# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name D.Aguila L.A.Barrios O.Roubeau S.J.Teat G.Aromi _publ_contact_author_name 'Olivier Roubeau' _publ_contact_author_email roubeau@unizar.es data_da112 _database_code_depnum_ccdc_archive 'CCDC 791562' #TrackingRef 'DA112.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 Co4 N6 O16, 4(C H4 O), 4(N O3), 2(H2 O)' _chemical_formula_sum 'C48 H66 Co4 N10 O34' _chemical_formula_weight 1562.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Co Co 0.1760 1.1404 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _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 10.5822(7) _cell_length_b 12.3023(8) _cell_length_c 13.8898(10) _cell_angle_alpha 64.4450(10) _cell_angle_beta 89.4460(10) _cell_angle_gamma 72.1670(10) _cell_volume 1537.11(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9998 _cell_measurement_theta_min 3.34 _cell_measurement_theta_max 33.54 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 1.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'SADABS v2.10 Bruker AXS Madison WI US' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 24109 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 33.57 _reflns_number_total 9091 _reflns_number_gt 8030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.56a' _computing_data_reduction 'Bruker SAINT v7.56a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogens were refined anisotropically. Hydrogens were found in difference Fourier maps, placed geometrically on their carrier atom when possible and refined with a riding model. Hydrogens on the coordinated water molecules as well as those on the lattice water molecule (O1W) were refined freely with their thermal paramter 1.5 times that of their carrier oxygen and a soft 1,3 H-H distance restraint. ; _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^)+(0.0523P)^2^+1.0903P] 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 9091 _refine_ls_number_parameters 460 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.88937(2) 0.075971(18) 0.194677(18) 0.01777(6) Uani 1 1 d . . . Co2 Co 0.663270(18) 0.386287(17) 0.070322(16) 0.01402(6) Uani 1 1 d . . . O1 O 0.69596(11) 0.18747(10) 0.10570(9) 0.0190(2) Uani 1 1 d . . . O2 O 0.46616(10) 0.40334(10) 0.01276(9) 0.0166(2) Uani 1 1 d . . . O3 O 0.13687(11) 0.74284(10) -0.16668(9) 0.0186(2) Uani 1 1 d . . . O4 O -0.07781(11) 0.97948(11) -0.26925(10) 0.0216(2) Uani 1 1 d . . . O5 O 0.98211(12) 0.09285(12) 0.05782(11) 0.0236(2) Uani 1 1 d . . . H5A H 1.063(2) 0.042(2) 0.0701(18) 0.028 Uiso 1 1 d D . . H5B H 0.938(2) 0.102(2) 0.005(2) 0.028 Uiso 1 1 d D . . O6 O 0.81984(13) 0.03038(12) 0.34891(10) 0.0267(3) Uani 1 1 d . . . H6 H 0.8521 -0.0491 0.3870 0.032 Uiso 1 1 calc R . . O7 O 0.73139(12) 0.40631(11) -0.07734(10) 0.0194(2) Uani 1 1 d . . . H7B H 0.706(2) 0.475(2) -0.1234(18) 0.023 Uiso 1 1 d D . . H7C H 0.730(2) 0.352(2) -0.0990(18) 0.023 Uiso 1 1 d D . . O8 O 0.59819(12) 0.36064(12) 0.21768(10) 0.0214(2) Uani 1 1 d . . . H8A H 0.528(2) 0.363(2) 0.2201(19) 0.026 Uiso 1 1 d D . . H8B H 0.619(2) 0.408(2) 0.2624(18) 0.026 Uiso 1 1 d D . . O9 O 0.81819(13) 0.20010(13) -0.13003(11) 0.0288(3) Uani 1 1 d . . . O10 O 0.74307(13) 0.04111(12) -0.09065(11) 0.0272(3) Uani 1 1 d . . . O11 O 0.61523(15) 0.23599(15) -0.19210(16) 0.0470(4) Uani 1 1 d . . . O12 O 0.91009(15) 0.23881(15) 0.52109(13) 0.0385(3) Uani 1 1 d . . . O13 O 1.11638(14) 0.22718(14) 0.50475(12) 0.0364(3) Uani 1 1 d . . . O14 O 0.95585(14) 0.39363(12) 0.39122(11) 0.0322(3) Uani 1 1 d . . . N1 N 0.80899(13) -0.06049(12) 0.19843(11) 0.0198(3) Uani 1 1 d . . . N2 N 0.21853(12) 0.49983(11) -0.07910(10) 0.0140(2) Uani 1 1 d . . . N3 N -0.36100(13) 0.89911(13) -0.31220(11) 0.0201(2) Uani 1 1 d . . . N4 N 0.72417(14) 0.15914(13) -0.13779(12) 0.0224(3) Uani 1 1 d . . . N5 N 0.99235(16) 0.28626(14) 0.47206(13) 0.0271(3) Uani 1 1 d . . . C1 C 0.87274(16) -0.18737(15) 0.24958(15) 0.0236(3) Uani 1 1 d . . . H1A H 0.9644 -0.2184 0.2793 0.028 Uiso 1 1 calc R . . C2 C 0.80945(16) -0.27495(14) 0.26054(14) 0.0229(3) Uani 1 1 d . . . H2A H 0.8565 -0.3643 0.2980 0.027 Uiso 1 1 calc R . . C3 C 0.67601(16) -0.22917(14) 0.21562(14) 0.0210(3) Uani 1 1 d . . . H3A H 0.6305 -0.2869 0.2214 0.025 Uiso 1 1 calc R . . C4 C 0.60950(15) -0.09753(14) 0.16192(13) 0.0185(3) Uani 1 1 d . . . H4A H 0.5184 -0.0644 0.1302 0.022 Uiso 1 1 calc R . . C5 C 0.67858(14) -0.01529(13) 0.15539(12) 0.0163(3) Uani 1 1 d . . . C6 C 0.61680(14) 0.12777(13) 0.10478(12) 0.0159(3) Uani 1 1 d . . . C7 C 0.48132(14) 0.18740(13) 0.06205(12) 0.0173(3) Uani 1 1 d . . . H7A H 0.4309 0.1353 0.0624 0.021 Uiso 1 1 calc R . . C8 C 0.41480(14) 0.31971(13) 0.01856(12) 0.0146(2) Uani 1 1 d . . . C9 C 0.26910(14) 0.37111(13) -0.02723(11) 0.0147(2) Uani 1 1 d . . . C10 C 0.19088(14) 0.29526(14) -0.01823(13) 0.0177(3) Uani 1 1 d . . . H10A H 0.2274 0.2048 0.0210 0.021 Uiso 1 1 calc R . . C11 C 0.05795(15) 0.35469(14) -0.06798(13) 0.0198(3) Uani 1 1 d . . . H11A H 0.0026 0.3051 -0.0630 0.024 Uiso 1 1 calc R . . C12 C 0.00740(14) 0.48696(14) -0.12483(13) 0.0183(3) Uani 1 1 d . . . H12A H -0.0821 0.5292 -0.1611 0.022 Uiso 1 1 calc R . . C13 C 0.09055(14) 0.55667(13) -0.12760(12) 0.0151(2) Uani 1 1 d . . . C14 C 0.04583(14) 0.69937(13) -0.17890(12) 0.0154(2) Uani 1 1 d . . . C15 C -0.08411(15) 0.77233(14) -0.23033(13) 0.0181(3) Uani 1 1 d . . . H15A H -0.1401 0.7291 -0.2394 0.022 Uiso 1 1 calc R . . C16 C -0.13983(15) 0.90702(14) -0.27045(12) 0.0175(3) Uani 1 1 d . . . C17 C -0.28584(15) 0.97222(14) -0.31891(12) 0.0178(3) Uani 1 1 d . . . C18 C -0.33771(16) 1.10555(15) -0.36906(14) 0.0232(3) Uani 1 1 d . . . H18A H -0.2826 1.1546 -0.3714 0.028 Uiso 1 1 calc R . . C19 C -0.47175(17) 1.16540(16) -0.41564(15) 0.0263(3) Uani 1 1 d . . . H19A H -0.5091 1.2560 -0.4515 0.032 Uiso 1 1 calc R . . C20 C -0.54971(16) 1.09108(17) -0.40892(14) 0.0255(3) Uani 1 1 d . . . H20A H -0.6415 1.1296 -0.4398 0.031 Uiso 1 1 calc R . . C21 C -0.49067(16) 0.95845(16) -0.35584(14) 0.0234(3) Uani 1 1 d . . . H21A H -0.5448 0.9076 -0.3503 0.028 Uiso 1 1 calc R . . C22 C 0.8404(2) 0.09318(19) 0.40917(16) 0.0320(4) Uani 1 1 d . . . H22A H 0.9321 0.0955 0.4079 0.048 Uiso 1 1 calc R . . H22B H 0.8266 0.0467 0.4838 0.048 Uiso 1 1 calc R . . H22C H 0.7766 0.1807 0.3774 0.048 Uiso 1 1 calc R . . O1W O 0.34368(12) 0.35468(12) 0.25227(10) 0.0231(2) Uani 1 1 d . . . H1W H 0.350(2) 0.272(2) 0.2681(18) 0.028 Uiso 1 1 d D . . H2W H 0.324(2) 0.364(2) 0.307(2) 0.028 Uiso 1 1 d D . . O1S O 0.25783(13) 0.40029(12) 0.41926(11) 0.0290(3) Uani 1 1 d . . . H1S H 0.2061 0.3574 0.4412 0.035 Uiso 1 1 calc R . . O2S O 0.68293(14) 0.47231(13) 0.32023(11) 0.0304(3) Uani 1 1 d . . . H2S H 0.7649 0.4390 0.3452 0.037 Uiso 1 1 calc R . . C1S C 0.1817(2) 0.53349(19) 0.37351(19) 0.0363(4) Uani 1 1 d . . . H1S1 H 0.1325 0.5522 0.4278 0.054 Uiso 1 1 calc R . . H1S2 H 0.1179 0.5562 0.3116 0.054 Uiso 1 1 calc R . . H1S3 H 0.2423 0.5834 0.3498 0.054 Uiso 1 1 calc R . . C2S C 0.6064(2) 0.4843(2) 0.40245(18) 0.0380(4) Uani 1 1 d . . . H2S1 H 0.6301 0.4008 0.4660 0.057 Uiso 1 1 calc R . . H2S2 H 0.5106 0.5145 0.3758 0.057 Uiso 1 1 calc R . . H2S3 H 0.6259 0.5456 0.4221 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01115(10) 0.01007(9) 0.02625(11) -0.00379(8) -0.00288(7) -0.00225(7) Co2 0.00925(9) 0.00963(9) 0.01969(10) -0.00412(7) -0.00110(7) -0.00218(7) O1 0.0124(5) 0.0108(4) 0.0285(6) -0.0047(4) -0.0029(4) -0.0030(4) O2 0.0123(4) 0.0104(4) 0.0242(5) -0.0054(4) -0.0016(4) -0.0034(3) O3 0.0116(4) 0.0124(4) 0.0272(5) -0.0057(4) -0.0026(4) -0.0026(4) O4 0.0142(5) 0.0160(5) 0.0282(6) -0.0052(4) -0.0033(4) -0.0034(4) O5 0.0166(5) 0.0210(5) 0.0288(6) -0.0095(5) -0.0014(4) -0.0030(4) O6 0.0215(6) 0.0212(6) 0.0274(6) -0.0034(5) 0.0011(5) -0.0053(5) O7 0.0197(5) 0.0135(5) 0.0230(5) -0.0072(4) 0.0019(4) -0.0045(4) O8 0.0164(5) 0.0240(5) 0.0241(6) -0.0098(5) 0.0033(4) -0.0086(4) O9 0.0253(6) 0.0248(6) 0.0342(7) -0.0103(5) -0.0033(5) -0.0097(5) O10 0.0252(6) 0.0176(5) 0.0360(7) -0.0094(5) 0.0054(5) -0.0074(5) O11 0.0215(7) 0.0292(7) 0.0675(11) -0.0071(7) -0.0105(7) 0.0000(6) O12 0.0332(7) 0.0332(7) 0.0455(8) -0.0115(6) 0.0080(6) -0.0155(6) O13 0.0216(6) 0.0280(7) 0.0379(7) 0.0012(6) -0.0016(5) -0.0034(5) O14 0.0284(7) 0.0198(6) 0.0339(7) -0.0020(5) -0.0001(5) -0.0038(5) N1 0.0133(5) 0.0122(5) 0.0277(7) -0.0049(5) -0.0024(5) -0.0022(4) N2 0.0102(5) 0.0112(5) 0.0173(5) -0.0046(4) -0.0005(4) -0.0019(4) N3 0.0141(6) 0.0188(6) 0.0238(6) -0.0075(5) -0.0004(5) -0.0037(5) N4 0.0177(6) 0.0195(6) 0.0270(7) -0.0101(5) 0.0013(5) -0.0031(5) N5 0.0244(7) 0.0204(6) 0.0297(7) -0.0069(6) 0.0015(6) -0.0051(5) C1 0.0155(7) 0.0127(6) 0.0341(8) -0.0053(6) -0.0030(6) -0.0011(5) C2 0.0200(7) 0.0107(6) 0.0310(8) -0.0048(6) -0.0002(6) -0.0027(5) C3 0.0193(7) 0.0125(6) 0.0288(8) -0.0071(6) 0.0020(6) -0.0052(5) C4 0.0150(6) 0.0122(6) 0.0248(7) -0.0060(5) 0.0001(5) -0.0037(5) C5 0.0127(6) 0.0113(6) 0.0209(6) -0.0049(5) 0.0000(5) -0.0022(5) C6 0.0132(6) 0.0106(5) 0.0193(6) -0.0040(5) -0.0005(5) -0.0023(5) C7 0.0122(6) 0.0110(6) 0.0254(7) -0.0057(5) -0.0019(5) -0.0034(5) C8 0.0112(6) 0.0116(6) 0.0185(6) -0.0050(5) 0.0005(5) -0.0031(5) C9 0.0114(6) 0.0113(6) 0.0183(6) -0.0050(5) 0.0001(5) -0.0024(5) C10 0.0124(6) 0.0127(6) 0.0251(7) -0.0060(5) -0.0002(5) -0.0040(5) C11 0.0133(6) 0.0152(6) 0.0287(8) -0.0076(6) 0.0000(5) -0.0053(5) C12 0.0118(6) 0.0147(6) 0.0256(7) -0.0072(5) -0.0011(5) -0.0035(5) C13 0.0111(6) 0.0122(6) 0.0185(6) -0.0051(5) 0.0002(5) -0.0021(5) C14 0.0120(6) 0.0126(6) 0.0179(6) -0.0049(5) -0.0004(5) -0.0022(5) C15 0.0128(6) 0.0121(6) 0.0243(7) -0.0048(5) -0.0028(5) -0.0024(5) C16 0.0136(6) 0.0154(6) 0.0186(6) -0.0047(5) 0.0003(5) -0.0027(5) C17 0.0123(6) 0.0160(6) 0.0198(6) -0.0055(5) -0.0003(5) -0.0015(5) C18 0.0163(7) 0.0161(6) 0.0302(8) -0.0065(6) -0.0010(6) -0.0021(5) C19 0.0170(7) 0.0178(7) 0.0338(9) -0.0068(6) -0.0027(6) 0.0005(6) C20 0.0136(7) 0.0235(7) 0.0312(8) -0.0089(6) -0.0024(6) -0.0002(6) C21 0.0144(7) 0.0225(7) 0.0298(8) -0.0096(6) -0.0010(6) -0.0045(6) C22 0.0320(9) 0.0295(9) 0.0277(8) -0.0108(7) 0.0020(7) -0.0044(7) O1W 0.0195(5) 0.0184(5) 0.0286(6) -0.0079(5) 0.0042(4) -0.0067(4) O1S 0.0234(6) 0.0224(6) 0.0330(7) -0.0083(5) 0.0023(5) -0.0034(5) O2S 0.0259(6) 0.0288(6) 0.0364(7) -0.0154(6) 0.0010(5) -0.0077(5) C1S 0.0322(10) 0.0252(8) 0.0459(11) -0.0155(8) -0.0013(8) -0.0029(7) C2S 0.0360(10) 0.0370(10) 0.0378(10) -0.0165(9) 0.0058(8) -0.0087(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.0179(11) 2_665 ? Co1 O4 2.0278(11) 2_665 ? Co1 N1 2.0840(14) . ? Co1 O5 2.0899(13) . ? Co1 O1 2.1130(11) . ? Co1 O6 2.1519(13) . ? Co2 O8 2.0765(12) . ? Co2 O7 2.1051(12) . ? Co2 O2 2.1572(11) . ? Co2 N2 2.1831(12) 2_665 ? Co2 O1 2.1890(11) . ? Co2 O3 2.2250(11) 2_665 ? Co2 O2 2.2778(10) 2_665 ? O1 C6 1.2753(18) . ? O2 C8 1.2769(17) . ? O2 Co2 2.2778(10) 2_665 ? O3 C14 1.2807(18) . ? O3 Co1 2.0179(11) 2_665 ? O3 Co2 2.2249(11) 2_665 ? O4 C16 1.2637(19) . ? O4 Co1 2.0278(11) 2_665 ? O5 H5A 0.86(2) . ? O5 H5B 0.82(2) . ? O6 C22 1.417(2) . ? O6 H6 0.8400 . ? O7 H7B 0.77(2) . ? O7 H7C 0.84(2) . ? O8 H8A 0.74(2) . ? O8 H8B 1.07(2) . ? O9 N4 1.2694(19) . ? O10 N4 1.2575(18) . ? O11 N4 1.2353(19) . ? O12 N5 1.233(2) . ? O13 N5 1.265(2) . ? O14 N5 1.2534(19) . ? N1 C1 1.3431(19) . ? N1 C5 1.3528(18) . ? N2 C13 1.3447(17) . ? N2 C9 1.3480(17) . ? N2 Co2 2.1831(12) 2_665 ? N3 C21 1.343(2) . ? N3 C17 1.347(2) . ? C1 C2 1.390(2) . ? C1 H1A 0.9500 . ? C2 C3 1.388(2) . ? C2 H2A 0.9500 . ? C3 C4 1.394(2) . ? C3 H3A 0.9500 . ? C4 C5 1.392(2) . ? C4 H4A 0.9500 . ? C5 C6 1.5019(19) . ? C6 C7 1.3938(19) . ? C7 C8 1.4029(19) . ? C7 H7A 0.9500 . ? C8 C9 1.5021(19) . ? C9 C10 1.394(2) . ? C10 C11 1.394(2) . ? C10 H10A 0.9500 . ? C11 C12 1.387(2) . ? C11 H11A 0.9500 . ? C12 C13 1.394(2) . ? C12 H12A 0.9500 . ? C13 C14 1.4940(19) . ? C14 C15 1.3843(19) . ? C15 C16 1.420(2) . ? C15 H15A 0.9500 . ? C16 C17 1.510(2) . ? C17 C18 1.395(2) . ? C18 C19 1.393(2) . ? C18 H18A 0.9500 . ? C19 C20 1.383(3) . ? C19 H19A 0.9500 . ? C20 C21 1.394(2) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O1W H1W 0.92(2) . ? O1W H2W 0.84(2) . ? O1S C1S 1.429(2) . ? O1S H1S 0.8400 . ? O2S C2S 1.427(3) . ? O2S H2S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O4 89.41(5) 2_665 2_665 ? O3 Co1 N1 149.66(5) 2_665 . ? O4 Co1 N1 120.07(5) 2_665 . ? O3 Co1 O5 93.80(5) 2_665 . ? O4 Co1 O5 84.67(5) 2_665 . ? N1 Co1 O5 95.85(5) . . ? O3 Co1 O1 73.86(4) 2_665 . ? O4 Co1 O1 163.10(5) 2_665 . ? N1 Co1 O1 76.83(5) . . ? O5 Co1 O1 93.92(5) . . ? O3 Co1 O6 92.41(5) 2_665 . ? O4 Co1 O6 88.71(5) 2_665 . ? N1 Co1 O6 82.04(6) . . ? O5 Co1 O6 170.87(5) . . ? O1 Co1 O6 94.23(5) . . ? O8 Co2 O7 178.29(5) . . ? O8 Co2 O2 88.09(5) . . ? O7 Co2 O2 91.99(4) . . ? O8 Co2 N2 92.86(5) . 2_665 ? O7 Co2 N2 88.13(5) . 2_665 ? O2 Co2 N2 142.01(4) . 2_665 ? O8 Co2 O1 92.54(5) . . ? O7 Co2 O1 85.80(5) . . ? O2 Co2 O1 79.85(4) . . ? N2 Co2 O1 137.94(4) 2_665 . ? O8 Co2 O3 85.49(5) . 2_665 ? O7 Co2 O3 93.52(4) . 2_665 ? O2 Co2 O3 147.29(4) . 2_665 ? N2 Co2 O3 70.44(4) 2_665 2_665 ? O1 Co2 O3 68.46(4) . 2_665 ? O8 Co2 O2 92.74(4) . 2_665 ? O7 Co2 O2 88.90(4) . 2_665 ? O2 Co2 O2 70.77(4) . 2_665 ? N2 Co2 O2 71.24(4) 2_665 2_665 ? O1 Co2 O2 149.93(4) . 2_665 ? O3 Co2 O2 141.50(4) 2_665 2_665 ? C6 O1 Co1 117.05(9) . . ? C6 O1 Co2 133.00(9) . . ? Co1 O1 Co2 107.76(5) . . ? C8 O2 Co2 131.92(9) . . ? C8 O2 Co2 118.85(9) . 2_665 ? Co2 O2 Co2 109.23(4) . 2_665 ? C14 O3 Co1 126.58(9) . 2_665 ? C14 O3 Co2 121.79(9) . 2_665 ? Co1 O3 Co2 109.90(5) 2_665 2_665 ? C16 O4 Co1 126.54(10) . 2_665 ? Co1 O5 H5A 115.4(15) . . ? Co1 O5 H5B 118.3(17) . . ? H5A O5 H5B 113(2) . . ? C22 O6 Co1 119.43(11) . . ? C22 O6 H6 109.5 . . ? Co1 O6 H6 108.2 . . ? Co2 O7 H7B 114.7(17) . . ? Co2 O7 H7C 118.6(15) . . ? H7B O7 H7C 112(2) . . ? Co2 O8 H8A 114.9(18) . . ? Co2 O8 H8B 123.3(12) . . ? H8A O8 H8B 108(2) . . ? C1 N1 C5 119.31(14) . . ? C1 N1 Co1 124.57(11) . . ? C5 N1 Co1 115.72(10) . . ? C13 N2 C9 119.10(12) . . ? C13 N2 Co2 120.50(9) . 2_665 ? C9 N2 Co2 120.12(9) . 2_665 ? C21 N3 C17 117.89(14) . . ? O11 N4 O10 120.83(16) . . ? O11 N4 O9 119.41(15) . . ? O10 N4 O9 119.76(14) . . ? O12 N5 O14 121.40(16) . . ? O12 N5 O13 119.73(15) . . ? O14 N5 O13 118.86(16) . . ? N1 C1 C2 122.37(14) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 118.60(14) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C2 C3 C4 119.28(14) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 119.05(14) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 121.38(13) . . ? N1 C5 C6 114.32(13) . . ? C4 C5 C6 124.28(13) . . ? O1 C6 C7 123.96(13) . . ? O1 C6 C5 115.40(12) . . ? C7 C6 C5 120.63(13) . . ? C6 C7 C8 124.01(13) . . ? C6 C7 H7A 118.0 . . ? C8 C7 H7A 118.0 . . ? O2 C8 C7 126.38(13) . . ? O2 C8 C9 115.41(12) . . ? C7 C8 C9 118.21(12) . . ? N2 C9 C10 121.90(13) . . ? N2 C9 C8 113.78(12) . . ? C10 C9 C8 124.32(12) . . ? C9 C10 C11 118.73(13) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 119.33(14) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C13 118.65(13) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? N2 C13 C12 122.21(13) . . ? N2 C13 C14 113.67(12) . . ? C12 C13 C14 124.06(13) . . ? O3 C14 C15 125.69(13) . . ? O3 C14 C13 113.38(12) . . ? C15 C14 C13 120.90(13) . . ? C14 C15 C16 124.80(14) . . ? C14 C15 H15A 117.6 . . ? C16 C15 H15A 117.6 . . ? O4 C16 C15 125.70(14) . . ? O4 C16 C17 115.74(13) . . ? C15 C16 C17 118.56(14) . . ? N3 C17 C18 122.54(14) . . ? N3 C17 C16 118.55(13) . . ? C18 C17 C16 118.91(14) . . ? C19 C18 C17 118.74(16) . . ? C19 C18 H18A 120.6 . . ? C17 C18 H18A 120.6 . . ? C20 C19 C18 119.09(15) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C19 C20 C21 118.54(15) . . ? C19 C20 H20A 120.7 . . ? C21 C20 H20A 120.7 . . ? N3 C21 C20 123.18(16) . . ? N3 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? H1W O1W H2W 107(2) . . ? C1S O1S H1S 109.5 . . ? C2S O2S H2S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.779 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.073 # Attachment '2293_web_deposit_cif_file_1_OlivierRoubeau_1283333469.cif' data_MF47 _database_code_depnum_ccdc_archive 'CCDC 791563' #TrackingRef '2293_web_deposit_cif_file_1_OlivierRoubeau_1283333469.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C124 H94 Co8 N22 O28, 2(C7 H8), 4(N O3), 6(H2 O)' _chemical_formula_sum 'C138 H122 Co8 N26 O46' _chemical_formula_weight 3352.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0018 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0038 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0069 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Co Co 0.1865 1.0799 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _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 12.775(3) _cell_length_b 16.956(3) _cell_length_c 18.838(4) _cell_angle_alpha 65.59(3) _cell_angle_beta 70.26(3) _cell_angle_gamma 87.57(3) _cell_volume 3474.9(17) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55394 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 29.1 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'HKL2000, Otwinoski, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.75150 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ESRF BM16' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'phi rotation at various kappa' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 13157 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.03 _reflns_number_total 13157 _reflns_number_gt 9567 _reflns_threshold_expression >2sigma(I) _computing_data_collection MxCube _computing_cell_refinement 'HKL-2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL-2000 (Otwinowski & Minor, 1997)' _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. All non-hydrogens were refined anisotropically. The lattice toluene molecule was disordered over two positions, while the water molecules were partially occupied at 0.4 and 0.6, to result in a total of 4 water molecules per asymmetric unit. All these as well as one of the free nitrate ions were refined with displacement parameters restraints. Hydrogens were placed geometrically on their carrier atom when possible and refined with a riding model. Hydrogens on the coordinated water and hydroxyl moeities were found in difference Fourier maps and refined with their thermal parameter 1.5 times that of their carrier oxygen, as well as with soft distance restraints. Hydrogens on the partial lattice water molecules could not be found nor fixed and are omitted in the structural model. The poor completeness (92.5%) is rather due to geometrical limitations of the single-axis goniometer on BM16 than to poor diffraction. The present data corresponds to two datasets acquired for two kappa positions manually fixed and differing by ca. 20 degrees, close to the maximum permitted by the goniometer head. ; _vrf_PLAT029_MF47 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: The low completeness (92.5%) is likely due to geometrical limitations of the single-axis goniometer on BM16. The present data corresponds to two datasets acquired for two kappa positions manually fixed and differing by ca. 20 degrees, close to the maximum permitted by the goniometer head. ; _vrf_PLAT430_MF47 ; PROBLEM: Short Inter D...A Contact O5W .. O6W .. 2.43 Ang. RESPONSE: Oxygen sites of lattice water molecules (O1W-O6W) are partially occupied (0.4 or 0.6 occupancy). Hydrogens on these partial water molecules could not be found nor fixed and are omitted in the structural model. Short D-A contacts are found likely corresponding to hydrogen bonds involving these lattice water molecules. ; _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^)+(0.1336P)^2^+7.8260P] 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 SHELXL _refine_ls_extinction_coef 0.0110(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13157 _refine_ls_number_parameters 1066 _refine_ls_number_restraints 330 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2403 _refine_ls_wR_factor_gt 0.2113 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.95168(6) 0.21049(5) 0.96463(4) 0.0414(2) Uani 1 1 d D . . Co2 Co 0.85921(5) 0.40913(4) 0.86981(4) 0.0381(2) Uani 1 1 d . . . Co3 Co 0.66133(5) 0.53295(5) 0.78165(4) 0.0404(2) Uani 1 1 d D . . Co4 Co 0.56742(6) 0.73073(5) 0.68731(4) 0.0451(2) Uani 1 1 d . . . O1 O 0.8208(3) 0.2676(2) 0.9247(2) 0.0420(8) Uani 1 1 d . . . O2 O 0.7067(3) 0.3980(2) 0.8457(2) 0.0428(8) Uani 1 1 d . . . O3 O 0.5338(3) 0.6008(2) 0.7290(2) 0.0467(8) Uani 1 1 d . . . O4 O 0.4265(3) 0.7466(3) 0.6600(2) 0.0558(10) Uani 1 1 d . . . O5 O 0.6967(3) 0.6746(2) 0.7302(2) 0.0430(8) Uani 1 1 d . . . O6 O 0.8145(3) 0.5443(2) 0.8058(2) 0.0418(8) Uani 1 1 d . . . O7 O 0.9917(3) 0.3415(2) 0.9154(2) 0.0444(8) Uani 1 1 d . . . O8 O 1.0932(3) 0.1934(3) 0.9923(2) 0.0503(9) Uani 1 1 d . . . O9 O 0.8745(3) 0.2088(3) 1.0862(2) 0.0533(9) Uani 1 1 d D . . H9B H 0.902(3) 0.193(5) 1.1288(18) 0.080 Uiso 1 1 d D . . H9C H 0.8016(18) 0.215(5) 1.112(2) 0.080 Uiso 1 1 d D . . O10 O 0.7553(3) 0.4057(3) 0.9858(2) 0.0504(9) Uani 1 1 d D . . H10B H 0.711(5) 0.356(3) 1.025(3) 0.076 Uiso 1 1 d D . . O11 O 0.5736(2) 0.5349(2) 0.9118(2) 0.0481(10) Uani 1 1 d DU . . H11B H 0.610(2) 0.565(3) 0.928(2) 0.072 Uiso 1 1 d D . . H11C H 0.507(2) 0.557(4) 0.917(2) 0.072 Uiso 1 1 d D . . O12 O 0.4656(3) 0.7102(3) 0.8152(2) 0.0577(10) Uani 1 1 d U . . O13 O 0.3481(4) 0.7563(3) 0.9004(3) 0.0739(13) Uani 1 1 d U . . O14 O 0.3957(5) 0.8334(4) 0.7697(3) 0.0933(18) Uani 1 1 d U . . N1 N 0.8354(4) 0.1031(3) 1.0081(3) 0.0445(10) Uani 1 1 d . . . N2 N 0.5294(3) 0.4372(3) 0.8065(2) 0.0423(10) Uani 1 1 d . . . C18 C 0.2347(6) 0.8065(5) 0.6374(5) 0.077(2) Uani 1 1 d . . . H18A H 0.2806 0.8430 0.6447 0.092 Uiso 1 1 calc R . . N4 N 0.6529(4) 0.8370(3) 0.6806(3) 0.0513(11) Uani 1 1 d . . . N5 N 0.9696(3) 0.5017(3) 0.8704(2) 0.0396(9) Uani 1 1 d . . . C39 C 1.2462(5) 0.1295(4) 1.0698(4) 0.0590(15) Uani 1 1 d . . . H39A H 1.1965 0.0893 1.0698 0.071 Uiso 1 1 calc R . . N7 N 1.0473(3) 0.5856(3) 0.2488(2) 0.0414(10) Uani 1 1 d . . . N8 N 0.7555(3) 0.5375(3) 0.6626(2) 0.0412(10) Uani 1 1 d . . . N9 N 0.9604(3) 0.7940(3) 0.1517(3) 0.0413(9) Uani 1 1 d . . . N10 N 0.6626(4) 0.7488(3) 0.5634(3) 0.0475(11) Uani 1 1 d . . . N11 N 0.4022(4) 0.7669(4) 0.8284(3) 0.0614(13) Uani 1 1 d U . . C1 C 0.8465(5) 0.0211(4) 1.0536(3) 0.0526(13) Uani 1 1 d . . . H1A H 0.9136 0.0083 1.0653 0.063 Uiso 1 1 calc R . . C2 C 0.7621(5) -0.0469(4) 1.0847(4) 0.0564(14) Uani 1 1 d . . . H2A H 0.7719 -0.1051 1.1169 0.068 Uiso 1 1 calc R . . C3 C 0.6656(5) -0.0287(4) 1.0684(4) 0.0585(15) Uani 1 1 d . . . H3A H 0.6072 -0.0739 1.0890 0.070 Uiso 1 1 calc R . . C4 C 0.6541(5) 0.0568(4) 1.0211(4) 0.0539(14) Uani 1 1 d . . . H4A H 0.5872 0.0708 1.0093 0.065 Uiso 1 1 calc R . . C5 C 0.7412(4) 0.1223(4) 0.9910(3) 0.0460(12) Uani 1 1 d . . . C6 C 0.7381(4) 0.2177(4) 0.9421(3) 0.0428(11) Uani 1 1 d . . . C7 C 0.6469(5) 0.2464(4) 0.9162(3) 0.0479(12) Uani 1 1 d . . . H7A H 0.5875 0.2039 0.9318 0.058 Uiso 1 1 calc R . . C8 C 0.6380(4) 0.3333(4) 0.8689(3) 0.0439(12) Uani 1 1 d . . . C9 C 0.5407(4) 0.3527(4) 0.8407(3) 0.0442(12) Uani 1 1 d . . . C10 C 0.4716(5) 0.2900(4) 0.8442(4) 0.0635(16) Uani 1 1 d . . . H10A H 0.4827 0.2302 0.8670 0.076 Uiso 1 1 calc R . . C11 C 0.3856(6) 0.3163(5) 0.8136(5) 0.078(2) Uani 1 1 d . . . H11A H 0.3365 0.2745 0.8154 0.093 Uiso 1 1 calc R . . C12 C 0.3717(5) 0.4033(4) 0.7807(5) 0.0662(17) Uani 1 1 d . . . H12A H 0.3122 0.4220 0.7603 0.079 Uiso 1 1 calc R . . C13 C 0.4444(4) 0.4631(4) 0.7777(3) 0.0468(12) Uani 1 1 d . . . C14 C 0.4452(4) 0.5589(4) 0.7385(3) 0.0442(12) Uani 1 1 d . . . C15 C 0.3583(4) 0.5967(4) 0.7156(3) 0.0519(14) Uani 1 1 d . . . H15A H 0.2962 0.5590 0.7267 0.062 Uiso 1 1 calc R . . C16 C 0.3532(4) 0.6879(4) 0.6765(3) 0.0521(14) Uani 1 1 d . . . C17 C 0.2546(5) 0.7200(4) 0.6519(4) 0.0559(15) Uani 1 1 d . . . N3 N 0.1912(4) 0.6667(4) 0.6444(4) 0.0655(14) Uani 1 1 d . . . C21 C 0.1076(6) 0.6986(5) 0.6178(5) 0.075(2) Uani 1 1 d . . . H21A H 0.0629 0.6609 0.6108 0.089 Uiso 1 1 calc R . . C20 C 0.0815(6) 0.7831(5) 0.5998(5) 0.0721(19) Uani 1 1 d . . . H20A H 0.0218 0.8032 0.5799 0.087 Uiso 1 1 calc R . . C19 C 0.1437(6) 0.8364(6) 0.6114(6) 0.088(2) Uani 1 1 d . . . H19A H 0.1258 0.8940 0.6021 0.106 Uiso 1 1 calc R . . C22 C 0.6305(6) 0.9197(4) 0.6510(4) 0.0621(16) Uani 1 1 d . . . H22A H 0.5701 0.9330 0.6308 0.074 Uiso 1 1 calc R . . C23 C 0.6915(7) 0.9862(5) 0.6486(5) 0.0747(19) Uani 1 1 d . . . H23A H 0.6737 1.0445 0.6275 0.090 Uiso 1 1 calc R . . C24 C 0.7783(7) 0.9662(5) 0.6774(5) 0.0733(19) Uani 1 1 d . . . H24A H 0.8211 1.0112 0.6767 0.088 Uiso 1 1 calc R . . C25 C 0.8049(6) 0.8825(4) 0.7072(4) 0.0612(15) Uani 1 1 d . . . H25A H 0.8661 0.8688 0.7263 0.073 Uiso 1 1 calc R . . C26 C 0.7401(5) 0.8191(4) 0.7084(3) 0.0483(13) Uani 1 1 d . . . C27 C 0.7577(5) 0.7232(4) 0.7403(3) 0.0458(12) Uani 1 1 d . . . C28 C 0.8375(5) 0.6936(4) 0.7786(3) 0.0467(12) Uani 1 1 d . . . H28A H 0.8775 0.7349 0.7848 0.056 Uiso 1 1 calc R . . C29 C 0.8620(4) 0.6079(3) 0.8080(3) 0.0421(11) Uani 1 1 d . . . C30 C 0.9538(4) 0.5862(3) 0.8428(3) 0.0407(11) Uani 1 1 d . . . C31 C 1.0195(5) 0.6471(4) 0.8459(3) 0.0459(12) Uani 1 1 d . . . H31A H 1.0068 0.7067 0.8265 0.055 Uiso 1 1 calc R . . C32 C 1.1038(5) 0.6187(4) 0.8780(3) 0.0489(13) Uani 1 1 d . . . H32A H 1.1499 0.6592 0.8807 0.059 Uiso 1 1 calc R . . C33 C 1.1212(4) 0.5333(4) 0.9057(3) 0.0451(12) Uani 1 1 d . . . H33A H 1.1797 0.5137 0.9271 0.054 Uiso 1 1 calc R . . C34 C 1.0522(4) 0.4751(3) 0.9022(3) 0.0418(11) Uani 1 1 d . . . C35 C 1.0593(4) 0.3796(4) 0.9312(3) 0.0428(12) Uani 1 1 d . . . C36 C 1.1335(4) 0.3395(4) 0.9692(3) 0.0460(12) Uani 1 1 d . . . H36A H 1.1799 0.3753 0.9770 0.055 Uiso 1 1 calc R . . C37 C 1.1472(5) 0.2499(4) 0.9980(3) 0.0497(13) Uani 1 1 d . . . C38 C 1.2363(5) 0.2162(4) 1.0369(3) 0.0516(13) Uani 1 1 d . . . N6 N 1.3038(4) 0.2761(4) 1.0360(3) 0.0571(12) Uani 1 1 d . . . C42 C 1.3841(5) 0.2482(5) 1.0676(4) 0.0610(16) Uani 1 1 d . . . H42A H 1.4322 0.2897 1.0672 0.073 Uiso 1 1 calc R . . C41 C 1.4002(5) 0.1613(5) 1.1008(4) 0.0670(18) Uani 1 1 d . . . H41A H 1.4592 0.1432 1.1219 0.080 Uiso 1 1 calc R . . C40 C 1.3277(6) 0.1004(5) 1.1028(4) 0.0692(18) Uani 1 1 d . . . H40A H 1.3352 0.0399 1.1267 0.083 Uiso 1 1 calc R . . C43 C 1.0817(5) 0.6342(4) 0.2794(3) 0.0465(12) Uani 1 1 d . . . H43A H 1.1466 0.6750 0.2447 0.056 Uiso 1 1 calc R . . C44 C 0.9532(4) 0.5305(4) 0.2985(3) 0.0451(12) Uani 1 1 d . . . H44A H 0.9261 0.4968 0.2774 0.054 Uiso 1 1 calc R . . C45 C 1.0272(4) 0.6276(4) 0.3593(3) 0.0446(12) Uani 1 1 d . . . H45A H 1.0551 0.6630 0.3784 0.054 Uiso 1 1 calc R . . C46 C 0.8944(4) 0.5202(4) 0.3780(3) 0.0456(12) Uani 1 1 d . . . H46A H 0.8286 0.4800 0.4105 0.055 Uiso 1 1 calc R . . C47 C 0.9312(4) 0.5689(3) 0.4114(3) 0.0415(11) Uani 1 1 d . . . C48 C 0.8710(4) 0.5579(3) 0.4983(3) 0.0412(11) Uani 1 1 d . . . C49 C 0.9044(5) 0.6072(4) 0.5312(3) 0.0492(13) Uani 1 1 d . . . H49A H 0.9682 0.6495 0.4982 0.059 Uiso 1 1 calc R . . C50 C 0.7775(5) 0.4973(4) 0.5502(3) 0.0559(15) Uani 1 1 d . . . H50A H 0.7505 0.4619 0.5306 0.067 Uiso 1 1 calc R . . C51 C 0.8454(4) 0.5953(4) 0.6117(3) 0.0455(12) Uani 1 1 d . . . H51A H 0.8705 0.6306 0.6323 0.055 Uiso 1 1 calc R . . C52 C 0.7239(5) 0.4886(4) 0.6308(4) 0.0578(15) Uani 1 1 d . . . H52A H 0.6612 0.4457 0.6657 0.069 Uiso 1 1 calc R . . C53 C 0.8695(4) 0.7357(4) 0.2031(3) 0.0461(12) Uani 1 1 d . . . H53A H 0.8467 0.6983 0.1837 0.055 Uiso 1 1 calc R . . C54 C 0.9901(5) 0.8453(4) 0.1815(3) 0.0514(13) Uani 1 1 d . . . H54A H 1.0543 0.8868 0.1469 0.062 Uiso 1 1 calc R . . C55 C 0.8072(4) 0.7269(4) 0.2823(3) 0.0466(12) Uani 1 1 d . . . H55A H 0.7434 0.6848 0.3156 0.056 Uiso 1 1 calc R . . C56 C 0.9323(5) 0.8414(4) 0.2603(3) 0.0503(13) Uani 1 1 d . . . H56A H 0.9563 0.8799 0.2781 0.060 Uiso 1 1 calc R . . C57 C 0.8387(4) 0.7803(4) 0.3128(3) 0.0443(12) Uani 1 1 d . . . C58 C 0.7771(4) 0.7702(4) 0.3991(3) 0.0452(12) Uani 1 1 d . . . C59 C 0.8115(5) 0.8193(4) 0.4321(3) 0.0518(13) Uani 1 1 d . . . H59A H 0.8753 0.8615 0.3991 0.062 Uiso 1 1 calc R . . C60 C 0.6840(5) 0.7092(4) 0.4522(3) 0.0535(14) Uani 1 1 d . . . H60A H 0.6575 0.6728 0.4333 0.064 Uiso 1 1 calc R . . C61 C 0.7529(5) 0.8068(4) 0.5133(3) 0.0549(14) Uani 1 1 d . . . H61A H 0.7782 0.8412 0.5345 0.066 Uiso 1 1 calc R . . C62 C 0.6299(5) 0.7013(4) 0.5320(3) 0.0520(14) Uani 1 1 d . . . H62A H 0.5657 0.6596 0.5664 0.062 Uiso 1 1 calc R . . N12 N 0.9707(5) 0.0689(4) 0.2323(4) 0.0705(14) Uani 1 1 d U . . O15 O 0.9877(5) 0.0114(3) 0.2935(3) 0.0789(14) Uani 1 1 d U . . O16 O 0.9914(5) 0.1460(3) 0.2110(4) 0.0950(17) Uani 1 1 d U . . O17 O 0.9299(7) 0.0517(5) 0.1898(5) 0.125(2) Uani 1 1 d U . . N13 N 0.6911(6) 0.1558(5) 0.7865(5) 0.0918(19) Uani 1 1 d U . . O18 O 0.6005(4) 0.1137(4) 0.8436(3) 0.0809(14) Uani 1 1 d U . . O19 O 0.7794(6) 0.1203(6) 0.7784(6) 0.147(3) Uani 1 1 d U . . O20 O 0.6933(6) 0.2355(5) 0.7397(4) 0.1084(19) Uani 1 1 d U . . C63 C 0.4960(10) 0.1290(8) 0.5700(8) 0.087(5) Uani 0.50 1 d PGU A 1 H63A H 0.5564 0.1743 0.5393 0.104 Uiso 0.50 1 calc PR A 1 C64 C 0.4654(10) 0.0848(8) 0.5309(6) 0.092(4) Uani 0.50 1 d PGU A 1 H64A H 0.5050 0.0999 0.4735 0.111 Uiso 0.50 1 calc PR A 1 C65 C 0.3771(11) 0.0184(9) 0.5758(7) 0.089(4) Uani 0.50 1 d PGU A 1 H65A H 0.3562 -0.0118 0.5490 0.107 Uiso 0.50 1 calc PR A 1 C66 C 0.3193(11) -0.0038(9) 0.6597(7) 0.099(5) Uani 0.50 1 d PGU A 1 H66A H 0.2589 -0.0491 0.6904 0.119 Uiso 0.50 1 calc PR A 1 C67 C 0.3498(10) 0.0404(9) 0.6988(6) 0.087(4) Uani 0.50 1 d PGU A 1 H67A H 0.3103 0.0253 0.7562 0.104 Uiso 0.50 1 calc PR A 1 C68 C 0.4382(11) 0.1068(8) 0.6540(8) 0.094(4) Uani 0.50 1 d PGDU A 1 C69 C 0.466(2) 0.1572(18) 0.6939(14) 0.110(6) Uani 0.50 1 d PDU A 1 H69A H 0.3994 0.1572 0.7389 0.165 Uiso 0.50 1 calc PR A 1 H69B H 0.4945 0.2173 0.6526 0.165 Uiso 0.50 1 calc PR A 1 H69C H 0.5241 0.1307 0.7169 0.165 Uiso 0.50 1 calc PR A 1 C73 C 0.4997(13) -0.1275(10) 0.4459(7) 0.093(5) Uani 0.50 1 d PGU B 2 H73A H 0.4866 -0.1264 0.4982 0.112 Uiso 0.50 1 calc PR B 2 C74 C 0.4374(11) -0.1888(8) 0.4406(7) 0.103(4) Uani 0.50 1 d PGU B 2 H74A H 0.3817 -0.2295 0.4893 0.124 Uiso 0.50 1 calc PR B 2 C75 C 0.4566(11) -0.1904(9) 0.3641(9) 0.104(5) Uani 0.50 1 d PGU B 2 H75A H 0.4140 -0.2323 0.3605 0.125 Uiso 0.50 1 calc PR B 2 C76 C 0.5380(13) -0.1307(11) 0.2928(7) 0.111(6) Uani 0.50 1 d PGU B 2 H76A H 0.5512 -0.1318 0.2405 0.133 Uiso 0.50 1 calc PR B 2 C77 C 0.6004(11) -0.0694(9) 0.2981(7) 0.106(5) Uani 0.50 1 d PGU B 2 H77A H 0.6561 -0.0286 0.2494 0.127 Uiso 0.50 1 calc PR B 2 C78 C 0.5812(11) -0.0678(8) 0.3746(9) 0.101(4) Uani 0.50 1 d PGDU B 2 C79 C 0.653(3) -0.010(2) 0.383(2) 0.155(8) Uani 0.50 1 d PDU B 2 H79A H 0.7098 0.0246 0.3287 0.232 Uiso 0.50 1 calc PR B 2 H79B H 0.6901 -0.0453 0.4220 0.232 Uiso 0.50 1 calc PR B 2 H79C H 0.6078 0.0284 0.4047 0.232 Uiso 0.50 1 calc PR B 2 O1W O 0.3353(6) 0.4580(5) 0.9782(6) 0.073(2) Uani 0.60 1 d PU . . O2W O 0.9721(8) 0.9463(6) 0.4650(5) 0.084(2) Uani 0.60 1 d PU . . O3W O 0.9075(7) 0.1916(7) 0.5951(6) 0.088(3) Uani 0.60 1 d PU . . O4W O 0.7768(15) 0.2985(10) 0.5639(9) 0.102(5) Uani 0.40 1 d PU . . O5W O 0.393(2) 0.4590(16) 0.5923(15) 0.162(8) Uani 0.40 1 d PU . . O6W O 0.3880(17) 0.6130(15) 0.5121(11) 0.135(6) Uani 0.40 1 d PU . . 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 0.0414(4) 0.0466(4) 0.0377(4) -0.0195(3) -0.0138(3) 0.0057(3) Co2 0.0396(4) 0.0453(4) 0.0308(3) -0.0179(3) -0.0116(3) 0.0030(3) Co3 0.0393(4) 0.0492(4) 0.0315(3) -0.0176(3) -0.0103(3) 0.0035(3) Co4 0.0445(4) 0.0512(4) 0.0382(4) -0.0179(3) -0.0145(3) 0.0073(3) O1 0.0375(17) 0.048(2) 0.0400(18) -0.0192(16) -0.0121(14) 0.0026(15) O2 0.0417(18) 0.049(2) 0.0384(17) -0.0172(16) -0.0167(15) 0.0042(15) O3 0.0424(19) 0.051(2) 0.0458(19) -0.0194(17) -0.0162(16) 0.0063(16) O4 0.053(2) 0.064(3) 0.047(2) -0.0194(19) -0.0186(18) 0.0135(19) O5 0.0437(18) 0.050(2) 0.0382(17) -0.0217(16) -0.0135(15) 0.0048(15) O6 0.0470(19) 0.0421(19) 0.0361(17) -0.0161(15) -0.0150(15) 0.0036(15) O7 0.0424(18) 0.051(2) 0.0432(19) -0.0235(17) -0.0144(15) 0.0067(15) O8 0.052(2) 0.059(2) 0.050(2) -0.0291(19) -0.0230(18) 0.0147(18) O9 0.059(2) 0.064(2) 0.0408(19) -0.0254(19) -0.0181(17) 0.0102(19) O10 0.048(2) 0.065(3) 0.0358(18) -0.0233(18) -0.0086(16) 0.0004(18) O11 0.0186(13) 0.0461(19) 0.067(2) -0.0374(18) 0.0177(14) -0.0063(13) O12 0.061(2) 0.065(3) 0.045(2) -0.0245(19) -0.0168(18) 0.019(2) O13 0.074(3) 0.088(3) 0.049(2) -0.037(2) 0.002(2) 0.004(2) O14 0.111(4) 0.089(4) 0.068(3) -0.028(3) -0.029(3) 0.046(3) N1 0.050(2) 0.045(2) 0.039(2) -0.0192(19) -0.0158(19) 0.0083(19) N2 0.037(2) 0.052(3) 0.0323(19) -0.0169(19) -0.0065(17) -0.0005(18) C18 0.069(4) 0.070(5) 0.096(5) -0.031(4) -0.042(4) 0.019(3) N4 0.059(3) 0.053(3) 0.043(2) -0.023(2) -0.017(2) 0.017(2) N5 0.044(2) 0.046(2) 0.0306(19) -0.0196(18) -0.0109(17) 0.0038(18) C39 0.063(4) 0.069(4) 0.056(3) -0.033(3) -0.026(3) 0.020(3) N7 0.040(2) 0.050(2) 0.0315(19) -0.0169(18) -0.0102(17) 0.0047(18) N8 0.042(2) 0.050(2) 0.034(2) -0.0195(19) -0.0138(17) 0.0076(18) N9 0.043(2) 0.045(2) 0.039(2) -0.0190(19) -0.0165(18) 0.0065(18) N10 0.046(2) 0.053(3) 0.038(2) -0.015(2) -0.0142(19) 0.006(2) N11 0.060(3) 0.075(3) 0.044(2) -0.025(2) -0.013(2) 0.015(3) C1 0.058(3) 0.052(3) 0.048(3) -0.022(3) -0.018(3) 0.009(3) C2 0.065(4) 0.044(3) 0.058(3) -0.020(3) -0.022(3) 0.008(3) C3 0.060(3) 0.049(3) 0.064(4) -0.022(3) -0.020(3) -0.001(3) C4 0.052(3) 0.054(3) 0.057(3) -0.023(3) -0.022(3) 0.008(3) C5 0.048(3) 0.053(3) 0.038(2) -0.023(2) -0.012(2) 0.006(2) C6 0.043(3) 0.054(3) 0.035(2) -0.023(2) -0.012(2) 0.007(2) C7 0.049(3) 0.049(3) 0.041(3) -0.015(2) -0.014(2) -0.001(2) C8 0.040(2) 0.054(3) 0.035(2) -0.019(2) -0.008(2) -0.001(2) C9 0.044(3) 0.050(3) 0.037(2) -0.017(2) -0.015(2) 0.000(2) C10 0.056(3) 0.058(4) 0.073(4) -0.017(3) -0.032(3) 0.003(3) C11 0.071(4) 0.061(4) 0.110(6) -0.023(4) -0.058(4) 0.001(3) C12 0.056(3) 0.062(4) 0.082(4) -0.022(3) -0.038(3) 0.007(3) C13 0.040(3) 0.061(3) 0.038(3) -0.019(2) -0.014(2) 0.003(2) C14 0.039(3) 0.055(3) 0.036(2) -0.018(2) -0.012(2) 0.004(2) C15 0.037(3) 0.063(4) 0.049(3) -0.019(3) -0.013(2) 0.007(2) C16 0.041(3) 0.068(4) 0.046(3) -0.025(3) -0.013(2) 0.003(3) C17 0.054(3) 0.061(4) 0.046(3) -0.019(3) -0.015(3) 0.011(3) N3 0.058(3) 0.070(4) 0.071(3) -0.028(3) -0.030(3) 0.012(3) C21 0.061(4) 0.079(5) 0.088(5) -0.031(4) -0.038(4) 0.020(3) C20 0.056(4) 0.085(5) 0.078(5) -0.031(4) -0.030(3) 0.010(3) C19 0.075(5) 0.077(5) 0.103(6) -0.029(5) -0.034(4) 0.030(4) C22 0.076(4) 0.054(4) 0.065(4) -0.028(3) -0.034(3) 0.018(3) C23 0.087(5) 0.055(4) 0.084(5) -0.027(4) -0.038(4) 0.015(3) C24 0.091(5) 0.055(4) 0.085(5) -0.029(4) -0.046(4) 0.010(3) C25 0.072(4) 0.051(3) 0.068(4) -0.026(3) -0.033(3) 0.012(3) C26 0.052(3) 0.049(3) 0.041(3) -0.018(2) -0.014(2) 0.008(2) C27 0.051(3) 0.048(3) 0.034(2) -0.020(2) -0.006(2) 0.004(2) C28 0.054(3) 0.047(3) 0.041(3) -0.022(2) -0.014(2) 0.004(2) C29 0.045(3) 0.047(3) 0.033(2) -0.017(2) -0.012(2) 0.003(2) C30 0.044(3) 0.048(3) 0.030(2) -0.019(2) -0.009(2) 0.003(2) C31 0.057(3) 0.045(3) 0.041(3) -0.021(2) -0.019(2) 0.004(2) C32 0.050(3) 0.058(3) 0.044(3) -0.026(3) -0.016(2) -0.002(2) C33 0.044(3) 0.057(3) 0.039(3) -0.024(2) -0.016(2) 0.004(2) C34 0.042(3) 0.052(3) 0.033(2) -0.022(2) -0.010(2) 0.005(2) C35 0.039(2) 0.060(3) 0.035(2) -0.027(2) -0.010(2) 0.003(2) C36 0.047(3) 0.051(3) 0.045(3) -0.024(2) -0.016(2) 0.005(2) C37 0.048(3) 0.064(4) 0.043(3) -0.030(3) -0.016(2) 0.010(3) C38 0.048(3) 0.069(4) 0.045(3) -0.032(3) -0.016(2) 0.010(3) N6 0.052(3) 0.074(3) 0.056(3) -0.034(3) -0.025(2) 0.011(2) C42 0.056(3) 0.079(4) 0.058(3) -0.034(3) -0.027(3) 0.019(3) C41 0.056(3) 0.095(5) 0.066(4) -0.045(4) -0.028(3) 0.023(3) C40 0.078(4) 0.078(5) 0.066(4) -0.038(4) -0.035(4) 0.028(4) C43 0.047(3) 0.056(3) 0.039(3) -0.028(2) -0.008(2) -0.001(2) C44 0.045(3) 0.053(3) 0.039(3) -0.023(2) -0.013(2) 0.002(2) C45 0.042(3) 0.058(3) 0.036(2) -0.025(2) -0.009(2) 0.000(2) C46 0.047(3) 0.054(3) 0.035(2) -0.020(2) -0.010(2) -0.003(2) C47 0.044(3) 0.047(3) 0.034(2) -0.017(2) -0.015(2) 0.007(2) C48 0.044(3) 0.049(3) 0.032(2) -0.018(2) -0.014(2) 0.010(2) C49 0.048(3) 0.060(3) 0.040(3) -0.025(3) -0.009(2) 0.002(2) C50 0.057(3) 0.068(4) 0.044(3) -0.031(3) -0.007(3) -0.009(3) C51 0.045(3) 0.060(3) 0.038(3) -0.027(2) -0.014(2) 0.000(2) C52 0.060(3) 0.066(4) 0.043(3) -0.028(3) -0.006(3) -0.011(3) C53 0.043(3) 0.059(3) 0.042(3) -0.027(3) -0.014(2) 0.006(2) C54 0.061(3) 0.045(3) 0.042(3) -0.017(2) -0.013(2) -0.002(2) C55 0.044(3) 0.055(3) 0.044(3) -0.024(2) -0.017(2) 0.005(2) C56 0.060(3) 0.050(3) 0.041(3) -0.022(2) -0.012(2) -0.002(2) C57 0.044(3) 0.049(3) 0.042(3) -0.022(2) -0.015(2) 0.009(2) C58 0.047(3) 0.050(3) 0.039(3) -0.018(2) -0.017(2) 0.012(2) C59 0.052(3) 0.062(3) 0.044(3) -0.027(3) -0.014(2) -0.002(3) C60 0.057(3) 0.059(3) 0.043(3) -0.024(3) -0.011(2) -0.006(3) C61 0.059(3) 0.064(4) 0.045(3) -0.027(3) -0.014(3) -0.003(3) C62 0.055(3) 0.054(3) 0.041(3) -0.019(3) -0.011(2) -0.004(3) N12 0.090(4) 0.054(2) 0.075(3) -0.021(2) -0.046(3) 0.005(3) O15 0.112(4) 0.059(2) 0.073(3) -0.017(2) -0.053(3) -0.004(3) O16 0.120(4) 0.049(2) 0.107(4) -0.027(2) -0.036(3) 0.010(3) O17 0.187(6) 0.101(4) 0.118(4) -0.030(3) -0.107(4) -0.002(4) N13 0.075(3) 0.096(4) 0.104(5) -0.054(3) -0.016(3) 0.006(3) O18 0.076(3) 0.085(3) 0.087(3) -0.043(3) -0.025(2) 0.003(2) O19 0.070(3) 0.151(6) 0.210(8) -0.078(6) -0.035(4) 0.016(3) O20 0.128(5) 0.099(3) 0.086(4) -0.043(3) -0.016(3) -0.002(3) C63 0.088(8) 0.085(8) 0.084(6) -0.026(6) -0.039(6) 0.026(6) C64 0.092(7) 0.089(8) 0.094(7) -0.031(6) -0.042(6) 0.019(6) C65 0.087(7) 0.087(7) 0.090(7) -0.033(6) -0.034(6) 0.027(5) C66 0.106(8) 0.094(8) 0.092(7) -0.038(6) -0.031(6) 0.016(6) C67 0.084(7) 0.090(7) 0.084(7) -0.030(5) -0.036(6) 0.023(5) C68 0.097(8) 0.088(8) 0.100(7) -0.043(6) -0.034(6) 0.023(6) C69 0.115(11) 0.118(10) 0.100(9) -0.041(8) -0.046(8) 0.005(7) C73 0.107(9) 0.102(9) 0.077(7) -0.035(6) -0.046(6) 0.039(6) C74 0.105(8) 0.105(8) 0.090(7) -0.038(6) -0.030(6) 0.024(6) C75 0.107(8) 0.104(8) 0.100(7) -0.051(6) -0.028(6) 0.021(6) C76 0.116(10) 0.115(10) 0.094(8) -0.044(7) -0.031(7) 0.023(7) C77 0.104(9) 0.105(9) 0.092(7) -0.034(7) -0.026(7) 0.021(6) C78 0.106(8) 0.091(8) 0.107(7) -0.045(6) -0.035(6) 0.032(6) C79 0.161(12) 0.150(12) 0.162(12) -0.075(9) -0.056(9) 0.005(7) O1W 0.051(4) 0.078(5) 0.101(5) -0.056(4) -0.016(4) -0.002(3) O2W 0.095(5) 0.085(5) 0.079(5) -0.028(4) -0.044(4) -0.004(4) O3W 0.077(5) 0.106(6) 0.075(5) -0.028(4) -0.030(4) -0.018(4) O4W 0.136(9) 0.087(7) 0.079(7) -0.045(6) -0.020(6) 0.021(7) O5W 0.207(12) 0.157(12) 0.156(11) -0.067(8) -0.098(9) -0.014(8) O6W 0.150(10) 0.168(11) 0.110(9) -0.066(8) -0.060(8) -0.018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O8 2.023(4) . ? Co1 O7 2.032(4) . ? Co1 N1 2.089(5) . ? Co1 O1 2.099(4) . ? Co1 N9 2.130(4) 2_766 ? Co1 O9 2.154(4) . ? Co2 N7 2.114(4) 2_766 ? Co2 O10 2.117(4) . ? Co2 N5 2.160(4) . ? Co2 O2 2.177(4) . ? Co2 O1 2.185(4) . ? Co2 O7 2.219(4) . ? Co2 O6 2.258(4) . ? Co3 N8 2.128(4) . ? Co3 N2 2.183(4) . ? Co3 O6 2.186(4) . ? Co3 O5 2.187(4) . ? Co3 O3 2.225(4) . ? Co3 O2 2.259(4) . ? Co3 O11 2.340(4) . ? Co4 O4 2.012(4) . ? Co4 O3 2.019(4) . ? Co4 N4 2.084(5) . ? Co4 O5 2.102(4) . ? Co4 N10 2.132(4) . ? Co4 O12 2.201(4) . ? O1 C6 1.247(6) . ? O2 C8 1.261(6) . ? O3 C14 1.281(6) . ? O4 C16 1.261(7) . ? O5 C27 1.269(7) . ? O6 C29 1.283(6) . ? O7 C35 1.277(6) . ? O8 C37 1.264(7) . ? O9 H9B 0.92(4) . ? O9 H9C 0.92(4) . ? O10 H10B 0.91(5) . ? O11 H11B 0.90(4) . ? O11 H11C 0.91(4) . ? O12 N11 1.280(6) . ? O13 N11 1.234(6) . ? O14 N11 1.234(7) . ? N1 C1 1.331(7) . ? N1 C5 1.341(7) . ? N2 C9 1.331(7) . ? N2 C13 1.352(7) . ? C18 C17 1.404(10) . ? C18 C19 1.406(10) . ? C18 H18A 0.9500 . ? N4 C22 1.337(8) . ? N4 C26 1.357(7) . ? N5 C30 1.340(7) . ? N5 C34 1.356(7) . ? C39 C38 1.358(9) . ? C39 C40 1.363(9) . ? C39 H39A 0.9500 . ? N7 C43 1.341(7) . ? N7 C44 1.344(7) . ? N7 Co2 2.114(4) 2_766 ? N8 C51 1.332(7) . ? N8 C52 1.345(7) . ? N9 C54 1.339(7) . ? N9 C53 1.345(7) . ? N9 Co1 2.130(4) 2_766 ? N10 C62 1.327(8) . ? N10 C61 1.335(7) . ? C1 C2 1.399(8) . ? C1 H1A 0.9500 . ? C2 C3 1.362(9) . ? C2 H2A 0.9500 . ? C3 C4 1.385(8) . ? C3 H3A 0.9500 . ? C4 C5 1.398(8) . ? C4 H4A 0.9500 . ? C5 C6 1.502(8) . ? C6 C7 1.405(8) . ? C7 C8 1.396(8) . ? C7 H7A 0.9500 . ? C8 C9 1.484(7) . ? C9 C10 1.377(8) . ? C10 C11 1.381(9) . ? C10 H10A 0.9500 . ? C11 C12 1.375(10) . ? C11 H11A 0.9500 . ? C12 C13 1.374(9) . ? C12 H12A 0.9500 . ? C13 C14 1.480(8) . ? C14 C15 1.366(8) . ? C15 C16 1.421(9) . ? C15 H15A 0.9500 . ? C16 C17 1.493(8) . ? C17 N3 1.318(9) . ? N3 C21 1.332(8) . ? C21 C20 1.383(10) . ? C21 H21A 0.9500 . ? C20 C19 1.356(11) . ? C20 H20A 0.9500 . ? C19 H19A 0.9500 . ? C22 C23 1.375(10) . ? C22 H22A 0.9500 . ? C23 C24 1.364(10) . ? C23 H23A 0.9500 . ? C24 C25 1.369(9) . ? C24 H24A 0.9500 . ? C25 C26 1.371(9) . ? C25 H25A 0.9500 . ? C26 C27 1.519(8) . ? C27 C28 1.403(8) . ? C28 C29 1.389(8) . ? C28 H28A 0.9500 . ? C29 C30 1.490(7) . ? C30 C31 1.390(8) . ? C31 C32 1.382(8) . ? C31 H31A 0.9500 . ? C32 C33 1.360(8) . ? C32 H32A 0.9500 . ? C33 C34 1.386(8) . ? C33 H33A 0.9500 . ? C34 C35 1.489(8) . ? C35 C36 1.369(8) . ? C36 C37 1.412(8) . ? C36 H36A 0.9500 . ? C37 C38 1.523(8) . ? C38 N6 1.351(8) . ? N6 C42 1.329(8) . ? C42 C41 1.381(10) . ? C42 H42A 0.9500 . ? C41 C40 1.395(10) . ? C41 H41A 0.9500 . ? C40 H40A 0.9500 . ? C43 C45 1.386(7) . ? C43 H43A 0.9500 . ? C44 C46 1.368(7) . ? C44 H44A 0.9500 . ? C45 C47 1.393(7) . ? C45 H45A 0.9500 . ? C46 C47 1.400(8) . ? C46 H46A 0.9500 . ? C47 C48 1.489(7) . ? C48 C49 1.380(8) . ? C48 C50 1.386(8) . ? C49 C51 1.378(7) . ? C49 H49A 0.9500 . ? C50 C52 1.386(8) . ? C50 H50A 0.9500 . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C55 1.380(7) . ? C53 H53A 0.9500 . ? C54 C56 1.391(7) . ? C54 H54A 0.9500 . ? C55 C57 1.388(8) . ? C55 H55A 0.9500 . ? C56 C57 1.393(8) . ? C56 H56A 0.9500 . ? C57 C58 1.485(7) . ? C58 C59 1.385(8) . ? C58 C60 1.390(8) . ? C59 C61 1.384(8) . ? C59 H59A 0.9500 . ? C60 C62 1.376(8) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? N12 O16 1.210(7) . ? N12 O17 1.218(8) . ? N12 O15 1.245(7) . ? N13 O19 1.249(9) . ? N13 O18 1.265(8) . ? N13 O20 1.268(9) . ? C63 C64 1.3900 . ? C63 C68 1.3900 . ? C63 H63A 0.9500 . ? C64 C65 1.3900 . ? C64 H64A 0.9500 . ? C65 C66 1.3900 . ? C65 H65A 0.9500 . ? C66 C67 1.3900 . ? C66 H66A 0.9500 . ? C67 C68 1.3900 . ? C67 H67A 0.9500 . ? C68 C69 1.47(2) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C73 H73A 0.9500 . ? C74 C75 1.3900 . ? C74 H74A 0.9500 . ? C75 C76 1.3900 . ? C75 H75A 0.9500 . ? C76 C77 1.3900 . ? C76 H76A 0.9500 . ? C77 C78 1.3900 . ? C77 H77A 0.9500 . ? C78 C79 1.46(2) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Co1 O7 88.97(16) . . ? O8 Co1 N1 119.83(17) . . ? O7 Co1 N1 150.25(16) . . ? O8 Co1 O1 162.71(16) . . ? O7 Co1 O1 73.80(15) . . ? N1 Co1 O1 77.11(16) . . ? O8 Co1 N9 90.04(16) . 2_766 ? O7 Co1 N9 92.24(16) . 2_766 ? N1 Co1 N9 94.84(17) . 2_766 ? O1 Co1 N9 91.98(15) . 2_766 ? O8 Co1 O9 85.07(16) . . ? O7 Co1 O9 89.59(16) . . ? N1 Co1 O9 85.96(17) . . ? O1 Co1 O9 93.27(15) . . ? N9 Co1 O9 174.74(16) 2_766 . ? N7 Co2 O10 175.80(16) 2_766 . ? N7 Co2 N5 97.87(16) 2_766 . ? O10 Co2 N5 84.68(15) . . ? N7 Co2 O2 88.75(15) 2_766 . ? O10 Co2 O2 87.20(14) . . ? N5 Co2 O2 142.08(15) . . ? N7 Co2 O1 92.41(16) 2_766 . ? O10 Co2 O1 87.91(15) . . ? N5 Co2 O1 137.35(15) . . ? O2 Co2 O1 79.04(14) . . ? N7 Co2 O7 88.69(15) 2_766 . ? O10 Co2 O7 95.33(14) . . ? N5 Co2 O7 70.40(15) . . ? O2 Co2 O7 147.38(14) . . ? O1 Co2 O7 68.58(14) . . ? N7 Co2 O6 88.62(15) 2_766 . ? O10 Co2 O6 89.02(15) . . ? N5 Co2 O6 71.73(15) . . ? O2 Co2 O6 71.15(14) . . ? O1 Co2 O6 150.15(13) . . ? O7 Co2 O6 141.26(14) . . ? N8 Co3 N2 93.77(16) . . ? N8 Co3 O6 91.20(15) . . ? N2 Co3 O6 142.05(15) . . ? N8 Co3 O5 89.55(15) . . ? N2 Co3 O5 138.52(16) . . ? O6 Co3 O5 79.04(14) . . ? N8 Co3 O3 88.29(15) . . ? N2 Co3 O3 70.27(15) . . ? O6 Co3 O3 147.56(14) . . ? O5 Co3 O3 68.52(14) . . ? N8 Co3 O2 91.08(15) . . ? N2 Co3 O2 71.32(15) . . ? O6 Co3 O2 70.98(13) . . ? O5 Co3 O2 150.03(14) . . ? O3 Co3 O2 141.46(14) . . ? N8 Co3 O11 174.33(15) . . ? N2 Co3 O11 91.71(14) . . ? O6 Co3 O11 83.58(13) . . ? O5 Co3 O11 87.29(13) . . ? O3 Co3 O11 94.92(14) . . ? O2 Co3 O11 89.32(13) . . ? O4 Co4 O3 88.68(17) . . ? O4 Co4 N4 119.32(19) . . ? O3 Co4 N4 150.58(17) . . ? O4 Co4 O5 162.74(17) . . ? O3 Co4 O5 74.10(15) . . ? N4 Co4 O5 77.51(17) . . ? O4 Co4 N10 90.40(17) . . ? O3 Co4 N10 93.48(17) . . ? N4 Co4 N10 95.02(18) . . ? O5 Co4 N10 91.87(16) . . ? O4 Co4 O12 88.40(16) . . ? O3 Co4 O12 85.57(16) . . ? N4 Co4 O12 86.38(18) . . ? O5 Co4 O12 89.01(15) . . ? N10 Co4 O12 178.48(18) . . ? C6 O1 Co1 117.1(3) . . ? C6 O1 Co2 134.3(3) . . ? Co1 O1 Co2 108.21(15) . . ? C8 O2 Co2 131.9(3) . . ? C8 O2 Co3 118.4(3) . . ? Co2 O2 Co3 109.08(16) . . ? C14 O3 Co4 127.9(3) . . ? C14 O3 Co3 121.7(3) . . ? Co4 O3 Co3 109.42(17) . . ? C16 O4 Co4 127.5(4) . . ? C27 O5 Co4 116.8(3) . . ? C27 O5 Co3 132.5(3) . . ? Co4 O5 Co3 107.86(16) . . ? C29 O6 Co3 130.9(3) . . ? C29 O6 Co2 117.9(3) . . ? Co3 O6 Co2 108.79(15) . . ? C35 O7 Co1 125.4(3) . . ? C35 O7 Co2 121.7(3) . . ? Co1 O7 Co2 109.41(17) . . ? C37 O8 Co1 125.1(4) . . ? Co1 O9 H9B 129.2(16) . . ? Co1 O9 H9C 129.0(16) . . ? H9B O9 H9C 101(3) . . ? Co2 O10 H10B 119(5) . . ? Co3 O11 H11B 118.6(18) . . ? Co3 O11 H11C 113.7(17) . . ? H11B O11 H11C 102(2) . . ? N11 O12 Co4 120.5(3) . . ? C1 N1 C5 119.9(5) . . ? C1 N1 Co1 125.0(4) . . ? C5 N1 Co1 115.0(4) . . ? C9 N2 C13 119.7(5) . . ? C9 N2 Co3 119.3(3) . . ? C13 N2 Co3 120.4(4) . . ? C17 C18 C19 116.8(8) . . ? C17 C18 H18A 121.6 . . ? C19 C18 H18A 121.6 . . ? C22 N4 C26 118.1(5) . . ? C22 N4 Co4 126.2(4) . . ? C26 N4 Co4 115.7(4) . . ? C30 N5 C34 118.9(5) . . ? C30 N5 Co2 120.1(3) . . ? C34 N5 Co2 120.9(3) . . ? C38 C39 C40 119.6(7) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? C43 N7 C44 116.9(4) . . ? C43 N7 Co2 121.6(3) . 2_766 ? C44 N7 Co2 121.4(4) . 2_766 ? C51 N8 C52 115.7(4) . . ? C51 N8 Co3 121.0(4) . . ? C52 N8 Co3 123.0(4) . . ? C54 N9 C53 116.0(5) . . ? C54 N9 Co1 126.7(4) . 2_766 ? C53 N9 Co1 117.1(4) . 2_766 ? C62 N10 C61 116.7(5) . . ? C62 N10 Co4 118.9(4) . . ? C61 N10 Co4 124.3(4) . . ? O13 N11 O14 119.2(6) . . ? O13 N11 O12 120.1(5) . . ? O14 N11 O12 120.7(5) . . ? N1 C1 C2 121.8(6) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 119.0(6) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 119.6(6) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 120.5(5) . . ? N1 C5 C6 114.3(5) . . ? C4 C5 C6 125.1(5) . . ? O1 C6 C7 123.3(5) . . ? O1 C6 C5 116.5(5) . . ? C7 C6 C5 120.2(5) . . ? C8 C7 C6 124.2(5) . . ? C8 C7 H7A 117.9 . . ? C6 C7 H7A 117.9 . . ? O2 C8 C7 126.2(5) . . ? O2 C8 C9 115.9(5) . . ? C7 C8 C9 117.9(5) . . ? N2 C9 C10 122.1(5) . . ? N2 C9 C8 114.2(5) . . ? C10 C9 C8 123.6(5) . . ? C9 C10 C11 118.3(6) . . ? C9 C10 H10A 120.8 . . ? C11 C10 H10A 120.8 . . ? C12 C11 C10 119.6(6) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C13 C12 C11 119.5(6) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? N2 C13 C12 120.7(6) . . ? N2 C13 C14 113.4(5) . . ? C12 C13 C14 125.7(5) . . ? O3 C14 C15 124.8(5) . . ? O3 C14 C13 113.5(5) . . ? C15 C14 C13 121.6(5) . . ? C14 C15 C16 125.2(6) . . ? C14 C15 H15A 117.4 . . ? C16 C15 H15A 117.4 . . ? O4 C16 C15 125.4(5) . . ? O4 C16 C17 115.2(6) . . ? C15 C16 C17 119.4(5) . . ? N3 C17 C18 123.4(6) . . ? N3 C17 C16 118.9(6) . . ? C18 C17 C16 117.7(6) . . ? C17 N3 C21 117.5(6) . . ? N3 C21 C20 124.2(8) . . ? N3 C21 H21A 117.9 . . ? C20 C21 H21A 117.9 . . ? C19 C20 C21 117.9(7) . . ? C19 C20 H20A 121.1 . . ? C21 C20 H20A 121.1 . . ? C20 C19 C18 120.0(8) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? N4 C22 C23 122.5(6) . . ? N4 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? C24 C23 C22 118.1(7) . . ? C24 C23 H23A 121.0 . . ? C22 C23 H23A 121.0 . . ? C23 C24 C25 121.2(7) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C24 C25 C26 117.8(6) . . ? C24 C25 H25A 121.1 . . ? C26 C25 H25A 121.1 . . ? N4 C26 C25 122.4(5) . . ? N4 C26 C27 113.3(5) . . ? C25 C26 C27 124.3(5) . . ? O5 C27 C28 124.2(5) . . ? O5 C27 C26 116.2(5) . . ? C28 C27 C26 119.7(5) . . ? C29 C28 C27 124.3(5) . . ? C29 C28 H28A 117.8 . . ? C27 C28 H28A 117.8 . . ? O6 C29 C28 125.6(5) . . ? O6 C29 C30 115.5(5) . . ? C28 C29 C30 118.9(5) . . ? N5 C30 C31 121.9(5) . . ? N5 C30 C29 114.0(5) . . ? C31 C30 C29 124.1(5) . . ? C32 C31 C30 118.3(5) . . ? C32 C31 H31A 120.8 . . ? C30 C31 H31A 120.8 . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 118.9(5) . . ? C32 C33 H33A 120.5 . . ? C34 C33 H33A 120.5 . . ? N5 C34 C33 121.6(5) . . ? N5 C34 C35 113.0(5) . . ? C33 C34 C35 125.3(5) . . ? O7 C35 C36 125.1(5) . . ? O7 C35 C34 113.1(5) . . ? C36 C35 C34 121.8(5) . . ? C35 C36 C37 126.0(5) . . ? C35 C36 H36A 117.0 . . ? C37 C36 H36A 117.0 . . ? O8 C37 C36 125.4(5) . . ? O8 C37 C38 115.3(5) . . ? C36 C37 C38 119.3(5) . . ? N6 C38 C39 122.8(6) . . ? N6 C38 C37 117.0(5) . . ? C39 C38 C37 120.2(6) . . ? C42 N6 C38 117.9(6) . . ? N6 C42 C41 122.5(7) . . ? N6 C42 H42A 118.8 . . ? C41 C42 H42A 118.8 . . ? C42 C41 C40 118.5(6) . . ? C42 C41 H41A 120.7 . . ? C40 C41 H41A 120.7 . . ? C39 C40 C41 118.7(7) . . ? C39 C40 H40A 120.6 . . ? C41 C40 H40A 120.6 . . ? N7 C43 C45 123.1(5) . . ? N7 C43 H43A 118.4 . . ? C45 C43 H43A 118.4 . . ? N7 C44 C46 123.5(5) . . ? N7 C44 H44A 118.2 . . ? C46 C44 H44A 118.2 . . ? C43 C45 C47 119.8(5) . . ? C43 C45 H45A 120.1 . . ? C47 C45 H45A 120.1 . . ? C44 C46 C47 120.0(5) . . ? C44 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C45 C47 C46 116.5(5) . . ? C45 C47 C48 122.0(5) . . ? C46 C47 C48 121.5(5) . . ? C49 C48 C50 116.7(5) . . ? C49 C48 C47 122.1(5) . . ? C50 C48 C47 121.2(5) . . ? C51 C49 C48 120.1(5) . . ? C51 C49 H49A 120.0 . . ? C48 C49 H49A 120.0 . . ? C52 C50 C48 119.5(6) . . ? C52 C50 H50A 120.2 . . ? C48 C50 H50A 120.2 . . ? N8 C51 C49 124.1(5) . . ? N8 C51 H51A 117.9 . . ? C49 C51 H51A 117.9 . . ? N8 C52 C50 123.8(5) . . ? N8 C52 H52A 118.1 . . ? C50 C52 H52A 118.1 . . ? N9 C53 C55 124.2(5) . . ? N9 C53 H53A 117.9 . . ? C55 C53 H53A 117.9 . . ? N9 C54 C56 123.8(5) . . ? N9 C54 H54A 118.1 . . ? C56 C54 H54A 118.1 . . ? C53 C55 C57 119.4(5) . . ? C53 C55 H55A 120.3 . . ? C57 C55 H55A 120.3 . . ? C54 C56 C57 119.2(5) . . ? C54 C56 H56A 120.4 . . ? C57 C56 H56A 120.4 . . ? C55 C57 C56 117.3(5) . . ? C55 C57 C58 121.2(5) . . ? C56 C57 C58 121.5(5) . . ? C59 C58 C60 116.0(5) . . ? C59 C58 C57 121.8(5) . . ? C60 C58 C57 122.1(5) . . ? C61 C59 C58 119.9(5) . . ? C61 C59 H59A 120.0 . . ? C58 C59 H59A 120.0 . . ? C62 C60 C58 120.4(6) . . ? C62 C60 H60A 119.8 . . ? C58 C60 H60A 119.8 . . ? N10 C61 C59 123.4(6) . . ? N10 C61 H61A 118.3 . . ? C59 C61 H61A 118.3 . . ? N10 C62 C60 123.4(5) . . ? N10 C62 H62A 118.3 . . ? C60 C62 H62A 118.3 . . ? O16 N12 O17 114.6(7) . . ? O16 N12 O15 122.9(7) . . ? O17 N12 O15 122.4(6) . . ? O19 N13 O18 120.4(8) . . ? O19 N13 O20 119.8(8) . . ? O18 N13 O20 119.8(7) . . ? C64 C63 C68 120.0 . . ? C64 C63 H63A 120.0 . . ? C68 C63 H63A 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 H64A 120.0 . . ? C63 C64 H64A 120.0 . . ? C64 C65 C66 120.0 . . ? C64 C65 H65A 120.0 . . ? C66 C65 H65A 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? C67 C68 C63 120.0 . . ? C67 C68 C69 120.1(13) . . ? C63 C68 C69 119.8(13) . . ? C74 C73 C78 120.0 . . ? C74 C73 H73A 120.0 . . ? C78 C73 H73A 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74A 120.0 . . ? C73 C74 H74A 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75A 120.0 . . ? C76 C75 H75A 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 H76A 120.0 . . ? C75 C76 H76A 120.0 . . ? C76 C77 C78 120.0 . . ? C76 C77 H77A 120.0 . . ? C78 C77 H77A 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 C79 120.9(17) . . ? C73 C78 C79 118.8(17) . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.279 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.130