# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _audit_creation_method CRYSTALS_ver_12-03-99 _publ_contact_author_name 'Jeremy K.M Sanders' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK ; _publ_contact_author_email JKMS@CAM.AC.UK _publ_section_title ; Cation-reinforced donor-acceptor pseudorotaxanes ; loop_ _publ_author_name J.Sanders 'Thibaut Jarrosson' 'Guido Kaiser' 'Christoph Naumann' 'Sijbren Otto' 'Sofia Ioana Pascu' ################################ ## denoted [Li212]Br2 in text ## ################################ data_1 _database_code_depnum_ccdc_archive 'CCDC 254110' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 15.8820(3) _cell_angle_alpha 90 _cell_length_b 10.2424(2) _cell_angle_beta 94.5550(7) _cell_length_c 26.2432(6) _cell_angle_gamma 90 _cell_volume 4255.49(15) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Li ' -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C63 H81 Br2 Cl15 N2 O16 ' _chemical_formula_moiety ; C36 H44 O10, C22 H28 N2 O4, 5(C H2 Cl3), 2(H2 O), 2Br ; _chemical_compound_source ; ? ; _chemical_formula_weight 1827.73 _cell_measurement_reflns_used 24872 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_measurement_temperature 180 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.481 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 24285 _reflns_number_total 7714 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 7714 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7775 _diffrn_reflns_theta_min 5.151 _diffrn_reflns_theta_max 25.347 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.586 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _refine_diff_density_min -1.31 _refine_diff_density_max 1.25 _refine_ls_number_reflns 3794 _refine_ls_number_restraints 204 _refine_ls_number_parameters 541 #_refine_ls_R_factor_ref 0.1000 _refine_ls_wR_factor_ref 0.1184 _refine_ls_goodness_of_fit_ref 1.0981 #_reflns_number_all 7714 _refine_ls_R_factor_all 0.1577 _refine_ls_wR_factor_all 0.1528 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3794 _refine_ls_R_factor_gt 0.1000 _refine_ls_wR_factor_gt 0.1184 _refine_ls_shift/su_max 0.088587 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.93 1.99 2.06 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; SIR97 (Altomare et al, 1999) Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001 Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Li1 Li 0.8192(11) -0.1927(16) 0.0558(7) 0.0585 1.0000 Uani . . . . . . Br1 Br 0.97035(7) 0.21643(10) 0.05204(4) 0.0556 1.0000 Uani . . . . . . N1 N 0.5749(6) -0.2416(10) 0.0772(4) 0.0768 1.0000 Uani . . . . . . O1 O 0.6953(4) 0.1056(7) 0.1232(3) 0.0560 1.0000 Uani . . . . . . O2 O 0.8278(4) -0.0995(7) 0.1330(2) 0.0532 1.0000 Uani . . . . . . O3 O 0.8757(5) -0.3303(7) 0.0972(2) 0.0568 1.0000 Uani . . . . . . O4 O 0.1962(4) 0.3641(7) -0.0028(3) 0.0583 1.0000 Uani . . . . . . O5 O 0.3420(5) 0.2848(8) 0.0673(3) 0.0658 1.0000 Uani . . . . . . O6 O 0.7014(5) -0.1646(8) 0.0503(3) 0.0717 1.0000 Uani . . . . . . O7 O 0.4319(6) -0.2706(11) 0.0869(4) 0.0912 1.0000 Uani . . . . . . O8 O 0.8909(5) -0.0786(7) 0.0201(3) 0.0673 1.0000 Uani . . . . . . C1 C 0.6363(7) 0.1868(9) 0.0984(3) 0.0554 1.0000 Uani . . . . . . C2 C 0.6560(7) 0.2813(11) 0.0631(4) 0.0621 1.0000 Uani . . . . . . C3 C 0.5874(8) 0.3581(11) 0.0410(4) 0.0688 1.0000 Uani . . . . . . C4 C 0.5067(8) 0.3374(11) 0.0510(4) 0.0642 1.0000 Uani . . . . . . C5 C 0.4008(7) 0.2093(12) 0.0936(4) 0.0635 1.0000 Uani . . . . . . C6 C 0.3804(7) 0.1064(13) 0.1251(4) 0.0684 1.0000 Uani . . . . . . C7 C 0.4485(8) 0.0336(13) 0.1500(4) 0.0726 1.0000 Uani . . . . . . C8 C 0.5317(8) 0.0625(12) 0.1434(4) 0.0652 1.0000 Uani . . . . . . C9 C 0.5519(7) 0.1628(11) 0.1103(4) 0.0551 1.0000 Uani . . . . . . C10 C 0.4865(7) 0.2400(10) 0.0841(4) 0.0569 1.0000 Uani . . . . . . C11 C 0.7800(7) 0.1186(11) 0.1103(4) 0.0617 1.0000 Uani . . . . . . C12 C 0.8362(7) 0.0343(11) 0.1454(4) 0.0595 1.0000 Uani . . . . . . C13 C 0.8897(8) -0.1730(12) 0.1625(4) 0.0638 1.0000 Uani . . . . . . C14 C 0.8735(8) -0.3171(12) 0.1509(4) 0.0682 1.0000 Uani . . . . . . C15 C 0.8606(8) -0.4610(10) 0.0798(5) 0.0659 1.0000 Uani . . . . . . C16 C 0.8645(7) -0.4580(10) 0.0228(4) 0.0593 1.0000 Uani . . . . . . C17 C 0.2005(7) 0.3641(12) 0.0527(4) 0.0682 1.0000 Uani . . . . . . C18 C 0.2545(8) 0.2572(12) 0.0743(4) 0.0702 1.0000 Uani . . . . . . C19 C 0.6255(8) -0.1577(13) 0.0500(4) 0.0664 1.0000 Uani . . . . . . C20 C 0.5668(6) -0.0666(13) 0.0212(4) 0.0621 1.0000 Uani . . . . . . C21 C 0.4840(6) -0.1002(12) 0.0325(4) 0.0607 1.0000 Uani . . . . . . C22 C 0.4895(8) -0.2113(15) 0.0688(5) 0.0772 1.0000 Uani . . . . . . C23 C 0.5856(6) 0.0292(13) -0.0118(4) 0.0629 1.0000 Uani . . . . . . C24 C 0.6036(18) -0.349(3) 0.1063(10) 0.1864 1.0000 Uani D U . . . . C25 C 0.6293(18) -0.331(2) 0.1610(10) 0.1870 1.0000 Uani D U . . . . C26 C 0.6595(17) -0.461(2) 0.1825(9) 0.1880 1.0000 Uani D U . . . . C27 C 0.6859(17) -0.453(2) 0.2366(9) 0.1889 1.0000 Uani D U . . . . C28 C 0.739(3) -0.560(4) 0.2568(13) 0.1892 0.5000 Uani D U . 1 1 . C29 C 0.792(3) -0.613(5) 0.218(2) 0.1895 0.5000 Uani D U . 1 1 . C280 C 0.685(3) -0.581(3) 0.2629(14) 0.1892 0.5000 Uani D U . 1 2 . C290 C 0.751(4) -0.669(4) 0.250(3) 0.1893 0.5000 Uani D U . 1 2 . C30 C 1.0267(5) 0.2690(5) 0.18292(16) 0.1413 1.0000 Uani D U . . . . C31 C 0.8663(2) 0.2082(4) -0.07485(13) 0.0878 1.0000 Uani D U . . . . Cl1 Cl 1.1130(6) 0.3783(8) 0.1890(4) 0.1443 0.5000 Uani D U . 2 1 . Cl2 Cl 1.0550(6) 0.1231(7) 0.2153(3) 0.1382 0.5000 Uani D U . 2 1 . Cl3 Cl 0.9421(6) 0.3380(9) 0.2101(3) 0.1418 0.5000 Uani D U . 2 1 . Cl101 Cl 1.0745(7) 0.4248(7) 0.1837(3) 0.1397 0.5000 Uani D U . 2 2 . Cl102 Cl 1.1028(7) 0.1524(8) 0.2041(3) 0.1423 0.5000 Uani D U . 2 2 . Cl103 Cl 0.9456(6) 0.2698(9) 0.2247(3) 0.1437 0.5000 Uani D U . 2 2 . Cl4 Cl 0.8922(5) 0.0578(7) -0.1010(3) 0.0900 0.5000 Uani D U . 3 1 . Cl5 Cl 0.8981(6) 0.3355(7) -0.1151(3) 0.0896 0.5000 Uani D U . 3 1 . Cl6 Cl 0.7567(5) 0.2163(9) -0.0714(4) 0.0863 0.5000 Uani D U . 3 1 . Cl104 Cl 0.7576(5) 0.2401(8) -0.0714(4) 0.0858 0.5000 Uani D U . 3 2 . Cl105 Cl 0.8781(6) 0.0723(7) -0.1157(3) 0.0905 0.5000 Uani D U . 3 2 . Cl106 Cl 0.9138(5) 0.3441(7) -0.1001(3) 0.0878 0.5000 Uani D U . 3 2 . C32 C 0.6032(8) -0.0137(14) 0.2756(5) 0.2104 0.5000 Uani D U . . . . Cl107 Cl 0.6154(10) 0.0492(18) 0.3374(6) 0.2108 0.5000 Uani D U . . . . Cl108 Cl 0.5375(9) -0.1489(18) 0.2750(6) 0.2095 0.5000 Uani D U . . . . Cl109 Cl 0.7021(9) -0.061(2) 0.2570(6) 0.2112 0.5000 Uani D U . . . . H1 H 0.9188 -0.0038 0.0289 0.0500 1.0000 Uiso . . . . . . H2 H 0.8992 -0.1041 -0.0121 0.0819 1.0000 Uiso . . . . . . H21 H 0.7152 0.2946 0.0537 0.0737 1.0000 Uiso . . . . . . H31 H 0.6000 0.4305 0.0172 0.0813 1.0000 Uiso . . . . . . H41 H 0.4610 0.3932 0.0341 0.0757 1.0000 Uiso . . . . . . H61 H 0.3203 0.0844 0.1302 0.0816 1.0000 Uiso . . . . . . H71 H 0.4354 -0.0406 0.1728 0.0871 1.0000 Uiso . . . . . . H81 H 0.5778 0.0116 0.1624 0.0779 1.0000 Uiso . . . . . . H111 H 0.7980 0.2119 0.1143 0.0735 1.0000 Uiso . . . . . . H112 H 0.7842 0.0905 0.0741 0.0735 1.0000 Uiso . . . . . . H121 H 0.8962 0.0610 0.1426 0.0709 1.0000 Uiso . . . . . . H122 H 0.8210 0.0474 0.1813 0.0709 1.0000 Uiso . . . . . . H131 H 0.9475 -0.1482 0.1532 0.0755 1.0000 Uiso . . . . . . H132 H 0.8852 -0.1559 0.1997 0.0755 1.0000 Uiso . . . . . . H141 H 0.9182 -0.3722 0.1691 0.0813 1.0000 Uiso . . . . . . H142 H 0.8169 -0.3435 0.1616 0.0813 1.0000 Uiso . . . . . . H151 H 0.9050 -0.5209 0.0957 0.0787 1.0000 Uiso . . . . . . H152 H 0.8037 -0.4911 0.0886 0.0787 1.0000 Uiso . . . . . . H161 H 0.9223 -0.4320 0.0142 0.0700 1.0000 Uiso . . . . . . H162 H 0.8504 -0.5461 0.0081 0.0700 1.0000 Uiso . . . . . . H171 H 0.2242 0.4494 0.0656 0.0807 1.0000 Uiso . . . . . . H172 H 0.1422 0.3529 0.0640 0.0807 1.0000 Uiso . . . . . . H181 H 0.2471 0.2486 0.1116 0.0836 1.0000 Uiso . . . . . . H182 H 0.2377 0.1737 0.0565 0.0836 1.0000 Uiso . . . . . . H231 H 0.6446 0.0475 -0.0205 0.0751 1.0000 Uiso . . . . . . H241 H 0.6537 -0.3845 0.0900 0.2247 1.0000 Uiso . . . . . . H242 H 0.5572 -0.4151 0.1038 0.2247 1.0000 Uiso . . . . . . H251 H 0.6759 -0.2651 0.1653 0.2255 1.0000 Uiso . . . . . . H252 H 0.5800 -0.2997 0.1792 0.2255 1.0000 Uiso . . . . . . H261 H 0.7085 -0.4909 0.1638 0.2266 1.0000 Uiso . . . . . . H262 H 0.6125 -0.5257 0.1774 0.2266 1.0000 Uiso . . . . . . H271 H 0.7185 -0.3698 0.2427 0.2277 1.0000 Uiso . . . . . . H272 H 0.6340 -0.4500 0.2559 0.2277 1.0000 Uiso . . . . . . H281 H 0.7760 -0.5288 0.2867 0.2281 0.5000 Uiso . . . 1 1 . H282 H 0.7015 -0.6320 0.2680 0.2281 0.5000 Uiso . . . 1 1 . H291 H 0.8274 -0.6861 0.2323 0.2285 0.5000 Uiso . . . 1 1 . H292 H 0.8297 -0.5417 0.2061 0.2285 0.5000 Uiso . . . 1 1 . H293 H 0.7551 -0.6449 0.1875 0.2285 0.5000 Uiso . . . 1 1 . H2801 H 0.6915 -0.5656 0.3007 0.2281 0.5000 Uiso . . . 1 2 . H2802 H 0.6291 -0.6237 0.2536 0.2281 0.5000 Uiso . . . 1 2 . H2901 H 0.7472 -0.7529 0.2683 0.2282 0.5000 Uiso . . . 1 2 . H2902 H 0.8077 -0.6277 0.2589 0.2282 0.5000 Uiso . . . 1 2 . H2903 H 0.7453 -0.6858 0.2118 0.2282 0.5000 Uiso . . . 1 2 . H301 H 1.0031 0.2473 0.1475 0.1670 1.0000 Uiso . . . . . . H311 H 0.8934 0.1889 -0.0399 0.1061 1.0000 Uiso . . . . . . H321 H 0.5781 0.0542 0.2515 0.2538 0.5000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.053(9) 0.052(10) 0.069(10) 0.002(8) -0.003(8) 0.009(7) Br1 0.0672(7) 0.0517(6) 0.0477(5) -0.0042(5) 0.0041(4) 0.0100(6) N1 0.059(6) 0.076(7) 0.092(7) -0.032(6) -0.014(5) 0.020(5) O1 0.056(4) 0.057(4) 0.053(4) -0.005(3) -0.006(3) 0.015(3) O2 0.053(4) 0.062(4) 0.043(4) -0.005(3) -0.006(3) 0.013(3) O3 0.070(5) 0.050(4) 0.048(4) 0.001(3) -0.008(3) 0.010(3) O4 0.060(4) 0.053(4) 0.059(4) -0.007(3) -0.011(3) 0.011(3) O5 0.066(5) 0.069(5) 0.061(4) 0.005(4) -0.009(3) 0.011(4) O6 0.045(4) 0.085(5) 0.083(5) -0.038(4) -0.010(4) 0.014(4) O7 0.065(5) 0.101(7) 0.107(7) -0.002(6) 0.001(5) 0.001(5) O8 0.084(5) 0.061(5) 0.060(4) -0.014(4) 0.023(4) -0.005(4) C1 0.079(7) 0.051(6) 0.035(5) -0.013(4) -0.008(5) 0.015(5) C2 0.074(7) 0.047(5) 0.063(6) -0.011(6) -0.008(5) 0.009(6) C3 0.084(9) 0.051(7) 0.068(7) 0.004(5) -0.013(6) 0.000(6) C4 0.064(7) 0.056(6) 0.069(7) -0.008(6) -0.015(6) 0.014(6) C5 0.065(7) 0.072(7) 0.051(6) -0.014(6) -0.011(5) 0.018(6) C6 0.061(7) 0.086(8) 0.056(6) 0.001(6) -0.002(5) 0.015(6) C7 0.083(9) 0.091(9) 0.044(6) 0.005(6) 0.004(5) 0.019(7) C8 0.077(8) 0.075(7) 0.042(6) -0.006(5) 0.000(5) 0.017(6) C9 0.059(6) 0.055(6) 0.050(6) -0.019(5) -0.006(5) 0.008(5) C10 0.069(7) 0.051(6) 0.049(5) -0.011(4) -0.010(5) 0.009(5) C11 0.066(7) 0.052(6) 0.065(7) -0.011(5) -0.004(5) 0.008(5) C12 0.062(6) 0.064(7) 0.052(6) -0.006(5) -0.002(5) 0.011(5) C13 0.075(7) 0.069(7) 0.045(5) -0.011(5) -0.012(5) 0.023(6) C14 0.079(8) 0.072(8) 0.052(6) 0.012(5) -0.004(5) 0.025(6) C15 0.074(7) 0.042(6) 0.081(8) -0.004(5) 0.000(6) 0.015(5) C16 0.071(7) 0.041(5) 0.064(6) -0.005(5) -0.013(5) 0.019(5) C17 0.058(6) 0.079(8) 0.064(7) -0.009(6) -0.012(5) 0.011(6) C18 0.067(7) 0.082(9) 0.060(6) -0.008(5) -0.005(5) 0.020(6) C19 0.062(8) 0.075(8) 0.059(7) -0.035(6) -0.010(6) 0.017(6) C20 0.043(6) 0.087(8) 0.056(6) -0.030(6) -0.002(5) 0.013(6) C21 0.045(6) 0.077(8) 0.060(6) -0.034(6) 0.000(5) 0.008(5) C22 0.064(8) 0.087(9) 0.078(8) -0.029(8) -0.011(6) 0.012(7) C23 0.045(6) 0.085(8) 0.057(6) -0.031(6) -0.002(5) 0.007(6) C24 0.170(11) 0.156(10) 0.236(15) 0.067(12) 0.033(12) 0.011(9) C25 0.171(11) 0.156(10) 0.236(15) 0.067(12) 0.033(12) 0.011(9) C26 0.172(11) 0.157(10) 0.237(15) 0.067(12) 0.033(12) 0.011(9) C27 0.173(11) 0.159(10) 0.238(15) 0.067(12) 0.033(12) 0.011(9) C28 0.173(12) 0.159(10) 0.238(15) 0.066(12) 0.033(12) 0.011(9) C29 0.173(12) 0.160(10) 0.238(15) 0.066(12) 0.033(12) 0.011(9) C280 0.173(12) 0.159(10) 0.238(15) 0.067(12) 0.033(12) 0.011(9) C290 0.174(12) 0.159(10) 0.238(15) 0.067(12) 0.033(12) 0.011(9) C30 0.240(6) 0.084(3) 0.094(3) 0.000(2) -0.028(3) -0.001(3) C31 0.0843(19) 0.0788(17) 0.102(2) -0.0004(16) 0.0192(17) 0.0148(14) Cl1 0.242(6) 0.089(3) 0.096(3) 0.002(3) -0.025(3) -0.005(3) Cl2 0.237(6) 0.080(3) 0.090(3) -0.002(2) -0.030(3) -0.003(3) Cl3 0.240(6) 0.082(3) 0.097(3) 0.000(3) -0.028(3) 0.002(3) Cl101 0.238(6) 0.080(3) 0.094(3) 0.005(3) -0.030(3) 0.002(3) Cl102 0.242(6) 0.085(3) 0.094(3) -0.001(3) -0.026(3) 0.002(3) Cl103 0.240(6) 0.088(3) 0.097(3) -0.003(3) -0.026(3) -0.003(3) Cl4 0.090(2) 0.078(2) 0.103(3) 0.001(2) 0.016(2) 0.020(2) Cl5 0.084(2) 0.082(2) 0.105(3) 0.000(2) 0.020(2) 0.012(2) Cl6 0.082(2) 0.077(2) 0.101(3) 0.001(2) 0.021(2) 0.013(2) Cl104 0.082(2) 0.077(2) 0.101(3) 0.001(2) 0.021(2) 0.012(2) Cl105 0.091(2) 0.079(2) 0.103(3) -0.001(2) 0.016(2) 0.020(2) Cl106 0.083(2) 0.0801(19) 0.102(3) -0.0016(19) 0.020(2) 0.0133(17) C32 0.180(8) 0.256(12) 0.198(9) -0.005(8) 0.036(6) 0.000(8) Cl107 0.181(8) 0.257(12) 0.198(9) -0.005(8) 0.035(7) 0.000(8) Cl108 0.180(8) 0.256(12) 0.197(9) -0.004(8) 0.036(7) 0.001(8) Cl109 0.180(8) 0.257(12) 0.200(9) -0.005(8) 0.036(7) 0.001(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C19 . 1.409(18) yes N1 . C22 . 1.391(16) yes N1 . C24 . 1.39(2) yes O1 . C1 . 1.375(12) yes O1 . C11 . 1.419(13) yes O2 . C12 . 1.412(13) yes O2 . C13 . 1.419(12) yes O3 . C14 . 1.419(13) yes O3 . C15 . 1.429(12) yes O4 . C16 2_655 1.432(12) yes O4 . C17 . 1.454(13) yes O5 . C5 . 1.357(13) yes O5 . C18 . 1.445(15) yes O6 . C19 . 1.207(14) yes O7 . C22 . 1.225(17) yes O8 . H1 . 0.907 no O8 . H2 . 0.903 no C1 . C2 . 1.393(16) yes C1 . C9 . 1.422(16) yes C2 . C3 . 1.429(16) yes C2 . H21 . 1.000 no C3 . C4 . 1.345(17) yes C3 . H31 . 1.000 no C4 . C10 . 1.379(17) yes C4 . H41 . 1.000 no C5 . C6 . 1.395(17) yes C5 . C10 . 1.438(17) yes C6 . C7 . 1.427(16) yes C6 . H61 . 1.000 no C7 . C8 . 1.379(18) yes C7 . H71 . 1.000 no C8 . C9 . 1.399(17) yes C8 . H81 . 1.000 no C9 . C10 . 1.437(15) yes C11 . C12 . 1.503(15) yes C11 . H111 . 1.000 no C11 . H112 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.000 no C13 . C14 . 1.525(17) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . C16 . 1.500(16) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . H161 . 1.000 no C16 . H162 . 1.000 no C17 . C18 . 1.476(16) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C19 . C20 . 1.483(17) yes C20 . C21 . 1.414(16) yes C20 . C23 . 1.357(17) yes C21 . C23 2_655 1.398(16) yes C21 . C22 . 1.48(2) yes C23 . H231 . 1.000 no C24 . C25 . 1.473(17) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . C26 . 1.511(17) yes C25 . H251 . 1.001 no C25 . H252 . 1.000 no C26 . C27 . 1.449(17) yes C26 . H261 . 1.001 no C26 . H262 . 1.001 no C27 . C28 . 1.457(17) yes C27 . H271 . 1.001 no C27 . H272 . 1.001 no C27 . C280 . 1.483(18) yes C27 . H271 . 1.001 no C27 . H272 . 1.001 no C28 . C29 . 1.484(19) yes C28 . H281 . 1.000 no C28 . H282 . 1.001 no C29 . H291 . 0.997 no C29 . H292 . 1.003 no C29 . H293 . 1.003 no C280 . C290 . 1.451(19) yes C280 . H2801 . 1.000 no C280 . H2802 . 1.000 no C290 . H2901 . 0.998 no C290 . H2902 . 1.001 no C290 . H2903 . 1.005 no C30 . Cl1 . 1.766(9) yes C30 . Cl2 . 1.759(8) yes C30 . Cl3 . 1.722(8) yes C30 . H301 . 1.000 no C30 . Cl101 . 1.766(8) yes C30 . Cl102 . 1.758(8) yes C30 . Cl103 . 1.757(9) yes C30 . H301 . 1.000 no C31 . Cl4 . 1.748(7) yes C31 . Cl5 . 1.777(8) yes C31 . Cl6 . 1.752(8) yes C31 . H311 . 1.000 no C31 . Cl104 . 1.766(8) yes C31 . Cl105 . 1.775(7) yes C31 . Cl106 . 1.739(8) yes C31 . H311 . 1.000 no C32 . Cl107 . 1.742(9) yes C32 . Cl108 . 1.733(9) yes C32 . Cl109 . 1.751(9) yes C32 . H321 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C19 . N1 . C22 . 111.8(12) yes C19 . N1 . C24 . 125.7(14) yes C22 . N1 . C24 . 122.4(17) yes C1 . O1 . C11 . 117.0(8) yes C12 . O2 . C13 . 109.9(7) yes C14 . O3 . C15 . 113.0(8) yes C16 2_655 O4 . C17 . 110.1(8) yes C5 . O5 . C18 . 117.0(9) yes H1 . O8 . H2 . 112.263 no O1 . C1 . C2 . 123.6(10) yes O1 . C1 . C9 . 114.2(9) yes C2 . C1 . C9 . 122.1(9) yes C1 . C2 . C3 . 116.6(11) yes C1 . C2 . H21 . 121.683 no C3 . C2 . H21 . 121.699 no C2 . C3 . C4 . 122.8(11) yes C2 . C3 . H31 . 118.583 no C4 . C3 . H31 . 118.582 no C3 . C4 . C10 . 120.7(10) yes C3 . C4 . H41 . 119.653 no C10 . C4 . H41 . 119.658 no O5 . C5 . C6 . 123.4(11) yes O5 . C5 . C10 . 114.2(11) yes C6 . C5 . C10 . 122.4(10) yes C5 . C6 . C7 . 117.6(11) yes C5 . C6 . H61 . 121.216 no C7 . C6 . H61 . 121.213 no C6 . C7 . C8 . 122.0(12) yes C6 . C7 . H71 . 119.001 no C8 . C7 . H71 . 119.001 no C7 . C8 . C9 . 120.3(10) yes C7 . C8 . H81 . 119.832 no C9 . C8 . H81 . 119.841 no C1 . C9 . C8 . 122.0(10) yes C1 . C9 . C10 . 117.3(10) yes C8 . C9 . C10 . 120.5(10) yes C5 . C10 . C9 . 117.1(10) yes C5 . C10 . C4 . 122.6(10) yes C9 . C10 . C4 . 120.3(11) yes O1 . C11 . C12 . 109.2(9) yes O1 . C11 . H111 . 109.527 no C12 . C11 . H111 . 109.530 no O1 . C11 . H112 . 109.528 no C12 . C11 . H112 . 109.532 no H111 . C11 . H112 . 109.471 no C11 . C12 . O2 . 112.1(8) yes C11 . C12 . H121 . 108.804 no O2 . C12 . H121 . 108.803 no C11 . C12 . H122 . 108.810 no O2 . C12 . H122 . 108.805 no H121 . C12 . H122 . 109.464 no O2 . C13 . C14 . 107.7(9) yes O2 . C13 . H131 . 109.908 no C14 . C13 . H131 . 109.908 no O2 . C13 . H132 . 109.908 no C14 . C13 . H132 . 109.910 no H131 . C13 . H132 . 109.465 no C13 . C14 . O3 . 105.9(9) yes C13 . C14 . H141 . 110.356 no O3 . C14 . H141 . 110.363 no C13 . C14 . H142 . 110.354 no O3 . C14 . H142 . 110.359 no H141 . C14 . H142 . 109.469 no O3 . C15 . C16 . 106.3(9) yes O3 . C15 . H151 . 110.254 no C16 . C15 . H151 . 110.262 no O3 . C15 . H152 . 110.251 no C16 . C15 . H152 . 110.259 no H151 . C15 . H152 . 109.466 no C15 . C16 . O4 2_655 107.4(8) yes C15 . C16 . H161 . 109.982 no O4 2_655 C16 . H161 . 109.980 no C15 . C16 . H162 . 109.982 no O4 2_655 C16 . H162 . 109.981 no H161 . C16 . H162 . 109.466 no O4 . C17 . C18 . 111.3(9) yes O4 . C17 . H171 . 109.003 no C18 . C17 . H171 . 109.004 no O4 . C17 . H172 . 109.006 no C18 . C17 . H172 . 109.006 no H171 . C17 . H172 . 109.463 no C17 . C18 . O5 . 110.0(10) yes C17 . C18 . H181 . 109.334 no O5 . C18 . H181 . 109.335 no C17 . C18 . H182 . 109.334 no O5 . C18 . H182 . 109.335 no H181 . C18 . H182 . 109.466 no N1 . C19 . O6 . 124.8(12) yes N1 . C19 . C20 . 106.4(10) yes O6 . C19 . C20 . 128.8(14) yes C19 . C20 . C21 . 107.3(12) yes C19 . C20 . C23 . 128.2(11) yes C21 . C20 . C23 . 124.5(11) yes C20 . C21 . C23 2_655 120.8(12) yes C20 . C21 . C22 . 108.3(10) yes C23 2_655 C21 . C22 . 130.9(11) yes C21 . C22 . N1 . 106.3(13) yes C21 . C22 . O7 . 128.4(11) yes N1 . C22 . O7 . 125.2(14) yes C21 2_655 C23 . C20 . 114.6(10) yes C21 2_655 C23 . H231 . 122.689 no C20 . C23 . H231 . 122.685 no N1 . C24 . C25 . 119(2) yes N1 . C24 . H241 . 106.966 no C25 . C24 . H241 . 107.097 no N1 . C24 . H242 . 106.964 no C25 . C24 . H242 . 107.090 no H241 . C24 . H242 . 109.390 no C24 . C25 . C26 . 108.0(16) yes C24 . C25 . H251 . 109.845 no C26 . C25 . H251 . 109.871 no C24 . C25 . H252 . 109.858 no C26 . C25 . H252 . 109.864 no H251 . C25 . H252 . 109.398 no C25 . C26 . C27 . 112.0(17) yes C25 . C26 . H261 . 108.889 no C27 . C26 . H261 . 108.821 no C25 . C26 . H262 . 108.908 no C27 . C26 . H262 . 108.865 no H261 . C26 . H262 . 109.330 no C26 . C27 . C28 . 115.1(17) yes C26 . C27 . H271 . 108.111 no C28 . C27 . H271 . 108.017 no C26 . C27 . H272 . 108.119 no C28 . C27 . H272 . 108.016 no H271 . C27 . H272 . 109.333 no C26 . C27 . C280 . 113.1(19) yes C26 . C27 . H271 . 108.111 no C280 . C27 . H271 . 134.518 no C26 . C27 . H272 . 108.119 no C280 . C27 . H272 . 75.421 no H271 . C27 . H272 . 109.333 no C27 . C28 . C29 . 111.5(17) yes C27 . C28 . H281 . 109.211 no C29 . C28 . H281 . 108.821 no C27 . C28 . H282 . 109.124 no C29 . C28 . H282 . 108.804 no H281 . C28 . H282 . 109.379 no C28 . C29 . H291 . 109.963 no C28 . C29 . H292 . 109.488 no H291 . C29 . H292 . 109.461 no C28 . C29 . H293 . 109.491 no H291 . C29 . H293 . 109.441 no H292 . C29 . H293 . 108.978 no C27 . C280 . C290 . 113.6(19) yes C27 . C280 . H2801 . 108.657 no C290 . C280 . H2801 . 108.178 no C27 . C280 . H2802 . 108.587 no C290 . C280 . H2802 . 108.342 no H2801 . C280 . H2802 . 109.419 no C280 . C290 . H2901 . 109.940 no C280 . C290 . H2902 . 109.644 no H2901 . C290 . H2902 . 109.543 no C280 . C290 . H2903 . 109.419 no H2901 . C290 . H2903 . 109.272 no H2902 . C290 . H2903 . 109.005 no Cl1 . C30 . Cl2 . 109.16(10) yes Cl1 . C30 . Cl3 . 109.14(10) yes Cl2 . C30 . Cl3 . 109.07(10) yes Cl1 . C30 . H301 . 117.137 no Cl2 . C30 . H301 . 108.782 no Cl3 . C30 . H301 . 103.217 no Cl101 . C30 . Cl102 . 109.06(10) yes Cl101 . C30 . Cl103 . 108.95(10) yes Cl102 . C30 . Cl103 . 109.01(10) yes Cl101 . C30 . H301 . 109.928 no Cl102 . C30 . H301 . 109.877 no Cl103 . C30 . H301 . 109.991 no Cl4 . C31 . Cl5 . 109.04(10) yes Cl4 . C31 . Cl6 . 109.11(10) yes Cl5 . C31 . Cl6 . 109.04(10) yes Cl4 . C31 . H311 . 95.035 no Cl5 . C31 . H311 . 124.602 no Cl6 . C31 . H311 . 108.612 no Cl104 . C31 . Cl105 . 109.08(10) yes Cl104 . C31 . Cl106 . 109.09(10) yes Cl105 . C31 . Cl106 . 109.14(10) yes Cl104 . C31 . H311 . 109.873 no Cl105 . C31 . H311 . 109.825 no Cl106 . C31 . H311 . 109.816 no Cl107 . C32 . Cl108 . 109.04(10) yes Cl107 . C32 . Cl109 . 109.07(10) yes Cl108 . C32 . Cl109 . 109.05(10) yes Cl107 . C32 . H321 . 109.888 no Cl108 . C32 . H321 . 109.896 no Cl109 . C32 . H321 . 109.868 no #===END ######################################## ## denoted [Li212][B(C6F5)4]2 in text ## ######################################## data_2 _database_code_depnum_ccdc_archive 'CCDC 254111' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.7147(2) _cell_angle_alpha 103.2331(7) _cell_length_b 13.4449(2) _cell_angle_beta 90.1735(7) _cell_length_c 19.5512(3) _cell_angle_gamma 94.5532(7) _cell_volume 2732.42(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'Li ' -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C108 H76 B2 Cl4 F40 Li2 N2 O16 ' _chemical_formula_moiety ' C108 H76 B2 Cl4 F40 Li2 N2 O16 ' _chemical_compound_source ; ? ; _chemical_formula_weight 2595.03 _cell_measurement_reflns_used 20750 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 180 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1310.000 _exptl_absorpt_coefficient_mu 0.243 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR97 (Altomare et al, 1999) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 180(2) _diffrn_reflns_number 26977 _reflns_number_total 12240 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections with Friedels Law is 12240 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12577 _diffrn_reflns_theta_min 5.124 _diffrn_reflns_theta_max 27.518 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -17 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -0.72 _refine_diff_density_max 0.54 _refine_ls_number_reflns 8775 _refine_ls_number_parameters 784 #_refine_ls_R_factor_ref 0.0452 _refine_ls_wR_factor_ref 0.0562 _refine_ls_goodness_of_fit_ref 1.0940 #_reflns_number_all 12240 _refine_ls_R_factor_all 0.0682 _refine_ls_wR_factor_all 0.0666 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 8775 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_gt 0.0562 _refine_ls_shift/su_max 0.002676 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 2.06 0.801 1.63 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) SIR97: a new tool for crystal structure determination and refinement.J. App. Cryst. 32, 115-119 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_attached_hydrogens N1 N 0.02193(14) 1.25618(11) 0.05543(8) 0.0277 1.0000 Uani . B1 B -0.2914(2) 0.73868(15) 0.3715(1) 0.0277 1.0000 Uani . F1 F -0.14202(13) 0.6211(1) 0.43967(7) 0.0459 1.0000 Uani . F2 F 0.08860(15) 0.66989(14) 0.49368(8) 0.0653 1.0000 Uani . F3 F 0.21707(15) 0.84968(16) 0.4858(1) 0.0802 1.0000 Uani . F4 F 0.10450(15) 0.98310(13) 0.42285(9) 0.0674 1.0000 Uani . F5 F -0.12421(12) 0.9375(1) 0.36923(7) 0.0467 1.0000 Uani . F6 F -0.26802(13) 0.77121(11) 0.53400(6) 0.0467 1.0000 Uani . F7 F -0.44559(15) 0.71905(12) 0.61546(6) 0.0550 1.0000 Uani . F8 F -0.67251(15) 0.62851(13) 0.56064(7) 0.0583 1.0000 Uani . F9 F -0.71281(13) 0.58701(13) 0.41827(7) 0.0578 1.0000 Uani . F10 F -0.53744(11) 0.6397(1) 0.33524(6) 0.0394 1.0000 Uani . F11 F -0.16132(11) 0.75204(8) 0.24442(6) 0.0373 1.0000 Uani . F12 F -0.13121(13) 0.60330(11) 0.13062(7) 0.0485 1.0000 Uani . F13 F -0.22371(13) 0.4060(1) 0.12715(7) 0.0507 1.0000 Uani . F14 F -0.32591(12) 0.36101(9) 0.24437(8) 0.0450 1.0000 Uani . F15 F -0.36048(13) 0.50599(9) 0.35618(6) 0.0424 1.0000 Uani . F16 F -0.42528(12) 0.73889(9) 0.23037(6) 0.0396 1.0000 Uani . F17 F -0.55012(14) 0.88802(12) 0.20549(7) 0.0555 1.0000 Uani . F18 F -0.56935(16) 1.06299(12) 0.3067(1) 0.0660 1.0000 Uani . F19 F -0.45623(15) 1.0837(1) 0.43494(9) 0.0597 1.0000 Uani . F20 F -0.32739(12) 0.93349(9) 0.46115(6) 0.0417 1.0000 Uani . Li1 Li 0.1299(4) 1.2458(3) 0.25456(17) 0.0387 1.0000 Uani . O1 O -0.04399(14) 1.2446(1) -0.05893(7) 0.0342 1.0000 Uani . O2 O 0.07107(13) 1.2151(1) 0.15995(6) 0.0329 1.0000 Uani . O3 O -0.21492(13) 1.1190(1) 0.20879(7) 0.0333 1.0000 Uani . O4 O -0.05350(13) 1.2798(1) 0.29929(7) 0.0345 1.0000 Uani . O5 O 0.16389(12) 1.3934(1) 0.29679(7) 0.0318 1.0000 Uani . O6 O 0.32387(12) 1.2801(1) 0.21004(7) 0.0350 1.0000 Uani . O7 O 0.35060(13) 1.1201(1) 0.08244(7) 0.0323 1.0000 Uani . O8 O 0.18005(15) 0.15988(12) 0.31650(8) 0.0455 1.0000 Uani . C1 C -0.01590(16) 1.20386(13) -0.01293(9) 0.0264 1.0000 Uani . C2 C -0.01221(15) 1.09289(13) -0.01432(9) 0.0237 1.0000 Uani . C3 C 0.02331(15) 1.08464(13) 0.05274(8) 0.0236 1.0000 Uani . C4 C 0.04335(15) 1.18987(13) 0.09765(9) 0.0255 1.0000 Uani . C5 C -0.03767(16) 1.00832(13) -0.06960(8) 0.0244 1.0000 Uani . C6 C 0.03555(18) 1.36774(14) 0.0774(1) 0.0310 1.0000 Uani . C7 C 0.16180(18) 1.41375(14) 0.0585(1) 0.0305 1.0000 Uani . C8 C 0.1674(2) 1.53084(15) 0.07994(11) 0.0361 1.0000 Uani . C9 C 0.2877(2) 1.58418(15) 0.05915(11) 0.0400 1.0000 Uani . C10 C 0.4049(2) 1.57030(17) 0.09833(12) 0.0436 1.0000 Uani . C11 C 0.5211(3) 1.6263(2) 0.07548(14) 0.0576 1.0000 Uani . C12 C -0.23612(16) 1.03012(13) 0.15820(9) 0.0274 1.0000 Uani . C13 C -0.21905(18) 0.93399(14) 0.1680(1) 0.0309 1.0000 Uani . C14 C -0.24570(18) 0.84715(14) 0.1120(1) 0.0316 1.0000 Uani . C15 C -0.28442(17) 0.85695(13) 0.0475(1) 0.0286 1.0000 Uani . C16 C -0.33658(15) 0.96924(13) -0.03168(9) 0.0262 1.0000 Uani . C17 C -0.35200(17) 1.06513(15) -0.0420(1) 0.0311 1.0000 Uani . C18 C -0.33096(18) 1.15129(14) 0.0145(1) 0.0328 1.0000 Uani . C19 C -0.29415(17) 1.14232(14) 0.0798(1) 0.0296 1.0000 Uani . C20 C -0.27775(15) 1.04384(13) 0.09159(9) 0.0251 1.0000 Uani . C21 C -0.30023(16) 0.95541(13) 0.03579(9) 0.0261 1.0000 Uani . C22 C -0.1605(2) 1.11042(15) 0.2739(1) 0.0358 1.0000 Uani . C23 C -0.1473(2) 1.21486(16) 0.3232(1) 0.0388 1.0000 Uani . C24 C -0.0338(2) 1.37751(16) 0.34728(11) 0.0388 1.0000 Uani . C25 C 0.0520(2) 1.44430(15) 0.31285(11) 0.0385 1.0000 Uani . C26 C 0.24969(19) 1.44293(15) 0.2570(1) 0.0347 1.0000 Uani . C27 C 0.36374(19) 1.38376(15) 0.2452(1) 0.0347 1.0000 Uani . C28 C 0.42866(18) 1.22092(16) 0.1928(1) 0.0347 1.0000 Uani . C29 C 0.38869(18) 1.11412(15) 0.1518(1) 0.0339 1.0000 Uani . C30 C -0.14929(18) 0.77757(15) 0.4038(1) 0.0318 1.0000 Uani . C31 C -0.0843(2) 0.71316(16) 0.4348(1) 0.0372 1.0000 Uani . C32 C 0.0357(2) 0.7359(2) 0.46273(11) 0.0473 1.0000 Uani . C33 C 0.1001(2) 0.8275(2) 0.45917(12) 0.0533 1.0000 Uani . C34 C 0.0430(2) 0.89350(19) 0.42797(12) 0.0478 1.0000 Uani . C35 C -0.0784(2) 0.86763(16) 0.40054(11) 0.0379 1.0000 Uani . C36 C -0.39073(18) 0.70570(14) 0.42874(9) 0.0296 1.0000 Uani . C37 C -0.3765(2) 0.72405(15) 0.5015(1) 0.0343 1.0000 Uani . C38 C -0.4680(2) 0.69775(16) 0.5455(1) 0.0392 1.0000 Uani . C39 C -0.5823(2) 0.65271(17) 0.51859(11) 0.0396 1.0000 Uani . C40 C -0.6026(2) 0.63300(17) 0.44678(11) 0.0394 1.0000 Uani . C41 C -0.50938(19) 0.66111(15) 0.40509(9) 0.0326 1.0000 Uani . C42 C -0.26927(17) 0.63996(13) 0.30566(9) 0.0267 1.0000 Uani . C43 C -0.30441(18) 0.53728(14) 0.3022(1) 0.0304 1.0000 Uani . C44 C -0.28788(18) 0.45883(14) 0.24382(11) 0.0330 1.0000 Uani . C45 C -0.23286(18) 0.48074(15) 0.1854(1) 0.0348 1.0000 Uani . C46 C -0.18809(18) 0.58045(16) 0.1870(1) 0.0330 1.0000 Uani . C47 C -0.20612(17) 0.65566(14) 0.2466(1) 0.0293 1.0000 Uani . C48 C -0.36463(17) 0.82959(14) 0.3468(1) 0.0292 1.0000 Uani . C49 C -0.42571(18) 0.82293(15) 0.2835(1) 0.0316 1.0000 Uani . C50 C -0.4937(2) 0.89994(17) 0.26899(11) 0.0400 1.0000 Uani . C51 C -0.5038(2) 0.98774(17) 0.31986(13) 0.0437 1.0000 Uani . C52 C -0.4470(2) 0.99777(15) 0.38451(12) 0.0411 1.0000 Uani . C53 C -0.37982(19) 0.91952(14) 0.3966(1) 0.0329 1.0000 Uani . C54 C 0.1468(3) 0.7832(2) 0.21138(13) 0.0534 1.0000 Uani . Cl1 Cl 0.12860(9) 0.91289(5) 0.24357(4) 0.0712 1.0000 Uani . Cl2 Cl 0.18045(16) 0.72148(8) 0.27622(4) 0.1229 1.0000 Uani . H51 H -0.0641 1.0140 -0.1175 0.0295 1.0000 Uiso . H61 H -0.0322 1.3957 0.0539 0.0365 1.0000 Uiso . H62 H 0.0266 1.3881 0.1295 0.0365 1.0000 Uiso . H71 H 0.1732 1.3916 0.0066 0.0360 1.0000 Uiso . H72 H 0.2301 1.3892 0.0837 0.0360 1.0000 Uiso . H81 H 0.0949 1.5539 0.0570 0.0438 1.0000 Uiso . H82 H 0.1602 1.5519 0.1322 0.0438 1.0000 Uiso . H91 H 0.2770 1.6593 0.0681 0.0483 1.0000 Uiso . H92 H 0.2999 1.5565 0.0078 0.0483 1.0000 Uiso . H101 H 0.3937 1.5976 0.1498 0.0510 1.0000 Uiso . H102 H 0.4173 1.4955 0.0892 0.0510 1.0000 Uiso . H111 H 0.5959 1.6151 0.1026 0.0647 1.0000 Uiso . H112 H 0.5100 1.7013 0.0848 0.0647 1.0000 Uiso . H113 H 0.5335 1.5991 0.0241 0.0647 1.0000 Uiso . H131 H -0.1880 0.9255 0.2145 0.0376 1.0000 Uiso . H141 H -0.2360 0.7772 0.1199 0.0387 1.0000 Uiso . H151 H -0.3016 0.7946 0.0085 0.0343 1.0000 Uiso . H171 H -0.3780 1.0738 -0.0893 0.0384 1.0000 Uiso . H181 H -0.3432 1.2209 0.0067 0.0403 1.0000 Uiso . H191 H -0.2789 1.2048 0.1189 0.0355 1.0000 Uiso . H221 H -0.2157 1.0625 0.2951 0.0430 1.0000 Uiso . H222 H -0.0761 1.0835 0.2655 0.0430 1.0000 Uiso . H231 H -0.2292 1.2462 0.3253 0.0455 1.0000 Uiso . H232 H -0.1230 1.2077 0.3712 0.0455 1.0000 Uiso . H241 H -0.1155 1.4085 0.3576 0.0444 1.0000 Uiso . H242 H 0.0055 1.3698 0.3920 0.0444 1.0000 Uiso . H251 H 0.0717 1.5128 0.3456 0.0452 1.0000 Uiso . H252 H 0.0118 1.4536 0.2688 0.0452 1.0000 Uiso . H261 H 0.2736 1.5148 0.2835 0.0416 1.0000 Uiso . H262 H 0.2101 1.4439 0.2108 0.0416 1.0000 Uiso . H271 H 0.4240 1.4147 0.2154 0.0410 1.0000 Uiso . H272 H 0.4051 1.3849 0.2913 0.0410 1.0000 Uiso . H281 H 0.4873 1.2551 0.1639 0.0407 1.0000 Uiso . H282 H 0.4725 1.2169 0.2372 0.0407 1.0000 Uiso . H291 H 0.4603 1.0700 0.1489 0.0407 1.0000 Uiso . H292 H 0.3170 1.0843 0.1754 0.0407 1.0000 Uiso . H541 H 0.2167 0.7763 0.1773 0.0637 1.0000 Uiso . H542 H 0.0673 0.7496 0.1866 0.0637 1.0000 Uiso . 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 N1 0.0295(8) 0.0254(7) 0.0272(7) 0.0056(6) 0.0007(6) -0.0020(6) B1 0.032(1) 0.0259(9) 0.0251(9) 0.0064(7) -0.0022(8) 0.0034(7) F1 0.0514(7) 0.0466(7) 0.0440(7) 0.0166(6) -0.0047(6) 0.0132(6) F2 0.0569(9) 0.0991(12) 0.0461(8) 0.0200(8) -0.0116(7) 0.0346(8) F3 0.0410(8) 0.1092(14) 0.0779(11) -0.003(1) -0.0282(8) 0.0020(8) F4 0.0502(8) 0.0606(9) 0.0778(11) -0.0033(8) -0.0045(8) -0.0206(7) F5 0.0456(7) 0.0373(6) 0.0585(8) 0.0152(6) -0.0019(6) -0.0010(5) F6 0.0525(7) 0.0589(8) 0.0257(5) 0.0048(5) -0.0093(5) 0.0013(6) F7 0.078(1) 0.0684(9) 0.0217(6) 0.0143(6) 0.0025(6) 0.0146(7) F8 0.0649(9) 0.074(1) 0.0436(7) 0.0269(7) 0.0223(7) 0.0124(7) F9 0.0394(7) 0.0848(11) 0.0450(7) 0.0118(7) 0.0061(6) -0.0107(7) F10 0.0366(6) 0.0555(7) 0.0244(5) 0.0080(5) -0.0029(4) -0.0021(5) F11 0.0455(7) 0.0307(6) 0.0382(6) 0.0141(5) 0.0050(5) 0.0004(5) F12 0.0570(8) 0.0533(8) 0.0361(6) 0.0110(6) 0.0173(6) 0.0080(6) F13 0.0500(8) 0.0437(7) 0.0476(7) -0.0122(6) 0.0098(6) 0.0057(6) F14 0.0416(7) 0.0245(5) 0.0654(8) 0.0041(5) 0.0031(6) -0.0011(5) F15 0.0593(8) 0.0327(6) 0.0389(6) 0.0157(5) 0.0105(6) 0.0031(5) F16 0.0494(7) 0.0415(6) 0.0270(5) 0.0038(5) -0.0077(5) 0.0104(5) F17 0.0599(9) 0.0660(9) 0.0478(7) 0.0236(7) -0.0144(6) 0.0188(7) F18 0.071(1) 0.0476(8) 0.0860(11) 0.0217(8) -0.0110(8) 0.0289(7) F19 0.0673(9) 0.0351(7) 0.071(1) -0.0048(6) -0.0045(8) 0.0188(6) F20 0.0524(7) 0.0355(6) 0.0330(6) -0.0022(5) -0.0067(5) 0.0075(5) Li1 0.056(2) 0.0298(16) 0.0298(16) 0.0058(13) -0.0094(15) 0.0043(14) O1 0.0447(8) 0.0307(7) 0.0302(7) 0.0132(5) -0.0049(6) 0.0035(6) O2 0.0359(7) 0.0381(7) 0.0222(6) 0.0036(5) -0.0024(5) -0.0023(5) O3 0.0433(8) 0.0286(6) 0.0270(6) 0.0051(5) -0.0040(5) 0.0009(5) O4 0.0389(7) 0.0317(7) 0.0288(6) -0.0001(5) 0.0031(5) -0.0015(5) O5 0.0355(7) 0.0287(6) 0.0307(6) 0.0058(5) -0.0000(5) 0.0022(5) O6 0.0296(7) 0.0345(7) 0.0369(7) 0.0015(6) -0.0015(5) -0.0017(5) O7 0.0420(7) 0.0281(6) 0.0261(6) 0.0048(5) -0.0027(5) 0.0028(5) O8 0.0511(9) 0.0467(8) 0.0421(8) 0.0158(7) -0.0122(7) 0.0081(7) C1 0.0242(8) 0.0290(8) 0.0263(8) 0.0081(7) 0.0001(6) -0.0013(6) C2 0.0212(8) 0.0274(8) 0.0230(8) 0.0081(6) 0.0005(6) -0.0025(6) C3 0.0204(7) 0.0290(8) 0.0213(7) 0.0066(6) -0.0001(6) -0.0019(6) C4 0.0220(8) 0.0281(8) 0.0251(8) 0.0047(7) -0.0006(6) -0.0020(6) C5 0.0237(8) 0.0286(8) 0.0213(7) 0.0083(6) -0.0022(6) -0.0023(6) C6 0.0329(9) 0.0264(8) 0.0318(9) 0.0034(7) -0.0007(7) 0.0016(7) C7 0.0338(9) 0.0249(8) 0.0315(9) 0.0046(7) 0.0032(7) -0.0009(7) C8 0.0427(11) 0.0264(9) 0.041(1) 0.0108(8) 0.0017(8) 0.0012(8) C9 0.0513(12) 0.0296(9) 0.0399(11) 0.0131(8) -0.0000(9) -0.0069(8) C10 0.0469(12) 0.0403(11) 0.0404(11) 0.0061(9) -0.0004(9) -0.0071(9) C11 0.0504(14) 0.0592(15) 0.0522(14) -0.0020(12) 0.0047(11) -0.0193(11) C12 0.0256(8) 0.0274(8) 0.0283(8) 0.0060(7) 0.0021(7) -0.0027(6) C13 0.0327(9) 0.0312(9) 0.0301(9) 0.0118(7) 0.0011(7) -0.0031(7) C14 0.035(1) 0.0267(8) 0.0351(9) 0.0128(7) 0.0032(8) -0.0015(7) C15 0.0288(9) 0.0239(8) 0.0330(9) 0.0074(7) 0.0019(7) -0.0015(6) C16 0.0215(8) 0.0299(9) 0.0271(8) 0.0066(7) 0.0024(6) 0.0012(6) C17 0.0309(9) 0.0345(9) 0.0305(9) 0.0121(7) 0.0007(7) 0.0050(7) C18 0.037(1) 0.0265(9) 0.038(1) 0.0112(7) 0.0036(8) 0.0067(7) C19 0.0300(9) 0.0251(8) 0.0336(9) 0.0060(7) 0.0038(7) 0.0030(7) C20 0.0211(8) 0.0259(8) 0.0290(8) 0.0077(7) 0.0053(6) 0.0012(6) C21 0.0217(8) 0.0264(8) 0.0312(9) 0.0089(7) 0.0026(6) 0.0001(6) C22 0.0432(11) 0.037(1) 0.0275(9) 0.0099(8) -0.0044(8) -0.0038(8) C23 0.0464(11) 0.0404(11) 0.0270(9) 0.0048(8) 0.0013(8) -0.0044(9) C24 0.0396(11) 0.038(1) 0.034(1) -0.0030(8) 0.0025(8) 0.0034(8) C25 0.0409(11) 0.0289(9) 0.0433(11) 0.0019(8) 0.0001(9) 0.0071(8) C26 0.039(1) 0.0299(9) 0.035(1) 0.0088(8) -0.0022(8) -0.0022(7) C27 0.035(1) 0.034(1) 0.0338(9) 0.0068(8) -0.0034(8) -0.0047(8) C28 0.0267(9) 0.041(1) 0.0335(9) 0.0035(8) -0.0032(7) 0.0031(8) C29 0.033(1) 0.039(1) 0.0297(9) 0.0075(8) -0.0022(7) 0.0048(8) C30 0.0336(9) 0.0337(9) 0.0261(8) 0.0023(7) -0.0037(7) 0.0043(7) C31 0.0394(11) 0.0427(11) 0.0288(9) 0.0054(8) -0.0032(8) 0.0085(8) C32 0.0448(12) 0.0673(15) 0.029(1) 0.004(1) -0.0072(9) 0.0227(11) C33 0.0375(12) 0.0732(17) 0.0396(12) -0.0065(11) -0.0113(9) 0.0037(11) C34 0.0400(12) 0.0510(13) 0.0435(12) -0.005(1) -0.0020(9) -0.004(1) C35 0.036(1) 0.038(1) 0.035(1) 0.0008(8) -0.0019(8) 0.0006(8) C36 0.037(1) 0.0274(8) 0.0245(8) 0.0056(7) 0.0004(7) 0.0056(7) C37 0.0444(11) 0.0334(9) 0.0258(9) 0.0071(7) -0.0041(8) 0.0069(8) C38 0.0598(13) 0.0402(11) 0.0210(8) 0.0101(8) 0.0026(8) 0.0163(9) C39 0.0472(12) 0.0428(11) 0.033(1) 0.0163(8) 0.0133(9) 0.0101(9) C40 0.0398(11) 0.0449(11) 0.034(1) 0.0102(8) 0.0039(8) 0.0031(9) C41 0.037(1) 0.037(1) 0.0230(8) 0.0069(7) -0.0001(7) 0.0043(8) C42 0.0292(9) 0.0260(8) 0.0258(8) 0.0072(7) -0.0032(7) 0.0036(6) C43 0.0314(9) 0.0296(9) 0.0319(9) 0.0105(7) 0.0009(7) 0.0029(7) C44 0.0316(9) 0.0228(8) 0.043(1) 0.0049(7) -0.0051(8) 0.0021(7) C45 0.0297(9) 0.036(1) 0.0349(9) -0.0012(8) 0.0015(7) 0.0074(7) C46 0.0311(9) 0.040(1) 0.0288(9) 0.0096(8) 0.0055(7) 0.0057(7) C47 0.0304(9) 0.0278(8) 0.0308(9) 0.0087(7) -0.0022(7) 0.0026(7) C48 0.0318(9) 0.0262(8) 0.0306(9) 0.0089(7) -0.0005(7) 0.0026(7) C49 0.0338(9) 0.0330(9) 0.0299(9) 0.0107(7) 0.0006(7) 0.0048(7) C50 0.0381(11) 0.0449(11) 0.0417(11) 0.0180(9) -0.0066(9) 0.0083(9) C51 0.0420(11) 0.0380(11) 0.0574(13) 0.020(1) -0.002(1) 0.0146(9) C52 0.0430(11) 0.0286(9) 0.0497(12) 0.0028(8) 0.0037(9) 0.0084(8) C53 0.036(1) 0.0305(9) 0.0308(9) 0.0047(7) -0.0026(7) 0.0034(7) C54 0.0668(16) 0.0466(13) 0.0457(13) 0.009(1) -0.0083(11) 0.0035(11) Cl1 0.1087(6) 0.0441(3) 0.0606(4) 0.0080(3) -0.0078(4) 0.0171(3) Cl2 0.2522(15) 0.0780(6) 0.0500(4) 0.0135(4) -0.0119(6) 0.0881(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C1 . 1.402(2) yes N1 . C4 . 1.377(2) yes N1 . C6 . 1.458(2) yes B1 . C30 . 1.646(3) yes B1 . C36 . 1.656(3) yes B1 . C42 . 1.656(3) yes B1 . C48 . 1.662(3) yes F1 . C31 . 1.363(3) yes F2 . C32 . 1.342(3) yes F3 . C33 . 1.340(3) yes F4 . C34 . 1.351(3) yes F5 . C35 . 1.354(3) yes F6 . C37 . 1.360(2) yes F7 . C38 . 1.349(2) yes F8 . C39 . 1.339(2) yes F9 . C40 . 1.345(3) yes F10 . C41 . 1.357(2) yes F11 . C47 . 1.355(2) yes F12 . C46 . 1.346(2) yes F13 . C45 . 1.346(2) yes F14 . C44 . 1.348(2) yes F15 . C43 . 1.349(2) yes F16 . C49 . 1.349(2) yes F17 . C50 . 1.350(2) yes F18 . C51 . 1.348(2) yes F19 . C52 . 1.347(2) yes F20 . C53 . 1.347(2) yes O1 . C1 . 1.204(2) yes O2 . C4 . 1.216(2) yes O3 . C12 . 1.368(2) yes O3 . C22 . 1.431(2) yes O4 . C23 . 1.429(3) yes O4 . C24 . 1.429(2) yes O5 . C25 . 1.428(2) yes O5 . C26 . 1.428(2) yes O6 . C27 . 1.437(2) yes O6 . C28 . 1.424(2) yes O7 . C16 2_575 1.370(2) yes O7 . C29 . 1.437(2) yes C1 . C2 . 1.490(2) yes C2 . C3 . 1.395(2) yes C2 . C5 . 1.386(2) yes C3 . C4 . 1.483(2) yes C3 . C5 2_575 1.383(2) yes C5 . H51 . 1.000 no C6 . C7 . 1.524(3) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C7 . C8 . 1.530(3) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . C9 . 1.527(3) yes C8 . H81 . 1.000 no C8 . H82 . 1.000 no C9 . C10 . 1.515(3) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . C11 . 1.524(3) yes C10 . H101 . 1.000 no C10 . H102 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . C13 . 1.375(3) yes C12 . C20 . 1.431(2) yes C13 . C14 . 1.415(3) yes C13 . H131 . 1.000 no C14 . C15 . 1.365(3) yes C14 . H141 . 1.000 no C15 . C21 . 1.417(2) yes C15 . H151 . 1.000 no C16 . C17 . 1.372(3) yes C16 . C21 . 1.431(2) yes C17 . C18 . 1.408(3) yes C17 . H171 . 1.000 no C18 . C19 . 1.369(3) yes C18 . H181 . 1.000 no C19 . C20 . 1.419(2) yes C19 . H191 . 1.000 no C20 . C21 . 1.422(2) yes C22 . C23 . 1.506(3) yes C22 . H221 . 1.000 no C22 . H222 . 1.000 no C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . C25 . 1.502(3) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . C27 . 1.500(3) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . C29 . 1.504(3) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C30 . C31 . 1.391(3) yes C30 . C35 . 1.392(3) yes C31 . C32 . 1.379(3) yes C32 . C33 . 1.378(4) yes C33 . C34 . 1.366(4) yes C34 . C35 . 1.393(3) yes C36 . C37 . 1.393(2) yes C36 . C41 . 1.392(3) yes C37 . C38 . 1.384(3) yes C38 . C39 . 1.369(3) yes C39 . C40 . 1.381(3) yes C40 . C41 . 1.375(3) yes C42 . C43 . 1.388(2) yes C42 . C47 . 1.390(3) yes C43 . C44 . 1.388(3) yes C44 . C45 . 1.366(3) yes C45 . C46 . 1.381(3) yes C46 . C47 . 1.381(3) yes C48 . C49 . 1.379(3) yes C48 . C53 . 1.389(3) yes C49 . C50 . 1.392(3) yes C50 . C51 . 1.370(3) yes C51 . C52 . 1.375(3) yes C52 . C53 . 1.383(3) yes C54 . Cl1 . 1.740(3) yes C54 . Cl2 . 1.718(3) yes C54 . H541 . 1.000 no C54 . H542 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . N1 . C4 . 111.97(14) yes C1 . N1 . C6 . 122.61(15) yes C4 . N1 . C6 . 125.41(14) yes C30 . B1 . C36 . 114.23(15) yes C30 . B1 . C42 . 103.69(14) yes C36 . B1 . C42 . 111.46(14) yes C30 . B1 . C48 . 113.53(15) yes C36 . B1 . C48 . 101.13(14) yes C42 . B1 . C48 . 113.18(14) yes C12 . O3 . C22 . 116.57(14) yes C23 . O4 . C24 . 111.59(15) yes C25 . O5 . C26 . 113.29(15) yes C27 . O6 . C28 . 110.82(14) yes C16 2_575 O7 . C29 . 117.73(14) yes N1 . C1 . O1 . 124.66(16) yes N1 . C1 . C2 . 105.65(14) yes O1 . C1 . C2 . 129.69(16) yes C1 . C2 . C3 . 107.86(14) yes C1 . C2 . C5 . 129.38(15) yes C3 . C2 . C5 . 122.76(15) yes C2 . C3 . C4 . 107.75(14) yes C2 . C3 . C5 2_575 123.00(16) yes C4 . C3 . C5 2_575 129.24(15) yes N1 . C4 . O2 . 125.33(16) yes N1 . C4 . C3 . 106.70(14) yes O2 . C4 . C3 . 127.96(16) yes C2 . C5 . C3 2_575 114.24(15) yes C2 . C5 . H51 . 122.883 no C3 2_575 C5 . H51 . 122.877 no N1 . C6 . C7 . 112.86(15) yes N1 . C6 . H61 . 108.622 no C7 . C6 . H61 . 108.620 no N1 . C6 . H62 . 108.619 no C7 . C6 . H62 . 108.615 no H61 . C6 . H62 . 109.465 no C6 . C7 . C8 . 110.05(16) yes C6 . C7 . H71 . 109.324 no C8 . C7 . H71 . 109.329 no C6 . C7 . H72 . 109.328 no C8 . C7 . H72 . 109.330 no H71 . C7 . H72 . 109.465 no C7 . C8 . C9 . 113.91(17) yes C7 . C8 . H81 . 108.356 no C9 . C8 . H81 . 108.350 no C7 . C8 . H82 . 108.356 no C9 . C8 . H82 . 108.350 no H81 . C8 . H82 . 109.465 no C8 . C9 . C10 . 114.97(17) yes C8 . C9 . H91 . 108.079 no C10 . C9 . H91 . 108.082 no C8 . C9 . H92 . 108.076 no C10 . C9 . H92 . 108.080 no H91 . C9 . H92 . 109.469 no C9 . C10 . C11 . 112.2(2) yes C9 . C10 . H101 . 108.789 no C11 . C10 . H101 . 108.793 no C9 . C10 . H102 . 108.793 no C11 . C10 . H102 . 108.794 no H101 . C10 . H102 . 109.466 no C10 . C11 . H111 . 109.462 no C10 . C11 . H112 . 109.465 no H111 . C11 . H112 . 109.472 no C10 . C11 . H113 . 109.467 no H111 . C11 . H113 . 109.479 no H112 . C11 . H113 . 109.481 no O3 . C12 . C13 . 124.54(16) yes O3 . C12 . C20 . 114.54(15) yes C13 . C12 . C20 . 120.92(16) yes C12 . C13 . C14 . 119.62(17) yes C12 . C13 . H131 . 120.190 no C14 . C13 . H131 . 120.193 no C13 . C14 . C15 . 121.30(16) yes C13 . C14 . H141 . 119.347 no C15 . C14 . H141 . 119.349 no C14 . C15 . C21 . 120.01(16) yes C14 . C15 . H151 . 119.994 no C21 . C15 . H151 . 119.994 no O7 2_575 C16 . C17 . 125.38(16) yes O7 2_575 C16 . C21 . 113.67(15) yes C17 . C16 . C21 . 120.93(16) yes C16 . C17 . C18 . 119.60(17) yes C16 . C17 . H171 . 120.201 no C18 . C17 . H171 . 120.203 no C17 . C18 . C19 . 121.73(16) yes C17 . C18 . H181 . 119.138 no C19 . C18 . H181 . 119.131 no C18 . C19 . C20 . 119.60(17) yes C18 . C19 . H191 . 120.201 no C20 . C19 . H191 . 120.200 no C12 . C20 . C19 . 122.01(16) yes C12 . C20 . C21 . 118.13(15) yes C19 . C20 . C21 . 119.84(16) yes C15 . C21 . C16 . 121.73(16) yes C15 . C21 . C20 . 119.98(16) yes C16 . C21 . C20 . 118.28(15) yes O3 . C22 . C23 . 108.86(16) yes O3 . C22 . H221 . 109.630 no C23 . C22 . H221 . 109.626 no O3 . C22 . H222 . 109.624 no C23 . C22 . H222 . 109.619 no H221 . C22 . H222 . 109.464 no O4 . C23 . C22 . 110.42(16) yes O4 . C23 . H231 . 109.231 no C22 . C23 . H231 . 109.230 no O4 . C23 . H232 . 109.239 no C22 . C23 . H232 . 109.240 no H231 . C23 . H232 . 109.468 no O4 . C24 . C25 . 107.30(16) yes O4 . C24 . H241 . 110.017 no C25 . C24 . H241 . 110.006 no O4 . C24 . H242 . 110.013 no C25 . C24 . H242 . 110.010 no H241 . C24 . H242 . 109.465 no O5 . C25 . C24 . 106.98(16) yes O5 . C25 . H251 . 110.084 no C24 . C25 . H251 . 110.090 no O5 . C25 . H252 . 110.094 no C24 . C25 . H252 . 110.097 no H251 . C25 . H252 . 109.472 no O5 . C26 . C27 . 108.02(15) yes O5 . C26 . H261 . 109.838 no C27 . C26 . H261 . 109.832 no O5 . C26 . H262 . 109.836 no C27 . C26 . H262 . 109.835 no H261 . C26 . H262 . 109.459 no O6 . C27 . C26 . 107.75(15) yes O6 . C27 . H271 . 109.892 no C26 . C27 . H271 . 109.902 no O6 . C27 . H272 . 109.902 no C26 . C27 . H272 . 109.905 no H271 . C27 . H272 . 109.468 no O6 . C28 . C29 . 111.29(15) yes O6 . C28 . H281 . 109.013 no C29 . C28 . H281 . 109.014 no O6 . C28 . H282 . 109.017 no C29 . C28 . H282 . 109.017 no H281 . C28 . H282 . 109.465 no O7 . C29 . C28 . 108.00(16) yes O7 . C29 . H291 . 109.836 no C28 . C29 . H291 . 109.832 no O7 . C29 . H292 . 109.845 no C28 . C29 . H292 . 109.838 no H291 . C29 . H292 . 109.466 no B1 . C30 . C31 . 119.16(17) yes B1 . C30 . C35 . 127.73(17) yes C31 . C30 . C35 . 112.97(18) yes F1 . C31 . C30 . 118.92(18) yes F1 . C31 . C32 . 116.27(19) yes C30 . C31 . C32 . 124.8(2) yes F2 . C32 . C31 . 120.2(2) yes F2 . C32 . C33 . 120.4(2) yes C31 . C32 . C33 . 119.4(2) yes F3 . C33 . C32 . 119.7(2) yes F3 . C33 . C34 . 121.3(3) yes C32 . C33 . C34 . 119.0(2) yes F4 . C34 . C33 . 120.3(2) yes F4 . C34 . C35 . 119.9(2) yes C33 . C34 . C35 . 119.8(2) yes F5 . C35 . C30 . 121.35(17) yes F5 . C35 . C34 . 114.65(19) yes C30 . C35 . C34 . 124.0(2) yes B1 . C36 . C37 . 128.39(17) yes B1 . C36 . C41 . 118.93(15) yes C37 . C36 . C41 . 112.45(17) yes F6 . C37 . C36 . 120.44(18) yes F6 . C37 . C38 . 115.47(17) yes C36 . C37 . C38 . 124.08(19) yes F7 . C38 . C37 . 119.8(2) yes F7 . C38 . C39 . 119.80(19) yes C37 . C38 . C39 . 120.42(18) yes F8 . C39 . C38 . 121.09(19) yes F8 . C39 . C40 . 120.6(2) yes C38 . C39 . C40 . 118.31(19) yes F9 . C40 . C39 . 120.05(19) yes F9 . C40 . C41 . 120.64(18) yes C39 . C40 . C41 . 119.3(2) yes F10 . C41 . C36 . 119.11(16) yes F10 . C41 . C40 . 115.50(17) yes C36 . C41 . C40 . 125.36(18) yes B1 . C42 . C43 . 127.16(16) yes B1 . C42 . C47 . 119.93(15) yes C43 . C42 . C47 . 112.89(16) yes F15 . C43 . C42 . 121.74(16) yes F15 . C43 . C44 . 114.27(16) yes C42 . C43 . C44 . 123.99(17) yes F14 . C44 . C43 . 120.33(18) yes F14 . C44 . C45 . 119.78(17) yes C43 . C44 . C45 . 119.89(17) yes F13 . C45 . C44 . 120.16(18) yes F13 . C45 . C46 . 120.72(18) yes C44 . C45 . C46 . 119.12(17) yes F12 . C46 . C45 . 120.08(18) yes F12 . C46 . C47 . 121.24(18) yes C45 . C46 . C47 . 118.66(17) yes F11 . C47 . C42 . 119.08(16) yes F11 . C47 . C46 . 115.74(16) yes C42 . C47 . C46 . 125.15(17) yes B1 . C48 . C49 . 127.36(16) yes B1 . C48 . C53 . 118.21(16) yes C49 . C48 . C53 . 114.04(16) yes F16 . C49 . C48 . 121.86(16) yes F16 . C49 . C50 . 114.30(17) yes C48 . C49 . C50 . 123.83(18) yes F17 . C50 . C49 . 120.3(2) yes F17 . C50 . C51 . 120.20(18) yes C49 . C50 . C51 . 119.46(19) yes F18 . C51 . C50 . 120.2(2) yes F18 . C51 . C52 . 120.5(2) yes C50 . C51 . C52 . 119.28(18) yes F19 . C52 . C51 . 119.82(19) yes F19 . C52 . C53 . 120.8(2) yes C51 . C52 . C53 . 119.33(19) yes F20 . C53 . C48 . 119.47(16) yes F20 . C53 . C52 . 116.51(17) yes C48 . C53 . C52 . 124.03(18) yes Cl1 . C54 . Cl2 . 113.01(14) yes Cl1 . C54 . H541 . 108.582 no Cl2 . C54 . H541 . 108.585 no Cl1 . C54 . H542 . 108.576 no Cl2 . C54 . H542 . 108.581 no H541 . C54 . H542 . 109.468 no #===END ############################## ## denoted [Li21]I2 in text ## ############################## data_3 _database_code_depnum_ccdc_archive 'CCDC 254112' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 7.566(1) _cell_angle_alpha 72.355(2) _cell_length_b 10.3074(14) _cell_angle_beta 88.102(2) _cell_length_c 15.598(2) _cell_angle_gamma 81.429(2) _cell_volume 1146.2(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'Li ' -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'I ' -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C38 H56 I2 Li2 O14 ' _chemical_formula_moiety ' C38 H56 I2 Li2 O14 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1004.55 _cell_measurement_reflns_used 8794 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 29.15 _cell_measurement_temperature 150(2) _exptl_crystal_description ' colourless ' _exptl_crystal_colour ' needle ' _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 508.000 _exptl_absorpt_coefficient_mu 1.430 # Sheldrick geometric definitions 1.00 1.00 _diffrn_measurement_device_type ; Bruker AXS SMART 1K CCD diffractometer ; _diffrn_radiation_monochromator 'silicon 111' _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; Bruker SAINT version 6.36a (Bruker, 2002) ; _computing_cell_refinement ; Bruker SAINT version 6.36a (Bruker, 2002) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_measurement_method 'thin slice \w-scans' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by CRYSTALS. ; _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 11642 _reflns_number_total 6117 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 6117 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6784 _diffrn_reflns_theta_min 2.033 _diffrn_reflns_theta_max 29.252 _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 23.402 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -0.54 _refine_diff_density_max 1.40 _refine_ls_number_reflns 5650 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 #_refine_ls_R_factor_ref 0.0342 _refine_ls_wR_factor_ref 0.0367 _refine_ls_goodness_of_fit_ref 0.9607 #_reflns_number_all 6098 _refine_ls_R_factor_all 0.0360 _refine_ls_wR_factor_all 0.0435 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5650 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_gt 0.0367 _refine_ls_shift/su_max 0.007556 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 A~i~ are: 0.228 0.242 0.862E-01 ; _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.6923 _diffrn_radiation_source 'Daresbury SRS, Station 9.8' ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags _atom_site_attached_hydrogens Li1 Li 0.1481(5) 0.0117(4) 0.1982(3) 0.0313 1.0000 Uani . . I1 I -0.420306(19) -0.292697(14) 0.068244(9) 0.0302 1.0000 Uani . . O1 O 0.25839(19) 0.35018(16) 0.25472(9) 0.0256 1.0000 Uani . . O2 O 0.0313(2) 0.26884(15) 0.1455(1) 0.0266 1.0000 Uani . . O3 O -0.09666(18) 0.03126(14) 0.1505(1) 0.0260 1.0000 Uani . . O4 O 0.10593(18) -0.19847(14) 0.25279(9) 0.0236 1.0000 Uani . . O5 O 0.37054(19) -0.31515(16) 0.40412(9) 0.0271 1.0000 Uani . . O6 O 0.1856(3) 0.06015(18) 0.30541(11) 0.0428 1.0000 Uani . . O7 O 0.3354(2) 0.00659(18) 0.11370(12) 0.0368 1.0000 Uani . . C1 C 0.4057(3) 0.34790(19) 0.30459(13) 0.0230 1.0000 Uani . . C2 C 0.5732(3) 0.3620(2) 0.27006(13) 0.0262 1.0000 Uani . . C3 C 0.7157(3) 0.3585(2) 0.32670(14) 0.0296 1.0000 Uani . . C4 C 0.6905(3) 0.3417(2) 0.41693(14) 0.0273 1.0000 Uani . . C5 C 0.4835(3) 0.3169(2) 0.54613(13) 0.0238 1.0000 Uani . . C6 C 0.3140(3) 0.3091(2) 0.57975(13) 0.0288 1.0000 Uani . . C7 C 0.1713(3) 0.3134(3) 0.52263(15) 0.0320 1.0000 Uani . . C8 C 0.1979(3) 0.3234(2) 0.43392(14) 0.0275 1.0000 Uani . . C9 C 0.3723(2) 0.33144(19) 0.39768(12) 0.0219 1.0000 Uani . . C10 C 0.5173(2) 0.32899(19) 0.45372(12) 0.0223 1.0000 Uani . . C11 C 0.2857(3) 0.3737(2) 0.15979(13) 0.0261 1.0000 Uani . . C12 C 0.1079(3) 0.3925(2) 0.11480(13) 0.0263 1.0000 Uani . . C13 C -0.1194(3) 0.2740(2) 0.09155(14) 0.0276 1.0000 Uani . . C14 C -0.2172(3) 0.1558(2) 0.13943(17) 0.0315 1.0000 Uani . . C15 C -0.1802(3) -0.0857(2) 0.19608(17) 0.0314 1.0000 Uani . . C16 C -0.0441(3) -0.2101(2) 0.20371(15) 0.0280 1.0000 Uani . . C17 C 0.2335(3) -0.3208(2) 0.26964(13) 0.0250 1.0000 Uani . . C18 C 0.4016(3) -0.3044(2) 0.31139(13) 0.0261 1.0000 Uani . . C19 C 0.1426(9) 0.0018(4) 0.3948(2) 0.0880 1.0000 Uani . . H1 H 0.2355 -0.0001 0.1181 0.0461 1.0000 Uiso . . H2 H 0.3555 0.0583 0.0700 0.0500 1.0000 Uiso . . H3 H 0.2080 0.1337 0.3022 0.0500 1.0000 Uiso . . H21 H 0.5940 0.3747 0.2046 0.0313 1.0000 Uiso . . H31 H 0.8375 0.3685 0.3009 0.0345 1.0000 Uiso . . H41 H 0.7935 0.3385 0.4564 0.0320 1.0000 Uiso . . H61 H 0.2919 0.3003 0.6447 0.0337 1.0000 Uiso . . H71 H 0.0481 0.3090 0.5475 0.0383 1.0000 Uiso . . H81 H 0.0952 0.3251 0.3947 0.0328 1.0000 Uiso . . H111 H 0.3435 0.4583 0.1345 0.0309 1.0000 Uiso . . H112 H 0.3643 0.2929 0.1496 0.0309 1.0000 Uiso . . H121 H 0.0265 0.4685 0.1295 0.0306 1.0000 Uiso . . H122 H 0.1240 0.4167 0.0482 0.0306 1.0000 Uiso . . H131 H -0.2003 0.3632 0.0830 0.0313 1.0000 Uiso . . H132 H -0.0787 0.2656 0.0316 0.0313 1.0000 Uiso . . H141 H -0.2573 0.1638 0.1996 0.0363 1.0000 Uiso . . H142 H -0.3235 0.1565 0.1028 0.0363 1.0000 Uiso . . H151 H -0.2184 -0.0816 0.2573 0.0374 1.0000 Uiso . . H152 H -0.2867 -0.0888 0.1609 0.0374 1.0000 Uiso . . H161 H -0.0956 -0.2953 0.2364 0.0342 1.0000 Uiso . . H162 H -0.0063 -0.2141 0.1424 0.0342 1.0000 Uiso . . H171 H 0.1806 -0.3993 0.3115 0.0293 1.0000 Uiso . . H172 H 0.2633 -0.3406 0.2115 0.0293 1.0000 Uiso . . H181 H 0.5000 -0.3781 0.3066 0.0305 1.0000 Uiso . . H182 H 0.4363 -0.2121 0.2793 0.0305 1.0000 Uiso . . H191 H 0.1126 -0.0925 0.4032 0.1037 1.0000 Uiso . . H192 H 0.2469 -0.0044 0.4343 0.1037 1.0000 Uiso . . H193 H 0.0373 0.0603 0.4111 0.1037 1.0000 Uiso . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0247(16) 0.042(2) 0.0276(17) -0.0103(15) -0.0020(13) -0.0060(14) I1 0.03560(8) 0.02762(8) 0.02669(8) -0.00653(5) 0.00329(5) -0.00694(5) O1 0.0264(7) 0.0322(7) 0.0184(6) -0.0059(5) -0.0028(5) -0.0080(5) O2 0.0269(7) 0.0237(6) 0.0248(6) -0.0002(5) -0.0086(5) -0.0035(5) O3 0.0211(6) 0.0216(6) 0.0339(7) -0.0067(5) -0.0042(5) -0.0010(5) O4 0.0227(6) 0.0223(6) 0.0256(6) -0.0073(5) -0.0048(5) -0.0011(5) O5 0.0233(6) 0.0373(8) 0.0185(6) -0.0055(5) -0.0039(5) -0.0028(5) O6 0.0737(13) 0.0284(8) 0.0268(8) -0.0050(6) -0.0060(8) -0.0147(8) O7 0.0342(8) 0.0323(8) 0.0367(8) -0.0019(7) 0.0105(7) -0.0032(6) C1 0.0253(9) 0.0217(8) 0.0212(8) -0.0050(6) -0.0036(6) -0.0030(6) C2 0.0270(9) 0.0290(9) 0.0224(8) -0.0083(7) 0.0013(7) -0.0022(7) C3 0.0217(9) 0.0393(11) 0.0253(9) -0.0076(8) 0.0017(7) -0.0018(7) C4 0.0188(8) 0.037(1) 0.0245(9) -0.0073(8) -0.0027(6) -0.0016(7) C5 0.0216(8) 0.0271(9) 0.0204(8) -0.0036(7) -0.0043(6) -0.0026(7) C6 0.0253(9) 0.0376(11) 0.0213(8) -0.0048(8) 0.0015(7) -0.0063(8) C7 0.0243(9) 0.0443(12) 0.027(1) -0.0077(8) 0.0023(7) -0.0105(8) C8 0.0222(9) 0.034(1) 0.0254(9) -0.0065(8) -0.0020(7) -0.0078(7) C9 0.0218(8) 0.0232(8) 0.0198(8) -0.0044(6) -0.0010(6) -0.0048(6) C10 0.0194(8) 0.0240(8) 0.0211(8) -0.0044(6) -0.0018(6) -0.0009(6) C11 0.0297(9) 0.0289(9) 0.0186(8) -0.0039(7) -0.0027(7) -0.0069(7) C12 0.0295(9) 0.0252(9) 0.0219(8) -0.0032(7) -0.0052(7) -0.0043(7) C13 0.0232(9) 0.0257(9) 0.0295(9) -0.0026(7) -0.0113(7) 0.0009(7) C14 0.0237(9) 0.0228(9) 0.0442(12) -0.0065(8) -0.0055(8) 0.0016(7) C15 0.0204(9) 0.0247(9) 0.0483(12) -0.0093(8) -0.0039(8) -0.0038(7) C16 0.0257(9) 0.0256(9) 0.034(1) -0.0102(8) -0.0057(7) -0.0043(7) C17 0.0250(9) 0.0236(8) 0.0246(9) -0.0066(7) -0.0054(7) 0.0018(7) C18 0.0274(9) 0.0306(9) 0.0182(8) -0.0052(7) -0.0034(6) -0.0016(7) C19 0.186(5) 0.0365(16) 0.0368(16) -0.0072(13) 0.014(2) -0.012(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 . C11 . 1.439(2) yes O1 . C1 . 1.374(2) yes O2 . C13 . 1.424(2) yes O2 . C12 . 1.422(2) yes O3 . C15 . 1.427(2) yes O3 . C14 . 1.427(2) yes O4 . C17 . 1.430(2) yes O4 . C16 . 1.429(2) yes O5 . C18 . 1.431(2) yes O5 . C5 2_656 1.366(2) yes O6 . H3 . 0.788 no O6 . C19 . 1.389(4) yes O7 . H2 . 0.755 no O7 . H1 . 0.768 no C1 . C9 . 1.428(3) yes C1 . C2 . 1.371(3) yes C2 . H21 . 1.000 no C2 . C3 . 1.406(3) yes C3 . H31 . 1.000 no C3 . C4 . 1.375(3) yes C4 . H41 . 1.000 no C4 . C10 . 1.421(3) yes C5 . C10 . 1.426(3) yes C5 . C6 . 1.374(3) yes C6 . H61 . 1.000 no C6 . C7 . 1.410(3) yes C7 . H71 . 1.000 no C7 . C8 . 1.366(3) yes C8 . H81 . 1.000 no C8 . C9 . 1.422(3) yes C9 . C10 . 1.417(3) yes C11 . H112 . 1.000 no C11 . H111 . 1.000 no C11 . C12 . 1.498(3) yes C12 . H122 . 1.000 no C12 . H121 . 1.000 no C13 . H132 . 1.000 no C13 . H131 . 1.000 no C13 . C14 . 1.507(3) yes C14 . H142 . 1.000 no C14 . H141 . 1.000 no C15 . H152 . 1.000 no C15 . H151 . 1.000 no C15 . C16 . 1.497(3) yes C16 . H162 . 1.000 no C16 . H161 . 1.000 no C17 . H172 . 1.000 no C17 . H171 . 1.000 no C17 . C18 . 1.502(3) yes C18 . H182 . 1.000 no C18 . H181 . 1.000 no C19 . H193 . 1.000 no C19 . H192 . 1.000 no C19 . H191 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 . O1 . C1 . 116.08(15) yes C13 . O2 . C12 . 111.19(15) yes C15 . O3 . C14 . 111.00(16) yes C17 . O4 . C16 . 110.06(15) yes C18 . O5 . C5 2_656 116.13(15) yes H3 . O6 . C19 . 105.637 no H2 . O7 . H1 . 112.033 no C9 . C1 . C2 . 120.97(17) yes C9 . C1 . O1 . 114.74(16) yes C2 . C1 . O1 . 124.28(17) yes H21 . C2 . C3 . 119.990 no H21 . C2 . C1 . 119.990 no C3 . C2 . C1 . 120.02(18) yes H31 . C3 . C4 . 119.429 no H31 . C3 . C2 . 119.429 no C4 . C3 . C2 . 121.14(18) yes H41 . C4 . C10 . 120.169 no H41 . C4 . C3 . 120.169 no C10 . C4 . C3 . 119.66(18) yes C10 . C5 . C6 . 120.68(17) yes C10 . C5 . O5 2_656 115.16(16) yes C6 . C5 . O5 2_656 124.15(18) yes H61 . C6 . C7 . 120.038 no H61 . C6 . C5 . 120.037 no C7 . C6 . C5 . 119.92(19) yes H71 . C7 . C8 . 119.323 no H71 . C7 . C6 . 119.323 no C8 . C7 . C6 . 121.35(19) yes H81 . C8 . C9 . 120.160 no H81 . C8 . C7 . 120.160 no C9 . C8 . C7 . 119.68(18) yes C10 . C9 . C8 . 119.85(17) yes C10 . C9 . C1 . 118.28(17) yes C8 . C9 . C1 . 121.82(17) yes C9 . C10 . C4 . 119.92(17) yes C9 . C10 . C5 . 118.49(17) yes C4 . C10 . C5 . 121.57(17) yes H112 . C11 . H111 . 109.467 no H112 . C11 . C12 . 109.688 no H111 . C11 . C12 . 109.688 no H112 . C11 . O1 . 109.688 no H111 . C11 . O1 . 109.688 no C12 . C11 . O1 . 108.61(16) yes H122 . C12 . H121 . 109.467 no H122 . C12 . O2 . 109.353 no H121 . C12 . O2 . 109.354 no H122 . C12 . C11 . 109.354 no H121 . C12 . C11 . 109.354 no O2 . C12 . C11 . 109.95(16) yes H132 . C13 . H131 . 109.466 no H132 . C13 . C14 . 109.818 no H131 . C13 . C14 . 109.818 no H132 . C13 . O2 . 109.818 no H131 . C13 . O2 . 109.818 no C14 . C13 . O2 . 108.08(16) yes H142 . C14 . H141 . 109.467 no H142 . C14 . O3 . 109.882 no H141 . C14 . O3 . 109.881 no H142 . C14 . C13 . 109.882 no H141 . C14 . C13 . 109.881 no O3 . C14 . C13 . 107.83(17) yes H152 . C15 . H151 . 109.466 no H152 . C15 . C16 . 110.137 no H151 . C15 . C16 . 110.137 no H152 . C15 . O3 . 110.136 no H151 . C15 . O3 . 110.136 no C16 . C15 . O3 . 106.80(17) yes H162 . C16 . H161 . 109.467 no H162 . C16 . O4 . 109.947 no H161 . C16 . O4 . 109.947 no H162 . C16 . C15 . 109.948 no H161 . C16 . C15 . 109.948 no O4 . C16 . C15 . 107.56(16) yes H172 . C17 . H171 . 109.466 no H172 . C17 . C18 . 109.113 no H171 . C17 . C18 . 109.113 no H172 . C17 . O4 . 109.113 no H171 . C17 . O4 . 109.113 no C18 . C17 . O4 . 110.90(16) yes H182 . C18 . H181 . 109.466 no H182 . C18 . O5 . 109.550 no H181 . C18 . O5 . 109.550 no H182 . C18 . C17 . 109.550 no H181 . C18 . C17 . 109.550 no O5 . C18 . C17 . 109.16(16) yes H193 . C19 . H192 . 109.476 no H193 . C19 . H191 . 109.479 no H192 . C19 . H191 . 109.474 no H193 . C19 . O6 . 109.468 no H192 . C19 . O6 . 109.463 no H191 . C19 . O6 . 109.467 no #===END ################################ ## denoted [Na212]I2 in text ## ################################ data_4 _database_code_depnum_ccdc_archive 'CCDC 254113' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.8071(2) _cell_angle_alpha 78.4706(8) _cell_length_b 11.2503(2) _cell_angle_beta 81.8524(7) _cell_length_c 18.3062(3) _cell_angle_gamma 86.3758(12) _cell_volume 2157.41(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Na ' 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 International_Tables_Vol_IV_Table_2.2B 'I ' -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 1 _chemical_formula_sum ' C64 H78 Cl18 I2 N2 Na2 O14 ' _chemical_formula_moiety 'C58 H72 I2 N2 Na2 O14, 6(C H Cl3)' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 2037.16 _cell_measurement_reflns_used 24277 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 180 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1022 _exptl_absorpt_coefficient_mu 1.352 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.87 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 21614 _reflns_number_total 9407 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 9407 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9528 _diffrn_reflns_theta_min 5.150 _diffrn_reflns_theta_max 27.111 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.026 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -0.86 _refine_diff_density_max 1.18 _refine_ls_number_reflns 8041 _refine_ls_number_restraints 0 _refine_ls_number_parameters 460 #_refine_ls_R_factor_ref 0.0344 _refine_ls_wR_factor_ref 0.0444 _refine_ls_goodness_of_fit_ref 1.0757 #_reflns_number_all 9407 _refine_ls_R_factor_all 0.0421 _refine_ls_wR_factor_all 0.0461 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 8041 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_gt 0.0444 _refine_ls_shift/su_max 0.003699 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.54 0.427 1.11 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Na1 Na 0.95129(9) 0.24841(9) 0.26250(5) 0.0348 1.0000 Uani . . . . . . I2 I 1.233837(15) 0.239889(15) 0.253379(9) 0.0375 1.0000 Uani . . . . . . C1 C 1.0536(3) 0.5544(2) 0.27363(16) 0.0429 1.0000 Uani . . . . . . C2 C 0.9666(3) 0.5099(3) 0.34391(17) 0.0484 1.0000 Uani . . . . . . C3 C 0.8146(3) 0.3687(3) 0.40215(16) 0.0499 1.0000 Uani . . . . . . C4 C 0.7314(3) 0.2772(3) 0.38828(18) 0.0514 1.0000 Uani . . . . . . C5 C 0.7336(3) 0.0873(3) 0.35102(18) 0.0547 1.0000 Uani . . . . . . C6 C 0.8204(3) -0.0070(3) 0.32296(17) 0.0529 1.0000 Uani . . . . . . C7 C 0.9559(3) -0.0424(2) 0.21582(16) 0.0432 1.0000 Uani . . . . . . C8 C 1.0451(3) 0.0156(2) 0.15002(15) 0.0385 1.0000 Uani . . . . . . C9 C 1.2270(2) 0.1998(2) -0.05645(16) 0.0402 1.0000 Uani . . . . . . C10 C 1.1686(2) 0.1381(2) 0.01323(15) 0.0385 1.0000 Uani . . . . . . C11 C 1.0402(2) 0.1392(2) 0.02815(14) 0.0342 1.0000 Uani . . . . . . C12 C 0.9649(2) 0.2024(2) -0.02647(13) 0.0313 1.0000 Uani . . . . . . C13 C 0.8324(2) 0.2048(2) -0.01264(15) 0.0349 1.0000 Uani . . . . . . C14 C 1.2357(2) 0.7325(2) 0.06624(16) 0.0390 1.0000 Uani . . . . . . C15 C 1.1772(2) 0.6704(2) 0.13587(16) 0.0382 1.0000 Uani . . . . . . C16 C 1.0490(2) 0.6723(2) 0.15075(14) 0.0345 1.0000 Uani . . . . . . C17 C 0.9738(2) 0.7351(2) 0.09604(14) 0.0320 1.0000 Uani . . . . . . C18 C 0.8408(2) 0.7377(2) 0.11020(15) 0.0363 1.0000 Uani . . . . . . C19 C 0.8160(2) 0.3953(2) 0.11695(14) 0.0317 1.0000 Uani . . . . . . C20 C 0.7358(2) 0.5111(2) 0.01423(14) 0.0322 1.0000 Uani . . . . . . C21 C 0.8750(2) 0.5149(2) -0.00098(13) 0.0294 1.0000 Uani . . . . . . C22 C 0.9231(2) 0.4444(2) 0.06085(13) 0.0289 1.0000 Uani . . . . . . C23 C 1.0509(2) 0.4276(2) 0.06421(13) 0.0313 1.0000 Uani . . . . . . C24 C 0.5809(2) 0.4029(2) 0.11790(15) 0.0378 1.0000 Uani . . . . . . C25 C 0.5080(2) 0.4980(2) 0.15627(16) 0.0403 1.0000 Uani . . . . . . C26 C 0.5552(3) 0.5091(3) 0.22886(16) 0.0437 1.0000 Uani . . . . . . C27 C 0.4804(3) 0.6015(3) 0.2687(2) 0.0551 1.0000 Uani . . . . . . C28 C 0.5332(3) 0.6178(3) 0.3388(2) 0.0593 1.0000 Uani . . . . . . C29 C 0.6533(4) 0.6842(4) 0.3208(2) 0.0727 1.0000 Uani . . . . . . C30 C 0.7476(4) -0.2959(4) 0.55045(19) 0.0619 1.0000 Uani . . . . . . C31 C 0.7551(3) 0.0714(3) 0.62462(18) 0.0486 1.0000 Uani . . . . . . C32 C 0.5230(3) -0.0608(3) 0.85346(18) 0.0470 1.0000 Uani . . . . . . N1 N 0.70826(18) 0.43800(18) 0.08563(11) 0.0318 1.0000 Uani . . . . . . O1 O 0.81862(16) 0.32986(16) 0.17842(10) 0.0380 1.0000 Uani . . . . . . O2 O 0.65904(16) 0.55865(18) -0.02487(11) 0.0427 1.0000 Uani . . . . . . O3 O 0.89415(19) 0.41407(17) 0.33404(10) 0.0417 1.0000 Uani . . . . . . O4 O 0.98261(18) 0.61625(17) 0.21656(11) 0.0408 1.0000 Uani . . . . . . O5 O 0.80648(17) 0.17915(18) 0.36607(10) 0.0402 1.0000 Uani . . . . . . O6 O 0.97417(17) 0.08364(17) 0.09430(10) 0.0393 1.0000 Uani . . . . . . O7 O 0.89393(19) 0.04700(16) 0.25477(10) 0.0409 1.0000 Uani . . . . . . Cl1 Cl 0.60535(11) 0.07307(9) 0.83644(8) 0.0821 1.0000 Uani . . . . . . Cl2 Cl 0.37467(9) -0.03844(11) 0.82313(6) 0.0770 1.0000 Uani . . . . . . Cl3 Cl 0.50406(11) -0.12445(14) 0.94876(7) 0.0961 1.0000 Uani . . . . . . Cl4 Cl 0.59864(10) 0.07769(11) 0.60912(9) 0.0912 1.0000 Uani . . . . . . Cl5 Cl 0.85395(12) 0.03377(12) 0.54816(7) 0.0884 1.0000 Uani . . . . . . Cl6 Cl 0.79631(11) 0.21141(9) 0.64174(8) 0.0792 1.0000 Uani . . . . . . Cl7 Cl 0.88412(9) -0.26106(9) 0.48701(5) 0.0661 1.0000 Uani . . . . . . Cl8 Cl 0.62039(11) -0.20813(15) 0.51540(8) 0.0991 1.0000 Uani . . . . . . Cl9 Cl 0.72480(15) -0.45181(12) 0.56355(8) 0.1006 1.0000 Uani . . . . . . H11 H 1.1134 0.6113 0.2841 0.0527 1.0000 Uiso . . . . . . H12 H 1.1014 0.4838 0.2563 0.0527 1.0000 Uiso . . . . . . H21 H 1.0166 0.4795 0.3863 0.0591 1.0000 Uiso . . . . . . H22 H 0.9092 0.5785 0.3561 0.0591 1.0000 Uiso . . . . . . H31 H 0.8669 0.3299 0.4419 0.0589 1.0000 Uiso . . . . . . H32 H 0.7625 0.4373 0.4192 0.0589 1.0000 Uiso . . . . . . H41 H 0.6742 0.2468 0.4354 0.0598 1.0000 Uiso . . . . . . H42 H 0.6806 0.3152 0.3475 0.0598 1.0000 Uiso . . . . . . H51 H 0.6804 0.0497 0.3982 0.0659 1.0000 Uiso . . . . . . H52 H 0.6789 0.1239 0.3120 0.0659 1.0000 Uiso . . . . . . H61 H 0.8765 -0.0418 0.3615 0.0631 1.0000 Uiso . . . . . . H62 H 0.7708 -0.0731 0.3133 0.0631 1.0000 Uiso . . . . . . H71 H 1.0032 -0.1017 0.2510 0.0531 1.0000 Uiso . . . . . . H72 H 0.8922 -0.0860 0.1975 0.0531 1.0000 Uiso . . . . . . H81 H 1.0997 0.0710 0.1665 0.0480 1.0000 Uiso . . . . . . H82 H 1.0982 -0.0485 0.1286 0.0480 1.0000 Uiso . . . . . . H91 H 1.3204 0.1977 -0.0668 0.0494 1.0000 Uiso . . . . . . H101 H 1.2203 0.0935 0.0519 0.0475 1.0000 Uiso . . . . . . H131 H 0.7889 0.1606 0.0362 0.0430 1.0000 Uiso . . . . . . H141 H 1.3291 0.7307 0.0558 0.0484 1.0000 Uiso . . . . . . H151 H 1.2289 0.6250 0.1743 0.0473 1.0000 Uiso . . . . . . H181 H 0.7973 0.6939 0.1592 0.0443 1.0000 Uiso . . . . . . H231 H 1.0861 0.3779 0.1087 0.0393 1.0000 Uiso . . . . . . H241 H 0.5857 0.3257 0.1557 0.0462 1.0000 Uiso . . . . . . H242 H 0.5353 0.3891 0.0766 0.0462 1.0000 Uiso . . . . . . H251 H 0.5150 0.5783 0.1210 0.0474 1.0000 Uiso . . . . . . H252 H 0.4183 0.4756 0.1680 0.0474 1.0000 Uiso . . . . . . H261 H 0.6442 0.5337 0.2169 0.0524 1.0000 Uiso . . . . . . H262 H 0.5505 0.4281 0.2635 0.0524 1.0000 Uiso . . . . . . H271 H 0.4804 0.6814 0.2330 0.0659 1.0000 Uiso . . . . . . H272 H 0.3926 0.5741 0.2837 0.0659 1.0000 Uiso . . . . . . H281 H 0.4701 0.6649 0.3683 0.0714 1.0000 Uiso . . . . . . H282 H 0.5490 0.5359 0.3699 0.0714 1.0000 Uiso . . . . . . H291 H 0.6838 0.6924 0.3686 0.0894 1.0000 Uiso . . . . . . H292 H 0.6387 0.7667 0.2901 0.0894 1.0000 Uiso . . . . . . H293 H 0.7175 0.6377 0.2917 0.0894 1.0000 Uiso . . . . . . H301 H 0.7552 -0.2760 0.6004 0.0757 1.0000 Uiso . . . . . . H311 H 0.7649 0.0068 0.6699 0.0576 1.0000 Uiso . . . . . . H321 H 0.5743 -0.1165 0.8239 0.0571 1.0000 Uiso . . . . . . 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 0.0338(5) 0.0349(5) 0.0344(5) -0.0025(4) -0.0049(4) -0.0032(4) I2 0.03553(9) 0.03604(9) 0.04163(10) -0.01058(6) -0.00462(6) 0.00178(6) C1 0.0521(15) 0.0296(11) 0.0499(15) -0.0054(10) -0.0208(12) 0.0003(10) C2 0.0679(19) 0.0367(13) 0.0431(14) -0.0071(11) -0.0164(13) -0.0028(13) C3 0.0620(18) 0.0461(15) 0.0392(14) -0.0121(11) 0.0037(12) 0.0049(13) C4 0.0431(15) 0.0581(18) 0.0483(15) -0.0060(13) 0.0018(12) 0.0031(13) C5 0.0544(17) 0.067(2) 0.0437(15) -0.0104(14) 0.0011(13) -0.0260(15) C6 0.072(2) 0.0456(15) 0.0403(14) -0.0014(12) -0.0036(13) -0.0246(14) C7 0.0546(16) 0.0318(12) 0.0464(14) -0.0084(10) -0.0156(12) -0.0025(11) C8 0.0451(13) 0.0356(12) 0.0394(13) -0.0117(10) -0.0160(10) 0.0018(10) C9 0.0310(11) 0.0436(13) 0.0488(14) -0.0159(11) -0.0074(10) 0.0036(10) C10 0.0338(12) 0.0394(12) 0.0456(13) -0.0119(10) -0.0132(10) 0.0045(10) C11 0.0361(12) 0.0307(11) 0.0397(12) -0.0140(9) -0.0087(9) 0.0008(9) C12 0.0321(11) 0.0277(10) 0.0377(11) -0.0125(9) -0.0086(9) -0.0006(8) C13 0.0292(11) 0.0350(11) 0.0432(13) -0.0139(10) -0.0052(9) -0.0010(9) C14 0.0312(11) 0.0392(12) 0.0506(14) -0.0155(11) -0.0098(10) 0.0008(10) C15 0.0370(12) 0.0336(12) 0.0478(14) -0.0111(10) -0.0166(10) 0.0044(9) C16 0.0373(12) 0.0273(10) 0.0421(12) -0.0119(9) -0.0097(10) 0.0002(9) C17 0.0327(11) 0.0289(10) 0.0381(12) -0.0137(9) -0.0083(9) 0.0026(8) C18 0.0327(12) 0.0343(12) 0.0438(13) -0.0131(10) -0.0037(10) -0.0008(9) C19 0.0291(11) 0.0302(10) 0.0393(12) -0.0119(9) -0.0115(9) 0.0037(8) C20 0.0269(10) 0.0345(11) 0.0391(12) -0.0122(9) -0.0115(9) 0.0015(8) C21 0.0272(10) 0.0294(10) 0.0352(11) -0.0113(9) -0.0115(8) 0.0043(8) C22 0.0273(10) 0.0290(10) 0.0345(11) -0.0132(8) -0.0101(8) 0.0047(8) C23 0.0298(11) 0.0330(11) 0.0354(11) -0.0119(9) -0.0140(9) 0.0054(8) C24 0.0272(11) 0.0398(12) 0.0484(14) -0.0105(11) -0.0083(10) -0.0041(9) C25 0.0294(11) 0.0429(13) 0.0461(14) -0.0050(11) -0.0041(10) 0.0036(10) C26 0.0384(13) 0.0443(14) 0.0482(15) -0.0106(11) -0.0059(11) 0.0061(11) C27 0.0484(16) 0.0547(17) 0.0617(18) -0.0172(14) -0.0032(14) 0.0108(13) C28 0.0575(18) 0.0608(19) 0.0602(19) -0.0224(15) 0.0014(15) 0.0068(15) C29 0.081(3) 0.074(2) 0.068(2) -0.0272(19) -0.0057(19) -0.012(2) C30 0.069(2) 0.075(2) 0.0454(16) -0.0163(15) -0.0078(15) -0.0142(17) C31 0.0535(16) 0.0388(14) 0.0517(16) -0.0054(12) -0.0074(13) 0.0023(12) C32 0.0420(14) 0.0458(14) 0.0550(16) -0.0172(12) -0.0050(12) 0.0055(11) N1 0.0242(9) 0.0347(10) 0.0387(10) -0.0089(8) -0.0095(7) 0.0002(7) O1 0.0344(9) 0.0398(9) 0.0397(9) -0.0047(7) -0.0103(7) 0.0009(7) O2 0.0283(8) 0.0517(11) 0.0486(10) -0.0049(8) -0.0163(7) 0.0038(7) O3 0.0505(11) 0.0364(9) 0.0387(9) -0.0109(7) -0.0023(8) -0.0010(8) O4 0.0421(10) 0.0377(9) 0.0418(9) -0.0042(7) -0.0095(7) 0.0035(7) O5 0.0398(9) 0.0446(10) 0.0356(9) -0.0059(7) -0.0034(7) -0.0065(8) O6 0.0371(9) 0.0443(10) 0.0365(9) -0.0067(7) -0.0080(7) 0.0012(7) O7 0.0549(11) 0.0330(9) 0.0348(9) -0.0045(7) -0.0056(8) -0.0091(8) Cl1 0.0783(6) 0.0499(5) 0.1124(8) 0.0036(5) -0.0157(6) -0.0148(4) Cl2 0.0602(5) 0.1008(8) 0.0730(6) -0.0117(5) -0.0299(4) 0.0056(5) Cl3 0.0767(7) 0.1286(10) 0.0773(6) 0.0261(7) -0.0371(5) -0.0462(7) Cl4 0.0573(5) 0.0813(7) 0.1444(11) -0.0341(7) -0.0283(6) -0.0001(5) Cl5 0.0896(7) 0.0980(8) 0.0785(7) -0.0384(6) 0.0232(6) -0.0199(6) Cl6 0.0781(6) 0.0579(5) 0.1126(8) -0.0356(5) -0.0219(6) -0.0029(4) Cl7 0.0662(5) 0.0621(5) 0.0650(5) -0.0007(4) -0.0050(4) -0.0092(4) Cl8 0.0673(6) 0.1346(11) 0.1031(9) -0.0413(8) -0.0182(6) 0.0132(7) Cl9 0.1238(10) 0.0841(8) 0.0927(8) -0.0023(6) -0.0093(7) -0.0533(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.500(4) yes C1 . O4 . 1.426(3) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . O3 . 1.426(3) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.490(5) yes C3 . O3 . 1.432(3) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . O5 . 1.419(4) yes C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . C6 . 1.492(5) yes C5 . O5 . 1.429(4) yes C5 . H51 . 1.000 no C5 . H52 . 1.000 no C6 . O7 . 1.427(3) yes C6 . H61 . 1.000 no C6 . H62 . 1.000 no C7 . C8 . 1.497(4) yes C7 . O7 . 1.427(3) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . O6 . 1.431(3) yes C8 . H81 . 1.000 no C8 . H82 . 1.000 no C9 . C18 2_765 1.365(4) yes C9 . C10 . 1.407(4) yes C9 . H91 . 1.000 no C10 . C11 . 1.375(4) yes C10 . H101 . 1.000 no C11 . C12 . 1.428(3) yes C11 . O6 . 1.369(3) yes C12 . C17 2_765 1.420(3) yes C12 . C13 . 1.419(3) yes C13 . C14 2_765 1.365(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.409(4) yes C14 . H141 . 1.000 no C15 . C16 . 1.374(4) yes C15 . H151 . 1.000 no C16 . C17 . 1.428(3) yes C16 . O4 . 1.368(3) yes C17 . C18 . 1.423(3) yes C18 . H181 . 1.000 no C19 . C22 . 1.488(3) yes C19 . N1 . 1.387(3) yes C19 . O1 . 1.218(3) yes C20 . C21 . 1.492(3) yes C20 . N1 . 1.402(3) yes C20 . O2 . 1.202(3) yes C21 . C23 2_765 1.380(3) yes C21 . C22 . 1.391(3) yes C22 . C23 . 1.390(3) yes C23 . H231 . 1.000 no C24 . C25 . 1.515(4) yes C24 . N1 . 1.465(3) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no C25 . C26 . 1.519(4) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . C27 . 1.515(4) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C27 . C28 . 1.525(5) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . C29 . 1.501(6) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C30 . Cl7 . 1.757(4) yes C30 . Cl8 . 1.761(4) yes C30 . Cl9 . 1.750(4) yes C30 . H301 . 1.000 no C31 . Cl4 . 1.749(3) yes C31 . Cl5 . 1.742(3) yes C31 . Cl6 . 1.761(3) yes C31 . H311 . 1.000 no C32 . Cl1 . 1.749(3) yes C32 . Cl2 . 1.757(3) yes C32 . Cl3 . 1.737(3) yes C32 . H321 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . O4 . 109.2(2) yes C2 . C1 . H11 . 109.536 no O4 . C1 . H11 . 109.536 no C2 . C1 . H12 . 109.536 no O4 . C1 . H12 . 109.536 no H11 . C1 . H12 . 109.467 no C1 . C2 . O3 . 110.7(2) yes C1 . C2 . H21 . 109.175 no O3 . C2 . H21 . 109.174 no C1 . C2 . H22 . 109.175 no O3 . C2 . H22 . 109.174 no H21 . C2 . H22 . 109.467 no C4 . C3 . O3 . 109.4(2) yes C4 . C3 . H31 . 109.492 no O3 . C3 . H31 . 109.492 no C4 . C3 . H32 . 109.492 no O3 . C3 . H32 . 109.492 no H31 . C3 . H32 . 109.467 no C3 . C4 . O5 . 108.8(2) yes C3 . C4 . H41 . 109.643 no O5 . C4 . H41 . 109.643 no C3 . C4 . H42 . 109.643 no O5 . C4 . H42 . 109.643 no H41 . C4 . H42 . 109.467 no C6 . C5 . O5 . 108.5(3) yes C6 . C5 . H51 . 109.716 no O5 . C5 . H51 . 109.716 no C6 . C5 . H52 . 109.716 no O5 . C5 . H52 . 109.716 no H51 . C5 . H52 . 109.467 no C5 . C6 . O7 . 109.3(2) yes C5 . C6 . H61 . 109.521 no O7 . C6 . H61 . 109.521 no C5 . C6 . H62 . 109.521 no O7 . C6 . H62 . 109.521 no H61 . C6 . H62 . 109.467 no C8 . C7 . O7 . 110.6(2) yes C8 . C7 . H71 . 109.190 no O7 . C7 . H71 . 109.190 no C8 . C7 . H72 . 109.190 no O7 . C7 . H72 . 109.190 no H71 . C7 . H72 . 109.467 no C7 . C8 . O6 . 108.5(2) yes C7 . C8 . H81 . 109.720 no O6 . C8 . H81 . 109.720 no C7 . C8 . H82 . 109.720 no O6 . C8 . H82 . 109.720 no H81 . C8 . H82 . 109.467 no C18 2_765 C9 . C10 . 121.6(2) yes C18 2_765 C9 . H91 . 119.218 no C10 . C9 . H91 . 119.218 no C9 . C10 . C11 . 119.9(2) yes C9 . C10 . H101 . 120.026 no C11 . C10 . H101 . 120.026 no C10 . C11 . C12 . 120.7(2) yes C10 . C11 . O6 . 124.6(2) yes C12 . C11 . O6 . 114.7(2) yes C11 . C12 . C17 2_765 118.2(2) yes C11 . C12 . C13 . 121.9(2) yes C17 2_765 C12 . C13 . 119.9(2) yes C12 . C13 . C14 2_765 119.8(2) yes C12 . C13 . H131 . 120.102 no C14 2_765 C13 . H131 . 120.102 no C13 2_765 C14 . C15 . 121.4(2) yes C13 2_765 C14 . H141 . 119.277 no C15 . C14 . H141 . 119.277 no C14 . C15 . C16 . 119.8(2) yes C14 . C15 . H151 . 120.121 no C16 . C15 . H151 . 120.121 no C15 . C16 . C17 . 120.8(2) yes C15 . C16 . O4 . 124.7(2) yes C17 . C16 . O4 . 114.5(2) yes C16 . C17 . C12 2_765 118.2(2) yes C16 . C17 . C18 . 121.7(2) yes C12 2_765 C17 . C18 . 120.0(2) yes C17 . C18 . C9 2_765 119.5(2) yes C17 . C18 . H181 . 120.242 no C9 2_765 C18 . H181 . 120.242 no C22 . C19 . N1 . 106.5(2) yes C22 . C19 . O1 . 128.4(2) yes N1 . C19 . O1 . 125.1(2) yes C21 . C20 . N1 . 106.03(18) yes C21 . C20 . O2 . 129.2(2) yes N1 . C20 . O2 . 124.8(2) yes C20 . C21 . C23 2_765 129.0(2) yes C20 . C21 . C22 . 107.8(2) yes C23 2_765 C21 . C22 . 123.2(2) yes C19 . C22 . C21 . 108.04(19) yes C19 . C22 . C23 . 129.6(2) yes C21 . C22 . C23 . 122.4(2) yes C22 . C23 . C21 2_765 114.4(2) yes C22 . C23 . H231 . 122.804 no C21 2_765 C23 . H231 . 122.804 no C25 . C24 . N1 . 113.1(2) yes C25 . C24 . H241 . 108.560 no N1 . C24 . H241 . 108.560 no C25 . C24 . H242 . 108.560 no N1 . C24 . H242 . 108.560 no H241 . C24 . H242 . 109.467 no C24 . C25 . C26 . 113.0(2) yes C24 . C25 . H251 . 108.585 no C26 . C25 . H251 . 108.586 no C24 . C25 . H252 . 108.585 no C26 . C25 . H252 . 108.586 no H251 . C25 . H252 . 109.467 no C25 . C26 . C27 . 113.3(2) yes C25 . C26 . H261 . 108.518 no C27 . C26 . H261 . 108.518 no C25 . C26 . H262 . 108.518 no C27 . C26 . H262 . 108.518 no H261 . C26 . H262 . 109.467 no C26 . C27 . C28 . 112.9(3) yes C26 . C27 . H271 . 108.606 no C28 . C27 . H271 . 108.605 no C26 . C27 . H272 . 108.606 no C28 . C27 . H272 . 108.605 no H271 . C27 . H272 . 109.467 no C27 . C28 . C29 . 112.7(3) yes C27 . C28 . H281 . 108.648 no C29 . C28 . H281 . 108.648 no C27 . C28 . H282 . 108.648 no C29 . C28 . H282 . 108.648 no H281 . C28 . H282 . 109.467 no C28 . C29 . H291 . 109.467 no C28 . C29 . H292 . 109.467 no H291 . C29 . H292 . 109.475 no C28 . C29 . H293 . 109.467 no H291 . C29 . H293 . 109.476 no H292 . C29 . H293 . 109.476 no Cl7 . C30 . Cl8 . 109.4(2) yes Cl7 . C30 . Cl9 . 108.6(2) yes Cl8 . C30 . Cl9 . 112.2(2) yes Cl7 . C30 . H301 . 111.065 no Cl8 . C30 . H301 . 107.447 no Cl9 . C30 . H301 . 108.175 no Cl4 . C31 . Cl5 . 111.01(19) yes Cl4 . C31 . Cl6 . 110.44(17) yes Cl5 . C31 . Cl6 . 109.88(18) yes Cl4 . C31 . H311 . 107.900 no Cl5 . C31 . H311 . 108.476 no Cl6 . C31 . H311 . 109.073 no Cl1 . C32 . Cl2 . 112.90(17) yes Cl1 . C32 . Cl3 . 110.55(18) yes Cl2 . C32 . Cl3 . 108.40(17) yes Cl1 . C32 . H321 . 106.007 no Cl2 . C32 . H321 . 108.253 no Cl3 . C32 . H321 . 110.706 no C24 . N1 . C20 . 122.58(19) yes C24 . N1 . C19 . 125.5(2) yes C20 . N1 . C19 . 111.69(19) yes C3 . O3 . C2 . 110.5(2) yes C1 . O4 . C16 . 116.6(2) yes C5 . O5 . C4 . 112.4(2) yes C8 . O6 . C11 . 116.9(2) yes C6 . O7 . C7 . 111.7(2) yes #===END #################################################### ## denoted [Na212][B{3,5-(CF3)2(C6H3)}4]2 in text ## #################################################### data_5 _database_code_depnum_ccdc_archive 'CCDC 254114' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 38.5110(1) _cell_angle_alpha 90 _cell_length_b 15.7246(2) _cell_angle_beta 93.6400(5) _cell_length_c 22.8791(3) _cell_angle_gamma 90 _cell_volume 13826.9(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'Na ' 0.0300 0.0250 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C122 H96 B2 F48 N2 Na2 O14 ' _chemical_formula_moiety ; C64 H24 B2 F48, (C36 H44 O10), (C22 H28 N2 O4), 2Na ; _chemical_compound_source ; ? ; _chemical_formula_weight 2793.36 _cell_measurement_reflns_used 87214 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 180 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 5672.001 _exptl_absorpt_coefficient_mu 0.135 # Sheldrick geometric definitions 0.97 0.98 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 180 _diffrn_reflns_number 15601 _reflns_number_total 15601 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 15601 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 15863 _diffrn_reflns_theta_min 5.152 _diffrn_reflns_theta_max 27.505 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.405 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -49 _reflns_limit_h_max 49 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _refine_diff_density_min -0.78 _refine_diff_density_max 2.01 _refine_ls_number_reflns 6111 _refine_ls_number_restraints 292 _refine_ls_number_parameters 690 #_refine_ls_R_factor_ref 0.1580 _refine_ls_wR_factor_ref 0.1728 _refine_ls_goodness_of_fit_ref 1.1708 #_reflns_number_all 15601 _refine_ls_R_factor_all 0.2420 _refine_ls_wR_factor_all 0.2243 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 6111 _refine_ls_R_factor_gt 0.1580 _refine_ls_wR_factor_gt 0.1728 _refine_ls_shift/su_max 0.027353 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 A~i~ are: 3.82 2.87 2.53 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _exptl_special_details ; Treatment of rezidual electron density using the SQUEEZE procedure (P. v.d. Sluis & A. L. Spek, Acta Crystallogr. 1990, A46, 194.), implemented in PLATON (PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998.). Therefore structure Contains Solvent Accessible VOIDS of 265.00 A**3 - equiv to ca 7 H2O molecules disordered per unit pseudorotaxane 3.5 molec /asym unit. Identification of the crystalising solvent as water is reliant upon additional chemical evidence; it cannot be deduced from the X-ray data alone Each of the 8 CF3 groups has been modelled as disordered over 2 sites with refined occupancies. In view of the severe shortage of data their temperature factors have been refined isotropically. One hexyl chain has been modelled as disordered over two sites with refined occupancy & isotropic temperature factors. ; ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Sortav (Blessing 1995) P. v.d. Sluis & A. L. Spek, Acta Crystallogr. 1990, A46, 194. PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998. Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags _atom_site_attached_hydrogens Na1 Na 0.38217(9) 0.5976(2) 0.38601(16) 0.0484 1.0000 Uani . . N1 N 0.47521(18) 0.7038(4) 0.5017(3) 0.0384 1.0000 Uani D . C1 C 0.4569(2) 0.6422(6) 0.4715(4) 0.0402 1.0000 Uani . . O1 O 0.42964(16) 0.6520(4) 0.4425(3) 0.0466 1.0000 Uani . . C2 C 0.4764(2) 0.5607(5) 0.4824(3) 0.0302 1.0000 Uani . . C3 C 0.5063(2) 0.5801(5) 0.5195(3) 0.0311 1.0000 Uani . . C4 C 0.5049(2) 0.6738(5) 0.5334(4) 0.0376 1.0000 Uani . . O2 O 0.52518(17) 0.7148(4) 0.5633(3) 0.0529 1.0000 Uani . . C5 C 0.5300(2) 0.5197(5) 0.5379(3) 0.0327 1.0000 Uani . . C6 C 0.4658(3) 0.7946(5) 0.5031(3) 0.0603 1.0000 Uani DU . C7 C 0.4496(3) 0.8242(5) 0.5566(4) 0.0701 1.0000 Uani DU . C8 C 0.4439(3) 0.9178(6) 0.5614(4) 0.0803 1.0000 Uani DU . C9 C 0.4462(7) 0.9537(8) 0.6222(6) 0.081(5) 0.48(2) Uiso DUP . C10 C 0.4452(7) 1.049(1) 0.6268(7) 0.082(6) 0.48(2) Uiso DUP . C11 C 0.4407(8) 1.0850(13) 0.687(1) 0.084(6) 0.48(2) Uiso DUP . C109 C 0.4750(5) 0.971(1) 0.5635(7) 0.111(6) 0.52(2) Uiso DUP . C110 C 0.5005(6) 0.9548(18) 0.6120(12) 0.114(7) 0.52(2) Uiso DUP . C111 C 0.5304(7) 1.017(2) 0.6187(14) 0.119(7) 0.52(2) Uiso DUP . C12 C 0.4248(2) 0.5214(7) 0.5993(4) 0.0461 1.0000 Uani . . C13 C 0.4346(3) 0.5992(6) 0.6221(4) 0.0499 1.0000 Uani . . C14 C 0.4662(3) 0.6052(6) 0.6568(4) 0.0488 1.0000 Uani . . C15 C 0.4869(3) 0.5357(7) 0.6695(4) 0.0494 1.0000 Uani . . C16 C 0.4762(2) 0.4547(7) 0.6466(4) 0.0473 1.0000 Uani . . C17 C 0.4966(2) 0.3793(6) 0.6562(4) 0.0438 1.0000 Uani . . C18 C 0.4861(2) 0.3042(6) 0.6339(4) 0.0468 1.0000 Uani . . C19 C 0.4552(3) 0.2980(6) 0.5999(5) 0.0488 1.0000 Uani . . C20 C 0.4346(2) 0.3669(6) 0.5872(4) 0.0450 1.0000 Uani . . C21 C 0.4447(2) 0.4474(6) 0.6103(4) 0.0367 1.0000 Uani . . O3 O 0.39465(17) 0.5090(4) 0.5661(3) 0.0558 1.0000 Uani . . C22 C 0.3727(3) 0.5800(7) 0.5509(4) 0.0528 1.0000 Uani . . C23 C 0.3425(3) 0.5492(8) 0.5123(6) 0.0685 1.0000 Uani . . O4 O 0.35379(19) 0.5203(5) 0.4573(4) 0.0653 1.0000 Uani . . C24 C 0.3612(4) 0.4307(8) 0.4537(7) 0.0910 1.0000 Uani . . C25 C 0.3608(4) 0.4062(9) 0.3916(8) 0.0954 1.0000 Uani . . O5 O 0.3862(2) 0.4522(5) 0.3646(4) 0.0796 1.0000 Uani . . C26 C 0.3846(3) 0.437(1) 0.3034(7) 0.0860 1.0000 Uani . . C27 C 0.4092(4) 0.4935(11) 0.2772(7) 0.0971 1.0000 Uani . . O6 O 0.40147(17) 0.5826(5) 0.2911(3) 0.0610 1.0000 Uani . . C28 C 0.4204(3) 0.6449(9) 0.2599(5) 0.0693 1.0000 Uani . . C29 C 0.4512(3) 0.6761(7) 0.2969(4) 0.0574 1.0000 Uani . . O7 O 0.47382(17) 0.6057(5) 0.3067(3) 0.0598 1.0000 Uani . . B1 B 0.1788(2) 0.5477(6) 0.2209(4) 0.0349 1.0000 Uani . . C30 C 0.18833(14) 0.4672(4) 0.1785(2) 0.0336 1.0000 Uani . . C31 C 0.16175(16) 0.4161(4) 0.1537(3) 0.0361 1.0000 Uani . . C32 C 0.16856(16) 0.3455(4) 0.1179(3) 0.0386 1.0000 Uani DU . C33 C 0.20162(18) 0.3245(4) 0.1061(3) 0.0490 1.0000 Uani . . C34 C 0.2289(2) 0.3753(4) 0.1301(3) 0.0557 1.0000 Uani DU . C35 C 0.22201(16) 0.4437(4) 0.1654(3) 0.0420 1.0000 Uani . . C36 C 0.14388(14) 0.5965(4) 0.1923(2) 0.0340 1.0000 Uani . . C37 C 0.11823(16) 0.6307(4) 0.2273(3) 0.0382 1.0000 Uani . . C38 C 0.08996(16) 0.6742(4) 0.2022(3) 0.0493 1.0000 Uani DU . C39 C 0.08444(18) 0.6834(4) 0.1423(3) 0.0574 1.0000 Uani . . C40 C 0.1083(2) 0.6482(4) 0.1080(3) 0.0647 1.0000 Uani DU . C41 C 0.13805(16) 0.6060(4) 0.1328(3) 0.0484 1.0000 Uani . . C42 C 0.21113(15) 0.6162(4) 0.2272(3) 0.0404 1.0000 Uani . . C43 C 0.24301(18) 0.5948(4) 0.2579(3) 0.0590 1.0000 Uani . . C44 C 0.2710(2) 0.6496(5) 0.2590(4) 0.0856 1.0000 Uani DU . C45 C 0.2694(2) 0.7284(6) 0.2346(4) 0.0828 1.0000 Uani . . C46 C 0.23853(19) 0.7522(5) 0.2033(4) 0.0627 1.0000 Uani DU . C47 C 0.21073(18) 0.6941(5) 0.2004(3) 0.0454 1.0000 Uani . . C48 C 0.17196(15) 0.5119(4) 0.2863(3) 0.0407 1.0000 Uani . . C49 C 0.16049(18) 0.4291(4) 0.2965(3) 0.0491 1.0000 Uani . . C50 C 0.1542(2) 0.4002(5) 0.3541(4) 0.0710 1.0000 Uani DU . C51 C 0.1572(2) 0.4550(6) 0.4008(4) 0.0723 1.0000 Uani . . C52 C 0.16810(19) 0.5372(5) 0.3909(4) 0.0855 1.0000 Uani DU . C53 C 0.17459(18) 0.5655(5) 0.3364(3) 0.0570 1.0000 Uani . . C54 C 0.13759(18) 0.2947(5) 0.0948(3) 0.0461(16) 1.0000 Uiso DU . C55 C 0.2652(2) 0.3523(6) 0.1173(4) 0.085(2) 1.0000 Uiso DU . C56 C 0.0638(2) 0.7114(5) 0.2404(4) 0.073(2) 1.0000 Uiso DU . C57 C 0.1031(3) 0.6566(6) 0.0432(4) 0.089(2) 1.0000 Uiso DU . C58 C 0.3053(2) 0.6184(6) 0.2842(4) 0.087(2) 1.0000 Uiso DU . C59 C 0.2346(2) 0.8357(6) 0.1749(4) 0.086(2) 1.0000 Uiso DU . C60 C 0.1453(3) 0.3093(6) 0.3641(5) 0.115(3) 1.0000 Uiso DU . C61 C 0.1721(3) 0.5983(7) 0.4411(4) 0.111(3) 1.0000 Uiso DU . F1 F 0.1484(3) 0.219(1) 0.0684(7) 0.046(3) 0.52(3) Uiso DUP . F2 F 0.1196(4) 0.3325(8) 0.0549(7) 0.049(3) 0.52(3) Uiso DUP . F3 F 0.1171(4) 0.269(1) 0.1382(5) 0.043(3) 0.52(3) Uiso DUP . F4 F 0.1106(4) 0.3471(8) 0.0705(7) 0.045(3) 0.48(3) Uiso DUP . F5 F 0.1436(3) 0.2415(11) 0.0529(8) 0.052(3) 0.48(3) Uiso DUP . F6 F 0.1229(4) 0.2503(11) 0.1359(6) 0.044(3) 0.48(3) Uiso DUP . F7 F 0.2898(4) 0.3941(11) 0.1487(8) 0.082(4) 0.456(15) Uiso DUP . F8 F 0.2708(4) 0.3640(15) 0.0613(9) 0.099(4) 0.456(15) Uiso DUP . F9 F 0.2726(4) 0.2676(12) 0.1305(9) 0.088(4) 0.456(15) Uiso DUP . F10 F 0.2676(3) 0.3174(12) 0.0651(7) 0.086(4) 0.544(15) Uiso DUP . F11 F 0.2866(3) 0.4219(9) 0.1177(7) 0.081(4) 0.544(15) Uiso DUP . F12 F 0.2800(4) 0.2976(11) 0.1555(8) 0.096(4) 0.544(15) Uiso DUP . F13 F 0.0399(5) 0.7590(12) 0.2128(6) 0.069(4) 0.420(14) Uiso DUP . F14 F 0.0822(4) 0.7624(13) 0.2877(7) 0.075(4) 0.420(14) Uiso DUP . F15 F 0.0484(5) 0.6574(11) 0.2713(9) 0.084(4) 0.420(14) Uiso DUP . F16 F 0.0725(3) 0.7180(9) 0.2937(5) 0.076(3) 0.580(14) Uiso DUP . F17 F 0.0519(3) 0.7902(8) 0.2197(5) 0.065(3) 0.580(14) Uiso DUP . F18 F 0.0345(4) 0.6567(8) 0.2413(7) 0.085(3) 0.580(14) Uiso DUP . F19 F 0.1169(3) 0.5913(7) 0.0136(5) 0.087(3) 0.678(11) Uiso DUP . F20 F 0.1037(4) 0.7351(8) 0.0240(5) 0.088(3) 0.678(11) Uiso DUP . F21 F 0.0664(3) 0.6334(8) 0.0253(5) 0.095(3) 0.678(11) Uiso DUP . F22 F 0.0850(7) 0.7195(16) 0.0252(8) 0.095(5) 0.322(11) Uiso DUP . F23 F 0.1396(6) 0.6771(14) 0.0171(8) 0.089(5) 0.322(11) Uiso DUP . F24 F 0.0941(7) 0.5974(16) 0.0187(8) 0.095(5) 0.322(11) Uiso DUP . F25 F 0.3323(3) 0.6795(8) 0.2793(7) 0.076(3) 0.570(13) Uiso DUP . F26 F 0.3035(3) 0.6067(11) 0.3393(7) 0.097(4) 0.570(13) Uiso DUP . F27 F 0.3154(3) 0.547(1) 0.2638(7) 0.091(4) 0.570(13) Uiso DUP . F28 F 0.3040(4) 0.5554(14) 0.3204(9) 0.093(4) 0.430(13) Uiso DUP . F29 F 0.3255(4) 0.674(1) 0.3115(9) 0.074(4) 0.430(13) Uiso DUP . F30 F 0.3244(5) 0.5750(12) 0.2384(9) 0.090(4) 0.430(13) Uiso DUP . F31 F 0.2133(6) 0.835(1) 0.127(1) 0.086(4) 0.43(2) Uiso DUP . F32 F 0.2240(7) 0.8904(12) 0.2047(9) 0.096(4) 0.43(2) Uiso DUP . F33 F 0.2675(5) 0.8657(11) 0.149(1) 0.085(4) 0.43(2) Uiso DUP . F34 F 0.2632(4) 0.8849(9) 0.1836(8) 0.088(4) 0.57(2) Uiso DUP . F35 F 0.2095(5) 0.8863(9) 0.2044(6) 0.093(4) 0.57(2) Uiso DUP . F36 F 0.2234(5) 0.8326(8) 0.1190(8) 0.087(4) 0.57(2) Uiso DUP . F37 F 0.1334(7) 0.2941(11) 0.4115(11) 0.111(5) 0.417(12) Uiso DUP . F38 F 0.1739(7) 0.2555(14) 0.3627(12) 0.129(5) 0.417(12) Uiso DUP . F39 F 0.1214(7) 0.2815(12) 0.321(1) 0.115(5) 0.417(12) Uiso DUP . F40 F 0.1474(4) 0.2594(9) 0.3184(7) 0.104(4) 0.583(12) Uiso DUP . F41 F 0.1671(5) 0.272(1) 0.4046(9) 0.127(4) 0.583(12) Uiso DUP . F42 F 0.1152(5) 0.3022(9) 0.3890(8) 0.122(4) 0.583(12) Uiso DUP . F43 F 0.1957(6) 0.6429(13) 0.4422(7) 0.108(4) 0.492(16) Uiso DUP . F44 F 0.1743(6) 0.5561(11) 0.4961(8) 0.104(4) 0.492(16) Uiso DUP . F45 F 0.1430(7) 0.6548(13) 0.4403(8) 0.123(5) 0.492(16) Uiso DUP . F46 F 0.1560(6) 0.5755(11) 0.4887(8) 0.108(4) 0.508(16) Uiso DUP . F47 F 0.2104(6) 0.6102(13) 0.4570(8) 0.114(4) 0.508(16) Uiso DUP . F48 F 0.1632(6) 0.6730(13) 0.4298(7) 0.118(4) 0.508(16) Uiso DUP . H51 H 0.5508 0.5335 0.5646 0.0391 1.0000 Uiso . . H61 H 0.4876 0.8284 0.4992 0.0720 1.0000 Uiso . . H62 H 0.4491 0.8062 0.4688 0.0720 1.0000 Uiso . . H71 H 0.4649 0.8061 0.5913 0.0840 1.0000 Uiso . . H72 H 0.4264 0.7957 0.5579 0.0840 1.0000 Uiso . . H81 H 0.4618 0.9470 0.5388 0.0963 1.0000 Uiso . . H82 H 0.4202 0.9308 0.5433 0.0963 1.0000 Uiso . . H91 H 0.4685 0.9337 0.6423 0.0971 0.4825 Uiso . . H92 H 0.4261 0.9307 0.6430 0.0971 0.4825 Uiso . . H101 H 0.4676 1.0717 0.6131 0.0980 0.4825 Uiso . . H102 H 0.4254 1.0701 0.6002 0.0980 0.4825 Uiso . . H111 H 0.4405 1.1485 0.6851 0.1013 0.4825 Uiso . . H112 H 0.4605 1.0659 0.7144 0.1013 0.4825 Uiso . . H113 H 0.4183 1.0643 0.7015 0.1013 0.4825 Uiso . . H1091 H 0.4675 1.0313 0.5659 0.1331 0.5175 Uiso . . H1092 H 0.4867 0.9614 0.5262 0.1331 0.5175 Uiso . . H1101 H 0.4881 0.9560 0.6490 0.1373 0.5175 Uiso . . H1102 H 0.5106 0.8970 0.6065 0.1373 0.5175 Uiso . . H1111 H 0.5462 1.0004 0.6531 0.1425 0.5175 Uiso . . H1112 H 0.5211 1.0755 0.6251 0.1425 0.5175 Uiso . . H1113 H 0.5436 1.0165 0.5825 0.1425 0.5175 Uiso . . H131 H 0.4197 0.6506 0.6143 0.0603 1.0000 Uiso . . H141 H 0.4737 0.6620 0.6726 0.0591 1.0000 Uiso . . H151 H 0.5091 0.5416 0.6944 0.0598 1.0000 Uiso . . H181 H 0.5006 0.2523 0.6420 0.0566 1.0000 Uiso . . H191 H 0.4477 0.2412 0.5840 0.0591 1.0000 Uiso . . H201 H 0.4126 0.3607 0.5618 0.0541 1.0000 Uiso . . H221 H 0.3641 0.6059 0.5872 0.0637 1.0000 Uiso . . H222 H 0.3860 0.6234 0.5295 0.0637 1.0000 Uiso . . H231 H 0.3255 0.5968 0.5053 0.0822 1.0000 Uiso . . H232 H 0.3309 0.5011 0.5322 0.0822 1.0000 Uiso . . H241 H 0.3846 0.4186 0.4733 0.1072 1.0000 Uiso . . H242 H 0.3431 0.3976 0.4735 0.1072 1.0000 Uiso . . H251 H 0.3658 0.3440 0.3885 0.1124 1.0000 Uiso . . H252 H 0.3374 0.4189 0.3720 0.1124 1.0000 Uiso . . H261 H 0.3909 0.3766 0.2958 0.1020 1.0000 Uiso . . H262 H 0.3606 0.4487 0.2863 0.1020 1.0000 Uiso . . H271 H 0.4333 0.4794 0.2930 0.1165 1.0000 Uiso . . H272 H 0.4074 0.4856 0.2338 0.1165 1.0000 Uiso . . H281 H 0.4047 0.6940 0.2492 0.0833 1.0000 Uiso . . H282 H 0.4285 0.6186 0.2234 0.0833 1.0000 Uiso . . H291 H 0.4632 0.7225 0.2762 0.0693 1.0000 Uiso . . H292 H 0.4436 0.6981 0.3351 0.0693 1.0000 Uiso . . H311 H 0.1371 0.4297 0.1616 0.0432 1.0000 Uiso . . H331 H 0.2064 0.2744 0.0809 0.0594 1.0000 Uiso . . H351 H 0.2420 0.4782 0.1823 0.0508 1.0000 Uiso . . H371 H 0.1206 0.6232 0.2708 0.0460 1.0000 Uiso . . H391 H 0.0637 0.7147 0.1247 0.0679 1.0000 Uiso . . H411 H 0.1553 0.5824 0.1064 0.0575 1.0000 Uiso . . H431 H 0.2453 0.5392 0.2791 0.0690 1.0000 Uiso . . H451 H 0.2896 0.7682 0.2389 0.0984 1.0000 Uiso . . H471 H 0.1890 0.7110 0.1771 0.0540 1.0000 Uiso . . H491 H 0.1566 0.3892 0.2627 0.0589 1.0000 Uiso . . H511 H 0.1517 0.4360 0.4409 0.0874 1.0000 Uiso . . H531 H 0.1815 0.6263 0.3314 0.0684 1.0000 Uiso . . 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 0.051(2) 0.046(2) 0.047(2) -0.0101(17) -0.0059(16) 0.0111(17) N1 0.043(4) 0.031(4) 0.041(4) -0.001(3) 0.002(3) 0.004(3) C1 0.041(5) 0.045(5) 0.034(5) 0.004(4) -0.001(4) 0.004(4) O1 0.038(3) 0.053(4) 0.048(4) 0.001(3) -0.008(3) 0.010(3) C2 0.024(4) 0.040(5) 0.027(4) -0.003(4) 0.001(3) 0.002(4) C3 0.029(4) 0.035(5) 0.029(4) -0.001(3) -0.001(3) -0.009(4) C4 0.041(5) 0.031(5) 0.040(5) -0.005(4) 0.006(4) -0.001(4) O2 0.046(4) 0.040(4) 0.071(5) -0.013(3) -0.013(3) -0.014(3) C5 0.025(4) 0.040(5) 0.033(4) -0.007(4) -0.001(3) -0.003(4) C6 0.078(6) 0.036(4) 0.065(5) 0.005(4) -0.003(4) 0.011(4) C7 0.089(5) 0.046(4) 0.075(5) 0.001(4) 0.004(4) 0.016(4) C8 0.102(6) 0.053(4) 0.085(5) -0.002(4) 0.005(5) 0.022(4) C12 0.042(5) 0.066(7) 0.032(5) 0.015(5) 0.013(4) 0.012(5) C13 0.064(7) 0.050(6) 0.036(5) -0.009(4) 0.010(5) 0.008(5) C14 0.051(6) 0.044(6) 0.053(6) -0.013(5) 0.013(5) 0.004(5) C15 0.046(5) 0.072(7) 0.031(5) -0.006(5) 0.014(4) 0.006(5) C16 0.043(5) 0.057(6) 0.043(5) -0.005(5) 0.009(4) 0.008(5) C17 0.037(5) 0.055(6) 0.040(5) 0.002(4) 0.009(4) 0.008(4) C18 0.041(5) 0.050(6) 0.051(6) 0.008(5) 0.011(4) 0.000(5) C19 0.050(6) 0.036(5) 0.062(6) 0.006(5) 0.014(5) 0.001(4) C20 0.041(5) 0.050(6) 0.043(5) 0.018(4) 0.005(4) -0.011(4) C21 0.036(5) 0.043(5) 0.031(4) -0.002(4) 0.003(4) -0.003(4) O3 0.049(4) 0.050(4) 0.068(5) 0.010(3) -0.006(3) 0.002(3) C22 0.055(6) 0.056(6) 0.049(6) 0.011(5) 0.011(5) 0.012(5) C23 0.038(6) 0.085(8) 0.082(9) 0.022(7) 0.004(6) 0.008(6) O4 0.059(4) 0.054(5) 0.080(5) 0.004(4) -0.016(4) 0.007(4) C24 0.102(11) 0.056(8) 0.110(12) 0.011(8) -0.032(9) -0.011(7) C25 0.094(11) 0.055(8) 0.132(14) -0.003(8) -0.03(1) -0.024(8) O5 0.061(5) 0.050(5) 0.123(8) -0.027(5) -0.034(5) 0.013(4) C26 0.058(8) 0.09(1) 0.107(11) -0.062(9) -0.019(7) 0.015(7) C27 0.072(9) 0.112(12) 0.107(11) -0.06(1) 0.005(8) 0.013(9) O6 0.040(4) 0.080(5) 0.063(5) -0.029(4) -0.002(3) 0.013(4) C28 0.052(6) 0.11(1) 0.045(6) -0.001(6) 0.005(5) 0.022(7) C29 0.058(6) 0.077(8) 0.038(5) 0.014(5) 0.011(5) 0.020(6) O7 0.043(4) 0.078(5) 0.057(4) -0.013(4) -0.007(3) 0.017(4) B1 0.030(5) 0.034(5) 0.040(5) 0.003(4) -0.004(4) 0.003(4) C30 0.035(3) 0.035(3) 0.030(3) -0.006(3) 0.002(2) -0.008(3) C31 0.039(3) 0.028(3) 0.041(3) 0.003(3) -0.001(3) -0.003(3) C32 0.044(3) 0.040(4) 0.032(4) 0.004(3) 0.005(3) -0.011(3) C33 0.054(4) 0.031(4) 0.064(5) -0.007(3) 0.017(3) -0.007(3) C34 0.072(4) 0.045(4) 0.051(4) -0.012(4) 0.010(4) -0.016(4) C35 0.035(3) 0.048(4) 0.044(4) 0.002(3) 0.011(3) -0.004(3) C36 0.027(3) 0.043(3) 0.032(3) -0.008(3) -0.002(2) 0.012(3) C37 0.048(3) 0.033(3) 0.035(3) -0.003(3) 0.007(3) 0.001(3) C38 0.042(3) 0.046(4) 0.058(4) 0.003(3) -0.010(3) 0.001(3) C39 0.051(4) 0.053(4) 0.066(5) -0.008(3) -0.016(3) 0.018(3) C40 0.071(4) 0.054(4) 0.070(4) -0.019(4) 0.009(4) 0.031(4) C41 0.042(3) 0.057(4) 0.044(4) -0.005(3) -0.007(3) 0.017(3) C42 0.023(3) 0.045(4) 0.054(4) -0.012(3) 0.001(3) 0.010(3) C43 0.052(4) 0.032(4) 0.088(4) -0.019(3) -0.033(3) 0.002(3) C44 0.080(5) 0.035(4) 0.139(6) -0.030(4) -0.022(4) 0.002(4) C45 0.036(5) 0.045(5) 0.165(5) -0.020(5) -0.014(4) -0.009(4) C46 0.030(4) 0.038(4) 0.118(5) -0.023(3) -0.008(4) 0.005(4) C47 0.036(4) 0.044(4) 0.055(4) -0.005(3) -0.006(3) 0.003(3) C48 0.035(3) 0.052(4) 0.035(4) -0.011(3) -0.003(3) 0.004(3) C49 0.046(4) 0.058(4) 0.043(4) -0.006(3) 0.002(3) -0.007(3) C50 0.055(5) 0.109(4) 0.048(6) -0.003(4) 0.001(4) -0.005(4) C51 0.086(5) 0.095(5) 0.037(5) -0.007(5) 0.015(4) -0.023(4) C52 0.085(4) 0.130(4) 0.043(5) 0.019(3) 0.013(4) -0.001(4) C53 0.072(4) 0.066(4) 0.033(4) -0.010(3) 0.004(3) 0.003(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . C6 . 1.474(11) yes N1 . C4 . 1.397(12) yes N1 . C1 . 1.360(12) yes C1 . C2 . 1.500(12) yes C1 . O1 . 1.22(1) yes C2 . C3 . 1.418(11) yes C2 . C5 2_666 1.363(12) yes C3 . C5 . 1.367(12) yes C3 . C4 . 1.508(12) yes C4 . O2 . 1.19(1) yes C5 . H51 . 1.000 no C6 . H62 . 1.000 no C6 . H61 . 1.000 no C6 . C7 . 1.486(12) yes C7 . H72 . 1.000 no C7 . H71 . 1.000 no C7 . C8 . 1.492(12) yes C8 . H82 . 1.000 no C8 . H81 . 1.000 no C8 . C109 . 1.456(17) yes C8 . C9 . 1.498(15) yes C9 . H92 . 1.000 no C9 . H91 . 1.000 no C9 . C10 . 1.506(17) yes C10 . H102 . 1.000 no C10 . H101 . 1.000 no C10 . C11 . 1.509(18) yes C11 . H113 . 1.000 no C11 . H112 . 1.000 no C11 . H111 . 1.000 no C109 . H1092 . 1.000 no C109 . H1091 . 1.000 no C109 . H81 . 0.823 no C109 . C110 . 1.457(18) yes C110 . H1102 . 1.000 no C110 . H1101 . 1.000 no C110 . C111 . 1.509(19) yes C111 . H1113 . 1.000 no C111 . H1112 . 1.000 no C111 . H1111 . 1.000 no C12 . O3 . 1.359(12) yes C12 . C21 . 1.408(13) yes C12 . C13 . 1.374(14) yes C13 . H131 . 1.000 no C13 . C14 . 1.412(14) yes C14 . H141 . 1.000 no C14 . C15 . 1.373(14) yes C15 . H151 . 1.000 no C15 . C16 . 1.427(15) yes C16 . C21 . 1.430(13) yes C16 . C17 . 1.431(13) yes C17 . C18 . 1.339(14) yes C17 . O7 2_666 1.399(12) yes C18 . H181 . 1.000 no C18 . C19 . 1.384(14) yes C19 . H191 . 1.000 no C19 . C20 . 1.362(14) yes C20 . H201 . 1.000 no C20 . C21 . 1.417(13) yes O3 . C22 . 1.431(12) yes C22 . H222 . 1.000 no C22 . H221 . 1.000 no C22 . C23 . 1.495(17) yes C23 . H232 . 1.000 no C23 . H231 . 1.000 no C23 . O4 . 1.432(15) yes O4 . C24 . 1.441(16) yes C24 . H242 . 1.000 no C24 . H241 . 1.000 no C24 . C25 . 1.47(2) yes C25 . H252 . 1.000 no C25 . H251 . 1.000 no C25 . O5 . 1.391(18) yes O5 . C26 . 1.416(17) yes C26 . H262 . 1.000 no C26 . H261 . 1.000 no C26 . C27 . 1.45(2) yes C27 . H272 . 1.000 no C27 . H271 . 1.000 no C27 . O6 . 1.472(17) yes O6 . C28 . 1.437(16) yes C28 . H282 . 1.000 no C28 . H281 . 1.000 no C28 . C29 . 1.496(17) yes C29 . H292 . 1.000 no C29 . H291 . 1.000 no C29 . O7 . 1.419(12) yes B1 . C48 . 1.636(12) yes B1 . C42 . 1.645(11) yes B1 . C36 . 1.649(11) yes B1 . C30 . 1.650(12) yes C30 . C35 . 1.399(8) yes C30 . C31 . 1.393(8) yes C31 . H311 . 1.000 no C31 . C32 . 1.415(9) yes C32 . C54 . 1.503(9) yes C32 . C33 . 1.359(9) yes C33 . H331 . 1.000 no C33 . C34 . 1.40(1) yes C34 . C55 . 1.491(11) yes C34 . C35 . 1.380(9) yes C35 . H351 . 1.000 no C36 . C41 . 1.373(9) yes C36 . C37 . 1.417(8) yes C37 . H371 . 1.000 no C37 . C38 . 1.380(9) yes C38 . C56 . 1.492(11) yes C38 . C39 . 1.38(1) yes C39 . H391 . 1.000 no C39 . C40 . 1.36(1) yes C40 . C57 . 1.489(12) yes C40 . C41 . 1.41(1) yes C41 . H411 . 1.000 no C42 . C47 . 1.37(1) yes C42 . C43 . 1.417(9) yes C43 . H431 . 1.000 no C43 . C44 . 1.378(11) yes C44 . C58 . 1.492(12) yes C44 . C45 . 1.360(12) yes C45 . H451 . 1.000 no C45 . C46 . 1.397(12) yes C46 . C59 . 1.469(12) yes C46 . C47 . 1.405(11) yes C47 . H471 . 1.000 no C48 . C53 . 1.421(9) yes C48 . C49 . 1.40(1) yes C49 . H491 . 1.000 no C49 . C50 . 1.427(12) yes C50 . C60 . 1.491(13) yes C50 . C51 . 1.373(11) yes C51 . H511 . 1.000 no C51 . C52 . 1.382(11) yes C52 . C61 . 1.500(13) yes C52 . C53 . 1.361(11) yes C53 . H531 . 1.000 no C60 . F42 . 1.33(2) yes C60 . F41 . 1.35(2) yes C60 . F40 . 1.315(18) yes C60 . F39 . 1.39(3) yes C60 . F38 . 1.39(3) yes C60 . F37 . 1.23(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C6 . N1 . C4 . 120.6(7) yes C6 . N1 . C1 . 125.6(8) yes C4 . N1 . C1 . 113.8(7) yes C2 . C1 . O1 . 127.3(8) yes C2 . C1 . N1 . 106.6(7) yes O1 . C1 . N1 . 126.0(8) yes C3 . C2 . C5 2_666 121.8(7) yes C3 . C2 . C1 . 107.1(7) yes C5 2_666 C2 . C1 . 131.1(7) yes C5 . C3 . C4 . 130.2(7) yes C5 . C3 . C2 . 122.4(7) yes C4 . C3 . C2 . 107.4(7) yes O2 . C4 . N1 . 126.9(8) yes O2 . C4 . C3 . 128.1(8) yes N1 . C4 . C3 . 105.0(7) yes H51 . C5 . C2 2_666 122.101 no H51 . C5 . C3 . 122.103 no C2 2_666 C5 . C3 . 115.8(7) yes H62 . C6 . H61 . 109.472 no H62 . C6 . C7 . 107.830 no H61 . C6 . C7 . 107.820 no H62 . C6 . N1 . 107.816 no H61 . C6 . N1 . 107.815 no C7 . C6 . N1 . 116.0(2) yes H72 . C7 . H71 . 109.458 no H72 . C7 . C8 . 107.768 no H71 . C7 . C8 . 107.781 no H72 . C7 . C6 . 107.765 no H71 . C7 . C6 . 107.787 no C8 . C7 . C6 . 116.2(2) yes H82 . C8 . H81 . 109.470 no H82 . C8 . C109 . 128.597 no H81 . C8 . C109 . 32.973 no H82 . C8 . C9 . 107.772 no H81 . C8 . C9 . 107.803 no C109 . C8 . C9 . 75.9(13) yes H82 . C8 . C7 . 107.772 no H81 . C8 . C7 . 107.789 no C109 . C8 . C7 . 116.2(2) yes C9 . C8 . C7 . 116.1(2) yes H92 . C9 . H91 . 109.460 no H92 . C9 . C10 . 107.774 no H91 . C9 . C10 . 107.767 no H92 . C9 . C8 . 107.789 no H91 . C9 . C8 . 107.767 no C10 . C9 . C8 . 116.2(2) yes H102 . C10 . H101 . 109.463 no H102 . C10 . C11 . 107.789 no H101 . C10 . C11 . 107.786 no H102 . C10 . C9 . 107.799 no H101 . C10 . C9 . 107.792 no C11 . C10 . C9 . 116.1(2) yes H113 . C11 . H112 . 109.468 no H113 . C11 . H111 . 109.461 no H112 . C11 . H111 . 109.429 no H113 . C11 . C10 . 109.499 no H112 . C11 . C10 . 109.478 no H111 . C11 . C10 . 109.474 no H1092 . C109 . H1091 . 109.456 no H1092 . C109 . H81 . 69.095 no H1091 . C109 . H81 . 107.470 no H1092 . C109 . C110 . 107.792 no H1091 . C109 . C110 . 107.791 no H81 . C109 . C110 . 143.290 no H1092 . C109 . C8 . 107.782 no H1091 . C109 . C8 . 107.778 no H81 . C109 . C8 . 41.409 no C110 . C109 . C8 . 116.1(2) yes H1102 . C110 . H1101 . 109.475 no H1102 . C110 . C111 . 107.788 no H1101 . C110 . C111 . 107.783 no H1102 . C110 . C109 . 107.821 no H1101 . C110 . C109 . 107.813 no C111 . C110 . C109 . 116.1(2) yes H1113 . C111 . H1112 . 109.446 no H1113 . C111 . H1111 . 109.457 no H1112 . C111 . H1111 . 109.439 no H1113 . C111 . C110 . 109.488 no H1112 . C111 . C110 . 109.477 no H1111 . C111 . C110 . 109.489 no O3 . C12 . C21 . 114.7(9) yes O3 . C12 . C13 . 123.0(9) yes C21 . C12 . C13 . 122.3(9) yes H131 . C13 . C14 . 120.692 no H131 . C13 . C12 . 120.690 no C14 . C13 . C12 . 118.6(9) yes H141 . C14 . C15 . 118.850 no H141 . C14 . C13 . 118.849 no C15 . C14 . C13 . 122.3(9) yes H151 . C15 . C16 . 120.611 no H151 . C15 . C14 . 120.614 no C16 . C15 . C14 . 118.8(9) yes C21 . C16 . C17 . 117.3(9) yes C21 . C16 . C15 . 120.0(9) yes C17 . C16 . C15 . 122.7(9) yes C18 . C17 . O7 2_666 126.5(9) yes C18 . C17 . C16 . 121.6(9) yes O7 2_666 C17 . C16 . 111.8(8) yes H181 . C18 . C19 . 119.867 no H181 . C18 . C17 . 119.873 no C19 . C18 . C17 . 120.3(9) yes H191 . C19 . C20 . 118.936 no H191 . C19 . C18 . 118.936 no C20 . C19 . C18 . 122.1(9) yes H201 . C20 . C21 . 120.362 no H201 . C20 . C19 . 120.364 no C21 . C20 . C19 . 119.3(9) yes C12 . C21 . C20 . 122.5(8) yes C12 . C21 . C16 . 118.0(8) yes C20 . C21 . C16 . 119.4(8) yes C22 . O3 . C12 . 119.7(8) yes H222 . C22 . H221 . 109.470 no H222 . C22 . C23 . 109.714 no H221 . C22 . C23 . 109.713 no H222 . C22 . O3 . 109.712 no H221 . C22 . O3 . 109.711 no C23 . C22 . O3 . 108.5(9) yes H232 . C23 . H231 . 109.467 no H232 . C23 . O4 . 109.186 no H231 . C23 . O4 . 109.187 no H232 . C23 . C22 . 109.187 no H231 . C23 . C22 . 109.186 no O4 . C23 . C22 . 110.6(8) yes C24 . O4 . C23 . 115.6(10) yes H242 . C24 . H241 . 109.464 no H242 . C24 . C25 . 109.671 no H241 . C24 . C25 . 109.657 no H242 . C24 . O4 . 109.674 no H241 . C24 . O4 . 109.665 no C25 . C24 . O4 . 108.7(11) yes H252 . C25 . H251 . 109.466 no H252 . C25 . O5 . 109.550 no H251 . C25 . O5 . 109.544 no H252 . C25 . C24 . 109.524 no H251 . C25 . C24 . 109.522 no O5 . C25 . C24 . 109.2(11) yes C26 . O5 . C25 . 111.4(11) yes H262 . C26 . H261 . 109.471 no H262 . C26 . C27 . 109.693 no H261 . C26 . C27 . 109.697 no H262 . C26 . O5 . 109.703 no H261 . C26 . O5 . 109.706 no C27 . C26 . O5 . 108.6(10) yes H272 . C27 . H271 . 109.466 no H272 . C27 . O6 . 109.268 no H271 . C27 . O6 . 109.267 no H272 . C27 . C26 . 109.271 no H271 . C27 . C26 . 109.267 no O6 . C27 . C26 . 110.3(10) yes C28 . O6 . C27 . 115.2(10) yes H282 . C28 . H281 . 109.460 no H282 . C28 . C29 . 109.222 no H281 . C28 . C29 . 109.218 no H282 . C28 . O6 . 109.224 no H281 . C28 . O6 . 109.219 no C29 . C28 . O6 . 110.5(9) yes H292 . C29 . H291 . 109.461 no H292 . C29 . O7 . 110.122 no H291 . C29 . O7 . 110.116 no H292 . C29 . C28 . 110.121 no H291 . C29 . C28 . 110.118 no O7 . C29 . C28 . 106.9(10) yes C17 2_666 O7 . C29 . 115.7(8) yes C48 . B1 . C42 . 108.1(6) yes C48 . B1 . C36 . 110.4(6) yes C42 . B1 . C36 . 108.9(6) yes C48 . B1 . C30 . 109.2(6) yes C42 . B1 . C30 . 111.0(6) yes C36 . B1 . C30 . 109.3(6) yes C35 . C30 . C31 . 115.3(5) yes C35 . C30 . B1 . 124.9(6) yes C31 . C30 . B1 . 119.8(5) yes H311 . C31 . C32 . 119.009 no H311 . C31 . C30 . 119.008 no C32 . C31 . C30 . 122.0(6) yes C54 . C32 . C33 . 122.3(6) yes C54 . C32 . C31 . 116.6(5) yes C33 . C32 . C31 . 121.1(6) yes H331 . C33 . C34 . 120.935 no H331 . C33 . C32 . 120.935 no C34 . C33 . C32 . 118.1(6) yes C55 . C34 . C35 . 121.5(6) yes C55 . C34 . C33 . 118.2(6) yes C35 . C34 . C33 . 120.4(7) yes H351 . C35 . C34 . 118.445 no H351 . C35 . C30 . 118.444 no C34 . C35 . C30 . 123.1(6) yes C41 . C36 . C37 . 116.3(5) yes C41 . C36 . B1 . 121.5(6) yes C37 . C36 . B1 . 122.2(6) yes H371 . C37 . C38 . 119.586 no H371 . C37 . C36 . 119.587 no C38 . C37 . C36 . 120.8(6) yes C56 . C38 . C39 . 118.2(6) yes C56 . C38 . C37 . 119.6(5) yes C39 . C38 . C37 . 122.2(6) yes H391 . C39 . C40 . 121.268 no H391 . C39 . C38 . 121.267 no C40 . C39 . C38 . 117.5(6) yes C57 . C40 . C41 . 119.7(6) yes C57 . C40 . C39 . 119.0(7) yes C41 . C40 . C39 . 121.3(7) yes H411 . C41 . C36 . 119.114 no H411 . C41 . C40 . 119.117 no C36 . C41 . C40 . 121.8(6) yes C47 . C42 . C43 . 114.8(6) yes C47 . C42 . B1 . 124.1(6) yes C43 . C42 . B1 . 120.9(6) yes H431 . C43 . C44 . 119.613 no H431 . C43 . C42 . 119.613 no C44 . C43 . C42 . 120.8(7) yes C58 . C44 . C45 . 118.3(7) yes C58 . C44 . C43 . 118.3(7) yes C45 . C44 . C43 . 123.2(8) yes H451 . C45 . C46 . 120.989 no H451 . C45 . C44 . 120.989 no C46 . C45 . C44 . 118.0(7) yes C59 . C46 . C47 . 120.3(6) yes C59 . C46 . C45 . 121.7(7) yes C47 . C46 . C45 . 118.0(7) yes H471 . C47 . C42 . 117.500 no H471 . C47 . C46 . 117.500 no C42 . C47 . C46 . 125.0(6) yes C53 . C48 . C49 . 115.1(6) yes C53 . C48 . B1 . 121.7(6) yes C49 . C48 . B1 . 123.0(6) yes H491 . C49 . C50 . 119.181 no H491 . C49 . C48 . 119.182 no C50 . C49 . C48 . 121.6(6) yes C60 . C50 . C51 . 119.3(7) yes C60 . C50 . C49 . 120.2(6) yes C51 . C50 . C49 . 120.5(8) yes H511 . C51 . C52 . 121.001 no H511 . C51 . C50 . 120.999 no C52 . C51 . C50 . 118.0(8) yes C61 . C52 . C53 . 118.5(6) yes C61 . C52 . C51 . 119.4(7) yes C53 . C52 . C51 . 122.1(8) yes H531 . C53 . C52 . 118.779 no H531 . C53 . C48 . 118.776 no C52 . C53 . C48 . 122.4(7) yes F42 . C60 . F41 . 101.1(11) yes F42 . C60 . F40 . 113.0(11) yes F41 . C60 . F40 . 102.5(11) yes F42 . C60 . F39 . 73.9(12) yes F41 . C60 . F39 . 135.4(10) yes F40 . C60 . F39 . 46.4(10) yes F42 . C60 . F38 . 132.2(11) yes F41 . C60 . F38 . 44.6(11) yes F40 . C60 . F38 . 61.9(12) yes F39 . C60 . F38 . 106.4(12) yes F42 . C60 . F37 . 38.7(11) yes F41 . C60 . F37 . 63.8(12) yes F40 . C60 . F37 . 129.2(10) yes F39 . C60 . F37 . 107.8(12) yes F38 . C60 . F37 . 104.0(13) yes F42 . C60 . C50 . 111.3(8) yes F41 . C60 . C50 . 112.9(8) yes F40 . C60 . C50 . 115.0(8) yes F39 . C60 . C50 . 109.9(8) yes F38 . C60 . C50 . 113.0(8) yes F37 . C60 . C50 . 115.2(8) yes C109 . H81 . C8 . 105.617 no #===END