data_p242lt_((C4H11)2NH2)2Co3(hfbba)4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H74 Co3 F24 N2 O16' _chemical_formula_weight 2000.24 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' 'O' 'O' 0.0106 0.0060 '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' 'F' 'F' 0.0171 0.0103 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'C2/c' 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' '-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 19.9107(8) _cell_length_b 18.7741(8) _cell_length_c 25.0540(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.4340(10) _cell_angle_gamma 90.00 _cell_volume 8884.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4068 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.698 _exptl_absorpt_process_details "Blessing, 1995" _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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-ApexII" _diffrn_measurement_method "narrow frame" _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27711 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.31 _reflns_number_total 10670 _reflns_number_gt 7896 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+0.0800P] 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 10670 _refine_ls_number_parameters 623 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.029 _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 0.76640(10) 0.27993(9) 0.62650(7) 0.0294(4) Uani 1 1 d . . 4 C2 C 0.74956(9) 0.23565(9) 0.67012(7) 0.0288(4) Uani 1 1 d . . 4 C3 C 0.73530(10) 0.16354(10) 0.65926(8) 0.0352(4) Uani 1 1 d . . 4 H3 H 0.7356 0.1443 0.6252 0.042 Uiso 1 1 calc R . 4 C4 C 0.72065(11) 0.12056(10) 0.69889(8) 0.0370(4) Uani 1 1 d . . 4 H4 H 0.7124 0.0723 0.6914 0.044 Uiso 1 1 calc R . 4 C5 C 0.71804(10) 0.14779(10) 0.74958(7) 0.0312(4) Uani 1 1 d . . 4 C6 C 0.73241(10) 0.22005(10) 0.76032(8) 0.0336(4) Uani 1 1 d . . 4 H6 H 0.7310 0.2396 0.7941 0.040 Uiso 1 1 calc R . 4 C7 C 0.74870(10) 0.26296(10) 0.72127(7) 0.0321(4) Uani 1 1 d . . 4 H7 H 0.7592 0.3108 0.7294 0.038 Uiso 1 1 calc R . 4 C8 C 0.70013(10) 0.09573(10) 0.79092(8) 0.0344(4) Uani 1 1 d . . 4 C9 C 0.76790(11) 0.05317(12) 0.82035(9) 0.0458(6) Uani 1 1 d . . 4 C10 C 0.67579(13) 0.13381(12) 0.83601(9) 0.0471(6) Uani 1 1 d . . 4 C11 C 0.63874(10) 0.04653(10) 0.75777(7) 0.0312(4) Uani 1 1 d . . 4 C12 C 0.58041(10) 0.07778(10) 0.71806(8) 0.0352(4) Uani 1 1 d . . 4 H12 H 0.5791 0.1269 0.7133 0.042 Uiso 1 1 calc R . 4 C13 C 0.52482(10) 0.03719(10) 0.68583(8) 0.0343(4) Uani 1 1 d . . 4 H13 H 0.4859 0.0591 0.6604 0.041 Uiso 1 1 calc R . 4 C14 C 0.52674(10) -0.03672(10) 0.69122(8) 0.0325(4) Uani 1 1 d . . 4 C15 C 0.58433(10) -0.06775(10) 0.73091(8) 0.0348(4) Uani 1 1 d . . 4 H15 H 0.5859 -0.1170 0.7352 0.042 Uiso 1 1 calc R . 4 C16 C 0.63944(10) -0.02690(10) 0.76427(8) 0.0343(4) Uani 1 1 d . . 4 H16 H 0.6771 -0.0487 0.7912 0.041 Uiso 1 1 calc R . 4 C17 C 0.46692(10) -0.08096(10) 0.65570(8) 0.0347(4) Uani 1 1 d . . 4 C18 C 0.71846(10) 0.41154(9) 0.49577(7) 0.0294(4) Uani 1 1 d . A 4 C19 C 0.66239(10) 0.46470(9) 0.46732(7) 0.0285(4) Uani 1 1 d . A 4 C20 C 0.66103(10) 0.53197(9) 0.48969(8) 0.0334(4) Uani 1 1 d . A 4 H20 H 0.6948 0.5443 0.5236 0.040 Uiso 1 1 calc R A 4 C21 C 0.60980(10) 0.58100(9) 0.46197(7) 0.0330(4) Uani 1 1 d . A 4 H21 H 0.6094 0.6259 0.4775 0.040 Uiso 1 1 calc R A 4 C22 C 0.55892(10) 0.56370(9) 0.41119(7) 0.0301(4) Uani 1 1 d . A 4 C23 C 0.56000(11) 0.49531(10) 0.38972(8) 0.0391(5) Uani 1 1 d . A 4 H23 H 0.5259 0.4823 0.3562 0.047 Uiso 1 1 calc R A 4 C24 C 0.61077(11) 0.44689(10) 0.41748(8) 0.0370(5) Uani 1 1 d . A 4 H24 H 0.6104 0.4015 0.4026 0.044 Uiso 1 1 calc R A 4 C25 C 0.50968(11) 0.62220(10) 0.37717(8) 0.0362(4) Uani 1 1 d . A 4 C26 C 0.55338(16) 0.66104(13) 0.34416(9) 0.0568(7) Uani 1 1 d . A 4 C27 C 0.44240(14) 0.59158(14) 0.33565(10) 0.0597(7) Uani 1 1 d . A 4 C28 C 0.48468(10) 0.67503(10) 0.41406(7) 0.0323(4) Uani 1 1 d . A 4 C29 C 0.47873(12) 0.74778(10) 0.40279(9) 0.0427(5) Uani 1 1 d . A 4 H29 H 0.4940 0.7663 0.3742 0.051 Uiso 1 1 calc R A 4 C30 C 0.45040(12) 0.79260(10) 0.43356(9) 0.0419(5) Uani 1 1 d . A 4 H30 H 0.4474 0.8411 0.4257 0.050 Uiso 1 1 calc R A 4 C31 C 0.42630(10) 0.76681(10) 0.47596(8) 0.0320(4) Uani 1 1 d . . 4 C32 C 0.43174(10) 0.69445(10) 0.48730(8) 0.0336(4) Uani 1 1 d . A 4 H32 H 0.4155 0.6760 0.5154 0.040 Uiso 1 1 calc R A 4 C33 C 0.46117(10) 0.64938(10) 0.45694(8) 0.0343(4) Uani 1 1 d . A 4 H33 H 0.4652 0.6010 0.4655 0.041 Uiso 1 1 calc R A 4 C34 C 0.60330(10) 0.18316(10) 0.49117(8) 0.0359(4) Uani 1 1 d . . 4 O1 O 0.59083(9) 0.11833(7) 0.49148(7) 0.0551(4) Uani 1 1 d . B 4 O2 O 0.64032(7) 0.20874(7) 0.46171(5) 0.0341(3) Uani 1 1 d . . 4 O3 O 0.80962(7) 0.33099(7) 0.64310(5) 0.0351(3) Uani 1 1 d . . 4 O4 O 0.73736(7) 0.26237(7) 0.57636(5) 0.0358(3) Uani 1 1 d . . 4 O5 O 0.46646(7) -0.14711(7) 0.66158(6) 0.0432(3) Uani 1 1 d . . 4 O6 O 0.41701(7) -0.04920(7) 0.61934(6) 0.0423(3) Uani 1 1 d . . 4 O7 O 0.71267(7) 0.35031(6) 0.47478(5) 0.0365(3) Uani 1 1 d . A 4 O8 O 0.76697(7) 0.43313(6) 0.53853(5) 0.0357(3) Uani 1 1 d . A 4 Co1 Co 0.7500 0.2500 0.5000 0.02446(9) Uani 1 2 d S . 4 Co2 Co 0.846415(13) 0.375461(12) 0.584876(10) 0.02793(8) Uani 1 1 d . . 4 F1 F 0.78631(6) 0.01208(7) 0.78405(5) 0.0510(3) Uani 1 1 d . . 4 F2 F 0.82288(7) 0.09692(7) 0.84367(5) 0.0609(4) Uani 1 1 d . . 4 F3 F 0.76206(7) 0.01139(7) 0.86193(5) 0.0569(4) Uani 1 1 d . . 4 F4 F 0.72732(8) 0.17134(7) 0.87263(5) 0.0612(4) Uani 1 1 d . . 4 F5 F 0.65214(8) 0.08786(7) 0.86670(5) 0.0622(4) Uani 1 1 d . . 4 F6 F 0.62318(8) 0.17916(7) 0.81278(5) 0.0567(4) Uani 1 1 d . . 4 F7 F 0.58260(11) 0.61374(8) 0.31780(6) 0.0822(5) Uani 1 1 d . A 4 F8 F 0.60522(8) 0.69892(7) 0.37823(6) 0.0601(4) Uani 1 1 d . A 4 F9 F 0.51356(11) 0.70367(8) 0.30403(5) 0.0821(6) Uani 1 1 d . A 4 F10 F 0.45240(9) 0.55599(8) 0.29249(5) 0.0775(5) Uani 1 1 d . A 4 F11 F 0.41204(7) 0.54556(8) 0.36190(7) 0.0709(4) Uani 1 1 d . A 4 F12 F 0.39439(9) 0.64181(9) 0.31318(7) 0.0922(6) Uani 1 1 d . A 4 N1 N 0.5000 0.75861(11) 0.7500 0.0390(6) Uani 1 2 d S . 4 H1A H 0.5103 0.7870 0.7805 0.047 Uiso 0.50 1 calc PR . 4 H1B H 0.4897 0.7870 0.7195 0.047 Uiso 0.50 1 calc PR . 4 C1S C 0.56459(11) 0.71653(11) 0.75265(10) 0.0454(5) Uani 1 1 d . C 4 H1S1 H 0.5801 0.6913 0.7882 0.054 Uiso 1 1 calc R C 4 H1S2 H 0.6020 0.7493 0.7520 0.054 Uiso 1 1 calc R C 4 C2S C 0.55467(14) 0.66360(12) 0.70586(10) 0.0554(6) Uani 1 1 d . C 4 H2S1 H 0.5203 0.6284 0.7089 0.067 Uiso 1 1 calc R C 4 H2S2 H 0.5992 0.6390 0.7116 0.067 Uiso 1 1 calc R C 4 C3S C 0.53023(13) 0.69345(12) 0.64589(10) 0.0560(6) Uani 1 1 d . C 4 H3S1 H 0.5234 0.6541 0.6196 0.067 Uiso 1 1 calc R C 4 H3S2 H 0.4847 0.7165 0.6393 0.067 Uiso 1 1 calc R C 4 C4S C 0.58099(14) 0.74650(13) 0.63336(11) 0.0620(7) Uani 1 1 d . C 4 H4S1 H 0.5619 0.7627 0.5952 0.093 Uiso 1 1 calc R C 4 H4S2 H 0.6258 0.7239 0.6385 0.093 Uiso 1 1 calc R C 4 H4S3 H 0.5873 0.7864 0.6585 0.093 Uiso 1 1 calc R C 4 N2 N 0.5000 1.0000 0.5000 0.0880(12) Uani 1 2 d SD . . C21S C 0.5594(2) 0.9532(2) 0.5008(4) 0.112(3) Uani 0.556(8) 1 d PD D 1 H21A H 0.5858 0.9726 0.4776 0.135 Uiso 0.556(8) 1 calc PR D 1 H21B H 0.5425 0.9061 0.4871 0.135 Uiso 0.556(8) 1 calc PR D 1 C22S C 0.6048(8) 0.9502(9) 0.5615(5) 0.281(12) Uani 0.556(8) 1 d PD D 1 H22A H 0.5790 0.9284 0.5843 0.338 Uiso 0.556(8) 1 calc PR D 1 H22B H 0.6191 0.9977 0.5758 0.338 Uiso 0.556(8) 1 calc PR D 1 C23S C 0.6691(5) 0.9056(5) 0.5631(5) 0.164(6) Uani 0.556(8) 1 d PD D 1 H23A H 0.6864 0.9193 0.5324 0.197 Uiso 0.556(8) 1 calc PR D 1 H23B H 0.6563 0.8556 0.5588 0.197 Uiso 0.556(8) 1 calc PR D 1 C24S C 0.7267(9) 0.9178(11) 0.6194(7) 0.264(11) Uani 0.556(8) 1 d PD D 1 H24A H 0.7510 0.9616 0.6180 0.396 Uiso 0.556(8) 1 calc PR D 1 H24B H 0.7597 0.8790 0.6269 0.396 Uiso 0.556(8) 1 calc PR D 1 H24C H 0.7054 0.9206 0.6488 0.396 Uiso 0.556(8) 1 calc PR D 1 C25S C 0.5577(2) 0.9853(3) 0.55217(17) 0.069(2) Uani 0.444(8) 1 d PD D 2 H25A H 0.5382 0.9625 0.5788 0.083 Uiso 0.444(8) 1 calc PR D 2 H25B H 0.5788 1.0300 0.5685 0.083 Uiso 0.444(8) 1 calc PR D 2 C26S C 0.6150(4) 0.9378(5) 0.5433(4) 0.098(4) Uani 0.444(8) 1 d PD D 2 H26A H 0.6309 0.9566 0.5132 0.118 Uiso 0.444(8) 1 calc PR D 2 H26B H 0.5968 0.8901 0.5331 0.118 Uiso 0.444(8) 1 calc PR D 2 C27S C 0.6760(9) 0.9362(11) 0.5982(8) 0.34(2) Uani 0.444(8) 1 d PD D 2 H27A H 0.6583 0.9280 0.6295 0.406 Uiso 0.444(8) 1 calc PR D 2 H27B H 0.7010 0.9814 0.6040 0.406 Uiso 0.444(8) 1 calc PR D 2 C28S C 0.7262(11) 0.8757(10) 0.5943(13) 0.37(3) Uani 0.444(8) 1 d PD D 2 H28A H 0.7662 0.8747 0.6279 0.560 Uiso 0.222(4) 1 calc PR D 2 H28B H 0.7422 0.8834 0.5624 0.560 Uiso 0.222(4) 1 calc PR D 2 H28C H 0.7016 0.8310 0.5901 0.560 Uiso 0.222(4) 1 calc PR D 2 H28D H 0.7071 0.8514 0.5590 0.560 Uiso 0.222(4) 1 calc PR D 2 H28E H 0.7311 0.8427 0.6245 0.560 Uiso 0.222(4) 1 calc PR D 2 H28F H 0.7717 0.8951 0.5968 0.560 Uiso 0.222(4) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0253(9) 0.0313(9) 0.0288(9) -0.0004(7) 0.0045(8) 0.0053(8) C2 0.0224(9) 0.0322(9) 0.0277(9) -0.0012(7) 0.0019(7) 0.0004(7) C3 0.0392(11) 0.0353(10) 0.0299(10) -0.0073(8) 0.0093(9) -0.0019(8) C4 0.0427(12) 0.0284(10) 0.0381(11) -0.0040(8) 0.0102(9) -0.0051(9) C5 0.0272(9) 0.0353(10) 0.0269(9) 0.0000(7) 0.0024(8) -0.0054(8) C6 0.0341(10) 0.0366(10) 0.0270(9) -0.0071(8) 0.0052(8) -0.0060(8) C7 0.0332(10) 0.0296(9) 0.0299(10) -0.0035(7) 0.0050(8) -0.0042(8) C8 0.0304(10) 0.0377(10) 0.0296(10) -0.0005(8) 0.0019(8) -0.0108(8) C9 0.0347(11) 0.0526(13) 0.0379(12) 0.0119(10) -0.0058(10) -0.0166(10) C10 0.0507(14) 0.0555(14) 0.0345(11) -0.0080(10) 0.0126(10) -0.0218(12) C11 0.0266(9) 0.0344(10) 0.0286(9) -0.0024(8) 0.0029(8) -0.0071(8) C12 0.0329(10) 0.0273(9) 0.0387(11) -0.0011(8) 0.0020(9) -0.0017(8) C13 0.0282(10) 0.0325(10) 0.0355(10) -0.0005(8) 0.0005(8) 0.0017(8) C14 0.0261(9) 0.0325(10) 0.0350(10) -0.0050(8) 0.0043(8) -0.0040(8) C15 0.0297(10) 0.0288(9) 0.0405(11) 0.0015(8) 0.0034(9) -0.0024(8) C16 0.0275(10) 0.0360(10) 0.0325(10) 0.0039(8) -0.0002(8) -0.0021(8) C17 0.0268(10) 0.0349(10) 0.0380(11) -0.0080(8) 0.0041(9) -0.0027(8) C18 0.0280(9) 0.0276(9) 0.0294(9) 0.0025(7) 0.0044(8) 0.0030(8) C19 0.0276(9) 0.0255(9) 0.0296(9) 0.0014(7) 0.0049(8) 0.0033(7) C20 0.0346(10) 0.0314(10) 0.0278(9) -0.0046(8) 0.0007(8) 0.0037(8) C21 0.0377(11) 0.0280(9) 0.0287(10) -0.0049(7) 0.0040(8) 0.0062(8) C22 0.0308(10) 0.0308(9) 0.0258(9) 0.0015(7) 0.0047(8) 0.0078(8) C23 0.0391(11) 0.0349(10) 0.0315(10) -0.0068(8) -0.0054(9) 0.0067(9) C24 0.0388(11) 0.0288(9) 0.0345(10) -0.0067(8) -0.0010(9) 0.0047(8) C25 0.0424(11) 0.0346(10) 0.0264(9) 0.0010(8) 0.0034(9) 0.0139(9) C26 0.086(2) 0.0589(15) 0.0344(12) 0.0161(11) 0.0314(13) 0.0358(15) C27 0.0508(15) 0.0561(15) 0.0505(14) -0.0145(12) -0.0148(12) 0.0230(13) C28 0.0326(10) 0.0326(10) 0.0278(9) 0.0002(7) 0.0039(8) 0.0100(8) C29 0.0531(13) 0.0357(11) 0.0434(12) 0.0071(9) 0.0208(11) 0.0077(10) C30 0.0515(13) 0.0256(10) 0.0512(13) 0.0038(9) 0.0199(11) 0.0066(9) C31 0.0251(9) 0.0311(9) 0.0366(10) -0.0035(8) 0.0053(8) 0.0036(8) C32 0.0303(10) 0.0338(10) 0.0358(10) 0.0027(8) 0.0094(8) 0.0033(8) C33 0.0354(11) 0.0281(9) 0.0381(11) 0.0040(8) 0.0097(9) 0.0066(8) C34 0.0270(10) 0.0364(11) 0.0399(11) -0.0081(8) 0.0041(9) 0.0027(8) O1 0.0631(11) 0.0321(8) 0.0765(11) -0.0166(7) 0.0313(9) -0.0036(7) O2 0.0267(7) 0.0397(7) 0.0325(7) -0.0089(6) 0.0046(6) 0.0003(6) O3 0.0370(7) 0.0337(7) 0.0321(7) -0.0019(5) 0.0072(6) -0.0056(6) O4 0.0329(7) 0.0464(8) 0.0255(7) -0.0034(6) 0.0058(6) -0.0025(6) O5 0.0377(8) 0.0307(7) 0.0535(9) -0.0061(6) 0.0035(7) -0.0050(6) O6 0.0319(8) 0.0355(7) 0.0455(8) -0.0053(6) -0.0076(7) -0.0033(6) O7 0.0393(8) 0.0247(6) 0.0360(7) -0.0007(5) -0.0017(6) 0.0057(6) O8 0.0308(7) 0.0294(7) 0.0377(7) -0.0019(6) -0.0023(6) 0.0048(6) Co1 0.02546(18) 0.02075(16) 0.02295(17) -0.00227(12) 0.00163(14) 0.00190(13) Co2 0.02708(13) 0.02270(13) 0.02849(14) -0.00260(9) 0.00092(10) -0.00020(10) F1 0.0334(7) 0.0576(8) 0.0550(8) 0.0110(6) 0.0042(6) 0.0052(6) F2 0.0364(7) 0.0689(9) 0.0582(8) 0.0138(7) -0.0126(6) -0.0238(6) F3 0.0494(8) 0.0657(8) 0.0406(7) 0.0206(6) -0.0072(6) -0.0180(6) F4 0.0725(9) 0.0738(9) 0.0345(7) -0.0182(6) 0.0131(7) -0.0395(8) F5 0.0746(10) 0.0720(9) 0.0472(7) -0.0071(7) 0.0295(7) -0.0340(8) F6 0.0605(9) 0.0573(8) 0.0569(8) -0.0199(6) 0.0251(7) -0.0070(7) F7 0.1380(15) 0.0689(10) 0.0645(9) 0.0108(7) 0.0676(10) 0.0375(10) F8 0.0716(10) 0.0536(8) 0.0665(9) 0.0138(7) 0.0381(8) 0.0043(7) F9 0.1417(16) 0.0700(10) 0.0364(7) 0.0238(7) 0.0307(9) 0.0426(10) F10 0.0977(12) 0.0710(10) 0.0355(7) -0.0174(7) -0.0190(7) 0.0381(9) F11 0.0366(8) 0.0743(10) 0.0846(11) -0.0331(9) -0.0054(8) -0.0029(7) F12 0.0773(11) 0.0792(10) 0.0759(10) -0.0237(8) -0.0387(9) 0.0490(9) N1 0.0322(13) 0.0325(12) 0.0463(14) 0.000 0.0039(11) 0.000 C1S 0.0282(11) 0.0461(12) 0.0567(14) 0.0023(10) 0.0060(10) 0.0039(9) C2S 0.0531(15) 0.0420(13) 0.0713(17) -0.0010(11) 0.0199(13) 0.0106(11) C3S 0.0516(14) 0.0509(14) 0.0612(15) -0.0129(12) 0.0116(13) 0.0041(12) C4S 0.0534(16) 0.0619(16) 0.0671(17) 0.0057(13) 0.0138(14) 0.0088(13) N2 0.060(2) 0.072(2) 0.126(4) 0.009(2) 0.021(2) -0.001(2) C21S 0.119(7) 0.056(4) 0.154(8) 0.003(4) 0.031(6) -0.047(4) C22S 0.32(2) 0.217(16) 0.45(3) -0.134(18) 0.32(2) -0.035(16) C23S 0.102(9) 0.109(7) 0.284(16) 0.058(10) 0.063(10) 0.003(7) C24S 0.097(10) 0.41(3) 0.239(15) -0.073(17) -0.018(11) 0.054(15) C25S 0.078(5) 0.046(4) 0.090(5) 0.009(3) 0.036(4) -0.010(3) C26S 0.036(4) 0.103(7) 0.144(9) 0.073(6) 0.012(5) 0.031(4) C27S 0.088(13) 0.27(3) 0.58(5) -0.19(3) -0.01(2) 0.010(15) C28S 0.132(15) 0.28(3) 0.76(7) 0.34(4) 0.22(3) 0.105(16) _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 O4 1.250(2) . ? C1 O3 1.267(2) . ? C1 C2 1.493(3) . ? C2 C7 1.385(3) . ? C2 C3 1.392(2) . ? C3 C4 1.380(3) . ? C4 C5 1.385(3) . ? C5 C6 1.395(3) . ? C5 C8 1.545(3) . ? C6 C7 1.383(3) . ? C8 C10 1.539(3) . ? C8 C9 1.541(3) . ? C8 C11 1.548(2) . ? C9 F1 1.330(3) . ? C9 F3 1.338(2) . ? C9 F2 1.345(2) . ? C10 F6 1.332(3) . ? C10 F5 1.336(2) . ? C10 F4 1.340(2) . ? C11 C16 1.388(2) . ? C11 C12 1.397(3) . ? C12 C13 1.376(3) . ? C13 C14 1.393(2) . ? C14 C15 1.386(3) . ? C14 C17 1.493(2) . ? C15 C16 1.382(3) . ? C17 O5 1.251(2) . ? C17 O6 1.265(2) . ? C18 O7 1.254(2) . ? C18 O8 1.261(2) . ? C18 C19 1.499(2) . ? C19 C24 1.384(2) . ? C19 C20 1.385(2) . ? C20 C21 1.386(2) . ? C21 C22 1.391(2) . ? C22 C23 1.395(2) . ? C22 C25 1.538(2) . ? C23 C24 1.374(3) . ? C25 C27 1.525(3) . ? C25 C28 1.542(2) . ? C25 C26 1.558(3) . ? C26 F8 1.320(3) . ? C26 F9 1.333(2) . ? C26 F7 1.344(2) . ? C27 F12 1.334(2) . ? C27 F10 1.339(3) . ? C27 F11 1.340(3) . ? C28 C33 1.387(3) . ? C28 C29 1.392(2) . ? C29 C30 1.377(3) . ? C30 C31 1.384(3) . ? C31 C32 1.385(2) . ? C31 C34 1.488(3) 5_666 ? C32 C33 1.385(3) . ? C34 O1 1.243(2) . ? C34 O2 1.289(2) . ? C34 C31 1.488(3) 5_666 ? O2 Co2 2.0312(12) 7_656 ? O2 Co1 2.2282(12) . ? O3 Co2 2.0094(13) . ? O4 Co1 2.0202(13) . ? O6 Co2 1.9886(13) 3_445 ? O7 Co1 2.0497(12) . ? O8 Co2 1.9649(12) . ? Co1 O4 2.0202(13) 7_656 ? Co1 O7 2.0497(12) 7_656 ? Co1 O2 2.2282(13) 7_656 ? Co2 O6 1.9886(13) 3 ? Co2 O2 2.0312(12) 7_656 ? N1 C1S 1.493(2) 6_657 ? N1 C1S 1.493(2) . ? C1S C2S 1.502(3) . ? C2S C3S 1.532(3) . ? C3S C4S 1.521(4) . ? N2 C25S 1.4678(10) . ? N2 C25S 1.4678(10) 5_676 ? N2 C21S 1.4682(10) 5_676 ? N2 C21S 1.4682(10) . ? C21S C22S 1.506(9) . ? C22S C23S 1.519(9) . ? C23S C24S 1.528(9) . ? C25S C26S 1.518(8) . ? C26S C27S 1.520(10) . ? C27S C28S 1.537(10) . ? 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 O4 C1 O3 125.43(17) . . ? O4 C1 C2 116.70(16) . . ? O3 C1 C2 117.85(15) . . ? C7 C2 C3 118.64(17) . . ? C7 C2 C1 122.84(16) . . ? C3 C2 C1 118.52(16) . . ? C4 C3 C2 120.28(17) . . ? C3 C4 C5 121.44(17) . . ? C4 C5 C6 118.09(18) . . ? C4 C5 C8 117.69(16) . . ? C6 C5 C8 124.22(17) . . ? C7 C6 C5 120.64(17) . . ? C6 C7 C2 120.88(17) . . ? C10 C8 C9 108.72(17) . . ? C10 C8 C5 113.02(16) . . ? C9 C8 C5 107.22(16) . . ? C10 C8 C11 107.01(16) . . ? C9 C8 C11 111.77(16) . . ? C5 C8 C11 109.16(14) . . ? F1 C9 F3 107.64(18) . . ? F1 C9 F2 106.78(19) . . ? F3 C9 F2 106.20(15) . . ? F1 C9 C8 111.26(16) . . ? F3 C9 C8 113.47(19) . . ? F2 C9 C8 111.13(17) . . ? F6 C10 F5 107.00(19) . . ? F6 C10 F4 106.81(18) . . ? F5 C10 F4 106.16(16) . . ? F6 C10 C8 111.27(17) . . ? F5 C10 C8 111.86(18) . . ? F4 C10 C8 113.33(19) . . ? C16 C11 C12 118.42(16) . . ? C16 C11 C8 123.57(17) . . ? C12 C11 C8 117.98(16) . . ? C13 C12 C11 121.25(17) . . ? C12 C13 C14 120.15(18) . . ? C15 C14 C13 118.63(17) . . ? C15 C14 C17 121.10(17) . . ? C13 C14 C17 120.26(17) . . ? C16 C15 C14 121.26(17) . . ? C15 C16 C11 120.23(17) . . ? O5 C17 O6 121.29(17) . . ? O5 C17 C14 121.08(17) . . ? O6 C17 C14 117.63(17) . . ? O7 C18 O8 126.52(16) . . ? O7 C18 C19 117.05(15) . . ? O8 C18 C19 116.43(15) . . ? C24 C19 C20 118.76(16) . . ? C24 C19 C18 119.81(16) . . ? C20 C19 C18 121.43(16) . . ? C19 C20 C21 120.53(17) . . ? C20 C21 C22 120.71(16) . . ? C21 C22 C23 118.16(16) . . ? C21 C22 C25 119.49(16) . . ? C23 C22 C25 121.91(16) . . ? C24 C23 C22 120.82(17) . . ? C23 C24 C19 120.98(17) . . ? C27 C25 C22 112.16(17) . . ? C27 C25 C28 105.73(17) . . ? C22 C25 C28 113.42(14) . . ? C27 C25 C26 109.37(19) . . ? C22 C25 C26 105.26(17) . . ? C28 C25 C26 110.95(16) . . ? F8 C26 F9 108.7(2) . . ? F8 C26 F7 107.6(2) . . ? F9 C26 F7 105.83(17) . . ? F8 C26 C25 111.25(17) . . ? F9 C26 C25 112.5(2) . . ? F7 C26 C25 110.7(2) . . ? F12 C27 F10 106.36(19) . . ? F12 C27 F11 106.8(2) . . ? F10 C27 F11 106.3(2) . . ? F12 C27 C25 112.3(2) . . ? F10 C27 C25 114.6(2) . . ? F11 C27 C25 110.09(19) . . ? C33 C28 C29 118.03(18) . . ? C33 C28 C25 119.54(16) . . ? C29 C28 C25 122.17(17) . . ? C30 C29 C28 120.64(19) . . ? C29 C30 C31 121.25(18) . . ? C30 C31 C32 118.49(18) . . ? C30 C31 C34 119.87(17) . 5_666 ? C32 C31 C34 121.63(18) . 5_666 ? C31 C32 C33 120.37(18) . . ? C32 C33 C28 121.21(17) . . ? O1 C34 O2 121.32(18) . . ? O1 C34 C31 119.99(19) . 5_666 ? O2 C34 C31 118.67(17) . 5_666 ? C34 O2 Co2 103.93(11) . 7_656 ? C34 O2 Co1 122.88(11) . . ? Co2 O2 Co1 103.30(5) 7_656 . ? C1 O3 Co2 116.21(11) . . ? C1 O4 Co1 145.66(13) . . ? C17 O6 Co2 105.30(12) . 3_445 ? C18 O7 Co1 137.43(11) . . ? C18 O8 Co2 125.60(11) . . ? O4 Co1 O4 180.000(12) . 7_656 ? O4 Co1 O7 87.44(5) . 7_656 ? O4 Co1 O7 92.56(5) 7_656 7_656 ? O4 Co1 O7 92.56(5) . . ? O4 Co1 O7 87.44(5) 7_656 . ? O7 Co1 O7 180.00(7) 7_656 . ? O4 Co1 O2 87.19(5) . 7_656 ? O4 Co1 O2 92.81(5) 7_656 7_656 ? O7 Co1 O2 88.64(5) 7_656 7_656 ? O7 Co1 O2 91.36(5) . 7_656 ? O4 Co1 O2 92.81(5) . . ? O4 Co1 O2 87.19(5) 7_656 . ? O7 Co1 O2 91.36(5) 7_656 . ? O7 Co1 O2 88.64(5) . . ? O2 Co1 O2 180.00(4) 7_656 . ? O8 Co2 O6 101.02(6) . 3 ? O8 Co2 O3 104.35(6) . . ? O6 Co2 O3 110.50(6) 3 . ? O8 Co2 O2 108.42(5) . 7_656 ? O6 Co2 O2 126.91(6) 3 7_656 ? O3 Co2 O2 103.73(5) . 7_656 ? C1S N1 C1S 116.1(2) 6_657 . ? N1 C1S C2S 114.63(17) . . ? C1S C2S C3S 116.51(19) . . ? C4S C3S C2S 114.6(2) . . ? C25S N2 C25S 180.000(1) . 5_676 ? C25S N2 C21S 121.6(4) . 5_676 ? C25S N2 C21S 58.4(4) 5_676 5_676 ? C25S N2 C21S 58.4(4) . . ? C25S N2 C21S 121.6(4) 5_676 . ? C21S N2 C21S 180.000(2) 5_676 . ? N2 C21S C22S 105.0(6) . . ? C21S C22S C23S 106.2(8) . . ? C22S C23S C24S 108.7(13) . . ? N2 C25S C26S 113.1(5) . . ? C25S C26S C27S 107.6(9) . . ? C26S C27S C28S 107.9(15) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.571 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.052