# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl _database_code_depnum_ccdc_archive 'CCDC 915137' #TrackingRef 'web_deposit_cif_file_0_AmandaKing_1355176363.aek1052.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AEK1052 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H28 Cl0 Co F12 N6 P2' _chemical_formula_weight 833.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.462 _cell_length_b 12.501 _cell_length_c 13.164 _cell_angle_alpha 109.79 _cell_angle_beta 108.38 _cell_angle_gamma 90.82 _cell_volume 1668.6 _cell_formula_units_Z 2 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9069 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details SADBS _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 9548 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.38 _reflns_number_total 5362 _reflns_number_gt 4400 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP _computing_publication_material WinGX _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^)+(0.0527P)^2^+1.5764P] 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 5362 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4541(3) 0.1926(2) 0.7939(3) 0.0265(7) Uani 1 1 d . . . C2 C 0.4004(3) 0.1381(3) 0.8472(3) 0.0340(8) Uani 1 1 d . . . H2 H 0.3153 0.1145 0.8184 0.041 Uiso 1 1 calc R . . C3 C 0.4738(3) 0.1192(3) 0.9429(3) 0.0347(8) Uani 1 1 d . . . H3 H 0.4380 0.0849 0.9806 0.042 Uiso 1 1 calc R . . C4 C 0.5992(3) 0.1510(2) 0.9828(3) 0.0288(7) Uani 1 1 d . . . H4 H 0.6494 0.1378 1.0471 0.035 Uiso 1 1 calc R . . C5 C 0.6508(3) 0.2034(2) 0.9257(3) 0.0230(6) Uani 1 1 d . . . C6 C 0.8549(2) 0.1884(2) 0.6936(2) 0.0210(6) Uani 1 1 d . . . H6 H 0.8335 0.2188 0.6358 0.025 Uiso 1 1 calc R . . C7 C 0.9360(3) 0.1079(2) 0.6897(3) 0.0243(7) Uani 1 1 d . . . H7 H 0.9693 0.0851 0.6310 0.029 Uiso 1 1 calc R . . C8 C 0.9665(3) 0.0620(2) 0.7746(3) 0.0269(7) Uani 1 1 d . . . H8 H 1.0185 0.0054 0.7728 0.032 Uiso 1 1 calc R . . C9 C 0.9187(3) 0.1015(2) 0.8625(3) 0.0247(7) Uani 1 1 d . . . H9 H 0.9397 0.0724 0.9213 0.030 Uiso 1 1 calc R . . C10 C 0.8397(2) 0.1843(2) 0.8636(2) 0.0198(6) Uani 1 1 d . . . C11 C 0.7925(3) 0.2372(2) 0.9653(3) 0.0230(6) Uani 1 1 d . . . C12 C 0.8570(3) 0.1933(2) 1.0613(3) 0.0276(7) Uani 1 1 d . . . H12A H 0.8333 0.2312 1.1270 0.041 Uiso 1 1 calc R . . H12B H 0.9453 0.2091 1.0820 0.041 Uiso 1 1 calc R . . H12C H 0.8330 0.1120 1.0352 0.041 Uiso 1 1 calc R . . C13 C 0.8045(3) 0.5365(2) 0.9710(3) 0.0247(7) Uani 1 1 d . . . H13 H 0.7688 0.5730 0.9201 0.030 Uiso 1 1 calc R . . C14 C 0.8875(3) 0.6017(2) 1.0770(3) 0.0285(7) Uani 1 1 d . . . H14 H 0.9070 0.6804 1.0977 0.034 Uiso 1 1 calc R . . C15 C 0.9412(3) 0.5470(3) 1.1518(3) 0.0291(7) Uani 1 1 d . . . H15 H 0.9969 0.5885 1.2247 0.035 Uiso 1 1 calc R . . C16 C 0.9112(3) 0.4302(3) 1.1171(3) 0.0270(7) Uani 1 1 d . . . H16 H 0.9484 0.3920 1.1661 0.032 Uiso 1 1 calc R . . C17 C 0.8257(3) 0.3691(2) 1.0092(2) 0.0209(6) Uani 1 1 d . . . C18 C 0.5036(3) 0.5242(3) 0.7791(3) 0.0310(7) Uani 1 1 d . . . H18 H 0.5822 0.5657 0.8063 0.037 Uiso 1 1 calc R . . C19 C 0.4022(3) 0.5825(3) 0.7629(3) 0.0350(8) Uani 1 1 d . . . H19 H 0.4118 0.6611 0.7785 0.042 Uiso 1 1 calc R . . C20 C 0.2865(3) 0.5208(3) 0.7229(3) 0.0355(8) Uani 1 1 d . . . H20 H 0.2158 0.5570 0.7109 0.043 Uiso 1 1 calc R . . C21 C 0.2766(3) 0.4047(3) 0.7008(3) 0.0353(8) Uani 1 1 d . . . H21 H 0.1986 0.3622 0.6737 0.042 Uiso 1 1 calc R . . C22 C 0.3819(3) 0.3506(3) 0.7185(3) 0.0270(7) Uani 1 1 d . . . C23 C 0.3757(3) 0.2195(3) 0.6885(3) 0.0293(7) Uani 1 1 d . . . C24 C 0.2397(3) 0.1668(3) 0.6519(3) 0.0401(9) Uani 1 1 d . . . H24A H 0.1914 0.1787 0.5834 0.060 Uiso 1 1 calc R . . H24B H 0.2072 0.2028 0.7122 0.060 Uiso 1 1 calc R . . H24C H 0.2360 0.0860 0.6374 0.060 Uiso 1 1 calc R . . C25 C 0.5750(3) 0.1874(3) 0.5100(3) 0.0295(7) Uani 1 1 d . . . H25 H 0.6526 0.2207 0.5196 0.035 Uiso 1 1 calc R . . C26 C 0.5053(3) 0.1090(3) 0.4024(3) 0.0333(8) Uani 1 1 d . . . H26 H 0.5346 0.0907 0.3411 0.040 Uiso 1 1 calc R . . C27 C 0.3914(3) 0.0597(3) 0.3900(3) 0.0383(9) Uani 1 1 d . . . H27 H 0.3426 0.0053 0.3199 0.046 Uiso 1 1 calc R . . C28 C 0.3499(3) 0.0913(3) 0.4823(3) 0.0358(8) Uani 1 1 d . . . H28 H 0.2727 0.0584 0.4743 0.043 Uiso 1 1 calc R . . C29 C 0.4228(3) 0.1718(2) 0.5867(3) 0.0278(7) Uani 1 1 d . . . C30 C 0.7567(3) 0.4812(3) 0.6482(3) 0.0271(7) Uani 1 1 d . . . C31 C 0.7925(4) 0.5479(3) 0.5887(3) 0.0423(9) Uani 1 1 d . . . H31A H 0.8631 0.5207 0.5687 0.063 Uiso 1 1 calc R . . H31B H 0.8133 0.6273 0.6379 0.063 Uiso 1 1 calc R . . H31C H 0.7246 0.5398 0.5202 0.063 Uiso 1 1 calc R . . N1 N 0.5787(2) 0.22457(19) 0.8343(2) 0.0227(5) Uani 1 1 d . . . N2 N 0.8050(2) 0.22514(18) 0.7776(2) 0.0195(5) Uani 1 1 d . . . N3 N 0.7719(2) 0.42271(19) 0.9367(2) 0.0220(5) Uani 1 1 d . . . N4 N 0.4956(2) 0.4114(2) 0.7580(2) 0.0259(6) Uani 1 1 d . . . N5 N 0.5369(2) 0.21752(19) 0.6003(2) 0.0236(6) Uani 1 1 d . . . N6 N 0.7283(2) 0.4282(2) 0.6941(2) 0.0250(6) Uani 1 1 d . . . F1 F 0.93112(19) 0.32740(19) 0.3688(2) 0.0520(6) Uani 1 1 d . . . F2 F 0.9551(2) 0.30892(17) 0.53975(18) 0.0518(6) Uani 1 1 d . . . F3 F 0.7656(2) 0.27735(19) 0.4065(2) 0.0590(7) Uani 1 1 d . . . F4 F 0.8301(2) 0.14587(19) 0.27580(17) 0.0519(6) Uani 1 1 d . . . F5 F 0.8506(3) 0.12904(18) 0.44397(19) 0.0678(8) Uani 1 1 d . . . F6 F 1.0202(2) 0.1821(2) 0.4099(2) 0.0715(8) Uani 1 1 d . . . F7 F 0.8008(2) -0.15126(17) 0.7726(2) 0.0511(6) Uani 1 1 d . . . F8 F 0.8402(2) -0.10312(17) 0.9624(2) 0.0661(8) Uani 1 1 d . . . F9 F 0.64888(19) -0.09881(16) 0.84863(17) 0.0462(5) Uani 1 1 d . . . F10 F 0.83514(18) -0.28706(16) 0.8518(2) 0.0459(5) Uani 1 1 d . . . F11 F 0.6837(2) -0.23720(17) 0.92588(19) 0.0500(6) Uani 1 1 d . . . F12 F 0.64365(18) -0.28310(16) 0.73659(18) 0.0427(5) Uani 1 1 d . . . P1 P 0.89251(8) 0.22846(7) 0.40698(8) 0.0325(2) Uani 1 1 d . . . P2 P 0.74192(8) -0.19220(7) 0.84958(8) 0.0331(2) Uani 1 1 d . . . Co1 Co 0.65534(3) 0.32512(3) 0.76589(3) 0.01948(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0266(16) 0.0203(14) 0.0367(18) 0.0120(13) 0.0144(14) 0.0039(12) C2 0.0278(17) 0.0301(17) 0.054(2) 0.0195(16) 0.0220(16) 0.0054(13) C3 0.0400(19) 0.0308(17) 0.052(2) 0.0244(16) 0.0294(17) 0.0108(14) C4 0.0390(18) 0.0261(15) 0.0316(18) 0.0159(14) 0.0198(14) 0.0094(13) C5 0.0294(16) 0.0161(13) 0.0256(16) 0.0066(12) 0.0130(13) 0.0024(11) C6 0.0218(14) 0.0218(14) 0.0176(14) 0.0062(12) 0.0057(11) -0.0015(11) C7 0.0217(15) 0.0240(15) 0.0233(16) 0.0028(13) 0.0087(12) -0.0006(11) C8 0.0244(15) 0.0208(14) 0.0302(17) 0.0049(13) 0.0070(13) 0.0046(11) C9 0.0293(16) 0.0186(14) 0.0245(16) 0.0087(12) 0.0058(13) 0.0020(11) C10 0.0215(14) 0.0170(13) 0.0177(14) 0.0051(11) 0.0040(11) -0.0017(10) C11 0.0294(16) 0.0200(14) 0.0212(15) 0.0081(12) 0.0097(12) 0.0031(11) C12 0.0370(18) 0.0249(15) 0.0231(16) 0.0103(13) 0.0112(13) 0.0046(13) C13 0.0323(16) 0.0199(14) 0.0258(16) 0.0110(13) 0.0120(13) 0.0048(12) C14 0.0333(17) 0.0198(14) 0.0296(18) 0.0051(13) 0.0114(14) -0.0019(12) C15 0.0282(16) 0.0290(16) 0.0240(16) 0.0053(13) 0.0056(13) -0.0002(12) C16 0.0312(16) 0.0279(15) 0.0221(16) 0.0101(13) 0.0080(13) 0.0051(12) C17 0.0236(15) 0.0205(14) 0.0200(15) 0.0065(12) 0.0101(12) 0.0020(11) C18 0.0328(17) 0.0241(15) 0.0357(19) 0.0114(14) 0.0107(14) 0.0024(12) C19 0.043(2) 0.0268(16) 0.040(2) 0.0154(15) 0.0170(16) 0.0135(14) C20 0.0364(19) 0.0401(19) 0.044(2) 0.0242(16) 0.0217(16) 0.0197(15) C21 0.0265(17) 0.0419(19) 0.046(2) 0.0206(16) 0.0174(15) 0.0075(14) C22 0.0247(16) 0.0298(16) 0.0297(17) 0.0140(14) 0.0101(13) 0.0046(12) C23 0.0223(16) 0.0268(15) 0.0394(19) 0.0139(14) 0.0094(14) 0.0006(12) C24 0.0232(17) 0.0414(19) 0.058(2) 0.0261(18) 0.0088(16) 0.0009(14) C25 0.0271(16) 0.0285(16) 0.0294(18) 0.0109(14) 0.0043(13) 0.0058(12) C26 0.042(2) 0.0296(16) 0.0213(17) 0.0072(14) 0.0038(14) 0.0099(14) C27 0.043(2) 0.0230(16) 0.0317(19) 0.0061(14) -0.0059(15) 0.0000(14) C28 0.0311(18) 0.0285(17) 0.038(2) 0.0110(15) 0.0008(15) -0.0034(13) C29 0.0235(16) 0.0225(15) 0.0333(18) 0.0130(13) 0.0014(13) 0.0007(11) C30 0.0282(16) 0.0247(15) 0.0262(17) 0.0061(14) 0.0099(13) 0.0022(12) C31 0.063(2) 0.0331(18) 0.043(2) 0.0191(16) 0.0291(19) 0.0057(16) N1 0.0255(13) 0.0188(12) 0.0261(14) 0.0076(10) 0.0125(11) 0.0032(9) N2 0.0214(12) 0.0176(11) 0.0160(12) 0.0032(10) 0.0049(9) -0.0010(9) N3 0.0254(13) 0.0205(12) 0.0210(13) 0.0066(10) 0.0101(10) 0.0027(9) N4 0.0283(13) 0.0227(13) 0.0286(15) 0.0100(11) 0.0115(11) 0.0054(10) N5 0.0241(13) 0.0200(12) 0.0269(14) 0.0098(11) 0.0073(11) 0.0048(9) N6 0.0251(13) 0.0226(12) 0.0253(14) 0.0084(11) 0.0065(11) 0.0029(10) F1 0.0465(12) 0.0632(14) 0.0649(16) 0.0421(12) 0.0230(11) 0.0064(10) F2 0.0726(15) 0.0434(12) 0.0345(12) 0.0035(10) 0.0234(11) 0.0041(10) F3 0.0445(13) 0.0567(14) 0.090(2) 0.0292(13) 0.0386(13) 0.0146(10) F4 0.0673(15) 0.0646(14) 0.0260(11) 0.0195(10) 0.0156(10) 0.0080(11) F5 0.140(2) 0.0320(11) 0.0344(13) 0.0149(10) 0.0309(14) 0.0009(13) F6 0.0658(16) 0.0881(18) 0.0504(14) 0.0145(13) 0.0157(12) 0.0523(14) F7 0.0515(13) 0.0442(12) 0.0730(16) 0.0371(11) 0.0243(11) 0.0049(10) F8 0.0736(16) 0.0325(11) 0.0579(16) 0.0145(11) -0.0205(12) -0.0011(10) F9 0.0589(13) 0.0372(11) 0.0396(12) 0.0146(9) 0.0116(10) 0.0216(9) F10 0.0466(12) 0.0356(11) 0.0669(15) 0.0309(10) 0.0206(11) 0.0131(9) F11 0.0746(15) 0.0388(11) 0.0501(14) 0.0202(10) 0.0344(12) 0.0192(10) F12 0.0432(11) 0.0334(10) 0.0419(12) 0.0057(9) 0.0106(9) -0.0015(8) P1 0.0466(5) 0.0332(5) 0.0286(5) 0.0167(4) 0.0206(4) 0.0165(4) P2 0.0362(5) 0.0228(4) 0.0380(5) 0.0132(4) 0.0073(4) 0.0035(3) Co1 0.0212(2) 0.0169(2) 0.0201(2) 0.00676(16) 0.00666(16) 0.00105(14) _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 C1 N1 1.357(4) . ? C1 C2 1.385(4) . ? C1 C23 1.545(5) . ? C2 C3 1.375(5) . ? C2 H2 0.9300 . ? C3 C4 1.366(4) . ? C3 H3 0.9300 . ? C4 C5 1.396(4) . ? C4 H4 0.9300 . ? C5 N1 1.340(4) . ? C5 C11 1.544(4) . ? C6 N2 1.350(4) . ? C6 C7 1.380(4) . ? C6 H6 0.9300 . ? C7 C8 1.377(5) . ? C7 H7 0.9300 . ? C8 C9 1.379(4) . ? C8 H8 0.9300 . ? C9 C10 1.385(4) . ? C9 H9 0.9300 . ? C10 N2 1.347(4) . ? C10 C11 1.546(4) . ? C11 C12 1.528(4) . ? C11 C17 1.547(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N3 1.345(4) . ? C13 C14 1.374(4) . ? C13 H13 0.9300 . ? C14 C15 1.379(5) . ? C14 H14 0.9300 . ? C15 C16 1.377(4) . ? C15 H15 0.9300 . ? C16 C17 1.388(4) . ? C16 H16 0.9300 . ? C17 N3 1.347(4) . ? C18 N4 1.338(4) . ? C18 C19 1.379(4) . ? C18 H18 0.9300 . ? C19 C20 1.374(5) . ? C19 H19 0.9300 . ? C20 C21 1.375(5) . ? C20 H20 0.9300 . ? C21 C22 1.386(4) . ? C21 H21 0.9300 . ? C22 N4 1.350(4) . ? C22 C23 1.545(4) . ? C23 C29 1.538(5) . ? C23 C24 1.541(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N5 1.332(4) . ? C25 C26 1.389(4) . ? C25 H25 0.9300 . ? C26 C27 1.373(5) . ? C26 H26 0.9300 . ? C27 C28 1.379(5) . ? C27 H27 0.9300 . ? C28 C29 1.384(4) . ? C28 H28 0.9300 . ? C29 N5 1.353(4) . ? C30 N6 1.140(4) . ? C30 C31 1.453(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 Co1 2.097(3) . ? N2 Co1 2.134(2) . ? N3 Co1 2.129(2) . ? N4 Co1 2.131(2) . ? N5 Co1 2.121(2) . ? N6 Co1 2.132(3) . ? F1 P1 1.589(2) . ? F2 P1 1.606(2) . ? F3 P1 1.585(2) . ? F4 P1 1.597(2) . ? F5 P1 1.598(2) . ? F6 P1 1.576(2) . ? F7 P2 1.587(2) . ? F8 P2 1.582(2) . ? F9 P2 1.593(2) . ? F10 P2 1.609(2) . ? F11 P2 1.602(2) . ? F12 P2 1.592(2) . ? 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 N1 C1 C2 120.2(3) . . ? N1 C1 C23 118.1(3) . . ? C2 C1 C23 121.7(3) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 120.8(3) . . ? N1 C5 C11 118.3(3) . . ? C4 C5 C11 120.9(3) . . ? N2 C6 C7 123.0(3) . . ? N2 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? C8 C7 C6 118.5(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 118.8(3) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N2 C10 C9 120.9(3) . . ? N2 C10 C11 117.4(2) . . ? C9 C10 C11 121.7(3) . . ? C12 C11 C5 109.4(2) . . ? C12 C11 C10 109.4(2) . . ? C5 C11 C10 110.0(2) . . ? C12 C11 C17 109.6(2) . . ? C5 C11 C17 110.7(2) . . ? C10 C11 C17 107.7(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 123.7(3) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? C13 C14 C15 118.0(3) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? N3 C17 C16 120.7(3) . . ? N3 C17 C11 117.4(2) . . ? C16 C17 C11 121.8(3) . . ? N4 C18 C19 123.7(3) . . ? N4 C18 H18 118.1 . . ? C19 C18 H18 118.1 . . ? C20 C19 C18 117.9(3) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C21 C20 C19 119.1(3) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? N4 C22 C21 120.3(3) . . ? N4 C22 C23 117.0(2) . . ? C21 C22 C23 122.6(3) . . ? C29 C23 C24 109.3(3) . . ? C29 C23 C22 107.0(3) . . ? C24 C23 C22 109.2(2) . . ? C29 C23 C1 112.0(2) . . ? C24 C23 C1 108.9(3) . . ? C22 C23 C1 110.3(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C26 123.7(3) . . ? N5 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C27 C26 C25 117.5(3) . . ? C27 C26 H26 121.3 . . ? C25 C26 H26 121.3 . . ? C26 C27 C28 119.5(3) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? N5 C29 C28 120.4(3) . . ? N5 C29 C23 117.1(3) . . ? C28 C29 C23 122.3(3) . . ? N6 C30 C31 179.4(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C5 N1 C1 120.4(3) . . ? C5 N1 Co1 119.72(19) . . ? C1 N1 Co1 119.5(2) . . ? C10 N2 C6 118.4(2) . . ? C10 N2 Co1 118.91(19) . . ? C6 N2 Co1 122.1(2) . . ? C13 N3 C17 118.3(2) . . ? C13 N3 Co1 121.4(2) . . ? C17 N3 Co1 119.93(18) . . ? C18 N4 C22 118.5(3) . . ? C18 N4 Co1 121.0(2) . . ? C22 N4 Co1 120.07(19) . . ? C25 N5 C29 118.7(3) . . ? C25 N5 Co1 121.52(19) . . ? C29 N5 Co1 119.6(2) . . ? C30 N6 Co1 173.7(2) . . ? F6 P1 F3 178.76(15) . . ? F6 P1 F1 89.96(15) . . ? F3 P1 F1 89.66(12) . . ? F6 P1 F5 91.14(17) . . ? F3 P1 F5 89.26(15) . . ? F1 P1 F5 178.76(15) . . ? F6 P1 F4 90.44(12) . . ? F3 P1 F4 90.75(13) . . ? F1 P1 F4 90.70(13) . . ? F5 P1 F4 88.71(12) . . ? F6 P1 F2 89.24(13) . . ? F3 P1 F2 89.58(13) . . ? F1 P1 F2 90.61(13) . . ? F5 P1 F2 89.98(12) . . ? F4 P1 F2 178.65(13) . . ? F8 P2 F7 90.60(15) . . ? F8 P2 F12 179.29(13) . . ? F7 P2 F12 89.77(13) . . ? F8 P2 F9 90.00(12) . . ? F7 P2 F9 91.09(12) . . ? F12 P2 F9 90.60(11) . . ? F8 P2 F11 90.15(14) . . ? F7 P2 F11 178.31(12) . . ? F12 P2 F11 89.46(12) . . ? F9 P2 F11 90.43(12) . . ? F8 P2 F10 89.93(12) . . ? F7 P2 F10 89.75(12) . . ? F12 P2 F10 89.46(11) . . ? F9 P2 F10 179.16(14) . . ? F11 P2 F10 88.74(12) . . ? N1 Co1 N5 88.15(10) . . ? N1 Co1 N3 87.61(10) . . ? N5 Co1 N3 175.52(10) . . ? N1 Co1 N4 86.68(10) . . ? N5 Co1 N4 81.17(9) . . ? N3 Co1 N4 100.03(9) . . ? N1 Co1 N6 178.43(9) . . ? N5 Co1 N6 90.96(10) . . ? N3 Co1 N6 93.31(9) . . ? N4 Co1 N6 91.90(10) . . ? N1 Co1 N2 87.16(9) . . ? N5 Co1 N2 97.40(9) . . ? N3 Co1 N2 80.94(9) . . ? N4 Co1 N2 173.73(9) . . ? N6 Co1 N2 94.23(9) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 0.476 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.065 _iucr_refine_instructions_details ; TITL aek1052 in P-1 CELL 0.71073 11.4620 12.5010 13.1640 109.795 108.383 90.824 ZERR 2.00 0.0000 0.0000 0.0000 0.000 0.000 0.000 LATT 1 SFAC C H N F P CL CO UNIT 62 56 12 24 4 0 2 MERG 2 FMAP 2 PLAN 25 SIZE 0.12 0.14 0.14 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP 100.00 WGHT 0.052700 1.576400 FVAR 0.46618 C1 1 0.454131 0.192584 0.793908 11.00000 0.02661 0.02034 = 0.03671 0.01197 0.01444 0.00390 C2 1 0.400378 0.138106 0.847152 11.00000 0.02781 0.03013 = 0.05392 0.01948 0.02203 0.00536 AFIX 43 H2 2 0.315287 0.114468 0.818357 11.00000 -1.20000 AFIX 0 C3 1 0.473799 0.119232 0.942936 11.00000 0.03996 0.03079 = 0.05181 0.02435 0.02943 0.01085 AFIX 43 H3 2 0.438050 0.084858 0.980558 11.00000 -1.20000 AFIX 0 C4 1 0.599170 0.150951 0.982806 11.00000 0.03903 0.02612 = 0.03164 0.01592 0.01980 0.00938 AFIX 43 H4 2 0.649439 0.137811 1.047116 11.00000 -1.20000 AFIX 0 C5 1 0.650829 0.203372 0.925700 11.00000 0.02937 0.01606 = 0.02565 0.00660 0.01300 0.00241 C6 1 0.854866 0.188419 0.693604 11.00000 0.02184 0.02183 = 0.01762 0.00622 0.00569 -0.00145 AFIX 43 H6 2 0.833545 0.218795 0.635759 11.00000 -1.20000 AFIX 0 C7 1 0.936011 0.107878 0.689682 11.00000 0.02169 0.02404 = 0.02328 0.00285 0.00872 -0.00064 AFIX 43 H7 2 0.969343 0.085088 0.630961 11.00000 -1.20000 AFIX 0 C8 1 0.966544 0.061993 0.774644 11.00000 0.02443 0.02075 = 0.03022 0.00493 0.00704 0.00457 AFIX 43 H8 2 1.018455 0.005391 0.772823 11.00000 -1.20000 AFIX 0 C9 1 0.918749 0.101493 0.862485 11.00000 0.02927 0.01861 = 0.02452 0.00866 0.00584 0.00198 AFIX 43 H9 2 0.939741 0.072397 0.921277 11.00000 -1.20000 AFIX 0 C10 1 0.839656 0.184259 0.863603 11.00000 0.02153 0.01699 = 0.01766 0.00509 0.00398 -0.00167 C11 1 0.792497 0.237205 0.965348 11.00000 0.02935 0.01996 = 0.02123 0.00811 0.00975 0.00315 C12 1 0.857013 0.193289 1.061305 11.00000 0.03700 0.02486 = 0.02309 0.01030 0.01117 0.00462 AFIX 137 H12A 2 0.833260 0.231181 1.127021 11.00000 -1.50000 H12B 2 0.945317 0.209069 1.081962 11.00000 -1.50000 H12C 2 0.832986 0.112032 1.035203 11.00000 -1.50000 AFIX 0 C13 1 0.804514 0.536478 0.970992 11.00000 0.03231 0.01987 = 0.02578 0.01105 0.01199 0.00483 AFIX 43 H13 2 0.768848 0.573018 0.920078 11.00000 -1.20000 AFIX 0 C14 1 0.887544 0.601685 1.076993 11.00000 0.03329 0.01983 = 0.02956 0.00507 0.01136 -0.00192 AFIX 43 H14 2 0.906971 0.680351 1.097677 11.00000 -1.20000 AFIX 0 C15 1 0.941227 0.547025 1.151812 11.00000 0.02823 0.02897 = 0.02397 0.00533 0.00561 -0.00018 AFIX 43 H15 2 0.996925 0.588533 1.224736 11.00000 -1.20000 AFIX 0 C16 1 0.911246 0.430160 1.117087 11.00000 0.03124 0.02786 = 0.02212 0.01013 0.00801 0.00511 AFIX 43 H16 2 0.948398 0.392026 1.166052 11.00000 -1.20000 AFIX 0 C17 1 0.825707 0.369077 1.009176 11.00000 0.02356 0.02047 = 0.01997 0.00648 0.01008 0.00195 C18 1 0.503642 0.524218 0.779098 11.00000 0.03283 0.02414 = 0.03570 0.01136 0.01067 0.00243 AFIX 43 H18 2 0.582165 0.565717 0.806291 11.00000 -1.20000 AFIX 0 C19 1 0.402219 0.582497 0.762852 11.00000 0.04325 0.02679 = 0.04012 0.01538 0.01698 0.01345 AFIX 43 H19 2 0.411844 0.661064 0.778468 11.00000 -1.20000 AFIX 0 C20 1 0.286493 0.520764 0.722855 11.00000 0.03637 0.04011 = 0.04387 0.02418 0.02166 0.01974 AFIX 43 H20 2 0.215786 0.556977 0.710877 11.00000 -1.20000 AFIX 0 C21 1 0.276594 0.404735 0.700769 11.00000 0.02647 0.04192 = 0.04552 0.02063 0.01742 0.00745 AFIX 43 H21 2 0.198649 0.362220 0.673703 11.00000 -1.20000 AFIX 0 C22 1 0.381906 0.350617 0.718533 11.00000 0.02472 0.02980 = 0.02971 0.01402 0.01009 0.00464 C23 1 0.375658 0.219514 0.688466 11.00000 0.02230 0.02681 = 0.03943 0.01388 0.00942 0.00065 C24 1 0.239729 0.166784 0.651910 11.00000 0.02323 0.04143 = 0.05844 0.02610 0.00884 0.00091 AFIX 137 H24A 2 0.191351 0.178727 0.583385 11.00000 -1.50000 H24B 2 0.207158 0.202808 0.712194 11.00000 -1.50000 H24C 2 0.236026 0.085978 0.637385 11.00000 -1.50000 AFIX 0 C25 1 0.574970 0.187404 0.510006 11.00000 0.02713 0.02845 = 0.02938 0.01091 0.00432 0.00583 AFIX 43 H25 2 0.652626 0.220740 0.519569 11.00000 -1.20000 AFIX 0 C26 1 0.505255 0.109025 0.402391 11.00000 0.04235 0.02959 = 0.02125 0.00718 0.00382 0.00991 AFIX 43 H26 2 0.534582 0.090680 0.341083 11.00000 -1.20000 AFIX 0 C27 1 0.391381 0.059656 0.389972 11.00000 0.04281 0.02299 = 0.03168 0.00610 -0.00594 0.00002 AFIX 43 H27 2 0.342590 0.005303 0.319870 11.00000 -1.20000 AFIX 0 C28 1 0.349885 0.091283 0.482260 11.00000 0.03109 0.02849 = 0.03833 0.01102 0.00083 -0.00340 AFIX 43 H28 2 0.272660 0.058406 0.474257 11.00000 -1.20000 AFIX 0 C29 1 0.422779 0.171767 0.586712 11.00000 0.02351 0.02249 = 0.03335 0.01302 0.00145 0.00074 C30 1 0.756720 0.481228 0.648216 11.00000 0.02823 0.02472 = 0.02623 0.00607 0.00989 0.00225 C31 1 0.792467 0.547910 0.588705 11.00000 0.06318 0.03306 = 0.04319 0.01905 0.02914 0.00570 AFIX 137 H31A 2 0.863087 0.520731 0.568716 11.00000 -1.50000 H31B 2 0.813301 0.627298 0.637893 11.00000 -1.50000 H31C 2 0.724629 0.539758 0.520190 11.00000 -1.50000 AFIX 0 N1 3 0.578690 0.224574 0.834298 11.00000 0.02552 0.01876 = 0.02610 0.00759 0.01248 0.00322 N2 3 0.804997 0.225142 0.777646 11.00000 0.02136 0.01764 = 0.01596 0.00321 0.00487 -0.00099 N3 3 0.771921 0.422715 0.936732 11.00000 0.02536 0.02046 = 0.02102 0.00658 0.01009 0.00266 N4 3 0.495557 0.411384 0.757980 11.00000 0.02830 0.02273 = 0.02858 0.00998 0.01149 0.00538 N5 3 0.536860 0.217518 0.600297 11.00000 0.02410 0.02002 = 0.02690 0.00981 0.00731 0.00483 N6 3 0.728289 0.428158 0.694080 11.00000 0.02514 0.02265 = 0.02533 0.00835 0.00647 0.00286 F1 4 0.931122 0.327398 0.368805 11.00000 0.04648 0.06323 = 0.06486 0.04208 0.02304 0.00641 F2 4 0.955077 0.308920 0.539749 11.00000 0.07256 0.04340 = 0.03451 0.00353 0.02341 0.00410 F3 4 0.765619 0.277354 0.406472 11.00000 0.04453 0.05675 = 0.09005 0.02916 0.03861 0.01460 F4 4 0.830123 0.145873 0.275795 11.00000 0.06729 0.06458 = 0.02604 0.01951 0.01557 0.00800 F5 4 0.850606 0.129036 0.443974 11.00000 0.13985 0.03200 = 0.03444 0.01492 0.03089 0.00092 F6 4 1.020233 0.182145 0.409905 11.00000 0.06578 0.08806 = 0.05044 0.01449 0.01572 0.05230 F7 4 0.800789 -0.151260 0.772552 11.00000 0.05147 0.04419 = 0.07295 0.03708 0.02426 0.00491 F8 4 0.840181 -0.103122 0.962416 11.00000 0.07359 0.03248 = 0.05791 0.01447 -0.02047 -0.00109 F9 4 0.648884 -0.098811 0.848626 11.00000 0.05894 0.03717 = 0.03961 0.01463 0.01156 0.02163 F10 4 0.835139 -0.287058 0.851805 11.00000 0.04661 0.03562 = 0.06687 0.03088 0.02062 0.01307 F11 4 0.683657 -0.237203 0.925877 11.00000 0.07464 0.03883 = 0.05012 0.02018 0.03435 0.01919 F12 4 0.643650 -0.283096 0.736586 11.00000 0.04319 0.03343 = 0.04189 0.00570 0.01062 -0.00148 P1 5 0.892514 0.228457 0.406977 11.00000 0.04655 0.03319 = 0.02859 0.01673 0.02062 0.01650 P2 5 0.741924 -0.192202 0.849584 11.00000 0.03623 0.02283 = 0.03795 0.01320 0.00731 0.00348 CO1 7 0.655340 0.325124 0.765892 11.00000 0.02117 0.01694 = 0.02007 0.00676 0.00666 0.00105 HKLF 4 REM aek1052_0m in P-1 REM R1 = 0.0399 for 4400 Fo > 4sig(Fo) and 0.0523 for all 5362 data REM 472 parameters refined using 0 restraints END WGHT 0.0493 1.6518 REM Highest difference peak 0.476, deepest hole -0.431, 1-sigma level 0.065 Q1 1 0.9378 0.1101 0.4369 11.00000 0.05 0.48 Q2 1 0.5838 0.3608 0.7881 11.00000 0.05 0.42 Q3 1 0.9496 0.3847 0.4415 11.00000 0.05 0.40 Q4 1 0.7855 0.2185 0.4223 11.00000 0.05 0.38 Q5 1 0.7436 0.2493 0.7714 11.00000 0.05 0.37 Q6 1 0.7675 -0.0816 0.9972 11.00000 0.05 0.37 Q7 1 0.7806 -0.1050 0.8459 11.00000 0.05 0.36 Q8 1 0.8735 0.2998 0.4997 11.00000 0.05 0.35 Q9 1 0.8244 -0.1155 0.8576 11.00000 0.05 0.35 Q10 1 0.7773 0.1966 0.3143 11.00000 0.05 0.35 Q11 1 0.9932 0.2059 0.3428 11.00000 0.05 0.32 Q12 1 0.3780 0.2799 0.7035 11.00000 0.05 0.31 Q13 1 0.7332 0.2925 0.7464 11.00000 0.05 0.31 Q14 1 0.7442 -0.0956 0.9066 11.00000 0.05 0.31 Q15 1 0.7979 0.2985 0.9858 11.00000 0.05 0.29 Q16 1 1.0602 0.2599 0.4463 11.00000 0.05 0.29 Q17 1 0.6325 0.3303 0.7106 11.00000 0.05 0.28 Q18 1 0.7289 0.2133 0.9478 11.00000 0.05 0.27 Q19 1 0.7116 0.3923 0.8847 11.00000 0.05 0.27 Q20 1 0.7579 -0.1647 0.9533 11.00000 0.05 0.26 Q21 1 0.6832 0.2598 0.7034 11.00000 0.05 0.26 Q22 1 0.8393 0.3176 0.3517 11.00000 0.05 0.26 Q23 1 0.7154 -0.1527 0.9157 11.00000 0.05 0.25 Q24 1 0.9331 0.3093 0.4403 11.00000 0.05 0.25 Q25 1 0.5999 0.2839 0.8417 11.00000 0.05 0.25 ; data_shelxl _database_code_depnum_ccdc_archive 'CCDC 915155' #TrackingRef '16056_web_deposit_cif_file_0_AmandaKing_1355197332.aek1071.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AEK1071_0m _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.50 H22.50 B0.50 Co0.50 F0 N2.50 O0' _chemical_formula_weight 410.84 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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 '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' O O 0.0492 0.0322 '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 10.9829(8) _cell_length_b 13.7142(9) _cell_length_c 17.0064(13) _cell_angle_alpha 102.458(5) _cell_angle_beta 107.971(5) _cell_angle_gamma 101.250(5) _cell_volume 2282.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plates _exptl_crystal_colour Blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 3.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7370 _exptl_absorpt_correction_T_max 0.9378 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator 'HELIOS multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 20067 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 63.68 _reflns_number_total 7242 _reflns_number_gt 4707 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0885P)^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 SHELXL _refine_ls_extinction_coef 0.00062(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7242 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7941(4) 0.8749(3) 0.7193(3) 0.0500(12) Uani 1 1 d . . . C2 C 0.9264(4) 0.8777(3) 0.7486(4) 0.0649(15) Uani 1 1 d . . . H53A H 0.9743 0.8820 0.7123 0.078 Uiso 1 1 calc R . . C3 C 0.9893(5) 0.8742(4) 0.8317(4) 0.0767(19) Uani 1 1 d . . . H54A H 1.0788 0.8757 0.8516 0.092 Uiso 1 1 calc R . . C4 C 0.9161(5) 0.8684(3) 0.8845(4) 0.0692(17) Uani 1 1 d . . . H23A H 0.9566 0.8670 0.9408 0.083 Uiso 1 1 calc R . . C5 C 0.7823(4) 0.8646(3) 0.8535(3) 0.0557(13) Uani 1 1 d . . . C6 C 0.5764(4) 1.0853(3) 0.8755(3) 0.0422(10) Uani 1 1 d . . . H15A H 0.5416 1.1099 0.8290 0.051 Uiso 1 1 calc R . . C7 C 0.6000(4) 1.1471(3) 0.9575(3) 0.0486(11) Uani 1 1 d . . . H16A H 0.5822 1.2113 0.9659 0.058 Uiso 1 1 calc R . . C8 C 0.6505(5) 1.1106(3) 1.0262(3) 0.0597(14) Uani 1 1 d . . . H17A H 0.6652 1.1489 1.0822 0.072 Uiso 1 1 calc R . . C9 C 0.6789(5) 1.0168(3) 1.0109(3) 0.0595(14) Uani 1 1 d . . . H18A H 0.7135 0.9916 1.0571 0.071 Uiso 1 1 calc R . . C10 C 0.6568(4) 0.9588(3) 0.9275(3) 0.0463(11) Uani 1 1 d . . . C11 C 0.6930(4) 0.8561(3) 0.9073(3) 0.0488(11) Uani 1 1 d . . . C12 C 0.7683(5) 0.8366(4) 0.9929(3) 0.0654(15) Uani 1 1 d . . . H21A H 0.7918 0.7727 0.9804 0.098 Uiso 1 1 calc R . . H21B H 0.7120 0.8319 1.0262 0.098 Uiso 1 1 calc R . . H21C H 0.8478 0.8931 1.0253 0.098 Uiso 1 1 calc R . . C13 C 0.3496(4) 0.7088(3) 0.7538(3) 0.0455(10) Uani 1 1 d . . . H1A H 0.2800 0.7238 0.7155 0.055 Uiso 1 1 calc R . . C14 C 0.3244(5) 0.6144(3) 0.7703(3) 0.0512(11) Uani 1 1 d . . . H3A H 0.2416 0.5654 0.7411 0.061 Uiso 1 1 calc R . . C15 C 0.4249(5) 0.5941(3) 0.8312(3) 0.0522(12) Uani 1 1 d . . . H4A H 0.4129 0.5297 0.8416 0.063 Uiso 1 1 calc R . . C16 C 0.5429(5) 0.6713(3) 0.8763(3) 0.0513(12) Uani 1 1 d . . . H5A H 0.6090 0.6603 0.9202 0.062 Uiso 1 1 calc R . . C17 C 0.5657(4) 0.7659(3) 0.8574(3) 0.0478(11) Uani 1 1 d . . . C18 C 0.3886(4) 0.6903(3) 0.5725(3) 0.0495(11) Uani 1 1 d . . . H50A H 0.3207 0.6842 0.5944 0.059 Uiso 1 1 calc R . . C19 C 0.3701(5) 0.6154(4) 0.4977(3) 0.0611(14) Uani 1 1 d . . . H51A H 0.2910 0.5620 0.4695 0.073 Uiso 1 1 calc R . . C20 C 0.4716(5) 0.6218(4) 0.4658(3) 0.0600(13) Uani 1 1 d . . . H11A H 0.4639 0.5710 0.4169 0.072 Uiso 1 1 calc R . . C21 C 0.5846(5) 0.7046(4) 0.5075(3) 0.0558(12) Uani 1 1 d . . . H10A H 0.6534 0.7108 0.4863 0.067 Uiso 1 1 calc R . . C22 C 0.5964(4) 0.7803(3) 0.5825(3) 0.0502(11) Uani 1 1 d . . . C23 C 0.7179(4) 0.8771(3) 0.6273(3) 0.0522(11) Uani 1 1 d . . . C24 C 0.8122(5) 0.8765(4) 0.5760(4) 0.0719(16) Uani 1 1 d . . . H25A H 0.7655 0.8775 0.5184 0.108 Uiso 1 1 calc R . . H25B H 0.8417 0.8148 0.5734 0.108 Uiso 1 1 calc R . . H25C H 0.8880 0.9368 0.6044 0.108 Uiso 1 1 calc R . . C25 C 0.5168(4) 1.0598(3) 0.6597(3) 0.0451(10) Uani 1 1 d . . . H7A H 0.4538 1.0655 0.6852 0.054 Uiso 1 1 calc R . . C26 C 0.5441(6) 1.1295(3) 0.6157(3) 0.0623(14) Uani 1 1 d . . . H8A H 0.4995 1.1804 0.6108 0.075 Uiso 1 1 calc R . . C27 C 0.6391(6) 1.1222(4) 0.5792(4) 0.0749(17) Uani 1 1 d . . . H12A H 0.6628 1.1703 0.5516 0.090 Uiso 1 1 calc R . . C28 C 0.6989(5) 1.0429(4) 0.5838(4) 0.0673(15) Uani 1 1 d . . . H13A H 0.7614 1.0363 0.5580 0.081 Uiso 1 1 calc R . . C29 C 0.6656(4) 0.9729(3) 0.6270(3) 0.0474(11) Uani 1 1 d . . . C30 C 0.6336(4) 0.7011(3) 0.1866(2) 0.0318(8) Uani 1 1 d . . . C31 C 0.5811(4) 0.6451(3) 0.0991(2) 0.0380(9) Uani 1 1 d . . . H28A H 0.6389 0.6392 0.0694 0.046 Uiso 1 1 calc R . . C32 C 0.4442(4) 0.5974(3) 0.0544(3) 0.0426(10) Uani 1 1 d . . . H29A H 0.4129 0.5602 -0.0039 0.051 Uiso 1 1 calc R . . C33 C 0.3559(4) 0.6051(3) 0.0959(3) 0.0457(10) Uani 1 1 d . . . H30A H 0.2652 0.5722 0.0666 0.055 Uiso 1 1 calc R . . C34 C 0.4039(4) 0.6625(4) 0.1820(3) 0.0534(12) Uani 1 1 d . . . H31A H 0.3453 0.6703 0.2108 0.064 Uiso 1 1 calc R . . C35 C 0.5385(4) 0.7080(3) 0.2249(3) 0.0481(11) Uani 1 1 d . . . H32A H 0.5683 0.7457 0.2830 0.058 Uiso 1 1 calc R . . C36 C 0.8484(4) 0.7077(3) 0.3230(2) 0.0429(10) Uani 1 1 d . . . C37 C 0.7713(5) 0.6423(3) 0.3526(3) 0.0581(13) Uani 1 1 d . . . H46A H 0.6789 0.6232 0.3257 0.070 Uiso 1 1 calc R . . C38 C 0.8271(7) 0.6043(4) 0.4207(3) 0.0780(19) Uani 1 1 d . . . H47A H 0.7716 0.5605 0.4382 0.094 Uiso 1 1 calc R . . C39 C 0.9617(8) 0.6304(5) 0.4622(3) 0.089(2) Uani 1 1 d . . . H48A H 0.9987 0.6057 0.5082 0.107 Uiso 1 1 calc R . . C40 C 1.0415(7) 0.6942(5) 0.4346(3) 0.087(2) Uani 1 1 d . . . H52A H 1.1338 0.7125 0.4618 0.104 Uiso 1 1 calc R . . C41 C 0.9860(5) 0.7310(4) 0.3671(3) 0.0604(13) Uani 1 1 d . . . H49A H 1.0428 0.7737 0.3497 0.072 Uiso 1 1 calc R . . C42 C 0.7993(3) 0.8824(3) 0.2880(2) 0.0333(8) Uani 1 1 d . . . C43 C 0.8505(4) 0.9356(3) 0.3757(3) 0.0397(9) Uani 1 1 d . . . H37A H 0.8848 0.9011 0.4150 0.048 Uiso 1 1 calc R . . C44 C 0.8524(4) 1.0385(3) 0.4071(3) 0.0381(9) Uani 1 1 d . . . H36A H 0.8883 1.0711 0.4664 0.046 Uiso 1 1 calc R . . C45 C 0.8020(4) 1.0926(3) 0.3516(3) 0.0401(9) Uani 1 1 d . . . H35A H 0.8036 1.1614 0.3729 0.048 Uiso 1 1 calc R . . C46 C 0.7488(4) 1.0428(3) 0.2631(3) 0.0404(9) Uani 1 1 d . . . H34A H 0.7142 1.0780 0.2245 0.048 Uiso 1 1 calc R . . C47 C 0.7474(4) 0.9400(3) 0.2328(3) 0.0372(9) Uani 1 1 d . . . H33A H 0.7107 0.9076 0.1735 0.045 Uiso 1 1 calc R . . C48 C 0.8894(4) 0.7537(3) 0.1890(3) 0.0418(10) Uani 1 1 d . . . C49 C 0.8942(5) 0.6583(4) 0.1409(4) 0.0721(17) Uani 1 1 d . . . H44A H 0.8367 0.5974 0.1388 0.087 Uiso 1 1 calc R . . C50 C 0.9805(7) 0.6504(4) 0.0966(5) 0.101(2) Uani 1 1 d . . . H43A H 0.9760 0.5858 0.0627 0.122 Uiso 1 1 calc R . . C51 C 1.0737(5) 0.7392(4) 0.1028(4) 0.0760(17) Uani 1 1 d . . . H42A H 1.1349 0.7345 0.0758 0.091 Uiso 1 1 calc R . . C52 C 1.0733(4) 0.8347(3) 0.1502(3) 0.0492(11) Uani 1 1 d . . . H41A H 1.1344 0.8951 0.1549 0.059 Uiso 1 1 calc R . . C53 C 0.9817(4) 0.8403(3) 0.1904(3) 0.0419(10) Uani 1 1 d . . . H40A H 0.9818 0.9058 0.2202 0.050 Uiso 1 1 calc R . . N1 N 0.7227(3) 0.8689(2) 0.7714(2) 0.0467(9) Uani 1 1 d . . . N2 N 0.6003(3) 0.9924(2) 0.8586(2) 0.0400(8) Uani 1 1 d . . . N3 N 0.4700(3) 0.7808(3) 0.7903(2) 0.0472(9) Uani 1 1 d . . . N4 N 0.4985(3) 0.7714(3) 0.6156(2) 0.0458(9) Uani 1 1 d . . . N5 N 0.5770(3) 0.9833(3) 0.6675(2) 0.0412(8) Uani 1 1 d . . . Co1 Co 0.54089(6) 0.88428(5) 0.73477(4) 0.0382(2) Uani 1 1 d . . . B1 B 0.7924(4) 0.7594(3) 0.2456(3) 0.0364(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0297(19) 0.027(2) 0.085(3) 0.007(2) 0.017(2) 0.0061(18) C2 0.037(2) 0.033(3) 0.112(4) 0.011(3) 0.020(3) 0.007(2) C3 0.032(2) 0.036(3) 0.143(6) 0.028(3) 0.007(3) 0.008(2) C4 0.038(2) 0.033(3) 0.113(4) 0.028(3) -0.006(3) 0.004(2) C5 0.039(2) 0.031(2) 0.080(3) 0.022(2) -0.003(2) 0.005(2) C6 0.041(2) 0.037(2) 0.052(2) 0.024(2) 0.0159(19) 0.0068(19) C7 0.040(2) 0.037(2) 0.060(3) 0.020(2) 0.005(2) 0.006(2) C8 0.067(3) 0.035(3) 0.049(3) 0.012(2) -0.012(2) 0.006(2) C9 0.063(3) 0.031(2) 0.052(3) 0.012(2) -0.015(2) 0.003(2) C10 0.043(2) 0.025(2) 0.050(3) 0.011(2) -0.005(2) -0.0004(19) C11 0.044(2) 0.031(2) 0.058(3) 0.019(2) -0.003(2) 0.0074(19) C12 0.069(3) 0.038(3) 0.066(3) 0.022(2) -0.011(3) 0.015(2) C13 0.040(2) 0.037(2) 0.053(2) 0.021(2) 0.009(2) 0.0007(19) C14 0.058(3) 0.038(3) 0.049(2) 0.018(2) 0.014(2) -0.001(2) C15 0.074(3) 0.033(2) 0.044(2) 0.019(2) 0.016(2) 0.004(2) C16 0.064(3) 0.036(3) 0.047(2) 0.020(2) 0.007(2) 0.010(2) C17 0.052(2) 0.035(2) 0.050(2) 0.022(2) 0.005(2) 0.012(2) C18 0.043(2) 0.035(3) 0.061(3) 0.021(2) 0.007(2) 0.002(2) C19 0.056(3) 0.045(3) 0.066(3) 0.026(3) 0.001(3) 0.003(2) C20 0.058(3) 0.046(3) 0.063(3) 0.015(3) 0.006(3) 0.014(3) C21 0.051(3) 0.040(3) 0.078(3) 0.019(3) 0.023(3) 0.017(2) C22 0.042(2) 0.031(2) 0.070(3) 0.013(2) 0.012(2) 0.010(2) C23 0.045(2) 0.039(3) 0.075(3) 0.014(2) 0.028(2) 0.009(2) C24 0.052(3) 0.052(3) 0.112(4) 0.006(3) 0.047(3) 0.008(2) C25 0.062(3) 0.037(2) 0.053(2) 0.025(2) 0.031(2) 0.021(2) C26 0.105(4) 0.042(3) 0.080(3) 0.036(3) 0.068(3) 0.035(3) C27 0.125(5) 0.042(3) 0.101(4) 0.038(3) 0.085(4) 0.030(3) C28 0.084(4) 0.043(3) 0.099(4) 0.021(3) 0.069(3) 0.011(3) C29 0.048(2) 0.033(2) 0.069(3) 0.015(2) 0.036(2) 0.006(2) C30 0.0378(19) 0.026(2) 0.0344(19) 0.0172(17) 0.0127(16) 0.0078(17) C31 0.049(2) 0.024(2) 0.041(2) 0.0103(19) 0.0186(19) 0.0065(18) C32 0.051(2) 0.031(2) 0.039(2) 0.0121(19) 0.0097(19) 0.004(2) C33 0.037(2) 0.034(2) 0.054(3) 0.013(2) 0.006(2) 0.0020(19) C34 0.046(2) 0.051(3) 0.059(3) 0.005(2) 0.026(2) 0.005(2) C35 0.048(2) 0.044(3) 0.044(2) 0.006(2) 0.019(2) 0.000(2) C36 0.058(3) 0.027(2) 0.030(2) 0.0076(18) -0.0001(19) 0.011(2) C37 0.083(3) 0.035(3) 0.044(2) 0.021(2) 0.008(2) 0.004(2) C38 0.151(6) 0.036(3) 0.037(3) 0.018(2) 0.017(3) 0.023(3) C39 0.159(7) 0.069(4) 0.025(2) 0.010(3) -0.001(3) 0.062(4) C40 0.105(5) 0.097(5) 0.046(3) 0.013(3) -0.007(3) 0.064(4) C41 0.060(3) 0.062(3) 0.048(3) 0.010(2) 0.003(2) 0.028(3) C42 0.0293(18) 0.028(2) 0.040(2) 0.0143(18) 0.0097(17) 0.0045(17) C43 0.036(2) 0.039(2) 0.047(2) 0.022(2) 0.0119(18) 0.0107(19) C44 0.0336(19) 0.037(2) 0.044(2) 0.0137(19) 0.0149(18) 0.0059(18) C45 0.044(2) 0.032(2) 0.052(2) 0.019(2) 0.025(2) 0.0104(19) C46 0.049(2) 0.034(2) 0.050(2) 0.024(2) 0.024(2) 0.0176(19) C47 0.038(2) 0.034(2) 0.044(2) 0.0181(19) 0.0167(18) 0.0074(18) C48 0.039(2) 0.031(2) 0.058(3) 0.018(2) 0.017(2) 0.0104(18) C49 0.064(3) 0.039(3) 0.140(5) 0.036(3) 0.066(4) 0.017(2) C50 0.107(5) 0.047(3) 0.199(8) 0.037(4) 0.114(5) 0.033(3) C51 0.067(3) 0.062(3) 0.147(5) 0.055(4) 0.077(4) 0.033(3) C52 0.038(2) 0.045(3) 0.074(3) 0.032(2) 0.023(2) 0.010(2) C53 0.041(2) 0.040(2) 0.046(2) 0.022(2) 0.0127(19) 0.0107(19) N1 0.0356(17) 0.0220(18) 0.073(2) 0.0123(18) 0.0091(18) 0.0064(15) N2 0.0347(16) 0.0344(18) 0.056(2) 0.0281(17) 0.0129(15) 0.0094(15) N3 0.0411(18) 0.037(2) 0.056(2) 0.0240(18) 0.0054(17) 0.0054(16) N4 0.0366(18) 0.036(2) 0.066(2) 0.0264(19) 0.0118(17) 0.0097(16) N5 0.0426(18) 0.0341(19) 0.053(2) 0.0192(17) 0.0227(16) 0.0095(16) Co1 0.0328(3) 0.0308(4) 0.0530(4) 0.0237(3) 0.0120(3) 0.0062(3) B1 0.041(2) 0.031(2) 0.042(2) 0.019(2) 0.015(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.357(6) . ? C1 C2 1.373(6) . ? C1 C23 1.541(7) . ? C2 C3 1.385(8) . ? C2 H53A 0.9300 . ? C3 C4 1.381(8) . ? C3 H54A 0.9300 . ? C4 C5 1.386(6) . ? C4 H23A 0.9300 . ? C5 N1 1.367(6) . ? C5 C11 1.539(7) . ? C6 N2 1.340(5) . ? C6 C7 1.382(6) . ? C6 H15A 0.9300 . ? C7 C8 1.371(6) . ? C7 H16A 0.9300 . ? C8 C9 1.373(6) . ? C8 H17A 0.9300 . ? C9 C10 1.390(6) . ? C9 H18A 0.9300 . ? C10 N2 1.366(5) . ? C10 C11 1.534(6) . ? C11 C17 1.531(6) . ? C11 C12 1.545(5) . ? C12 H21A 0.9600 . ? C12 H21B 0.9600 . ? C12 H21C 0.9600 . ? C13 N3 1.352(5) . ? C13 C14 1.376(5) . ? C13 H1A 0.9300 . ? C14 C15 1.381(6) . ? C14 H3A 0.9300 . ? C15 C16 1.375(6) . ? C15 H4A 0.9300 . ? C16 C17 1.398(5) . ? C16 H5A 0.9300 . ? C17 N3 1.375(5) . ? C18 N4 1.345(5) . ? C18 C19 1.381(7) . ? C18 H50A 0.9300 . ? C19 C20 1.379(7) . ? C19 H51A 0.9300 . ? C20 C21 1.376(7) . ? C20 H11A 0.9300 . ? C21 C22 1.412(7) . ? C21 H10A 0.9300 . ? C22 N4 1.357(6) . ? C22 C23 1.539(6) . ? C23 C29 1.533(6) . ? C23 C24 1.547(7) . ? C24 H25A 0.9600 . ? C24 H25B 0.9600 . ? C24 H25C 0.9600 . ? C25 N5 1.354(5) . ? C25 C26 1.379(5) . ? C25 H7A 0.9300 . ? C26 C27 1.378(7) . ? C26 H8A 0.9300 . ? C27 C28 1.380(7) . ? C27 H12A 0.9300 . ? C28 C29 1.389(6) . ? C28 H13A 0.9300 . ? C29 N5 1.366(5) . ? C30 C31 1.393(5) . ? C30 C35 1.398(6) . ? C30 B1 1.649(5) . ? C31 C32 1.401(6) . ? C31 H28A 0.9300 . ? C32 C33 1.371(6) . ? C32 H29A 0.9300 . ? C33 C34 1.380(6) . ? C33 H30A 0.9300 . ? C34 C35 1.373(6) . ? C34 H31A 0.9300 . ? C35 H32A 0.9300 . ? C36 C37 1.391(6) . ? C36 C41 1.398(6) . ? C36 B1 1.640(5) . ? C37 C38 1.392(6) . ? C37 H46A 0.9300 . ? C38 C39 1.361(9) . ? C38 H47A 0.9300 . ? C39 C40 1.373(9) . ? C39 H48A 0.9300 . ? C40 C41 1.373(7) . ? C40 H52A 0.9300 . ? C41 H49A 0.9300 . ? C42 C43 1.388(5) . ? C42 C47 1.411(5) . ? C42 B1 1.662(6) . ? C43 C44 1.389(5) . ? C43 H37A 0.9300 . ? C44 C45 1.374(5) . ? C44 H36A 0.9300 . ? C45 C46 1.389(6) . ? C45 H35A 0.9300 . ? C46 C47 1.388(5) . ? C46 H34A 0.9300 . ? C47 H33A 0.9300 . ? C48 C53 1.393(5) . ? C48 C49 1.406(6) . ? C48 B1 1.642(6) . ? C49 C50 1.387(7) . ? C49 H44A 0.9300 . ? C50 C51 1.390(7) . ? C50 H43A 0.9300 . ? C51 C52 1.383(7) . ? C51 H42A 0.9300 . ? C52 C53 1.385(6) . ? C52 H41A 0.9300 . ? C53 H40A 0.9300 . ? N1 Co1 1.968(3) . ? N2 Co1 2.117(4) . ? N3 Co1 2.028(4) . ? N4 Co1 2.122(4) . ? N5 Co1 2.012(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 N1 C1 C2 120.6(5) . . ? N1 C1 C23 116.2(4) . . ? C2 C1 C23 123.2(5) . . ? C1 C2 C3 120.6(6) . . ? C1 C2 H53A 119.7 . . ? C3 C2 H53A 119.7 . . ? C4 C3 C2 118.5(5) . . ? C4 C3 H54A 120.7 . . ? C2 C3 H54A 120.7 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H23A 120.0 . . ? C5 C4 H23A 120.0 . . ? N1 C5 C4 120.3(5) . . ? N1 C5 C11 116.3(4) . . ? C4 C5 C11 123.4(5) . . ? N2 C6 C7 124.4(4) . . ? N2 C6 H15A 117.8 . . ? C7 C6 H15A 117.8 . . ? C8 C7 C6 117.9(4) . . ? C8 C7 H16A 121.0 . . ? C6 C7 H16A 121.0 . . ? C7 C8 C9 118.9(5) . . ? C7 C8 H17A 120.5 . . ? C9 C8 H17A 120.5 . . ? C8 C9 C10 121.0(4) . . ? C8 C9 H18A 119.5 . . ? C10 C9 H18A 119.5 . . ? N2 C10 C9 120.2(4) . . ? N2 C10 C11 116.8(4) . . ? C9 C10 C11 123.1(4) . . ? C17 C11 C10 109.8(3) . . ? C17 C11 C5 110.7(4) . . ? C10 C11 C5 108.4(4) . . ? C17 C11 C12 108.5(4) . . ? C10 C11 C12 109.3(4) . . ? C5 C11 C12 110.1(4) . . ? C11 C12 H21A 109.5 . . ? C11 C12 H21B 109.5 . . ? H21A C12 H21B 109.5 . . ? C11 C12 H21C 109.5 . . ? H21A C12 H21C 109.5 . . ? H21B C12 H21C 109.5 . . ? N3 C13 C14 123.6(4) . . ? N3 C13 H1A 118.2 . . ? C14 C13 H1A 118.2 . . ? C13 C14 C15 118.5(4) . . ? C13 C14 H3A 120.7 . . ? C15 C14 H3A 120.7 . . ? C16 C15 C14 118.5(4) . . ? C16 C15 H4A 120.8 . . ? C14 C15 H4A 120.8 . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H5A 119.3 . . ? C17 C16 H5A 119.3 . . ? N3 C17 C16 119.3(4) . . ? N3 C17 C11 116.9(3) . . ? C16 C17 C11 123.7(4) . . ? N4 C18 C19 124.3(5) . . ? N4 C18 H50A 117.8 . . ? C19 C18 H50A 117.8 . . ? C20 C19 C18 118.5(4) . . ? C20 C19 H51A 120.8 . . ? C18 C19 H51A 120.8 . . ? C21 C20 C19 118.7(5) . . ? C21 C20 H11A 120.6 . . ? C19 C20 H11A 120.6 . . ? C20 C21 C22 120.3(5) . . ? C20 C21 H10A 119.9 . . ? C22 C21 H10A 119.9 . . ? N4 C22 C21 120.8(4) . . ? N4 C22 C23 117.9(4) . . ? C21 C22 C23 121.3(4) . . ? C29 C23 C22 107.4(3) . . ? C29 C23 C1 112.6(4) . . ? C22 C23 C1 109.1(4) . . ? C29 C23 C24 109.1(4) . . ? C22 C23 C24 109.8(4) . . ? C1 C23 C24 108.8(4) . . ? C23 C24 H25A 109.5 . . ? C23 C24 H25B 109.5 . . ? H25A C24 H25B 109.5 . . ? C23 C24 H25C 109.5 . . ? H25A C24 H25C 109.5 . . ? H25B C24 H25C 109.5 . . ? N5 C25 C26 123.3(4) . . ? N5 C25 H7A 118.4 . . ? C26 C25 H7A 118.4 . . ? C27 C26 C25 118.4(4) . . ? C27 C26 H8A 120.8 . . ? C25 C26 H8A 120.8 . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H12A 120.2 . . ? C28 C27 H12A 120.2 . . ? C27 C28 C29 119.9(5) . . ? C27 C28 H13A 120.0 . . ? C29 C28 H13A 120.0 . . ? N5 C29 C28 120.8(4) . . ? N5 C29 C23 116.5(4) . . ? C28 C29 C23 122.6(4) . . ? C31 C30 C35 114.6(3) . . ? C31 C30 B1 126.2(3) . . ? C35 C30 B1 119.2(3) . . ? C30 C31 C32 122.2(4) . . ? C30 C31 H28A 118.9 . . ? C32 C31 H28A 118.9 . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H29A 119.7 . . ? C31 C32 H29A 119.7 . . ? C32 C33 C34 118.9(4) . . ? C32 C33 H30A 120.6 . . ? C34 C33 H30A 120.6 . . ? C35 C34 C33 119.8(4) . . ? C35 C34 H31A 120.1 . . ? C33 C34 H31A 120.1 . . ? C34 C35 C30 124.0(4) . . ? C34 C35 H32A 118.0 . . ? C30 C35 H32A 118.0 . . ? C37 C36 C41 114.3(4) . . ? C37 C36 B1 126.2(4) . . ? C41 C36 B1 119.4(4) . . ? C36 C37 C38 122.5(5) . . ? C36 C37 H46A 118.7 . . ? C38 C37 H46A 118.7 . . ? C39 C38 C37 120.8(6) . . ? C39 C38 H47A 119.6 . . ? C37 C38 H47A 119.6 . . ? C38 C39 C40 118.5(5) . . ? C38 C39 H48A 120.7 . . ? C40 C39 H48A 120.7 . . ? C39 C40 C41 120.4(6) . . ? C39 C40 H52A 119.8 . . ? C41 C40 H52A 119.8 . . ? C40 C41 C36 123.4(6) . . ? C40 C41 H49A 118.3 . . ? C36 C41 H49A 118.3 . . ? C43 C42 C47 115.1(3) . . ? C43 C42 B1 125.4(3) . . ? C47 C42 B1 119.5(3) . . ? C42 C43 C44 122.6(4) . . ? C42 C43 H37A 118.7 . . ? C44 C43 H37A 118.7 . . ? C45 C44 C43 120.9(4) . . ? C45 C44 H36A 119.6 . . ? C43 C44 H36A 119.6 . . ? C44 C45 C46 118.9(4) . . ? C44 C45 H35A 120.6 . . ? C46 C45 H35A 120.6 . . ? C47 C46 C45 119.6(4) . . ? C47 C46 H34A 120.2 . . ? C45 C46 H34A 120.2 . . ? C46 C47 C42 123.0(4) . . ? C46 C47 H33A 118.5 . . ? C42 C47 H33A 118.5 . . ? C53 C48 C49 114.1(4) . . ? C53 C48 B1 123.8(4) . . ? C49 C48 B1 121.8(4) . . ? C50 C49 C48 123.3(4) . . ? C50 C49 H44A 118.3 . . ? C48 C49 H44A 118.3 . . ? C49 C50 C51 119.9(5) . . ? C49 C50 H43A 120.1 . . ? C51 C50 H43A 120.1 . . ? C52 C51 C50 118.6(5) . . ? C52 C51 H42A 120.7 . . ? C50 C51 H42A 120.7 . . ? C51 C52 C53 120.0(4) . . ? C51 C52 H41A 120.0 . . ? C53 C52 H41A 120.0 . . ? C52 C53 C48 123.9(4) . . ? C52 C53 H40A 118.0 . . ? C48 C53 H40A 118.0 . . ? C1 N1 C5 119.9(4) . . ? C1 N1 Co1 120.2(3) . . ? C5 N1 Co1 119.5(3) . . ? C6 N2 C10 117.4(4) . . ? C6 N2 Co1 126.3(3) . . ? C10 N2 Co1 115.9(3) . . ? C13 N3 C17 117.7(4) . . ? C13 N3 Co1 125.1(3) . . ? C17 N3 Co1 114.8(3) . . ? C18 N4 C22 117.4(4) . . ? C18 N4 Co1 126.9(3) . . ? C22 N4 Co1 115.6(3) . . ? C25 N5 C29 118.0(4) . . ? C25 N5 Co1 123.1(3) . . ? C29 N5 Co1 118.9(3) . . ? N1 Co1 N5 94.71(15) . . ? N1 Co1 N3 94.95(14) . . ? N5 Co1 N3 169.85(13) . . ? N1 Co1 N2 86.91(14) . . ? N5 Co1 N2 99.47(13) . . ? N3 Co1 N2 84.16(13) . . ? N1 Co1 N4 87.64(14) . . ? N5 Co1 N4 82.33(13) . . ? N3 Co1 N4 94.96(14) . . ? N2 Co1 N4 174.38(12) . . ? C36 B1 C48 106.7(3) . . ? C36 B1 C30 111.7(3) . . ? C48 B1 C30 113.1(3) . . ? C36 B1 C42 109.9(3) . . ? C48 B1 C42 110.3(3) . . ? C30 B1 C42 105.2(3) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 63.68 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.408 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.061 _iucr_refine_instructions_details ; TITL aek1071_0m in P-1 CELL 1.54178 10.9829 13.7142 17.0064 102.458 107.971 101.250 ZERR 4.00 0.0008 0.0009 0.0013 0.005 0.005 0.005 LATT 1 SFAC C H N CO B F O UNIT 106 90 10 2 2 0 0 MERG 2 FMAP 2 PLAN 20 SIZE 0.02 0.06 0.10 ACTA 134.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP 100.00 WGHT 0.088500 EXTI 0.000617 FVAR 1.78711 C1 1 0.794133 0.874917 0.719316 11.00000 0.02971 0.02688 = 0.08487 0.00659 0.01742 0.00612 C2 1 0.926443 0.877726 0.748644 11.00000 0.03730 0.03319 = 0.11216 0.01112 0.02031 0.00677 AFIX 43 H53A 2 0.974314 0.882046 0.712346 11.00000 -1.20000 AFIX 0 C3 1 0.989295 0.874189 0.831750 11.00000 0.03228 0.03615 = 0.14301 0.02759 0.00709 0.00818 AFIX 43 H54A 2 1.078791 0.875689 0.851615 11.00000 -1.20000 AFIX 0 C4 1 0.916102 0.868383 0.884494 11.00000 0.03766 0.03300 = 0.11276 0.02828 -0.00584 0.00413 AFIX 43 H23A 2 0.956635 0.866986 0.940844 11.00000 -1.20000 AFIX 0 C5 1 0.782263 0.864636 0.853491 11.00000 0.03860 0.03064 = 0.07950 0.02160 -0.00341 0.00455 C6 1 0.576415 1.085307 0.875518 11.00000 0.04065 0.03657 = 0.05214 0.02378 0.01590 0.00682 AFIX 43 H15A 2 0.541580 1.109914 0.829000 11.00000 -1.20000 AFIX 0 C7 1 0.600015 1.147065 0.957523 11.00000 0.04021 0.03696 = 0.05958 0.02031 0.00544 0.00556 AFIX 43 H16A 2 0.582233 1.211312 0.965864 11.00000 -1.20000 AFIX 0 C8 1 0.650459 1.110641 1.026181 11.00000 0.06663 0.03497 = 0.04883 0.01184 -0.01183 0.00607 AFIX 43 H17A 2 0.665164 1.148912 1.082181 11.00000 -1.20000 AFIX 0 C9 1 0.678919 1.016750 1.010936 11.00000 0.06350 0.03105 = 0.05180 0.01222 -0.01538 0.00254 AFIX 43 H18A 2 0.713499 0.991591 1.057149 11.00000 -1.20000 AFIX 0 C10 1 0.656800 0.958789 0.927463 11.00000 0.04263 0.02489 = 0.05041 0.01135 -0.00520 -0.00041 C11 1 0.692959 0.856055 0.907279 11.00000 0.04353 0.03074 = 0.05772 0.01930 -0.00340 0.00743 C12 1 0.768268 0.836607 0.992900 11.00000 0.06892 0.03831 = 0.06556 0.02202 -0.01124 0.01500 AFIX 33 H21A 2 0.791769 0.772701 0.980418 11.00000 -1.50000 H21B 2 0.712041 0.831936 1.026178 11.00000 -1.50000 H21C 2 0.847797 0.893096 1.025318 11.00000 -1.50000 AFIX 0 C13 1 0.349619 0.708752 0.753830 11.00000 0.03991 0.03679 = 0.05274 0.02067 0.00866 0.00068 AFIX 43 H1A 2 0.279962 0.723836 0.715519 11.00000 -1.20000 AFIX 0 C14 1 0.324419 0.614404 0.770309 11.00000 0.05849 0.03805 = 0.04891 0.01832 0.01362 -0.00080 AFIX 43 H3A 2 0.241572 0.565399 0.741058 11.00000 -1.20000 AFIX 0 C15 1 0.424879 0.594092 0.831247 11.00000 0.07404 0.03300 = 0.04444 0.01903 0.01606 0.00431 AFIX 43 H4A 2 0.412928 0.529661 0.841583 11.00000 -1.20000 AFIX 0 C16 1 0.542940 0.671276 0.876277 11.00000 0.06413 0.03562 = 0.04675 0.02030 0.00729 0.00996 AFIX 43 H5A 2 0.609038 0.660284 0.920229 11.00000 -1.20000 AFIX 0 C17 1 0.565693 0.765943 0.857370 11.00000 0.05212 0.03543 = 0.05003 0.02215 0.00490 0.01183 C18 1 0.388619 0.690287 0.572465 11.00000 0.04316 0.03487 = 0.06077 0.02061 0.00709 0.00216 AFIX 43 H50A 2 0.320665 0.684210 0.594440 11.00000 -1.20000 AFIX 0 C19 1 0.370081 0.615423 0.497686 11.00000 0.05620 0.04524 = 0.06556 0.02583 0.00107 0.00269 AFIX 43 H51A 2 0.290960 0.561981 0.469524 11.00000 -1.20000 AFIX 0 C20 1 0.471608 0.621754 0.465751 11.00000 0.05772 0.04557 = 0.06334 0.01453 0.00577 0.01352 AFIX 43 H11A 2 0.463857 0.571011 0.416928 11.00000 -1.20000 AFIX 0 C21 1 0.584555 0.704587 0.507521 11.00000 0.05109 0.04039 = 0.07812 0.01856 0.02334 0.01682 AFIX 43 H10A 2 0.653362 0.710756 0.486305 11.00000 -1.20000 AFIX 0 C22 1 0.596421 0.780277 0.582478 11.00000 0.04181 0.03099 = 0.07026 0.01281 0.01171 0.01020 C23 1 0.717874 0.877079 0.627255 11.00000 0.04453 0.03898 = 0.07482 0.01371 0.02791 0.00914 C24 1 0.812222 0.876496 0.575978 11.00000 0.05194 0.05236 = 0.11179 0.00608 0.04719 0.00771 AFIX 33 H25A 2 0.765486 0.877465 0.518364 11.00000 -1.50000 H25B 2 0.841721 0.814835 0.573364 11.00000 -1.50000 H25C 2 0.888020 0.936827 0.604379 11.00000 -1.50000 AFIX 0 C25 1 0.516750 1.059767 0.659656 11.00000 0.06241 0.03690 = 0.05272 0.02487 0.03145 0.02100 AFIX 43 H7A 2 0.453782 1.065520 0.685190 11.00000 -1.20000 AFIX 0 C26 1 0.544106 1.129549 0.615687 11.00000 0.10547 0.04206 = 0.08028 0.03625 0.06754 0.03547 AFIX 43 H8A 2 0.499536 1.180351 0.610796 11.00000 -1.20000 AFIX 0 C27 1 0.639114 1.122180 0.579161 11.00000 0.12549 0.04222 = 0.10087 0.03800 0.08509 0.02980 AFIX 43 H12A 2 0.662776 1.170311 0.551589 11.00000 -1.20000 AFIX 0 C28 1 0.698869 1.042880 0.583794 11.00000 0.08390 0.04290 = 0.09854 0.02062 0.06922 0.01112 AFIX 43 H13A 2 0.761362 1.036294 0.557983 11.00000 -1.20000 AFIX 0 C29 1 0.665628 0.972900 0.627030 11.00000 0.04791 0.03312 = 0.06920 0.01455 0.03569 0.00637 C30 1 0.633550 0.701118 0.186633 11.00000 0.03784 0.02621 = 0.03444 0.01723 0.01265 0.00779 C31 1 0.581113 0.645122 0.099127 11.00000 0.04914 0.02440 = 0.04060 0.01033 0.01865 0.00653 AFIX 43 H28A 2 0.638903 0.639216 0.069420 11.00000 -1.20000 AFIX 0 C32 1 0.444188 0.597410 0.054400 11.00000 0.05112 0.03071 = 0.03878 0.01211 0.00975 0.00445 AFIX 43 H29A 2 0.412939 0.560223 -0.003916 11.00000 -1.20000 AFIX 0 C33 1 0.355902 0.605113 0.095928 11.00000 0.03743 0.03414 = 0.05423 0.01320 0.00629 0.00196 AFIX 43 H30A 2 0.265240 0.572236 0.066596 11.00000 -1.20000 AFIX 0 C34 1 0.403906 0.662500 0.182011 11.00000 0.04577 0.05070 = 0.05916 0.00490 0.02617 0.00498 AFIX 43 H31A 2 0.345300 0.670308 0.210831 11.00000 -1.20000 AFIX 0 C35 1 0.538505 0.708013 0.224934 11.00000 0.04789 0.04448 = 0.04371 0.00567 0.01890 -0.00009 AFIX 43 H32A 2 0.568261 0.745731 0.283033 11.00000 -1.20000 AFIX 0 C36 1 0.848444 0.707724 0.323049 11.00000 0.05839 0.02679 = 0.03049 0.00760 -0.00014 0.01142 C37 1 0.771306 0.642298 0.352555 11.00000 0.08280 0.03519 = 0.04363 0.02062 0.00767 0.00389 AFIX 43 H46A 2 0.678950 0.623205 0.325713 11.00000 -1.20000 AFIX 0 C38 1 0.827070 0.604309 0.420728 11.00000 0.15061 0.03564 = 0.03736 0.01818 0.01729 0.02326 AFIX 43 H47A 2 0.771640 0.560514 0.438167 11.00000 -1.20000 AFIX 0 C39 1 0.961662 0.630441 0.462180 11.00000 0.15858 0.06940 = 0.02465 0.00956 -0.00129 0.06245 AFIX 43 H48A 2 0.998713 0.605674 0.508172 11.00000 -1.20000 AFIX 0 C40 1 1.041544 0.694161 0.434620 11.00000 0.10452 0.09681 = 0.04560 0.01311 -0.00708 0.06389 AFIX 43 H52A 2 1.133787 0.712458 0.461833 11.00000 -1.20000 AFIX 0 C41 1 0.985970 0.731037 0.367074 11.00000 0.06021 0.06200 = 0.04807 0.01034 0.00262 0.02786 AFIX 43 H49A 2 1.042774 0.773736 0.349718 11.00000 -1.20000 AFIX 0 C42 1 0.799327 0.882430 0.287957 11.00000 0.02932 0.02844 = 0.04018 0.01428 0.00966 0.00450 C43 1 0.850463 0.935647 0.375693 11.00000 0.03636 0.03879 = 0.04652 0.02236 0.01193 0.01071 AFIX 43 H37A 2 0.884776 0.901090 0.415023 11.00000 -1.20000 AFIX 0 C44 1 0.852417 1.038472 0.407077 11.00000 0.03358 0.03672 = 0.04361 0.01372 0.01487 0.00594 AFIX 43 H36A 2 0.888309 1.071091 0.466419 11.00000 -1.20000 AFIX 0 C45 1 0.802036 1.092591 0.351617 11.00000 0.04372 0.03243 = 0.05225 0.01858 0.02460 0.01040 AFIX 43 H35A 2 0.803558 1.161410 0.372923 11.00000 -1.20000 AFIX 0 C46 1 0.748769 1.042755 0.263148 11.00000 0.04944 0.03426 = 0.05002 0.02408 0.02364 0.01759 AFIX 43 H34A 2 0.714231 1.078026 0.224495 11.00000 -1.20000 AFIX 0 C47 1 0.747440 0.939989 0.232838 11.00000 0.03755 0.03400 = 0.04350 0.01813 0.01674 0.00744 AFIX 43 H33A 2 0.710662 0.907560 0.173467 11.00000 -1.20000 AFIX 0 C48 1 0.889356 0.753727 0.189001 11.00000 0.03854 0.03083 = 0.05808 0.01804 0.01692 0.01039 C49 1 0.894210 0.658323 0.140941 11.00000 0.06433 0.03932 = 0.13968 0.03554 0.06603 0.01675 AFIX 43 H44A 2 0.836659 0.597412 0.138765 11.00000 -1.20000 AFIX 0 C50 1 0.980492 0.650395 0.096582 11.00000 0.10655 0.04703 = 0.19948 0.03726 0.11396 0.03347 AFIX 43 H43A 2 0.976021 0.585768 0.062723 11.00000 -1.20000 AFIX 0 C51 1 1.073650 0.739227 0.102831 11.00000 0.06653 0.06161 = 0.14692 0.05477 0.07725 0.03264 AFIX 43 H42A 2 1.134949 0.734529 0.075753 11.00000 -1.20000 AFIX 0 C52 1 1.073252 0.834708 0.150151 11.00000 0.03829 0.04458 = 0.07362 0.03247 0.02310 0.01015 AFIX 43 H41A 2 1.134439 0.895141 0.154942 11.00000 -1.20000 AFIX 0 C53 1 0.981694 0.840302 0.190405 11.00000 0.04114 0.04035 = 0.04616 0.02232 0.01268 0.01069 AFIX 43 H40A 2 0.981846 0.905764 0.220158 11.00000 -1.20000 AFIX 0 N1 3 0.722658 0.868895 0.771366 11.00000 0.03563 0.02200 = 0.07281 0.01233 0.00907 0.00636 N2 3 0.600346 0.992404 0.858552 11.00000 0.03467 0.03443 = 0.05561 0.02810 0.01295 0.00936 N3 3 0.470049 0.780758 0.790250 11.00000 0.04109 0.03746 = 0.05644 0.02397 0.00545 0.00535 N4 3 0.498457 0.771381 0.615583 11.00000 0.03658 0.03558 = 0.06562 0.02639 0.01183 0.00973 N5 3 0.576995 0.983288 0.667507 11.00000 0.04257 0.03407 = 0.05323 0.01916 0.02268 0.00948 CO1 4 0.540891 0.884278 0.734773 11.00000 0.03279 0.03075 = 0.05297 0.02373 0.01204 0.00624 B1 5 0.792449 0.759427 0.245552 11.00000 0.04078 0.03071 = 0.04183 0.01911 0.01465 0.01043 HKLF 4 REM aek1071_0m in P-1 REM R1 = 0.0625 for 4707 Fo > 4sig(Fo) and 0.0957 for all 7242 data REM 542 parameters refined using 0 restraints END WGHT 0.0888 0.0000 REM Highest difference peak 0.408, deepest hole -0.402, 1-sigma level 0.061 Q1 1 0.6198 0.9125 0.7344 11.00000 0.05 0.41 Q2 1 0.4536 0.8564 0.7414 11.00000 0.05 0.30 Q3 1 0.5793 0.8392 0.8140 11.00000 0.05 0.29 Q4 1 0.4984 0.8920 0.8316 11.00000 0.05 0.28 Q5 1 0.6479 0.9184 0.8307 11.00000 0.05 0.28 Q6 1 0.2053 0.3877 0.3301 11.00000 0.05 0.27 Q7 1 0.6833 0.9147 0.7919 11.00000 0.05 0.27 Q8 1 0.2594 0.4011 0.2861 11.00000 0.05 0.27 Q9 1 0.8034 0.6472 0.6114 11.00000 0.05 0.26 Q10 1 0.7919 0.9061 0.7708 11.00000 0.05 0.26 Q11 1 0.6652 1.0825 0.2099 11.00000 0.05 0.25 Q12 1 1.0258 0.6596 0.1475 11.00000 0.05 0.25 Q13 1 0.4192 0.8333 0.7849 11.00000 0.05 0.24 Q14 1 0.6540 0.8361 0.6187 11.00000 0.05 0.24 Q15 1 1.2295 0.9336 0.1966 11.00000 0.05 0.23 Q16 1 0.5124 0.9285 0.6553 11.00000 0.05 0.23 Q17 1 0.7518 1.0023 0.7241 11.00000 0.05 0.23 Q18 1 1.0265 0.5858 0.6524 11.00000 0.05 0.23 Q19 1 0.7337 0.5800 0.4251 11.00000 0.05 0.23 Q20 1 0.3934 0.8476 0.6684 11.00000 0.05 0.22 ; # 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 0.105 0.423 0.236 194 58 ' ' 2 -0.105 0.577 0.764 194 58 ' ' _platon_squeeze_details ; ; data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 915156' #TrackingRef '16057_web_deposit_cif_file_1_AmandaKing_1355197332.aek1145cooac.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AEK1145CoOAc _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H28 Cl0 Co F6 N5 O8 S2' _chemical_formula_weight 859.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9400(3) _cell_length_b 12.8220(3) _cell_length_c 15.3280(3) _cell_angle_alpha 65.6960(10) _cell_angle_beta 78.9150(10) _cell_angle_gamma 66.5570(10) _cell_volume 1960.99(8) _cell_formula_units_Z 2 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 9799 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.36 _exptl_crystal_description Needles _exptl_crystal_colour pink _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9084 _exptl_absorpt_correction_T_max 0.9584 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocused sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 33375 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.39 _reflns_number_total 7167 _reflns_number_gt 6288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.0429P)^2^+1.7504P] 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 7167 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7385(2) 0.36940(19) 0.23719(15) 0.0174(4) Uani 1 1 d . . . C2 C 0.6309(2) 0.4688(2) 0.21187(16) 0.0235(5) Uani 1 1 d . . . H2 H 0.5885 0.5059 0.2553 0.028 Uiso 1 1 calc R . . C3 C 0.5867(2) 0.5127(2) 0.12206(17) 0.0249(5) Uani 1 1 d . . . H3 H 0.5151 0.5804 0.1038 0.030 Uiso 1 1 calc R . . C4 C 0.6500(2) 0.4551(2) 0.05985(16) 0.0207(5) Uani 1 1 d . . . H4 H 0.6203 0.4819 -0.0004 0.025 Uiso 1 1 calc R . . C5 C 0.75868(19) 0.35657(19) 0.08768(14) 0.0164(4) Uani 1 1 d . . . C6 C 0.7902(2) 0.31766(19) 0.33579(15) 0.0185(5) Uani 1 1 d . . . C7 C 0.7009(2) 0.3809(2) 0.40103(16) 0.0258(5) Uani 1 1 d . . . H7A H 0.6882 0.4667 0.3738 0.039 Uiso 1 1 calc R . . H7B H 0.7345 0.3453 0.4632 0.039 Uiso 1 1 calc R . . H7C H 0.6244 0.3701 0.4068 0.039 Uiso 1 1 calc R . . C8 C 0.8174(2) 0.1788(2) 0.38147(15) 0.0182(4) Uani 1 1 d . . . C9 C 0.7612(2) 0.1253(2) 0.46682(16) 0.0267(5) Uani 1 1 d . . . H9 H 0.6967 0.1743 0.4938 0.032 Uiso 1 1 calc R . . C10 C 0.8009(2) -0.0004(2) 0.51176(17) 0.0305(6) Uani 1 1 d . . . H10 H 0.7611 -0.0372 0.5673 0.037 Uiso 1 1 calc R . . C11 C 0.9005(2) -0.0703(2) 0.47292(16) 0.0266(5) Uani 1 1 d . . . H11 H 0.9327 -0.1550 0.5040 0.032 Uiso 1 1 calc R . . C12 C 0.9518(2) -0.01280(19) 0.38703(15) 0.0192(5) Uani 1 1 d . . . H12 H 1.0202 -0.0601 0.3616 0.023 Uiso 1 1 calc R . . C13 C 0.9131(2) 0.33467(18) 0.32341(15) 0.0182(5) Uani 1 1 d . . . C14 C 0.9341(2) 0.3988(2) 0.36880(16) 0.0239(5) Uani 1 1 d . . . H14 H 0.8708 0.4386 0.4029 0.029 Uiso 1 1 calc R . . C15 C 1.0490(2) 0.4035(2) 0.36334(16) 0.0275(5) Uani 1 1 d . . . H15 H 1.0638 0.4471 0.3929 0.033 Uiso 1 1 calc R . . C16 C 1.1411(2) 0.3426(2) 0.31346(16) 0.0268(5) Uani 1 1 d . . . H16 H 1.2195 0.3433 0.3094 0.032 Uiso 1 1 calc R . . C17 C 1.1153(2) 0.2803(2) 0.26933(15) 0.0213(5) Uani 1 1 d . . . H17 H 1.1785 0.2371 0.2373 0.026 Uiso 1 1 calc R . . C18 C 0.8346(2) 0.29213(19) 0.02020(14) 0.0175(4) Uani 1 1 d . . . C19 C 0.7678(2) 0.3432(2) -0.07290(15) 0.0218(5) Uani 1 1 d . . . H19A H 0.7538 0.4291 -0.1043 0.033 Uiso 1 1 calc R . . H19B H 0.6909 0.3311 -0.0583 0.033 Uiso 1 1 calc R . . H19C H 0.8168 0.3013 -0.1143 0.033 Uiso 1 1 calc R . . C20 C 0.9557(2) 0.31278(19) -0.00036(15) 0.0187(5) Uani 1 1 d . . . C21 C 0.9956(2) 0.3696(2) -0.09282(16) 0.0244(5) Uani 1 1 d . . . H21 H 0.9468 0.3983 -0.1443 0.029 Uiso 1 1 calc R . . C22 C 1.1070(3) 0.3836(2) -0.10824(18) 0.0344(6) Uani 1 1 d . . . H22 H 1.1337 0.4227 -0.1698 0.041 Uiso 1 1 calc R . . C23 C 1.1779(3) 0.3387(3) -0.03115(19) 0.0392(7) Uani 1 1 d . . . H23 H 1.2539 0.3464 -0.0396 0.047 Uiso 1 1 calc R . . C24 C 1.1350(2) 0.2822(2) 0.05889(17) 0.0284(5) Uani 1 1 d . . . H24 H 1.1844 0.2502 0.1106 0.034 Uiso 1 1 calc R . . C25 C 0.86172(19) 0.15366(19) 0.06946(14) 0.0170(4) Uani 1 1 d . . . C26 C 0.8254(2) 0.0909(2) 0.03195(16) 0.0215(5) Uani 1 1 d . . . H26 H 0.7794 0.1334 -0.0228 0.026 Uiso 1 1 calc R . . C27 C 0.8573(2) -0.0345(2) 0.07573(17) 0.0254(5) Uani 1 1 d . . . H27 H 0.8311 -0.0771 0.0523 0.030 Uiso 1 1 calc R . . C28 C 0.9290(2) -0.0954(2) 0.15476(16) 0.0231(5) Uani 1 1 d . . . H28 H 0.9538 -0.1801 0.1847 0.028 Uiso 1 1 calc R . . C29 C 0.9631(2) -0.0287(2) 0.18858(15) 0.0202(5) Uani 1 1 d . . . H29 H 1.0131 -0.0706 0.2410 0.024 Uiso 1 1 calc R . . C30 C 1.2086(2) 0.0071(2) 0.19891(18) 0.0279(5) Uani 1 1 d . . . C31 C 1.3194(3) -0.0790(2) 0.2596(2) 0.0371(6) Uani 1 1 d . . . H31A H 1.3759 -0.1307 0.2275 0.056 Uiso 1 1 calc R . . H31B H 1.2942 -0.1287 0.3205 0.056 Uiso 1 1 calc R . . H31C H 1.3583 -0.0321 0.2694 0.056 Uiso 1 1 calc R . . C32 C 0.5497(3) 0.1330(3) 0.2497(2) 0.0511(9) Uani 1 1 d . . . C33 C 0.6747(2) 0.4153(2) 0.67567(19) 0.0326(6) Uani 1 1 d . . . N1 N 0.80374(16) 0.31567(15) 0.17495(12) 0.0155(4) Uani 1 1 d . . . N2 N 0.90681(16) 0.10900(16) 0.33858(12) 0.0165(4) Uani 1 1 d . . . N3 N 1.00245(16) 0.27931(15) 0.27069(12) 0.0169(4) Uani 1 1 d . . . N4 N 1.02512(17) 0.27108(16) 0.07548(12) 0.0187(4) Uani 1 1 d . . . N5 N 0.92772(16) 0.09412(16) 0.14961(12) 0.0170(4) Uani 1 1 d . . . O1 O 0.54396(17) 0.25043(18) 0.06750(14) 0.0434(5) Uani 1 1 d . . . O2 O 0.3880(2) 0.1647(2) 0.14668(17) 0.0587(6) Uani 1 1 d . . . O3 O 0.3872(3) 0.34046(19) 0.16619(17) 0.0746(9) Uani 1 1 d . . . O4 O 0.83546(17) 0.46896(15) 0.54758(11) 0.0293(4) Uani 1 1 d . . . O5 O 0.85066(16) 0.25659(14) 0.62054(12) 0.0289(4) Uani 1 1 d . . . O6 O 0.89825(16) 0.35009(16) 0.71138(11) 0.0314(4) Uani 1 1 d . . . O7 O 1.12446(14) 0.06815(14) 0.24449(10) 0.0205(3) Uani 1 1 d . . . O9 O 1.20265(17) 0.01581(18) 0.11702(13) 0.0390(5) Uani 1 1 d . . . F1 F 0.6198(2) 0.0255(2) 0.24059(17) 0.0898(8) Uani 1 1 d . . . F2 F 0.6240(3) 0.1781(3) 0.26052(17) 0.1314(14) Uani 1 1 d . . . F3 F 0.4816(2) 0.10684(19) 0.32880(13) 0.0667(6) Uani 1 1 d . . . F4 F 0.59970(14) 0.43219(16) 0.61298(12) 0.0474(4) Uani 1 1 d . . . F5 F 0.64191(16) 0.52126(16) 0.68790(14) 0.0530(5) Uani 1 1 d . . . F6 F 0.65424(15) 0.33392(16) 0.75874(11) 0.0430(4) Uani 1 1 d . . . S1 S 0.45748(6) 0.23327(6) 0.14528(5) 0.03056(15) Uani 1 1 d . . . S2 S 0.83352(5) 0.36690(5) 0.63405(4) 0.02329(14) Uani 1 1 d . . . Co1 Co 0.96765(3) 0.18774(2) 0.206869(18) 0.01394(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0195(11) 0.0162(10) 0.0159(10) -0.0050(9) -0.0013(9) -0.0066(9) C2 0.0226(12) 0.0243(12) 0.0215(11) -0.0110(10) -0.0012(9) -0.0036(10) C3 0.0191(12) 0.0240(12) 0.0256(12) -0.0082(10) -0.0061(9) -0.0003(10) C4 0.0193(11) 0.0235(11) 0.0174(11) -0.0051(9) -0.0058(9) -0.0060(9) C5 0.0188(11) 0.0170(10) 0.0134(10) -0.0036(8) -0.0017(8) -0.0081(9) C6 0.0205(11) 0.0174(11) 0.0143(10) -0.0063(9) -0.0011(9) -0.0028(9) C7 0.0291(13) 0.0252(12) 0.0176(11) -0.0106(10) -0.0022(10) -0.0011(10) C8 0.0183(11) 0.0209(11) 0.0142(10) -0.0058(9) -0.0037(8) -0.0052(9) C9 0.0251(12) 0.0272(12) 0.0183(11) -0.0046(10) 0.0012(9) -0.0051(10) C10 0.0344(14) 0.0310(13) 0.0171(11) -0.0001(10) 0.0026(10) -0.0137(11) C11 0.0373(14) 0.0196(11) 0.0215(12) -0.0023(10) -0.0072(10) -0.0114(11) C12 0.0238(12) 0.0168(11) 0.0179(11) -0.0067(9) -0.0040(9) -0.0063(9) C13 0.0252(12) 0.0117(10) 0.0132(10) -0.0013(8) -0.0067(9) -0.0030(9) C14 0.0373(14) 0.0157(11) 0.0160(11) -0.0041(9) -0.0059(10) -0.0064(10) C15 0.0482(16) 0.0192(11) 0.0198(11) -0.0027(10) -0.0109(11) -0.0171(11) C16 0.0369(14) 0.0263(12) 0.0211(12) -0.0014(10) -0.0091(10) -0.0191(11) C17 0.0261(12) 0.0216(11) 0.0164(11) -0.0028(9) -0.0036(9) -0.0119(10) C18 0.0211(11) 0.0170(10) 0.0122(10) -0.0022(8) -0.0037(8) -0.0066(9) C19 0.0255(12) 0.0223(11) 0.0148(11) -0.0056(9) -0.0049(9) -0.0052(10) C20 0.0232(12) 0.0142(10) 0.0176(11) -0.0047(9) -0.0026(9) -0.0062(9) C21 0.0322(13) 0.0208(11) 0.0179(11) -0.0018(9) -0.0022(10) -0.0120(10) C22 0.0441(16) 0.0412(15) 0.0201(12) -0.0017(11) 0.0041(11) -0.0300(13) C23 0.0388(16) 0.0554(18) 0.0309(14) -0.0072(13) 0.0031(12) -0.0353(14) C24 0.0276(13) 0.0371(14) 0.0232(12) -0.0059(11) -0.0023(10) -0.0191(11) C25 0.0174(11) 0.0198(11) 0.0140(10) -0.0064(9) 0.0008(8) -0.0072(9) C26 0.0218(12) 0.0255(12) 0.0184(11) -0.0096(10) -0.0023(9) -0.0073(10) C27 0.0287(13) 0.0287(13) 0.0274(12) -0.0154(11) 0.0001(10) -0.0141(11) C28 0.0274(13) 0.0185(11) 0.0228(12) -0.0073(9) 0.0009(10) -0.0088(10) C29 0.0212(12) 0.0180(11) 0.0173(11) -0.0048(9) -0.0011(9) -0.0047(9) C30 0.0264(13) 0.0271(13) 0.0348(14) -0.0131(11) -0.0005(11) -0.0127(11) C31 0.0407(16) 0.0336(14) 0.0406(15) -0.0151(12) 0.0016(12) -0.0168(13) C32 0.0520(19) 0.057(2) 0.0401(17) 0.0068(15) -0.0108(14) -0.0371(18) C33 0.0371(15) 0.0345(14) 0.0336(14) -0.0205(12) -0.0022(12) -0.0116(12) N1 0.0179(9) 0.0139(9) 0.0143(9) -0.0038(7) -0.0009(7) -0.0067(7) N2 0.0180(9) 0.0165(9) 0.0165(9) -0.0064(7) -0.0043(7) -0.0058(7) N3 0.0216(10) 0.0132(9) 0.0132(8) -0.0012(7) -0.0046(7) -0.0057(7) N4 0.0215(10) 0.0182(9) 0.0171(9) -0.0047(8) -0.0025(7) -0.0090(8) N5 0.0168(9) 0.0183(9) 0.0153(9) -0.0044(7) -0.0004(7) -0.0076(8) O1 0.0314(10) 0.0431(11) 0.0371(11) -0.0008(9) 0.0033(8) -0.0117(9) O2 0.0503(13) 0.0641(15) 0.0635(15) -0.0034(12) -0.0148(11) -0.0376(12) O3 0.101(2) 0.0278(11) 0.0508(14) -0.0064(10) 0.0261(14) -0.0012(12) O4 0.0456(11) 0.0235(9) 0.0190(8) -0.0075(7) -0.0060(7) -0.0109(8) O5 0.0355(10) 0.0181(8) 0.0312(9) -0.0113(7) -0.0025(8) -0.0050(7) O6 0.0388(10) 0.0339(10) 0.0205(8) -0.0047(7) -0.0074(7) -0.0147(8) O7 0.0233(8) 0.0222(8) 0.0175(8) -0.0062(6) -0.0017(6) -0.0104(7) O9 0.0341(10) 0.0517(12) 0.0368(11) -0.0270(9) -0.0007(8) -0.0103(9) F1 0.0536(13) 0.0623(14) 0.0791(16) 0.0171(12) -0.0111(11) 0.0111(11) F2 0.176(3) 0.185(3) 0.0652(15) 0.0328(17) -0.0600(17) -0.153(3) F3 0.0880(15) 0.0694(13) 0.0337(10) 0.0018(9) -0.0002(10) -0.0419(12) F4 0.0302(9) 0.0614(11) 0.0538(10) -0.0312(9) -0.0099(8) -0.0055(8) F5 0.0493(10) 0.0457(10) 0.0764(13) -0.0457(10) 0.0143(9) -0.0127(8) F6 0.0473(10) 0.0576(10) 0.0371(9) -0.0253(8) 0.0112(7) -0.0291(8) S1 0.0251(3) 0.0249(3) 0.0324(3) -0.0026(3) -0.0005(3) -0.0084(3) S2 0.0285(3) 0.0215(3) 0.0194(3) -0.0079(2) -0.0029(2) -0.0070(2) Co1 0.01686(16) 0.01424(15) 0.01132(15) -0.00389(11) -0.00150(11) -0.00658(12) _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 C1 N1 1.349(3) . ? C1 C2 1.381(3) . ? C1 C6 1.521(3) . ? C2 C3 1.376(3) . ? C2 H2 0.9300 . ? C3 C4 1.372(3) . ? C3 H3 0.9300 . ? C4 C5 1.389(3) . ? C4 H4 0.9300 . ? C5 N1 1.352(3) . ? C5 C18 1.524(3) . ? C6 C13 1.533(3) . ? C6 C7 1.537(3) . ? C6 C8 1.538(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N2 1.352(3) . ? C8 C9 1.387(3) . ? C9 C10 1.379(3) . ? C9 H9 0.9300 . ? C10 C11 1.375(4) . ? C10 H10 0.9300 . ? C11 C12 1.379(3) . ? C11 H11 0.9300 . ? C12 N2 1.345(3) . ? C12 H12 0.9300 . ? C13 N3 1.354(3) . ? C13 C14 1.387(3) . ? C14 C15 1.383(4) . ? C14 H14 0.9300 . ? C15 C16 1.374(4) . ? C15 H15 0.9300 . ? C16 C17 1.383(3) . ? C16 H16 0.9300 . ? C17 N3 1.348(3) . ? C17 H17 0.9300 . ? C18 C20 1.524(3) . ? C18 C19 1.535(3) . ? C18 C25 1.536(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N4 1.353(3) . ? C20 C21 1.390(3) . ? C21 C22 1.375(3) . ? C21 H21 0.9300 . ? C22 C23 1.372(4) . ? C22 H22 0.9300 . ? C23 C24 1.376(3) . ? C23 H23 0.9300 . ? C24 N4 1.340(3) . ? C24 H24 0.9300 . ? C25 N5 1.355(3) . ? C25 C26 1.386(3) . ? C26 C27 1.380(3) . ? C26 H26 0.9300 . ? C27 C28 1.377(3) . ? C27 H27 0.9300 . ? C28 C29 1.374(3) . ? C28 H28 0.9300 . ? C29 N5 1.345(3) . ? C29 H29 0.9300 . ? C30 O9 1.227(3) . ? C30 O7 1.291(3) . ? C30 C31 1.517(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 F2 1.301(4) . ? C32 F3 1.322(4) . ? C32 F1 1.347(4) . ? C32 S1 1.812(3) . ? C33 F6 1.327(3) . ? C33 F4 1.334(3) . ? C33 F5 1.338(3) . ? C33 S2 1.820(3) . ? N1 Co1 1.9782(18) . ? N2 Co1 1.9911(18) . ? N3 Co1 1.9995(18) . ? N4 Co1 1.9873(18) . ? N5 Co1 1.9804(18) . ? O1 S1 1.4239(19) . ? O2 S1 1.421(2) . ? O3 S1 1.427(2) . ? O4 S2 1.4333(17) . ? O5 S2 1.4421(17) . ? O6 S2 1.4347(17) . ? O7 Co1 1.8954(15) . ? 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 N1 C1 C2 121.55(19) . . ? N1 C1 C6 117.06(18) . . ? C2 C1 C6 121.38(19) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.4(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C18 116.96(18) . . ? C4 C5 C18 121.54(18) . . ? C1 C6 C13 108.30(17) . . ? C1 C6 C7 110.96(18) . . ? C13 C6 C7 111.10(18) . . ? C1 C6 C8 109.90(17) . . ? C13 C6 C8 106.42(17) . . ? C7 C6 C8 110.04(18) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 120.7(2) . . ? N2 C8 C6 116.75(18) . . ? C9 C8 C6 122.3(2) . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 118.7(2) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 118.8(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N2 C12 C11 122.6(2) . . ? N2 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? N3 C13 C14 121.2(2) . . ? N3 C13 C6 117.49(18) . . ? C14 C13 C6 121.2(2) . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 118.7(2) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 119.0(2) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N3 C17 C16 122.8(2) . . ? N3 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C20 C18 C5 107.30(17) . . ? C20 C18 C19 110.72(17) . . ? C5 C18 C19 110.71(18) . . ? C20 C18 C25 108.03(17) . . ? C5 C18 C25 109.96(16) . . ? C19 C18 C25 110.05(17) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 C21 120.8(2) . . ? N4 C20 C18 117.10(18) . . ? C21 C20 C18 122.09(19) . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 118.7(2) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 119.0(2) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? N4 C24 C23 123.0(2) . . ? N4 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? N5 C25 C26 121.12(19) . . ? N5 C25 C18 116.82(18) . . ? C26 C25 C18 121.99(19) . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 118.6(2) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C29 C28 C27 118.9(2) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? N5 C29 C28 123.2(2) . . ? N5 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? O9 C30 O7 125.7(2) . . ? O9 C30 C31 123.1(2) . . ? O7 C30 C31 111.2(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? F2 C32 F3 109.4(3) . . ? F2 C32 F1 106.5(3) . . ? F3 C32 F1 106.5(2) . . ? F2 C32 S1 112.4(2) . . ? F3 C32 S1 111.8(2) . . ? F1 C32 S1 109.9(2) . . ? F6 C33 F4 107.3(2) . . ? F6 C33 F5 107.2(2) . . ? F4 C33 F5 107.4(2) . . ? F6 C33 S2 112.19(18) . . ? F4 C33 S2 111.43(17) . . ? F5 C33 S2 111.00(18) . . ? C1 N1 C5 118.74(18) . . ? C1 N1 Co1 120.72(14) . . ? C5 N1 Co1 120.39(14) . . ? C12 N2 C8 118.30(18) . . ? C12 N2 Co1 122.01(15) . . ? C8 N2 Co1 119.68(14) . . ? C17 N3 C13 118.05(18) . . ? C17 N3 Co1 122.08(15) . . ? C13 N3 Co1 119.67(14) . . ? C24 N4 C20 118.31(19) . . ? C24 N4 Co1 121.45(15) . . ? C20 N4 Co1 120.16(14) . . ? C29 N5 C25 117.92(18) . . ? C29 N5 Co1 121.96(14) . . ? C25 N5 Co1 120.11(14) . . ? C30 O7 Co1 130.79(15) . . ? O2 S1 O1 115.84(14) . . ? O2 S1 O3 113.95(17) . . ? O1 S1 O3 114.54(13) . . ? O2 S1 C32 102.36(13) . . ? O1 S1 C32 104.46(14) . . ? O3 S1 C32 103.46(17) . . ? O4 S2 O6 115.04(10) . . ? O4 S2 O5 114.93(10) . . ? O6 S2 O5 115.50(10) . . ? O4 S2 C33 102.56(12) . . ? O6 S2 C33 102.85(11) . . ? O5 S2 C33 103.33(11) . . ? O7 Co1 N1 176.14(7) . . ? O7 Co1 N5 93.99(7) . . ? N1 Co1 N5 89.40(7) . . ? O7 Co1 N4 93.99(7) . . ? N1 Co1 N4 88.11(7) . . ? N5 Co1 N4 85.55(7) . . ? O7 Co1 N2 87.33(7) . . ? N1 Co1 N2 90.51(7) . . ? N5 Co1 N2 95.39(7) . . ? N4 Co1 N2 178.33(7) . . ? O7 Co1 N3 86.64(7) . . ? N1 Co1 N3 89.88(7) . . ? N5 Co1 N3 176.99(7) . . ? N4 Co1 N3 97.34(7) . . ? N2 Co1 N3 81.69(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.628 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.058 # 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 0.500 0.000 1.000 392 95 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL AEK1145CoOAc in P-1 CELL 0.71073 11.9400 12.8220 15.3280 65.696 78.915 66.557 ZERR 2.00 0.0003 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H N O F S CO CL UNIT 54 48 10 12 12 4 2 0 MERG 2 FMAP 2 PLAN 20 SIZE 0.07 0.10 0.16 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP 100.00 WGHT 0.042900 1.750400 FVAR 1.63496 C1 1 0.738457 0.369401 0.237189 11.00000 0.01953 0.01622 = 0.01592 -0.00503 -0.00127 -0.00656 C2 1 0.630883 0.468808 0.211872 11.00000 0.02265 0.02432 = 0.02147 -0.01099 -0.00125 -0.00360 AFIX 43 H2 2 0.588466 0.505907 0.255287 11.00000 -1.20000 AFIX 0 C3 1 0.586740 0.512720 0.122064 11.00000 0.01905 0.02396 = 0.02563 -0.00825 -0.00615 -0.00031 AFIX 43 H3 2 0.515101 0.580431 0.103807 11.00000 -1.20000 AFIX 0 C4 1 0.649960 0.455148 0.059855 11.00000 0.01927 0.02351 = 0.01743 -0.00512 -0.00584 -0.00601 AFIX 43 H4 2 0.620253 0.481916 -0.000404 11.00000 -1.20000 AFIX 0 C5 1 0.758682 0.356570 0.087678 11.00000 0.01885 0.01696 = 0.01341 -0.00357 -0.00172 -0.00814 C6 1 0.790168 0.317662 0.335790 11.00000 0.02049 0.01740 = 0.01429 -0.00635 -0.00110 -0.00281 C7 1 0.700936 0.380886 0.401028 11.00000 0.02914 0.02521 = 0.01764 -0.01058 -0.00221 -0.00109 AFIX 137 H7A 2 0.688156 0.466726 0.373814 11.00000 -1.50000 H7B 2 0.734507 0.345349 0.463239 11.00000 -1.50000 H7C 2 0.624413 0.370071 0.406775 11.00000 -1.50000 AFIX 0 C8 1 0.817444 0.178836 0.381466 11.00000 0.01829 0.02092 = 0.01422 -0.00578 -0.00366 -0.00518 C9 1 0.761224 0.125303 0.466824 11.00000 0.02513 0.02723 = 0.01834 -0.00462 0.00118 -0.00508 AFIX 43 H9 2 0.696692 0.174260 0.493793 11.00000 -1.20000 AFIX 0 C10 1 0.800880 -0.000412 0.511759 11.00000 0.03445 0.03097 = 0.01714 -0.00013 0.00261 -0.01372 AFIX 43 H10 2 0.761054 -0.037201 0.567256 11.00000 -1.20000 AFIX 0 C11 1 0.900471 -0.070345 0.472917 11.00000 0.03728 0.01956 = 0.02146 -0.00232 -0.00722 -0.01145 AFIX 43 H11 2 0.932671 -0.154956 0.504015 11.00000 -1.20000 AFIX 0 C12 1 0.951762 -0.012799 0.387028 11.00000 0.02382 0.01684 = 0.01790 -0.00674 -0.00403 -0.00631 AFIX 43 H12 2 1.020163 -0.060090 0.361586 11.00000 -1.20000 AFIX 0 C13 1 0.913102 0.334668 0.323410 11.00000 0.02520 0.01172 = 0.01321 -0.00129 -0.00671 -0.00296 C14 1 0.934057 0.398806 0.368795 11.00000 0.03728 0.01568 = 0.01604 -0.00414 -0.00591 -0.00640 AFIX 43 H14 2 0.870818 0.438629 0.402877 11.00000 -1.20000 AFIX 0 C15 1 1.049039 0.403499 0.363336 11.00000 0.04823 0.01921 = 0.01976 -0.00269 -0.01086 -0.01713 AFIX 43 H15 2 1.063778 0.447061 0.392871 11.00000 -1.20000 AFIX 0 C16 1 1.141070 0.342594 0.313457 11.00000 0.03689 0.02626 = 0.02114 -0.00139 -0.00909 -0.01906 AFIX 43 H16 2 1.219511 0.343273 0.309434 11.00000 -1.20000 AFIX 0 C17 1 1.115267 0.280271 0.269331 11.00000 0.02610 0.02156 = 0.01641 -0.00276 -0.00363 -0.01194 AFIX 43 H17 2 1.178483 0.237146 0.237329 11.00000 -1.20000 AFIX 0 C18 1 0.834615 0.292133 0.020201 11.00000 0.02110 0.01701 = 0.01224 -0.00221 -0.00369 -0.00656 C19 1 0.767779 0.343173 -0.072897 11.00000 0.02551 0.02230 = 0.01480 -0.00564 -0.00494 -0.00517 AFIX 137 H19A 2 0.753787 0.429109 -0.104310 11.00000 -1.50000 H19B 2 0.690938 0.331081 -0.058330 11.00000 -1.50000 H19C 2 0.816805 0.301258 -0.114291 11.00000 -1.50000 AFIX 0 C20 1 0.955722 0.312783 -0.000357 11.00000 0.02318 0.01424 = 0.01759 -0.00465 -0.00262 -0.00621 C21 1 0.995561 0.369638 -0.092819 11.00000 0.03220 0.02076 = 0.01785 -0.00184 -0.00224 -0.01198 AFIX 43 H21 2 0.946798 0.398282 -0.144316 11.00000 -1.20000 AFIX 0 C22 1 1.106963 0.383582 -0.108238 11.00000 0.04411 0.04115 = 0.02013 -0.00165 0.00414 -0.02998 AFIX 43 H22 2 1.133719 0.422670 -0.169754 11.00000 -1.20000 AFIX 0 C23 1 1.177894 0.338736 -0.031149 11.00000 0.03883 0.05539 = 0.03087 -0.00718 0.00306 -0.03528 AFIX 43 H23 2 1.253868 0.346436 -0.039624 11.00000 -1.20000 AFIX 0 C24 1 1.134955 0.282196 0.058892 11.00000 0.02758 0.03711 = 0.02316 -0.00586 -0.00231 -0.01912 AFIX 43 H24 2 1.184419 0.250241 0.110595 11.00000 -1.20000 AFIX 0 C25 1 0.861724 0.153658 0.069463 11.00000 0.01738 0.01979 = 0.01397 -0.00637 0.00083 -0.00717 C26 1 0.825367 0.090894 0.031945 11.00000 0.02175 0.02550 = 0.01836 -0.00959 -0.00232 -0.00725 AFIX 43 H26 2 0.779384 0.133358 -0.022784 11.00000 -1.20000 AFIX 0 C27 1 0.857339 -0.034512 0.075725 11.00000 0.02873 0.02873 = 0.02741 -0.01542 0.00009 -0.01415 AFIX 43 H27 2 0.831072 -0.077070 0.052346 11.00000 -1.20000 AFIX 0 C28 1 0.928951 -0.095389 0.154762 11.00000 0.02741 0.01851 = 0.02276 -0.00730 0.00087 -0.00880 AFIX 43 H28 2 0.953766 -0.180139 0.184731 11.00000 -1.20000 AFIX 0 C29 1 0.963103 -0.028731 0.188576 11.00000 0.02120 0.01798 = 0.01734 -0.00476 -0.00108 -0.00473 AFIX 43 H29 2 1.013149 -0.070624 0.240984 11.00000 -1.20000 AFIX 0 C30 1 1.208632 0.007072 0.198908 11.00000 0.02640 0.02706 = 0.03483 -0.01308 -0.00046 -0.01275 C31 1 1.319390 -0.078999 0.259637 11.00000 0.04065 0.03365 = 0.04055 -0.01509 0.00157 -0.01684 AFIX 137 H31A 2 1.375856 -0.130692 0.227520 11.00000 -1.50000 H31B 2 1.294164 -0.128679 0.320465 11.00000 -1.50000 H31C 2 1.358265 -0.032112 0.269368 11.00000 -1.50000 AFIX 0 C32 1 0.549731 0.132961 0.249683 11.00000 0.05200 0.05696 = 0.04012 0.00685 -0.01077 -0.03710 C33 1 0.674720 0.415337 0.675667 11.00000 0.03712 0.03455 = 0.03361 -0.02046 -0.00216 -0.01159 N1 3 0.803742 0.315674 0.174948 11.00000 0.01795 0.01393 = 0.01425 -0.00381 -0.00089 -0.00671 N2 3 0.906810 0.108997 0.338581 11.00000 0.01800 0.01655 = 0.01655 -0.00639 -0.00426 -0.00584 N3 3 1.002448 0.279310 0.270686 11.00000 0.02159 0.01315 = 0.01320 -0.00117 -0.00461 -0.00567 N4 3 1.025122 0.271077 0.075479 11.00000 0.02152 0.01824 = 0.01712 -0.00466 -0.00251 -0.00903 N5 3 0.927721 0.094116 0.149614 11.00000 0.01682 0.01834 = 0.01527 -0.00444 -0.00037 -0.00764 O1 4 0.543958 0.250433 0.067502 11.00000 0.03144 0.04308 = 0.03709 -0.00077 0.00331 -0.01175 O2 4 0.387970 0.164720 0.146676 11.00000 0.05028 0.06415 = 0.06353 -0.00343 -0.01485 -0.03760 O3 4 0.387209 0.340461 0.166190 11.00000 0.10112 0.02778 = 0.05080 -0.00639 0.02610 -0.00123 O4 4 0.835459 0.468955 0.547576 11.00000 0.04563 0.02354 = 0.01897 -0.00754 -0.00602 -0.01085 O5 4 0.850656 0.256590 0.620536 11.00000 0.03553 0.01815 = 0.03122 -0.01127 -0.00249 -0.00504 O6 4 0.898255 0.350085 0.711377 11.00000 0.03884 0.03388 = 0.02045 -0.00474 -0.00736 -0.01469 O7 4 1.124462 0.068148 0.244492 11.00000 0.02335 0.02219 = 0.01749 -0.00621 -0.00175 -0.01037 O9 4 1.202653 0.015813 0.117016 11.00000 0.03414 0.05175 = 0.03676 -0.02700 -0.00065 -0.01026 F1 5 0.619766 0.025461 0.240593 11.00000 0.05362 0.06229 = 0.07908 0.01710 -0.01113 0.01114 F2 5 0.623950 0.178106 0.260524 11.00000 0.17595 0.18514 = 0.06522 0.03277 -0.06001 -0.15329 F3 5 0.481593 0.106842 0.328799 11.00000 0.08798 0.06938 = 0.03367 0.00181 -0.00017 -0.04187 F4 5 0.599701 0.432185 0.612980 11.00000 0.03015 0.06145 = 0.05378 -0.03116 -0.00991 -0.00553 F5 5 0.641913 0.521262 0.687896 11.00000 0.04931 0.04572 = 0.07645 -0.04569 0.01432 -0.01270 F6 5 0.654245 0.333917 0.758736 11.00000 0.04733 0.05759 = 0.03711 -0.02526 0.01122 -0.02913 S1 6 0.457482 0.233265 0.145282 11.00000 0.02507 0.02494 = 0.03241 -0.00264 -0.00048 -0.00843 S2 6 0.833516 0.366896 0.634048 11.00000 0.02846 0.02146 = 0.01936 -0.00794 -0.00290 -0.00702 CO1 7 0.967646 0.187741 0.206869 11.00000 0.01686 0.01424 = 0.01132 -0.00389 -0.00150 -0.00658 HKLF 4 REM AEK1145CoH_0m in P-1 REM R1 = 0.0362 for 6288 Fo > 4sig(Fo) and 0.0412 for all 7167 data REM 499 parameters refined using 0 restraints END WGHT 0.0429 1.7500 REM Highest difference peak 0.628, deepest hole -0.644, 1-sigma level 0.058 Q1 1 1.2412 -0.0183 0.2681 11.00000 0.05 0.63 Q2 1 0.5417 0.2469 0.2803 11.00000 0.05 0.63 Q3 1 0.6453 0.0834 0.2593 11.00000 0.05 0.50 Q4 1 1.3980 -0.1236 0.2952 11.00000 0.05 0.40 Q5 1 0.4687 0.1229 0.1393 11.00000 0.05 0.38 Q6 1 0.3528 0.2983 0.1533 11.00000 0.05 0.35 Q7 1 0.7495 0.3797 0.6663 11.00000 0.05 0.33 Q8 1 0.7731 0.4586 0.5799 11.00000 0.05 0.33 Q9 1 0.8548 0.3226 0.3325 11.00000 0.05 0.32 Q10 1 0.7441 0.3414 0.3740 11.00000 0.05 0.29 Q11 1 0.8026 0.2504 0.3552 11.00000 0.05 0.28 Q12 1 0.7994 0.3237 0.0567 11.00000 0.05 0.28 Q13 1 0.8424 0.2191 0.0516 11.00000 0.05 0.27 Q14 1 0.5162 0.1833 0.1928 11.00000 0.05 0.26 Q15 1 0.7640 0.3414 0.2892 11.00000 0.05 0.26 Q16 1 0.6311 -0.0019 0.2354 11.00000 0.05 0.26 Q17 1 0.8283 0.3494 0.7250 11.00000 0.05 0.26 Q18 1 0.4199 0.1410 0.3757 11.00000 0.05 0.26 Q19 1 0.8951 0.3036 0.0059 11.00000 0.05 0.25 Q20 1 0.8789 0.1227 0.1236 11.00000 0.05 0.25 ; data_shelxl _database_code_depnum_ccdc_archive 'CCDC 915338' #TrackingRef 'web_deposit_cif_file_0_AmandaKing_1355262136.aek1145co.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AEK1145Co _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H130 B4 Co4 F40 N30 O24 S8' _chemical_formula_weight 3960.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.791 _cell_length_b 16.341 _cell_length_c 27.415 _cell_angle_alpha 90.00 _cell_angle_beta 97.47 _cell_angle_gamma 90.00 _cell_volume 7902.4 _cell_formula_units_Z 2 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 9696 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.31 _exptl_crystal_description Prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4024 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8818 _exptl_absorpt_correction_T_max 0.9266 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 55077 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.37 _reflns_number_total 13504 _reflns_number_gt 12161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _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^)+(0.1420P)^2^+18.4489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(16) _refine_ls_number_reflns 13504 _refine_ls_number_parameters 1175 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1975 _refine_ls_wR_factor_gt 0.1880 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 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 C1 C 0.0594(3) 0.8283(4) 0.9212(2) 0.0279(13) Uani 1 1 d . . . C2 C 0.0670(4) 0.7497(4) 0.9061(3) 0.0404(16) Uani 1 1 d . . . H2 H 0.0553 0.7068 0.9261 0.049 Uiso 1 1 calc R . . C3 C 0.0916(4) 0.7332(4) 0.8615(3) 0.0392(16) Uani 1 1 d . . . H3 H 0.0980 0.6795 0.8516 0.047 Uiso 1 1 calc R . . C4 C 0.1065(4) 0.7970(4) 0.8322(3) 0.0330(14) Uani 1 1 d . . . H4 H 0.1231 0.7872 0.8019 0.040 Uiso 1 1 calc R . . C5 C 0.0967(4) 0.8768(4) 0.8476(2) 0.0288(13) Uani 1 1 d . . . C6 C 0.1098(4) 0.9494(4) 0.8152(3) 0.0343(15) Uani 1 1 d . . . C7 C 0.1284(6) 0.9195(5) 0.7659(3) 0.047(2) Uani 1 1 d . . . H7A H 0.1792 0.8985 0.7696 0.071 Uiso 1 1 calc R . . H7B H 0.1241 0.9641 0.7429 0.071 Uiso 1 1 calc R . . H7C H 0.0936 0.8770 0.7539 0.071 Uiso 1 1 calc R . . C8 C -0.0388(4) 1.0924(4) 0.8433(3) 0.0349(15) Uani 1 1 d . . . H8 H -0.0492 1.1214 0.8709 0.042 Uiso 1 1 calc R . . C9 C -0.0824(5) 1.1087(4) 0.7995(3) 0.0447(18) Uani 1 1 d . . . H9 H -0.1211 1.1474 0.7974 0.054 Uiso 1 1 calc R . . C10 C -0.0670(6) 1.0659(5) 0.7589(3) 0.052(2) Uani 1 1 d . . . H10 H -0.0981 1.0707 0.7291 0.062 Uiso 1 1 calc R . . C11 C -0.0037(6) 1.0154(4) 0.7635(3) 0.049(2) Uani 1 1 d . . . H11 H 0.0107 0.9901 0.7358 0.059 Uiso 1 1 calc R . . C12 C 0.0376(4) 1.0027(4) 0.8087(3) 0.0320(14) Uani 1 1 d . . . C13 C 0.2175(4) 1.0810(5) 0.9097(3) 0.0394(16) Uani 1 1 d . . . H13 H 0.2085 1.1068 0.9386 0.047 Uiso 1 1 calc R . . C14 C 0.2847(5) 1.0951(6) 0.8930(4) 0.062(3) Uani 1 1 d . . . H14 H 0.3217 1.1270 0.9110 0.075 Uiso 1 1 calc R . . C15 C 0.2969(6) 1.0609(8) 0.8484(4) 0.084(4) Uani 1 1 d . . . H15 H 0.3426 1.0690 0.8361 0.101 Uiso 1 1 calc R . . C16 C 0.2402(6) 1.0146(5) 0.8224(4) 0.059(3) Uani 1 1 d . . . H16 H 0.2465 0.9935 0.7917 0.071 Uiso 1 1 calc R . . C17 C 0.1743(5) 0.9997(5) 0.8424(3) 0.0413(17) Uani 1 1 d . . . C18 C 0.1672(4) 1.0195(5) 1.0085(3) 0.0369(15) Uani 1 1 d . . . H25 H 0.1780 1.0708 0.9963 0.044 Uiso 1 1 calc R . . C19 C 0.2031(5) 0.9968(6) 1.0538(3) 0.052(2) Uani 1 1 d . . . H26 H 0.2378 1.0315 1.0717 0.063 Uiso 1 1 calc R . . C20 C 0.1866(5) 0.9217(6) 1.0719(3) 0.056(2) Uani 1 1 d . . . H27 H 0.2111 0.9041 1.1021 0.067 Uiso 1 1 calc R . . C21 C 0.1344(5) 0.8733(5) 1.0457(3) 0.0484(19) Uani 1 1 d . . . H28 H 0.1224 0.8226 1.0581 0.058 Uiso 1 1 calc R . . C22 C 0.0988(4) 0.8995(4) 1.0004(2) 0.0298(13) Uani 1 1 d . . . C23 C 0.0359(4) 0.8502(4) 0.9708(2) 0.0301(13) Uani 1 1 d . . . C24 C 0.0190(5) 0.7719(5) 0.9979(3) 0.0430(17) Uani 1 1 d . . . H19A H 0.0643 0.7396 1.0041 0.064 Uiso 1 1 calc R . . H19B H -0.0194 0.7411 0.9780 0.064 Uiso 1 1 calc R . . H19C H 0.0016 0.7858 1.0285 0.064 Uiso 1 1 calc R . . C25 C -0.0855(4) 1.0329(4) 0.9406(3) 0.0348(14) Uani 1 1 d . . . H20 H -0.0790 1.0857 0.9292 0.042 Uiso 1 1 calc R . . C26 C -0.1537(4) 1.0129(4) 0.9553(3) 0.0353(15) Uani 1 1 d . . . H21 H -0.1931 1.0507 0.9527 0.042 Uiso 1 1 calc R . . C27 C -0.1634(4) 0.9351(5) 0.9741(3) 0.0454(18) Uani 1 1 d . . . H22 H -0.2095 0.9193 0.9837 0.054 Uiso 1 1 calc R . . C28 C -0.1029(4) 0.8824(5) 0.9779(3) 0.0419(17) Uani 1 1 d . . . H23 H -0.1076 0.8305 0.9911 0.050 Uiso 1 1 calc R . . C29 C -0.0346(4) 0.9053(4) 0.9624(2) 0.0328(14) Uani 1 1 d . . . C30 C 0.0515(4) 1.1790(5) 0.9519(3) 0.048(2) Uani 1 1 d . . . C31 C 0.0346(5) 1.2596(7) 0.9709(6) 0.088(4) Uani 1 1 d . . . H45A H 0.0326 1.2559 1.0057 0.132 Uiso 1 1 calc R . . H45B H -0.0134 1.2783 0.9547 0.132 Uiso 1 1 calc R . . H45C H 0.0735 1.2975 0.9649 0.132 Uiso 1 1 calc R . . C32 C -0.0367(3) 0.6334(4) 1.1283(2) 0.0247(12) Uani 1 1 d . . . C33 C -0.0795(3) 0.6433(4) 1.0838(2) 0.0271(13) Uani 1 1 d . . . H303 H -0.1075 0.6909 1.0771 0.032 Uiso 1 1 calc R . . C34 C -0.0814(3) 0.5819(4) 1.0480(2) 0.0270(12) Uani 1 1 d . . . H302 H -0.1092 0.5886 1.0171 0.032 Uiso 1 1 calc R . . C35 C -0.0404(4) 0.5109(4) 1.0600(3) 0.0299(13) Uani 1 1 d . . . H301 H -0.0414 0.4682 1.0375 0.036 Uiso 1 1 calc R . . C36 C 0.0018(3) 0.5043(3) 1.1060(2) 0.0232(12) Uani 1 1 d . . . C37 C -0.0185(4) 0.5891(4) 1.2851(2) 0.0291(13) Uani 1 1 d . . . H402 H 0.0164 0.5539 1.3025 0.035 Uiso 1 1 calc R . . C38 C -0.0761(4) 0.6210(4) 1.3093(2) 0.0297(13) Uani 1 1 d . . . H403 H -0.0799 0.6075 1.3418 0.036 Uiso 1 1 calc R . . C39 C -0.1274(4) 0.6733(4) 1.2834(3) 0.0342(14) Uani 1 1 d . . . H404 H -0.1694 0.6922 1.2970 0.041 Uiso 1 1 calc R . . C40 C -0.1152(3) 0.6967(3) 1.2374(2) 0.0270(13) Uani 1 1 d . . . H405 H -0.1476 0.7347 1.2204 0.032 Uiso 1 1 calc R . . C41 C -0.0559(3) 0.6653(4) 1.2153(2) 0.0247(12) Uani 1 1 d . . . C42 C -0.0323(3) 0.6996(4) 1.1676(2) 0.0260(12) Uani 1 1 d . . . C43 C -0.0843(4) 0.7719(4) 1.1492(2) 0.0291(13) Uani 1 1 d . . . H40A H -0.1360 0.7536 1.1435 0.044 Uiso 1 1 calc R . . H40B H -0.0696 0.7926 1.1190 0.044 Uiso 1 1 calc R . . H40C H -0.0796 0.8145 1.1735 0.044 Uiso 1 1 calc R . . C44 C 0.1692(4) 0.6948(4) 1.2200(3) 0.0338(14) Uani 1 1 d . . . H31 H 0.2025 0.6572 1.2366 0.041 Uiso 1 1 calc R . . C45 C 0.1929(4) 0.7780(5) 1.2157(3) 0.0405(16) Uani 1 1 d . . . H32 H 0.2408 0.7945 1.2299 0.049 Uiso 1 1 calc R . . C46 C 0.1448(4) 0.8326(4) 1.1908(3) 0.0402(16) Uani 1 1 d . . . H33 H 0.1612 0.8854 1.1850 0.048 Uiso 1 1 calc R . . C47 C 0.0711(4) 0.8091(4) 1.1739(2) 0.0347(15) Uani 1 1 d . . . H34 H 0.0364 0.8470 1.1590 0.042 Uiso 1 1 calc R . . C48 C 0.0493(3) 0.7264(4) 1.1798(2) 0.0245(12) Uani 1 1 d . . . C49 C 0.2210(3) 0.5288(4) 1.1816(2) 0.0278(13) Uani 1 1 d . . . H38 H 0.2334 0.5634 1.2084 0.033 Uiso 1 1 calc R . . C50 C 0.2787(4) 0.4999(4) 1.1558(3) 0.0335(15) Uani 1 1 d . . . H39 H 0.3285 0.5167 1.1648 0.040 Uiso 1 1 calc R . . C51 C 0.2615(4) 0.4477(4) 1.1177(3) 0.0344(15) Uani 1 1 d . . . H40 H 0.2990 0.4294 1.0997 0.041 Uiso 1 1 calc R . . C52 C 0.1872(4) 0.4217(4) 1.1059(2) 0.0328(14) Uani 1 1 d . . . H41 H 0.1751 0.3834 1.0810 0.039 Uiso 1 1 calc R . . C53 C 0.1308(4) 0.4528(4) 1.1313(2) 0.0258(12) Uani 1 1 d . . . C54 C 0.0483(3) 0.4282(4) 1.1206(2) 0.0240(12) Uani 1 1 d . . . C55 C 0.0376(4) 0.3648(4) 1.0785(2) 0.0277(13) Uani 1 1 d . . . H37A H 0.0635 0.3151 1.0890 0.041 Uiso 1 1 calc R . . H37B H 0.0581 0.3862 1.0504 0.041 Uiso 1 1 calc R . . H37C H -0.0154 0.3538 1.0698 0.041 Uiso 1 1 calc R . . C56 C 0.0084(3) 0.4103(4) 1.2491(2) 0.0275(13) Uani 1 1 d . . . H42 H 0.0138 0.4431 1.2771 0.033 Uiso 1 1 calc R . . C57 C -0.0189(4) 0.3332(4) 1.2528(2) 0.0305(13) Uani 1 1 d . . . H43 H -0.0316 0.3142 1.2827 0.037 Uiso 1 1 calc R . . C58 C -0.0275(4) 0.2831(4) 1.2116(2) 0.0336(14) Uani 1 1 d . . . H44 H -0.0472 0.2305 1.2127 0.040 Uiso 1 1 calc R . . C59 C -0.0058(4) 0.3144(4) 1.1689(2) 0.0307(13) Uani 1 1 d . . . H45 H -0.0105 0.2822 1.1407 0.037 Uiso 1 1 calc R . . C60 C 0.0226(3) 0.3918(4) 1.1673(2) 0.0243(12) Uani 1 1 d . . . C61 C 0.1714(3) 0.5052(4) 1.2947(3) 0.0276(13) Uani 1 1 d . . . C62 C 0.2215(4) 0.4674(5) 1.3343(3) 0.0374(15) Uani 1 1 d . . . H62A H 0.2419 0.4178 1.3226 0.056 Uiso 1 1 calc R . . H62B H 0.1936 0.4551 1.3611 0.056 Uiso 1 1 calc R . . H62C H 0.2621 0.5043 1.3454 0.056 Uiso 1 1 calc R . . C64 C 0.1128(4) 0.5229(5) 0.9595(3) 0.0453(18) Uani 1 1 d . . . C65 C 0.481(2) 0.5860(14) 1.0725(5) 0.218(18) Uani 1 1 d . . . C67 C 0.2157(9) 0.6898(8) 1.0990(6) 0.091(4) Uani 1 1 d . . . C68 C 0.2991(8) 0.7186(9) 1.1119(6) 0.104(5) Uani 1 1 d . . . H68A H 0.2999 0.7759 1.1198 0.156 Uiso 1 1 calc R . . H68B H 0.3261 0.7096 1.0842 0.156 Uiso 1 1 calc R . . H68C H 0.3229 0.6883 1.1397 0.156 Uiso 1 1 calc R . . C69 C 0.1189(8) 0.7402(7) 1.3401(4) 0.099(5) Uani 1 1 d D . . C70 C 0.0884(7) 0.7980(8) 1.3071(4) 0.082(3) Uani 1 1 d D . . H60A H 0.0978 0.7829 1.2746 0.123 Uiso 1 1 calc R . . H60B H 0.1112 0.8502 1.3156 0.123 Uiso 1 1 calc R . . H60C H 0.0347 0.8014 1.3081 0.123 Uiso 1 1 calc R . . C71 C 0.1929(5) 0.2613(6) 1.2011(3) 0.0495(19) Uani 1 1 d . . . C72 C 0.1860(5) 0.1985(6) 1.1643(3) 0.058(2) Uani 1 1 d . . . H10A H 0.2126 0.1504 1.1772 0.087 Uiso 1 1 calc R . . H10B H 0.2073 0.2173 1.1359 0.087 Uiso 1 1 calc R . . H10C H 0.1334 0.1855 1.1551 0.087 Uiso 1 1 calc R . . B1 B -0.2581(4) 0.7475(5) 1.0212(3) 0.0367(17) Uani 1 1 d . . . B2 B -0.1849(4) 0.4793(5) 1.1894(3) 0.0360(18) Uani 1 1 d . . . N1 N 0.0749(3) 0.8934(3) 0.89135(19) 0.0245(10) Uani 1 1 d . . . N2 N 0.0174(3) 1.0382(3) 0.8494(2) 0.0298(11) Uani 1 1 d . . . N3 N 0.1624(3) 1.0314(3) 0.8868(2) 0.0309(12) Uani 1 1 d . . . N4 N 0.1177(3) 0.9718(4) 0.9810(2) 0.0298(12) Uani 1 1 d . . . N5 N -0.0262(3) 0.9793(3) 0.9418(2) 0.0282(11) Uani 1 1 d . . . N6 N 0.0619(3) 1.1156(3) 0.9376(2) 0.0310(12) Uani 1 1 d . . . N7 N 0.0049(3) 0.5661(3) 1.13986(19) 0.0241(11) Uani 1 1 d . . . N8 N -0.0104(3) 0.6060(3) 1.23887(19) 0.0260(10) Uani 1 1 d . . . N9 N 0.0993(3) 0.6702(3) 1.20035(19) 0.0264(11) Uani 1 1 d . . . N10 N 0.1483(3) 0.5075(3) 1.16864(19) 0.0238(10) Uani 1 1 d . . . N11 N 0.0282(3) 0.4421(3) 1.20702(19) 0.0249(10) Uani 1 1 d . . . N12 N 0.1321(3) 0.5333(3) 1.2632(2) 0.0263(11) Uani 1 1 d . . . N13 N 0.1503(7) 0.6670(6) 1.0909(3) 0.074(3) Uani 1 1 d . . . N14 N 0.1278(15) 0.6860(12) 1.3693(8) 0.196(9) Uiso 1 1 d D . . N15 N 0.2017(4) 0.3121(5) 1.2302(3) 0.0547(18) Uani 1 1 d . . . O1 O 0.4363(3) 0.6585(3) 1.2930(2) 0.0519(14) Uani 1 1 d . . . O2 O 0.3132(3) 0.6087(3) 1.2752(2) 0.0514(14) Uani 1 1 d . . . O3 O 0.3826(4) 0.5836(6) 1.3508(2) 0.085(3) Uani 1 1 d . . . O4 O -0.0193(3) 0.5838(3) 0.9376(2) 0.0423(12) Uani 1 1 d . . . O5 O 0.0478(4) 0.5326(4) 0.8720(2) 0.0514(14) Uani 1 1 d . . . O6 O -0.0032(4) 0.4366(4) 0.9279(3) 0.0579(15) Uani 1 1 d . . . O7 O 0.5686(4) 0.5266(5) 1.1450(3) 0.075(2) Uani 1 1 d . . . O8 O 0.4503(4) 0.5990(4) 1.1611(2) 0.0550(15) Uani 1 1 d . . . O9 O 0.4492(4) 0.4649(4) 1.1245(4) 0.091(3) Uani 1 1 d . . . O10 O -0.1089(3) 0.7634(4) 1.4010(2) 0.0543(14) Uani 1 1 d . . . O11 O -0.2351(6) 0.8084(9) 1.3967(7) 0.177(8) Uani 1 1 d . . . O12 O -0.2224(6) 0.6926(14) 1.3703(4) 0.214(12) Uani 1 1 d . . . F1 F -0.2089(2) 0.7886(3) 1.05547(17) 0.0455(10) Uani 1 1 d . . . F2 F -0.2202(4) 0.6911(4) 0.9980(2) 0.085(2) Uani 1 1 d . . . F3 F -0.2931(3) 0.8016(4) 0.9871(2) 0.081(2) Uani 1 1 d . . . F4 F -0.3136(4) 0.7110(4) 1.0431(2) 0.0786(17) Uani 1 1 d . . . F5 F -0.1538(3) 0.5301(4) 1.1592(2) 0.0698(16) Uani 1 1 d . . . F6 F -0.1871(3) 0.3985(3) 1.1714(2) 0.0571(12) Uani 1 1 d . . . F7 F -0.2601(2) 0.5030(3) 1.1914(2) 0.0475(11) Uani 1 1 d . . . F8 F -0.1462(3) 0.4814(3) 1.23636(19) 0.0518(12) Uani 1 1 d . . . F9 F 0.2796(7) 0.7031(7) 1.3635(5) 0.176(6) Uani 1 1 d D . . F10 F 0.3224(6) 0.7804(6) 1.3091(3) 0.119(3) Uani 1 1 d D . . F11 F 0.3919(6) 0.7500(6) 1.3739(4) 0.129(3) Uiso 1 1 d D . . F12 F 0.1057(3) 0.5112(5) 1.0063(2) 0.084(2) Uani 1 1 d . . . F13 F 0.1613(3) 0.4653(4) 0.9475(3) 0.0769(17) Uani 1 1 d . . . F14 F 0.1493(3) 0.5941(3) 0.9566(2) 0.0567(12) Uani 1 1 d . . . F15 F 0.5103(8) 0.6623(4) 1.0785(4) 0.146(4) Uani 1 1 d . . . F16 F 0.5083(4) 0.5402(6) 1.0411(2) 0.094(2) Uani 1 1 d . . . F17 F 0.4008(5) 0.5940(7) 1.0581(3) 0.129(4) Uani 1 1 d . . . S1 S 0.37038(13) 0.63267(14) 1.31057(9) 0.0552(5) Uani 1 1 d . . . S2 S 0.02453(10) 0.51816(10) 0.91960(7) 0.0356(4) Uani 1 1 d . . . S3 S 0.48762(14) 0.54090(16) 1.13297(9) 0.0571(5) Uani 1 1 d . . . S4 S -0.18763(12) 0.75169(13) 1.40507(8) 0.0497(5) Uani 1 1 d . A . Co1 Co 0.06842(4) 1.00498(5) 0.91462(3) 0.02331(19) Uani 1 1 d . . . Co2 Co 0.06688(4) 0.55489(5) 1.20315(3) 0.02117(18) Uani 1 1 d . . . F18 F -0.1447(14) 0.6403(17) 1.4691(10) 0.162(14) Uani 0.664(14) 1 d PD A 1 F19 F -0.1571(7) 0.7600(10) 1.4949(4) 0.121(6) Uani 0.664(14) 1 d PD A 1 F20 F -0.2631(5) 0.6511(7) 1.4481(5) 0.093(5) Uani 0.664(14) 1 d PD A 1 C66 C -0.1919(8) 0.7020(12) 1.4597(8) 0.142(15) Uani 0.664(14) 1 d PD A 1 C66A C -0.2048(14) 0.6591(11) 1.4377(8) 0.052(9) Uani 0.336(14) 1 d PD A 2 F18A F -0.1784(10) 0.6042(7) 1.4044(7) 0.064(6) Uani 0.336(14) 1 d PD A 2 F19A F -0.1512(15) 0.6396(17) 1.4757(8) 0.047(6) Uani 0.336(14) 1 d PD A 2 F20A F -0.2526(9) 0.6915(10) 1.4748(5) 0.050(4) Uiso 0.336(14) 1 d PD A 2 C63 C 0.3385(5) 0.7213(5) 1.3353(5) 0.082(4) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.022(3) 0.035(3) -0.001(2) -0.002(3) 0.001(2) C2 0.043(4) 0.031(4) 0.044(4) 0.005(3) -0.005(3) 0.006(3) C3 0.039(4) 0.027(3) 0.048(4) -0.007(3) -0.008(3) 0.011(3) C4 0.028(3) 0.034(3) 0.036(3) -0.012(3) -0.002(3) 0.003(3) C5 0.027(3) 0.031(3) 0.028(3) -0.004(3) 0.004(2) -0.001(3) C6 0.045(4) 0.020(3) 0.040(4) -0.010(3) 0.013(3) -0.005(3) C7 0.077(6) 0.031(4) 0.039(4) -0.013(3) 0.022(4) -0.014(4) C8 0.038(4) 0.026(3) 0.041(4) 0.005(3) 0.005(3) -0.005(3) C9 0.051(4) 0.022(3) 0.056(5) 0.012(3) -0.012(4) 0.002(3) C10 0.072(6) 0.029(4) 0.048(5) 0.010(3) -0.013(4) -0.009(4) C11 0.096(7) 0.028(4) 0.024(3) 0.001(3) 0.006(4) -0.012(4) C12 0.042(4) 0.022(3) 0.032(4) -0.002(3) 0.007(3) -0.005(3) C13 0.036(4) 0.044(4) 0.041(4) -0.011(3) 0.013(3) -0.013(3) C14 0.049(5) 0.072(6) 0.073(6) -0.033(5) 0.032(4) -0.029(4) C15 0.059(6) 0.108(9) 0.098(8) -0.065(7) 0.059(6) -0.047(6) C16 0.069(6) 0.051(5) 0.067(6) -0.025(4) 0.045(5) -0.034(4) C17 0.039(4) 0.050(4) 0.038(4) -0.010(3) 0.018(3) -0.006(3) C18 0.030(3) 0.047(4) 0.034(4) -0.007(3) 0.003(3) -0.009(3) C19 0.046(5) 0.068(6) 0.040(4) -0.005(4) -0.001(4) -0.012(4) C20 0.061(5) 0.071(6) 0.031(4) 0.009(4) -0.012(4) -0.012(5) C21 0.054(5) 0.055(5) 0.038(4) 0.015(4) 0.015(4) 0.002(4) C22 0.032(3) 0.031(3) 0.027(3) 0.003(3) 0.006(3) 0.003(3) C23 0.032(3) 0.026(3) 0.032(3) 0.006(3) 0.005(3) 0.004(3) C24 0.050(4) 0.043(4) 0.036(4) 0.012(3) 0.003(3) -0.011(3) C25 0.031(3) 0.031(3) 0.042(4) -0.005(3) 0.004(3) 0.002(3) C26 0.029(3) 0.036(4) 0.042(4) -0.008(3) 0.009(3) 0.001(3) C27 0.034(4) 0.053(5) 0.050(5) -0.001(4) 0.011(3) -0.011(3) C28 0.035(4) 0.050(4) 0.042(4) 0.007(3) 0.011(3) -0.009(3) C29 0.033(3) 0.040(4) 0.026(3) -0.004(3) 0.004(3) -0.002(3) C30 0.024(3) 0.043(4) 0.075(6) -0.023(4) -0.002(3) 0.001(3) C31 0.038(4) 0.065(6) 0.158(12) -0.074(7) -0.004(6) 0.009(4) C32 0.026(3) 0.019(3) 0.030(3) 0.001(2) 0.007(2) -0.002(2) C33 0.027(3) 0.019(3) 0.035(3) 0.003(2) 0.007(3) -0.001(2) C34 0.026(3) 0.029(3) 0.025(3) -0.003(2) 0.001(2) 0.000(2) C35 0.027(3) 0.033(3) 0.030(3) -0.004(3) 0.006(3) 0.000(3) C36 0.019(3) 0.026(3) 0.026(3) 0.000(2) 0.007(2) -0.001(2) C37 0.032(3) 0.022(3) 0.034(3) -0.003(2) 0.006(3) -0.001(2) C38 0.034(3) 0.030(3) 0.028(3) -0.004(3) 0.013(3) -0.004(3) C39 0.027(3) 0.033(3) 0.044(4) -0.009(3) 0.012(3) 0.000(3) C40 0.024(3) 0.018(3) 0.039(3) -0.003(2) 0.003(3) 0.002(2) C41 0.030(3) 0.022(3) 0.023(3) 0.004(2) 0.004(2) 0.002(2) C42 0.028(3) 0.023(3) 0.028(3) 0.002(2) 0.006(2) 0.001(2) C43 0.035(3) 0.018(3) 0.035(3) 0.002(2) 0.005(3) 0.003(2) C44 0.024(3) 0.039(4) 0.038(4) -0.007(3) 0.003(3) -0.012(3) C45 0.031(3) 0.050(4) 0.041(4) -0.005(3) 0.007(3) -0.016(3) C46 0.051(4) 0.025(3) 0.046(4) -0.001(3) 0.011(3) -0.017(3) C47 0.041(4) 0.032(3) 0.032(4) 0.002(3) 0.011(3) -0.006(3) C48 0.025(3) 0.020(3) 0.029(3) 0.004(2) 0.005(2) -0.001(2) C49 0.024(3) 0.033(3) 0.026(3) -0.001(3) 0.001(2) 0.003(3) C50 0.021(3) 0.039(4) 0.041(4) 0.003(3) 0.007(3) 0.004(3) C51 0.030(3) 0.041(4) 0.035(4) 0.003(3) 0.015(3) 0.011(3) C52 0.039(3) 0.033(3) 0.028(3) 0.001(3) 0.012(3) 0.014(3) C53 0.025(3) 0.023(3) 0.031(3) 0.002(2) 0.006(2) 0.004(2) C54 0.023(3) 0.025(3) 0.025(3) 0.001(2) 0.004(2) 0.005(2) C55 0.032(3) 0.026(3) 0.026(3) -0.007(2) 0.004(2) 0.004(2) C56 0.029(3) 0.021(3) 0.033(3) 0.000(2) 0.004(3) -0.006(2) C57 0.035(3) 0.026(3) 0.031(3) 0.004(3) 0.005(3) -0.002(3) C58 0.034(3) 0.031(3) 0.034(3) 0.002(3) 0.001(3) -0.006(3) C59 0.037(3) 0.017(3) 0.038(4) -0.008(3) 0.003(3) -0.002(2) C60 0.023(3) 0.022(3) 0.028(3) -0.004(2) 0.004(2) 0.002(2) C61 0.019(3) 0.034(3) 0.031(4) 0.001(3) 0.007(3) -0.001(2) C62 0.031(3) 0.049(4) 0.031(4) 0.005(3) 0.000(3) 0.005(3) C64 0.038(4) 0.047(4) 0.051(5) 0.022(4) 0.002(3) 0.006(3) C65 0.45(5) 0.159(18) 0.034(6) -0.017(8) 0.002(13) 0.20(3) C67 0.093(9) 0.067(7) 0.124(11) 0.030(7) 0.052(9) 0.023(7) C68 0.088(9) 0.087(9) 0.142(13) 0.009(9) 0.030(9) -0.002(7) C69 0.179(14) 0.077(7) 0.056(6) -0.020(6) 0.067(8) -0.066(9) C70 0.075(7) 0.097(9) 0.080(7) -0.016(7) 0.032(6) 0.021(6) C71 0.042(4) 0.054(5) 0.053(5) 0.013(4) 0.011(4) 0.010(4) C72 0.046(4) 0.074(6) 0.052(5) 0.025(5) 0.000(4) 0.001(4) B1 0.024(3) 0.039(4) 0.046(5) -0.011(3) 0.000(3) -0.006(3) B2 0.021(3) 0.046(4) 0.042(5) -0.018(4) 0.011(3) -0.012(3) N1 0.022(2) 0.024(2) 0.028(3) -0.008(2) 0.005(2) -0.0004(19) N2 0.033(3) 0.023(2) 0.034(3) -0.005(2) 0.008(2) -0.008(2) N3 0.028(3) 0.028(3) 0.038(3) -0.010(2) 0.008(2) -0.005(2) N4 0.027(3) 0.036(3) 0.027(3) -0.003(2) 0.004(2) 0.003(2) N5 0.026(3) 0.031(3) 0.028(3) -0.003(2) 0.006(2) -0.002(2) N6 0.026(3) 0.028(3) 0.039(3) -0.003(2) 0.005(2) 0.001(2) N7 0.019(2) 0.028(3) 0.027(3) 0.000(2) 0.008(2) -0.0052(19) N8 0.024(2) 0.025(2) 0.030(3) -0.001(2) 0.006(2) 0.000(2) N9 0.027(2) 0.028(3) 0.025(3) -0.001(2) 0.008(2) -0.002(2) N10 0.022(2) 0.027(3) 0.023(3) -0.001(2) 0.003(2) 0.0008(19) N11 0.027(3) 0.021(2) 0.027(3) 0.001(2) 0.003(2) 0.0052(19) N12 0.026(3) 0.026(3) 0.028(3) -0.010(2) 0.005(2) -0.005(2) N13 0.109(8) 0.073(6) 0.039(4) 0.013(4) 0.006(4) 0.030(6) N15 0.063(5) 0.043(4) 0.056(4) 0.015(4) 0.001(4) 0.014(3) O1 0.040(3) 0.037(3) 0.080(4) 0.005(3) 0.014(3) -0.009(2) O2 0.045(3) 0.038(3) 0.063(4) -0.006(3) -0.022(3) -0.008(2) O3 0.072(5) 0.141(7) 0.039(4) 0.032(4) -0.010(3) -0.030(5) O4 0.033(2) 0.039(3) 0.055(3) 0.000(2) 0.007(2) 0.003(2) O5 0.058(3) 0.055(3) 0.041(3) -0.012(3) 0.006(3) 0.004(3) O6 0.055(3) 0.041(3) 0.077(4) 0.001(3) 0.006(3) -0.003(3) O7 0.057(4) 0.102(5) 0.061(4) 0.011(4) -0.010(3) 0.010(4) O8 0.066(4) 0.062(4) 0.039(3) -0.007(3) 0.014(3) 0.003(3) O9 0.046(4) 0.046(4) 0.179(9) -0.020(5) 0.005(5) 0.001(3) O10 0.050(3) 0.049(3) 0.066(4) 0.008(3) 0.013(3) -0.013(3) O11 0.061(5) 0.151(11) 0.306(19) 0.137(13) -0.031(8) -0.011(6) O12 0.064(6) 0.49(3) 0.091(7) -0.148(13) 0.023(5) -0.100(11) F1 0.040(2) 0.036(2) 0.057(3) -0.0230(19) -0.0072(19) 0.0020(18) F2 0.072(4) 0.099(5) 0.077(4) -0.057(4) -0.020(3) 0.034(3) F3 0.048(3) 0.082(4) 0.104(5) 0.056(4) -0.027(3) -0.016(3) F4 0.076(4) 0.086(4) 0.073(4) 0.018(3) 0.004(3) -0.036(3) F5 0.076(4) 0.084(4) 0.053(3) -0.005(3) 0.025(3) -0.046(3) F6 0.056(3) 0.044(3) 0.069(3) -0.017(2) -0.004(2) 0.008(2) F7 0.030(2) 0.047(2) 0.068(3) 0.000(2) 0.015(2) 0.0036(17) F8 0.039(2) 0.059(3) 0.053(3) -0.015(2) -0.006(2) -0.003(2) F9 0.156(10) 0.138(9) 0.260(15) 0.036(9) 0.122(11) 0.068(8) F10 0.142(8) 0.114(7) 0.092(5) -0.011(5) -0.019(5) 0.022(6) F12 0.053(3) 0.151(6) 0.046(3) 0.038(3) 0.000(2) -0.010(4) F13 0.053(3) 0.064(3) 0.112(5) 0.001(3) 0.002(3) 0.032(3) F14 0.046(3) 0.052(3) 0.069(3) 0.014(2) -0.007(2) -0.010(2) F15 0.273(14) 0.044(4) 0.128(7) 0.002(4) 0.055(8) -0.058(6) F16 0.087(4) 0.140(6) 0.059(4) -0.038(4) 0.024(3) 0.006(4) F17 0.114(6) 0.178(9) 0.082(5) -0.041(5) -0.036(5) 0.086(6) S1 0.0482(11) 0.0571(12) 0.0581(13) 0.0010(10) -0.0012(9) -0.0081(10) S2 0.0365(9) 0.0281(8) 0.0420(10) -0.0013(7) 0.0047(7) -0.0001(7) S3 0.0527(12) 0.0666(14) 0.0524(12) 0.0018(10) 0.0083(10) 0.0083(11) S4 0.0461(10) 0.0439(10) 0.0625(13) 0.0228(9) 0.0198(9) 0.0100(8) Co1 0.0253(4) 0.0214(4) 0.0238(4) -0.0041(3) 0.0056(3) -0.0015(3) Co2 0.0202(3) 0.0214(4) 0.0222(4) -0.0021(3) 0.0036(3) 0.0001(3) F18 0.079(13) 0.18(2) 0.22(2) 0.173(19) 0.003(13) 0.009(12) F19 0.096(9) 0.203(16) 0.062(7) -0.052(8) 0.002(6) -0.022(9) F20 0.039(5) 0.084(7) 0.162(12) 0.059(8) 0.036(6) -0.006(4) C66 0.029(8) 0.21(3) 0.18(3) 0.15(3) 0.008(13) -0.025(14) C66A 0.09(3) 0.006(9) 0.067(18) 0.005(9) 0.026(16) -0.007(11) F18A 0.086(12) 0.009(6) 0.103(14) 0.000(6) 0.037(10) 0.007(6) F19A 0.034(10) 0.067(14) 0.040(9) 0.031(9) 0.000(7) -0.003(9) C63 0.044(5) 0.027(4) 0.169(12) -0.005(6) -0.009(6) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.362(10) . ? C1 N1 1.391(8) . ? C1 C23 1.519(9) . ? C2 C3 1.378(11) . ? C2 H2 0.9300 . ? C3 C4 1.363(11) . ? C3 H3 0.9300 . ? C4 C5 1.389(9) . ? C4 H4 0.9300 . ? C5 N1 1.334(8) . ? C5 C6 1.520(9) . ? C6 C7 1.513(10) . ? C6 C17 1.526(11) . ? C6 C12 1.543(10) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N2 1.330(9) . ? C8 C9 1.368(11) . ? C8 H8 0.9300 . ? C9 C10 1.372(13) . ? C9 H9 0.9300 . ? C10 C11 1.388(14) . ? C10 H10 0.9300 . ? C11 C12 1.372(11) . ? C11 H11 0.9300 . ? C12 N2 1.346(9) . ? C13 C14 1.354(11) . ? C13 N3 1.360(9) . ? C13 H13 0.9300 . ? C14 C15 1.387(13) . ? C14 H14 0.9300 . ? C15 C16 1.381(13) . ? C15 H15 0.9300 . ? C16 C17 1.378(11) . ? C16 H16 0.9300 . ? C17 N3 1.364(9) . ? C18 N4 1.335(9) . ? C18 C19 1.372(12) . ? C18 H25 0.9300 . ? C19 C20 1.370(13) . ? C19 H26 0.9300 . ? C20 C21 1.353(13) . ? C20 H27 0.9300 . ? C21 C22 1.387(10) . ? C21 H28 0.9300 . ? C22 N4 1.356(9) . ? C22 C23 1.523(10) . ? C23 C24 1.528(9) . ? C23 C29 1.537(9) . ? C24 H19A 0.9600 . ? C24 H19B 0.9600 . ? C24 H19C 0.9600 . ? C25 N5 1.368(9) . ? C25 C26 1.367(10) . ? C25 H20 0.9300 . ? C26 C27 1.390(11) . ? C26 H21 0.9300 . ? C27 C28 1.373(12) . ? C27 H22 0.9300 . ? C28 C29 1.390(10) . ? C28 H23 0.9300 . ? C29 N5 1.350(9) . ? C30 N6 1.131(9) . ? C30 C31 1.463(11) . ? C31 H45A 0.9600 . ? C31 H45B 0.9600 . ? C31 H45C 0.9600 . ? C32 N7 1.342(8) . ? C32 C33 1.360(9) . ? C32 C42 1.521(8) . ? C33 C34 1.399(9) . ? C33 H303 0.9300 . ? C34 C35 1.388(9) . ? C34 H302 0.9300 . ? C35 C36 1.385(9) . ? C35 H301 0.9300 . ? C36 N7 1.368(8) . ? C36 C54 1.518(8) . ? C37 N8 1.324(8) . ? C37 C38 1.392(9) . ? C37 H402 0.9300 . ? C38 C39 1.378(10) . ? C38 H403 0.9300 . ? C39 C40 1.361(10) . ? C39 H404 0.9300 . ? C40 C41 1.381(9) . ? C40 H405 0.9300 . ? C41 N8 1.369(8) . ? C41 C42 1.532(8) . ? C42 C48 1.513(8) . ? C42 C43 1.545(8) . ? C43 H40A 0.9600 . ? C43 H40B 0.9600 . ? C43 H40C 0.9600 . ? C44 N9 1.351(8) . ? C44 C45 1.433(10) . ? C44 H31 0.9300 . ? C45 C46 1.357(11) . ? C45 H32 0.9300 . ? C46 C47 1.387(11) . ? C46 H33 0.9300 . ? C47 C48 1.421(9) . ? C47 H34 0.9300 . ? C48 N9 1.349(8) . ? C49 N10 1.343(8) . ? C49 C50 1.402(9) . ? C49 H38 0.9300 . ? C50 C51 1.352(10) . ? C50 H39 0.9300 . ? C51 C52 1.385(10) . ? C51 H40 0.9300 . ? C52 C53 1.389(9) . ? C52 H41 0.9300 . ? C53 N10 1.365(8) . ? C53 C54 1.513(8) . ? C54 C60 1.535(9) . ? C54 C55 1.545(8) . ? C55 H37A 0.9600 . ? C55 H37B 0.9600 . ? C55 H37C 0.9600 . ? C56 N11 1.353(8) . ? C56 C57 1.359(9) . ? C56 H42 0.9300 . ? C57 C58 1.388(10) . ? C57 H43 0.9300 . ? C58 C59 1.379(10) . ? C58 H44 0.9300 . ? C59 C60 1.365(9) . ? C59 H45 0.9300 . ? C60 N11 1.357(8) . ? C61 N12 1.135(9) . ? C61 C62 1.450(10) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C64 F12 1.320(10) . ? C64 F14 1.340(9) . ? C64 F13 1.346(10) . ? C64 S2 1.794(8) . ? C65 F16 1.283(15) . ? C65 F15 1.36(3) . ? C65 F17 1.43(3) . ? C65 S3 1.803(16) . ? C67 N13 1.214(17) . ? C67 C68 1.55(2) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 N14 1.190(10) . ? C69 C70 1.369(9) . ? C70 H60A 0.9600 . ? C70 H60B 0.9600 . ? C70 H60C 0.9600 . ? C71 N15 1.148(12) . ? C71 C72 1.433(14) . ? C72 H10A 0.9600 . ? C72 H10B 0.9600 . ? C72 H10C 0.9600 . ? B1 F2 1.351(10) . ? B1 F4 1.358(10) . ? B1 F1 1.372(9) . ? B1 F3 1.377(10) . ? B2 F5 1.342(10) . ? B2 F8 1.379(10) . ? B2 F7 1.402(9) . ? B2 F6 1.408(9) . ? N1 Co1 1.939(5) . ? N2 Co1 1.974(6) . ? N3 Co1 1.974(6) . ? N4 Co1 1.990(6) . ? N5 Co1 1.974(5) . ? N6 Co1 1.923(6) . ? N7 Co2 1.939(5) . ? N8 Co2 1.974(5) . ? N9 Co2 1.975(5) . ? N10 Co2 1.987(5) . ? N11 Co2 1.976(5) . ? N12 Co2 1.920(6) . ? O1 S1 1.390(6) . ? O2 S1 1.368(6) . ? O3 S1 1.358(7) . ? O4 S2 1.449(5) . ? O5 S2 1.438(6) . ? O6 S2 1.450(6) . ? O7 S3 1.454(8) . ? O8 S3 1.439(6) . ? O9 S3 1.422(8) . ? O10 S4 1.433(6) . ? O11 S4 1.255(12) . ? O12 S4 1.440(12) . ? O12 C66A 1.91(3) . ? F9 C63 1.413(13) . ? F10 C63 1.215(12) . ? F11 C63 1.408(12) . ? S1 C63 1.726(9) . ? S4 C66A 1.80(2) . ? S4 C66 1.713(19) . ? F18 C66 1.316(18) . ? F19 C66 1.435(18) . ? F20 C66 1.513(14) . ? C66A F19A 1.354(19) . ? C66A F18A 1.404(16) . ? C66A F20A 1.505(17) . ? 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 C2 C1 N1 120.6(6) . . ? C2 C1 C23 122.9(6) . . ? N1 C1 C23 116.5(5) . . ? C1 C2 C3 120.6(7) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 118.8(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.8(6) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.9(6) . . ? N1 C5 C6 116.8(5) . . ? C4 C5 C6 121.3(6) . . ? C7 C6 C5 109.8(5) . . ? C7 C6 C17 111.9(6) . . ? C5 C6 C17 107.3(6) . . ? C7 C6 C12 110.8(7) . . ? C5 C6 C12 108.5(5) . . ? C17 C6 C12 108.3(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 124.8(7) . . ? N2 C8 H8 117.6 . . ? C9 C8 H8 117.6 . . ? C8 C9 C10 117.6(7) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? C9 C10 C11 118.3(7) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 120.3(7) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? N2 C12 C11 120.8(7) . . ? N2 C12 C6 117.2(6) . . ? C11 C12 C6 122.0(7) . . ? C14 C13 N3 124.0(7) . . ? C14 C13 H13 118.0 . . ? N3 C13 H13 118.0 . . ? C13 C14 C15 118.4(8) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 119.2(8) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 119.6(8) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N3 C17 C16 121.8(7) . . ? N3 C17 C6 116.5(6) . . ? C16 C17 C6 121.7(7) . . ? N4 C18 C19 123.3(7) . . ? N4 C18 H25 118.4 . . ? C19 C18 H25 118.4 . . ? C20 C19 C18 118.3(8) . . ? C20 C19 H26 120.9 . . ? C18 C19 H26 120.9 . . ? C21 C20 C19 119.8(8) . . ? C21 C20 H27 120.1 . . ? C19 C20 H27 120.1 . . ? C20 C21 C22 119.8(8) . . ? C20 C21 H28 120.1 . . ? C22 C21 H28 120.1 . . ? N4 C22 C21 120.8(7) . . ? N4 C22 C23 117.0(6) . . ? C21 C22 C23 122.1(6) . . ? C1 C23 C22 109.5(5) . . ? C1 C23 C24 109.4(6) . . ? C22 C23 C24 111.2(6) . . ? C1 C23 C29 108.5(5) . . ? C22 C23 C29 107.4(5) . . ? C24 C23 C29 110.8(6) . . ? C23 C24 H19A 109.5 . . ? C23 C24 H19B 109.5 . . ? H19A C24 H19B 109.5 . . ? C23 C24 H19C 109.5 . . ? H19A C24 H19C 109.5 . . ? H19B C24 H19C 109.5 . . ? N5 C25 C26 123.4(7) . . ? N5 C25 H20 118.3 . . ? C26 C25 H20 118.3 . . ? C25 C26 C27 119.1(7) . . ? C25 C26 H21 120.5 . . ? C27 C26 H21 120.5 . . ? C28 C27 C26 117.9(7) . . ? C28 C27 H22 121.0 . . ? C26 C27 H22 121.0 . . ? C27 C28 C29 121.0(7) . . ? C27 C28 H23 119.5 . . ? C29 C28 H23 119.5 . . ? N5 C29 C28 121.1(7) . . ? N5 C29 C23 117.1(6) . . ? C28 C29 C23 121.7(6) . . ? N6 C30 C31 177.4(9) . . ? C30 C31 H45A 109.5 . . ? C30 C31 H45B 109.5 . . ? H45A C31 H45B 109.5 . . ? C30 C31 H45C 109.5 . . ? H45A C31 H45C 109.5 . . ? H45B C31 H45C 109.5 . . ? N7 C32 C33 122.4(6) . . ? N7 C32 C42 116.0(5) . . ? C33 C32 C42 121.5(5) . . ? C32 C33 C34 120.2(6) . . ? C32 C33 H303 119.9 . . ? C34 C33 H303 119.9 . . ? C35 C34 C33 118.0(6) . . ? C35 C34 H302 121.0 . . ? C33 C34 H302 121.0 . . ? C36 C35 C34 119.1(6) . . ? C36 C35 H301 120.4 . . ? C34 C35 H301 120.4 . . ? N7 C36 C35 122.0(5) . . ? N7 C36 C54 116.9(5) . . ? C35 C36 C54 121.1(5) . . ? N8 C37 C38 123.8(6) . . ? N8 C37 H402 118.1 . . ? C38 C37 H402 118.1 . . ? C39 C38 C37 117.8(6) . . ? C39 C38 H403 121.1 . . ? C37 C38 H403 121.1 . . ? C40 C39 C38 118.5(6) . . ? C40 C39 H404 120.8 . . ? C38 C39 H404 120.8 . . ? C39 C40 C41 121.6(6) . . ? C39 C40 H405 119.2 . . ? C41 C40 H405 119.2 . . ? N8 C41 C40 119.7(5) . . ? N8 C41 C42 116.8(5) . . ? C40 C41 C42 123.2(5) . . ? C48 C42 C32 108.8(5) . . ? C48 C42 C41 106.2(5) . . ? C32 C42 C41 110.6(5) . . ? C48 C42 C43 111.5(5) . . ? C32 C42 C43 109.8(5) . . ? C41 C42 C43 109.9(5) . . ? C42 C43 H40A 109.5 . . ? C42 C43 H40B 109.5 . . ? H40A C43 H40B 109.5 . . ? C42 C43 H40C 109.5 . . ? H40A C43 H40C 109.5 . . ? H40B C43 H40C 109.5 . . ? N9 C44 C45 121.0(7) . . ? N9 C44 H31 119.5 . . ? C45 C44 H31 119.5 . . ? C46 C45 C44 119.5(6) . . ? C46 C45 H32 120.2 . . ? C44 C45 H32 120.2 . . ? C45 C46 C47 119.5(6) . . ? C45 C46 H33 120.2 . . ? C47 C46 H33 120.2 . . ? C46 C47 C48 119.0(7) . . ? C46 C47 H34 120.5 . . ? C48 C47 H34 120.5 . . ? N9 C48 C47 121.4(6) . . ? N9 C48 C42 117.2(5) . . ? C47 C48 C42 121.2(5) . . ? N10 C49 C50 121.5(6) . . ? N10 C49 H38 119.3 . . ? C50 C49 H38 119.3 . . ? C51 C50 C49 119.7(6) . . ? C51 C50 H39 120.2 . . ? C49 C50 H39 120.2 . . ? C50 C51 C52 119.1(6) . . ? C50 C51 H40 120.4 . . ? C52 C51 H40 120.4 . . ? C51 C52 C53 120.0(6) . . ? C51 C52 H41 120.0 . . ? C53 C52 H41 120.0 . . ? N10 C53 C52 120.4(6) . . ? N10 C53 C54 116.1(5) . . ? C52 C53 C54 123.5(6) . . ? C53 C54 C36 108.4(5) . . ? C53 C54 C60 109.2(5) . . ? C36 C54 C60 109.0(5) . . ? C53 C54 C55 110.2(5) . . ? C36 C54 C55 110.0(5) . . ? C60 C54 C55 110.1(5) . . ? C54 C55 H37A 109.5 . . ? C54 C55 H37B 109.5 . . ? H37A C55 H37B 109.5 . . ? C54 C55 H37C 109.5 . . ? H37A C55 H37C 109.5 . . ? H37B C55 H37C 109.5 . . ? N11 C56 C57 123.6(6) . . ? N11 C56 H42 118.2 . . ? C57 C56 H42 118.2 . . ? C56 C57 C58 119.3(6) . . ? C56 C57 H43 120.4 . . ? C58 C57 H43 120.4 . . ? C59 C58 C57 117.4(6) . . ? C59 C58 H44 121.3 . . ? C57 C58 H44 121.3 . . ? C60 C59 C58 121.1(6) . . ? C60 C59 H45 119.5 . . ? C58 C59 H45 119.5 . . ? N11 C60 C59 121.7(6) . . ? N11 C60 C54 115.9(5) . . ? C59 C60 C54 122.5(6) . . ? N12 C61 C62 178.5(7) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? F12 C64 F14 106.9(8) . . ? F12 C64 F13 106.3(7) . . ? F14 C64 F13 105.1(7) . . ? F12 C64 S2 113.6(6) . . ? F14 C64 S2 113.2(5) . . ? F13 C64 S2 111.1(6) . . ? F16 C65 F15 116(3) . . ? F16 C65 F17 108.6(18) . . ? F15 C65 F17 107.7(12) . . ? F16 C65 S3 113.1(11) . . ? F15 C65 S3 106.6(12) . . ? F17 C65 S3 104(2) . . ? N13 C67 C68 177.3(15) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N14 C69 C70 164.4(19) . . ? C69 C70 H60A 109.5 . . ? C69 C70 H60B 109.5 . . ? H60A C70 H60B 109.5 . . ? C69 C70 H60C 109.5 . . ? H60A C70 H60C 109.5 . . ? H60B C70 H60C 109.5 . . ? N15 C71 C72 177.0(10) . . ? C71 C72 H10A 109.5 . . ? C71 C72 H10B 109.5 . . ? H10A C72 H10B 109.5 . . ? C71 C72 H10C 109.5 . . ? H10A C72 H10C 109.5 . . ? H10B C72 H10C 109.5 . . ? F2 B1 F4 110.2(7) . . ? F2 B1 F1 110.2(6) . . ? F4 B1 F1 110.5(7) . . ? F2 B1 F3 109.1(8) . . ? F4 B1 F3 106.9(6) . . ? F1 B1 F3 110.0(7) . . ? F5 B2 F8 111.5(6) . . ? F5 B2 F7 109.0(7) . . ? F8 B2 F7 108.6(6) . . ? F5 B2 F6 111.0(6) . . ? F8 B2 F6 109.8(7) . . ? F7 B2 F6 106.8(6) . . ? C5 N1 C1 118.3(5) . . ? C5 N1 Co1 121.6(4) . . ? C1 N1 Co1 120.0(4) . . ? C8 N2 C12 117.5(6) . . ? C8 N2 Co1 123.1(5) . . ? C12 N2 Co1 119.4(5) . . ? C13 N3 C17 116.9(6) . . ? C13 N3 Co1 123.2(5) . . ? C17 N3 Co1 120.0(5) . . ? C18 N4 C22 117.8(6) . . ? C18 N4 Co1 122.5(5) . . ? C22 N4 Co1 119.6(4) . . ? C29 N5 C25 117.2(6) . . ? C29 N5 Co1 119.6(4) . . ? C25 N5 Co1 123.2(5) . . ? C30 N6 Co1 173.7(6) . . ? C32 N7 C36 118.2(5) . . ? C32 N7 Co2 121.4(4) . . ? C36 N7 Co2 120.4(4) . . ? C37 N8 C41 117.9(5) . . ? C37 N8 Co2 123.8(4) . . ? C41 N8 Co2 118.2(4) . . ? C48 N9 C44 119.1(6) . . ? C48 N9 Co2 119.1(4) . . ? C44 N9 Co2 121.8(5) . . ? C49 N10 C53 119.1(5) . . ? C49 N10 Co2 120.6(4) . . ? C53 N10 Co2 120.3(4) . . ? C56 N11 C60 116.9(5) . . ? C56 N11 Co2 122.3(4) . . ? C60 N11 Co2 120.8(4) . . ? C61 N12 Co2 166.1(5) . . ? S4 O12 C66A 63.2(7) . . ? O3 S1 O2 115.6(4) . . ? O3 S1 O1 114.1(5) . . ? O2 S1 O1 115.1(4) . . ? O3 S1 C63 101.7(6) . . ? O2 S1 C63 105.5(4) . . ? O1 S1 C63 102.5(4) . . ? O5 S2 O4 114.7(3) . . ? O5 S2 O6 115.9(4) . . ? O4 S2 O6 114.7(4) . . ? O5 S2 C64 102.3(4) . . ? O4 S2 C64 103.1(4) . . ? O6 S2 C64 103.5(4) . . ? O9 S3 O8 114.7(5) . . ? O9 S3 O7 109.7(5) . . ? O8 S3 O7 119.8(5) . . ? O9 S3 C65 103.5(11) . . ? O8 S3 C65 104.1(5) . . ? O7 S3 C65 102.7(12) . . ? O11 S4 O10 121.9(6) . . ? O11 S4 O12 98.8(11) . . ? O10 S4 O12 112.2(5) . . ? O11 S4 C66A 123.9(9) . . ? O10 S4 C66A 112.4(8) . . ? O12 S4 C66A 71.3(11) . . ? O11 S4 C66 113.9(11) . . ? O10 S4 C66 106.7(6) . . ? O12 S4 C66 101.3(10) . . ? C66A S4 C66 30.6(8) . . ? N6 Co1 N1 179.9(3) . . ? N6 Co1 N3 90.7(2) . . ? N1 Co1 N3 89.3(2) . . ? N6 Co1 N5 89.2(2) . . ? N1 Co1 N5 90.8(2) . . ? N3 Co1 N5 179.3(3) . . ? N6 Co1 N2 89.9(2) . . ? N1 Co1 N2 90.0(2) . . ? N3 Co1 N2 84.4(2) . . ? N5 Co1 N2 94.9(2) . . ? N6 Co1 N4 89.7(2) . . ? N1 Co1 N4 90.4(2) . . ? N3 Co1 N4 96.8(2) . . ? N5 Co1 N4 83.8(2) . . ? N2 Co1 N4 178.7(2) . . ? N12 Co2 N7 174.0(2) . . ? N12 Co2 N8 92.0(2) . . ? N7 Co2 N8 93.0(2) . . ? N12 Co2 N9 93.5(2) . . ? N7 Co2 N9 90.6(2) . . ? N8 Co2 N9 80.9(2) . . ? N12 Co2 N11 87.6(2) . . ? N7 Co2 N11 88.5(2) . . ? N8 Co2 N11 95.6(2) . . ? N9 Co2 N11 176.4(2) . . ? N12 Co2 N10 86.6(2) . . ? N7 Co2 N10 88.6(2) . . ? N8 Co2 N10 177.2(2) . . ? N9 Co2 N10 96.8(2) . . ? N11 Co2 N10 86.7(2) . . ? F18 C66 F19 99.5(18) . . ? F18 C66 F20 96.7(17) . . ? F19 C66 F20 141.3(18) . . ? F18 C66 S4 115.8(17) . . ? F19 C66 S4 102.1(11) . . ? F20 C66 S4 102.0(11) . . ? F19A C66A F18A 95.1(17) . . ? F19A C66A F20A 88.1(18) . . ? F18A C66A F20A 159(2) . . ? F19A C66A S4 116(2) . . ? F18A C66A S4 96.9(12) . . ? F20A C66A S4 100.8(11) . . ? F19A C66A O12 145(2) . . ? F18A C66A O12 65.2(11) . . ? F20A C66A O12 121.1(15) . . ? S4 C66A O12 45.4(8) . . ? F10 C63 F11 105.3(9) . . ? F10 C63 F9 110.9(9) . . ? F11 C63 F9 97.7(12) . . ? F10 C63 S1 119.9(11) . . ? F11 C63 S1 110.5(7) . . ? F9 C63 S1 110.1(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.371 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.115 _iucr_refine_instructions_details ; TITL AEK1145Co_0m in Cc CELL 0.71073 17.7910 16.3410 27.4150 90.000 97.474 90.000 ZERR 2.00 0.0000 0.0000 0.0000 0.000 0.000 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H B N O F S CO UNIT 288 260 8 60 48 80 16 8 MERG 2 DFIX 1.33 0.02 F9 C63 C63 F10 C63 F11 DFIX 1.33 0.02 F18 C66 C66 F19 C66 F20 DFIX 1.33 0.02 F18A C66A C66A F19A C66A F20A DFIX 1.46 0.01 C69 C70 DFIX 1.16 0.01 C69 N14 FMAP 2 PLAN 20 SIZE 0.12 0.16 0.20 ACTA 50.00 BOND $H LIST 4 WPDB 2 L.S. 20 TEMP 100.00 WGHT 0.142000 18.448900 FVAR 0.05637 0.66449 C1 1 0.059414 0.828333 0.921153 11.00000 0.02576 0.02174 = 0.03466 -0.00101 -0.00169 0.00103 C2 1 0.066951 0.749712 0.906079 11.00000 0.04337 0.03102 = 0.04401 0.00457 -0.00518 0.00634 AFIX 43 H2 2 0.055349 0.706751 0.926059 11.00000 -1.20000 AFIX 0 C3 1 0.091613 0.733199 0.861486 11.00000 0.03898 0.02705 = 0.04772 -0.00660 -0.00836 0.01079 AFIX 43 H3 2 0.098004 0.679498 0.851571 11.00000 -1.20000 AFIX 0 C4 1 0.106469 0.797016 0.832177 11.00000 0.02783 0.03413 = 0.03553 -0.01217 -0.00175 0.00300 AFIX 43 H4 2 0.123101 0.787166 0.801930 11.00000 -1.20000 AFIX 0 C5 1 0.096681 0.876796 0.847644 11.00000 0.02729 0.03104 = 0.02806 -0.00424 0.00363 -0.00119 C6 1 0.109826 0.949427 0.815180 11.00000 0.04469 0.02014 = 0.04005 -0.00973 0.01324 -0.00475 C7 1 0.128360 0.919532 0.765896 11.00000 0.07691 0.03084 = 0.03855 -0.01296 0.02237 -0.01397 AFIX 137 H7A 2 0.179177 0.898531 0.769572 11.00000 -1.50000 H7B 2 0.124089 0.964129 0.742907 11.00000 -1.50000 H7C 2 0.093573 0.876965 0.753934 11.00000 -1.50000 AFIX 0 C8 1 -0.038821 1.092447 0.843313 11.00000 0.03799 0.02551 = 0.04112 0.00501 0.00519 -0.00463 AFIX 43 H8 2 -0.049225 1.121431 0.870851 11.00000 -1.20000 AFIX 0 C9 1 -0.082391 1.108724 0.799527 11.00000 0.05076 0.02209 = 0.05642 0.01243 -0.01159 0.00208 AFIX 43 H9 2 -0.121059 1.147366 0.797354 11.00000 -1.20000 AFIX 0 C10 1 -0.066954 1.065944 0.758921 11.00000 0.07167 0.02939 = 0.04803 0.01002 -0.01328 -0.00851 AFIX 43 H10 2 -0.098088 1.070686 0.729063 11.00000 -1.20000 AFIX 0 C11 1 -0.003733 1.015430 0.763520 11.00000 0.09601 0.02767 = 0.02351 0.00092 0.00624 -0.01186 AFIX 43 H11 2 0.010711 0.990095 0.735819 11.00000 -1.20000 AFIX 0 C12 1 0.037595 1.002663 0.808738 11.00000 0.04225 0.02179 = 0.03240 -0.00197 0.00681 -0.00501 C13 1 0.217506 1.080994 0.909695 11.00000 0.03551 0.04352 = 0.04123 -0.01060 0.01291 -0.01319 AFIX 43 H13 2 0.208464 1.106769 0.938611 11.00000 -1.20000 AFIX 0 C14 1 0.284676 1.095122 0.892988 11.00000 0.04888 0.07160 = 0.07323 -0.03327 0.03155 -0.02906 AFIX 43 H14 2 0.321745 1.126991 0.910984 11.00000 -1.20000 AFIX 0 C15 1 0.296855 1.060898 0.848371 11.00000 0.05859 0.10774 = 0.09815 -0.06521 0.05920 -0.04678 AFIX 43 H15 2 0.342591 1.069047 0.836072 11.00000 -1.20000 AFIX 0 C16 1 0.240200 1.014572 0.822447 11.00000 0.06880 0.05143 = 0.06661 -0.02501 0.04529 -0.03357 AFIX 43 H16 2 0.246473 0.993528 0.791717 11.00000 -1.20000 AFIX 0 C17 1 0.174342 0.999744 0.842404 11.00000 0.03934 0.04988 = 0.03794 -0.00960 0.01769 -0.00558 C18 1 0.167240 1.019535 1.008487 11.00000 0.02954 0.04723 = 0.03353 -0.00709 0.00294 -0.00880 AFIX 43 H25 2 0.177967 1.070763 0.996326 11.00000 -1.20000 AFIX 0 C19 1 0.203122 0.996813 1.053784 11.00000 0.04593 0.06814 = 0.04048 -0.00467 -0.00094 -0.01180 AFIX 43 H26 2 0.237796 1.031487 1.071740 11.00000 -1.20000 AFIX 0 C20 1 0.186570 0.921726 1.071898 11.00000 0.06053 0.07140 = 0.03147 0.00938 -0.01164 -0.01216 AFIX 43 H27 2 0.211139 0.904110 1.102090 11.00000 -1.20000 AFIX 0 C21 1 0.134385 0.873289 1.045738 11.00000 0.05441 0.05461 = 0.03845 0.01463 0.01493 0.00162 AFIX 43 H28 2 0.122445 0.822590 1.058091 11.00000 -1.20000 AFIX 0 C22 1 0.098752 0.899492 1.000435 11.00000 0.03183 0.03125 = 0.02703 0.00250 0.00617 0.00313 C23 1 0.035944 0.850200 0.970846 11.00000 0.03230 0.02614 = 0.03199 0.00600 0.00482 0.00362 C24 1 0.019029 0.771894 0.997896 11.00000 0.04977 0.04263 = 0.03598 0.01165 0.00328 -0.01075 AFIX 137 H19A 2 0.064326 0.739585 1.004145 11.00000 -1.50000 H19B 2 -0.019439 0.741137 0.977992 11.00000 -1.50000 H19C 2 0.001577 0.785775 1.028542 11.00000 -1.50000 AFIX 0 C25 1 -0.085488 1.032882 0.940617 11.00000 0.03079 0.03117 = 0.04230 -0.00472 0.00441 0.00169 AFIX 43 H20 2 -0.079019 1.085705 0.929244 11.00000 -1.20000 AFIX 0 C26 1 -0.153723 1.012862 0.955265 11.00000 0.02885 0.03576 = 0.04238 -0.00765 0.00889 0.00106 AFIX 43 H21 2 -0.193076 1.050714 0.952698 11.00000 -1.20000 AFIX 0 C27 1 -0.163446 0.935119 0.974051 11.00000 0.03432 0.05347 = 0.04969 -0.00144 0.01055 -0.01079 AFIX 43 H22 2 -0.209524 0.919331 0.983695 11.00000 -1.20000 AFIX 0 C28 1 -0.102894 0.882369 0.977923 11.00000 0.03542 0.04998 = 0.04185 0.00745 0.01078 -0.00921 AFIX 43 H23 2 -0.107642 0.830494 0.991138 11.00000 -1.20000 AFIX 0 C29 1 -0.034584 0.905303 0.962396 11.00000 0.03312 0.03957 = 0.02574 -0.00394 0.00377 -0.00214 C30 1 0.051458 1.178996 0.951889 11.00000 0.02443 0.04264 = 0.07515 -0.02347 -0.00194 0.00131 C31 1 0.034591 1.259636 0.970925 11.00000 0.03795 0.06456 = 0.15773 -0.07447 -0.00446 0.00886 AFIX 137 H45A 2 0.032571 1.255941 1.005678 11.00000 -1.50000 H45B 2 -0.013417 1.278347 0.954722 11.00000 -1.50000 H45C 2 0.073548 1.297543 0.964867 11.00000 -1.50000 AFIX 0 C32 1 -0.036736 0.633440 1.128264 11.00000 0.02616 0.01930 = 0.02968 0.00144 0.00724 -0.00221 C33 1 -0.079476 0.643284 1.083774 11.00000 0.02706 0.01937 = 0.03545 0.00258 0.00652 -0.00100 AFIX 43 H303 2 -0.107527 0.690928 1.077100 11.00000 -1.20000 AFIX 0 C34 1 -0.081363 0.581947 1.048023 11.00000 0.02638 0.02883 = 0.02524 -0.00266 0.00117 0.00005 AFIX 43 H302 2 -0.109210 0.588621 1.017144 11.00000 -1.20000 AFIX 0 C35 1 -0.040431 0.510855 1.060029 11.00000 0.02720 0.03258 = 0.03048 -0.00393 0.00562 0.00044 AFIX 43 H301 2 -0.041353 0.468195 1.037505 11.00000 -1.20000 AFIX 0 C36 1 0.001810 0.504275 1.106000 11.00000 0.01903 0.02574 = 0.02580 -0.00031 0.00652 -0.00055 C37 1 -0.018473 0.589117 1.285144 11.00000 0.03165 0.02156 = 0.03441 -0.00334 0.00567 -0.00105 AFIX 43 H402 2 0.016357 0.553910 1.302511 11.00000 -1.20000 AFIX 0 C38 1 -0.076105 0.621022 1.309285 11.00000 0.03355 0.03027 = 0.02764 -0.00377 0.01335 -0.00449 AFIX 43 H403 2 -0.079859 0.607504 1.341832 11.00000 -1.20000 AFIX 0 C39 1 -0.127407 0.673288 1.283372 11.00000 0.02717 0.03297 = 0.04436 -0.00935 0.01211 0.00033 AFIX 43 H404 2 -0.169399 0.692165 1.296977 11.00000 -1.20000 AFIX 0 C40 1 -0.115194 0.696654 1.237390 11.00000 0.02446 0.01756 = 0.03884 -0.00265 0.00329 0.00247 AFIX 43 H405 2 -0.147578 0.734679 1.220412 11.00000 -1.20000 AFIX 0 C41 1 -0.055897 0.665277 1.215337 11.00000 0.02982 0.02210 = 0.02254 0.00425 0.00428 0.00197 C42 1 -0.032334 0.699552 1.167590 11.00000 0.02797 0.02303 = 0.02777 0.00175 0.00616 0.00103 C43 1 -0.084285 0.771922 1.149165 11.00000 0.03477 0.01782 = 0.03491 0.00233 0.00549 0.00262 AFIX 137 H40A 2 -0.135952 0.753587 1.143530 11.00000 -1.50000 H40B 2 -0.069617 0.792639 1.119024 11.00000 -1.50000 H40C 2 -0.079572 0.814511 1.173491 11.00000 -1.50000 AFIX 0 C44 1 0.169217 0.694793 1.220004 11.00000 0.02434 0.03870 = 0.03831 -0.00684 0.00348 -0.01184 AFIX 43 H31 2 0.202490 0.657163 1.236572 11.00000 -1.20000 AFIX 0 C45 1 0.192865 0.778048 1.215697 11.00000 0.03064 0.05026 = 0.04131 -0.00517 0.00692 -0.01573 AFIX 43 H32 2 0.240797 0.794547 1.229885 11.00000 -1.20000 AFIX 0 C46 1 0.144793 0.832620 1.190760 11.00000 0.05071 0.02539 = 0.04588 -0.00090 0.01140 -0.01713 AFIX 43 H33 2 0.161172 0.885378 1.185016 11.00000 -1.20000 AFIX 0 C47 1 0.071075 0.809146 1.173907 11.00000 0.04138 0.03220 = 0.03238 0.00152 0.01148 -0.00594 AFIX 43 H34 2 0.036386 0.846965 1.158961 11.00000 -1.20000 AFIX 0 C48 1 0.049345 0.726424 1.179823 11.00000 0.02527 0.01954 = 0.02893 0.00395 0.00476 -0.00091 C49 1 0.221015 0.528778 1.181630 11.00000 0.02356 0.03289 = 0.02643 -0.00106 0.00101 0.00321 AFIX 43 H38 2 0.233421 0.563443 1.208370 11.00000 -1.20000 AFIX 0 C50 1 0.278669 0.499942 1.155797 11.00000 0.02144 0.03880 = 0.04095 0.00282 0.00715 0.00351 AFIX 43 H39 2 0.328505 0.516692 1.164785 11.00000 -1.20000 AFIX 0 C51 1 0.261493 0.447651 1.117743 11.00000 0.02994 0.04108 = 0.03501 0.00275 0.01507 0.01130 AFIX 43 H40 2 0.299037 0.429357 1.099740 11.00000 -1.20000 AFIX 0 C52 1 0.187231 0.421704 1.105940 11.00000 0.03931 0.03285 = 0.02819 0.00085 0.01186 0.01447 AFIX 43 H41 2 0.175145 0.383450 1.081037 11.00000 -1.20000 AFIX 0 C53 1 0.130816 0.452772 1.131266 11.00000 0.02474 0.02252 = 0.03093 0.00249 0.00649 0.00393 C54 1 0.048344 0.428186 1.120600 11.00000 0.02283 0.02491 = 0.02469 0.00066 0.00441 0.00546 C55 1 0.037635 0.364816 1.078457 11.00000 0.03168 0.02560 = 0.02582 -0.00663 0.00421 0.00402 AFIX 137 H37A 2 0.063536 0.315109 1.089047 11.00000 -1.50000 H37B 2 0.058126 0.386207 1.050357 11.00000 -1.50000 H37C 2 -0.015413 0.353750 1.069775 11.00000 -1.50000 AFIX 0 C56 1 0.008421 0.410346 1.249127 11.00000 0.02871 0.02076 = 0.03298 0.00036 0.00415 -0.00572 AFIX 43 H42 2 0.013808 0.443140 1.277090 11.00000 -1.20000 AFIX 0 C57 1 -0.018859 0.333202 1.252831 11.00000 0.03480 0.02596 = 0.03083 0.00417 0.00465 -0.00189 AFIX 43 H43 2 -0.031569 0.314194 1.282669 11.00000 -1.20000 AFIX 0 C58 1 -0.027536 0.283119 1.211601 11.00000 0.03429 0.03127 = 0.03415 0.00174 0.00075 -0.00590 AFIX 43 H44 2 -0.047243 0.230543 1.212745 11.00000 -1.20000 AFIX 0 C59 1 -0.005776 0.314401 1.168863 11.00000 0.03687 0.01705 = 0.03773 -0.00806 0.00280 -0.00232 AFIX 43 H45 2 -0.010489 0.282219 1.140651 11.00000 -1.20000 AFIX 0 C60 1 0.022561 0.391828 1.167310 11.00000 0.02337 0.02230 = 0.02755 -0.00440 0.00397 0.00192 C61 1 0.171372 0.505231 1.294736 11.00000 0.01872 0.03367 = 0.03139 0.00115 0.00703 -0.00073 C62 1 0.221489 0.467402 1.334290 11.00000 0.03146 0.04900 = 0.03069 0.00481 -0.00040 0.00549 AFIX 137 H62A 2 0.241913 0.417802 1.322618 11.00000 -1.50000 H62B 2 0.193601 0.455052 1.361091 11.00000 -1.50000 H62C 2 0.262142 0.504301 1.345354 11.00000 -1.50000 AFIX 0 C64 1 0.112768 0.522881 0.959484 11.00000 0.03785 0.04659 = 0.05053 0.02206 0.00223 0.00603 C65 1 0.480829 0.585966 1.072521 11.00000 0.45291 0.15889 = 0.03380 -0.01736 0.00158 0.19958 C67 1 0.215687 0.689800 1.098951 11.00000 0.09332 0.06738 = 0.12367 0.03020 0.05214 0.02280 C68 1 0.299106 0.718639 1.111894 11.00000 0.08785 0.08737 = 0.14158 0.00887 0.03021 -0.00158 AFIX 137 H68A 2 0.299936 0.775902 1.119769 11.00000 -1.50000 H68B 2 0.326063 0.709578 1.084234 11.00000 -1.50000 H68C 2 0.322867 0.688258 1.139679 11.00000 -1.50000 AFIX 0 C69 1 0.118887 0.740225 1.340128 11.00000 0.17858 0.07688 = 0.05572 -0.02013 0.06726 -0.06580 C70 1 0.088377 0.797981 1.307142 11.00000 0.07472 0.09672 = 0.07983 -0.01627 0.03216 0.02074 AFIX 137 H60A 2 0.097790 0.782855 1.274646 11.00000 -1.50000 H60B 2 0.111243 0.850153 1.315604 11.00000 -1.50000 H60C 2 0.034710 0.801423 1.308052 11.00000 -1.50000 AFIX 0 C71 1 0.192920 0.261320 1.201065 11.00000 0.04211 0.05444 = 0.05314 0.01288 0.01104 0.00976 C72 1 0.186002 0.198472 1.164276 11.00000 0.04556 0.07437 = 0.05214 0.02534 0.00028 0.00117 AFIX 137 H10A 2 0.212614 0.150447 1.177179 11.00000 -1.50000 H10B 2 0.207334 0.217348 1.135890 11.00000 -1.50000 H10C 2 0.133425 0.185531 1.155121 11.00000 -1.50000 AFIX 0 B1 3 -0.258052 0.747487 1.021242 11.00000 0.02404 0.03857 = 0.04622 -0.01061 0.00018 -0.00603 B2 3 -0.184866 0.479268 1.189403 11.00000 0.02131 0.04641 = 0.04204 -0.01772 0.01109 -0.01151 N1 4 0.074930 0.893446 0.891350 11.00000 0.02219 0.02398 = 0.02759 -0.00778 0.00462 -0.00045 N2 4 0.017355 1.038179 0.849385 11.00000 0.03259 0.02324 = 0.03438 -0.00453 0.00756 -0.00825 N3 4 0.162432 1.031413 0.886783 11.00000 0.02781 0.02822 = 0.03776 -0.01033 0.00788 -0.00497 N4 4 0.117697 0.971774 0.980999 11.00000 0.02714 0.03595 = 0.02654 -0.00299 0.00433 0.00312 N5 4 -0.026240 0.979278 0.941817 11.00000 0.02570 0.03131 = 0.02818 -0.00310 0.00570 -0.00163 N6 4 0.061873 1.115634 0.937592 11.00000 0.02563 0.02840 = 0.03912 -0.00342 0.00495 0.00080 N7 4 0.004933 0.566079 1.139861 11.00000 0.01874 0.02795 = 0.02695 -0.00037 0.00823 -0.00523 N8 4 -0.010390 0.606013 1.238874 11.00000 0.02449 0.02466 = 0.02952 -0.00091 0.00631 -0.00005 N9 4 0.099317 0.670211 1.200351 11.00000 0.02694 0.02834 = 0.02498 -0.00088 0.00773 -0.00235 N10 4 0.148279 0.507477 1.168636 11.00000 0.02164 0.02707 = 0.02273 -0.00148 0.00284 0.00082 N11 4 0.028171 0.442061 1.207016 11.00000 0.02692 0.02063 = 0.02688 0.00051 0.00277 0.00517 N12 4 0.132148 0.533344 1.263223 11.00000 0.02561 0.02612 = 0.02760 -0.01043 0.00456 -0.00521 N13 4 0.150280 0.667015 1.090928 11.00000 0.10921 0.07318 = 0.03880 0.01348 0.00631 0.02994 N14 4 0.127755 0.686026 1.369300 11.00000 0.19574 N15 4 0.201715 0.312122 1.230164 11.00000 0.06331 0.04257 = 0.05644 0.01457 0.00090 0.01389 O1 5 0.436251 0.658495 1.292991 11.00000 0.03992 0.03707 = 0.08028 0.00467 0.01432 -0.00928 O2 5 0.313214 0.608682 1.275225 11.00000 0.04519 0.03842 = 0.06303 -0.00629 -0.02180 -0.00811 O3 5 0.382607 0.583623 1.350823 11.00000 0.07157 0.14102 = 0.03875 0.03167 -0.00994 -0.02977 O4 5 -0.019251 0.583762 0.937616 11.00000 0.03297 0.03873 = 0.05538 0.00032 0.00695 0.00265 O5 5 0.047791 0.532641 0.872039 11.00000 0.05832 0.05479 = 0.04099 -0.01241 0.00602 0.00351 O6 5 -0.003234 0.436576 0.927866 11.00000 0.05483 0.04079 = 0.07741 0.00074 0.00586 -0.00270 O7 5 0.568556 0.526619 1.145001 11.00000 0.05658 0.10236 = 0.06141 0.01089 -0.01044 0.01044 O8 5 0.450295 0.599017 1.161125 11.00000 0.06563 0.06200 = 0.03935 -0.00652 0.01377 0.00325 O9 5 0.449196 0.464907 1.124521 11.00000 0.04646 0.04592 = 0.17948 -0.02048 0.00506 0.00067 O10 5 -0.108878 0.763376 1.400950 11.00000 0.04963 0.04918 = 0.06571 0.00838 0.01349 -0.01296 O11 5 -0.235061 0.808428 1.396670 11.00000 0.06094 0.15069 = 0.30583 0.13700 -0.03122 -0.01053 O12 5 -0.222433 0.692551 1.370284 11.00000 0.06409 0.48965 = 0.09119 -0.14768 0.02317 -0.09990 F1 6 -0.208905 0.788634 1.055470 11.00000 0.04035 0.03614 = 0.05655 -0.02298 -0.00722 0.00200 F2 6 -0.220166 0.691067 0.997953 11.00000 0.07164 0.09947 = 0.07700 -0.05734 -0.01958 0.03353 F3 6 -0.293123 0.801638 0.987130 11.00000 0.04800 0.08178 = 0.10422 0.05591 -0.02736 -0.01595 F4 6 -0.313600 0.710951 1.043061 11.00000 0.07556 0.08616 = 0.07276 0.01816 0.00410 -0.03639 F5 6 -0.153801 0.530121 1.159167 11.00000 0.07610 0.08427 = 0.05328 -0.00528 0.02496 -0.04649 F6 6 -0.187114 0.398514 1.171386 11.00000 0.05557 0.04393 = 0.06864 -0.01686 -0.00371 0.00775 F7 6 -0.260103 0.502985 1.191421 11.00000 0.02983 0.04680 = 0.06807 -0.00028 0.01452 0.00364 F8 6 -0.146222 0.481371 1.236359 11.00000 0.03933 0.05948 = 0.05342 -0.01464 -0.00550 -0.00321 F9 6 0.279601 0.703103 1.363520 11.00000 0.15637 0.13787 = 0.25997 0.03590 0.12161 0.06822 F10 6 0.322400 0.780385 1.309087 11.00000 0.14244 0.11432 = 0.09229 -0.01059 -0.01922 0.02220 F11 6 0.391895 0.750006 1.373879 11.00000 0.12855 F12 6 0.105665 0.511194 1.006325 11.00000 0.05282 0.15051 = 0.04574 0.03846 0.00013 -0.01019 F13 6 0.161311 0.465315 0.947526 11.00000 0.05257 0.06427 = 0.11181 0.00133 0.00245 0.03163 F14 6 0.149279 0.594066 0.956636 11.00000 0.04569 0.05194 = 0.06865 0.01356 -0.00747 -0.01024 F15 6 0.510347 0.662326 1.078495 11.00000 0.27323 0.04408 = 0.12777 0.00163 0.05546 -0.05796 F16 6 0.508255 0.540218 1.041121 11.00000 0.08676 0.14025 = 0.05932 -0.03799 0.02442 0.00556 F17 6 0.400769 0.593996 1.058115 11.00000 0.11374 0.17849 = 0.08193 -0.04109 -0.03609 0.08620 S1 7 0.370376 0.632665 1.310575 11.00000 0.04819 0.05712 = 0.05810 0.00099 -0.00116 -0.00814 S2 7 0.024526 0.518157 0.919601 11.00000 0.03645 0.02814 = 0.04200 -0.00125 0.00471 -0.00011 S3 7 0.487618 0.540904 1.132972 11.00000 0.05275 0.06662 = 0.05240 0.00183 0.00828 0.00834 S4 7 -0.187632 0.751690 1.405069 11.00000 0.04608 0.04388 = 0.06252 0.02283 0.01979 0.00999 CO1 8 0.068423 1.004984 0.914622 11.00000 0.02535 0.02143 = 0.02378 -0.00412 0.00560 -0.00146 CO2 8 0.066881 0.554892 1.203151 11.00000 0.02020 0.02136 = 0.02218 -0.00205 0.00361 0.00011 PART 1 F18 6 -0.144659 0.640310 1.469137 21.00000 0.07852 0.18195 = 0.22010 0.17254 0.00292 0.00855 F19 6 -0.157131 0.760040 1.494860 21.00000 0.09642 0.20279 = 0.06240 -0.05155 0.00225 -0.02224 F20 6 -0.263065 0.651110 1.448082 21.00000 0.03893 0.08381 = 0.16213 0.05866 0.03638 -0.00576 C66 1 -0.191911 0.701978 1.459659 21.00000 0.02882 0.21338 = 0.18358 0.14672 0.00802 -0.02454 PART 2 C66A 1 -0.204778 0.659078 1.437735 -21.00000 0.08803 0.00604 = 0.06746 0.00450 0.02572 -0.00656 F18A 6 -0.178418 0.604189 1.404382 -21.00000 0.08609 0.00887 = 0.10304 -0.00006 0.03748 0.00657 F19A 6 -0.151213 0.639554 1.475683 -21.00000 0.03413 0.06656 = 0.04004 0.03086 -0.00033 -0.00296 F20A 6 -0.252627 0.691503 1.474844 -21.00000 0.04978 PART 0 C63 1 0.338485 0.721297 1.335279 11.00000 0.04368 0.02742 = 0.16922 -0.00518 -0.00902 0.02138 HKLF 4 REM AEK1145Co_0m in Cc REM R1 = 0.0692 for 12161 Fo > 4sig(Fo) and 0.0761 for all 13504 data REM 1175 parameters refined using 13 restraints END WGHT 0.1418 18.8801 REM Highest difference peak 1.371, deepest hole -1.010, 1-sigma level 0.115 Q1 1 0.4640 0.5023 1.0986 11.00000 0.05 1.37 Q2 1 0.4624 0.6036 1.1109 11.00000 0.05 1.29 Q3 1 -0.2045 0.8094 1.4529 11.00000 0.05 0.98 Q4 1 0.1040 0.7605 1.3322 11.00000 0.05 0.88 Q5 1 0.0741 0.4962 0.9282 11.00000 0.05 0.88 Q6 1 0.3285 0.7211 1.3037 11.00000 0.05 0.77 Q7 1 -0.2289 0.7641 1.3651 11.00000 0.05 0.74 Q8 1 -0.1613 0.7633 1.4295 11.00000 0.05 0.72 Q9 1 0.2702 0.3406 1.2197 11.00000 0.05 0.64 Q10 1 0.1637 0.2863 1.1700 11.00000 0.05 0.59 Q11 1 0.4932 0.4372 1.0730 11.00000 0.05 0.54 Q12 1 0.0858 0.4444 0.8885 11.00000 0.05 0.54 Q13 1 0.2274 0.2188 1.2359 11.00000 0.05 0.53 Q14 1 0.1555 0.3297 1.2488 11.00000 0.05 0.52 Q15 1 -0.2873 0.6869 1.0242 11.00000 0.05 0.52 Q16 1 0.3451 0.6231 1.3560 11.00000 0.05 0.52 Q17 1 -0.1882 0.6714 1.4276 11.00000 0.05 0.51 Q18 1 0.1895 0.6555 1.0687 11.00000 0.05 0.51 Q19 1 0.5110 0.4762 1.0641 11.00000 0.05 0.50 Q20 1 0.1719 1.0020 0.7328 11.00000 0.05 0.49 ;