# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Gareth J. Pritchard' 'Eric A. Allart' 'Steven D. R. Christie' 'Mark R. J. Elsegood' _publ_contact_author_name 'Gareth J. Pritchard' _publ_contact_author_email G.J.PRITCHARD@LBORO.AC.UK _publ_section_title ; Preparation of Highly Substituted Tetrahydropyrans via a Metal Assisted Dipolar Cycloaddition Reaction ; # Attachment 'Pritchard.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 745432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 Co2 O11' _chemical_formula_sum 'C24 H20 Co2 O11' _chemical_formula_weight 602.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.4100(16) _cell_length_b 8.0633(4) _cell_length_c 22.1301(12) _cell_angle_alpha 90.00 _cell_angle_beta 109.3822(8) _cell_angle_gamma 90.00 _cell_volume 5118.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4882 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 24.73 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.656 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; Crystal was face indexed then inter-frame scaling applied with SADABS. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25700 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6367 _reflns_number_gt 4643 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0389P)^2^+2.1101P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'all non-H atoms found by direct methods' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6367 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.084426(10) 0.23321(4) 0.374468(13) 0.03433(9) Uani 1 1 d . . . Co2 Co 0.049931(10) 0.49915(4) 0.392093(14) 0.03389(9) Uani 1 1 d . . . C1 C 0.09004(7) 0.3451(3) 0.45562(9) 0.0269(4) Uani 1 1 d . . . C2 C 0.11480(7) 0.4265(3) 0.42534(9) 0.0271(4) Uani 1 1 d . . . C3 C 0.09058(7) 0.2930(3) 0.51926(9) 0.0261(4) Uani 1 1 d . . . C4 C 0.05855(8) 0.1804(3) 0.52691(11) 0.0375(5) Uani 1 1 d . . . H4 H 0.0362 0.1329 0.4902 0.045 Uiso 1 1 calc R . . C5 C 0.05870(8) 0.1360(3) 0.58731(11) 0.0428(6) Uani 1 1 d . . . H5 H 0.0367 0.0574 0.5919 0.051 Uiso 1 1 calc R . . C6 C 0.09051(9) 0.2054(3) 0.64081(11) 0.0418(6) Uani 1 1 d . . . H6 H 0.0903 0.1761 0.6823 0.050 Uiso 1 1 calc R . . C7 C 0.12281(9) 0.3178(3) 0.63391(11) 0.0462(6) Uani 1 1 d . . . H7 H 0.1449 0.3658 0.6708 0.055 Uiso 1 1 calc R . . C8 C 0.12320(8) 0.3610(3) 0.57351(10) 0.0379(5) Uani 1 1 d . . . H8 H 0.1458 0.4371 0.5691 0.045 Uiso 1 1 calc R . . C9 C 0.15916(7) 0.5161(3) 0.43384(9) 0.0247(4) Uani 1 1 d . . . H9 H 0.1622 0.6088 0.4650 0.030 Uiso 1 1 calc R . . C10 C 0.20215(7) 0.4062(3) 0.45782(9) 0.0257(4) Uani 1 1 d . . . H10A H 0.1973 0.3049 0.4311 0.031 Uiso 1 1 calc R . . H10B H 0.2068 0.3720 0.5025 0.031 Uiso 1 1 calc R . . C11 C 0.24561(7) 0.4973(2) 0.45524(9) 0.0246(4) Uani 1 1 d . . . H11A H 0.2722 0.4190 0.4658 0.030 Uiso 1 1 calc R . . H11B H 0.2536 0.5870 0.4876 0.030 Uiso 1 1 calc R . . C12 C 0.23767(7) 0.5726(2) 0.38795(9) 0.0217(4) Uani 1 1 d . . . C13 C 0.19411(7) 0.6843(3) 0.37333(9) 0.0249(4) Uani 1 1 d . . . H13 H 0.1998 0.7661 0.4091 0.030 Uiso 1 1 calc R . . O1 O 0.15499(5) 0.58485(17) 0.37227(6) 0.0255(3) Uani 1 1 d . . . C14 C 0.27987(7) 0.6793(3) 0.39193(9) 0.0258(4) Uani 1 1 d . . . O2 O 0.28773(5) 0.81114(19) 0.41914(7) 0.0360(4) Uani 1 1 d . . . O3 O 0.30682(5) 0.61068(18) 0.36254(8) 0.0353(4) Uani 1 1 d . . . C15 C 0.34792(8) 0.7046(3) 0.36385(13) 0.0454(6) Uani 1 1 d . . . H15A H 0.3383 0.8078 0.3397 0.068 Uiso 1 1 calc R . . H15B H 0.3668 0.6386 0.3444 0.068 Uiso 1 1 calc R . . H15C H 0.3664 0.7307 0.4083 0.068 Uiso 1 1 calc R . . C16 C 0.23148(7) 0.4406(2) 0.33576(10) 0.0253(4) Uani 1 1 d . . . O4 O 0.21408(6) 0.46467(18) 0.27942(7) 0.0353(4) Uani 1 1 d . . . O5 O 0.24918(5) 0.29438(17) 0.36069(7) 0.0316(3) Uani 1 1 d . . . C17 C 0.24812(9) 0.1674(3) 0.31378(12) 0.0443(6) Uani 1 1 d . . . H17A H 0.2158 0.1474 0.2867 0.066 Uiso 1 1 calc R . . H17B H 0.2616 0.0646 0.3359 0.066 Uiso 1 1 calc R . . H17C H 0.2663 0.2045 0.2871 0.066 Uiso 1 1 calc R . . C18 C 0.17925(8) 0.7799(3) 0.31081(10) 0.0334(5) Uani 1 1 d . . . H18A H 0.1642 0.7041 0.2753 0.050 Uiso 1 1 calc R . . H18B H 0.2067 0.8301 0.3043 0.050 Uiso 1 1 calc R . . H18C H 0.1572 0.8672 0.3124 0.050 Uiso 1 1 calc R . . C19 C 0.10159(9) 0.2715(4) 0.30400(12) 0.0554(8) Uani 1 1 d . . . O19 O 0.11292(8) 0.2938(4) 0.26116(10) 0.0906(9) Uani 1 1 d . . . C20 C 0.02980(9) 0.1254(3) 0.34176(11) 0.0434(6) Uani 1 1 d . . . O20 O -0.00503(7) 0.0581(3) 0.31996(8) 0.0605(5) Uani 1 1 d . . . C21 C 0.12020(9) 0.0621(4) 0.41317(13) 0.0466(6) Uani 1 1 d . . . O21 O 0.14187(7) -0.0455(3) 0.44088(11) 0.0696(6) Uani 1 1 d . . . C22 C -0.00877(9) 0.4299(3) 0.38305(12) 0.0460(6) Uani 1 1 d . . . O22 O -0.04414(7) 0.3788(3) 0.38126(11) 0.0721(6) Uani 1 1 d . . . C23 C 0.05033(9) 0.6077(4) 0.32014(13) 0.0597(8) Uani 1 1 d . . . O23 O 0.05296(7) 0.6764(4) 0.27652(10) 0.0967(9) Uani 1 1 d . . . C24 C 0.05350(8) 0.6718(3) 0.44419(13) 0.0444(6) Uani 1 1 d . . . O24 O 0.05754(7) 0.7777(3) 0.47935(12) 0.0709(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02945(17) 0.0495(2) 0.02695(16) -0.01071(13) 0.01326(12) -0.00981(14) Co2 0.02335(15) 0.0495(2) 0.02846(16) 0.00756(13) 0.00811(12) 0.00198(13) C1 0.0233(10) 0.0332(11) 0.0242(10) -0.0024(9) 0.0080(8) 0.0014(8) C2 0.0246(10) 0.0346(11) 0.0224(10) -0.0014(9) 0.0084(8) 0.0019(9) C3 0.0260(10) 0.0310(11) 0.0235(10) 0.0019(8) 0.0112(8) 0.0044(8) C4 0.0337(12) 0.0474(14) 0.0307(11) -0.0014(10) 0.0097(10) -0.0104(10) C5 0.0407(14) 0.0512(16) 0.0402(13) 0.0080(11) 0.0181(11) -0.0079(11) C6 0.0482(15) 0.0527(15) 0.0283(11) 0.0088(11) 0.0180(11) 0.0057(12) C7 0.0507(15) 0.0584(16) 0.0254(11) 0.0018(11) 0.0073(11) -0.0094(13) C8 0.0373(13) 0.0458(14) 0.0302(11) 0.0020(10) 0.0109(10) -0.0102(11) C9 0.0232(10) 0.0327(11) 0.0182(9) 0.0002(8) 0.0069(8) 0.0005(8) C10 0.0269(10) 0.0304(11) 0.0205(9) 0.0036(8) 0.0087(8) -0.0002(8) C11 0.0232(10) 0.0289(10) 0.0209(9) 0.0023(8) 0.0061(8) 0.0029(8) C12 0.0236(10) 0.0214(10) 0.0207(9) -0.0009(8) 0.0081(8) -0.0007(8) C13 0.0256(10) 0.0255(10) 0.0230(10) 0.0010(8) 0.0073(8) -0.0001(8) O1 0.0218(7) 0.0338(8) 0.0197(7) 0.0037(6) 0.0052(5) -0.0013(6) C14 0.0242(10) 0.0301(11) 0.0219(10) 0.0034(8) 0.0059(8) -0.0021(8) O2 0.0378(9) 0.0344(9) 0.0382(9) -0.0112(7) 0.0159(7) -0.0118(7) O3 0.0287(8) 0.0328(8) 0.0511(10) -0.0060(7) 0.0224(7) -0.0053(6) C15 0.0310(13) 0.0504(15) 0.0626(17) -0.0069(13) 0.0261(12) -0.0131(11) C16 0.0261(10) 0.0245(10) 0.0291(11) -0.0013(8) 0.0141(9) -0.0057(8) O4 0.0465(10) 0.0351(9) 0.0235(8) -0.0033(6) 0.0105(7) -0.0032(7) O5 0.0421(9) 0.0230(7) 0.0333(8) -0.0018(6) 0.0171(7) 0.0037(6) C17 0.0594(16) 0.0286(12) 0.0497(15) -0.0117(11) 0.0248(13) -0.0002(11) C18 0.0379(12) 0.0310(12) 0.0300(11) 0.0085(9) 0.0097(9) 0.0021(9) C19 0.0481(16) 0.086(2) 0.0387(14) -0.0247(14) 0.0227(12) -0.0307(15) O19 0.0899(17) 0.152(2) 0.0485(12) -0.0376(14) 0.0479(12) -0.0616(16) C20 0.0426(14) 0.0632(17) 0.0280(12) -0.0090(11) 0.0166(11) -0.0144(13) O20 0.0500(12) 0.0889(15) 0.0447(10) -0.0145(10) 0.0184(9) -0.0359(11) C21 0.0337(13) 0.0501(16) 0.0585(17) -0.0253(13) 0.0188(12) -0.0028(12) O21 0.0529(13) 0.0502(12) 0.1011(17) -0.0188(12) 0.0193(12) 0.0103(10) C22 0.0295(13) 0.0589(17) 0.0486(15) 0.0010(13) 0.0115(11) 0.0016(12) O22 0.0334(11) 0.0837(16) 0.1028(17) -0.0086(13) 0.0274(11) -0.0098(10) C23 0.0264(13) 0.099(2) 0.0483(16) 0.0284(16) 0.0051(12) 0.0054(14) O23 0.0427(12) 0.182(3) 0.0610(14) 0.0718(16) 0.0114(10) 0.0049(14) C24 0.0294(13) 0.0464(15) 0.0556(16) 0.0072(13) 0.0115(11) 0.0075(11) O24 0.0577(13) 0.0555(13) 0.0959(17) -0.0203(12) 0.0209(12) 0.0058(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C21 1.790(3) . ? Co1 C20 1.801(2) . ? Co1 C19 1.828(3) . ? Co1 C2 1.964(2) . ? Co1 C1 1.966(2) . ? Co1 Co2 2.4743(5) . ? Co2 C24 1.788(3) . ? Co2 C22 1.817(3) . ? Co2 C23 1.821(3) . ? Co2 C2 1.953(2) . ? Co2 C1 1.967(2) . ? C1 C2 1.335(3) . ? C1 C3 1.465(3) . ? C2 C9 1.486(3) . ? C3 C4 1.383(3) . ? C3 C8 1.391(3) . ? C4 C5 1.382(3) . ? C5 C6 1.375(3) . ? C6 C7 1.382(4) . ? C7 C8 1.385(3) . ? C9 O1 1.437(2) . ? C9 C10 1.522(3) . ? C10 C11 1.529(3) . ? C11 C12 1.551(3) . ? C12 C14 1.524(3) . ? C12 C16 1.535(3) . ? C12 C13 1.545(3) . ? C13 O1 1.428(2) . ? C13 C18 1.516(3) . ? C14 O2 1.206(2) . ? C14 O3 1.325(2) . ? O3 C15 1.453(2) . ? C16 O4 1.198(2) . ? C16 O5 1.337(2) . ? O5 C17 1.451(3) . ? C19 O19 1.125(3) . ? C20 O20 1.144(3) . ? C21 O21 1.138(3) . ? C22 O22 1.140(3) . ? C23 O23 1.138(3) . ? C24 O24 1.134(3) . ? 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 C21 Co1 C20 98.81(12) . . ? C21 Co1 C19 103.77(13) . . ? C20 Co1 C19 103.01(11) . . ? C21 Co1 C2 103.99(10) . . ? C20 Co1 C2 144.02(10) . . ? C19 Co1 C2 98.17(10) . . ? C21 Co1 C1 93.55(10) . . ? C20 Co1 C1 112.20(9) . . ? C19 Co1 C1 137.67(11) . . ? C2 Co1 C1 39.70(8) . . ? C21 Co1 Co2 144.59(8) . . ? C20 Co1 Co2 95.69(9) . . ? C19 Co1 Co2 104.14(10) . . ? C2 Co1 Co2 50.62(6) . . ? C1 Co1 Co2 51.03(6) . . ? C24 Co2 C22 99.07(11) . . ? C24 Co2 C23 99.95(14) . . ? C22 Co2 C23 110.06(11) . . ? C24 Co2 C2 98.82(10) . . ? C22 Co2 C2 141.43(11) . . ? C23 Co2 C2 100.07(10) . . ? C24 Co2 C1 98.07(10) . . ? C22 Co2 C1 103.77(10) . . ? C23 Co2 C1 138.26(10) . . ? C2 Co2 C1 39.81(8) . . ? C24 Co2 Co1 146.97(8) . . ? C22 Co2 Co1 99.70(9) . . ? C23 Co2 Co1 98.78(11) . . ? C2 Co2 Co1 51.03(6) . . ? C1 Co2 Co1 51.00(6) . . ? C2 C1 C3 142.73(19) . . ? C2 C1 Co1 70.08(12) . . ? C3 C1 Co1 135.77(16) . . ? C2 C1 Co2 69.52(12) . . ? C3 C1 Co2 132.45(14) . . ? Co1 C1 Co2 77.97(7) . . ? C1 C2 C9 144.59(19) . . ? C1 C2 Co2 70.67(12) . . ? C9 C2 Co2 131.51(15) . . ? C1 C2 Co1 70.22(13) . . ? C9 C2 Co1 133.84(14) . . ? Co2 C2 Co1 78.35(7) . . ? C4 C3 C8 118.86(19) . . ? C4 C3 C1 121.51(19) . . ? C8 C3 C1 119.61(19) . . ? C5 C4 C3 120.8(2) . . ? C6 C5 C4 120.2(2) . . ? C5 C6 C7 119.6(2) . . ? C6 C7 C8 120.4(2) . . ? C7 C8 C3 120.1(2) . . ? O1 C9 C2 106.08(15) . . ? O1 C9 C10 110.52(15) . . ? C2 C9 C10 113.57(17) . . ? C9 C10 C11 111.13(16) . . ? C10 C11 C12 111.27(15) . . ? C14 C12 C16 109.02(15) . . ? C14 C12 C13 109.25(16) . . ? C16 C12 C13 111.35(16) . . ? C14 C12 C11 107.81(15) . . ? C16 C12 C11 113.10(16) . . ? C13 C12 C11 106.18(15) . . ? O1 C13 C18 106.03(16) . . ? O1 C13 C12 109.12(16) . . ? C18 C13 C12 117.57(16) . . ? C13 O1 C9 112.97(14) . . ? O2 C14 O3 124.15(19) . . ? O2 C14 C12 123.40(18) . . ? O3 C14 C12 112.45(17) . . ? C14 O3 C15 116.13(17) . . ? O4 C16 O5 123.42(19) . . ? O4 C16 C12 124.92(19) . . ? O5 C16 C12 111.63(16) . . ? C16 O5 C17 114.62(16) . . ? O19 C19 Co1 178.8(3) . . ? O20 C20 Co1 178.8(2) . . ? O21 C21 Co1 175.7(2) . . ? O22 C22 Co2 174.8(3) . . ? O23 C23 Co2 176.5(2) . . ? O24 C24 Co2 176.7(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 C21 Co1 Co2 C24 24.0(2) . . . . ? C20 Co1 Co2 C24 137.96(17) . . . . ? C19 Co1 Co2 C24 -117.07(17) . . . . ? C2 Co1 Co2 C24 -28.06(17) . . . . ? C1 Co1 Co2 C24 23.89(17) . . . . ? C21 Co1 Co2 C22 -99.80(17) . . . . ? C20 Co1 Co2 C22 14.14(11) . . . . ? C19 Co1 Co2 C22 119.12(12) . . . . ? C2 Co1 Co2 C22 -151.87(11) . . . . ? C1 Co1 Co2 C22 -99.92(11) . . . . ? C21 Co1 Co2 C23 147.96(17) . . . . ? C20 Co1 Co2 C23 -98.10(11) . . . . ? C19 Co1 Co2 C23 6.88(12) . . . . ? C2 Co1 Co2 C23 95.89(11) . . . . ? C1 Co1 Co2 C23 147.84(11) . . . . ? C21 Co1 Co2 C2 52.07(16) . . . . ? C20 Co1 Co2 C2 166.02(10) . . . . ? C19 Co1 Co2 C2 -89.01(11) . . . . ? C1 Co1 Co2 C2 51.95(10) . . . . ? C21 Co1 Co2 C1 0.12(16) . . . . ? C20 Co1 Co2 C1 114.07(11) . . . . ? C19 Co1 Co2 C1 -140.96(11) . . . . ? C2 Co1 Co2 C1 -51.95(10) . . . . ? C21 Co1 C1 C2 107.73(14) . . . . ? C20 Co1 C1 C2 -151.25(14) . . . . ? C19 Co1 C1 C2 -7.3(2) . . . . ? Co2 Co1 C1 C2 -72.34(12) . . . . ? C21 Co1 C1 C3 -39.5(2) . . . . ? C20 Co1 C1 C3 61.5(2) . . . . ? C19 Co1 C1 C3 -154.5(2) . . . . ? C2 Co1 C1 C3 -147.3(3) . . . . ? Co2 Co1 C1 C3 140.4(2) . . . . ? C21 Co1 C1 Co2 -179.93(9) . . . . ? C20 Co1 C1 Co2 -78.91(11) . . . . ? C19 Co1 C1 Co2 65.09(18) . . . . ? C2 Co1 C1 Co2 72.34(12) . . . . ? C24 Co2 C1 C2 -94.11(14) . . . . ? C22 Co2 C1 C2 164.43(14) . . . . ? C23 Co2 C1 C2 20.8(2) . . . . ? Co1 Co2 C1 C2 73.01(12) . . . . ? C24 Co2 C1 C3 49.9(2) . . . . ? C22 Co2 C1 C3 -51.5(2) . . . . ? C23 Co2 C1 C3 164.8(2) . . . . ? C2 Co2 C1 C3 144.1(3) . . . . ? Co1 Co2 C1 C3 -142.9(2) . . . . ? C24 Co2 C1 Co1 -167.12(9) . . . . ? C22 Co2 C1 Co1 91.42(10) . . . . ? C23 Co2 C1 Co1 -52.21(19) . . . . ? C2 Co2 C1 Co1 -73.01(12) . . . . ? C3 C1 C2 C9 1.6(6) . . . . ? Co1 C1 C2 C9 -139.9(3) . . . . ? Co2 C1 C2 C9 135.9(3) . . . . ? C3 C1 C2 Co2 -134.3(3) . . . . ? Co1 C1 C2 Co2 84.19(6) . . . . ? C3 C1 C2 Co1 141.5(3) . . . . ? Co2 C1 C2 Co1 -84.19(6) . . . . ? C24 Co2 C2 C1 92.05(14) . . . . ? C22 Co2 C2 C1 -24.7(2) . . . . ? C23 Co2 C2 C1 -166.11(16) . . . . ? Co1 Co2 C2 C1 -72.91(12) . . . . ? C24 Co2 C2 C9 -55.4(2) . . . . ? C22 Co2 C2 C9 -172.18(18) . . . . ? C23 Co2 C2 C9 46.4(2) . . . . ? C1 Co2 C2 C9 -147.5(2) . . . . ? Co1 Co2 C2 C9 139.6(2) . . . . ? C24 Co2 C2 Co1 164.96(9) . . . . ? C22 Co2 C2 Co1 48.19(17) . . . . ? C23 Co2 C2 Co1 -93.20(12) . . . . ? C1 Co2 C2 Co1 72.91(12) . . . . ? C21 Co1 C2 C1 -78.45(15) . . . . ? C20 Co1 C2 C1 49.3(2) . . . . ? C19 Co1 C2 C1 175.07(15) . . . . ? Co2 Co1 C2 C1 73.44(12) . . . . ? C21 Co1 C2 C9 70.4(2) . . . . ? C20 Co1 C2 C9 -161.90(19) . . . . ? C19 Co1 C2 C9 -36.1(2) . . . . ? C1 Co1 C2 C9 148.8(3) . . . . ? Co2 Co1 C2 C9 -137.7(2) . . . . ? C21 Co1 C2 Co2 -151.90(9) . . . . ? C20 Co1 C2 Co2 -24.16(18) . . . . ? C19 Co1 C2 Co2 101.63(11) . . . . ? C1 Co1 C2 Co2 -73.44(12) . . . . ? C2 C1 C3 C4 -168.6(3) . . . . ? Co1 C1 C3 C4 -45.7(3) . . . . ? Co2 C1 C3 C4 76.6(3) . . . . ? C2 C1 C3 C8 13.1(4) . . . . ? Co1 C1 C3 C8 136.0(2) . . . . ? Co2 C1 C3 C8 -101.7(2) . . . . ? C8 C3 C4 C5 0.2(3) . . . . ? C1 C3 C4 C5 -178.1(2) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C4 C5 C6 C7 -1.0(4) . . . . ? C5 C6 C7 C8 0.1(4) . . . . ? C6 C7 C8 C3 0.9(4) . . . . ? C4 C3 C8 C7 -1.0(3) . . . . ? C1 C3 C8 C7 177.3(2) . . . . ? C1 C2 C9 O1 -173.4(3) . . . . ? Co2 C2 C9 O1 -54.6(2) . . . . ? Co1 C2 C9 O1 63.8(2) . . . . ? C1 C2 C9 C10 65.0(4) . . . . ? Co2 C2 C9 C10 -176.19(14) . . . . ? Co1 C2 C9 C10 -57.8(2) . . . . ? O1 C9 C10 C11 51.7(2) . . . . ? C2 C9 C10 C11 170.74(16) . . . . ? C9 C10 C11 C12 -52.0(2) . . . . ? C10 C11 C12 C14 172.67(16) . . . . ? C10 C11 C12 C16 -66.7(2) . . . . ? C10 C11 C12 C13 55.7(2) . . . . ? C14 C12 C13 O1 -177.61(14) . . . . ? C16 C12 C13 O1 61.92(19) . . . . ? C11 C12 C13 O1 -61.58(19) . . . . ? C14 C12 C13 C18 61.7(2) . . . . ? C16 C12 C13 C18 -58.8(2) . . . . ? C11 C12 C13 C18 177.71(17) . . . . ? C18 C13 O1 C9 -166.27(16) . . . . ? C12 C13 O1 C9 66.20(19) . . . . ? C2 C9 O1 C13 176.41(15) . . . . ? C10 C9 O1 C13 -60.1(2) . . . . ? C16 C12 C14 O2 164.82(19) . . . . ? C13 C12 C14 O2 42.9(2) . . . . ? C11 C12 C14 O2 -72.0(2) . . . . ? C16 C12 C14 O3 -15.5(2) . . . . ? C13 C12 C14 O3 -137.38(17) . . . . ? C11 C12 C14 O3 107.64(18) . . . . ? O2 C14 O3 C15 -0.5(3) . . . . ? C12 C14 O3 C15 179.86(18) . . . . ? C14 C12 C16 O4 -79.2(2) . . . . ? C13 C12 C16 O4 41.4(3) . . . . ? C11 C12 C16 O4 160.88(19) . . . . ? C14 C12 C16 O5 99.07(18) . . . . ? C13 C12 C16 O5 -140.32(16) . . . . ? C11 C12 C16 O5 -20.9(2) . . . . ? O4 C16 O5 C17 3.3(3) . . . . ? C12 C16 O5 C17 -175.00(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.451 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.063 #===END data_10.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 745433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Co2 O11, C H2 Cl2' _chemical_formula_sum 'C31 H26 Cl2 Co2 O11' _chemical_formula_weight 763.28 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2516(12) _cell_length_b 13.8248(19) _cell_length_c 14.0220(19) _cell_angle_alpha 109.6525(19) _cell_angle_beta 91.9541(19) _cell_angle_gamma 104.8855(19) _cell_volume 1617.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3436 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12711 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5678 _reflns_number_gt 4097 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1371P)^2^+6.2845P] 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 5678 _refine_ls_number_parameters 464 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2425 _refine_ls_wR_factor_gt 0.2160 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.18838(9) 0.67549(7) 0.18591(6) 0.0320(3) Uani 1 1 d . . . Co2 Co -0.01537(9) 0.61398(8) 0.27873(7) 0.0341(3) Uani 1 1 d . . . C1 C 0.1720(7) 0.7313(6) 0.3327(5) 0.0360(15) Uani 1 1 d . . . C2 C 0.2006(7) 0.6364(6) 0.3071(5) 0.0324(14) Uani 1 1 d . . . C3 C 0.2122(7) 0.8389(6) 0.4118(5) 0.0369(16) Uani 1 1 d . . . C4 C 0.1548(16) 0.9171(9) 0.4070(9) 0.116(6) Uani 1 1 d . . . H4 H 0.0862 0.9034 0.3489 0.139 Uiso 1 1 calc R . . C5 C 0.1924(18) 1.0176(10) 0.4841(9) 0.120(6) Uani 1 1 d . . . H5 H 0.1474 1.0700 0.4776 0.144 Uiso 1 1 calc R . . C6 C 0.2885(10) 1.0420(7) 0.5657(7) 0.060(2) Uani 1 1 d . . . H6 H 0.3166 1.1116 0.6168 0.072 Uiso 1 1 calc R . . C7 C 0.3465(15) 0.9628(8) 0.5739(9) 0.095(4) Uani 1 1 d . . . H7 H 0.4136 0.9774 0.6331 0.114 Uiso 1 1 calc R . . C8 C 0.3099(13) 0.8620(8) 0.4981(7) 0.075(3) Uani 1 1 d . . . H8 H 0.3522 0.8088 0.5056 0.090 Uiso 1 1 calc R . . C9 C 0.2894(7) 0.5765(6) 0.3428(5) 0.0348(15) Uani 1 1 d . . . H9 H 0.2769 0.5868 0.4158 0.042 Uiso 1 1 calc R . . C10 C 0.4569(7) 0.6137(7) 0.3345(6) 0.0470(19) Uani 1 1 d . . . H10A H 0.5020 0.6867 0.3854 0.056 Uiso 1 1 calc R . . H10B H 0.4697 0.6166 0.2656 0.056 Uiso 1 1 calc R . . C11 C 0.5384(8) 0.5363(7) 0.3534(6) 0.050(2) Uani 1 1 d . . . H11A H 0.6417 0.5540 0.3349 0.061 Uiso 1 1 calc R . . H11B H 0.5475 0.5480 0.4273 0.061 Uiso 1 1 calc R . . C12 C 0.4590(8) 0.4175(7) 0.2933(5) 0.0440(19) Uani 1 1 d . A . C13 C 0.2905(7) 0.3964(6) 0.3159(5) 0.0369(16) Uani 1 1 d . . . H13 H 0.2923 0.4196 0.3917 0.044 Uiso 1 1 calc R . . O1 O 0.2260(5) 0.4656(4) 0.2820(3) 0.0346(10) Uani 1 1 d . . . C14 C 0.5415(8) 0.3548(7) 0.3354(5) 0.0455(19) Uani 1 1 d D . . O2 O 0.5056(6) 0.3219(5) 0.4030(4) 0.0518(14) Uani 1 1 d D . . O3 O 0.6663(6) 0.3498(6) 0.2939(5) 0.0672(19) Uani 1 1 d D . . C15 C 0.7610(12) 0.2957(11) 0.3297(9) 0.088(4) Uani 1 1 d D . . H15A H 0.8063 0.3388 0.4005 0.132 Uiso 1 1 calc R . . H15B H 0.8410 0.2868 0.2863 0.132 Uiso 1 1 calc R . . H15C H 0.6991 0.2252 0.3264 0.132 Uiso 1 1 calc R . . C16 C 0.4732(10) 0.3927(8) 0.1831(6) 0.073(2) Uani 1 1 d DU . . O4 O 0.5356(16) 0.4637(11) 0.1516(9) 0.075(4) Uani 0.661(18) 1 d PDU A 1 O5 O 0.413(2) 0.2920(12) 0.1231(12) 0.085(4) Uani 0.661(18) 1 d PDU A 1 C17 C 0.4429(18) 0.2758(16) 0.0190(10) 0.088(6) Uani 0.661(18) 1 d PDU A 1 H17A H 0.3945 0.2010 -0.0244 0.132 Uiso 0.661(18) 1 calc PR A 1 H17B H 0.5520 0.2924 0.0169 0.132 Uiso 0.661(18) 1 calc PR A 1 H17C H 0.4024 0.3230 -0.0060 0.132 Uiso 0.661(18) 1 calc PR A 1 O4X O 0.449(3) 0.2933(17) 0.139(2) 0.059(5) Uani 0.339(18) 1 d PDU A 2 O5X O 0.487(3) 0.448(2) 0.1242(15) 0.079(5) Uani 0.339(18) 1 d PDU A 2 C17X C 0.477(3) 0.381(2) 0.0171(14) 0.055(6) Uani 0.339(18) 1 d PDU A 2 H17D H 0.4925 0.4270 -0.0245 0.083 Uiso 0.339(18) 1 calc PR A 2 H17E H 0.3765 0.3294 -0.0054 0.083 Uiso 0.339(18) 1 calc PR A 2 H17F H 0.5540 0.3435 0.0091 0.083 Uiso 0.339(18) 1 calc PR A 2 C18 C 0.1831(8) 0.2854(6) 0.2698(5) 0.0382(16) Uani 1 1 d . . . C19 C 0.1453(9) 0.2225(7) 0.3298(6) 0.0505(19) Uani 1 1 d . . . H19 H 0.1942 0.2477 0.3978 0.061 Uiso 1 1 calc R . . C20 C 0.0388(10) 0.1250(7) 0.2921(7) 0.059(2) Uani 1 1 d . . . H20 H 0.0155 0.0836 0.3346 0.071 Uiso 1 1 calc R . . C21 C -0.0358(9) 0.0850(6) 0.1938(7) 0.053(2) Uani 1 1 d . . . C22 C 0.0013(8) 0.1477(7) 0.1336(6) 0.0480(19) Uani 1 1 d . . . H22 H -0.0475 0.1220 0.0654 0.058 Uiso 1 1 calc R . . C23 C 0.1082(8) 0.2468(7) 0.1716(6) 0.0454(18) Uani 1 1 d . . . H23 H 0.1304 0.2888 0.1297 0.054 Uiso 1 1 calc R . . C24 C -0.1564(12) -0.0242(7) 0.1510(9) 0.074(3) Uani 1 1 d . . . H24A H -0.2536 -0.0138 0.1340 0.111 Uiso 1 1 calc R . . H24B H -0.1655 -0.0584 0.2023 0.111 Uiso 1 1 calc R . . H24C H -0.1269 -0.0701 0.0893 0.111 Uiso 1 1 calc R . . C25 C 0.1911(8) 0.5493(6) 0.0887(5) 0.0376(16) Uani 1 1 d . . . O25 O 0.1931(7) 0.4706(5) 0.0299(4) 0.0537(14) Uani 1 1 d . . . C26 C 0.0848(8) 0.7361(6) 0.1205(6) 0.0440(17) Uani 1 1 d . . . O26 O 0.0160(7) 0.7702(5) 0.0796(5) 0.0659(17) Uani 1 1 d . . . C27 C 0.3747(8) 0.7601(6) 0.1951(5) 0.0370(15) Uani 1 1 d . . . O27 O 0.4944(6) 0.8140(5) 0.2050(4) 0.0530(14) Uani 1 1 d . . . C28 C -0.1497(8) 0.6819(7) 0.2557(6) 0.0470(19) Uani 1 1 d . . . O28 O -0.2303(6) 0.7269(6) 0.2411(6) 0.0698(18) Uani 1 1 d . . . C29 C -0.0860(7) 0.4785(6) 0.1870(5) 0.0386(16) Uani 1 1 d . . . O29 O -0.1274(6) 0.3945(5) 0.1273(4) 0.0512(13) Uani 1 1 d . . . C30 C -0.0631(7) 0.5901(7) 0.3927(6) 0.0439(18) Uani 1 1 d . . . O30 O -0.0860(6) 0.5746(6) 0.4663(4) 0.0621(17) Uani 1 1 d . . . Cl1 Cl 0.3630(7) -0.1032(5) 0.0165(6) 0.185(2) Uani 1 1 d DU . . C31 C 0.2705(17) -0.0307(10) 0.1105(11) 0.128(6) Uani 0.668(8) 1 d PDU B 1 H31A H 0.1769 -0.0810 0.1170 0.154 Uiso 0.668(8) 1 calc PR B 1 H31B H 0.2408 0.0222 0.0870 0.154 Uiso 0.668(8) 1 calc PR B 1 Cl2 Cl 0.3813(9) 0.0393(6) 0.2356(8) 0.198(5) Uani 0.668(8) 1 d PDU B 1 C31X C 0.359(3) 0.0255(13) 0.106(2) 0.132(8) Uani 0.332(8) 1 d PDU B 2 H31C H 0.3061 0.0174 0.1639 0.158 Uiso 0.332(8) 1 calc PR B 2 H31D H 0.3089 0.0627 0.0717 0.158 Uiso 0.332(8) 1 calc PR B 2 Cl2X Cl 0.5575(11) 0.0974(8) 0.1475(12) 0.131(5) Uani 0.332(8) 1 d PDU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0249(5) 0.0439(6) 0.0298(5) 0.0106(4) 0.0030(3) 0.0179(4) Co2 0.0190(5) 0.0516(6) 0.0338(5) 0.0122(4) 0.0029(3) 0.0180(4) C1 0.022(3) 0.058(4) 0.032(3) 0.015(3) 0.005(3) 0.020(3) C2 0.019(3) 0.051(4) 0.028(3) 0.011(3) 0.004(2) 0.016(3) C3 0.027(3) 0.051(4) 0.030(3) 0.007(3) 0.005(3) 0.017(3) C4 0.164(13) 0.093(8) 0.076(7) -0.026(6) -0.066(8) 0.095(9) C5 0.176(14) 0.092(8) 0.077(8) -0.027(6) -0.052(8) 0.098(9) C6 0.057(5) 0.057(5) 0.053(5) 0.002(4) -0.003(4) 0.017(4) C7 0.115(10) 0.063(7) 0.073(7) 0.002(5) -0.045(7) 0.007(6) C8 0.094(8) 0.055(5) 0.061(6) 0.014(5) -0.028(5) 0.012(5) C9 0.022(3) 0.056(4) 0.032(3) 0.018(3) 0.000(3) 0.016(3) C10 0.024(3) 0.073(5) 0.061(5) 0.040(4) 0.004(3) 0.021(3) C11 0.023(3) 0.087(6) 0.061(5) 0.043(5) 0.011(3) 0.026(4) C12 0.031(4) 0.088(6) 0.034(4) 0.031(4) 0.012(3) 0.039(4) C13 0.029(3) 0.064(5) 0.034(3) 0.024(3) 0.010(3) 0.030(3) O1 0.024(2) 0.053(3) 0.034(2) 0.017(2) 0.0036(18) 0.022(2) C14 0.037(4) 0.077(5) 0.033(4) 0.018(4) 0.008(3) 0.034(4) O2 0.048(3) 0.081(4) 0.047(3) 0.031(3) 0.006(2) 0.041(3) O3 0.050(3) 0.124(6) 0.069(4) 0.054(4) 0.027(3) 0.066(4) C15 0.070(6) 0.158(11) 0.092(8) 0.071(8) 0.033(6) 0.090(8) C16 0.053(5) 0.160(6) 0.035(4) 0.041(3) 0.018(3) 0.071(5) O4 0.101(10) 0.154(7) 0.034(6) 0.056(6) 0.032(6) 0.109(6) O5 0.025(9) 0.184(7) 0.036(6) 0.028(5) -0.001(5) 0.027(6) C17 0.064(9) 0.124(13) 0.045(6) 0.014(6) 0.019(7) -0.005(9) O4X 0.007(11) 0.149(7) 0.021(10) 0.029(7) -0.002(8) 0.022(9) O5X 0.081(12) 0.173(11) 0.032(8) 0.047(7) 0.014(8) 0.104(10) C17X 0.074(14) 0.085(15) 0.046(7) 0.046(9) 0.049(10) 0.054(12) C18 0.032(3) 0.056(4) 0.036(4) 0.015(3) 0.007(3) 0.030(3) C19 0.053(5) 0.061(5) 0.050(5) 0.024(4) 0.004(4) 0.031(4) C20 0.064(5) 0.060(5) 0.073(6) 0.037(5) 0.011(5) 0.033(5) C21 0.051(5) 0.049(5) 0.065(5) 0.017(4) 0.009(4) 0.031(4) C22 0.039(4) 0.061(5) 0.048(4) 0.015(4) 0.005(3) 0.027(4) C23 0.038(4) 0.060(5) 0.047(4) 0.022(4) 0.007(3) 0.025(4) C24 0.074(7) 0.050(5) 0.101(8) 0.027(5) 0.003(6) 0.026(5) C25 0.033(4) 0.052(4) 0.034(4) 0.017(3) 0.009(3) 0.020(3) O25 0.060(4) 0.054(3) 0.047(3) 0.011(3) 0.009(3) 0.025(3) C26 0.040(4) 0.058(5) 0.039(4) 0.015(4) 0.008(3) 0.025(4) O26 0.070(4) 0.087(5) 0.067(4) 0.039(4) 0.009(3) 0.052(4) C27 0.034(4) 0.048(4) 0.031(4) 0.011(3) 0.006(3) 0.020(3) O27 0.033(3) 0.064(4) 0.053(3) 0.013(3) 0.007(2) 0.010(3) C28 0.025(3) 0.068(5) 0.051(5) 0.021(4) 0.006(3) 0.019(4) O28 0.042(3) 0.091(5) 0.102(5) 0.045(4) 0.018(3) 0.045(3) C29 0.024(3) 0.056(5) 0.037(4) 0.014(4) 0.004(3) 0.017(3) O29 0.041(3) 0.061(4) 0.044(3) 0.009(3) 0.007(2) 0.014(3) C30 0.024(3) 0.066(5) 0.045(4) 0.016(4) 0.006(3) 0.023(3) O30 0.040(3) 0.115(5) 0.046(3) 0.037(3) 0.013(3) 0.035(3) Cl1 0.140(4) 0.158(4) 0.238(6) 0.045(4) -0.006(4) 0.046(4) C31 0.052(8) 0.025(7) 0.279(11) 0.021(9) -0.052(7) 0.019(6) Cl2 0.143(6) 0.119(5) 0.277(8) -0.025(6) -0.063(6) 0.087(5) C31X 0.117(11) 0.068(11) 0.240(19) 0.103(9) -0.055(18) 0.022(11) Cl2X 0.078(6) 0.095(6) 0.237(15) 0.052(6) 0.066(6) 0.055(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C27 1.790(8) . ? Co1 C25 1.824(7) . ? Co1 C26 1.825(8) . ? Co1 C2 1.957(7) . ? Co1 C1 1.966(7) . ? Co1 Co2 2.4614(13) . ? Co2 C30 1.784(8) . ? Co2 C29 1.812(8) . ? Co2 C28 1.819(8) . ? Co2 C2 1.947(6) . ? Co2 C1 1.962(7) . ? C1 C2 1.338(10) . ? C1 C3 1.469(10) . ? C2 C9 1.487(9) . ? C3 C4 1.340(12) . ? C3 C8 1.378(11) . ? C4 C5 1.392(14) . ? C5 C6 1.316(14) . ? C6 C7 1.373(14) . ? C7 C8 1.387(14) . ? C9 O1 1.430(8) . ? C9 C10 1.525(9) . ? C10 C11 1.541(10) . ? C11 C12 1.535(12) . ? C12 C16 1.485(10) . ? C12 C14 1.528(10) . ? C12 C13 1.574(9) . ? C13 O1 1.442(8) . ? C13 C18 1.505(11) . ? C14 O2 1.204(9) . ? C14 O3 1.318(8) . ? O3 C15 1.462(9) . ? C16 O4 1.229(14) . ? C16 O4X 1.256(18) . ? C16 O5X 1.290(17) . ? C16 O5 1.318(16) . ? O5 C17 1.448(17) . ? O5X C17X 1.459(19) . ? C18 C23 1.383(10) . ? C18 C19 1.393(11) . ? C19 C20 1.368(12) . ? C20 C21 1.381(12) . ? C21 C22 1.393(12) . ? C21 C24 1.538(12) . ? C22 C23 1.385(11) . ? C25 O25 1.128(8) . ? C26 O26 1.126(9) . ? C27 O27 1.139(8) . ? C28 O28 1.140(9) . ? C29 O29 1.136(9) . ? C30 O30 1.139(9) . ? Cl1 C31 1.761(13) . ? Cl1 C31X 1.807(18) . ? Cl1 Cl2X 2.459(17) 2_655 ? C31 Cl2 1.814(13) . ? C31X Cl2X 1.816(18) . ? Cl2X Cl1 2.459(17) 2_655 ? 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 C27 Co1 C25 102.7(3) . . ? C27 Co1 C26 98.6(3) . . ? C25 Co1 C26 105.1(3) . . ? C27 Co1 C2 102.5(3) . . ? C25 Co1 C2 99.1(3) . . ? C26 Co1 C2 143.3(3) . . ? C27 Co1 C1 95.7(3) . . ? C25 Co1 C1 138.3(3) . . ? C26 Co1 C1 108.7(3) . . ? C2 Co1 C1 39.9(3) . . ? C27 Co1 Co2 146.6(2) . . ? C25 Co1 Co2 101.5(2) . . ? C26 Co1 Co2 97.0(2) . . ? C2 Co1 Co2 50.74(17) . . ? C1 Co1 Co2 51.1(2) . . ? C30 Co2 C29 99.5(3) . . ? C30 Co2 C28 103.4(3) . . ? C29 Co2 C28 104.6(3) . . ? C30 Co2 C2 96.1(3) . . ? C29 Co2 C2 104.8(3) . . ? C28 Co2 C2 141.1(3) . . ? C30 Co2 C1 100.4(3) . . ? C29 Co2 C1 141.1(3) . . ? C28 Co2 C1 102.8(3) . . ? C2 Co2 C1 40.0(3) . . ? C30 Co2 Co1 146.4(2) . . ? C29 Co2 Co1 96.4(2) . . ? C28 Co2 Co1 100.8(2) . . ? C2 Co2 Co1 51.1(2) . . ? C1 Co2 Co1 51.28(19) . . ? C2 C1 C3 142.7(6) . . ? C2 C1 Co2 69.4(4) . . ? C3 C1 Co2 134.5(5) . . ? C2 C1 Co1 69.7(4) . . ? C3 C1 Co1 134.4(5) . . ? Co2 C1 Co1 77.6(3) . . ? C1 C2 C9 142.8(6) . . ? C1 C2 Co2 70.6(4) . . ? C9 C2 Co2 132.5(5) . . ? C1 C2 Co1 70.5(4) . . ? C9 C2 Co1 134.6(5) . . ? Co2 C2 Co1 78.2(2) . . ? C4 C3 C8 116.8(8) . . ? C4 C3 C1 123.5(7) . . ? C8 C3 C1 119.7(7) . . ? C3 C4 C5 122.3(9) . . ? C6 C5 C4 121.7(10) . . ? C5 C6 C7 117.3(9) . . ? C6 C7 C8 121.8(9) . . ? C3 C8 C7 120.1(9) . . ? O1 C9 C2 106.7(5) . . ? O1 C9 C10 111.0(6) . . ? C2 C9 C10 112.5(6) . . ? C9 C10 C11 110.3(6) . . ? C12 C11 C10 114.2(6) . . ? C16 C12 C14 109.7(6) . . ? C16 C12 C11 109.9(7) . . ? C14 C12 C11 105.9(6) . . ? C16 C12 C13 113.2(6) . . ? C14 C12 C13 111.1(6) . . ? C11 C12 C13 106.8(6) . . ? O1 C13 C18 106.8(5) . . ? O1 C13 C12 107.2(5) . . ? C18 C13 C12 119.9(6) . . ? C9 O1 C13 112.8(5) . . ? O2 C14 O3 123.9(7) . . ? O2 C14 C12 125.3(6) . . ? O3 C14 C12 110.5(6) . . ? C14 O3 C15 116.9(7) . . ? O4 C16 O4X 127.5(17) . . ? O4X C16 O5X 116.1(15) . . ? O4 C16 O5 123.4(12) . . ? O5X C16 O5 106.0(16) . . ? O4 C16 C12 120.6(11) . . ? O4X C16 C12 109.5(15) . . ? O5X C16 C12 133.9(13) . . ? O5 C16 C12 115.9(11) . . ? C16 O5 C17 111.0(15) . . ? C16 O5X C17X 112.1(18) . . ? C23 C18 C19 117.9(8) . . ? C23 C18 C13 121.9(7) . . ? C19 C18 C13 119.9(7) . . ? C20 C19 C18 121.0(8) . . ? C19 C20 C21 121.7(8) . . ? C20 C21 C22 117.6(8) . . ? C20 C21 C24 122.0(8) . . ? C22 C21 C24 120.3(8) . . ? C23 C22 C21 120.9(8) . . ? C18 C23 C22 120.9(8) . . ? O25 C25 Co1 178.7(6) . . ? O26 C26 Co1 177.3(8) . . ? O27 C27 Co1 177.1(6) . . ? O28 C28 Co2 177.9(7) . . ? O29 C29 Co2 177.7(7) . . ? O30 C30 Co2 176.3(6) . . ? C31 Cl1 Cl2X 136.0(7) . 2_655 ? C31X Cl1 Cl2X 113.7(12) . 2_655 ? Cl1 C31 Cl2 114.8(8) . . ? Cl1 C31X Cl2X 103.4(13) . . ? C31X Cl2X Cl1 99.5(14) . 2_655 ? 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 C27 Co1 Co2 C30 -28.9(6) . . . . ? C25 Co1 Co2 C30 106.7(5) . . . . ? C26 Co1 Co2 C30 -146.3(5) . . . . ? C2 Co1 Co2 C30 14.2(5) . . . . ? C1 Co1 Co2 C30 -37.9(5) . . . . ? C27 Co1 Co2 C29 -147.0(5) . . . . ? C25 Co1 Co2 C29 -11.5(3) . . . . ? C26 Co1 Co2 C29 95.6(3) . . . . ? C2 Co1 Co2 C29 -103.9(3) . . . . ? C1 Co1 Co2 C29 -156.0(3) . . . . ? C27 Co1 Co2 C28 106.7(5) . . . . ? C25 Co1 Co2 C28 -117.7(3) . . . . ? C26 Co1 Co2 C28 -10.7(4) . . . . ? C2 Co1 Co2 C28 149.9(4) . . . . ? C1 Co1 Co2 C28 97.8(4) . . . . ? C27 Co1 Co2 C2 -43.1(5) . . . . ? C25 Co1 Co2 C2 92.4(3) . . . . ? C26 Co1 Co2 C2 -160.5(4) . . . . ? C1 Co1 Co2 C2 -52.1(4) . . . . ? C27 Co1 Co2 C1 9.0(5) . . . . ? C25 Co1 Co2 C1 144.5(3) . . . . ? C26 Co1 Co2 C1 -108.4(4) . . . . ? C2 Co1 Co2 C1 52.1(4) . . . . ? C30 Co2 C1 C2 87.1(4) . . . . ? C29 Co2 C1 C2 -32.6(7) . . . . ? C28 Co2 C1 C2 -166.4(4) . . . . ? Co1 Co2 C1 C2 -72.7(4) . . . . ? C30 Co2 C1 C3 -58.1(7) . . . . ? C29 Co2 C1 C3 -177.9(6) . . . . ? C28 Co2 C1 C3 48.3(8) . . . . ? C2 Co2 C1 C3 -145.3(9) . . . . ? Co1 Co2 C1 C3 142.0(8) . . . . ? C30 Co2 C1 Co1 159.8(3) . . . . ? C29 Co2 C1 Co1 40.1(5) . . . . ? C28 Co2 C1 Co1 -93.7(3) . . . . ? C2 Co2 C1 Co1 72.7(4) . . . . ? C27 Co1 C1 C2 -102.7(4) . . . . ? C25 Co1 C1 C2 13.7(6) . . . . ? C26 Co1 C1 C2 156.2(4) . . . . ? Co2 Co1 C1 C2 72.4(4) . . . . ? C27 Co1 C1 C3 42.9(7) . . . . ? C25 Co1 C1 C3 159.2(6) . . . . ? C26 Co1 C1 C3 -58.2(7) . . . . ? C2 Co1 C1 C3 145.6(8) . . . . ? Co2 Co1 C1 C3 -142.1(7) . . . . ? C27 Co1 C1 Co2 -175.0(3) . . . . ? C25 Co1 C1 Co2 -58.7(4) . . . . ? C26 Co1 C1 Co2 83.8(3) . . . . ? C2 Co1 C1 Co2 -72.4(4) . . . . ? C3 C1 C2 C9 1.7(17) . . . . ? Co2 C1 C2 C9 -136.1(10) . . . . ? Co1 C1 C2 C9 139.9(10) . . . . ? C3 C1 C2 Co2 137.8(10) . . . . ? Co1 C1 C2 Co2 -83.95(19) . . . . ? C3 C1 C2 Co1 -138.2(10) . . . . ? Co2 C1 C2 Co1 83.95(19) . . . . ? C30 Co2 C2 C1 -98.9(5) . . . . ? C29 Co2 C2 C1 159.5(4) . . . . ? C28 Co2 C2 C1 21.4(7) . . . . ? Co1 Co2 C2 C1 73.2(4) . . . . ? C30 Co2 C2 C9 46.4(7) . . . . ? C29 Co2 C2 C9 -55.2(7) . . . . ? C28 Co2 C2 C9 166.8(6) . . . . ? C1 Co2 C2 C9 145.3(8) . . . . ? Co1 Co2 C2 C9 -141.4(7) . . . . ? C30 Co2 C2 Co1 -172.1(3) . . . . ? C29 Co2 C2 Co1 86.3(3) . . . . ? C28 Co2 C2 Co1 -51.8(5) . . . . ? C1 Co2 C2 Co1 -73.2(4) . . . . ? C27 Co1 C2 C1 83.9(4) . . . . ? C25 Co1 C2 C1 -170.8(4) . . . . ? C26 Co1 C2 C1 -39.8(7) . . . . ? Co2 Co1 C2 C1 -73.4(4) . . . . ? C27 Co1 C2 C9 -62.9(7) . . . . ? C25 Co1 C2 C9 42.3(7) . . . . ? C26 Co1 C2 C9 173.4(6) . . . . ? C1 Co1 C2 C9 -146.8(9) . . . . ? Co2 Co1 C2 C9 139.8(8) . . . . ? C27 Co1 C2 Co2 157.3(3) . . . . ? C25 Co1 C2 Co2 -97.4(3) . . . . ? C26 Co1 C2 Co2 33.6(6) . . . . ? C1 Co1 C2 Co2 73.4(4) . . . . ? C2 C1 C3 C4 178.8(12) . . . . ? Co2 C1 C3 C4 -62.9(13) . . . . ? Co1 C1 C3 C4 59.8(13) . . . . ? C2 C1 C3 C8 -3.4(14) . . . . ? Co2 C1 C3 C8 114.9(9) . . . . ? Co1 C1 C3 C8 -122.4(8) . . . . ? C8 C3 C4 C5 1(2) . . . . ? C1 C3 C4 C5 178.6(13) . . . . ? C3 C4 C5 C6 1(3) . . . . ? C4 C5 C6 C7 -2(2) . . . . ? C5 C6 C7 C8 2(2) . . . . ? C4 C3 C8 C7 -1.1(17) . . . . ? C1 C3 C8 C7 -179.0(10) . . . . ? C6 C7 C8 C3 0(2) . . . . ? C1 C2 C9 O1 164.7(9) . . . . ? Co2 C2 C9 O1 47.2(8) . . . . ? Co1 C2 C9 O1 -73.7(8) . . . . ? C1 C2 C9 C10 -73.3(11) . . . . ? Co2 C2 C9 C10 169.2(5) . . . . ? Co1 C2 C9 C10 48.2(9) . . . . ? O1 C9 C10 C11 -50.2(8) . . . . ? C2 C9 C10 C11 -169.7(6) . . . . ? C9 C10 C11 C12 47.9(9) . . . . ? C10 C11 C12 C16 70.7(8) . . . . ? C10 C11 C12 C14 -170.9(6) . . . . ? C10 C11 C12 C13 -52.4(8) . . . . ? C16 C12 C13 O1 -61.2(9) . . . . ? C14 C12 C13 O1 174.9(6) . . . . ? C11 C12 C13 O1 59.9(7) . . . . ? C16 C12 C13 C18 60.6(9) . . . . ? C14 C12 C13 C18 -63.3(8) . . . . ? C11 C12 C13 C18 -178.4(6) . . . . ? C2 C9 O1 C13 -173.5(5) . . . . ? C10 C9 O1 C13 63.6(7) . . . . ? C18 C13 O1 C9 162.0(5) . . . . ? C12 C13 O1 C9 -68.3(7) . . . . ? C16 C12 C14 O2 -148.2(9) . . . . ? C11 C12 C14 O2 93.3(9) . . . . ? C13 C12 C14 O2 -22.3(11) . . . . ? C16 C12 C14 O3 37.5(10) . . . . ? C11 C12 C14 O3 -81.0(8) . . . . ? C13 C12 C14 O3 163.3(7) . . . . ? O2 C14 O3 C15 3.2(14) . . . . ? C12 C14 O3 C15 177.7(8) . . . . ? C14 C12 C16 O4 -118.9(11) . . . . ? C11 C12 C16 O4 -2.9(11) . . . . ? C13 C12 C16 O4 116.4(11) . . . . ? C14 C12 C16 O4X 44.7(17) . . . . ? C11 C12 C16 O4X 160.7(16) . . . . ? C13 C12 C16 O4X -80.0(16) . . . . ? C14 C12 C16 O5X -144.6(19) . . . . ? C11 C12 C16 O5X -29(2) . . . . ? C13 C12 C16 O5X 91(2) . . . . ? C14 C12 C16 O5 62.2(13) . . . . ? C11 C12 C16 O5 178.2(11) . . . . ? C13 C12 C16 O5 -62.5(13) . . . . ? O4 C16 O5 C17 5(2) . . . . ? O4X C16 O5 C17 -104(8) . . . . ? O5X C16 O5 C17 24(2) . . . . ? C12 C16 O5 C17 -175.9(12) . . . . ? O4 C16 O5X C17X 122(5) . . . . ? O4X C16 O5X C17X -2(3) . . . . ? O5 C16 O5X C17X -17(3) . . . . ? C12 C16 O5X C17X -172.4(15) . . . . ? O1 C13 C18 C23 38.5(8) . . . . ? C12 C13 C18 C23 -83.5(8) . . . . ? O1 C13 C18 C19 -135.1(6) . . . . ? C12 C13 C18 C19 102.9(8) . . . . ? C23 C18 C19 C20 0.8(11) . . . . ? C13 C18 C19 C20 174.7(7) . . . . ? C18 C19 C20 C21 -0.2(12) . . . . ? C19 C20 C21 C22 0.1(12) . . . . ? C19 C20 C21 C24 -179.6(8) . . . . ? C20 C21 C22 C23 -0.6(11) . . . . ? C24 C21 C22 C23 179.1(7) . . . . ? C19 C18 C23 C22 -1.3(10) . . . . ? C13 C18 C23 C22 -175.0(6) . . . . ? C21 C22 C23 C18 1.2(11) . . . . ? C31X Cl1 C31 Cl2 -61.5(19) . . . . ? Cl2X Cl1 C31 Cl2 -118.1(10) 2_655 . . . ? C31 Cl1 C31X Cl2X 146(3) . . . . ? Cl2X Cl1 C31X Cl2X -73.2(16) 2_655 . . . ? Cl1 C31X Cl2X Cl1 62.7(15) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.322 _refine_diff_density_min -1.730 _refine_diff_density_rms 0.137 #===END data_18 _database_code_depnum_ccdc_archive 'CCDC 745434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H20 Co2 O12' _chemical_formula_sum 'C27 H20 Co2 O12' _chemical_formula_weight 654.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0886(5) _cell_length_b 11.7239(7) _cell_length_c 15.7788(9) _cell_angle_alpha 106.5335(8) _cell_angle_beta 102.7961(9) _cell_angle_gamma 91.9661(9) _cell_volume 1391.20(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6766 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 31.37 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 1.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16756 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 31.85 _reflns_number_total 8572 _reflns_number_gt 6949 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0377P)^2^+0.3533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 8572 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.17853(3) 0.613819(18) 0.359208(13) 0.02330(5) Uani 1 1 d . . . Co2 Co 0.47441(3) 0.711231(18) 0.412678(13) 0.02359(6) Uani 1 1 d . . . C1 C 0.27912(18) 0.74700(13) 0.32769(10) 0.0222(3) Uani 1 1 d . . . C2 C 0.33603(18) 0.64378(13) 0.28790(9) 0.0211(3) Uani 1 1 d . . . C3 C 0.22940(19) 0.85987(13) 0.31261(10) 0.0249(3) Uani 1 1 d . . . C4 C 0.1552(2) 0.93972(15) 0.37349(12) 0.0340(4) Uani 1 1 d . . . H4 H 0.1344 0.9208 0.4251 0.041 Uiso 1 1 calc R . . C5 C 0.1116(3) 1.04751(16) 0.35829(15) 0.0484(5) Uani 1 1 d . . . H5 H 0.0614 1.1021 0.3999 0.058 Uiso 1 1 calc R . . C6 C 0.1408(3) 1.07552(16) 0.28356(16) 0.0524(6) Uani 1 1 d . . . H6 H 0.1091 1.1487 0.2734 0.063 Uiso 1 1 calc R . . C7 C 0.2156(3) 0.99785(17) 0.22349(15) 0.0461(5) Uani 1 1 d . . . H7 H 0.2367 1.0179 0.1723 0.055 Uiso 1 1 calc R . . C8 C 0.2603(2) 0.89034(15) 0.23765(12) 0.0337(4) Uani 1 1 d . . . H8 H 0.3122 0.8371 0.1961 0.040 Uiso 1 1 calc R . . C9 C 0.36664(18) 0.57198(12) 0.19950(9) 0.0203(3) Uani 1 1 d . . . H9 H 0.4633 0.6139 0.1863 0.024 Uiso 1 1 calc R . . C10 C 0.20920(19) 0.55464(13) 0.12172(9) 0.0234(3) Uani 1 1 d . . . H10A H 0.1835 0.6331 0.1130 0.028 Uiso 1 1 calc R . . H10B H 0.1102 0.5206 0.1372 0.028 Uiso 1 1 calc R . . C11 C 0.23765(18) 0.47094(13) 0.03367(9) 0.0215(3) Uani 1 1 d . . . H11A H 0.3264 0.5098 0.0138 0.026 Uiso 1 1 calc R . . H11B H 0.1308 0.4549 -0.0147 0.026 Uiso 1 1 calc R . . C12 C 0.29395(17) 0.35137(12) 0.04776(9) 0.0181(2) Uani 1 1 d . . . C13 C 0.45313(17) 0.38334(12) 0.12891(9) 0.0188(2) Uani 1 1 d . . . H13 H 0.5433 0.4286 0.1133 0.023 Uiso 1 1 calc R . . O1 O 0.41297(13) 0.45811(9) 0.20874(6) 0.02058(19) Uani 1 1 d . . . C14 C 0.34120(17) 0.28497(12) -0.04011(9) 0.0193(2) Uani 1 1 d . . . O2 O 0.47038(14) 0.31016(10) -0.05948(7) 0.0272(2) Uani 1 1 d . . . O3 O 0.21763(14) 0.20272(10) -0.09536(7) 0.0285(2) Uani 1 1 d . . . C15 C 0.2406(2) 0.15080(16) -0.18663(11) 0.0358(4) Uani 1 1 d . . . H15A H 0.2379 0.2128 -0.2174 0.054 Uiso 1 1 calc R . . H15B H 0.1487 0.0869 -0.2211 0.054 Uiso 1 1 calc R . . H15C H 0.3506 0.1177 -0.1831 0.054 Uiso 1 1 calc R . . C16 C 0.15326(18) 0.27764(14) 0.06620(10) 0.0228(3) Uani 1 1 d . . . O4 O 0.17719(15) 0.20783(13) 0.10882(10) 0.0408(3) Uani 1 1 d . . . O5 O -0.00167(13) 0.30159(11) 0.02895(8) 0.0304(2) Uani 1 1 d . . . C17 C -0.1414(2) 0.2318(2) 0.04042(14) 0.0427(5) Uani 1 1 d . . . H17A H -0.1324 0.1465 0.0141 0.064 Uiso 1 1 calc R . . H17B H -0.2497 0.2528 0.0095 0.064 Uiso 1 1 calc R . . H17C H -0.1367 0.2489 0.1055 0.064 Uiso 1 1 calc R . . C18 C 0.52692(18) 0.27966(13) 0.15444(9) 0.0211(3) Uani 1 1 d . . . C19 C 0.6048(2) 0.26480(15) 0.23472(11) 0.0338(4) Uani 1 1 d . . . H19 H 0.6250 0.3225 0.2930 0.041 Uiso 1 1 calc R . . C20 C 0.6509(2) 0.14538(16) 0.21504(11) 0.0349(4) Uani 1 1 d . . . H20 H 0.7075 0.1080 0.2578 0.042 Uiso 1 1 calc R . . C21 C 0.5991(2) 0.09598(14) 0.12444(11) 0.0286(3) Uani 1 1 d . . . H21 H 0.6131 0.0164 0.0924 0.034 Uiso 1 1 calc R . . O6 O 0.52275(13) 0.17734(9) 0.08480(7) 0.0236(2) Uani 1 1 d . . . C22 C 0.2214(2) 0.46000(15) 0.35496(11) 0.0330(3) Uani 1 1 d . . . O22 O 0.2525(2) 0.36643(11) 0.35316(10) 0.0510(4) Uani 1 1 d . . . C23 C 0.1114(2) 0.66901(16) 0.46465(13) 0.0356(4) Uani 1 1 d . . . O23 O 0.0693(2) 0.70113(14) 0.53089(10) 0.0553(4) Uani 1 1 d . . . C24 C -0.0278(2) 0.58860(16) 0.28227(13) 0.0363(4) Uani 1 1 d . . . O24 O -0.15888(18) 0.57394(15) 0.23409(11) 0.0564(4) Uani 1 1 d . . . C25 C 0.4580(2) 0.80327(17) 0.52444(11) 0.0354(4) Uani 1 1 d . . . O25 O 0.4394(2) 0.86360(16) 0.59099(9) 0.0583(4) Uani 1 1 d . . . C26 C 0.5931(2) 0.58608(17) 0.42687(11) 0.0378(4) Uani 1 1 d . . . O26 O 0.6674(2) 0.50741(14) 0.43219(10) 0.0596(5) Uani 1 1 d . . . C27 C 0.6379(2) 0.80649(17) 0.39916(11) 0.0348(4) Uani 1 1 d . . . O27 O 0.7388(2) 0.86880(16) 0.39044(10) 0.0602(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02730(11) 0.02093(10) 0.02290(10) 0.00703(8) 0.00780(8) 0.00344(8) Co2 0.02525(10) 0.02711(11) 0.01689(9) 0.00593(8) 0.00248(7) 0.00512(8) C1 0.0232(7) 0.0209(6) 0.0212(6) 0.0066(5) 0.0027(5) 0.0017(5) C2 0.0211(6) 0.0232(7) 0.0186(6) 0.0077(5) 0.0018(5) 0.0028(5) C3 0.0235(7) 0.0186(6) 0.0275(7) 0.0052(5) -0.0020(6) 0.0001(5) C4 0.0345(8) 0.0250(8) 0.0324(8) 0.0000(6) -0.0016(7) 0.0058(6) C5 0.0440(11) 0.0221(8) 0.0567(12) -0.0057(8) -0.0113(9) 0.0109(7) C6 0.0487(11) 0.0206(8) 0.0719(15) 0.0172(9) -0.0215(10) -0.0034(8) C7 0.0457(11) 0.0339(10) 0.0573(12) 0.0268(9) -0.0057(9) -0.0061(8) C8 0.0345(9) 0.0291(8) 0.0378(9) 0.0158(7) 0.0027(7) -0.0012(7) C9 0.0236(6) 0.0205(6) 0.0172(6) 0.0072(5) 0.0033(5) 0.0049(5) C10 0.0264(7) 0.0236(7) 0.0188(6) 0.0069(5) 0.0011(5) 0.0080(5) C11 0.0234(6) 0.0230(7) 0.0177(6) 0.0084(5) 0.0014(5) 0.0029(5) C12 0.0165(6) 0.0208(6) 0.0176(6) 0.0071(5) 0.0033(5) 0.0019(5) C13 0.0171(6) 0.0226(6) 0.0168(6) 0.0064(5) 0.0038(5) 0.0035(5) O1 0.0240(5) 0.0221(5) 0.0164(4) 0.0069(4) 0.0044(4) 0.0078(4) C14 0.0204(6) 0.0198(6) 0.0173(6) 0.0074(5) 0.0016(5) 0.0014(5) O2 0.0260(5) 0.0326(6) 0.0226(5) 0.0058(4) 0.0091(4) -0.0036(4) O3 0.0258(5) 0.0293(6) 0.0234(5) -0.0006(4) 0.0036(4) -0.0046(4) C15 0.0417(10) 0.0338(9) 0.0219(7) -0.0025(6) 0.0017(7) 0.0035(7) C16 0.0176(6) 0.0286(7) 0.0236(7) 0.0101(6) 0.0046(5) 0.0017(5) O4 0.0245(6) 0.0534(8) 0.0590(8) 0.0412(7) 0.0079(5) 0.0019(5) O5 0.0157(5) 0.0435(7) 0.0373(6) 0.0217(5) 0.0046(4) 0.0017(4) C17 0.0180(7) 0.0670(13) 0.0503(11) 0.0293(10) 0.0087(7) -0.0037(8) C18 0.0197(6) 0.0239(7) 0.0197(6) 0.0059(5) 0.0052(5) 0.0063(5) C19 0.0455(10) 0.0327(8) 0.0214(7) 0.0072(6) 0.0035(7) 0.0186(7) C20 0.0447(10) 0.0345(9) 0.0284(8) 0.0136(7) 0.0067(7) 0.0196(7) C21 0.0337(8) 0.0257(7) 0.0293(7) 0.0110(6) 0.0088(6) 0.0112(6) O6 0.0271(5) 0.0226(5) 0.0208(5) 0.0068(4) 0.0043(4) 0.0062(4) C22 0.0465(10) 0.0264(8) 0.0267(8) 0.0076(6) 0.0111(7) 0.0015(7) O22 0.0850(11) 0.0244(6) 0.0466(8) 0.0119(6) 0.0198(8) 0.0096(7) C23 0.0389(9) 0.0309(9) 0.0398(9) 0.0089(7) 0.0169(8) 0.0052(7) O23 0.0687(10) 0.0549(9) 0.0489(8) 0.0071(7) 0.0377(8) 0.0143(8) C24 0.0325(9) 0.0372(9) 0.0408(9) 0.0132(8) 0.0107(7) 0.0009(7) O24 0.0302(7) 0.0700(11) 0.0636(10) 0.0219(8) -0.0010(7) -0.0019(7) C25 0.0325(8) 0.0463(10) 0.0238(7) 0.0070(7) 0.0043(6) 0.0006(7) O25 0.0541(9) 0.0786(11) 0.0278(7) -0.0083(7) 0.0134(6) -0.0001(8) C26 0.0429(10) 0.0415(10) 0.0228(7) 0.0073(7) -0.0028(7) 0.0120(8) O26 0.0767(11) 0.0537(9) 0.0375(8) 0.0093(7) -0.0074(7) 0.0363(8) C27 0.0312(8) 0.0473(10) 0.0200(7) 0.0036(7) 0.0035(6) -0.0002(7) O27 0.0528(9) 0.0792(12) 0.0418(8) 0.0082(8) 0.0150(7) -0.0254(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C24 1.7919(19) . ? Co1 C23 1.8145(17) . ? Co1 C22 1.8333(17) . ? Co1 C2 1.9599(14) . ? Co1 C1 1.9701(14) . ? Co1 Co2 2.4725(3) . ? Co2 C27 1.7892(19) . ? Co2 C26 1.8203(18) . ? Co2 C25 1.8226(17) . ? Co2 C2 1.9574(14) . ? Co2 C1 1.9740(14) . ? C1 C2 1.343(2) . ? C1 C3 1.464(2) . ? C2 C9 1.4881(19) . ? C3 C4 1.393(2) . ? C3 C8 1.398(2) . ? C4 C5 1.394(2) . ? C5 C6 1.375(3) . ? C6 C7 1.377(3) . ? C7 C8 1.388(2) . ? C9 O1 1.4369(16) . ? C9 C10 1.5222(19) . ? C10 C11 1.5256(19) . ? C11 C12 1.5487(19) . ? C12 C14 1.5216(18) . ? C12 C16 1.5327(19) . ? C12 C13 1.5495(18) . ? C13 O1 1.4259(16) . ? C13 C18 1.4893(19) . ? C14 O2 1.2017(17) . ? C14 O3 1.3260(17) . ? O3 C15 1.4512(19) . ? C16 O4 1.1942(18) . ? C16 O5 1.3367(17) . ? O5 C17 1.4457(19) . ? C18 C19 1.346(2) . ? C18 O6 1.3704(17) . ? C19 C20 1.427(2) . ? C20 C21 1.342(2) . ? C21 O6 1.3753(18) . ? C22 O22 1.128(2) . ? C23 O23 1.137(2) . ? C24 O24 1.135(2) . ? C25 O25 1.131(2) . ? C26 O26 1.131(2) . ? C27 O27 1.133(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Co1 C23 97.80(8) . . ? C24 Co1 C22 100.95(8) . . ? C23 Co1 C22 103.51(8) . . ? C24 Co1 C2 104.47(7) . . ? C23 Co1 C2 145.23(7) . . ? C22 Co1 C2 98.11(7) . . ? C24 Co1 C1 99.55(7) . . ? C23 Co1 C1 110.55(7) . . ? C22 Co1 C1 137.05(7) . . ? C2 Co1 C1 39.97(6) . . ? C24 Co1 Co2 150.22(6) . . ? C23 Co1 Co2 98.52(6) . . ? C22 Co1 Co2 99.22(6) . . ? C2 Co1 Co2 50.82(4) . . ? C1 Co1 Co2 51.25(4) . . ? C27 Co2 C26 100.03(9) . . ? C27 Co2 C25 97.18(8) . . ? C26 Co2 C25 108.61(8) . . ? C27 Co2 C2 102.59(7) . . ? C26 Co2 C2 101.05(7) . . ? C25 Co2 C2 140.64(7) . . ? C27 Co2 C1 98.52(7) . . ? C26 Co2 C1 139.91(7) . . ? C25 Co2 C1 103.89(7) . . ? C2 Co2 C1 39.95(6) . . ? C27 Co2 Co1 148.81(6) . . ? C26 Co2 Co1 101.22(6) . . ? C25 Co2 Co1 97.37(6) . . ? C2 Co2 Co1 50.91(4) . . ? C1 Co2 Co1 51.11(4) . . ? C2 C1 C3 142.12(14) . . ? C2 C1 Co1 69.61(9) . . ? C3 C1 Co1 137.71(11) . . ? C2 C1 Co2 69.36(8) . . ? C3 C1 Co2 131.57(10) . . ? Co1 C1 Co2 77.64(5) . . ? C1 C2 C9 142.12(13) . . ? C1 C2 Co2 70.69(9) . . ? C9 C2 Co2 135.73(10) . . ? C1 C2 Co1 70.42(9) . . ? C9 C2 Co1 131.91(10) . . ? Co2 C2 Co1 78.27(5) . . ? C4 C3 C8 119.03(15) . . ? C4 C3 C1 120.90(14) . . ? C8 C3 C1 120.05(14) . . ? C3 C4 C5 119.72(18) . . ? C6 C5 C4 120.57(19) . . ? C5 C6 C7 120.20(17) . . ? C6 C7 C8 120.03(19) . . ? C7 C8 C3 120.45(18) . . ? O1 C9 C2 107.64(10) . . ? O1 C9 C10 110.20(11) . . ? C2 C9 C10 111.54(11) . . ? C9 C10 C11 110.62(11) . . ? C10 C11 C12 110.68(11) . . ? C14 C12 C16 110.98(11) . . ? C14 C12 C11 104.87(10) . . ? C16 C12 C11 112.66(11) . . ? C14 C12 C13 110.53(10) . . ? C16 C12 C13 110.72(11) . . ? C11 C12 C13 106.87(11) . . ? O1 C13 C18 106.01(10) . . ? O1 C13 C12 110.33(10) . . ? C18 C13 C12 115.42(11) . . ? C13 O1 C9 112.57(10) . . ? O2 C14 O3 124.15(13) . . ? O2 C14 C12 123.63(12) . . ? O3 C14 C12 112.03(11) . . ? C14 O3 C15 114.99(12) . . ? O4 C16 O5 123.60(13) . . ? O4 C16 C12 124.89(13) . . ? O5 C16 C12 111.50(12) . . ? C16 O5 C17 114.70(13) . . ? C19 C18 O6 110.23(13) . . ? C19 C18 C13 132.82(13) . . ? O6 C18 C13 116.92(11) . . ? C18 C19 C20 106.52(14) . . ? C21 C20 C19 106.81(14) . . ? C20 C21 O6 110.07(14) . . ? C18 O6 C21 106.36(11) . . ? O22 C22 Co1 178.08(18) . . ? O23 C23 Co1 178.50(17) . . ? O24 C24 Co1 179.2(2) . . ? O25 C25 Co2 175.51(17) . . ? O26 C26 Co2 177.24(16) . . ? O27 C27 Co2 178.36(19) . . ? 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 C24 Co1 Co2 C27 -2.28(17) . . . . ? C23 Co1 Co2 C27 -124.83(13) . . . . ? C22 Co1 Co2 C27 129.88(12) . . . . ? C2 Co1 Co2 C27 36.89(12) . . . . ? C1 Co1 Co2 C27 -15.26(12) . . . . ? C24 Co1 Co2 C26 -134.38(13) . . . . ? C23 Co1 Co2 C26 103.07(8) . . . . ? C22 Co1 Co2 C26 -2.22(7) . . . . ? C2 Co1 Co2 C26 -95.21(8) . . . . ? C1 Co1 Co2 C26 -147.36(8) . . . . ? C24 Co1 Co2 C25 114.92(13) . . . . ? C23 Co1 Co2 C25 -7.64(8) . . . . ? C22 Co1 Co2 C25 -112.93(8) . . . . ? C2 Co1 Co2 C25 154.09(8) . . . . ? C1 Co1 Co2 C25 101.93(8) . . . . ? C24 Co1 Co2 C2 -39.17(13) . . . . ? C23 Co1 Co2 C2 -161.72(8) . . . . ? C22 Co1 Co2 C2 92.99(7) . . . . ? C1 Co1 Co2 C2 -52.15(7) . . . . ? C24 Co1 Co2 C1 12.98(13) . . . . ? C23 Co1 Co2 C1 -109.57(8) . . . . ? C22 Co1 Co2 C1 145.14(7) . . . . ? C2 Co1 Co2 C1 52.15(7) . . . . ? C24 Co1 C1 C2 -101.18(10) . . . . ? C23 Co1 C1 C2 156.70(10) . . . . ? C22 Co1 C1 C2 16.43(14) . . . . ? Co2 Co1 C1 C2 72.33(8) . . . . ? C24 Co1 C1 C3 46.26(17) . . . . ? C23 Co1 C1 C3 -55.87(17) . . . . ? C22 Co1 C1 C3 163.86(14) . . . . ? C2 Co1 C1 C3 147.4(2) . . . . ? Co2 Co1 C1 C3 -140.24(17) . . . . ? C24 Co1 C1 Co2 -173.50(7) . . . . ? C23 Co1 C1 Co2 84.37(8) . . . . ? C22 Co1 C1 Co2 -55.90(11) . . . . ? C2 Co1 C1 Co2 -72.33(8) . . . . ? C27 Co2 C1 C2 99.46(10) . . . . ? C26 Co2 C1 C2 -17.38(15) . . . . ? C25 Co2 C1 C2 -160.91(10) . . . . ? Co1 Co2 C1 C2 -72.62(8) . . . . ? C27 Co2 C1 C3 -43.04(15) . . . . ? C26 Co2 C1 C3 -159.88(15) . . . . ? C25 Co2 C1 C3 56.60(16) . . . . ? C2 Co2 C1 C3 -142.49(19) . . . . ? Co1 Co2 C1 C3 144.88(16) . . . . ? C27 Co2 C1 Co1 172.08(6) . . . . ? C26 Co2 C1 Co1 55.24(12) . . . . ? C25 Co2 C1 Co1 -88.29(7) . . . . ? C2 Co2 C1 Co1 72.62(8) . . . . ? C3 C1 C2 C9 -9.6(4) . . . . ? Co1 C1 C2 C9 134.2(2) . . . . ? Co2 C1 C2 C9 -141.7(2) . . . . ? C3 C1 C2 Co2 132.1(2) . . . . ? Co1 C1 C2 Co2 -84.03(4) . . . . ? C3 C1 C2 Co1 -143.9(2) . . . . ? Co2 C1 C2 Co1 84.03(4) . . . . ? C27 Co2 C2 C1 -88.27(10) . . . . ? C26 Co2 C2 C1 168.69(10) . . . . ? C25 Co2 C2 C1 30.04(15) . . . . ? Co1 Co2 C2 C1 73.15(8) . . . . ? C27 Co2 C2 C9 58.72(16) . . . . ? C26 Co2 C2 C9 -44.31(16) . . . . ? C25 Co2 C2 C9 177.04(14) . . . . ? C1 Co2 C2 C9 147.00(19) . . . . ? Co1 Co2 C2 C9 -139.85(17) . . . . ? C27 Co2 C2 Co1 -161.42(7) . . . . ? C26 Co2 C2 Co1 95.54(7) . . . . ? C25 Co2 C2 Co1 -43.11(12) . . . . ? C1 Co2 C2 Co1 -73.15(8) . . . . ? C24 Co1 C2 C1 87.64(10) . . . . ? C23 Co1 C2 C1 -40.51(16) . . . . ? C22 Co1 C2 C1 -168.77(10) . . . . ? Co2 Co1 C2 C1 -73.46(8) . . . . ? C24 Co1 C2 C9 -56.12(14) . . . . ? C23 Co1 C2 C9 175.74(13) . . . . ? C22 Co1 C2 C9 47.47(14) . . . . ? C1 Co1 C2 C9 -143.75(17) . . . . ? Co2 Co1 C2 C9 142.79(15) . . . . ? C24 Co1 C2 Co2 161.10(7) . . . . ? C23 Co1 C2 Co2 32.95(14) . . . . ? C22 Co1 C2 Co2 -95.31(7) . . . . ? C1 Co1 C2 Co2 73.46(8) . . . . ? C2 C1 C3 C4 172.05(19) . . . . ? Co1 C1 C3 C4 47.3(2) . . . . ? Co2 C1 C3 C4 -76.07(19) . . . . ? C2 C1 C3 C8 -9.7(3) . . . . ? Co1 C1 C3 C8 -134.41(15) . . . . ? Co2 C1 C3 C8 102.22(17) . . . . ? C8 C3 C4 C5 0.6(2) . . . . ? C1 C3 C4 C5 178.95(15) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C7 -0.9(3) . . . . ? C5 C6 C7 C8 0.7(3) . . . . ? C6 C7 C8 C3 0.2(3) . . . . ? C4 C3 C8 C7 -0.8(2) . . . . ? C1 C3 C8 C7 -179.15(15) . . . . ? C1 C2 C9 O1 -172.76(19) . . . . ? Co2 C2 C9 O1 64.08(17) . . . . ? Co1 C2 C9 O1 -57.89(16) . . . . ? C1 C2 C9 C10 -51.8(3) . . . . ? Co2 C2 C9 C10 -174.92(11) . . . . ? Co1 C2 C9 C10 63.11(16) . . . . ? O1 C9 C10 C11 -55.01(15) . . . . ? C2 C9 C10 C11 -174.51(12) . . . . ? C9 C10 C11 C12 54.14(15) . . . . ? C10 C11 C12 C14 -172.32(11) . . . . ? C10 C11 C12 C16 66.87(15) . . . . ? C10 C11 C12 C13 -54.95(14) . . . . ? C14 C12 C13 O1 172.84(10) . . . . ? C16 C12 C13 O1 -63.77(14) . . . . ? C11 C12 C13 O1 59.26(13) . . . . ? C14 C12 C13 C18 -67.04(14) . . . . ? C16 C12 C13 C18 56.36(15) . . . . ? C11 C12 C13 C18 179.39(11) . . . . ? C18 C13 O1 C9 170.30(11) . . . . ? C12 C13 O1 C9 -64.07(14) . . . . ? C2 C9 O1 C13 -177.31(11) . . . . ? C10 C9 O1 C13 60.85(14) . . . . ? C16 C12 C14 O2 -163.02(13) . . . . ? C11 C12 C14 O2 75.06(16) . . . . ? C13 C12 C14 O2 -39.78(18) . . . . ? C16 C12 C14 O3 21.83(15) . . . . ? C11 C12 C14 O3 -100.09(13) . . . . ? C13 C12 C14 O3 145.07(12) . . . . ? O2 C14 O3 C15 -5.6(2) . . . . ? C12 C14 O3 C15 169.49(12) . . . . ? C14 C12 C16 O4 90.20(18) . . . . ? C11 C12 C16 O4 -152.55(16) . . . . ? C13 C12 C16 O4 -32.9(2) . . . . ? C14 C12 C16 O5 -90.23(14) . . . . ? C11 C12 C16 O5 27.02(16) . . . . ? C13 C12 C16 O5 146.63(12) . . . . ? O4 C16 O5 C17 -2.8(2) . . . . ? C12 C16 O5 C17 177.67(14) . . . . ? O1 C13 C18 C19 -23.7(2) . . . . ? C12 C13 C18 C19 -146.12(17) . . . . ? O1 C13 C18 O6 158.54(11) . . . . ? C12 C13 C18 O6 36.08(17) . . . . ? O6 C18 C19 C20 -0.7(2) . . . . ? C13 C18 C19 C20 -178.65(15) . . . . ? C18 C19 C20 C21 0.3(2) . . . . ? C19 C20 C21 O6 0.2(2) . . . . ? C19 C18 O6 C21 0.89(17) . . . . ? C13 C18 O6 C21 179.17(12) . . . . ? C20 C21 O6 C18 -0.69(18) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.434 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.060 #===END data_19 _database_code_depnum_ccdc_archive 'CCDC 745435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H20 Co2 O11 S' _chemical_formula_sum 'C27 H20 Co2 O11 S' _chemical_formula_weight 670.35 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6480(5) _cell_length_b 12.0683(7) _cell_length_c 14.2184(9) _cell_angle_alpha 107.2871(9) _cell_angle_beta 93.7267(9) _cell_angle_gamma 91.7003(9) _cell_volume 1412.03(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6351 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 30.44 _exptl_crystal_description shard _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.848 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17036 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.55 _reflns_number_total 8495 _reflns_number_gt 7011 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0420P)^2^+0.3069P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 8495 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.16466(2) 0.234436(18) 0.118997(16) 0.02303(6) Uani 1 1 d . . . Co2 Co 0.41626(2) 0.345909(18) 0.142359(15) 0.02164(6) Uani 1 1 d . . . C1 C 0.41163(17) 0.16957(12) 0.26733(11) 0.0200(3) Uani 1 1 d . . . C2 C 0.5085(2) 0.08543(14) 0.21633(13) 0.0278(3) Uani 1 1 d . . . H2 H 0.5235 0.0772 0.1490 0.033 Uiso 1 1 calc R . . C3 C 0.5828(2) 0.01388(15) 0.26315(14) 0.0325(4) Uani 1 1 d . . . H3 H 0.6486 -0.0431 0.2280 0.039 Uiso 1 1 calc R . . C4 C 0.5613(2) 0.02538(16) 0.36107(14) 0.0317(4) Uani 1 1 d . . . H4 H 0.6128 -0.0233 0.3932 0.038 Uiso 1 1 calc R . . C5 C 0.4648(2) 0.10772(15) 0.41215(13) 0.0300(3) Uani 1 1 d . . . H5 H 0.4499 0.1152 0.4793 0.036 Uiso 1 1 calc R . . C6 C 0.38942(19) 0.17957(14) 0.36588(12) 0.0251(3) Uani 1 1 d . . . H6 H 0.3227 0.2356 0.4013 0.030 Uiso 1 1 calc R . . C7 C 0.33753(17) 0.24833(13) 0.21946(11) 0.0206(3) Uani 1 1 d . . . C8 C 0.26303(17) 0.34775(13) 0.23819(11) 0.0201(3) Uani 1 1 d . . . C9 C 0.20046(17) 0.43849(13) 0.31996(11) 0.0200(3) Uani 1 1 d . . . H9 H 0.1359 0.3998 0.3582 0.024 Uiso 1 1 calc R . . O1 O 0.10272(12) 0.50731(9) 0.27644(8) 0.0195(2) Uani 1 1 d . . . C10 C 0.02053(17) 0.58645(12) 0.34897(11) 0.0188(3) Uani 1 1 d . . . H10 H -0.0274 0.5423 0.3900 0.023 Uiso 1 1 calc R . . C11 C 0.13943(17) 0.68063(13) 0.41789(11) 0.0195(3) Uani 1 1 d . . . C12 C 0.25630(19) 0.61570(13) 0.46705(11) 0.0236(3) Uani 1 1 d . . . H12A H 0.3403 0.6714 0.5056 0.028 Uiso 1 1 calc R . . H12B H 0.2026 0.5837 0.5134 0.028 Uiso 1 1 calc R . . C13 C 0.32727(18) 0.51655(13) 0.39051(12) 0.0239(3) Uani 1 1 d . . . H13A H 0.3982 0.5493 0.3525 0.029 Uiso 1 1 calc R . . H13B H 0.3885 0.4700 0.4247 0.029 Uiso 1 1 calc R . . C14 C -0.10810(17) 0.62837(13) 0.29409(11) 0.0205(3) Uani 1 1 d . . . C15 C -0.12427(18) 0.61106(15) 0.19367(12) 0.0261(3) Uani 1 1 d . . . H15 H -0.0527 0.5722 0.1487 0.031 Uiso 1 1 calc R . . C16 C -0.2629(2) 0.65932(17) 0.16595(14) 0.0336(4) Uani 1 1 d . . . H16 H -0.2932 0.6563 0.0998 0.040 Uiso 1 1 calc R . . C17 C -0.34678(19) 0.70965(15) 0.24306(14) 0.0307(4) Uani 1 1 d . . . H17 H -0.4416 0.7457 0.2374 0.037 Uiso 1 1 calc R . . S1 S -0.26108(5) 0.70033(4) 0.35192(3) 0.02860(9) Uani 1 1 d . . . C18 C 0.05428(18) 0.75948(13) 0.50096(11) 0.0225(3) Uani 1 1 d . . . O2 O -0.03925(16) 0.72306(11) 0.54469(9) 0.0338(3) Uani 1 1 d . . . O3 O 0.09905(14) 0.87098(9) 0.52055(8) 0.0269(2) Uani 1 1 d . . . C19 C 0.0246(2) 0.95077(15) 0.60021(13) 0.0349(4) Uani 1 1 d . . . H19A H -0.0880 0.9435 0.5847 0.052 Uiso 1 1 calc R . . H19B H 0.0623 1.0306 0.6078 0.052 Uiso 1 1 calc R . . H19C H 0.0492 0.9321 0.6619 0.052 Uiso 1 1 calc R . . C20 C 0.22509(18) 0.74970(13) 0.36085(11) 0.0212(3) Uani 1 1 d . . . O4 O 0.36367(13) 0.76081(11) 0.36274(9) 0.0307(3) Uani 1 1 d . . . O5 O 0.12680(13) 0.79480(10) 0.30762(9) 0.0255(2) Uani 1 1 d . . . C22 C 0.1955(2) 0.85074(16) 0.24223(13) 0.0318(4) Uani 1 1 d . . . H22A H 0.2617 0.9181 0.2813 0.048 Uiso 1 1 calc R . . H22B H 0.1132 0.8764 0.2040 0.048 Uiso 1 1 calc R . . H22C H 0.2581 0.7956 0.1971 0.048 Uiso 1 1 calc R . . C23 C 0.0562(2) 0.31838(17) 0.05260(13) 0.0324(4) Uani 1 1 d . . . O23 O -0.01282(19) 0.37067(15) 0.01249(12) 0.0515(4) Uani 1 1 d . . . C24 C 0.0033(2) 0.19288(18) 0.17604(14) 0.0363(4) Uani 1 1 d . . . O24 O -0.10024(19) 0.17162(18) 0.21355(13) 0.0619(5) Uani 1 1 d . . . C25 C 0.2060(2) 0.09870(19) 0.02972(17) 0.0465(5) Uani 1 1 d . . . O25 O 0.2355(2) 0.01209(17) -0.02219(17) 0.0857(7) Uani 1 1 d . . . C26 C 0.3652(2) 0.47921(15) 0.11388(13) 0.0296(3) Uani 1 1 d . . . O26 O 0.33059(18) 0.56177(12) 0.09795(12) 0.0451(4) Uani 1 1 d . . . C27 C 0.5929(2) 0.38544(15) 0.22150(14) 0.0311(4) Uani 1 1 d . . . O27 O 0.70039(17) 0.40095(13) 0.27442(13) 0.0490(4) Uani 1 1 d . . . C28 C 0.4991(2) 0.25532(16) 0.03364(14) 0.0332(4) Uani 1 1 d . . . O28 O 0.5497(2) 0.19772(14) -0.03455(12) 0.0554(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02365(11) 0.02093(11) 0.02246(11) 0.00371(8) -0.00024(8) 0.00205(8) Co2 0.02399(11) 0.01940(10) 0.02277(11) 0.00743(8) 0.00448(8) 0.00349(8) C1 0.0204(7) 0.0156(6) 0.0236(7) 0.0055(5) 0.0010(5) 0.0001(5) C2 0.0330(8) 0.0242(8) 0.0303(8) 0.0121(7) 0.0099(7) 0.0093(6) C3 0.0319(9) 0.0258(8) 0.0453(10) 0.0164(8) 0.0107(8) 0.0115(7) C4 0.0299(8) 0.0298(8) 0.0404(10) 0.0195(8) -0.0023(7) 0.0014(7) C5 0.0367(9) 0.0293(8) 0.0261(8) 0.0124(7) -0.0001(7) -0.0016(7) C6 0.0288(8) 0.0218(7) 0.0240(7) 0.0055(6) 0.0042(6) 0.0015(6) C7 0.0222(7) 0.0165(6) 0.0219(7) 0.0041(5) 0.0016(6) 0.0010(5) C8 0.0202(7) 0.0183(7) 0.0217(7) 0.0059(5) 0.0020(5) 0.0009(5) C9 0.0231(7) 0.0175(6) 0.0204(7) 0.0067(5) 0.0023(5) 0.0048(5) O1 0.0211(5) 0.0182(5) 0.0193(5) 0.0048(4) 0.0034(4) 0.0068(4) C10 0.0199(6) 0.0179(6) 0.0194(6) 0.0055(5) 0.0060(5) 0.0036(5) C11 0.0222(7) 0.0178(6) 0.0188(6) 0.0048(5) 0.0052(5) 0.0048(5) C12 0.0286(8) 0.0208(7) 0.0197(7) 0.0035(6) 0.0001(6) 0.0046(6) C13 0.0248(7) 0.0206(7) 0.0247(7) 0.0044(6) -0.0011(6) 0.0064(6) C14 0.0169(6) 0.0192(7) 0.0257(7) 0.0064(6) 0.0056(5) 0.0034(5) C15 0.0220(7) 0.0312(8) 0.0268(8) 0.0105(7) 0.0023(6) 0.0090(6) C16 0.0297(9) 0.0418(10) 0.0303(9) 0.0123(8) 0.0005(7) 0.0104(7) C17 0.0228(8) 0.0320(9) 0.0387(9) 0.0120(7) 0.0023(7) 0.0090(6) S1 0.02480(19) 0.0300(2) 0.0315(2) 0.00773(17) 0.00952(16) 0.00948(16) C18 0.0268(7) 0.0219(7) 0.0189(7) 0.0054(6) 0.0039(6) 0.0059(6) O2 0.0423(7) 0.0305(6) 0.0296(6) 0.0072(5) 0.0181(5) 0.0030(5) O3 0.0352(6) 0.0188(5) 0.0253(6) 0.0022(4) 0.0099(5) 0.0070(5) C19 0.0484(11) 0.0256(8) 0.0286(9) 0.0017(7) 0.0139(8) 0.0145(8) C20 0.0247(7) 0.0174(7) 0.0197(7) 0.0015(5) 0.0063(6) 0.0038(5) O4 0.0221(5) 0.0361(7) 0.0363(7) 0.0129(5) 0.0084(5) 0.0029(5) O5 0.0258(5) 0.0261(6) 0.0289(6) 0.0143(5) 0.0058(5) 0.0006(4) C22 0.0386(9) 0.0315(9) 0.0309(9) 0.0163(7) 0.0101(7) 0.0001(7) C23 0.0312(9) 0.0383(10) 0.0280(8) 0.0107(7) 0.0004(7) 0.0013(7) O23 0.0547(9) 0.0616(10) 0.0459(9) 0.0286(8) -0.0039(7) 0.0142(8) C24 0.0351(9) 0.0416(10) 0.0332(9) 0.0158(8) -0.0075(8) -0.0079(8) O24 0.0445(9) 0.0941(14) 0.0542(10) 0.0370(10) -0.0020(8) -0.0252(9) C25 0.0375(11) 0.0395(11) 0.0475(12) -0.0083(9) -0.0046(9) 0.0014(9) O25 0.0725(13) 0.0544(11) 0.0917(15) -0.0372(11) 0.0038(11) 0.0088(10) C26 0.0321(9) 0.0270(8) 0.0307(8) 0.0107(7) 0.0012(7) 0.0014(7) O26 0.0518(9) 0.0321(7) 0.0573(9) 0.0241(7) -0.0053(7) 0.0043(6) C27 0.0301(8) 0.0259(8) 0.0408(10) 0.0153(7) 0.0030(7) -0.0020(7) O27 0.0375(8) 0.0436(8) 0.0682(11) 0.0257(8) -0.0168(7) -0.0093(6) C28 0.0392(10) 0.0312(9) 0.0328(9) 0.0128(7) 0.0108(8) 0.0078(7) O28 0.0729(11) 0.0496(9) 0.0438(9) 0.0075(7) 0.0283(8) 0.0198(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C24 1.790(2) . ? Co1 C25 1.811(2) . ? Co1 C23 1.8185(18) . ? Co1 C8 1.9575(15) . ? Co1 C7 1.9669(15) . ? Co1 Co2 2.4741(3) . ? Co2 C27 1.8008(19) . ? Co2 C28 1.8121(18) . ? Co2 C26 1.8312(17) . ? Co2 C8 1.9574(15) . ? Co2 C7 1.9670(15) . ? C1 C2 1.396(2) . ? C1 C6 1.397(2) . ? C1 C7 1.463(2) . ? C2 C3 1.386(2) . ? C3 C4 1.383(3) . ? C4 C5 1.382(3) . ? C5 C6 1.388(2) . ? C7 C8 1.343(2) . ? C8 C9 1.485(2) . ? C9 O1 1.4375(17) . ? C9 C13 1.527(2) . ? O1 C10 1.4252(16) . ? C10 C14 1.503(2) . ? C10 C11 1.564(2) . ? C11 C18 1.526(2) . ? C11 C20 1.531(2) . ? C11 C12 1.551(2) . ? C12 C13 1.533(2) . ? C14 C15 1.377(2) . ? C14 S1 1.7221(15) . ? C15 C16 1.431(2) . ? C16 C17 1.353(2) . ? C17 S1 1.7079(18) . ? C18 O2 1.200(2) . ? C18 O3 1.3306(19) . ? O3 C19 1.4520(19) . ? C20 O4 1.1997(19) . ? C20 O5 1.3342(19) . ? O5 C22 1.4472(19) . ? C23 O23 1.128(2) . ? C24 O24 1.132(2) . ? C25 O25 1.133(3) . ? C26 O26 1.130(2) . ? C27 O27 1.131(2) . ? C28 O28 1.135(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Co1 C25 102.43(10) . . ? C24 Co1 C23 96.31(8) . . ? C25 Co1 C23 107.41(10) . . ? C24 Co1 C8 96.51(8) . . ? C25 Co1 C8 139.32(8) . . ? C23 Co1 C8 105.83(7) . . ? C24 Co1 C7 102.46(7) . . ? C25 Co1 C7 100.25(8) . . ? C23 Co1 C7 142.18(7) . . ? C8 Co1 C7 40.03(6) . . ? C24 Co1 Co2 146.97(6) . . ? C25 Co1 Co2 101.79(7) . . ? C23 Co1 Co2 97.51(6) . . ? C8 Co1 Co2 50.80(4) . . ? C7 Co1 Co2 51.03(4) . . ? C27 Co2 C28 97.77(9) . . ? C27 Co2 C26 104.72(8) . . ? C28 Co2 C26 106.02(8) . . ? C27 Co2 C8 101.49(7) . . ? C28 Co2 C8 143.93(8) . . ? C26 Co2 C8 98.20(7) . . ? C27 Co2 C7 92.04(7) . . ? C28 Co2 C7 109.61(7) . . ? C26 Co2 C7 137.91(7) . . ? C8 Co2 C7 40.03(6) . . ? C27 Co2 Co1 143.03(6) . . ? C28 Co2 Co1 96.99(6) . . ? C26 Co2 Co1 103.43(6) . . ? C8 Co2 Co1 50.81(4) . . ? C7 Co2 Co1 51.03(4) . . ? C2 C1 C6 118.97(14) . . ? C2 C1 C7 120.75(14) . . ? C6 C1 C7 120.25(14) . . ? C3 C2 C1 120.50(16) . . ? C4 C3 C2 120.03(16) . . ? C5 C4 C3 120.03(16) . . ? C4 C5 C6 120.39(16) . . ? C5 C6 C1 120.07(15) . . ? C8 C7 C1 142.69(14) . . ? C8 C7 Co1 69.61(9) . . ? C1 C7 Co1 135.53(11) . . ? C8 C7 Co2 69.60(9) . . ? C1 C7 Co2 133.04(11) . . ? Co1 C7 Co2 77.94(6) . . ? C7 C8 C9 141.90(14) . . ? C7 C8 Co2 70.37(9) . . ? C9 C8 Co2 135.31(11) . . ? C7 C8 Co1 70.36(9) . . ? C9 C8 Co1 132.77(11) . . ? Co2 C8 Co1 78.39(6) . . ? O1 C9 C8 107.59(12) . . ? O1 C9 C13 109.81(12) . . ? C8 C9 C13 112.97(12) . . ? C10 O1 C9 111.36(11) . . ? O1 C10 C14 106.72(11) . . ? O1 C10 C11 108.57(11) . . ? C14 C10 C11 117.13(12) . . ? C18 C11 C20 111.91(12) . . ? C18 C11 C12 106.61(12) . . ? C20 C11 C12 110.24(12) . . ? C18 C11 C10 108.80(12) . . ? C20 C11 C10 112.13(12) . . ? C12 C11 C10 106.87(12) . . ? C13 C12 C11 111.88(12) . . ? C9 C13 C12 110.65(13) . . ? C15 C14 C10 125.96(13) . . ? C15 C14 S1 111.54(11) . . ? C10 C14 S1 122.44(11) . . ? C14 C15 C16 111.16(15) . . ? C17 C16 C15 113.54(16) . . ? C16 C17 S1 111.66(13) . . ? C17 S1 C14 92.09(8) . . ? O2 C18 O3 124.62(14) . . ? O2 C18 C11 122.91(14) . . ? O3 C18 C11 112.44(13) . . ? C18 O3 C19 115.35(13) . . ? O4 C20 O5 124.03(15) . . ? O4 C20 C11 124.21(15) . . ? O5 C20 C11 111.75(13) . . ? C20 O5 C22 116.23(13) . . ? O23 C23 Co1 178.88(17) . . ? O24 C24 Co1 177.0(2) . . ? O25 C25 Co1 176.4(2) . . ? O26 C26 Co2 178.18(17) . . ? O27 C27 Co2 173.07(16) . . ? O28 C28 Co2 179.26(19) . . ? 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 C24 Co1 Co2 C27 39.38(16) . . . . ? C25 Co1 Co2 C27 -97.02(13) . . . . ? C23 Co1 Co2 C27 153.36(11) . . . . ? C8 Co1 Co2 C27 49.03(11) . . . . ? C7 Co1 Co2 C27 -3.29(11) . . . . ? C24 Co1 Co2 C28 152.29(13) . . . . ? C25 Co1 Co2 C28 15.89(10) . . . . ? C23 Co1 Co2 C28 -93.73(8) . . . . ? C8 Co1 Co2 C28 161.94(8) . . . . ? C7 Co1 Co2 C28 109.62(8) . . . . ? C24 Co1 Co2 C26 -99.33(13) . . . . ? C25 Co1 Co2 C26 124.26(10) . . . . ? C23 Co1 Co2 C26 14.64(8) . . . . ? C8 Co1 Co2 C26 -89.69(8) . . . . ? C7 Co1 Co2 C26 -142.01(8) . . . . ? C24 Co1 Co2 C8 -9.65(13) . . . . ? C25 Co1 Co2 C8 -146.05(10) . . . . ? C23 Co1 Co2 C8 104.33(8) . . . . ? C7 Co1 Co2 C8 -52.32(8) . . . . ? C24 Co1 Co2 C7 42.68(13) . . . . ? C25 Co1 Co2 C7 -93.73(10) . . . . ? C23 Co1 Co2 C7 156.65(8) . . . . ? C8 Co1 Co2 C7 52.32(8) . . . . ? C6 C1 C2 C3 -0.8(3) . . . . ? C7 C1 C2 C3 177.64(16) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -0.5(3) . . . . ? C2 C1 C6 C5 0.9(2) . . . . ? C7 C1 C6 C5 -177.46(15) . . . . ? C2 C1 C7 C8 -164.9(2) . . . . ? C6 C1 C7 C8 13.4(3) . . . . ? C2 C1 C7 Co1 74.0(2) . . . . ? C6 C1 C7 Co1 -107.62(17) . . . . ? C2 C1 C7 Co2 -48.9(2) . . . . ? C6 C1 C7 Co2 129.47(15) . . . . ? C24 Co1 C7 C8 -85.27(11) . . . . ? C25 Co1 C7 C8 169.43(12) . . . . ? C23 Co1 C7 C8 32.64(16) . . . . ? Co2 Co1 C7 C8 72.49(9) . . . . ? C24 Co1 C7 C1 61.10(17) . . . . ? C25 Co1 C7 C1 -44.21(18) . . . . ? C23 Co1 C7 C1 179.01(14) . . . . ? C8 Co1 C7 C1 146.4(2) . . . . ? Co2 Co1 C7 C1 -141.14(18) . . . . ? C24 Co1 C7 Co2 -157.77(7) . . . . ? C25 Co1 C7 Co2 96.93(9) . . . . ? C23 Co1 C7 Co2 -39.85(13) . . . . ? C8 Co1 C7 Co2 -72.49(9) . . . . ? C27 Co2 C7 C8 105.52(10) . . . . ? C28 Co2 C7 C8 -155.49(10) . . . . ? C26 Co2 C7 C8 -9.24(14) . . . . ? Co1 Co2 C7 C8 -72.50(9) . . . . ? C27 Co2 C7 C1 -38.96(16) . . . . ? C28 Co2 C7 C1 60.04(16) . . . . ? C26 Co2 C7 C1 -153.71(14) . . . . ? C8 Co2 C7 C1 -144.47(19) . . . . ? Co1 Co2 C7 C1 143.03(17) . . . . ? C27 Co2 C7 Co1 178.02(7) . . . . ? C28 Co2 C7 Co1 -82.99(8) . . . . ? C26 Co2 C7 Co1 63.26(11) . . . . ? C8 Co2 C7 Co1 72.50(9) . . . . ? C1 C7 C8 C9 -4.7(4) . . . . ? Co1 C7 C8 C9 135.5(2) . . . . ? Co2 C7 C8 C9 -140.2(2) . . . . ? C1 C7 C8 Co2 135.5(2) . . . . ? Co1 C7 C8 Co2 -84.28(5) . . . . ? C1 C7 C8 Co1 -140.2(2) . . . . ? Co2 C7 C8 Co1 84.28(5) . . . . ? C27 Co2 C8 C7 -79.31(10) . . . . ? C28 Co2 C8 C7 41.58(16) . . . . ? C26 Co2 C8 C7 173.76(10) . . . . ? Co1 Co2 C8 C7 73.08(9) . . . . ? C27 Co2 C8 C9 66.53(16) . . . . ? C28 Co2 C8 C9 -172.58(14) . . . . ? C26 Co2 C8 C9 -40.41(16) . . . . ? C7 Co2 C8 C9 145.8(2) . . . . ? Co1 Co2 C8 C9 -141.08(17) . . . . ? C27 Co2 C8 Co1 -152.39(6) . . . . ? C28 Co2 C8 Co1 -31.51(14) . . . . ? C26 Co2 C8 Co1 100.67(7) . . . . ? C7 Co2 C8 Co1 -73.08(9) . . . . ? C24 Co1 C8 C7 101.63(11) . . . . ? C25 Co1 C8 C7 -16.08(18) . . . . ? C23 Co1 C8 C7 -159.89(10) . . . . ? Co2 Co1 C8 C7 -73.09(9) . . . . ? C24 Co1 C8 C9 -42.28(16) . . . . ? C25 Co1 C8 C9 -159.99(17) . . . . ? C23 Co1 C8 C9 56.20(16) . . . . ? C7 Co1 C8 C9 -143.91(19) . . . . ? Co2 Co1 C8 C9 143.00(17) . . . . ? C24 Co1 C8 Co2 174.73(7) . . . . ? C25 Co1 C8 Co2 57.01(15) . . . . ? C23 Co1 C8 Co2 -86.80(7) . . . . ? C7 Co1 C8 Co2 73.09(9) . . . . ? C7 C8 C9 O1 -167.11(19) . . . . ? Co2 C8 C9 O1 71.89(18) . . . . ? Co1 C8 C9 O1 -51.15(18) . . . . ? C7 C8 C9 C13 71.5(3) . . . . ? Co2 C8 C9 C13 -49.5(2) . . . . ? Co1 C8 C9 C13 -172.52(11) . . . . ? C8 C9 O1 C10 171.88(12) . . . . ? C13 C9 O1 C10 -64.80(15) . . . . ? C9 O1 C10 C14 -164.37(11) . . . . ? C9 O1 C10 C11 68.53(14) . . . . ? O1 C10 C11 C18 -175.20(11) . . . . ? C14 C10 C11 C18 63.92(16) . . . . ? O1 C10 C11 C20 60.46(15) . . . . ? C14 C10 C11 C20 -60.41(16) . . . . ? O1 C10 C11 C12 -60.45(14) . . . . ? C14 C10 C11 C12 178.68(12) . . . . ? C18 C11 C12 C13 168.95(13) . . . . ? C20 C11 C12 C13 -69.38(16) . . . . ? C10 C11 C12 C13 52.73(16) . . . . ? O1 C9 C13 C12 54.22(16) . . . . ? C8 C9 C13 C12 174.32(13) . . . . ? C11 C12 C13 C9 -50.70(17) . . . . ? O1 C10 C14 C15 -11.3(2) . . . . ? C11 C10 C14 C15 110.55(17) . . . . ? O1 C10 C14 S1 165.65(10) . . . . ? C11 C10 C14 S1 -72.50(16) . . . . ? C10 C14 C15 C16 178.02(15) . . . . ? S1 C14 C15 C16 0.80(19) . . . . ? C14 C15 C16 C17 -0.5(2) . . . . ? C15 C16 C17 S1 -0.1(2) . . . . ? C16 C17 S1 C14 0.44(15) . . . . ? C15 C14 S1 C17 -0.72(13) . . . . ? C10 C14 S1 C17 -178.06(13) . . . . ? C20 C11 C18 O2 167.97(15) . . . . ? C12 C11 C18 O2 -71.43(19) . . . . ? C10 C11 C18 O2 43.5(2) . . . . ? C20 C11 C18 O3 -13.90(18) . . . . ? C12 C11 C18 O3 106.70(14) . . . . ? C10 C11 C18 O3 -138.37(13) . . . . ? O2 C18 O3 C19 -0.8(2) . . . . ? C11 C18 O3 C19 -178.93(13) . . . . ? C18 C11 C20 O4 111.52(17) . . . . ? C12 C11 C20 O4 -6.9(2) . . . . ? C10 C11 C20 O4 -125.89(16) . . . . ? C18 C11 C20 O5 -69.34(16) . . . . ? C12 C11 C20 O5 172.20(12) . . . . ? C10 C11 C20 O5 53.25(16) . . . . ? O4 C20 O5 C22 5.9(2) . . . . ? C11 C20 O5 C22 -173.29(13) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.486 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.064 #===END