# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 921192' #TrackingRef 'web_deposit_cif_file_0_RichardLewis_1361299243.Complex 1 Final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H88 Co Li2 N4 O2' _chemical_formula_weight 777.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4875(18) _cell_length_b 19.709(2) _cell_length_c 19.089(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.876(7) _cell_angle_gamma 90.00 _cell_volume 4664.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9234 _exptl_absorpt_correction_T_max 0.9800 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 37397 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.81 _reflns_number_total 8016 _reflns_number_gt 5745 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+0.2299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8016 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24377(3) 0.243134(19) 0.992458(19) 0.01339(14) Uani 1 1 d . . . N1 N 0.28990(19) 0.32993(12) 1.04385(12) 0.0160(5) Uani 1 1 d . . . N2 N 0.08575(19) 0.26453(12) 0.98487(12) 0.0148(5) Uani 1 1 d . . . N3 N 0.32623(19) 0.21367(12) 0.91418(12) 0.0145(5) Uani 1 1 d . . . N4 N 0.29546(18) 0.16314(12) 1.05608(12) 0.0156(5) Uani 1 1 d . . . C1 C 0.3652(2) 0.36519(15) 1.07476(15) 0.0166(6) Uani 1 1 d . . . C2 C 0.4838(2) 0.35633(15) 1.05554(17) 0.0217(7) Uani 1 1 d . . . C3 C 0.5136(3) 0.28180(17) 1.0632(2) 0.0363(9) Uani 1 1 d . . . H3A H 0.4560 0.2542 1.0381 0.054 Uiso 1 1 calc R . . H3B H 0.5230 0.2694 1.1132 0.054 Uiso 1 1 calc R . . H3C H 0.5811 0.2737 1.0431 0.054 Uiso 1 1 calc R . . C4 C 0.4799(3) 0.3759(2) 0.97753(19) 0.0430(10) Uani 1 1 d . . . H4A H 0.4610 0.4240 0.9717 0.065 Uiso 1 1 calc R . . H4B H 0.4256 0.3482 0.9493 0.065 Uiso 1 1 calc R . . H4C H 0.5508 0.3680 0.9618 0.065 Uiso 1 1 calc R . . C5 C 0.5766(3) 0.3967(2) 1.0949(2) 0.0570(13) Uani 1 1 d . . . H5A H 0.5602 0.4452 1.0912 0.086 Uiso 1 1 calc R . . H5B H 0.6431 0.3874 1.0739 0.086 Uiso 1 1 calc R . . H5C H 0.5863 0.3832 1.1446 0.086 Uiso 1 1 calc R . . C6 C 0.3410(2) 0.41761(16) 1.13298(15) 0.0223(7) Uani 1 1 d . . . C7 C 0.3898(3) 0.3908(2) 1.20549(17) 0.0405(10) Uani 1 1 d . . . H7A H 0.3633 0.3447 1.2122 0.061 Uiso 1 1 calc R . . H7B H 0.3685 0.4204 1.2426 0.061 Uiso 1 1 calc R . . H7C H 0.4686 0.3901 1.2078 0.061 Uiso 1 1 calc R . . C8 C 0.3817(3) 0.49017(17) 1.1214(2) 0.0350(9) Uani 1 1 d . . . H8A H 0.3502 0.5067 1.0751 0.053 Uiso 1 1 calc R . . H8B H 0.4605 0.4898 1.1237 0.053 Uiso 1 1 calc R . . H8C H 0.3601 0.5201 1.1583 0.053 Uiso 1 1 calc R . . C9 C 0.2193(3) 0.42282(17) 1.13516(17) 0.0259(8) Uani 1 1 d . . . H9A H 0.1847 0.4398 1.0897 0.039 Uiso 1 1 calc R . . H9B H 0.2048 0.4541 1.1728 0.039 Uiso 1 1 calc R . . H9C H 0.1904 0.3779 1.1444 0.039 Uiso 1 1 calc R . . C10 C -0.0084(2) 0.24044(14) 0.97498(14) 0.0157(6) Uani 1 1 d . . . C11 C -0.0309(2) 0.17178(16) 0.93303(16) 0.0215(7) Uani 1 1 d . . . C12 C 0.0359(3) 0.17204(17) 0.87062(17) 0.0264(8) Uani 1 1 d . . . H12A H 0.0116 0.2092 0.8384 0.040 Uiso 1 1 calc R . . H12B H 0.0264 0.1287 0.8454 0.040 Uiso 1 1 calc R . . H12C H 0.1123 0.1784 0.8881 0.040 Uiso 1 1 calc R . . C13 C 0.0094(3) 0.11374(16) 0.98255(18) 0.0303(8) Uani 1 1 d . . . H13A H -0.0324 0.1128 1.0229 0.045 Uiso 1 1 calc R . . H13B H 0.0858 0.1207 0.9994 0.045 Uiso 1 1 calc R . . H13C H 0.0004 0.0706 0.9571 0.045 Uiso 1 1 calc R . . C14 C -0.1475(3) 0.15632(18) 0.90053(18) 0.0316(8) Uani 1 1 d . . . H14A H -0.1739 0.1933 0.8687 0.047 Uiso 1 1 calc R . . H14B H -0.1939 0.1522 0.9382 0.047 Uiso 1 1 calc R . . H14C H -0.1488 0.1137 0.8740 0.047 Uiso 1 1 calc R . . C15 C -0.1012(2) 0.27480(16) 1.01046(15) 0.0183(7) Uani 1 1 d . . . C16 C -0.0573(3) 0.33467(17) 1.05551(17) 0.0211(7) Uani 1 1 d . . . C17 C -0.1906(2) 0.30360(18) 0.95581(17) 0.0286(8) Uani 1 1 d . . . H17A H -0.2214 0.2669 0.9251 0.043 Uiso 1 1 calc R . . H17B H -0.1599 0.3382 0.9272 0.043 Uiso 1 1 calc R . . H17C H -0.2472 0.3240 0.9803 0.043 Uiso 1 1 calc R . . C18 C -0.1499(3) 0.22582(17) 1.06100(17) 0.0259(8) Uani 1 1 d . . . H18A H -0.1792 0.1859 1.0347 0.039 Uiso 1 1 calc R . . H18B H -0.2077 0.2488 1.0821 0.039 Uiso 1 1 calc R . . H18C H -0.0936 0.2115 1.0983 0.039 Uiso 1 1 calc R . . C19 C 0.3578(2) 0.22896(14) 0.85630(15) 0.0147(6) Uani 1 1 d . . . C20 C 0.2913(2) 0.27741(15) 0.80164(15) 0.0199(7) Uani 1 1 d . . . C21 C 0.2213(3) 0.23343(16) 0.74689(16) 0.0243(7) Uani 1 1 d . . . H21A H 0.2682 0.2057 0.7208 0.037 Uiso 1 1 calc R . . H21B H 0.1767 0.2629 0.7139 0.037 Uiso 1 1 calc R . . H21C H 0.1747 0.2038 0.7712 0.037 Uiso 1 1 calc R . . C22 C 0.3565(3) 0.32713(17) 0.76176(18) 0.0311(8) Uani 1 1 d . . . H22A H 0.4062 0.3017 0.7356 0.047 Uiso 1 1 calc R . . H22B H 0.3977 0.3576 0.7955 0.047 Uiso 1 1 calc R . . H22C H 0.3072 0.3539 0.7287 0.047 Uiso 1 1 calc R . . C23 C 0.2151(3) 0.31999(16) 0.84043(17) 0.0244(7) Uani 1 1 d . . . H23A H 0.1714 0.2900 0.8666 0.037 Uiso 1 1 calc R . . H23B H 0.1677 0.3466 0.8062 0.037 Uiso 1 1 calc R . . H23C H 0.2572 0.3507 0.8735 0.037 Uiso 1 1 calc R . . C24 C 0.4686(2) 0.19838(15) 0.83716(15) 0.0187(7) Uani 1 1 d . . . C25 C 0.5574(3) 0.25300(17) 0.84464(17) 0.0268(8) Uani 1 1 d . . . H25A H 0.5371 0.2901 0.8114 0.040 Uiso 1 1 calc R . . H25B H 0.6256 0.2330 0.8343 0.040 Uiso 1 1 calc R . . H25C H 0.5660 0.2707 0.8929 0.040 Uiso 1 1 calc R . . C26 C 0.4630(3) 0.16691(17) 0.76272(16) 0.0238(7) Uani 1 1 d . . . H26A H 0.4374 0.2011 0.7273 0.036 Uiso 1 1 calc R . . H26B H 0.4132 0.1283 0.7592 0.036 Uiso 1 1 calc R . . H26C H 0.5350 0.1514 0.7544 0.036 Uiso 1 1 calc R . . C27 C 0.5086(3) 0.14384(16) 0.89052(16) 0.0234(7) Uani 1 1 d . . . H27A H 0.4557 0.1070 0.8887 0.035 Uiso 1 1 calc R . . H27B H 0.5183 0.1635 0.9380 0.035 Uiso 1 1 calc R . . H27C H 0.5777 0.1259 0.8791 0.035 Uiso 1 1 calc R . . C28 C 0.3074(2) 0.13705(15) 1.11617(15) 0.0165(6) Uani 1 1 d . . . C29 C 0.2346(3) 0.15555(17) 1.17499(16) 0.0269(8) Uani 1 1 d . . . C30 C 0.1727(3) 0.2195(2) 1.15410(19) 0.0426(10) Uani 1 1 d . . . H30A H 0.1371 0.2150 1.1057 0.064 Uiso 1 1 calc R . . H30B H 0.2224 0.2581 1.1568 0.064 Uiso 1 1 calc R . . H30C H 0.1181 0.2270 1.1862 0.064 Uiso 1 1 calc R . . C31 C 0.2891(3) 0.1619(2) 1.24954(19) 0.0510(12) Uani 1 1 d . . . H31A H 0.3294 0.1203 1.2628 0.076 Uiso 1 1 calc R . . H31B H 0.2345 0.1691 1.2816 0.076 Uiso 1 1 calc R . . H31C H 0.3389 0.2006 1.2526 0.076 Uiso 1 1 calc R . . C32 C 0.1452(3) 0.0993(2) 1.1746(2) 0.0503(11) Uani 1 1 d . . . H32A H 0.1791 0.0556 1.1883 0.075 Uiso 1 1 calc R . . H32B H 0.1060 0.0955 1.1271 0.075 Uiso 1 1 calc R . . H32C H 0.0947 0.1116 1.2081 0.075 Uiso 1 1 calc R . . C33 C 0.4015(2) 0.08342(16) 1.13516(15) 0.0208(7) Uani 1 1 d . . . C34 C 0.4959(3) 0.11654(18) 1.18243(19) 0.0356(9) Uani 1 1 d . . . H34A H 0.5179 0.1581 1.1599 0.053 Uiso 1 1 calc R . . H34B H 0.5568 0.0849 1.1890 0.053 Uiso 1 1 calc R . . H34C H 0.4729 0.1276 1.2284 0.053 Uiso 1 1 calc R . . C35 C 0.3666(3) 0.01875(16) 1.17046(18) 0.0315(8) Uani 1 1 d . . . H35A H 0.3365 0.0306 1.2140 0.047 Uiso 1 1 calc R . . H35B H 0.4293 -0.0110 1.1817 0.047 Uiso 1 1 calc R . . H35C H 0.3118 -0.0048 1.1383 0.047 Uiso 1 1 calc R . . C36 C 0.4481(3) 0.0614(2) 1.06858(17) 0.0389(10) Uani 1 1 d . . . H36A H 0.4719 0.1014 1.0442 0.058 Uiso 1 1 calc R . . H36B H 0.3927 0.0373 1.0373 0.058 Uiso 1 1 calc R . . H36C H 0.5098 0.0312 1.0813 0.058 Uiso 1 1 calc R . . C37 C 0.1920(2) 0.48378(16) 0.94330(17) 0.0247(7) Uani 1 1 d . . . H37A H 0.2648 0.4636 0.9537 0.030 Uiso 1 1 calc R . . H37B H 0.1875 0.5241 0.9737 0.030 Uiso 1 1 calc R . . C38 C 0.1699(3) 0.50307(16) 0.86608(17) 0.0263(8) Uani 1 1 d . . . H38A H 0.2042 0.4708 0.8358 0.032 Uiso 1 1 calc R . . H38B H 0.1954 0.5496 0.8577 0.032 Uiso 1 1 calc R . . C39 C 0.0479(3) 0.49851(16) 0.85331(16) 0.0259(7) Uani 1 1 d . . . H39A H 0.0142 0.5411 0.8673 0.031 Uiso 1 1 calc R . . H39B H 0.0232 0.4892 0.8030 0.031 Uiso 1 1 calc R . . C40 C 0.0209(2) 0.44018(17) 0.89928(16) 0.0250(7) Uani 1 1 d . . . H40A H -0.0474 0.4491 0.9191 0.030 Uiso 1 1 calc R . . H40B H 0.0131 0.3976 0.8716 0.030 Uiso 1 1 calc R . . C41 C 0.2242(3) -0.01119(18) 0.9355(2) 0.0427(10) Uani 1 1 d . . . H41A H 0.1815 -0.0021 0.9750 0.051 Uiso 1 1 calc R . . H41B H 0.2818 -0.0441 0.9516 0.051 Uiso 1 1 calc R . . C42 C 0.1545(7) -0.0379(3) 0.8741(3) 0.154(4) Uani 1 1 d . . . H42A H 0.1755 -0.0852 0.8647 0.185 Uiso 1 1 calc R . . H42B H 0.0785 -0.0380 0.8840 0.185 Uiso 1 1 calc R . . C43 C 0.1649(3) 0.0035(2) 0.8133(2) 0.0505(12) Uani 1 1 d . . . H43A H 0.0983 0.0301 0.7999 0.061 Uiso 1 1 calc R . . H43B H 0.1795 -0.0248 0.7727 0.061 Uiso 1 1 calc R . . C44 C 0.2586(3) 0.04954(17) 0.83608(17) 0.0300(8) Uani 1 1 d . . . H44A H 0.3252 0.0320 0.8191 0.036 Uiso 1 1 calc R . . H44B H 0.2444 0.0957 0.8168 0.036 Uiso 1 1 calc R . . H16A H -0.033(3) 0.3708(19) 1.025(2) 0.045 Uiso 1 1 d . . . H16B H -0.002(3) 0.3225(19) 1.088(2) 0.045 Uiso 1 1 d . . . H16C H -0.117(3) 0.3519(19) 1.0790(19) 0.045 Uiso 1 1 d . . . Li1 Li 0.1387(4) 0.3542(3) 1.0162(3) 0.0193(11) Uani 1 1 d . . . Li2 Li 0.3381(4) 0.1286(3) 0.9671(3) 0.0230(12) Uani 1 1 d . . . O1 O 0.11002(16) 0.43491(10) 0.95531(11) 0.0223(5) Uani 1 1 d . . . O2 O 0.27017(19) 0.05087(11) 0.91222(11) 0.0304(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0121(2) 0.0155(2) 0.0129(2) 0.00002(16) 0.00260(14) 0.00133(16) N1 0.0158(13) 0.0188(13) 0.0134(13) 0.0027(10) 0.0020(10) -0.0018(11) N2 0.0155(13) 0.0190(14) 0.0099(12) 0.0033(10) 0.0015(9) 0.0006(10) N3 0.0151(13) 0.0156(13) 0.0131(13) -0.0012(10) 0.0025(10) -0.0036(10) N4 0.0155(13) 0.0167(13) 0.0147(13) 0.0016(10) 0.0015(10) -0.0027(10) C1 0.0172(16) 0.0172(16) 0.0150(15) 0.0030(12) 0.0003(12) 0.0031(13) C2 0.0144(16) 0.0196(17) 0.0308(18) -0.0024(14) 0.0007(13) -0.0022(13) C3 0.0207(19) 0.0265(19) 0.062(3) 0.0050(18) 0.0070(17) 0.0052(15) C4 0.031(2) 0.055(3) 0.047(2) 0.016(2) 0.0226(18) 0.0098(19) C5 0.019(2) 0.068(3) 0.084(3) -0.044(3) 0.004(2) -0.0094(19) C6 0.0257(18) 0.0244(18) 0.0164(16) -0.0048(13) 0.0012(13) -0.0045(14) C7 0.035(2) 0.066(3) 0.0190(18) -0.0013(18) -0.0034(15) -0.0014(19) C8 0.034(2) 0.027(2) 0.045(2) -0.0140(17) 0.0084(17) -0.0054(16) C9 0.0275(18) 0.0269(19) 0.0241(17) -0.0110(14) 0.0062(14) 0.0010(14) C10 0.0155(16) 0.0187(16) 0.0122(14) 0.0016(12) -0.0006(11) 0.0011(12) C11 0.0192(17) 0.0239(18) 0.0218(17) -0.0076(13) 0.0038(13) -0.0021(13) C12 0.0208(17) 0.033(2) 0.0261(18) -0.0120(15) 0.0059(14) -0.0026(14) C13 0.032(2) 0.0234(18) 0.036(2) -0.0030(15) 0.0087(15) -0.0048(15) C14 0.0213(18) 0.041(2) 0.033(2) -0.0179(17) 0.0039(15) -0.0085(15) C15 0.0146(15) 0.0244(17) 0.0163(15) -0.0013(13) 0.0031(12) 0.0014(13) C16 0.0202(18) 0.0225(18) 0.0215(17) -0.0022(14) 0.0062(14) 0.0046(14) C17 0.0148(17) 0.040(2) 0.0306(19) -0.0035(16) 0.0023(14) 0.0062(15) C18 0.0201(17) 0.0321(19) 0.0276(18) -0.0062(15) 0.0109(14) -0.0027(14) C19 0.0162(15) 0.0134(15) 0.0142(15) -0.0021(12) 0.0011(12) -0.0032(12) C20 0.0229(17) 0.0208(17) 0.0168(16) 0.0039(13) 0.0052(13) 0.0006(13) C21 0.0264(18) 0.0308(19) 0.0158(16) 0.0017(14) 0.0020(13) 0.0028(14) C22 0.038(2) 0.029(2) 0.0281(19) 0.0102(15) 0.0088(16) 0.0008(16) C23 0.0285(18) 0.0205(18) 0.0235(18) 0.0029(14) 0.0002(14) 0.0049(14) C24 0.0177(16) 0.0215(17) 0.0179(16) -0.0022(13) 0.0061(12) -0.0016(13) C25 0.0209(17) 0.035(2) 0.0259(17) -0.0053(15) 0.0074(13) -0.0038(15) C26 0.0240(18) 0.0289(19) 0.0205(17) -0.0036(14) 0.0106(13) 0.0005(14) C27 0.0206(17) 0.0254(18) 0.0256(17) -0.0019(14) 0.0087(13) 0.0055(14) C28 0.0197(16) 0.0163(16) 0.0142(15) -0.0006(12) 0.0041(12) -0.0033(13) C29 0.034(2) 0.034(2) 0.0141(16) 0.0075(14) 0.0061(14) 0.0120(15) C30 0.047(2) 0.056(3) 0.027(2) 0.0054(18) 0.0164(17) 0.028(2) C31 0.061(3) 0.069(3) 0.023(2) 0.001(2) 0.0067(18) 0.034(2) C32 0.039(2) 0.060(3) 0.055(3) 0.018(2) 0.020(2) 0.001(2) C33 0.0244(17) 0.0221(17) 0.0167(16) 0.0044(13) 0.0058(13) 0.0083(13) C34 0.0224(18) 0.037(2) 0.045(2) 0.0071(17) -0.0057(16) 0.0059(16) C35 0.039(2) 0.0225(19) 0.033(2) 0.0030(15) 0.0057(16) 0.0073(16) C36 0.047(2) 0.045(2) 0.0270(19) 0.0121(17) 0.0142(17) 0.0332(19) C37 0.0194(17) 0.0205(17) 0.0338(19) 0.0025(14) 0.0016(14) -0.0029(13) C38 0.035(2) 0.0161(17) 0.0290(19) 0.0005(14) 0.0098(15) -0.0011(14) C39 0.0320(19) 0.0249(18) 0.0196(17) 0.0005(14) -0.0024(14) -0.0024(15) C40 0.0197(17) 0.0294(19) 0.0245(17) 0.0018(14) -0.0028(13) 0.0009(14) C41 0.042(2) 0.026(2) 0.066(3) 0.0120(19) 0.028(2) -0.0059(17) C42 0.299(10) 0.132(6) 0.048(3) -0.056(4) 0.086(5) -0.177(7) C43 0.041(2) 0.030(2) 0.078(3) -0.021(2) -0.002(2) -0.0032(18) C44 0.037(2) 0.0241(19) 0.0288(19) -0.0010(15) 0.0039(15) -0.0016(15) Li1 0.017(3) 0.020(3) 0.021(3) 0.000(2) 0.003(2) 0.001(2) Li2 0.028(3) 0.020(3) 0.022(3) 0.003(2) 0.007(2) 0.008(2) O1 0.0205(12) 0.0206(12) 0.0247(12) 0.0029(9) -0.0015(9) -0.0020(9) O2 0.0454(15) 0.0200(12) 0.0285(13) -0.0013(10) 0.0162(11) -0.0081(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 N3 2.000(2) . ? Co1 N2 2.006(2) . ? Co1 N1 2.021(2) . ? Co1 N4 2.047(2) . ? Co1 Li2 2.617(5) . ? Co1 Li1 2.618(5) . ? N1 C1 1.258(4) . ? N1 Li1 1.957(5) . ? N2 C10 1.261(4) . ? N2 Li1 1.955(5) . ? N3 C19 1.253(4) . ? N3 Li2 1.954(6) . ? N4 C28 1.249(4) . ? N4 Li2 1.961(5) . ? C1 C6 1.573(4) . ? C1 C2 1.577(4) . ? C2 C3 1.518(4) . ? C2 C5 1.527(4) . ? C2 C4 1.533(5) . ? C6 C9 1.529(4) . ? C6 C7 1.538(4) . ? C6 C8 1.542(5) . ? C10 C15 1.564(4) . ? C10 C11 1.580(4) . ? C11 C13 1.530(4) . ? C11 C12 1.534(4) . ? C11 C14 1.544(4) . ? C15 C16 1.523(4) . ? C15 C18 1.540(4) . ? C15 C17 1.542(4) . ? C19 C20 1.576(4) . ? C19 C24 1.591(4) . ? C20 C23 1.525(4) . ? C20 C22 1.533(4) . ? C20 C21 1.545(4) . ? C24 C27 1.524(4) . ? C24 C25 1.540(4) . ? C24 C26 1.544(4) . ? C28 C29 1.570(4) . ? C28 C33 1.590(4) . ? C29 C31 1.507(5) . ? C29 C30 1.508(5) . ? C29 C32 1.574(5) . ? C33 C36 1.523(4) . ? C33 C35 1.529(4) . ? C33 C34 1.541(4) . ? C37 O1 1.444(4) . ? C37 C38 1.515(4) . ? C38 C39 1.516(5) . ? C39 C40 1.509(4) . ? C40 O1 1.452(3) . ? C41 O2 1.444(4) . ? C41 C42 1.472(7) . ? C42 C43 1.436(7) . ? C43 C44 1.504(5) . ? C44 O2 1.444(4) . ? Li1 O1 1.978(5) . ? Li2 O2 1.989(6) . ? 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 N3 Co1 N2 126.67(9) . . ? N3 Co1 N1 117.78(9) . . ? N2 Co1 N1 94.47(10) . . ? N3 Co1 N4 93.77(10) . . ? N2 Co1 N4 116.25(9) . . ? N1 Co1 N4 108.22(10) . . ? N3 Co1 Li2 47.79(13) . . ? N2 Co1 Li2 128.95(14) . . ? N1 Co1 Li2 135.30(14) . . ? N4 Co1 Li2 47.81(13) . . ? N3 Co1 Li1 133.26(13) . . ? N2 Co1 Li1 47.78(13) . . ? N1 Co1 Li1 47.81(12) . . ? N4 Co1 Li1 132.07(13) . . ? Li2 Co1 Li1 176.72(16) . . ? C1 N1 Li1 129.4(3) . . ? C1 N1 Co1 148.1(2) . . ? Li1 N1 Co1 82.28(17) . . ? C10 N2 Li1 131.4(3) . . ? C10 N2 Co1 145.4(2) . . ? Li1 N2 Co1 82.75(17) . . ? C19 N3 Li2 130.5(3) . . ? C19 N3 Co1 146.4(2) . . ? Li2 N3 Co1 82.90(17) . . ? C28 N4 Li2 129.6(3) . . ? C28 N4 Co1 148.9(2) . . ? Li2 N4 Co1 81.51(17) . . ? N1 C1 C6 119.9(3) . . ? N1 C1 C2 120.0(3) . . ? C6 C1 C2 120.1(2) . . ? C3 C2 C5 107.1(3) . . ? C3 C2 C4 108.4(3) . . ? C5 C2 C4 106.3(3) . . ? C3 C2 C1 108.1(2) . . ? C5 C2 C1 120.5(3) . . ? C4 C2 C1 106.1(2) . . ? C9 C6 C7 106.6(3) . . ? C9 C6 C8 106.7(3) . . ? C7 C6 C8 110.2(3) . . ? C9 C6 C1 109.8(2) . . ? C7 C6 C1 108.7(3) . . ? C8 C6 C1 114.4(3) . . ? N2 C10 C15 119.9(3) . . ? N2 C10 C11 120.2(3) . . ? C15 C10 C11 119.6(2) . . ? C13 C11 C12 108.3(3) . . ? C13 C11 C14 109.0(3) . . ? C12 C11 C14 105.2(3) . . ? C13 C11 C10 107.6(2) . . ? C12 C11 C10 108.1(2) . . ? C14 C11 C10 118.3(3) . . ? C16 C15 C18 105.9(3) . . ? C16 C15 C17 106.2(3) . . ? C18 C15 C17 110.3(3) . . ? C16 C15 C10 110.2(2) . . ? C18 C15 C10 111.6(2) . . ? C17 C15 C10 112.3(2) . . ? N3 C19 C20 122.2(3) . . ? N3 C19 C24 119.0(3) . . ? C20 C19 C24 118.8(2) . . ? C23 C20 C22 106.8(3) . . ? C23 C20 C21 107.6(3) . . ? C22 C20 C21 108.3(3) . . ? C23 C20 C19 108.8(2) . . ? C22 C20 C19 116.5(3) . . ? C21 C20 C19 108.6(2) . . ? C27 C24 C25 104.8(2) . . ? C27 C24 C26 107.9(2) . . ? C25 C24 C26 108.6(2) . . ? C27 C24 C19 109.8(2) . . ? C25 C24 C19 110.5(2) . . ? C26 C24 C19 114.8(2) . . ? N4 C28 C29 123.0(3) . . ? N4 C28 C33 119.1(3) . . ? C29 C28 C33 117.8(2) . . ? C31 C29 C30 109.8(3) . . ? C31 C29 C28 117.4(3) . . ? C30 C29 C28 109.1(3) . . ? C31 C29 C32 107.7(3) . . ? C30 C29 C32 104.3(3) . . ? C28 C29 C32 107.7(3) . . ? C36 C33 C35 106.7(3) . . ? C36 C33 C34 105.5(3) . . ? C35 C33 C34 109.5(3) . . ? C36 C33 C28 110.2(2) . . ? C35 C33 C28 114.4(3) . . ? C34 C33 C28 110.1(3) . . ? O1 C37 C38 105.8(2) . . ? C37 C38 C39 101.8(3) . . ? C40 C39 C38 104.0(3) . . ? O1 C40 C39 106.2(2) . . ? O2 C41 C42 106.0(3) . . ? C43 C42 C41 109.8(4) . . ? C42 C43 C44 104.6(4) . . ? O2 C44 C43 106.4(3) . . ? N2 Li1 N1 98.2(2) . . ? N2 Li1 O1 121.1(3) . . ? N1 Li1 O1 117.1(3) . . ? N2 Li1 Co1 49.47(13) . . ? N1 Li1 Co1 49.91(13) . . ? O1 Li1 Co1 129.1(2) . . ? N3 Li2 N4 98.0(2) . . ? N3 Li2 O2 112.8(3) . . ? N4 Li2 O2 125.5(3) . . ? N3 Li2 Co1 49.30(13) . . ? N4 Li2 Co1 50.67(13) . . ? O2 Li2 Co1 126.1(2) . . ? C37 O1 C40 109.3(2) . . ? C37 O1 Li1 123.2(2) . . ? C40 O1 Li1 124.0(2) . . ? C44 O2 C41 107.4(3) . . ? C44 O2 Li2 122.0(2) . . ? C41 O2 Li2 130.6(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.81 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.817 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.062 data_Complex_2 _database_code_depnum_ccdc_archive 'CCDC 921193' #TrackingRef 'web_deposit_cif_file_1_RichardLewis_1361299243.Complex 2 Final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H70 Co Li N3 O4' _chemical_formula_weight 662.81 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8516(11) _cell_length_b 13.2752(14) _cell_length_c 13.4533(12) _cell_angle_alpha 82.003(6) _cell_angle_beta 87.087(7) _cell_angle_gamma 81.136(7) _cell_volume 1895.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 121 _cell_measurement_theta_min 2.355 _cell_measurement_theta_max 20.54 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9083 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 14057 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.1162 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 24.93 _reflns_number_total 6577 _reflns_number_gt 4151 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+0.2822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6577 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.810 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.28227(5) 0.26904(4) 0.26903(4) 0.01259(16) Uani 1 1 d . . . N1 N 0.2288(3) 0.2521(2) 0.4043(2) 0.0157(7) Uani 1 1 d . . . N2 N 0.3722(3) 0.3924(2) 0.2362(2) 0.0127(7) Uani 1 1 d . . . N3 N 0.2586(3) 0.1941(2) 0.1644(2) 0.0148(7) Uani 1 1 d . . . O1 O 0.4855(2) 0.17175(18) 0.29329(18) 0.0143(6) Uani 1 1 d . . . C1 C 0.3308(3) 0.4843(3) 0.2007(3) 0.0119(8) Uani 1 1 d . . . C2 C 0.4153(3) 0.5712(3) 0.2030(3) 0.0127(8) Uani 1 1 d . . . C3 C 0.5495(4) 0.5208(3) 0.2238(3) 0.0245(10) Uani 1 1 d . . . H3A H 0.5536 0.4838 0.2921 0.037 Uiso 1 1 calc R . . H3B H 0.6041 0.5739 0.2170 0.037 Uiso 1 1 calc R . . H3C H 0.5770 0.4724 0.1755 0.037 Uiso 1 1 calc R . . C4 C 0.3722(4) 0.6336(3) 0.2901(3) 0.0219(9) Uani 1 1 d . . . H4A H 0.2900 0.6739 0.2760 0.033 Uiso 1 1 calc R . . H4B H 0.4322 0.6801 0.2971 0.033 Uiso 1 1 calc R . . H4C H 0.3670 0.5866 0.3526 0.033 Uiso 1 1 calc R . . C5 C 0.4222(4) 0.6450(3) 0.1051(3) 0.0199(9) Uani 1 1 d . . . H5A H 0.4562 0.6060 0.0506 0.030 Uiso 1 1 calc R . . H5B H 0.4765 0.6956 0.1136 0.030 Uiso 1 1 calc R . . H5C H 0.3384 0.6807 0.0885 0.030 Uiso 1 1 calc R . . C6 C 0.1990(3) 0.5159(3) 0.1519(3) 0.0153(8) Uani 1 1 d . . . C7 C 0.1250(4) 0.6180(3) 0.1778(3) 0.0267(10) Uani 1 1 d . . . H7A H 0.0419 0.6282 0.1494 0.040 Uiso 1 1 calc R . . H7B H 0.1693 0.6750 0.1496 0.040 Uiso 1 1 calc R . . H7C H 0.1167 0.6159 0.2509 0.040 Uiso 1 1 calc R . . C8 C 0.2162(4) 0.5209(3) 0.0372(3) 0.0237(10) Uani 1 1 d . . . H8A H 0.1343 0.5339 0.0066 0.036 Uiso 1 1 calc R . . H8B H 0.2617 0.4554 0.0206 0.036 Uiso 1 1 calc R . . H8C H 0.2636 0.5766 0.0114 0.036 Uiso 1 1 calc R . . C9 C 0.1143(3) 0.4341(3) 0.1853(3) 0.0184(9) Uani 1 1 d . . . H9A H 0.1099 0.4210 0.2588 0.028 Uiso 1 1 calc R . . H9B H 0.1484 0.3703 0.1584 0.028 Uiso 1 1 calc R . . H9C H 0.0304 0.4588 0.1600 0.028 Uiso 1 1 calc R . . C10 C 0.1994(3) 0.2668(3) 0.4932(3) 0.0137(8) Uani 1 1 d . . . C11 C 0.2243(3) 0.3702(3) 0.5306(3) 0.0153(8) Uani 1 1 d . . . C12 C 0.1686(4) 0.4587(3) 0.4531(3) 0.0193(9) Uani 1 1 d . . . H12A H 0.2131 0.4535 0.3883 0.029 Uiso 1 1 calc R . . H12B H 0.1770 0.5244 0.4755 0.029 Uiso 1 1 calc R . . H12C H 0.0802 0.4549 0.4457 0.029 Uiso 1 1 calc R . . C13 C 0.3664(4) 0.3669(3) 0.5276(3) 0.0261(10) Uani 1 1 d . . . H13A H 0.3996 0.3575 0.4599 0.039 Uiso 1 1 calc R . . H13B H 0.4039 0.3094 0.5758 0.039 Uiso 1 1 calc R . . H13C H 0.3864 0.4316 0.5453 0.039 Uiso 1 1 calc R . . C14 C 0.1740(4) 0.3948(3) 0.6347(3) 0.0217(9) Uani 1 1 d . . . H14A H 0.2013 0.4584 0.6482 0.033 Uiso 1 1 calc R . . H14B H 0.2060 0.3382 0.6859 0.033 Uiso 1 1 calc R . . H14C H 0.0826 0.4034 0.6363 0.033 Uiso 1 1 calc R . . C15 C 0.1452(4) 0.1818(3) 0.5685(3) 0.0165(9) Uani 1 1 d . . . C16 C 0.2423(4) 0.1329(3) 0.6474(3) 0.0232(10) Uani 1 1 d . . . H16A H 0.2089 0.0785 0.6926 0.035 Uiso 1 1 calc R . . H16B H 0.2610 0.1857 0.6863 0.035 Uiso 1 1 calc R . . H16C H 0.3189 0.1036 0.6136 0.035 Uiso 1 1 calc R . . C17 C 0.0206(4) 0.2223(3) 0.6211(3) 0.0212(9) Uani 1 1 d . . . H17A H 0.0382 0.2492 0.6823 0.032 Uiso 1 1 calc R . . H17B H -0.0285 0.1660 0.6386 0.032 Uiso 1 1 calc R . . H17C H -0.0265 0.2773 0.5757 0.032 Uiso 1 1 calc R . . C18 C 0.1202(4) 0.0959(3) 0.5104(3) 0.0229(10) Uani 1 1 d . . . H18A H 0.1984 0.0658 0.4794 0.034 Uiso 1 1 calc R . . H18B H 0.0602 0.1244 0.4580 0.034 Uiso 1 1 calc R . . H18C H 0.0860 0.0426 0.5566 0.034 Uiso 1 1 calc R . . C19 C 0.2286(3) 0.1265(3) 0.1177(3) 0.0132(8) Uani 1 1 d . . . C20 C 0.1871(3) 0.0251(3) 0.1764(3) 0.0164(9) Uani 1 1 d . . . C21 C 0.2568(4) -0.0025(3) 0.2750(3) 0.0235(10) Uani 1 1 d . . . H21A H 0.2194 -0.0561 0.3182 0.035 Uiso 1 1 calc R . . H21B H 0.2509 0.0587 0.3091 0.035 Uiso 1 1 calc R . . H21C H 0.3447 -0.0278 0.2606 0.035 Uiso 1 1 calc R . . C22 C 0.0478(4) 0.0516(3) 0.2034(3) 0.0274(10) Uani 1 1 d . . . H22A H 0.0187 -0.0081 0.2436 0.041 Uiso 1 1 calc R . . H22B H 0.0005 0.0699 0.1417 0.041 Uiso 1 1 calc R . . H22C H 0.0352 0.1098 0.2422 0.041 Uiso 1 1 calc R . . C23 C 0.2094(4) -0.0730(3) 0.1256(3) 0.0267(10) Uani 1 1 d . . . H23A H 0.2989 -0.0916 0.1117 0.040 Uiso 1 1 calc R . . H23B H 0.1649 -0.0608 0.0625 0.040 Uiso 1 1 calc R . . H23C H 0.1786 -0.1292 0.1702 0.040 Uiso 1 1 calc R . . C24 C 0.2273(4) 0.1456(3) -0.0008(3) 0.0168(9) Uani 1 1 d . . . C25 C 0.2422(4) 0.2574(3) -0.0363(3) 0.0232(10) Uani 1 1 d . . . H25A H 0.3205 0.2717 -0.0119 0.035 Uiso 1 1 calc R . . H25B H 0.1720 0.3028 -0.0098 0.035 Uiso 1 1 calc R . . H25C H 0.2436 0.2696 -0.1098 0.035 Uiso 1 1 calc R . . C26 C 0.3368(4) 0.0781(3) -0.0475(3) 0.0326(11) Uani 1 1 d . . . H26A H 0.3264 0.0056 -0.0309 0.049 Uiso 1 1 calc R . . H26B H 0.4153 0.0890 -0.0206 0.049 Uiso 1 1 calc R . . H26C H 0.3385 0.0967 -0.1206 0.049 Uiso 1 1 calc R . . C27 C 0.1037(4) 0.1300(3) -0.0429(3) 0.0271(10) Uani 1 1 d . . . H27A H 0.1059 0.1479 -0.1161 0.041 Uiso 1 1 calc R . . H27B H 0.0346 0.1742 -0.0137 0.041 Uiso 1 1 calc R . . H27C H 0.0916 0.0579 -0.0258 0.041 Uiso 1 1 calc R . . C30 C 0.7703(3) 0.2388(3) 0.1608(3) 0.0194(9) Uani 1 1 d . . . H30A H 0.8054 0.2288 0.0929 0.023 Uiso 1 1 calc R . . H30B H 0.7873 0.1726 0.2053 0.023 Uiso 1 1 calc R . . C31 C 0.8281(4) 0.3196(3) 0.2009(3) 0.0228(10) Uani 1 1 d . . . H31A H 0.9185 0.2961 0.2090 0.027 Uiso 1 1 calc R . . H31B H 0.8178 0.3835 0.1525 0.027 Uiso 1 1 calc R . . C32 C 0.8250(4) 0.2748(3) 0.3798(3) 0.0233(10) Uani 1 1 d . . . H32A H 0.8979 0.3012 0.4023 0.028 Uiso 1 1 calc R . . H32B H 0.8523 0.2043 0.3630 0.028 Uiso 1 1 calc R . . C33 C 0.7230(4) 0.2749(3) 0.4603(3) 0.0240(10) Uani 1 1 d . . . H33A H 0.7536 0.2280 0.5207 0.029 Uiso 1 1 calc R . . H33B H 0.7011 0.3450 0.4794 0.029 Uiso 1 1 calc R . . C34 C 0.6217(4) 0.1343(3) 0.4333(3) 0.0200(9) Uani 1 1 d . . . H34A H 0.6297 0.1023 0.5041 0.024 Uiso 1 1 calc R . . H34B H 0.6948 0.1052 0.3938 0.024 Uiso 1 1 calc R . . C35 C 0.5028(3) 0.1152(3) 0.3917(3) 0.0169(9) Uani 1 1 d . . . H35A H 0.5064 0.0408 0.3882 0.020 Uiso 1 1 calc R . . H35B H 0.4313 0.1369 0.4365 0.020 Uiso 1 1 calc R . . C36 C 0.5463(4) 0.1195(3) 0.2126(3) 0.0172(9) Uani 1 1 d . . . H36A H 0.4931 0.0722 0.1920 0.021 Uiso 1 1 calc R . . H36B H 0.6270 0.0790 0.2344 0.021 Uiso 1 1 calc R . . C37 C 0.5668(4) 0.2013(3) 0.1265(3) 0.0167(9) Uani 1 1 d . . . H37A H 0.6110 0.1687 0.0702 0.020 Uiso 1 1 calc R . . H37B H 0.4851 0.2382 0.1025 0.020 Uiso 1 1 calc R . . Li1 Li 0.5425(6) 0.3218(5) 0.2819(5) 0.0211(15) Uani 1 1 d . . . O2 O 0.6145(2) 0.24287(19) 0.4264(2) 0.0201(6) Uani 1 1 d . . . O3 O 0.7716(3) 0.3405(2) 0.2950(2) 0.0245(7) Uani 1 1 d . . . O4 O 0.6390(2) 0.27334(18) 0.15686(19) 0.0162(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0158(3) 0.0121(3) 0.0106(3) -0.0019(2) -0.0003(2) -0.0043(2) N1 0.0152(17) 0.0175(17) 0.0130(18) -0.0025(14) 0.0009(14) 0.0020(13) N2 0.0162(17) 0.0134(16) 0.0089(16) -0.0052(13) 0.0022(14) -0.0008(13) N3 0.0146(17) 0.0141(16) 0.0153(18) 0.0011(14) -0.0034(14) -0.0021(13) O1 0.0168(14) 0.0140(13) 0.0112(14) -0.0008(11) 0.0002(11) -0.0006(10) C1 0.0131(19) 0.0138(19) 0.0090(19) -0.0033(16) 0.0000(16) -0.0011(15) C2 0.015(2) 0.0090(18) 0.014(2) -0.0003(15) -0.0001(16) -0.0029(15) C3 0.018(2) 0.018(2) 0.038(3) -0.0027(19) -0.004(2) -0.0055(17) C4 0.026(2) 0.016(2) 0.026(2) -0.0046(18) -0.0034(19) -0.0083(17) C5 0.024(2) 0.014(2) 0.023(2) 0.0018(17) -0.0018(19) -0.0100(17) C6 0.013(2) 0.0154(19) 0.017(2) -0.0012(16) -0.0024(17) -0.0013(15) C7 0.021(2) 0.017(2) 0.041(3) -0.003(2) -0.002(2) 0.0017(17) C8 0.028(2) 0.029(2) 0.017(2) 0.0009(18) -0.0068(19) -0.0126(19) C9 0.012(2) 0.020(2) 0.023(2) 0.0008(18) -0.0035(17) -0.0024(16) C10 0.012(2) 0.0120(19) 0.015(2) 0.0010(16) -0.0037(17) 0.0029(15) C11 0.013(2) 0.018(2) 0.015(2) -0.0037(16) 0.0012(17) -0.0027(15) C12 0.027(2) 0.016(2) 0.015(2) -0.0039(17) 0.0045(18) -0.0015(17) C13 0.021(2) 0.029(2) 0.032(3) -0.014(2) -0.001(2) -0.0052(18) C14 0.029(2) 0.021(2) 0.016(2) -0.0069(18) -0.0010(19) -0.0031(18) C15 0.020(2) 0.018(2) 0.010(2) -0.0013(16) 0.0005(17) -0.0005(16) C16 0.031(2) 0.020(2) 0.016(2) 0.0012(18) -0.0018(19) 0.0029(18) C17 0.022(2) 0.023(2) 0.016(2) -0.0020(18) 0.0054(18) -0.0016(17) C18 0.028(2) 0.019(2) 0.019(2) 0.0003(18) 0.0009(19) -0.0028(18) C19 0.0081(19) 0.0144(19) 0.017(2) -0.0042(16) 0.0008(16) 0.0001(15) C20 0.017(2) 0.0149(19) 0.018(2) -0.0035(16) 0.0022(17) -0.0048(16) C21 0.030(2) 0.018(2) 0.022(2) 0.0041(18) -0.0025(19) -0.0107(18) C22 0.019(2) 0.026(2) 0.036(3) 0.003(2) 0.005(2) -0.0051(18) C23 0.037(3) 0.013(2) 0.032(3) -0.0057(19) -0.008(2) -0.0035(18) C24 0.022(2) 0.016(2) 0.013(2) -0.0059(16) -0.0027(17) -0.0026(16) C25 0.027(2) 0.030(2) 0.014(2) -0.0008(18) -0.0039(19) -0.0103(19) C26 0.034(3) 0.041(3) 0.019(2) -0.007(2) -0.001(2) 0.007(2) C27 0.031(3) 0.032(2) 0.020(2) -0.001(2) -0.008(2) -0.011(2) C30 0.015(2) 0.026(2) 0.017(2) -0.0059(18) 0.0019(18) -0.0008(17) C31 0.016(2) 0.034(2) 0.019(2) 0.0034(19) -0.0047(18) -0.0079(18) C32 0.022(2) 0.028(2) 0.020(2) 0.0006(19) -0.0114(19) -0.0053(18) C33 0.021(2) 0.033(2) 0.019(2) -0.0058(19) -0.0061(19) -0.0022(18) C34 0.023(2) 0.016(2) 0.019(2) 0.0036(17) -0.0068(18) 0.0028(17) C35 0.016(2) 0.017(2) 0.017(2) -0.0005(17) 0.0017(17) -0.0035(16) C36 0.019(2) 0.0151(19) 0.017(2) -0.0051(17) 0.0023(18) 0.0006(16) C37 0.016(2) 0.018(2) 0.017(2) -0.0056(17) -0.0005(17) -0.0045(16) Li1 0.024(4) 0.020(3) 0.017(4) 0.003(3) -0.006(3) -0.002(3) O2 0.0169(15) 0.0209(14) 0.0242(16) -0.0080(12) -0.0060(12) -0.0019(11) O3 0.0314(17) 0.0240(15) 0.0174(16) -0.0017(12) -0.0084(13) 0.0000(12) O4 0.0146(14) 0.0167(14) 0.0183(15) -0.0030(11) -0.0012(12) -0.0047(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 N1 1.875(3) . ? Co1 N3 1.882(3) . ? Co1 N2 2.019(3) . ? Co1 O1 2.391(2) . ? N1 C10 1.256(5) . ? N2 C1 1.269(4) . ? N2 Li1 2.024(7) . ? N3 C19 1.255(5) . ? O1 C35 1.434(4) . ? O1 C36 1.446(4) . ? O1 Li1 2.159(7) . ? C1 C6 1.576(5) . ? C1 C2 1.585(5) . ? C2 C3 1.528(5) . ? C2 C5 1.534(5) . ? C2 C4 1.541(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C9 1.535(5) . ? C6 C8 1.538(5) . ? C6 C7 1.540(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.572(5) . ? C10 C11 1.591(5) . ? C11 C12 1.529(5) . ? C11 C13 1.534(5) . ? C11 C14 1.536(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C18 1.533(5) . ? C15 C16 1.539(5) . ? C15 C17 1.550(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.579(5) . ? C19 C24 1.580(5) . ? C20 C21 1.531(5) . ? C20 C23 1.534(5) . ? C20 C22 1.535(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.525(5) . ? C24 C27 1.536(6) . ? C24 C26 1.536(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C30 O4 1.430(4) . ? C30 C31 1.496(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O3 1.421(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 O3 1.425(5) . ? C32 C33 1.510(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 O2 1.429(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O2 1.421(4) . ? C34 C35 1.503(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.506(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O4 1.438(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? Li1 O4 2.063(7) . ? Li1 O2 2.196(7) . ? Li1 O3 2.554(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N3 130.26(13) . . ? N1 Co1 N2 111.49(13) . . ? N3 Co1 N2 118.19(12) . . ? N1 Co1 O1 96.38(11) . . ? N3 Co1 O1 89.77(11) . . ? N2 Co1 O1 85.54(10) . . ? C10 N1 Co1 163.5(3) . . ? C1 N2 Co1 129.9(3) . . ? C1 N2 Li1 132.9(3) . . ? Co1 N2 Li1 97.2(2) . . ? C19 N3 Co1 161.6(3) . . ? C35 O1 C36 114.8(3) . . ? C35 O1 Li1 112.3(3) . . ? C36 O1 Li1 108.6(3) . . ? C35 O1 Co1 114.1(2) . . ? C36 O1 Co1 119.1(2) . . ? Li1 O1 Co1 83.40(19) . . ? N2 C1 C6 122.7(3) . . ? N2 C1 C2 119.1(3) . . ? C6 C1 C2 118.2(3) . . ? C3 C2 C5 105.8(3) . . ? C3 C2 C4 106.5(3) . . ? C5 C2 C4 109.4(3) . . ? C3 C2 C1 109.1(3) . . ? C5 C2 C1 115.4(3) . . ? C4 C2 C1 110.2(3) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C9 C6 C8 106.3(3) . . ? C9 C6 C7 105.6(3) . . ? C8 C6 C7 109.4(3) . . ? C9 C6 C1 111.0(3) . . ? C8 C6 C1 108.8(3) . . ? C7 C6 C1 115.2(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C15 120.6(3) . . ? N1 C10 C11 119.2(3) . . ? C15 C10 C11 120.1(3) . . ? C12 C11 C13 108.3(3) . . ? C12 C11 C14 107.6(3) . . ? C13 C11 C14 108.1(3) . . ? C12 C11 C10 106.7(3) . . ? C13 C11 C10 106.3(3) . . ? C14 C11 C10 119.4(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C16 107.0(3) . . ? C18 C15 C17 107.4(3) . . ? C16 C15 C17 110.1(3) . . ? C18 C15 C10 108.8(3) . . ? C16 C15 C10 110.0(3) . . ? C17 C15 C10 113.3(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 120.6(3) . . ? N3 C19 C24 119.4(3) . . ? C20 C19 C24 120.0(3) . . ? C21 C20 C23 105.5(3) . . ? C21 C20 C22 107.5(3) . . ? C23 C20 C22 109.8(3) . . ? C21 C20 C19 108.8(3) . . ? C23 C20 C19 118.5(3) . . ? C22 C20 C19 106.4(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C27 105.9(3) . . ? C25 C24 C26 107.2(3) . . ? C27 C24 C26 110.0(3) . . ? C25 C24 C19 108.8(3) . . ? C27 C24 C19 113.1(3) . . ? C26 C24 C19 111.4(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C30 C31 107.3(3) . . ? O4 C30 H30A 110.3 . . ? C31 C30 H30A 110.3 . . ? O4 C30 H30B 110.3 . . ? C31 C30 H30B 110.3 . . ? H30A C30 H30B 108.5 . . ? O3 C31 C30 110.8(3) . . ? O3 C31 H31A 109.5 . . ? C30 C31 H31A 109.5 . . ? O3 C31 H31B 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? O3 C32 C33 105.6(3) . . ? O3 C32 H32A 110.6 . . ? C33 C32 H32A 110.6 . . ? O3 C32 H32B 110.6 . . ? C33 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? O2 C33 C32 111.1(3) . . ? O2 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? O2 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? O2 C34 C35 106.2(3) . . ? O2 C34 H34A 110.5 . . ? C35 C34 H34A 110.5 . . ? O2 C34 H34B 110.5 . . ? C35 C34 H34B 110.5 . . ? H34A C34 H34B 108.7 . . ? O1 C35 C34 109.8(3) . . ? O1 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? O1 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? O1 C36 C37 106.9(3) . . ? O1 C36 H36A 110.3 . . ? C37 C36 H36A 110.3 . . ? O1 C36 H36B 110.3 . . ? C37 C36 H36B 110.3 . . ? H36A C36 H36B 108.6 . . ? O4 C37 C36 110.8(3) . . ? O4 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? O4 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? N2 Li1 O4 106.8(3) . . ? N2 Li1 O1 91.9(3) . . ? O4 Li1 O1 81.9(3) . . ? N2 Li1 O2 133.8(3) . . ? O4 Li1 O2 115.1(3) . . ? O1 Li1 O2 76.0(2) . . ? N2 Li1 O3 145.8(3) . . ? O4 Li1 O3 71.6(2) . . ? O1 Li1 O3 120.8(3) . . ? O2 Li1 O3 69.7(2) . . ? C34 O2 C33 113.6(3) . . ? C34 O2 Li1 112.1(3) . . ? C33 O2 Li1 116.6(3) . . ? C31 O3 C32 114.7(3) . . ? C31 O3 Li1 105.1(3) . . ? C32 O3 Li1 110.6(3) . . ? C30 O4 C37 115.0(3) . . ? C30 O4 Li1 119.8(3) . . ? C37 O4 Li1 103.9(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.288 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.069 data_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 921194' #TrackingRef 'web_deposit_cif_file_2_RichardLewis_1361299243.complex 3 final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H104 Co Li N4 O8' _chemical_formula_weight 979.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5073(4) _cell_length_b 13.5432(4) _cell_length_c 16.3252(5) _cell_angle_alpha 88.668(2) _cell_angle_beta 74.519(2) _cell_angle_gamma 89.944(2) _cell_volume 2877.23(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9027 _exptl_absorpt_correction_T_max 0.9336 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 31151 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 28.36 _reflns_number_total 14294 _reflns_number_gt 11106 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14294 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.29891(2) 0.25298(2) 0.258622(17) 0.01281(8) Uani 1 1 d . . . N1 N 0.30155(13) 0.38492(14) 0.22835(12) 0.0187(4) Uani 1 1 d . . . N2 N 0.42805(14) 0.25355(13) 0.27285(13) 0.0195(4) Uani 1 1 d . . . N3 N 0.30414(13) 0.12267(13) 0.22985(12) 0.0180(4) Uani 1 1 d . . . N4 N 0.15677(13) 0.25029(13) 0.30749(12) 0.0169(3) Uani 1 1 d . . . C1 C 0.29422(15) 0.47457(16) 0.24379(14) 0.0168(4) Uani 1 1 d . . . C2 C 0.26433(18) 0.51320(17) 0.33723(15) 0.0231(5) Uani 1 1 d . . . C3 C 0.1485(2) 0.5379(2) 0.36398(19) 0.0363(6) Uani 1 1 d . . . H3A H 0.1090 0.4816 0.3527 0.054 Uiso 1 1 calc R . . H3B H 0.1357 0.5960 0.3314 0.054 Uiso 1 1 calc R . . H3C H 0.1274 0.5519 0.4248 0.054 Uiso 1 1 calc R . . C4 C 0.3269(2) 0.6019(2) 0.35198(18) 0.0345(6) Uani 1 1 d . . . H4A H 0.3040 0.6201 0.4118 0.052 Uiso 1 1 calc R . . H4B H 0.3169 0.6578 0.3159 0.052 Uiso 1 1 calc R . . H4C H 0.3999 0.5846 0.3377 0.052 Uiso 1 1 calc R . . C5 C 0.2805(2) 0.42997(19) 0.39745(16) 0.0280(5) Uani 1 1 d . . . H5A H 0.2663 0.4546 0.4554 0.042 Uiso 1 1 calc R . . H5B H 0.3517 0.4072 0.3792 0.042 Uiso 1 1 calc R . . H5C H 0.2339 0.3750 0.3963 0.042 Uiso 1 1 calc R . . C6 C 0.31673(17) 0.54954(17) 0.16554(15) 0.0217(4) Uani 1 1 d . . . C7 C 0.4277(2) 0.58740(19) 0.14832(18) 0.0301(5) Uani 1 1 d . . . H7A H 0.4742 0.5312 0.1458 0.045 Uiso 1 1 calc R . . H7B H 0.4332 0.6307 0.1942 0.045 Uiso 1 1 calc R . . H7C H 0.4466 0.6244 0.0940 0.045 Uiso 1 1 calc R . . C8 C 0.2426(2) 0.63716(19) 0.17467(19) 0.0324(6) Uani 1 1 d . . . H8A H 0.2615 0.6788 0.1229 0.049 Uiso 1 1 calc R . . H8B H 0.2466 0.6761 0.2235 0.049 Uiso 1 1 calc R . . H8C H 0.1723 0.6125 0.1834 0.049 Uiso 1 1 calc R . . C9 C 0.3088(2) 0.49497(19) 0.08686(16) 0.0312(6) Uani 1 1 d . . . H9A H 0.2386 0.4699 0.0956 0.047 Uiso 1 1 calc R . . H9B H 0.3569 0.4396 0.0770 0.047 Uiso 1 1 calc R . . H9C H 0.3258 0.5403 0.0374 0.047 Uiso 1 1 calc R . . C10 C 0.52435(16) 0.25011(15) 0.25297(14) 0.0165(4) Uani 1 1 d . . . C11 C 0.57810(16) 0.25419(17) 0.32689(15) 0.0214(4) Uani 1 1 d . . . C12 C 0.4987(2) 0.2321(2) 0.41129(16) 0.0347(6) Uani 1 1 d . . . H12A H 0.4731 0.1644 0.4118 0.052 Uiso 1 1 calc R . . H12B H 0.4414 0.2785 0.4181 0.052 Uiso 1 1 calc R . . H12C H 0.5307 0.2394 0.4581 0.052 Uiso 1 1 calc R . . C13 C 0.6213(2) 0.3580(2) 0.3318(2) 0.0390(7) Uani 1 1 d . . . H13A H 0.5680 0.4072 0.3320 0.059 Uiso 1 1 calc R . . H13B H 0.6802 0.3704 0.2824 0.059 Uiso 1 1 calc R . . H13C H 0.6435 0.3628 0.3840 0.059 Uiso 1 1 calc R . . C14 C 0.66239(19) 0.1763(2) 0.32087(18) 0.0310(6) Uani 1 1 d . . . H14A H 0.6913 0.1816 0.3696 0.046 Uiso 1 1 calc R . . H14B H 0.7168 0.1874 0.2681 0.046 Uiso 1 1 calc R . . H14C H 0.6328 0.1102 0.3210 0.046 Uiso 1 1 calc R . . C15 C 0.58806(18) 0.24092(17) 0.15818(15) 0.0237(5) Uani 1 1 d . . . C16 C 0.6865(2) 0.3035(2) 0.1329(2) 0.0393(7) Uani 1 1 d . . . H16A H 0.7318 0.2837 0.1682 0.059 Uiso 1 1 calc R . . H16B H 0.6690 0.3734 0.1414 0.059 Uiso 1 1 calc R . . H16C H 0.7216 0.2933 0.0729 0.059 Uiso 1 1 calc R . . C17 C 0.5211(2) 0.2735(2) 0.10005(16) 0.0311(6) Uani 1 1 d . . . H17A H 0.5002 0.3423 0.1113 0.047 Uiso 1 1 calc R . . H17B H 0.4600 0.2312 0.1112 0.047 Uiso 1 1 calc R . . H17C H 0.5604 0.2680 0.0405 0.047 Uiso 1 1 calc R . . C18 C 0.6152(2) 0.1316(2) 0.14000(18) 0.0355(6) Uani 1 1 d . . . H18A H 0.6445 0.1238 0.0788 0.053 Uiso 1 1 calc R . . H18B H 0.5530 0.0910 0.1593 0.053 Uiso 1 1 calc R . . H18C H 0.6655 0.1105 0.1703 0.053 Uiso 1 1 calc R . . C19 C 0.30642(15) 0.03143(16) 0.24210(14) 0.0170(4) Uani 1 1 d . . . C20 C 0.31547(17) -0.03560(16) 0.16303(15) 0.0213(4) Uani 1 1 d . . . C21 C 0.2091(2) -0.0746(2) 0.1628(2) 0.0406(7) Uani 1 1 d . . . H21A H 0.1609 -0.0194 0.1688 0.061 Uiso 1 1 calc R . . H21B H 0.1848 -0.1219 0.2103 0.061 Uiso 1 1 calc R . . H21C H 0.2135 -0.1074 0.1091 0.061 Uiso 1 1 calc R . . C22 C 0.39092(19) -0.12210(18) 0.15598(17) 0.0270(5) Uani 1 1 d . . . H22A H 0.3682 -0.1661 0.2060 0.041 Uiso 1 1 calc R . . H22B H 0.4597 -0.0964 0.1529 0.041 Uiso 1 1 calc R . . H22C H 0.3929 -0.1589 0.1046 0.041 Uiso 1 1 calc R . . C23 C 0.3556(2) 0.0277(2) 0.08170(16) 0.0334(6) Uani 1 1 d . . . H23A H 0.3607 -0.0131 0.0320 0.050 Uiso 1 1 calc R . . H23B H 0.4236 0.0542 0.0801 0.050 Uiso 1 1 calc R . . H23C H 0.3081 0.0823 0.0811 0.050 Uiso 1 1 calc R . . C24 C 0.30130(19) -0.01540(18) 0.33186(15) 0.0247(5) Uani 1 1 d . . . C25 C 0.2589(2) 0.0615(2) 0.39964(15) 0.0286(5) Uani 1 1 d . . . H25A H 0.2542 0.0325 0.4561 0.043 Uiso 1 1 calc R . . H25B H 0.1905 0.0822 0.3963 0.043 Uiso 1 1 calc R . . H25C H 0.3050 0.1190 0.3898 0.043 Uiso 1 1 calc R . . C26 C 0.2313(2) -0.1071(2) 0.3554(2) 0.0407(7) Uani 1 1 d . . . H26A H 0.2550 -0.1576 0.3126 0.061 Uiso 1 1 calc R . . H26B H 0.1606 -0.0887 0.3573 0.061 Uiso 1 1 calc R . . H26C H 0.2340 -0.1334 0.4112 0.061 Uiso 1 1 calc R . . C27 C 0.4099(2) -0.0415(2) 0.33737(17) 0.0375(7) Uani 1 1 d . . . H27A H 0.4557 0.0153 0.3177 0.056 Uiso 1 1 calc R . . H27B H 0.4353 -0.0980 0.3015 0.056 Uiso 1 1 calc R . . H27C H 0.4081 -0.0584 0.3964 0.056 Uiso 1 1 calc R . . C28 C 0.06849(15) 0.25213(15) 0.29644(13) 0.0149(4) Uani 1 1 d . . . C29 C 0.04713(16) 0.26574(17) 0.20691(14) 0.0194(4) Uani 1 1 d . . . C30 C 0.14577(17) 0.24586(18) 0.13762(14) 0.0214(4) Uani 1 1 d . . . H30A H 0.1320 0.2516 0.0817 0.032 Uiso 1 1 calc R . . H30B H 0.1700 0.1791 0.1458 0.032 Uiso 1 1 calc R . . H30C H 0.1985 0.2941 0.1409 0.032 Uiso 1 1 calc R . . C31 C 0.0174(2) 0.3739(2) 0.19402(18) 0.0374(7) Uani 1 1 d . . . H31A H 0.0704 0.4182 0.2037 0.056 Uiso 1 1 calc R . . H31B H -0.0486 0.3883 0.2344 0.056 Uiso 1 1 calc R . . H31C H 0.0117 0.3840 0.1358 0.056 Uiso 1 1 calc R . . C32 C -0.03464(19) 0.1956(2) 0.19161(16) 0.0337(6) Uani 1 1 d . . . H32A H -0.0440 0.2089 0.1349 0.051 Uiso 1 1 calc R . . H32B H -0.0998 0.2059 0.2346 0.051 Uiso 1 1 calc R . . H32C H -0.0125 0.1271 0.1956 0.051 Uiso 1 1 calc R . . C33 C -0.02364(16) 0.23799(17) 0.37868(14) 0.0192(4) Uani 1 1 d . . . C34 C -0.11549(19) 0.3065(2) 0.38301(16) 0.0314(6) Uani 1 1 d . . . H34A H -0.1693 0.2921 0.4355 0.047 Uiso 1 1 calc R . . H34B H -0.1425 0.2957 0.3339 0.047 Uiso 1 1 calc R . . H34C H -0.0932 0.3754 0.3825 0.047 Uiso 1 1 calc R . . C35 C -0.0582(2) 0.1295(2) 0.38673(17) 0.0333(6) Uani 1 1 d . . . H35A H -0.1073 0.1175 0.4422 0.050 Uiso 1 1 calc R . . H35B H 0.0017 0.0868 0.3816 0.050 Uiso 1 1 calc R . . H35C H -0.0909 0.1149 0.3415 0.050 Uiso 1 1 calc R . . C36 C 0.01383(18) 0.2596(2) 0.45679(14) 0.0257(5) Uani 1 1 d . . . H36A H 0.0358 0.3288 0.4544 0.039 Uiso 1 1 calc R . . H36B H 0.0719 0.2166 0.4578 0.039 Uiso 1 1 calc R . . H36C H -0.0421 0.2474 0.5083 0.039 Uiso 1 1 calc R . . C37 C 0.79104(18) 0.55617(16) 0.34306(15) 0.0223(4) Uani 1 1 d . . . H37A H 0.8280 0.5150 0.2953 0.027 Uiso 1 1 calc R . . H37B H 0.7551 0.5115 0.3905 0.027 Uiso 1 1 calc R . . C38 C 0.86783(19) 0.61983(18) 0.37165(15) 0.0250(5) Uani 1 1 d . . . H38A H 0.8324 0.6589 0.4214 0.030 Uiso 1 1 calc R . . H38B H 0.9202 0.5780 0.3876 0.030 Uiso 1 1 calc R . . C39 C 0.97271(17) 0.76121(17) 0.32308(15) 0.0223(5) Uani 1 1 d . . . H39A H 1.0235 0.7864 0.2713 0.027 Uiso 1 1 calc R . . H39B H 1.0107 0.7357 0.3632 0.027 Uiso 1 1 calc R . . C40 C 0.90300(19) 0.84506(18) 0.36364(16) 0.0258(5) Uani 1 1 d . . . H40A H 0.8543 0.8220 0.4174 0.031 Uiso 1 1 calc R . . H40B H 0.9441 0.9004 0.3761 0.031 Uiso 1 1 calc R . . C41 C 0.76207(18) 0.93512(17) 0.33868(15) 0.0231(5) Uani 1 1 d . . . H41A H 0.7465 0.9767 0.2931 0.028 Uiso 1 1 calc R . . H41B H 0.7776 0.9794 0.3811 0.028 Uiso 1 1 calc R . . C42 C 0.66859(18) 0.87107(18) 0.38118(15) 0.0245(5) Uani 1 1 d . . . H42A H 0.6813 0.8321 0.4294 0.029 Uiso 1 1 calc R . . H42B H 0.6074 0.9128 0.4028 0.029 Uiso 1 1 calc R . . C43 C 0.58190(16) 0.72968(17) 0.34956(14) 0.0217(4) Uani 1 1 d . . . H43A H 0.5539 0.7056 0.3034 0.026 Uiso 1 1 calc R . . H43B H 0.5240 0.7546 0.3952 0.026 Uiso 1 1 calc R . . C44 C 0.63389(19) 0.64497(18) 0.38457(15) 0.0250(5) Uani 1 1 d . . . H44A H 0.6585 0.6670 0.4332 0.030 Uiso 1 1 calc R . . H44B H 0.5852 0.5893 0.4041 0.030 Uiso 1 1 calc R . . C45 C 0.95678(19) 0.89208(19) 0.10417(16) 0.0275(5) Uani 1 1 d . . . H45A H 1.0173 0.9071 0.0559 0.033 Uiso 1 1 calc R . . H45B H 0.9579 0.9376 0.1505 0.033 Uiso 1 1 calc R . . C46 C 0.8589(2) 0.9084(2) 0.07602(16) 0.0296(5) Uani 1 1 d . . . H46A H 0.8528 0.9787 0.0601 0.036 Uiso 1 1 calc R . . H46B H 0.8594 0.8676 0.0264 0.036 Uiso 1 1 calc R . . C47 C 0.68095(17) 0.86967(18) 0.12554(15) 0.0232(5) Uani 1 1 d . . . H47A H 0.6761 0.9207 0.0824 0.028 Uiso 1 1 calc R . . H47B H 0.6236 0.8797 0.1769 0.028 Uiso 1 1 calc R . . C48 C 0.67154(18) 0.76787(18) 0.09104(15) 0.0238(5) Uani 1 1 d . . . H48A H 0.6031 0.7592 0.0808 0.029 Uiso 1 1 calc R . . H48B H 0.7248 0.7588 0.0369 0.029 Uiso 1 1 calc R . . C49 C 0.70222(18) 0.60020(18) 0.12558(15) 0.0235(5) Uani 1 1 d . . . H49A H 0.6612 0.5869 0.0850 0.028 Uiso 1 1 calc R . . H49B H 0.6795 0.5536 0.1746 0.028 Uiso 1 1 calc R . . C50 C 0.81497(19) 0.58392(19) 0.08269(15) 0.0253(5) Uani 1 1 d . . . H50A H 0.8273 0.5139 0.0669 0.030 Uiso 1 1 calc R . . H50B H 0.8372 0.6259 0.0305 0.030 Uiso 1 1 calc R . . C51 C 0.97726(18) 0.62249(19) 0.10640(16) 0.0263(5) Uani 1 1 d . . . H51A H 1.0019 0.5728 0.0621 0.032 Uiso 1 1 calc R . . H51B H 1.0137 0.6115 0.1510 0.032 Uiso 1 1 calc R . . C52 C 1.00195(18) 0.7251(2) 0.06748(15) 0.0277(5) Uani 1 1 d . . . H52A H 1.0771 0.7339 0.0449 0.033 Uiso 1 1 calc R . . H52B H 0.9695 0.7357 0.0203 0.033 Uiso 1 1 calc R . . Li1 Li 0.8011(3) 0.7453(3) 0.2282(3) 0.0251(8) Uani 1 1 d . . . O1 O 0.96255(14) 0.79307(13) 0.13302(11) 0.0276(4) Uani 1 1 d . . . O2 O 0.91453(13) 0.68346(12) 0.30143(10) 0.0233(3) Uani 1 1 d . . . O3 O 0.84907(13) 0.87564(13) 0.30361(11) 0.0243(3) Uani 1 1 d . . . O4 O 0.77582(13) 0.88025(13) 0.14646(11) 0.0253(4) Uani 1 1 d . . . O5 O 0.71798(12) 0.61556(12) 0.31677(10) 0.0237(3) Uani 1 1 d . . . O6 O 0.87019(12) 0.60990(13) 0.14246(10) 0.0256(4) Uani 1 1 d . . . O7 O 0.65322(13) 0.80747(12) 0.31763(10) 0.0232(3) Uani 1 1 d . . . O8 O 0.68511(13) 0.69878(12) 0.15405(10) 0.0235(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01121(13) 0.01195(14) 0.01575(14) -0.00082(9) -0.00438(10) 0.00039(9) N1 0.0126(8) 0.0172(9) 0.0263(10) 0.0017(7) -0.0052(7) 0.0004(6) N2 0.0162(8) 0.0133(9) 0.0295(10) -0.0004(7) -0.0070(7) -0.0001(6) N3 0.0118(8) 0.0155(9) 0.0268(10) -0.0026(7) -0.0054(7) 0.0009(6) N4 0.0137(8) 0.0137(8) 0.0225(9) -0.0012(7) -0.0036(7) 0.0001(6) C1 0.0138(9) 0.0156(10) 0.0216(10) 0.0009(8) -0.0059(8) 0.0005(7) C2 0.0241(11) 0.0202(11) 0.0246(11) -0.0050(9) -0.0058(9) 0.0023(9) C3 0.0251(12) 0.0395(16) 0.0397(15) -0.0056(12) -0.0006(11) 0.0093(11) C4 0.0431(15) 0.0274(13) 0.0353(14) -0.0067(11) -0.0140(12) -0.0058(11) C5 0.0346(13) 0.0271(13) 0.0217(11) -0.0023(9) -0.0061(10) 0.0001(10) C6 0.0224(11) 0.0165(10) 0.0286(12) 0.0041(8) -0.0112(9) -0.0014(8) C7 0.0284(12) 0.0259(13) 0.0358(14) 0.0103(10) -0.0092(10) -0.0084(10) C8 0.0339(13) 0.0203(12) 0.0478(16) 0.0038(11) -0.0194(12) 0.0040(10) C9 0.0455(15) 0.0252(13) 0.0258(12) 0.0055(10) -0.0152(11) -0.0064(11) C10 0.0145(9) 0.0137(10) 0.0222(10) -0.0018(8) -0.0063(8) 0.0004(7) C11 0.0154(10) 0.0243(11) 0.0263(11) -0.0057(9) -0.0083(8) 0.0015(8) C12 0.0302(13) 0.0519(18) 0.0229(12) -0.0036(11) -0.0087(10) 0.0100(12) C13 0.0437(16) 0.0276(14) 0.0554(18) -0.0111(12) -0.0293(14) -0.0014(11) C14 0.0220(11) 0.0315(14) 0.0427(15) -0.0027(11) -0.0143(10) 0.0065(10) C15 0.0236(11) 0.0211(11) 0.0233(11) -0.0022(9) -0.0007(9) 0.0031(9) C16 0.0298(14) 0.0393(16) 0.0393(16) 0.0064(12) 0.0066(11) -0.0037(11) C17 0.0372(14) 0.0335(14) 0.0214(12) 0.0004(10) -0.0056(10) 0.0058(11) C18 0.0465(16) 0.0280(14) 0.0298(13) -0.0098(10) -0.0057(12) 0.0117(12) C19 0.0117(9) 0.0161(10) 0.0233(10) -0.0027(8) -0.0045(8) -0.0002(7) C20 0.0200(10) 0.0171(11) 0.0288(12) -0.0064(9) -0.0098(9) 0.0035(8) C21 0.0280(13) 0.0334(15) 0.068(2) -0.0211(14) -0.0251(13) 0.0039(11) C22 0.0264(12) 0.0211(12) 0.0338(13) -0.0079(10) -0.0080(10) 0.0062(9) C23 0.0489(16) 0.0284(13) 0.0241(12) -0.0073(10) -0.0115(11) 0.0112(11) C24 0.0258(11) 0.0217(11) 0.0250(12) 0.0009(9) -0.0039(9) 0.0055(9) C25 0.0324(13) 0.0316(13) 0.0200(11) -0.0009(9) -0.0042(9) 0.0079(10) C26 0.0448(16) 0.0251(14) 0.0409(16) 0.0076(11) 0.0072(13) -0.0014(12) C27 0.0331(14) 0.0540(18) 0.0262(13) 0.0007(12) -0.0094(11) 0.0183(13) C28 0.0128(9) 0.0146(9) 0.0174(10) -0.0013(7) -0.0038(7) 0.0004(7) C29 0.0167(10) 0.0240(11) 0.0176(10) -0.0008(8) -0.0049(8) 0.0028(8) C30 0.0195(10) 0.0292(12) 0.0153(10) -0.0002(8) -0.0042(8) 0.0013(9) C31 0.0488(17) 0.0349(15) 0.0283(13) 0.0025(11) -0.0102(12) 0.0209(13) C32 0.0233(12) 0.0588(18) 0.0203(12) -0.0037(11) -0.0079(9) -0.0073(11) C33 0.0137(9) 0.0256(11) 0.0173(10) -0.0028(8) -0.0025(7) -0.0004(8) C34 0.0192(11) 0.0483(16) 0.0257(12) -0.0063(11) -0.0039(9) 0.0101(10) C35 0.0319(13) 0.0337(14) 0.0284(13) -0.0001(10) 0.0019(10) -0.0132(11) C36 0.0206(11) 0.0394(14) 0.0168(10) -0.0043(9) -0.0042(8) 0.0001(9) C37 0.0287(11) 0.0161(10) 0.0224(11) 0.0005(8) -0.0078(9) 0.0022(9) C38 0.0310(12) 0.0249(12) 0.0212(11) 0.0021(9) -0.0108(9) 0.0030(9) C39 0.0199(10) 0.0263(12) 0.0236(11) -0.0020(9) -0.0107(9) -0.0016(9) C40 0.0304(12) 0.0234(12) 0.0279(12) -0.0016(9) -0.0149(10) -0.0011(9) C41 0.0269(11) 0.0174(11) 0.0254(11) -0.0025(8) -0.0075(9) 0.0035(9) C42 0.0254(11) 0.0247(12) 0.0227(11) -0.0053(9) -0.0049(9) 0.0045(9) C43 0.0150(10) 0.0278(12) 0.0206(11) -0.0006(9) -0.0018(8) -0.0014(8) C44 0.0268(12) 0.0249(12) 0.0205(11) 0.0012(9) -0.0018(9) -0.0016(9) C45 0.0275(12) 0.0282(13) 0.0258(12) 0.0057(10) -0.0058(9) -0.0089(10) C46 0.0320(13) 0.0306(13) 0.0247(12) 0.0092(10) -0.0054(10) -0.0044(10) C47 0.0202(10) 0.0287(12) 0.0221(11) 0.0018(9) -0.0084(8) 0.0043(9) C48 0.0216(11) 0.0323(13) 0.0193(11) 0.0007(9) -0.0089(8) 0.0032(9) C49 0.0253(11) 0.0244(12) 0.0211(11) -0.0037(9) -0.0067(9) -0.0025(9) C50 0.0299(12) 0.0261(12) 0.0201(11) -0.0048(9) -0.0069(9) 0.0011(9) C51 0.0198(11) 0.0328(13) 0.0258(12) -0.0033(10) -0.0048(9) 0.0060(9) C52 0.0188(11) 0.0412(15) 0.0204(11) -0.0001(10) -0.0010(9) 0.0002(10) Li1 0.0224(19) 0.032(2) 0.0220(19) 0.0009(16) -0.0077(15) -0.0001(16) O1 0.0306(9) 0.0299(9) 0.0223(8) 0.0011(7) -0.0074(7) -0.0007(7) O2 0.0273(8) 0.0223(8) 0.0213(8) 0.0005(6) -0.0083(6) -0.0045(6) O3 0.0228(8) 0.0267(9) 0.0242(8) 0.0005(7) -0.0077(6) 0.0038(6) O4 0.0225(8) 0.0320(9) 0.0214(8) 0.0033(7) -0.0062(6) -0.0039(7) O5 0.0222(8) 0.0272(9) 0.0208(8) -0.0016(6) -0.0041(6) 0.0043(6) O6 0.0202(8) 0.0353(10) 0.0216(8) -0.0022(7) -0.0058(6) -0.0008(7) O7 0.0256(8) 0.0236(8) 0.0203(8) -0.0009(6) -0.0056(6) -0.0028(6) O8 0.0272(8) 0.0242(9) 0.0194(8) -0.0014(6) -0.0067(6) 0.0029(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 Co1 N2 1.8201(18) . ? Co1 N3 1.8332(18) . ? Co1 N1 1.8407(19) . ? Co1 N4 1.8722(18) . ? N1 C1 1.244(3) . ? N2 C10 1.255(3) . ? N3 C19 1.249(3) . ? N4 C28 1.253(3) . ? C1 C2 1.572(3) . ? C1 C6 1.577(3) . ? C2 C4 1.530(3) . ? C2 C5 1.532(3) . ? C2 C3 1.546(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C9 1.525(3) . ? C6 C8 1.536(3) . ? C6 C7 1.536(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.565(3) . ? C10 C11 1.568(3) . ? C11 C12 1.527(3) . ? C11 C13 1.535(3) . ? C11 C14 1.537(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.533(4) . ? C15 C17 1.533(4) . ? C15 C18 1.541(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.568(3) . ? C19 C20 1.573(3) . ? C20 C21 1.533(3) . ? C20 C23 1.534(4) . ? C20 C22 1.538(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.533(3) . ? C24 C27 1.534(3) . ? C24 C26 1.539(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.570(3) . ? C28 C33 1.576(3) . ? C29 C30 1.528(3) . ? C29 C32 1.531(3) . ? C29 C31 1.543(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.526(3) . ? C33 C35 1.534(3) . ? C33 C34 1.536(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O5 1.419(3) . ? C37 C38 1.522(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 O2 1.423(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O2 1.421(3) . ? C39 C40 1.521(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O3 1.423(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O3 1.420(3) . ? C41 C42 1.528(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O7 1.421(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O7 1.421(3) . ? C43 C44 1.523(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O5 1.422(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O1 1.420(3) . ? C45 C46 1.526(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 O4 1.421(3) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O4 1.420(3) . ? C47 C48 1.519(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 O8 1.422(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 O8 1.422(3) . ? C49 C50 1.515(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 O6 1.427(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O6 1.417(3) . ? C51 C52 1.515(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 O1 1.420(3) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? Li1 O7 2.308(4) . ? Li1 O8 2.317(4) . ? Li1 O4 2.317(4) . ? Li1 O2 2.325(4) . ? Li1 O5 2.336(5) . ? Li1 O3 2.362(5) . ? Li1 O6 2.369(5) . ? Li1 O1 2.395(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 N2 Co1 N3 93.89(8) . . ? N2 Co1 N1 94.35(8) . . ? N3 Co1 N1 150.32(9) . . ? N2 Co1 N4 148.70(9) . . ? N3 Co1 N4 93.66(8) . . ? N1 Co1 N4 93.94(8) . . ? C1 N1 Co1 153.71(18) . . ? C10 N2 Co1 158.31(18) . . ? C19 N3 Co1 156.16(18) . . ? C28 N4 Co1 147.75(17) . . ? N1 C1 C2 122.0(2) . . ? N1 C1 C6 117.5(2) . . ? C2 C1 C6 120.50(18) . . ? C4 C2 C5 106.8(2) . . ? C4 C2 C3 109.9(2) . . ? C5 C2 C3 106.6(2) . . ? C4 C2 C1 115.1(2) . . ? C5 C2 C1 108.83(18) . . ? C3 C2 C1 109.3(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C9 C6 C8 106.3(2) . . ? C9 C6 C7 107.3(2) . . ? C8 C6 C7 110.0(2) . . ? C9 C6 C1 108.96(19) . . ? C8 C6 C1 115.2(2) . . ? C7 C6 C1 108.81(18) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C15 121.2(2) . . ? N2 C10 C11 117.4(2) . . ? C15 C10 C11 121.39(18) . . ? C12 C11 C13 107.4(2) . . ? C12 C11 C14 105.5(2) . . ? C13 C11 C14 110.4(2) . . ? C12 C11 C10 109.09(18) . . ? C13 C11 C10 110.5(2) . . ? C14 C11 C10 113.67(19) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 107.2(2) . . ? C16 C15 C18 109.4(2) . . ? C17 C15 C18 107.1(2) . . ? C16 C15 C10 114.8(2) . . ? C17 C15 C10 108.93(18) . . ? C18 C15 C10 109.18(19) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C24 122.0(2) . . ? N3 C19 C20 117.1(2) . . ? C24 C19 C20 120.85(18) . . ? C21 C20 C23 107.4(2) . . ? C21 C20 C22 109.8(2) . . ? C23 C20 C22 105.8(2) . . ? C21 C20 C19 109.91(19) . . ? C23 C20 C19 108.70(19) . . ? C22 C20 C19 114.89(19) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C27 107.1(2) . . ? C25 C24 C26 107.0(2) . . ? C27 C24 C26 109.6(2) . . ? C25 C24 C19 108.83(18) . . ? C27 C24 C19 109.74(19) . . ? C26 C24 C19 114.3(2) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C29 123.63(19) . . ? N4 C28 C33 116.18(19) . . ? C29 C28 C33 120.19(17) . . ? C30 C29 C32 106.46(19) . . ? C30 C29 C31 106.7(2) . . ? C32 C29 C31 110.1(2) . . ? C30 C29 C28 109.25(17) . . ? C32 C29 C28 114.31(19) . . ? C31 C29 C28 109.65(19) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 107.0(2) . . ? C36 C33 C34 106.11(19) . . ? C35 C33 C34 110.5(2) . . ? C36 C33 C28 109.09(17) . . ? C35 C33 C28 108.90(18) . . ? C34 C33 C28 114.94(19) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O5 C37 C38 110.95(18) . . ? O5 C37 H37A 109.4 . . ? C38 C37 H37A 109.4 . . ? O5 C37 H37B 109.4 . . ? C38 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? O2 C38 C37 106.39(18) . . ? O2 C38 H38A 110.5 . . ? C37 C38 H38A 110.5 . . ? O2 C38 H38B 110.5 . . ? C37 C38 H38B 110.5 . . ? H38A C38 H38B 108.6 . . ? O2 C39 C40 110.73(19) . . ? O2 C39 H39A 109.5 . . ? C40 C39 H39A 109.5 . . ? O2 C39 H39B 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? O3 C40 C39 106.21(19) . . ? O3 C40 H40A 110.5 . . ? C39 C40 H40A 110.5 . . ? O3 C40 H40B 110.5 . . ? C39 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? O3 C41 C42 110.87(18) . . ? O3 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? O7 C42 C41 106.29(18) . . ? O7 C42 H42A 110.5 . . ? C41 C42 H42A 110.5 . . ? O7 C42 H42B 110.5 . . ? C41 C42 H42B 110.5 . . ? H42A C42 H42B 108.7 . . ? O7 C43 C44 110.38(18) . . ? O7 C43 H43A 109.6 . . ? C44 C43 H43A 109.6 . . ? O7 C43 H43B 109.6 . . ? C44 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? O5 C44 C43 106.38(18) . . ? O5 C44 H44A 110.5 . . ? C43 C44 H44A 110.5 . . ? O5 C44 H44B 110.5 . . ? C43 C44 H44B 110.5 . . ? H44A C44 H44B 108.6 . . ? O1 C45 C46 110.9(2) . . ? O1 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? O1 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.0 . . ? O4 C46 C45 106.42(19) . . ? O4 C46 H46A 110.4 . . ? C45 C46 H46A 110.4 . . ? O4 C46 H46B 110.4 . . ? C45 C46 H46B 110.4 . . ? H46A C46 H46B 108.6 . . ? O4 C47 C48 110.96(18) . . ? O4 C47 H47A 109.4 . . ? C48 C47 H47A 109.4 . . ? O4 C47 H47B 109.4 . . ? C48 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? O8 C48 C47 106.23(18) . . ? O8 C48 H48A 110.5 . . ? C47 C48 H48A 110.5 . . ? O8 C48 H48B 110.5 . . ? C47 C48 H48B 110.5 . . ? H48A C48 H48B 108.7 . . ? O8 C49 C50 110.70(19) . . ? O8 C49 H49A 109.5 . . ? C50 C49 H49A 109.5 . . ? O8 C49 H49B 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? O6 C50 C49 106.71(18) . . ? O6 C50 H50A 110.4 . . ? C49 C50 H50A 110.4 . . ? O6 C50 H50B 110.4 . . ? C49 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? O6 C51 C52 111.19(19) . . ? O6 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? O6 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? O1 C52 C51 106.97(19) . . ? O1 C52 H52A 110.3 . . ? C51 C52 H52A 110.3 . . ? O1 C52 H52B 110.3 . . ? C51 C52 H52B 110.3 . . ? H52A C52 H52B 108.6 . . ? O7 Li1 O8 81.16(14) . . ? O7 Li1 O4 80.48(14) . . ? O8 Li1 O4 72.27(13) . . ? O7 Li1 O2 112.62(18) . . ? O8 Li1 O2 143.1(2) . . ? O4 Li1 O2 141.6(2) . . ? O7 Li1 O5 72.34(13) . . ? O8 Li1 O5 80.37(15) . . ? O4 Li1 O5 143.9(2) . . ? O2 Li1 O5 72.50(13) . . ? O7 Li1 O3 72.20(14) . . ? O8 Li1 O3 143.7(2) . . ? O4 Li1 O3 79.28(15) . . ? O2 Li1 O3 71.72(13) . . ? O5 Li1 O3 113.08(18) . . ? O7 Li1 O6 144.1(2) . . ? O8 Li1 O6 71.45(13) . . ? O4 Li1 O6 111.44(18) . . ? O2 Li1 O6 79.65(14) . . ? O5 Li1 O6 80.38(15) . . ? O3 Li1 O6 141.85(19) . . ? O7 Li1 O1 142.9(2) . . ? O8 Li1 O1 111.07(17) . . ? O4 Li1 O1 71.12(13) . . ? O2 Li1 O1 79.14(14) . . ? O5 Li1 O1 142.6(2) . . ? O3 Li1 O1 79.31(14) . . ? O6 Li1 O1 70.82(13) . . ? C52 O1 C45 114.57(19) . . ? C52 O1 Li1 114.31(18) . . ? C45 O1 Li1 109.51(17) . . ? C39 O2 C38 113.23(18) . . ? C39 O2 Li1 110.62(17) . . ? C38 O2 Li1 114.01(17) . . ? C41 O3 C40 113.65(18) . . ? C41 O3 Li1 109.56(16) . . ? C40 O3 Li1 114.33(17) . . ? C47 O4 C46 113.63(18) . . ? C47 O4 Li1 109.66(17) . . ? C46 O4 Li1 117.02(17) . . ? C37 O5 C44 113.98(18) . . ? C37 O5 Li1 109.98(16) . . ? C44 O5 Li1 114.46(17) . . ? C51 O6 C50 114.02(18) . . ? C51 O6 Li1 110.78(17) . . ? C50 O6 Li1 114.56(17) . . ? C43 O7 C42 113.98(18) . . ? C43 O7 Li1 109.98(17) . . ? C42 O7 Li1 115.29(17) . . ? C48 O8 C49 114.29(18) . . ? C48 O8 Li1 115.53(17) . . ? C49 O8 Li1 111.49(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.292 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.067 data_ac_1_84_0m _database_code_depnum_ccdc_archive 'CCDC 921195' #TrackingRef 'web_deposit_cif_file_3_RichardLewis_1358797319.Complex_4_final.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H72 Co N4' _chemical_formula_weight 619.91 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3082(9) _cell_length_b 11.5753(10) _cell_length_c 16.4021(14) _cell_angle_alpha 70.220(3) _cell_angle_beta 78.481(3) _cell_angle_gamma 73.509(3) _cell_volume 1924.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 686 _exptl_absorpt_coefficient_mu 0.473 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.918 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 31564 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.26 _reflns_number_total 6849 _reflns_number_gt 5459 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0852P)^2^+4.3000P] 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 6849 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.22055(4) 0.25349(4) 0.24896(3) 0.02113(16) Uani 1 1 d . . . N1 N 0.3013(3) 0.3740(3) 0.2337(2) 0.0339(7) Uani 1 1 d . . . N2 N 0.3544(3) 0.1244(3) 0.2630(2) 0.0303(7) Uani 1 1 d . . . N3 N 0.0841(3) 0.3098(3) 0.3147(2) 0.0387(8) Uani 1 1 d . . . N4 N 0.1419(3) 0.2034(3) 0.1869(2) 0.0333(7) Uani 1 1 d . . . C1 C 0.3629(4) 0.4423(3) 0.2431(2) 0.0319(8) Uani 1 1 d . . . C2 C 0.3957(4) 0.5500(4) 0.1603(3) 0.0425(10) Uani 1 1 d . . . C3 C 0.3554(5) 0.5377(5) 0.0812(3) 0.0548(12) Uani 1 1 d . . . H3A H 0.3795 0.6024 0.0288 0.082 Uiso 1 1 calc R . . H3B H 0.2651 0.5489 0.0889 0.082 Uiso 1 1 calc R . . H3C H 0.3957 0.4538 0.0748 0.082 Uiso 1 1 calc R . . C4 C 0.5337(5) 0.5441(4) 0.1422(3) 0.0525(12) Uani 1 1 d . . . H4A H 0.5790 0.4604 0.1374 0.079 Uiso 1 1 calc R . . H4B H 0.5608 0.5593 0.1901 0.079 Uiso 1 1 calc R . . H4C H 0.5505 0.6087 0.0875 0.079 Uiso 1 1 calc R . . C5 C 0.3240(5) 0.6808(4) 0.1702(4) 0.0641(15) Uani 1 1 d . . . H5A H 0.3309 0.7457 0.1139 0.096 Uiso 1 1 calc R . . H5B H 0.3594 0.6991 0.2131 0.096 Uiso 1 1 calc R . . H5C H 0.2364 0.6804 0.1900 0.096 Uiso 1 1 calc R . . C6 C 0.4085(4) 0.4115(4) 0.3334(3) 0.0404(10) Uani 1 1 d . . . C7 C 0.5308(4) 0.3116(4) 0.3362(3) 0.0493(11) Uani 1 1 d . . . H7A H 0.5935 0.3470 0.2917 0.074 Uiso 1 1 calc R . . H7B H 0.5184 0.2382 0.3249 0.074 Uiso 1 1 calc R . . H7C H 0.5589 0.2855 0.3939 0.074 Uiso 1 1 calc R . . C8 C 0.3131(5) 0.3547(4) 0.4052(3) 0.0461(11) Uani 1 1 d . . . H8A H 0.3058 0.2767 0.3976 0.069 Uiso 1 1 calc R . . H8B H 0.2323 0.4152 0.4016 0.069 Uiso 1 1 calc R . . H8C H 0.3404 0.3358 0.4624 0.069 Uiso 1 1 calc R . . C9 C 0.4255(6) 0.5243(5) 0.3546(3) 0.0670(16) Uani 1 1 d . . . H9A H 0.4522 0.4961 0.4129 0.101 Uiso 1 1 calc R . . H9B H 0.3466 0.5878 0.3530 0.101 Uiso 1 1 calc R . . H9C H 0.4886 0.5614 0.3114 0.101 Uiso 1 1 calc R . . C10 C 0.4531(3) 0.0433(3) 0.2558(2) 0.0276(8) Uani 1 1 d . . . C11 C 0.4947(4) -0.0603(3) 0.3415(2) 0.0306(8) Uani 1 1 d . . . C12 C 0.6287(4) -0.0702(4) 0.3538(3) 0.0451(10) Uani 1 1 d . . . H12A H 0.6491 -0.1325 0.4098 0.068 Uiso 1 1 calc R . . H12B H 0.6369 0.0123 0.3529 0.068 Uiso 1 1 calc R . . H12C H 0.6856 -0.0966 0.3064 0.068 Uiso 1 1 calc R . . C13 C 0.4797(4) -0.1893(4) 0.3448(3) 0.0427(10) Uani 1 1 d . . . H13A H 0.4946 -0.2493 0.4026 0.064 Uiso 1 1 calc R . . H13B H 0.5396 -0.2200 0.3003 0.064 Uiso 1 1 calc R . . H13C H 0.3952 -0.1811 0.3337 0.064 Uiso 1 1 calc R . . C14 C 0.4114(4) -0.0265(4) 0.4200(3) 0.0413(10) Uani 1 1 d . . . H14A H 0.3250 -0.0224 0.4157 0.062 Uiso 1 1 calc R . . H14B H 0.4183 0.0557 0.4206 0.062 Uiso 1 1 calc R . . H14C H 0.4376 -0.0911 0.4739 0.062 Uiso 1 1 calc R . . C15 C 0.5280(4) 0.0503(4) 0.1646(3) 0.0421(10) Uani 1 1 d . . . C16 C 0.4397(5) 0.1190(6) 0.0941(3) 0.0690(16) Uani 1 1 d . . . H16A H 0.3983 0.2035 0.0989 0.103 Uiso 1 1 calc R . . H16B H 0.3773 0.0710 0.1019 0.103 Uiso 1 1 calc R . . H16C H 0.4872 0.1263 0.0363 0.103 Uiso 1 1 calc R . . C17 C 0.6211(6) 0.1299(7) 0.1497(4) 0.084(2) Uani 1 1 d . . . H17A H 0.6844 0.0851 0.1898 0.126 Uiso 1 1 calc R . . H17B H 0.5781 0.2108 0.1602 0.126 Uiso 1 1 calc R . . H17C H 0.6609 0.1453 0.0894 0.126 Uiso 1 1 calc R . . C18 C 0.5939(7) -0.0774(7) 0.1504(4) 0.090(2) Uani 1 1 d . . . H18A H 0.6331 -0.0643 0.0900 0.135 Uiso 1 1 calc R . . H18B H 0.5335 -0.1287 0.1617 0.135 Uiso 1 1 calc R . . H18C H 0.6576 -0.1211 0.1903 0.135 Uiso 1 1 calc R . . C19 C -0.0149(4) 0.3610(4) 0.3528(2) 0.0328(8) Uani 1 1 d . . . C20 C -0.0542(4) 0.2845(4) 0.4493(3) 0.0417(10) Uani 1 1 d . . . C21 C -0.0526(5) 0.3563(4) 0.5134(3) 0.0546(13) Uani 1 1 d . . . H21A H -0.1183 0.4343 0.5032 0.082 Uiso 1 1 calc R . . H21B H 0.0282 0.3772 0.5041 0.082 Uiso 1 1 calc R . . H21C H -0.0667 0.3029 0.5735 0.082 Uiso 1 1 calc R . . C22 C 0.0394(5) 0.1601(4) 0.4760(3) 0.0474(11) Uani 1 1 d . . . H22A H 0.0140 0.1125 0.5358 0.071 Uiso 1 1 calc R . . H22B H 0.1211 0.1758 0.4730 0.071 Uiso 1 1 calc R . . H22C H 0.0439 0.1112 0.4365 0.071 Uiso 1 1 calc R . . C23 C -0.1806(5) 0.2578(5) 0.4602(3) 0.0570(13) Uani 1 1 d . . . H23A H -0.1820 0.2150 0.4182 0.086 Uiso 1 1 calc R . . H23B H -0.2439 0.3375 0.4498 0.086 Uiso 1 1 calc R . . H23C H -0.1978 0.2036 0.5195 0.086 Uiso 1 1 calc R . . C24 C -0.0908(4) 0.4909(4) 0.3016(3) 0.0432(10) Uani 1 1 d . . . C25 C -0.0005(5) 0.5703(5) 0.2460(4) 0.0723(17) Uani 1 1 d . . . H25A H -0.0468 0.6520 0.2119 0.108 Uiso 1 1 calc R . . H25B H 0.0556 0.5262 0.2063 0.108 Uiso 1 1 calc R . . H25C H 0.0481 0.5837 0.2838 0.108 Uiso 1 1 calc R . . C26 C -0.1557(6) 0.4621(6) 0.2403(4) 0.0750(17) Uani 1 1 d . . . H26A H -0.2113 0.4071 0.2745 0.113 Uiso 1 1 calc R . . H26B H -0.0935 0.4196 0.2023 0.113 Uiso 1 1 calc R . . H26C H -0.2040 0.5411 0.2045 0.113 Uiso 1 1 calc R . . C27 C -0.1835(8) 0.5670(6) 0.3547(4) 0.111(3) Uani 1 1 d . . . H27A H -0.1408 0.5826 0.3950 0.167 Uiso 1 1 calc R . . H27B H -0.2464 0.5201 0.3880 0.167 Uiso 1 1 calc R . . H27C H -0.2237 0.6478 0.3157 0.167 Uiso 1 1 calc R . . C28 C 0.0846(3) 0.1561(3) 0.1532(2) 0.0287(8) Uani 1 1 d . . . C29 C 0.0348(4) 0.0397(4) 0.2148(3) 0.0416(10) Uani 1 1 d . . . C30 C 0.1353(4) -0.0463(4) 0.2724(3) 0.0478(11) Uani 1 1 d . . . H30A H 0.1059 -0.1200 0.3121 0.072 Uiso 1 1 calc R . . H30B H 0.1541 0.0001 0.3065 0.072 Uiso 1 1 calc R . . H30C H 0.2105 -0.0743 0.2358 0.072 Uiso 1 1 calc R . . C31 C -0.0807(5) 0.0903(5) 0.2722(3) 0.0524(12) Uani 1 1 d . . . H31A H -0.1461 0.1438 0.2353 0.079 Uiso 1 1 calc R . . H31B H -0.0587 0.1399 0.3023 0.079 Uiso 1 1 calc R . . H31C H -0.1107 0.0192 0.3152 0.079 Uiso 1 1 calc R . . C32 C -0.0019(6) -0.0395(5) 0.1715(4) 0.0636(14) Uani 1 1 d . . . H32A H 0.0682 -0.0676 0.1312 0.095 Uiso 1 1 calc R . . H32B H -0.0728 0.0110 0.1391 0.095 Uiso 1 1 calc R . . H32C H -0.0250 -0.1133 0.2162 0.095 Uiso 1 1 calc R . . C33 C 0.0574(4) 0.2254(5) 0.0578(3) 0.0492(11) Uani 1 1 d . . . C34 C -0.0795(5) 0.2706(5) 0.0496(3) 0.0610(13) Uani 1 1 d . . . H34A H -0.1175 0.3299 0.0835 0.091 Uiso 1 1 calc R . . H34B H -0.1180 0.1982 0.0718 0.091 Uiso 1 1 calc R . . H34C H -0.0921 0.3130 -0.0118 0.091 Uiso 1 1 calc R . . C35 C 0.1165(6) 0.3393(6) 0.0227(4) 0.0759(18) Uani 1 1 d . . . H35A H 0.0927 0.3889 -0.0356 0.114 Uiso 1 1 calc R . . H35B H 0.2071 0.3097 0.0195 0.114 Uiso 1 1 calc R . . H35C H 0.0876 0.3920 0.0619 0.114 Uiso 1 1 calc R . . C36 C 0.1169(6) 0.1325(7) 0.0024(3) 0.0803(19) Uani 1 1 d . . . H36A H 0.0705 0.0668 0.0183 0.120 Uiso 1 1 calc R . . H36B H 0.2034 0.0933 0.0138 0.120 Uiso 1 1 calc R . . H36C H 0.1143 0.1792 -0.0597 0.120 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 0.0180(3) 0.0205(2) 0.0248(2) -0.00693(17) -0.00353(17) -0.00358(17) N1 0.0288(19) 0.0269(15) 0.0478(18) -0.0156(13) -0.0056(14) -0.0030(13) N2 0.0220(18) 0.0261(15) 0.0461(18) -0.0108(13) -0.0077(14) -0.0083(13) N3 0.031(2) 0.0476(19) 0.0453(19) -0.0235(16) -0.0008(15) -0.0122(16) N4 0.0201(18) 0.0440(18) 0.0379(17) -0.0197(14) -0.0014(13) -0.0031(14) C1 0.030(2) 0.0254(17) 0.042(2) -0.0103(15) -0.0028(16) -0.0110(16) C2 0.043(3) 0.040(2) 0.043(2) -0.0039(18) -0.0047(19) -0.0180(19) C3 0.045(3) 0.068(3) 0.046(2) 0.001(2) -0.012(2) -0.023(2) C4 0.050(3) 0.053(3) 0.053(3) 0.001(2) -0.008(2) -0.030(2) C5 0.069(4) 0.033(2) 0.076(3) 0.003(2) -0.004(3) -0.016(2) C6 0.050(3) 0.036(2) 0.042(2) -0.0110(17) -0.0054(19) -0.0230(19) C7 0.043(3) 0.051(3) 0.053(3) -0.002(2) -0.015(2) -0.020(2) C8 0.053(3) 0.043(2) 0.046(2) -0.0115(19) -0.006(2) -0.019(2) C9 0.109(5) 0.060(3) 0.054(3) -0.017(2) -0.013(3) -0.052(3) C10 0.018(2) 0.0295(17) 0.0400(19) -0.0122(15) -0.0076(15) -0.0073(15) C11 0.025(2) 0.0264(17) 0.042(2) -0.0087(15) -0.0124(16) -0.0049(15) C12 0.032(3) 0.040(2) 0.063(3) -0.0049(19) -0.023(2) -0.0090(18) C13 0.040(3) 0.0294(19) 0.060(3) -0.0117(18) -0.017(2) -0.0052(18) C14 0.045(3) 0.040(2) 0.039(2) -0.0094(17) -0.0086(18) -0.0098(19) C15 0.024(2) 0.061(3) 0.039(2) -0.0110(19) -0.0039(17) -0.0114(19) C16 0.045(3) 0.118(5) 0.041(3) -0.022(3) -0.003(2) -0.018(3) C17 0.064(4) 0.140(6) 0.054(3) -0.004(3) -0.003(3) -0.066(4) C18 0.079(5) 0.111(5) 0.066(4) -0.044(4) 0.010(3) 0.009(4) C19 0.026(2) 0.0370(19) 0.040(2) -0.0193(16) 0.0016(16) -0.0091(16) C20 0.043(3) 0.034(2) 0.045(2) -0.0108(17) 0.0029(19) -0.0112(18) C21 0.078(4) 0.047(2) 0.044(2) -0.016(2) 0.000(2) -0.023(2) C22 0.053(3) 0.039(2) 0.052(2) -0.0119(19) -0.003(2) -0.017(2) C23 0.049(3) 0.071(3) 0.055(3) -0.020(2) 0.007(2) -0.026(3) C24 0.033(3) 0.047(2) 0.042(2) -0.0058(18) -0.0047(18) -0.0058(19) C25 0.060(4) 0.040(3) 0.108(5) 0.003(3) -0.021(3) -0.020(2) C26 0.084(5) 0.072(4) 0.074(4) 0.002(3) -0.040(3) -0.032(3) C27 0.119(7) 0.067(4) 0.080(4) -0.006(3) 0.004(4) 0.052(4) C28 0.018(2) 0.0373(19) 0.0334(18) -0.0150(15) -0.0037(15) -0.0042(15) C29 0.039(3) 0.042(2) 0.050(2) -0.0117(18) -0.0141(19) -0.0149(19) C30 0.045(3) 0.043(2) 0.054(3) -0.0040(19) -0.017(2) -0.014(2) C31 0.043(3) 0.064(3) 0.054(3) -0.017(2) -0.001(2) -0.022(2) C32 0.075(4) 0.059(3) 0.073(3) -0.026(3) -0.020(3) -0.025(3) C33 0.039(3) 0.071(3) 0.037(2) -0.003(2) -0.0131(19) -0.020(2) C34 0.053(3) 0.071(3) 0.054(3) -0.007(2) -0.022(2) -0.010(3) C35 0.062(4) 0.092(4) 0.057(3) 0.024(3) -0.020(3) -0.040(3) C36 0.056(4) 0.142(6) 0.047(3) -0.045(3) -0.008(3) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.789(3) . ? Co1 N3 1.792(3) . ? Co1 N4 1.794(3) . ? Co1 N1 1.800(3) . ? N1 C1 1.254(5) . ? N2 C10 1.252(5) . ? N3 C19 1.261(5) . ? N4 C28 1.254(5) . ? C1 C6 1.558(6) . ? C1 C2 1.566(5) . ? C2 C3 1.521(6) . ? C2 C4 1.515(6) . ? C2 C5 1.546(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.528(6) . ? C6 C9 1.530(5) . ? C6 C8 1.534(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.554(5) . ? C10 C11 1.562(5) . ? C11 C14 1.531(5) . ? C11 C13 1.532(5) . ? C11 C12 1.536(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.522(7) . ? C15 C18 1.527(8) . ? C15 C16 1.535(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.551(6) . ? C19 C20 1.575(5) . ? C20 C23 1.510(6) . ? C20 C22 1.510(6) . ? C20 C21 1.552(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C27 1.504(7) . ? C24 C25 1.521(6) . ? C24 C26 1.524(7) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.546(5) . ? C28 C29 1.560(5) . ? C29 C32 1.514(6) . ? C29 C30 1.526(6) . ? C29 C31 1.544(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.505(7) . ? C33 C35 1.533(7) . ? C33 C36 1.563(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 N2 Co1 N3 137.57(15) . . ? N2 Co1 N4 98.33(14) . . ? N3 Co1 N4 95.89(14) . . ? N2 Co1 N1 96.19(14) . . ? N3 Co1 N1 98.60(14) . . ? N4 Co1 N1 139.17(15) . . ? C1 N1 Co1 165.1(3) . . ? C10 N2 Co1 167.9(3) . . ? C19 N3 Co1 172.9(3) . . ? C28 N4 Co1 171.9(3) . . ? N1 C1 C6 119.1(3) . . ? N1 C1 C2 116.9(4) . . ? C6 C1 C2 123.9(3) . . ? C3 C2 C4 107.7(4) . . ? C3 C2 C5 107.3(4) . . ? C4 C2 C5 109.7(4) . . ? C3 C2 C1 109.2(3) . . ? C4 C2 C1 112.4(4) . . ? C5 C2 C1 110.4(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C9 109.9(4) . . ? C7 C6 C8 108.3(3) . . ? C9 C6 C8 106.8(4) . . ? C7 C6 C1 107.4(3) . . ? C9 C6 C1 115.4(3) . . ? C8 C6 C1 108.7(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C15 119.7(3) . . ? N2 C10 C11 116.8(3) . . ? C15 C10 C11 123.4(3) . . ? C14 C11 C13 106.7(3) . . ? C14 C11 C12 106.9(3) . . ? C13 C11 C12 110.1(3) . . ? C14 C11 C10 109.3(3) . . ? C13 C11 C10 111.3(3) . . ? C12 C11 C10 112.3(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C18 110.2(5) . . ? C17 C15 C16 106.9(4) . . ? C18 C15 C16 106.7(5) . . ? C17 C15 C10 108.5(4) . . ? C18 C15 C10 115.0(4) . . ? C16 C15 C10 109.3(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C24 118.6(4) . . ? N3 C19 C20 116.6(4) . . ? C24 C19 C20 124.8(3) . . ? C23 C20 C22 108.4(4) . . ? C23 C20 C21 109.8(4) . . ? C22 C20 C21 105.8(4) . . ? C23 C20 C19 112.3(4) . . ? C22 C20 C19 109.8(3) . . ? C21 C20 C19 110.5(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C24 C25 108.0(5) . . ? C27 C24 C26 110.4(5) . . ? C25 C24 C26 107.7(4) . . ? C27 C24 C19 116.8(4) . . ? C25 C24 C19 108.4(4) . . ? C26 C24 C19 105.2(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C33 117.7(3) . . ? N4 C28 C29 116.6(3) . . ? C33 C28 C29 125.4(3) . . ? C32 C29 C30 107.7(4) . . ? C32 C29 C31 107.9(4) . . ? C30 C29 C31 109.4(4) . . ? C32 C29 C28 116.8(4) . . ? C30 C29 C28 107.9(3) . . ? C31 C29 C28 107.0(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C35 109.0(4) . . ? C34 C33 C28 112.4(4) . . ? C35 C33 C28 108.7(4) . . ? C34 C33 C36 108.8(4) . . ? C35 C33 C36 109.3(5) . . ? C28 C33 C36 108.5(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.554 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.083