#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000335.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000335 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_name_common 01364e _chemical_formula_sum 'C20 H44 As2 F12 Li2 O10' _chemical_formula_weight 836.27 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 12.3788(18) _cell_length_b 22.512(3) _cell_length_c 12.3431(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3439.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type multiscans _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS sheldrick, 2002)' _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^)+(0.0400P)^2^+2.039P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8445 _refine_ls_number_parameters 590 _refine_ls_number_restraints 442 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.298 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.2024(2) -1.0734(4) 0.31463(19) 0.0393(9) Uani 1 1 d . A . Li2 Li 0.2991(2) -0.9289(4) 0.1980(2) 0.0399(9) Uani 1 1 d . A . C1 C 0.03112(15) -1.0554(4) 0.29714(15) 0.0665(9) Uani 1 1 d . . . H1A H -0.0069 -0.9862 0.2988 0.100 Uiso 1 1 calc R . . H1B H 0.0319 -1.1348 0.3288 0.100 Uiso 1 1 calc R . . H1C H 0.0240 -1.0990 0.2541 0.100 Uiso 1 1 calc R . . O1 O 0.09563(9) -0.9771(2) 0.31129(8) 0.0478(4) Uani 1 1 d . . . C2 C 0.10496(15) -0.9065(3) 0.37274(12) 0.0499(7) Uani 1 1 d . . . H2A H 0.1123 -0.9825 0.4071 0.060 Uiso 1 1 calc R . . H2B H 0.0632 -0.8477 0.3753 0.060 Uiso 1 1 calc R . . C3 C 0.16675(16) -0.8071(3) 0.38070(14) 0.0551(7) Uani 1 1 d . . . H3A H 0.1577 -0.7250 0.3490 0.066 Uiso 1 1 calc R . . H3B H 0.1775 -0.7634 0.4243 0.066 Uiso 1 1 calc R . . O2 O 0.22348(9) -0.89615(17) 0.37083(9) 0.0449(4) Uani 1 1 d . . . C4 C 0.28608(15) -0.8167(3) 0.37186(12) 0.0494(6) Uani 1 1 d . . . H4A H 0.2991 -0.7568 0.4116 0.059 Uiso 1 1 calc R . . H4B H 0.2802 -0.7488 0.3345 0.059 Uiso 1 1 calc R . . C5 C 0.34056(13) -0.9295(3) 0.36925(11) 0.0478(6) Uani 1 1 d . A . H5A H 0.3839 -0.8793 0.3646 0.057 Uiso 1 1 calc R . . H5B H 0.3506 -0.9884 0.4094 0.057 Uiso 1 1 calc R . . O3 O 0.31612(8) -1.02559(18) 0.31552(7) 0.0384(4) Uani 1 1 d . . . C6 C 0.3707(3) -1.1337(6) 0.3194(2) 0.0359(10) Uani 0.702(10) 1 d PU A 1 H6A H 0.3703 -1.2038 0.3551 0.043 Uiso 0.702(10) 1 calc PR A 1 H6B H 0.4164 -1.0832 0.3276 0.043 Uiso 0.702(10) 1 calc PR A 1 C6' C 0.3438(7) -1.1816(12) 0.3090(5) 0.038(2) Uani 0.298(10) 1 d PU A 2 H6'A H 0.3668 -1.2214 0.3515 0.045 Uiso 0.298(10) 1 calc PR A 2 H6'B H 0.3055 -1.2496 0.2894 0.045 Uiso 0.298(10) 1 calc PR A 2 C7 C 0.3589(3) -1.2165(4) 0.25731(18) 0.0365(11) Uani 0.702(10) 1 d PDU A 1 H7A H 0.3958 -1.2921 0.2589 0.044 Uiso 0.702(10) 1 calc PR A 1 H7B H 0.3136 -1.2683 0.2496 0.044 Uiso 0.702(10) 1 calc PR A 1 C7' C 0.3938(6) -1.1674(12) 0.2676(4) 0.041(2) Uani 0.298(10) 1 d PU A 2 H7C H 0.4313 -1.0978 0.2873 0.049 Uiso 0.298(10) 1 calc PR A 2 H7D H 0.4149 -1.2657 0.2629 0.049 Uiso 0.298(10) 1 calc PR A 2 O4 O 0.35989(8) -1.11383(17) 0.20691(7) 0.0369(4) Uani 1 1 d D . . C8 C 0.3662(3) -1.1794(6) 0.14820(19) 0.0465(13) Uani 0.731(13) 1 d PDU A 1 H8A H 0.3302 -1.2571 0.1354 0.056 Uiso 0.731(13) 1 calc PR A 1 H8B H 0.4124 -1.2268 0.1532 0.056 Uiso 0.731(13) 1 calc PR A 1 C8' C 0.3969(8) -1.1200(17) 0.1566(5) 0.045(3) Uani 0.269(13) 1 d PU A 2 H8C H 0.4407 -1.0628 0.1695 0.054 Uiso 0.269(13) 1 calc PR A 2 H8D H 0.4092 -1.2248 0.1498 0.054 Uiso 0.269(13) 1 calc PR A 2 C9 C 0.35766(16) -1.0616(4) 0.09840(13) 0.0564(7) Uani 1 1 d . . . H9A H 0.4016 -1.0049 0.1032 0.068 Uiso 1 1 calc R A 1 H9B H 0.3476 -1.1084 0.0554 0.068 Uiso 1 1 calc R A 1 O5 O 0.30421(11) -0.9647(2) 0.10316(9) 0.0607(5) Uani 1 1 d . A . C10 C 0.28018(18) -0.8703(4) 0.04974(13) 0.0650(8) Uani 1 1 d . . . H10A H 0.3191 -0.8115 0.0413 0.097 Uiso 1 1 calc R A . H10B H 0.2444 -0.8033 0.0590 0.097 Uiso 1 1 calc R . . H10C H 0.2604 -0.9310 0.0120 0.097 Uiso 1 1 calc R . . C11 C 0.23960(16) -1.2111(3) 0.45314(12) 0.0539(7) Uani 1 1 d . A . H11A H 0.2129 -1.2663 0.4792 0.081 Uiso 1 1 calc R . . H11B H 0.2429 -1.1063 0.4663 0.081 Uiso 1 1 calc R . . H11C H 0.2864 -1.2537 0.4593 0.081 Uiso 1 1 calc R . . O6 O 0.20541(9) -1.22151(18) 0.38700(8) 0.0423(4) Uani 1 1 d . . . C12 C 0.20023(13) -1.3716(3) 0.36467(12) 0.0429(6) Uani 1 1 d . A . H12A H 0.1813 -1.4361 0.3944 0.051 Uiso 1 1 calc R . . H12B H 0.2465 -1.4097 0.3618 0.051 Uiso 1 1 calc R . . C13 C 0.15239(13) -1.3703(3) 0.29979(12) 0.0424(6) Uani 1 1 d . . . H13A H 0.1507 -1.4702 0.2799 0.051 Uiso 1 1 calc R A . H13B H 0.1048 -1.3424 0.3034 0.051 Uiso 1 1 calc R . . O7 O 0.17908(8) -1.26302(17) 0.26169(7) 0.0359(4) Uani 1 1 d . A . C14 C 0.13866(12) -1.2524(3) 0.19737(11) 0.0380(5) Uani 1 1 d . . . H14A H 0.0929 -1.2070 0.1972 0.046 Uiso 1 1 calc R A . H14B H 0.1311 -1.3525 0.1777 0.046 Uiso 1 1 calc R . . C15 C 0.17886(12) -1.1568(3) 0.16103(11) 0.0377(5) Uani 1 1 d . A . H15A H 0.2227 -1.2078 0.1584 0.045 Uiso 1 1 calc R . . H15B H 0.1515 -1.1420 0.1168 0.045 Uiso 1 1 calc R . . O8 O 0.19460(8) -1.01462(17) 0.19143(8) 0.0362(4) Uani 1 1 d . . . C16 C 0.14426(12) -0.9021(3) 0.16556(12) 0.0452(6) Uani 1 1 d . A . H16A H 0.0991 -0.9247 0.1765 0.054 Uiso 1 1 calc R . . H16B H 0.1374 -0.8980 0.1183 0.054 Uiso 1 1 calc R . . C17 C 0.17189(14) -0.7575(3) 0.19449(13) 0.0487(6) Uani 1 1 d . . . H17A H 0.1424 -0.6741 0.1739 0.058 Uiso 1 1 calc R A . H17B H 0.1727 -0.7565 0.2410 0.058 Uiso 1 1 calc R . . O9 O 0.24034(9) -0.74308(18) 0.18414(8) 0.0444(4) Uani 1 1 d . A . C18 C 0.27580(16) -0.6084(3) 0.20543(14) 0.0554(7) Uani 1 1 d . . . H18A H 0.2737 -0.5880 0.2505 0.066 Uiso 1 1 calc R A . H18B H 0.2542 -0.5239 0.1785 0.066 Uiso 1 1 calc R . . C19 C 0.34928(16) -0.6281(3) 0.19989(13) 0.0525(7) Uani 1 1 d . A . H19A H 0.3520 -0.6312 0.1542 0.063 Uiso 1 1 calc R . . H19B H 0.3781 -0.5441 0.2208 0.063 Uiso 1 1 calc R . . O10 O 0.37355(9) -0.76458(19) 0.23059(9) 0.0494(4) Uani 1 1 d . . . C20 C 0.44664(15) -0.7804(4) 0.23772(17) 0.0672(8) Uani 1 1 d . A . H20A H 0.4697 -0.6868 0.2537 0.101 Uiso 1 1 calc R . . H20B H 0.4571 -0.8048 0.1961 0.101 Uiso 1 1 calc R . . H20C H 0.4635 -0.8606 0.2683 0.101 Uiso 1 1 calc R . . Li3 Li -0.0025(2) -0.7489(4) 0.00566(18) 0.0367(8) Uani 1 1 d . . . B1 B 0.03751(13) -0.9840(3) -0.07871(12) 0.0322(5) Uani 1 1 d . . . F1 F 0.09954(7) -0.97022(18) -0.03562(8) 0.0541(4) Uani 1 1 d . . . F2 F -0.00994(7) -0.87873(14) -0.06427(6) 0.0421(3) Uani 1 1 d . . . F3 F 0.04393(8) -0.96141(17) -0.14066(7) 0.0503(4) Uani 1 1 d . . . F4 F 0.00927(7) -1.12643(14) -0.07396(6) 0.0409(3) Uani 1 1 d . . . B2 B 0.09751(13) -0.5049(3) 0.04891(12) 0.0332(5) Uani 1 1 d . . . F5 F 0.06113(9) -0.50105(19) 0.09719(7) 0.0587(4) Uani 1 1 d . . . F6 F 0.07686(7) -0.38472(15) 0.00729(7) 0.0468(3) Uani 1 1 d . . . F7 F 0.16724(8) -0.49782(19) 0.07279(8) 0.0583(4) Uani 1 1 d . . . F8 F 0.07980(7) -0.63701(14) 0.01435(7) 0.0444(3) Uani 1 1 d . . . Li4 Li 0.4968(2) -0.7513(4) 0.00344(15) 0.0370(8) Uani 1 1 d D . . B3 B 0.43174(13) -0.9959(3) -0.09311(12) 0.0391(6) Uani 1 1 d D . . F9 F 0.4645(7) -0.8684(10) -0.0683(5) 0.090(10) Uani 0.33 1 d PD B 1 F10 F 0.3816(6) -1.0143(19) -0.0554(7) 0.084(4) Uani 0.33 1 d PDU B 1 F11 F 0.3988(8) -0.9920(19) -0.1543(4) 0.069(3) Uani 0.33 1 d PDU B 1 F12 F 0.4757(8) -1.1179(13) -0.0747(5) 0.047(3) Uani 0.33 1 d PDU . 1 F9' F 0.4687(6) -0.8667(10) -0.0712(4) 0.036(3) Uani 0.33 1 d PD B 2 F10' F 0.3728(6) -1.0080(18) -0.0695(8) 0.085(4) Uani 0.33 1 d PDU B 2 F11' F 0.4190(9) -0.9952(16) -0.1574(3) 0.076(5) Uani 0.33 1 d PDU B 2 F12' F 0.4764(8) -1.1141(12) -0.0714(6) 0.049(3) Uani 0.33 1 d PDU . 2 F9" F 0.4563(8) -0.8654(11) -0.0661(5) 0.086(8) Uani 0.33 1 d PD B 3 F10" F 0.3636(3) -0.9916(8) -0.1172(6) 0.091(2) Uani 0.33 1 d PDU B 3 F11" F 0.4584(5) -1.0049(12) -0.1506(3) 0.097(3) Uani 0.33 1 d PDU B 3 F12" F 0.4534(5) -1.1188(9) -0.0609(5) 0.075(3) Uani 0.33 1 d PDU . 3 B4 B 0.42176(14) -0.4897(3) 0.05246(13) 0.0360(5) Uani 1 1 d . . . F13 F 0.42889(8) -0.62624(16) 0.02279(8) 0.0552(4) Uani 1 1 d . B . F14 F 0.35505(8) -0.47628(19) 0.05982(8) 0.0565(4) Uani 1 1 d . B . F15 F 0.46855(9) -0.4802(2) 0.10956(8) 0.0698(5) Uani 1 1 d . B . F16 F 0.43423(8) -0.37654(16) 0.01095(8) 0.0546(4) 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 0.046(2) 0.0273(19) 0.043(2) -0.0022(16) 0.0064(17) -0.0021(16) Li2 0.043(2) 0.0312(19) 0.047(2) 0.0000(17) 0.0114(17) 0.0033(16) C1 0.0434(16) 0.105(3) 0.0525(17) -0.0095(17) 0.0131(13) 0.0166(16) O1 0.0527(11) 0.0576(11) 0.0382(9) 0.0042(8) 0.0209(8) 0.0173(9) C2 0.0619(17) 0.0511(15) 0.0441(14) 0.0015(12) 0.0278(12) 0.0175(13) C3 0.081(2) 0.0378(14) 0.0555(16) -0.0051(12) 0.0344(15) 0.0150(13) O2 0.0564(11) 0.0281(8) 0.0557(10) -0.0083(7) 0.0243(8) -0.0018(7) C4 0.0693(18) 0.0392(14) 0.0415(13) -0.0139(11) 0.0158(12) -0.0172(12) C5 0.0441(14) 0.0632(17) 0.0315(12) -0.0062(11) -0.0015(10) -0.0136(12) O3 0.0426(9) 0.0383(9) 0.0311(8) -0.0015(7) 0.0010(7) 0.0106(7) C6 0.035(2) 0.031(2) 0.037(2) 0.0045(17) -0.0011(17) 0.0055(17) C6' 0.036(6) 0.025(5) 0.048(5) 0.005(4) 0.001(4) 0.002(4) C7 0.035(2) 0.0244(18) 0.048(2) -0.0007(15) 0.0046(17) 0.0056(16) C7' 0.035(5) 0.033(5) 0.049(5) 0.002(4) -0.001(4) 0.005(4) O4 0.0411(9) 0.0337(8) 0.0363(8) -0.0054(7) 0.0091(7) 0.0055(7) C8 0.043(3) 0.050(3) 0.049(2) -0.0174(18) 0.0138(18) 0.006(2) C8' 0.039(6) 0.048(7) 0.050(5) -0.010(5) 0.013(5) 0.004(5) C9 0.0598(17) 0.074(2) 0.0399(14) -0.0132(14) 0.0200(12) 0.0018(15) O5 0.0725(13) 0.0743(14) 0.0388(10) 0.0130(9) 0.0201(9) 0.0240(11) C10 0.086(2) 0.071(2) 0.0360(14) 0.0101(14) 0.0088(14) -0.0044(17) C11 0.0677(18) 0.0534(17) 0.0352(13) 0.0043(12) -0.0005(12) 0.0013(14) O6 0.0557(10) 0.0314(8) 0.0355(8) 0.0030(7) 0.0008(7) 0.0000(7) C12 0.0488(14) 0.0272(11) 0.0517(14) 0.0069(10) 0.0087(11) -0.0015(10) C13 0.0497(14) 0.0287(12) 0.0489(14) -0.0005(10) 0.0108(11) -0.0105(10) O7 0.0401(8) 0.0313(8) 0.0350(8) -0.0029(6) 0.0052(7) -0.0097(7) C14 0.0364(12) 0.0415(13) 0.0355(12) -0.0113(10) 0.0065(9) -0.0097(10) C15 0.0353(12) 0.0454(13) 0.0314(11) -0.0087(10) 0.0053(9) -0.0054(10) O8 0.0317(8) 0.0333(8) 0.0391(8) 0.0026(7) -0.0022(6) -0.0006(6) C16 0.0323(12) 0.0551(16) 0.0452(14) 0.0142(12) 0.0023(10) 0.0092(11) C17 0.0515(15) 0.0453(14) 0.0497(15) 0.0118(12) 0.0120(12) 0.0194(12) O9 0.0507(10) 0.0291(8) 0.0539(10) 0.0028(7) 0.0128(8) 0.0028(7) C18 0.082(2) 0.0246(12) 0.0532(16) 0.0062(11) 0.0011(14) 0.0024(12) C19 0.0717(19) 0.0346(13) 0.0472(15) 0.0067(11) 0.0042(13) -0.0140(13) O10 0.0519(10) 0.0351(9) 0.0586(11) 0.0054(8) 0.0062(8) -0.0055(8) C20 0.0508(17) 0.0617(19) 0.085(2) -0.0039(17) 0.0063(15) -0.0121(14) Li3 0.043(2) 0.0279(18) 0.039(2) -0.0001(15) 0.0077(16) -0.0004(16) B1 0.0387(13) 0.0272(12) 0.0323(12) -0.0011(9) 0.0110(10) -0.0014(10) F1 0.0408(8) 0.0591(10) 0.0574(9) -0.0062(8) -0.0002(7) -0.0051(7) F2 0.0492(8) 0.0340(7) 0.0436(7) -0.0072(6) 0.0109(6) 0.0063(6) F3 0.0704(10) 0.0475(8) 0.0398(8) 0.0038(6) 0.0268(7) 0.0015(7) F4 0.0548(8) 0.0268(6) 0.0391(7) 0.0033(5) 0.0056(6) -0.0041(6) B2 0.0370(13) 0.0303(12) 0.0308(12) -0.0012(10) 0.0040(10) -0.0031(10) F5 0.0644(10) 0.0764(11) 0.0396(8) -0.0118(8) 0.0206(7) -0.0124(8) F6 0.0530(8) 0.0303(7) 0.0568(9) 0.0081(6) 0.0114(7) 0.0085(6) F7 0.0362(8) 0.0673(11) 0.0645(10) 0.0096(8) -0.0037(7) -0.0053(7) F8 0.0542(8) 0.0286(7) 0.0516(8) -0.0078(6) 0.0136(7) -0.0043(6) Li4 0.046(2) 0.0230(18) 0.040(2) 0.0003(15) 0.0036(16) 0.0000(15) B3 0.0448(15) 0.0254(12) 0.0411(14) -0.0020(11) -0.0040(11) -0.0012(11) F9 0.137(19) 0.049(14) 0.074(17) -0.012(11) 0.003(12) -0.029(12) F10 0.063(7) 0.102(8) 0.101(7) 0.020(5) 0.052(7) 0.006(6) F11 0.099(7) 0.045(5) 0.047(5) -0.003(4) -0.016(4) 0.006(5) F12 0.058(6) 0.028(5) 0.051(5) 0.004(4) 0.006(5) 0.009(5) F9' 0.057(6) 0.016(5) 0.033(5) -0.005(4) 0.008(5) -0.014(4) F10' 0.038(4) 0.079(6) 0.132(10) 0.021(7) 0.004(6) 0.006(4) F11' 0.134(12) 0.042(5) 0.028(4) 0.008(4) -0.038(5) -0.005(7) F12' 0.059(6) 0.033(5) 0.057(5) 0.016(5) 0.016(5) 0.010(5) F9" 0.106(12) 0.035(8) 0.087(13) -0.020(7) -0.047(8) 0.011(7) F10" 0.045(4) 0.070(4) 0.144(7) 0.002(5) -0.008(5) 0.004(3) F11" 0.121(7) 0.117(7) 0.057(5) -0.012(4) 0.027(5) 0.005(6) F12" 0.096(6) 0.040(3) 0.071(5) 0.018(3) -0.023(4) -0.003(4) B4 0.0386(14) 0.0314(13) 0.0381(13) 0.0004(10) 0.0085(11) 0.0012(10) F13 0.0607(10) 0.0325(8) 0.0750(11) -0.0082(7) 0.0208(8) 0.0021(7) F14 0.0439(8) 0.0655(10) 0.0638(10) 0.0118(8) 0.0202(7) 0.0105(7) F15 0.0633(11) 0.0812(13) 0.0537(10) -0.0046(9) -0.0117(8) 0.0068(9) F16 0.0595(9) 0.0386(8) 0.0665(10) 0.0091(7) 0.0158(8) -0.0120(7) _cod_database_code 4000335