Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _publ_contact_letter ; Please consider this CIF submission as crystallographic information file for compound C~12~H~33~B~18~CoKNO~2~ or potassium salt of compound 3. This CIF file has been deposited earlier at the Cambridge Crystallographic Data Centre with reference number CCDC-168258 but journal, title of the article, order of the authors and title of the compound have been changed. ; _publ_contact_author_name 'Prof Francesc Teixidor' _publ_contact_author_address ; ICMAB CSIC Campus UAB Bellaterra Catalonia 08193 SPAIN ; _publ_contact_author_phone '+ 34 93 5801853' _publ_contact_author_fax '+ 34 93 5805729' _publ_contact_author_email teixidor@icmab.es loop_ _publ_author_name _publ_author_address 'Jordi Llop' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Carlos Masalles' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Clara Vinas' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Francesc Teixidor' ; Institut de Ciencia de Materials de Barcelona C.S.C.I. Campus U.A.B. 08193 Bellaterra Spain ; 'Reijo Sillanpaa' ; Department of Chemistry University of Jyvaskyla FIN-40351 Jyvaskyla Finland ; 'Raikko Kivekas' ; Department of Chemistry P.O.Box 55 FIN-00014 University of Helsinki Finland ; _publ_section_title ; The [3,3'-Co(1,2-C~2~B~9~H~11~)~2~]^-^ anion as platform for new materials: Synthesis of its functionalized monosubstituted derivatives incorporating synthons for conducting organic polymers. ; data_potassium_salt_of_3 _database_code_CSD 168258 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C12 H33 B18 Co N O2, K' _chemical_formula_sum 'C12 H33 B18 Co K N O2' _chemical_formula_weight 516.00 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' K K 0.2009 0.2494 '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 'P 1 2(1)/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.305(3) _cell_length_b 12.316(2) _cell_length_c 13.848(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.31(3) _cell_angle_gamma 90.00 _cell_volume 2575.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 10.1 _exptl_crystal_description orange _exptl_crystal_colour plate _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North, Phillips & Mathews 1968' _exptl_absorpt_correction_T_min 0.8364 _exptl_absorpt_correction_T_max 0.9512 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'Rigaku AFC7S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 4754 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.1114 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4547 _reflns_number_gt 2580 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993) ; _computing_data_reduction ; Texsan Process (Molecular Structure Corporation, 1993) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _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 ; w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4547 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1411 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co3 Co 0.38338(4) 0.17845(5) 0.62451(4) 0.0326(2) Uani 1 d . . . K K 0.21971(10) 0.47063(14) 0.71127(10) 0.0810(5) Uani 1 d . . . O1 O 0.2639(2) 0.3750(3) 0.5541(2) 0.0516(10) Uani 1 d . . . O2 O 0.1725(3) 0.5708(3) 0.5174(3) 0.0810(14) Uani 1 d . . . N N 0.0606(5) 0.6553(7) 0.6405(5) 0.096(2) Uani 1 d . . . C1 C 0.3192(3) 0.0440(4) 0.5648(4) 0.0435(13) Uani 1 d . . . H1 H 0.3704 -0.0138 0.5505 0.052 Uiso 1 calc R . . C2 C 0.3015(3) 0.0697(4) 0.6751(3) 0.0451(14) Uani 1 d . . . H2 H 0.3401 0.0306 0.7397 0.054 Uiso 1 calc R . . B4 B 0.3006(4) 0.1544(5) 0.4904(4) 0.0398(15) Uani 1 d . . . H4 H 0.3343 0.1737 0.4281 0.048 Uiso 1 calc R . . B5 B 0.2244(4) 0.0425(6) 0.4854(5) 0.0503(16) Uani 1 d . . . H5 H 0.2114 -0.0102 0.4205 0.060 Uiso 1 calc R . . B6 B 0.2275(5) -0.0129(7) 0.6027(5) 0.066(2) Uani 1 d . . . H6 H 0.2174 -0.0999 0.6152 0.079 Uiso 1 calc R . . B7 B 0.2681(4) 0.2002(5) 0.6858(4) 0.0434(15) Uani 1 d . . . H7 H 0.2807 0.2502 0.7524 0.052 Uiso 1 calc R . . B8 B 0.2627(4) 0.2607(6) 0.5660(4) 0.0425(15) Uani 1 d . . . B9 B 0.1848(4) 0.1774(6) 0.4852(4) 0.0496(16) Uani 1 d . . . H9 H 0.1448 0.2133 0.4198 0.060 Uiso 1 calc R . . B10 B 0.1412(4) 0.0757(7) 0.5542(5) 0.066(2) Uani 1 d . . . H10 H 0.0726 0.0471 0.5337 0.079 Uiso 1 calc R . . B11 B 0.1930(4) 0.0878(6) 0.6771(5) 0.0595(19) Uani 1 d . . . H11 H 0.1594 0.0652 0.7386 0.071 Uiso 1 calc R . . B12 B 0.1650(4) 0.2055(6) 0.6071(4) 0.0534(18) Uani 1 d . . . H12 H 0.1118 0.2598 0.6224 0.064 Uiso 1 calc R . . C1' C 0.4708(3) 0.1994(4) 0.7544(4) 0.0453(13) Uani 1 d . . . H1' H 0.4366 0.1796 0.8161 0.054 Uiso 1 calc R . . C2' C 0.5017(3) 0.1070(4) 0.6814(3) 0.0430(13) Uani 1 d . . . H2' H 0.4879 0.0207 0.6929 0.052 Uiso 1 calc R . . B4' B 0.4452(4) 0.3187(5) 0.6886(4) 0.0372(12) Uani 1 d . . . H4' H 0.3967 0.3793 0.7046 0.045 Uiso 1 calc R . . B5' B 0.5496(4) 0.3018(5) 0.7693(4) 0.0474(16) Uani 1 d . . . H5' H 0.5660 0.3507 0.8363 0.057 Uiso 1 calc R . . B6' B 0.5822(4) 0.1644(5) 0.7666(4) 0.0499(17) Uani 1 d . . . H6' H 0.6190 0.1231 0.8310 0.060 Uiso 1 calc R . . B7' B 0.4990(4) 0.1528(5) 0.5683(4) 0.0416(15) Uani 1 d . . . H7' H 0.4846 0.1021 0.5022 0.050 Uiso 1 calc R . . B8' B 0.4657(4) 0.2900(5) 0.5654(4) 0.0432(15) Uani 1 d . . . H8' H 0.4318 0.3325 0.5001 0.052 Uiso 1 calc R . . B9' B 0.5479(4) 0.3576(6) 0.6514(4) 0.0513(17) Uani 1 d . . . H9' H 0.5636 0.4435 0.6412 0.062 Uiso 1 calc R . . B10' B 0.6313(4) 0.2631(6) 0.6992(5) 0.0567(18) Uani 1 d . . . H10' H 0.7009 0.2876 0.7195 0.068 Uiso 1 calc R . . B11' B 0.5995(4) 0.1347(6) 0.6465(5) 0.0567(18) Uani 1 d . . . H11' H 0.6482 0.0732 0.6328 0.068 Uiso 1 calc R . . B12' B 0.5800(4) 0.2523(6) 0.5757(5) 0.058(2) Uani 1 d . . . H12' H 0.6172 0.2686 0.5156 0.070 Uiso 1 calc R . . C13 C 0.2438(5) 0.4199(5) 0.4597(4) 0.0684(18) Uani 1 d . . . H13A H 0.1872 0.3925 0.4272 0.082 Uiso 1 calc R . . H13B H 0.2887 0.3990 0.4212 0.082 Uiso 1 calc R . . C14 C 0.2403(4) 0.5389(5) 0.4668(4) 0.0691(18) Uani 1 d . . . H14A H 0.2966 0.5659 0.5007 0.083 Uiso 1 calc R . . H14B H 0.2301 0.5702 0.4017 0.083 Uiso 1 calc R . . C15 C 0.1639(6) 0.6846(6) 0.5240(6) 0.105(3) Uani 1 d . . . H15A H 0.1694 0.7182 0.4619 0.126 Uiso 1 calc R . . H15B H 0.2099 0.7134 0.5738 0.126 Uiso 1 calc R . . C16 C 0.0752(6) 0.7076(7) 0.5497(7) 0.116(3) Uani 1 d . . . H16A H 0.0686 0.7855 0.5561 0.139 Uiso 1 calc R . . H16B H 0.0302 0.6831 0.4967 0.139 Uiso 1 calc R . . C17 C 0.0188(5) 0.5595(10) 0.6472(8) 0.115(3) Uani 1 d . . . H17 H -0.0100 0.5203 0.5940 0.138 Uiso 1 calc R . . C18 C 0.0248(6) 0.5281(11) 0.7434(10) 0.132(4) Uani 1 d . . . H18 H 0.0048 0.4643 0.7683 0.158 Uiso 1 calc R . . C19 C 0.0684(7) 0.6159(12) 0.7947(8) 0.130(4) Uani 1 d . . . H19 H 0.0803 0.6216 0.8626 0.155 Uiso 1 calc R . . C20 C 0.0908(6) 0.6910(9) 0.7324(8) 0.117(3) Uani 1 d . . . H20 H 0.1213 0.7553 0.7492 0.141 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co3 0.0334(3) 0.0325(3) 0.0309(3) -0.0012(3) 0.0022(2) 0.0008(3) K 0.0791(11) 0.0959(13) 0.0676(9) -0.0216(9) 0.0104(8) 0.0239(10) O1 0.065(3) 0.047(2) 0.040(2) 0.0040(18) 0.0006(18) 0.020(2) O2 0.099(4) 0.049(3) 0.099(4) 0.008(2) 0.029(3) 0.027(3) N 0.072(4) 0.109(6) 0.098(5) -0.011(5) -0.010(4) 0.029(4) C1 0.038(3) 0.042(3) 0.047(3) -0.008(2) -0.004(2) -0.004(3) C2 0.044(3) 0.052(4) 0.036(3) 0.011(2) -0.004(2) -0.011(3) B4 0.043(3) 0.045(4) 0.029(3) 0.002(2) -0.002(2) 0.000(3) B5 0.043(4) 0.055(4) 0.048(4) -0.005(3) -0.005(3) -0.007(3) B6 0.061(5) 0.065(5) 0.066(5) 0.005(4) -0.006(4) -0.033(4) B7 0.038(3) 0.052(4) 0.042(3) -0.007(3) 0.010(3) -0.005(3) B8 0.036(3) 0.056(4) 0.033(3) -0.004(3) -0.001(3) 0.012(3) B9 0.039(3) 0.064(4) 0.043(3) -0.004(3) -0.005(3) -0.001(4) B10 0.040(4) 0.097(6) 0.056(4) -0.002(4) -0.006(3) -0.015(4) B11 0.052(4) 0.078(5) 0.050(4) 0.000(4) 0.011(3) -0.021(4) B12 0.034(3) 0.078(5) 0.048(4) -0.010(3) 0.007(3) 0.001(3) C1' 0.046(3) 0.049(4) 0.039(3) -0.006(2) 0.001(2) -0.003(3) C2' 0.049(3) 0.027(3) 0.049(3) -0.004(2) -0.005(2) 0.003(2) B4' 0.047(3) 0.030(3) 0.034(3) -0.001(3) 0.002(2) -0.001(3) B5' 0.045(4) 0.047(4) 0.046(3) -0.011(3) -0.006(3) -0.007(3) B6' 0.044(4) 0.051(4) 0.048(3) -0.004(3) -0.011(3) 0.007(3) B7' 0.036(3) 0.050(4) 0.038(3) -0.008(3) 0.006(3) 0.002(3) B8' 0.043(3) 0.050(4) 0.036(3) 0.004(3) 0.004(3) -0.011(3) B9' 0.056(4) 0.048(4) 0.048(4) 0.001(3) 0.005(3) -0.018(3) B10' 0.041(4) 0.073(5) 0.056(4) -0.011(4) 0.008(3) -0.013(4) B11' 0.037(4) 0.063(5) 0.067(4) -0.012(4) -0.001(3) 0.013(3) B12' 0.046(4) 0.086(6) 0.045(4) -0.019(4) 0.015(3) -0.018(4) C13 0.098(5) 0.057(4) 0.050(4) 0.008(3) 0.011(3) 0.014(4) C14 0.081(5) 0.066(5) 0.060(4) 0.018(3) 0.009(3) 0.015(4) C15 0.139(8) 0.060(5) 0.119(7) 0.003(5) 0.027(6) 0.037(5) C16 0.128(8) 0.097(7) 0.117(7) 0.013(6) 0.000(6) 0.052(6) C17 0.063(5) 0.144(10) 0.128(9) -0.026(8) -0.013(5) 0.006(6) C18 0.068(6) 0.201(13) 0.133(9) 0.019(10) 0.034(6) 0.013(7) C19 0.097(8) 0.192(13) 0.098(7) -0.008(8) 0.011(6) 0.071(8) C20 0.119(8) 0.119(9) 0.104(7) -0.034(7) -0.011(6) 0.022(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co3 C1 2.032(5) . ? Co3 C2 2.035(5) . ? Co3 C2' 2.053(5) . ? Co3 B7' 2.070(6) . ? Co3 C1' 2.076(5) . ? Co3 B4 2.093(5) . ? Co3 B7 2.095(6) . ? Co3 B4' 2.097(6) . ? Co3 B8' 2.117(6) . ? Co3 B8 2.147(6) . ? K O1 2.656(4) . ? K O2 2.937(5) . ? K C18 3.167(8) . ? K C17 3.249(8) . ? K C19 3.281(9) . ? K N 3.360(6) . ? K C20 3.396(9) . ? K B8 3.405(6) . ? K B7 3.442(7) . ? O1 C13 1.408(6) . ? O1 B8 1.418(7) . ? O2 C14 1.399(7) . ? O2 C15 1.412(8) . ? N C17 1.352(11) . ? N C20 1.354(10) . ? N C16 1.462(10) . ? C1 C2 1.624(7) . ? C1 B5 1.673(7) . ? C1 B4 1.702(7) . ? C1 B6 1.724(8) . ? C1 H1 1.1000 . ? C2 B11 1.680(8) . ? C2 B7 1.700(8) . ? C2 B6 1.719(8) . ? C2 H2 1.1000 . ? B4 B9 1.786(8) . ? B4 B5 1.800(8) . ? B4 B8 1.829(8) . ? B4 H4 1.1000 . ? B5 B6 1.755(9) . ? B5 B10 1.757(9) . ? B5 B9 1.768(9) . ? B5 H5 1.1000 . ? B6 B11 1.748(11) . ? B6 B10 1.761(10) . ? B6 H6 1.1000 . ? B7 B12 1.768(8) . ? B7 B11 1.791(9) . ? B7 B8 1.809(8) . ? B7 H7 1.1000 . ? B8 B9 1.816(8) . ? B8 B12 1.817(9) . ? B9 B10 1.770(10) . ? B9 B12 1.797(8) . ? B9 H9 1.1000 . ? B10 B11 1.764(9) . ? B10 B12 1.772(10) . ? B10 H10 1.1000 . ? B11 B12 1.758(10) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1' C2' 1.642(7) . ? C1' B5' 1.735(8) . ? C1' B4' 1.740(8) . ? C1' B6' 1.741(8) . ? C1' H1' 1.1000 . ? C2' B7' 1.659(7) . ? C2' B11' 1.681(8) . ? C2' B6' 1.714(7) . ? C2' H2' 1.1000 . ? B4' B9' 1.796(8) . ? B4' B5' 1.807(8) . ? B4' B8' 1.818(7) . ? B4' H4' 1.1000 . ? B5' B6' 1.767(9) . ? B5' B10' 1.768(9) . ? B5' B9' 1.769(8) . ? B5' H5' 1.1000 . ? B6' B11' 1.764(9) . ? B6' B10' 1.772(9) . ? B6' H6' 1.1000 . ? B7' B12' 1.734(9) . ? B7' B11' 1.746(8) . ? B7' B8' 1.764(8) . ? B7' H7' 1.1000 . ? B8' B9' 1.790(8) . ? B8' B12' 1.793(9) . ? B8' H8' 1.1000 . ? B9' B10' 1.773(10) . ? B9' B12' 1.785(9) . ? B9' H9' 1.1000 . ? B10' B12' 1.767(9) . ? B10' B11' 1.776(10) . ? B10' H10' 1.1000 . ? B11' B12' 1.747(10) . ? B11' H11' 1.1000 . ? B12' H12' 1.1000 . ? C13 C14 1.471(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.485(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.376(12) . ? C17 H17 0.9300 . ? C18 C19 1.403(14) . ? C18 H18 0.9300 . ? C19 C20 1.347(13) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co3 C2 47.1(2) . . ? C1 Co3 C2' 98.3(2) . . ? C2 Co3 C2' 98.1(2) . . ? C1 Co3 B7' 96.3(2) . . ? C2 Co3 B7' 129.8(2) . . ? C2' Co3 B7' 47.4(2) . . ? C1 Co3 C1' 130.9(2) . . ? C2 Co3 C1' 97.5(2) . . ? C2' Co3 C1' 46.84(19) . . ? B7' Co3 C1' 82.8(2) . . ? C1 Co3 B4 48.7(2) . . ? C2 Co3 B4 83.9(2) . . ? C2' Co3 B4 130.5(2) . . ? B7' Co3 B4 94.3(2) . . ? C1' Co3 B4 177.1(2) . . ? C1 Co3 B7 83.4(2) . . ? C2 Co3 B7 48.6(2) . . ? C2' Co3 B7 130.4(2) . . ? B7' Co3 B7 177.8(2) . . ? C1' Co3 B7 95.7(2) . . ? B4 Co3 B7 87.1(2) . . ? C1 Co3 B4' 177.8(2) . . ? C2 Co3 B4' 131.1(2) . . ? C2' Co3 B4' 83.2(2) . . ? B7' Co3 B4' 86.0(2) . . ? C1' Co3 B4' 49.3(2) . . ? B4 Co3 B4' 131.3(2) . . ? B7 Co3 B4' 94.3(2) . . ? C1 Co3 B8' 130.6(2) . . ? C2 Co3 B8' 177.4(2) . . ? C2' Co3 B8' 83.3(2) . . ? B7' Co3 B8' 49.8(2) . . ? C1' Co3 B8' 85.0(2) . . ? B4 Co3 B8' 93.5(2) . . ? B7 Co3 B8' 131.8(2) . . ? B4' Co3 B8' 51.1(2) . . ? C1 Co3 B8 84.3(2) . . ? C2 Co3 B8 84.3(2) . . ? C2' Co3 B8 177.2(2) . . ? B7' Co3 B8 131.7(2) . . ? C1' Co3 B8 131.5(2) . . ? B4 Co3 B8 51.1(2) . . ? B7 Co3 B8 50.5(2) . . ? B4' Co3 B8 94.2(2) . . ? B8' Co3 B8 94.4(2) . . ? O1 K O2 59.66(12) . . ? O1 K C18 125.8(3) . . ? O2 K C18 86.4(3) . . ? O1 K C17 106.3(2) . . ? O2 K C17 61.8(2) . . ? C18 K C17 24.7(2) . . ? O1 K C19 144.9(2) . . ? O2 K C19 90.6(2) . . ? C18 K C19 25.0(2) . . ? C17 K C19 38.9(2) . . ? O1 K N 109.25(16) . . ? O2 K N 52.37(16) . . ? C18 K N 40.1(3) . . ? C17 K N 23.54(19) . . ? C19 K N 38.2(2) . . ? O1 K C20 130.8(2) . . ? O2 K C20 71.5(2) . . ? C18 K C20 40.1(3) . . ? C17 K C20 38.4(2) . . ? C19 K C20 23.2(2) . . ? N K C20 23.12(17) . . ? O1 K B8 23.09(13) . . ? O2 K B8 79.70(14) . . ? C18 K B8 122.0(3) . . ? C17 K B8 111.1(2) . . ? C19 K B8 146.8(3) . . ? N K B8 122.80(17) . . ? C20 K B8 145.91(19) . . ? O1 K B7 53.11(13) . . ? O2 K B7 109.76(14) . . ? C18 K B7 117.0(3) . . ? C17 K B7 120.5(2) . . ? C19 K B7 137.7(3) . . ? N K B7 141.52(18) . . ? C20 K B7 156.9(2) . . ? B8 K B7 30.64(14) . . ? C13 O1 B8 119.5(4) . . ? C13 O1 K 122.8(3) . . ? B8 O1 K 109.6(3) . . ? C14 O2 C15 113.3(6) . . ? C14 O2 K 104.3(3) . . ? C15 O2 K 111.7(4) . . ? C17 N C20 108.2(9) . . ? C17 N C16 125.7(9) . . ? C20 N C16 126.0(10) . . ? C17 N K 73.6(5) . . ? C20 N K 79.9(5) . . ? C16 N K 110.2(5) . . ? C2 C1 B5 111.1(4) . . ? C2 C1 B4 112.1(4) . . ? B5 C1 B4 64.4(3) . . ? C2 C1 B6 61.7(3) . . ? B5 C1 B6 62.2(4) . . ? B4 C1 B6 116.4(4) . . ? C2 C1 Co3 66.5(2) . . ? B5 C1 Co3 125.9(4) . . ? B4 C1 Co3 67.5(3) . . ? B6 C1 Co3 124.8(4) . . ? C2 C1 H1 121.9 . . ? B5 C1 H1 116.2 . . ? B4 C1 H1 117.5 . . ? B6 C1 H1 115.5 . . ? Co3 C1 H1 106.8 . . ? C1 C2 B11 110.9(4) . . ? C1 C2 B7 111.4(4) . . ? B11 C2 B7 64.0(4) . . ? C1 C2 B6 62.0(3) . . ? B11 C2 B6 61.9(4) . . ? B7 C2 B6 115.6(5) . . ? C1 C2 Co3 66.4(2) . . ? B11 C2 Co3 125.7(4) . . ? B7 C2 Co3 67.6(3) . . ? B6 C2 Co3 125.0(3) . . ? C1 C2 H2 122.0 . . ? B11 C2 H2 116.5 . . ? B7 C2 H2 118.2 . . ? B6 C2 H2 115.6 . . ? Co3 C2 H2 106.8 . . ? C1 B4 B9 102.6(4) . . ? C1 B4 B5 57.0(3) . . ? B9 B4 B5 59.1(4) . . ? C1 B4 B8 105.2(4) . . ? B9 B4 B8 60.3(3) . . ? B5 B4 B8 107.8(4) . . ? C1 B4 Co3 63.8(2) . . ? B9 B4 Co3 117.9(3) . . ? B5 B4 Co3 116.0(3) . . ? B8 B4 Co3 66.0(2) . . ? C1 B4 H4 126.4 . . ? B9 B4 H4 121.5 . . ? B5 B4 H4 121.3 . . ? B8 B4 H4 121.8 . . ? Co3 B4 H4 111.9 . . ? C1 B5 B6 60.3(3) . . ? C1 B5 B10 105.6(4) . . ? B6 B5 B10 60.2(4) . . ? C1 B5 B9 104.6(4) . . ? B6 B5 B9 109.0(5) . . ? B10 B5 B9 60.3(4) . . ? C1 B5 B4 58.6(3) . . ? B6 B5 B4 110.0(4) . . ? B10 B5 B4 108.9(5) . . ? B9 B5 B4 60.1(3) . . ? C1 B5 H5 124.5 . . ? B6 B5 H5 120.1 . . ? B10 B5 H5 122.0 . . ? B9 B5 H5 122.4 . . ? B4 B5 H5 120.8 . . ? C2 B6 C1 56.3(3) . . ? C2 B6 B11 58.0(4) . . ? C1 B6 B11 103.2(5) . . ? C2 B6 B5 103.1(4) . . ? C1 B6 B5 57.5(3) . . ? B11 B6 B5 107.7(5) . . ? C2 B6 B10 103.8(5) . . ? C1 B6 B10 103.3(5) . . ? B11 B6 B10 60.3(4) . . ? B5 B6 B10 60.0(4) . . ? C2 B6 H6 125.5 . . ? C1 B6 H6 125.8 . . ? B11 B6 H6 122.3 . . ? B5 B6 H6 122.7 . . ? B10 B6 H6 123.2 . . ? C2 B7 B12 103.4(4) . . ? C2 B7 B11 57.4(3) . . ? B12 B7 B11 59.2(4) . . ? C2 B7 B8 106.2(4) . . ? B12 B7 B8 61.0(3) . . ? B11 B7 B8 108.8(4) . . ? C2 B7 Co3 63.8(2) . . ? B12 B7 Co3 118.8(4) . . ? B11 B7 Co3 116.6(4) . . ? B8 B7 Co3 66.3(3) . . ? C2 B7 K 175.0(3) . . ? B12 B7 K 80.9(3) . . ? B11 B7 K 127.5(4) . . ? B8 B7 K 73.5(3) . . ? Co3 B7 K 112.0(2) . . ? C2 B7 H7 126.0 . . ? B12 B7 H7 121.0 . . ? B11 B7 H7 120.9 . . ? B8 B7 H7 121.0 . . ? Co3 B7 H7 111.5 . . ? K B7 H7 52.0 . . ? O1 B8 B7 121.0(5) . . ? O1 B8 B9 120.7(5) . . ? B7 B8 B9 105.1(5) . . ? O1 B8 B12 115.8(5) . . ? B7 B8 B12 58.4(3) . . ? B9 B8 B12 59.3(3) . . ? O1 B8 B4 129.3(5) . . ? B7 B8 B4 105.0(4) . . ? B9 B8 B4 58.7(3) . . ? B12 B8 B4 105.4(4) . . ? O1 B8 Co3 119.0(4) . . ? B7 B8 Co3 63.3(3) . . ? B9 B8 Co3 113.9(4) . . ? B12 B8 Co3 114.0(4) . . ? B4 B8 Co3 62.9(2) . . ? O1 B8 K 47.3(2) . . ? B7 B8 K 75.8(3) . . ? B9 B8 K 128.5(3) . . ? B12 B8 K 81.5(3) . . ? B4 B8 K 172.5(4) . . ? Co3 B8 K 111.8(2) . . ? B5 B9 B10 59.5(4) . . ? B5 B9 B4 60.9(3) . . ? B10 B9 B4 108.9(5) . . ? B5 B9 B12 106.8(5) . . ? B10 B9 B12 59.6(4) . . ? B4 B9 B12 108.0(4) . . ? B5 B9 B8 109.8(4) . . ? B10 B9 B8 109.6(4) . . ? B4 B9 B8 61.0(3) . . ? B12 B9 B8 60.4(3) . . ? B5 B9 H9 121.7 . . ? B10 B9 H9 121.4 . . ? B4 B9 H9 120.9 . . ? B12 B9 H9 122.6 . . ? B8 B9 H9 120.1 . . ? B5 B10 B6 59.9(4) . . ? B5 B10 B11 106.9(5) . . ? B6 B10 B11 59.5(4) . . ? B5 B10 B9 60.2(4) . . ? B6 B10 B9 108.6(5) . . ? B11 B10 B9 108.1(5) . . ? B5 B10 B12 108.4(5) . . ? B6 B10 B12 108.1(5) . . ? B11 B10 B12 59.6(4) . . ? B9 B10 B12 61.0(4) . . ? B5 B10 H10 122.0 . . ? B6 B10 H10 121.7 . . ? B11 B10 H10 122.5 . . ? B9 B10 H10 121.0 . . ? B12 B10 H10 121.3 . . ? C2 B11 B6 60.2(4) . . ? C2 B11 B12 104.7(4) . . ? B6 B11 B12 109.3(5) . . ? C2 B11 B10 105.3(5) . . ? B6 B11 B10 60.2(4) . . ? B12 B11 B10 60.4(4) . . ? C2 B11 B7 58.6(3) . . ? B6 B11 B7 109.7(5) . . ? B12 B11 B7 59.8(4) . . ? B10 B11 B7 108.3(5) . . ? C2 B11 H11 124.5 . . ? B6 B11 H11 120.0 . . ? B12 B11 H11 122.2 . . ? B10 B11 H11 122.2 . . ? B7 B11 H11 121.2 . . ? B11 B12 B7 61.1(4) . . ? B11 B12 B10 60.0(4) . . ? B7 B12 B10 109.0(5) . . ? B11 B12 B9 107.2(5) . . ? B7 B12 B9 107.6(4) . . ? B10 B12 B9 59.5(4) . . ? B11 B12 B8 110.0(4) . . ? B7 B12 B8 60.6(3) . . ? B10 B12 B8 109.4(4) . . ? B9 B12 B8 60.3(3) . . ? B11 B12 H12 121.2 . . ? B7 B12 H12 121.2 . . ? B10 B12 H12 121.3 . . ? B9 B12 H12 122.7 . . ? B8 B12 H12 120.3 . . ? C2' C1' B5' 108.3(4) . . ? C2' C1' B4' 109.0(4) . . ? B5' C1' B4' 62.7(3) . . ? C2' C1' B6' 60.8(3) . . ? B5' C1' B6' 61.1(3) . . ? B4' C1' B6' 113.2(4) . . ? C2' C1' Co3 65.8(2) . . ? B5' C1' Co3 122.1(3) . . ? B4' C1' Co3 66.0(2) . . ? B6' C1' Co3 122.5(3) . . ? C2' C1' H1' 123.2 . . ? B5' C1' H1' 118.5 . . ? B4' C1' H1' 119.9 . . ? B6' C1' H1' 116.9 . . ? Co3 C1' H1' 109.0 . . ? C1' C2' B7' 112.3(4) . . ? C1' C2' B11' 113.3(4) . . ? B7' C2' B11' 63.0(3) . . ? C1' C2' B6' 62.5(3) . . ? B7' C2' B6' 114.5(4) . . ? B11' C2' B6' 62.6(4) . . ? C1' C2' Co3 67.3(2) . . ? B7' C2' Co3 66.8(3) . . ? B11' C2' Co3 125.0(4) . . ? B6' C2' Co3 125.4(3) . . ? C1' C2' H2' 119.9 . . ? B7' C2' H2' 119.3 . . ? B11' C2' H2' 116.0 . . ? B6' C2' H2' 115.6 . . ? Co3 C2' H2' 106.9 . . ? C1' B4' B9' 104.0(4) . . ? C1' B4' B5' 58.5(3) . . ? B9' B4' B5' 58.8(3) . . ? C1' B4' B8' 105.6(4) . . ? B9' B4' B8' 59.4(3) . . ? B5' B4' B8' 106.8(4) . . ? C1' B4' Co3 64.7(2) . . ? B9' B4' Co3 117.0(4) . . ? B5' B4' Co3 117.4(4) . . ? B8' B4' Co3 65.0(3) . . ? C1' B4' H4' 124.7 . . ? B9' B4' H4' 121.8 . . ? B5' B4' H4' 120.8 . . ? B8' B4' H4' 123.0 . . ? Co3 B4' H4' 111.7 . . ? C1' B5' B6' 59.6(3) . . ? C1' B5' B10' 106.1(4) . . ? B6' B5' B10' 60.2(4) . . ? C1' B5' B9' 105.4(4) . . ? B6' B5' B9' 108.3(5) . . ? B10' B5' B9' 60.2(4) . . ? C1' B5' B4' 58.8(3) . . ? B6' B5' B4' 108.8(4) . . ? B10' B5' B4' 108.9(4) . . ? B9' B5' B4' 60.3(3) . . ? C1' B5' H5' 123.9 . . ? B6' B5' H5' 121.1 . . ? B10' B5' H5' 121.7 . . ? B9' B5' H5' 122.2 . . ? B4' B5' H5' 121.1 . . ? C2' B6' C1' 56.7(3) . . ? C2' B6' B11' 57.8(3) . . ? C1' B6' B11' 104.7(4) . . ? C2' B6' B5' 103.6(4) . . ? C1' B6' B5' 59.3(3) . . ? B11' B6' B5' 107.8(5) . . ? C2' B6' B10' 103.8(4) . . ? C1' B6' B10' 105.7(4) . . ? B11' B6' B10' 60.3(4) . . ? B5' B6' B10' 60.0(4) . . ? C2' B6' H6' 125.7 . . ? C1' B6' H6' 123.9 . . ? B11' B6' H6' 122.3 . . ? B5' B6' H6' 122.3 . . ? B10' B6' H6' 122.7 . . ? C2' B7' B12' 106.0(4) . . ? C2' B7' B11' 59.1(3) . . ? B12' B7' B11' 60.3(4) . . ? C2' B7' B8' 108.0(4) . . ? B12' B7' B8' 61.6(4) . . ? B11' B7' B8' 111.0(4) . . ? C2' B7' Co3 65.7(3) . . ? B12' B7' Co3 121.0(4) . . ? B11' B7' Co3 120.5(4) . . ? B8' B7' Co3 66.4(3) . . ? C2' B7' H7' 124.3 . . ? B12' B7' H7' 119.7 . . ? B11' B7' H7' 118.8 . . ? B8' B7' H7' 120.5 . . ? Co3 B7' H7' 109.3 . . ? B7' B8' B9' 105.1(4) . . ? B7' B8' B12' 58.4(4) . . ? B9' B8' B12' 59.7(4) . . ? B7' B8' B4' 105.0(4) . . ? B9' B8' B4' 59.7(3) . . ? B12' B8' B4' 106.9(4) . . ? B7' B8' Co3 63.7(3) . . ? B9' B8' Co3 116.3(3) . . ? B12' B8' Co3 115.8(4) . . ? B4' B8' Co3 63.9(3) . . ? B7' B8' H8' 124.7 . . ? B9' B8' H8' 120.9 . . ? B12' B8' H8' 120.8 . . ? B4' B8' H8' 123.3 . . ? Co3 B8' H8' 113.3 . . ? B5' B9' B10' 59.9(4) . . ? B5' B9' B12' 107.2(5) . . ? B10' B9' B12' 59.6(4) . . ? B5' B9' B8' 109.7(4) . . ? B10' B9' B8' 109.2(5) . . ? B12' B9' B8' 60.2(3) . . ? B5' B9' B4' 60.9(3) . . ? B10' B9' B4' 109.1(4) . . ? B12' B9' B4' 108.2(4) . . ? B8' B9' B4' 60.9(3) . . ? B5' B9' H9' 121.4 . . ? B10' B9' H9' 121.3 . . ? B12' B9' H9' 122.5 . . ? B8' B9' H9' 120.5 . . ? B4' B9' H9' 120.9 . . ? B12' B10' B5' 108.0(5) . . ? B12' B10' B6' 107.4(5) . . ? B5' B10' B6' 59.9(4) . . ? B12' B10' B9' 60.5(4) . . ? B5' B10' B9' 59.9(4) . . ? B6' B10' B9' 107.9(4) . . ? B12' B10' B11' 59.1(4) . . ? B5' B10' B11' 107.2(4) . . ? B6' B10' B11' 59.6(4) . . ? B9' B10' B11' 107.4(4) . . ? B12' B10' H10' 121.9 . . ? B5' B10' H10' 121.9 . . ? B6' B10' H10' 122.0 . . ? B9' B10' H10' 121.6 . . ? B11' B10' H10' 122.6 . . ? C2' B11' B7' 57.9(3) . . ? C2' B11' B12' 104.5(4) . . ? B7' B11' B12' 59.5(4) . . ? C2' B11' B6' 59.6(3) . . ? B7' B11' B6' 107.9(4) . . ? B12' B11' B6' 108.6(5) . . ? C2' B11' B10' 105.0(4) . . ? B7' B11' B10' 107.2(5) . . ? B12' B11' B10' 60.2(4) . . ? B6' B11' B10' 60.0(4) . . ? C2' B11' H11' 124.7 . . ? B7' B11' H11' 122.3 . . ? B12' B11' H11' 122.3 . . ? B6' B11' H11' 120.9 . . ? B10' B11' H11' 122.4 . . ? B7' B12' B11' 60.2(4) . . ? B7' B12' B10' 108.2(5) . . ? B11' B12' B10' 60.7(4) . . ? B7' B12' B9' 106.6(4) . . ? B11' B12' B9' 108.1(4) . . ? B10' B12' B9' 59.9(4) . . ? B7' B12' B8' 60.0(3) . . ? B11' B12' B8' 109.6(5) . . ? B10' B12' B8' 109.4(5) . . ? B9' B12' B8' 60.1(4) . . ? B7' B12' H12' 122.4 . . ? B11' B12' H12' 120.9 . . ? B10' B12' H12' 121.0 . . ? B9' B12' H12' 122.5 . . ? B8' B12' H12' 120.7 . . ? O1 C13 C14 109.5(5) . . ? O1 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? O1 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? O2 C14 C13 110.6(5) . . ? O2 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O2 C15 C16 107.7(7) . . ? O2 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? O2 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? N C16 C15 113.2(7) . . ? N C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? N C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N C17 C18 110.7(10) . . ? N C17 K 82.8(4) . . ? C18 C17 K 74.3(5) . . ? N C17 H17 124.7 . . ? C18 C17 H17 124.7 . . ? K C17 H17 110.4 . . ? C17 C18 C19 103.0(11) . . ? C17 C18 K 81.0(5) . . ? C19 C18 K 82.0(5) . . ? C17 C18 H18 128.5 . . ? C19 C18 H18 128.5 . . ? K C18 H18 103.7 . . ? C20 C19 C18 110.7(10) . . ? C20 C19 K 83.2(6) . . ? C18 C19 K 72.9(5) . . ? C20 C19 H19 124.6 . . ? C18 C19 H19 124.6 . . ? K C19 H19 111.3 . . ? C19 C20 N 107.2(10) . . ? C19 C20 K 73.6(6) . . ? N C20 K 77.0(5) . . ? C19 C20 H20 126.4 . . ? N C20 H20 126.4 . . ? K C20 H20 115.3 . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.467 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.072 #===END