# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Rick Wong' _publ_contact_author_address ; Department of Chemistry Hong Kong Baptist University 224 Waterloo Road Kowloon CHINA ; _publ_contact_author_email WKWONG@HKBU.EDU.HK _publ_section_title ; Synthesis and crystal structure of the first lanthanide complex of N-confused porphyrin with an (eta)2 agostic C-H interaction ; loop_ _publ_author_name 'Rick Wong' 'Wing-Kit Lo' 'Wai-Yeung Wong' 'Xunjin Zhu' data_wy1066wm _database_code_depnum_ccdc_archive 'CCDC 253410' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H53 Co N4 O10 P3 Yb' _chemical_formula_weight 1254.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7713(8) _cell_length_b 28.6597(18) _cell_length_c 14.9785(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.9420(10) _cell_angle_gamma 90.00 _cell_volume 5360.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2532 _exptl_absorpt_coefficient_mu 2.195 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8571 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Smart CCD' _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 26345 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9439 _reflns_number_gt 7304 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction SAINT _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^)+(0.0494P)^2^+16.2701P] 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 9439 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.004 _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 C1 C 0.8796(10) 0.1560(4) 0.5874(6) 0.100(4) Uani 1 1 d . . . H1A H 0.9386 0.1338 0.6183 0.121 Uiso 1 1 calc R . . C2 C 0.7739(11) 0.1523(3) 0.5821(6) 0.091(3) Uani 1 1 d . . . H2A H 0.7467 0.1264 0.6075 0.109 Uiso 1 1 calc R . . C3 C 0.7184(8) 0.1915(3) 0.5384(6) 0.081(3) Uani 1 1 d . . . H3A H 0.6439 0.1979 0.5259 0.097 Uiso 1 1 calc R . . C4 C 0.7835(7) 0.2205(3) 0.5142(6) 0.068(2) Uani 1 1 d . . . H4A H 0.7626 0.2509 0.4818 0.081 Uiso 1 1 calc R . . C5 C 0.8834(7) 0.1999(3) 0.5429(6) 0.075(2) Uani 1 1 d . . . H5A H 0.9457 0.2134 0.5366 0.090 Uiso 1 1 calc R . . C6 C 0.7340(8) 0.0142(4) 0.4788(7) 0.097(3) Uani 1 1 d . . . H6A H 0.6627 0.0205 0.4717 0.145 Uiso 1 1 calc R . . H6B H 0.7693 -0.0062 0.5340 0.145 Uiso 1 1 calc R . . H6C H 0.7309 -0.0005 0.4201 0.145 Uiso 1 1 calc R . . C7 C 0.9964(10) 0.0553(4) 0.4363(10) 0.133(5) Uani 1 1 d . . . H7A H 0.9721 0.0246 0.4427 0.199 Uiso 1 1 calc R . . H7B H 1.0711 0.0582 0.4792 0.199 Uiso 1 1 calc R . . H7C H 0.9858 0.0602 0.3694 0.199 Uiso 1 1 calc R . . C8 C 0.9828(9) 0.1731(4) 0.2989(10) 0.127(4) Uani 1 1 d . . . H8A H 0.9504 0.1458 0.2608 0.191 Uiso 1 1 calc R . . H8B H 1.0557 0.1663 0.3428 0.191 Uiso 1 1 calc R . . H8C H 0.9812 0.1981 0.2556 0.191 Uiso 1 1 calc R . . C9 C 0.7386(9) 0.2567(3) 0.2115(7) 0.099(3) Uani 1 1 d . . . H9A H 0.8064 0.2683 0.2175 0.149 Uiso 1 1 calc R . . H9B H 0.6901 0.2823 0.2014 0.149 Uiso 1 1 calc R . . H9C H 0.7096 0.2357 0.1564 0.149 Uiso 1 1 calc R . . C10 C 0.4474(8) 0.0957(3) 0.3507(7) 0.090(3) Uani 1 1 d . . . H10A H 0.4488 0.0770 0.2981 0.136 Uiso 1 1 calc R . . H10B H 0.3936 0.1194 0.3240 0.136 Uiso 1 1 calc R . . H10C H 0.4313 0.0763 0.3950 0.136 Uiso 1 1 calc R . . C11 C 0.4854(7) 0.2158(3) 0.2310(7) 0.083(3) Uani 1 1 d . . . H11A H 0.5382 0.2279 0.2111 0.124 Uiso 1 1 calc R . . H11B H 0.4417 0.2409 0.2358 0.124 Uiso 1 1 calc R . . H11C H 0.4412 0.1936 0.1832 0.124 Uiso 1 1 calc R . . C12 C 0.5517(6) -0.1094(2) 0.2495(6) 0.0575(18) Uani 1 1 d . . . H12A H 0.5782 -0.1191 0.2048 0.069 Uiso 1 1 calc R . . C13 C 0.5358(7) -0.1421(3) 0.3112(7) 0.081(3) Uani 1 1 d . . . H13A H 0.5512 -0.1734 0.3069 0.097 Uiso 1 1 calc R . . C14 C 0.4979(6) -0.1284(3) 0.3771(7) 0.081(3) Uani 1 1 d . . . H14A H 0.4892 -0.1503 0.4190 0.097 Uiso 1 1 calc R . . C15 C 0.4726(6) -0.0829(3) 0.3822(6) 0.069(2) Uani 1 1 d . . . H15A H 0.4448 -0.0738 0.4263 0.082 Uiso 1 1 calc R . . C16 C 0.4882(5) -0.0502(3) 0.3219(5) 0.0503(16) Uani 1 1 d . . . H16A H 0.4716 -0.0191 0.3266 0.060 Uiso 1 1 calc R . . C17 C 0.5283(5) -0.0627(2) 0.2543(5) 0.0420(14) Uani 1 1 d . . . C18 C 0.5518(4) -0.02694(19) 0.1946(4) 0.0351(13) Uani 1 1 d . . . C19 C 0.6551(4) -0.02579(18) 0.1968(4) 0.0347(13) Uani 1 1 d . . . C20 C 0.6928(5) 0.0005(2) 0.1384(5) 0.0362(13) Uani 1 1 d . . . C21 C 0.8040(5) -0.0063(2) 0.1761(5) 0.0385(13) Uani 1 1 d . . . C22 C 0.8292(5) -0.0378(2) 0.2569(5) 0.0414(14) Uani 1 1 d . . . H22A H 0.8978 -0.0488 0.2956 0.050 Uiso 1 1 calc R . . C23 C 0.8803(5) 0.0160(2) 0.1502(5) 0.0431(15) Uani 1 1 d . . . C24 C 0.9885(5) -0.0055(2) 0.1830(5) 0.0460(15) Uani 1 1 d . . . C25 C 1.0818(5) 0.0204(3) 0.2243(6) 0.065(2) Uani 1 1 d . . . H25A H 1.0782 0.0523 0.2337 0.078 Uiso 1 1 calc R . . C26 C 1.1812(6) -0.0011(4) 0.2521(7) 0.081(3) Uani 1 1 d . . . H26A H 1.2435 0.0166 0.2797 0.097 Uiso 1 1 calc R . . C27 C 1.1875(6) -0.0481(4) 0.2389(7) 0.076(3) Uani 1 1 d . . . H27A H 1.2539 -0.0622 0.2568 0.091 Uiso 1 1 calc R . . C28 C 1.0962(6) -0.0741(3) 0.1994(6) 0.068(2) Uani 1 1 d . . . H28A H 1.1005 -0.1062 0.1920 0.082 Uiso 1 1 calc R . . C29 C 0.9977(5) -0.0530(2) 0.1704(5) 0.0543(17) Uani 1 1 d . . . H29A H 0.9359 -0.0710 0.1418 0.065 Uiso 1 1 calc R . . C30 C 0.8577(5) 0.0572(2) 0.0965(5) 0.0441(15) Uani 1 1 d . . . C31 C 0.9218(5) 0.0778(3) 0.0509(6) 0.0578(19) Uani 1 1 d . . . H31A H 0.9848 0.0657 0.0517 0.069 Uiso 1 1 calc R . . C32 C 0.8736(5) 0.1178(2) 0.0073(6) 0.0557(18) Uani 1 1 d . . . H32A H 0.8975 0.1383 -0.0271 0.067 Uiso 1 1 calc R . . C33 C 0.7781(5) 0.1228(2) 0.0236(5) 0.0420(14) Uani 1 1 d . . . C34 C 0.7043(5) 0.1595(2) -0.0140(4) 0.0398(14) Uani 1 1 d . . . C35 C 0.7347(5) 0.1992(2) -0.0642(5) 0.0520(17) Uani 1 1 d . . . C36 C 0.7900(12) 0.2360(4) -0.0142(9) 0.161(7) Uani 1 1 d . . . H36A H 0.8116 0.2376 0.0536 0.193 Uiso 1 1 calc R . . C37 C 0.8158(15) 0.2727(4) -0.0634(11) 0.178(8) Uani 1 1 d . . . H37A H 0.8529 0.2985 -0.0278 0.213 Uiso 1 1 calc R . . C38 C 0.7890(11) 0.2709(4) -0.1568(10) 0.112(4) Uani 1 1 d . . . H38A H 0.8034 0.2960 -0.1886 0.134 Uiso 1 1 calc R . . C39 C 0.7421(10) 0.2342(4) -0.2062(8) 0.116(4) Uani 1 1 d . . . H39A H 0.7280 0.2319 -0.2725 0.140 Uiso 1 1 calc R . . C40 C 0.7123(8) 0.1979(3) -0.1599(7) 0.097(3) Uani 1 1 d . . . H40A H 0.6760 0.1722 -0.1970 0.116 Uiso 1 1 calc R . . C41 C 0.6030(5) 0.1619(2) -0.0136(4) 0.0397(14) Uani 1 1 d . . . C42 C 0.5251(5) 0.1978(2) -0.0580(5) 0.0469(15) Uani 1 1 d . . . H42A H 0.5349 0.2247 -0.0878 0.056 Uiso 1 1 calc R . . C43 C 0.4361(5) 0.1859(2) -0.0491(5) 0.0444(15) Uani 1 1 d . . . H43A H 0.3731 0.2032 -0.0710 0.053 Uiso 1 1 calc R . . C44 C 0.4547(5) 0.1415(2) 0.0004(4) 0.0377(13) Uani 1 1 d . . . C45 C 0.3785(4) 0.1156(2) 0.0194(4) 0.0377(13) Uani 1 1 d . . . C46 C 0.2694(5) 0.1373(2) -0.0123(5) 0.0427(14) Uani 1 1 d . . . C47 C 0.2316(5) 0.1486(2) 0.0576(6) 0.0547(17) Uani 1 1 d . . . H47A H 0.2721 0.1413 0.1235 0.066 Uiso 1 1 calc R . . C48 C 0.1327(6) 0.1710(3) 0.0290(7) 0.072(2) Uani 1 1 d . . . H48A H 0.1079 0.1789 0.0760 0.086 Uiso 1 1 calc R . . C49 C 0.0723(6) 0.1812(3) -0.0684(8) 0.075(3) Uani 1 1 d . . . H49A H 0.0067 0.1961 -0.0875 0.090 Uiso 1 1 calc R . . C50 C 0.1086(6) 0.1694(3) -0.1370(7) 0.067(2) Uani 1 1 d . . . H50A H 0.0676 0.1764 -0.2029 0.081 Uiso 1 1 calc R . . C51 C 0.2054(5) 0.1472(2) -0.1096(5) 0.0516(16) Uani 1 1 d . . . H51A H 0.2281 0.1386 -0.1576 0.062 Uiso 1 1 calc R . . C52 C 0.3964(4) 0.0710(2) 0.0649(4) 0.0359(13) Uani 1 1 d . . . C53 C 0.3139(5) 0.0425(2) 0.0737(4) 0.0399(14) Uani 1 1 d . . . H53A H 0.2417 0.0500 0.0506 0.048 Uiso 1 1 calc R . . C54 C 0.3609(5) 0.0035(2) 0.1210(4) 0.0406(14) Uani 1 1 d . . . H54A H 0.3272 -0.0212 0.1369 0.049 Uiso 1 1 calc R . . C55 C 0.4729(4) 0.0064(2) 0.1431(4) 0.0353(13) Uani 1 1 d . . . Co1 Co 0.76841(7) 0.15656(3) 0.44194(6) 0.0468(2) Uani 1 1 d . . . N1 N 0.7432(4) -0.04944(18) 0.2697(4) 0.0495(13) Uani 1 1 d . . . N2 N 0.7702(4) 0.08558(16) 0.0779(4) 0.0389(11) Uani 1 1 d . . . N3 N 0.5592(4) 0.12795(16) 0.0234(4) 0.0373(11) Uani 1 1 d . . . N4 N 0.4917(4) 0.04827(15) 0.1067(3) 0.0334(10) Uani 1 1 d . . . O1 O 0.7870(14) 0.0529(2) 0.4932(5) 0.257(9) Uani 1 1 d . . . O2 O 0.9414(7) 0.0866(4) 0.4604(6) 0.173(5) Uani 1 1 d . . . O3 O 0.7599(4) 0.06454(16) 0.3200(4) 0.0680(14) Uani 1 1 d . . . O4 O 0.9258(5) 0.1864(3) 0.3539(5) 0.131(3) Uani 1 1 d . . . O5 O 0.7524(6) 0.23311(18) 0.2968(4) 0.098(2) Uani 1 1 d . . . O6 O 0.7582(4) 0.15274(17) 0.2249(4) 0.0669(14) Uani 1 1 d . . . O7 O 0.5474(5) 0.1167(2) 0.4017(4) 0.0870(19) Uani 1 1 d . . . O8 O 0.5364(6) 0.1940(2) 0.3225(5) 0.111(3) Uani 1 1 d . . . O9 O 0.5737(4) 0.12314(18) 0.2451(4) 0.0639(13) Uani 1 1 d . . . O10 O 0.8254(11) 0.8655(5) 0.3954(13) 0.290(9) Uani 1 1 d . . . P1 P 0.8094(2) 0.08591(8) 0.42097(16) 0.0786(7) Uani 1 1 d . . . P2 P 0.80083(18) 0.18006(7) 0.31971(15) 0.0639(5) Uani 1 1 d . . . P3 P 0.60113(16) 0.14620(7) 0.34233(14) 0.0580(5) Uani 1 1 d . . . Yb1 Yb 0.660562(19) 0.087633(8) 0.166513(18) 0.03353(9) Uani 1 1 d . . . H20 H 0.654(5) 0.010(2) 0.078(5) 0.036(17) 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 C1 0.125(9) 0.090(7) 0.037(5) -0.026(5) -0.015(5) 0.033(7) C2 0.157(11) 0.075(6) 0.039(5) -0.014(4) 0.040(6) -0.029(7) C3 0.109(7) 0.093(7) 0.055(5) -0.031(5) 0.048(5) -0.021(6) C4 0.098(6) 0.055(4) 0.051(5) -0.017(4) 0.033(5) -0.011(4) C5 0.077(6) 0.085(6) 0.057(5) -0.035(5) 0.023(4) -0.026(5) C6 0.097(7) 0.121(9) 0.082(7) -0.002(6) 0.047(6) -0.013(6) C7 0.107(9) 0.120(10) 0.166(13) -0.006(9) 0.054(9) 0.022(8) C8 0.101(8) 0.146(11) 0.163(12) -0.025(9) 0.084(9) -0.029(8) C9 0.151(10) 0.071(6) 0.084(7) 0.012(5) 0.058(7) 0.001(6) C10 0.088(7) 0.098(7) 0.080(6) -0.003(5) 0.030(5) -0.035(5) C11 0.090(6) 0.070(5) 0.087(7) 0.016(5) 0.036(6) 0.015(5) C12 0.067(5) 0.047(4) 0.073(5) 0.003(4) 0.044(4) -0.006(3) C13 0.093(6) 0.054(5) 0.117(8) 0.027(5) 0.066(6) 0.005(4) C14 0.069(5) 0.090(6) 0.098(7) 0.049(5) 0.050(5) 0.005(5) C15 0.053(4) 0.109(7) 0.059(5) 0.025(5) 0.038(4) 0.008(4) C16 0.043(4) 0.067(4) 0.047(4) 0.009(3) 0.026(3) 0.004(3) C17 0.040(3) 0.046(4) 0.043(4) 0.006(3) 0.020(3) -0.004(3) C18 0.042(3) 0.036(3) 0.034(3) -0.005(3) 0.023(3) -0.009(3) C19 0.040(3) 0.029(3) 0.040(3) -0.004(2) 0.022(3) -0.002(2) C20 0.039(3) 0.035(3) 0.041(4) -0.002(3) 0.023(3) -0.003(3) C21 0.038(3) 0.038(3) 0.045(4) -0.005(3) 0.024(3) -0.002(2) C22 0.040(3) 0.043(3) 0.045(4) 0.004(3) 0.022(3) 0.004(3) C23 0.038(3) 0.050(4) 0.048(4) -0.006(3) 0.025(3) -0.001(3) C24 0.035(3) 0.065(4) 0.046(4) 0.001(3) 0.025(3) -0.002(3) C25 0.043(4) 0.080(5) 0.069(5) 0.006(4) 0.022(4) -0.007(4) C26 0.041(4) 0.117(8) 0.078(6) 0.014(6) 0.020(4) -0.016(5) C27 0.047(5) 0.106(7) 0.081(6) 0.031(5) 0.033(4) 0.021(5) C28 0.061(5) 0.082(5) 0.072(5) 0.013(4) 0.038(4) 0.019(4) C29 0.048(4) 0.062(4) 0.059(5) 0.003(4) 0.029(4) 0.005(3) C30 0.041(3) 0.050(4) 0.049(4) -0.003(3) 0.027(3) -0.009(3) C31 0.046(4) 0.075(5) 0.067(5) 0.004(4) 0.039(4) 0.000(3) C32 0.053(4) 0.062(4) 0.068(5) 0.013(4) 0.040(4) -0.007(3) C33 0.045(3) 0.046(3) 0.046(4) -0.006(3) 0.029(3) -0.011(3) C34 0.047(3) 0.044(3) 0.037(3) -0.005(3) 0.025(3) -0.014(3) C35 0.061(4) 0.049(4) 0.065(5) 0.003(3) 0.044(4) -0.006(3) C36 0.284(17) 0.142(10) 0.109(9) -0.069(8) 0.135(11) -0.155(12) C37 0.32(2) 0.116(10) 0.157(13) -0.066(9) 0.165(15) -0.148(12) C38 0.177(12) 0.065(6) 0.144(11) 0.008(7) 0.117(10) -0.026(7) C39 0.154(11) 0.126(10) 0.089(8) 0.028(7) 0.071(8) -0.026(8) C40 0.134(9) 0.096(7) 0.067(6) 0.010(5) 0.049(6) -0.044(6) C41 0.049(4) 0.038(3) 0.036(3) 0.001(3) 0.021(3) -0.009(3) C42 0.057(4) 0.036(3) 0.059(4) 0.008(3) 0.035(3) -0.001(3) C43 0.044(3) 0.038(3) 0.054(4) 0.001(3) 0.023(3) 0.003(3) C44 0.039(3) 0.041(3) 0.038(3) -0.002(3) 0.021(3) 0.001(3) C45 0.040(3) 0.041(3) 0.034(3) 0.002(3) 0.018(3) -0.001(3) C46 0.038(3) 0.037(3) 0.055(4) 0.000(3) 0.021(3) -0.007(3) C47 0.043(4) 0.062(4) 0.063(5) 0.004(4) 0.026(4) 0.001(3) C48 0.057(5) 0.074(5) 0.106(7) -0.002(5) 0.055(5) 0.005(4) C49 0.037(4) 0.062(5) 0.122(8) 0.019(5) 0.030(5) 0.007(3) C50 0.048(4) 0.060(5) 0.079(6) 0.024(4) 0.012(4) 0.000(4) C51 0.045(4) 0.050(4) 0.050(4) 0.005(3) 0.011(3) -0.003(3) C52 0.039(3) 0.040(3) 0.032(3) -0.004(2) 0.017(3) -0.006(2) C53 0.032(3) 0.052(4) 0.039(3) 0.002(3) 0.017(3) -0.009(3) C54 0.038(3) 0.048(4) 0.042(3) 0.000(3) 0.023(3) -0.010(3) C55 0.038(3) 0.042(3) 0.032(3) -0.005(3) 0.021(3) -0.010(3) Co1 0.0624(6) 0.0422(5) 0.0351(5) -0.0075(4) 0.0198(4) -0.0114(4) N1 0.053(3) 0.044(3) 0.058(4) -0.002(3) 0.029(3) -0.001(2) N2 0.040(3) 0.041(3) 0.043(3) -0.002(2) 0.024(2) -0.006(2) N3 0.040(3) 0.041(3) 0.038(3) 0.006(2) 0.023(2) -0.007(2) N4 0.036(3) 0.033(2) 0.036(3) -0.004(2) 0.020(2) -0.006(2) O1 0.62(3) 0.050(4) 0.042(4) -0.003(3) 0.079(8) -0.065(8) O2 0.105(6) 0.215(10) 0.114(6) -0.087(7) -0.037(5) 0.089(6) O3 0.095(4) 0.049(3) 0.045(3) -0.006(2) 0.015(3) 0.008(3) O4 0.090(5) 0.233(9) 0.090(5) -0.070(6) 0.058(4) -0.085(5) O5 0.186(7) 0.044(3) 0.068(4) -0.005(3) 0.058(4) -0.022(4) O6 0.096(4) 0.060(3) 0.055(3) -0.014(2) 0.041(3) -0.032(3) O7 0.079(4) 0.134(5) 0.063(4) -0.023(4) 0.045(3) -0.042(4) O8 0.134(6) 0.114(5) 0.065(4) -0.020(4) 0.022(4) 0.068(5) O9 0.057(3) 0.084(4) 0.051(3) -0.018(3) 0.025(3) 0.000(3) O10 0.219(13) 0.177(12) 0.311(19) -0.011(12) -0.046(12) -0.050(10) P1 0.1059(18) 0.0589(12) 0.0455(11) -0.0047(10) 0.0071(12) 0.0151(12) P2 0.0804(14) 0.0603(12) 0.0555(12) -0.0146(9) 0.0332(11) -0.0292(10) P3 0.0634(12) 0.0672(12) 0.0482(11) -0.0104(9) 0.0283(10) -0.0003(9) Yb1 0.03629(14) 0.03522(14) 0.03324(14) -0.00302(11) 0.01873(11) -0.00588(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.427(14) . ? C1 C5 1.436(14) . ? C1 Co1 2.068(8) . ? C1 H1A 0.9800 . ? C2 C3 1.360(13) . ? C2 Co1 2.071(8) . ? C2 H2A 0.9800 . ? C3 C4 1.381(11) . ? C3 Co1 2.098(8) . ? C3 H3A 0.9800 . ? C4 C5 1.389(12) . ? C4 Co1 2.094(7) . ? C4 H4A 0.9800 . ? C5 Co1 2.078(7) . ? C5 H5A 0.9800 . ? C6 O1 1.295(13) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O2 1.320(12) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O4 1.409(12) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O5 1.386(10) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 O7 1.398(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O8 1.397(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.384(9) . ? C12 C13 1.396(10) . ? C12 H12A 0.9300 . ? C13 C14 1.354(12) . ? C13 H13A 0.9300 . ? C14 C15 1.361(12) . ? C14 H14A 0.9300 . ? C15 C16 1.380(9) . ? C15 H15A 0.9300 . ? C16 C17 1.389(9) . ? C16 H16A 0.9300 . ? C17 C18 1.483(8) . ? C18 C55 1.408(8) . ? C18 C19 1.409(7) . ? C19 C20 1.409(8) . ? C19 N1 1.417(8) . ? C20 C21 1.405(8) . ? C20 Yb1 2.601(6) . ? C20 H20 0.88(6) . ? C21 C23 1.416(8) . ? C21 C22 1.430(8) . ? C22 N1 1.320(8) . ? C22 H22A 0.9300 . ? C23 C30 1.389(9) . ? C23 C24 1.491(8) . ? C24 C25 1.383(9) . ? C24 C29 1.388(9) . ? C25 C26 1.396(11) . ? C25 H25A 0.9300 . ? C26 C27 1.370(12) . ? C26 H26A 0.9300 . ? C27 C28 1.364(12) . ? C27 H27A 0.9300 . ? C28 C29 1.378(9) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 N2 1.382(8) . ? C30 C31 1.450(8) . ? C31 C32 1.346(10) . ? C31 H31A 0.9300 . ? C32 C33 1.443(8) . ? C32 H32A 0.9300 . ? C33 N2 1.374(7) . ? C33 C34 1.403(9) . ? C34 C41 1.400(8) . ? C34 C35 1.517(8) . ? C35 C40 1.333(11) . ? C35 C36 1.333(11) . ? C36 C37 1.412(14) . ? C36 H36A 0.9300 . ? C37 C38 1.288(16) . ? C37 H37A 0.9300 . ? C38 C39 1.291(15) . ? C38 H38A 0.9300 . ? C39 C40 1.405(12) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 N3 1.378(7) . ? C41 C42 1.432(8) . ? C42 C43 1.332(8) . ? C42 H42A 0.9300 . ? C43 C44 1.440(8) . ? C43 H43A 0.9300 . ? C44 N3 1.386(7) . ? C44 C45 1.409(8) . ? C45 C52 1.420(8) . ? C45 C46 1.506(8) . ? C46 C51 1.377(9) . ? C46 C47 1.391(9) . ? C47 C48 1.399(10) . ? C47 H47A 0.9300 . ? C48 C49 1.372(12) . ? C48 H48A 0.9300 . ? C49 C50 1.361(12) . ? C49 H49A 0.9300 . ? C50 C51 1.375(10) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 N4 1.359(7) . ? C52 C53 1.450(7) . ? C53 C54 1.336(8) . ? C53 H53A 0.9300 . ? C54 C55 1.436(8) . ? C54 H54A 0.9300 . ? C55 N4 1.387(7) . ? Co1 P1 2.160(2) . ? Co1 P2 2.167(2) . ? Co1 P3 2.173(2) . ? N2 Yb1 2.395(5) . ? N3 Yb1 2.314(5) . ? N4 Yb1 2.393(4) . ? O1 P1 1.563(9) . ? O2 P1 1.658(9) . ? O3 P1 1.503(5) . ? O3 Yb1 2.223(5) . ? O4 P2 1.586(7) . ? O5 P2 1.637(6) . ? O6 P2 1.507(5) . ? O6 Yb1 2.250(4) . ? O7 P3 1.615(6) . ? O8 P3 1.592(6) . ? O9 P3 1.496(5) . ? O9 Yb1 2.245(5) . ? P1 Yb1 3.484(2) . ? P2 Yb1 3.5036(19) . ? P3 Yb1 3.4986(18) . ? Yb1 H20 2.57(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 106.0(8) . . ? C2 C1 Co1 70.0(5) . . ? C5 C1 Co1 70.1(5) . . ? C2 C1 H1A 127.0 . . ? C5 C1 H1A 127.0 . . ? Co1 C1 H1A 127.0 . . ? C3 C2 C1 108.7(9) . . ? C3 C2 Co1 72.0(5) . . ? C1 C2 Co1 69.7(5) . . ? C3 C2 H2A 125.7 . . ? C1 C2 H2A 125.7 . . ? Co1 C2 H2A 125.7 . . ? C2 C3 C4 109.1(9) . . ? C2 C3 Co1 69.9(5) . . ? C4 C3 Co1 70.6(5) . . ? C2 C3 H3A 125.4 . . ? C4 C3 H3A 125.4 . . ? Co1 C3 H3A 125.4 . . ? C3 C4 C5 109.3(8) . . ? C3 C4 Co1 71.0(5) . . ? C5 C4 Co1 69.9(4) . . ? C3 C4 H4A 125.3 . . ? C5 C4 H4A 125.3 . . ? Co1 C4 H4A 125.3 . . ? C4 C5 C1 106.9(9) . . ? C4 C5 Co1 71.2(4) . . ? C1 C5 Co1 69.4(5) . . ? C4 C5 H5A 126.5 . . ? C1 C5 H5A 126.5 . . ? Co1 C5 H5A 126.5 . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O7 C10 H10A 109.5 . . ? O7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O8 C11 H11A 109.5 . . ? O8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 120.6(7) . . ? C17 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C14 C13 C12 120.3(8) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 120.3(7) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C15 C16 120.0(7) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C15 C16 C17 121.4(7) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C12 C17 C16 117.4(6) . . ? C12 C17 C18 121.5(6) . . ? C16 C17 C18 121.0(6) . . ? C55 C18 C19 122.4(5) . . ? C55 C18 C17 119.1(5) . . ? C19 C18 C17 118.5(5) . . ? C20 C19 C18 129.1(6) . . ? C20 C19 N1 108.3(5) . . ? C18 C19 N1 122.3(5) . . ? C21 C20 C19 107.5(6) . . ? C21 C20 Yb1 107.4(4) . . ? C19 C20 Yb1 106.3(4) . . ? C21 C20 H20 123(4) . . ? C19 C20 H20 126(4) . . ? Yb1 C20 H20 78(4) . . ? C20 C21 C23 129.6(6) . . ? C20 C21 C22 105.2(5) . . ? C23 C21 C22 124.9(5) . . ? N1 C22 C21 111.7(5) . . ? N1 C22 H22A 124.1 . . ? C21 C22 H22A 124.1 . . ? C30 C23 C21 122.1(5) . . ? C30 C23 C24 119.4(5) . . ? C21 C23 C24 118.6(6) . . ? C25 C24 C29 117.9(6) . . ? C25 C24 C23 122.4(6) . . ? C29 C24 C23 119.7(6) . . ? C24 C25 C26 120.3(8) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 120.4(8) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C28 C27 C26 119.9(7) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 120.1(8) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C28 C29 C24 121.4(7) . . ? C28 C29 H29A 119.3 . . ? C24 C29 H29A 119.3 . . ? N2 C30 C23 125.5(5) . . ? N2 C30 C31 108.5(5) . . ? C23 C30 C31 126.0(6) . . ? C32 C31 C30 107.6(6) . . ? C32 C31 H31A 126.2 . . ? C30 C31 H31A 126.2 . . ? C31 C32 C33 107.6(6) . . ? C31 C32 H32A 126.2 . . ? C33 C32 H32A 126.2 . . ? N2 C33 C34 126.5(5) . . ? N2 C33 C32 109.1(5) . . ? C34 C33 C32 124.4(6) . . ? C41 C34 C33 126.1(5) . . ? C41 C34 C35 116.7(5) . . ? C33 C34 C35 117.1(5) . . ? C40 C35 C36 116.5(7) . . ? C40 C35 C34 121.7(7) . . ? C36 C35 C34 121.8(7) . . ? C35 C36 C37 120.3(10) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C38 C37 C36 121.2(10) . . ? C38 C37 H37A 119.4 . . ? C36 C37 H37A 119.4 . . ? C37 C38 C39 120.0(10) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C38 C39 C40 120.0(10) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? C35 C40 C39 121.8(10) . . ? C35 C40 H40A 119.1 . . ? C39 C40 H40A 119.1 . . ? N3 C41 C34 125.0(5) . . ? N3 C41 C42 108.9(5) . . ? C34 C41 C42 125.9(5) . . ? C43 C42 C41 108.1(5) . . ? C43 C42 H42A 125.9 . . ? C41 C42 H42A 125.9 . . ? C42 C43 C44 107.8(5) . . ? C42 C43 H43A 126.1 . . ? C44 C43 H43A 126.1 . . ? N3 C44 C45 125.8(5) . . ? N3 C44 C43 108.5(5) . . ? C45 C44 C43 125.7(5) . . ? C44 C45 C52 125.3(5) . . ? C44 C45 C46 116.6(5) . . ? C52 C45 C46 118.1(5) . . ? C51 C46 C47 118.2(6) . . ? C51 C46 C45 121.7(6) . . ? C47 C46 C45 120.0(6) . . ? C46 C47 C48 120.1(7) . . ? C46 C47 H47A 119.9 . . ? C48 C47 H47A 119.9 . . ? C49 C48 C47 119.9(8) . . ? C49 C48 H48A 120.1 . . ? C47 C48 H48A 120.1 . . ? C50 C49 C48 119.9(7) . . ? C50 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C49 C50 C51 120.6(8) . . ? C49 C50 H50A 119.7 . . ? C51 C50 H50A 119.7 . . ? C50 C51 C46 121.2(7) . . ? C50 C51 H51A 119.4 . . ? C46 C51 H51A 119.4 . . ? N4 C52 C45 126.3(5) . . ? N4 C52 C53 109.2(5) . . ? C45 C52 C53 124.5(5) . . ? C54 C53 C52 107.3(5) . . ? C54 C53 H53A 126.4 . . ? C52 C53 H53A 126.4 . . ? C53 C54 C55 107.8(5) . . ? C53 C54 H54A 126.1 . . ? C55 C54 H54A 126.1 . . ? N4 C55 C18 125.0(5) . . ? N4 C55 C54 108.7(5) . . ? C18 C55 C54 126.3(5) . . ? C1 Co1 C2 40.3(4) . . ? C1 Co1 C5 40.5(4) . . ? C2 Co1 C5 66.9(4) . . ? C1 Co1 C4 66.1(3) . . ? C2 Co1 C4 64.8(3) . . ? C5 Co1 C4 38.9(3) . . ? C1 Co1 C3 65.8(4) . . ? C2 Co1 C3 38.1(4) . . ? C5 Co1 C3 65.5(4) . . ? C4 Co1 C3 38.5(3) . . ? C1 Co1 P1 91.3(3) . . ? C2 Co1 P1 101.1(3) . . ? C5 Co1 P1 120.0(3) . . ? C4 Co1 P1 157.0(3) . . ? C3 Co1 P1 136.8(3) . . ? C1 Co1 P2 124.6(4) . . ? C2 Co1 P2 160.4(3) . . ? C5 Co1 P2 93.6(3) . . ? C4 Co1 P2 98.8(2) . . ? C3 Co1 P2 132.7(3) . . ? P1 Co1 P2 90.52(10) . . ? C1 Co1 P3 145.2(4) . . ? C2 Co1 P3 105.2(4) . . ? C5 Co1 P3 147.5(3) . . ? C4 Co1 P3 108.7(3) . . ? C3 Co1 P3 88.7(3) . . ? P1 Co1 P3 92.20(9) . . ? P2 Co1 P3 89.93(8) . . ? C22 N1 C19 107.2(5) . . ? C33 N2 C30 107.3(5) . . ? C33 N2 Yb1 122.3(4) . . ? C30 N2 Yb1 127.1(4) . . ? C41 N3 C44 106.6(5) . . ? C41 N3 Yb1 122.0(4) . . ? C44 N3 Yb1 121.9(3) . . ? C52 N4 C55 107.0(4) . . ? C52 N4 Yb1 122.9(3) . . ? C55 N4 Yb1 125.0(4) . . ? C6 O1 P1 131.8(7) . . ? C7 O2 P1 124.3(8) . . ? P1 O3 Yb1 137.7(3) . . ? C8 O4 P2 125.2(7) . . ? C9 O5 P2 122.1(6) . . ? P2 O6 Yb1 136.8(3) . . ? C10 O7 P3 119.9(6) . . ? C11 O8 P3 125.3(6) . . ? P3 O9 Yb1 137.6(3) . . ? O3 P1 O1 108.2(4) . . ? O3 P1 O2 109.1(4) . . ? O1 P1 O2 105.6(7) . . ? O3 P1 Co1 119.5(2) . . ? O1 P1 Co1 109.1(4) . . ? O2 P1 Co1 104.5(3) . . ? O3 P1 Yb1 25.43(19) . . ? O1 P1 Yb1 124.7(4) . . ? O2 P1 Yb1 116.1(4) . . ? Co1 P1 Yb1 94.39(7) . . ? O6 P2 O4 107.6(3) . . ? O6 P2 O5 108.8(3) . . ? O4 P2 O5 104.6(4) . . ? O6 P2 Co1 119.8(2) . . ? O4 P2 Co1 110.2(3) . . ? O5 P2 Co1 104.8(2) . . ? O6 P2 Yb1 26.10(18) . . ? O4 P2 Yb1 121.4(3) . . ? O5 P2 Yb1 120.1(3) . . ? Co1 P2 Yb1 93.74(6) . . ? O9 P3 O8 107.9(3) . . ? O9 P3 O7 108.6(3) . . ? O8 P3 O7 101.7(4) . . ? O9 P3 Co1 119.2(2) . . ? O8 P3 Co1 111.0(3) . . ? O7 P3 Co1 107.0(2) . . ? O9 P3 Yb1 25.61(19) . . ? O8 P3 Yb1 124.3(3) . . ? O7 P3 Yb1 118.0(2) . . ? Co1 P3 Yb1 93.76(6) . . ? O3 Yb1 O9 79.90(19) . . ? O3 Yb1 O6 80.71(19) . . ? O9 Yb1 O6 77.50(19) . . ? O3 Yb1 N3 166.99(17) . . ? O9 Yb1 N3 90.70(18) . . ? O6 Yb1 N3 88.52(18) . . ? O3 Yb1 N4 108.90(18) . . ? O9 Yb1 N4 76.18(16) . . ? O6 Yb1 N4 149.71(18) . . ? N3 Yb1 N4 77.12(15) . . ? O3 Yb1 N2 107.99(19) . . ? O9 Yb1 N2 154.38(17) . . ? O6 Yb1 N2 79.79(17) . . ? N3 Yb1 N2 76.95(16) . . ? N4 Yb1 N2 121.42(16) . . ? O3 Yb1 C20 79.00(19) . . ? O9 Yb1 C20 133.23(19) . . ? O6 Yb1 C20 138.10(19) . . ? N3 Yb1 C20 114.00(19) . . ? N4 Yb1 C20 72.06(17) . . ? N2 Yb1 C20 72.32(17) . . ? O3 Yb1 P1 16.87(12) . . ? O9 Yb1 P1 68.33(13) . . ? O6 Yb1 P1 66.87(13) . . ? N3 Yb1 P1 150.12(13) . . ? N4 Yb1 P1 115.67(12) . . ? N2 Yb1 P1 112.85(13) . . ? C20 Yb1 P1 95.84(15) . . ? O3 Yb1 P3 66.54(13) . . ? O9 Yb1 P3 16.74(13) . . ? O6 Yb1 P3 66.46(13) . . ? N3 Yb1 P3 102.49(12) . . ? N4 Yb1 P3 90.51(11) . . ? N2 Yb1 P3 146.23(12) . . ? C20 Yb1 P3 133.82(14) . . ? P1 Yb1 P3 53.12(5) . . ? O3 Yb1 P2 67.60(13) . . ? O9 Yb1 P2 65.32(13) . . ? O6 Yb1 P2 17.13(13) . . ? N3 Yb1 P2 100.36(12) . . ? N4 Yb1 P2 141.43(11) . . ? N2 Yb1 P2 94.54(12) . . ? C20 Yb1 P2 138.36(15) . . ? P1 Yb1 P2 52.18(5) . . ? P3 Yb1 P2 51.95(5) . . ? O3 Yb1 H20 98.6(14) . . ? O9 Yb1 H20 138.9(13) . . ? O6 Yb1 H20 143.3(12) . . ? N3 Yb1 H20 94.4(14) . . ? N4 Yb1 H20 65.4(12) . . ? N2 Yb1 H20 65.4(13) . . ? C20 Yb1 H20 19.6(13) . . ? P1 Yb1 H20 115.4(14) . . ? P3 Yb1 H20 146.7(13) . . ? P2 Yb1 H20 151.7(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.891 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.101 data_wy1098wm _database_code_depnum_ccdc_archive 'CCDC 253411' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H53 Co Er N4 O10 P3' _chemical_formula_weight 1249.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.7562(9) _cell_length_b 28.5604(19) _cell_length_c 15.0423(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.5140(10) _cell_angle_gamma 90.00 _cell_volume 5333.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2524 _exptl_absorpt_coefficient_mu 2.026 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8495 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'Smart CCD' _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 26205 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9350 _reflns_number_gt 7307 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction SAINT _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^)+(0.0755P)^2^+15.8486P] 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 9350 _refine_ls_number_parameters 677 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1192(11) 0.1562(4) -0.0903(6) 0.106(5) Uani 1 1 d . . . H1A H 0.0596 0.1341 -0.1215 0.127 Uiso 1 1 calc R . . C2 C 0.2247(11) 0.1515(4) -0.0837(6) 0.080(3) Uani 1 1 d . . . H2A H 0.2520 0.1256 -0.1091 0.096 Uiso 1 1 calc R . . C3 C 0.2791(9) 0.1912(4) -0.0391(6) 0.081(3) Uani 1 1 d . . . H3A H 0.3543 0.1979 -0.0250 0.098 Uiso 1 1 calc R . . C4 C 0.2130(8) 0.2204(3) -0.0159(6) 0.069(2) Uani 1 1 d . . . H4A H 0.2341 0.2509 0.0167 0.082 Uiso 1 1 calc R . . C5 C 0.1147(8) 0.2005(4) -0.0457(7) 0.076(3) Uani 1 1 d . . . H5A H 0.0519 0.2140 -0.0406 0.092 Uiso 1 1 calc R . . C6 C 0.2625(10) 0.0151(4) 0.0183(8) 0.099(3) Uani 1 1 d . . . H6A H 0.3303 0.0246 0.0202 0.148 Uiso 1 1 calc R . . H6B H 0.2294 -0.0076 -0.0330 0.148 Uiso 1 1 calc R . . H6C H 0.2740 0.0016 0.0805 0.148 Uiso 1 1 calc R . . C7 C -0.0052(11) 0.0570(5) 0.0609(11) 0.129(5) Uani 1 1 d . . . H7A H 0.0159 0.0266 0.0479 0.194 Uiso 1 1 calc R . . H7B H -0.0809 0.0613 0.0213 0.194 Uiso 1 1 calc R . . H7C H 0.0100 0.0592 0.1293 0.194 Uiso 1 1 calc R . . C8 C 0.0167(11) 0.1746(5) 0.1977(11) 0.127(5) Uani 1 1 d . . . H8A H 0.0505 0.1474 0.2359 0.191 Uiso 1 1 calc R . . H8B H -0.0566 0.1675 0.1537 0.191 Uiso 1 1 calc R . . H8C H 0.0180 0.1996 0.2409 0.191 Uiso 1 1 calc R . . C9 C 0.2617(11) 0.2564(4) 0.2877(7) 0.098(4) Uani 1 1 d . . . H9A H 0.1958 0.2721 0.2767 0.147 Uiso 1 1 calc R . . H9B H 0.3189 0.2789 0.3056 0.147 Uiso 1 1 calc R . . H9C H 0.2788 0.2340 0.3400 0.147 Uiso 1 1 calc R . . C10 C 0.5516(9) 0.0946(4) 0.1485(8) 0.087(3) Uani 1 1 d . . . H10A H 0.6052 0.1188 0.1698 0.131 Uiso 1 1 calc R . . H10B H 0.5658 0.0732 0.1063 0.131 Uiso 1 1 calc R . . H10C H 0.5538 0.0781 0.2049 0.131 Uiso 1 1 calc R . . C11 C 0.5126(8) 0.2152(3) 0.2663(7) 0.080(3) Uani 1 1 d . . . H11A H 0.4585 0.2259 0.2858 0.120 Uiso 1 1 calc R . . H11B H 0.5528 0.2415 0.2603 0.120 Uiso 1 1 calc R . . H11C H 0.5604 0.1939 0.3150 0.120 Uiso 1 1 calc R . . C12 C 0.4415(7) -0.1103(3) 0.2480(6) 0.059(2) Uani 1 1 d . . . H12A H 0.4127 -0.1198 0.2907 0.070 Uiso 1 1 calc R . . C13 C 0.4595(8) -0.1432(3) 0.1869(8) 0.079(3) Uani 1 1 d . . . H13A H 0.4454 -0.1747 0.1917 0.094 Uiso 1 1 calc R . . C14 C 0.4973(8) -0.1294(4) 0.1209(8) 0.084(3) Uani 1 1 d . . . H14A H 0.5053 -0.1513 0.0787 0.100 Uiso 1 1 calc R . . C15 C 0.5235(6) -0.0835(4) 0.1164(6) 0.069(3) Uani 1 1 d . . . H15A H 0.5517 -0.0743 0.0729 0.082 Uiso 1 1 calc R . . C16 C 0.5076(6) -0.0504(3) 0.1778(5) 0.0515(18) Uani 1 1 d . . . H16A H 0.5245 -0.0191 0.1741 0.062 Uiso 1 1 calc R . . C17 C 0.4671(5) -0.0637(2) 0.2439(5) 0.0406(15) Uani 1 1 d . . . C18 C 0.4457(5) -0.0281(2) 0.3045(4) 0.0343(13) Uani 1 1 d . . . C19 C 0.3415(5) -0.0267(2) 0.3019(4) 0.0353(13) Uani 1 1 d . . . C20 C 0.3053(5) -0.0001(2) 0.3612(5) 0.0372(14) Uani 1 1 d . . . C21 C 0.1929(5) -0.0064(2) 0.3223(5) 0.0386(14) Uani 1 1 d . . . C22 C 0.1659(5) -0.0378(2) 0.2408(5) 0.0423(15) Uani 1 1 d . . . H22A H 0.0966 -0.0486 0.2021 0.051 Uiso 1 1 calc R . . C23 C 0.1165(5) 0.0160(2) 0.3482(5) 0.0422(15) Uani 1 1 d . . . C24 C 0.0082(5) -0.0058(3) 0.3158(5) 0.0460(16) Uani 1 1 d . . . C25 C -0.0855(6) 0.0206(3) 0.2748(6) 0.063(2) Uani 1 1 d . . . H25A H -0.0824 0.0526 0.2655 0.075 Uiso 1 1 calc R . . C26 C -0.1851(7) -0.0019(4) 0.2476(7) 0.082(3) Uani 1 1 d . . . H26A H -0.2481 0.0156 0.2191 0.098 Uiso 1 1 calc R . . C27 C -0.1917(7) -0.0484(4) 0.2617(7) 0.074(3) Uani 1 1 d . . . H27A H -0.2584 -0.0622 0.2450 0.088 Uiso 1 1 calc R . . C28 C -0.1000(7) -0.0749(3) 0.3005(6) 0.066(2) Uani 1 1 d . . . H28A H -0.1041 -0.1070 0.3086 0.079 Uiso 1 1 calc R . . C29 C -0.0002(6) -0.0533(3) 0.3279(5) 0.0534(18) Uani 1 1 d . . . H29A H 0.0621 -0.0714 0.3548 0.064 Uiso 1 1 calc R . . C30 C 0.1395(5) 0.0570(2) 0.4025(5) 0.0425(15) Uani 1 1 d . . . C31 C 0.0763(6) 0.0781(3) 0.4479(6) 0.057(2) Uani 1 1 d . . . H31A H 0.0129 0.0663 0.4469 0.069 Uiso 1 1 calc R . . C32 C 0.1259(6) 0.1176(3) 0.4916(6) 0.0564(19) Uani 1 1 d . . . H32A H 0.1025 0.1383 0.5259 0.068 Uiso 1 1 calc R . . C33 C 0.2218(5) 0.1226(2) 0.4762(5) 0.0413(15) Uani 1 1 d . . . C34 C 0.2961(5) 0.1590(2) 0.5138(5) 0.0410(15) Uani 1 1 d . . . C35 C 0.2664(6) 0.1991(2) 0.5645(5) 0.0482(17) Uani 1 1 d . . . C36 C 0.2180(13) 0.2375(4) 0.5181(8) 0.146(7) Uani 1 1 d . . . H36A H 0.2005 0.2405 0.4513 0.175 Uiso 1 1 calc R . . C37 C 0.1922(16) 0.2737(5) 0.5657(11) 0.170(8) Uani 1 1 d . . . H37A H 0.1583 0.3004 0.5306 0.204 Uiso 1 1 calc R . . C38 C 0.2152(11) 0.2707(4) 0.6594(9) 0.099(4) Uani 1 1 d . . . H38A H 0.2000 0.2955 0.6913 0.119 Uiso 1 1 calc R . . C39 C 0.2598(11) 0.2326(4) 0.7078(8) 0.107(4) Uani 1 1 d . . . H39A H 0.2728 0.2294 0.7735 0.128 Uiso 1 1 calc R . . C40 C 0.2877(10) 0.1966(4) 0.6607(7) 0.095(4) Uani 1 1 d . . . H40A H 0.3221 0.1702 0.6966 0.115 Uiso 1 1 calc R . . C41 C 0.3979(5) 0.1613(2) 0.5145(5) 0.0405(15) Uani 1 1 d . . . C42 C 0.4764(6) 0.1973(2) 0.5581(5) 0.0473(16) Uani 1 1 d . . . H42A H 0.4671 0.2245 0.5877 0.057 Uiso 1 1 calc R . . C43 C 0.5649(6) 0.1852(2) 0.5491(5) 0.0463(16) Uani 1 1 d . . . H43A H 0.6282 0.2026 0.5705 0.056 Uiso 1 1 calc R . . C44 C 0.5459(5) 0.1406(2) 0.5005(4) 0.0380(14) Uani 1 1 d . . . C45 C 0.6215(5) 0.1143(2) 0.4802(4) 0.0365(14) Uani 1 1 d . . . C46 C 0.7300(5) 0.1364(2) 0.5116(5) 0.0414(15) Uani 1 1 d . . . C47 C 0.7684(6) 0.1479(3) 0.4424(6) 0.0551(18) Uani 1 1 d . . . H47A H 0.7269 0.1407 0.3764 0.066 Uiso 1 1 calc R . . C48 C 0.8667(7) 0.1698(3) 0.4695(8) 0.071(2) Uani 1 1 d . . . H48A H 0.8917 0.1769 0.4226 0.085 Uiso 1 1 calc R . . C49 C 0.9269(7) 0.1811(3) 0.5666(8) 0.075(3) Uani 1 1 d . . . H49A H 0.9922 0.1965 0.5851 0.090 Uiso 1 1 calc R . . C50 C 0.8927(7) 0.1701(3) 0.6358(7) 0.067(2) Uani 1 1 d . . . H50A H 0.9340 0.1782 0.7013 0.080 Uiso 1 1 calc R . . C51 C 0.7958(6) 0.1468(3) 0.6085(5) 0.0540(18) Uani 1 1 d . . . H51A H 0.7745 0.1380 0.6570 0.065 Uiso 1 1 calc R . . C52 C 0.6037(5) 0.0699(2) 0.4352(4) 0.0341(13) Uani 1 1 d . . . C53 C 0.6852(5) 0.0415(2) 0.4270(4) 0.0387(14) Uani 1 1 d . . . H53A H 0.7579 0.0490 0.4510 0.046 Uiso 1 1 calc R . . C54 C 0.6381(5) 0.0021(2) 0.3784(4) 0.0389(14) Uani 1 1 d . . . H54A H 0.6717 -0.0223 0.3619 0.047 Uiso 1 1 calc R . . C55 C 0.5253(5) 0.0050(2) 0.3570(4) 0.0354(13) Uani 1 1 d . . . Co1 Co 0.22911(8) 0.15650(3) 0.05555(6) 0.0460(2) Uani 1 1 d . . . Er1 Er 0.33681(2) 0.087012(9) 0.331749(19) 0.03334(11) Uani 1 1 d . . . N1 N 0.2508(5) -0.0495(2) 0.2276(4) 0.0489(14) Uani 1 1 d . . . N2 N 0.2283(4) 0.08549(18) 0.4218(4) 0.0383(12) Uani 1 1 d . . . N3 N 0.4412(4) 0.12731(18) 0.4769(4) 0.0391(12) Uani 1 1 d . . . N4 N 0.5072(4) 0.04726(17) 0.3935(4) 0.0352(11) Uani 1 1 d . . . O1 O 0.1990(14) 0.0519(3) 0.0007(5) 0.226(8) Uani 1 1 d . . . O2 O 0.0497(6) 0.0899(3) 0.0389(6) 0.128(4) Uani 1 1 d . . . O3 O 0.2341(5) 0.0639(2) 0.1756(4) 0.0728(16) Uani 1 1 d . . . O4 O 0.0726(6) 0.1885(3) 0.1428(6) 0.123(3) Uani 1 1 d . . . O5 O 0.2495(6) 0.2332(2) 0.2017(4) 0.084(2) Uani 1 1 d . . . O6 O 0.2410(5) 0.1538(2) 0.2723(4) 0.0763(18) Uani 1 1 d . . . O7 O 0.4485(5) 0.1148(2) 0.0964(4) 0.0794(18) Uani 1 1 d . . . O8 O 0.4636(6) 0.1924(3) 0.1762(5) 0.102(3) Uani 1 1 d . . . O9 O 0.4253(4) 0.1223(2) 0.2530(4) 0.0669(15) Uani 1 1 d . . . O10 O 0.1653(13) 0.8642(5) 0.1089(13) 0.253(8) Uani 1 1 d . . . P1 P 0.1833(2) 0.08626(8) 0.07542(17) 0.0766(7) Uani 1 1 d . . . P2 P 0.1989(2) 0.18088(8) 0.17811(17) 0.0671(6) Uani 1 1 d . . . P3 P 0.39741(18) 0.14475(8) 0.15534(15) 0.0594(5) Uani 1 1 d . . . H20 H 0.340(4) 0.0122(19) 0.419(4) 0.020(14) 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 C1 0.134(11) 0.099(8) 0.033(4) 0.023(5) -0.012(5) -0.044(8) C2 0.120(9) 0.078(7) 0.038(4) 0.007(4) 0.031(5) 0.019(6) C3 0.107(8) 0.098(7) 0.047(5) 0.028(5) 0.041(5) 0.014(6) C4 0.092(7) 0.065(5) 0.052(5) 0.019(4) 0.034(5) 0.009(5) C5 0.080(7) 0.087(7) 0.061(5) 0.038(5) 0.029(5) 0.032(6) C6 0.123(10) 0.103(9) 0.085(7) -0.005(6) 0.059(7) 0.011(7) C7 0.100(9) 0.124(11) 0.150(12) 0.012(9) 0.042(9) -0.029(8) C8 0.105(9) 0.154(12) 0.160(13) 0.026(10) 0.092(10) 0.018(9) C9 0.150(11) 0.078(7) 0.080(7) -0.010(5) 0.063(7) 0.003(7) C10 0.089(7) 0.098(8) 0.073(6) 0.003(5) 0.033(6) 0.027(6) C11 0.084(7) 0.075(6) 0.080(6) -0.011(5) 0.035(5) -0.017(5) C12 0.069(5) 0.047(4) 0.075(5) -0.001(4) 0.045(4) 0.005(4) C13 0.091(7) 0.055(5) 0.115(8) -0.029(5) 0.067(6) -0.011(5) C14 0.071(6) 0.090(7) 0.107(8) -0.055(6) 0.054(6) -0.014(5) C15 0.050(5) 0.113(8) 0.056(5) -0.033(5) 0.035(4) -0.010(5) C16 0.046(4) 0.070(5) 0.048(4) -0.013(4) 0.028(3) -0.008(4) C17 0.038(3) 0.050(4) 0.041(3) -0.004(3) 0.024(3) 0.004(3) C18 0.040(3) 0.036(3) 0.032(3) 0.007(3) 0.021(3) 0.011(3) C19 0.038(3) 0.035(3) 0.038(3) 0.004(3) 0.022(3) 0.005(3) C20 0.039(3) 0.040(3) 0.042(4) -0.002(3) 0.026(3) 0.001(3) C21 0.040(3) 0.043(3) 0.043(3) 0.005(3) 0.027(3) 0.003(3) C22 0.037(3) 0.046(4) 0.049(4) -0.004(3) 0.022(3) -0.003(3) C23 0.034(3) 0.053(4) 0.047(4) 0.004(3) 0.025(3) 0.001(3) C24 0.034(3) 0.069(5) 0.044(4) -0.002(3) 0.025(3) 0.002(3) C25 0.044(4) 0.078(5) 0.069(5) -0.003(4) 0.028(4) 0.010(4) C26 0.038(5) 0.122(9) 0.080(6) -0.017(6) 0.021(4) 0.018(5) C27 0.047(5) 0.110(8) 0.072(6) -0.031(6) 0.033(4) -0.023(5) C28 0.058(5) 0.083(6) 0.070(5) -0.012(4) 0.039(5) -0.019(4) C29 0.049(4) 0.063(5) 0.057(4) 0.000(4) 0.031(4) -0.002(4) C30 0.034(3) 0.055(4) 0.047(4) 0.004(3) 0.026(3) 0.012(3) C31 0.046(4) 0.080(6) 0.064(5) -0.010(4) 0.041(4) -0.004(4) C32 0.054(4) 0.065(5) 0.066(5) -0.013(4) 0.040(4) 0.007(4) C33 0.044(4) 0.046(4) 0.047(4) 0.002(3) 0.032(3) 0.009(3) C34 0.048(4) 0.046(4) 0.037(3) 0.006(3) 0.026(3) 0.016(3) C35 0.054(4) 0.047(4) 0.059(4) -0.008(3) 0.039(4) 0.007(3) C36 0.256(18) 0.127(10) 0.087(7) 0.050(7) 0.106(10) 0.133(12) C37 0.29(2) 0.124(11) 0.125(11) 0.050(9) 0.119(13) 0.147(14) C38 0.141(10) 0.075(7) 0.120(9) -0.019(7) 0.094(9) 0.016(7) C39 0.142(11) 0.110(9) 0.083(7) -0.031(7) 0.063(8) 0.022(8) C40 0.146(10) 0.090(7) 0.062(6) -0.002(5) 0.056(6) 0.042(7) C41 0.046(4) 0.042(4) 0.037(3) -0.005(3) 0.022(3) 0.010(3) C42 0.057(4) 0.041(4) 0.054(4) -0.010(3) 0.033(4) 0.001(3) C43 0.051(4) 0.038(3) 0.058(4) -0.005(3) 0.031(4) -0.005(3) C44 0.039(3) 0.043(3) 0.035(3) 0.003(3) 0.020(3) 0.001(3) C45 0.035(3) 0.045(4) 0.032(3) -0.002(3) 0.016(3) 0.000(3) C46 0.034(3) 0.042(3) 0.051(4) -0.002(3) 0.020(3) 0.003(3) C47 0.045(4) 0.070(5) 0.057(4) -0.006(4) 0.028(4) -0.005(4) C48 0.054(5) 0.074(6) 0.104(7) 0.002(5) 0.054(5) -0.007(4) C49 0.042(5) 0.063(5) 0.116(8) -0.021(5) 0.030(5) -0.008(4) C50 0.049(5) 0.060(5) 0.077(6) -0.014(4) 0.014(4) 0.001(4) C51 0.044(4) 0.054(4) 0.053(4) -0.007(3) 0.011(3) 0.005(3) C52 0.035(3) 0.042(3) 0.030(3) 0.003(3) 0.018(3) 0.003(3) C53 0.027(3) 0.053(4) 0.036(3) -0.002(3) 0.014(3) 0.008(3) C54 0.035(3) 0.051(4) 0.036(3) -0.002(3) 0.020(3) 0.011(3) C55 0.040(3) 0.041(3) 0.032(3) 0.003(3) 0.022(3) 0.011(3) Co1 0.0587(6) 0.0453(5) 0.0343(5) 0.0077(4) 0.0202(4) 0.0100(4) Er1 0.03500(17) 0.03783(17) 0.03203(16) 0.00355(11) 0.01902(12) 0.00599(12) N1 0.053(4) 0.049(3) 0.054(3) -0.006(3) 0.032(3) -0.003(3) N2 0.034(3) 0.044(3) 0.045(3) 0.003(2) 0.025(2) 0.005(2) N3 0.038(3) 0.046(3) 0.041(3) -0.007(2) 0.024(2) 0.001(2) N4 0.035(3) 0.039(3) 0.038(3) 0.003(2) 0.023(2) 0.004(2) O1 0.51(2) 0.059(5) 0.045(4) 0.000(4) 0.061(8) 0.038(9) O2 0.074(5) 0.157(8) 0.103(6) 0.047(5) -0.009(4) -0.050(5) O3 0.092(5) 0.059(3) 0.053(3) 0.004(3) 0.018(3) -0.011(3) O4 0.097(5) 0.196(9) 0.102(5) 0.062(6) 0.067(5) 0.079(6) O5 0.140(6) 0.053(3) 0.062(3) 0.001(3) 0.046(4) 0.022(4) O6 0.112(5) 0.070(4) 0.061(3) 0.015(3) 0.051(4) 0.038(3) O7 0.072(4) 0.114(5) 0.063(4) 0.017(3) 0.040(3) 0.034(4) O8 0.112(6) 0.114(5) 0.065(4) 0.021(4) 0.024(4) -0.057(5) O9 0.057(3) 0.090(4) 0.058(3) 0.015(3) 0.029(3) -0.005(3) O10 0.212(14) 0.149(11) 0.260(16) 0.009(11) -0.028(12) 0.038(10) P1 0.0948(19) 0.0653(14) 0.0475(12) 0.0038(10) 0.0096(12) -0.0106(13) P2 0.0835(16) 0.0646(13) 0.0608(13) 0.0164(10) 0.0381(12) 0.0272(12) P3 0.0638(13) 0.0693(13) 0.0504(11) 0.0081(10) 0.0296(10) -0.0001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.418(16) . ? C1 C5 1.444(15) . ? C1 Co1 2.059(8) . ? C1 H1A 0.9800 . ? C2 C3 1.363(14) . ? C2 Co1 2.074(8) . ? C2 H2A 0.9800 . ? C3 C4 1.386(13) . ? C3 Co1 2.080(9) . ? C3 H3A 0.9800 . ? C4 C5 1.354(13) . ? C4 Co1 2.082(8) . ? C4 H4A 0.9800 . ? C5 Co1 2.075(8) . ? C5 H5A 0.9800 . ? C6 O1 1.318(15) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O2 1.334(13) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O4 1.406(13) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O5 1.399(10) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 O7 1.414(11) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O8 1.389(11) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C17 1.385(10) . ? C12 C13 1.409(11) . ? C12 H12A 0.9300 . ? C13 C14 1.362(13) . ? C13 H13A 0.9300 . ? C14 C15 1.371(13) . ? C14 H14A 0.9300 . ? C15 C16 1.403(10) . ? C15 H15A 0.9300 . ? C16 C17 1.386(9) . ? C16 H16A 0.9300 . ? C17 C18 1.477(8) . ? C18 C55 1.403(9) . ? C18 C19 1.418(8) . ? C19 C20 1.416(8) . ? C19 N1 1.424(8) . ? C20 C21 1.410(9) . ? C20 Er1 2.595(6) . ? C20 H20 0.87(6) . ? C21 C23 1.420(8) . ? C21 C22 1.433(9) . ? C22 N1 1.310(8) . ? C22 H22A 0.9300 . ? C23 C30 1.384(10) . ? C23 C24 1.489(9) . ? C24 C29 1.382(10) . ? C24 C25 1.387(10) . ? C25 C26 1.405(12) . ? C25 H25A 0.9300 . ? C26 C27 1.352(14) . ? C26 H26A 0.9300 . ? C27 C28 1.368(13) . ? C27 H27A 0.9300 . ? C28 C29 1.395(11) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 N2 1.391(8) . ? C30 C31 1.447(9) . ? C31 C32 1.336(11) . ? C31 H31A 0.9300 . ? C32 C33 1.442(9) . ? C32 H32A 0.9300 . ? C33 N2 1.365(8) . ? C33 C34 1.395(10) . ? C34 C41 1.398(9) . ? C34 C35 1.526(8) . ? C35 C36 1.317(12) . ? C35 C40 1.349(11) . ? C36 C37 1.387(15) . ? C36 H36A 0.9300 . ? C37 C38 1.308(16) . ? C37 H37A 0.9300 . ? C38 C39 1.306(15) . ? C38 H38A 0.9300 . ? C39 C40 1.392(13) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 N3 1.381(8) . ? C41 C42 1.430(10) . ? C42 C43 1.328(9) . ? C42 H42A 0.9300 . ? C43 C44 1.437(9) . ? C43 H43A 0.9300 . ? C44 N3 1.380(8) . ? C44 C45 1.417(8) . ? C45 C52 1.409(9) . ? C45 C46 1.497(9) . ? C46 C51 1.377(10) . ? C46 C47 1.396(9) . ? C47 C48 1.383(11) . ? C47 H47A 0.9300 . ? C48 C49 1.371(13) . ? C48 H48A 0.9300 . ? C49 C50 1.350(13) . ? C49 H49A 0.9300 . ? C50 C51 1.385(11) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 N4 1.363(8) . ? C52 C53 1.431(8) . ? C53 C54 1.346(9) . ? C53 H53A 0.9300 . ? C54 C55 1.444(8) . ? C54 H54A 0.9300 . ? C55 N4 1.391(7) . ? Co1 P1 2.162(3) . ? Co1 P2 2.172(2) . ? Co1 P3 2.175(2) . ? Er1 O3 2.256(6) . ? Er1 O9 2.267(5) . ? Er1 O6 2.271(5) . ? Er1 N3 2.336(5) . ? Er1 N4 2.402(5) . ? Er1 N2 2.410(5) . ? Er1 H20 2.50(5) . ? O1 P1 1.575(10) . ? O2 P1 1.679(9) . ? O3 P1 1.503(6) . ? O4 P2 1.598(8) . ? O5 P2 1.621(7) . ? O6 P2 1.495(6) . ? O7 P3 1.597(6) . ? O8 P3 1.590(7) . ? O9 P3 1.494(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.3(9) . . ? C2 C1 Co1 70.5(5) . . ? C5 C1 Co1 70.1(5) . . ? C2 C1 H1A 126.3 . . ? C5 C1 H1A 126.3 . . ? Co1 C1 H1A 126.3 . . ? C3 C2 C1 106.6(10) . . ? C3 C2 Co1 71.1(5) . . ? C1 C2 Co1 69.4(5) . . ? C3 C2 H2A 126.7 . . ? C1 C2 H2A 126.7 . . ? Co1 C2 H2A 126.7 . . ? C2 C3 C4 110.1(10) . . ? C2 C3 Co1 70.6(6) . . ? C4 C3 Co1 70.6(5) . . ? C2 C3 H3A 125.0 . . ? C4 C3 H3A 125.0 . . ? Co1 C3 H3A 125.0 . . ? C5 C4 C3 109.5(9) . . ? C5 C4 Co1 70.7(5) . . ? C3 C4 Co1 70.5(5) . . ? C5 C4 H4A 125.3 . . ? C3 C4 H4A 125.3 . . ? Co1 C4 H4A 125.3 . . ? C4 C5 C1 106.6(10) . . ? C4 C5 Co1 71.3(5) . . ? C1 C5 Co1 69.0(5) . . ? C4 C5 H5A 126.7 . . ? C1 C5 H5A 126.7 . . ? Co1 C5 H5A 126.7 . . ? O1 C6 H6A 109.5 . . ? O1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4 C8 H8A 109.5 . . ? O4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 C9 H9A 109.5 . . ? O5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O7 C10 H10A 109.5 . . ? O7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O8 C11 H11A 109.5 . . ? O8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 119.6(7) . . ? C17 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C14 C13 C12 120.8(8) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 120.3(8) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C15 C16 119.5(8) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C16 C15 120.9(8) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C12 C17 C16 118.9(6) . . ? C12 C17 C18 120.9(6) . . ? C16 C17 C18 120.2(6) . . ? C55 C18 C19 122.1(5) . . ? C55 C18 C17 119.7(5) . . ? C19 C18 C17 118.0(6) . . ? C20 C19 C18 128.5(6) . . ? C20 C19 N1 108.3(5) . . ? C18 C19 N1 122.9(5) . . ? C21 C20 C19 106.9(6) . . ? C21 C20 Er1 106.6(4) . . ? C19 C20 Er1 106.1(4) . . ? C21 C20 H20 120(4) . . ? C19 C20 H20 131(4) . . ? Er1 C20 H20 74(4) . . ? C20 C21 C23 129.7(6) . . ? C20 C21 C22 105.6(5) . . ? C23 C21 C22 124.5(6) . . ? N1 C22 C21 111.7(6) . . ? N1 C22 H22A 124.1 . . ? C21 C22 H22A 124.1 . . ? C30 C23 C21 122.3(6) . . ? C30 C23 C24 119.3(6) . . ? C21 C23 C24 118.5(6) . . ? C29 C24 C25 118.5(7) . . ? C29 C24 C23 119.7(6) . . ? C25 C24 C23 121.7(7) . . ? C24 C25 C26 119.0(9) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.5 . . ? C27 C26 C25 121.7(8) . . ? C27 C26 H26A 119.1 . . ? C25 C26 H26A 119.1 . . ? C26 C27 C28 119.9(8) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C29 119.3(9) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C24 C29 C28 121.5(8) . . ? C24 C29 H29A 119.2 . . ? C28 C29 H29A 119.2 . . ? C23 C30 N2 125.1(5) . . ? C23 C30 C31 126.8(6) . . ? N2 C30 C31 108.1(6) . . ? C32 C31 C30 107.5(6) . . ? C32 C31 H31A 126.3 . . ? C30 C31 H31A 126.3 . . ? C31 C32 C33 108.3(6) . . ? C31 C32 H32A 125.8 . . ? C33 C32 H32A 125.8 . . ? N2 C33 C34 126.6(5) . . ? N2 C33 C32 108.6(6) . . ? C34 C33 C32 124.8(6) . . ? C33 C34 C41 126.5(6) . . ? C33 C34 C35 117.0(6) . . ? C41 C34 C35 116.4(6) . . ? C36 C35 C40 116.0(8) . . ? C36 C35 C34 122.9(7) . . ? C40 C35 C34 121.0(7) . . ? C35 C36 C37 122.0(10) . . ? C35 C36 H36A 119.0 . . ? C37 C36 H36A 119.0 . . ? C38 C37 C36 120.7(11) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C39 C38 C37 119.6(10) . . ? C39 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? C38 C39 C40 119.8(10) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C35 C40 C39 121.8(10) . . ? C35 C40 H40A 119.1 . . ? C39 C40 H40A 119.1 . . ? N3 C41 C34 124.8(6) . . ? N3 C41 C42 108.7(5) . . ? C34 C41 C42 126.4(6) . . ? C43 C42 C41 108.0(6) . . ? C43 C42 H42A 126.0 . . ? C41 C42 H42A 126.0 . . ? C42 C43 C44 108.0(6) . . ? C42 C43 H43A 126.0 . . ? C44 C43 H43A 126.0 . . ? N3 C44 C45 125.5(6) . . ? N3 C44 C43 108.4(5) . . ? C45 C44 C43 126.1(6) . . ? C52 C45 C44 126.0(6) . . ? C52 C45 C46 118.2(5) . . ? C44 C45 C46 115.7(5) . . ? C51 C46 C47 116.9(7) . . ? C51 C46 C45 122.4(6) . . ? C47 C46 C45 120.7(6) . . ? C48 C47 C46 121.5(8) . . ? C48 C47 H47A 119.2 . . ? C46 C47 H47A 119.2 . . ? C49 C48 C47 119.0(8) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C50 C49 C48 121.1(8) . . ? C50 C49 H49A 119.4 . . ? C48 C49 H49A 119.4 . . ? C49 C50 C51 119.5(8) . . ? C49 C50 H50A 120.2 . . ? C51 C50 H50A 120.2 . . ? C46 C51 C50 121.8(8) . . ? C46 C51 H51A 119.1 . . ? C50 C51 H51A 119.1 . . ? N4 C52 C45 125.5(5) . . ? N4 C52 C53 109.6(5) . . ? C45 C52 C53 124.8(6) . . ? C54 C53 C52 107.9(5) . . ? C54 C53 H53A 126.0 . . ? C52 C53 H53A 126.0 . . ? C53 C54 C55 107.1(5) . . ? C53 C54 H54A 126.5 . . ? C55 C54 H54A 126.5 . . ? N4 C55 C18 125.2(5) . . ? N4 C55 C54 108.6(5) . . ? C18 C55 C54 126.1(5) . . ? C1 Co1 C2 40.1(5) . . ? C1 Co1 C5 40.9(4) . . ? C2 Co1 C5 67.5(4) . . ? C1 Co1 C3 65.2(4) . . ? C2 Co1 C3 38.3(4) . . ? C5 Co1 C3 65.1(4) . . ? C1 Co1 C4 65.6(4) . . ? C2 Co1 C4 65.7(4) . . ? C5 Co1 C4 38.0(4) . . ? C3 Co1 C4 38.9(4) . . ? C1 Co1 P1 91.1(3) . . ? C2 Co1 P1 101.1(3) . . ? C5 Co1 P1 119.3(3) . . ? C3 Co1 P1 137.6(3) . . ? C4 Co1 P1 155.9(3) . . ? C1 Co1 P2 125.7(5) . . ? C2 Co1 P2 161.1(3) . . ? C5 Co1 P2 93.8(3) . . ? C3 Co1 P2 132.0(3) . . ? C4 Co1 P2 98.1(3) . . ? P1 Co1 P2 90.36(10) . . ? C1 Co1 P3 144.0(5) . . ? C2 Co1 P3 104.2(4) . . ? C5 Co1 P3 147.7(3) . . ? C3 Co1 P3 88.8(3) . . ? C4 Co1 P3 109.7(3) . . ? P1 Co1 P3 92.79(10) . . ? P2 Co1 P3 89.98(9) . . ? O3 Er1 O9 79.8(2) . . ? O3 Er1 O6 80.7(2) . . ? O9 Er1 O6 76.9(2) . . ? O3 Er1 N3 167.10(19) . . ? O9 Er1 N3 91.00(19) . . ? O6 Er1 N3 88.5(2) . . ? O3 Er1 N4 109.5(2) . . ? O9 Er1 N4 75.98(18) . . ? O6 Er1 N4 148.6(2) . . ? N3 Er1 N4 76.52(17) . . ? O3 Er1 N2 108.6(2) . . ? O9 Er1 N2 154.65(19) . . ? O6 Er1 N2 80.89(19) . . ? N3 Er1 N2 76.33(18) . . ? N4 Er1 N2 120.78(17) . . ? O3 Er1 C20 79.7(2) . . ? O9 Er1 C20 133.0(2) . . ? O6 Er1 C20 139.5(2) . . ? N3 Er1 C20 113.2(2) . . ? N4 Er1 C20 71.81(18) . . ? N2 Er1 C20 72.38(18) . . ? O3 Er1 H20 99.2(14) . . ? O9 Er1 H20 139.7(12) . . ? O6 Er1 H20 143.2(12) . . ? N3 Er1 H20 93.7(14) . . ? N4 Er1 H20 66.4(12) . . ? N2 Er1 H20 64.1(12) . . ? C20 Er1 H20 19.5(13) . . ? C22 N1 C19 107.5(5) . . ? C33 N2 C30 107.5(5) . . ? C33 N2 Er1 122.6(4) . . ? C30 N2 Er1 126.5(4) . . ? C44 N3 C41 106.8(5) . . ? C44 N3 Er1 121.9(4) . . ? C41 N3 Er1 122.0(4) . . ? C52 N4 C55 106.7(5) . . ? C52 N4 Er1 123.3(4) . . ? C55 N4 Er1 124.6(4) . . ? C6 O1 P1 129.5(8) . . ? C7 O2 P1 122.1(9) . . ? P1 O3 Er1 137.1(3) . . ? C8 O4 P2 123.9(8) . . ? C9 O5 P2 120.5(6) . . ? P2 O6 Er1 136.9(3) . . ? C10 O7 P3 119.1(6) . . ? C11 O8 P3 126.1(6) . . ? P3 O9 Er1 137.4(3) . . ? O3 P1 O1 107.6(4) . . ? O3 P1 O2 109.0(4) . . ? O1 P1 O2 105.8(7) . . ? O3 P1 Co1 119.7(3) . . ? O1 P1 Co1 110.0(5) . . ? O2 P1 Co1 103.9(3) . . ? O6 P2 O4 107.9(4) . . ? O6 P2 O5 108.4(4) . . ? O4 P2 O5 104.5(5) . . ? O6 P2 Co1 120.0(2) . . ? O4 P2 Co1 109.8(3) . . ? O5 P2 Co1 105.0(2) . . ? O9 P3 O8 106.9(3) . . ? O9 P3 O7 109.1(3) . . ? O8 P3 O7 102.5(4) . . ? O9 P3 Co1 119.4(2) . . ? O8 P3 Co1 110.7(3) . . ? O7 P3 Co1 107.0(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.733 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.118