data_Co(ttp)COiPr 1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Co N4 O' _chemical_formula_weight 798.83 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' '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 11.1015(10) _cell_length_b 11.8717(11) _cell_length_c 16.5406(14) _cell_angle_alpha 82.010(2) _cell_angle_beta 77.176(2) _cell_angle_gamma 84.527(2) _cell_volume 2100.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 95 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6694 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30229 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7587 _reflns_number_gt 5409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+1.0576P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7587 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 -0.90727(3) 0.12484(3) 0.22813(2) 0.03740(13) Uani 1 1 d . . . O1 O -0.8227(3) 0.3272(3) 0.1511(3) 0.1370(16) Uani 1 1 d . . . N1 N -0.8442(2) 0.06015(19) 0.12344(14) 0.0407(5) Uani 1 1 d . . . N2 N -1.0415(2) 0.2046(2) 0.18124(13) 0.0413(6) Uani 1 1 d . . . N3 N -0.9773(2) 0.18335(19) 0.33430(13) 0.0407(5) Uani 1 1 d . . . N4 N -0.8050(2) 0.01219(19) 0.28453(14) 0.0400(5) Uani 1 1 d . . . C1 C -0.7539(3) -0.0275(2) 0.10876(18) 0.0440(7) Uani 1 1 d . . . C2 C -0.7168(3) -0.0349(3) 0.02079(19) 0.0561(8) Uani 1 1 d . . . H2A H -0.6580 -0.0872 -0.0048 0.067 Uiso 1 1 calc R . . C3 C -0.7832(3) 0.0479(3) -0.01792(18) 0.0554(8) Uani 1 1 d . . . H3A H -0.7767 0.0646 -0.0753 0.066 Uiso 1 1 calc R . . C4 C -0.8654(3) 0.1057(2) 0.04529(17) 0.0451(7) Uani 1 1 d . . . C5 C -0.9620(3) 0.1842(2) 0.03232(17) 0.0453(7) Uani 1 1 d . . . C6 C -1.0516(3) 0.2186(2) 0.09869(17) 0.0443(7) Uani 1 1 d . . . C7 C -1.1702(3) 0.2719(3) 0.09090(19) 0.0525(8) Uani 1 1 d . . . H7A H -1.1994 0.2892 0.0418 0.063 Uiso 1 1 calc R . . C8 C -1.2315(3) 0.2922(3) 0.16740(19) 0.0521(8) Uani 1 1 d . . . H8A H -1.3123 0.3236 0.1815 0.063 Uiso 1 1 calc R . . C9 C -1.1501(3) 0.2566(2) 0.22350(17) 0.0429(7) Uani 1 1 d . . . C10 C -1.1690(3) 0.2846(2) 0.30441(17) 0.0446(7) Uani 1 1 d . . . C11 C -1.0809(3) 0.2564(2) 0.35327(17) 0.0448(7) Uani 1 1 d . . . C12 C -1.0876(3) 0.2957(3) 0.43207(19) 0.0562(8) Uani 1 1 d . . . H12A H -1.1482 0.3466 0.4577 0.067 Uiso 1 1 calc R . . C13 C -0.9905(3) 0.2459(3) 0.46221(19) 0.0575(9) Uani 1 1 d . . . H13A H -0.9699 0.2574 0.5119 0.069 Uiso 1 1 calc R . . C14 C -0.9240(3) 0.1713(3) 0.40362(17) 0.0452(7) Uani 1 1 d . . . C15 C -0.8342(3) 0.0870(3) 0.41972(17) 0.0425(7) Uani 1 1 d . . . C16 C -0.7879(3) 0.0061(2) 0.36601(17) 0.0421(7) Uani 1 1 d . . . C17 C -0.7155(3) -0.0961(3) 0.38572(19) 0.0517(8) Uani 1 1 d . . . H17A H -0.6943 -0.1207 0.4369 0.062 Uiso 1 1 calc R . . C18 C -0.6835(3) -0.1500(3) 0.3173(2) 0.0535(8) Uani 1 1 d . . . H18A H -0.6367 -0.2190 0.3124 0.064 Uiso 1 1 calc R . . C19 C -0.7349(3) -0.0814(2) 0.25285(18) 0.0428(7) Uani 1 1 d . . . C20 C -0.7071(3) -0.0995(2) 0.16943(18) 0.0442(7) Uani 1 1 d . . . C21 C -0.9729(3) 0.2343(3) -0.05444(17) 0.0460(7) Uani 1 1 d . . . C22 C -0.9857(3) 0.1695(3) -0.11507(19) 0.0562(8) Uani 1 1 d . . . H22A H -0.9856 0.0906 -0.1033 0.067 Uiso 1 1 calc R . . C23 C -0.9985(3) 0.2221(4) -0.1933(2) 0.0694(10) Uani 1 1 d . . . H23A H -1.0074 0.1772 -0.2332 0.083 Uiso 1 1 calc R . . C24 C -0.9986(3) 0.3383(4) -0.2137(2) 0.0735(11) Uani 1 1 d . . . C25 C -0.9879(3) 0.4026(3) -0.1535(2) 0.0739(11) Uani 1 1 d . . . H25A H -0.9895 0.4816 -0.1653 0.089 Uiso 1 1 calc R . . C26 C -0.9748(3) 0.3517(3) -0.0751(2) 0.0582(8) Uani 1 1 d . . . H26A H -0.9670 0.3973 -0.0354 0.070 Uiso 1 1 calc R . . C27 C -1.0139(5) 0.3936(5) -0.2999(3) 0.130(2) Uani 1 1 d . . . H27A H -1.0116 0.4747 -0.3031 0.195 Uiso 1 1 calc R . . H27B H -1.0918 0.3758 -0.3093 0.195 Uiso 1 1 calc R . . H27C H -0.9479 0.3650 -0.3416 0.195 Uiso 1 1 calc R . . C31 C -1.2886(3) 0.3480(3) 0.33877(17) 0.0484(7) Uani 1 1 d . . . C32 C -1.3158(3) 0.4597(3) 0.3096(2) 0.0686(10) Uani 1 1 d . . . H32A H -1.2565 0.4988 0.2696 0.082 Uiso 1 1 calc R . . C33 C -1.4296(4) 0.5151(3) 0.3385(3) 0.0767(11) Uani 1 1 d . . . H33A H -1.4454 0.5905 0.3172 0.092 Uiso 1 1 calc R . . C34 C -1.5195(3) 0.4612(3) 0.3979(2) 0.0654(10) Uani 1 1 d . . . C35 C -1.4915(3) 0.3509(3) 0.4281(2) 0.0676(10) Uani 1 1 d . . . H35A H -1.5501 0.3129 0.4693 0.081 Uiso 1 1 calc R . . C36 C -1.3779(3) 0.2935(3) 0.3991(2) 0.0586(9) Uani 1 1 d . . . H36A H -1.3623 0.2182 0.4205 0.070 Uiso 1 1 calc R . . C37 C -1.6462(4) 0.5196(4) 0.4278(3) 0.1011(16) Uani 1 1 d . . . H37A H -1.6495 0.5960 0.3999 0.152 Uiso 1 1 calc R . . H37B H -1.6606 0.5218 0.4870 0.152 Uiso 1 1 calc R . . H37C H -1.7086 0.4781 0.4154 0.152 Uiso 1 1 calc R . . C41 C -0.7902(3) 0.0758(3) 0.50008(18) 0.0456(7) Uani 1 1 d . . . C42 C -0.6692(3) 0.0910(4) 0.4995(2) 0.0714(11) Uani 1 1 d . . . H42A H -0.6153 0.1116 0.4490 0.086 Uiso 1 1 calc R . . C43 C -0.6257(4) 0.0760(4) 0.5733(2) 0.0841(13) Uani 1 1 d . . . H43A H -0.5432 0.0867 0.5714 0.101 Uiso 1 1 calc R . . C44 C -0.7032(4) 0.0455(3) 0.6489(2) 0.0688(10) Uani 1 1 d . . . C45 C -0.8215(3) 0.0288(3) 0.6490(2) 0.0626(9) Uani 1 1 d . . . H45A H -0.8747 0.0061 0.6994 0.075 Uiso 1 1 calc R . . C46 C -0.8662(3) 0.0444(3) 0.57612(19) 0.0573(8) Uani 1 1 d . . . H46A H -0.9489 0.0335 0.5787 0.069 Uiso 1 1 calc R . . C47 C -0.6564(5) 0.0280(5) 0.7296(3) 0.1177(19) Uani 1 1 d . . . H47A H -0.7231 0.0071 0.7757 0.177 Uiso 1 1 calc R . . H47B H -0.6251 0.0974 0.7376 0.177 Uiso 1 1 calc R . . H47C H -0.5914 -0.0317 0.7267 0.177 Uiso 1 1 calc R . . C51 C -0.6155(3) -0.1956(2) 0.14279(18) 0.0469(7) Uani 1 1 d . . . C52 C -0.4917(3) -0.1850(3) 0.1324(3) 0.0832(13) Uani 1 1 d . . . H52A H -0.4645 -0.1177 0.1426 0.100 Uiso 1 1 calc R . . C53 C -0.4058(4) -0.2716(3) 0.1071(3) 0.0910(14) Uani 1 1 d . . . H53A H -0.3221 -0.2612 0.1005 0.109 Uiso 1 1 calc R . . C54 C -0.4404(4) -0.3715(3) 0.0914(2) 0.0612(9) Uani 1 1 d . . . C55 C -0.5639(4) -0.3831(3) 0.1027(3) 0.0829(12) Uani 1 1 d . . . H55A H -0.5906 -0.4512 0.0934 0.099 Uiso 1 1 calc R . . C56 C -0.6518(4) -0.2957(3) 0.1278(3) 0.0722(11) Uani 1 1 d . . . H56A H -0.7356 -0.3059 0.1343 0.087 Uiso 1 1 calc R . . C57 C -0.3441(4) -0.4640(3) 0.0612(3) 0.0885(13) Uani 1 1 d . . . H57A H -0.2629 -0.4394 0.0575 0.133 Uiso 1 1 calc R . . H57B H -0.3522 -0.4790 0.0072 0.133 Uiso 1 1 calc R . . H57C H -0.3561 -0.5322 0.0999 0.133 Uiso 1 1 calc R . . C61 C -0.7950(3) 0.2446(3) 0.1909(2) 0.0529(8) Uani 1 1 d . . . C62 C -0.6669(4) 0.2264(4) 0.2103(3) 0.0929(15) Uani 1 1 d . . . H62A H -0.6612 0.1546 0.2468 0.112 Uiso 1 1 calc R . . C63 C -0.5706(5) 0.2211(6) 0.1304(4) 0.145(3) Uani 1 1 d . . . H63A H -0.4897 0.2088 0.1431 0.218 Uiso 1 1 calc R . . H63B H -0.5755 0.2916 0.0946 0.218 Uiso 1 1 calc R . . H63C H -0.5852 0.1595 0.1026 0.218 Uiso 1 1 calc R . . C64 C -0.6437(8) 0.3225(8) 0.2533(4) 0.238(5) Uani 1 1 d . . . H64A H -0.7038 0.3252 0.3047 0.357 Uiso 1 1 calc R . . H64B H -0.6501 0.3931 0.2178 0.357 Uiso 1 1 calc R . . H64C H -0.5621 0.3109 0.2649 0.357 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 0.0349(2) 0.0414(2) 0.0337(2) -0.00305(15) -0.00661(15) 0.00464(16) O1 0.070(2) 0.076(2) 0.243(4) 0.069(3) -0.040(2) -0.0129(16) N1 0.0397(14) 0.0418(13) 0.0386(13) -0.0034(10) -0.0088(10) 0.0065(11) N2 0.0380(13) 0.0494(14) 0.0337(12) -0.0041(10) -0.0064(10) 0.0072(11) N3 0.0374(13) 0.0473(14) 0.0361(12) -0.0032(10) -0.0086(10) 0.0029(11) N4 0.0365(13) 0.0423(13) 0.0388(13) -0.0014(10) -0.0068(10) 0.0009(10) C1 0.0417(17) 0.0431(16) 0.0448(16) -0.0077(13) -0.0070(13) 0.0073(13) C2 0.056(2) 0.058(2) 0.0494(18) -0.0128(15) -0.0045(15) 0.0179(16) C3 0.061(2) 0.063(2) 0.0356(16) -0.0061(14) -0.0059(14) 0.0171(17) C4 0.0470(18) 0.0487(17) 0.0364(15) -0.0049(13) -0.0065(13) 0.0065(14) C5 0.0482(18) 0.0491(17) 0.0363(15) -0.0041(13) -0.0090(13) 0.0068(14) C6 0.0440(17) 0.0522(18) 0.0351(15) -0.0040(13) -0.0105(13) 0.0083(14) C7 0.0493(19) 0.065(2) 0.0419(17) -0.0049(14) -0.0156(14) 0.0132(16) C8 0.0390(17) 0.066(2) 0.0489(18) -0.0071(15) -0.0111(14) 0.0150(15) C9 0.0371(16) 0.0483(17) 0.0398(16) -0.0025(13) -0.0066(12) 0.0067(13) C10 0.0423(17) 0.0473(17) 0.0389(16) -0.0027(13) -0.0033(13) 0.0077(13) C11 0.0448(18) 0.0495(17) 0.0367(15) -0.0039(13) -0.0069(13) 0.0071(14) C12 0.057(2) 0.066(2) 0.0432(17) -0.0166(15) -0.0092(15) 0.0196(17) C13 0.062(2) 0.070(2) 0.0421(17) -0.0165(15) -0.0142(15) 0.0083(18) C14 0.0409(17) 0.0551(18) 0.0382(15) -0.0037(13) -0.0072(13) -0.0017(14) C15 0.0341(16) 0.0539(18) 0.0393(15) 0.0001(13) -0.0099(12) -0.0043(13) C16 0.0344(16) 0.0512(17) 0.0385(15) 0.0021(13) -0.0093(12) 0.0003(13) C17 0.0481(19) 0.058(2) 0.0470(18) 0.0051(15) -0.0156(14) 0.0053(15) C18 0.053(2) 0.0479(18) 0.057(2) 0.0030(15) -0.0170(15) 0.0105(15) C19 0.0371(16) 0.0421(16) 0.0480(17) -0.0023(13) -0.0104(13) 0.0019(13) C20 0.0385(17) 0.0412(16) 0.0519(18) -0.0065(13) -0.0094(13) 0.0029(13) C21 0.0415(17) 0.0563(19) 0.0368(15) -0.0025(13) -0.0079(13) 0.0087(14) C22 0.056(2) 0.069(2) 0.0435(18) -0.0095(15) -0.0114(15) 0.0041(17) C23 0.063(2) 0.107(3) 0.0410(18) -0.0164(19) -0.0149(16) 0.001(2) C24 0.064(3) 0.104(3) 0.046(2) 0.011(2) -0.0132(17) 0.003(2) C25 0.073(3) 0.074(3) 0.064(2) 0.022(2) -0.0148(19) 0.003(2) C26 0.065(2) 0.058(2) 0.0494(19) -0.0044(15) -0.0138(16) 0.0080(17) C27 0.145(5) 0.173(5) 0.066(3) 0.037(3) -0.044(3) -0.004(4) C31 0.0437(18) 0.060(2) 0.0382(16) -0.0084(14) -0.0083(13) 0.0127(15) C32 0.064(2) 0.061(2) 0.068(2) -0.0027(18) 0.0021(18) 0.0147(18) C33 0.074(3) 0.066(2) 0.079(3) -0.008(2) -0.006(2) 0.028(2) C34 0.053(2) 0.084(3) 0.061(2) -0.0284(19) -0.0164(18) 0.0254(19) C35 0.052(2) 0.087(3) 0.057(2) -0.0163(19) 0.0024(17) 0.005(2) C36 0.058(2) 0.061(2) 0.0510(19) -0.0055(16) -0.0048(16) 0.0105(17) C37 0.065(3) 0.131(4) 0.107(3) -0.051(3) -0.018(2) 0.044(3) C41 0.0394(17) 0.0557(18) 0.0414(16) -0.0018(13) -0.0101(13) -0.0038(14) C42 0.050(2) 0.119(3) 0.0443(19) 0.0016(19) -0.0094(15) -0.018(2) C43 0.049(2) 0.145(4) 0.064(2) -0.009(2) -0.0227(18) -0.017(2) C44 0.068(2) 0.098(3) 0.0453(19) -0.0032(18) -0.0228(17) -0.011(2) C45 0.065(2) 0.082(3) 0.0386(17) 0.0046(16) -0.0094(16) -0.0165(19) C46 0.0471(19) 0.076(2) 0.0484(19) 0.0016(16) -0.0106(15) -0.0153(17) C47 0.106(4) 0.197(6) 0.062(3) 0.004(3) -0.048(3) -0.029(4) C51 0.0481(19) 0.0413(17) 0.0508(18) -0.0054(13) -0.0131(14) 0.0061(14) C52 0.053(2) 0.057(2) 0.146(4) -0.043(2) -0.021(2) 0.0080(18) C53 0.053(2) 0.071(3) 0.151(4) -0.042(3) -0.016(2) 0.016(2) C54 0.068(3) 0.048(2) 0.062(2) -0.0043(16) -0.0146(18) 0.0199(17) C55 0.090(3) 0.043(2) 0.114(3) -0.027(2) -0.011(3) 0.003(2) C56 0.056(2) 0.057(2) 0.106(3) -0.024(2) -0.014(2) -0.0002(18) C57 0.093(3) 0.065(2) 0.098(3) -0.015(2) -0.015(2) 0.036(2) C61 0.058(2) 0.0431(18) 0.0519(18) 0.0001(14) -0.0049(15) -0.0011(15) C62 0.102(3) 0.097(3) 0.091(3) 0.046(3) -0.059(3) -0.056(3) C63 0.063(3) 0.174(6) 0.207(7) -0.083(5) -0.004(4) -0.018(4) C64 0.275(10) 0.373(12) 0.106(5) -0.077(6) -0.003(5) -0.240(10) _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 C61 1.925(3) . ? Co1 N2 1.939(2) . ? Co1 N4 1.944(2) . ? Co1 N3 1.950(2) . ? Co1 N1 1.951(2) . ? O1 C61 1.159(4) . ? N1 C1 1.382(3) . ? N1 C4 1.391(3) . ? N2 C6 1.381(3) . ? N2 C9 1.388(3) . ? N3 C11 1.378(3) . ? N3 C14 1.387(3) . ? N4 C19 1.389(3) . ? N4 C16 1.393(3) . ? C1 C20 1.384(4) . ? C1 C2 1.434(4) . ? C2 C3 1.348(4) . ? C3 C4 1.433(4) . ? C4 C5 1.386(4) . ? C5 C6 1.387(4) . ? C5 C21 1.501(4) . ? C6 C7 1.429(4) . ? C7 C8 1.339(4) . ? C8 C9 1.431(4) . ? C9 C10 1.390(4) . ? C10 C11 1.390(4) . ? C10 C31 1.499(4) . ? C11 C12 1.429(4) . ? C12 C13 1.340(4) . ? C13 C14 1.436(4) . ? C14 C15 1.386(4) . ? C15 C16 1.385(4) . ? C15 C41 1.500(4) . ? C16 C17 1.429(4) . ? C17 C18 1.341(4) . ? C18 C19 1.437(4) . ? C19 C20 1.388(4) . ? C20 C51 1.500(4) . ? C21 C22 1.384(4) . ? C21 C26 1.388(4) . ? C22 C23 1.388(5) . ? C23 C24 1.375(5) . ? C24 C25 1.367(5) . ? C24 C27 1.523(5) . ? C25 C26 1.384(5) . ? C31 C32 1.376(4) . ? C31 C36 1.379(4) . ? C32 C33 1.386(5) . ? C33 C34 1.373(5) . ? C34 C35 1.368(5) . ? C34 C37 1.518(5) . ? C35 C36 1.393(5) . ? C41 C42 1.370(4) . ? C41 C46 1.375(4) . ? C42 C43 1.393(5) . ? C43 C44 1.376(5) . ? C44 C45 1.346(5) . ? C44 C47 1.518(5) . ? C45 C46 1.386(4) . ? C51 C52 1.362(5) . ? C51 C56 1.363(4) . ? C52 C53 1.377(5) . ? C53 C54 1.356(5) . ? C54 C55 1.360(5) . ? C54 C57 1.513(5) . ? C55 C56 1.395(5) . ? C61 C62 1.515(5) . ? C62 C64 1.496(7) . ? C62 C63 1.509(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 C61 Co1 N2 95.70(12) . . ? C61 Co1 N4 100.20(12) . . ? N2 Co1 N4 164.10(10) . . ? C61 Co1 N3 93.14(12) . . ? N2 Co1 N3 90.09(9) . . ? N4 Co1 N3 89.30(9) . . ? C61 Co1 N1 90.01(12) . . ? N2 Co1 N1 89.21(9) . . ? N4 Co1 N1 90.53(9) . . ? N3 Co1 N1 176.83(10) . . ? C1 N1 C4 105.6(2) . . ? C1 N1 Co1 127.25(18) . . ? C4 N1 Co1 126.35(18) . . ? C6 N2 C9 105.0(2) . . ? C6 N2 Co1 127.35(18) . . ? C9 N2 Co1 127.63(18) . . ? C11 N3 C14 105.1(2) . . ? C11 N3 Co1 127.80(18) . . ? C14 N3 Co1 126.61(19) . . ? C19 N4 C16 104.8(2) . . ? C19 N4 Co1 127.48(19) . . ? C16 N4 Co1 127.71(19) . . ? N1 C1 C20 125.6(3) . . ? N1 C1 C2 110.0(2) . . ? C20 C1 C2 124.5(3) . . ? C3 C2 C1 107.3(3) . . ? C2 C3 C4 107.6(3) . . ? C5 C4 N1 124.5(2) . . ? C5 C4 C3 125.5(3) . . ? N1 C4 C3 109.5(2) . . ? C4 C5 C6 121.3(3) . . ? C4 C5 C21 120.8(2) . . ? C6 C5 C21 117.9(2) . . ? N2 C6 C5 125.7(3) . . ? N2 C6 C7 110.2(2) . . ? C5 C6 C7 124.1(3) . . ? C8 C7 C6 107.4(3) . . ? C7 C8 C9 107.5(3) . . ? N2 C9 C10 124.8(3) . . ? N2 C9 C8 109.7(2) . . ? C10 C9 C8 124.9(3) . . ? C9 C10 C11 122.2(3) . . ? C9 C10 C31 118.0(3) . . ? C11 C10 C31 119.8(3) . . ? N3 C11 C10 125.0(3) . . ? N3 C11 C12 110.2(2) . . ? C10 C11 C12 124.7(3) . . ? C13 C12 C11 107.5(3) . . ? C12 C13 C14 107.3(3) . . ? C15 C14 N3 124.6(3) . . ? C15 C14 C13 125.0(3) . . ? N3 C14 C13 109.6(3) . . ? C16 C15 C14 122.1(3) . . ? C16 C15 C41 117.5(3) . . ? C14 C15 C41 120.2(3) . . ? C15 C16 N4 124.9(2) . . ? C15 C16 C17 125.2(3) . . ? N4 C16 C17 109.9(2) . . ? C18 C17 C16 107.9(3) . . ? C17 C18 C19 107.2(3) . . ? C20 C19 N4 125.1(3) . . ? C20 C19 C18 124.6(3) . . ? N4 C19 C18 110.0(3) . . ? C1 C20 C19 122.5(3) . . ? C1 C20 C51 118.5(3) . . ? C19 C20 C51 118.8(3) . . ? C22 C21 C26 117.5(3) . . ? C22 C21 C5 123.4(3) . . ? C26 C21 C5 119.1(3) . . ? C21 C22 C23 120.1(3) . . ? C24 C23 C22 122.0(3) . . ? C25 C24 C23 117.9(3) . . ? C25 C24 C27 121.3(4) . . ? C23 C24 C27 120.8(4) . . ? C24 C25 C26 120.9(4) . . ? C25 C26 C21 121.5(3) . . ? C32 C31 C36 117.7(3) . . ? C32 C31 C10 122.0(3) . . ? C36 C31 C10 120.3(3) . . ? C31 C32 C33 121.3(4) . . ? C34 C33 C32 121.4(4) . . ? C35 C34 C33 117.2(3) . . ? C35 C34 C37 120.9(4) . . ? C33 C34 C37 121.9(4) . . ? C34 C35 C36 122.2(4) . . ? C31 C36 C35 120.2(3) . . ? C42 C41 C46 117.4(3) . . ? C42 C41 C15 120.4(3) . . ? C46 C41 C15 122.1(3) . . ? C41 C42 C43 121.0(3) . . ? C44 C43 C42 120.9(3) . . ? C45 C44 C43 117.9(3) . . ? C45 C44 C47 120.9(3) . . ? C43 C44 C47 121.2(4) . . ? C44 C45 C46 121.8(3) . . ? C41 C46 C45 121.0(3) . . ? C52 C51 C56 117.5(3) . . ? C52 C51 C20 120.6(3) . . ? C56 C51 C20 121.9(3) . . ? C51 C52 C53 121.6(4) . . ? C54 C53 C52 121.6(4) . . ? C53 C54 C55 117.1(3) . . ? C53 C54 C57 120.6(4) . . ? C55 C54 C57 122.3(4) . . ? C54 C55 C56 121.9(4) . . ? C51 C56 C55 120.3(4) . . ? O1 C61 C62 120.3(3) . . ? O1 C61 Co1 120.6(3) . . ? C62 C61 Co1 119.0(2) . . ? C64 C62 C63 109.3(4) . . ? C64 C62 C61 109.9(5) . . ? C63 C62 C61 109.9(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.322 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.048 # === END data_Co(tap)COiPr 1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H43 Co N4 O5' _chemical_formula_weight 862.83 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' '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 11.1135(15) _cell_length_b 12.9262(18) _cell_length_c 16.206(2) _cell_angle_alpha 73.844(2) _cell_angle_beta 81.948(2) _cell_angle_gamma 74.511(2) _cell_volume 2149.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 575 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6285 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23575 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7707 _reflns_number_gt 5775 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.5920P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7707 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.37380(3) 0.85507(2) 0.22938(2) 0.03169(12) Uani 1 1 d . . . N1 N 0.26106(18) 0.98359(15) 0.26561(13) 0.0344(5) Uani 1 1 d . . . N2 N 0.44023(18) 0.79980(16) 0.34350(13) 0.0355(5) Uani 1 1 d . . . N3 N 0.50869(18) 0.74489(15) 0.18579(13) 0.0347(5) Uani 1 1 d . . . N4 N 0.31602(19) 0.91813(16) 0.11277(13) 0.0370(5) Uani 1 1 d . . . C1 C 0.1831(2) 1.07563(19) 0.21512(17) 0.0366(6) Uani 1 1 d . . . C2 C 0.1233(2) 1.1526(2) 0.26552(18) 0.0444(7) Uani 1 1 d . . . H2A H 0.0695 1.2217 0.2458 0.053 Uiso 1 1 calc R . . C3 C 0.1583(2) 1.1078(2) 0.34583(18) 0.0442(6) Uani 1 1 d . . . H3A H 0.1321 1.1389 0.3925 0.053 Uiso 1 1 calc R . . C4 C 0.2436(2) 1.0028(2) 0.34670(17) 0.0375(6) Uani 1 1 d . . . C5 C 0.3013(2) 0.9330(2) 0.41893(17) 0.0379(6) Uani 1 1 d . . . C6 C 0.3935(2) 0.8366(2) 0.41675(16) 0.0369(6) Uani 1 1 d . . . C7 C 0.4600(3) 0.7662(2) 0.48915(18) 0.0461(7) Uani 1 1 d . . . H7A H 0.4445 0.7731 0.5455 0.055 Uiso 1 1 calc R . . C8 C 0.5487(3) 0.6886(2) 0.46103(17) 0.0448(7) Uani 1 1 d . . . H8A H 0.6070 0.6322 0.4940 0.054 Uiso 1 1 calc R . . C9 C 0.5372(2) 0.7082(2) 0.37089(16) 0.0362(6) Uani 1 1 d . . . C10 C 0.6172(2) 0.64638(19) 0.31851(16) 0.0356(6) Uani 1 1 d . . . C11 C 0.6019(2) 0.66455(19) 0.23219(17) 0.0363(6) Uani 1 1 d . . . C12 C 0.6783(2) 0.5981(2) 0.17810(18) 0.0434(6) Uani 1 1 d . . . H12A H 0.7473 0.5395 0.1941 0.052 Uiso 1 1 calc R . . C13 C 0.6325(2) 0.6355(2) 0.10014(18) 0.0424(6) Uani 1 1 d . . . H13A H 0.6637 0.6080 0.0521 0.051 Uiso 1 1 calc R . . C14 C 0.5264(2) 0.7257(2) 0.10506(16) 0.0366(6) Uani 1 1 d . . . C15 C 0.4512(2) 0.7832(2) 0.03723(16) 0.0375(6) Uani 1 1 d . . . C16 C 0.3487(2) 0.8703(2) 0.04357(16) 0.0395(6) Uani 1 1 d . . . C17 C 0.2652(3) 0.9269(2) -0.02319(18) 0.0503(7) Uani 1 1 d . . . H17A H 0.2662 0.9083 -0.0748 0.060 Uiso 1 1 calc R . . C18 C 0.1851(3) 1.0118(2) 0.00251(18) 0.0497(7) Uani 1 1 d . . . H18A H 0.1203 1.0630 -0.0280 0.060 Uiso 1 1 calc R . . C19 C 0.2177(2) 1.00885(19) 0.08556(16) 0.0388(6) Uani 1 1 d . . . C20 C 0.1599(2) 1.08781(19) 0.13089(17) 0.0375(6) Uani 1 1 d . . . C21 C 0.2730(2) 0.9642(2) 0.50362(17) 0.0400(6) Uani 1 1 d . . . C22 C 0.1891(4) 0.9235(3) 0.5660(2) 0.0861(13) Uani 1 1 d . . . H22A H 0.1413 0.8809 0.5541 0.103 Uiso 1 1 calc R . . C23 C 0.1742(4) 0.9446(4) 0.6462(2) 0.0959(15) Uani 1 1 d . . . H23A H 0.1161 0.9168 0.6876 0.115 Uiso 1 1 calc R . . C24 C 0.2448(3) 1.0069(2) 0.66531(18) 0.0520(7) Uani 1 1 d . . . C25 C 0.3240(3) 1.0516(2) 0.60289(18) 0.0481(7) Uani 1 1 d . . . H25A H 0.3695 1.0965 0.6138 0.058 Uiso 1 1 calc R . . C26 C 0.3368(3) 1.0302(2) 0.52311(18) 0.0499(7) Uani 1 1 d . . . H26A H 0.3911 1.0620 0.4807 0.060 Uiso 1 1 calc R . . C27 C 0.2938(4) 1.0896(3) 0.7667(2) 0.0708(10) Uani 1 1 d . . . H27A H 0.2731 1.0940 0.8253 0.106 Uiso 1 1 calc R . . H27B H 0.2724 1.1626 0.7289 0.106 Uiso 1 1 calc R . . H27C H 0.3819 1.0583 0.7586 0.106 Uiso 1 1 calc R . . C31 C 0.7277(2) 0.5582(2) 0.35647(17) 0.0381(6) Uani 1 1 d . . . C32 C 0.7143(3) 0.4604(2) 0.4155(2) 0.0563(8) Uani 1 1 d . . . H32A H 0.6348 0.4479 0.4325 0.068 Uiso 1 1 calc R . . C33 C 0.8175(3) 0.3817(2) 0.4492(2) 0.0648(9) Uani 1 1 d . . . H33A H 0.8069 0.3169 0.4891 0.078 Uiso 1 1 calc R . . C34 C 0.9371(3) 0.3977(2) 0.4244(2) 0.0527(7) Uani 1 1 d . . . C35 C 0.9511(3) 0.4937(3) 0.3676(2) 0.0629(9) Uani 1 1 d . . . H35A H 1.0305 0.5066 0.3514 0.075 Uiso 1 1 calc R . . C36 C 0.8461(3) 0.5730(2) 0.3335(2) 0.0597(9) Uani 1 1 d . . . H36A H 0.8571 0.6379 0.2940 0.072 Uiso 1 1 calc R . . C37 C 1.1545(3) 0.3350(3) 0.4483(3) 0.0969(14) Uani 1 1 d . . . H37A H 1.2134 0.2701 0.4769 0.145 Uiso 1 1 calc R . . H37B H 1.1533 0.3959 0.4717 0.145 Uiso 1 1 calc R . . H37C H 1.1789 0.3533 0.3878 0.145 Uiso 1 1 calc R . . C41 C 0.4828(2) 0.7522(2) -0.04690(16) 0.0379(6) Uani 1 1 d . . . C42 C 0.4659(2) 0.6544(2) -0.05660(17) 0.0431(6) Uani 1 1 d . . . H42A H 0.4357 0.6060 -0.0093 0.052 Uiso 1 1 calc R . . C43 C 0.4927(3) 0.6263(2) -0.13468(18) 0.0457(7) Uani 1 1 d . . . H43A H 0.4811 0.5597 -0.1396 0.055 Uiso 1 1 calc R . . C44 C 0.5370(3) 0.6984(2) -0.20532(17) 0.0449(6) Uani 1 1 d . . . C45 C 0.5554(3) 0.7969(2) -0.19689(18) 0.0497(7) Uani 1 1 d . . . H45A H 0.5859 0.8451 -0.2442 0.060 Uiso 1 1 calc R . . C46 C 0.5288(3) 0.8234(2) -0.11898(18) 0.0483(7) Uani 1 1 d . . . H46A H 0.5414 0.8896 -0.1140 0.058 Uiso 1 1 calc R . . C47 C 0.5565(5) 0.5762(3) -0.2941(2) 0.0995(15) Uani 1 1 d . . . H47A H 0.5808 0.5716 -0.3524 0.149 Uiso 1 1 calc R . . H47B H 0.4712 0.5706 -0.2801 0.149 Uiso 1 1 calc R . . H47C H 0.6098 0.5166 -0.2559 0.149 Uiso 1 1 calc R . . C51 C 0.0703(2) 1.1901(2) 0.08490(17) 0.0397(6) Uani 1 1 d . . . C52 C 0.1110(3) 1.2601(2) 0.01177(19) 0.0490(7) Uani 1 1 d . . . H52A H 0.1948 1.2434 -0.0080 0.059 Uiso 1 1 calc R . . C53 C 0.0309(3) 1.3548(2) -0.03336(19) 0.0508(7) Uani 1 1 d . . . H53A H 0.0609 1.4003 -0.0827 0.061 Uiso 1 1 calc R . . C54 C -0.0934(3) 1.3806(2) -0.0045(2) 0.0511(7) Uani 1 1 d . . . C55 C -0.1354(3) 1.3114(3) 0.0686(2) 0.0652(9) Uani 1 1 d . . . H55A H -0.2191 1.3287 0.0886 0.078 Uiso 1 1 calc R . . C56 C -0.0558(3) 1.2171(3) 0.1123(2) 0.0559(8) Uani 1 1 d . . . H56A H -0.0866 1.1708 0.1608 0.067 Uiso 1 1 calc R . . C57 C -0.1436(4) 1.5411(3) -0.1220(2) 0.0824(11) Uani 1 1 d . . . H57A H -0.2138 1.6006 -0.1426 0.124 Uiso 1 1 calc R . . H57B H -0.1136 1.4987 -0.1641 0.124 Uiso 1 1 calc R . . H57C H -0.0780 1.5710 -0.1124 0.124 Uiso 1 1 calc R . . C61 C 0.2617(2) 0.7576(2) 0.26348(18) 0.0436(6) Uani 1 1 d . . . C62 C 0.1228(3) 0.8072(2) 0.2484(2) 0.0521(7) Uani 1 1 d . . . H62A H 0.1092 0.8874 0.2236 0.063 Uiso 1 1 calc R . . C63 C 0.0500(3) 0.7861(3) 0.3345(3) 0.0824(11) Uani 1 1 d . . . H63A H 0.0775 0.8197 0.3721 0.124 Uiso 1 1 calc R . . H63B H 0.0637 0.7077 0.3593 0.124 Uiso 1 1 calc R . . H63C H -0.0376 0.8176 0.3271 0.124 Uiso 1 1 calc R . . C64 C 0.0831(4) 0.7549(4) 0.1858(3) 0.0910(13) Uani 1 1 d . . . H64A H -0.0039 0.7865 0.1764 0.137 Uiso 1 1 calc R . . H64B H 0.0963 0.6763 0.2098 0.137 Uiso 1 1 calc R . . H64C H 0.1321 0.7690 0.1320 0.137 Uiso 1 1 calc R . . O1 O 0.2259(2) 1.02149(19) 0.74771(13) 0.0708(7) Uani 1 1 d . . . O2 O 1.0338(2) 0.31402(18) 0.46098(16) 0.0733(7) Uani 1 1 d . . . O3 O 0.5675(2) 0.67855(17) -0.28503(13) 0.0651(6) Uani 1 1 d . . . O4 O -0.1812(2) 1.47113(18) -0.04334(16) 0.0746(7) Uani 1 1 d . . . O5 O 0.2995(2) 0.66287(17) 0.29632(18) 0.0797(8) 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 0.03313(19) 0.03185(18) 0.0285(2) -0.00866(14) -0.00119(13) -0.00455(13) N1 0.0368(11) 0.0338(10) 0.0325(12) -0.0117(9) -0.0014(9) -0.0053(9) N2 0.0349(11) 0.0358(11) 0.0346(12) -0.0098(9) -0.0009(9) -0.0061(9) N3 0.0328(11) 0.0352(11) 0.0328(12) -0.0073(9) -0.0034(9) -0.0034(9) N4 0.0423(12) 0.0328(10) 0.0328(12) -0.0104(9) -0.0024(9) -0.0019(9) C1 0.0367(13) 0.0327(12) 0.0394(15) -0.0111(11) 0.0006(11) -0.0064(10) C2 0.0447(15) 0.0387(14) 0.0485(18) -0.0162(13) -0.0028(13) -0.0024(12) C3 0.0473(15) 0.0459(15) 0.0400(17) -0.0213(13) 0.0002(13) -0.0028(12) C4 0.0388(14) 0.0398(13) 0.0352(15) -0.0148(11) 0.0024(11) -0.0089(11) C5 0.0398(14) 0.0415(14) 0.0354(15) -0.0147(11) 0.0038(11) -0.0131(11) C6 0.0404(14) 0.0409(13) 0.0311(14) -0.0104(11) -0.0004(11) -0.0121(11) C7 0.0554(17) 0.0509(16) 0.0303(15) -0.0095(12) -0.0038(13) -0.0106(13) C8 0.0505(16) 0.0456(15) 0.0341(15) -0.0057(12) -0.0092(13) -0.0058(13) C9 0.0372(13) 0.0384(13) 0.0321(14) -0.0063(11) -0.0048(11) -0.0091(11) C10 0.0340(13) 0.0365(13) 0.0346(15) -0.0064(11) -0.0039(11) -0.0073(10) C11 0.0320(13) 0.0376(13) 0.0363(15) -0.0098(11) 0.0002(11) -0.0042(10) C12 0.0365(14) 0.0437(14) 0.0428(17) -0.0113(12) 0.0003(12) 0.0011(11) C13 0.0411(14) 0.0467(15) 0.0358(16) -0.0146(12) 0.0037(12) -0.0031(12) C14 0.0372(13) 0.0383(13) 0.0327(15) -0.0115(11) 0.0036(11) -0.0067(11) C15 0.0435(14) 0.0374(13) 0.0293(14) -0.0096(11) -0.0009(11) -0.0052(11) C16 0.0495(15) 0.0351(13) 0.0302(14) -0.0088(11) -0.0029(12) -0.0032(11) C17 0.0628(18) 0.0477(16) 0.0360(16) -0.0144(13) -0.0121(14) 0.0025(14) C18 0.0568(17) 0.0453(15) 0.0379(16) -0.0097(13) -0.0146(13) 0.0081(13) C19 0.0443(14) 0.0347(13) 0.0326(15) -0.0065(11) -0.0052(12) -0.0024(11) C20 0.0391(14) 0.0338(13) 0.0362(15) -0.0081(11) -0.0014(11) -0.0045(11) C21 0.0429(14) 0.0420(14) 0.0349(15) -0.0132(12) 0.0002(12) -0.0079(12) C22 0.117(3) 0.118(3) 0.061(2) -0.050(2) 0.038(2) -0.087(3) C23 0.135(4) 0.137(4) 0.057(2) -0.053(2) 0.053(2) -0.104(3) C24 0.074(2) 0.0528(16) 0.0332(16) -0.0144(13) 0.0080(14) -0.0244(15) C25 0.0523(16) 0.0583(17) 0.0413(17) -0.0189(14) 0.0022(13) -0.0222(14) C26 0.0504(16) 0.0651(18) 0.0393(17) -0.0175(14) 0.0120(13) -0.0253(14) C27 0.111(3) 0.071(2) 0.0421(19) -0.0218(16) 0.0003(19) -0.036(2) C31 0.0379(14) 0.0384(13) 0.0367(15) -0.0101(11) -0.0049(11) -0.0054(11) C32 0.0477(16) 0.0503(17) 0.066(2) 0.0004(15) -0.0103(15) -0.0157(14) C33 0.067(2) 0.0447(16) 0.072(2) 0.0054(16) -0.0197(18) -0.0094(15) C34 0.0488(17) 0.0451(16) 0.059(2) -0.0124(14) -0.0185(15) 0.0048(13) C35 0.0366(15) 0.0584(18) 0.083(3) -0.0030(17) -0.0094(15) -0.0071(14) C36 0.0438(16) 0.0455(16) 0.076(2) 0.0071(15) -0.0088(15) -0.0093(13) C37 0.056(2) 0.082(3) 0.146(4) -0.029(3) -0.045(2) 0.0158(19) C41 0.0387(14) 0.0396(13) 0.0309(14) -0.0103(11) -0.0028(11) -0.0002(11) C42 0.0509(16) 0.0390(14) 0.0344(15) -0.0043(11) -0.0014(12) -0.0082(12) C43 0.0575(17) 0.0403(14) 0.0407(16) -0.0155(12) -0.0017(13) -0.0095(12) C44 0.0501(16) 0.0482(15) 0.0336(15) -0.0150(12) 0.0002(12) -0.0036(12) C45 0.0632(18) 0.0495(16) 0.0359(16) -0.0103(13) 0.0086(14) -0.0191(14) C46 0.0605(18) 0.0428(15) 0.0441(17) -0.0135(13) -0.0002(14) -0.0158(13) C47 0.186(5) 0.076(2) 0.049(2) -0.0348(19) 0.010(3) -0.040(3) C51 0.0419(14) 0.0364(13) 0.0383(16) -0.0119(11) -0.0036(12) -0.0020(11) C52 0.0405(15) 0.0438(15) 0.0520(18) -0.0056(13) 0.0017(13) -0.0014(12) C53 0.0527(17) 0.0407(15) 0.0489(18) -0.0033(13) -0.0044(14) -0.0024(13) C54 0.0475(16) 0.0471(16) 0.0533(19) -0.0148(14) -0.0156(14) 0.0060(13) C55 0.0361(16) 0.080(2) 0.064(2) -0.0097(18) -0.0013(15) 0.0022(15) C56 0.0448(16) 0.0638(19) 0.0466(18) -0.0026(15) 0.0011(14) -0.0062(14) C57 0.095(3) 0.056(2) 0.078(3) 0.0002(19) -0.037(2) 0.0096(19) C61 0.0473(15) 0.0361(14) 0.0473(17) -0.0143(12) -0.0005(13) -0.0075(12) C62 0.0458(16) 0.0543(17) 0.058(2) -0.0112(15) -0.0072(14) -0.0164(13) C63 0.055(2) 0.101(3) 0.089(3) -0.030(2) 0.0091(19) -0.0164(19) C64 0.109(3) 0.115(3) 0.072(3) -0.027(2) -0.010(2) -0.061(3) O1 0.1103(18) 0.0814(15) 0.0348(12) -0.0225(11) 0.0168(12) -0.0499(14) O2 0.0602(14) 0.0596(13) 0.0859(18) -0.0100(12) -0.0285(13) 0.0127(11) O3 0.0982(17) 0.0635(13) 0.0371(12) -0.0239(10) 0.0106(11) -0.0213(12) O4 0.0603(14) 0.0594(13) 0.0835(18) -0.0043(13) -0.0252(13) 0.0164(11) O5 0.0624(14) 0.0426(12) 0.125(2) -0.0090(13) 0.0014(14) -0.0152(10) _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 C61 1.925(3) . ? Co1 N2 1.960(2) . ? Co1 N4 1.962(2) . ? Co1 N3 1.9742(19) . ? Co1 N1 1.9747(19) . ? N1 C4 1.382(3) . ? N1 C1 1.394(3) . ? N2 C6 1.384(3) . ? N2 C9 1.386(3) . ? N3 C14 1.376(3) . ? N3 C11 1.388(3) . ? N4 C16 1.387(3) . ? N4 C19 1.388(3) . ? C1 C20 1.383(4) . ? C1 C2 1.431(3) . ? C2 C3 1.335(4) . ? C3 C4 1.430(3) . ? C4 C5 1.382(4) . ? C5 C6 1.391(3) . ? C5 C21 1.505(4) . ? C6 C7 1.429(4) . ? C7 C8 1.336(4) . ? C8 C9 1.429(4) . ? C9 C10 1.391(3) . ? C10 C11 1.379(4) . ? C10 C31 1.504(3) . ? C11 C12 1.431(3) . ? C12 C13 1.341(4) . ? C13 C14 1.431(3) . ? C14 C15 1.390(3) . ? C15 C16 1.386(3) . ? C15 C41 1.496(3) . ? C16 C17 1.430(4) . ? C17 C18 1.341(4) . ? C18 C19 1.430(4) . ? C19 C20 1.389(3) . ? C20 C51 1.500(3) . ? C21 C26 1.365(4) . ? C21 C22 1.367(4) . ? C22 C23 1.380(5) . ? C23 C24 1.379(4) . ? C24 C25 1.352(4) . ? C24 O1 1.380(3) . ? C25 C26 1.377(4) . ? C27 O1 1.417(4) . ? C31 C36 1.365(4) . ? C31 C32 1.387(4) . ? C32 C33 1.375(4) . ? C33 C34 1.387(4) . ? C34 C35 1.356(4) . ? C34 O2 1.370(3) . ? C35 C36 1.394(4) . ? C37 O2 1.415(4) . ? C41 C42 1.380(4) . ? C41 C46 1.399(4) . ? C42 C43 1.383(4) . ? C43 C44 1.383(4) . ? C44 O3 1.365(3) . ? C44 C45 1.388(4) . ? C45 C46 1.371(4) . ? C47 O3 1.410(4) . ? C51 C52 1.379(4) . ? C51 C56 1.391(4) . ? C52 C53 1.388(4) . ? C53 C54 1.378(4) . ? C54 O4 1.368(3) . ? C54 C55 1.378(4) . ? C55 C56 1.375(4) . ? C57 O4 1.425(4) . ? C61 O5 1.176(3) . ? C61 C62 1.531(4) . ? C62 C63 1.506(5) . ? C62 C64 1.532(5) . ? 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 C61 Co1 N2 90.49(10) . . ? C61 Co1 N4 93.93(11) . . ? N2 Co1 N4 175.58(8) . . ? C61 Co1 N3 93.41(10) . . ? N2 Co1 N3 90.39(8) . . ? N4 Co1 N3 89.45(8) . . ? C61 Co1 N1 97.39(10) . . ? N2 Co1 N1 89.78(8) . . ? N4 Co1 N1 89.56(8) . . ? N3 Co1 N1 169.20(8) . . ? C4 N1 C1 104.71(19) . . ? C4 N1 Co1 127.46(16) . . ? C1 N1 Co1 127.82(17) . . ? C6 N2 C9 104.5(2) . . ? C6 N2 Co1 127.78(16) . . ? C9 N2 Co1 127.42(17) . . ? C14 N3 C11 104.81(19) . . ? C14 N3 Co1 127.96(16) . . ? C11 N3 Co1 127.10(17) . . ? C16 N4 C19 104.3(2) . . ? C16 N4 Co1 127.11(16) . . ? C19 N4 Co1 127.67(17) . . ? C20 C1 N1 125.4(2) . . ? C20 C1 C2 124.8(2) . . ? N1 C1 C2 109.7(2) . . ? C3 C2 C1 107.8(2) . . ? C2 C3 C4 107.3(2) . . ? C5 C4 N1 125.7(2) . . ? C5 C4 C3 123.8(2) . . ? N1 C4 C3 110.4(2) . . ? C4 C5 C6 123.0(2) . . ? C4 C5 C21 120.1(2) . . ? C6 C5 C21 116.7(2) . . ? N2 C6 C5 125.1(2) . . ? N2 C6 C7 110.3(2) . . ? C5 C6 C7 124.4(2) . . ? C8 C7 C6 107.4(2) . . ? C7 C8 C9 107.3(2) . . ? N2 C9 C10 125.7(2) . . ? N2 C9 C8 110.3(2) . . ? C10 C9 C8 123.9(2) . . ? C11 C10 C9 122.9(2) . . ? C11 C10 C31 118.2(2) . . ? C9 C10 C31 118.9(2) . . ? C10 C11 N3 126.1(2) . . ? C10 C11 C12 124.0(2) . . ? N3 C11 C12 109.9(2) . . ? C13 C12 C11 107.7(2) . . ? C12 C13 C14 106.8(2) . . ? N3 C14 C15 125.5(2) . . ? N3 C14 C13 110.8(2) . . ? C15 C14 C13 123.7(2) . . ? C16 C15 C14 122.6(2) . . ? C16 C15 C41 118.2(2) . . ? C14 C15 C41 119.1(2) . . ? C15 C16 N4 125.4(2) . . ? C15 C16 C17 124.0(2) . . ? N4 C16 C17 110.5(2) . . ? C18 C17 C16 107.2(3) . . ? C17 C18 C19 107.3(2) . . ? N4 C19 C20 125.5(2) . . ? N4 C19 C18 110.5(2) . . ? C20 C19 C18 124.1(2) . . ? C1 C20 C19 122.5(2) . . ? C1 C20 C51 119.8(2) . . ? C19 C20 C51 117.6(2) . . ? C26 C21 C22 117.1(3) . . ? C26 C21 C5 120.5(2) . . ? C22 C21 C5 122.3(3) . . ? C21 C22 C23 121.0(3) . . ? C24 C23 C22 120.4(3) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 O1 124.5(3) . . ? C23 C24 O1 116.5(3) . . ? C24 C25 C26 119.6(3) . . ? C21 C26 C25 122.7(3) . . ? C36 C31 C32 117.7(2) . . ? C36 C31 C10 120.2(2) . . ? C32 C31 C10 122.1(2) . . ? C33 C32 C31 120.6(3) . . ? C32 C33 C34 120.9(3) . . ? C35 C34 O2 124.6(3) . . ? C35 C34 C33 119.0(3) . . ? O2 C34 C33 116.4(3) . . ? C34 C35 C36 119.8(3) . . ? C31 C36 C35 122.1(3) . . ? C42 C41 C46 117.9(2) . . ? C42 C41 C15 121.6(2) . . ? C46 C41 C15 120.5(2) . . ? C41 C42 C43 121.8(2) . . ? C44 C43 C42 119.3(2) . . ? O3 C44 C43 124.2(3) . . ? O3 C44 C45 116.0(2) . . ? C43 C44 C45 119.8(3) . . ? C46 C45 C44 120.2(3) . . ? C45 C46 C41 120.9(3) . . ? C52 C51 C56 117.4(2) . . ? C52 C51 C20 120.3(2) . . ? C56 C51 C20 122.2(2) . . ? C51 C52 C53 122.2(3) . . ? C54 C53 C52 119.4(3) . . ? O4 C54 C53 124.8(3) . . ? O4 C54 C55 116.1(3) . . ? C53 C54 C55 119.1(3) . . ? C56 C55 C54 121.1(3) . . ? C55 C56 C51 120.7(3) . . ? O5 C61 C62 121.4(3) . . ? O5 C61 Co1 120.4(2) . . ? C62 C61 Co1 118.23(19) . . ? C63 C62 C61 107.7(3) . . ? C63 C62 C64 111.7(3) . . ? C61 C62 C64 109.9(3) . . ? C24 O1 C27 116.8(2) . . ? C34 O2 C37 117.8(3) . . ? C44 O3 C47 117.1(2) . . ? C54 O4 C57 117.9(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.349 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.049 # === END data_Co(tpclp)COiPr 1c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H31 Cl4 Co N4 O' _chemical_formula_weight 880.50 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' 'Cl' 'Cl' 0.1484 0.1585 '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 13.419(2) _cell_length_b 13.549(2) _cell_length_c 16.161(2) _cell_angle_alpha 86.518(3) _cell_angle_beta 68.511(3) _cell_angle_gamma 60.584(3) _cell_volume 2355.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 234 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4648 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30999 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8380 _reflns_number_gt 5764 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8380 _refine_ls_number_parameters 551 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0848 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1795 _refine_ls_wR_factor_gt 0.1621 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.997 _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 0.21033(4) 0.43910(3) 0.35170(3) 0.04641(17) Uani 1 1 d . A . Cl1 Cl -0.06657(12) -0.05975(10) 0.28999(9) 0.0923(4) Uani 1 1 d . . . Cl2 Cl 0.19628(14) 0.22384(12) 0.91846(8) 0.1032(4) Uani 1 1 d . . . Cl3 Cl 0.41968(13) 0.97963(12) 0.44657(10) 0.1132(5) Uani 1 1 d . . . Cl4 Cl 0.31707(12) 0.58929(10) -0.23977(7) 0.0916(4) Uani 1 1 d . . . N1 N 0.1683(2) 0.3988(2) 0.26032(18) 0.0488(6) Uani 1 1 d . . . N2 N 0.1402(2) 0.3578(2) 0.43387(17) 0.0479(6) Uani 1 1 d . . . N3 N 0.2463(2) 0.4836(2) 0.44546(17) 0.0482(6) Uani 1 1 d . . . N4 N 0.2423(2) 0.5504(2) 0.28123(17) 0.0492(6) Uani 1 1 d . . . C1 C 0.1954(3) 0.4236(3) 0.1733(2) 0.0550(8) Uani 1 1 d . . . C2 C 0.1812(4) 0.3552(3) 0.1191(3) 0.0674(10) Uani 1 1 d . . . H2A H 0.1957 0.3557 0.0583 0.081 Uiso 1 1 calc R . . C3 C 0.1436(4) 0.2907(3) 0.1719(2) 0.0644(10) Uani 1 1 d . . . H3A H 0.1276 0.2376 0.1544 0.077 Uiso 1 1 calc R . . C4 C 0.1320(3) 0.3178(3) 0.2610(2) 0.0521(8) Uani 1 1 d . . . C5 C 0.0878(3) 0.2746(3) 0.3366(2) 0.0507(8) Uani 1 1 d . . . C6 C 0.0839(3) 0.3016(3) 0.4200(2) 0.0504(8) Uani 1 1 d . . . C7 C 0.0303(3) 0.2654(3) 0.5006(2) 0.0588(9) Uani 1 1 d . . . H7A H -0.0151 0.2290 0.5080 0.071 Uiso 1 1 calc R . . C8 C 0.0581(3) 0.2941(3) 0.5638(2) 0.0567(8) Uani 1 1 d . . . H8A H 0.0349 0.2819 0.6234 0.068 Uiso 1 1 calc R . . C9 C 0.1301(3) 0.3470(3) 0.5218(2) 0.0496(7) Uani 1 1 d . . . C10 C 0.1906(3) 0.3758(3) 0.5621(2) 0.0514(8) Uani 1 1 d . . . C11 C 0.2492(3) 0.4362(3) 0.5230(2) 0.0501(8) Uani 1 1 d . . . C12 C 0.3110(4) 0.4698(3) 0.5620(3) 0.0610(9) Uani 1 1 d . . . H12A H 0.3296 0.4449 0.6121 0.073 Uiso 1 1 calc R . . C13 C 0.3365(4) 0.5434(3) 0.5127(3) 0.0615(9) Uani 1 1 d . . . H13A H 0.3740 0.5808 0.5232 0.074 Uiso 1 1 calc R . . C14 C 0.2954(3) 0.5539(3) 0.4409(2) 0.0498(8) Uani 1 1 d . . . C15 C 0.2983(3) 0.6286(3) 0.3791(2) 0.0491(8) Uani 1 1 d . . . C16 C 0.2698(3) 0.6282(3) 0.3045(2) 0.0488(7) Uani 1 1 d . . . C17 C 0.2756(3) 0.7010(3) 0.2372(2) 0.0561(8) Uani 1 1 d . . . H17A H 0.2885 0.7620 0.2392 0.067 Uiso 1 1 calc R . . C18 C 0.2588(3) 0.6649(3) 0.1707(2) 0.0592(9) Uani 1 1 d . . . H18A H 0.2593 0.6953 0.1175 0.071 Uiso 1 1 calc R . . C19 C 0.2402(3) 0.5705(3) 0.1971(2) 0.0520(8) Uani 1 1 d . . . C20 C 0.2265(3) 0.5054(3) 0.1427(2) 0.0539(8) Uani 1 1 d . . . C21 C 0.0461(3) 0.1936(3) 0.3276(2) 0.0534(8) Uani 1 1 d . . . C22 C -0.0493(4) 0.2246(3) 0.2985(3) 0.0634(10) Uani 1 1 d . . . H22A H -0.0912 0.2991 0.2871 0.076 Uiso 1 1 calc R . . C23 C -0.0839(4) 0.1470(3) 0.2860(3) 0.0657(10) Uani 1 1 d . . . H23A H -0.1465 0.1684 0.2649 0.079 Uiso 1 1 calc R . . C24 C -0.0237(4) 0.0383(3) 0.3055(3) 0.0660(10) Uani 1 1 d . . . C25 C 0.0681(4) 0.0058(3) 0.3362(3) 0.0683(10) Uani 1 1 d . . . H25A H 0.1073 -0.0681 0.3495 0.082 Uiso 1 1 calc R . . C26 C 0.1034(4) 0.0830(3) 0.3477(3) 0.0641(9) Uani 1 1 d . . . H26A H 0.1661 0.0604 0.3690 0.077 Uiso 1 1 calc R . . C31 C 0.1908(3) 0.3384(3) 0.6516(2) 0.0509(8) Uani 1 1 d . . . C32 C 0.2369(3) 0.2243(3) 0.6620(2) 0.0554(8) Uani 1 1 d . . . H32A H 0.2678 0.1706 0.6129 0.066 Uiso 1 1 calc R . . C33 C 0.2382(4) 0.1880(3) 0.7433(2) 0.0613(9) Uani 1 1 d . . . H33A H 0.2686 0.1110 0.7496 0.074 Uiso 1 1 calc R . . C34 C 0.1932(4) 0.2689(4) 0.8155(2) 0.0668(10) Uani 1 1 d . . . C35 C 0.1460(4) 0.3832(4) 0.8078(2) 0.0697(10) Uani 1 1 d . . . H35A H 0.1164 0.4367 0.8567 0.084 Uiso 1 1 calc R . . C36 C 0.1432(4) 0.4170(3) 0.7264(2) 0.0636(9) Uani 1 1 d . . . H36A H 0.1085 0.4946 0.7213 0.076 Uiso 1 1 calc R . . C41 C 0.3317(3) 0.7147(3) 0.3936(2) 0.0511(8) Uani 1 1 d . . . C42 C 0.2545(4) 0.7981(3) 0.4685(2) 0.0622(9) Uani 1 1 d . . . H42A H 0.1836 0.7992 0.5092 0.075 Uiso 1 1 calc R . . C43 C 0.2819(4) 0.8802(3) 0.4836(3) 0.0718(11) Uani 1 1 d . . . H43A H 0.2288 0.9367 0.5336 0.086 Uiso 1 1 calc R . . C44 C 0.3853(4) 0.8779(3) 0.4258(3) 0.0647(10) Uani 1 1 d . . . C45 C 0.4653(4) 0.7957(4) 0.3503(3) 0.0758(11) Uani 1 1 d . . . H45A H 0.5366 0.7946 0.3107 0.091 Uiso 1 1 calc R . . C46 C 0.4364(4) 0.7146(3) 0.3351(3) 0.0682(10) Uani 1 1 d . . . H46A H 0.4891 0.6591 0.2844 0.082 Uiso 1 1 calc R . . C51 C 0.2480(3) 0.5266(3) 0.0473(2) 0.0543(8) Uani 1 1 d . . . C52 C 0.3670(4) 0.4893(4) -0.0147(2) 0.0702(11) Uani 1 1 d . . . H52A H 0.4336 0.4504 0.0030 0.084 Uiso 1 1 calc R . . C53 C 0.3884(4) 0.5092(4) -0.1033(3) 0.0755(11) Uani 1 1 d . . . H53A H 0.4687 0.4842 -0.1448 0.091 Uiso 1 1 calc R . . C54 C 0.2901(4) 0.5660(3) -0.1285(2) 0.0622(9) Uani 1 1 d . . . C55 C 0.1730(4) 0.6032(4) -0.0694(3) 0.0801(12) Uani 1 1 d . . . H55A H 0.1070 0.6417 -0.0877 0.096 Uiso 1 1 calc R . . C56 C 0.1520(4) 0.5837(4) 0.0190(3) 0.0801(12) Uani 1 1 d . . . H56A H 0.0711 0.6098 0.0599 0.096 Uiso 1 1 calc R . . C61 C 0.3786(4) 0.3167(4) 0.2927(3) 0.0914(15) Uani 1 1 d D . . O1 O 0.4479(4) 0.3357(4) 0.2193(4) 0.097(2) Uani 0.639(8) 1 d PD A 1 C62 C 0.4377(6) 0.2079(5) 0.3280(5) 0.080(2) Uani 0.639(8) 1 d PD A 1 C63 C 0.4619(10) 0.1188(7) 0.2561(7) 0.118(3) Uani 0.639(8) 1 d PD A 1 O1' O 0.3728(11) 0.2198(8) 0.3061(8) 0.120(5) Uani 0.361(8) 1 d PDU A 2 C62' C 0.4937(9) 0.3007(10) 0.2890(8) 0.091(4) Uani 0.361(8) 1 d PDU A 2 C63' C 0.5513(19) 0.2617(18) 0.1872(9) 0.129(6) Uani 0.361(8) 1 d PDU A 2 C64 C 0.5481(6) 0.2041(7) 0.3432(5) 0.146(3) Uani 1 1 d 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 0.0548(3) 0.0457(3) 0.0513(3) 0.00331(18) -0.0263(2) -0.0298(2) Cl1 0.1188(9) 0.0764(7) 0.1077(9) -0.0048(6) -0.0339(7) -0.0724(7) Cl2 0.1362(11) 0.1282(11) 0.0717(7) 0.0351(7) -0.0626(8) -0.0720(10) Cl3 0.1257(10) 0.1038(9) 0.1347(11) -0.0279(8) -0.0244(8) -0.0885(9) Cl4 0.1226(10) 0.0863(8) 0.0590(6) 0.0134(5) -0.0474(6) -0.0394(7) N1 0.0598(16) 0.0460(15) 0.0538(16) 0.0051(11) -0.0282(13) -0.0314(14) N2 0.0563(15) 0.0506(16) 0.0514(15) 0.0039(11) -0.0292(13) -0.0311(14) N3 0.0561(16) 0.0452(15) 0.0553(16) 0.0063(12) -0.0286(13) -0.0289(13) N4 0.0577(16) 0.0566(16) 0.0476(15) 0.0024(12) -0.0240(13) -0.0358(14) C1 0.070(2) 0.058(2) 0.0516(19) 0.0062(15) -0.0295(17) -0.0376(19) C2 0.102(3) 0.075(2) 0.057(2) 0.0095(18) -0.042(2) -0.059(2) C3 0.093(3) 0.065(2) 0.061(2) 0.0047(17) -0.041(2) -0.050(2) C4 0.064(2) 0.0529(19) 0.057(2) 0.0051(15) -0.0325(17) -0.0355(18) C5 0.061(2) 0.0461(18) 0.063(2) 0.0088(15) -0.0355(17) -0.0323(17) C6 0.0583(19) 0.0494(19) 0.060(2) 0.0112(15) -0.0336(17) -0.0321(17) C7 0.063(2) 0.068(2) 0.066(2) 0.0152(17) -0.0299(18) -0.045(2) C8 0.064(2) 0.063(2) 0.056(2) 0.0121(16) -0.0288(17) -0.0384(19) C9 0.0534(18) 0.0449(18) 0.0574(19) 0.0053(14) -0.0245(16) -0.0273(16) C10 0.060(2) 0.0456(18) 0.0546(19) 0.0013(14) -0.0271(16) -0.0264(17) C11 0.064(2) 0.0461(18) 0.0538(19) 0.0067(14) -0.0334(17) -0.0299(17) C12 0.089(3) 0.062(2) 0.069(2) 0.0183(17) -0.053(2) -0.049(2) C13 0.079(2) 0.067(2) 0.071(2) 0.0138(18) -0.046(2) -0.048(2) C14 0.0585(19) 0.0469(18) 0.059(2) 0.0040(14) -0.0317(17) -0.0304(17) C15 0.0534(18) 0.0466(18) 0.0578(19) 0.0001(14) -0.0233(16) -0.0305(16) C16 0.0551(19) 0.0453(18) 0.0518(18) 0.0017(14) -0.0200(15) -0.0293(16) C17 0.068(2) 0.054(2) 0.057(2) 0.0036(15) -0.0218(17) -0.0397(19) C18 0.077(2) 0.063(2) 0.056(2) 0.0132(16) -0.0304(18) -0.045(2) C19 0.0570(19) 0.057(2) 0.0505(19) 0.0040(15) -0.0223(16) -0.0334(17) C20 0.060(2) 0.057(2) 0.0518(19) 0.0037(15) -0.0262(16) -0.0311(18) C21 0.067(2) 0.052(2) 0.063(2) 0.0107(15) -0.0346(18) -0.0392(18) C22 0.083(3) 0.047(2) 0.087(3) 0.0150(17) -0.053(2) -0.039(2) C23 0.082(3) 0.063(2) 0.083(3) 0.0119(19) -0.046(2) -0.049(2) C24 0.085(3) 0.056(2) 0.072(2) -0.0005(17) -0.026(2) -0.048(2) C25 0.084(3) 0.044(2) 0.083(3) 0.0098(17) -0.038(2) -0.033(2) C26 0.070(2) 0.057(2) 0.081(3) 0.0156(18) -0.042(2) -0.035(2) C31 0.062(2) 0.0481(19) 0.0571(19) 0.0075(14) -0.0308(17) -0.0331(17) C32 0.067(2) 0.054(2) 0.057(2) 0.0032(15) -0.0304(17) -0.0341(18) C33 0.078(2) 0.059(2) 0.068(2) 0.0197(17) -0.040(2) -0.042(2) C34 0.075(2) 0.089(3) 0.058(2) 0.0185(19) -0.0374(19) -0.049(2) C35 0.091(3) 0.072(3) 0.056(2) -0.0014(18) -0.030(2) -0.046(2) C36 0.082(3) 0.048(2) 0.067(2) 0.0031(16) -0.037(2) -0.031(2) C41 0.060(2) 0.0483(19) 0.060(2) 0.0069(15) -0.0310(17) -0.0330(17) C42 0.071(2) 0.070(2) 0.058(2) -0.0059(17) -0.0177(18) -0.048(2) C43 0.078(3) 0.077(3) 0.071(2) -0.0170(19) -0.018(2) -0.050(2) C44 0.077(2) 0.061(2) 0.078(3) -0.0004(18) -0.034(2) -0.047(2) C45 0.074(3) 0.078(3) 0.087(3) -0.008(2) -0.016(2) -0.055(2) C46 0.070(2) 0.062(2) 0.074(2) -0.0124(18) -0.015(2) -0.040(2) C51 0.068(2) 0.056(2) 0.0518(19) 0.0052(15) -0.0291(17) -0.0365(19) C52 0.066(2) 0.083(3) 0.054(2) 0.0079(18) -0.0307(19) -0.027(2) C53 0.068(2) 0.088(3) 0.053(2) 0.0022(19) -0.0195(19) -0.028(2) C54 0.082(3) 0.056(2) 0.0467(19) 0.0029(15) -0.030(2) -0.030(2) C55 0.088(3) 0.095(3) 0.077(3) 0.029(2) -0.054(3) -0.046(3) C56 0.066(2) 0.105(3) 0.075(3) 0.019(2) -0.029(2) -0.047(3) C61 0.088(3) 0.074(3) 0.098(4) -0.018(3) -0.050(3) -0.017(3) O1 0.059(3) 0.077(3) 0.096(4) 0.019(3) 0.006(3) -0.019(3) C62 0.060(4) 0.063(4) 0.103(5) 0.024(4) -0.044(4) -0.014(3) C63 0.152(9) 0.063(5) 0.152(8) 0.001(5) -0.071(7) -0.052(6) O1' 0.087(7) 0.098(7) 0.107(7) 0.033(6) -0.026(5) -0.009(5) C62' 0.088(7) 0.098(8) 0.092(8) 0.010(6) -0.025(6) -0.056(6) C63' 0.133(10) 0.142(10) 0.114(9) -0.005(7) -0.029(7) -0.083(8) C64 0.098(4) 0.193(7) 0.146(6) 0.062(5) -0.080(4) -0.053(5) _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 C61 1.922(5) . ? Co1 N2 1.946(3) . ? Co1 N1 1.952(2) . ? Co1 N4 1.955(3) . ? Co1 N3 1.956(2) . ? Cl1 C24 1.748(3) . ? Cl2 C34 1.745(4) . ? Cl3 C44 1.737(3) . ? Cl4 C54 1.741(3) . ? N1 C1 1.382(4) . ? N1 C4 1.400(4) . ? N2 C6 1.383(4) . ? N2 C9 1.383(4) . ? N3 C11 1.377(4) . ? N3 C14 1.385(4) . ? N4 C19 1.378(4) . ? N4 C16 1.386(4) . ? C1 C20 1.372(5) . ? C1 C2 1.434(5) . ? C2 C3 1.331(5) . ? C3 C4 1.441(4) . ? C4 C5 1.382(5) . ? C5 C6 1.393(4) . ? C5 C21 1.490(4) . ? C6 C7 1.427(5) . ? C7 C8 1.342(5) . ? C8 C9 1.431(5) . ? C9 C10 1.403(4) . ? C10 C11 1.376(5) . ? C10 C31 1.503(4) . ? C11 C12 1.442(4) . ? C12 C13 1.335(5) . ? C13 C14 1.429(4) . ? C14 C15 1.383(4) . ? C15 C16 1.393(4) . ? C15 C41 1.496(4) . ? C16 C17 1.430(5) . ? C17 C18 1.339(5) . ? C18 C19 1.432(5) . ? C19 C20 1.400(4) . ? C20 C51 1.497(5) . ? C21 C22 1.388(5) . ? C21 C26 1.391(5) . ? C22 C23 1.391(5) . ? C23 C24 1.372(5) . ? C24 C25 1.359(5) . ? C25 C26 1.388(5) . ? C31 C32 1.380(4) . ? C31 C36 1.389(5) . ? C32 C33 1.378(5) . ? C33 C34 1.384(5) . ? C34 C35 1.373(5) . ? C35 C36 1.374(5) . ? C41 C46 1.376(5) . ? C41 C42 1.384(5) . ? C42 C43 1.391(5) . ? C43 C44 1.345(5) . ? C44 C45 1.383(5) . ? C45 C46 1.392(5) . ? C51 C56 1.370(5) . ? C51 C52 1.380(5) . ? C52 C53 1.391(5) . ? C53 C54 1.363(5) . ? C54 C55 1.348(6) . ? C55 C56 1.386(6) . ? C61 O1 1.314(6) . ? C61 O1' 1.352(8) . ? C61 C62' 1.429(8) . ? C61 C62 1.486(7) . ? C62 C63 1.557(8) . ? C62 C64 1.565(7) . ? C62' C63' 1.535(10) . ? C62' C64 1.550(9) . ? 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 C61 Co1 N2 100.20(19) . . ? C61 Co1 N1 89.22(15) . . ? N2 Co1 N1 89.71(10) . . ? C61 Co1 N4 92.87(19) . . ? N2 Co1 N4 166.93(11) . . ? N1 Co1 N4 90.16(10) . . ? C61 Co1 N3 92.80(15) . . ? N2 Co1 N3 89.79(10) . . ? N1 Co1 N3 177.97(11) . . ? N4 Co1 N3 89.88(10) . . ? C1 N1 C4 104.8(3) . . ? C1 N1 Co1 126.5(2) . . ? C4 N1 Co1 127.2(2) . . ? C6 N2 C9 103.4(3) . . ? C6 N2 Co1 128.6(2) . . ? C9 N2 Co1 128.0(2) . . ? C11 N3 C14 104.9(2) . . ? C11 N3 Co1 127.0(2) . . ? C14 N3 Co1 127.2(2) . . ? C19 N4 C16 104.2(3) . . ? C19 N4 Co1 127.5(2) . . ? C16 N4 Co1 128.4(2) . . ? C20 C1 N1 125.5(3) . . ? C20 C1 C2 123.9(3) . . ? N1 C1 C2 110.5(3) . . ? C3 C2 C1 107.4(3) . . ? C2 C3 C4 107.9(3) . . ? C5 C4 N1 124.7(3) . . ? C5 C4 C3 125.9(3) . . ? N1 C4 C3 109.3(3) . . ? C4 C5 C6 122.5(3) . . ? C4 C5 C21 118.5(3) . . ? C6 C5 C21 119.0(3) . . ? N2 C6 C5 124.5(3) . . ? N2 C6 C7 111.4(3) . . ? C5 C6 C7 123.8(3) . . ? C8 C7 C6 106.8(3) . . ? C7 C8 C9 106.9(3) . . ? N2 C9 C10 124.3(3) . . ? N2 C9 C8 111.1(3) . . ? C10 C9 C8 124.5(3) . . ? C11 C10 C9 122.6(3) . . ? C11 C10 C31 119.4(3) . . ? C9 C10 C31 118.0(3) . . ? C10 C11 N3 124.8(3) . . ? C10 C11 C12 125.0(3) . . ? N3 C11 C12 109.9(3) . . ? C13 C12 C11 107.3(3) . . ? C12 C13 C14 107.4(3) . . ? C15 C14 N3 125.3(3) . . ? C15 C14 C13 124.4(3) . . ? N3 C14 C13 110.3(3) . . ? C14 C15 C16 122.7(3) . . ? C14 C15 C41 118.7(3) . . ? C16 C15 C41 118.6(3) . . ? N4 C16 C15 124.5(3) . . ? N4 C16 C17 110.5(3) . . ? C15 C16 C17 124.8(3) . . ? C18 C17 C16 107.3(3) . . ? C17 C18 C19 106.9(3) . . ? N4 C19 C20 125.0(3) . . ? N4 C19 C18 111.0(3) . . ? C20 C19 C18 124.0(3) . . ? C1 C20 C19 122.6(3) . . ? C1 C20 C51 119.7(3) . . ? C19 C20 C51 117.8(3) . . ? C22 C21 C26 117.8(3) . . ? C22 C21 C5 121.8(3) . . ? C26 C21 C5 120.4(3) . . ? C21 C22 C23 121.6(3) . . ? C24 C23 C22 118.6(3) . . ? C25 C24 C23 121.3(3) . . ? C25 C24 Cl1 119.7(3) . . ? C23 C24 Cl1 118.9(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C21 120.6(3) . . ? C32 C31 C36 117.9(3) . . ? C32 C31 C10 120.7(3) . . ? C36 C31 C10 121.4(3) . . ? C33 C32 C31 121.7(3) . . ? C32 C33 C34 118.4(3) . . ? C35 C34 C33 121.5(3) . . ? C35 C34 Cl2 119.6(3) . . ? C33 C34 Cl2 118.9(3) . . ? C34 C35 C36 118.7(3) . . ? C35 C36 C31 121.7(3) . . ? C46 C41 C42 118.4(3) . . ? C46 C41 C15 122.7(3) . . ? C42 C41 C15 119.0(3) . . ? C41 C42 C43 120.5(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 121.3(3) . . ? C43 C44 Cl3 119.5(3) . . ? C45 C44 Cl3 119.3(3) . . ? C44 C45 C46 118.4(4) . . ? C41 C46 C45 121.4(3) . . ? C56 C51 C52 118.1(3) . . ? C56 C51 C20 121.8(3) . . ? C52 C51 C20 120.1(3) . . ? C51 C52 C53 120.8(3) . . ? C54 C53 C52 119.1(4) . . ? C55 C54 C53 121.3(3) . . ? C55 C54 Cl4 119.6(3) . . ? C53 C54 Cl4 119.1(3) . . ? C54 C55 C56 119.4(4) . . ? C51 C56 C55 121.3(4) . . ? O1 C61 O1' 127.1(6) . . ? O1 C61 C62' 62.4(5) . . ? O1' C61 C62' 111.6(7) . . ? O1 C61 C62 118.4(5) . . ? O1' C61 C62 40.7(5) . . ? C62' C61 C62 73.3(5) . . ? O1 C61 Co1 116.6(4) . . ? O1' C61 Co1 104.8(6) . . ? C62' C61 Co1 131.9(6) . . ? C62 C61 Co1 124.9(4) . . ? C61 C62 C63 101.5(5) . . ? C61 C62 C64 106.4(5) . . ? C63 C62 C64 120.7(7) . . ? C61 C62' C63' 90.0(10) . . ? C61 C62' C64 110.1(7) . . ? C63' C62' C64 113.8(12) . . ? C62' C64 C62 67.9(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.897 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.082 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.016 0.000 0.000 475.1 32.3 _platon_squeeze_details ; ; # === END data_Co(ttp)COCMe(CH2)3COMe 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H47 Co N4 O2' _chemical_formula_weight 854.90 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 21.954(2) _cell_length_b 25.303(2) _cell_length_c 17.5417(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9744.2(16) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15 _exptl_crystal_description bloc _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5543 _exptl_absorpt_correction_T_max 0.6888 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _diffrn_measurement_method 'PHI & OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44714 _diffrn_reflns_av_R_equivalents 0.1079 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8830 _reflns_number_gt 6000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_cell_refinement 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_data_reduction 'BRUKER KAPPA APEXII DUO DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1697P)^2^+1.8713P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.29(3) _refine_ls_number_reflns 8830 _refine_ls_number_parameters 650 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2614 _refine_ls_wR_factor_gt 0.2269 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.003 _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 0.13715(5) 0.5000 1.0000 0.0345(3) Uani 1 2 d S . . Co1 Co 0.0000 0.11394(4) 0.7500 0.0488(4) Uani 1 2 d S . . C1' C 0.0114(2) 0.5474(2) 0.9885(4) 0.0397(14) Uani 1 1 d . . . C2' C -0.0189(3) 0.5969(2) 0.9758(4) 0.0470(17) Uani 1 1 d . . . H2' H -0.0616 0.6022 0.9718 0.056 Uiso 1 1 calc R . . C3' C 0.2929(3) 0.5000 1.0000 0.044(2) Uani 1 2 d S . . C4' C 0.2619(2) 0.4526(3) 1.0074(5) 0.0484(16) Uani 1 1 d . . . C5' C 0.2928(3) 0.4025(3) 1.0110(5) 0.059(2) Uani 1 1 d . . . H5'A H 0.3356 0.3970 1.0094 0.071 Uiso 1 1 calc R . . C6' C 0.2504(3) 0.3655(3) 1.0167(5) 0.063(2) Uani 1 1 d . . . H6'A H 0.2571 0.3285 1.0204 0.076 Uiso 1 1 calc R . . C7' C 0.1923(2) 0.3915(3) 1.0165(4) 0.0463(17) Uani 1 1 d . . . C8' C 0.1377(3) 0.3656(2) 1.0224(4) 0.0495(15) Uani 1 1 d . . . C9' C 0.0820(3) 0.3916(2) 1.0219(4) 0.0439(16) Uani 1 1 d . . . C10 C 0.0000 0.2474(3) 0.7500 0.071(3) Uani 1 2 d S . . C11 C 0.0000 -0.0222(3) 0.7500 0.053(2) Uani 1 2 d S . . C21 C 0.2216(4) 0.1126(3) 0.7756(5) 0.065(2) Uani 1 1 d . . . C22 C 0.2591(5) 0.0952(7) 0.7133(6) 0.141(6) Uani 1 1 d . . . H22A H 0.2402 0.0825 0.6681 0.169 Uiso 1 1 calc R . . C23 C 0.3219(5) 0.0964(7) 0.7176(6) 0.135(6) Uani 1 1 d . . . H23A H 0.3444 0.0849 0.6744 0.162 Uiso 1 1 calc R . . C24 C 0.3526(4) 0.1125(3) 0.7779(6) 0.076(2) Uani 1 1 d . . . C25 C 0.3170(5) 0.1307(7) 0.8372(7) 0.149(7) Uani 1 1 d . . . H25A H 0.3362 0.1479 0.8789 0.178 Uiso 1 1 calc R . . C26 C 0.2533(5) 0.1248(8) 0.8382(7) 0.171(8) Uani 1 1 d . . . H26A H 0.2321 0.1296 0.8849 0.205 Uiso 1 1 calc R . . C27 C 0.4203(4) 0.1140(4) 0.7765(7) 0.101(3) Uani 1 1 d . . . H27A H 0.4350 0.0973 0.7296 0.151 Uiso 1 1 calc R . . H27B H 0.4363 0.0948 0.8208 0.151 Uiso 1 1 calc R . . H27C H 0.4341 0.1508 0.7784 0.151 Uiso 1 1 calc R . . C31 C 0.0000 0.3089(3) 0.7500 0.074(4) Uani 1 2 d S . . C32 C -0.0106(6) 0.3356(3) 0.6865(5) 0.105(4) Uani 1 1 d . . . H32A H -0.0186 0.3166 0.6409 0.126 Uiso 1 1 calc R . . C33 C -0.0105(8) 0.3922(3) 0.6841(5) 0.139(6) Uani 1 1 d . . . H33A H -0.0176 0.4104 0.6375 0.167 Uiso 1 1 calc R . . C34 C 0.0000 0.4195(5) 0.7500 0.174(11) Uani 1 2 d S . . C35 C 0.0000 0.4788(5) 0.7500 0.226(15) Uani 1 2 d SU . . H35A H 0.0077 0.4917 0.8018 0.338 Uiso 0.50 1 calc PR . . H35B H -0.0397 0.4917 0.7324 0.338 Uiso 0.50 1 calc PR . . H35C H 0.0320 0.4917 0.7158 0.338 Uiso 0.50 1 calc PR . . C41 C 0.0000 -0.0818(4) 0.7500 0.065(3) Uani 1 2 d S . . C42 C 0.0183(8) -0.1083(3) 0.6897(8) 0.148(6) Uani 1 1 d . . . H42A H 0.0343 -0.0894 0.6474 0.177 Uiso 1 1 calc R . . C43 C 0.0148(12) -0.1649(5) 0.6859(11) 0.206(10) Uani 1 1 d . . . H43A H 0.0227 -0.1831 0.6396 0.247 Uiso 1 1 calc R . . C44 C 0.0000 -0.1917(6) 0.7500 0.166(12) Uani 1 2 d S . . C45 C 0.0000 -0.2535(5) 0.7500 0.254(18) Uani 1 2 d SU . . H45A H -0.0096 -0.2664 0.8013 0.381 Uiso 0.50 1 calc PR . . H45B H 0.0403 -0.2664 0.7348 0.381 Uiso 0.50 1 calc PR . . H45C H -0.0307 -0.2664 0.7140 0.381 Uiso 0.50 1 calc PR . . C10' C 0.0239(3) 0.3659(3) 1.0292(4) 0.0506(18) Uani 1 1 d . . . H10' H 0.0173 0.3291 1.0362 0.061 Uiso 1 1 calc R . . C11' C -0.0191(3) 0.5000 1.0000 0.0435(19) Uani 1 2 d S . . C21' C 0.3612(4) 0.5000 1.0000 0.048(2) Uani 1 2 d S . . C22' C 0.3929(3) 0.4911(5) 1.0637(5) 0.093(4) Uani 1 1 d . . . H22B H 0.3717 0.4842 1.1099 0.112 Uiso 1 1 calc R . . C23' C 0.4568(3) 0.4917(6) 1.0637(5) 0.101(4) Uani 1 1 d . . . H23' H 0.4778 0.4860 1.1104 0.121 Uiso 1 1 calc R . . C24' C 0.4893(4) 0.5000 1.0000 0.052(2) Uani 1 2 d S . . C25' C 0.5582(4) 0.5000 1.0000 0.071(3) Uani 1 2 d S . . H25B H 0.5731 0.5032 0.9475 0.106 Uiso 0.50 1 calc PR . . H25C H 0.5731 0.4669 1.0222 0.106 Uiso 0.50 1 calc PR . . H25D H 0.5731 0.5299 1.0303 0.106 Uiso 0.50 1 calc PR . . C31' C 0.1369(3) 0.3071(2) 1.0308(4) 0.0523(16) Uani 1 1 d . . . C32' C 0.1396(7) 0.2838(3) 1.1004(6) 0.116(4) Uani 1 1 d . . . H32B H 0.1410 0.3050 1.1450 0.139 Uiso 1 1 calc R . . C33' C 0.1404(7) 0.2278(4) 1.1067(7) 0.125(4) Uani 1 1 d . . . H33B H 0.1435 0.2121 1.1558 0.151 Uiso 1 1 calc R . . C34' C 0.1370(5) 0.1963(3) 1.0448(7) 0.089(3) Uani 1 1 d . . . C35' C 0.1340(5) 0.2203(3) 0.9755(6) 0.085(3) Uani 1 1 d . . . H35D H 0.1308 0.1991 0.9309 0.102 Uiso 1 1 calc R . . C36' C 0.1353(5) 0.2738(3) 0.9682(6) 0.085(3) Uani 1 1 d . . . H36A H 0.1351 0.2888 0.9185 0.102 Uiso 1 1 calc R . . C37' C 0.1371(7) 0.1369(3) 1.0542(8) 0.141(5) Uani 1 1 d . . . H37A H 0.1330 0.1200 1.0042 0.212 Uiso 1 1 calc R . . H37B H 0.1030 0.1263 1.0868 0.212 Uiso 1 1 calc R . . H37C H 0.1755 0.1257 1.0779 0.212 Uiso 1 1 calc R . . C41' C -0.0880(4) 0.5000 1.0000 0.048(2) Uani 1 2 d S . . C42' C -0.1191(3) 0.4910(8) 0.9372(5) 0.131(6) Uani 1 1 d . . . H42B H -0.0983 0.4841 0.8908 0.157 Uiso 1 1 calc R . . C43' C -0.1828(4) 0.4917(9) 0.9384(6) 0.172(8) Uani 1 1 d . . . H43B H -0.2037 0.4858 0.8917 0.207 Uiso 1 1 calc R . . C44' C -0.2160(4) 0.5000 1.0000 0.059(3) Uani 1 2 d S . . C45' C -0.2840(4) 0.5000 1.0000 0.084(4) Uani 1 2 d S . . H45D H -0.2988 0.5067 1.0518 0.126 Uiso 0.50 1 calc PR . . H45E H -0.2988 0.4656 0.9825 0.126 Uiso 0.50 1 calc PR . . H45F H -0.2988 0.5277 0.9657 0.126 Uiso 0.50 1 calc PR . . O1' O 0.0853(5) 0.4974(6) 0.8572(6) 0.089(4) Uani 0.50 1 d PD . . C51' C 0.1323(5) 0.4933(5) 0.8898(7) 0.048(3) Uani 0.50 1 d PD . . C52' C 0.1918(6) 0.4834(8) 0.8482(9) 0.090(6) Uani 0.50 1 d PD . . H52C H 0.2106 0.5180 0.8362 0.108 Uiso 0.50 1 calc PR . . H52D H 0.2197 0.4645 0.8830 0.108 Uiso 0.50 1 calc PR . . C53' C 0.1866(8) 0.4520(7) 0.7750(8) 0.077(5) Uani 0.50 1 d PD . . H53C H 0.2282 0.4568 0.7543 0.093 Uiso 0.50 1 calc PR . . H53D H 0.1610 0.4762 0.7444 0.093 Uiso 0.50 1 calc PR . . C54' C 0.1698(15) 0.3995(7) 0.7391(18) 0.180(16) Uani 0.50 1 d PD . . H54C H 0.1886 0.3934 0.6885 0.216 Uiso 0.50 1 calc PR . . H54D H 0.1255 0.3922 0.7381 0.216 Uiso 0.50 1 calc PR . . O2' O 0.2666(15) 0.3724(13) 0.7141(18) 0.250(15) Uani 0.50 1 d PDU . . C56' C 0.2624(8) 0.3481(9) 0.7732(13) 0.093(7) Uani 0.50 1 d PD . . C55' C 0.2037(9) 0.3729(11) 0.8051(11) 0.28(3) Uani 0.50 1 d PD . . H55A H 0.1778 0.3453 0.8285 0.342 Uiso 0.50 1 calc PR . . H55B H 0.2139 0.3994 0.8447 0.342 Uiso 0.50 1 calc PR . . C57' C 0.3155(15) 0.3222(15) 0.8147(14) 0.23(2) Uani 0.50 1 d PDU . . H57D H 0.3435 0.3067 0.7774 0.338 Uiso 0.50 1 calc PR . . H57E H 0.3001 0.2945 0.8485 0.338 Uiso 0.50 1 calc PR . . H57F H 0.3371 0.3489 0.8449 0.338 Uiso 0.50 1 calc PR . . N1' N 0.0738(2) 0.55487(19) 0.9895(4) 0.0399(13) Uani 1 1 d . . . N2' N 0.2005(2) 0.4459(2) 1.0104(4) 0.0437(13) Uani 1 1 d . . . N1 N 0.0624(3) 0.05886(19) 0.7604(4) 0.0496(15) Uani 1 1 d . . . N2 N 0.0628(3) 0.1691(2) 0.7582(5) 0.071(2) Uani 1 1 d . . . C1 C 0.0537(3) 0.0039(3) 0.7641(4) 0.0503(16) Uani 1 1 d . . . C2 C 0.1100(3) -0.0214(3) 0.7796(5) 0.057(2) Uani 1 1 d . . . H2A H 0.1162 -0.0583 0.7851 0.069 Uiso 1 1 calc R . . C3 C 0.1530(3) 0.0162(3) 0.7850(4) 0.059(2) Uani 1 1 d . . . H3A H 0.1950 0.0108 0.7953 0.071 Uiso 1 1 calc R . . C4 C 0.1240(4) 0.0657(3) 0.7722(4) 0.059(2) Uani 1 1 d . . . C5 C 0.1544(4) 0.1143(3) 0.7706(4) 0.062(2) Uani 1 1 d . . . C6 C 0.1253(4) 0.1613(3) 0.7622(5) 0.067(2) Uani 1 1 d . . . C7 C 0.1564(5) 0.2117(3) 0.7579(7) 0.097(4) Uani 1 1 d . . . H7A H 0.1992 0.2174 0.7584 0.117 Uiso 1 1 calc R . . C8 C 0.1131(4) 0.2484(3) 0.7531(7) 0.092(3) Uani 1 1 d . . . H8A H 0.1196 0.2854 0.7496 0.111 Uiso 1 1 calc R . . C9 C 0.0545(4) 0.2221(2) 0.7541(6) 0.076(3) Uani 1 1 d . . . O1 O 0.0485(7) 0.1176(6) 0.8964(7) 0.108(5) Uani 0.50 1 d PD . . C51 C 0.0059(8) 0.1216(6) 0.8592(8) 0.086(6) Uani 0.50 1 d PD . . C52 C -0.0556(7) 0.1292(8) 0.8979(8) 0.098(6) Uani 0.50 1 d PDU . . H52A H -0.0763 0.0949 0.9060 0.118 Uiso 0.50 1 calc PR . . H52B H -0.0824 0.1525 0.8674 0.118 Uiso 0.50 1 calc PR . . C53 C -0.0385(7) 0.1549(4) 0.9735(7) 0.055(4) Uani 0.50 1 d PD . . H53A H -0.0685 0.1435 1.0123 0.066 Uiso 0.50 1 calc PR . . H53B H 0.0017 0.1410 0.9893 0.066 Uiso 0.50 1 calc PR . . C54 C -0.0354(5) 0.2149(4) 0.9744(8) 0.052(3) Uani 0.50 1 d PD . . H54A H -0.0103 0.2294 0.9325 0.062 Uiso 0.50 1 calc PR . . H54B H -0.0216 0.2292 1.0240 0.062 Uiso 0.50 1 calc PR . . O2 O -0.1059(16) 0.2828(12) 1.0353(13) 0.250(15) Uani 0.50 1 d PDU . . C56 C -0.1192(6) 0.2808(5) 0.9701(12) 0.077(5) Uani 0.50 1 d PD . . C55 C -0.1042(6) 0.2223(6) 0.9612(11) 0.083(5) Uani 0.50 1 d PD . . H55C H -0.1153 0.2101 0.9093 0.099 Uiso 0.50 1 calc PR . . H55D H -0.1275 0.2012 0.9987 0.099 Uiso 0.50 1 calc PR . . C57 C -0.1858(6) 0.2945(7) 0.9556(12) 0.086(6) Uani 0.50 1 d PD . . H57A H -0.1922 0.3323 0.9645 0.130 Uiso 0.50 1 calc PR . . H57B H -0.2117 0.2741 0.9902 0.130 Uiso 0.50 1 calc PR . . H57C H -0.1963 0.2859 0.9027 0.130 Uiso 0.50 1 calc PR . . 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' 0.0311(5) 0.0349(6) 0.0376(6) -0.0039(5) 0.000 0.000 Co1 0.0796(10) 0.0229(5) 0.0438(7) 0.000 -0.0099(6) 0.000 C1' 0.028(3) 0.039(3) 0.053(4) -0.005(3) 0.000(3) 0.001(2) C2' 0.031(3) 0.047(4) 0.063(5) -0.001(3) -0.005(3) 0.011(3) C3' 0.033(4) 0.051(5) 0.049(5) 0.015(5) 0.000 0.000 C4' 0.037(3) 0.054(4) 0.055(4) -0.002(3) -0.004(3) 0.009(3) C5' 0.033(3) 0.056(4) 0.089(6) -0.001(4) 0.001(4) 0.004(3) C6' 0.053(4) 0.050(4) 0.086(7) 0.003(4) 0.000(4) 0.016(4) C7' 0.030(3) 0.047(4) 0.062(5) 0.006(3) 0.002(3) 0.007(3) C8' 0.053(3) 0.039(3) 0.057(4) 0.008(3) 0.001(3) 0.009(3) C9' 0.037(3) 0.038(3) 0.057(5) 0.003(3) 0.004(3) -0.005(3) C10 0.111(9) 0.021(4) 0.081(7) 0.000 -0.046(7) 0.000 C11 0.065(6) 0.027(4) 0.065(6) 0.000 -0.006(5) 0.000 C21 0.086(6) 0.036(4) 0.073(5) 0.004(3) -0.025(5) -0.021(4) C22 0.078(7) 0.29(2) 0.053(6) 0.003(9) -0.016(5) -0.062(9) C23 0.093(8) 0.253(18) 0.058(6) 0.019(8) 0.003(6) -0.063(10) C24 0.077(6) 0.056(4) 0.095(6) 0.016(4) -0.024(5) -0.010(4) C25 0.095(8) 0.246(18) 0.105(9) -0.083(10) -0.049(7) 0.061(10) C26 0.082(8) 0.34(2) 0.089(8) -0.081(12) -0.035(6) 0.041(11) C27 0.092(7) 0.075(6) 0.134(9) 0.001(6) -0.038(6) -0.017(5) C31 0.151(11) 0.017(4) 0.055(6) 0.000 -0.023(7) 0.000 C32 0.208(12) 0.044(4) 0.063(5) 0.000(4) 0.005(7) 0.039(7) C33 0.310(18) 0.033(4) 0.075(6) 0.024(4) 0.069(9) 0.049(8) C34 0.37(3) 0.033(7) 0.114(13) 0.000 0.113(19) 0.000 C35 0.44(4) 0.027(7) 0.21(2) 0.000 0.16(3) 0.000 C41 0.067(7) 0.031(5) 0.098(9) 0.000 -0.031(7) 0.000 C42 0.263(19) 0.021(4) 0.160(12) -0.009(5) 0.022(12) -0.016(7) C43 0.37(3) 0.050(7) 0.194(18) -0.041(9) -0.023(19) 0.044(13) C44 0.180(19) 0.039(8) 0.28(3) 0.000 -0.14(2) 0.000 C45 0.33(4) 0.022(7) 0.41(4) 0.000 -0.16(4) 0.000 C10' 0.040(3) 0.040(3) 0.072(5) -0.005(3) 0.013(3) -0.010(3) C11' 0.029(4) 0.058(5) 0.043(5) -0.014(5) 0.000 0.000 C21' 0.040(4) 0.062(5) 0.042(5) -0.001(5) 0.000 0.000 C22' 0.036(4) 0.190(11) 0.053(5) -0.004(6) 0.006(3) -0.007(6) C23' 0.042(4) 0.209(12) 0.052(5) -0.001(7) -0.010(3) -0.028(7) C24' 0.033(4) 0.065(5) 0.059(5) -0.011(5) 0.000 0.000 C25' 0.042(5) 0.062(7) 0.108(9) -0.018(7) 0.000 0.000 C31' 0.052(4) 0.039(3) 0.066(4) 0.004(3) -0.005(3) 0.007(3) C32' 0.217(13) 0.050(5) 0.081(7) 0.015(4) 0.017(8) 0.028(7) C33' 0.210(14) 0.069(6) 0.098(8) 0.025(6) -0.007(9) 0.007(8) C34' 0.104(7) 0.043(5) 0.120(8) 0.007(5) -0.015(7) 0.018(5) C35' 0.117(8) 0.049(5) 0.090(7) -0.012(4) -0.019(6) -0.007(5) C36' 0.125(8) 0.042(4) 0.088(6) -0.001(4) -0.034(6) -0.011(5) C37' 0.205(13) 0.040(5) 0.179(13) 0.018(6) -0.044(11) 0.012(7) C41' 0.043(4) 0.050(5) 0.052(5) -0.012(5) 0.000 0.000 C42' 0.036(4) 0.303(18) 0.055(6) -0.054(9) 0.009(3) -0.018(8) C43' 0.034(4) 0.40(3) 0.083(7) -0.090(12) -0.006(4) -0.017(10) C44' 0.035(5) 0.065(6) 0.079(7) -0.007(6) 0.000 0.000 C45' 0.039(5) 0.122(11) 0.092(9) -0.041(9) 0.000 0.000 O1' 0.091(8) 0.124(10) 0.052(6) -0.017(7) -0.019(6) 0.033(9) C51' 0.051(7) 0.052(8) 0.042(7) 0.006(6) 0.005(6) -0.004(7) C52' 0.059(10) 0.119(18) 0.092(14) 0.025(12) 0.011(9) -0.017(10) C53' 0.055(9) 0.115(15) 0.061(11) 0.012(10) 0.018(8) -0.015(9) C54' 0.18(3) 0.10(2) 0.26(4) 0.06(3) -0.06(3) 0.051(19) O2' 0.247(17) 0.250(17) 0.252(17) -0.012(10) 0.004(10) -0.001(10) C56' 0.075(12) 0.114(17) 0.089(17) -0.051(13) 0.026(11) 0.002(11) C55' 0.41(6) 0.38(6) 0.073(18) -0.12(3) 0.12(3) -0.30(6) C57' 0.31(5) 0.30(5) 0.067(18) -0.08(2) 0.04(3) 0.01(5) N1' 0.031(2) 0.037(3) 0.052(4) -0.004(2) -0.002(2) -0.0027(19) N2' 0.031(2) 0.045(3) 0.055(4) 0.009(3) 0.004(2) 0.002(2) N1 0.072(4) 0.030(3) 0.047(4) 0.004(3) -0.015(3) -0.005(2) N2 0.099(5) 0.029(3) 0.085(5) 0.009(4) -0.032(4) -0.010(3) C1 0.071(4) 0.030(3) 0.049(4) 0.011(3) -0.011(3) -0.002(3) C2 0.065(4) 0.029(3) 0.077(5) 0.011(3) -0.006(4) -0.001(3) C3 0.064(4) 0.053(4) 0.060(4) 0.007(3) -0.016(3) 0.000(3) C4 0.087(6) 0.035(3) 0.054(5) 0.006(3) -0.019(4) -0.007(3) C5 0.079(5) 0.043(4) 0.064(5) 0.015(3) -0.023(4) -0.017(3) C6 0.087(6) 0.033(3) 0.080(6) 0.011(4) -0.037(5) -0.015(3) C7 0.112(7) 0.040(4) 0.140(9) 0.016(6) -0.054(7) -0.023(4) C8 0.119(8) 0.031(4) 0.128(8) 0.003(5) -0.047(7) -0.022(5) C9 0.121(7) 0.021(3) 0.085(6) -0.001(4) -0.048(5) -0.007(4) O1 0.160(12) 0.116(11) 0.049(7) 0.011(7) -0.043(8) -0.067(10) C51 0.146(18) 0.062(10) 0.049(9) -0.020(7) -0.027(11) -0.025(12) C52 0.108(10) 0.084(9) 0.103(10) 0.023(8) 0.022(8) 0.018(8) C53 0.078(9) 0.031(7) 0.054(8) -0.011(6) 0.005(7) -0.018(6) C54 0.059(8) 0.045(8) 0.052(8) -0.013(6) 0.000(6) -0.015(6) O2 0.236(17) 0.255(17) 0.259(17) -0.022(10) 0.004(10) 0.011(10) C56 0.072(11) 0.052(9) 0.106(15) -0.030(9) -0.005(9) -0.022(8) C55 0.069(11) 0.101(15) 0.078(12) 0.017(11) -0.014(9) 0.014(10) C57 0.071(11) 0.063(11) 0.125(16) -0.023(11) -0.017(11) 0.012(9) _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' C51' 1.944(12) 4_567 ? Co1' C51' 1.944(12) . ? Co1' N2' 1.960(5) . ? Co1' N2' 1.960(5) 4_567 ? Co1' N1' 1.973(5) 4_567 ? Co1' N1' 1.973(5) . ? Co1 C51 1.930(15) . ? Co1 C51 1.930(15) 3_556 ? Co1 N1 1.962(6) . ? Co1 N1 1.962(6) 3_556 ? Co1 N2 1.966(6) 3_556 ? Co1 N2 1.966(6) . ? C1' N1' 1.384(7) . ? C1' C11' 1.389(6) . ? C1' C2' 1.435(8) . ? C2' C10' 1.334(9) 4_567 ? C3' C4' 1.386(7) . ? C3' C4' 1.386(7) 4_567 ? C3' C21' 1.500(12) . ? C4' N2' 1.359(7) . ? C4' C5' 1.440(9) . ? C5' C6' 1.326(9) . ? C6' C7' 1.435(8) . ? C7' C8' 1.370(9) . ? C7' N2' 1.392(8) . ? C8' C9' 1.387(9) . ? C8' C31' 1.489(9) . ? C9' N1' 1.381(8) 4_567 ? C9' C10' 1.437(8) . ? C10 C9 1.358(10) 3_556 ? C10 C9 1.359(10) . ? C10 C31 1.557(12) . ? C11 C1 1.374(7) . ? C11 C1 1.374(7) 3_556 ? C11 C41 1.508(12) . ? C21 C26 1.337(13) . ? C21 C22 1.437(15) . ? C21 C5 1.477(11) . ? C22 C23 1.383(15) . ? C23 C24 1.319(13) . ? C24 C25 1.381(14) . ? C24 C27 1.486(13) . ? C25 C26 1.406(16) . ? C31 C32 1.324(9) . ? C31 C32 1.324(9) 3_556 ? C32 C33 1.432(11) . ? C33 C34 1.368(12) . ? C34 C33 1.368(12) 3_556 ? C34 C35 1.499(18) . ? C41 C42 1.314(13) . ? C41 C42 1.314(13) 3_556 ? C42 C43 1.436(13) . ? C43 C44 1.352(19) . ? C44 C43 1.352(19) 3_556 ? C44 C45 1.56(2) . ? C10' C2' 1.334(9) 4_567 ? C11' C1' 1.389(6) 4_567 ? C11' C41' 1.512(11) . ? C21' C22' 1.335(9) . ? C21' C22' 1.336(9) 4_567 ? C22' C23' 1.403(10) . ? C23' C24' 1.343(9) . ? C24' C23' 1.343(9) 4_567 ? C24' C25' 1.514(12) . ? C31' C32' 1.356(12) . ? C31' C36' 1.385(11) . ? C32' C33' 1.423(12) . ? C33' C34' 1.349(15) . ? C34' C35' 1.361(13) . ? C34' C37' 1.512(11) . ? C35' C36' 1.360(11) . ? C41' C42' 1.316(9) . ? C41' C42' 1.316(9) 4_567 ? C42' C43' 1.398(11) . ? C43' C44' 1.319(10) . ? C44' C43' 1.319(10) 4_567 ? C44' C45' 1.492(13) . ? O1' C51' 1.184(13) . ? C51' C52' 1.516(9) . ? C52' C53' 1.514(10) . ? C53' C54' 1.515(10) . ? C54' C55' 1.532(10) . ? O2' C56' 1.209(9) . ? C56' C57' 1.522(10) . ? C56' C55' 1.538(9) . ? N1' C9' 1.381(8) 4_567 ? N1 C4 1.379(9) . ? N1 C1 1.404(8) . ? N2 C9 1.356(8) . ? N2 C6 1.388(10) . ? C1 C2 1.418(9) . ? C2 C3 1.344(9) . ? C3 C4 1.422(10) . ? C4 C5 1.401(9) . ? C5 C6 1.358(10) . ? C6 C7 1.448(10) . ? C7 C8 1.331(12) . ? C8 C9 1.448(12) . ? O1 C51 1.145(15) . ? C51 C52 1.523(9) . ? C52 C53 1.524(10) . ? C53 C54 1.520(9) . ? C54 C55 1.538(9) . ? O2 C56 1.183(10) . ? C56 C57 1.524(10) . ? C56 C55 1.525(9) . ? 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 C51' Co1' C51' 173.8(6) 4_567 . ? C51' Co1' N2' 90.4(4) 4_567 . ? C51' Co1' N2' 94.0(4) . . ? C51' Co1' N2' 94.0(4) 4_567 4_567 ? C51' Co1' N2' 90.4(4) . 4_567 ? N2' Co1' N2' 89.6(3) . 4_567 ? C51' Co1' N1' 86.0(4) 4_567 4_567 ? C51' Co1' N1' 89.6(4) . 4_567 ? N2' Co1' N1' 89.98(18) . 4_567 ? N2' Co1' N1' 179.6(2) 4_567 4_567 ? C51' Co1' N1' 89.6(4) 4_567 . ? C51' Co1' N1' 86.0(4) . . ? N2' Co1' N1' 179.6(2) . . ? N2' Co1' N1' 89.98(18) 4_567 . ? N1' Co1' N1' 90.4(3) 4_567 . ? C51 Co1 C51 168.5(10) . 3_556 ? C51 Co1 N1 86.1(5) . . ? C51 Co1 N1 102.1(5) 3_556 . ? C51 Co1 N1 102.1(5) . 3_556 ? C51 Co1 N1 86.1(5) 3_556 3_556 ? N1 Co1 N1 89.5(3) . 3_556 ? C51 Co1 N2 92.8(6) . 3_556 ? C51 Co1 N2 79.0(5) 3_556 3_556 ? N1 Co1 N2 178.9(4) . 3_556 ? N1 Co1 N2 90.5(2) 3_556 3_556 ? C51 Co1 N2 79.0(5) . . ? C51 Co1 N2 92.8(6) 3_556 . ? N1 Co1 N2 90.5(2) . . ? N1 Co1 N2 178.9(4) 3_556 . ? N2 Co1 N2 89.6(4) 3_556 . ? N1' C1' C11' 126.4(5) . . ? N1' C1' C2' 110.0(5) . . ? C11' C1' C2' 123.6(5) . . ? C10' C2' C1' 107.4(5) 4_567 . ? C4' C3' C4' 121.1(7) . 4_567 ? C4' C3' C21' 119.5(3) . . ? C4' C3' C21' 119.5(3) 4_567 . ? N2' C4' C3' 126.8(6) . . ? N2' C4' C5' 110.9(6) . . ? C3' C4' C5' 122.2(5) . . ? C6' C5' C4' 107.1(5) . . ? C5' C6' C7' 107.4(6) . . ? C8' C7' N2' 126.3(5) . . ? C8' C7' C6' 123.9(6) . . ? N2' C7' C6' 109.8(5) . . ? C7' C8' C9' 123.0(6) . . ? C7' C8' C31' 119.6(6) . . ? C9' C8' C31' 117.5(6) . . ? N1' C9' C8' 125.4(5) 4_567 . ? N1' C9' C10' 110.0(5) 4_567 . ? C8' C9' C10' 124.5(6) . . ? C9 C10 C9 124.0(9) 3_556 . ? C9 C10 C31 118.0(4) 3_556 . ? C9 C10 C31 118.0(4) . . ? C1 C11 C1 122.5(8) . 3_556 ? C1 C11 C41 118.8(4) . . ? C1 C11 C41 118.8(4) 3_556 . ? C26 C21 C22 113.4(9) . . ? C26 C21 C5 124.2(9) . . ? C22 C21 C5 122.3(7) . . ? C23 C22 C21 121.6(10) . . ? C24 C23 C22 124.0(12) . . ? C23 C24 C25 114.8(10) . . ? C23 C24 C27 120.3(11) . . ? C25 C24 C27 124.7(9) . . ? C24 C25 C26 122.4(11) . . ? C21 C26 C25 122.2(12) . . ? C32 C31 C32 118.6(10) . 3_556 ? C32 C31 C10 120.7(5) . . ? C32 C31 C10 120.7(5) 3_556 . ? C31 C32 C33 122.4(9) . . ? C34 C33 C32 118.7(9) . . ? C33 C34 C33 119.2(11) . 3_556 ? C33 C34 C35 120.4(5) . . ? C33 C34 C35 120.4(5) 3_556 . ? C42 C41 C42 118.7(12) . 3_556 ? C42 C41 C11 120.6(6) . . ? C42 C41 C11 120.6(6) 3_556 . ? C41 C42 C43 122.0(13) . . ? C44 C43 C42 118.4(15) . . ? C43 C44 C43 119.8(16) . 3_556 ? C43 C44 C45 120.1(8) . . ? C43 C44 C45 120.1(8) 3_556 . ? C2' C10' C9' 107.5(6) 4_567 . ? C1' C11' C1' 122.3(7) 4_567 . ? C1' C11' C41' 118.8(3) 4_567 . ? C1' C11' C41' 118.8(3) . . ? C22' C21' C22' 117.3(9) . 4_567 ? C22' C21' C3' 121.3(4) . . ? C22' C21' C3' 121.3(4) 4_567 . ? C21' C22' C23' 121.2(8) . . ? C24' C23' C22' 122.2(7) . . ? C23' C24' C23' 115.8(9) . 4_567 ? C23' C24' C25' 122.1(4) . . ? C23' C24' C25' 122.1(4) 4_567 . ? C32' C31' C36' 116.8(7) . . ? C32' C31' C8' 121.4(7) . . ? C36' C31' C8' 121.8(7) . . ? C31' C32' C33' 120.2(10) . . ? C34' C33' C32' 121.7(10) . . ? C33' C34' C35' 117.3(8) . . ? C33' C34' C37' 119.9(10) . . ? C35' C34' C37' 122.8(10) . . ? C36' C35' C34' 121.8(9) . . ? C35' C36' C31' 122.1(9) . . ? C42' C41' C42' 117.4(9) . 4_567 ? C42' C41' C11' 121.3(5) . . ? C42' C41' C11' 121.3(5) 4_567 . ? C41' C42' C43' 120.3(8) . . ? C44' C43' C42' 124.5(8) . . ? C43' C44' C43' 113.1(9) 4_567 . ? C43' C44' C45' 123.5(5) 4_567 . ? C43' C44' C45' 123.5(5) . . ? O1' C51' C52' 122.2(12) . . ? O1' C51' Co1' 121.2(9) . . ? C52' C51' Co1' 116.5(9) . . ? C53' C52' C51' 115.4(12) . . ? C52' C53' C54' 146(2) . . ? C53' C54' C55' 87.2(19) . . ? O2' C56' C57' 125(3) . . ? O2' C56' C55' 100(2) . . ? C57' C56' C55' 130(2) . . ? C54' C55' C56' 108.1(19) . . ? C9' N1' C1' 105.1(5) 4_567 . ? C9' N1' Co1' 127.7(4) 4_567 . ? C1' N1' Co1' 127.1(4) . . ? C4' N2' C7' 104.7(5) . . ? C4' N2' Co1' 127.8(4) . . ? C7' N2' Co1' 127.3(4) . . ? C4 N1 C1 104.5(5) . . ? C4 N1 Co1 127.6(4) . . ? C1 N1 Co1 127.8(5) . . ? C9 N2 C6 106.0(7) . . ? C9 N2 Co1 127.2(6) . . ? C6 N2 Co1 126.5(5) . . ? C11 C1 N1 125.7(6) . . ? C11 C1 C2 124.4(6) . . ? N1 C1 C2 109.7(6) . . ? C3 C2 C1 107.9(6) . . ? C2 C3 C4 107.2(6) . . ? N1 C4 C5 125.1(7) . . ? N1 C4 C3 110.7(6) . . ? C5 C4 C3 124.2(7) . . ? C6 C5 C4 123.1(7) . . ? C6 C5 C21 120.2(6) . . ? C4 C5 C21 116.7(7) . . ? C5 C6 N2 126.6(6) . . ? C5 C6 C7 123.6(8) . . ? N2 C6 C7 109.8(7) . . ? C8 C7 C6 106.3(8) . . ? C7 C8 C9 108.3(6) . . ? N2 C9 C10 125.8(8) . . ? N2 C9 C8 109.6(8) . . ? C10 C9 C8 124.5(6) . . ? O1 C51 C52 118.8(14) . . ? O1 C51 Co1 127.8(13) . . ? C52 C51 Co1 113.3(11) . . ? C51 C52 C53 102.9(12) . . ? C54 C53 C52 116.5(13) . . ? C53 C54 C55 94.4(10) . . ? O2 C56 C57 113(2) . . ? O2 C56 C55 95.0(18) . . ? C57 C56 C55 114.3(11) . . ? C56 C55 C54 108.4(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.797 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.115 # === END