# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_SR20 _database_code_depnum_ccdc_archive 'CCDC 885948' #TrackingRef 'SR20_150K_APEX_05mars12_archive.cif' _audit_creation_date 2012-03-05T17:34:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H72 Li2 N2 O6' _chemical_formula_sum 'C42 H72 Li2 N2 O6' _chemical_formula_weight 714.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.792(9) _cell_length_b 8.593(3) _cell_length_c 19.310(8) _cell_angle_alpha 90 _cell_angle_beta 99.763(19) _cell_angle_gamma 90 _cell_volume 4381(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2946 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 25.14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.992 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_unetI/netI 0.0824 _diffrn_reflns_number 17316 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 4946 _reflns_number_gt 2889 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4946 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2802 _refine_ls_wR_factor_gt 0.229 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.615 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.086 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in C 2/c CELL 0.71073 26.7920 8.5930 19.3100 90.000 99.763 90.000 ZERR 4.00 0.0090 0.0030 0.0080 0.000 0.019 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O SI LI UNIT 168 288 8 24 0 8 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.190200 FVAR 0.33898 O1 4 0.949725 0.143620 0.214114 11.00000 0.01740 0.03665 = 0.02638 -0.00187 0.00677 0.00198 C2 1 0.901109 0.184226 0.199361 11.00000 0.01716 0.03230 = 0.02211 0.00216 0.00625 -0.00015 C3 1 0.863807 0.092170 0.155716 11.00000 0.02174 0.03276 = 0.02430 0.00035 0.00626 -0.00002 C4 1 0.813963 0.147067 0.142823 11.00000 0.02253 0.03823 = 0.02791 -0.00084 0.00491 -0.00483 AFIX 43 H4 2 0.789353 0.086269 0.113453 11.00000 -1.20000 AFIX 0 C5 1 0.798026 0.284068 0.169961 11.00000 0.01979 0.04346 = 0.03231 0.00277 0.00559 0.00343 C6 1 0.834839 0.370961 0.213215 11.00000 0.02523 0.03115 = 0.03126 0.00057 0.00865 0.00542 AFIX 43 H6 2 0.825298 0.464992 0.233314 11.00000 -1.20000 AFIX 0 C7 1 0.885074 0.323341 0.227594 11.00000 0.02265 0.03115 = 0.02452 -0.00001 0.00562 0.00008 C8 1 0.877926 -0.060916 0.123036 11.00000 0.02939 0.03169 = 0.03248 -0.00409 0.00619 -0.00182 C9 1 0.913355 -0.026300 0.069378 11.00000 0.04070 0.04633 = 0.03027 -0.00690 0.01169 0.00199 AFIX 137 H9A 2 0.895955 0.042116 0.032380 11.00000 -1.50000 H9B 2 0.922362 -0.124049 0.048436 11.00000 -1.50000 H9C 2 0.944175 0.024947 0.093351 11.00000 -1.50000 AFIX 0 C10 1 0.904391 -0.173179 0.179674 11.00000 0.04320 0.03263 = 0.04009 -0.00052 0.01047 0.00208 AFIX 137 H10A 2 0.933850 -0.121514 0.207207 11.00000 -1.50000 H10B 2 0.915487 -0.266164 0.157120 11.00000 -1.50000 H10C 2 0.880694 -0.203376 0.210776 11.00000 -1.50000 AFIX 0 C11 1 0.831451 -0.146282 0.083181 11.00000 0.03808 0.04178 = 0.06220 -0.01805 0.00079 -0.00347 AFIX 137 H11A 2 0.806795 -0.162762 0.114599 11.00000 -1.50000 H11B 2 0.841898 -0.247077 0.066673 11.00000 -1.50000 H11C 2 0.815986 -0.083512 0.042824 11.00000 -1.50000 AFIX 0 C12 1 0.742973 0.343082 0.153062 11.00000 0.01898 0.05130 = 0.04651 -0.00224 0.00550 0.00776 C13 1 0.722858 0.370439 0.222407 11.00000 0.03593 0.09788 = 0.07582 0.00512 0.01850 0.01473 AFIX 137 H13A 2 0.745161 0.443541 0.251890 11.00000 -1.50000 H13B 2 0.722075 0.271355 0.247330 11.00000 -1.50000 H13C 2 0.688570 0.413786 0.212020 11.00000 -1.50000 AFIX 0 C14 1 0.742618 0.499477 0.115036 11.00000 0.04202 0.09855 = 0.09074 0.03571 0.01028 0.02179 AFIX 137 H14A 2 0.707750 0.537780 0.103365 11.00000 -1.50000 H14B 2 0.756699 0.486020 0.071776 11.00000 -1.50000 H14C 2 0.763177 0.574762 0.145622 11.00000 -1.50000 AFIX 0 C15 1 0.707932 0.229979 0.108791 11.00000 0.02533 0.10786 = 0.14948 -0.04796 -0.00893 0.00816 AFIX 137 H15A 2 0.673172 0.269768 0.102335 11.00000 -1.50000 H15B 2 0.709493 0.128792 0.132473 11.00000 -1.50000 H15C 2 0.718413 0.218044 0.062862 11.00000 -1.50000 AFIX 0 C21 1 0.923356 0.428039 0.271888 11.00000 0.02533 0.02865 = 0.02899 -0.00045 0.00646 -0.00017 AFIX 23 H21A 2 0.948826 0.460275 0.243098 11.00000 -1.20000 H21B 2 0.905655 0.523162 0.283559 11.00000 -1.20000 AFIX 0 N22 3 0.950464 0.359243 0.338418 11.00000 0.02277 0.02850 = 0.02446 -0.00293 0.00584 -0.00268 C23 1 0.915150 0.300169 0.384077 11.00000 0.02059 0.04210 = 0.02643 -0.00303 0.00950 0.00049 AFIX 23 H23A 2 0.882941 0.358825 0.373745 11.00000 -1.20000 H23B 2 0.930057 0.319112 0.433865 11.00000 -1.20000 AFIX 0 C24 1 0.904254 0.129627 0.373736 11.00000 0.02472 0.03946 = 0.02948 0.00097 0.01115 -0.00345 AFIX 23 H24A 2 0.885143 0.090916 0.409846 11.00000 -1.20000 H24B 2 0.883795 0.110784 0.326785 11.00000 -1.20000 AFIX 0 O25 4 0.952433 0.050806 0.379856 11.00000 0.02924 0.03092 = 0.04274 0.00132 0.01836 -0.00038 C26 1 0.947943 -0.113613 0.382606 11.00000 0.04993 0.03415 = 0.05058 0.00463 0.02391 -0.00468 AFIX 137 H26A 2 0.933754 -0.142889 0.424317 11.00000 -1.50000 H26B 2 0.981455 -0.161089 0.385058 11.00000 -1.50000 H26C 2 0.925521 -0.150356 0.340340 11.00000 -1.50000 AFIX 0 C27 1 0.985545 0.475322 0.376125 11.00000 0.02836 0.02578 = 0.03057 -0.00530 0.00539 -0.00176 AFIX 23 H27A 2 0.967377 0.539739 0.406341 11.00000 -1.20000 H27B 2 0.997797 0.544891 0.341732 11.00000 -1.20000 AFIX 0 C28 1 1.030225 0.396741 0.420929 11.00000 0.02820 0.03159 = 0.03296 -0.00620 0.00014 -0.00225 AFIX 23 H28A 2 1.018543 0.334068 0.458124 11.00000 -1.20000 H28B 2 1.047171 0.326325 0.391605 11.00000 -1.20000 AFIX 0 O29 4 1.064751 0.513183 0.451843 11.00000 0.02705 0.03826 = 0.03669 -0.00757 0.00121 -0.00256 C30 1 1.112985 0.447357 0.477731 11.00000 0.02892 0.04716 = 0.03810 -0.00560 0.00512 -0.00354 AFIX 137 H30A 2 1.109557 0.368805 0.513417 11.00000 -1.50000 H30B 2 1.136150 0.529373 0.498683 11.00000 -1.50000 H30C 2 1.126501 0.398513 0.438938 11.00000 -1.50000 AFIX 0 LI1 6 1.014192 0.158599 0.192535 11.00000 0.02051 0.02940 = 0.03223 0.00029 0.00808 -0.00106 HKLF 4 REM import in C 2/c REM R1 = 0.0825 for 2889 Fo > 4sig(Fo) and 0.1347 for all 4946 data REM 243 parameters refined using 0 restraints END WGHT 0.1749 0.0000 REM Highest difference peak 0.61, deepest hole -0.46, 1-sigma level 0.09 Q1 1 0.7293 0.3637 0.0689 11.00000 0.05 0.61 Q2 1 0.7068 0.2278 0.1802 11.00000 0.05 0.57 Q3 1 0.7316 0.5005 0.1858 11.00000 0.05 0.54 Q4 1 0.9470 0.4574 0.3227 11.00000 0.05 0.39 Q5 1 0.9402 0.4206 0.3109 11.00000 0.05 0.37 Q6 1 0.8827 0.1351 0.1728 11.00000 0.05 0.37 Q7 1 0.9353 0.2804 0.4338 11.00000 0.05 0.36 Q8 1 0.8858 -0.1294 0.1479 11.00000 0.05 0.36 Q9 1 0.9784 0.0612 0.4379 11.00000 0.05 0.35 Q10 1 0.9693 0.1665 0.2581 11.00000 0.05 0.35 Q11 1 0.9087 0.3591 0.2591 11.00000 0.05 0.34 Q12 1 0.8907 0.2462 0.3415 11.00000 0.05 0.34 Q13 1 0.9315 -0.0177 0.3429 11.00000 0.05 0.32 Q14 1 0.9930 -0.0429 0.4720 11.00000 0.05 0.28 Q15 1 0.9294 -0.1259 0.2231 11.00000 0.05 0.28 Q16 1 1.0505 0.6398 0.4316 11.00000 0.05 0.27 Q17 1 0.9599 0.1086 0.3948 11.00000 0.05 0.27 Q18 1 0.8307 0.1281 0.0802 11.00000 0.05 0.27 Q19 1 0.9797 -0.1124 0.4361 11.00000 0.05 0.26 Q20 1 1.0425 0.5426 0.4028 11.00000 0.05 0.25 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 O1 O 0.94973(6) 0.1436(2) 0.21411(9) 0.0265(5) Uani 1 1 d . . . C2 C 0.90111(9) 0.1842(3) 0.19936(12) 0.0235(6) Uani 1 1 d . . . C3 C 0.86381(9) 0.0922(3) 0.15572(13) 0.0260(6) Uani 1 1 d . . . C4 C 0.81396(10) 0.1471(3) 0.14282(14) 0.0295(6) Uani 1 1 d . . . H4 H 0.7894 0.0863 0.1135 0.035 Uiso 1 1 calc R . . C5 C 0.79803(10) 0.2841(3) 0.16996(14) 0.0317(7) Uani 1 1 d . . . C6 C 0.83484(9) 0.3710(3) 0.21321(13) 0.0288(6) Uani 1 1 d . . . H6 H 0.8253 0.465 0.2333 0.035 Uiso 1 1 calc R . . C7 C 0.88507(9) 0.3233(3) 0.22759(13) 0.0259(6) Uani 1 1 d . . . C8 C 0.87793(10) -0.0609(3) 0.12304(14) 0.0311(6) Uani 1 1 d . . . C9 C 0.91335(11) -0.0263(4) 0.06938(15) 0.0384(7) Uani 1 1 d . . . H9A H 0.896 0.0421 0.0324 0.058 Uiso 1 1 calc R . . H9B H 0.9224 -0.124 0.0484 0.058 Uiso 1 1 calc R . . H9C H 0.9442 0.0249 0.0934 0.058 Uiso 1 1 calc R . . C10 C 0.90439(12) -0.1732(3) 0.17967(16) 0.0382(7) Uani 1 1 d . . . H10A H 0.9339 -0.1215 0.2072 0.057 Uiso 1 1 calc R . . H10B H 0.9155 -0.2662 0.1571 0.057 Uiso 1 1 calc R . . H10C H 0.8807 -0.2034 0.2108 0.057 Uiso 1 1 calc R . . C11 C 0.83145(12) -0.1463(4) 0.08318(18) 0.0483(9) Uani 1 1 d . . . H11A H 0.8068 -0.1628 0.1146 0.072 Uiso 1 1 calc R . . H11B H 0.8419 -0.2471 0.0667 0.072 Uiso 1 1 calc R . . H11C H 0.816 -0.0835 0.0428 0.072 Uiso 1 1 calc R . . C12 C 0.74297(10) 0.3431(4) 0.15306(16) 0.0389(7) Uani 1 1 d . . . C13 C 0.72286(14) 0.3704(5) 0.2224(2) 0.0688(12) Uani 1 1 d . . . H13A H 0.7452 0.4435 0.2519 0.103 Uiso 1 1 calc R . . H13B H 0.7221 0.2714 0.2473 0.103 Uiso 1 1 calc R . . H13C H 0.6886 0.4138 0.212 0.103 Uiso 1 1 calc R . . C14 C 0.74262(15) 0.4995(5) 0.1150(3) 0.0772(14) Uani 1 1 d . . . H14A H 0.7078 0.5378 0.1034 0.116 Uiso 1 1 calc R . . H14B H 0.7567 0.486 0.0718 0.116 Uiso 1 1 calc R . . H14C H 0.7632 0.5748 0.1456 0.116 Uiso 1 1 calc R . . C15 C 0.70793(14) 0.2300(6) 0.1088(3) 0.0970(19) Uani 1 1 d . . . H15A H 0.6732 0.2698 0.1023 0.145 Uiso 1 1 calc R . . H15B H 0.7095 0.1288 0.1325 0.145 Uiso 1 1 calc R . . H15C H 0.7184 0.218 0.0629 0.145 Uiso 1 1 calc R . . C21 C 0.92336(9) 0.4280(3) 0.27189(13) 0.0274(6) Uani 1 1 d . . . H21A H 0.9488 0.4603 0.2431 0.033 Uiso 1 1 calc R . . H21B H 0.9057 0.5232 0.2836 0.033 Uiso 1 1 calc R . . N22 N 0.95046(8) 0.3592(2) 0.33842(10) 0.0250(5) Uani 1 1 d . . . C23 C 0.91515(10) 0.3002(3) 0.38408(13) 0.0291(6) Uani 1 1 d . . . H23A H 0.8829 0.3588 0.3737 0.035 Uiso 1 1 calc R . . H23B H 0.9301 0.3191 0.4339 0.035 Uiso 1 1 calc R . . C24 C 0.90425(10) 0.1296(3) 0.37374(14) 0.0305(6) Uani 1 1 d . . . H24A H 0.8851 0.0909 0.4098 0.037 Uiso 1 1 calc R . . H24B H 0.8838 0.1108 0.3268 0.037 Uiso 1 1 calc R . . O25 O 0.95243(7) 0.0508(2) 0.37986(10) 0.0329(5) Uani 1 1 d . . . C26 C 0.94794(12) -0.1136(3) 0.38261(17) 0.0431(8) Uani 1 1 d . . . H26A H 0.9338 -0.1429 0.4243 0.065 Uiso 1 1 calc R . . H26B H 0.9815 -0.1611 0.3851 0.065 Uiso 1 1 calc R . . H26C H 0.9255 -0.1504 0.3403 0.065 Uiso 1 1 calc R . . C27 C 0.98555(9) 0.4753(3) 0.37612(14) 0.0282(6) Uani 1 1 d . . . H27A H 0.9674 0.5397 0.4063 0.034 Uiso 1 1 calc R . . H27B H 0.9978 0.5449 0.3417 0.034 Uiso 1 1 calc R . . C28 C 1.03022(10) 0.3967(3) 0.42093(14) 0.0315(7) Uani 1 1 d . . . H28A H 1.0185 0.3341 0.4581 0.038 Uiso 1 1 calc R . . H28B H 1.0472 0.3263 0.3916 0.038 Uiso 1 1 calc R . . O29 O 1.06475(7) 0.5132(2) 0.45184(10) 0.0345(5) Uani 1 1 d . . . C30 C 1.11299(10) 0.4474(4) 0.47773(16) 0.0381(7) Uani 1 1 d . . . H30A H 1.1096 0.3688 0.5134 0.057 Uiso 1 1 calc R . . H30B H 1.1361 0.5294 0.4987 0.057 Uiso 1 1 calc R . . H30C H 1.1265 0.3985 0.4389 0.057 Uiso 1 1 calc R . . Li1 Li 1.01419(15) 0.1586(5) 0.1925(2) 0.0270(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0174(9) 0.0366(11) 0.0264(9) -0.0019(8) 0.0068(7) 0.0020(7) C2 0.0172(12) 0.0323(15) 0.0221(12) 0.0022(11) 0.0063(9) -0.0001(10) C3 0.0217(13) 0.0328(15) 0.0243(13) 0.0004(11) 0.0063(10) 0.0000(10) C4 0.0225(13) 0.0382(16) 0.0279(13) -0.0008(12) 0.0049(10) -0.0048(11) C5 0.0198(13) 0.0435(17) 0.0323(14) 0.0028(12) 0.0056(11) 0.0034(11) C6 0.0252(14) 0.0311(15) 0.0313(14) 0.0006(11) 0.0086(11) 0.0054(11) C7 0.0226(13) 0.0312(15) 0.0245(12) 0.0000(11) 0.0056(10) 0.0001(10) C8 0.0294(14) 0.0317(16) 0.0325(14) -0.0041(12) 0.0062(11) -0.0018(11) C9 0.0407(17) 0.0463(19) 0.0303(15) -0.0069(13) 0.0117(12) 0.0020(13) C10 0.0432(17) 0.0326(17) 0.0401(16) -0.0005(13) 0.0105(13) 0.0021(13) C11 0.0381(18) 0.0418(19) 0.062(2) -0.0181(16) 0.0008(15) -0.0035(14) C12 0.0190(14) 0.051(2) 0.0465(17) -0.0022(14) 0.0055(12) 0.0078(12) C13 0.036(2) 0.098(3) 0.076(3) 0.005(2) 0.0185(18) 0.0147(19) C14 0.042(2) 0.099(3) 0.091(3) 0.036(3) 0.010(2) 0.022(2) C15 0.0253(19) 0.108(4) 0.149(5) -0.048(3) -0.009(2) 0.008(2) C21 0.0253(13) 0.0287(15) 0.0290(14) -0.0005(11) 0.0065(10) -0.0002(11) N22 0.0228(11) 0.0285(12) 0.0245(11) -0.0029(9) 0.0058(8) -0.0027(8) C23 0.0206(13) 0.0421(17) 0.0264(13) -0.0030(12) 0.0095(10) 0.0005(11) C24 0.0247(13) 0.0395(17) 0.0295(14) 0.0010(12) 0.0112(11) -0.0034(11) O25 0.0292(10) 0.0309(11) 0.0427(12) 0.0013(9) 0.0184(8) -0.0004(8) C26 0.0499(19) 0.0341(18) 0.0506(19) 0.0046(14) 0.0239(15) -0.0047(14) C27 0.0284(14) 0.0258(15) 0.0306(14) -0.0053(11) 0.0054(11) -0.0018(11) C28 0.0282(14) 0.0316(16) 0.0330(14) -0.0062(12) 0.0001(11) -0.0023(11) O29 0.0271(10) 0.0383(12) 0.0367(11) -0.0076(9) 0.0012(8) -0.0026(8) C30 0.0289(15) 0.0472(19) 0.0381(16) -0.0056(14) 0.0051(12) -0.0035(13) Li1 0.021(2) 0.029(2) 0.032(2) 0.0003(19) 0.0081(17) -0.0011(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 C2 1.332(3) . ? O1 Li1 1.849(5) . ? C2 C7 1.411(4) . ? C2 C3 1.431(3) . ? C3 C4 1.398(3) . ? C3 C8 1.534(4) . ? C4 C5 1.385(4) . ? C4 H4 0.95 . ? C5 C6 1.396(4) . ? C5 C12 1.541(4) . ? C6 C7 1.389(3) . ? C6 H6 0.95 . ? C7 C21 1.515(3) . ? C8 C11 1.535(4) . ? C8 C10 1.538(4) . ? C8 C9 1.548(4) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C15 1.511(5) . ? C12 C14 1.531(5) . ? C12 C13 1.544(5) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C21 N22 1.487(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? N22 C27 1.475(3) . ? N22 C23 1.488(3) . ? C23 C24 1.501(4) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 O25 1.445(3) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? O25 C26 1.420(3) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.512(3) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 O29 1.423(3) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? O29 C30 1.422(3) . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? Li1 O1 1.900(4) 2_755 ? Li1 O25 2.009(5) 2_755 ? Li1 N22 2.102(5) 2_755 ? Li1 Li1 2.465(9) 2_755 ? Li1 C24 2.724(5) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 Li1 148.3(2) . . ? C2 O1 Li1 120.5(2) . 2_755 ? Li1 O1 Li1 82.2(2) . 2_755 ? O1 C2 C7 119.4(2) . . ? O1 C2 C3 122.8(2) . . ? C7 C2 C3 117.9(2) . . ? C4 C3 C2 118.0(2) . . ? C4 C3 C8 120.7(2) . . ? C2 C3 C8 121.3(2) . . ? C5 C4 C3 124.5(2) . . ? C5 C4 H4 117.8 . . ? C3 C4 H4 117.8 . . ? C4 C5 C6 116.7(2) . . ? C4 C5 C12 123.0(2) . . ? C6 C5 C12 120.3(3) . . ? C7 C6 C5 121.6(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C2 121.4(2) . . ? C6 C7 C21 118.6(2) . . ? C2 C7 C21 120.0(2) . . ? C3 C8 C11 112.4(2) . . ? C3 C8 C10 111.2(2) . . ? C11 C8 C10 107.1(2) . . ? C3 C8 C9 109.4(2) . . ? C11 C8 C9 107.1(2) . . ? C10 C8 C9 109.6(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 109.9(3) . . ? C15 C12 C5 112.9(3) . . ? C14 C12 C5 108.6(3) . . ? C15 C12 C13 108.3(3) . . ? C14 C12 C13 107.9(3) . . ? C5 C12 C13 109.2(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N22 C21 C7 115.9(2) . . ? N22 C21 H21A 108.3 . . ? C7 C21 H21A 108.3 . . ? N22 C21 H21B 108.3 . . ? C7 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C27 N22 C21 109.5(2) . . ? C27 N22 C23 110.7(2) . . ? C21 N22 C23 112.4(2) . . ? C27 N22 Li1 114.51(19) . 2_755 ? C21 N22 Li1 104.95(19) . 2_755 ? C23 N22 Li1 104.5(2) . 2_755 ? N22 C23 C24 112.5(2) . . ? N22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? O25 C24 C23 107.2(2) . . ? O25 C24 Li1 45.94(14) . 2_755 ? C23 C24 Li1 79.62(17) . 2_755 ? O25 C24 H24A 110.3 . . ? C23 C24 H24A 110.3 . . ? Li1 C24 H24A 156 2_755 . ? O25 C24 H24B 110.3 . . ? C23 C24 H24B 110.3 . . ? Li1 C24 H24B 87 2_755 . ? H24A C24 H24B 108.5 . . ? C26 O25 C24 112.9(2) . . ? C26 O25 Li1 122.4(2) . 2_755 ? C24 O25 Li1 102.94(19) . 2_755 ? O25 C26 H26A 109.5 . . ? O25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N22 C27 C28 110.9(2) . . ? N22 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N22 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108 . . ? O29 C28 C27 108.7(2) . . ? O29 C28 H28A 109.9 . . ? C27 C28 H28A 109.9 . . ? O29 C28 H28B 109.9 . . ? C27 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C30 O29 C28 110.8(2) . . ? O29 C30 H30A 109.5 . . ? O29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 Li1 O1 97.2(2) . 2_755 ? O1 Li1 O25 131.9(2) . 2_755 ? O1 Li1 O25 114.5(2) 2_755 2_755 ? O1 Li1 N22 127.2(2) . 2_755 ? O1 Li1 N22 98.28(19) 2_755 2_755 ? O25 Li1 N22 84.56(19) 2_755 2_755 ? O1 Li1 Li1 49.79(16) . 2_755 ? O1 Li1 Li1 47.99(15) 2_755 2_755 ? O25 Li1 Li1 150.25(17) 2_755 2_755 ? N22 Li1 Li1 118.60(15) 2_755 2_755 ? O1 Li1 C24 162.5(2) . 2_755 ? O1 Li1 C24 96.88(18) 2_755 2_755 ? O25 Li1 C24 31.12(10) 2_755 2_755 ? N22 Li1 C24 60.37(14) 2_755 2_755 ? Li1 Li1 C24 144.8(3) 2_755 2_755 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 O1 C2 C7 -86.0(4) . . . . ? Li1 O1 C2 C7 44.8(3) 2_755 . . . ? Li1 O1 C2 C3 94.0(4) . . . . ? Li1 O1 C2 C3 -135.1(3) 2_755 . . . ? O1 C2 C3 C4 -179.1(2) . . . . ? C7 C2 C3 C4 1.0(4) . . . . ? O1 C2 C3 C8 0.1(4) . . . . ? C7 C2 C3 C8 -179.8(2) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C8 C3 C4 C5 -179.8(3) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C3 C4 C5 C12 178.4(3) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C12 C5 C6 C7 -177.9(3) . . . . ? C5 C6 C7 C2 -0.4(4) . . . . ? C5 C6 C7 C21 176.8(2) . . . . ? O1 C2 C7 C6 179.5(2) . . . . ? C3 C2 C7 C6 -0.6(4) . . . . ? O1 C2 C7 C21 2.4(4) . . . . ? C3 C2 C7 C21 -177.7(2) . . . . ? C4 C3 C8 C11 -5.4(4) . . . . ? C2 C3 C8 C11 175.5(3) . . . . ? C4 C3 C8 C10 -125.4(3) . . . . ? C2 C3 C8 C10 55.5(3) . . . . ? C4 C3 C8 C9 113.4(3) . . . . ? C2 C3 C8 C9 -65.7(3) . . . . ? C4 C5 C12 C15 4.5(5) . . . . ? C6 C5 C12 C15 -176.9(3) . . . . ? C4 C5 C12 C14 -117.6(3) . . . . ? C6 C5 C12 C14 61.0(4) . . . . ? C4 C5 C12 C13 125.0(3) . . . . ? C6 C5 C12 C13 -56.4(4) . . . . ? C6 C7 C21 N22 120.1(3) . . . . ? C2 C7 C21 N22 -62.7(3) . . . . ? C7 C21 N22 C27 -179.0(2) . . . . ? C7 C21 N22 C23 -55.4(3) . . . . ? C7 C21 N22 Li1 57.6(3) . . . 2_755 ? C27 N22 C23 C24 -142.3(2) . . . . ? C21 N22 C23 C24 94.8(3) . . . . ? Li1 N22 C23 C24 -18.5(3) 2_755 . . . ? N22 C23 C24 O25 51.1(3) . . . . ? N22 C23 C24 Li1 13.92(19) . . . 2_755 ? C23 C24 O25 C26 170.3(2) . . . . ? Li1 C24 O25 C26 -133.9(3) 2_755 . . . ? C23 C24 O25 Li1 -55.8(2) . . . 2_755 ? C21 N22 C27 C28 -151.8(2) . . . . ? C23 N22 C27 C28 83.7(3) . . . . ? Li1 N22 C27 C28 -34.2(3) 2_755 . . . ? N22 C27 C28 O29 175.6(2) . . . . ? C27 C28 O29 C30 -163.6(2) . . . . ? C2 O1 Li1 O1 146.6(3) . . . 2_755 ? Li1 O1 Li1 O1 7.8(3) 2_755 . . 2_755 ? C2 O1 Li1 O25 -80.9(5) . . . 2_755 ? Li1 O1 Li1 O25 140.2(2) 2_755 . . 2_755 ? C2 O1 Li1 N22 40.5(5) . . . 2_755 ? Li1 O1 Li1 N22 -98.4(3) 2_755 . . 2_755 ? C2 O1 Li1 Li1 138.8(5) . . . 2_755 ? C2 O1 Li1 C24 -69.6(9) . . . 2_755 ? Li1 O1 Li1 C24 151.6(7) 2_755 . . 2_755 ? data_SR8 _database_code_depnum_ccdc_archive 'CCDC 885949' #TrackingRef 'SR8_150K_APEX_28fev12_archive.cif' _audit_creation_date 2012-02-29T10:08:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C23 H38 Li N O3)' _chemical_formula_sum 'C46 H76 Li2 N2 O6' _chemical_formula_weight 766.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.740(3) _cell_length_b 11.668(3) _cell_length_c 18.746(5) _cell_angle_alpha 91.944(12) _cell_angle_beta 100.525(12) _cell_angle_gamma 95.069(13) _cell_volume 2297.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4022 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 23.08 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.996 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_unetI/netI 0.0847 _diffrn_reflns_number 28356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.968 _reflns_number_total 10200 _reflns_number_gt 5702 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0667P)^2^+0.6046P] 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_number_reflns 10200 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.06 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.371 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.049 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P -1 CELL 0.71073 10.7400 11.6680 18.7460 91.944 100.525 95.069 ZERR 2.00 0.0030 0.0030 0.0050 0.012 0.012 0.013 LATT 1 SFAC C H LI N O UNIT 92 152 4 4 12 MERG 2 EXYZ C63A C63B EADP C63a c63b EADP c64a C65A c66a EADP c64b C65b C66B FMAP 2 PLAN 20 ACTA 50.00 BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.066700 0.604600 FVAR 0.57066 MOLE 1 LI1 3 -0.005091 -0.110797 -0.004185 11.00000 0.02875 0.02854 = 0.02284 0.00322 0.00377 0.00103 O2 5 0.053602 -0.000303 0.075658 11.00000 0.02613 0.02745 = 0.01671 0.00100 -0.00187 0.00093 C3 1 0.150084 0.028822 0.130475 11.00000 0.02633 0.02217 = 0.02009 0.00092 0.00158 0.00566 C4 1 0.146034 0.003682 0.204131 11.00000 0.02661 0.01768 = 0.02175 0.00323 0.00113 0.00244 C5 1 0.254994 0.035977 0.257298 11.00000 0.03446 0.02438 = 0.01492 0.00336 0.00171 0.00578 AFIX 43 H5 2 0.251496 0.018768 0.306104 11.00000 -1.20000 AFIX 0 C6 1 0.367486 0.091311 0.243498 11.00000 0.02661 0.02419 = 0.02420 0.00309 -0.00093 0.00607 C7 1 0.368130 0.117284 0.172169 11.00000 0.02447 0.03069 = 0.02781 0.00578 0.00356 0.00084 AFIX 43 H7 2 0.442575 0.156437 0.160460 11.00000 -1.20000 AFIX 0 C8 1 0.263691 0.088096 0.117068 11.00000 0.02801 0.02913 = 0.02046 0.00524 0.00477 0.00744 C9 1 0.028161 -0.062602 0.224510 11.00000 0.03343 0.02895 = 0.01768 0.00328 0.00267 -0.00150 C10 1 -0.095250 -0.009490 0.193565 11.00000 0.03468 0.03626 = 0.02685 0.00146 0.00873 0.00100 AFIX 137 H10A 2 -0.091001 0.069543 0.213921 11.00000 -1.50000 H10B 2 -0.167972 -0.055456 0.206496 11.00000 -1.50000 H10C 2 -0.105403 -0.008720 0.140562 11.00000 -1.50000 AFIX 0 C11 1 0.034816 -0.064035 0.307340 11.00000 0.04678 0.05261 = 0.02334 0.00718 0.00823 -0.00820 AFIX 137 H11A 2 0.106977 -0.105061 0.329186 11.00000 -1.50000 H11B 2 -0.044203 -0.103205 0.317396 11.00000 -1.50000 H11C 2 0.045905 0.015252 0.328081 11.00000 -1.50000 AFIX 0 C12 1 0.022869 -0.187380 0.195596 11.00000 0.04145 0.02558 = 0.03696 0.00644 0.00096 -0.00311 AFIX 137 H12A 2 0.021161 -0.189064 0.143121 11.00000 -1.50000 H12B 2 -0.054052 -0.230933 0.205267 11.00000 -1.50000 H12C 2 0.098107 -0.222127 0.219864 11.00000 -1.50000 AFIX 0 C13 1 0.482066 0.132413 0.304448 11.00000 0.02797 0.03049 = 0.02579 0.00004 -0.00182 0.00342 C14 1 0.480818 0.262641 0.319559 11.00000 0.04194 0.03306 = 0.03737 -0.00117 -0.00249 0.00123 AFIX 137 H14A 2 0.401886 0.277467 0.335947 11.00000 -1.50000 H14B 2 0.485914 0.302854 0.274976 11.00000 -1.50000 H14C 2 0.553861 0.290589 0.357384 11.00000 -1.50000 AFIX 0 C15 1 0.476460 0.071014 0.374485 11.00000 0.03763 0.03894 = 0.02745 0.00369 -0.00687 0.00332 AFIX 137 H15A 2 0.400168 0.088913 0.392766 11.00000 -1.50000 H15B 2 0.552281 0.097030 0.410899 11.00000 -1.50000 H15C 2 0.473330 -0.012357 0.364798 11.00000 -1.50000 AFIX 0 C16 1 0.609142 0.110912 0.281573 11.00000 0.03111 0.05643 = 0.03954 -0.00418 0.00020 0.00524 AFIX 137 H16A 2 0.679632 0.135228 0.321761 11.00000 -1.50000 H16B 2 0.618995 0.155185 0.239119 11.00000 -1.50000 H16C 2 0.609581 0.028653 0.269295 11.00000 -1.50000 AFIX 0 C17 1 0.269332 0.126576 0.041615 11.00000 0.02565 0.03367 = 0.02556 0.00516 0.00708 0.00422 AFIX 23 H17A 2 0.358842 0.151004 0.038713 11.00000 -1.20000 H17B 2 0.239513 0.060535 0.006246 11.00000 -1.20000 AFIX 0 N18 4 0.190273 0.223711 0.021140 11.00000 0.03132 0.02739 = 0.01582 0.00291 0.00342 0.00043 C19 1 0.225159 0.271193 -0.044784 11.00000 0.03824 0.03473 = 0.02086 0.00607 0.00545 -0.00022 AFIX 23 H19A 2 0.203237 0.211875 -0.085244 11.00000 -1.20000 H19B 2 0.318156 0.292445 -0.036466 11.00000 -1.20000 AFIX 0 C20 1 0.156097 0.376546 -0.065363 11.00000 0.05482 0.03297 = 0.02727 0.00452 0.00313 -0.00063 AFIX 23 H20A 2 0.179450 0.405787 -0.110584 11.00000 -1.20000 H20B 2 0.063141 0.354781 -0.074811 11.00000 -1.20000 AFIX 0 O21 5 0.187458 0.465309 -0.009061 11.00000 0.05995 0.02673 = 0.03472 0.00437 0.00620 -0.00345 C22 1 0.151893 0.421463 0.054988 11.00000 0.05349 0.02863 = 0.03346 0.00066 0.00810 0.00133 AFIX 23 H22A 2 0.058862 0.400177 0.045880 11.00000 -1.20000 H22B 2 0.172276 0.482369 0.094538 11.00000 -1.20000 AFIX 0 C23 1 0.219672 0.317458 0.078686 11.00000 0.04103 0.03171 = 0.02393 -0.00199 0.00482 -0.00178 AFIX 23 H23A 2 0.312619 0.339240 0.089806 11.00000 -1.20000 H23B 2 0.193138 0.289856 0.123495 11.00000 -1.20000 AFIX 0 MOLE 2 LI51 3 0.051296 0.493669 0.443451 11.00000 0.03029 0.02972 = 0.02990 0.00505 0.00328 0.00573 O52 5 -0.083073 0.578641 0.467237 11.00000 0.02476 0.02907 = 0.02564 0.00374 0.00016 0.00760 C53 1 -0.177621 0.605599 0.415856 11.00000 0.02123 0.02676 = 0.02255 0.00584 0.00558 0.00331 C54 1 -0.228996 0.714552 0.414150 11.00000 0.02451 0.02313 = 0.02179 0.00121 0.00424 0.00325 C55 1 -0.325725 0.734209 0.356478 11.00000 0.02694 0.02559 = 0.02510 0.00419 0.00388 0.00546 AFIX 43 H55 2 -0.357355 0.807759 0.355457 11.00000 -1.20000 AFIX 0 C56 1 -0.379301 0.653156 0.300104 11.00000 0.02625 0.03042 = 0.02797 0.00312 0.00220 0.00284 C57 1 -0.329424 0.547625 0.303561 11.00000 0.02625 0.02825 = 0.02981 -0.00130 0.00122 -0.00049 AFIX 43 H57 2 -0.363773 0.489465 0.266808 11.00000 -1.20000 AFIX 0 C58 1 -0.231163 0.523162 0.358564 11.00000 0.02522 0.02318 = 0.02803 0.00181 0.00426 0.00258 C59 1 -0.183497 0.805984 0.477341 11.00000 0.02919 0.02796 = 0.02390 0.00200 0.00257 0.00774 C60 1 -0.224038 0.757750 0.545156 11.00000 0.03055 0.03810 = 0.02745 -0.00194 0.00603 0.00673 AFIX 137 H60A 2 -0.316996 0.743783 0.536949 11.00000 -1.50000 H60B 2 -0.194676 0.813305 0.586484 11.00000 -1.50000 H60C 2 -0.186472 0.685195 0.555574 11.00000 -1.50000 AFIX 0 C61 1 -0.038864 0.834572 0.491608 11.00000 0.03464 0.02992 = 0.02625 -0.00037 0.00337 0.00337 AFIX 137 H61A 2 -0.013479 0.889476 0.533582 11.00000 -1.50000 H61B 2 -0.013375 0.868635 0.448774 11.00000 -1.50000 H61C 2 0.002795 0.763893 0.501597 11.00000 -1.50000 AFIX 0 C62 1 -0.245069 0.918942 0.463755 11.00000 0.04351 0.03244 = 0.03602 -0.00439 -0.00353 0.01243 AFIX 137 H62A 2 -0.337522 0.904058 0.459055 11.00000 -1.50000 H62B 2 -0.225088 0.950376 0.418904 11.00000 -1.50000 H62C 2 -0.211920 0.974535 0.504628 11.00000 -1.50000 AFIX 0 PART 1 C63A 1 -0.483145 0.680180 0.236888 10.50000 0.03304 0.04005 = 0.02687 -0.00359 -0.00435 0.00652 C64A 1 -0.421172 0.778110 0.193147 10.50000 0.03985 0.06098 = 0.03065 0.00558 -0.01084 0.00582 AFIX 137 H64A 2 -0.349839 0.749404 0.174285 10.50000 -1.50000 H64B 2 -0.390372 0.846226 0.225700 10.50000 -1.50000 H64C 2 -0.485268 0.798804 0.152608 10.50000 -1.50000 AFIX 0 C65A 1 -0.593585 0.723268 0.260170 10.50000 0.03985 0.06098 = 0.03065 0.00558 -0.01084 0.00582 AFIX 137 H65A 2 -0.652934 0.744735 0.217655 10.50000 -1.50000 H65B 2 -0.565921 0.790950 0.293542 10.50000 -1.50000 H65C 2 -0.636061 0.663054 0.284948 10.50000 -1.50000 AFIX 0 C66A 1 -0.525188 0.580307 0.179400 10.50000 0.03985 0.06098 = 0.03065 0.00558 -0.01084 0.00582 AFIX 137 H66A 2 -0.593746 0.602448 0.141877 10.50000 -1.50000 H66B 2 -0.555786 0.512025 0.202551 10.50000 -1.50000 H66C 2 -0.452811 0.562833 0.157153 10.50000 -1.50000 AFIX 0 PART 2 C63B 1 -0.483145 0.680180 0.236888 10.50000 0.03304 0.04005 = 0.02687 -0.00359 -0.00435 0.00652 C64B 1 -0.549671 0.787077 0.251781 10.50000 0.05193 0.08702 = 0.06498 0.01087 -0.01961 0.01707 AFIX 137 H64D 2 -0.492004 0.856513 0.250217 10.50000 -1.50000 H64E 2 -0.572934 0.783830 0.299897 10.50000 -1.50000 H64F 2 -0.626595 0.789215 0.214748 10.50000 -1.50000 AFIX 0 C65B 1 -0.595421 0.580448 0.232052 10.50000 0.05193 0.08702 = 0.06498 0.01087 -0.01961 0.01707 AFIX 137 H65D 2 -0.668309 0.598086 0.195809 10.50000 -1.50000 H65E 2 -0.620747 0.574538 0.279536 10.50000 -1.50000 H65F 2 -0.566502 0.507168 0.217825 10.50000 -1.50000 AFIX 0 C66B 1 -0.439115 0.680048 0.172057 10.50000 0.05193 0.08702 = 0.06498 0.01087 -0.01961 0.01707 AFIX 137 H66D 2 -0.510023 0.687114 0.131853 10.50000 -1.50000 H66E 2 -0.401740 0.607805 0.165058 10.50000 -1.50000 H66F 2 -0.374364 0.745130 0.173295 10.50000 -1.50000 AFIX 0 C67 1 -0.174878 0.410245 0.353645 11.00000 0.02706 0.02586 = 0.03033 -0.00110 0.00178 -0.00160 AFIX 23 H67A 2 -0.167375 0.374810 0.401298 11.00000 -1.20000 H67B 2 -0.233405 0.357576 0.317484 11.00000 -1.20000 AFIX 0 PART 0 N68 4 -0.047481 0.422389 0.332625 11.00000 0.03075 0.02583 = 0.02423 0.00231 0.00595 0.00709 C73 1 -0.017604 0.307692 0.309462 11.00000 0.03644 0.02746 = 0.02978 -0.00180 0.00304 0.00855 AFIX 23 H73A 2 -0.087561 0.272855 0.270894 11.00000 -1.20000 H73B 2 -0.010940 0.257236 0.351131 11.00000 -1.20000 AFIX 0 C72 1 0.106163 0.314968 0.281061 11.00000 0.04807 0.03698 = 0.02934 0.00226 0.00748 0.01672 AFIX 23 H72A 2 0.176771 0.347223 0.320086 11.00000 -1.20000 H72B 2 0.124209 0.236709 0.266447 11.00000 -1.20000 AFIX 0 O71 5 0.098889 0.385836 0.220429 11.00000 0.05432 0.04562 = 0.02809 0.00104 0.01248 0.01847 C70 1 0.073033 0.497420 0.242227 11.00000 0.04882 0.03949 = 0.03322 0.00517 0.01365 0.01242 AFIX 23 H70A 2 0.069044 0.547423 0.200404 11.00000 -1.20000 H70B 2 0.143519 0.530907 0.280936 11.00000 -1.20000 AFIX 0 C69 1 -0.049888 0.495749 0.269803 11.00000 0.04092 0.03059 = 0.02960 0.00621 0.00850 0.00994 AFIX 23 H69A 2 -0.064052 0.575209 0.284358 11.00000 -1.20000 H69B 2 -0.121236 0.466033 0.230481 11.00000 -1.20000 AFIX 0 MOLE 3 O101 5 0.206398 0.579142 0.424801 11.00000 0.03043 0.03740 = 0.05009 0.00938 0.00516 0.00041 C102 1 0.198450 0.695652 0.403765 11.00000 0.04829 0.04047 = 0.04812 0.00695 0.01770 0.00316 AFIX 23 H10D 2 0.113929 0.721030 0.406792 11.00000 -1.20000 H10E 2 0.213437 0.703541 0.353522 11.00000 -1.20000 AFIX 0 C103 1 0.299659 0.763356 0.456374 11.00000 0.07492 0.04827 = 0.05301 -0.00375 0.00765 -0.00257 AFIX 23 H10F 2 0.271132 0.779577 0.502699 11.00000 -1.20000 H10G 2 0.326835 0.837059 0.436532 11.00000 -1.20000 AFIX 0 C104 1 0.405929 0.684412 0.466710 11.00000 0.03650 0.09260 = 0.04232 -0.00496 0.00232 -0.02686 AFIX 23 H10H 2 0.460324 0.698434 0.515425 11.00000 -1.20000 H10I 2 0.459504 0.695341 0.429285 11.00000 -1.20000 AFIX 0 C105 1 0.335009 0.563846 0.458510 11.00000 0.02805 0.06548 = 0.05449 0.01555 0.00066 0.00658 AFIX 23 H10J 2 0.373632 0.512069 0.427643 11.00000 -1.20000 H10K 2 0.337228 0.530520 0.506543 11.00000 -1.20000 AFIX 0 MOLE 4 C111 1 0.351507 -0.216549 -0.005699 11.00000 0.03834 0.17614 = 0.06210 0.02018 0.01218 0.02347 AFIX 23 H11D 2 0.401770 -0.283051 0.005272 11.00000 -1.20000 H11E 2 0.408631 -0.144578 0.006947 11.00000 -1.20000 AFIX 0 C112 1 0.288720 -0.222157 -0.084982 11.00000 0.05229 0.11084 = 0.05189 0.01341 0.02312 0.01332 AFIX 23 H11F 2 0.300790 -0.146507 -0.106408 11.00000 -1.20000 H11G 2 0.323942 -0.280720 -0.113014 11.00000 -1.20000 AFIX 0 C113 1 0.150908 -0.255034 -0.084412 11.00000 0.05396 0.04493 = 0.03229 -0.00214 0.00665 0.01280 AFIX 23 H11I 2 0.096179 -0.222309 -0.125552 11.00000 -1.20000 H11J 2 0.131970 -0.339841 -0.087560 11.00000 -1.20000 AFIX 0 O114 5 0.131412 -0.207357 -0.016709 11.00000 0.03441 0.04394 = 0.02823 -0.00216 0.00258 0.01477 C115 1 0.244595 -0.219609 0.035513 11.00000 0.03786 0.05123 = 0.03456 0.00275 -0.00027 0.01698 AFIX 23 H11K 2 0.236632 -0.293549 0.059443 11.00000 -1.20000 H11L 2 0.259607 -0.155867 0.073212 11.00000 -1.20000 HKLF 4 REM import in P -1 REM R1 = 0.0600 for 5702 Fo > 4sig(Fo) and 0.1245 for all 10200 data REM 523 parameters refined using 0 restraints END WGHT 0.0665 0.6076 REM Highest difference peak 0.37, deepest hole -0.44, 1-sigma level 0.05 Q1 1 -0.5665 0.7779 0.2636 11.00000 0.05 0.37 Q2 1 0.3765 0.7382 0.4273 11.00000 0.05 0.36 Q3 1 -0.4821 0.6123 0.1609 11.00000 0.05 0.36 Q4 1 -0.3949 0.7531 0.1862 11.00000 0.05 0.36 Q5 1 -0.5597 0.5710 0.1961 11.00000 0.05 0.33 Q6 1 0.2249 0.6139 0.4773 11.00000 0.05 0.33 Q7 1 -0.4615 0.8065 0.2104 11.00000 0.05 0.30 Q8 1 0.2947 -0.3068 -0.0747 11.00000 0.05 0.28 Q9 1 0.4520 0.6230 0.4365 11.00000 0.05 0.27 Q10 1 -0.6126 0.6602 0.2630 11.00000 0.05 0.27 Q11 1 0.0187 0.4662 0.3754 11.00000 0.05 0.26 Q12 1 -0.5958 0.5653 0.2514 11.00000 0.05 0.25 Q13 1 -0.4649 0.5096 0.1764 11.00000 0.05 0.23 Q14 1 -0.6549 0.6769 0.2242 11.00000 0.05 0.23 Q15 1 0.1385 0.0182 0.1668 11.00000 0.05 0.22 Q16 1 0.2315 0.7013 0.4622 11.00000 0.05 0.22 Q17 1 0.1018 -0.0262 0.2118 11.00000 0.05 0.21 Q18 1 0.4273 0.1065 0.2735 11.00000 0.05 0.20 Q19 1 0.3223 0.4786 0.4737 11.00000 0.05 0.20 Q20 1 0.4405 -0.2146 0.0282 11.00000 0.05 0.19 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.0051(3) -0.1108(3) -0.00419(19) 0.0269(8) Uani 1 1 d . . . O2 O 0.05360(13) -0.00030(12) 0.07566(7) 0.0243(3) Uani 1 1 d . . . C3 C 0.1501(2) 0.02882(17) 0.13047(11) 0.0230(5) Uani 1 1 d . . . C4 C 0.1460(2) 0.00368(17) 0.20413(11) 0.0224(5) Uani 1 1 d . . . C5 C 0.2550(2) 0.03598(18) 0.25730(11) 0.0247(5) Uani 1 1 d . . . H5 H 0.2515 0.0188 0.3061 0.03 Uiso 1 1 calc R . . C6 C 0.3675(2) 0.09131(18) 0.24350(11) 0.0255(5) Uani 1 1 d . . . C7 C 0.3681(2) 0.11728(19) 0.17217(12) 0.0278(5) Uani 1 1 d . . . H7 H 0.4426 0.1564 0.1605 0.033 Uiso 1 1 calc R . . C8 C 0.2637(2) 0.08810(18) 0.11707(11) 0.0255(5) Uani 1 1 d . . . C9 C 0.0282(2) -0.06260(18) 0.22451(11) 0.0272(5) Uani 1 1 d . . . C10 C -0.0952(2) -0.0095(2) 0.19357(12) 0.0324(5) Uani 1 1 d . . . H10A H -0.091 0.0695 0.2139 0.049 Uiso 1 1 calc R . . H10B H -0.168 -0.0555 0.2065 0.049 Uiso 1 1 calc R . . H10C H -0.1054 -0.0087 0.1406 0.049 Uiso 1 1 calc R . . C11 C 0.0348(3) -0.0640(2) 0.30734(12) 0.0414(6) Uani 1 1 d . . . H11A H 0.107 -0.1051 0.3292 0.062 Uiso 1 1 calc R . . H11B H -0.0442 -0.1032 0.3174 0.062 Uiso 1 1 calc R . . H11C H 0.0459 0.0153 0.3281 0.062 Uiso 1 1 calc R . . C12 C 0.0229(2) -0.18738(19) 0.19560(13) 0.0357(6) Uani 1 1 d . . . H12A H 0.0212 -0.1891 0.1431 0.054 Uiso 1 1 calc R . . H12B H -0.0541 -0.2309 0.2053 0.054 Uiso 1 1 calc R . . H12C H 0.0981 -0.2221 0.2199 0.054 Uiso 1 1 calc R . . C13 C 0.4821(2) 0.13241(19) 0.30445(12) 0.0289(5) Uani 1 1 d . . . C14 C 0.4808(2) 0.2626(2) 0.31956(14) 0.0389(6) Uani 1 1 d . . . H14A H 0.4019 0.2775 0.3359 0.058 Uiso 1 1 calc R . . H14B H 0.4859 0.3029 0.275 0.058 Uiso 1 1 calc R . . H14C H 0.5539 0.2906 0.3574 0.058 Uiso 1 1 calc R . . C15 C 0.4765(2) 0.0710(2) 0.37449(12) 0.0363(6) Uani 1 1 d . . . H15A H 0.4002 0.0889 0.3928 0.054 Uiso 1 1 calc R . . H15B H 0.5523 0.097 0.4109 0.054 Uiso 1 1 calc R . . H15C H 0.4733 -0.0124 0.3648 0.054 Uiso 1 1 calc R . . C16 C 0.6091(2) 0.1109(2) 0.28157(14) 0.0433(7) Uani 1 1 d . . . H16A H 0.6796 0.1352 0.3218 0.065 Uiso 1 1 calc R . . H16B H 0.619 0.1552 0.2391 0.065 Uiso 1 1 calc R . . H16C H 0.6096 0.0287 0.2693 0.065 Uiso 1 1 calc R . . C17 C 0.2693(2) 0.12658(19) 0.04162(12) 0.0278(5) Uani 1 1 d . . . H17A H 0.3588 0.151 0.0387 0.033 Uiso 1 1 calc R . . H17B H 0.2395 0.0605 0.0062 0.033 Uiso 1 1 calc R . . N18 N 0.19027(17) 0.22371(15) 0.02114(9) 0.0251(4) Uani 1 1 d . . . C19 C 0.2252(2) 0.2712(2) -0.04478(12) 0.0314(5) Uani 1 1 d . . . H19A H 0.2032 0.2119 -0.0852 0.038 Uiso 1 1 calc R . . H19B H 0.3182 0.2924 -0.0365 0.038 Uiso 1 1 calc R . . C20 C 0.1561(3) 0.3765(2) -0.06536(13) 0.0392(6) Uani 1 1 d . . . H20A H 0.1794 0.4058 -0.1106 0.047 Uiso 1 1 calc R . . H20B H 0.0631 0.3548 -0.0748 0.047 Uiso 1 1 calc R . . O21 O 0.18746(17) 0.46531(13) -0.00906(9) 0.0412(4) Uani 1 1 d . . . C22 C 0.1519(3) 0.4215(2) 0.05499(13) 0.0387(6) Uani 1 1 d . . . H22A H 0.0589 0.4002 0.0459 0.046 Uiso 1 1 calc R . . H22B H 0.1723 0.4824 0.0945 0.046 Uiso 1 1 calc R . . C23 C 0.2197(2) 0.31746(19) 0.07869(12) 0.0328(6) Uani 1 1 d . . . H23A H 0.3126 0.3392 0.0898 0.039 Uiso 1 1 calc R . . H23B H 0.1931 0.2899 0.1235 0.039 Uiso 1 1 calc R . . Li51 Li 0.0513(4) 0.4937(3) 0.4435(2) 0.0300(9) Uani 1 1 d . . . O52 O -0.08307(14) 0.57864(12) 0.46724(8) 0.0267(4) Uani 1 1 d . . . C53 C -0.1776(2) 0.60560(18) 0.41586(11) 0.0232(5) Uani 1 1 d . . . C54 C -0.2290(2) 0.71455(18) 0.41415(11) 0.0231(5) Uani 1 1 d . B . C55 C -0.3257(2) 0.73421(18) 0.35648(11) 0.0258(5) Uani 1 1 d . . . H55 H -0.3574 0.8078 0.3555 0.031 Uiso 1 1 calc R B . C56 C -0.3793(2) 0.65316(19) 0.30010(12) 0.0285(5) Uani 1 1 d . A . C57 C -0.3294(2) 0.54763(19) 0.30356(12) 0.0289(5) Uani 1 1 d . . . H57 H -0.3638 0.4895 0.2668 0.035 Uiso 1 1 calc R B . C58 C -0.2312(2) 0.52316(18) 0.35856(12) 0.0255(5) Uani 1 1 d . B . C59 C -0.1835(2) 0.80598(19) 0.47734(12) 0.0270(5) Uani 1 1 d . . . C60 C -0.2240(2) 0.7578(2) 0.54516(12) 0.0318(5) Uani 1 1 d . B . H60A H -0.317 0.7438 0.5369 0.048 Uiso 1 1 calc R . . H60B H -0.1947 0.8133 0.5865 0.048 Uiso 1 1 calc R . . H60C H -0.1865 0.6852 0.5556 0.048 Uiso 1 1 calc R . . C61 C -0.0389(2) 0.8346(2) 0.49161(12) 0.0306(5) Uani 1 1 d . B . H61A H -0.0135 0.8895 0.5336 0.046 Uiso 1 1 calc R . . H61B H -0.0134 0.8686 0.4488 0.046 Uiso 1 1 calc R . . H61C H 0.0028 0.7639 0.5016 0.046 Uiso 1 1 calc R . . C62 C -0.2451(2) 0.9189(2) 0.46375(13) 0.0383(6) Uani 1 1 d . B . H62A H -0.3375 0.9041 0.4591 0.057 Uiso 1 1 calc R . . H62B H -0.2251 0.9504 0.4189 0.057 Uiso 1 1 calc R . . H62C H -0.2119 0.9745 0.5046 0.057 Uiso 1 1 calc R . . C63A C -0.4831(2) 0.6802(2) 0.23689(13) 0.0345(6) Uani 0.5 1 d P A 1 C64A C -0.4212(5) 0.7781(5) 0.1931(3) 0.0459(8) Uani 0.5 1 d P A 1 H64A H -0.3498 0.7494 0.1743 0.069 Uiso 0.5 1 calc PR A 1 H64B H -0.3904 0.8462 0.2257 0.069 Uiso 0.5 1 calc PR A 1 H64C H -0.4853 0.7988 0.1526 0.069 Uiso 0.5 1 calc PR A 1 C65A C -0.5936(5) 0.7233(6) 0.2602(3) 0.0459(8) Uani 0.5 1 d P A 1 H65A H -0.6529 0.7447 0.2177 0.069 Uiso 0.5 1 calc PR A 1 H65B H -0.5659 0.791 0.2935 0.069 Uiso 0.5 1 calc PR A 1 H65C H -0.6361 0.6631 0.2849 0.069 Uiso 0.5 1 calc PR A 1 C66A C -0.5252(5) 0.5803(5) 0.1794(3) 0.0459(8) Uani 0.5 1 d P A 1 H66A H -0.5937 0.6024 0.1419 0.069 Uiso 0.5 1 calc PR A 1 H66B H -0.5558 0.512 0.2026 0.069 Uiso 0.5 1 calc PR A 1 H66C H -0.4528 0.5628 0.1572 0.069 Uiso 0.5 1 calc PR A 1 C63B C -0.4831(2) 0.6802(2) 0.23689(13) 0.0345(6) Uani 0.5 1 d P A 2 C64B C -0.5497(7) 0.7871(7) 0.2518(4) 0.0711(12) Uani 0.5 1 d P A 2 H64D H -0.492 0.8565 0.2502 0.107 Uiso 0.5 1 calc PR A 2 H64E H -0.5729 0.7838 0.2999 0.107 Uiso 0.5 1 calc PR A 2 H64F H -0.6266 0.7892 0.2147 0.107 Uiso 0.5 1 calc PR A 2 C65B C -0.5954(6) 0.5804(6) 0.2321(4) 0.0711(12) Uani 0.5 1 d P A 2 H65D H -0.6683 0.5981 0.1958 0.107 Uiso 0.5 1 calc PR A 2 H65E H -0.6207 0.5745 0.2795 0.107 Uiso 0.5 1 calc PR A 2 H65F H -0.5665 0.5072 0.2178 0.107 Uiso 0.5 1 calc PR A 2 C66B C -0.4391(6) 0.6800(7) 0.1721(4) 0.0711(12) Uani 0.5 1 d P A 2 H66D H -0.51 0.6871 0.1319 0.107 Uiso 0.5 1 calc PR A 2 H66E H -0.4017 0.6078 0.1651 0.107 Uiso 0.5 1 calc PR A 2 H66F H -0.3744 0.7451 0.1733 0.107 Uiso 0.5 1 calc PR A 2 C67 C -0.1749(2) 0.41025(18) 0.35364(12) 0.0285(5) Uani 1 1 d . B 2 H67A H -0.1674 0.3748 0.4013 0.034 Uiso 1 1 calc R B 2 H67B H -0.2334 0.3576 0.3175 0.034 Uiso 1 1 calc R B 2 N68 N -0.04748(17) 0.42239(15) 0.33263(9) 0.0265(4) Uani 1 1 d . B . C73 C -0.0176(2) 0.30769(19) 0.30946(13) 0.0314(5) Uani 1 1 d . . . H73A H -0.0876 0.2729 0.2709 0.038 Uiso 1 1 calc R B . H73B H -0.0109 0.2572 0.3511 0.038 Uiso 1 1 calc R . . C72 C 0.1062(2) 0.3150(2) 0.28106(13) 0.0373(6) Uani 1 1 d . B . H72A H 0.1768 0.3472 0.3201 0.045 Uiso 1 1 calc R . . H72B H 0.1242 0.2367 0.2664 0.045 Uiso 1 1 calc R . . O71 O 0.09889(17) 0.38584(14) 0.22043(8) 0.0413(4) Uani 1 1 d . . . C70 C 0.0730(3) 0.4974(2) 0.24223(14) 0.0392(6) Uani 1 1 d . B . H70A H 0.069 0.5474 0.2004 0.047 Uiso 1 1 calc R . . H70B H 0.1435 0.5309 0.2809 0.047 Uiso 1 1 calc R . . C69 C -0.0499(2) 0.4957(2) 0.26980(12) 0.0330(6) Uani 1 1 d . . . H69A H -0.0641 0.5752 0.2844 0.04 Uiso 1 1 calc R B . H69B H -0.1212 0.466 0.2305 0.04 Uiso 1 1 calc R . . O101 O 0.20640(15) 0.57914(14) 0.42480(9) 0.0396(4) Uani 1 1 d . B . C102 C 0.1984(3) 0.6957(2) 0.40376(15) 0.0445(7) Uani 1 1 d . . . H10D H 0.1139 0.721 0.4068 0.053 Uiso 1 1 calc R B . H10E H 0.2134 0.7035 0.3535 0.053 Uiso 1 1 calc R . . C103 C 0.2997(3) 0.7634(3) 0.45637(17) 0.0599(8) Uani 1 1 d . B . H10F H 0.2711 0.7796 0.5027 0.072 Uiso 1 1 calc R . . H10G H 0.3268 0.8371 0.4365 0.072 Uiso 1 1 calc R . . C104 C 0.4059(3) 0.6844(3) 0.46671(16) 0.0600(9) Uani 1 1 d . . . H10H H 0.4603 0.6984 0.5154 0.072 Uiso 1 1 calc R B . H10I H 0.4595 0.6953 0.4293 0.072 Uiso 1 1 calc R . . C105 C 0.3350(2) 0.5638(3) 0.45851(16) 0.0498(7) Uani 1 1 d . B . H10J H 0.3736 0.5121 0.4276 0.06 Uiso 1 1 calc R . . H10K H 0.3372 0.5305 0.5065 0.06 Uiso 1 1 calc R . . C111 C 0.3515(3) -0.2165(4) -0.00570(19) 0.0907(13) Uani 1 1 d . . . H11D H 0.4018 -0.2831 0.0053 0.109 Uiso 1 1 calc R . . H11E H 0.4086 -0.1446 0.0069 0.109 Uiso 1 1 calc R . . C112 C 0.2887(3) -0.2222(3) -0.08498(17) 0.0694(10) Uani 1 1 d . . . H11F H 0.3008 -0.1465 -0.1064 0.083 Uiso 1 1 calc R . . H11G H 0.3239 -0.2807 -0.113 0.083 Uiso 1 1 calc R . . C113 C 0.1509(3) -0.2550(2) -0.08441(14) 0.0435(7) Uani 1 1 d . . . H11I H 0.0962 -0.2223 -0.1256 0.052 Uiso 1 1 calc R . . H11J H 0.132 -0.3398 -0.0876 0.052 Uiso 1 1 calc R . . O114 O 0.13141(15) -0.20736(14) -0.01671(8) 0.0354(4) Uani 1 1 d . . . C115 C 0.2446(2) -0.2196(2) 0.03551(14) 0.0413(6) Uani 1 1 d . . . H11K H 0.2366 -0.2935 0.0594 0.05 Uiso 1 1 calc R . . H11L H 0.2596 -0.1559 0.0732 0.05 Uiso 1 1 calc R . . 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 0.029(2) 0.029(2) 0.0228(19) 0.0032(15) 0.0038(16) 0.0010(16) O2 0.0261(8) 0.0275(8) 0.0167(7) 0.0010(6) -0.0019(6) 0.0009(6) C3 0.0263(12) 0.0222(11) 0.0201(11) 0.0009(9) 0.0016(9) 0.0057(9) C4 0.0266(12) 0.0177(11) 0.0217(11) 0.0032(8) 0.0011(9) 0.0024(9) C5 0.0345(13) 0.0244(12) 0.0149(10) 0.0034(9) 0.0017(10) 0.0058(10) C6 0.0266(12) 0.0242(12) 0.0242(12) 0.0031(9) -0.0009(10) 0.0061(10) C7 0.0245(12) 0.0307(13) 0.0278(12) 0.0058(10) 0.0036(10) 0.0008(10) C8 0.0280(13) 0.0291(12) 0.0205(11) 0.0052(9) 0.0048(10) 0.0074(10) C9 0.0334(13) 0.0290(12) 0.0177(11) 0.0033(9) 0.0027(10) -0.0015(10) C10 0.0347(14) 0.0363(14) 0.0269(12) 0.0015(10) 0.0087(11) 0.0010(11) C11 0.0468(16) 0.0526(16) 0.0233(13) 0.0072(11) 0.0082(12) -0.0082(13) C12 0.0415(15) 0.0256(13) 0.0370(14) 0.0064(11) 0.0010(12) -0.0031(11) C13 0.0280(13) 0.0305(13) 0.0258(12) 0.0000(10) -0.0018(10) 0.0034(10) C14 0.0419(15) 0.0331(14) 0.0374(14) -0.0012(11) -0.0025(12) 0.0012(11) C15 0.0376(15) 0.0389(14) 0.0274(13) 0.0037(11) -0.0069(11) 0.0033(11) C16 0.0311(14) 0.0564(17) 0.0395(15) -0.0042(13) 0.0002(12) 0.0052(12) C17 0.0256(12) 0.0337(13) 0.0256(12) 0.0052(10) 0.0071(10) 0.0042(10) N18 0.0313(11) 0.0274(10) 0.0158(9) 0.0029(7) 0.0034(8) 0.0004(8) C19 0.0382(14) 0.0347(13) 0.0209(11) 0.0061(10) 0.0054(10) -0.0002(11) C20 0.0548(17) 0.0330(14) 0.0273(13) 0.0045(11) 0.0031(12) -0.0006(12) O21 0.0600(12) 0.0267(9) 0.0347(10) 0.0044(7) 0.0062(9) -0.0035(8) C22 0.0535(17) 0.0286(13) 0.0335(14) 0.0007(11) 0.0081(12) 0.0013(12) C23 0.0410(15) 0.0317(13) 0.0239(12) -0.0020(10) 0.0048(11) -0.0018(11) Li51 0.030(2) 0.030(2) 0.030(2) 0.0050(16) 0.0033(17) 0.0057(17) O52 0.0248(8) 0.0291(8) 0.0256(8) 0.0037(6) 0.0002(7) 0.0076(7) C53 0.0212(12) 0.0268(12) 0.0226(11) 0.0058(9) 0.0056(9) 0.0033(9) C54 0.0245(12) 0.0231(11) 0.0218(11) 0.0012(9) 0.0042(9) 0.0033(9) C55 0.0269(12) 0.0256(12) 0.0251(12) 0.0042(9) 0.0039(10) 0.0055(10) C56 0.0262(12) 0.0304(13) 0.0280(12) 0.0031(10) 0.0022(10) 0.0028(10) C57 0.0263(13) 0.0282(13) 0.0298(13) -0.0013(10) 0.0012(10) -0.0005(10) C58 0.0252(12) 0.0232(12) 0.0280(12) 0.0018(9) 0.0043(10) 0.0026(9) C59 0.0292(13) 0.0280(12) 0.0239(12) 0.0020(9) 0.0026(10) 0.0077(10) C60 0.0305(13) 0.0381(14) 0.0275(12) -0.0019(10) 0.0060(10) 0.0067(11) C61 0.0346(14) 0.0299(13) 0.0262(12) -0.0004(10) 0.0034(10) 0.0034(10) C62 0.0435(15) 0.0324(14) 0.0360(14) -0.0044(11) -0.0035(12) 0.0124(11) C63A 0.0330(14) 0.0400(14) 0.0269(13) -0.0036(11) -0.0044(11) 0.0065(11) C64A 0.0399(19) 0.061(2) 0.0306(16) 0.0056(15) -0.0108(14) 0.0058(16) C65A 0.0399(19) 0.061(2) 0.0306(16) 0.0056(15) -0.0108(14) 0.0058(16) C66A 0.0399(19) 0.061(2) 0.0306(16) 0.0056(15) -0.0108(14) 0.0058(16) C63B 0.0330(14) 0.0400(14) 0.0269(13) -0.0036(11) -0.0044(11) 0.0065(11) C64B 0.052(2) 0.087(3) 0.065(3) 0.011(2) -0.020(2) 0.017(2) C65B 0.052(2) 0.087(3) 0.065(3) 0.011(2) -0.020(2) 0.017(2) C66B 0.052(2) 0.087(3) 0.065(3) 0.011(2) -0.020(2) 0.017(2) C67 0.0271(13) 0.0259(12) 0.0303(12) -0.0011(10) 0.0018(10) -0.0016(10) N68 0.0308(11) 0.0258(10) 0.0242(10) 0.0023(8) 0.0059(8) 0.0071(8) C73 0.0364(14) 0.0275(13) 0.0298(13) -0.0018(10) 0.0030(11) 0.0086(10) C72 0.0481(16) 0.0370(14) 0.0293(13) 0.0023(11) 0.0075(12) 0.0167(12) O71 0.0543(12) 0.0456(11) 0.0281(9) 0.0010(8) 0.0125(8) 0.0185(9) C70 0.0488(16) 0.0395(15) 0.0332(14) 0.0052(11) 0.0137(12) 0.0124(12) C69 0.0409(15) 0.0306(13) 0.0296(13) 0.0062(10) 0.0085(11) 0.0099(11) O101 0.0304(10) 0.0374(10) 0.0501(11) 0.0094(8) 0.0052(8) 0.0004(8) C102 0.0483(17) 0.0405(16) 0.0481(16) 0.0070(13) 0.0177(14) 0.0032(13) C103 0.075(2) 0.0483(18) 0.0530(19) -0.0037(15) 0.0076(17) -0.0026(16) C104 0.0365(17) 0.093(2) 0.0423(17) -0.0050(16) 0.0023(13) -0.0269(16) C105 0.0280(15) 0.0655(19) 0.0545(18) 0.0156(15) 0.0007(13) 0.0066(13) C111 0.0383(19) 0.176(4) 0.062(2) 0.020(2) 0.0122(17) 0.023(2) C112 0.052(2) 0.111(3) 0.0519(19) 0.0134(19) 0.0231(16) 0.0133(19) C113 0.0540(18) 0.0449(16) 0.0323(14) -0.0021(12) 0.0066(13) 0.0128(13) O114 0.0344(10) 0.0439(10) 0.0282(9) -0.0022(7) 0.0026(7) 0.0148(8) C115 0.0379(15) 0.0512(16) 0.0346(14) 0.0028(12) -0.0003(12) 0.0170(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O2 1.918(4) . ? Li1 O2 1.931(4) 2 ? Li1 O114 1.968(4) . ? Li1 N18 2.252(4) 2 ? Li1 Li1 2.576(7) 2 ? Li1 C17 2.784(4) 2 ? O2 C3 1.331(2) . ? O2 Li1 1.931(4) 2 ? C3 C8 1.416(3) . ? C3 C4 1.429(3) . ? C4 C5 1.405(3) . ? C4 C9 1.540(3) . ? C5 C6 1.390(3) . ? C5 H5 0.95 . ? C6 C7 1.382(3) . ? C6 C13 1.547(3) . ? C7 C8 1.388(3) . ? C7 H7 0.95 . ? C8 C17 1.508(3) . ? C9 C12 1.529(3) . ? C9 C10 1.538(3) . ? C9 C11 1.542(3) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C15 1.525(3) . ? C13 C14 1.538(3) . ? C13 C16 1.542(3) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 N18 1.494(3) . ? C17 Li1 2.784(4) 2 ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? N18 C19 1.467(3) . ? N18 C23 1.481(3) . ? N18 Li1 2.252(4) 2 ? C19 C20 1.516(3) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 O21 1.426(3) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? O21 C22 1.423(3) . ? C22 C23 1.508(3) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? Li51 O52 1.889(4) 2_566 ? Li51 O52 1.929(4) . ? Li51 O101 1.958(4) . ? Li51 N68 2.248(4) . ? Li51 Li51 2.567(8) 2_566 ? Li51 C67 2.768(5) . ? O52 C53 1.333(2) . ? O52 Li51 1.889(4) 2_566 ? C53 C58 1.420(3) . ? C53 C54 1.429(3) . ? C54 C55 1.396(3) . ? C54 C59 1.546(3) . ? C55 C56 1.399(3) . ? C55 H55 0.95 . ? C56 C57 1.384(3) . ? C56 C63A 1.534(3) . ? C57 C58 1.391(3) . ? C57 H57 0.95 . ? C58 C67 1.504(3) . ? C59 C60 1.526(3) . ? C59 C61 1.532(3) . ? C59 C62 1.534(3) . ? C60 H60A 0.98 . ? C60 H60B 0.98 . ? C60 H60C 0.98 . ? C61 H61A 0.98 . ? C61 H61B 0.98 . ? C61 H61C 0.98 . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? C63A C65A 1.459(6) . ? C63A C66A 1.539(6) . ? C63A C64A 1.597(6) . ? C64A H64A 0.98 . ? C64A H64B 0.98 . ? C64A H64C 0.98 . ? C65A H65A 0.98 . ? C65A H65B 0.98 . ? C65A H65C 0.98 . ? C66A H66A 0.98 . ? C66A H66B 0.98 . ? C66A H66C 0.98 . ? C64B H64D 0.98 . ? C64B H64E 0.98 . ? C64B H64F 0.98 . ? C65B H65D 0.98 . ? C65B H65E 0.98 . ? C65B H65F 0.98 . ? C66B H66D 0.98 . ? C66B H66E 0.98 . ? C66B H66F 0.98 . ? C67 N68 1.488(3) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? N68 C73 1.473(3) . ? N68 C69 1.477(3) . ? C73 C72 1.516(3) . ? C73 H73A 0.99 . ? C73 H73B 0.99 . ? C72 O71 1.423(3) . ? C72 H72A 0.99 . ? C72 H72B 0.99 . ? O71 C70 1.417(3) . ? C70 C69 1.502(3) . ? C70 H70A 0.99 . ? C70 H70B 0.99 . ? C69 H69A 0.99 . ? C69 H69B 0.99 . ? O101 C102 1.434(3) . ? O101 C105 1.439(3) . ? C102 C103 1.477(4) . ? C102 H10D 0.99 . ? C102 H10E 0.99 . ? C103 C104 1.518(4) . ? C103 H10F 0.99 . ? C103 H10G 0.99 . ? C104 C105 1.528(4) . ? C104 H10H 0.99 . ? C104 H10I 0.99 . ? C105 H10J 0.99 . ? C105 H10K 0.99 . ? C111 C115 1.495(4) . ? C111 C112 1.512(4) . ? C111 H11D 0.99 . ? C111 H11E 0.99 . ? C112 C113 1.498(4) . ? C112 H11F 0.99 . ? C112 H11G 0.99 . ? C113 O114 1.426(3) . ? C113 H11I 0.99 . ? C113 H11J 0.99 . ? O114 C115 1.436(3) . ? C115 H11K 0.99 . ? C115 H11L 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li1 O2 95.98(17) . 2 ? O2 Li1 O114 109.98(19) . . ? O2 Li1 O114 118.85(19) 2 . ? O2 Li1 N18 124.83(19) . 2 ? O2 Li1 N18 98.48(16) 2 2 ? O114 Li1 N18 108.51(17) . 2 ? O2 Li1 Li1 48.20(13) . 2 ? O2 Li1 Li1 47.78(12) 2 2 ? O114 Li1 Li1 128.0(2) . 2 ? N18 Li1 Li1 122.4(2) 2 2 ? O2 Li1 C17 110.22(16) . 2 ? O2 Li1 C17 70.92(12) 2 2 ? O114 Li1 C17 137.02(18) . 2 ? N18 Li1 C17 32.38(8) 2 2 ? Li1 Li1 C17 90.71(18) 2 2 ? C3 O2 Li1 142.63(17) . . ? C3 O2 Li1 119.30(16) . 2 ? Li1 O2 Li1 84.02(17) . 2 ? O2 C3 C8 119.88(18) . . ? O2 C3 C4 123.29(19) . . ? C8 C3 C4 116.84(19) . . ? C5 C4 C3 118.3(2) . . ? C5 C4 C9 120.55(18) . . ? C3 C4 C9 121.09(19) . . ? C6 C5 C4 124.60(19) . . ? C6 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C7 C6 C5 116.1(2) . . ? C7 C6 C13 120.9(2) . . ? C5 C6 C13 122.79(19) . . ? C6 C7 C8 122.2(2) . . ? C6 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C7 C8 C3 121.92(19) . . ? C7 C8 C17 118.8(2) . . ? C3 C8 C17 119.23(19) . . ? C12 C9 C10 110.78(19) . . ? C12 C9 C4 107.49(18) . . ? C10 C9 C4 112.10(17) . . ? C12 C9 C11 107.60(19) . . ? C10 C9 C11 106.19(19) . . ? C4 C9 C11 112.63(19) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 108.99(19) . . ? C15 C13 C16 107.62(19) . . ? C14 C13 C16 108.5(2) . . ? C15 C13 C6 112.07(19) . . ? C14 C13 C6 108.29(18) . . ? C16 C13 C6 111.31(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N18 C17 C8 112.79(17) . . ? N18 C17 Li1 53.80(12) . 2 ? C8 C17 Li1 91.74(15) . 2 ? N18 C17 H17A 109 . . ? C8 C17 H17A 109 . . ? Li1 C17 H17A 157.9 2 . ? N18 C17 H17B 109 . . ? C8 C17 H17B 109 . . ? Li1 C17 H17B 70.7 2 . ? H17A C17 H17B 107.8 . . ? C19 N18 C23 107.05(17) . . ? C19 N18 C17 107.99(17) . . ? C23 N18 C17 110.36(17) . . ? C19 N18 Li1 115.41(16) . 2 ? C23 N18 Li1 120.90(17) . 2 ? C17 N18 Li1 93.82(15) . 2 ? N18 C19 C20 110.89(19) . . ? N18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? N18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? O21 C20 C19 111.25(19) . . ? O21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? O21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108 . . ? C22 O21 C20 108.23(17) . . ? O21 C22 C23 111.8(2) . . ? O21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? O21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? N18 C23 C22 110.87(19) . . ? N18 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? N18 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? O52 Li51 O52 95.51(18) 2_566 . ? O52 Li51 O101 110.9(2) 2_566 . ? O52 Li51 O101 118.8(2) . . ? O52 Li51 N68 130.4(2) 2_566 . ? O52 Li51 N68 98.11(17) . . ? O101 Li51 N68 103.52(18) . . ? O52 Li51 Li51 48.42(13) 2_566 2_566 ? O52 Li51 Li51 47.09(13) . 2_566 ? O101 Li51 Li51 128.6(3) . 2_566 ? N68 Li51 Li51 125.6(2) . 2_566 ? O52 Li51 C67 113.96(18) 2_566 . ? O52 Li51 C67 71.39(13) . . ? O101 Li51 C67 132.61(19) . . ? N68 Li51 C67 32.46(8) . . ? Li51 Li51 C67 93.4(2) 2_566 . ? C53 O52 Li51 141.99(18) . 2_566 ? C53 O52 Li51 121.22(17) . . ? Li51 O52 Li51 84.49(18) 2_566 . ? O52 C53 C58 119.26(18) . . ? O52 C53 C54 123.78(19) . . ? C58 C53 C54 116.96(19) . . ? C55 C54 C53 118.73(19) . . ? C55 C54 C59 120.77(18) . . ? C53 C54 C59 120.40(18) . . ? C54 C55 C56 124.56(19) . . ? C54 C55 H55 117.7 . . ? C56 C55 H55 117.7 . . ? C57 C56 C55 115.6(2) . . ? C57 C56 C63A 121.8(2) . . ? C55 C56 C63A 122.49(19) . . ? C56 C57 C58 122.8(2) . . ? C56 C57 H57 118.6 . . ? C58 C57 H57 118.6 . . ? C57 C58 C53 121.30(19) . . ? C57 C58 C67 118.75(19) . . ? C53 C58 C67 119.79(19) . . ? C60 C59 C61 109.56(18) . . ? C60 C59 C62 107.09(19) . . ? C61 C59 C62 107.88(19) . . ? C60 C59 C54 107.65(18) . . ? C61 C59 C54 112.02(18) . . ? C62 C59 C54 112.52(18) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C65A C63A C56 113.6(3) . . ? C65A C63A C66A 110.5(4) . . ? C56 C63A C66A 114.0(3) . . ? C65A C63A C64A 107.9(4) . . ? C56 C63A C64A 107.0(3) . . ? C66A C63A C64A 103.2(3) . . ? H64D C64B H64E 109.5 . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? H65D C65B H65E 109.5 . . ? H65D C65B H65F 109.5 . . ? H65E C65B H65F 109.5 . . ? H66D C66B H66E 109.5 . . ? H66D C66B H66F 109.5 . . ? H66E C66B H66F 109.5 . . ? N68 C67 C58 113.09(18) . . ? N68 C67 Li51 54.20(13) . . ? C58 C67 Li51 92.68(15) . . ? N68 C67 H67A 109 . . ? C58 C67 H67A 109 . . ? Li51 C67 H67A 69.7 . . ? N68 C67 H67B 109 . . ? C58 C67 H67B 109 . . ? Li51 C67 H67B 157.4 . . ? H67A C67 H67B 107.8 . . ? C73 N68 C69 107.21(17) . . ? C73 N68 C67 108.46(17) . . ? C69 N68 C67 110.13(17) . . ? C73 N68 Li51 117.01(16) . . ? C69 N68 Li51 119.39(17) . . ? C67 N68 Li51 93.34(16) . . ? N68 C73 C72 111.33(19) . . ? N68 C73 H73A 109.4 . . ? C72 C73 H73A 109.4 . . ? N68 C73 H73B 109.4 . . ? C72 C73 H73B 109.4 . . ? H73A C73 H73B 108 . . ? O71 C72 C73 110.67(19) . . ? O71 C72 H72A 109.5 . . ? C73 C72 H72A 109.5 . . ? O71 C72 H72B 109.5 . . ? C73 C72 H72B 109.5 . . ? H72A C72 H72B 108.1 . . ? C70 O71 C72 108.81(17) . . ? O71 C70 C69 112.3(2) . . ? O71 C70 H70A 109.2 . . ? C69 C70 H70A 109.2 . . ? O71 C70 H70B 109.2 . . ? C69 C70 H70B 109.2 . . ? H70A C70 H70B 107.9 . . ? N68 C69 C70 110.83(19) . . ? N68 C69 H69A 109.5 . . ? C70 C69 H69A 109.5 . . ? N68 C69 H69B 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 108.1 . . ? C102 O101 C105 109.81(19) . . ? C102 O101 Li51 117.65(18) . . ? C105 O101 Li51 126.57(19) . . ? O101 C102 C103 104.4(2) . . ? O101 C102 H10D 110.9 . . ? C103 C102 H10D 110.9 . . ? O101 C102 H10E 110.9 . . ? C103 C102 H10E 110.9 . . ? H10D C102 H10E 108.9 . . ? C102 C103 C104 102.7(2) . . ? C102 C103 H10F 111.2 . . ? C104 C103 H10F 111.2 . . ? C102 C103 H10G 111.2 . . ? C104 C103 H10G 111.2 . . ? H10F C103 H10G 109.1 . . ? C103 C104 C105 103.5(2) . . ? C103 C104 H10H 111.1 . . ? C105 C104 H10H 111.1 . . ? C103 C104 H10I 111.1 . . ? C105 C104 H10I 111.1 . . ? H10H C104 H10I 109 . . ? O101 C105 C104 105.4(2) . . ? O101 C105 H10J 110.7 . . ? C104 C105 H10J 110.7 . . ? O101 C105 H10K 110.7 . . ? C104 C105 H10K 110.7 . . ? H10J C105 H10K 108.8 . . ? C115 C111 C112 105.3(2) . . ? C115 C111 H11D 110.7 . . ? C112 C111 H11D 110.7 . . ? C115 C111 H11E 110.7 . . ? C112 C111 H11E 110.7 . . ? H11D C111 H11E 108.8 . . ? C113 C112 C111 104.2(2) . . ? C113 C112 H11F 110.9 . . ? C111 C112 H11F 110.9 . . ? C113 C112 H11G 110.9 . . ? C111 C112 H11G 110.9 . . ? H11F C112 H11G 108.9 . . ? O114 C113 C112 104.5(2) . . ? O114 C113 H11I 110.8 . . ? C112 C113 H11I 110.8 . . ? O114 C113 H11J 110.8 . . ? C112 C113 H11J 110.8 . . ? H11I C113 H11J 108.9 . . ? C113 O114 C115 106.73(17) . . ? C113 O114 Li1 125.27(18) . . ? C115 O114 Li1 126.45(17) . . ? O114 C115 C111 106.4(2) . . ? O114 C115 H11K 110.4 . . ? C111 C115 H11K 110.4 . . ? O114 C115 H11L 110.4 . . ? C111 C115 H11L 110.4 . . ? H11K C115 H11L 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Li1 O2 C3 -132.3(3) 2 . . . ? O114 Li1 O2 C3 -8.7(4) . . . . ? N18 Li1 O2 C3 123.0(3) 2 . . . ? Li1 Li1 O2 C3 -132.4(3) 2 . . . ? C17 Li1 O2 C3 155.8(2) 2 . . . ? O2 Li1 O2 Li1 0 2 . . 2 ? O114 Li1 O2 Li1 123.7(2) . . . 2 ? N18 Li1 O2 Li1 -104.7(3) 2 . . 2 ? C17 Li1 O2 Li1 -71.83(15) 2 . . 2 ? Li1 O2 C3 C8 78.0(3) . . . . ? Li1 O2 C3 C8 -44.5(3) 2 . . . ? Li1 O2 C3 C4 -102.2(3) . . . . ? Li1 O2 C3 C4 135.2(2) 2 . . . ? O2 C3 C4 C5 178.36(18) . . . . ? C8 C3 C4 C5 -1.9(3) . . . . ? O2 C3 C4 C9 1.5(3) . . . . ? C8 C3 C4 C9 -178.74(18) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C9 C4 C5 C6 177.04(19) . . . . ? C4 C5 C6 C7 1.4(3) . . . . ? C4 C5 C6 C13 175.87(19) . . . . ? C5 C6 C7 C8 -1.2(3) . . . . ? C13 C6 C7 C8 -175.8(2) . . . . ? C6 C7 C8 C3 -0.6(3) . . . . ? C6 C7 C8 C17 176.01(19) . . . . ? O2 C3 C8 C7 -178.10(19) . . . . ? C4 C3 C8 C7 2.1(3) . . . . ? O2 C3 C8 C17 5.3(3) . . . . ? C4 C3 C8 C17 -174.46(18) . . . . ? C5 C4 C9 C12 -106.2(2) . . . . ? C3 C4 C9 C12 70.6(2) . . . . ? C5 C4 C9 C10 131.8(2) . . . . ? C3 C4 C9 C10 -51.4(3) . . . . ? C5 C4 C9 C11 12.1(3) . . . . ? C3 C4 C9 C11 -171.0(2) . . . . ? C7 C6 C13 C15 -166.0(2) . . . . ? C5 C6 C13 C15 19.7(3) . . . . ? C7 C6 C13 C14 73.7(3) . . . . ? C5 C6 C13 C14 -100.5(2) . . . . ? C7 C6 C13 C16 -45.5(3) . . . . ? C5 C6 C13 C16 140.3(2) . . . . ? C7 C8 C17 N18 -105.9(2) . . . . ? C3 C8 C17 N18 70.8(3) . . . . ? C7 C8 C17 Li1 -157.00(19) . . . 2 ? C3 C8 C17 Li1 19.7(2) . . . 2 ? C8 C17 N18 C19 167.17(18) . . . . ? Li1 C17 N18 C19 -118.29(18) 2 . . . ? C8 C17 N18 C23 50.5(2) . . . . ? Li1 C17 N18 C23 125.01(19) 2 . . . ? C8 C17 N18 Li1 -74.5(2) . . . 2 ? C23 N18 C19 C20 -56.6(2) . . . . ? C17 N18 C19 C20 -175.44(19) . . . . ? Li1 N18 C19 C20 81.2(2) 2 . . . ? N18 C19 C20 O21 60.5(3) . . . . ? C19 C20 O21 C22 -59.6(3) . . . . ? C20 O21 C22 C23 59.5(3) . . . . ? C19 N18 C23 C22 56.2(2) . . . . ? C17 N18 C23 C22 173.46(19) . . . . ? Li1 N18 C23 C22 -78.8(2) 2 . . . ? O21 C22 C23 N18 -59.6(3) . . . . ? O52 Li51 O52 C53 -150.13(19) 2_566 . . . ? O101 Li51 O52 C53 92.4(3) . . . . ? N68 Li51 O52 C53 -18.0(2) . . . . ? Li51 Li51 O52 C53 -150.13(19) 2_566 . . . ? C67 Li51 O52 C53 -36.68(18) . . . . ? O52 Li51 O52 Li51 0 2_566 . . 2_566 ? O101 Li51 O52 Li51 -117.5(3) . . . 2_566 ? N68 Li51 O52 Li51 132.1(2) . . . 2_566 ? C67 Li51 O52 Li51 113.45(17) . . . 2_566 ? Li51 O52 C53 C58 -85.9(3) 2_566 . . . ? Li51 O52 C53 C58 40.5(3) . . . . ? Li51 O52 C53 C54 94.7(3) 2_566 . . . ? Li51 O52 C53 C54 -138.9(2) . . . . ? O52 C53 C54 C55 178.24(19) . . . . ? C58 C53 C54 C55 -1.2(3) . . . . ? O52 C53 C54 C59 -5.3(3) . . . . ? C58 C53 C54 C59 175.35(19) . . . . ? C53 C54 C55 C56 1.6(3) . . . . ? C59 C54 C55 C56 -174.9(2) . . . . ? C54 C55 C56 C57 -0.5(3) . . . . ? C54 C55 C56 C63A -178.4(2) . . . . ? C55 C56 C57 C58 -0.9(3) . . . . ? C63A C56 C57 C58 176.9(2) . . . . ? C56 C57 C58 C53 1.3(3) . . . . ? C56 C57 C58 C67 -174.1(2) . . . . ? O52 C53 C58 C57 -179.64(19) . . . . ? C54 C53 C58 C57 -0.2(3) . . . . ? O52 C53 C58 C67 -4.3(3) . . . . ? C54 C53 C58 C67 175.16(19) . . . . ? C55 C54 C59 C60 111.5(2) . . . . ? C53 C54 C59 C60 -65.0(2) . . . . ? C55 C54 C59 C61 -128.0(2) . . . . ? C53 C54 C59 C61 55.5(3) . . . . ? C55 C54 C59 C62 -6.3(3) . . . . ? C53 C54 C59 C62 177.3(2) . . . . ? C57 C56 C63A C65A 127.8(4) . . . . ? C55 C56 C63A C65A -54.5(4) . . . . ? C57 C56 C63A C66A 0.2(4) . . . . ? C55 C56 C63A C66A 177.9(3) . . . . ? C57 C56 C63A C64A -113.2(3) . . . . ? C55 C56 C63A C64A 64.5(3) . . . . ? C57 C58 C67 N68 105.2(2) . . . . ? C53 C58 C67 N68 -70.3(3) . . . . ? C57 C58 C67 Li51 157.1(2) . . . . ? C53 C58 C67 Li51 -18.4(2) . . . . ? O52 Li51 C67 N68 -128.4(2) 2_566 . . . ? O52 Li51 C67 N68 143.77(19) . . . . ? O101 Li51 C67 N68 31.4(2) . . . . ? Li51 Li51 C67 N68 -173.9(2) 2_566 . . . ? O52 Li51 C67 C58 114.8(2) 2_566 . . . ? O52 Li51 C67 C58 27.00(15) . . . . ? O101 Li51 C67 C58 -85.4(3) . . . . ? N68 Li51 C67 C58 -116.77(19) . . . . ? Li51 Li51 C67 C58 69.3(2) 2_566 . . . ? C58 C67 N68 C73 -164.23(18) . . . . ? Li51 C67 N68 C73 119.94(19) . . . . ? C58 C67 N68 C69 -47.2(2) . . . . ? Li51 C67 N68 C69 -123.02(19) . . . . ? C58 C67 N68 Li51 75.8(2) . . . . ? O52 Li51 N68 C73 -42.8(3) 2_566 . . . ? O52 Li51 N68 C73 -147.15(17) . . . . ? O101 Li51 N68 C73 90.5(2) . . . . ? Li51 Li51 N68 C73 -105.2(3) 2_566 . . . ? C67 Li51 N68 C73 -112.7(2) . . . . ? O52 Li51 N68 C69 -174.7(2) 2_566 . . . ? O52 Li51 N68 C69 80.9(2) . . . . ? O101 Li51 N68 C69 -41.4(2) . . . . ? Li51 Li51 N68 C69 122.9(3) 2_566 . . . ? C67 Li51 N68 C69 115.4(2) . . . . ? O52 Li51 N68 C67 69.9(3) 2_566 . . . ? O52 Li51 N68 C67 -34.46(18) . . . . ? O101 Li51 N68 C67 -156.80(17) . . . . ? Li51 Li51 N68 C67 7.5(3) 2_566 . . . ? C69 N68 C73 C72 56.2(2) . . . . ? C67 N68 C73 C72 175.11(18) . . . . ? Li51 N68 C73 C72 -81.1(2) . . . . ? N68 C73 C72 O71 -59.8(3) . . . . ? C73 C72 O71 C70 59.2(3) . . . . ? C72 O71 C70 C69 -59.6(3) . . . . ? C73 N68 C69 C70 -55.4(2) . . . . ? C67 N68 C69 C70 -173.20(19) . . . . ? Li51 N68 C69 C70 80.7(2) . . . . ? O71 C70 C69 N68 59.1(3) . . . . ? O52 Li51 O101 C102 -131.1(2) 2_566 . . . ? O52 Li51 O101 C102 -22.0(3) . . . . ? N68 Li51 O101 C102 85.3(2) . . . . ? Li51 Li51 O101 C102 -78.3(3) 2_566 . . . ? C67 Li51 O101 C102 68.6(3) . . . . ? O52 Li51 O101 C105 18.8(3) 2_566 . . . ? O52 Li51 O101 C105 127.9(2) . . . . ? N68 Li51 O101 C105 -124.8(2) . . . . ? Li51 Li51 O101 C105 71.6(4) 2_566 . . . ? C67 Li51 O101 C105 -141.5(2) . . . . ? C105 O101 C102 C103 -28.8(3) . . . . ? Li51 O101 C102 C103 125.8(2) . . . . ? O101 C102 C103 C104 37.8(3) . . . . ? C102 C103 C104 C105 -32.8(3) . . . . ? C102 O101 C105 C104 7.4(3) . . . . ? Li51 O101 C105 C104 -144.4(2) . . . . ? C103 C104 C105 O101 16.1(3) . . . . ? C115 C111 C112 C113 -12.5(4) . . . . ? C111 C112 C113 O114 30.1(3) . . . . ? C112 C113 O114 C115 -37.1(3) . . . . ? C112 C113 O114 Li1 129.4(2) . . . . ? O2 Li1 O114 C113 -147.2(2) . . . . ? O2 Li1 O114 C113 -38.1(3) 2 . . . ? N18 Li1 O114 C113 73.1(3) 2 . . . ? Li1 Li1 O114 C113 -95.3(3) 2 . . . ? C17 Li1 O114 C113 54.4(3) 2 . . . ? O2 Li1 O114 C115 16.6(3) . . . . ? O2 Li1 O114 C115 125.7(2) 2 . . . ? N18 Li1 O114 C115 -123.1(2) 2 . . . ? Li1 Li1 O114 C115 68.6(4) 2 . . . ? C17 Li1 O114 C115 -141.8(2) 2 . . . ? C113 O114 C115 C111 29.0(3) . . . . ? Li1 O114 C115 C111 -137.3(3) . . . . ? C112 C111 C115 O114 -9.3(4) . . . . ? data_job _database_code_depnum_ccdc_archive 'CCDC 885950' #TrackingRef 'archive.cif' _audit_creation_date 2011-10-20T14:12:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H42 Li N O5' _chemical_formula_sum 'C25 H42 Li N O5' _chemical_formula_weight 443.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 15.9897(10) _cell_length_b 9.9413(7) _cell_length_c 16.3045(14) _cell_angle_alpha 90 _cell_angle_beta 95.297(4) _cell_angle_gamma 90 _cell_volume 2580.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7544 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.49 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.982 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0424 _diffrn_reflns_number 20944 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 5845 _reflns_number_gt 4619 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0710P)^2^+0.4156P] 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_number_reflns 5845 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.32 _refine_diff_density_min -0.33 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C18 C 0.39851(9) 0.54042(14) -0.06241(9) 0.0254(3) Uani 1 1 d . . . H18A H 0.3497 0.5433 -0.1025 0.03 Uiso 1 1 calc R . . H18B H 0.4482 0.5283 -0.0915 0.03 Uiso 1 1 calc R . . O19 O 0.39086(6) 0.43276(9) -0.00579(6) 0.0240(2) Uani 1 1 d . . . C20 C 0.36004(9) 0.31206(15) -0.04466(10) 0.0300(3) Uani 1 1 d . . . H20A H 0.3959 0.2845 -0.0865 0.036 Uiso 1 1 calc R . . H20B H 0.3036 0.3254 -0.0705 0.036 Uiso 1 1 calc R . . C21 C 0.36028(10) 0.20805(15) 0.02115(10) 0.0348(4) Uani 1 1 d . . . H21A H 0.3302 0.1284 0.0006 0.042 Uiso 1 1 calc R . . H21B H 0.4174 0.1826 0.04 0.042 Uiso 1 1 calc R . . O22 O 0.32004(7) 0.26640(10) 0.08636(7) 0.0342(3) Uani 1 1 d . . . C23 C 0.28827(10) 0.17119(15) 0.14097(11) 0.0362(4) Uani 1 1 d . . . H23A H 0.3318 0.1076 0.1602 0.043 Uiso 1 1 calc R . . H23B H 0.2416 0.1218 0.1132 0.043 Uiso 1 1 calc R . . C24 C 0.25977(10) 0.25001(15) 0.21230(10) 0.0340(4) Uani 1 1 d . . . H24A H 0.2208 0.1956 0.2403 0.041 Uiso 1 1 calc R . . H24B H 0.308 0.2689 0.2512 0.041 Uiso 1 1 calc R . . O25 O 0.21995(6) 0.37384(10) 0.18734(7) 0.0312(3) Uani 1 1 d . . . C26 C 0.14276(9) 0.36184(16) 0.13708(10) 0.0331(4) Uani 1 1 d . . . H26A H 0.0989 0.3282 0.169 0.04 Uiso 1 1 calc R . . H26B H 0.1487 0.3006 0.0916 0.04 Uiso 1 1 calc R . . C27 C 0.12185(9) 0.50056(16) 0.10568(10) 0.0324(4) Uani 1 1 d . . . H27A H 0.069 0.4997 0.0714 0.039 Uiso 1 1 calc R . . H27B H 0.1167 0.5615 0.1514 0.039 Uiso 1 1 calc R . . Li1 Li 0.31624(14) 0.4847(2) 0.10311(15) 0.0246(5) Uani 1 1 d . . . C1 C 0.43711(7) 0.63677(12) 0.20762(8) 0.0168(3) Uani 1 1 d . . . C2 C 0.43160(7) 0.75881(12) 0.16174(8) 0.0175(3) Uani 1 1 d . . . C3 C 0.49272(8) 0.85869(12) 0.17397(8) 0.0175(3) Uani 1 1 d . . . H3 H 0.4872 0.9366 0.1424 0.021 Uiso 1 1 calc R . . C4 C 0.56171(8) 0.84559(12) 0.23193(8) 0.0172(3) Uani 1 1 d . . . C5 C 0.56631(7) 0.72649(12) 0.27809(8) 0.0171(3) Uani 1 1 d . . . H5 H 0.6116 0.7159 0.3177 0.021 Uiso 1 1 calc R . . C6 C 0.50752(8) 0.62303(11) 0.26851(8) 0.0163(3) Uani 1 1 d . . . C7 C 0.62884(8) 0.95511(12) 0.24763(8) 0.0202(3) Uani 1 1 d . . . C8 C 0.71726(8) 0.89485(15) 0.24586(10) 0.0275(3) Uani 1 1 d . . . H8A H 0.7585 0.9641 0.2574 0.041 Uiso 1 1 calc R . . H8B H 0.723 0.8575 0.1924 0.041 Uiso 1 1 calc R . . H8C H 0.7254 0.8253 0.2867 0.041 Uiso 1 1 calc R . . C9 C 0.61924(9) 1.06619(14) 0.18232(9) 0.0284(3) Uani 1 1 d . . . H9A H 0.5659 1.1097 0.1844 0.043 Uiso 1 1 calc R . . H9B H 0.6224 1.0275 0.1287 0.043 Uiso 1 1 calc R . . H9C H 0.6634 1.131 0.1929 0.043 Uiso 1 1 calc R . . C10 C 0.62094(9) 1.01917(13) 0.33212(9) 0.0255(3) Uani 1 1 d . . . H10A H 0.5662 1.0586 0.333 0.038 Uiso 1 1 calc R . . H10B H 0.663 1.0876 0.3422 0.038 Uiso 1 1 calc R . . H10C H 0.6287 0.9514 0.3741 0.038 Uiso 1 1 calc R . . C11 C 0.51471(8) 0.49692(12) 0.32326(8) 0.0197(3) Uani 1 1 d . . . C12 C 0.52018(10) 0.37062(13) 0.27018(9) 0.0280(3) Uani 1 1 d . . . H12A H 0.4736 0.3688 0.2286 0.042 Uiso 1 1 calc R . . H12B H 0.5186 0.2921 0.3043 0.042 Uiso 1 1 calc R . . H12C H 0.5718 0.3718 0.2444 0.042 Uiso 1 1 calc R . . C13 C 0.43723(9) 0.48728(14) 0.37238(9) 0.0267(3) Uani 1 1 d . . . H13A H 0.4347 0.5652 0.4068 0.04 Uiso 1 1 calc R . . H13B H 0.4413 0.4079 0.406 0.04 Uiso 1 1 calc R . . H13C H 0.3873 0.4827 0.3349 0.04 Uiso 1 1 calc R . . C14 C 0.59226(9) 0.49917(14) 0.38591(9) 0.0269(3) Uani 1 1 d . . . H14A H 0.6419 0.5075 0.3574 0.04 Uiso 1 1 calc R . . H14B H 0.5948 0.4172 0.4171 0.04 Uiso 1 1 calc R . . H14C H 0.5886 0.5743 0.4224 0.04 Uiso 1 1 calc R . . C15 C 0.35492(8) 0.78666(12) 0.10285(8) 0.0200(3) Uani 1 1 d . . . H15A H 0.3067 0.7955 0.1345 0.024 Uiso 1 1 calc R . . H15B H 0.3627 0.8723 0.0761 0.024 Uiso 1 1 calc R . . C17 C 0.40511(8) 0.66861(13) -0.01307(8) 0.0219(3) Uani 1 1 d . . . H17A H 0.4578 0.669 0.0216 0.026 Uiso 1 1 calc R . . H17B H 0.4055 0.7446 -0.0504 0.026 Uiso 1 1 calc R . . O28 O 0.18820(6) 0.54348(9) 0.05880(6) 0.0256(2) Uani 1 1 d . . . C29 C 0.18117(8) 0.68155(13) 0.03608(9) 0.0249(3) Uani 1 1 d . . . H29A H 0.1802 0.7373 0.0848 0.03 Uiso 1 1 calc R . . H29B H 0.1296 0.6966 0.0011 0.03 Uiso 1 1 calc R . . C30 C 0.25619(8) 0.71693(13) -0.00963(8) 0.0231(3) Uani 1 1 d . . . H30A H 0.2529 0.668 -0.0613 0.028 Uiso 1 1 calc R . . H30B H 0.2549 0.8123 -0.0222 0.028 Uiso 1 1 calc R . . N16 N 0.33564(6) 0.68418(10) 0.03875(7) 0.0184(2) Uani 1 1 d . . . O1 O 0.37927(5) 0.54476(9) 0.19612(6) 0.0217(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C18 0.0277(7) 0.0332(7) 0.0154(7) 0.0026(6) 0.0025(5) 0.0042(5) O19 0.0294(5) 0.0225(5) 0.0199(5) -0.0025(4) 0.0017(4) 0.0006(4) C20 0.0301(8) 0.0315(8) 0.0292(8) -0.0128(6) 0.0064(6) -0.0010(6) C21 0.0396(9) 0.0262(7) 0.0408(10) -0.0096(7) 0.0159(7) -0.0030(6) O22 0.0451(6) 0.0250(5) 0.0355(6) -0.0040(4) 0.0201(5) -0.0064(4) C23 0.0415(9) 0.0278(8) 0.0412(10) 0.0042(7) 0.0151(7) -0.0066(6) C24 0.0363(9) 0.0339(8) 0.0330(9) 0.0065(7) 0.0097(7) -0.0045(6) O25 0.0278(5) 0.0310(6) 0.0349(6) -0.0005(5) 0.0038(4) -0.0054(4) C26 0.0254(7) 0.0396(9) 0.0349(9) -0.0008(7) 0.0064(6) -0.0119(6) C27 0.0191(7) 0.0422(9) 0.0372(9) -0.0008(7) 0.0088(6) -0.0030(6) Li1 0.0253(12) 0.0233(11) 0.0249(13) -0.0035(9) 0.0001(9) -0.0006(9) C1 0.0187(6) 0.0157(6) 0.0162(6) -0.0017(5) 0.0031(5) 0.0003(4) C2 0.0188(6) 0.0172(6) 0.0164(6) -0.0012(5) 0.0008(5) 0.0024(4) C3 0.0223(6) 0.0140(6) 0.0161(6) 0.0025(5) 0.0019(5) 0.0021(4) C4 0.0188(6) 0.0166(6) 0.0164(6) -0.0007(5) 0.0022(5) 0.0001(4) C5 0.0173(6) 0.0187(6) 0.0153(6) 0.0005(5) 0.0007(5) 0.0029(4) C6 0.0197(6) 0.0145(6) 0.0152(6) 0.0007(5) 0.0040(5) 0.0030(4) C7 0.0218(6) 0.0191(6) 0.0193(7) 0.0016(5) -0.0006(5) -0.0028(5) C8 0.0220(7) 0.0309(7) 0.0296(8) -0.0014(6) 0.0033(6) -0.0042(5) C9 0.0343(8) 0.0239(7) 0.0262(8) 0.0037(6) -0.0021(6) -0.0109(6) C10 0.0297(7) 0.0219(6) 0.0240(8) -0.0022(5) -0.0022(6) -0.0020(5) C11 0.0246(7) 0.0174(6) 0.0172(7) 0.0038(5) 0.0030(5) 0.0011(5) C12 0.0402(8) 0.0166(6) 0.0273(8) 0.0030(6) 0.0040(6) 0.0046(5) C13 0.0316(8) 0.0268(7) 0.0225(7) 0.0063(6) 0.0070(6) -0.0017(5) C14 0.0308(8) 0.0262(7) 0.0234(8) 0.0093(6) 0.0000(6) 0.0029(5) C15 0.0228(7) 0.0167(6) 0.0198(7) 0.0005(5) -0.0014(5) 0.0020(5) C17 0.0206(6) 0.0262(7) 0.0189(7) 0.0062(5) 0.0023(5) 0.0008(5) O28 0.0204(5) 0.0264(5) 0.0310(6) 0.0004(4) 0.0074(4) 0.0000(4) C29 0.0195(7) 0.0260(7) 0.0282(8) -0.0031(6) -0.0029(5) 0.0035(5) C30 0.0223(7) 0.0246(7) 0.0211(7) 0.0022(5) -0.0053(5) 0.0021(5) N16 0.0159(5) 0.0216(5) 0.0170(6) 0.0002(4) -0.0017(4) 0.0014(4) O1 0.0244(5) 0.0193(5) 0.0209(5) 0.0017(4) -0.0003(4) -0.0056(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C18 O19 1.4260(17) . ? C18 C17 1.5056(19) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? O19 C20 1.4236(16) . ? O19 Li1 2.288(3) . ? C20 C21 1.490(2) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 O22 1.4168(19) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? O22 C23 1.4248(18) . ? O22 Li1 2.189(2) . ? C23 C24 1.507(2) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 O25 1.4278(18) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? O25 C26 1.4221(17) . ? O25 Li1 2.421(3) . ? C26 C27 1.498(2) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 O28 1.4289(17) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? Li1 O1 1.841(2) . ? Li1 O28 2.187(2) . ? Li1 N16 2.278(3) . ? C1 O1 1.3020(14) . ? C1 C2 1.4238(17) . ? C1 C6 1.4371(16) . ? C2 C3 1.3946(17) . ? C2 C15 1.5115(16) . ? C3 C4 1.3908(17) . ? C3 H3 0.93 . ? C4 C5 1.4012(17) . ? C4 C7 1.5338(17) . ? C5 C6 1.3925(17) . ? C5 H5 0.93 . ? C6 C11 1.5371(17) . ? C7 C9 1.5319(19) . ? C7 C10 1.5334(19) . ? C7 C8 1.5382(19) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 C12 1.5320(18) . ? C11 C14 1.5323(18) . ? C11 C13 1.5391(19) . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 N16 1.4717(16) . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C17 N16 1.4647(17) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? O28 C29 1.4235(16) . ? C29 C30 1.511(2) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 N16 1.4687(15) . ? C30 H30A 0.97 . ? C30 H30B 0.97 . ? 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 O19 C18 C17 107.18(11) . . ? O19 C18 H18A 110.3 . . ? C17 C18 H18A 110.3 . . ? O19 C18 H18B 110.3 . . ? C17 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? C20 O19 C18 113.03(11) . . ? C20 O19 Li1 110.60(10) . . ? C18 O19 Li1 114.52(9) . . ? O19 C20 C21 106.65(12) . . ? O19 C20 H20A 110.4 . . ? C21 C20 H20A 110.4 . . ? O19 C20 H20B 110.4 . . ? C21 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? O22 C21 C20 106.57(12) . . ? O22 C21 H21A 110.4 . . ? C20 C21 H21A 110.4 . . ? O22 C21 H21B 110.4 . . ? C20 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? C21 O22 C23 114.19(11) . . ? C21 O22 Li1 121.28(11) . . ? C23 O22 Li1 124.41(11) . . ? O22 C23 C24 106.70(12) . . ? O22 C23 H23A 110.4 . . ? C24 C23 H23A 110.4 . . ? O22 C23 H23B 110.4 . . ? C24 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? O25 C24 C23 112.76(13) . . ? O25 C24 H24A 109 . . ? C23 C24 H24A 109 . . ? O25 C24 H24B 109 . . ? C23 C24 H24B 109 . . ? H24A C24 H24B 107.8 . . ? C26 O25 C24 115.62(11) . . ? C26 O25 Li1 105.95(10) . . ? C24 O25 Li1 105.30(10) . . ? O25 C26 C27 105.91(11) . . ? O25 C26 H26A 110.6 . . ? C27 C26 H26A 110.6 . . ? O25 C26 H26B 110.6 . . ? C27 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? O28 C27 C26 107.72(12) . . ? O28 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? O28 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O1 Li1 O28 127.59(13) . . ? O1 Li1 O22 113.89(12) . . ? O28 Li1 O22 105.05(10) . . ? O1 Li1 N16 90.55(10) . . ? O28 Li1 N16 77.19(8) . . ? O22 Li1 N16 143.04(13) . . ? O1 Li1 O19 115.30(11) . . ? O28 Li1 O19 110.08(11) . . ? O22 Li1 O19 69.94(8) . . ? N16 Li1 O19 74.69(8) . . ? O1 Li1 O25 90.50(11) . . ? O28 Li1 O25 71.58(8) . . ? O22 Li1 O25 69.26(8) . . ? N16 Li1 O25 141.10(11) . . ? O19 Li1 O25 137.91(10) . . ? O1 C1 C2 120.95(11) . . ? O1 C1 C6 122.24(11) . . ? C2 C1 C6 116.78(10) . . ? C3 C2 C1 121.53(11) . . ? C3 C2 C15 118.49(11) . . ? C1 C2 C15 119.81(11) . . ? C4 C3 C2 122.14(11) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 116.30(11) . . ? C3 C4 C7 123.09(11) . . ? C5 C4 C7 120.59(11) . . ? C6 C5 C4 124.23(11) . . ? C6 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C5 C6 C1 119.01(11) . . ? C5 C6 C11 121.59(11) . . ? C1 C6 C11 119.37(10) . . ? C9 C7 C10 108.29(11) . . ? C9 C7 C4 111.83(10) . . ? C10 C7 C4 109.29(11) . . ? C9 C7 C8 107.52(12) . . ? C10 C7 C8 109.32(11) . . ? C4 C7 C8 110.53(10) . . ? 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 . . ? C12 C11 C14 107.68(11) . . ? C12 C11 C6 110.21(11) . . ? C14 C11 C6 112.82(10) . . ? C12 C11 C13 109.49(11) . . ? C14 C11 C13 107.14(11) . . ? C6 C11 C13 109.41(10) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N16 C15 C2 115.39(10) . . ? N16 C15 H15A 108.4 . . ? C2 C15 H15A 108.4 . . ? N16 C15 H15B 108.4 . . ? C2 C15 H15B 108.4 . . ? H15A C15 H15B 107.5 . . ? N16 C17 C18 112.22(11) . . ? N16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C29 O28 C27 112.49(10) . . ? C29 O28 Li1 113.13(9) . . ? C27 O28 Li1 117.53(11) . . ? O28 C29 C30 107.80(10) . . ? O28 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? O28 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.5 . . ? N16 C30 C29 111.72(11) . . ? N16 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? N16 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C17 N16 C30 112.22(10) . . ? C17 N16 C15 111.25(10) . . ? C30 N16 C15 110.00(10) . . ? C17 N16 Li1 108.45(10) . . ? C30 N16 Li1 107.01(9) . . ? C15 N16 Li1 107.70(10) . . ? C1 O1 Li1 132.38(11) . . ? data_SR42 _database_code_depnum_ccdc_archive 'CCDC 905220' #TrackingRef 'SR42_150K_28mar12_APEX_VD_archive.cif' _audit_creation_date 2012-03-29T14:18:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H84 K2 N2 O10' _chemical_formula_sum 'C50 H84 K2 N2 O10' _chemical_formula_weight 951.39 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 17.3807(5) _cell_length_b 17.0158(5) _cell_length_c 20.0753(5) _cell_angle_alpha 90 _cell_angle_beta 111.7240(10) _cell_angle_gamma 90 _cell_volume 5515.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9998 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.4 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description stick _exptl_crystal_colour stick _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 0.982 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_number 46530 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 12537 _reflns_number_gt 8806 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0408P)^2^+1.9134P] 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_number_reflns 12537 _refine_ls_number_parameters 590 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.458 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 K1 K 0.11973(2) 0.23989(2) 0.970833(19) 0.02526(9) Uani 1 1 d . . . K2 K 0.34457(2) 0.29969(2) 1.012003(19) 0.02814(10) Uani 1 1 d . . . O1 O 0.24642(7) 0.29417(7) 1.08191(6) 0.0249(3) Uani 1 1 d . . . O2 O 0.20034(7) 0.31114(7) 0.90069(6) 0.0254(3) Uani 1 1 d . . . N1 N 0.15520(9) 0.12584(8) 1.08915(7) 0.0264(3) Uani 1 1 d . . . C2 C 0.08665(11) 0.11715(11) 1.11471(10) 0.0339(4) Uani 1 1 d . . . H2A H 0.1096 0.0994 1.1652 0.041 Uiso 1 1 calc R . . H2B H 0.0492 0.0754 1.0863 0.041 Uiso 1 1 calc R . . C3 C 0.03644(11) 0.19033(13) 1.11037(10) 0.0377(5) Uani 1 1 d . . . H3A H -0.0025 0.1817 1.1353 0.045 Uiso 1 1 calc R . . H3B H 0.0736 0.2344 1.1342 0.045 Uiso 1 1 calc R . . O4 O -0.00837(8) 0.20910(8) 1.03722(7) 0.0404(3) Uani 1 1 d . . . C5 C -0.04537(14) 0.28479(14) 1.03110(12) 0.0516(6) Uani 1 1 d . . . H5A H -0.002 0.3254 1.0504 0.062 Uiso 1 1 calc R . . H5B H -0.0822 0.2865 1.0587 0.062 Uiso 1 1 calc R . . C6 C -0.09396(14) 0.29992(16) 0.95379(14) 0.0614(7) Uani 1 1 d . . . H6A H -0.1331 0.2561 0.9332 0.074 Uiso 1 1 calc R . . H6B H -0.1263 0.349 0.9483 0.074 Uiso 1 1 calc R . . O7 O -0.03794(8) 0.30683(9) 0.91709(7) 0.0445(4) Uani 1 1 d . . . C8 C -0.07500(14) 0.29300(13) 0.84191(11) 0.0491(6) Uani 1 1 d . . . H8A H -0.04 0.3168 0.818 0.059 Uiso 1 1 calc R . . H8B H -0.1298 0.3191 0.8229 0.059 Uiso 1 1 calc R . . C9 C -0.08579(13) 0.20705(13) 0.82411(13) 0.0526(6) Uani 1 1 d . . . H9A H -0.1187 0.182 0.8494 0.063 Uiso 1 1 calc R . . H9B H -0.1155 0.1999 0.7719 0.063 Uiso 1 1 calc R . . O10 O -0.00524(8) 0.17169(8) 0.84623(7) 0.0387(3) Uani 1 1 d . . . C11 C -0.01016(12) 0.08884(12) 0.84147(11) 0.0413(5) Uani 1 1 d . . . H11A H -0.0425 0.0728 0.7915 0.05 Uiso 1 1 calc R . . H11B H -0.0385 0.0684 0.8725 0.05 Uiso 1 1 calc R . . C12 C 0.07592(12) 0.05577(12) 0.86492(10) 0.0404(5) Uani 1 1 d . . . H12A H 0.0723 -0.0022 0.8604 0.048 Uiso 1 1 calc R . . H12B H 0.1026 0.0753 0.8322 0.048 Uiso 1 1 calc R . . O13 O 0.12693(8) 0.07563(7) 0.93678(6) 0.0337(3) Uani 1 1 d . . . C14 C 0.11145(14) 0.02838(12) 0.98904(10) 0.0422(5) Uani 1 1 d . . . H14A H 0.1175 -0.0279 0.9794 0.051 Uiso 1 1 calc R . . H14B H 0.0542 0.0372 0.9867 0.051 Uiso 1 1 calc R . . C15 C 0.17234(13) 0.05002(11) 1.06225(10) 0.0369(4) Uani 1 1 d . . . H15A H 0.1721 0.0083 1.0965 0.044 Uiso 1 1 calc R . . H15B H 0.2285 0.0518 1.0606 0.044 Uiso 1 1 calc R . . C16 C 0.23258(10) 0.15290(10) 1.14731(9) 0.0271(4) Uani 1 1 d . . . H16A H 0.2773 0.1562 1.128 0.033 Uiso 1 1 calc R . . H16B H 0.2493 0.1133 1.1862 0.033 Uiso 1 1 calc R . . C17 C 0.22413(10) 0.23119(10) 1.17834(8) 0.0241(4) Uani 1 1 d . . . C18 C 0.23000(9) 0.29985(10) 1.13967(8) 0.0217(3) Uani 1 1 d . . . C19 C 0.21409(10) 0.37377(10) 1.16707(8) 0.0247(4) Uani 1 1 d . . . C20 C 0.19149(11) 0.37373(11) 1.22673(9) 0.0289(4) Uani 1 1 d . . . H20 H 0.1792 0.4229 1.243 0.035 Uiso 1 1 calc R . . C21 C 0.18557(10) 0.30617(11) 1.26443(9) 0.0289(4) Uani 1 1 d . . . C22 C 0.20437(10) 0.23565(11) 1.23972(9) 0.0275(4) Uani 1 1 d . . . H22 H 0.2038 0.1888 1.2652 0.033 Uiso 1 1 calc R . . C23 C 0.21991(12) 0.45063(11) 1.12925(9) 0.0313(4) Uani 1 1 d . . . C24 C 0.15704(13) 0.45028(12) 1.05155(10) 0.0409(5) Uani 1 1 d . . . H24A H 0.1692 0.4064 1.0254 0.061 Uiso 1 1 calc R . . H24B H 0.1609 0.4999 1.0282 0.061 Uiso 1 1 calc R . . H24C H 0.101 0.4444 1.0516 0.061 Uiso 1 1 calc R . . C25 C 0.30806(12) 0.46004(12) 1.12934(11) 0.0402(5) Uani 1 1 d . . . H25A H 0.3469 0.4694 1.1784 0.06 Uiso 1 1 calc R . . H25B H 0.3094 0.5047 1.0989 0.06 Uiso 1 1 calc R . . H25C H 0.3239 0.412 1.1107 0.06 Uiso 1 1 calc R . . C26 C 0.20299(16) 0.52301(12) 1.16673(12) 0.0518(6) Uani 1 1 d . . . H26A H 0.1452 0.5224 1.1631 0.078 Uiso 1 1 calc R . . H26B H 0.2132 0.5706 1.1438 0.078 Uiso 1 1 calc R . . H26C H 0.2397 0.5225 1.2174 0.078 Uiso 1 1 calc R . . C27 C 0.15188(12) 0.31295(13) 1.32498(10) 0.0380(5) Uani 1 1 d . . . C28 C 0.06195(14) 0.34334(15) 1.29264(13) 0.0566(6) Uani 1 1 d . . . H28A H 0.0607 0.3933 1.268 0.085 Uiso 1 1 calc R . . H28B H 0.0407 0.3513 1.3311 0.085 Uiso 1 1 calc R . . H28C H 0.0274 0.3047 1.2584 0.085 Uiso 1 1 calc R . . C29 C 0.20352(16) 0.37153(16) 1.38195(12) 0.0587(7) Uani 1 1 d . . . H29A H 0.2609 0.3531 1.4029 0.088 Uiso 1 1 calc R . . H29B H 0.1806 0.3759 1.4197 0.088 Uiso 1 1 calc R . . H29C H 0.202 0.4231 1.3597 0.088 Uiso 1 1 calc R . . C30 C 0.15200(14) 0.23415(14) 1.36156(11) 0.0476(6) Uani 1 1 d . . . H30A H 0.1161 0.197 1.3265 0.071 Uiso 1 1 calc R . . H30B H 0.1314 0.2416 1.4005 0.071 Uiso 1 1 calc R . . H30C H 0.2086 0.2133 1.3812 0.071 Uiso 1 1 calc R . . N31 N 0.33976(9) 0.17636(9) 0.90915(7) 0.0288(3) Uani 1 1 d . . . C32 C 0.35285(14) 0.10117(12) 0.94791(11) 0.0428(5) Uani 1 1 d . . . H32A H 0.3608 0.0594 0.9167 0.051 Uiso 1 1 calc R . . H32B H 0.3023 0.0882 0.9573 0.051 Uiso 1 1 calc R . . C33 C 0.42582(16) 0.10051(15) 1.01807(11) 0.0583(7) Uani 1 1 d . . . H33A H 0.4337 0.047 1.0388 0.07 Uiso 1 1 calc R . . H33B H 0.4767 0.1155 1.0099 0.07 Uiso 1 1 calc R . . O34 O 0.41182(10) 0.15408(10) 1.06630(7) 0.0558(4) Uani 1 1 d . . . C35 C 0.4800(2) 0.15613(18) 1.13425(13) 0.0856(10) Uani 1 1 d . . . H35A H 0.5322 0.1662 1.1265 0.103 Uiso 1 1 calc R . . H35B H 0.485 0.1047 1.1585 0.103 Uiso 1 1 calc R . . C36 C 0.46661(19) 0.21795(18) 1.17932(12) 0.0727(8) Uani 1 1 d . . . H36A H 0.4139 0.2073 1.1859 0.087 Uiso 1 1 calc R . . H36B H 0.5117 0.2154 1.2271 0.087 Uiso 1 1 calc R . . O37 O 0.46370(9) 0.29503(10) 1.15204(7) 0.0537(4) Uani 1 1 d . . . C38 C 0.54093(13) 0.33310(16) 1.16790(11) 0.0556(7) Uani 1 1 d . . . H38A H 0.5758 0.3027 1.1478 0.067 Uiso 1 1 calc R . . H38B H 0.5704 0.3368 1.2205 0.067 Uiso 1 1 calc R . . C39 C 0.52532(14) 0.41269(16) 1.13596(11) 0.0537(6) Uani 1 1 d . . . H39A H 0.4891 0.4418 1.1556 0.064 Uiso 1 1 calc R . . H39B H 0.5785 0.4414 1.1499 0.064 Uiso 1 1 calc R . . O40 O 0.48718(8) 0.41108(9) 1.05959(7) 0.0439(4) Uani 1 1 d . . . C41 C 0.54476(12) 0.40314(14) 1.02453(11) 0.0471(5) Uani 1 1 d . . . H41A H 0.5866 0.3627 1.0491 0.057 Uiso 1 1 calc R . . H41B H 0.5737 0.4536 1.0263 0.057 Uiso 1 1 calc R . . C42 C 0.49866(13) 0.37969(13) 0.94829(11) 0.0427(5) Uani 1 1 d . . . H42A H 0.4507 0.415 0.9261 0.051 Uiso 1 1 calc R . . H42B H 0.5354 0.3839 0.9207 0.051 Uiso 1 1 calc R . . O43 O 0.47090(8) 0.30082(8) 0.94692(7) 0.0369(3) Uani 1 1 d . . . C44 C 0.42614(11) 0.27457(12) 0.87539(10) 0.0341(4) Uani 1 1 d . . . H44A H 0.4607 0.2804 0.846 0.041 Uiso 1 1 calc R . . H44B H 0.3754 0.3065 0.8533 0.041 Uiso 1 1 calc R . . C45 C 0.40359(11) 0.18960(12) 0.87821(10) 0.0348(4) Uani 1 1 d . . . H45A H 0.3835 0.1679 0.829 0.042 Uiso 1 1 calc R . . H45B H 0.4541 0.1602 0.9069 0.042 Uiso 1 1 calc R . . C46 C 0.25531(10) 0.17550(10) 0.85269(9) 0.0269(4) Uani 1 1 d . . . H46A H 0.2145 0.1669 0.8757 0.032 Uiso 1 1 calc R . . H46B H 0.2511 0.1305 0.8202 0.032 Uiso 1 1 calc R . . C47 C 0.23267(10) 0.24935(10) 0.80879(8) 0.0233(3) Uani 1 1 d . . . C48 C 0.20695(9) 0.31595(10) 0.83826(8) 0.0218(3) Uani 1 1 d . . . C49 C 0.19110(10) 0.38717(10) 0.79667(8) 0.0243(4) Uani 1 1 d . . . C50 C 0.20269(10) 0.38716(11) 0.73148(9) 0.0272(4) Uani 1 1 d . A . H50 H 0.1931 0.4349 0.7051 0.033 Uiso 1 1 calc R . . C51 C 0.22741(10) 0.32164(11) 0.70233(9) 0.0270(4) Uani 1 1 d . . . C52 C 0.24115(10) 0.25274(11) 0.74250(9) 0.0259(4) Uani 1 1 d . A . H52 H 0.2568 0.2066 0.7241 0.031 Uiso 1 1 calc R . . C53 C 0.16608(11) 0.46238(11) 0.82595(9) 0.0286(4) Uani 1 1 d . . . C54 C 0.23602(12) 0.48585(12) 0.89663(10) 0.0393(5) Uani 1 1 d . . . H54A H 0.2211 0.5348 0.9147 0.059 Uiso 1 1 calc R . . H54B H 0.2874 0.4937 0.888 0.059 Uiso 1 1 calc R . . H54C H 0.244 0.4441 0.9322 0.059 Uiso 1 1 calc R . . C55 C 0.08590(11) 0.44966(12) 0.83969(10) 0.0335(4) Uani 1 1 d . . . H55A H 0.0406 0.4377 0.7943 0.05 Uiso 1 1 calc R . . H55B H 0.0726 0.4974 0.8605 0.05 Uiso 1 1 calc R . . H55C H 0.0932 0.4057 0.873 0.05 Uiso 1 1 calc R . . C56 C 0.15118(14) 0.53206(12) 0.77419(11) 0.0443(5) Uani 1 1 d . . . H56A H 0.1074 0.5186 0.7283 0.066 Uiso 1 1 calc R . . H56B H 0.2024 0.5441 0.7664 0.066 Uiso 1 1 calc R . . H56C H 0.1342 0.5781 0.7948 0.066 Uiso 1 1 calc R . . C57A C 0.24355(12) 0.32676(12) 0.63216(9) 0.0343(4) Uani 0.5187(19) 1 d PD A 1 C58A C 0.2674(3) 0.2452(3) 0.6088(2) 0.0425(4) Uani 0.5187(19) 1 d PD A 1 H58A H 0.2694 0.2498 0.5608 0.064 Uiso 0.5187(19) 1 calc PR A 1 H58B H 0.2258 0.2059 0.608 0.064 Uiso 0.5187(19) 1 calc PR A 1 H58C H 0.3218 0.229 0.643 0.064 Uiso 0.5187(19) 1 calc PR A 1 C59A C 0.3035(2) 0.3863(3) 0.6362(2) 0.0425(4) Uani 0.5187(19) 1 d PD A 1 H59A H 0.2832 0.4374 0.6452 0.064 Uiso 0.5187(19) 1 calc PR A 1 H59B H 0.3125 0.3882 0.5908 0.064 Uiso 0.5187(19) 1 calc PR A 1 H59C H 0.3559 0.3739 0.6754 0.064 Uiso 0.5187(19) 1 calc PR A 1 C60A C 0.1573(2) 0.3465(3) 0.56948(19) 0.0425(4) Uani 0.5187(19) 1 d PD A 1 H60A H 0.1348 0.3952 0.5809 0.064 Uiso 0.5187(19) 1 calc PR A 1 H60B H 0.1182 0.3034 0.5649 0.064 Uiso 0.5187(19) 1 calc PR A 1 H60C H 0.1659 0.3529 0.5242 0.064 Uiso 0.5187(19) 1 calc PR A 1 C57B C 0.24355(12) 0.32676(12) 0.63216(9) 0.0343(4) Uani 0.4813(19) 1 d PD A 2 C58B C 0.2220(3) 0.4090(3) 0.5944(2) 0.0425(4) Uani 0.4813(19) 1 d PD A 2 H58D H 0.2352 0.4087 0.551 0.064 Uiso 0.4813(19) 1 calc PR A 2 H58E H 0.2546 0.4498 0.6272 0.064 Uiso 0.4813(19) 1 calc PR A 2 H58F H 0.1629 0.4197 0.5815 0.064 Uiso 0.4813(19) 1 calc PR A 2 C59B C 0.2059(3) 0.2643(3) 0.5819(2) 0.0425(4) Uani 0.4813(19) 1 d PD A 2 H59D H 0.2264 0.2134 0.6045 0.064 Uiso 0.4813(19) 1 calc PR A 2 H59E H 0.2203 0.2705 0.5394 0.064 Uiso 0.4813(19) 1 calc PR A 2 H59F H 0.1456 0.2665 0.5677 0.064 Uiso 0.4813(19) 1 calc PR A 2 C60B C 0.3426(3) 0.3233(3) 0.6544(2) 0.0425(4) Uani 0.4813(19) 1 d PD A 2 H60D H 0.3633 0.2723 0.6764 0.064 Uiso 0.4813(19) 1 calc PR A 2 H60E H 0.3684 0.3654 0.6888 0.064 Uiso 0.4813(19) 1 calc PR A 2 H60F H 0.3563 0.3302 0.6116 0.064 Uiso 0.4813(19) 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 K1 0.02429(19) 0.0275(2) 0.02201(18) 0.00165(15) 0.00631(14) -0.00434(15) K2 0.02174(18) 0.0415(2) 0.02032(18) -0.00215(16) 0.00681(14) 0.00136(16) O1 0.0284(6) 0.0289(7) 0.0193(6) -0.0011(5) 0.0109(5) -0.0035(5) O2 0.0271(6) 0.0316(7) 0.0181(6) 0.0023(5) 0.0091(5) 0.0013(5) N1 0.0294(8) 0.0230(8) 0.0247(7) 0.0014(6) 0.0077(6) -0.0022(6) C2 0.0335(10) 0.0361(11) 0.0299(10) 0.0053(8) 0.0093(8) -0.0104(8) C3 0.0268(10) 0.0558(14) 0.0325(10) 0.0027(9) 0.0133(8) -0.0024(9) O4 0.0302(7) 0.0472(9) 0.0383(8) 0.0036(6) 0.0064(6) 0.0014(6) C5 0.0466(13) 0.0556(15) 0.0594(14) 0.0109(12) 0.0277(11) 0.0169(11) C6 0.0402(13) 0.0717(18) 0.0722(17) 0.0219(14) 0.0208(12) 0.0198(12) O7 0.0363(8) 0.0489(9) 0.0392(8) 0.0063(7) 0.0035(6) 0.0020(6) C8 0.0468(13) 0.0380(12) 0.0445(12) 0.0053(10) -0.0042(10) 0.0018(10) C9 0.0339(12) 0.0417(13) 0.0594(14) 0.0051(11) -0.0095(10) -0.0010(10) O10 0.0334(7) 0.0318(8) 0.0387(7) 0.0020(6) -0.0009(6) -0.0075(6) C11 0.0417(12) 0.0330(11) 0.0392(11) -0.0075(9) 0.0033(9) -0.0098(9) C12 0.0466(12) 0.0365(11) 0.0315(10) -0.0111(9) 0.0069(9) -0.0043(9) O13 0.0366(7) 0.0323(7) 0.0289(7) -0.0034(6) 0.0083(6) -0.0040(6) C14 0.0588(14) 0.0265(11) 0.0397(11) -0.0047(9) 0.0162(10) -0.0100(9) C15 0.0496(12) 0.0232(10) 0.0351(10) 0.0034(8) 0.0123(9) 0.0007(8) C16 0.0268(9) 0.0273(9) 0.0238(9) 0.0060(7) 0.0052(7) 0.0028(7) C17 0.0201(8) 0.0299(9) 0.0191(8) 0.0016(7) 0.0035(6) -0.0021(7) C18 0.0178(8) 0.0285(9) 0.0160(7) -0.0007(7) 0.0029(6) -0.0026(7) C19 0.0259(9) 0.0275(9) 0.0193(8) -0.0009(7) 0.0067(7) -0.0026(7) C20 0.0324(10) 0.0305(10) 0.0252(9) -0.0039(7) 0.0123(7) -0.0014(8) C21 0.0270(9) 0.0407(11) 0.0201(8) -0.0010(8) 0.0100(7) -0.0044(8) C22 0.0253(9) 0.0345(10) 0.0194(8) 0.0060(7) 0.0045(7) -0.0040(7) C23 0.0448(11) 0.0250(9) 0.0251(9) -0.0017(7) 0.0140(8) -0.0023(8) C24 0.0506(12) 0.0337(11) 0.0338(11) 0.0084(9) 0.0101(9) 0.0033(9) C25 0.0480(12) 0.0348(11) 0.0379(11) -0.0020(9) 0.0160(9) -0.0143(9) C26 0.0892(18) 0.0282(11) 0.0471(13) -0.0003(10) 0.0357(13) 0.0038(11) C27 0.0413(11) 0.0518(13) 0.0286(10) -0.0010(9) 0.0218(9) -0.0054(9) C28 0.0512(14) 0.0731(17) 0.0624(15) 0.0079(13) 0.0408(12) 0.0060(12) C29 0.0780(17) 0.0753(18) 0.0360(12) -0.0169(12) 0.0365(12) -0.0193(14) C30 0.0528(13) 0.0653(15) 0.0330(11) 0.0073(10) 0.0255(10) -0.0075(11) N31 0.0295(8) 0.0316(8) 0.0246(7) 0.0022(6) 0.0091(6) 0.0068(6) C32 0.0573(13) 0.0334(11) 0.0341(11) 0.0042(9) 0.0127(10) 0.0121(10) C33 0.0706(17) 0.0538(15) 0.0394(12) 0.0116(11) 0.0074(11) 0.0294(13) O34 0.0664(10) 0.0610(11) 0.0259(7) 0.0062(7) 0.0007(7) 0.0212(8) C35 0.104(2) 0.084(2) 0.0349(13) 0.0133(14) -0.0136(14) 0.0387(18) C36 0.084(2) 0.089(2) 0.0262(12) 0.0052(13) -0.0004(12) -0.0026(16) O37 0.0435(9) 0.0749(12) 0.0319(8) 0.0041(8) 0.0014(7) -0.0005(8) C38 0.0320(12) 0.090(2) 0.0320(11) -0.0100(12) -0.0025(9) 0.0098(12) C39 0.0401(12) 0.0799(18) 0.0335(11) -0.0183(12) 0.0049(9) -0.0093(12) O40 0.0310(7) 0.0648(10) 0.0334(7) -0.0129(7) 0.0089(6) -0.0039(7) C41 0.0297(11) 0.0642(15) 0.0469(12) -0.0167(11) 0.0135(9) -0.0107(10) C42 0.0358(11) 0.0531(14) 0.0427(12) -0.0100(10) 0.0187(9) -0.0104(10) O43 0.0308(7) 0.0486(9) 0.0283(7) -0.0077(6) 0.0075(5) -0.0047(6) C44 0.0247(9) 0.0507(13) 0.0287(9) -0.0083(9) 0.0121(7) -0.0029(8) C45 0.0287(10) 0.0454(12) 0.0303(10) -0.0088(9) 0.0106(8) 0.0075(8) C46 0.0281(9) 0.0292(10) 0.0235(8) -0.0038(7) 0.0096(7) -0.0014(7) C47 0.0182(8) 0.0294(9) 0.0197(8) 0.0000(7) 0.0040(6) -0.0031(7) C48 0.0157(8) 0.0305(9) 0.0172(8) -0.0008(7) 0.0037(6) -0.0034(7) C49 0.0202(8) 0.0307(10) 0.0207(8) 0.0000(7) 0.0062(7) -0.0015(7) C50 0.0260(9) 0.0325(10) 0.0216(8) 0.0051(7) 0.0071(7) -0.0001(7) C51 0.0224(8) 0.0396(11) 0.0189(8) -0.0002(7) 0.0075(7) -0.0026(7) C52 0.0223(8) 0.0337(10) 0.0217(8) -0.0053(7) 0.0081(7) -0.0011(7) C53 0.0336(10) 0.0284(10) 0.0242(9) 0.0005(7) 0.0113(7) -0.0003(8) C54 0.0410(11) 0.0366(11) 0.0388(11) -0.0117(9) 0.0130(9) -0.0075(9) C55 0.0332(10) 0.0377(11) 0.0308(10) 0.0007(8) 0.0133(8) 0.0065(8) C56 0.0644(14) 0.0323(11) 0.0439(12) 0.0069(9) 0.0291(11) 0.0078(10) C57A 0.0398(11) 0.0436(12) 0.0241(9) 0.0034(8) 0.0173(8) 0.0025(9) C58A 0.0473(10) 0.0563(11) 0.0312(9) 0.0023(8) 0.0230(8) -0.0001(8) C59A 0.0473(10) 0.0563(11) 0.0312(9) 0.0023(8) 0.0230(8) -0.0001(8) C60A 0.0473(10) 0.0563(11) 0.0312(9) 0.0023(8) 0.0230(8) -0.0001(8) C57B 0.0398(11) 0.0436(12) 0.0241(9) 0.0034(8) 0.0173(8) 0.0025(9) C58B 0.0473(10) 0.0563(11) 0.0312(9) 0.0023(8) 0.0230(8) -0.0001(8) C59B 0.0473(10) 0.0563(11) 0.0312(9) 0.0023(8) 0.0230(8) -0.0001(8) C60B 0.0473(10) 0.0563(11) 0.0312(9) 0.0023(8) 0.0230(8) -0.0001(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K1 O2 2.6222(12) . ? K1 O1 2.6532(12) . ? K1 O7 2.7896(14) . ? K1 O10 2.8809(13) . ? K1 O13 2.8912(13) . ? K1 N1 2.9503(14) . ? K1 O4 3.0338(14) . ? K1 C18 3.3754(16) . ? K1 C8 3.533(2) . ? K1 K2 3.8209(5) . ? K2 O1 2.5810(11) . ? K2 O2 2.6776(12) . ? K2 O34 2.7839(16) . ? K2 O37 2.8086(14) . ? K2 N31 2.9234(15) . ? K2 O43 2.9413(13) . ? K2 O40 2.9826(14) . ? K2 C48 3.4333(16) . ? K2 C36 3.527(2) . ? O1 C18 1.2961(18) . ? O2 C48 1.3027(18) . ? N1 C2 1.469(2) . ? N1 C15 1.471(2) . ? N1 C16 1.491(2) . ? C2 C3 1.504(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 O4 1.421(2) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C5 1.425(3) . ? C5 C6 1.489(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 O7 1.427(3) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O7 C8 1.424(2) . ? C8 C9 1.501(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 O10 1.435(2) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? O10 C11 1.413(2) . ? C11 C12 1.502(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 O13 1.426(2) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? O13 C14 1.424(2) . ? C14 C15 1.505(3) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.501(2) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C22 1.398(2) . ? C17 C18 1.427(2) . ? C18 C19 1.440(2) . ? C19 C20 1.392(2) . ? C19 C23 1.534(2) . ? C20 C21 1.401(2) . ? C20 H20 0.95 . ? C21 C22 1.383(3) . ? C21 C27 1.537(2) . ? C22 H22 0.95 . ? C23 C26 1.527(3) . ? C23 C24 1.538(3) . ? C23 C25 1.540(3) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C30 1.528(3) . ? C27 C29 1.532(3) . ? C27 C28 1.543(3) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? N31 C32 1.471(2) . ? N31 C45 1.476(2) . ? N31 C46 1.486(2) . ? C32 C33 1.507(3) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 O34 1.415(3) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? O34 C35 1.439(3) . ? C35 C36 1.461(4) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 O37 1.415(3) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? O37 C38 1.417(3) . ? C38 C39 1.480(3) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 O40 1.428(2) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? O40 C41 1.427(2) . ? C41 C42 1.495(3) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 O43 1.423(2) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? O43 C44 1.428(2) . ? C44 C45 1.505(3) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 C47 1.501(2) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C47 C52 1.393(2) . ? C47 C48 1.425(2) . ? C48 C49 1.439(2) . ? C49 C50 1.396(2) . ? C49 C53 1.537(2) . ? C50 C51 1.399(2) . ? C50 H50 0.95 . ? C51 C52 1.393(2) . ? C51 C57A 1.537(2) . ? C52 H52 0.95 . ? C53 C55 1.533(2) . ? C53 C56 1.534(3) . ? C53 C54 1.541(3) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C57A C59A 1.434(4) . ? C57A C58A 1.569(4) . ? C57A C60A 1.596(4) . ? C58A H58A 0.98 . ? C58A H58B 0.98 . ? C58A H58C 0.98 . ? C59A H59A 0.98 . ? C59A H59B 0.98 . ? C59A H59C 0.98 . ? C60A H60A 0.98 . ? C60A H60B 0.98 . ? C60A H60C 0.98 . ? C58B H58D 0.98 . ? C58B H58E 0.98 . ? C58B H58F 0.98 . ? C59B H59D 0.98 . ? C59B H59E 0.98 . ? C59B H59F 0.98 . ? C60B H60D 0.98 . ? C60B H60E 0.98 . ? C60B H60F 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 K1 O1 81.27(4) . . ? O2 K1 O7 104.31(4) . . ? O1 K1 O7 125.02(4) . . ? O2 K1 O10 95.79(4) . . ? O1 K1 O10 173.96(4) . . ? O7 K1 O10 60.77(4) . . ? O2 K1 O13 103.97(4) . . ? O1 K1 O13 116.12(4) . . ? O7 K1 O13 115.18(4) . . ? O10 K1 O13 59.33(4) . . ? O2 K1 N1 137.94(4) . . ? O1 K1 N1 72.01(4) . . ? O7 K1 N1 117.55(4) . . ? O10 K1 N1 107.44(4) . . ? O13 K1 N1 62.61(4) . . ? O2 K1 O4 160.15(4) . . ? O1 K1 O4 101.92(4) . . ? O7 K1 O4 57.65(4) . . ? O10 K1 O4 82.64(4) . . ? O13 K1 O4 92.29(4) . . ? N1 K1 O4 60.09(4) . . ? O2 K1 C18 100.48(4) . . ? O1 K1 C18 20.72(4) . . ? O7 K1 C18 112.11(4) . . ? O10 K1 C18 163.54(4) . . ? O13 K1 C18 118.13(4) . . ? N1 K1 C18 61.23(4) . . ? O4 K1 C18 81.22(4) . . ? O2 K1 C8 92.62(5) . . ? O1 K1 C8 142.99(5) . . ? O7 K1 C8 22.30(5) . . ? O10 K1 C8 42.03(4) . . ? O13 K1 C8 100.81(4) . . ? N1 K1 C8 128.02(5) . . ? O4 K1 C8 72.92(5) . . ? C18 K1 C8 133.80(5) . . ? O2 K1 K2 44.44(3) . . ? O1 K1 K2 42.38(2) . . ? O7 K1 K2 138.99(3) . . ? O10 K1 K2 132.62(3) . . ? O13 K1 K2 100.27(3) . . ? N1 K1 K2 96.25(3) . . ? O4 K1 K2 144.01(3) . . ? C18 K1 K2 63.07(3) . . ? C8 K1 K2 135.73(4) . . ? O1 K2 O2 81.57(4) . . ? O1 K2 O34 91.20(5) . . ? O2 K2 O34 121.28(4) . . ? O1 K2 O37 81.11(4) . . ? O2 K2 O37 162.38(4) . . ? O34 K2 O37 62.34(5) . . ? O1 K2 N31 120.40(4) . . ? O2 K2 N31 71.91(4) . . ? O34 K2 N31 62.34(4) . . ? O37 K2 N31 120.30(5) . . ? O1 K2 O43 173.77(4) . . ? O2 K2 O43 104.54(3) . . ? O34 K2 O43 84.58(5) . . ? O37 K2 O43 92.86(4) . . ? N31 K2 O43 61.44(4) . . ? O1 K2 O40 119.15(4) . . ? O2 K2 O40 129.16(4) . . ? O34 K2 O40 105.16(5) . . ? O37 K2 O40 58.67(4) . . ? N31 K2 O40 119.05(4) . . ? O43 K2 O40 57.97(4) . . ? O1 K2 C48 101.72(4) . . ? O2 K2 C48 20.16(3) . . ? O34 K2 C48 120.21(4) . . ? O37 K2 C48 175.93(5) . . ? N31 K2 C48 60.87(4) . . ? O43 K2 C48 84.38(4) . . ? O40 K2 C48 117.26(4) . . ? O1 K2 C36 75.72(6) . . ? O2 K2 C36 150.54(6) . . ? O34 K2 C36 42.17(6) . . ? O37 K2 C36 22.33(6) . . ? N31 K2 C36 103.85(6) . . ? O43 K2 C36 98.10(6) . . ? O40 K2 C36 79.05(6) . . ? C48 K2 C36 161.17(6) . . ? O1 K2 K1 43.86(3) . . ? O2 K2 K1 43.29(2) . . ? O34 K2 K1 95.46(4) . . ? O37 K2 K1 121.67(4) . . ? N31 K2 K1 84.06(3) . . ? O43 K2 K1 141.03(3) . . ? O40 K2 K1 154.25(3) . . ? C48 K2 K1 61.93(3) . . ? C36 K2 K1 107.90(5) . . ? C18 O1 K2 153.17(10) . . ? C18 O1 K1 112.88(9) . . ? K2 O1 K1 93.76(4) . . ? C48 O2 K1 143.19(10) . . ? C48 O2 K2 114.75(9) . . ? K1 O2 K2 92.26(4) . . ? C2 N1 C15 109.92(14) . . ? C2 N1 C16 111.76(13) . . ? C15 N1 C16 108.18(14) . . ? C2 N1 K1 113.12(10) . . ? C15 N1 K1 106.96(10) . . ? C16 N1 K1 106.65(9) . . ? N1 C2 C3 115.13(15) . . ? N1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? N1 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? O4 C3 C2 109.28(16) . . ? O4 C3 H3A 109.8 . . ? C2 C3 H3A 109.8 . . ? O4 C3 H3B 109.8 . . ? C2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 O4 C5 110.46(16) . . ? C3 O4 K1 106.39(10) . . ? C5 O4 K1 100.80(11) . . ? O4 C5 C6 108.05(19) . . ? O4 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O4 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O7 C6 C5 108.68(18) . . ? O7 C6 H6A 110 . . ? C5 C6 H6A 110 . . ? O7 C6 H6B 110 . . ? C5 C6 H6B 110 . . ? H6A C6 H6B 108.3 . . ? C8 O7 C6 113.96(17) . . ? C8 O7 K1 109.68(12) . . ? C6 O7 K1 121.81(12) . . ? O7 C8 C9 112.39(18) . . ? O7 C8 K1 48.02(9) . . ? C9 C8 K1 85.79(11) . . ? O7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? K1 C8 H8A 82.2 . . ? O7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? K1 C8 H8B 157 . . ? H8A C8 H8B 107.9 . . ? O10 C9 C8 108.26(17) . . ? O10 C9 H9A 110 . . ? C8 C9 H9A 110 . . ? O10 C9 H9B 110 . . ? C8 C9 H9B 110 . . ? H9A C9 H9B 108.4 . . ? C11 O10 C9 111.69(15) . . ? C11 O10 K1 117.89(10) . . ? C9 O10 K1 115.82(12) . . ? O10 C11 C12 108.91(16) . . ? O10 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O10 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O13 C12 C11 113.73(16) . . ? O13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? O13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C14 O13 C12 113.28(15) . . ? C14 O13 K1 109.58(10) . . ? C12 O13 K1 113.77(11) . . ? O13 C14 C15 108.97(16) . . ? O13 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? O13 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N1 C15 C14 114.11(16) . . ? N1 C15 H15A 108.7 . . ? C14 C15 H15A 108.7 . . ? N1 C15 H15B 108.7 . . ? C14 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? N1 C16 C17 113.64(13) . . ? N1 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? N1 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C22 C17 C18 121.68(16) . . ? C22 C17 C16 120.50(15) . . ? C18 C17 C16 117.60(14) . . ? O1 C18 C17 120.62(15) . . ? O1 C18 C19 122.94(15) . . ? C17 C18 C19 116.41(14) . . ? O1 C18 K1 46.40(7) . . ? C17 C18 K1 99.81(10) . . ? C19 C18 K1 121.98(10) . . ? C20 C19 C18 118.92(15) . . ? C20 C19 C23 121.16(16) . . ? C18 C19 C23 119.89(14) . . ? C19 C20 C21 124.46(17) . . ? C19 C20 H20 117.8 . . ? C21 C20 H20 117.8 . . ? C22 C21 C20 116.35(15) . . ? C22 C21 C27 123.96(17) . . ? C20 C21 C27 119.44(17) . . ? C21 C22 C17 122.06(16) . . ? C21 C22 H22 119 . . ? C17 C22 H22 119 . . ? C26 C23 C19 112.56(15) . . ? C26 C23 C24 107.98(17) . . ? C19 C23 C24 110.27(15) . . ? C26 C23 C25 106.76(17) . . ? C19 C23 C25 109.62(15) . . ? C24 C23 C25 109.55(15) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C29 108.41(17) . . ? C30 C27 C21 112.41(17) . . ? C29 C27 C21 110.49(16) . . ? C30 C27 C28 108.49(17) . . ? C29 C27 C28 108.56(19) . . ? C21 C27 C28 108.39(16) . . ? 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 . . ? C32 N31 C45 111.25(15) . . ? C32 N31 C46 108.10(15) . . ? C45 N31 C46 111.39(13) . . ? C32 N31 K2 107.00(11) . . ? C45 N31 K2 111.00(11) . . ? C46 N31 K2 107.93(10) . . ? N31 C32 C33 114.39(18) . . ? N31 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? N31 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? O34 C33 C32 109.65(18) . . ? O34 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? O34 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C33 O34 C35 111.99(18) . . ? C33 O34 K2 117.32(12) . . ? C35 O34 K2 115.39(15) . . ? O34 C35 C36 109.9(2) . . ? O34 C35 H35A 109.7 . . ? C36 C35 H35A 109.7 . . ? O34 C35 H35B 109.7 . . ? C36 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? O37 C36 C35 114.8(2) . . ? O37 C36 K2 48.94(9) . . ? C35 C36 K2 82.62(13) . . ? O37 C36 H36A 108.6 . . ? C35 C36 H36A 108.6 . . ? K2 C36 H36A 86.5 . . ? O37 C36 H36B 108.6 . . ? C35 C36 H36B 108.6 . . ? K2 C36 H36B 157.2 . . ? H36A C36 H36B 107.6 . . ? C36 O37 C38 116.22(19) . . ? C36 O37 K2 108.73(13) . . ? C38 O37 K2 119.88(12) . . ? O37 C38 C39 108.34(18) . . ? O37 C38 H38A 110 . . ? C39 C38 H38A 110 . . ? O37 C38 H38B 110 . . ? C39 C38 H38B 110 . . ? H38A C38 H38B 108.4 . . ? O40 C39 C38 112.68(19) . . ? O40 C39 H39A 109.1 . . ? C38 C39 H39A 109.1 . . ? O40 C39 H39B 109.1 . . ? C38 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C41 O40 C39 113.57(15) . . ? C41 O40 K2 115.67(11) . . ? C39 O40 K2 110.89(12) . . ? O40 C41 C42 108.80(16) . . ? O40 C41 H41A 109.9 . . ? C42 C41 H41A 109.9 . . ? O40 C41 H41B 109.9 . . ? C42 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? O43 C42 C41 108.72(18) . . ? O43 C42 H42A 109.9 . . ? C41 C42 H42A 109.9 . . ? O43 C42 H42B 109.9 . . ? C41 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? C42 O43 C44 111.66(15) . . ? C42 O43 K2 107.53(11) . . ? C44 O43 K2 103.08(9) . . ? O43 C44 C45 108.37(15) . . ? O43 C44 H44A 110 . . ? C45 C44 H44A 110 . . ? O43 C44 H44B 110 . . ? C45 C44 H44B 110 . . ? H44A C44 H44B 108.4 . . ? N31 C45 C44 114.17(15) . . ? N31 C45 H45A 108.7 . . ? C44 C45 H45A 108.7 . . ? N31 C45 H45B 108.7 . . ? C44 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? N31 C46 C47 114.19(14) . . ? N31 C46 H46A 108.7 . . ? C47 C46 H46A 108.7 . . ? N31 C46 H46B 108.7 . . ? C47 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? C52 C47 C48 121.61(15) . . ? C52 C47 C46 119.87(15) . . ? C48 C47 C46 118.44(14) . . ? O2 C48 C47 120.17(15) . . ? O2 C48 C49 123.02(15) . . ? C47 C48 C49 116.80(14) . . ? O2 C48 K2 45.09(7) . . ? C47 C48 K2 98.64(10) . . ? C49 C48 K2 124.68(10) . . ? C50 C49 C48 118.74(15) . . ? C50 C49 C53 121.21(15) . . ? C48 C49 C53 119.98(14) . . ? C49 C50 C51 124.44(16) . . ? C49 C50 H50 117.8 . . ? C51 C50 H50 117.8 . . ? C52 C51 C50 116.24(15) . . ? C52 C51 C57A 121.88(16) . . ? C50 C51 C57A 121.78(16) . . ? C51 C52 C47 122.13(16) . . ? C51 C52 H52 118.9 . . ? C47 C52 H52 118.9 . . ? C55 C53 C56 107.11(15) . . ? C55 C53 C49 110.87(15) . . ? C56 C53 C49 112.65(14) . . ? C55 C53 C54 109.32(14) . . ? C56 C53 C54 107.54(16) . . ? C49 C53 C54 109.25(14) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C59A C57A C51 111.3(2) . . ? C59A C57A C58A 112.0(3) . . ? C51 C57A C58A 112.43(19) . . ? C59A C57A C60A 110.3(3) . . ? C51 C57A C60A 107.32(18) . . ? C58A C57A C60A 103.0(2) . . ? H58D C58B H58E 109.5 . . ? H58D C58B H58F 109.5 . . ? H58E C58B H58F 109.5 . . ? H59D C59B H59E 109.5 . . ? H59D C59B H59F 109.5 . . ? H59E C59B H59F 109.5 . . ? H60D C60B H60E 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 K1 K2 O1 142.74(5) . . . . ? O7 K1 K2 O1 92.12(6) . . . . ? O10 K1 K2 O1 -175.19(6) . . . . ? O13 K1 K2 O1 -117.72(5) . . . . ? N1 K1 K2 O1 -54.49(5) . . . . ? O4 K1 K2 O1 -9.15(6) . . . . ? C18 K1 K2 O1 -1.27(5) . . . . ? C8 K1 K2 O1 124.96(7) . . . . ? O1 K1 K2 O2 -142.74(5) . . . . ? O7 K1 K2 O2 -50.62(6) . . . . ? O10 K1 K2 O2 42.07(5) . . . . ? O13 K1 K2 O2 99.54(5) . . . . ? N1 K1 K2 O2 162.76(5) . . . . ? O4 K1 K2 O2 -151.89(6) . . . . ? C18 K1 K2 O2 -144.01(5) . . . . ? C8 K1 K2 O2 -17.78(7) . . . . ? O2 K1 K2 O34 -131.23(5) . . . . ? O1 K1 K2 O34 86.03(5) . . . . ? O7 K1 K2 O34 178.15(6) . . . . ? O10 K1 K2 O34 -89.16(5) . . . . ? O13 K1 K2 O34 -31.69(4) . . . . ? N1 K1 K2 O34 31.53(4) . . . . ? O4 K1 K2 O34 76.88(6) . . . . ? C18 K1 K2 O34 84.76(4) . . . . ? C8 K1 K2 O34 -149.01(6) . . . . ? O2 K1 K2 O37 168.04(6) . . . . ? O1 K1 K2 O37 25.30(6) . . . . ? O7 K1 K2 O37 117.42(6) . . . . ? O10 K1 K2 O37 -149.89(6) . . . . ? O13 K1 K2 O37 -92.42(5) . . . . ? N1 K1 K2 O37 -29.20(5) . . . . ? O4 K1 K2 O37 16.15(7) . . . . ? C18 K1 K2 O37 24.02(5) . . . . ? C8 K1 K2 O37 150.26(7) . . . . ? O2 K1 K2 N31 -69.84(5) . . . . ? O1 K1 K2 N31 147.42(5) . . . . ? O7 K1 K2 N31 -120.45(6) . . . . ? O10 K1 K2 N31 -27.77(5) . . . . ? O13 K1 K2 N31 29.70(4) . . . . ? N1 K1 K2 N31 92.93(4) . . . . ? O4 K1 K2 N31 138.27(6) . . . . ? C18 K1 K2 N31 146.15(4) . . . . ? C8 K1 K2 N31 -87.62(6) . . . . ? O2 K1 K2 O43 -43.10(6) . . . . ? O1 K1 K2 O43 174.16(6) . . . . ? O7 K1 K2 O43 -93.72(7) . . . . ? O10 K1 K2 O43 -1.03(7) . . . . ? O13 K1 K2 O43 56.44(6) . . . . ? N1 K1 K2 O43 119.67(6) . . . . ? O4 K1 K2 O43 165.01(7) . . . . ? C18 K1 K2 O43 172.89(6) . . . . ? C8 K1 K2 O43 -60.88(7) . . . . ? O2 K1 K2 O40 85.36(8) . . . . ? O1 K1 K2 O40 -57.38(8) . . . . ? O7 K1 K2 O40 34.74(9) . . . . ? O10 K1 K2 O40 127.43(8) . . . . ? O13 K1 K2 O40 -175.10(7) . . . . ? N1 K1 K2 O40 -111.87(7) . . . . ? O4 K1 K2 O40 -66.53(9) . . . . ? C18 K1 K2 O40 -58.65(7) . . . . ? C8 K1 K2 O40 67.58(9) . . . . ? O2 K1 K2 C48 -9.78(5) . . . . ? O1 K1 K2 C48 -152.52(5) . . . . ? O7 K1 K2 C48 -60.39(6) . . . . ? O10 K1 K2 C48 32.29(5) . . . . ? O13 K1 K2 C48 89.76(4) . . . . ? N1 K1 K2 C48 152.99(4) . . . . ? O4 K1 K2 C48 -161.67(6) . . . . ? C18 K1 K2 C48 -153.79(5) . . . . ? C8 K1 K2 C48 -27.56(6) . . . . ? O2 K1 K2 C36 -172.51(6) . . . . ? O1 K1 K2 C36 44.75(6) . . . . ? O7 K1 K2 C36 136.87(7) . . . . ? O10 K1 K2 C36 -130.44(6) . . . . ? O13 K1 K2 C36 -72.97(6) . . . . ? N1 K1 K2 C36 -9.74(6) . . . . ? O4 K1 K2 C36 35.60(7) . . . . ? C18 K1 K2 C36 43.48(6) . . . . ? C8 K1 K2 C36 169.71(8) . . . . ? O2 K2 O1 C18 -161.7(2) . . . . ? O34 K2 O1 C18 76.8(2) . . . . ? O37 K2 O1 C18 15.0(2) . . . . ? N31 K2 O1 C18 135.1(2) . . . . ? O43 K2 O1 C18 29.6(5) . . . . ? O40 K2 O1 C18 -31.3(2) . . . . ? C48 K2 O1 C18 -162.0(2) . . . . ? C36 K2 O1 C18 37.2(2) . . . . ? K1 K2 O1 C18 173.4(3) . . . . ? O2 K2 O1 K1 24.81(4) . . . . ? O34 K2 O1 K1 -96.65(4) . . . . ? O37 K2 O1 K1 -158.40(5) . . . . ? N31 K2 O1 K1 -38.39(5) . . . . ? O43 K2 O1 K1 -143.9(4) . . . . ? O40 K2 O1 K1 155.23(4) . . . . ? C48 K2 O1 K1 24.57(4) . . . . ? C36 K2 O1 K1 -136.27(6) . . . . ? O2 K1 O1 C18 157.81(11) . . . . ? O7 K1 O1 C18 56.40(12) . . . . ? O10 K1 O1 C18 -140.9(3) . . . . ? O13 K1 O1 C18 -100.84(11) . . . . ? N1 K1 O1 C18 -55.09(11) . . . . ? O4 K1 O1 C18 -2.27(11) . . . . ? C8 K1 O1 C18 75.10(13) . . . . ? K2 K1 O1 C18 -176.79(13) . . . . ? O2 K1 O1 K2 -25.40(4) . . . . ? O7 K1 O1 K2 -126.80(5) . . . . ? O10 K1 O1 K2 35.9(4) . . . . ? O13 K1 O1 K2 75.95(5) . . . . ? N1 K1 O1 K2 121.70(5) . . . . ? O4 K1 O1 K2 174.52(4) . . . . ? C18 K1 O1 K2 176.79(13) . . . . ? C8 K1 O1 K2 -108.11(8) . . . . ? O1 K1 O2 C48 163.15(17) . . . . ? O7 K1 O2 C48 -72.79(17) . . . . ? O10 K1 O2 C48 -11.52(17) . . . . ? O13 K1 O2 C48 48.27(17) . . . . ? N1 K1 O2 C48 112.69(17) . . . . ? O4 K1 O2 C48 -95.9(2) . . . . ? C18 K1 O2 C48 170.96(17) . . . . ? C8 K1 O2 C48 -53.55(17) . . . . ? K2 K1 O2 C48 138.77(18) . . . . ? O1 K1 O2 K2 24.38(4) . . . . ? O7 K1 O2 K2 148.44(4) . . . . ? O10 K1 O2 K2 -150.29(4) . . . . ? O13 K1 O2 K2 -90.50(4) . . . . ? N1 K1 O2 K2 -26.08(7) . . . . ? O4 K1 O2 K2 125.36(10) . . . . ? C18 K1 O2 K2 32.19(4) . . . . ? C8 K1 O2 K2 167.68(4) . . . . ? O1 K2 O2 C48 -179.32(11) . . . . ? O34 K2 O2 C48 -93.06(12) . . . . ? O37 K2 O2 C48 170.13(16) . . . . ? N31 K2 O2 C48 -53.40(11) . . . . ? O43 K2 O2 C48 -0.58(12) . . . . ? O40 K2 O2 C48 59.73(12) . . . . ? C36 K2 O2 C48 -139.61(14) . . . . ? K1 K2 O2 C48 -154.22(13) . . . . ? O1 K2 O2 K1 -25.09(4) . . . . ? O34 K2 O2 K1 61.16(6) . . . . ? O37 K2 O2 K1 -35.65(17) . . . . ? N31 K2 O2 K1 100.83(4) . . . . ? O43 K2 O2 K1 153.65(4) . . . . ? O40 K2 O2 K1 -146.05(4) . . . . ? C48 K2 O2 K1 154.22(12) . . . . ? C36 K2 O2 K1 14.61(13) . . . . ? O2 K1 N1 C2 169.81(10) . . . . ? O1 K1 N1 C2 116.53(12) . . . . ? O7 K1 N1 C2 -4.20(12) . . . . ? O10 K1 N1 C2 -69.78(12) . . . . ? O13 K1 N1 C2 -109.88(12) . . . . ? O4 K1 N1 C2 0.60(10) . . . . ? C18 K1 N1 C2 97.21(12) . . . . ? C8 K1 N1 C2 -27.75(13) . . . . ? K2 K1 N1 C2 151.77(11) . . . . ? O2 K1 N1 C15 -69.02(12) . . . . ? O1 K1 N1 C15 -122.30(11) . . . . ? O7 K1 N1 C15 116.97(11) . . . . ? O10 K1 N1 C15 51.39(12) . . . . ? O13 K1 N1 C15 11.29(10) . . . . ? O4 K1 N1 C15 121.77(12) . . . . ? C18 K1 N1 C15 -141.63(12) . . . . ? C8 K1 N1 C15 93.42(12) . . . . ? K2 K1 N1 C15 -87.07(11) . . . . ? O2 K1 N1 C16 46.55(12) . . . . ? O1 K1 N1 C16 -6.73(9) . . . . ? O7 K1 N1 C16 -127.46(10) . . . . ? O10 K1 N1 C16 166.96(10) . . . . ? O13 K1 N1 C16 126.86(11) . . . . ? O4 K1 N1 C16 -122.66(11) . . . . ? C18 K1 N1 C16 -26.05(9) . . . . ? C8 K1 N1 C16 -151.01(10) . . . . ? K2 K1 N1 C16 28.51(10) . . . . ? C15 N1 C2 C3 -152.05(16) . . . . ? C16 N1 C2 C3 87.82(18) . . . . ? K1 N1 C2 C3 -32.57(18) . . . . ? N1 C2 C3 O4 68.1(2) . . . . ? C2 C3 O4 C5 -170.27(16) . . . . ? C2 C3 O4 K1 -61.72(15) . . . . ? O2 K1 O4 C3 -127.02(14) . . . . ? O1 K1 O4 C3 -29.65(12) . . . . ? O7 K1 O4 C3 -153.74(13) . . . . ? O10 K1 O4 C3 146.32(12) . . . . ? O13 K1 O4 C3 87.65(12) . . . . ? N1 K1 O4 C3 31.30(11) . . . . ? C18 K1 O4 C3 -30.47(12) . . . . ? C8 K1 O4 C3 -171.74(13) . . . . ? K2 K1 O4 C3 -23.37(14) . . . . ? O2 K1 O4 C5 -11.74(18) . . . . ? O1 K1 O4 C5 85.63(12) . . . . ? O7 K1 O4 C5 -38.46(12) . . . . ? O10 K1 O4 C5 -98.39(12) . . . . ? O13 K1 O4 C5 -157.07(12) . . . . ? N1 K1 O4 C5 146.58(13) . . . . ? C18 K1 O4 C5 84.82(12) . . . . ? C8 K1 O4 C5 -56.45(12) . . . . ? K2 K1 O4 C5 91.92(12) . . . . ? C3 O4 C5 C6 -177.87(17) . . . . ? K1 O4 C5 C6 69.93(18) . . . . ? O4 C5 C6 O7 -66.9(3) . . . . ? C5 C6 O7 C8 158.48(19) . . . . ? C5 C6 O7 K1 23.3(3) . . . . ? O2 K1 O7 C8 60.16(13) . . . . ? O1 K1 O7 C8 149.45(12) . . . . ? O10 K1 O7 C8 -28.50(12) . . . . ? O13 K1 O7 C8 -53.12(13) . . . . ? N1 K1 O7 C8 -123.97(12) . . . . ? O4 K1 O7 C8 -128.90(13) . . . . ? C18 K1 O7 C8 167.99(12) . . . . ? K2 K1 O7 C8 94.12(13) . . . . ? O2 K1 O7 C6 -163.01(16) . . . . ? O1 K1 O7 C6 -73.72(17) . . . . ? O10 K1 O7 C6 108.33(17) . . . . ? O13 K1 O7 C6 83.70(17) . . . . ? N1 K1 O7 C6 12.85(18) . . . . ? O4 K1 O7 C6 7.93(16) . . . . ? C18 K1 O7 C6 -55.18(17) . . . . ? C8 K1 O7 C6 136.8(2) . . . . ? K2 K1 O7 C6 -129.05(16) . . . . ? C6 O7 C8 C9 -79.0(2) . . . . ? K1 O7 C8 C9 61.5(2) . . . . ? C6 O7 C8 K1 -140.48(19) . . . . ? O2 K1 C8 O7 -122.71(12) . . . . ? O1 K1 C8 O7 -43.76(16) . . . . ? O10 K1 C8 O7 141.54(16) . . . . ? O13 K1 C8 O7 132.52(12) . . . . ? N1 K1 C8 O7 68.96(13) . . . . ? O4 K1 C8 O7 43.45(12) . . . . ? C18 K1 C8 O7 -15.49(15) . . . . ? K2 K1 C8 O7 -110.35(12) . . . . ? O2 K1 C8 C9 111.83(14) . . . . ? O1 K1 C8 C9 -169.22(12) . . . . ? O7 K1 C8 C9 -125.5(2) . . . . ? O10 K1 C8 C9 16.08(13) . . . . ? O13 K1 C8 C9 7.07(15) . . . . ? N1 K1 C8 C9 -56.50(16) . . . . ? O4 K1 C8 C9 -82.01(14) . . . . ? C18 K1 C8 C9 -140.95(13) . . . . ? K2 K1 C8 C9 124.19(13) . . . . ? O7 C8 C9 O10 -64.0(3) . . . . ? K1 C8 C9 O10 -23.08(16) . . . . ? C8 C9 O10 C11 170.93(18) . . . . ? C8 C9 O10 K1 32.2(2) . . . . ? O2 K1 O10 C11 117.69(13) . . . . ? O1 K1 O10 C11 57.1(4) . . . . ? O7 K1 O10 C11 -139.14(14) . . . . ? O13 K1 O10 C11 14.86(13) . . . . ? N1 K1 O10 C11 -26.81(14) . . . . ? O4 K1 O10 C11 -82.23(13) . . . . ? C18 K1 O10 C11 -71.0(2) . . . . ? C8 K1 O10 C11 -154.83(16) . . . . ? K2 K1 O10 C11 89.55(13) . . . . ? O2 K1 O10 C9 -106.21(14) . . . . ? O1 K1 O10 C9 -166.8(3) . . . . ? O7 K1 O10 C9 -3.03(13) . . . . ? O13 K1 O10 C9 150.97(15) . . . . ? N1 K1 O10 C9 109.29(14) . . . . ? O4 K1 O10 C9 53.88(14) . . . . ? C18 K1 O10 C9 65.1(2) . . . . ? C8 K1 O10 C9 -18.72(14) . . . . ? K2 K1 O10 C9 -134.34(13) . . . . ? C9 O10 C11 C12 179.68(17) . . . . ? K1 O10 C11 C12 -42.5(2) . . . . ? O10 C11 C12 O13 59.9(2) . . . . ? C11 C12 O13 C14 79.4(2) . . . . ? C11 C12 O13 K1 -46.6(2) . . . . ? O2 K1 O13 C14 160.12(11) . . . . ? O1 K1 O13 C14 73.10(12) . . . . ? O7 K1 O13 C14 -86.40(12) . . . . ? O10 K1 O13 C14 -111.41(12) . . . . ? N1 K1 O13 C14 22.99(11) . . . . ? O4 K1 O13 C14 -31.36(12) . . . . ? C18 K1 O13 C14 49.90(12) . . . . ? C8 K1 O13 C14 -104.41(12) . . . . ? K2 K1 O13 C14 114.75(11) . . . . ? O2 K1 O13 C12 -71.93(12) . . . . ? O1 K1 O13 C12 -158.94(11) . . . . ? O7 K1 O13 C12 41.55(13) . . . . ? O10 K1 O13 C12 16.54(11) . . . . ? N1 K1 O13 C12 150.94(13) . . . . ? O4 K1 O13 C12 96.59(12) . . . . ? C18 K1 O13 C12 177.85(11) . . . . ? C8 K1 O13 C12 23.55(13) . . . . ? K2 K1 O13 C12 -117.30(12) . . . . ? C12 O13 C14 C15 175.92(16) . . . . ? K1 O13 C14 C15 -55.85(18) . . . . ? C2 N1 C15 C14 77.16(19) . . . . ? C16 N1 C15 C14 -160.56(16) . . . . ? K1 N1 C15 C14 -46.01(18) . . . . ? O13 C14 C15 N1 74.0(2) . . . . ? C2 N1 C16 C17 -60.35(18) . . . . ? C15 N1 C16 C17 178.51(14) . . . . ? K1 N1 C16 C17 63.76(14) . . . . ? N1 C16 C17 C22 94.27(18) . . . . ? N1 C16 C17 C18 -80.53(18) . . . . ? K2 O1 C18 C17 -99.8(2) . . . . ? K1 O1 C18 C17 73.14(16) . . . . ? K2 O1 C18 C19 82.4(3) . . . . ? K1 O1 C18 C19 -104.74(15) . . . . ? K2 O1 C18 K1 -172.9(3) . . . . ? C22 C17 C18 O1 -178.30(15) . . . . ? C16 C17 C18 O1 -3.6(2) . . . . ? C22 C17 C18 C19 -0.3(2) . . . . ? C16 C17 C18 C19 174.45(14) . . . . ? C22 C17 C18 K1 -133.60(14) . . . . ? C16 C17 C18 K1 41.14(15) . . . . ? O2 K1 C18 O1 -22.31(11) . . . . ? O7 K1 C18 O1 -132.58(11) . . . . ? O10 K1 C18 O1 166.45(13) . . . . ? O13 K1 C18 O1 89.86(11) . . . . ? N1 K1 C18 O1 117.14(12) . . . . ? O4 K1 C18 O1 177.75(11) . . . . ? C8 K1 C18 O1 -126.30(11) . . . . ? K2 K1 C18 O1 2.42(10) . . . . ? O2 K1 C18 C17 -145.61(10) . . . . ? O1 K1 C18 C17 -123.30(16) . . . . ? O7 K1 C18 C17 104.12(10) . . . . ? O10 K1 C18 C17 43.1(2) . . . . ? O13 K1 C18 C17 -33.44(11) . . . . ? N1 K1 C18 C17 -6.16(9) . . . . ? O4 K1 C18 C17 54.45(10) . . . . ? C8 K1 C18 C17 110.40(11) . . . . ? K2 K1 C18 C17 -120.88(10) . . . . ? O2 K1 C18 C19 84.59(12) . . . . ? O1 K1 C18 C19 106.90(17) . . . . ? O7 K1 C18 C19 -25.68(13) . . . . ? O10 K1 C18 C19 -86.65(19) . . . . ? O13 K1 C18 C19 -163.24(11) . . . . ? N1 K1 C18 C19 -135.96(13) . . . . ? O4 K1 C18 C19 -75.35(12) . . . . ? C8 K1 C18 C19 -19.40(15) . . . . ? K2 K1 C18 C19 109.32(12) . . . . ? O1 C18 C19 C20 175.69(15) . . . . ? C17 C18 C19 C20 -2.3(2) . . . . ? K1 C18 C19 C20 120.04(14) . . . . ? O1 C18 C19 C23 -2.7(2) . . . . ? C17 C18 C19 C23 179.38(15) . . . . ? K1 C18 C19 C23 -58.31(18) . . . . ? C18 C19 C20 C21 2.3(3) . . . . ? C23 C19 C20 C21 -179.40(16) . . . . ? C19 C20 C21 C22 0.5(3) . . . . ? C19 C20 C21 C27 -174.13(17) . . . . ? C20 C21 C22 C17 -3.2(2) . . . . ? C27 C21 C22 C17 171.15(16) . . . . ? C18 C17 C22 C21 3.1(3) . . . . ? C16 C17 C22 C21 -171.45(15) . . . . ? C20 C19 C23 C26 3.0(2) . . . . ? C18 C19 C23 C26 -178.70(17) . . . . ? C20 C19 C23 C24 -117.66(18) . . . . ? C18 C19 C23 C24 60.6(2) . . . . ? C20 C19 C23 C25 121.64(18) . . . . ? C18 C19 C23 C25 -60.0(2) . . . . ? C22 C21 C27 C30 7.5(3) . . . . ? C20 C21 C27 C30 -178.40(17) . . . . ? C22 C21 C27 C29 128.7(2) . . . . ? C20 C21 C27 C29 -57.2(2) . . . . ? C22 C21 C27 C28 -112.4(2) . . . . ? C20 C21 C27 C28 61.7(2) . . . . ? O1 K2 N31 C32 -55.82(13) . . . . ? O2 K2 N31 C32 -124.07(12) . . . . ? O34 K2 N31 C32 17.91(12) . . . . ? O37 K2 N31 C32 41.96(13) . . . . ? O43 K2 N31 C32 117.34(12) . . . . ? O40 K2 N31 C32 110.59(12) . . . . ? C48 K2 N31 C32 -142.53(13) . . . . ? C36 K2 N31 C32 25.57(13) . . . . ? K1 K2 N31 C32 -81.45(12) . . . . ? O1 K2 N31 C45 -177.36(10) . . . . ? O2 K2 N31 C45 114.38(11) . . . . ? O34 K2 N31 C45 -103.64(12) . . . . ? O37 K2 N31 C45 -79.59(12) . . . . ? O43 K2 N31 C45 -4.20(10) . . . . ? O40 K2 N31 C45 -10.96(12) . . . . ? C48 K2 N31 C45 95.92(11) . . . . ? C36 K2 N31 C45 -95.98(12) . . . . ? K1 K2 N31 C45 157.00(11) . . . . ? O1 K2 N31 C46 60.31(11) . . . . ? O2 K2 N31 C46 -7.95(10) . . . . ? O34 K2 N31 C46 134.04(11) . . . . ? O37 K2 N31 C46 158.08(10) . . . . ? O43 K2 N31 C46 -126.53(11) . . . . ? O40 K2 N31 C46 -133.29(10) . . . . ? C48 K2 N31 C46 -26.41(9) . . . . ? C36 K2 N31 C46 141.69(11) . . . . ? K1 K2 N31 C46 34.68(10) . . . . ? C45 N31 C32 C33 72.2(2) . . . . ? C46 N31 C32 C33 -165.16(17) . . . . ? K2 N31 C32 C33 -49.1(2) . . . . ? N31 C32 C33 O34 64.5(3) . . . . ? C32 C33 O34 C35 -179.7(2) . . . . ? C32 C33 O34 K2 -42.9(2) . . . . ? O1 K2 O34 C33 137.50(17) . . . . ? O2 K2 O34 C33 56.64(18) . . . . ? O37 K2 O34 C33 -143.19(18) . . . . ? N31 K2 O34 C33 13.41(16) . . . . ? O43 K2 O34 C33 -47.09(17) . . . . ? O40 K2 O34 C33 -101.80(17) . . . . ? C48 K2 O34 C33 33.18(18) . . . . ? C36 K2 O34 C33 -155.5(2) . . . . ? K1 K2 O34 C33 93.76(17) . . . . ? O1 K2 O34 C35 -87.13(19) . . . . ? O2 K2 O34 C35 -167.98(18) . . . . ? O37 K2 O34 C35 -7.82(18) . . . . ? N31 K2 O34 C35 148.8(2) . . . . ? O43 K2 O34 C35 88.29(19) . . . . ? O40 K2 O34 C35 33.57(19) . . . . ? C48 K2 O34 C35 168.56(18) . . . . ? C36 K2 O34 C35 -20.11(19) . . . . ? K1 K2 O34 C35 -130.86(18) . . . . ? C33 O34 C35 C36 174.0(2) . . . . ? K2 O34 C35 C36 36.3(3) . . . . ? O34 C35 C36 O37 -63.1(4) . . . . ? O34 C35 C36 K2 -25.2(2) . . . . ? O1 K2 C36 O37 -101.52(16) . . . . ? O2 K2 C36 O37 -142.22(13) . . . . ? O34 K2 C36 O37 150.2(2) . . . . ? N31 K2 C36 O37 140.11(15) . . . . ? O43 K2 C36 O37 77.65(16) . . . . ? O40 K2 C36 O37 22.62(15) . . . . ? C48 K2 C36 O37 174.02(13) . . . . ? K1 K2 C36 O37 -131.75(15) . . . . ? O1 K2 C36 C35 126.2(2) . . . . ? O2 K2 C36 C35 85.5(2) . . . . ? O34 K2 C36 C35 17.96(18) . . . . ? O37 K2 C36 C35 -132.3(3) . . . . ? N31 K2 C36 C35 7.8(2) . . . . ? O43 K2 C36 C35 -54.6(2) . . . . ? O40 K2 C36 C35 -109.7(2) . . . . ? C48 K2 C36 C35 41.7(3) . . . . ? K1 K2 C36 C35 96.0(2) . . . . ? C35 C36 O37 C38 -85.0(3) . . . . ? K2 C36 O37 C38 -138.9(2) . . . . ? C35 C36 O37 K2 53.9(3) . . . . ? O1 K2 O37 C36 73.97(16) . . . . ? O2 K2 O37 C36 84.5(2) . . . . ? O34 K2 O37 C36 -22.10(16) . . . . ? N31 K2 O37 C36 -46.15(17) . . . . ? O43 K2 O37 C36 -104.47(16) . . . . ? O40 K2 O37 C36 -153.77(18) . . . . ? C48 K2 O37 C36 -151.8(6) . . . . ? K1 K2 O37 C36 56.53(17) . . . . ? O1 K2 O37 C38 -148.91(16) . . . . ? O2 K2 O37 C38 -138.34(17) . . . . ? O34 K2 O37 C38 115.01(17) . . . . ? N31 K2 O37 C38 90.97(16) . . . . ? O43 K2 O37 C38 32.65(16) . . . . ? O40 K2 O37 C38 -16.65(15) . . . . ? C48 K2 O37 C38 -14.6(7) . . . . ? C36 K2 O37 C38 137.1(3) . . . . ? K1 K2 O37 C38 -166.35(14) . . . . ? C36 O37 C38 C39 -179.30(19) . . . . ? K2 O37 C38 C39 46.6(2) . . . . ? O37 C38 C39 O40 -63.1(2) . . . . ? C38 C39 O40 C41 -84.8(2) . . . . ? C38 C39 O40 K2 47.5(2) . . . . ? O1 K2 O40 C41 171.79(13) . . . . ? O2 K2 O40 C41 -84.46(14) . . . . ? O34 K2 O40 C41 71.65(14) . . . . ? O37 K2 O40 C41 114.94(15) . . . . ? N31 K2 O40 C41 5.21(15) . . . . ? O43 K2 O40 C41 -1.79(13) . . . . ? C48 K2 O40 C41 -64.90(14) . . . . ? C36 K2 O40 C41 105.09(15) . . . . ? K1 K2 O40 C41 -146.28(12) . . . . ? O1 K2 O40 C39 40.62(14) . . . . ? O2 K2 O40 C39 144.37(13) . . . . ? O34 K2 O40 C39 -59.51(14) . . . . ? O37 K2 O40 C39 -16.23(13) . . . . ? N31 K2 O40 C39 -125.96(13) . . . . ? O43 K2 O40 C39 -132.96(14) . . . . ? C48 K2 O40 C39 163.93(13) . . . . ? C36 K2 O40 C39 -26.08(14) . . . . ? K1 K2 O40 C39 82.55(15) . . . . ? C39 O40 C41 C42 164.30(19) . . . . ? K2 O40 C41 C42 34.4(2) . . . . ? O40 C41 C42 O43 -70.5(2) . . . . ? C41 C42 O43 C44 179.96(15) . . . . ? C41 C42 O43 K2 67.59(16) . . . . ? O1 K2 O43 C42 -96.7(4) . . . . ? O2 K2 O43 C42 94.85(11) . . . . ? O34 K2 O43 C42 -144.21(11) . . . . ? O37 K2 O43 C42 -82.34(11) . . . . ? N31 K2 O43 C42 154.43(12) . . . . ? O40 K2 O43 C42 -32.54(11) . . . . ? C48 K2 O43 C42 94.65(11) . . . . ? C36 K2 O43 C42 -104.16(12) . . . . ? K1 K2 O43 C42 123.80(10) . . . . ? O1 K2 O43 C44 145.2(4) . . . . ? O2 K2 O43 C44 -23.23(12) . . . . ? O34 K2 O43 C44 97.72(11) . . . . ? O37 K2 O43 C44 159.58(11) . . . . ? N31 K2 O43 C44 36.35(11) . . . . ? O40 K2 O43 C44 -150.62(12) . . . . ? C48 K2 O43 C44 -23.43(11) . . . . ? C36 K2 O43 C44 137.77(12) . . . . ? K1 K2 O43 C44 5.72(13) . . . . ? C42 O43 C44 C45 176.57(14) . . . . ? K2 O43 C44 C45 -68.29(14) . . . . ? C32 N31 C45 C44 -147.37(16) . . . . ? C46 N31 C45 C44 91.96(18) . . . . ? K2 N31 C45 C44 -28.34(17) . . . . ? O43 C44 C45 N31 70.43(18) . . . . ? C32 N31 C46 C47 179.47(15) . . . . ? C45 N31 C46 C47 -58.02(19) . . . . ? K2 N31 C46 C47 64.06(14) . . . . ? N31 C46 C47 C52 97.28(18) . . . . ? N31 C46 C47 C48 -79.46(18) . . . . ? K1 O2 C48 C47 -63.0(2) . . . . ? K2 O2 C48 C47 70.48(16) . . . . ? K1 O2 C48 C49 118.40(17) . . . . ? K2 O2 C48 C49 -108.08(14) . . . . ? K1 O2 C48 K2 -133.5(2) . . . . ? C52 C47 C48 O2 -179.36(14) . . . . ? C46 C47 C48 O2 -2.7(2) . . . . ? C52 C47 C48 C49 -0.7(2) . . . . ? C46 C47 C48 C49 175.96(14) . . . . ? C52 C47 C48 K2 -136.89(14) . . . . ? C46 C47 C48 K2 39.79(15) . . . . ? O1 K2 C48 O2 0.69(11) . . . . ? O34 K2 C48 O2 99.06(12) . . . . ? O37 K2 C48 O2 -133.1(6) . . . . ? N31 K2 C48 O2 119.12(12) . . . . ? O43 K2 C48 O2 179.44(11) . . . . ? O40 K2 C48 O2 -131.12(11) . . . . ? C36 K2 C48 O2 80.8(2) . . . . ? K1 K2 C48 O2 19.75(10) . . . . ? O1 K2 C48 C47 -123.80(10) . . . . ? O2 K2 C48 C47 -124.49(16) . . . . ? O34 K2 C48 C47 -25.43(11) . . . . ? O37 K2 C48 C47 102.5(7) . . . . ? N31 K2 C48 C47 -5.37(9) . . . . ? O43 K2 C48 C47 54.95(10) . . . . ? O40 K2 C48 C47 104.39(10) . . . . ? C36 K2 C48 C47 -43.7(2) . . . . ? K1 K2 C48 C47 -104.74(10) . . . . ? O1 K2 C48 C49 104.93(12) . . . . ? O2 K2 C48 C49 104.24(18) . . . . ? O34 K2 C48 C49 -156.71(12) . . . . ? O37 K2 C48 C49 -28.8(7) . . . . ? N31 K2 C48 C49 -136.64(13) . . . . ? O43 K2 C48 C49 -76.33(12) . . . . ? O40 K2 C48 C49 -26.88(14) . . . . ? C36 K2 C48 C49 -174.97(18) . . . . ? K1 K2 C48 C49 123.99(13) . . . . ? O2 C48 C49 C50 177.79(15) . . . . ? C47 C48 C49 C50 -0.8(2) . . . . ? K2 C48 C49 C50 122.83(14) . . . . ? O2 C48 C49 C53 0.7(2) . . . . ? C47 C48 C49 C53 -177.87(14) . . . . ? K2 C48 C49 C53 -54.22(18) . . . . ? C48 C49 C50 C51 1.3(3) . . . . ? C53 C49 C50 C51 178.33(16) . . . . ? C49 C50 C51 C52 -0.2(3) . . . . ? C49 C50 C51 C57A -176.66(16) . . . . ? C50 C51 C52 C47 -1.4(2) . . . . ? C57A C51 C52 C47 175.04(16) . . . . ? C48 C47 C52 C51 1.9(2) . . . . ? C46 C47 C52 C51 -174.74(15) . . . . ? C50 C49 C53 C55 123.44(17) . . . . ? C48 C49 C53 C55 -59.6(2) . . . . ? C50 C49 C53 C56 3.4(2) . . . . ? C48 C49 C53 C56 -179.60(16) . . . . ? C50 C49 C53 C54 -116.02(18) . . . . ? C48 C49 C53 C54 60.9(2) . . . . ? C52 C51 C57A C59A -120.7(3) . . . . ? C50 C51 C57A C59A 55.5(3) . . . . ? C52 C51 C57A C58A 5.9(3) . . . . ? C50 C51 C57A C58A -177.9(2) . . . . ? C52 C51 C57A C60A 118.4(2) . . . . ? C50 C51 C57A C60A -65.3(3) . . . . ? data_job2 _database_code_depnum_ccdc_archive 'CCDC 905352' #TrackingRef 'RD22_150K_APEX_18fev10_archive.cif' _audit_creation_date 2010-02-18T15:01:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H56 Li2 N2 O5 Si2' _chemical_formula_sum 'C29 H56 Li2 N2 O5 Si2' _chemical_formula_weight 582.82 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 10.0152(3) _cell_length_b 22.0468(6) _cell_length_c 16.1844(5) _cell_angle_alpha 90 _cell_angle_beta 98.016(2) _cell_angle_gamma 90 _cell_volume 3538.65(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5648 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.42 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.963 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_number 23321 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 8033 _reflns_number_gt 6683 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SAINT (Bruker, 2002)' _computing_cell_refinement 'Bruker SMART (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT (Bruker, 2002)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0535P)^2^+1.2765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8033 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.383 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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' 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 Si1 Si 0.42655(4) 0.393556(17) 0.19763(2) 0.02491(10) Uani 1 1 d . . . H1 H 0.5331(19) 0.3700(9) 0.1593(12) 0.05 Uiso 1 1 d . . . Si2 Si 0.15419(4) 0.447893(18) 0.13293(2) 0.02861(11) Uani 1 1 d . . . H2 H 0.1332(19) 0.4987(8) 0.0757(12) 0.05 Uiso 1 1 d . . . Li1 Li 0.2903(3) 0.35332(11) 0.03008(14) 0.0288(5) Uani 1 1 d . . . Li2 Li 0.3702(2) 0.31745(10) -0.12124(14) 0.0258(5) Uani 1 1 d . . . N1 N 0.29634(13) 0.40980(5) 0.12410(7) 0.0278(3) Uani 1 1 d . . . C1 C 0.38612(17) 0.33613(7) 0.27661(9) 0.0347(3) Uani 1 1 d . . . H1A H 0.3187 0.353 0.3086 0.052 Uiso 1 1 calc R . . H1B H 0.4683 0.3263 0.3145 0.052 Uiso 1 1 calc R . . H1C H 0.3504 0.2993 0.2478 0.052 Uiso 1 1 calc R . . C2 C 0.5075(2) 0.45795(8) 0.26281(11) 0.0483(5) Uani 1 1 d . . . H2A H 0.534 0.4898 0.2262 0.073 Uiso 1 1 calc R . . H2B H 0.5875 0.4431 0.2989 0.073 Uiso 1 1 calc R . . H2C H 0.4431 0.4745 0.2973 0.073 Uiso 1 1 calc R . . C3A C 0.1283(17) 0.4775(9) 0.2381(15) 0.061(3) Uani 0.5 1 d P . . H3A1 H 0.1217 0.4434 0.2761 0.091 Uiso 0.5 1 calc PR . . H3A2 H 0.0448 0.5013 0.2329 0.091 Uiso 0.5 1 calc PR . . H3A3 H 0.2046 0.5033 0.2601 0.091 Uiso 0.5 1 calc PR . . C3B C 0.1601(17) 0.4918(10) 0.2344(15) 0.061(3) Uani 0.5 1 d P . . H3B1 H 0.1607 0.4633 0.2809 0.091 Uiso 0.5 1 calc PR . . H3B2 H 0.0806 0.5181 0.2316 0.091 Uiso 0.5 1 calc PR . . H3B3 H 0.2419 0.5167 0.2431 0.091 Uiso 0.5 1 calc PR . . C4 C -0.00220(18) 0.40077(8) 0.10666(13) 0.0479(4) Uani 1 1 d . . . H4A H -0.0155 0.3915 0.0469 0.072 Uiso 1 1 calc R . . H4B H -0.0802 0.4233 0.1208 0.072 Uiso 1 1 calc R . . H4C H 0.0076 0.3629 0.1386 0.072 Uiso 1 1 calc R . . O11 O 0.16107(10) 0.37969(4) -0.07365(6) 0.0260(2) Uani 1 1 d . . . C12 C 0.04170(15) 0.34775(7) -0.10833(10) 0.0335(3) Uani 1 1 d . . . H12A H -0.0368 0.3753 -0.1108 0.04 Uiso 1 1 calc R . . H12B H 0.0267 0.3134 -0.0714 0.04 Uiso 1 1 calc R . . C13 C 0.05117(16) 0.32390(7) -0.19499(10) 0.0345(3) Uani 1 1 d . . . H13A H -0.0273 0.2977 -0.2144 0.041 Uiso 1 1 calc R . . H13B H 0.0526 0.3579 -0.2347 0.041 Uiso 1 1 calc R . . O14 O 0.17250(10) 0.29004(4) -0.18976(6) 0.0284(2) Uani 1 1 d . . . C15 C 0.18535(16) 0.25839(7) -0.26593(9) 0.0334(3) Uani 1 1 d . . . H15A H 0.1922 0.2876 -0.3116 0.04 Uiso 1 1 calc R . . H15B H 0.106 0.232 -0.2822 0.04 Uiso 1 1 calc R . . C16 C 0.31071(17) 0.22118(7) -0.24912(10) 0.0362(4) Uani 1 1 d . . . H16A H 0.3002 0.1894 -0.2073 0.043 Uiso 1 1 calc R . . H16B H 0.3298 0.2012 -0.301 0.043 Uiso 1 1 calc R . . O17 O 0.41809(10) 0.26146(4) -0.21829(6) 0.0298(2) Uani 1 1 d . . . C18 C 0.54409(16) 0.23202(7) -0.19282(9) 0.0326(3) Uani 1 1 d . . . H18A H 0.5729 0.2093 -0.24 0.039 Uiso 1 1 calc R . . H18B H 0.5363 0.2033 -0.1467 0.039 Uiso 1 1 calc R . . C19 C 0.64488(15) 0.28171(7) -0.16408(9) 0.0312(3) Uani 1 1 d . . . H19A H 0.7301 0.2631 -0.1374 0.037 Uiso 1 1 calc R . . H19B H 0.6648 0.3051 -0.2131 0.037 Uiso 1 1 calc R . . N20 N 0.59328(11) 0.32319(5) -0.10438(7) 0.0220(2) Uani 1 1 d . . . C21 C 0.62954(15) 0.38681(6) -0.11882(10) 0.0304(3) Uani 1 1 d . . . H21A H 0.6202 0.3945 -0.1796 0.036 Uiso 1 1 calc R . . H21B H 0.725 0.3936 -0.0954 0.036 Uiso 1 1 calc R . . C22 C 0.54189(15) 0.43075(6) -0.07950(9) 0.0300(3) Uani 1 1 d . . . H22A H 0.5577 0.4267 -0.018 0.036 Uiso 1 1 calc R . . H22B H 0.5631 0.4729 -0.0942 0.036 Uiso 1 1 calc R . . O23 O 0.40429(10) 0.41677(4) -0.11067(6) 0.0272(2) Uani 1 1 d . . . C24 C 0.31398(16) 0.45996(6) -0.08260(9) 0.0300(3) Uani 1 1 d . . . H24A H 0.3278 0.5004 -0.1066 0.036 Uiso 1 1 calc R . . H24B H 0.3303 0.4632 -0.021 0.036 Uiso 1 1 calc R . . C25 C 0.17367(16) 0.43828(6) -0.11062(9) 0.0307(3) Uani 1 1 d . . . H25A H 0.1074 0.4669 -0.0923 0.037 Uiso 1 1 calc R . . H25B H 0.157 0.4353 -0.1722 0.037 Uiso 1 1 calc R . . O31 O 0.36581(9) 0.28582(4) -0.00970(5) 0.01949(19) Uani 1 1 d . . . C32 C 0.44733(13) 0.23910(5) 0.01263(7) 0.0178(2) Uani 1 1 d . . . C33 C 0.40127(13) 0.18227(6) 0.04000(7) 0.0200(3) Uani 1 1 d . . . C34 C 0.25211(14) 0.17163(6) 0.04950(8) 0.0236(3) Uani 1 1 d . . . C35 C 0.16559(16) 0.17467(8) -0.03675(9) 0.0376(4) Uani 1 1 d . . . H35A H 0.1807 0.2136 -0.0632 0.056 Uiso 1 1 calc R . . H35B H 0.0701 0.1709 -0.0302 0.056 Uiso 1 1 calc R . . H35C H 0.1909 0.1415 -0.0717 0.056 Uiso 1 1 calc R . . C36 C 0.20273(16) 0.21941(7) 0.10709(10) 0.0367(4) Uani 1 1 d . . . H36A H 0.2592 0.2182 0.1616 0.055 Uiso 1 1 calc R . . H36B H 0.1089 0.2109 0.1141 0.055 Uiso 1 1 calc R . . H36C H 0.2085 0.2598 0.0824 0.055 Uiso 1 1 calc R . . C37 C 0.22814(17) 0.10947(7) 0.08760(12) 0.0429(4) Uani 1 1 d . . . H37A H 0.257 0.0774 0.0521 0.064 Uiso 1 1 calc R . . H37B H 0.132 0.1046 0.0916 0.064 Uiso 1 1 calc R . . H37C H 0.2801 0.1067 0.1434 0.064 Uiso 1 1 calc R . . C38 C 0.49514(14) 0.13497(6) 0.05669(8) 0.0229(3) Uani 1 1 d . . . H38 H 0.4634 0.0972 0.0744 0.027 Uiso 1 1 calc R . . C39 C 0.63194(14) 0.13973(6) 0.04899(8) 0.0221(3) Uani 1 1 d . . . C40 C 0.73232(15) 0.08703(6) 0.06787(9) 0.0278(3) Uani 1 1 d . . . C41 C 0.66506(17) 0.02920(7) 0.09489(12) 0.0414(4) Uani 1 1 d . . . H41A H 0.5947 0.0161 0.0502 0.062 Uiso 1 1 calc R . . H41B H 0.6247 0.0374 0.1455 0.062 Uiso 1 1 calc R . . H41C H 0.7328 -0.0029 0.1062 0.062 Uiso 1 1 calc R . . C42 C 0.84336(16) 0.10511(7) 0.13962(11) 0.0375(4) Uani 1 1 d . . . H42A H 0.9106 0.0726 0.1488 0.056 Uiso 1 1 calc R . . H42B H 0.803 0.1115 0.1907 0.056 Uiso 1 1 calc R . . H42C H 0.8869 0.1426 0.1249 0.056 Uiso 1 1 calc R . . C43 C 0.7984(2) 0.07263(8) -0.00994(12) 0.0479(4) Uani 1 1 d . . . H43A H 0.729 0.0597 -0.0553 0.072 Uiso 1 1 calc R . . H43B H 0.8644 0.04 0.0029 0.072 Uiso 1 1 calc R . . H43C H 0.8438 0.109 -0.0271 0.072 Uiso 1 1 calc R . . C44 C 0.67553(13) 0.19622(6) 0.02424(8) 0.0215(3) Uani 1 1 d . . . H44 H 0.7681 0.2016 0.0189 0.026 Uiso 1 1 calc R . . C45 C 0.58752(13) 0.24488(6) 0.00717(7) 0.0194(3) Uani 1 1 d . . . C46 C 0.64003(13) 0.30563(6) -0.01664(8) 0.0215(3) Uani 1 1 d . . . H46A H 0.611 0.3371 0.0208 0.026 Uiso 1 1 calc R . . H46B H 0.7398 0.3046 -0.0077 0.026 Uiso 1 1 calc R . . 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 Si1 0.0273(2) 0.02476(19) 0.02108(18) -0.00012(14) -0.00202(14) -0.00147(15) Si2 0.0346(2) 0.02553(19) 0.02497(19) -0.00272(14) 0.00153(16) 0.00943(16) Li1 0.0316(13) 0.0285(12) 0.0252(11) -0.0045(9) 0.0003(9) 0.0077(10) Li2 0.0298(12) 0.0259(11) 0.0215(10) 0.0008(9) 0.0028(9) 0.0022(9) N1 0.0327(7) 0.0274(6) 0.0216(5) -0.0052(4) -0.0021(5) 0.0087(5) C1 0.0411(9) 0.0337(8) 0.0272(7) 0.0036(6) -0.0022(6) -0.0053(7) C2 0.0634(12) 0.0393(9) 0.0373(9) 0.0001(7) -0.0104(8) -0.0200(9) C3A 0.048(7) 0.087(8) 0.044(2) -0.031(5) -0.002(5) 0.029(4) C3B 0.048(7) 0.087(8) 0.044(2) -0.031(5) -0.002(5) 0.029(4) C4 0.0388(10) 0.0377(9) 0.0715(13) 0.0046(8) 0.0229(9) 0.0014(8) O11 0.0242(5) 0.0254(5) 0.0271(5) 0.0003(4) -0.0014(4) 0.0025(4) C12 0.0207(7) 0.0376(8) 0.0413(8) -0.0039(6) 0.0010(6) 0.0019(6) C13 0.0278(8) 0.0362(8) 0.0355(8) -0.0035(6) -0.0095(6) 0.0018(6) O14 0.0308(5) 0.0322(5) 0.0207(4) -0.0030(4) -0.0021(4) 0.0026(4) C15 0.0388(9) 0.0379(8) 0.0225(7) -0.0089(6) 0.0013(6) -0.0113(7) C16 0.0453(10) 0.0325(8) 0.0323(8) -0.0139(6) 0.0103(7) -0.0080(7) O17 0.0336(6) 0.0285(5) 0.0273(5) -0.0047(4) 0.0039(4) -0.0010(4) C18 0.0400(9) 0.0331(7) 0.0258(7) -0.0063(6) 0.0083(6) 0.0075(6) C19 0.0303(8) 0.0396(8) 0.0259(7) -0.0021(6) 0.0108(6) 0.0055(6) N20 0.0249(6) 0.0216(5) 0.0206(5) 0.0029(4) 0.0068(4) 0.0011(4) C21 0.0269(8) 0.0280(7) 0.0371(8) 0.0120(6) 0.0075(6) -0.0036(6) C22 0.0291(8) 0.0215(6) 0.0378(8) 0.0050(6) -0.0014(6) -0.0054(6) O23 0.0260(5) 0.0217(5) 0.0330(5) -0.0027(4) 0.0017(4) 0.0007(4) C24 0.0372(8) 0.0205(6) 0.0324(7) -0.0021(5) 0.0055(6) 0.0033(6) C25 0.0333(8) 0.0248(7) 0.0336(7) 0.0024(6) 0.0030(6) 0.0090(6) O31 0.0208(5) 0.0186(4) 0.0191(4) 0.0008(3) 0.0029(3) 0.0036(3) C32 0.0204(6) 0.0188(6) 0.0141(5) -0.0007(4) 0.0014(4) 0.0015(5) C33 0.0205(6) 0.0214(6) 0.0177(6) 0.0015(5) 0.0012(5) -0.0004(5) C34 0.0218(7) 0.0240(6) 0.0246(6) 0.0035(5) 0.0023(5) -0.0028(5) C35 0.0257(8) 0.0559(10) 0.0292(7) 0.0000(7) -0.0028(6) -0.0105(7) C36 0.0344(9) 0.0419(9) 0.0377(8) -0.0048(7) 0.0187(7) -0.0061(7) C37 0.0293(9) 0.0348(8) 0.0666(12) 0.0192(8) 0.0131(8) -0.0044(7) C38 0.0246(7) 0.0195(6) 0.0238(6) 0.0037(5) 0.0006(5) -0.0016(5) C39 0.0235(7) 0.0209(6) 0.0209(6) 0.0015(5) -0.0009(5) 0.0033(5) C40 0.0256(7) 0.0224(6) 0.0345(7) 0.0047(5) 0.0007(6) 0.0056(5) C41 0.0339(9) 0.0239(7) 0.0634(11) 0.0123(7) -0.0041(8) 0.0050(6) C42 0.0285(8) 0.0315(8) 0.0490(9) 0.0078(7) -0.0067(7) 0.0065(6) C43 0.0590(12) 0.0395(9) 0.0475(10) 0.0019(8) 0.0152(8) 0.0231(9) C44 0.0187(6) 0.0243(6) 0.0214(6) 0.0014(5) 0.0021(5) 0.0012(5) C45 0.0218(7) 0.0195(6) 0.0167(5) 0.0010(4) 0.0015(5) -0.0011(5) C46 0.0209(6) 0.0210(6) 0.0223(6) 0.0018(5) 0.0020(5) -0.0015(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 N1 1.6769(12) . ? Si1 C1 1.8830(15) . ? Si1 C2 1.8833(16) . ? Si1 Li1 2.995(2) . ? Si1 H1 1.41(2) . ? Si2 N1 1.6760(13) . ? Si2 C3A 1.87(2) . ? Si2 C4 1.8782(19) . ? Si2 C3B 1.90(2) . ? Si2 Li1 3.100(2) . ? Si2 H2 1.451(19) . ? Li1 O31 1.827(2) . ? Li1 N1 1.961(3) . ? Li1 O11 2.056(2) . ? Li1 Li2 2.795(3) . ? Li2 O31 1.941(2) . ? Li2 O17 2.105(2) . ? Li2 O14 2.214(3) . ? Li2 N20 2.216(3) . ? Li2 O23 2.219(2) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? O11 C12 1.4329(17) . ? O11 C25 1.4366(17) . ? C12 C13 1.513(2) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 O14 1.4186(18) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? O14 C15 1.4377(16) . ? C15 C16 1.493(2) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 O17 1.4300(18) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? O17 C18 1.4277(18) . ? C18 C19 1.518(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 N20 1.4752(17) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? N20 C21 1.4755(17) . ? N20 C46 1.4834(16) . ? C21 C22 1.507(2) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O23 1.4335(17) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? O23 C24 1.4303(17) . ? C24 C25 1.494(2) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? O31 C32 1.3327(14) . ? C32 C45 1.4247(18) . ? C32 C33 1.4269(17) . ? C33 C38 1.4049(18) . ? C33 C34 1.5409(19) . ? C34 C36 1.534(2) . ? C34 C37 1.5352(19) . ? C34 C35 1.5383(19) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 C39 1.3969(19) . ? C38 H38 0.95 . ? C39 C44 1.3967(18) . ? C39 C40 1.5390(18) . ? C40 C41 1.534(2) . ? C40 C43 1.535(2) . ? C40 C42 1.544(2) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 C45 1.3915(18) . ? C44 H44 0.95 . ? C45 C46 1.5086(17) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? 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 N1 Si1 C1 113.94(7) . . ? N1 Si1 C2 117.89(7) . . ? C1 Si1 C2 104.07(7) . . ? C1 Si1 Li1 107.55(7) . . ? C2 Si1 Li1 146.78(7) . . ? N1 Si1 H1 109.2(7) . . ? C1 Si1 H1 107.4(8) . . ? C2 Si1 H1 103.4(8) . . ? Li1 Si1 H1 76.6(7) . . ? N1 Si2 C3A 118.6(7) . . ? N1 Si2 C4 113.27(7) . . ? C3A Si2 C4 100.5(4) . . ? N1 Si2 C3B 113.9(6) . . ? C4 Si2 C3B 113.7(4) . . ? C3A Si2 Li1 148.1(7) . . ? C4 Si2 Li1 85.51(8) . . ? C3B Si2 Li1 147.5(7) . . ? N1 Si2 H2 112.5(8) . . ? C3A Si2 H2 106.5(10) . . ? C4 Si2 H2 103.9(7) . . ? C3B Si2 H2 98.2(11) . . ? Li1 Si2 H2 102.3(8) . . ? O31 Li1 N1 145.24(14) . . ? O31 Li1 O11 100.78(11) . . ? N1 Li1 O11 113.70(12) . . ? O31 Li1 Li2 43.73(7) . . ? N1 Li1 Li2 151.43(14) . . ? O11 Li1 Li2 65.73(8) . . ? O31 Li1 Si1 113.69(10) . . ? N1 Li1 Si1 31.61(5) . . ? O11 Li1 Si1 144.20(11) . . ? Li2 Li1 Si1 136.66(11) . . ? O31 Li1 Si2 166.39(13) . . ? N1 Li1 Si2 28.88(5) . . ? O11 Li1 Si2 88.53(8) . . ? Li2 Li1 Si2 149.54(10) . . ? Si1 Li1 Si2 59.57(4) . . ? O31 Li2 O17 121.35(12) . . ? O31 Li2 O14 103.47(11) . . ? O17 Li2 O14 75.35(8) . . ? O31 Li2 N20 93.40(10) . . ? O17 Li2 N20 78.16(9) . . ? O14 Li2 N20 153.24(12) . . ? O31 Li2 O23 107.82(11) . . ? O17 Li2 O23 125.99(12) . . ? O14 Li2 O23 115.16(11) . . ? N20 Li2 O23 78.03(9) . . ? O31 Li2 Li1 40.57(7) . . ? O17 Li2 Li1 160.51(12) . . ? O14 Li2 Li1 99.83(10) . . ? N20 Li2 Li1 106.43(10) . . ? O23 Li2 Li1 73.32(9) . . ? Si2 N1 Si1 129.22(7) . . ? Si2 N1 Li1 116.73(10) . . ? Si1 N1 Li1 110.60(9) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3A H3A1 109.5 . . ? Si2 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Si2 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? Si2 C3B H3B1 109.5 . . ? Si2 C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? Si2 C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C12 O11 C25 113.31(11) . . ? C12 O11 Li1 125.23(11) . . ? C25 O11 Li1 120.84(11) . . ? O11 C12 C13 112.16(13) . . ? O11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? O11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O14 C13 C12 106.95(11) . . ? O14 C13 H13A 110.3 . . ? C12 C13 H13A 110.3 . . ? O14 C13 H13B 110.3 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? C13 O14 C15 112.50(11) . . ? C13 O14 Li2 125.80(10) . . ? C15 O14 Li2 112.40(10) . . ? O14 C15 C16 106.51(11) . . ? O14 C15 H15A 110.4 . . ? C16 C15 H15A 110.4 . . ? O14 C15 H15B 110.4 . . ? C16 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? O17 C16 C15 107.14(12) . . ? O17 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? O17 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.5 . . ? C18 O17 C16 114.19(11) . . ? C18 O17 Li2 109.58(10) . . ? C16 O17 Li2 112.71(11) . . ? O17 C18 C19 106.48(12) . . ? O17 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? O17 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? N20 C19 C18 111.67(12) . . ? N20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? N20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 N20 C21 111.66(11) . . ? C19 N20 C46 111.88(10) . . ? C21 N20 C46 110.36(10) . . ? C19 N20 Li2 108.85(10) . . ? C21 N20 Li2 107.51(10) . . ? C46 N20 Li2 106.33(10) . . ? N20 C21 C22 111.93(11) . . ? N20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? O23 C22 C21 107.53(11) . . ? O23 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? O23 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C24 O23 C22 111.38(11) . . ? C24 O23 Li2 125.74(11) . . ? C22 O23 Li2 111.67(10) . . ? O23 C24 C25 107.48(11) . . ? O23 C24 H24A 110.2 . . ? C25 C24 H24A 110.2 . . ? O23 C24 H24B 110.2 . . ? C25 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? O11 C25 C24 107.14(11) . . ? O11 C25 H25A 110.3 . . ? C24 C25 H25A 110.3 . . ? O11 C25 H25B 110.3 . . ? C24 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? C32 O31 Li1 143.34(10) . . ? C32 O31 Li2 115.93(10) . . ? Li1 O31 Li2 95.70(11) . . ? O31 C32 C45 119.07(11) . . ? O31 C32 C33 123.40(11) . . ? C45 C32 C33 117.51(11) . . ? C38 C33 C32 118.34(12) . . ? C38 C33 C34 119.99(11) . . ? C32 C33 C34 121.65(11) . . ? C36 C34 C37 106.70(12) . . ? C36 C34 C35 109.45(13) . . ? C37 C34 C35 107.67(13) . . ? C36 C34 C33 110.81(11) . . ? C37 C34 C33 112.58(11) . . ? C35 C34 C33 109.52(11) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C33 124.44(12) . . ? C39 C38 H38 117.8 . . ? C33 C38 H38 117.8 . . ? C44 C39 C38 116.25(12) . . ? C44 C39 C40 120.56(12) . . ? C38 C39 C40 123.17(12) . . ? C41 C40 C43 108.58(14) . . ? C41 C40 C39 112.55(12) . . ? C43 C40 C39 109.72(12) . . ? C41 C40 C42 107.40(12) . . ? C43 C40 C42 108.84(14) . . ? C39 C40 C42 109.66(11) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C39 121.98(12) . . ? C45 C44 H44 119 . . ? C39 C44 H44 119 . . ? C44 C45 C32 121.42(11) . . ? C44 C45 C46 120.10(12) . . ? C32 C45 C46 118.48(11) . . ? N20 C46 C45 113.67(10) . . ? N20 C46 H46A 108.8 . . ? C45 C46 H46A 108.8 . . ? N20 C46 H46B 108.8 . . ? C45 C46 H46B 108.8 . . ? H46A C46 H46B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Si1 Li1 O31 -177.21(19) . . . . ? C1 Si1 Li1 O31 -70.55(14) . . . . ? C2 Si1 Li1 O31 127.95(16) . . . . ? C1 Si1 Li1 N1 106.66(11) . . . . ? C2 Si1 Li1 N1 -54.8(2) . . . . ? N1 Si1 Li1 O11 19.56(16) . . . . ? C1 Si1 Li1 O11 126.2(2) . . . . ? C2 Si1 Li1 O11 -35.3(3) . . . . ? N1 Si1 Li1 Li2 136.0(2) . . . . ? C1 Si1 Li1 Li2 -117.32(15) . . . . ? C2 Si1 Li1 Li2 81.2(2) . . . . ? N1 Si1 Li1 Si2 -10.51(8) . . . . ? C1 Si1 Li1 Si2 96.16(6) . . . . ? C2 Si1 Li1 Si2 -65.35(16) . . . . ? N1 Si2 Li1 O31 74.9(5) . . . . ? C3A Si2 Li1 O31 32.9(10) . . . . ? C4 Si2 Li1 O31 -69.8(5) . . . . ? C3B Si2 Li1 O31 59.1(11) . . . . ? C3A Si2 Li1 N1 -42.1(8) . . . . ? C4 Si2 Li1 N1 -144.70(12) . . . . ? C3B Si2 Li1 N1 -15.8(10) . . . . ? N1 Si2 Li1 O11 -151.54(16) . . . . ? C3A Si2 Li1 O11 166.4(8) . . . . ? C4 Si2 Li1 O11 63.76(10) . . . . ? C3B Si2 Li1 O11 -167.4(10) . . . . ? N1 Si2 Li1 Li2 -120.3(3) . . . . ? C3A Si2 Li1 Li2 -162.3(8) . . . . ? C4 Si2 Li1 Li2 95.0(2) . . . . ? C3B Si2 Li1 Li2 -136.1(10) . . . . ? N1 Si2 Li1 Si1 11.42(9) . . . . ? C3A Si2 Li1 Si1 -30.7(8) . . . . ? C4 Si2 Li1 Si1 -133.28(7) . . . . ? C3B Si2 Li1 Si1 -4.4(10) . . . . ? N1 Li1 Li2 O31 124.4(3) . . . . ? O11 Li1 Li2 O31 -140.18(14) . . . . ? Si1 Li1 Li2 O31 74.88(15) . . . . ? Si2 Li1 Li2 O31 -174.9(2) . . . . ? O31 Li1 Li2 O17 25.5(4) . . . . ? N1 Li1 Li2 O17 149.9(3) . . . . ? O11 Li1 Li2 O17 -114.7(4) . . . . ? Si1 Li1 Li2 O17 100.4(4) . . . . ? Si2 Li1 Li2 O17 -149.4(3) . . . . ? O31 Li1 Li2 O14 99.27(12) . . . . ? N1 Li1 Li2 O14 -136.3(2) . . . . ? O11 Li1 Li2 O14 -40.91(9) . . . . ? Si1 Li1 Li2 O14 174.15(12) . . . . ? Si2 Li1 Li2 O14 -75.6(2) . . . . ? O31 Li1 Li2 N20 -75.55(11) . . . . ? N1 Li1 Li2 N20 48.9(3) . . . . ? O11 Li1 Li2 N20 144.27(11) . . . . ? Si1 Li1 Li2 N20 -0.67(19) . . . . ? Si2 Li1 Li2 N20 109.6(2) . . . . ? O31 Li1 Li2 O23 -147.25(13) . . . . ? N1 Li1 Li2 O23 -22.8(3) . . . . ? O11 Li1 Li2 O23 72.57(8) . . . . ? Si1 Li1 Li2 O23 -72.37(14) . . . . ? Si2 Li1 Li2 O23 37.9(2) . . . . ? C3A Si2 N1 Si1 -0.6(6) . . . . ? C4 Si2 N1 Si1 -117.99(11) . . . . ? C3B Si2 N1 Si1 14.0(7) . . . . ? Li1 Si2 N1 Si1 -156.83(18) . . . . ? C3A Si2 N1 Li1 156.2(6) . . . . ? C4 Si2 N1 Li1 38.83(13) . . . . ? C3B Si2 N1 Li1 170.8(6) . . . . ? C1 Si1 N1 Si2 69.91(12) . . . . ? C2 Si1 N1 Si2 -52.50(14) . . . . ? Li1 Si1 N1 Si2 157.95(17) . . . . ? C1 Si1 N1 Li1 -88.04(12) . . . . ? C2 Si1 N1 Li1 149.55(12) . . . . ? O31 Li1 N1 Si2 -156.5(2) . . . . ? O11 Li1 N1 Si2 31.35(17) . . . . ? Li2 Li1 N1 Si2 113.7(2) . . . . ? Si1 Li1 N1 Si2 -160.99(15) . . . . ? O31 Li1 N1 Si1 4.5(3) . . . . ? O11 Li1 N1 Si1 -167.65(10) . . . . ? Li2 Li1 N1 Si1 -85.3(3) . . . . ? Si2 Li1 N1 Si1 160.99(15) . . . . ? O31 Li1 O11 C12 69.39(16) . . . . ? N1 Li1 O11 C12 -115.17(15) . . . . ? Li2 Li1 O11 C12 96.17(13) . . . . ? Si1 Li1 O11 C12 -126.21(19) . . . . ? Si2 Li1 O11 C12 -100.61(12) . . . . ? O31 Li1 O11 C25 -120.27(13) . . . . ? N1 Li1 O11 C25 55.18(18) . . . . ? Li2 Li1 O11 C25 -93.48(12) . . . . ? Si1 Li1 O11 C25 44.1(3) . . . . ? Si2 Li1 O11 C25 69.74(12) . . . . ? C25 O11 C12 C13 73.37(15) . . . . ? Li1 O11 C12 C13 -115.64(15) . . . . ? O11 C12 C13 O14 52.80(16) . . . . ? C12 C13 O14 C15 172.62(12) . . . . ? C12 C13 O14 Li2 -43.55(18) . . . . ? O31 Li2 O14 C13 88.39(15) . . . . ? O17 Li2 O14 C13 -152.24(12) . . . . ? N20 Li2 O14 C13 -144.0(2) . . . . ? O23 Li2 O14 C13 -29.00(18) . . . . ? Li1 Li2 O14 C13 47.09(15) . . . . ? O31 Li2 O14 C15 -127.75(12) . . . . ? O17 Li2 O14 C15 -8.39(11) . . . . ? N20 Li2 O14 C15 -0.1(3) . . . . ? O23 Li2 O14 C15 114.86(13) . . . . ? Li1 Li2 O14 C15 -169.05(11) . . . . ? C13 O14 C15 C16 -175.52(12) . . . . ? Li2 O14 C15 C16 35.67(15) . . . . ? O14 C15 C16 O17 -54.55(15) . . . . ? C15 C16 O17 C18 175.31(12) . . . . ? C15 C16 O17 Li2 49.41(15) . . . . ? O31 Li2 O17 C18 -54.04(17) . . . . ? O14 Li2 O17 C18 -151.09(10) . . . . ? N20 Li2 O17 C18 32.70(11) . . . . ? O23 Li2 O17 C18 98.23(15) . . . . ? Li1 Li2 O17 C18 -73.2(4) . . . . ? O31 Li2 O17 C16 74.31(17) . . . . ? O14 Li2 O17 C16 -22.74(12) . . . . ? N20 Li2 O17 C16 161.05(10) . . . . ? O23 Li2 O17 C16 -133.42(14) . . . . ? Li1 Li2 O17 C16 55.2(4) . . . . ? C16 O17 C18 C19 178.85(11) . . . . ? Li2 O17 C18 C19 -53.62(14) . . . . ? O17 C18 C19 N20 49.93(15) . . . . ? C18 C19 N20 C21 -140.76(12) . . . . ? C18 C19 N20 C46 94.99(14) . . . . ? C18 C19 N20 Li2 -22.22(15) . . . . ? O31 Li2 N20 C19 116.58(11) . . . . ? O17 Li2 N20 C19 -4.76(11) . . . . ? O14 Li2 N20 C19 -12.9(3) . . . . ? O23 Li2 N20 C19 -135.92(10) . . . . ? Li1 Li2 N20 C19 155.69(10) . . . . ? O31 Li2 N20 C21 -122.31(11) . . . . ? O17 Li2 N20 C21 116.35(10) . . . . ? O14 Li2 N20 C21 108.2(3) . . . . ? O23 Li2 N20 C21 -14.81(11) . . . . ? Li1 Li2 N20 C21 -83.20(12) . . . . ? O31 Li2 N20 C46 -4.11(12) . . . . ? O17 Li2 N20 C46 -125.45(9) . . . . ? O14 Li2 N20 C46 -133.6(3) . . . . ? O23 Li2 N20 C46 103.39(9) . . . . ? Li1 Li2 N20 C46 35.01(12) . . . . ? C19 N20 C21 C22 161.05(12) . . . . ? C46 N20 C21 C22 -73.85(14) . . . . ? Li2 N20 C21 C22 41.71(14) . . . . ? N20 C21 C22 O23 -55.04(15) . . . . ? C21 C22 O23 C24 -174.56(11) . . . . ? C21 C22 O23 Li2 39.28(14) . . . . ? O31 Li2 O23 C24 -64.52(16) . . . . ? O17 Li2 O23 C24 140.14(14) . . . . ? O14 Li2 O23 C24 50.39(16) . . . . ? N20 Li2 O23 C24 -154.26(11) . . . . ? Li1 Li2 O23 C24 -42.83(13) . . . . ? O31 Li2 O23 C22 75.76(14) . . . . ? O17 Li2 O23 C22 -79.57(16) . . . . ? O14 Li2 O23 C22 -169.33(11) . . . . ? N20 Li2 O23 C22 -13.98(11) . . . . ? Li1 Li2 O23 C22 97.45(11) . . . . ? C22 O23 C24 C25 -174.28(11) . . . . ? Li2 O23 C24 C25 -33.90(16) . . . . ? C12 O11 C25 C24 -167.81(11) . . . . ? Li1 O11 C25 C24 20.76(17) . . . . ? O23 C24 C25 O11 59.79(14) . . . . ? N1 Li1 O31 C32 14.3(4) . . . . ? O11 Li1 O31 C32 -173.06(14) . . . . ? Li2 Li1 O31 C32 150.5(2) . . . . ? Si1 Li1 O31 C32 16.8(2) . . . . ? Si2 Li1 O31 C32 -40.6(6) . . . . ? N1 Li1 O31 Li2 -136.2(3) . . . . ? O11 Li1 O31 Li2 36.46(13) . . . . ? Si1 Li1 O31 Li2 -133.65(11) . . . . ? Si2 Li1 O31 Li2 168.9(5) . . . . ? O17 Li2 O31 C32 28.79(18) . . . . ? O14 Li2 O31 C32 109.66(11) . . . . ? N20 Li2 O31 C32 -49.41(12) . . . . ? O23 Li2 O31 C32 -127.92(11) . . . . ? Li1 Li2 O31 C32 -160.90(14) . . . . ? O17 Li2 O31 Li1 -170.31(14) . . . . ? O14 Li2 O31 Li1 -89.44(12) . . . . ? N20 Li2 O31 Li1 111.49(11) . . . . ? O23 Li2 O31 Li1 32.98(13) . . . . ? Li1 O31 C32 C45 -92.1(2) . . . . ? Li2 O31 C32 C45 54.84(15) . . . . ? Li1 O31 C32 C33 89.6(2) . . . . ? Li2 O31 C32 C33 -123.44(13) . . . . ? O31 C32 C33 C38 175.85(11) . . . . ? C45 C32 C33 C38 -2.45(17) . . . . ? O31 C32 C33 C34 -2.75(18) . . . . ? C45 C32 C33 C34 178.95(11) . . . . ? C38 C33 C34 C36 126.31(13) . . . . ? C32 C33 C34 C36 -55.11(16) . . . . ? C38 C33 C34 C37 6.91(18) . . . . ? C32 C33 C34 C37 -174.51(13) . . . . ? C38 C33 C34 C35 -112.84(14) . . . . ? C32 C33 C34 C35 65.74(16) . . . . ? C32 C33 C38 C39 0.55(19) . . . . ? C34 C33 C38 C39 179.18(12) . . . . ? C33 C38 C39 C44 1.09(19) . . . . ? C33 C38 C39 C40 179.92(12) . . . . ? C44 C39 C40 C41 179.38(13) . . . . ? C38 C39 C40 C41 0.60(19) . . . . ? C44 C39 C40 C43 -59.61(17) . . . . ? C38 C39 C40 C43 121.62(15) . . . . ? C44 C39 C40 C42 59.89(17) . . . . ? C38 C39 C40 C42 -118.89(14) . . . . ? C38 C39 C44 C45 -0.77(18) . . . . ? C40 C39 C44 C45 -179.63(12) . . . . ? C39 C44 C45 C32 -1.20(19) . . . . ? C39 C44 C45 C46 177.99(11) . . . . ? O31 C32 C45 C44 -175.57(11) . . . . ? C33 C32 C45 C44 2.81(17) . . . . ? O31 C32 C45 C46 5.23(16) . . . . ? C33 C32 C45 C46 -176.39(11) . . . . ? C19 N20 C46 C45 -64.47(14) . . . . ? C21 N20 C46 C45 170.56(11) . . . . ? Li2 N20 C46 C45 54.25(13) . . . . ? C44 C45 C46 N20 111.98(13) . . . . ? C32 C45 C46 N20 -68.81(15) . . . . ?