# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Braga, Dario' 'Gladiali, S.' 'Grepioni, F.' 'Ribeiro, P.' 'Scaccianoce, L.' _publ_contact_author_name 'Dr F Grepioni' _publ_contact_author_address ; Dr F Grepioni Dipartimento di Chimica Universita di Sassari Via Vienna 2 Sassari 07100 ITALY ; data_1 _database_code_CSD 154549 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H37 Co O4' _chemical_formula_weight 760.73 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' '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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z-1/2' '-y-1/2, x-1/2, z-1/4' 'y-1/2, -x-1/2, z-3/4' '-x-1/2, y-1/2, -z-1/4' 'x-1/2, -y-1/2, -z-3/4' 'y, x, -z' '-y, -x, -z-1/2' _cell_length_a 14.3580(7) _cell_length_b 14.3580(7) _cell_length_c 37.944(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7822.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99054 _diffrn_reflns_av_R_equivalents 0.3837 _diffrn_reflns_av_sigmaI/netI 0.8576 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 34.29 _reflns_number_total 15120 _reflns_number_gt 2323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^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 mixed _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 0.01(3) _refine_ls_number_reflns 15120 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.4191 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 0.644 _refine_ls_restrained_S_all 0.644 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.004 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 0.35103(6) 0.83629(6) 0.991788(19) 0.0673(3) Uani 1 1 d . . . C1 C 0.4019(6) 0.8267(8) 1.04113(17) 0.174(5) Uani 1 1 d G . . H1 H 0.3745 0.7960 1.0601 0.209 Uiso 1 1 calc R . . C2 C 0.4647(6) 0.7869(5) 1.0165(3) 0.158(5) Uani 1 1 d G . . H2 H 0.4856 0.7256 1.0164 0.190 Uiso 1 1 calc R . . C3 C 0.4899(4) 0.8571(11) 0.99190(18) 0.173(7) Uani 1 1 d G . . H3 H 0.5303 0.8498 0.9729 0.207 Uiso 1 1 calc R . . C4 C 0.4427(7) 0.9403(6) 1.0014(3) 0.166(6) Uani 1 1 d G . . H4 H 0.4468 0.9971 0.9897 0.200 Uiso 1 1 calc R . . C5 C 0.3883(5) 0.9215(7) 1.0318(3) 0.182(7) Uani 1 1 d G . . H5 H 0.3504 0.9638 1.0436 0.218 Uiso 1 1 calc R . . C6 C 0.2277(4) 0.7753(6) 0.99116(14) 0.110(3) Uani 1 1 d G . . H6 H 0.1979 0.7471 1.0101 0.131 Uiso 1 1 calc R . . C7 C 0.2887(5) 0.7309(3) 0.9670(2) 0.105(3) Uani 1 1 d G . . H7 H 0.3059 0.6685 0.9673 0.126 Uiso 1 1 calc R . . C8 C 0.3190(3) 0.7987(6) 0.94222(12) 0.088(2) Uani 1 1 d G . . H8 H 0.3595 0.7883 0.9235 0.105 Uiso 1 1 calc R . . C9 C 0.2767(5) 0.8849(4) 0.95111(18) 0.099(3) Uani 1 1 d G . . H9 H 0.2846 0.9410 0.9392 0.119 Uiso 1 1 calc R . . C10 C 0.2203(4) 0.8705(6) 0.98136(18) 0.097(3) Uani 1 1 d G . . H10 H 0.1847 0.9155 0.9927 0.117 Uiso 1 1 calc R . . C11 C 0.5132(4) 0.5197(5) 0.95596(16) 0.0553(18) Uani 1 1 d . . . C12 C 0.4948(4) 0.4590(5) 0.98178(15) 0.0501(17) Uani 1 1 d . . . C13 C 0.5119(4) 0.3617(5) 0.97731(14) 0.0525(16) Uani 1 1 d . . . C14 C 0.4927(4) 0.2916(5) 1.00290(15) 0.0706(18) Uani 1 1 d . . . H14 H 0.4664 0.3097 1.0242 0.085 Uiso 1 1 calc R . . C15 C 0.5105(5) 0.2021(5) 0.9979(2) 0.093(3) Uani 1 1 d . . . H15 H 0.4943 0.1585 1.0149 0.112 Uiso 1 1 calc R . . C16 C 0.5554(6) 0.1728(5) 0.9654(2) 0.098(3) Uani 1 1 d . . . H16 H 0.5756 0.1117 0.9624 0.118 Uiso 1 1 calc R . . C17 C 0.5666(5) 0.2352(6) 0.94060(18) 0.086(2) Uani 1 1 d . . . H17 H 0.5879 0.2154 0.9187 0.104 Uiso 1 1 calc R . . C18 C 0.5481(4) 0.3295(5) 0.94527(15) 0.0594(18) Uani 1 1 d . . . C19 C 0.5678(5) 0.3946(6) 0.91953(16) 0.075(2) Uani 1 1 d . . . H19 H 0.5949 0.3738 0.8987 0.090 Uiso 1 1 calc R . . C20 C 0.5501(4) 0.4872(5) 0.92275(15) 0.068(2) Uani 1 1 d . . . H20 H 0.5613 0.5282 0.9042 0.082 Uiso 1 1 calc R . . C21 C -0.0785(6) 0.2909(5) 0.84588(15) 0.0567(18) Uani 1 1 d . . . C22 C -0.1628(7) 0.2832(5) 0.82801(16) 0.079(2) Uani 1 1 d . . . H22 H -0.1761 0.2283 0.8160 0.094 Uiso 1 1 calc R . . C23 C -0.2273(5) 0.3545(6) 0.82760(16) 0.079(2) Uani 1 1 d . . . H23 H -0.2819 0.3477 0.8146 0.095 Uiso 1 1 calc R . . C24 C -0.2110(6) 0.4407(6) 0.84729(17) 0.071(2) Uani 1 1 d . . . C25 C -0.2729(5) 0.5116(6) 0.84920(18) 0.086(2) Uani 1 1 d . . . H25 H -0.3283 0.5074 0.8366 0.103 Uiso 1 1 calc R . . C26 C -0.2563(6) 0.5896(6) 0.8693(2) 0.093(3) Uani 1 1 d . . . H26 H -0.2997 0.6377 0.8695 0.111 Uiso 1 1 calc R . . C27 C -0.1753(6) 0.5974(5) 0.88931(17) 0.081(2) Uani 1 1 d . . . H27 H -0.1650 0.6496 0.9033 0.098 Uiso 1 1 calc R . . C28 C -0.1111(5) 0.5271(5) 0.88816(16) 0.069(2) Uani 1 1 d . . . H28 H -0.0570 0.5316 0.9015 0.083 Uiso 1 1 calc R . . C29 C -0.1266(5) 0.4448(5) 0.86612(16) 0.0596(18) Uani 1 1 d . . . C30 C -0.0570(5) 0.3709(4) 0.86376(14) 0.0505(17) Uani 1 1 d . . . C31 C 0.0343(5) 0.3781(4) 0.88141(14) 0.0480(16) Uani 1 1 d . . . C32 C 0.0956(5) 0.4545(5) 0.87651(15) 0.0598(18) Uani 1 1 d . . . C33 C 0.0764(5) 0.5300(5) 0.85333(17) 0.0675(19) Uani 1 1 d . . . H33 H 0.0210 0.5307 0.8406 0.081 Uiso 1 1 calc R . . C34 C 0.1406(7) 0.6040(5) 0.84935(18) 0.089(2) Uani 1 1 d . . . H34 H 0.1276 0.6531 0.8342 0.107 Uiso 1 1 calc R . . C35 C 0.2237(7) 0.6025(7) 0.8685(2) 0.107(3) Uani 1 1 d . . . H35 H 0.2660 0.6510 0.8658 0.128 Uiso 1 1 calc R . . C36 C 0.2439(7) 0.5328(8) 0.8906(2) 0.107(3) Uani 1 1 d . . . H36 H 0.2984 0.5345 0.9038 0.129 Uiso 1 1 calc R . . C37 C 0.1827(6) 0.4570(6) 0.89388(19) 0.074(2) Uani 1 1 d . . . C38 C 0.2086(6) 0.3792(8) 0.9165(2) 0.098(3) Uani 1 1 d . . . H38 H 0.2643 0.3810 0.9289 0.117 Uiso 1 1 calc R . . C39 C 0.1539(7) 0.3069(6) 0.91940(16) 0.088(2) Uani 1 1 d . . . H39 H 0.1726 0.2555 0.9326 0.106 Uiso 1 1 calc R . . C40 C 0.0676(6) 0.3070(5) 0.90275(17) 0.066(2) Uani 1 1 d . . . C41 C 0.0139(4) 1.0252(5) 0.95658(16) 0.0505(17) Uani 1 1 d . . . C42 C 0.0424(4) 0.9979(5) 0.92242(16) 0.0634(19) Uani 1 1 d . . . H42 H 0.0560 1.0431 0.9056 0.076 Uiso 1 1 calc R . . C43 C 0.0500(5) 0.9076(6) 0.91405(16) 0.071(2) Uani 1 1 d . . . H43 H 0.0710 0.8903 0.8918 0.085 Uiso 1 1 calc R . . C44 C 0.0261(4) 0.8393(6) 0.93889(16) 0.0626(17) Uani 1 1 d . . . C45 C 0.0326(5) 0.7437(6) 0.9317(2) 0.093(3) Uani 1 1 d . . . H45 H 0.0523 0.7241 0.9095 0.112 Uiso 1 1 calc R . . C46 C 0.0099(6) 0.6773(5) 0.9574(3) 0.099(3) Uani 1 1 d . . . H46 H 0.0134 0.6142 0.9521 0.119 Uiso 1 1 calc R . . C47 C -0.0172(6) 0.7045(6) 0.9901(2) 0.105(3) Uani 1 1 d . . . H47 H -0.0316 0.6607 1.0073 0.126 Uiso 1 1 calc R . . C48 C -0.0226(4) 0.7956(5) 0.99691(17) 0.076(2) Uani 1 1 d . . . H48 H -0.0414 0.8128 1.0195 0.092 Uiso 1 1 calc R . . C49 C -0.0027(4) 0.8675(5) 0.97328(14) 0.0499(16) Uani 1 1 d . . . C50 C -0.0081(4) 0.9622(4) 0.98260(13) 0.0407(15) Uani 1 1 d . . . O1 O 0.4960(3) 0.6109(3) 0.96045(10) 0.0760(14) Uani 1 1 d . . . O2 O -0.0244(3) 0.2163(3) 0.84528(10) 0.0767(14) Uani 1 1 d . . . O3 O 0.0158(3) 0.2267(3) 0.90707(9) 0.0836(15) Uani 1 1 d . . . O4 O 0.0063(3) 1.1186(3) 0.96432(8) 0.0713(13) Uani 1 1 d . . . H4A H 0.0093 1.1490 0.9460 0.107 Uiso 1 1 calc R . . H101 H 0.508(3) 0.655(4) 0.9390(13) 0.060(15) Uiso 1 1 d . . . H100 H -0.0079 0.2160 0.8777 0.050 Uiso 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 0.0589(6) 0.0772(7) 0.0659(5) -0.0104(5) -0.0044(5) -0.0080(5) C1 0.146(10) 0.295(19) 0.082(6) -0.087(10) -0.055(6) -0.004(11) C2 0.164(12) 0.160(10) 0.151(10) -0.102(10) -0.096(9) 0.057(9) C3 0.048(5) 0.37(2) 0.103(8) -0.133(12) 0.015(5) -0.006(10) C4 0.112(10) 0.256(16) 0.131(9) -0.045(9) 0.003(7) -0.109(10) C5 0.178(12) 0.111(9) 0.257(16) -0.129(9) -0.132(12) 0.064(9) C6 0.062(6) 0.180(10) 0.087(6) -0.012(7) 0.003(5) -0.053(6) C7 0.148(9) 0.055(5) 0.112(7) -0.017(6) -0.024(6) -0.022(6) C8 0.075(6) 0.137(8) 0.050(4) -0.005(5) -0.003(4) 0.015(6) C9 0.088(7) 0.131(9) 0.080(6) 0.024(5) -0.026(5) 0.015(6) C10 0.055(5) 0.148(9) 0.089(6) -0.035(5) -0.002(5) -0.017(6) C11 0.070(5) 0.053(5) 0.042(4) 0.010(4) 0.007(3) -0.003(4) C12 0.046(4) 0.058(5) 0.046(4) -0.011(3) -0.012(3) -0.014(4) C13 0.059(4) 0.053(5) 0.045(4) -0.005(3) -0.011(3) -0.004(4) C14 0.102(6) 0.053(5) 0.057(4) 0.004(4) 0.011(4) -0.024(4) C15 0.124(7) 0.036(5) 0.119(7) 0.013(5) -0.011(5) -0.019(5) C16 0.149(8) 0.057(6) 0.090(6) -0.020(5) -0.017(5) -0.008(5) C17 0.123(7) 0.083(7) 0.054(5) -0.007(5) -0.005(5) -0.009(5) C18 0.091(5) 0.040(5) 0.048(4) 0.000(4) -0.012(3) 0.009(4) C19 0.100(6) 0.074(6) 0.052(4) -0.020(4) 0.001(4) 0.022(5) C20 0.081(5) 0.088(6) 0.036(4) 0.001(4) 0.005(4) 0.006(5) C21 0.092(6) 0.047(5) 0.031(4) 0.005(3) 0.004(4) -0.014(4) C22 0.126(8) 0.060(5) 0.049(4) -0.012(4) 0.015(5) -0.017(6) C23 0.085(6) 0.092(7) 0.060(4) 0.002(5) 0.000(4) -0.021(6) C24 0.071(6) 0.084(7) 0.058(5) 0.023(4) -0.002(4) 0.009(5) C25 0.074(6) 0.118(7) 0.066(5) 0.014(5) -0.002(4) 0.031(6) C26 0.112(7) 0.096(7) 0.070(5) -0.001(5) 0.026(5) 0.031(5) C27 0.102(7) 0.089(6) 0.053(4) -0.010(4) -0.001(5) 0.015(5) C28 0.069(5) 0.075(6) 0.063(4) 0.006(4) 0.015(3) 0.006(4) C29 0.077(6) 0.052(5) 0.049(4) 0.017(4) 0.014(4) -0.009(4) C30 0.073(5) 0.042(5) 0.037(3) 0.009(3) 0.014(3) 0.000(4) C31 0.068(5) 0.037(4) 0.039(4) 0.003(3) -0.005(3) 0.000(4) C32 0.079(6) 0.064(5) 0.037(4) -0.003(4) 0.015(4) 0.003(4) C33 0.066(5) 0.065(5) 0.071(4) -0.010(4) 0.020(4) -0.002(4) C34 0.130(8) 0.069(6) 0.069(5) 0.001(4) 0.024(5) -0.026(5) C35 0.113(9) 0.108(8) 0.099(7) -0.041(6) 0.033(6) -0.038(6) C36 0.102(8) 0.141(10) 0.079(6) -0.013(6) 0.002(5) 0.011(8) C37 0.082(7) 0.071(6) 0.069(5) -0.004(5) 0.005(5) -0.004(5) C38 0.103(7) 0.108(8) 0.083(6) -0.048(6) 0.002(5) 0.012(7) C39 0.139(8) 0.073(6) 0.051(4) -0.002(4) -0.023(5) 0.000(6) C40 0.089(6) 0.062(6) 0.048(4) -0.014(4) 0.009(4) 0.002(5) C41 0.051(4) 0.054(5) 0.047(4) -0.004(4) 0.001(3) 0.007(4) C42 0.071(5) 0.070(6) 0.049(4) 0.012(4) -0.002(4) 0.000(4) C43 0.106(6) 0.068(6) 0.039(4) -0.007(4) -0.009(4) 0.015(5) C44 0.052(4) 0.062(5) 0.074(5) -0.011(5) -0.023(3) -0.005(4) C45 0.114(7) 0.080(7) 0.086(6) -0.032(5) -0.040(5) 0.025(5) C46 0.142(8) 0.036(5) 0.119(7) -0.024(5) -0.012(6) -0.003(5) C47 0.161(8) 0.062(6) 0.091(6) 0.009(5) -0.005(6) -0.032(6) C48 0.082(5) 0.063(6) 0.083(5) -0.025(5) -0.007(4) -0.004(4) C49 0.060(4) 0.054(5) 0.036(3) 0.002(3) -0.005(3) -0.010(4) C50 0.047(4) 0.040(4) 0.036(3) 0.008(3) -0.006(3) 0.002(3) O1 0.122(4) 0.052(3) 0.053(3) 0.009(2) 0.014(3) 0.009(3) O2 0.124(4) 0.049(3) 0.057(3) -0.004(2) 0.011(2) 0.005(3) O3 0.130(4) 0.070(3) 0.051(3) 0.021(2) 0.008(3) 0.024(3) O4 0.104(4) 0.065(3) 0.045(2) 0.012(2) 0.019(2) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C6 1.975(5) . ? Co1 C10 1.980(5) . ? Co1 C7 1.993(5) . ? Co1 C9 2.002(5) . ? Co1 C8 2.010(4) . ? Co1 C2 2.011(6) . ? Co1 C3 2.017(6) . ? Co1 C1 2.014(5) . ? Co1 C4 2.024(6) . ? Co1 C5 2.022(6) . ? C1 C5 1.4200 . ? C1 C2 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 C7 1.4200 . ? C6 C10 1.4200 . ? C7 C8 1.4200 . ? C8 C9 1.4200 . ? C9 C10 1.4200 . ? C11 C12 1.338(7) . ? C11 O1 1.343(7) . ? C11 C20 1.444(8) . ? C12 C13 1.429(7) . ? C12 C12 1.562(11) 7_557 ? C13 C18 1.400(7) . ? C13 C14 1.425(7) . ? C14 C15 1.324(8) . ? C15 C16 1.452(9) . ? C16 C17 1.310(8) . ? C17 C18 1.391(8) . ? C18 C19 1.382(8) . ? C19 C20 1.359(8) . ? C21 O2 1.324(7) . ? C21 C30 1.369(8) . ? C21 C22 1.393(9) . ? C22 C23 1.380(8) . ? C23 C24 1.465(9) . ? C24 C25 1.353(9) . ? C24 C29 1.408(8) . ? C25 C26 1.375(9) . ? C26 C27 1.394(9) . ? C27 C28 1.368(8) . ? C28 C29 1.464(8) . ? C29 C30 1.460(8) . ? C30 C31 1.476(8) . ? C31 C40 1.388(8) . ? C31 C32 1.419(8) . ? C32 C37 1.413(9) . ? C32 C33 1.423(8) . ? C33 C34 1.414(8) . ? C34 C35 1.397(10) . ? C35 C36 1.339(10) . ? C36 C37 1.403(10) . ? C37 C38 1.457(10) . ? C38 C39 1.306(9) . ? C39 C40 1.391(10) . ? C40 O3 1.380(7) . ? C41 O4 1.377(6) . ? C41 C50 1.377(7) . ? C41 C42 1.414(8) . ? C42 C43 1.339(8) . ? C43 C44 1.403(8) . ? C44 C45 1.402(9) . ? C44 C49 1.428(7) . ? C45 C46 1.405(9) . ? C46 C47 1.356(9) . ? C47 C48 1.336(8) . ? C48 C49 1.397(8) . ? C49 C50 1.407(7) . ? C50 C50 1.452(10) 7_467 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Co1 C10 42.08(9) . . ? C6 Co1 C7 41.93(9) . . ? C10 Co1 C7 70.65(10) . . ? C6 Co1 C9 70.58(11) . . ? C10 Co1 C9 41.78(9) . . ? C7 Co1 C9 70.21(10) . . ? C6 Co1 C8 70.41(10) . . ? C10 Co1 C8 70.31(10) . . ? C7 Co1 C8 41.55(9) . . ? C9 Co1 C8 41.46(8) . . ? C6 Co1 C2 125.2(4) . . ? C10 Co1 C2 161.8(5) . . ? C7 Co1 C2 108.4(2) . . ? C9 Co1 C2 156.1(5) . . ? C8 Co1 C2 121.7(3) . . ? C6 Co1 C3 162.2(5) . . ? C10 Co1 C3 154.3(5) . . ? C7 Co1 C3 123.8(4) . . ? C9 Co1 C3 118.5(4) . . ? C8 Co1 C3 105.5(2) . . ? C2 Co1 C3 41.29(11) . . ? C6 Co1 C1 107.8(2) . . ? C10 Co1 C1 123.1(4) . . ? C7 Co1 C1 123.3(3) . . ? C9 Co1 C1 159.0(5) . . ? C8 Co1 C1 159.1(4) . . ? C2 Co1 C1 41.31(10) . . ? C3 Co1 C1 69.49(12) . . ? C6 Co1 C4 155.8(5) . . ? C10 Co1 C4 118.0(4) . . ? C7 Co1 C4 159.5(5) . . ? C9 Co1 C4 103.2(2) . . ? C8 Co1 C4 121.0(4) . . ? C2 Co1 C4 69.42(12) . . ? C3 Co1 C4 41.15(10) . . ? C1 Co1 C4 69.35(11) . . ? C6 Co1 C5 120.9(4) . . ? C10 Co1 C5 104.5(2) . . ? C7 Co1 C5 158.8(4) . . ? C9 Co1 C5 120.6(4) . . ? C8 Co1 C5 157.8(4) . . ? C2 Co1 C5 69.45(11) . . ? C3 Co1 C5 69.34(12) . . ? C1 Co1 C5 41.19(9) . . ? C4 Co1 C5 41.09(11) . . ? C5 C1 C2 108.0 . . ? C5 C1 Co1 69.7(2) . . ? C2 C1 Co1 69.2(2) . . ? C3 C2 C1 108.0 . . ? C3 C2 Co1 69.6(2) . . ? C1 C2 Co1 69.5(2) . . ? C2 C3 C4 108.0 . . ? C2 C3 Co1 69.1(2) . . ? C4 C3 Co1 69.7(2) . . ? C3 C4 C5 108.0 . . ? C3 C4 Co1 69.2(2) . . ? C5 C4 Co1 69.4(2) . . ? C1 C5 C4 108.0 . . ? C1 C5 Co1 69.1(2) . . ? C4 C5 Co1 69.5(2) . . ? C7 C6 C10 108.0 . . ? C7 C6 Co1 69.73(19) . . ? C10 C6 Co1 69.2(2) . . ? C8 C7 C6 108.0 . . ? C8 C7 Co1 69.85(18) . . ? C6 C7 Co1 68.34(18) . . ? C9 C8 C7 108.0 . . ? C9 C8 Co1 69.0(2) . . ? C7 C8 Co1 68.61(19) . . ? C8 C9 C10 108.0 . . ? C8 C9 Co1 69.58(19) . . ? C10 C9 Co1 68.30(18) . . ? C6 C10 C9 108.0 . . ? C6 C10 Co1 68.76(19) . . ? C9 C10 Co1 69.92(18) . . ? C12 C11 O1 120.4(6) . . ? C12 C11 C20 120.1(6) . . ? O1 C11 C20 119.5(6) . . ? C11 C12 C13 121.1(6) . . ? C11 C12 C12 119.9(6) . 7_557 ? C13 C12 C12 118.9(6) . 7_557 ? C18 C13 C14 115.5(6) . . ? C18 C13 C12 119.3(6) . . ? C14 C13 C12 125.1(6) . . ? C15 C14 C13 123.3(6) . . ? C14 C15 C16 119.3(7) . . ? C17 C16 C15 117.7(7) . . ? C16 C17 C18 123.4(7) . . ? C19 C18 C17 122.0(7) . . ? C19 C18 C13 117.8(6) . . ? C17 C18 C13 120.2(7) . . ? C20 C19 C18 124.1(6) . . ? C19 C20 C11 117.6(6) . . ? O2 C21 C30 123.7(7) . . ? O2 C21 C22 115.9(7) . . ? C30 C21 C22 120.3(7) . . ? C23 C22 C21 122.0(7) . . ? C22 C23 C24 120.9(7) . . ? C25 C24 C29 120.5(8) . . ? C25 C24 C23 123.9(8) . . ? C29 C24 C23 115.6(7) . . ? C24 C25 C26 121.9(8) . . ? C25 C26 C27 120.8(7) . . ? C28 C27 C26 119.1(7) . . ? C27 C28 C29 120.7(7) . . ? C24 C29 C30 121.8(7) . . ? C24 C29 C28 117.0(7) . . ? C30 C29 C28 121.2(7) . . ? C21 C30 C29 119.1(7) . . ? C21 C30 C31 118.9(6) . . ? C29 C30 C31 121.9(6) . . ? C40 C31 C32 115.6(6) . . ? C40 C31 C30 121.2(6) . . ? C32 C31 C30 123.1(6) . . ? C37 C32 C31 120.5(7) . . ? C37 C32 C33 116.1(7) . . ? C31 C32 C33 123.3(7) . . ? C34 C33 C32 120.8(7) . . ? C35 C34 C33 119.3(7) . . ? C36 C35 C34 121.5(9) . . ? C35 C36 C37 120.0(9) . . ? C36 C37 C32 122.1(8) . . ? C36 C37 C38 119.1(9) . . ? C32 C37 C38 118.7(8) . . ? C39 C38 C37 120.4(8) . . ? C38 C39 C40 119.8(8) . . ? O3 C40 C31 119.9(7) . . ? O3 C40 C39 115.1(7) . . ? C31 C40 C39 124.9(7) . . ? O4 C41 C50 118.0(5) . . ? O4 C41 C42 119.2(6) . . ? C50 C41 C42 122.8(6) . . ? C43 C42 C41 120.6(6) . . ? C42 C43 C44 119.9(6) . . ? C45 C44 C43 122.5(7) . . ? C45 C44 C49 118.4(7) . . ? C43 C44 C49 119.1(7) . . ? C44 C45 C46 120.9(7) . . ? C47 C46 C45 120.5(7) . . ? C48 C47 C46 118.4(7) . . ? C47 C48 C49 126.0(7) . . ? C48 C49 C50 122.8(5) . . ? C48 C49 C44 115.9(6) . . ? C50 C49 C44 121.3(6) . . ? C41 C50 C49 116.3(5) . . ? C41 C50 C50 121.8(5) . 7_467 ? C49 C50 C50 121.9(5) . 7_467 ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 34.29 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.019 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.062 data_2 _database_code_CSD 154550 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 Co O3' _chemical_formula_weight 617.57 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' '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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.2613(4) _cell_length_b 13.2613(4) _cell_length_c 33.4406(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5880.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83597 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0802 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 33.98 _reflns_number_total 11365 _reflns_number_gt 5210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^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 mixed _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 -0.006(9) _refine_ls_number_reflns 11365 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.840088(18) 0.145915(16) 0.117920(6) 0.05162(7) Uani 1 1 d . . . C1 C 0.94917(16) 0.06534(19) 0.09050(6) 0.0813(7) Uani 1 1 d . . . H1 H 0.9406 0.0239 0.0683 0.098 Uiso 1 1 calc R . . C2 C 0.97257(14) 0.1686(2) 0.08957(6) 0.0784(6) Uani 1 1 d . . . H2 H 0.9822 0.2076 0.0668 0.094 Uiso 1 1 calc R . . C3 C 0.97876(14) 0.20253(16) 0.12959(7) 0.0730(6) Uani 1 1 d . . . H3 H 0.9929 0.2679 0.1379 0.088 Uiso 1 1 calc R . . C4 C 0.95975(15) 0.11994(16) 0.15439(6) 0.0712(6) Uani 1 1 d . . . H4 H 0.9597 0.1211 0.1822 0.085 Uiso 1 1 calc R . . C5 C 0.94087(17) 0.03542(16) 0.13065(7) 0.0803(6) Uani 1 1 d . . . H5 H 0.9256 -0.0290 0.1398 0.096 Uiso 1 1 calc R . . C6 C 0.73435(14) 0.21585(17) 0.08426(6) 0.0702(6) Uani 1 1 d . . . H6 H 0.7456 0.2499 0.0604 0.084 Uiso 1 1 calc R . . C7 C 0.73725(13) 0.25841(14) 0.12278(6) 0.0638(5) Uani 1 1 d . . . H7 H 0.7504 0.3256 0.1289 0.077 Uiso 1 1 calc R . . C8 C 0.71670(14) 0.18127(15) 0.15043(5) 0.0626(5) Uani 1 1 d . . . H8 H 0.7144 0.1883 0.1781 0.075 Uiso 1 1 calc R . . C9 C 0.70038(15) 0.09215(14) 0.12910(6) 0.0690(5) Uani 1 1 d . . . H9 H 0.6848 0.0296 0.1400 0.083 Uiso 1 1 calc R . . C10 C 0.71165(15) 0.11367(17) 0.08824(6) 0.0716(6) Uani 1 1 d . . . H10 H 0.7051 0.0677 0.0674 0.086 Uiso 1 1 calc R . . C11 C 0.91783(14) 0.26761(12) -0.01025(4) 0.0477(4) Uani 1 1 d . . . C12 C 1.00519(15) 0.21442(14) -0.02299(5) 0.0593(5) Uani 1 1 d . . . H12 H 0.9991 0.1476 -0.0311 0.071 Uiso 1 1 calc R . . C13 C 1.09652(16) 0.25861(14) -0.02353(5) 0.0644(5) Uani 1 1 d . . . H13 H 1.1522 0.2215 -0.0318 0.077 Uiso 1 1 calc R . . C14 C 1.10991(14) 0.36102(15) -0.01173(5) 0.0577(5) Uani 1 1 d . . . C15 C 1.20475(15) 0.40907(19) -0.01316(6) 0.0765(6) Uani 1 1 d . . . H15 H 1.2610 0.3729 -0.0215 0.092 Uiso 1 1 calc R . . C16 C 1.21526(16) 0.50724(18) -0.00249(7) 0.0826(6) Uani 1 1 d . . . H16 H 1.2787 0.5371 -0.0028 0.099 Uiso 1 1 calc R . . C17 C 1.13138(15) 0.56341(15) 0.00898(6) 0.0690(5) Uani 1 1 d . . . H17 H 1.1387 0.6313 0.0153 0.083 Uiso 1 1 calc R . . C18 C 1.03841(14) 0.51930(13) 0.01095(5) 0.0558(5) Uani 1 1 d . . . H18 H 0.9831 0.5580 0.0185 0.067 Uiso 1 1 calc R . . C19 C 1.02423(12) 0.41561(12) 0.00165(5) 0.0467(4) Uani 1 1 d . . . C20 C 0.92804(12) 0.36594(11) 0.00423(4) 0.0432(4) Uani 1 1 d . . . C21 C 0.84262(13) 0.46189(10) 0.06094(4) 0.0450(4) Uani 1 1 d . . . C22 C 0.74966(12) 0.42623(12) 0.00030(5) 0.0500(4) Uani 1 1 d . . . C23 C 0.66822(15) 0.48271(13) 0.01510(6) 0.0637(5) Uani 1 1 d . . . H23 H 0.6099 0.4889 -0.0001 0.076 Uiso 1 1 calc R . . C24 C 0.67366(16) 0.52841(13) 0.05139(6) 0.0698(5) Uani 1 1 d . . . H24 H 0.6199 0.5675 0.0603 0.084 Uiso 1 1 calc R . . C25 C 0.75931(14) 0.51756(12) 0.07569(5) 0.0560(5) Uani 1 1 d . . . C26 C 0.76433(17) 0.55787(13) 0.11499(6) 0.0704(6) Uani 1 1 d . . . H26 H 0.7098 0.5944 0.1248 0.084 Uiso 1 1 calc R . . C27 C 0.8466(2) 0.54447(14) 0.13863(6) 0.0747(6) Uani 1 1 d . . . H27 H 0.8489 0.5730 0.1640 0.090 Uiso 1 1 calc R . . C28 C 0.92710(16) 0.48790(14) 0.12454(5) 0.0654(5) Uani 1 1 d . . . H28 H 0.9827 0.4770 0.1409 0.078 Uiso 1 1 calc R . . C29 C 0.92557(14) 0.44807(12) 0.08691(4) 0.0518(4) Uani 1 1 d . . . H29 H 0.9807 0.4108 0.0781 0.062 Uiso 1 1 calc R . . C30 C 0.83882(12) 0.41919(10) 0.02131(4) 0.0416(3) Uani 1 1 d . . . C31 C 0.82145(11) -0.03305(11) -0.02889(4) 0.0403(3) Uani 1 1 d . . . C32 C 0.83637(10) -0.13400(10) -0.02068(4) 0.0366(3) Uani 1 1 d . . . C33 C 0.83022(10) -0.20622(11) -0.05169(4) 0.0386(3) Uani 1 1 d . . . C34 C 0.84346(12) -0.31068(11) -0.04447(5) 0.0479(4) Uani 1 1 d . . . H34 H 0.8512 -0.3334 -0.0183 0.057 Uiso 1 1 calc R . . C35 C 0.84503(13) -0.37851(12) -0.07512(5) 0.0569(4) Uani 1 1 d . . . H35 H 0.8543 -0.4467 -0.0698 0.068 Uiso 1 1 calc R . . C36 C 0.83268(12) -0.34578(14) -0.11448(5) 0.0582(4) Uani 1 1 d . . . H36 H 0.8367 -0.3920 -0.1353 0.070 Uiso 1 1 calc R . . C37 C 0.81491(12) -0.24752(13) -0.12262(5) 0.0555(4) Uani 1 1 d . . . H37 H 0.8046 -0.2277 -0.1490 0.067 Uiso 1 1 calc R . . C38 C 0.81166(11) -0.17371(12) -0.09167(4) 0.0447(4) Uani 1 1 d . . . C39 C 0.79463(12) -0.07083(13) -0.09857(5) 0.0490(4) Uani 1 1 d . . . H39 H 0.7796 -0.0491 -0.1243 0.059 Uiso 1 1 calc R . . C40 C 0.79954(12) -0.00201(12) -0.06838(4) 0.0461(4) Uani 1 1 d . . . H40 H 0.7884 0.0659 -0.0738 0.055 Uiso 1 1 calc R . . O1 O 0.82879(10) 0.22280(8) -0.01262(3) 0.0557(3) Uani 1 1 d . . . O2 O 0.73521(10) 0.37910(10) -0.03555(4) 0.0634(4) Uani 1 1 d . . . O3 O 0.82791(9) 0.03347(9) 0.00158(3) 0.0525(3) Uani 1 1 d . . . H101 H 0.8346(13) 0.0933(15) -0.0062(5) 0.067(6) Uiso 1 1 d . . . H100 H 0.7660(14) 0.3197(15) -0.0312(6) 0.072(6) Uiso 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 0.05697(15) 0.05113(14) 0.04675(11) -0.00521(10) -0.00487(10) 0.00086(11) C1 0.0747(15) 0.0972(18) 0.0721(14) -0.0317(13) -0.0106(11) 0.0238(13) C2 0.0537(12) 0.114(2) 0.0675(13) 0.0033(13) 0.0039(10) 0.0103(12) C3 0.0554(12) 0.0704(13) 0.0931(16) -0.0100(13) -0.0147(11) 0.0006(10) C4 0.0776(14) 0.0757(15) 0.0602(12) -0.0115(11) -0.0211(10) 0.0164(11) C5 0.0926(16) 0.0635(13) 0.0849(15) -0.0126(12) -0.0250(13) 0.0201(11) C6 0.0581(12) 0.0917(17) 0.0609(12) 0.0207(11) -0.0054(9) 0.0017(11) C7 0.0559(12) 0.0503(11) 0.0852(14) -0.0011(10) 0.0005(10) 0.0011(8) C8 0.0654(12) 0.0699(13) 0.0524(10) -0.0090(9) 0.0072(9) -0.0027(10) C9 0.0678(12) 0.0540(11) 0.0852(15) 0.0028(11) 0.0029(11) -0.0120(9) C10 0.0602(12) 0.0892(16) 0.0653(13) -0.0214(11) -0.0100(10) -0.0076(11) C11 0.0634(12) 0.0450(10) 0.0347(8) 0.0036(7) 0.0057(7) 0.0126(8) C12 0.0829(15) 0.0457(11) 0.0495(10) -0.0012(8) 0.0128(9) 0.0142(10) C13 0.0754(14) 0.0641(13) 0.0539(11) 0.0033(9) 0.0218(10) 0.0283(11) C14 0.0625(12) 0.0643(12) 0.0462(10) 0.0097(8) 0.0127(8) 0.0123(9) C15 0.0628(14) 0.0856(16) 0.0812(15) 0.0131(12) 0.0262(11) 0.0129(11) C16 0.0600(13) 0.0923(18) 0.0955(16) 0.0114(14) 0.0209(12) -0.0103(11) C17 0.0701(14) 0.0618(12) 0.0751(13) 0.0094(10) 0.0113(10) -0.0097(10) C18 0.0629(12) 0.0523(11) 0.0521(11) 0.0077(8) 0.0084(9) 0.0035(9) C19 0.0576(10) 0.0454(9) 0.0370(8) 0.0067(7) 0.0072(8) 0.0081(8) C20 0.0554(10) 0.0421(9) 0.0321(7) 0.0032(7) 0.0044(7) 0.0075(7) C21 0.0597(10) 0.0320(8) 0.0431(8) 0.0000(6) 0.0118(8) -0.0018(7) C22 0.0627(11) 0.0370(9) 0.0504(9) 0.0037(8) 0.0002(9) 0.0055(8) C23 0.0534(11) 0.0543(11) 0.0834(14) 0.0021(10) -0.0013(10) 0.0149(9) C24 0.0640(13) 0.0493(11) 0.0960(15) -0.0075(10) 0.0217(11) 0.0154(9) C25 0.0662(12) 0.0366(9) 0.0652(11) -0.0065(8) 0.0213(10) -0.0003(8) C26 0.0894(16) 0.0445(11) 0.0772(13) -0.0192(10) 0.0393(12) -0.0077(9) C27 0.1098(18) 0.0620(12) 0.0524(11) -0.0160(9) 0.0233(13) -0.0239(13) C28 0.0912(14) 0.0597(11) 0.0451(10) -0.0096(8) 0.0036(10) -0.0204(11) C29 0.0665(11) 0.0456(10) 0.0433(9) -0.0044(7) 0.0069(8) -0.0041(8) C30 0.0500(9) 0.0326(8) 0.0423(8) 0.0015(6) 0.0050(7) 0.0057(7) C31 0.0400(9) 0.0444(9) 0.0366(8) 0.0012(7) -0.0028(6) 0.0072(7) C32 0.0350(8) 0.0385(8) 0.0362(7) 0.0034(6) -0.0035(6) 0.0036(6) C33 0.0337(8) 0.0421(8) 0.0401(8) -0.0017(6) -0.0038(6) 0.0015(6) C34 0.0498(10) 0.0444(9) 0.0494(9) 0.0008(7) -0.0055(8) -0.0009(8) C35 0.0549(10) 0.0422(9) 0.0736(12) -0.0108(8) -0.0082(9) -0.0045(8) C36 0.0511(10) 0.0597(11) 0.0636(11) -0.0247(9) -0.0132(8) -0.0018(9) C37 0.0522(10) 0.0702(12) 0.0440(9) -0.0114(8) -0.0147(8) -0.0010(8) C38 0.0388(8) 0.0550(10) 0.0403(8) -0.0053(7) -0.0099(6) 0.0027(7) C39 0.0486(10) 0.0583(11) 0.0400(9) 0.0085(8) -0.0125(7) 0.0077(8) C40 0.0521(10) 0.0427(9) 0.0436(9) 0.0057(7) -0.0083(7) 0.0097(7) O1 0.0714(9) 0.0403(6) 0.0555(7) -0.0040(5) -0.0009(6) 0.0051(6) O2 0.0799(9) 0.0535(8) 0.0567(8) -0.0026(6) -0.0176(6) 0.0125(7) O3 0.0811(9) 0.0368(6) 0.0397(6) -0.0015(5) -0.0047(6) 0.0055(6) _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 C10 2.0172(19) . ? Co1 C1 2.019(2) . ? Co1 C2 2.019(2) . ? Co1 C8 2.0198(18) . ? Co1 C9 2.0201(19) . ? Co1 C6 2.0232(19) . ? Co1 C3 2.0243(18) . ? Co1 C7 2.0277(18) . ? Co1 C5 2.028(2) . ? Co1 C4 2.0309(18) . ? C1 C5 1.404(3) . ? C1 C2 1.405(3) . ? C2 C3 1.414(3) . ? C3 C4 1.397(3) . ? C4 C5 1.396(3) . ? C6 C10 1.394(3) . ? C6 C7 1.407(3) . ? C7 C8 1.406(3) . ? C8 C9 1.397(2) . ? C9 C10 1.404(3) . ? C11 O1 1.324(2) . ? C11 C20 1.398(2) . ? C11 C12 1.422(2) . ? C12 C13 1.346(3) . ? C13 C14 1.425(3) . ? C14 C15 1.411(3) . ? C14 C19 1.420(2) . ? C15 C16 1.357(3) . ? C16 C17 1.393(3) . ? C17 C18 1.366(2) . ? C18 C19 1.422(2) . ? C19 C20 1.438(2) . ? C20 C30 1.492(2) . ? C21 C29 1.413(2) . ? C21 C25 1.417(2) . ? C21 C30 1.4422(19) . ? C22 O2 1.366(2) . ? C22 C30 1.379(2) . ? C22 C23 1.404(2) . ? C23 C24 1.358(3) . ? C24 C25 1.404(3) . ? C25 C26 1.420(3) . ? C26 C27 1.359(3) . ? C27 C28 1.387(3) . ? C28 C29 1.365(2) . ? C31 O3 1.3503(18) . ? C31 C32 1.381(2) . ? C31 C40 1.4134(19) . ? C32 C33 1.4140(19) . ? C32 C32 1.490(3) 7_645 ? C33 C34 1.417(2) . ? C33 C38 1.4264(19) . ? C34 C35 1.364(2) . ? C35 C36 1.396(2) . ? C36 C37 1.352(2) . ? C37 C38 1.425(2) . ? C38 C39 1.402(2) . ? C39 C40 1.362(2) . ? 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 C10 Co1 C1 105.63(9) . . ? C10 Co1 C2 122.37(9) . . ? C1 Co1 C2 40.72(10) . . ? C10 Co1 C8 68.29(8) . . ? C1 Co1 C8 161.43(10) . . ? C2 Co1 C8 157.39(9) . . ? C10 Co1 C9 40.70(8) . . ? C1 Co1 C9 123.67(10) . . ? C2 Co1 C9 159.66(9) . . ? C8 Co1 C9 40.47(7) . . ? C10 Co1 C6 40.38(8) . . ? C1 Co1 C6 119.12(8) . . ? C2 Co1 C6 105.87(8) . . ? C8 Co1 C6 68.38(8) . . ? C9 Co1 C6 68.23(8) . . ? C10 Co1 C3 160.14(9) . . ? C1 Co1 C3 68.46(9) . . ? C2 Co1 C3 40.95(8) . . ? C8 Co1 C3 123.10(8) . . ? C9 Co1 C3 158.19(9) . . ? C6 Co1 C3 124.53(8) . . ? C10 Co1 C7 68.13(8) . . ? C1 Co1 C7 155.20(9) . . ? C2 Co1 C7 120.87(9) . . ? C8 Co1 C7 40.64(7) . . ? C9 Co1 C7 68.16(7) . . ? C6 Co1 C7 40.64(8) . . ? C3 Co1 C7 108.82(8) . . ? C10 Co1 C5 120.43(9) . . ? C1 Co1 C5 40.61(8) . . ? C2 Co1 C5 68.47(10) . . ? C8 Co1 C5 126.05(9) . . ? C9 Co1 C5 108.09(10) . . ? C6 Co1 C5 154.77(9) . . ? C3 Co1 C5 68.21(9) . . ? C7 Co1 C5 163.28(8) . . ? C10 Co1 C4 156.82(9) . . ? C1 Co1 C4 67.86(8) . . ? C2 Co1 C4 68.13(9) . . ? C8 Co1 C4 110.43(8) . . ? C9 Co1 C4 123.06(9) . . ? C6 Co1 C4 162.44(9) . . ? C3 Co1 C4 40.30(8) . . ? C7 Co1 C4 127.02(8) . . ? C5 Co1 C4 40.23(8) . . ? C5 C1 C2 108.31(19) . . ? C5 C1 Co1 70.07(11) . . ? C2 C1 Co1 69.66(11) . . ? C1 C2 C3 107.55(19) . . ? C1 C2 Co1 69.62(13) . . ? C3 C2 Co1 69.73(11) . . ? C4 C3 C2 107.60(19) . . ? C4 C3 Co1 70.10(11) . . ? C2 C3 Co1 69.33(11) . . ? C5 C4 C3 108.91(18) . . ? C5 C4 Co1 69.79(11) . . ? C3 C4 Co1 69.60(11) . . ? C4 C5 C1 107.6(2) . . ? C4 C5 Co1 69.98(11) . . ? C1 C5 Co1 69.32(12) . . ? C10 C6 C7 107.96(18) . . ? C10 C6 Co1 69.58(12) . . ? C7 C6 Co1 69.85(11) . . ? C8 C7 C6 107.76(17) . . ? C8 C7 Co1 69.38(11) . . ? C6 C7 Co1 69.50(11) . . ? C9 C8 C7 108.04(16) . . ? C9 C8 Co1 69.78(11) . . ? C7 C8 Co1 69.98(10) . . ? C8 C9 C10 107.97(17) . . ? C8 C9 Co1 69.75(11) . . ? C10 C9 Co1 69.54(11) . . ? C6 C10 C9 108.26(17) . . ? C6 C10 Co1 70.04(12) . . ? C9 C10 Co1 69.76(11) . . ? O1 C11 C20 121.72(14) . . ? O1 C11 C12 119.08(15) . . ? C20 C11 C12 119.20(17) . . ? C13 C12 C11 121.43(17) . . ? C12 C13 C14 121.55(17) . . ? C15 C14 C19 119.59(18) . . ? C15 C14 C13 122.14(18) . . ? C19 C14 C13 118.26(17) . . ? C16 C15 C14 121.06(19) . . ? C15 C16 C17 120.24(19) . . ? C18 C17 C16 120.33(19) . . ? C17 C18 C19 121.51(17) . . ? C14 C19 C18 117.14(16) . . ? C14 C19 C20 119.68(15) . . ? C18 C19 C20 123.15(15) . . ? C11 C20 C19 119.50(14) . . ? C11 C20 C30 119.84(14) . . ? C19 C20 C30 120.65(13) . . ? C29 C21 C25 117.41(14) . . ? C29 C21 C30 122.75(14) . . ? C25 C21 C30 119.81(16) . . ? O2 C22 C30 122.46(15) . . ? O2 C22 C23 116.46(16) . . ? C30 C22 C23 121.08(16) . . ? C24 C23 C22 120.79(19) . . ? C23 C24 C25 120.96(17) . . ? C24 C25 C21 118.84(16) . . ? C24 C25 C26 122.34(18) . . ? C21 C25 C26 118.79(18) . . ? C27 C26 C25 121.78(18) . . ? C26 C27 C28 119.40(17) . . ? C29 C28 C27 120.7(2) . . ? C28 C29 C21 121.86(18) . . ? C22 C30 C21 118.14(14) . . ? C22 C30 C20 121.16(13) . . ? C21 C30 C20 120.66(14) . . ? O3 C31 C32 118.30(13) . . ? O3 C31 C40 121.85(14) . . ? C32 C31 C40 119.84(14) . . ? C31 C32 C33 120.17(13) . . ? C31 C32 C32 118.55(13) . 7_645 ? C33 C32 C32 121.14(13) . 7_645 ? C32 C33 C34 122.01(13) . . ? C32 C33 C38 119.52(13) . . ? C34 C33 C38 118.47(13) . . ? C35 C34 C33 121.23(15) . . ? C34 C35 C36 120.12(16) . . ? C37 C36 C35 120.67(16) . . ? C36 C37 C38 121.42(16) . . ? C39 C38 C37 123.64(14) . . ? C39 C38 C33 118.43(13) . . ? C37 C38 C33 117.89(15) . . ? C40 C39 C38 121.49(14) . . ? C39 C40 C31 120.46(15) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 33.98 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.147 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.033 data_3 _database_code_CSD 154551 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51.50 H41.50 Co N1.50 O7' _chemical_formula_weight 852.29 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' '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' 'N' 'N' 0.0061 0.0033 '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 10.4464(16) _cell_length_b 14.850(2) _cell_length_c 15.985(2) _cell_angle_alpha 68.894(5) _cell_angle_beta 80.311(5) _cell_angle_gamma 87.814(5) _cell_volume 2279.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32872 _diffrn_reflns_av_R_equivalents 0.0988 _diffrn_reflns_av_sigmaI/netI 0.4160 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 34.04 _reflns_number_total 16744 _reflns_number_gt 3177 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1110P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16744 _refine_ls_number_parameters 513 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.3358 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2554 _refine_ls_wR_factor_gt 0.1959 _refine_ls_goodness_of_fit_ref 0.717 _refine_ls_restrained_S_all 0.721 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.15013(6) 0.15131(4) 0.06056(4) 0.0701(3) Uani 1 1 d . . . C1 C 0.3118(9) 0.1248(5) -0.0208(7) 0.083(3) Uiso 0.55 1 d PG A 1 H1 H 0.3733 0.0783 -0.0011 0.099 Uiso 0.55 1 calc PR A 1 C2 C 0.1943(10) 0.1100(6) -0.0482(8) 0.128(5) Uiso 0.55 1 d PG A 1 H2 H 0.1653 0.0522 -0.0496 0.153 Uiso 0.55 1 calc PR A 1 C3 C 0.1287(9) 0.1989(8) -0.0730(9) 0.158(8) Uiso 0.55 1 d PG A 1 H3 H 0.0494 0.2097 -0.0935 0.190 Uiso 0.55 1 calc PR A 1 C4 C 0.2057(9) 0.2687(5) -0.0609(8) 0.089(4) Uiso 0.55 1 d PG A 1 H4 H 0.1856 0.3331 -0.0722 0.107 Uiso 0.55 1 calc PR A 1 C5 C 0.3188(8) 0.2228(5) -0.0287(6) 0.090(3) Uiso 0.55 1 d PG A 1 H5 H 0.3858 0.2519 -0.0151 0.108 Uiso 0.55 1 calc PR A 1 C6 C 0.1246(19) 0.0541(7) 0.1859(12) 0.123(5) Uiso 0.50 1 d PG A 1 H6 H 0.1678 -0.0038 0.2052 0.148 Uiso 0.50 1 calc PR A 1 C7 C 0.010(2) 0.0695(13) 0.1458(14) 0.276(14) Uiso 0.50 1 d PG A 1 H7 H -0.0342 0.0234 0.1342 0.331 Uiso 0.50 1 calc PR A 1 C8 C -0.0236(13) 0.1676(14) 0.1265(12) 0.186(12) Uiso 0.50 1 d PG A 1 H8 H -0.0944 0.1970 0.1000 0.223 Uiso 0.50 1 calc PR A 1 C9 C 0.0695(13) 0.2128(7) 0.1547(8) 0.112(4) Uiso 0.50 1 d PG A 1 H9 H 0.0704 0.2771 0.1499 0.134 Uiso 0.50 1 calc PR A 1 C10 C 0.1611(11) 0.1427(11) 0.1914(10) 0.161(6) Uiso 0.50 1 d PG A 1 H10 H 0.2325 0.1530 0.2149 0.193 Uiso 0.50 1 calc PR A 1 C1' C 0.2426(11) 0.1230(6) -0.0492(7) 0.089(4) Uiso 0.45 1 d PG A 2 H1' H 0.2356 0.0681 -0.0633 0.106 Uiso 0.45 1 calc PR A 2 C2' C 0.1627(10) 0.2050(7) -0.0728(8) 0.082(4) Uiso 0.45 1 d PG A 2 H2' H 0.0942 0.2130 -0.1051 0.098 Uiso 0.45 1 calc PR A 2 C3' C 0.2058(11) 0.2724(6) -0.0386(9) 0.110(7) Uiso 0.45 1 d PG A 2 H3' H 0.1705 0.3324 -0.0445 0.132 Uiso 0.45 1 calc PR A 2 C4' C 0.3123(10) 0.2321(7) 0.0062(7) 0.092(4) Uiso 0.45 1 d PG A 2 H4' H 0.3590 0.2611 0.0348 0.110 Uiso 0.45 1 calc PR A 2 C5' C 0.3350(9) 0.1398(6) -0.0004(7) 0.077(4) Uiso 0.45 1 d PG A 2 H5' H 0.3992 0.0978 0.0232 0.092 Uiso 0.45 1 calc PR A 2 C6' C 0.1595(10) 0.0774(13) 0.1958(9) 0.119(6) Uiso 0.50 1 d PG A 2 H6' H 0.2330 0.0538 0.2216 0.143 Uiso 0.50 1 calc PR A 2 C7' C 0.0835(11) 0.0286(6) 0.1588(8) 0.098(4) Uiso 0.50 1 d PG A 2 H7' H 0.0986 -0.0325 0.1560 0.118 Uiso 0.50 1 calc PR A 2 C8' C -0.0195(10) 0.0894(8) 0.1266(9) 0.140(6) Uiso 0.50 1 d PG A 2 H8' H -0.0837 0.0752 0.0991 0.168 Uiso 0.50 1 calc PR A 2 C9' C -0.0072(14) 0.1759(6) 0.1438(10) 0.100(5) Uiso 0.50 1 d PG A 2 H9' H -0.0619 0.2282 0.1295 0.120 Uiso 0.50 1 calc PR A 2 C10' C 0.1034(15) 0.1684(11) 0.1865(11) 0.181(7) Uiso 0.50 1 d PG A 2 H10' H 0.1338 0.2149 0.2052 0.217 Uiso 0.50 1 calc PR A 2 O1 O 0.0172(3) 0.55987(18) 0.13748(19) 0.0657(8) Uani 1 1 d . . . O2 O -0.0664(3) 0.40796(19) 0.04609(19) 0.0675(8) Uani 1 1 d . . . O3 O 0.3295(3) 0.92061(19) -0.06242(19) 0.0804(10) Uani 1 1 d . . . O4 O 0.5975(3) 1.05974(18) -0.1627(2) 0.0745(9) Uani 1 1 d . . . C11 C 0.0137(4) 0.4706(3) 0.2043(3) 0.0526(10) Uani 1 1 d . . . C12 C 0.1163(4) 0.4406(3) 0.2552(3) 0.0633(12) Uani 1 1 d . . . H12 H 0.1876 0.4817 0.2428 0.076 Uiso 1 1 calc R . . C13 C 0.1113(5) 0.3542(3) 0.3204(3) 0.0694(13) Uani 1 1 d . . . H13 H 0.1780 0.3365 0.3547 0.083 Uiso 1 1 calc R . . C14 C 0.0071(4) 0.2885(3) 0.3388(3) 0.0593(11) Uani 1 1 d . . . C15 C 0.0003(5) 0.1936(3) 0.4057(3) 0.0764(14) Uani 1 1 d . . . H15 H 0.0687 0.1724 0.4379 0.092 Uiso 1 1 calc R . . C16 C -0.1021(6) 0.1341(3) 0.4234(3) 0.0807(15) Uani 1 1 d . . . H16 H -0.1056 0.0733 0.4688 0.097 Uiso 1 1 calc R . . C17 C -0.2018(5) 0.1632(3) 0.3743(3) 0.0733(13) Uani 1 1 d . . . H17 H -0.2719 0.1211 0.3863 0.088 Uiso 1 1 calc R . . C18 C -0.2003(4) 0.2517(3) 0.3086(3) 0.0566(11) Uani 1 1 d . . . H18 H -0.2691 0.2694 0.2763 0.068 Uiso 1 1 calc R . . C19 C -0.0956(4) 0.3175(3) 0.2887(3) 0.0484(10) Uani 1 1 d . . . C20 C -0.0912(4) 0.4113(3) 0.2205(3) 0.0475(10) Uani 1 1 d . . . C21 C -0.1964(4) 0.4452(2) 0.1641(3) 0.0534(11) Uani 1 1 d . . . C22 C -0.3144(4) 0.4802(3) 0.1986(3) 0.0581(11) Uani 1 1 d . . . C23 C -0.3450(4) 0.4741(3) 0.2883(4) 0.0693(13) Uani 1 1 d . . . H23 H -0.2843 0.4498 0.3268 0.083 Uiso 1 1 calc R . . C24 C -0.4635(5) 0.5032(3) 0.3221(4) 0.0847(15) Uani 1 1 d . . . H24 H -0.4824 0.4965 0.3831 0.102 Uiso 1 1 calc R . . C25 C -0.5528(6) 0.5418(4) 0.2667(6) 0.099(2) Uani 1 1 d . . . H25 H -0.6324 0.5607 0.2902 0.118 Uiso 1 1 calc R . . C26 C -0.5265(5) 0.5527(3) 0.1777(6) 0.094(2) Uani 1 1 d . . . H26 H -0.5874 0.5816 0.1405 0.113 Uiso 1 1 calc R . . C27 C -0.4064(4) 0.5207(3) 0.1389(4) 0.0687(13) Uani 1 1 d . . . C28 C -0.3773(5) 0.5277(3) 0.0496(4) 0.0747(15) Uani 1 1 d . . . H28 H -0.4349 0.5582 0.0103 0.090 Uiso 1 1 calc R . . C29 C -0.2670(5) 0.4915(3) 0.0172(3) 0.0699(13) Uani 1 1 d . . . H29 H -0.2508 0.4953 -0.0430 0.084 Uiso 1 1 calc R . . C30 C -0.1764(4) 0.4476(3) 0.0760(3) 0.0549(11) Uani 1 1 d . . . C31 C 0.3909(4) 0.8822(3) -0.1233(3) 0.0587(11) Uani 1 1 d . . . C32 C 0.3981(4) 0.7811(3) -0.0996(3) 0.0608(12) Uani 1 1 d . . . H32 H 0.3629 0.7406 -0.0412 0.073 Uiso 1 1 calc R . . C33 C 0.4556(4) 0.7428(3) -0.1607(3) 0.0575(11) Uani 1 1 d . . . H33 H 0.4600 0.6760 -0.1434 0.069 Uiso 1 1 calc R . . C34 C 0.5086(4) 0.8005(3) -0.2491(3) 0.0527(10) Uani 1 1 d . . . C35 C 0.5636(4) 0.7618(3) -0.3143(3) 0.0658(12) Uani 1 1 d . . . H35 H 0.5664 0.6951 -0.2985 0.079 Uiso 1 1 calc R . . C36 C 0.6138(5) 0.8207(4) -0.4017(4) 0.0753(14) Uani 1 1 d . . . H36 H 0.6495 0.7935 -0.4442 0.090 Uiso 1 1 calc R . . C37 C 0.6112(5) 0.9223(3) -0.4268(3) 0.0759(14) Uani 1 1 d . . . H37 H 0.6469 0.9622 -0.4853 0.091 Uiso 1 1 calc R . . C38 C 0.5550(4) 0.9614(3) -0.3634(3) 0.0676(12) Uani 1 1 d . . . H38 H 0.5529 1.0282 -0.3803 0.081 Uiso 1 1 calc R . . C39 C 0.5009(4) 0.9034(3) -0.2740(3) 0.0510(10) Uani 1 1 d . . . C40 C 0.4388(4) 0.9431(2) -0.2087(3) 0.0498(10) Uani 1 1 d . . . C41 C 0.4220(4) 1.0496(3) -0.2340(3) 0.0505(10) Uani 1 1 d . . . C42 C 0.3213(4) 1.0960(3) -0.2832(3) 0.0538(11) Uani 1 1 d . . . C43 C 0.2371(4) 1.0459(3) -0.3106(3) 0.0619(12) Uani 1 1 d . . . H43 H 0.2460 0.9798 -0.2964 0.074 Uiso 1 1 calc R . . C44 C 0.1424(5) 1.0915(4) -0.3577(3) 0.0805(14) Uani 1 1 d . . . H44 H 0.0878 1.0564 -0.3757 0.097 Uiso 1 1 calc R . . C45 C 0.1260(6) 1.1911(4) -0.3795(4) 0.0921(17) Uani 1 1 d . . . H45 H 0.0611 1.2217 -0.4123 0.111 Uiso 1 1 calc R . . C46 C 0.2028(6) 1.2419(4) -0.3535(4) 0.0842(15) Uani 1 1 d . . . H46 H 0.1918 1.3079 -0.3681 0.101 Uiso 1 1 calc R . . C47 C 0.3017(5) 1.1949(3) -0.3034(3) 0.0673(13) Uani 1 1 d . . . C48 C 0.3844(5) 1.2480(3) -0.2749(3) 0.0763(14) Uani 1 1 d . . . H48 H 0.3722 1.3137 -0.2878 0.092 Uiso 1 1 calc R . . C49 C 0.4805(5) 1.2039(3) -0.2294(3) 0.0716(13) Uani 1 1 d . . . H49 H 0.5352 1.2393 -0.2118 0.086 Uiso 1 1 calc R . . C50 C 0.4978(4) 1.1035(3) -0.2084(3) 0.0607(12) Uani 1 1 d . . . C100 C 0.1365(6) 0.7250(4) 0.2394(4) 0.1049(18) Uani 1 1 d D . . H10A H 0.0512 0.6993 0.2452 0.157 Uiso 1 1 calc R . . H10B H 0.1295 0.7831 0.2530 0.157 Uiso 1 1 calc R . . H10C H 0.1839 0.6784 0.2812 0.157 Uiso 1 1 calc R . . N1 N 0.2040(4) 0.7463(3) 0.1476(3) 0.0859(12) Uani 1 1 d D . . O5 O 0.2693(3) 0.8218(2) 0.1104(2) 0.0831(10) Uani 1 1 d D . . O6 O 0.1932(3) 0.6879(2) 0.1105(2) 0.0770(9) Uani 1 1 d D . . C51 C 0.3940(9) 0.7375(6) 0.4734(7) 0.088(3) Uiso 0.25 1 d PD B 1 H51A H 0.4758 0.7058 0.4775 0.133 Uiso 0.25 1 calc PR B 1 H51B H 0.3627 0.7482 0.5290 0.133 Uiso 0.25 1 calc PR B 1 H51C H 0.4052 0.7984 0.4237 0.133 Uiso 0.25 1 calc PR B 1 N2 N 0.3033(11) 0.6790(8) 0.4587(10) 0.070(4) Uiso 0.25 1 d PD B 1 O7 O 0.1889(11) 0.6991(7) 0.4619(8) 0.192(4) Uiso 0.25 1 d PD B 1 O8 O 0.3251(14) 0.5985(9) 0.4661(10) 0.114(5) Uiso 0.25 1 d PD B 1 C51' C 0.3940(9) 0.7375(6) 0.4734(7) 0.088(3) Uiso 0.25 1 d PD C 2 H51D H 0.4607 0.7842 0.4360 0.133 Uiso 0.25 1 calc PR C 2 H51E H 0.4223 0.6740 0.4777 0.133 Uiso 0.25 1 calc PR C 2 H51F H 0.3767 0.7410 0.5330 0.133 Uiso 0.25 1 calc PR C 2 N2' N 0.2790(10) 0.7574(8) 0.4341(8) 0.062(4) Uiso 0.25 1 d PD C 2 O7' O 0.1889(11) 0.6991(7) 0.4619(8) 0.192(4) Uiso 0.25 1 d PD C 2 O8' O 0.2531(13) 0.8364(8) 0.3889(9) 0.103(4) Uiso 0.25 1 d PD C 2 H101 H 0.6373 1.1049 -0.1448 0.050 Uiso 1 1 d . . . H100 H 0.2823 0.8834 -0.0028 0.050 Uiso 1 1 d . . . H102 H 0.0842 0.6048 0.1392 0.050 Uiso 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 0.0682(5) 0.0573(4) 0.0832(5) -0.0269(3) -0.0070(3) 0.0126(3) O1 0.063(2) 0.0518(16) 0.078(2) -0.0116(15) -0.0248(16) -0.0140(14) O2 0.068(2) 0.0627(18) 0.074(2) -0.0237(16) -0.0198(17) 0.0052(16) O3 0.122(3) 0.0529(17) 0.0553(19) -0.0182(15) 0.0130(18) -0.0023(17) O4 0.090(2) 0.0481(16) 0.097(2) -0.0298(16) -0.038(2) -0.0004(16) C11 0.053(3) 0.047(2) 0.055(3) -0.015(2) -0.009(2) 0.001(2) C12 0.048(3) 0.073(3) 0.070(3) -0.023(3) -0.016(2) -0.004(2) C13 0.065(3) 0.067(3) 0.078(3) -0.018(3) -0.038(3) 0.011(3) C14 0.064(3) 0.060(3) 0.055(3) -0.017(2) -0.021(2) 0.010(2) C15 0.097(4) 0.060(3) 0.072(3) -0.014(3) -0.040(3) 0.013(3) C16 0.120(5) 0.051(3) 0.066(3) -0.010(2) -0.028(3) 0.007(3) C17 0.082(4) 0.057(3) 0.076(3) -0.018(3) -0.009(3) -0.010(2) C18 0.056(3) 0.048(2) 0.065(3) -0.017(2) -0.013(2) -0.001(2) C19 0.049(3) 0.047(2) 0.052(2) -0.020(2) -0.013(2) 0.006(2) C20 0.041(2) 0.044(2) 0.058(3) -0.0166(19) -0.011(2) -0.0020(19) C21 0.047(3) 0.033(2) 0.074(3) -0.009(2) -0.018(2) -0.0026(18) C22 0.049(3) 0.040(2) 0.087(4) -0.022(2) -0.015(3) 0.0015(19) C23 0.055(3) 0.052(3) 0.105(4) -0.034(3) -0.009(3) 0.005(2) C24 0.067(4) 0.071(3) 0.128(5) -0.052(3) -0.013(4) 0.006(3) C25 0.058(4) 0.075(4) 0.178(7) -0.068(4) -0.012(5) 0.011(3) C26 0.057(4) 0.049(3) 0.190(7) -0.049(4) -0.048(4) 0.007(2) C27 0.051(3) 0.040(2) 0.122(5) -0.029(3) -0.033(3) 0.005(2) C28 0.067(4) 0.046(3) 0.116(5) -0.020(3) -0.049(3) 0.003(2) C29 0.083(4) 0.050(2) 0.077(3) -0.011(2) -0.040(3) -0.005(2) C30 0.061(3) 0.039(2) 0.066(3) -0.012(2) -0.028(3) -0.007(2) C31 0.071(3) 0.048(2) 0.059(3) -0.020(2) -0.010(2) -0.007(2) C32 0.076(3) 0.042(2) 0.057(3) -0.008(2) -0.010(2) -0.008(2) C33 0.062(3) 0.042(2) 0.069(3) -0.017(2) -0.017(2) -0.003(2) C34 0.049(3) 0.040(2) 0.070(3) -0.019(2) -0.011(2) 0.0003(19) C35 0.060(3) 0.055(3) 0.090(4) -0.037(3) -0.007(3) 0.006(2) C36 0.070(3) 0.081(3) 0.087(4) -0.050(3) -0.006(3) 0.016(3) C37 0.074(4) 0.071(3) 0.073(3) -0.021(3) 0.003(3) 0.007(3) C38 0.075(3) 0.050(2) 0.070(3) -0.018(2) 0.003(3) 0.003(2) C39 0.046(3) 0.050(2) 0.061(3) -0.022(2) -0.013(2) -0.0018(19) C40 0.057(3) 0.037(2) 0.057(3) -0.019(2) -0.010(2) -0.0019(19) C41 0.058(3) 0.041(2) 0.053(2) -0.0205(19) 0.000(2) -0.009(2) C42 0.060(3) 0.045(2) 0.053(3) -0.018(2) 0.001(2) 0.003(2) C43 0.067(3) 0.063(3) 0.055(3) -0.020(2) -0.010(2) 0.006(2) C44 0.081(4) 0.093(4) 0.077(3) -0.042(3) -0.016(3) 0.012(3) C45 0.088(4) 0.109(5) 0.084(4) -0.038(3) -0.026(3) 0.039(4) C46 0.090(4) 0.074(3) 0.088(4) -0.029(3) -0.019(3) 0.024(3) C47 0.070(3) 0.057(3) 0.068(3) -0.019(2) -0.005(3) 0.015(2) C48 0.084(4) 0.044(2) 0.095(4) -0.025(3) -0.002(3) 0.003(3) C49 0.082(4) 0.047(3) 0.092(4) -0.030(2) -0.020(3) 0.000(2) C50 0.067(3) 0.043(2) 0.068(3) -0.015(2) -0.013(2) 0.005(2) C100 0.125(5) 0.109(4) 0.076(4) -0.042(3) 0.015(4) -0.011(4) N1 0.093(3) 0.086(3) 0.083(3) -0.033(3) -0.020(3) -0.003(3) O5 0.118(3) 0.0598(19) 0.068(2) -0.0171(16) -0.011(2) -0.0416(19) O6 0.084(2) 0.0669(19) 0.085(2) -0.0349(18) -0.0024(18) -0.0266(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C7 1.933(18) . ? Co1 C3' 1.949(12) . ? Co1 C2' 1.972(11) . ? Co1 C8' 1.973(12) . ? Co1 C7' 1.985(10) . ? Co1 C6 1.984(15) . ? Co1 C8 1.992(19) . ? Co1 C4' 1.994(10) . ? Co1 C2 2.021(11) . ? Co1 C1' 2.029(11) . ? Co1 C5' 2.042(10) . ? Co1 C3 2.041(12) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 H1 0.9300 . ? C2 C3 1.4200 . ? C2 H2 0.9300 . ? C3 C4 1.4200 . ? C3 H3 0.9300 . ? C4 C5 1.4200 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.4200 . ? C6 C10 1.4200 . ? C6 H6 0.9300 . ? C7 C8 1.4200 . ? C7 H7 0.9300 . ? C8 C9 1.4200 . ? C8 H8 0.9300 . ? C9 C10 1.4200 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C1' C2' 1.4200 . ? C1' C5' 1.4200 . ? C1' H1' 0.9300 . ? C2' C3' 1.4200 . ? C2' H2' 0.9300 . ? C3' C4' 1.4200 . ? C3' H3' 0.9300 . ? C4' C5' 1.4200 . ? C4' H4' 0.9300 . ? C5' H5' 0.9300 . ? C6' C7' 1.4200 . ? C6' C10' 1.4200 . ? C6' H6' 0.9300 . ? C7' C8' 1.4200 . ? C7' H7' 0.9300 . ? C8' C9' 1.4200 . ? C8' H8' 0.9300 . ? C9' C10' 1.4200 . ? C9' H9' 0.9300 . ? C10' H10' 0.9300 . ? O1 C11 1.367(4) . ? O1 H102 0.9953 . ? O2 C30 1.364(5) . ? O3 C31 1.358(5) . ? O3 H100 0.9695 . ? O4 C50 1.379(5) . ? O4 H101 0.9514 . ? C11 C20 1.363(5) . ? C11 C12 1.417(5) . ? C12 C13 1.326(6) . ? C12 H12 0.9300 . ? C13 C14 1.412(6) . ? C13 H13 0.9300 . ? C14 C19 1.407(5) . ? C14 C15 1.425(6) . ? C15 C16 1.339(6) . ? C15 H15 0.9300 . ? C16 C17 1.373(6) . ? C16 H16 0.9300 . ? C17 C18 1.354(5) . ? C17 H17 0.9300 . ? C18 C19 1.412(5) . ? C18 H18 0.9300 . ? C19 C20 1.423(5) . ? C20 C21 1.496(5) . ? C21 C30 1.376(6) . ? C21 C22 1.423(6) . ? C22 C23 1.386(6) . ? C22 C27 1.431(6) . ? C23 C24 1.384(6) . ? C23 H23 0.9300 . ? C24 C25 1.361(7) . ? C24 H24 0.9300 . ? C25 C26 1.354(8) . ? C25 H25 0.9300 . ? C26 C27 1.446(8) . ? C26 H26 0.9300 . ? C27 C28 1.374(7) . ? C28 C29 1.355(7) . ? C28 H28 0.9300 . ? C29 C30 1.419(5) . ? C29 H29 0.9300 . ? C31 C40 1.359(5) . ? C31 C32 1.412(5) . ? C32 C33 1.348(5) . ? C32 H32 0.9300 . ? C33 C34 1.392(5) . ? C33 H33 0.9300 . ? C34 C35 1.396(6) . ? C34 C39 1.437(5) . ? C35 C36 1.378(6) . ? C35 H35 0.9300 . ? C36 C37 1.416(6) . ? C36 H36 0.9300 . ? C37 C38 1.380(6) . ? C37 H37 0.9300 . ? C38 C39 1.408(6) . ? C38 H38 0.9300 . ? C39 C40 1.431(5) . ? C40 C41 1.495(5) . ? C41 C50 1.352(5) . ? C41 C42 1.426(5) . ? C42 C43 1.391(6) . ? C42 C47 1.400(5) . ? C43 C44 1.355(6) . ? C43 H43 0.9300 . ? C44 C45 1.403(7) . ? C44 H44 0.9300 . ? C45 C46 1.330(7) . ? C45 H45 0.9300 . ? C46 C47 1.419(6) . ? C46 H46 0.9300 . ? C47 C48 1.421(6) . ? C48 C49 1.348(6) . ? C48 H48 0.9300 . ? C49 C50 1.416(5) . ? C49 H49 0.9300 . ? C100 N1 1.444(6) . ? C100 H10A 0.9600 . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? N1 O6 1.231(4) . ? N1 O5 1.232(4) . ? C51 N2 1.411(9) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? N2 O8 1.176(8) . ? N2 O7 1.218(9) . ? N2' O8' 1.185(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Co1 C3' 148.8(8) . . ? C7 Co1 C2' 126.0(6) . . ? C3' Co1 C2' 42.5(2) . . ? C7 Co1 C8' 14.3(7) . . ? C3' Co1 C8' 134.9(4) . . ? C2' Co1 C8' 114.4(4) . . ? C7 Co1 C7' 28.3(8) . . ? C3' Co1 C7' 176.6(4) . . ? C2' Co1 C7' 135.4(4) . . ? C8' Co1 C7' 42.0(2) . . ? C7 Co1 C6 42.5(3) . . ? C3' Co1 C6 158.1(7) . . ? C2' Co1 C6 158.9(6) . . ? C8' Co1 C6 56.4(6) . . ? C7' Co1 C6 24.5(5) . . ? C7 Co1 C8 42.4(4) . . ? C3' Co1 C8 109.2(6) . . ? C2' Co1 C8 113.3(5) . . ? C8' Co1 C8 34.0(5) . . ? C7' Co1 C8 68.7(6) . . ? C6 Co1 C8 70.6(4) . . ? C7 Co1 C4' 163.2(6) . . ? C3' Co1 C4' 42.2(2) . . ? C2' Co1 C4' 70.8(3) . . ? C8' Co1 C4' 168.8(4) . . ? C7' Co1 C4' 141.2(4) . . ? C6 Co1 C4' 122.1(7) . . ? C8 Co1 C4' 135.3(6) . . ? C7 Co1 C2 109.3(5) . . ? C3' Co1 C2 77.3(4) . . ? C2' Co1 C2 39.9(4) . . ? C8' Co1 C2 106.3(4) . . ? C7' Co1 C2 101.9(4) . . ? C6 Co1 C2 120.7(5) . . ? C8 Co1 C2 129.1(5) . . ? C4' Co1 C2 84.1(3) . . ? C7 Co1 C1' 122.3(5) . . ? C3' Co1 C1' 70.5(3) . . ? C2' Co1 C1' 41.5(2) . . ? C8' Co1 C1' 121.1(4) . . ? C7' Co1 C1' 109.5(4) . . ? C6 Co1 C1' 123.2(4) . . ? C8 Co1 C1' 144.0(5) . . ? C4' Co1 C1' 69.7(2) . . ? C2 Co1 C1' 15.4(4) . . ? C7 Co1 C5' 139.3(7) . . ? C3' Co1 C5' 70.2(2) . . ? C2' Co1 C5' 69.8(3) . . ? C8' Co1 C5' 149.1(4) . . ? C7' Co1 C5' 112.1(4) . . ? C6 Co1 C5' 107.9(5) . . ? C8 Co1 C5' 175.0(5) . . ? C4' Co1 C5' 41.18(18) . . ? C2 Co1 C5' 55.8(3) . . ? C1' Co1 C5' 40.83(19) . . ? C7 Co1 C3 115.8(6) . . ? C3' Co1 C3 49.4(5) . . ? C2' Co1 C3 10.4(5) . . ? C8' Co1 C3 104.0(4) . . ? C7' Co1 C3 128.0(4) . . ? C6 Co1 C3 152.5(7) . . ? C8 Co1 C3 104.7(5) . . ? C4' Co1 C3 80.9(4) . . ? C2 Co1 C3 40.9(2) . . ? C1' Co1 C3 46.4(4) . . ? C5' Co1 C3 78.9(4) . . ? C2 C1 C5 108.0 . . ? C2 C1 Co1 67.9(4) . . ? C5 C1 Co1 72.0(4) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Co1 C1 H1 125.6 . . ? C1 C2 C3 108.0 . . ? C1 C2 Co1 71.5(4) . . ? C3 C2 Co1 70.3(4) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Co1 C2 H2 123.9 . . ? C4 C3 C2 108.0 . . ? C4 C3 Co1 72.2(4) . . ? C2 C3 Co1 68.8(4) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Co1 C3 H3 124.6 . . ? C3 C4 C5 108.0 . . ? C3 C4 Co1 67.8(4) . . ? C5 C4 Co1 70.9(4) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Co1 C4 H4 126.9 . . ? C4 C5 C1 108.0 . . ? C4 C5 Co1 69.7(4) . . ? C1 C5 Co1 68.4(4) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Co1 C5 H5 127.5 . . ? C7 C6 C10 108.0 . . ? C7 C6 Co1 66.8(7) . . ? C10 C6 Co1 72.9(5) . . ? C7 C6 H6 126.0 . . ? C10 C6 H6 126.0 . . ? Co1 C6 H6 125.9 . . ? C8 C7 C6 108.0 . . ? C8 C7 Co1 71.0(5) . . ? C6 C7 Co1 70.7(7) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Co1 C7 H7 123.9 . . ? C7 C8 C9 108.0 . . ? C7 C8 Co1 66.6(5) . . ? C9 C8 Co1 72.8(6) . . ? C7 C8 H8 126.0 . . ? C9 C8 H8 126.0 . . ? Co1 C8 H8 126.1 . . ? C10 C9 C8 108.0 . . ? C10 C9 Co1 69.8(6) . . ? C8 C9 Co1 66.4(7) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Co1 C9 H9 129.4 . . ? C9 C10 C6 108.0 . . ? C9 C10 Co1 70.2(6) . . ? C6 C10 Co1 66.2(5) . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Co1 C10 H10 129.2 . . ? C2' C1' C5' 108.0 . . ? C2' C1' Co1 67.1(4) . . ? C5' C1' Co1 70.1(4) . . ? C2' C1' H1' 126.0 . . ? C5' C1' H1' 126.0 . . ? Co1 C1' H1' 128.4 . . ? C3' C2' C1' 108.0 . . ? C3' C2' Co1 67.9(4) . . ? C1' C2' Co1 71.4(4) . . ? C3' C2' H2' 126.0 . . ? C1' C2' H2' 126.0 . . ? Co1 C2' H2' 126.2 . . ? C4' C3' C2' 108.0 . . ? C4' C3' Co1 70.6(4) . . ? C2' C3' Co1 69.6(4) . . ? C4' C3' H3' 126.0 . . ? C2' C3' H3' 126.0 . . ? Co1 C3' H3' 125.4 . . ? C5' C4' C3' 108.0 . . ? C5' C4' Co1 71.2(4) . . ? C3' C4' Co1 67.2(4) . . ? C5' C4' H4' 126.0 . . ? C3' C4' H4' 126.0 . . ? Co1 C4' H4' 127.1 . . ? C4' C5' C1' 108.0 . . ? C4' C5' Co1 67.6(4) . . ? C1' C5' Co1 69.1(4) . . ? C4' C5' H5' 126.0 . . ? C1' C5' H5' 126.0 . . ? Co1 C5' H5' 128.9 . . ? C7' C6' C10' 108.0 . . ? C7' C6' Co1 66.6(4) . . ? C10' C6' Co1 71.3(4) . . ? C7' C6' H6' 126.0 . . ? C10' C6' H6' 126.0 . . ? Co1 C6' H6' 127.5 . . ? C8' C7' C6' 108.0 . . ? C8' C7' Co1 68.5(5) . . ? C6' C7' Co1 72.3(5) . . ? C8' C7' H7' 126.0 . . ? C6' C7' H7' 126.0 . . ? Co1 C7' H7' 124.7 . . ? C7' C8' C9' 108.0 . . ? C7' C8' Co1 69.4(5) . . ? C9' C8' Co1 71.9(4) . . ? C7' C8' H8' 126.0 . . ? C9' C8' H8' 126.0 . . ? Co1 C8' H8' 124.3 . . ? C10' C9' C8' 108.0 . . ? C10' C9' Co1 71.9(5) . . ? C8' C9' Co1 66.7(4) . . ? C10' C9' H9' 126.0 . . ? C8' C9' H9' 126.0 . . ? Co1 C9' H9' 126.9 . . ? C9' C10' C6' 108.0 . . ? C9' C10' Co1 68.0(5) . . ? C6' C10' Co1 68.7(4) . . ? C9' C10' H10' 126.0 . . ? C6' C10' H10' 126.0 . . ? Co1 C10' H10' 128.9 . . ? C11 O1 H102 113.7 . . ? C31 O3 H100 124.7 . . ? C50 O4 H101 109.3 . . ? C20 C11 O1 118.2(3) . . ? C20 C11 C12 120.9(4) . . ? O1 C11 C12 120.9(4) . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 121.4(4) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C19 C14 C13 118.7(4) . . ? C19 C14 C15 118.0(4) . . ? C13 C14 C15 123.3(4) . . ? C16 C15 C14 121.7(4) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 121.4(5) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 120.8(4) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 118.2(4) . . ? C14 C19 C20 119.6(4) . . ? C18 C19 C20 122.2(3) . . ? C11 C20 C19 119.0(3) . . ? C11 C20 C21 119.2(3) . . ? C19 C20 C21 121.8(3) . . ? C30 C21 C22 119.3(4) . . ? C30 C21 C20 119.8(4) . . ? C22 C21 C20 120.8(4) . . ? C23 C22 C21 122.5(4) . . ? C23 C22 C27 119.0(4) . . ? C21 C22 C27 118.5(5) . . ? C24 C23 C22 121.7(5) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C23 120.5(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 120.4(6) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 121.8(5) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C22 119.7(5) . . ? C28 C27 C26 123.8(5) . . ? C22 C27 C26 116.6(6) . . ? C29 C28 C27 121.9(4) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 119.4(5) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? O2 C30 C21 118.3(3) . . ? O2 C30 C29 120.8(4) . . ? C21 C30 C29 120.9(4) . . ? C40 C31 O3 118.4(3) . . ? C40 C31 C32 121.0(4) . . ? O3 C31 C32 120.5(4) . . ? C33 C32 C31 120.6(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 121.7(4) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C35 122.4(4) . . ? C33 C34 C39 118.0(4) . . ? C35 C34 C39 119.5(4) . . ? C36 C35 C34 121.2(4) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C37 120.2(4) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 119.2(4) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 122.1(4) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C38 C39 C40 122.6(4) . . ? C38 C39 C34 117.7(4) . . ? C40 C39 C34 119.7(4) . . ? C31 C40 C39 118.9(3) . . ? C31 C40 C41 120.0(4) . . ? C39 C40 C41 121.0(3) . . ? C50 C41 C42 118.4(4) . . ? C50 C41 C40 121.4(4) . . ? C42 C41 C40 120.2(4) . . ? C43 C42 C47 117.4(4) . . ? C43 C42 C41 122.3(4) . . ? C47 C42 C41 120.3(4) . . ? C44 C43 C42 121.4(4) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C45 120.5(5) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 120.3(5) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 119.8(5) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C42 C47 C46 120.6(5) . . ? C42 C47 C48 118.9(4) . . ? C46 C47 C48 120.5(4) . . ? C49 C48 C47 120.5(4) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 119.8(4) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C41 C50 O4 118.8(3) . . ? C41 C50 C49 122.1(4) . . ? O4 C50 C49 119.1(4) . . ? N1 C100 H10A 109.5 . . ? N1 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? N1 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O6 N1 O5 123.3(4) . . ? O6 N1 C100 118.2(4) . . ? O5 N1 C100 118.4(4) . . ? O8 N2 O7 114.6(10) . . ? O8 N2 C51 121.6(11) . . ? O7 N2 C51 121.1(9) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 34.04 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 0.780 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.083 data_4 _database_code_CSD 154552 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H27 Cs O4' _chemical_formula_weight 704.53 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 '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 10.6220(10) _cell_length_b 12.3900(10) _cell_length_c 12.5900(10) _cell_angle_alpha 89.400(10) _cell_angle_beta 112.130(10) _cell_angle_gamma 100.140(10) _cell_volume 1508.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4689 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4428 _reflns_number_gt 3288 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1152P)^2^+3.7524P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4428 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _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 Cs1 Cs 0.00404(5) 0.24308(3) 0.16647(4) 0.0594(2) Uani 1 1 d . . . O1 O -0.0906(4) 0.5918(3) 0.1346(3) 0.0370(9) Uani 1 1 d . . . C1 C 0.2022(3) 0.59346(18) 0.2306(3) 0.0306(12) Uani 1 1 d G . . C2 C 0.1960(3) 0.55282(19) 0.1259(3) 0.0343(13) Uani 1 1 d G . . C3 C 0.2816(3) 0.6082(2) 0.0745(2) 0.0412(14) Uani 1 1 d G . . H3 H 0.2775 0.5810 0.0044 0.049 Uiso 1 1 calc R . . C4 C 0.3735(3) 0.7042(2) 0.1278(2) 0.0419(15) Uani 1 1 d G . . H4 H 0.4308 0.7412 0.0933 0.050 Uiso 1 1 calc R . . C5 C 0.3797(2) 0.74485(16) 0.2325(2) 0.0358(14) Uani 1 1 d G . . C6 C 0.2941(2) 0.68948(15) 0.2839(2) 0.0324(13) Uani 1 1 d G . . C7 C 0.3004(3) 0.7301(2) 0.3886(2) 0.0353(13) Uani 1 1 d G . . H7 H 0.2431 0.6931 0.4230 0.042 Uiso 1 1 calc R . . C8 C 0.3922(3) 0.8261(2) 0.4419(2) 0.0464(16) Uani 1 1 d G . . H8 H 0.3964 0.8533 0.5119 0.056 Uiso 1 1 calc R . . C9 C 0.4779(3) 0.8815(2) 0.3904(3) 0.0511(18) Uani 1 1 d G . . H9 H 0.5393 0.9458 0.4261 0.061 Uiso 1 1 calc R . . C10 C 0.4716(3) 0.84086(19) 0.2857(3) 0.0447(16) Uani 1 1 d G . . H10 H 0.5289 0.8779 0.2513 0.054 Uiso 1 1 calc R . . O2 O 0.1170(4) 0.4527(3) 0.0792(4) 0.0422(10) Uani 1 1 d . . . H200 H 0.1076 0.4250 0.0037 0.050 Uiso 1 1 d . . . C11 C 0.1030(2) 0.5264(2) 0.2807(2) 0.0309(12) Uani 1 1 d G . . C12 C -0.0359(3) 0.5340(2) 0.2291(2) 0.0313(12) Uani 1 1 d G . . C13 C -0.1316(2) 0.4750(3) 0.2688(3) 0.0416(14) Uani 1 1 d G . . H13 H -0.2245 0.4801 0.2342 0.050 Uiso 1 1 calc R . . C14 C -0.0885(2) 0.4082(3) 0.3601(3) 0.0478(16) Uani 1 1 d G . . H14 H -0.1525 0.3687 0.3866 0.057 Uiso 1 1 calc R . . C15 C 0.0503(2) 0.40055(18) 0.4117(2) 0.0415(14) Uani 1 1 d G . . C16 C 0.14606(19) 0.45961(16) 0.3721(2) 0.0338(13) Uani 1 1 d G . . C17 C 0.2849(2) 0.4519(3) 0.4237(3) 0.0470(16) Uani 1 1 d G . . H17 H 0.3489 0.4915 0.3971 0.056 Uiso 1 1 calc R . . C18 C 0.3280(3) 0.3852(3) 0.5150(3) 0.0598(19) Uani 1 1 d G . . H18 H 0.4209 0.3800 0.5496 0.072 Uiso 1 1 calc R . . C19 C 0.2323(3) 0.3261(3) 0.5547(3) 0.068(2) Uani 1 1 d G . . H19 H 0.2611 0.2815 0.6158 0.081 Uiso 1 1 calc R . . C20 C 0.0934(3) 0.3338(3) 0.5030(3) 0.0560(18) Uani 1 1 d G . . H20 H 0.0294 0.2943 0.5296 0.067 Uiso 1 1 calc R . . O3 O 0.1181(4) -0.0801(3) 0.0295(4) 0.0437(10) Uani 1 1 d . . . H300 H -0.0548 0.1387 -0.0558 0.050 Uiso 1 1 d . . . C21 C 0.2318(3) 0.10474(19) 0.0317(2) 0.0331(13) Uani 1 1 d G . . C22 C 0.1895(3) 0.01728(17) 0.0880(3) 0.0351(13) Uani 1 1 d G . . C23 C 0.2290(3) 0.0260(2) 0.2066(3) 0.0433(15) Uani 1 1 d G . . H23 H 0.2007 -0.0325 0.2443 0.052 Uiso 1 1 calc R . . C24 C 0.3108(3) 0.1222(2) 0.2689(2) 0.0457(15) Uani 1 1 d G . . H24 H 0.3373 0.1281 0.3482 0.055 Uiso 1 1 calc R . . C25 C 0.3532(2) 0.20969(18) 0.2125(2) 0.0381(14) Uani 1 1 d G . . C26 C 0.3136(2) 0.20095(16) 0.0940(2) 0.0330(13) Uani 1 1 d G . . C27 C 0.3560(3) 0.2884(2) 0.0376(3) 0.0414(15) Uani 1 1 d G . . H27 H 0.3295 0.2826 -0.0417 0.050 Uiso 1 1 calc R . . C28 C 0.4378(3) 0.38462(19) 0.0999(4) 0.0498(17) Uani 1 1 d G . . H28 H 0.4661 0.4431 0.0622 0.060 Uiso 1 1 calc R . . C29 C 0.4773(3) 0.39336(19) 0.2185(3) 0.058(2) Uani 1 1 d G . . H29 H 0.5321 0.4577 0.2601 0.069 Uiso 1 1 calc R . . C30 C 0.4350(3) 0.3059(2) 0.2748(3) 0.0530(17) Uani 1 1 d G . . H30 H 0.4614 0.3117 0.3541 0.064 Uiso 1 1 calc R . . O4 O 0.0232(4) 0.2140(3) -0.1169(4) 0.0394(10) Uani 1 1 d . . . H400 H -0.0348 0.6993 0.1401 0.050 Uiso 1 1 d . . . C31 C 0.1806(3) 0.0891(2) -0.1007(2) 0.0328(13) Uani 1 1 d G . . C32 C 0.0865(3) 0.1529(2) -0.1647(3) 0.0343(13) Uani 1 1 d G . . C33 C 0.0375(3) 0.1443(2) -0.2840(3) 0.0417(15) Uani 1 1 d G . . H33 H -0.0255 0.1870 -0.3269 0.050 Uiso 1 1 calc R . . C34 C 0.0826(3) 0.0720(2) -0.3392(2) 0.0460(15) Uani 1 1 d G . . H34 H 0.0498 0.0662 -0.4190 0.055 Uiso 1 1 calc R . . C35 C 0.1767(2) 0.00814(18) -0.2752(2) 0.0384(14) Uani 1 1 d G . . C36 C 0.2257(2) 0.01670(16) -0.1559(2) 0.0318(13) Uani 1 1 d G . . C37 C 0.3198(3) -0.0471(2) -0.0919(2) 0.0403(14) Uani 1 1 d G . . H37 H 0.3525 -0.0414 -0.0121 0.048 Uiso 1 1 calc R . . C38 C 0.3648(3) -0.1195(2) -0.1471(3) 0.0498(17) Uani 1 1 d G . . H38 H 0.4278 -0.1622 -0.1042 0.060 Uiso 1 1 calc R . . C39 C 0.3158(3) -0.1281(2) -0.2664(3) 0.0531(18) Uani 1 1 d G . . H39 H 0.3460 -0.1765 -0.3033 0.064 Uiso 1 1 calc R . . C40 C 0.2218(3) -0.0642(2) -0.3304(3) 0.0495(16) Uani 1 1 d G . . H40 H 0.1890 -0.0700 -0.4102 0.059 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 Cs1 0.0661(3) 0.0395(2) 0.0722(4) -0.0128(2) 0.0305(2) -0.00186(17) O1 0.044(2) 0.0284(17) 0.035(3) 0.0000(16) 0.0122(18) 0.0058(15) C1 0.038(3) 0.029(2) 0.028(4) 0.004(2) 0.015(2) 0.009(2) C2 0.036(3) 0.031(3) 0.035(4) 0.001(2) 0.013(2) 0.005(2) C3 0.056(3) 0.046(3) 0.030(4) 0.000(3) 0.025(3) 0.008(3) C4 0.046(3) 0.046(3) 0.042(4) 0.013(3) 0.028(3) 0.004(2) C5 0.044(3) 0.028(2) 0.038(4) 0.008(2) 0.020(3) 0.005(2) C6 0.039(3) 0.028(2) 0.033(4) 0.007(2) 0.014(2) 0.011(2) C7 0.040(3) 0.034(3) 0.033(4) 0.002(2) 0.016(3) 0.005(2) C8 0.056(4) 0.038(3) 0.041(4) -0.004(3) 0.015(3) 0.005(3) C9 0.050(3) 0.033(3) 0.061(5) -0.001(3) 0.017(3) -0.007(2) C10 0.041(3) 0.036(3) 0.056(5) 0.009(3) 0.022(3) -0.001(2) O2 0.054(2) 0.036(2) 0.036(3) -0.0087(18) 0.020(2) -0.0010(17) C11 0.038(3) 0.025(2) 0.030(3) -0.002(2) 0.015(2) 0.002(2) C12 0.039(3) 0.021(2) 0.035(4) -0.003(2) 0.016(2) 0.0035(19) C13 0.037(3) 0.041(3) 0.048(4) 0.000(3) 0.019(3) 0.005(2) C14 0.051(3) 0.043(3) 0.055(5) 0.007(3) 0.032(3) -0.003(3) C15 0.053(3) 0.034(3) 0.040(4) 0.007(3) 0.023(3) 0.002(2) C16 0.045(3) 0.026(2) 0.032(4) 0.001(2) 0.017(3) 0.006(2) C17 0.055(4) 0.039(3) 0.049(5) 0.004(3) 0.022(3) 0.009(3) C18 0.061(4) 0.058(4) 0.063(6) 0.017(4) 0.021(4) 0.022(3) C19 0.089(6) 0.061(4) 0.054(5) 0.031(4) 0.022(4) 0.029(4) C20 0.074(5) 0.047(4) 0.056(5) 0.019(3) 0.036(4) 0.008(3) O3 0.054(2) 0.0331(19) 0.046(3) 0.0015(18) 0.025(2) -0.0007(17) C21 0.033(3) 0.034(3) 0.041(4) 0.009(2) 0.021(2) 0.011(2) C22 0.038(3) 0.040(3) 0.031(4) 0.005(2) 0.017(3) 0.008(2) C23 0.046(3) 0.045(3) 0.041(4) 0.015(3) 0.020(3) 0.008(2) C24 0.048(3) 0.061(4) 0.026(4) 0.006(3) 0.012(3) 0.010(3) C25 0.038(3) 0.047(3) 0.029(4) 0.001(3) 0.010(3) 0.012(2) C26 0.029(2) 0.034(3) 0.043(4) 0.006(2) 0.018(2) 0.014(2) C27 0.039(3) 0.040(3) 0.047(4) 0.006(3) 0.017(3) 0.012(2) C28 0.053(4) 0.038(3) 0.060(5) 0.006(3) 0.026(3) 0.002(3) C29 0.052(4) 0.042(3) 0.075(6) -0.014(3) 0.021(4) 0.001(3) C30 0.047(3) 0.062(4) 0.047(5) -0.009(3) 0.014(3) 0.012(3) O4 0.050(2) 0.0323(19) 0.050(3) 0.0124(18) 0.031(2) 0.0167(16) C31 0.036(3) 0.031(3) 0.034(4) 0.008(2) 0.018(2) 0.003(2) C32 0.038(3) 0.029(2) 0.038(4) 0.008(2) 0.016(3) 0.008(2) C33 0.052(3) 0.044(3) 0.031(4) 0.015(3) 0.015(3) 0.018(3) C34 0.056(4) 0.052(3) 0.028(4) 0.006(3) 0.012(3) 0.012(3) C35 0.042(3) 0.038(3) 0.036(4) 0.001(3) 0.018(3) 0.000(2) C36 0.032(3) 0.031(3) 0.034(4) 0.004(2) 0.016(2) 0.003(2) C37 0.039(3) 0.048(3) 0.037(4) 0.006(3) 0.017(3) 0.013(2) C38 0.046(3) 0.053(4) 0.058(5) 0.011(3) 0.024(3) 0.020(3) C39 0.058(4) 0.048(3) 0.074(6) -0.005(3) 0.047(4) 0.010(3) C40 0.051(3) 0.054(4) 0.047(5) -0.011(3) 0.026(3) 0.001(3) _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 Cs1 O3 2.936(4) 2 ? Cs1 O2 3.038(4) . ? Cs1 C16 3.457(2) . ? Cs1 C15 3.497(3) . ? Cs1 C24 3.611(3) . ? Cs1 C11 3.628(3) . ? Cs1 C25 3.630(2) . ? Cs1 C37 3.644(9) 2 ? Cs1 C36 3.651(9) 2 ? Cs1 O4 3.674(4) . ? Cs1 C14 3.703(4) . ? Cs1 C23 3.811(3) . ? Cs1 H200 3.3494 . ? Cs1 H300 2.8927 . ? O1 C12 1.369(4) . ? O1 H400 1.3503 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C11 1.544(3) . ? C2 O2 1.366(4) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O2 H200 0.9766 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? O3 C22 1.360(4) . ? O3 Cs1 2.936(4) 2 ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C21 C31 1.549(4) . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? O4 C32 1.371(4) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C35 Cs1 3.877(2) 2 ? C36 C37 1.3900 . ? C36 Cs1 3.651(2) 2 ? C37 C38 1.3900 . ? C37 Cs1 3.644(3) 2 ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 Cs1 3.864(3) 2 ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cs1 O2 106.51(11) 2 . ? O3 Cs1 C16 172.78(9) 2 . ? O2 Cs1 C16 66.60(9) . . ? O3 Cs1 C15 161.33(9) 2 . ? O2 Cs1 C15 87.33(8) . . ? C16 Cs1 C15 23.1 . . ? O3 Cs1 C24 89.45(9) 2 . ? O2 Cs1 C24 99.18(9) . . ? C16 Cs1 C24 93.77(6) . . ? C15 Cs1 C24 100.86(6) . . ? O3 Cs1 C11 150.46(9) 2 . ? O2 Cs1 C11 48.13(9) . . ? C16 Cs1 C11 22.5 . . ? C15 Cs1 C11 39.4 . . ? C24 Cs1 C11 107.62(6) . . ? O3 Cs1 C25 92.45(9) 2 . ? O2 Cs1 C25 77.30(9) . . ? C16 Cs1 C25 88.2 . . ? C15 Cs1 C25 102.99(5) . . ? C24 Cs1 C25 22.1 . . ? C11 Cs1 C25 95.06(5) . . ? O3 Cs1 C37 53.71(13) 2 2 ? O2 Cs1 C37 138.66(17) . 2 ? C16 Cs1 C37 129.83(10) . 2 ? C15 Cs1 C37 107.63(11) . 2 ? C24 Cs1 C37 114.67(14) . 2 ? C11 Cs1 C37 131.43(11) . 2 ? C25 Cs1 C37 132.33(12) . 2 ? O3 Cs1 C36 55.03(14) 2 2 ? O2 Cs1 C36 157.70(18) . 2 ? C16 Cs1 C36 131.05(12) . 2 ? C15 Cs1 C36 108.34(11) . 2 ? C24 Cs1 C36 93.45(14) . 2 ? C11 Cs1 C36 143.35(9) . 2 ? C25 Cs1 C36 112.96(12) . 2 ? C37 Cs1 C36 21.97(6) 2 2 ? O3 Cs1 O4 43.78(10) 2 . ? O2 Cs1 O4 64.44(10) . . ? C16 Cs1 O4 130.07(7) . . ? C15 Cs1 O4 151.77(7) . . ? C24 Cs1 O4 84.82(7) . . ? C11 Cs1 O4 112.40(7) . . ? C25 Cs1 O4 72.37(7) . . ? C37 Cs1 O4 94.55(14) 2 . ? C36 Cs1 O4 98.79(13) 2 . ? O3 Cs1 C14 142.11(9) 2 . ? O2 Cs1 C14 89.97(9) . . ? C16 Cs1 C14 39.1 . . ? C15 Cs1 C14 22.0 . . ? C24 Cs1 C14 121.99(6) . . ? C11 Cs1 C14 44.6 . . ? C25 Cs1 C14 124.82(5) . . ? C37 Cs1 C14 91.40(10) 2 . ? C36 Cs1 C14 98.86(9) 2 . ? O4 Cs1 C14 146.65(7) . . ? O3 Cs1 C23 69.90(10) 2 . ? O2 Cs1 C23 112.29(9) . . ? C16 Cs1 C23 114.16(6) . . ? C15 Cs1 C23 117.00(7) . . ? C24 Cs1 C23 21.4 . . ? C11 Cs1 C23 128.99(6) . . ? C25 Cs1 C23 37.7 . . ? C37 Cs1 C23 95.19(13) 2 . ? C36 Cs1 C23 75.31(12) 2 . ? O4 Cs1 C23 76.90(8) . . ? C14 Cs1 C23 135.19(7) . . ? O3 Cs1 H200 90.1 2 . ? O2 Cs1 H200 16.7 . . ? C16 Cs1 H200 83.2 . . ? C15 Cs1 H200 104.0 . . ? C24 Cs1 H200 96.6 . . ? C11 Cs1 H200 64.7 . . ? C25 Cs1 H200 74.7 . . ? C37 Cs1 H200 129.3 2 . ? C36 Cs1 H200 143.6 2 . ? O4 Cs1 H200 47.8 . . ? C14 Cs1 H200 105.1 . . ? C23 Cs1 H200 104.5 . . ? O3 Cs1 H300 20.5 2 . ? O2 Cs1 H300 86.9 . . ? C16 Cs1 H300 153.3 . . ? C15 Cs1 H300 171.3 . . ? C24 Cs1 H300 86.5 . . ? C11 Cs1 H300 133.9 . . ? C25 Cs1 H300 82.1 . . ? C37 Cs1 H300 72.9 2 . ? C36 Cs1 H300 75.5 2 . ? O4 Cs1 H300 23.3 . . ? C14 Cs1 H300 151.4 . . ? C23 Cs1 H300 71.3 . . ? H200 Cs1 H300 70.3 . . ? C12 O1 H400 117.4 . . ? C2 C1 C6 120.0 . . ? C2 C1 C11 116.16(18) . . ? C6 C1 C11 123.84(18) . . ? O2 C2 C1 120.2(3) . . ? O2 C2 C3 119.4(3) . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C10 120.0 . . ? C6 C5 C10 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C1 120.0 . . ? C5 C6 C1 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C5 120.0 . . ? C9 C10 H10 120.0 . . ? C5 C10 H10 120.0 . . ? C2 O2 Cs1 136.7(3) . . ? C2 O2 H200 121.1 . . ? Cs1 O2 H200 100.0 . . ? C12 C11 C16 120.0 . . ? C12 C11 C1 116.76(17) . . ? C16 C11 C1 123.23(17) . . ? C12 C11 Cs1 87.47(8) . . ? C16 C11 Cs1 71.85(8) . . ? C1 C11 Cs1 110.71(17) . . ? O1 C12 C11 124.8(2) . . ? O1 C12 C13 115.1(2) . . ? C11 C12 C13 120.0 . . ? O1 C12 Cs1 115.5(2) . . ? C11 C12 Cs1 71.26(8) . . ? C13 C12 Cs1 81.05(10) . . ? C12 C13 C14 120.0 . . ? C12 C13 Cs1 78.13(10) . . ? C14 C13 Cs1 72.99(8) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? Cs1 C13 H13 119.9 . . ? C15 C14 C13 120.0 . . ? C15 C14 Cs1 70.61(7) . . ? C13 C14 Cs1 85.98(8) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? Cs1 C14 H14 113.7 . . ? C14 C15 C16 120.0 . . ? C14 C15 C20 120.0 . . ? C16 C15 C20 120.0 . . ? C14 C15 Cs1 87.37(9) . . ? C16 C15 Cs1 76.87(10) . . ? C20 C15 Cs1 105.84(8) . . ? C17 C16 C15 120.0 . . ? C17 C16 C11 120.0 . . ? C15 C16 C11 120.0 . . ? C17 C16 Cs1 104.33(8) . . ? C15 C16 Cs1 80.08(11) . . ? C11 C16 Cs1 85.69(9) . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C22 O3 Cs1 157.0(3) . 2 ? C22 C21 C26 120.0 . . ? C22 C21 C31 116.66(18) . . ? C26 C21 C31 123.33(18) . . ? O3 C22 C23 119.2(3) . . ? O3 C22 C21 120.6(3) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 Cs1 71.18(8) . . ? C22 C23 Cs1 88.33(10) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? Cs1 C23 H23 110.6 . . ? C23 C24 C25 120.0 . . ? C23 C24 Cs1 87.45(8) . . ? C25 C24 Cs1 79.70(8) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? Cs1 C24 H24 102.9 . . ? C24 C25 C26 120.0 . . ? C24 C25 C30 120.0 . . ? C26 C25 C30 120.0 . . ? C24 C25 Cs1 78.16(8) . . ? C26 C25 Cs1 88.25(10) . . ? C30 C25 Cs1 103.63(8) . . ? C27 C26 C25 120.0 . . ? C27 C26 C21 120.0 . . ? C25 C26 C21 120.0 . . ? C27 C26 Cs1 111.98(8) . . ? C25 C26 Cs1 70.58(10) . . ? C21 C26 Cs1 87.61(8) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 O4 Cs1 135.8(2) . . ? C32 C31 C36 120.0 . . ? C32 C31 C21 116.81(17) . . ? C36 C31 C21 123.18(17) . . ? O4 C32 C31 122.8(3) . . ? O4 C32 C33 116.6(3) . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 C40 120.0 . . ? C36 C35 C40 120.0 . . ? C34 C35 Cs1 111.30(7) . 2 ? C36 C35 Cs1 70.29(10) . 2 ? C40 C35 Cs1 88.51(7) . 2 ? C37 C36 C35 120.0 . . ? C37 C36 C31 120.0 . . ? C35 C36 C31 120.0 . . ? C37 C36 Cs1 78.74(8) . 2 ? C35 C36 Cs1 88.70(10) . 2 ? C31 C36 Cs1 102.59(8) . 2 ? C38 C37 C36 120.0 . . ? C38 C37 Cs1 88.42(8) . 2 ? C36 C37 Cs1 79.30(7) . 2 ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? Cs1 C37 H37 102.3 2 . ? C37 C38 C39 120.0 . . ? C37 C38 Cs1 70.51(7) . 2 ? C39 C38 Cs1 88.78(10) . 2 ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? Cs1 C38 H38 110.8 2 . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? _diffrn_measured_fraction_theta_max 0.835 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.835 _refine_diff_density_max 0.647 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.087 data_5 _database_code_CSD 154553 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H27 O4 Rb' _chemical_formula_weight 657.09 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 '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 10.6820(10) _cell_length_b 12.2140(10) _cell_length_c 12.6680(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 112.600(10) _cell_angle_gamma 100.030(10) _cell_volume 1498.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.696 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4373 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 22.98 _reflns_number_total 4153 _reflns_number_gt 2703 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1039P)^2^+3.8108P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4153 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Rb1 Rb 0.00697(9) 0.24687(6) 0.15917(8) 0.0792(4) Uani 1 1 d . . . O1 O -0.0897(4) 0.5905(3) 0.1363(3) 0.0416(10) Uani 1 1 d . . . C1 C 0.2012(3) 0.59015(19) 0.2298(2) 0.0332(13) Uani 1 1 d G . . C2 C 0.1927(3) 0.5489(2) 0.1245(2) 0.0388(14) Uani 1 1 d G . . C3 C 0.2770(3) 0.6049(2) 0.0734(2) 0.0460(16) Uani 1 1 d G . . H3 H 0.2713 0.5773 0.0029 0.055 Uiso 1 1 calc R . . C4 C 0.3699(3) 0.7021(2) 0.1276(2) 0.0480(16) Uani 1 1 d G . . H4 H 0.4263 0.7396 0.0934 0.058 Uiso 1 1 calc R . . C5 C 0.3784(2) 0.74337(17) 0.23289(19) 0.0398(14) Uani 1 1 d G . . C6 C 0.2941(2) 0.68739(16) 0.28399(18) 0.0326(13) Uani 1 1 d G . . C7 C 0.3026(3) 0.7286(2) 0.3893(2) 0.0413(15) Uani 1 1 d G . . H7 H 0.2462 0.6912 0.4235 0.050 Uiso 1 1 calc R . . C8 C 0.3955(3) 0.8258(2) 0.4435(2) 0.0499(17) Uani 1 1 d G . . H8 H 0.4012 0.8534 0.5140 0.060 Uiso 1 1 calc R . . C9 C 0.4798(3) 0.8818(2) 0.3924(3) 0.0573(19) Uani 1 1 d G . . H9 H 0.5420 0.9469 0.4287 0.069 Uiso 1 1 calc R . . C10 C 0.4713(3) 0.8406(2) 0.2871(3) 0.0510(17) Uani 1 1 d G . . H10 H 0.5277 0.8781 0.2529 0.061 Uiso 1 1 calc R . . O2 O 0.1131(4) 0.4472(3) 0.0771(3) 0.0471(11) Uani 1 1 d . . . H200 H 0.1076 0.4250 0.0037 0.050 Uiso 1 1 d . . . C11 C 0.1031(3) 0.5227(2) 0.2799(2) 0.0335(13) Uani 1 1 d G . . C12 C -0.0354(3) 0.5307(2) 0.2285(2) 0.0372(14) Uani 1 1 d G . . C13 C -0.1302(2) 0.4720(3) 0.2683(3) 0.0474(16) Uani 1 1 d G . . H13 H -0.2229 0.4774 0.2339 0.057 Uiso 1 1 calc R . . C14 C -0.0865(2) 0.4053(3) 0.3594(3) 0.0550(18) Uani 1 1 d G . . H14 H -0.1499 0.3661 0.3860 0.066 Uiso 1 1 calc R . . C15 C 0.0520(3) 0.3973(2) 0.4107(2) 0.0430(15) Uani 1 1 d G . . C16 C 0.1468(2) 0.45600(18) 0.37097(19) 0.0363(14) Uani 1 1 d G . . C17 C 0.2853(2) 0.4480(3) 0.4223(3) 0.0464(16) Uani 1 1 d G . . H17 H 0.3487 0.4873 0.3957 0.056 Uiso 1 1 calc R . . C18 C 0.3290(3) 0.3813(3) 0.5134(3) 0.0612(19) Uani 1 1 d G . . H18 H 0.4217 0.3760 0.5478 0.073 Uiso 1 1 calc R . . C19 C 0.2342(4) 0.3226(3) 0.5532(3) 0.070(2) Uani 1 1 d G . . H19 H 0.2635 0.2780 0.6142 0.084 Uiso 1 1 calc R . . C20 C 0.0957(3) 0.3306(3) 0.5019(3) 0.064(2) Uani 1 1 d G . . H20 H 0.0323 0.2914 0.5285 0.077 Uiso 1 1 calc R . . O3 O 0.1134(4) -0.0855(3) 0.0252(3) 0.0440(10) Uani 1 1 d . . . H300 H -0.0548 0.1387 -0.0558 0.050 Uiso 1 1 d . . . C21 C 0.2293(3) 0.1020(2) 0.0283(2) 0.0392(14) Uani 1 1 d G . . C22 C 0.1854(3) 0.01427(19) 0.0835(3) 0.0392(14) Uani 1 1 d G . . C23 C 0.2242(3) 0.0243(2) 0.2016(3) 0.0483(16) Uani 1 1 d G . . H23 H 0.1949 -0.0344 0.2385 0.058 Uiso 1 1 calc R . . C24 C 0.3069(3) 0.1221(2) 0.2646(2) 0.0508(17) Uani 1 1 d G . . H24 H 0.3328 0.1288 0.3436 0.061 Uiso 1 1 calc R . . C25 C 0.3507(2) 0.20974(19) 0.20938(18) 0.0421(15) Uani 1 1 d G . . C26 C 0.3119(2) 0.19970(18) 0.09124(18) 0.0381(14) Uani 1 1 d G . . C27 C 0.3557(3) 0.2874(2) 0.0361(2) 0.0449(15) Uani 1 1 d G . . H27 H 0.3298 0.2807 -0.0430 0.054 Uiso 1 1 calc R . . C28 C 0.4384(4) 0.3851(2) 0.0990(3) 0.0557(18) Uani 1 1 d G . . H28 H 0.4677 0.4438 0.0621 0.067 Uiso 1 1 calc R . . C29 C 0.4772(3) 0.3952(2) 0.2171(3) 0.061(2) Uani 1 1 d G . . H29 H 0.5325 0.4606 0.2593 0.073 Uiso 1 1 calc R . . C30 C 0.4333(3) 0.3075(2) 0.2723(2) 0.0531(17) Uani 1 1 d G . . H30 H 0.4593 0.3142 0.3514 0.064 Uiso 1 1 calc R . . O4 O 0.0228(4) 0.2136(3) -0.1192(3) 0.0424(10) Uani 1 1 d . . . H400 H -0.0348 0.6993 0.1401 0.050 Uiso 1 1 d . . . C31 C 0.1767(3) 0.0845(2) -0.1037(2) 0.0357(14) Uani 1 1 d G . . C32 C 0.0837(3) 0.1498(2) -0.1672(3) 0.0376(14) Uani 1 1 d G . . C33 C 0.0369(3) 0.1430(2) -0.2861(3) 0.0466(16) Uani 1 1 d G . . H33 H -0.0253 0.1866 -0.3286 0.056 Uiso 1 1 calc R . . C34 C 0.0832(3) 0.0708(3) -0.34152(19) 0.0489(16) Uani 1 1 d G . . H34 H 0.0519 0.0662 -0.4211 0.059 Uiso 1 1 calc R . . C35 C 0.1762(2) 0.00556(19) -0.27805(18) 0.0422(15) Uani 1 1 d G . . C36 C 0.2230(2) 0.01241(17) -0.15916(18) 0.0350(14) Uani 1 1 d G . . C37 C 0.3161(3) -0.0529(3) -0.0957(2) 0.0466(16) Uani 1 1 d G . . H37 H 0.3474 -0.0483 -0.0161 0.056 Uiso 1 1 calc R . . C38 C 0.3624(3) -0.1250(3) -0.1511(3) 0.0570(18) Uani 1 1 d G . . H38 H 0.4246 -0.1687 -0.1086 0.068 Uiso 1 1 calc R . . C39 C 0.3156(4) -0.1319(3) -0.2700(3) 0.0609(19) Uani 1 1 d G . . H39 H 0.3466 -0.1801 -0.3071 0.073 Uiso 1 1 calc R . . C40 C 0.2225(4) -0.0666(3) -0.3335(2) 0.0544(17) Uani 1 1 d G . . H40 H 0.1912 -0.0712 -0.4130 0.065 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 Rb1 0.0906(7) 0.0474(5) 0.0905(7) -0.0112(4) 0.0325(5) -0.0034(4) O1 0.042(2) 0.032(2) 0.047(2) 0.0051(19) 0.013(2) 0.0081(18) C1 0.034(3) 0.032(3) 0.034(3) 0.007(2) 0.012(3) 0.013(3) C2 0.041(3) 0.034(3) 0.045(4) 0.005(3) 0.019(3) 0.008(3) C3 0.058(4) 0.043(4) 0.042(4) 0.002(3) 0.026(3) 0.007(3) C4 0.054(4) 0.046(4) 0.052(4) 0.016(3) 0.031(3) 0.006(3) C5 0.036(3) 0.031(3) 0.053(4) 0.007(3) 0.018(3) 0.007(3) C6 0.034(3) 0.026(3) 0.038(3) 0.005(2) 0.013(3) 0.008(2) C7 0.041(4) 0.032(3) 0.052(4) 0.003(3) 0.021(3) 0.004(3) C8 0.058(4) 0.038(4) 0.052(4) -0.001(3) 0.020(3) 0.009(3) C9 0.051(4) 0.032(3) 0.074(5) 0.000(3) 0.013(4) -0.005(3) C10 0.047(4) 0.041(4) 0.065(5) 0.007(3) 0.024(3) 0.001(3) O2 0.055(3) 0.040(2) 0.046(2) -0.0086(19) 0.023(2) 0.001(2) C11 0.033(3) 0.026(3) 0.041(3) -0.003(2) 0.016(3) 0.000(2) C12 0.048(4) 0.027(3) 0.038(3) -0.003(3) 0.020(3) 0.004(3) C13 0.039(4) 0.044(4) 0.060(4) 0.007(3) 0.021(3) 0.003(3) C14 0.056(5) 0.052(4) 0.064(4) 0.018(3) 0.035(4) 0.003(3) C15 0.051(4) 0.036(3) 0.046(4) 0.012(3) 0.023(3) 0.009(3) C16 0.043(4) 0.032(3) 0.037(3) 0.007(3) 0.018(3) 0.010(3) C17 0.050(4) 0.041(4) 0.053(4) 0.014(3) 0.022(3) 0.016(3) C18 0.059(5) 0.065(5) 0.062(5) 0.020(4) 0.021(4) 0.025(4) C19 0.095(6) 0.058(5) 0.060(5) 0.032(4) 0.028(5) 0.025(4) C20 0.070(5) 0.060(5) 0.069(5) 0.028(4) 0.036(4) 0.007(4) O3 0.047(3) 0.036(2) 0.054(3) 0.010(2) 0.027(2) 0.0035(19) C21 0.036(3) 0.045(4) 0.044(4) 0.015(3) 0.020(3) 0.017(3) C22 0.038(3) 0.039(3) 0.046(4) 0.010(3) 0.022(3) 0.009(3) C23 0.046(4) 0.051(4) 0.048(4) 0.017(3) 0.019(3) 0.008(3) C24 0.049(4) 0.061(4) 0.038(4) 0.007(3) 0.013(3) 0.010(3) C25 0.035(3) 0.046(4) 0.044(4) 0.000(3) 0.012(3) 0.012(3) C26 0.034(3) 0.035(3) 0.051(4) 0.007(3) 0.020(3) 0.012(3) C27 0.040(4) 0.044(4) 0.055(4) 0.008(3) 0.022(3) 0.012(3) C28 0.052(4) 0.040(4) 0.079(5) 0.012(4) 0.031(4) 0.008(3) C29 0.052(4) 0.040(4) 0.083(6) -0.004(4) 0.019(4) 0.007(3) C30 0.051(4) 0.056(4) 0.054(4) -0.004(3) 0.018(3) 0.019(3) O4 0.047(3) 0.032(2) 0.059(3) 0.0159(19) 0.030(2) 0.0137(19) C31 0.034(3) 0.029(3) 0.042(3) 0.008(3) 0.014(3) 0.001(3) C32 0.043(4) 0.029(3) 0.044(4) 0.009(3) 0.022(3) 0.005(3) C33 0.047(4) 0.043(4) 0.053(4) 0.015(3) 0.020(3) 0.014(3) C34 0.051(4) 0.053(4) 0.047(4) 0.008(3) 0.022(3) 0.013(3) C35 0.044(4) 0.041(3) 0.048(4) 0.004(3) 0.026(3) 0.005(3) C36 0.030(3) 0.030(3) 0.048(4) 0.006(3) 0.019(3) 0.005(2) C37 0.040(4) 0.056(4) 0.051(4) 0.011(3) 0.022(3) 0.016(3) C38 0.049(4) 0.053(4) 0.081(5) 0.017(4) 0.032(4) 0.024(3) C39 0.056(4) 0.059(4) 0.081(5) -0.005(4) 0.039(4) 0.013(4) C40 0.050(4) 0.058(4) 0.055(4) -0.006(3) 0.022(3) 0.008(3) _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 Rb1 O3 2.793(4) 2 ? Rb1 O2 2.880(4) . ? Rb1 C16 3.398(2) . ? Rb1 C15 3.504(3) . ? Rb1 C11 3.511(3) . ? Rb1 C24 3.575(4) . ? Rb1 C25 3.588(3) . ? Rb1 O4 3.620(4) . ? Rb1 C37 3.632(10) 2 ? Rb1 C36 3.654(10) 2 ? Rb1 C14 3.714(4) . ? Rb1 C12 3.721(3) . ? Rb1 H200 3.2527 . ? Rb1 H300 2.8129 . ? O1 C12 1.365(4) . ? O1 H400 1.3480 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C11 1.546(3) . ? C2 O2 1.366(4) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? O2 H200 0.9455 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? O3 C22 1.364(4) . ? O3 Rb1 2.793(4) 2 ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C21 C31 1.547(3) . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? O4 C32 1.371(4) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C36 Rb1 3.654(2) 2 ? C37 C38 1.3900 . ? C37 Rb1 3.632(4) 2 ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Rb1 O2 107.45(11) 2 . ? O3 Rb1 C16 176.24(9) 2 . ? O2 Rb1 C16 69.41(9) . . ? O3 Rb1 C15 158.39(9) 2 . ? O2 Rb1 C15 90.21(9) . . ? C16 Rb1 C15 23.2 . . ? O3 Rb1 C11 153.11(9) 2 . ? O2 Rb1 C11 50.30(8) . . ? C16 Rb1 C11 23.1 . . ? C15 Rb1 C11 40.1 . . ? O3 Rb1 C24 89.66(10) 2 . ? O2 Rb1 C24 100.37(10) . . ? C16 Rb1 C24 92.95(6) . . ? C15 Rb1 C24 99.52(6) . . ? C11 Rb1 C24 107.72(7) . . ? O3 Rb1 C25 93.12(9) 2 . ? O2 Rb1 C25 78.24(10) . . ? C16 Rb1 C25 88.28(6) . . ? C15 Rb1 C25 102.83(6) . . ? C11 Rb1 C25 95.77(6) . . ? C24 Rb1 C25 22.4 . . ? O3 Rb1 O4 44.65(10) 2 . ? O2 Rb1 O4 64.58(10) . . ? C16 Rb1 O4 132.85(8) . . ? C15 Rb1 O4 154.79(7) . . ? C11 Rb1 O4 114.74(7) . . ? C24 Rb1 O4 85.66(7) . . ? C25 Rb1 O4 73.13(7) . . ? O3 Rb1 C37 55.28(14) 2 2 ? O2 Rb1 C37 139.60(18) . 2 ? C16 Rb1 C37 125.66(12) . 2 ? C15 Rb1 C37 103.17(13) . 2 ? C11 Rb1 C37 128.64(12) . 2 ? C24 Rb1 C37 114.33(14) . 2 ? C25 Rb1 C37 132.99(13) . 2 ? O4 Rb1 C37 96.91(15) . 2 ? O3 Rb1 C36 56.42(15) 2 2 ? O2 Rb1 C36 159.28(19) . 2 ? C16 Rb1 C36 126.06(13) . 2 ? C15 Rb1 C36 103.28(13) . 2 ? C11 Rb1 C36 139.38(10) . 2 ? C24 Rb1 C36 92.93(14) . 2 ? C25 Rb1 C36 113.14(13) . 2 ? O4 Rb1 C36 101.05(14) . 2 ? C37 Rb1 C36 21.99(6) 2 2 ? O3 Rb1 C14 140.50(10) 2 . ? O2 Rb1 C14 92.65(9) . . ? C16 Rb1 C14 39.3 . . ? C15 Rb1 C14 22.0 . . ? C11 Rb1 C14 45.1 . . ? C24 Rb1 C14 120.39(6) . . ? C25 Rb1 C14 124.67(6) . . ? O4 Rb1 C14 149.15(8) . . ? C37 Rb1 C14 87.34(12) 2 . ? C36 Rb1 C14 94.24(10) 2 . ? O3 Rb1 C12 137.42(9) 2 . ? O2 Rb1 C12 55.95(9) . . ? C16 Rb1 C12 39.2 . . ? C15 Rb1 C12 45.1 . . ? C11 Rb1 C12 21.9 . . ? C24 Rb1 C12 129.52(7) . . ? C25 Rb1 C12 116.98(6) . . ? O4 Rb1 C12 113.57(7) . . ? C37 Rb1 C12 109.17(12) 2 . ? C36 Rb1 C12 125.02(10) 2 . ? C14 Rb1 C12 37.8 . . ? O3 Rb1 H200 91.4 2 . ? O2 Rb1 H200 16.3 . . ? C16 Rb1 H200 85.6 . . ? C15 Rb1 H200 106.5 . . ? C11 Rb1 H200 66.5 . . ? C24 Rb1 H200 97.7 . . ? C25 Rb1 H200 75.5 . . ? O4 Rb1 H200 48.3 . . ? C37 Rb1 H200 131.4 2 . ? C36 Rb1 H200 146.1 2 . ? C14 Rb1 H200 107.6 . . ? C12 Rb1 H200 70.0 . . ? O3 Rb1 H300 20.7 2 . ? O2 Rb1 H300 87.8 . . ? C16 Rb1 H300 156.8 . . ? C15 Rb1 H300 173.4 . . ? C11 Rb1 H300 136.9 . . ? C24 Rb1 H300 87.1 . . ? C25 Rb1 H300 82.9 . . ? O4 Rb1 H300 24.0 . . ? C37 Rb1 H300 74.6 2 . ? C36 Rb1 H300 77.0 2 . ? C14 Rb1 H300 151.9 . . ? C12 Rb1 H300 129.3 . . ? H200 Rb1 H300 71.5 . . ? C12 O1 H400 119.6 . . ? C2 C1 C6 120.0 . . ? C2 C1 C11 116.41(17) . . ? C6 C1 C11 123.59(17) . . ? O2 C2 C1 120.1(2) . . ? O2 C2 C3 119.5(2) . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C10 120.0 . . ? C6 C5 C10 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 C1 120.0 . . ? C5 C6 C1 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C5 120.0 . . ? C9 C10 H10 120.0 . . ? C5 C10 H10 120.0 . . ? C2 O2 Rb1 136.4(3) . . ? C2 O2 H200 116.4 . . ? Rb1 O2 H200 104.8 . . ? C12 C11 C16 120.0 . . ? C12 C11 C1 116.59(18) . . ? C16 C11 C1 123.41(18) . . ? C12 C11 Rb1 87.56(9) . . ? C16 C11 Rb1 73.84(8) . . ? C1 C11 Rb1 108.86(17) . . ? O1 C12 C11 124.6(2) . . ? O1 C12 C13 115.3(2) . . ? C11 C12 C13 120.0 . . ? O1 C12 Rb1 115.3(2) . . ? C11 C12 Rb1 70.52(8) . . ? C13 C12 Rb1 83.34(11) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 Rb1 70.48(8) . . ? C13 C14 Rb1 83.62(8) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? Rb1 C14 H14 116.4 . . ? C14 C15 C16 120.0 . . ? C14 C15 C20 120.0 . . ? C16 C15 C20 120.0 . . ? C14 C15 Rb1 87.56(9) . . ? C16 C15 Rb1 74.12(11) . . ? C20 C15 Rb1 108.43(8) . . ? C17 C16 C15 120.0 . . ? C17 C16 C11 120.0 . . ? C15 C16 C11 120.0 . . ? C17 C16 Rb1 104.39(9) . . ? C15 C16 Rb1 82.71(12) . . ? C11 C16 Rb1 83.02(9) . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 120.0 . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C22 O3 Rb1 157.7(3) . 2 ? C22 C21 C26 120.0 . . ? C22 C21 C31 116.24(18) . . ? C26 C21 C31 123.73(18) . . ? O3 C22 C23 118.7(2) . . ? O3 C22 C21 121.1(2) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 Rb1 79.34(8) . . ? C23 C24 Rb1 87.62(8) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? Rb1 C24 H24 103.1 . . ? C26 C25 C24 120.0 . . ? C26 C25 C30 120.0 . . ? C24 C25 C30 120.0 . . ? C26 C25 Rb1 88.17(11) . . ? C24 C25 Rb1 78.28(9) . . ? C30 C25 Rb1 103.59(8) . . ? C27 C26 C25 120.0 . . ? C27 C26 C21 120.0 . . ? C25 C26 C21 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 O4 Rb1 135.8(2) . . ? C32 C31 C36 120.0 . . ? C32 C31 C21 116.56(18) . . ? C36 C31 C21 123.36(18) . . ? O4 C32 C33 116.8(2) . . ? O4 C32 C31 122.9(2) . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C40 120.0 . . ? C34 C35 C40 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 C31 120.0 . . ? C35 C36 C31 120.0 . . ? C37 C36 Rb1 78.08(9) . 2 ? C35 C36 Rb1 92.71(11) . 2 ? C31 C36 Rb1 99.16(8) . 2 ? C36 C37 C38 120.0 . . ? C36 C37 Rb1 79.93(8) . 2 ? C38 C37 Rb1 91.79(9) . 2 ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? Rb1 C37 H37 98.3 2 . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C35 120.0 . . ? C39 C40 H40 120.0 . . ? C35 C40 H40 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.695 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.085