Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email SARGESON@RSC.ANU.EDU.AU _publ_contact_author_name 'Prof Alan Sargeson' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Sargeson R.J.Geue K.J.Haller A.D.Rae G.W.Walker data_kjh3 _database_code_CSD 198021 #------------------------------------------------------------------------------ _audit_creation_date 2002-03-14 _audit_creation_method 'by teXsan v1.8' _audit_update_record ; structure also known as glen 2002-03-15 run through checkcif ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; Shelxs86 (Sheldrick, 1986) ; _computing_structure_refinement 'RAELS96 (Rae, 1996)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 15.315(2) _cell_length_b 15.315(2) _cell_length_c 13.764(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3228(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 40.3 _cell_measurement_theta_max 48.7 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_Int_Tables_number 92 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, 1/2+z' ' 1/2-x, 1/2+y, 1/4-z' ' 1/2+x, 1/2-y, 3/4-z' ' +y, x, -z' ' -y, -x, 1/2-z' ' 1/2-y, 1/2+x, 1/4+z' ' 1/2+y, 1/2-x, 3/4+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description octahedron _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 704.07 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H54 Cl3 Co N6 O4 ' _chemical_formula_moiety '(C28 H54 N6 Co 3+), (Cl -)2, (Cl O4 -)' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 6.8 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.495 _exptl_absorpt_correction_T_min 0.367 _exptl_special_details ; The scan width was (1.21+0.14tan\q)\% with an \w scan speed of 5.33\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 4 2 2 0 1 0 3 _diffrn_reflns_number 10049 _reflns_number_total 2414 _reflns_number_gt 1752 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 60.0 _diffrn_reflns_reduction_process 'Lp corrections applied' #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 112 0.0181 0.0091 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 216 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 12 0.3639 0.7018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 4 -2.3653 3.6143 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.00311 0.0180 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.0492 0.0322 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Co1 0.82504(5) 0.17496(5) 0.25000(0) 1.0 0.0305(3) . Uani d ? C1 0.6866(4) 0.0346(4) 0.5045(4) 1.0 0.069(2) . Uani d ? C2 0.7349(4) 0.0795(4) 0.4201(4) 1.0 0.056(2) . Uani d ? C11 0.8302(4) 0.0660(4) 0.4300(4) 1.0 0.052(1) . Uani d ? N12 0.8841(2) 0.0981(2) 0.3467(3) 1.0 0.036(1) . Uani d ? C13 0.9311(3) 0.0261(3) 0.2942(3) 1.0 0.040(1) . Uani d ? C14 0.9973(4) -0.0218(4) 0.3554(4) 1.0 0.055(1) . Uani d ? C15 1.0455(4) -0.0873(4) 0.2946(5) 1.0 0.068(2) . Uani d ? C21 0.7127(4) 0.1777(4) 0.4274(4) 1.0 0.060(2) . Uani d ? N22 0.7565(3) 0.2348(3) 0.3527(3) 1.0 0.037(1) . Uani d ? C23 0.8128(3) 0.3036(3) 0.3987(3) 1.0 0.041(1) . Uani d ? C24 0.7604(4) 0.3738(4) 0.4515(4) 1.0 0.057(2) . Uani d ? C25 0.8213(4) 0.4438(4) 0.4917(5) 1.0 0.068(2) . Uani d ? C26 0.8788(4) 0.4820(4) 0.4129(5) 1.0 0.065(2) . Uani d ? C27 0.9308(4) 0.4121(4) 0.3602(4) 1.0 0.056(2) . Uani d ? C28 0.8674(3) 0.3448(3) 0.3190(4) 1.0 0.038(1) . Uani d ? N29 0.9117(3) 0.2703(2) 0.2660(3) 1.0 0.037(1) . Uani d ? C30 0.9559(4) 0.3001(4) 0.1737(4) 1.0 0.058(1) . Uani d ? Cl1 1.0446(1) 0.2052(1) 0.4307(1) 1.0 0.056(1) . Uani d ? Cl2 0.7358(6) 0.2733(7) 0.7400(8) 0.5 0.112(6) . Uani d ? O1 0.8007(10) 0.2656(16) 0.6733(14) 0.5 0.243(10) . Uani d ? O2 0.7677(11) 0.3115(13) 0.8218(14) 0.5 0.249(11) . Uani d ? O3 0.6705(9) 0.3234(10) 0.7029(9) 0.5 0.177(8) . Uani d ? O4 0.7041(14) 0.1928(9) 0.7621(18) 0.5 0.220(8) . Uani d ? H1C1 0.6223 0.0440 0.4973 1.0 0.069 . Uani d ? H2C1 0.6995 -0.0294 0.5035 1.0 0.069 . Uani d ? H3C1 0.7068 0.0600 0.5676 1.0 0.069 . Uani d ? H1C11 0.8410 0.0020 0.4373 1.0 0.052 . Uani d ? H2C11 0.8501 0.0971 0.4899 1.0 0.052 . Uani d ? H1N12 0.9310 0.1348 0.3765 1.0 0.036 . Uani d ? H1C13 0.8868 -0.0169 0.2706 1.0 0.040 . Uani d ? H1C14 0.9665 -0.0528 0.4095 1.0 0.055 . Uani d ? H2C14 1.0398 0.0210 0.3832 1.0 0.055 . Uani d ? H1C15 1.0036 -0.1333 0.2727 1.0 0.068 . Uani d ? H2C15 1.0923 -0.1147 0.3350 1.0 0.068 . Uani d ? H1C21 0.7307 0.1987 0.4933 1.0 0.060 . Uani d ? H2C21 0.6481 0.1844 0.4199 1.0 0.060 . Uani d ? H1N22 0.7085 0.2666 0.3185 1.0 0.037 . Uani d ? H1C23 0.8528 0.2748 0.4464 1.0 0.041 . Uani d ? H1C24 0.7274 0.3464 0.5063 1.0 0.057 . Uani d ? H2C24 0.7184 0.4012 0.4050 1.0 0.057 . Uani d ? H1C25 0.8591 0.4173 0.5430 1.0 0.068 . Uani d ? H2C25 0.7853 0.4916 0.5209 1.0 0.068 . Uani d ? H1C26 0.9204 0.5244 0.4432 1.0 0.065 . Uani d ? H2C26 0.8412 0.5132 0.3648 1.0 0.065 . Uani d ? H1C27 0.9717 0.3831 0.4066 1.0 0.056 . Uani d ? H2C27 0.9649 0.4392 0.3061 1.0 0.056 . Uani d ? H1C28 0.8273 0.3750 0.2726 1.0 0.038 . Uani d ? H1N29 0.9586 0.2476 0.3099 1.0 0.037 . Uani d ? H1C30 0.9516 0.3652 0.1711 1.0 0.058 . Uani d ? H2C30 1.0187 0.2825 0.1778 1.0 0.058 . Uani 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0304(3) 0.0304(3) 0.0305(5) -0.0005(5) -0.0006(3) -0.0006(3) C1 0.066(4) 0.080(4) 0.060(3) 0.001(3) 0.015(4) 0.028(4) C2 0.050(3) 0.069(4) 0.050(3) -0.001(3) 0.007(3) 0.016(3) C11 0.051(3) 0.061(4) 0.044(3) 0.000(3) -0.003(3) 0.016(3) N12 0.033(2) 0.036(2) 0.040(2) 0.001(2) -0.003(2) 0.003(2) C13 0.044(3) 0.032(3) 0.044(3) 0.000(2) -0.008(2) -0.003(2) C14 0.053(4) 0.054(3) 0.057(3) 0.009(3) -0.011(3) 0.005(3) C15 0.064(4) 0.057(4) 0.084(5) 0.021(3) -0.021(3) -0.003(3) C21 0.069(4) 0.063(3) 0.048(3) 0.001(3) 0.011(3) 0.001(3) N22 0.034(2) 0.043(3) 0.034(2) 0.002(2) 0.000(2) -0.002(2) C23 0.039(3) 0.046(3) 0.038(3) 0.010(2) -0.001(2) -0.009(2) C24 0.058(4) 0.067(4) 0.046(3) 0.015(3) -0.003(3) -0.019(3) C25 0.070(4) 0.062(4) 0.073(4) 0.013(3) -0.016(4) -0.034(3) C26 0.059(4) 0.045(3) 0.093(5) 0.001(3) -0.015(4) -0.025(3) C27 0.052(4) 0.044(3) 0.073(4) 0.000(3) -0.017(3) -0.011(3) C28 0.043(3) 0.034(3) 0.038(3) 0.002(2) -0.007(2) -0.005(2) N29 0.037(2) 0.031(2) 0.042(2) 0.003(2) 0.001(2) -0.004(2) C30 0.066(4) 0.053(3) 0.053(3) -0.021(3) 0.003(3) 0.001(3) Cl1 0.049(1) 0.053(1) 0.067(1) -0.003(1) -0.019(1) -0.008(1) Cl2 0.098(6) 0.100(6) 0.139(7) -0.019(6) 0.031(4) 0.030(4) O1 0.217(11) 0.253(14) 0.258(13) 0.085(11) 0.149(12) 0.122(12) O2 0.232(13) 0.265(13) 0.249(15) -0.028(18) -0.072(13) -0.055(11) O3 0.149(6) 0.204(11) 0.179(10) 0.038(8) 0.028(6) 0.071(9) O4 0.218(17) 0.100(11) 0.342(22) -0.038(6) 0.078(7) 0.044(6) H1C1 0.066 0.080 0.060 0.001 0.015 0.028 H2C1 0.066 0.080 0.060 0.001 0.015 0.028 H3C1 0.066 0.080 0.060 0.001 0.015 0.028 H1C11 0.051 0.061 0.044 0.000 -0.003 0.016 H2C11 0.051 0.061 0.044 0.000 -0.003 0.016 H1N12 0.033 0.036 0.040 0.001 -0.003 0.003 H1C13 0.044 0.032 0.044 0.000 -0.008 -0.003 H1C14 0.053 0.054 0.057 0.009 -0.011 0.005 H2C14 0.053 0.054 0.057 0.009 -0.011 0.005 H1C15 0.064 0.057 0.084 0.021 -0.021 -0.003 H2C15 0.064 0.057 0.084 0.021 -0.021 -0.003 H1C21 0.069 0.063 0.048 0.001 0.011 0.001 H2C21 0.069 0.063 0.048 0.001 0.011 0.001 H1N22 0.034 0.043 0.034 0.002 0.000 -0.002 H1C23 0.039 0.046 0.038 0.010 -0.001 -0.009 H1C24 0.058 0.067 0.046 0.015 -0.003 -0.019 H2C24 0.058 0.067 0.046 0.015 -0.003 -0.019 H1C25 0.070 0.062 0.073 0.013 -0.016 -0.034 H2C25 0.070 0.062 0.073 0.013 -0.016 -0.034 H1C26 0.059 0.045 0.093 0.001 -0.015 -0.025 H2C26 0.059 0.045 0.093 0.001 -0.015 -0.025 H1C27 0.052 0.044 0.073 0.000 -0.017 -0.011 H2C27 0.052 0.044 0.073 0.000 -0.017 -0.011 H1C28 0.043 0.034 0.038 0.002 -0.007 -0.005 H1N29 0.037 0.031 0.042 0.003 0.001 -0.004 H1C30 0.066 0.053 0.053 -0.021 0.003 0.001 H2C30 0.066 0.053 0.053 -0.021 0.003 0.001 #------------------------------------------------------------------------------ _refine_special_details ; The perchlorate anion is 1:1 disordered about a crystallographic two-fold axis. It was refined in a general position with half-occupancy. It was constrained to have exact tetrahedral geometry with a refinable bond length, and to have anisotropic thermal parameters defined by a refinable 15 parameter TLX model. Hydrogen atoms were included at sensible geometric positions before each cycle and given the same anisotropic thermal parameters as the atoms to which they were attached. The alternative configuration requiring space group P43212 was tested. The large anomalous dispersion with Cu radiation allows a clear preference for P41212. _refine_ls_R_factor_gt = 0.126 compared to 0.0395. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Absolute structure by comparative refinement. Opposite hand in P4~3~2~1~2 gives R=0.126, wR=0.178, S=4.66. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1752 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_all 0.0582 _refine_ls_wR_factor_ref 0.0526 _refine_ls_goodness_of_fit_all 1.300 _refine_ls_goodness_of_fit_ref 1.376 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.020 _refine_diff_density_min -0.9 _refine_diff_density_max 1.5 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N12 1.995(4) . . yes Co1 N22 1.985(4) . . yes Co1 N29 1.986(4) . . yes C1 C2 1.540(7) . . yes C2 C30 1.499(7) . 6_665 yes C2 C11 1.481(8) . . yes C11 N12 1.495(6) . . yes N12 C13 1.502(6) . . yes C13 C13 1.528(9) . 6_665 yes C13 C14 1.509(7) . . yes C14 C15 1.501(8) . . yes C15 C15 1.525(13) . 6_665 yes C2 C21 1.545(8) . . yes C21 N22 1.506(7) . . yes N22 C23 1.501(6) . . yes C23 C24 1.525(7) . . yes C24 C25 1.525(8) . . yes C25 C26 1.516(9) . . yes C26 C27 1.519(7) . . yes C23 C28 1.517(7) . . yes C27 C28 1.524(7) . . yes C28 N29 1.515(6) . . yes N29 C30 1.510(6) . . yes C30 C2 1.499(7) . *6_665 yes N12 Cl1 3.173(4) . . yes N29 Cl1 3.205(4) . . yes N22 Cl1 3.404(4) . 4_455 yes Cl2 O1 1.359(7) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N22 Co1 N29 86.3(2) . . . yes N12 Co1 N12 84.8(2) . . 6_665 yes N12 Co1 N22 92.1(1) . . . yes N12 Co1 N29 93.2(2) . . . yes N12 Co1 N29 90.8(2) . . 6_665 yes N22 Co1 N22 91.1(2) . . 6_665 yes N22 Co1 N29 89.9(2) . . 6_665 yes N12 Co1 N22 175.6(2) . . 6_665 yes N29 Co1 N29 174.6(2) . . 6_665 yes C1 C2 C11 110.0(4) . . . yes C1 C2 C21 106.3(5) . . . yes C11 C2 C21 110.3(5) . . . yes C1 C2 C30 108.4(5) . . 6_665 yes C11 C2 C30 112.4(5) . . 6_665 yes C21 C2 C30 109.3(5) . . 6_665 yes C2 C11 N12 115.4(4) . . . yes Co1 N12 C11 117.0(3) . . . yes Co1 N12 C13 109.2(3) . . . yes C11 N12 C13 113.1(4) . . . yes N12 C13 C14 114.2(4) . . . yes N12 C13 C13 105.9(3) . . 6_665 yes C14 C13 C13 111.4(3) . . 6_665 yes C13 C14 C15 110.1(4) . . . yes C14 C15 C15 112.1(4) . . 6_665 yes C2 C21 N22 115.0(4) . . . yes Co1 N22 C21 117.0(3) . . . yes Co1 N22 C23 108.7(3) . . . yes C21 N22 C23 112.0(4) . . . yes N22 C23 C24 113.2(4) . . . yes N22 C23 C28 107.7(4) . . . yes C24 C23 C28 109.9(4) . . . yes C23 C24 C25 110.4(4) . . . yes C24 C25 C26 111.5(5) . . . yes C25 C26 C27 112.0(5) . . . yes C26 C27 C28 108.7(4) . . . yes C23 C28 C27 111.3(4) . . . yes C23 C28 N29 106.4(3) . . . yes C27 C28 N29 113.8(4) . . . yes Co1 N29 C28 107.9(3) . . . yes Co1 N29 C30 115.3(3) . . . yes C28 N29 C30 112.2(4) . . . yes N29 C30 C2 117.0(4) . . 6_665 yes Co1 N12 Cl1 106.8(1) . . . yes C11 N12 Cl1 108.6(3) . . . yes C13 N12 Cl1 100.6(2) . . . yes Co1 N22 Cl1 122.2(2) . . 4_455 yes C21 N22 Cl1 79.9(3) . . 4_455 yes C23 N22 Cl1 114.5(2) . . 4_455 yes Co1 N29 Cl1 105.9(1) . . . yes C28 N29 Cl1 100.2(2) . . . yes C30 N29 Cl1 113.9(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 N12 Co1 N22 37.8(4) . . . . no C13 N12 Co1 N22 167.9(3) . . . . no C11 N12 Co1 N29 124.2(3) . . . . no C13 N12 Co1 N29 -105.6(3) . . . . no C11 N12 Co1 N12 -145.3(4) . . . 6_665 no C13 N12 Co1 N12 -15.2(2) . . . 6_665 no C11 N12 Co1 N29 -52.2(4) . . . 6_665 no C13 N12 Co1 N29 78.0(3) . . . 6_665 no C21 N22 Co1 N12 -46.5(4) . . . . no C23 N22 Co1 N12 81.5(3) . . . . no C21 N22 Co1 N29 -139.6(4) . . . . no C23 N22 Co1 N29 -11.6(3) . . . . no C21 N22 Co1 N22 130.5(4) . . . 6_665 no C23 N22 Co1 N22 -101.4(3) . . . 6_665 no C21 N22 Co1 N29 44.2(4) . . . 6_665 no C23 N22 Co1 N29 172.3(3) . . . 6_665 no C28 N29 Co1 N12 -109.0(3) . . . . no C30 N29 Co1 N12 124.6(4) . . . . no C28 N29 Co1 N22 -17.1(3) . . . . no C30 N29 Co1 N22 -143.5(4) . . . . no C28 N29 Co1 N12 166.2(3) . . . 6_665 no C30 N29 Co1 N12 39.8(4) . . . 6_665 no C28 N29 Co1 N22 74.1(3) . . . 6_665 no C30 N29 Co1 N22 -52.4(4) . . . 6_665 no N12 C11 C2 C1 173.6(5) . . . . no N12 C11 C2 C21 -69.5(6) . . . . no N12 C11 C2 C30 52.7(7) . . . 6_665 no N22 C21 C2 C1 177.9(5) . . . . no N22 C21 C2 C11 58.7(6) . . . . no N22 C21 C2 C30 -65.3(6) . . . 6_665 no Co1 N12 C11 C2 12.5(6) . . . . no C13 N12 C11 C2 -115.8(5) . . . . no C14 C13 N12 Co1 164.6(3) . . . . no C13 C13 N12 Co1 41.6(4) 6_665 . . . no C14 C13 N12 C11 -63.2(5) . . . . no C13 C13 N12 C11 173.8(4) 6_665 . . . no C15 C14 C13 N12 -175.5(4) . . . . no C15 C14 C13 C13 -55.6(6) . . . 6_665 no C15 C15 C14 C13 54.8(7) 6_665 . . . no Co1 N22 C21 C2 5.9(6) . . . . no C23 N22 C21 C2 -120.5(5) . . . . no C24 C23 N22 Co1 159.6(3) . . . . no C28 C23 N22 Co1 37.9(4) . . . . no C24 C23 N22 C21 -69.6(5) . . . . no C28 C23 N22 C21 168.7(4) . . . . no C25 C24 C23 N22 -177.1(5) . . . . no C25 C24 C23 C28 -56.6(6) . . . . no C27 C28 C23 N22 -176.7(4) . . . . no N29 C28 C23 N22 -52.2(4) . . . . no C27 C28 C23 C24 59.6(5) . . . . no N29 C28 C23 C24 -175.9(4) . . . . no C26 C25 C24 C23 54.8(6) . . . . no C27 C26 C25 C24 -55.6(6) . . . . no C28 C27 C26 C25 56.4(6) . . . . no C23 C28 C27 C26 -58.7(5) . . . . no N29 C28 C27 C26 181.1(4) . . . . no Co1 N29 C28 C23 41.7(4) . . . . no C30 N29 C28 C23 169.9(4) . . . . no Cl1 N29 C28 C23 -68.9(3) . . . . no Co1 N29 C28 C27 164.7(3) . . . . no C30 N29 C28 C27 -67.1(5) . . . . no C2 C30 N29 Co1 9.1(6) 6_665 . . . no C2 C30 N29 C28 -115.1(5) 6_665 . . . no #------------------------------------------------------------------------------ #===END