# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3_mm #TrackingRef '3_mm.cif' _audit_creation_date '04-Feb-02 T09:24:53-00:00' _audit_creation_method 'XD routine XDCIF' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C30 H30 Al N3 O6, 1.5(C6 F4 I2), H2 O' _chemical_formula_sum 'C39 H32 Al F6 I3 N3 O7' _chemical_formula_weight 1176.36 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 _cell_length_a 12.8817(8) _cell_length_b 14.0348(8) _cell_length_c 14.2560(8) _cell_angle_alpha 63.3510(10) _cell_angle_beta 71.0120(10) _cell_angle_gamma 76.0780(10) _cell_volume 2164.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8510 _cell_measurement_theta_min 2.4733 _cell_measurement_theta_max 29.3882 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.262 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6480 _exptl_absorpt_correction_T_max 0.8762 _exptl_absorpt_process_details SADABS #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Incoatec microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54848 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 52.23 _reflns_number_total 48264 _reflns_number_gt 27920 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Volkov et al, (2006)' _computing_molecular_graphics 'Volkov et al, (2006)' _computing_publication_material 'Volkov et al, (2006)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w2 = 1/[s^2^(Fo^2^)] ; _refine_ls_extinction_method none _refine_ls_number_reflns 44531 _refine_ls_number_parameters 1610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.073 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_shift/su_max 0.00004 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 52.23 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.023 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.136 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_symmetry_multiplicity I(1) 0.095754(19) 0.109670(19) 0.60722(2) 0.025 1 2 I(2) 0.05933(3) -0.42551(2) 0.73286(3) 0.03 1 2 I(3) 0.24628(3) 0.87273(3) 0.07609(3) 0.037 1 2 AL(1) 0.49707(8) 0.76008(7) 0.24340(7) 0.015 1 2 F(1) -0.1097(2) -0.0183(3) 0.6653(5) 0.039 1 2 F(2) -0.1226(3) -0.2230(3) 0.7174(5) 0.042 1 2 F(3) 0.2786(2) -0.0896(3) 0.6066(5) 0.039 1 2 F(4) 0.2661(3) -0.2934(3) 0.6557(4) 0.039 1 2 F(5) 0.0694(3) 1.0556(3) 0.1270(3) 0.034 1 2 F(6) 0.1208(4) 0.8491(4) -0.0747(4) 0.041 1 2 O(1) 0.45507(13) 0.72133(14) 0.15069(14) 0.016 1 2 O(2) 0.64332(14) 0.75504(14) 0.16048(14) 0.016 1 2 O(3) 0.35074(15) 0.75791(14) 0.32674(15) 0.017 1 2 O(4) 0.52315(13) 0.61356(13) 0.33084(13) 0.015 1 2 O(5) 0.54113(15) 0.79913(14) 0.33189(14) 0.017 1 2 O(6) 0.46291(15) 0.90292(14) 0.15690(14) 0.017 1 2 O(7) 0.9967(3) 0.3552(4) -0.2032(4) 0.036 1 2 N(1) 0.8099(2) 0.4379(2) -0.0830(3) 0.032 1 2 N(2) 0.12754(18) 0.31781(19) 0.5700(2) 0.026 1 2 N(3) 0.4293(2) 1.28601(19) 0.2947(2) 0.028 1 2 C(1) 0.45101(16) 0.6031(2) 0.0764(2) 0.025 1 2 C(2) 0.51398(13) 0.65939(13) 0.10491(13) 0.016 1 2 C(3) 0.63006(13) 0.64248(12) 0.08228(12) 0.015 1 2 C(4) 0.68922(13) 0.69972(13) 0.10464(13) 0.016 1 2 C(5) 0.81138(15) 0.70188(18) 0.05855(18) 0.023 1 2 C(6) 0.69183(13) 0.57176(14) 0.02524(15) 0.018 1 2 C(7) 0.70404(17) 0.60431(18) -0.08548(17) 0.024 1 2 C(8) 0.76262(17) 0.53542(18) -0.13517(17) 0.03 1 2 C(9) 0.79865(17) 0.40600(16) 0.0238(2) 0.032 1 2 C(10) 0.74027(18) 0.46956(16) 0.08005(19) 0.026 1 2 C(11) 0.17282(15) 0.71023(18) 0.41591(19) 0.025 1 2 C(12) 0.29365(13) 0.67903(13) 0.38022(13) 0.016 1 2 C(13) 0.33869(13) 0.57085(13) 0.40560(13) 0.016 1 2 C(14) 0.45452(12) 0.54344(12) 0.37941(12) 0.014 1 2 C(15) 0.50561(14) 0.43004(13) 0.40348(15) 0.018 1 2 C(16) 0.26460(13) 0.48459(13) 0.46331(14) 0.016 1 2 C(17) 0.18753(15) 0.47876(16) 0.41649(16) 0.022 1 2 C(18) 0.12075(14) 0.39596(16) 0.47233(16) 0.026 1 2 C(19) 0.20162(14) 0.32314(13) 0.61489(14) 0.023 1 2 C(20) 0.26962(14) 0.40443(14) 0.56605(15) 0.02 1 2 C(21) 0.55805(18) 0.89017(17) 0.42862(17) 0.023 1 2 C(22) 0.52531(13) 0.88996(13) 0.33699(13) 0.016 1 2 C(23) 0.47902(14) 0.98520(13) 0.26409(13) 0.016 1 2 C(24) 0.45007(14) 0.98586(13) 0.17655(13) 0.016 1 2 C(25) 0.4016(2) 1.08674(15) 0.09921(16) 0.025 1 2 C(26) 0.46335(14) 1.08773(13) 0.27695(14) 0.017 1 2 C(27) 0.36288(16) 1.12274(15) 0.33427(15) 0.02 1 2 C(28) 0.35021(16) 1.22118(14) 0.34056(14) 0.024 1 2 C(29) 0.52612(18) 1.25184(16) 0.24123(18) 0.03 1 2 C(30) 0.54712(19) 1.15500(18) 0.2299(2) 0.027 1 2 C(31) 0.08478(15) -0.04779(16) 0.63479(17) 0.022 1 2 C(32) -0.01578(15) -0.08491(18) 0.6622(2) 0.025 1 2 C(33) -0.02258(16) -0.19167(18) 0.6890(2) 0.025 1 2 C(34) 0.07171(17) -0.26520(16) 0.68844(17) 0.023 1 2 C(35) 0.17242(16) -0.22698(18) 0.65826(19) 0.025 1 2 C(36) 0.17872(15) -0.12048(17) 0.63241(18) 0.024 1 2 C(37) 0.10049(16) 0.94874(18) 0.02930(18) 0.024 1 2 C(38) 0.03615(19) 1.02711(18) 0.06462(18) 0.024 1 2 C(39) 0.06227(19) 0.92347(18) -0.03637(19) 0.026 1 2 H(1A) 0.449272 0.52047 0.133248 0.035 1 2 H(1B) 0.490771 0.606964 -0.004165 0.035 1 2 H(1C) 0.367976 0.6425 0.078575 0.035 1 2 H(5A) 0.828 0.778235 -0.007946 0.033 1 2 H(5B) 0.844653 0.638796 0.030016 0.033 1 2 H(5C) 0.849623 0.690099 0.12039 0.033 1 2 H(7) 0.667252 0.682557 -0.132182 0.028 1 2 H(8) 0.770743 0.562071 -0.220992 0.035 1 2 H(9) 0.837193 0.327469 0.067638 0.038 1 2 H(10) 0.732306 0.439461 0.166268 0.029 1 2 H(11A) 0.160197 0.777457 0.437205 0.036 1 2 H(11B) 0.135409 0.643645 0.485177 0.036 1 2 H(11C) 0.134665 0.732302 0.350979 0.036 1 2 H(15A) 0.59422 0.428046 0.377022 0.025 1 2 H(15B) 0.477974 0.397337 0.361474 0.025 1 2 H(15C) 0.481814 0.382658 0.48942 0.025 1 2 H(17) 0.179694 0.538614 0.337308 0.025 1 2 H(18) 0.060313 0.393795 0.435564 0.03 1 2 H(19) 0.207886 0.261105 0.693619 0.027 1 2 H(20) 0.32655 0.405494 0.607099 0.022 1 2 H(21A) 0.484815 0.898983 0.489161 0.032 1 2 H(21B) 0.60535 0.956139 0.398964 0.032 1 2 H(21C) 0.606792 0.815692 0.46419 0.032 1 2 H(25A) 0.420894 1.082544 0.02166 0.035 1 2 H(25B) 0.43524 1.15451 0.090083 0.035 1 2 H(25C) 0.313258 1.095746 0.130097 0.035 1 2 H(27) 0.295097 1.073807 0.373765 0.023 1 2 H(28) 0.271467 1.246526 0.385427 0.028 1 2 H(29) 0.591813 1.303069 0.204042 0.035 1 2 H(30) 0.627168 1.132164 0.184916 0.031 1 2 H(7D) 0.99924 0.315411 -0.2457 0.059 1 2 H(7E) 0.917674 0.370363 -0.173063 0.059 1 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 I(1) 0.01822(9) 0.01922(11) 0.03518(15) -0.01083(10) -0.00558(9) -0.00099(8) I(2) 0.03583(16) 0.02016(12) 0.03510(17) -0.00833(12) -0.01561(14) -0.00253(11) I(3) 0.02607(14) 0.0466(2) 0.0376(2) -0.01604(18) -0.01678(14) 0.00881(15) AL(1) 0.0187(4) 0.0118(4) 0.0139(4) -0.0051(3) -0.0063(3) -0.0003(3) F(1) 0.0148(9) 0.0265(14) 0.0737(19) -0.0218(16) -0.0126(12) 0.0045(9) F(2) 0.0212(11) 0.0277(16) 0.081(2) -0.0202(18) -0.0197(15) -0.0042(10) F(3) 0.0143(9) 0.0270(14) 0.0662(19) -0.0146(16) -0.0050(12) -0.0019(8) F(4) 0.0227(11) 0.0200(12) 0.0608(19) -0.0133(15) -0.0035(14) 0.0052(9) F(5) 0.0364(15) 0.0400(16) 0.0386(15) -0.0219(14) -0.0181(13) -0.0025(14) F(6) 0.0430(17) 0.0381(17) 0.055(2) -0.0339(16) -0.0231(16) 0.0180(14) O(1) 0.0164(5) 0.0161(6) 0.0185(6) -0.0094(5) -0.0071(5) 0.0017(4) O(2) 0.0173(6) 0.0158(6) 0.0170(6) -0.0073(5) -0.0037(5) -0.0031(5) O(3) 0.0178(6) 0.0134(6) 0.0187(6) -0.0070(5) -0.0043(5) 0.0014(5) O(4) 0.0154(5) 0.0116(5) 0.0162(6) -0.0041(5) -0.0056(4) -0.0004(4) O(5) 0.0238(6) 0.0133(6) 0.0168(6) -0.0060(5) -0.0101(5) 0.0007(5) O(6) 0.0245(6) 0.0115(5) 0.0157(6) -0.0054(5) -0.0085(5) 0.0003(5) O(7) 0.0255(11) 0.0472(16) 0.0457(15) -0.0328(15) -0.0041(11) -0.0005(11) N(1) 0.0254(9) 0.0305(11) 0.0448(13) -0.0279(11) 0.0012(9) -0.0019(8) N(2) 0.0201(7) 0.0224(9) 0.0353(10) -0.0097(8) -0.0051(8) -0.0066(6) N(3) 0.0411(11) 0.0180(8) 0.0325(10) -0.0140(8) -0.0172(9) 0.0002(8) C(1) 0.0211(7) 0.0303(9) 0.0359(9) -0.0232(8) -0.0103(7) -0.0006(6) C(2) 0.0161(5) 0.0160(6) 0.0171(6) -0.0079(5) -0.0066(5) -0.0001(4) C(3) 0.0167(5) 0.0144(5) 0.0167(6) -0.0078(5) -0.0052(5) -0.0003(4) C(4) 0.0169(5) 0.0148(6) 0.0166(6) -0.0066(5) -0.0049(5) -0.0021(4) C(5) 0.0164(6) 0.0260(8) 0.0269(8) -0.0124(7) -0.0035(6) -0.0029(6) C(6) 0.0187(6) 0.0164(6) 0.0191(7) -0.0095(5) -0.0051(5) 0.0008(5) C(7) 0.0275(8) 0.0260(8) 0.0209(7) -0.0140(7) -0.0053(6) 0.0026(7) C(8) 0.0322(8) 0.0348(9) 0.0296(8) -0.0234(8) -0.0009(6) -0.0024(7) C(9) 0.0322(8) 0.0203(7) 0.0468(11) -0.0202(8) -0.0077(8) 0.0041(6) C(10) 0.0306(9) 0.0164(7) 0.0293(9) -0.0104(7) -0.0102(7) 0.0046(6) C(11) 0.0169(6) 0.0231(8) 0.0292(8) -0.0111(7) -0.0027(6) 0.0032(6) C(12) 0.0158(5) 0.0135(6) 0.0176(6) -0.0062(5) -0.0050(5) 0.0021(4) C(13) 0.0146(5) 0.0128(6) 0.0185(6) -0.0052(5) -0.0061(5) 0.0008(4) C(14) 0.0140(5) 0.0118(5) 0.0160(5) -0.0057(4) -0.0045(4) 0.0000(4) C(15) 0.0191(6) 0.0129(6) 0.0209(6) -0.0072(5) -0.0057(5) 0.0008(4) C(16) 0.0154(5) 0.0160(6) 0.0183(6) -0.0066(5) -0.0060(5) -0.0009(4) C(17) 0.0198(6) 0.0234(7) 0.0241(7) -0.0082(6) -0.0091(6) -0.0045(5) C(18) 0.0234(6) 0.0264(8) 0.0331(8) -0.0107(7) -0.0106(6) -0.0071(5) C(19) 0.0217(6) 0.0179(6) 0.0251(7) -0.0035(5) -0.0042(5) -0.0053(5) C(20) 0.0189(6) 0.0170(6) 0.0220(7) -0.0041(6) -0.0079(5) -0.0026(5) C(21) 0.0292(8) 0.0219(7) 0.0239(7) -0.0126(6) -0.0144(7) 0.0019(6) C(22) 0.0199(6) 0.0145(6) 0.0181(6) -0.0085(5) -0.0084(5) 0.0005(5) C(23) 0.0216(6) 0.0125(5) 0.0169(6) -0.0067(5) -0.0076(5) 0.0006(5) C(24) 0.0233(6) 0.0124(5) 0.0144(5) -0.0050(5) -0.0076(5) -0.0003(5) C(25) 0.0394(10) 0.0148(7) 0.0197(7) -0.0056(6) -0.0142(7) 0.0033(6) C(26) 0.0177(6) 0.0146(6) 0.0195(6) -0.0086(5) -0.0041(5) -0.0006(5) C(27) 0.0238(7) 0.0176(6) 0.0215(7) -0.0103(6) -0.0058(6) -0.0001(6) C(28) 0.0320(7) 0.0200(6) 0.0250(6) -0.0139(6) -0.0102(6) 0.0041(6) C(29) 0.0346(9) 0.0204(7) 0.0424(10) -0.0151(7) -0.0107(7) -0.0073(6) C(30) 0.0252(8) 0.0218(8) 0.0384(10) -0.0165(8) -0.0034(8) -0.0070(7) C(31) 0.0154(6) 0.0179(7) 0.0309(8) -0.0095(6) -0.0058(6) -0.0006(5) C(32) 0.0150(6) 0.0220(8) 0.0401(10) -0.0144(8) -0.0091(6) 0.0009(6) C(33) 0.0177(7) 0.0214(8) 0.0394(10) -0.0128(8) -0.0112(7) -0.0007(6) C(34) 0.0220(7) 0.0183(7) 0.0289(8) -0.0091(6) -0.0099(6) -0.0004(6) C(35) 0.0177(7) 0.0185(8) 0.0347(9) -0.0093(7) -0.0056(6) 0.0016(6) C(36) 0.0149(6) 0.0201(8) 0.0355(9) -0.0110(7) -0.0051(6) 0.0001(6) C(37) 0.0211(7) 0.0274(9) 0.0273(8) -0.0135(7) -0.0121(6) 0.0052(6) C(38) 0.0264(8) 0.0251(9) 0.0280(8) -0.0142(7) -0.0126(7) 0.0011(7) C(39) 0.0273(8) 0.0236(8) 0.0327(9) -0.0176(8) -0.0138(8) 0.0077(7) loop_ _atom_site_anharm_GC_C_label _atom_site_anharm_GC_C_111 _atom_site_anharm_GC_C_222 _atom_site_anharm_GC_C_333 _atom_site_anharm_GC_C_112 _atom_site_anharm_GC_C_122 _atom_site_anharm_GC_C_113 _atom_site_anharm_GC_C_133 _atom_site_anharm_GC_C_223 _atom_site_anharm_GC_C_233 _atom_site_anharm_GC_C_123 I(1) -0.000008(13) 0.000058(13) -0.00023(2) -0.000018(7) 0.000027(7) -0.000008(9) 0.000024(11) -0.000055(10) 0.000090(12) -0.000028(6) I(2) 0.00029(2) 0.000094(15) 0.00030(2) 0.000215(11) -0.000076(9) -0.000089(15) -0.000042(15) 0.000030(11) 0.000221(12) -0.000167(8) I(3) 0.000032(19) 0.00224(4) -0.00023(3) 0.000210(13) 0.000361(17) -0.000033(14) 0.000055(16) -0.00060(2) 0.00054(2) -0.000321(12) Al(1) 0.00004(6) -0.00001(5) 0.00002(5) 0.00004(3) 0.00007(3) -0.00001(3) 0.00005(3) -0.00002(3) 0.00002(3) -0.00003(2) loop_ _atom_site_anharm_GC_D_label _atom_site_anharm_GC_D_1111 _atom_site_anharm_GC_D_2222 _atom_site_anharm_GC_D_3333 _atom_site_anharm_GC_D_1112 _atom_site_anharm_GC_D_1222 _atom_site_anharm_GC_D_1113 _atom_site_anharm_GC_D_1333 _atom_site_anharm_GC_D_2223 _atom_site_anharm_GC_D_2333 _atom_site_anharm_GC_D_1122 _atom_site_anharm_GC_D_1133 _atom_site_anharm_GC_D_2233 _atom_site_anharm_GC_D_1123 _atom_site_anharm_GC_D_1223 _atom_site_anharm_GC_D_1233 I(1) 0.000091(6) 0.000052(7) 0.000206(14) 0.000014(3) 0.000009(3) -0.000050(4) -0.000075(6) -0.000021(5) -0.000054(7) 0.000031(2) 0.000065(4) 0.000029(5) -0.000023(2) -0.000019(2) 0.000027(3) I(2) 0.000210(14) 0.000055(8) 0.000245(15) -0.000013(6) -0.000004(4) -0.000113(9) -0.000138(9) -0.000012(5) -0.000011(7) 0.000039(4) 0.000126(7) 0.000045(5) -0.000003(4) -0.000023(3) 0.000000(4) I(3) 0.000151(11) 0.00042(2) 0.000269(18) 0.000047(7) 0.000133(10) -0.000095(8) -0.000130(10) -0.000209(13) -0.000146(11) 0.000095(6) 0.000121(7) 0.000180(10) -0.000067(5) -0.000100(6) 0.000082(6) Al(1) 0.00010(3) 0.00005(2) 0.00001(3) -0.000032(14) 0.000022(12) 0.000006(16) -0.000001(16) -0.000020(15) -0.000010(16) -0.000002(10) -0.000001(13) 0.000014(14) 0.000006(9) -0.000015(8) -0.000002(9) #----------------------------------------------------------------------------# # MULTIPOLE PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_rho_multipole_atom_label _atom_rho_multipole_coeff_Pv _atom_rho_multipole_coeff_P00 _atom_rho_multipole_coeff_P11 _atom_rho_multipole_coeff_P1-1 _atom_rho_multipole_coeff_P10 _atom_rho_multipole_coeff_P20 _atom_rho_multipole_coeff_P21 _atom_rho_multipole_coeff_P2-1 _atom_rho_multipole_coeff_P22 _atom_rho_multipole_coeff_P2-2 _atom_rho_multipole_coeff_P30 _atom_rho_multipole_coeff_P31 _atom_rho_multipole_coeff_P3-1 _atom_rho_multipole_coeff_P32 _atom_rho_multipole_coeff_P3-2 _atom_rho_multipole_coeff_P33 _atom_rho_multipole_coeff_P3-3 _atom_rho_multipole_coeff_P40 _atom_rho_multipole_coeff_P41 _atom_rho_multipole_coeff_P4-1 _atom_rho_multipole_coeff_P42 _atom_rho_multipole_coeff_P4-2 _atom_rho_multipole_coeff_P43 _atom_rho_multipole_coeff_P4-3 _atom_rho_multipole_coeff_P44 _atom_rho_multipole_coeff_P4-4 _atom_rho_multipole_kappa _atom_rho_multipole_kappa_prime0 _atom_rho_multipole_kappa_prime1 _atom_rho_multipole_kappa_prime2 _atom_rho_multipole_kappa_prime3 _atom_rho_multipole_kappa_prime4 _atom_rho_multipole_radial_slater_n0 _atom_rho_multipole_radial_slater_zeta0 _atom_rho_multipole_radial_slater_n1 _atom_rho_multipole_radial_slater_zeta1 _atom_rho_multipole_radial_slater_n2 _atom_rho_multipole_radial_slater_zeta2 _atom_rho_multipole_radial_slater_n3 _atom_rho_multipole_radial_slater_zeta3 _atom_rho_multipole_radial_slater_n4 _atom_rho_multipole_radial_slater_zeta4 I(1) 6.80(6) 0 0.02(4) 0.06(4) -0.08(4) -0.36(5) 0.12(4) -0.02(4) -0.22(4) 0.30(4) 0.15(5) 0.06(5) -0.02(5) -0.06(4) -0.10(4) 0.02(4) 0.09(4) 0.13(6) 0.21(6) -0.24(5) 0.44(5) -0.18(5) 0.05(5) -0.10(5) 0.20(5) -0.27(5) 1.158393 1.105468 1.105468 1.105468 1.105468 1.105468 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 I(2) 6.81(7) 0 -0.02(4) 0.01(4) 0.04(4) -0.46(5) -0.24(4) -0.11(4) -0.17(4) -0.14(4) 0.17(5) -0.11(5) 0.00(5) -0.12(5) -0.04(5) 0.12(5) 0.16(5) 0.05(6) -0.18(6) -0.02(6) 0.53(6) 0.20(6) -0.03(6) 0.07(6) 0.30(6) 0.14(6) 1.158393 1.105468 1.105468 1.105468 1.105468 1.105468 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 I(3) 6.69(6) 0 -0.06(5) -0.01(4) -0.17(4) -0.17(5) 0.41(5) 0.08(5) -0.25(5) -0.01(5) 0.03(5) 0.19(5) -0.10(5) -0.10(5) -0.21(5) -0.03(5) 0.09(5) 0.19(7) 0.37(6) 0.17(6) 0.31(6) 0.33(6) -0.15(6) 0.21(6) 0.11(7) 0.23(7) 1.158393 1.105468 1.105468 1.105468 1.105468 1.105468 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 8 4.8152571428571 AL(1) 1.52(9) 0 -0.17(8) 0.02(8) 0.04(8) -0.19(10) 0.10(7) -0.18(7) -0.03(10) 0.08(7) 0.19(10) 0.07(8) 0.25(8) 0.05(8) -0.23(7) -0.14(9) -0.10(9) 0.68(10) -0.14(10) -0.05(9) -0.14(10) 0.07(8) -0.04(8) -0.01(8) 0.56(9) -0.04(9) 1.291171 0.892124 0.892124 0.892124 0.892124 0.892124 4 2.505 4 2.505 4 2.505 4 2.505 4 2.505 F(1) 7.08(5) 0 -0.25(9) -0.06(6) -0.02(5) 0.14(6) 0.04(9) -0.03(6) -0.27(9) 0.09(11) -0.13(5) 0.02(5) -0.01(4) 0.13(5) 0.02(5) -0.06(5) 0.07(5) 0 0 0 0 0 0 0 0 0 1.006513 1.011957 1.011957 1.011957 1.011957 1.011957 2 5.186 2 5.186 2 5.186 3 5.186 4 5.186 F(2) 7.12(5) 0 0.03(10) -0.04(7) 0.07(6) 0.20(8) -0.20(10) 0.08(7) -0.34(10) 0.03(11) -0.04(5) -0.02(5) -0.06(4) 0.01(5) -0.08(5) 0.01(6) -0.09(6) 0 0 0 0 0 0 0 0 0 1.006513 1.011957 1.011957 1.011957 1.011957 1.011957 2 5.186 2 5.186 2 5.186 3 5.186 4 5.186 F(3) 6.93(5) 0 0.14(9) 0.03(6) 0.03(6) 0.04(7) -0.12(9) -0.06(7) 0.04(9) 0.06(10) -0.07(5) 0.02(5) 0.01(4) 0.06(5) 0.02(5) -0.06(5) 0.03(5) 0 0 0 0 0 0 0 0 0 1.006513 1.011957 1.011957 1.011957 1.011957 1.011957 2 5.186 2 5.186 2 5.186 3 5.186 4 5.186 F(4) 7.17(5) 0 -0.21(9) -0.10(7) 0.04(6) 0.06(7) 0.27(9) 0.16(7) -0.18(10) -0.14(11) 0.05(5) 0.15(5) 0.12(4) -0.02(5) 0.01(5) 0.07(5) -0.04(5) 0 0 0 0 0 0 0 0 0 1.006513 1.011957 1.011957 1.011957 1.011957 1.011957 2 5.186 2 5.186 2 5.186 3 5.186 4 5.186 F(5) 7.01(5) 0 0.00(8) -0.22(7) -0.03(6) -0.08(8) -0.06(9) -0.20(8) -0.10(10) 0.14(10) -0.03(5) -0.05(4) 0.07(4) 0.04(4) -0.05(4) -0.02(5) 0.06(5) 0 0 0 0 0 0 0 0 0 1.006513 1.011957 1.011957 1.011957 1.011957 1.011957 2 5.186 2 5.186 2 5.186 3 5.186 4 5.186 F(6) 6.93(5) 0 -0.18(10) 0.26(7) 0.14(6) -0.02(8) -0.08(10) -0.06(8) -0.14(11) -0.05(12) -0.13(5) 0.05(5) -0.01(4) 0.16(5) 0.03(5) -0.02(6) -0.10(6) 0 0 0 0 0 0 0 0 0 1.006513 1.011957 1.011957 1.011957 1.011957 1.011957 2 5.186 2 5.186 2 5.186 3 5.186 4 5.186 O(1) 6.53(7) 0 -0.03(4) 0.02(4) -0.05(5) 0.08(5) 0.02(4) 0.01(4) -0.14(4) 0.04(4) 0.12(4) 0.00(4) -0.04(3) -0.03(3) 0.01(3) 0.01(3) 0.00(3) 0 0 0 0 0 0 0 0 0 0.961384 0.932874 0.932874 0.932874 0.932874 0.932874 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 O(2) 6.46(7) 0 -0.04(4) -0.11(4) -0.04(5) 0.06(5) -0.06(5) -0.07(4) -0.16(4) 0.05(4) 0.06(4) -0.06(4) -0.02(4) 0.03(3) -0.06(3) 0.00(3) 0.00(3) 0 0 0 0 0 0 0 0 0 0.961384 0.932874 0.932874 0.932874 0.932874 0.932874 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 O(3) 6.47(7) 0 -0.04(4) 0.02(4) -0.05(5) -0.03(5) 0.06(5) -0.02(4) -0.10(4) 0.01(4) -0.01(4) 0.01(4) -0.06(4) 0.03(4) 0.07(4) -0.04(3) -0.02(3) 0 0 0 0 0 0 0 0 0 0.961384 0.932874 0.932874 0.932874 0.932874 0.932874 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 O(4) 6.57(6) 0 0.02(4) -0.02(4) -0.07(5) 0.01(5) 0.04(4) -0.01(4) -0.05(4) 0.02(4) 0.11(4) -0.02(3) -0.09(3) -0.04(3) 0.02(3) 0.00(3) 0.00(3) 0 0 0 0 0 0 0 0 0 0.961384 0.932874 0.932874 0.932874 0.932874 0.932874 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 O(5) 6.43(7) 0 0.04(4) 0.00(4) -0.06(5) -0.13(5) 0.00(5) -0.03(4) -0.08(4) -0.03(4) 0.13(4) -0.02(4) -0.03(3) 0.03(4) 0.05(4) 0.01(3) 0.02(3) 0 0 0 0 0 0 0 0 0 0.961384 0.932874 0.932874 0.932874 0.932874 0.932874 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 O(6) 6.47(7) 0 0.04(4) 0.02(4) -0.02(5) 0.03(5) 0.01(5) -0.02(4) -0.03(4) 0.01(4) 0.04(4) -0.01(4) 0.01(3) -0.04(3) 0.03(3) 0.04(3) 0.04(3) 0 0 0 0 0 0 0 0 0 0.961384 0.932874 0.932874 0.932874 0.932874 0.932874 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 O(7) 7.11(10) 0 0.09(6) 0.24(6) 0.17(6) -0.02(6) 0.05(6) -0.01(5) -0.07(7) 0.16(7) 0.01(5) 0.08(5) -0.14(4) 0.00(5) 0.14(5) 0.04(5) 0.11(5) 0 0 0 0 0 0 0 0 0 0.835481 1 1 1 1 1 2 4.4974 2 4.4974 2 4.4974 3 4.4974 4 4.4974 N(1) 5.09(7) 0 -0.04(4) -0.09(4) -0.19(4) -0.06(6) -0.06(6) 0.09(5) -0.17(5) 0.06(5) 0.06(5) 0.06(5) 0.04(5) -0.03(5) 0.00(4) 0.05(4) 0.07(4) 0 0 0 0 0 0 0 0 0 0.997649 1.052497 1.052497 1.052497 1.052497 1.052497 2 3.81056 2 3.81056 2 3.81056 3 3.81056 4 3.81056 N(2) 5.04(6) 0 -0.06(4) -0.18(4) 0.01(4) -0.10(5) 0.01(5) 0.05(5) -0.04(4) -0.02(4) 0.18(5) -0.05(4) -0.05(4) 0.09(4) 0.02(4) 0.03(4) 0.02(4) 0 0 0 0 0 0 0 0 0 0.997649 1.052497 1.052497 1.052497 1.052497 1.052497 2 3.81056 2 3.81056 2 3.81056 3 3.81056 4 3.81056 N(3) 5.10(6) 0 -0.02(4) -0.10(4) -0.02(4) 0.03(5) -0.05(5) 0.02(5) -0.16(4) -0.04(5) 0.09(5) 0.07(4) -0.02(4) -0.06(4) -0.06(4) 0.04(4) 0.03(4) 0 0 0 0 0 0 0 0 0 0.997649 1.052497 1.052497 1.052497 1.052497 1.052497 2 3.81056 2 3.81056 2 3.81056 3 3.81056 4 3.81056 C(1) 4.72(13) 0 -0.03(5) -0.05(6) 0.11(6) 0.09(6) -0.01(5) 0.06(5) 0.03(6) -0.08(5) 0.06(6) -0.13(5) 0.06(5) -0.24(5) 0.29(5) -0.05(5) -0.13(5) 0 0 0 0 0 0 0 0 0 0.960389 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(2) 3.95(9) 0 0.00(4) 0.10(5) -0.11(5) 0.17(6) 0.11(4) -0.06(5) -0.27(5) 0.09(4) 0.25(6) 0.03(5) 0.03(6) 0.20(5) -0.03(5) 0.02(5) 0.04(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(3) 4.08(10) 0 0.03(4) 0.02(5) -0.07(5) 0.05(5) 0.05(5) 0.13(5) -0.08(5) 0.07(5) 0.14(6) -0.06(5) -0.09(6) 0.21(5) 0.02(5) 0.08(5) -0.13(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(4) 3.91(9) 0 -0.06(4) 0.08(5) 0.03(5) 0.23(6) -0.12(5) -0.14(5) -0.25(5) 0.01(5) 0.35(6) -0.06(5) 0.11(6) 0.23(5) 0.12(5) 0.02(5) 0.06(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(5) 4.67(13) 0 0.10(5) 0.05(6) 0.05(6) 0.03(6) -0.04(5) 0.06(5) 0.18(6) 0.04(5) 0.06(6) 0.00(5) 0.26(5) -0.24(5) -0.35(5) 0.14(5) -0.15(5) 0 0 0 0 0 0 0 0 0 0.960389 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(6) 4.27(11) 0 0.02(4) 0.05(6) 0.01(6) 0.32(6) -0.09(5) 0.06(6) -0.10(5) 0.11(5) 0.23(6) 0.03(5) -0.02(6) 0.23(5) -0.10(5) 0.02(5) -0.13(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(7) 3.78(10) 0 0.00(4) 0.00(5) -0.03(6) -0.05(6) 0.11(5) 0.06(5) -0.14(5) 0.11(5) 0.00(6) 0.00(5) 0.07(5) 0.10(5) 0.08(5) -0.02(5) -0.03(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(8) 4.2009 0 0.0068 0.0629 -0.0926 0.0684 0.0184 0.0318 -0.207 0.0103 0.2582 -0.034 -0.0044 0.1897 -0.0056 -0.0132 -0.0581 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(9) 4.2009 0 0.0068 0.0629 -0.0926 0.0684 0.0184 0.0318 -0.207 0.0103 0.2582 -0.034 -0.0044 0.1897 -0.0056 -0.0132 -0.0581 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(10) 3.86(11) 0 0.00(4) 0.06(5) -0.10(6) 0.09(6) -0.08(5) 0.01(5) -0.15(5) -0.07(5) 0.31(6) -0.01(5) -0.05(5) 0.06(5) 0.01(5) 0.04(5) -0.01(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(11) 4.83(13) 0 0.18(6) 0.03(6) 0.09(6) 0.04(7) 0.07(5) -0.05(5) 0.05(6) 0.01(5) 0.28(6) -0.05(5) 0.03(5) -0.09(5) -0.09(5) -0.04(5) -0.32(5) 0 0 0 0 0 0 0 0 0 0.960389 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(12) 3.98(10) 0 -0.03(4) 0.09(5) -0.05(6) 0.25(6) 0.09(5) -0.01(5) -0.25(5) 0.00(4) 0.37(6) -0.03(5) 0.04(6) 0.24(5) -0.04(5) 0.01(5) 0.11(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(13) 4.33(10) 0 -0.13(4) -0.13(5) 0.10(5) 0.13(5) -0.05(5) 0.15(5) -0.21(5) 0.06(5) 0.18(6) -0.01(5) 0.08(6) 0.22(5) -0.06(5) 0.00(5) 0.01(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(14) 4.01(9) 0 0.02(4) 0.15(5) -0.03(5) 0.24(5) 0.06(4) -0.12(5) -0.22(4) -0.14(4) 0.21(6) 0.06(5) 0.07(6) 0.24(5) 0.00(5) 0.04(5) 0.08(4) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(15) 4.81(12) 0 -0.10(5) 0.02(5) 0.05(5) 0.06(5) 0.07(4) -0.01(4) -0.05(5) -0.04(5) 0.31(5) -0.06(4) 0.05(4) -0.12(5) 0.10(5) 0.02(4) -0.17(5) 0 0 0 0 0 0 0 0 0 0.960389 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(16) 3.80(10) 0 0.05(4) 0.11(6) 0.07(5) 0.12(6) -0.05(5) -0.12(6) -0.07(5) -0.01(5) 0.27(6) -0.02(5) -0.05(6) 0.16(5) -0.02(5) -0.03(5) 0.04(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(17) 4.17(10) 0 0.04(4) 0.00(5) -0.03(6) -0.03(6) 0.01(4) 0.04(5) -0.16(5) 0.03(5) 0.18(6) 0.09(5) -0.04(5) 0.25(5) -0.04(5) -0.15(5) -0.06(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(18) 4.20(5) 0 0.007(19) 0.06(3) -0.09(3) 0.07(3) 0.02(2) 0.03(3) -0.21(3) 0.01(2) 0.26(3) -0.03(2) 0.00(3) 0.19(3) -0.01(2) -0.01(2) -0.06(2) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(19) 4.2009 0 0.0068 0.0629 -0.0926 0.0684 0.0184 0.0318 -0.207 0.0103 0.2582 -0.034 -0.0044 0.1897 -0.0056 -0.0132 -0.0581 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(20) 4.33(10) 0 -0.01(4) 0.02(5) -0.02(6) 0.13(6) -0.16(4) 0.10(5) -0.13(5) 0.03(5) 0.22(5) -0.09(4) -0.05(5) 0.26(5) 0.07(5) 0.11(5) 0.02(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(21) 4.91(13) 0 -0.07(5) -0.08(6) 0.12(6) 0.07(6) 0.01(5) -0.07(5) 0.06(5) 0.09(5) 0.02(6) -0.12(5) 0.17(5) -0.21(5) 0.22(5) -0.08(5) -0.10(5) 0 0 0 0 0 0 0 0 0 0.960389 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(22) 3.84(9) 0 -0.05(4) 0.05(5) -0.04(5) 0.22(6) -0.02(5) -0.02(5) -0.22(5) 0.08(5) 0.29(6) 0.02(5) 0.10(6) 0.21(5) -0.07(5) -0.03(5) 0.01(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(23) 3.87(10) 0 -0.09(4) -0.03(5) 0.02(5) 0.12(5) -0.10(5) 0.06(5) 0.01(5) -0.10(5) 0.09(6) -0.04(5) 0.10(6) 0.21(5) 0.05(5) 0.04(5) -0.04(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(24) 3.89(9) 0 0.03(4) 0.20(5) 0.01(5) 0.11(6) 0.06(5) -0.02(5) -0.30(5) -0.03(5) 0.43(6) -0.04(5) 0.04(6) 0.27(5) 0.09(5) 0.02(5) -0.05(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(25) 4.38(13) 0 -0.02(5) 0.05(7) 0.09(6) 0.06(6) -0.02(5) -0.03(5) -0.04(6) 0.04(5) 0.14(6) -0.10(5) 0.18(5) -0.29(5) 0.28(5) -0.02(5) -0.07(5) 0 0 0 0 0 0 0 0 0 0.960389 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(26) 4.36(11) 0 -0.03(4) 0.12(6) 0.09(6) 0.38(6) -0.14(5) -0.05(6) -0.27(5) 0.03(5) 0.29(6) -0.05(5) -0.09(6) 0.33(5) 0.00(5) -0.02(5) 0.04(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(27) 3.76(10) 0 0.02(4) 0.05(5) -0.05(6) 0.20(6) -0.02(4) 0.01(5) -0.13(5) -0.01(5) 0.24(6) 0.04(5) -0.02(5) 0.13(5) 0.03(5) -0.05(5) 0.07(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(28) 4.2009 0 0.0068 0.0629 -0.0926 0.0684 0.0184 0.0318 -0.207 0.0103 0.2582 -0.034 -0.0044 0.1897 -0.0056 -0.0132 -0.0581 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(29) 4.2009 0 0.0068 0.0629 -0.0926 0.0684 0.0184 0.0318 -0.207 0.0103 0.2582 -0.034 -0.0044 0.1897 -0.0056 -0.0132 -0.0581 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(30) 4.05(11) 0 0.14(4) 0.05(5) 0.07(6) 0.12(6) 0.03(5) -0.03(5) -0.21(5) -0.06(5) 0.24(6) -0.01(5) -0.10(5) 0.15(5) 0.05(5) -0.06(5) -0.09(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(31) 4.06(11) 0 -0.01(4) 0.00(5) -0.07(6) 0.20(6) -0.06(5) 0.04(6) -0.23(5) 0.04(5) 0.12(6) -0.02(6) -0.01(6) 0.15(6) -0.04(6) -0.01(5) -0.02(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(32) 4.04(12) 0 -0.08(5) 0.07(7) -0.04(5) 0.13(6) 0.02(5) -0.08(6) -0.19(6) 0.01(6) 0.43(6) 0.01(5) -0.05(6) 0.10(6) -0.02(6) 0.06(6) -0.06(6) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(33) 3.86(12) 0 -0.01(5) 0.08(7) -0.14(6) 0.07(6) -0.02(5) 0.05(6) -0.28(6) 0.06(6) 0.24(7) -0.03(6) -0.11(7) 0.08(6) 0.05(6) 0.09(6) -0.09(6) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(34) 4.07(11) 0 0.01(5) -0.13(6) 0.14(6) 0.10(6) 0.03(5) 0.01(6) -0.18(5) 0.01(5) 0.26(6) 0.04(6) -0.09(7) 0.12(6) -0.05(6) -0.09(5) 0.07(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(35) 3.94(12) 0 0.01(5) -0.22(7) -0.14(6) 0.10(6) 0.14(5) 0.06(6) -0.35(6) -0.11(6) 0.22(7) -0.03(6) -0.03(7) 0.22(6) 0.13(6) 0.13(6) 0.14(6) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(36) 4.11(11) 0 -0.02(5) 0.11(7) -0.10(6) 0.09(6) 0.08(5) 0.03(6) -0.29(6) -0.25(6) 0.46(7) -0.02(6) 0.01(6) 0.22(6) 0.07(6) 0.02(6) -0.07(6) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(37) 4.31(11) 0 -0.07(5) 0.10(6) -0.15(7) 0.08(7) -0.13(6) 0.06(6) -0.27(5) 0.14(5) 0.06(6) 0.11(6) -0.01(7) 0.13(6) -0.12(6) -0.09(5) -0.03(5) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(38) 4.00(11) 0 -0.02(5) -0.12(7) 0.00(6) 0.00(6) -0.01(5) 0.07(7) -0.07(6) -0.09(6) 0.33(7) -0.02(6) -0.01(7) 0.09(6) -0.04(6) 0.18(6) 0.17(6) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 C(39) 4.07(11) 0 0.16(5) 0.20(7) -0.08(6) 0.04(6) 0.02(5) 0.04(6) -0.25(6) 0.00(6) 0.26(7) 0.02(6) -0.04(7) 0.02(6) 0.17(6) 0.03(6) -0.05(6) 0 0 0 0 0 0 0 0 0 1.002256 1 1 1 1 1 2 3.1303 2 3.1303 2 3.1303 3 3.1303 4 3.1303 H(1A) 0.76(8) 0 0 0 0.12(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(1B) 0.60(8) 0 0 0 0.09(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(1C) 0.79(8) 0 0 0 0.26(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(5A) 0.68(8) 0 0 0 0.24(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(5B) 0.51(8) 0 0 0 0.12(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(5C) 0.70(8) 0 0 0 0.20(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(7) 0.96(7) 0 0 0 0.25(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(8) 0.90(5) 0 0 0 0.25(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(9) 0.68(5) 0 0 0 0.17(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(10) 0.87(7) 0 0 0 0.18(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(11A) 0.76(8) 0 0 0 0.11(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(11B) 0.73(8) 0 0 0 0.05(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(11C) 0.60(8) 0 0 0 0.00(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(15A) 0.71(7) 0 0 0 0.06(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(15B) 0.75(7) 0 0 0 0.10(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(15C) 0.71(7) 0 0 0 0.04(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(17) 0.87(7) 0 0 0 0.16(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(18) 0.94(5) 0 0 0 0.19(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(19) 0.86(5) 0 0 0 0.12(3) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(20) 0.82(7) 0 0 0 0.06(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(21A) 0.51(8) 0 0 0 0.01(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(21B) 0.56(8) 0 0 0 0.20(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(21C) 0.72(8) 0 0 0 0.23(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(25A) 0.68(8) 0 0 0 0.21(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(25B) 0.73(8) 0 0 0 0.19(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(25C) 0.82(8) 0 0 0 0.25(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(27) 0.75(7) 0 0 0 0.15(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(28) 0.91(5) 0 0 0 0.22(3) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(29) 0.87(5) 0 0 0 0.21(4) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(30) 0.79(7) 0 0 0 0.09(5) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(7D) 0.46(7) 0 0 0 -0.03(6) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 H(7E) 0.43(7) 0 0 0 -0.08(6) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 1.21957 1.2 1.2 1.2 1.2 1.2 0 1.9154 1 1.9154 2 1.9154 3 1.9154 4 1.9154 loop_ _atom_local_axes_atom_label _atom_local_axes_atom0 _atom_local_axes_ax1 _atom_local_axes_atom1 _atom_local_axes_atom2 _atom_local_axes_ax2 I(1) C(31) Z I(1) N(2) Y I(2) C(34) Z I(2) C(33) Y I(3) C(37) Z I(3) C(38) Y AL(1) O(6) Z AL(1) O(5) Y F(1) C(32) Z F(1) C(33) Y F(2) C(33) Z F(2) C(32) Y F(3) C(36) Z F(3) C(35) Y F(4) C(35) Z F(4) C(36) Y F(5) C(38) Z F(5) C(37) Y F(6) C(39) Z F(6) C(37) Y O(1) C(2) Z O(1) AL(1) Y O(2) C(4) Z O(2) AL(1) Y O(3) C(12) Z O(3) AL(1) Y O(4) C(14) Z O(4) AL(1) Y O(5) C(22) Z O(5) AL(1) Y O(6) C(24) Z O(6) AL(1) Y O(7) H(7E) Z O(7) H(7D) Y N(1) C(8) Z N(1) C(9) Y N(2) C(18) Z N(2) C(19) Y N(3) C(29) Z N(3) C(28) Y C(1) H(1B) Z C(1) H(1A) Y C(2) O(1) Z C(2) C(3) Y C(3) C(2) Z C(3) C(4) Y C(4) O(2) Z C(4) C(3) Y C(5) H(5C) Z C(5) H(5A) Y C(6) C(7) Z C(6) C(10) Y C(7) H(7) Z C(7) C(6) Y C(8) H(8) Z C(8) N(1) Y C(9) H(9) Z C(9) N(1) Y C(10) H(10) Z C(10) C(9) Y C(11) H(11C) Z C(11) H(11A) Y C(12) O(3) Z C(12) C(13) Y C(13) C(14) Z C(13) C(12) Y C(14) O(4) Z C(14) C(13) Y C(15) H(15A) Z C(15) H(15C) Y C(16) C(17) Z C(16) C(20) Y C(17) H(17) Z C(17) C(18) Y C(18) H(18) Z C(18) N(2) Y C(19) H(19) Z C(19) N(2) Y C(20) H(20) Z C(20) C(19) Y C(21) H(21A) Z C(21) H(21C) Y C(22) O(5) Z C(22) C(23) Y C(23) C(22) Z C(23) C(24) Y C(24) O(6) Z C(24) C(23) Y C(25) H(25A) Z C(25) H(25C) Y C(26) C(27) Z C(26) C(30) Y C(27) H(27) Z C(27) C(28) Y C(28) H(28) Z C(28) N(3) Y C(29) H(29) Z C(29) N(3) Y C(30) H(30) Z C(30) C(29) Y C(31) C(32) Z C(31) C(36) Y C(32) F(1) Z C(32) C(31) Y C(33) F(2) Z C(33) C(32) Y C(34) C(33) Z C(34) C(35) Y C(35) F(4) Z C(35) C(36) Y C(36) F(3) Z C(36) C(35) Y C(37) C(39) Z C(37) C(38) Y C(38) F(5) Z C(38) C(37) Y C(39) F(6) Z C(39) C(37) Y H(1A) C(1) Z H(1A) H(1C) Y H(1B) C(1) Z H(1B) H(1C) Y H(1C) C(1) Z H(1C) H(1B) Y H(5A) C(5) Z H(5A) H(5C) Y H(5B) C(5) Z H(5B) H(5A) Y H(5C) C(5) Z H(5C) H(5A) Y H(7) C(7) Z H(7) C(6) Y H(8) C(8) Z H(8) N(1) Y H(9) C(9) Z H(9) N(1) Y H(10) C(10) Z H(10) C(9) Y H(11A) C(11) Z H(11A) H(11C) Y H(11B) C(11) Z H(11B) H(11C) Y H(11C) C(11) Z H(11C) H(11A) Y H(15A) C(15) Z H(15A) H(15B) Y H(15B) C(15) Z H(15B) H(15C) Y H(15C) C(15) Z H(15C) H(15B) Y H(17) C(17) Z H(17) C(18) Y H(18) C(18) Z H(18) N(2) Y H(19) C(19) Z H(19) N(2) Y H(20) C(20) Z H(20) C(19) Y H(21A) C(21) Z H(21A) H(21B) Y H(21B) C(21) Z H(21B) H(21A) Y H(21C) C(21) Z H(21C) H(21A) Y H(25A) C(25) Z H(25A) H(25C) Y H(25B) C(25) Z H(25B) H(25A) Y H(25C) C(25) Z H(25C) H(25A) Y H(27) C(27) Z H(27) C(28) Y H(28) C(28) Z H(28) N(3) Y H(29) C(29) Z H(29) N(3) Y H(30) C(30) Z H(30) C(29) Y H(7D) O(7) Z H(7D) H(7E) Y H(7E) O(7) Z H(7E) H(7D) Y #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I(1) C(31) 2.096(2) 1_555 1_555 yes I(2) C(34) 2.078(2) 1_555 1_555 yes I(3) C(37) 2.0791(18) 1_555 1_555 yes AL(1) O(1) 1.8940(18) 1_555 1_555 yes AL(1) O(2) 1.874(2) 1_555 1_555 yes AL(1) O(3) 1.872(2) 1_555 1_555 yes AL(1) O(4) 1.8805(18) 1_555 1_555 yes AL(1) O(5) 1.8573(19) 1_555 1_555 yes AL(1) O(6) 1.8558(19) 1_555 1_555 yes F(1) C(32) 1.340(3) 1_555 1_555 yes F(2) C(33) 1.338(4) 1_555 1_555 yes F(3) C(36) 1.340(4) 1_555 1_555 yes F(4) C(35) 1.337(3) 1_555 1_555 yes F(5) C(38) 1.336(3) 1_555 1_555 yes F(6) C(39) 1.349(4) 1_555 1_555 yes O(1) C(2) 1.275(2) 1_555 1_555 yes O(2) C(4) 1.270(2) 1_555 1_555 yes O(3) C(12) 1.272(2) 1_555 1_555 yes O(4) C(14) 1.280(2) 1_555 1_555 yes O(5) C(22) 1.273(2) 1_555 1_555 yes O(6) C(24) 1.277(2) 1_555 1_555 yes N(1) C(8) 1.333(4) 1_555 1_555 yes N(1) C(9) 1.347(4) 1_555 1_555 yes N(2) C(18) 1.346(3) 1_555 1_555 yes N(2) C(19) 1.342(3) 1_555 1_555 yes N(3) C(28) 1.332(4) 1_555 1_555 yes N(3) C(29) 1.337(4) 1_555 1_555 yes C(1) C(2) 1.502(2) 1_555 1_555 yes C(1) H(1A) 1.077 1_555 1_555 yes C(1) H(1B) 1.077 1_555 1_555 yes C(1) H(1C) 1.077 1_555 1_555 yes C(2) C(3) 1.407(2) 1_555 1_555 yes C(3) C(4) 1.418(2) 1_555 1_555 yes C(3) C(6) 1.484(2) 1_555 1_555 yes C(4) C(5) 1.497(2) 1_555 1_555 yes C(5) H(5A) 1.077 1_555 1_555 yes C(5) H(5B) 1.077 1_555 1_555 yes C(5) H(5C) 1.077 1_555 1_555 yes C(6) C(7) 1.397(2) 1_555 1_555 yes C(6) C(10) 1.392(2) 1_555 1_555 yes C(7) C(8) 1.386(3) 1_555 1_555 yes C(7) H(7) 1.083 1_555 1_555 yes C(8) H(8) 1.083 1_555 1_555 yes C(9) C(10) 1.390(3) 1_555 1_555 yes C(9) H(9) 1.083 1_555 1_555 yes C(10) H(10) 1.083 1_555 1_555 yes C(11) C(12) 1.493(2) 1_555 1_555 yes C(11) H(11A) 1.077 1_555 1_555 yes C(11) H(11B) 1.077 1_555 1_555 yes C(11) H(11C) 1.077 1_555 1_555 yes C(12) C(13) 1.412(2) 1_555 1_555 yes C(13) C(14) 1.416(2) 1_555 1_555 yes C(13) C(16) 1.485(2) 1_555 1_555 yes C(14) C(15) 1.496(2) 1_555 1_555 yes C(15) H(15A) 1.077 1_555 1_555 yes C(15) H(15B) 1.077 1_555 1_555 yes C(15) H(15C) 1.077 1_555 1_555 yes C(16) C(17) 1.399(2) 1_555 1_555 yes C(16) C(20) 1.401(2) 1_555 1_555 yes C(17) C(18) 1.389(3) 1_555 1_555 yes C(17) H(17) 1.083 1_555 1_555 yes C(18) H(18) 1.083 1_555 1_555 yes C(19) C(20) 1.388(2) 1_555 1_555 yes C(19) H(19) 1.083 1_555 1_555 yes C(20) H(20) 1.083 1_555 1_555 yes C(21) C(22) 1.499(2) 1_555 1_555 yes C(21) H(21A) 1.077 1_555 1_555 yes C(21) H(21B) 1.077 1_555 1_555 yes C(21) H(21C) 1.077 1_555 1_555 yes C(22) C(23) 1.413(2) 1_555 1_555 yes C(23) C(24) 1.410(2) 1_555 1_555 yes C(23) C(26) 1.489(2) 1_555 1_555 yes C(24) C(25) 1.494(2) 1_555 1_555 yes C(25) H(25A) 1.077 1_555 1_555 yes C(25) H(25B) 1.077 1_555 1_555 yes C(25) H(25C) 1.077 1_555 1_555 yes C(26) C(27) 1.397(2) 1_555 1_555 yes C(26) C(30) 1.399(3) 1_555 1_555 yes C(27) C(28) 1.392(2) 1_555 1_555 yes C(27) H(27) 1.083 1_555 1_555 yes C(28) H(28) 1.083 1_555 1_555 yes C(29) C(30) 1.392(3) 1_555 1_555 yes C(29) H(29) 1.083 1_555 1_555 yes C(30) H(30) 1.083 1_555 1_555 yes C(31) C(32) 1.384(3) 1_555 1_555 yes C(31) C(36) 1.384(2) 1_555 1_555 yes C(32) C(33) 1.388(3) 1_555 1_555 yes C(33) C(34) 1.392(3) 1_555 1_555 yes C(34) C(35) 1.386(3) 1_555 1_555 yes C(35) C(36) 1.386(3) 1_555 1_555 yes C(37) C(38) 1.392(3) 1_555 1_555 yes C(37) C(39) 1.388(3) 1_555 1_555 yes C(38) C(39) 1.382(3) 1_555 2_575 yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) AL(1) O(2) 88.83(8) 1_555 1_555 1_555 yes O(1) AL(1) O(3) 89.25(8) 1_555 1_555 1_555 yes O(1) AL(1) O(4) 88.98(8) 1_555 1_555 1_555 yes O(1) AL(1) O(5) 178.71(10) 1_555 1_555 1_555 yes O(1) AL(1) O(6) 88.48(8) 1_555 1_555 1_555 yes O(2) AL(1) O(3) 176.98(9) 1_555 1_555 1_555 yes O(2) AL(1) O(4) 89.14(8) 1_555 1_555 1_555 yes O(2) AL(1) O(5) 89.96(9) 1_555 1_555 1_555 yes O(2) AL(1) O(6) 93.42(9) 1_555 1_555 1_555 yes O(3) AL(1) O(4) 88.49(8) 1_555 1_555 1_555 yes O(3) AL(1) O(5) 91.98(9) 1_555 1_555 1_555 yes O(3) AL(1) O(6) 88.87(9) 1_555 1_555 1_555 yes O(4) AL(1) O(5) 91.46(8) 1_555 1_555 1_555 yes O(4) AL(1) O(6) 176.36(9) 1_555 1_555 1_555 yes O(5) AL(1) O(6) 91.13(8) 1_555 1_555 1_555 yes AL(1) O(1) C(2) 125.46(13) 1_555 1_555 1_555 yes AL(1) O(2) C(4) 128.11(14) 1_555 1_555 1_555 yes AL(1) O(3) C(12) 128.47(14) 1_555 1_555 1_555 yes AL(1) O(4) C(14) 127.81(12) 1_555 1_555 1_555 yes AL(1) O(5) C(22) 129.09(13) 1_555 1_555 1_555 yes AL(1) O(6) C(24) 129.03(13) 1_555 1_555 1_555 yes C(8) N(1) C(9) 117.2(2) 1_555 1_555 1_555 yes C(18) N(2) C(19) 117.2(2) 1_555 1_555 1_555 yes C(28) N(3) C(29) 116.69(19) 1_555 1_555 1_555 yes C(2) C(1) H(1A) 109.85 1_555 1_555 1_555 yes C(2) C(1) H(1B) 109.24 1_555 1_555 1_555 yes C(2) C(1) H(1C) 109.33 1_555 1_555 1_555 yes H(1A) C(1) H(1B) 109.51 1_555 1_555 1_555 yes H(1A) C(1) H(1C) 109.9 1_555 1_555 1_555 yes H(1B) C(1) H(1C) 109.03 1_555 1_555 1_555 yes O(1) C(2) C(1) 115.43(16) 1_555 1_555 1_555 yes O(1) C(2) C(3) 123.62(15) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.94(15) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.62(14) 1_555 1_555 1_555 yes C(2) C(3) C(6) 119.75(14) 1_555 1_555 1_555 yes C(4) C(3) C(6) 119.39(14) 1_555 1_555 1_555 yes O(2) C(4) C(3) 123.31(15) 1_555 1_555 1_555 yes O(2) C(4) C(5) 115.70(16) 1_555 1_555 1_555 yes C(3) C(4) C(5) 120.95(15) 1_555 1_555 1_555 yes C(4) C(5) H(5A) 109.55 1_555 1_555 1_555 yes C(4) C(5) H(5B) 109.51 1_555 1_555 1_555 yes C(4) C(5) H(5C) 109.51 1_555 1_555 1_555 yes H(5A) C(5) H(5B) 109.45 1_555 1_555 1_555 yes H(5A) C(5) H(5C) 109.41 1_555 1_555 1_555 yes H(5B) C(5) H(5C) 109.40 1_555 1_555 1_555 yes C(3) C(6) C(7) 121.76(16) 1_555 1_555 1_555 yes C(3) C(6) C(10) 121.31(17) 1_555 1_555 1_555 yes C(7) C(6) C(10) 116.94(17) 1_555 1_555 1_555 yes C(6) C(7) C(8) 119.62(19) 1_555 1_555 1_555 yes C(6) C(7) H(7) 120.28 1_555 1_555 1_555 yes C(8) C(7) H(7) 120.09 1_555 1_555 1_555 yes N(1) C(8) C(7) 123.5(2) 1_555 1_555 1_555 yes N(1) C(8) H(8) 118.04 1_555 1_555 1_555 yes C(7) C(8) H(8) 118.4 1_555 1_555 1_555 yes N(1) C(9) C(10) 122.9(2) 1_555 1_555 1_555 yes N(1) C(9) H(9) 118.53 1_555 1_555 1_555 yes C(10) C(9) H(9) 118.5 1_555 1_555 1_555 yes C(6) C(10) C(9) 119.8(2) 1_555 1_555 1_555 yes C(6) C(10) H(10) 120.22 1_555 1_555 1_555 yes C(9) C(10) H(10) 120.03 1_555 1_555 1_555 yes C(12) C(11) H(11A) 109.79 1_555 1_555 1_555 yes C(12) C(11) H(11B) 109.75 1_555 1_555 1_555 yes C(12) C(11) H(11C) 109.55 1_555 1_555 1_555 yes H(11A) C(11) H(11B) 109.41 1_555 1_555 1_555 yes H(11A) C(11) H(11C) 109.21 1_555 1_555 1_555 yes H(11B) C(11) H(11C) 109.1 1_555 1_555 1_555 yes O(3) C(12) C(11) 114.06(16) 1_555 1_555 1_555 yes O(3) C(12) C(13) 123.95(15) 1_555 1_555 1_555 yes C(11) C(12) C(13) 121.99(17) 1_555 1_555 1_555 yes C(12) C(13) C(14) 120.46(15) 1_555 1_555 1_555 yes C(12) C(13) C(16) 119.99(14) 1_555 1_555 1_555 yes C(14) C(13) C(16) 119.52(14) 1_555 1_555 1_555 yes O(4) C(14) C(13) 122.80(15) 1_555 1_555 1_555 yes O(4) C(14) C(15) 114.98(14) 1_555 1_555 1_555 yes C(13) C(14) C(15) 122.19(15) 1_555 1_555 1_555 yes C(14) C(15) H(15A) 109.45 1_555 1_555 1_555 yes C(14) C(15) H(15B) 109.70 1_555 1_555 1_555 yes C(14) C(15) H(15C) 109.60 1_555 1_555 1_555 yes H(15A) C(15) H(15B) 109.38 1_555 1_555 1_555 yes H(15A) C(15) H(15C) 109.35 1_555 1_555 1_555 yes H(15B) C(15) H(15C) 109.35 1_555 1_555 1_555 yes C(13) C(16) C(17) 121.30(16) 1_555 1_555 1_555 yes C(13) C(16) C(20) 121.81(14) 1_555 1_555 1_555 yes C(17) C(16) C(20) 116.88(16) 1_555 1_555 1_555 yes C(16) C(17) C(18) 119.63(17) 1_555 1_555 1_555 yes C(16) C(17) H(17) 120.23 1_555 1_555 1_555 yes C(18) C(17) H(17) 120.14 1_555 1_555 1_555 yes N(2) C(18) C(17) 123.26(17) 1_555 1_555 1_555 yes N(2) C(18) H(18) 118.18 1_555 1_555 1_555 yes C(17) C(18) H(18) 118.56 1_555 1_555 1_555 yes N(2) C(19) C(20) 123.36(18) 1_555 1_555 1_555 yes N(2) C(19) H(19) 118.12 1_555 1_555 1_555 yes C(20) C(19) H(19) 118.52 1_555 1_555 1_555 yes C(16) C(20) C(19) 119.67(16) 1_555 1_555 1_555 yes C(16) C(20) H(20) 120.31 1_555 1_555 1_555 yes C(19) C(20) H(20) 120.02 1_555 1_555 1_555 yes C(22) C(21) H(21A) 109.27 1_555 1_555 1_555 yes C(22) C(21) H(21B) 109.72 1_555 1_555 1_555 yes C(22) C(21) H(21C) 109.66 1_555 1_555 1_555 yes H(21A) C(21) H(21B) 109.20 1_555 1_555 1_555 yes H(21A) C(21) H(21C) 109.33 1_555 1_555 1_555 yes H(21B) C(21) H(21C) 109.65 1_555 1_555 1_555 yes O(5) C(22) C(21) 115.20(16) 1_555 1_555 1_555 yes O(5) C(22) C(23) 124.01(15) 1_555 1_555 1_555 yes C(21) C(22) C(23) 120.79(15) 1_555 1_555 1_555 yes C(22) C(23) C(24) 121.01(14) 1_555 1_555 1_555 yes C(22) C(23) C(26) 120.06(14) 1_555 1_555 1_555 yes C(24) C(23) C(26) 118.90(14) 1_555 1_555 1_555 yes O(6) C(24) C(23) 123.71(15) 1_555 1_555 1_555 yes O(6) C(24) C(25) 115.32(15) 1_555 1_555 1_555 yes C(23) C(24) C(25) 120.97(15) 1_555 1_555 1_555 yes C(24) C(25) H(25A) 109.48 1_555 1_555 1_555 yes C(24) C(25) H(25B) 109.70 1_555 1_555 1_555 yes C(24) C(25) H(25C) 109.35 1_555 1_555 1_555 yes H(25A) C(25) H(25B) 109.6 1_555 1_555 1_555 yes H(25A) C(25) H(25C) 109.26 1_555 1_555 1_555 yes H(25B) C(25) H(25C) 109.47 1_555 1_555 1_555 yes C(23) C(26) C(27) 121.39(16) 1_555 1_555 1_555 yes C(23) C(26) C(30) 121.85(16) 1_555 1_555 1_555 yes C(27) C(26) C(30) 116.74(17) 1_555 1_555 1_555 yes C(26) C(27) C(28) 119.57(18) 1_555 1_555 1_555 yes C(26) C(27) H(27) 120.45 1_555 1_555 1_555 yes C(28) C(27) H(27) 119.99 1_555 1_555 1_555 yes N(3) C(28) C(27) 123.81(19) 1_555 1_555 1_555 yes N(3) C(28) H(28) 118.07 1_555 1_555 1_555 yes C(27) C(28) H(28) 118.12 1_555 1_555 1_555 yes N(3) C(29) C(30) 124.0(2) 1_555 1_555 1_555 yes N(3) C(29) H(29) 117.82 1_555 1_555 1_555 yes C(30) C(29) H(29) 118.2 1_555 1_555 1_555 yes C(26) C(30) C(29) 119.2(2) 1_555 1_555 1_555 yes C(26) C(30) H(30) 120.35 1_555 1_555 1_555 yes C(29) C(30) H(30) 120.4 1_555 1_555 1_555 yes I(1) C(31) C(32) 121.87(14) 1_555 1_555 1_555 yes I(1) C(31) C(36) 120.47(15) 1_555 1_555 1_555 yes C(32) C(31) C(36) 117.54(19) 1_555 1_555 1_555 yes F(1) C(32) C(31) 120.4(2) 1_555 1_555 1_555 yes F(1) C(32) C(33) 118.3(2) 1_555 1_555 1_555 yes C(31) C(32) C(33) 121.28(18) 1_555 1_555 1_555 yes F(2) C(33) C(32) 118.3(2) 1_555 1_555 1_555 yes F(2) C(33) C(34) 120.5(3) 1_555 1_555 1_555 yes C(32) C(33) C(34) 121.19(19) 1_555 1_555 1_555 yes I(2) C(34) C(33) 120.57(16) 1_555 1_555 1_555 yes I(2) C(34) C(35) 122.17(15) 1_555 1_555 1_555 yes C(33) C(34) C(35) 117.26(19) 1_555 1_555 1_555 yes F(4) C(35) C(34) 120.3(3) 1_555 1_555 1_555 yes F(4) C(35) C(36) 118.4(3) 1_555 1_555 1_555 yes C(34) C(35) C(36) 121.32(18) 1_555 1_555 1_555 yes F(3) C(36) C(31) 120.5(2) 1_555 1_555 1_555 yes F(3) C(36) C(35) 118.2(2) 1_555 1_555 1_555 yes C(31) C(36) C(35) 121.38(18) 1_555 1_555 1_555 yes I(3) C(37) C(38) 120.50(15) 1_555 1_555 1_555 yes I(3) C(37) C(39) 122.30(16) 1_555 1_555 1_555 yes C(38) C(37) C(39) 117.20(17) 1_555 1_555 1_555 yes F(5) C(38) C(37) 119.8(2) 1_555 1_555 1_555 yes F(5) C(38) C(39) 119.0(3) 1_555 1_555 2_575 yes C(37) C(38) C(39) 121.20(18) 1_555 1_555 2_575 yes F(6) C(39) C(37) 120.6(3) 1_555 1_555 1_555 yes F(6) C(39) C(38) 117.8(3) 1_555 1_555 2_575 yes C(37) C(39) C(38) 121.59(18) 1_555 1_555 2_575 yes _database_code_depnum_ccdc_archive 'CCDC 935896' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef 'complete_all_iam.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HacacPy-TFDIB _chemical_melting_point ? _chemical_formula_moiety 'C10 H11 N O2, 0.5(C6 F4 I2)' _chemical_formula_sum 'C13 H11 F2 I N O2' _chemical_formula_weight 378.13 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.142(6) _cell_length_b 7.388(6) _cell_length_c 14.672(13) _cell_angle_alpha 81.132(15) _cell_angle_beta 78.539(15) _cell_angle_gamma 62.600(12) _cell_volume 671.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1848 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 23.23 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 366 _exptl_absorpt_coefficient_mu 2.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5229 _exptl_absorpt_correction_T_max 0.9314 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7608 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.1070 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.26 _reflns_number_total 2821 _reflns_number_gt 2079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2821 _refine_ls_number_parameters 178 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _iucr_refine_instruction_details ; TITL c12_33 in P-1 CELL 0.71073 7.1425 7.3878 14.6716 81.1323 78.5386 62.6004 ZERR 2.00 0.0062 0.0064 0.0128 0.0149 0.0146 0.0123 LATT 1 SFAC C H N O F I UNIT 26 22 2 4 4 2 TEMP -173.000 L.S. 8 BOND SIZE 0.31 0.12 0.03 BOND$H ACTA 50 FMAP 2 PLAN -20 WGHT 0.067500 FVAR 0.52889 MOLE 1 I1 6 0.771933 0.521367 0.421799 11.00000 0.02305 0.01818 = 0.05244 0.00305 -0.01076 -0.00649 F2 5 0.782727 0.281421 0.629028 11.00000 0.03362 0.02083 = 0.05093 -0.00106 -0.01195 -0.00370 F1 5 1.056230 0.112914 0.315117 11.00000 0.03510 0.03027 = 0.03760 0.00512 -0.00788 -0.00780 C11 1 0.916027 0.207735 0.470120 11.00000 0.01960 0.01749 = 0.05333 -0.00003 -0.01203 -0.00200 C12 1 0.889255 0.144816 0.563257 11.00000 0.02019 0.02061 = 0.04166 -0.00418 -0.00786 -0.00226 C13 1 1.027174 0.059972 0.407289 11.00000 0.02089 0.02940 = 0.04811 0.00152 -0.01075 -0.00808 MOLE 2 DFIX 0.90 O1 H1D O1 4 0.686826 0.224709 0.921578 11.00000 0.03435 0.01806 = 0.05315 0.00354 -0.01286 -0.00374 H1D 2 0.550883 0.243303 0.936224 11.00000 0.06747 O2 4 0.296087 0.398783 0.957961 11.00000 0.03604 0.02572 = 0.04949 0.00077 -0.00494 -0.01218 N1 3 0.434639 1.081588 0.666987 11.00000 0.02466 0.01923 = 0.05464 -0.00269 -0.00649 -0.00817 C1 1 0.892806 0.371807 0.822581 11.00000 0.03136 0.02544 = 0.05462 0.00059 -0.01272 -0.00406 AFIX 137 H1A 2 0.980199 0.346427 0.871149 11.00000 -1.50000 H1B 2 0.875233 0.499938 0.786020 11.00000 -1.50000 H1C 2 0.963137 0.258868 0.781518 11.00000 -1.50000 AFIX 0 C2 1 0.679162 0.387338 0.866870 11.00000 0.02977 0.02539 = 0.04616 0.00060 -0.01187 -0.01011 C3 1 0.486802 0.555142 0.855801 11.00000 0.02953 0.01345 = 0.04208 -0.00196 -0.00855 -0.00544 C4 1 0.293088 0.554389 0.906753 11.00000 0.02654 0.02486 = 0.04597 -0.00477 -0.00733 -0.01083 C5 1 0.082939 0.737794 0.900339 11.00000 0.02411 0.03172 = 0.05342 0.00219 -0.01044 -0.00648 AFIX 137 H5A 2 -0.032406 0.703518 0.931753 11.00000 -1.50000 H5B 2 0.065813 0.780027 0.834641 11.00000 -1.50000 H5C 2 0.077890 0.849855 0.930425 11.00000 -1.50000 AFIX 0 C6 1 0.477880 0.737371 0.790507 11.00000 0.01474 0.01900 = 0.04801 0.00413 -0.01002 -0.00269 C7 1 0.477019 0.736826 0.697010 11.00000 0.03584 0.02207 = 0.04083 -0.00264 -0.00926 -0.01159 AFIX 43 H7 2 0.492365 0.618244 0.672456 11.00000 -1.20000 AFIX 0 C8 1 0.453555 0.910855 0.638375 11.00000 0.03626 0.02300 = 0.04489 -0.00215 -0.01158 -0.00826 AFIX 43 H8 2 0.450903 0.907442 0.574195 11.00000 -1.20000 AFIX 0 C9 1 0.443466 1.078564 0.757010 11.00000 0.03514 0.01976 = 0.04583 -0.00507 -0.00845 -0.01114 AFIX 43 H9 2 0.434839 1.197025 0.778937 11.00000 -1.20000 AFIX 0 C10 1 0.464620 0.912135 0.821289 11.00000 0.03896 0.02008 = 0.04925 -0.00353 -0.01475 -0.00886 AFIX 43 H10 2 0.469840 0.918363 0.884877 11.00000 -1.20000 HKLF 4 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.77193(7) 0.52137(7) 0.42180(4) 0.0321(2) Uani 1 1 d . . . F2 F 0.7827(7) 0.2814(6) 0.6290(3) 0.0377(11) Uani 1 1 d . . . F1 F 1.0562(7) 0.1129(6) 0.3151(3) 0.0375(10) Uani 1 1 d . . . C11 C 0.9160(11) 0.2077(11) 0.4701(6) 0.0319(17) Uani 1 1 d . . . C12 C 0.8893(11) 0.1448(11) 0.5633(5) 0.0294(16) Uani 1 1 d . . . C13 C 1.0272(11) 0.0600(12) 0.4073(6) 0.0336(18) Uani 1 1 d . . . O1 O 0.6868(9) 0.2247(8) 0.9216(4) 0.0380(13) Uani 1 1 d D . . H1D H 0.551(6) 0.243(15) 0.936(6) 0.07(3) Uiso 1 1 d D . . O2 O 0.2961(8) 0.3988(8) 0.9580(4) 0.0383(13) Uani 1 1 d . . . N1 N 0.4346(9) 1.0816(9) 0.6670(5) 0.0333(15) Uani 1 1 d . . . C1 C 0.8928(12) 0.3718(12) 0.8226(6) 0.0399(19) Uani 1 1 d . . . H1A H 0.9802 0.3464 0.8711 0.060 Uiso 1 1 calc R . . H1B H 0.8752 0.4999 0.7860 0.060 Uiso 1 1 calc R . . H1C H 0.9631 0.2589 0.7815 0.060 Uiso 1 1 calc R . . C2 C 0.6792(12) 0.3873(11) 0.8669(6) 0.0340(18) Uani 1 1 d . . . C3 C 0.4868(11) 0.5551(10) 0.8558(5) 0.0295(16) Uani 1 1 d . . . C4 C 0.2931(11) 0.5544(11) 0.9068(5) 0.0321(17) Uani 1 1 d . . . C5 C 0.0829(12) 0.7378(12) 0.9003(6) 0.0386(19) Uani 1 1 d . . . H5A H -0.0324 0.7035 0.9318 0.058 Uiso 1 1 calc R . . H5B H 0.0658 0.7800 0.8346 0.058 Uiso 1 1 calc R . . H5C H 0.0779 0.8499 0.9304 0.058 Uiso 1 1 calc R . . C6 C 0.4779(10) 0.7374(10) 0.7905(5) 0.0291(17) Uani 1 1 d . . . C7 C 0.4770(12) 0.7368(11) 0.6970(5) 0.0328(17) Uani 1 1 d . . . H7 H 0.4924 0.6182 0.6725 0.039 Uiso 1 1 calc R . . C8 C 0.4536(12) 0.9109(11) 0.6384(6) 0.0358(18) Uani 1 1 d . . . H8 H 0.4509 0.9074 0.5742 0.043 Uiso 1 1 calc R . . C9 C 0.4435(12) 1.0786(11) 0.7570(6) 0.0333(17) Uani 1 1 d . . . H9 H 0.4348 1.1970 0.7789 0.040 Uiso 1 1 calc R . . C10 C 0.4646(12) 0.9121(11) 0.8213(6) 0.0364(18) Uani 1 1 d . . . H10 H 0.4698 0.9184 0.8849 0.044 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 I1 0.0230(3) 0.0182(3) 0.0524(4) 0.0031(2) -0.0108(2) -0.00649(19) F2 0.034(2) 0.021(2) 0.051(3) -0.001(2) -0.012(2) -0.0037(19) F1 0.035(2) 0.030(2) 0.038(3) 0.0051(19) -0.0079(19) -0.008(2) C11 0.020(4) 0.017(3) 0.053(5) 0.000(3) -0.012(3) -0.002(3) C12 0.020(4) 0.021(4) 0.042(5) -0.004(3) -0.008(3) -0.002(3) C13 0.021(4) 0.029(4) 0.048(5) 0.002(3) -0.011(3) -0.008(3) O1 0.034(3) 0.018(3) 0.053(4) 0.004(2) -0.013(3) -0.004(2) O2 0.036(3) 0.026(3) 0.049(4) 0.001(2) -0.005(3) -0.012(2) N1 0.025(3) 0.019(3) 0.055(5) -0.003(3) -0.006(3) -0.008(3) C1 0.031(4) 0.025(4) 0.055(5) 0.001(4) -0.013(4) -0.004(3) C2 0.030(4) 0.025(4) 0.046(5) 0.001(3) -0.012(3) -0.010(3) C3 0.030(4) 0.013(3) 0.042(5) -0.002(3) -0.009(3) -0.005(3) C4 0.027(4) 0.025(4) 0.046(5) -0.005(3) -0.007(3) -0.011(3) C5 0.024(4) 0.032(4) 0.053(5) 0.002(4) -0.010(4) -0.006(3) C6 0.015(3) 0.019(3) 0.048(5) 0.004(3) -0.010(3) -0.003(3) C7 0.036(4) 0.022(4) 0.041(5) -0.003(3) -0.009(3) -0.012(3) C8 0.036(4) 0.023(4) 0.045(5) -0.002(3) -0.012(4) -0.008(3) C9 0.035(4) 0.020(4) 0.046(5) -0.005(3) -0.008(3) -0.011(3) C10 0.039(4) 0.020(4) 0.049(5) -0.004(3) -0.015(4) -0.009(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 I1 C11 2.126(7) . ? F2 C12 1.353(9) . ? F1 C13 1.351(9) . ? C11 C13 1.376(11) . ? C11 C12 1.379(11) . ? C12 C13 1.379(10) 2_756 ? C13 C12 1.379(10) 2_756 ? O1 C2 1.323(9) . ? O1 H1D 0.90(2) . ? O2 C4 1.266(9) . ? N1 C8 1.330(10) . ? N1 C9 1.331(10) . ? C1 C2 1.494(10) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.382(10) . ? C3 C4 1.438(10) . ? C3 C6 1.511(9) . ? C4 C5 1.498(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.374(11) . ? C6 C10 1.389(10) . ? C7 C8 1.393(10) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.397(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 C13 C11 C12 118.0(7) . . ? C13 C11 I1 120.0(6) . . ? C12 C11 I1 121.8(6) . . ? F2 C12 C13 117.6(7) . 2_756 ? F2 C12 C11 121.3(6) . . ? C13 C12 C11 121.1(7) 2_756 . ? F1 C13 C11 120.5(7) . . ? F1 C13 C12 118.6(7) . 2_756 ? C11 C13 C12 120.9(7) . 2_756 ? C2 O1 H1D 106(6) . . ? C8 N1 C9 116.2(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 121.0(7) . . ? O1 C2 C1 114.0(6) . . ? C3 C2 C1 125.0(7) . . ? C2 C3 C4 119.2(6) . . ? C2 C3 C6 120.9(7) . . ? C4 C3 C6 119.9(6) . . ? O2 C4 C3 120.8(6) . . ? O2 C4 C5 118.5(7) . . ? C3 C4 C5 120.7(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C10 117.3(7) . . ? C7 C6 C3 120.1(7) . . ? C10 C6 C3 122.6(7) . . ? C6 C7 C8 119.7(7) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N1 C8 C7 123.8(8) . . ? N1 C8 H8 118.1 . . ? C7 C8 H8 118.1 . . ? N1 C9 C10 124.1(7) . . ? N1 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C6 C10 C9 118.8(7) . . ? C6 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.848 _refine_diff_density_min -1.687 _refine_diff_density_rms 0.205 _database_code_depnum_ccdc_archive 'CCDC 935897' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef 'complete_all_iam.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Fe(acacPy)3 - TFDIB' _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Fe N3 O6, C6 F4 I2, C H Cl3' _chemical_formula_sum 'C37 H31 Cl3 F4 Fe I2 N3 O6' _chemical_formula_weight 1105.65 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' F F 0.0171 0.0103 '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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6330(4) _cell_length_b 16.4167(8) _cell_length_c 18.6385(9) _cell_angle_alpha 113.3409(6) _cell_angle_beta 98.4034(7) _cell_angle_gamma 95.2702(7) _cell_volume 2092.38(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8110 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 29.26 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1082 _exptl_absorpt_coefficient_mu 2.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5919 _exptl_absorpt_correction_T_max 0.7443 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31874 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.91 _reflns_number_total 12075 _reflns_number_gt 10084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0382P)^2^+0.9373P] 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 12075 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _iucr_refine_instruction_details ; TITL c12_59 in P-1 CELL 0.71073 7.6330 16.4167 18.6385 113.3409 98.4034 95.2702 ZERR 2.00 0.0004 0.0008 0.0009 0.0006 0.0007 0.0007 LATT 1 SFAC C H N O F CL FE I UNIT 74 62 6 12 8 6 2 4 TEMP -173 L.S. 8 BOND SIZE 0.28 0.17 0.15 ACTA 55 FMAP 2 PLAN -20 WGHT 0.038200 0.937300 FVAR 0.25161 MOLE 1 FE1 7 0.359976 0.143521 0.897860 11.00000 0.01820 0.01968 = 0.01561 0.00691 0.00810 0.00928 O1 4 0.435142 0.037939 0.913769 11.00000 0.02360 0.02442 = 0.01714 0.00943 0.01070 0.01286 O2 4 0.586233 0.150547 0.857174 11.00000 0.01994 0.02215 = 0.02136 0.00964 0.00870 0.00854 O3 4 0.230721 0.059415 0.789223 11.00000 0.02095 0.02153 = 0.01822 0.00937 0.00720 0.00700 O4 4 0.286936 0.239138 0.863259 11.00000 0.02624 0.02143 = 0.01976 0.00746 0.00919 0.01199 O5 4 0.155175 0.140293 0.950260 11.00000 0.02024 0.02172 = 0.01653 0.00518 0.00874 0.00741 O6 4 0.486559 0.241231 1.002046 11.00000 0.01833 0.02427 = 0.01822 0.00546 0.00874 0.00743 C1 1 0.534156 -0.101353 0.887808 11.00000 0.02762 0.02598 = 0.02834 0.01515 0.01271 0.01247 AFIX 137 H1A 2 0.445488 -0.104981 0.919970 11.00000 -1.50000 H1B 2 0.653314 -0.102524 0.914980 11.00000 -1.50000 H1C 2 0.502171 -0.152654 0.835546 11.00000 -1.50000 AFIX 0 C2 1 0.536448 -0.015231 0.876953 11.00000 0.01967 0.02108 = 0.01352 0.00556 0.00291 0.00844 C3 1 0.648711 0.003148 0.829497 11.00000 0.01678 0.01936 = 0.01640 0.00532 0.00462 0.00816 C4 1 0.669919 0.085704 0.822968 11.00000 0.01522 0.02393 = 0.01596 0.00672 0.00520 0.00889 C5 1 0.801325 0.105053 0.776652 11.00000 0.02583 0.02471 = 0.02906 0.01308 0.01556 0.01196 AFIX 137 H5A 2 0.780192 0.159273 0.768914 11.00000 -1.50000 H5B 2 0.785332 0.054004 0.724617 11.00000 -1.50000 H5C 2 0.924038 0.114486 0.806259 11.00000 -1.50000 AFIX 0 C6 1 0.761268 -0.063959 0.789447 11.00000 0.01719 0.01858 = 0.01916 0.00722 0.00932 0.00749 C7 1 0.706077 -0.124939 0.709834 11.00000 0.02168 0.02122 = 0.01955 0.00618 0.00549 0.00550 AFIX 43 H7 2 0.591402 -0.126870 0.680825 11.00000 -1.20000 AFIX 0 C8 1 0.819338 -0.182817 0.673123 11.00000 0.02623 0.01900 = 0.01950 0.00380 0.01082 0.00548 AFIX 43 H8 2 0.779506 -0.223545 0.618739 11.00000 -1.20000 AFIX 0 C9 1 1.033759 -0.126554 0.786666 11.00000 0.02115 0.02349 = 0.03201 0.00874 0.00899 0.01096 AFIX 43 H9 2 1.148467 -0.127007 0.814170 11.00000 -1.20000 AFIX 0 C10 1 0.930357 -0.065957 0.828248 11.00000 0.02003 0.02282 = 0.01948 0.00385 0.00296 0.00711 AFIX 43 H10 2 0.974366 -0.026206 0.882643 11.00000 -1.20000 AFIX 0 C11 1 0.175959 -0.013261 0.649826 11.00000 0.04443 0.02358 = 0.01769 0.00583 0.00727 0.00270 AFIX 137 H11A 2 0.280616 -0.043727 0.641545 11.00000 -1.50000 H11B 2 0.137019 0.001466 0.604553 11.00000 -1.50000 H11C 2 0.078073 -0.052955 0.654224 11.00000 -1.50000 AFIX 0 C12 1 0.225401 0.071941 0.725381 11.00000 0.01824 0.02306 = 0.01848 0.00778 0.00681 0.00601 C13 1 0.250268 0.156574 0.723481 11.00000 0.02147 0.02156 = 0.01878 0.00931 0.00561 0.00769 C14 1 0.261718 0.236246 0.792999 11.00000 0.02168 0.02294 = 0.02522 0.01094 0.00771 0.00951 C15 1 0.234485 0.323165 0.787348 11.00000 0.04608 0.02727 = 0.02981 0.01274 0.00926 0.01736 AFIX 137 H15A 2 0.105655 0.324049 0.774689 11.00000 -1.50000 H15B 2 0.291603 0.328467 0.745251 11.00000 -1.50000 H15C 2 0.288436 0.373670 0.838417 11.00000 -1.50000 AFIX 0 C16 1 0.256687 0.160956 0.645084 11.00000 0.03271 0.02096 = 0.02044 0.00947 0.00516 0.00406 C17 1 0.119048 0.185568 0.603361 11.00000 0.04603 0.03186 = 0.02845 0.01412 0.00129 0.01288 AFIX 43 H17 2 0.015051 0.201867 0.624410 11.00000 -1.20000 AFIX 0 C18 1 0.138509 0.185548 0.530061 11.00000 0.06644 0.03635 = 0.02873 0.01888 -0.00542 0.00634 AFIX 43 H18 2 0.044319 0.202534 0.502420 11.00000 -1.20000 AFIX 0 C19 1 0.406353 0.140808 0.536429 11.00000 0.05750 0.04985 = 0.02561 0.01716 0.01522 0.00169 AFIX 43 H19 2 0.507692 0.124023 0.513307 11.00000 -1.20000 AFIX 0 C20 1 0.403786 0.139522 0.609975 11.00000 0.03670 0.03757 = 0.02650 0.01487 0.01075 0.00395 AFIX 43 H20 2 0.502636 0.123981 0.636357 11.00000 -1.20000 AFIX 0 C21 1 -0.069091 0.182217 1.026660 11.00000 0.01989 0.02817 = 0.01878 0.00532 0.00795 0.00545 AFIX 137 H21A 2 -0.146037 0.216652 1.007034 11.00000 -1.50000 H21B 2 -0.065605 0.200707 1.083779 11.00000 -1.50000 H21C 2 -0.117376 0.117903 0.997829 11.00000 -1.50000 AFIX 0 C22 1 0.118970 0.199809 1.013282 11.00000 0.01736 0.02127 = 0.01548 0.00853 0.00632 0.00846 C23 1 0.241567 0.275992 1.068069 11.00000 0.02128 0.01941 = 0.01355 0.00703 0.00664 0.00764 C24 1 0.421867 0.290926 1.060879 11.00000 0.02395 0.01920 = 0.01789 0.00711 0.00560 0.00752 C25 1 0.552179 0.368325 1.125332 11.00000 0.02500 0.03319 = 0.02438 0.00060 0.00776 0.00056 AFIX 137 H25A 2 0.671812 0.367075 1.112096 11.00000 -1.50000 H25B 2 0.556625 0.363355 1.176235 11.00000 -1.50000 H25C 2 0.513124 0.425045 1.129717 11.00000 -1.50000 AFIX 0 C26 1 0.178816 0.341137 1.138223 11.00000 0.01922 0.01926 = 0.01698 0.00474 0.00718 0.00603 C27 1 0.118839 0.417463 1.136780 11.00000 0.05240 0.02769 = 0.02887 0.01503 0.02625 0.01970 AFIX 43 H27 2 0.123561 0.431735 1.092361 11.00000 -1.20000 AFIX 0 C28 1 0.051636 0.473043 1.200901 11.00000 0.05283 0.02517 = 0.03917 0.01452 0.02864 0.02023 AFIX 43 H28 2 0.009678 0.524857 1.198631 11.00000 -1.20000 AFIX 0 C29 1 0.101802 0.384868 1.266794 11.00000 0.03491 0.03980 = 0.01764 0.00960 0.01069 0.01504 AFIX 43 H29 2 0.095150 0.372241 1.311944 11.00000 -1.20000 AFIX 0 C30 1 0.172650 0.326127 1.206098 11.00000 0.03377 0.03283 = 0.01882 0.01104 0.00931 0.01781 AFIX 43 H30 2 0.216785 0.275856 1.210834 11.00000 -1.20000 AFIX 0 N1 3 0.981454 -0.184022 0.710520 11.00000 0.02490 0.02011 = 0.02979 0.00941 0.01412 0.00991 N2 3 0.278230 0.163663 0.496035 11.00000 0.07206 0.04343 = 0.02630 0.01724 0.00568 -0.00062 N3 3 0.042643 0.457817 1.265504 11.00000 0.02975 0.02668 = 0.02292 0.00340 0.01160 0.00763 MOLE 2 I1 8 -0.793183 0.725199 1.611132 11.00000 0.02231 0.01991 = 0.03019 0.00715 0.01466 0.00826 I2 8 -0.193343 0.536297 1.363603 11.00000 0.02406 0.02190 = 0.02148 0.00496 0.01209 0.00767 F1 5 -0.457785 0.628182 1.631909 11.00000 0.02741 0.03448 = 0.02053 0.00995 0.01102 0.01037 F2 5 -0.230916 0.556227 1.538095 11.00000 0.02415 0.03121 = 0.02472 0.01039 0.00897 0.01267 F3 5 -0.542615 0.626555 1.337293 11.00000 0.03902 0.05552 = 0.03050 0.02719 0.01707 0.02341 F4 5 -0.768741 0.699778 1.431567 11.00000 0.03222 0.04347 = 0.04232 0.02551 0.01595 0.02243 C31 1 -0.622344 0.664688 1.534379 11.00000 0.02214 0.01808 = 0.02601 0.00571 0.01129 0.00505 C32 1 -0.482755 0.627727 1.558699 11.00000 0.02204 0.02081 = 0.02094 0.00649 0.00932 0.00498 C33 1 -0.364159 0.590690 1.510131 11.00000 0.01977 0.01786 = 0.02299 0.00530 0.00709 0.00691 C34 1 -0.379475 0.589046 1.434703 11.00000 0.02215 0.02054 = 0.02230 0.00561 0.01048 0.00639 C35 1 -0.521712 0.625017 1.409793 11.00000 0.02782 0.02728 = 0.02564 0.01261 0.01213 0.00823 C36 1 -0.638545 0.662523 1.458468 11.00000 0.02241 0.02520 = 0.03355 0.01401 0.00927 0.01173 MOLE 3 CL1 6 0.683476 0.344458 0.808596 11.00000 0.04268 0.04460 = 0.04390 0.02328 0.00372 0.00789 CL3 6 0.955899 0.335675 0.927626 11.00000 0.03701 0.06472 = 0.05166 0.02293 -0.00033 0.01175 CL2 6 0.692319 0.453138 0.975061 11.00000 0.09284 0.03758 = 0.06128 0.01958 0.04583 0.02241 C40 1 0.732313 0.350445 0.906297 11.00000 0.03391 0.03275 = 0.04168 0.01781 0.01099 0.00966 AFIX 13 H40 2 0.651741 0.300514 0.908894 11.00000 -1.20000 HKLF 4 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.35998(5) 0.14352(2) 0.89786(2) 0.01702(8) Uani 1 1 d . . . O1 O 0.4351(2) 0.03794(12) 0.91377(10) 0.0201(4) Uani 1 1 d . . . O2 O 0.5862(2) 0.15055(12) 0.85717(11) 0.0201(4) Uani 1 1 d . . . O3 O 0.2307(2) 0.05941(12) 0.78922(10) 0.0193(4) Uani 1 1 d . . . O4 O 0.2869(3) 0.23914(12) 0.86326(11) 0.0218(4) Uani 1 1 d . . . O5 O 0.1552(2) 0.14029(12) 0.95026(10) 0.0196(4) Uani 1 1 d . . . O6 O 0.4866(2) 0.24123(12) 1.00205(10) 0.0205(4) Uani 1 1 d . . . C1 C 0.5342(4) -0.10135(19) 0.88781(17) 0.0247(6) Uani 1 1 d . . . H1A H 0.4455 -0.1050 0.9200 0.037 Uiso 1 1 calc R . . H1B H 0.6533 -0.1025 0.9150 0.037 Uiso 1 1 calc R . . H1C H 0.5022 -0.1527 0.8355 0.037 Uiso 1 1 calc R . . C2 C 0.5364(3) -0.01523(17) 0.87695(14) 0.0183(5) Uani 1 1 d . . . C3 C 0.6487(3) 0.00315(17) 0.82950(14) 0.0177(5) Uani 1 1 d . . . C4 C 0.6699(3) 0.08570(17) 0.82297(15) 0.0183(5) Uani 1 1 d . . . C5 C 0.8013(4) 0.10505(19) 0.77665(17) 0.0243(6) Uani 1 1 d . . . H5A H 0.7802 0.1593 0.7689 0.036 Uiso 1 1 calc R . . H5B H 0.7853 0.0540 0.7246 0.036 Uiso 1 1 calc R . . H5C H 0.9240 0.1145 0.8063 0.036 Uiso 1 1 calc R . . C6 C 0.7613(3) -0.06396(17) 0.78945(15) 0.0176(5) Uani 1 1 d . . . C7 C 0.7061(4) -0.12494(17) 0.70983(15) 0.0213(5) Uani 1 1 d . . . H7 H 0.5914 -0.1269 0.6808 0.026 Uiso 1 1 calc R . . C8 C 0.8193(4) -0.18282(17) 0.67312(16) 0.0221(5) Uani 1 1 d . . . H8 H 0.7795 -0.2235 0.6187 0.027 Uiso 1 1 calc R . . C9 C 1.0338(4) -0.12655(18) 0.78667(17) 0.0255(6) Uani 1 1 d . . . H9 H 1.1485 -0.1270 0.8142 0.031 Uiso 1 1 calc R . . C10 C 0.9304(4) -0.06596(18) 0.82825(16) 0.0222(5) Uani 1 1 d . . . H10 H 0.9744 -0.0262 0.8826 0.027 Uiso 1 1 calc R . . C11 C 0.1760(4) -0.01326(19) 0.64983(16) 0.0295(6) Uani 1 1 d . . . H11A H 0.2806 -0.0437 0.6415 0.044 Uiso 1 1 calc R . . H11B H 0.1370 0.0015 0.6046 0.044 Uiso 1 1 calc R . . H11C H 0.0781 -0.0530 0.6542 0.044 Uiso 1 1 calc R . . C12 C 0.2254(3) 0.07194(18) 0.72538(15) 0.0197(5) Uani 1 1 d . . . C13 C 0.2503(4) 0.15657(17) 0.72348(15) 0.0198(5) Uani 1 1 d . . . C14 C 0.2617(4) 0.23625(18) 0.79300(16) 0.0222(5) Uani 1 1 d . . . C15 C 0.2345(5) 0.3232(2) 0.78735(19) 0.0331(7) Uani 1 1 d . . . H15A H 0.1057 0.3240 0.7747 0.050 Uiso 1 1 calc R . . H15B H 0.2916 0.3285 0.7453 0.050 Uiso 1 1 calc R . . H15C H 0.2884 0.3737 0.8384 0.050 Uiso 1 1 calc R . . C16 C 0.2567(4) 0.16096(18) 0.64508(16) 0.0245(6) Uani 1 1 d . . . C17 C 0.1190(5) 0.1856(2) 0.60336(19) 0.0352(7) Uani 1 1 d . . . H17 H 0.0151 0.2019 0.6244 0.042 Uiso 1 1 calc R . . C18 C 0.1385(6) 0.1855(2) 0.5301(2) 0.0439(9) Uani 1 1 d . . . H18 H 0.0443 0.2025 0.5024 0.053 Uiso 1 1 calc R . . C19 C 0.4064(5) 0.1408(3) 0.5364(2) 0.0436(9) Uani 1 1 d . . . H19 H 0.5077 0.1240 0.5133 0.052 Uiso 1 1 calc R . . C20 C 0.4038(4) 0.1395(2) 0.60998(18) 0.0327(7) Uani 1 1 d . . . H20 H 0.5026 0.1240 0.6364 0.039 Uiso 1 1 calc R . . C21 C -0.0691(4) 0.18222(19) 1.02666(16) 0.0232(5) Uani 1 1 d . . . H21A H -0.1460 0.2167 1.0070 0.035 Uiso 1 1 calc R . . H21B H -0.0656 0.2007 1.0838 0.035 Uiso 1 1 calc R . . H21C H -0.1174 0.1179 0.9978 0.035 Uiso 1 1 calc R . . C22 C 0.1190(3) 0.19981(17) 1.01328(14) 0.0170(5) Uani 1 1 d . . . C23 C 0.2416(3) 0.27599(17) 1.06807(14) 0.0174(5) Uani 1 1 d . . . C24 C 0.4219(4) 0.29093(17) 1.06088(15) 0.0201(5) Uani 1 1 d . . . C25 C 0.5522(4) 0.3683(2) 1.12533(17) 0.0312(7) Uani 1 1 d . . . H25A H 0.6718 0.3671 1.1121 0.047 Uiso 1 1 calc R . . H25B H 0.5566 0.3634 1.1762 0.047 Uiso 1 1 calc R . . H25C H 0.5131 0.4250 1.1297 0.047 Uiso 1 1 calc R . . C26 C 0.1788(3) 0.34114(17) 1.13822(15) 0.0188(5) Uani 1 1 d . . . C27 C 0.1188(5) 0.4175(2) 1.13678(18) 0.0323(7) Uani 1 1 d . . . H27 H 0.1236 0.4317 1.0924 0.039 Uiso 1 1 calc R . . C28 C 0.0516(5) 0.4730(2) 1.20090(19) 0.0356(7) Uani 1 1 d . . . H28 H 0.0097 0.5249 1.1986 0.043 Uiso 1 1 calc R . . C29 C 0.1018(4) 0.3849(2) 1.26679(17) 0.0303(6) Uani 1 1 d . . . H29 H 0.0951 0.3722 1.3119 0.036 Uiso 1 1 calc R . . C30 C 0.1726(4) 0.3261(2) 1.20610(16) 0.0271(6) Uani 1 1 d . . . H30 H 0.2168 0.2759 1.2108 0.032 Uiso 1 1 calc R . . N1 N 0.9815(3) -0.18402(15) 0.71052(14) 0.0239(5) Uani 1 1 d . . . N2 N 0.2782(5) 0.1637(2) 0.49603(17) 0.0475(8) Uani 1 1 d . . . N3 N 0.0426(3) 0.45782(16) 1.26550(14) 0.0278(5) Uani 1 1 d . . . I1 I -0.79318(2) 0.725199(11) 1.611132(11) 0.02382(5) Uani 1 1 d . . . I2 I -0.19334(2) 0.536297(11) 1.363603(10) 0.02269(5) Uani 1 1 d . . . F1 F -0.4578(2) 0.62818(11) 1.63191(9) 0.0269(4) Uani 1 1 d . . . F2 F -0.2309(2) 0.55623(11) 1.53809(9) 0.0261(3) Uani 1 1 d . . . F3 F -0.5426(3) 0.62656(13) 1.33729(11) 0.0365(4) Uani 1 1 d . . . F4 F -0.7687(2) 0.69978(13) 1.43157(11) 0.0348(4) Uani 1 1 d . . . C31 C -0.6223(4) 0.66469(17) 1.53438(16) 0.0224(5) Uani 1 1 d . . . C32 C -0.4828(4) 0.62773(18) 1.55870(16) 0.0213(5) Uani 1 1 d . . . C33 C -0.3642(4) 0.59069(17) 1.51013(16) 0.0207(5) Uani 1 1 d . . . C34 C -0.3795(4) 0.58905(18) 1.43470(16) 0.0219(5) Uani 1 1 d . . . C35 C -0.5217(4) 0.62502(19) 1.40979(17) 0.0254(6) Uani 1 1 d . . . C36 C -0.6385(4) 0.66252(19) 1.45847(18) 0.0255(6) Uani 1 1 d . . . Cl1 Cl 0.68348(12) 0.34446(6) 0.80860(5) 0.0426(2) Uani 1 1 d . . . Cl3 Cl 0.95590(13) 0.33567(7) 0.92763(6) 0.0523(2) Uani 1 1 d . . . Cl2 Cl 0.69232(17) 0.45314(6) 0.97506(7) 0.0600(3) Uani 1 1 d . . . C40 C 0.7323(4) 0.3504(2) 0.9063(2) 0.0347(7) Uani 1 1 d . . . H40 H 0.6517 0.3005 0.9089 0.042 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 Fe1 0.01820(18) 0.01968(18) 0.01561(17) 0.00691(14) 0.00810(14) 0.00928(14) O1 0.0236(9) 0.0244(9) 0.0171(9) 0.0094(7) 0.0107(7) 0.0129(7) O2 0.0199(9) 0.0221(9) 0.0214(9) 0.0096(7) 0.0087(7) 0.0085(7) O3 0.0209(9) 0.0215(9) 0.0182(9) 0.0094(7) 0.0072(7) 0.0070(7) O4 0.0262(10) 0.0214(9) 0.0198(9) 0.0075(7) 0.0092(8) 0.0120(8) O5 0.0202(9) 0.0217(9) 0.0165(8) 0.0052(7) 0.0087(7) 0.0074(7) O6 0.0183(9) 0.0243(9) 0.0182(9) 0.0055(7) 0.0087(7) 0.0074(7) C1 0.0276(14) 0.0260(14) 0.0283(14) 0.0151(12) 0.0127(12) 0.0125(11) C2 0.0197(12) 0.0211(12) 0.0135(11) 0.0056(9) 0.0029(9) 0.0084(10) C3 0.0168(12) 0.0194(12) 0.0164(11) 0.0053(9) 0.0046(9) 0.0082(9) C4 0.0152(11) 0.0239(13) 0.0160(11) 0.0067(10) 0.0052(9) 0.0089(10) C5 0.0258(14) 0.0247(13) 0.0291(14) 0.0131(11) 0.0156(12) 0.0120(11) C6 0.0172(12) 0.0186(12) 0.0192(12) 0.0072(10) 0.0093(10) 0.0075(9) C7 0.0217(13) 0.0212(12) 0.0195(12) 0.0062(10) 0.0055(10) 0.0055(10) C8 0.0262(14) 0.0190(12) 0.0195(12) 0.0038(10) 0.0108(11) 0.0055(10) C9 0.0212(13) 0.0235(13) 0.0320(15) 0.0087(11) 0.0090(11) 0.0110(11) C10 0.0200(13) 0.0228(13) 0.0195(12) 0.0038(10) 0.0030(10) 0.0071(10) C11 0.0444(18) 0.0236(14) 0.0177(13) 0.0058(11) 0.0073(12) 0.0027(13) C12 0.0182(12) 0.0231(13) 0.0185(12) 0.0078(10) 0.0068(10) 0.0060(10) C13 0.0215(13) 0.0216(12) 0.0188(12) 0.0093(10) 0.0056(10) 0.0077(10) C14 0.0217(13) 0.0229(13) 0.0252(13) 0.0109(11) 0.0077(11) 0.0095(10) C15 0.0461(19) 0.0273(15) 0.0298(15) 0.0127(13) 0.0093(14) 0.0174(14) C16 0.0327(15) 0.0210(13) 0.0204(13) 0.0095(11) 0.0052(11) 0.0041(11) C17 0.0460(19) 0.0319(16) 0.0284(16) 0.0141(13) 0.0013(14) 0.0129(14) C18 0.066(3) 0.0364(18) 0.0287(17) 0.0189(15) -0.0054(17) 0.0063(17) C19 0.057(2) 0.050(2) 0.0256(16) 0.0172(15) 0.0152(16) 0.0017(18) C20 0.0367(17) 0.0376(17) 0.0265(15) 0.0149(13) 0.0108(13) 0.0039(14) C21 0.0199(13) 0.0282(14) 0.0188(12) 0.0053(11) 0.0079(10) 0.0054(11) C22 0.0174(12) 0.0213(12) 0.0155(11) 0.0085(10) 0.0063(9) 0.0085(9) C23 0.0213(12) 0.0194(12) 0.0135(11) 0.0070(9) 0.0066(9) 0.0076(10) C24 0.0239(13) 0.0192(12) 0.0179(12) 0.0071(10) 0.0056(10) 0.0075(10) C25 0.0250(15) 0.0332(16) 0.0244(14) 0.0006(12) 0.0078(12) 0.0006(12) C26 0.0192(12) 0.0193(12) 0.0170(11) 0.0047(10) 0.0072(10) 0.0060(10) C27 0.052(2) 0.0277(15) 0.0289(15) 0.0150(12) 0.0262(15) 0.0197(14) C28 0.053(2) 0.0252(15) 0.0392(18) 0.0145(13) 0.0286(16) 0.0202(14) C29 0.0349(16) 0.0398(17) 0.0176(13) 0.0096(12) 0.0107(12) 0.0150(13) C30 0.0338(16) 0.0328(15) 0.0188(13) 0.0110(11) 0.0093(11) 0.0178(13) N1 0.0249(12) 0.0201(11) 0.0298(12) 0.0094(10) 0.0141(10) 0.0099(9) N2 0.072(2) 0.0434(17) 0.0263(14) 0.0172(13) 0.0057(15) -0.0006(16) N3 0.0298(13) 0.0267(12) 0.0229(12) 0.0034(10) 0.0116(10) 0.0076(10) I1 0.02231(9) 0.01991(9) 0.03019(10) 0.00715(7) 0.01466(7) 0.00826(7) I2 0.02406(9) 0.02190(9) 0.02148(9) 0.00496(7) 0.01209(7) 0.00767(7) F1 0.0274(9) 0.0345(9) 0.0205(8) 0.0100(7) 0.0110(7) 0.0104(7) F2 0.0242(8) 0.0312(9) 0.0247(8) 0.0104(7) 0.0090(7) 0.0127(7) F3 0.0390(10) 0.0555(12) 0.0305(9) 0.0272(9) 0.0171(8) 0.0234(9) F4 0.0322(10) 0.0435(11) 0.0423(10) 0.0255(9) 0.0160(8) 0.0224(8) C31 0.0221(13) 0.0181(12) 0.0260(13) 0.0057(10) 0.0113(11) 0.0051(10) C32 0.0220(13) 0.0208(12) 0.0209(12) 0.0065(10) 0.0093(10) 0.0050(10) C33 0.0198(13) 0.0179(12) 0.0230(13) 0.0053(10) 0.0071(10) 0.0069(10) C34 0.0221(13) 0.0205(12) 0.0223(13) 0.0056(10) 0.0105(11) 0.0064(10) C35 0.0278(15) 0.0273(14) 0.0256(14) 0.0126(12) 0.0121(12) 0.0082(11) C36 0.0224(14) 0.0252(14) 0.0336(15) 0.0140(12) 0.0093(12) 0.0117(11) Cl1 0.0427(5) 0.0446(5) 0.0439(5) 0.0233(4) 0.0037(4) 0.0079(4) Cl3 0.0370(5) 0.0647(6) 0.0517(5) 0.0229(5) -0.0003(4) 0.0117(4) Cl2 0.0928(8) 0.0376(5) 0.0613(6) 0.0196(4) 0.0458(6) 0.0224(5) C40 0.0339(17) 0.0327(16) 0.0417(18) 0.0178(14) 0.0110(14) 0.0097(13) _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 Fe1 O5 1.9678(18) . ? Fe1 O3 1.9825(18) . ? Fe1 O1 1.9904(18) . ? Fe1 O6 1.9940(18) . ? Fe1 O2 1.9966(18) . ? Fe1 O4 2.0121(19) . ? O1 C2 1.279(3) . ? O2 C4 1.286(3) . ? O3 C12 1.281(3) . ? O4 C14 1.277(3) . ? O5 C22 1.283(3) . ? O6 C24 1.279(3) . ? C1 C2 1.504(4) . ? C2 C3 1.412(4) . ? C3 C4 1.405(4) . ? C3 C6 1.490(3) . ? C4 C5 1.505(4) . ? C6 C10 1.394(4) . ? C6 C7 1.394(3) . ? C7 C8 1.388(4) . ? C8 N1 1.334(4) . ? C9 N1 1.330(4) . ? C9 C10 1.388(4) . ? C11 C12 1.506(4) . ? C12 C13 1.400(4) . ? C13 C14 1.414(4) . ? C13 C16 1.499(4) . ? C14 C15 1.503(4) . ? C16 C20 1.385(4) . ? C16 C17 1.400(4) . ? C17 C18 1.396(5) . ? C18 N2 1.325(5) . ? C19 N2 1.319(5) . ? C19 C20 1.382(4) . ? C21 C22 1.514(4) . ? C22 C23 1.406(4) . ? C23 C24 1.411(4) . ? C23 C26 1.501(3) . ? C24 C25 1.502(4) . ? C26 C27 1.382(4) . ? C26 C30 1.388(4) . ? C27 C28 1.387(4) . ? C28 N3 1.333(4) . ? C29 N3 1.326(4) . ? C29 C30 1.383(4) . ? I1 C31 2.095(3) . ? I2 C34 2.096(3) . ? F1 C32 1.347(3) . ? F2 C33 1.346(3) . ? F3 C35 1.348(3) . ? F4 C36 1.350(3) . ? C31 C32 1.380(4) . ? C31 C36 1.388(4) . ? C32 C33 1.383(4) . ? C33 C34 1.383(4) . ? C34 C35 1.390(4) . ? C35 C36 1.376(4) . ? Cl1 C40 1.766(3) . ? Cl3 C40 1.756(3) . ? Cl2 C40 1.754(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 O5 Fe1 O3 95.81(8) . . ? O5 Fe1 O1 91.45(8) . . ? O3 Fe1 O1 88.16(7) . . ? O5 Fe1 O6 86.17(7) . . ? O3 Fe1 O6 172.26(8) . . ? O1 Fe1 O6 99.29(8) . . ? O5 Fe1 O2 173.25(8) . . ? O3 Fe1 O2 90.27(8) . . ? O1 Fe1 O2 85.82(7) . . ? O6 Fe1 O2 88.18(8) . . ? O5 Fe1 O4 94.45(8) . . ? O3 Fe1 O4 84.12(7) . . ? O1 Fe1 O4 170.72(7) . . ? O6 Fe1 O4 88.27(8) . . ? O2 Fe1 O4 89.05(8) . . ? C2 O1 Fe1 128.30(17) . . ? C4 O2 Fe1 127.61(17) . . ? C12 O3 Fe1 126.47(17) . . ? C14 O4 Fe1 127.96(17) . . ? C22 O5 Fe1 129.94(17) . . ? C24 O6 Fe1 129.50(17) . . ? O1 C2 C3 124.2(2) . . ? O1 C2 C1 115.9(2) . . ? C3 C2 C1 119.8(2) . . ? C4 C3 C2 122.6(2) . . ? C4 C3 C6 117.7(2) . . ? C2 C3 C6 119.5(2) . . ? O2 C4 C3 123.9(2) . . ? O2 C4 C5 115.2(2) . . ? C3 C4 C5 120.9(2) . . ? C10 C6 C7 116.7(2) . . ? C10 C6 C3 121.8(2) . . ? C7 C6 C3 121.4(2) . . ? C8 C7 C6 119.7(2) . . ? N1 C8 C7 123.2(2) . . ? N1 C9 C10 123.7(3) . . ? C9 C10 C6 119.4(2) . . ? O3 C12 C13 124.4(2) . . ? O3 C12 C11 114.1(2) . . ? C13 C12 C11 121.4(2) . . ? C12 C13 C14 121.1(2) . . ? C12 C13 C16 118.5(2) . . ? C14 C13 C16 120.4(2) . . ? O4 C14 C13 123.5(2) . . ? O4 C14 C15 115.6(2) . . ? C13 C14 C15 120.8(2) . . ? C20 C16 C17 116.5(3) . . ? C20 C16 C13 120.1(3) . . ? C17 C16 C13 123.4(3) . . ? C18 C17 C16 118.3(3) . . ? N2 C18 C17 125.0(3) . . ? N2 C19 C20 124.7(4) . . ? C19 C20 C16 119.8(3) . . ? O5 C22 C23 124.2(2) . . ? O5 C22 C21 115.1(2) . . ? C23 C22 C21 120.7(2) . . ? C22 C23 C24 122.3(2) . . ? C22 C23 C26 118.3(2) . . ? C24 C23 C26 119.4(2) . . ? O6 C24 C23 124.1(2) . . ? O6 C24 C25 115.7(2) . . ? C23 C24 C25 120.2(2) . . ? C27 C26 C30 117.1(2) . . ? C27 C26 C23 121.1(2) . . ? C30 C26 C23 121.8(2) . . ? C26 C27 C28 119.3(3) . . ? N3 C28 C27 123.7(3) . . ? N3 C29 C30 123.7(3) . . ? C29 C30 C26 119.5(3) . . ? C9 N1 C8 117.2(2) . . ? C19 N2 C18 115.6(3) . . ? C29 N3 C28 116.7(2) . . ? C32 C31 C36 116.7(2) . . ? C32 C31 I1 120.9(2) . . ? C36 C31 I1 122.4(2) . . ? F1 C32 C31 120.0(2) . . ? F1 C32 C33 118.2(2) . . ? C31 C32 C33 121.8(3) . . ? F2 C33 C34 120.0(2) . . ? F2 C33 C32 118.4(2) . . ? C34 C33 C32 121.6(2) . . ? C33 C34 C35 116.6(2) . . ? C33 C34 I2 120.9(2) . . ? C35 C34 I2 122.5(2) . . ? F3 C35 C36 118.7(3) . . ? F3 C35 C34 119.5(2) . . ? C36 C35 C34 121.7(3) . . ? F4 C36 C35 118.4(3) . . ? F4 C36 C31 120.0(2) . . ? C35 C36 C31 121.6(3) . . ? Cl2 C40 Cl3 111.64(19) . . ? Cl2 C40 Cl1 110.34(18) . . ? Cl3 C40 Cl1 109.07(18) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.873 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 935898' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3_iam #TrackingRef 'complete_all_iam.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Al N3 O6, 1.5(C6 F4 I2), H2 O' _chemical_formula_sum 'C39 H32 Al F6 I3 N3 O7' _chemical_formula_weight 1176.36 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' Al Al 0.0645 0.0514 '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' I I -0.4742 1.8119 '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' N N 0.0061 0.0033 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8817(8) _cell_length_b 14.0348(8) _cell_length_c 14.2560(8) _cell_angle_alpha 63.3512(8) _cell_angle_beta 71.0117(8) _cell_angle_gamma 76.0783(8) _cell_volume 2164.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8510 _cell_measurement_theta_min 2.4733 _cell_measurement_theta_max 29.3882 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 2.262 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6480 _exptl_absorpt_correction_T_max 0.8762 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_detector_area_resol_mean ? _diffrn_radiation_source 'Incoatec microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54848 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 52.23 _reflns_number_total 48264 _reflns_number_gt 27901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0232P)^2^+0.0000P] 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 48264 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _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 Al1 Al 0.49692(4) 0.76003(4) 0.24335(4) 0.01345(7) Uani 1 1 d . . . O1 O 0.45502(9) 0.72142(9) 0.15082(9) 0.01512(16) Uani 1 1 d . . . O2 O 0.64339(9) 0.75520(9) 0.16041(9) 0.01561(16) Uani 1 1 d . . . O3 O 0.35087(10) 0.75787(9) 0.32682(9) 0.01624(17) Uani 1 1 d . . . O4 O 0.52330(9) 0.61368(9) 0.33085(9) 0.01398(15) Uani 1 1 d . . . O5 O 0.54130(10) 0.79899(9) 0.33184(9) 0.01656(17) Uani 1 1 d . . . O6 O 0.46284(10) 0.90282(9) 0.15703(9) 0.01593(17) Uani 1 1 d . . . C1 C 0.45113(14) 0.60348(16) 0.07589(17) 0.0237(3) Uani 1 1 d . . . H1A H 0.4498 0.5283 0.1276 0.035 Uiso 1 1 calc R . . H1B H 0.4872 0.6070 0.0025 0.035 Uiso 1 1 calc R . . H1C H 0.3753 0.6388 0.0787 0.035 Uiso 1 1 calc R . . C2 C 0.51424(12) 0.65933(12) 0.10484(12) 0.0147(2) Uani 1 1 d . . . C3 C 0.63014(12) 0.64252(12) 0.08230(12) 0.01446(19) Uani 1 1 d . . . C4 C 0.68911(12) 0.69977(12) 0.10469(12) 0.0149(2) Uani 1 1 d . . . C5 C 0.81147(13) 0.70187(15) 0.05855(15) 0.0220(3) Uani 1 1 d . . . H5A H 0.8265 0.7712 -0.0022 0.033 Uiso 1 1 calc R . . H5B H 0.8417 0.6442 0.0330 0.033 Uiso 1 1 calc R . . H5C H 0.8462 0.6916 0.1147 0.033 Uiso 1 1 calc R . . C6 C 0.69189(12) 0.57187(13) 0.02498(13) 0.0168(2) Uani 1 1 d . . . C7 C 0.70382(16) 0.60402(16) -0.08526(15) 0.0234(3) Uani 1 1 d . . . H7 H 0.6718 0.6728 -0.1263 0.028 Uiso 1 1 calc R . . C8 C 0.76272(18) 0.53501(19) -0.13467(18) 0.0294(4) Uani 1 1 d . . . H8 H 0.7697 0.5586 -0.2100 0.035 Uiso 1 1 calc R . . C9 C 0.79870(18) 0.40636(17) 0.0234(2) 0.0316(4) Uani 1 1 d . . . H9 H 0.8323 0.3374 0.0620 0.038 Uiso 1 1 calc R . . C10 C 0.74028(16) 0.46961(15) 0.07972(16) 0.0243(3) Uani 1 1 d . . . H10 H 0.7333 0.4433 0.1553 0.029 Uiso 1 1 calc R . . C11 C 0.17242(14) 0.71029(15) 0.41586(16) 0.0239(3) Uani 1 1 d . . . H11A H 0.1613 0.7714 0.4352 0.036 Uiso 1 1 calc R . . H11B H 0.1387 0.6496 0.4790 0.036 Uiso 1 1 calc R . . H11C H 0.1379 0.7303 0.3566 0.036 Uiso 1 1 calc R . . C12 C 0.29373(12) 0.67897(12) 0.38022(12) 0.0154(2) Uani 1 1 d . . . C13 C 0.33881(12) 0.57045(12) 0.40584(12) 0.01453(19) Uani 1 1 d . . . C14 C 0.45422(11) 0.54341(11) 0.37943(11) 0.01329(18) Uani 1 1 d . . . C15 C 0.50568(13) 0.42986(12) 0.40354(13) 0.0169(2) Uani 1 1 d . . . H15A H 0.5863 0.4282 0.3794 0.025 Uiso 1 1 calc R . . H15B H 0.4805 0.4003 0.3652 0.025 Uiso 1 1 calc R . . H15C H 0.4839 0.3869 0.4818 0.025 Uiso 1 1 calc R . . C16 C 0.26472(12) 0.48428(12) 0.46332(12) 0.0156(2) Uani 1 1 d . . . C17 C 0.18757(14) 0.47862(15) 0.41667(14) 0.0205(3) Uani 1 1 d . . . H17 H 0.1807 0.5311 0.3472 0.025 Uiso 1 1 calc R . . C18 C 0.12099(15) 0.39558(16) 0.47266(17) 0.0251(3) Uani 1 1 d . . . H18 H 0.0680 0.3940 0.4402 0.030 Uiso 1 1 calc R . . C19 C 0.20134(15) 0.32335(14) 0.61470(15) 0.0223(3) Uani 1 1 d . . . H19 H 0.2071 0.2689 0.6837 0.027 Uiso 1 1 calc R . . C20 C 0.26966(13) 0.40424(13) 0.56597(14) 0.0187(2) Uani 1 1 d . . . H20 H 0.3195 0.4053 0.6020 0.022 Uiso 1 1 calc R . . C21 C 0.55779(15) 0.89029(15) 0.42882(14) 0.0216(3) Uani 1 1 d . . . H21A H 0.4911 0.8978 0.4841 0.032 Uiso 1 1 calc R . . H21B H 0.6007 0.9504 0.4017 0.032 Uiso 1 1 calc R . . H21C H 0.6027 0.8227 0.4607 0.032 Uiso 1 1 calc R . . C22 C 0.52543(12) 0.89013(12) 0.33673(12) 0.0152(2) Uani 1 1 d . . . C23 C 0.47918(13) 0.98532(12) 0.26410(12) 0.0154(2) Uani 1 1 d . . . C24 C 0.45022(13) 0.98583(12) 0.17659(12) 0.0157(2) Uani 1 1 d . . . C25 C 0.40143(17) 1.08669(14) 0.09919(14) 0.0235(3) Uani 1 1 d . . . H25A H 0.4191 1.0829 0.0286 0.035 Uiso 1 1 calc R . . H25B H 0.4322 1.1483 0.0909 0.035 Uiso 1 1 calc R . . H25C H 0.3210 1.0950 0.1274 0.035 Uiso 1 1 calc R . . C26 C 0.46327(13) 1.08794(12) 0.27706(12) 0.0163(2) Uani 1 1 d . . . C27 C 0.36292(14) 1.12298(14) 0.33431(13) 0.0195(2) Uani 1 1 d . . . H27 H 0.3036 1.0799 0.3688 0.023 Uiso 1 1 calc R . . C28 C 0.35053(17) 1.22112(15) 0.34041(15) 0.0236(3) Uani 1 1 d . . . H28 H 0.2814 1.2433 0.3798 0.028 Uiso 1 1 calc R . . C29 C 0.52557(19) 1.25206(17) 0.24120(19) 0.0293(4) Uani 1 1 d . . . H29 H 0.5835 1.2966 0.2087 0.035 Uiso 1 1 calc R . . C30 C 0.54698(16) 1.15505(16) 0.22975(18) 0.0258(3) Uani 1 1 d . . . H30 H 0.6173 1.1350 0.1904 0.031 Uiso 1 1 calc R . . N1 N 0.81015(15) 0.43747(16) -0.08285(17) 0.0298(3) Uani 1 1 d . . . N2 N 0.12747(13) 0.31783(14) 0.56957(15) 0.0252(3) Uani 1 1 d . . . N3 N 0.42965(17) 1.28636(13) 0.29445(15) 0.0265(3) Uani 1 1 d . . . I1 I 0.095752(9) 0.109600(9) 0.607417(11) 0.02251(2) Uani 1 1 d . . . I2 I 0.059328(12) -0.425885(10) 0.732522(11) 0.02660(3) Uani 1 1 d . . . F1 F -0.10930(10) -0.01805(12) 0.66416(15) 0.0368(3) Uani 1 1 d . . . F2 F -0.12228(11) -0.22302(12) 0.71710(16) 0.0394(4) Uani 1 1 d . . . F3 F 0.27854(10) -0.08977(11) 0.60599(15) 0.0377(3) Uani 1 1 d . . . F4 F 0.26580(11) -0.29336(11) 0.65469(14) 0.0369(3) Uani 1 1 d . . . C31 C 0.08479(13) -0.04781(14) 0.63472(15) 0.0204(3) Uani 1 1 d . . . C32 C -0.01559(14) -0.08510(15) 0.66209(17) 0.0237(3) Uani 1 1 d . . . C33 C -0.02244(14) -0.19138(16) 0.68896(17) 0.0240(3) Uani 1 1 d . . . C34 C 0.07131(15) -0.26516(14) 0.68864(15) 0.0213(3) Uani 1 1 d . . . C35 C 0.17198(15) -0.22699(15) 0.65824(17) 0.0240(3) Uani 1 1 d . . . C36 C 0.17862(14) -0.12082(15) 0.63240(16) 0.0231(3) Uani 1 1 d . . . I3 I 0.246166(11) 0.871092(14) 0.076397(12) 0.03299(3) Uani 1 1 d . . . F5 F 0.06869(12) 1.05619(12) 0.12710(12) 0.0325(3) Uani 1 1 d . . . F6 F 0.12153(14) 0.85022(13) -0.07478(14) 0.0398(4) Uani 1 1 d . . . C37 C 0.10054(15) 0.94937(16) 0.02905(15) 0.0231(3) Uani 1 1 d . . . C38 C 0.03602(16) 1.02723(16) 0.06470(16) 0.0232(3) Uani 1 1 d . . . C39 C 0.06254(16) 0.92406(16) -0.03649(17) 0.0245(3) Uani 1 1 d . . . O7 O 0.99622(15) 0.35503(17) -0.20380(17) 0.0398(4) Uani 1 1 d . . . H7D H 1.0001 0.3181 -0.2449 0.060 Uiso 1 1 d R . . H7E H 0.9216 0.3702 -0.1747 0.060 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.01699(18) 0.01070(17) 0.01320(16) -0.00463(14) -0.00585(14) 0.00002(13) O1 0.0161(4) 0.0146(4) 0.0168(4) -0.0082(3) -0.0061(3) 0.0012(3) O2 0.0177(4) 0.0144(4) 0.0163(4) -0.0066(3) -0.0051(3) -0.0024(3) O3 0.0178(4) 0.0125(4) 0.0170(4) -0.0059(3) -0.0045(3) 0.0012(3) O4 0.0147(4) 0.0116(4) 0.0149(4) -0.0041(3) -0.0052(3) -0.0006(3) O5 0.0231(5) 0.0124(4) 0.0161(4) -0.0057(3) -0.0092(4) 0.0005(3) O6 0.0230(5) 0.0115(4) 0.0145(4) -0.0051(3) -0.0078(3) 0.0001(3) C1 0.0201(6) 0.0277(8) 0.0349(9) -0.0214(7) -0.0104(6) -0.0005(5) C2 0.0165(5) 0.0135(5) 0.0157(5) -0.0060(4) -0.0066(4) -0.0005(4) C3 0.0162(5) 0.0127(5) 0.0157(5) -0.0066(4) -0.0053(4) -0.0004(4) C4 0.0162(5) 0.0128(5) 0.0153(5) -0.0046(4) -0.0048(4) -0.0019(4) C5 0.0160(5) 0.0240(7) 0.0259(7) -0.0108(6) -0.0034(5) -0.0036(5) C6 0.0168(5) 0.0151(5) 0.0199(6) -0.0092(5) -0.0043(4) -0.0002(4) C7 0.0270(7) 0.0245(8) 0.0201(6) -0.0126(6) -0.0052(5) 0.0009(6) C8 0.0298(8) 0.0357(10) 0.0290(8) -0.0234(8) -0.0005(7) -0.0033(7) C9 0.0297(9) 0.0204(8) 0.0469(12) -0.0203(8) -0.0072(8) 0.0034(6) C10 0.0286(8) 0.0160(6) 0.0278(8) -0.0100(6) -0.0087(6) 0.0030(5) C11 0.0162(6) 0.0216(7) 0.0281(8) -0.0098(6) -0.0018(5) 0.0024(5) C12 0.0158(5) 0.0142(5) 0.0155(5) -0.0066(4) -0.0052(4) 0.0026(4) C13 0.0146(4) 0.0125(5) 0.0164(5) -0.0060(4) -0.0054(4) 0.0011(4) C14 0.0145(4) 0.0115(4) 0.0147(5) -0.0056(4) -0.0056(4) 0.0006(3) C15 0.0187(5) 0.0119(5) 0.0197(6) -0.0071(4) -0.0053(4) 0.0012(4) C16 0.0143(5) 0.0148(5) 0.0180(5) -0.0064(4) -0.0047(4) -0.0015(4) C17 0.0189(6) 0.0222(7) 0.0220(6) -0.0073(5) -0.0082(5) -0.0038(5) C18 0.0217(7) 0.0261(8) 0.0320(8) -0.0120(7) -0.0098(6) -0.0055(6) C19 0.0210(6) 0.0169(6) 0.0239(7) -0.0043(5) -0.0038(5) -0.0038(5) C20 0.0183(5) 0.0156(6) 0.0209(6) -0.0045(5) -0.0068(5) -0.0024(4) C21 0.0282(7) 0.0211(7) 0.0223(6) -0.0114(6) -0.0141(6) 0.0014(5) C22 0.0177(5) 0.0151(5) 0.0155(5) -0.0073(4) -0.0065(4) -0.0006(4) C23 0.0207(5) 0.0117(5) 0.0154(5) -0.0061(4) -0.0065(4) -0.0006(4) C24 0.0213(5) 0.0121(5) 0.0139(5) -0.0047(4) -0.0063(4) -0.0006(4) C25 0.0376(9) 0.0138(6) 0.0190(6) -0.0048(5) -0.0139(6) 0.0031(6) C26 0.0208(6) 0.0131(5) 0.0171(5) -0.0071(4) -0.0070(4) -0.0002(4) C27 0.0235(6) 0.0171(6) 0.0193(6) -0.0095(5) -0.0059(5) 0.0005(5) C28 0.0312(8) 0.0200(7) 0.0231(7) -0.0128(6) -0.0105(6) 0.0044(6) C29 0.0339(9) 0.0210(8) 0.0390(10) -0.0137(7) -0.0109(8) -0.0080(7) C30 0.0241(7) 0.0204(7) 0.0348(9) -0.0134(7) -0.0040(6) -0.0064(6) N1 0.0233(7) 0.0291(8) 0.0431(10) -0.0257(8) -0.0005(6) -0.0020(6) N2 0.0191(6) 0.0213(6) 0.0338(8) -0.0092(6) -0.0054(5) -0.0056(5) N3 0.0406(9) 0.0178(6) 0.0304(7) -0.0132(6) -0.0184(7) 0.0010(6) I1 0.01600(4) 0.01769(4) 0.03200(5) -0.00985(4) -0.00431(3) -0.00141(3) I2 0.03227(6) 0.01855(5) 0.03109(6) -0.00841(4) -0.01329(5) -0.00231(4) F1 0.0156(4) 0.0274(6) 0.0683(10) -0.0221(7) -0.0127(5) 0.0045(4) F2 0.0215(5) 0.0285(7) 0.0705(11) -0.0180(7) -0.0163(6) -0.0044(5) F3 0.0140(4) 0.0250(6) 0.0661(10) -0.0141(6) -0.0069(5) -0.0014(4) F4 0.0214(5) 0.0211(6) 0.0571(9) -0.0124(6) -0.0064(5) 0.0054(4) C31 0.0159(5) 0.0173(6) 0.0274(7) -0.0088(5) -0.0058(5) -0.0004(4) C32 0.0155(5) 0.0218(7) 0.0362(9) -0.0138(7) -0.0089(6) 0.0013(5) C33 0.0179(6) 0.0219(7) 0.0355(9) -0.0121(7) -0.0103(6) -0.0019(5) C34 0.0220(6) 0.0175(6) 0.0257(7) -0.0084(5) -0.0091(5) -0.0006(5) C35 0.0181(6) 0.0186(7) 0.0303(8) -0.0081(6) -0.0055(5) 0.0020(5) C36 0.0145(5) 0.0199(7) 0.0312(8) -0.0085(6) -0.0043(5) -0.0011(5) I3 0.02304(5) 0.04075(8) 0.03314(6) -0.01326(6) -0.01461(5) 0.00717(5) F5 0.0390(7) 0.0360(7) 0.0355(7) -0.0205(6) -0.0177(6) -0.0027(6) F6 0.0428(8) 0.0375(8) 0.0510(9) -0.0327(7) -0.0211(7) 0.0177(6) C37 0.0202(6) 0.0254(8) 0.0254(7) -0.0111(6) -0.0111(5) 0.0039(5) C38 0.0260(7) 0.0233(7) 0.0259(7) -0.0125(6) -0.0120(6) 0.0005(6) C39 0.0268(7) 0.0215(7) 0.0300(8) -0.0156(7) -0.0118(6) 0.0063(6) O7 0.0269(7) 0.0521(12) 0.0514(11) -0.0362(10) -0.0031(7) -0.0021(7) _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 Al1 O6 1.8545(12) . ? Al1 O5 1.8589(12) . ? Al1 O3 1.8695(13) . ? Al1 O2 1.8765(13) . ? Al1 O4 1.8793(12) . ? Al1 O1 1.8896(12) . ? O1 C2 1.2798(17) . ? O2 C4 1.2699(18) . ? O3 C12 1.2723(19) . ? O4 C14 1.2856(17) . ? O5 C22 1.2758(18) . ? O6 C24 1.2776(18) . ? C1 C2 1.504(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.405(2) . ? C3 C4 1.416(2) . ? C3 C6 1.486(2) . ? C4 C5 1.499(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.392(2) . ? C6 C10 1.392(2) . ? C7 C8 1.386(2) . ? C7 H7 0.9500 . ? C8 N1 1.333(3) . ? C8 H8 0.9500 . ? C9 N1 1.341(3) . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.499(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.4156(19) . ? C13 C14 1.4101(19) . ? C13 C16 1.484(2) . ? C14 C15 1.4987(19) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.397(2) . ? C16 C20 1.400(2) . ? C17 C18 1.390(3) . ? C17 H17 0.9500 . ? C18 N2 1.336(3) . ? C18 H18 0.9500 . ? C19 N2 1.343(2) . ? C19 C20 1.386(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.502(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.410(2) . ? C23 C24 1.4105(19) . ? C23 C26 1.491(2) . ? C24 C25 1.496(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.395(2) . ? C26 C30 1.397(2) . ? C27 C28 1.387(2) . ? C27 H27 0.9500 . ? C28 N3 1.335(3) . ? C28 H28 0.9500 . ? C29 N3 1.329(3) . ? C29 C30 1.395(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? I1 C31 2.0965(18) . ? I2 C34 2.0839(18) . ? F1 C32 1.341(2) . ? F2 C33 1.338(2) . ? F3 C36 1.340(2) . ? F4 C35 1.338(2) . ? C31 C32 1.383(2) . ? C31 C36 1.386(2) . ? C32 C33 1.381(3) . ? C33 C34 1.389(2) . ? C34 C35 1.385(3) . ? C35 C36 1.383(3) . ? I3 C37 2.0853(17) . ? F5 C38 1.336(2) . ? F6 C39 1.345(2) . ? C37 C39 1.385(3) . ? C37 C38 1.389(3) . ? C38 C39 1.382(2) 2_575 ? C39 C38 1.382(2) 2_575 ? O7 H7D 0.9242 . ? O7 H7E 0.9287 . ? 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 Al1 O5 91.11(5) . . ? O6 Al1 O3 88.90(6) . . ? O5 Al1 O3 91.96(6) . . ? O6 Al1 O2 93.36(6) . . ? O5 Al1 O2 89.75(6) . . ? O3 Al1 O2 177.13(6) . . ? O6 Al1 O4 176.56(6) . . ? O5 Al1 O4 91.28(5) . . ? O3 Al1 O4 88.54(5) . . ? O2 Al1 O4 89.13(5) . . ? O6 Al1 O1 88.54(5) . . ? O5 Al1 O1 178.61(6) . . ? O3 Al1 O1 89.37(5) . . ? O2 Al1 O1 88.93(5) . . ? O4 Al1 O1 89.13(5) . . ? C2 O1 Al1 125.42(10) . . ? C4 O2 Al1 127.87(10) . . ? C12 O3 Al1 128.43(10) . . ? C14 O4 Al1 127.54(9) . . ? C22 O5 Al1 128.90(10) . . ? C24 O6 Al1 129.11(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.62(13) . . ? O1 C2 C1 115.31(13) . . ? C3 C2 C1 121.07(13) . . ? C2 C3 C4 120.62(13) . . ? C2 C3 C6 119.62(13) . . ? C4 C3 C6 119.51(13) . . ? O2 C4 C3 123.49(13) . . ? O2 C4 C5 115.60(14) . . ? C3 C4 C5 120.86(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C10 116.80(15) . . ? C7 C6 C3 121.96(14) . . ? C10 C6 C3 121.24(15) . . ? C8 C7 C6 119.51(18) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? N1 C8 C7 123.9(2) . . ? N1 C8 H8 118.0 . . ? C7 C8 H8 118.0 . . ? N1 C9 C10 123.4(2) . . ? N1 C9 H9 118.3 . . ? C10 C9 H9 118.3 . . ? C9 C10 C6 119.72(19) . . ? C9 C10 H10 120.1 . . ? C6 C10 H10 120.1 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 C13 124.00(13) . . ? O3 C12 C11 114.07(14) . . ? C13 C12 C11 121.93(15) . . ? C14 C13 C12 120.28(13) . . ? C14 C13 C16 119.67(13) . . ? C12 C13 C16 120.03(13) . . ? O4 C14 C13 123.04(13) . . ? O4 C14 C15 114.75(12) . . ? C13 C14 C15 122.19(13) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C20 116.87(15) . . ? C17 C16 C13 121.40(14) . . ? C20 C16 C13 121.73(13) . . ? C18 C17 C16 119.49(16) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? N2 C18 C17 123.61(16) . . ? N2 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? N2 C19 C20 123.49(17) . . ? N2 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C16 119.54(15) . . ? C19 C20 H20 120.2 . . ? C16 C20 H20 120.2 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 C23 124.24(13) . . ? O5 C22 C21 115.09(13) . . ? C23 C22 C21 120.66(13) . . ? C22 C23 C24 120.82(13) . . ? C22 C23 C26 120.21(13) . . ? C24 C23 C26 118.95(13) . . ? O6 C24 C23 123.81(13) . . ? O6 C24 C25 115.21(13) . . ? C23 C24 C25 120.99(14) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C30 116.86(15) . . ? C27 C26 C23 121.53(15) . . ? C30 C26 C23 121.58(15) . . ? C28 C27 C26 119.47(17) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? N3 C28 C27 124.10(18) . . ? N3 C28 H28 117.9 . . ? C27 C28 H28 117.9 . . ? N3 C29 C30 124.44(19) . . ? N3 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? C29 C30 C26 118.87(18) . . ? C29 C30 H30 120.6 . . ? C26 C30 H30 120.6 . . ? C8 N1 C9 116.66(17) . . ? C18 N2 C19 116.96(16) . . ? C29 N3 C28 116.24(16) . . ? C32 C31 C36 117.24(16) . . ? C32 C31 I1 121.99(12) . . ? C36 C31 I1 120.65(13) . . ? F1 C32 C33 118.42(16) . . ? F1 C32 C31 120.15(17) . . ? C33 C32 C31 121.43(16) . . ? F2 C33 C32 118.57(16) . . ? F2 C33 C34 120.00(17) . . ? C32 C33 C34 121.42(16) . . ? C35 C34 C33 117.03(16) . . ? C35 C34 I2 122.00(13) . . ? C33 C34 I2 120.97(13) . . ? F4 C35 C36 118.33(17) . . ? F4 C35 C34 120.21(17) . . ? C36 C35 C34 121.46(16) . . ? F3 C36 C35 118.36(16) . . ? F3 C36 C31 120.25(17) . . ? C35 C36 C31 121.38(16) . . ? C39 C37 C38 117.25(15) . . ? C39 C37 I3 121.63(13) . . ? C38 C37 I3 121.09(13) . . ? F5 C38 C39 118.91(17) . 2_575 ? F5 C38 C37 120.21(17) . . ? C39 C38 C37 120.88(16) 2_575 . ? F6 C39 C38 117.80(17) . 2_575 ? F6 C39 C37 120.34(17) . . ? C38 C39 C37 121.86(16) 2_575 . ? H7D O7 H7E 106.3 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 52.23 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 4.898 _refine_diff_density_min -3.385 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 935899'