# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Michael Chetcuti' 'Aline Devoille' 'Amel Ben Othman' 'Rachid Souane' 'Pierre Thuery' 'Jacques Vicens' _publ_contact_author_name 'Michael Chetcuti' _publ_contact_author_email CHETCUTI@CHIMIE.U-STRASBG.FR _publ_section_title ; Synthesis of Mono-, Di- and Tetra-Alkyne Functionalized Calix[4]arenes: Reactions of these Multipodal Ligands with Dicobalt Octacarbonyl to give Complexes which Contain up to Eight Cobalt Atoms. ; # Attachment 'Co_calix.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 711451' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H64 O4' _chemical_formula_weight 801.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2014(6) _cell_length_b 13.8433(7) _cell_length_c 17.0902(9) _cell_angle_alpha 79.184(3) _cell_angle_beta 84.737(3) _cell_angle_gamma 66.210(2) _cell_volume 2381.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 117841 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.68 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type none _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f and eight \w scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 117841 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9030 _reflns_number_gt 6889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. One tert-butyl group is rotationally disordered over two positions which have been refined with occupancy parameters constrained to sum to unity. All non-hydrogen atoms were refined with anisotropic displacement parameters, with restraints on bond lengths and/or displacement parameters for some badly behaving atoms. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.0756P)^2^+0.9896P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9030 _refine_ls_number_parameters 584 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.338 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.523 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.101 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 O1 O 0.27242(15) 0.63589(13) 0.23948(10) 0.0288(4) Uani 1 1 d . . . O2 O 0.11164(15) 0.77269(13) 0.34894(9) 0.0258(4) Uani 1 1 d . . . O3 O 0.16065(15) 0.89783(12) 0.17514(10) 0.0272(4) Uani 1 1 d . . . O4 O 0.25842(15) 0.75548(13) 0.04849(9) 0.0260(4) Uani 1 1 d . . . C1 C 0.4671(2) 0.49414(18) 0.20046(14) 0.0246(5) Uani 1 1 d . . . C2 C 0.3842(2) 0.54467(17) 0.25996(14) 0.0243(5) Uani 1 1 d . . . C3 C 0.4190(2) 0.51356(17) 0.33998(14) 0.0242(5) Uani 1 1 d . . . C4 C 0.5391(2) 0.43041(18) 0.35977(14) 0.0260(5) Uani 1 1 d . . . H4 H 0.5626 0.4091 0.4130 0.031 Uiso 1 1 calc R . . C5 C 0.6256(2) 0.37784(18) 0.30241(14) 0.0266(5) Uani 1 1 d . A . C6 C 0.5852(2) 0.41033(18) 0.22337(14) 0.0262(5) Uani 1 1 d . . . H6 H 0.6395 0.3745 0.1845 0.031 Uiso 1 1 calc R . . C7 C 0.7616(2) 0.2916(2) 0.32399(15) 0.0367(6) Uani 1 1 d D . . C8A C 0.7842(4) 0.2612(4) 0.4108(3) 0.0368(12) Uani 0.587(5) 1 d P A 1 H8A1 H 0.7197 0.2359 0.4362 0.055 Uiso 0.587(5) 1 calc PR A 1 H8A2 H 0.7780 0.3224 0.4322 0.055 Uiso 0.587(5) 1 calc PR A 1 H8A3 H 0.8696 0.2055 0.4204 0.055 Uiso 0.587(5) 1 calc PR A 1 C9A C 0.7660(5) 0.1872(3) 0.2949(3) 0.0378(12) Uani 0.587(5) 1 d PD A 1 H9A1 H 0.8494 0.1298 0.3068 0.057 Uiso 0.587(5) 1 calc PR A 1 H9A2 H 0.7528 0.2021 0.2385 0.057 Uiso 0.587(5) 1 calc PR A 1 H9A3 H 0.6985 0.1670 0.3219 0.057 Uiso 0.587(5) 1 calc PR A 1 C10A C 0.8633(4) 0.3226(4) 0.2780(3) 0.0387(12) Uani 0.587(5) 1 d P A 1 H10A H 0.8615 0.3865 0.2932 0.058 Uiso 0.587(5) 1 calc PR A 1 H10B H 0.8467 0.3354 0.2221 0.058 Uiso 0.587(5) 1 calc PR A 1 H10C H 0.9475 0.2658 0.2890 0.058 Uiso 0.587(5) 1 calc PR A 1 C8B C 0.7594(7) 0.2039(6) 0.3872(4) 0.0414(19) Uani 0.413(5) 1 d P A 2 H8B1 H 0.8472 0.1567 0.4017 0.062 Uiso 0.413(5) 1 calc PR A 2 H8B2 H 0.7172 0.1649 0.3681 0.062 Uiso 0.413(5) 1 calc PR A 2 H8B3 H 0.7125 0.2330 0.4329 0.062 Uiso 0.413(5) 1 calc PR A 2 C9B C 0.8513(6) 0.2573(6) 0.2566(4) 0.042(2) Uani 0.413(5) 1 d P A 2 H9B1 H 0.9364 0.2105 0.2764 0.063 Uiso 0.413(5) 1 calc PR A 2 H9B2 H 0.8565 0.3190 0.2223 0.063 Uiso 0.413(5) 1 calc PR A 2 H9B3 H 0.8194 0.2202 0.2272 0.063 Uiso 0.413(5) 1 calc PR A 2 C10B C 0.8296(7) 0.3502(6) 0.3655(4) 0.049(2) Uani 0.413(5) 1 d PD A 2 H10D H 0.7804 0.3733 0.4124 0.073 Uiso 0.413(5) 1 calc PR A 2 H10E H 0.8324 0.4111 0.3290 0.073 Uiso 0.413(5) 1 calc PR A 2 H10F H 0.9168 0.3013 0.3800 0.073 Uiso 0.413(5) 1 calc PR A 2 C11 C 0.1592(2) 0.6207(2) 0.22266(16) 0.0381(6) Uani 1 1 d . . . H11A H 0.1763 0.5886 0.1748 0.046 Uiso 1 1 calc R . . H11B H 0.0877 0.6901 0.2117 0.046 Uiso 1 1 calc R . . C12 C 0.1184(3) 0.5533(2) 0.28671(18) 0.0389(6) Uani 1 1 d . . . C13 C 0.0830(3) 0.4985(3) 0.3364(2) 0.0554(8) Uani 1 1 d . . . H13 H 0.0551 0.4553 0.3755 0.066 Uiso 1 1 calc R . . C14 C 0.3312(2) 0.57457(18) 0.40283(14) 0.0256(5) Uani 1 1 d . . . H14A H 0.3595 0.5336 0.4552 0.031 Uiso 1 1 calc R . . H14B H 0.2426 0.5820 0.3964 0.031 Uiso 1 1 calc R . . C15 C 0.3322(2) 0.68506(18) 0.39792(13) 0.0242(5) Uani 1 1 d . . . C16 C 0.2250(2) 0.77852(18) 0.37149(13) 0.0232(5) Uani 1 1 d . . . C17 C 0.2327(2) 0.87846(18) 0.36199(13) 0.0235(5) Uani 1 1 d . . . C18 C 0.3454(2) 0.88286(18) 0.38603(13) 0.0254(5) Uani 1 1 d . . . H18 H 0.3491 0.9495 0.3823 0.031 Uiso 1 1 calc R . . C19 C 0.4534(2) 0.79150(19) 0.41565(13) 0.0254(5) Uani 1 1 d . . . C20 C 0.4448(2) 0.69325(18) 0.41883(13) 0.0251(5) Uani 1 1 d . . . H20 H 0.5168 0.6309 0.4355 0.030 Uiso 1 1 calc R . . C21 C 0.5721(2) 0.8031(2) 0.44461(15) 0.0303(5) Uani 1 1 d . . . C22 C 0.5338(3) 0.8472(2) 0.52348(16) 0.0414(7) Uani 1 1 d . . . H22A H 0.5135 0.7967 0.5631 0.062 Uiso 1 1 calc R . . H22B H 0.4589 0.9138 0.5155 0.062 Uiso 1 1 calc R . . H22C H 0.6052 0.8588 0.5411 0.062 Uiso 1 1 calc R . . C23 C 0.6899(3) 0.6956(2) 0.45953(18) 0.0404(6) Uani 1 1 d . . . H23A H 0.6686 0.6480 0.5014 0.061 Uiso 1 1 calc R . . H23B H 0.7630 0.7070 0.4748 0.061 Uiso 1 1 calc R . . H23C H 0.7117 0.6647 0.4117 0.061 Uiso 1 1 calc R . . C24 C 0.6133(3) 0.8809(2) 0.38342(16) 0.0352(6) Uani 1 1 d . . . H24A H 0.6890 0.8854 0.4020 0.053 Uiso 1 1 calc R . . H24B H 0.5433 0.9505 0.3767 0.053 Uiso 1 1 calc R . . H24C H 0.6335 0.8554 0.3333 0.053 Uiso 1 1 calc R . . C25 C 0.0235(2) 0.76375(19) 0.41310(15) 0.0300(5) Uani 1 1 d . . . H25A H 0.0721 0.7077 0.4553 0.036 Uiso 1 1 calc R . . H25B H -0.0398 0.7422 0.3944 0.036 Uiso 1 1 calc R . . C26 C -0.0467(2) 0.8628(2) 0.44624(15) 0.0306(5) Uani 1 1 d . . . C27 C -0.1059(3) 0.9412(2) 0.47424(16) 0.0378(6) Uani 1 1 d . . . H27 H -0.1523 1.0028 0.4962 0.045 Uiso 1 1 calc R . . C28 C 0.1263(2) 0.98001(18) 0.32068(14) 0.0256(5) Uani 1 1 d . . . H28A H 0.0547 0.9640 0.3073 0.031 Uiso 1 1 calc R . . H28B H 0.0929 1.0327 0.3560 0.031 Uiso 1 1 calc R . . C29 C 0.1833(2) 1.02407(17) 0.24565(13) 0.0243(5) Uani 1 1 d . . . C30 C 0.2035(2) 0.97852(18) 0.17680(14) 0.0246(5) Uani 1 1 d . . . C31 C 0.2758(2) 1.00618(18) 0.11195(14) 0.0248(5) Uani 1 1 d . . . C32 C 0.3203(2) 1.08619(18) 0.11547(14) 0.0251(5) Uani 1 1 d . . . H32 H 0.3675 1.1057 0.0723 0.030 Uiso 1 1 calc R . . C33 C 0.2964(2) 1.13769(18) 0.18152(14) 0.0254(5) Uani 1 1 d . . . C34 C 0.2282(2) 1.10448(18) 0.24581(14) 0.0251(5) Uani 1 1 d . . . H34 H 0.2120 1.1373 0.2907 0.030 Uiso 1 1 calc R . . C35 C 0.3450(3) 1.2265(2) 0.18303(15) 0.0321(6) Uani 1 1 d . . . C36 C 0.4815(5) 1.1949(5) 0.1526(4) 0.1138(16) Uani 1 1 d U . . H36A H 0.5116 1.2497 0.1562 0.171 Uiso 1 1 calc R . . H36B H 0.4852 1.1857 0.0980 0.171 Uiso 1 1 calc R . . H36C H 0.5360 1.1288 0.1840 0.171 Uiso 1 1 calc R . . C37 C 0.2614(6) 1.3259(4) 0.1306(4) 0.1193(17) Uani 1 1 d U . . H37A H 0.1730 1.3490 0.1506 0.179 Uiso 1 1 calc R . . H37B H 0.2645 1.3116 0.0775 0.179 Uiso 1 1 calc R . . H37C H 0.2928 1.3811 0.1301 0.179 Uiso 1 1 calc R . . C38 C 0.3435(4) 1.2512(3) 0.2647(2) 0.0690(10) Uani 1 1 d U . . H38A H 0.3778 1.3050 0.2623 0.104 Uiso 1 1 calc R . . H38B H 0.3961 1.1874 0.2992 0.104 Uiso 1 1 calc R . . H38C H 0.2554 1.2769 0.2852 0.104 Uiso 1 1 calc R . . C39 C 0.0421(2) 0.9324(2) 0.13223(16) 0.0324(6) Uani 1 1 d . . . H39A H 0.0474 0.8767 0.1034 0.039 Uiso 1 1 calc R . . H39B H 0.0334 0.9957 0.0934 0.039 Uiso 1 1 calc R . . C40 C -0.0737(3) 0.9570(2) 0.18444(18) 0.0423(7) Uani 1 1 d . . . C41 C -0.1662(3) 0.9732(4) 0.2262(2) 0.0693(11) Uani 1 1 d . . . H41 H -0.2398 0.9862 0.2593 0.083 Uiso 1 1 calc R . . C42 C 0.3113(2) 0.94563(18) 0.04193(14) 0.0264(5) Uani 1 1 d . . . H42A H 0.3460 0.9833 -0.0016 0.032 Uiso 1 1 calc R . . H42B H 0.2333 0.9432 0.0235 0.032 Uiso 1 1 calc R . . C43 C 0.4118(2) 0.83203(18) 0.06491(13) 0.0247(5) Uani 1 1 d . . . C44 C 0.3827(2) 0.74254(19) 0.06893(13) 0.0245(5) Uani 1 1 d . . . C45 C 0.4745(2) 0.63983(18) 0.09498(13) 0.0245(5) Uani 1 1 d . . . C46 C 0.5986(2) 0.62819(19) 0.11229(14) 0.0272(5) Uani 1 1 d . . . H46 H 0.6613 0.5596 0.1273 0.033 Uiso 1 1 calc R . . C47 C 0.6332(2) 0.7150(2) 0.10820(14) 0.0275(5) Uani 1 1 d . . . C48 C 0.5370(2) 0.81652(19) 0.08545(13) 0.0265(5) Uani 1 1 d . . . H48 H 0.5567 0.8760 0.0839 0.032 Uiso 1 1 calc R . . C49 C 0.7681(2) 0.6963(2) 0.13595(16) 0.0341(6) Uani 1 1 d . . . C50 C 0.7642(3) 0.6733(3) 0.22682(19) 0.0634(10) Uani 1 1 d . . . H50A H 0.8451 0.6661 0.2469 0.095 Uiso 1 1 calc R . . H50B H 0.7513 0.6081 0.2442 0.095 Uiso 1 1 calc R . . H50C H 0.6937 0.7312 0.2465 0.095 Uiso 1 1 calc R . . C51 C 0.8751(3) 0.6017(3) 0.1049(2) 0.0543(8) Uani 1 1 d . . . H51A H 0.9585 0.5949 0.1209 0.081 Uiso 1 1 calc R . . H51B H 0.8725 0.6130 0.0479 0.081 Uiso 1 1 calc R . . H51C H 0.8620 0.5374 0.1265 0.081 Uiso 1 1 calc R . . C52 C 0.8008(4) 0.7940(3) 0.1084(3) 0.0705(11) Uani 1 1 d U . . H52A H 0.7410 0.8526 0.1330 0.106 Uiso 1 1 calc R . . H52B H 0.7937 0.8133 0.0516 0.106 Uiso 1 1 calc R . . H52C H 0.8882 0.7777 0.1233 0.106 Uiso 1 1 calc R . . C53 C 0.2561(2) 0.7453(2) -0.03304(15) 0.0335(6) Uani 1 1 d . . . H53A H 0.3196 0.6756 -0.0420 0.040 Uiso 1 1 calc R . . H53B H 0.2793 0.7996 -0.0673 0.040 Uiso 1 1 calc R . . C54 C 0.1263(3) 0.7573(2) -0.05263(16) 0.0353(6) Uani 1 1 d . . . C55 C 0.0233(3) 0.7684(2) -0.07330(19) 0.0471(7) Uani 1 1 d . . . H55 H -0.0579 0.7772 -0.0896 0.056 Uiso 1 1 calc R . . C56 C 0.4398(2) 0.54203(19) 0.11330(14) 0.0268(5) Uani 1 1 d . . . H56A H 0.3483 0.5628 0.1028 0.032 Uiso 1 1 calc R . . H56B H 0.4917 0.4898 0.0799 0.032 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 O1 0.0240(8) 0.0258(9) 0.0322(9) -0.0047(7) -0.0042(7) -0.0046(7) O2 0.0223(8) 0.0270(8) 0.0285(9) -0.0055(7) 0.0007(6) -0.0099(7) O3 0.0276(9) 0.0244(8) 0.0316(9) -0.0047(7) -0.0003(7) -0.0123(7) O4 0.0251(8) 0.0277(8) 0.0253(8) -0.0063(7) -0.0024(6) -0.0094(7) C1 0.0282(12) 0.0218(11) 0.0272(12) -0.0046(9) -0.0012(9) -0.0129(9) C2 0.0220(11) 0.0197(11) 0.0304(12) -0.0040(9) -0.0024(9) -0.0071(9) C3 0.0258(12) 0.0207(11) 0.0273(12) -0.0036(9) 0.0004(9) -0.0109(9) C4 0.0281(12) 0.0233(12) 0.0254(12) -0.0023(9) -0.0018(9) -0.0093(10) C5 0.0268(12) 0.0210(11) 0.0289(12) -0.0024(9) -0.0006(9) -0.0068(10) C6 0.0279(12) 0.0217(11) 0.0277(12) -0.0057(9) 0.0013(9) -0.0083(10) C7 0.0288(13) 0.0336(14) 0.0321(14) 0.0014(11) 0.0014(11) 0.0003(11) C8A 0.032(2) 0.034(3) 0.034(2) -0.006(2) -0.0064(18) -0.001(2) C9A 0.038(3) 0.029(2) 0.036(2) -0.0065(19) -0.0052(19) -0.0008(19) C10A 0.028(2) 0.040(3) 0.041(3) -0.006(2) -0.0015(19) -0.006(2) C8B 0.036(4) 0.034(4) 0.037(4) 0.003(3) 0.005(3) -0.001(3) C9B 0.029(3) 0.041(4) 0.035(4) 0.002(3) 0.007(3) 0.002(3) C10B 0.033(4) 0.049(4) 0.051(4) 0.002(3) -0.007(3) -0.006(3) C11 0.0245(13) 0.0479(16) 0.0396(15) -0.0092(12) -0.0063(11) -0.0100(12) C12 0.0287(14) 0.0404(15) 0.0499(17) -0.0137(13) -0.0057(12) -0.0123(12) C13 0.0518(19) 0.057(2) 0.067(2) -0.0022(17) -0.0080(16) -0.0326(17) C14 0.0259(12) 0.0226(11) 0.0263(12) -0.0039(9) 0.0005(9) -0.0079(9) C15 0.0264(12) 0.0244(12) 0.0211(11) -0.0051(9) 0.0018(9) -0.0093(10) C16 0.0222(11) 0.0255(12) 0.0218(11) -0.0050(9) 0.0007(9) -0.0089(9) C17 0.0241(11) 0.0230(11) 0.0213(11) -0.0048(9) 0.0017(9) -0.0072(9) C18 0.0292(12) 0.0235(12) 0.0244(12) -0.0055(9) 0.0015(9) -0.0108(10) C19 0.0255(12) 0.0290(12) 0.0221(11) -0.0047(9) 0.0001(9) -0.0111(10) C20 0.0243(12) 0.0241(11) 0.0238(11) -0.0036(9) -0.0002(9) -0.0066(9) C21 0.0295(13) 0.0302(13) 0.0324(13) -0.0039(10) -0.0032(10) -0.0131(11) C22 0.0457(16) 0.0534(17) 0.0345(14) -0.0102(13) -0.0048(12) -0.0269(14) C23 0.0307(14) 0.0369(15) 0.0537(17) 0.0003(13) -0.0119(12) -0.0145(12) C24 0.0332(14) 0.0360(14) 0.0395(15) -0.0030(11) -0.0027(11) -0.0178(11) C25 0.0257(12) 0.0287(12) 0.0359(13) -0.0055(10) 0.0040(10) -0.0119(10) C26 0.0244(12) 0.0360(14) 0.0307(13) -0.0051(11) 0.0006(10) -0.0116(11) C27 0.0347(14) 0.0393(15) 0.0364(14) -0.0118(12) 0.0032(11) -0.0099(12) C28 0.0249(12) 0.0227(11) 0.0267(12) -0.0040(9) 0.0014(9) -0.0074(9) C29 0.0212(11) 0.0208(11) 0.0265(12) -0.0018(9) -0.0014(9) -0.0044(9) C30 0.0247(12) 0.0206(11) 0.0282(12) -0.0027(9) -0.0018(9) -0.0090(9) C31 0.0227(11) 0.0219(11) 0.0271(12) -0.0032(9) -0.0027(9) -0.0059(9) C32 0.0245(12) 0.0242(11) 0.0257(12) -0.0014(9) -0.0001(9) -0.0101(9) C33 0.0242(12) 0.0226(11) 0.0276(12) -0.0027(9) -0.0033(9) -0.0074(9) C34 0.0248(12) 0.0234(11) 0.0251(12) -0.0044(9) -0.0018(9) -0.0070(9) C35 0.0403(14) 0.0324(13) 0.0309(13) -0.0051(11) -0.0002(11) -0.0219(12) C36 0.100(3) 0.138(3) 0.167(3) -0.105(3) 0.061(2) -0.090(2) C37 0.177(3) 0.064(2) 0.143(3) 0.024(2) -0.095(3) -0.073(2) C38 0.112(3) 0.079(2) 0.0537(18) -0.0230(16) 0.0134(17) -0.073(2) C39 0.0285(13) 0.0351(14) 0.0374(14) -0.0082(11) -0.0017(10) -0.0151(11) C40 0.0315(15) 0.0501(17) 0.0472(16) -0.0097(14) -0.0018(12) -0.0171(13) C41 0.0339(17) 0.111(3) 0.061(2) -0.020(2) 0.0083(16) -0.0259(19) C42 0.0285(12) 0.0241(12) 0.0261(12) -0.0032(9) -0.0012(9) -0.0101(10) C43 0.0275(12) 0.0239(12) 0.0214(11) -0.0039(9) 0.0006(9) -0.0091(10) C44 0.0242(12) 0.0291(12) 0.0210(11) -0.0057(9) 0.0002(9) -0.0108(10) C45 0.0278(12) 0.0255(12) 0.0208(11) -0.0054(9) 0.0002(9) -0.0105(10) C46 0.0283(12) 0.0262(12) 0.0247(12) -0.0032(9) -0.0016(9) -0.0084(10) C47 0.0296(13) 0.0325(13) 0.0221(11) -0.0031(10) -0.0007(9) -0.0146(10) C48 0.0317(13) 0.0270(12) 0.0237(11) -0.0042(9) 0.0000(9) -0.0147(10) C49 0.0304(13) 0.0339(14) 0.0392(15) -0.0021(11) -0.0088(11) -0.0139(11) C50 0.0444(18) 0.097(3) 0.0454(18) -0.0178(18) -0.0150(14) -0.0183(18) C51 0.0274(15) 0.063(2) 0.075(2) -0.0255(18) -0.0007(14) -0.0147(14) C52 0.0525(18) 0.062(2) 0.103(2) 0.0142(18) -0.0302(17) -0.0354(16) C53 0.0318(13) 0.0415(15) 0.0278(13) -0.0108(11) -0.0038(10) -0.0120(11) C54 0.0357(15) 0.0311(14) 0.0371(14) -0.0071(11) -0.0080(11) -0.0091(11) C55 0.0389(16) 0.0470(17) 0.0568(19) -0.0114(14) -0.0152(14) -0.0142(13) C56 0.0287(12) 0.0254(12) 0.0265(12) -0.0061(10) -0.0024(9) -0.0097(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 O1 C2 1.387(3) . ? O1 C11 1.428(3) . ? O2 C16 1.397(3) . ? O2 C25 1.429(3) . ? O3 C30 1.388(3) . ? O3 C39 1.436(3) . ? O4 C44 1.399(3) . ? O4 C53 1.430(3) . ? C1 C6 1.391(3) . ? C1 C2 1.398(3) . ? C1 C56 1.517(3) . ? C2 C3 1.396(3) . ? C3 C4 1.392(3) . ? C3 C14 1.520(3) . ? C4 C5 1.398(3) . ? C4 H4 0.9300 . ? C5 C6 1.397(3) . ? C5 C7 1.534(3) . ? C6 H6 0.9300 . ? C7 C8B 1.471(7) . ? C7 C9B 1.473(7) . ? C7 C8A 1.480(5) . ? C7 C10A 1.485(5) . ? C7 C9A 1.594(4) . ? C7 C10B 1.599(5) . ? C8A H8A1 0.9600 . ? C8A H8A2 0.9600 . ? C8A H8A3 0.9600 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C8B H8B1 0.9600 . ? C8B H8B2 0.9600 . ? C8B H8B3 0.9600 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? C11 C12 1.465(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.180(4) . ? C13 H13 0.9300 . ? C14 C15 1.521(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.395(3) . ? C15 C16 1.395(3) . ? C16 C17 1.399(3) . ? C17 C18 1.390(3) . ? C17 C28 1.525(3) . ? C18 C19 1.399(3) . ? C18 H18 0.9300 . ? C19 C20 1.392(3) . ? C19 C21 1.537(3) . ? C20 H20 0.9300 . ? C21 C23 1.534(4) . ? C21 C24 1.535(3) . ? C21 C22 1.538(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.469(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.185(4) . ? C27 H27 0.9300 . ? C28 C29 1.515(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.395(3) . ? C29 C30 1.396(3) . ? C30 C31 1.399(3) . ? C31 C32 1.399(3) . ? C31 C42 1.521(3) . ? C32 C33 1.395(3) . ? C32 H32 0.9300 . ? C33 C34 1.393(3) . ? C33 C35 1.537(3) . ? C34 H34 0.9300 . ? C35 C36 1.482(5) . ? C35 C37 1.492(5) . ? C35 C38 1.496(4) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.463(4) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.171(4) . ? C41 H41 0.9300 . ? C42 C43 1.522(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.392(3) . ? C43 C48 1.398(3) . ? C44 C45 1.395(3) . ? C45 C46 1.386(3) . ? C45 C56 1.525(3) . ? C46 C47 1.392(3) . ? C46 H46 0.9300 . ? C47 C48 1.392(3) . ? C47 C49 1.531(3) . ? C48 H48 0.9300 . ? C49 C52 1.520(4) . ? C49 C51 1.520(4) . ? C49 C50 1.526(4) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.458(4) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.179(4) . ? C55 H55 0.9300 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? 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 O1 C11 117.08(19) . . ? C16 O2 C25 114.76(17) . . ? C30 O3 C39 114.16(18) . . ? C44 O4 C53 110.99(17) . . ? C6 C1 C2 118.0(2) . . ? C6 C1 C56 120.7(2) . . ? C2 C1 C56 120.3(2) . . ? O1 C2 C3 118.1(2) . . ? O1 C2 C1 120.1(2) . . ? C3 C2 C1 121.3(2) . . ? C4 C3 C2 118.5(2) . . ? C4 C3 C14 121.1(2) . . ? C2 C3 C14 120.3(2) . . ? C3 C4 C5 122.3(2) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 117.1(2) . . ? C6 C5 C7 120.9(2) . . ? C4 C5 C7 122.0(2) . . ? C1 C6 C5 122.7(2) . . ? C1 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C8B C7 C9B 114.9(4) . . ? C8A C7 C10A 113.9(3) . . ? C8B C7 C5 113.5(3) . . ? C9B C7 C5 116.1(3) . . ? C8A C7 C5 113.6(3) . . ? C10A C7 C5 110.1(3) . . ? C8A C7 C9A 105.8(3) . . ? C10A C7 C9A 107.5(3) . . ? C5 C7 C9A 105.4(2) . . ? C8B C7 C10B 103.3(5) . . ? C9B C7 C10B 102.4(5) . . ? C5 C7 C10B 104.3(3) . . ? C7 C8A H8A1 109.5 . . ? C7 C8A H8A2 109.5 . . ? C7 C8A H8A3 109.5 . . ? C7 C9A H9A1 109.5 . . ? C7 C9A H9A2 109.5 . . ? C7 C9A H9A3 109.5 . . ? C7 C10A H10A 109.5 . . ? C7 C10A H10B 109.5 . . ? C7 C10A H10C 109.5 . . ? C7 C8B H8B1 109.5 . . ? C7 C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7 C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7 C9B H9B1 109.5 . . ? C7 C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7 C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7 C10B H10D 109.5 . . ? C7 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? O1 C11 C12 114.6(2) . . ? O1 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? O1 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 177.6(3) . . ? C12 C13 H13 180.0 . . ? C3 C14 C15 112.68(19) . . ? C3 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? C3 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C20 C15 C16 118.9(2) . . ? C20 C15 C14 119.0(2) . . ? C16 C15 C14 122.1(2) . . ? C15 C16 O2 120.2(2) . . ? C15 C16 C17 120.6(2) . . ? O2 C16 C17 119.14(19) . . ? C18 C17 C16 118.3(2) . . ? C18 C17 C28 119.6(2) . . ? C16 C17 C28 121.9(2) . . ? C17 C18 C19 122.9(2) . . ? C17 C18 H18 118.6 . . ? C19 C18 H18 118.6 . . ? C20 C19 C18 116.7(2) . . ? C20 C19 C21 123.4(2) . . ? C18 C19 C21 119.9(2) . . ? C19 C20 C15 122.3(2) . . ? C19 C20 H20 118.8 . . ? C15 C20 H20 118.8 . . ? C23 C21 C24 108.2(2) . . ? C23 C21 C19 112.2(2) . . ? C24 C21 C19 110.8(2) . . ? C23 C21 C22 108.3(2) . . ? C24 C21 C22 109.1(2) . . ? C19 C21 C22 108.2(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 C26 114.2(2) . . ? O2 C25 H25A 108.7 . . ? C26 C25 H25A 108.7 . . ? O2 C25 H25B 108.7 . . ? C26 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C27 C26 C25 177.9(3) . . ? C26 C27 H27 180.0 . . ? C29 C28 C17 108.97(18) . . ? C29 C28 H28A 109.9 . . ? C17 C28 H28A 109.9 . . ? C29 C28 H28B 109.9 . . ? C17 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C34 C29 C30 118.1(2) . . ? C34 C29 C28 120.8(2) . . ? C30 C29 C28 120.8(2) . . ? O3 C30 C29 119.4(2) . . ? O3 C30 C31 119.2(2) . . ? C29 C30 C31 121.2(2) . . ? C30 C31 C32 118.3(2) . . ? C30 C31 C42 120.3(2) . . ? C32 C31 C42 121.3(2) . . ? C33 C32 C31 122.2(2) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C34 C33 C32 117.3(2) . . ? C34 C33 C35 121.8(2) . . ? C32 C33 C35 120.9(2) . . ? C33 C34 C29 122.7(2) . . ? C33 C34 H34 118.7 . . ? C29 C34 H34 118.7 . . ? C36 C35 C37 108.3(4) . . ? C36 C35 C38 106.8(3) . . ? C37 C35 C38 108.8(3) . . ? C36 C35 C33 110.5(2) . . ? C37 C35 C33 109.1(2) . . ? C38 C35 C33 113.2(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O3 C39 C40 112.7(2) . . ? O3 C39 H39A 109.1 . . ? C40 C39 H39A 109.1 . . ? O3 C39 H39B 109.1 . . ? C40 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C39 177.7(4) . . ? C40 C41 H41 180.0 . . ? C31 C42 C43 111.41(19) . . ? C31 C42 H42A 109.3 . . ? C43 C42 H42A 109.3 . . ? C31 C42 H42B 109.3 . . ? C43 C42 H42B 109.3 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C48 118.4(2) . . ? C44 C43 C42 122.4(2) . . ? C48 C43 C42 119.1(2) . . ? C43 C44 C45 121.0(2) . . ? C43 C44 O4 119.8(2) . . ? C45 C44 O4 119.2(2) . . ? C46 C45 C44 118.4(2) . . ? C46 C45 C56 118.8(2) . . ? C44 C45 C56 122.5(2) . . ? C45 C46 C47 122.7(2) . . ? C45 C46 H46 118.6 . . ? C47 C46 H46 118.6 . . ? C46 C47 C48 117.1(2) . . ? C46 C47 C49 119.6(2) . . ? C48 C47 C49 123.0(2) . . ? C47 C48 C43 122.2(2) . . ? C47 C48 H48 118.9 . . ? C43 C48 H48 118.9 . . ? C52 C49 C51 107.9(3) . . ? C52 C49 C50 109.4(3) . . ? C51 C49 C50 109.3(3) . . ? C52 C49 C47 111.7(2) . . ? C51 C49 C47 111.8(2) . . ? C50 C49 C47 106.7(2) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O4 C53 C54 110.0(2) . . ? O4 C53 H53A 109.7 . . ? C54 C53 H53A 109.7 . . ? O4 C53 H53B 109.7 . . ? C54 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C55 C54 C53 175.9(3) . . ? C54 C55 H55 180.0 . . ? C1 C56 C45 108.11(18) . . ? C1 C56 H56A 110.1 . . ? C45 C56 H56A 110.1 . . ? C1 C56 H56B 110.1 . . ? C45 C56 H56B 110.1 . . ? H56A C56 H56B 108.4 . . ? #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 711452' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H64 O4' _chemical_formula_weight 801.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.2796(16) _cell_length_b 20.2796(16) _cell_length_c 11.3604(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4672.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 35199 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.68 _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type none _exptl_special_details 'crystal-to-detector distance 30 mm' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD area-detector diffractometer' _diffrn_measurement_method 'two \f scans with 2\% steps' _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35199 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2210 _reflns_number_gt 1627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)' _refine_special_details ; Structure solved by direct methods and subsequent Fourier-difference synthesis. All non-hydrogen atoms were refined with anisotropic displacement parameters. The H atoms were introduced at calculated positions and were treated as riding atoms with an isotropic displacement parameter equal to 1.2 (CH, CH~2~) or 1.5 (CH~3~) times that of the parent atom. 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^)+(0.1077P)^2^+2.9154P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2210 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.211 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.127 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 O1 O 0.58115(8) 0.67312(8) 0.00825(13) 0.0308(4) Uani 1 1 d . . . C1 C 0.63629(10) 0.69636(11) 0.19440(19) 0.0260(5) Uani 1 1 d . . . C2 C 0.59185(11) 0.65948(11) 0.12656(18) 0.0255(5) Uani 1 1 d . . . C3 C 0.55346(10) 0.60963(11) 0.17771(19) 0.0258(5) Uani 1 1 d . . . C4 C 0.56355(11) 0.59413(11) 0.29535(19) 0.0267(5) Uani 1 1 d . . . H4 H 0.5392 0.5601 0.3287 0.032 Uiso 1 1 calc R . . C5 C 0.60877(11) 0.62773(11) 0.36523(19) 0.0277(5) Uani 1 1 d . . . C6 C 0.64329(11) 0.67928(11) 0.31237(19) 0.0283(5) Uani 1 1 d . . . H6 H 0.6725 0.7035 0.3583 0.034 Uiso 1 1 calc R . . C7 C 0.62081(14) 0.61063(13) 0.4950(2) 0.0396(7) Uani 1 1 d . . . C8 C 0.6070(3) 0.67165(16) 0.5697(2) 0.0818(14) Uani 1 1 d . . . H8A H 0.6377 0.7058 0.5496 0.123 Uiso 1 1 calc R . . H8B H 0.6116 0.6607 0.6515 0.123 Uiso 1 1 calc R . . H8C H 0.5629 0.6868 0.5550 0.123 Uiso 1 1 calc R . . C9 C 0.69265(15) 0.58761(19) 0.5096(3) 0.0654(11) Uani 1 1 d . . . H9A H 0.7007 0.5506 0.4590 0.098 Uiso 1 1 calc R . . H9B H 0.7001 0.5750 0.5899 0.098 Uiso 1 1 calc R . . H9C H 0.7220 0.6230 0.4890 0.098 Uiso 1 1 calc R . . C10 C 0.57613(14) 0.55515(13) 0.5387(2) 0.0397(6) Uani 1 1 d . . . H10A H 0.5308 0.5680 0.5296 0.060 Uiso 1 1 calc R . . H10B H 0.5851 0.5467 0.6203 0.060 Uiso 1 1 calc R . . H10C H 0.5844 0.5160 0.4937 0.060 Uiso 1 1 calc R . . C11 C 0.63309(14) 0.65346(12) -0.0691(2) 0.0386(6) Uani 1 1 d . . . H11A H 0.6739 0.6731 -0.0418 0.046 Uiso 1 1 calc R . . H11B H 0.6241 0.6710 -0.1469 0.046 Uiso 1 1 calc R . . C12 C 0.64245(13) 0.58165(13) -0.0786(2) 0.0379(6) Uani 1 1 d . . . C13 C 0.65384(14) 0.52498(14) -0.0877(3) 0.0485(7) Uani 1 1 d . . . H13 H 0.6628 0.4802 -0.0949 0.058 Uiso 1 1 calc R . . C14 C 0.50311(11) 0.57299(11) 0.1047(2) 0.0279(5) Uani 1 1 d . . . H14A H 0.4847 0.5380 0.1526 0.033 Uiso 1 1 calc R . . H14B H 0.5258 0.5524 0.0392 0.033 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 O1 0.0359(10) 0.0312(9) 0.0252(9) 0.0011(6) -0.0016(6) 0.0013(7) C1 0.0229(11) 0.0259(12) 0.0293(12) 0.0007(9) 0.0002(8) 0.0027(9) C2 0.0263(12) 0.0262(11) 0.0239(11) 0.0008(8) -0.0014(8) 0.0039(9) C3 0.0232(11) 0.0249(11) 0.0293(12) -0.0026(8) -0.0012(8) 0.0040(9) C4 0.0256(11) 0.0243(11) 0.0302(12) 0.0005(9) 0.0013(9) 0.0005(9) C5 0.0285(12) 0.0290(12) 0.0255(12) -0.0011(9) 0.0010(9) 0.0018(10) C6 0.0260(12) 0.0299(12) 0.0290(12) -0.0018(9) -0.0033(9) -0.0035(9) C7 0.0509(17) 0.0410(15) 0.0270(13) 0.0035(10) -0.0057(11) -0.0140(12) C8 0.166(4) 0.052(2) 0.0275(15) -0.0081(13) 0.0162(19) -0.041(2) C9 0.0506(19) 0.089(3) 0.0568(19) 0.0375(17) -0.0257(15) -0.0258(18) C10 0.0489(16) 0.0417(15) 0.0286(12) 0.0063(10) 0.0005(11) -0.0075(12) C11 0.0529(16) 0.0366(14) 0.0262(12) -0.0011(10) 0.0088(11) -0.0042(12) C12 0.0387(14) 0.0420(16) 0.0329(13) -0.0070(11) 0.0037(10) -0.0065(11) C13 0.0415(16) 0.0378(16) 0.0663(19) -0.0153(13) 0.0090(13) -0.0066(12) C14 0.0280(12) 0.0242(12) 0.0315(12) -0.0001(9) -0.0010(9) -0.0005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.389(3) . ? O1 C11 1.428(3) . ? C1 C6 1.391(3) . ? C1 C2 1.402(3) . ? C1 C14 1.522(3) 12_766 ? C2 C3 1.402(3) . ? C3 C4 1.388(3) . ? C3 C14 1.511(3) . ? C4 C5 1.391(3) . ? C4 H4 0.9300 . ? C5 C6 1.394(3) . ? C5 C7 1.534(3) . ? C6 H6 0.9300 . ? C7 C8 1.527(4) . ? C7 C10 1.528(3) . ? C7 C9 1.539(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.473(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.177(4) . ? C13 H13 0.9300 . ? C14 C1 1.522(3) 15_565 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? 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 O1 C11 115.10(17) . . ? C6 C1 C2 117.5(2) . . ? C6 C1 C14 119.05(19) . 12_766 ? C2 C1 C14 123.42(19) . 12_766 ? O1 C2 C1 121.74(19) . . ? O1 C2 C3 117.24(19) . . ? C1 C2 C3 120.92(19) . . ? C4 C3 C2 118.7(2) . . ? C4 C3 C14 121.1(2) . . ? C2 C3 C14 120.16(19) . . ? C3 C4 C5 122.4(2) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C4 C5 C6 116.9(2) . . ? C4 C5 C7 122.9(2) . . ? C6 C5 C7 120.2(2) . . ? C1 C6 C5 123.4(2) . . ? C1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? C8 C7 C10 107.9(2) . . ? C8 C7 C5 108.8(2) . . ? C10 C7 C5 112.6(2) . . ? C8 C7 C9 111.1(3) . . ? C10 C7 C9 107.6(2) . . ? C5 C7 C9 108.9(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 114.6(2) . . ? O1 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? O1 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 176.0(3) . . ? C12 C13 H13 180.0 . . ? C3 C14 C1 116.44(18) . 15_565 ? C3 C14 H14A 108.2 . . ? C1 C14 H14A 108.2 15_565 . ? C3 C14 H14B 108.2 . . ? C1 C14 H14B 108.2 15_565 . ? H14A C14 H14B 107.3 . . ? #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 711453' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H60 Co4 O16' _chemical_formula_sum 'C62 H60 Co4 O16' _chemical_formula_weight 1296.82 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.5746(3) _cell_length_b 25.3144(4) _cell_length_c 20.2062(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.9700(10) _cell_angle_gamma 90.00 _cell_volume 6324.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 36254 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 29.131 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67564 _exptl_absorpt_correction_T_max 0.80804 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47386 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 29.13 _reflns_number_total 16873 _reflns_number_gt 9099 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1021P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16873 _refine_ls_number_parameters 735 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1315 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.2000 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 C1 C 0.3604(3) -0.29559(13) 0.7873(2) 0.0317(8) Uani 1 1 d . . . C2 C 0.3875(3) -0.24231(13) 0.80106(18) 0.0283(7) Uani 1 1 d . . . C3 C 0.4938(3) -0.22596(13) 0.85114(18) 0.0304(8) Uani 1 1 d . . . C4 C 0.5720(3) -0.26495(14) 0.8896(2) 0.0370(9) Uani 1 1 d . . . H4 H 0.6448 -0.2544 0.9246 0.044 Uiso 1 1 calc R . . C5 C 0.5484(3) -0.31845(14) 0.8792(2) 0.0407(9) Uani 1 1 d . A . C6 C 0.4417(3) -0.33284(14) 0.8267(2) 0.0395(9) Uani 1 1 d . . . H6 H 0.4238 -0.3693 0.8175 0.047 Uiso 1 1 calc R . . C7 C 0.6358(3) -0.36024(16) 0.9188(3) 0.0532(11) Uani 1 1 d . . . C8 C 0.6024(11) -0.4025(6) 0.9627(9) 0.0834(18) Uani 0.50 1 d P A 1 H8A H 0.5376 -0.4218 0.9239 0.125 Uiso 0.50 1 calc PR A 1 H8B H 0.5875 -0.3839 0.9985 0.125 Uiso 0.50 1 calc PR A 1 H8C H 0.6619 -0.4275 0.9922 0.125 Uiso 0.50 1 calc PR A 1 C9 C 0.7454(9) -0.3352(5) 0.9945(7) 0.0834(18) Uani 0.50 1 d P A 1 H9A H 0.7946 -0.3638 1.0258 0.125 Uiso 0.50 1 calc PR A 1 H9B H 0.7256 -0.3149 1.0263 0.125 Uiso 0.50 1 calc PR A 1 H9C H 0.7815 -0.3119 0.9763 0.125 Uiso 0.50 1 calc PR A 1 C10 C 0.6549(10) -0.3851(5) 0.8633(8) 0.0834(18) Uani 0.50 1 d P A 1 H10A H 0.6984 -0.4170 0.8864 0.125 Uiso 0.50 1 calc PR A 1 H10B H 0.6938 -0.3606 0.8491 0.125 Uiso 0.50 1 calc PR A 1 H10C H 0.5856 -0.3946 0.8165 0.125 Uiso 0.50 1 calc PR A 1 C8B C 0.6327(12) -0.3873(6) 0.9823(9) 0.0834(18) Uani 0.50 1 d P A 2 H8B1 H 0.5609 -0.4028 0.9617 0.125 Uiso 0.50 1 calc PR A 2 H8B2 H 0.6475 -0.3617 1.0232 0.125 Uiso 0.50 1 calc PR A 2 H8B3 H 0.6875 -0.4152 1.0042 0.125 Uiso 0.50 1 calc PR A 2 C9B C 0.7472(9) -0.3401(5) 0.9438(7) 0.0834(18) Uani 0.50 1 d P A 2 H9B1 H 0.8018 -0.3656 0.9793 0.125 Uiso 0.50 1 calc PR A 2 H9B2 H 0.7597 -0.3061 0.9705 0.125 Uiso 0.50 1 calc PR A 2 H9B3 H 0.7524 -0.3355 0.8977 0.125 Uiso 0.50 1 calc PR A 2 C10B C 0.6100(10) -0.4087(5) 0.8595(8) 0.0834(18) Uani 0.50 1 d P A 2 H10D H 0.5817 -0.3948 0.8068 0.125 Uiso 0.50 1 calc PR A 2 H10E H 0.5561 -0.4320 0.8592 0.125 Uiso 0.50 1 calc PR A 2 H10F H 0.6765 -0.4286 0.8764 0.125 Uiso 0.50 1 calc PR A 2 C11 C 0.5280(3) -0.16822(14) 0.8599(2) 0.0352(8) Uani 1 1 d . . . H11A H 0.4647 -0.1458 0.8251 0.042 Uiso 1 1 calc R . . H11B H 0.5582 -0.1565 0.9144 0.042 Uiso 1 1 calc R . . C12 C 0.6127(3) -0.16315(13) 0.8384(2) 0.0315(8) Uani 1 1 d . . . C13 C 0.5818(3) -0.16547(13) 0.76078(19) 0.0311(8) Uani 1 1 d . . . C14 C 0.6590(3) -0.16785(13) 0.7403(2) 0.0336(8) Uani 1 1 d . . . C15 C 0.7678(3) -0.16751(14) 0.7998(2) 0.0383(9) Uani 1 1 d . . . H15 H 0.8205 -0.1693 0.7859 0.046 Uiso 1 1 calc R . . C16 C 0.8026(3) -0.16480(14) 0.8774(2) 0.0392(9) Uani 1 1 d . B . C17 C 0.7220(3) -0.16251(13) 0.8956(2) 0.0360(8) Uani 1 1 d . . . H17 H 0.7431 -0.1605 0.9488 0.043 Uiso 1 1 calc R . . C18 C 0.9237(3) -0.16725(18) 0.9417(2) 0.0513(11) Uani 1 1 d . . . C19 C 0.9453(10) -0.1759(5) 1.0215(9) 0.0717(16) Uani 0.50 1 d P B 1 H19A H 1.0235 -0.1773 1.0589 0.108 Uiso 0.50 1 calc PR B 1 H19B H 0.9123 -0.2093 1.0229 0.108 Uiso 0.50 1 calc PR B 1 H19C H 0.9142 -0.1467 1.0353 0.108 Uiso 0.50 1 calc PR B 1 C20 C 0.9731(11) -0.1110(6) 0.9323(11) 0.0717(16) Uani 0.50 1 d P B 1 H20A H 1.0520 -0.1112 0.9670 0.108 Uiso 0.50 1 calc PR B 1 H20B H 0.9429 -0.0816 0.9463 0.108 Uiso 0.50 1 calc PR B 1 H20C H 0.9537 -0.1070 0.8782 0.108 Uiso 0.50 1 calc PR B 1 C21 C 0.9821(8) -0.2102(5) 0.9198(7) 0.0717(16) Uani 0.50 1 d P B 1 H21A H 0.9810 -0.1988 0.8730 0.108 Uiso 0.50 1 calc PR B 1 H21B H 0.9442 -0.2440 0.9096 0.108 Uiso 0.50 1 calc PR B 1 H21C H 1.0571 -0.2142 0.9632 0.108 Uiso 0.50 1 calc PR B 1 C19B C 0.9439(10) -0.1529(5) 1.0221(9) 0.0717(16) Uani 0.50 1 d P B 2 H19D H 1.0189 -0.1612 1.0624 0.108 Uiso 0.50 1 calc PR B 2 H19E H 0.8947 -0.1732 1.0316 0.108 Uiso 0.50 1 calc PR B 2 H19F H 0.9308 -0.1150 1.0235 0.108 Uiso 0.50 1 calc PR B 2 C20B C 0.9860(11) -0.1273(6) 0.9309(11) 0.0717(16) Uani 0.50 1 d P B 2 H20D H 0.9383 -0.0982 0.8997 0.108 Uiso 0.50 1 calc PR B 2 H20E H 1.0187 -0.1429 0.9037 0.108 Uiso 0.50 1 calc PR B 2 H20F H 1.0431 -0.1140 0.9818 0.108 Uiso 0.50 1 calc PR B 2 C21B C 0.9621(8) -0.2223(5) 0.9452(7) 0.0717(16) Uani 0.50 1 d P B 2 H21D H 0.9382 -0.2344 0.8924 0.108 Uiso 0.50 1 calc PR B 2 H21E H 0.9320 -0.2455 0.9679 0.108 Uiso 0.50 1 calc PR B 2 H21F H 1.0412 -0.2232 0.9776 0.108 Uiso 0.50 1 calc PR B 2 C22 C 0.6272(3) -0.17284(14) 0.6551(2) 0.0361(8) Uani 1 1 d . . . H22A H 0.5691 -0.1472 0.6228 0.043 Uiso 1 1 calc R . . H22B H 0.6904 -0.1640 0.6512 0.043 Uiso 1 1 calc R . . C23 C 0.5882(3) -0.22838(13) 0.62303(19) 0.0316(8) Uani 1 1 d . . . C24 C 0.4793(3) -0.24054(14) 0.57546(19) 0.0317(8) Uani 1 1 d . . . C25 C 0.4426(3) -0.29149(14) 0.55157(18) 0.0317(8) Uani 1 1 d . . . C26 C 0.5193(3) -0.33076(14) 0.57412(19) 0.0349(8) Uani 1 1 d . . . H26 H 0.4956 -0.3659 0.5571 0.042 Uiso 1 1 calc R . . C27 C 0.6292(3) -0.32125(14) 0.62036(19) 0.0341(8) Uani 1 1 d . C . C28 C 0.6618(3) -0.26922(14) 0.6444(2) 0.0346(8) Uani 1 1 d . . . H28 H 0.7368 -0.2616 0.6764 0.041 Uiso 1 1 calc R . . C29 C 0.7112(3) -0.36707(15) 0.6466(2) 0.0396(9) Uani 1 1 d . . . C30 C 0.8226(9) -0.3515(4) 0.7196(7) 0.0714(14) Uani 0.50 1 d P C 1 H30A H 0.8718 -0.3818 0.7363 0.107 Uiso 0.50 1 calc PR C 1 H30B H 0.8126 -0.3409 0.7620 0.107 Uiso 0.50 1 calc PR C 1 H30C H 0.8535 -0.3220 0.7064 0.107 Uiso 0.50 1 calc PR C 1 C31 C 0.7114(9) -0.3886(4) 0.5796(7) 0.0714(14) Uani 0.50 1 d P C 1 H31A H 0.7492 -0.3642 0.5643 0.107 Uiso 0.50 1 calc PR C 1 H31B H 0.6367 -0.3933 0.5359 0.107 Uiso 0.50 1 calc PR C 1 H31C H 0.7484 -0.4229 0.5936 0.107 Uiso 0.50 1 calc PR C 1 C32 C 0.6739(9) -0.4131(5) 0.6792(7) 0.0714(14) Uani 0.50 1 d P C 1 H32A H 0.7301 -0.4404 0.7022 0.107 Uiso 0.50 1 calc PR C 1 H32B H 0.6066 -0.4284 0.6366 0.107 Uiso 0.50 1 calc PR C 1 H32C H 0.6618 -0.3992 0.7192 0.107 Uiso 0.50 1 calc PR C 1 C30B C 0.8247(9) -0.3511(4) 0.6795(7) 0.0714(14) Uani 0.50 1 d P C 2 H30D H 0.8715 -0.3823 0.6992 0.107 Uiso 0.50 1 calc PR C 2 H30E H 0.8462 -0.3261 0.7224 0.107 Uiso 0.50 1 calc PR C 2 H30F H 0.8319 -0.3342 0.6388 0.107 Uiso 0.50 1 calc PR C 2 C31B C 0.6753(9) -0.4084(4) 0.5771(7) 0.0714(14) Uani 0.50 1 d P C 2 H31D H 0.6540 -0.3892 0.5289 0.107 Uiso 0.50 1 calc PR C 2 H31E H 0.6141 -0.4293 0.5697 0.107 Uiso 0.50 1 calc PR C 2 H31F H 0.7360 -0.4319 0.5901 0.107 Uiso 0.50 1 calc PR C 2 C32B C 0.7056(9) -0.3991(5) 0.7083(7) 0.0714(14) Uani 0.50 1 d P C 2 H32D H 0.7484 -0.4315 0.7196 0.107 Uiso 0.50 1 calc PR C 2 H32E H 0.6302 -0.4084 0.6889 0.107 Uiso 0.50 1 calc PR C 2 H32F H 0.7348 -0.3781 0.7560 0.107 Uiso 0.50 1 calc PR C 2 C33 C 0.3230(3) -0.30621(15) 0.50771(19) 0.0388(9) Uani 1 1 d . . . H33A H 0.2789 -0.2736 0.4896 0.047 Uiso 1 1 calc R . . H33B H 0.3051 -0.3274 0.4612 0.047 Uiso 1 1 calc R . . C34 C 0.2941(3) -0.33753(13) 0.55815(18) 0.0306(8) Uani 1 1 d . . . C35 C 0.2750(2) -0.31223(13) 0.61067(19) 0.0305(8) Uani 1 1 d . . . C36 C 0.2560(3) -0.34141(13) 0.6607(2) 0.0317(8) Uani 1 1 d . . . C37 C 0.2569(3) -0.39604(13) 0.6570(2) 0.0334(8) Uani 1 1 d . . . H37 H 0.2438 -0.4159 0.6910 0.040 Uiso 1 1 calc R . . C38 C 0.2764(3) -0.42310(13) 0.6055(2) 0.0328(8) Uani 1 1 d . . . C39 C 0.2946(3) -0.39235(14) 0.55652(19) 0.0343(8) Uani 1 1 d . . . H39 H 0.3078 -0.4095 0.5206 0.041 Uiso 1 1 calc R . . C40 C 0.2823(3) -0.48390(15) 0.6040(2) 0.0471(10) Uani 1 1 d . . . C41 C 0.3955(4) -0.50022(18) 0.6235(4) 0.0813(17) Uani 1 1 d . . . H41A H 0.4104 -0.4838 0.5862 0.122 Uiso 1 1 calc R . . H41B H 0.3987 -0.5387 0.6202 0.122 Uiso 1 1 calc R . . H41C H 0.4497 -0.4886 0.6764 0.122 Uiso 1 1 calc R . . C42 C 0.1990(5) -0.50414(18) 0.5221(3) 0.0805(17) Uani 1 1 d . . . H42A H 0.1263 -0.4935 0.5083 0.121 Uiso 1 1 calc R . . H42B H 0.2028 -0.5428 0.5212 0.121 Uiso 1 1 calc R . . H42C H 0.2146 -0.4891 0.4843 0.121 Uiso 1 1 calc R . . C43 C 0.2620(4) -0.51037(16) 0.6626(3) 0.0672(14) Uani 1 1 d . . . H43A H 0.3135 -0.4968 0.7150 0.101 Uiso 1 1 calc R . . H43B H 0.2713 -0.5486 0.6616 0.101 Uiso 1 1 calc R . . H43C H 0.1881 -0.5027 0.6490 0.101 Uiso 1 1 calc R . . C44 C 0.2476(3) -0.31414(15) 0.7234(2) 0.0386(9) Uani 1 1 d . . . H44A H 0.2181 -0.3388 0.7456 0.046 Uiso 1 1 calc R . . H44B H 0.1982 -0.2835 0.7011 0.046 Uiso 1 1 calc R . . C45 C 0.2643(3) -0.19558(14) 0.8144(2) 0.0351(8) Uani 1 1 d . . . H45A H 0.3257 -0.1889 0.8681 0.042 Uiso 1 1 calc R . . H45B H 0.2273 -0.2281 0.8154 0.042 Uiso 1 1 calc R . . C46 C 0.1881(3) -0.15091(13) 0.78956(19) 0.0312(8) Uani 1 1 d . . . C47 C 0.1306(3) -0.12756(14) 0.8157(2) 0.0341(8) Uani 1 1 d . . . H47 H 0.1196 -0.1329 0.8600 0.041 Uiso 1 1 calc R . . C48 C -0.0237(4) -0.19382(19) 0.6873(3) 0.0732(16) Uani 1 1 d . . . C49 C -0.0693(4) -0.09016(19) 0.6796(3) 0.0615(13) Uani 1 1 d . . . C50 C 0.0493(4) -0.1348(2) 0.6178(3) 0.0721(15) Uani 1 1 d . . . C51 C 0.3239(4) -0.06267(16) 0.8738(2) 0.0477(10) Uani 1 1 d . . . C52 C 0.2372(5) -0.0615(2) 0.7182(3) 0.0806(17) Uani 1 1 d . . . C53 C 0.1225(4) -0.01897(18) 0.7830(4) 0.0787(18) Uani 1 1 d . . . C54 C 0.3683(3) -0.17359(14) 0.48446(19) 0.0336(8) Uani 1 1 d . . . H54A H 0.3350 -0.1990 0.4406 0.040 Uiso 1 1 calc R . . H54B H 0.4306 -0.1566 0.4861 0.040 Uiso 1 1 calc R . . C55 C 0.2873(3) -0.13283(13) 0.47453(19) 0.0316(8) Uani 1 1 d . . . C56 C 0.2287(3) -0.12450(14) 0.5064(2) 0.0362(8) Uani 1 1 d . . . H56 H 0.2205 -0.1415 0.5476 0.043 Uiso 1 1 calc R . . C57 C 0.0979(4) -0.1794(2) 0.3578(3) 0.0640(13) Uani 1 1 d . . . C58 C 0.0191(4) -0.0876(2) 0.3896(3) 0.0646(13) Uani 1 1 d . . . C59 C 0.1384(4) -0.0846(2) 0.3124(3) 0.0630(14) Uani 1 1 d . . . C60 C 0.1924(4) -0.00927(18) 0.4955(3) 0.0582(12) Uani 1 1 d . . . C61 C 0.3382(4) -0.02793(19) 0.4402(3) 0.0641(13) Uani 1 1 d . . . C62 C 0.3998(4) -0.04954(17) 0.5905(3) 0.0577(12) Uani 1 1 d . . . Co1 Co 0.04232(4) -0.13323(2) 0.70221(3) 0.03800(15) Uani 1 1 d . . . Co2 Co 0.19647(4) -0.074014(19) 0.78467(3) 0.03806(15) Uani 1 1 d . . . Co3 Co 0.13878(4) -0.11419(2) 0.39388(3) 0.04236(16) Uani 1 1 d . . . Co4 Co 0.28373(4) -0.05761(2) 0.49308(3) 0.04181(16) Uani 1 1 d . . . O1 O 0.30570(17) -0.20426(8) 0.76475(12) 0.0288(5) Uani 1 1 d . . . O2 O 0.47198(18) -0.16569(10) 0.70738(13) 0.0368(6) Uani 1 1 d . . . H2O H 0.4598 -0.1767 0.6642 0.044 Uiso 1 1 calc R . . O3 O 0.40271(18) -0.19998(9) 0.55669(13) 0.0343(6) Uani 1 1 d . . . O4 O 0.2738(2) -0.25797(9) 0.61116(14) 0.0358(6) Uani 1 1 d . . . H4O H 0.2731 -0.2473 0.6503 0.043 Uiso 1 1 calc R . . O5 O -0.0664(4) -0.2335(2) 0.6767(3) 0.1128(8) Uani 1 1 d . . . O6 O -0.1396(3) -0.06334(17) 0.6690(2) 0.1006(15) Uani 1 1 d . . . O7 O 0.0539(4) -0.13488(19) 0.5627(3) 0.1128(8) Uani 1 1 d . . . O8 O 0.4045(3) -0.05578(14) 0.92960(19) 0.0723(10) Uani 1 1 d . . . O9 O 0.2665(4) -0.05397(19) 0.6758(3) 0.1128(8) Uani 1 1 d . . . O10 O 0.0716(4) 0.0157(2) 0.7864(3) 0.1128(8) Uani 1 1 d . . . O11 O 0.0794(3) -0.22245(15) 0.3375(2) 0.0918(13) Uani 1 1 d . . . O12 O -0.0543(3) -0.07137(18) 0.3888(2) 0.0969(14) Uani 1 1 d . . . O13 O 0.1403(4) -0.06486(16) 0.2633(2) 0.0950(14) Uani 1 1 d . . . O14 O 0.1318(3) 0.01911(13) 0.4944(3) 0.0865(12) Uani 1 1 d . . . O15 O 0.3736(3) -0.01106(17) 0.4061(3) 0.1046(15) Uani 1 1 d . . . O16 O 0.4731(3) -0.04495(15) 0.6515(2) 0.0876(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0323(19) 0.0333(18) 0.0358(18) -0.0081(15) 0.0224(16) -0.0024(15) C2 0.0277(17) 0.0351(18) 0.0236(15) -0.0023(14) 0.0147(14) 0.0030(14) C3 0.0308(18) 0.0345(18) 0.0272(16) -0.0051(14) 0.0161(14) -0.0008(14) C4 0.0265(18) 0.047(2) 0.0324(18) 0.0020(16) 0.0119(15) 0.0027(16) C5 0.041(2) 0.040(2) 0.044(2) 0.0058(17) 0.0238(18) 0.0095(17) C6 0.043(2) 0.0333(19) 0.050(2) -0.0045(17) 0.0292(19) 0.0001(16) C7 0.047(3) 0.047(2) 0.067(3) 0.014(2) 0.031(2) 0.0166(19) C8 0.071(4) 0.085(4) 0.088(4) 0.028(3) 0.038(3) 0.044(3) C9 0.071(4) 0.085(4) 0.088(4) 0.028(3) 0.038(3) 0.044(3) C10 0.071(4) 0.085(4) 0.088(4) 0.028(3) 0.038(3) 0.044(3) C8B 0.071(4) 0.085(4) 0.088(4) 0.028(3) 0.038(3) 0.044(3) C9B 0.071(4) 0.085(4) 0.088(4) 0.028(3) 0.038(3) 0.044(3) C10B 0.071(4) 0.085(4) 0.088(4) 0.028(3) 0.038(3) 0.044(3) C11 0.0268(18) 0.0384(19) 0.0332(18) -0.0065(15) 0.0110(15) -0.0014(15) C12 0.0262(17) 0.0270(17) 0.0358(18) -0.0039(14) 0.0127(15) -0.0022(13) C13 0.0244(17) 0.0268(17) 0.0335(18) -0.0007(14) 0.0095(14) -0.0021(13) C14 0.0311(19) 0.0302(18) 0.0357(18) -0.0018(15) 0.0151(16) -0.0009(14) C15 0.0268(19) 0.041(2) 0.046(2) -0.0041(17) 0.0183(17) -0.0036(15) C16 0.0254(18) 0.041(2) 0.041(2) -0.0039(16) 0.0109(16) -0.0006(15) C17 0.0291(19) 0.0369(19) 0.0343(19) -0.0068(15) 0.0117(15) 0.0001(15) C18 0.027(2) 0.067(3) 0.047(2) -0.008(2) 0.0111(18) 0.0017(19) C19 0.0287(19) 0.090(5) 0.070(2) -0.009(4) 0.0082(17) 0.006(2) C20 0.0287(19) 0.090(5) 0.070(2) -0.009(4) 0.0082(17) 0.006(2) C21 0.0287(19) 0.090(5) 0.070(2) -0.009(4) 0.0082(17) 0.006(2) C19B 0.0287(19) 0.090(5) 0.070(2) -0.009(4) 0.0082(17) 0.006(2) C20B 0.0287(19) 0.090(5) 0.070(2) -0.009(4) 0.0082(17) 0.006(2) C21B 0.0287(19) 0.090(5) 0.070(2) -0.009(4) 0.0082(17) 0.006(2) C22 0.034(2) 0.0369(19) 0.0377(19) 0.0013(16) 0.0191(16) -0.0032(15) C23 0.0291(18) 0.0368(19) 0.0293(17) 0.0039(15) 0.0157(14) -0.0021(15) C24 0.0271(17) 0.043(2) 0.0250(16) 0.0056(15) 0.0141(14) 0.0024(15) C25 0.0247(17) 0.044(2) 0.0215(15) 0.0026(14) 0.0088(13) -0.0037(15) C26 0.033(2) 0.0376(19) 0.0299(18) 0.0014(15) 0.0138(15) -0.0053(15) C27 0.0290(19) 0.037(2) 0.0312(18) 0.0081(15) 0.0126(15) 0.0046(15) C28 0.0223(17) 0.043(2) 0.0329(18) 0.0010(16) 0.0111(14) -0.0042(15) C29 0.034(2) 0.042(2) 0.038(2) 0.0056(16) 0.0156(17) 0.0081(16) C30 0.060(3) 0.064(3) 0.076(3) 0.015(3) 0.026(3) 0.023(2) C31 0.060(3) 0.064(3) 0.076(3) 0.015(3) 0.026(3) 0.023(2) C32 0.060(3) 0.064(3) 0.076(3) 0.015(3) 0.026(3) 0.023(2) C30B 0.060(3) 0.064(3) 0.076(3) 0.015(3) 0.026(3) 0.023(2) C31B 0.060(3) 0.064(3) 0.076(3) 0.015(3) 0.026(3) 0.023(2) C32B 0.060(3) 0.064(3) 0.076(3) 0.015(3) 0.026(3) 0.023(2) C33 0.0317(19) 0.047(2) 0.0266(17) 0.0039(15) 0.0081(15) -0.0075(16) C34 0.0209(16) 0.039(2) 0.0240(16) -0.0002(14) 0.0067(13) -0.0057(14) C35 0.0184(16) 0.0314(18) 0.0329(18) 0.0006(14) 0.0076(14) -0.0024(13) C36 0.0259(17) 0.0302(18) 0.0362(18) -0.0031(15) 0.0147(15) -0.0024(14) C37 0.0335(19) 0.0335(19) 0.0358(18) -0.0015(15) 0.0202(16) -0.0060(15) C38 0.0329(19) 0.0294(17) 0.0351(18) -0.0033(15) 0.0173(16) -0.0054(14) C39 0.0256(18) 0.046(2) 0.0253(16) -0.0077(15) 0.0092(14) -0.0019(15) C40 0.055(3) 0.033(2) 0.059(3) -0.0077(18) 0.034(2) -0.0026(18) C41 0.084(4) 0.051(3) 0.127(5) 0.015(3) 0.069(4) 0.026(3) C42 0.112(5) 0.049(3) 0.079(4) -0.027(3) 0.049(3) -0.020(3) C43 0.105(4) 0.034(2) 0.085(3) -0.003(2) 0.066(3) -0.004(2) C44 0.036(2) 0.039(2) 0.046(2) -0.0110(17) 0.0262(17) -0.0061(16) C45 0.037(2) 0.040(2) 0.0356(18) 0.0065(16) 0.0242(16) 0.0097(16) C46 0.0303(18) 0.0312(18) 0.0308(17) 0.0027(14) 0.0153(15) 0.0029(14) C47 0.0303(19) 0.041(2) 0.0333(18) 0.0046(15) 0.0187(15) 0.0051(15) C48 0.062(3) 0.055(3) 0.068(3) 0.000(2) 0.011(3) -0.024(2) C49 0.036(2) 0.072(3) 0.054(3) 0.002(2) 0.009(2) 0.011(2) C50 0.051(3) 0.126(5) 0.041(2) -0.003(3) 0.026(2) -0.012(3) C51 0.049(3) 0.050(2) 0.046(2) 0.0085(19) 0.027(2) 0.0026(19) C52 0.089(4) 0.113(5) 0.053(3) 0.005(3) 0.047(3) -0.031(3) C53 0.042(3) 0.038(2) 0.127(5) 0.003(3) 0.026(3) 0.010(2) C54 0.0309(19) 0.042(2) 0.0276(17) 0.0061(15) 0.0151(15) 0.0024(15) C55 0.0293(18) 0.0326(18) 0.0279(17) 0.0007(14) 0.0117(15) -0.0016(14) C56 0.035(2) 0.037(2) 0.0346(19) 0.0025(15) 0.0168(16) 0.0002(15) C57 0.037(2) 0.083(4) 0.053(3) -0.018(3) 0.011(2) 0.002(2) C58 0.039(3) 0.093(4) 0.050(3) -0.013(2) 0.015(2) 0.007(2) C59 0.062(3) 0.085(3) 0.044(2) 0.015(2) 0.029(2) 0.044(3) C60 0.056(3) 0.047(3) 0.077(3) -0.014(2) 0.039(3) -0.009(2) C61 0.061(3) 0.055(3) 0.087(4) 0.020(3) 0.047(3) 0.012(2) C62 0.057(3) 0.052(3) 0.063(3) -0.012(2) 0.032(3) -0.011(2) Co1 0.0299(3) 0.0437(3) 0.0365(3) 0.0032(2) 0.0150(2) 0.0015(2) Co2 0.0340(3) 0.0373(3) 0.0383(3) 0.0035(2) 0.0160(2) 0.0012(2) Co3 0.0311(3) 0.0544(3) 0.0354(3) -0.0028(2) 0.0134(2) 0.0093(2) Co4 0.0411(3) 0.0362(3) 0.0489(3) 0.0002(2) 0.0244(3) 0.0015(2) O1 0.0263(12) 0.0323(12) 0.0264(11) 0.0002(9) 0.0131(10) 0.0024(9) O2 0.0216(12) 0.0490(15) 0.0311(12) -0.0018(11) 0.0081(10) 0.0016(10) O3 0.0280(12) 0.0447(14) 0.0266(12) 0.0053(10) 0.0121(10) 0.0079(11) O4 0.0390(14) 0.0316(13) 0.0360(14) -0.0036(10) 0.0193(12) -0.0019(10) O5 0.0936(17) 0.131(2) 0.1014(17) -0.0090(14) 0.0434(14) -0.0300(14) O6 0.046(2) 0.114(3) 0.108(3) -0.021(2) 0.018(2) 0.030(2) O7 0.0936(17) 0.131(2) 0.1014(17) -0.0090(14) 0.0434(14) -0.0300(14) O8 0.0468(19) 0.090(2) 0.0548(19) 0.0005(17) 0.0095(16) -0.0142(17) O9 0.0936(17) 0.131(2) 0.1014(17) -0.0090(14) 0.0434(14) -0.0300(14) O10 0.0936(17) 0.131(2) 0.1014(17) -0.0090(14) 0.0434(14) -0.0300(14) O11 0.068(2) 0.073(2) 0.110(3) -0.044(2) 0.031(2) -0.0154(19) O12 0.043(2) 0.156(4) 0.084(3) -0.033(2) 0.0288(19) 0.021(2) O13 0.127(3) 0.114(3) 0.073(2) 0.039(2) 0.073(3) 0.069(3) O14 0.072(2) 0.058(2) 0.136(3) -0.022(2) 0.059(2) 0.0065(18) O15 0.103(3) 0.111(3) 0.140(4) 0.048(3) 0.092(3) 0.014(2) O16 0.073(2) 0.090(3) 0.067(2) -0.014(2) 0.014(2) -0.026(2) _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 C6 1.389(5) . ? C1 C2 1.391(5) . ? C1 C44 1.530(5) . ? C2 C3 1.392(5) . ? C2 O1 1.400(4) . ? C3 C4 1.393(5) . ? C3 C11 1.524(5) . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? C5 C6 1.389(5) . ? C5 C7 1.518(5) . ? C6 H6 0.9500 . ? C7 C10 1.436(14) . ? C7 C8B 1.476(19) . ? C7 C9B 1.511(13) . ? C7 C10B 1.614(14) . ? C7 C8 1.621(18) . ? C7 C9 1.644(13) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11 C12 1.517(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.385(5) . ? C12 C17 1.387(5) . ? C13 O2 1.378(4) . ? C13 C14 1.391(5) . ? C14 C15 1.393(5) . ? C14 C22 1.533(5) . ? C15 C16 1.369(5) . ? C15 H15 0.9500 . ? C16 C17 1.407(5) . ? C16 C18 1.543(5) . ? C17 H17 0.9500 . ? C18 C20B 1.45(2) . ? C18 C19 1.486(18) . ? C18 C21B 1.489(14) . ? C18 C19B 1.532(17) . ? C18 C21 1.580(14) . ? C18 C20 1.65(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22 C23 1.526(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.384(5) . ? C23 C24 1.387(5) . ? C24 C25 1.382(5) . ? C24 O3 1.413(4) . ? C25 C26 1.381(5) . ? C25 C33 1.525(5) . ? C26 C27 1.383(5) . ? C26 H26 0.9500 . ? C27 C28 1.397(5) . ? C27 C29 1.543(5) . ? C28 H28 0.9500 . ? C29 C31 1.461(14) . ? C29 C30B 1.477(12) . ? C29 C32B 1.525(14) . ? C29 C30 1.560(12) . ? C29 C32 1.570(14) . ? C29 C31B 1.601(13) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33 C34 1.516(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.388(5) . ? C34 C35 1.388(5) . ? C35 O4 1.374(4) . ? C35 C36 1.393(5) . ? C36 C37 1.385(5) . ? C36 C44 1.503(5) . ? C37 C38 1.394(5) . ? C37 H37 0.9500 . ? C38 C39 1.391(5) . ? C38 C40 1.543(5) . ? C39 H39 0.9500 . ? C40 C43 1.520(6) . ? C40 C42 1.533(6) . ? C40 C41 1.536(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O1 1.434(4) . ? C45 C46 1.475(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.340(5) . ? C46 Co2 1.956(3) . ? C46 Co1 1.964(3) . ? C47 Co2 1.946(4) . ? C47 Co1 1.951(4) . ? C47 H47 1.0000 . ? C48 O5 1.140(6) . ? C48 Co1 1.750(5) . ? C49 O6 1.150(5) . ? C49 Co1 1.805(5) . ? C50 O7 1.150(6) . ? C50 Co1 1.762(5) . ? C51 O8 1.131(5) . ? C51 Co2 1.798(4) . ? C52 O9 1.157(6) . ? C52 Co2 1.762(5) . ? C53 O10 1.173(6) . ? C53 Co2 1.752(5) . ? C54 O3 1.433(4) . ? C54 C55 1.500(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.330(5) . ? C55 Co4 1.947(3) . ? C55 Co3 1.957(3) . ? C56 Co3 1.949(4) . ? C56 Co4 1.952(4) . ? C56 H56 1.0000 . ? C57 O11 1.145(5) . ? C57 Co3 1.776(5) . ? C58 O12 1.138(5) . ? C58 Co3 1.828(5) . ? C59 O13 1.124(6) . ? C59 Co3 1.806(5) . ? C60 O14 1.130(5) . ? C60 Co4 1.827(5) . ? C61 O15 1.141(6) . ? C61 Co4 1.799(5) . ? C62 O16 1.132(5) . ? C62 Co4 1.803(5) . ? Co1 Co2 2.4712(7) . ? Co3 Co4 2.4594(7) . ? O2 H2O 0.8400 . ? O4 H4O 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.5(3) . . ? C6 C1 C44 119.0(3) . . ? C2 C1 C44 122.0(3) . . ? C1 C2 C3 121.5(3) . . ? C1 C2 O1 119.3(3) . . ? C3 C2 O1 119.2(3) . . ? C2 C3 C4 117.5(3) . . ? C2 C3 C11 122.6(3) . . ? C4 C3 C11 119.6(3) . . ? C5 C4 C3 122.9(3) . . ? C5 C4 H4 118.5 . . ? C3 C4 H4 118.5 . . ? C4 C5 C6 117.4(3) . . ? C4 C5 C7 122.0(4) . . ? C6 C5 C7 120.5(3) . . ? C1 C6 C5 122.0(3) . . ? C1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C10 C7 C8B 125.8(8) . . ? C10 C7 C9B 77.9(7) . . ? C8B C7 C9B 112.9(8) . . ? C10 C7 C5 110.4(5) . . ? C8B C7 C5 112.2(7) . . ? C9B C7 C5 113.2(5) . . ? C8B C7 C10B 101.0(8) . . ? C9B C7 C10B 106.9(7) . . ? C5 C7 C10B 109.7(5) . . ? C10 C7 C8 112.1(8) . . ? C9B C7 C8 128.4(7) . . ? C5 C7 C8 109.7(6) . . ? C10B C7 C8 83.4(7) . . ? C10 C7 C9 113.6(7) . . ? C8B C7 C9 80.4(7) . . ? C5 C7 C9 110.7(5) . . ? C10B C7 C9 135.5(6) . . ? C8 C7 C9 99.9(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C8B H8B1 109.5 . . ? C7 C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7 C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7 C9B H9B1 109.5 . . ? C7 C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7 C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7 C10B H10D 109.5 . . ? C7 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C12 C11 C3 108.3(3) . . ? C12 C11 H11A 110.0 . . ? C3 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? C3 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C13 C12 C17 119.1(3) . . ? C13 C12 C11 119.7(3) . . ? C17 C12 C11 120.8(3) . . ? O2 C13 C12 115.7(3) . . ? O2 C13 C14 123.7(3) . . ? C12 C13 C14 120.6(3) . . ? C13 C14 C15 118.2(3) . . ? C13 C14 C22 121.8(3) . . ? C15 C14 C22 120.0(3) . . ? C16 C15 C14 123.5(4) . . ? C16 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C15 C16 C17 116.5(3) . . ? C15 C16 C18 121.9(4) . . ? C17 C16 C18 121.4(3) . . ? C12 C17 C16 122.0(3) . . ? C12 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C20B C18 C19 118.5(9) . . ? C20B C18 C21B 114.2(7) . . ? C19 C18 C21B 87.3(7) . . ? C20B C18 C19B 102.1(10) . . ? C21B C18 C19B 108.4(7) . . ? C20B C18 C16 111.9(6) . . ? C19 C18 C16 114.3(6) . . ? C21B C18 C16 108.1(5) . . ? C19B C18 C16 112.1(6) . . ? C20B C18 C21 87.9(7) . . ? C19 C18 C21 111.5(7) . . ? C19B C18 C21 129.1(7) . . ? C16 C18 C21 109.7(5) . . ? C19 C18 C20 113.4(9) . . ? C21B C18 C20 129.5(8) . . ? C19B C18 C20 93.8(8) . . ? C16 C18 C20 104.0(5) . . ? C21 C18 C20 103.2(8) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? C18 C19B H19D 109.5 . . ? C18 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C18 C20B H20D 109.5 . . ? C18 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C18 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C18 C21B H21D 109.5 . . ? C18 C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C18 C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C23 C22 C14 112.0(3) . . ? C23 C22 H22A 109.2 . . ? C14 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C14 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C28 C23 C24 117.6(3) . . ? C28 C23 C22 120.2(3) . . ? C24 C23 C22 122.1(3) . . ? C25 C24 C23 122.6(3) . . ? C25 C24 O3 118.7(3) . . ? C23 C24 O3 118.4(3) . . ? C26 C25 C24 117.4(3) . . ? C26 C25 C33 119.5(3) . . ? C24 C25 C33 122.9(3) . . ? C25 C26 C27 123.0(3) . . ? C25 C26 H26 118.5 . . ? C27 C26 H26 118.5 . . ? C26 C27 C28 117.2(3) . . ? C26 C27 C29 120.7(3) . . ? C28 C27 C29 122.1(3) . . ? C23 C28 C27 122.1(3) . . ? C23 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C31 C29 C30B 88.2(7) . . ? C31 C29 C32B 125.9(7) . . ? C30B C29 C32B 108.0(6) . . ? C31 C29 C27 110.1(5) . . ? C30B C29 C27 115.3(5) . . ? C32B C29 C27 108.3(5) . . ? C31 C29 C30 117.3(7) . . ? C32B C29 C30 80.8(6) . . ? C27 C29 C30 111.3(5) . . ? C31 C29 C32 106.4(7) . . ? C30B C29 C32 124.7(6) . . ? C27 C29 C32 109.0(5) . . ? C30 C29 C32 102.0(6) . . ? C30B C29 C31B 110.0(7) . . ? C32B C29 C31B 103.7(6) . . ? C27 C29 C31B 110.9(5) . . ? C30 C29 C31B 133.4(6) . . ? C32 C29 C31B 81.9(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? C29 C30B H30D 109.5 . . ? C29 C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29 C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C29 C31B H31D 109.5 . . ? C29 C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C29 C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C29 C32B H32D 109.5 . . ? C29 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C29 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C34 C33 C25 112.1(3) . . ? C34 C33 H33A 109.2 . . ? C25 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C25 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C39 C34 C35 119.0(3) . . ? C39 C34 C33 120.0(3) . . ? C35 C34 C33 120.8(3) . . ? O4 C35 C34 118.4(3) . . ? O4 C35 C36 121.1(3) . . ? C34 C35 C36 120.5(3) . . ? C37 C36 C35 118.6(3) . . ? C37 C36 C44 120.7(3) . . ? C35 C36 C44 120.3(3) . . ? C36 C37 C38 122.8(3) . . ? C36 C37 H37 118.6 . . ? C38 C37 H37 118.6 . . ? C39 C38 C37 116.5(3) . . ? C39 C38 C40 120.7(3) . . ? C37 C38 C40 122.7(3) . . ? C34 C39 C38 122.5(3) . . ? C34 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C43 C40 C42 108.9(4) . . ? C43 C40 C41 107.9(4) . . ? C42 C40 C41 108.4(4) . . ? C43 C40 C38 112.8(3) . . ? C42 C40 C38 109.5(3) . . ? C41 C40 C38 109.1(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C36 C44 C1 108.7(3) . . ? C36 C44 H44A 109.9 . . ? C1 C44 H44A 109.9 . . ? C36 C44 H44B 109.9 . . ? C1 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? O1 C45 C46 113.6(3) . . ? O1 C45 H45A 108.8 . . ? C46 C45 H45A 108.8 . . ? O1 C45 H45B 108.8 . . ? C46 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? C47 C46 C45 136.1(3) . . ? C47 C46 Co2 69.5(2) . . ? C45 C46 Co2 136.4(3) . . ? C47 C46 Co1 69.5(2) . . ? C45 C46 Co1 137.9(3) . . ? Co2 C46 Co1 78.15(12) . . ? C46 C47 Co2 70.3(2) . . ? C46 C47 Co1 70.5(2) . . ? Co2 C47 Co1 78.70(14) . . ? C46 C47 H47 136.4 . . ? Co2 C47 H47 136.4 . . ? Co1 C47 H47 136.4 . . ? O5 C48 Co1 178.8(6) . . ? O6 C49 Co1 176.4(5) . . ? O7 C50 Co1 178.7(6) . . ? O8 C51 Co2 179.3(5) . . ? O9 C52 Co2 178.2(6) . . ? O10 C53 Co2 174.3(6) . . ? O3 C54 C55 106.4(3) . . ? O3 C54 H54A 110.4 . . ? C55 C54 H54A 110.4 . . ? O3 C54 H54B 110.4 . . ? C55 C54 H54B 110.4 . . ? H54A C54 H54B 108.6 . . ? C56 C55 C54 134.9(3) . . ? C56 C55 Co4 70.3(2) . . ? C54 C55 Co4 138.3(3) . . ? C56 C55 Co3 69.8(2) . . ? C54 C55 Co3 136.3(2) . . ? Co4 C55 Co3 78.11(13) . . ? C55 C56 Co3 70.4(2) . . ? C55 C56 Co4 69.8(2) . . ? Co3 C56 Co4 78.17(14) . . ? C55 C56 H56 136.6 . . ? Co3 C56 H56 136.6 . . ? Co4 C56 H56 136.6 . . ? O11 C57 Co3 175.0(4) . . ? O12 C58 Co3 178.3(5) . . ? O13 C59 Co3 177.7(5) . . ? O14 C60 Co4 176.6(4) . . ? O15 C61 Co4 177.3(5) . . ? O16 C62 Co4 179.2(5) . . ? C48 Co1 C50 97.0(3) . . ? C48 Co1 C49 98.4(2) . . ? C50 Co1 C49 106.0(2) . . ? C48 Co1 C47 103.1(2) . . ? C50 Co1 C47 142.98(19) . . ? C49 Co1 C47 101.46(18) . . ? C48 Co1 C46 100.92(19) . . ? C50 Co1 C46 106.0(2) . . ? C49 Co1 C46 140.03(18) . . ? C47 Co1 C46 40.02(14) . . ? C48 Co1 Co2 150.28(16) . . ? C50 Co1 Co2 99.71(17) . . ? C49 Co1 Co2 100.38(15) . . ? C47 Co1 Co2 50.55(11) . . ? C46 Co1 Co2 50.79(10) . . ? C53 Co2 C52 107.2(3) . . ? C53 Co2 C51 101.0(2) . . ? C52 Co2 C51 98.6(2) . . ? C53 Co2 C47 99.0(2) . . ? C52 Co2 C47 142.5(2) . . ? C51 Co2 C47 102.27(16) . . ? C53 Co2 C46 137.6(2) . . ? C52 Co2 C46 105.8(2) . . ? C51 Co2 C46 99.64(16) . . ? C47 Co2 C46 40.17(15) . . ? C53 Co2 Co1 97.98(16) . . ? C52 Co2 Co1 98.51(18) . . ? C51 Co2 Co1 149.35(13) . . ? C47 Co2 Co1 50.75(10) . . ? C46 Co2 Co1 51.06(10) . . ? C57 Co3 C59 99.9(2) . . ? C57 Co3 C58 102.6(2) . . ? C59 Co3 C58 105.2(2) . . ? C57 Co3 C56 103.10(19) . . ? C59 Co3 C56 142.6(2) . . ? C58 Co3 C56 98.08(18) . . ? C57 Co3 C55 95.75(17) . . ? C59 Co3 C55 109.09(18) . . ? C58 Co3 C55 137.34(18) . . ? C56 Co3 C55 39.82(15) . . ? C57 Co3 Co4 146.39(14) . . ? C59 Co3 Co4 95.06(17) . . ? C58 Co3 Co4 102.17(15) . . ? C56 Co3 Co4 50.97(11) . . ? C55 Co3 Co4 50.77(10) . . ? C61 Co4 C62 98.5(2) . . ? C61 Co4 C60 107.0(2) . . ? C62 Co4 C60 99.8(2) . . ? C61 Co4 C55 103.25(19) . . ? C62 Co4 C55 102.46(17) . . ? C60 Co4 C55 138.94(18) . . ? C61 Co4 C56 141.9(2) . . ? C62 Co4 C56 99.45(18) . . ? C60 Co4 C56 102.66(18) . . ? C55 Co4 C56 39.89(15) . . ? C61 Co4 Co3 102.59(17) . . ? C62 Co4 Co3 149.33(14) . . ? C60 Co4 Co3 95.06(14) . . ? C55 Co4 Co3 51.12(10) . . ? C56 Co4 Co3 50.86(10) . . ? C2 O1 C45 107.2(2) . . ? C13 O2 H2O 109.5 . . ? C24 O3 C54 114.4(3) . . ? C35 O4 H4O 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.0(5) . . . . ? C44 C1 C2 C3 -170.5(3) . . . . ? C6 C1 C2 O1 -176.9(3) . . . . ? C44 C1 C2 O1 10.6(5) . . . . ? C1 C2 C3 C4 -2.5(5) . . . . ? O1 C2 C3 C4 176.4(3) . . . . ? C1 C2 C3 C11 172.5(3) . . . . ? O1 C2 C3 C11 -8.6(5) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C11 C3 C4 C5 -174.2(3) . . . . ? C3 C4 C5 C6 1.1(6) . . . . ? C3 C4 C5 C7 177.0(4) . . . . ? C2 C1 C6 C5 0.1(6) . . . . ? C44 C1 C6 C5 172.8(4) . . . . ? C4 C5 C6 C1 -1.6(6) . . . . ? C7 C5 C6 C1 -177.6(4) . . . . ? C4 C5 C7 C10 -106.6(7) . . . . ? C6 C5 C7 C10 69.2(8) . . . . ? C4 C5 C7 C8B 107.8(7) . . . . ? C6 C5 C7 C8B -76.4(8) . . . . ? C4 C5 C7 C9B -21.4(8) . . . . ? C6 C5 C7 C9B 154.4(7) . . . . ? C4 C5 C7 C10B -140.8(6) . . . . ? C6 C5 C7 C10B 35.0(7) . . . . ? C4 C5 C7 C8 129.3(7) . . . . ? C6 C5 C7 C8 -54.9(8) . . . . ? C4 C5 C7 C9 20.0(7) . . . . ? C6 C5 C7 C9 -164.2(6) . . . . ? C2 C3 C11 C12 -120.9(3) . . . . ? C4 C3 C11 C12 54.0(4) . . . . ? C3 C11 C12 C13 74.7(4) . . . . ? C3 C11 C12 C17 -97.6(4) . . . . ? C17 C12 C13 O2 -179.7(3) . . . . ? C11 C12 C13 O2 7.9(4) . . . . ? C17 C12 C13 C14 0.9(5) . . . . ? C11 C12 C13 C14 -171.6(3) . . . . ? O2 C13 C14 C15 -179.8(3) . . . . ? C12 C13 C14 C15 -0.4(5) . . . . ? O2 C13 C14 C22 -2.1(5) . . . . ? C12 C13 C14 C22 177.3(3) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? C22 C14 C15 C16 -178.0(3) . . . . ? C14 C15 C16 C17 0.3(5) . . . . ? C14 C15 C16 C18 177.0(3) . . . . ? C13 C12 C17 C16 -0.8(5) . . . . ? C11 C12 C17 C16 171.5(3) . . . . ? C15 C16 C17 C12 0.2(5) . . . . ? C18 C16 C17 C12 -176.5(3) . . . . ? C15 C16 C18 C20B 54.9(8) . . . . ? C17 C16 C18 C20B -128.5(8) . . . . ? C15 C16 C18 C19 -166.9(6) . . . . ? C17 C16 C18 C19 9.6(7) . . . . ? C15 C16 C18 C21B -71.6(7) . . . . ? C17 C16 C18 C21B 104.9(6) . . . . ? C15 C16 C18 C19B 169.0(6) . . . . ? C17 C16 C18 C19B -14.5(8) . . . . ? C15 C16 C18 C21 -40.9(7) . . . . ? C17 C16 C18 C21 135.6(6) . . . . ? C15 C16 C18 C20 68.9(8) . . . . ? C17 C16 C18 C20 -114.6(8) . . . . ? C13 C14 C22 C23 -74.5(4) . . . . ? C15 C14 C22 C23 103.1(4) . . . . ? C14 C22 C23 C28 -75.5(4) . . . . ? C14 C22 C23 C24 101.1(4) . . . . ? C28 C23 C24 C25 2.4(5) . . . . ? C22 C23 C24 C25 -174.3(3) . . . . ? C28 C23 C24 O3 176.5(3) . . . . ? C22 C23 C24 O3 -0.3(5) . . . . ? C23 C24 C25 C26 -2.8(5) . . . . ? O3 C24 C25 C26 -176.8(3) . . . . ? C23 C24 C25 C33 172.3(3) . . . . ? O3 C24 C25 C33 -1.8(5) . . . . ? C24 C25 C26 C27 1.6(5) . . . . ? C33 C25 C26 C27 -173.6(3) . . . . ? C25 C26 C27 C28 -0.1(5) . . . . ? C25 C26 C27 C29 177.4(3) . . . . ? C24 C23 C28 C27 -0.8(5) . . . . ? C22 C23 C28 C27 176.0(3) . . . . ? C26 C27 C28 C23 -0.3(5) . . . . ? C29 C27 C28 C23 -177.8(3) . . . . ? C26 C27 C29 C31 68.5(7) . . . . ? C28 C27 C29 C31 -114.1(6) . . . . ? C26 C27 C29 C30B 166.3(6) . . . . ? C28 C27 C29 C30B -16.3(7) . . . . ? C26 C27 C29 C32B -72.6(6) . . . . ? C28 C27 C29 C32B 104.8(6) . . . . ? C26 C27 C29 C30 -159.7(6) . . . . ? C28 C27 C29 C30 17.8(7) . . . . ? C26 C27 C29 C32 -47.9(6) . . . . ? C28 C27 C29 C32 129.6(6) . . . . ? C26 C27 C29 C31B 40.5(7) . . . . ? C28 C27 C29 C31B -142.1(6) . . . . ? C26 C25 C33 C34 66.7(4) . . . . ? C24 C25 C33 C34 -108.2(4) . . . . ? C25 C33 C34 C39 -93.7(4) . . . . ? C25 C33 C34 C35 81.4(4) . . . . ? C39 C34 C35 O4 -179.4(3) . . . . ? C33 C34 C35 O4 5.4(4) . . . . ? C39 C34 C35 C36 -0.3(5) . . . . ? C33 C34 C35 C36 -175.4(3) . . . . ? O4 C35 C36 C37 179.3(3) . . . . ? C34 C35 C36 C37 0.1(5) . . . . ? O4 C35 C36 C44 -7.7(5) . . . . ? C34 C35 C36 C44 173.2(3) . . . . ? C35 C36 C37 C38 0.2(5) . . . . ? C44 C36 C37 C38 -172.8(3) . . . . ? C36 C37 C38 C39 -0.4(5) . . . . ? C36 C37 C38 C40 177.2(3) . . . . ? C35 C34 C39 C38 0.1(5) . . . . ? C33 C34 C39 C38 175.3(3) . . . . ? C37 C38 C39 C34 0.2(5) . . . . ? C40 C38 C39 C34 -177.4(3) . . . . ? C39 C38 C40 C43 179.0(4) . . . . ? C37 C38 C40 C43 1.5(5) . . . . ? C39 C38 C40 C42 -59.5(5) . . . . ? C37 C38 C40 C42 123.0(4) . . . . ? C39 C38 C40 C41 59.0(5) . . . . ? C37 C38 C40 C41 -118.5(4) . . . . ? C37 C36 C44 C1 100.7(4) . . . . ? C35 C36 C44 C1 -72.2(4) . . . . ? C6 C1 C44 C36 -60.3(4) . . . . ? C2 C1 C44 C36 112.1(4) . . . . ? O1 C45 C46 C47 -179.3(4) . . . . ? O1 C45 C46 Co2 -68.3(5) . . . . ? O1 C45 C46 Co1 67.5(5) . . . . ? C45 C46 C47 Co2 136.5(5) . . . . ? Co1 C46 C47 Co2 -84.60(10) . . . . ? C45 C46 C47 Co1 -138.9(5) . . . . ? Co2 C46 C47 Co1 84.60(10) . . . . ? O3 C54 C55 C56 -16.6(5) . . . . ? O3 C54 C55 Co4 97.1(4) . . . . ? O3 C54 C55 Co3 -126.3(3) . . . . ? C54 C55 C56 Co3 -136.1(4) . . . . ? Co4 C55 C56 Co3 84.20(10) . . . . ? C54 C55 C56 Co4 139.7(4) . . . . ? Co3 C55 C56 Co4 -84.20(10) . . . . ? C46 C47 Co1 C48 91.4(3) . . . . ? Co2 C47 Co1 C48 164.4(2) . . . . ? C46 C47 Co1 C50 -29.7(4) . . . . ? Co2 C47 Co1 C50 43.2(4) . . . . ? C46 C47 Co1 C49 -167.0(3) . . . . ? Co2 C47 Co1 C49 -94.09(19) . . . . ? Co2 C47 Co1 C46 72.9(2) . . . . ? C46 C47 Co1 Co2 -72.9(2) . . . . ? C47 C46 Co1 C48 -97.4(3) . . . . ? C45 C46 Co1 C48 39.7(5) . . . . ? Co2 C46 Co1 C48 -169.8(2) . . . . ? C47 C46 Co1 C50 161.9(3) . . . . ? C45 C46 Co1 C50 -61.0(5) . . . . ? Co2 C46 Co1 C50 89.6(2) . . . . ? C47 C46 Co1 C49 20.0(4) . . . . ? C45 C46 Co1 C49 157.1(4) . . . . ? Co2 C46 Co1 C49 -52.3(3) . . . . ? C45 C46 Co1 C47 137.1(5) . . . . ? Co2 C46 Co1 C47 -72.3(2) . . . . ? C47 C46 Co1 Co2 72.3(2) . . . . ? C45 C46 Co1 Co2 -150.6(5) . . . . ? C46 C47 Co2 C53 166.1(3) . . . . ? Co1 C47 Co2 C53 93.0(2) . . . . ? C46 C47 Co2 C52 31.8(4) . . . . ? Co1 C47 Co2 C52 -41.3(4) . . . . ? C46 C47 Co2 C51 -90.5(2) . . . . ? Co1 C47 Co2 C51 -163.59(15) . . . . ? Co1 C47 Co2 C46 -73.1(2) . . . . ? C46 C47 Co2 Co1 73.1(2) . . . . ? C47 C46 Co2 C53 -20.6(4) . . . . ? C45 C46 Co2 C53 -156.8(4) . . . . ? Co1 C46 Co2 C53 51.7(3) . . . . ? C47 C46 Co2 C52 -160.5(3) . . . . ? C45 C46 Co2 C52 63.3(4) . . . . ? Co1 C46 Co2 C52 -88.2(2) . . . . ? C47 C46 Co2 C51 97.6(2) . . . . ? C45 C46 Co2 C51 -38.6(4) . . . . ? Co1 C46 Co2 C51 169.95(16) . . . . ? C45 C46 Co2 C47 -136.2(5) . . . . ? Co1 C46 Co2 C47 72.3(2) . . . . ? C47 C46 Co2 Co1 -72.3(2) . . . . ? C45 C46 Co2 Co1 151.5(4) . . . . ? C48 Co1 Co2 C53 -127.1(5) . . . . ? C50 Co1 Co2 C53 109.6(3) . . . . ? C49 Co1 Co2 C53 1.2(3) . . . . ? C47 Co1 Co2 C53 -95.2(3) . . . . ? C46 Co1 Co2 C53 -147.7(3) . . . . ? C48 Co1 Co2 C52 124.1(5) . . . . ? C50 Co1 Co2 C52 0.8(3) . . . . ? C49 Co1 Co2 C52 -107.6(3) . . . . ? C47 Co1 Co2 C52 156.0(2) . . . . ? C46 Co1 Co2 C52 103.5(3) . . . . ? C48 Co1 Co2 C51 0.9(5) . . . . ? C50 Co1 Co2 C51 -122.5(3) . . . . ? C49 Co1 Co2 C51 129.2(3) . . . . ? C47 Co1 Co2 C51 32.8(3) . . . . ? C46 Co1 Co2 C51 -19.7(3) . . . . ? C48 Co1 Co2 C47 -31.9(5) . . . . ? C50 Co1 Co2 C47 -155.3(2) . . . . ? C49 Co1 Co2 C47 96.4(2) . . . . ? C46 Co1 Co2 C47 -52.52(18) . . . . ? C48 Co1 Co2 C46 20.6(5) . . . . ? C50 Co1 Co2 C46 -102.7(2) . . . . ? C49 Co1 Co2 C46 148.9(2) . . . . ? C47 Co1 Co2 C46 52.52(18) . . . . ? C55 C56 Co3 C57 83.2(3) . . . . ? Co4 C56 Co3 C57 155.80(18) . . . . ? C55 C56 Co3 C59 -43.4(4) . . . . ? Co4 C56 Co3 C59 29.2(3) . . . . ? C55 C56 Co3 C58 -171.7(3) . . . . ? Co4 C56 Co3 C58 -99.15(19) . . . . ? Co4 C56 Co3 C55 72.6(2) . . . . ? C55 C56 Co3 Co4 -72.6(2) . . . . ? C56 C55 Co3 C57 -103.6(3) . . . . ? C54 C55 Co3 C57 31.2(4) . . . . ? Co4 C55 Co3 C57 -176.72(19) . . . . ? C56 C55 Co3 C59 153.8(3) . . . . ? C54 C55 Co3 C59 -71.5(4) . . . . ? Co4 C55 Co3 C59 80.7(2) . . . . ? C56 C55 Co3 C58 12.1(4) . . . . ? C54 C55 Co3 C58 146.8(4) . . . . ? Co4 C55 Co3 C58 -61.0(3) . . . . ? C54 C55 Co3 C56 134.7(5) . . . . ? Co4 C55 Co3 C56 -73.1(2) . . . . ? C56 C55 Co3 Co4 73.1(2) . . . . ? C54 C55 Co3 Co4 -152.1(4) . . . . ? C56 C55 Co4 C61 -168.2(2) . . . . ? C54 C55 Co4 C61 55.3(4) . . . . ? Co3 C55 Co4 C61 -95.62(19) . . . . ? C56 C55 Co4 C62 89.9(3) . . . . ? C54 C55 Co4 C62 -46.6(4) . . . . ? Co3 C55 Co4 C62 162.43(18) . . . . ? C56 C55 Co4 C60 -31.4(4) . . . . ? C54 C55 Co4 C60 -167.9(4) . . . . ? Co3 C55 Co4 C60 41.1(3) . . . . ? C54 C55 Co4 C56 -136.5(5) . . . . ? Co3 C55 Co4 C56 72.6(2) . . . . ? C56 C55 Co4 Co3 -72.6(2) . . . . ? C54 C55 Co4 Co3 151.0(4) . . . . ? C55 C56 Co4 C61 18.9(4) . . . . ? Co3 C56 Co4 C61 -54.4(3) . . . . ? C55 C56 Co4 C62 -98.2(2) . . . . ? Co3 C56 Co4 C62 -171.41(17) . . . . ? C55 C56 Co4 C60 159.4(2) . . . . ? Co3 C56 Co4 C60 86.20(19) . . . . ? Co3 C56 Co4 C55 -73.3(2) . . . . ? C55 C56 Co4 Co3 73.3(2) . . . . ? C57 Co3 Co4 C61 102.9(4) . . . . ? C59 Co3 Co4 C61 -13.6(2) . . . . ? C58 Co3 Co4 C61 -120.4(2) . . . . ? C56 Co3 Co4 C61 149.1(2) . . . . ? C55 Co3 Co4 C61 97.0(2) . . . . ? C57 Co3 Co4 C62 -29.4(5) . . . . ? C59 Co3 Co4 C62 -145.9(3) . . . . ? C58 Co3 Co4 C62 107.4(4) . . . . ? C56 Co3 Co4 C62 16.8(3) . . . . ? C55 Co3 Co4 C62 -35.3(3) . . . . ? C57 Co3 Co4 C60 -148.4(4) . . . . ? C59 Co3 Co4 C60 95.1(2) . . . . ? C58 Co3 Co4 C60 -11.6(2) . . . . ? C56 Co3 Co4 C60 -102.2(2) . . . . ? C55 Co3 Co4 C60 -154.3(2) . . . . ? C57 Co3 Co4 C55 5.9(3) . . . . ? C59 Co3 Co4 C55 -110.58(19) . . . . ? C58 Co3 Co4 C55 142.7(2) . . . . ? C56 Co3 Co4 C55 52.08(19) . . . . ? C57 Co3 Co4 C56 -46.2(4) . . . . ? C59 Co3 Co4 C56 -162.66(19) . . . . ? C58 Co3 Co4 C56 90.6(2) . . . . ? C55 Co3 Co4 C56 -52.08(19) . . . . ? C1 C2 O1 C45 87.5(4) . . . . ? C3 C2 O1 C45 -91.4(4) . . . . ? C46 C45 O1 C2 171.8(3) . . . . ? C25 C24 O3 C54 -91.4(4) . . . . ? C23 C24 O3 C54 94.3(4) . . . . ? C55 C54 O3 C24 179.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O O3 0.84 1.96 2.791(3) 169.2 . O4 H4O O1 0.84 2.37 3.189(3) 166.1 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.338 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.088 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 711454' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H64 Co8 O28' _chemical_formula_sum 'C80 H64 Co8 O28' _chemical_formula_weight 1944.75 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0934(3) _cell_length_b 29.5203(8) _cell_length_c 22.3018(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.0460(10) _cell_angle_gamma 90.00 _cell_volume 8473.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 75295 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 1.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57257 _exptl_absorpt_correction_T_max 0.71681 _exptl_absorpt_process_details 'MULscanABS in PLATON (Spek, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42107 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.49 _reflns_number_total 18400 _reflns_number_gt 10285 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0513P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18400 _refine_ls_number_parameters 1057 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1228 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 C1 C -0.1718(3) -0.15273(12) 0.17089(15) 0.0277(8) Uani 1 1 d . . . C2 C -0.2301(3) -0.15802(13) 0.20857(15) 0.0303(9) Uani 1 1 d . . . C3 C -0.2471(3) -0.20191(13) 0.22458(16) 0.0318(9) Uani 1 1 d . . . H3 H -0.2895 -0.2060 0.2481 0.038 Uiso 1 1 calc R . . C4 C -0.2057(3) -0.24001(13) 0.20809(16) 0.0340(9) Uani 1 1 d . . . C5 C -0.1393(3) -0.23279(13) 0.17684(16) 0.0331(9) Uani 1 1 d . . . H5 H -0.1053 -0.2580 0.1679 0.040 Uiso 1 1 calc R . . C6 C -0.1212(3) -0.18978(13) 0.15832(15) 0.0285(9) Uani 1 1 d . . . C7 C -0.2341(3) -0.28741(14) 0.22387(19) 0.0414(10) Uani 1 1 d . . . C8 C -0.3482(4) -0.29565(16) 0.1815(3) 0.0721(15) Uani 1 1 d . . . H8A H -0.3599 -0.2948 0.1351 0.108 Uiso 1 1 calc R . . H8B H -0.3900 -0.2721 0.1901 0.108 Uiso 1 1 calc R . . H8C H -0.3685 -0.3254 0.1919 0.108 Uiso 1 1 calc R . . C9 C -0.1713(4) -0.32471(14) 0.2098(2) 0.0561(12) Uani 1 1 d . . . H9A H -0.1919 -0.3542 0.2208 0.084 Uiso 1 1 calc R . . H9B H -0.0971 -0.3197 0.2364 0.084 Uiso 1 1 calc R . . H9C H -0.1843 -0.3242 0.1631 0.084 Uiso 1 1 calc R . . C10 C -0.2149(4) -0.29084(16) 0.2967(2) 0.0677(14) Uani 1 1 d . . . H10A H -0.2608 -0.2697 0.3060 0.102 Uiso 1 1 calc R . . H10B H -0.1423 -0.2832 0.3241 0.102 Uiso 1 1 calc R . . H10C H -0.2293 -0.3218 0.3065 0.102 Uiso 1 1 calc R . . C11 C -0.0456(3) -0.18378(13) 0.12599(16) 0.0323(9) Uani 1 1 d . . . H11A H -0.0440 -0.1516 0.1142 0.039 Uiso 1 1 calc R . . H11B H -0.0693 -0.2019 0.0851 0.039 Uiso 1 1 calc R . . C12 C 0.0636(3) -0.19886(12) 0.17230(15) 0.0258(8) Uani 1 1 d . . . C13 C 0.1207(3) -0.17263(12) 0.22712(16) 0.0269(8) Uani 1 1 d . . . C14 C 0.2157(3) -0.18794(12) 0.27416(15) 0.0254(8) Uani 1 1 d . . . C15 C 0.2554(3) -0.22773(13) 0.26190(16) 0.0308(9) Uani 1 1 d . . . H15 H 0.3209 -0.2379 0.2931 0.037 Uiso 1 1 calc R . . C16 C 0.2036(3) -0.25403(12) 0.20549(16) 0.0298(9) Uani 1 1 d . . . C17 C 0.1058(3) -0.23895(13) 0.16226(16) 0.0307(9) Uani 1 1 d . . . H17 H 0.0670 -0.2568 0.1248 0.037 Uiso 1 1 calc R . . C18 C 0.2551(3) -0.29708(13) 0.19436(18) 0.0405(10) Uani 1 1 d . . . C19 C 0.3624(3) -0.28536(15) 0.1962(2) 0.0571(12) Uani 1 1 d . . . H19A H 0.3542 -0.2643 0.1604 0.086 Uiso 1 1 calc R . . H19B H 0.3964 -0.3131 0.1909 0.086 Uiso 1 1 calc R . . H19C H 0.4051 -0.2712 0.2384 0.086 Uiso 1 1 calc R . . C20 C 0.2674(4) -0.33098(14) 0.2497(2) 0.0596(13) Uani 1 1 d . . . H20A H 0.3098 -0.3173 0.2923 0.089 Uiso 1 1 calc R . . H20B H 0.3014 -0.3585 0.2438 0.089 Uiso 1 1 calc R . . H20C H 0.1987 -0.3386 0.2481 0.089 Uiso 1 1 calc R . . C21 C 0.1911(3) -0.31915(14) 0.12757(19) 0.0526(12) Uani 1 1 d . . . H21A H 0.1223 -0.3274 0.1253 0.079 Uiso 1 1 calc R . . H21B H 0.2268 -0.3464 0.1225 0.079 Uiso 1 1 calc R . . H21C H 0.1833 -0.2977 0.0923 0.079 Uiso 1 1 calc R . . C22 C 0.2712(3) -0.16365(12) 0.33918(15) 0.0284(8) Uani 1 1 d . . . H22A H 0.2748 -0.1308 0.3312 0.034 Uiso 1 1 calc R . . H22B H 0.3431 -0.1753 0.3612 0.034 Uiso 1 1 calc R . . C23 C 0.2135(3) -0.17109(13) 0.38339(15) 0.0272(8) Uani 1 1 d . . . C24 C 0.1691(3) -0.13569(12) 0.40504(15) 0.0252(8) Uani 1 1 d . . . C25 C 0.1022(3) -0.14497(12) 0.43550(15) 0.0261(8) Uani 1 1 d . . . C26 C 0.0876(3) -0.19010(12) 0.44811(16) 0.0301(9) Uani 1 1 d . . . H26 H 0.0410 -0.1966 0.4680 0.036 Uiso 1 1 calc R . . C27 C 0.1378(3) -0.22609(13) 0.43295(16) 0.0318(9) Uani 1 1 d . . . C28 C 0.1982(3) -0.21512(12) 0.39892(16) 0.0295(9) Uani 1 1 d . . . H28 H 0.2306 -0.2390 0.3857 0.035 Uiso 1 1 calc R . . C29 C 0.1285(3) -0.27535(13) 0.45020(19) 0.0431(10) Uani 1 1 d . . . C30 C 0.0451(4) -0.28174(15) 0.4767(2) 0.0560(12) Uani 1 1 d . . . H30A H 0.0414 -0.3138 0.4871 0.084 Uiso 1 1 calc R . . H30B H -0.0224 -0.2720 0.4436 0.084 Uiso 1 1 calc R . . H30C H 0.0627 -0.2636 0.5166 0.084 Uiso 1 1 calc R . . C31 C 0.0984(4) -0.30452(16) 0.3880(3) 0.0825(18) Uani 1 1 d . . . H31A H 0.1550 -0.3040 0.3731 0.124 Uiso 1 1 calc R . . H31B H 0.0351 -0.2924 0.3533 0.124 Uiso 1 1 calc R . . H31C H 0.0861 -0.3358 0.3978 0.124 Uiso 1 1 calc R . . C32 C 0.2320(4) -0.29122(16) 0.5015(3) 0.0737(15) Uani 1 1 d . . . H32A H 0.2862 -0.2865 0.4852 0.111 Uiso 1 1 calc R . . H32B H 0.2277 -0.3235 0.5103 0.111 Uiso 1 1 calc R . . H32C H 0.2489 -0.2739 0.5420 0.111 Uiso 1 1 calc R . . C33 C 0.0411(3) -0.10823(12) 0.45207(15) 0.0284(8) Uani 1 1 d . . . H33A H 0.0574 -0.1092 0.4996 0.034 Uiso 1 1 calc R . . H33B H 0.0623 -0.0782 0.4420 0.034 Uiso 1 1 calc R . . C34 C -0.0744(3) -0.11434(12) 0.41350(16) 0.0269(8) Uani 1 1 d . . . C35 C -0.1230(3) -0.10593(11) 0.34630(16) 0.0266(8) Uani 1 1 d . . . C36 C -0.2249(3) -0.12055(12) 0.30991(16) 0.0287(8) Uani 1 1 d . . . C37 C -0.2793(3) -0.14076(13) 0.34211(17) 0.0349(9) Uani 1 1 d . . . H37 H -0.3489 -0.1502 0.3173 0.042 Uiso 1 1 calc R . . C38 C -0.2353(3) -0.14785(13) 0.41000(17) 0.0346(9) Uani 1 1 d . A . C39 C -0.1332(3) -0.13458(12) 0.44370(17) 0.0325(9) Uani 1 1 d . . . H39 H -0.1014 -0.1395 0.4898 0.039 Uiso 1 1 calc R . . C40 C -0.2957(3) -0.17100(16) 0.4449(2) 0.0478(11) Uani 1 1 d . . . C41 C -0.3918(9) -0.1409(4) 0.4354(6) 0.0845(16) Uani 0.50 1 d P A 1 H41A H -0.3681 -0.1117 0.4576 0.127 Uiso 0.50 1 calc PR A 1 H41B H -0.4349 -0.1562 0.4542 0.127 Uiso 0.50 1 calc PR A 1 H41C H -0.4327 -0.1357 0.3885 0.127 Uiso 0.50 1 calc PR A 1 C42 C -0.3382(9) -0.2171(4) 0.4110(5) 0.0845(16) Uani 0.50 1 d P A 1 H42A H -0.3832 -0.2119 0.3646 0.127 Uiso 0.50 1 calc PR A 1 H42B H -0.3782 -0.2317 0.4327 0.127 Uiso 0.50 1 calc PR A 1 H42C H -0.2800 -0.2366 0.4144 0.127 Uiso 0.50 1 calc PR A 1 C43 C -0.2339(9) -0.1791(4) 0.5177(5) 0.0845(16) Uani 0.50 1 d P A 1 H43A H -0.1731 -0.1978 0.5242 0.127 Uiso 0.50 1 calc PR A 1 H43B H -0.2777 -0.1946 0.5359 0.127 Uiso 0.50 1 calc PR A 1 H43C H -0.2110 -0.1499 0.5400 0.127 Uiso 0.50 1 calc PR A 1 C41B C -0.4079(9) -0.1761(4) 0.4041(5) 0.0845(16) Uani 0.50 1 d P A 2 H41D H -0.4360 -0.1473 0.3821 0.127 Uiso 0.50 1 calc PR A 2 H41E H -0.4436 -0.1846 0.4320 0.127 Uiso 0.50 1 calc PR A 2 H41F H -0.4186 -0.1997 0.3711 0.127 Uiso 0.50 1 calc PR A 2 C42B C -0.2365(9) -0.2123(4) 0.4822(6) 0.0845(16) Uani 0.50 1 d P A 2 H42D H -0.2313 -0.2346 0.4512 0.127 Uiso 0.50 1 calc PR A 2 H42E H -0.2735 -0.2258 0.5067 0.127 Uiso 0.50 1 calc PR A 2 H42F H -0.1667 -0.2032 0.5129 0.127 Uiso 0.50 1 calc PR A 2 C43B C -0.2924(9) -0.1391(4) 0.5021(5) 0.0845(16) Uani 0.50 1 d P A 2 H43D H -0.2199 -0.1333 0.5319 0.127 Uiso 0.50 1 calc PR A 2 H43E H -0.3284 -0.1538 0.5264 0.127 Uiso 0.50 1 calc PR A 2 H43F H -0.3268 -0.1104 0.4838 0.127 Uiso 0.50 1 calc PR A 2 C44 C -0.2692(3) -0.11798(13) 0.23546(16) 0.0333(9) Uani 1 1 d . . . H44A H -0.2477 -0.0892 0.2218 0.040 Uiso 1 1 calc R . . H44B H -0.3461 -0.1186 0.2175 0.040 Uiso 1 1 calc R . . C45 C -0.2592(3) -0.09389(13) 0.09711(16) 0.0359(9) Uani 1 1 d . . . H45A H -0.2468 -0.0642 0.0809 0.043 Uiso 1 1 calc R . . H45B H -0.3080 -0.0889 0.1182 0.043 Uiso 1 1 calc R . . C46 C -0.3092(3) -0.12475(14) 0.03977(16) 0.0337(9) Uani 1 1 d . . . C47 C -0.3130(3) -0.16752(15) 0.01974(17) 0.0411(10) Uani 1 1 d . . . H47 H -0.2740 -0.1962 0.0380 0.049 Uiso 1 1 calc R . . C48 C -0.1982(4) -0.12520(17) -0.0458(2) 0.0549(12) Uani 1 1 d . . . C49 C -0.3663(4) -0.0674(2) -0.0776(3) 0.0701(15) Uani 1 1 d . . . C50 C -0.3897(4) -0.1597(2) -0.1265(2) 0.0672(15) Uani 1 1 d . . . C51 C -0.4780(3) -0.16373(16) 0.0653(2) 0.0499(11) Uani 1 1 d . . . C52 C -0.5256(3) -0.0927(2) -0.0247(2) 0.0582(13) Uani 1 1 d . . . C53 C -0.5293(4) -0.18983(19) -0.0602(2) 0.0593(13) Uani 1 1 d . . . C54 C 0.1235(3) -0.09125(12) 0.22909(18) 0.0353(9) Uani 1 1 d . . . H54A H 0.1781 -0.0833 0.2726 0.042 Uiso 1 1 calc R . . H54B H 0.0701 -0.0672 0.2169 0.042 Uiso 1 1 calc R . . C55 C 0.1708(3) -0.09102(12) 0.18046(18) 0.0343(9) Uani 1 1 d . . . C56 C 0.1770(3) -0.11422(13) 0.13020(18) 0.0379(9) Uani 1 1 d . . . H56 H 0.1503 -0.1437 0.1076 0.046 Uiso 1 1 calc R . . C57 C 0.0188(4) -0.04329(16) 0.0747(2) 0.0582(13) Uani 1 1 d . . . C58 C 0.1764(4) -0.05121(19) 0.0309(2) 0.0706(15) Uani 1 1 d . . . C59 C 0.1957(4) 0.00573(17) 0.1405(2) 0.0574(13) Uani 1 1 d . . . C60 C 0.3823(4) -0.1379(2) 0.2220(3) 0.0666(14) Uani 1 1 d . . . C61 C 0.3838(4) -0.07971(17) 0.1322(2) 0.0623(13) Uani 1 1 d . . . C62 C 0.3722(4) -0.0471(2) 0.2483(3) 0.0689(15) Uani 1 1 d . . . C63 C 0.2947(3) -0.07715(13) 0.43411(16) 0.0326(9) Uani 1 1 d . . . H63A H 0.3094 -0.0490 0.4153 0.039 Uiso 1 1 calc R . . H63B H 0.3426 -0.1009 0.4316 0.039 Uiso 1 1 calc R . . C64 C 0.3163(3) -0.06901(12) 0.50495(16) 0.0300(9) Uani 1 1 d . . . C65 C 0.2764(3) -0.07603(13) 0.54859(16) 0.0364(9) Uani 1 1 d . . . H65 H 0.2126 -0.0909 0.5486 0.044 Uiso 1 1 calc R . . C66 C 0.2198(4) 0.01423(17) 0.5024(2) 0.0649(14) Uani 1 1 d . . . C67 C 0.4347(4) 0.01813(15) 0.5535(2) 0.0470(11) Uani 1 1 d . . . C68 C 0.3327(4) 0.00586(16) 0.6357(2) 0.0541(12) Uani 1 1 d . . . C69 C 0.4213(3) -0.14706(17) 0.5703(2) 0.0551(12) Uani 1 1 d . . . C70 C 0.5498(4) -0.07414(16) 0.58919(19) 0.0537(12) Uani 1 1 d . . . C71 C 0.4515(3) -0.08702(16) 0.6764(2) 0.0560(13) Uani 1 1 d . . . C72 C -0.0345(3) -0.04042(12) 0.33127(17) 0.0344(9) Uani 1 1 d . . . H72A H 0.0422 -0.0407 0.3544 0.041 Uiso 1 1 calc R . . H72B H -0.0632 -0.0287 0.3621 0.041 Uiso 1 1 calc R . . C73 C -0.0661(3) -0.00984(12) 0.27281(17) 0.0307(9) Uani 1 1 d . . . C74 C -0.0843(3) -0.00875(12) 0.20916(17) 0.0339(9) Uani 1 1 d . . . H74 H -0.0894 -0.0313 0.1745 0.041 Uiso 1 1 calc R . . C75 C 0.1361(3) 0.01934(14) 0.2890(2) 0.0429(10) Uani 1 1 d . . . C76 C 0.0259(3) 0.08501(15) 0.3159(2) 0.0489(11) Uani 1 1 d . . . C77 C 0.0093(3) 0.07076(15) 0.1830(2) 0.0525(12) Uani 1 1 d . . . C78 C -0.2999(3) 0.00320(14) 0.18998(19) 0.0427(10) Uani 1 1 d . . . C79 C -0.1835(3) 0.05534(14) 0.2999(2) 0.0437(10) Uani 1 1 d . . . C80 C -0.2150(3) 0.07844(15) 0.1655(2) 0.0449(11) Uani 1 1 d . . . Co1 Co -0.32957(4) -0.12591(2) -0.05270(2) 0.04104(15) Uani 1 1 d . . . Co2 Co -0.45393(4) -0.14567(2) -0.00453(2) 0.04139(15) Uani 1 1 d . . . Co3 Co 0.15565(5) -0.04967(2) 0.10665(3) 0.04540(16) Uani 1 1 d . . . Co4 Co 0.31370(4) -0.08769(2) 0.18318(3) 0.04429(16) Uani 1 1 d . . . Co5 Co 0.33079(4) -0.014507(19) 0.55866(2) 0.03783(14) Uani 1 1 d . . . Co6 Co 0.42539(4) -0.087624(19) 0.58955(2) 0.03916(15) Uani 1 1 d . . . Co7 Co 0.00785(4) 0.042118(17) 0.25463(2) 0.03640(14) Uani 1 1 d . . . Co8 Co -0.17865(4) 0.033548(17) 0.22581(2) 0.03528(14) Uani 1 1 d . . . O1 O -0.16184(17) -0.11040(8) 0.14613(11) 0.0312(6) Uani 1 1 d . . . O2 O 0.07680(18) -0.13271(8) 0.23535(11) 0.0314(6) Uani 1 1 d . . . O3 O 0.18964(17) -0.09094(8) 0.39507(10) 0.0283(6) Uani 1 1 d . . . O4 O -0.07128(18) -0.08576(8) 0.31209(11) 0.0307(6) Uani 1 1 d . . . O5 O -0.1147(3) -0.12465(13) -0.03994(16) 0.0768(11) Uani 1 1 d . . . O6 O -0.3867(3) -0.03153(15) -0.0914(2) 0.1155(17) Uani 1 1 d . . . O7 O -0.4292(3) -0.18055(16) -0.17250(17) 0.1059(16) Uani 1 1 d . . . O8 O -0.4922(2) -0.17576(12) 0.10897(15) 0.0666(10) Uani 1 1 d . . . O9 O -0.5654(3) -0.05854(14) -0.03581(17) 0.0802(11) Uani 1 1 d . . . O10 O -0.5726(3) -0.21894(14) -0.09239(17) 0.0902(13) Uani 1 1 d . . . O11 O -0.0698(3) -0.03985(13) 0.05581(17) 0.0844(12) Uani 1 1 d . . . O12 O 0.1900(3) -0.05399(16) -0.01529(17) 0.1080(15) Uani 1 1 d . . . O13 O 0.2246(3) 0.04032(12) 0.16396(19) 0.0792(11) Uani 1 1 d . . . O14 O 0.4298(3) -0.16900(15) 0.2439(2) 0.1018(15) Uani 1 1 d . . . O15 O 0.4265(3) -0.07479(13) 0.09940(19) 0.0864(12) Uani 1 1 d . . . O16 O 0.4090(3) -0.02171(17) 0.2900(2) 0.1214(18) Uani 1 1 d . . . O17 O 0.1472(3) 0.03096(14) 0.4642(2) 0.1149(16) Uani 1 1 d . . . O18 O 0.5027(3) 0.03797(12) 0.55271(17) 0.0762(10) Uani 1 1 d . . . O19 O 0.3349(3) 0.01899(12) 0.68432(17) 0.0837(12) Uani 1 1 d . . . O20 O 0.4133(3) -0.18378(12) 0.55373(17) 0.0829(12) Uani 1 1 d . . . O21 O 0.6295(3) -0.06607(14) 0.58963(17) 0.0840(12) Uani 1 1 d . . . O22 O 0.4649(3) -0.08522(13) 0.73017(15) 0.0881(12) Uani 1 1 d . . . O23 O 0.2178(2) 0.00447(11) 0.31159(15) 0.0588(8) Uani 1 1 d . . . O24 O 0.0354(3) 0.11194(11) 0.35475(17) 0.0710(10) Uani 1 1 d . . . O25 O 0.0121(3) 0.08581(12) 0.13677(17) 0.0806(11) Uani 1 1 d . . . O26 O -0.3773(2) -0.01452(11) 0.16590(15) 0.0605(9) Uani 1 1 d . . . O27 O -0.1782(3) 0.06652(11) 0.35033(15) 0.0638(9) Uani 1 1 d . . . O28 O -0.2359(2) 0.10708(11) 0.12808(15) 0.0632(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0220(19) 0.033(2) 0.0238(17) -0.0031(17) 0.0047(15) -0.0060(17) C2 0.021(2) 0.040(2) 0.0243(18) -0.0045(18) 0.0038(15) 0.0004(18) C3 0.027(2) 0.039(2) 0.0284(19) -0.0039(18) 0.0107(16) -0.0029(18) C4 0.030(2) 0.040(2) 0.0284(19) 0.0000(18) 0.0084(17) -0.0020(19) C5 0.028(2) 0.038(2) 0.0308(19) -0.0054(18) 0.0090(17) 0.0003(18) C6 0.0209(19) 0.039(2) 0.0201(17) -0.0038(17) 0.0026(15) -0.0023(17) C7 0.044(3) 0.037(2) 0.044(2) 0.001(2) 0.019(2) -0.002(2) C8 0.059(3) 0.047(3) 0.106(4) -0.002(3) 0.029(3) -0.016(3) C9 0.074(3) 0.037(3) 0.068(3) 0.001(2) 0.039(3) 0.004(2) C10 0.094(4) 0.060(3) 0.069(3) 0.013(3) 0.054(3) 0.010(3) C11 0.026(2) 0.042(2) 0.0256(18) -0.0048(18) 0.0070(16) 0.0018(18) C12 0.025(2) 0.033(2) 0.0229(17) 0.0001(17) 0.0135(15) -0.0042(17) C13 0.027(2) 0.031(2) 0.0290(18) 0.0000(17) 0.0178(16) -0.0032(17) C14 0.027(2) 0.029(2) 0.0231(17) -0.0024(16) 0.0128(15) -0.0062(17) C15 0.030(2) 0.034(2) 0.0285(19) 0.0033(18) 0.0118(16) -0.0001(18) C16 0.035(2) 0.029(2) 0.0301(19) 0.0021(18) 0.0179(17) 0.0007(18) C17 0.033(2) 0.037(2) 0.0247(18) -0.0074(17) 0.0141(16) -0.0056(18) C18 0.048(3) 0.033(2) 0.037(2) -0.0038(19) 0.0130(19) 0.006(2) C19 0.055(3) 0.053(3) 0.069(3) -0.009(2) 0.031(2) 0.015(2) C20 0.089(4) 0.034(3) 0.054(3) -0.004(2) 0.028(3) 0.004(2) C21 0.068(3) 0.044(3) 0.043(2) -0.014(2) 0.020(2) 0.010(2) C22 0.027(2) 0.032(2) 0.0281(18) -0.0038(17) 0.0141(16) -0.0037(17) C23 0.0211(19) 0.036(2) 0.0222(17) -0.0049(17) 0.0064(15) -0.0026(17) C24 0.0214(19) 0.028(2) 0.0212(17) 0.0013(16) 0.0039(15) -0.0043(16) C25 0.0240(19) 0.031(2) 0.0191(16) -0.0046(16) 0.0048(15) -0.0019(17) C26 0.029(2) 0.036(2) 0.0273(18) -0.0025(18) 0.0136(16) -0.0073(18) C27 0.032(2) 0.035(2) 0.0269(18) -0.0046(18) 0.0106(17) -0.0075(18) C28 0.028(2) 0.029(2) 0.0302(19) -0.0069(17) 0.0107(16) -0.0006(17) C29 0.055(3) 0.032(2) 0.053(2) -0.005(2) 0.032(2) -0.011(2) C30 0.074(3) 0.042(3) 0.068(3) -0.003(2) 0.045(3) -0.018(2) C31 0.120(5) 0.047(3) 0.116(4) -0.033(3) 0.085(4) -0.032(3) C32 0.069(4) 0.050(3) 0.104(4) 0.038(3) 0.037(3) 0.016(3) C33 0.028(2) 0.032(2) 0.0277(18) -0.0050(17) 0.0135(16) -0.0038(17) C34 0.029(2) 0.024(2) 0.0305(19) -0.0059(17) 0.0151(16) 0.0014(16) C35 0.032(2) 0.0200(19) 0.0329(19) -0.0039(17) 0.0179(17) 0.0012(17) C36 0.030(2) 0.025(2) 0.0325(19) -0.0061(17) 0.0141(17) 0.0011(17) C37 0.028(2) 0.037(2) 0.039(2) -0.0135(19) 0.0122(17) -0.0049(18) C38 0.037(2) 0.037(2) 0.039(2) -0.0095(19) 0.0240(18) -0.0057(19) C39 0.036(2) 0.035(2) 0.0321(19) -0.0037(18) 0.0191(17) -0.0005(18) C40 0.043(3) 0.056(3) 0.048(2) -0.001(2) 0.023(2) -0.011(2) C41 0.102(4) 0.092(4) 0.094(4) -0.005(3) 0.076(3) -0.031(3) C42 0.102(4) 0.092(4) 0.094(4) -0.005(3) 0.076(3) -0.031(3) C43 0.102(4) 0.092(4) 0.094(4) -0.005(3) 0.076(3) -0.031(3) C41B 0.102(4) 0.092(4) 0.094(4) -0.005(3) 0.076(3) -0.031(3) C42B 0.102(4) 0.092(4) 0.094(4) -0.005(3) 0.076(3) -0.031(3) C43B 0.102(4) 0.092(4) 0.094(4) -0.005(3) 0.076(3) -0.031(3) C44 0.025(2) 0.038(2) 0.036(2) -0.0034(19) 0.0106(16) 0.0026(17) C45 0.033(2) 0.036(2) 0.034(2) 0.0028(19) 0.0076(17) 0.0031(18) C46 0.027(2) 0.047(3) 0.0227(18) -0.0008(19) 0.0057(16) -0.0012(19) C47 0.040(2) 0.047(3) 0.028(2) -0.001(2) 0.0056(18) 0.005(2) C48 0.053(3) 0.071(3) 0.046(2) 0.005(2) 0.025(2) 0.012(3) C49 0.062(3) 0.079(4) 0.087(4) 0.035(3) 0.048(3) 0.017(3) C50 0.048(3) 0.115(5) 0.041(3) -0.009(3) 0.020(2) 0.005(3) C51 0.038(3) 0.063(3) 0.043(2) 0.001(2) 0.011(2) -0.004(2) C52 0.034(3) 0.088(4) 0.049(3) 0.009(3) 0.013(2) 0.005(3) C53 0.048(3) 0.085(4) 0.039(2) -0.004(3) 0.013(2) -0.009(3) C54 0.038(2) 0.032(2) 0.038(2) 0.0019(18) 0.0189(18) 0.0031(19) C55 0.034(2) 0.030(2) 0.040(2) -0.0019(19) 0.0155(18) -0.0025(18) C56 0.041(2) 0.033(2) 0.042(2) -0.0024(19) 0.0198(19) -0.0051(19) C57 0.067(4) 0.060(3) 0.043(3) 0.014(2) 0.018(2) 0.003(3) C58 0.078(4) 0.086(4) 0.049(3) 0.008(3) 0.027(3) 0.011(3) C59 0.071(4) 0.048(3) 0.070(3) 0.013(3) 0.046(3) 0.001(3) C60 0.039(3) 0.079(4) 0.088(4) 0.028(3) 0.032(3) -0.001(3) C61 0.068(4) 0.062(3) 0.065(3) -0.001(3) 0.036(3) 0.005(3) C62 0.044(3) 0.097(4) 0.066(3) -0.028(3) 0.023(3) -0.011(3) C63 0.033(2) 0.036(2) 0.0309(19) -0.0029(18) 0.0147(17) -0.0090(18) C64 0.029(2) 0.029(2) 0.0301(19) -0.0067(17) 0.0108(16) -0.0077(17) C65 0.031(2) 0.043(2) 0.034(2) -0.0042(19) 0.0123(17) -0.0101(19) C66 0.060(3) 0.051(3) 0.068(3) -0.023(3) 0.011(3) -0.003(3) C67 0.052(3) 0.044(3) 0.051(2) -0.014(2) 0.027(2) -0.011(2) C68 0.065(3) 0.053(3) 0.060(3) -0.013(2) 0.041(3) -0.019(2) C69 0.056(3) 0.052(3) 0.048(3) 0.004(3) 0.012(2) 0.005(3) C70 0.048(3) 0.062(3) 0.042(2) 0.001(2) 0.009(2) 0.001(3) C71 0.055(3) 0.063(3) 0.044(3) 0.001(3) 0.014(2) -0.017(2) C72 0.034(2) 0.029(2) 0.038(2) 0.0008(19) 0.0120(17) -0.0049(18) C73 0.025(2) 0.027(2) 0.040(2) -0.0014(18) 0.0125(17) -0.0020(17) C74 0.035(2) 0.029(2) 0.037(2) -0.0074(18) 0.0143(17) -0.0067(18) C75 0.044(3) 0.037(3) 0.047(2) -0.002(2) 0.019(2) -0.013(2) C76 0.046(3) 0.044(3) 0.062(3) -0.004(2) 0.027(2) -0.013(2) C77 0.053(3) 0.046(3) 0.065(3) 0.017(3) 0.031(2) 0.007(2) C78 0.046(3) 0.039(3) 0.045(2) -0.001(2) 0.021(2) 0.009(2) C79 0.045(3) 0.037(3) 0.057(3) 0.006(2) 0.028(2) -0.002(2) C80 0.045(3) 0.044(3) 0.046(2) 0.000(2) 0.019(2) -0.001(2) Co1 0.0370(3) 0.0557(4) 0.0300(3) 0.0024(3) 0.0132(2) 0.0075(3) Co2 0.0318(3) 0.0560(4) 0.0320(3) -0.0022(3) 0.0085(2) -0.0015(3) Co3 0.0528(4) 0.0482(4) 0.0395(3) 0.0067(3) 0.0232(3) 0.0006(3) Co4 0.0408(3) 0.0483(4) 0.0505(3) 0.0005(3) 0.0254(3) -0.0023(3) Co5 0.0382(3) 0.0404(3) 0.0378(3) -0.0103(3) 0.0185(2) -0.0087(3) Co6 0.0363(3) 0.0440(4) 0.0315(3) -0.0020(3) 0.0081(2) -0.0068(3) Co7 0.0390(3) 0.0304(3) 0.0425(3) -0.0002(3) 0.0194(2) -0.0042(2) Co8 0.0369(3) 0.0316(3) 0.0385(3) 0.0006(2) 0.0166(2) 0.0019(3) O1 0.0248(14) 0.0314(15) 0.0331(13) 0.0001(12) 0.0075(11) -0.0035(11) O2 0.0331(14) 0.0311(15) 0.0343(13) -0.0053(12) 0.0182(11) 0.0009(12) O3 0.0269(14) 0.0295(15) 0.0261(12) -0.0020(11) 0.0085(10) -0.0027(11) O4 0.0378(15) 0.0237(14) 0.0375(14) -0.0036(11) 0.0223(12) -0.0062(12) O5 0.051(2) 0.097(3) 0.089(2) 0.013(2) 0.036(2) 0.015(2) O6 0.115(4) 0.085(3) 0.187(5) 0.070(3) 0.103(3) 0.045(3) O7 0.077(3) 0.180(5) 0.055(2) -0.055(3) 0.0216(19) -0.013(3) O8 0.057(2) 0.097(3) 0.0489(18) 0.0103(19) 0.0241(16) -0.0077(19) O9 0.063(2) 0.095(3) 0.087(3) 0.029(2) 0.035(2) 0.030(2) O10 0.084(3) 0.106(3) 0.066(2) -0.040(2) 0.017(2) -0.040(2) O11 0.054(2) 0.115(3) 0.075(2) 0.022(2) 0.016(2) 0.009(2) O12 0.132(4) 0.156(4) 0.054(2) 0.012(3) 0.056(2) 0.023(3) O13 0.099(3) 0.048(2) 0.113(3) 0.000(2) 0.065(2) -0.010(2) O14 0.057(2) 0.098(3) 0.160(4) 0.066(3) 0.053(3) 0.023(2) O15 0.100(3) 0.086(3) 0.113(3) 0.010(2) 0.085(3) 0.007(2) O16 0.058(3) 0.176(5) 0.118(3) -0.085(3) 0.024(2) -0.023(3) O17 0.084(3) 0.090(3) 0.117(3) -0.015(3) -0.014(3) 0.027(2) O18 0.071(2) 0.074(3) 0.100(3) -0.010(2) 0.052(2) -0.032(2) O19 0.130(3) 0.076(3) 0.077(2) -0.030(2) 0.074(2) -0.023(2) O20 0.096(3) 0.047(2) 0.075(2) -0.008(2) 0.004(2) 0.006(2) O21 0.043(2) 0.118(3) 0.094(3) -0.012(2) 0.030(2) -0.014(2) O22 0.116(3) 0.105(3) 0.0353(18) -0.002(2) 0.0222(19) -0.027(2) O23 0.045(2) 0.053(2) 0.071(2) -0.0037(17) 0.0152(17) -0.0029(16) O24 0.079(2) 0.055(2) 0.090(2) -0.033(2) 0.045(2) -0.0190(19) O25 0.083(3) 0.091(3) 0.087(2) 0.048(2) 0.054(2) 0.023(2) O26 0.0384(19) 0.059(2) 0.071(2) -0.0073(17) 0.0082(16) -0.0071(16) O27 0.085(2) 0.062(2) 0.066(2) -0.0190(18) 0.0521(19) -0.0129(19) O28 0.070(2) 0.054(2) 0.060(2) 0.0165(18) 0.0215(17) 0.0039(18) _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 C6 1.395(5) . ? C1 O1 1.396(4) . ? C1 C2 1.403(5) . ? C2 C3 1.391(5) . ? C2 C44 1.527(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.392(5) . ? C4 C7 1.535(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C11 1.521(5) . ? C7 C8 1.517(6) . ? C7 C9 1.524(5) . ? C7 C10 1.538(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.383(5) . ? C12 C13 1.393(5) . ? C13 O2 1.377(4) . ? C13 C14 1.397(5) . ? C14 C15 1.376(5) . ? C14 C22 1.518(4) . ? C15 C16 1.404(5) . ? C15 H15 0.9500 . ? C16 C17 1.395(5) . ? C16 C18 1.533(5) . ? C17 H17 0.9500 . ? C18 C19 1.536(6) . ? C18 C21 1.537(5) . ? C18 C20 1.542(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.528(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.385(5) . ? C23 C24 1.401(5) . ? C24 O3 1.389(4) . ? C24 C25 1.396(5) . ? C25 C26 1.394(5) . ? C25 C33 1.521(5) . ? C26 C27 1.392(5) . ? C26 H26 0.9500 . ? C27 C28 1.390(5) . ? C27 C29 1.524(5) . ? C28 H28 0.9500 . ? C29 C32 1.515(6) . ? C29 C30 1.528(5) . ? C29 C31 1.539(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.511(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.393(4) . ? C34 C39 1.398(5) . ? C35 O4 1.386(4) . ? C35 C36 1.399(5) . ? C36 C37 1.382(5) . ? C36 C44 1.519(4) . ? C37 C38 1.398(5) . ? C37 H37 0.9500 . ? C38 C39 1.381(5) . ? C38 C40 1.528(5) . ? C39 H39 0.9500 . ? C40 C41B 1.476(12) . ? C40 C43 1.517(11) . ? C40 C42B 1.520(12) . ? C40 C42 1.552(11) . ? C40 C41 1.562(12) . ? C40 C43B 1.572(11) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C41B H41D 0.9800 . ? C41B H41E 0.9800 . ? C41B H41F 0.9800 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 O1 1.447(4) . ? C45 C46 1.493(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.333(5) . ? C46 Co1 1.963(3) . ? C46 Co2 1.968(4) . ? C47 Co2 1.943(4) . ? C47 Co1 1.966(4) . ? C47 H47 1.0000 . ? C48 O5 1.131(5) . ? C48 Co1 1.793(5) . ? C49 O6 1.108(6) . ? C49 Co1 1.822(6) . ? C50 O7 1.130(5) . ? C50 Co1 1.812(5) . ? C51 O8 1.127(4) . ? C51 Co2 1.805(5) . ? C52 O9 1.132(5) . ? C52 Co2 1.815(6) . ? C53 O10 1.127(5) . ? C53 Co2 1.815(5) . ? C54 O2 1.423(4) . ? C54 C55 1.487(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.346(5) . ? C55 Co3 1.990(4) . ? C55 Co4 1.992(4) . ? C56 Co4 1.967(4) . ? C56 Co3 1.967(4) . ? C56 H56 1.0000 . ? C57 O11 1.147(5) . ? C57 Co3 1.773(5) . ? C58 O12 1.126(5) . ? C58 Co3 1.828(5) . ? C59 O13 1.144(5) . ? C59 Co3 1.793(5) . ? C60 O14 1.124(6) . ? C60 Co4 1.788(6) . ? C61 O15 1.130(5) . ? C61 Co4 1.800(5) . ? C62 O16 1.142(5) . ? C62 Co4 1.802(5) . ? C63 O3 1.437(4) . ? C63 C64 1.501(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.324(5) . ? C64 Co6 1.965(3) . ? C64 Co5 1.966(3) . ? C65 Co5 1.948(4) . ? C65 Co6 1.949(4) . ? C65 H65 1.0000 . ? C66 O17 1.143(5) . ? C66 Co5 1.772(5) . ? C67 O18 1.129(5) . ? C67 Co5 1.796(5) . ? C68 O19 1.141(4) . ? C68 Co5 1.809(4) . ? C69 O20 1.136(5) . ? C69 Co6 1.802(5) . ? C70 O21 1.144(5) . ? C70 Co6 1.802(5) . ? C71 O22 1.137(5) . ? C71 Co6 1.818(4) . ? C72 O4 1.436(4) . ? C72 C73 1.497(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.336(5) . ? C73 Co8 1.975(4) . ? C73 Co7 1.987(4) . ? C74 Co8 1.966(4) . ? C74 Co7 1.974(4) . ? C74 H74 1.0000 . ? C75 O23 1.140(5) . ? C75 Co7 1.783(5) . ? C76 O24 1.143(5) . ? C76 Co7 1.803(5) . ? C77 O25 1.137(5) . ? C77 Co7 1.816(5) . ? C78 O26 1.130(5) . ? C78 Co8 1.802(5) . ? C79 O27 1.146(4) . ? C79 Co8 1.799(4) . ? C80 O28 1.139(5) . ? C80 Co8 1.808(5) . ? Co1 Co2 2.4700(7) . ? Co3 Co4 2.4570(8) . ? Co5 Co6 2.4824(8) . ? Co7 Co8 2.4512(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 O1 118.7(3) . . ? C6 C1 C2 120.3(3) . . ? O1 C1 C2 120.9(3) . . ? C3 C2 C1 117.5(3) . . ? C3 C2 C44 119.5(3) . . ? C1 C2 C44 122.9(3) . . ? C4 C3 C2 123.6(3) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 116.8(4) . . ? C3 C4 C7 120.1(3) . . ? C5 C4 C7 123.1(4) . . ? C6 C5 C4 122.1(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 119.0(3) . . ? C5 C6 C11 119.7(3) . . ? C1 C6 C11 121.2(3) . . ? C8 C7 C9 108.3(4) . . ? C8 C7 C4 108.2(3) . . ? C9 C7 C4 112.5(3) . . ? C8 C7 C10 109.5(4) . . ? C9 C7 C10 107.7(3) . . ? C4 C7 C10 110.6(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 C12 110.6(3) . . ? C6 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C17 C12 C13 119.0(3) . . ? C17 C12 C11 121.4(3) . . ? C13 C12 C11 119.6(3) . . ? O2 C13 C12 117.5(3) . . ? O2 C13 C14 121.4(3) . . ? C12 C13 C14 120.9(3) . . ? C15 C14 C13 118.0(3) . . ? C15 C14 C22 120.0(3) . . ? C13 C14 C22 121.9(3) . . ? C14 C15 C16 123.1(3) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 116.7(3) . . ? C17 C16 C18 123.5(3) . . ? C15 C16 C18 119.8(3) . . ? C12 C17 C16 122.0(3) . . ? C12 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C16 C18 C19 109.6(3) . . ? C16 C18 C21 112.3(3) . . ? C19 C18 C21 107.7(3) . . ? C16 C18 C20 108.4(3) . . ? C19 C18 C20 109.7(3) . . ? C21 C18 C20 109.3(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 C23 110.2(3) . . ? C14 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? C14 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C28 C23 C24 118.5(3) . . ? C28 C23 C22 118.3(3) . . ? C24 C23 C22 123.0(3) . . ? O3 C24 C25 119.4(3) . . ? O3 C24 C23 120.2(3) . . ? C25 C24 C23 120.4(3) . . ? C26 C25 C24 118.1(3) . . ? C26 C25 C33 119.2(3) . . ? C24 C25 C33 122.7(3) . . ? C27 C26 C25 123.2(3) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C28 C27 C26 116.1(3) . . ? C28 C27 C29 119.7(3) . . ? C26 C27 C29 124.2(3) . . ? C23 C28 C27 123.2(3) . . ? C23 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? C32 C29 C27 109.3(3) . . ? C32 C29 C30 109.0(4) . . ? C27 C29 C30 112.0(3) . . ? C32 C29 C31 109.5(4) . . ? C27 C29 C31 109.1(3) . . ? C30 C29 C31 107.9(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C25 111.2(3) . . ? C34 C33 H33A 109.4 . . ? C25 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C25 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C39 117.8(3) . . ? C35 C34 C33 122.3(3) . . ? C39 C34 C33 119.4(3) . . ? O4 C35 C34 122.0(3) . . ? O4 C35 C36 117.3(3) . . ? C34 C35 C36 120.5(3) . . ? C37 C36 C35 119.2(3) . . ? C37 C36 C44 121.4(3) . . ? C35 C36 C44 119.1(3) . . ? C36 C37 C38 122.2(3) . . ? C36 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C39 C38 C37 116.8(3) . . ? C39 C38 C40 121.5(3) . . ? C37 C38 C40 121.7(3) . . ? C38 C39 C34 123.4(3) . . ? C38 C39 H39 118.3 . . ? C34 C39 H39 118.3 . . ? C41B C40 C43 130.3(6) . . ? C41B C40 C42B 117.8(7) . . ? C43 C40 C42B 48.7(6) . . ? C41B C40 C38 114.3(5) . . ? C43 C40 C38 114.8(5) . . ? C42B C40 C38 110.1(5) . . ? C41B C40 C42 60.5(6) . . ? C43 C40 C42 108.8(7) . . ? C42B C40 C42 65.2(6) . . ? C38 C40 C42 109.2(4) . . ? C41B C40 C41 47.3(6) . . ? C43 C40 C41 108.8(7) . . ? C42B C40 C41 141.5(6) . . ? C38 C40 C41 108.0(5) . . ? C42 C40 C41 107.0(7) . . ? C41B C40 C43B 103.3(7) . . ? C43 C40 C43B 53.8(6) . . ? C42B C40 C43B 101.9(6) . . ? C38 C40 C43B 107.9(5) . . ? C42 C40 C43B 142.9(6) . . ? C41 C40 C43B 60.3(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? C40 C41B H41D 109.5 . . ? C40 C41B H41E 109.5 . . ? H41D C41B H41E 109.5 . . ? C40 C41B H41F 109.5 . . ? H41D C41B H41F 109.5 . . ? H41E C41B H41F 109.5 . . ? C40 C42B H42D 109.5 . . ? C40 C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C40 C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C40 C43B H43D 109.5 . . ? C40 C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C40 C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C36 C44 C2 109.7(3) . . ? C36 C44 H44A 109.7 . . ? C2 C44 H44A 109.7 . . ? C36 C44 H44B 109.7 . . ? C2 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? O1 C45 C46 114.4(3) . . ? O1 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? O1 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C45 143.7(4) . . ? C47 C46 Co1 70.3(2) . . ? C45 C46 Co1 136.6(3) . . ? C47 C46 Co2 69.1(2) . . ? C45 C46 Co2 130.8(3) . . ? Co1 C46 Co2 77.84(12) . . ? C46 C47 Co2 71.1(2) . . ? C46 C47 Co1 70.1(2) . . ? Co2 C47 Co1 78.36(15) . . ? C46 C47 H47 136.4 . . ? Co2 C47 H47 136.4 . . ? Co1 C47 H47 136.4 . . ? O5 C48 Co1 178.5(4) . . ? O6 C49 Co1 178.3(7) . . ? O7 C50 Co1 178.5(4) . . ? O8 C51 Co2 178.7(5) . . ? O9 C52 Co2 176.4(5) . . ? O10 C53 Co2 176.2(5) . . ? O2 C54 C55 116.0(3) . . ? O2 C54 H54A 108.3 . . ? C55 C54 H54A 108.3 . . ? O2 C54 H54B 108.3 . . ? C55 C54 H54B 108.3 . . ? H54A C54 H54B 107.4 . . ? C56 C55 C54 143.6(4) . . ? C56 C55 Co3 69.2(2) . . ? C54 C55 Co3 132.6(3) . . ? C56 C55 Co4 69.1(2) . . ? C54 C55 Co4 136.6(3) . . ? Co3 C55 Co4 76.20(13) . . ? C55 C56 Co4 71.1(2) . . ? C55 C56 Co3 71.0(2) . . ? Co4 C56 Co3 77.30(14) . . ? C55 C56 H56 136.4 . . ? Co4 C56 H56 136.4 . . ? Co3 C56 H56 136.4 . . ? O11 C57 Co3 177.7(4) . . ? O12 C58 Co3 177.2(5) . . ? O13 C59 Co3 177.3(5) . . ? O14 C60 Co4 174.9(5) . . ? O15 C61 Co4 179.0(5) . . ? O16 C62 Co4 179.1(5) . . ? O3 C63 C64 113.6(3) . . ? O3 C63 H63A 108.9 . . ? C64 C63 H63A 108.9 . . ? O3 C63 H63B 108.9 . . ? C64 C63 H63B 108.9 . . ? H63A C63 H63B 107.7 . . ? C65 C64 C63 141.6(3) . . ? C65 C64 Co6 69.6(2) . . ? C63 C64 Co6 135.2(3) . . ? C65 C64 Co5 69.5(2) . . ? C63 C64 Co5 134.3(3) . . ? Co6 C64 Co5 78.31(12) . . ? C64 C65 Co5 71.0(2) . . ? C64 C65 Co6 70.9(2) . . ? Co5 C65 Co6 79.13(14) . . ? C64 C65 H65 136.0 . . ? Co5 C65 H65 136.0 . . ? Co6 C65 H65 136.0 . . ? O17 C66 Co5 176.7(4) . . ? O18 C67 Co5 177.2(4) . . ? O19 C68 Co5 179.2(4) . . ? O20 C69 Co6 175.0(4) . . ? O21 C70 Co6 179.0(5) . . ? O22 C71 Co6 177.2(5) . . ? O4 C72 C73 111.1(3) . . ? O4 C72 H72A 109.4 . . ? C73 C72 H72A 109.4 . . ? O4 C72 H72B 109.4 . . ? C73 C72 H72B 109.4 . . ? H72A C72 H72B 108.0 . . ? C74 C73 C72 143.1(3) . . ? C74 C73 Co8 69.8(2) . . ? C72 C73 Co8 138.0(3) . . ? C74 C73 Co7 69.8(2) . . ? C72 C73 Co7 130.4(3) . . ? Co8 C73 Co7 76.45(13) . . ? C73 C74 Co8 70.5(2) . . ? C73 C74 Co7 70.8(2) . . ? Co8 C74 Co7 76.94(13) . . ? C73 C74 H74 136.7 . . ? Co8 C74 H74 136.7 . . ? Co7 C74 H74 136.7 . . ? O23 C75 Co7 179.1(4) . . ? O24 C76 Co7 178.5(4) . . ? O25 C77 Co7 175.1(4) . . ? O26 C78 Co8 177.4(4) . . ? O27 C79 Co8 173.2(4) . . ? O28 C80 Co8 178.6(4) . . ? C48 Co1 C50 99.7(2) . . ? C48 Co1 C49 99.8(2) . . ? C50 Co1 C49 106.0(3) . . ? C48 Co1 C46 101.86(16) . . ? C50 Co1 C46 141.0(2) . . ? C49 Co1 C46 101.8(2) . . ? C48 Co1 C47 99.43(18) . . ? C50 Co1 C47 104.9(2) . . ? C49 Co1 C47 140.0(2) . . ? C46 Co1 C47 39.66(15) . . ? C48 Co1 Co2 148.82(14) . . ? C50 Co1 Co2 96.50(15) . . ? C49 Co1 Co2 101.09(15) . . ? C46 Co1 Co2 51.17(11) . . ? C47 Co1 Co2 50.41(11) . . ? C51 Co2 C53 96.6(2) . . ? C51 Co2 C52 100.8(2) . . ? C53 Co2 C52 109.7(2) . . ? C51 Co2 C47 101.06(18) . . ? C53 Co2 C47 101.47(19) . . ? C52 Co2 C47 139.2(2) . . ? C51 Co2 C46 100.38(16) . . ? C53 Co2 C46 140.04(19) . . ? C52 Co2 C46 102.25(19) . . ? C47 Co2 C46 39.84(15) . . ? C51 Co2 Co1 149.49(13) . . ? C53 Co2 Co1 101.14(14) . . ? C52 Co2 Co1 96.34(15) . . ? C47 Co2 Co1 51.23(11) . . ? C46 Co2 Co1 50.99(10) . . ? C57 Co3 C59 100.2(2) . . ? C57 Co3 C58 100.9(2) . . ? C59 Co3 C58 105.6(2) . . ? C57 Co3 C56 103.48(19) . . ? C59 Co3 C56 141.61(19) . . ? C58 Co3 C56 99.1(2) . . ? C57 Co3 C55 97.50(18) . . ? C59 Co3 C55 107.61(17) . . ? C58 Co3 C55 138.2(2) . . ? C56 Co3 C55 39.78(14) . . ? C57 Co3 Co4 149.06(14) . . ? C59 Co3 Co4 94.80(16) . . ? C58 Co3 Co4 100.91(16) . . ? C56 Co3 Co4 51.34(11) . . ? C55 Co3 Co4 51.94(11) . . ? C60 Co4 C61 95.0(2) . . ? C60 Co4 C62 100.5(2) . . ? C61 Co4 C62 103.5(2) . . ? C60 Co4 C56 99.49(19) . . ? C61 Co4 C56 109.17(19) . . ? C62 Co4 C56 139.79(19) . . ? C60 Co4 C55 108.31(18) . . ? C61 Co4 C55 142.69(19) . . ? C62 Co4 C55 100.52(18) . . ? C56 Co4 C55 39.75(14) . . ? C60 Co4 Co3 150.82(16) . . ? C61 Co4 Co3 94.41(16) . . ? C62 Co4 Co3 104.10(17) . . ? C56 Co4 Co3 51.36(11) . . ? C55 Co4 Co3 51.85(11) . . ? C66 Co5 C67 101.9(2) . . ? C66 Co5 C68 100.4(2) . . ? C67 Co5 C68 100.67(18) . . ? C66 Co5 C65 99.92(19) . . ? C67 Co5 C65 141.80(18) . . ? C68 Co5 C65 105.79(17) . . ? C66 Co5 C64 96.78(18) . . ? C67 Co5 C64 106.58(16) . . ? C68 Co5 C64 143.88(18) . . ? C65 Co5 C64 39.53(14) . . ? C66 Co5 Co6 146.31(15) . . ? C67 Co5 Co6 97.15(14) . . ? C68 Co5 Co6 103.12(16) . . ? C65 Co5 Co6 50.45(11) . . ? C64 Co5 Co6 50.83(10) . . ? C70 Co6 C69 98.7(2) . . ? C70 Co6 C71 103.18(19) . . ? C69 Co6 C71 103.7(2) . . ? C70 Co6 C65 145.49(18) . . ? C69 Co6 C65 97.79(18) . . ? C71 Co6 C65 102.06(18) . . ? C70 Co6 C64 108.44(17) . . ? C69 Co6 C64 96.14(17) . . ? C71 Co6 C64 139.40(18) . . ? C65 Co6 C64 39.53(14) . . ? C70 Co6 Co5 102.73(15) . . ? C69 Co6 Co5 145.00(14) . . ? C71 Co6 Co5 98.03(16) . . ? C65 Co6 Co5 50.42(12) . . ? C64 Co6 Co5 50.86(10) . . ? C75 Co7 C76 97.65(19) . . ? C75 Co7 C77 100.44(19) . . ? C76 Co7 C77 106.9(2) . . ? C75 Co7 C74 105.89(17) . . ? C76 Co7 C74 141.60(17) . . ? C77 Co7 C74 98.24(18) . . ? C75 Co7 C73 98.36(16) . . ? C76 Co7 C73 108.14(17) . . ? C77 Co7 C73 137.25(18) . . ? C74 Co7 C73 39.43(14) . . ? C75 Co7 Co8 149.86(13) . . ? C76 Co7 Co8 94.39(13) . . ? C77 Co7 Co8 102.30(14) . . ? C74 Co7 Co8 51.39(11) . . ? C73 Co7 Co8 51.55(10) . . ? C79 Co8 C78 101.61(18) . . ? C79 Co8 C80 108.42(18) . . ? C78 Co8 C80 96.01(18) . . ? C79 Co8 C74 132.98(17) . . ? C78 Co8 C74 101.09(16) . . ? C80 Co8 C74 109.45(17) . . ? C79 Co8 C73 93.85(17) . . ? C78 Co8 C73 108.91(16) . . ? C80 Co8 C73 142.48(17) . . ? C74 Co8 C73 39.64(14) . . ? C79 Co8 Co7 99.20(13) . . ? C78 Co8 Co7 152.76(13) . . ? C80 Co8 Co7 93.87(13) . . ? C74 Co8 Co7 51.67(10) . . ? C73 Co8 Co7 52.00(10) . . ? C1 O1 C45 112.6(3) . . ? C13 O2 C54 118.1(3) . . ? C24 O3 C63 113.7(3) . . ? C35 O4 C72 116.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -8.8(5) . . . . ? O1 C1 C2 C3 172.2(3) . . . . ? C6 C1 C2 C44 167.6(3) . . . . ? O1 C1 C2 C44 -11.4(5) . . . . ? C1 C2 C3 C4 3.2(5) . . . . ? C44 C2 C3 C4 -173.3(3) . . . . ? C2 C3 C4 C5 3.5(5) . . . . ? C2 C3 C4 C7 -176.1(3) . . . . ? C3 C4 C5 C6 -4.8(5) . . . . ? C7 C4 C5 C6 174.7(3) . . . . ? C4 C5 C6 C1 -0.6(5) . . . . ? C4 C5 C6 C11 178.3(3) . . . . ? O1 C1 C6 C5 -173.4(3) . . . . ? C2 C1 C6 C5 7.6(5) . . . . ? O1 C1 C6 C11 7.7(5) . . . . ? C2 C1 C6 C11 -171.3(3) . . . . ? C3 C4 C7 C8 67.4(5) . . . . ? C5 C4 C7 C8 -112.1(4) . . . . ? C3 C4 C7 C9 -173.0(3) . . . . ? C5 C4 C7 C9 7.4(5) . . . . ? C3 C4 C7 C10 -52.6(5) . . . . ? C5 C4 C7 C10 127.9(4) . . . . ? C5 C6 C11 C12 -61.7(4) . . . . ? C1 C6 C11 C12 117.2(4) . . . . ? C6 C11 C12 C17 106.3(4) . . . . ? C6 C11 C12 C13 -71.4(4) . . . . ? C17 C12 C13 O2 179.4(3) . . . . ? C11 C12 C13 O2 -2.8(5) . . . . ? C17 C12 C13 C14 -4.9(5) . . . . ? C11 C12 C13 C14 172.9(3) . . . . ? O2 C13 C14 C15 -178.9(3) . . . . ? C12 C13 C14 C15 5.6(5) . . . . ? O2 C13 C14 C22 5.1(5) . . . . ? C12 C13 C14 C22 -170.4(3) . . . . ? C13 C14 C15 C16 -1.9(5) . . . . ? C22 C14 C15 C16 174.2(3) . . . . ? C14 C15 C16 C17 -2.5(5) . . . . ? C14 C15 C16 C18 177.8(3) . . . . ? C13 C12 C17 C16 0.3(5) . . . . ? C11 C12 C17 C16 -177.4(3) . . . . ? C15 C16 C17 C12 3.3(5) . . . . ? C18 C16 C17 C12 -177.0(3) . . . . ? C17 C16 C18 C19 124.7(4) . . . . ? C15 C16 C18 C19 -55.7(4) . . . . ? C17 C16 C18 C21 5.1(5) . . . . ? C15 C16 C18 C21 -175.3(3) . . . . ? C17 C16 C18 C20 -115.7(4) . . . . ? C15 C16 C18 C20 63.9(4) . . . . ? C15 C14 C22 C23 -104.2(4) . . . . ? C13 C14 C22 C23 71.7(4) . . . . ? C14 C22 C23 C28 57.7(4) . . . . ? C14 C22 C23 C24 -117.6(4) . . . . ? C28 C23 C24 O3 174.8(3) . . . . ? C22 C23 C24 O3 -9.9(5) . . . . ? C28 C23 C24 C25 -6.6(5) . . . . ? C22 C23 C24 C25 168.7(3) . . . . ? O3 C24 C25 C26 -176.5(3) . . . . ? C23 C24 C25 C26 4.8(5) . . . . ? O3 C24 C25 C33 6.6(5) . . . . ? C23 C24 C25 C33 -172.0(3) . . . . ? C24 C25 C26 C27 1.2(5) . . . . ? C33 C25 C26 C27 178.2(3) . . . . ? C25 C26 C27 C28 -5.2(5) . . . . ? C25 C26 C27 C29 175.9(3) . . . . ? C24 C23 C28 C27 2.4(5) . . . . ? C22 C23 C28 C27 -173.1(3) . . . . ? C26 C27 C28 C23 3.4(5) . . . . ? C29 C27 C28 C23 -177.7(3) . . . . ? C28 C27 C29 C32 68.9(4) . . . . ? C26 C27 C29 C32 -112.2(4) . . . . ? C28 C27 C29 C30 -170.2(3) . . . . ? C26 C27 C29 C30 8.7(5) . . . . ? C28 C27 C29 C31 -50.8(5) . . . . ? C26 C27 C29 C31 128.1(4) . . . . ? C26 C25 C33 C34 -61.4(4) . . . . ? C24 C25 C33 C34 115.4(3) . . . . ? C25 C33 C34 C35 -71.6(4) . . . . ? C25 C33 C34 C39 100.0(4) . . . . ? C39 C34 C35 O4 179.6(3) . . . . ? C33 C34 C35 O4 -8.7(5) . . . . ? C39 C34 C35 C36 -4.8(5) . . . . ? C33 C34 C35 C36 166.9(3) . . . . ? O4 C35 C36 C37 -179.9(3) . . . . ? C34 C35 C36 C37 4.3(5) . . . . ? O4 C35 C36 C44 6.0(5) . . . . ? C34 C35 C36 C44 -169.8(3) . . . . ? C35 C36 C37 C38 -1.1(5) . . . . ? C44 C36 C37 C38 172.9(3) . . . . ? C36 C37 C38 C39 -1.5(5) . . . . ? C36 C37 C38 C40 -178.9(4) . . . . ? C37 C38 C39 C34 0.9(5) . . . . ? C40 C38 C39 C34 178.4(4) . . . . ? C35 C34 C39 C38 2.2(5) . . . . ? C33 C34 C39 C38 -169.8(3) . . . . ? C39 C38 C40 C41B 170.4(7) . . . . ? C37 C38 C40 C41B -12.2(8) . . . . ? C39 C38 C40 C43 -1.6(8) . . . . ? C37 C38 C40 C43 175.7(6) . . . . ? C39 C38 C40 C42B -54.3(7) . . . . ? C37 C38 C40 C42B 123.0(6) . . . . ? C39 C38 C40 C42 -124.1(6) . . . . ? C37 C38 C40 C42 53.2(7) . . . . ? C39 C38 C40 C41 119.9(6) . . . . ? C37 C38 C40 C41 -62.8(7) . . . . ? C39 C38 C40 C43B 56.1(7) . . . . ? C37 C38 C40 C43B -126.5(6) . . . . ? C37 C36 C44 C2 -94.3(4) . . . . ? C35 C36 C44 C2 79.7(4) . . . . ? C3 C2 C44 C36 56.2(4) . . . . ? C1 C2 C44 C36 -120.1(3) . . . . ? O1 C45 C46 C47 21.2(7) . . . . ? O1 C45 C46 Co1 -106.3(4) . . . . ? O1 C45 C46 Co2 133.3(3) . . . . ? C45 C46 C47 Co2 131.3(6) . . . . ? Co1 C46 C47 Co2 -84.12(10) . . . . ? C45 C46 C47 Co1 -144.6(6) . . . . ? Co2 C46 C47 Co1 84.12(10) . . . . ? O2 C54 C55 C56 12.8(8) . . . . ? O2 C54 C55 Co3 128.7(3) . . . . ? O2 C54 C55 Co4 -111.2(4) . . . . ? C54 C55 C56 Co4 -142.4(6) . . . . ? Co3 C55 C56 Co4 82.64(11) . . . . ? C54 C55 C56 Co3 134.9(6) . . . . ? Co4 C55 C56 Co3 -82.64(11) . . . . ? O3 C63 C64 C65 13.4(7) . . . . ? O3 C63 C64 Co6 131.6(3) . . . . ? O3 C63 C64 Co5 -103.0(4) . . . . ? C63 C64 C65 Co5 -136.8(6) . . . . ? Co6 C64 C65 Co5 84.74(10) . . . . ? C63 C64 C65 Co6 138.5(6) . . . . ? Co5 C64 C65 Co6 -84.74(10) . . . . ? O4 C72 C73 C74 -32.6(7) . . . . ? O4 C72 C73 Co8 96.0(4) . . . . ? O4 C72 C73 Co7 -144.9(3) . . . . ? C72 C73 C74 Co8 146.2(5) . . . . ? Co7 C73 C74 Co8 -82.49(11) . . . . ? C72 C73 C74 Co7 -131.4(5) . . . . ? Co8 C73 C74 Co7 82.49(11) . . . . ? C47 C46 Co1 C48 -90.5(3) . . . . ? C45 C46 Co1 C48 59.5(4) . . . . ? Co2 C46 Co1 C48 -162.40(18) . . . . ? C47 C46 Co1 C50 31.7(4) . . . . ? C45 C46 Co1 C50 -178.2(4) . . . . ? Co2 C46 Co1 C50 -40.1(3) . . . . ? C47 C46 Co1 C49 166.7(3) . . . . ? C45 C46 Co1 C49 -43.3(4) . . . . ? Co2 C46 Co1 C49 94.80(19) . . . . ? C45 C46 Co1 C47 150.1(5) . . . . ? Co2 C46 Co1 C47 -71.9(2) . . . . ? C47 C46 Co1 Co2 71.9(2) . . . . ? C45 C46 Co1 Co2 -138.1(5) . . . . ? C46 C47 Co1 C48 97.2(3) . . . . ? Co2 C47 Co1 C48 171.14(17) . . . . ? C46 C47 Co1 C50 -160.0(2) . . . . ? Co2 C47 Co1 C50 -86.08(18) . . . . ? C46 C47 Co1 C49 -20.5(4) . . . . ? Co2 C47 Co1 C49 53.4(3) . . . . ? Co2 C47 Co1 C46 73.9(2) . . . . ? C46 C47 Co1 Co2 -73.9(2) . . . . ? C46 C47 Co2 C51 -93.0(3) . . . . ? Co1 C47 Co2 C51 -165.69(16) . . . . ? C46 C47 Co2 C53 167.8(2) . . . . ? Co1 C47 Co2 C53 95.16(18) . . . . ? C46 C47 Co2 C52 28.2(4) . . . . ? Co1 C47 Co2 C52 -44.5(3) . . . . ? Co1 C47 Co2 C46 -72.7(2) . . . . ? C46 C47 Co2 Co1 72.7(2) . . . . ? C47 C46 Co2 C51 94.9(3) . . . . ? C45 C46 Co2 C51 -49.1(4) . . . . ? Co1 C46 Co2 C51 168.19(17) . . . . ? C47 C46 Co2 C53 -18.7(4) . . . . ? C45 C46 Co2 C53 -162.8(3) . . . . ? Co1 C46 Co2 C53 54.6(3) . . . . ? C47 C46 Co2 C52 -161.6(2) . . . . ? C45 C46 Co2 C52 54.4(4) . . . . ? Co1 C46 Co2 C52 -88.26(18) . . . . ? C45 C46 Co2 C47 -144.0(5) . . . . ? Co1 C46 Co2 C47 73.3(2) . . . . ? C47 C46 Co2 Co1 -73.3(2) . . . . ? C45 C46 Co2 Co1 142.7(4) . . . . ? C48 Co1 Co2 C51 11.5(4) . . . . ? C50 Co1 Co2 C51 132.5(3) . . . . ? C49 Co1 Co2 C51 -119.7(4) . . . . ? C46 Co1 Co2 C51 -23.4(3) . . . . ? C47 Co1 Co2 C51 28.5(3) . . . . ? C48 Co1 Co2 C53 -112.9(3) . . . . ? C50 Co1 Co2 C53 8.2(2) . . . . ? C49 Co1 Co2 C53 115.9(2) . . . . ? C46 Co1 Co2 C53 -147.8(2) . . . . ? C47 Co1 Co2 C53 -95.8(2) . . . . ? C48 Co1 Co2 C52 135.5(3) . . . . ? C50 Co1 Co2 C52 -103.4(2) . . . . ? C49 Co1 Co2 C52 4.3(2) . . . . ? C46 Co1 Co2 C52 100.6(2) . . . . ? C47 Co1 Co2 C52 152.6(2) . . . . ? C48 Co1 Co2 C47 -17.1(3) . . . . ? C50 Co1 Co2 C47 104.0(2) . . . . ? C49 Co1 Co2 C47 -148.3(2) . . . . ? C46 Co1 Co2 C47 -51.92(19) . . . . ? C48 Co1 Co2 C46 34.9(3) . . . . ? C50 Co1 Co2 C46 155.9(2) . . . . ? C49 Co1 Co2 C46 -96.3(2) . . . . ? C47 Co1 Co2 C46 51.92(19) . . . . ? C55 C56 Co3 C57 -85.5(3) . . . . ? Co4 C56 Co3 C57 -159.69(16) . . . . ? C55 C56 Co3 C59 41.0(4) . . . . ? Co4 C56 Co3 C59 -33.2(3) . . . . ? C55 C56 Co3 C58 170.9(3) . . . . ? Co4 C56 Co3 C58 96.74(18) . . . . ? Co4 C56 Co3 C55 -74.2(2) . . . . ? C55 C56 Co3 Co4 74.2(2) . . . . ? C56 C55 Co3 C57 102.1(3) . . . . ? C54 C55 Co3 C57 -43.1(4) . . . . ? Co4 C55 Co3 C57 174.64(17) . . . . ? C56 C55 Co3 C59 -154.7(3) . . . . ? C54 C55 Co3 C59 60.1(4) . . . . ? Co4 C55 Co3 C59 -82.13(19) . . . . ? C56 C55 Co3 C58 -13.5(4) . . . . ? C54 C55 Co3 C58 -158.7(4) . . . . ? Co4 C55 Co3 C58 59.0(3) . . . . ? C54 C55 Co3 C56 -145.2(5) . . . . ? Co4 C55 Co3 C56 72.6(2) . . . . ? C56 C55 Co3 Co4 -72.6(2) . . . . ? C54 C55 Co3 Co4 142.2(4) . . . . ? C55 C56 Co4 C60 107.3(3) . . . . ? Co3 C56 Co4 C60 -178.70(18) . . . . ? C55 C56 Co4 C61 -154.0(3) . . . . ? Co3 C56 Co4 C61 -80.0(2) . . . . ? C55 C56 Co4 C62 -11.6(4) . . . . ? Co3 C56 Co4 C62 62.4(3) . . . . ? Co3 C56 Co4 C55 74.0(2) . . . . ? C55 C56 Co4 Co3 -74.0(2) . . . . ? C56 C55 Co4 C60 -82.7(3) . . . . ? C54 C55 Co4 C60 65.5(4) . . . . ? Co3 C55 Co4 C60 -155.4(2) . . . . ? C56 C55 Co4 C61 43.1(4) . . . . ? C54 C55 Co4 C61 -168.7(4) . . . . ? Co3 C55 Co4 C61 -29.6(3) . . . . ? C56 C55 Co4 C62 172.4(3) . . . . ? C54 C55 Co4 C62 -39.3(4) . . . . ? Co3 C55 Co4 C62 99.7(2) . . . . ? C54 C55 Co4 C56 148.3(5) . . . . ? Co3 C55 Co4 C56 -72.7(2) . . . . ? C56 C55 Co4 Co3 72.7(2) . . . . ? C54 C55 Co4 Co3 -139.0(4) . . . . ? C57 Co3 Co4 C60 43.7(5) . . . . ? C59 Co3 Co4 C60 162.7(4) . . . . ? C58 Co3 Co4 C60 -90.3(4) . . . . ? C56 Co3 Co4 C60 2.6(4) . . . . ? C55 Co3 Co4 C60 54.0(4) . . . . ? C57 Co3 Co4 C61 152.1(3) . . . . ? C59 Co3 Co4 C61 -88.8(2) . . . . ? C58 Co3 Co4 C61 18.1(2) . . . . ? C56 Co3 Co4 C61 111.1(2) . . . . ? C55 Co3 Co4 C61 162.5(2) . . . . ? C57 Co3 Co4 C62 -102.8(3) . . . . ? C59 Co3 Co4 C62 16.2(2) . . . . ? C58 Co3 Co4 C62 123.2(2) . . . . ? C56 Co3 Co4 C62 -143.8(2) . . . . ? C55 Co3 Co4 C62 -92.4(2) . . . . ? C57 Co3 Co4 C56 41.0(3) . . . . ? C59 Co3 Co4 C56 160.07(19) . . . . ? C58 Co3 Co4 C56 -93.0(2) . . . . ? C55 Co3 Co4 C56 51.42(18) . . . . ? C57 Co3 Co4 C55 -10.4(3) . . . . ? C59 Co3 Co4 C55 108.65(19) . . . . ? C58 Co3 Co4 C55 -144.4(2) . . . . ? C56 Co3 Co4 C55 -51.42(18) . . . . ? C64 C65 Co5 C66 88.6(3) . . . . ? Co6 C65 Co5 C66 162.00(18) . . . . ? C64 C65 Co5 C67 -35.4(4) . . . . ? Co6 C65 Co5 C67 38.0(3) . . . . ? C64 C65 Co5 C68 -167.5(2) . . . . ? Co6 C65 Co5 C68 -94.15(19) . . . . ? Co6 C65 Co5 C64 73.4(2) . . . . ? C64 C65 Co5 Co6 -73.4(2) . . . . ? C65 C64 Co5 C66 -97.4(3) . . . . ? C63 C64 Co5 C66 46.2(4) . . . . ? Co6 C64 Co5 C66 -169.75(19) . . . . ? C65 C64 Co5 C67 158.0(2) . . . . ? C63 C64 Co5 C67 -58.4(4) . . . . ? Co6 C64 Co5 C67 85.69(17) . . . . ? C65 C64 Co5 C68 20.7(4) . . . . ? C63 C64 Co5 C68 164.2(4) . . . . ? Co6 C64 Co5 C68 -51.7(3) . . . . ? C63 C64 Co5 C65 143.6(5) . . . . ? Co6 C64 Co5 C65 -72.4(2) . . . . ? C65 C64 Co5 Co6 72.4(2) . . . . ? C63 C64 Co5 Co6 -144.1(4) . . . . ? C64 C65 Co6 C70 27.7(4) . . . . ? Co5 C65 Co6 C70 -45.8(3) . . . . ? C64 C65 Co6 C69 -90.2(3) . . . . ? Co5 C65 Co6 C69 -163.65(16) . . . . ? C64 C65 Co6 C71 163.9(3) . . . . ? Co5 C65 Co6 C71 90.49(18) . . . . ? Co5 C65 Co6 C64 -73.4(2) . . . . ? C64 C65 Co6 Co5 73.4(2) . . . . ? C65 C64 Co6 C70 -163.9(3) . . . . ? C63 C64 Co6 C70 51.8(4) . . . . ? Co5 C64 Co6 C70 -91.61(18) . . . . ? C65 C64 Co6 C69 94.8(3) . . . . ? C63 C64 Co6 C69 -49.5(4) . . . . ? Co5 C64 Co6 C69 167.10(17) . . . . ? C65 C64 Co6 C71 -24.6(4) . . . . ? C63 C64 Co6 C71 -168.9(3) . . . . ? Co5 C64 Co6 C71 47.7(3) . . . . ? C63 C64 Co6 C65 -144.3(5) . . . . ? Co5 C64 Co6 C65 72.3(2) . . . . ? C65 C64 Co6 Co5 -72.3(2) . . . . ? C63 C64 Co6 Co5 143.4(4) . . . . ? C66 Co5 Co6 C70 122.1(3) . . . . ? C67 Co5 Co6 C70 -2.05(19) . . . . ? C68 Co5 Co6 C70 -104.81(19) . . . . ? C65 Co5 Co6 C70 155.41(19) . . . . ? C64 Co5 Co6 C70 103.54(19) . . . . ? C66 Co5 Co6 C69 -4.2(4) . . . . ? C67 Co5 Co6 C69 -128.4(3) . . . . ? C68 Co5 Co6 C69 128.9(3) . . . . ? C65 Co5 Co6 C69 29.1(3) . . . . ? C64 Co5 Co6 C69 -22.8(3) . . . . ? C66 Co5 Co6 C71 -132.3(3) . . . . ? C67 Co5 Co6 C71 103.49(19) . . . . ? C68 Co5 Co6 C71 0.7(2) . . . . ? C65 Co5 Co6 C71 -99.05(19) . . . . ? C64 Co5 Co6 C71 -150.92(19) . . . . ? C66 Co5 Co6 C65 -33.3(3) . . . . ? C67 Co5 Co6 C65 -157.46(18) . . . . ? C68 Co5 Co6 C65 99.78(19) . . . . ? C64 Co5 Co6 C65 -51.87(18) . . . . ? C66 Co5 Co6 C64 18.6(3) . . . . ? C67 Co5 Co6 C64 -105.59(18) . . . . ? C68 Co5 Co6 C64 151.65(19) . . . . ? C65 Co5 Co6 C64 51.87(18) . . . . ? C73 C74 Co7 C75 83.8(2) . . . . ? Co8 C74 Co7 C75 157.42(15) . . . . ? C73 C74 Co7 C76 -41.8(4) . . . . ? Co8 C74 Co7 C76 31.8(3) . . . . ? C73 C74 Co7 C77 -172.8(2) . . . . ? Co8 C74 Co7 C77 -99.20(16) . . . . ? Co8 C74 Co7 C73 73.6(2) . . . . ? C73 C74 Co7 Co8 -73.6(2) . . . . ? C74 C73 Co7 C75 -104.9(2) . . . . ? C72 C73 Co7 C75 38.8(4) . . . . ? Co8 C73 Co7 C75 -178.11(15) . . . . ? C74 C73 Co7 C76 154.2(2) . . . . ? C72 C73 Co7 C76 -62.1(4) . . . . ? Co8 C73 Co7 C76 80.95(17) . . . . ? C74 C73 Co7 C77 10.5(3) . . . . ? C72 C73 Co7 C77 154.2(3) . . . . ? Co8 C73 Co7 C77 -62.7(3) . . . . ? C72 C73 Co7 C74 143.7(5) . . . . ? Co8 C73 Co7 C74 -73.2(2) . . . . ? C74 C73 Co7 Co8 73.2(2) . . . . ? C72 C73 Co7 Co8 -143.1(4) . . . . ? C73 C74 Co8 C79 11.2(3) . . . . ? Co7 C74 Co8 C79 -62.7(2) . . . . ? C73 C74 Co8 C78 -106.3(2) . . . . ? Co7 C74 Co8 C78 179.68(14) . . . . ? C73 C74 Co8 C80 153.2(2) . . . . ? Co7 C74 Co8 C80 79.17(17) . . . . ? Co7 C74 Co8 C73 -74.0(2) . . . . ? C73 C74 Co8 Co7 74.0(2) . . . . ? C74 C73 Co8 C79 -171.8(2) . . . . ? C72 C73 Co8 C79 38.2(4) . . . . ? Co7 C73 Co8 C79 -98.67(15) . . . . ? C74 C73 Co8 C78 84.6(2) . . . . ? C72 C73 Co8 C78 -65.5(4) . . . . ? Co7 C73 Co8 C78 157.66(14) . . . . ? C74 C73 Co8 C80 -44.3(4) . . . . ? C72 C73 Co8 C80 165.6(4) . . . . ? Co7 C73 Co8 C80 28.8(3) . . . . ? C72 C73 Co8 C74 -150.0(5) . . . . ? Co7 C73 Co8 C74 73.1(2) . . . . ? C74 C73 Co8 Co7 -73.1(2) . . . . ? C72 C73 Co8 Co7 136.9(4) . . . . ? C75 Co7 Co8 C79 91.4(3) . . . . ? C76 Co7 Co8 C79 -22.04(19) . . . . ? C77 Co7 Co8 C79 -130.4(2) . . . . ? C74 Co7 Co8 C79 138.79(19) . . . . ? C73 Co7 Co8 C79 87.70(18) . . . . ? C75 Co7 Co8 C78 -48.0(4) . . . . ? C76 Co7 Co8 C78 -161.5(3) . . . . ? C77 Co7 Co8 C78 90.1(3) . . . . ? C74 Co7 Co8 C78 -0.7(3) . . . . ? C73 Co7 Co8 C78 -51.8(3) . . . . ? C75 Co7 Co8 C80 -159.2(3) . . . . ? C76 Co7 Co8 C80 87.34(19) . . . . ? C77 Co7 Co8 C80 -21.1(2) . . . . ? C74 Co7 Co8 C80 -111.83(19) . . . . ? C73 Co7 Co8 C80 -162.92(18) . . . . ? C75 Co7 Co8 C74 -47.4(3) . . . . ? C76 Co7 Co8 C74 -160.83(19) . . . . ? C77 Co7 Co8 C74 90.8(2) . . . . ? C73 Co7 Co8 C74 -51.09(18) . . . . ? C75 Co7 Co8 C73 3.7(3) . . . . ? C76 Co7 Co8 C73 -109.74(19) . . . . ? C77 Co7 Co8 C73 141.9(2) . . . . ? C74 Co7 Co8 C73 51.09(18) . . . . ? C6 C1 O1 C45 114.3(3) . . . . ? C2 C1 O1 C45 -66.7(4) . . . . ? C46 C45 O1 C1 -57.3(4) . . . . ? C12 C13 O2 C54 -112.5(3) . . . . ? C14 C13 O2 C54 71.9(4) . . . . ? C55 C54 O2 C13 33.7(4) . . . . ? C25 C24 O3 C63 111.9(3) . . . . ? C23 C24 O3 C63 -69.5(4) . . . . ? C64 C63 O3 C24 -75.4(4) . . . . ? C34 C35 O4 C72 -62.6(4) . . . . ? C36 C35 O4 C72 121.6(3) . . . . ? C73 C72 O4 C35 -130.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.582 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.077