#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-09-10 at 15:09:00 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : osu008 scrals #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2009-09-10 _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 _audit_update_record ? #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Pandian1746 _audit_creation_date 2009-09-10T15:09:00-00:00 _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 _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C80 H88 Li N8 O8' _chemical_formula_sum 'C80 H88 Li N8 O8' _chemical_formula_weight 1296.52 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P41212 _symmetry_space_group_name_Hall 'P 4abw 2nw' _symmetry_Int_Tables_number 92 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+3/4' '-x, -y, z+1/2' '-x+1/2, y+1/2, -z+1/4' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' '-y, -x, -z+1/2' _cell_length_a 15.4360(10) _cell_length_b 15.4360(10) _cell_length_c 28.831(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6869.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2764 _exptl_special_details ;Because of the weakly diffracting nature of these crystals, a synchrotron data collection was necessary. Intensity data were collected at 150K on a D8 goniostat equipped with a Bruker APEXII CCD detector at Beamline 11.3.1 at the Advanced Light Source Lawrence Berkeley National Laboratory) using synchrotron radiation tuned to 0.7749 Ang. For data collection, frames were measured with a frame width of 0.3 degrees in omega and an exposure time of 1 second per frame for low angle data and 5 seconds per frame for high angle data out to a maximum two theta value of 58 degrees. The data frames were collected using the program APEX2 and integrated using the program SAINT within APEX2. The data were corrected for absorption and beam corrections based on the multi-scan technique as implemented in SADABS. Crystallographic data were collected through the SCrALS program (Service Crystallography at Advanced Light Source) at the Small-Crystal Crystallography Beamline 11.3.1 (developed by the Experimental Systems Group) at the Advanced Light Source (ALS). The ALS is supported by the U.S. Department of Energy, Office of Energy Sciences Materials Sciences Division, under contract DE-AC02-05CH11231 at Lawrence Berkeley National Laboratory. We thank Dr. Jeanette Krause of the University of Cincinnati for this data set. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS v2008/1 (Sheldrick)' _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.746 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7749 _diffrn_radiation_type synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_number 104308 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 29.04 _diffrn_reflns_theta_full 29.04 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7085 _reflns_number_gt 3180 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 v2008.6.0' _computing_cell_refinement 'Bruker SAINT v7.46A' _computing_data_reduction 'Bruker SAINT v7.46A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The molecule contains a crystallographic two-fold rotation axis which passes through atoms Li, N(4) and N(5). One of the n-butyl groups is disordered over two sites with one orientation consisting of atoms C(37), C(38), C(39) and C(40), and the other orientation containing atoms C(37A), C(38A), C(39) and C(40A). The occupancy factor for the first group [C(37), C(38) and C(40)] refined to 0.544(9), while that for the second group [C(37A), C(38A) and C(40A)] is 0.456(9). Since atom C(39) is common to both orientations, its occupancy factor was fixed at 1.0. Atom C(40A) was refined only isotropically. The SADI and DFIX restraints in the SHELXL program were used in the refinement of this disorder model. (DFIX is a distance restraint, where the distance between two atoms is restrained to a target value. SADI is a similarity restraint which restrains the distance between two or more pairs of atoms to be equal.) For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5*Ueq(bonded carbon atom). The remaining hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(attached atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.1360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7085 _refine_ls_number_parameters 462 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1586 _refine_ls_R_factor_gt 0.072 _refine_ls_wR_factor_ref 0.2496 _refine_ls_wR_factor_gt 0.1896 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.356 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.04 #----------------------------------------------------------------------------# # 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 0.004 0.002 '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 0.0004 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0073 '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 C1 C 1.0573(3) 0.9600(3) 0.01679(16) 0.0825(12) Uani 1 1 d . . . C2 C 1.0756(3) 0.8751(3) 0.03769(16) 0.0841(12) Uani 1 1 d . . . C3 C 1.1641(3) 0.8779(3) 0.05054(16) 0.0855(12) Uani 1 1 d . . . C4 C 1.1946(3) 0.9638(3) 0.03623(15) 0.0834(12) Uani 1 1 d . . . C5 C 1.3066(3) 1.0677(3) 0.02970(16) 0.0860(13) Uani 1 1 d . . . C6 C 1.3983(3) 1.0921(4) 0.03083(18) 0.0960(15) Uani 1 1 d . . . C7 C 1.4015(3) 1.1809(4) 0.02148(18) 0.0960(15) Uani 1 1 d . . . C8 C 1.3102(3) 1.2066(4) 0.01202(18) 0.0915(13) Uani 1 1 d . . . C9 C 1.0241(4) 0.8032(3) 0.04643(16) 0.0905(14) Uani 1 1 d . . . C10 C 1.0646(4) 0.7275(3) 0.06588(17) 0.0936(14) Uani 1 1 d . . . C11 C 1.0160(4) 0.6516(4) 0.07467(19) 0.1062(16) Uani 1 1 d . . . H11 H 0.9559 0.6508 0.0675 0.127 Uiso 1 1 calc R . . C12 C 1.0534(5) 0.5797(4) 0.0932(2) 0.1164(18) Uani 1 1 d . . . H12 H 1.0204 0.5283 0.0975 0.14 Uiso 1 1 calc R . . C13 C 1.1379(5) 0.5820(4) 0.1054(2) 0.120(2) Uani 1 1 d . . . H13 H 1.1623 0.532 0.1194 0.143 Uiso 1 1 calc R . . C14 C 1.1910(5) 0.6537(4) 0.09838(19) 0.1158(19) Uani 1 1 d . . . H14 H 1.2506 0.6524 0.1065 0.139 Uiso 1 1 calc R . . C15 C 1.1520(4) 0.7301(3) 0.07838(17) 0.0957(14) Uani 1 1 d . . . C16 C 1.2023(4) 0.8069(3) 0.07078(18) 0.0925(14) Uani 1 1 d . . . C17 C 1.4740(4) 1.0449(4) 0.04070(18) 0.0983(15) Uani 1 1 d . . . C18 C 1.5526(4) 1.0908(5) 0.04272(18) 0.1046(16) Uani 1 1 d . . . C19 C 1.6308(4) 1.0477(5) 0.0524(2) 0.1191(19) Uani 1 1 d . . . H19 H 1.6308 0.9869 0.0573 0.143 Uiso 1 1 calc R . . C20 C 1.7062(5) 1.0926(7) 0.0549(2) 0.139(3) Uani 1 1 d . . . H20 H 1.7577 1.063 0.0637 0.167 Uiso 1 1 calc R . . C21 C 1.7102(4) 1.1803(7) 0.0450(2) 0.139(3) Uani 1 1 d . . . H21 H 1.7647 1.2089 0.045 0.166 Uiso 1 1 calc R . . C22 C 1.6358(4) 1.2265(5) 0.0351(2) 0.124(2) Uani 1 1 d . . . H22 H 1.638 1.2872 0.0296 0.149 Uiso 1 1 calc R . . C23 C 1.5550(3) 1.1804(5) 0.03325(18) 0.1074(18) Uani 1 1 d . . . C24 C 1.4777(4) 1.2264(4) 0.0224(2) 0.1090(17) Uani 1 1 d . A . Li Li 1.1315(5) 1.1315(5) 0 0.084(3) Uani 1 2 d S . . N1 N 1.1292(3) 1.0101(2) 0.01714(13) 0.0828(10) Uani 1 1 d . . . N2 N 1.2770(3) 0.9892(3) 0.04158(14) 0.0914(11) Uani 1 1 d . . . N3 N 1.2569(3) 1.1377(3) 0.01793(14) 0.0888(11) Uani 1 1 d . . . N4 N 1.2868(3) 1.2868(3) 0 0.0961(17) Uani 1 2 d S . . N5 N 0.9791(3) 0.9791(3) 0 0.0835(14) Uani 1 2 d S . . O1 O 0.9380(2) 0.7984(2) 0.03653(11) 0.0928(9) Uani 1 1 d . . . O2 O 1.2880(2) 0.8072(2) 0.08450(12) 0.1003(10) Uani 1 1 d . . . O3 O 1.4775(2) 0.9603(3) 0.04961(14) 0.1153(12) Uani 1 1 d . . . O4 O 1.4837(3) 1.3135(3) 0.01386(17) 0.1270(13) Uani 1 1 d D . . C25 C 0.8840(4) 0.8451(4) 0.0685(2) 0.1117(17) Uani 1 1 d . . . H25A H 0.8884 0.908 0.062 0.134 Uiso 1 1 calc R . . H25B H 0.9047 0.8349 0.1005 0.134 Uiso 1 1 calc R . . C26 C 0.7903(6) 0.8169(6) 0.0645(3) 0.157(3) Uani 1 1 d . . . H26A H 0.756 0.8485 0.0881 0.188 Uiso 1 1 calc R . . H26B H 0.7683 0.8343 0.0336 0.188 Uiso 1 1 calc R . . C27 C 0.7755(6) 0.7228(6) 0.0706(3) 0.161(3) Uani 1 1 d . . . H27A H 0.7944 0.7048 0.102 0.193 Uiso 1 1 calc R . . H27B H 0.8101 0.6901 0.0476 0.193 Uiso 1 1 calc R . . C28 C 0.6803(8) 0.7022(12) 0.0643(6) 0.297(8) Uani 1 1 d . . . H28A H 0.6712 0.6397 0.0676 0.445 Uiso 1 1 calc R . . H28B H 0.6616 0.7207 0.0334 0.445 Uiso 1 1 calc R . . H28C H 0.6464 0.733 0.0879 0.445 Uiso 1 1 calc R . . C29 C 1.2969(4) 0.8402(4) 0.13155(19) 0.1055(16) Uani 1 1 d . . . H29A H 1.2663 0.8014 0.1535 0.127 Uiso 1 1 calc R . . H29B H 1.2705 0.8985 0.1337 0.127 Uiso 1 1 calc R . . C30 C 1.3901(4) 0.8450(3) 0.1441(2) 0.1045(16) Uani 1 1 d . . . H30A H 1.3956 0.8741 0.1746 0.125 Uiso 1 1 calc R . . H30B H 1.4204 0.8813 0.1209 0.125 Uiso 1 1 calc R . . C31 C 1.4346(4) 0.7582(4) 0.14665(19) 0.1060(17) Uani 1 1 d . . . H31A H 1.4337 0.7309 0.1156 0.127 Uiso 1 1 calc R . . H31B H 1.4021 0.7201 0.1681 0.127 Uiso 1 1 calc R . . C32 C 1.5295(4) 0.7653(5) 0.1634(2) 0.126(2) Uani 1 1 d . . . H32A H 1.5555 0.7074 0.1646 0.188 Uiso 1 1 calc R . . H32B H 1.5307 0.7912 0.1945 0.188 Uiso 1 1 calc R . . H32C H 1.5624 0.8019 0.1419 0.188 Uiso 1 1 calc R . . C33 C 1.4448(4) 0.9019(4) 0.0146(3) 0.128(2) Uani 1 1 d . . . H33A H 1.3857 0.8825 0.0231 0.154 Uiso 1 1 calc R . . H33B H 1.4415 0.9321 -0.0156 0.154 Uiso 1 1 calc R . . C34 C 1.5008(5) 0.8288(6) 0.0109(3) 0.159(3) Uani 1 1 d . . . H34A H 1.5114 0.8053 0.0424 0.19 Uiso 1 1 calc R . . H34B H 1.5572 0.8482 -0.0017 0.19 Uiso 1 1 calc R . . C35 C 1.4652(6) 0.7554(6) -0.0201(4) 0.181(4) Uani 1 1 d . . . H35A H 1.504 0.7045 -0.018 0.217 Uiso 1 1 calc R . . H35B H 1.4073 0.7379 -0.0088 0.217 Uiso 1 1 calc R . . C36 C 1.4586(8) 0.7834(7) -0.0691(5) 0.235(6) Uani 1 1 d . . . H36A H 1.4348 0.736 -0.0878 0.352 Uiso 1 1 calc R . . H36B H 1.5163 0.7987 -0.0807 0.352 Uiso 1 1 calc R . . H36C H 1.4204 0.8339 -0.0712 0.352 Uiso 1 1 calc R . . C37 C 1.4730(8) 1.3327(7) -0.0376(3) 0.123(4) Uani 0.544(9) 1 d PD A 1 H37A H 1.4104 1.3373 -0.0446 0.147 Uiso 0.544(9) 1 calc PR A 1 H37B H 1.4961 1.2831 -0.0555 0.147 Uiso 0.544(9) 1 calc PR A 1 C38 C 1.5182(9) 1.4161(7) -0.0544(4) 0.146(5) Uani 0.544(9) 1 d PD A 1 H38A H 1.503 1.4631 -0.0325 0.175 Uiso 0.544(9) 1 calc PR A 1 H38B H 1.5815 1.4068 -0.0519 0.175 Uiso 0.544(9) 1 calc PR A 1 C40 C 1.5420(8) 1.5244(9) -0.1155(4) 0.138(5) Uani 0.544(9) 1 d P A 1 H40A H 1.5267 1.5406 -0.1473 0.207 Uiso 0.544(9) 1 calc PR A 1 H40B H 1.6047 1.5153 -0.1134 0.207 Uiso 0.544(9) 1 calc PR A 1 H40C H 1.5249 1.5709 -0.0942 0.207 Uiso 0.544(9) 1 calc PR A 1 C37A C 1.4447(9) 1.3625(8) 0.0542(4) 0.118(5) Uani 0.456(9) 1 d PD A 2 H37C H 1.441 1.3235 0.0814 0.141 Uiso 0.456(9) 1 calc PR A 2 H37D H 1.385 1.3804 0.046 0.141 Uiso 0.456(9) 1 calc PR A 2 C38A C 1.4437(9) 1.4980(9) -0.0675(4) 0.127(5) Uani 0.456(9) 1 d PD A 2 H38C H 1.4787 1.5093 -0.0393 0.152 Uiso 0.456(9) 1 calc PR A 2 H38D H 1.4255 1.5545 -0.0805 0.152 Uiso 0.456(9) 1 calc PR A 2 C40A C 1.546(2) 1.3711(15) -0.0896(10) 0.283(16) Uiso 0.456(9) 1 d PD A 2 H40D H 1.5793 1.3486 -0.1161 0.425 Uiso 0.456(9) 1 calc PR A 2 H40E H 1.505 1.3271 -0.0791 0.425 Uiso 0.456(9) 1 calc PR A 2 H40F H 1.5863 1.3851 -0.0643 0.425 Uiso 0.456(9) 1 calc PR A 2 C39 C 1.4996(5) 1.4491(7) -0.1036(3) 0.165(3) Uani 1 1 d D . . H39A H 1.516 1.4033 -0.126 0.199 Uiso 0.544(9) 1 calc PR A 1 H39B H 1.4365 1.4588 -0.1067 0.199 Uiso 0.544(9) 1 calc PR A 1 H39C H 1.4612 1.4331 -0.1297 0.199 Uiso 0.456(9) 1 calc PR A 2 H39D H 1.5428 1.4906 -0.1159 0.199 Uiso 0.456(9) 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 C1 0.095(4) 0.074(3) 0.079(3) 0.003(2) -0.003(2) 0.004(3) C2 0.086(3) 0.080(3) 0.087(3) 0.001(2) -0.012(2) 0.007(3) C3 0.097(3) 0.081(3) 0.079(3) -0.007(2) -0.010(2) 0.015(3) C4 0.089(3) 0.079(3) 0.081(3) -0.005(2) -0.006(2) 0.004(3) C5 0.086(3) 0.088(4) 0.084(3) -0.005(3) -0.013(2) 0.012(3) C6 0.079(3) 0.111(4) 0.099(4) -0.005(3) -0.009(3) 0.005(3) C7 0.087(4) 0.110(4) 0.091(3) -0.012(3) -0.001(3) -0.006(3) C8 0.082(3) 0.096(4) 0.097(3) -0.007(3) -0.001(2) 0.000(3) C9 0.107(4) 0.086(3) 0.078(3) 0.002(2) -0.009(3) 0.013(3) C10 0.118(4) 0.086(3) 0.077(3) 0.008(2) -0.007(3) 0.004(3) C11 0.128(4) 0.090(4) 0.100(4) 0.007(3) -0.016(3) 0.004(3) C12 0.146(6) 0.094(4) 0.109(4) 0.011(3) -0.029(4) 0.000(4) C13 0.179(7) 0.079(4) 0.100(4) 0.010(3) -0.032(4) 0.014(4) C14 0.158(5) 0.091(4) 0.099(4) -0.002(3) -0.037(4) 0.030(4) C15 0.119(4) 0.086(3) 0.081(3) 0.000(2) -0.016(3) 0.012(3) C16 0.099(4) 0.090(4) 0.088(3) -0.005(3) -0.022(3) 0.019(3) C17 0.087(4) 0.120(5) 0.088(3) -0.013(3) -0.007(3) 0.006(3) C18 0.097(4) 0.138(5) 0.079(3) -0.002(3) -0.005(3) 0.005(4) C19 0.082(4) 0.175(6) 0.100(4) -0.008(4) -0.005(3) 0.010(4) C20 0.088(5) 0.221(9) 0.108(5) 0.006(5) -0.001(3) 0.003(5) C21 0.085(5) 0.223(9) 0.107(4) -0.001(5) 0.006(3) -0.024(6) C22 0.094(4) 0.172(6) 0.107(4) 0.005(4) 0.001(3) -0.018(4) C23 0.074(4) 0.163(6) 0.085(3) -0.001(4) -0.002(3) -0.011(4) C24 0.100(4) 0.123(5) 0.104(4) -0.006(3) 0.001(3) -0.019(4) Li 0.077(4) 0.077(4) 0.097(7) -0.002(4) 0.002(4) 0.006(5) N1 0.080(2) 0.079(2) 0.089(2) 0.0040(18) -0.008(2) 0.006(2) N2 0.083(3) 0.095(3) 0.096(3) -0.007(2) -0.015(2) 0.012(2) N3 0.086(3) 0.094(3) 0.086(2) -0.008(2) -0.009(2) 0.001(2) N4 0.093(3) 0.093(3) 0.102(4) -0.003(2) 0.003(2) -0.007(3) N5 0.086(2) 0.086(2) 0.078(3) 0.0103(19) -0.0103(19) 0.012(3) O1 0.099(2) 0.089(2) 0.090(2) 0.0008(17) -0.0017(18) 0.0014(18) O2 0.107(3) 0.098(2) 0.096(2) -0.0040(18) -0.0219(19) 0.0248(19) O3 0.097(3) 0.125(3) 0.123(3) -0.024(2) -0.027(2) 0.026(2) O4 0.111(3) 0.128(4) 0.142(4) -0.004(3) -0.002(3) -0.025(3) C25 0.105(4) 0.108(4) 0.122(4) -0.015(3) 0.001(3) 0.003(3) C26 0.175(8) 0.156(7) 0.139(6) -0.013(5) 0.042(5) 0.018(6) C27 0.165(8) 0.150(7) 0.168(7) 0.015(5) 0.038(5) -0.024(6) C28 0.177(11) 0.43(2) 0.283(16) -0.078(16) 0.085(11) -0.023(13) C29 0.118(4) 0.107(4) 0.091(3) -0.016(3) -0.020(3) 0.022(3) C30 0.124(4) 0.092(4) 0.097(3) -0.002(3) -0.013(3) 0.010(3) C31 0.128(4) 0.101(4) 0.089(3) -0.003(3) -0.022(3) 0.012(3) C32 0.112(4) 0.156(6) 0.109(4) -0.010(4) -0.027(3) 0.006(4) C33 0.098(4) 0.125(5) 0.160(6) -0.025(4) -0.031(4) 0.038(4) C34 0.144(6) 0.173(7) 0.159(6) -0.026(6) -0.010(5) 0.029(6) C35 0.171(8) 0.149(7) 0.221(10) -0.051(7) -0.037(7) 0.025(6) C36 0.263(13) 0.201(10) 0.240(12) -0.015(9) -0.141(11) 0.046(9) C37 0.109(8) 0.129(9) 0.130(10) 0.001(7) -0.001(7) -0.024(7) C38 0.149(11) 0.154(12) 0.134(11) -0.043(9) 0.025(9) -0.045(9) C40 0.121(9) 0.163(12) 0.130(10) 0.026(8) -0.021(7) -0.030(9) C37A 0.119(10) 0.105(9) 0.129(10) 0.006(8) -0.007(8) -0.005(8) C38A 0.149(12) 0.133(12) 0.098(9) 0.026(8) 0.005(9) -0.012(10) C39 0.143(6) 0.240(10) 0.114(5) -0.001(6) -0.003(5) -0.073(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N5 1.333(6) . ? C1 N1 1.353(6) . ? C1 C2 1.471(7) . ? C2 C9 1.389(7) . ? C2 C3 1.415(7) . ? C3 C16 1.375(7) . ? C3 C4 1.466(7) . ? C4 N2 1.340(6) . ? C4 N1 1.353(6) . ? C5 N2 1.339(6) . ? C5 N3 1.368(6) . ? C5 C6 1.465(7) . ? C6 C7 1.397(7) . ? C6 C17 1.407(8) . ? C7 C24 1.370(8) . ? C7 C8 1.489(7) . ? C8 N4 1.335(6) . ? C8 N3 1.355(7) . ? C9 O1 1.361(6) . ? C9 C10 1.438(7) . ? C10 C15 1.397(8) . ? C10 C11 1.414(8) . ? C11 C12 1.361(8) . ? C11 H11 0.95 . ? C12 C13 1.351(9) . ? C12 H12 0.95 . ? C13 C14 1.392(9) . ? C13 H13 0.95 . ? C14 C15 1.444(7) . ? C14 H14 0.95 . ? C15 C16 1.434(7) . ? C16 O2 1.381(6) . ? C17 O3 1.331(7) . ? C17 C18 1.406(8) . ? C18 C19 1.406(8) . ? C18 C23 1.411(9) . ? C19 C20 1.357(10) . ? C19 H19 0.95 . ? C20 C21 1.385(11) . ? C20 H20 0.95 . ? C21 C22 1.382(10) . ? C21 H21 0.95 . ? C22 C23 1.438(8) . ? C22 H22 0.95 . ? C23 C24 1.424(9) . ? C24 O4 1.369(7) . ? Li N1 1.938(9) . ? Li N1 1.938(9) 5 ? Li N3 2.007(9) . ? Li N3 2.007(9) 5 ? N4 C8 1.335(6) 5 ? N5 C1 1.333(6) 5 ? O1 C25 1.436(6) . ? O2 C29 1.455(6) . ? O3 C33 1.444(7) . ? O4 C37A 1.512(7) . ? O4 C37 1.522(7) . ? C25 C26 1.514(10) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.482(11) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.514(15) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C30 1.486(8) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.508(7) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.547(8) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 C34 1.426(9) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 C35 1.545(11) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 C36 1.480(15) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C38 1.543(9) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.533(9) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C40 C39 1.378(14) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C37A C38A 1.548(19) 5 ? C37A H37C 0.99 . ? C37A H37D 0.99 . ? C38A C37A 1.548(19) 5 ? C38A C39 1.549(9) . ? C38A H38C 0.99 . ? C38A H38D 0.99 . ? C40A C39 1.461(10) . ? C40A H40D 0.98 . ? C40A H40E 0.98 . ? C40A H40F 0.98 . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C39 H39C 0.99 . ? C39 H39D 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 N5 C1 N1 128.3(4) . . ? N5 C1 C2 121.3(4) . . ? N1 C1 C2 110.4(4) . . ? C9 C2 C3 122.0(4) . . ? C9 C2 C1 132.6(5) . . ? C3 C2 C1 105.4(4) . . ? C16 C3 C2 120.0(5) . . ? C16 C3 C4 134.6(5) . . ? C2 C3 C4 105.4(4) . . ? N2 C4 N1 126.9(4) . . ? N2 C4 C3 122.5(4) . . ? N1 C4 C3 110.6(4) . . ? N2 C5 N3 126.0(4) . . ? N2 C5 C6 123.8(4) . . ? N3 C5 C6 110.0(5) . . ? C7 C6 C17 121.2(5) . . ? C7 C6 C5 106.5(4) . . ? C17 C6 C5 132.3(6) . . ? C24 C7 C6 122.0(5) . . ? C24 C7 C8 132.7(6) . . ? C6 C7 C8 105.2(5) . . ? N4 C8 N3 126.5(5) . . ? N4 C8 C7 123.4(5) . . ? N3 C8 C7 110.0(5) . . ? O1 C9 C2 124.3(4) . . ? O1 C9 C10 117.6(5) . . ? C2 C9 C10 118.1(5) . . ? C15 C10 C11 119.3(5) . . ? C15 C10 C9 119.9(5) . . ? C11 C10 C9 120.8(5) . . ? C12 C11 C10 121.4(6) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C13 C12 C11 119.4(6) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 123.5(5) . . ? C12 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 117.5(6) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C10 C15 C16 120.4(5) . . ? C10 C15 C14 118.9(6) . . ? C16 C15 C14 120.7(6) . . ? C3 C16 O2 122.0(5) . . ? C3 C16 C15 119.5(5) . . ? O2 C16 C15 118.5(4) . . ? O3 C17 C18 116.8(5) . . ? O3 C17 C6 125.5(5) . . ? C18 C17 C6 117.6(6) . . ? C19 C18 C17 120.7(7) . . ? C19 C18 C23 118.7(6) . . ? C17 C18 C23 120.6(6) . . ? C20 C19 C18 120.4(7) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 121.7(7) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C22 C21 C20 120.7(7) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 118.2(7) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C18 C23 C24 120.7(5) . . ? C18 C23 C22 120.1(6) . . ? C24 C23 C22 119.2(7) . . ? O4 C24 C7 123.9(6) . . ? O4 C24 C23 118.2(5) . . ? C7 C24 C23 117.8(6) . . ? N1 Li N1 91.8(5) . 5 ? N1 Li N3 89.89(16) . . ? N1 Li N3 178.2(5) 5 . ? N1 Li N3 178.2(5) . 5 ? N1 Li N3 89.89(16) 5 5 ? N3 Li N3 88.5(5) . 5 ? C1 N1 C4 108.3(4) . . ? C1 N1 Li 124.4(4) . . ? C4 N1 Li 126.9(4) . . ? C5 N2 C4 124.0(4) . . ? C8 N3 C5 108.1(4) . . ? C8 N3 Li 126.3(4) . . ? C5 N3 Li 124.5(4) . . ? C8 N4 C8 124.7(6) 5 . ? C1 N5 C1 122.1(6) . 5 ? C9 O1 C25 113.9(4) . . ? C16 O2 C29 111.0(4) . . ? C17 O3 C33 117.6(5) . . ? C24 O4 C37A 109.0(7) . . ? C24 O4 C37 111.1(6) . . ? C37A O4 C37 127.5(8) . . ? O1 C25 C26 111.2(5) . . ? O1 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? O1 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108 . . ? C27 C26 C25 114.9(7) . . ? C27 C26 H26A 108.5 . . ? C25 C26 H26A 108.5 . . ? C27 C26 H26B 108.5 . . ? C25 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C26 C27 C28 110.0(10) . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 C29 C30 109.6(5) . . ? O2 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? O2 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C29 C30 C31 114.1(5) . . ? C29 C30 H30A 108.7 . . ? C31 C30 H30A 108.7 . . ? C29 C30 H30B 108.7 . . ? C31 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C30 C31 C32 112.5(5) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 O3 109.5(5) . . ? C34 C33 H33A 109.8 . . ? O3 C33 H33A 109.8 . . ? C34 C33 H33B 109.8 . . ? O3 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? C33 C34 C35 114.0(7) . . ? C33 C34 H34A 108.7 . . ? C35 C34 H34A 108.7 . . ? C33 C34 H34B 108.7 . . ? C35 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C36 C35 C34 111.3(9) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O4 C37 C38 114.9(7) . . ? O4 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? O4 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? C39 C38 C37 118.9(8) . . ? C39 C38 H38A 107.6 . . ? C37 C38 H38A 107.6 . . ? C39 C38 H38B 107.6 . . ? C37 C38 H38B 107.6 . . ? H38A C38 H38B 107 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4 C37A C38A 112.5(9) . 5 ? O4 C37A H37C 109.1 . . ? C38A C37A H37C 109.1 5 . ? O4 C37A H37D 109.1 . . ? C38A C37A H37D 109.1 5 . ? H37C C37A H37D 107.8 . . ? C37A C38A C39 111.0(10) 5 . ? C37A C38A H38C 109.4 5 . ? C39 C38A H38C 109.4 . . ? C37A C38A H38D 109.4 5 . ? C39 C38A H38D 109.4 . . ? H38C C38A H38D 108 . . ? C39 C40A H40D 109.5 . . ? C39 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C39 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C40 C39 C38 114.9(8) . . ? C40A C39 C38A 119.4(10) . . ? C40 C39 H39A 108.5 . . ? C38 C39 H39A 108.5 . . ? C40 C39 H39B 108.5 . . ? C38 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C40A C39 H39C 107.5 . . ? C38A C39 H39C 107.5 . . ? C40A C39 H39D 107.5 . . ? C38A C39 H39D 107.5 . . ? H39C C39 H39D 107 . . ? 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 N5 C1 C2 C9 -2.9(8) . . . . ? N1 C1 C2 C9 178.1(5) . . . . ? N5 C1 C2 C3 178.9(4) . . . . ? N1 C1 C2 C3 -0.1(5) . . . . ? C9 C2 C3 C16 2.5(7) . . . . ? C1 C2 C3 C16 -179.1(4) . . . . ? C9 C2 C3 C4 -179.1(4) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C16 C3 C4 N2 0.2(8) . . . . ? C2 C3 C4 N2 -177.9(4) . . . . ? C16 C3 C4 N1 179.3(5) . . . . ? C2 C3 C4 N1 1.3(5) . . . . ? N2 C5 C6 C7 -173.1(4) . . . . ? N3 C5 C6 C7 2.8(5) . . . . ? N2 C5 C6 C17 4.2(9) . . . . ? N3 C5 C6 C17 -179.8(5) . . . . ? C17 C6 C7 C24 -1.4(8) . . . . ? C5 C6 C7 C24 176.3(5) . . . . ? C17 C6 C7 C8 179.0(5) . . . . ? C5 C6 C7 C8 -3.4(5) . . . . ? C24 C7 C8 N4 2.8(9) . . . . ? C6 C7 C8 N4 -177.6(4) . . . . ? C24 C7 C8 N3 -176.6(6) . . . . ? C6 C7 C8 N3 3.0(6) . . . . ? C3 C2 C9 O1 177.2(4) . . . . ? C1 C2 C9 O1 -0.7(8) . . . . ? C3 C2 C9 C10 -4.9(7) . . . . ? C1 C2 C9 C10 177.2(5) . . . . ? O1 C9 C10 C15 -177.5(4) . . . . ? C2 C9 C10 C15 4.4(7) . . . . ? O1 C9 C10 C11 -0.6(7) . . . . ? C2 C9 C10 C11 -178.7(5) . . . . ? C15 C10 C11 C12 -2.9(8) . . . . ? C9 C10 C11 C12 -179.8(5) . . . . ? C10 C11 C12 C13 3.0(9) . . . . ? C11 C12 C13 C14 -2.6(10) . . . . ? C12 C13 C14 C15 2.0(9) . . . . ? C11 C10 C15 C16 -178.6(5) . . . . ? C9 C10 C15 C16 -1.7(7) . . . . ? C11 C10 C15 C14 2.3(8) . . . . ? C9 C10 C15 C14 179.2(5) . . . . ? C13 C14 C15 C10 -1.8(8) . . . . ? C13 C14 C15 C16 179.1(5) . . . . ? C2 C3 C16 O2 -179.0(4) . . . . ? C4 C3 C16 O2 3.1(9) . . . . ? C2 C3 C16 C15 0.5(7) . . . . ? C4 C3 C16 C15 -177.4(5) . . . . ? C10 C15 C16 C3 -0.8(8) . . . . ? C14 C15 C16 C3 178.3(5) . . . . ? C10 C15 C16 O2 178.7(4) . . . . ? C14 C15 C16 O2 -2.2(7) . . . . ? C7 C6 C17 O3 -179.4(5) . . . . ? C5 C6 C17 O3 3.6(9) . . . . ? C7 C6 C17 C18 2.6(7) . . . . ? C5 C6 C17 C18 -174.4(5) . . . . ? O3 C17 C18 C19 1.7(7) . . . . ? C6 C17 C18 C19 179.9(5) . . . . ? O3 C17 C18 C23 179.3(5) . . . . ? C6 C17 C18 C23 -2.5(8) . . . . ? C17 C18 C19 C20 -179.1(6) . . . . ? C23 C18 C19 C20 3.3(9) . . . . ? C18 C19 C20 C21 -4.5(10) . . . . ? C19 C20 C21 C22 4.3(11) . . . . ? C20 C21 C22 C23 -2.8(10) . . . . ? C19 C18 C23 C24 178.9(5) . . . . ? C17 C18 C23 C24 1.3(8) . . . . ? C19 C18 C23 C22 -1.9(8) . . . . ? C17 C18 C23 C22 -179.5(5) . . . . ? C21 C22 C23 C18 1.7(8) . . . . ? C21 C22 C23 C24 -179.0(6) . . . . ? C6 C7 C24 O4 -179.4(5) . . . . ? C8 C7 C24 O4 0.2(10) . . . . ? C6 C7 C24 C23 0.0(8) . . . . ? C8 C7 C24 C23 179.6(5) . . . . ? C18 C23 C24 O4 179.5(5) . . . . ? C22 C23 C24 O4 0.3(8) . . . . ? C18 C23 C24 C7 0.0(8) . . . . ? C22 C23 C24 C7 -179.2(5) . . . . ? N5 C1 N1 C4 -178.0(4) . . . . ? C2 C1 N1 C4 0.9(5) . . . . ? N5 C1 N1 Li 8.9(6) . . . . ? C2 C1 N1 Li -172.2(3) . . . . ? N2 C4 N1 C1 177.8(5) . . . . ? C3 C4 N1 C1 -1.3(5) . . . . ? N2 C4 N1 Li -9.4(7) . . . . ? C3 C4 N1 Li 171.5(3) . . . . ? N1 Li N1 C1 -3.9(3) 5 . . . ? N3 Li N1 C1 175.5(4) . . . . ? N1 Li N1 C4 -175.6(5) 5 . . . ? N3 Li N1 C4 3.7(4) . . . . ? N3 C5 N2 C4 11.6(7) . . . . ? C6 C5 N2 C4 -173.1(5) . . . . ? N1 C4 N2 C5 2.3(8) . . . . ? C3 C4 N2 C5 -178.7(4) . . . . ? N4 C8 N3 C5 179.4(4) . . . . ? C7 C8 N3 C5 -1.3(5) . . . . ? N4 C8 N3 Li 11.1(7) . . . . ? C7 C8 N3 Li -169.5(3) . . . . ? N2 C5 N3 C8 174.9(5) . . . . ? C6 C5 N3 C8 -0.9(5) . . . . ? N2 C5 N3 Li -16.5(6) . . . . ? C6 C5 N3 Li 167.6(3) . . . . ? N1 Li N3 C8 174.4(4) . . . . ? N3 Li N3 C8 -5.0(3) 5 . . . ? N1 Li N3 C5 7.9(4) . . . . ? N3 Li N3 C5 -171.5(4) 5 . . . ? N3 C8 N4 C8 -6.0(4) . . . 5 ? C7 C8 N4 C8 174.8(5) . . . 5 ? N1 C1 N5 C1 -4.9(4) . . . 5 ? C2 C1 N5 C1 176.3(5) . . . 5 ? C2 C9 O1 C25 -76.2(6) . . . . ? C10 C9 O1 C25 105.9(5) . . . . ? C3 C16 O2 C29 87.6(6) . . . . ? C15 C16 O2 C29 -91.9(5) . . . . ? C18 C17 O3 C33 -123.5(5) . . . . ? C6 C17 O3 C33 58.5(7) . . . . ? C7 C24 O4 C37A 71.2(8) . . . . ? C23 C24 O4 C37A -108.2(8) . . . . ? C7 C24 O4 C37 -74.1(8) . . . . ? C23 C24 O4 C37 106.4(7) . . . . ? C9 O1 C25 C26 -163.4(6) . . . . ? O1 C25 C26 C27 55.5(9) . . . . ? C25 C26 C27 C28 -178.1(8) . . . . ? C16 O2 C29 C30 -176.3(4) . . . . ? O2 C29 C30 C31 -65.3(6) . . . . ? C29 C30 C31 C32 -175.6(5) . . . . ? C17 O3 C33 C34 139.1(7) . . . . ? O3 C33 C34 C35 171.3(7) . . . . ? C33 C34 C35 C36 65.7(12) . . . . ? C24 O4 C37 C38 -153.1(9) . . . . ? C37A O4 C37 C38 69.6(13) . . . . ? O4 C37 C38 C39 -170.3(10) . . . . ? C24 O4 C37A C38A 139.2(9) . . . 5 ? C37 O4 C37A C38A -82.7(12) . . . 5 ? C37 C38 C39 C40 179.3(12) . . . . ? C37 C38 C39 C40A -69(2) . . . . ? C37 C38 C39 C38A 98.0(13) . . . . ? C37A C38A C39 C40 162.0(11) 5 . . . ? C37A C38A C39 C40A -70(2) 5 . . . ? C37A C38A C39 C38 -81.7(10) 5 . . . ? # END of CIF