# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sheng-Hsien Chiu' _publ_contact_author_email shchiu@ntu.edu.tw loop_ _publ_author_name 'Sheng-Hsien Chiu' 'Chien-Chen Lai' 'Shie-Ming Peng' # Attachment '- CCDC-768489.cif' data_ic13566 _database_code_depnum_ccdc_archive 'CCDC 768489' #TrackingRef '- CCDC-768489.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H80 K2 N2 O18 P2 F12' _chemical_formula_sum 'C74 H84 Cl6 F12 K2 N2 O19 P2' _chemical_formula_weight 1886.27 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' 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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' _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 9.3095(10) _cell_length_b 13.4294(10) _cell_length_c 17.4556(15) _cell_angle_alpha 92.960(7) _cell_angle_beta 101.960(8) _cell_angle_gamma 102.545(8) _cell_volume 2073.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2457 _cell_measurement_theta_min 4.0532 _cell_measurement_theta_max 70.4097 _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 3.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60455 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17681 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 67.98 _reflns_number_total 7490 _reflns_number_gt 3916 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 7490 _refine_ls_number_parameters 524 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.2069 _refine_ls_R_factor_gt 0.1417 _refine_ls_wR_factor_ref 0.3727 _refine_ls_wR_factor_gt 0.3387 _refine_ls_goodness_of_fit_ref 1.953 _refine_ls_restrained_S_all 2.011 _refine_ls_shift/su_max 0.095 _refine_ls_shift/su_mean 0.007 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 K1 K 0.4203(2) 0.63300(13) 0.78516(10) 0.0654(6) Uani 1 1 d U . . O1 O 0.6079(10) 0.8012(5) 0.7364(3) 0.098(2) Uani 1 1 d . . . O2 O 0.6069(15) 0.7925(8) 0.8907(6) 0.149(4) Uani 1 1 d U . . O3 O 0.5935(12) 0.5802(6) 0.9286(4) 0.109(3) Uani 1 1 d . . . O4 O 0.5186(9) 0.4514(5) 0.7900(3) 0.0820(19) Uani 1 1 d . . . O5 O 0.3128(12) 0.7670(7) 0.6707(5) 0.111(3) Uani 1 1 d . . . O6 O 0.1672(14) 0.7110(8) 0.7846(7) 0.141(3) Uani 1 1 d U . . O7 O 0.1920(10) 0.5343(5) 0.8534(4) 0.090(2) Uani 1 1 d . . . O8 O 0.2215(8) 0.4263(4) 0.7196(4) 0.0737(17) Uani 1 1 d . . . O9 O 0.4277(13) 0.5725(6) 0.6278(5) 0.121(2) Uani 1 1 d U . . N1 N 0.1069(19) 0.4836(16) 0.3969(9) 0.163(6) Uani 1 1 d . . . H1A H 0.0131 0.4900 0.3829 0.195 Uiso 1 1 calc R . . C1 C 0.6874(11) 0.6330(6) 0.3090(5) 0.061(2) Uani 1 1 d . . . C2 C 0.7546(10) 0.7047(5) 0.3739(5) 0.0576(19) Uani 1 1 d . . . H2A H 0.8590 0.7144 0.3973 0.069 Uiso 1 1 calc R . . C3 C 0.6681(10) 0.7616(5) 0.4041(4) 0.0550(19) Uani 1 1 d . . . C4 C 0.7285(12) 0.8472(6) 0.4729(5) 0.066(2) Uani 1 1 d . . . C5 C 0.6242(12) 0.8251(5) 0.5293(5) 0.060(2) Uani 1 1 d . . . C6 C 0.6704(12) 0.8255(6) 0.6097(5) 0.069(2) Uani 1 1 d . . . H6A H 0.7753 0.8386 0.6330 0.083 Uiso 1 1 calc R . . C7 C 0.5695(14) 0.8077(6) 0.6564(5) 0.072(3) Uani 1 1 d . . . C8 C 0.4178(14) 0.7905(6) 0.6229(5) 0.073(3) Uani 1 1 d . . . C9 C 0.3661(12) 0.7908(6) 0.5424(5) 0.066(2) Uani 1 1 d . . . H9A H 0.2611 0.7789 0.5199 0.079 Uiso 1 1 calc R . . C10 C 0.4722(12) 0.8090(5) 0.4947(5) 0.063(2) Uani 1 1 d . . . C11 C 0.4315(12) 0.8170(6) 0.4061(5) 0.065(2) Uani 1 1 d . . . C12 C 0.5179(11) 0.7474(6) 0.3708(4) 0.060(2) Uani 1 1 d . . . C13 C 0.4508(11) 0.6752(6) 0.3054(5) 0.063(2) Uani 1 1 d . . . H13A H 0.3459 0.6641 0.2830 0.076 Uiso 1 1 calc R . . C14 C 0.5379(11) 0.6200(5) 0.2733(4) 0.059(2) Uani 1 1 d . . . C15 C 0.6922(13) 0.9433(6) 0.4346(5) 0.073(3) Uani 1 1 d . . . H15A H 0.7240 1.0028 0.4752 0.087 Uiso 1 1 calc R . . H15B H 0.7507 0.9588 0.3936 0.087 Uiso 1 1 calc R . . C16 C 0.5251(13) 0.9280(6) 0.3978(5) 0.075(3) Uani 1 1 d . . . H16A H 0.5122 0.9388 0.3414 0.090 Uiso 1 1 calc R . . H16B H 0.4848 0.9799 0.4236 0.090 Uiso 1 1 calc R . . C17 C 0.8903(13) 0.8627(7) 0.5084(6) 0.077(3) Uani 1 1 d . . . H17A H 0.9092 0.8005 0.5316 0.116 Uiso 1 1 calc R . . H17B H 0.9214 0.9206 0.5494 0.116 Uiso 1 1 calc R . . H17C H 0.9483 0.8772 0.4677 0.116 Uiso 1 1 calc R . . C18 C 0.2689(13) 0.7998(8) 0.3701(5) 0.077(3) Uani 1 1 d . . . H18A H 0.2174 0.7300 0.3766 0.116 Uiso 1 1 calc R . . H18B H 0.2552 0.8089 0.3140 0.116 Uiso 1 1 calc R . . H18C H 0.2261 0.8492 0.3960 0.116 Uiso 1 1 calc R . . C19 C 0.696(3) 0.8729(10) 0.7833(7) 0.170(7) Uani 1 1 d U . . H19A H 0.6532 0.9342 0.7775 0.204 Uiso 1 1 calc R . . H19B H 0.7926 0.8887 0.7663 0.204 Uiso 1 1 calc R . . C20 C 0.730(3) 0.8592(10) 0.8664(7) 0.167(6) Uani 1 1 d U . . H20A H 0.7543 0.9270 0.8973 0.201 Uiso 1 1 calc R . . H20B H 0.8201 0.8302 0.8784 0.201 Uiso 1 1 calc RD . . C21 C 0.691(3) 0.7568(11) 0.9644(7) 0.184(7) Uani 1 1 d DU . . H21A H 0.7937 0.8026 0.9775 0.221 Uiso 1 1 calc RD . . H21B H 0.6415 0.7725 1.0070 0.221 Uiso 1 1 calc R . . C22 C 0.712(2) 0.6565(13) 0.9719(7) 0.178(10) Uani 1 1 d D . . H22A H 0.8054 0.6515 0.9551 0.214 Uiso 1 1 calc R . . H22B H 0.7259 0.6443 1.0281 0.214 Uiso 1 1 calc R . . C23 C 0.632(3) 0.4918(14) 0.9248(7) 0.157(9) Uani 1 1 d . . . H23A H 0.5864 0.4502 0.9626 0.189 Uiso 1 1 calc R . . H23B H 0.7431 0.5061 0.9447 0.189 Uiso 1 1 calc R . . C24 C 0.598(2) 0.4306(10) 0.8547(9) 0.157(9) Uani 1 1 d . . . H24A H 0.6959 0.4240 0.8433 0.188 Uiso 1 1 calc R . . H24B H 0.5467 0.3615 0.8648 0.188 Uiso 1 1 calc R . . C25 C 0.232(2) 0.8158(13) 0.6859(12) 0.147(4) Uani 1 1 d U . . H25A H 0.1706 0.8280 0.6354 0.176 Uiso 1 1 calc R . . H25B H 0.2958 0.8833 0.7106 0.176 Uiso 1 1 calc R . . C26 C 0.126(2) 0.7794(12) 0.7374(10) 0.134(4) Uani 1 1 d U . . H26A H 0.1173 0.8393 0.7701 0.161 Uiso 1 1 calc R . . H26B H 0.0249 0.7486 0.7037 0.161 Uiso 1 1 calc R . . C27 C 0.0816(18) 0.6800(11) 0.8384(7) 0.110(4) Uani 1 1 d . . . H27A H 0.0784 0.7412 0.8716 0.132 Uiso 1 1 calc R . . H27B H -0.0230 0.6479 0.8097 0.132 Uiso 1 1 calc R . . C28 C 0.135(2) 0.6116(10) 0.8867(10) 0.139(4) Uani 1 1 d U . . H28A H 0.0512 0.5772 0.9103 0.167 Uiso 1 1 calc R . . H28B H 0.2154 0.6516 0.9304 0.167 Uiso 1 1 calc R . . C29 C 0.0775(12) 0.4519(7) 0.8109(7) 0.081(3) Uani 1 1 d . . . H29A H 0.0077 0.4782 0.7705 0.098 Uiso 1 1 calc R . . H29B H 0.0189 0.4169 0.8471 0.098 Uiso 1 1 calc R . . C30 C 0.1424(12) 0.3801(7) 0.7736(7) 0.083(3) Uani 1 1 d . . . H30A H 0.2120 0.3539 0.8142 0.100 Uiso 1 1 calc R . . H30B H 0.0612 0.3212 0.7460 0.100 Uiso 1 1 calc R . . C31 C 0.175(3) 0.5168(13) 0.4749(11) 0.154(5) Uani 1 1 d U . . H31A H 0.1233 0.5406 0.5112 0.185 Uiso 1 1 calc R . . C32 C 0.3498(14) 0.5112(8) 0.4981(8) 0.093(3) Uani 1 1 d . . . C33 C 0.4614(14) 0.5397(7) 0.5700(6) 0.078(3) Uani 1 1 d . . . C34 C 0.6118(14) 0.5301(7) 0.5700(6) 0.083(3) Uani 1 1 d . . . C35 C 0.711(2) 0.5626(12) 0.6453(11) 0.149(7) Uani 1 1 d D . . C36 C 0.845(2) 0.5547(17) 0.6588(12) 0.149(6) Uani 1 1 d D . . P1 P 0.1644(5) 0.7976(3) 0.09326(19) 0.1112(12) Uani 1 1 d . . . F1 F -0.0028(17) 0.7846(11) 0.1130(8) 0.196(5) Uani 1 1 d . . . F2 F 0.3175(15) 0.7940(9) 0.0736(9) 0.192(5) Uani 1 1 d . . . F3 F 0.2087(16) 0.7462(9) 0.1720(5) 0.173(4) Uani 1 1 d . . . F4 F 0.1074(13) 0.6906(8) 0.0515(5) 0.160(4) Uani 1 1 d . . . F5 F 0.116(2) 0.8458(13) 0.0169(8) 0.224(7) Uani 1 1 d . . . F6 F 0.213(3) 0.9016(8) 0.1359(11) 0.279(11) Uani 1 1 d . . . Cl1 Cl 0.9643(5) 0.9573(3) 0.2795(2) 0.1261(12) Uani 1 1 d . . . Cl2 Cl 0.8718(6) 1.0043(3) 0.1180(2) 0.1363(14) Uani 1 1 d . . . Cl3 Cl 0.6650(6) 0.8742(4) 0.1927(3) 0.1538(17) Uani 1 1 d . . . C37 C 0.850(2) 0.9115(12) 0.1858(9) 0.128(5) Uani 1 1 d . . . H37A H 0.8806 0.8499 0.1663 0.153 Uiso 1 1 calc R . . O10 O 0.5000 1.0000 1.0000 0.306(18) Uiso 1 2 d S . . H10 H 0.5728 1.0110 1.0362 0.367 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 K1 0.0898(14) 0.0571(9) 0.0570(9) 0.0164(7) 0.0265(9) 0.0214(8) O1 0.156(7) 0.076(4) 0.048(3) 0.006(3) 0.037(4) -0.014(4) O2 0.197(8) 0.120(6) 0.093(5) 0.021(5) -0.002(5) -0.016(6) O3 0.161(8) 0.084(5) 0.066(4) -0.014(4) -0.007(5) 0.032(5) O4 0.129(6) 0.065(3) 0.054(3) 0.000(3) 0.014(3) 0.033(3) O5 0.184(8) 0.116(5) 0.101(5) 0.069(5) 0.101(6) 0.100(6) O6 0.197(7) 0.126(5) 0.181(7) 0.093(5) 0.144(6) 0.095(5) O7 0.134(6) 0.067(4) 0.082(4) 0.005(3) 0.057(4) 0.023(4) O8 0.113(5) 0.050(3) 0.075(4) 0.008(3) 0.047(4) 0.029(3) O9 0.208(7) 0.084(4) 0.087(4) 0.008(3) 0.078(5) 0.024(4) N1 0.145(12) 0.242(19) 0.115(10) 0.013(11) 0.041(9) 0.066(12) C1 0.090(7) 0.046(4) 0.055(4) 0.007(3) 0.036(5) 0.015(4) C2 0.078(6) 0.038(3) 0.062(4) 0.006(3) 0.028(4) 0.012(3) C3 0.078(6) 0.037(3) 0.050(4) 0.010(3) 0.019(4) 0.009(3) C4 0.100(8) 0.042(4) 0.061(4) 0.002(3) 0.036(5) 0.008(4) C5 0.092(7) 0.039(4) 0.050(4) 0.005(3) 0.022(4) 0.010(4) C6 0.101(7) 0.042(4) 0.059(5) 0.006(3) 0.023(5) 0.000(4) C7 0.112(9) 0.050(4) 0.058(5) 0.011(4) 0.036(5) 0.010(4) C8 0.126(10) 0.052(4) 0.067(5) 0.029(4) 0.054(6) 0.040(5) C9 0.091(6) 0.058(4) 0.069(5) 0.021(4) 0.038(5) 0.039(4) C10 0.108(8) 0.040(4) 0.056(4) 0.015(3) 0.039(5) 0.028(4) C11 0.108(8) 0.048(4) 0.054(4) 0.017(3) 0.037(5) 0.031(4) C12 0.096(7) 0.047(4) 0.042(4) 0.012(3) 0.025(4) 0.020(4) C13 0.087(6) 0.057(4) 0.053(4) 0.013(4) 0.018(4) 0.027(4) C14 0.087(7) 0.043(4) 0.051(4) 0.009(3) 0.018(4) 0.019(4) C15 0.120(9) 0.040(4) 0.068(5) 0.012(3) 0.047(6) 0.014(4) C16 0.129(9) 0.053(4) 0.064(5) 0.019(4) 0.051(6) 0.033(5) C17 0.102(8) 0.056(5) 0.068(5) 0.005(4) 0.026(5) 0.002(4) C18 0.112(9) 0.082(6) 0.058(5) 0.015(4) 0.038(5) 0.046(5) C19 0.278(15) 0.089(7) 0.067(6) 0.016(5) -0.015(8) -0.071(8) C20 0.284(15) 0.080(6) 0.068(5) 0.001(5) -0.015(7) -0.054(8) C21 0.307(16) 0.100(8) 0.068(6) -0.001(6) -0.034(9) -0.041(9) C22 0.203(18) 0.202(19) 0.045(6) 0.014(8) -0.026(8) -0.079(15) C23 0.27(2) 0.164(14) 0.055(6) 0.001(7) -0.024(9) 0.148(16) C24 0.24(2) 0.090(8) 0.110(10) -0.018(8) -0.071(12) 0.083(11) C25 0.191(8) 0.135(7) 0.196(8) 0.106(6) 0.132(7) 0.105(7) C26 0.185(8) 0.122(6) 0.180(8) 0.084(6) 0.135(7) 0.108(6) C27 0.160(13) 0.127(10) 0.090(7) 0.033(7) 0.077(8) 0.082(9) C28 0.228(10) 0.093(6) 0.168(9) 0.058(7) 0.155(8) 0.073(7) C29 0.090(7) 0.070(5) 0.097(7) 0.014(5) 0.045(6) 0.021(5) C30 0.089(7) 0.053(5) 0.121(8) 0.008(5) 0.057(6) 0.014(4) C31 0.240(11) 0.111(8) 0.116(8) 0.010(7) 0.060(8) 0.035(8) C32 0.097(8) 0.067(6) 0.116(10) 0.012(6) 0.029(7) 0.015(5) C33 0.125(10) 0.059(5) 0.066(6) 0.015(4) 0.055(6) 0.023(5) C34 0.109(9) 0.056(5) 0.067(6) 0.017(4) -0.003(6) 0.002(5) C35 0.145(15) 0.108(10) 0.158(15) 0.060(10) -0.022(12) -0.003(9) C36 0.154(17) 0.173(17) 0.127(13) -0.003(12) 0.047(13) 0.040(13) P1 0.168(4) 0.099(2) 0.0753(17) 0.0175(16) 0.029(2) 0.048(2) F1 0.243(14) 0.233(14) 0.171(10) 0.054(9) 0.109(10) 0.113(11) F2 0.155(10) 0.159(9) 0.247(14) 0.073(9) 0.026(9) 0.013(7) F3 0.242(13) 0.173(9) 0.096(5) 0.006(6) -0.009(6) 0.081(9) F4 0.198(10) 0.162(8) 0.099(5) -0.035(5) 0.051(6) -0.005(7) F5 0.293(17) 0.294(17) 0.156(9) 0.132(11) 0.087(10) 0.161(15) F6 0.49(3) 0.085(6) 0.255(18) -0.006(8) 0.084(19) 0.056(11) Cl1 0.162(3) 0.120(2) 0.111(2) 0.032(2) 0.044(2) 0.048(2) Cl2 0.197(4) 0.116(2) 0.106(2) 0.0352(19) 0.053(3) 0.035(2) Cl3 0.157(4) 0.157(4) 0.143(3) 0.050(3) 0.042(3) 0.010(3) C37 0.178(15) 0.108(9) 0.118(10) 0.032(8) 0.061(10) 0.046(9) _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 K1 O2 2.766(10) . ? K1 O7 2.772(7) . ? K1 O6 2.778(9) . ? K1 O4 2.784(6) . ? K1 O1 2.824(6) . ? K1 O9 2.842(8) . ? K1 O3 2.894(8) . ? K1 O5 2.926(7) . ? K1 O8 3.001(7) . ? K1 C28 3.461(12) . ? O1 C19 1.252(14) . ? O1 C7 1.381(11) . ? O2 C20 1.44(2) . ? O2 C21 1.520(19) . ? O3 C23 1.316(15) . ? O3 C22 1.386(17) . ? O4 C24 1.295(14) . ? O4 C14 1.359(10) 2_666 ? O5 C25 1.156(14) . ? O5 C8 1.408(12) . ? O6 C26 1.330(15) . ? O6 C27 1.377(14) . ? O7 C29 1.409(13) . ? O7 C28 1.417(13) . ? O8 C30 1.401(11) . ? O8 C1 1.425(10) 2_666 ? O9 C33 1.207(12) . ? N1 C36 1.28(2) 2_666 ? N1 C31 1.38(2) . ? N1 H1A 0.8800 . ? C1 C14 1.371(13) . ? C1 C2 1.391(12) . ? C1 O8 1.425(10) 2_666 ? C2 C3 1.383(12) . ? C2 H2A 0.9500 . ? C3 C12 1.366(13) . ? C3 C4 1.542(11) . ? C4 C17 1.470(15) . ? C4 C5 1.516(12) . ? C4 C15 1.552(12) . ? C5 C6 1.380(12) . ? C5 C10 1.383(13) . ? C6 C7 1.358(14) . ? C6 H6A 0.9500 . ? C7 C8 1.376(15) . ? C8 C9 1.388(13) . ? C9 C10 1.409(12) . ? C9 H9A 0.9500 . ? C10 C11 1.531(11) . ? C11 C18 1.476(15) . ? C11 C12 1.540(12) . ? C11 C16 1.586(12) . ? C12 C13 1.400(12) . ? C13 C14 1.389(12) . ? C13 H13A 0.9500 . ? C14 O4 1.359(10) 2_666 ? C15 C16 1.519(15) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.449(17) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.409(17) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.378(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.494(18) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.379(19) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.439(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.62(3) . ? C31 H31A 0.9500 . ? C32 C33 1.427(18) . ? C32 C34 1.430(17) 2_666 ? C33 C34 1.434(17) . ? C34 C35 1.42(2) . ? C34 C32 1.430(18) 2_666 ? C35 C36 1.250(17) . ? C36 N1 1.28(2) 2_666 ? P1 F6 1.480(13) . ? P1 F4 1.509(10) . ? P1 F5 1.538(11) . ? P1 F2 1.543(15) . ? P1 F3 1.587(10) . ? P1 F1 1.638(14) . ? Cl1 C37 1.755(18) . ? Cl2 C37 1.773(14) . ? Cl3 C37 1.713(18) . ? C37 H37A 1.0000 . ? O10 H10 0.8064 . ? 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 O2 K1 O7 108.8(3) . . ? O2 K1 O6 92.7(4) . . ? O7 K1 O6 59.3(2) . . ? O2 K1 O4 114.1(3) . . ? O7 K1 O4 86.3(2) . . ? O6 K1 O4 142.4(3) . . ? O2 K1 O1 57.8(3) . . ? O7 K1 O1 156.4(2) . . ? O6 K1 O1 99.9(3) . . ? O4 K1 O1 116.4(3) . . ? O2 K1 O9 130.1(3) . . ? O7 K1 O9 121.0(3) . . ? O6 K1 O9 109.3(4) . . ? O4 K1 O9 74.0(2) . . ? O1 K1 O9 74.2(2) . . ? O2 K1 O3 62.6(3) . . ? O7 K1 O3 78.8(3) . . ? O6 K1 O3 121.5(3) . . ? O4 K1 O3 58.4(2) . . ? O1 K1 O3 107.0(3) . . ? O9 K1 O3 127.5(3) . . ? O2 K1 O5 94.4(3) . . ? O7 K1 O5 111.5(3) . . ? O6 K1 O5 56.0(2) . . ? O4 K1 O5 139.9(2) . . ? O1 K1 O5 55.5(3) . . ? O9 K1 O5 66.0(3) . . ? O3 K1 O5 157.0(3) . . ? O2 K1 O8 161.1(2) . . ? O7 K1 O8 57.39(18) . . ? O6 K1 O8 90.2(3) . . ? O4 K1 O8 56.0(2) . . ? O1 K1 O8 139.78(18) . . ? O9 K1 O8 65.7(2) . . ? O3 K1 O8 100.2(2) . . ? O5 K1 O8 102.7(3) . . ? O2 K1 C28 92.5(4) . . ? O7 K1 C28 23.1(3) . . ? O6 K1 C28 41.7(3) . . ? O4 K1 C28 108.1(3) . . ? O1 K1 C28 133.4(3) . . ? O9 K1 C28 133.6(4) . . ? O3 K1 C28 84.6(4) . . ? O5 K1 C28 97.6(3) . . ? O8 K1 C28 77.4(3) . . ? C19 O1 C7 122.6(8) . . ? C19 O1 K1 123.2(7) . . ? C7 O1 K1 112.8(5) . . ? C20 O2 C21 100.9(13) . . ? C20 O2 K1 118.9(8) . . ? C21 O2 K1 113.3(8) . . ? C23 O3 C22 111.1(15) . . ? C23 O3 K1 116.8(6) . . ? C22 O3 K1 117.0(8) . . ? C24 O4 C14 121.3(8) . 2_666 ? C24 O4 K1 120.3(7) . . ? C14 O4 K1 117.7(5) 2_666 . ? C25 O5 C8 127.6(9) . . ? C25 O5 K1 118.7(8) . . ? C8 O5 K1 108.2(6) . . ? C26 O6 C27 117.7(10) . . ? C26 O6 K1 124.1(7) . . ? C27 O6 K1 118.2(7) . . ? C29 O7 C28 113.0(11) . . ? C29 O7 K1 120.5(5) . . ? C28 O7 K1 106.9(6) . . ? C30 O8 C1 114.7(6) . 2_666 ? C30 O8 K1 112.4(5) . . ? C1 O8 K1 107.6(5) 2_666 . ? C33 O9 K1 164.2(10) . . ? C36 N1 C31 132(2) 2_666 . ? C36 N1 H1A 114.0 2_666 . ? C31 N1 H1A 114.0 . . ? C14 C1 C2 121.0(8) . . ? C14 C1 O8 120.9(7) . 2_666 ? C2 C1 O8 118.1(9) . 2_666 ? C3 C2 C1 119.4(9) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C12 C3 C2 120.4(7) . . ? C12 C3 C4 114.4(7) . . ? C2 C3 C4 125.2(8) . . ? C17 C4 C5 115.5(8) . . ? C17 C4 C3 114.2(8) . . ? C5 C4 C3 106.4(7) . . ? C17 C4 C15 111.7(7) . . ? C5 C4 C15 104.9(7) . . ? C3 C4 C15 103.1(7) . . ? C6 C5 C10 120.0(8) . . ? C6 C5 C4 125.2(9) . . ? C10 C5 C4 114.7(7) . . ? C7 C6 C5 121.5(10) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C8 119.3(9) . . ? C6 C7 O1 124.3(11) . . ? C8 C7 O1 116.4(8) . . ? C7 C8 C9 121.2(8) . . ? C7 C8 O5 119.2(9) . . ? C9 C8 O5 119.4(11) . . ? C8 C9 C10 118.8(10) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C5 C10 C9 119.2(8) . . ? C5 C10 C11 116.5(7) . . ? C9 C10 C11 124.3(9) . . ? C18 C11 C10 115.8(7) . . ? C18 C11 C12 116.4(8) . . ? C10 C11 C12 104.6(7) . . ? C18 C11 C16 113.2(7) . . ? C10 C11 C16 102.9(7) . . ? C12 C11 C16 102.1(7) . . ? C3 C12 C13 120.0(8) . . ? C3 C12 C11 117.0(7) . . ? C13 C12 C11 123.0(9) . . ? C14 C13 C12 119.9(9) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? O4 C14 C1 117.2(8) 2_666 . ? O4 C14 C13 123.5(9) 2_666 . ? C1 C14 C13 119.2(7) . . ? C16 C15 C4 112.1(7) . . ? C16 C15 H15A 109.2 . . ? C4 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C4 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C11 112.1(7) . . ? C15 C16 H16A 109.2 . . ? C11 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C11 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C4 C17 H17A 109.5 . . ? C4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 118.7(10) . . ? O1 C19 H19A 107.7 . . ? C20 C19 H19A 107.7 . . ? O1 C19 H19B 107.6 . . ? C20 C19 H19B 107.6 . . ? H19A C19 H19B 107.1 . . ? C19 C20 O2 113.1(14) . . ? C19 C20 H20A 108.9 . . ? O2 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? O2 C20 H20B 108.9 . . ? H20A C20 H20B 107.8 . . ? C22 C21 O2 125.2(11) . . ? C22 C21 H21A 106.0 . . ? O2 C21 H21A 106.0 . . ? C22 C21 H21B 106.0 . . ? O2 C21 H21B 106.1 . . ? H21A C21 H21B 106.3 . . ? O3 C22 C21 114.4(14) . . ? O3 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? O3 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? O3 C23 C24 121.0(10) . . ? O3 C23 H23A 107.1 . . ? C24 C23 H23A 107.1 . . ? O3 C23 H23B 107.1 . . ? C24 C23 H23B 107.1 . . ? H23A C23 H23B 106.8 . . ? O4 C24 C23 123.3(11) . . ? O4 C24 H24A 106.5 . . ? C23 C24 H24A 106.5 . . ? O4 C24 H24B 106.5 . . ? C23 C24 H24B 106.5 . . ? H24A C24 H24B 106.5 . . ? O5 C25 C26 121.1(11) . . ? O5 C25 H25A 107.1 . . ? C26 C25 H25A 107.1 . . ? O5 C25 H25B 107.1 . . ? C26 C25 H25B 107.1 . . ? H25A C25 H25B 106.8 . . ? O6 C26 C25 114.2(11) . . ? O6 C26 H26A 108.7 . . ? C25 C26 H26A 108.7 . . ? O6 C26 H26B 108.7 . . ? C25 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 O6 114.0(11) . . ? C28 C27 H27A 108.7 . . ? O6 C27 H27A 108.7 . . ? C28 C27 H27B 108.8 . . ? O6 C27 H27B 108.8 . . ? H27A C27 H27B 107.6 . . ? C27 C28 O7 118.4(12) . . ? C27 C28 K1 86.1(7) . . ? O7 C28 K1 50.0(5) . . ? C27 C28 H28A 107.7 . . ? O7 C28 H28A 107.7 . . ? K1 C28 H28A 157.7 . . ? C27 C28 H28B 107.7 . . ? O7 C28 H28B 107.7 . . ? K1 C28 H28B 84.3 . . ? H28A C28 H28B 107.1 . . ? O7 C29 C30 110.3(9) . . ? O7 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? O7 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O8 C30 C29 111.1(8) . . ? O8 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? O8 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? N1 C31 C32 113.3(16) . . ? N1 C31 H31A 123.4 . . ? C32 C31 H31A 123.4 . . ? C33 C32 C34 119.8(11) . 2_666 ? C33 C32 C31 131.9(13) . . ? C34 C32 C31 108.3(12) 2_666 . ? O9 C33 C32 119.6(13) . . ? O9 C33 C34 122.3(12) . . ? C32 C33 C34 118.1(9) . . ? C35 C34 C32 126.2(15) . 2_666 ? C35 C34 C33 111.7(14) . . ? C32 C34 C33 122.1(10) 2_666 . ? C36 C35 C34 122(2) . . ? C35 C36 N1 119(2) . 2_666 ? F6 P1 F4 177.0(11) . . ? F6 P1 F5 88.8(10) . . ? F4 P1 F5 91.8(9) . . ? F6 P1 F2 96.6(11) . . ? F4 P1 F2 86.3(7) . . ? F5 P1 F2 91.1(8) . . ? F6 P1 F3 91.9(8) . . ? F4 P1 F3 87.4(6) . . ? F5 P1 F3 178.3(10) . . ? F2 P1 F3 90.4(7) . . ? F6 P1 F1 90.3(11) . . ? F4 P1 F1 86.7(7) . . ? F5 P1 F1 92.2(8) . . ? F2 P1 F1 172.4(7) . . ? F3 P1 F1 86.2(7) . . ? Cl3 C37 Cl1 109.5(8) . . ? Cl3 C37 Cl2 111.3(10) . . ? Cl1 C37 Cl2 111.5(9) . . ? Cl3 C37 H37A 108.1 . . ? Cl1 C37 H37A 108.1 . . ? Cl2 C37 H37A 108.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.966 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.136 # Attachment '- CCDC-768490.cif' data_ic14179 _database_code_depnum_ccdc_archive 'CCDC 768490' #TrackingRef '- CCDC-768490.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 O16, C12 H8 N2 O2, 2(C2 F3 O2), C H2 Cl2' _chemical_formula_sum 'C77 H86 Cl2 F6 N2 O22' _chemical_formula_weight 1576.38 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' 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 12.3293(4) _cell_length_b 13.3179(5) _cell_length_c 13.9601(5) _cell_angle_alpha 106.715(3) _cell_angle_beta 96.272(3) _cell_angle_gamma 93.438(3) _cell_volume 2172.18(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15458 _cell_measurement_theta_min 3.3298 _cell_measurement_theta_max 77.4413 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 1.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54024 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23326 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 67.98 _reflns_number_total 7905 _reflns_number_gt 6981 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+11.0000P] 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 7905 _refine_ls_number_parameters 564 _refine_ls_number_restraints 229 _refine_ls_R_factor_all 0.1786 _refine_ls_R_factor_gt 0.1688 _refine_ls_wR_factor_ref 0.4102 _refine_ls_wR_factor_gt 0.4053 _refine_ls_goodness_of_fit_ref 1.591 _refine_ls_restrained_S_all 1.607 _refine_ls_shift/su_max 0.165 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.1320(3) -0.2412(3) 0.1707(3) 0.0272(10) Uani 1 1 d . . . O2 O 0.2729(4) -0.3608(4) 0.2552(3) 0.0326(11) Uani 1 1 d . . . O3 O 0.3891(4) -0.4043(4) 0.4239(4) 0.0392(12) Uani 1 1 d . . . O4 O 0.2253(4) -0.3573(4) 0.5482(3) 0.0322(11) Uani 1 1 d . . . O5 O -0.0759(4) -0.2796(3) 0.1233(4) 0.0316(10) Uani 1 1 d . . . O6 O -0.1387(4) -0.4869(4) 0.0295(3) 0.0348(11) Uani 1 1 d . . . O7 O -0.0236(4) -0.4378(3) 0.2519(3) 0.0303(10) Uani 1 1 d . . . O8 O 0.0280(4) -0.3942(3) 0.4611(3) 0.0294(10) Uani 1 1 d . . . C1 C 0.0761(5) -0.1537(5) 0.1724(4) 0.0245(13) Uani 1 1 d . . . C2 C 0.1232(5) -0.0508(5) 0.2045(4) 0.0249(13) Uani 1 1 d . . . H2A H 0.1990 -0.0354 0.2297 0.030 Uiso 1 1 calc R . . C3 C 0.0581(5) 0.0299(5) 0.1994(4) 0.0245(13) Uani 1 1 d . . . C4 C 0.0975(5) 0.1475(5) 0.2323(5) 0.0270(13) Uani 1 1 d . . . C5 C 0.0155(5) 0.2034(5) 0.2977(5) 0.0251(13) Uani 1 1 d . . . C6 C 0.0418(5) 0.2750(5) 0.3947(5) 0.0253(13) Uani 1 1 d . . . H6A H 0.1157 0.2903 0.4260 0.030 Uiso 1 1 calc R . . C7 C -0.0415(5) 0.3230(5) 0.4443(4) 0.0250(13) Uani 1 1 d . . . C8 C -0.1509(5) 0.3013(5) 0.3969(5) 0.0269(13) Uani 1 1 d . . . C9 C -0.1768(5) 0.2300(5) 0.3020(5) 0.0274(13) Uani 1 1 d . . . H9A H -0.2507 0.2144 0.2705 0.033 Uiso 1 1 calc R . . C10 C -0.0928(5) 0.1813(5) 0.2532(4) 0.0252(13) Uani 1 1 d . . . C11 C -0.1094(5) 0.1018(5) 0.1479(5) 0.0274(13) Uani 1 1 d . . . C12 C -0.0517(5) 0.0071(5) 0.1594(4) 0.0247(13) Uani 1 1 d . . . C13 C -0.1009(5) -0.0959(5) 0.1331(4) 0.0254(13) Uani 1 1 d . . . H13A H -0.1771 -0.1111 0.1095 0.031 Uiso 1 1 calc R . . C14 C -0.0367(5) -0.1759(5) 0.1419(4) 0.0243(12) Uani 1 1 d . . . C15 C 0.0795(6) 0.1811(5) 0.1333(5) 0.0326(15) Uani 1 1 d . . . H15A H 0.0977 0.2581 0.1496 0.039 Uiso 1 1 calc R . . H15B H 0.1290 0.1454 0.0858 0.039 Uiso 1 1 calc R . . C16 C -0.0403(6) 0.1517(5) 0.0833(5) 0.0322(15) Uani 1 1 d . . . H16A H -0.0424 0.1010 0.0154 0.039 Uiso 1 1 calc R . . H16B H -0.0725 0.2156 0.0753 0.039 Uiso 1 1 calc R . . C17 C 0.2165(5) 0.1732(5) 0.2800(6) 0.0344(15) Uani 1 1 d . . . H17A H 0.2262 0.1519 0.3418 0.052 Uiso 1 1 calc R . . H17B H 0.2366 0.2491 0.2965 0.052 Uiso 1 1 calc R . . H17C H 0.2636 0.1351 0.2325 0.052 Uiso 1 1 calc R . . C18 C -0.2279(6) 0.0757(5) 0.0985(5) 0.0325(15) Uani 1 1 d . . . H18A H -0.2706 0.0446 0.1398 0.049 Uiso 1 1 calc R . . H18B H -0.2309 0.0254 0.0312 0.049 Uiso 1 1 calc R . . H18C H -0.2585 0.1402 0.0926 0.049 Uiso 1 1 calc R . . C19 C 0.2486(5) -0.2274(5) 0.1742(6) 0.0330(15) Uani 1 1 d . . . H19A H 0.2815 -0.1749 0.2383 0.040 Uiso 1 1 calc R . . H19B H 0.2677 -0.2023 0.1175 0.040 Uiso 1 1 calc R . . C20 C 0.2908(6) -0.3327(5) 0.1666(5) 0.0318(14) Uani 1 1 d . . . H20A H 0.2520 -0.3866 0.1061 0.038 Uiso 1 1 calc R . . H20B H 0.3701 -0.3287 0.1605 0.038 Uiso 1 1 calc R . . C21 C 0.3101(6) -0.4609(5) 0.2530(5) 0.0337(15) Uani 1 1 d . . . H21A H 0.3859 -0.4634 0.2359 0.040 Uiso 1 1 calc R . . H21B H 0.2625 -0.5174 0.2008 0.040 Uiso 1 1 calc R . . C22 C 0.3068(6) -0.4772(6) 0.3541(5) 0.0369(16) Uani 1 1 d . . . H22A H 0.2336 -0.4650 0.3758 0.044 Uiso 1 1 calc R . . H22B H 0.3212 -0.5504 0.3511 0.044 Uiso 1 1 calc R . . C23 C 0.3992(6) -0.4156(7) 0.5238(5) 0.0423(18) Uani 1 1 d . . . H23A H 0.4776 -0.4048 0.5525 0.051 Uiso 1 1 calc R . . H23B H 0.3710 -0.4880 0.5201 0.051 Uiso 1 1 calc R . . C24 C 0.3366(6) -0.3375(6) 0.5924(5) 0.0350(15) Uani 1 1 d . . . H24A H 0.3440 -0.3469 0.6605 0.042 Uiso 1 1 calc R . . H24B H 0.3651 -0.2646 0.5984 0.042 Uiso 1 1 calc R . . C25 C -0.1885(5) -0.3104(5) 0.0823(5) 0.0318(14) Uani 1 1 d . . . H25A H -0.2012 -0.3079 0.0118 0.038 Uiso 1 1 calc R . . H25B H -0.2365 -0.2630 0.1226 0.038 Uiso 1 1 calc R . . C26 C -0.2116(6) -0.4214(5) 0.0864(5) 0.0336(15) Uani 1 1 d . . . H26A H -0.2007 -0.4228 0.1573 0.040 Uiso 1 1 calc R . . H26B H -0.2885 -0.4478 0.0578 0.040 Uiso 1 1 calc R . . C27 C -0.0877(6) -0.5561(5) 0.0776(5) 0.0317(14) Uani 1 1 d . . . H27A H -0.0599 -0.6129 0.0259 0.038 Uiso 1 1 calc R . . H27B H -0.1435 -0.5893 0.1077 0.038 Uiso 1 1 calc R . . C28 C 0.0064(6) -0.5026(5) 0.1594(5) 0.0313(14) Uani 1 1 d . . . H28A H 0.0497 -0.5576 0.1747 0.038 Uiso 1 1 calc R . . H28B H 0.0549 -0.4585 0.1322 0.038 Uiso 1 1 calc R . . C29 C -0.0738(6) -0.4974(5) 0.3082(5) 0.0318(15) Uani 1 1 d . . . H29A H -0.0293 -0.5552 0.3140 0.038 Uiso 1 1 calc R . . H29B H -0.1478 -0.5285 0.2736 0.038 Uiso 1 1 calc R . . C30 C -0.0820(5) -0.4248(5) 0.4109(5) 0.0309(14) Uani 1 1 d . . . H30A H -0.1184 -0.3621 0.4053 0.037 Uiso 1 1 calc R . . H30B H -0.1250 -0.4613 0.4491 0.037 Uiso 1 1 calc R . . O9 O -0.1659(5) -0.1134(5) 0.3631(5) 0.0666(19) Uani 1 1 d . . . N1 N 0.1375(6) -0.2311(5) 0.3773(5) 0.0473(18) Uani 1 1 d . . . H1A H 0.1481 -0.2923 0.3358 0.057 Uiso 1 1 calc R . . C31 C -0.0911(6) -0.0616(6) 0.4252(6) 0.0398(17) Uani 1 1 d . . . C32 C 0.0184(6) -0.1017(5) 0.4345(5) 0.0320(15) Uani 1 1 d . . . C33 C 0.1053(6) -0.0428(5) 0.5058(5) 0.0340(15) Uani 1 1 d . . . C34 C 0.2083(7) -0.0825(7) 0.5091(6) 0.0466(19) Uani 1 1 d . . . H34A H 0.2678 -0.0434 0.5570 0.056 Uiso 1 1 calc R . . C35 C 0.2227(8) -0.1772(7) 0.4435(6) 0.050(2) Uani 1 1 d . . . H35A H 0.2922 -0.2044 0.4447 0.060 Uiso 1 1 calc R . . C36 C 0.0358(7) -0.1981(6) 0.3696(5) 0.0398(17) Uani 1 1 d . . . H36A H -0.0218 -0.2398 0.3212 0.048 Uiso 1 1 calc R . . F1 F 0.4532(11) 0.7717(15) 0.8699(14) 0.105(4) Uani 0.479(6) 1 d PU . . F2 F 0.6009(13) 0.7737(17) 0.9576(17) 0.118(4) Uani 0.479(6) 1 d PU . . F3 F 0.5884(12) 0.7019(16) 0.8503(16) 0.113(4) Uani 0.479(6) 1 d PU . . O10 O 0.5313(10) 0.5974(12) 0.9784(15) 0.100(4) Uani 0.479(6) 1 d PDU . . O11 O 0.3743(13) 0.6482(19) 0.9433(18) 0.109(5) Uani 0.479(6) 1 d PU . . C37 C 0.515(2) 0.724(3) 0.912(3) 0.105(4) Uani 0.479(6) 1 d PU . . C38 C 0.4745(19) 0.630(3) 0.929(3) 0.104(4) Uani 0.479(6) 1 d PU . . F4 F 0.4254(7) -0.0142(9) 0.1870(6) 0.054(2) Uani 0.521(6) 1 d PU . . F5 F 0.5778(11) -0.0590(13) 0.2321(9) 0.089(3) Uani 0.521(6) 1 d PU . . F6 F 0.5800(10) 0.0633(12) 0.2660(8) 0.090(3) Uani 0.521(6) 1 d PU . . O12 O 0.5316(11) 0.0649(14) 0.4350(10) 0.078(4) Uani 0.521(6) 1 d PU . . O13 O 0.3673(7) -0.0190(8) 0.3585(7) 0.036(2) Uani 0.521(6) 1 d PU . . C39 C 0.5032(13) 0.0061(17) 0.2586(12) 0.060(3) Uani 0.521(6) 1 d PU . . C40 C 0.4645(15) 0.0014(19) 0.3581(12) 0.066(3) Uani 0.521(6) 1 d PU . . Cl1 Cl 0.3798(7) 0.4038(10) 0.7193(7) 0.155(4) Uani 0.50 1 d PU . . Cl2 Cl 0.3436(7) 0.2734(9) 0.5218(6) 0.126(3) Uani 0.50 1 d PU . . C41 C 0.393(3) 0.304(2) 0.640(2) 0.101(6) Uiso 0.50 1 d PU . . H41A H 0.3642 0.2466 0.6646 0.121 Uiso 0.50 1 calc PR . . H41B H 0.4728 0.2998 0.6418 0.121 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.026(2) 0.022(2) 0.033(2) 0.0055(18) 0.0043(18) 0.0044(17) O2 0.039(3) 0.027(2) 0.029(2) 0.0018(19) 0.0065(19) 0.0132(19) O3 0.034(3) 0.049(3) 0.030(2) 0.003(2) 0.006(2) 0.007(2) O4 0.030(2) 0.033(2) 0.029(2) -0.0021(19) 0.0097(19) 0.0082(19) O5 0.027(2) 0.024(2) 0.041(3) 0.0076(19) -0.0011(19) -0.0005(18) O6 0.046(3) 0.027(2) 0.027(2) 0.0013(19) 0.001(2) 0.003(2) O7 0.042(3) 0.026(2) 0.020(2) 0.0026(17) 0.0044(19) -0.0022(19) O8 0.034(2) 0.030(2) 0.020(2) -0.0005(18) 0.0044(18) 0.0052(19) C1 0.026(3) 0.026(3) 0.022(3) 0.007(2) 0.005(2) 0.006(2) C2 0.026(3) 0.025(3) 0.023(3) 0.004(2) 0.005(2) 0.001(2) C3 0.029(3) 0.022(3) 0.021(3) 0.002(2) 0.008(2) 0.002(2) C4 0.033(3) 0.021(3) 0.026(3) 0.003(2) 0.009(3) 0.001(2) C5 0.031(3) 0.021(3) 0.024(3) 0.006(2) 0.008(2) 0.003(2) C6 0.028(3) 0.023(3) 0.025(3) 0.007(2) 0.004(2) 0.001(2) C7 0.033(3) 0.022(3) 0.019(3) 0.003(2) 0.007(2) 0.002(2) C8 0.032(3) 0.025(3) 0.024(3) 0.005(2) 0.009(3) 0.005(3) C9 0.030(3) 0.026(3) 0.025(3) 0.005(3) 0.004(3) 0.004(3) C10 0.031(3) 0.022(3) 0.021(3) 0.004(2) 0.005(2) 0.003(2) C11 0.033(3) 0.026(3) 0.022(3) 0.003(2) 0.004(3) 0.007(3) C12 0.029(3) 0.025(3) 0.020(3) 0.005(2) 0.006(2) 0.005(2) C13 0.027(3) 0.025(3) 0.021(3) 0.002(2) 0.002(2) 0.002(2) C14 0.027(3) 0.022(3) 0.023(3) 0.005(2) 0.003(2) 0.001(2) C15 0.044(4) 0.025(3) 0.030(3) 0.006(3) 0.017(3) 0.004(3) C16 0.047(4) 0.027(3) 0.025(3) 0.007(3) 0.010(3) 0.010(3) C17 0.028(3) 0.028(3) 0.043(4) 0.001(3) 0.011(3) -0.001(3) C18 0.036(4) 0.029(3) 0.027(3) 0.001(3) -0.003(3) 0.011(3) C19 0.025(3) 0.032(3) 0.041(4) 0.010(3) 0.006(3) 0.002(3) C20 0.028(3) 0.032(3) 0.033(3) 0.006(3) 0.005(3) 0.006(3) C21 0.035(4) 0.026(3) 0.036(4) 0.001(3) 0.006(3) 0.012(3) C22 0.040(4) 0.032(4) 0.036(4) 0.006(3) 0.006(3) 0.009(3) C23 0.041(4) 0.053(5) 0.031(4) 0.006(3) 0.006(3) 0.022(4) C24 0.031(4) 0.043(4) 0.029(3) 0.007(3) 0.005(3) 0.011(3) C25 0.025(3) 0.031(3) 0.036(4) 0.008(3) -0.001(3) -0.002(3) C26 0.032(4) 0.028(3) 0.036(4) 0.004(3) 0.001(3) 0.002(3) C27 0.047(4) 0.020(3) 0.024(3) 0.000(2) 0.004(3) 0.002(3) C28 0.038(4) 0.029(3) 0.024(3) 0.002(3) 0.008(3) 0.004(3) C29 0.043(4) 0.028(3) 0.023(3) 0.006(3) 0.004(3) -0.002(3) C30 0.033(4) 0.030(3) 0.027(3) 0.005(3) 0.005(3) -0.002(3) O9 0.049(4) 0.058(4) 0.068(4) -0.014(3) -0.001(3) -0.006(3) N1 0.080(5) 0.035(3) 0.038(3) 0.016(3) 0.028(4) 0.032(3) C31 0.046(4) 0.033(4) 0.034(4) 0.000(3) 0.008(3) -0.005(3) C32 0.045(4) 0.023(3) 0.027(3) 0.004(3) 0.013(3) 0.002(3) C33 0.036(4) 0.033(4) 0.034(4) 0.009(3) 0.014(3) 0.004(3) C34 0.045(4) 0.055(5) 0.044(4) 0.017(4) 0.011(4) 0.013(4) C35 0.059(5) 0.061(5) 0.041(4) 0.024(4) 0.019(4) 0.032(4) C36 0.066(5) 0.027(3) 0.027(3) 0.006(3) 0.013(3) 0.004(3) F1 0.050(6) 0.152(10) 0.140(9) 0.087(8) 0.004(6) 0.032(6) F2 0.067(6) 0.164(9) 0.153(8) 0.093(8) 0.007(6) 0.019(6) F3 0.068(6) 0.158(9) 0.151(8) 0.097(8) 0.036(6) 0.018(6) O10 0.035(6) 0.175(10) 0.133(9) 0.110(8) 0.006(6) 0.036(7) O11 0.044(7) 0.165(11) 0.148(10) 0.092(9) 0.013(7) 0.018(7) C37 0.047(6) 0.158(9) 0.144(9) 0.093(8) 0.015(6) 0.031(6) C38 0.043(6) 0.165(9) 0.141(9) 0.099(8) 0.024(6) 0.019(6) F4 0.035(4) 0.099(6) 0.024(4) 0.019(4) -0.002(3) -0.017(4) F5 0.076(5) 0.136(7) 0.059(5) 0.032(5) 0.023(4) 0.003(5) F6 0.069(5) 0.130(6) 0.054(5) 0.010(5) 0.022(4) -0.049(5) O12 0.052(6) 0.124(8) 0.046(6) 0.014(6) 0.006(5) -0.024(6) O13 0.016(4) 0.063(6) 0.031(4) 0.017(4) 0.008(3) -0.011(4) C39 0.040(5) 0.110(7) 0.032(5) 0.023(5) 0.023(4) -0.023(5) C40 0.049(5) 0.116(7) 0.032(5) 0.022(5) 0.015(4) -0.017(5) Cl1 0.108(5) 0.214(9) 0.093(5) -0.028(6) 0.042(4) -0.058(6) Cl2 0.100(5) 0.177(8) 0.080(4) 0.019(5) -0.007(4) -0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.385(7) . ? O1 C19 1.432(8) . ? O2 C20 1.426(8) . ? O2 C21 1.429(8) . ? O3 C22 1.430(9) . ? O3 C23 1.438(9) . ? O4 C8 1.375(7) 2_556 ? O4 C24 1.419(8) . ? O5 C14 1.378(7) . ? O5 C25 1.430(8) . ? O6 C27 1.425(8) . ? O6 C26 1.431(8) . ? O7 C29 1.427(8) . ? O7 C28 1.433(7) . ? O8 C7 1.373(7) 2_556 ? O8 C30 1.434(8) . ? C1 C2 1.381(9) . ? C1 C14 1.398(9) . ? C2 C3 1.393(9) . ? C3 C12 1.387(9) . ? C3 C4 1.532(8) . ? C4 C5 1.519(8) . ? C4 C17 1.520(9) . ? C4 C15 1.568(9) . ? C5 C10 1.387(9) . ? C5 C6 1.404(9) . ? C6 C7 1.386(9) . ? C7 O8 1.373(7) 2_556 ? C7 C8 1.410(9) . ? C8 O4 1.375(7) 2_556 ? C8 C9 1.381(9) . ? C9 C10 1.391(9) . ? C10 C11 1.528(8) . ? C11 C18 1.520(9) . ? C11 C12 1.524(8) . ? C11 C16 1.557(9) . ? C12 C13 1.395(9) . ? C13 C14 1.389(9) . ? C15 C16 1.540(10) . ? C19 C20 1.504(9) . ? C21 C22 1.494(10) . ? C23 C24 1.509(9) . ? C25 C26 1.506(9) . ? C27 C28 1.517(9) . ? C29 C30 1.499(9) . ? O9 C31 1.217(10) . ? N1 C35 1.338(12) . ? N1 C36 1.357(11) . ? C31 C33 1.479(10) 2_556 ? C31 C32 1.487(11) . ? C32 C36 1.386(9) . ? C32 C33 1.403(10) . ? C33 C34 1.406(11) . ? C33 C31 1.479(10) 2_556 ? C34 C35 1.364(12) . ? F1 C37 1.23(3) . ? F2 C37 1.22(4) . ? F2 F3 1.51(3) . ? F3 C37 1.30(3) . ? O10 C38 1.13(3) . ? O11 C38 1.30(3) . ? C37 C38 1.40(4) . ? F4 C39 1.264(19) . ? F5 C39 1.31(2) . ? F5 F6 1.56(2) . ? F6 C39 1.155(18) . ? O12 C40 1.32(2) . ? O13 C40 1.214(19) . ? C39 C40 1.533(19) . ? Cl1 C41 1.49(3) . ? Cl2 C41 1.62(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 C1 O1 C19 116.5(5) . . ? C20 O2 C21 111.9(5) . . ? C22 O3 C23 113.7(6) . . ? C8 O4 C24 116.8(5) 2_556 . ? C14 O5 C25 118.2(5) . . ? C27 O6 C26 115.1(5) . . ? C29 O7 C28 112.8(5) . . ? C7 O8 C30 117.3(5) 2_556 . ? C2 C1 O1 125.0(6) . . ? C2 C1 C14 120.4(6) . . ? O1 C1 C14 114.6(5) . . ? C1 C2 C3 119.1(6) . . ? C12 C3 C2 120.4(6) . . ? C12 C3 C4 114.0(5) . . ? C2 C3 C4 125.5(6) . . ? C5 C4 C17 114.9(5) . . ? C5 C4 C3 106.4(5) . . ? C17 C4 C3 114.1(5) . . ? C5 C4 C15 105.1(5) . . ? C17 C4 C15 110.6(5) . . ? C3 C4 C15 104.8(5) . . ? C10 C5 C6 119.8(6) . . ? C10 C5 C4 114.7(5) . . ? C6 C5 C4 125.5(6) . . ? C7 C6 C5 119.2(6) . . ? O8 C7 C6 125.5(6) 2_556 . ? O8 C7 C8 114.3(5) 2_556 . ? C6 C7 C8 120.2(6) . . ? O4 C8 C9 124.7(6) 2_556 . ? O4 C8 C7 114.7(5) 2_556 . ? C9 C8 C7 120.6(6) . . ? C8 C9 C10 118.8(6) . . ? C5 C10 C9 121.4(6) . . ? C5 C10 C11 114.2(5) . . ? C9 C10 C11 124.5(6) . . ? C18 C11 C12 114.5(5) . . ? C18 C11 C10 114.9(5) . . ? C12 C11 C10 105.4(5) . . ? C18 C11 C16 110.2(5) . . ? C12 C11 C16 105.7(5) . . ? C10 C11 C16 105.4(5) . . ? C3 C12 C13 120.4(6) . . ? C3 C12 C11 114.6(5) . . ? C13 C12 C11 125.1(6) . . ? C14 C13 C12 118.9(6) . . ? O5 C14 C13 124.7(6) . . ? O5 C14 C1 115.0(5) . . ? C13 C14 C1 120.2(6) . . ? C16 C15 C4 110.5(5) . . ? C15 C16 C11 111.0(5) . . ? O1 C19 C20 107.3(5) . . ? O2 C20 C19 108.6(5) . . ? O2 C21 C22 109.1(5) . . ? O3 C22 C21 107.8(6) . . ? O3 C23 C24 111.5(6) . . ? O4 C24 C23 106.8(6) . . ? O5 C25 C26 106.0(5) . . ? O6 C26 C25 108.9(6) . . ? O6 C27 C28 114.0(5) . . ? O7 C28 C27 115.9(6) . . ? O7 C29 C30 108.2(5) . . ? O8 C30 C29 106.7(5) . . ? C35 N1 C36 124.6(7) . . ? O9 C31 C33 121.6(8) . 2_556 ? O9 C31 C32 120.9(7) . . ? C33 C31 C32 117.5(6) 2_556 . ? C36 C32 C33 119.3(7) . . ? C36 C32 C31 119.2(7) . . ? C33 C32 C31 121.5(6) . . ? C32 C33 C34 119.3(7) . . ? C32 C33 C31 121.0(7) . 2_556 ? C34 C33 C31 119.7(7) . 2_556 ? C35 C34 C33 119.9(8) . . ? N1 C35 C34 118.9(8) . . ? N1 C36 C32 118.1(7) . . ? C37 F2 F3 55.7(19) . . ? C37 F3 F2 50.7(18) . . ? F2 C37 F1 116(3) . . ? F2 C37 F3 73.6(19) . . ? F1 C37 F3 102(2) . . ? F2 C37 C38 122(3) . . ? F1 C37 C38 120(3) . . ? F3 C37 C38 109(3) . . ? O10 C38 O11 124(3) . . ? O10 C38 C37 116(3) . . ? O11 C38 C37 102(3) . . ? C39 F5 F6 46.5(10) . . ? C39 F6 F5 55.5(13) . . ? F6 C39 F4 124.0(16) . . ? F6 C39 F5 78.0(14) . . ? F4 C39 F5 108.6(15) . . ? F6 C39 C40 115.9(15) . . ? F4 C39 C40 112.5(12) . . ? F5 C39 C40 111.6(17) . . ? O13 C40 O12 124.9(16) . . ? O13 C40 C39 118.0(15) . . ? O12 C40 C39 109.7(14) . . ? Cl1 C41 Cl2 126(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 67.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.700 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.217 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons #_platon_squeeze_void_content #1 0.000 0.500 0.500 300 101 . #_platon_squeeze_details # Attachment 'ic14420-platon_3.cif' data_ic14420 _database_code_depnum_ccdc_archive 'CCDC 786869' #TrackingRef 'ic14420-platon_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'K2, C60 H76 O16, C12 H6 N2 O2, P2F12' _chemical_formula_sum 'C72 H82 F12 K2 N2 O18 P2' _chemical_formula_weight 1631.54 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' 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' _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 9.3277(5) _cell_length_b 13.4654(4) _cell_length_c 17.3928(6) _cell_angle_alpha 92.660(3) _cell_angle_beta 102.016(4) _cell_angle_gamma 102.569(4) _cell_volume 2075.84(15) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4868 _cell_measurement_theta_min 4.0636 _cell_measurement_theta_max 76.4313 _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 2.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.73533 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12165 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 67.99 _reflns_number_total 7496 _reflns_number_gt 4849 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The disordered atoms were divided into two groups each representing one component of the disorder. To make the anisotropic displacement parameters behave 'reasonably', the 'similar Uij' restraints were applied. Geometrical restraints were applied to 'correct' the bond lengths and angles. Since the disordered lattice solvent could not be unambiguously modeled, the PLATON SQUEEZE option was utilized. Details from SQUEEZE are given below. Note: Data are Listed for all Voids in the P1 Unit Cell i.e. Centre of Gravity, Solvent Accessible Volume, Recovered number of Electrons in the Void and Details about the Squeezed Material ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 300 101 . _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^)+(0.1000P)^2^+8.0000P] 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 7496 _refine_ls_number_parameters 569 _refine_ls_number_restraints 749 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.1133 _refine_ls_wR_factor_ref 0.2866 _refine_ls_wR_factor_gt 0.2674 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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 K1 K -0.08134(17) 0.13194(10) 0.28467(8) 0.0526(4) Uani 1 1 d D . . O1 O 0.1069(8) 0.3002(4) 0.2366(3) 0.0852(18) Uani 1 1 d U A . O4 O 0.0188(7) -0.0488(4) 0.2905(3) 0.0743(14) Uani 1 1 d U . . O5 O -0.1839(8) 0.2670(5) 0.1713(4) 0.095(2) Uani 1 1 d U A . O8 O -0.2776(6) -0.0752(3) 0.2198(3) 0.0634(13) Uani 1 1 d U . . O9 O -0.0703(10) 0.0729(4) 0.1292(4) 0.1104(19) Uani 1 1 d U A . N1 N -0.3956(15) -0.0151(9) -0.1019(7) 0.138(3) Uani 1 1 d U . . C1 C 0.1915(8) 0.1341(4) -0.1906(4) 0.0508(14) Uani 1 1 d U . . C2 C 0.2558(8) 0.2045(4) -0.1259(4) 0.0519(14) Uani 1 1 d U . . H2A H 0.3597 0.2140 -0.1017 0.062 Uiso 1 1 calc R . . C3 C 0.1687(8) 0.2617(4) -0.0959(3) 0.0491(14) Uani 1 1 d U . . C4 C 0.2267(8) 0.3472(4) -0.0282(4) 0.0547(16) Uani 1 1 d U A . C5 C 0.1233(9) 0.3251(4) 0.0295(4) 0.0541(16) Uani 1 1 d U . . C6 C 0.1698(9) 0.3252(5) 0.1099(4) 0.0619(18) Uani 1 1 d U A . H6A H 0.2745 0.3382 0.1332 0.074 Uiso 1 1 calc R . . C7 C 0.0679(10) 0.3068(5) 0.1566(4) 0.0628(19) Uani 1 1 d U . . C8 C -0.0868(10) 0.2900(5) 0.1220(4) 0.064(2) Uani 1 1 d U A . C9 C -0.1341(9) 0.2905(5) 0.0413(4) 0.0565(16) Uani 1 1 d U . . H9A H -0.2385 0.2781 0.0177 0.068 Uiso 1 1 calc R A . C10 C -0.0278(9) 0.3093(4) -0.0052(4) 0.0527(15) Uani 1 1 d U A . C11 C -0.0652(9) 0.3182(5) -0.0944(4) 0.0569(16) Uani 1 1 d U . . C12 C 0.0162(8) 0.2470(4) -0.1306(3) 0.0522(15) Uani 1 1 d U A . C13 C -0.0493(8) 0.1771(5) -0.1962(4) 0.0535(15) Uani 1 1 d U . . H13A H -0.1532 0.1672 -0.2202 0.064 Uiso 1 1 calc R A . C14 C 0.0406(8) 0.1213(4) -0.2265(4) 0.0534(15) Uani 1 1 d U . . C15 C 0.1920(9) 0.4442(5) -0.0656(4) 0.0649(19) Uani 1 1 d U . . H15A H 0.2226 0.5026 -0.0244 0.078 Uiso 1 1 calc R A . H15B H 0.2515 0.4609 -0.1062 0.078 Uiso 1 1 calc R . . C16 C 0.0269(10) 0.4286(5) -0.1030(4) 0.067(2) Uani 1 1 d U A . H16A H 0.0147 0.4392 -0.1597 0.080 Uiso 1 1 calc R . . H16B H -0.0144 0.4801 -0.0777 0.080 Uiso 1 1 calc R . . C17 C 0.3916(9) 0.3611(5) 0.0097(4) 0.072(2) Uani 1 1 d U . . H17A H 0.4083 0.2981 0.0323 0.107 Uiso 1 1 calc R A . H17B H 0.4221 0.4176 0.0516 0.107 Uiso 1 1 calc R . . H17C H 0.4515 0.3765 -0.0302 0.107 Uiso 1 1 calc R . . C18 C -0.2301(9) 0.3015(6) -0.1318(4) 0.068(2) Uani 1 1 d U A . H18A H -0.2824 0.2322 -0.1248 0.102 Uiso 1 1 calc R . . H18B H -0.2428 0.3100 -0.1883 0.102 Uiso 1 1 calc R . . H18C H -0.2726 0.3514 -0.1067 0.102 Uiso 1 1 calc R . . C31 C -0.3232(18) 0.0198(9) -0.0184(8) 0.131(3) Uani 1 1 d U . . H31A H -0.3702 0.0438 0.0199 0.157 Uiso 1 1 calc R . . C32 C -0.1509(15) 0.0102(7) -0.0033(6) 0.099(2) Uani 1 1 d U . . C33 C -0.0363(14) 0.0405(6) 0.0707(5) 0.089(2) Uani 1 1 d U . . C34 C 0.1150(14) 0.0287(6) 0.0692(6) 0.095(2) Uani 1 1 d U . . C35 C 0.2063(18) 0.0633(9) 0.1443(8) 0.121(3) Uani 1 1 d U . . H35A H 0.1727 0.0949 0.1850 0.146 Uiso 1 1 calc R A . C36 C 0.3345(19) 0.0488(10) 0.1528(9) 0.126(3) Uani 1 1 d U . . H36A H 0.3958 0.0651 0.2047 0.151 Uiso 1 1 calc R . . P1 P 0.3370(4) 0.7026(2) 0.40790(15) 0.0940(8) Uani 1 1 d U . . F1 F 0.3908(10) 0.8127(6) 0.4478(4) 0.152(3) Uani 1 1 d U . . F2 F 0.2934(12) 0.7520(7) 0.3299(4) 0.173(4) Uani 1 1 d U . . F3 F 0.1857(10) 0.7008(8) 0.4273(8) 0.201(5) Uani 1 1 d U . . F4 F 0.5020(12) 0.7203(8) 0.3875(6) 0.184(4) Uani 1 1 d U . . F5 F 0.2942(17) 0.5983(7) 0.3665(8) 0.251(6) Uani 1 1 d U . . F6 F 0.3874(14) 0.6571(9) 0.4847(6) 0.212(5) Uani 1 1 d U . . C26 C -0.3755(11) 0.2795(7) 0.2353(6) 0.087(3) Uani 1 1 d U . . H26A H -0.3862 0.3264 0.2758 0.105 Uiso 1 1 d R A . H26B H -0.4684 0.2631 0.1961 0.105 Uiso 1 1 d R . . C27 C -0.4234(12) 0.1782(7) 0.3368(5) 0.091(3) Uani 1 1 d U . . H27A H -0.4062 0.2432 0.3666 0.109 Uiso 1 1 d R A . H27B H -0.5305 0.1523 0.3201 0.109 Uiso 1 1 d R . . C28 C -0.3857(16) 0.1073(7) 0.3852(7) 0.131(5) Uani 1 1 d DU A . H28A H -0.4642 0.0746 0.4098 0.157 Uiso 1 1 d R . . H28B H -0.3071 0.1482 0.4264 0.157 Uiso 1 1 d R . . C29 C -0.4235(9) -0.0485(6) 0.3118(5) 0.070(2) Uani 1 1 d U . . H29A H -0.4847 -0.0815 0.3455 0.084 Uiso 1 1 d R A . H29B H -0.4853 -0.0199 0.2716 0.084 Uiso 1 1 d R . . C30 C -0.3549(9) -0.1220(5) 0.2742(5) 0.072(2) Uani 1 1 d U A . H30A H -0.2843 -0.1470 0.3153 0.086 Uiso 1 1 calc R . . H30B H -0.4348 -0.1816 0.2470 0.086 Uiso 1 1 calc R . . O2 O 0.2261(19) 0.2541(10) 0.3792(7) 0.094(2) Uani 0.454(8) 1 d PU A 1 O3 O 0.125(2) 0.0817(12) 0.4183(10) 0.095(2) Uani 0.454(8) 1 d PDU A 1 O6 O -0.363(2) 0.1939(15) 0.2628(9) 0.075(4) Uani 0.454(8) 1 d PU A 1 O7 O -0.3095(7) 0.0341(4) 0.3527(3) 0.0789(16) Uani 1 1 d U A 1 C19 C 0.157(4) 0.384(2) 0.2879(16) 0.089(5) Uani 0.454(8) 1 d PU A 1 H19A H 0.0717 0.4071 0.3028 0.107 Uiso 0.454(8) 1 calc PR A 1 H19B H 0.2165 0.4404 0.2649 0.107 Uiso 0.454(8) 1 calc PR A 1 C20 C 0.255(3) 0.3520(15) 0.3592(12) 0.090(4) Uani 0.454(8) 1 d PDU A 1 H20A H 0.3595 0.3681 0.3515 0.109 Uiso 0.454(8) 1 calc PR A 1 H20B H 0.2540 0.3969 0.4056 0.109 Uiso 0.454(8) 1 calc PR A 1 C21 C 0.246(3) 0.2607(13) 0.4547(10) 0.099(3) Uani 0.454(8) 1 d PDU A 1 H21A H 0.1802 0.3008 0.4725 0.119 Uiso 0.454(8) 1 calc PR A 1 H21B H 0.3526 0.2937 0.4799 0.119 Uiso 0.454(8) 1 calc PR A 1 C22 C 0.2092(14) 0.1584(7) 0.4735(5) 0.1038(19) Uani 0.454(8) 1 d PDU A 1 H22A H 0.3053 0.1392 0.4949 0.125 Uiso 0.454(8) 1 calc PR A 1 H22B H 0.1563 0.1584 0.5173 0.125 Uiso 0.454(8) 1 calc PR A 1 C23 C 0.108(3) -0.0232(13) 0.4271(9) 0.089(3) Uani 0.454(8) 1 d PDU A 1 H23A H 0.0057 -0.0551 0.4344 0.107 Uiso 0.454(8) 1 calc PR A 1 H23B H 0.1846 -0.0361 0.4716 0.107 Uiso 0.454(8) 1 calc PR A 1 C24 C 0.132(3) -0.0605(16) 0.3457(10) 0.081(3) Uani 0.454(8) 1 d PDU A 1 H24A H 0.2281 -0.0200 0.3367 0.098 Uiso 0.454(8) 1 calc PR A 1 H24D H 0.1364 -0.1333 0.3447 0.098 Uiso 0.454(8) 1 calc PR A 1 C25 C -0.257(2) 0.3287(12) 0.1992(10) 0.060(4) Uani 0.454(8) 1 d PU A 1 H25A H -0.3012 0.3650 0.1554 0.072 Uiso 0.454(8) 1 calc PR A 1 H25D H -0.1840 0.3807 0.2387 0.072 Uiso 0.454(8) 1 calc PR A 1 O2' O 0.0934(14) 0.2931(7) 0.3932(5) 0.085(2) Uani 0.546(8) 1 d PDU A 2 O3' O 0.0796(19) 0.0800(11) 0.4311(8) 0.087(2) Uani 0.546(8) 1 d PU A 2 O6' O -0.310(2) 0.2224(14) 0.3007(9) 0.097(5) Uani 0.546(8) 1 d PU A 2 C19' C 0.223(3) 0.3625(17) 0.2816(10) 0.110(8) Uani 0.546(8) 1 d PDU A 2 H19C H 0.2339 0.4318 0.2634 0.132 Uiso 0.546(8) 1 calc PR A 2 H19D H 0.3159 0.3392 0.2791 0.132 Uiso 0.546(8) 1 calc PR A 2 C20' C 0.201(2) 0.3656(14) 0.3698(9) 0.098(3) Uani 0.546(8) 1 d PDU A 2 H20C H 0.2994 0.3645 0.4044 0.117 Uiso 0.546(8) 1 calc PR A 2 H20D H 0.1808 0.4330 0.3822 0.117 Uiso 0.546(8) 1 calc PR A 2 C21' C 0.145(2) 0.2585(11) 0.4702(7) 0.097(3) Uani 0.546(8) 1 d PDU A 2 H21C H 0.0591 0.2470 0.4967 0.117 Uiso 0.546(8) 1 calc PR A 2 H21D H 0.2241 0.3151 0.5020 0.117 Uiso 0.546(8) 1 calc PR A 2 C22' C 0.2092(14) 0.1584(7) 0.4735(5) 0.1038(19) Uani 0.546(8) 1 d PDU A 2 H22C H 0.2944 0.1650 0.4469 0.125 Uiso 0.546(8) 1 calc PR A 2 H22D H 0.2426 0.1433 0.5287 0.125 Uiso 0.546(8) 1 calc PR A 2 C23' C 0.169(2) 0.0091(13) 0.4215(10) 0.092(3) Uani 0.546(8) 1 d PDU A 2 H23C H 0.2086 -0.0141 0.4732 0.110 Uiso 0.546(8) 1 calc PR A 2 H23D H 0.2563 0.0424 0.4000 0.110 Uiso 0.546(8) 1 calc PR A 2 C24' C 0.075(2) -0.0807(11) 0.3659(10) 0.089(3) Uani 0.546(8) 1 d PDU A 2 H24B H 0.1358 -0.1310 0.3597 0.107 Uiso 0.546(8) 1 calc PR A 2 H24C H -0.0110 -0.1145 0.3880 0.107 Uiso 0.546(8) 1 calc PR A 2 C25' C -0.310(2) 0.2779(14) 0.1524(10) 0.076(4) Uani 0.546(8) 1 d PU A 2 H25B H -0.3735 0.2208 0.1138 0.092 Uiso 0.546(8) 1 calc PR A 2 H25C H -0.3110 0.3429 0.1281 0.092 Uiso 0.546(8) 1 calc PR 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 K1 0.0703(9) 0.0436(7) 0.0488(7) 0.0091(5) 0.0203(6) 0.0158(6) O1 0.132(5) 0.066(3) 0.043(2) 0.000(2) 0.026(3) -0.014(3) O4 0.121(4) 0.058(2) 0.045(2) -0.0070(19) 0.006(2) 0.036(3) O5 0.141(6) 0.112(4) 0.090(4) 0.065(4) 0.082(4) 0.089(4) O8 0.093(4) 0.038(2) 0.071(3) 0.006(2) 0.040(3) 0.019(2) O9 0.203(5) 0.065(3) 0.083(3) 0.005(3) 0.084(4) 0.023(3) N1 0.172(7) 0.121(6) 0.118(6) -0.002(5) 0.042(6) 0.022(6) C1 0.076(4) 0.031(3) 0.052(3) 0.003(2) 0.026(3) 0.014(3) C2 0.067(4) 0.033(3) 0.058(4) 0.004(2) 0.025(3) 0.006(3) C3 0.076(4) 0.031(3) 0.045(3) 0.007(2) 0.026(3) 0.010(3) C4 0.081(5) 0.032(3) 0.054(3) 0.003(2) 0.032(3) 0.004(3) C5 0.088(5) 0.027(3) 0.049(3) 0.000(2) 0.028(3) 0.006(3) C6 0.089(5) 0.040(3) 0.050(3) 0.001(3) 0.023(3) -0.004(3) C7 0.106(6) 0.036(3) 0.050(3) 0.002(3) 0.034(4) 0.009(3) C8 0.115(6) 0.042(3) 0.059(4) 0.020(3) 0.049(4) 0.038(4) C9 0.088(5) 0.044(3) 0.054(4) 0.017(3) 0.032(3) 0.033(3) C10 0.090(5) 0.029(3) 0.048(3) 0.007(2) 0.031(3) 0.018(3) C11 0.092(5) 0.045(3) 0.048(3) 0.011(3) 0.032(3) 0.030(3) C12 0.089(5) 0.034(3) 0.043(3) 0.007(2) 0.027(3) 0.020(3) C13 0.072(4) 0.048(3) 0.045(3) 0.009(3) 0.016(3) 0.022(3) C14 0.088(5) 0.034(3) 0.042(3) 0.003(2) 0.019(3) 0.018(3) C15 0.103(6) 0.033(3) 0.068(4) 0.004(3) 0.046(4) 0.009(3) C16 0.123(7) 0.042(3) 0.058(4) 0.018(3) 0.049(4) 0.034(4) C17 0.093(6) 0.049(4) 0.066(4) -0.005(3) 0.030(4) -0.007(4) C18 0.097(6) 0.072(5) 0.054(4) 0.016(3) 0.032(4) 0.045(4) C31 0.188(7) 0.089(5) 0.120(6) 0.007(5) 0.053(6) 0.024(5) C32 0.157(6) 0.058(3) 0.096(4) 0.013(3) 0.055(4) 0.029(4) C33 0.172(5) 0.046(3) 0.071(3) 0.012(3) 0.073(4) 0.026(4) C34 0.166(6) 0.053(3) 0.075(4) 0.018(3) 0.046(4) 0.019(4) C35 0.184(6) 0.082(4) 0.104(5) 0.010(4) 0.047(5) 0.029(5) C36 0.171(8) 0.103(6) 0.118(6) 0.002(5) 0.063(6) 0.034(6) P1 0.138(2) 0.0808(15) 0.0704(14) 0.0084(11) 0.0218(14) 0.0409(15) F1 0.190(8) 0.146(6) 0.112(5) -0.040(4) 0.057(5) 0.012(5) F2 0.257(11) 0.164(7) 0.092(5) 0.002(5) -0.015(6) 0.093(7) F3 0.115(6) 0.169(8) 0.297(13) 0.054(9) 0.035(7) -0.008(6) F4 0.219(10) 0.200(9) 0.201(9) 0.065(7) 0.133(8) 0.099(8) F5 0.394(18) 0.088(5) 0.254(13) -0.046(7) 0.067(12) 0.041(8) F6 0.275(12) 0.259(12) 0.166(8) 0.129(9) 0.084(8) 0.144(10) C26 0.104(6) 0.094(6) 0.097(6) 0.027(5) 0.052(5) 0.061(5) C27 0.131(8) 0.090(6) 0.085(6) 0.020(5) 0.071(6) 0.050(5) C28 0.236(13) 0.062(5) 0.141(9) 0.016(6) 0.133(9) 0.048(7) C29 0.079(5) 0.060(4) 0.085(5) 0.008(4) 0.039(4) 0.023(4) C30 0.081(5) 0.044(3) 0.101(6) 0.002(4) 0.048(5) 0.012(3) O2 0.138(5) 0.079(4) 0.046(4) -0.006(3) 0.003(4) 0.006(4) O3 0.136(5) 0.077(3) 0.056(4) -0.017(3) -0.009(4) 0.025(4) O6 0.094(10) 0.092(10) 0.065(9) 0.037(8) 0.058(8) 0.037(8) O7 0.113(4) 0.056(3) 0.080(3) 0.000(2) 0.055(3) 0.015(3) C19 0.133(9) 0.061(7) 0.056(7) 0.001(6) 0.016(7) -0.009(7) C20 0.135(9) 0.059(7) 0.058(7) -0.014(6) 0.019(7) -0.010(7) C21 0.139(5) 0.086(4) 0.051(4) -0.016(4) 0.002(4) 0.007(4) C22 0.143(4) 0.093(3) 0.053(3) -0.007(3) -0.004(3) 0.008(3) C23 0.132(5) 0.075(4) 0.050(4) -0.001(4) -0.005(4) 0.029(4) C24 0.128(6) 0.066(5) 0.046(5) -0.003(4) 0.000(5) 0.033(5) C25 0.096(11) 0.050(8) 0.051(8) 0.020(6) 0.031(8) 0.036(8) O2' 0.138(5) 0.067(4) 0.036(3) -0.008(3) 0.007(4) 0.009(4) O3' 0.131(5) 0.077(3) 0.045(3) -0.013(3) 0.004(3) 0.021(4) O6' 0.158(14) 0.101(10) 0.077(9) 0.047(8) 0.070(9) 0.080(10) C19' 0.165(18) 0.065(11) 0.055(9) 0.012(8) -0.009(12) -0.040(12) C20' 0.145(7) 0.082(5) 0.044(5) -0.018(5) 0.011(5) -0.005(6) C21' 0.142(5) 0.083(4) 0.047(4) -0.011(4) 0.000(4) 0.008(4) C22' 0.143(4) 0.093(3) 0.053(3) -0.007(3) -0.004(3) 0.008(3) C23' 0.133(5) 0.077(4) 0.055(4) -0.003(4) -0.005(4) 0.028(4) C24' 0.133(6) 0.068(4) 0.056(4) 0.000(4) -0.007(4) 0.028(5) C25' 0.089(10) 0.084(10) 0.061(9) 0.024(8) 0.024(8) 0.020(8) _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 K1 O6' 2.735(17) . ? K1 O7 2.764(5) . ? K1 O2' 2.780(9) . ? K1 O4 2.789(5) . ? K1 O9 2.812(6) . ? K1 O1 2.823(5) . ? K1 O3' 2.874(15) . ? K1 O6 2.881(19) . ? K1 O3 2.900(19) . ? K1 O5 2.901(5) . ? K1 O8 3.005(5) . ? K1 O2 3.060(14) . ? O1 C19' 1.30(2) . ? O1 C19 1.34(3) . ? O1 C7 1.376(8) . ? O4 C24 1.31(2) . ? O4 C14 1.381(7) 2 ? O4 C24' 1.428(16) . ? O5 C25' 1.198(17) . ? O5 C25 1.320(15) . ? O5 C8 1.370(8) . ? O8 C1 1.393(7) 2 ? O8 C30 1.398(8) . ? O9 C33 1.217(9) . ? N1 C36 1.265(15) 2 ? N1 C31 1.476(16) . ? C1 C2 1.378(9) . ? C1 C14 1.385(10) . ? C1 O8 1.393(7) 2 ? C2 C3 1.392(9) . ? C3 C12 1.391(10) . ? C3 C4 1.530(8) . ? C4 C17 1.509(11) . ? C4 C5 1.528(8) . ? C4 C15 1.552(9) . ? C5 C6 1.374(9) . ? C5 C10 1.379(10) . ? C6 C7 1.365(10) . ? C7 C8 1.407(11) . ? C8 C9 1.381(10) . ? C9 C10 1.395(9) . ? C10 C11 1.535(8) . ? C11 C18 1.503(11) . ? C11 C12 1.534(8) . ? C11 C16 1.578(9) . ? C12 C13 1.385(9) . ? C13 C14 1.403(9) . ? C14 O4 1.381(7) 2 ? C15 C16 1.506(11) . ? C31 C32 1.608(18) . ? C32 C34 1.371(13) 2 ? C32 C33 1.468(15) . ? C33 C34 1.460(15) . ? C34 C32 1.371(13) 2 ? C34 C35 1.399(16) . ? C35 C36 1.233(18) . ? C36 N1 1.265(15) 2 ? P1 F5 1.481(8) . ? P1 F3 1.514(10) . ? P1 F6 1.522(8) . ? P1 F1 1.539(8) . ? P1 F2 1.556(8) . ? P1 F4 1.621(9) . ? C26 O6 1.29(2) . ? C26 C25 1.435(18) . ? C26 O6' 1.500(17) . ? C26 C25' 1.679(17) . ? C27 C28 1.358(14) . ? C27 O6' 1.38(2) . ? C27 O6 1.516(15) . ? C28 O7 1.489(10) . ? C29 O7 1.403(9) . ? C29 C30 1.486(9) . ? O2 C21 1.28(2) . ? O2 C20 1.36(2) . ? O3 C22 1.359(15) . ? O3 C23 1.406(14) . ? C19 C20 1.52(4) . ? C21 C22 1.416(16) . ? C23 C24 1.558(18) . ? O2' C20' 1.381(15) . ? O2' C21' 1.459(14) . ? O3' C23' 1.43(2) . ? C19' C20' 1.590(18) . ? C23' C24' 1.500(16) . ? 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' K1 O7 59.6(4) . . ? O6' K1 O2' 83.4(5) . . ? O7 K1 O2' 106.6(3) . . ? O6' K1 O4 145.6(4) . . ? O7 K1 O4 86.77(17) . . ? O2' K1 O4 115.6(3) . . ? O6' K1 O9 116.1(4) . . ? O7 K1 O9 121.5(2) . . ? O2' K1 O9 131.8(3) . . ? O4 K1 O9 73.76(17) . . ? O6' K1 O1 98.1(4) . . ? O7 K1 O1 156.16(18) . . ? O2' K1 O1 58.9(2) . . ? O4 K1 O1 116.1(2) . . ? O9 K1 O1 74.26(17) . . ? O6' K1 O3' 113.7(4) . . ? O7 K1 O3' 76.9(3) . . ? O2' K1 O3' 63.0(3) . . ? O4 K1 O3' 59.5(3) . . ? O9 K1 O3' 129.2(3) . . ? O1 K1 O3' 108.1(3) . . ? O6' K1 O6 15.3(4) . . ? O7 K1 O6 59.2(3) . . ? O2' K1 O6 98.0(5) . . ? O4 K1 O6 138.3(4) . . ? O9 K1 O6 102.5(4) . . ? O1 K1 O6 101.9(4) . . ? O3' K1 O6 125.1(4) . . ? O6' K1 O3 122.9(5) . . ? O7 K1 O3 86.3(4) . . ? O2' K1 O3 63.0(4) . . ? O4 K1 O3 55.3(3) . . ? O9 K1 O3 120.7(4) . . ? O1 K1 O3 101.1(4) . . ? O3' K1 O3 10.2(5) . . ? O6 K1 O3 135.1(5) . . ? O6' K1 O5 59.1(3) . . ? O7 K1 O5 111.85(19) . . ? O2' K1 O5 93.1(3) . . ? O4 K1 O5 140.27(16) . . ? O9 K1 O5 66.56(18) . . ? O1 K1 O5 55.0(2) . . ? O3' K1 O5 156.2(3) . . ? O6 K1 O5 53.7(3) . . ? O3 K1 O5 154.0(4) . . ? O6' K1 O8 96.3(4) . . ? O7 K1 O8 57.57(14) . . ? O2' K1 O8 160.1(2) . . ? O4 K1 O8 55.83(16) . . ? O9 K1 O8 66.07(16) . . ? O1 K1 O8 140.21(14) . . ? O3' K1 O8 99.5(3) . . ? O6 K1 O8 84.2(4) . . ? O3 K1 O8 101.6(3) . . ? O5 K1 O8 103.9(2) . . ? O6' K1 O2 112.6(5) . . ? O7 K1 O2 123.8(3) . . ? O2' K1 O2 29.4(4) . . ? O4 K1 O2 91.2(3) . . ? O9 K1 O2 111.5(3) . . ? O1 K1 O2 53.5(3) . . ? O3' K1 O2 54.8(4) . . ? O6 K1 O2 126.7(5) . . ? O3 K1 O2 49.3(4) . . ? O5 K1 O2 104.8(3) . . ? O8 K1 O2 146.8(3) . . ? C19' O1 C19 33.6(17) . . ? C19' O1 C7 121.7(9) . . ? C19 O1 C7 121.3(13) . . ? C19' O1 K1 126.0(9) . . ? C19 O1 K1 116.3(13) . . ? C7 O1 K1 112.2(4) . . ? C24 O4 C14 120.0(9) . 2 ? C24 O4 C24' 29.7(12) . . ? C14 O4 C24' 119.2(7) 2 . ? C24 O4 K1 122.3(9) . . ? C14 O4 K1 117.1(4) 2 . ? C24' O4 K1 118.7(7) . . ? C25' O5 C25 46.7(10) . . ? C25' O5 C8 120.3(9) . . ? C25 O5 C8 126.8(8) . . ? C25' O5 K1 125.7(8) . . ? C25 O5 K1 113.1(7) . . ? C8 O5 K1 110.6(4) . . ? C1 O8 C30 113.9(5) 2 . ? C1 O8 K1 109.2(4) 2 . ? C30 O8 K1 112.4(4) . . ? C33 O9 K1 164.9(8) . . ? C36 N1 C31 126.2(15) 2 . ? C2 C1 C14 120.0(6) . . ? C2 C1 O8 120.2(6) . 2 ? C14 C1 O8 119.9(5) . 2 ? C1 C2 C3 120.0(7) . . ? C12 C3 C2 120.1(6) . . ? C12 C3 C4 114.2(5) . . ? C2 C3 C4 125.7(6) . . ? C17 C4 C5 113.7(6) . . ? C17 C4 C3 113.5(6) . . ? C5 C4 C3 106.9(5) . . ? C17 C4 C15 112.3(6) . . ? C5 C4 C15 104.9(5) . . ? C3 C4 C15 104.7(5) . . ? C6 C5 C10 120.3(6) . . ? C6 C5 C4 125.6(7) . . ? C10 C5 C4 114.0(6) . . ? C7 C6 C5 121.0(8) . . ? C6 C7 O1 123.7(8) . . ? C6 C7 C8 119.3(7) . . ? O1 C7 C8 116.9(6) . . ? O5 C8 C9 123.3(8) . . ? O5 C8 C7 116.6(7) . . ? C9 C8 C7 119.9(6) . . ? C8 C9 C10 119.7(7) . . ? C5 C10 C9 119.7(6) . . ? C5 C10 C11 115.5(6) . . ? C9 C10 C11 124.7(7) . . ? C18 C11 C12 114.7(6) . . ? C18 C11 C10 115.3(6) . . ? C12 C11 C10 105.8(5) . . ? C18 C11 C16 112.5(6) . . ? C12 C11 C16 103.7(5) . . ? C10 C11 C16 103.7(5) . . ? C13 C12 C3 120.4(6) . . ? C13 C12 C11 124.6(7) . . ? C3 C12 C11 114.9(6) . . ? C12 C13 C14 118.8(7) . . ? O4 C14 C1 117.7(6) 2 . ? O4 C14 C13 121.6(7) 2 . ? C1 C14 C13 120.7(6) . . ? C16 C15 C4 111.4(5) . . ? C15 C16 C11 111.9(5) . . ? N1 C31 C32 108.2(11) . . ? C34 C32 C33 120.5(11) 2 . ? C34 C32 C31 113.1(11) 2 . ? C33 C32 C31 126.5(9) . . ? O9 C33 C34 123.6(11) . . ? O9 C33 C32 119.8(11) . . ? C34 C33 C32 116.6(8) . . ? C32 C34 C35 129.7(13) 2 . ? C32 C34 C33 122.9(11) 2 . ? C35 C34 C33 107.4(10) . . ? C36 C35 C34 113.7(14) . . ? C35 C36 N1 128.9(17) . 2 ? F5 P1 F3 96.2(8) . . ? F5 P1 F6 88.8(7) . . ? F3 P1 F6 90.3(6) . . ? F5 P1 F1 175.9(7) . . ? F3 P1 F1 87.6(5) . . ? F6 P1 F1 92.7(6) . . ? F5 P1 F2 92.5(6) . . ? F3 P1 F2 91.9(6) . . ? F6 P1 F2 177.3(7) . . ? F1 P1 F2 85.8(5) . . ? F5 P1 F4 90.4(7) . . ? F3 P1 F4 172.6(6) . . ? F6 P1 F4 93.1(6) . . ? F1 P1 F4 85.6(5) . . ? F2 P1 F4 84.5(6) . . ? O6 C26 C25 116.2(11) . . ? O6 C26 O6' 30.5(10) . . ? C25 C26 O6' 108.9(12) . . ? O6 C26 C25' 104.5(10) . . ? C25 C26 C25' 36.6(9) . . ? O6' C26 C25' 117.5(10) . . ? C28 C27 O6' 113.4(11) . . ? C28 C27 O6 120.9(10) . . ? O6' C27 O6 30.1(9) . . ? C27 C28 O7 115.5(8) . . ? O7 C29 C30 109.5(6) . . ? O8 C30 C29 110.4(6) . . ? C21 O2 C20 106.2(13) . . ? C21 O2 K1 116.8(15) . . ? C20 O2 K1 110.9(13) . . ? C22 O3 C23 125.0(17) . . ? C22 O3 K1 118.5(11) . . ? C23 O3 K1 115.3(11) . . ? C26 O6 C27 112.7(13) . . ? C26 O6 K1 120.9(10) . . ? C27 O6 K1 108.8(10) . . ? C29 O7 C28 106.9(8) . . ? C29 O7 K1 121.5(4) . . ? C28 O7 K1 112.0(5) . . ? O1 C19 C20 105(2) . . ? O2 C20 C19 121(2) . . ? O2 C21 C22 105.0(14) . . ? O3 C22 C21 121.5(13) . . ? O3 C23 C24 99.5(15) . . ? O4 C24 C23 108.2(16) . . ? O5 C25 C26 115.1(12) . . ? C20' O2' C21' 114.2(15) . . ? C20' O2' K1 119.1(8) . . ? C21' O2' K1 111.7(8) . . ? C23' O3' K1 113.8(10) . . ? C27 O6' C26 108.6(14) . . ? C27 O6' K1 122.4(10) . . ? C26 O6' K1 119.5(8) . . ? O1 C19' C20' 108.7(16) . . ? O2' C20' C19' 122.0(13) . . ? O3' C23' C24' 109.1(16) . . ? O4 C24' C23' 110.6(12) . . ? O5 C25' C26 106.6(12) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 67.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.010 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.093 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material #loop_ #_platon_squeeze_void_nr #_platon_squeeze_void_average_x #_platon_squeeze_void_average_y #_platon_squeeze_void_average_z #_platon_squeeze_void_volume #_platon_squeeze_void_count_electrons #_platon_squeeze_void_content #1 0.000 0.500 0.500 300 101 ' ' #_platon_squeeze_details #; #; data_ic14179 _database_code_depnum_ccdc_archive 'CCDC 786870' #TrackingRef 'ic14179-platon_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 O16, C12 H8 N2 O2, 2(C2 F3 O2)' _chemical_formula_sum 'C76 H84 F6 N2 O22' _chemical_formula_weight 1491.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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' F F 0.0727 0.0534 '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 12.3239(18) _cell_length_b 13.3177(18) _cell_length_c 13.939(2) _cell_angle_alpha 106.705(12) _cell_angle_beta 96.177(12) _cell_angle_gamma 93.527(12) _cell_volume 2168.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15458 _cell_measurement_theta_min 3.3298 _cell_measurement_theta_max 77.4413 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54024 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23756 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 68.00 _reflns_number_total 7889 _reflns_number_gt 7049 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _publ_section_exptl_refinement ; There is untreated twinning where overlap from the second twin domain in non-merohedral twins causes different in the intensities of some reflections. The R-factors will be larger. ; _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. To make the anisotropic displacement parameters behave 'reasonably', the 'similar Uij' restraints were applied. Geometrical restraints were also applied to 'correct' the bond lengths and angles. The residual electron density may be due to the inadequately corrected absorption and Fourier series truncation errors which often lead to accumulation of spurious electron density at special positions. Since the disordered lattice solvent could not be unambiguously modeled, the PLATON SQUEEZE option was utilized. Details from SQUEEZE are given below. Note: Data are Listed for all Voids in the P1 Unit Cell i.e. Centre of Gravity, Solvent Accessible Volume, Recovered number of Electrons in the Void and Details about the Squeezed Material ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 300 101 . _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^)+(0.1000P)^2^+11.0000P] 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 7889 _refine_ls_number_parameters 542 _refine_ls_number_restraints 213 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.1290 _refine_ls_wR_factor_ref 0.3262 _refine_ls_wR_factor_gt 0.3204 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.292 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.1322(3) -0.2410(3) 0.1708(3) 0.0277(8) Uani 1 1 d . . . O2 O 0.2727(3) -0.3609(3) 0.2551(3) 0.0341(9) Uani 1 1 d . . . O3 O 0.3890(3) -0.4041(3) 0.4241(3) 0.0399(10) Uani 1 1 d . . . O4 O 0.2250(3) -0.3574(3) 0.5482(3) 0.0326(8) Uani 1 1 d . . . O5 O -0.0759(3) -0.2792(3) 0.1232(3) 0.0321(8) Uani 1 1 d . . . O6 O -0.1389(3) -0.4868(3) 0.0291(3) 0.0353(9) Uani 1 1 d . . . O7 O -0.0237(3) -0.4379(3) 0.2517(3) 0.0308(8) Uani 1 1 d . . . O8 O 0.0275(3) -0.3939(3) 0.4611(3) 0.0303(8) Uani 1 1 d . . . C1 C 0.0761(4) -0.1540(4) 0.1725(4) 0.0250(10) Uani 1 1 d . . . C2 C 0.1237(4) -0.0506(4) 0.2046(4) 0.0258(10) Uani 1 1 d . . . H2A H 0.1995 -0.0351 0.2297 0.031 Uiso 1 1 calc R . . C3 C 0.0583(4) 0.0302(4) 0.1993(4) 0.0261(10) Uani 1 1 d . . . C4 C 0.0978(4) 0.1475(4) 0.2320(4) 0.0275(11) Uani 1 1 d . . . C5 C 0.0155(4) 0.2038(4) 0.2977(4) 0.0256(10) Uani 1 1 d . . . C6 C 0.0417(4) 0.2751(4) 0.3947(4) 0.0258(10) Uani 1 1 d . . . H6A H 0.1156 0.2903 0.4261 0.031 Uiso 1 1 calc R . . C7 C -0.0418(4) 0.3231(4) 0.4442(4) 0.0261(10) Uani 1 1 d . . . C8 C -0.1505(4) 0.3012(4) 0.3971(4) 0.0275(11) Uani 1 1 d . . . C9 C -0.1766(4) 0.2300(4) 0.3019(4) 0.0276(11) Uani 1 1 d . . . H9A H -0.2505 0.2147 0.2706 0.033 Uiso 1 1 calc R . . C10 C -0.0928(4) 0.1810(4) 0.2528(4) 0.0266(11) Uani 1 1 d . . . C11 C -0.1096(4) 0.1023(4) 0.1480(4) 0.0281(11) Uani 1 1 d . . . C12 C -0.0517(4) 0.0069(4) 0.1595(4) 0.0251(10) Uani 1 1 d . . . C13 C -0.1011(4) -0.0956(4) 0.1331(4) 0.0271(11) Uani 1 1 d . . . H13A H -0.1773 -0.1107 0.1094 0.032 Uiso 1 1 calc R . . C14 C -0.0368(4) -0.1764(4) 0.1420(4) 0.0250(10) Uani 1 1 d . . . C15 C 0.0794(5) 0.1808(4) 0.1330(4) 0.0330(12) Uani 1 1 d . . . H15A H 0.0976 0.2578 0.1492 0.040 Uiso 1 1 calc R . . H15B H 0.1287 0.1452 0.0852 0.040 Uiso 1 1 calc R . . C16 C -0.0404(5) 0.1515(4) 0.0831(4) 0.0332(12) Uani 1 1 d . . . H16A H -0.0426 0.1006 0.0151 0.040 Uiso 1 1 calc R . . H16B H -0.0723 0.2154 0.0748 0.040 Uiso 1 1 calc R . . C17 C 0.2167(4) 0.1731(4) 0.2807(5) 0.0356(13) Uani 1 1 d . . . H17A H 0.2255 0.1515 0.3424 0.053 Uiso 1 1 calc R . . H17B H 0.2369 0.2490 0.2976 0.053 Uiso 1 1 calc R . . H17C H 0.2643 0.1351 0.2335 0.053 Uiso 1 1 calc R . . C18 C -0.2278(5) 0.0759(4) 0.0985(4) 0.0341(12) Uani 1 1 d . . . H18A H -0.2706 0.0448 0.1399 0.051 Uiso 1 1 calc R . . H18B H -0.2306 0.0256 0.0311 0.051 Uiso 1 1 calc R . . H18C H -0.2584 0.1404 0.0925 0.051 Uiso 1 1 calc R . . C19 C 0.2484(4) -0.2271(4) 0.1739(4) 0.0330(12) Uani 1 1 d . . . H19A H 0.2815 -0.1742 0.2377 0.040 Uiso 1 1 calc R . . H19B H 0.2674 -0.2024 0.1166 0.040 Uiso 1 1 calc R . . C20 C 0.2908(4) -0.3330(4) 0.1668(4) 0.0320(12) Uani 1 1 d . . . H20A H 0.2520 -0.3870 0.1063 0.038 Uiso 1 1 calc R . . H20B H 0.3701 -0.3291 0.1607 0.038 Uiso 1 1 calc R . . C21 C 0.3095(5) -0.4608(4) 0.2531(4) 0.0334(12) Uani 1 1 d . . . H21A H 0.3850 -0.4637 0.2353 0.040 Uiso 1 1 calc R . . H21B H 0.2614 -0.5174 0.2013 0.040 Uiso 1 1 calc R . . C22 C 0.3071(5) -0.4770(5) 0.3544(4) 0.0375(13) Uani 1 1 d . . . H22A H 0.2340 -0.4652 0.3763 0.045 Uiso 1 1 calc R . . H22B H 0.3219 -0.5500 0.3512 0.045 Uiso 1 1 calc R . . C23 C 0.3990(5) -0.4154(5) 0.5234(4) 0.0430(15) Uani 1 1 d . . . H23A H 0.4774 -0.4050 0.5518 0.052 Uiso 1 1 calc R . . H23B H 0.3705 -0.4878 0.5196 0.052 Uiso 1 1 calc R . . C24 C 0.3374(4) -0.3378(5) 0.5921(4) 0.0355(12) Uani 1 1 d . . . H24A H 0.3451 -0.3473 0.6603 0.043 Uiso 1 1 calc R . . H24B H 0.3660 -0.2649 0.5981 0.043 Uiso 1 1 calc R . . C25 C -0.1881(4) -0.3107(4) 0.0824(4) 0.0326(12) Uani 1 1 d . . . H25A H -0.2010 -0.3079 0.0119 0.039 Uiso 1 1 calc R . . H25B H -0.2363 -0.2636 0.1230 0.039 Uiso 1 1 calc R . . C26 C -0.2110(5) -0.4217(4) 0.0861(5) 0.0353(12) Uani 1 1 d . . . H26A H -0.1998 -0.4233 0.1571 0.042 Uiso 1 1 calc R . . H26B H -0.2880 -0.4481 0.0578 0.042 Uiso 1 1 calc R . . C27 C -0.0878(5) -0.5563(4) 0.0775(4) 0.0329(12) Uani 1 1 d . . . H27A H -0.0597 -0.6129 0.0259 0.039 Uiso 1 1 calc R . . H27B H -0.1438 -0.5897 0.1075 0.039 Uiso 1 1 calc R . . C28 C 0.0057(5) -0.5024(4) 0.1594(4) 0.0325(12) Uani 1 1 d . . . H28A H 0.0491 -0.5574 0.1747 0.039 Uiso 1 1 calc R . . H28B H 0.0541 -0.4583 0.1321 0.039 Uiso 1 1 calc R . . C29 C -0.0742(5) -0.4976(4) 0.3080(4) 0.0323(12) Uani 1 1 d . . . H29A H -0.0299 -0.5556 0.3138 0.039 Uiso 1 1 calc R . . H29B H -0.1483 -0.5286 0.2735 0.039 Uiso 1 1 calc R . . C30 C -0.0818(4) -0.4244(4) 0.4110(4) 0.0312(11) Uani 1 1 d . . . H30A H -0.1180 -0.3618 0.4051 0.037 Uiso 1 1 calc R . . H30B H -0.1251 -0.4605 0.4494 0.037 Uiso 1 1 calc R . . O9 O -0.1650(4) -0.1137(4) 0.3639(4) 0.0672(15) Uani 1 1 d . . . N1 N 0.1365(5) -0.2314(4) 0.3767(4) 0.0491(15) Uani 1 1 d . . . H1A H 0.1469 -0.2926 0.3350 0.059 Uiso 1 1 calc R . . C31 C -0.0910(5) -0.0623(5) 0.4248(5) 0.0404(14) Uani 1 1 d . . . C32 C 0.0190(5) -0.1015(4) 0.4345(4) 0.0331(12) Uani 1 1 d . . . C33 C 0.1055(5) -0.0430(4) 0.5055(4) 0.0352(12) Uani 1 1 d . . . C34 C 0.2076(6) -0.0824(6) 0.5091(5) 0.0472(15) Uani 1 1 d . . . H34A H 0.2669 -0.0433 0.5572 0.057 Uiso 1 1 calc R . . C35 C 0.2220(6) -0.1769(6) 0.4436(5) 0.0511(17) Uani 1 1 d . . . H35A H 0.2915 -0.2040 0.4451 0.061 Uiso 1 1 calc R . . C36 C 0.0365(6) -0.1981(4) 0.3697(4) 0.0402(14) Uani 1 1 d . . . H36A H -0.0213 -0.2397 0.3213 0.048 Uiso 1 1 calc R . . F1 F 0.4536(9) 0.7726(12) 0.8690(12) 0.104(4) Uani 0.463(5) 1 d PU . . F2 F 0.5966(11) 0.7847(14) 0.9716(14) 0.131(4) Uani 0.463(5) 1 d PDU . . F3 F 0.5835(11) 0.6971(12) 0.8409(13) 0.118(4) Uani 0.463(5) 1 d PDU . . O10 O 0.5312(8) 0.5952(10) 0.9779(12) 0.099(4) Uani 0.463(5) 1 d PDU . . O11 O 0.3751(10) 0.6474(16) 0.9420(14) 0.107(4) Uani 0.463(5) 1 d PU . . C37 C 0.5166(14) 0.725(2) 0.914(2) 0.100(4) Uani 0.463(5) 1 d PU . . C38 C 0.4735(13) 0.621(2) 0.9246(19) 0.096(4) Uani 0.463(5) 1 d PU . . F4 F 0.4250(5) -0.0142(7) 0.1868(5) 0.057(2) Uani 0.537(5) 1 d PU . . F5 F 0.5677(10) -0.0820(11) 0.2227(8) 0.108(3) Uani 0.537(5) 1 d PDU . . F6 F 0.5555(10) 0.0890(10) 0.2617(7) 0.121(4) Uani 0.537(5) 1 d PDU . . O12 O 0.5315(9) 0.0655(11) 0.4353(8) 0.084(3) Uani 0.537(5) 1 d PU . . O13 O 0.3674(5) -0.0190(6) 0.3588(5) 0.0367(17) Uani 0.537(5) 1 d PU . . C39 C 0.5047(9) 0.0051(12) 0.2589(7) 0.049(3) Uani 0.537(5) 1 d PU . . C40 C 0.4626(10) 0.0006(13) 0.3574(8) 0.056(3) Uani 0.537(5) 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0251(18) 0.0239(17) 0.0329(19) 0.0058(14) 0.0045(14) 0.0049(14) O2 0.039(2) 0.0299(19) 0.0315(19) 0.0025(15) 0.0076(16) 0.0150(16) O3 0.035(2) 0.051(2) 0.029(2) 0.0033(17) 0.0060(16) 0.0080(18) O4 0.0302(19) 0.035(2) 0.0282(19) -0.0017(15) 0.0105(15) 0.0077(15) O5 0.0282(19) 0.0235(18) 0.041(2) 0.0064(15) -0.0010(16) 0.0017(14) O6 0.047(2) 0.0288(19) 0.0256(19) 0.0024(15) 0.0018(16) 0.0050(16) O7 0.043(2) 0.0264(18) 0.0200(17) 0.0028(14) 0.0050(15) -0.0003(15) O8 0.034(2) 0.0330(19) 0.0200(17) 0.0003(14) 0.0059(14) 0.0053(15) C1 0.030(3) 0.026(2) 0.021(2) 0.0065(19) 0.0062(19) 0.007(2) C2 0.026(2) 0.028(3) 0.022(2) 0.0040(19) 0.0050(19) 0.003(2) C3 0.033(3) 0.023(2) 0.022(2) 0.0030(19) 0.009(2) 0.004(2) C4 0.032(3) 0.023(2) 0.027(3) 0.003(2) 0.010(2) 0.005(2) C5 0.030(3) 0.023(2) 0.024(2) 0.0051(19) 0.010(2) 0.005(2) C6 0.028(3) 0.024(2) 0.025(2) 0.006(2) 0.006(2) 0.0030(19) C7 0.034(3) 0.025(2) 0.019(2) 0.0042(19) 0.008(2) 0.002(2) C8 0.031(3) 0.027(2) 0.026(2) 0.006(2) 0.010(2) 0.009(2) C9 0.030(3) 0.027(3) 0.025(2) 0.005(2) 0.005(2) 0.006(2) C10 0.033(3) 0.024(2) 0.022(2) 0.005(2) 0.007(2) 0.006(2) C11 0.033(3) 0.028(3) 0.022(2) 0.004(2) 0.005(2) 0.008(2) C12 0.030(3) 0.025(2) 0.020(2) 0.0039(19) 0.0069(19) 0.007(2) C13 0.027(3) 0.029(3) 0.023(2) 0.003(2) 0.0030(19) 0.005(2) C14 0.028(3) 0.024(2) 0.022(2) 0.0050(19) 0.0027(19) 0.0018(19) C15 0.045(3) 0.027(3) 0.029(3) 0.007(2) 0.017(2) 0.005(2) C16 0.048(3) 0.029(3) 0.026(3) 0.009(2) 0.011(2) 0.012(2) C17 0.031(3) 0.026(3) 0.045(3) 0.001(2) 0.013(2) 0.001(2) C18 0.038(3) 0.032(3) 0.028(3) 0.003(2) -0.002(2) 0.013(2) C19 0.026(3) 0.031(3) 0.041(3) 0.009(2) 0.005(2) 0.003(2) C20 0.027(3) 0.034(3) 0.032(3) 0.004(2) 0.006(2) 0.008(2) C21 0.036(3) 0.028(3) 0.033(3) 0.001(2) 0.006(2) 0.013(2) C22 0.038(3) 0.035(3) 0.039(3) 0.007(2) 0.007(2) 0.009(2) C23 0.041(3) 0.056(4) 0.033(3) 0.009(3) 0.009(3) 0.024(3) C24 0.031(3) 0.044(3) 0.030(3) 0.006(2) 0.006(2) 0.014(2) C25 0.027(3) 0.030(3) 0.037(3) 0.007(2) -0.001(2) 0.002(2) C26 0.029(3) 0.031(3) 0.041(3) 0.005(2) 0.001(2) 0.002(2) C27 0.045(3) 0.022(2) 0.027(3) 0.002(2) 0.004(2) 0.003(2) C28 0.040(3) 0.031(3) 0.024(3) 0.003(2) 0.009(2) 0.006(2) C29 0.042(3) 0.029(3) 0.024(3) 0.006(2) 0.005(2) -0.002(2) C30 0.034(3) 0.031(3) 0.027(3) 0.007(2) 0.005(2) 0.000(2) O9 0.048(3) 0.061(3) 0.068(3) -0.015(3) -0.001(2) -0.004(2) N1 0.086(4) 0.037(3) 0.036(3) 0.015(2) 0.028(3) 0.034(3) C31 0.045(3) 0.033(3) 0.036(3) 0.000(2) 0.008(3) -0.001(3) C32 0.047(3) 0.025(3) 0.028(3) 0.005(2) 0.013(2) 0.004(2) C33 0.039(3) 0.033(3) 0.035(3) 0.007(2) 0.015(2) 0.006(2) C34 0.046(4) 0.055(4) 0.045(4) 0.018(3) 0.012(3) 0.015(3) C35 0.061(4) 0.062(4) 0.041(4) 0.021(3) 0.019(3) 0.032(4) C36 0.067(4) 0.028(3) 0.027(3) 0.007(2) 0.016(3) 0.006(3) F1 0.048(5) 0.146(8) 0.147(8) 0.086(7) 0.010(5) 0.036(5) F2 0.071(6) 0.170(9) 0.169(9) 0.092(8) -0.020(7) 0.016(7) F3 0.087(6) 0.142(8) 0.174(9) 0.105(7) 0.063(6) 0.030(6) O10 0.030(5) 0.184(9) 0.131(8) 0.116(7) 0.009(5) 0.043(6) O11 0.033(5) 0.168(10) 0.151(10) 0.092(8) 0.013(6) 0.018(6) C37 0.029(6) 0.160(9) 0.143(9) 0.092(8) 0.006(6) 0.043(6) C38 0.023(5) 0.174(9) 0.135(8) 0.108(7) 0.029(6) 0.020(6) F4 0.041(3) 0.105(5) 0.023(3) 0.021(3) -0.002(3) -0.017(3) F5 0.109(7) 0.168(8) 0.068(5) 0.050(6) 0.045(5) 0.052(6) F6 0.126(6) 0.146(7) 0.058(5) -0.004(5) 0.031(5) -0.101(6) O12 0.058(5) 0.136(8) 0.045(5) 0.016(5) 0.002(4) -0.027(6) O13 0.020(3) 0.059(4) 0.031(4) 0.015(3) 0.008(3) -0.010(3) C39 0.029(4) 0.097(6) 0.018(4) 0.019(4) 0.008(4) -0.024(5) C40 0.039(5) 0.112(7) 0.016(4) 0.018(5) 0.003(4) -0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.380(6) . ? O1 C19 1.428(6) . ? O2 C20 1.420(7) . ? O2 C21 1.425(6) . ? O3 C22 1.426(7) . ? O3 C23 1.428(7) . ? O4 C8 1.374(6) 2_556 ? O4 C24 1.429(7) . ? O5 C14 1.365(6) . ? O5 C25 1.426(6) . ? O6 C26 1.423(7) . ? O6 C27 1.431(7) . ? O7 C28 1.424(6) . ? O7 C29 1.428(6) . ? O8 C7 1.370(6) 2_556 ? O8 C30 1.427(6) . ? C1 C2 1.390(7) . ? C1 C14 1.398(7) . ? C2 C3 1.398(7) . ? C3 C12 1.389(7) . ? C3 C4 1.528(7) . ? C4 C17 1.522(7) . ? C4 C5 1.526(6) . ? C4 C15 1.565(7) . ? C5 C10 1.388(7) . ? C5 C6 1.401(7) . ? C6 C7 1.386(7) . ? C7 O8 1.370(6) 2_556 ? C7 C8 1.402(7) . ? C8 O4 1.374(6) 2_556 ? C8 C9 1.382(7) . ? C9 C10 1.392(7) . ? C10 C11 1.517(7) . ? C11 C18 1.517(7) . ? C11 C12 1.535(7) . ? C11 C16 1.554(7) . ? C12 C13 1.389(7) . ? C13 C14 1.400(7) . ? C15 C16 1.538(8) . ? C19 C20 1.514(7) . ? C21 C22 1.490(8) . ? C23 C24 1.498(7) . ? C25 C26 1.505(8) . ? C27 C28 1.513(7) . ? C29 C30 1.502(7) . ? O9 C31 1.201(8) . ? N1 C36 1.338(9) . ? N1 C35 1.347(10) . ? C31 C32 1.489(9) . ? C31 C33 1.493(8) 2_556 ? C32 C36 1.388(8) . ? C32 C33 1.396(8) . ? C33 C34 1.394(9) . ? C33 C31 1.493(8) 2_556 ? C34 C35 1.361(10) . ? F1 C37 1.26(2) . ? F2 C37 1.27(3) . ? F3 C37 1.37(3) . ? O10 C38 1.12(2) . ? O11 C38 1.31(2) . ? C37 C38 1.50(3) . ? F4 C39 1.284(12) . ? F5 C39 1.436(18) . ? F6 C39 1.235(16) . ? O12 C40 1.348(16) . ? O13 C40 1.189(13) . ? C39 C40 1.535(13) . ? 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 C1 O1 C19 116.7(4) . . ? C20 O2 C21 112.0(4) . . ? C22 O3 C23 113.7(5) . . ? C8 O4 C24 117.3(4) 2_556 . ? C14 O5 C25 118.8(4) . . ? C26 O6 C27 114.9(4) . . ? C28 O7 C29 112.7(4) . . ? C7 O8 C30 117.8(4) 2_556 . ? O1 C1 C2 124.7(4) . . ? O1 C1 C14 114.8(4) . . ? C2 C1 C14 120.5(5) . . ? C1 C2 C3 119.0(5) . . ? C12 C3 C2 120.3(5) . . ? C12 C3 C4 114.3(4) . . ? C2 C3 C4 125.4(5) . . ? C17 C4 C5 114.5(4) . . ? C17 C4 C3 114.0(4) . . ? C5 C4 C3 106.5(4) . . ? C17 C4 C15 111.5(4) . . ? C5 C4 C15 104.8(4) . . ? C3 C4 C15 104.8(4) . . ? C10 C5 C6 120.1(4) . . ? C10 C5 C4 114.3(4) . . ? C6 C5 C4 125.5(5) . . ? C7 C6 C5 119.1(5) . . ? O8 C7 C6 125.0(5) 2_556 . ? O8 C7 C8 114.7(4) 2_556 . ? C6 C7 C8 120.3(4) . . ? O4 C8 C9 124.5(5) 2_556 . ? O4 C8 C7 114.8(4) 2_556 . ? C9 C8 C7 120.7(5) . . ? C8 C9 C10 119.0(5) . . ? C5 C10 C9 120.8(5) . . ? C5 C10 C11 114.7(4) . . ? C9 C10 C11 124.5(5) . . ? C10 C11 C18 115.1(4) . . ? C10 C11 C12 105.2(4) . . ? C18 C11 C12 114.3(4) . . ? C10 C11 C16 105.7(4) . . ? C18 C11 C16 110.1(4) . . ? C12 C11 C16 105.5(4) . . ? C3 C12 C13 120.8(5) . . ? C3 C12 C11 114.2(4) . . ? C13 C12 C11 125.0(5) . . ? C12 C13 C14 118.9(5) . . ? O5 C14 C1 115.2(4) . . ? O5 C14 C13 124.8(4) . . ? C1 C14 C13 120.0(4) . . ? C16 C15 C4 110.8(4) . . ? C15 C16 C11 111.0(4) . . ? O1 C19 C20 107.1(4) . . ? O2 C20 C19 108.9(4) . . ? O2 C21 C22 109.4(4) . . ? O3 C22 C21 108.2(5) . . ? O3 C23 C24 111.7(5) . . ? O4 C24 C23 106.8(5) . . ? O5 C25 C26 106.3(4) . . ? O6 C26 C25 109.2(5) . . ? O6 C27 C28 113.8(4) . . ? O7 C28 C27 116.5(5) . . ? O7 C29 C30 107.8(4) . . ? O8 C30 C29 107.1(4) . . ? C36 N1 C35 123.9(5) . . ? O9 C31 C32 121.3(6) . . ? O9 C31 C33 121.6(6) . 2_556 ? C32 C31 C33 117.1(5) . 2_556 ? C36 C32 C33 119.1(6) . . ? C36 C32 C31 118.9(5) . . ? C33 C32 C31 121.9(5) . . ? C34 C33 C32 119.4(5) . . ? C34 C33 C31 119.6(6) . 2_556 ? C32 C33 C31 121.0(5) . 2_556 ? C35 C34 C33 119.8(7) . . ? N1 C35 C34 119.1(6) . . ? N1 C36 C32 118.7(6) . . ? F1 C37 F2 113(2) . . ? F1 C37 F3 96.1(18) . . ? F2 C37 F3 88.6(15) . . ? F1 C37 C38 118.4(19) . . ? F2 C37 C38 124.9(19) . . ? F3 C37 C38 104(2) . . ? O10 C38 O11 124(2) . . ? O10 C38 C37 110.9(19) . . ? O11 C38 C37 96.5(19) . . ? F6 C39 F4 107.2(12) . . ? F6 C39 F5 110.9(11) . . ? F4 C39 F5 101.2(10) . . ? F6 C39 C40 116.0(11) . . ? F4 C39 C40 110.6(8) . . ? F5 C39 C40 109.9(11) . . ? O13 C40 O12 124.6(11) . . ? O13 C40 C39 120.1(10) . . ? O12 C40 C39 108.1(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.648 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.172