Electronic Supplementary Information for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sofia Ioana Pascu' _publ_contact_author_address ; Chemistry Research Laboratory University of Oxford 12 Mansfield Road Oxford Oxfordshire OX1 3TA UNITED KINGDOM ; _publ_contact_author_email SOFIA.PASCU@CHEM.OX.AC.UK _publ_section_title ; Structures and solution dynamics of pseudorotaxanes mediated by alkali-metal cations ; loop_ _publ_author_name 'Sofia Ioana Pascu' 'Andrew D. Bond' 'Thibaut Jarrosson' 'Guido Kaiser' 'Christoph Naumann' 'J. Sanders' data_[1.A] _database_code_depnum_ccdc_archive 'CCDC 644501' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O10, C26 H30 N2 O4, 2(C H Cl3)' _chemical_formula_sum 'C64 H76 Cl6 N2 O14' _chemical_formula_weight 1309.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9237(3) _cell_length_b 12.3078(3) _cell_length_c 13.8877(4) _cell_angle_alpha 67.987(1) _cell_angle_beta 86.014(1) _cell_angle_gamma 69.563(2) _cell_volume 1618.03(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 11095 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 17731 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _reflns_number_total 7299 _reflns_number_gt 4766 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_data_reduction Denzo/Scalepack _computing_structure_solution 'SHELXTL v6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+1.2030P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7299 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.324 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.054 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.53864(19) 0.62928(19) 0.17766(15) 0.0513(5) Uani 1 1 d . . . O2 O 0.36682(18) 0.89051(16) 0.35135(16) 0.0458(5) Uani 1 1 d . . . O3 O 0.62850(17) 0.72427(17) 0.70472(16) 0.0465(5) Uani 1 1 d . . . O4 O 0.42087(18) 0.75066(18) 0.83141(15) 0.0456(5) Uani 1 1 d . . . O5 O 0.20770(18) 0.66427(17) 0.89801(15) 0.0450(5) Uani 1 1 d . . . O6 O 0.08526(16) 0.65032(18) 0.73082(16) 0.0452(5) Uani 1 1 d . . . O7 O 0.11630(18) 0.57236(16) 0.55517(16) 0.0469(5) Uani 1 1 d . . . N1 N 0.4554(2) 0.75958(19) 0.26519(17) 0.0374(5) Uani 1 1 d . . . C1 C 0.4147(2) 0.7828(2) 0.3549(2) 0.0347(6) Uani 1 1 d . . . C2 C 0.5107(2) 0.6407(2) 0.2602(2) 0.0364(6) Uani 1 1 d . . . C3 C 0.5322(2) 0.5321(2) 0.3601(2) 0.0307(5) Uani 1 1 d . . . C4 C 0.4911(2) 0.5517(2) 0.45270(19) 0.0267(5) Uani 1 1 d . . . C5 C 0.4321(2) 0.6738(2) 0.4530(2) 0.0296(5) Uani 1 1 d . . . C6 C 0.3921(2) 0.6902(2) 0.5444(2) 0.0345(6) Uani 1 1 d . . . H6A H 0.3522 0.7725 0.5438 0.041 Uiso 1 1 calc R . . C7 C 0.4091(2) 0.5878(2) 0.6381(2) 0.0353(6) Uani 1 1 d . . . H7A H 0.3803 0.6008 0.7003 0.042 Uiso 1 1 calc R . . C8 C 0.4344(3) 0.8698(3) 0.1676(2) 0.0479(7) Uani 1 1 d . . . H8A H 0.4948 0.8453 0.1168 0.057 Uiso 1 1 calc R . . H8B H 0.4558 0.9345 0.1817 0.057 Uiso 1 1 calc R . . C9 C 0.2948(3) 0.9250(2) 0.1202(2) 0.0415(6) Uani 1 1 d . . . H9A H 0.2335 0.9263 0.1761 0.050 Uiso 1 1 calc R . . H9B H 0.2815 0.8713 0.0867 0.050 Uiso 1 1 calc R . . C10 C 0.2641(3) 1.0583(3) 0.0391(3) 0.0618(9) Uani 1 1 d . . . H10A H 0.2921 1.1074 0.0698 0.074 Uiso 1 1 calc R . . H10B H 0.3164 1.0544 -0.0214 0.074 Uiso 1 1 calc R . . C11 C 0.1211(3) 1.1262(3) 0.0012(2) 0.0543(8) Uani 1 1 d . . . H11A H 0.0676 1.1184 0.0624 0.065 Uiso 1 1 calc R . . H11B H 0.0967 1.0848 -0.0394 0.065 Uiso 1 1 calc R . . C12 C 0.0872(3) 1.2651(3) -0.0664(3) 0.0590(8) Uani 1 1 d . . . H12A H -0.0090 1.3043 -0.0813 0.071 Uiso 1 1 calc R . . H12B H 0.1139 1.3062 -0.0266 0.071 Uiso 1 1 calc R . . C13 C 0.1510(3) 1.2885(3) -0.1667(3) 0.0625(9) Uani 1 1 d . . . H13A H 0.1254 1.3788 -0.2059 0.094 Uiso 1 1 calc R . . H13B H 0.1233 1.2501 -0.2075 0.094 Uiso 1 1 calc R . . H13C H 0.2464 1.2519 -0.1527 0.094 Uiso 1 1 calc R . . C14 C 0.8420(2) 0.4387(2) 0.5369(2) 0.0381(6) Uani 1 1 d . . . C15 C 0.8599(3) 0.3412(2) 0.6302(2) 0.0456(7) Uani 1 1 d . . . H15A H 0.9039 0.2578 0.6345 0.055 Uiso 1 1 calc R . . C16 C 0.8131(3) 0.3645(3) 0.7196(3) 0.0490(8) Uani 1 1 d . . . H16A H 0.8258 0.2961 0.7842 0.059 Uiso 1 1 calc R . . C17 C 0.7496(2) 0.4839(3) 0.7161(2) 0.0422(7) Uani 1 1 d . . . H17A H 0.7186 0.4977 0.7776 0.051 Uiso 1 1 calc R . . C18 C 0.6663(2) 0.7125(2) 0.6123(2) 0.0381(6) Uani 1 1 d . . . C19 C 0.6923(2) 0.7865(2) 0.4285(2) 0.0422(7) Uani 1 1 d . . . H19A H 0.6784 0.8548 0.3637 0.051 Uiso 1 1 calc R . . C20 C 0.6481(2) 0.8099(2) 0.5188(2) 0.0416(7) Uani 1 1 d . . . H20A H 0.6056 0.8934 0.5147 0.050 Uiso 1 1 calc R . . C21 C 0.7551(2) 0.6668(2) 0.4324(2) 0.0400(6) Uani 1 1 d . . . H21A H 0.7848 0.6523 0.3709 0.048 Uiso 1 1 calc R . . C22 C 0.7753(2) 0.5652(2) 0.5289(2) 0.0361(6) Uani 1 1 d . . . C23 C 0.7305(2) 0.5858(2) 0.6204(2) 0.0354(6) Uani 1 1 d . . . C24 C 0.5434(3) 0.8447(3) 0.7011(3) 0.0511(8) Uani 1 1 d . . . H24A H 0.4673 0.8776 0.6505 0.061 Uiso 1 1 calc R . . H24B H 0.5907 0.9046 0.6801 0.061 Uiso 1 1 calc R . . C25 C 0.4990(3) 0.8262(3) 0.8089(3) 0.0562(8) Uani 1 1 d . . . H25A H 0.5758 0.7851 0.8600 0.067 Uiso 1 1 calc R . . H25B H 0.4477 0.9080 0.8134 0.067 Uiso 1 1 calc R . . C26 C 0.3827(3) 0.7185(3) 0.9349(2) 0.0527(8) Uani 1 1 d . . . H26A H 0.3157 0.7924 0.9433 0.063 Uiso 1 1 calc R . . H26B H 0.4592 0.6898 0.9839 0.063 Uiso 1 1 calc R . . C27 C 0.3281(3) 0.6170(3) 0.9577(2) 0.0550(8) Uani 1 1 d . . . H27A H 0.3909 0.5475 0.9404 0.066 Uiso 1 1 calc R . . H27B H 0.3139 0.5840 1.0327 0.066 Uiso 1 1 calc R . . C28 C 0.1594(3) 0.5677(3) 0.9078(3) 0.0508(8) Uani 1 1 d . . . H28A H 0.1347 0.5325 0.9798 0.061 Uiso 1 1 calc R . . H28B H 0.2282 0.4997 0.8928 0.061 Uiso 1 1 calc R . . C29 C 0.0431(3) 0.6202(3) 0.8333(3) 0.0514(8) Uani 1 1 d . . . H29A H -0.0007 0.5581 0.8474 0.062 Uiso 1 1 calc R . . H29B H -0.0203 0.6961 0.8412 0.062 Uiso 1 1 calc R . . C30 C -0.0164(3) 0.6797(3) 0.6562(3) 0.0539(8) Uani 1 1 d . . . H30A H -0.0875 0.7582 0.6521 0.065 Uiso 1 1 calc R . . H30B H -0.0535 0.6120 0.6781 0.065 Uiso 1 1 calc R . . C31 C 0.0364(3) 0.6945(3) 0.5528(3) 0.0495(8) Uani 1 1 d . . . H31A H -0.0363 0.7333 0.4982 0.059 Uiso 1 1 calc R . . H31B H 0.0895 0.7491 0.5368 0.059 Uiso 1 1 calc R . . C32 C 0.1002(3) 0.9312(2) 0.7061(2) 0.0394(6) Uani 1 1 d . . . H32A H 0.1397 0.8392 0.7465 0.047 Uiso 1 1 calc R . . Cl1 Cl -0.07007(7) 0.97318(7) 0.68530(6) 0.0505(2) Uani 1 1 d . . . Cl2 Cl 0.12989(8) 1.01300(7) 0.77729(7) 0.0557(2) Uani 1 1 d . . . Cl3 Cl 0.17002(7) 0.96956(7) 0.58526(6) 0.0541(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0573(12) 0.0542(13) 0.0349(12) -0.0134(10) 0.0069(9) -0.0151(10) O2 0.0467(11) 0.0232(9) 0.0599(13) -0.0100(9) -0.0110(9) -0.0068(8) O3 0.0421(10) 0.0399(11) 0.0539(13) -0.0164(10) 0.0022(9) -0.0113(8) O4 0.0514(11) 0.0523(12) 0.0444(12) -0.0254(10) 0.0022(9) -0.0233(9) O5 0.0460(11) 0.0391(11) 0.0414(11) -0.0090(9) 0.0014(9) -0.0111(8) O6 0.0320(9) 0.0505(12) 0.0589(13) -0.0237(10) 0.0030(9) -0.0177(8) O7 0.0447(11) 0.0308(10) 0.0596(14) -0.0171(10) -0.0104(9) -0.0039(8) N1 0.0359(11) 0.0315(12) 0.0368(13) -0.0034(10) 0.0003(9) -0.0122(9) C1 0.0268(12) 0.0271(13) 0.0451(16) -0.0070(12) -0.0075(11) -0.0088(10) C2 0.0316(13) 0.0359(14) 0.0387(16) -0.0106(12) -0.0008(11) -0.0112(11) C3 0.0236(11) 0.0309(13) 0.0366(14) -0.0120(11) -0.0013(10) -0.0085(9) C4 0.0204(10) 0.0247(12) 0.0355(14) -0.0113(10) -0.0030(9) -0.0076(9) C5 0.0222(11) 0.0249(12) 0.0401(15) -0.0109(11) -0.0053(10) -0.0065(9) C6 0.0297(12) 0.0270(13) 0.0478(16) -0.0187(12) -0.0026(11) -0.0051(10) C7 0.0309(12) 0.0364(14) 0.0397(15) -0.0180(12) 0.0014(11) -0.0088(10) C8 0.0465(16) 0.0379(15) 0.0431(17) 0.0034(13) 0.0034(13) -0.0161(12) C9 0.0454(15) 0.0383(15) 0.0338(15) -0.0059(12) 0.0012(12) -0.0143(12) C10 0.0560(19) 0.058(2) 0.053(2) 0.0058(17) -0.0067(15) -0.0259(16) C11 0.0591(19) 0.0524(19) 0.0419(18) -0.0077(15) -0.0010(14) -0.0184(15) C12 0.065(2) 0.0470(18) 0.051(2) -0.0157(16) 0.0003(16) -0.0057(15) C13 0.072(2) 0.0437(18) 0.059(2) -0.0102(16) 0.0010(17) -0.0150(16) C14 0.0320(13) 0.0302(14) 0.0501(18) -0.0116(13) -0.0110(12) -0.0098(10) C15 0.0422(15) 0.0260(14) 0.062(2) -0.0091(14) -0.0165(14) -0.0080(11) C16 0.0448(16) 0.0336(15) 0.057(2) 0.0022(14) -0.0162(14) -0.0169(12) C17 0.0362(14) 0.0398(15) 0.0458(17) -0.0065(13) -0.0056(12) -0.0165(12) C18 0.0268(12) 0.0336(14) 0.0523(18) -0.0110(13) -0.0032(12) -0.0129(10) C19 0.0343(13) 0.0318(14) 0.0506(18) -0.0006(13) -0.0033(12) -0.0149(11) C20 0.0313(13) 0.0281(14) 0.061(2) -0.0103(13) 0.0020(12) -0.0115(11) C21 0.0336(13) 0.0334(14) 0.0478(17) -0.0081(13) -0.0035(12) -0.0123(11) C22 0.0250(12) 0.0291(13) 0.0505(17) -0.0071(12) -0.0095(11) -0.0113(10) C23 0.0270(12) 0.0308(13) 0.0452(16) -0.0073(12) -0.0062(11) -0.0124(10) C24 0.0469(16) 0.0413(16) 0.075(2) -0.0285(16) 0.0078(15) -0.0203(13) C25 0.0559(18) 0.058(2) 0.074(2) -0.0417(18) 0.0062(16) -0.0250(15) C26 0.0597(18) 0.0577(19) 0.0369(17) -0.0210(15) -0.0105(14) -0.0097(15) C27 0.064(2) 0.0537(19) 0.0319(16) -0.0034(14) -0.0073(14) -0.0138(15) C28 0.0550(18) 0.0365(15) 0.0533(19) -0.0086(14) 0.0161(15) -0.0181(13) C29 0.0412(15) 0.0448(17) 0.069(2) -0.0206(16) 0.0184(15) -0.0200(13) C30 0.0312(14) 0.0505(18) 0.089(3) -0.0378(18) -0.0060(15) -0.0098(13) C31 0.0402(15) 0.0347(15) 0.071(2) -0.0219(15) -0.0168(14) -0.0042(12) C32 0.0432(14) 0.0315(14) 0.0410(16) -0.0150(12) 0.0041(12) -0.0086(11) Cl1 0.0442(4) 0.0505(4) 0.0591(5) -0.0259(4) 0.0055(3) -0.0139(3) Cl2 0.0627(5) 0.0491(4) 0.0604(5) -0.0290(4) -0.0029(4) -0.0149(3) Cl3 0.0575(4) 0.0447(4) 0.0522(5) -0.0186(4) 0.0170(3) -0.0104(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.212(3) . ? O2 C1 1.226(3) . ? O3 C18 1.364(3) . ? O3 C24 1.433(3) . ? O4 C25 1.410(3) . ? O4 C26 1.415(4) . ? O5 C27 1.418(3) . ? O5 C28 1.420(3) . ? O6 C29 1.417(4) . ? O6 C30 1.427(3) . ? O7 C14 1.366(3) 2_666 ? O7 C31 1.439(3) . ? N1 C1 1.390(3) . ? N1 C2 1.402(3) . ? N1 C8 1.476(3) . ? C1 C5 1.477(4) . ? C2 C3 1.484(4) . ? C3 C7 1.379(3) 2_666 ? C3 C4 1.411(3) . ? C4 C4 1.412(5) 2_666 ? C4 C5 1.414(3) . ? C5 C6 1.377(4) . ? C6 C7 1.398(4) . ? C6 H6A 0.950 . ? C7 C3 1.379(3) 2_666 ? C7 H7A 0.950 . ? C8 C9 1.517(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.535(4) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C10 C11 1.513(4) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 C12 1.531(4) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.488(5) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 C15 1.365(4) . ? C14 O7 1.367(3) 2_666 ? C14 C22 1.434(3) . ? C15 C16 1.401(4) . ? C15 H15A 0.950 . ? C16 C17 1.371(4) . ? C16 H16A 0.950 . ? C17 C23 1.411(4) . ? C17 H17A 0.950 . ? C18 C20 1.366(4) . ? C18 C23 1.432(4) . ? C19 C21 1.372(4) . ? C19 C20 1.406(4) . ? C19 H19A 0.950 . ? C20 H20A 0.950 . ? C21 C22 1.414(4) . ? C21 H21A 0.950 . ? C22 C23 1.410(4) . ? C24 C25 1.500(4) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.488(4) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 C29 1.487(4) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 C31 1.481(5) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 Cl3 1.761(3) . ? C32 Cl1 1.761(3) . ? C32 Cl2 1.765(3) . ? C32 H32A 1.000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 O3 C24 117.5(2) . . ? C25 O4 C26 113.2(2) . . ? C27 O5 C28 111.7(2) . . ? C29 O6 C30 111.8(2) . . ? C14 O7 C31 117.9(2) 2_666 . ? C1 N1 C2 125.2(2) . . ? C1 N1 C8 116.7(2) . . ? C2 N1 C8 118.1(2) . . ? O2 C1 N1 120.4(2) . . ? O2 C1 C5 122.0(3) . . ? N1 C1 C5 117.6(2) . . ? O1 C2 N1 120.7(2) . . ? O1 C2 C3 122.8(2) . . ? N1 C2 C3 116.6(2) . . ? C7 C3 C4 120.2(2) 2_666 . ? C7 C3 C2 119.9(2) 2_666 . ? C4 C3 C2 119.9(2) . . ? C3 C4 C4 119.8(3) . 2_666 ? C3 C4 C5 121.2(2) . . ? C4 C4 C5 118.9(3) 2_666 . ? C6 C5 C4 120.0(2) . . ? C6 C5 C1 120.6(2) . . ? C4 C5 C1 119.4(2) . . ? C5 C6 C7 121.2(2) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C3 C7 C6 119.9(2) 2_666 . ? C3 C7 H7A 120.1 2_666 . ? C6 C7 H7A 120.1 . . ? N1 C8 C9 112.6(2) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 111.6(2) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 114.2(3) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 C12 114.1(3) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 113.7(3) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 O7 125.1(2) . 2_666 ? C15 C14 C22 120.9(3) . . ? O7 C14 C22 114.0(2) 2_666 . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 121.6(3) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? C16 C17 C23 119.5(3) . . ? C16 C17 H17A 120.3 . . ? C23 C17 H17A 120.3 . . ? O3 C18 C20 125.0(2) . . ? O3 C18 C23 114.0(2) . . ? C20 C18 C23 121.0(3) . . ? C21 C19 C20 121.2(3) . . ? C21 C19 H19A 119.4 . . ? C20 C19 H19A 119.4 . . ? C18 C20 C19 120.0(2) . . ? C18 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C19 C21 C22 119.4(3) . . ? C19 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 120.7(2) . . ? C23 C22 C14 118.0(2) . . ? C21 C22 C14 121.3(3) . . ? C22 C23 C17 120.3(2) . . ? C22 C23 C18 117.8(2) . . ? C17 C23 C18 121.9(3) . . ? O3 C24 C25 106.2(3) . . ? O3 C24 H24A 110.5 . . ? C25 C24 H24A 110.5 . . ? O3 C24 H24B 110.5 . . ? C25 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? O4 C25 C24 108.5(2) . . ? O4 C25 H25A 110.0 . . ? C24 C25 H25A 110.0 . . ? O4 C25 H25B 110.0 . . ? C24 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O4 C26 C27 108.7(2) . . ? O4 C26 H26A 110.0 . . ? C27 C26 H26A 110.0 . . ? O4 C26 H26B 110.0 . . ? C27 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? O5 C27 C26 109.6(2) . . ? O5 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? O5 C27 H27B 109.7 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? O5 C28 C29 109.1(2) . . ? O5 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? O5 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? O6 C29 C28 108.6(2) . . ? O6 C29 H29A 110.0 . . ? C28 C29 H29A 110.0 . . ? O6 C29 H29B 110.0 . . ? C28 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? O6 C30 C31 109.9(2) . . ? O6 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? O6 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? O7 C31 C30 108.1(2) . . ? O7 C31 H31A 110.1 . . ? C30 C31 H31A 110.1 . . ? O7 C31 H31B 110.1 . . ? C30 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? Cl3 C32 Cl1 109.47(15) . . ? Cl3 C32 Cl2 109.92(15) . . ? Cl1 C32 Cl2 109.09(14) . . ? Cl3 C32 H32A 109.5 . . ? Cl1 C32 H32A 109.5 . . ? Cl2 C32 H32A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 O2 -179.7(2) . . . . ? C8 N1 C1 O2 -1.6(3) . . . . ? C2 N1 C1 C5 0.5(3) . . . . ? C8 N1 C1 C5 178.6(2) . . . . ? C1 N1 C2 O1 177.1(2) . . . . ? C8 N1 C2 O1 -1.0(4) . . . . ? C1 N1 C2 C3 -2.8(3) . . . . ? C8 N1 C2 C3 179.1(2) . . . . ? O1 C2 C3 C7 2.6(4) . . . 2_666 ? N1 C2 C3 C7 -177.5(2) . . . 2_666 ? O1 C2 C3 C4 -176.6(2) . . . . ? N1 C2 C3 C4 3.3(3) . . . . ? C7 C3 C4 C4 -0.6(4) 2_666 . . 2_666 ? C2 C3 C4 C4 178.6(2) . . . 2_666 ? C7 C3 C4 C5 179.2(2) 2_666 . . . ? C2 C3 C4 C5 -1.6(3) . . . . ? C3 C4 C5 C6 179.6(2) . . . . ? C4 C4 C5 C6 -0.6(4) 2_666 . . . ? C3 C4 C5 C1 -0.8(3) . . . . ? C4 C4 C5 C1 179.0(2) 2_666 . . . ? O2 C1 C5 C6 1.3(3) . . . . ? N1 C1 C5 C6 -179.0(2) . . . . ? O2 C1 C5 C4 -178.4(2) . . . . ? N1 C1 C5 C4 1.4(3) . . . . ? C4 C5 C6 C7 0.3(3) . . . . ? C1 C5 C6 C7 -179.4(2) . . . . ? C5 C6 C7 C3 0.5(4) . . . 2_666 ? C1 N1 C8 C9 -80.3(3) . . . . ? C2 N1 C8 C9 98.0(3) . . . . ? N1 C8 C9 C10 163.2(3) . . . . ? C8 C9 C10 C11 -170.9(3) . . . . ? C9 C10 C11 C12 171.0(3) . . . . ? C10 C11 C12 C13 64.7(4) . . . . ? O7 C14 C15 C16 179.7(2) 2_666 . . . ? C22 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C15 C16 C17 C23 0.0(4) . . . . ? C24 O3 C18 C20 11.7(3) . . . . ? C24 O3 C18 C23 -169.0(2) . . . . ? O3 C18 C20 C19 179.4(2) . . . . ? C23 C18 C20 C19 0.2(4) . . . . ? C21 C19 C20 C18 -0.7(4) . . . . ? C20 C19 C21 C22 0.2(4) . . . . ? C19 C21 C22 C23 0.6(4) . . . . ? C19 C21 C22 C14 -179.2(2) . . . . ? C15 C14 C22 C23 0.9(4) . . . . ? O7 C14 C22 C23 -179.1(2) 2_666 . . . ? C15 C14 C22 C21 -179.4(2) . . . . ? O7 C14 C22 C21 0.7(3) 2_666 . . . ? C21 C22 C23 C17 179.2(2) . . . . ? C14 C22 C23 C17 -1.0(3) . . . . ? C21 C22 C23 C18 -1.0(3) . . . . ? C14 C22 C23 C18 178.8(2) . . . . ? C16 C17 C23 C22 0.6(4) . . . . ? C16 C17 C23 C18 -179.2(2) . . . . ? O3 C18 C23 C22 -178.7(2) . . . . ? C20 C18 C23 C22 0.6(3) . . . . ? O3 C18 C23 C17 1.1(3) . . . . ? C20 C18 C23 C17 -179.6(2) . . . . ? C18 O3 C24 C25 170.2(2) . . . . ? C26 O4 C25 C24 175.0(2) . . . . ? O3 C24 C25 O4 -66.1(3) . . . . ? C25 O4 C26 C27 -167.2(2) . . . . ? C28 O5 C27 C26 173.1(2) . . . . ? O4 C26 C27 O5 -68.3(3) . . . . ? C27 O5 C28 C29 -172.7(2) . . . . ? C30 O6 C29 C28 169.4(2) . . . . ? O5 C28 C29 O6 69.3(3) . . . . ? C29 O6 C30 C31 -172.7(2) . . . . ? C14 O7 C31 C30 169.7(2) 2_666 . . . ? O6 C30 C31 O7 72.6(3) . . . . ? #============================================================================== data_[Li2.1.A]I2 _database_code_depnum_ccdc_archive 'CCDC 644502' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H82 Li2 N2 O16 2+, 2(I -), 4(C H Cl3)' _chemical_formula_sum 'C68 H86 Cl12 I2 Li2 N2 O16' _chemical_formula_weight 1880.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1350(5) _cell_length_b 10.6602(2) _cell_length_c 32.3295(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.692(1) _cell_angle_gamma 90.00 _cell_volume 4173.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23289 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 19389 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.05 _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.943 _reflns_number_total 6987 _reflns_number_gt 4436 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_data_reduction Denzo/Scalepack _computing_structure_solution 'SHELXTL v6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+12.0177P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6987 _refine_ls_number_parameters 455 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2072 _refine_ls_wR_factor_gt 0.1829 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.535 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.106 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.64315(4) 0.99558(4) 0.311508(17) 0.0527(2) Uani 1 1 d . . . Li1 Li 0.7145(11) 0.5898(11) 0.3571(4) 0.057(3) Uani 1 1 d . . . O1 O 0.8738(4) 0.4996(4) 0.47573(17) 0.0519(13) Uani 1 1 d . . . O2 O 0.8653(4) 0.4916(4) 0.3887(2) 0.0629(15) Uani 1 1 d . . . O3 O 0.7212(5) 0.4224(5) 0.33037(19) 0.0748(18) Uani 1 1 d . . . O4 O 0.5444(4) 0.5689(5) 0.32343(17) 0.0589(14) Uani 1 1 d . . . O5 O 0.3655(4) 0.6183(5) 0.37287(19) 0.0624(15) Uani 1 1 d . . . O7 O 0.5670(4) 0.8820(4) 0.52030(15) 0.0524(13) Uani 1 1 d . . . O6 O 0.6625(4) 0.6770(4) 0.40520(14) 0.0435(11) Uani 1 1 d . . . O8 O 0.7831(4) 0.7223(5) 0.33130(19) 0.0695(17) Uani 1 1 d . . . H8 H 0.7456 0.7896 0.3294 0.083 Uiso 1 1 d R . . N1 N 0.6031(4) 0.7814(5) 0.46037(16) 0.0373(12) Uani 1 1 d . . . C1 C 0.8291(5) 0.5307(6) 0.5120(3) 0.0465(18) Uani 1 1 d . . . C2 C 0.8311(6) 0.6485(6) 0.5289(3) 0.053(2) Uani 1 1 d . . . H2A H 0.8630 0.7164 0.5149 0.064 Uiso 1 1 calc R . . C3 C 0.7854(6) 0.6680(7) 0.5673(3) 0.058(2) Uani 1 1 d . . . H3A H 0.7892 0.7495 0.5792 0.070 Uiso 1 1 calc R . . C4 C 0.7362(6) 0.5748(7) 0.5880(3) 0.058(2) Uani 1 1 d . . . H4A H 0.7051 0.5912 0.6137 0.070 Uiso 1 1 calc R . . C5 C 0.7320(5) 0.4532(7) 0.5707(3) 0.0484(18) Uani 1 1 d . . . C6 C 0.7784(5) 0.4287(6) 0.5327(3) 0.0476(18) Uani 1 1 d . . . C7 C 0.6801(6) 0.3508(7) 0.5911(3) 0.0524(19) Uani 1 1 d . . . C8 C 0.6792(6) 0.2316(7) 0.5737(3) 0.055(2) Uani 1 1 d . . . H8A H 0.6454 0.1638 0.5872 0.066 Uiso 1 1 calc R . . C9 C 0.7284(6) 0.2116(7) 0.5362(3) 0.057(2) Uani 1 1 d . . . H9A H 0.7281 0.1294 0.5249 0.069 Uiso 1 1 calc R . . C10 C 0.7763(6) 0.3057(7) 0.5154(3) 0.0536(19) Uani 1 1 d . . . H10A H 0.8079 0.2898 0.4898 0.064 Uiso 1 1 calc R . . C11 C 0.9161(6) 0.5994(7) 0.4515(3) 0.0516(19) Uani 1 1 d . . . H11A H 0.9779 0.6417 0.4674 0.062 Uiso 1 1 calc R . . H11B H 0.8575 0.6622 0.4450 0.062 Uiso 1 1 calc R . . C12 C 0.9553(6) 0.5462(8) 0.4126(3) 0.061(2) Uani 1 1 d . . . H12A H 0.9889 0.6133 0.3964 0.073 Uiso 1 1 calc R . . H12B H 1.0123 0.4817 0.4193 0.073 Uiso 1 1 calc R . . C13 C 0.8898(8) 0.3875(8) 0.3659(3) 0.081(3) Uani 1 1 d . . . H13A H 0.9264 0.3244 0.3845 0.097 Uiso 1 1 calc R . . H13B H 0.9427 0.4117 0.3452 0.097 Uiso 1 1 calc R . . C14 C 0.7948(7) 0.3320(7) 0.3448(3) 0.069(2) Uani 1 1 d . . . H14A H 0.8179 0.2811 0.3213 0.082 Uiso 1 1 calc R . . H14B H 0.7583 0.2756 0.3641 0.082 Uiso 1 1 calc R . . C15 C 0.6270(7) 0.3798(8) 0.3056(3) 0.066(2) Uani 1 1 d . . . H15A H 0.5818 0.3238 0.3221 0.080 Uiso 1 1 calc R . . H15B H 0.6510 0.3319 0.2815 0.080 Uiso 1 1 calc R . . C16 C 0.5628(10) 0.4867(9) 0.2915(4) 0.098(4) Uani 1 1 d . . . H16A H 0.6019 0.5313 0.2699 0.118 Uiso 1 1 calc R . . H16B H 0.4909 0.4577 0.2787 0.118 Uiso 1 1 calc R . . C17 C 0.4605(7) 0.6618(8) 0.3131(3) 0.064(2) Uani 1 1 d . . . H17A H 0.3990 0.6226 0.2961 0.076 Uiso 1 1 calc R . . H17B H 0.4920 0.7294 0.2965 0.076 Uiso 1 1 calc R . . C18 C 0.4183(6) 0.7156(7) 0.3511(2) 0.0544(19) Uani 1 1 d . . . H18A H 0.4800 0.7515 0.3688 0.065 Uiso 1 1 calc R . . H18B H 0.3650 0.7835 0.3437 0.065 Uiso 1 1 calc R . . C20 C 0.4685(6) 0.6654(6) 0.5535(2) 0.0446(17) Uani 1 1 d . . . H19 H 0.4648 0.7403 0.5693 0.054 Uiso 1 1 calc R . . C19 C 0.4246(6) 0.5548(6) 0.5683(2) 0.0447(17) Uani 1 1 d . . . H20 H 0.3914 0.5550 0.5941 0.054 Uiso 1 1 calc R . . C23 C 0.5713(5) 0.5552(6) 0.4541(2) 0.0357(15) Uani 1 1 d . . . C22 C 0.5222(5) 0.5563(6) 0.4923(2) 0.0336(14) Uani 1 1 d . . . C21 C 0.5175(5) 0.6679(6) 0.5161(2) 0.0380(15) Uani 1 1 d . . . C25 C 0.5634(5) 0.7845(6) 0.5003(2) 0.0401(16) Uani 1 1 d . . . C24 C 0.6156(5) 0.6731(6) 0.4378(2) 0.0374(15) Uani 1 1 d . . . C26 C 0.6403(5) 0.9023(6) 0.4428(2) 0.0424(16) Uani 1 1 d . . . H26A H 0.5967 0.9715 0.4540 0.051 Uiso 1 1 calc R . . H26B H 0.6252 0.9009 0.4124 0.051 Uiso 1 1 calc R . . C27 C 0.7604(6) 0.9280(6) 0.4524(2) 0.0477(18) Uani 1 1 d . . . H27A H 0.8042 0.8579 0.4419 0.057 Uiso 1 1 calc R . . H27B H 0.7754 0.9319 0.4829 0.057 Uiso 1 1 calc R . . C28 C 0.7973(7) 1.0511(7) 0.4332(3) 0.056(2) Uani 1 1 d . . . H28A H 0.7500 1.1202 0.4423 0.067 Uiso 1 1 calc R . . H28B H 0.7867 1.0449 0.4026 0.067 Uiso 1 1 calc R . . C29 C 0.9188(7) 1.0832(7) 0.4451(3) 0.066(2) Uani 1 1 d . . . H29A H 0.9347 1.1664 0.4332 0.079 Uiso 1 1 calc R . . H29B H 0.9277 1.0912 0.4756 0.079 Uiso 1 1 calc R . . C30 C 1.0058(10) 0.9913(10) 0.4315(4) 0.100(4) Uani 1 1 d . . . H30A H 1.0793 1.0204 0.4426 0.121 Uiso 1 1 calc R . . H30B H 0.9921 0.9084 0.4440 0.121 Uiso 1 1 calc R . . C31 C 1.0081(14) 0.9762(17) 0.3871(5) 0.169(7) Uani 1 1 d . . . H31A H 1.0527 0.9026 0.3811 0.253 Uiso 1 1 calc R . . H31B H 1.0405 1.0511 0.3752 0.253 Uiso 1 1 calc R . . H31C H 0.9326 0.9646 0.3750 0.253 Uiso 1 1 calc R . . C32 C 0.8607(8) 0.7182(9) 0.3014(3) 0.089(3) Uani 1 1 d . . . H32A H 0.8300 0.7579 0.2758 0.133 Uiso 1 1 calc R . . H32B H 0.8793 0.6307 0.2957 0.133 Uiso 1 1 calc R . . H32C H 0.9275 0.7631 0.3115 0.133 Uiso 1 1 calc R . . C33 C 0.8673(6) 0.0840(7) 0.2423(3) 0.072(2) Uani 0.67 1 d PD A 1 H33 H 0.8024 0.0586 0.2579 0.086 Uiso 0.67 1 calc PR A 1 Cl1 Cl 0.8406(4) 0.2344(4) 0.22462(15) 0.1011(7) Uiso 0.67 1 d PD A 1 Cl2 Cl 0.9802(4) 0.0781(4) 0.27684(15) 0.1011(7) Uiso 0.67 1 d PD A 1 Cl3 Cl 0.8751(4) -0.0226(4) 0.20224(16) 0.1011(7) Uiso 0.67 1 d PD A 1 C33' C 0.8673(6) 0.0840(7) 0.2423(3) 0.072(2) Uani 0.33 1 d P B 2 H33' H 0.8022 0.0589 0.2579 0.086 Uiso 0.33 1 calc PR B 2 Cl1' Cl 0.9811(7) -0.0168(8) 0.2530(3) 0.1011(7) Uiso 0.33 1 d PD B 2 Cl2' Cl 0.8393(7) 0.0714(9) 0.1880(3) 0.1011(7) Uiso 0.33 1 d PD B 2 Cl3' Cl 0.9090(7) 0.2400(8) 0.2537(3) 0.1011(7) Uiso 0.33 1 d PD B 2 C34 C 0.3584(6) 0.1000(8) 0.3252(3) 0.064(2) Uani 1 1 d . . . H34 H 0.4274 0.0669 0.3138 0.077 Uiso 1 1 calc R . . Cl4 Cl 0.3365(3) 0.2525(3) 0.30688(13) 0.1386(14) Uani 1 1 d . . . Cl5 Cl 0.3757(2) 0.0981(2) 0.37975(8) 0.0858(7) Uani 1 1 d . . . Cl6 Cl 0.2491(3) 0.0046(3) 0.30799(12) 0.1128(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0472(3) 0.0509(3) 0.0598(4) 0.0042(2) 0.0023(2) 0.0082(2) Li1 0.076(9) 0.048(7) 0.050(8) -0.010(6) 0.022(7) 0.007(6) O1 0.050(3) 0.044(3) 0.061(4) -0.003(2) 0.000(3) 0.005(2) O2 0.049(3) 0.055(3) 0.084(4) -0.019(3) -0.008(3) 0.014(2) O3 0.091(4) 0.048(3) 0.079(4) -0.016(3) -0.038(3) 0.020(3) O4 0.050(3) 0.072(3) 0.053(4) -0.014(3) -0.008(2) 0.012(3) O5 0.057(3) 0.049(3) 0.083(4) -0.005(3) 0.017(3) 0.003(2) O7 0.074(3) 0.037(3) 0.048(3) -0.012(2) 0.015(3) 0.005(2) O6 0.048(3) 0.046(3) 0.038(3) -0.003(2) 0.012(2) 0.002(2) O8 0.066(4) 0.056(3) 0.091(5) 0.020(3) 0.041(3) 0.019(3) N1 0.041(3) 0.036(3) 0.035(3) -0.004(2) 0.007(2) 0.007(2) C1 0.030(4) 0.041(4) 0.067(5) -0.004(3) -0.008(3) 0.006(3) C2 0.045(4) 0.037(4) 0.078(6) -0.004(4) 0.001(4) 0.006(3) C3 0.054(5) 0.040(4) 0.082(6) -0.014(4) 0.002(4) 0.008(3) C4 0.046(4) 0.051(5) 0.076(6) -0.009(4) 0.002(4) 0.012(4) C5 0.032(4) 0.044(4) 0.068(6) 0.000(4) -0.006(4) 0.009(3) C6 0.030(4) 0.042(4) 0.069(6) -0.004(4) -0.006(3) 0.006(3) C7 0.037(4) 0.052(5) 0.068(6) -0.005(4) -0.003(4) 0.008(3) C8 0.050(4) 0.048(4) 0.067(6) 0.004(4) -0.002(4) 0.003(3) C9 0.061(5) 0.042(4) 0.068(6) -0.006(4) -0.007(4) 0.000(4) C10 0.049(4) 0.049(4) 0.061(5) -0.010(4) -0.011(4) 0.004(3) C11 0.036(4) 0.044(4) 0.073(6) -0.002(4) -0.006(4) 0.005(3) C12 0.043(4) 0.060(5) 0.077(6) -0.006(4) -0.010(4) 0.006(4) C13 0.090(7) 0.057(5) 0.092(8) -0.012(5) -0.025(6) 0.030(5) C14 0.070(6) 0.051(5) 0.083(7) -0.016(4) -0.012(5) 0.012(4) C15 0.086(6) 0.059(5) 0.052(6) -0.018(4) -0.010(4) 0.005(4) C16 0.107(8) 0.094(8) 0.086(8) -0.030(6) -0.049(7) 0.022(6) C17 0.054(5) 0.074(5) 0.062(6) 0.006(4) -0.001(4) 0.008(4) C18 0.052(4) 0.049(4) 0.062(5) 0.008(4) -0.002(4) 0.009(3) C20 0.050(4) 0.047(4) 0.038(4) -0.015(3) 0.010(3) 0.002(3) C19 0.054(4) 0.047(4) 0.034(4) -0.009(3) 0.012(3) -0.002(3) C23 0.032(3) 0.044(4) 0.031(4) -0.005(3) 0.003(3) 0.006(3) C22 0.028(3) 0.038(3) 0.034(4) -0.001(3) 0.002(3) 0.010(2) C21 0.037(4) 0.041(4) 0.036(4) -0.006(3) 0.003(3) 0.006(3) C25 0.047(4) 0.037(4) 0.038(4) -0.003(3) 0.007(3) 0.004(3) C24 0.033(4) 0.042(4) 0.036(4) -0.003(3) -0.001(3) 0.006(3) C26 0.051(4) 0.037(4) 0.040(4) 0.003(3) 0.004(3) 0.006(3) C27 0.062(5) 0.037(4) 0.044(5) 0.004(3) 0.002(4) 0.001(3) C28 0.076(6) 0.040(4) 0.052(5) 0.006(4) 0.009(4) -0.002(4) C29 0.071(6) 0.050(5) 0.076(6) 0.015(4) 0.008(5) -0.008(4) C30 0.086(8) 0.097(8) 0.121(11) 0.000(7) 0.026(7) -0.019(6) C31 0.153(15) 0.25(2) 0.108(14) -0.023(12) 0.022(11) 0.033(13) C32 0.088(7) 0.082(6) 0.102(9) 0.022(6) 0.046(6) 0.017(5) C33 0.054(5) 0.082(6) 0.079(7) 0.011(5) 0.003(4) -0.009(4) C33' 0.054(5) 0.082(6) 0.079(7) 0.011(5) 0.003(4) -0.009(4) C34 0.047(5) 0.070(5) 0.076(6) -0.003(4) 0.001(4) 0.013(4) Cl4 0.167(3) 0.090(2) 0.154(4) 0.030(2) -0.021(3) 0.014(2) Cl5 0.0943(18) 0.0887(16) 0.0753(17) -0.0175(13) 0.0130(13) 0.0185(13) Cl6 0.0837(19) 0.128(3) 0.122(3) -0.0013(19) -0.0244(18) -0.0202(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O8 1.863(14) . ? Li1 O6 1.951(12) . ? Li1 O3 1.987(13) . ? Li1 O4 2.282(15) . ? Li1 O2 2.290(15) . ? O1 C1 1.365(9) . ? O1 C11 1.435(9) . ? O2 C13 1.376(9) . ? O2 C12 1.420(9) . ? O3 C14 1.375(9) . ? O3 C15 1.428(9) . ? O4 C16 1.384(11) . ? O4 C17 1.444(9) . ? O5 C7 1.362(9) 3_666 ? O5 C18 1.429(9) . ? O7 C25 1.224(7) . ? O6 C24 1.229(8) . ? O8 C32 1.395(10) . ? O8 H8 0.850 . ? N1 C24 1.380(8) . ? N1 C25 1.406(8) . ? N1 C26 1.489(8) . ? C1 C2 1.370(10) . ? C1 C6 1.435(10) . ? C2 C3 1.407(11) . ? C2 H2A 0.950 . ? C3 C4 1.357(11) . ? C3 H3A 0.950 . ? C4 C5 1.412(11) . ? C4 H4A 0.950 . ? C5 C6 1.408(11) . ? C5 C7 1.440(11) . ? C6 C10 1.425(10) . ? C7 O5 1.362(9) 3_666 ? C7 C8 1.390(10) . ? C8 C9 1.403(11) . ? C8 H8A 0.950 . ? C9 C10 1.359(11) . ? C9 H9A 0.950 . ? C10 H10A 0.950 . ? C11 C12 1.486(11) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.429(12) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.438(12) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 C18 1.477(11) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C20 C21 1.379(9) . ? C20 C19 1.392(10) . ? C20 H19 0.950 . ? C19 C23 1.381(9) 3_666 ? C19 H20 0.950 . ? C23 C19 1.381(9) 3_666 ? C23 C22 1.405(9) . ? C23 C24 1.478(9) . ? C22 C22 1.419(13) 3_666 ? C22 C21 1.419(9) . ? C21 C25 1.468(9) . ? C26 C27 1.496(9) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.533(10) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 C29 1.538(11) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C29 C30 1.524(13) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 C31 1.447(19) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.980 . ? C31 H31B 0.980 . ? C31 H31C 0.980 . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C33 Cl2 1.713(8) . ? C33 Cl1 1.726(8) . ? C33 Cl3 1.731(9) . ? C33 H33 1.000 . ? C34 Cl6 1.734(9) . ? C34 Cl4 1.745(9) . ? C34 Cl5 1.764(9) . ? C34 H34 1.000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Li1 O6 99.9(6) . . ? O8 Li1 O3 117.0(7) . . ? O6 Li1 O3 143.0(7) . . ? O8 Li1 O4 106.0(7) . . ? O6 Li1 O4 95.6(5) . . ? O3 Li1 O4 76.4(5) . . ? O8 Li1 O2 100.4(6) . . ? O6 Li1 O2 98.7(6) . . ? O3 Li1 O2 74.4(4) . . ? O4 Li1 O2 147.2(6) . . ? C1 O1 C11 117.7(5) . . ? C13 O2 C12 115.9(6) . . ? C13 O2 Li1 108.8(6) . . ? C12 O2 Li1 128.3(5) . . ? C14 O3 C15 116.6(6) . . ? C14 O3 Li1 121.6(6) . . ? C15 O3 Li1 118.5(6) . . ? C16 O4 C17 114.0(6) . . ? C16 O4 Li1 103.5(6) . . ? C17 O4 Li1 130.3(6) . . ? C7 O5 C18 117.8(6) 3_666 . ? C24 O6 Li1 149.1(6) . . ? C32 O8 Li1 128.9(6) . . ? C32 O8 H8 111.0 . . ? Li1 O8 H8 114.9 . . ? C24 N1 C25 124.2(5) . . ? C24 N1 C26 118.4(5) . . ? C25 N1 C26 117.3(5) . . ? O1 C1 C2 124.6(7) . . ? O1 C1 C6 115.0(6) . . ? C2 C1 C6 120.4(7) . . ? C1 C2 C3 119.3(7) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 122.5(7) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 118.9(8) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 120.6(7) . . ? C6 C5 C7 118.0(7) . . ? C4 C5 C7 121.4(7) . . ? C5 C6 C10 121.0(7) . . ? C5 C6 C1 118.3(6) . . ? C10 C6 C1 120.7(7) . . ? O5 C7 C8 125.0(7) 3_666 . ? O5 C7 C5 114.9(6) 3_666 . ? C8 C7 C5 120.0(7) . . ? C7 C8 C9 119.7(7) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C10 C9 C8 122.4(7) . . ? C10 C9 H9A 118.8 . . ? C8 C9 H9A 118.8 . . ? C9 C10 C6 118.8(8) . . ? C9 C10 H10A 120.6 . . ? C6 C10 H10A 120.6 . . ? O1 C11 C12 108.9(6) . . ? O1 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O1 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O2 C12 C11 109.9(6) . . ? O2 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? O2 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? O2 C13 C14 113.2(7) . . ? O2 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? O2 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? O3 C14 C13 111.0(7) . . ? O3 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? O3 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? O3 C15 C16 108.9(7) . . ? O3 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? O3 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O4 C16 C15 112.1(8) . . ? O4 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? O4 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? O4 C17 C18 110.5(7) . . ? O4 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O5 C18 C17 108.6(6) . . ? O5 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? O5 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? C21 C20 C19 120.9(6) . . ? C21 C20 H19 119.6 . . ? C19 C20 H19 119.6 . . ? C23 C19 C20 120.7(6) 3_666 . ? C23 C19 H20 119.6 3_666 . ? C20 C19 H20 119.6 . . ? C19 C23 C22 120.0(6) 3_666 . ? C19 C23 C24 120.5(6) 3_666 . ? C22 C23 C24 119.5(6) . . ? C23 C22 C22 119.5(7) . 3_666 ? C23 C22 C21 121.2(6) . . ? C22 C22 C21 119.4(7) 3_666 . ? C20 C21 C22 119.6(6) . . ? C20 C21 C25 121.1(6) . . ? C22 C21 C25 119.4(6) . . ? O7 C25 N1 120.2(6) . . ? O7 C25 C21 122.4(6) . . ? N1 C25 C21 117.4(5) . . ? O6 C24 N1 119.9(6) . . ? O6 C24 C23 122.3(6) . . ? N1 C24 C23 117.8(6) . . ? N1 C26 C27 113.2(5) . . ? N1 C26 H26A 108.9 . . ? C27 C26 H26A 108.9 . . ? N1 C26 H26B 108.9 . . ? C27 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? C26 C27 C28 112.3(6) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C29 112.9(6) . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C28 117.1(8) . . ? C30 C29 H29A 108.0 . . ? C28 C29 H29A 108.0 . . ? C30 C29 H29B 108.0 . . ? C28 C29 H29B 108.0 . . ? H29A C29 H29B 107.3 . . ? C31 C30 C29 114.5(12) . . ? C31 C30 H30A 108.6 . . ? C29 C30 H30A 108.6 . . ? C31 C30 H30B 108.6 . . ? C29 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O8 C32 H32A 109.5 . . ? O8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl2 C33 Cl1 112.1(5) . . ? Cl2 C33 Cl3 112.5(5) . . ? Cl1 C33 Cl3 112.4(5) . . ? Cl2 C33 H33 106.4 . . ? Cl1 C33 H33 106.4 . . ? Cl3 C33 H33 106.4 . . ? Cl6 C34 Cl4 109.9(5) . . ? Cl6 C34 Cl5 110.7(5) . . ? Cl4 C34 Cl5 110.8(5) . . ? Cl6 C34 H34 108.5 . . ? Cl4 C34 H34 108.5 . . ? Cl5 C34 H34 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Li1 O2 C13 -102.0(7) . . . . ? O6 Li1 O2 C13 156.1(7) . . . . ? O3 Li1 O2 C13 13.3(7) . . . . ? O4 Li1 O2 C13 41.2(14) . . . . ? O8 Li1 O2 C12 46.9(9) . . . . ? O6 Li1 O2 C12 -55.0(9) . . . . ? O3 Li1 O2 C12 162.2(7) . . . . ? O4 Li1 O2 C12 -169.9(10) . . . . ? O8 Li1 O3 C14 101.1(10) . . . . ? O6 Li1 O3 C14 -76.4(15) . . . . ? O4 Li1 O3 C14 -157.6(7) . . . . ? O2 Li1 O3 C14 7.3(8) . . . . ? O8 Li1 O3 C15 -100.1(10) . . . . ? O6 Li1 O3 C15 82.4(15) . . . . ? O4 Li1 O3 C15 1.2(8) . . . . ? O2 Li1 O3 C15 166.1(7) . . . . ? O8 Li1 O4 C16 89.0(8) . . . . ? O6 Li1 O4 C16 -169.0(7) . . . . ? O3 Li1 O4 C16 -25.6(7) . . . . ? O2 Li1 O4 C16 -53.3(13) . . . . ? O8 Li1 O4 C17 -49.8(9) . . . . ? O6 Li1 O4 C17 52.3(9) . . . . ? O3 Li1 O4 C17 -164.4(7) . . . . ? O2 Li1 O4 C17 168.0(10) . . . . ? O8 Li1 O6 C24 -177.7(9) . . . . ? O3 Li1 O6 C24 0(2) . . . . ? O4 Li1 O6 C24 74.9(12) . . . . ? O2 Li1 O6 C24 -75.5(13) . . . . ? O6 Li1 O8 C32 161.7(8) . . . . ? O3 Li1 O8 C32 -16.8(14) . . . . ? O4 Li1 O8 C32 -99.5(9) . . . . ? O2 Li1 O8 C32 60.8(11) . . . . ? C11 O1 C1 C2 -6.5(10) . . . . ? C11 O1 C1 C6 174.1(6) . . . . ? O1 C1 C2 C3 -177.8(7) . . . . ? C6 C1 C2 C3 1.6(11) . . . . ? C1 C2 C3 C4 -1.9(12) . . . . ? C2 C3 C4 C5 1.0(12) . . . . ? C3 C4 C5 C6 0.2(10) . . . . ? C3 C4 C5 C7 -179.5(7) . . . . ? C4 C5 C6 C10 178.8(6) . . . . ? C7 C5 C6 C10 -1.4(10) . . . . ? C4 C5 C6 C1 -0.4(10) . . . . ? C7 C5 C6 C1 179.3(6) . . . . ? O1 C1 C6 C5 179.0(6) . . . . ? C2 C1 C6 C5 -0.5(10) . . . . ? O1 C1 C6 C10 -0.3(9) . . . . ? C2 C1 C6 C10 -179.7(7) . . . . ? C6 C5 C7 O5 -178.3(6) . . . 3_666 ? C4 C5 C7 O5 1.4(10) . . . 3_666 ? C6 C5 C7 C8 1.5(10) . . . . ? C4 C5 C7 C8 -178.8(7) . . . . ? O5 C7 C8 C9 179.5(7) 3_666 . . . ? C5 C7 C8 C9 -0.4(11) . . . . ? C7 C8 C9 C10 -1.0(12) . . . . ? C8 C9 C10 C6 1.1(11) . . . . ? C5 C6 C10 C9 0.2(10) . . . . ? C1 C6 C10 C9 179.4(7) . . . . ? C1 O1 C11 C12 -177.1(6) . . . . ? C13 O2 C12 C11 -146.6(8) . . . . ? Li1 O2 C12 C11 66.3(10) . . . . ? O1 C11 C12 O2 62.8(8) . . . . ? C12 O2 C13 C14 175.9(8) . . . . ? Li1 O2 C13 C14 -30.8(10) . . . . ? C15 O3 C14 C13 174.6(8) . . . . ? Li1 O3 C14 C13 -26.2(12) . . . . ? O2 C13 C14 O3 37.5(12) . . . . ? C14 O3 C15 C16 -177.0(9) . . . . ? Li1 O3 C15 C16 23.1(11) . . . . ? C17 O4 C16 C15 -166.6(8) . . . . ? Li1 O4 C16 C15 46.8(11) . . . . ? O3 C15 C16 O4 -48.5(13) . . . . ? C16 O4 C17 C18 160.3(8) . . . . ? Li1 O4 C17 C18 -64.3(10) . . . . ? C7 O5 C18 C17 -179.4(6) 3_666 . . . ? O4 C17 C18 O5 -63.8(8) . . . . ? C21 C20 C19 C23 -0.2(11) . . . 3_666 ? C19 C23 C22 C22 0.4(10) 3_666 . . 3_666 ? C24 C23 C22 C22 178.8(6) . . . 3_666 ? C19 C23 C22 C21 179.6(6) 3_666 . . . ? C24 C23 C22 C21 -2.0(9) . . . . ? C19 C20 C21 C22 0.6(10) . . . . ? C19 C20 C21 C25 179.7(6) . . . . ? C23 C22 C21 C20 180.0(6) . . . . ? C22 C22 C21 C20 -0.9(11) 3_666 . . . ? C23 C22 C21 C25 0.8(9) . . . . ? C22 C22 C21 C25 180.0(7) 3_666 . . . ? C24 N1 C25 O7 171.3(6) . . . . ? C26 N1 C25 O7 -4.8(9) . . . . ? C24 N1 C25 C21 -9.3(9) . . . . ? C26 N1 C25 C21 174.6(6) . . . . ? C20 C21 C25 O7 4.8(11) . . . . ? C22 C21 C25 O7 -176.1(6) . . . . ? C20 C21 C25 N1 -174.6(6) . . . . ? C22 C21 C25 N1 4.5(9) . . . . ? Li1 O6 C24 N1 -179.7(10) . . . . ? Li1 O6 C24 C23 0.4(15) . . . . ? C25 N1 C24 O6 -171.7(6) . . . . ? C26 N1 C24 O6 4.3(9) . . . . ? C25 N1 C24 C23 8.2(9) . . . . ? C26 N1 C24 C23 -175.8(5) . . . . ? C19 C23 C24 O6 -4.0(10) 3_666 . . . ? C22 C23 C24 O6 177.6(6) . . . . ? C19 C23 C24 N1 176.1(6) 3_666 . . . ? C22 C23 C24 N1 -2.2(9) . . . . ? C24 N1 C26 C27 -85.5(7) . . . . ? C25 N1 C26 C27 90.8(7) . . . . ? N1 C26 C27 C28 178.6(6) . . . . ? C26 C27 C28 C29 176.3(7) . . . . ? C27 C28 C29 C30 62.0(11) . . . . ? C28 C29 C30 C31 61.9(13) . . . . ? #============================================================================== data_[Na2.1.A]I2 _database_code_depnum_ccdc_archive 'CCDC 644503' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H78 I2 N2 Na2 O16, 2(C H Cl3)' _chemical_formula_sum 'C64 H80 Cl6 I2 N2 Na2 O16' _chemical_formula_weight 1645.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7604(5) _cell_length_b 23.6245(6) _cell_length_c 15.4728(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.281(1) _cell_angle_gamma 90.00 _cell_volume 3755.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 20952 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; n-Hexyl chain modelled as disordered over two equally-occupied orientations. All 1,2- distances are restrained to a common refined value and all 1,3- distances are restrained to be 1.633 times that value. The displacement parameters are isotropic, and a single refined value was given to all C atoms at equivalent positions along the chain - i.e. the two C atoms bound directly to N have a common displacement parameter, the two C atoms bound to that have a common displacement parameter, and so on. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'thin-slice /w and /f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 21958 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.01 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 6586 _reflns_number_gt 4404 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_data_reduction Denzo/Scalepack _computing_structure_solution 'SHELXTL v6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+12.7893P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6586 _refine_ls_number_parameters 403 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1809 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.991 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.088 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.79280(6) 0.55325(2) 1.06709(3) 0.0697(2) Uani 1 1 d . . . Na1 Na 0.8156(2) 0.58589(9) 0.86283(16) 0.0499(6) Uani 1 1 d . . . O1 O 0.9156(4) 0.53013(18) 0.6087(3) 0.0511(11) Uani 1 1 d . . . O2 O 0.9523(4) 0.60960(17) 0.7532(3) 0.0478(10) Uani 1 1 d . . . O3 O 0.8276(4) 0.68326(17) 0.8415(3) 0.0514(11) Uani 1 1 d . . . O4 O 0.5946(4) 0.63757(17) 0.8503(3) 0.0476(10) Uani 1 1 d . . . O5 O 0.3790(4) 0.57224(18) 0.7458(3) 0.0519(11) Uani 1 1 d . . . O6 O 0.7196(4) 0.51189(17) 0.7737(3) 0.0508(10) Uani 1 1 d . . . O7 O 0.6078(5) 0.34406(18) 0.6281(3) 0.0688(14) Uani 1 1 d . . . O8 O 1.0278(5) 0.5685(2) 0.9568(4) 0.0775(15) Uani 1 1 d . . . H81 H 1.0139 0.5628 1.0074 0.116 Uiso 1 1 d R . . H82 H 1.0819 0.5430 0.9535 0.116 Uiso 1 1 d R . . N1 N 0.6683(5) 0.4283(2) 0.7003(4) 0.0493(13) Uani 1 1 d D B . C1 C 0.8712(5) 0.4852(3) 0.5528(4) 0.0442(14) Uani 1 1 d . . . C2 C 0.8917(6) 0.4293(3) 0.5773(5) 0.0490(15) Uani 1 1 d . . . H2A H 0.9411 0.4193 0.6371 0.059 Uiso 1 1 calc R . . C3 C 0.8385(6) 0.3867(3) 0.5128(5) 0.0530(16) Uani 1 1 d . . . H3A H 0.8536 0.3481 0.5299 0.064 Uiso 1 1 calc R . . C4 C 0.7661(6) 0.3994(3) 0.4263(4) 0.0474(15) Uani 1 1 d . . . H4A H 0.7308 0.3700 0.3843 0.057 Uiso 1 1 calc R . . C5 C 0.7441(5) 0.4568(2) 0.4000(4) 0.0429(14) Uani 1 1 d . . . C6 C 0.7981(5) 0.5005(2) 0.4628(4) 0.0413(13) Uani 1 1 d . . . C7 C 0.6706(5) 0.4727(3) 0.3106(4) 0.0436(14) Uani 1 1 d . . . C8 C 0.6542(6) 0.5281(3) 0.2846(4) 0.0479(15) Uani 1 1 d . . . H8B H 0.6063 0.5378 0.2243 0.057 Uiso 1 1 calc R . . C9 C 0.7093(6) 0.5711(3) 0.3485(5) 0.0497(16) Uani 1 1 d . . . H9A H 0.6977 0.6097 0.3306 0.060 Uiso 1 1 calc R . . C10 C 0.7786(6) 0.5578(3) 0.4352(5) 0.0476(15) Uani 1 1 d . . . H10A H 0.8140 0.5872 0.4773 0.057 Uiso 1 1 calc R . . C11 C 0.9954(6) 0.5184(3) 0.6996(4) 0.0506(15) Uani 1 1 d . . . H11A H 1.0654 0.4914 0.6986 0.061 Uiso 1 1 calc R . . H11B H 0.9421 0.5014 0.7352 0.061 Uiso 1 1 calc R . . C12 C 1.0527(6) 0.5731(3) 0.7410(5) 0.0530(16) Uani 1 1 d . . . H12A H 1.1179 0.5658 0.8002 0.064 Uiso 1 1 calc R . . H12B H 1.0973 0.5919 0.7012 0.064 Uiso 1 1 calc R . . C13 C 1.0071(7) 0.6634(3) 0.7879(5) 0.0630(19) Uani 1 1 d . . . H13A H 1.0620 0.6779 0.7516 0.076 Uiso 1 1 calc R . . H13B H 1.0622 0.6593 0.8514 0.076 Uiso 1 1 calc R . . C14 C 0.8975(7) 0.7037(3) 0.7829(5) 0.0633(19) Uani 1 1 d . . . H14A H 0.9321 0.7420 0.8019 0.076 Uiso 1 1 calc R . . H14B H 0.8391 0.7059 0.7200 0.076 Uiso 1 1 calc R . . C15 C 0.7182(7) 0.7185(3) 0.8390(5) 0.0625(19) Uani 1 1 d . . . H15A H 0.6643 0.7240 0.7755 0.075 Uiso 1 1 calc R . . H15B H 0.7487 0.7560 0.8653 0.075 Uiso 1 1 calc R . . C16 C 0.6400(7) 0.6911(3) 0.8913(5) 0.0582(17) Uani 1 1 d . . . H16A H 0.6938 0.6855 0.9548 0.070 Uiso 1 1 calc R . . H16B H 0.5651 0.7155 0.8912 0.070 Uiso 1 1 calc R . . C17 C 0.4943(6) 0.6155(3) 0.8834(5) 0.0572(17) Uani 1 1 d . . . H17A H 0.4206 0.6424 0.8706 0.069 Uiso 1 1 calc R . . H17B H 0.5277 0.6100 0.9497 0.069 Uiso 1 1 calc R . . C18 C 0.4493(6) 0.5600(3) 0.8378(4) 0.0526(16) Uani 1 1 d . . . H18A H 0.5249 0.5354 0.8405 0.063 Uiso 1 1 calc R . . H18B H 0.3925 0.5403 0.8680 0.063 Uiso 1 1 calc R . . C19 C 0.4094(6) 0.4248(2) 0.3827(4) 0.0458(15) Uani 1 1 d . . . H19A H 0.3678 0.4038 0.3296 0.055 Uiso 1 1 calc R . . C20 C 0.4753(6) 0.3965(2) 0.4631(4) 0.0473(15) Uani 1 1 d . . . H20A H 0.4787 0.3563 0.4635 0.057 Uiso 1 1 calc R . . C21 C 0.5344(5) 0.4256(2) 0.5404(4) 0.0406(13) Uani 1 1 d . . . C22 C 0.5326(5) 0.4858(2) 0.5400(4) 0.0390(13) Uani 1 1 d . . . C23 C 0.5949(5) 0.5167(2) 0.6190(4) 0.0386(13) Uani 1 1 d . . . C24 C 0.6647(6) 0.4869(2) 0.7032(5) 0.0446(14) Uani 1 1 d . . . C25 C 0.6045(6) 0.3955(2) 0.6240(5) 0.0498(15) Uani 1 1 d . . . C26 C 0.7430(7) 0.3973(3) 0.7821(5) 0.079(2) Uani 1 1 d D . . H26A H 0.8010 0.3701 0.7646 0.094 Uiso 1 1 calc R A 1 H26B H 0.7989 0.4248 0.8246 0.094 Uiso 1 1 calc R A 1 C27 C 0.6651(13) 0.3663(7) 0.8302(9) 0.084(4) Uiso 0.50 1 d PD B 1 H27A H 0.5930 0.3454 0.7873 0.101 Uiso 0.50 1 calc PR B 1 H27B H 0.6286 0.3924 0.8666 0.101 Uiso 0.50 1 calc PR B 1 C28 C 0.7627(15) 0.3257(7) 0.8908(11) 0.089(4) Uiso 0.50 1 d PD B 1 H28A H 0.7836 0.2954 0.8533 0.107 Uiso 0.50 1 calc PR B 1 H28B H 0.8441 0.3464 0.9207 0.107 Uiso 0.50 1 calc PR B 1 C29 C 0.712(2) 0.3002(9) 0.9602(15) 0.125(6) Uiso 0.50 1 d PD B 1 H29A H 0.6228 0.2860 0.9318 0.150 Uiso 0.50 1 calc PR B 1 H29B H 0.7086 0.3291 1.0057 0.150 Uiso 0.50 1 calc PR B 1 C30 C 0.7995(18) 0.2515(8) 1.0065(13) 0.100(4) Uiso 0.50 1 d PD B 1 H30A H 0.8060 0.2231 0.9611 0.120 Uiso 0.50 1 calc PR B 1 H30B H 0.8881 0.2658 1.0376 0.120 Uiso 0.50 1 calc PR B 1 C31 C 0.741(3) 0.2249(13) 1.074(2) 0.182(9) Uiso 0.50 1 d PD B 1 H31A H 0.7707 0.1855 1.0849 0.273 Uiso 0.50 1 calc PR B 1 H31B H 0.6463 0.2259 1.0507 0.273 Uiso 0.50 1 calc PR B 1 H31C H 0.7696 0.2460 1.1314 0.273 Uiso 0.50 1 calc PR B 1 C27' C 0.6625(16) 0.3886(7) 0.8477(10) 0.084(4) Uiso 0.50 1 d PD B 2 H27C H 0.6427 0.4265 0.8677 0.101 Uiso 0.50 1 calc PR B 2 H27D H 0.5786 0.3714 0.8131 0.101 Uiso 0.50 1 calc PR B 2 C28' C 0.7170(17) 0.3537(6) 0.9301(9) 0.089(4) Uiso 0.50 1 d PD B 2 H28C H 0.7081 0.3752 0.9828 0.107 Uiso 0.50 1 calc PR B 2 H28D H 0.8112 0.3485 0.9387 0.107 Uiso 0.50 1 calc PR B 2 C29' C 0.658(2) 0.2968(7) 0.9307(13) 0.125(6) Uiso 0.50 1 d PD B 2 H29C H 0.6754 0.2734 0.8826 0.150 Uiso 0.50 1 calc PR B 2 H29D H 0.5621 0.3013 0.9158 0.150 Uiso 0.50 1 calc PR B 2 C30' C 0.707(2) 0.2654(7) 1.0203(11) 0.100(4) Uiso 0.50 1 d PD B 2 H30C H 0.7855 0.2841 1.0598 0.120 Uiso 0.50 1 calc PR B 2 H30D H 0.6392 0.2651 1.0520 0.120 Uiso 0.50 1 calc PR B 2 C31' C 0.738(3) 0.2060(9) 1.000(2) 0.182(9) Uiso 0.50 1 d PD B 2 H31D H 0.7156 0.2010 0.9338 0.273 Uiso 0.50 1 calc PR B 2 H31E H 0.6880 0.1793 1.0243 0.273 Uiso 0.50 1 calc PR B 2 H31F H 0.8313 0.1989 1.0268 0.273 Uiso 0.50 1 calc PR B 2 C32 C 0.3297(9) 0.8032(6) 0.6641(9) 0.072(9) Uiso 0.50 1 d PD C 1 H32 H 0.3232 0.8367 0.6235 0.087 Uiso 0.50 1 calc PR C 1 Cl1 Cl 0.3918(6) 0.7467(2) 0.6144(4) 0.0972(15) Uiso 0.50 1 d PD C 1 Cl2 Cl 0.1717(7) 0.7889(3) 0.6686(5) 0.128(2) Uiso 0.50 1 d PD C 1 Cl3 Cl 0.4547(5) 0.8182(2) 0.7650(4) 0.0834(15) Uiso 0.50 1 d PD C 1 C32' C 0.3484(11) 0.7996(7) 0.6628(8) 0.073(8) Uiso 0.50 1 d PD D 2 H32' H 0.3226 0.8376 0.6345 0.088 Uiso 0.50 1 calc PR D 2 Cl1' Cl 0.4352(7) 0.7645(3) 0.5969(4) 0.117(2) Uiso 0.50 1 d PD D 2 Cl2' Cl 0.2027(7) 0.7611(3) 0.6512(5) 0.133(2) Uiso 0.50 1 d PD D 2 Cl3' Cl 0.4176(6) 0.8109(2) 0.7821(4) 0.0909(17) Uiso 0.50 1 d PD D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0925(4) 0.0585(3) 0.0648(3) 0.0133(2) 0.0337(3) 0.0125(3) Na1 0.0523(15) 0.0391(12) 0.0569(15) -0.0005(10) 0.0140(12) -0.0020(10) O1 0.045(3) 0.056(3) 0.047(3) -0.004(2) 0.006(2) 0.004(2) O2 0.041(2) 0.050(2) 0.057(3) -0.0057(19) 0.022(2) -0.0050(19) O3 0.055(3) 0.040(2) 0.061(3) 0.0053(19) 0.020(2) 0.0007(19) O4 0.047(2) 0.047(2) 0.051(3) -0.0083(19) 0.017(2) -0.0038(19) O5 0.047(3) 0.053(3) 0.052(3) -0.001(2) 0.010(2) -0.003(2) O6 0.048(3) 0.049(2) 0.053(3) -0.003(2) 0.011(2) -0.001(2) O7 0.082(3) 0.032(2) 0.081(3) 0.004(2) 0.007(3) 0.008(2) O8 0.083(4) 0.077(3) 0.078(4) 0.014(3) 0.032(3) 0.009(3) N1 0.047(3) 0.034(3) 0.062(3) 0.007(2) 0.009(3) 0.005(2) C1 0.031(3) 0.052(4) 0.053(4) 0.002(3) 0.017(3) 0.006(3) C2 0.036(3) 0.058(4) 0.053(4) 0.008(3) 0.013(3) 0.007(3) C3 0.048(4) 0.048(4) 0.065(5) 0.007(3) 0.019(3) 0.007(3) C4 0.041(3) 0.050(4) 0.055(4) 0.003(3) 0.020(3) 0.002(3) C5 0.033(3) 0.048(4) 0.053(4) 0.000(3) 0.021(3) 0.001(3) C6 0.032(3) 0.050(3) 0.045(4) 0.004(3) 0.016(3) 0.005(3) C7 0.031(3) 0.053(4) 0.050(4) 0.002(3) 0.018(3) 0.000(3) C8 0.036(3) 0.060(4) 0.050(4) 0.008(3) 0.016(3) 0.002(3) C9 0.040(4) 0.043(3) 0.066(4) 0.009(3) 0.017(3) 0.001(3) C10 0.038(3) 0.047(3) 0.059(4) -0.002(3) 0.015(3) 0.003(3) C11 0.041(4) 0.058(4) 0.055(4) 0.000(3) 0.016(3) 0.008(3) C12 0.039(4) 0.070(4) 0.052(4) 0.000(3) 0.015(3) 0.003(3) C13 0.059(4) 0.059(4) 0.077(5) -0.001(4) 0.030(4) -0.015(3) C14 0.075(5) 0.048(4) 0.072(5) 0.009(3) 0.029(4) -0.005(4) C15 0.064(5) 0.038(3) 0.086(5) 0.003(3) 0.023(4) 0.004(3) C16 0.062(4) 0.045(4) 0.069(5) -0.012(3) 0.022(4) 0.003(3) C17 0.050(4) 0.069(4) 0.052(4) -0.003(3) 0.015(3) 0.000(3) C18 0.041(4) 0.068(4) 0.049(4) 0.005(3) 0.014(3) -0.006(3) C19 0.041(3) 0.034(3) 0.061(4) -0.007(3) 0.012(3) -0.002(3) C20 0.046(4) 0.029(3) 0.065(4) -0.001(3) 0.015(3) 0.000(3) C21 0.031(3) 0.032(3) 0.061(4) -0.001(3) 0.016(3) 0.001(2) C22 0.031(3) 0.033(3) 0.060(4) -0.004(2) 0.023(3) 0.000(2) C23 0.027(3) 0.037(3) 0.055(4) 0.000(3) 0.018(3) 0.000(2) C24 0.037(3) 0.040(3) 0.062(4) -0.005(3) 0.024(3) -0.001(3) C25 0.046(4) 0.037(4) 0.064(4) 0.002(3) 0.012(3) 0.002(3) C26 0.071(5) 0.057(4) 0.084(6) 0.001(4) -0.013(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Na1 3.332(2) . ? Na1 O6 2.276(5) . ? Na1 O3 2.333(5) . ? Na1 O8 2.350(6) . ? Na1 O2 2.615(5) . ? Na1 O4 2.629(5) . ? O1 C1 1.364(7) . ? O1 C11 1.440(7) . ? O2 C13 1.435(8) . ? O2 C12 1.437(7) . ? O3 C14 1.424(8) . ? O3 C15 1.432(8) . ? O4 C17 1.424(8) . ? O4 C16 1.435(7) . ? O5 C7 1.377(7) 3_666 ? O5 C18 1.429(8) . ? O6 C24 1.227(7) . ? O7 C25 1.216(7) . ? O8 H81 0.850 . ? O8 H82 0.850 . ? N1 C24 1.386(7) . ? N1 C25 1.409(8) . ? N1 C26 1.475(8) . ? C1 C2 1.373(9) . ? C1 C6 1.428(8) . ? C2 C3 1.413(9) . ? C2 H2A 0.950 . ? C3 C4 1.367(9) . ? C3 H3A 0.950 . ? C4 C5 1.414(8) . ? C4 H4A 0.950 . ? C5 C6 1.420(8) . ? C5 C7 1.426(9) . ? C6 C10 1.416(8) . ? C7 C8 1.365(8) . ? C7 O5 1.377(7) 3_666 ? C8 C9 1.418(9) . ? C8 H8B 0.950 . ? C9 C10 1.364(9) . ? C9 H9A 0.950 . ? C10 H10A 0.950 . ? C11 C12 1.492(9) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.501(10) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.477(10) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 C18 1.498(9) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C23 1.383(8) 3_666 ? C19 C20 1.404(9) . ? C19 H19A 0.950 . ? C20 C21 1.364(8) . ? C20 H20A 0.950 . ? C21 C22 1.421(8) . ? C21 C25 1.473(9) . ? C22 C22 1.399(12) 3_666 ? C22 C23 1.411(8) . ? C23 C19 1.383(8) 3_666 ? C23 C24 1.476(9) . ? C26 C27 1.471(10) . ? C26 C27' 1.531(10) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.522(10) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 C29 1.469(11) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C29 C30 1.523(11) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 C31 1.508(11) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.980 . ? C31 H31B 0.980 . ? C31 H31C 0.980 . ? C27' C28' 1.485(18) . ? C27' H27C 0.990 . ? C27' H27D 0.990 . ? C28' C29' 1.488(11) . ? C28' H28C 0.990 . ? C28' H28D 0.990 . ? C29' C30' 1.523(11) . ? C29' H29C 0.990 . ? C29' H29D 0.990 . ? C30' C31' 1.500(11) . ? C30' H30C 0.990 . ? C30' H30D 0.990 . ? C31' H31D 0.980 . ? C31' H31E 0.980 . ? C31' H31F 0.980 . ? C32 Cl2 1.754(9) . ? C32 Cl1 1.767(10) . ? C32 Cl3 1.768(9) . ? C32 H32 1.000 . ? C32' Cl2' 1.776(10) . ? C32' Cl1' 1.779(10) . ? C32' Cl3' 1.794(9) . ? C32' H32' 1.000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Na1 O3 134.91(19) . . ? O6 Na1 O8 115.04(19) . . ? O3 Na1 O8 100.10(19) . . ? O6 Na1 O2 90.73(16) . . ? O3 Na1 O2 68.39(15) . . ? O8 Na1 O2 78.94(17) . . ? O6 Na1 O4 94.27(16) . . ? O3 Na1 O4 67.56(15) . . ? O8 Na1 O4 144.91(19) . . ? O2 Na1 O4 121.58(15) . . ? O6 Na1 I1 104.43(13) . . ? O3 Na1 I1 112.64(14) . . ? O8 Na1 I1 72.81(14) . . ? O2 Na1 I1 151.50(13) . . ? O4 Na1 I1 81.82(11) . . ? C1 O1 C11 117.7(5) . . ? C13 O2 C12 109.8(5) . . ? C13 O2 Na1 101.2(4) . . ? C12 O2 Na1 123.1(4) . . ? C14 O3 C15 111.8(5) . . ? C14 O3 Na1 119.1(4) . . ? C15 O3 Na1 119.8(4) . . ? C17 O4 C16 111.1(5) . . ? C17 O4 Na1 124.7(4) . . ? C16 O4 Na1 101.2(4) . . ? C7 O5 C18 117.8(5) 3_666 . ? C24 O6 Na1 157.1(4) . . ? Na1 O8 H81 101.1 . . ? Na1 O8 H82 130.1 . . ? H81 O8 H82 104.7 . . ? C24 N1 C25 124.4(5) . . ? C24 N1 C26 118.7(6) . . ? C25 N1 C26 116.9(5) . . ? O1 C1 C2 125.2(6) . . ? O1 C1 C6 114.1(5) . . ? C2 C1 C6 120.7(6) . . ? C1 C2 C3 119.4(6) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 121.9(6) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 119.3(6) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 120.1(6) . . ? C4 C5 C7 121.9(6) . . ? C6 C5 C7 117.9(5) . . ? C10 C6 C5 119.7(5) . . ? C10 C6 C1 121.8(6) . . ? C5 C6 C1 118.5(5) . . ? C8 C7 O5 124.1(6) . 3_666 ? C8 C7 C5 121.6(6) . . ? O5 C7 C5 114.2(5) 3_666 . ? C7 C8 C9 119.4(6) . . ? C7 C8 H8B 120.3 . . ? C9 C8 H8B 120.3 . . ? C10 C9 C8 120.9(6) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C6 120.3(6) . . ? C9 C10 H10A 119.8 . . ? C6 C10 H10A 119.8 . . ? O1 C11 C12 107.6(5) . . ? O1 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O1 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O2 C12 C11 110.2(5) . . ? O2 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? O2 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? O2 C13 C14 108.2(6) . . ? O2 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? O2 C13 H13B 110.1 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? O3 C14 C13 107.9(5) . . ? O3 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O3 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? O3 C15 C16 109.2(5) . . ? O3 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? O3 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? O4 C16 C15 108.6(5) . . ? O4 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O4 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O4 C17 C18 108.9(5) . . ? O4 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O4 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O5 C18 C17 107.1(5) . . ? O5 C18 H18A 110.3 . . ? C17 C18 H18A 110.3 . . ? O5 C18 H18B 110.3 . . ? C17 C18 H18B 110.3 . . ? H18A C18 H18B 108.6 . . ? C23 C19 C20 119.9(6) 3_666 . ? C23 C19 H19A 120.1 3_666 . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 121.1(5) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 119.9(5) . . ? C20 C21 C25 120.6(5) . . ? C22 C21 C25 119.4(5) . . ? C22 C22 C23 120.1(6) 3_666 . ? C22 C22 C21 119.1(7) 3_666 . ? C23 C22 C21 120.8(5) . . ? C19 C23 C22 119.8(5) 3_666 . ? C19 C23 C24 120.0(5) 3_666 . ? C22 C23 C24 120.3(5) . . ? O6 C24 N1 119.9(6) . . ? O6 C24 C23 122.6(5) . . ? N1 C24 C23 117.4(5) . . ? O7 C25 N1 120.4(6) . . ? O7 C25 C21 121.9(6) . . ? N1 C25 C21 117.7(5) . . ? C27 C26 N1 115.7(7) . . ? N1 C26 C27' 111.4(8) . . ? C27 C26 H26A 108.3 . . ? N1 C26 H26A 108.4 . . ? C27' C26 H26A 128.4 . . ? C27 C26 H26B 108.4 . . ? N1 C26 H26B 108.4 . . ? C27' C26 H26B 90.0 . . ? H26A C26 H26B 107.4 . . ? C26 C27 C28 103.5(9) . . ? C26 C27 H27A 111.1 . . ? C28 C27 H27A 111.1 . . ? C26 C27 H27B 111.1 . . ? C28 C27 H27B 111.1 . . ? H27A C27 H27B 109.0 . . ? C29 C28 C27 111.8(10) . . ? C29 C28 H28A 109.2 . . ? C27 C28 H28A 109.2 . . ? C29 C28 H28B 109.2 . . ? C27 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 110.1(12) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 108.5(12) . . ? C31 C30 H30A 110.0 . . ? C29 C30 H30A 110.0 . . ? C31 C30 H30B 110.0 . . ? C29 C30 H30B 110.0 . . ? H30A C30 H30B 108.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28' C27' C26 119.2(13) . . ? C28' C27' H27C 107.5 . . ? C26 C27' H27C 107.5 . . ? C28' C27' H27D 107.5 . . ? C26 C27' H27D 107.5 . . ? H27C C27' H27D 107.0 . . ? C27' C28' C29' 116.5(13) . . ? C27' C28' H28C 108.2 . . ? C29' C28' H28C 108.2 . . ? C27' C28' H28D 108.2 . . ? C29' C28' H28D 108.2 . . ? H28C C28' H28D 107.3 . . ? C28' C29' C30' 114.3(13) . . ? C28' C29' H29C 108.7 . . ? C30' C29' H29C 108.7 . . ? C28' C29' H29D 108.7 . . ? C30' C29' H29D 108.7 . . ? H29C C29' H29D 107.6 . . ? C31' C30' C29' 107.5(13) . . ? C31' C30' H30C 110.2 . . ? C29' C30' H30C 110.2 . . ? C31' C30' H30D 110.2 . . ? C29' C30' H30D 110.2 . . ? H30C C30' H30D 108.5 . . ? C30' C31' H31D 109.5 . . ? C30' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? Cl2 C32 Cl1 111.6(7) . . ? Cl2 C32 Cl3 119.7(8) . . ? Cl1 C32 Cl3 104.4(6) . . ? Cl2 C32 H32 106.8 . . ? Cl1 C32 H32 106.8 . . ? Cl3 C32 H32 106.8 . . ? Cl2' C32' Cl1' 107.6(7) . . ? Cl2' C32' Cl3' 105.3(7) . . ? Cl1' C32' Cl3' 122.1(9) . . ? Cl2' C32' H32' 107.0 . . ? Cl1' C32' H32' 107.0 . . ? Cl3' C32' H32' 107.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Na1 O2 C13 170.0(4) . . . . ? O3 Na1 O2 C13 31.0(4) . . . . ? O8 Na1 O2 C13 -74.6(4) . . . . ? O4 Na1 O2 C13 74.5(4) . . . . ? I1 Na1 O2 C13 -66.9(5) . . . . ? O6 Na1 O2 C12 -67.2(4) . . . . ? O3 Na1 O2 C12 153.8(4) . . . . ? O8 Na1 O2 C12 48.2(4) . . . . ? O4 Na1 O2 C12 -162.7(4) . . . . ? I1 Na1 O2 C12 55.9(5) . . . . ? O6 Na1 O3 C14 -67.3(5) . . . . ? O8 Na1 O3 C14 74.4(5) . . . . ? O2 Na1 O3 C14 0.7(4) . . . . ? O4 Na1 O3 C14 -140.0(5) . . . . ? I1 Na1 O3 C14 149.9(4) . . . . ? O6 Na1 O3 C15 76.6(5) . . . . ? O8 Na1 O3 C15 -141.7(5) . . . . ? O2 Na1 O3 C15 144.5(5) . . . . ? O4 Na1 O3 C15 3.9(4) . . . . ? I1 Na1 O3 C15 -66.3(5) . . . . ? O6 Na1 O4 C17 63.8(4) . . . . ? O3 Na1 O4 C17 -158.9(5) . . . . ? O8 Na1 O4 C17 -83.8(5) . . . . ? O2 Na1 O4 C17 157.3(4) . . . . ? I1 Na1 O4 C17 -40.2(4) . . . . ? O6 Na1 O4 C16 -170.5(4) . . . . ? O3 Na1 O4 C16 -33.2(4) . . . . ? O8 Na1 O4 C16 41.9(5) . . . . ? O2 Na1 O4 C16 -77.0(4) . . . . ? I1 Na1 O4 C16 85.5(4) . . . . ? O3 Na1 O6 C24 13.3(11) . . . . ? O8 Na1 O6 C24 -124.3(10) . . . . ? O2 Na1 O6 C24 -46.2(10) . . . . ? O4 Na1 O6 C24 75.6(10) . . . . ? I1 Na1 O6 C24 158.2(10) . . . . ? C11 O1 C1 C2 3.0(8) . . . . ? C11 O1 C1 C6 -177.2(5) . . . . ? O1 C1 C2 C3 179.2(5) . . . . ? C6 C1 C2 C3 -0.6(9) . . . . ? C1 C2 C3 C4 -0.5(9) . . . . ? C2 C3 C4 C5 0.5(9) . . . . ? C3 C4 C5 C6 0.6(8) . . . . ? C3 C4 C5 C7 179.3(6) . . . . ? C4 C5 C6 C10 178.3(5) . . . . ? C7 C5 C6 C10 -0.5(8) . . . . ? C4 C5 C6 C1 -1.7(8) . . . . ? C7 C5 C6 C1 179.6(5) . . . . ? O1 C1 C6 C10 1.9(8) . . . . ? C2 C1 C6 C10 -178.2(5) . . . . ? O1 C1 C6 C5 -178.1(5) . . . . ? C2 C1 C6 C5 1.7(8) . . . . ? C4 C5 C7 C8 -177.3(5) . . . . ? C6 C5 C7 C8 1.4(8) . . . . ? C4 C5 C7 O5 1.7(8) . . . 3_666 ? C6 C5 C7 O5 -179.6(5) . . . 3_666 ? O5 C7 C8 C9 179.8(5) 3_666 . . . ? C5 C7 C8 C9 -1.3(9) . . . . ? C7 C8 C9 C10 0.2(9) . . . . ? C8 C9 C10 C6 0.7(9) . . . . ? C5 C6 C10 C9 -0.6(9) . . . . ? C1 C6 C10 C9 179.4(5) . . . . ? C1 O1 C11 C12 169.1(5) . . . . ? C13 O2 C12 C11 -176.5(5) . . . . ? Na1 O2 C12 C11 64.7(6) . . . . ? O1 C11 C12 O2 67.3(6) . . . . ? C12 O2 C13 C14 169.2(5) . . . . ? Na1 O2 C13 C14 -59.2(6) . . . . ? C15 O3 C14 C13 -178.3(6) . . . . ? Na1 O3 C14 C13 -31.7(7) . . . . ? O2 C13 C14 O3 64.2(7) . . . . ? C14 O3 C15 C16 172.5(6) . . . . ? Na1 O3 C15 C16 26.1(7) . . . . ? C17 O4 C16 C15 -166.0(5) . . . . ? Na1 O4 C16 C15 59.7(6) . . . . ? O3 C15 C16 O4 -60.9(7) . . . . ? C16 O4 C17 C18 179.3(5) . . . . ? Na1 O4 C17 C18 -59.3(6) . . . . ? C7 O5 C18 C17 178.9(5) 3_666 . . . ? O4 C17 C18 O5 -71.1(6) . . . . ? C23 C19 C20 C21 0.8(9) 3_666 . . . ? C19 C20 C21 C22 -1.5(9) . . . . ? C19 C20 C21 C25 -179.3(6) . . . . ? C20 C21 C22 C22 1.3(9) . . . 3_666 ? C25 C21 C22 C22 179.1(6) . . . 3_666 ? C20 C21 C22 C23 -179.1(5) . . . . ? C25 C21 C22 C23 -1.3(8) . . . . ? C22 C22 C23 C19 0.4(9) 3_666 . . 3_666 ? C21 C22 C23 C19 -179.3(5) . . . 3_666 ? C22 C22 C23 C24 -179.4(6) 3_666 . . . ? C21 C22 C23 C24 0.9(8) . . . . ? Na1 O6 C24 N1 159.0(8) . . . . ? Na1 O6 C24 C23 -20.2(14) . . . . ? C25 N1 C24 O6 177.5(6) . . . . ? C26 N1 C24 O6 -2.3(8) . . . . ? C25 N1 C24 C23 -3.3(8) . . . . ? C26 N1 C24 C23 176.9(5) . . . . ? C19 C23 C24 O6 0.6(8) 3_666 . . . ? C22 C23 C24 O6 -179.6(5) . . . . ? C19 C23 C24 N1 -178.5(5) 3_666 . . . ? C22 C23 C24 N1 1.3(8) . . . . ? C24 N1 C25 O7 -176.8(6) . . . . ? C26 N1 C25 O7 3.0(9) . . . . ? C24 N1 C25 C21 2.9(9) . . . . ? C26 N1 C25 C21 -177.3(6) . . . . ? C20 C21 C25 O7 -3.0(10) . . . . ? C22 C21 C25 O7 179.2(6) . . . . ? C20 C21 C25 N1 177.2(5) . . . . ? C22 C21 C25 N1 -0.5(8) . . . . ? C24 N1 C26 C27 108.3(10) . . . . ? C25 N1 C26 C27 -71.5(11) . . . . ? C24 N1 C26 C27' 83.8(10) . . . . ? C25 N1 C26 C27' -96.0(10) . . . . ? N1 C26 C27 C28 163.4(10) . . . . ? C26 C27 C28 C29 166.5(17) . . . . ? C27 C28 C29 C30 168.5(18) . . . . ? C28 C29 C30 C31 -178(2) . . . . ? N1 C26 C27' C28' 174.4(12) . . . . ? C26 C27' C28' C29' -108(2) . . . . ? C27' C28' C29' C30' -173.8(16) . . . . ? C28' C29' C30' C31' -133(2) . . . . ? #============================================================================== data_[Li2.2.A]Br2 _database_code_depnum_ccdc_archive 'CCDC 644504' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C62 H78 Li2 N2 O16 2+, 2(Br -), 8(C H Cl3) ; _chemical_formula_sum 'C70 H86 Br2 Cl24 Li2 N2 O16' _chemical_formula_weight 2235.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0570(5) _cell_length_b 15.2801(7) _cell_length_c 17.2223(8) _cell_angle_alpha 70.219(2) _cell_angle_beta 78.484(2) _cell_angle_gamma 83.267(2) _cell_volume 2436.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15344 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 29.14 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.912 _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 SHELXL. ; _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6923 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 24659 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 29.49 _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _reflns_number_total 13055 _reflns_number_gt 11170 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1994)' _computing_cell_refinement 'SAINT (Bruker, 1994)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL v.6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1068P)^2^+1.6592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13055 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.818 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.207 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.6011(4) 0.2133(3) 0.3211(3) 0.0279(8) Uani 1 1 d . . . Br1 Br 0.49722(3) 0.080342(16) 0.606105(15) 0.03242(9) Uani 1 1 d . . . N1 N 0.51772(19) 0.48064(13) 0.30021(11) 0.0203(3) Uani 1 1 d . . . O1 O 0.21474(19) 0.29746(13) 0.39616(12) 0.0302(4) Uani 1 1 d . . . O2 O 0.39208(17) 0.19685(12) 0.30723(11) 0.0272(3) Uani 1 1 d . . . O3 O 0.62905(18) 0.18909(13) 0.20961(11) 0.0278(3) Uani 1 1 d . . . O4 O 0.81940(17) 0.24581(12) 0.26663(11) 0.0259(3) Uani 1 1 d . . . O5 O 0.87669(19) 0.38451(12) 0.32617(11) 0.0287(3) Uani 1 1 d . . . O6 O 0.55539(17) 0.32407(11) 0.35357(11) 0.0245(3) Uani 1 1 d . . . O7 O 0.4894(2) 0.63741(12) 0.24567(11) 0.0297(4) Uani 1 1 d . . . O8 O 0.6344(2) 0.10110(13) 0.40966(12) 0.0332(4) Uani 1 1 d . . . H81 H 0.5985 0.1015 0.4586 0.050 Uiso 1 1 d R . . H82 H 0.6141 0.0509 0.4049 0.050 Uiso 1 1 d R . . C1 C 0.1707(2) 0.52363(16) 0.42310(14) 0.0234(4) Uani 1 1 d . . . H1A H 0.1639 0.5867 0.3884 0.028 Uiso 1 1 calc R . . C2 C 0.1872(2) 0.45394(17) 0.38821(15) 0.0246(4) Uani 1 1 d . . . H2A H 0.1917 0.4689 0.3296 0.030 Uiso 1 1 calc R . . C3 C 0.1977(2) 0.35973(17) 0.43912(15) 0.0249(4) Uani 1 1 d . . . C4 C 0.1907(2) 0.33651(17) 0.52429(15) 0.0256(4) Uani 1 1 d . . . H4A H 0.1982 0.2731 0.5581 0.031 Uiso 1 1 calc R . . C5 C 0.1626(2) 0.38782(17) 0.64905(15) 0.0260(4) Uani 1 1 d . . . H5A H 0.1676 0.3248 0.6843 0.031 Uiso 1 1 calc R . . C6 C 0.1461(2) 0.45774(17) 0.68337(15) 0.0264(4) Uani 1 1 d . . . H6A H 0.1392 0.4430 0.7422 0.032 Uiso 1 1 calc R . . C7 C 0.1393(2) 0.55210(17) 0.63178(15) 0.0245(4) Uani 1 1 d . . . C8 C 0.1481(2) 0.57443(16) 0.54706(14) 0.0232(4) Uani 1 1 d . . . H8A H 0.1439 0.6379 0.5128 0.028 Uiso 1 1 calc R . . C9 C 0.1636(2) 0.50269(15) 0.51050(14) 0.0214(4) Uani 1 1 d . . . C10 C 0.1722(2) 0.40816(16) 0.56119(14) 0.0227(4) Uani 1 1 d . . . C11 C 0.2653(2) 0.20565(17) 0.43749(16) 0.0288(5) Uani 1 1 d . . . H11A H 0.1984 0.1743 0.4871 0.035 Uiso 1 1 calc R . . H11B H 0.3513 0.2080 0.4563 0.035 Uiso 1 1 calc R . . C12 C 0.2890(3) 0.15402(18) 0.37556(17) 0.0307(5) Uani 1 1 d . . . H12A H 0.3177 0.0883 0.4029 0.037 Uiso 1 1 calc R . . H12B H 0.2038 0.1550 0.3547 0.037 Uiso 1 1 calc R . . C13 C 0.3973(3) 0.16408(18) 0.23888(16) 0.0296(5) Uani 1 1 d . . . H13A H 0.3101 0.1799 0.2177 0.036 Uiso 1 1 calc R . . H13B H 0.4140 0.0956 0.2567 0.036 Uiso 1 1 calc R . . C14 C 0.5105(3) 0.20998(19) 0.17196(16) 0.0303(5) Uani 1 1 d . . . H14A H 0.5228 0.1855 0.1245 0.036 Uiso 1 1 calc R . . H14B H 0.4910 0.2782 0.1509 0.036 Uiso 1 1 calc R . . C15 C 0.7502(3) 0.22159(19) 0.15317(16) 0.0306(5) Uani 1 1 d . . . H15A H 0.7403 0.2895 0.1242 0.037 Uiso 1 1 calc R . . H15B H 0.7718 0.1895 0.1106 0.037 Uiso 1 1 calc R . . C16 C 0.8599(3) 0.1998(2) 0.20564(17) 0.0323(5) Uani 1 1 d . . . H16A H 0.8711 0.1318 0.2333 0.039 Uiso 1 1 calc R . . H16B H 0.9475 0.2224 0.1703 0.039 Uiso 1 1 calc R . . C17 C 0.9208(3) 0.23257(19) 0.31713(17) 0.0298(5) Uani 1 1 d . . . H17A H 1.0090 0.2520 0.2809 0.036 Uiso 1 1 calc R . . H17B H 0.9313 0.1657 0.3498 0.036 Uiso 1 1 calc R . . C18 C 0.8822(2) 0.28840(17) 0.37556(15) 0.0272(4) Uani 1 1 d . . . H18A H 0.7925 0.2709 0.4107 0.033 Uiso 1 1 calc R . . H18B H 0.9503 0.2764 0.4128 0.033 Uiso 1 1 calc R . . C19 C 0.5347(2) 0.39950(15) 0.36564(13) 0.0187(4) Uani 1 1 d . . . C20 C 0.52484(19) 0.40783(14) 0.44965(13) 0.0174(4) Uani 1 1 d . . . C21 C 0.5360(2) 0.32890(14) 0.51762(13) 0.0203(4) Uani 1 1 d . . . H21A H 0.5495 0.2694 0.5104 0.024 Uiso 1 1 calc R . . C22 C 0.5273(2) 0.33655(14) 0.59723(14) 0.0207(4) Uani 1 1 d . . . H22A H 0.5352 0.2819 0.6438 0.025 Uiso 1 1 calc R . . C23 C 0.50744(19) 0.42238(14) 0.60888(12) 0.0175(4) Uani 1 1 d . . . C24 C 0.49552(19) 0.50382(13) 0.54020(12) 0.0162(3) Uani 1 1 d . . . C25 C 0.4997(2) 0.56980(15) 0.30745(13) 0.0206(4) Uani 1 1 d . . . C26 C 0.5159(2) 0.47372(17) 0.21705(14) 0.0249(4) Uani 1 1 d . . . H26A H 0.4495 0.5214 0.1895 0.030 Uiso 1 1 calc R . . H26B H 0.4852 0.4118 0.2242 0.030 Uiso 1 1 calc R . . C27 C 0.6549(2) 0.48725(19) 0.16053(15) 0.0277(5) Uani 1 1 d . . . H27A H 0.6938 0.5434 0.1615 0.033 Uiso 1 1 calc R . . H27B H 0.7171 0.4329 0.1820 0.033 Uiso 1 1 calc R . . C28 C 0.6435(3) 0.49807(18) 0.07062(15) 0.0287(5) Uani 1 1 d . . . H28A H 0.6019 0.4425 0.0705 0.034 Uiso 1 1 calc R . . H28B H 0.5818 0.5529 0.0496 0.034 Uiso 1 1 calc R . . C29 C 0.7783(3) 0.5098(2) 0.01124(16) 0.0329(5) Uani 1 1 d . . . H29A H 0.8336 0.4504 0.0257 0.039 Uiso 1 1 calc R . . H29B H 0.8279 0.5577 0.0190 0.039 Uiso 1 1 calc R . . C30 C 0.7632(3) 0.5382(3) -0.08002(18) 0.0439(7) Uani 1 1 d . . . H30A H 0.7091 0.5981 -0.0947 0.053 Uiso 1 1 calc R . . H30B H 0.7124 0.4908 -0.0876 0.053 Uiso 1 1 calc R . . C31 C 0.8991(4) 0.5486(3) -0.1397(2) 0.0589(10) Uani 1 1 d . . . H31A H 0.8829 0.5674 -0.1975 0.088 Uiso 1 1 calc R . . H31B H 0.9521 0.4890 -0.1267 0.088 Uiso 1 1 calc R . . H31C H 0.9494 0.5962 -0.1332 0.088 Uiso 1 1 calc R . . C32 C 0.8534(4) 0.8205(3) 0.0086(2) 0.0560(9) Uani 1 1 d . . . H32A H 0.8073 0.8341 0.0607 0.067 Uiso 1 1 calc R . . C33 C 0.2788(3) 0.7474(2) 0.14184(18) 0.0392(6) Uani 1 1 d . . . H33A H 0.3480 0.7465 0.1766 0.047 Uiso 1 1 calc R . . C34 C 0.1697(4) 0.9109(2) 0.3554(2) 0.0443(7) Uani 1 1 d . . . H34A H 0.2671 0.9092 0.3613 0.053 Uiso 1 1 calc R . . C35 C 0.3173(4) 0.0765(2) 0.8029(2) 0.0494(8) Uani 1 1 d . . . H35A H 0.3725 0.0549 0.7570 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.95260(11) 0.91257(6) -0.05457(7) 0.0611(2) Uani 1 1 d . . . Cl2 Cl 0.95957(18) 0.71738(9) 0.03629(12) 0.0967(5) Uani 1 1 d . . . Cl3 Cl 0.7329(2) 0.8033(2) -0.04149(18) 0.1624(11) Uani 1 1 d . . . Cl4 Cl 0.36053(13) 0.71334(9) 0.05632(6) 0.0740(3) Uani 1 1 d . . . Cl5 Cl 0.15426(10) 0.66992(7) 0.20400(5) 0.0563(2) Uani 1 1 d . . . Cl6 Cl 0.20836(13) 0.86067(7) 0.10685(7) 0.0705(3) Uani 1 1 d . . . Cl7 Cl 0.13554(14) 0.80101(6) 0.35465(8) 0.0701(3) Uani 1 1 d . . . Cl8 Cl 0.06777(18) 0.93703(11) 0.44058(10) 0.0958(5) Uani 1 1 d . . . Cl9 Cl 0.14501(13) 0.99687(6) 0.26145(7) 0.0662(3) Uani 1 1 d . . . Cl10 Cl 0.14708(14) 0.09583(12) 0.78811(11) 0.0935(5) Uani 1 1 d . . . Cl11 Cl 0.32882(15) -0.00952(7) 0.89889(7) 0.0712(3) Uani 1 1 d . . . Cl12 Cl 0.37959(10) 0.18133(6) 0.79873(5) 0.0526(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.034(2) 0.0265(19) 0.0253(19) -0.0111(16) -0.0046(16) -0.0020(15) Br1 0.04698(16) 0.02219(13) 0.02610(13) -0.00556(9) -0.00451(10) -0.00396(10) N1 0.0226(8) 0.0219(8) 0.0172(8) -0.0074(7) -0.0032(6) -0.0021(6) O1 0.0314(9) 0.0295(9) 0.0321(9) -0.0126(7) -0.0104(7) 0.0058(7) O2 0.0267(8) 0.0296(8) 0.0290(8) -0.0137(7) -0.0044(6) -0.0043(6) O3 0.0280(8) 0.0337(9) 0.0225(8) -0.0097(7) -0.0046(6) -0.0027(7) O4 0.0248(8) 0.0300(8) 0.0261(8) -0.0136(7) -0.0043(6) 0.0001(6) O5 0.0357(9) 0.0278(8) 0.0230(8) -0.0076(7) -0.0048(7) -0.0058(7) O6 0.0267(8) 0.0220(7) 0.0267(8) -0.0117(6) -0.0014(6) -0.0025(6) O7 0.0434(10) 0.0249(8) 0.0190(7) -0.0030(6) -0.0098(7) 0.0003(7) O8 0.0464(11) 0.0254(8) 0.0268(9) -0.0062(7) -0.0059(8) -0.0060(7) C1 0.0190(9) 0.0266(10) 0.0221(10) -0.0043(8) -0.0031(7) -0.0037(8) C2 0.0200(9) 0.0305(11) 0.0233(10) -0.0079(9) -0.0041(8) -0.0023(8) C3 0.0181(9) 0.0294(11) 0.0277(11) -0.0097(9) -0.0051(8) -0.0004(8) C4 0.0208(10) 0.0260(10) 0.0273(11) -0.0053(9) -0.0041(8) -0.0003(8) C5 0.0232(10) 0.0280(11) 0.0220(10) -0.0023(8) -0.0031(8) -0.0021(8) C6 0.0235(10) 0.0318(11) 0.0211(10) -0.0044(9) -0.0032(8) -0.0041(8) C7 0.0202(9) 0.0288(11) 0.0251(10) -0.0083(9) -0.0036(8) -0.0048(8) C8 0.0179(9) 0.0252(10) 0.0249(10) -0.0056(8) -0.0027(7) -0.0046(7) C9 0.0137(8) 0.0259(10) 0.0225(10) -0.0050(8) -0.0025(7) -0.0031(7) C10 0.0164(9) 0.0273(10) 0.0227(10) -0.0057(8) -0.0026(7) -0.0023(7) C11 0.0255(11) 0.0269(11) 0.0314(12) -0.0084(9) -0.0021(9) 0.0004(8) C12 0.0273(11) 0.0280(11) 0.0373(13) -0.0122(10) -0.0024(9) -0.0042(9) C13 0.0316(12) 0.0322(12) 0.0308(12) -0.0149(10) -0.0094(9) -0.0029(9) C14 0.0349(12) 0.0329(12) 0.0256(11) -0.0099(9) -0.0104(9) -0.0007(9) C15 0.0330(12) 0.0371(13) 0.0233(11) -0.0134(10) -0.0003(9) -0.0043(10) C16 0.0302(12) 0.0381(13) 0.0319(12) -0.0192(11) 0.0007(9) -0.0012(10) C17 0.0261(11) 0.0336(12) 0.0314(12) -0.0127(10) -0.0071(9) 0.0022(9) C18 0.0271(11) 0.0282(11) 0.0268(11) -0.0081(9) -0.0069(8) -0.0025(8) C19 0.0161(8) 0.0204(9) 0.0196(9) -0.0071(7) -0.0006(7) -0.0031(7) C20 0.0157(8) 0.0180(9) 0.0186(9) -0.0060(7) -0.0019(7) -0.0024(6) C21 0.0218(9) 0.0161(9) 0.0215(10) -0.0055(7) -0.0011(7) -0.0011(7) C22 0.0224(9) 0.0170(9) 0.0203(9) -0.0032(7) -0.0034(7) -0.0011(7) C23 0.0160(8) 0.0182(9) 0.0172(9) -0.0043(7) -0.0029(7) -0.0010(6) C24 0.0135(8) 0.0173(8) 0.0173(9) -0.0049(7) -0.0017(6) -0.0024(6) C25 0.0214(9) 0.0208(9) 0.0192(9) -0.0053(7) -0.0045(7) -0.0009(7) C26 0.0283(11) 0.0300(11) 0.0192(10) -0.0107(8) -0.0053(8) -0.0023(8) C27 0.0281(11) 0.0363(12) 0.0192(10) -0.0100(9) -0.0032(8) -0.0026(9) C28 0.0337(12) 0.0330(12) 0.0198(10) -0.0093(9) -0.0046(9) -0.0012(9) C29 0.0378(13) 0.0386(13) 0.0220(11) -0.0101(10) -0.0004(9) -0.0080(10) C30 0.0495(17) 0.0583(19) 0.0226(12) -0.0119(12) 0.0001(11) -0.0119(14) C31 0.068(2) 0.076(3) 0.0300(15) -0.0176(16) 0.0123(15) -0.025(2) C32 0.063(2) 0.070(2) 0.0388(17) -0.0225(17) -0.0041(15) -0.0115(18) C33 0.0463(16) 0.0363(14) 0.0263(12) 0.0001(10) -0.0075(11) 0.0029(11) C34 0.0483(17) 0.0391(15) 0.0432(16) -0.0055(12) -0.0117(13) -0.0101(12) C35 0.063(2) 0.0445(17) 0.0370(16) -0.0139(13) 0.0106(14) -0.0175(15) Cl1 0.0730(6) 0.0428(4) 0.0588(5) -0.0142(4) 0.0009(4) 0.0029(4) Cl2 0.1071(10) 0.0507(6) 0.1233(12) 0.0049(7) -0.0516(9) -0.0142(6) Cl3 0.1119(15) 0.221(3) 0.165(2) -0.026(2) -0.0864(15) -0.0539(16) Cl4 0.0921(8) 0.0762(7) 0.0346(4) -0.0109(4) 0.0024(4) 0.0262(6) Cl5 0.0659(5) 0.0549(5) 0.0393(4) 0.0016(3) -0.0097(4) -0.0188(4) Cl6 0.0895(7) 0.0387(4) 0.0593(6) 0.0033(4) -0.0025(5) 0.0147(4) Cl7 0.1018(8) 0.0319(4) 0.0764(7) -0.0060(4) -0.0334(6) -0.0067(4) Cl8 0.1111(11) 0.0845(9) 0.0842(9) -0.0375(7) 0.0381(8) -0.0391(8) Cl9 0.0932(7) 0.0400(4) 0.0652(6) 0.0024(4) -0.0382(5) -0.0197(4) Cl10 0.0605(7) 0.0946(10) 0.1118(11) -0.0104(8) -0.0105(7) -0.0278(6) Cl11 0.1155(9) 0.0374(4) 0.0485(5) -0.0072(4) 0.0035(5) -0.0074(5) Cl12 0.0700(5) 0.0422(4) 0.0388(4) -0.0088(3) 0.0099(4) -0.0220(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O8 1.918(5) . ? Li1 O6 1.934(4) . ? Li1 O3 2.036(4) . ? Li1 O2 2.215(5) . ? Li1 O4 2.250(5) . ? N1 C19 1.385(3) . ? N1 C25 1.397(3) . ? N1 C26 1.475(3) . ? O1 C3 1.367(3) . ? O1 C11 1.426(3) . ? O2 C13 1.417(3) . ? O2 C12 1.428(3) . ? O3 C15 1.421(3) . ? O3 C14 1.422(3) . ? O4 C16 1.423(3) . ? O4 C17 1.423(3) . ? O5 C7 1.371(3) 2_666 ? O5 C18 1.428(3) . ? O6 C19 1.226(3) . ? O7 C25 1.219(3) . ? O8 H81 0.850 . ? O8 H82 0.850 . ? C1 C2 1.369(3) . ? C1 C9 1.417(3) . ? C1 H1A 0.950 . ? C2 C3 1.414(3) . ? C2 H2A 0.950 . ? C3 C4 1.377(3) . ? C4 C10 1.419(3) . ? C4 H4A 0.950 . ? C5 C6 1.366(4) . ? C5 C10 1.423(3) . ? C5 H5A 0.950 . ? C6 C7 1.417(3) . ? C6 H6A 0.950 . ? C7 C8 1.368(3) . ? C7 O5 1.371(3) 2_666 ? C8 C9 1.418(3) . ? C8 H8A 0.950 . ? C9 C10 1.415(3) . ? C11 C12 1.497(4) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.494(4) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.501(4) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 C18 1.496(3) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.478(3) . ? C20 C21 1.379(3) . ? C20 C24 1.406(3) 2_666 ? C21 C22 1.400(3) . ? C21 H21A 0.950 . ? C22 C23 1.379(3) . ? C22 H22A 0.950 . ? C23 C24 1.410(3) . ? C23 C25 1.473(3) 2_666 ? C24 C20 1.406(3) 2_666 ? C24 C24 1.413(4) 2_666 ? C25 C23 1.473(3) 2_666 ? C26 C27 1.528(3) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.527(3) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 C29 1.515(4) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C29 C30 1.517(4) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 C31 1.526(5) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.980 . ? C31 H31B 0.980 . ? C31 H31C 0.980 . ? C32 Cl3 1.711(4) . ? C32 Cl1 1.738(4) . ? C32 Cl2 1.775(5) . ? C32 H32A 1.000 . ? C33 Cl6 1.743(3) . ? C33 Cl4 1.746(3) . ? C33 Cl5 1.753(3) . ? C33 H33A 1.000 . ? C34 Cl9 1.747(3) . ? C34 Cl8 1.750(4) . ? C34 Cl7 1.757(3) . ? C34 H34A 1.000 . ? C35 Cl11 1.745(4) . ? C35 Cl10 1.756(4) . ? C35 Cl12 1.761(3) . ? C35 H35A 1.000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Li1 O6 115.5(2) . . ? O8 Li1 O3 110.8(2) . . ? O6 Li1 O3 133.6(2) . . ? O8 Li1 O2 101.8(2) . . ? O6 Li1 O2 95.27(19) . . ? O3 Li1 O2 76.78(16) . . ? O8 Li1 O4 97.5(2) . . ? O6 Li1 O4 95.26(19) . . ? O3 Li1 O4 76.67(16) . . ? O2 Li1 O4 151.4(2) . . ? C19 N1 C25 124.48(18) . . ? C19 N1 C26 118.60(18) . . ? C25 N1 C26 116.92(18) . . ? C3 O1 C11 116.9(2) . . ? C13 O2 C12 111.40(19) . . ? C13 O2 Li1 109.58(18) . . ? C12 O2 Li1 123.89(19) . . ? C15 O3 C14 114.17(19) . . ? C15 O3 Li1 115.95(19) . . ? C14 O3 Li1 113.39(19) . . ? C16 O4 C17 111.06(19) . . ? C16 O4 Li1 106.04(17) . . ? C17 O4 Li1 122.71(18) . . ? C7 O5 C18 116.77(19) 2_666 . ? C19 O6 Li1 172.8(2) . . ? Li1 O8 H81 114.9 . . ? Li1 O8 H82 116.1 . . ? H81 O8 H82 107.4 . . ? C2 C1 C9 120.7(2) . . ? C2 C1 H1A 119.6 . . ? C9 C1 H1A 119.6 . . ? C1 C2 C3 120.3(2) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? O1 C3 C4 125.1(2) . . ? O1 C3 C2 114.2(2) . . ? C4 C3 C2 120.8(2) . . ? C3 C4 C10 119.4(2) . . ? C3 C4 H4A 120.3 . . ? C10 C4 H4A 120.3 . . ? C6 C5 C10 120.8(2) . . ? C6 C5 H5A 119.6 . . ? C10 C5 H5A 119.6 . . ? C5 C6 C7 120.4(2) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C8 C7 O5 124.8(2) . 2_666 ? C8 C7 C6 120.5(2) . . ? O5 C7 C6 114.6(2) 2_666 . ? C7 C8 C9 119.8(2) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C10 C9 C1 118.7(2) . . ? C10 C9 C8 120.2(2) . . ? C1 C9 C8 121.1(2) . . ? C9 C10 C4 120.1(2) . . ? C9 C10 C5 118.2(2) . . ? C4 C10 C5 121.6(2) . . ? O1 C11 C12 107.0(2) . . ? O1 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? O1 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? O2 C12 C11 109.4(2) . . ? O2 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? O2 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? O2 C13 C14 107.6(2) . . ? O2 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? O2 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? O3 C14 C13 106.2(2) . . ? O3 C14 H14A 110.5 . . ? C13 C14 H14A 110.5 . . ? O3 C14 H14B 110.5 . . ? C13 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? O3 C15 C16 105.9(2) . . ? O3 C15 H15A 110.6 . . ? C16 C15 H15A 110.6 . . ? O3 C15 H15B 110.6 . . ? C16 C15 H15B 110.6 . . ? H15A C15 H15B 108.7 . . ? O4 C16 C15 107.1(2) . . ? O4 C16 H16A 110.3 . . ? C15 C16 H16A 110.3 . . ? O4 C16 H16B 110.3 . . ? C15 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? O4 C17 C18 110.27(19) . . ? O4 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? O4 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? O5 C18 C17 107.9(2) . . ? O5 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? O5 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? O6 C19 N1 120.61(19) . . ? O6 C19 C20 122.01(19) . . ? N1 C19 C20 117.38(18) . . ? C21 C20 C24 120.38(19) . 2_666 ? C21 C20 C19 119.83(18) . . ? C24 C20 C19 119.80(18) 2_666 . ? C20 C21 C22 119.99(19) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C21 120.79(19) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 120.03(19) . . ? C22 C23 C25 120.60(18) . 2_666 ? C24 C23 C25 119.36(18) . 2_666 ? C20 C24 C23 121.19(18) 2_666 . ? C20 C24 C24 119.6(2) 2_666 2_666 ? C23 C24 C24 119.2(2) . 2_666 ? O7 C25 N1 119.7(2) . . ? O7 C25 C23 122.6(2) . 2_666 ? N1 C25 C23 117.70(18) . 2_666 ? N1 C26 C27 112.62(18) . . ? N1 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? N1 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C28 C27 C26 110.9(2) . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 113.8(2) . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C28 C29 C30 113.2(2) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.8 . . ? C29 C30 C31 113.2(3) . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Cl3 C32 Cl1 111.5(2) . . ? Cl3 C32 Cl2 108.9(3) . . ? Cl1 C32 Cl2 109.1(2) . . ? Cl3 C32 H32A 109.1 . . ? Cl1 C32 H32A 109.1 . . ? Cl2 C32 H32A 109.1 . . ? Cl6 C33 Cl4 109.83(16) . . ? Cl6 C33 Cl5 110.99(18) . . ? Cl4 C33 Cl5 110.69(19) . . ? Cl6 C33 H33A 108.4 . . ? Cl4 C33 H33A 108.4 . . ? Cl5 C33 H33A 108.4 . . ? Cl9 C34 Cl8 110.5(2) . . ? Cl9 C34 Cl7 110.53(19) . . ? Cl8 C34 Cl7 110.67(19) . . ? Cl9 C34 H34A 108.4 . . ? Cl8 C34 H34A 108.4 . . ? Cl7 C34 H34A 108.4 . . ? Cl11 C35 Cl10 109.67(19) . . ? Cl11 C35 Cl12 110.8(2) . . ? Cl10 C35 Cl12 109.5(2) . . ? Cl11 C35 H35A 108.9 . . ? Cl10 C35 H35A 108.9 . . ? Cl12 C35 H35A 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Li1 O2 C13 -99.2(2) . . . . ? O6 Li1 O2 C13 143.33(19) . . . . ? O3 Li1 O2 C13 9.7(2) . . . . ? O4 Li1 O2 C13 32.2(5) . . . . ? O8 Li1 O2 C12 35.6(3) . . . . ? O6 Li1 O2 C12 -81.8(2) . . . . ? O3 Li1 O2 C12 144.57(19) . . . . ? O4 Li1 O2 C12 167.0(4) . . . . ? O8 Li1 O3 C15 -105.2(3) . . . . ? O6 Li1 O3 C15 72.3(4) . . . . ? O2 Li1 O3 C15 156.97(19) . . . . ? O4 Li1 O3 C15 -12.2(2) . . . . ? O8 Li1 O3 C14 119.8(2) . . . . ? O6 Li1 O3 C14 -62.6(4) . . . . ? O2 Li1 O3 C14 22.0(2) . . . . ? O4 Li1 O3 C14 -147.14(18) . . . . ? O8 Li1 O4 C16 89.4(2) . . . . ? O6 Li1 O4 C16 -154.00(19) . . . . ? O3 Li1 O4 C16 -20.4(2) . . . . ? O2 Li1 O4 C16 -42.8(5) . . . . ? O8 Li1 O4 C17 -39.6(3) . . . . ? O6 Li1 O4 C17 77.0(2) . . . . ? O3 Li1 O4 C17 -149.35(19) . . . . ? O2 Li1 O4 C17 -171.8(4) . . . . ? C9 C1 C2 C3 -0.1(3) . . . . ? C11 O1 C3 C4 -17.9(3) . . . . ? C11 O1 C3 C2 162.1(2) . . . . ? C1 C2 C3 O1 -179.6(2) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? O1 C3 C4 C10 -179.7(2) . . . . ? C2 C3 C4 C10 0.3(3) . . . . ? C10 C5 C6 C7 -0.4(3) . . . . ? C5 C6 C7 C8 0.4(3) . . . . ? C5 C6 C7 O5 -179.7(2) . . . 2_666 ? O5 C7 C8 C9 -179.5(2) 2_666 . . . ? C6 C7 C8 C9 0.3(3) . . . . ? C2 C1 C9 C10 -0.8(3) . . . . ? C2 C1 C9 C8 179.2(2) . . . . ? C7 C8 C9 C10 -1.1(3) . . . . ? C7 C8 C9 C1 178.9(2) . . . . ? C1 C9 C10 C4 1.4(3) . . . . ? C8 C9 C10 C4 -178.59(19) . . . . ? C1 C9 C10 C5 -178.91(19) . . . . ? C8 C9 C10 C5 1.1(3) . . . . ? C3 C4 C10 C9 -1.2(3) . . . . ? C3 C4 C10 C5 179.2(2) . . . . ? C6 C5 C10 C9 -0.3(3) . . . . ? C6 C5 C10 C4 179.3(2) . . . . ? C3 O1 C11 C12 -174.2(2) . . . . ? C13 O2 C12 C11 -167.0(2) . . . . ? Li1 O2 C12 C11 58.8(3) . . . . ? O1 C11 C12 O2 63.7(3) . . . . ? C12 O2 C13 C14 -178.1(2) . . . . ? Li1 O2 C13 C14 -37.3(3) . . . . ? C15 O3 C14 C13 175.5(2) . . . . ? Li1 O3 C14 C13 -48.7(3) . . . . ? O2 C13 C14 O3 55.7(3) . . . . ? C14 O3 C15 C16 175.5(2) . . . . ? Li1 O3 C15 C16 40.9(3) . . . . ? C17 O4 C16 C15 -177.3(2) . . . . ? Li1 O4 C16 C15 47.2(3) . . . . ? O3 C15 C16 O4 -58.4(3) . . . . ? C16 O4 C17 C18 174.9(2) . . . . ? Li1 O4 C17 C18 -58.3(3) . . . . ? C7 O5 C18 C17 -171.50(19) 2_666 . . . ? O4 C17 C18 O5 -62.9(3) . . . . ? C25 N1 C19 O6 -177.06(19) . . . . ? C26 N1 C19 O6 4.1(3) . . . . ? C25 N1 C19 C20 3.8(3) . . . . ? C26 N1 C19 C20 -175.11(18) . . . . ? O6 C19 C20 C21 -1.5(3) . . . . ? N1 C19 C20 C21 177.65(18) . . . . ? O6 C19 C20 C24 178.35(19) . . . 2_666 ? N1 C19 C20 C24 -2.5(3) . . . 2_666 ? C24 C20 C21 C22 -0.1(3) 2_666 . . . ? C19 C20 C21 C22 179.73(19) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C21 C22 C23 C25 -179.13(19) . . . 2_666 ? C22 C23 C24 C20 179.97(18) . . . 2_666 ? C25 C23 C24 C20 -0.9(3) 2_666 . . 2_666 ? C22 C23 C24 C24 -0.1(3) . . . 2_666 ? C25 C23 C24 C24 179.0(2) 2_666 . . 2_666 ? C19 N1 C25 O7 177.9(2) . . . . ? C26 N1 C25 O7 -3.2(3) . . . . ? C19 N1 C25 C23 -2.7(3) . . . 2_666 ? C26 N1 C25 C23 176.22(18) . . . 2_666 ? C19 N1 C26 C27 -95.2(2) . . . . ? C25 N1 C26 C27 85.8(2) . . . . ? N1 C26 C27 C28 -169.2(2) . . . . ? C26 C27 C28 C29 -178.8(2) . . . . ? C27 C28 C29 C30 -169.4(2) . . . . ? C28 C29 C30 C31 -179.1(3) . . . . ? #============================================================================== data_[Li2.2.A](CF3SO3)2 _database_code_depnum_ccdc_archive 'CCDC 644505' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H74 F12 Li4 N2 O26 S4, 2(C H Cl3)' _chemical_formula_sum 'C68 H76 Cl6 F12 Li4 N2 O26 S4' _chemical_formula_weight 1934.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.413(6) _cell_length_b 12.236(5) _cell_length_c 16.274(5) _cell_angle_alpha 98.19(3) _cell_angle_beta 105.66(2) _cell_angle_gamma 99.55(4) _cell_volume 2115.6(16) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19000 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.34 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.924 _exptl_absorpt_correction_T_max 0.992 _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 SHELXL. ; _exptl_special_details ; 1,2- and 1-3- distance restraints applied along the n-hexyl chain and within the ether chain. The displacement parameters, particularly within the ether chain are elongated. However, attempts to resolve two orientations did not significantly improve the model, and the elongated anisotropic description was retained. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6904 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 14812 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 24.26 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.26 _diffrn_measured_fraction_theta_full 0.982 _reflns_number_total 7350 _reflns_number_gt 5584 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1994)' _computing_cell_refinement 'SAINT (Bruker, 1994)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL v.6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1421P)^2^+7.6621P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7350 _refine_ls_number_parameters 552 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.1017 _refine_ls_wR_factor_ref 0.2897 _refine_ls_wR_factor_gt 0.2691 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.658 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.118 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.1175(8) 0.1987(7) 0.1915(5) 0.0309(18) Uani 1 1 d . . . Li2 Li 0.3686(9) 0.8785(7) 0.3893(6) 0.037(2) Uani 1 1 d . . . S1 S 0.16559(14) -0.03142(13) 0.25158(9) 0.0426(4) Uani 1 1 d . . . S2 S 0.36032(13) 0.97318(11) 0.58264(9) 0.0348(4) Uani 1 1 d . . . N1 N 0.2892(4) 0.5282(3) 0.3054(3) 0.0293(9) Uani 1 1 d . . . O1 O 0.2224(3) 0.3384(3) 0.2682(2) 0.0341(8) Uani 1 1 d . . . O2 O 0.3408(4) 0.7173(3) 0.3472(2) 0.0378(9) Uani 1 1 d . . . O3 O 0.0234(5) 0.3728(4) 0.3788(4) 0.0738(16) Uani 1 1 d D . . O4 O -0.0623(4) 0.2219(4) 0.2128(3) 0.0673(15) Uani 1 1 d D . . O5 O -0.0010(5) 0.1639(5) 0.0702(3) 0.0837(19) Uani 1 1 d D . . O6 O 0.2433(5) 0.1945(4) 0.1107(4) 0.0814(18) Uani 1 1 d D . . O7 O 0.4802(7) 0.3350(5) 0.1880(6) 0.117(3) Uani 1 1 d D . . O8 O 0.1510(5) 0.0832(4) 0.2554(4) 0.0703(15) Uani 1 1 d . . . O9 O 0.2632(4) -0.0411(4) 0.3239(3) 0.0593(12) Uani 1 1 d . . . O10 O 0.1649(6) -0.0870(8) 0.1700(4) 0.116(3) Uani 1 1 d . . . O11 O 0.3510(4) 0.9235(3) 0.6559(3) 0.0468(10) Uani 1 1 d . . . O12 O 0.4611(4) 1.0694(3) 0.6020(3) 0.0471(10) Uani 1 1 d . . . O13 O 0.3452(4) 0.8937(3) 0.5047(3) 0.0449(10) Uani 1 1 d . . . C1 C 0.3580(5) 0.6265(4) 0.3636(3) 0.0299(11) Uani 1 1 d . . . C2 C 0.4501(4) 0.6142(4) 0.4439(3) 0.0252(10) Uani 1 1 d . . . C3 C 0.4568(4) 0.5057(4) 0.4610(3) 0.0218(9) Uani 1 1 d . . . C4 C 0.3791(4) 0.4083(4) 0.4035(3) 0.0226(9) Uani 1 1 d . . . C5 C 0.2907(4) 0.4195(4) 0.3213(3) 0.0278(10) Uani 1 1 d . . . C6 C 0.3856(4) 0.3027(4) 0.4224(3) 0.0288(10) Uani 1 1 d . . . H6A H 0.3319 0.2373 0.3834 0.035 Uiso 1 1 calc R . . C7 C 0.5283(5) 0.7082(4) 0.5007(3) 0.0299(11) Uani 1 1 d . . . H7A H 0.5241 0.7811 0.4880 0.036 Uiso 1 1 calc R . . C8 C 0.2014(5) 0.5384(5) 0.2213(3) 0.0382(12) Uani 1 1 d D . . H8A H 0.2019 0.4767 0.1749 0.046 Uiso 1 1 calc R . . H8B H 0.2328 0.6109 0.2062 0.046 Uiso 1 1 calc R . . C9 C 0.0678(6) 0.5335(8) 0.2218(5) 0.072(2) Uani 1 1 d D . . H9A H 0.0361 0.4618 0.2379 0.086 Uiso 1 1 calc R . . H9B H 0.0660 0.5966 0.2666 0.086 Uiso 1 1 calc R . . C10 C -0.0153(6) 0.5411(8) 0.1357(5) 0.084(3) Uani 1 1 d D . . H10A H 0.0109 0.6170 0.1236 0.101 Uiso 1 1 calc R . . H10B H -0.0035 0.4848 0.0902 0.101 Uiso 1 1 calc R . . C11 C -0.1493(6) 0.5221(9) 0.1283(7) 0.126(5) Uani 1 1 d D . . H11A H -0.1644 0.5851 0.1668 0.151 Uiso 1 1 calc R . . H11B H -0.1742 0.4513 0.1479 0.151 Uiso 1 1 calc R . . C12 C -0.2283(9) 0.5142(13) 0.0352(8) 0.164(8) Uani 1 1 d D . . H12A H -0.2133 0.5890 0.0188 0.197 Uiso 1 1 calc R . . H12B H -0.2036 0.4598 -0.0045 0.197 Uiso 1 1 calc R . . C13 C -0.3604(11) 0.478(2) 0.0253(10) 0.32(2) Uani 1 1 d D . . H13A H -0.4089 0.4729 -0.0353 0.478 Uiso 1 1 calc R . . H13B H -0.3855 0.5327 0.0636 0.478 Uiso 1 1 calc R . . H13C H -0.3756 0.4035 0.0410 0.478 Uiso 1 1 calc R . . C14 C 0.1289(7) 0.5515(5) 0.4609(6) 0.065(2) Uani 1 1 d . . . H14A H 0.0828 0.5824 0.4154 0.079 Uiso 1 1 calc R . . C15 C 0.2131(7) 0.6203(5) 0.5308(6) 0.066(2) Uani 1 1 d . . . H15A H 0.2277 0.6995 0.5332 0.079 Uiso 1 1 calc R . . C16 C 0.2805(7) 0.5781(5) 0.6008(6) 0.063(2) Uani 1 1 d . . . C17 C 0.3671(7) 0.6489(6) 0.6723(7) 0.074(3) Uani 1 1 d . . . H17A H 0.3814 0.7284 0.6759 0.089 Uiso 1 1 calc R . . C18 C 0.4321(9) 0.6050(7) 0.7379(8) 0.086(3) Uani 1 1 d . . . C19 C 0.4103(10) 0.4848(7) 0.7341(7) 0.083(3) Uani 1 1 d . . . H19A H 0.4546 0.4551 0.7811 0.100 Uiso 1 1 calc R . . C20 C 0.3288(9) 0.4161(6) 0.6653(6) 0.076(3) Uani 1 1 d . . . H20A H 0.3167 0.3368 0.6626 0.091 Uiso 1 1 calc R . . C21 C 0.2581(7) 0.4581(5) 0.5946(6) 0.063(2) Uani 1 1 d . . . C22 C 0.1708(8) 0.3873(5) 0.5202(6) 0.065(2) Uani 1 1 d . . . H22A H 0.1555 0.3076 0.5157 0.078 Uiso 1 1 calc R . . C23 C 0.1083(8) 0.4326(5) 0.4547(6) 0.065(2) Uani 1 1 d . . . C24 C -0.0028(8) 0.2524(5) 0.3681(5) 0.080(3) Uani 1 1 d D . . H24A H -0.0283 0.2298 0.4179 0.096 Uiso 1 1 calc R . . H24B H 0.0726 0.2235 0.3661 0.096 Uiso 1 1 calc R . . C25 C -0.1049(7) 0.2044(7) 0.2856(6) 0.097(4) Uani 1 1 d D . . H25A H -0.1337 0.1224 0.2819 0.117 Uiso 1 1 calc R . . H25B H -0.1761 0.2411 0.2849 0.117 Uiso 1 1 calc R . . C26 C -0.1602(6) 0.1756(7) 0.1325(6) 0.106(4) Uani 1 1 d D . . H26A H -0.2343 0.2077 0.1325 0.127 Uiso 1 1 calc R . . H26B H -0.1844 0.0924 0.1253 0.127 Uiso 1 1 calc R . . C27 C -0.1121(8) 0.2052(8) 0.0612(6) 0.133(6) Uani 1 1 d D . . H27A H -0.1739 0.1696 0.0040 0.160 Uiso 1 1 calc R . . H27B H -0.0944 0.2881 0.0655 0.160 Uiso 1 1 calc R . . C28 C 0.0573(9) 0.1900(12) 0.0069(5) 0.178(10) Uani 1 1 d D . . H28A H 0.0792 0.2729 0.0118 0.214 Uiso 1 1 calc R . . H28B H 0.0005 0.1559 -0.0523 0.214 Uiso 1 1 calc R . . C29 C 0.1693(10) 0.1439(10) 0.0229(6) 0.167(9) Uani 1 1 d D . . H29A H 0.1475 0.0607 0.0158 0.201 Uiso 1 1 calc R . . H29B H 0.2156 0.1628 -0.0185 0.201 Uiso 1 1 calc R . . C30 C 0.3520(8) 0.1547(9) 0.1218(10) 0.192(10) Uani 1 1 d D . . H30A H 0.3772 0.1554 0.0682 0.231 Uiso 1 1 calc R . . H30B H 0.3344 0.0751 0.1288 0.231 Uiso 1 1 calc R . . C31 C 0.4575(14) 0.2189(8) 0.1966(12) 0.225(12) Uani 1 1 d D . . H31A H 0.4375 0.2130 0.2516 0.270 Uiso 1 1 calc R . . H31B H 0.5326 0.1879 0.1980 0.270 Uiso 1 1 calc R . . C32 C 0.0276(8) -0.0991(7) 0.2709(7) 0.085(3) Uani 1 1 d . . . C33 C 0.2250(6) 1.0359(5) 0.5562(4) 0.0424(13) Uani 1 1 d . . . C34 C 0.5466(8) 0.8710(7) 0.1691(4) 0.0625(19) Uani 1 1 d . . . H34A H 0.5897 0.9220 0.2270 0.075 Uiso 1 1 calc R . . F1 F 0.0275(10) -0.2022(6) 0.2724(11) 0.266(8) Uani 1 1 d . . . F2 F -0.0740(5) -0.0932(8) 0.2066(5) 0.150(3) Uani 1 1 d . . . F3 F 0.0123(5) -0.0493(7) 0.3408(4) 0.116(2) Uani 1 1 d . . . F4 F 0.2248(4) 1.1086(3) 0.6250(3) 0.0665(11) Uani 1 1 d . . . F5 F 0.1211(3) 0.9578(3) 0.5327(3) 0.0607(10) Uani 1 1 d . . . F6 F 0.2229(3) 1.0920(3) 0.4918(3) 0.0558(10) Uani 1 1 d . . . Cl1 Cl 0.6314(3) 0.7679(2) 0.1576(2) 0.1001(8) Uani 1 1 d . . . Cl2 Cl 0.5509(4) 0.9523(2) 0.08906(19) 0.1206(12) Uani 1 1 d . . . Cl3 Cl 0.4006(3) 0.8230(4) 0.1660(2) 0.1457(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.035(4) 0.028(4) 0.023(4) 0.003(3) -0.002(3) 0.008(3) Li2 0.041(5) 0.032(4) 0.041(5) 0.013(4) 0.009(4) 0.013(4) S1 0.0393(8) 0.0461(8) 0.0360(8) 0.0027(6) 0.0005(6) 0.0140(6) S2 0.0430(8) 0.0285(6) 0.0390(7) 0.0132(5) 0.0163(6) 0.0127(6) N1 0.030(2) 0.031(2) 0.024(2) 0.0051(16) 0.0015(17) 0.0095(17) O1 0.0304(18) 0.0336(19) 0.0285(18) -0.0045(15) -0.0009(15) 0.0052(15) O2 0.048(2) 0.0294(19) 0.0334(19) 0.0116(15) 0.0024(16) 0.0124(16) O3 0.091(4) 0.039(2) 0.112(5) 0.004(3) 0.068(4) 0.017(3) O4 0.034(2) 0.044(3) 0.108(4) 0.000(3) 0.003(3) 0.012(2) O5 0.096(4) 0.072(4) 0.045(3) 0.012(2) -0.021(3) -0.016(3) O6 0.102(4) 0.045(3) 0.106(5) -0.006(3) 0.062(4) 0.008(3) O7 0.108(5) 0.057(4) 0.167(8) -0.001(4) 0.019(5) 0.024(4) O8 0.066(3) 0.066(3) 0.099(4) 0.051(3) 0.027(3) 0.036(3) O9 0.054(3) 0.072(3) 0.055(3) 0.030(2) 0.003(2) 0.030(2) O10 0.066(4) 0.183(7) 0.066(4) -0.057(4) 0.006(3) 0.026(4) O11 0.069(3) 0.041(2) 0.041(2) 0.0191(18) 0.025(2) 0.018(2) O12 0.041(2) 0.038(2) 0.065(3) 0.0201(19) 0.013(2) 0.0088(18) O13 0.065(3) 0.036(2) 0.042(2) 0.0137(17) 0.021(2) 0.0223(19) C1 0.032(3) 0.030(3) 0.027(2) 0.007(2) 0.006(2) 0.008(2) C2 0.027(2) 0.025(2) 0.025(2) 0.0058(18) 0.0074(19) 0.0072(19) C3 0.023(2) 0.023(2) 0.020(2) 0.0031(17) 0.0084(18) 0.0063(18) C4 0.022(2) 0.024(2) 0.021(2) 0.0033(17) 0.0056(17) 0.0053(18) C5 0.025(2) 0.031(2) 0.027(2) 0.003(2) 0.007(2) 0.007(2) C6 0.027(2) 0.024(2) 0.032(3) 0.0011(19) 0.007(2) 0.0017(19) C7 0.033(3) 0.024(2) 0.033(3) 0.010(2) 0.007(2) 0.007(2) C8 0.044(3) 0.041(3) 0.022(2) 0.006(2) -0.004(2) 0.013(2) C9 0.067(5) 0.077(5) 0.062(5) 0.010(4) 0.000(4) 0.024(4) C10 0.083(6) 0.082(6) 0.075(6) 0.023(5) -0.005(5) 0.022(5) C11 0.066(6) 0.076(6) 0.179(12) 0.033(7) -0.059(7) 0.012(5) C12 0.080(8) 0.160(13) 0.213(16) 0.115(12) -0.040(9) -0.008(8) C13 0.38(4) 0.22(2) 0.163(18) 0.012(16) -0.17(2) -0.02(2) C14 0.060(4) 0.036(3) 0.126(7) 0.016(4) 0.063(5) 0.020(3) C15 0.056(4) 0.030(3) 0.137(7) 0.023(4) 0.064(5) 0.017(3) C16 0.060(4) 0.027(3) 0.126(7) 0.013(4) 0.067(5) 0.010(3) C17 0.062(5) 0.029(3) 0.156(9) 0.024(5) 0.065(5) 0.019(3) C18 0.087(6) 0.044(4) 0.137(9) -0.001(5) 0.060(6) 0.012(4) C19 0.115(7) 0.049(4) 0.113(7) 0.025(5) 0.070(6) 0.024(5) C20 0.123(7) 0.033(3) 0.096(6) 0.013(4) 0.074(6) 0.012(4) C21 0.081(5) 0.029(3) 0.109(6) 0.015(4) 0.077(5) 0.014(3) C22 0.093(6) 0.026(3) 0.105(6) 0.009(4) 0.079(5) 0.012(3) C23 0.073(5) 0.033(3) 0.113(7) 0.008(4) 0.070(5) 0.011(3) C24 0.103(7) 0.038(4) 0.120(7) 0.002(4) 0.082(6) 0.005(4) C25 0.060(5) 0.052(5) 0.183(11) -0.014(6) 0.067(7) 0.002(4) C26 0.041(4) 0.055(5) 0.172(11) -0.012(6) -0.037(6) 0.018(4) C27 0.124(10) 0.059(5) 0.131(10) 0.018(6) -0.090(8) -0.003(6) C28 0.196(15) 0.236(18) 0.023(4) 0.018(7) -0.002(7) -0.111(14) C29 0.226(17) 0.128(10) 0.114(10) -0.078(9) 0.122(12) -0.087(12) C30 0.152(13) 0.094(9) 0.44(3) 0.108(14) 0.210(18) 0.075(9) C31 0.220(19) 0.068(8) 0.30(2) -0.018(11) -0.069(18) 0.080(10) C32 0.065(5) 0.060(5) 0.116(8) -0.002(5) 0.029(5) -0.015(4) C33 0.047(3) 0.033(3) 0.055(3) 0.014(3) 0.022(3) 0.013(3) C34 0.080(5) 0.068(4) 0.042(4) 0.010(3) 0.020(3) 0.024(4) F1 0.206(10) 0.066(4) 0.57(2) 0.071(8) 0.213(13) -0.011(5) F2 0.048(3) 0.221(8) 0.120(5) -0.062(5) 0.003(3) -0.020(4) F3 0.067(3) 0.190(7) 0.085(4) 0.024(4) 0.035(3) -0.009(4) F4 0.075(3) 0.055(2) 0.080(3) 0.002(2) 0.038(2) 0.029(2) F5 0.0391(19) 0.056(2) 0.086(3) 0.022(2) 0.0162(19) 0.0036(17) F6 0.055(2) 0.048(2) 0.074(3) 0.0320(19) 0.0178(19) 0.0220(17) Cl1 0.0949(17) 0.1044(18) 0.120(2) 0.0381(16) 0.0349(15) 0.0557(15) Cl2 0.227(4) 0.0897(17) 0.0949(18) 0.0485(15) 0.088(2) 0.078(2) Cl3 0.0723(16) 0.269(5) 0.111(2) 0.054(3) 0.0508(16) 0.026(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O8 1.899(9) . ? Li1 O1 1.955(9) . ? Li1 O5 2.010(9) . ? Li1 O6 2.195(10) . ? Li1 O4 2.227(10) . ? Li2 O9 1.883(10) 1_565 ? Li2 O12 1.903(10) 2_676 ? Li2 O2 1.937(10) . ? Li2 O13 1.955(10) . ? S1 O10 1.400(6) . ? S1 O9 1.420(4) . ? S1 O8 1.435(5) . ? S1 C32 1.782(9) . ? S2 O11 1.433(4) . ? S2 O12 1.434(4) . ? S2 O13 1.435(4) . ? S2 C33 1.813(6) . ? N1 C1 1.386(6) . ? N1 C5 1.392(6) . ? N1 C8 1.498(6) . ? O1 C5 1.213(6) . ? O2 C1 1.214(6) . ? O3 C23 1.364(10) . ? O3 C24 1.430(7) . ? O4 C25 1.427(8) . ? O4 C26 1.437(7) . ? O5 C28 1.413(8) . ? O5 C27 1.421(8) . ? O6 C30 1.383(8) . ? O6 C29 1.436(8) . ? O7 C18 1.360(12) 2_666 ? O7 C31 1.435(10) . ? O9 Li2 1.883(10) 1_545 ? O12 Li2 1.903(10) 2_676 ? C1 C2 1.484(7) . ? C2 C7 1.373(7) . ? C2 C3 1.404(6) . ? C3 C4 1.402(6) . ? C3 C3 1.422(9) 2_666 ? C4 C6 1.379(7) . ? C4 C5 1.482(6) . ? C6 C7 1.406(7) 2_666 ? C6 H6A 0.950 . ? C7 C6 1.406(7) 2_666 ? C7 H7A 0.950 . ? C8 C9 1.518(7) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.491(7) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C10 C11 1.477(8) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 C12 1.519(9) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.456(10) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 C15 1.340(12) . ? C14 C23 1.419(9) . ? C14 H14A 0.950 . ? C15 C16 1.407(12) . ? C15 H15A 0.950 . ? C16 C17 1.375(12) . ? C16 C21 1.432(8) . ? C17 C18 1.359(14) . ? C17 H17A 0.950 . ? C18 O7 1.360(12) 2_666 ? C18 C19 1.440(11) . ? C19 C20 1.318(13) . ? C19 H19A 0.950 . ? C20 C21 1.429(13) . ? C20 H20A 0.950 . ? C21 C22 1.405(12) . ? C22 C23 1.356(12) . ? C22 H22A 0.950 . ? C24 C25 1.486(8) . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.476(9) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 C29 1.457(10) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 C31 1.473(5) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 F1 1.266(12) . ? C32 F3 1.281(11) . ? C32 F2 1.356(13) . ? C33 F5 1.319(7) . ? C33 F4 1.329(7) . ? C33 F6 1.330(7) . ? C34 Cl3 1.657(9) . ? C34 Cl1 1.732(8) . ? C34 Cl2 1.753(8) . ? C34 H34A 1.000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Li1 O1 104.9(4) . . ? O8 Li1 O5 121.8(5) . . ? O1 Li1 O5 133.3(5) . . ? O8 Li1 O6 102.9(4) . . ? O1 Li1 O6 91.8(4) . . ? O5 Li1 O6 77.4(4) . . ? O8 Li1 O4 100.3(4) . . ? O1 Li1 O4 97.5(4) . . ? O5 Li1 O4 76.8(4) . . ? O6 Li1 O4 151.8(4) . . ? O9 Li2 O12 112.5(5) 1_565 2_676 ? O9 Li2 O2 117.6(5) 1_565 . ? O12 Li2 O2 103.0(5) 2_676 . ? O9 Li2 O13 107.6(5) 1_565 . ? O12 Li2 O13 110.7(5) 2_676 . ? O2 Li2 O13 105.2(4) . . ? O10 S1 O9 116.1(4) . . ? O10 S1 O8 114.7(5) . . ? O9 S1 O8 111.3(3) . . ? O10 S1 C32 106.6(5) . . ? O9 S1 C32 104.0(4) . . ? O8 S1 C32 102.5(4) . . ? O11 S2 O12 114.7(3) . . ? O11 S2 O13 114.8(2) . . ? O12 S2 O13 114.7(3) . . ? O11 S2 C33 104.3(3) . . ? O12 S2 C33 102.2(3) . . ? O13 S2 C33 104.0(3) . . ? C1 N1 C5 124.6(4) . . ? C1 N1 C8 118.3(4) . . ? C5 N1 C8 117.0(4) . . ? C5 O1 Li1 174.2(4) . . ? C1 O2 Li2 147.3(4) . . ? C23 O3 C24 117.0(7) . . ? C25 O4 C26 110.8(6) . . ? C25 O4 Li1 128.1(5) . . ? C26 O4 Li1 108.3(5) . . ? C28 O5 C27 112.4(7) . . ? C28 O5 Li1 113.3(5) . . ? C27 O5 Li1 115.2(5) . . ? C30 O6 C29 104.8(7) . . ? C30 O6 Li1 130.6(7) . . ? C29 O6 Li1 107.9(5) . . ? C18 O7 C31 107.6(9) 2_666 . ? S1 O8 Li1 146.2(5) . . ? S1 O9 Li2 153.6(5) . 1_545 ? S2 O12 Li2 146.2(4) . 2_676 ? S2 O13 Li2 143.9(4) . . ? O2 C1 N1 119.4(4) . . ? O2 C1 C2 123.3(4) . . ? N1 C1 C2 117.3(4) . . ? C7 C2 C3 120.4(4) . . ? C7 C2 C1 120.1(4) . . ? C3 C2 C1 119.4(4) . . ? C4 C3 C2 121.5(4) . . ? C4 C3 C3 119.2(5) . 2_666 ? C2 C3 C3 119.3(5) . 2_666 ? C6 C4 C3 120.5(4) . . ? C6 C4 C5 120.0(4) . . ? C3 C4 C5 119.4(4) . . ? O1 C5 N1 120.0(4) . . ? O1 C5 C4 122.6(4) . . ? N1 C5 C4 117.4(4) . . ? C4 C6 C7 120.1(4) . 2_666 ? C4 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 2_666 . ? C2 C7 C6 120.4(4) . 2_666 ? C2 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 2_666 . ? N1 C8 C9 114.9(5) . . ? N1 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 112.2(6) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 115.0(7) . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10B 108.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C10 C11 C12 111.4(8) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C11 111.3(9) . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12B 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C23 120.1(8) . . ? C15 C14 H14A 120.0 . . ? C23 C14 H14A 120.0 . . ? C14 C15 C16 121.7(6) . . ? C14 C15 H15A 119.1 . . ? C16 C15 H15A 119.1 . . ? C17 C16 C15 121.6(6) . . ? C17 C16 C21 120.6(8) . . ? C15 C16 C21 117.9(8) . . ? C18 C17 C16 119.9(7) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 O7 126.0(8) . 2_666 ? C17 C18 C19 120.8(10) . . ? O7 C18 C19 113.2(10) 2_666 . ? C20 C19 C18 119.8(10) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 121.5(7) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C22 C21 C20 123.0(6) . . ? C22 C21 C16 119.5(8) . . ? C20 C21 C16 117.4(8) . . ? C23 C22 C21 120.1(6) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 O3 125.5(6) . . ? C22 C23 C14 120.7(8) . . ? O3 C23 C14 113.8(8) . . ? O3 C24 C25 108.5(7) . . ? O3 C24 H24A 110.0 . . ? C25 C24 H24A 110.0 . . ? O3 C24 H24B 110.0 . . ? C25 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? O4 C25 C24 110.2(6) . . ? O4 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? O4 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? O4 C26 C27 107.4(6) . . ? O4 C26 H26A 110.2 . . ? C27 C26 H26A 110.2 . . ? O4 C26 H26B 110.2 . . ? C27 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? O5 C27 C26 106.6(6) . . ? O5 C27 H27A 110.4 . . ? C26 C27 H27A 110.4 . . ? O5 C27 H27B 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? O5 C28 C29 107.3(8) . . ? O5 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? O5 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.5 . . ? O6 C29 C28 106.3(7) . . ? O6 C29 H29A 110.5 . . ? C28 C29 H29A 110.5 . . ? O6 C29 H29B 110.5 . . ? C28 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? O6 C30 C31 115.1(10) . . ? O6 C30 H30A 108.5 . . ? C31 C30 H30A 108.5 . . ? O6 C30 H30B 108.5 . . ? C31 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? O7 C31 C30 108.5(9) . . ? O7 C31 H31A 110.0 . . ? C30 C31 H31A 110.0 . . ? O7 C31 H31B 110.0 . . ? C30 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? F1 C32 F3 110.7(12) . . ? F1 C32 F2 108.3(10) . . ? F3 C32 F2 104.7(8) . . ? F1 C32 S1 110.6(8) . . ? F3 C32 S1 112.4(6) . . ? F2 C32 S1 109.9(8) . . ? F5 C33 F4 108.0(5) . . ? F5 C33 F6 107.9(5) . . ? F4 C33 F6 107.4(5) . . ? F5 C33 S2 110.9(4) . . ? F4 C33 S2 110.2(4) . . ? F6 C33 S2 112.2(4) . . ? Cl3 C34 Cl1 115.0(5) . . ? Cl3 C34 Cl2 110.3(5) . . ? Cl1 C34 Cl2 108.8(4) . . ? Cl3 C34 H34A 107.5 . . ? Cl1 C34 H34A 107.5 . . ? Cl2 C34 H34A 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Li2 O2 C1 -161.7(7) 1_565 . . . ? O12 Li2 O2 C1 73.9(10) 2_676 . . . ? O13 Li2 O2 C1 -42.1(10) . . . . ? O8 Li1 O4 C25 29.1(7) . . . . ? O1 Li1 O4 C25 -77.6(6) . . . . ? O5 Li1 O4 C25 149.6(5) . . . . ? O6 Li1 O4 C25 174.1(8) . . . . ? O8 Li1 O4 C26 -108.0(6) . . . . ? O1 Li1 O4 C26 145.3(5) . . . . ? O5 Li1 O4 C26 12.5(6) . . . . ? O6 Li1 O4 C26 37.0(11) . . . . ? O8 Li1 O5 C28 -115.7(9) . . . . ? O1 Li1 O5 C28 62.4(10) . . . . ? O6 Li1 O5 C28 -18.2(8) . . . . ? O4 Li1 O5 C28 150.3(8) . . . . ? O8 Li1 O5 C27 112.9(7) . . . . ? O1 Li1 O5 C27 -69.0(9) . . . . ? O6 Li1 O5 C27 -149.5(6) . . . . ? O4 Li1 O5 C27 18.9(6) . . . . ? O8 Li1 O6 C30 -22.6(8) . . . . ? O1 Li1 O6 C30 83.1(8) . . . . ? O5 Li1 O6 C30 -142.8(7) . . . . ? O4 Li1 O6 C30 -167.2(9) . . . . ? O8 Li1 O6 C29 106.5(7) . . . . ? O1 Li1 O6 C29 -147.8(6) . . . . ? O5 Li1 O6 C29 -13.7(7) . . . . ? O4 Li1 O6 C29 -38.1(12) . . . . ? O10 S1 O8 Li1 7.1(9) . . . . ? O9 S1 O8 Li1 141.4(7) . . . . ? C32 S1 O8 Li1 -107.9(8) . . . . ? O1 Li1 O8 S1 -143.9(6) . . . . ? O5 Li1 O8 S1 34.6(11) . . . . ? O6 Li1 O8 S1 -48.5(9) . . . . ? O4 Li1 O8 S1 115.3(7) . . . . ? O10 S1 O9 Li2 -43.2(12) . . . 1_545 ? O8 S1 O9 Li2 -176.8(10) . . . 1_545 ? C32 S1 O9 Li2 73.5(11) . . . 1_545 ? O11 S2 O12 Li2 89.6(7) . . . 2_676 ? O13 S2 O12 Li2 -46.4(8) . . . 2_676 ? C33 S2 O12 Li2 -158.3(7) . . . 2_676 ? O11 S2 O13 Li2 -165.5(6) . . . . ? O12 S2 O13 Li2 -29.5(7) . . . . ? C33 S2 O13 Li2 81.2(7) . . . . ? O9 Li2 O13 S2 -64.3(8) 1_565 . . . ? O12 Li2 O13 S2 59.0(8) 2_676 . . . ? O2 Li2 O13 S2 169.6(5) . . . . ? Li2 O2 C1 N1 167.0(7) . . . . ? Li2 O2 C1 C2 -13.0(11) . . . . ? C5 N1 C1 O2 -172.6(5) . . . . ? C8 N1 C1 O2 3.9(7) . . . . ? C5 N1 C1 C2 7.4(7) . . . . ? C8 N1 C1 C2 -176.2(4) . . . . ? O2 C1 C2 C7 -5.3(8) . . . . ? N1 C1 C2 C7 174.7(4) . . . . ? O2 C1 C2 C3 174.8(5) . . . . ? N1 C1 C2 C3 -5.1(7) . . . . ? C7 C2 C3 C4 -179.2(4) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C7 C2 C3 C3 1.5(8) . . . 2_666 ? C1 C2 C3 C3 -178.6(5) . . . 2_666 ? C2 C3 C4 C6 -178.8(4) . . . . ? C3 C3 C4 C6 0.5(8) 2_666 . . . ? C2 C3 C4 C5 2.0(7) . . . . ? C3 C3 C4 C5 -178.7(5) 2_666 . . . ? C1 N1 C5 O1 176.2(5) . . . . ? C8 N1 C5 O1 -0.3(7) . . . . ? C1 N1 C5 C4 -4.8(7) . . . . ? C8 N1 C5 C4 178.7(4) . . . . ? C6 C4 C5 O1 -0.4(7) . . . . ? C3 C4 C5 O1 178.8(4) . . . . ? C6 C4 C5 N1 -179.4(4) . . . . ? C3 C4 C5 N1 -0.2(6) . . . . ? C3 C4 C6 C7 -0.8(7) . . . 2_666 ? C5 C4 C6 C7 178.4(4) . . . 2_666 ? C3 C2 C7 C6 -1.2(7) . . . 2_666 ? C1 C2 C7 C6 178.9(5) . . . 2_666 ? C1 N1 C8 C9 -94.6(6) . . . . ? C5 N1 C8 C9 82.2(6) . . . . ? N1 C8 C9 C10 -178.5(6) . . . . ? C8 C9 C10 C11 172.4(8) . . . . ? C9 C10 C11 C12 -171.6(9) . . . . ? C10 C11 C12 C13 171.0(14) . . . . ? C23 C14 C15 C16 -1.9(10) . . . . ? C14 C15 C16 C17 179.9(6) . . . . ? C14 C15 C16 C21 1.1(9) . . . . ? C15 C16 C17 C18 -178.8(7) . . . . ? C21 C16 C17 C18 0.0(10) . . . . ? C16 C17 C18 O7 -179.9(8) . . . 2_666 ? C16 C17 C18 C19 -0.9(12) . . . . ? C17 C18 C19 C20 1.8(13) . . . . ? O7 C18 C19 C20 -179.1(8) 2_666 . . . ? C18 C19 C20 C21 -1.8(13) . . . . ? C19 C20 C21 C22 179.7(7) . . . . ? C19 C20 C21 C16 0.9(11) . . . . ? C17 C16 C21 C22 -178.8(6) . . . . ? C15 C16 C21 C22 0.0(9) . . . . ? C17 C16 C21 C20 0.0(9) . . . . ? C15 C16 C21 C20 178.8(6) . . . . ? C20 C21 C22 C23 -178.8(6) . . . . ? C16 C21 C22 C23 -0.1(9) . . . . ? C21 C22 C23 O3 178.7(6) . . . . ? C21 C22 C23 C14 -0.8(9) . . . . ? C24 O3 C23 C22 0.8(9) . . . . ? C24 O3 C23 C14 -179.6(5) . . . . ? C15 C14 C23 C22 1.8(10) . . . . ? C15 C14 C23 O3 -177.8(6) . . . . ? C23 O3 C24 C25 175.0(6) . . . . ? C26 O4 C25 C24 179.9(6) . . . . ? Li1 O4 C25 C24 43.6(8) . . . . ? O3 C24 C25 O4 68.5(8) . . . . ? C25 O4 C26 C27 175.5(7) . . . . ? Li1 O4 C26 C27 -39.5(8) . . . . ? C28 O5 C27 C26 -178.1(7) . . . . ? Li1 O5 C27 C26 -46.3(8) . . . . ? O4 C26 C27 O5 55.4(9) . . . . ? C27 O5 C28 C29 179.9(8) . . . . ? Li1 O5 C28 C29 47.1(11) . . . . ? C30 O6 C29 C28 -176.3(9) . . . . ? Li1 O6 C29 C28 41.3(10) . . . . ? O5 C28 C29 O6 -57.8(12) . . . . ? C29 O6 C30 C31 162.9(12) . . . . ? Li1 O6 C30 C31 -66.9(14) . . . . ? C18 O7 C31 C30 173.2(12) 2_666 . . . ? O6 C30 C31 O7 -56.4(18) . . . . ? O10 S1 C32 F1 61.2(12) . . . . ? O9 S1 C32 F1 -61.9(11) . . . . ? O8 S1 C32 F1 -178.0(11) . . . . ? O10 S1 C32 F3 -174.5(8) . . . . ? O9 S1 C32 F3 62.4(9) . . . . ? O8 S1 C32 F3 -53.7(9) . . . . ? O10 S1 C32 F2 -58.3(8) . . . . ? O9 S1 C32 F2 178.6(6) . . . . ? O8 S1 C32 F2 62.5(7) . . . . ? O11 S2 C33 F5 -62.8(5) . . . . ? O12 S2 C33 F5 177.4(4) . . . . ? O13 S2 C33 F5 57.8(5) . . . . ? O11 S2 C33 F4 56.7(4) . . . . ? O12 S2 C33 F4 -63.0(4) . . . . ? O13 S2 C33 F4 177.4(4) . . . . ? O11 S2 C33 F6 176.4(4) . . . . ? O12 S2 C33 F6 56.6(5) . . . . ? O13 S2 C33 F6 -63.0(5) . . . . ? #============================================================================== data_[Na2.2.A]I2 _database_code_depnum_ccdc_archive 'CCDC 644506' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H74 I2 N2 Na2 O14, 8(C H Cl3)' _chemical_formula_sum 'C70 H82 Cl24 I2 N2 Na2 O14' _chemical_formula_weight 2325.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0338(3) _cell_length_b 13.4294(3) _cell_length_c 17.6513(4) _cell_angle_alpha 68.066(1) _cell_angle_beta 81.761(1) _cell_angle_gamma 86.115(1) _cell_volume 2400.87(10) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 56088 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 27.59 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 1.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 26869 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 5.13 _diffrn_reflns_theta_max 27.59 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _reflns_number_total 10852 _reflns_number_gt 8375 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_data_reduction Denzo/Scalepack _computing_structure_solution 'SHELXTL v6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+8.2595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10852 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1872 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.391 _refine_diff_density_min -1.264 _refine_diff_density_rms 0.113 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.6140(4) 0.1340(3) 0.8126(2) 0.0887(10) Uani 1 1 d . . . N1 N 0.5134(4) 0.2183(4) 0.5796(3) 0.0410(10) Uani 1 1 d . . . O1 O 0.5645(4) 0.2191(3) 0.6992(3) 0.0500(10) Uani 1 1 d . . . O2 O 0.4726(4) 0.2165(4) 0.4583(3) 0.0574(11) Uani 1 1 d . . . O3 O 0.2544(4) 0.2035(3) 0.7547(3) 0.0488(9) Uani 1 1 d . . . O4 O 0.4191(4) 0.0609(3) 0.8609(2) 0.0461(9) Uani 1 1 d . . . O5 O 0.6409(4) -0.0369(3) 0.8752(3) 0.0504(10) Uani 1 1 d . . . O6 O 0.8134(3) 0.1010(3) 0.7698(2) 0.0458(9) Uani 1 1 d . . . C11 C 0.2969(6) 0.2225(5) 0.8220(4) 0.0494(14) Uani 1 1 d . . . H11A H 0.2352 0.2654 0.8438 0.059 Uiso 1 1 calc R . . H11B H 0.3744 0.2626 0.8027 0.059 Uiso 1 1 calc R . . C12 C 0.3165(6) 0.1159(6) 0.8876(4) 0.0554(15) Uani 1 1 d . . . H12A H 0.3312 0.1262 0.9383 0.066 Uiso 1 1 calc R . . H12B H 0.2422 0.0721 0.9008 0.066 Uiso 1 1 calc R . . C13 C 0.4286(6) -0.0465(5) 0.9175(4) 0.0512(14) Uani 1 1 d . . . H13A H 0.3531 -0.0858 0.9230 0.061 Uiso 1 1 calc R . . H13B H 0.4391 -0.0469 0.9723 0.061 Uiso 1 1 calc R . . C14 C 0.5368(6) -0.0996(5) 0.8857(4) 0.0541(15) Uani 1 1 d . . . H14A H 0.5485 -0.1734 0.9254 0.065 Uiso 1 1 calc R . . H14B H 0.5241 -0.1036 0.8325 0.065 Uiso 1 1 calc R . . C15 C 0.7509(6) -0.0781(6) 0.8452(4) 0.0599(16) Uani 1 1 d . . . H15A H 0.7406 -0.0893 0.7941 0.072 Uiso 1 1 calc R . . H15B H 0.7729 -0.1479 0.8866 0.072 Uiso 1 1 calc R . . C16 C 0.8496(6) 0.0018(6) 0.8280(4) 0.0577(16) Uani 1 1 d . . . H16A H 0.8618 0.0109 0.8795 0.069 Uiso 1 1 calc R . . H16B H 0.9278 -0.0238 0.8058 0.069 Uiso 1 1 calc R . . C17 C 0.9124(6) 0.1753(6) 0.7413(4) 0.0542(15) Uani 1 1 d . . . H17A H 0.9837 0.1441 0.7164 0.065 Uiso 1 1 calc R . . H17B H 0.9373 0.1883 0.7885 0.065 Uiso 1 1 calc R . . C19 C 0.4895(5) 0.2684(5) 0.4987(4) 0.0439(12) Uani 1 1 d . . . C20 C 0.4840(4) 0.3875(4) 0.4651(3) 0.0378(11) Uani 1 1 d . . . C21 C 0.5036(4) 0.4425(4) 0.5163(3) 0.0346(10) Uani 1 1 d . . . C22 C 0.5297(4) 0.3888(4) 0.5972(3) 0.0363(11) Uani 1 1 d . . . C23 C 0.5383(5) 0.2700(5) 0.6303(4) 0.0418(12) Uani 1 1 d . . . C24 C 0.5477(5) 0.4457(5) 0.6455(3) 0.0429(12) Uani 1 1 d . . . H24A H 0.5659 0.4087 0.7002 0.051 Uiso 1 1 calc R . . C25 C 0.5391(5) 0.5578(5) 0.6141(3) 0.0424(12) Uani 1 1 d . . . H25A H 0.5495 0.5964 0.6481 0.051 Uiso 1 1 calc R . . C26 C 0.5191(6) 0.0995(5) 0.6129(4) 0.0548(15) Uani 1 1 d . . . H26A H 0.4604 0.0716 0.5884 0.066 Uiso 1 1 calc R . . H26B H 0.4953 0.0724 0.6732 0.066 Uiso 1 1 calc R . . C27 C 0.6489(6) 0.0588(5) 0.5934(5) 0.0613(17) Uani 1 1 d . . . H27A H 0.6738 0.0892 0.5332 0.074 Uiso 1 1 calc R . . H27B H 0.7067 0.0847 0.6198 0.074 Uiso 1 1 calc R . . C28 C 0.6577(7) -0.0612(6) 0.6228(5) 0.0640(17) Uani 1 1 d . . . H28A H 0.5980 -0.0872 0.5978 0.077 Uiso 1 1 calc R . . H28B H 0.6352 -0.0914 0.6832 0.077 Uiso 1 1 calc R . . C29 C 0.7840(7) -0.1019(7) 0.6017(6) 0.075(2) Uani 1 1 d . . . H29A H 0.7889 -0.1800 0.6338 0.090 Uiso 1 1 calc R . . H29B H 0.8447 -0.0666 0.6192 0.090 Uiso 1 1 calc R . . C30 C 0.8200(7) -0.0827(7) 0.5092(6) 0.076(2) Uani 1 1 d . . . H30A H 0.7588 -0.1157 0.4903 0.091 Uiso 1 1 calc R . . H30B H 0.8208 -0.0046 0.4765 0.091 Uiso 1 1 calc R . . C32 C 0.9450(7) -0.1309(7) 0.4959(7) 0.087(3) Uani 1 1 d . . . H32A H 0.9671 -0.1180 0.4373 0.131 Uiso 1 1 calc R . . H32B H 0.9436 -0.2084 0.5276 0.131 Uiso 1 1 calc R . . H32C H 1.0055 -0.0978 0.5144 0.131 Uiso 1 1 calc R . . C35 C 0.9207(6) 0.2618(8) 0.9725(5) 0.073(2) Uani 1 1 d . . . H35A H 0.8300 0.2682 0.9720 0.087 Uiso 1 1 calc R . . Cl7 Cl 0.9559(3) 0.2966(4) 1.0514(2) 0.1308(13) Uani 1 1 d . . . Cl8 Cl 0.9659(4) 0.1284(3) 0.9872(2) 0.1313(12) Uani 1 1 d . . . Cl9 Cl 0.9913(2) 0.3445(3) 0.87585(16) 0.1025(8) Uani 1 1 d . . . C36 C 0.7817(8) 0.5722(7) 0.7926(5) 0.074(2) Uani 1 1 d . . . H36A H 0.7633 0.4968 0.8308 0.089 Uiso 1 1 calc R . . Cl10 Cl 0.6433(3) 0.6467(2) 0.7820(2) 0.1076(8) Uani 1 1 d . . . Cl11 Cl 0.8795(3) 0.6255(3) 0.8346(2) 0.1402(13) Uani 1 1 d . . . Cl12 Cl 0.8510(4) 0.5696(2) 0.69866(15) 0.1324(13) Uani 1 1 d . . . C33 C 0.2217(7) 0.8395(6) 0.7421(5) 0.0677(19) Uani 1 1 d . . . H33A H 0.2276 0.7784 0.7956 0.081 Uiso 1 1 calc R . . C34 C 0.3707(7) 0.4935(6) 0.9094(4) 0.0627(17) Uani 1 1 d . . . H34A H 0.4564 0.4658 0.9026 0.075 Uiso 1 1 calc R . . Cl1 Cl 0.0834(2) 0.8326(3) 0.7096(2) 0.1186(11) Uani 1 1 d . . . Cl2 Cl 0.2326(2) 0.95983(18) 0.75741(15) 0.0808(6) Uani 1 1 d . . . Cl3 Cl 0.3426(2) 0.82688(18) 0.66899(14) 0.0840(6) Uani 1 1 d . . . Cl4 Cl 0.3235(3) 0.5509(2) 0.81312(16) 0.1161(10) Uani 1 1 d . . . Cl5 Cl 0.3710(2) 0.5846(2) 0.95841(17) 0.0915(7) Uani 1 1 d . . . Cl6 Cl 0.2764(3) 0.3824(3) 0.9712(2) 0.1244(11) Uani 1 1 d . . . I1 I 0.62503(4) 0.29274(3) 0.88487(2) 0.04746(14) Uani 1 1 d . . . O7 O 0.8580(4) 0.2619(3) 0.6058(2) 0.0467(9) Uani 1 1 d . . . C1 C 0.7747(5) 0.6037(5) 0.3154(3) 0.0412(12) Uani 1 1 d . . . H1A H 0.7610 0.5889 0.2687 0.049 Uiso 1 1 calc R . . C2 C 0.7705(5) 0.7074(5) 0.3119(4) 0.0416(12) Uani 1 1 d . . . C3 C 0.7925(5) 0.7301(5) 0.3812(4) 0.0415(12) Uani 1 1 d . . . H3A H 0.7899 0.8021 0.3785 0.050 Uiso 1 1 calc R . . C4 C 0.8171(5) 0.6489(5) 0.4511(3) 0.0430(12) Uani 1 1 d . . . H4A H 0.8325 0.6656 0.4966 0.052 Uiso 1 1 calc R . . C5 C 0.8416(5) 0.4550(5) 0.5319(3) 0.0406(12) Uani 1 1 d . . . H5A H 0.8567 0.4702 0.5780 0.049 Uiso 1 1 calc R . . C6 C 0.8405(5) 0.3507(5) 0.5376(3) 0.0397(11) Uani 1 1 d . . . C7 C 0.8203(5) 0.3284(5) 0.4681(4) 0.0435(12) Uani 1 1 d . . . H7A H 0.8204 0.2560 0.4717 0.052 Uiso 1 1 calc R . . C8 C 0.8006(5) 0.4094(5) 0.3961(4) 0.0422(12) Uani 1 1 d . . . H8A H 0.7874 0.3923 0.3504 0.051 Uiso 1 1 calc R . . C9 C 0.7994(4) 0.5188(4) 0.3880(3) 0.0365(11) Uani 1 1 d . . . C10 C 0.8206(4) 0.5399(4) 0.4586(3) 0.0358(10) Uani 1 1 d . . . C18 C 0.8753(5) 0.2796(5) 0.6788(3) 0.0468(13) Uani 1 1 d . . . H18A H 0.7983 0.3071 0.7009 0.056 Uiso 1 1 calc R . . H18B H 0.9397 0.3335 0.6657 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.097(2) 0.082(2) 0.080(2) -0.0212(18) -0.0153(19) 0.0014(18) N1 0.037(2) 0.039(2) 0.051(3) -0.021(2) -0.0022(19) -0.0022(18) O1 0.052(2) 0.052(2) 0.042(2) -0.0137(19) -0.0037(18) -0.0033(19) O2 0.069(3) 0.052(2) 0.068(3) -0.037(2) -0.018(2) -0.001(2) O3 0.049(2) 0.049(2) 0.053(2) -0.0207(19) -0.0200(19) 0.0041(18) O4 0.044(2) 0.050(2) 0.040(2) -0.0107(18) -0.0063(16) -0.0006(17) O5 0.046(2) 0.057(3) 0.046(2) -0.0164(19) -0.0050(17) -0.0043(18) O6 0.040(2) 0.049(2) 0.040(2) -0.0079(17) -0.0036(16) -0.0027(17) C11 0.043(3) 0.062(4) 0.049(3) -0.026(3) -0.012(2) 0.007(3) C12 0.050(3) 0.073(4) 0.042(3) -0.020(3) -0.007(3) 0.006(3) C13 0.051(3) 0.054(4) 0.041(3) -0.007(3) -0.009(3) -0.005(3) C14 0.056(4) 0.047(3) 0.054(4) -0.010(3) -0.009(3) -0.010(3) C15 0.056(4) 0.054(4) 0.058(4) -0.008(3) -0.010(3) 0.007(3) C16 0.043(3) 0.066(4) 0.054(4) -0.010(3) -0.008(3) 0.002(3) C17 0.047(3) 0.066(4) 0.045(3) -0.012(3) -0.007(3) -0.009(3) C19 0.037(3) 0.052(3) 0.051(3) -0.029(3) -0.003(2) -0.004(2) C20 0.029(2) 0.045(3) 0.046(3) -0.025(2) -0.002(2) -0.003(2) C21 0.022(2) 0.048(3) 0.041(3) -0.026(2) -0.0008(18) -0.0028(19) C22 0.028(2) 0.046(3) 0.036(3) -0.018(2) 0.0007(19) -0.002(2) C23 0.030(2) 0.051(3) 0.048(3) -0.025(3) 0.001(2) -0.003(2) C24 0.039(3) 0.056(3) 0.039(3) -0.024(3) -0.007(2) 0.001(2) C25 0.043(3) 0.052(3) 0.042(3) -0.027(3) -0.008(2) -0.004(2) C26 0.061(4) 0.043(3) 0.065(4) -0.023(3) -0.011(3) -0.011(3) C27 0.053(4) 0.050(4) 0.088(5) -0.032(4) -0.019(3) 0.003(3) C28 0.062(4) 0.057(4) 0.072(5) -0.024(4) -0.002(3) -0.009(3) C29 0.067(5) 0.063(5) 0.107(7) -0.043(5) -0.014(4) 0.003(4) C30 0.048(4) 0.090(6) 0.117(7) -0.070(5) -0.013(4) 0.005(4) C32 0.050(4) 0.088(6) 0.155(9) -0.087(6) 0.003(5) -0.004(4) C35 0.040(3) 0.114(7) 0.064(4) -0.031(4) -0.009(3) -0.005(4) Cl7 0.0774(15) 0.246(4) 0.109(2) -0.108(3) -0.0091(14) -0.026(2) Cl8 0.146(3) 0.115(2) 0.129(3) -0.031(2) -0.059(2) 0.036(2) Cl9 0.0609(12) 0.138(2) 0.0842(15) -0.0132(15) -0.0053(11) -0.0084(13) C36 0.094(6) 0.064(5) 0.064(4) -0.018(4) -0.009(4) -0.030(4) Cl10 0.115(2) 0.0894(17) 0.122(2) -0.0416(16) -0.0181(17) -0.0016(15) Cl11 0.129(2) 0.190(4) 0.155(3) -0.115(3) -0.023(2) -0.049(2) Cl12 0.237(4) 0.0986(19) 0.0605(13) -0.0378(13) -0.0084(18) 0.031(2) C33 0.068(4) 0.065(4) 0.062(4) -0.018(4) 0.007(3) -0.015(4) C34 0.060(4) 0.079(5) 0.054(4) -0.030(4) -0.011(3) 0.003(3) Cl1 0.0788(15) 0.182(3) 0.121(2) -0.084(2) 0.0076(14) -0.0554(17) Cl2 0.0821(13) 0.0824(13) 0.0913(14) -0.0472(12) -0.0072(11) -0.0099(10) Cl3 0.0835(14) 0.0749(13) 0.0849(14) -0.0296(11) 0.0212(11) -0.0106(10) Cl4 0.182(3) 0.1071(19) 0.0772(15) -0.0405(14) -0.0686(18) 0.0260(19) Cl5 0.0795(13) 0.1241(19) 0.1106(17) -0.0847(16) -0.0333(12) 0.0203(13) Cl6 0.109(2) 0.135(3) 0.116(2) -0.040(2) 0.0270(17) -0.0398(18) I1 0.0499(2) 0.0558(2) 0.0371(2) -0.01431(16) -0.01115(15) -0.00852(16) O7 0.053(2) 0.049(2) 0.038(2) -0.0159(18) -0.0011(17) -0.0064(18) C1 0.035(3) 0.050(3) 0.045(3) -0.025(3) -0.006(2) 0.000(2) C2 0.030(2) 0.049(3) 0.050(3) -0.022(3) -0.007(2) -0.003(2) C3 0.033(3) 0.046(3) 0.049(3) -0.021(3) -0.003(2) -0.006(2) C4 0.038(3) 0.057(3) 0.043(3) -0.028(3) -0.001(2) -0.009(2) C5 0.032(2) 0.057(3) 0.038(3) -0.026(3) 0.002(2) -0.011(2) C6 0.030(2) 0.049(3) 0.040(3) -0.018(2) 0.003(2) -0.005(2) C7 0.039(3) 0.048(3) 0.050(3) -0.025(3) -0.006(2) -0.001(2) C8 0.039(3) 0.049(3) 0.045(3) -0.024(3) -0.006(2) 0.000(2) C9 0.025(2) 0.048(3) 0.039(3) -0.021(2) -0.0016(19) -0.001(2) C10 0.027(2) 0.043(3) 0.039(3) -0.017(2) -0.0024(19) -0.006(2) C18 0.045(3) 0.056(3) 0.038(3) -0.016(3) 0.000(2) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O1 2.033(6) . ? Na1 O5 2.164(6) . ? Na1 O6 2.291(6) . ? Na1 O4 2.334(6) . ? Na1 I1 2.881(4) . ? N1 C23 1.385(7) . ? N1 C19 1.388(8) . ? N1 C26 1.481(8) . ? O1 C23 1.217(7) . ? O2 C19 1.208(7) . ? O3 C2 1.374(7) 2_666 ? O3 C11 1.448(7) . ? O4 C13 1.423(7) . ? O4 C12 1.430(7) . ? O5 C15 1.416(8) . ? O5 C14 1.419(7) . ? O6 C16 1.420(8) . ? O6 C17 1.435(7) . ? C11 C12 1.493(9) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.496(9) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.500(10) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 C18 1.498(9) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C19 C20 1.484(8) . ? C20 C25 1.367(8) 2_666 ? C20 C21 1.409(7) . ? C21 C22 1.400(7) . ? C21 C21 1.434(11) 2_666 ? C22 C24 1.381(7) . ? C22 C23 1.481(8) . ? C24 C25 1.398(8) . ? C24 H24A 0.950 . ? C25 C20 1.367(8) 2_666 ? C25 H25A 0.950 . ? C26 C27 1.537(10) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.498(10) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C28 C29 1.510(11) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C29 C30 1.550(13) . ? C29 H29A 0.990 . ? C29 H29B 0.990 . ? C30 C32 1.509(10) . ? C30 H30A 0.990 . ? C30 H30B 0.990 . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C35 Cl7 1.725(8) . ? C35 Cl9 1.753(8) . ? C35 Cl8 1.758(10) . ? C35 H35A 1.000 . ? C36 Cl11 1.720(8) . ? C36 Cl12 1.736(9) . ? C36 Cl10 1.761(10) . ? C36 H36A 1.000 . ? C33 Cl1 1.725(9) . ? C33 Cl2 1.749(8) . ? C33 Cl3 1.765(8) . ? C33 H33A 1.000 . ? C34 Cl4 1.726(7) . ? C34 Cl5 1.742(7) . ? C34 Cl6 1.780(8) . ? C34 H34A 1.000 . ? O7 C6 1.368(7) . ? O7 C18 1.434(7) . ? C1 C2 1.369(8) . ? C1 C9 1.408(8) . ? C1 H1A 0.950 . ? C2 O3 1.374(7) 2_666 ? C2 C3 1.422(8) . ? C3 C4 1.354(8) . ? C3 H3A 0.950 . ? C4 C10 1.418(8) . ? C4 H4A 0.950 . ? C5 C6 1.367(8) . ? C5 C10 1.406(8) . ? C5 H5A 0.950 . ? C6 C7 1.416(8) . ? C7 C8 1.364(8) . ? C7 H7A 0.950 . ? C8 C9 1.422(8) . ? C8 H8A 0.950 . ? C9 C10 1.429(7) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Na1 O5 130.8(3) . . ? O1 Na1 O6 97.1(2) . . ? O5 Na1 O6 75.22(19) . . ? O1 Na1 O4 91.6(2) . . ? O5 Na1 O4 73.54(19) . . ? O6 Na1 O4 145.1(2) . . ? O1 Na1 I1 104.23(18) . . ? O5 Na1 I1 124.86(19) . . ? O6 Na1 I1 105.36(18) . . ? O4 Na1 I1 105.10(17) . . ? C23 N1 C19 125.5(5) . . ? C23 N1 C26 117.4(5) . . ? C19 N1 C26 117.0(5) . . ? C23 O1 Na1 178.1(4) . . ? C2 O3 C11 116.7(4) 2_666 . ? C13 O4 C12 111.0(5) . . ? C13 O4 Na1 109.8(3) . . ? C12 O4 Na1 123.8(4) . . ? C15 O5 C14 113.6(5) . . ? C15 O5 Na1 113.9(4) . . ? C14 O5 Na1 114.6(4) . . ? C16 O6 C17 110.6(5) . . ? C16 O6 Na1 107.4(3) . . ? C17 O6 Na1 127.1(4) . . ? O3 C11 C12 107.8(5) . . ? O3 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O3 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.5 . . ? O4 C12 C11 110.3(5) . . ? O4 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? O4 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? O4 C13 C14 108.3(5) . . ? O4 C13 H13A 110.0 . . ? C14 C13 H13A 110.0 . . ? O4 C13 H13B 110.0 . . ? C14 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? O5 C14 C13 107.5(5) . . ? O5 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? O5 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? O5 C15 C16 107.8(6) . . ? O5 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? O5 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.5 . . ? O6 C16 C15 108.3(5) . . ? O6 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O6 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O6 C17 C18 110.8(5) . . ? O6 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? O6 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? O2 C19 N1 120.8(6) . . ? O2 C19 C20 122.0(6) . . ? N1 C19 C20 117.2(5) . . ? C25 C20 C21 121.1(5) 2_666 . ? C25 C20 C19 120.3(5) 2_666 . ? C21 C20 C19 118.7(5) . . ? C22 C21 C20 122.3(5) . . ? C22 C21 C21 119.5(6) . 2_666 ? C20 C21 C21 118.2(6) . 2_666 ? C24 C22 C21 120.5(5) . . ? C24 C22 C23 120.3(5) . . ? C21 C22 C23 119.2(5) . . ? O1 C23 N1 120.9(5) . . ? O1 C23 C22 122.2(5) . . ? N1 C23 C22 117.0(5) . . ? C22 C24 C25 120.1(5) . . ? C22 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C20 C25 C24 120.6(5) 2_666 . ? C20 C25 H25A 119.7 2_666 . ? C24 C25 H25A 119.7 . . ? N1 C26 C27 110.7(5) . . ? N1 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? N1 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 112.6(6) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C29 113.0(6) . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 C30 114.7(7) . . ? C28 C29 H29A 108.6 . . ? C30 C29 H29A 108.6 . . ? C28 C29 H29B 108.6 . . ? C30 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? C32 C30 C29 110.1(8) . . ? C32 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C32 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl7 C35 Cl9 112.6(5) . . ? Cl7 C35 Cl8 111.0(5) . . ? Cl9 C35 Cl8 107.9(5) . . ? Cl7 C35 H35A 108.4 . . ? Cl9 C35 H35A 108.4 . . ? Cl8 C35 H35A 108.4 . . ? Cl11 C36 Cl12 110.0(5) . . ? Cl11 C36 Cl10 110.0(5) . . ? Cl12 C36 Cl10 111.3(5) . . ? Cl11 C36 H36A 108.5 . . ? Cl12 C36 H36A 108.5 . . ? Cl10 C36 H36A 108.5 . . ? Cl1 C33 Cl2 111.0(5) . . ? Cl1 C33 Cl3 109.5(5) . . ? Cl2 C33 Cl3 110.6(4) . . ? Cl1 C33 H33A 108.6 . . ? Cl2 C33 H33A 108.6 . . ? Cl3 C33 H33A 108.6 . . ? Cl4 C34 Cl5 112.8(5) . . ? Cl4 C34 Cl6 109.6(4) . . ? Cl5 C34 Cl6 110.5(4) . . ? Cl4 C34 H34A 107.9 . . ? Cl5 C34 H34A 107.9 . . ? Cl6 C34 H34A 107.9 . . ? C6 O7 C18 117.2(4) . . ? C2 C1 C9 120.2(5) . . ? C2 C1 H1A 119.9 . . ? C9 C1 H1A 119.9 . . ? C1 C2 O3 125.6(5) . 2_666 ? C1 C2 C3 120.2(5) . . ? O3 C2 C3 114.3(5) 2_666 . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C10 122.2(5) . . ? C3 C4 H4A 118.9 . . ? C10 C4 H4A 118.9 . . ? C6 C5 C10 120.9(5) . . ? C6 C5 H5A 119.6 . . ? C10 C5 H5A 119.6 . . ? C5 C6 O7 125.9(5) . . ? C5 C6 C7 119.4(5) . . ? O7 C6 C7 114.7(5) . . ? C8 C7 C6 120.9(5) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C7 C8 C9 121.4(5) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C1 C9 C8 122.6(5) . . ? C1 C9 C10 120.5(5) . . ? C8 C9 C10 116.9(5) . . ? C5 C10 C4 122.5(5) . . ? C5 C10 C9 120.5(5) . . ? C4 C10 C9 117.0(5) . . ? O7 C18 C17 108.6(5) . . ? O7 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? O7 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Na1 O4 C13 144.7(4) . . . . ? O5 Na1 O4 C13 12.4(4) . . . . ? O6 Na1 O4 C13 39.8(6) . . . . ? I1 Na1 O4 C13 -110.1(4) . . . . ? O1 Na1 O4 C12 -80.8(4) . . . . ? O5 Na1 O4 C12 146.9(4) . . . . ? O6 Na1 O4 C12 174.3(4) . . . . ? I1 Na1 O4 C12 24.4(4) . . . . ? O1 Na1 O5 C15 74.8(5) . . . . ? O6 Na1 O5 C15 -11.8(4) . . . . ? O4 Na1 O5 C15 152.4(4) . . . . ? I1 Na1 O5 C15 -110.4(4) . . . . ? O1 Na1 O5 C14 -58.3(5) . . . . ? O6 Na1 O5 C14 -144.9(4) . . . . ? O4 Na1 O5 C14 19.2(4) . . . . ? I1 Na1 O5 C14 116.4(4) . . . . ? O1 Na1 O6 C16 -150.2(4) . . . . ? O5 Na1 O6 C16 -19.9(4) . . . . ? O4 Na1 O6 C16 -47.0(6) . . . . ? I1 Na1 O6 C16 102.9(4) . . . . ? O1 Na1 O6 C17 75.4(5) . . . . ? O5 Na1 O6 C17 -154.2(4) . . . . ? O4 Na1 O6 C17 178.6(4) . . . . ? I1 Na1 O6 C17 -31.5(5) . . . . ? C2 O3 C11 C12 179.2(5) 2_666 . . . ? C13 O4 C12 C11 -171.6(5) . . . . ? Na1 O4 C12 C11 54.3(6) . . . . ? O3 C11 C12 O4 69.3(6) . . . . ? C12 O4 C13 C14 179.6(5) . . . . ? Na1 O4 C13 C14 -39.8(6) . . . . ? C15 O5 C14 C13 180.0(5) . . . . ? Na1 O5 C14 C13 -46.7(6) . . . . ? O4 C13 C14 O5 56.8(6) . . . . ? C14 O5 C15 C16 173.7(5) . . . . ? Na1 O5 C15 C16 40.1(6) . . . . ? C17 O6 C16 C15 -170.7(5) . . . . ? Na1 O6 C16 C15 46.8(6) . . . . ? O5 C15 C16 O6 -58.5(7) . . . . ? C16 O6 C17 C18 179.0(5) . . . . ? Na1 O6 C17 C18 -47.7(7) . . . . ? C23 N1 C19 O2 177.6(5) . . . . ? C26 N1 C19 O2 1.0(8) . . . . ? C23 N1 C19 C20 -3.3(8) . . . . ? C26 N1 C19 C20 -179.9(5) . . . . ? O2 C19 C20 C25 -0.9(8) . . . 2_666 ? N1 C19 C20 C25 180.0(5) . . . 2_666 ? O2 C19 C20 C21 179.4(5) . . . . ? N1 C19 C20 C21 0.2(7) . . . . ? C25 C20 C21 C22 -178.8(5) 2_666 . . . ? C19 C20 C21 C22 0.9(7) . . . . ? C25 C20 C21 C21 1.1(8) 2_666 . . 2_666 ? C19 C20 C21 C21 -179.1(5) . . . 2_666 ? C20 C21 C22 C24 -179.7(5) . . . . ? C21 C21 C22 C24 0.4(8) 2_666 . . . ? C20 C21 C22 C23 0.6(7) . . . . ? C21 C21 C22 C23 -179.3(5) 2_666 . . . ? C19 N1 C23 O1 -176.2(5) . . . . ? C26 N1 C23 O1 0.4(7) . . . . ? C19 N1 C23 C22 4.8(7) . . . . ? C26 N1 C23 C22 -178.6(5) . . . . ? C24 C22 C23 O1 -2.0(8) . . . . ? C21 C22 C23 O1 177.7(5) . . . . ? C24 C22 C23 N1 177.0(5) . . . . ? C21 C22 C23 N1 -3.3(7) . . . . ? C21 C22 C24 C25 0.5(8) . . . . ? C23 C22 C24 C25 -179.9(5) . . . . ? C22 C24 C25 C20 -1.6(8) . . . 2_666 ? C23 N1 C26 C27 -89.7(6) . . . . ? C19 N1 C26 C27 87.2(7) . . . . ? N1 C26 C27 C28 -177.5(6) . . . . ? C26 C27 C28 C29 178.3(7) . . . . ? C27 C28 C29 C30 -71.8(9) . . . . ? C28 C29 C30 C32 -177.4(7) . . . . ? C9 C1 C2 O3 -179.0(5) . . . 2_666 ? C9 C1 C2 C3 0.7(8) . . . . ? C1 C2 C3 C4 -0.3(8) . . . . ? O3 C2 C3 C4 179.4(5) 2_666 . . . ? C2 C3 C4 C10 -0.8(8) . . . . ? C10 C5 C6 O7 -179.0(5) . . . . ? C10 C5 C6 C7 1.2(7) . . . . ? C18 O7 C6 C5 2.0(7) . . . . ? C18 O7 C6 C7 -178.2(5) . . . . ? C5 C6 C7 C8 -0.7(8) . . . . ? O7 C6 C7 C8 179.5(5) . . . . ? C6 C7 C8 C9 -0.1(8) . . . . ? C2 C1 C9 C8 177.7(5) . . . . ? C2 C1 C9 C10 -0.2(7) . . . . ? C7 C8 C9 C1 -177.5(5) . . . . ? C7 C8 C9 C10 0.4(7) . . . . ? C6 C5 C10 C4 177.9(5) . . . . ? C6 C5 C10 C9 -0.9(7) . . . . ? C3 C4 C10 C5 -177.6(5) . . . . ? C3 C4 C10 C9 1.3(7) . . . . ? C1 C9 C10 C5 178.1(5) . . . . ? C8 C9 C10 C5 0.1(7) . . . . ? C1 C9 C10 C4 -0.8(7) . . . . ? C8 C9 C10 C4 -178.8(5) . . . . ? C6 O7 C18 C17 -171.1(4) . . . . ? O6 C17 C18 O7 -68.0(6) . . . . ? #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 644507' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O10, 2(C H Cl3)' _chemical_formula_sum 'C38 H46 Cl6 O10' _chemical_formula_weight 875.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7936(12) _cell_length_b 11.3413(13) _cell_length_c 17.171(2) _cell_angle_alpha 92.089(2) _cell_angle_beta 105.095(2) _cell_angle_gamma 94.500(2) _cell_volume 2019.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4179 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.56 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.981 _exptl_absorpt_correction_T_max 0.990 _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 SHELXL. ; _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6923 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'thin-slice \w-scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 16892 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.64 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 8245 _reflns_number_gt 5266 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 1994)' _computing_cell_refinement 'SAINT (Bruker, 1994)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL v.6.10 (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0736P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8245 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.516 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.067 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.81112(19) 0.56470(17) 0.30692(12) 0.0271(5) Uani 1 1 d . . . O2 O 0.91285(19) 0.44123(18) 0.19905(12) 0.0301(5) Uani 1 1 d . . . O3 O 0.68438(19) 0.93752(16) 0.66336(12) 0.0257(4) Uani 1 1 d . . . O4 O 0.74265(18) 1.15737(17) 0.76100(12) 0.0270(5) Uani 1 1 d . . . O5 O 0.93210(19) 1.36031(16) 0.82860(12) 0.0260(5) Uani 1 1 d . . . O6 O 0.83048(17) 0.07972(17) 0.29598(11) 0.0235(4) Uani 1 1 d . . . O7 O 0.66675(18) 0.40389(17) 0.65833(11) 0.0237(4) Uani 1 1 d . . . O8 O 0.60301(18) 0.60529(16) 0.74005(11) 0.0241(4) Uani 1 1 d . . . O9 O 0.80322(18) 0.73615(17) 0.85459(12) 0.0260(5) Uani 1 1 d . . . O10 O 0.98814(19) 0.90118(17) 0.80191(12) 0.0272(5) Uani 1 1 d . . . C1 C 0.7212(3) 0.8311(2) 0.38979(17) 0.0251(6) Uani 1 1 d . . . H1A H 0.6945 0.9049 0.3705 0.030 Uiso 1 1 calc R . . C2 C 0.7485(3) 0.7497(2) 0.33818(18) 0.0263(6) Uani 1 1 d . . . H2A H 0.7409 0.7670 0.2835 0.032 Uiso 1 1 calc R . . C3 C 0.7885(3) 0.6390(2) 0.36594(18) 0.0242(6) Uani 1 1 d . . . C4 C 0.8015(3) 0.6138(3) 0.44453(17) 0.0250(6) Uani 1 1 d . . . H4A H 0.8306 0.5402 0.4629 0.030 Uiso 1 1 calc R . . C5 C 0.7796(3) 0.6737(3) 0.58019(17) 0.0256(6) Uani 1 1 d . . . H5A H 0.8057 0.5995 0.5992 0.031 Uiso 1 1 calc R . . C6 C 0.7507(3) 0.7544(2) 0.63201(18) 0.0245(6) Uani 1 1 d . . . H6A H 0.7574 0.7364 0.6865 0.029 Uiso 1 1 calc R . . C7 C 0.7109(3) 0.8653(2) 0.60483(18) 0.0245(6) Uani 1 1 d . . . C8 C 0.7013(3) 0.8921(2) 0.52651(17) 0.0247(6) Uani 1 1 d . . . H8A H 0.6744 0.9666 0.5085 0.030 Uiso 1 1 calc R . . C9 C 0.7315(3) 0.8084(2) 0.47202(17) 0.0222(6) Uani 1 1 d . . . C10 C 0.7716(3) 0.6974(2) 0.49888(17) 0.0214(6) Uani 1 1 d . . . C11 C 0.6097(3) 0.2263(2) 0.38424(16) 0.0221(6) Uani 1 1 d . . . H11A H 0.5237 0.2472 0.3668 0.027 Uiso 1 1 calc R . . C12 C 0.6617(3) 0.1675(2) 0.33143(17) 0.0232(6) Uani 1 1 d . . . H12A H 0.6113 0.1472 0.2778 0.028 Uiso 1 1 calc R . . C13 C 0.7899(3) 0.1363(2) 0.35567(17) 0.0206(6) Uani 1 1 d . . . C14 C 0.8622(3) 0.1626(2) 0.43324(17) 0.0221(6) Uani 1 1 d . . . H14A H 0.9478 0.1403 0.4498 0.027 Uiso 1 1 calc R . . C15 C 0.8825(3) 0.2513(2) 0.57025(17) 0.0233(6) Uani 1 1 d . . . H15A H 0.9680 0.2291 0.5874 0.028 Uiso 1 1 calc R . . C16 C 0.8319(3) 0.3092(2) 0.62373(17) 0.0236(6) Uani 1 1 d . . . H16A H 0.8816 0.3257 0.6780 0.028 Uiso 1 1 calc R . . C17 C 0.7052(3) 0.3452(2) 0.59883(16) 0.0205(6) Uani 1 1 d . . . C18 C 0.6310(3) 0.3187(2) 0.52133(16) 0.0216(6) Uani 1 1 d . . . H18A H 0.5456 0.3416 0.5052 0.026 Uiso 1 1 calc R . . C19 C 0.6827(3) 0.2565(2) 0.46508(16) 0.0198(6) Uani 1 1 d . . . C20 C 0.8098(3) 0.2233(2) 0.48916(16) 0.0199(6) Uani 1 1 d . . . C21 C 0.6333(3) 1.0468(2) 0.63851(18) 0.0275(7) Uani 1 1 d . . . H21A H 0.5487 1.0311 0.5983 0.033 Uiso 1 1 calc R . . H21B H 0.6925 1.0934 0.6134 0.033 Uiso 1 1 calc R . . C22 C 0.6184(3) 1.1150(3) 0.71190(19) 0.0286(7) Uani 1 1 d . . . H22A H 0.5666 1.1825 0.6952 0.034 Uiso 1 1 calc R . . H22B H 0.5732 1.0630 0.7428 0.034 Uiso 1 1 calc R . . C23 C 0.7367(3) 1.2332(3) 0.82709(18) 0.0289(7) Uani 1 1 d . . . H23A H 0.6950 1.1889 0.8635 0.035 Uiso 1 1 calc R . . H23B H 0.6849 1.2996 0.8073 0.035 Uiso 1 1 calc R . . C24 C 0.8721(3) 1.2807(3) 0.87239(18) 0.0304(7) Uani 1 1 d . . . H24A H 0.8696 1.3217 0.9238 0.036 Uiso 1 1 calc R . . H24B H 0.9252 1.2132 0.8860 0.036 Uiso 1 1 calc R . . C25 C 0.8639(3) 0.4553(2) 0.33132(18) 0.0264(6) Uani 1 1 d . . . H25A H 0.8133 0.4130 0.3640 0.032 Uiso 1 1 calc R . . H25B H 0.9543 0.4706 0.3641 0.032 Uiso 1 1 calc R . . C26 C 0.8570(3) 0.3821(3) 0.25442(18) 0.0311(7) Uani 1 1 d . . . H26A H 0.9008 0.3095 0.2690 0.037 Uiso 1 1 calc R . . H26B H 0.7654 0.3574 0.2273 0.037 Uiso 1 1 calc R . . C27 C 1.0489(3) 0.4477(3) 0.22139(19) 0.0286(7) Uani 1 1 d . . . H27A H 1.0774 0.3669 0.2202 0.034 Uiso 1 1 calc R . . H27B H 1.0826 0.4835 0.2771 0.034 Uiso 1 1 calc R . . C28 C 0.9596(3) 0.0454(3) 0.31880(17) 0.0247(6) Uani 1 1 d . . . H28A H 0.9657 -0.0179 0.3575 0.030 Uiso 1 1 calc R . . H28B H 1.0201 0.1140 0.3453 0.030 Uiso 1 1 calc R . . C29 C 0.5434(3) 0.4496(3) 0.63618(17) 0.0245(6) Uani 1 1 d . . . H29A H 0.4759 0.3851 0.6113 0.029 Uiso 1 1 calc R . . H29B H 0.5429 0.5107 0.5964 0.029 Uiso 1 1 calc R . . C30 C 0.5171(3) 0.5027(2) 0.71085(18) 0.0258(6) Uani 1 1 d . . . H30A H 0.4271 0.5240 0.6984 0.031 Uiso 1 1 calc R . . H30B H 0.5281 0.4441 0.7529 0.031 Uiso 1 1 calc R . . C31 C 0.5863(3) 0.6532(3) 0.81356(18) 0.0264(6) Uani 1 1 d . . . H31A H 0.6066 0.5951 0.8556 0.032 Uiso 1 1 calc R . . H31B H 0.4955 0.6703 0.8060 0.032 Uiso 1 1 calc R . . C32 C 0.6735(3) 0.7652(3) 0.84004(19) 0.0276(7) Uani 1 1 d . . . H32A H 0.6554 0.8228 0.7975 0.033 Uiso 1 1 calc R . . H32B H 0.6590 0.8013 0.8899 0.033 Uiso 1 1 calc R . . C33 C 0.8971(3) 0.8227(3) 0.90350(18) 0.0296(7) Uani 1 1 d . . . H33A H 0.9790 0.7861 0.9231 0.035 Uiso 1 1 calc R . . H33B H 0.8679 0.8467 0.9513 0.035 Uiso 1 1 calc R . . C34 C 0.9221(3) 0.9308(3) 0.86094(18) 0.0280(7) Uani 1 1 d . . . H34A H 0.8394 0.9623 0.8343 0.034 Uiso 1 1 calc R . . H34B H 0.9750 0.9928 0.9004 0.034 Uiso 1 1 calc R . . C35 C 1.0060(3) 0.9985(3) 0.75512(18) 0.0275(7) Uani 1 1 d . . . H35A H 1.0756 1.0563 0.7873 0.033 Uiso 1 1 calc R . . H35B H 0.9258 1.0388 0.7396 0.033 Uiso 1 1 calc R . . C36 C 1.1010(3) 0.5212(2) 0.16422(18) 0.0260(6) Uani 1 1 d . . . H36A H 1.1959 0.5204 0.1772 0.031 Uiso 1 1 calc R . . H36B H 1.0641 0.4879 0.1081 0.031 Uiso 1 1 calc R . . C37 C 0.2971(3) 0.8797(3) 0.9109(2) 0.0428(9) Uani 1 1 d . . . H37A H 0.2234 0.8638 0.8615 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.20794(10) 0.43628(9) 0.98703(5) 0.0516(3) Uani 1 1 d . . . Cl2 Cl 0.24251(9) 0.95245(8) 0.98656(5) 0.0434(2) Uani 1 1 d . . . Cl3 Cl 0.35233(14) 0.74464(10) 0.94394(7) 0.0784(4) Uani 1 1 d . . . C38 C 0.2452(3) 0.3814(3) 0.90010(18) 0.0306(7) Uani 1 1 d . . . H38A H 0.1782 0.4017 0.8514 0.037 Uiso 1 1 calc R . . Cl4 Cl 0.39659(9) 0.44521(9) 0.89567(6) 0.0516(3) Uani 1 1 d . . . Cl5 Cl 0.41974(10) 0.96916(10) 0.88649(6) 0.0566(3) Uani 1 1 d . . . Cl6 Cl 0.24650(11) 0.22737(8) 0.90109(7) 0.0603(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0310(12) 0.0241(10) 0.0262(11) 0.0011(8) 0.0069(9) 0.0043(9) O2 0.0294(12) 0.0331(12) 0.0294(11) 0.0047(9) 0.0098(9) 0.0040(9) O3 0.0299(11) 0.0208(10) 0.0237(10) 0.0001(8) 0.0028(9) 0.0012(8) O4 0.0252(11) 0.0262(11) 0.0269(11) -0.0051(9) 0.0027(9) 0.0023(8) O5 0.0278(11) 0.0201(10) 0.0289(11) 0.0007(8) 0.0055(9) 0.0030(8) O6 0.0196(10) 0.0261(10) 0.0242(10) -0.0028(8) 0.0047(8) 0.0032(8) O7 0.0218(10) 0.0265(11) 0.0215(10) -0.0020(8) 0.0032(8) 0.0044(8) O8 0.0225(10) 0.0237(10) 0.0247(11) -0.0047(8) 0.0060(8) -0.0024(8) O9 0.0219(10) 0.0235(10) 0.0319(11) -0.0060(9) 0.0077(9) -0.0011(8) O10 0.0301(11) 0.0240(10) 0.0301(11) 0.0006(9) 0.0128(9) 0.0032(8) C1 0.0245(15) 0.0189(14) 0.0299(16) 0.0039(12) 0.0037(13) 0.0010(11) C2 0.0259(15) 0.0251(15) 0.0267(16) 0.0024(12) 0.0059(13) -0.0018(12) C3 0.0187(14) 0.0243(15) 0.0290(16) -0.0003(12) 0.0065(12) -0.0014(11) C4 0.0220(15) 0.0214(14) 0.0294(16) 0.0034(12) 0.0030(12) 0.0003(11) C5 0.0230(15) 0.0219(14) 0.0292(16) 0.0057(12) 0.0024(12) -0.0004(12) C6 0.0219(15) 0.0225(14) 0.0272(15) 0.0035(12) 0.0040(12) -0.0019(11) C7 0.0222(15) 0.0201(14) 0.0287(16) -0.0023(12) 0.0043(12) -0.0044(11) C8 0.0231(15) 0.0174(14) 0.0287(16) 0.0006(12) -0.0003(12) -0.0024(11) C9 0.0188(14) 0.0203(14) 0.0238(15) 0.0013(11) 0.0005(11) -0.0041(11) C10 0.0171(14) 0.0200(14) 0.0238(15) 0.0021(11) 0.0004(11) -0.0019(11) C11 0.0161(14) 0.0228(14) 0.0243(15) 0.0008(12) -0.0001(11) 0.0013(11) C12 0.0186(14) 0.0249(15) 0.0222(15) -0.0009(12) 0.0000(11) -0.0025(11) C13 0.0227(14) 0.0153(13) 0.0253(15) 0.0001(11) 0.0098(12) 0.0000(11) C14 0.0184(14) 0.0217(14) 0.0262(15) 0.0016(12) 0.0058(12) 0.0018(11) C15 0.0182(14) 0.0247(15) 0.0254(15) 0.0017(12) 0.0029(12) 0.0014(11) C16 0.0227(15) 0.0240(15) 0.0213(15) 0.0002(12) 0.0016(12) -0.0012(12) C17 0.0228(14) 0.0170(13) 0.0221(14) 0.0010(11) 0.0070(12) 0.0003(11) C18 0.0193(14) 0.0191(14) 0.0245(15) 0.0018(11) 0.0024(12) 0.0021(11) C19 0.0175(14) 0.0189(13) 0.0204(14) 0.0010(11) 0.0021(11) -0.0034(11) C20 0.0187(14) 0.0173(13) 0.0218(14) 0.0009(11) 0.0032(11) -0.0024(11) C21 0.0256(16) 0.0198(14) 0.0328(17) -0.0002(12) 0.0005(13) 0.0011(12) C22 0.0233(15) 0.0237(15) 0.0368(18) -0.0007(13) 0.0049(13) 0.0016(12) C23 0.0338(17) 0.0268(16) 0.0269(16) -0.0001(13) 0.0105(14) -0.0003(13) C24 0.0395(18) 0.0250(15) 0.0251(16) 0.0016(13) 0.0062(14) 0.0015(13) C25 0.0295(16) 0.0206(14) 0.0308(17) 0.0046(12) 0.0098(13) 0.0047(12) C26 0.0400(19) 0.0252(16) 0.0320(17) 0.0035(13) 0.0160(15) 0.0034(14) C27 0.0298(17) 0.0254(15) 0.0327(17) 0.0037(13) 0.0101(14) 0.0086(13) C28 0.0214(15) 0.0251(15) 0.0283(16) 0.0024(12) 0.0072(12) 0.0031(12) C29 0.0188(14) 0.0247(15) 0.0282(16) -0.0034(12) 0.0043(12) 0.0003(11) C30 0.0202(15) 0.0227(15) 0.0342(17) -0.0025(12) 0.0084(13) -0.0012(12) C31 0.0233(15) 0.0299(16) 0.0266(16) -0.0029(13) 0.0083(12) 0.0019(12) C32 0.0280(16) 0.0257(15) 0.0301(16) -0.0046(13) 0.0099(13) 0.0043(12) C33 0.0289(17) 0.0316(16) 0.0255(16) -0.0057(13) 0.0051(13) -0.0026(13) C34 0.0289(16) 0.0259(15) 0.0299(16) -0.0064(13) 0.0109(13) 0.0000(12) C35 0.0287(16) 0.0232(15) 0.0320(17) -0.0006(13) 0.0111(13) 0.0013(12) C36 0.0286(16) 0.0241(15) 0.0255(16) -0.0022(12) 0.0077(13) 0.0037(12) C37 0.043(2) 0.042(2) 0.0369(19) -0.0111(16) -0.0001(16) 0.0083(16) Cl1 0.0575(6) 0.0712(7) 0.0276(5) 0.0005(4) 0.0126(4) 0.0117(5) Cl2 0.0445(5) 0.0419(5) 0.0442(5) -0.0048(4) 0.0118(4) 0.0091(4) Cl3 0.1223(11) 0.0420(6) 0.0710(8) -0.0045(5) 0.0192(7) 0.0339(6) C38 0.0334(17) 0.0292(16) 0.0269(16) 0.0018(13) 0.0049(13) -0.0004(13) Cl4 0.0442(5) 0.0507(6) 0.0610(6) 0.0034(5) 0.0197(5) -0.0081(4) Cl5 0.0519(6) 0.0748(7) 0.0420(5) -0.0121(5) 0.0140(4) 0.0012(5) Cl6 0.0801(8) 0.0274(5) 0.0656(7) 0.0039(4) 0.0069(6) -0.0011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C3 1.377(3) . ? O1 C25 1.437(3) . ? O2 C27 1.413(3) . ? O2 C26 1.414(3) . ? O3 C7 1.374(3) . ? O3 C21 1.430(3) . ? O4 C23 1.417(3) . ? O4 C22 1.421(3) . ? O5 C24 1.418(4) . ? O5 C36 1.427(3) 2_776 ? O6 C13 1.373(3) . ? O6 C28 1.435(3) . ? O7 C17 1.369(3) . ? O7 C29 1.430(3) . ? O8 C31 1.416(3) . ? O8 C30 1.418(3) . ? O9 C32 1.424(3) . ? O9 C33 1.427(3) . ? O10 C35 1.418(3) . ? O10 C34 1.428(3) . ? C1 C2 1.358(4) . ? C1 C9 1.422(4) . ? C2 C3 1.418(4) . ? C3 C4 1.363(4) . ? C4 C10 1.420(4) . ? C5 C6 1.363(4) . ? C5 C10 1.413(4) . ? C6 C7 1.417(4) . ? C7 C8 1.369(4) . ? C8 C9 1.423(4) . ? C9 C10 1.418(4) . ? C11 C12 1.365(4) . ? C11 C19 1.421(4) . ? C12 C13 1.414(4) . ? C13 C14 1.366(4) . ? C14 C20 1.419(4) . ? C15 C16 1.358(4) . ? C15 C20 1.420(4) . ? C16 C17 1.420(4) . ? C17 C18 1.371(4) . ? C18 C19 1.427(4) . ? C19 C20 1.411(4) . ? C21 C22 1.505(4) . ? C23 C24 1.512(4) . ? C25 C26 1.515(4) . ? C27 C36 1.500(4) . ? C28 C35 1.492(4) 2_766 ? C29 C30 1.499(4) . ? C31 C32 1.501(4) . ? C33 C34 1.492(4) . ? C35 C28 1.492(4) 2_766 ? C36 O5 1.427(3) 2_776 ? C37 Cl3 1.748(4) . ? C37 Cl5 1.752(4) . ? C37 Cl2 1.764(3) . ? Cl1 C38 1.749(3) . ? C38 Cl6 1.749(3) . ? C38 Cl4 1.756(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 O1 C25 117.5(2) . . ? C27 O2 C26 113.2(2) . . ? C7 O3 C21 116.8(2) . . ? C23 O4 C22 112.4(2) . . ? C24 O5 C36 112.9(2) . 2_776 ? C13 O6 C28 116.0(2) . . ? C17 O7 C29 117.3(2) . . ? C31 O8 C30 111.3(2) . . ? C32 O9 C33 114.8(2) . . ? C35 O10 C34 111.9(2) . . ? C2 C1 C9 121.6(3) . . ? C1 C2 C3 120.0(3) . . ? C4 C3 O1 125.7(3) . . ? C4 C3 C2 120.6(3) . . ? O1 C3 C2 113.7(2) . . ? C3 C4 C10 120.0(3) . . ? C6 C5 C10 121.7(3) . . ? C5 C6 C7 120.1(3) . . ? C8 C7 O3 125.9(3) . . ? C8 C7 C6 120.3(3) . . ? O3 C7 C6 113.8(2) . . ? C7 C8 C9 120.0(3) . . ? C10 C9 C1 117.8(3) . . ? C10 C9 C8 120.0(3) . . ? C1 C9 C8 122.2(3) . . ? C5 C10 C9 117.9(3) . . ? C5 C10 C4 122.0(3) . . ? C9 C10 C4 120.0(3) . . ? C12 C11 C19 120.7(3) . . ? C11 C12 C13 120.8(3) . . ? C14 C13 O6 125.4(2) . . ? C14 C13 C12 120.0(2) . . ? O6 C13 C12 114.6(2) . . ? C13 C14 C20 120.0(3) . . ? C16 C15 C20 121.2(3) . . ? C15 C16 C17 120.3(3) . . ? O7 C17 C18 125.2(3) . . ? O7 C17 C16 114.3(2) . . ? C18 C17 C16 120.5(3) . . ? C17 C18 C19 119.6(3) . . ? C20 C19 C11 118.1(2) . . ? C20 C19 C18 120.0(2) . . ? C11 C19 C18 121.8(2) . . ? C19 C20 C14 120.3(2) . . ? C19 C20 C15 118.4(2) . . ? C14 C20 C15 121.3(3) . . ? O3 C21 C22 108.3(2) . . ? O4 C22 C21 108.9(2) . . ? O4 C23 C24 108.8(2) . . ? O5 C24 C23 113.7(2) . . ? O1 C25 C26 106.6(2) . . ? O2 C26 C25 114.6(2) . . ? O2 C27 C36 109.9(2) . . ? O6 C28 C35 108.9(2) . 2_766 ? O7 C29 C30 108.4(2) . . ? O8 C30 C29 109.9(2) . . ? O8 C31 C32 109.7(2) . . ? O9 C32 C31 108.1(2) . . ? O9 C33 C34 114.0(2) . . ? O10 C34 C33 109.2(2) . . ? O10 C35 C28 109.2(2) . 2_766 ? O5 C36 C27 109.0(2) 2_776 . ? Cl3 C37 Cl5 110.4(2) . . ? Cl3 C37 Cl2 109.9(2) . . ? Cl5 C37 Cl2 110.35(18) . . ? Cl6 C38 Cl1 109.71(17) . . ? Cl6 C38 Cl4 109.61(18) . . ? Cl1 C38 Cl4 110.14(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C1 C2 C3 0.0(4) . . . . ? C25 O1 C3 C4 -5.9(4) . . . . ? C25 O1 C3 C2 174.1(2) . . . . ? C1 C2 C3 C4 -0.9(4) . . . . ? C1 C2 C3 O1 179.1(2) . . . . ? O1 C3 C4 C10 -178.3(2) . . . . ? C2 C3 C4 C10 1.7(4) . . . . ? C10 C5 C6 C7 0.4(4) . . . . ? C21 O3 C7 C8 4.8(4) . . . . ? C21 O3 C7 C6 -175.0(2) . . . . ? C5 C6 C7 C8 -0.1(4) . . . . ? C5 C6 C7 O3 179.7(2) . . . . ? O3 C7 C8 C9 -179.8(2) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C2 C1 C9 C10 0.0(4) . . . . ? C2 C1 C9 C8 -179.0(3) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? C7 C8 C9 C1 179.0(3) . . . . ? C6 C5 C10 C9 -0.4(4) . . . . ? C6 C5 C10 C4 180.0(3) . . . . ? C1 C9 C10 C5 -178.8(3) . . . . ? C8 C9 C10 C5 0.3(4) . . . . ? C1 C9 C10 C4 0.8(4) . . . . ? C8 C9 C10 C4 179.9(2) . . . . ? C3 C4 C10 C5 177.9(3) . . . . ? C3 C4 C10 C9 -1.7(4) . . . . ? C19 C11 C12 C13 -0.6(4) . . . . ? C28 O6 C13 C14 0.6(4) . . . . ? C28 O6 C13 C12 -179.2(2) . . . . ? C11 C12 C13 C14 1.5(4) . . . . ? C11 C12 C13 O6 -178.7(2) . . . . ? O6 C13 C14 C20 179.0(2) . . . . ? C12 C13 C14 C20 -1.2(4) . . . . ? C20 C15 C16 C17 -1.3(4) . . . . ? C29 O7 C17 C18 -5.4(4) . . . . ? C29 O7 C17 C16 176.0(2) . . . . ? C15 C16 C17 O7 -179.3(2) . . . . ? C15 C16 C17 C18 2.1(4) . . . . ? O7 C17 C18 C19 -179.8(2) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C12 C11 C19 C20 -0.5(4) . . . . ? C12 C11 C19 C18 179.5(3) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C17 C18 C19 C11 179.6(3) . . . . ? C11 C19 C20 C14 0.8(4) . . . . ? C18 C19 C20 C14 -179.3(2) . . . . ? C11 C19 C20 C15 -178.9(2) . . . . ? C18 C19 C20 C15 1.1(4) . . . . ? C13 C14 C20 C19 0.1(4) . . . . ? C13 C14 C20 C15 179.7(3) . . . . ? C16 C15 C20 C19 -0.3(4) . . . . ? C16 C15 C20 C14 -179.9(3) . . . . ? C7 O3 C21 C22 -176.9(2) . . . . ? C23 O4 C22 C21 173.7(2) . . . . ? O3 C21 C22 O4 71.5(3) . . . . ? C22 O4 C23 C24 -176.1(2) . . . . ? C36 O5 C24 C23 83.8(3) 2_776 . . . ? O4 C23 C24 O5 68.6(3) . . . . ? C3 O1 C25 C26 170.2(2) . . . . ? C27 O2 C26 C25 77.0(3) . . . . ? O1 C25 C26 O2 52.6(3) . . . . ? C26 O2 C27 C36 -174.7(2) . . . . ? C13 O6 C28 C35 -171.9(2) . . . 2_766 ? C17 O7 C29 C30 176.3(2) . . . . ? C31 O8 C30 C29 -176.2(2) . . . . ? O7 C29 C30 O8 67.8(3) . . . . ? C30 O8 C31 C32 -176.9(2) . . . . ? C33 O9 C32 C31 -161.1(2) . . . . ? O8 C31 C32 O9 -62.6(3) . . . . ? C32 O9 C33 C34 -74.5(3) . . . . ? C35 O10 C34 C33 175.5(2) . . . . ? O9 C33 C34 O10 -70.0(3) . . . . ? C34 O10 C35 C28 -164.1(2) . . . 2_766 ? O2 C27 C36 O5 64.0(3) . . . 2_776 ? #===END