#------------------------------------------------------------------------------ #$Date: 2026-05-11 23:53:49 +0100 (Mon, 11 May 2026) $ #$Revision: 305925 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721016.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7721016 loop_ _publ_author_name 'Dollberg, Kevin' 'Lochte, Mark' 'Wei\&s, Pauline' 'Nitzsche, Joel' 'M\'esz\'aros, Katalin' 'von H\"anisch, Carsten' 'Tambornino, Frank' _publ_section_title ; Synthesis of Lewis acid-base adducts between trimesityltrieles and potassium cyanate and its heavier homologues ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00831C _journal_year 2026 _chemical_formula_moiety 'C40 H57 Al K N O7, 2(C6 H4 F2)' _chemical_formula_sum 'C52 H65 Al F4 K N O7' _chemical_formula_weight 958.13 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _audit_creation_date 2026-04-10 _audit_creation_method ; Olex2 1.5 (compiled 2026.03.20 svn.r2bc28608 for OlexSys, GUI svn.r7530) ; _audit_update_record ; 2026-04-10 deposited with the CCDC. 2026-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.3321(2) _cell_length_b 24.4640(5) _cell_length_c 29.1550(6) _cell_measurement_reflns_used 83142 _cell_measurement_temperature 100 _cell_measurement_theta_max 75.98 _cell_measurement_theta_min 3.03 _cell_volume 10222.3(3) _computing_cell_refinement 'X-Area Recipe 2.0.2 (STOE, 2024)' _computing_data_collection 'X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)' _computing_data_reduction ; X-Area Integrate 2.5.18.0 (STOE, 2024) X-Area LANA 2.8.4 (STOE, 2024) ; _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.00 _diffrn_detector 'hybrid photon-counting area detector' _diffrn_detector_area_resol_mean 5.81 _diffrn_detector_type 'DECTRIS PILATUS3 R 300K' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details '5045 frames, detector distance = 70 mm' _diffrn_measurement_device '4-circle diffractometer' _diffrn_measurement_device_type 'STOE STADIVARI' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'graded multilayer mirror' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54186 _diffrn_radiation_xray_symbol K-L~2,3~ _diffrn_reflns_av_R_equivalents 0.1193 _diffrn_reflns_av_unetI/netI 0.0477 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 163614 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 66.598 _diffrn_reflns_theta_max 66.598 _diffrn_reflns_theta_min 3.031 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type 'XENOCS GENIX 3D CU HIGH FLUX' _exptl_absorpt_coefficient_mu 1.615 _exptl_absorpt_correction_T_max 0.0293 _exptl_absorpt_correction_T_min 0.0122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; STOE LANA, absorption correction by scaling of reflection intensities. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(\m~2~-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Afterwards a spherical absorption correction was performed within STOE LANA. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 4064 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad 0.062 _refine_diff_density_max 0.631 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 696 _refine_ls_number_reflns 8987 _refine_ls_number_restraints 147 _refine_ls_restrained_S_all 0.974 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0801 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1499P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2070 _refine_ls_wR_factor_ref 0.2228 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5827 _reflns_number_total 8987 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00831c2.cif _cod_data_source_block kdp1 _cod_database_code 7721016 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.924 _shelx_estimated_absorpt_t_min 0.738 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C47-C48 = C47-C54 = C48-C49 1.39 with sigma of 0.02 C48-F9 1.35 with sigma of 0.02 C49-C56 = C56-C55 = C55-C54 1.4 with sigma of 0.02 C47-C49 = C49-C55 = C56-C54 2.42 with sigma of 0.04 C47-F9 2.37 with sigma of 0.04 C47-C55 = C48-C56 2.4 with sigma of 0.04 C47-C54 \\sim C55-C54 \\sim C47-C48 \\sim C56-C55 \\sim C49-C56 \\sim C48-C49 with sigma of 0.02 C47-F9 \\sim C49-F9 with sigma of 0.04 C56-C54 \\sim C49-C55 \\sim C48-C56 \\sim C47-C49 \\sim C48-C54 \\sim C47-C55 with sigma of 0.04 3. Restrained planarity C47, C48, C49, C56, C55, C54, F9 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C47 \\sim C48 \\sim C49 \\sim C56 \\sim C55 \\sim C54 \\sim F9: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(O1A) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02 5. Rigid body (RIGU) restrains C47, C48, C49, C56, C55, C54, F9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(F2)=Sof(C47)=Sof(C48)=Sof(C49)=Sof(H49)=Sof(C56)=Sof(H56)=Sof(C55)= Sof(H55)=Sof(C54)=Sof(H54)=Sof(F9)=1-FVAR(1) Sof(C50)=Sof(H50)=Sof(C53)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C58)= Sof(C57)=Sof(H57)=Sof(F1)=Sof(F4)=FVAR(1) Sof(O1A)=Sof(C1A)=1-FVAR(2) Sof(C1B)=Sof(O1B)=FVAR(2) 7.a Secondary CH2 refined with riding coordinates: C38(H38A,H38B), C37(H37A,H37B), C39(H39A,H39B), C36(H36A,H36B), C35(H35A, H35B), C40(H40A,H40B), C34(H34A,H34B), C29(H29A,H29B), C33(H33A,H33B), C32(H32A,H32B), C30(H30A,H30B), C31(H31A,H31B) 7.b Aromatic/amide H refined with riding coordinates: C4(H4), C15(H15), C22(H22), C6(H6), C13(H13), C24(H24), C42(H42), C43(H43), C50(H50), C44(H44), C45(H45), C51(H51), C52(H52), C57(H57), C49(H49), C56(H56), C55(H55), C54(H54) 7.c Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C8(H8A,H8B, H8C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C9(H9A,H9B,H9C), C17(H17A,H17B, H17C), C28(H28A,H28B,H28C) ; _shelx_res_file ; TITL kdp1_a.res in Pbca kdp1.res created by SHELXL-2019/3 at 09:22:13 on 10-Apr-2026 REM Old TITL REM SHELXT solution in Pbca: R1 0.224, Rweak 0.023, Alpha 0.059 REM 1.519 for 898 systematic absences, Orientation as input REM Formula found by SHELXT: C55 N8 O3 K Al CELL 1.54186 14.3321 24.464 29.155 90 90 90 ZERR 8 0.0002 0.0005 0.0006 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Al F K N O UNIT 416 520 8 32 8 8 56 DFIX 1.39 C47 C48 C47 C54 C48 C49 DANG 2.42 C47 C49 C49 C55 C56 C54 DANG 2.37 C47 F9 DANG 2.4 C47 C55 C48 C56 DFIX 1.35 C48 F9 DFIX 1.4 C49 C56 C56 C55 C55 C54 SADI C47 C54 C55 C54 C47 C48 C56 C55 C49 C56 C48 C49 SADI 0.04 C47 F9 C49 F9 SADI 0.04 C56 C54 C49 C55 C48 C56 C47 C49 C48 C54 C47 C55 FLAT C47 C48 C49 C56 C55 C54 F9 SIMU C47 C48 C49 C56 C55 C54 F9 RIGU C47 C48 C49 C56 C55 C54 F9 ISOR 0.02 0.02 O1A O1B L.S. 20 0 0 PLAN 11 SIZE 0.05 0.1 0.2 TEMP -173.15 CONF FREE K001 C1A list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 999 0.84 OMIT 1 1 12 OMIT 1 2 14 OMIT 2 1 8 OMIT 3 1 6 OMIT 3 2 3 OMIT 4 1 10 REM REM REM WGHT 0.149900 FVAR 0.14823 0.55019 0.66447 K001 5 0.984038 0.950421 0.702737 11.00000 0.07594 0.06710 = 0.06242 0.00185 -0.01662 0.00063 AL1 3 0.910724 0.712939 0.656501 11.00000 0.04171 0.06767 = 0.03873 -0.00109 0.00036 0.00136 O5 7 0.839230 1.020510 0.723726 11.00000 0.07931 0.06661 = 0.04909 -0.00120 -0.00427 -0.00571 O6 7 0.912023 1.013995 0.632525 11.00000 0.06624 0.07819 = 0.04932 -0.00330 -0.00956 0.00362 N1 6 0.878769 0.786138 0.670019 11.00000 0.05427 0.07498 = 0.06027 -0.00746 -0.00039 -0.00107 O4 7 0.934043 0.966896 0.794537 11.00000 0.12144 0.08362 = 0.05464 0.01012 -0.02417 -0.01877 F007 4 0.364744 0.570927 0.507841 11.00000 0.07905 0.13326 = 0.10481 -0.03209 0.01430 -0.01180 O7 7 1.038723 0.931139 0.612472 11.00000 0.07426 0.08725 = 0.07650 -0.01695 -0.00853 0.00242 F009 4 0.292013 0.471694 0.505986 11.00000 0.15308 0.10010 = 0.10741 -0.03185 0.04301 0.00589 O2 7 1.147794 0.890571 0.684910 11.00000 0.09044 0.07246 = 0.12744 -0.01287 -0.03806 0.01025 C2 1 0.916832 0.667901 0.714979 11.00000 0.03769 0.08867 = 0.03696 -0.00118 0.00143 0.00425 C7 1 0.915111 0.611201 0.710899 11.00000 0.03939 0.08389 = 0.03761 0.00694 -0.00026 0.00796 C20 1 1.032895 0.726066 0.622578 11.00000 0.04747 0.06449 = 0.04005 -0.00010 0.00131 0.00117 C11 1 0.795635 0.685411 0.622156 11.00000 0.04933 0.05895 = 0.03820 0.00190 -0.00098 0.00100 C16 1 0.795226 0.659703 0.578535 11.00000 0.05038 0.06295 = 0.03921 0.00491 0.00049 -0.00121 PART 1 O1A 7 0.850554 0.872506 0.698837 -31.00000 0.06213 0.06238 = 0.11205 -0.01876 0.00993 -0.00196 PART 0 C18 1 0.884399 0.643790 0.554121 11.00000 0.05696 0.08123 = 0.03751 -0.00197 0.00311 0.00310 AFIX 137 H18A 2 0.938008 0.658991 0.570634 11.00000 -1.50000 H18B 2 0.883375 0.658216 0.522767 11.00000 -1.50000 H18C 2 0.889544 0.603861 0.553158 11.00000 -1.50000 AFIX 0 C3 1 0.913648 0.688947 0.760792 11.00000 0.04344 0.09780 = 0.03993 -0.00536 -0.00055 0.00521 C4 1 0.901067 0.652614 0.798033 11.00000 0.03761 0.12902 = 0.03579 -0.00192 -0.00077 0.01344 AFIX 43 H4 2 0.898144 0.667447 0.828112 11.00000 -1.20000 AFIX 0 O3 7 1.058318 0.884762 0.770739 11.00000 0.13093 0.08456 = 0.09765 0.01412 -0.05200 0.00264 PART 1 C1A 1 0.864890 0.829358 0.687613 -31.00000 0.04712 0.07617 = 0.02199 -0.00825 0.00281 0.00102 PART 0 C25 1 1.032774 0.755908 0.580834 11.00000 0.04834 0.06999 = 0.04446 0.00477 -0.00316 -0.00075 C21 1 1.121485 0.712265 0.639818 11.00000 0.04798 0.06769 = 0.04293 0.00309 0.00067 0.00151 C12 1 0.706255 0.692784 0.642100 11.00000 0.04691 0.06431 = 0.04793 0.00099 -0.00008 0.00253 C15 1 0.712073 0.645614 0.556331 11.00000 0.06098 0.06498 = 0.04346 0.00296 -0.00328 -0.00530 AFIX 43 H15 2 0.714974 0.629353 0.526775 11.00000 -1.20000 AFIX 0 C22 1 1.203852 0.725977 0.616084 11.00000 0.04595 0.07363 = 0.04981 0.00613 0.00079 0.00187 AFIX 43 H22 2 1.262521 0.716565 0.629030 11.00000 -1.20000 AFIX 0 C10 1 0.927368 0.583729 0.664632 11.00000 0.05743 0.07224 = 0.04858 0.00266 0.00147 0.00592 AFIX 137 H10A 2 0.868673 0.585659 0.647465 11.00000 -1.50000 H10B 2 0.944740 0.545365 0.669180 11.00000 -1.50000 H10C 2 0.976608 0.602418 0.647368 11.00000 -1.50000 AFIX 0 C6 1 0.902349 0.576474 0.749096 11.00000 0.04931 0.09296 = 0.04944 0.01373 -0.00046 0.01073 AFIX 43 H6 2 0.900215 0.538041 0.744552 11.00000 -1.20000 AFIX 0 C13 1 0.625215 0.677827 0.619517 11.00000 0.04949 0.07251 = 0.05611 0.00248 0.00331 0.00035 AFIX 43 H13 2 0.566992 0.683656 0.634304 11.00000 -1.20000 AFIX 0 C5 1 0.892895 0.597246 0.792976 11.00000 0.04574 0.10494 = 0.04416 0.01382 -0.00238 0.01195 C27 1 0.943508 0.779015 0.560335 11.00000 0.05123 0.09012 = 0.06006 0.02178 -0.00806 -0.00685 AFIX 137 H27A 2 0.889482 0.761440 0.574725 11.00000 -1.50000 H27B 2 0.942550 0.771984 0.527247 11.00000 -1.50000 H27C 2 0.940977 0.818507 0.565827 11.00000 -1.50000 AFIX 0 C23 1 1.201218 0.752773 0.574454 11.00000 0.05094 0.07784 = 0.05416 0.00806 0.00693 -0.00364 C14 1 0.625870 0.654668 0.576145 11.00000 0.05060 0.07281 = 0.05420 0.00661 -0.00596 -0.00682 C38 1 0.830633 1.062836 0.690437 11.00000 0.06064 0.06500 = 0.06258 0.00396 -0.00158 -0.00224 AFIX 23 H38A 2 0.885699 1.087221 0.691708 11.00000 -1.20000 H38B 2 0.774147 1.084932 0.696621 11.00000 -1.20000 AFIX 0 C37 1 0.823728 1.036599 0.643940 11.00000 0.05768 0.07846 = 0.05534 0.00435 -0.00752 0.00088 AFIX 23 H37A 2 0.775756 1.007487 0.644367 11.00000 -1.20000 H37B 2 0.805425 1.064180 0.620778 11.00000 -1.20000 AFIX 0 C24 1 1.115879 0.767554 0.557354 11.00000 0.05668 0.07875 = 0.04692 0.01156 0.00143 -0.00199 AFIX 43 H24 2 1.112866 0.786203 0.528811 11.00000 -1.20000 AFIX 0 C8 1 0.920713 0.748973 0.770483 11.00000 0.07243 0.10502 = 0.04909 -0.01597 -0.00358 0.00543 AFIX 137 H8A 2 0.968695 0.765183 0.750773 11.00000 -1.50000 H8B 2 0.937568 0.754529 0.802724 11.00000 -1.50000 H8C 2 0.860494 0.766455 0.764289 11.00000 -1.50000 AFIX 0 C39 1 0.845163 1.041969 0.768998 11.00000 0.07467 0.08348 = 0.05260 -0.01138 0.00095 -0.01409 AFIX 23 H39A 2 0.790257 1.065276 0.775483 11.00000 -1.20000 H39B 2 0.902077 1.064586 0.772172 11.00000 -1.20000 AFIX 0 C41 1 0.281314 0.563469 0.526421 11.00000 0.06725 0.09263 = 0.06201 -0.01765 0.00237 0.00132 C19 1 0.694771 0.716461 0.689885 11.00000 0.04994 0.08206 = 0.05770 -0.01211 0.00914 0.00117 AFIX 137 H19A 2 0.745867 0.703728 0.709501 11.00000 -1.50000 H19B 2 0.635048 0.704480 0.702802 11.00000 -1.50000 H19C 2 0.695983 0.756464 0.688205 11.00000 -1.50000 AFIX 0 C26 1 1.134194 0.682078 0.684683 11.00000 0.04905 0.10246 = 0.04971 0.02004 -0.00377 0.00059 AFIX 137 H26A 2 1.100627 0.701375 0.709084 11.00000 -1.50000 H26B 2 1.200733 0.680407 0.692298 11.00000 -1.50000 H26C 2 1.109452 0.644900 0.681726 11.00000 -1.50000 AFIX 0 C36 1 0.913302 0.987160 0.589342 11.00000 0.07472 0.10583 = 0.04910 -0.00945 -0.01128 -0.00226 AFIX 23 H36A 2 0.890115 1.012223 0.565242 11.00000 -1.20000 H36B 2 0.871896 0.954786 0.590242 11.00000 -1.20000 AFIX 0 C46 1 0.244258 0.513471 0.525313 11.00000 0.10158 0.08773 = 0.06435 -0.02017 0.01829 0.00370 C9 1 0.875372 0.560864 0.834244 11.00000 0.07634 0.14365 = 0.04931 0.02872 0.00367 0.01743 AFIX 137 H9A 2 0.933591 0.556151 0.851424 11.00000 -1.50000 H9B 2 0.852831 0.525120 0.823876 11.00000 -1.50000 H9C 2 0.828377 0.577827 0.854083 11.00000 -1.50000 AFIX 0 C17 1 0.535761 0.638390 0.552595 11.00000 0.05993 0.09856 = 0.05875 0.00667 -0.00950 -0.01488 AFIX 137 H17A 2 0.549861 0.622721 0.522446 11.00000 -1.50000 H17B 2 0.496122 0.670713 0.548780 11.00000 -1.50000 H17C 2 0.503045 0.611213 0.571335 11.00000 -1.50000 AFIX 0 C28 1 1.291045 0.766614 0.549002 11.00000 0.05742 0.10945 = 0.06994 0.02464 0.01367 -0.00175 AFIX 137 H28A 2 1.311140 0.803607 0.557292 11.00000 -1.50000 H28B 2 1.280007 0.764759 0.515866 11.00000 -1.50000 H28C 2 1.339749 0.740375 0.557481 11.00000 -1.50000 AFIX 0 C35 1 1.009697 0.969990 0.578544 11.00000 0.07455 0.11167 = 0.05998 -0.02213 -0.00566 0.00039 AFIX 23 H35A 2 1.012014 0.953212 0.547664 11.00000 -1.20000 H35B 2 1.051811 1.002064 0.578824 11.00000 -1.20000 AFIX 0 C42 1 0.234964 0.605838 0.546903 11.00000 0.08396 0.08977 = 0.07917 -0.02672 -0.00602 0.00866 AFIX 43 H42 2 0.262445 0.641134 0.548356 11.00000 -1.20000 AFIX 0 C40 1 0.848350 0.995416 0.801848 11.00000 0.10241 0.10581 = 0.05033 -0.00329 -0.00347 -0.01971 AFIX 23 H40A 2 0.845184 1.009094 0.833769 11.00000 -1.20000 H40B 2 0.794778 0.970650 0.796592 11.00000 -1.20000 AFIX 0 C43 1 0.148920 0.596735 0.565178 11.00000 0.08269 0.11638 = 0.09734 -0.03852 0.00892 0.00991 AFIX 43 H43 2 0.115488 0.626003 0.578908 11.00000 -1.20000 AFIX 0 C34 1 1.132161 0.913694 0.606524 11.00000 0.07485 0.09280 = 0.10599 -0.03260 -0.00954 0.00500 AFIX 23 H34A 2 1.174952 0.944949 0.611293 11.00000 -1.20000 H34B 2 1.140958 0.900113 0.574831 11.00000 -1.20000 AFIX 0 PART 1 C50 1 -0.136338 0.303877 0.559293 21.00000 0.10678 0.09860 = 0.07778 0.00514 0.00872 0.00616 AFIX 43 H50 2 -0.134057 0.265351 0.555363 21.00000 -1.20000 AFIX 0 PART 0 C44 1 0.110299 0.545361 0.563824 11.00000 0.09599 0.13928 = 0.10744 -0.03686 0.03818 -0.00446 AFIX 43 H44 2 0.050799 0.539139 0.577202 11.00000 -1.20000 AFIX 0 C29 1 0.940033 0.917553 0.820401 11.00000 0.20155 0.10128 = 0.06525 0.02578 -0.03255 -0.02524 AFIX 23 H29A 2 0.897353 0.889697 0.807498 11.00000 -1.20000 H29B 2 0.922080 0.924371 0.852688 11.00000 -1.20000 AFIX 0 C33 1 1.154394 0.870057 0.639296 11.00000 0.08359 0.08361 = 0.14829 -0.03576 -0.01979 0.00931 AFIX 23 H33A 2 1.110377 0.839247 0.635234 11.00000 -1.20000 H33B 2 1.218353 0.856371 0.633587 11.00000 -1.20000 AFIX 0 PART 1 C53 1 -0.129912 0.413263 0.573619 21.00000 0.08698 0.07041 = 0.05639 0.00341 -0.00701 -0.02007 PART 0 C45 1 0.157690 0.502399 0.543009 11.00000 0.11918 0.11199 = 0.08494 -0.01771 0.03064 -0.02403 AFIX 43 H45 2 0.131182 0.466878 0.541133 11.00000 -1.20000 AFIX 0 C32 1 1.165623 0.848945 0.718186 11.00000 0.10513 0.07153 = 0.19440 0.01830 -0.04842 0.01339 AFIX 23 H32A 2 1.230014 0.835001 0.714421 11.00000 -1.20000 H32B 2 1.121917 0.818103 0.713533 11.00000 -1.20000 AFIX 0 C30 1 1.037520 0.898089 0.818026 11.00000 0.22144 0.09892 = 0.08123 0.01359 -0.07106 0.01141 AFIX 23 H30A 2 1.080465 0.926903 0.829107 11.00000 -1.20000 H30B 2 1.045518 0.865358 0.837605 11.00000 -1.20000 AFIX 0 PART 1 C51 1 -0.200496 0.326298 0.588561 21.00000 0.07764 0.08299 = 0.06482 0.01171 -0.00099 -0.01060 AFIX 43 H51 2 -0.246195 0.303862 0.602796 21.00000 -1.20000 AFIX 0 PART 0 C31 1 1.153761 0.871486 0.765108 11.00000 0.14317 0.09489 = 0.16098 0.02671 -0.08439 -0.00039 AFIX 23 H31A 2 1.172981 0.844107 0.788259 11.00000 -1.20000 H31B 2 1.192782 0.904550 0.769025 11.00000 -1.20000 AFIX 0 PART 1 C52 1 -0.198234 0.382587 0.597356 21.00000 0.07523 0.09696 = 0.05765 0.00593 0.01340 -0.00349 AFIX 43 H52 2 -0.240440 0.399302 0.618203 21.00000 -1.20000 AFIX 0 C58 1 -0.074766 0.389133 0.544104 21.00000 0.06523 0.09401 = 0.06856 -0.00304 0.01556 -0.01903 C57 1 -0.077573 0.335364 0.536468 21.00000 0.09390 0.11194 = 0.07894 -0.00377 0.03151 0.00351 AFIX 43 H57 2 -0.036916 0.319578 0.514404 21.00000 -1.20000 AFIX 0 F1 4 -0.134099 0.468202 0.582144 21.00000 0.18378 0.08351 = 0.08389 -0.00461 0.01939 -0.00134 F4 4 -0.014714 0.424388 0.524850 21.00000 0.13858 0.15734 = 0.16262 0.00418 0.05741 -0.03359 PART 2 F2 4 -0.050038 0.459818 0.573544 -21.00000 0.12579 0.07674 = 0.15140 -0.02825 -0.04201 -0.00651 C47 1 -0.082069 0.410834 0.569137 -21.00000 0.06143 0.08184 = 0.08079 -0.01123 -0.00900 -0.00237 C48 1 -0.029448 0.365613 0.561141 -21.00000 0.05582 0.08912 = 0.05536 0.00510 0.01120 -0.00287 C49 1 -0.066482 0.314582 0.559374 -21.00000 0.06287 0.08448 = 0.08913 -0.00498 0.00075 0.00348 AFIX 43 H49 2 -0.026927 0.283846 0.555076 -21.00000 -1.20000 AFIX 0 C56 1 -0.161623 0.307311 0.563818 -21.00000 0.05060 0.07747 = 0.07301 0.01003 -0.01253 -0.00995 AFIX 43 H56 2 -0.189560 0.272542 0.559134 -21.00000 -1.20000 AFIX 0 C55 1 -0.214850 0.352536 0.575352 -21.00000 0.06578 0.10619 = 0.07452 -0.00433 -0.00435 0.00026 AFIX 43 H55 2 -0.279291 0.348253 0.582086 -21.00000 -1.20000 AFIX 0 C54 1 -0.175013 0.403433 0.577099 -21.00000 0.06014 0.09427 = 0.07534 -0.02826 -0.00799 0.01219 AFIX 43 H54 2 -0.212930 0.434205 0.583999 -21.00000 -1.20000 AFIX 0 F9 4 0.063064 0.375992 0.557110 -21.00000 0.06796 0.12635 = 0.12278 -0.03255 0.03543 -0.01185 C1B 1 0.867452 0.833265 0.671071 31.00000 0.04346 0.06992 = 0.05245 -0.01056 0.00950 -0.00614 O1B 7 0.853588 0.882105 0.676684 31.00000 0.07808 0.07004 = 0.11673 -0.01489 0.00688 -0.00255 HKLF 4 REM kdp1_a.res in Pbca REM wR2 = 0.2228, GooF = S = 0.978, Restrained GooF = 0.974 for all data REM R1 = 0.0801 for 5827 Fo > 4sig(Fo) and 0.1028 for all 8987 data REM 696 parameters refined using 147 restraints END WGHT 0.1499 0.0000 REM Highest difference peak 0.631, deepest hole -0.297, 1-sigma level 0.087 Q1 1 0.9830 1.0049 0.6997 11.00000 0.05 0.63 Q2 1 0.9841 0.8965 0.7003 11.00000 0.05 0.52 Q3 1 0.9021 0.7650 0.6607 11.00000 0.05 0.52 Q4 1 -0.2337 0.4165 0.6230 11.00000 0.05 0.50 Q5 1 0.1599 0.4456 0.5463 11.00000 0.05 0.48 Q6 1 0.9114 0.6578 0.6601 11.00000 0.05 0.42 Q7 1 1.1595 0.9736 0.7708 11.00000 0.05 0.33 Q8 1 0.9058 0.6216 0.7550 11.00000 0.05 0.32 Q9 1 0.3419 0.5208 0.5074 11.00000 0.05 0.31 Q10 1 -0.1565 0.3555 0.5652 11.00000 0.05 0.30 Q11 1 0.8545 0.8173 0.6811 11.00000 0.05 0.28 ; _shelx_res_checksum 28403 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K001 K 0.98404(7) 0.95042(4) 0.70274(3) 0.0685(3) Uani 1 1 d . . . . . Al1 Al 0.91072(7) 0.71294(4) 0.65650(3) 0.0494(2) Uani 1 1 d . . . . . O5 O 0.8392(2) 1.02051(11) 0.72373(9) 0.0650(6) Uani 1 1 d . . . . . O6 O 0.91202(19) 1.01399(11) 0.63253(8) 0.0646(6) Uani 1 1 d . . . . . N1 N 0.8788(2) 0.78614(14) 0.67002(11) 0.0632(8) Uani 1 1 d . . . . . O4 O 0.9340(3) 0.96690(13) 0.79454(10) 0.0866(10) Uani 1 1 d . . . . . F007 F 0.3647(2) 0.57093(14) 0.50784(12) 0.1057(10) Uani 1 1 d . . . . . O7 O 1.0387(2) 0.93114(13) 0.61247(11) 0.0793(8) Uani 1 1 d . . . . . F009 F 0.2920(3) 0.47169(13) 0.50599(12) 0.1202(12) Uani 1 1 d . . . . . O2 O 1.1478(2) 0.89057(13) 0.68491(15) 0.0968(11) Uani 1 1 d . . . . . C2 C 0.9168(2) 0.66790(16) 0.71498(11) 0.0544(8) Uani 1 1 d . . . . . C7 C 0.9151(2) 0.61120(16) 0.71090(11) 0.0536(8) Uani 1 1 d . . . . . C20 C 1.0329(2) 0.72607(14) 0.62258(11) 0.0507(7) Uani 1 1 d . . . . . C11 C 0.7956(2) 0.68541(13) 0.62216(10) 0.0488(7) Uani 1 1 d . . . . . C16 C 0.7952(2) 0.65970(14) 0.57853(11) 0.0508(7) Uani 1 1 d . . . . . O1A O 0.8506(12) 0.8725(11) 0.699(2) 0.079(8) Uani 0.34(7) 1 d . U P A 1 C18 C 0.8844(3) 0.64379(16) 0.55412(11) 0.0586(8) Uani 1 1 d . . . . . H18A H 0.938008 0.658991 0.570634 0.088 Uiso 1 1 calc R U . . . H18B H 0.883375 0.658216 0.522767 0.088 Uiso 1 1 calc R U . . . H18C H 0.889544 0.603861 0.553158 0.088 Uiso 1 1 calc R U . . . C3 C 0.9136(2) 0.68895(17) 0.76079(11) 0.0604(9) Uani 1 1 d . . . . . C4 C 0.9011(2) 0.6526(2) 0.79803(11) 0.0675(11) Uani 1 1 d . . . . . H4 H 0.898144 0.667447 0.828112 0.081 Uiso 1 1 calc R U . . . O3 O 1.0583(3) 0.88476(14) 0.77074(13) 0.1044(12) Uani 1 1 d . . . . . C1A C 0.8649(18) 0.8294(12) 0.6876(12) 0.048(5) Uani 0.34(7) 1 d . . P A 1 C25 C 1.0328(2) 0.75591(15) 0.58083(11) 0.0543(7) Uani 1 1 d . . . . . C21 C 1.1215(2) 0.71226(14) 0.63982(11) 0.0529(7) Uani 1 1 d . . . . . C12 C 0.7063(2) 0.69278(14) 0.64210(12) 0.0531(7) Uani 1 1 d . . . . . C15 C 0.7121(3) 0.64561(15) 0.55633(12) 0.0565(8) Uani 1 1 d . . . . . H15 H 0.714974 0.629353 0.526775 0.068 Uiso 1 1 calc R U . . . C22 C 1.2039(2) 0.72598(15) 0.61608(12) 0.0565(8) Uani 1 1 d . . . . . H22 H 1.262521 0.716565 0.629030 0.068 Uiso 1 1 calc R U . . . C10 C 0.9274(3) 0.58373(16) 0.66463(12) 0.0594(8) Uani 1 1 d . . . . . H10A H 0.868673 0.585659 0.647465 0.089 Uiso 1 1 calc R U . . . H10B H 0.944740 0.545365 0.669180 0.089 Uiso 1 1 calc R U . . . H10C H 0.976608 0.602418 0.647368 0.089 Uiso 1 1 calc R U . . . C6 C 0.9023(3) 0.57647(18) 0.74910(12) 0.0639(9) Uani 1 1 d . . . . . H6 H 0.900215 0.538041 0.744552 0.077 Uiso 1 1 calc R U . . . C13 C 0.6252(3) 0.67783(15) 0.61952(13) 0.0594(8) Uani 1 1 d . . . . . H13 H 0.566992 0.683656 0.634304 0.071 Uiso 1 1 calc R U . . . C5 C 0.8929(3) 0.5972(2) 0.79298(12) 0.0649(10) Uani 1 1 d . . . . . C27 C 0.9435(3) 0.77901(18) 0.56034(14) 0.0671(10) Uani 1 1 d . . . . . H27A H 0.889482 0.761440 0.574725 0.101 Uiso 1 1 calc R U . . . H27B H 0.942550 0.771984 0.527247 0.101 Uiso 1 1 calc R U . . . H27C H 0.940977 0.818507 0.565827 0.101 Uiso 1 1 calc R U . . . C23 C 1.2012(3) 0.75277(17) 0.57445(13) 0.0610(9) Uani 1 1 d . . . . . C14 C 0.6259(3) 0.65467(16) 0.57614(13) 0.0592(8) Uani 1 1 d . . . . . C38 C 0.8306(3) 1.06284(15) 0.69044(13) 0.0627(9) Uani 1 1 d . . . . . H38A H 0.885699 1.087221 0.691708 0.075 Uiso 1 1 calc R U . . . H38B H 0.774147 1.084932 0.696621 0.075 Uiso 1 1 calc R U . . . C37 C 0.8237(3) 1.03660(17) 0.64394(13) 0.0638(9) Uani 1 1 d . . . . . H37A H 0.775756 1.007487 0.644367 0.077 Uiso 1 1 calc R U . . . H37B H 0.805425 1.064180 0.620778 0.077 Uiso 1 1 calc R U . . . C24 C 1.1159(3) 0.76755(16) 0.55735(12) 0.0608(8) Uani 1 1 d . . . . . H24 H 1.112866 0.786203 0.528811 0.073 Uiso 1 1 calc R U . . . C8 C 0.9207(3) 0.74897(19) 0.77048(14) 0.0755(11) Uani 1 1 d . . . . . H8A H 0.968695 0.765183 0.750773 0.113 Uiso 1 1 calc R U . . . H8B H 0.937568 0.754529 0.802724 0.113 Uiso 1 1 calc R U . . . H8C H 0.860494 0.766455 0.764289 0.113 Uiso 1 1 calc R U . . . C39 C 0.8452(3) 1.04197(18) 0.76900(13) 0.0703(10) Uani 1 1 d . . . . . H39A H 0.790257 1.065276 0.775483 0.084 Uiso 1 1 calc R U . . . H39B H 0.902077 1.064586 0.772172 0.084 Uiso 1 1 calc R U . . . C41 C 0.2813(3) 0.56347(19) 0.52642(14) 0.0740(11) Uani 1 1 d . . . . . C19 C 0.6948(3) 0.71646(17) 0.68988(13) 0.0632(9) Uani 1 1 d . . . . . H19A H 0.745867 0.703728 0.709501 0.095 Uiso 1 1 calc R U . . . H19B H 0.635048 0.704480 0.702802 0.095 Uiso 1 1 calc R U . . . H19C H 0.695983 0.756464 0.688205 0.095 Uiso 1 1 calc R U . . . C26 C 1.1342(3) 0.68208(19) 0.68468(13) 0.0671(10) Uani 1 1 d . . . . . H26A H 1.100627 0.701375 0.709084 0.101 Uiso 1 1 calc R U . . . H26B H 1.200733 0.680407 0.692298 0.101 Uiso 1 1 calc R U . . . H26C H 1.109452 0.644900 0.681726 0.101 Uiso 1 1 calc R U . . . C36 C 0.9133(3) 0.9872(2) 0.58934(14) 0.0765(11) Uani 1 1 d . . . . . H36A H 0.890115 1.012223 0.565242 0.092 Uiso 1 1 calc R U . . . H36B H 0.871896 0.954786 0.590242 0.092 Uiso 1 1 calc R U . . . C46 C 0.2443(4) 0.5135(2) 0.52531(15) 0.0846(13) Uani 1 1 d . . . . . C9 C 0.8754(3) 0.5609(2) 0.83424(14) 0.0898(15) Uani 1 1 d . . . . . H9A H 0.933591 0.556151 0.851424 0.135 Uiso 1 1 calc R U . . . H9B H 0.852831 0.525120 0.823876 0.135 Uiso 1 1 calc R U . . . H9C H 0.828377 0.577827 0.854083 0.135 Uiso 1 1 calc R U . . . C17 C 0.5358(3) 0.63839(19) 0.55260(14) 0.0724(11) Uani 1 1 d . . . . . H17A H 0.549861 0.622721 0.522446 0.109 Uiso 1 1 calc R U . . . H17B H 0.496122 0.670713 0.548780 0.109 Uiso 1 1 calc R U . . . H17C H 0.503045 0.611213 0.571335 0.109 Uiso 1 1 calc R U . . . C28 C 1.2910(3) 0.7666(2) 0.54900(16) 0.0789(12) Uani 1 1 d . . . . . H28A H 1.311140 0.803607 0.557292 0.118 Uiso 1 1 calc R U . . . H28B H 1.280007 0.764759 0.515866 0.118 Uiso 1 1 calc R U . . . H28C H 1.339749 0.740375 0.557481 0.118 Uiso 1 1 calc R U . . . C35 C 1.0097(3) 0.9700(2) 0.57854(15) 0.0821(13) Uani 1 1 d . . . . . H35A H 1.012014 0.953212 0.547664 0.098 Uiso 1 1 calc R U . . . H35B H 1.051811 1.002064 0.578824 0.098 Uiso 1 1 calc R U . . . C42 C 0.2350(4) 0.6058(2) 0.54690(17) 0.0843(13) Uani 1 1 d . . . . . H42 H 0.262445 0.641134 0.548356 0.101 Uiso 1 1 calc R U . . . C40 C 0.8484(4) 0.9954(2) 0.80185(15) 0.0862(14) Uani 1 1 d . . . . . H40A H 0.845184 1.009094 0.833769 0.103 Uiso 1 1 calc R U . . . H40B H 0.794778 0.970650 0.796592 0.103 Uiso 1 1 calc R U . . . C43 C 0.1489(4) 0.5967(3) 0.5652(2) 0.0988(17) Uani 1 1 d . . . . . H43 H 0.115488 0.626003 0.578908 0.119 Uiso 1 1 calc R U . . . C34 C 1.1322(4) 0.9137(2) 0.6065(2) 0.0912(15) Uani 1 1 d . . . . . H34A H 1.174952 0.944949 0.611293 0.109 Uiso 1 1 calc R U . . . H34B H 1.140958 0.900113 0.574831 0.109 Uiso 1 1 calc R U . . . C50 C -0.1363(15) 0.3039(8) 0.5593(11) 0.094(5) Uani 0.550(6) 1 d . . P B 1 H50 H -0.134057 0.265351 0.555363 0.113 Uiso 0.550(6) 1 calc R U P B 1 C44 C 0.1103(5) 0.5454(3) 0.5638(2) 0.114(2) Uani 1 1 d . . . . . H44 H 0.050799 0.539139 0.577202 0.137 Uiso 1 1 calc R U . . . C29 C 0.9400(6) 0.9176(3) 0.8204(2) 0.123(3) Uani 1 1 d . . . . . H29A H 0.897353 0.889697 0.807498 0.147 Uiso 1 1 calc R U . . . H29B H 0.922080 0.924371 0.852688 0.147 Uiso 1 1 calc R U . . . C33 C 1.1544(4) 0.8701(2) 0.6393(2) 0.1052(19) Uani 1 1 d . . . . . H33A H 1.110377 0.839247 0.635234 0.126 Uiso 1 1 calc R U . . . H33B H 1.218353 0.856371 0.633587 0.126 Uiso 1 1 calc R U . . . C53 C -0.1299(11) 0.4133(4) 0.5736(4) 0.071(3) Uani 0.550(6) 1 d . . P B 1 C45 C 0.1577(5) 0.5024(3) 0.5430(2) 0.1054(18) Uani 1 1 d . . . . . H45 H 0.131182 0.466878 0.541133 0.126 Uiso 1 1 calc R U . . . C32 C 1.1656(5) 0.8489(2) 0.7182(3) 0.124(3) Uani 1 1 d . . . . . H32A H 1.230014 0.835001 0.714421 0.148 Uiso 1 1 calc R U . . . H32B H 1.121917 0.818103 0.713533 0.148 Uiso 1 1 calc R U . . . C30 C 1.0375(7) 0.8981(3) 0.8180(2) 0.134(3) Uani 1 1 d . . . . . H30A H 1.080465 0.926903 0.829107 0.161 Uiso 1 1 calc R U . . . H30B H 1.045518 0.865358 0.837605 0.161 Uiso 1 1 calc R U . . . C51 C -0.2005(8) 0.3263(5) 0.5886(3) 0.075(3) Uani 0.550(6) 1 d . . P B 1 H51 H -0.246195 0.303862 0.602796 0.090 Uiso 0.550(6) 1 calc R U P B 1 C31 C 1.1538(6) 0.8715(3) 0.7651(3) 0.133(3) Uani 1 1 d . . . . . H31A H 1.172981 0.844107 0.788259 0.160 Uiso 1 1 calc R U . . . H31B H 1.192782 0.904550 0.769025 0.160 Uiso 1 1 calc R U . . . C52 C -0.1982(7) 0.3826(5) 0.5974(3) 0.077(3) Uani 0.550(6) 1 d . . P B 1 H52 H -0.240440 0.399302 0.618203 0.092 Uiso 0.550(6) 1 calc R U P B 1 C58 C -0.0748(6) 0.3891(5) 0.5441(3) 0.076(2) Uani 0.550(6) 1 d . . P B 1 C57 C -0.0776(8) 0.3354(5) 0.5365(4) 0.095(3) Uani 0.550(6) 1 d . . P B 1 H57 H -0.036916 0.319578 0.514404 0.114 Uiso 0.550(6) 1 calc R U P B 1 F1 F -0.1341(7) 0.4682(2) 0.5821(2) 0.117(3) Uani 0.550(6) 1 d . . P B 1 F4 F -0.0147(6) 0.4244(3) 0.5248(3) 0.153(4) Uani 0.550(6) 1 d . . P B 1 F2 F -0.0500(7) 0.4598(3) 0.5735(3) 0.118(3) Uani 0.450(6) 1 d . . P B 2 C47 C -0.0821(8) 0.4108(5) 0.5691(6) 0.075(4) Uani 0.450(6) 1 d D U P B 2 C48 C -0.0294(6) 0.3656(4) 0.5611(3) 0.067(2) Uani 0.450(6) 1 d D U P B 2 C49 C -0.0665(8) 0.3146(4) 0.5594(5) 0.079(3) Uani 0.450(6) 1 d D U P B 2 H49 H -0.026927 0.283846 0.555076 0.095 Uiso 0.450(6) 1 calc R U P B 2 C56 C -0.1616(10) 0.3073(7) 0.5638(11) 0.067(4) Uani 0.450(6) 1 d D U P B 2 H56 H -0.189560 0.272542 0.559134 0.080 Uiso 0.450(6) 1 calc R U P B 2 C55 C -0.2149(8) 0.3525(6) 0.5754(5) 0.082(3) Uani 0.450(6) 1 d D U P B 2 H55 H -0.279291 0.348253 0.582086 0.099 Uiso 0.450(6) 1 calc R U P B 2 C54 C -0.1750(8) 0.4034(6) 0.5771(6) 0.077(4) Uani 0.450(6) 1 d D U P B 2 H54 H -0.212930 0.434205 0.583999 0.092 Uiso 0.450(6) 1 calc R U P B 2 F9 F 0.0631(4) 0.3760(3) 0.5571(3) 0.106(3) Uani 0.450(6) 1 d D U P B 2 C1B C 0.8675(8) 0.8333(6) 0.6711(11) 0.055(3) Uani 0.66(7) 1 d . . P A 2 O1B O 0.8536(7) 0.8821(6) 0.6767(11) 0.088(4) Uani 0.66(7) 1 d . U P A 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 K001 0.0759(6) 0.0671(5) 0.0624(5) 0.0019(4) -0.0166(4) 0.0006(4) Al1 0.0417(5) 0.0677(6) 0.0387(4) -0.0011(4) 0.0004(3) 0.0014(4) O5 0.0793(18) 0.0666(15) 0.0491(13) -0.0012(11) -0.0043(11) -0.0057(12) O6 0.0662(16) 0.0782(16) 0.0493(13) -0.0033(11) -0.0096(11) 0.0036(12) N1 0.0543(18) 0.075(2) 0.0603(18) -0.0075(16) -0.0004(13) -0.0011(14) O4 0.121(3) 0.084(2) 0.0546(16) 0.0101(14) -0.0242(16) -0.0188(18) F007 0.0790(19) 0.133(2) 0.105(2) -0.0321(19) 0.0143(16) -0.0118(16) O7 0.074(2) 0.087(2) 0.0765(19) -0.0169(15) -0.0085(15) 0.0024(14) F009 0.153(3) 0.100(2) 0.107(2) -0.0319(18) 0.043(2) 0.0059(19) O2 0.090(2) 0.0725(19) 0.127(3) -0.0129(19) -0.038(2) 0.0102(16) C2 0.0377(17) 0.089(2) 0.0370(15) -0.0012(15) 0.0014(11) 0.0042(14) C7 0.0394(17) 0.084(2) 0.0376(15) 0.0069(14) -0.0003(12) 0.0080(14) C20 0.0475(18) 0.0645(19) 0.0401(15) -0.0001(13) 0.0013(12) 0.0012(13) C11 0.0493(18) 0.0590(18) 0.0382(15) 0.0019(12) -0.0010(12) 0.0010(13) C16 0.0504(19) 0.0629(19) 0.0392(15) 0.0049(13) 0.0005(12) -0.0012(14) O1A 0.062(6) 0.062(8) 0.112(18) -0.019(9) 0.010(8) -0.002(5) C18 0.057(2) 0.081(2) 0.0375(16) -0.0020(15) 0.0031(13) 0.0031(16) C3 0.0434(18) 0.098(3) 0.0399(16) -0.0054(16) -0.0005(13) 0.0052(16) C4 0.0376(18) 0.129(4) 0.0358(16) -0.0019(18) -0.0008(12) 0.0134(18) O3 0.131(3) 0.085(2) 0.098(3) 0.0141(19) -0.052(2) 0.003(2) C1A 0.047(7) 0.076(11) 0.022(10) -0.008(8) 0.003(7) 0.001(5) C25 0.0483(19) 0.070(2) 0.0445(16) 0.0048(14) -0.0032(13) -0.0007(14) C21 0.0480(18) 0.068(2) 0.0429(16) 0.0031(14) 0.0007(13) 0.0015(14) C12 0.0469(18) 0.0643(19) 0.0479(17) 0.0010(14) -0.0001(13) 0.0025(13) C15 0.061(2) 0.065(2) 0.0435(17) 0.0030(14) -0.0033(14) -0.0053(15) C22 0.0459(19) 0.074(2) 0.0498(18) 0.0061(15) 0.0008(13) 0.0019(14) C10 0.057(2) 0.072(2) 0.0486(18) 0.0027(15) 0.0015(14) 0.0059(16) C6 0.049(2) 0.093(3) 0.0494(19) 0.0137(17) -0.0005(14) 0.0107(17) C13 0.049(2) 0.073(2) 0.0561(19) 0.0025(16) 0.0033(14) 0.0004(15) C5 0.046(2) 0.105(3) 0.0442(18) 0.0138(18) -0.0024(13) 0.0119(18) C27 0.051(2) 0.090(3) 0.060(2) 0.0218(19) -0.0081(15) -0.0068(17) C23 0.051(2) 0.078(2) 0.0542(19) 0.0081(16) 0.0069(15) -0.0036(16) C14 0.051(2) 0.073(2) 0.0542(19) 0.0066(16) -0.0060(14) -0.0068(15) C38 0.061(2) 0.065(2) 0.063(2) 0.0040(16) -0.0016(16) -0.0022(15) C37 0.058(2) 0.078(2) 0.055(2) 0.0043(17) -0.0075(16) 0.0009(16) C24 0.057(2) 0.079(2) 0.0469(18) 0.0116(16) 0.0014(14) -0.0020(16) C8 0.072(3) 0.105(3) 0.049(2) -0.016(2) -0.0036(17) 0.005(2) C39 0.075(3) 0.083(3) 0.053(2) -0.0114(18) 0.0010(17) -0.0141(19) C41 0.067(3) 0.093(3) 0.062(2) -0.018(2) 0.0024(18) 0.001(2) C19 0.050(2) 0.082(2) 0.058(2) -0.0121(17) 0.0091(15) 0.0012(16) C26 0.049(2) 0.102(3) 0.0497(19) 0.0200(19) -0.0038(14) 0.0006(18) C36 0.075(3) 0.106(3) 0.049(2) -0.009(2) -0.0113(18) -0.002(2) C46 0.102(4) 0.088(3) 0.064(2) -0.020(2) 0.018(2) 0.004(2) C9 0.076(3) 0.144(4) 0.049(2) 0.029(2) 0.0037(19) 0.017(3) C17 0.060(2) 0.099(3) 0.059(2) 0.007(2) -0.0095(17) -0.015(2) C28 0.057(2) 0.109(3) 0.070(3) 0.025(2) 0.0137(18) -0.002(2) C35 0.075(3) 0.112(4) 0.060(2) -0.022(2) -0.0057(19) 0.000(2) C42 0.084(3) 0.090(3) 0.079(3) -0.027(2) -0.006(2) 0.009(2) C40 0.102(4) 0.106(4) 0.050(2) -0.003(2) -0.003(2) -0.020(3) C43 0.083(4) 0.116(4) 0.097(4) -0.039(3) 0.009(3) 0.010(3) C34 0.075(3) 0.093(3) 0.106(4) -0.033(3) -0.010(3) 0.005(2) C50 0.107(15) 0.099(8) 0.078(8) 0.005(6) 0.009(13) 0.006(8) C44 0.096(4) 0.139(5) 0.107(4) -0.037(4) 0.038(3) -0.004(3) C29 0.202(8) 0.101(4) 0.065(3) 0.026(3) -0.033(4) -0.025(4) C33 0.084(4) 0.084(3) 0.148(6) -0.036(3) -0.020(3) 0.009(3) C53 0.087(11) 0.070(5) 0.056(5) 0.003(4) -0.007(9) -0.020(6) C45 0.119(5) 0.112(4) 0.085(3) -0.018(3) 0.031(3) -0.024(3) C32 0.105(5) 0.072(3) 0.194(8) 0.018(4) -0.048(5) 0.013(3) C30 0.221(9) 0.099(4) 0.081(4) 0.014(3) -0.071(5) 0.011(5) C51 0.078(6) 0.083(7) 0.065(6) 0.012(5) -0.001(5) -0.011(5) C31 0.143(6) 0.095(4) 0.161(7) 0.027(4) -0.084(5) 0.000(4) C52 0.075(6) 0.097(7) 0.058(5) 0.006(5) 0.013(4) -0.003(5) C58 0.065(5) 0.094(7) 0.069(5) -0.003(5) 0.016(4) -0.019(4) C57 0.094(8) 0.112(9) 0.079(7) -0.004(6) 0.032(6) 0.004(6) F1 0.184(9) 0.084(4) 0.084(4) -0.005(3) 0.019(4) -0.001(4) F4 0.139(7) 0.157(7) 0.163(7) 0.004(6) 0.057(5) -0.034(5) F2 0.126(7) 0.077(4) 0.151(8) -0.028(4) -0.042(6) -0.007(4) C47 0.061(7) 0.082(6) 0.081(8) -0.011(6) -0.009(7) -0.002(5) C48 0.056(4) 0.089(5) 0.055(5) 0.005(4) 0.011(4) -0.003(4) C49 0.063(6) 0.084(6) 0.089(8) -0.005(6) 0.001(6) 0.003(4) C56 0.051(6) 0.077(7) 0.073(13) 0.010(7) -0.013(7) -0.010(5) C55 0.066(6) 0.106(8) 0.075(8) -0.004(8) -0.004(5) 0.000(5) C54 0.060(7) 0.094(8) 0.075(9) -0.028(8) -0.008(7) 0.012(5) F9 0.068(4) 0.126(6) 0.123(6) -0.033(4) 0.035(4) -0.012(3) C1B 0.043(3) 0.070(6) 0.052(10) -0.011(6) 0.009(5) -0.006(3) O1B 0.078(4) 0.070(5) 0.117(11) -0.015(5) 0.007(5) -0.003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 K001 O6 62.29(8) . . ? O5 K001 O4 60.42(10) . . ? O5 K001 O7 121.74(9) . . ? O5 K001 O2 172.25(10) . . ? O5 K001 O3 119.43(12) . . ? O5 K001 C38 22.00(8) . . ? O5 K001 C9 91.22(11) . 3_756 ? O5 K001 C1B 102.2(2) . . ? O6 K001 O4 122.02(10) . . ? O6 K001 O7 60.13(9) . . ? O6 K001 O2 117.79(11) . . ? O6 K001 C38 42.05(8) . . ? O6 K001 C9 63.79(10) . 3_756 ? O6 K001 C1B 95.1(5) . . ? O4 K001 O2 117.70(12) . . ? O4 K001 C38 79.98(10) . . ? O4 K001 C9 109.09(10) . 3_756 ? O4 K001 C1B 104.6(5) . . ? O7 K001 O4 177.84(11) . . ? O7 K001 O2 60.19(11) . . ? O7 K001 C38 102.16(9) . . ? O7 K001 C9 71.42(10) . 3_756 ? O7 K001 C1B 75.1(5) . . ? O2 K001 C38 154.62(11) . . ? O2 K001 C9 82.31(12) . 3_756 ? O2 K001 C1B 85.5(2) . . ? O1A K001 O5 85.1(4) . . ? O1A K001 O6 95.8(11) . . ? O1A K001 O4 87.7(11) . . ? O1A K001 O7 92.3(11) . . ? O1A K001 O2 102.4(4) . . ? O1A K001 O3 83.9(11) . . ? O1A K001 C38 96.0(6) . . ? O1A K001 C9 158.2(13) . 3_756 ? O3 K001 O6 178.17(12) . . ? O3 K001 O4 59.78(12) . . ? O3 K001 O7 118.08(12) . . ? O3 K001 O2 60.60(14) . . ? O3 K001 C38 139.76(12) . . ? O3 K001 C9 116.28(13) . 3_756 ? O3 K001 C1B 84.0(5) . . ? C9 K001 C38 74.31(11) 3_756 . ? C1B K001 C38 108.5(3) . . ? C1B K001 C9 146.1(5) . 3_756 ? O1B K001 O5 85.6(2) . . ? O1B K001 O6 83.0(7) . . ? O1B K001 O4 100.7(7) . . ? O1B K001 O7 79.6(7) . . ? O1B K001 O2 102.1(2) . . ? O1B K001 O3 96.4(7) . . ? O1B K001 C38 91.3(3) . . ? O1B K001 C9 143.6(8) . 3_756 ? O1B K001 C1B 17.3(3) . . ? N1 Al1 C2 110.44(15) . . ? N1 Al1 C20 99.22(15) . . ? N1 Al1 C11 102.64(14) . . ? C2 Al1 C20 117.13(13) . . ? C2 Al1 C11 105.50(14) . . ? C20 Al1 C11 120.53(13) . . ? C38 O5 K001 111.4(2) . . ? C39 O5 K001 112.9(2) . . ? C39 O5 C38 111.7(3) . . ? C37 O6 K001 112.2(2) . . ? C36 O6 K001 113.0(2) . . ? C36 O6 C37 113.5(3) . . ? C1A N1 Al1 166.1(16) . . ? C1B N1 Al1 167.7(14) . . ? C40 O4 K001 115.7(2) . . ? C29 O4 K001 111.6(3) . . ? C29 O4 C40 112.7(5) . . ? C35 O7 K001 117.3(2) . . ? C34 O7 K001 115.6(3) . . ? C34 O7 C35 112.9(4) . . ? C33 O2 K001 114.3(3) . . ? C33 O2 C32 111.8(5) . . ? C32 O2 K001 113.2(4) . . ? C7 C2 Al1 117.9(2) . . ? C7 C2 C3 115.9(3) . . ? C3 C2 Al1 125.9(3) . . ? C2 C7 C10 121.0(3) . . ? C2 C7 C6 122.3(3) . . ? C6 C7 C10 116.7(3) . . ? C25 C20 Al1 119.8(2) . . ? C21 C20 Al1 124.4(2) . . ? C21 C20 C25 115.5(3) . . ? C16 C11 Al1 126.1(2) . . ? C12 C11 Al1 119.1(2) . . ? C12 C11 C16 114.8(3) . . ? C11 C16 C18 122.1(3) . . ? C15 C16 C11 121.8(3) . . ? C15 C16 C18 116.0(3) . . ? C1A O1A K001 123.0(16) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C3 C8 121.7(3) . . ? C4 C3 C2 119.6(4) . . ? C4 C3 C8 118.7(3) . . ? C3 C4 H4 118.3 . . ? C5 C4 C3 123.4(3) . . ? C5 C4 H4 118.3 . . ? C30 O3 K001 118.2(3) . . ? C31 O3 K001 115.0(4) . . ? C31 O3 C30 111.2(5) . . ? O1A C1A N1 171.4(19) . . ? C20 C25 C27 121.9(3) . . ? C24 C25 C20 121.5(3) . . ? C24 C25 C27 116.5(3) . . ? C20 C21 C22 121.6(3) . . ? C20 C21 C26 122.3(3) . . ? C22 C21 C26 116.1(3) . . ? C11 C12 C19 121.5(3) . . ? C13 C12 C11 122.0(3) . . ? C13 C12 C19 116.5(3) . . ? C16 C15 H15 119.0 . . ? C14 C15 C16 121.9(3) . . ? C14 C15 H15 119.0 . . ? C21 C22 H22 119.3 . . ? C23 C22 C21 121.5(3) . . ? C23 C22 H22 119.3 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C6 H6 119.3 . . ? C5 C6 C7 121.4(4) . . ? C5 C6 H6 119.3 . . ? C12 C13 H13 118.8 . . ? C12 C13 C14 122.4(3) . . ? C14 C13 H13 118.8 . . ? C4 C5 C6 117.1(4) . . ? C4 C5 C9 120.6(4) . . ? C6 C5 C9 122.3(4) . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C23 C28 120.7(3) . . ? C24 C23 C22 118.0(3) . . ? C24 C23 C28 121.2(3) . . ? C15 C14 C13 116.9(3) . . ? C15 C14 C17 122.0(3) . . ? C13 C14 C17 121.0(4) . . ? K001 C38 H38A 88.2 . . ? K001 C38 H38B 156.0 . . ? O5 C38 K001 46.56(17) . . ? O5 C38 H38A 110.1 . . ? O5 C38 H38B 110.1 . . ? O5 C38 C37 108.0(3) . . ? H38A C38 H38B 108.4 . . ? C37 C38 K001 78.5(2) . . ? C37 C38 H38A 110.1 . . ? C37 C38 H38B 110.1 . . ? O6 C37 C38 108.6(3) . . ? O6 C37 H37A 110.0 . . ? O6 C37 H37B 110.0 . . ? C38 C37 H37A 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? C25 C24 H24 119.1 . . ? C23 C24 C25 121.8(3) . . ? C23 C24 H24 119.1 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C39 H39A 110.0 . . ? O5 C39 H39B 110.0 . . ? O5 C39 C40 108.4(3) . . ? H39A C39 H39B 108.4 . . ? C40 C39 H39A 110.0 . . ? C40 C39 H39B 110.0 . . ? F007 C41 C46 118.4(4) . . ? F007 C41 C42 120.8(4) . . ? C46 C41 C42 120.8(5) . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O6 C36 H36A 109.8 . . ? O6 C36 H36B 109.8 . . ? O6 C36 C35 109.4(3) . . ? H36A C36 H36B 108.2 . . ? C35 C36 H36A 109.8 . . ? C35 C36 H36B 109.8 . . ? F009 C46 C45 117.7(5) . . ? C41 C46 F009 120.1(5) . . ? C41 C46 C45 122.2(5) . . ? K001 C9 H9A 65.2 3_746 . ? K001 C9 H9B 54.0 3_746 . ? K001 C9 H9C 153.4 3_746 . ? C5 C9 K001 96.4(3) . 3_746 ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7 C35 C36 108.2(4) . . ? O7 C35 H35A 110.1 . . ? O7 C35 H35B 110.1 . . ? C36 C35 H35A 110.1 . . ? C36 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? C41 C42 H42 120.4 . . ? C43 C42 C41 119.1(5) . . ? C43 C42 H42 120.4 . . ? O4 C40 C39 107.7(4) . . ? O4 C40 H40A 110.2 . . ? O4 C40 H40B 110.2 . . ? C39 C40 H40A 110.2 . . ? C39 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? C42 C43 H43 119.9 . . ? C42 C43 C44 120.2(5) . . ? C44 C43 H43 119.9 . . ? O7 C34 H34A 109.6 . . ? O7 C34 H34B 109.6 . . ? O7 C34 C33 110.2(5) . . ? H34A C34 H34B 108.1 . . ? C33 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C51 C50 H50 119.7 . . ? C57 C50 H50 119.7 . . ? C57 C50 C51 120.6(16) . . ? C43 C44 H44 119.8 . . ? C43 C44 C45 120.5(6) . . ? C45 C44 H44 119.8 . . ? O4 C29 H29A 110.2 . . ? O4 C29 H29B 110.2 . . ? O4 C29 C30 107.8(6) . . ? H29A C29 H29B 108.5 . . ? C30 C29 H29A 110.2 . . ? C30 C29 H29B 110.2 . . ? O2 C33 C34 109.7(4) . . ? O2 C33 H33A 109.7 . . ? O2 C33 H33B 109.7 . . ? C34 C33 H33A 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C58 C53 C52 120.0(10) . . ? C58 C53 F1 126.1(11) . . ? F1 C53 C52 113.7(13) . . ? C46 C45 C44 117.2(6) . . ? C46 C45 H45 121.4 . . ? C44 C45 H45 121.4 . . ? O2 C32 H32A 109.7 . . ? O2 C32 H32B 109.7 . . ? O2 C32 C31 109.9(5) . . ? H32A C32 H32B 108.2 . . ? C31 C32 H32A 109.7 . . ? C31 C32 H32B 109.7 . . ? O3 C30 C29 108.2(5) . . ? O3 C30 H30A 110.1 . . ? O3 C30 H30B 110.1 . . ? C29 C30 H30A 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C50 C51 H51 120.3 . . ? C50 C51 C52 119.5(12) . . ? C52 C51 H51 120.3 . . ? O3 C31 C32 107.6(5) . . ? O3 C31 H31A 110.2 . . ? O3 C31 H31B 110.2 . . ? C32 C31 H31A 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? C53 C52 H52 121.7 . . ? C51 C52 C53 116.6(10) . . ? C51 C52 H52 121.7 . . ? C53 C58 C57 122.4(9) . . ? C53 C58 F4 111.9(11) . . ? C57 C58 F4 125.7(10) . . ? C50 C57 C58 120.7(12) . . ? C50 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? F2 C47 C48 125.2(11) . . ? F2 C47 C54 117.0(11) . . ? C48 C47 C54 117.6(10) . . ? C49 C48 C47 122.6(8) . . ? F9 C48 C47 113.9(8) . . ? F9 C48 C49 123.5(9) . . ? C48 C49 H49 120.0 . . ? C48 C49 C56 120.1(10) . . ? C56 C49 H49 120.0 . . ? C49 C56 H56 121.2 . . ? C49 C56 C55 117.6(11) . . ? C55 C56 H56 121.2 . . ? C56 C55 H55 119.8 . . ? C54 C55 C56 120.3(10) . . ? C54 C55 H55 119.8 . . ? C47 C54 C55 121.4(10) . . ? C47 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? N1 C1B K001 139.8(11) . . ? N1 C1B O1B 173.7(17) . . ? O1B C1B K001 39.6(6) . . ? C1B O1B K001 123.1(8) . . ? 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 K001 O5 2.761(3) . ? K001 O6 2.770(3) . ? K001 O4 2.800(3) . ? K001 O7 2.786(3) . ? K001 O2 2.815(4) . ? K001 O1A 2.70(2) . ? K001 O3 2.765(3) . ? K001 C38 3.539(4) . ? K001 C9 3.539(6) 3_756 ? K001 C1B 3.444(14) . ? K001 O1B 2.620(10) . ? Al1 N1 1.890(4) . ? Al1 C2 2.032(4) . ? Al1 C20 2.036(3) . ? Al1 C11 2.044(3) . ? O5 C38 1.425(4) . ? O5 C39 1.423(4) . ? O6 C37 1.421(5) . ? O6 C36 1.420(5) . ? N1 C1A 1.19(3) . ? N1 C1B 1.165(14) . ? O4 C40 1.429(6) . ? O4 C29 1.426(6) . ? F007 C41 1.325(5) . ? O7 C35 1.433(6) . ? O7 C34 1.416(6) . ? F009 C46 1.353(5) . ? O2 C33 1.425(7) . ? O2 C32 1.430(7) . ? C2 C7 1.392(5) . ? C2 C3 1.432(5) . ? C7 C10 1.517(5) . ? C7 C6 1.413(5) . ? C20 C25 1.419(5) . ? C20 C21 1.407(5) . ? C11 C16 1.419(4) . ? C11 C12 1.418(4) . ? C16 C18 1.514(5) . ? C16 C15 1.399(5) . ? O1A C1A 1.12(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C3 C4 1.415(6) . ? C3 C8 1.499(6) . ? C4 H4 0.9500 . ? C4 C5 1.368(6) . ? O3 C30 1.448(8) . ? O3 C31 1.415(9) . ? C25 C27 1.521(5) . ? C25 C24 1.403(5) . ? C21 C22 1.409(5) . ? C21 C26 1.513(4) . ? C12 C13 1.384(5) . ? C12 C19 1.518(5) . ? C15 H15 0.9500 . ? C15 C14 1.382(5) . ? C22 H22 0.9500 . ? C22 C23 1.380(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C6 H6 0.9500 . ? C6 C5 1.383(6) . ? C13 H13 0.9500 . ? C13 C14 1.386(5) . ? C5 C9 1.518(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C23 C24 1.369(5) . ? C23 C28 1.524(5) . ? C14 C17 1.516(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C37 1.503(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C24 H24 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.489(6) . ? C41 C46 1.334(7) . ? C41 C42 1.368(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 C35 1.478(6) . ? C46 C45 1.371(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C42 H42 0.9500 . ? C42 C43 1.362(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C43 H43 0.9500 . ? C43 C44 1.374(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C33 1.468(8) . ? C50 H50 0.9500 . ? C50 C51 1.37(2) . ? C50 C57 1.32(2) . ? C44 H44 0.9500 . ? C44 C45 1.391(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.478(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C53 C52 1.415(13) . ? C53 C58 1.309(16) . ? C53 F1 1.368(12) . ? C45 H45 0.9500 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C31 1.485(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C51 H51 0.9500 . ? C51 C52 1.401(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C52 H52 0.9500 . ? C58 C57 1.335(15) . ? C58 F4 1.342(10) . ? C57 H57 0.9500 . ? F2 C47 1.290(14) . ? C47 C48 1.359(10) . ? C47 C54 1.364(10) . ? C48 C49 1.358(10) . ? C48 F9 1.355(9) . ? C49 H49 0.9500 . ? C49 C56 1.381(11) . ? C56 H56 0.9500 . ? C56 C55 1.385(11) . ? C55 H55 0.9500 . ? C55 C54 1.371(10) . ? C54 H54 0.9500 . ? C1B O1B 1.222(17) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag K001 O5 C38 C37 53.3(3) . . . . ? K001 O5 C39 C40 -56.8(4) . . . . ? K001 O6 C37 C38 49.4(3) . . . . ? K001 O6 C36 C35 -56.4(4) . . . . ? K001 O4 C40 C39 -42.9(4) . . . . ? K001 O4 C29 C30 59.8(5) . . . . ? K001 O7 C35 C36 -39.1(4) . . . . ? K001 O7 C34 C33 46.7(5) . . . . ? K001 O2 C33 C34 47.7(5) . . . . ? K001 O2 C32 C31 -46.7(6) . . . . ? K001 O3 C30 C29 37.4(7) . . . . ? K001 O3 C31 C32 -52.3(6) . . . . ? K001 C38 C37 O6 -34.2(2) . . . . ? Al1 N1 C1B K001 -82(7) . . . . ? Al1 C2 C7 C10 11.7(4) . . . . ? Al1 C2 C7 C6 -168.5(3) . . . . ? Al1 C2 C3 C4 168.2(3) . . . . ? Al1 C2 C3 C8 -10.1(5) . . . . ? Al1 C20 C25 C27 0.3(5) . . . . ? Al1 C20 C25 C24 177.6(3) . . . . ? Al1 C20 C21 C22 -175.4(3) . . . . ? Al1 C20 C21 C26 4.5(5) . . . . ? Al1 C11 C16 C18 7.0(5) . . . . ? Al1 C11 C16 C15 -175.5(3) . . . . ? Al1 C11 C12 C13 176.4(3) . . . . ? Al1 C11 C12 C19 -5.0(5) . . . . ? O5 C38 C37 O6 -70.6(4) . . . . ? O5 C39 C40 O4 66.3(4) . . . . ? O6 C36 C35 O7 63.1(5) . . . . ? O4 C29 C30 O3 -64.1(6) . . . . ? F007 C41 C46 F009 0.7(7) . . . . ? F007 C41 C46 C45 -178.8(5) . . . . ? F007 C41 C42 C43 179.3(5) . . . . ? O7 C34 C33 O2 -63.1(5) . . . . ? F009 C46 C45 C44 178.4(6) . . . . ? O2 C32 C31 O3 66.3(7) . . . . ? C2 Al1 N1 C1A 20(6) . . . . ? C2 Al1 N1 C1B 154(5) . . . . ? C2 C7 C6 C5 -1.5(5) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C7 C2 C3 C4 -5.4(5) . . . . ? C7 C2 C3 C8 176.3(3) . . . . ? C7 C6 C5 C4 -3.2(5) . . . . ? C7 C6 C5 C9 177.6(4) . . . . ? C20 Al1 N1 C1A -104(6) . . . . ? C20 Al1 N1 C1B 31(5) . . . . ? C20 C25 C24 C23 -2.8(6) . . . . ? C20 C21 C22 C23 -1.1(6) . . . . ? C11 Al1 N1 C1A 132(6) . . . . ? C11 Al1 N1 C1B -94(5) . . . . ? C11 C16 C15 C14 -1.7(5) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C16 C11 C12 C13 -2.5(5) . . . . ? C16 C11 C12 C19 176.2(3) . . . . ? C16 C15 C14 C13 -0.8(5) . . . . ? C16 C15 C14 C17 -178.7(4) . . . . ? C18 C16 C15 C14 175.9(3) . . . . ? C3 C2 C7 C10 -174.1(3) . . . . ? C3 C2 C7 C6 5.6(5) . . . . ? C3 C4 C5 C6 3.3(5) . . . . ? C3 C4 C5 C9 -177.4(4) . . . . ? C4 C5 C9 K001 -143.0(3) . . . 3_746 ? C25 C20 C21 C22 -1.9(5) . . . . ? C25 C20 C21 C26 178.0(3) . . . . ? C21 C20 C25 C27 -173.5(3) . . . . ? C21 C20 C25 C24 3.8(5) . . . . ? C21 C22 C23 C24 2.2(6) . . . . ? C21 C22 C23 C28 -179.2(4) . . . . ? C12 C11 C16 C18 -174.2(3) . . . . ? C12 C11 C16 C15 3.2(5) . . . . ? C12 C13 C14 C15 1.6(6) . . . . ? C12 C13 C14 C17 179.5(4) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C10 C7 C6 C5 178.3(3) . . . . ? C6 C5 C9 K001 36.2(4) . . . 3_746 ? C27 C25 C24 C23 174.6(4) . . . . ? C38 O5 C39 C40 176.7(4) . . . . ? C37 O6 C36 C35 174.4(4) . . . . ? C8 C3 C4 C5 179.4(3) . . . . ? C39 O5 C38 K001 127.3(3) . . . . ? C39 O5 C38 C37 -179.4(3) . . . . ? C41 C46 C45 C44 -2.1(9) . . . . ? C41 C42 C43 C44 1.3(9) . . . . ? C19 C12 C13 C14 -178.6(4) . . . . ? C26 C21 C22 C23 179.0(4) . . . . ? C36 O6 C37 C38 179.0(3) . . . . ? C46 C41 C42 C43 -1.8(8) . . . . ? C28 C23 C24 C25 -178.9(4) . . . . ? C35 O7 C34 C33 -174.3(4) . . . . ? C42 C41 C46 F009 -178.3(5) . . . . ? C42 C41 C46 C45 2.2(8) . . . . ? C42 C43 C44 C45 -1.3(10) . . . . ? C40 O4 C29 C30 -168.1(4) . . . . ? C43 C44 C45 C46 1.6(10) . . . . ? C34 O7 C35 C36 -177.4(4) . . . . ? C50 C51 C52 C53 2(2) . . . . ? C29 O4 C40 C39 -173.0(4) . . . . ? C33 O2 C32 C31 -177.4(5) . . . . ? C53 C58 C57 C50 -1(2) . . . . ? C32 O2 C33 C34 177.9(5) . . . . ? C30 O3 C31 C32 170.0(5) . . . . ? C51 C50 C57 C58 5(3) . . . . ? C31 O3 C30 C29 173.6(5) . . . . ? C52 C53 C58 C57 -2.7(19) . . . . ? C52 C53 C58 F4 179.9(10) . . . . ? C58 C53 C52 C51 2.1(15) . . . . ? C57 C50 C51 C52 -6(3) . . . . ? F1 C53 C52 C51 177.2(10) . . . . ? F1 C53 C58 C57 -177.2(12) . . . . ? F1 C53 C58 F4 5.3(18) . . . . ? F4 C58 C57 C50 176.1(19) . . . . ? F2 C47 C48 C49 176.2(15) . . . . ? F2 C47 C48 F9 -1.2(18) . . . . ? F2 C47 C54 C55 -177.0(13) . . . . ? C47 C48 C49 C56 2.8(19) . . . . ? C48 C47 C54 C55 -3(3) . . . . ? C48 C49 C56 C55 -7(3) . . . . ? C49 C56 C55 C54 7(3) . . . . ? C56 C55 C54 C47 -2(3) . . . . ? C54 C47 C48 C49 2.2(18) . . . . ? C54 C47 C48 F9 -175.1(15) . . . . ? F9 C48 C49 C56 179.9(18) . . . . ?