0.031 Uiso 1 1 calc R . . H17B H -0.3649 0.5908 0.8049 0.031 Uiso 1 1 calc R . . C18 C -0.37490(19) 0.46971(16) 0.81394(16) 0.0276(6) Uani 1 1 d . . . H18A H -0.4327 0.4856 0.8685 0.033 Uiso 1 1 calc R . . H18B H -0.3855 0.4296 0.7826 0.033 Uiso 1 1 calc R . . C19 C -0.2820(2) 0.45321(18) 0.89768(15) 0.0331(7) Uani 1 1 d . . . H19A H -0.3086 0.5165 0.9080 0.050 Uiso 1 1 calc R . . H19B H -0.2128 0.4289 0.8979 0.050 Uiso 1 1 calc R . . H19C H -0.3298 0.4321 0.9396 0.050 Uiso 1 1 calc R . . C20 C -0.2329(2) 0.33112(16) 0.80098(15) 0.0261(6) Uani 1 1 d . . . H20A H -0.2869 0.3098 0.8360 0.031 Uiso 1 1 calc R . . H20B H -0.1714 0.3057 0.8131 0.031 Uiso 1 1 calc R . . C21 C -0.11348(19) 0.31036(15) 0.65268(15) 0.0218(6) Uani 1 1 d . . . C22 C -0.09039(19) 0.28697(15) 0.57148(14) 0.0223(6) Uani 1 1 d . . . C23 C -0.15402(19) 0.25266(16) 0.55700(15) 0.0251(6) Uani 1 1 d . . . H23 H -0.1384 0.2365 0.5027 0.030 Uiso 1 1 calc R . . C24 C -0.23948(19) 0.24041(16) 0.61715(15) 0.0242(6) Uani 1 1 d . B . C25 C -0.26203(19) 0.26653(15) 0.69538(15) 0.0240(6) Uani 1 1 d . . . H25 H -0.3204 0.2603 0.7377 0.029 Uiso 1 1 calc R . . C26 C -0.20204(19) 0.30157(15) 0.71418(14) 0.0225(6) Uani 1 1 d . . . C27 C 0.0008(2) 0.29944(16) 0.49991(15) 0.0273(6) Uani 1 1 d . . . C28 C 0.0092(2) 0.2694(2) 0.41849(16) 0.0413(8) Uani 1 1 d . . . H28A H 0.0211 0.2078 0.4144 0.062 Uiso 1 1 calc R . . H28B H 0.0677 0.2787 0.3753 0.062 Uiso 1 1 calc R . . H28C H -0.0557 0.3026 0.4137 0.062 Uiso 1 1 calc R . . C29 C 0.1066(2) 0.24770(18) 0.50120(16) 0.0336(7) Uani 1 1 d . . . H29A H 0.1078 0.2689 0.5499 0.050 Uiso 1 1 calc R . . H29B H 0.1625 0.2548 0.4538 0.050 Uiso 1 1 calc R . . H29C H 0.1170 0.1864 0.5008 0.050 Uiso 1 1 calc R . . C30 C -0.0168(2) 0.39600(17) 0.50249(16) 0.0325(7) Uani 1 1 d . . . H30A H -0.0826 0.4286 0.4986 0.049 Uiso 1 1 calc R . . H30B H 0.0410 0.4038 0.4574 0.049 Uiso 1 1 calc R . . H30C H -0.0202 0.4171 0.5531 0.049 Uiso 1 1 calc R . . C31 C -0.3050(2) 0.20041(18) 0.59693(16) 0.0328(7) Uani 1 1 d . . . C32 C -0.4208(4) 0.2727(4) 0.6308(4) 0.075(2) Uani 0.619(5) 1 d P B 1 H32A H -0.4203 0.3228 0.6019 0.113 Uiso 0.619(5) 1 calc PR B 1 H32B H -0.4456 0.2907 0.6882 0.113 Uiso 0.619(5) 1 calc PR B 1 H32C H -0.4673 0.2489 0.6230 0.113 Uiso 0.619(5) 1 calc PR B 1 C33 C -0.2741(5) 0.1820(5) 0.5088(3) 0.073(2) Uani 0.619(5) 1 d P B 1 H33A H -0.3246 0.1634 0.5011 0.109 Uiso 0.619(5) 1 calc PR B 1 H33B H -0.2045 0.1360 0.4838 0.109 Uiso 0.619(5) 1 calc PR B 1 H33C H -0.2730 0.2344 0.4841 0.109 Uiso 0.619(5) 1 calc PR B 1 C34 C -0.3135(6) 0.1263(4) 0.6398(4) 0.076(3) Uani 0.619(5) 1 d P B 1 H34A H -0.3630 0.1072 0.6311 0.113 Uiso 0.619(5) 1 calc PR B 1 H34B H -0.3382 0.1433 0.6974 0.113 Uiso 0.619(5) 1 calc PR B 1 H34C H -0.2449 0.0788 0.6196 0.113 Uiso 0.619(5) 1 calc PR B 1 C35 C 0.16967(19) 0.05877(16) 0.70799(14) 0.0246(6) Uani 1 1 d . . . C36 C 0.11708(19) 0.00436(16) 0.70478(15) 0.0255(6) Uani 1 1 d . . . C37 C 0.1629(2) -0.08397(16) 0.70802(15) 0.0289(6) Uani 1 1 d . . . H37 H 0.1283 -0.1200 0.7039 0.035 Uiso 1 1 calc R . . C38 C 0.2549(2) -0.12254(16) 0.71684(15) 0.0281(6) Uani 1 1 d . . . C39 C 0.3037(2) -0.06779(17) 0.72140(15) 0.0289(6) Uani 1 1 d . . . H39 H 0.3665 -0.0914 0.7284 0.035 Uiso 1 1 calc R . . C40 C 0.26479(19) 0.02075(16) 0.71618(15) 0.0260(6) Uani 1 1 d . . . C41 C 0.0124(2) 0.03990(17) 0.69831(16) 0.0302(7) Uani 1 1 d . . . C42 C -0.0687(2) 0.10776(18) 0.77158(17) 0.0373(7) Uani 1 1 d . . . H42A H -0.0784 0.0806 0.8206 0.056 Uiso 1 1 calc R . . H42B H -0.1353 0.1318 0.7671 0.056 Uiso 1 1 calc R . . H42C H -0.0443 0.1542 0.7738 0.056 Uiso 1 1 calc R . . C43 C 0.0251(2) 0.07971(18) 0.62047(16) 0.0359(7) Uani 1 1 d . . . H43A H -0.0434 0.1074 0.6195 0.054 Uiso 1 1 calc R . . H43B H 0.0710 0.0342 0.5743 0.054 Uiso 1 1 calc R . . H43C H 0.0558 0.1230 0.6178 0.054 Uiso 1 1 calc R . . C44 C -0.0318(2) -0.02957(19) 0.6972(2) 0.0444(8) Uani 1 1 d . . . H44A H -0.0436 -0.0553 0.7471 0.067 Uiso 1 1 calc R . . H44B H 0.0181 -0.0746 0.6514 0.067 Uiso 1 1 calc R . . H44C H -0.0980 -0.0031 0.6924 0.067 Uiso 1 1 calc R . . C45 C 0.3027(2) -0.21990(17) 0.72011(17) 0.0351(7) Uani 1 1 d . . . C46 C 0.2363(3) -0.26774(19) 0.7137(2) 0.0505(9) Uani 1 1 d . . . H46A H 0.1676 -0.2455 0.7596 0.076 Uiso 1 1 calc R . . H46B H 0.2710 -0.3297 0.7138 0.076 Uiso 1 1 calc R . . H46C H 0.2277 -0.2587 0.6638 0.076 Uiso 1 1 calc R . . C47 C 0.4119(2) -0.26019(19) 0.65043(19) 0.0534(9) Uani 1 1 d . . . H47A H 0.4065 -0.2513 0.5993 0.080 Uiso 1 1 calc R . . H47B H 0.4418 -0.3223 0.6524 0.080 Uiso 1 1 calc R . . H47C H 0.4571 -0.2327 0.6552 0.080 Uiso 1 1 calc R . . C48 C 0.3128(3) -0.23347(19) 0.79959(19) 0.0504(9) Uani 1 1 d . . . H48A H 0.3569 -0.2046 0.8040 0.076 Uiso 1 1 calc R . . H48B H 0.3444 -0.2955 0.8011 0.076 Uiso 1 1 calc R . . H48C H 0.2434 -0.2089 0.8444 0.076 Uiso 1 1 calc R . . C49 C 0.33291(19) 0.06952(17) 0.71127(16) 0.0290(6) Uani 1 1 d . . . H49A H 0.3970 0.0290 0.7146 0.035 Uiso 1 1 calc R . . H49B H 0.3543 0.0894 0.6579 0.035 Uiso 1 1 calc R . . C50 C 0.3644(2) 0.18136(18) 0.76371(18) 0.0357(7) Uani 1 1 d . . . H50A H 0.4208 0.1390 0.7740 0.054 Uiso 1 1 calc R . . H50B H 0.3324 0.2344 0.8017 0.054 Uiso 1 1 calc R . . H50C H 0.3927 0.1946 0.7088 0.054 Uiso 1 1 calc R . . C51 C 0.2387(2) 0.12668(17) 0.85621(15) 0.0321(7) Uani 1 1 d . . . H51A H 0.2940 0.0993 0.8748 0.039 Uiso 1 1 calc R . . H51B H 0.2045 0.0857 0.8572 0.039 Uiso 1 1 calc R . . C52 C 0.1588(2) 0.20945(17) 0.91192(16) 0.0316(7) Uani 1 1 d . . . H52A H 0.1275 0.1961 0.9671 0.038 Uiso 1 1 calc R . . H52B H 0.1936 0.2493 0.9129 0.038 Uiso 1 1 calc R . . C53 C -0.0137(2) 0.22672(18) 0.92629(17) 0.0359(7) Uani 1 1 d . . . H53A H 0.0098 0.1635 0.9195 0.054 Uiso 1 1 calc R . . H53B H -0.0647 0.2510 0.9037 0.054 Uiso 1 1 calc R . . H53C H -0.0462 0.2489 0.9836 0.054 Uiso 1 1 calc R . . C54 C 0.04262(19) 0.34705(16) 0.89253(15) 0.0254(6) Uani 1 1 d . . . H54A H 0.0247 0.3697 0.9480 0.031 Uiso 1 1 calc R . . H54B H -0.0208 0.3724 0.8826 0.031 Uiso 1 1 calc R . . C55 C 0.15480(19) 0.36287(15) 0.75103(15) 0.0228(6) Uani 1 1 d . . . C56 C 0.23717(19) 0.38633(16) 0.69728(15) 0.0243(6) Uani 1 1 d . . . C57 C 0.28496(19) 0.42226(16) 0.73036(15) 0.0255(6) Uani 1 1 d . . . H57 H 0.3403 0.4378 0.6945 0.031 Uiso 1 1 calc R . . C58 C 0.25741(19) 0.43701(16) 0.81220(15) 0.0239(6) Uani 1 1 d . . . C59 C 0.17792(19) 0.41191(16) 0.86299(15) 0.0250(6) Uani 1 1 d . . . H59 H 0.1572 0.4206 0.9192 0.030 Uiso 1 1 calc R . . C60 C 0.12737(18) 0.37436(15) 0.83406(15) 0.0233(6) Uani 1 1 d . . . C61 C 0.2748(2) 0.37201(17) 0.60520(15) 0.0293(6) Uani 1 1 d . . . C62 C 0.3587(2) 0.4090(2) 0.56063(16) 0.0441(8) Uani 1 1 d . . . H62A H 0.3305 0.4712 0.5786 0.066 Uiso 1 1 calc R . . H62B H 0.3796 0.3992 0.5027 0.066 Uiso 1 1 calc R . . H62C H 0.4196 0.3802 0.5721 0.066 Uiso 1 1 calc R . . C63 C 0.1858(2) 0.41568(18) 0.57987(16) 0.0350(7) Uani 1 1 d . . . H63A H 0.1367 0.3861 0.5979 0.053 Uiso 1 1 calc R . . H63B H 0.2145 0.4124 0.5213 0.053 Uiso 1 1 calc R . . H63C H 0.1492 0.4764 0.6043 0.053 Uiso 1 1 calc R . . C64 C 0.3227(2) 0.27488(18) 0.57468(17) 0.0403(8) Uani 1 1 d . . . H64A H 0.3855 0.2475 0.5840 0.060 Uiso 1 1 calc R . . H64B H 0.3413 0.2664 0.5171 0.060 Uiso 1 1 calc R . . H64C H 0.2719 0.2488 0.6035 0.060 Uiso 1 1 calc R . . C65 C 0.3097(2) 0.47905(17) 0.84662(15) 0.0286(6) Uani 1 1 d . . . C66 C 0.3946(2) 0.50253(18) 0.78153(17) 0.0350(7) Uani 1 1 d . . . H66A H 0.4498 0.4499 0.7462 0.052 Uiso 1 1 calc R . . H66B H 0.4241 0.5307 0.8066 0.052 Uiso 1 1 calc R . . H66C H 0.3644 0.5421 0.7501 0.052 Uiso 1 1 calc R . . C67 C 0.2270(2) 0.56186(19) 0.90350(18) 0.0451(8) Uani 1 1 d . . . H67A H 0.1945 0.6023 0.8737 0.068 Uiso 1 1 calc R . . H67B H 0.2602 0.5887 0.9259 0.068 Uiso 1 1 calc R . . H67C H 0.1736 0.5475 0.9472 0.068 Uiso 1 1 calc R . . C68 C 0.3604(2) 0.41618(19) 0.89387(17) 0.0391(7) Uani 1 1 d . . . H68A H 0.3069 0.4014 0.9371 0.059 Uiso 1 1 calc R . . H68B H 0.3924 0.4436 0.9169 0.059 Uiso 1 1 calc R . . H68C H 0.4140 0.3635 0.8577 0.059 Uiso 1 1 calc R . . C1S C 0.2856(3) 0.7809(2) 1.0143(2) 0.0692(11) Uani 1 1 d . . . H1S1 H 0.2654 0.8264 0.9829 0.104 Uiso 1 1 calc R . . H1S2 H 0.2309 0.7948 1.0693 0.104 Uiso 1 1 calc R . . H1S3 H 0.2947 0.7254 0.9897 0.104 Uiso 1 1 calc R . . C2S C 0.3834(3) 0.7749(2) 1.0155(2) 0.0560(9) Uani 1 1 d . . . C3S C 0.4773(3) 0.7254(2) 0.9532(2) 0.0620(10) Uani 1 1 d . . . H3S H 0.4776 0.6938 0.9108 0.074 Uiso 1 1 calc R . . C4S C 0.5701(3) 0.7213(2) 0.9519(2) 0.0660(10) Uani 1 1 d . . . H4S H 0.6336 0.6881 0.9077 0.079 Uiso 1 1 calc R . . C5S C 0.5736(3) 0.7650(3) 1.0140(3) 0.0722(12) Uani 1 1 d . . . H5S H 0.6382 0.7624 1.0122 0.087 Uiso 1 1 calc R . . C6S C 0.4822(3) 0.8108(2) 1.0768(3) 0.0739(12) Uani 1 1 d . . . H6S H 0.4829 0.8386 1.1209 0.089 Uiso 1 1 calc R . . C7S C 0.3872(3) 0.8178(2) 1.0778(2) 0.0590(9) Uiso 1 1 d . . . H7S H 0.3239 0.8523 1.1215 0.071 Uiso 1 1 calc R . . C8S C 0.4699(7) -0.0538(5) 0.5298(4) 0.030(2) Uiso 0.50 1 d P C -1 H8S H 0.4270 -0.0867 0.5461 0.036 Uiso 0.50 1 calc PR C -1 C9S C 0.6000(5) 0.0340(4) 0.4766(3) 0.0403(15) Uiso 0.50 1 d P C -1 H9S H 0.6446 0.0654 0.4584 0.048 Uiso 0.50 1 calc PR C -1 C10S C 0.6295(8) -0.0369(6) 0.5099(5) 0.052(3) Uiso 0.50 1 d P C -1 H10S H 0.6950 -0.0559 0.5128 0.062 Uiso 0.50 1 calc PR C -1 C11S C 0.5653(6) -0.0827(4) 0.5401(4) 0.0532(18) Uiso 0.50 1 d P C -1 H11S H 0.5834 -0.1314 0.5665 0.064 Uiso 0.50 1 calc PR C -1 C12S C 0.4408(5) 0.0169(4) 0.4985(4) 0.0404(15) Uiso 0.50 1 d P C -1 C81S C 0.5024(7) 0.0659(5) 0.4669(4) 0.034(3) Uiso 0.50 1 d P C -1 H81S H 0.4828 0.1152 0.4415 0.041 Uiso 0.50 1 calc PR C -1 C91S C 0.3383(7) 0.0509(7) 0.4909(6) 0.061(3) Uiso 0.50 1 d P C -1 H91A H 0.3003 0.0128 0.5130 0.091 Uiso 0.50 1 calc PR C -1 H91B H 0.3521 0.0526 0.4341 0.091 Uiso 0.50 1 calc PR C -1 H91C H 0.2962 0.1093 0.5206 0.091 Uiso 0.50 1 calc PR C -1 C33A C -0.2241(7) 0.1044(5) 0.5512(5) 0.053(3) Uiso 0.381(5) 1 d P B 2 H33D H -0.2611 0.0741 0.5373 0.080 Uiso 0.381(5) 1 calc PR B 2 H33E H -0.1942 0.0723 0.5864 0.080 Uiso 0.381(5) 1 calc PR B 2 H33F H -0.1681 0.1087 0.5021 0.080 Uiso 0.381(5) 1 calc PR B 2 C34A C -0.3894(7) 0.1884(6) 0.6696(5) 0.047(3) Uiso 0.381(5) 1 d P B 2 H34D H -0.4402 0.2450 0.7002 0.071 Uiso 0.381(5) 1 calc PR B 2 H34E H -0.3586 0.1538 0.7034 0.071 Uiso 0.381(5) 1 calc PR B 2 H34F H -0.4246 0.1584 0.6528 0.071 Uiso 0.381(5) 1 calc PR B 2 C32A C -0.3507(8) 0.2516(7) 0.5468(6) 0.063(3) Uiso 0.381(5) 1 d P B 2 H32D H -0.4012 0.2306 0.5422 0.094 Uiso 0.381(5) 1 calc PR B 2 H32E H -0.2955 0.2463 0.4933 0.094 Uiso 0.381(5) 1 calc PR B 2 H32F H -0.3862 0.3124 0.5712 0.094 Uiso 0.381(5) 1 calc PR B 2 C14A C -0.4076(13) 0.9237(9) 0.8881(8) 0.043(4) Uiso 0.213(6) 1 d P A 2 H14D H -0.4355 0.9870 0.8987 0.065 Uiso 0.213(6) 1 calc PR A 2 H14E H -0.3551 0.8997 0.9094 0.065 Uiso 0.213(6) 1 calc PR A 2 H14F H -0.4644 0.9030 0.9143 0.065 Uiso 0.213(6) 1 calc PR A 2 C12A C -0.4430(13) 0.9209(10) 0.7683(11) 0.051(5) Uiso 0.213(6) 1 d P A 2 H12D H -0.4869 0.8875 0.7921 0.076 Uiso 0.213(6) 1 calc PR A 2 H12E H -0.4152 0.9106 0.7097 0.076 Uiso 0.213(6) 1 calc PR A 2 H12F H -0.4848 0.9826 0.7872 0.076 Uiso 0.213(6) 1 calc PR A 2 C13A C -0.2796(12) 0.9401(10) 0.7549(10) 0.052(5) Uiso 0.213(6) 1 d P A 2 H13D H -0.2430 0.9218 0.6968 0.077 Uiso 0.213(6) 1 calc PR A 2 H13E H -0.2287 0.9258 0.7780 0.077 Uiso 0.213(6) 1 calc PR A 2 H13F H -0.3193 1.0027 0.7658 0.077 Uiso 0.213(6) 1 calc PR A 2 C13S C 0.0174(11) -0.0363(7) 0.9285(7) 0.011(3) Uiso 0.25 1 d PG D -1 H13S H 0.0350 -0.0632 0.8770 0.013 Uiso 0.25 1 calc PR D -1 C14S C 0.0944(11) -0.0268(9) 0.9461(8) 0.036(5) Uiso 0.25 1 d PG D -1 H14S H 0.1647 -0.0472 0.9067 0.043 Uiso 0.25 1 calc PR D -1 C15S C 0.0687(13) 0.0126(12) 1.0214(9) 0.057(9) Uiso 0.25 1 d PG D -1 C16S C -0.0341(15) 0.0425(14) 1.0791(8) 0.128(14) Uiso 0.25 1 d PG D -1 H16S H -0.0517 0.0694 1.1306 0.154 Uiso 0.25 1 calc PR D -1 C17S C -0.1112(12) 0.0330(12) 1.0615(8) 0.059(8) Uiso 0.25 1 d PG D -1 H17S H -0.1814 0.0534 1.1009 0.071 Uiso 0.25 1 calc PR D -1 C18S C -0.0854(11) -0.0064(9) 0.9861(8) 0.047(8) Uiso 0.25 1 d PG D -1 H18S H -0.1381 -0.0129 0.9741 0.057 Uiso 0.25 1 calc PR D -1 C19S C 0.0535(8) -0.0313(7) 0.9344(5) 0.036(7) Uiso 0.25 1 d PG E -2 H19S H 0.0684 -0.0574 0.8834 0.044 Uiso 0.25 1 calc PR E -2 C20S C 0.1332(5) -0.0231(6) 0.9492(4) 0.032(3) Uiso 0.25 1 d PG E -2 H20S H 0.2025 -0.0435 0.9083 0.039 Uiso 0.25 1 calc PR E -2 C21S C 0.1114(5) 0.0152(5) 1.0239(5) 0.023(3) Uiso 0.25 1 d PG E -2 C22S C 0.0099(6) 0.0451(5) 1.0838(4) 0.025(3) Uiso 0.25 1 d PG E -2 H22S H -0.0049 0.0712 1.1348 0.030 Uiso 0.25 1 calc PR E -2 C23S C -0.0697(5) 0.0369(6) 1.0690(5) 0.015(5) Uiso 0.25 1 d PG E -2 H23S H -0.1390 0.0573 1.1099 0.019 Uiso 0.25 1 calc PR E -2 C24S C -0.0479(7) -0.0014(7) 0.9943(6) 0.027(3) Uiso 0.25 1 d PG E -2 H24S H -0.1024 -0.0070 0.9842 0.032 Uiso 0.25 1 calc PR E -2 C25S C 0.1839(6) 0.0222(5) 1.0393(4) 0.065(2) Uiso 0.50 1 d P D -1 H25A H 0.1572 0.0507 1.0940 0.098 Uiso 0.50 1 calc PR D -1 H25B H 0.2155 0.0565 1.0006 0.098 Uiso 0.50 1 calc PR D -1 H25C H 0.2366 -0.0356 1.0321 0.098 Uiso 0.50 1 calc PR D -1 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 Li1 0.026(2) 0.031(3) 0.036(3) 0.004(2) -0.015(2) -0.010(2) Li2 0.028(2) 0.031(3) 0.034(3) 0.002(2) -0.016(2) -0.009(2) Li3 0.029(3) 0.026(2) 0.039(3) 0.005(2) -0.019(2) -0.008(2) Li4 0.033(3) 0.030(3) 0.028(3) 0.002(2) -0.014(2) -0.007(2) O1 0.0207(9) 0.0225(10) 0.0299(10) 0.0031(8) -0.0113(8) -0.0074(8) O2 0.0229(10) 0.0263(10) 0.0297(10) 0.0054(8) -0.0145(8) -0.0108(8) O3 0.0271(10) 0.0201(10) 0.0310(10) 0.0045(8) -0.0133(8) -0.0073(8) O4 0.0248(10) 0.0247(10) 0.0298(10) 0.0010(8) -0.0157(8) -0.0079(8) N1 0.0236(12) 0.0278(12) 0.0247(12) 0.0024(10) -0.0115(10) -0.0128(10) N2 0.0221(12) 0.0269(13) 0.0277(12) 0.0013(10) -0.0115(10) -0.0088(10) N3 0.0239(12) 0.0288(13) 0.0289(13) 0.0011(10) -0.0127(10) -0.0079(10) N4 0.0233(12) 0.0256(13) 0.0279(12) 0.0019(10) -0.0103(10) -0.0070(10) C1 0.0190(14) 0.0233(15) 0.0247(14) 0.0026(12) -0.0048(12) -0.0100(12) C2 0.0197(14) 0.0259(15) 0.0231(14) 0.0030(11) -0.0060(12) -0.0090(12) C3 0.0274(15) 0.0260(16) 0.0297(15) -0.0014(12) -0.0113(13) -0.0101(13) C4 0.0245(15) 0.0257(15) 0.0356(16) 0.0057(13) -0.0134(13) -0.0075(12) C5 0.0227(15) 0.0298(16) 0.0344(16) 0.0083(13) -0.0146(13) -0.0093(13) C6 0.0212(14) 0.0228(15) 0.0265(15) 0.0030(12) -0.0098(12) -0.0087(12) C7 0.0249(15) 0.0271(15) 0.0269(15) -0.0023(12) -0.0115(12) -0.0055(12) C8 0.0350(17) 0.0414(18) 0.0309(16) 0.0068(14) -0.0169(14) -0.0113(14) C9 0.0274(16) 0.0356(17) 0.0350(16) 0.0029(13) -0.0160(13) -0.0109(13) C10 0.0430(19) 0.0389(18) 0.0481(19) -0.0078(15) -0.0282(16) -0.0050(15) C11 0.0409(19) 0.0246(16) 0.061(2) 0.0002(15) -0.0289(17) -0.0057(14) C12 0.040(3) 0.034(3) 0.099(4) -0.004(3) -0.026(3) 0.009(2) C13 0.100(4) 0.030(3) 0.093(4) 0.020(3) -0.041(3) -0.008(3) C14 0.092(5) 0.029(3) 0.159(6) -0.028(3) -0.088(5) 0.011(3) C15 0.0259(15) 0.0285(15) 0.0285(15) 0.0062(12) -0.0140(13) -0.0103(12) C16 0.0282(16) 0.0331(16) 0.0338(16) 0.0054(13) -0.0167(13) -0.0125(13) C17 0.0177(14) 0.0291(15) 0.0288(15) 0.0028(12) -0.0084(12) -0.0083(12) C18 0.0228(15) 0.0298(16) 0.0298(15) 0.0033(12) -0.0110(12) -0.0095(12) C19 0.0339(17) 0.0354(17) 0.0305(16) 0.0016(13) -0.0150(14) -0.0121(14) C20 0.0253(15) 0.0272(15) 0.0282(15) 0.0072(12) -0.0122(12) -0.0119(12) C21 0.0206(14) 0.0204(14) 0.0299(15) 0.0058(11) -0.0160(12) -0.0077(11) C22 0.0201(14) 0.0215(14) 0.0251(15) 0.0058(11) -0.0095(12) -0.0079(11) C23 0.0239(15) 0.0262(15) 0.0246(15) 0.0026(12) -0.0108(12) -0.0084(12) C24 0.0222(14) 0.0242(15) 0.0293(16) 0.0019(12) -0.0130(12) -0.0095(12) C25 0.0177(14) 0.0240(15) 0.0288(15) 0.0056(12) -0.0085(12) -0.0081(12) C26 0.0223(14) 0.0217(14) 0.0237(14) 0.0047(11) -0.0113(12) -0.0068(11) C27 0.0241(15) 0.0312(16) 0.0276(15) 0.0055(12) -0.0102(12) -0.0128(12) C28 0.0417(18) 0.058(2) 0.0285(16) 0.0057(15) -0.0086(14) -0.0302(16) C29 0.0238(15) 0.0350(17) 0.0332(16) 0.0055(13) -0.0046(13) -0.0103(13) C30 0.0286(16) 0.0340(17) 0.0355(16) 0.0117(13) -0.0129(13) -0.0137(13) C31 0.0315(16) 0.0389(17) 0.0353(17) 0.0021(13) -0.0153(14) -0.0196(14) C32 0.042(4) 0.074(5) 0.121(6) -0.012(4) -0.045(4) -0.018(3) C33 0.086(5) 0.139(7) 0.039(3) 0.009(4) -0.029(3) -0.089(5) C34 0.124(7) 0.070(5) 0.112(6) 0.054(4) -0.094(6) -0.076(5) C35 0.0240(15) 0.0247(16) 0.0200(14) 0.0022(11) -0.0062(12) -0.0072(12) C36 0.0230(15) 0.0265(16) 0.0232(14) 0.0053(12) -0.0078(12) -0.0076(12) C37 0.0307(16) 0.0261(16) 0.0286(15) 0.0036(12) -0.0115(13) -0.0105(13) C38 0.0281(16) 0.0239(15) 0.0256(15) 0.0042(12) -0.0092(13) -0.0053(13) C39 0.0240(15) 0.0300(16) 0.0270(15) 0.0029(12) -0.0103(12) -0.0045(13) C40 0.0239(15) 0.0266(16) 0.0222(14) 0.0015(12) -0.0065(12) -0.0074(12) C41 0.0277(16) 0.0275(16) 0.0387(17) 0.0053(13) -0.0158(14) -0.0120(13) C42 0.0281(16) 0.0355(17) 0.0430(18) 0.0093(14) -0.0120(14) -0.0099(13) C43 0.0350(17) 0.0314(17) 0.0443(18) 0.0031(14) -0.0228(15) -0.0089(14) C44 0.0379(18) 0.0375(18) 0.067(2) 0.0137(16) -0.0285(17) -0.0181(15) C45 0.0365(17) 0.0254(16) 0.0389(17) 0.0067(13) -0.0175(15) -0.0050(13) C46 0.065(2) 0.0294(18) 0.071(2) 0.0136(16) -0.042(2) -0.0173(16) C47 0.051(2) 0.0309(18) 0.056(2) 0.0047(16) -0.0158(18) 0.0013(15) C48 0.067(2) 0.0345(18) 0.053(2) 0.0137(15) -0.0341(19) -0.0126(16) C49 0.0209(14) 0.0295(16) 0.0316(16) -0.0006(12) -0.0104(12) -0.0045(12) C50 0.0267(16) 0.0346(17) 0.0453(18) -0.0003(14) -0.0177(14) -0.0077(13) C51 0.0346(16) 0.0308(16) 0.0324(16) 0.0059(13) -0.0198(14) -0.0075(13) C52 0.0330(16) 0.0339(17) 0.0273(15) 0.0033(13) -0.0148(13) -0.0095(13) C53 0.0334(17) 0.0364(17) 0.0367(17) 0.0062(14) -0.0091(14) -0.0184(14) C54 0.0199(14) 0.0280(15) 0.0255(15) 0.0015(12) -0.0078(12) -0.0079(12) C55 0.0181(14) 0.0228(14) 0.0276(15) 0.0010(12) -0.0132(12) -0.0035(11) C56 0.0205(14) 0.0243(15) 0.0259(15) 0.0030(12) -0.0111(12) -0.0045(12) C57 0.0182(14) 0.0278(15) 0.0278(15) 0.0051(12) -0.0082(12) -0.0076(12) C58 0.0177(14) 0.0237(14) 0.0280(15) 0.0030(12) -0.0103(12) -0.0047(11) C59 0.0219(14) 0.0286(15) 0.0226(14) 0.0011(12) -0.0101(12) -0.0066(12) C60 0.0176(14) 0.0228(14) 0.0273(15) 0.0001(12) -0.0103(12) -0.0039(11) C61 0.0245(15) 0.0369(17) 0.0245(15) 0.0012(12) -0.0114(13) -0.0080(13) C62 0.0403(19) 0.071(2) 0.0248(16) 0.0099(15) -0.0107(14) -0.0286(17) C63 0.0336(17) 0.0434(18) 0.0259(15) 0.0035(13) -0.0147(14) -0.0097(14) C64 0.0336(17) 0.0470(19) 0.0291(16) -0.0037(14) -0.0127(14) -0.0030(14) C65 0.0248(15) 0.0358(16) 0.0305(16) 0.0034(13) -0.0148(13) -0.0134(13) C66 0.0330(17) 0.0392(17) 0.0412(18) 0.0092(14) -0.0190(14) -0.0194(14) C67 0.0367(18) 0.048(2) 0.050(2) -0.0103(15) -0.0136(16) -0.0199(16) C68 0.0403(18) 0.055(2) 0.0408(18) 0.0174(15) -0.0270(15) -0.0281(16) C1S 0.062(3) 0.077(3) 0.062(2) 0.018(2) -0.027(2) -0.018(2) C2S 0.052(2) 0.055(2) 0.052(2) 0.0158(18) -0.0146(19) -0.0209(18) C3S 0.055(2) 0.051(2) 0.051(2) -0.0012(18) -0.003(2) -0.0099(19) C4S 0.064(3) 0.057(2) 0.063(3) 0.006(2) -0.017(2) -0.020(2) C5S 0.056(3) 0.063(3) 0.085(3) 0.026(2) -0.022(2) -0.018(2) C6S 0.074(3) 0.055(2) 0.090(3) 0.010(2) -0.038(3) -0.018(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 Li1 O1 1.857(5) . ? Li1 O2 1.975(5) . ? Li1 N1 1.999(5) . ? Li1 N2 2.054(5) . ? Li1 C21 2.397(5) . ? Li2 O1 1.860(5) . ? Li2 O4 1.931(4) . ? Li2 O2 1.934(5) . ? Li3 O3 1.844(4) . ? Li3 O2 1.934(4) . ? Li3 O4 1.940(5) . ? Li4 O3 1.852(5) . ? Li4 O4 1.978(4) . ? Li4 N3 2.003(5) . ? Li4 N4 2.046(5) . ? Li4 C55 2.437(5) . ? O1 C1 1.344(3) . ? O2 C21 1.358(3) . ? O3 C35 1.344(3) . ? O4 C55 1.359(3) . ? N1 C16 1.467(3) . ? N1 C17 1.469(3) . ? N1 C15 1.486(3) . ? N2 C19 1.469(3) . ? N2 C18 1.480(3) . ? N2 C20 1.482(3) . ? N3 C50 1.465(3) . ? N3 C51 1.474(3) . ? N3 C49 1.485(3) . ? N4 C53 1.465(3) . ? N4 C52 1.479(3) . ? N4 C54 1.482(3) . ? C1 C6 1.423(3) . ? C1 C2 1.425(4) . ? C2 C3 1.393(3) . ? C2 C7 1.536(3) . ? C3 C4 1.386(3) . ? C3 H3 0.950 . ? C4 C5 1.384(4) . ? C4 C11 1.541(4) . ? C5 C6 1.392(3) . ? C5 H5 0.950 . ? C6 C15 1.508(3) . ? C7 C9 1.530(4) . ? C7 C8 1.535(4) . ? C7 C10 1.535(4) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 C14 1.493(5) . ? C11 C12A 1.497(16) . ? C11 C13A 1.532(15) . ? C11 C12 1.534(5) . ? C11 C13 1.547(5) . ? C11 C14A 1.612(14) . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 C18 1.525(3) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 C26 1.511(3) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C26 1.415(3) . ? C21 C22 1.420(3) . ? C22 C23 1.392(3) . ? C22 C27 1.549(3) . ? C23 C24 1.399(3) . ? C23 H23 0.950 . ? C24 C25 1.381(3) . ? C24 C31 1.534(4) . ? C25 C26 1.390(3) . ? C25 H25 0.950 . ? C27 C28 1.533(4) . ? C27 C29 1.535(3) . ? C27 C30 1.538(4) . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? C29 H29A 0.980 . ? C29 H29B 0.980 . ? C29 H29C 0.980 . ? C30 H30A 0.980 . ? C30 H30B 0.980 . ? C30 H30C 0.980 . ? C31 C32A 1.453(9) . ? C31 C34 1.468(6) . ? C31 C34A 1.499(8) . ? C31 C33 1.500(6) . ? C31 C32 1.601(6) . ? C31 C33A 1.617(9) . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 H34A 0.980 . ? C34 H34B 0.980 . ? C34 H34C 0.980 . ? C35 C40 1.420(3) . ? C35 C36 1.422(4) . ? C36 C37 1.401(3) . ? C36 C41 1.535(4) . ? C37 C38 1.386(4) . ? C37 H37 0.950 . ? C38 C39 1.388(4) . ? C38 C45 1.538(4) . ? C39 C40 1.401(3) . ? C39 H39 0.950 . ? C40 C49 1.502(4) . ? C41 C43 1.533(4) . ? C41 C42 1.535(4) . ? C41 C44 1.536(4) . ? C42 H42A 0.980 . ? C42 H42B 0.980 . ? C42 H42C 0.980 . ? C43 H43A 0.980 . ? C43 H43B 0.980 . ? C43 H43C 0.980 . ? C44 H44A 0.980 . ? C44 H44B 0.980 . ? C44 H44C 0.980 . ? C45 C46 1.529(4) . ? C45 C48 1.533(4) . ? C45 C47 1.537(4) . ? C46 H46A 0.980 . ? C46 H46B 0.980 . ? C46 H46C 0.980 . ? C47 H47A 0.980 . ? C47 H47B 0.980 . ? C47 H47C 0.980 . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C49 H49A 0.990 . ? C49 H49B 0.990 . ? C50 H50A 0.980 . ? C50 H50B 0.980 . ? C50 H50C 0.980 . ? C51 C52 1.517(4) . ? C51 H51A 0.990 . ? C51 H51B 0.990 . ? C52 H52A 0.990 . ? C52 H52B 0.990 . ? C53 H53A 0.980 . ? C53 H53B 0.980 . ? C53 H53C 0.980 . ? C54 C60 1.512(3) . ? C54 H54A 0.990 . ? C54 H54B 0.990 . ? C55 C60 1.409(3) . ? C55 C56 1.420(3) . ? C56 C57 1.393(3) . ? C56 C61 1.547(3) . ? C57 C58 1.392(3) . ? C57 H57 0.950 . ? C58 C59 1.388(3) . ? C58 C65 1.532(4) . ? C59 C60 1.397(3) . ? C59 H59 0.950 . ? C61 C64 1.534(4) . ? C61 C63 1.535(3) . ? C61 C62 1.535(4) . ? C62 H62A 0.980 . ? C62 H62B 0.980 . ? C62 H62C 0.980 . ? C63 H63A 0.980 . ? C63 H63B 0.980 . ? C63 H63C 0.980 . ? C64 H64A 0.980 . ? C64 H64B 0.980 . ? C64 H64C 0.980 . ? C65 C66 1.526(4) . ? C65 C67 1.535(4) . ? C65 C68 1.538(3) . ? C66 H66A 0.980 . ? C66 H66B 0.980 . ? C66 H66C 0.980 . ? C67 H67A 0.980 . ? C67 H67B 0.980 . ? C67 H67C 0.980 . ? C68 H68A 0.980 . ? C68 H68B 0.980 . ? C68 H68C 0.980 . ? C1S C2S 1.459(5) . ? C1S H1S1 0.980 . ? C1S H1S2 0.980 . ? C1S H1S3 0.980 . ? C2S C3S 1.382(5) . ? C2S C7S 1.397(5) . ? C3S C4S 1.372(5) . ? C3S H3S 0.950 . ? C4S C5S 1.400(5) . ? C4S H4S 0.950 . ? C5S C6S 1.352(5) . ? C5S H5S 0.950 . ? C6S C7S 1.394(5) . ? C6S H6S 0.950 . ? C7S H7S 0.950 . ? C8S C12S 1.311(9) . ? C8S C11S 1.439(10) . ? C8S H8S 0.950 . ? C9S C10S 1.336(11) . ? C9S C81S 1.465(10) . ? C9S H9S 0.950 . ? C10S C11S 1.384(11) . ? C10S H10S 0.950 . ? C11S H11S 0.950 . ? C12S C81S 1.401(10) . ? C12S C91S 1.514(10) . ? C81S H81S 0.950 . ? C91S H91A 0.980 . ? C91S H91B 0.980 . ? C91S H91C 0.980 . ? C33A H33D 0.980 . ? C33A H33E 0.980 . ? C33A H33F 0.980 . ? C34A H34D 0.980 . ? C34A H34E 0.980 . ? C34A H34F 0.980 . ? C32A H32D 0.980 . ? C32A H32E 0.980 . ? C32A H32F 0.980 . ? C14A H14D 0.980 . ? C14A H14E 0.980 . ? C14A H14F 0.980 . ? C12A H12D 0.980 . ? C12A H12E 0.980 . ? C12A H12F 0.980 . ? C13A H13D 0.980 . ? C13A H13E 0.980 . ? C13A H13F 0.980 . ? C13S C14S 1.390 . ? C13S C18S 1.390 . ? C13S H13S 0.950 . ? C14S C15S 1.390 . ? C14S H14S 0.950 . ? C15S C16S 1.390 . ? C15S C25S 1.96(2) . ? C16S C17S 1.390 . ? C16S H16S 0.950 . ? C17S C18S 1.390 . ? C17S H17S 0.950 . ? C18S H18S 0.950 . ? C19S C20S 1.390 . ? C19S C24S 1.390 . ? C19S H19S 0.950 . ? C20S C21S 1.390 . ? C20S H20S 0.950 . ? C21S C22S 1.390 . ? C22S C23S 1.390 . ? C22S H22S 0.950 . ? C23S C24S 1.390 . ? C23S H23S 0.950 . ? C24S H24S 0.950 . ? C25S H25A 0.980 . ? C25S H25B 0.980 . ? C25S H25C 0.980 . ? 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 Li1 O2 102.5(2) . . ? O1 Li1 N1 105.4(2) . . ? O2 Li1 N1 137.4(3) . . ? O1 Li1 N2 120.6(2) . . ? O2 Li1 N2 101.8(2) . . ? N1 Li1 N2 90.87(19) . . ? O1 Li1 C21 134.9(2) . . ? O2 Li1 C21 34.49(10) . . ? N1 Li1 C21 106.5(2) . . ? N2 Li1 C21 89.97(18) . . ? O1 Li2 O4 156.5(3) . . ? O1 Li2 O2 104.0(2) . . ? O4 Li2 O2 93.8(2) . . ? O3 Li3 O2 158.7(3) . . ? O3 Li3 O4 103.2(2) . . ? O2 Li3 O4 93.52(19) . . ? O3 Li4 O4 101.5(2) . . ? O3 Li4 N3 105.4(2) . . ? O4 Li4 N3 136.9(3) . . ? O3 Li4 N4 124.6(2) . . ? O4 Li4 N4 101.0(2) . . ? N3 Li4 N4 90.72(19) . . ? O3 Li4 C55 132.8(2) . . ? O4 Li4 C55 33.87(10) . . ? N3 Li4 C55 106.6(2) . . ? N4 Li4 C55 88.67(18) . . ? C1 O1 Li1 118.8(2) . . ? C1 O1 Li2 163.0(2) . . ? Li1 O1 Li2 77.8(2) . . ? C21 O2 Li2 162.34(19) . . ? C21 O2 Li3 111.57(19) . . ? Li2 O2 Li3 86.09(19) . . ? C21 O2 Li1 90.03(18) . . ? Li2 O2 Li1 73.30(19) . . ? Li3 O2 Li1 150.3(2) . . ? C35 O3 Li3 161.7(2) . . ? C35 O3 Li4 118.5(2) . . ? Li3 O3 Li4 79.3(2) . . ? C55 O4 Li2 110.05(19) . . ? C55 O4 Li3 163.32(19) . . ? Li2 O4 Li3 86.01(19) . . ? C55 O4 Li4 91.91(18) . . ? Li2 O4 Li4 153.1(2) . . ? Li3 O4 Li4 74.04(19) . . ? C16 N1 C17 111.47(19) . . ? C16 N1 C15 108.73(19) . . ? C17 N1 C15 113.33(19) . . ? C16 N1 Li1 121.7(2) . . ? C17 N1 Li1 98.68(19) . . ? C15 N1 Li1 102.54(19) . . ? C19 N2 C18 110.7(2) . . ? C19 N2 C20 111.04(19) . . ? C18 N2 C20 113.1(2) . . ? C19 N2 Li1 119.7(2) . . ? C18 N2 Li1 101.52(18) . . ? C20 N2 Li1 100.29(19) . . ? C50 N3 C51 111.3(2) . . ? C50 N3 C49 108.7(2) . . ? C51 N3 C49 113.7(2) . . ? C50 N3 Li4 120.4(2) . . ? C51 N3 Li4 99.22(19) . . ? C49 N3 Li4 103.27(19) . . ? C53 N4 C52 111.0(2) . . ? C53 N4 C54 110.88(19) . . ? C52 N4 C54 112.9(2) . . ? C53 N4 Li4 117.4(2) . . ? C52 N4 Li4 102.30(19) . . ? C54 N4 Li4 101.91(18) . . ? O1 C1 C6 119.4(2) . . ? O1 C1 C2 123.2(2) . . ? C6 C1 C2 117.4(2) . . ? C3 C2 C1 118.6(2) . . ? C3 C2 C7 119.8(2) . . ? C1 C2 C7 121.6(2) . . ? C4 C3 C2 124.5(3) . . ? C4 C3 H3 117.8 . . ? C2 C3 H3 117.8 . . ? C5 C4 C3 116.2(2) . . ? C5 C4 C11 121.3(2) . . ? C3 C4 C11 122.5(3) . . ? C4 C5 C6 122.6(2) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 120.6(2) . . ? C5 C6 C15 117.0(2) . . ? C1 C6 C15 122.4(2) . . ? C9 C7 C8 110.7(2) . . ? C9 C7 C10 106.3(2) . . ? C8 C7 C10 107.0(2) . . ? C9 C7 C2 110.3(2) . . ? C8 C7 C2 109.6(2) . . ? C10 C7 C2 112.9(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12A 130.6(7) . . ? C14 C11 C13A 59.1(7) . . ? C12A C11 C13A 112.5(9) . . ? C14 C11 C12 109.9(4) . . ? C12A C11 C12 43.2(7) . . ? C13A C11 C12 141.6(6) . . ? C14 C11 C4 112.9(3) . . ? C12A C11 C4 115.5(7) . . ? C13A C11 C4 108.0(6) . . ? C12 C11 C4 109.9(3) . . ? C14 C11 C13 108.8(4) . . ? C12A C11 C13 64.5(7) . . ? C13A C11 C13 54.1(6) . . ? C12 C11 C13 107.0(3) . . ? C4 C11 C13 108.2(3) . . ? C14 C11 C14A 48.2(6) . . ? C12A C11 C14A 105.4(9) . . ? C13A C11 C14A 106.3(9) . . ? C12 C11 C14A 66.9(6) . . ? C4 C11 C14A 108.7(5) . . ? C13 C11 C14A 142.2(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? N1 C15 C6 116.2(2) . . ? N1 C15 H15A 108.2 . . ? C6 C15 H15A 108.2 . . ? N1 C15 H15B 108.2 . . ? C6 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 109.5(2) . . ? N1 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? N1 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? N2 C18 C17 109.8(2) . . ? N2 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? N2 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 C26 112.01(19) . . ? N2 C20 H20A 109.2 . . ? C26 C20 H20A 109.2 . . ? N2 C20 H20B 109.2 . . ? C26 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? O2 C21 C26 118.3(2) . . ? O2 C21 C22 122.9(2) . . ? C26 C21 C22 118.8(2) . . ? O2 C21 Li1 55.48(15) . . ? C26 C21 Li1 88.29(19) . . ? C22 C21 Li1 125.66(19) . . ? C23 C22 C21 117.7(2) . . ? C23 C22 C27 119.7(2) . . ? C21 C22 C27 122.6(2) . . ? C22 C23 C24 124.3(2) . . ? C22 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C25 C24 C23 116.6(2) . . ? C25 C24 C31 121.8(2) . . ? C23 C24 C31 121.5(2) . . ? C24 C25 C26 122.1(2) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C21 120.4(2) . . ? C25 C26 C20 119.3(2) . . ? C21 C26 C20 120.2(2) . . ? C28 C27 C29 106.3(2) . . ? C28 C27 C30 107.1(2) . . ? C29 C27 C30 109.5(2) . . ? C28 C27 C22 112.5(2) . . ? C29 C27 C22 111.7(2) . . ? C30 C27 C22 109.5(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32A C31 C34 136.9(5) . . ? C32A C31 C34A 109.4(6) . . ? C34 C31 C34A 46.4(4) . . ? C32A C31 C33 50.9(4) . . ? C34 C31 C33 113.3(4) . . ? C34A C31 C33 132.1(4) . . ? C32A C31 C24 111.1(4) . . ? C34 C31 C24 111.7(3) . . ? C34A C31 C24 113.4(4) . . ? C33 C31 C24 114.5(3) . . ? C32A C31 C32 55.9(5) . . ? C34 C31 C32 106.0(4) . . ? C34A C31 C32 60.8(4) . . ? C33 C31 C32 104.3(4) . . ? C24 C31 C32 106.1(3) . . ? C32A C31 C33A 111.9(6) . . ? C34 C31 C33A 61.6(4) . . ? C34A C31 C33A 106.2(5) . . ? C33 C31 C33A 62.0(4) . . ? C24 C31 C33A 104.7(4) . . ? C32 C31 C33A 149.2(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? O3 C35 C40 119.2(2) . . ? O3 C35 C36 122.8(2) . . ? C40 C35 C36 118.0(2) . . ? C37 C36 C35 118.4(2) . . ? C37 C36 C41 119.8(2) . . ? C35 C36 C41 121.8(2) . . ? C38 C37 C36 124.7(3) . . ? C38 C37 H37 117.6 . . ? C36 C37 H37 117.6 . . ? C37 C38 C39 115.8(2) . . ? C37 C38 C45 123.1(3) . . ? C39 C38 C45 121.1(2) . . ? C38 C39 C40 123.1(2) . . ? C38 C39 H39 118.5 . . ? C40 C39 H39 118.5 . . ? C39 C40 C35 120.0(2) . . ? C39 C40 C49 117.0(2) . . ? C35 C40 C49 122.7(2) . . ? C43 C41 C42 110.6(2) . . ? C43 C41 C36 110.1(2) . . ? C42 C41 C36 109.1(2) . . ? C43 C41 C44 106.8(2) . . ? C42 C41 C44 106.8(2) . . ? C36 C41 C44 113.3(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C48 108.3(2) . . ? C46 C45 C47 108.1(3) . . ? C48 C45 C47 108.8(2) . . ? C46 C45 C38 112.2(2) . . ? C48 C45 C38 109.6(2) . . ? C47 C45 C38 109.7(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N3 C49 C40 115.9(2) . . ? N3 C49 H49A 108.3 . . ? C40 C49 H49A 108.3 . . ? N3 C49 H49B 108.3 . . ? C40 C49 H49B 108.3 . . ? H49A C49 H49B 107.4 . . ? N3 C50 H50A 109.5 . . ? N3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C51 C52 110.1(2) . . ? N3 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? N3 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? N4 C52 C51 110.4(2) . . ? N4 C52 H52A 109.6 . . ? C51 C52 H52A 109.6 . . ? N4 C52 H52B 109.6 . . ? C51 C52 H52B 109.6 . . ? H52A C52 H52B 108.1 . . ? N4 C53 H53A 109.5 . . ? N4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C54 C60 111.6(2) . . ? N4 C54 H54A 109.3 . . ? C60 C54 H54A 109.3 . . ? N4 C54 H54B 109.3 . . ? C60 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? O4 C55 C60 118.4(2) . . ? O4 C55 C56 122.3(2) . . ? C60 C55 C56 119.2(2) . . ? O4 C55 Li4 54.22(15) . . ? C60 C55 Li4 88.46(18) . . ? C56 C55 Li4 126.9(2) . . ? C57 C56 C55 117.5(2) . . ? C57 C56 C61 120.3(2) . . ? C55 C56 C61 122.2(2) . . ? C58 C57 C56 124.6(2) . . ? C58 C57 H57 117.7 . . ? C56 C57 H57 117.7 . . ? C59 C58 C57 116.4(2) . . ? C59 C58 C65 120.4(2) . . ? C57 C58 C65 123.2(2) . . ? C58 C59 C60 122.1(2) . . ? C58 C59 H59 118.9 . . ? C60 C59 H59 118.9 . . ? C59 C60 C55 120.0(2) . . ? C59 C60 C54 119.5(2) . . ? C55 C60 C54 120.5(2) . . ? C64 C61 C63 108.6(2) . . ? C64 C61 C62 107.4(2) . . ? C63 C61 C62 106.3(2) . . ? C64 C61 C56 109.9(2) . . ? C63 C61 C56 112.2(2) . . ? C62 C61 C56 112.3(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C58 112.6(2) . . ? C66 C65 C67 108.4(2) . . ? C58 C65 C67 109.3(2) . . ? C66 C65 C68 107.9(2) . . ? C58 C65 C68 109.5(2) . . ? C67 C65 C68 109.0(2) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3S C2S C7S 117.6(4) . . ? C3S C2S C1S 119.7(4) . . ? C7S C2S C1S 122.7(3) . . ? C4S C3S C2S 120.6(4) . . ? C4S C3S H3S 119.7 . . ? C2S C3S H3S 119.7 . . ? C3S C4S C5S 121.7(4) . . ? C3S C4S H4S 119.2 . . ? C5S C4S H4S 119.2 . . ? C6S C5S C4S 118.0(4) . . ? C6S C5S H5S 121.0 . . ? C4S C5S H5S 121.0 . . ? C5S C6S C7S 121.0(4) . . ? C5S C6S H6S 119.5 . . ? C7S C6S H6S 119.5 . . ? C6S C7S C2S 121.1(4) . . ? C6S C7S H7S 119.5 . . ? C2S C7S H7S 119.5 . . ? C12S C8S C11S 121.6(7) . . ? C12S C8S H8S 119.2 . . ? C11S C8S H8S 119.2 . . ? C10S C9S C81S 123.3(7) . . ? C10S C9S H9S 118.3 . . ? C81S C9S H9S 118.3 . . ? C9S C10S C11S 120.4(9) . . ? C9S C10S H10S 119.8 . . ? C11S C10S H10S 119.8 . . ? C10S C11S C8S 117.4(7) . . ? C10S C11S H11S 121.3 . . ? C8S C11S H11S 121.3 . . ? C8S C12S C81S 123.5(7) . . ? C8S C12S C91S 122.5(7) . . ? C81S C12S C91S 114.0(7) . . ? C12S C81S C9S 113.6(7) . . ? C12S C81S H81S 123.2 . . ? C9S C81S H81S 123.2 . . ? C12S C91S H91A 109.5 . . ? C12S C91S H91B 109.5 . . ? H91A C91S H91B 109.5 . . ? C12S C91S H91C 109.5 . . ? H91A C91S H91C 109.5 . . ? H91B C91S H91C 109.5 . . ? C31 C33A H33D 109.5 . . ? C31 C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31 C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C31 C34A H34D 109.5 . . ? C31 C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? C31 C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C31 C32A H32D 109.5 . . ? C31 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C11 C14A H14D 109.5 . . ? C11 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C11 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C11 C12A H12D 109.5 . . ? C11 C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11 C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11 C13A H13D 109.5 . . ? C11 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C11 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C14S C13S C18S 120.0 . . ? C14S C13S H13S 120.0 . . ? C18S C13S H13S 120.0 . . ? C13S C14S C15S 120.0 . . ? C13S C14S H14S 120.0 . . ? C15S C14S H14S 120.0 . . ? C16S C15S C14S 120.0 . . ? C16S C15S C25S 123.7(7) . . ? C14S C15S C25S 116.3(7) . . ? C15S C16S C17S 120.0 . . ? C15S C16S H16S 120.0 . . ? C17S C16S H16S 120.0 . . ? C18S C17S C16S 120.0 . . ? C18S C17S H17S 120.0 . . ? C16S C17S H17S 120.0 . . ? C17S C18S C13S 120.0 . . ? C17S C18S H18S 120.0 . . ? C13S C18S H18S 120.0 . . ? C20S C19S C24S 120.0 . . ? C20S C19S H19S 120.0 . . ? C24S C19S H19S 120.0 . . ? C21S C20S C19S 120.0 . . ? C21S C20S H20S 120.0 . . ? C19S C20S H20S 120.0 . . ? C20S C21S C22S 120.0 . . ? C23S C22S C21S 120.0 . . ? C23S C22S H22S 120.0 . . ? C21S C22S H22S 120.0 . . ? C22S C23S C24S 120.0 . . ? C22S C23S H23S 120.0 . . ? C24S C23S H23S 120.0 . . ? C23S C24S C19S 120.0 . . ? C23S C24S H24S 120.0 . . ? C19S C24S H24S 120.0 . . ? C15S C25S H25A 109.5 . . ? C15S C25S H25B 109.5 . . ? H25A C25S H25B 109.5 . . ? C15S C25S H25C 109.5 . . ? H25A C25S H25C 109.5 . . ? H25B C25S H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.334 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.046 #===END #--------------------------------------------------------------- #----------------COMPOUND 2 ----------------------------------- #--------------------------------------------------------------- data_rem387 _database_code_depnum_ccdc_archive 'CCDC 669062' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H46 Li2 N4 O2' _chemical_formula_sum 'C28 H46 Li2 N4 O2' _chemical_formula_weight 484.57 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.151(3) _cell_length_b 15.012(3) _cell_length_c 16.937(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.913(3) _cell_angle_gamma 90.00 _cell_volume 2904.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.947 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25601 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7055 _reflns_number_gt 5988 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.5' _computing_publication_material ? _refine_special_details ; The following restraints were applied to the disordered TMEDA ligand: similarity of bond lengths and angles for the two components [SAME] similarity of displacement parameters for atoms close together [SIMU] approximate 'rigid bond' restraints on displacement parameters [DELU] approximate isotropic behaviour for displacement parameters [ISOR] ; _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^)+(0.0737P)^2^+0.9276P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7055 _refine_ls_number_parameters 412 _refine_ls_number_restraints 358 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.055 _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 Li1 Li 0.47415(18) 0.49035(14) 0.23198(14) 0.0301(4) Uani 1 1 d . A . Li2 Li 0.28510(16) 0.50152(13) 0.24936(12) 0.0257(4) Uani 1 1 d . . . O3 O 0.39584(7) 0.40521(5) 0.27204(6) 0.02840(19) Uani 1 1 d . A . C4 C 0.47133(9) 0.34284(7) 0.31122(7) 0.0222(2) Uani 1 1 d . . . C5 C 0.47968(10) 0.31379(8) 0.39280(7) 0.0260(2) Uani 1 1 d . A . C6 C 0.56293(11) 0.25101(8) 0.43482(7) 0.0285(2) Uani 1 1 d . . . H6 H 0.5668 0.2329 0.4895 0.034 Uiso 1 1 calc R A . C7 C 0.64099(10) 0.21346(8) 0.40015(8) 0.0282(2) Uani 1 1 d . A . C8 C 0.63075(10) 0.24021(7) 0.31947(7) 0.0247(2) Uani 1 1 d . . . H8 H 0.6817 0.2147 0.2938 0.030 Uiso 1 1 calc R A . C9 C 0.54857(9) 0.30302(7) 0.27458(7) 0.0218(2) Uani 1 1 d . A . C10 C 0.54143(10) 0.32719(8) 0.18651(7) 0.0260(2) Uani 1 1 d . . . H10A H 0.5950 0.2881 0.1694 0.031 Uiso 1 1 calc R A . H10B H 0.4609 0.3159 0.1478 0.031 Uiso 1 1 calc R . . N11 N 0.57214(8) 0.42132(6) 0.17791(6) 0.0232(2) Uani 1 1 d . A . C12 C 0.69340(9) 0.44369(7) 0.22811(7) 0.0243(2) Uani 1 1 d . . . H12A H 0.7450 0.4326 0.1948 0.029 Uiso 1 1 calc R A . H12B H 0.7200 0.4054 0.2787 0.029 Uiso 1 1 calc R . . C13 C 0.70163(10) 0.54150(8) 0.25430(7) 0.0253(2) Uani 1 1 d . A . H13A H 0.7829 0.5556 0.2901 0.030 Uiso 1 1 calc R . . H13B H 0.6809 0.5799 0.2038 0.030 Uiso 1 1 calc R . . N14 N 0.62175(9) 0.55939(6) 0.30083(6) 0.0254(2) Uani 1 1 d . . . C15 C 0.58510(11) 0.65377(8) 0.29677(8) 0.0303(3) Uani 1 1 d . A . H15A H 0.6558 0.6915 0.3192 0.036 Uiso 1 1 calc R . . H15B H 0.5374 0.6620 0.3334 0.036 Uiso 1 1 calc R . . C16 C 0.51536(10) 0.68521(7) 0.20946(7) 0.0252(2) Uani 1 1 d . . . C17 C 0.55770(10) 0.75488(8) 0.17359(9) 0.0307(3) Uani 1 1 d . A . H17 H 0.6315 0.7802 0.2044 0.037 Uiso 1 1 calc R . . C18 C 0.49634(11) 0.78870(8) 0.09462(9) 0.0347(3) Uani 1 1 d . . . C19 C 0.38843(11) 0.74970(8) 0.05114(8) 0.0325(3) Uani 1 1 d . A . H19 H 0.3447 0.7716 -0.0031 0.039 Uiso 1 1 calc R . . C20 C 0.34242(10) 0.68007(8) 0.08413(8) 0.0278(2) Uani 1 1 d . . . C21 C 0.40506(9) 0.64596(7) 0.16503(7) 0.0237(2) Uani 1 1 d . A . O22 O 0.36269(7) 0.57929(6) 0.19677(6) 0.0291(2) Uani 1 1 d . A . C23 C 0.39966(14) 0.35477(10) 0.43347(9) 0.0406(3) Uani 1 1 d . . . H23A H 0.4147 0.3280 0.4889 0.061 Uiso 1 1 calc R A . H23B H 0.3181 0.3440 0.3984 0.061 Uiso 1 1 calc R . . H23C H 0.4140 0.4191 0.4396 0.061 Uiso 1 1 calc R . . C24 C 0.73343(13) 0.14720(10) 0.44794(10) 0.0433(3) Uani 1 1 d . . . H24A H 0.7117 0.0876 0.4242 0.065 Uiso 1 1 calc R A . H24B H 0.7395 0.1470 0.5071 0.065 Uiso 1 1 calc R . . H24C H 0.8090 0.1641 0.4435 0.065 Uiso 1 1 calc R . . C25 C 0.54484(14) 0.44494(10) 0.08935(8) 0.0391(3) Uani 1 1 d . . . H25A H 0.5657 0.5074 0.0851 0.059 Uiso 1 1 calc R A . H25B H 0.4609 0.4366 0.0593 0.059 Uiso 1 1 calc R . . H25C H 0.5896 0.4066 0.0644 0.059 Uiso 1 1 calc R . . C26 C 0.67100(14) 0.52993(10) 0.38823(8) 0.0397(3) Uani 1 1 d . A . H26A H 0.6916 0.4667 0.3898 0.060 Uiso 1 1 calc R . . H26B H 0.6131 0.5386 0.4161 0.060 Uiso 1 1 calc R . . H26C H 0.7413 0.5648 0.4173 0.060 Uiso 1 1 calc R . . C27 C 0.54495(15) 0.86402(11) 0.05704(12) 0.0546(4) Uani 1 1 d . A . H27A H 0.5491 0.9183 0.0901 0.082 Uiso 1 1 calc R . . H27B H 0.4937 0.8743 -0.0010 0.082 Uiso 1 1 calc R . . H27C H 0.6235 0.8483 0.0577 0.082 Uiso 1 1 calc R . . C28 C 0.22673(12) 0.63918(10) 0.03472(10) 0.0405(3) Uani 1 1 d . A . H28A H 0.1983 0.6651 -0.0218 0.061 Uiso 1 1 calc R . . H28B H 0.1701 0.6510 0.0630 0.061 Uiso 1 1 calc R . . H28C H 0.2362 0.5747 0.0306 0.061 Uiso 1 1 calc R . . N29 N 0.1095(15) 0.4599(7) 0.1935(7) 0.0308(17) Uani 0.411(5) 1 d PDU A 1 C30 C 0.0399(3) 0.5321(3) 0.2133(3) 0.0479(11) Uani 0.411(5) 1 d PDU A 1 H30A H 0.0166 0.5737 0.1651 0.058 Uiso 0.411(5) 1 calc PR A 1 H30B H -0.0329 0.5050 0.2163 0.058 Uiso 0.411(5) 1 calc PR A 1 C31 C 0.0855(5) 0.5799(3) 0.2814(3) 0.0349(11) Uani 0.411(5) 1 d PDU A 1 H31A H 0.0501 0.5578 0.3224 0.042 Uiso 0.411(5) 1 calc PR A 1 H31B H 0.0560 0.6413 0.2667 0.042 Uiso 0.411(5) 1 calc PR A 1 N32 N 0.2105(10) 0.5878(9) 0.3270(7) 0.0289(16) Uani 0.411(5) 1 d PDU A 1 C33 C 0.0906(5) 0.3751(3) 0.2284(4) 0.0528(12) Uani 0.411(5) 1 d PDU A 1 H33A H 0.0094 0.3561 0.2008 0.079 Uiso 0.411(5) 1 calc PR A 1 H33B H 0.1061 0.3818 0.2888 0.079 Uiso 0.411(5) 1 calc PR A 1 H33C H 0.1436 0.3302 0.2192 0.079 Uiso 0.411(5) 1 calc PR A 1 C34 C 0.0747(6) 0.4504(5) 0.1029(3) 0.0615(16) Uani 0.411(5) 1 d PDU A 1 H34A H 0.1235 0.4051 0.0894 0.092 Uiso 0.411(5) 1 calc PR A 1 H34B H 0.0846 0.5075 0.0780 0.092 Uiso 0.411(5) 1 calc PR A 1 H34C H -0.0076 0.4322 0.0802 0.092 Uiso 0.411(5) 1 calc PR A 1 C35 C 0.2507(8) 0.6798(6) 0.3225(5) 0.0363(13) Uani 0.411(5) 1 d PDU A 1 H35A H 0.2082 0.7207 0.3470 0.054 Uiso 0.411(5) 1 calc PR A 1 H35B H 0.2358 0.6959 0.2637 0.054 Uiso 0.411(5) 1 calc PR A 1 H35C H 0.3348 0.6839 0.3539 0.054 Uiso 0.411(5) 1 calc PR A 1 C36 C 0.2415(9) 0.5630(8) 0.4149(6) 0.0419(17) Uani 0.411(5) 1 d PDU A 1 H36A H 0.2086 0.6066 0.4438 0.063 Uiso 0.411(5) 1 calc PR A 1 H36B H 0.3269 0.5620 0.4411 0.063 Uiso 0.411(5) 1 calc PR A 1 H36C H 0.2099 0.5038 0.4190 0.063 Uiso 0.411(5) 1 calc PR A 1 N29A N 0.1072(10) 0.4544(5) 0.1962(5) 0.0287(12) Uani 0.589(5) 1 d PDU A 2 C30A C 0.0526(2) 0.4856(2) 0.25604(19) 0.0428(7) Uani 0.589(5) 1 d PDU A 2 H30C H -0.0312 0.4958 0.2238 0.051 Uiso 0.589(5) 1 calc PR A 2 H30D H 0.0562 0.4357 0.2950 0.051 Uiso 0.589(5) 1 calc PR A 2 C31A C 0.0916(5) 0.5582(4) 0.3033(4) 0.0654(13) Uani 0.589(5) 1 d PDU A 2 H31C H 0.0724 0.5510 0.3552 0.078 Uiso 0.589(5) 1 calc PR A 2 H31D H 0.0457 0.6096 0.2726 0.078 Uiso 0.589(5) 1 calc PR A 2 N32A N 0.2159(7) 0.5826(6) 0.3286(5) 0.0337(15) Uani 0.589(5) 1 d PDU A 2 C33A C 0.1099(3) 0.35700(19) 0.1933(2) 0.0451(7) Uani 0.589(5) 1 d PDU A 2 H33D H 0.0296 0.3340 0.1733 0.068 Uiso 0.589(5) 1 calc PR A 2 H33E H 0.1516 0.3337 0.2496 0.068 Uiso 0.589(5) 1 calc PR A 2 H33F H 0.1503 0.3381 0.1549 0.068 Uiso 0.589(5) 1 calc PR A 2 C34A C 0.0473(3) 0.4878(2) 0.1115(2) 0.0435(8) Uani 0.589(5) 1 d PDU A 2 H34D H -0.0330 0.4648 0.0908 0.065 Uiso 0.589(5) 1 calc PR A 2 H34E H 0.0891 0.4680 0.0743 0.065 Uiso 0.589(5) 1 calc PR A 2 H34F H 0.0455 0.5531 0.1125 0.065 Uiso 0.589(5) 1 calc PR A 2 C35A C 0.2270(7) 0.6726(5) 0.3006(4) 0.0598(16) Uani 0.589(5) 1 d PDU A 2 H35D H 0.1895 0.7145 0.3279 0.090 Uiso 0.589(5) 1 calc PR A 2 H35E H 0.1889 0.6762 0.2395 0.090 Uiso 0.589(5) 1 calc PR A 2 H35F H 0.3100 0.6877 0.3154 0.090 Uiso 0.589(5) 1 calc PR A 2 C36A C 0.2680(7) 0.5791(7) 0.4197(5) 0.062(2) Uani 0.589(5) 1 d PDU A 2 H36D H 0.3524 0.5897 0.4363 0.093 Uiso 0.589(5) 1 calc PR A 2 H36E H 0.2540 0.5203 0.4396 0.093 Uiso 0.589(5) 1 calc PR A 2 H36F H 0.2325 0.6251 0.4445 0.093 Uiso 0.589(5) 1 calc PR A 2 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 Li1 0.0252(9) 0.0248(9) 0.0439(12) 0.0077(8) 0.0166(9) 0.0032(8) Li2 0.0212(9) 0.0268(9) 0.0304(10) 0.0039(8) 0.0106(7) 0.0018(7) O3 0.0226(4) 0.0252(4) 0.0396(5) 0.0111(3) 0.0134(3) 0.0064(3) C4 0.0193(5) 0.0183(5) 0.0290(5) 0.0029(4) 0.0085(4) 0.0001(4) C5 0.0287(5) 0.0222(5) 0.0308(6) 0.0024(4) 0.0148(5) 0.0010(4) C6 0.0329(6) 0.0257(5) 0.0264(5) 0.0046(4) 0.0094(5) 0.0005(4) C7 0.0245(5) 0.0229(5) 0.0338(6) 0.0049(4) 0.0057(4) 0.0030(4) C8 0.0217(5) 0.0195(5) 0.0342(6) -0.0005(4) 0.0112(4) 0.0010(4) C9 0.0207(5) 0.0188(5) 0.0261(5) 0.0001(4) 0.0082(4) -0.0025(4) C10 0.0294(6) 0.0237(5) 0.0257(5) -0.0020(4) 0.0107(4) -0.0039(4) N11 0.0233(4) 0.0246(5) 0.0215(4) 0.0020(3) 0.0073(3) -0.0030(4) C12 0.0193(5) 0.0251(5) 0.0302(5) 0.0002(4) 0.0107(4) 0.0007(4) C13 0.0199(5) 0.0254(5) 0.0301(6) 0.0007(4) 0.0082(4) -0.0012(4) N14 0.0281(5) 0.0250(5) 0.0230(4) 0.0013(4) 0.0085(4) 0.0050(4) C15 0.0334(6) 0.0249(6) 0.0300(6) -0.0034(4) 0.0073(5) 0.0042(5) C16 0.0244(5) 0.0199(5) 0.0314(6) -0.0001(4) 0.0096(4) 0.0030(4) C17 0.0225(5) 0.0223(5) 0.0462(7) 0.0008(5) 0.0103(5) -0.0020(4) C18 0.0305(6) 0.0270(6) 0.0494(8) 0.0105(5) 0.0171(6) -0.0016(5) C19 0.0295(6) 0.0301(6) 0.0369(6) 0.0110(5) 0.0102(5) 0.0019(5) C20 0.0224(5) 0.0243(5) 0.0359(6) 0.0046(4) 0.0089(5) 0.0010(4) C21 0.0222(5) 0.0186(5) 0.0333(6) 0.0034(4) 0.0135(4) 0.0029(4) O22 0.0249(4) 0.0241(4) 0.0420(5) 0.0100(3) 0.0165(4) 0.0023(3) C23 0.0524(8) 0.0361(7) 0.0455(8) 0.0074(6) 0.0326(7) 0.0106(6) C24 0.0364(7) 0.0405(7) 0.0486(8) 0.0155(6) 0.0088(6) 0.0144(6) C25 0.0496(8) 0.0424(7) 0.0236(6) 0.0043(5) 0.0102(5) -0.0120(6) C26 0.0518(8) 0.0400(7) 0.0246(6) 0.0036(5) 0.0095(6) 0.0110(6) C27 0.0448(8) 0.0464(9) 0.0736(11) 0.0253(8) 0.0214(8) -0.0096(7) C28 0.0283(6) 0.0371(7) 0.0478(8) 0.0091(6) 0.0020(6) -0.0052(5) N29 0.031(3) 0.025(2) 0.038(3) 0.000(2) 0.015(2) -0.006(2) C30 0.0241(14) 0.049(2) 0.062(2) -0.0032(18) 0.0032(14) 0.0061(14) C31 0.0209(15) 0.0330(17) 0.048(2) 0.0042(15) 0.0088(16) 0.0183(13) N32 0.030(3) 0.034(3) 0.026(3) -0.001(2) 0.015(2) 0.012(2) C33 0.056(3) 0.038(2) 0.060(3) 0.009(2) 0.013(2) -0.0141(19) C34 0.067(4) 0.073(4) 0.041(2) -0.007(3) 0.014(2) -0.034(3) C35 0.038(2) 0.028(2) 0.042(3) -0.005(2) 0.013(2) 0.0009(16) C36 0.048(3) 0.052(4) 0.031(3) 0.005(3) 0.021(2) 0.018(3) N29A 0.0224(19) 0.031(2) 0.0315(18) 0.0022(16) 0.0078(15) -0.0045(17) C30A 0.0277(11) 0.0514(15) 0.0563(15) -0.0026(12) 0.0233(10) -0.0068(10) C31A 0.0420(19) 0.086(3) 0.077(3) -0.028(2) 0.032(2) -0.003(2) N32A 0.029(2) 0.033(2) 0.036(2) -0.0017(17) 0.0071(17) 0.0042(18) C33A 0.0506(16) 0.0293(13) 0.0530(19) 0.0039(12) 0.0145(14) -0.0078(11) C34A 0.0345(14) 0.0426(17) 0.0440(16) 0.0107(14) 0.0013(11) -0.0049(12) C35A 0.080(4) 0.039(2) 0.071(4) 0.006(2) 0.039(3) 0.026(2) C36A 0.081(4) 0.060(4) 0.038(2) -0.0070(19) 0.012(3) 0.025(3) _geom_special_details ; ; 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 Li1 O3 1.854(2) . ? Li1 N11 2.018(2) . ? Li1 N14 2.056(2) . ? Li1 O22 1.850(2) . ? Li2 O3 1.923(2) . ? Li2 O22 1.902(2) . ? Li2 N29 2.112(17) . ? Li2 N32 2.245(13) . ? Li2 N29A 2.158(11) . ? Li2 N32A 2.182(11) . ? O3 C4 1.3206(13) . ? C4 C5 1.4191(15) . ? C4 C9 1.4213(15) . ? C5 C6 1.3884(16) . ? C5 C23 1.5014(17) . ? C6 H6 0.950 . ? C6 C7 1.3934(17) . ? C7 C8 1.3885(17) . ? C7 C24 1.5122(17) . ? C8 H8 0.950 . ? C8 C9 1.3954(15) . ? C9 C10 1.5087(15) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 N11 1.4814(14) . ? N11 C12 1.4674(14) . ? N11 C25 1.4651(15) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C12 C13 1.5273(16) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 N14 1.4684(15) . ? N14 C15 1.4798(15) . ? N14 C26 1.4634(15) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.5080(16) . ? C16 C17 1.3931(16) . ? C16 C21 1.4221(16) . ? C17 H17 0.950 . ? C17 C18 1.3868(19) . ? C18 C19 1.3952(18) . ? C18 C27 1.5128(18) . ? C19 H19 0.950 . ? C19 C20 1.3893(16) . ? C20 C21 1.4173(16) . ? C20 C28 1.5006(17) . ? C21 O22 1.3208(13) . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C27 H27A 0.980 . ? C27 H27B 0.980 . ? C27 H27C 0.980 . ? C28 H28A 0.980 . ? C28 H28B 0.980 . ? C28 H28C 0.980 . ? N29 C30 1.482(11) . ? N29 C33 1.455(12) . ? N29 C34 1.454(11) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C30 C31 1.310(7) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C31 N32 1.455(10) . ? N32 C35 1.476(11) . ? N32 C36 1.455(10) . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 H34A 0.980 . ? C34 H34B 0.980 . ? C34 H34C 0.980 . ? C35 H35A 0.980 . ? C35 H35B 0.980 . ? C35 H35C 0.980 . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? N29A C30A 1.464(8) . ? N29A C33A 1.464(7) . ? N29A C34A 1.459(8) . ? C30A H30C 0.990 . ? C30A H30D 0.990 . ? C30A C31A 1.340(5) . ? C31A H31C 0.990 . ? C31A H31D 0.990 . ? C31A N32A 1.469(8) . ? N32A C35A 1.453(8) . ? N32A C36A 1.456(8) . ? C33A H33D 0.980 . ? C33A H33E 0.980 . ? C33A H33F 0.980 . ? C34A H34D 0.980 . ? C34A H34E 0.980 . ? C34A H34F 0.980 . ? C35A H35D 0.980 . ? C35A H35E 0.980 . ? C35A H35F 0.980 . ? C36A H36D 0.980 . ? C36A H36E 0.980 . ? C36A H36F 0.980 . ? 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 O3 Li1 N11 105.52(10) . . ? O3 Li1 N14 126.67(12) . . ? O3 Li1 O22 101.82(10) . . ? N11 Li1 N14 88.90(9) . . ? N11 Li1 O22 134.80(13) . . ? N14 Li1 O22 102.74(10) . . ? O3 Li2 O22 97.49(9) . . ? O3 Li2 N29 113.5(3) . . ? O3 Li2 N32 135.4(3) . . ? O3 Li2 N29A 111.7(2) . . ? O3 Li2 N32A 133.4(3) . . ? O22 Li2 N29 123.9(3) . . ? O22 Li2 N32 106.5(3) . . ? O22 Li2 N29A 126.3(2) . . ? O22 Li2 N32A 107.6(2) . . ? N29 Li2 N32 83.4(4) . . ? N29A Li2 N32A 84.1(3) . . ? Li1 O3 Li2 79.63(9) . . ? Li1 O3 C4 108.52(9) . . ? Li2 O3 C4 162.30(10) . . ? O3 C4 C5 120.95(10) . . ? O3 C4 C9 121.84(10) . . ? C5 C4 C9 117.20(10) . . ? C4 C5 C6 120.37(10) . . ? C4 C5 C23 118.55(10) . . ? C6 C5 C23 121.04(11) . . ? C5 C6 H6 118.6 . . ? C5 C6 C7 122.71(11) . . ? H6 C6 C7 118.6 . . ? C6 C7 C8 116.87(10) . . ? C6 C7 C24 121.91(12) . . ? C8 C7 C24 121.21(11) . . ? C7 C8 H8 118.7 . . ? C7 C8 C9 122.63(10) . . ? H8 C8 C9 118.7 . . ? C4 C9 C8 120.18(10) . . ? C4 C9 C10 120.43(10) . . ? C8 C9 C10 119.39(10) . . ? C9 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C9 C10 N11 113.27(9) . . ? H10A C10 H10B 107.7 . . ? H10A C10 N11 108.9 . . ? H10B C10 N11 108.9 . . ? Li1 N11 C10 103.77(9) . . ? Li1 N11 C12 104.52(9) . . ? Li1 N11 C25 112.17(10) . . ? C10 N11 C12 113.46(9) . . ? C10 N11 C25 110.78(9) . . ? C12 N11 C25 111.73(9) . . ? N11 C12 H12A 109.7 . . ? N11 C12 H12B 109.7 . . ? N11 C12 C13 109.99(9) . . ? H12A C12 H12B 108.2 . . ? H12A C12 C13 109.7 . . ? H12B C12 C13 109.7 . . ? C12 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C12 C13 N14 109.99(9) . . ? H13A C13 H13B 108.2 . . ? H13A C13 N14 109.7 . . ? H13B C13 N14 109.7 . . ? Li1 N14 C13 102.23(9) . . ? Li1 N14 C15 105.42(9) . . ? Li1 N14 C26 113.49(10) . . ? C13 N14 C15 113.18(10) . . ? C13 N14 C26 111.73(10) . . ? C15 N14 C26 110.45(10) . . ? N14 C15 H15A 108.8 . . ? N14 C15 H15B 108.8 . . ? N14 C15 C16 113.89(9) . . ? H15A C15 H15B 107.7 . . ? H15A C15 C16 108.8 . . ? H15B C15 C16 108.8 . . ? C15 C16 C17 119.67(11) . . ? C15 C16 C21 120.18(10) . . ? C17 C16 C21 120.12(11) . . ? C16 C17 H17 118.7 . . ? C16 C17 C18 122.57(11) . . ? H17 C17 C18 118.7 . . ? C17 C18 C19 117.09(11) . . ? C17 C18 C27 121.38(13) . . ? C19 C18 C27 121.53(13) . . ? C18 C19 H19 118.7 . . ? C18 C19 C20 122.54(12) . . ? H19 C19 C20 118.7 . . ? C19 C20 C21 120.23(11) . . ? C19 C20 C28 120.82(11) . . ? C21 C20 C28 118.95(11) . . ? C16 C21 C20 117.44(10) . . ? C16 C21 O22 121.76(10) . . ? C20 C21 O22 120.79(10) . . ? Li1 O22 Li2 80.28(9) . . ? Li1 O22 C21 109.51(9) . . ? Li2 O22 C21 168.51(10) . . ? C5 C23 H23A 109.5 . . ? C5 C23 H23B 109.5 . . ? C5 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C7 C24 H24A 109.5 . . ? C7 C24 H24B 109.5 . . ? C7 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N11 C25 H25A 109.5 . . ? N11 C25 H25B 109.5 . . ? N11 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N14 C26 H26A 109.5 . . ? N14 C26 H26B 109.5 . . ? N14 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C18 C27 H27A 109.5 . . ? C18 C27 H27B 109.5 . . ? C18 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Li2 N29 C30 104.5(7) . . ? Li2 N29 C33 110.6(8) . . ? Li2 N29 C34 112.9(9) . . ? C30 N29 C33 111.5(10) . . ? C30 N29 C34 109.1(9) . . ? C33 N29 C34 108.2(8) . . ? N29 C30 H30A 107.4 . . ? N29 C30 H30B 107.4 . . ? N29 C30 C31 119.8(7) . . ? H30A C30 H30B 106.9 . . ? H30A C30 C31 107.4 . . ? H30B C30 C31 107.4 . . ? C30 C31 H31A 106.3 . . ? C30 C31 H31B 106.3 . . ? C30 C31 N32 124.3(7) . . ? H31A C31 H31B 106.4 . . ? H31A C31 N32 106.3 . . ? H31B C31 N32 106.2 . . ? Li2 N32 C31 101.5(6) . . ? Li2 N32 C35 107.7(7) . . ? Li2 N32 C36 115.9(9) . . ? C31 N32 C35 110.7(9) . . ? C31 N32 C36 112.4(8) . . ? C35 N32 C36 108.5(8) . . ? Li2 N29A C30A 103.4(4) . . ? Li2 N29A C33A 108.1(5) . . ? Li2 N29A C34A 113.0(6) . . ? C30A N29A C33A 111.3(6) . . ? C30A N29A C34A 112.2(6) . . ? C33A N29A C34A 108.6(5) . . ? N29A C30A H30C 107.0 . . ? N29A C30A H30D 107.0 . . ? N29A C30A C31A 121.5(5) . . ? H30C C30A H30D 106.7 . . ? H30C C30A C31A 107.0 . . ? H30D C30A C31A 107.0 . . ? C30A C31A H31C 107.4 . . ? C30A C31A H31D 107.4 . . ? C30A C31A N32A 119.7(5) . . ? H31C C31A H31D 106.9 . . ? H31C C31A N32A 107.4 . . ? H31D C31A N32A 107.4 . . ? Li2 N32A C31A 104.8(5) . . ? Li2 N32A C35A 102.7(6) . . ? Li2 N32A C36A 120.8(7) . . ? C31A N32A C35A 109.7(7) . . ? C31A N32A C36A 109.4(7) . . ? C35A N32A C36A 108.9(7) . . ? N29A C33A H33D 109.5 . . ? N29A C33A H33E 109.5 . . ? N29A C33A H33F 109.5 . . ? H33D C33A H33E 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? N29A C34A H34D 109.5 . . ? N29A C34A H34E 109.5 . . ? N29A C34A H34F 109.5 . . ? H34D C34A H34E 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? N32A C35A H35D 109.5 . . ? N32A C35A H35E 109.5 . . ? N32A C35A H35F 109.5 . . ? H35D C35A H35E 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? N32A C36A H36D 109.5 . . ? N32A C36A H36E 109.5 . . ? N32A C36A H36F 109.5 . . ? H36D C36A H36E 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.400 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.055 #===END #--------------------------------------------------------------- #----------------COMPOUND 3----------------------------------- #--------------------------------------------------------------- data_dvgcoh2 _database_code_depnum_ccdc_archive 'CCDC 669063' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H80 N4 Na4 O6' _chemical_formula_weight 949.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2626(4) _cell_length_b 16.8683(6) _cell_length_c 21.4569(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.185(2) _cell_angle_gamma 90.00 _cell_volume 5488.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10847 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.68 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.101 _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 123(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' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16661 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8619 _reflns_number_gt 5131 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+8.2310P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8619 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1479 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.2350 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 0.13984(11) 0.16865(11) 0.92667(8) 0.0274(5) Uani 1 1 d . . . Na2 Na 0.16251(11) 0.35365(11) 0.93112(8) 0.0284(5) Uani 1 1 d . A . Na3 Na 0.33160(11) 0.24175(12) 0.99652(8) 0.0299(5) Uani 1 1 d . A . Na4 Na 0.19756(11) 0.26369(11) 1.06763(8) 0.0265(5) Uani 1 1 d . A . O2 O 0.1747(3) 0.4897(2) 0.90671(18) 0.0491(11) Uani 1 1 d . . . O3 O 0.2209(2) 0.2495(2) 0.88720(14) 0.0287(8) Uani 1 1 d . A . O4 O 0.2783(2) 0.3510(2) 1.02968(15) 0.0290(8) Uani 1 1 d . . . O5 O 0.07893(18) 0.26807(19) 0.96811(13) 0.0232(8) Uani 1 1 d . A . O6 O 0.25065(19) 0.15250(19) 1.02957(14) 0.0278(8) Uani 1 1 d . A . N1 N 0.4193(3) 0.1777(3) 0.94564(19) 0.0356(11) Uani 1 1 d . . . N2 N 0.4819(3) 0.3043(3) 1.04848(19) 0.0345(11) Uani 1 1 d . . . N3 N 0.1017(2) 0.2068(2) 1.12011(18) 0.0278(10) Uani 1 1 d . . . N4 N 0.2958(3) 0.2271(3) 1.17955(19) 0.0335(11) Uani 1 1 d . . . C5 C 0.1539(5) 0.5590(4) 0.9380(3) 0.068(2) Uani 1 1 d . A . H5A H 0.1602 0.6071 0.9137 0.082 Uiso 1 1 calc R . . H5B H 0.1961 0.5631 0.9846 0.082 Uiso 1 1 calc R . . C6 C 0.0627(5) 0.5545(4) 0.9378(3) 0.071(2) Uani 1 1 d . . . H6A H 0.0515 0.6002 0.9619 0.106 Uiso 1 1 calc R A . H6B H 0.0556 0.5055 0.9598 0.106 Uiso 1 1 calc R . . H6C H 0.0206 0.5549 0.8916 0.106 Uiso 1 1 calc R . . C7 C 0.2539(4) 0.4960(5) 0.8943(3) 0.072(2) Uani 1 1 d . A . H7A H 0.2751 0.4421 0.8895 0.086 Uiso 1 1 calc R . . H7B H 0.2993 0.5216 0.9331 0.086 Uiso 1 1 calc R . . C8 C 0.2430(5) 0.5436(6) 0.8315(4) 0.102(3) Uani 1 1 d . . . H8A H 0.2941 0.5348 0.8184 0.153 Uiso 1 1 calc R A . H8B H 0.2387 0.6001 0.8405 0.153 Uiso 1 1 calc R . . H8C H 0.1892 0.5267 0.7953 0.153 Uiso 1 1 calc R . . C9 C 0.2459(3) 0.2575(3) 0.8349(2) 0.0267(12) Uani 1 1 d . . . C10 C 0.1964(3) 0.3086(3) 0.7805(2) 0.0281(12) Uani 1 1 d . A . C11 C 0.2247(3) 0.3196(3) 0.7275(2) 0.0337(13) Uani 1 1 d . . . H11 H 0.1927 0.3551 0.6929 0.040 Uiso 1 1 calc R A . C12 C 0.2974(3) 0.2811(4) 0.7225(2) 0.0382(14) Uani 1 1 d . A . C13 C 0.3422(3) 0.2298(3) 0.7739(2) 0.0360(13) Uani 1 1 d . . . H13 H 0.3925 0.2027 0.7720 0.043 Uiso 1 1 calc R A . C14 C 0.3164(3) 0.2162(3) 0.8283(2) 0.0295(12) Uani 1 1 d . A . C15 C 0.1127(3) 0.3461(4) 0.7795(2) 0.0401(14) Uani 1 1 d . . . H15A H 0.1265 0.3901 0.8115 0.060 Uiso 1 1 calc R A . H15B H 0.0771 0.3066 0.7919 0.060 Uiso 1 1 calc R . . H15C H 0.0796 0.3662 0.7346 0.060 Uiso 1 1 calc R . . C16 C 0.3261(4) 0.2950(4) 0.6634(3) 0.0546(18) Uani 1 1 d . . . H16A H 0.3612 0.3437 0.6706 0.082 Uiso 1 1 calc R A . H16B H 0.2739 0.3002 0.6225 0.082 Uiso 1 1 calc R . . H16C H 0.3617 0.2500 0.6589 0.082 Uiso 1 1 calc R . . C17 C 0.3638(3) 0.1517(3) 0.8774(2) 0.0357(13) Uani 1 1 d . A . H17A H 0.3190 0.1143 0.8813 0.043 Uiso 1 1 calc R . . H17B H 0.4016 0.1219 0.8584 0.043 Uiso 1 1 calc R . . C18 C 0.4606(4) 0.1081(4) 0.9846(3) 0.0540(17) Uani 1 1 d . A . H18A H 0.5033 0.0856 0.9669 0.081 Uiso 1 1 calc R . . H18B H 0.4153 0.0685 0.9817 0.081 Uiso 1 1 calc R . . H18C H 0.4911 0.1234 1.0314 0.081 Uiso 1 1 calc R . . C19 C 0.4834(3) 0.2370(4) 0.9442(3) 0.0414(14) Uani 1 1 d . A . H19A H 0.4521 0.2811 0.9146 0.050 Uiso 1 1 calc R . . H19B H 0.5245 0.2131 0.9250 0.050 Uiso 1 1 calc R . . C20 C 0.5369(3) 0.2706(4) 1.0139(2) 0.0448(15) Uani 1 1 d . A . H20A H 0.5737 0.2278 1.0417 0.054 Uiso 1 1 calc R . . H20B H 0.5770 0.3123 1.0090 0.054 Uiso 1 1 calc R . . C21 C 0.5368(3) 0.3084(4) 1.1213(2) 0.0437(15) Uani 1 1 d . A . H21A H 0.5567 0.2550 1.1380 0.066 Uiso 1 1 calc R . . H21B H 0.5015 0.3304 1.1458 0.066 Uiso 1 1 calc R . . H21C H 0.5881 0.3424 1.1280 0.066 Uiso 1 1 calc R . . C22 C 0.4499(3) 0.3844(3) 1.0223(2) 0.0355(13) Uani 1 1 d . A . H22A H 0.4061 0.3787 0.9764 0.043 Uiso 1 1 calc R . . H22B H 0.5002 0.4151 1.0193 0.043 Uiso 1 1 calc R . . C23 C 0.4083(3) 0.4316(3) 1.0627(2) 0.0298(12) Uani 1 1 d . . . C24 C 0.4543(3) 0.4970(3) 1.0999(2) 0.0364(13) Uani 1 1 d . A . H24 H 0.5105 0.5096 1.0984 0.044 Uiso 1 1 calc R . . C25 C 0.4217(4) 0.5436(3) 1.1385(2) 0.0382(14) Uani 1 1 d . . . C26 C 0.3387(3) 0.5235(3) 1.1388(2) 0.0367(13) Uani 1 1 d . A . H26 H 0.3147 0.5544 1.1651 0.044 Uiso 1 1 calc R . . C27 C 0.2895(3) 0.4606(3) 1.1025(2) 0.0322(13) Uani 1 1 d . . . C28 C 0.3240(3) 0.4122(3) 1.0636(2) 0.0281(12) Uani 1 1 d . A . C29 C 0.4721(4) 0.6139(3) 1.1786(3) 0.0538(17) Uani 1 1 d . A . H29A H 0.5324 0.6138 1.1787 0.081 Uiso 1 1 calc R . . H29B H 0.4738 0.6101 1.2247 0.081 Uiso 1 1 calc R . . H29C H 0.4425 0.6632 1.1584 0.081 Uiso 1 1 calc R . . C30 C 0.1991(3) 0.4435(3) 1.1038(3) 0.0410(14) Uani 1 1 d . A . H30A H 0.2028 0.3996 1.1346 0.062 Uiso 1 1 calc R . . H30B H 0.1591 0.4291 1.0588 0.062 Uiso 1 1 calc R . . H30C H 0.1766 0.4908 1.1189 0.062 Uiso 1 1 calc R . . C31 C -0.0025(3) 0.2686(3) 0.9673(2) 0.0221(11) Uani 1 1 d . . . C32 C -0.0696(3) 0.3136(3) 0.9186(2) 0.0237(11) Uani 1 1 d . A . C33 C -0.1546(3) 0.3131(3) 0.9179(2) 0.0291(12) Uani 1 1 d . . . H33 H -0.1974 0.3443 0.8851 0.035 Uiso 1 1 calc R A . C34 C -0.1812(3) 0.2703(3) 0.9617(2) 0.0302(12) Uani 1 1 d . A . C35 C -0.1170(3) 0.2256(3) 1.0088(2) 0.0267(11) Uani 1 1 d . . . H35 H -0.1331 0.1953 1.0400 0.032 Uiso 1 1 calc R A . C36 C -0.0292(3) 0.2231(3) 1.0123(2) 0.0245(11) Uani 1 1 d . A . C37 C 0.0346(3) 0.1681(3) 1.0619(2) 0.0263(11) Uani 1 1 d . A . H37A H 0.0005 0.1307 1.0786 0.032 Uiso 1 1 calc R . . H37B H 0.0655 0.1365 1.0382 0.032 Uiso 1 1 calc R . . C38 C -0.0442(3) 0.3612(3) 0.8692(2) 0.0368(13) Uani 1 1 d . . . H38A H -0.0964 0.3882 0.8384 0.055 Uiso 1 1 calc R A . H38B H -0.0199 0.3258 0.8440 0.055 Uiso 1 1 calc R . . H38C H 0.0003 0.4006 0.8931 0.055 Uiso 1 1 calc R . . C39 C -0.2749(3) 0.2724(3) 0.9593(3) 0.0395(14) Uani 1 1 d . . . H39A H -0.2920 0.3274 0.9631 0.059 Uiso 1 1 calc R A . H39B H -0.2796 0.2412 0.9963 0.059 Uiso 1 1 calc R . . H39C H -0.3141 0.2501 0.9167 0.059 Uiso 1 1 calc R . . C40 C 0.0605(4) 0.2520(3) 1.1591(2) 0.0422(14) Uani 1 1 d . A . H40A H 0.0254 0.2163 1.1755 0.063 Uiso 1 1 calc R . . H40B H 0.0222 0.2929 1.1308 0.063 Uiso 1 1 calc R . . H40C H 0.1064 0.2771 1.1971 0.063 Uiso 1 1 calc R . . C41 C 0.1615(3) 0.1458(3) 1.1619(2) 0.0317(12) Uani 1 1 d . A . H41A H 0.1767 0.1079 1.1325 0.038 Uiso 1 1 calc R . . H41B H 0.1304 0.1161 1.1865 0.038 Uiso 1 1 calc R . . C42 C 0.2467(3) 0.1806(3) 1.2121(2) 0.0383(14) Uani 1 1 d . A . H42A H 0.2320 0.2149 1.2441 0.046 Uiso 1 1 calc R . . H42B H 0.2845 0.1369 1.2378 0.046 Uiso 1 1 calc R . . C43 C 0.3370(4) 0.2979(3) 1.2200(3) 0.0507(16) Uani 1 1 d . A . H43A H 0.2914 0.3297 1.2281 0.076 Uiso 1 1 calc R . . H43B H 0.3660 0.3298 1.1958 0.076 Uiso 1 1 calc R . . H43C H 0.3807 0.2808 1.2628 0.076 Uiso 1 1 calc R . . C44 C 0.3662(3) 0.1828(3) 1.1663(2) 0.0359(13) Uani 1 1 d . A . H44A H 0.4168 0.1776 1.2090 0.043 Uiso 1 1 calc R . . H44B H 0.3862 0.2151 1.1359 0.043 Uiso 1 1 calc R . . C45 C 0.3431(3) 0.1016(3) 1.1362(2) 0.0342(13) Uani 1 1 d . . . C46 C 0.3787(4) 0.0354(4) 1.1753(3) 0.0491(16) Uani 1 1 d . A . H46 H 0.4155 0.0434 1.2207 0.059 Uiso 1 1 calc R . . C47 C 0.3634(5) -0.0402(4) 1.1518(3) 0.067(2) Uani 1 1 d . . . C48 C 0.3093(5) -0.0502(4) 1.0841(3) 0.0601(19) Uani 1 1 d . A . H48 H 0.2981 -0.1022 1.0659 0.072 Uiso 1 1 calc R . . C49 C 0.2723(4) 0.0135(3) 1.0437(2) 0.0387(14) Uani 1 1 d . . . C50 C 0.2874(3) 0.0913(3) 1.0679(2) 0.0296(12) Uani 1 1 d . A . C51 C 0.4010(6) -0.1120(5) 1.1958(4) 0.099(3) Uani 1 1 d . A . H51A H 0.4313 -0.0947 1.2421 0.149 Uiso 1 1 calc R . . H51B H 0.4429 -0.1394 1.1799 0.149 Uiso 1 1 calc R . . H51C H 0.3530 -0.1483 1.1937 0.149 Uiso 1 1 calc R . . C52 C 0.2133(4) -0.0004(4) 0.9707(3) 0.0543(17) Uani 1 1 d . A . H52A H 0.2187 -0.0557 0.9586 0.082 Uiso 1 1 calc R . . H52B H 0.2316 0.0348 0.9418 0.082 Uiso 1 1 calc R . . H52C H 0.1518 0.0107 0.9649 0.082 Uiso 1 1 calc R . . O1B O 0.0387(6) 0.1025(6) 0.8386(5) 0.045(3) Uiso 0.436(9) 1 d P A 2 C2B C -0.0294(9) 0.0459(9) 0.8366(7) 0.046(4) Uiso 0.436(9) 1 d P A 2 H2B1 H -0.0823 0.0526 0.7956 0.056 Uiso 0.436(9) 1 calc PR A 2 H2B2 H -0.0077 -0.0092 0.8386 0.056 Uiso 0.436(9) 1 calc PR A 2 C4B C 0.1255(12) 0.0319(12) 0.7868(10) 0.078(6) Uiso 0.436(9) 1 d P A 2 H4B1 H 0.1315 0.0226 0.7435 0.116 Uiso 0.436(9) 1 calc PR A 2 H4B2 H 0.1055 -0.0168 0.8017 0.116 Uiso 0.436(9) 1 calc PR A 2 H4B3 H 0.1827 0.0477 0.8197 0.116 Uiso 0.436(9) 1 calc PR A 2 C3B C 0.0600(10) 0.0961(9) 0.7798(7) 0.035(4) Uiso 0.436(9) 1 d P A 2 H3B1 H 0.0844 0.1471 0.7715 0.042 Uiso 0.436(9) 1 calc PR A 2 H3B2 H 0.0057 0.0848 0.7409 0.042 Uiso 0.436(9) 1 calc PR A 2 O1 O 0.0167(4) 0.0954(4) 0.8625(4) 0.036(2) Uiso 0.564(9) 1 d P A 1 C2 C -0.1341(6) 0.0816(7) 0.8587(5) 0.051(3) Uiso 0.564(9) 1 d P A 1 H2A H -0.1712 0.0519 0.8777 0.077 Uiso 0.564(9) 1 calc PR A 1 H2B H -0.1492 0.0668 0.8117 0.077 Uiso 0.564(9) 1 calc PR A 1 H2C H -0.1439 0.1386 0.8618 0.077 Uiso 0.564(9) 1 calc PR A 1 C3 C 0.0174(7) 0.0507(7) 0.8063(5) 0.044(3) Uiso 0.564(9) 1 d P A 1 H3A H -0.0410 0.0546 0.7698 0.052 Uiso 0.564(9) 1 calc PR A 1 H3B H 0.0288 -0.0058 0.8190 0.052 Uiso 0.564(9) 1 calc PR A 1 C4 C 0.0905(8) 0.0830(8) 0.7815(6) 0.044(3) Uiso 0.564(9) 1 d P A 1 H4A H 0.0844 0.0578 0.7389 0.065 Uiso 0.564(9) 1 calc PR A 1 H4B H 0.1487 0.0708 0.8148 0.065 Uiso 0.564(9) 1 calc PR A 1 H4C H 0.0841 0.1405 0.7754 0.065 Uiso 0.564(9) 1 calc PR A 1 C1 C -0.0477(4) 0.0644(4) 0.8933(3) 0.0587(17) Uiso 1 1 d . . . H1A H -0.0937 0.0286 0.8960 0.088 Uiso 0.436(9) 1 d PR A . H1B H -0.0684 0.1193 0.8906 0.088 Uiso 0.436(9) 1 d PR . . H1C H 0.0056 0.0580 0.9332 0.088 Uiso 0.436(9) 1 d PR . . H1D H -0.0417 0.0075 0.8976 0.070 Uiso 0.564(9) 1 d PR . . H1E H -0.0321 0.0881 0.9385 0.070 Uiso 0.564(9) 1 d PR . . 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 0.0307(10) 0.0322(12) 0.0147(9) -0.0015(8) 0.0027(8) -0.0021(8) Na2 0.0279(10) 0.0337(12) 0.0187(9) 0.0017(8) 0.0024(8) 0.0000(9) Na3 0.0267(10) 0.0383(13) 0.0210(9) 0.0013(8) 0.0043(8) 0.0007(9) Na4 0.0245(9) 0.0343(12) 0.0147(9) 0.0009(8) -0.0001(7) -0.0019(8) O2 0.058(3) 0.037(3) 0.037(2) 0.0036(19) -0.0013(19) -0.006(2) O3 0.0288(18) 0.038(2) 0.0184(16) 0.0002(15) 0.0075(14) 0.0011(16) O4 0.0285(18) 0.031(2) 0.0227(17) -0.0041(15) 0.0029(14) -0.0045(16) O5 0.0194(17) 0.036(2) 0.0121(15) -0.0007(14) 0.0026(13) -0.0019(15) O6 0.0288(18) 0.029(2) 0.0188(16) 0.0042(15) 0.0008(14) 0.0010(15) N1 0.033(2) 0.046(3) 0.025(2) 0.006(2) 0.0066(19) 0.008(2) N2 0.026(2) 0.053(3) 0.020(2) 0.001(2) 0.0020(18) 0.000(2) N3 0.029(2) 0.037(3) 0.0164(19) -0.0013(18) 0.0062(17) 0.0018(19) N4 0.031(2) 0.039(3) 0.021(2) -0.0036(19) -0.0031(18) -0.004(2) C5 0.093(6) 0.034(4) 0.042(4) -0.003(3) -0.019(4) -0.007(4) C6 0.088(6) 0.057(5) 0.045(4) -0.011(3) -0.003(4) 0.015(4) C7 0.055(4) 0.071(5) 0.066(5) 0.023(4) -0.005(4) -0.017(4) C8 0.075(5) 0.117(8) 0.100(6) 0.044(6) 0.014(5) -0.032(5) C9 0.026(3) 0.037(3) 0.017(2) -0.006(2) 0.007(2) -0.008(2) C10 0.026(3) 0.042(3) 0.013(2) -0.002(2) 0.004(2) -0.004(2) C11 0.033(3) 0.049(4) 0.015(2) 0.002(2) 0.005(2) -0.001(3) C12 0.036(3) 0.062(4) 0.016(3) -0.009(3) 0.008(2) -0.009(3) C13 0.027(3) 0.055(4) 0.028(3) -0.008(3) 0.012(2) -0.002(3) C14 0.030(3) 0.037(3) 0.021(3) -0.003(2) 0.008(2) -0.005(2) C15 0.035(3) 0.064(4) 0.017(3) 0.007(3) 0.005(2) 0.006(3) C16 0.047(3) 0.095(5) 0.025(3) 0.000(3) 0.017(3) 0.001(4) C17 0.039(3) 0.037(3) 0.031(3) -0.003(2) 0.013(2) 0.007(3) C18 0.048(4) 0.060(4) 0.046(4) 0.009(3) 0.007(3) 0.017(3) C19 0.025(3) 0.067(4) 0.035(3) 0.004(3) 0.014(2) 0.004(3) C20 0.024(3) 0.077(5) 0.029(3) 0.005(3) 0.005(2) 0.004(3) C21 0.035(3) 0.061(4) 0.022(3) 0.003(3) -0.005(2) 0.000(3) C22 0.025(3) 0.051(4) 0.025(3) 0.007(3) 0.002(2) -0.012(3) C23 0.031(3) 0.037(3) 0.014(2) 0.009(2) 0.000(2) -0.002(2) C24 0.034(3) 0.042(4) 0.022(3) 0.010(3) -0.004(2) -0.008(3) C25 0.044(3) 0.029(3) 0.024(3) 0.007(2) -0.008(2) -0.005(3) C26 0.044(3) 0.032(3) 0.025(3) 0.001(2) 0.000(2) 0.005(3) C27 0.034(3) 0.035(3) 0.021(3) 0.007(2) 0.001(2) 0.001(2) C28 0.029(3) 0.027(3) 0.020(2) 0.007(2) -0.002(2) 0.000(2) C29 0.068(4) 0.040(4) 0.035(3) 0.000(3) -0.004(3) -0.015(3) C30 0.045(3) 0.036(3) 0.039(3) -0.007(3) 0.012(3) 0.003(3) C31 0.020(2) 0.029(3) 0.016(2) -0.009(2) 0.005(2) -0.003(2) C32 0.029(3) 0.027(3) 0.012(2) -0.002(2) 0.004(2) 0.000(2) C33 0.025(3) 0.034(3) 0.021(2) -0.001(2) 0.000(2) 0.006(2) C34 0.025(3) 0.038(3) 0.025(3) -0.002(2) 0.005(2) -0.001(2) C35 0.029(3) 0.034(3) 0.021(2) -0.003(2) 0.012(2) -0.003(2) C36 0.025(3) 0.029(3) 0.017(2) -0.004(2) 0.004(2) -0.002(2) C37 0.027(3) 0.033(3) 0.015(2) -0.001(2) 0.003(2) -0.003(2) C38 0.031(3) 0.047(4) 0.028(3) 0.007(3) 0.005(2) 0.003(3) C39 0.032(3) 0.046(4) 0.040(3) 0.001(3) 0.012(3) 0.006(3) C40 0.043(3) 0.053(4) 0.026(3) -0.001(3) 0.007(2) 0.013(3) C41 0.031(3) 0.040(3) 0.018(2) 0.009(2) 0.002(2) 0.005(2) C42 0.038(3) 0.050(4) 0.016(2) 0.001(2) -0.004(2) 0.004(3) C43 0.055(4) 0.041(4) 0.034(3) 0.000(3) -0.010(3) -0.001(3) C44 0.027(3) 0.054(4) 0.016(2) 0.005(2) -0.005(2) -0.003(3) C45 0.030(3) 0.047(4) 0.022(3) 0.006(2) 0.005(2) 0.005(3) C46 0.057(4) 0.058(5) 0.021(3) 0.010(3) 0.000(3) 0.022(3) C47 0.097(5) 0.063(5) 0.034(3) 0.022(3) 0.016(4) 0.038(4) C48 0.102(5) 0.031(4) 0.036(3) 0.006(3) 0.012(4) 0.018(4) C49 0.054(3) 0.033(3) 0.023(3) 0.006(2) 0.007(3) 0.009(3) C50 0.029(3) 0.035(3) 0.024(3) 0.007(2) 0.008(2) 0.006(2) C51 0.162(8) 0.066(6) 0.050(4) 0.025(4) 0.014(5) 0.052(6) C52 0.079(4) 0.039(4) 0.031(3) -0.005(3) 0.003(3) -0.001(3) _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 O3 2.263(4) . ? Na1 O5 2.285(4) . ? Na1 O1B 2.296(9) . ? Na1 O6 2.307(3) . ? Na1 O1 2.332(7) . ? Na2 O4 2.268(3) . ? Na2 O5 2.311(3) . ? Na2 O3 2.350(4) . ? Na2 O2 2.379(4) . ? Na3 O4 2.259(4) . ? Na3 O6 2.275(4) . ? Na3 N1 2.349(4) . ? Na3 O3 2.389(3) . ? Na3 N2 2.522(4) . ? Na4 O5 2.304(3) . ? Na4 O4 2.309(4) . ? Na4 O6 2.332(4) . ? Na4 N3 2.427(4) . ? Na4 N4 2.435(4) . ? O2 C7 1.411(8) . ? O2 C5 1.447(8) . ? O3 C9 1.331(5) . ? O4 C28 1.326(6) . ? O5 C31 1.318(5) . ? O6 C50 1.321(6) . ? N1 C19 1.452(7) . ? N1 C18 1.456(7) . ? N1 C17 1.481(6) . ? N2 C20 1.468(7) . ? N2 C22 1.484(7) . ? N2 C21 1.495(6) . ? N3 C40 1.461(6) . ? N3 C41 1.476(6) . ? N3 C37 1.480(6) . ? N4 C42 1.466(7) . ? N4 C44 1.477(6) . ? N4 C43 1.486(7) . ? C5 C6 1.485(9) . ? C5 H5A 0.990 . ? C5 H5B 0.990 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 C8 1.523(9) . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 C14 1.393(7) . ? C9 C10 1.441(7) . ? C10 C11 1.385(6) . ? C10 C15 1.495(7) . ? C11 C12 1.386(7) . ? C11 H11 0.950 . ? C12 C13 1.384(8) . ? C12 C16 1.521(7) . ? C13 C14 1.395(7) . ? C13 H13 0.950 . ? C14 C17 1.518(7) . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.980 . ? C18 H18B 0.980 . ? C18 H18C 0.980 . ? C19 C20 1.540(7) . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C22 C23 1.505(7) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C23 C24 1.408(7) . ? C23 C28 1.417(7) . ? C24 C25 1.378(8) . ? C24 H24 0.950 . ? C25 C26 1.393(7) . ? C25 C29 1.520(7) . ? C26 C27 1.388(7) . ? C26 H26 0.950 . ? C27 C28 1.419(7) . ? C27 C30 1.508(7) . ? C29 H29A 0.980 . ? C29 H29B 0.980 . ? C29 H29C 0.980 . ? C30 H30A 0.980 . ? C30 H30B 0.980 . ? C30 H30C 0.980 . ? C31 C36 1.419(7) . ? C31 C32 1.427(6) . ? C32 C33 1.377(6) . ? C32 C38 1.500(7) . ? C33 C34 1.374(7) . ? C33 H33 0.950 . ? C34 C35 1.385(7) . ? C34 C39 1.505(6) . ? C35 C36 1.405(6) . ? C35 H35 0.950 . ? C36 C37 1.507(6) . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C39 H39A 0.980 . ? C39 H39B 0.980 . ? C39 H39C 0.980 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 C42 1.532(7) . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C42 H42A 0.990 . ? C42 H42B 0.990 . ? C43 H43A 0.980 . ? C43 H43B 0.980 . ? C43 H43C 0.980 . ? C44 C45 1.503(8) . ? C44 H44A 0.990 . ? C44 H44B 0.990 . ? C45 C46 1.390(8) . ? C45 C50 1.429(7) . ? C46 C47 1.361(9) . ? C46 H46 0.950 . ? C47 C48 1.412(8) . ? C47 C51 1.521(9) . ? C48 C49 1.374(7) . ? C48 H48 0.950 . ? C49 C50 1.399(7) . ? C49 C52 1.531(7) . ? C51 H51A 0.980 . ? C51 H51B 0.980 . ? C51 H51C 0.980 . ? C52 H52A 0.980 . ? C52 H52B 0.980 . ? C52 H52C 0.980 . ? O1B C3B 1.430(17) . ? O1B C2B 1.451(18) . ? C2B C1 1.388(14) . ? C2B H2B1 0.990 . ? C2B H2B2 0.990 . ? C2B H1D 1.5360 . ? C4B C3B 1.49(2) . ? C4B H4B1 0.980 . ? C4B H4B2 0.980 . ? C4B H4B3 0.980 . ? C3B H3B1 0.990 . ? C3B H3B2 0.990 . ? O1 C3 1.425(14) . ? O1 C1 1.519(10) . ? C2 C1 1.362(11) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C2 H1A 1.2218 . ? C2 H1B 1.2183 . ? C3 C4 1.565(15) . ? C3 H3A 0.990 . ? C3 H3B 0.990 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C1 H1A 0.980 . ? C1 H1B 0.980 . ? C1 H1C 0.980 . ? C1 H1D 0.9668 . ? C1 H1E 0.9929 . ? 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 O3 Na1 O5 95.52(13) . . ? O3 Na1 O1B 109.0(3) . . ? O5 Na1 O1B 113.2(3) . . ? O3 Na1 O6 94.03(12) . . ? O5 Na1 O6 90.73(12) . . ? O1B Na1 O6 144.1(3) . . ? O3 Na1 O1 126.2(2) . . ? O5 Na1 O1 102.6(2) . . ? O1B Na1 O1 18.2(2) . . ? O6 Na1 O1 135.2(2) . . ? O4 Na2 O5 93.49(12) . . ? O4 Na2 O3 92.28(13) . . ? O5 Na2 O3 92.50(13) . . ? O4 Na2 O2 96.71(14) . . ? O5 Na2 O2 141.67(15) . . ? O3 Na2 O2 123.74(15) . . ? O4 Na3 O6 96.36(13) . . ? O4 Na3 N1 152.65(17) . . ? O6 Na3 N1 110.94(16) . . ? O4 Na3 O3 91.48(12) . . ? O6 Na3 O3 91.51(12) . . ? N1 Na3 O3 86.44(13) . . ? O4 Na3 N2 86.55(14) . . ? O6 Na3 N2 135.77(14) . . ? N1 Na3 N2 75.16(15) . . ? O3 Na3 N2 132.63(14) . . ? O5 Na4 O4 92.59(12) . . ? O5 Na4 O6 89.61(12) . . ? O4 Na4 O6 93.44(13) . . ? O5 Na4 N3 88.83(12) . . ? O4 Na4 N3 163.47(15) . . ? O6 Na4 N3 103.05(14) . . ? O5 Na4 N4 162.46(15) . . ? O4 Na4 N4 104.78(14) . . ? O6 Na4 N4 86.99(14) . . ? N3 Na4 N4 75.23(14) . . ? C7 O2 C5 114.2(5) . . ? C7 O2 Na2 105.5(4) . . ? C5 O2 Na2 128.7(4) . . ? C9 O3 Na1 140.6(3) . . ? C9 O3 Na2 123.6(3) . . ? Na1 O3 Na2 85.78(12) . . ? C9 O3 Na3 118.8(3) . . ? Na1 O3 Na3 86.21(12) . . ? Na2 O3 Na3 85.27(12) . . ? C28 O4 Na3 127.3(3) . . ? C28 O4 Na2 127.5(3) . . ? Na3 O4 Na2 90.34(13) . . ? C28 O4 Na4 125.5(3) . . ? Na3 O4 Na4 85.54(13) . . ? Na2 O4 Na4 87.40(12) . . ? C31 O5 Na1 125.1(3) . . ? C31 O5 Na4 120.8(2) . . ? Na1 O5 Na4 90.09(12) . . ? C31 O5 Na2 134.7(3) . . ? Na1 O5 Na2 86.18(12) . . ? Na4 O5 Na2 86.50(11) . . ? C50 O6 Na3 121.9(3) . . ? C50 O6 Na1 135.2(3) . . ? Na3 O6 Na1 87.90(12) . . ? C50 O6 Na4 123.5(3) . . ? Na3 O6 Na4 84.62(13) . . ? Na1 O6 Na4 88.86(12) . . ? C19 N1 C18 112.4(4) . . ? C19 N1 C17 111.7(4) . . ? C18 N1 C17 108.6(4) . . ? C19 N1 Na3 104.7(3) . . ? C18 N1 Na3 109.6(3) . . ? C17 N1 Na3 109.8(3) . . ? C20 N2 C22 110.8(4) . . ? C20 N2 C21 107.7(4) . . ? C22 N2 C21 110.5(4) . . ? C20 N2 Na3 106.5(3) . . ? C22 N2 Na3 93.6(3) . . ? C21 N2 Na3 126.7(3) . . ? C40 N3 C41 110.7(4) . . ? C40 N3 C37 111.3(4) . . ? C41 N3 C37 109.1(4) . . ? C40 N3 Na4 124.3(3) . . ? C41 N3 Na4 99.5(3) . . ? C37 N3 Na4 100.6(3) . . ? C42 N4 C44 114.5(4) . . ? C42 N4 C43 111.1(4) . . ? C44 N4 C43 107.6(4) . . ? C42 N4 Na4 109.2(3) . . ? C44 N4 Na4 102.5(3) . . ? C43 N4 Na4 111.7(3) . . ? O2 C5 C6 111.0(5) . . ? O2 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O2 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 C8 112.6(6) . . ? O2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? O2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 C14 123.3(4) . . ? O3 C9 C10 119.5(4) . . ? C14 C9 C10 117.1(4) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 C15 120.2(4) . . ? C9 C10 C15 120.3(4) . . ? C10 C11 C12 123.1(5) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 116.8(5) . . ? C13 C12 C16 121.8(5) . . ? C11 C12 C16 121.3(5) . . ? C12 C13 C14 122.5(5) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C9 C14 C13 120.8(5) . . ? C9 C14 C17 121.2(4) . . ? C13 C14 C17 118.0(5) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C14 116.7(4) . . ? N1 C17 H17A 108.1 . . ? C14 C17 H17A 108.1 . . ? N1 C17 H17B 108.1 . . ? C14 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 113.1(4) . . ? N1 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N1 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? N2 C20 C19 113.6(4) . . ? N2 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? N2 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 C23 115.6(4) . . ? N2 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? N2 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.4 . . ? C24 C23 C28 119.4(5) . . ? C24 C23 C22 119.0(5) . . ? C28 C23 C22 121.6(4) . . ? C25 C24 C23 123.1(5) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 C26 116.6(5) . . ? C24 C25 C29 122.6(5) . . ? C26 C25 C29 120.8(5) . . ? C27 C26 C25 123.1(5) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C26 C27 C28 119.9(5) . . ? C26 C27 C30 120.3(5) . . ? C28 C27 C30 119.8(5) . . ? O4 C28 C23 121.7(5) . . ? O4 C28 C27 120.5(4) . . ? C23 C28 C27 117.8(5) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O5 C31 C36 122.7(4) . . ? O5 C31 C32 120.8(4) . . ? C36 C31 C32 116.5(4) . . ? C33 C32 C31 120.2(4) . . ? C33 C32 C38 121.8(4) . . ? C31 C32 C38 118.0(4) . . ? C34 C33 C32 124.0(4) . . ? C34 C33 H33 118.0 . . ? C32 C33 H33 118.0 . . ? C33 C34 C35 116.4(4) . . ? C33 C34 C39 121.9(4) . . ? C35 C34 C39 121.7(5) . . ? C34 C35 C36 122.7(4) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C31 120.2(4) . . ? C35 C36 C37 118.9(4) . . ? C31 C36 C37 120.8(4) . . ? N3 C37 C36 115.7(4) . . ? N3 C37 H37A 108.4 . . ? C36 C37 H37A 108.4 . . ? N3 C37 H37B 108.4 . . ? C36 C37 H37B 108.4 . . ? H37A C37 H37B 107.4 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N3 C40 H40A 109.5 . . ? N3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 C42 113.0(4) . . ? N3 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? N3 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? N4 C42 C41 112.3(4) . . ? N4 C42 H42A 109.1 . . ? C41 C42 H42A 109.1 . . ? N4 C42 H42B 109.1 . . ? C41 C42 H42B 109.1 . . ? H42A C42 H42B 107.9 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 C45 116.9(4) . . ? N4 C44 H44A 108.1 . . ? C45 C44 H44A 108.1 . . ? N4 C44 H44B 108.1 . . ? C45 C44 H44B 108.1 . . ? H44A C44 H44B 107.3 . . ? C46 C45 C50 119.5(5) . . ? C46 C45 C44 119.2(4) . . ? C50 C45 C44 121.2(4) . . ? C47 C46 C45 123.3(5) . . ? C47 C46 H46 118.4 . . ? C45 C46 H46 118.4 . . ? C46 C47 C48 117.1(5) . . ? C46 C47 C51 122.6(6) . . ? C48 C47 C51 120.4(7) . . ? C49 C48 C47 121.6(6) . . ? C49 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? C48 C49 C50 121.4(5) . . ? C48 C49 C52 119.6(5) . . ? C50 C49 C52 119.0(5) . . ? O6 C50 C49 121.6(4) . . ? O6 C50 C45 121.3(5) . . ? C49 C50 C45 117.1(4) . . ? C47 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C47 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C3B O1B C2B 110.5(11) . . ? C3B O1B Na1 115.7(9) . . ? C2B O1B Na1 131.0(9) . . ? C1 C2B O1B 103.2(11) . . ? C1 C2B H2B1 111.1 . . ? O1B C2B H2B1 111.1 . . ? C1 C2B H2B2 111.1 . . ? O1B C2B H2B2 111.1 . . ? H2B1 C2B H2B2 109.1 . . ? C1 C2B H1D 38.2 . . ? O1B C2B H1D 125.8 . . ? H2B1 C2B H1D 117.8 . . ? H2B2 C2B H1D 73.8 . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? O1B C3B C4B 111.0(12) . . ? O1B C3B H3B1 109.4 . . ? C4B C3B H3B1 109.4 . . ? O1B C3B H3B2 109.4 . . ? C4B C3B H3B2 109.4 . . ? H3B1 C3B H3B2 108.0 . . ? C3 O1 C1 113.7(7) . . ? C3 O1 Na1 120.8(6) . . ? C1 O1 Na1 120.4(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? C1 C2 H1A 44.2 . . ? H2A C2 H1A 67.6 . . ? H2B C2 H1A 111.3 . . ? H2C C2 H1A 137.4 . . ? C1 C2 H1B 44.2 . . ? H2A C2 H1B 125.5 . . ? H2B C2 H1B 123.7 . . ? H2C C2 H1B 65.3 . . ? H1A C2 H1B 82.0 . . ? O1 C3 C4 110.0(9) . . ? O1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C2 C1 C2B 94.3(8) . . ? C2 C1 O1 115.3(7) . . ? C2B C1 O1 45.3(6) . . ? C2 C1 H1A 60.3 . . ? C2B C1 H1A 108.8 . . ? O1 C1 H1A 154.1 . . ? C2 C1 H1B 60.1 . . ? C2B C1 H1B 109.7 . . ? O1 C1 H1B 85.7 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 155.8 . . ? C2B C1 H1C 109.9 . . ? O1 C1 H1C 83.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 108.2 . . ? C2B C1 H1D 79.2 . . ? O1 C1 H1D 108.8 . . ? H1A C1 H1D 55.5 . . ? H1B C1 H1D 164.9 . . ? H1C C1 H1D 77.3 . . ? C2 C1 H1E 107.2 . . ? C2B C1 H1E 152.4 . . ? O1 C1 H1E 108.3 . . ? H1A C1 H1E 96.9 . . ? H1B C1 H1E 68.9 . . ? H1C C1 H1E 50.0 . . ? H1D C1 H1E 109.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.513 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.087 #===END