# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1806 data_GLOBAL # 1. SUBMISSION DETAILS _publ_contact_author_name 'Gleiter, Rolf' _publ_contact_author_address ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8400' _publ_contact_author_fax '049 6221 54- 4205' _publ_contact_author_email 'rolf.gleiter@urz.uni-heidelberg.de' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; paper to be submitted for publication in J. Chem. Soc. Dalton Trans. ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Reaction of N,N'-bridged 1,10-diazacyclooctadeca-5,14-diynes with [CpCo(COD)]- A new type of superphanes ; loop_ _publ_author_name _publ_author_address 'Gleiter, Rolf' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'von Hirschheydt, Thomas' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Volker Wolfart' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #======================================================================= data_3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H39 Co N2' _chemical_formula_weight 438.52 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' '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 7.65670(10) _cell_length_b 9.7915(2) _cell_length_c 16.0835(3) _cell_angle_alpha 87.2610(10) _cell_angle_beta 77.4330(10) _cell_angle_gamma 75.0540(10) _cell_volume 1137.04(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_absorpt_correction_T_min .81 _exptl_absorpt_correction_T_max .90 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8530 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.62 _reflns_number_total 3796 _reflns_number_gt 3542 _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^)+(0.0446P)^2^+0.4958P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3796 _refine_ls_number_parameters 263 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.14582(3) 0.23524(3) 0.116990(14) 0.02440(10) Uani 1 1 d . . . N1 N 0.3981(2) 0.12890(17) 0.37821(10) 0.0299(4) Uani 1 1 d . . . C2 C 0.5376(3) 0.0148(2) 0.32748(13) 0.0385(5) Uani 1 1 d . . . H2A H 0.5339 -0.0763 0.3564 0.046 Uiso 1 1 calc R . . H2B H 0.6617 0.0300 0.3246 0.046 Uiso 1 1 calc R . . C3 C 0.5092(3) 0.0055(2) 0.23684(13) 0.0390(5) Uani 1 1 d . . . H3A H 0.6103 -0.0707 0.2053 0.047 Uiso 1 1 calc R . . H3B H 0.3911 -0.0199 0.2395 0.047 Uiso 1 1 calc R . . C4 C 0.5058(3) 0.1430(2) 0.18870(12) 0.0319(4) Uani 1 1 d . . . H4A H 0.5807 0.1944 0.2118 0.038 Uiso 1 1 calc R . . H4B H 0.5656 0.1204 0.1282 0.038 Uiso 1 1 calc R . . C5 C 0.3174(2) 0.2387(2) 0.19274(11) 0.0243(4) Uani 1 1 d . . . C6 C 0.2530(2) 0.3770(2) 0.15628(11) 0.0249(4) Uani 1 1 d . . . C7 C 0.3503(3) 0.4708(2) 0.09814(12) 0.0333(4) Uani 1 1 d . . . H7A H 0.2719 0.5146 0.0576 0.040 Uiso 1 1 calc R . . H7B H 0.4668 0.4112 0.0645 0.040 Uiso 1 1 calc R . . C8 C 0.3971(3) 0.5887(3) 0.14152(15) 0.0444(5) Uani 1 1 d . . . H8A H 0.4702 0.5463 0.1843 0.053 Uiso 1 1 calc R . . H8B H 0.4749 0.6357 0.0983 0.053 Uiso 1 1 calc R . . C9 C 0.2263(4) 0.6994(2) 0.18527(16) 0.0488(6) Uani 1 1 d . . . H9A H 0.2604 0.7892 0.1902 0.059 Uiso 1 1 calc R . . H9B H 0.1324 0.7171 0.1497 0.059 Uiso 1 1 calc R . . N10 N 0.1464(2) 0.65609(17) 0.26959(11) 0.0347(4) Uani 1 1 d . . . C11 C -0.0556(3) 0.7023(2) 0.29489(17) 0.0489(6) Uani 1 1 d . . . H11A H -0.1023 0.7698 0.2521 0.059 Uiso 1 1 calc R . . H11B H -0.0894 0.7533 0.3501 0.059 Uiso 1 1 calc R . . C12 C -0.1510(3) 0.5834(2) 0.30355(14) 0.0400(5) Uani 1 1 d . . . H12A H -0.2858 0.6245 0.3222 0.048 Uiso 1 1 calc R . . H12B H -0.1103 0.5200 0.3493 0.048 Uiso 1 1 calc R . . C13 C -0.1170(3) 0.4934(2) 0.22271(13) 0.0328(4) Uani 1 1 d . . . H13A H -0.2169 0.4442 0.2287 0.039 Uiso 1 1 calc R . . H13B H -0.1247 0.5572 0.1733 0.039 Uiso 1 1 calc R . . C14 C 0.0654(2) 0.38566(19) 0.20453(11) 0.0244(4) Uani 1 1 d . . . C15 C 0.1289(2) 0.24663(19) 0.24085(11) 0.0236(4) Uani 1 1 d . . . C16 C 0.0308(3) 0.1629(2) 0.30641(12) 0.0308(4) Uani 1 1 d . . . H16A H 0.0779 0.0617 0.2901 0.037 Uiso 1 1 calc R . . H16B H -0.1024 0.1909 0.3052 0.037 Uiso 1 1 calc R . . C17 C 0.0504(3) 0.1792(2) 0.39833(12) 0.0329(4) Uani 1 1 d . . . H17A H 0.0434 0.2796 0.4085 0.040 Uiso 1 1 calc R . . H17B H -0.0558 0.1552 0.4378 0.040 Uiso 1 1 calc R . . C18 C 0.2281(3) 0.0886(2) 0.41986(12) 0.0337(4) Uani 1 1 d . . . H18A H 0.2163 0.0922 0.4823 0.040 Uiso 1 1 calc R . . H18B H 0.2412 -0.0106 0.4041 0.040 Uiso 1 1 calc R . . C19 C 0.4725(3) 0.1970(2) 0.43663(13) 0.0366(5) Uani 1 1 d . . . H19A H 0.6010 0.1990 0.4096 0.044 Uiso 1 1 calc R . . H19B H 0.4766 0.1399 0.4890 0.044 Uiso 1 1 calc R . . C20 C 0.3606(3) 0.3458(2) 0.46080(13) 0.0376(5) Uani 1 1 d . . . H20A H 0.4142 0.3832 0.5027 0.045 Uiso 1 1 calc R . . H20B H 0.2329 0.3432 0.4889 0.045 Uiso 1 1 calc R . . C21 C 0.3527(3) 0.4456(2) 0.38632(13) 0.0363(5) Uani 1 1 d . . . H21A H 0.4804 0.4490 0.3589 0.044 Uiso 1 1 calc R . . H21B H 0.3013 0.4069 0.3440 0.044 Uiso 1 1 calc R . . C22 C 0.2386(3) 0.5946(2) 0.40900(15) 0.0423(5) Uani 1 1 d . . . H22A H 0.1100 0.5918 0.4352 0.051 Uiso 1 1 calc R . . H22B H 0.2882 0.6330 0.4521 0.051 Uiso 1 1 calc R . . C23 C 0.2355(4) 0.6932(2) 0.33439(16) 0.0463(6) Uani 1 1 d . . . H23A H 0.1697 0.7901 0.3556 0.056 Uiso 1 1 calc R . . H23B H 0.3644 0.6940 0.3073 0.056 Uiso 1 1 calc R . . C25 C 0.2042(3) 0.0516(2) 0.04624(15) 0.0456(6) Uani 1 1 d D . . H25 H 0.2883 -0.0352 0.0550 0.055 Uiso 1 1 calc R . . C26 C 0.0137(3) 0.0919(2) 0.08372(14) 0.0414(5) Uani 1 1 d D . . H26 H -0.0529 0.0370 0.1220 0.050 Uiso 1 1 calc R . . C27 C -0.0604(3) 0.2278(3) 0.05445(14) 0.0430(5) Uani 1 1 d D . . H27 H -0.1858 0.2806 0.0697 0.052 Uiso 1 1 calc R . . C28 C 0.0841(4) 0.2721(3) -0.00152(14) 0.0473(6) Uani 1 1 d D . . H28 H 0.0729 0.3597 -0.0305 0.057 Uiso 1 1 calc R . . C29 C 0.2481(3) 0.1628(3) -0.00663(13) 0.0474(6) Uani 1 1 d D . . H29 H 0.3667 0.1639 -0.0397 0.057 Uiso 1 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 Co1 0.02553(16) 0.02960(16) 0.01938(15) -0.00095(10) -0.00691(10) -0.00733(11) N1 0.0340(9) 0.0300(9) 0.0269(8) 0.0026(7) -0.0111(7) -0.0067(7) C2 0.0405(12) 0.0339(11) 0.0361(11) 0.0043(9) -0.0123(9) 0.0024(9) C3 0.0410(12) 0.0318(11) 0.0381(12) -0.0044(9) -0.0089(9) 0.0029(9) C4 0.0249(10) 0.0408(11) 0.0260(10) 0.0011(8) -0.0045(8) -0.0023(8) C5 0.0246(9) 0.0311(10) 0.0178(8) -0.0003(7) -0.0044(7) -0.0084(8) C6 0.0235(9) 0.0304(10) 0.0215(9) -0.0003(7) -0.0052(7) -0.0077(8) C7 0.0324(11) 0.0402(11) 0.0269(10) 0.0073(8) -0.0035(8) -0.0122(9) C8 0.0465(13) 0.0518(14) 0.0424(12) 0.0110(10) -0.0052(10) -0.0313(11) C9 0.0696(16) 0.0289(11) 0.0531(14) 0.0104(10) -0.0203(12) -0.0174(11) N10 0.0363(9) 0.0249(8) 0.0444(10) -0.0005(7) -0.0134(8) -0.0062(7) C11 0.0422(13) 0.0319(12) 0.0677(16) -0.0088(11) -0.0164(12) 0.0048(10) C12 0.0269(10) 0.0400(12) 0.0461(13) -0.0095(10) -0.0036(9) 0.0023(9) C13 0.0250(10) 0.0374(11) 0.0344(11) 0.0008(8) -0.0083(8) -0.0035(8) C14 0.0234(9) 0.0292(10) 0.0216(9) -0.0019(7) -0.0054(7) -0.0076(8) C15 0.0229(9) 0.0295(10) 0.0200(9) -0.0008(7) -0.0060(7) -0.0078(7) C16 0.0291(10) 0.0397(11) 0.0271(10) 0.0042(8) -0.0069(8) -0.0149(9) C17 0.0336(11) 0.0421(12) 0.0226(10) 0.0046(8) -0.0014(8) -0.0134(9) C18 0.0456(12) 0.0316(11) 0.0273(10) 0.0077(8) -0.0107(9) -0.0148(9) C19 0.0408(12) 0.0426(12) 0.0308(11) 0.0068(9) -0.0168(9) -0.0122(10) C20 0.0396(12) 0.0471(13) 0.0301(11) -0.0047(9) -0.0110(9) -0.0140(10) C21 0.0421(12) 0.0349(11) 0.0327(11) -0.0028(9) -0.0063(9) -0.0121(9) C22 0.0444(12) 0.0405(12) 0.0437(12) -0.0132(10) -0.0159(10) -0.0061(10) C23 0.0599(15) 0.0264(11) 0.0575(15) -0.0060(10) -0.0198(12) -0.0126(10) C25 0.0536(14) 0.0419(13) 0.0431(13) -0.0163(10) -0.0181(11) -0.0059(11) C26 0.0502(13) 0.0478(13) 0.0359(12) -0.0044(10) -0.0144(10) -0.0245(11) C27 0.0373(12) 0.0577(15) 0.0403(12) -0.0058(10) -0.0211(10) -0.0117(11) C28 0.0691(16) 0.0561(15) 0.0277(11) 0.0076(10) -0.0260(11) -0.0233(13) C29 0.0487(14) 0.0725(17) 0.0229(10) -0.0153(10) 0.0001(9) -0.0225(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 Co1 C14 1.9707(18) . ? Co1 C6 1.9741(18) . ? Co1 C15 1.9747(17) . ? Co1 C5 1.9834(18) . ? Co1 C28 2.056(2) . ? Co1 C29 2.059(2) . ? Co1 C27 2.066(2) . ? Co1 C25 2.071(2) . ? Co1 C26 2.078(2) . ? N1 C19 1.464(3) . ? N1 C2 1.465(3) . ? N1 C18 1.469(3) . ? C2 C3 1.530(3) . ? C3 C4 1.518(3) . ? C4 C5 1.494(3) . ? C5 C6 1.458(3) . ? C5 C15 1.466(2) . ? C6 C14 1.460(3) . ? C6 C7 1.497(3) . ? C7 C8 1.532(3) . ? C8 C9 1.524(3) . ? C9 N10 1.453(3) . ? N10 C11 1.465(3) . ? N10 C23 1.469(3) . ? C11 C12 1.512(3) . ? C12 C13 1.543(3) . ? C13 C14 1.497(3) . ? C14 C15 1.462(3) . ? C15 C16 1.496(3) . ? C16 C17 1.538(3) . ? C17 C18 1.520(3) . ? C19 C20 1.507(3) . ? C20 C21 1.511(3) . ? C21 C22 1.510(3) . ? C22 C23 1.504(3) . ? C25 C26 1.410(3) . ? C25 C29 1.413(3) . ? C26 C27 1.407(3) . ? C27 C28 1.414(3) . ? C28 C29 1.414(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 C14 Co1 C6 43.44(7) . . ? C14 Co1 C15 43.50(7) . . ? C6 Co1 C15 63.19(7) . . ? C14 Co1 C5 62.97(8) . . ? C6 Co1 C5 43.25(7) . . ? C15 Co1 C5 43.48(7) . . ? C14 Co1 C28 121.19(9) . . ? C6 Co1 C28 114.87(9) . . ? C15 Co1 C28 161.46(9) . . ? C5 Co1 C28 148.21(9) . . ? C14 Co1 C29 152.44(9) . . ? C6 Co1 C29 117.38(9) . . ? C15 Co1 C29 158.30(9) . . ? C5 Co1 C29 120.23(9) . . ? C28 Co1 C29 40.19(10) . . ? C14 Co1 C27 112.60(8) . . ? C6 Co1 C27 139.04(9) . . ? C15 Co1 C27 128.12(8) . . ? C5 Co1 C27 171.48(8) . . ? C28 Co1 C27 40.12(9) . . ? C29 Co1 C27 67.29(9) . . ? C14 Co1 C25 167.37(9) . . ? C6 Co1 C25 144.81(9) . . ? C15 Co1 C25 126.01(9) . . ? C5 Co1 C25 115.66(9) . . ? C28 Co1 C25 67.24(10) . . ? C29 Co1 C25 40.02(10) . . ? C27 Co1 C25 66.90(9) . . ? C14 Co1 C26 131.78(8) . . ? C6 Co1 C26 175.22(8) . . ? C15 Co1 C26 113.45(8) . . ? C5 Co1 C26 137.02(8) . . ? C28 Co1 C26 67.09(9) . . ? C29 Co1 C26 67.07(9) . . ? C27 Co1 C26 39.70(9) . . ? C25 Co1 C26 39.75(9) . . ? C19 N1 C2 113.11(17) . . ? C19 N1 C18 112.92(16) . . ? C2 N1 C18 113.66(17) . . ? N1 C2 C3 113.04(16) . . ? C4 C3 C2 112.57(18) . . ? C5 C4 C3 114.88(17) . . ? C6 C5 C15 90.05(14) . . ? C6 C5 C4 132.57(16) . . ? C15 C5 C4 136.91(17) . . ? C6 C5 Co1 68.04(10) . . ? C15 C5 Co1 67.94(10) . . ? C4 C5 Co1 127.14(13) . . ? C5 C6 C14 90.08(14) . . ? C5 C6 C7 132.97(17) . . ? C14 C6 C7 136.81(17) . . ? C5 C6 Co1 68.71(10) . . ? C14 C6 Co1 68.15(10) . . ? C7 C6 Co1 124.12(13) . . ? C6 C7 C8 115.87(16) . . ? C9 C8 C7 113.11(19) . . ? N10 C9 C8 112.37(18) . . ? C9 N10 C11 115.44(19) . . ? C9 N10 C23 111.28(19) . . ? C11 N10 C23 111.63(18) . . ? N10 C11 C12 114.20(17) . . ? C11 C12 C13 116.04(19) . . ? C14 C13 C12 114.33(16) . . ? C6 C14 C15 90.16(14) . . ? C6 C14 C13 137.63(17) . . ? C15 C14 C13 131.77(16) . . ? C6 C14 Co1 68.40(10) . . ? C15 C14 Co1 68.39(10) . . ? C13 C14 Co1 126.43(13) . . ? C14 C15 C5 89.71(14) . . ? C14 C15 C16 131.61(16) . . ? C5 C15 C16 138.47(17) . . ? C14 C15 Co1 68.11(10) . . ? C5 C15 Co1 68.57(10) . . ? C16 C15 Co1 124.77(13) . . ? C15 C16 C17 115.63(16) . . ? C18 C17 C16 114.92(17) . . ? N1 C18 C17 115.58(16) . . ? N1 C19 C20 113.09(17) . . ? C19 C20 C21 113.94(17) . . ? C22 C21 C20 114.77(18) . . ? C23 C22 C21 114.02(19) . . ? N10 C23 C22 114.13(18) . . ? C26 C25 C29 108.1(2) . . ? C26 C25 Co1 70.41(12) . . ? C29 C25 Co1 69.55(12) . . ? C27 C26 C25 108.1(2) . . ? C27 C26 Co1 69.69(12) . . ? C25 C26 Co1 69.84(12) . . ? C26 C27 C28 108.2(2) . . ? C26 C27 Co1 70.62(12) . . ? C28 C27 Co1 69.54(12) . . ? C29 C28 C27 107.9(2) . . ? C29 C28 Co1 70.04(12) . . ? C27 C28 Co1 70.34(12) . . ? C25 C29 C28 107.8(2) . . ? C25 C29 Co1 70.43(12) . . ? C28 C29 Co1 69.76(12) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.436 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.054 #======================================================================= data_3d _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H45 Co N2' _chemical_formula_weight 480.60 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' '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 P2(1)/c 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 8.54240(10) _cell_length_b 29.0936(3) _cell_length_c 10.94860(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.09 _cell_angle_gamma 90.00 _cell_volume 2555.55(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max .44 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18908 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.60 _reflns_number_total 4439 _reflns_number_gt 3964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+1.2880P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4439 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.006 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 Co1 Co 0.18482(3) 0.319448(8) 0.82206(2) 0.02580(10) Uani 1 1 d . . . N1 N 0.5830(2) 0.33075(6) 1.20550(14) 0.0300(4) Uani 1 1 d . . . C2 C 0.4717(3) 0.35400(8) 1.26097(19) 0.0368(5) Uani 1 1 d . . . H2A H 0.5284 0.3819 1.3069 0.044 Uiso 1 1 calc R . . H2B H 0.4524 0.3335 1.3265 0.044 Uiso 1 1 calc R . . C3 C 0.3035(2) 0.36792(8) 1.16333(18) 0.0367(5) Uani 1 1 d . . . H3A H 0.2435 0.3860 1.2099 0.044 Uiso 1 1 calc R . . H3B H 0.2381 0.3396 1.1310 0.044 Uiso 1 1 calc R . . C4 C 0.3061(2) 0.39593(7) 1.04541(18) 0.0301(4) Uani 1 1 d . . . H4A H 0.2050 0.4154 1.0179 0.036 Uiso 1 1 calc R . . H4B H 0.4031 0.4169 1.0758 0.036 Uiso 1 1 calc R . . C5 C 0.3140(2) 0.37185(6) 0.92619(17) 0.0245(4) Uani 1 1 d . . . C6 C 0.2278(2) 0.38429(6) 0.79033(18) 0.0278(4) Uani 1 1 d . . . C7 C 0.0950(2) 0.41847(7) 0.7245(2) 0.0375(5) Uani 1 1 d . . . H7A H 0.0230 0.4225 0.7778 0.045 Uiso 1 1 calc R . . H7B H 0.0249 0.4056 0.6395 0.045 Uiso 1 1 calc R . . C8 C 0.1576(3) 0.46567(7) 0.7013(2) 0.0446(5) Uani 1 1 d . . . H8A H 0.0616 0.4870 0.6713 0.053 Uiso 1 1 calc R . . H8B H 0.2350 0.4775 0.7850 0.053 Uiso 1 1 calc R . . C9 C 0.2466(3) 0.46587(8) 0.6022(2) 0.0494(6) Uani 1 1 d . . . H9A H 0.1862 0.4454 0.5289 0.059 Uiso 1 1 calc R . . H9B H 0.2436 0.4974 0.5672 0.059 Uiso 1 1 calc R . . N10 N 0.4200(2) 0.45073(6) 0.65749(17) 0.0411(4) Uani 1 1 d . . . C11 C 0.4781(3) 0.42181(8) 0.5714(2) 0.0453(5) Uani 1 1 d . . . H11A H 0.5784 0.4361 0.5617 0.054 Uiso 1 1 calc R . . H11B H 0.3905 0.4208 0.4843 0.054 Uiso 1 1 calc R . . C12 C 0.5201(3) 0.37282(8) 0.62095(19) 0.0384(5) Uani 1 1 d . . . H12A H 0.6065 0.3741 0.7086 0.046 Uiso 1 1 calc R . . H12B H 0.5689 0.3566 0.5630 0.046 Uiso 1 1 calc R . . C13 C 0.3726(3) 0.34440(7) 0.62929(18) 0.0330(4) Uani 1 1 d . . . H13A H 0.2727 0.3515 0.5529 0.040 Uiso 1 1 calc R . . H13B H 0.3980 0.3113 0.6256 0.040 Uiso 1 1 calc R . . C14 C 0.3342(2) 0.35341(6) 0.75019(17) 0.0263(4) Uani 1 1 d . . . C15 C 0.4212(2) 0.34020(6) 0.88510(16) 0.0230(4) Uani 1 1 d . . . C16 C 0.5797(2) 0.31352(6) 0.94294(17) 0.0259(4) Uani 1 1 d . . . H16A H 0.6685 0.3354 0.9907 0.031 Uiso 1 1 calc R . . H16B H 0.6109 0.3008 0.8706 0.031 Uiso 1 1 calc R . . C17 C 0.5795(2) 0.27399(7) 1.03514(18) 0.0332(4) Uani 1 1 d . . . H17A H 0.5118 0.2484 0.9841 0.040 Uiso 1 1 calc R . . H17B H 0.6950 0.2627 1.0767 0.040 Uiso 1 1 calc R . . C18 C 0.5104(3) 0.28792(7) 1.14043(18) 0.0337(4) Uani 1 1 d . . . H18A H 0.3880 0.2916 1.1011 0.040 Uiso 1 1 calc R . . H18B H 0.5326 0.2630 1.2059 0.040 Uiso 1 1 calc R . . C19 C 0.7468(3) 0.32187(8) 1.3053(2) 0.0409(5) Uani 1 1 d . . . H19A H 0.8068 0.2993 1.2701 0.049 Uiso 1 1 calc R . . H19B H 0.7287 0.3075 1.3814 0.049 Uiso 1 1 calc R . . C20 C 0.8581(3) 0.36383(8) 1.3519(2) 0.0450(5) Uani 1 1 d . . . H20A H 0.7974 0.3868 1.3852 0.054 Uiso 1 1 calc R . . H20B H 0.9584 0.3545 1.4254 0.054 Uiso 1 1 calc R . . C21 C 0.9139(3) 0.38646(8) 1.2482(2) 0.0459(6) Uani 1 1 d . . . H21A H 1.0125 0.4059 1.2916 0.055 Uiso 1 1 calc R . . H21B H 0.9486 0.3622 1.1995 0.055 Uiso 1 1 calc R . . C22 C 0.7811(3) 0.41591(7) 1.1522(2) 0.0379(5) Uani 1 1 d . . . H22A H 0.6784 0.3973 1.1170 0.046 Uiso 1 1 calc R . . H22B H 0.7554 0.4419 1.2005 0.046 Uiso 1 1 calc R . . C23 C 0.8227(3) 0.43531(9) 1.0386(2) 0.0486(6) Uani 1 1 d . . . H23A H 0.8678 0.4105 0.9984 0.058 Uiso 1 1 calc R . . H23B H 0.9099 0.4592 1.0706 0.058 Uiso 1 1 calc R . . C24 C 0.6692(3) 0.45637(8) 0.9356(2) 0.0474(6) Uani 1 1 d . . . H24A H 0.5812 0.4326 0.9080 0.057 Uiso 1 1 calc R . . H24B H 0.6270 0.4815 0.9769 0.057 Uiso 1 1 calc R . . C25 C 0.6954(3) 0.47532(9) 0.8157(2) 0.0515(6) Uani 1 1 d . . . H25A H 0.7501 0.4517 0.7792 0.062 Uiso 1 1 calc R . . H25B H 0.7706 0.5023 0.8403 0.062 Uiso 1 1 calc R . . C26 C 0.5328(3) 0.48957(8) 0.7128(3) 0.0535(6) Uani 1 1 d . . . H26A H 0.4752 0.5117 0.7514 0.064 Uiso 1 1 calc R . . H26B H 0.5578 0.5055 0.6417 0.064 Uiso 1 1 calc R . . C27 C 0.1265(3) 0.25228(7) 0.7651(2) 0.0468(6) Uani 1 1 d . . . H27 H 0.1971 0.2317 0.7408 0.056 Uiso 1 1 calc R . . C28 C 0.1224(3) 0.25796(8) 0.8903(2) 0.0470(6) Uani 1 1 d . . . H28 H 0.1895 0.2419 0.9656 0.056 Uiso 1 1 calc R . . C29 C 0.0036(3) 0.29116(9) 0.8865(2) 0.0503(6) Uani 1 1 d . . . H29 H -0.0245 0.3018 0.9584 0.060 Uiso 1 1 calc R . . C30 C -0.0674(3) 0.30611(8) 0.7566(3) 0.0546(7) Uani 1 1 d . . . H30 H -0.1524 0.3286 0.7253 0.066 Uiso 1 1 calc R . . C31 C 0.0096(3) 0.28186(8) 0.6814(2) 0.0482(6) Uani 1 1 d . . . H31 H -0.0137 0.2850 0.5905 0.058 Uiso 1 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 Co1 0.02192(15) 0.02573(16) 0.02635(15) -0.00190(10) 0.00392(10) 0.00007(10) N1 0.0291(8) 0.0347(9) 0.0221(8) 0.0000(6) 0.0035(6) -0.0009(7) C2 0.0392(11) 0.0467(12) 0.0252(10) -0.0036(9) 0.0120(9) -0.0040(10) C3 0.0320(10) 0.0495(13) 0.0321(10) -0.0080(9) 0.0153(9) -0.0020(9) C4 0.0257(9) 0.0326(10) 0.0313(10) -0.0071(8) 0.0091(8) 0.0030(8) C5 0.0216(9) 0.0239(9) 0.0273(9) -0.0006(7) 0.0075(7) 0.0008(7) C6 0.0258(9) 0.0255(10) 0.0290(10) -0.0010(7) 0.0054(8) 0.0015(8) C7 0.0318(11) 0.0354(11) 0.0387(11) 0.0016(9) 0.0037(9) 0.0091(9) C8 0.0430(12) 0.0327(12) 0.0489(13) 0.0052(10) 0.0041(10) 0.0131(10) C9 0.0543(14) 0.0445(13) 0.0414(13) 0.0148(10) 0.0063(11) 0.0070(11) N10 0.0470(11) 0.0375(10) 0.0367(10) 0.0036(8) 0.0116(8) 0.0006(8) C11 0.0592(14) 0.0475(13) 0.0318(11) 0.0063(9) 0.0187(10) -0.0017(11) C12 0.0461(12) 0.0475(13) 0.0247(10) 0.0011(9) 0.0163(9) 0.0080(10) C13 0.0431(11) 0.0302(10) 0.0225(9) -0.0001(8) 0.0071(8) 0.0067(9) C14 0.0277(9) 0.0238(9) 0.0249(9) -0.0001(7) 0.0059(7) 0.0015(7) C15 0.0234(9) 0.0216(9) 0.0238(9) -0.0015(7) 0.0076(7) -0.0011(7) C16 0.0227(9) 0.0281(10) 0.0251(9) -0.0034(7) 0.0058(7) 0.0034(7) C17 0.0340(10) 0.0289(10) 0.0303(10) 0.0013(8) 0.0029(8) 0.0068(8) C18 0.0378(11) 0.0328(11) 0.0260(10) 0.0044(8) 0.0053(8) -0.0031(9) C19 0.0369(12) 0.0483(13) 0.0274(11) 0.0043(9) -0.0020(9) 0.0032(10) C20 0.0321(11) 0.0585(15) 0.0323(11) -0.0053(10) -0.0046(9) -0.0005(10) C21 0.0271(11) 0.0567(15) 0.0483(13) -0.0099(11) 0.0059(9) -0.0049(10) C22 0.0328(11) 0.0365(12) 0.0451(12) -0.0080(9) 0.0142(9) -0.0059(9) C23 0.0411(12) 0.0524(14) 0.0563(15) -0.0050(11) 0.0219(11) -0.0072(11) C24 0.0424(13) 0.0492(14) 0.0523(14) -0.0008(11) 0.0185(11) -0.0020(11) C25 0.0509(14) 0.0503(15) 0.0555(15) -0.0037(11) 0.0214(12) -0.0120(11) C26 0.0620(16) 0.0413(13) 0.0583(15) 0.0021(11) 0.0219(13) -0.0046(12) C27 0.0408(12) 0.0303(11) 0.0706(16) -0.0166(11) 0.0209(12) -0.0098(10) C28 0.0377(12) 0.0413(13) 0.0502(14) 0.0097(10) 0.0001(10) -0.0147(10) C29 0.0449(13) 0.0592(16) 0.0527(14) -0.0188(12) 0.0241(11) -0.0239(12) C30 0.0213(10) 0.0411(13) 0.089(2) 0.0018(13) 0.0033(11) -0.0021(10) C31 0.0443(13) 0.0559(15) 0.0347(12) -0.0077(10) 0.0011(10) -0.0190(11) _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 Co1 C6 1.9754(19) . ? Co1 C14 1.9784(19) . ? Co1 C15 1.9903(17) . ? Co1 C5 1.9944(18) . ? Co1 C31 2.055(2) . ? Co1 C27 2.060(2) . ? Co1 C30 2.061(2) . ? Co1 C28 2.077(2) . ? Co1 C29 2.079(2) . ? N1 C2 1.458(3) . ? N1 C18 1.463(2) . ? N1 C19 1.472(2) . ? C2 C3 1.522(3) . ? C3 C4 1.533(3) . ? C4 C5 1.503(2) . ? C5 C6 1.461(3) . ? C5 C15 1.474(2) . ? C6 C14 1.449(3) . ? C6 C7 1.495(3) . ? C7 C8 1.526(3) . ? C8 C9 1.524(3) . ? C9 N10 1.463(3) . ? N10 C11 1.471(3) . ? N10 C26 1.473(3) . ? C11 C12 1.523(3) . ? C12 C13 1.536(3) . ? C13 C14 1.492(3) . ? C14 C15 1.459(2) . ? C15 C16 1.499(2) . ? C16 C17 1.531(3) . ? C17 C18 1.520(3) . ? C19 C20 1.524(3) . ? C20 C21 1.523(3) . ? C21 C22 1.519(3) . ? C22 C23 1.515(3) . ? C23 C24 1.533(3) . ? C24 C25 1.510(3) . ? C25 C26 1.515(3) . ? C27 C28 1.392(3) . ? C27 C31 1.396(3) . ? C28 C29 1.392(3) . ? C29 C30 1.410(4) . ? C30 C31 1.407(4) . ? 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 C6 Co1 C14 43.01(8) . . ? C6 Co1 C15 62.84(7) . . ? C14 Co1 C15 43.13(7) . . ? C6 Co1 C5 43.17(7) . . ? C14 Co1 C5 62.59(7) . . ? C15 Co1 C5 43.41(7) . . ? C6 Co1 C31 120.53(9) . . ? C14 Co1 C31 111.79(9) . . ? C15 Co1 C31 144.33(9) . . ? C5 Co1 C31 162.29(9) . . ? C6 Co1 C27 153.27(9) . . ? C14 Co1 C27 118.39(9) . . ? C15 Co1 C27 120.26(8) . . ? C5 Co1 C27 157.99(9) . . ? C31 Co1 C27 39.67(10) . . ? C6 Co1 C30 110.73(9) . . ? C14 Co1 C30 134.10(9) . . ? C15 Co1 C30 173.18(8) . . ? C5 Co1 C30 130.54(9) . . ? C31 Co1 C30 39.97(10) . . ? C27 Co1 C30 66.47(10) . . ? C6 Co1 C28 166.35(9) . . ? C14 Co1 C28 148.58(9) . . ? C15 Co1 C28 119.45(8) . . ? C5 Co1 C28 127.78(8) . . ? C31 Co1 C28 66.44(9) . . ? C27 Co1 C28 39.33(10) . . ? C30 Co1 C28 66.18(10) . . ? C6 Co1 C29 130.00(9) . . ? C14 Co1 C29 171.88(9) . . ? C15 Co1 C29 141.95(9) . . ? C5 Co1 C29 116.03(8) . . ? C31 Co1 C29 66.92(10) . . ? C27 Co1 C29 66.19(10) . . ? C30 Co1 C29 39.83(10) . . ? C28 Co1 C29 39.12(10) . . ? C2 N1 C18 111.69(16) . . ? C2 N1 C19 111.19(16) . . ? C18 N1 C19 110.35(16) . . ? N1 C2 C3 115.09(15) . . ? C2 C3 C4 116.72(16) . . ? C5 C4 C3 120.10(16) . . ? C6 C5 C15 89.58(14) . . ? C6 C5 C4 127.71(16) . . ? C15 C5 C4 140.72(16) . . ? C6 C5 Co1 67.72(10) . . ? C15 C5 Co1 68.14(10) . . ? C4 C5 Co1 132.20(13) . . ? C14 C6 C5 90.34(14) . . ? C14 C6 C7 135.82(17) . . ? C5 C6 C7 133.62(17) . . ? C14 C6 Co1 68.60(10) . . ? C5 C6 Co1 69.11(10) . . ? C7 C6 Co1 124.34(14) . . ? C6 C7 C8 115.31(17) . . ? C9 C8 C7 114.25(19) . . ? N10 C9 C8 112.70(17) . . ? C9 N10 C11 115.05(18) . . ? C9 N10 C26 111.45(18) . . ? C11 N10 C26 112.64(19) . . ? N10 C11 C12 113.38(17) . . ? C11 C12 C13 115.30(18) . . ? C14 C13 C12 113.12(16) . . ? C6 C14 C15 90.62(14) . . ? C6 C14 C13 136.86(17) . . ? C15 C14 C13 131.39(16) . . ? C6 C14 Co1 68.39(10) . . ? C15 C14 Co1 68.87(10) . . ? C13 C14 Co1 129.29(13) . . ? C14 C15 C5 89.46(14) . . ? C14 C15 C16 129.51(16) . . ? C5 C15 C16 139.49(16) . . ? C14 C15 Co1 68.00(10) . . ? C5 C15 Co1 68.44(10) . . ? C16 C15 Co1 130.61(13) . . ? C15 C16 C17 117.51(16) . . ? C18 C17 C16 112.88(16) . . ? N1 C18 C17 112.70(16) . . ? N1 C19 C20 115.63(18) . . ? C21 C20 C19 114.55(18) . . ? C22 C21 C20 114.17(18) . . ? C23 C22 C21 116.64(19) . . ? C22 C23 C24 111.71(19) . . ? C25 C24 C23 116.1(2) . . ? C24 C25 C26 112.0(2) . . ? N10 C26 C25 113.5(2) . . ? C28 C27 C31 108.6(2) . . ? C28 C27 Co1 71.02(13) . . ? C31 C27 Co1 70.00(13) . . ? C29 C28 C27 108.5(2) . . ? C29 C28 Co1 70.50(13) . . ? C27 C28 Co1 69.64(13) . . ? C28 C29 C30 107.5(2) . . ? C28 C29 Co1 70.38(13) . . ? C30 C29 Co1 69.39(13) . . ? C31 C30 C29 108.1(2) . . ? C31 C30 Co1 69.81(13) . . ? C29 C30 Co1 70.79(13) . . ? C27 C31 C30 107.3(2) . . ? C27 C31 Co1 70.33(12) . . ? C30 C31 Co1 70.22(13) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.60 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.419 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.049 #====================================================================== data_4d _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H90 Co2 N4' _chemical_formula_weight 961.20 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' '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 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 23.9708(16) _cell_length_b 9.4887(7) _cell_length_c 23.9264(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.2140(10) _cell_angle_gamma 90.00 _cell_volume 5386.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lamina _exptl_crystal_colour yellow _exptl_crystal_size_max .38 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19435 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.59 _reflns_number_total 4623 _reflns_number_gt 2413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+12.7767P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4623 _refine_ls_number_parameters 308 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.2032 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.208 _refine_ls_shift/su_mean 0.015 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 Co1 Co 0.07327(3) 0.95940(9) -0.10556(3) 0.0694(3) Uani 1 1 d . . . C1 C 0.0414(3) 1.1560(8) -0.1249(5) 0.105(2) Uani 1 1 d . . . H1 H 0.0626 1.2385 -0.1233 0.126 Uiso 1 1 calc R . . C2 C 0.0157(4) 1.0986(11) -0.0805(3) 0.108(3) Uani 1 1 d . . . H2 H 0.0168 1.1352 -0.0443 0.130 Uiso 1 1 calc R . . C3 C -0.0114(3) 0.9768(10) -0.1017(4) 0.108(3) Uani 1 1 d . . . H3 H -0.0320 0.9170 -0.0816 0.130 Uiso 1 1 calc R . . C4 C -0.0032(3) 0.9575(9) -0.1569(4) 0.102(2) Uani 1 1 d . . . H4 H -0.0172 0.8836 -0.1803 0.122 Uiso 1 1 calc R . . C5 C 0.0297(3) 1.0683(10) -0.1713(3) 0.096(2) Uani 1 1 d . . . H5 H 0.0417 1.0814 -0.2062 0.116 Uiso 1 1 calc R . . C6 C 0.1563(2) 0.9529(7) -0.0939(2) 0.0730(17) Uani 1 1 d . A . C7 C 0.1315(2) 0.8310(7) -0.1244(2) 0.0755(17) Uani 1 1 d . . . C8 C 0.1337(2) 0.7707(7) -0.1825(2) 0.0888(19) Uani 1 1 d . . . H8A H 0.1154 0.8360 -0.2105 0.107 Uiso 1 1 calc R . . H8B H 0.1125 0.6833 -0.1862 0.107 Uiso 1 1 calc R . . C9 C 0.1934(2) 0.7418(7) -0.1950(2) 0.0808(18) Uani 1 1 d . . . H9A H 0.1913 0.7109 -0.2339 0.097 Uiso 1 1 calc R . . H9B H 0.2146 0.8293 -0.1913 0.097 Uiso 1 1 calc R . . C10 C 0.2251(2) 0.6322(7) -0.1571(2) 0.0745(16) Uani 1 1 d . . . H10A H 0.2190 0.6498 -0.1185 0.089 Uiso 1 1 calc R . . H10B H 0.2098 0.5399 -0.1678 0.089 Uiso 1 1 calc R . . N11 N 0.28522(18) 0.6305(5) -0.15922(17) 0.0677(13) Uani 1 1 d . A . C12 C 0.3160(2) 0.5455(7) -0.1146(2) 0.0792(17) Uani 1 1 d . . . H12A H 0.3535 0.5276 -0.1236 0.095 Uiso 1 1 calc R . . H12B H 0.2971 0.4554 -0.1132 0.095 Uiso 1 1 calc R . . C13 C 0.3209(2) 0.6151(7) -0.0565(2) 0.0776(17) Uani 1 1 d . . . H13A H 0.3322 0.7127 -0.0593 0.093 Uiso 1 1 calc R . . H13B H 0.2845 0.6137 -0.0433 0.093 Uiso 1 1 calc R . . C14 C 0.1368(3) 0.9602(8) 0.0150(2) 0.092(2) Uani 1 1 d . . . H14A H 0.1465 1.0595 0.0153 0.111 Uiso 1 1 calc R . . H14B H 0.1000 0.9519 0.0271 0.111 Uiso 1 1 calc R . . C15 C 0.1331(2) 0.9060(8) -0.0444(2) 0.0793(19) Uani 1 1 d . . . C16 C 0.1090(2) 0.7847(8) -0.0748(3) 0.0810(18) Uani 1 1 d . . . C17 C 0.0792(4) 0.6573(10) -0.0589(4) 0.148(4) Uani 1 1 d . . . H17A H 0.0644 0.6815 -0.0244 0.177 Uiso 1 1 calc R . . H17B H 0.0467 0.6461 -0.0878 0.177 Uiso 1 1 calc R . . C19 C 0.3567(5) 1.0186(14) 0.0187(5) 0.235(8) Uani 1 1 d . A . H19A H 0.3523 1.1135 0.0324 0.282 Uiso 1 1 calc R . . H19B H 0.3238 0.9660 0.0260 0.282 Uiso 1 1 calc R . . C18 C 0.3996(9) 0.9643(17) 0.0507(9) 0.382(17) Uani 1 1 d . . . H18A H 0.4310 1.0206 0.0420 0.458 Uiso 1 1 calc R . . H18B H 0.3937 0.9936 0.0883 0.458 Uiso 1 1 calc R . . N20 N 0.3529(3) 1.0297(9) -0.0469(3) 0.123(2) Uani 1 1 d DU . . C21 C 0.2983(4) 1.0949(12) -0.0729(6) 0.112(5) Uani 0.646(13) 1 d PDU A 1 H21A H 0.2881 1.1706 -0.0491 0.134 Uiso 0.646(13) 1 calc PR A 1 H21B H 0.3024 1.1341 -0.1096 0.134 Uiso 0.646(13) 1 calc PR A 1 C22 C 0.2560(4) 0.9908(13) -0.0789(7) 0.111(5) Uani 0.646(13) 1 d PDU A 1 H22A H 0.2530 0.9484 -0.0426 0.133 Uiso 0.646(13) 1 calc PR A 1 H22B H 0.2652 0.9173 -0.1043 0.133 Uiso 0.646(13) 1 calc PR A 1 C23 C 0.1964(2) 1.0654(8) -0.1044(3) 0.105(2) Uani 1 1 d DU . . H23A H 0.1900 1.1513 -0.0843 0.126 Uiso 0.646(13) 1 calc PR A 1 H23B H 0.1944 1.0857 -0.1444 0.126 Uiso 0.646(13) 1 calc PR A 1 H23C H 0.1742 1.1513 -0.1083 0.126 Uiso 0.354(13) 1 calc PR A 2 H23D H 0.2060 1.0456 -0.1416 0.126 Uiso 0.354(13) 1 calc PR A 2 C24 C 0.3923(6) 1.1253(12) -0.0715(6) 0.179(6) Uani 1 1 d . A . H24A H 0.3771 1.2202 -0.0731 0.214 Uiso 1 1 calc R . . H24B H 0.4281 1.1270 -0.0467 0.214 Uiso 1 1 calc R . . C25 C 0.4024(5) 1.0823(12) -0.1294(7) 0.187(5) Uani 1 1 d . . . H25A H 0.3669 1.0890 -0.1545 0.224 Uiso 1 1 calc R A . H25B H 0.4281 1.1495 -0.1425 0.224 Uiso 1 1 calc R . . C26 C 0.4250(4) 0.9424(13) -0.1345(6) 0.180(5) Uani 1 1 d . A . H26A H 0.3979 0.8744 -0.1244 0.215 Uiso 1 1 calc R . . H26B H 0.4590 0.9329 -0.1074 0.215 Uiso 1 1 calc R . . C27 C 0.4394(5) 0.9048(15) -0.1950(6) 0.203(6) Uani 1 1 d . . . H27A H 0.4677 0.9713 -0.2036 0.244 Uiso 1 1 calc R A . H27B H 0.4569 0.8124 -0.1925 0.244 Uiso 1 1 calc R . . C28 C 0.3967(5) 0.9027(13) -0.2414(5) 0.182(5) Uani 1 1 d . A . H28A H 0.4129 0.8704 -0.2740 0.219 Uiso 1 1 calc R . . H28B H 0.3840 0.9988 -0.2490 0.219 Uiso 1 1 calc R . . C29 C 0.3447(4) 0.8116(12) -0.2365(4) 0.155(4) Uani 1 1 d . . . H29A H 0.3266 0.8495 -0.2060 0.186 Uiso 1 1 calc R A . H29B H 0.3185 0.8231 -0.2710 0.186 Uiso 1 1 calc R . . C30 C 0.3531(3) 0.6587(11) -0.2264(3) 0.123(3) Uani 1 1 d . A . H30A H 0.3825 0.6449 -0.1945 0.147 Uiso 1 1 calc R . . H30B H 0.3656 0.6161 -0.2592 0.147 Uiso 1 1 calc R . . C31 C 0.2999(3) 0.5850(8) -0.2145(2) 0.092(2) Uani 1 1 d . . . H31A H 0.2691 0.6073 -0.2441 0.110 Uiso 1 1 calc R A . H31B H 0.3056 0.4838 -0.2143 0.110 Uiso 1 1 calc R . . C21B C 0.2901(6) 0.9902(18) -0.0688(9) 0.080(6) Uani 0.354(13) 1 d PDU A 2 H21C H 0.2875 0.9552 -0.1071 0.096 Uiso 0.354(13) 1 calc PR A 2 H21D H 0.2784 0.9152 -0.0455 0.096 Uiso 0.354(13) 1 calc PR A 2 C22B C 0.2532(6) 1.1069(19) -0.0676(9) 0.094(7) Uani 0.354(13) 1 d PDU A 2 H22C H 0.2690 1.1901 -0.0830 0.112 Uiso 0.354(13) 1 calc PR A 2 H22D H 0.2472 1.1270 -0.0292 0.112 Uiso 0.354(13) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0496(4) 0.0913(6) 0.0673(5) 0.0037(5) 0.0083(3) 0.0166(4) C1 0.080(5) 0.094(6) 0.135(7) 0.012(6) -0.008(5) 0.023(4) C2 0.098(6) 0.136(7) 0.089(6) -0.002(6) 0.011(5) 0.061(5) C3 0.056(4) 0.131(7) 0.144(8) 0.026(6) 0.035(4) 0.024(5) C4 0.053(4) 0.144(7) 0.105(6) -0.010(5) -0.003(4) 0.019(5) C5 0.059(4) 0.140(7) 0.088(5) 0.030(5) 0.007(4) 0.022(4) C6 0.045(3) 0.109(5) 0.062(4) -0.010(4) -0.001(3) 0.023(3) C7 0.061(3) 0.105(5) 0.059(4) -0.008(4) 0.002(3) 0.028(3) C8 0.073(4) 0.114(5) 0.075(4) -0.016(4) -0.004(3) 0.024(4) C9 0.082(4) 0.107(5) 0.052(3) -0.010(3) 0.004(3) 0.029(4) C10 0.081(4) 0.086(4) 0.056(3) -0.016(3) 0.007(3) 0.012(3) N11 0.068(3) 0.087(3) 0.047(3) -0.009(2) 0.006(2) 0.020(3) C12 0.082(4) 0.093(5) 0.063(4) -0.003(4) 0.013(3) 0.032(4) C13 0.082(4) 0.096(5) 0.056(3) 0.007(3) 0.017(3) 0.034(4) C14 0.089(4) 0.126(6) 0.062(4) 0.000(4) 0.013(3) 0.049(4) C15 0.064(3) 0.115(6) 0.058(4) -0.006(4) 0.005(3) 0.036(4) C16 0.077(4) 0.093(5) 0.073(4) 0.012(4) 0.010(3) 0.025(4) C17 0.176(9) 0.103(7) 0.169(9) 0.042(6) 0.041(7) 0.044(7) C19 0.175(10) 0.314(17) 0.181(11) -0.143(11) -0.088(9) 0.152(11) C18 0.41(3) 0.184(15) 0.47(3) 0.144(18) -0.23(3) -0.069(17) N20 0.081(4) 0.133(6) 0.146(6) -0.045(5) -0.018(4) 0.038(4) C21 0.064(6) 0.063(8) 0.206(14) 0.021(9) 0.009(7) 0.015(5) C22 0.067(6) 0.124(12) 0.139(12) -0.045(9) 0.008(7) -0.013(6) C23 0.057(3) 0.158(7) 0.101(5) -0.036(5) 0.016(3) -0.006(4) C24 0.168(11) 0.117(9) 0.228(14) -0.053(10) -0.050(10) 0.030(8) C25 0.155(10) 0.101(9) 0.303(19) 0.044(10) 0.031(11) -0.013(7) C26 0.137(8) 0.173(12) 0.238(14) 0.056(10) 0.055(9) 0.041(7) C27 0.117(8) 0.289(16) 0.222(14) 0.116(13) 0.084(9) 0.062(9) C28 0.153(10) 0.217(12) 0.199(12) 0.103(10) 0.096(9) 0.061(9) C29 0.155(9) 0.185(11) 0.136(8) 0.056(7) 0.061(7) 0.057(8) C30 0.122(7) 0.177(9) 0.076(5) 0.012(5) 0.040(4) 0.049(6) C31 0.104(5) 0.119(6) 0.054(4) -0.017(4) 0.014(3) 0.037(4) C21B 0.100(10) 0.060(14) 0.071(12) 0.033(10) -0.015(12) 0.011(9) C22B 0.067(9) 0.072(13) 0.140(18) -0.028(13) 0.009(10) -0.006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C7 1.953(5) . ? Co1 C15 1.963(5) . ? Co1 C16 1.961(6) . ? Co1 C6 1.972(5) . ? Co1 C5 2.041(6) . ? Co1 C1 2.044(7) . ? Co1 C3 2.051(6) . ? Co1 C4 2.056(6) . ? Co1 C2 2.060(7) . ? C1 C5 1.384(10) . ? C1 C2 1.411(10) . ? C2 C3 1.386(10) . ? C3 C4 1.374(10) . ? C4 C5 1.386(9) . ? C6 C15 1.448(8) . ? C6 C7 1.449(8) . ? C6 C23 1.480(9) . ? C7 C16 1.441(8) . ? C7 C8 1.512(8) . ? C7 C15 2.036(8) . ? C8 C9 1.528(7) . ? C9 C10 1.513(7) . ? C10 N11 1.449(6) . ? N11 C12 1.452(6) . ? N11 C31 1.480(7) . ? C12 C13 1.529(7) . ? C13 C14 1.495(7) 7_565 ? C14 C13 1.495(7) 7_565 ? C14 C15 1.503(8) . ? C15 C16 1.437(9) . ? C16 C17 1.481(11) . ? C17 C18 1.266(16) 7_565 ? C19 C18 1.297(15) . ? C19 N20 1.562(14) . ? C18 C17 1.266(16) 7_565 ? N20 C24 1.490(14) . ? N20 C21 1.500(10) . ? N20 C21B 1.567(15) . ? C21 C22 1.410(12) . ? C22 C23 1.633(11) . ? C23 C22B 1.564(14) . ? C24 C25 1.497(15) . ? C25 C26 1.445(13) . ? C26 C27 1.578(15) . ? C27 C28 1.399(14) . ? C28 C29 1.534(13) . ? C29 C30 1.480(11) . ? C30 C31 1.517(9) . ? C21B C22B 1.421(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Co1 C15 62.6(2) . . ? C7 Co1 C16 43.2(2) . . ? C15 Co1 C16 43.0(2) . . ? C7 Co1 C6 43.3(2) . . ? C15 Co1 C6 43.2(2) . . ? C16 Co1 C6 62.8(3) . . ? C7 Co1 C5 116.2(3) . . ? C15 Co1 C5 160.8(3) . . ? C16 Co1 C5 150.0(4) . . ? C6 Co1 C5 121.4(3) . . ? C7 Co1 C1 140.6(3) . . ? C15 Co1 C1 127.9(3) . . ? C16 Co1 C1 170.4(4) . . ? C6 Co1 C1 113.4(3) . . ? C5 Co1 C1 39.6(3) . . ? C7 Co1 C3 143.6(4) . . ? C15 Co1 C3 127.6(3) . . ? C16 Co1 C3 115.7(3) . . ? C6 Co1 C3 169.1(4) . . ? C5 Co1 C3 66.0(3) . . ? C1 Co1 C3 66.2(3) . . ? C7 Co1 C4 117.6(3) . . ? C15 Co1 C4 159.6(3) . . ? C16 Co1 C4 121.4(3) . . ? C6 Co1 C4 151.7(3) . . ? C5 Co1 C4 39.5(3) . . ? C1 Co1 C4 66.4(3) . . ? C3 Co1 C4 39.1(3) . . ? C7 Co1 C2 175.9(3) . . ? C15 Co1 C2 113.4(3) . . ? C16 Co1 C2 135.1(3) . . ? C6 Co1 C2 133.1(4) . . ? C5 Co1 C2 67.0(3) . . ? C1 Co1 C2 40.2(3) . . ? C3 Co1 C2 39.4(3) . . ? C4 Co1 C2 66.6(3) . . ? C5 C1 C2 108.1(8) . . ? C5 C1 Co1 70.1(4) . . ? C2 C1 Co1 70.5(4) . . ? C3 C2 C1 106.1(7) . . ? C3 C2 Co1 69.9(4) . . ? C1 C2 Co1 69.3(4) . . ? C4 C3 C2 109.8(8) . . ? C4 C3 Co1 70.7(4) . . ? C2 C3 Co1 70.7(4) . . ? C3 C4 C5 107.6(8) . . ? C3 C4 Co1 70.2(4) . . ? C5 C4 Co1 69.6(4) . . ? C1 C5 C4 108.3(7) . . ? C1 C5 Co1 70.3(4) . . ? C4 C5 Co1 70.8(4) . . ? C15 C6 C7 89.3(5) . . ? C15 C6 C23 134.0(6) . . ? C7 C6 C23 136.0(5) . . ? C15 C6 Co1 68.1(3) . . ? C7 C6 Co1 67.7(3) . . ? C23 C6 Co1 128.3(5) . . ? C16 C7 C6 90.2(5) . . ? C16 C7 C8 135.1(7) . . ? C6 C7 C8 134.4(6) . . ? C16 C7 Co1 68.7(3) . . ? C6 C7 Co1 69.0(3) . . ? C8 C7 Co1 124.6(4) . . ? C16 C7 C15 44.9(4) . . ? C6 C7 C15 45.3(3) . . ? C8 C7 C15 176.5(4) . . ? Co1 C7 C15 58.9(2) . . ? C7 C8 C9 113.9(5) . . ? C10 C9 C8 114.2(5) . . ? N11 C10 C9 113.8(5) . . ? C10 N11 C12 112.5(4) . . ? C10 N11 C31 113.5(4) . . ? C12 N11 C31 109.6(4) . . ? N11 C12 C13 113.2(5) . . ? C14 C13 C12 110.8(5) 7_565 . ? C13 C14 C15 114.0(5) 7_565 . ? C16 C15 C6 90.5(5) . . ? C16 C15 C14 135.8(6) . . ? C6 C15 C14 133.6(7) . . ? C16 C15 Co1 68.4(3) . . ? C6 C15 Co1 68.7(3) . . ? C14 C15 Co1 123.7(4) . . ? C16 C15 C7 45.1(4) . . ? C6 C15 C7 45.4(3) . . ? C14 C15 C7 177.7(4) . . ? Co1 C15 C7 58.5(2) . . ? C15 C16 C7 90.0(6) . . ? C15 C16 C17 134.3(7) . . ? C7 C16 C17 135.4(7) . . ? C15 C16 Co1 68.6(4) . . ? C7 C16 Co1 68.1(3) . . ? C17 C16 Co1 125.8(5) . . ? C18 C17 C16 125.8(13) 7_565 . ? C18 C19 N20 123.3(15) . . ? C17 C18 C19 136.1(17) 7_565 . ? C24 N20 C21 98.6(8) . . ? C24 N20 C21B 130.3(10) . . ? C21 N20 C21B 38.8(7) . . ? C24 N20 C19 119.2(9) . . ? C21 N20 C19 111.6(8) . . ? C21B N20 C19 103.6(11) . . ? C22 C21 N20 109.0(9) . . ? C21 C22 C23 108.3(9) . . ? C6 C23 C22B 128.3(10) . . ? C6 C23 C22 100.2(6) . . ? C22B C23 C22 41.7(7) . . ? C25 C24 N20 113.2(9) . . ? C26 C25 C24 116.1(12) . . ? C25 C26 C27 114.8(12) . . ? C28 C27 C26 120.0(9) . . ? C27 C28 C29 117.2(9) . . ? C30 C29 C28 118.2(8) . . ? C29 C30 C31 112.6(7) . . ? N11 C31 C30 110.3(5) . . ? C22B C21B N20 112.3(12) . . ? C21B C22B C23 106.7(12) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.59 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.484 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.055 #=======================================================================