# Electronic Supplementary Material (ESI) for Chemical Communications # 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_Compound_3_k08mgd02 #TrackingRef '16352_web_deposit_cif_file_0_DanielGarcia-Vivo_1356029066.LiCage_final.cif' _audit_creation_date 2010-01-07T15:04:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_common k08mgd02 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C70 H92 Li6 N2 O10, 2(C4 H8 O)' _chemical_formula_sum 'C78 H108 Li6 N2 O12' _chemical_formula_weight 1307.3634 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8870(2) _cell_length_b 13.0390(2) _cell_length_c 21.4410(3) _cell_angle_alpha 90 _cell_angle_beta 89.79 _cell_angle_gamma 90 _cell_volume 3602.78(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 109828 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 3.513 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 63006 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.53 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0072363 _diffrn_orient_matrix_ub_12 -0.0245949 _diffrn_orient_matrix_ub_13 -0.0439462 _diffrn_orient_matrix_ub_21 -0.0229693 _diffrn_orient_matrix_ub_22 -0.0686569 _diffrn_orient_matrix_ub_23 0.0156132 _diffrn_orient_matrix_ub_31 -0.0737666 _diffrn_orient_matrix_ub_32 0.0237343 _diffrn_orient_matrix_ub_33 -0.0003735 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _reflns_number_gt 7010 _reflns_number_total 8233 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_diff_density_max 0.996 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 589 _refine_ls_number_reflns 8233 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.098 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+7.4704P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2448 _refine_ls_wR_factor_ref 0.2525 #----------------------------------------------------------------------------# # 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.89329(14) 0.46391(14) 0.51325(9) 0.0255(4) Uani 1 1 d . . . C1 C 0.8543(2) 0.2499(3) 0.47429(16) 0.0266(8) Uani 0.816(5) 1 d P A 1 H10A H 0.8303 0.1778 0.4763 0.032 Uiso 0.816(5) 1 calc PR A 1 H10B H 0.8506 0.2717 0.4301 0.032 Uiso 0.816(5) 1 calc PR A 1 Li1 Li 0.9509(4) 0.4494(4) 0.6051(2) 0.0319(10) Uani 1 1 d . . . O2 O 1.00493(17) 0.40668(16) 0.39431(10) 0.0328(5) Uani 1 1 d . . . C2 C 1.0304(3) 0.1948(3) 0.45082(17) 0.0271(8) Uani 0.816(5) 1 d P A 1 H2A H 1.0159 0.1208 0.4562 0.032 Uiso 0.816(5) 1 calc PR A 1 H2B H 1.1032 0.2067 0.4635 0.032 Uiso 0.816(5) 1 calc PR A 1 Li2 Li 0.8697(4) 0.4746(4) 0.4160(2) 0.0328(11) Uani 1 1 d . . . O3 O 1.08492(16) 0.38322(15) 0.58757(11) 0.0337(5) Uani 1 1 d . . . C3 C 0.9687(3) 0.2032(3) 0.55657(15) 0.0262(8) Uani 0.816(5) 1 d P A 1 H3A H 0.9218 0.2402 0.5855 0.031 Uiso 0.816(5) 1 calc PR A 1 H3B H 0.9428 0.132 0.553 0.031 Uiso 0.816(5) 1 calc PR A 1 Li3 Li 1.0277(4) 0.3992(4) 0.4902(2) 0.0281(10) Uani 1 1 d . . . O4 O 0.88344(16) 0.36226(18) 0.67166(9) 0.0351(5) Uani 1 1 d . . . C4 C 0.8975(6) 0.2049(4) 0.7248(3) 0.0519(15) Uani 0.8 1 d P A 1 H4A H 0.9025 0.1817 0.7686 0.062 Uiso 0.8 1 calc PR A 1 H4B H 0.9322 0.1538 0.6976 0.062 Uiso 0.8 1 calc PR A 1 O5 O 0.74808(16) 0.39674(18) 0.37231(10) 0.0369(5) Uani 1 1 d . . . O6 O 0.2312(6) 0.5288(6) 0.0719(4) 0.179(3) Uani 1 1 d . . . N6 N 0.96181(17) 0.25289(18) 0.49346(11) 0.0254(5) Uani 1 1 d . A . C11 C 0.8002(2) 0.4217(2) 0.52555(13) 0.0263(6) Uani 1 1 d . . . C12 C 0.7801(4) 0.3148(4) 0.5115(2) 0.0254(10) Uani 0.816(5) 1 d P A 1 C13 C 0.6815(5) 0.2752(6) 0.5265(3) 0.0298(12) Uani 0.816(5) 1 d P A 1 H13 H 0.6684 0.2044 0.5195 0.036 Uiso 0.816(5) 1 calc PR A 1 C14 C 0.6018(2) 0.3361(3) 0.55130(14) 0.0347(7) Uani 1 1 d . . . C15 C 0.6204(2) 0.4400(3) 0.55886(15) 0.0370(7) Uani 1 1 d . A . H15 H 0.5655 0.483 0.5727 0.044 Uiso 1 1 calc R . . C16 C 0.7176(2) 0.4837(2) 0.54683(15) 0.0335(6) Uani 1 1 d . A . C17 C 0.4954(2) 0.2907(3) 0.56246(17) 0.0445(8) Uani 1 1 d . A . H17A H 0.4648 0.3211 0.6001 0.067 Uiso 1 1 calc R . . H17B H 0.5015 0.2163 0.568 0.067 Uiso 1 1 calc R . . H17C H 0.4509 0.3052 0.5266 0.067 Uiso 1 1 calc R . . C18 C 0.7355(3) 0.5974(3) 0.5557(2) 0.0507(10) Uani 1 1 d . . . H18A H 0.6721 0.6294 0.5718 0.076 Uiso 1 1 calc R A . H18B H 0.7541 0.6286 0.5156 0.076 Uiso 1 1 calc R . . H18C H 0.7921 0.6079 0.5855 0.076 Uiso 1 1 calc R . . C21 C 1.0120(2) 0.3241(2) 0.35711(13) 0.0299(6) Uani 1 1 d . . . C22 C 1.0202(3) 0.2210(3) 0.38232(16) 0.0252(7) Uani 0.816(5) 1 d P A 1 C23 C 1.0219(4) 0.1375(3) 0.34086(18) 0.0295(8) Uani 0.816(5) 1 d P A 1 H23 H 1.024 0.07 0.3575 0.035 Uiso 0.816(5) 1 calc PR A 1 C24 C 1.0207(2) 0.1499(2) 0.27640(14) 0.0338(6) Uani 1 1 d . . . C25 C 1.0208(3) 0.2483(3) 0.25346(15) 0.0421(8) Uani 1 1 d . A . H25 H 1.0232 0.2579 0.2096 0.051 Uiso 1 1 calc R . . C26 C 1.0176(3) 0.3344(2) 0.29161(14) 0.0357(7) Uani 1 1 d . A . C27 C 1.0256(3) 0.0559(3) 0.23480(16) 0.0436(8) Uani 1 1 d . A . H27A H 1.0914 0.0199 0.2416 0.065 Uiso 1 1 calc R . . H27B H 1.0208 0.0769 0.191 0.065 Uiso 1 1 calc R . . H27C H 0.9677 0.01 0.2449 0.065 Uiso 1 1 calc R . . C28 C 1.0144(4) 0.4401(3) 0.26396(16) 0.0574(11) Uani 1 1 d . . . H28A H 1.0823 0.473 0.2689 0.086 Uiso 1 1 calc R A . H28B H 0.9613 0.4809 0.2854 0.086 Uiso 1 1 calc R . . H28C H 0.9977 0.4354 0.2195 0.086 Uiso 1 1 calc R . . C31 C 1.1253(2) 0.2905(2) 0.60045(14) 0.0299(6) Uani 1 1 d . . . C32 C 1.0748(3) 0.2001(3) 0.5850(2) 0.0255(8) Uani 0.816(5) 1 d P A 1 C33 C 1.1208(4) 0.1046(4) 0.5962(2) 0.0279(10) Uani 0.816(5) 1 d P A 1 H33 H 1.0865 0.0445 0.582 0.033 Uiso 0.816(5) 1 calc PR A 1 C34 C 1.2143(2) 0.0941(2) 0.62707(13) 0.0312(6) Uani 1 1 d . . . C35 C 1.2580(3) 0.1845(3) 0.64872(15) 0.0369(7) Uani 1 1 d . A . H35 H 1.3199 0.1807 0.6726 0.044 Uiso 1 1 calc R . . C36 C 1.2151(2) 0.2807(2) 0.63706(14) 0.0334(6) Uani 1 1 d . A . C37 C 1.2611(3) -0.0099(3) 0.64090(17) 0.0444(8) Uani 1 1 d . A . H37A H 1.2844 -0.0418 0.6019 0.067 Uiso 1 1 calc R . . H37B H 1.2089 -0.0536 0.6609 0.067 Uiso 1 1 calc R . . H37C H 1.3205 -0.0016 0.6689 0.067 Uiso 1 1 calc R . . C38 C 1.2656(4) 0.3746(3) 0.6639(2) 0.0634(12) Uani 1 1 d . . . H38A H 1.3232 0.354 0.6909 0.095 Uiso 1 1 calc R A . H38B H 1.2146 0.4132 0.6885 0.095 Uiso 1 1 calc R . . H38C H 1.292 0.4178 0.63 0.095 Uiso 1 1 calc R . . C101 C 0.9452(3) 0.3077(3) 0.71691(16) 0.0419(8) Uani 1 1 d . A . H10C H 0.9454 0.3449 0.7571 0.05 Uiso 1 1 calc R B 1 H10D H 1.0176 0.301 0.702 0.05 Uiso 1 1 calc R B 1 C110 C 0.7859(6) 0.2190(6) 0.7061(4) 0.0732(18) Uani 0.8 1 d P A 1 H11A H 0.7388 0.2038 0.7415 0.088 Uiso 0.8 1 calc PR A 1 H11B H 0.768 0.1733 0.6708 0.088 Uiso 0.8 1 calc PR A 1 C125 C 0.7773(4) 0.3309(5) 0.6869(3) 0.0439(13) Uani 0.8 1 d P A 1 H12A H 0.7315 0.3385 0.6502 0.053 Uiso 0.8 1 calc PR A 1 H12B H 0.7491 0.3728 0.7215 0.053 Uiso 0.8 1 calc PR A 1 C151 C 0.2153(6) 0.6100(10) 0.1239(4) 0.163(5) Uani 1 1 d . C 1 H15A H 0.2371 0.5826 0.1648 0.195 Uiso 1 1 calc R C 1 H15B H 0.2559 0.6728 0.1147 0.195 Uiso 1 1 calc R C 1 C152 C 0.1096(4) 0.6312(6) 0.1239(3) 0.096(2) Uani 1 1 d . C 1 H15C H 0.0984 0.7058 0.1186 0.115 Uiso 1 1 calc R C 1 H15D H 0.0786 0.6103 0.1642 0.115 Uiso 1 1 calc R C 1 C153 C 0.0605(5) 0.5769(9) 0.0741(5) 0.158(4) Uani 1 1 d . C 1 H15E H 0.0055 0.6187 0.0545 0.189 Uiso 1 1 calc R C 1 H15F H 0.0302 0.5114 0.0889 0.189 Uiso 1 1 calc R C 1 C154 C 0.1475(8) 0.5587(11) 0.0306(4) 0.200(7) Uani 1 1 d . C 1 H15G H 0.131 0.5033 0.0007 0.24 Uiso 1 1 calc R C 1 H15H H 0.1653 0.6218 0.0072 0.24 Uiso 1 1 calc R C 1 C1' C 0.8806(11) 0.2489(11) 0.5403(7) 0.024(3) Uani 0.184(5) 1 d P A 2 H1'1 H 0.9135 0.2594 0.5814 0.028 Uiso 0.184(5) 1 calc PR A 2 H1'2 H 0.8518 0.1785 0.5402 0.028 Uiso 0.184(5) 1 calc PR A 2 C2' C 0.8992(12) 0.2303(12) 0.4292(6) 0.026(3) Uani 0.184(5) 1 d P A 2 H2'1 H 0.8697 0.1603 0.4314 0.032 Uiso 0.184(5) 1 calc PR A 2 H2'2 H 0.8405 0.2791 0.4263 0.032 Uiso 0.184(5) 1 calc PR A 2 C3' C 1.0410(11) 0.1897(12) 0.4960(7) 0.026(3) Uani 0.184(5) 1 d P A 2 H3'1 H 1.0885 0.2047 0.4608 0.031 Uiso 0.184(5) 1 calc PR A 2 H3'2 H 1.0154 0.1187 0.4907 0.031 Uiso 0.184(5) 1 calc PR A 2 C12' C 0.7883(15) 0.324(2) 0.5357(11) 0.029(5) Uani 0.184(5) 1 d P A 2 C13' C 0.694(3) 0.280(2) 0.5478(13) 0.033(6) Uani 0.184(5) 1 d P A 2 H13' H 0.6905 0.2084 0.5541 0.039 Uiso 0.184(5) 1 calc PR A 2 C22' C 0.9635(16) 0.2389(12) 0.3707(7) 0.028(3) Uani 0.184(5) 1 d P A 2 C23' C 0.9770(16) 0.1507(14) 0.3347(8) 0.026(4) Uiso 0.184(5) 1 d P A 2 H23' H 0.9546 0.0871 0.3518 0.032 Uiso 0.184(5) 1 calc PR A 2 C32' C 1.1025(13) 0.1963(12) 0.5574(9) 0.023(3) Uani 0.184(5) 1 d P A 2 C33' C 1.146(2) 0.103(2) 0.5753(12) 0.034(5) Uani 0.184(5) 1 d P A 2 H33' H 1.1289 0.0428 0.5522 0.041 Uiso 0.184(5) 1 calc PR A 2 C5 C 0.6411(3) 0.3890(6) 0.3881(3) 0.0332(16) Uani 0.83(2) 1 d P A 2 H5A H 0.6008 0.4446 0.3682 0.04 Uiso 0.83(2) 1 calc PR A 2 H5B H 0.6312 0.3929 0.4339 0.04 Uiso 0.83(2) 1 calc PR A 2 C6 C 0.6622(6) 0.2792(4) 0.3008(4) 0.0512(16) Uani 0.83(2) 1 d P A 2 H6A H 0.681 0.2077 0.2899 0.061 Uiso 0.83(2) 1 calc PR A 2 H6B H 0.6194 0.3089 0.2671 0.061 Uiso 0.83(2) 1 calc PR A 2 C7 C 0.7560(3) 0.3429(4) 0.3136(2) 0.0643(12) Uani 1 1 d . A . H7A H 0.818 0.2981 0.3143 0.077 Uiso 1 1 calc R D 2 H7B H 0.7652 0.3933 0.2795 0.077 Uiso 1 1 calc R D 2 C8 C 0.6076(6) 0.2852(5) 0.3636(4) 0.0458(19) Uani 0.83(2) 1 d P A 2 H8A H 0.5314 0.2818 0.3588 0.055 Uiso 0.83(2) 1 calc PR A 2 H8B H 0.6305 0.2293 0.3916 0.055 Uiso 0.83(2) 1 calc PR A 2 C29 C 0.873(4) 0.271(4) 0.763(2) 0.060(11) Uani 0.1 1 d PU A 2 H29A H 0.9026 0.2741 0.8051 0.072 Uiso 0.1 1 calc PR A 2 H29B H 0.851 0.1998 0.7536 0.072 Uiso 0.1 1 calc PR A 2 C290 C 0.859(5) 0.235(5) 0.741(4) 0.067(14) Uani 0.1 1 d PU A 5 H29C H 0.8695 0.1662 0.723 0.08 Uiso 0.1 1 calc PR A 5 H29D H 0.8637 0.2297 0.7868 0.08 Uiso 0.1 1 calc PR A 5 C30 C 0.7840(19) 0.385(3) 0.6968(12) 0.060(7) Uani 0.2 1 d P A 2 H30A H 0.772 0.4596 0.698 0.072 Uiso 0.2 1 calc PR A 2 H30B H 0.7289 0.3523 0.6715 0.072 Uiso 0.2 1 calc PR A 2 C300 C 0.78 0.38 0.7 0.05 Uiso 0 1 d P A 5 H30C H 0.7269 0.3986 0.6687 0.06 Uiso 0 1 calc PR A 5 H30D H 0.7817 0.4321 0.7336 0.06 Uiso 0 1 calc PR A 5 C39 C 0.785(4) 0.345(7) 0.7552(19) 0.10(2) Uani 0.1 1 d P A 2 H39A H 0.7186 0.3094 0.7635 0.115 Uiso 0.1 1 calc PR A 2 H39B H 0.7923 0.4012 0.7859 0.115 Uiso 0.1 1 calc PR A 2 C390 C 0.765(3) 0.268(4) 0.726(2) 0.045(11) Uani 0.1 1 d P A 5 H39C H 0.7192 0.2684 0.7631 0.055 Uiso 0.1 1 calc PR A 5 H39D H 0.7339 0.2231 0.6938 0.055 Uiso 0.1 1 calc PR A 5 C9 C 0.585(3) 0.329(5) 0.3798(12) 0.058(12) Uani 0.17(2) 1 d P A 1 H9A H 0.5846 0.2781 0.4138 0.07 Uiso 0.17(2) 1 calc PR A 1 H9B H 0.5115 0.3438 0.3687 0.07 Uiso 0.17(2) 1 calc PR A 1 C10 C 0.635(2) 0.428(3) 0.4033(15) 0.043(7) Uiso 0.17(2) 1 d P A 1 H10E H 0.6369 0.4334 0.4494 0.052 Uiso 0.17(2) 1 calc PR A 1 H10F H 0.6048 0.4911 0.3849 0.052 Uiso 0.17(2) 1 calc PR A 1 C19 C 0.6406(17) 0.2849(16) 0.3231(17) 0.025(5) Uiso 0.17(2) 1 d P A 1 H19A H 0.5977 0.2951 0.2853 0.03 Uiso 0.17(2) 1 calc PR A 1 H19B H 0.651 0.2103 0.3289 0.03 Uiso 0.17(2) 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0200(9) 0.0254(9) 0.0310(10) 0.0003(8) 0.0018(7) -0.0028(7) C1 0.0251(16) 0.0239(16) 0.0308(18) 0.0015(13) -0.0068(13) -0.0030(13) Li1 0.030(2) 0.032(3) 0.033(2) -0.002(2) 0.0003(19) 0.002(2) O2 0.0376(11) 0.0288(10) 0.0320(11) -0.0082(8) 0.0072(8) -0.0064(9) C2 0.0280(17) 0.0222(16) 0.031(2) -0.0017(13) -0.0049(13) 0.0033(13) Li2 0.030(2) 0.032(3) 0.036(3) 0.002(2) -0.006(2) -0.004(2) O3 0.0281(10) 0.0249(10) 0.0481(13) 0.0061(9) -0.0070(9) -0.0011(8) C3 0.0277(17) 0.0244(16) 0.0263(16) 0.0051(13) -0.0030(12) -0.0040(13) Li3 0.028(2) 0.026(2) 0.031(2) -0.0019(18) -0.0001(18) -0.0022(18) O4 0.0332(11) 0.0453(13) 0.0270(10) 0.0052(9) -0.0007(8) -0.0036(9) C4 0.086(5) 0.035(3) 0.035(3) 0.0037(19) 0.006(3) -0.004(3) O5 0.0249(10) 0.0441(13) 0.0417(12) 0.0083(10) -0.0104(9) -0.0062(9) O6 0.159(6) 0.147(6) 0.231(8) -0.039(6) 0.021(6) 0.043(5) N6 0.0244(11) 0.0250(11) 0.0269(11) -0.0017(9) -0.0002(9) -0.0019(9) C11 0.0207(12) 0.0298(14) 0.0285(13) 0.0031(11) 0.0002(10) -0.0017(10) C12 0.0238(19) 0.025(2) 0.027(3) -0.001(2) -0.005(2) -0.0038(15) C13 0.023(2) 0.034(2) 0.032(3) 0.006(3) -0.009(2) -0.0075(18) C14 0.0245(13) 0.0489(18) 0.0307(14) 0.0057(13) 0.0013(11) -0.0079(13) C15 0.0236(14) 0.0467(18) 0.0407(17) -0.0034(14) 0.0058(12) 0.0007(13) C16 0.0258(14) 0.0351(16) 0.0397(16) -0.0048(13) 0.0035(11) -0.0010(12) C17 0.0274(15) 0.058(2) 0.0484(19) 0.0002(16) 0.0050(13) -0.0109(14) C18 0.0317(16) 0.0377(18) 0.082(3) -0.0168(18) 0.0130(17) 0.0008(14) C21 0.0292(14) 0.0302(14) 0.0302(14) -0.0076(11) 0.0030(11) -0.0057(11) C22 0.0225(18) 0.0267(17) 0.0264(17) -0.0041(13) -0.0046(14) 0.0015(14) C23 0.029(2) 0.0257(18) 0.0340(19) -0.0051(14) -0.0035(15) -0.0003(15) C24 0.0323(15) 0.0359(16) 0.0332(15) -0.0108(12) -0.0055(12) -0.0001(12) C25 0.061(2) 0.0399(18) 0.0260(15) -0.0043(13) -0.0047(14) 0.0003(16) C26 0.0449(17) 0.0331(16) 0.0291(15) -0.0019(12) -0.0084(12) 0.0015(13) C27 0.056(2) 0.0381(17) 0.0363(17) -0.0124(14) -0.0006(15) -0.0010(15) C28 0.103(3) 0.041(2) 0.0280(17) 0.0022(14) -0.0076(18) 0.000(2) C31 0.0249(13) 0.0279(14) 0.0370(15) 0.0064(12) -0.0008(11) -0.0003(11) C32 0.0278(19) 0.0280(18) 0.0206(19) 0.0038(16) 0.0005(15) 0.0006(14) C33 0.032(3) 0.027(2) 0.025(3) 0.004(2) -0.0014(19) 0.0002(18) C34 0.0337(15) 0.0322(15) 0.0277(14) 0.0042(11) -0.0009(11) 0.0057(12) C35 0.0377(16) 0.0379(17) 0.0351(16) 0.0045(13) -0.0111(12) 0.0033(13) C36 0.0368(16) 0.0325(15) 0.0310(15) 0.0037(12) -0.0058(12) -0.0002(12) C37 0.051(2) 0.0369(17) 0.0456(19) 0.0017(14) -0.0137(15) 0.0110(15) C38 0.069(3) 0.039(2) 0.082(3) -0.004(2) -0.043(2) 0.0022(18) C101 0.0420(18) 0.0476(19) 0.0362(16) 0.0126(14) 0.0022(13) 0.0063(15) C110 0.071(4) 0.068(4) 0.080(5) 0.018(4) 0.000(4) -0.026(4) C125 0.033(2) 0.069(4) 0.029(2) 0.009(3) -0.0008(18) -0.012(3) C151 0.098(5) 0.280(13) 0.110(6) -0.064(7) 0.009(4) 0.051(7) C152 0.067(3) 0.159(6) 0.062(3) -0.014(4) 0.007(2) 0.051(4) C153 0.054(3) 0.213(10) 0.207(10) -0.096(8) -0.019(5) 0.041(5) C154 0.153(8) 0.355(17) 0.093(5) -0.003(8) -0.004(5) 0.165(10) C1' 0.022(7) 0.025(7) 0.024(7) -0.003(5) 0.007(5) -0.003(5) C2' 0.029(7) 0.035(8) 0.015(6) -0.004(5) 0.005(5) 0.000(6) C3' 0.029(7) 0.031(8) 0.018(8) 0.002(6) -0.002(5) 0.004(6) C12' 0.008(7) 0.047(11) 0.031(12) -0.032(11) 0.003(8) 0.003(6) C13' 0.037(11) 0.026(9) 0.037(16) -0.005(11) -0.030(11) 0.001(7) C22' 0.032(9) 0.031(8) 0.022(7) 0.002(6) 0.000(6) 0.007(7) C32' 0.021(8) 0.025(8) 0.021(9) 0.000(7) -0.007(6) 0.005(6) C33' 0.045(13) 0.020(8) 0.037(14) 0.006(9) 0.017(9) 0.008(8) C5 0.0216(19) 0.043(3) 0.035(2) 0.005(2) -0.0055(14) -0.0007(18) C6 0.066(3) 0.051(3) 0.037(3) -0.001(2) 0.002(3) -0.010(2) C7 0.052(2) 0.095(3) 0.046(2) -0.011(2) -0.0158(17) -0.026(2) C8 0.052(3) 0.046(3) 0.040(4) 0.006(2) -0.015(3) -0.023(2) C29 0.06(2) 0.07(3) 0.05(2) -0.002(19) -0.011(18) -0.02(2) C290 0.06(2) 0.06(3) 0.08(3) 0.00(2) 0.00(2) -0.05(2) C30 0.033(10) 0.10(2) 0.050(13) -0.021(15) -0.004(8) 0.004(14) C39 0.05(2) 0.22(8) 0.024(18) 0.03(3) 0.007(16) 0.03(4) C390 0.021(16) 0.07(3) 0.05(2) -0.03(2) 0.019(14) -0.028(17) C9 0.039(14) 0.11(3) 0.021(10) -0.021(15) 0.009(9) -0.045(18) _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 Li1 2.116(5) . ? O1 Li2 2.112(5) . ? O1 Li3 2.056(5) 3_766 ? O1 Li3 1.987(5) . ? O1 C11 1.345(3) . ? C1 H10A 0.99 . ? C1 H10B 0.99 . ? C1 N6 1.447(4) . ? C1 C12 1.503(6) . ? Li1 O2 1.961(6) 3_766 ? Li1 Li2 2.554(7) 3_766 ? Li1 O3 1.965(5) . ? Li1 Li3 2.854(7) 3_766 ? Li1 Li3 2.731(7) . ? Li1 O4 2.019(6) . ? Li1 C11 2.615(6) . ? O2 Li1 1.961(6) 3_766 ? O2 Li2 2.008(6) . ? O2 Li3 2.081(5) . ? O2 C21 1.343(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C2 N6 1.478(4) . ? C2 C22 1.514(5) . ? Li2 Li1 2.554(7) 3_766 ? Li2 O3 1.945(5) 3_766 ? Li2 Li3 2.918(7) 3_766 ? Li2 Li3 2.769(7) . ? Li2 O5 2.092(5) . ? Li2 C11 2.603(6) . ? O3 Li2 1.945(5) 3_766 ? O3 Li3 2.226(5) . ? O3 C31 1.345(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C3 N6 1.503(4) . ? C3 C32 1.500(5) . ? Li3 O1 2.056(5) 3_766 ? Li3 Li1 2.854(7) 3_766 ? Li3 Li2 2.918(7) 3_766 ? Li3 Li3 2.755(10) 3_766 ? Li3 N6 2.089(5) . ? Li3 C3' 2.740(16) . ? O4 C101 1.444(4) . ? O4 C125 1.463(6) . ? O4 C30 1.42(2) . ? O4 C300 1.481(2) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C4 C101 1.484(7) . ? C4 C110 1.506(10) . ? O5 C5 1.422(4) . ? O5 C7 1.444(5) . ? O5 C10 1.65(3) . ? O6 C151 1.550(10) . ? O6 C154 1.451(10) . ? N6 C1' 1.449(13) . ? N6 C2' 1.626(14) . ? N6 C3' 1.313(15) . ? C11 C12 1.451(6) . ? C11 C16 1.411(4) . ? C11 C12' 1.30(3) . ? C12 C13 1.408(8) . ? C13 H13 0.95 . ? C13 C14 1.402(8) . ? C14 C15 1.385(5) . ? C14 C17 1.512(4) . ? C14 C13' 1.39(3) . ? C15 H15 0.95 . ? C15 C16 1.398(4) . ? C16 C18 1.513(5) . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C21 C22 1.453(5) . ? C21 C26 1.412(4) . ? C21 C22' 1.307(17) . ? C22 C23 1.406(5) . ? C23 H23 0.95 . ? C23 C24 1.392(5) . ? C24 C25 1.374(5) . ? C24 C27 1.518(4) . ? C24 C23' 1.369(17) . ? C25 H25 0.95 . ? C25 C26 1.389(4) . ? C26 C28 1.501(5) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C31 C32 1.387(5) . ? C31 C36 1.406(4) . ? C31 C32' 1.564(17) . ? C32 C33 1.401(7) . ? C33 H33 0.95 . ? C33 C34 1.384(6) . ? C34 C35 1.387(4) . ? C34 C37 1.514(4) . ? C34 C33' 1.43(3) . ? C35 H35 0.95 . ? C35 C36 1.394(4) . ? C36 C38 1.502(5) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C101 H10C 0.99 . ? C101 H10D 0.99 . ? C101 C29 1.43(5) . ? C101 C290 1.55(5) . ? C110 H11A 0.99 . ? C110 H11B 0.99 . ? C110 C125 1.520(9) . ? C125 H12A 0.99 . ? C125 H12B 0.99 . ? C151 H15A 0.99 . ? C151 H15B 0.99 . ? C151 C152 1.390(9) . ? C152 H15C 0.99 . ? C152 H15D 0.99 . ? C152 C153 1.430(10) . ? C153 H15E 0.99 . ? C153 H15F 0.99 . ? C153 C154 1.475(11) . ? C154 H15G 0.99 . ? C154 H15H 0.99 . ? C1' H1'1 0.99 . ? C1' H1'2 0.99 . ? C1' C12' 1.55(3) . ? C2' H2'1 0.99 . ? C2' H2'2 0.99 . ? C2' C22' 1.50(2) . ? C3' H3'1 0.99 . ? C3' H3'2 0.99 . ? C3' C32' 1.54(2) . ? C12' C13' 1.37(4) . ? C13' H13' 0.95 . ? C22' C23' 1.40(2) . ? C23' H23' 0.95 . ? C32' C33' 1.40(3) . ? C33' H33' 0.95 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C5 C8 1.514(7) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C6 C7 1.493(7) . ? C6 C8 1.520(8) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C7 C19 1.68(2) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C29 C39 1.50(8) . ? C290 H29C 0.99 . ? C290 H29D 0.99 . ? C290 C390 1.32(8) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C30 C39 1.36(5) . ? C300 H30C 0.99 . ? C300 H30D 0.99 . ? C300 C390 1.57(5) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C390 H39C 0.99 . ? C390 H39D 0.99 . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C9 C10 1.53(4) . ? C9 C19 1.53(3) . ? C10 H10E 0.99 . ? C10 H10F 0.99 . ? C19 H19A 0.99 . ? C19 H19B 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 Li2 O1 Li1 167.6(2) . . ? Li3 O1 Li1 83.4(2) . . ? Li3 O1 Li1 86.3(2) 3_766 . ? Li3 O1 Li2 88.9(2) 3_766 . ? Li3 O1 Li2 84.9(2) . . ? Li3 O1 Li3 85.9(2) . 3_766 ? C11 O1 Li1 95.5(2) . . ? C11 O1 Li2 95.1(2) . . ? C11 O1 Li3 130.6(2) . . ? C11 O1 Li3 143.5(2) . 3_766 ? H10A C1 H10B 107.4 . . ? N6 C1 H10A 108.2 . . ? N6 C1 H10B 108.2 . . ? N6 C1 C12 116.2(3) . . ? C12 C1 H10A 108.2 . . ? C12 C1 H10B 108.2 . . ? O1 Li1 Li2 96.9(2) . 3_766 ? O1 Li1 Li3 46.28(15) . . ? O1 Li1 Li3 45.96(15) . 3_766 ? O1 Li1 C11 30.79(10) . . ? O2 Li1 O1 91.3(2) 3_766 . ? O2 Li1 Li2 50.78(18) 3_766 3_766 ? O2 Li1 O3 99.6(2) 3_766 . ? O2 Li1 Li3 97.5(2) 3_766 . ? O2 Li1 Li3 46.80(16) 3_766 3_766 ? O2 Li1 O4 131.2(3) 3_766 . ? O2 Li1 C11 110.6(2) 3_766 . ? Li2 Li1 Li3 66.93(19) 3_766 . ? Li2 Li1 Li3 61.30(18) 3_766 3_766 ? Li2 Li1 C11 127.7(2) 3_766 . ? O3 Li1 O1 99.9(2) . . ? O3 Li1 Li2 48.88(17) . 3_766 ? O3 Li1 Li3 53.63(17) . . ? O3 Li1 Li3 94.8(2) . 3_766 ? O3 Li1 O4 105.3(2) . . ? O3 Li1 C11 117.9(2) . . ? Li3 Li1 Li3 59.1(2) . 3_766 ? O4 Li1 O1 123.8(3) . . ? O4 Li1 Li2 137.0(3) . 3_766 ? O4 Li1 Li3 159.4(3) . 3_766 ? O4 Li1 Li3 131.0(3) . . ? O4 Li1 C11 93.7(2) . . ? C11 Li1 Li3 72.43(17) . 3_766 ? C11 Li1 Li3 69.25(17) . . ? Li1 O2 Li2 80.1(2) 3_766 . ? Li1 O2 Li3 89.8(2) 3_766 . ? Li2 O2 Li3 85.2(2) . . ? C21 O2 Li1 138.8(2) . 3_766 ? C21 O2 Li2 123.2(2) . . ? C21 O2 Li3 122.7(2) . . ? H2A C2 H2B 107.5 . . ? N6 C2 H2A 108.4 . . ? N6 C2 H2B 108.4 . . ? N6 C2 C22 115.5(3) . . ? C22 C2 H2A 108.4 . . ? C22 C2 H2B 108.4 . . ? O1 Li2 Li1 93.9(2) . 3_766 ? O1 Li2 Li3 44.78(14) . 3_766 ? O1 Li2 Li3 45.62(15) . . ? O1 Li2 C11 30.97(11) . . ? Li1 Li2 Li3 59.43(18) 3_766 3_766 ? Li1 Li2 Li3 64.71(19) 3_766 . ? Li1 Li2 C11 124.8(2) 3_766 . ? O2 Li2 O1 94.1(2) . . ? O2 Li2 Li1 49.13(17) . 3_766 ? O2 Li2 Li3 48.48(16) . . ? O2 Li2 Li3 90.8(2) . 3_766 ? O2 Li2 O5 109.4(3) . . ? O2 Li2 C11 112.8(2) . . ? O3 Li2 O1 93.3(2) 3_766 . ? O3 Li2 Li1 49.57(17) 3_766 3_766 ? O3 Li2 O2 98.7(2) 3_766 . ? O3 Li2 Li3 49.69(16) 3_766 3_766 ? O3 Li2 Li3 98.0(2) 3_766 . ? O3 Li2 O5 132.1(3) 3_766 . ? O3 Li2 C11 113.0(2) 3_766 . ? Li3 Li2 Li3 57.88(19) . 3_766 ? O5 Li2 O1 121.4(3) . . ? O5 Li2 Li1 142.0(3) . 3_766 ? O5 Li2 Li3 157.6(3) . 3_766 ? O5 Li2 Li3 129.7(3) . . ? O5 Li2 C11 91.1(2) . . ? C11 Li2 Li3 71.53(17) . 3_766 ? C11 Li2 Li3 68.82(17) . . ? Li1 O3 Li3 81.1(2) . . ? Li2 O3 Li1 81.6(2) 3_766 . ? Li2 O3 Li3 88.5(2) 3_766 . ? C31 O3 Li1 134.1(2) . . ? C31 O3 Li2 138.4(2) . 3_766 ? C31 O3 Li3 114.0(2) . . ? H3A C3 H3B 107.4 . . ? N6 C3 H3A 108.3 . . ? N6 C3 H3B 108.3 . . ? C32 C3 H3A 108.3 . . ? C32 C3 H3B 108.3 . . ? C32 C3 N6 115.7(3) . . ? O1 Li3 O1 94.1(2) . 3_766 ? O1 Li3 Li1 90.1(2) 3_766 . ? O1 Li3 Li1 50.34(16) . . ? O1 Li3 Li1 47.73(15) 3_766 3_766 ? O1 Li3 Li1 88.1(2) . 3_766 ? O1 Li3 O2 89.7(2) 3_766 . ? O1 Li3 O2 95.7(2) . . ? O1 Li3 Li2 92.1(2) 3_766 . ? O1 Li3 Li2 46.36(15) 3_766 3_766 ? O1 Li3 Li2 49.45(16) . . ? O1 Li3 Li2 89.2(2) . 3_766 ? O1 Li3 O3 95.6(2) . . ? O1 Li3 O3 87.10(19) 3_766 . ? O1 Li3 Li3 46.00(15) 3_766 3_766 ? O1 Li3 Li3 48.11(16) . 3_766 ? O1 Li3 N6 91.5(2) . . ? O1 Li3 N6 174.3(3) 3_766 . ? O1 Li3 C3' 146.7(4) 3_766 . ? O1 Li3 C3' 117.8(4) . . ? Li1 Li3 Li1 120.9(2) . 3_766 ? Li1 Li3 Li2 99.7(2) . . ? Li1 Li3 Li2 53.63(17) . 3_766 ? Li1 Li3 Li2 93.5(2) 3_766 3_766 ? Li1 Li3 Li3 62.7(2) . 3_766 ? Li1 Li3 C3' 102.8(4) . . ? O2 Li3 Li1 43.39(15) . 3_766 ? O2 Li3 Li1 146.0(3) . . ? O2 Li3 Li2 136.1(2) . 3_766 ? O2 Li3 Li2 46.29(16) . . ? O2 Li3 O3 168.4(3) . . ? O2 Li3 Li3 93.9(3) . 3_766 ? O2 Li3 N6 91.0(2) . . ? O2 Li3 C3' 95.8(4) . . ? Li2 Li3 Li1 54.00(17) . 3_766 ? Li2 Li3 Li2 122.12(19) . 3_766 ? O3 Li3 Li1 45.31(15) . . ? O3 Li3 Li1 134.8(2) . 3_766 ? O3 Li3 Li2 41.78(14) . 3_766 ? O3 Li3 Li2 145.0(2) . . ? O3 Li3 Li3 91.9(2) . 3_766 ? O3 Li3 C3' 81.0(3) . . ? Li3 Li3 Li1 58.2(2) 3_766 3_766 ? Li3 Li3 Li2 58.3(2) 3_766 3_766 ? Li3 Li3 Li2 63.8(2) 3_766 . ? N6 Li3 Li1 133.9(2) . 3_766 ? N6 Li3 Li1 92.5(2) . . ? N6 Li3 Li2 92.5(2) . . ? N6 Li3 Li2 132.6(2) . 3_766 ? N6 Li3 O3 91.1(2) . . ? N6 Li3 Li3 139.6(3) . 3_766 ? N6 Li3 C3' 27.6(3) . . ? C3' Li3 Li1 135.7(4) . 3_766 ? C3' Li3 Li2 120.2(4) . 3_766 ? C3' Li3 Li2 115.2(4) . . ? C3' Li3 Li3 163.8(4) . 3_766 ? C101 O4 Li1 121.0(2) . . ? C101 O4 C125 103.2(3) . . ? C101 O4 C300 107.37(19) . . ? C125 O4 Li1 135.7(3) . . ? C125 O4 C300 27.5(3) . . ? C30 O4 Li1 122.6(14) . . ? C30 O4 C101 110.2(13) . . ? C30 O4 C300 3.3(14) . . ? C300 O4 Li1 125.94(19) . . ? H4A C4 H4B 108.9 . . ? C101 C4 H4A 110.8 . . ? C101 C4 H4B 110.8 . . ? C101 C4 C110 104.8(5) . . ? C110 C4 H4A 110.8 . . ? C110 C4 H4B 110.8 . . ? C5 O5 Li2 130.9(4) . . ? C5 O5 C7 103.8(4) . . ? C7 O5 Li2 125.2(3) . . ? C7 O5 C10 122.1(13) . . ? C10 O5 Li2 111.1(13) . . ? C154 O6 C151 99.1(7) . . ? C1 N6 C2 112.4(2) . . ? C1 N6 C3 107.7(2) . . ? C1 N6 Li3 113.9(2) . . ? C1 N6 C1' 60.4(6) . . ? C2 N6 C3 107.4(2) . . ? C2 N6 Li3 101.8(2) . . ? C2 N6 C2' 71.4(5) . . ? C3 N6 Li3 113.5(2) . . ? C3 N6 C2' 135.7(6) . . ? C1' N6 C2 147.1(6) . . ? C1' N6 C3 53.5(6) . . ? C1' N6 Li3 110.4(6) . . ? C1' N6 C2' 102.8(8) . . ? C2' N6 Li3 109.9(6) . . ? C3' N6 C1 137.7(7) . . ? C3' N6 C3 69.1(7) . . ? C3' N6 Li3 105.0(7) . . ? C3' N6 C1' 120.6(9) . . ? C3' N6 C2' 108.0(9) . . ? O1 C11 Li1 53.66(17) . . ? O1 C11 Li2 53.92(16) . . ? O1 C11 C12 120.8(3) . . ? O1 C11 C16 120.1(3) . . ? Li2 C11 Li1 107.35(18) . . ? C12 C11 Li1 113.7(3) . . ? C12 C11 Li2 97.4(3) . . ? C16 C11 Li1 105.8(2) . . ? C16 C11 Li2 113.4(2) . . ? C16 C11 C12 118.8(3) . . ? C12' C11 O1 122.5(9) . . ? C12' C11 Li1 96.5(10) . . ? C12' C11 Li2 116.8(9) . . ? C12' C11 C16 114.7(9) . . ? C11 C12 C1 122.6(4) . . ? C13 C12 C1 119.1(5) . . ? C13 C12 C11 117.8(5) . . ? C12 C13 H13 118.7 . . ? C14 C13 C12 122.6(6) . . ? C14 C13 H13 118.7 . . ? C13 C14 C17 120.0(4) . . ? C15 C14 C13 118.1(4) . . ? C15 C14 C17 121.5(3) . . ? C15 C14 C13' 111.6(13) . . ? C13' C14 C17 125.1(14) . . ? C14 C15 H15 118.9 . . ? C14 C15 C16 122.2(3) . . ? C16 C15 H15 118.9 . . ? C11 C16 C18 119.1(3) . . ? C15 C16 C11 120.1(3) . . ? C15 C16 C18 120.9(3) . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C21 C22 121.7(3) . . ? O2 C21 C26 121.2(3) . . ? C26 C21 C22 117.0(3) . . ? C22' C21 O2 121.1(7) . . ? C22' C21 C26 109.0(7) . . ? C21 C22 C2 125.2(3) . . ? C23 C22 C2 115.9(3) . . ? C23 C22 C21 118.9(3) . . ? C22 C23 H23 118.7 . . ? C24 C23 C22 122.5(3) . . ? C24 C23 H23 118.7 . . ? C23 C24 C27 119.3(3) . . ? C25 C24 C23 117.7(3) . . ? C25 C24 C27 123.0(3) . . ? C23' C24 C25 108.7(8) . . ? C23' C24 C27 123.9(8) . . ? C24 C25 H25 118.5 . . ? C24 C25 C26 122.9(3) . . ? C26 C25 H25 118.5 . . ? C21 C26 C28 118.6(3) . . ? C25 C26 C21 120.7(3) . . ? C25 C26 C28 120.7(3) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C31 C32 122.2(3) . . ? O3 C31 C36 121.1(3) . . ? O3 C31 C32' 120.7(6) . . ? C32 C31 C36 116.4(3) . . ? C36 C31 C32' 114.5(6) . . ? C31 C32 C3 120.2(3) . . ? C31 C32 C33 121.0(4) . . ? C33 C32 C3 118.7(4) . . ? C32 C33 H33 118.7 . . ? C34 C33 C32 122.6(4) . . ? C34 C33 H33 118.7 . . ? C33 C34 C35 115.6(3) . . ? C33 C34 C37 122.0(3) . . ? C35 C34 C37 122.2(3) . . ? C35 C34 C33' 116.6(11) . . ? C33' C34 C37 118.1(11) . . ? C34 C35 H35 118.5 . . ? C34 C35 C36 122.9(3) . . ? C36 C35 H35 118.5 . . ? C31 C36 C38 119.9(3) . . ? C35 C36 C31 120.6(3) . . ? C35 C36 C38 119.4(3) . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C101 C4 107.0(4) . . ? O4 C101 H10C 110.3 . . ? O4 C101 H10D 110.3 . . ? O4 C101 C290 97(3) . . ? C4 C101 H10C 110.3 . . ? C4 C101 H10D 110.3 . . ? H10C C101 H10D 108.6 . . ? C29 C101 O4 105(2) . . ? C29 C101 C4 50(2) . . ? C29 C101 H10C 64.6 . . ? C29 C101 H10D 143.3 . . ? C290 C101 H10C 90.8 . . ? C290 C101 H10D 137.1 . . ? C4 C110 H11A 110.7 . . ? C4 C110 H11B 110.7 . . ? C4 C110 C125 105.0(5) . . ? H11A C110 H11B 108.8 . . ? C125 C110 H11A 110.7 . . ? C125 C110 H11B 110.7 . . ? O4 C125 C110 105.1(5) . . ? O4 C125 H12A 110.7 . . ? O4 C125 H12B 110.7 . . ? C110 C125 H12A 110.7 . . ? C110 C125 H12B 110.7 . . ? H12A C125 H12B 108.8 . . ? O6 C151 H15A 110.7 . . ? O6 C151 H15B 110.7 . . ? H15A C151 H15B 108.8 . . ? C152 C151 O6 105.2(7) . . ? C152 C151 H15A 110.7 . . ? C152 C151 H15B 110.7 . . ? C151 C152 H15C 109.7 . . ? C151 C152 H15D 109.7 . . ? C151 C152 C153 109.7(6) . . ? H15C C152 H15D 108.2 . . ? C153 C152 H15C 109.7 . . ? C153 C152 H15D 109.7 . . ? C152 C153 H15E 111.3 . . ? C152 C153 H15F 111.3 . . ? C152 C153 C154 102.4(7) . . ? H15E C153 H15F 109.2 . . ? C154 C153 H15E 111.3 . . ? C154 C153 H15F 111.3 . . ? O6 C154 C153 102.8(7) . . ? O6 C154 H15G 111.2 . . ? O6 C154 H15H 111.2 . . ? C153 C154 H15G 111.2 . . ? C153 C154 H15H 111.2 . . ? H15G C154 H15H 109.1 . . ? N6 C1' H1'1 107.5 . . ? N6 C1' H1'2 107.5 . . ? N6 C1' C12' 119.1(14) . . ? H1'1 C1' H1'2 107 . . ? C12' C1' H1'1 107.5 . . ? C12' C1' H1'2 107.5 . . ? N6 C2' H2'1 108.6 . . ? N6 C2' H2'2 108.6 . . ? H2'1 C2' H2'2 107.5 . . ? C22' C2' N6 114.8(12) . . ? C22' C2' H2'1 108.6 . . ? C22' C2' H2'2 108.6 . . ? Li3 C3' H3'1 78.9 . . ? Li3 C3' H3'2 155 . . ? N6 C3' H3'1 108.8 . . ? N6 C3' H3'2 108.8 . . ? N6 C3' C32' 113.7(12) . . ? H3'1 C3' H3'2 107.7 . . ? C32' C3' Li3 90.9(9) . . ? C32' C3' H3'1 108.8 . . ? C32' C3' H3'2 108.8 . . ? C11 C12' C1' 122.9(16) . . ? C11 C12' C13' 123(2) . . ? C13' C12' C1' 114(2) . . ? C14 C13' H13' 118.3 . . ? C12' C13' C14 123(3) . . ? C12' C13' H13' 118.3 . . ? C21 C22' C2' 120.7(13) . . ? C21 C22' C23' 121.2(14) . . ? C23' C22' C2' 117.8(15) . . ? C24 C23' C22' 124.1(14) . . ? C24 C23' H23' 117.9 . . ? C22' C23' H23' 117.9 . . ? C3' C32' C31 130.3(12) . . ? C33' C32' C31 116.6(16) . . ? C33' C32' C3' 113.1(17) . . ? C34 C33' H33' 119 . . ? C32' C33' C34 122(2) . . ? C32' C33' H33' 119 . . ? O5 C5 H5A 110.8 . . ? O5 C5 H5B 110.8 . . ? O5 C5 C8 105.0(4) . . ? H5A C5 H5B 108.8 . . ? C8 C5 H5A 110.8 . . ? C8 C5 H5B 110.8 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6A 111.7 . . ? C7 C6 H6B 111.7 . . ? C7 C6 C8 100.3(5) . . ? C8 C6 H6A 111.7 . . ? C8 C6 H6B 111.7 . . ? O5 C7 C6 112.2(5) . . ? O5 C7 H7A 109.2 . . ? O5 C7 H7B 109.2 . . ? O5 C7 C19 93.1(12) . . ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C19 C7 H7A 116.6 . . ? C19 C7 H7B 119.5 . . ? C5 C8 C6 102.9(4) . . ? C5 C8 H8A 111.2 . . ? C5 C8 H8B 111.2 . . ? C6 C8 H8A 111.2 . . ? C6 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? C101 C29 H29A 111.4 . . ? C101 C29 H29B 111.4 . . ? C101 C29 C39 102(4) . . ? H29A C29 H29B 109.3 . . ? C39 C29 H29A 111.4 . . ? C39 C29 H29B 111.4 . . ? C101 C290 H29C 109.1 . . ? C101 C290 H29D 109.1 . . ? H29C C290 H29D 107.8 . . ? C390 C290 C101 112(5) . . ? C390 C290 H29C 109.1 . . ? C390 C290 H29D 109.1 . . ? O4 C30 H30A 110.7 . . ? O4 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? C39 C30 O4 105(3) . . ? C39 C30 H30A 110.7 . . ? C39 C30 H30B 110.7 . . ? O4 C300 H30C 112.5 . . ? O4 C300 H30D 112.5 . . ? O4 C300 C390 96.3(13) . . ? H30C C300 H30D 110 . . ? C390 C300 H30C 112.5 . . ? C390 C300 H30D 112.5 . . ? C29 C39 H39A 109.5 . . ? C29 C39 H39B 109.5 . . ? C30 C39 C29 111(4) . . ? C30 C39 H39A 109.5 . . ? C30 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? C290 C390 C300 106(3) . . ? C290 C390 H39C 110.6 . . ? C290 C390 H39D 110.6 . . ? C300 C390 H39C 110.6 . . ? C300 C390 H39D 110.6 . . ? H39C C390 H39D 108.7 . . ? H9A C9 H9B 107.8 . . ? C10 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C19 C9 H9A 109.1 . . ? C19 C9 H9B 109.1 . . ? C19 C9 C10 113(2) . . ? O5 C10 H10E 113.3 . . ? O5 C10 H10F 113.3 . . ? C9 C10 O5 91.9(18) . . ? C9 C10 H10E 113.3 . . ? C9 C10 H10F 113.3 . . ? H10E C10 H10F 110.6 . . ? C7 C19 H19A 109.7 . . ? C7 C19 H19B 109.7 . . ? C9 C19 C7 109.8(16) . . ? C9 C19 H19A 109.7 . . ? C9 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _database_code_depnum_ccdc_archive 'CCDC 916821' ####################################################################### # # 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_Compound_4_h08mgd04 #TrackingRef '16352_web_deposit_cif_file_0_DanielGarcia-Vivo_1356029066.LiCage_final.cif' _audit_creation_date 2008-05-29T14:37:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C70 H100 N2 Na6 O10' _chemical_formula_weight 1267.47 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 20.0070(2) _cell_length_b 21.3360(3) _cell_length_c 32.6610(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13942.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_number 102918 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 22.54 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 9025 _reflns_number_gt 7060 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0949P)^2^+22.1407P] 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 9025 _refine_ls_number_parameters 813 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.066 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # 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' Na Na 0.0362 0.0249 '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 Na1 Na 0.69767(6) 0.22953(6) 0.40364(4) 0.0293(3) Uani 1 1 d . . . O1 O 0.70579(11) 0.34017(10) 0.41131(7) 0.0303(6) Uani 1 1 d . . . N1 N 0.77656(13) 0.23480(12) 0.45548(8) 0.0261(6) Uani 1 1 d . . . C1 C 0.77298(18) 0.28788(16) 0.48382(10) 0.0310(8) Uani 1 1 d . . . H1A H 0.806 0.2807 0.5059 0.037 Uiso 1 1 calc R . . H1B H 0.7282 0.2877 0.4967 0.037 Uiso 1 1 calc R . . Na2 Na 0.79321(6) 0.32954(6) 0.35874(4) 0.0332(3) Uani 1 1 d . . . O2 O 0.62042(11) 0.22252(11) 0.45483(7) 0.0335(6) Uani 1 1 d . . . N2 N 0.55055(14) 0.33025(12) 0.30698(8) 0.0279(7) Uani 1 1 d . . . C2 C 0.75803(17) 0.17563(16) 0.47632(10) 0.0317(8) Uani 1 1 d . . . H2A H 0.7967 0.1619 0.493 0.038 Uiso 1 1 calc R . . H2B H 0.7506 0.1433 0.4551 0.038 Uiso 1 1 calc R . . Na3 Na 0.53685(6) 0.23581(6) 0.40756(4) 0.0349(4) Uani 1 1 d . . . O3 O 0.78393(11) 0.22356(10) 0.35636(7) 0.0299(6) Uani 1 1 d . . . C3 C 0.84420(16) 0.23048(16) 0.43794(10) 0.0289(8) Uani 1 1 d . . . H3A H 0.8763 0.2252 0.4607 0.035 Uiso 1 1 calc R . . H3B H 0.8546 0.2709 0.4244 0.035 Uiso 1 1 calc R . . Na4 Na 0.63148(6) 0.33915(6) 0.35864(4) 0.0300(3) Uani 1 1 d . . . O4 O 0.61665(11) 0.22812(10) 0.35607(7) 0.0305(6) Uani 1 1 d . . . C4 C 0.50373(16) 0.27744(16) 0.30939(11) 0.0296(8) Uani 1 1 d . . . H4A H 0.4691 0.2834 0.2881 0.036 Uiso 1 1 calc R . . H4B H 0.481 0.2792 0.3363 0.036 Uiso 1 1 calc R . . Na5 Na 0.61436(7) 0.33327(6) 0.45583(4) 0.0347(3) Uani 1 1 d . . . O5 O 0.54083(11) 0.34495(11) 0.40061(7) 0.0316(6) Uani 1 1 d . . . C5 C 0.51606(18) 0.39056(16) 0.31391(10) 0.0325(8) Uani 1 1 d . . . H5A H 0.49 0.4005 0.289 0.039 Uiso 1 1 calc R . . H5B H 0.5506 0.4235 0.3168 0.039 Uiso 1 1 calc R . . O6 O 0.71344(11) 0.34050(11) 0.30802(7) 0.0314(6) Uani 1 1 d . . . C6 C 0.58418(17) 0.33059(17) 0.26672(10) 0.0313(8) Uani 1 1 d . . . H6A H 0.5495 0.3331 0.2452 0.038 Uiso 1 1 calc R . . H6B H 0.6077 0.2901 0.2633 0.038 Uiso 1 1 calc R . . O7 O 0.62612(15) 0.37347(12) 0.52196(8) 0.0490(7) Uani 1 1 d . . . Na8 Na 0.70991(6) 0.23510(6) 0.30397(4) 0.0337(3) Uani 1 1 d . . . O8 O 0.91066(12) 0.33190(12) 0.34767(8) 0.0455(7) Uani 1 1 d . . . O9 O 0.44230(15) 0.16917(16) 0.40432(9) 0.0647(9) Uani 1 1 d . . . O10 O 0.71648(16) 0.22449(14) 0.23252(8) 0.0584(8) Uani 1 1 d . . . C11 C 0.74797(16) 0.37647(15) 0.43269(10) 0.0286(8) Uani 1 1 d . . . C12 C 0.78500(17) 0.35242(16) 0.46640(10) 0.0308(8) Uani 1 1 d . . . C13 C 0.82794(18) 0.39306(17) 0.48763(11) 0.0380(9) Uani 1 1 d . . . H13 H 0.8539 0.3765 0.5095 0.046 Uiso 1 1 calc R . . C14 C 0.83433(19) 0.45602(18) 0.47828(12) 0.0427(10) Uani 1 1 d . . . C15 C 0.79740(19) 0.47850(18) 0.44578(12) 0.0409(9) Uani 1 1 d . . . H15 H 0.8006 0.5217 0.4389 0.049 Uiso 1 1 calc R . . C16 C 0.75550(17) 0.44015(16) 0.42263(11) 0.0339(8) Uani 1 1 d . . . C17 C 0.8793(3) 0.4989(2) 0.50326(17) 0.0697(14) Uani 1 1 d . . . H17A H 0.8708 0.4923 0.5325 0.104 Uiso 1 1 calc R . . H17B H 0.8699 0.5427 0.4962 0.104 Uiso 1 1 calc R . . H17C H 0.9262 0.4894 0.4972 0.104 Uiso 1 1 calc R . . C18 C 0.71344(19) 0.46752(18) 0.38848(12) 0.0405(9) Uani 1 1 d . . . H18A H 0.7228 0.5124 0.3859 0.061 Uiso 1 1 calc R . . H18B H 0.666 0.4614 0.3947 0.061 Uiso 1 1 calc R . . H18C H 0.7243 0.4464 0.3627 0.061 Uiso 1 1 calc R . . C21 C 0.63218(17) 0.19674(16) 0.49142(10) 0.0311(8) Uani 1 1 d . . . C22 C 0.69680(17) 0.17719(16) 0.50396(11) 0.0322(8) Uani 1 1 d . . . C23 C 0.70593(19) 0.15546(18) 0.54383(12) 0.0408(10) Uani 1 1 d . . . H23 H 0.7497 0.1436 0.552 0.049 Uiso 1 1 calc R . . C24 C 0.6546(2) 0.1502(2) 0.57213(12) 0.0484(11) Uani 1 1 d . . . C25 C 0.5912(2) 0.16712(19) 0.55858(12) 0.0470(11) Uani 1 1 d . . . H25 H 0.5546 0.1631 0.5769 0.056 Uiso 1 1 calc R . . C26 C 0.57926(18) 0.18957(18) 0.51957(11) 0.0386(9) Uani 1 1 d . . . C27 C 0.6660(3) 0.1278(3) 0.61555(14) 0.0813(18) Uani 1 1 d . . . H27A H 0.6402 0.1539 0.6345 0.122 Uiso 1 1 calc R . . H27B H 0.7136 0.1309 0.6222 0.122 Uiso 1 1 calc R . . H27C H 0.6515 0.0841 0.618 0.122 Uiso 1 1 calc R . . C28 C 0.5097(2) 0.2116(2) 0.50865(13) 0.0563(12) Uani 1 1 d . . . H28A H 0.4783 0.1984 0.53 0.084 Uiso 1 1 calc R . . H28B H 0.4964 0.1933 0.4824 0.084 Uiso 1 1 calc R . . H28C H 0.5094 0.2574 0.5065 0.084 Uiso 1 1 calc R . . C31 C 0.82660(16) 0.17891(16) 0.36791(10) 0.0277(8) Uani 1 1 d . . . C32 C 0.85613(16) 0.17860(16) 0.40742(10) 0.0269(8) Uani 1 1 d . . . C33 C 0.90216(16) 0.13177(16) 0.41752(11) 0.0319(8) Uani 1 1 d . . . H33 H 0.9221 0.1326 0.4439 0.038 Uiso 1 1 calc R . . C34 C 0.91998(17) 0.08402(16) 0.39060(11) 0.0334(9) Uani 1 1 d . . . C35 C 0.89007(17) 0.08428(16) 0.35258(11) 0.0330(9) Uani 1 1 d . . . H35 H 0.9013 0.052 0.3338 0.04 Uiso 1 1 calc R . . C36 C 0.84422(17) 0.12976(16) 0.34043(10) 0.0309(8) Uani 1 1 d . . . C37 C 0.81564(19) 0.12843(18) 0.29808(11) 0.0402(9) Uani 1 1 d . . . H37A H 0.8343 0.0927 0.283 0.06 Uiso 1 1 calc R . . H37B H 0.827 0.1674 0.2839 0.06 Uiso 1 1 calc R . . H37C H 0.7669 0.1242 0.2996 0.06 Uiso 1 1 calc R . . C38 C 0.97057(19) 0.03428(18) 0.40253(13) 0.0441(10) Uani 1 1 d . . . H38A H 0.9884 0.0437 0.4298 0.066 Uiso 1 1 calc R . . H38B H 1.0071 0.0339 0.3826 0.066 Uiso 1 1 calc R . . H38C H 0.9488 -0.0069 0.4029 0.066 Uiso 1 1 calc R . . C41 C 0.58597(16) 0.19053(16) 0.32941(10) 0.0295(8) Uani 1 1 d . . . C42 C 0.53304(16) 0.21257(16) 0.30427(10) 0.0285(8) Uani 1 1 d . . . C43 C 0.50466(17) 0.17182(17) 0.27583(10) 0.0331(9) Uani 1 1 d . . . H43 H 0.4697 0.187 0.2588 0.04 Uiso 1 1 calc R . . C44 C 0.52501(18) 0.10997(17) 0.27115(11) 0.0363(9) Uani 1 1 d . . . C45 C 0.57474(18) 0.08875(17) 0.29729(11) 0.0368(9) Uani 1 1 d . . . H45 H 0.5884 0.0462 0.2954 0.044 Uiso 1 1 calc R . . C46 C 0.60553(17) 0.12698(17) 0.32611(11) 0.0332(9) Uani 1 1 d . . . C47 C 0.4958(2) 0.06820(19) 0.23818(12) 0.0480(10) Uani 1 1 d . . . H47A H 0.4476 0.0754 0.2362 0.072 Uiso 1 1 calc R . . H47B H 0.5042 0.0242 0.2451 0.072 Uiso 1 1 calc R . . H47C H 0.5169 0.078 0.2118 0.072 Uiso 1 1 calc R . . C48 C 0.65654(19) 0.10122(17) 0.35534(12) 0.0407(9) Uani 1 1 d . . . H48A H 0.6668 0.0578 0.348 0.061 Uiso 1 1 calc R . . H48B H 0.6387 0.1026 0.3833 0.061 Uiso 1 1 calc R . . H48C H 0.6974 0.1265 0.3538 0.061 Uiso 1 1 calc R . . C51 C 0.48513(17) 0.37595(15) 0.39080(10) 0.0286(8) Uani 1 1 d . . . C52 C 0.46944(16) 0.39555(15) 0.35019(10) 0.0287(8) Uani 1 1 d . . . C53 C 0.41027(18) 0.42844(16) 0.34337(11) 0.0342(9) Uani 1 1 d . . . H53 H 0.4005 0.4414 0.3162 0.041 Uiso 1 1 calc R . . C54 C 0.36498(17) 0.44327(17) 0.37383(11) 0.0346(9) Uani 1 1 d . . . C55 C 0.37961(17) 0.42269(16) 0.41293(11) 0.0341(9) Uani 1 1 d . . . H55 H 0.349 0.4313 0.4344 0.041 Uiso 1 1 calc R . . C56 C 0.43777(17) 0.38973(16) 0.42174(10) 0.0309(8) Uani 1 1 d . . . C57 C 0.30294(19) 0.4820(2) 0.36472(13) 0.0493(10) Uani 1 1 d . . . H57A H 0.316 0.5253 0.3588 0.074 Uiso 1 1 calc R . . H57B H 0.2732 0.4814 0.3885 0.074 Uiso 1 1 calc R . . H57C H 0.2797 0.4643 0.341 0.074 Uiso 1 1 calc R . . C58 C 0.4506(2) 0.3680(2) 0.46493(11) 0.0450(10) Uani 1 1 d . . . H58A H 0.4134 0.3809 0.4825 0.067 Uiso 1 1 calc R . . H58B H 0.4922 0.3867 0.475 0.067 Uiso 1 1 calc R . . H58C H 0.4546 0.3222 0.4653 0.067 Uiso 1 1 calc R . . C61 C 0.69712(17) 0.38366(16) 0.28005(10) 0.0299(8) Uani 1 1 d . . . C62 C 0.63369(17) 0.38276(16) 0.25984(10) 0.0311(8) Uani 1 1 d . . . C63 C 0.61867(18) 0.42901(17) 0.23137(10) 0.0338(9) Uani 1 1 d . . . H63 H 0.5763 0.4277 0.2182 0.041 Uiso 1 1 calc R . . C64 C 0.66233(19) 0.47709(18) 0.22109(11) 0.0380(9) Uani 1 1 d . . . C65 C 0.72403(19) 0.47635(17) 0.24031(11) 0.0386(9) Uani 1 1 d . . . H65 H 0.7553 0.5083 0.2337 0.046 Uiso 1 1 calc R . . C66 C 0.74234(18) 0.43121(17) 0.26877(10) 0.0338(8) Uani 1 1 d . . . C67 C 0.6441(2) 0.52696(19) 0.19026(12) 0.0477(10) Uani 1 1 d . . . H67A H 0.6417 0.5677 0.204 0.072 Uiso 1 1 calc R . . H67B H 0.6007 0.517 0.178 0.072 Uiso 1 1 calc R . . H67C H 0.6783 0.5285 0.1688 0.072 Uiso 1 1 calc R . . C68 C 0.81182(19) 0.43123(19) 0.28686(12) 0.0437(10) Uani 1 1 d . . . H68A H 0.8397 0.4617 0.2722 0.066 Uiso 1 1 calc R . . H68B H 0.8314 0.3893 0.2842 0.066 Uiso 1 1 calc R . . H68C H 0.8094 0.4427 0.3159 0.066 Uiso 1 1 calc R . . C71 C 0.6477(2) 0.4364(2) 0.52611(13) 0.0554(11) Uani 1 1 d . . . H71A H 0.6971 0.4382 0.5254 0.067 Uiso 1 1 calc R . . H71B H 0.6325 0.4534 0.5527 0.067 Uiso 1 1 calc R . . C72 C 0.6199(3) 0.4747(2) 0.49230(13) 0.0608(12) Uani 1 1 d . . . H72A H 0.6307 0.4549 0.466 0.091 Uiso 1 1 calc R . . H72B H 0.6394 0.5168 0.4932 0.091 Uiso 1 1 calc R . . H72C H 0.5712 0.4776 0.4953 0.091 Uiso 1 1 calc R . . C73 C 0.6491(4) 0.3355(3) 0.5598(2) 0.114(3) Uani 1 1 d . . . H73A H 0.656 0.2909 0.5526 0.137 Uiso 1 1 calc R . . H73B H 0.6911 0.3527 0.5712 0.137 Uiso 1 1 calc R . . C74 C 0.6005(4) 0.3418(4) 0.5852(4) 0.155(4) Uani 1 1 d . . . H74A H 0.5998 0.3849 0.5956 0.232 Uiso 1 1 calc R . . H74B H 0.6067 0.3128 0.6082 0.232 Uiso 1 1 calc R . . H74C H 0.5582 0.3326 0.5714 0.232 Uiso 1 1 calc R . . C81 C 0.9323(2) 0.2824(2) 0.32029(13) 0.0488(11) Uani 1 1 d . . . H81A H 0.9476 0.3013 0.2942 0.059 Uiso 1 1 calc R . . H81B H 0.8939 0.2547 0.3141 0.059 Uiso 1 1 calc R . . C82 C 0.9882(2) 0.2438(2) 0.33824(15) 0.0624(12) Uani 1 1 d . . . H82A H 1.0287 0.2695 0.3403 0.094 Uiso 1 1 calc R . . H82B H 0.997 0.2077 0.3205 0.094 Uiso 1 1 calc R . . H82C H 0.9753 0.2291 0.3655 0.094 Uiso 1 1 calc R . . C83 C 0.9558(2) 0.3833(2) 0.34731(15) 0.0616(12) Uani 1 1 d . . . H83A H 0.9534 0.4054 0.3207 0.074 Uiso 1 1 calc R . . H83B H 1.0022 0.3682 0.3513 0.074 Uiso 1 1 calc R . . C84 C 0.9370(3) 0.4263(3) 0.38088(19) 0.0877(18) Uani 1 1 d . . . H84A H 0.8928 0.4442 0.3753 0.132 Uiso 1 1 calc R . . H84B H 0.97 0.4602 0.3828 0.132 Uiso 1 1 calc R . . H84C H 0.9358 0.4032 0.4068 0.132 Uiso 1 1 calc R . . C91 C 0.4644(3) 0.1024(2) 0.39884(17) 0.0782(16) Uani 1 1 d . . . H91A H 0.484 0.0966 0.3713 0.094 Uiso 1 1 calc R . . H91B H 0.4257 0.0738 0.4016 0.094 Uiso 1 1 calc R . . C92 C 0.5158(3) 0.0880(3) 0.4312(2) 0.097(2) Uani 1 1 d . . . H92A H 0.554 0.1164 0.4281 0.145 Uiso 1 1 calc R . . H92B H 0.5309 0.0445 0.4281 0.145 Uiso 1 1 calc R . . H92C H 0.4959 0.0936 0.4583 0.145 Uiso 1 1 calc R . . C93 C 0.3822(3) 0.1817(3) 0.38445(18) 0.0872(18) Uani 1 1 d . . . H93A H 0.3484 0.15 0.3923 0.105 Uiso 1 1 calc R . . H93B H 0.3887 0.1795 0.3544 0.105 Uiso 1 1 calc R . . C94 C 0.3590(3) 0.2446(3) 0.39615(17) 0.0772(15) Uani 1 1 d . . . H94A H 0.36 0.2487 0.426 0.116 Uiso 1 1 calc R . . H94B H 0.3132 0.2509 0.3863 0.116 Uiso 1 1 calc R . . H94C H 0.3884 0.2763 0.3839 0.116 Uiso 1 1 calc R . . C101 C 0.7437(4) 0.2630(4) 0.2034(2) 0.127(3) Uani 1 1 d . . . H10A H 0.7138 0.2992 0.1982 0.153 Uiso 1 1 calc R . . H10B H 0.7501 0.24 0.1774 0.153 Uiso 1 1 calc R . . C102 C 0.8045(3) 0.2833(3) 0.21859(18) 0.0873(18) Uani 1 1 d . . . H10C H 0.7991 0.2968 0.2471 0.131 Uiso 1 1 calc R . . H10D H 0.8206 0.3186 0.2021 0.131 Uiso 1 1 calc R . . H10E H 0.837 0.249 0.2173 0.131 Uiso 1 1 calc R . . C103 C 0.6564(3) 0.1869(3) 0.21500(17) 0.0818(16) Uani 1 1 d . . . H10F H 0.6244 0.1781 0.2374 0.098 Uiso 1 1 calc R . . H10G H 0.6331 0.213 0.1944 0.098 Uiso 1 1 calc R . . C104 C 0.6742(4) 0.1328(3) 0.1977(3) 0.118(2) Uani 1 1 d . . . H10H H 0.7121 0.1399 0.1793 0.178 Uiso 1 1 calc R . . H10I H 0.6365 0.1158 0.1821 0.178 Uiso 1 1 calc R . . H10J H 0.6872 0.1028 0.219 0.178 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 Na1 0.0261(7) 0.0334(8) 0.0284(7) 0.0006(6) -0.0018(5) -0.0002(6) O1 0.0294(13) 0.0291(13) 0.0323(13) 0.0008(10) -0.0043(10) 0.0003(11) N1 0.0262(15) 0.0250(15) 0.0271(15) -0.0004(12) -0.0004(12) 0.0010(12) C1 0.032(2) 0.033(2) 0.0286(19) -0.0027(15) -0.0031(15) 0.0041(16) Na2 0.0286(7) 0.0369(8) 0.0342(8) 0.0017(6) -0.0008(6) 0.0002(6) O2 0.0292(13) 0.0395(14) 0.0318(14) 0.0070(11) -0.0014(10) 0.0023(11) N2 0.0300(16) 0.0267(16) 0.0272(16) 0.0005(12) 0.0008(12) -0.0008(13) C2 0.0301(19) 0.032(2) 0.0328(19) 0.0030(16) -0.0003(16) 0.0035(16) Na3 0.0284(7) 0.0372(8) 0.0391(8) 0.0023(6) -0.0020(6) -0.0019(6) O3 0.0259(12) 0.0338(14) 0.0299(13) 0.0009(10) -0.0007(10) 0.0039(11) C3 0.0236(18) 0.031(2) 0.0319(19) 0.0010(15) -0.0012(15) 0.0003(15) Na4 0.0264(7) 0.0337(8) 0.0300(7) 0.0003(6) -0.0023(5) 0.0000(6) O4 0.0297(13) 0.0296(13) 0.0321(14) -0.0022(10) -0.0056(10) 0.0008(10) C4 0.0237(18) 0.034(2) 0.0313(19) -0.0001(15) -0.0045(15) -0.0020(15) Na5 0.0351(8) 0.0382(8) 0.0308(8) -0.0012(6) -0.0010(6) 0.0029(6) O5 0.0286(13) 0.0342(14) 0.0321(13) 0.0014(10) -0.0023(10) 0.0060(11) C5 0.035(2) 0.031(2) 0.031(2) 0.0036(15) -0.0003(16) 0.0040(16) O6 0.0284(13) 0.0349(14) 0.0308(13) 0.0066(11) -0.0018(10) -0.0002(10) C6 0.0278(19) 0.038(2) 0.0284(19) -0.0012(15) -0.0038(15) 0.0008(16) O7 0.076(2) 0.0400(17) 0.0306(15) 0.0026(12) -0.0037(13) 0.0020(14) Na8 0.0327(8) 0.0375(8) 0.0309(8) -0.0004(6) -0.0027(6) 0.0013(6) O8 0.0325(15) 0.0491(16) 0.0550(17) 0.0027(13) 0.0032(12) -0.0067(13) O9 0.0485(19) 0.082(2) 0.063(2) -0.0216(17) 0.0060(16) -0.0226(17) O10 0.079(2) 0.062(2) 0.0346(16) 0.0033(14) 0.0074(15) 0.0076(16) C11 0.0251(18) 0.032(2) 0.0290(19) -0.0039(16) 0.0027(15) 0.0003(15) C12 0.0294(19) 0.031(2) 0.032(2) -0.0010(16) -0.0009(16) 0.0028(16) C13 0.035(2) 0.038(2) 0.041(2) -0.0034(17) -0.0085(17) 0.0049(17) C14 0.039(2) 0.036(2) 0.053(3) -0.0062(19) -0.0099(19) -0.0025(18) C15 0.041(2) 0.028(2) 0.054(3) 0.0004(18) -0.0014(19) -0.0025(17) C16 0.031(2) 0.031(2) 0.039(2) 0.0037(17) 0.0026(17) 0.0015(16) C17 0.073(3) 0.048(3) 0.088(4) -0.006(3) -0.030(3) -0.014(2) C18 0.044(2) 0.034(2) 0.044(2) 0.0091(17) 0.0004(18) 0.0013(18) C21 0.032(2) 0.0270(19) 0.034(2) 0.0032(16) 0.0018(16) 0.0014(16) C22 0.033(2) 0.0287(19) 0.035(2) 0.0029(16) 0.0019(16) 0.0040(16) C23 0.038(2) 0.044(2) 0.040(2) 0.0077(18) -0.0014(18) 0.0105(18) C24 0.051(3) 0.055(3) 0.040(2) 0.016(2) 0.008(2) 0.014(2) C25 0.041(2) 0.056(3) 0.043(2) 0.017(2) 0.0145(19) 0.010(2) C26 0.034(2) 0.040(2) 0.041(2) 0.0092(18) 0.0059(17) 0.0084(17) C27 0.068(3) 0.130(5) 0.047(3) 0.034(3) 0.009(2) 0.032(3) C28 0.036(2) 0.080(3) 0.053(3) 0.025(2) 0.011(2) 0.011(2) C31 0.0209(17) 0.030(2) 0.032(2) 0.0035(15) 0.0020(15) -0.0012(15) C32 0.0211(17) 0.0283(19) 0.031(2) -0.0005(15) 0.0037(15) 0.0005(15) C33 0.0258(18) 0.037(2) 0.033(2) 0.0054(16) 0.0003(16) -0.0013(16) C34 0.030(2) 0.030(2) 0.040(2) 0.0029(17) 0.0075(17) 0.0044(16) C35 0.034(2) 0.030(2) 0.035(2) -0.0014(16) 0.0091(17) 0.0011(16) C36 0.0271(19) 0.033(2) 0.033(2) -0.0008(16) 0.0036(15) -0.0021(16) C37 0.042(2) 0.044(2) 0.035(2) -0.0072(17) 0.0007(17) 0.0025(18) C38 0.040(2) 0.038(2) 0.054(3) 0.0028(18) 0.0031(19) 0.0125(18) C41 0.0265(19) 0.032(2) 0.0302(19) -0.0024(16) 0.0026(16) -0.0046(16) C42 0.0252(18) 0.033(2) 0.0277(19) 0.0021(15) 0.0018(15) -0.0020(15) C43 0.0269(19) 0.040(2) 0.032(2) 0.0000(16) -0.0006(15) -0.0036(16) C44 0.032(2) 0.037(2) 0.040(2) -0.0098(17) 0.0010(17) -0.0034(17) C45 0.035(2) 0.027(2) 0.049(2) -0.0048(17) 0.0019(18) -0.0002(16) C46 0.0260(19) 0.034(2) 0.040(2) 0.0005(17) 0.0000(16) -0.0001(16) C47 0.047(2) 0.045(2) 0.052(3) -0.015(2) -0.004(2) -0.003(2) C48 0.040(2) 0.031(2) 0.052(2) -0.0018(17) -0.0059(18) 0.0025(17) C51 0.0266(19) 0.0251(19) 0.034(2) -0.0001(15) -0.0016(16) -0.0016(15) C52 0.0279(19) 0.0247(18) 0.033(2) -0.0001(15) -0.0013(15) -0.0019(15) C53 0.037(2) 0.033(2) 0.033(2) 0.0029(16) -0.0067(17) -0.0008(17) C54 0.0284(19) 0.033(2) 0.042(2) -0.0013(17) -0.0035(17) 0.0010(16) C55 0.027(2) 0.033(2) 0.043(2) -0.0029(17) 0.0056(16) 0.0001(16) C56 0.030(2) 0.0296(19) 0.033(2) 0.0004(15) -0.0008(16) -0.0015(16) C57 0.036(2) 0.055(3) 0.058(3) 0.004(2) 0.0005(19) 0.013(2) C58 0.045(2) 0.052(3) 0.038(2) 0.0033(18) 0.0063(18) 0.013(2) C61 0.033(2) 0.032(2) 0.0247(19) -0.0012(16) 0.0042(15) 0.0031(16) C62 0.033(2) 0.033(2) 0.0276(19) -0.0016(16) 0.0019(16) 0.0010(16) C63 0.033(2) 0.039(2) 0.0291(19) 0.0010(17) 0.0023(16) 0.0059(17) C64 0.041(2) 0.038(2) 0.035(2) 0.0055(17) 0.0086(18) 0.0093(18) C65 0.042(2) 0.035(2) 0.038(2) 0.0053(17) 0.0104(18) -0.0036(17) C66 0.035(2) 0.034(2) 0.033(2) 0.0001(16) 0.0027(16) -0.0033(17) C67 0.050(2) 0.045(2) 0.048(2) 0.0143(19) 0.009(2) 0.008(2) C68 0.039(2) 0.047(2) 0.045(2) 0.0060(19) -0.0003(18) -0.0100(19) C71 0.067(3) 0.046(3) 0.053(3) -0.007(2) -0.004(2) 0.005(2) C72 0.081(3) 0.053(3) 0.048(3) -0.001(2) 0.010(2) 0.012(2) C73 0.135(6) 0.067(4) 0.140(6) -0.048(4) 0.072(5) -0.026(4) C74 0.092(5) 0.085(5) 0.288(13) 0.001(6) 0.016(7) 0.013(4) C81 0.039(2) 0.059(3) 0.049(3) -0.004(2) 0.0088(19) -0.005(2) C82 0.049(3) 0.061(3) 0.078(3) -0.001(3) 0.011(2) 0.005(2) C83 0.046(3) 0.061(3) 0.078(3) -0.006(3) -0.003(2) -0.006(2) C84 0.070(4) 0.086(4) 0.108(5) -0.039(3) -0.013(3) 0.004(3) C91 0.081(4) 0.066(4) 0.088(4) -0.026(3) 0.025(3) -0.031(3) C92 0.090(4) 0.060(4) 0.141(6) -0.010(4) 0.010(4) -0.001(3) C93 0.080(4) 0.110(5) 0.072(4) -0.003(3) -0.010(3) -0.032(4) C94 0.077(4) 0.078(4) 0.076(4) 0.009(3) -0.021(3) -0.011(3) C101 0.099(5) 0.203(9) 0.079(4) 0.012(5) 0.012(4) -0.044(6) C102 0.062(3) 0.116(5) 0.084(4) -0.035(4) 0.007(3) -0.006(3) C103 0.066(3) 0.113(5) 0.066(3) -0.012(3) -0.006(3) -0.004(3) C104 0.124(6) 0.081(5) 0.150(7) 0.009(5) -0.017(5) 0.007(4) #----------------------------------------------------------------------------# # 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 Na1 O4 2.246(2) . ? Na1 O2 2.282(3) . ? Na1 N1 2.317(3) . ? Na1 O3 2.319(2) . ? Na1 O1 2.379(3) . ? O1 C11 1.342(4) . ? O1 Na4 2.274(2) . ? O1 Na5 2.341(3) . ? O1 Na2 2.461(3) . ? N1 C1 1.464(4) . ? N1 C3 1.472(4) . ? N1 C2 1.481(4) . ? C1 C12 1.509(5) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? Na2 O3 2.270(3) . ? Na2 O6 2.312(3) . ? Na2 O8 2.378(3) . ? O2 C21 1.336(4) . ? O2 Na3 2.293(3) . ? O2 Na5 2.366(3) . ? N2 C4 1.468(4) . ? N2 C6 1.477(4) . ? N2 C5 1.477(4) . ? N2 Na4 2.346(3) . ? C2 C22 1.522(5) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? Na3 O4 2.325(3) . ? Na3 O5 2.341(3) . ? Na3 O9 2.369(3) . ? O3 C31 1.334(4) . ? O3 Na8 2.276(2) . ? C3 C32 1.508(5) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? Na4 O5 2.277(3) . ? Na4 O6 2.329(3) . ? Na4 O4 2.389(3) . ? O4 C41 1.333(4) . ? O4 Na8 2.530(3) . ? C4 C42 1.513(5) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? Na5 O7 2.336(3) . ? Na5 O5 2.341(3) . ? O5 C51 1.335(4) . ? C5 C52 1.512(5) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? O6 C61 1.337(4) . ? O6 Na8 2.254(3) . ? C6 C62 1.507(5) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O7 C71 1.417(5) . ? O7 C73 1.547(9) . ? Na8 O10 2.348(3) . ? O8 C83 1.421(5) . ? O8 C81 1.449(5) . ? O9 C93 1.391(6) . ? O9 C91 1.502(6) . ? O10 C101 1.369(7) . ? O10 C103 1.555(6) . ? C11 C16 1.406(5) . ? C11 C12 1.423(5) . ? C12 C13 1.404(5) . ? C13 C14 1.384(5) . ? C13 H13 0.95 . ? C14 C15 1.379(5) . ? C14 C17 1.521(6) . ? C15 C16 1.394(5) . ? C15 H15 0.95 . ? C16 C18 1.514(5) . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C21 C26 1.411(5) . ? C21 C22 1.419(5) . ? C22 C23 1.394(5) . ? C23 C24 1.386(5) . ? C23 H23 0.95 . ? C24 C25 1.391(6) . ? C24 C27 1.514(6) . ? C25 C26 1.382(5) . ? C25 H25 0.95 . ? C26 C28 1.511(5) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C31 C32 1.420(5) . ? C31 C36 1.425(5) . ? C32 C33 1.398(5) . ? C33 C34 1.392(5) . ? C33 H33 0.95 . ? C34 C35 1.378(5) . ? C34 C38 1.517(5) . ? C35 C36 1.393(5) . ? C35 H35 0.95 . ? C36 C37 1.497(5) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C41 C46 1.415(5) . ? C41 C42 1.420(5) . ? C42 C43 1.393(5) . ? C43 C44 1.389(5) . ? C43 H43 0.95 . ? C44 C45 1.387(5) . ? C44 C47 1.515(5) . ? C45 C46 1.390(5) . ? C45 H45 0.95 . ? C46 C48 1.502(5) . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C51 C56 1.416(5) . ? C51 C52 1.426(5) . ? C52 C53 1.394(5) . ? C53 C54 1.382(5) . ? C53 H53 0.95 . ? C54 C55 1.382(5) . ? C54 C57 1.520(5) . ? C55 C56 1.390(5) . ? C55 H55 0.95 . ? C56 C58 1.507(5) . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? C58 H58A 0.98 . ? C58 H58B 0.98 . ? C58 H58C 0.98 . ? C61 C66 1.408(5) . ? C61 C62 1.431(5) . ? C62 C63 1.389(5) . ? C63 C64 1.389(5) . ? C63 H63 0.95 . ? C64 C65 1.385(5) . ? C64 C67 1.509(5) . ? C65 C66 1.388(5) . ? C65 H65 0.95 . ? C66 C68 1.510(5) . ? C67 H67A 0.98 . ? C67 H67B 0.98 . ? C67 H67C 0.98 . ? C68 H68A 0.98 . ? C68 H68B 0.98 . ? C68 H68C 0.98 . ? C71 C72 1.481(6) . ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? C73 C74 1.286(10) . ? C73 H73A 0.99 . ? C73 H73B 0.99 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? C81 C82 1.508(6) . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? C83 C84 1.479(7) . ? C83 H83A 0.99 . ? C83 H83B 0.99 . ? C84 H84A 0.98 . ? C84 H84B 0.98 . ? C84 H84C 0.98 . ? C91 C92 1.505(8) . ? C91 H91A 0.99 . ? C91 H91B 0.99 . ? C92 H92A 0.98 . ? C92 H92B 0.98 . ? C92 H92C 0.98 . ? C93 C94 1.472(8) . ? C93 H93A 0.99 . ? C93 H93B 0.99 . ? C94 H94A 0.98 . ? C94 H94B 0.98 . ? C94 H94C 0.98 . ? C101 C102 1.384(8) . ? C101 H10A 0.99 . ? C101 H10B 0.99 . ? C102 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? C103 C104 1.334(8) . ? C103 H10F 0.99 . ? C103 H10G 0.99 . ? C104 H10H 0.98 . ? C104 H10I 0.98 . ? C104 H10J 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 O4 Na1 O2 90.99(9) . . ? O4 Na1 N1 176.21(10) . . ? O2 Na1 N1 85.94(9) . . ? O4 Na1 O3 94.34(9) . . ? O2 Na1 O3 171.22(10) . . ? N1 Na1 O3 88.99(9) . . ? O4 Na1 O1 97.78(9) . . ? O2 Na1 O1 91.96(9) . . ? N1 Na1 O1 80.13(9) . . ? O3 Na1 O1 94.23(9) . . ? C11 O1 Na4 144.2(2) . . ? C11 O1 Na5 101.78(18) . . ? Na4 O1 Na5 87.62(9) . . ? C11 O1 Na1 132.1(2) . . ? Na4 O1 Na1 82.32(8) . . ? Na5 O1 Na1 87.12(9) . . ? C11 O1 Na2 88.25(18) . . ? Na4 O1 Na2 86.33(8) . . ? Na5 O1 Na2 169.29(11) . . ? Na1 O1 Na2 83.32(8) . . ? C1 N1 C3 109.8(3) . . ? C1 N1 C2 110.9(3) . . ? C3 N1 C2 110.8(3) . . ? C1 N1 Na1 117.8(2) . . ? C3 N1 Na1 109.80(19) . . ? C2 N1 Na1 97.12(19) . . ? N1 C1 C12 117.4(3) . . ? N1 C1 H1A 108 . . ? C12 C1 H1A 108 . . ? N1 C1 H1B 108 . . ? C12 C1 H1B 108 . . ? H1A C1 H1B 107.2 . . ? O3 Na2 O6 91.13(9) . . ? O3 Na2 O8 95.56(10) . . ? O6 Na2 O8 124.82(10) . . ? O3 Na2 O1 93.29(9) . . ? O6 Na2 O1 89.99(9) . . ? O8 Na2 O1 143.73(10) . . ? C21 O2 Na1 124.3(2) . . ? C21 O2 Na3 141.4(2) . . ? Na1 O2 Na3 89.57(9) . . ? C21 O2 Na5 114.1(2) . . ? Na1 O2 Na5 88.82(9) . . ? Na3 O2 Na5 81.29(9) . . ? C4 N2 C6 110.0(3) . . ? C4 N2 C5 111.2(3) . . ? C6 N2 C5 110.2(3) . . ? C4 N2 Na4 117.6(2) . . ? C6 N2 Na4 108.99(19) . . ? C5 N2 Na4 98.15(19) . . ? N1 C2 C22 117.1(3) . . ? N1 C2 H2A 108 . . ? C22 C2 H2A 108 . . ? N1 C2 H2B 108 . . ? C22 C2 H2B 108 . . ? H2A C2 H2B 107.3 . . ? O2 Na3 O4 88.72(9) . . ? O2 Na3 O5 99.41(9) . . ? O4 Na3 O5 88.66(9) . . ? O2 Na3 O9 122.56(12) . . ? O4 Na3 O9 118.28(11) . . ? O5 Na3 O9 128.31(12) . . ? C31 O3 Na2 130.5(2) . . ? C31 O3 Na8 134.9(2) . . ? Na2 O3 Na8 88.35(9) . . ? C31 O3 Na1 109.11(19) . . ? Na2 O3 Na1 89.05(9) . . ? Na8 O3 Na1 90.61(9) . . ? N1 C3 C32 116.6(3) . . ? N1 C3 H3A 108.1 . . ? C32 C3 H3A 108.1 . . ? N1 C3 H3B 108.1 . . ? C32 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? O1 Na4 O5 93.72(9) . . ? O1 Na4 O6 94.40(9) . . ? O5 Na4 O6 170.99(10) . . ? O1 Na4 N2 174.94(10) . . ? O5 Na4 N2 83.54(9) . . ? O6 Na4 N2 88.64(9) . . ? O1 Na4 O4 96.74(9) . . ? O5 Na4 O4 88.63(9) . . ? O6 Na4 O4 94.29(9) . . ? N2 Na4 O4 78.97(9) . . ? C41 O4 Na1 142.4(2) . . ? C41 O4 Na3 101.46(19) . . ? Na1 O4 Na3 89.66(9) . . ? C41 O4 Na4 132.6(2) . . ? Na1 O4 Na4 82.68(8) . . ? Na3 O4 Na4 89.42(9) . . ? C41 O4 Na8 86.31(18) . . ? Na1 O4 Na8 86.11(8) . . ? Na3 O4 Na8 171.51(11) . . ? Na4 O4 Na8 82.74(8) . . ? N2 C4 C42 116.7(3) . . ? N2 C4 H4A 108.1 . . ? C42 C4 H4A 108.1 . . ? N2 C4 H4B 108.1 . . ? C42 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? O7 Na5 O5 137.45(11) . . ? O7 Na5 O1 118.20(11) . . ? O5 Na5 O1 90.32(9) . . ? O7 Na5 O2 111.98(10) . . ? O5 Na5 O2 97.35(9) . . ? O1 Na5 O2 90.81(9) . . ? C51 O5 Na4 123.2(2) . . ? C51 O5 Na3 119.2(2) . . ? Na4 O5 Na3 91.80(9) . . ? C51 O5 Na5 139.7(2) . . ? Na4 O5 Na5 87.56(9) . . ? Na3 O5 Na5 80.83(8) . . ? N2 C5 C52 118.0(3) . . ? N2 C5 H5A 107.8 . . ? C52 C5 H5A 107.8 . . ? N2 C5 H5B 107.8 . . ? C52 C5 H5B 107.8 . . ? H5A C5 H5B 107.1 . . ? C61 O6 Na8 129.7(2) . . ? C61 O6 Na2 136.7(2) . . ? Na8 O6 Na2 87.86(9) . . ? C61 O6 Na4 108.76(19) . . ? Na8 O6 Na4 90.42(9) . . ? Na2 O6 Na4 88.63(9) . . ? N2 C6 C62 115.8(3) . . ? N2 C6 H6A 108.3 . . ? C62 C6 H6A 108.3 . . ? N2 C6 H6B 108.3 . . ? C62 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C71 O7 C73 109.3(3) . . ? C71 O7 Na5 117.9(2) . . ? C73 O7 Na5 125.1(3) . . ? O6 Na8 O3 92.49(9) . . ? O6 Na8 O10 98.79(11) . . ? O3 Na8 O10 134.44(11) . . ? O6 Na8 O4 92.42(9) . . ? O3 Na8 O4 88.15(8) . . ? O10 Na8 O4 134.75(11) . . ? C83 O8 C81 111.5(3) . . ? C83 O8 Na2 130.2(3) . . ? C81 O8 Na2 112.0(2) . . ? C93 O9 C91 112.4(4) . . ? C93 O9 Na3 126.6(3) . . ? C91 O9 Na3 109.8(3) . . ? C101 O10 C103 111.2(4) . . ? C101 O10 Na8 130.8(4) . . ? C103 O10 Na8 111.8(3) . . ? O1 C11 C16 120.2(3) . . ? O1 C11 C12 121.5(3) . . ? C16 C11 C12 118.3(3) . . ? C13 C12 C11 118.6(3) . . ? C13 C12 C1 118.4(3) . . ? C11 C12 C1 122.5(3) . . ? C14 C13 C12 123.2(3) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C15 C14 C13 117.3(3) . . ? C15 C14 C17 121.4(4) . . ? C13 C14 C17 121.3(4) . . ? C14 C15 C16 122.4(4) . . ? C14 C15 H15 118.8 . . ? C16 C15 H15 118.8 . . ? C15 C16 C11 120.3(3) . . ? C15 C16 C18 120.5(3) . . ? C11 C16 C18 119.0(3) . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C21 C26 119.7(3) . . ? O2 C21 C22 122.7(3) . . ? C26 C21 C22 117.6(3) . . ? C23 C22 C21 119.1(3) . . ? C23 C22 C2 116.2(3) . . ? C21 C22 C2 124.6(3) . . ? C24 C23 C22 123.5(3) . . ? C24 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? C23 C24 C25 116.2(3) . . ? C23 C24 C27 122.6(4) . . ? C25 C24 C27 121.2(4) . . ? C26 C25 C24 122.8(4) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C25 C26 C21 120.6(3) . . ? C25 C26 C28 119.0(3) . . ? C21 C26 C28 120.2(3) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C31 C32 121.8(3) . . ? O3 C31 C36 120.4(3) . . ? C32 C31 C36 117.8(3) . . ? C33 C32 C31 119.5(3) . . ? C33 C32 C3 118.2(3) . . ? C31 C32 C3 122.1(3) . . ? C34 C33 C32 122.9(3) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C35 C34 C33 117.1(3) . . ? C35 C34 C38 121.6(3) . . ? C33 C34 C38 121.4(3) . . ? C34 C35 C36 123.1(3) . . ? C34 C35 H35 118.5 . . ? C36 C35 H35 118.5 . . ? C35 C36 C31 119.7(3) . . ? C35 C36 C37 120.1(3) . . ? C31 C36 C37 120.1(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C41 C46 119.9(3) . . ? O4 C41 C42 121.4(3) . . ? C46 C41 C42 118.6(3) . . ? C43 C42 C41 118.9(3) . . ? C43 C42 C4 119.1(3) . . ? C41 C42 C4 121.9(3) . . ? C44 C43 C42 123.1(3) . . ? C44 C43 H43 118.4 . . ? C42 C43 H43 118.4 . . ? C45 C44 C43 116.9(3) . . ? C45 C44 C47 121.5(3) . . ? C43 C44 C47 121.6(3) . . ? C44 C45 C46 122.9(3) . . ? C44 C45 H45 118.5 . . ? C46 C45 H45 118.5 . . ? C45 C46 C41 119.4(3) . . ? C45 C46 C48 121.1(3) . . ? C41 C46 C48 119.3(3) . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O5 C51 C56 119.4(3) . . ? O5 C51 C52 123.5(3) . . ? C56 C51 C52 117.1(3) . . ? C53 C52 C51 118.9(3) . . ? C53 C52 C5 115.7(3) . . ? C51 C52 C5 124.9(3) . . ? C54 C53 C52 123.8(3) . . ? C54 C53 H53 118.1 . . ? C52 C53 H53 118.1 . . ? C53 C54 C55 117.0(3) . . ? C53 C54 C57 121.3(3) . . ? C55 C54 C57 121.8(3) . . ? C54 C55 C56 122.0(3) . . ? C54 C55 H55 119 . . ? C56 C55 H55 119 . . ? C55 C56 C51 121.2(3) . . ? C55 C56 C58 119.5(3) . . ? C51 C56 C58 119.3(3) . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O6 C61 C66 121.2(3) . . ? O6 C61 C62 121.5(3) . . ? C66 C61 C62 117.3(3) . . ? C63 C62 C61 119.4(3) . . ? C63 C62 C6 118.9(3) . . ? C61 C62 C6 121.6(3) . . ? C62 C63 C64 123.4(3) . . ? C62 C63 H63 118.3 . . ? C64 C63 H63 118.3 . . ? C65 C64 C63 116.3(3) . . ? C65 C64 C67 121.7(3) . . ? C63 C64 C67 122.0(3) . . ? C64 C65 C66 123.2(3) . . ? C64 C65 H65 118.4 . . ? C66 C65 H65 118.4 . . ? C65 C66 C61 120.4(3) . . ? C65 C66 C68 120.3(3) . . ? C61 C66 C68 119.3(3) . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O7 C71 C72 109.7(4) . . ? O7 C71 H71A 109.7 . . ? C72 C71 H71A 109.7 . . ? O7 C71 H71B 109.7 . . ? C72 C71 H71B 109.7 . . ? H71A C71 H71B 108.2 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 O7 103.7(7) . . ? C74 C73 H73A 111 . . ? O7 C73 H73A 111 . . ? C74 C73 H73B 111 . . ? O7 C73 H73B 111 . . ? H73A C73 H73B 109 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O8 C81 C82 112.3(4) . . ? O8 C81 H81A 109.1 . . ? C82 C81 H81A 109.1 . . ? O8 C81 H81B 109.1 . . ? C82 C81 H81B 109.1 . . ? H81A C81 H81B 107.9 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O8 C83 C84 108.1(4) . . ? O8 C83 H83A 110.1 . . ? C84 C83 H83A 110.1 . . ? O8 C83 H83B 110.1 . . ? C84 C83 H83B 110.1 . . ? H83A C83 H83B 108.4 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O9 C91 C92 108.2(4) . . ? O9 C91 H91A 110.1 . . ? C92 C91 H91A 110.1 . . ? O9 C91 H91B 110.1 . . ? C92 C91 H91B 110.1 . . ? H91A C91 H91B 108.4 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? O9 C93 C94 109.0(4) . . ? O9 C93 H93A 109.9 . . ? C94 C93 H93A 109.9 . . ? O9 C93 H93B 109.9 . . ? C94 C93 H93B 109.9 . . ? H93A C93 H93B 108.3 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O10 C101 C102 106.8(6) . . ? O10 C101 H10A 110.4 . . ? C102 C101 H10A 110.4 . . ? O10 C101 H10B 110.4 . . ? C102 C101 H10B 110.4 . . ? H10A C101 H10B 108.6 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C104 C103 O10 113.3(5) . . ? C104 C103 H10F 108.9 . . ? O10 C103 H10F 108.9 . . ? C104 C103 H10G 108.9 . . ? O10 C103 H10G 108.9 . . ? H10F C103 H10G 107.7 . . ? C103 C104 H10H 109.5 . . ? C103 C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? C103 C104 H10J 109.5 . . ? H10H C104 H10J 109.5 . . ? H10I C104 H10J 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 916822' ####################################################################### # # 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_Compound_5_k09mgd06 #TrackingRef '16352_web_deposit_cif_file_0_DanielGarcia-Vivo_1356029066.LiCage_final.cif' _audit_creation_date 2009-06-05T10:08:26-00:00 _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_name_common 'Compound X' _chemical_formula_moiety 'C45 H55 Cl5 Li3 N O7' _chemical_formula_sum 'C45 H55 Cl5 Li3 N O7' _chemical_formula_weight 919.97 #----------------------------------------------------------------------------# # 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 9.8010(2) _cell_length_b 13.9220(3) _cell_length_c 18.4310(3) _cell_angle_alpha 89.201(2) _cell_angle_beta 87.934(2) _cell_angle_gamma 70.5530(10) _cell_volume 2369.88(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 43098 _cell_measurement_theta_min 3.513 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour White _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.25 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0445998 _diffrn_orient_matrix_ub_12 -0.0566843 _diffrn_orient_matrix_ub_13 0.0347289 _diffrn_orient_matrix_ub_21 -0.0951418 _diffrn_orient_matrix_ub_22 0.0155418 _diffrn_orient_matrix_ub_23 0.0270475 _diffrn_orient_matrix_ub_31 -0.0260742 _diffrn_orient_matrix_ub_32 -0.0484509 _diffrn_orient_matrix_ub_33 -0.031779 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 31166 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 27.55 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 10697 _reflns_number_gt 8035 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0523P)^2^+1.7875P] 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 10697 _refine_ls_number_parameters 570 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.534 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Cl Cl 0.1484 0.1585 '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 0.28356(15) 0.31140(10) 0.83620(7) 0.0265(3) Uani 1 1 d . . . O2 O 0.29916(14) 0.30543(10) 0.67009(7) 0.0250(3) Uani 1 1 d . . . O3 O 0.05423(14) 0.24732(10) 0.75409(7) 0.0259(3) Uani 1 1 d . . . O4 O -0.02106(17) 0.32801(12) 0.59764(8) 0.0362(4) Uani 1 1 d . . . O5 O 0.04944(19) 0.27483(13) 0.93311(8) 0.0401(4) Uani 1 1 d . B . O6 O 0.05287(15) 0.44628(10) 0.75511(8) 0.0277(3) Uani 1 1 d . . . O7 O 0.35563(18) 0.50222(12) 0.74371(9) 0.0385(4) Uani 1 1 d . . . N1 N 0.34671(17) 0.12724(13) 0.75799(9) 0.0225(3) Uani 1 1 d . . . Cl1 Cl 0.05919(7) 0.55923(4) 0.62059(3) 0.04077(15) Uani 1 1 d . . . Cl2 Cl -0.18929(8) 0.77000(5) 0.61259(4) 0.05207(18) Uani 1 1 d . . . Cl3 Cl -0.42387(7) 0.83584(5) 0.73745(4) 0.05587(19) Uani 1 1 d . . . Cl4 Cl -0.40155(7) 0.69465(5) 0.87286(4) 0.05214(18) Uani 1 1 d . . . Cl5 Cl -0.14992(7) 0.48732(5) 0.88058(3) 0.04496(16) Uani 1 1 d . . . Li1 Li 0.2726(4) 0.3941(3) 0.75113(19) 0.0283(7) Uani 1 1 d . . . Li2 Li 0.0931(4) 0.3333(3) 0.68065(18) 0.0275(7) Uani 1 1 d . . . Li3 Li 0.0806(4) 0.3287(3) 0.83180(19) 0.0292(7) Uani 1 1 d . . . C1 C 0.3510(2) 0.09633(16) 0.83645(11) 0.0279(4) Uani 1 1 d . . . H1A H 0.2526 0.1109 0.8555 0.033 Uiso 1 1 calc R . . H1B H 0.3998 0.0234 0.84 0.033 Uiso 1 1 calc R . . C2 C 0.4930(2) 0.12293(15) 0.72766(11) 0.0262(4) Uani 1 1 d . . . H2A H 0.5266 0.1698 0.7545 0.031 Uiso 1 1 calc R . . H2B H 0.5609 0.0548 0.7347 0.031 Uiso 1 1 calc R . . C3 C 0.2777(2) 0.06883(15) 0.71254(12) 0.0280(4) Uani 1 1 d . . . H3A H 0.343 -0.0007 0.7077 0.034 Uiso 1 1 calc R . . H3B H 0.264 0.0987 0.6644 0.034 Uiso 1 1 calc R . . C10 C 0.4267(2) 0.14969(16) 0.88228(11) 0.0270(4) Uani 1 1 d . . . C11 C 0.5350(2) 0.09241(18) 0.92777(12) 0.0323(5) Uani 1 1 d . . . H11 H 0.5609 0.0218 0.9275 0.039 Uiso 1 1 calc R . . C12 C 0.6047(2) 0.1376(2) 0.97317(12) 0.0372(5) Uani 1 1 d . . . C13 C 0.5639(2) 0.2427(2) 0.97116(12) 0.0368(5) Uani 1 1 d . . . H13 H 0.6099 0.2744 1.0013 0.044 Uiso 1 1 calc R . . C14 C 0.4575(2) 0.30369(18) 0.92639(11) 0.0314(5) Uani 1 1 d . . . C15 C 0.3853(2) 0.25711(16) 0.88022(10) 0.0261(4) Uani 1 1 d . . . C16 C 0.7230(3) 0.0736(2) 1.02166(16) 0.0559(8) Uani 1 1 d . . . H16A H 0.7589 0.1175 1.0493 0.084 Uiso 0.5 1 calc PR . . H16B H 0.8006 0.0292 0.9923 0.084 Uiso 0.5 1 calc PR . . H16C H 0.6844 0.0338 1.0541 0.084 Uiso 0.5 1 calc PR . . H16D H 0.7371 0.0028 1.0144 0.084 Uiso 0.5 1 calc PR . . H16E H 0.6953 0.0912 1.0715 0.084 Uiso 0.5 1 calc PR . . H16F H 0.8115 0.0865 1.0097 0.084 Uiso 0.5 1 calc PR . . C17 C 0.4176(3) 0.4178(2) 0.92605(14) 0.0447(6) Uani 1 1 d . . . H17A H 0.3428 0.4465 0.892 0.067 Uiso 0.5 1 calc PR . . H17B H 0.5011 0.436 0.9122 0.067 Uiso 0.5 1 calc PR . . H17C H 0.3832 0.4437 0.9737 0.067 Uiso 0.5 1 calc PR . . H17D H 0.4753 0.4376 0.96 0.067 Uiso 0.5 1 calc PR . . H17E H 0.317 0.4481 0.9397 0.067 Uiso 0.5 1 calc PR . . H17F H 0.4349 0.4404 0.8782 0.067 Uiso 0.5 1 calc PR . . C20 C 0.4924(2) 0.14940(15) 0.64837(11) 0.0251(4) Uani 1 1 d . . . C21 C 0.5894(2) 0.08170(16) 0.60034(12) 0.0292(4) Uani 1 1 d . . . H21 H 0.651 0.0201 0.6178 0.035 Uiso 1 1 calc R . . C22 C 0.5961(2) 0.10418(17) 0.52685(12) 0.0318(5) Uani 1 1 d . . . C23 C 0.5034(2) 0.19754(17) 0.50361(11) 0.0319(5) Uani 1 1 d . . . H23 H 0.5072 0.2144 0.4548 0.038 Uiso 1 1 calc R . . C24 C 0.4047(2) 0.26727(16) 0.54988(11) 0.0277(4) Uani 1 1 d . . . C25 C 0.3953(2) 0.24318(15) 0.62423(10) 0.0236(4) Uani 1 1 d . . . C26 C 0.6991(3) 0.0288(2) 0.47494(14) 0.0441(6) Uani 1 1 d . . . H26A H 0.7539 -0.0307 0.5013 0.066 Uiso 0.5 1 calc PR . . H26B H 0.7638 0.0595 0.4518 0.066 Uiso 0.5 1 calc PR . . H26C H 0.6449 0.0098 0.4387 0.066 Uiso 0.5 1 calc PR . . H26D H 0.6878 0.0564 0.4266 0.066 Uiso 0.5 1 calc PR . . H26E H 0.6779 -0.0338 0.4761 0.066 Uiso 0.5 1 calc PR . . H26F H 0.7969 0.0159 0.4892 0.066 Uiso 0.5 1 calc PR . . C27 C 0.3085(3) 0.36837(18) 0.52236(12) 0.0385(5) Uani 1 1 d . . . H27A H 0.2485 0.406 0.5617 0.058 Uiso 0.5 1 calc PR . . H27B H 0.2485 0.3576 0.4855 0.058 Uiso 0.5 1 calc PR . . H27C H 0.3671 0.4061 0.5023 0.058 Uiso 0.5 1 calc PR . . H27D H 0.3275 0.3738 0.4713 0.058 Uiso 0.5 1 calc PR . . H27E H 0.3275 0.4222 0.5475 0.058 Uiso 0.5 1 calc PR . . H27F H 0.209 0.3737 0.5307 0.058 Uiso 0.5 1 calc PR . . C30 C 0.1343(2) 0.06739(16) 0.74331(12) 0.0285(4) Uani 1 1 d . . . C31 C 0.1077(3) -0.02425(18) 0.75196(14) 0.0395(5) Uani 1 1 d . . . H31 H 0.1814 -0.085 0.7412 0.047 Uiso 1 1 calc R . . C32 C -0.0268(3) -0.02676(19) 0.77635(15) 0.0459(6) Uani 1 1 d . . . C33 C -0.1343(3) 0.0654(2) 0.79085(13) 0.0409(6) Uani 1 1 d . . . H33 H -0.2248 0.0647 0.8073 0.049 Uiso 1 1 calc R . . C34 C -0.1135(2) 0.15941(17) 0.78202(11) 0.0303(4) Uani 1 1 d . . . C35 C 0.0252(2) 0.16086(15) 0.75956(10) 0.0248(4) Uani 1 1 d . . . C36 C -0.0559(4) -0.1273(3) 0.7831(2) 0.0775(11) Uani 1 1 d . . . H36A H 0.0311 -0.1824 0.7709 0.116 Uiso 0.5 1 calc PR . . H36B H -0.1304 -0.1272 0.7507 0.116 Uiso 0.5 1 calc PR . . H36C H -0.0868 -0.1357 0.8321 0.116 Uiso 0.5 1 calc PR . . H36D H -0.1551 -0.1144 0.7983 0.116 Uiso 0.5 1 calc PR . . H36E H 0.0063 -0.1696 0.8185 0.116 Uiso 0.5 1 calc PR . . H36F H -0.0373 -0.1611 0.737 0.116 Uiso 0.5 1 calc PR . . C37 C -0.2344(2) 0.2578(2) 0.79424(14) 0.0418(6) Uani 1 1 d . . . H37A H -0.1991 0.3137 0.7855 0.063 Uiso 0.5 1 calc PR . . H37B H -0.2711 0.2605 0.8434 0.063 Uiso 0.5 1 calc PR . . H37C H -0.3105 0.2624 0.7616 0.063 Uiso 0.5 1 calc PR . . H37D H -0.3214 0.2441 0.8082 0.063 Uiso 0.5 1 calc PR . . H37E H -0.2493 0.2972 0.7503 0.063 Uiso 0.5 1 calc PR . . H37F H -0.21 0.2953 0.8321 0.063 Uiso 0.5 1 calc PR . . C40 C -0.0526(2) 0.53190(14) 0.75099(11) 0.0247(4) Uani 1 1 d . . . C41 C -0.0682(2) 0.59857(15) 0.69061(11) 0.0279(4) Uani 1 1 d . . . C42 C -0.1803(2) 0.69111(16) 0.68661(12) 0.0316(5) Uani 1 1 d . . . C43 C -0.2843(2) 0.72114(16) 0.74242(13) 0.0342(5) Uani 1 1 d . . . C44 C -0.2752(2) 0.65795(16) 0.80213(12) 0.0328(5) Uani 1 1 d . . . C45 C -0.1618(2) 0.56576(16) 0.80598(11) 0.0290(4) Uani 1 1 d . . . C50 C -0.0017(3) 0.2287(2) 0.56821(15) 0.0512(7) Uani 1 1 d . . . H50A H 0.0021 0.18 0.6069 0.061 Uiso 1 1 calc R . . H50B H 0.0873 0.2045 0.5389 0.061 Uiso 1 1 calc R . . C51 C -0.1304(4) 0.2423(3) 0.52248(19) 0.0678(9) Uani 1 1 d . . . H51A H -0.1119 0.2603 0.473 0.081 Uiso 1 1 calc R . . H51B H -0.1562 0.1808 0.5221 0.081 Uiso 1 1 calc R . . C52 C -0.2457(4) 0.3267(3) 0.5589(2) 0.0823(12) Uani 1 1 d . . . H52A H -0.2969 0.3008 0.5961 0.099 Uiso 1 1 calc R . . H52B H -0.3145 0.3661 0.5241 0.099 Uiso 1 1 calc R . . C53 C -0.1674(3) 0.3902(2) 0.59178(19) 0.0618(8) Uani 1 1 d . . . H53A H -0.1742 0.4489 0.5613 0.074 Uiso 1 1 calc R . . H53B H -0.2096 0.4142 0.6393 0.074 Uiso 1 1 calc R . . C60 C 0.4838(3) 0.4948(2) 0.7024(2) 0.0631(8) Uani 1 1 d . . . H60A H 0.5074 0.4382 0.6687 0.076 Uiso 1 1 calc R . . H60B H 0.5645 0.4844 0.734 0.076 Uiso 1 1 calc R . . C61 C 0.4532(5) 0.5923(3) 0.6626(2) 0.0782(11) Uani 1 1 d . . . H61A H 0.424 0.5859 0.6137 0.094 Uiso 1 1 calc R . . H61B H 0.5382 0.6133 0.6599 0.094 Uiso 1 1 calc R . . C62 C 0.3324(4) 0.6678(2) 0.7054(2) 0.0774(11) Uani 1 1 d . . . H62A H 0.3645 0.7203 0.7255 0.093 Uiso 1 1 calc R . . H62B H 0.2507 0.6997 0.675 0.093 Uiso 1 1 calc R . . C63 C 0.2917(3) 0.6066(2) 0.76473(18) 0.0562(7) Uani 1 1 d . . . H63A H 0.3287 0.6185 0.8106 0.067 Uiso 1 1 calc R . . H63B H 0.1873 0.6249 0.7698 0.067 Uiso 1 1 calc R . . C70 C 0.1012(3) 0.3146(2) 0.99404(13) 0.0569(8) Uani 1 1 d . . . H70A H 0.0296 0.3774 1.0113 0.068 Uiso 1 1 calc R A 1 H70B H 0.1902 0.3277 0.981 0.068 Uiso 1 1 calc R A 1 C71A C 0.1264(3) 0.2349(2) 1.04938(13) 0.111(5) Uani 0.445(7) 1 d PRU B 1 H71A H 0.1207 0.2626 1.0978 0.133 Uiso 0.445(7) 1 d PR B 1 H71B H 0.2197 0.1822 1.0416 0.133 Uiso 0.445(7) 1 d PR B 1 C72A C 0.0007(12) 0.1924(7) 1.0367(3) 0.062(3) Uani 0.445(7) 1 d P B 1 H72A H 0.0306 0.1198 1.0463 0.075 Uiso 0.445(7) 1 calc PR B 1 H72B H -0.0835 0.2267 1.0674 0.075 Uiso 0.445(7) 1 calc PR B 1 C71B C 0.0007(5) 0.3267(5) 1.0561(2) 0.0547(18) Uani 0.555(7) 1 d P B 2 H71C H 0.0497 0.2899 1.0979 0.066 Uiso 0.555(7) 1 calc PR B 2 H71D H -0.0438 0.398 1.0687 0.066 Uiso 0.555(7) 1 calc PR B 2 C72B C -0.1053(11) 0.2849(10) 1.0321(4) 0.106(4) Uani 0.555(7) 1 d P B 2 H72C H -0.1926 0.3389 1.0185 0.128 Uiso 0.555(7) 1 calc PR B 2 H72D H -0.1301 0.2443 1.0702 0.128 Uiso 0.555(7) 1 calc PR B 2 C73 C -0.0295(4) 0.2136(3) 0.96136(16) 0.0641(9) Uani 1 1 d . . . H73A H -0.0027 0.1503 0.9345 0.077 Uiso 1 1 calc R B 1 H73B H -0.1323 0.2487 0.9562 0.077 Uiso 1 1 calc R B 1 H1 H 0.293(3) 0.189(2) 0.7570(13) 0.032(6) Uiso 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 0.0244(7) 0.0267(7) 0.0271(7) 0.0022(5) -0.0017(5) -0.0068(6) O2 0.0240(7) 0.0231(7) 0.0249(7) -0.0021(5) 0.0043(5) -0.0044(6) O3 0.0240(7) 0.0218(7) 0.0308(8) 0.0021(5) 0.0017(5) -0.0064(6) O4 0.0341(8) 0.0347(8) 0.0378(9) -0.0004(7) -0.0084(6) -0.0080(7) O5 0.0481(10) 0.0460(10) 0.0303(8) 0.0035(7) 0.0051(7) -0.0220(8) O6 0.0258(7) 0.0191(7) 0.0336(8) -0.0008(5) 0.0033(6) -0.0016(6) O7 0.0396(9) 0.0282(8) 0.0502(10) -0.0032(7) 0.0091(7) -0.0157(7) N1 0.0196(8) 0.0190(8) 0.0269(9) 0.0003(6) -0.0003(6) -0.0037(7) Cl1 0.0470(3) 0.0333(3) 0.0356(3) 0.0022(2) 0.0114(2) -0.0063(2) Cl2 0.0668(4) 0.0321(3) 0.0487(4) 0.0134(3) -0.0101(3) -0.0046(3) Cl3 0.0384(3) 0.0273(3) 0.0879(5) -0.0020(3) -0.0060(3) 0.0082(2) Cl4 0.0376(3) 0.0469(4) 0.0598(4) -0.0142(3) 0.0188(3) 0.0005(3) Cl5 0.0505(4) 0.0370(3) 0.0376(3) 0.0034(2) 0.0148(2) -0.0034(3) Li1 0.0281(18) 0.0261(17) 0.0309(18) -0.0008(13) 0.0039(13) -0.0098(14) Li2 0.0252(17) 0.0259(17) 0.0288(18) 0.0003(13) 0.0002(13) -0.0048(14) Li3 0.0263(17) 0.0290(18) 0.0304(18) 0.0009(14) 0.0048(13) -0.0073(14) C1 0.0263(10) 0.0261(10) 0.0301(11) 0.0069(8) -0.0009(8) -0.0074(8) C2 0.0193(9) 0.0254(10) 0.0315(11) 0.0000(8) 0.0000(7) -0.0042(8) C3 0.0259(10) 0.0214(10) 0.0352(11) -0.0047(8) -0.0011(8) -0.0056(8) C10 0.0226(10) 0.0338(11) 0.0243(10) 0.0035(8) 0.0018(7) -0.0097(8) C11 0.0248(10) 0.0385(12) 0.0322(11) 0.0115(9) -0.0012(8) -0.0090(9) C12 0.0285(11) 0.0563(15) 0.0287(11) 0.0133(10) -0.0026(8) -0.0171(11) C13 0.0313(11) 0.0610(16) 0.0249(11) 0.0014(10) -0.0006(8) -0.0245(11) C14 0.0298(11) 0.0428(12) 0.0241(10) -0.0030(9) 0.0042(8) -0.0157(9) C15 0.0220(9) 0.0339(11) 0.0220(10) 0.0009(8) 0.0027(7) -0.0089(8) C16 0.0457(15) 0.076(2) 0.0538(17) 0.0304(14) -0.0238(12) -0.0295(15) C17 0.0511(15) 0.0447(14) 0.0440(14) -0.0093(11) -0.0050(11) -0.0228(12) C20 0.0209(9) 0.0268(10) 0.0278(10) -0.0026(8) 0.0019(7) -0.0083(8) C21 0.0235(10) 0.0254(10) 0.0365(11) -0.0051(8) 0.0023(8) -0.0051(8) C22 0.0272(11) 0.0343(12) 0.0340(12) -0.0113(9) 0.0074(8) -0.0105(9) C23 0.0332(11) 0.0381(12) 0.0250(10) -0.0042(8) 0.0077(8) -0.0134(10) C24 0.0282(10) 0.0280(10) 0.0276(10) -0.0006(8) 0.0014(8) -0.0105(8) C25 0.0210(9) 0.0238(10) 0.0266(10) -0.0039(7) 0.0035(7) -0.0086(8) C26 0.0424(14) 0.0422(14) 0.0450(14) -0.0177(11) 0.0137(11) -0.0111(11) C27 0.0465(14) 0.0346(12) 0.0284(12) 0.0057(9) 0.0069(9) -0.0065(10) C30 0.0269(10) 0.0262(10) 0.0340(11) 0.0033(8) -0.0061(8) -0.0104(8) C31 0.0396(13) 0.0264(11) 0.0553(15) 0.0069(10) -0.0127(11) -0.0137(10) C32 0.0461(15) 0.0383(13) 0.0642(17) 0.0174(12) -0.0181(12) -0.0277(12) C33 0.0338(12) 0.0575(16) 0.0426(13) 0.0157(11) -0.0099(10) -0.0298(12) C34 0.0263(10) 0.0407(12) 0.0267(10) 0.0044(9) -0.0035(8) -0.0149(9) C35 0.0255(10) 0.0265(10) 0.0241(10) 0.0032(7) -0.0038(7) -0.0110(8) C36 0.080(2) 0.058(2) 0.116(3) 0.0256(19) -0.022(2) -0.0510(19) C37 0.0235(11) 0.0547(15) 0.0444(14) -0.0012(11) 0.0039(9) -0.0098(10) C40 0.0237(10) 0.0184(9) 0.0311(10) -0.0028(7) -0.0017(8) -0.0058(8) C41 0.0291(10) 0.0233(10) 0.0305(11) -0.0033(8) 0.0006(8) -0.0076(8) C42 0.0358(12) 0.0209(10) 0.0381(12) 0.0008(8) -0.0083(9) -0.0085(9) C43 0.0263(11) 0.0188(10) 0.0528(14) -0.0054(9) -0.0068(9) -0.0002(8) C44 0.0251(10) 0.0281(11) 0.0417(12) -0.0105(9) 0.0028(9) -0.0042(9) C45 0.0283(11) 0.0246(10) 0.0319(11) -0.0036(8) 0.0017(8) -0.0058(8) C50 0.0674(18) 0.0388(14) 0.0439(15) -0.0066(11) -0.0112(13) -0.0119(13) C51 0.072(2) 0.077(2) 0.068(2) -0.0135(17) -0.0056(16) -0.0417(19) C52 0.0456(18) 0.112(3) 0.095(3) -0.039(2) -0.0051(17) -0.031(2) C53 0.0355(14) 0.0577(18) 0.084(2) -0.0130(16) -0.0179(14) -0.0028(13) C60 0.0479(16) 0.0490(17) 0.090(2) 0.0020(15) 0.0254(15) -0.0160(14) C61 0.106(3) 0.070(2) 0.075(2) 0.0123(18) 0.016(2) -0.052(2) C62 0.079(2) 0.0362(16) 0.121(3) 0.0160(18) -0.013(2) -0.0246(16) C63 0.0568(17) 0.0327(13) 0.081(2) -0.0195(13) 0.0074(15) -0.0178(13) C70 0.072(2) 0.080(2) 0.0336(14) -0.0101(13) 0.0128(13) -0.0468(18) C71A 0.189(13) 0.128(10) 0.059(5) 0.027(5) -0.053(7) -0.106(10) C72A 0.120(7) 0.077(5) 0.026(3) 0.013(3) -0.013(3) -0.080(6) C71B 0.043(3) 0.111(5) 0.024(2) -0.006(2) 0.0086(18) -0.044(3) C72B 0.114(7) 0.216(13) 0.041(3) -0.033(5) 0.023(4) -0.125(8) C73 0.071(2) 0.090(2) 0.0518(17) 0.0187(16) -0.0026(14) -0.0556(19) #----------------------------------------------------------------------------# # 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 C15 1.328(2) . ? O1 Li1 1.917(4) . ? O1 Li3 1.927(4) . ? O2 C25 1.332(2) . ? O2 Li1 1.906(4) . ? O2 Li2 1.929(4) . ? O3 C35 1.327(2) . ? O3 Li2 1.906(4) . ? O3 Li3 1.915(4) . ? O4 C53 1.415(3) . ? O4 C50 1.443(3) . ? O4 Li2 1.944(4) . ? O5 C73 1.412(3) . ? O5 C70 1.439(3) . ? O5 Li3 2.053(4) . ? O6 C40 1.295(2) . ? O6 Li1 2.030(4) . ? O6 Li2 2.030(4) . ? O6 Li3 2.102(4) . ? O7 C60 1.419(3) . ? O7 C63 1.430(3) . ? O7 Li1 1.936(4) . ? N1 C3 1.499(3) . ? N1 C1 1.501(3) . ? N1 C2 1.503(2) . ? N1 H1 0.84(3) . ? Cl1 C41 1.724(2) . ? Cl2 C42 1.726(2) . ? Cl3 C43 1.726(2) . ? Cl4 C44 1.725(2) . ? Cl5 C45 1.727(2) . ? Li1 Li2 2.586(5) . ? Li1 Li3 2.736(5) . ? Li2 Li3 2.785(5) . ? C1 C10 1.499(3) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C2 C20 1.502(3) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C30 1.503(3) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C10 C11 1.395(3) . ? C10 C15 1.413(3) . ? C11 C12 1.380(3) . ? C11 H11 0.93 . ? C12 C13 1.383(4) . ? C12 C16 1.517(3) . ? C13 C14 1.394(3) . ? C13 H13 0.93 . ? C14 C15 1.418(3) . ? C14 C17 1.504(3) . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C16 H16D 0.96 . ? C16 H16E 0.96 . ? C16 H16F 0.96 . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C17 H17C 0.96 . ? C17 H17D 0.96 . ? C17 H17E 0.96 . ? C17 H17F 0.96 . ? C20 C21 1.394(3) . ? C20 C25 1.412(3) . ? C21 C22 1.390(3) . ? C21 H21 0.93 . ? C22 C23 1.387(3) . ? C22 C26 1.513(3) . ? C23 C24 1.394(3) . ? C23 H23 0.93 . ? C24 C25 1.413(3) . ? C24 C27 1.503(3) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C26 H26D 0.96 . ? C26 H26E 0.96 . ? C26 H26F 0.96 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C27 H27D 0.96 . ? C27 H27E 0.96 . ? C27 H27F 0.96 . ? C30 C31 1.391(3) . ? C30 C35 1.410(3) . ? C31 C32 1.388(4) . ? C31 H31 0.93 . ? C32 C33 1.385(4) . ? C32 C36 1.521(4) . ? C33 C34 1.396(3) . ? C33 H33 0.93 . ? C34 C35 1.413(3) . ? C34 C37 1.497(3) . ? C36 H36A 0.96 . ? C36 H36B 0.96 . ? C36 H36C 0.96 . ? C36 H36D 0.96 . ? C36 H36E 0.96 . ? C36 H36F 0.96 . ? C37 H37A 0.96 . ? C37 H37B 0.96 . ? C37 H37C 0.96 . ? C37 H37D 0.96 . ? C37 H37E 0.96 . ? C37 H37F 0.96 . ? C40 C45 1.412(3) . ? C40 C41 1.419(3) . ? C41 C42 1.390(3) . ? C42 C43 1.387(3) . ? C43 C44 1.386(3) . ? C44 C45 1.393(3) . ? C50 C51 1.501(4) . ? C50 H50A 0.97 . ? C50 H50B 0.97 . ? C51 C52 1.480(5) . ? C51 H51A 0.97 . ? C51 H51B 0.97 . ? C52 C53 1.495(4) . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? C53 H53A 0.97 . ? C53 H53B 0.97 . ? C60 C61 1.479(4) . ? C60 H60A 0.97 . ? C60 H60B 0.97 . ? C61 C62 1.502(5) . ? C61 H61A 0.97 . ? C61 H61B 0.97 . ? C62 C63 1.499(5) . ? C62 H62A 0.97 . ? C62 H62B 0.97 . ? C63 H63A 0.97 . ? C63 H63B 0.97 . ? C70 C71B 1.456(5) . ? C70 C71A 1.4619 . ? C70 H70A 0.97 . ? C70 H70B 0.97 . ? C71A C72A 1.560(7) . ? C71A H71A 0.97 . ? C71A H71B 0.97 . ? C72A C73 1.435(6) . ? C72A H72A 0.97 . ? C72A H72B 0.97 . ? C71B C72B 1.434(8) . ? C71B H71A 1.4562 . ? C71B H71C 0.97 . ? C71B H71D 0.97 . ? C72B C73 1.647(9) . ? C72B H72C 0.97 . ? C72B H72D 0.97 . ? C73 H73A 0.97 . ? C73 H73B 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 C15 O1 Li1 137.29(16) . . ? C15 O1 Li3 131.86(16) . . ? Li1 O1 Li3 90.74(16) . . ? C25 O2 Li1 145.41(16) . . ? C25 O2 Li2 129.65(16) . . ? Li1 O2 Li2 84.81(15) . . ? C35 O3 Li2 139.10(16) . . ? C35 O3 Li3 127.25(16) . . ? Li2 O3 Li3 93.59(16) . . ? C53 O4 C50 109.3(2) . . ? C53 O4 Li2 122.65(19) . . ? C50 O4 Li2 116.95(17) . . ? C73 O5 C70 107.10(19) . . ? C73 O5 Li3 134.78(19) . . ? C70 O5 Li3 117.60(17) . . ? C40 O6 Li1 139.05(16) . . ? C40 O6 Li2 123.50(16) . . ? Li1 O6 Li2 79.13(14) . . ? C40 O6 Li3 128.54(16) . . ? Li1 O6 Li3 82.90(14) . . ? Li2 O6 Li3 84.73(14) . . ? C60 O7 C63 106.7(2) . . ? C60 O7 Li1 123.75(19) . . ? C63 O7 Li1 128.50(19) . . ? C3 N1 C1 112.25(15) . . ? C3 N1 C2 112.18(15) . . ? C1 N1 C2 112.21(15) . . ? C3 N1 H1 106.6(16) . . ? C1 N1 H1 105.6(16) . . ? C2 N1 H1 107.5(16) . . ? O2 Li1 O1 106.40(17) . . ? O2 Li1 O7 117.78(18) . . ? O1 Li1 O7 123.29(19) . . ? O2 Li1 O6 97.71(16) . . ? O1 Li1 O6 93.07(15) . . ? O7 Li1 O6 113.04(18) . . ? O2 Li1 Li2 47.98(12) . . ? O1 Li1 Li2 98.24(16) . . ? O7 Li1 Li2 137.54(19) . . ? O6 Li1 Li2 50.44(11) . . ? O2 Li1 Li3 98.64(16) . . ? O1 Li1 Li3 44.79(11) . . ? O7 Li1 Li3 142.64(18) . . ? O6 Li1 Li3 49.69(11) . . ? Li2 Li1 Li3 63.04(13) . . ? O3 Li2 O2 109.49(17) . . ? O3 Li2 O4 107.44(18) . . ? O2 Li2 O4 121.04(18) . . ? O3 Li2 O6 89.24(15) . . ? O2 Li2 O6 96.96(16) . . ? O4 Li2 O6 127.82(18) . . ? O3 Li2 Li1 97.82(16) . . ? O2 Li2 Li1 47.22(11) . . ? O4 Li2 Li1 154.73(19) . . ? O6 Li2 Li1 50.43(11) . . ? O3 Li2 Li3 43.34(11) . . ? O2 Li2 Li3 96.45(15) . . ? O4 Li2 Li3 140.88(18) . . ? O6 Li2 Li3 48.74(11) . . ? Li1 Li2 Li3 61.11(13) . . ? O3 Li3 O1 108.76(17) . . ? O3 Li3 O5 113.76(18) . . ? O1 Li3 O5 99.04(17) . . ? O3 Li3 O6 86.88(15) . . ? O1 Li3 O6 90.53(15) . . ? O5 Li3 O6 152.49(19) . . ? O3 Li3 Li1 92.78(15) . . ? O1 Li3 Li1 44.48(11) . . ? O5 Li3 Li1 141.80(19) . . ? O6 Li3 Li1 47.41(11) . . ? O3 Li3 Li2 43.08(11) . . ? O1 Li3 Li2 91.65(15) . . ? O5 Li3 Li2 156.82(19) . . ? O6 Li3 Li2 46.53(11) . . ? Li1 Li3 Li2 55.85(12) . . ? C10 C1 N1 113.21(16) . . ? C10 C1 H1A 108.9 . . ? N1 C1 H1A 108.9 . . ? C10 C1 H1B 108.9 . . ? N1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C20 C2 N1 113.08(16) . . ? C20 C2 H2A 109 . . ? N1 C2 H2A 109 . . ? C20 C2 H2B 109 . . ? N1 C2 H2B 109 . . ? H2A C2 H2B 107.8 . . ? N1 C3 C30 113.53(17) . . ? N1 C3 H3A 108.9 . . ? C30 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C30 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C11 C10 C15 121.0(2) . . ? C11 C10 C1 119.28(19) . . ? C15 C10 C1 119.72(17) . . ? C12 C11 C10 121.9(2) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 117.1(2) . . ? C11 C12 C16 120.9(2) . . ? C13 C12 C16 122.0(2) . . ? C12 C13 C14 123.6(2) . . ? C12 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 119.2(2) . . ? C13 C14 C17 121.5(2) . . ? C15 C14 C17 119.3(2) . . ? O1 C15 C10 120.90(18) . . ? O1 C15 C14 121.82(19) . . ? C10 C15 C14 117.28(19) . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C16 H16D 109.5 . . ? H16A C16 H16D 141.1 . . ? H16B C16 H16D 56.3 . . ? H16C C16 H16D 56.3 . . ? C12 C16 H16E 109.5 . . ? H16A C16 H16E 56.3 . . ? H16B C16 H16E 141.1 . . ? H16C C16 H16E 56.3 . . ? H16D C16 H16E 109.5 . . ? C12 C16 H16F 109.5 . . ? H16A C16 H16F 56.3 . . ? H16B C16 H16F 56.3 . . ? H16C C16 H16F 141.1 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C17 H17D 109.5 . . ? H17A C17 H17D 141.1 . . ? H17B C17 H17D 56.3 . . ? H17C C17 H17D 56.3 . . ? C14 C17 H17E 109.5 . . ? H17A C17 H17E 56.3 . . ? H17B C17 H17E 141.1 . . ? H17C C17 H17E 56.3 . . ? H17D C17 H17E 109.5 . . ? C14 C17 H17F 109.5 . . ? H17A C17 H17F 56.3 . . ? H17B C17 H17F 56.3 . . ? H17C C17 H17F 141.1 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? C21 C20 C25 121.37(19) . . ? C21 C20 C2 119.29(18) . . ? C25 C20 C2 119.33(17) . . ? C22 C21 C20 121.4(2) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C23 C22 C21 117.08(19) . . ? C23 C22 C26 122.0(2) . . ? C21 C22 C26 120.9(2) . . ? C22 C23 C24 123.2(2) . . ? C22 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C23 C24 C25 119.64(19) . . ? C23 C24 C27 121.23(19) . . ? C25 C24 C27 119.13(18) . . ? O2 C25 C20 120.84(17) . . ? O2 C25 C24 121.97(18) . . ? C20 C25 C24 117.19(17) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C22 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C22 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C24 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C24 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C31 C30 C35 120.8(2) . . ? C31 C30 C3 120.4(2) . . ? C35 C30 C3 118.71(18) . . ? C32 C31 C30 121.3(2) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C33 C32 C31 117.6(2) . . ? C33 C32 C36 121.6(3) . . ? C31 C32 C36 120.7(3) . . ? C32 C33 C34 123.2(2) . . ? C32 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C33 C34 C35 118.7(2) . . ? C33 C34 C37 121.8(2) . . ? C35 C34 C37 119.6(2) . . ? O3 C35 C30 120.05(18) . . ? O3 C35 C34 121.60(19) . . ? C30 C35 C34 118.35(19) . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C36 H36D 109.5 . . ? H36A C36 H36D 141.1 . . ? H36B C36 H36D 56.3 . . ? H36C C36 H36D 56.3 . . ? C32 C36 H36E 109.5 . . ? H36A C36 H36E 56.3 . . ? H36B C36 H36E 141.1 . . ? H36C C36 H36E 56.3 . . ? H36D C36 H36E 109.5 . . ? C32 C36 H36F 109.5 . . ? H36A C36 H36F 56.3 . . ? H36B C36 H36F 56.3 . . ? H36C C36 H36F 141.1 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 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 . . ? C34 C37 H37D 109.5 . . ? H37A C37 H37D 141.1 . . ? H37B C37 H37D 56.3 . . ? H37C C37 H37D 56.3 . . ? C34 C37 H37E 109.5 . . ? H37A C37 H37E 56.3 . . ? H37B C37 H37E 141.1 . . ? H37C C37 H37E 56.3 . . ? H37D C37 H37E 109.5 . . ? C34 C37 H37F 109.5 . . ? H37A C37 H37F 56.3 . . ? H37B C37 H37F 56.3 . . ? H37C C37 H37F 141.1 . . ? H37D C37 H37F 109.5 . . ? H37E C37 H37F 109.5 . . ? O6 C40 C45 122.61(18) . . ? O6 C40 C41 122.64(18) . . ? C45 C40 C41 114.74(18) . . ? C42 C41 C40 122.66(19) . . ? C42 C41 Cl1 120.62(17) . . ? C40 C41 Cl1 116.72(15) . . ? C43 C42 C41 120.3(2) . . ? C43 C42 Cl2 119.66(16) . . ? C41 C42 Cl2 120.06(17) . . ? C44 C43 C42 119.31(19) . . ? C44 C43 Cl3 120.32(17) . . ? C42 C43 Cl3 120.36(18) . . ? C43 C44 C45 120.0(2) . . ? C43 C44 Cl4 120.14(16) . . ? C45 C44 Cl4 119.83(18) . . ? C44 C45 C40 123.0(2) . . ? C44 C45 Cl5 120.04(16) . . ? C40 C45 Cl5 116.99(15) . . ? O4 C50 C51 105.6(2) . . ? O4 C50 H50A 110.6 . . ? C51 C50 H50A 110.6 . . ? O4 C50 H50B 110.6 . . ? C51 C50 H50B 110.6 . . ? H50A C50 H50B 108.8 . . ? C52 C51 C50 103.3(3) . . ? C52 C51 H51A 111.1 . . ? C50 C51 H51A 111.1 . . ? C52 C51 H51B 111.1 . . ? C50 C51 H51B 111.1 . . ? H51A C51 H51B 109.1 . . ? C51 C52 C53 104.6(3) . . ? C51 C52 H52A 110.8 . . ? C53 C52 H52A 110.8 . . ? C51 C52 H52B 110.8 . . ? C53 C52 H52B 110.8 . . ? H52A C52 H52B 108.9 . . ? O4 C53 C52 107.3(3) . . ? O4 C53 H53A 110.3 . . ? C52 C53 H53A 110.3 . . ? O4 C53 H53B 110.3 . . ? C52 C53 H53B 110.3 . . ? H53A C53 H53B 108.5 . . ? O7 C60 C61 106.1(3) . . ? O7 C60 H60A 110.5 . . ? C61 C60 H60A 110.5 . . ? O7 C60 H60B 110.5 . . ? C61 C60 H60B 110.5 . . ? H60A C60 H60B 108.7 . . ? C60 C61 C62 105.4(3) . . ? C60 C61 H61A 110.7 . . ? C62 C61 H61A 110.7 . . ? C60 C61 H61B 110.7 . . ? C62 C61 H61B 110.7 . . ? H61A C61 H61B 108.8 . . ? C63 C62 C61 105.0(2) . . ? C63 C62 H62A 110.7 . . ? C61 C62 H62A 110.7 . . ? C63 C62 H62B 110.7 . . ? C61 C62 H62B 110.7 . . ? H62A C62 H62B 108.8 . . ? O7 C63 C62 106.0(2) . . ? O7 C63 H63A 110.5 . . ? C62 C63 H63A 110.5 . . ? O7 C63 H63B 110.5 . . ? C62 C63 H63B 110.5 . . ? H63A C63 H63B 108.7 . . ? O5 C70 C71B 110.0(3) . . ? O5 C70 C71A 104.68(14) . . ? C71B C70 C71A 59.8(3) . . ? O5 C70 H70A 110.8 . . ? C71B C70 H70A 53 . . ? C71A C70 H70A 110.8 . . ? O5 C70 H70B 110.8 . . ? C71B C70 H70B 139.1 . . ? C71A C70 H70B 110.8 . . ? H70A C70 H70B 108.9 . . ? C70 C71A C72A 101.8(3) . . ? C70 C71A H71A 111.5 . . ? C72A C71A H71A 111.9 . . ? C70 C71A H71B 111.5 . . ? C72A C71A H71B 110.7 . . ? H71A C71A H71B 109.3 . . ? C73 C72A C71A 103.6(4) . . ? C73 C72A H72A 111 . . ? C71A C72A H72A 111 . . ? C73 C72A H72B 111 . . ? C71A C72A H72B 111 . . ? H72A C72A H72B 109 . . ? C72B C71B C70 104.3(4) . . ? C72B C71B H71A 118.9 . . ? C70 C71B H71A 88.3 . . ? C72B C71B H71C 110.9 . . ? C70 C71B H71C 110.9 . . ? C72B C71B H71D 110.9 . . ? C70 C71B H71D 110.9 . . ? H71A C71B H71D 119.5 . . ? H71C C71B H71D 108.9 . . ? C71B C72B C73 105.6(5) . . ? C71B C72B H72C 110.6 . . ? C73 C72B H72C 110.6 . . ? C71B C72B H72D 110.6 . . ? C73 C72B H72D 110.6 . . ? H72C C72B H72D 108.8 . . ? O5 C73 C72A 109.8(3) . . ? O5 C73 C72B 97.5(4) . . ? C72A C73 C72B 51.9(5) . . ? O5 C73 H73A 109.7 . . ? C72A C73 H73A 109.7 . . ? C72B C73 H73A 151.9 . . ? O5 C73 H73B 109.7 . . ? C72A C73 H73B 109.7 . . ? C72B C73 H73B 67.3 . . ? H73A C73 H73B 108.2 . . ? _database_code_depnum_ccdc_archive 'CCDC 916823' ####################################################################### # # 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_Compound_6_h10mgd03 #TrackingRef '16352_web_deposit_cif_file_0_DanielGarcia-Vivo_1356029066.LiCage_final.cif' _audit_creation_date 2012-12-20 _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 ? #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 6' _chemical_formula_sum 'C94 H132 Cl10 N2 Na6 O15' _chemical_formula_weight 2022.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8510(3) _cell_length_b 20.6590(5) _cell_length_c 21.2810(5) _cell_angle_alpha 107.1770(10) _cell_angle_beta 90.7680(10) _cell_angle_gamma 92.202(2) _cell_volume 5392.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 91569 _cell_measurement_theta_min 3.513 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2132 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.34 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.0558832 _diffrn_orient_matrix_ub_12 0.0223656 _diffrn_orient_matrix_ub_13 0.0299819 _diffrn_orient_matrix_ub_21 -0.0379657 _diffrn_orient_matrix_ub_22 -0.0449363 _diffrn_orient_matrix_ub_23 -0.0076837 _diffrn_orient_matrix_ub_31 0.0387774 _diffrn_orient_matrix_ub_32 -0.0072436 _diffrn_orient_matrix_ub_33 0.038247 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.164 _diffrn_reflns_av_unetI/netI 0.1271 _diffrn_reflns_number 59857 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.937 _reflns_number_total 23305 _reflns_number_gt 12240 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0400+15.3349*P+(0.0797P)^2^+0.0000sin\q/\l] where P = 0.10000Fo^2^ + 0.90000Fc^2^ ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 23305 _refine_ls_number_parameters 1177 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1766 _refine_ls_R_factor_gt 0.1079 _refine_ls_wR_factor_ref 0.3557 _refine_ls_wR_factor_gt 0.2834 _refine_ls_goodness_of_fit_ref 1.471 _refine_ls_restrained_S_all 1.471 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.675 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 Na1A Na 0.7892(2) 0.71996(16) 0.34050(15) 0.0726(8) Uani 1 1 d . . . Na2A Na 0.6587(2) 0.69566(15) 0.46471(12) 0.0648(7) Uani 1 1 d . . . Na3A Na 0.5606(3) 0.76779(15) 0.36319(13) 0.0679(7) Uani 1 1 d . . . O1A O 0.6382(5) 0.7006(2) 0.2782(2) 0.0670(13) Uani 1 1 d . . . O2A O 0.7593(4) 0.6352(3) 0.3817(3) 0.0688(13) Uani 1 1 d . . . O3A O 0.5115(4) 0.6841(3) 0.4058(2) 0.0667(12) Uani 1 1 d . . . O4A O 0.7078(4) 0.7929(2) 0.4336(2) 0.0629(12) Uani 1 1 d . . . O5A O 0.9676(6) 0.7159(4) 0.3167(5) 0.117(3) Uani 1 1 d . . . O6A O 0.6110(7) 0.6456(4) 0.5455(4) 0.106(2) Uani 1 1 d . . . O7A O 0.4510(7) 0.8467(5) 0.3430(5) 0.127(3) Uani 1 1 d . . . Cl1A Cl 0.7834(4) 0.87677(14) 0.35391(11) 0.1292(13) Uani 1 1 d . . . Cl2A Cl 0.8655(6) 1.02135(19) 0.43700(19) 0.217(3) Uani 1 1 d . . . Cl3A Cl 0.8671(5) 1.06286(16) 0.59083(18) 0.169(2) Uani 1 1 d . . . Cl4A Cl 0.7814(4) 0.96049(15) 0.66028(12) 0.1438(16) Uani 1 1 d . . . Cl5A Cl 0.7018(4) 0.81643(14) 0.57626(11) 0.1439(16) Uani 1 1 d . . . N1A N 0.5820(4) 0.5696(3) 0.3003(2) 0.0437(10) Uani 1 1 d . . . C1A C 0.5194(5) 0.5756(4) 0.2414(3) 0.0545(14) Uani 1 1 d . . . H1A1 H 0.4875 0.5304 0.2177 0.065 Uiso 1 1 calc R . . H1A2 H 0.4621 0.6064 0.2574 0.065 Uiso 1 1 calc R . . C2A C 0.6739(5) 0.5259(4) 0.2772(3) 0.0538(14) Uani 1 1 d . . . H2A1 H 0.7186 0.5471 0.2505 0.065 Uiso 1 1 calc R . . H2A2 H 0.6481 0.481 0.2485 0.065 Uiso 1 1 calc R . . C3A C 0.5177(5) 0.5417(4) 0.3459(3) 0.0578(16) Uani 1 1 d . . . H3A1 H 0.56 0.5452 0.3861 0.069 Uiso 1 1 calc R . . H3A2 H 0.5005 0.493 0.3241 0.069 Uiso 1 1 calc R . . C4A C 0.7430(6) 0.8519(3) 0.4674(3) 0.0572(15) Uani 1 1 d . . . C5A C 0.7832(8) 0.9008(4) 0.4385(4) 0.074(2) Uani 1 1 d . . . C6A C 0.8206(10) 0.9641(5) 0.4757(4) 0.100(3) Uani 1 1 d . . . C7A C 0.8216(9) 0.9829(4) 0.5436(4) 0.091(3) Uani 1 1 d . . . C8A C 0.7814(9) 0.9380(4) 0.5746(4) 0.086(3) Uani 1 1 d . . . C9A C 0.7454(7) 0.8750(4) 0.5377(4) 0.072(2) Uani 1 1 d . . . C10A C 0.5815(5) 0.6014(4) 0.1934(3) 0.0555(15) Uani 1 1 d . . . C11A C 0.6328(6) 0.6655(4) 0.2153(3) 0.0579(16) Uani 1 1 d . . . C12A C 0.6792(6) 0.6916(4) 0.1672(3) 0.0617(17) Uani 1 1 d . . . C13A C 0.6776(6) 0.6511(4) 0.1013(3) 0.0642(18) Uani 1 1 d . . . H13A H 0.7071 0.6694 0.0692 0.077 Uiso 1 1 calc R . . C14A C 0.6347(5) 0.5855(4) 0.0811(3) 0.0583(16) Uani 1 1 d . . . C15A C 0.5859(6) 0.5617(4) 0.1280(3) 0.0574(15) Uani 1 1 d . . . H15A H 0.5546 0.5172 0.1153 0.069 Uiso 1 1 calc R . . C16A C 0.7288(9) 0.7622(5) 0.1879(4) 0.087(3) Uani 1 1 d . . . H16A H 0.6776 0.7945 0.2105 0.131 Uiso 1 1 calc R . . H16B H 0.7526 0.774 0.149 0.131 Uiso 1 1 calc R . . H16C H 0.7883 0.7642 0.2178 0.131 Uiso 1 1 calc R . . C17A C 0.6427(8) 0.5423(5) 0.0109(3) 0.082(2) Uani 1 1 d . . . H17A H 0.6192 0.4956 0.0071 0.122 Uiso 1 1 calc R . . H17B H 0.7153 0.543 -0.0025 0.122 Uiso 1 1 calc R . . H17C H 0.5988 0.5601 -0.0176 0.122 Uiso 1 1 calc R . . C18A C 0.7391(5) 0.5161(4) 0.3333(3) 0.0548(15) Uani 1 1 d . . . C19A C 0.7819(5) 0.5737(4) 0.3818(3) 0.0581(15) Uani 1 1 d . . . C20A C 0.8493(5) 0.5614(4) 0.4304(3) 0.0572(15) Uani 1 1 d . . . C21A C 0.8667(5) 0.4960(4) 0.4307(4) 0.0640(17) Uani 1 1 d . . . H21A H 0.9131 0.4896 0.4633 0.077 Uiso 1 1 calc R . . C22A C 0.8199(6) 0.4392(4) 0.3857(4) 0.0664(18) Uani 1 1 d . . . C23A C 0.7563(6) 0.4501(4) 0.3361(4) 0.0629(17) Uani 1 1 d . . . H23A H 0.7242 0.4123 0.3039 0.075 Uiso 1 1 calc R . . C24A C 0.9053(7) 0.6223(5) 0.4794(4) 0.081(2) Uani 1 1 d . . . H24A H 0.8564 0.6585 0.4952 0.121 Uiso 1 1 calc R . . H24B H 0.9632 0.6387 0.4579 0.121 Uiso 1 1 calc R . . H24C H 0.9324 0.6088 0.5167 0.121 Uiso 1 1 calc R . . C25A C 0.8401(9) 0.3680(5) 0.3908(5) 0.095(3) Uani 1 1 d . . . H25A H 0.8079 0.3338 0.3526 0.142 Uiso 1 1 calc R . . H25B H 0.8099 0.3629 0.4312 0.142 Uiso 1 1 calc R . . H25C H 0.9153 0.3621 0.3918 0.142 Uiso 1 1 calc R . . C26A C 0.4176(5) 0.5779(4) 0.3656(3) 0.0589(16) Uani 1 1 d . . . C27A C 0.4226(5) 0.6480(4) 0.3982(3) 0.0574(15) Uani 1 1 d . . . C28A C 0.3293(6) 0.6789(4) 0.4256(3) 0.0626(17) Uani 1 1 d . . . C29A C 0.2388(6) 0.6384(5) 0.4172(4) 0.069(2) Uani 1 1 d . . . H29A H 0.1778 0.6586 0.4373 0.083 Uiso 1 1 calc R . . C30A C 0.2313(6) 0.5704(5) 0.3813(4) 0.070(2) Uani 1 1 d . . . C31A C 0.3221(6) 0.5402(4) 0.3564(4) 0.0671(18) Uani 1 1 d . . . H31A H 0.3201 0.4933 0.3328 0.08 Uiso 1 1 calc R . . C32A C 0.3329(8) 0.7535(5) 0.4635(5) 0.093(3) Uani 1 1 d . . . H32A H 0.3907 0.7635 0.4959 0.139 Uiso 1 1 calc R . . H32B H 0.2672 0.7649 0.4861 0.139 Uiso 1 1 calc R . . H32C H 0.3433 0.7804 0.4329 0.139 Uiso 1 1 calc R . . C33A C 0.1308(7) 0.5278(6) 0.3733(6) 0.102(3) Uani 1 1 d . . . H33A H 0.1465 0.4797 0.3611 0.153 Uiso 1 1 calc R . . H33B H 0.0869 0.5361 0.3387 0.153 Uiso 1 1 calc R . . H33C H 0.0939 0.5399 0.4148 0.153 Uiso 1 1 calc R . . C34A C 0.5111(19) 0.6541(13) 0.5646(8) 0.192(9) Uani 1 1 d . . . H34A H 0.4826 0.6875 0.5447 0.23 Uiso 1 1 calc R . . H34B H 0.5136 0.6757 0.6128 0.23 Uiso 1 1 calc R . . C35A C 0.4373(15) 0.5991(17) 0.5518(12) 0.248(15) Uani 1 1 d . . . H35A H 0.391 0.6056 0.5892 0.372 Uiso 1 1 calc R . . H35B H 0.4735 0.5569 0.5454 0.372 Uiso 1 1 calc R . . H35C H 0.3963 0.5968 0.512 0.372 Uiso 1 1 calc R . . C36A C 0.6688(14) 0.6121(10) 0.5780(10) 0.161(7) Uani 1 1 d . . . H36A H 0.7149 0.5815 0.547 0.193 Uiso 1 1 calc R . . H36B H 0.6226 0.5843 0.5976 0.193 Uiso 1 1 calc R . . C37A C 0.7347(15) 0.6631(10) 0.6324(8) 0.160(6) Uani 1 1 d . . . H37A H 0.7732 0.6388 0.6577 0.24 Uiso 1 1 calc R . . H37B H 0.6891 0.6949 0.6616 0.24 Uiso 1 1 calc R . . H37C H 0.784 0.6882 0.6125 0.24 Uiso 1 1 calc R . . C38A C 1.0444(13) 0.7445(17) 0.3610(10) 0.220(13) Uani 1 1 d . . . H38A H 1.0915 0.772 0.3414 0.264 Uiso 1 1 calc R . . H38B H 1.0854 0.7079 0.3688 0.264 Uiso 1 1 calc R . . C39A C 1.0118(12) 0.7875(8) 0.4241(11) 0.153(6) Uani 1 1 d . . . H39A H 1.0734 0.8075 0.4516 0.229 Uiso 1 1 calc R . . H39B H 0.97 0.7603 0.4459 0.229 Uiso 1 1 calc R . . H39C H 0.9701 0.8237 0.4173 0.229 Uiso 1 1 calc R . . C40A C 1.0009(15) 0.6637(11) 0.2616(10) 0.161(7) Uani 1 1 d . . . H40A H 1.0462 0.6844 0.2348 0.193 Uiso 1 1 calc R . . H40B H 1.0431 0.6324 0.2775 0.193 Uiso 1 1 calc R . . C41A C 0.9240(17) 0.6288(10) 0.2240(15) 0.28(2) Uani 1 1 d . . . H41A H 0.9466 0.5834 0.2008 0.416 Uiso 1 1 calc R . . H41B H 0.9034 0.6519 0.192 0.416 Uiso 1 1 calc R . . H41C H 0.8646 0.625 0.2513 0.416 Uiso 1 1 calc R . . C42A C 0.442(3) 0.9143(13) 0.371(2) 0.267(16) Uani 1 1 d . . . H42A H 0.4659 0.9392 0.3403 0.32 Uiso 1 1 calc R . . H42B H 0.3686 0.9242 0.3811 0.32 Uiso 1 1 calc R . . C43A C 0.500(4) 0.9349(18) 0.4262(19) 0.37(3) Uani 1 1 d U . . H43A H 0.4567 0.9342 0.4637 0.549 Uiso 1 1 calc R . . H43B H 0.5278 0.9812 0.4321 0.549 Uiso 1 1 calc R . . H43C H 0.5575 0.9046 0.4236 0.549 Uiso 1 1 calc R . . C44A C 0.3724(15) 0.8244(10) 0.2930(10) 0.174(8) Uani 1 1 d . . . H44A H 0.3884 0.8427 0.256 0.209 Uiso 1 1 calc R . . H44B H 0.3042 0.8409 0.3106 0.209 Uiso 1 1 calc R . . C45A C 0.3679(12) 0.7514(7) 0.2703(5) 0.132(5) Uani 1 1 d . . . H45A H 0.3111 0.7354 0.2375 0.197 Uiso 1 1 calc R . . H45B H 0.3555 0.7336 0.3076 0.197 Uiso 1 1 calc R . . H45C H 0.4341 0.7355 0.2503 0.197 Uiso 1 1 calc R . . Na1B Na 0.9016(2) 0.17318(12) 0.93339(11) 0.0524(6) Uani 1 1 d . A . Na2B Na 0.76921(18) 0.15161(12) 1.05591(12) 0.0499(5) Uani 1 1 d . . . Na3B Na 0.89340(18) 0.29430(12) 1.07075(12) 0.0498(5) Uani 1 1 d . A . N1B N 0.6400(4) 0.2700(2) 0.9724(2) 0.0415(10) Uani 1 1 d . . . O1B O 0.8612(3) 0.2833(2) 0.9639(2) 0.0494(9) Uani 1 1 d . . . O2B O 0.7359(3) 0.1390(2) 0.9481(2) 0.0541(10) Uani 1 1 d . . . O3B O 0.7343(3) 0.2639(2) 1.0932(2) 0.0509(9) Uani 1 1 d . . . O4B O 0.9445(3) 0.1794(2) 1.0435(2) 0.0496(9) Uani 1 1 d . A . O5B O 0.9877(5) 0.1199(3) 0.8330(3) 0.0807(16) Uani 1 1 d . . . O6B O 0.7081(4) 0.0447(3) 1.0632(3) 0.0723(14) Uani 1 1 d . . . O7B O 0.9681(6) 0.3782(4) 1.1569(3) 0.0949(19) Uani 1 1 d . . . Cl1B Cl 1.13252(15) 0.20737(11) 0.97852(9) 0.0713(5) Uani 1 1 d . . . Cl2B Cl 1.33743(14) 0.20746(12) 1.05812(11) 0.0801(6) Uani 1 1 d . A . Cl3B Cl 1.32959(15) 0.18243(12) 1.19639(12) 0.0799(6) Uani 1 1 d . . . Cl4B Cl 1.11635(16) 0.15288(12) 1.25095(10) 0.0757(5) Uani 1 1 d . A . Cl5B Cl 0.91149(13) 0.15043(11) 1.16945(9) 0.0667(5) Uani 1 1 d . . . C1B C 0.6598(5) 0.2805(3) 0.9064(3) 0.0488(13) Uani 1 1 d . . . H1B1 H 0.6811 0.2373 0.8755 0.059 Uiso 1 1 calc R . . H1B2 H 0.5941 0.2928 0.8889 0.059 Uiso 1 1 calc R . . C2B C 0.5545(5) 0.2164(3) 0.9679(3) 0.0506(13) Uani 1 1 d . . . H2B1 H 0.5533 0.2052 1.01 0.061 Uiso 1 1 calc R . . H2B2 H 0.4869 0.2357 0.9623 0.061 Uiso 1 1 calc R . . C3B C 0.6164(5) 0.3362(3) 1.0227(3) 0.0482(13) Uani 1 1 d . . . H3B1 H 0.6784 0.3676 1.029 0.058 Uiso 1 1 calc R . . H3B2 H 0.5587 0.357 1.0055 0.058 Uiso 1 1 calc R . . C4B C 1.0288(5) 0.1779(3) 1.0762(3) 0.0444(12) Uani 1 1 d . . . C5B C 1.1294(5) 0.1912(3) 1.0537(3) 0.0496(13) Uani 1 1 d . A . C6B C 1.2204(5) 0.1915(3) 1.0899(3) 0.0541(14) Uani 1 1 d . . . C7B C 1.2178(5) 0.1796(3) 1.1502(4) 0.0566(15) Uani 1 1 d . A . C8B C 1.1206(5) 0.1663(3) 1.1748(3) 0.0528(14) Uani 1 1 d . . . C9B C 1.0313(5) 0.1650(3) 1.1381(3) 0.0484(13) Uani 1 1 d . A . C10B C 0.7426(4) 0.3349(3) 0.9094(2) 0.0425(12) Uani 1 1 d . . . C11B C 0.8422(5) 0.3315(3) 0.9377(3) 0.0454(12) Uani 1 1 d . . . C12B C 0.9189(5) 0.3837(3) 0.9376(3) 0.0515(14) Uani 1 1 d . . . C13B C 0.8934(6) 0.4343(3) 0.9097(3) 0.0584(16) Uani 1 1 d . . . H13B H 0.945 0.4687 0.9101 0.07 Uiso 1 1 calc R . . C14B C 0.7968(6) 0.4372(3) 0.8812(3) 0.0577(16) Uani 1 1 d . . . C15B C 0.7215(5) 0.3875(3) 0.8819(3) 0.0503(14) Uani 1 1 d . . . H15B H 0.6542 0.389 0.8635 0.06 Uiso 1 1 calc R . . C16B C 1.0248(6) 0.3808(4) 0.9669(4) 0.071(2) Uani 1 1 d . . . H16D H 1.0533 0.3365 0.946 0.107 Uiso 1 1 calc R . . H16E H 1.0192 0.3874 1.0143 0.107 Uiso 1 1 calc R . . H16F H 1.071 0.4166 0.9597 0.107 Uiso 1 1 calc R . . C17B C 0.7719(8) 0.4933(4) 0.8504(4) 0.080(2) Uani 1 1 d . . . H17D H 0.8147 0.5343 0.8722 0.12 Uiso 1 1 calc R . . H17E H 0.698 0.5032 0.8559 0.12 Uiso 1 1 calc R . . H17F H 0.787 0.4783 0.8034 0.12 Uiso 1 1 calc R . . C18B C 0.5644(5) 0.1517(3) 0.9128(3) 0.0519(14) Uani 1 1 d . . . C19B C 0.6566(5) 0.1155(3) 0.9076(3) 0.0505(13) Uani 1 1 d . . . C20B C 0.6588(7) 0.0538(4) 0.8553(4) 0.0680(19) Uani 1 1 d . . . C21B C 0.5731(8) 0.0330(4) 0.8143(5) 0.087(3) Uani 1 1 d . . . H21B H 0.5758 -0.0088 0.7804 0.105 Uiso 1 1 calc R . . C22B C 0.4830(9) 0.0684(5) 0.8187(6) 0.104(3) Uani 1 1 d . . . C23B C 0.4806(6) 0.1284(4) 0.8701(4) 0.074(2) Uani 1 1 d . . . H23B H 0.4196 0.1538 0.8758 0.088 Uiso 1 1 calc R . . C24B C 0.7540(8) 0.0127(4) 0.8455(5) 0.083(2) Uani 1 1 d . . . H24D H 0.8149 0.0415 0.8423 0.125 Uiso 1 1 calc R . . H24E H 0.7454 -0.0251 0.8049 0.125 Uiso 1 1 calc R . . H24F H 0.764 -0.0051 0.8829 0.125 Uiso 1 1 calc R . . C25B C 0.3876(13) 0.0425(7) 0.7738(9) 0.170(8) Uani 1 1 d U . . H25D H 0.4028 -0.0002 0.7407 0.255 Uiso 1 1 calc R . . H25E H 0.3697 0.0762 0.7518 0.255 Uiso 1 1 calc R . . H25F H 0.3288 0.0348 0.8 0.255 Uiso 1 1 calc R . . C26B C 0.5867(5) 0.3284(3) 1.0887(3) 0.0430(12) Uani 1 1 d . . . C27B C 0.6516(5) 0.2944(3) 1.1215(3) 0.0443(12) Uani 1 1 d . . . C28B C 0.6225(5) 0.2935(3) 1.1855(3) 0.0485(13) Uani 1 1 d . . . C29B C 0.5307(5) 0.3217(3) 1.2113(3) 0.0510(14) Uani 1 1 d . . . H29B H 0.5124 0.3199 1.2539 0.061 Uiso 1 1 calc R . . C30B C 0.4643(5) 0.3523(3) 1.1785(3) 0.0492(13) Uani 1 1 d . . . C31B C 0.4947(5) 0.3564(3) 1.1168(3) 0.0489(13) Uani 1 1 d . . . H31B H 0.452 0.3786 1.0935 0.059 Uiso 1 1 calc R . . C32B C 0.6922(6) 0.2592(4) 1.2227(3) 0.0648(18) Uani 1 1 d . . . H32D H 0.7619 0.2814 1.2288 0.097 Uiso 1 1 calc R . . H32E H 0.6969 0.2113 1.1977 0.097 Uiso 1 1 calc R . . H32F H 0.6629 0.2626 1.2658 0.097 Uiso 1 1 calc R . . C33B C 0.3603(6) 0.3768(4) 1.2057(4) 0.069(2) Uani 1 1 d . . . H33D H 0.3096 0.3704 1.1694 0.104 Uiso 1 1 calc R . . H33E H 0.3677 0.425 1.2304 0.104 Uiso 1 1 calc R . . H33F H 0.3362 0.3509 1.235 0.104 Uiso 1 1 calc R . . C34B C 1.034(2) 0.0481(18) 0.8301(18) 0.149(13) Uani 0.58(3) 1 d PU A 1 H34C H 1.0417 0.0436 0.875 0.178 Uiso 0.58(3) 1 calc PR A 1 H34D H 0.9874 0.0105 0.8036 0.178 Uiso 0.58(3) 1 calc PR A 1 C35B C 1.122(4) 0.046(3) 0.804(3) 0.22(2) Uani 0.58(3) 1 d PU A 1 H35D H 1.1731 0.0287 0.8288 0.331 Uiso 0.58(3) 1 calc PR A 1 H35E H 1.1454 0.0922 0.8042 0.331 Uiso 0.58(3) 1 calc PR A 1 H35F H 1.1171 0.0168 0.7584 0.331 Uiso 0.58(3) 1 calc PR A 1 C34D C 1.0827(16) 0.0858(9) 0.8200(8) 0.053(6) Uani 0.42(3) 1 d P A 2 H34E H 1.1191 0.0881 0.8619 0.064 Uiso 0.42(3) 1 calc PR A 2 H34F H 1.1286 0.1082 0.7948 0.064 Uiso 0.42(3) 1 calc PR A 2 C35D C 1.0589(18) 0.0107(10) 0.7797(15) 0.082(9) Uani 0.42(3) 1 d P A 2 H35G H 1.1236 -0.01 0.7616 0.124 Uiso 0.42(3) 1 calc PR A 2 H35H H 1.0094 0.0087 0.7436 0.124 Uiso 0.42(3) 1 calc PR A 2 H35I H 1.0286 -0.014 0.8084 0.124 Uiso 0.42(3) 1 calc PR A 2 C36B C 0.9591(10) 0.1367(7) 0.7753(5) 0.109(4) Uani 1 1 d . A . H36C H 0.9407 0.0948 0.7392 0.131 Uiso 1 1 calc R . . H36D H 1.0185 0.1606 0.7612 0.131 Uiso 1 1 calc R . . C37B C 0.8699(11) 0.1802(7) 0.7887(5) 0.123(5) Uani 1 1 d . . . H37D H 0.8429 0.1857 0.7473 0.185 Uiso 1 1 calc R A . H37E H 0.8918 0.2247 0.8187 0.185 Uiso 1 1 calc R . . H37F H 0.8152 0.1594 0.809 0.185 Uiso 1 1 calc R . . C38B C 0.7563(10) -0.0155(5) 1.0275(8) 0.126(5) Uani 1 1 d . . . H38C H 0.722 -0.0337 0.9835 0.151 Uiso 1 1 calc R . . H38D H 0.7473 -0.0501 1.0509 0.151 Uiso 1 1 calc R . . C39B C 0.8670(10) -0.0025(5) 1.0200(8) 0.125(5) Uani 1 1 d . . . H39D H 0.9018 -0.0456 1.0063 0.188 Uiso 1 1 calc R . . H39E H 0.8974 0.0258 1.0621 0.188 Uiso 1 1 calc R . . H39F H 0.8761 0.0211 0.9866 0.188 Uiso 1 1 calc R . . C40B C 0.6012(9) 0.0355(7) 1.0699(10) 0.144(6) Uani 1 1 d . . . H40C H 0.5686 0.0155 1.0256 0.173 Uiso 1 1 calc R . . H40D H 0.5897 0.0025 1.0949 0.173 Uiso 1 1 calc R . . C41B C 0.5510(9) 0.0946(7) 1.1015(9) 0.139(6) Uani 1 1 d . . . H41D H 0.4764 0.0838 1.1038 0.209 Uiso 1 1 calc R . . H41E H 0.5606 0.1275 1.0767 0.209 Uiso 1 1 calc R . . H41F H 0.5806 0.1139 1.1461 0.209 Uiso 1 1 calc R . . C42B C 1.0585(9) 0.3596(7) 1.1981(6) 0.108(3) Uani 1 1 d . . . H42C H 1.097 0.3218 1.1695 0.13 Uiso 1 1 calc R . . H42D H 1.1079 0.3992 1.2147 0.13 Uiso 1 1 calc R . . C43B C 1.0184(12) 0.3406(8) 1.2509(9) 0.146(6) Uani 1 1 d . . . H43D H 1.0749 0.3257 1.274 0.22 Uiso 1 1 calc R . . H43E H 0.966 0.3034 1.2346 0.22 Uiso 1 1 calc R . . H43F H 0.9861 0.3794 1.2813 0.22 Uiso 1 1 calc R . . C44B C 0.9269(9) 0.4398(9) 1.1788(5) 0.126(5) Uani 1 1 d . . . H44C H 0.9826 0.4755 1.1834 0.151 Uiso 1 1 calc R . . H44D H 0.8974 0.4453 1.2228 0.151 Uiso 1 1 calc R . . C45B C 0.8409(8) 0.4483(5) 1.1312(6) 0.104(4) Uani 1 1 d . . . H45D H 0.8136 0.4937 1.1477 0.157 Uiso 1 1 calc R . . H45E H 0.7845 0.4141 1.128 0.157 Uiso 1 1 calc R . . H45F H 0.8699 0.4425 1.0876 0.157 Uiso 1 1 calc R . . O1C O 0.787(2) 0.1646(9) 0.3738(8) 0.264(11) Uani 1 1 d D . . C1C C 0.705(3) 0.1368(14) 0.3349(11) 0.235(16) Uani 1 1 d . . . H1C1 H 0.7169 0.0876 0.3202 0.282 Uiso 1 1 calc R . . H1C2 H 0.7132 0.1524 0.2955 0.282 Uiso 1 1 calc R . . C2C C 0.596(4) 0.1405(17) 0.3474(17) 0.35(3) Uani 1 1 d U . . H2C1 H 0.557 0.1098 0.3099 0.521 Uiso 1 1 calc R . . H2C2 H 0.5752 0.1871 0.3538 0.521 Uiso 1 1 calc R . . H2C3 H 0.5818 0.1273 0.3871 0.521 Uiso 1 1 calc R . . C3C C 0.889(2) 0.1645(14) 0.3619(11) 0.194(10) Uani 1 1 d D . . H3C1 H 0.8951 0.1826 0.3239 0.233 Uiso 1 1 calc R . . H3C2 H 0.904 0.1159 0.3451 0.233 Uiso 1 1 calc R . . C4C C 0.977(2) 0.1956(13) 0.4053(10) 0.33(2) Uani 1 1 d U . . H4C1 H 1.041 0.1897 0.38 0.493 Uiso 1 1 calc R . . H4C2 H 0.9833 0.1739 0.4404 0.493 Uiso 1 1 calc R . . H4C3 H 0.9666 0.2441 0.4249 0.493 Uiso 1 1 calc R . . H1A H 0.6038 0.6103 0.3276 0.018(11) Uiso 1 1 d R . . H1B H 0.6903 0.2531 0.9858 0.015(10) Uiso 1 1 d 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 Na1A 0.0707(18) 0.0674(17) 0.0699(17) 0.0070(14) 0.0121(14) -0.0131(14) Na2A 0.0841(19) 0.0647(16) 0.0445(13) 0.0170(12) -0.0091(12) -0.0120(14) Na3A 0.0849(19) 0.0652(17) 0.0479(14) 0.0083(12) -0.0094(13) 0.0056(14) O1A 0.102(4) 0.056(3) 0.038(2) 0.0085(19) 0.007(2) -0.010(3) O2A 0.071(3) 0.060(3) 0.073(3) 0.016(2) -0.005(2) 0.002(2) O3A 0.064(3) 0.069(3) 0.059(3) 0.008(2) 0.010(2) -0.006(2) O4A 0.082(3) 0.054(3) 0.047(2) 0.008(2) -0.006(2) -0.011(2) O5A 0.081(4) 0.100(5) 0.177(8) 0.050(6) 0.023(5) -0.014(4) O6A 0.118(6) 0.128(6) 0.099(5) 0.074(5) 0.020(4) 0.012(5) O7A 0.116(6) 0.103(6) 0.162(8) 0.040(6) -0.031(6) 0.021(5) Cl1A 0.249(4) 0.0866(16) 0.0512(11) 0.0243(11) 0.0012(16) -0.030(2) Cl2A 0.447(9) 0.093(2) 0.105(2) 0.0358(19) 0.025(4) -0.101(4) Cl3A 0.297(6) 0.0791(18) 0.106(2) 0.0004(16) -0.019(3) -0.078(3) Cl4A 0.280(5) 0.0901(17) 0.0495(11) 0.0109(11) -0.0357(18) -0.041(2) Cl5A 0.290(5) 0.0810(16) 0.0536(11) 0.0173(11) 0.0124(18) -0.060(2) N1A 0.044(2) 0.055(3) 0.034(2) 0.015(2) -0.0002(18) 0.000(2) C1A 0.055(3) 0.066(4) 0.044(3) 0.021(3) -0.004(3) -0.004(3) C2A 0.054(3) 0.065(4) 0.044(3) 0.018(3) 0.010(3) 0.007(3) C3A 0.059(4) 0.067(4) 0.055(3) 0.030(3) 0.012(3) -0.001(3) C4A 0.076(4) 0.047(3) 0.048(3) 0.014(3) -0.004(3) -0.005(3) C5A 0.119(7) 0.052(4) 0.053(4) 0.020(3) -0.006(4) -0.006(4) C6A 0.168(10) 0.068(5) 0.067(5) 0.029(4) -0.011(6) -0.032(6) C7A 0.142(9) 0.055(4) 0.067(5) 0.010(4) -0.015(5) -0.024(5) C8A 0.143(8) 0.064(5) 0.048(4) 0.015(3) -0.018(4) -0.009(5) C9A 0.100(6) 0.064(4) 0.049(4) 0.013(3) -0.005(4) -0.012(4) C10A 0.066(4) 0.063(4) 0.040(3) 0.018(3) 0.008(3) 0.007(3) C11A 0.077(4) 0.058(4) 0.037(3) 0.012(3) 0.004(3) -0.007(3) C12A 0.082(5) 0.060(4) 0.044(3) 0.018(3) 0.007(3) -0.009(3) C13A 0.077(5) 0.078(5) 0.045(3) 0.030(3) 0.009(3) 0.000(4) C14A 0.063(4) 0.074(4) 0.035(3) 0.012(3) 0.006(3) 0.004(3) C15A 0.068(4) 0.062(4) 0.040(3) 0.014(3) -0.006(3) -0.003(3) C16A 0.123(7) 0.082(6) 0.060(4) 0.030(4) 0.009(5) -0.029(5) C17A 0.106(6) 0.099(6) 0.037(3) 0.014(4) 0.011(4) 0.011(5) C18A 0.049(3) 0.068(4) 0.051(3) 0.024(3) 0.003(3) 0.007(3) C19A 0.058(4) 0.064(4) 0.053(3) 0.018(3) 0.004(3) 0.003(3) C20A 0.044(3) 0.075(4) 0.047(3) 0.011(3) -0.001(3) -0.002(3) C21A 0.054(4) 0.080(5) 0.063(4) 0.028(4) -0.006(3) 0.007(3) C22A 0.061(4) 0.070(5) 0.070(4) 0.024(4) -0.011(3) 0.008(3) C23A 0.062(4) 0.066(4) 0.062(4) 0.022(3) -0.010(3) 0.000(3) C24A 0.076(5) 0.084(6) 0.074(5) 0.012(4) -0.021(4) -0.003(4) C25A 0.106(7) 0.082(6) 0.106(7) 0.042(5) -0.025(6) 0.019(5) C26A 0.054(3) 0.076(5) 0.049(3) 0.023(3) 0.011(3) -0.003(3) C27A 0.051(3) 0.074(4) 0.043(3) 0.011(3) 0.007(3) 0.001(3) C28A 0.058(4) 0.081(5) 0.046(3) 0.013(3) 0.008(3) 0.012(3) C29A 0.052(4) 0.101(6) 0.054(4) 0.021(4) 0.016(3) 0.010(4) C30A 0.050(4) 0.095(6) 0.064(4) 0.021(4) 0.015(3) 0.003(4) C31A 0.065(4) 0.075(5) 0.063(4) 0.022(4) 0.015(3) 0.001(4) C32A 0.087(6) 0.105(7) 0.074(5) 0.005(5) 0.014(5) 0.014(5) C33A 0.055(5) 0.121(8) 0.125(8) 0.028(7) 0.026(5) -0.006(5) C34A 0.22(2) 0.29(3) 0.116(11) 0.137(16) 0.027(13) 0.03(2) C35A 0.137(14) 0.45(4) 0.26(3) 0.28(3) 0.003(15) -0.05(2) C36A 0.143(13) 0.202(18) 0.178(16) 0.124(15) -0.004(12) -0.022(12) C37A 0.190(16) 0.208(18) 0.110(10) 0.094(12) -0.010(10) -0.017(14) C38A 0.103(11) 0.46(4) 0.151(15) 0.17(2) 0.009(11) 0.082(18) C39A 0.113(10) 0.116(10) 0.24(2) 0.077(12) -0.029(12) -0.043(8) C40A 0.158(15) 0.167(16) 0.184(17) 0.081(14) 0.082(14) 0.074(13) C41A 0.176(18) 0.142(15) 0.39(4) -0.12(2) 0.18(2) -0.056(13) C42A 0.30(4) 0.133(19) 0.37(5) 0.07(2) -0.05(3) 0.06(2) C43A 0.46(6) 0.25(3) 0.27(4) -0.12(3) -0.08(3) 0.13(4) C44A 0.162(14) 0.172(17) 0.202(18) 0.084(15) -0.093(13) -0.019(12) C45A 0.188(13) 0.131(10) 0.063(5) 0.002(6) -0.034(7) 0.080(10) Na1B 0.0617(14) 0.0507(13) 0.0461(12) 0.0159(10) 0.0066(10) 0.0063(11) Na2B 0.0515(13) 0.0478(12) 0.0559(13) 0.0234(10) 0.0070(10) 0.0031(10) Na3B 0.0498(12) 0.0488(13) 0.0537(13) 0.0196(10) 0.0016(10) 0.0030(10) N1B 0.047(2) 0.041(2) 0.039(2) 0.0157(19) 0.0046(19) 0.004(2) O1B 0.055(2) 0.045(2) 0.055(2) 0.0254(19) 0.0019(18) 0.0034(18) O2B 0.058(2) 0.051(2) 0.052(2) 0.0138(19) 0.0007(19) -0.0012(19) O3B 0.048(2) 0.053(2) 0.052(2) 0.0154(19) 0.0103(18) 0.0069(18) O4B 0.051(2) 0.057(2) 0.049(2) 0.0270(19) 0.0038(18) 0.0047(18) O5B 0.089(4) 0.097(4) 0.053(3) 0.014(3) 0.006(3) 0.032(3) O6B 0.081(3) 0.057(3) 0.085(4) 0.031(3) 0.004(3) -0.007(3) O7B 0.106(5) 0.095(5) 0.076(4) 0.018(4) -0.020(3) -0.031(4) Cl1B 0.0671(10) 0.0963(14) 0.0632(10) 0.0425(10) 0.0147(8) 0.0012(9) Cl2B 0.0519(9) 0.0979(15) 0.0917(14) 0.0311(12) 0.0164(9) -0.0113(9) Cl3B 0.0575(10) 0.0936(14) 0.0905(14) 0.0316(12) -0.0149(9) -0.0020(9) Cl4B 0.0740(11) 0.1026(15) 0.0653(10) 0.0470(11) -0.0021(9) 0.0099(10) Cl5B 0.0509(8) 0.0983(13) 0.0681(10) 0.0504(10) 0.0115(7) 0.0068(8) C1B 0.059(3) 0.055(3) 0.037(3) 0.020(2) 0.002(2) -0.003(3) C2B 0.045(3) 0.056(3) 0.052(3) 0.019(3) -0.001(2) -0.009(3) C3B 0.062(3) 0.041(3) 0.044(3) 0.014(2) 0.012(3) 0.007(3) C4B 0.050(3) 0.041(3) 0.045(3) 0.017(2) 0.005(2) 0.006(2) C5B 0.057(3) 0.042(3) 0.053(3) 0.019(3) 0.012(3) 0.003(3) C6B 0.052(3) 0.048(3) 0.061(4) 0.015(3) 0.008(3) -0.001(3) C7B 0.049(3) 0.047(3) 0.073(4) 0.017(3) 0.007(3) 0.001(3) C8B 0.054(3) 0.057(4) 0.054(3) 0.026(3) 0.004(3) 0.010(3) C9B 0.046(3) 0.044(3) 0.059(3) 0.020(3) 0.012(3) 0.004(2) C10B 0.052(3) 0.045(3) 0.034(2) 0.017(2) 0.003(2) 0.000(2) C11B 0.055(3) 0.044(3) 0.040(3) 0.016(2) 0.010(2) 0.001(2) C12B 0.054(3) 0.048(3) 0.055(3) 0.019(3) 0.010(3) -0.002(3) C13B 0.069(4) 0.052(4) 0.061(4) 0.028(3) 0.016(3) -0.002(3) C14B 0.074(4) 0.053(4) 0.057(4) 0.032(3) 0.016(3) 0.012(3) C15B 0.062(4) 0.055(3) 0.041(3) 0.023(3) 0.008(3) 0.011(3) C16B 0.057(4) 0.072(5) 0.093(5) 0.041(4) -0.002(4) -0.014(3) C17B 0.102(6) 0.075(5) 0.085(5) 0.055(5) 0.018(5) 0.014(5) C18B 0.058(4) 0.045(3) 0.050(3) 0.012(3) -0.003(3) -0.012(3) C19B 0.061(4) 0.041(3) 0.050(3) 0.017(2) 0.001(3) -0.009(3) C20B 0.084(5) 0.054(4) 0.064(4) 0.014(3) 0.006(4) -0.012(4) C21B 0.112(7) 0.050(4) 0.081(5) -0.008(4) -0.006(5) -0.017(4) C22B 0.096(7) 0.060(5) 0.133(9) -0.002(5) -0.042(6) -0.012(5) C23B 0.068(4) 0.056(4) 0.092(6) 0.015(4) -0.023(4) -0.009(3) C24B 0.110(7) 0.055(4) 0.076(5) 0.006(4) 0.012(5) 0.010(4) C25B 0.162(13) 0.111(10) 0.178(14) -0.044(9) -0.103(11) -0.004(9) C26B 0.052(3) 0.035(3) 0.042(3) 0.012(2) 0.005(2) 0.000(2) C27B 0.050(3) 0.037(3) 0.045(3) 0.010(2) 0.007(2) 0.003(2) C28B 0.055(3) 0.046(3) 0.045(3) 0.014(2) 0.003(2) 0.006(3) C29B 0.062(4) 0.053(3) 0.040(3) 0.015(3) 0.013(3) 0.008(3) C30B 0.053(3) 0.045(3) 0.049(3) 0.012(2) 0.010(3) 0.002(3) C31B 0.055(3) 0.041(3) 0.054(3) 0.019(3) 0.010(3) 0.008(2) C32B 0.071(4) 0.078(5) 0.050(3) 0.025(3) 0.004(3) 0.016(4) C33B 0.072(4) 0.071(5) 0.076(5) 0.036(4) 0.031(4) 0.023(4) C34B 0.117(19) 0.15(3) 0.18(3) 0.05(2) 0.041(17) 0.063(18) C35B 0.25(5) 0.21(5) 0.24(5) 0.11(4) 0.12(4) 0.02(4) C34D 0.064(11) 0.045(10) 0.048(8) 0.009(7) 0.019(7) 0.007(7) C35D 0.062(12) 0.042(11) 0.13(2) 0.004(11) 0.002(12) 0.001(8) C36B 0.118(8) 0.148(10) 0.060(5) 0.026(6) 0.010(5) 0.026(8) C37B 0.150(10) 0.170(12) 0.069(6) 0.056(7) 0.012(6) 0.077(9) C38B 0.124(10) 0.056(5) 0.188(14) 0.024(7) 0.019(9) -0.010(6) C39B 0.126(10) 0.063(6) 0.179(13) 0.020(7) 0.041(9) 0.021(6) C40B 0.069(6) 0.120(10) 0.246(19) 0.061(11) 0.004(9) -0.014(7) C41B 0.077(7) 0.114(10) 0.230(17) 0.052(10) 0.048(9) 0.016(7) C42B 0.091(7) 0.132(10) 0.090(7) 0.022(7) -0.014(6) -0.019(7) C43B 0.127(11) 0.130(11) 0.202(17) 0.084(12) -0.042(11) -0.029(9) C44B 0.087(7) 0.184(14) 0.073(6) -0.008(7) 0.011(5) -0.050(8) C45B 0.075(6) 0.082(6) 0.124(8) -0.019(6) 0.025(6) -0.007(5) O1C 0.38(3) 0.216(16) 0.140(12) -0.037(11) 0.113(17) -0.061(18) C1C 0.39(5) 0.18(2) 0.125(16) 0.038(15) -0.09(2) -0.10(3) C2C 0.45(5) 0.23(3) 0.26(3) -0.09(2) 0.19(4) -0.08(3) C3C 0.25(3) 0.23(2) 0.123(15) 0.066(16) 0.015(17) 0.08(2) C4C 0.42(5) 0.40(5) 0.114(15) 0.02(2) 0.02(2) -0.18(4) #----------------------------------------------------------------------------# # 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 Na1A O2A 2.202(6) . ? Na1A O1A 2.290(7) . ? Na1A O5A 2.354(8) . ? Na1A O4A 2.388(6) . ? Na1A Na3A 3.134(4) . ? Na1A Cl1A 3.171(4) . ? Na1A Na2A 3.300(4) . ? Na2A O3A 2.221(6) . ? Na2A O2A 2.289(6) . ? Na2A O6A 2.329(7) . ? Na2A O4A 2.360(5) . ? Na2A Cl5A 2.920(4) . ? Na2A C19A 3.118(8) . ? Na2A Na3A 3.233(4) . ? Na3A O1A 2.206(5) . ? Na3A O3A 2.250(6) . ? Na3A O7A 2.323(8) . ? Na3A O4A 2.341(6) . ? O1A C11A 1.320(7) . ? O2A C19A 1.313(9) . ? O3A C27A 1.322(8) . ? O4A C4A 1.282(8) . ? O5A C38A 1.35(2) . ? O5A C40A 1.422(19) . ? O6A C36A 1.349(17) . ? O6A C34A 1.35(2) . ? O7A C42A 1.36(3) . ? O7A C44A 1.418(17) . ? Cl1A C5A 1.720(8) . ? Cl2A C6A 1.716(9) . ? Cl3A C7A 1.734(9) . ? Cl4A C8A 1.743(8) . ? Cl5A C9A 1.731(8) . ? N1A C3A 1.508(7) . ? N1A C2A 1.513(8) . ? N1A C1A 1.518(7) . ? N1A H1A 0.8999 . ? C1A C10A 1.508(8) . ? C1A H1A1 0.99 . ? C1A H1A2 0.99 . ? C2A C18A 1.517(9) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C3A C26A 1.515(9) . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C4A C5A 1.415(10) . ? C4A C9A 1.428(9) . ? C5A C6A 1.379(12) . ? C6A C7A 1.380(12) . ? C7A C8A 1.378(12) . ? C8A C9A 1.366(11) . ? C10A C15A 1.393(9) . ? C10A C11A 1.402(10) . ? C11A C12A 1.418(8) . ? C12A C13A 1.405(10) . ? C12A C16A 1.507(11) . ? C13A C14A 1.384(11) . ? C13A H13A 0.95 . ? C14A C15A 1.383(9) . ? C14A C17A 1.504(9) . ? C15A H15A 0.95 . ? C16A H16A 0.98 . ? C16A H16B 0.98 . ? C16A H16C 0.98 . ? C17A H17A 0.98 . ? C17A H17B 0.98 . ? C17A H17C 0.98 . ? C18A C23A 1.409(10) . ? C18A C19A 1.411(10) . ? C19A C20A 1.427(10) . ? C20A C21A 1.379(11) . ? C20A C24A 1.524(11) . ? C21A C22A 1.387(11) . ? C21A H21A 0.95 . ? C22A C23A 1.400(10) . ? C22A C25A 1.538(12) . ? C23A H23A 0.95 . ? C24A H24A 0.98 . ? C24A H24B 0.98 . ? C24A H24C 0.98 . ? C25A H25A 0.98 . ? C25A H25B 0.98 . ? C25A H25C 0.98 . ? C26A C27A 1.406(10) . ? C26A C31A 1.407(10) . ? C27A C28A 1.429(9) . ? C28A C29A 1.382(11) . ? C28A C32A 1.512(13) . ? C29A C30A 1.386(12) . ? C29A H29A 0.95 . ? C30A C31A 1.382(10) . ? C30A C33A 1.514(12) . ? C31A H31A 0.95 . ? C32A H32A 0.98 . ? C32A H32B 0.98 . ? C32A H32C 0.98 . ? C33A H33A 0.98 . ? C33A H33B 0.98 . ? C33A H33C 0.98 . ? C34A C35A 1.41(3) . ? C34A H34A 0.99 . ? C34A H34B 0.99 . ? C35A H35A 0.98 . ? C35A H35B 0.98 . ? C35A H35C 0.98 . ? C36A C37A 1.53(2) . ? C36A H36A 0.99 . ? C36A H36B 0.99 . ? C37A H37A 0.98 . ? C37A H37B 0.98 . ? C37A H37C 0.98 . ? C38A C39A 1.45(3) . ? C38A H38A 0.99 . ? C38A H38B 0.99 . ? C39A H39A 0.98 . ? C39A H39B 0.98 . ? C39A H39C 0.98 . ? C40A C41A 1.31(3) . ? C40A H40A 0.99 . ? C40A H40B 0.99 . ? C41A H41A 0.98 . ? C41A H41B 0.98 . ? C41A H41C 0.98 . ? C42A C43A 1.32(4) . ? C42A H42A 0.99 . ? C42A H42B 0.99 . ? C43A H43A 0.98 . ? C43A H43B 0.98 . ? C43A H43C 0.98 . ? C44A C45A 1.44(2) . ? C44A H44A 0.99 . ? C44A H44B 0.99 . ? C45A H45A 0.98 . ? C45A H45B 0.98 . ? C45A H45C 0.98 . ? Na1B O1B 2.256(5) . ? Na1B O2B 2.274(5) . ? Na1B O4B 2.364(5) . ? Na1B O5B 2.401(6) . ? Na1B Cl1B 3.096(3) . ? Na1B Na3B 3.244(3) . ? Na1B Na2B 3.262(3) . ? Na2B O2B 2.264(5) . ? Na2B O3B 2.284(5) . ? Na2B O4B 2.341(5) . ? Na2B O6B 2.364(5) . ? Na2B Cl5B 3.017(3) . ? Na2B Na3B 3.227(3) . ? Na3B O3B 2.215(5) . ? Na3B O1B 2.247(5) . ? Na3B O7B 2.288(7) . ? Na3B O4B 2.391(5) . ? Na3B C4B 3.050(6) . ? N1B C1B 1.506(6) . ? N1B C2B 1.511(7) . ? N1B C3B 1.513(7) . ? N1B H1B 0.8319 . ? O1B C11B 1.309(7) . ? O2B C19B 1.306(8) . ? O3B C27B 1.317(7) . ? O4B C4B 1.287(7) . ? O5B C36B 1.421(11) . ? O5B C34D 1.422(19) . ? O5B C34B 1.60(3) . ? O6B C40B 1.395(12) . ? O6B C38B 1.422(12) . ? O7B C44B 1.351(17) . ? O7B C42B 1.571(14) . ? Cl1B C5B 1.730(6) . ? Cl2B C6B 1.717(6) . ? Cl3B C7B 1.719(7) . ? Cl4B C8B 1.724(6) . ? Cl5B C9B 1.736(6) . ? C1B C10B 1.505(8) . ? C1B H1B1 0.99 . ? C1B H1B2 0.99 . ? C2B C18B 1.506(9) . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C3B C26B 1.511(7) . ? C3B H3B1 0.99 . ? C3B H3B2 0.99 . ? C4B C9B 1.420(8) . ? C4B C5B 1.429(8) . ? C5B C6B 1.389(10) . ? C6B C7B 1.378(10) . ? C7B C8B 1.409(9) . ? C8B C9B 1.375(9) . ? C10B C15B 1.410(8) . ? C10B C11B 1.421(8) . ? C11B C12B 1.432(8) . ? C12B C13B 1.394(9) . ? C12B C16B 1.500(10) . ? C13B C14B 1.385(10) . ? C13B H13B 0.95 . ? C14B C15B 1.386(10) . ? C14B C17B 1.533(9) . ? C15B H15B 0.95 . ? C16B H16D 0.98 . ? C16B H16E 0.98 . ? C16B H16F 0.98 . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? C18B C23B 1.375(10) . ? C18B C19B 1.413(9) . ? C19B C20B 1.427(10) . ? C20B C21B 1.369(13) . ? C20B C24B 1.497(12) . ? C21B C22B 1.383(14) . ? C21B H21B 0.95 . ? C22B C23B 1.391(13) . ? C22B C25B 1.523(14) . ? C23B H23B 0.95 . ? C24B H24D 0.98 . ? C24B H24E 0.98 . ? C24B H24F 0.98 . ? C25B H25D 0.98 . ? C25B H25E 0.98 . ? C25B H25F 0.98 . ? C26B C31B 1.398(8) . ? C26B C27B 1.413(8) . ? C27B C28B 1.423(8) . ? C28B C29B 1.384(8) . ? C28B C32B 1.515(9) . ? C29B C30B 1.377(9) . ? C29B H29B 0.95 . ? C30B C31B 1.401(8) . ? C30B C33B 1.509(9) . ? C31B H31B 0.95 . ? C32B H32D 0.98 . ? C32B H32E 0.98 . ? C32B H32F 0.98 . ? C33B H33D 0.98 . ? C33B H33E 0.98 . ? C33B H33F 0.98 . ? C34B C35B 1.27(5) . ? C34B H34C 0.99 . ? C34B H34D 0.99 . ? C35B H35D 0.98 . ? C35B H35E 0.98 . ? C35B H35F 0.98 . ? C34D C35D 1.55(3) . ? C34D H34E 0.99 . ? C34D H34F 0.99 . ? C35D H35G 0.98 . ? C35D H35H 0.98 . ? C35D H35I 0.98 . ? C36B C37B 1.463(15) . ? C36B H36C 0.99 . ? C36B H36D 0.99 . ? C37B H37D 0.98 . ? C37B H37E 0.98 . ? C37B H37F 0.98 . ? C38B C39B 1.457(17) . ? C38B H38C 0.99 . ? C38B H38D 0.99 . ? C39B H39D 0.98 . ? C39B H39E 0.98 . ? C39B H39F 0.98 . ? C40B C41B 1.394(18) . ? C40B H40C 0.99 . ? C40B H40D 0.99 . ? C41B H41D 0.98 . ? C41B H41E 0.98 . ? C41B H41F 0.98 . ? C42B C43B 1.396(18) . ? C42B H42C 0.99 . ? C42B H42D 0.99 . ? C43B H43D 0.98 . ? C43B H43E 0.98 . ? C43B H43F 0.98 . ? C44B C45B 1.539(18) . ? C44B H44C 0.99 . ? C44B H44D 0.99 . ? C45B H45D 0.98 . ? C45B H45E 0.98 . ? C45B H45F 0.98 . ? O1C C3C 1.327(17) . ? O1C C1C 1.34(3) . ? C1C C2C 1.42(4) . ? C1C H1C1 0.99 . ? C1C H1C2 0.99 . ? C2C H2C1 0.98 . ? C2C H2C2 0.98 . ? C2C H2C3 0.98 . ? C3C C4C 1.46(3) . ? C3C H3C1 0.99 . ? C3C H3C2 0.99 . ? C4C H4C1 0.98 . ? C4C H4C2 0.98 . ? C4C H4C3 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 O2A Na1A O1A 94.7(2) . . ? O2A Na1A O5A 104.4(3) . . ? O1A Na1A O5A 134.5(3) . . ? O2A Na1A O4A 88.8(2) . . ? O1A Na1A O4A 92.6(2) . . ? O5A Na1A O4A 128.0(3) . . ? O2A Na1A Na3A 92.75(18) . . ? O1A Na1A Na3A 44.72(14) . . ? O5A Na1A Na3A 162.5(2) . . ? O4A Na1A Na3A 47.84(14) . . ? O2A Na1A Cl1A 149.93(19) . . ? O1A Na1A Cl1A 89.84(18) . . ? O5A Na1A Cl1A 93.0(2) . . ? O4A Na1A Cl1A 61.24(14) . . ? Na3A Na1A Cl1A 70.02(12) . . ? O2A Na1A Na2A 43.74(16) . . ? O1A Na1A Na2A 89.68(15) . . ? O5A Na1A Na2A 132.1(3) . . ? O4A Na1A Na2A 45.63(13) . . ? Na3A Na1A Na2A 60.26(9) . . ? Cl1A Na1A Na2A 106.75(11) . . ? O3A Na2A O2A 97.0(2) . . ? O3A Na2A O6A 101.8(3) . . ? O2A Na2A O6A 117.5(3) . . ? O3A Na2A O4A 90.0(2) . . ? O2A Na2A O4A 87.5(2) . . ? O6A Na2A O4A 150.2(3) . . ? O3A Na2A Cl5A 120.3(2) . . ? O2A Na2A Cl5A 132.8(2) . . ? O6A Na2A Cl5A 84.0(2) . . ? O4A Na2A Cl5A 66.50(14) . . ? O3A Na2A C19A 101.9(2) . . ? O2A Na2A C19A 21.98(18) . . ? O6A Na2A C19A 95.6(3) . . ? O4A Na2A C19A 108.8(2) . . ? Cl5A Na2A C19A 137.1(2) . . ? O3A Na2A Na3A 44.06(15) . . ? O2A Na2A Na3A 88.61(16) . . ? O6A Na2A Na3A 141.6(3) . . ? O4A Na2A Na3A 46.30(14) . . ? Cl5A Na2A Na3A 98.63(12) . . ? C19A Na2A Na3A 107.10(15) . . ? O3A Na2A Na1A 89.73(16) . . ? O2A Na2A Na1A 41.69(15) . . ? O6A Na2A Na1A 158.1(3) . . ? O4A Na2A Na1A 46.32(14) . . ? Cl5A Na2A Na1A 106.28(11) . . ? C19A Na2A Na1A 63.57(15) . . ? Na3A Na2A Na1A 57.33(9) . . ? O1A Na3A O3A 94.8(2) . . ? O1A Na3A O7A 117.4(3) . . ? O3A Na3A O7A 125.2(3) . . ? O1A Na3A O4A 96.0(2) . . ? O3A Na3A O4A 89.7(2) . . ? O7A Na3A O4A 125.6(3) . . ? O1A Na3A Na1A 46.92(17) . . ? O3A Na3A Na1A 93.52(17) . . ? O7A Na3A Na1A 141.0(3) . . ? O4A Na3A Na1A 49.13(14) . . ? O1A Na3A Na2A 92.94(17) . . ? O3A Na3A Na2A 43.33(15) . . ? O7A Na3A Na2A 149.5(3) . . ? O4A Na3A Na2A 46.80(14) . . ? Na1A Na3A Na2A 62.41(10) . . ? C11A O1A Na3A 147.7(5) . . ? C11A O1A Na1A 123.5(5) . . ? Na3A O1A Na1A 88.36(19) . . ? C19A O2A Na1A 147.6(5) . . ? C19A O2A Na2A 117.3(4) . . ? Na1A O2A Na2A 94.6(2) . . ? C27A O3A Na2A 137.5(5) . . ? C27A O3A Na3A 129.7(5) . . ? Na2A O3A Na3A 92.6(2) . . ? C4A O4A Na3A 126.7(5) . . ? C4A O4A Na2A 131.4(4) . . ? Na3A O4A Na2A 86.90(19) . . ? C4A O4A Na1A 125.5(4) . . ? Na3A O4A Na1A 83.03(18) . . ? Na2A O4A Na1A 88.05(19) . . ? C38A O5A C40A 113.9(15) . . ? C38A O5A Na1A 124.1(10) . . ? C40A O5A Na1A 118.7(10) . . ? C36A O6A C34A 115.1(11) . . ? C36A O6A Na2A 129.9(9) . . ? C34A O6A Na2A 114.9(8) . . ? C42A O7A C44A 107.9(18) . . ? C42A O7A Na3A 133.1(16) . . ? C44A O7A Na3A 119.0(10) . . ? C5A Cl1A Na1A 93.8(3) . . ? C9A Cl5A Na2A 101.9(3) . . ? C3A N1A C2A 110.0(5) . . ? C3A N1A C1A 112.9(5) . . ? C2A N1A C1A 109.8(4) . . ? C3A N1A H1A 100.9 . . ? C2A N1A H1A 110.3 . . ? C1A N1A H1A 112.6 . . ? C10A C1A N1A 114.6(5) . . ? C10A C1A H1A1 108.6 . . ? N1A C1A H1A1 108.6 . . ? C10A C1A H1A2 108.6 . . ? N1A C1A H1A2 108.6 . . ? H1A1 C1A H1A2 107.6 . . ? N1A C2A C18A 113.0(5) . . ? N1A C2A H2A1 109 . . ? C18A C2A H2A1 109 . . ? N1A C2A H2A2 109 . . ? C18A C2A H2A2 109 . . ? H2A1 C2A H2A2 107.8 . . ? N1A C3A C26A 113.5(5) . . ? N1A C3A H3A1 108.9 . . ? C26A C3A H3A1 108.9 . . ? N1A C3A H3A2 108.9 . . ? C26A C3A H3A2 108.9 . . ? H3A1 C3A H3A2 107.7 . . ? O4A C4A C5A 122.9(6) . . ? O4A C4A C9A 123.6(6) . . ? C5A C4A C9A 113.5(6) . . ? C6A C5A C4A 122.1(7) . . ? C6A C5A Cl1A 121.6(6) . . ? C4A C5A Cl1A 116.3(6) . . ? C5A C6A C7A 121.5(8) . . ? C5A C6A Cl2A 119.4(7) . . ? C7A C6A Cl2A 119.2(7) . . ? C8A C7A C6A 119.1(8) . . ? C8A C7A Cl3A 119.1(7) . . ? C6A C7A Cl3A 121.7(7) . . ? C9A C8A C7A 119.4(7) . . ? C9A C8A Cl4A 120.5(6) . . ? C7A C8A Cl4A 120.0(7) . . ? C8A C9A C4A 124.4(7) . . ? C8A C9A Cl5A 119.8(6) . . ? C4A C9A Cl5A 115.8(6) . . ? C15A C10A C11A 121.1(6) . . ? C15A C10A C1A 119.7(6) . . ? C11A C10A C1A 119.2(5) . . ? O1A C11A C10A 121.7(5) . . ? O1A C11A C12A 120.8(6) . . ? C10A C11A C12A 117.5(6) . . ? C13A C12A C11A 119.2(6) . . ? C13A C12A C16A 121.5(6) . . ? C11A C12A C16A 119.3(6) . . ? C14A C13A C12A 122.7(6) . . ? C14A C13A H13A 118.6 . . ? C12A C13A H13A 118.6 . . ? C15A C14A C13A 117.4(6) . . ? C15A C14A C17A 122.1(7) . . ? C13A C14A C17A 120.6(6) . . ? C14A C15A C10A 121.7(7) . . ? C14A C15A H15A 119.1 . . ? C10A C15A H15A 119.1 . . ? C12A C16A H16A 109.5 . . ? C12A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C12A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C14A C17A H17A 109.5 . . ? C14A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C14A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C23A C18A C19A 121.2(6) . . ? C23A C18A C2A 119.7(6) . . ? C19A C18A C2A 119.0(6) . . ? O2A C19A C18A 121.0(6) . . ? O2A C19A C20A 122.5(7) . . ? C18A C19A C20A 116.6(6) . . ? C18A C19A Na2A 126.0(5) . . ? C20A C19A Na2A 102.0(4) . . ? C21A C20A C19A 120.6(6) . . ? C21A C20A C24A 121.3(7) . . ? C19A C20A C24A 118.0(7) . . ? C20A C21A C22A 123.1(7) . . ? C20A C21A H21A 118.4 . . ? C22A C21A H21A 118.4 . . ? C21A C22A C23A 117.1(7) . . ? C21A C22A C25A 120.1(7) . . ? C23A C22A C25A 122.8(8) . . ? C22A C23A C18A 121.1(7) . . ? C22A C23A H23A 119.4 . . ? C18A C23A H23A 119.4 . . ? C20A C24A H24A 109.5 . . ? C20A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C20A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C22A C25A H25A 109.5 . . ? C22A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C22A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C27A C26A C31A 121.0(6) . . ? C27A C26A C3A 119.2(6) . . ? C31A C26A C3A 119.6(7) . . ? O3A C27A C26A 121.4(6) . . ? O3A C27A C28A 120.5(7) . . ? C26A C27A C28A 118.1(6) . . ? C29A C28A C27A 118.1(7) . . ? C29A C28A C32A 122.5(7) . . ? C27A C28A C32A 119.4(7) . . ? C28A C29A C30A 124.4(6) . . ? C28A C29A H29A 117.8 . . ? C30A C29A H29A 117.8 . . ? C31A C30A C29A 117.4(7) . . ? C31A C30A C33A 119.6(8) . . ? C29A C30A C33A 122.8(7) . . ? C30A C31A C26A 120.9(8) . . ? C30A C31A H31A 119.6 . . ? C26A C31A H31A 119.6 . . ? C28A C32A H32A 109.5 . . ? C28A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C28A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30A C33A H33A 109.5 . . ? C30A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C30A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? O6A C34A C35A 122(2) . . ? O6A C34A H34A 106.9 . . ? C35A C34A H34A 106.9 . . ? O6A C34A H34B 106.9 . . ? C35A C34A H34B 106.9 . . ? H34A C34A H34B 106.7 . . ? C34A C35A H35A 109.5 . . ? C34A C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C34A C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? O6A C36A C37A 109.7(16) . . ? O6A C36A H36A 109.7 . . ? C37A C36A H36A 109.7 . . ? O6A C36A H36B 109.7 . . ? C37A C36A H36B 109.7 . . ? H36A C36A H36B 108.2 . . ? C36A C37A H37A 109.5 . . ? C36A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C36A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? O5A C38A C39A 116.1(14) . . ? O5A C38A H38A 108.3 . . ? C39A C38A H38A 108.3 . . ? O5A C38A H38B 108.3 . . ? C39A C38A H38B 108.3 . . ? H38A C38A H38B 107.4 . . ? C38A C39A H39A 109.5 . . ? C38A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C38A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? C41A C40A O5A 113.7(14) . . ? C41A C40A H40A 108.8 . . ? O5A C40A H40A 108.8 . . ? C41A C40A H40B 108.8 . . ? O5A C40A H40B 108.8 . . ? H40A C40A H40B 107.7 . . ? C40A C41A H41A 109.5 . . ? C40A C41A H41B 109.5 . . ? H41A C41A H41B 109.5 . . ? C40A C41A H41C 109.5 . . ? H41A C41A H41C 109.5 . . ? H41B C41A H41C 109.5 . . ? C43A C42A O7A 110(3) . . ? C43A C42A H42A 109.7 . . ? O7A C42A H42A 109.7 . . ? C43A C42A H42B 109.7 . . ? O7A C42A H42B 109.7 . . ? H42A C42A H42B 108.2 . . ? C42A C43A H43A 109.5 . . ? C42A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C42A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? O7A C44A C45A 108.9(12) . . ? O7A C44A H44A 109.9 . . ? C45A C44A H44A 109.9 . . ? O7A C44A H44B 109.9 . . ? C45A C44A H44B 109.9 . . ? H44A C44A H44B 108.3 . . ? C44A C45A H45A 109.5 . . ? C44A C45A H45B 109.5 . . ? H45A C45A H45B 109.5 . . ? C44A C45A H45C 109.5 . . ? H45A C45A H45C 109.5 . . ? H45B C45A H45C 109.5 . . ? O1B Na1B O2B 91.99(18) . . ? O1B Na1B O4B 91.10(17) . . ? O2B Na1B O4B 89.61(17) . . ? O1B Na1B O5B 123.2(2) . . ? O2B Na1B O5B 119.8(2) . . ? O4B Na1B O5B 130.6(2) . . ? O1B Na1B Cl1B 92.91(14) . . ? O2B Na1B Cl1B 152.28(15) . . ? O4B Na1B Cl1B 63.04(12) . . ? O5B Na1B Cl1B 79.34(17) . . ? O1B Na1B Na3B 43.81(12) . . ? O2B Na1B Na3B 89.71(14) . . ? O4B Na1B Na3B 47.34(12) . . ? O5B Na1B Na3B 150.0(2) . . ? Cl1B Na1B Na3B 75.33(8) . . ? O1B Na1B Na2B 89.43(13) . . ? O2B Na1B Na2B 43.93(13) . . ? O4B Na1B Na2B 45.82(12) . . ? O5B Na1B Na2B 146.53(19) . . ? Cl1B Na1B Na2B 108.85(9) . . ? Na3B Na1B Na2B 59.46(7) . . ? O2B Na2B O3B 96.38(18) . . ? O2B Na2B O4B 90.43(17) . . ? O3B Na2B O4B 90.62(17) . . ? O2B Na2B O6B 100.7(2) . . ? O3B Na2B O6B 141.0(2) . . ? O4B Na2B O6B 123.8(2) . . ? O2B Na2B Cl5B 152.57(15) . . ? O3B Na2B Cl5B 96.48(15) . . ? O4B Na2B Cl5B 65.32(12) . . ? O6B Na2B Cl5B 84.02(16) . . ? O2B Na2B Na3B 90.31(14) . . ? O3B Na2B Na3B 43.34(12) . . ? O4B Na2B Na3B 47.67(12) . . ? O6B Na2B Na3B 166.54(18) . . ? Cl5B Na2B Na3B 82.66(8) . . ? O2B Na2B Na1B 44.15(13) . . ? O3B Na2B Na1B 92.26(13) . . ? O4B Na2B Na1B 46.41(11) . . ? O6B Na2B Na1B 124.04(17) . . ? Cl5B Na2B Na1B 111.18(9) . . ? Na3B Na2B Na1B 60.00(7) . . ? O3B Na3B O1B 96.61(18) . . ? O3B Na3B O7B 111.7(2) . . ? O1B Na3B O7B 134.4(2) . . ? O3B Na3B O4B 91.02(17) . . ? O1B Na3B O4B 90.62(16) . . ? O7B Na3B O4B 122.4(3) . . ? O3B Na3B C4B 105.36(17) . . ? O1B Na3B C4B 107.06(17) . . ? O7B Na3B C4B 99.2(3) . . ? O4B Na3B C4B 23.62(16) . . ? O3B Na3B Na2B 45.04(12) . . ? O1B Na3B Na2B 90.48(14) . . ? O7B Na3B Na2B 134.8(2) . . ? O4B Na3B Na2B 46.36(12) . . ? C4B Na3B Na2B 64.68(13) . . ? O3B Na3B Na1B 94.04(14) . . ? O1B Na3B Na1B 44.02(12) . . ? O7B Na3B Na1B 153.2(2) . . ? O4B Na3B Na1B 46.64(11) . . ? C4B Na3B Na1B 65.42(13) . . ? Na2B Na3B Na1B 60.54(7) . . ? C1B N1B C2B 111.6(5) . . ? C1B N1B C3B 110.7(4) . . ? C2B N1B C3B 111.4(4) . . ? C1B N1B H1B 111.8 . . ? C2B N1B H1B 101.5 . . ? C3B N1B H1B 109.4 . . ? C11B O1B Na3B 127.3(4) . . ? C11B O1B Na1B 139.8(4) . . ? Na3B O1B Na1B 92.17(16) . . ? C19B O2B Na2B 134.9(4) . . ? C19B O2B Na1B 132.9(4) . . ? Na2B O2B Na1B 91.91(18) . . ? C27B O3B Na3B 137.1(4) . . ? C27B O3B Na2B 131.1(4) . . ? Na3B O3B Na2B 91.62(16) . . ? C4B O4B Na2B 133.7(3) . . ? C4B O4B Na1B 135.6(3) . . ? Na2B O4B Na1B 87.78(17) . . ? C4B O4B Na3B 108.3(4) . . ? Na2B O4B Na3B 85.97(16) . . ? Na1B O4B Na3B 86.03(15) . . ? C36B O5B C34D 106.9(9) . . ? C36B O5B C34B 122.1(14) . . ? C36B O5B Na1B 118.6(5) . . ? C34D O5B Na1B 132.5(8) . . ? C34B O5B Na1B 114.2(13) . . ? C40B O6B C38B 113.4(9) . . ? C40B O6B Na2B 117.2(7) . . ? C38B O6B Na2B 120.6(6) . . ? C44B O7B C42B 119.2(9) . . ? C44B O7B Na3B 121.6(7) . . ? C42B O7B Na3B 118.4(7) . . ? C5B Cl1B Na1B 99.9(2) . . ? C9B Cl5B Na2B 100.2(2) . . ? C10B C1B N1B 113.1(5) . . ? C10B C1B H1B1 109 . . ? N1B C1B H1B1 109 . . ? C10B C1B H1B2 109 . . ? N1B C1B H1B2 109 . . ? H1B1 C1B H1B2 107.8 . . ? C18B C2B N1B 115.0(5) . . ? C18B C2B H2B1 108.5 . . ? N1B C2B H2B1 108.5 . . ? C18B C2B H2B2 108.5 . . ? N1B C2B H2B2 108.5 . . ? H2B1 C2B H2B2 107.5 . . ? C26B C3B N1B 113.6(4) . . ? C26B C3B H3B1 108.9 . . ? N1B C3B H3B1 108.9 . . ? C26B C3B H3B2 108.9 . . ? N1B C3B H3B2 108.9 . . ? H3B1 C3B H3B2 107.7 . . ? O4B C4B C9B 123.9(5) . . ? O4B C4B C5B 122.4(5) . . ? C9B C4B C5B 113.7(5) . . ? O4B C4B Na3B 48.1(3) . . ? C9B C4B Na3B 114.4(4) . . ? C5B C4B Na3B 107.3(4) . . ? C6B C5B C4B 122.5(5) . . ? C6B C5B Cl1B 121.2(5) . . ? C4B C5B Cl1B 116.3(5) . . ? C7B C6B C5B 121.2(6) . . ? C7B C6B Cl2B 120.1(5) . . ? C5B C6B Cl2B 118.7(5) . . ? C6B C7B C8B 118.8(6) . . ? C6B C7B Cl3B 121.5(5) . . ? C8B C7B Cl3B 119.8(5) . . ? C9B C8B C7B 119.6(6) . . ? C9B C8B Cl4B 121.4(5) . . ? C7B C8B Cl4B 119.1(5) . . ? C8B C9B C4B 124.3(5) . . ? C8B C9B Cl5B 119.4(5) . . ? C4B C9B Cl5B 116.3(5) . . ? C15B C10B C11B 120.7(5) . . ? C15B C10B C1B 119.5(5) . . ? C11B C10B C1B 119.8(5) . . ? O1B C11B C10B 120.6(5) . . ? O1B C11B C12B 122.0(6) . . ? C10B C11B C12B 117.4(5) . . ? C13B C12B C11B 119.2(6) . . ? C13B C12B C16B 122.5(6) . . ? C11B C12B C16B 118.2(6) . . ? C14B C13B C12B 123.5(6) . . ? C14B C13B H13B 118.3 . . ? C12B C13B H13B 118.3 . . ? C13B C14B C15B 117.8(5) . . ? C13B C14B C17B 122.0(7) . . ? C15B C14B C17B 120.3(7) . . ? C14B C15B C10B 121.4(6) . . ? C14B C15B H15B 119.3 . . ? C10B C15B H15B 119.3 . . ? C12B C16B H16D 109.5 . . ? C12B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C12B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C14B C17B H17D 109.5 . . ? C14B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C14B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C23B C18B C19B 121.9(6) . . ? C23B C18B C2B 118.2(6) . . ? C19B C18B C2B 119.8(6) . . ? O2B C19B C18B 121.0(6) . . ? O2B C19B C20B 122.5(6) . . ? C18B C19B C20B 116.5(6) . . ? C21B C20B C19B 119.1(8) . . ? C21B C20B C24B 120.8(8) . . ? C19B C20B C24B 120.1(7) . . ? C20B C21B C22B 124.7(8) . . ? C20B C21B H21B 117.6 . . ? C22B C21B H21B 117.6 . . ? C21B C22B C23B 116.1(8) . . ? C21B C22B C25B 123.4(10) . . ? C23B C22B C25B 120.4(10) . . ? C18B C23B C22B 121.6(8) . . ? C18B C23B H23B 119.2 . . ? C22B C23B H23B 119.2 . . ? C20B C24B H24D 109.5 . . ? C20B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C20B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C22B C25B H25D 109.5 . . ? C22B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C22B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C31B C26B C27B 120.9(5) . . ? C31B C26B C3B 118.7(5) . . ? C27B C26B C3B 120.4(5) . . ? O3B C27B C26B 121.1(5) . . ? O3B C27B C28B 121.7(5) . . ? C26B C27B C28B 117.2(5) . . ? C29B C28B C27B 119.8(5) . . ? C29B C28B C32B 121.8(5) . . ? C27B C28B C32B 118.4(5) . . ? C30B C29B C28B 123.5(5) . . ? C30B C29B H29B 118.2 . . ? C28B C29B H29B 118.2 . . ? C29B C30B C31B 117.1(5) . . ? C29B C30B C33B 121.8(5) . . ? C31B C30B C33B 120.9(6) . . ? C26B C31B C30B 121.3(6) . . ? C26B C31B H31B 119.3 . . ? C30B C31B H31B 119.3 . . ? C28B C32B H32D 109.5 . . ? C28B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C28B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C30B C33B H33D 109.5 . . ? C30B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C30B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C35B C34B O5B 107(4) . . ? C35B C34B H34C 110.3 . . ? O5B C34B H34C 110.3 . . ? C35B C34B H34D 110.3 . . ? O5B C34B H34D 110.3 . . ? H34C C34B H34D 108.6 . . ? C34B C35B H35D 109.5 . . ? C34B C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C34B C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? O5B C34D C35D 109.3(16) . . ? O5B C34D H34E 109.8 . . ? C35D C34D H34E 109.8 . . ? O5B C34D H34F 109.8 . . ? C35D C34D H34F 109.8 . . ? H34E C34D H34F 108.3 . . ? C34D C35D H35G 109.5 . . ? C34D C35D H35H 109.5 . . ? H35G C35D H35H 109.5 . . ? C34D C35D H35I 109.5 . . ? H35G C35D H35I 109.5 . . ? H35H C35D H35I 109.5 . . ? O5B C36B C37B 109.4(8) . . ? O5B C36B H36C 109.8 . . ? C37B C36B H36C 109.8 . . ? O5B C36B H36D 109.8 . . ? C37B C36B H36D 109.8 . . ? H36C C36B H36D 108.2 . . ? C36B C37B H37D 109.5 . . ? C36B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C36B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? O6B C38B C39B 111.1(9) . . ? O6B C38B H38C 109.4 . . ? C39B C38B H38C 109.4 . . ? O6B C38B H38D 109.4 . . ? C39B C38B H38D 109.4 . . ? H38C C38B H38D 108 . . ? C38B C39B H39D 109.5 . . ? C38B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C38B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C41B C40B O6B 114.6(11) . . ? C41B C40B H40C 108.6 . . ? O6B C40B H40C 108.6 . . ? C41B C40B H40D 108.6 . . ? O6B C40B H40D 108.6 . . ? H40C C40B H40D 107.6 . . ? C40B C41B H41D 109.5 . . ? C40B C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C40B C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C43B C42B O7B 110.4(10) . . ? C43B C42B H42C 109.6 . . ? O7B C42B H42C 109.6 . . ? C43B C42B H42D 109.6 . . ? O7B C42B H42D 109.6 . . ? H42C C42B H42D 108.1 . . ? C42B C43B H43D 109.5 . . ? C42B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C42B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? O7B C44B C45B 111.1(9) . . ? O7B C44B H44C 109.4 . . ? C45B C44B H44C 109.4 . . ? O7B C44B H44D 109.4 . . ? C45B C44B H44D 109.4 . . ? H44C C44B H44D 108 . . ? C44B C45B H45D 109.5 . . ? C44B C45B H45E 109.5 . . ? H45D C45B H45E 109.5 . . ? C44B C45B H45F 109.5 . . ? H45D C45B H45F 109.5 . . ? H45E C45B H45F 109.5 . . ? C3C O1C C1C 131(2) . . ? O1C C1C C2C 131(3) . . ? O1C C1C H1C1 104.6 . . ? C2C C1C H1C1 104.6 . . ? O1C C1C H1C2 104.6 . . ? C2C C1C H1C2 104.6 . . ? H1C1 C1C H1C2 105.7 . . ? C1C C2C H2C1 109.5 . . ? C1C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? C1C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? O1C C3C C4C 130(2) . . ? O1C C3C H3C1 104.7 . . ? C4C C3C H3C1 104.7 . . ? O1C C3C H3C2 104.7 . . ? C4C C3C H3C2 104.7 . . ? H3C1 C3C H3C2 105.7 . . ? C3C C4C H4C1 109.5 . . ? C3C C4C H4C2 109.5 . . ? H4C1 C4C H4C2 109.5 . . ? C3C C4C H4C3 109.5 . . ? H4C1 C4C H4C3 109.5 . . ? H4C2 C4C H4C3 109.5 . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 916824'