Supplementary Information (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_GLOBAL _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Rolf Gleiter' _publ_contact_author_address ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8400' _publ_contact_author_fax '049 6221 54- 4205' _publ_contact_author_email 'rolf.gleiter@urz.uni-heidelberg.de' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; paper submitted for publication in J. Chem. Soc., Dalton Trans. ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Syntheses and structural properties of bis(hexacarbonyldicobalt) complexes from cyclic diynes ; loop_ _publ_author_name _publ_author_address 'Rausch, Bernhard, J.' ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Gleiter, Rolf' ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #======================================================================== data_ramm6_7 _database_code_CSD 168766 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H16 Co4 O12' _chemical_formula_weight 828.17 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.044(7) _cell_length_b 16.345(9) _cell_length_c 16.476(7) _cell_angle_alpha 75.02(4) _cell_angle_beta 70.57(3) _cell_angle_gamma 72.45(4) _cell_volume 3348(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max .50 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 2.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; Comment on the bad Rint (43.6%): The calculation of Rint is based on only 154 out of 11958 reflections. All of these 154 reflections are very weak, not one of it is listed in the "inconsistent equivalents" list of SHELXL. Thus the given number is almost meaningless. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11958 _diffrn_reflns_av_R_equivalents 0.4360 _diffrn_reflns_av_sigmaI/netI 0.1385 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11804 _reflns_number_gt 5838 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+10.2570P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11804 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1960 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.362 _refine_ls_shift/su_mean 0.019 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 0.08173(11) 0.58343(10) 0.60652(10) 0.0544(4) Uani 1 1 d . . . Co2 Co -0.04174(11) 0.50895(10) 0.72369(10) 0.0631(5) Uani 1 1 d . . . Co3 Co 0.42071(12) 0.41979(9) 0.86067(9) 0.0527(4) Uani 1 1 d . . . Co4 Co 0.53561(11) 0.51786(10) 0.77276(10) 0.0571(4) Uani 1 1 d . . . C1 C -0.0103(9) 0.6673(8) 0.5592(7) 0.060(3) Uani 1 1 d . . . O1 O -0.0706(7) 0.7203(6) 0.5285(6) 0.092(3) Uani 1 1 d . . . C2 C 0.1882(9) 0.6361(8) 0.5658(7) 0.063(3) Uani 1 1 d . . . O2 O 0.2559(7) 0.6680(6) 0.5388(5) 0.085(3) Uani 1 1 d . . . C3 C 0.1325(9) 0.5029(8) 0.5347(8) 0.070(3) Uani 1 1 d . . . O3 O 0.1621(8) 0.4546(7) 0.4891(6) 0.123(4) Uani 1 1 d . . . C4 C -0.0207(10) 0.4138(10) 0.6816(10) 0.092(5) Uani 1 1 d . . . O4 O -0.0036(9) 0.3521(7) 0.6526(8) 0.137(4) Uani 1 1 d . . . C5 C -0.1617(10) 0.5791(9) 0.7027(8) 0.076(4) Uani 1 1 d . . . O5 O -0.2340(7) 0.6261(7) 0.6875(7) 0.121(4) Uani 1 1 d . . . C6 C -0.0819(10) 0.4667(10) 0.8357(10) 0.088(4) Uani 1 1 d . . . O6 O -0.1009(9) 0.4427(8) 0.9092(7) 0.128(4) Uani 1 1 d . . . C7 C 0.4599(8) 0.3289(7) 0.8022(8) 0.058(3) Uani 1 1 d . . . O7 O 0.4814(7) 0.2702(5) 0.7704(5) 0.083(3) Uani 1 1 d . . . C8 C 0.2974(11) 0.4127(7) 0.9286(8) 0.071(4) Uani 1 1 d . . . O8 O 0.2148(8) 0.4112(6) 0.9730(6) 0.108(4) Uani 1 1 d . . . C9 C 0.4892(11) 0.3796(8) 0.9429(8) 0.077(4) Uani 1 1 d . . . O9 O 0.5339(9) 0.3531(6) 0.9941(7) 0.123(4) Uani 1 1 d . . . C10 C 0.6056(11) 0.5169(9) 0.8479(9) 0.084(4) Uani 1 1 d . . . O10 O 0.6488(7) 0.5157(7) 0.8960(6) 0.119(4) Uani 1 1 d . . . C11 C 0.5423(10) 0.6201(10) 0.7044(10) 0.088(4) Uani 1 1 d . . . O11 O 0.5429(8) 0.6876(7) 0.6638(8) 0.127(4) Uani 1 1 d . . . C12 C 0.6263(10) 0.4486(9) 0.6997(9) 0.085(4) Uani 1 1 d . . . O12 O 0.6833(8) 0.4058(7) 0.6506(7) 0.122(4) Uani 1 1 d . . . C13 C 0.2777(8) 0.4148(7) 0.6857(7) 0.050(3) Uani 1 1 d . . . C14 C 0.3597(8) 0.4560(6) 0.6544(6) 0.043(2) Uani 1 1 d . . . C15 C 0.4461(8) 0.4229(7) 0.5920(6) 0.053(3) Uani 1 1 d . . . H15 H 0.5011 0.4502 0.5701 0.080 Uiso 1 1 calc R . . C16 C 0.4530(11) 0.3494(9) 0.5608(8) 0.079(4) Uani 1 1 d . . . H16 H 0.5134 0.3265 0.5204 0.080 Uiso 1 1 calc R . . C17 C 0.3723(12) 0.3113(9) 0.5891(9) 0.083(4) Uani 1 1 d . . . H17 H 0.3751 0.2641 0.5661 0.080 Uiso 1 1 calc R . . C18 C 0.2870(10) 0.3425(7) 0.6515(8) 0.070(3) Uani 1 1 d . . . H18 H 0.2326 0.3145 0.6722 0.080 Uiso 1 1 calc R . . C19 C 0.2391(8) 0.6760(6) 0.8302(7) 0.050(3) Uani 1 1 d . . . C20 C 0.2616(9) 0.7491(7) 0.7688(8) 0.065(3) Uani 1 1 d . . . H20 H 0.3197 0.7679 0.7642 0.080 Uiso 1 1 calc R . . C21 C 0.1996(10) 0.7934(7) 0.7154(8) 0.071(3) Uani 1 1 d . . . H21 H 0.2158 0.8419 0.6746 0.080 Uiso 1 1 calc R . . C22 C 0.1136(9) 0.7668(7) 0.7216(8) 0.069(3) Uani 1 1 d . . . H22 H 0.0717 0.7975 0.6850 0.080 Uiso 1 1 calc R . . C23 C 0.0884(7) 0.6946(6) 0.7819(7) 0.046(3) Uani 1 1 d . . . C24 C 0.1526(7) 0.6514(6) 0.8356(6) 0.045(3) Uani 1 1 d . . . H24 H 0.1358 0.6035 0.8773 0.080 Uiso 1 1 calc R . . C25 C 0.1820(8) 0.4481(7) 0.7542(7) 0.061(3) Uani 1 1 d . . . H25A H 0.1544 0.3989 0.7908 0.080 Uiso 1 1 calc R . . H25B H 0.2015 0.4743 0.7910 0.080 Uiso 1 1 calc R . . C26 C 0.0981(7) 0.5130(7) 0.7202(6) 0.044(3) Uani 1 1 d . . . C27 C 0.0312(7) 0.5908(7) 0.7319(6) 0.046(3) Uani 1 1 d . . . C28 C -0.0017(8) 0.6614(7) 0.7851(7) 0.064(3) Uani 1 1 d . . . H28A H -0.0346 0.6391 0.8453 0.080 Uiso 1 1 calc R . . H28B H -0.0526 0.7093 0.7632 0.080 Uiso 1 1 calc R . . C29 C 0.3154(8) 0.6197(6) 0.8812(6) 0.052(3) Uani 1 1 d . . . H29A H 0.3559 0.6550 0.8879 0.080 Uiso 1 1 calc R . . H29B H 0.2778 0.5953 0.9390 0.080 Uiso 1 1 calc R . . C30 C 0.3867(7) 0.5472(6) 0.8330(7) 0.048(3) Uani 1 1 d . . . C31 C 0.4006(7) 0.5164(6) 0.7636(6) 0.046(3) Uani 1 1 d . . . C32 C 0.3575(8) 0.5345(6) 0.6871(6) 0.049(3) Uani 1 1 d . . . H32A H 0.3962 0.5711 0.6392 0.080 Uiso 1 1 calc R . . H32B H 0.2860 0.5677 0.7032 0.080 Uiso 1 1 calc R . . Co5 Co 0.81390(11) 1.12131(9) 0.88884(9) 0.0524(4) Uani 1 1 d . . . Co6 Co 0.99491(11) 1.07721(10) 0.80239(10) 0.0618(5) Uani 1 1 d . . . Co7 Co 0.64399(12) 0.89521(10) 0.68502(10) 0.0591(4) Uani 1 1 d . . . Co8 Co 0.46232(12) 0.97313(11) 0.74024(10) 0.0607(5) Uani 1 1 d . . . C41 C 0.6805(10) 1.1547(6) 0.9008(7) 0.050(3) Uani 1 1 d . . . O41 O 0.5918(7) 1.1776(6) 0.9111(6) 0.089(3) Uani 1 1 d . . . C42 C 0.8122(10) 1.0371(9) 0.9823(9) 0.078(4) Uani 1 1 d . . . O42 O 0.8086(8) 0.9819(7) 1.0436(6) 0.113(4) Uani 1 1 d . . . C43 C 0.8226(10) 1.2160(9) 0.9205(10) 0.096(5) Uani 1 1 d . . . O43 O 0.8269(9) 1.2742(8) 0.9420(9) 0.165(6) Uani 1 1 d . . . C44 C 1.0380(10) 0.9770(9) 0.8713(11) 0.096(5) Uani 1 1 d . . . O44 O 1.0655(9) 0.9100(7) 0.9097(8) 0.137(5) Uani 1 1 d . . . C45 C 1.0819(9) 1.0632(9) 0.7022(10) 0.090(4) Uani 1 1 d . . . O45 O 1.1373(8) 1.0579(9) 0.6312(7) 0.154(5) Uani 1 1 d . . . C46 C 1.0418(9) 1.1588(9) 0.8233(9) 0.080(4) Uani 1 1 d . . . O46 O 1.0708(7) 1.2119(7) 0.8343(7) 0.121(4) Uani 1 1 d . . . C47 C 0.7813(10) 0.8834(7) 0.6493(8) 0.067(4) Uani 1 1 d . . . O47 O 0.8694(7) 0.8723(6) 0.6267(6) 0.096(3) Uani 1 1 d . . . C48 C 0.6450(11) 0.7991(9) 0.7687(9) 0.092(5) Uani 1 1 d . . . O48 O 0.6437(11) 0.7416(6) 0.8251(7) 0.151(5) Uani 1 1 d . . . C49 C 0.6306(11) 0.8670(9) 0.5914(9) 0.094(5) Uani 1 1 d . . . O49 O 0.6269(9) 0.8513(7) 0.5297(7) 0.137(4) Uani 1 1 d . . . C50 C 0.3751(11) 1.0698(10) 0.7729(9) 0.088(4) Uani 1 1 d . . . O50 O 0.3229(8) 1.1360(7) 0.7924(8) 0.131(4) Uani 1 1 d . . . C51 C 0.4200(10) 0.8937(9) 0.8344(9) 0.078(4) Uani 1 1 d . . . O51 O 0.3931(8) 0.8425(7) 0.8912(6) 0.116(4) Uani 1 1 d . . . C52 C 0.4111(11) 0.9607(10) 0.6603(9) 0.102(5) Uani 1 1 d . . . O52 O 0.3781(9) 0.9579(9) 0.6066(7) 0.151(5) Uani 1 1 d . . . C53 C 0.7869(9) 0.9231(6) 0.8509(6) 0.051(3) Uani 1 1 d . . . C54 C 0.6784(9) 0.9426(7) 0.8751(7) 0.055(3) Uani 1 1 d . . . C55 C 0.6305(11) 0.8926(8) 0.9482(8) 0.082(4) Uani 1 1 d . . . H55 H 0.5583 0.9045 0.9660 0.080 Uiso 1 1 calc R . . C56 C 0.6850(15) 0.8259(9) 0.9960(9) 0.100(5) Uani 1 1 d . . . H56 H 0.6499 0.7939 1.0464 0.080 Uiso 1 1 calc R . . C57 C 0.7912(14) 0.8055(9) 0.9705(9) 0.095(5) Uani 1 1 d . . . H57 H 0.8282 0.7581 1.0019 0.080 Uiso 1 1 calc R . . C58 C 0.8425(11) 0.8543(7) 0.8993(9) 0.079(4) Uani 1 1 d . . . H58 H 0.9147 0.8419 0.8829 0.080 Uiso 1 1 calc R . . C59 C 0.7058(8) 1.1149(6) 0.5814(6) 0.045(3) Uani 1 1 d . . . C60 C 0.7837(8) 1.0820(7) 0.5152(6) 0.056(3) Uani 1 1 d . . . H60 H 0.7703 1.0544 0.4788 0.080 Uiso 1 1 calc R . . C61 C 0.8835(9) 1.0897(8) 0.5018(6) 0.063(3) Uani 1 1 d . . . H61 H 0.9377 1.0660 0.4573 0.080 Uiso 1 1 calc R . . C62 C 0.9022(9) 1.1330(7) 0.5553(7) 0.061(3) Uani 1 1 d . . . H62 H 0.9691 1.1394 0.5451 0.080 Uiso 1 1 calc R . . C63 C 0.8242(8) 1.1665(6) 0.6226(6) 0.049(3) Uani 1 1 d . . . C64 C 0.7239(8) 1.1597(6) 0.6337(6) 0.046(3) Uani 1 1 d . . . H64 H 0.6687 1.1853 0.6764 0.080 Uiso 1 1 calc R . . C65 C 0.8469(8) 0.9773(6) 0.7734(6) 0.050(3) Uani 1 1 d . . . H65A H 0.8089 0.9978 0.7297 0.080 Uiso 1 1 calc R . . H65B H 0.9131 0.9399 0.7483 0.080 Uiso 1 1 calc R . . C66 C 0.8679(7) 1.0560(7) 0.7922(6) 0.048(3) Uani 1 1 d . . . C67 C 0.8708(8) 1.1374(7) 0.7616(7) 0.050(3) Uani 1 1 d . . . C68 C 0.8473(9) 1.2050(7) 0.6844(7) 0.065(3) Uani 1 1 d . . . H68A H 0.7882 1.2511 0.7051 0.080 Uiso 1 1 calc R . . H68B H 0.9065 1.2306 0.6539 0.080 Uiso 1 1 calc R . . C69 C 0.5951(8) 1.1011(7) 0.6033(7) 0.057(3) Uani 1 1 d . . . H69A H 0.5442 1.1520 0.6235 0.080 Uiso 1 1 calc R . . H69B H 0.5834 1.0937 0.5511 0.080 Uiso 1 1 calc R . . C70 C 0.5824(7) 1.0217(7) 0.6731(7) 0.050(3) Uani 1 1 d . . . C71 C 0.5902(7) 0.9893(6) 0.7518(6) 0.043(2) Uani 1 1 d . . . C72 C 0.6144(8) 1.0144(7) 0.8244(6) 0.053(3) Uani 1 1 d . . . H72A H 0.6505 1.0610 0.7987 0.080 Uiso 1 1 calc R . . H72B H 0.5491 1.0374 0.8649 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0534(10) 0.0592(10) 0.0568(10) -0.0159(8) -0.0160(8) -0.0163(8) Co2 0.0523(10) 0.0768(12) 0.0709(12) -0.0228(9) -0.0077(8) -0.0325(9) Co3 0.0683(11) 0.0444(9) 0.0454(9) -0.0047(7) -0.0208(8) -0.0102(8) Co4 0.0516(10) 0.0627(10) 0.0617(10) -0.0107(8) -0.0204(8) -0.0153(8) C1 0.060(8) 0.072(9) 0.059(8) -0.017(7) -0.017(6) -0.024(7) O1 0.084(7) 0.081(7) 0.117(8) -0.009(6) -0.052(6) -0.010(5) C2 0.062(8) 0.063(8) 0.059(8) 0.005(6) -0.026(7) -0.010(7) O2 0.081(7) 0.106(7) 0.076(6) 0.014(5) -0.031(5) -0.050(6) C3 0.079(9) 0.087(10) 0.051(8) -0.015(7) -0.018(7) -0.027(8) O3 0.154(10) 0.124(9) 0.100(8) -0.079(7) -0.028(7) -0.006(7) C4 0.078(10) 0.111(13) 0.103(12) -0.032(10) -0.006(8) -0.053(9) O4 0.173(11) 0.116(9) 0.147(10) -0.063(8) -0.022(8) -0.063(8) C5 0.054(8) 0.103(11) 0.074(9) -0.020(8) -0.009(7) -0.029(8) O5 0.051(6) 0.141(10) 0.170(10) -0.040(8) -0.034(7) -0.008(6) C6 0.081(10) 0.106(12) 0.094(11) -0.039(10) -0.002(9) -0.055(9) O6 0.153(10) 0.160(11) 0.081(8) -0.020(8) -0.001(8) -0.086(8) C7 0.062(8) 0.041(7) 0.073(9) 0.000(6) -0.031(7) -0.011(6) O7 0.110(7) 0.052(5) 0.079(6) -0.022(5) -0.025(5) -0.002(5) C8 0.092(11) 0.051(8) 0.068(9) -0.003(7) -0.017(8) -0.028(8) O8 0.097(8) 0.093(7) 0.100(8) -0.009(6) 0.021(6) -0.033(6) C9 0.106(11) 0.058(8) 0.062(9) -0.009(7) -0.032(8) -0.004(7) O9 0.185(11) 0.105(8) 0.100(8) -0.002(6) -0.099(8) -0.014(7) C10 0.091(11) 0.102(11) 0.073(10) -0.006(8) -0.041(8) -0.029(8) O10 0.096(8) 0.184(11) 0.102(8) -0.034(7) -0.055(6) -0.031(7) C11 0.070(9) 0.085(11) 0.124(13) -0.013(10) -0.033(9) -0.037(9) O11 0.127(9) 0.089(8) 0.171(11) 0.015(8) -0.046(8) -0.062(7) C12 0.064(9) 0.101(12) 0.077(10) 0.002(9) -0.029(8) -0.007(8) O12 0.094(8) 0.130(10) 0.116(9) -0.038(7) -0.006(7) -0.003(7) C13 0.046(7) 0.054(7) 0.051(7) -0.011(6) -0.016(6) -0.011(6) C14 0.046(6) 0.041(6) 0.034(6) -0.005(5) -0.013(5) 0.002(5) C15 0.061(8) 0.058(7) 0.042(7) 0.001(6) -0.020(6) -0.018(6) C16 0.074(10) 0.100(11) 0.053(8) -0.038(8) -0.030(7) 0.028(8) C17 0.093(11) 0.077(10) 0.095(11) -0.043(9) -0.041(9) 0.000(9) C18 0.069(9) 0.054(8) 0.105(11) -0.023(7) -0.039(8) -0.018(7) C19 0.067(8) 0.035(6) 0.056(7) -0.017(5) -0.027(6) -0.005(6) C20 0.074(8) 0.044(7) 0.093(10) -0.015(7) -0.036(8) -0.016(6) C21 0.082(9) 0.060(8) 0.086(9) -0.005(7) -0.037(8) -0.029(7) C22 0.072(9) 0.048(7) 0.094(10) -0.002(7) -0.048(8) -0.006(6) C23 0.037(6) 0.039(6) 0.067(8) -0.026(6) -0.020(6) 0.002(5) C24 0.046(6) 0.045(6) 0.050(7) -0.016(5) -0.015(5) -0.010(5) C25 0.059(8) 0.057(7) 0.061(8) -0.004(6) -0.014(6) -0.015(6) C26 0.040(6) 0.054(7) 0.042(6) -0.015(5) -0.002(5) -0.024(5) C27 0.040(6) 0.055(7) 0.044(6) -0.008(5) 0.001(5) -0.026(5) C28 0.061(8) 0.063(8) 0.070(8) -0.032(7) -0.015(6) -0.006(6) C29 0.066(7) 0.047(6) 0.053(7) -0.009(5) -0.031(6) -0.015(6) C30 0.048(6) 0.045(6) 0.052(7) -0.013(5) -0.014(5) -0.010(5) C31 0.044(6) 0.054(7) 0.033(6) -0.012(5) -0.008(5) -0.003(5) C32 0.065(7) 0.031(6) 0.053(7) -0.005(5) -0.018(6) -0.013(5) Co5 0.0582(10) 0.0554(9) 0.0512(10) -0.0171(8) -0.0150(8) -0.0178(8) Co6 0.0515(10) 0.0700(11) 0.0743(11) -0.0238(9) -0.0237(9) -0.0129(8) Co7 0.0721(11) 0.0560(10) 0.0564(10) -0.0190(8) -0.0118(8) -0.0243(8) Co8 0.0572(10) 0.0805(12) 0.0547(10) -0.0099(9) -0.0136(8) -0.0348(9) C41 0.073(8) 0.036(6) 0.043(6) -0.010(5) -0.008(6) -0.021(6) O41 0.074(6) 0.095(7) 0.106(7) -0.056(6) -0.021(6) -0.005(6) C42 0.094(10) 0.091(11) 0.061(9) -0.014(8) -0.037(8) -0.024(8) O42 0.155(10) 0.117(8) 0.073(7) 0.014(6) -0.054(7) -0.044(7) C43 0.089(11) 0.090(11) 0.119(13) -0.057(10) -0.009(9) -0.026(9) O43 0.154(11) 0.163(11) 0.222(14) -0.140(11) 0.008(9) -0.074(9) C44 0.079(10) 0.065(9) 0.161(15) -0.040(10) -0.071(10) 0.018(8) O44 0.152(10) 0.081(8) 0.206(13) -0.018(8) -0.124(10) 0.008(7) C45 0.046(8) 0.111(11) 0.113(12) -0.042(10) -0.010(8) -0.012(8) O45 0.085(8) 0.250(14) 0.115(9) -0.095(10) 0.018(7) -0.020(8) C46 0.062(8) 0.080(10) 0.116(11) -0.048(9) -0.024(8) -0.013(7) O46 0.104(8) 0.112(8) 0.186(11) -0.054(8) -0.047(7) -0.049(7) C47 0.083(9) 0.053(7) 0.080(9) -0.045(7) -0.048(8) 0.020(7) O47 0.066(6) 0.099(7) 0.122(8) -0.061(6) -0.016(6) 0.005(6) C48 0.123(12) 0.063(9) 0.080(11) -0.018(8) -0.007(9) -0.028(9) O48 0.258(15) 0.061(7) 0.100(9) 0.008(6) -0.021(9) -0.042(8) C49 0.118(12) 0.117(12) 0.065(9) -0.038(9) -0.005(9) -0.061(10) O49 0.195(12) 0.170(11) 0.087(8) -0.068(8) -0.028(8) -0.075(9) C50 0.068(10) 0.099(12) 0.093(11) 0.004(10) -0.017(9) -0.035(9) O50 0.095(8) 0.105(9) 0.148(10) -0.006(8) 0.001(7) -0.011(7) C51 0.079(10) 0.089(11) 0.070(10) -0.016(8) -0.012(8) -0.035(8) O51 0.140(9) 0.119(9) 0.078(7) 0.006(6) -0.004(6) -0.066(7) C52 0.103(12) 0.140(14) 0.071(10) 0.030(9) -0.037(9) -0.066(10) O52 0.128(10) 0.256(15) 0.111(9) -0.030(9) -0.063(8) -0.075(9) C53 0.086(9) 0.039(6) 0.039(6) 0.005(5) -0.024(6) -0.030(6) C54 0.065(8) 0.057(7) 0.056(8) -0.012(6) -0.017(6) -0.030(6) C55 0.102(11) 0.085(10) 0.068(9) 0.017(8) -0.024(8) -0.058(9) C56 0.174(17) 0.086(11) 0.055(9) 0.028(8) -0.039(11) -0.080(12) C57 0.160(16) 0.070(10) 0.088(11) 0.033(9) -0.078(12) -0.063(11) C58 0.106(11) 0.050(8) 0.106(11) 0.004(8) -0.064(9) -0.034(8) C59 0.048(7) 0.044(6) 0.039(6) 0.005(5) -0.014(5) -0.014(5) C60 0.061(8) 0.069(8) 0.039(7) -0.010(6) -0.014(6) -0.014(6) C61 0.049(7) 0.092(9) 0.031(6) -0.011(6) 0.006(5) -0.013(7) C62 0.058(8) 0.074(8) 0.054(8) 0.019(7) -0.023(6) -0.037(7) C63 0.059(7) 0.047(7) 0.037(6) 0.004(5) -0.009(6) -0.020(6) C64 0.048(7) 0.046(6) 0.041(6) -0.003(5) -0.007(5) -0.017(5) C65 0.062(7) 0.041(6) 0.052(7) -0.011(5) -0.017(6) -0.018(5) C66 0.035(6) 0.051(7) 0.061(7) -0.026(6) -0.014(5) -0.002(5) C67 0.059(7) 0.040(6) 0.057(7) -0.016(6) -0.010(6) -0.021(5) C68 0.082(9) 0.056(7) 0.069(8) 0.001(6) -0.028(7) -0.037(7) C69 0.054(7) 0.072(8) 0.055(7) -0.030(6) -0.014(6) -0.013(6) C70 0.042(6) 0.065(8) 0.051(7) -0.010(6) -0.013(5) -0.025(6) C71 0.042(6) 0.050(6) 0.037(6) -0.011(5) -0.006(5) -0.014(5) C72 0.049(7) 0.069(8) 0.043(7) -0.017(6) -0.012(5) -0.013(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.791(13) . ? Co1 C2 1.799(13) . ? Co1 C3 1.821(13) . ? Co1 C27 1.972(10) . ? Co1 C26 1.974(10) . ? Co1 Co2 2.459(2) . ? Co2 C6 1.756(15) . ? Co2 C4 1.770(15) . ? Co2 C5 1.813(14) . ? Co2 C26 1.967(9) . ? Co2 C27 1.967(10) . ? Co3 C8 1.741(14) . ? Co3 C9 1.794(14) . ? Co3 C7 1.824(12) . ? Co3 C30 1.956(10) . ? Co3 C31 1.964(10) . ? Co3 Co4 2.465(3) . ? Co4 C11 1.766(15) . ? Co4 C12 1.780(15) . ? Co4 C10 1.814(13) . ? Co4 C31 1.959(10) . ? Co4 C30 1.961(10) . ? C1 O1 1.157(12) . ? C2 O2 1.128(12) . ? C3 O3 1.123(12) . ? C4 O4 1.153(14) . ? C5 O5 1.134(13) . ? C6 O6 1.139(14) . ? C7 O7 1.125(11) . ? C8 O8 1.151(13) . ? C9 O9 1.136(13) . ? C10 O10 1.140(12) . ? C11 O11 1.135(14) . ? C12 O12 1.144(14) . ? C13 C18 1.391(13) . ? C13 C14 1.393(13) . ? C13 C25 1.498(13) . ? C14 C15 1.372(13) . ? C14 C32 1.503(12) . ? C15 C16 1.391(15) . ? C16 C17 1.346(16) . ? C17 C18 1.354(15) . ? C19 C24 1.360(12) . ? C19 C20 1.393(13) . ? C19 C29 1.518(13) . ? C20 C21 1.363(14) . ? C21 C22 1.366(14) . ? C22 C23 1.385(14) . ? C23 C24 1.386(12) . ? C23 C28 1.501(13) . ? C25 C26 1.485(13) . ? C26 C27 1.349(12) . ? C27 C28 1.498(13) . ? C29 C30 1.511(13) . ? C30 C31 1.300(12) . ? C31 C32 1.500(12) . ? Co5 C41 1.743(13) . ? Co5 C42 1.779(14) . ? Co5 C43 1.805(14) . ? Co5 C67 1.957(10) . ? Co5 C66 1.959(9) . ? Co5 Co6 2.455(2) . ? Co6 C45 1.720(15) . ? Co6 C44 1.798(15) . ? Co6 C46 1.803(13) . ? Co6 C67 1.965(11) . ? Co6 C66 1.983(10) . ? Co7 C47 1.784(14) . ? Co7 C49 1.800(14) . ? Co7 C48 1.803(15) . ? Co7 C71 1.941(9) . ? Co7 C70 1.972(11) . ? Co7 Co8 2.461(3) . ? Co8 C50 1.767(16) . ? Co8 C52 1.776(16) . ? Co8 C51 1.804(14) . ? Co8 C70 1.952(10) . ? Co8 C71 1.968(10) . ? C41 O41 1.155(11) . ? C42 O42 1.166(13) . ? C43 O43 1.121(13) . ? C44 O44 1.140(14) . ? C45 O45 1.177(14) . ? C46 O46 1.138(12) . ? C47 O47 1.139(13) . ? C48 O48 1.138(14) . ? C49 O49 1.131(13) . ? C50 O50 1.164(15) . ? C51 O51 1.127(13) . ? C52 O52 1.143(14) . ? C53 C58 1.390(14) . ? C53 C54 1.397(14) . ? C53 C65 1.507(12) . ? C54 C55 1.362(14) . ? C54 C72 1.497(13) . ? C55 C56 1.361(17) . ? C56 C57 1.366(18) . ? C57 C58 1.353(16) . ? C59 C60 1.352(12) . ? C59 C64 1.389(13) . ? C59 C69 1.547(13) . ? C60 C61 1.383(13) . ? C61 C62 1.393(14) . ? C62 C63 1.369(13) . ? C63 C64 1.394(13) . ? C63 C68 1.487(13) . ? C65 C66 1.528(12) . ? C66 C67 1.303(12) . ? C67 C68 1.510(13) . ? C69 C70 1.506(13) . ? C70 C71 1.297(12) . ? C71 C72 1.523(12) . ? 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 C1 Co1 C2 98.2(5) . . ? C1 Co1 C3 104.6(5) . . ? C2 Co1 C3 98.1(5) . . ? C1 Co1 C27 104.2(5) . . ? C2 Co1 C27 103.8(5) . . ? C3 Co1 C27 140.5(5) . . ? C1 Co1 C26 141.4(5) . . ? C2 Co1 C26 104.1(4) . . ? C3 Co1 C26 103.0(5) . . ? C27 Co1 C26 40.0(4) . . ? C1 Co1 Co2 98.2(4) . . ? C2 Co1 Co2 153.1(4) . . ? C3 Co1 Co2 98.2(4) . . ? C27 Co1 Co2 51.3(3) . . ? C26 Co1 Co2 51.3(3) . . ? C6 Co2 C4 98.8(6) . . ? C6 Co2 C5 102.4(6) . . ? C4 Co2 C5 105.5(6) . . ? C6 Co2 C26 97.0(5) . . ? C4 Co2 C26 104.1(5) . . ? C5 Co2 C26 141.3(5) . . ? C6 Co2 C27 97.9(5) . . ? C4 Co2 C27 142.2(5) . . ? C5 Co2 C27 103.6(5) . . ? C26 Co2 C27 40.1(4) . . ? C6 Co2 Co1 146.4(4) . . ? C4 Co2 Co1 100.3(4) . . ? C5 Co2 Co1 98.7(4) . . ? C26 Co2 Co1 51.5(3) . . ? C27 Co2 Co1 51.5(3) . . ? C8 Co3 C9 97.7(6) . . ? C8 Co3 C7 103.5(5) . . ? C9 Co3 C7 103.4(5) . . ? C8 Co3 C30 95.0(5) . . ? C9 Co3 C30 111.7(5) . . ? C7 Co3 C30 137.5(5) . . ? C8 Co3 C31 106.6(5) . . ? C9 Co3 C31 142.0(5) . . ? C7 Co3 C31 98.9(4) . . ? C30 Co3 C31 38.7(4) . . ? C8 Co3 Co4 145.9(4) . . ? C9 Co3 Co4 93.2(4) . . ? C7 Co3 Co4 105.2(4) . . ? C30 Co3 Co4 51.1(3) . . ? C31 Co3 Co4 51.0(3) . . ? C11 Co4 C12 99.4(6) . . ? C11 Co4 C10 101.2(6) . . ? C12 Co4 C10 104.1(6) . . ? C11 Co4 C31 95.9(5) . . ? C12 Co4 C31 103.6(5) . . ? C10 Co4 C31 144.3(5) . . ? C11 Co4 C30 97.5(5) . . ? C12 Co4 C30 140.3(5) . . ? C10 Co4 C30 107.5(5) . . ? C31 Co4 C30 38.7(3) . . ? C11 Co4 Co3 145.3(4) . . ? C12 Co4 Co3 99.4(5) . . ? C10 Co4 Co3 102.2(4) . . ? C31 Co4 Co3 51.2(3) . . ? C30 Co4 Co3 50.9(3) . . ? O1 C1 Co1 178.7(11) . . ? O2 C2 Co1 178.4(12) . . ? O3 C3 Co1 178.1(12) . . ? O4 C4 Co2 177.7(13) . . ? O5 C5 Co2 176.5(13) . . ? O6 C6 Co2 173.3(13) . . ? O7 C7 Co3 176.1(11) . . ? O8 C8 Co3 177.6(12) . . ? O9 C9 Co3 178.7(13) . . ? O10 C10 Co4 179.1(14) . . ? O11 C11 Co4 176.5(15) . . ? O12 C12 Co4 177.8(13) . . ? C18 C13 C14 118.3(10) . . ? C18 C13 C25 121.1(11) . . ? C14 C13 C25 120.6(9) . . ? C15 C14 C13 118.5(10) . . ? C15 C14 C32 119.0(10) . . ? C13 C14 C32 122.5(9) . . ? C14 C15 C16 121.3(11) . . ? C17 C16 C15 120.1(12) . . ? C16 C17 C18 119.3(13) . . ? C17 C18 C13 122.4(12) . . ? C24 C19 C20 117.7(10) . . ? C24 C19 C29 121.1(10) . . ? C20 C19 C29 120.8(10) . . ? C21 C20 C19 120.9(11) . . ? C20 C21 C22 120.3(12) . . ? C21 C22 C23 120.7(11) . . ? C22 C23 C24 117.6(10) . . ? C22 C23 C28 121.0(10) . . ? C24 C23 C28 121.3(10) . . ? C19 C24 C23 122.9(10) . . ? C26 C25 C13 115.1(9) . . ? C27 C26 C25 141.3(9) . . ? C27 C26 Co2 70.0(6) . . ? C25 C26 Co2 132.5(7) . . ? C27 C26 Co1 69.9(6) . . ? C25 C26 Co1 137.3(7) . . ? Co2 C26 Co1 77.2(4) . . ? C26 C27 C28 142.7(10) . . ? C26 C27 Co2 69.9(6) . . ? C28 C27 Co2 132.2(7) . . ? C26 C27 Co1 70.1(6) . . ? C28 C27 Co1 136.2(8) . . ? Co2 C27 Co1 77.2(4) . . ? C27 C28 C23 112.1(8) . . ? C30 C29 C19 109.4(8) . . ? C31 C30 C29 139.8(9) . . ? C31 C30 Co3 71.0(6) . . ? C29 C30 Co3 135.3(7) . . ? C31 C30 Co4 70.5(6) . . ? C29 C30 Co4 134.6(7) . . ? Co3 C30 Co4 78.0(4) . . ? C30 C31 C32 140.7(9) . . ? C30 C31 Co4 70.8(6) . . ? C32 C31 Co4 132.6(7) . . ? C30 C31 Co3 70.3(6) . . ? C32 C31 Co3 136.7(7) . . ? Co4 C31 Co3 77.9(4) . . ? C31 C32 C14 116.0(8) . . ? C41 Co5 C42 98.2(5) . . ? C41 Co5 C43 95.5(5) . . ? C42 Co5 C43 106.4(6) . . ? C41 Co5 C67 102.0(5) . . ? C42 Co5 C67 140.0(5) . . ? C43 Co5 C67 105.7(6) . . ? C41 Co5 C66 104.0(4) . . ? C42 Co5 C66 102.7(5) . . ? C43 Co5 C66 142.1(5) . . ? C67 Co5 C66 38.9(4) . . ? C41 Co5 Co6 152.5(3) . . ? C42 Co5 Co6 100.2(4) . . ? C43 Co5 Co6 98.7(4) . . ? C67 Co5 Co6 51.4(3) . . ? C66 Co5 Co6 51.9(3) . . ? C45 Co6 C44 102.0(7) . . ? C45 Co6 C46 98.1(6) . . ? C44 Co6 C46 106.3(6) . . ? C45 Co6 C67 97.8(5) . . ? C44 Co6 C67 137.6(5) . . ? C46 Co6 C67 107.5(5) . . ? C45 Co6 C66 102.8(5) . . ? C44 Co6 C66 100.1(5) . . ? C46 Co6 C66 141.8(5) . . ? C67 Co6 C66 38.5(4) . . ? C45 Co6 Co5 148.5(4) . . ? C44 Co6 Co5 100.2(5) . . ? C46 Co6 Co5 96.8(4) . . ? C67 Co6 Co5 51.1(3) . . ? C66 Co6 Co5 51.0(3) . . ? C47 Co7 C49 97.6(6) . . ? C47 Co7 C48 96.1(6) . . ? C49 Co7 C48 107.0(6) . . ? C47 Co7 C71 105.0(4) . . ? C49 Co7 C71 139.9(6) . . ? C48 Co7 C71 102.9(5) . . ? C47 Co7 C70 105.9(5) . . ? C49 Co7 C70 103.5(6) . . ? C48 Co7 C70 139.3(5) . . ? C71 Co7 C70 38.7(4) . . ? C47 Co7 Co8 154.7(3) . . ? C49 Co7 Co8 97.7(5) . . ? C48 Co7 Co8 98.4(5) . . ? C71 Co7 Co8 51.5(3) . . ? C70 Co7 Co8 50.8(3) . . ? C50 Co8 C52 100.6(7) . . ? C50 Co8 C51 100.4(6) . . ? C52 Co8 C51 104.2(6) . . ? C50 Co8 C70 98.0(5) . . ? C52 Co8 C70 104.7(5) . . ? C51 Co8 C70 141.9(5) . . ? C50 Co8 C71 99.3(5) . . ? C52 Co8 C71 140.5(5) . . ? C51 Co8 C71 105.2(5) . . ? C70 Co8 C71 38.6(4) . . ? C50 Co8 Co7 147.4(4) . . ? C52 Co8 Co7 98.9(5) . . ? C51 Co8 Co7 99.8(4) . . ? C70 Co8 Co7 51.5(3) . . ? C71 Co8 Co7 50.5(3) . . ? O41 C41 Co5 177.9(10) . . ? O42 C42 Co5 178.3(13) . . ? O43 C43 Co5 178.5(15) . . ? O44 C44 Co6 174.3(14) . . ? O45 C45 Co6 175.8(14) . . ? O46 C46 Co6 177.9(14) . . ? O47 C47 Co7 177.3(11) . . ? O48 C48 Co7 176.0(13) . . ? O49 C49 Co7 176.0(13) . . ? O50 C50 Co8 175.7(13) . . ? O51 C51 Co8 177.4(13) . . ? O52 C52 Co8 175.8(15) . . ? C58 C53 C54 120.6(11) . . ? C58 C53 C65 118.2(11) . . ? C54 C53 C65 121.2(10) . . ? C55 C54 C53 117.3(11) . . ? C55 C54 C72 119.7(11) . . ? C53 C54 C72 123.1(10) . . ? C56 C55 C54 122.0(14) . . ? C55 C56 C57 120.4(14) . . ? C58 C57 C56 119.8(14) . . ? C57 C58 C53 119.9(13) . . ? C60 C59 C64 120.8(10) . . ? C60 C59 C69 121.3(10) . . ? C64 C59 C69 117.9(9) . . ? C59 C60 C61 119.7(10) . . ? C60 C61 C62 119.7(10) . . ? C63 C62 C61 121.3(10) . . ? C62 C63 C64 118.1(10) . . ? C62 C63 C68 120.6(11) . . ? C64 C63 C68 121.3(10) . . ? C59 C64 C63 120.4(9) . . ? C53 C65 C66 116.0(8) . . ? C67 C66 C65 143.3(10) . . ? C67 C66 Co5 70.5(6) . . ? C65 C66 Co5 135.5(7) . . ? C67 C66 Co6 70.0(7) . . ? C65 C66 Co6 132.1(7) . . ? Co5 C66 Co6 77.1(4) . . ? C66 C67 C68 136.8(10) . . ? C66 C67 Co5 70.6(6) . . ? C68 C67 Co5 136.4(8) . . ? C66 C67 Co6 71.5(6) . . ? C68 C67 Co6 136.0(8) . . ? Co5 C67 Co6 77.5(4) . . ? C63 C68 C67 111.6(8) . . ? C70 C69 C59 110.2(8) . . ? C71 C70 C69 141.0(10) . . ? C71 C70 Co8 71.4(6) . . ? C69 C70 Co8 132.6(7) . . ? C71 C70 Co7 69.4(6) . . ? C69 C70 Co7 136.8(7) . . ? Co8 C70 Co7 77.7(4) . . ? C70 C71 C72 139.1(10) . . ? C70 C71 Co7 71.9(6) . . ? C72 C71 Co7 137.3(7) . . ? C70 C71 Co8 70.0(6) . . ? C72 C71 Co8 132.7(7) . . ? Co7 C71 Co8 78.0(4) . . ? C54 C72 C71 115.8(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.428 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.093 #===END data_ramm4_8 _database_code_CSD 168767 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 Co4 O12' _chemical_formula_weight 780.13 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.761(2) _cell_length_b 12.608(5) _cell_length_c 16.058(6) _cell_angle_alpha 80.78(3) _cell_angle_beta 87.97(3) _cell_angle_gamma 86.97(3) _cell_volume 1548.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'platy' _exptl_crystal_colour brown _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.165 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6256 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.25 _reflns_number_total 6256 _reflns_number_gt 3976 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.5825P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6256 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.011 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 1.08326(10) -0.18505(7) 0.30100(5) 0.0530(2) Uani 1 1 d . . . Co2 Co 0.94342(11) -0.32527(6) 0.40154(5) 0.0531(2) Uani 1 1 d . . . Co3 Co 0.44863(10) 0.33980(6) 0.22186(5) 0.0492(2) Uani 1 1 d . . . Co4 Co 0.68606(10) 0.33385(6) 0.11598(5) 0.0461(2) Uani 1 1 d . . . C1 C 1.0678(8) -0.0619(6) 0.2282(4) 0.0676(19) Uani 1 1 d . . . O1 O 1.0621(7) 0.0166(5) 0.1823(3) 0.0970(18) Uani 1 1 d . . . C2 C 1.2519(10) -0.1541(7) 0.3653(5) 0.080(2) Uani 1 1 d . . . O2 O 1.3532(8) -0.1296(6) 0.4073(4) 0.126(3) Uani 1 1 d . . . C3 C 1.1771(10) -0.2695(7) 0.2296(5) 0.088(2) Uani 1 1 d . . . O3 O 1.2310(10) -0.3231(6) 0.1839(5) 0.157(3) Uani 1 1 d . . . C4 C 0.9929(10) -0.4432(6) 0.3510(4) 0.073(2) Uani 1 1 d . . . O4 O 1.0252(9) -0.5142(5) 0.3187(4) 0.113(2) Uani 1 1 d . . . C5 C 1.0944(11) -0.3341(6) 0.4851(5) 0.076(2) Uani 1 1 d . . . O5 O 1.1936(9) -0.3363(5) 0.5348(4) 0.122(2) Uani 1 1 d . . . C6 C 0.7558(11) -0.3674(6) 0.4631(4) 0.075(2) Uani 1 1 d . . . O6 O 0.6361(9) -0.3910(5) 0.5011(4) 0.126(2) Uani 1 1 d . . . C7 C 0.2913(8) 0.4047(5) 0.1481(5) 0.0624(17) Uani 1 1 d . . . O7 O 0.1957(7) 0.4444(5) 0.1004(4) 0.0984(18) Uani 1 1 d . . . C8 C 0.5149(9) 0.4431(6) 0.2800(5) 0.0687(19) Uani 1 1 d . . . O8 O 0.5586(8) 0.5052(5) 0.3157(4) 0.106(2) Uani 1 1 d . . . C9 C 0.3111(10) 0.2679(6) 0.2989(5) 0.075(2) Uani 1 1 d . . . O9 O 0.2260(8) 0.2200(5) 0.3483(4) 0.118(2) Uani 1 1 d . . . C10 C 0.8830(9) 0.2710(5) 0.0844(4) 0.0661(18) Uani 1 1 d . . . O10 O 1.0093(7) 0.2315(4) 0.0648(4) 0.0994(18) Uani 1 1 d . . . C11 C 0.5745(9) 0.3573(5) 0.0169(4) 0.0611(17) Uani 1 1 d . . . O11 O 0.5004(7) 0.3640(5) -0.0435(3) 0.0953(17) Uani 1 1 d . . . C12 C 0.7744(8) 0.4592(5) 0.1306(4) 0.0573(16) Uani 1 1 d . . . O12 O 0.8285(6) 0.5380(4) 0.1391(3) 0.0851(15) Uani 1 1 d . . . C13 C 0.8758(7) -0.1698(4) 0.3730(3) 0.0437(13) Uani 1 1 d . . . C14 C 0.8382(7) -0.2213(4) 0.3102(3) 0.0451(13) Uani 1 1 d . . . C15 C 0.7080(8) -0.2368(4) 0.2475(3) 0.0496(14) Uani 1 1 d . . . H15A H 0.5969 -0.2477 0.2763 0.080 Uiso 1 1 calc R . . H15B H 0.7411 -0.3013 0.2238 0.080 Uiso 1 1 calc R . . C16 C 0.6898(7) -0.1429(4) 0.1766(3) 0.0403(12) Uani 1 1 d . . . C17 C 0.7871(7) -0.1418(5) 0.1026(3) 0.0490(14) Uani 1 1 d . . . H17 H 0.8585 -0.2012 0.0947 0.080 Uiso 1 1 calc R . . C18 C 0.7776(8) -0.0515(5) 0.0403(3) 0.0530(15) Uani 1 1 d . . . H18 H 0.8444 -0.0502 -0.0091 0.080 Uiso 1 1 calc R . . C19 C 0.6707(8) 0.0356(4) 0.0511(3) 0.0508(15) Uani 1 1 d . . . H19 H 0.6663 0.0956 0.0090 0.080 Uiso 1 1 calc R . . C20 C 0.5680(7) 0.0353(4) 0.1247(3) 0.0422(13) Uani 1 1 d . . . C21 C 0.5797(7) -0.0557(4) 0.1856(3) 0.0420(13) Uani 1 1 d . . . H21 H 0.5107 -0.0581 0.2343 0.080 Uiso 1 1 calc R . . C22 C 0.4500(8) 0.1302(4) 0.1382(4) 0.0567(16) Uani 1 1 d . . . H22A H 0.3589 0.1058 0.1785 0.080 Uiso 1 1 calc R . . H22B H 0.3967 0.1602 0.0853 0.080 Uiso 1 1 calc R . . C23 C 0.5438(7) 0.2170(4) 0.1701(3) 0.0431(13) Uani 1 1 d . . . C24 C 0.6517(7) 0.2400(4) 0.2252(4) 0.0452(13) Uani 1 1 d . . . C25 C 0.7743(9) 0.1894(5) 0.2925(4) 0.0667(18) Uani 1 1 d . . . H25A H 0.7743 0.2345 0.3361 0.080 Uiso 1 1 calc R . . H25B H 0.8901 0.1867 0.2679 0.080 Uiso 1 1 calc R . . C26 C 0.7297(8) 0.0769(5) 0.3327(4) 0.0588(16) Uani 1 1 d . . . H26A H 0.6133 0.0795 0.3566 0.080 Uiso 1 1 calc R . . H26B H 0.7309 0.0317 0.2891 0.080 Uiso 1 1 calc R . . C27 C 0.8492(8) 0.0262(5) 0.4003(4) 0.0569(16) Uani 1 1 d . . . H27A H 0.8360 0.0656 0.4474 0.080 Uiso 1 1 calc R . . H27B H 0.9671 0.0325 0.3786 0.080 Uiso 1 1 calc R . . C28 C 0.8186(8) -0.0930(5) 0.4323(4) 0.0539(15) Uani 1 1 d . . . H28A H 0.8784 -0.1143 0.4848 0.080 Uiso 1 1 calc R . . H28B H 0.6962 -0.1003 0.4449 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0490(5) 0.0630(5) 0.0451(5) -0.0037(4) 0.0050(4) -0.0044(4) Co2 0.0673(6) 0.0434(5) 0.0451(5) 0.0009(4) 0.0006(4) 0.0042(4) Co3 0.0490(5) 0.0405(4) 0.0586(5) -0.0110(4) 0.0069(4) -0.0020(4) Co4 0.0444(5) 0.0367(4) 0.0579(5) -0.0114(3) 0.0042(4) -0.0010(3) C1 0.062(4) 0.091(6) 0.052(4) -0.009(4) -0.001(3) -0.030(4) O1 0.104(4) 0.095(4) 0.083(4) 0.025(3) -0.008(3) -0.039(3) C2 0.057(5) 0.111(6) 0.070(5) -0.004(4) 0.015(4) -0.015(4) O2 0.085(4) 0.215(8) 0.085(4) -0.024(4) -0.011(3) -0.057(5) C3 0.081(6) 0.103(6) 0.075(5) -0.003(5) 0.021(4) 0.002(5) O3 0.184(7) 0.149(7) 0.142(6) -0.064(5) 0.084(6) 0.015(5) C4 0.093(5) 0.057(4) 0.062(4) -0.002(4) 0.011(4) 0.013(4) O4 0.160(6) 0.070(4) 0.111(5) -0.034(3) 0.009(4) 0.024(4) C5 0.099(6) 0.065(5) 0.060(4) 0.007(4) -0.017(4) -0.008(4) O5 0.153(6) 0.123(5) 0.086(4) 0.007(4) -0.059(4) -0.018(4) C6 0.096(6) 0.059(4) 0.064(4) 0.004(4) 0.011(4) -0.001(4) O6 0.128(5) 0.112(5) 0.130(5) 0.000(4) 0.065(4) -0.028(4) C7 0.049(4) 0.053(4) 0.085(5) -0.017(4) 0.007(4) 0.007(3) O7 0.066(3) 0.108(5) 0.113(4) 0.004(4) -0.013(3) 0.019(3) C8 0.072(5) 0.057(4) 0.080(5) -0.018(4) 0.016(4) -0.015(4) O8 0.147(5) 0.084(4) 0.099(4) -0.045(3) 0.010(4) -0.041(4) C9 0.082(5) 0.069(5) 0.072(5) -0.011(4) 0.014(4) -0.005(4) O9 0.112(5) 0.121(5) 0.113(5) 0.011(4) 0.043(4) -0.033(4) C10 0.066(5) 0.049(4) 0.082(5) -0.010(3) 0.018(4) -0.006(3) O10 0.076(4) 0.087(4) 0.135(5) -0.032(3) 0.036(3) 0.016(3) C11 0.070(5) 0.048(4) 0.065(4) -0.012(3) 0.007(4) 0.004(3) O11 0.108(4) 0.105(4) 0.071(3) -0.008(3) -0.021(3) 0.009(3) C12 0.046(4) 0.048(4) 0.078(4) -0.015(3) 0.006(3) -0.001(3) O12 0.074(3) 0.059(3) 0.130(4) -0.035(3) 0.010(3) -0.022(3) C13 0.048(3) 0.038(3) 0.041(3) 0.005(3) 0.000(3) -0.003(3) C14 0.047(3) 0.039(3) 0.046(3) 0.000(3) 0.000(3) -0.002(3) C15 0.062(4) 0.038(3) 0.049(3) -0.003(3) -0.006(3) -0.010(3) C16 0.048(3) 0.036(3) 0.039(3) -0.010(2) -0.008(2) -0.010(3) C17 0.062(4) 0.047(3) 0.044(3) -0.023(3) -0.006(3) -0.002(3) C18 0.063(4) 0.061(4) 0.036(3) -0.012(3) 0.004(3) -0.011(3) C19 0.067(4) 0.040(3) 0.046(3) -0.003(3) -0.012(3) -0.011(3) C20 0.042(3) 0.035(3) 0.053(3) -0.012(3) -0.017(3) -0.006(2) C21 0.042(3) 0.039(3) 0.049(3) -0.018(3) -0.002(2) -0.008(2) C22 0.051(4) 0.040(3) 0.081(4) -0.013(3) -0.014(3) 0.001(3) C23 0.040(3) 0.031(3) 0.057(3) -0.006(3) 0.002(3) 0.001(2) C24 0.044(3) 0.030(3) 0.063(4) -0.011(3) -0.002(3) 0.001(2) C25 0.070(4) 0.051(4) 0.079(5) -0.006(3) -0.030(4) -0.006(3) C26 0.067(4) 0.051(4) 0.059(4) -0.007(3) -0.013(3) -0.006(3) C27 0.068(4) 0.050(4) 0.056(4) -0.016(3) -0.013(3) 0.002(3) C28 0.060(4) 0.050(4) 0.052(3) -0.010(3) -0.006(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.789(8) . ? Co1 C2 1.792(9) . ? Co1 C3 1.797(9) . ? Co1 C13 1.968(5) . ? Co1 C14 1.974(5) . ? Co1 Co2 2.4646(15) . ? Co2 C6 1.786(8) . ? Co2 C5 1.799(8) . ? Co2 C4 1.822(8) . ? Co2 C14 1.972(5) . ? Co2 C13 1.986(5) . ? Co3 C9 1.772(8) . ? Co3 C7 1.803(7) . ? Co3 C8 1.824(7) . ? Co3 C24 1.961(5) . ? Co3 C23 1.971(5) . ? Co3 Co4 2.4691(14) . ? Co4 C10 1.780(7) . ? Co4 C12 1.808(7) . ? Co4 C11 1.813(8) . ? Co4 C23 1.959(5) . ? Co4 C24 1.971(6) . ? C1 O1 1.135(8) . ? C2 O2 1.140(8) . ? C3 O3 1.130(9) . ? C4 O4 1.117(8) . ? C5 O5 1.125(8) . ? C6 O6 1.120(8) . ? C7 O7 1.125(7) . ? C8 O8 1.115(7) . ? C9 O9 1.132(8) . ? C10 O10 1.133(7) . ? C11 O11 1.135(7) . ? C12 O12 1.128(7) . ? C13 C14 1.331(7) . ? C13 C28 1.505(8) . ? C14 C15 1.494(7) . ? C15 C16 1.510(7) . ? C16 C21 1.379(7) . ? C16 C17 1.383(7) . ? C17 C18 1.392(8) . ? C18 C19 1.370(8) . ? C19 C20 1.402(8) . ? C20 C21 1.385(7) . ? C20 C22 1.507(7) . ? C22 C23 1.510(8) . ? C23 C24 1.315(7) . ? C24 C25 1.506(8) . ? C25 C26 1.514(8) . ? C26 C27 1.495(8) . ? C27 C28 1.536(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C2 99.5(3) . . ? C1 Co1 C3 98.0(3) . . ? C2 Co1 C3 107.7(4) . . ? C1 Co1 C13 101.1(3) . . ? C2 Co1 C13 102.4(3) . . ? C3 Co1 C13 140.8(3) . . ? C1 Co1 C14 99.9(3) . . ? C2 Co1 C14 140.1(3) . . ? C3 Co1 C14 103.7(3) . . ? C13 Co1 C14 39.5(2) . . ? C1 Co1 Co2 149.8(2) . . ? C2 Co1 Co2 99.7(2) . . ? C3 Co1 Co2 98.2(3) . . ? C13 Co1 Co2 51.78(15) . . ? C14 Co1 Co2 51.33(15) . . ? C6 Co2 C5 99.1(3) . . ? C6 Co2 C4 100.2(3) . . ? C5 Co2 C4 105.8(3) . . ? C6 Co2 C14 100.7(3) . . ? C5 Co2 C14 141.5(3) . . ? C4 Co2 C14 102.8(3) . . ? C6 Co2 C13 98.3(3) . . ? C5 Co2 C13 105.2(3) . . ? C4 Co2 C13 140.6(3) . . ? C14 Co2 C13 39.3(2) . . ? C6 Co2 Co1 148.2(2) . . ? C5 Co2 Co1 97.7(2) . . ? C4 Co2 Co1 100.9(2) . . ? C14 Co2 Co1 51.39(16) . . ? C13 Co2 Co1 51.11(15) . . ? C9 Co3 C7 100.2(3) . . ? C9 Co3 C8 100.0(3) . . ? C7 Co3 C8 106.2(3) . . ? C9 Co3 C24 101.1(3) . . ? C7 Co3 C24 139.6(3) . . ? C8 Co3 C24 103.4(3) . . ? C9 Co3 C23 98.0(3) . . ? C7 Co3 C23 104.1(3) . . ? C8 Co3 C23 141.2(3) . . ? C24 Co3 C23 39.1(2) . . ? C9 Co3 Co4 148.0(2) . . ? C7 Co3 Co4 95.5(2) . . ? C8 Co3 Co4 102.2(2) . . ? C24 Co3 Co4 51.28(17) . . ? C23 Co3 Co4 50.87(16) . . ? C10 Co4 C12 96.8(3) . . ? C10 Co4 C11 100.4(3) . . ? C12 Co4 C11 107.7(3) . . ? C10 Co4 C23 105.9(3) . . ? C12 Co4 C23 143.6(3) . . ? C11 Co4 C23 95.8(3) . . ? C10 Co4 C24 97.7(3) . . ? C12 Co4 C24 110.8(3) . . ? C11 Co4 C24 134.7(3) . . ? C23 Co4 C24 39.1(2) . . ? C10 Co4 Co3 148.6(2) . . ? C12 Co4 Co3 95.65(19) . . ? C11 Co4 Co3 103.0(2) . . ? C23 Co4 Co3 51.28(15) . . ? C24 Co4 Co3 50.91(15) . . ? O1 C1 Co1 178.3(6) . . ? O2 C2 Co1 176.0(8) . . ? O3 C3 Co1 177.8(9) . . ? O4 C4 Co2 178.5(7) . . ? O5 C5 Co2 176.7(7) . . ? O6 C6 Co2 178.1(7) . . ? O7 C7 Co3 178.2(6) . . ? O8 C8 Co3 178.6(7) . . ? O9 C9 Co3 178.4(7) . . ? O10 C10 Co4 179.3(7) . . ? O11 C11 Co4 174.7(6) . . ? O12 C12 Co4 179.3(7) . . ? C14 C13 C28 148.6(5) . . ? C14 C13 Co1 70.5(3) . . ? C28 C13 Co1 133.8(4) . . ? C14 C13 Co2 69.8(3) . . ? C28 C13 Co2 128.0(4) . . ? Co1 C13 Co2 77.1(2) . . ? C13 C14 C15 146.5(5) . . ? C13 C14 Co2 70.9(3) . . ? C15 C14 Co2 130.2(4) . . ? C13 C14 Co1 70.0(3) . . ? C15 C14 Co1 133.7(4) . . ? Co2 C14 Co1 77.3(2) . . ? C14 C15 C16 113.2(4) . . ? C21 C16 C17 119.1(5) . . ? C21 C16 C15 120.5(5) . . ? C17 C16 C15 120.4(5) . . ? C16 C17 C18 119.6(5) . . ? C19 C18 C17 120.5(5) . . ? C18 C19 C20 120.8(5) . . ? C21 C20 C19 117.5(5) . . ? C21 C20 C22 120.7(5) . . ? C19 C20 C22 121.8(5) . . ? C16 C21 C20 122.4(5) . . ? C20 C22 C23 112.5(5) . . ? C24 C23 C22 146.6(5) . . ? C24 C23 Co4 70.9(3) . . ? C22 C23 Co4 134.0(4) . . ? C24 C23 Co3 70.0(3) . . ? C22 C23 Co3 129.2(4) . . ? Co4 C23 Co3 77.84(19) . . ? C23 C24 C25 142.7(5) . . ? C23 C24 Co3 70.9(3) . . ? C25 C24 Co3 134.9(4) . . ? C23 C24 Co4 70.0(3) . . ? C25 C24 Co4 132.7(4) . . ? Co3 C24 Co4 77.8(2) . . ? C24 C25 C26 113.5(5) . . ? C27 C26 C25 114.1(5) . . ? C26 C27 C28 113.8(5) . . ? C13 C28 C27 115.7(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.442 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.080 #===END data_br11_9 _database_code_CSD 168768 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Co4 O12' _chemical_formula_weight 760.14 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7821(2) _cell_length_b 10.8413(2) _cell_length_c 13.1236(2) _cell_angle_alpha 93.1920(10) _cell_angle_beta 90.0893(3) _cell_angle_gamma 96.5130(10) _cell_volume 1521.73(5) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 15640 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6919 _reflns_number_gt 6007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0356P)^2^+0.3313P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6919 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.351110(19) 0.23760(2) 0.356584(16) 0.02536(6) Uani 1 1 d . . . Co2 Co 0.43565(2) 0.08719(2) 0.234869(17) 0.02696(6) Uani 1 1 d . . . Co3 Co 0.99958(2) 0.72765(2) 0.305085(19) 0.03453(7) Uani 1 1 d . . . Co4 Co 0.95723(2) 0.74833(2) 0.121586(18) 0.03221(7) Uani 1 1 d . . . C1 C 0.47469(14) 0.27013(14) 0.24784(12) 0.0249(3) Uani 1 1 d . . . C2 C 0.52776(14) 0.22026(14) 0.32467(12) 0.0250(3) Uani 1 1 d . . . C3 C 0.64054(15) 0.22390(16) 0.39223(13) 0.0296(3) Uani 1 1 d . . . H3A H 0.6201 0.1684 0.4487 0.036 Uiso 1 1 calc R . . H3B H 0.6605 0.3095 0.4226 0.036 Uiso 1 1 calc R . . C4 C 0.75671(16) 0.18464(16) 0.33746(14) 0.0332(4) Uani 1 1 d . . . H4A H 0.8253 0.1877 0.3881 0.040 Uiso 1 1 calc R . . H4B H 0.7381 0.0972 0.3108 0.040 Uiso 1 1 calc R . . C5 C 0.80196(15) 0.26355(15) 0.24972(13) 0.0302(3) Uani 1 1 d . . . H5A H 0.7334 0.2607 0.1991 0.036 Uiso 1 1 calc R . . H5B H 0.8719 0.2263 0.2158 0.036 Uiso 1 1 calc R . . C6 C 0.84549(15) 0.39936(15) 0.28090(13) 0.0293(3) Uani 1 1 d . . . H6A H 0.7753 0.4386 0.3126 0.035 Uiso 1 1 calc R . . H6B H 0.9133 0.4033 0.3323 0.035 Uiso 1 1 calc R . . C7 C 0.89241(17) 0.47113(15) 0.18926(13) 0.0313(4) Uani 1 1 d . . . H7A H 0.9753 0.4469 0.1698 0.038 Uiso 1 1 calc R . . H7B H 0.8348 0.4469 0.1310 0.038 Uiso 1 1 calc R . . C8 C 0.90315(15) 0.60912(16) 0.20791(12) 0.0285(3) Uani 1 1 d . . . C9 C 0.83772(15) 0.70434(15) 0.23064(12) 0.0276(3) Uani 1 1 d . . . C10 C 0.71238(16) 0.74239(16) 0.25821(14) 0.0315(4) Uani 1 1 d . . . H10A H 0.7225 0.8320 0.2797 0.038 Uiso 1 1 calc R . . H10B H 0.6804 0.6961 0.3174 0.038 Uiso 1 1 calc R . . C11 C 0.61450(16) 0.71999(16) 0.17171(14) 0.0331(4) Uani 1 1 d . . . H11A H 0.5373 0.7534 0.1957 0.040 Uiso 1 1 calc R . . H11B H 0.6459 0.7681 0.1132 0.040 Uiso 1 1 calc R . . C12 C 0.58107(16) 0.58430(16) 0.13381(13) 0.0305(3) Uani 1 1 d . . . H12A H 0.5186 0.5811 0.0781 0.037 Uiso 1 1 calc R . . H12B H 0.6568 0.5528 0.1046 0.037 Uiso 1 1 calc R . . C13 C 0.52922(16) 0.49762(15) 0.21499(13) 0.0294(3) Uani 1 1 d . . . H13A H 0.4541 0.5288 0.2456 0.035 Uiso 1 1 calc R . . H13B H 0.5923 0.4972 0.2699 0.035 Uiso 1 1 calc R . . C14 C 0.49518(15) 0.36500(15) 0.16972(12) 0.0284(3) Uani 1 1 d . . . H14A H 0.4183 0.3624 0.1280 0.034 Uiso 1 1 calc R . . H14B H 0.5630 0.3429 0.1238 0.034 Uiso 1 1 calc R . . C15 C 0.36489(18) 0.37860(19) 0.43484(17) 0.0439(5) Uani 1 1 d . . . O15 O 0.36833(17) 0.46663(18) 0.48555(17) 0.0809(6) Uani 1 1 d . . . C16 C 0.30886(18) 0.13020(18) 0.45498(14) 0.0372(4) Uani 1 1 d . . . O16 O 0.28195(19) 0.06145(16) 0.51535(12) 0.0648(5) Uani 1 1 d . . . C17 C 0.20381(17) 0.25637(18) 0.29509(14) 0.0365(4) Uani 1 1 d . . . O17 O 0.11194(14) 0.26938(19) 0.25762(13) 0.0625(5) Uani 1 1 d . . . C25 C 0.29896(18) 0.06205(19) 0.15266(15) 0.0412(4) Uani 1 1 d . . . O25 O 0.21301(15) 0.05099(19) 0.10139(14) 0.0683(5) Uani 1 1 d . . . C26 C 0.4364(2) -0.04479(18) 0.31409(15) 0.0445(5) Uani 1 1 d . . . O26 O 0.4411(2) -0.12466(17) 0.36510(14) 0.0824(7) Uani 1 1 d . . . C27 C 0.54961(17) 0.05302(17) 0.14132(14) 0.0357(4) Uani 1 1 d . . . O27 O 0.62069(15) 0.03275(16) 0.08115(12) 0.0576(4) Uani 1 1 d . . . C35 C 1.0209(2) 0.8934(2) 0.34140(18) 0.0534(5) Uani 1 1 d . . . O35 O 1.0296(2) 0.99689(17) 0.36220(17) 0.0851(6) Uani 1 1 d . . . C36 C 0.95208(18) 0.6688(2) 0.42533(15) 0.0427(5) Uani 1 1 d . . . O36 O 0.92169(17) 0.63014(19) 0.50122(12) 0.0644(5) Uani 1 1 d . . . C37 C 1.1509(2) 0.6689(3) 0.2970(2) 0.0611(6) Uani 1 1 d . . . O37 O 1.24084(19) 0.6263(3) 0.2915(2) 0.1113(9) Uani 1 1 d . . . C45 C 1.1144(2) 0.7337(2) 0.07746(17) 0.0472(5) Uani 1 1 d . . . O45 O 1.21303(16) 0.7239(2) 0.05112(16) 0.0767(6) Uani 1 1 d . . . C46 C 0.8737(2) 0.6816(2) 0.01019(15) 0.0431(5) Uani 1 1 d . . . O46 O 0.81860(17) 0.63273(18) -0.05715(12) 0.0641(5) Uani 1 1 d . . . C47 C 0.93636(19) 0.91355(19) 0.11715(15) 0.0404(4) Uani 1 1 d . . . O47 O 0.91904(16) 1.01387(14) 0.11627(14) 0.0593(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 0.02166(11) 0.02598(11) 0.02802(11) -0.00038(8) 0.00239(8) 0.00178(8) Co2 0.02735(12) 0.02417(11) 0.02821(11) -0.00186(8) 0.00319(8) -0.00046(8) Co3 0.02808(12) 0.03715(14) 0.03680(13) -0.00213(10) -0.00124(10) -0.00099(10) Co4 0.03264(13) 0.02919(13) 0.03439(13) 0.00318(9) 0.00836(10) 0.00094(9) C1 0.0218(7) 0.0235(7) 0.0289(8) 0.0001(6) 0.0025(6) 0.0010(6) C2 0.0220(7) 0.0240(7) 0.0285(8) -0.0011(6) 0.0033(6) 0.0009(6) C3 0.0277(8) 0.0324(9) 0.0291(8) 0.0055(7) -0.0020(6) 0.0026(7) C4 0.0247(8) 0.0294(9) 0.0464(10) 0.0067(7) -0.0026(7) 0.0051(7) C5 0.0235(8) 0.0277(8) 0.0396(9) -0.0009(7) 0.0035(7) 0.0048(6) C6 0.0266(8) 0.0280(8) 0.0338(8) 0.0010(7) 0.0010(6) 0.0056(6) C7 0.0333(9) 0.0256(8) 0.0355(9) -0.0006(7) 0.0054(7) 0.0059(7) C8 0.0293(8) 0.0277(8) 0.0280(8) 0.0011(6) 0.0028(6) 0.0009(6) C9 0.0272(8) 0.0259(8) 0.0285(8) 0.0005(6) 0.0022(6) -0.0010(6) C10 0.0306(8) 0.0261(8) 0.0370(9) -0.0043(7) 0.0065(7) 0.0021(7) C11 0.0311(9) 0.0263(8) 0.0425(10) 0.0044(7) 0.0018(7) 0.0051(7) C12 0.0307(8) 0.0280(8) 0.0326(8) 0.0043(7) -0.0008(7) 0.0018(7) C13 0.0288(8) 0.0271(8) 0.0327(8) 0.0039(7) 0.0018(6) 0.0037(6) C14 0.0270(8) 0.0297(8) 0.0280(8) 0.0046(6) -0.0030(6) 0.0001(6) C15 0.0297(9) 0.0433(11) 0.0563(12) -0.0120(9) 0.0071(8) 0.0005(8) O15 0.0598(11) 0.0625(11) 0.1120(16) -0.0508(11) 0.0130(10) -0.0029(9) C16 0.0399(10) 0.0380(10) 0.0343(9) 0.0007(8) 0.0057(8) 0.0077(8) O16 0.0939(13) 0.0575(10) 0.0462(9) 0.0209(8) 0.0222(9) 0.0127(9) C17 0.0311(9) 0.0439(10) 0.0353(9) 0.0040(8) 0.0055(7) 0.0067(8) O17 0.0372(8) 0.0977(14) 0.0570(9) 0.0102(9) -0.0059(7) 0.0238(8) C25 0.0344(10) 0.0428(11) 0.0435(10) -0.0123(8) 0.0028(8) -0.0014(8) O25 0.0429(9) 0.0903(14) 0.0674(11) -0.0279(10) -0.0162(8) 0.0048(9) C26 0.0635(13) 0.0319(10) 0.0384(10) -0.0021(8) 0.0166(9) 0.0089(9) O26 0.150(2) 0.0467(10) 0.0568(10) 0.0209(8) 0.0372(12) 0.0311(11) C27 0.0361(9) 0.0328(9) 0.0365(9) -0.0045(7) 0.0016(8) -0.0002(7) O27 0.0514(9) 0.0651(10) 0.0538(9) -0.0145(8) 0.0208(7) 0.0040(8) C35 0.0526(13) 0.0470(13) 0.0558(13) -0.0055(10) -0.0088(10) -0.0112(10) O35 0.1063(16) 0.0456(10) 0.0958(15) -0.0150(10) -0.0172(12) -0.0143(10) C36 0.0357(10) 0.0536(12) 0.0383(10) -0.0061(9) -0.0044(8) 0.0069(9) O36 0.0629(10) 0.0936(14) 0.0375(8) 0.0087(8) 0.0052(7) 0.0107(9) C37 0.0378(12) 0.0825(18) 0.0632(15) 0.0025(13) -0.0007(10) 0.0087(12) O37 0.0498(12) 0.170(3) 0.123(2) 0.0091(18) 0.0014(12) 0.0511(14) C45 0.0441(12) 0.0472(12) 0.0494(12) 0.0020(9) 0.0135(9) 0.0013(9) O45 0.0464(10) 0.0965(15) 0.0868(13) -0.0015(11) 0.0297(9) 0.0091(10) C46 0.0457(11) 0.0479(12) 0.0362(10) 0.0096(9) 0.0125(9) 0.0034(9) O46 0.0622(10) 0.0897(13) 0.0360(8) -0.0039(8) -0.0015(7) -0.0062(9) C47 0.0409(10) 0.0375(11) 0.0426(10) 0.0039(8) 0.0078(8) 0.0027(8) O47 0.0695(11) 0.0365(8) 0.0732(11) 0.0019(7) 0.0028(9) 0.0133(7) _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 C15 1.785(2) . ? Co1 C16 1.8109(19) . ? Co1 C17 1.8174(19) . ? Co1 C1 1.9728(16) . ? Co1 C2 1.9782(15) . ? Co1 Co2 2.4684(3) . ? Co2 C27 1.7921(19) . ? Co2 C25 1.812(2) . ? Co2 C26 1.816(2) . ? Co2 C1 1.9780(16) . ? Co2 C2 1.9846(16) . ? Co3 C36 1.789(2) . ? Co3 C37 1.819(2) . ? Co3 C35 1.822(2) . ? Co3 C8 1.9670(17) . ? Co3 C9 1.9827(16) . ? Co3 Co4 2.4775(3) . ? Co4 C46 1.789(2) . ? Co4 C45 1.813(2) . ? Co4 C47 1.835(2) . ? Co4 C9 1.9694(16) . ? Co4 C8 1.9733(17) . ? C1 C2 1.329(2) . ? C1 C14 1.491(2) . ? C2 C3 1.499(2) . ? C3 C4 1.535(2) . ? C4 C5 1.521(2) . ? C5 C6 1.527(2) . ? C6 C7 1.525(2) . ? C7 C8 1.494(2) . ? C8 C9 1.336(2) . ? C9 C10 1.496(2) . ? C10 C11 1.539(2) . ? C11 C12 1.529(2) . ? C12 C13 1.525(2) . ? C13 C14 1.530(2) . ? C15 O15 1.130(2) . ? C16 O16 1.134(2) . ? C17 O17 1.132(2) . ? C25 O25 1.136(2) . ? C26 O26 1.129(3) . ? C27 O27 1.131(2) . ? C35 O35 1.133(3) . ? C36 O36 1.136(3) . ? C37 O37 1.121(3) . ? C45 O45 1.133(3) . ? C46 O46 1.136(3) . ? C47 O47 1.125(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 C15 Co1 C16 98.28(10) . . ? C15 Co1 C17 97.47(9) . . ? C16 Co1 C17 104.41(9) . . ? C15 Co1 C1 104.24(8) . . ? C16 Co1 C1 141.29(8) . . ? C17 Co1 C1 103.38(7) . . ? C15 Co1 C2 101.73(8) . . ? C16 Co1 C2 105.63(8) . . ? C17 Co1 C2 141.29(7) . . ? C1 Co1 C2 39.31(7) . . ? C15 Co1 Co2 152.26(6) . . ? C16 Co1 Co2 96.84(6) . . ? C17 Co1 Co2 101.09(6) . . ? C1 Co1 Co2 51.43(5) . . ? C2 Co1 Co2 51.59(5) . . ? C27 Co2 C25 97.98(8) . . ? C27 Co2 C26 100.89(9) . . ? C25 Co2 C26 108.63(10) . . ? C27 Co2 C1 98.85(7) . . ? C25 Co2 C1 104.17(8) . . ? C26 Co2 C1 138.57(8) . . ? C27 Co2 C2 102.96(7) . . ? C25 Co2 C2 139.85(8) . . ? C26 Co2 C2 100.59(8) . . ? C1 Co2 C2 39.19(7) . . ? C27 Co2 Co1 149.49(6) . . ? C25 Co2 Co1 95.85(6) . . ? C26 Co2 Co1 100.22(6) . . ? C1 Co2 Co1 51.24(4) . . ? C2 Co2 Co1 51.36(4) . . ? C36 Co3 C37 98.26(11) . . ? C36 Co3 C35 99.38(10) . . ? C37 Co3 C35 109.59(12) . . ? C36 Co3 C8 102.17(8) . . ? C37 Co3 C8 100.13(10) . . ? C35 Co3 C8 140.05(9) . . ? C36 Co3 C9 100.34(8) . . ? C37 Co3 C9 138.39(10) . . ? C35 Co3 C9 103.64(9) . . ? C8 Co3 C9 39.53(7) . . ? C36 Co3 Co4 149.93(6) . . ? C37 Co3 Co4 100.04(8) . . ? C35 Co3 Co4 96.69(8) . . ? C8 Co3 Co4 51.15(5) . . ? C9 Co3 Co4 50.94(5) . . ? C46 Co4 C45 98.42(10) . . ? C46 Co4 C47 102.33(9) . . ? C45 Co4 C47 106.11(9) . . ? C46 Co4 C9 101.85(8) . . ? C45 Co4 C9 143.67(9) . . ? C47 Co4 C9 98.63(8) . . ? C46 Co4 C8 95.17(8) . . ? C45 Co4 C8 109.05(9) . . ? C47 Co4 C8 137.66(8) . . ? C9 Co4 C8 39.60(7) . . ? C46 Co4 Co3 145.92(6) . . ? C45 Co4 Co3 96.72(7) . . ? C47 Co4 Co3 102.49(6) . . ? C9 Co4 Co3 51.42(5) . . ? C8 Co4 Co3 50.93(5) . . ? C2 C1 C14 144.07(15) . . ? C2 C1 Co1 70.57(9) . . ? C14 C1 Co1 134.45(12) . . ? C2 C1 Co2 70.68(10) . . ? C14 C1 Co2 131.73(12) . . ? Co1 C1 Co2 77.33(6) . . ? C1 C2 C3 146.54(15) . . ? C1 C2 Co1 70.13(9) . . ? C3 C2 Co1 131.45(11) . . ? C1 C2 Co2 70.14(10) . . ? C3 C2 Co2 132.98(12) . . ? Co1 C2 Co2 77.05(6) . . ? C2 C3 C4 114.23(14) . . ? C5 C4 C3 115.00(14) . . ? C4 C5 C6 114.58(14) . . ? C7 C6 C5 111.33(14) . . ? C8 C7 C6 113.88(14) . . ? C9 C8 C7 143.47(16) . . ? C9 C8 Co3 70.87(10) . . ? C7 C8 Co3 133.90(13) . . ? C9 C8 Co4 70.04(10) . . ? C7 C8 Co4 132.81(12) . . ? Co3 C8 Co4 77.92(6) . . ? C8 C9 C10 145.74(16) . . ? C8 C9 Co4 70.36(10) . . ? C10 C9 Co4 133.55(12) . . ? C8 C9 Co3 69.60(10) . . ? C10 C9 Co3 131.62(12) . . ? Co4 C9 Co3 77.64(6) . . ? C9 C10 C11 114.55(14) . . ? C12 C11 C10 115.54(14) . . ? C13 C12 C11 114.95(14) . . ? C12 C13 C14 111.31(14) . . ? C1 C14 C13 113.80(14) . . ? O15 C15 Co1 176.99(18) . . ? O16 C16 Co1 178.86(19) . . ? O17 C17 Co1 179.1(2) . . ? O25 C25 Co2 177.4(2) . . ? O26 C26 Co2 177.3(2) . . ? O27 C27 Co2 178.82(19) . . ? O35 C35 Co3 177.3(2) . . ? O36 C36 Co3 179.2(2) . . ? O37 C37 Co3 176.2(3) . . ? O45 C45 Co4 179.0(2) . . ? O46 C46 Co4 175.65(19) . . ? O47 C47 Co4 177.22(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.347 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.055 #===END data_br8_10 _database_code_CSD 168769 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Co4 O12 S' _chemical_formula_weight 778.17 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.81230(10) _cell_length_b 13.7006(2) _cell_length_c 15.1082(2) _cell_angle_alpha 105.3670(10) _cell_angle_beta 101.7320(10) _cell_angle_gamma 91.2380(10) _cell_volume 1521.80(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description orthorhombic _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 15418 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6965 _reflns_number_gt 5825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0357P)^2^+0.2673P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6965 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.005 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 1.54643(3) 0.87497(2) 0.802147(19) 0.02850(7) Uani 1 1 d . . . Co2 Co 1.26840(4) 0.77438(2) 0.785376(19) 0.02900(7) Uani 1 1 d . . . Co3 Co 1.18564(4) 0.62130(2) 0.198217(19) 0.02851(7) Uani 1 1 d . . . Co4 Co 0.92745(3) 0.72290(2) 0.185285(18) 0.02691(7) Uani 1 1 d . . . S50 S 1.25379(6) 1.01186(4) 0.50285(3) 0.02460(10) Uani 1 1 d . . . O11 O 1.8244(2) 0.92378(15) 0.71319(14) 0.0534(5) Uani 1 1 d . . . C11 C 1.7172(3) 0.90662(17) 0.74887(16) 0.0363(5) Uani 1 1 d . . . C12 C 1.6762(3) 0.8140(2) 0.88316(17) 0.0461(6) Uani 1 1 d . . . O12 O 1.7534(3) 0.77338(18) 0.93201(16) 0.0771(7) Uani 1 1 d . . . C13 C 1.5064(3) 1.00024(19) 0.87133(17) 0.0436(6) Uani 1 1 d . . . O13 O 1.4751(3) 1.07799(15) 0.91097(15) 0.0702(6) Uani 1 1 d . . . C21 C 1.3465(3) 0.66882(19) 0.83136(17) 0.0420(5) Uani 1 1 d . . . O21 O 1.3976(3) 0.60045(16) 0.85387(15) 0.0660(6) Uani 1 1 d . . . C22 C 1.0599(3) 0.71943(17) 0.71437(18) 0.0403(5) Uani 1 1 d . . . O22 O 0.9274(2) 0.68670(15) 0.66763(17) 0.0689(6) Uani 1 1 d . . . C23 C 1.1914(3) 0.8656(2) 0.87724(17) 0.0446(6) Uani 1 1 d . . . O23 O 1.1443(3) 0.92519(18) 0.93328(15) 0.0724(6) Uani 1 1 d . . . C31 C 1.2839(3) 0.66500(18) 0.11476(17) 0.0416(5) Uani 1 1 d . . . O31 O 1.3453(3) 0.69544(16) 0.06451(14) 0.0675(6) Uani 1 1 d . . . C32 C 1.3795(3) 0.59428(19) 0.27015(18) 0.0437(6) Uani 1 1 d . . . O32 O 1.5021(3) 0.57901(18) 0.31890(16) 0.0715(6) Uani 1 1 d . . . C33 C 1.0835(3) 0.49316(18) 0.13868(17) 0.0420(5) Uani 1 1 d . . . O33 O 1.0154(3) 0.41449(14) 0.10573(17) 0.0696(6) Uani 1 1 d . . . O41 O 0.6471(2) 0.81427(15) 0.27316(14) 0.0578(5) Uani 1 1 d . . . C41 C 0.7569(3) 0.78085(17) 0.23846(16) 0.0377(5) Uani 1 1 d . . . O42 O 0.7010(2) 0.56449(14) 0.03195(13) 0.0563(5) Uani 1 1 d . . . C42 C 0.7873(3) 0.62583(18) 0.09060(15) 0.0372(5) Uani 1 1 d . . . C43 C 0.9993(3) 0.81866(19) 0.13336(17) 0.0439(6) Uani 1 1 d . . . O43 O 1.0532(3) 0.88114(17) 0.10831(15) 0.0756(7) Uani 1 1 d . . . C51 C 1.3606(2) 0.94798(15) 0.58745(13) 0.0241(4) Uani 1 1 d . . . H51A H 1.4106 0.8871 0.5535 0.029 Uiso 1 1 calc R . . H51B H 1.4592 0.9939 0.6314 0.029 Uiso 1 1 calc R . . C52 C 1.2411(2) 0.91516(15) 0.64478(13) 0.0246(4) Uani 1 1 d . . . H52A H 1.2065 0.9760 0.6875 0.030 Uiso 1 1 calc R . . H52B H 1.1333 0.8772 0.6019 0.030 Uiso 1 1 calc R . . C53 C 1.3338(2) 0.84934(15) 0.70112(13) 0.0241(4) Uani 1 1 d . . . C54 C 1.4182(2) 0.76521(15) 0.69394(13) 0.0251(4) Uani 1 1 d . . . C55 C 1.4818(3) 0.67847(16) 0.62800(15) 0.0307(4) Uani 1 1 d . . . H55A H 1.5582 0.6404 0.6654 0.037 Uiso 1 1 calc R . . H55B H 1.5539 0.7061 0.5921 0.037 Uiso 1 1 calc R . . C56 C 1.3336(3) 0.60470(16) 0.55843(15) 0.0329(5) Uani 1 1 d . . . H56A H 1.3860 0.5466 0.5219 0.039 Uiso 1 1 calc R . . H56B H 1.2605 0.5779 0.5945 0.039 Uiso 1 1 calc R . . C57 C 1.2152(3) 0.65201(16) 0.48995(14) 0.0311(4) Uani 1 1 d . . . H57A H 1.2887 0.6870 0.4597 0.037 Uiso 1 1 calc R . . H57B H 1.1485 0.7033 0.5252 0.037 Uiso 1 1 calc R . . C58 C 1.0869(3) 0.57190(17) 0.41410(15) 0.0376(5) Uani 1 1 d . . . H58A H 1.1549 0.5241 0.3761 0.045 Uiso 1 1 calc R . . H58B H 1.0226 0.5327 0.4452 0.045 Uiso 1 1 calc R . . C59 C 0.9534(3) 0.61453(18) 0.34804(15) 0.0354(5) Uani 1 1 d . . . H59A H 0.8679 0.5585 0.3067 0.042 Uiso 1 1 calc R . . H59B H 0.8883 0.6643 0.3860 0.042 Uiso 1 1 calc R . . C60 C 1.0336(2) 0.66496(15) 0.28807(13) 0.0250(4) Uani 1 1 d . . . C61 C 1.1363(2) 0.74452(15) 0.28847(13) 0.0240(4) Uani 1 1 d . . . C62 C 1.2437(2) 0.83805(14) 0.35144(13) 0.0245(4) Uani 1 1 d . . . H62A H 1.2890 0.8766 0.3130 0.029 Uiso 1 1 calc R . . H62B H 1.3452 0.8188 0.3925 0.029 Uiso 1 1 calc R . . C63 C 1.1321(2) 0.90484(15) 0.41205(13) 0.0249(4) Uani 1 1 d . . . H63A H 1.0724 0.8622 0.4421 0.030 Uiso 1 1 calc R . . H63B H 1.0402 0.9307 0.3705 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02700(14) 0.03173(15) 0.02347(14) 0.00797(11) -0.00196(11) -0.00248(11) Co2 0.02914(14) 0.03326(15) 0.02788(14) 0.01291(12) 0.00786(11) 0.00068(11) Co3 0.02835(14) 0.02754(15) 0.02691(14) 0.00136(11) 0.00816(11) 0.00011(11) Co4 0.02712(14) 0.02988(15) 0.02026(13) 0.00477(11) 0.00044(10) -0.00083(11) S50 0.0279(2) 0.0231(2) 0.0222(2) 0.00563(18) 0.00487(18) 0.00105(18) O11 0.0365(9) 0.0625(12) 0.0698(13) 0.0303(10) 0.0151(9) 0.0004(8) C11 0.0290(11) 0.0359(12) 0.0409(12) 0.0132(10) -0.0026(9) -0.0020(9) C12 0.0436(13) 0.0494(15) 0.0391(13) 0.0159(11) -0.0088(11) -0.0044(11) O12 0.0757(15) 0.0837(16) 0.0692(14) 0.0439(13) -0.0211(12) 0.0072(12) C13 0.0475(14) 0.0429(14) 0.0345(12) 0.0069(11) 0.0010(10) -0.0047(11) O13 0.0946(16) 0.0425(11) 0.0637(13) -0.0042(10) 0.0200(12) 0.0063(11) C21 0.0470(13) 0.0471(14) 0.0385(13) 0.0210(11) 0.0122(11) 0.0049(11) O21 0.0846(15) 0.0575(12) 0.0714(14) 0.0415(11) 0.0189(12) 0.0202(11) C22 0.0344(12) 0.0337(12) 0.0555(15) 0.0131(11) 0.0147(11) 0.0020(10) O22 0.0338(10) 0.0529(12) 0.1023(17) 0.0030(11) 0.0004(10) -0.0083(8) C23 0.0474(14) 0.0546(15) 0.0376(13) 0.0173(12) 0.0162(11) 0.0037(12) O23 0.0875(16) 0.0799(15) 0.0529(12) 0.0056(11) 0.0374(12) 0.0198(12) C31 0.0425(13) 0.0425(13) 0.0359(12) -0.0004(10) 0.0152(10) -0.0028(10) O31 0.0778(14) 0.0765(14) 0.0546(12) 0.0137(11) 0.0366(11) -0.0130(11) C32 0.0378(13) 0.0432(14) 0.0487(14) 0.0073(11) 0.0131(11) 0.0068(10) O32 0.0429(11) 0.0890(16) 0.0808(15) 0.0285(13) 0.0012(10) 0.0211(10) C33 0.0409(13) 0.0348(13) 0.0456(14) 0.0007(10) 0.0129(11) 0.0003(10) O33 0.0645(13) 0.0360(10) 0.0942(16) -0.0073(10) 0.0205(12) -0.0105(9) O41 0.0402(10) 0.0576(12) 0.0629(12) -0.0071(9) 0.0128(9) 0.0101(9) C41 0.0323(11) 0.0368(12) 0.0334(12) 0.0011(10) -0.0053(9) 0.0011(9) O42 0.0512(10) 0.0543(11) 0.0423(10) -0.0093(9) -0.0062(8) -0.0084(9) C42 0.0348(11) 0.0437(13) 0.0284(11) 0.0048(10) 0.0029(9) 0.0029(10) C43 0.0488(14) 0.0452(14) 0.0344(12) 0.0142(11) -0.0015(11) -0.0044(11) O43 0.0982(17) 0.0672(14) 0.0652(14) 0.0380(12) 0.0033(12) -0.0223(12) C51 0.0216(9) 0.0271(10) 0.0218(9) 0.0064(7) 0.0017(7) -0.0004(7) C52 0.0219(9) 0.0291(10) 0.0232(9) 0.0084(8) 0.0039(7) 0.0031(7) C53 0.0208(9) 0.0310(10) 0.0200(9) 0.0089(8) 0.0014(7) -0.0026(7) C54 0.0197(9) 0.0314(10) 0.0223(9) 0.0078(8) 0.0003(7) -0.0033(7) C55 0.0265(10) 0.0336(11) 0.0303(10) 0.0074(9) 0.0037(8) 0.0067(8) C56 0.0364(11) 0.0279(10) 0.0306(11) 0.0049(9) 0.0025(9) 0.0047(9) C57 0.0364(11) 0.0278(10) 0.0256(10) 0.0061(8) 0.0007(8) -0.0034(8) C58 0.0474(13) 0.0362(12) 0.0273(10) 0.0140(9) -0.0016(9) -0.0150(10) C59 0.0306(11) 0.0482(13) 0.0262(10) 0.0126(10) 0.0023(8) -0.0137(9) C60 0.0230(9) 0.0309(10) 0.0200(9) 0.0071(8) 0.0023(7) 0.0002(8) C61 0.0226(9) 0.0292(10) 0.0191(9) 0.0045(8) 0.0045(7) 0.0035(7) C62 0.0221(9) 0.0277(10) 0.0227(9) 0.0046(8) 0.0056(7) -0.0012(7) C63 0.0217(9) 0.0288(10) 0.0214(9) 0.0038(8) 0.0021(7) 0.0013(7) _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 C11 1.792(2) . ? Co1 C12 1.816(2) . ? Co1 C13 1.828(3) . ? Co1 C53 1.9678(18) . ? Co1 C54 1.9757(19) . ? Co1 Co2 2.4785(4) . ? Co2 C22 1.783(2) . ? Co2 C23 1.817(3) . ? Co2 C21 1.829(2) . ? Co2 C54 1.9662(19) . ? Co2 C53 1.9675(19) . ? Co3 C32 1.783(3) . ? Co3 C31 1.820(2) . ? Co3 C33 1.827(2) . ? Co3 C60 1.9665(19) . ? Co3 C61 1.9698(19) . ? Co3 Co4 2.4798(4) . ? Co4 C41 1.787(2) . ? Co4 C42 1.818(2) . ? Co4 C43 1.829(3) . ? Co4 C61 1.9698(18) . ? Co4 C60 1.9717(19) . ? S50 C63 1.8107(19) . ? S50 C51 1.8130(19) . ? O11 C11 1.136(3) . ? C12 O12 1.126(3) . ? C13 O13 1.134(3) . ? C21 O21 1.132(3) . ? C22 O22 1.134(3) . ? C23 O23 1.137(3) . ? C31 O31 1.135(3) . ? C32 O32 1.143(3) . ? C33 O33 1.130(3) . ? O41 C41 1.137(3) . ? O42 C42 1.133(3) . ? C43 O43 1.129(3) . ? C51 C52 1.530(3) . ? C52 C53 1.499(3) . ? C53 C54 1.331(3) . ? C54 C55 1.500(3) . ? C55 C56 1.536(3) . ? C56 C57 1.529(3) . ? C57 C58 1.530(3) . ? C58 C59 1.529(3) . ? C59 C60 1.495(3) . ? C60 C61 1.337(3) . ? C61 C62 1.495(3) . ? C62 C63 1.533(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 C11 Co1 C12 98.22(11) . . ? C11 Co1 C13 101.43(11) . . ? C12 Co1 C13 107.14(11) . . ? C11 Co1 C53 104.30(9) . . ? C12 Co1 C53 141.00(10) . . ? C13 Co1 C53 99.15(10) . . ? C11 Co1 C54 97.68(9) . . ? C12 Co1 C54 106.73(10) . . ? C13 Co1 C54 137.93(10) . . ? C53 Co1 C54 39.44(8) . . ? C11 Co1 Co2 148.38(7) . . ? C12 Co1 Co2 94.92(8) . . ? C13 Co1 Co2 101.95(8) . . ? C53 Co1 Co2 50.96(5) . . ? C54 Co1 Co2 50.87(5) . . ? C22 Co2 C23 98.08(11) . . ? C22 Co2 C21 100.62(11) . . ? C23 Co2 C21 108.07(11) . . ? C22 Co2 C54 103.68(9) . . ? C23 Co2 C54 141.77(10) . . ? C21 Co2 C54 98.40(10) . . ? C22 Co2 C53 97.66(9) . . ? C23 Co2 C53 107.02(10) . . ? C21 Co2 C53 137.34(10) . . ? C54 Co2 C53 39.54(8) . . ? C22 Co2 Co1 148.39(8) . . ? C23 Co2 Co1 95.68(8) . . ? C21 Co2 Co1 101.92(8) . . ? C54 Co2 Co1 51.21(5) . . ? C53 Co2 Co1 50.97(5) . . ? C32 Co3 C31 99.23(11) . . ? C32 Co3 C33 100.86(11) . . ? C31 Co3 C33 107.46(11) . . ? C32 Co3 C60 102.66(10) . . ? C31 Co3 C60 141.27(10) . . ? C33 Co3 C60 99.32(9) . . ? C32 Co3 C61 97.73(10) . . ? C31 Co3 C61 106.06(9) . . ? C33 Co3 C61 138.16(9) . . ? C60 Co3 C61 39.72(8) . . ? C32 Co3 Co4 148.20(8) . . ? C31 Co3 Co4 95.80(8) . . ? C33 Co3 Co4 101.09(8) . . ? C60 Co3 Co4 51.07(5) . . ? C61 Co3 Co4 50.99(5) . . ? C41 Co4 C42 96.90(10) . . ? C41 Co4 C43 102.86(12) . . ? C42 Co4 C43 107.16(11) . . ? C41 Co4 C61 105.50(9) . . ? C42 Co4 C61 143.34(9) . . ? C43 Co4 C61 95.83(9) . . ? C41 Co4 C60 96.48(9) . . ? C42 Co4 C60 110.15(9) . . ? C43 Co4 C60 135.18(9) . . ? C61 Co4 C60 39.67(8) . . ? C41 Co4 Co3 147.35(7) . . ? C42 Co4 Co3 95.60(7) . . ? C43 Co4 Co3 102.02(8) . . ? C61 Co4 Co3 50.99(5) . . ? C60 Co4 Co3 50.88(6) . . ? C63 S50 C51 100.47(9) . . ? O11 C11 Co1 177.9(2) . . ? O12 C12 Co1 177.8(2) . . ? O13 C13 Co1 176.8(2) . . ? O21 C21 Co2 175.2(2) . . ? O22 C22 Co2 177.8(2) . . ? O23 C23 Co2 177.6(2) . . ? O31 C31 Co3 177.7(2) . . ? O32 C32 Co3 177.7(2) . . ? O33 C33 Co3 176.2(2) . . ? O41 C41 Co4 177.3(2) . . ? O42 C42 Co4 179.2(2) . . ? O43 C43 Co4 174.2(2) . . ? C52 C51 S50 114.75(13) . . ? C53 C52 C51 110.36(15) . . ? C54 C53 C52 142.93(18) . . ? C54 C53 Co2 70.17(12) . . ? C52 C53 Co2 134.92(13) . . ? C54 C53 Co1 70.60(11) . . ? C52 C53 Co1 132.32(14) . . ? Co2 C53 Co1 78.07(7) . . ? C53 C54 C55 145.27(18) . . ? C53 C54 Co2 70.28(12) . . ? C55 C54 Co2 133.94(15) . . ? C53 C54 Co1 69.96(11) . . ? C55 C54 Co1 131.37(14) . . ? Co2 C54 Co1 77.92(7) . . ? C54 C55 C56 113.74(17) . . ? C57 C56 C55 114.16(17) . . ? C56 C57 C58 111.64(17) . . ? C59 C58 C57 114.68(18) . . ? C60 C59 C58 113.75(17) . . ? C61 C60 C59 144.67(18) . . ? C61 C60 Co3 70.27(11) . . ? C59 C60 Co3 134.15(15) . . ? C61 C60 Co4 70.09(11) . . ? C59 C60 Co4 131.61(14) . . ? Co3 C60 Co4 78.05(7) . . ? C60 C61 C62 143.20(18) . . ? C60 C61 Co3 70.01(12) . . ? C62 C61 Co3 134.69(13) . . ? C60 C61 Co4 70.24(11) . . ? C62 C61 Co4 132.67(14) . . ? Co3 C61 Co4 78.02(7) . . ? C61 C62 C63 110.19(15) . . ? C62 C63 S50 114.61(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.395 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.068 #===END data_br12_11 _database_code_CSD 168770 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Co4 O12' _chemical_formula_weight 732.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6522(3) _cell_length_b 9.5811(3) _cell_length_c 9.9672(2) _cell_angle_alpha 92.300(2) _cell_angle_beta 98.9510(10) _cell_angle_gamma 104.5690(10) _cell_volume 696.24(4) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max .12 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 2.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 7216 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3174 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3174 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.012 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 0.86138(6) 0.72453(5) 0.80229(5) 0.02707(14) Uani 1 1 d . . . Co2 Co 0.60158(6) 0.83751(5) 0.75692(5) 0.02677(14) Uani 1 1 d . . . C1 C 0.6008(4) 0.7704(3) 0.3780(3) 0.0297(8) Uani 1 1 d . . . H1A H 0.5448 0.8489 0.4008 0.036 Uiso 1 1 calc R . . H1B H 0.6481 0.7911 0.2919 0.036 Uiso 1 1 calc R . . C2 C 0.7630(4) 0.7744(3) 0.4910(3) 0.0278(7) Uani 1 1 d . . . H2A H 0.8288 0.7044 0.4629 0.033 Uiso 1 1 calc R . . H2B H 0.8490 0.8721 0.5004 0.033 Uiso 1 1 calc R . . C3 C 0.7114(4) 0.7402(3) 0.6273(3) 0.0241(7) Uani 1 1 d . . . C4 C 0.6140(4) 0.6423(3) 0.6972(3) 0.0229(7) Uani 1 1 d . . . C5 C 0.4798(4) 0.4996(3) 0.6923(3) 0.0268(7) Uani 1 1 d . . . H5A H 0.3666 0.5005 0.6292 0.032 Uiso 1 1 calc R . . H5B H 0.4476 0.4852 0.7841 0.032 Uiso 1 1 calc R . . C6 C 0.5483(4) 0.3719(3) 0.6463(3) 0.0260(7) Uani 1 1 d . . . H6A H 0.5977 0.3926 0.5611 0.031 Uiso 1 1 calc R . . H6B H 0.6498 0.3614 0.7167 0.031 Uiso 1 1 calc R . . C11 C 0.8310(5) 0.6523(5) 0.9655(4) 0.0459(10) Uani 1 1 d . . . O11 O 0.8077(4) 0.6033(4) 1.0639(3) 0.0866(12) Uani 1 1 d . . . C12 C 0.9798(5) 0.6078(4) 0.7331(4) 0.0373(9) Uani 1 1 d . . . O12 O 1.0461(4) 0.5326(3) 0.6799(3) 0.0586(8) Uani 1 1 d . . . C13 C 1.0446(5) 0.8895(4) 0.8397(4) 0.0360(8) Uani 1 1 d . . . O13 O 1.1592(4) 0.9935(3) 0.8618(3) 0.0585(8) Uani 1 1 d . . . C21 C 0.5121(5) 0.8042(4) 0.9147(4) 0.0408(9) Uani 1 1 d . . . O21 O 0.4542(4) 0.7777(4) 1.0107(3) 0.0667(9) Uani 1 1 d . . . C22 C 0.7332(5) 1.0252(4) 0.7699(4) 0.0403(9) Uani 1 1 d . . . O22 O 0.8194(4) 1.1411(3) 0.7774(3) 0.0673(9) Uani 1 1 d . . . C23 C 0.3956(5) 0.8458(3) 0.6475(4) 0.0305(8) Uani 1 1 d . . . O23 O 0.2660(3) 0.8488(3) 0.5767(3) 0.0469(7) 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 0.0233(2) 0.0304(3) 0.0276(3) 0.0039(2) 0.0030(2) 0.00781(19) Co2 0.0268(2) 0.0229(3) 0.0313(3) -0.00216(19) 0.0036(2) 0.00906(19) C1 0.0365(19) 0.0215(17) 0.0282(19) 0.0054(14) 0.0003(15) 0.0050(14) C2 0.0272(17) 0.0226(17) 0.0304(19) 0.0026(14) 0.0055(15) 0.0003(14) C3 0.0223(16) 0.0220(17) 0.0299(19) -0.0006(14) 0.0045(14) 0.0096(13) C4 0.0225(15) 0.0215(17) 0.0251(17) 0.0022(13) 0.0025(13) 0.0077(13) C5 0.0287(17) 0.0225(17) 0.0291(19) 0.0026(14) 0.0106(15) 0.0031(14) C6 0.0305(17) 0.0216(17) 0.0247(18) 0.0023(13) 0.0022(14) 0.0063(14) C11 0.033(2) 0.062(3) 0.044(3) 0.017(2) 0.0077(19) 0.0131(19) O11 0.079(2) 0.134(3) 0.057(2) 0.056(2) 0.0235(18) 0.031(2) C12 0.0272(18) 0.039(2) 0.048(2) 0.0155(18) 0.0025(17) 0.0128(16) O12 0.0493(17) 0.0581(19) 0.081(2) 0.0037(16) 0.0193(16) 0.0329(15) C13 0.0312(19) 0.043(2) 0.034(2) 0.0015(17) 0.0042(16) 0.0107(17) O13 0.0400(15) 0.0482(18) 0.076(2) -0.0088(16) 0.0060(15) -0.0044(14) C21 0.040(2) 0.045(2) 0.039(2) -0.0063(18) 0.0063(18) 0.0152(18) O21 0.067(2) 0.098(3) 0.0420(19) 0.0074(17) 0.0240(16) 0.0251(18) C22 0.039(2) 0.028(2) 0.051(2) -0.0047(17) -0.0022(18) 0.0118(17) O22 0.0560(18) 0.0265(17) 0.108(3) -0.0023(16) -0.0103(18) 0.0048(14) C23 0.0317(18) 0.0215(18) 0.039(2) -0.0035(15) 0.0084(17) 0.0070(15) O23 0.0301(14) 0.0505(17) 0.0589(18) 0.0040(14) -0.0016(13) 0.0139(12) _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 C12 1.786(4) . ? Co1 C13 1.811(4) . ? Co1 C11 1.818(4) . ? Co1 C3 1.966(3) . ? Co1 C4 1.966(3) . ? Co1 Co2 2.4841(6) . ? Co2 C23 1.793(4) . ? Co2 C22 1.815(4) . ? Co2 C21 1.820(4) . ? Co2 C4 1.969(3) . ? Co2 C3 1.970(3) . ? C1 C6 1.524(4) 2_666 ? C1 C2 1.532(4) . ? C2 C3 1.500(4) . ? C3 C4 1.334(4) . ? C4 C5 1.483(4) . ? C5 C6 1.528(4) . ? C6 C1 1.525(4) 2_666 ? C11 O11 1.124(4) . ? C12 O12 1.138(4) . ? C13 O13 1.137(4) . ? C21 O21 1.127(4) . ? C22 O22 1.133(4) . ? C23 O23 1.131(4) . ? 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 C12 Co1 C13 100.02(16) . . ? C12 Co1 C11 101.83(17) . . ? C13 Co1 C11 106.06(17) . . ? C12 Co1 C3 95.11(15) . . ? C13 Co1 C3 107.40(14) . . ? C11 Co1 C3 138.94(15) . . ? C12 Co1 C4 99.64(15) . . ? C13 Co1 C4 142.97(14) . . ? C11 Co1 C4 100.17(15) . . ? C3 Co1 C4 39.67(13) . . ? C12 Co1 Co2 145.26(12) . . ? C13 Co1 Co2 97.80(11) . . ? C11 Co1 Co2 101.52(12) . . ? C3 Co1 Co2 50.94(9) . . ? C4 Co1 Co2 50.92(9) . . ? C23 Co2 C22 100.85(15) . . ? C23 Co2 C21 99.24(16) . . ? C22 Co2 C21 107.89(17) . . ? C23 Co2 C4 99.83(14) . . ? C22 Co2 C4 140.76(15) . . ? C21 Co2 C4 101.19(15) . . ? C23 Co2 C3 99.58(14) . . ? C22 Co2 C3 103.89(15) . . ? C21 Co2 C3 138.96(15) . . ? C4 Co2 C3 39.60(12) . . ? C23 Co2 Co1 148.12(11) . . ? C22 Co2 Co1 98.26(11) . . ? C21 Co2 Co1 98.85(12) . . ? C4 Co2 Co1 50.81(9) . . ? C3 Co2 Co1 50.80(9) . . ? C6 C1 C2 115.3(3) 2_666 . ? C3 C2 C1 114.5(3) . . ? C4 C3 C2 145.8(3) . . ? C4 C3 Co1 70.18(19) . . ? C2 C3 Co1 131.2(2) . . ? C4 C3 Co2 70.18(19) . . ? C2 C3 Co2 133.3(2) . . ? Co1 C3 Co2 78.27(12) . . ? C3 C4 C5 146.8(3) . . ? C3 C4 Co1 70.15(18) . . ? C5 C4 Co1 132.7(2) . . ? C3 C4 Co2 70.23(19) . . ? C5 C4 Co2 130.8(2) . . ? Co1 C4 Co2 78.27(11) . . ? C4 C5 C6 114.1(2) . . ? C1 C6 C5 113.0(3) 2_666 . ? O11 C11 Co1 177.5(4) . . ? O12 C12 Co1 174.8(3) . . ? O13 C13 Co1 179.3(4) . . ? O21 C21 Co2 177.2(4) . . ? O22 C22 Co2 178.2(3) . . ? O23 C23 Co2 178.6(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.452 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.086 #===END data_br25_12 _database_code_CSD 168771 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Co4 O12' _chemical_formula_weight 784.16 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 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 19.6831(5) _cell_length_b 7.6322(2) _cell_length_c 22.7230(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.9220(10) _cell_angle_gamma 90.00 _cell_volume 3166.74(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 2.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 15755 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3623 _reflns_number_gt 3258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0283P)^2^+2.2712P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3623 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.005 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 0.074701(11) 0.09505(3) 0.401279(9) 0.02349(6) Uani 1 1 d . . . Co2 Co 0.127264(11) 0.37629(3) 0.384622(9) 0.02312(6) Uani 1 1 d . . . C1 C 0.02974(8) 0.27456(18) 0.33585(6) 0.0211(3) Uani 1 1 d . . . C2 C 0.08124(8) 0.18952(18) 0.32232(6) 0.0209(3) Uani 1 1 d . . . C3 C 0.09977(9) 0.09841(19) 0.27199(7) 0.0243(3) Uani 1 1 d . . . H3A H 0.0626 0.0062 0.2531 0.029 Uiso 1 1 calc R . . H3B H 0.1475 0.0390 0.2926 0.029 Uiso 1 1 calc R . . C4 C 0.10428(8) 0.2112(2) 0.21843(7) 0.0245(3) Uani 1 1 d . . . C5 C -0.04566(8) 0.35051(19) 0.30706(7) 0.0245(3) Uani 1 1 d . . . H5A H -0.0478 0.4303 0.2721 0.029 Uiso 1 1 calc R . . H5B H -0.0558 0.4206 0.3395 0.029 Uiso 1 1 calc R . . C11 C 0.15936(10) -0.0279(2) 0.43490(8) 0.0376(4) Uani 1 1 d . . . O11 O 0.21286(9) -0.1035(2) 0.45338(9) 0.0673(5) Uani 1 1 d . . . C12 C 0.04812(11) 0.1592(2) 0.46698(8) 0.0386(4) Uani 1 1 d . . . O12 O 0.03168(11) 0.2004(2) 0.50746(8) 0.0681(5) Uani 1 1 d . . . C13 C 0.01302(10) -0.0862(2) 0.37180(8) 0.0322(3) Uani 1 1 d . . . O13 O -0.02482(8) -0.20218(18) 0.35332(7) 0.0503(4) Uani 1 1 d . . . C21 C 0.22303(10) 0.3129(2) 0.41035(8) 0.0381(4) Uani 1 1 d . . . O21 O 0.28181(8) 0.2692(3) 0.42419(9) 0.0677(5) Uani 1 1 d . . . C22 C 0.11539(10) 0.4951(2) 0.44956(8) 0.0358(4) Uani 1 1 d . . . O22 O 0.10601(10) 0.5704(2) 0.48867(7) 0.0604(4) Uani 1 1 d . . . C23 C 0.12705(10) 0.5628(2) 0.33710(8) 0.0316(3) Uani 1 1 d . . . O23 O 0.12642(9) 0.68302(17) 0.30786(7) 0.0526(4) Uani 1 1 d . . . C44 C 0.15395(10) 0.1776(3) 0.19275(8) 0.0390(4) Uani 1 1 d . . . C45 C 0.20977(13) 0.0319(4) 0.21576(12) 0.0653(7) Uani 1 1 d . . . H45A H 0.2488 0.0674 0.2555 0.098 Uiso 1 1 calc R . . H45B H 0.2308 0.0081 0.1837 0.098 Uiso 1 1 calc R . . H45C H 0.1859 -0.0741 0.2230 0.098 Uiso 1 1 calc R . . C46 C 0.15838(13) 0.2736(4) 0.13602(11) 0.0641(7) Uani 1 1 d . . . H46A H 0.1394 0.1983 0.0985 0.096 Uiso 1 1 calc R . . H46B H 0.2095 0.3036 0.1442 0.096 Uiso 1 1 calc R . . H46C H 0.1291 0.3811 0.1287 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.03018(12) 0.02342(11) 0.01676(10) 0.00265(7) 0.00861(8) -0.00159(8) Co2 0.02599(11) 0.02263(11) 0.01901(10) -0.00111(7) 0.00641(8) -0.00320(7) C1 0.0269(7) 0.0195(6) 0.0160(6) 0.0000(5) 0.0070(5) -0.0029(5) C2 0.0265(7) 0.0196(6) 0.0156(6) 0.0021(5) 0.0068(5) -0.0018(5) C3 0.0308(8) 0.0232(7) 0.0209(7) 0.0008(5) 0.0120(6) 0.0039(6) C4 0.0255(7) 0.0283(7) 0.0192(7) 0.0003(5) 0.0078(6) -0.0017(6) C5 0.0275(7) 0.0238(7) 0.0217(7) -0.0034(5) 0.0087(6) 0.0028(6) C11 0.0409(10) 0.0299(8) 0.0342(9) 0.0083(7) 0.0051(7) -0.0020(7) O11 0.0458(9) 0.0509(9) 0.0864(13) 0.0204(8) 0.0029(8) 0.0135(7) C12 0.0512(11) 0.0394(9) 0.0304(8) 0.0004(7) 0.0212(8) -0.0097(8) O12 0.1025(14) 0.0716(11) 0.0552(9) -0.0139(8) 0.0584(10) -0.0166(10) C13 0.0417(9) 0.0300(8) 0.0249(8) 0.0059(6) 0.0125(7) -0.0014(7) O13 0.0615(9) 0.0357(7) 0.0455(8) 0.0010(6) 0.0106(7) -0.0180(7) C21 0.0338(9) 0.0398(10) 0.0362(9) 0.0051(7) 0.0078(7) -0.0038(7) O21 0.0321(8) 0.0816(12) 0.0808(12) 0.0172(10) 0.0110(8) 0.0089(8) C22 0.0429(10) 0.0341(9) 0.0294(8) -0.0049(7) 0.0123(7) -0.0077(7) O22 0.0836(12) 0.0605(9) 0.0442(8) -0.0226(7) 0.0319(8) -0.0078(8) C23 0.0357(8) 0.0264(8) 0.0309(8) -0.0045(6) 0.0102(7) -0.0061(6) O23 0.0762(10) 0.0304(7) 0.0500(8) 0.0089(6) 0.0222(7) -0.0088(7) C44 0.0340(9) 0.0567(11) 0.0314(9) 0.0071(8) 0.0180(7) 0.0053(8) C45 0.0564(14) 0.0933(19) 0.0636(14) 0.0196(13) 0.0423(12) 0.0352(13) C46 0.0572(13) 0.103(2) 0.0475(12) 0.0227(13) 0.0371(11) 0.0102(13) _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 C13 1.7972(17) . ? Co1 C11 1.8138(19) . ? Co1 C12 1.8235(18) . ? Co1 C1 1.9718(14) . ? Co1 C2 1.9819(13) . ? Co1 Co2 2.4725(3) . ? Co2 C23 1.7857(17) . ? Co2 C21 1.8183(19) . ? Co2 C22 1.8200(17) . ? Co2 C2 1.9747(14) . ? Co2 C1 1.9817(14) . ? C1 C2 1.333(2) . ? C1 C5 1.497(2) . ? C2 C3 1.4953(19) . ? C3 C4 1.520(2) . ? C4 C44 1.337(2) . ? C4 C5 1.516(2) 2 ? C5 C4 1.516(2) 2 ? C11 O11 1.135(2) . ? C12 O12 1.128(2) . ? C13 O13 1.132(2) . ? C21 O21 1.130(2) . ? C22 O22 1.130(2) . ? C23 O23 1.130(2) . ? C44 C45 1.513(3) . ? C44 C46 1.513(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 C13 Co1 C11 98.36(8) . . ? C13 Co1 C12 98.71(8) . . ? C11 Co1 C12 107.06(9) . . ? C13 Co1 C1 101.73(7) . . ? C11 Co1 C1 139.47(7) . . ? C12 Co1 C1 104.22(7) . . ? C13 Co1 C2 101.88(6) . . ? C11 Co1 C2 102.09(7) . . ? C12 Co1 C2 141.17(7) . . ? C1 Co1 C2 39.39(6) . . ? C13 Co1 Co2 150.97(5) . . ? C11 Co1 Co2 98.18(6) . . ? C12 Co1 Co2 99.02(6) . . ? C1 Co1 Co2 51.47(4) . . ? C2 Co1 Co2 51.19(4) . . ? C23 Co2 C21 100.05(8) . . ? C23 Co2 C22 96.96(8) . . ? C21 Co2 C22 107.66(8) . . ? C23 Co2 C2 104.18(6) . . ? C21 Co2 C2 100.46(7) . . ? C22 Co2 C2 141.04(7) . . ? C23 Co2 C1 101.01(7) . . ? C21 Co2 C1 138.34(8) . . ? C22 Co2 C1 104.95(7) . . ? C2 Co2 C1 39.37(6) . . ? C23 Co2 Co1 151.39(5) . . ? C21 Co2 Co1 99.36(6) . . ? C22 Co2 Co1 96.94(6) . . ? C2 Co2 Co1 51.46(4) . . ? C1 Co2 Co1 51.11(4) . . ? C2 C1 C5 143.41(13) . . ? C2 C1 Co1 70.71(8) . . ? C5 C1 Co1 133.72(10) . . ? C2 C1 Co2 70.03(8) . . ? C5 C1 Co2 133.46(10) . . ? Co1 C1 Co2 77.42(5) . . ? C1 C2 C3 145.77(13) . . ? C1 C2 Co2 70.60(8) . . ? C3 C2 Co2 134.94(11) . . ? C1 C2 Co1 69.89(8) . . ? C3 C2 Co1 129.79(10) . . ? Co2 C2 Co1 77.35(5) . . ? C2 C3 C4 116.93(12) . . ? C44 C4 C5 122.94(14) . 2 ? C44 C4 C3 120.78(14) . . ? C5 C4 C3 116.06(12) 2 . ? C1 C5 C4 112.60(12) . 2 ? O11 C11 Co1 176.81(19) . . ? O12 C12 Co1 179.36(18) . . ? O13 C13 Co1 178.81(17) . . ? O21 C21 Co2 177.13(19) . . ? O22 C22 Co2 177.95(19) . . ? O23 C23 Co2 178.49(17) . . ? C4 C44 C45 123.03(16) . . ? C4 C44 C46 124.27(18) . . ? C45 C44 C46 112.64(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.301 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.056 #===END data_br30_13 _database_code_CSD 168772 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H10 Co4 O12 S' _chemical_formula_weight 722.07 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' '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 Monoclinic _symmetry_space_group_name_H-M C2/c 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 25.0971(6) _cell_length_b 7.7272(2) _cell_length_c 13.8406(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.6010(10) _cell_angle_gamma 90.00 _cell_volume 2558.46(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lamina _exptl_crystal_colour red _exptl_crystal_size_max .22 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 2.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 8932 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1832 _reflns_number_gt 1447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1832 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36690(2) 0.13823(6) 0.13319(4) 0.02681(17) Uani 1 1 d . . . Co2 Co 0.36813(2) 0.40637(6) 0.23090(4) 0.02744(17) Uani 1 1 d . . . S1 S 0.4976(2) 0.2723(7) 0.0554(5) 0.0301(13) Uani 0.50 1 d P A 1 C1 C 0.42621(14) 0.2277(4) 0.2524(3) 0.0233(9) Uani 1 1 d . . . C2 C 0.42502(14) 0.3172(4) 0.1696(3) 0.0234(9) Uani 1 1 d . A . C3 C 0.46101(17) 0.4040(5) 0.1171(3) 0.0271(9) Uani 1 1 d . . . H3A H 0.4394(13) 0.467(4) 0.063(2) 0.016(9) Uiso 1 1 d . . . H3B H 0.4896(15) 0.488(5) 0.166(3) 0.036(11) Uiso 1 1 d . . . C4 C 0.4991(10) 0.273(3) 0.0750(16) 0.035(8) Uiso 0.50 1 d P A 2 H4A H 0.4741 0.2054 0.0183 0.042 Uiso 0.50 1 calc PR A 2 H4B H 0.5241 0.3421 0.0470 0.042 Uiso 0.50 1 calc PR A 2 C5 C 0.53645(16) 0.1398(5) 0.1559(3) 0.0258(9) Uani 1 1 d . . . H5A H 0.5106(14) 0.059(4) 0.178(3) 0.028(10) Uiso 1 1 d . . . H5B H 0.5558(14) 0.064(5) 0.118(3) 0.041(11) Uiso 1 1 d . . . C15 C 0.40225(17) -0.0490(6) 0.1041(3) 0.0365(10) Uani 1 1 d . . . O15 O 0.42430(13) -0.1665(4) 0.0872(2) 0.0586(9) Uani 1 1 d . . . C16 C 0.31754(18) 0.0264(5) 0.1835(3) 0.0420(11) Uani 1 1 d . . . O16 O 0.28796(14) -0.0435(5) 0.2186(3) 0.0705(11) Uani 1 1 d . . . C17 C 0.32982(17) 0.2104(5) 0.0049(3) 0.0385(10) Uani 1 1 d . . . O17 O 0.30926(14) 0.2609(4) -0.0745(2) 0.0662(10) Uani 1 1 d . . . C25 C 0.40325(17) 0.5993(6) 0.2865(3) 0.0373(10) Uani 1 1 d . . . O25 O 0.42445(14) 0.7252(4) 0.3187(2) 0.0634(10) Uani 1 1 d . . . C26 C 0.34014(17) 0.3336(5) 0.3313(3) 0.0393(11) Uani 1 1 d . . . O26 O 0.32639(14) 0.2840(5) 0.3969(3) 0.0695(10) Uani 1 1 d . . . C27 C 0.31215(18) 0.5093(5) 0.1347(3) 0.0398(11) Uani 1 1 d . . . O27 O 0.27681(14) 0.5729(4) 0.0721(3) 0.0627(10) 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 0.0255(3) 0.0259(3) 0.0274(3) -0.0009(2) 0.0056(2) -0.0032(2) Co2 0.0262(3) 0.0262(3) 0.0315(3) 0.0002(2) 0.0110(2) 0.0038(2) S1 0.031(2) 0.037(2) 0.0232(19) 0.0043(15) 0.0082(16) 0.0082(9) C1 0.024(2) 0.019(2) 0.026(2) -0.0037(17) 0.0068(17) -0.0019(16) C2 0.026(2) 0.020(2) 0.024(2) -0.0040(17) 0.0060(18) 0.0029(16) C3 0.026(2) 0.028(2) 0.028(2) 0.007(2) 0.009(2) 0.0015(19) C5 0.028(2) 0.027(2) 0.023(2) -0.0028(18) 0.0092(18) -0.0016(19) C15 0.040(3) 0.037(3) 0.031(2) -0.007(2) 0.009(2) -0.012(2) O15 0.062(2) 0.0391(19) 0.077(2) -0.0215(17) 0.0239(19) 0.0037(17) C16 0.038(3) 0.043(3) 0.041(3) -0.001(2) 0.006(2) -0.007(2) O16 0.059(2) 0.077(3) 0.084(3) 0.006(2) 0.033(2) -0.027(2) C17 0.039(3) 0.035(2) 0.037(3) -0.003(2) 0.006(2) -0.003(2) O17 0.082(3) 0.069(2) 0.0338(19) 0.0088(18) -0.0034(18) 0.0028(19) C25 0.040(3) 0.035(3) 0.037(3) 0.003(2) 0.011(2) 0.012(2) O25 0.076(2) 0.0326(19) 0.068(2) -0.0155(17) 0.0020(19) -0.0041(18) C26 0.034(2) 0.039(3) 0.046(3) 0.002(2) 0.015(2) 0.008(2) O26 0.068(2) 0.094(3) 0.060(2) 0.026(2) 0.040(2) 0.012(2) C27 0.041(3) 0.035(3) 0.045(3) -0.001(2) 0.016(2) 0.005(2) O27 0.051(2) 0.064(2) 0.063(2) 0.0113(18) 0.0024(18) 0.0212(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 Co1 C15 1.805(5) . ? Co1 C16 1.813(5) . ? Co1 C17 1.825(4) . ? Co1 C2 1.962(3) . ? Co1 C1 1.983(3) . ? Co1 Co2 2.4693(7) . ? Co2 C25 1.784(5) . ? Co2 C27 1.802(5) . ? Co2 C26 1.825(5) . ? Co2 C1 1.964(3) . ? Co2 C2 1.991(3) . ? S1 C3 1.755(7) . ? S1 C5 1.766(7) . ? C1 C2 1.331(5) . ? C1 C5 1.493(5) 2_655 ? C2 C3 1.481(5) . ? C3 C4 1.62(2) . ? C4 C5 1.60(2) . ? C5 C1 1.493(5) 2_655 ? C15 O15 1.124(5) . ? C16 O16 1.139(5) . ? C17 O17 1.133(4) . ? C25 O25 1.133(5) . ? C26 O26 1.131(5) . ? C27 O27 1.146(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Co1 C16 98.18(19) . . ? C15 Co1 C17 99.68(18) . . ? C16 Co1 C17 108.22(18) . . ? C15 Co1 C2 104.18(16) . . ? C16 Co1 C2 141.12(17) . . ? C17 Co1 C2 98.95(16) . . ? C15 Co1 C1 99.74(16) . . ? C16 Co1 C1 105.95(17) . . ? C17 Co1 C1 137.47(16) . . ? C2 Co1 C1 39.44(13) . . ? C15 Co1 Co2 150.35(13) . . ? C16 Co1 Co2 94.97(14) . . ? C17 Co1 Co2 101.24(13) . . ? C2 Co1 Co2 51.87(10) . . ? C1 Co1 Co2 50.93(10) . . ? C25 Co2 C27 97.07(18) . . ? C25 Co2 C26 100.54(19) . . ? C27 Co2 C26 107.76(18) . . ? C25 Co2 C1 105.96(16) . . ? C27 Co2 C1 143.06(17) . . ? C26 Co2 C1 96.13(16) . . ? C25 Co2 C2 98.55(16) . . ? C27 Co2 C2 109.70(17) . . ? C26 Co2 C2 135.10(16) . . ? C1 Co2 C2 39.32(13) . . ? C25 Co2 Co1 149.36(13) . . ? C27 Co2 Co1 95.03(13) . . ? C26 Co2 Co1 102.39(13) . . ? C1 Co2 Co1 51.61(10) . . ? C2 Co2 Co1 50.81(10) . . ? C3 S1 C5 101.4(4) . . ? C2 C1 C5 144.4(3) . 2_655 ? C2 C1 Co2 71.4(2) . . ? C5 C1 Co2 134.0(3) 2_655 . ? C2 C1 Co1 69.4(2) . . ? C5 C1 Co1 132.0(3) 2_655 . ? Co2 C1 Co1 77.46(13) . . ? C1 C2 C3 143.1(3) . . ? C1 C2 Co1 71.1(2) . . ? C3 C2 Co1 135.2(3) . . ? C1 C2 Co2 69.2(2) . . ? C3 C2 Co2 132.4(3) . . ? Co1 C2 Co2 77.31(13) . . ? C2 C3 C4 114.0(9) . . ? C2 C3 S1 117.5(3) . . ? C4 C3 S1 7.6(9) . . ? C5 C4 C3 115.9(13) . . ? C1 C5 C4 112.8(9) 2_655 . ? C1 C5 S1 117.4(3) 2_655 . ? C4 C5 S1 6.9(10) . . ? O15 C15 Co1 179.1(4) . . ? O16 C16 Co1 177.4(4) . . ? O17 C17 Co1 176.2(4) . . ? O25 C25 Co2 177.4(4) . . ? O26 C26 Co2 175.2(4) . . ? O27 C27 Co2 178.7(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.364 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.073 #===END data_br35_14 _database_code_CSD 168773 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H12 Co4 O12' _chemical_formula_weight 704.04 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 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 24.9890(5) _cell_length_b 7.7330(2) _cell_length_c 13.7310(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.5170(10) _cell_angle_gamma 90.00 _cell_volume 2530.33(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max .30 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 10986 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2885 _reflns_number_gt 2548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0312P)^2^+1.4747P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2885 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.130877(9) 0.90316(3) 0.268897(17) 0.02305(7) Uani 1 1 d . . . Co2 Co 0.132447(9) 0.63297(3) 0.365431(17) 0.02295(7) Uani 1 1 d . . . C1 C 0.07395(6) 0.8117(2) 0.33006(12) 0.0204(3) Uani 1 1 d . . . C2 C 0.07257(6) 0.7240(2) 0.24574(12) 0.0198(3) Uani 1 1 d . . . C3 C 0.03455(7) 0.6403(2) 0.15261(12) 0.0219(3) Uani 1 1 d . . . H3A H 0.0099 0.5580 0.1739 0.026 Uiso 1 1 calc R . . H3B H 0.0577 0.5728 0.1190 0.026 Uiso 1 1 calc R . . C4 C -0.00225(7) 0.7657(2) 0.07435(12) 0.0243(3) Uani 1 1 d . . . H4A H -0.0279 0.6968 0.0189 0.029 Uiso 1 1 calc R . . H4B H 0.0224 0.8331 0.0439 0.029 Uiso 1 1 calc R . . C5 C 0.03780(7) 0.8935(2) 0.38577(13) 0.0228(3) Uani 1 1 d . . . H5A H 0.0124 0.9770 0.3396 0.027 Uiso 1 1 calc R . . H5B H 0.0620 0.9595 0.4443 0.027 Uiso 1 1 calc R . . C11 C 0.16023(8) 0.8306(3) 0.16869(16) 0.0367(4) Uani 1 1 d . . . O11 O 0.17419(7) 0.7808(3) 0.10360(13) 0.0641(5) Uani 1 1 d . . . C12 C 0.18710(8) 1.0073(3) 0.36728(16) 0.0348(4) Uani 1 1 d . . . O12 O 0.22218(7) 1.0712(2) 0.42897(13) 0.0565(4) Uani 1 1 d . . . C13 C 0.09640(8) 1.0958(2) 0.21226(15) 0.0326(4) Uani 1 1 d . . . O13 O 0.07452(7) 1.22073(19) 0.17772(12) 0.0531(4) Uani 1 1 d . . . C21 C 0.16981(8) 0.7064(3) 0.49450(15) 0.0361(4) Uani 1 1 d . . . O21 O 0.19055(8) 0.7562(3) 0.57404(12) 0.0635(5) Uani 1 1 d . . . C22 C 0.18244(8) 0.5232(3) 0.31436(16) 0.0374(4) Uani 1 1 d . . . O22 O 0.21226(7) 0.4556(3) 0.27972(15) 0.0662(5) Uani 1 1 d . . . C23 C 0.09795(8) 0.4453(2) 0.39400(15) 0.0321(4) Uani 1 1 d . . . O23 O 0.07599(7) 0.3260(2) 0.41084(13) 0.0509(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 0.01780(12) 0.02472(13) 0.02720(13) -0.00022(9) 0.00761(9) -0.00323(8) Co2 0.01796(12) 0.02416(12) 0.02496(13) 0.00099(9) 0.00377(9) 0.00340(8) C1 0.0162(7) 0.0199(7) 0.0248(8) 0.0018(6) 0.0057(6) 0.0001(6) C2 0.0161(7) 0.0196(7) 0.0235(8) 0.0025(6) 0.0057(6) 0.0010(6) C3 0.0201(8) 0.0225(8) 0.0236(8) -0.0020(6) 0.0070(6) 0.0002(6) C4 0.0215(8) 0.0317(9) 0.0203(8) 0.0021(7) 0.0070(6) 0.0012(6) C5 0.0205(8) 0.0233(8) 0.0248(8) -0.0053(6) 0.0072(6) -0.0007(6) C11 0.0269(9) 0.0470(11) 0.0392(11) -0.0039(9) 0.0146(8) -0.0072(8) O11 0.0565(11) 0.0928(14) 0.0555(11) -0.0224(10) 0.0355(9) -0.0116(10) C12 0.0282(9) 0.0347(10) 0.0415(11) 0.0009(8) 0.0103(8) -0.0047(8) O12 0.0418(9) 0.0616(10) 0.0548(10) -0.0119(8) -0.0025(8) -0.0196(8) C13 0.0318(9) 0.0325(10) 0.0307(10) 0.0017(8) 0.0053(7) -0.0095(8) O13 0.0614(10) 0.0328(8) 0.0529(10) 0.0123(7) -0.0015(8) 0.0019(7) C21 0.0335(10) 0.0370(10) 0.0339(11) 0.0027(8) 0.0040(8) 0.0026(8) O21 0.0738(12) 0.0688(12) 0.0331(9) -0.0091(8) -0.0063(8) -0.0042(9) C22 0.0274(9) 0.0401(11) 0.0423(11) 0.0000(9) 0.0071(8) 0.0084(8) O22 0.0501(10) 0.0773(12) 0.0779(13) -0.0099(11) 0.0293(9) 0.0267(9) C23 0.0307(9) 0.0302(9) 0.0337(10) 0.0049(8) 0.0072(8) 0.0069(7) O23 0.0528(10) 0.0347(8) 0.0681(11) 0.0158(8) 0.0225(8) -0.0016(7) _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 C13 1.779(2) . ? Co1 C12 1.8180(19) . ? Co1 C11 1.831(2) . ? Co1 C2 1.9658(15) . ? Co1 C1 1.9869(16) . ? Co1 Co2 2.4683(3) . ? Co2 C23 1.791(2) . ? Co2 C22 1.817(2) . ? Co2 C21 1.827(2) . ? Co2 C1 1.9636(15) . ? Co2 C2 1.9887(15) . ? C1 C2 1.333(2) . ? C1 C5 1.489(2) . ? C2 C3 1.492(2) . ? C3 C4 1.532(2) . ? C4 C5 1.536(2) 2 ? C5 C4 1.536(2) 2 ? C11 O11 1.121(2) . ? C12 O12 1.133(2) . ? C13 O13 1.141(2) . ? C21 O21 1.127(2) . ? C22 O22 1.126(3) . ? C23 O23 1.132(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 C13 Co1 C12 96.79(8) . . ? C13 Co1 C11 100.31(9) . . ? C12 Co1 C11 107.41(9) . . ? C13 Co1 C2 106.36(7) . . ? C12 Co1 C2 143.30(8) . . ? C11 Co1 C2 96.18(8) . . ? C13 Co1 C1 99.72(8) . . ? C12 Co1 C1 109.57(8) . . ? C11 Co1 C1 135.09(8) . . ? C2 Co1 C1 39.42(6) . . ? C13 Co1 Co2 150.60(6) . . ? C12 Co1 Co2 95.28(6) . . ? C11 Co1 Co2 101.48(7) . . ? C2 Co1 Co2 51.80(4) . . ? C1 Co1 Co2 50.91(4) . . ? C23 Co2 C22 97.93(9) . . ? C23 Co2 C21 100.28(9) . . ? C22 Co2 C21 108.03(9) . . ? C23 Co2 C1 104.66(7) . . ? C22 Co2 C1 141.32(8) . . ? C21 Co2 C1 98.41(8) . . ? C23 Co2 C2 100.13(7) . . ? C22 Co2 C2 106.27(8) . . ? C21 Co2 C2 136.83(8) . . ? C1 Co2 C2 39.42(6) . . ? C23 Co2 Co1 150.78(6) . . ? C22 Co2 Co1 95.16(7) . . ? C21 Co2 Co1 100.30(6) . . ? C1 Co2 Co1 51.76(5) . . ? C2 Co2 Co1 50.97(4) . . ? C2 C1 C5 143.22(14) . . ? C2 C1 Co2 71.31(9) . . ? C5 C1 Co2 133.91(12) . . ? C2 C1 Co1 69.44(9) . . ? C5 C1 Co1 133.48(12) . . ? Co2 C1 Co1 77.33(6) . . ? C1 C2 C3 143.95(14) . . ? C1 C2 Co1 71.14(9) . . ? C3 C2 Co1 133.96(12) . . ? C1 C2 Co2 69.27(9) . . ? C3 C2 Co2 132.96(11) . . ? Co1 C2 Co2 77.24(6) . . ? C2 C3 C4 114.83(13) . . ? C3 C4 C5 116.53(13) . 2 ? C1 C5 C4 114.54(13) . 2 ? O11 C11 Co1 174.55(18) . . ? O12 C12 Co1 179.5(2) . . ? O13 C13 Co1 178.72(19) . . ? O21 C21 Co2 176.6(2) . . ? O22 C22 Co2 177.8(2) . . ? O23 C23 Co2 179.16(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.420 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.060 #===END data_br15_15 _database_code_CSD 168774 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H8 Co4 O12 S2' _chemical_formula_weight 740.10 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 Monoclinic _symmetry_space_group_name_H-M C2/c 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 25.13270(10) _cell_length_b 7.71950(10) _cell_length_c 13.88680(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.51 _cell_angle_gamma 90.00 _cell_volume 2569.41(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lamina _exptl_crystal_colour dark_red _exptl_crystal_size_max .70 _exptl_crystal_size_mid .44 _exptl_crystal_size_min .02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 2.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 12658 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2929 _reflns_number_gt 2651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0353P)^2^+1.6022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2929 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.010 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 0.366903(9) 0.41204(3) 0.730442(17) 0.02279(8) Uani 1 1 d . . . Co2 Co 0.366299(9) 0.14605(3) 0.631549(17) 0.02228(8) Uani 1 1 d . . . S1 S 0.501610(18) 0.28091(6) 0.94289(3) 0.02649(11) Uani 1 1 d . . . C1 C 0.42353(7) 0.3263(2) 0.66891(12) 0.0201(3) Uani 1 1 d . . . C2 C 0.42484(7) 0.2341(2) 0.75138(12) 0.0199(3) Uani 1 1 d . . . C3 C 0.46152(7) 0.1427(2) 0.84079(12) 0.0218(3) Uani 1 1 d . . . H3A H 0.4408(9) 0.070(3) 0.8738(16) 0.025(5) Uiso 1 1 d . . . H3B H 0.4877(9) 0.069(3) 0.8203(15) 0.025(5) Uiso 1 1 d . . . C4 C 0.54100(7) 0.4188(2) 0.88304(13) 0.0233(3) Uani 1 1 d . . . H4A H 0.5146(8) 0.496(3) 0.8354(15) 0.025(5) Uiso 1 1 d . . . H4B H 0.5631(8) 0.490(3) 0.9378(15) 0.022(5) Uiso 1 1 d . . . C15 C 0.40138(8) 0.6074(3) 0.78373(15) 0.0321(4) Uani 1 1 d . . . O15 O 0.42313(8) 0.7337(2) 0.81412(14) 0.0560(5) Uani 1 1 d . . . C16 C 0.33986(9) 0.3390(3) 0.83200(17) 0.0365(4) Uani 1 1 d . . . O16 O 0.32735(8) 0.2895(3) 0.89845(15) 0.0633(5) Uani 1 1 d . . . C17 C 0.30972(8) 0.5127(3) 0.63445(16) 0.0347(4) Uani 1 1 d . . . O17 O 0.27415(7) 0.5743(3) 0.57331(14) 0.0572(5) Uani 1 1 d . . . C25 C 0.40177(8) -0.0376(3) 0.60163(15) 0.0322(4) Uani 1 1 d . . . O25 O 0.42455(8) -0.1553(2) 0.58471(15) 0.0535(4) Uani 1 1 d . . . C26 C 0.32900(9) 0.2186(3) 0.50381(15) 0.0352(4) Uani 1 1 d . . . O26 O 0.30837(9) 0.2664(3) 0.42449(13) 0.0611(5) Uani 1 1 d . . . C27 C 0.31762(8) 0.0304(3) 0.68176(16) 0.0360(4) Uani 1 1 d . . . O27 O 0.28858(7) -0.0404(3) 0.71671(16) 0.0615(5) 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 0.01953(13) 0.02262(13) 0.02722(13) -0.00071(9) 0.00856(10) 0.00295(8) Co2 0.01868(13) 0.02252(13) 0.02410(13) -0.00187(9) 0.00410(9) -0.00209(8) S1 0.0247(2) 0.0362(2) 0.0198(2) -0.00431(17) 0.00866(16) -0.00619(17) C1 0.0178(7) 0.0189(7) 0.0230(8) -0.0027(6) 0.0053(6) -0.0001(6) C2 0.0176(7) 0.0189(7) 0.0232(7) -0.0034(6) 0.0059(6) -0.0012(6) C3 0.0220(8) 0.0215(8) 0.0217(7) 0.0006(6) 0.0064(6) -0.0011(6) C4 0.0209(8) 0.0230(8) 0.0269(8) -0.0045(7) 0.0087(7) -0.0028(6) C15 0.0338(10) 0.0278(9) 0.0313(9) -0.0025(7) 0.0045(8) 0.0070(8) O15 0.0683(12) 0.0313(8) 0.0538(10) -0.0100(7) -0.0040(8) -0.0050(8) C16 0.0315(10) 0.0405(11) 0.0421(11) 0.0027(9) 0.0179(9) 0.0072(8) O16 0.0599(11) 0.0858(15) 0.0575(11) 0.0225(10) 0.0376(9) 0.0115(10) C17 0.0303(10) 0.0317(10) 0.0421(11) -0.0022(9) 0.0108(9) 0.0055(8) O17 0.0442(10) 0.0590(11) 0.0568(10) 0.0074(9) -0.0023(8) 0.0213(8) C25 0.0301(9) 0.0308(9) 0.0346(9) -0.0075(8) 0.0080(8) -0.0059(8) O25 0.0553(11) 0.0368(9) 0.0723(12) -0.0186(8) 0.0254(9) 0.0031(7) C26 0.0329(10) 0.0359(10) 0.0324(10) -0.0019(8) 0.0032(8) -0.0028(8) O26 0.0715(13) 0.0641(12) 0.0343(9) 0.0097(8) -0.0045(8) 0.0031(10) C27 0.0288(9) 0.0354(10) 0.0412(10) -0.0014(9) 0.0067(8) -0.0060(8) O27 0.0474(10) 0.0679(12) 0.0759(12) 0.0089(10) 0.0284(9) -0.0214(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 Co1 C15 1.786(2) . ? Co1 C17 1.815(2) . ? Co1 C16 1.829(2) . ? Co1 C2 1.9587(16) . ? Co1 C1 1.9811(16) . ? Co1 Co2 2.4677(3) . ? Co2 C25 1.789(2) . ? Co2 C27 1.815(2) . ? Co2 C26 1.827(2) . ? Co2 C1 1.9560(16) . ? Co2 C2 1.9805(16) . ? S1 C4 1.8163(18) . ? S1 C3 1.8181(17) . ? C1 C2 1.340(2) . ? C1 C4 1.487(2) 2_656 ? C2 C3 1.484(2) . ? C4 C1 1.487(2) 2_656 ? C15 O15 1.135(3) . ? C16 O16 1.127(3) . ? C17 O17 1.135(3) . ? C25 O25 1.135(3) . ? C26 O26 1.129(3) . ? C27 O27 1.132(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 C15 Co1 C17 96.95(9) . . ? C15 Co1 C16 100.81(10) . . ? C17 Co1 C16 107.61(9) . . ? C15 Co1 C2 106.53(8) . . ? C17 Co1 C2 142.98(8) . . ? C16 Co1 C2 95.82(8) . . ? C15 Co1 C1 97.98(8) . . ? C17 Co1 C1 109.82(8) . . ? C16 Co1 C1 135.34(8) . . ? C2 Co1 C1 39.78(7) . . ? C15 Co1 Co2 148.71(7) . . ? C17 Co1 Co2 94.40(6) . . ? C16 Co1 Co2 103.35(7) . . ? C2 Co1 Co2 51.61(5) . . ? C1 Co1 Co2 50.73(5) . . ? C25 Co2 C27 98.06(9) . . ? C25 Co2 C26 99.41(9) . . ? C27 Co2 C26 108.39(9) . . ? C25 Co2 C1 104.33(8) . . ? C27 Co2 C1 140.81(8) . . ? C26 Co2 C1 99.26(8) . . ? C25 Co2 C2 99.85(8) . . ? C27 Co2 C2 105.20(8) . . ? C26 Co2 C2 138.15(8) . . ? C1 Co2 C2 39.81(7) . . ? C25 Co2 Co1 150.30(6) . . ? C27 Co2 Co1 95.01(7) . . ? C26 Co2 Co1 101.57(7) . . ? C1 Co2 Co1 51.64(5) . . ? C2 Co2 Co1 50.82(5) . . ? C4 S1 C3 103.74(8) . . ? C2 C1 C4 143.62(15) . 2_656 ? C2 C1 Co2 71.08(10) . . ? C4 C1 Co2 135.49(12) 2_656 . ? C2 C1 Co1 69.21(9) . . ? C4 C1 Co1 131.48(12) 2_656 . ? Co2 C1 Co1 77.63(6) . . ? C1 C2 C3 144.80(15) . . ? C1 C2 Co1 71.01(10) . . ? C3 C2 Co1 134.82(12) . . ? C1 C2 Co2 69.11(10) . . ? C3 C2 Co2 131.10(12) . . ? Co1 C2 Co2 77.57(6) . . ? C2 C3 S1 115.62(12) . . ? C1 C4 S1 115.45(12) 2_656 . ? O15 C15 Co1 177.5(2) . . ? O16 C16 Co1 174.5(2) . . ? O17 C17 Co1 179.0(2) . . ? O25 C25 Co2 178.5(2) . . ? O26 C26 Co2 176.6(2) . . ? O27 C27 Co2 177.3(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.399 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.068 #===END data_ramm2_17 _database_code_CSD 168775 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H14 Co4 O12' _chemical_formula_weight 778.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.830(4) _cell_length_b 12.886(5) _cell_length_c 16.209(6) _cell_angle_alpha 91.32(3) _cell_angle_beta 102.09(3) _cell_angle_gamma 105.68(3) _cell_volume 1534.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rod' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max .70 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 2.185 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4787 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 23.99 _reflns_number_total 4787 _reflns_number_gt 3391 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+1.7109P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4787 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.007 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 0.97683(11) 1.31840(6) 0.37180(5) 0.0567(2) Uani 1 1 d . . . C1 C 0.9443(10) 1.4516(6) 0.3646(5) 0.085(2) Uani 1 1 d . . . O1 O 0.9241(9) 1.5343(5) 0.3581(5) 0.144(3) Uani 1 1 d . . . C2 C 1.1460(10) 1.3261(6) 0.4671(5) 0.082(2) Uani 1 1 d . . . O2 O 1.2504(8) 1.3277(5) 0.5272(4) 0.128(2) Uani 1 1 d . . . C3 C 1.1091(10) 1.3262(5) 0.2938(5) 0.081(2) Uani 1 1 d . . . O3 O 1.1881(10) 1.3317(5) 0.2434(5) 0.135(3) Uani 1 1 d . . . Co2 Co 0.69889(10) 1.22743(6) 0.41919(5) 0.0534(2) Uani 1 1 d . . . C4 C 0.4964(9) 1.1205(6) 0.4092(4) 0.0718(18) Uani 1 1 d . . . O4 O 0.3657(7) 1.0504(5) 0.4043(4) 0.111(2) Uani 1 1 d . . . C5 C 0.8007(9) 1.2196(5) 0.5287(5) 0.0666(17) Uani 1 1 d . . . O5 O 0.8679(8) 1.2110(5) 0.5961(3) 0.1020(18) Uani 1 1 d . . . C6 C 0.6039(9) 1.3416(6) 0.4157(5) 0.083(2) Uani 1 1 d . . . O6 O 0.5463(8) 1.4117(5) 0.4122(5) 0.146(3) Uani 1 1 d . . . Co3 Co 0.48266(12) 0.76200(6) 0.08501(5) 0.0606(3) Uani 1 1 d . . . C7 C 0.6227(14) 0.6935(7) 0.0441(5) 0.101(3) Uani 1 1 d . . . O7 O 0.7114(13) 0.6486(7) 0.0196(5) 0.167(4) Uani 1 1 d . . . C8 C 0.2688(12) 0.7381(5) 0.0077(5) 0.080(2) Uani 1 1 d . . . O8 O 0.1330(9) 0.7289(5) -0.0367(4) 0.123(2) Uani 1 1 d . . . C9 C 0.5955(9) 0.8968(6) 0.0662(4) 0.0694(18) Uani 1 1 d . . . O9 O 0.6721(7) 0.9827(4) 0.0580(3) 0.0902(15) Uani 1 1 d . . . Co4 Co 0.39818(12) 0.63256(6) 0.19027(5) 0.0638(3) Uani 1 1 d . . . C10 C 0.5380(13) 0.5442(6) 0.1796(5) 0.095(2) Uani 1 1 d . . . O10 O 0.6237(12) 0.4890(6) 0.1740(5) 0.156(3) Uani 1 1 d . . . C11 C 0.3743(9) 0.6118(5) 0.2952(5) 0.0700(18) Uani 1 1 d . . . O11 O 0.3561(7) 0.6009(4) 0.3629(4) 0.0914(16) Uani 1 1 d . . . C12 C 0.1715(13) 0.5598(6) 0.1339(5) 0.098(3) Uani 1 1 d . . . O12 O 0.0254(10) 0.5192(6) 0.1001(5) 0.154(3) Uani 1 1 d . . . C13 C 0.7525(7) 1.2163(4) 0.3074(4) 0.0503(14) Uani 1 1 d . . . C14 C 0.8461(7) 1.1640(4) 0.3603(4) 0.0499(14) Uani 1 1 d . . . C15 C 0.9112(8) 1.0640(5) 0.3668(4) 0.0656(17) Uani 1 1 d . . . H15A H 0.9317 1.0446 0.3123 0.080 Uiso 1 1 calc R . . H15B H 1.0271 1.0808 0.4074 0.080 Uiso 1 1 calc R . . C16 C 0.7874(9) 0.9715(5) 0.3920(4) 0.0702(18) Uani 1 1 d . . . H16 H 0.7545 0.9811 0.4429 0.080 Uiso 1 1 calc R . . C17 C 0.7150(9) 0.8731(5) 0.3497(4) 0.075(2) Uani 1 1 d . . . H17 H 0.6381 0.8226 0.3754 0.080 Uiso 1 1 calc R . . C18 C 0.7405(8) 0.8347(5) 0.2688(4) 0.0668(17) Uani 1 1 d . . . H18A H 0.8124 0.7838 0.2787 0.080 Uiso 1 1 calc R . . H18B H 0.8071 0.8954 0.2432 0.080 Uiso 1 1 calc R . . C19 C 0.5617(8) 0.7808(4) 0.2090(4) 0.0541(15) Uani 1 1 d . . . C20 C 0.3915(8) 0.7834(4) 0.1862(4) 0.0522(14) Uani 1 1 d . . . C21 C 0.2537(8) 0.8346(5) 0.2052(4) 0.0619(16) Uani 1 1 d . . . H21A H 0.2568 0.8334 0.2653 0.080 Uiso 1 1 calc R . . H21B H 0.1340 0.7913 0.1751 0.080 Uiso 1 1 calc R . . C22 C 0.2794(8) 0.9495(4) 0.1819(4) 0.0525(14) Uani 1 1 d . . . C23 C 0.1383(8) 0.9815(6) 0.1354(4) 0.0729(19) Uani 1 1 d . . . H23 H 0.0258 0.9308 0.1158 0.080 Uiso 1 1 calc R . . C24 C 0.1599(10) 1.0872(6) 0.1171(5) 0.090(2) Uani 1 1 d . . . H24 H 0.0621 1.1077 0.0858 0.080 Uiso 1 1 calc R . . C25 C 0.3238(10) 1.1619(5) 0.1446(4) 0.0683(18) Uani 1 1 d . . . H25 H 0.3368 1.2333 0.1321 0.080 Uiso 1 1 calc R . . C26 C 0.4709(8) 1.1337(4) 0.1905(3) 0.0500(14) Uani 1 1 d . . . C27 C 0.4459(8) 1.0264(5) 0.2087(4) 0.0543(15) Uani 1 1 d . . . H27 H 0.5437 1.0059 0.2397 0.080 Uiso 1 1 calc R . . C28 C 0.6551(9) 1.2152(5) 0.2169(4) 0.0693(18) Uani 1 1 d . . . H28A H 0.7316 1.2012 0.1805 0.080 Uiso 1 1 calc R . . H28B H 0.6405 1.2867 0.2075 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0498(5) 0.0481(5) 0.0657(6) -0.0038(4) 0.0188(4) -0.0007(4) C1 0.071(5) 0.054(4) 0.126(7) -0.009(4) 0.039(5) -0.003(4) O1 0.131(5) 0.057(3) 0.257(9) 0.009(4) 0.076(6) 0.024(4) C2 0.056(4) 0.085(5) 0.085(6) 0.003(4) 0.011(4) -0.007(4) O2 0.081(4) 0.147(6) 0.117(5) 0.030(4) -0.014(4) -0.007(4) C3 0.076(5) 0.054(4) 0.111(6) -0.009(4) 0.043(5) -0.002(3) O3 0.164(6) 0.100(4) 0.163(6) -0.002(4) 0.123(5) 0.010(4) Co2 0.0456(5) 0.0517(5) 0.0613(5) 0.0028(4) 0.0168(4) 0.0073(4) C4 0.060(4) 0.082(5) 0.072(5) 0.007(4) 0.023(4) 0.011(4) O4 0.074(4) 0.108(4) 0.132(5) 0.000(4) 0.042(3) -0.022(3) C5 0.066(4) 0.067(4) 0.064(5) 0.001(4) 0.023(4) 0.007(3) O5 0.104(4) 0.124(5) 0.062(3) 0.014(3) 0.010(3) 0.013(3) C6 0.058(4) 0.082(5) 0.121(7) 0.020(5) 0.037(4) 0.024(4) O6 0.104(5) 0.099(4) 0.275(9) 0.043(5) 0.081(5) 0.065(4) Co3 0.0731(6) 0.0510(5) 0.0584(5) 0.0089(4) 0.0139(4) 0.0188(4) C7 0.144(8) 0.088(6) 0.096(6) 0.035(5) 0.043(6) 0.057(6) O7 0.252(9) 0.174(7) 0.171(7) 0.076(6) 0.129(7) 0.152(7) C8 0.099(6) 0.064(4) 0.064(5) 0.016(4) 0.013(4) 0.007(4) O8 0.108(5) 0.123(5) 0.097(5) 0.023(4) -0.027(4) 0.002(4) C9 0.069(5) 0.073(5) 0.069(5) 0.013(4) 0.015(4) 0.025(4) O9 0.081(3) 0.071(3) 0.114(4) 0.029(3) 0.024(3) 0.011(3) Co4 0.0814(6) 0.0383(4) 0.0647(6) 0.0074(4) 0.0086(5) 0.0107(4) C10 0.130(7) 0.070(5) 0.092(6) 0.018(4) 0.029(5) 0.038(5) O10 0.221(8) 0.114(5) 0.194(8) 0.055(5) 0.090(6) 0.112(6) C11 0.068(4) 0.048(4) 0.081(5) 0.008(4) 0.007(4) 0.002(3) O11 0.103(4) 0.090(4) 0.078(4) 0.020(3) 0.028(3) 0.014(3) C12 0.111(7) 0.063(5) 0.090(6) 0.010(4) -0.005(5) -0.008(5) O12 0.134(6) 0.119(5) 0.141(6) 0.007(4) -0.028(5) -0.034(5) C13 0.046(3) 0.042(3) 0.054(4) -0.001(3) 0.007(3) 0.001(3) C14 0.045(3) 0.047(3) 0.050(3) -0.001(3) 0.009(3) 0.000(3) C15 0.055(4) 0.055(4) 0.080(5) 0.000(3) 0.005(3) 0.012(3) C16 0.082(5) 0.064(4) 0.059(4) 0.009(3) 0.005(4) 0.019(4) C17 0.074(5) 0.062(4) 0.077(5) 0.022(4) -0.001(4) 0.011(3) C18 0.066(4) 0.067(4) 0.065(4) -0.009(3) 0.002(3) 0.026(3) C19 0.066(4) 0.043(3) 0.053(4) 0.005(3) 0.011(3) 0.016(3) C20 0.059(4) 0.036(3) 0.056(4) 0.008(3) 0.009(3) 0.006(3) C21 0.051(4) 0.053(4) 0.077(4) 0.004(3) 0.016(3) 0.006(3) C22 0.051(4) 0.055(3) 0.055(4) -0.001(3) 0.011(3) 0.021(3) C23 0.048(4) 0.078(5) 0.085(5) 0.000(4) -0.007(3) 0.021(3) C24 0.075(5) 0.086(5) 0.104(6) 0.015(4) -0.016(4) 0.042(5) C25 0.085(5) 0.053(4) 0.075(5) 0.014(3) 0.010(4) 0.040(4) C26 0.066(4) 0.043(3) 0.039(3) 0.004(2) 0.007(3) 0.016(3) C27 0.052(4) 0.056(4) 0.054(4) 0.007(3) -0.001(3) 0.023(3) C28 0.086(5) 0.049(4) 0.057(4) 0.017(3) 0.002(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C3 1.783(8) . ? Co1 C2 1.793(9) . ? Co1 C1 1.805(8) . ? Co1 C13 1.956(5) . ? Co1 C14 1.961(5) . ? Co1 Co2 2.4624(16) . ? C1 O1 1.123(8) . ? C2 O2 1.129(8) . ? C3 O3 1.116(8) . ? Co2 C4 1.771(7) . ? Co2 C5 1.804(8) . ? Co2 C6 1.816(8) . ? Co2 C13 1.955(6) . ? Co2 C14 1.960(6) . ? C4 O4 1.155(7) . ? C5 O5 1.131(7) . ? C6 O6 1.111(8) . ? Co3 C9 1.788(8) . ? Co3 C7 1.795(10) . ? Co3 C8 1.815(9) . ? Co3 C20 1.963(6) . ? Co3 C19 1.964(6) . ? Co3 Co4 2.4776(15) . ? C7 O7 1.138(9) . ? C8 O8 1.127(8) . ? C9 O9 1.133(7) . ? Co4 C11 1.768(8) . ? Co4 C12 1.802(9) . ? Co4 C10 1.808(9) . ? Co4 C20 1.961(5) . ? Co4 C19 1.967(6) . ? C10 O10 1.116(9) . ? C11 O11 1.144(8) . ? C12 O12 1.133(9) . ? C13 C14 1.326(7) . ? C13 C28 1.502(8) . ? C14 C15 1.507(8) . ? C15 C16 1.446(9) . ? C16 C17 1.344(9) . ? C17 C18 1.462(9) . ? C18 C19 1.502(8) . ? C19 C20 1.317(8) . ? C20 C21 1.486(8) . ? C21 C22 1.507(8) . ? C22 C23 1.368(8) . ? C22 C27 1.384(8) . ? C23 C24 1.374(9) . ? C24 C25 1.358(9) . ? C25 C26 1.375(8) . ? C26 C27 1.390(7) . ? C26 C28 1.507(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Co1 C2 101.2(4) . . ? C3 Co1 C1 97.3(3) . . ? C2 Co1 C1 106.2(4) . . ? C3 Co1 C13 98.1(3) . . ? C2 Co1 C13 138.9(3) . . ? C1 Co1 C13 106.9(3) . . ? C3 Co1 C14 102.0(3) . . ? C2 Co1 C14 100.6(3) . . ? C1 Co1 C14 143.0(3) . . ? C13 Co1 C14 39.6(2) . . ? C3 Co1 Co2 148.3(2) . . ? C2 Co1 Co2 100.5(2) . . ? C1 Co1 Co2 98.6(2) . . ? C13 Co1 Co2 50.96(17) . . ? C14 Co1 Co2 51.07(17) . . ? O1 C1 Co1 178.3(8) . . ? O2 C2 Co1 177.9(7) . . ? O3 C3 Co1 178.1(8) . . ? C4 Co2 C5 98.8(3) . . ? C4 Co2 C6 99.4(3) . . ? C5 Co2 C6 106.9(3) . . ? C4 Co2 C13 102.1(3) . . ? C5 Co2 C13 139.4(3) . . ? C6 Co2 C13 103.6(3) . . ? C4 Co2 C14 102.9(3) . . ? C5 Co2 C14 101.8(3) . . ? C6 Co2 C14 140.1(3) . . ? C13 Co2 C14 39.6(2) . . ? C4 Co2 Co1 151.4(2) . . ? C5 Co2 Co1 98.7(2) . . ? C6 Co2 Co1 97.0(2) . . ? C13 Co2 Co1 50.99(16) . . ? C14 Co2 Co1 51.10(15) . . ? O4 C4 Co2 178.6(7) . . ? O5 C5 Co2 176.7(7) . . ? O6 C6 Co2 178.9(8) . . ? C9 Co3 C7 98.1(4) . . ? C9 Co3 C8 100.7(3) . . ? C7 Co3 C8 108.1(4) . . ? C9 Co3 C20 103.1(3) . . ? C7 Co3 C20 142.8(3) . . ? C8 Co3 C20 97.6(3) . . ? C9 Co3 C19 96.6(3) . . ? C7 Co3 C19 108.6(3) . . ? C8 Co3 C19 136.4(3) . . ? C20 Co3 C19 39.2(2) . . ? C9 Co3 Co4 147.3(2) . . ? C7 Co3 Co4 96.8(2) . . ? C8 Co3 Co4 102.0(2) . . ? C20 Co3 Co4 50.80(15) . . ? C19 Co3 Co4 50.99(17) . . ? O7 C7 Co3 178.4(8) . . ? O8 C8 Co3 174.7(8) . . ? O9 C9 Co3 176.8(6) . . ? C11 Co4 C12 99.4(3) . . ? C11 Co4 C10 99.5(3) . . ? C12 Co4 C10 105.5(4) . . ? C11 Co4 C20 99.8(3) . . ? C12 Co4 C20 102.2(3) . . ? C10 Co4 C20 143.0(3) . . ? C11 Co4 C19 99.3(3) . . ? C12 Co4 C19 139.5(3) . . ? C10 Co4 C19 106.4(3) . . ? C20 Co4 C19 39.2(2) . . ? C11 Co4 Co3 148.1(2) . . ? C12 Co4 Co3 99.3(3) . . ? C10 Co4 Co3 100.2(3) . . ? C20 Co4 Co3 50.87(17) . . ? C19 Co4 Co3 50.87(17) . . ? O10 C10 Co4 179.1(8) . . ? O11 C11 Co4 177.9(7) . . ? O12 C12 Co4 175.8(9) . . ? C14 C13 C28 143.7(5) . . ? C14 C13 Co2 70.4(3) . . ? C28 C13 Co2 136.9(5) . . ? C14 C13 Co1 70.4(3) . . ? C28 C13 Co1 129.3(4) . . ? Co2 C13 Co1 78.0(2) . . ? C13 C14 C15 143.2(5) . . ? C13 C14 Co2 70.0(4) . . ? C15 C14 Co2 135.5(4) . . ? C13 C14 Co1 70.0(3) . . ? C15 C14 Co1 132.1(4) . . ? Co2 C14 Co1 77.8(2) . . ? C16 C15 C14 114.5(5) . . ? C17 C16 C15 127.0(7) . . ? C16 C17 C18 128.8(7) . . ? C17 C18 C19 111.6(5) . . ? C20 C19 C18 143.0(5) . . ? C20 C19 Co3 70.4(4) . . ? C18 C19 Co3 133.3(5) . . ? C20 C19 Co4 70.2(3) . . ? C18 C19 Co4 134.0(4) . . ? Co3 C19 Co4 78.1(2) . . ? C19 C20 C21 145.0(6) . . ? C19 C20 Co4 70.7(3) . . ? C21 C20 Co4 129.9(4) . . ? C19 C20 Co3 70.5(4) . . ? C21 C20 Co3 134.8(4) . . ? Co4 C20 Co3 78.3(2) . . ? C20 C21 C22 114.7(5) . . ? C23 C22 C27 118.0(6) . . ? C23 C22 C21 121.1(6) . . ? C27 C22 C21 120.9(5) . . ? C22 C23 C24 121.1(6) . . ? C25 C24 C23 120.1(6) . . ? C24 C25 C26 121.1(6) . . ? C25 C26 C27 117.8(5) . . ? C25 C26 C28 121.1(5) . . ? C27 C26 C28 121.0(5) . . ? C22 C27 C26 121.8(5) . . ? C13 C28 C26 115.5(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.641 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.071 #===END data_ramm5_18 _database_code_CSD 168776 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H18 Co4 O12' _chemical_formula_weight 794.15 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.032(4) _cell_length_b 14.263(7) _cell_length_c 14.655(6) _cell_angle_alpha 93.60(4) _cell_angle_beta 95.73(4) _cell_angle_gamma 102.93(4) _cell_volume 1621.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 1.10 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.069 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4242 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4242 _reflns_number_gt 3018 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+2.8550P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4242 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.016 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 0.11288(13) 0.03602(8) 0.30866(7) 0.0566(3) Uani 1 1 d . . . C1 C -0.0020(10) 0.1249(7) 0.3358(6) 0.067(2) Uani 1 1 d . . . O1 O -0.0716(9) 0.1850(6) 0.3486(5) 0.103(2) Uani 1 1 d . . . C2 C 0.1540(13) -0.0130(8) 0.4170(8) 0.088(3) Uani 1 1 d . . . O2 O 0.1878(11) -0.0395(7) 0.4859(6) 0.140(4) Uani 1 1 d . . . C3 C -0.0623(13) -0.0517(7) 0.2407(7) 0.084(3) Uani 1 1 d . . . O3 O -0.1678(10) -0.1076(6) 0.1992(6) 0.132(3) Uani 1 1 d . . . Co2 Co 0.33700(14) -0.00279(8) 0.21937(8) 0.0621(3) Uani 1 1 d . . . C4 C 0.5347(13) 0.0363(7) 0.1699(7) 0.078(3) Uani 1 1 d . . . O4 O 0.6578(10) 0.0632(6) 0.1408(6) 0.130(3) Uani 1 1 d . . . C5 C 0.3960(16) -0.0862(8) 0.2955(9) 0.106(4) Uani 1 1 d . . . O5 O 0.4309(15) -0.1344(7) 0.3499(7) 0.169(5) Uani 1 1 d . . . C6 C 0.2076(14) -0.0680(8) 0.1174(8) 0.096(3) Uani 1 1 d . . . O6 O 0.1253(12) -0.1040(8) 0.0525(6) 0.161(4) Uani 1 1 d . . . Co3 Co 0.97930(13) 0.56551(8) 0.30144(7) 0.0527(3) Uani 1 1 d . . . C7 C 1.1055(11) 0.4900(7) 0.3509(6) 0.068(2) Uani 1 1 d . . . O7 O 1.1822(9) 0.4384(6) 0.3797(6) 0.111(3) Uani 1 1 d . . . C8 C 1.1368(12) 0.6301(8) 0.2347(6) 0.079(3) Uani 1 1 d . . . O8 O 1.2333(9) 0.6716(6) 0.1927(5) 0.125(3) Uani 1 1 d . . . C9 C 0.9708(12) 0.6531(8) 0.3946(7) 0.080(3) Uani 1 1 d . . . O9 O 0.9557(11) 0.7045(6) 0.4532(6) 0.132(3) Uani 1 1 d . . . Co4 Co 0.72264(13) 0.57457(8) 0.19748(7) 0.0571(3) Uani 1 1 d . . . C10 C 0.8249(12) 0.6186(7) 0.0985(7) 0.082(3) Uani 1 1 d . . . O10 O 0.8941(9) 0.6439(7) 0.0383(5) 0.128(3) Uani 1 1 d . . . C11 C 0.6707(12) 0.6746(7) 0.2612(7) 0.079(3) Uani 1 1 d . . . O11 O 0.6376(11) 0.7337(6) 0.3057(6) 0.129(3) Uani 1 1 d . . . C12 C 0.5104(14) 0.5179(7) 0.1401(8) 0.092(3) Uani 1 1 d . . . O12 O 0.3791(10) 0.4839(6) 0.1065(7) 0.140(4) Uani 1 1 d . . . C13 C 0.3492(9) 0.1096(5) 0.3059(5) 0.0482(19) Uani 1 1 d . . . C14 C 0.2548(9) 0.1159(5) 0.2272(5) 0.0493(19) Uani 1 1 d . . . C15 C 0.2239(9) 0.1878(6) 0.1614(5) 0.056(2) Uani 1 1 d . . . H15A H 0.1970 0.2423 0.1950 0.080 Uiso 1 1 calc R . . H15B H 0.1254 0.1584 0.1169 0.080 Uiso 1 1 calc R . . C16 C 0.3774(9) 0.2232(5) 0.1114(5) 0.0499(19) Uani 1 1 d . . . C17 C 0.3704(11) 0.2003(6) 0.0175(5) 0.064(2) Uani 1 1 d . . . H17 H 0.2711 0.1618 -0.0155 0.080 Uiso 1 1 calc R . . C18 C 0.5116(12) 0.2350(7) -0.0259(6) 0.078(3) Uani 1 1 d . . . H18 H 0.5063 0.2203 -0.0890 0.080 Uiso 1 1 calc R . . C19 C 0.6611(11) 0.2907(6) 0.0208(5) 0.060(2) Uani 1 1 d . . . H19 H 0.7554 0.3126 -0.0106 0.080 Uiso 1 1 calc R . . C20 C 0.6716(9) 0.3142(5) 0.1142(5) 0.0479(19) Uani 1 1 d . . . C21 C 0.5264(9) 0.2804(5) 0.1579(5) 0.0493(19) Uani 1 1 d . . . H21 H 0.5304 0.2970 0.2206 0.080 Uiso 1 1 calc R . . C22 C 0.8361(9) 0.3758(6) 0.1669(5) 0.058(2) Uani 1 1 d . . . H22A H 0.8869 0.3357 0.2073 0.080 Uiso 1 1 calc R . . H22B H 0.9166 0.3976 0.1234 0.080 Uiso 1 1 calc R . . C23 C 0.8133(9) 0.4610(5) 0.2228(5) 0.0488(19) Uani 1 1 d . . . C24 C 0.7414(9) 0.4874(5) 0.2943(5) 0.0481(19) Uani 1 1 d . . . C25 C 0.6310(9) 0.4512(5) 0.3670(5) 0.054(2) Uani 1 1 d . . . H25A H 0.5164 0.4197 0.3382 0.080 Uiso 1 1 calc R . . H25B H 0.6214 0.5055 0.4078 0.080 Uiso 1 1 calc R . . C26 C 0.7038(10) 0.3804(6) 0.4233(5) 0.058(2) Uani 1 1 d . . . H26A H 0.7396 0.3350 0.3818 0.080 Uiso 1 1 calc R . . H26B H 0.8052 0.4157 0.4631 0.080 Uiso 1 1 calc R . . C27 C 0.5783(10) 0.3246(6) 0.4819(5) 0.066(2) Uani 1 1 d . . . H27A H 0.5318 0.3698 0.5180 0.080 Uiso 1 1 calc R . . H27B H 0.6398 0.2911 0.5243 0.080 Uiso 1 1 calc R . . C28 C 0.4287(10) 0.2505(6) 0.4258(5) 0.061(2) Uani 1 1 d . . . H28A H 0.3440 0.2257 0.4663 0.080 Uiso 1 1 calc R . . H28B H 0.3740 0.2828 0.3792 0.080 Uiso 1 1 calc R . . C29 C 0.4852(10) 0.1661(5) 0.3791(5) 0.057(2) Uani 1 1 d . . . H29A H 0.5896 0.1904 0.3516 0.080 Uiso 1 1 calc R . . H29B H 0.5107 0.1235 0.4249 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0451(6) 0.0589(7) 0.0642(7) 0.0079(6) 0.0118(5) 0.0058(5) C1 0.038(5) 0.088(7) 0.071(6) 0.003(5) 0.008(4) 0.008(5) O1 0.077(5) 0.117(6) 0.126(6) -0.007(5) 0.026(4) 0.043(4) C2 0.079(7) 0.101(8) 0.099(8) 0.040(7) 0.037(6) 0.036(6) O2 0.137(7) 0.208(10) 0.108(6) 0.082(7) 0.043(6) 0.075(7) C3 0.064(6) 0.079(7) 0.105(8) 0.011(6) 0.019(6) 0.001(5) O3 0.092(6) 0.105(6) 0.159(8) -0.027(5) 0.001(5) -0.044(5) Co2 0.0612(7) 0.0569(7) 0.0692(8) -0.0014(6) 0.0131(6) 0.0155(6) C4 0.074(7) 0.082(7) 0.090(7) 0.011(6) 0.016(6) 0.040(6) O4 0.088(6) 0.145(7) 0.181(8) 0.040(6) 0.070(6) 0.044(5) C5 0.139(10) 0.071(7) 0.129(10) 0.017(7) 0.045(8) 0.056(7) O5 0.250(12) 0.159(9) 0.166(9) 0.071(7) 0.076(8) 0.148(9) C6 0.083(7) 0.097(8) 0.101(8) -0.044(7) 0.019(6) 0.018(6) O6 0.126(7) 0.201(10) 0.124(7) -0.091(7) -0.004(6) 0.005(7) Co3 0.0414(6) 0.0596(7) 0.0507(7) -0.0027(5) 0.0004(5) 0.0028(5) C7 0.054(6) 0.070(6) 0.071(6) -0.005(5) 0.001(5) 0.002(5) O7 0.079(5) 0.115(6) 0.141(7) 0.014(5) -0.021(5) 0.044(4) C8 0.056(6) 0.108(8) 0.058(6) -0.010(5) -0.003(5) -0.006(5) O8 0.081(5) 0.178(8) 0.092(5) 0.032(5) 0.020(4) -0.029(5) C9 0.064(6) 0.093(8) 0.079(7) -0.002(6) -0.001(5) 0.020(5) O9 0.146(7) 0.147(8) 0.102(6) -0.053(6) -0.008(5) 0.056(6) Co4 0.0478(6) 0.0609(7) 0.0591(7) 0.0072(6) -0.0013(5) 0.0076(5) C10 0.059(6) 0.112(8) 0.073(7) 0.032(6) -0.005(5) 0.014(5) O10 0.086(5) 0.215(9) 0.079(5) 0.052(6) 0.018(4) 0.014(6) C11 0.075(6) 0.076(7) 0.093(8) 0.017(6) 0.009(6) 0.027(5) O11 0.146(7) 0.111(6) 0.142(7) -0.022(6) 0.012(6) 0.067(6) C12 0.075(7) 0.081(7) 0.116(9) 0.012(6) -0.008(6) 0.018(6) O12 0.068(5) 0.130(7) 0.196(9) -0.004(6) -0.059(6) 0.009(5) C13 0.045(4) 0.048(5) 0.052(5) 0.004(4) 0.015(4) 0.007(4) C14 0.047(4) 0.058(5) 0.044(5) 0.007(4) 0.016(4) 0.009(4) C15 0.037(4) 0.063(5) 0.063(5) 0.012(4) -0.002(4) 0.004(4) C16 0.035(4) 0.052(5) 0.058(5) 0.011(4) -0.003(4) 0.004(4) C17 0.058(5) 0.079(6) 0.045(5) 0.000(4) -0.007(4) 0.003(4) C18 0.081(7) 0.106(8) 0.035(5) 0.000(5) 0.003(5) -0.001(6) C19 0.064(5) 0.069(6) 0.043(5) 0.001(4) 0.014(4) 0.004(4) C20 0.051(5) 0.052(5) 0.039(4) 0.000(4) 0.010(4) 0.008(4) C21 0.049(5) 0.056(5) 0.040(4) -0.003(4) 0.007(4) 0.008(4) C22 0.045(5) 0.067(5) 0.061(5) 0.001(4) 0.014(4) 0.009(4) C23 0.038(4) 0.060(5) 0.045(5) 0.000(4) 0.001(4) 0.007(4) C24 0.040(4) 0.043(4) 0.057(5) -0.002(4) -0.002(4) 0.005(3) C25 0.045(5) 0.056(5) 0.059(5) -0.004(4) 0.016(4) 0.005(4) C26 0.055(5) 0.067(5) 0.045(5) 0.001(4) -0.002(4) 0.002(4) C27 0.068(6) 0.076(6) 0.047(5) 0.000(4) 0.009(4) 0.004(5) C28 0.059(5) 0.065(5) 0.057(5) 0.000(4) 0.015(4) 0.008(4) C29 0.054(5) 0.056(5) 0.063(5) 0.004(4) 0.002(4) 0.019(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 C1 1.775(10) . ? Co1 C2 1.804(11) . ? Co1 C3 1.820(11) . ? Co1 C13 1.958(7) . ? Co1 C14 1.971(7) . ? Co1 Co2 2.4667(18) . ? C1 O1 1.139(10) . ? C2 O2 1.129(11) . ? C3 O3 1.122(11) . ? Co2 C5 1.788(13) . ? Co2 C4 1.801(11) . ? Co2 C6 1.805(12) . ? Co2 C14 1.951(8) . ? Co2 C13 1.959(7) . ? C4 O4 1.114(10) . ? C5 O5 1.139(12) . ? C6 O6 1.126(11) . ? Co3 C7 1.776(11) . ? Co3 C8 1.801(10) . ? Co3 C9 1.808(11) . ? Co3 C24 1.974(7) . ? Co3 C23 1.979(7) . ? Co3 Co4 2.4707(19) . ? C7 O7 1.135(10) . ? C8 O8 1.125(10) . ? C9 O9 1.128(10) . ? Co4 C11 1.804(11) . ? Co4 C12 1.811(11) . ? Co4 C10 1.816(11) . ? Co4 C23 1.960(8) . ? Co4 C24 1.961(8) . ? C10 O10 1.124(10) . ? C11 O11 1.128(10) . ? C12 O12 1.107(11) . ? C13 C14 1.334(10) . ? C13 C29 1.502(10) . ? C14 C15 1.494(10) . ? C15 C16 1.503(10) . ? C16 C21 1.376(9) . ? C16 C17 1.388(10) . ? C17 C18 1.367(11) . ? C18 C19 1.371(11) . ? C19 C20 1.378(9) . ? C20 C21 1.392(9) . ? C20 C22 1.519(10) . ? C22 C23 1.478(10) . ? C23 C24 1.320(10) . ? C24 C25 1.498(10) . ? C25 C26 1.521(10) . ? C26 C27 1.512(10) . ? C27 C28 1.536(10) . ? C28 C29 1.526(10) . ? 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 C1 Co1 C2 104.0(4) . . ? C1 Co1 C3 98.3(4) . . ? C2 Co1 C3 107.0(5) . . ? C1 Co1 C13 104.3(3) . . ? C2 Co1 C13 95.8(4) . . ? C3 Co1 C13 142.7(4) . . ? C1 Co1 C14 94.2(4) . . ? C2 Co1 C14 135.3(4) . . ? C3 Co1 C14 110.2(4) . . ? C13 Co1 C14 39.7(3) . . ? C1 Co1 Co2 144.9(3) . . ? C2 Co1 Co2 103.2(3) . . ? C3 Co1 Co2 94.5(3) . . ? C13 Co1 Co2 51.0(2) . . ? C14 Co1 Co2 50.7(2) . . ? O1 C1 Co1 175.6(9) . . ? O2 C2 Co1 176.1(11) . . ? O3 C3 Co1 178.1(10) . . ? C5 Co2 C4 100.6(5) . . ? C5 Co2 C6 109.8(5) . . ? C4 Co2 C6 98.0(5) . . ? C5 Co2 C14 138.1(4) . . ? C4 Co2 C14 101.5(3) . . ? C6 Co2 C14 101.9(4) . . ? C5 Co2 C13 101.2(4) . . ? C4 Co2 C13 100.1(4) . . ? C6 Co2 C13 140.3(4) . . ? C14 Co2 C13 39.9(3) . . ? C5 Co2 Co1 95.1(4) . . ? C4 Co2 Co1 149.5(3) . . ? C6 Co2 Co1 101.0(3) . . ? C14 Co2 Co1 51.4(2) . . ? C13 Co2 Co1 51.0(2) . . ? O4 C4 Co2 177.9(10) . . ? O5 C5 Co2 174.2(11) . . ? O6 C6 Co2 176.2(12) . . ? C7 Co3 C8 97.6(4) . . ? C7 Co3 C9 104.8(4) . . ? C8 Co3 C9 104.1(4) . . ? C7 Co3 C24 103.7(3) . . ? C8 Co3 C24 143.8(4) . . ? C9 Co3 C24 98.5(4) . . ? C7 Co3 C23 95.9(3) . . ? C8 Co3 C23 110.4(3) . . ? C9 Co3 C23 136.7(4) . . ? C24 Co3 C23 39.0(3) . . ? C7 Co3 Co4 146.7(3) . . ? C8 Co3 Co4 96.8(3) . . ? C9 Co3 Co4 100.6(3) . . ? C24 Co3 Co4 50.9(2) . . ? C23 Co3 Co4 50.8(2) . . ? O7 C7 Co3 176.9(8) . . ? O8 C8 Co3 178.7(10) . . ? O9 C9 Co3 175.8(10) . . ? C11 Co4 C12 99.0(5) . . ? C11 Co4 C10 108.7(5) . . ? C12 Co4 C10 99.1(5) . . ? C11 Co4 C23 138.3(4) . . ? C12 Co4 C23 100.9(4) . . ? C10 Co4 C23 103.8(4) . . ? C11 Co4 C24 101.2(4) . . ? C12 Co4 C24 100.2(4) . . ? C10 Co4 C24 141.1(4) . . ? C23 Co4 C24 39.3(3) . . ? C11 Co4 Co3 97.1(3) . . ? C12 Co4 Co3 149.7(3) . . ? C10 Co4 Co3 99.8(3) . . ? C23 Co4 Co3 51.5(2) . . ? C24 Co4 Co3 51.3(2) . . ? O10 C10 Co4 176.9(9) . . ? O11 C11 Co4 175.7(10) . . ? O12 C12 Co4 178.5(12) . . ? C14 C13 C29 143.9(7) . . ? C14 C13 Co1 70.7(4) . . ? C29 C13 Co1 133.1(5) . . ? C14 C13 Co2 69.7(4) . . ? C29 C13 Co2 133.5(5) . . ? Co1 C13 Co2 78.0(3) . . ? C13 C14 C15 141.0(7) . . ? C13 C14 Co2 70.4(5) . . ? C15 C14 Co2 135.2(5) . . ? C13 C14 Co1 69.6(4) . . ? C15 C14 Co1 134.5(5) . . ? Co2 C14 Co1 77.9(3) . . ? C14 C15 C16 112.0(6) . . ? C21 C16 C17 118.8(7) . . ? C21 C16 C15 120.5(7) . . ? C17 C16 C15 120.7(7) . . ? C18 C17 C16 119.1(7) . . ? C17 C18 C19 122.1(8) . . ? C18 C19 C20 120.0(7) . . ? C19 C20 C21 117.8(7) . . ? C19 C20 C22 120.7(7) . . ? C21 C20 C22 121.5(6) . . ? C16 C21 C20 122.2(7) . . ? C23 C22 C20 114.7(6) . . ? C24 C23 C22 143.1(7) . . ? C24 C23 Co4 70.4(5) . . ? C22 C23 Co4 135.4(6) . . ? C24 C23 Co3 70.3(4) . . ? C22 C23 Co3 132.0(5) . . ? Co4 C23 Co3 77.7(3) . . ? C23 C24 C25 144.4(7) . . ? C23 C24 Co4 70.3(5) . . ? C25 C24 Co4 133.7(5) . . ? C23 C24 Co3 70.7(4) . . ? C25 C24 Co3 132.1(5) . . ? Co4 C24 Co3 77.8(3) . . ? C24 C25 C26 112.0(6) . . ? C27 C26 C25 113.7(7) . . ? C26 C27 C28 113.6(6) . . ? C29 C28 C27 113.1(7) . . ? C13 C29 C28 111.9(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.357 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.075 #===END data_ramm3_19 _database_code_CSD 168777 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Co4 O12' _chemical_formula_weight 806.16 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.573(4) _cell_length_b 10.648(3) _cell_length_c 22.761(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.38(3) _cell_angle_gamma 90.00 _cell_volume 3275.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max .85 _exptl_crystal_size_mid .75 _exptl_crystal_size_min .25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 2.050 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6767 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.25 _reflns_number_total 6506 _reflns_number_gt 4254 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+2.8250P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6506 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.009 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 0.09962(5) 0.24574(7) 0.09533(3) 0.0505(2) Uani 1 1 d . . . C1 C 0.1523(4) 0.3980(7) 0.0831(2) 0.0693(16) Uani 1 1 d . . . O1 O 0.1847(4) 0.4949(5) 0.0760(3) 0.1069(17) Uani 1 1 d . . . C2 C 0.0982(4) 0.1622(6) 0.0260(2) 0.0735(17) Uani 1 1 d . . . O2 O 0.0986(4) 0.1095(6) -0.0164(2) 0.122(2) Uani 1 1 d . . . C3 C 0.2057(5) 0.1730(6) 0.1334(3) 0.0703(16) Uani 1 1 d . . . O3 O 0.2718(4) 0.1283(5) 0.1581(2) 0.1095(17) Uani 1 1 d . . . Co2 Co -0.07501(5) 0.31029(7) 0.09160(3) 0.0529(2) Uani 1 1 d . . . C4 C -0.0597(5) 0.4750(7) 0.0747(3) 0.0724(17) Uani 1 1 d . . . O4 O -0.0482(4) 0.5762(5) 0.0625(2) 0.1077(17) Uani 1 1 d . . . C5 C -0.1870(5) 0.3149(7) 0.1267(3) 0.0778(18) Uani 1 1 d . . . O5 O -0.2570(3) 0.3139(6) 0.1499(2) 0.118(2) Uani 1 1 d . . . C6 C -0.1216(5) 0.2413(6) 0.0206(3) 0.0739(17) Uani 1 1 d . . . O6 O -0.1474(4) 0.1969(5) -0.0225(2) 0.1096(17) Uani 1 1 d . . . Co3 Co 0.03846(5) 0.29768(7) 0.40232(3) 0.0548(2) Uani 1 1 d . . . C7 C 0.1449(5) 0.2712(6) 0.3626(2) 0.0713(17) Uani 1 1 d . . . O7 O 0.2139(3) 0.2544(5) 0.3392(2) 0.1036(16) Uani 1 1 d . . . C8 C 0.0511(5) 0.4663(7) 0.4140(3) 0.0763(18) Uani 1 1 d . . . O8 O 0.0585(5) 0.5700(5) 0.4220(3) 0.124(2) Uani 1 1 d . . . C9 C 0.0836(5) 0.2217(6) 0.4711(3) 0.0755(17) Uani 1 1 d . . . O9 O 0.1117(4) 0.1704(6) 0.5126(2) 0.121(2) Uani 1 1 d . . . Co4 Co -0.13983(5) 0.28406(7) 0.41438(3) 0.0584(2) Uani 1 1 d . . . C10 C -0.1358(5) 0.2007(7) 0.4840(3) 0.0812(19) Uani 1 1 d . . . O10 O -0.1325(4) 0.1476(6) 0.5269(2) 0.124(2) Uani 1 1 d . . . C11 C -0.1648(5) 0.4473(7) 0.4308(3) 0.0779(18) Uani 1 1 d . . . O11 O -0.1823(5) 0.5476(6) 0.4395(3) 0.125(2) Uani 1 1 d . . . C12 C -0.2597(6) 0.2459(8) 0.3807(3) 0.097(2) Uani 1 1 d . . . O12 O -0.3332(4) 0.2211(8) 0.3567(3) 0.161(3) Uani 1 1 d . . . C13 C -0.0107(3) 0.1668(5) 0.13271(19) 0.0479(11) Uani 1 1 d . . . C14 C 0.0175(3) 0.2721(4) 0.16163(18) 0.0436(11) Uani 1 1 d . . . C15 C 0.0466(4) 0.3193(5) 0.22296(19) 0.0474(11) Uani 1 1 d . . . H15A H 0.1085 0.3647 0.2225 0.080 Uiso 1 1 calc R . . H15B H 0.0592 0.2472 0.2486 0.080 Uiso 1 1 calc R . . C16 C -0.0268(4) 0.4043(4) 0.25041(18) 0.0461(11) Uani 1 1 d . . . C17 C -0.1044(4) 0.3355(5) 0.2801(2) 0.0537(12) Uani 1 1 d . . . H17A H -0.1288 0.2671 0.2546 0.080 Uiso 1 1 calc R . . H17B H -0.1593 0.3923 0.2839 0.080 Uiso 1 1 calc R . . C18 C -0.0724(4) 0.2817(5) 0.34066(19) 0.0498(12) Uani 1 1 d . . . C19 C -0.0586(4) 0.1737(5) 0.36934(19) 0.0502(12) Uani 1 1 d . . . C20 C -0.0585(5) 0.0332(5) 0.3616(2) 0.0689(16) Uani 1 1 d . . . H20A H -0.0278 -0.0058 0.3972 0.080 Uiso 1 1 calc R . . H20B H -0.1262 0.0033 0.3553 0.080 Uiso 1 1 calc R . . C21 C -0.0034(4) -0.0047(4) 0.3101(2) 0.0542(13) Uani 1 1 d . . . C22 C 0.0909(5) -0.0519(6) 0.3171(3) 0.0744(17) Uani 1 1 d . . . H22 H 0.1215 -0.0652 0.3548 0.080 Uiso 1 1 calc R . . C23 C 0.1406(5) -0.0797(6) 0.2690(3) 0.0786(18) Uani 1 1 d . . . H23 H 0.2036 -0.1145 0.2745 0.080 Uiso 1 1 calc R . . C24 C 0.0987(5) -0.0569(5) 0.2131(3) 0.0681(16) Uani 1 1 d . . . H24 H 0.1337 -0.0748 0.1809 0.080 Uiso 1 1 calc R . . C25 C 0.0045(4) -0.0076(4) 0.2042(2) 0.0511(12) Uani 1 1 d . . . C26 C -0.0464(4) 0.0149(4) 0.2529(2) 0.0521(12) Uani 1 1 d . . . H26 H -0.1112 0.0441 0.2473 0.080 Uiso 1 1 calc R . . C27 C -0.0397(4) 0.0329(5) 0.1436(2) 0.0623(14) Uani 1 1 d . . . H27A H -0.0158 -0.0214 0.1138 0.080 Uiso 1 1 calc R . . H27B H -0.1112 0.0259 0.1413 0.080 Uiso 1 1 calc R . . C28 C -0.0199(5) 0.5295(5) 0.2495(2) 0.0684(16) Uani 1 1 d . . . C29 C 0.0577(6) 0.5966(6) 0.2168(3) 0.097(2) Uani 1 1 d . . . H29A H 0.0969 0.5356 0.1984 0.080 Uiso 1 1 calc R . . H29B H 0.0997 0.6457 0.2443 0.080 Uiso 1 1 calc R . . H29C H 0.0255 0.6506 0.1872 0.080 Uiso 1 1 calc R . . C30 C -0.0875(6) 0.6145(6) 0.2796(3) 0.114(3) Uani 1 1 d . . . H30A H -0.1335 0.5649 0.2993 0.080 Uiso 1 1 calc R . . H30B H -0.1231 0.6675 0.2508 0.080 Uiso 1 1 calc R . . H30C H -0.0491 0.6656 0.3080 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0547(4) 0.0638(4) 0.0340(3) -0.0021(3) 0.0096(3) 0.0033(3) C1 0.067(4) 0.087(5) 0.054(3) 0.005(3) 0.011(3) 0.004(3) O1 0.107(4) 0.087(3) 0.130(5) 0.015(3) 0.025(3) -0.020(3) C2 0.078(4) 0.098(5) 0.046(3) -0.011(3) 0.014(3) -0.009(3) O2 0.147(5) 0.159(5) 0.063(3) -0.056(3) 0.021(3) -0.010(4) C3 0.062(4) 0.089(5) 0.061(4) 0.000(3) 0.008(3) 0.007(3) O3 0.070(3) 0.139(5) 0.116(4) 0.024(4) -0.010(3) 0.023(3) Co2 0.0566(4) 0.0677(5) 0.0339(3) 0.0050(3) 0.0018(3) 0.0087(3) C4 0.091(4) 0.074(4) 0.052(3) 0.010(3) 0.006(3) 0.020(4) O4 0.163(5) 0.072(3) 0.089(4) 0.018(3) 0.015(3) 0.023(3) C5 0.065(4) 0.110(5) 0.057(4) 0.012(3) 0.004(3) 0.026(4) O5 0.068(3) 0.191(6) 0.098(4) 0.035(4) 0.029(3) 0.038(3) C6 0.079(4) 0.092(5) 0.048(3) 0.005(3) -0.009(3) 0.004(3) O6 0.125(4) 0.138(5) 0.059(3) -0.017(3) -0.026(3) -0.002(3) Co3 0.0608(4) 0.0671(5) 0.0363(3) 0.0044(3) 0.0042(3) -0.0142(4) C7 0.061(4) 0.106(5) 0.046(3) 0.016(3) 0.002(3) -0.016(3) O7 0.065(3) 0.168(5) 0.081(3) 0.001(3) 0.019(3) -0.009(3) C8 0.088(5) 0.080(5) 0.061(4) -0.003(3) 0.006(3) -0.025(4) O8 0.169(6) 0.077(3) 0.126(5) -0.019(3) 0.017(4) -0.043(4) C9 0.079(4) 0.095(5) 0.051(3) 0.013(3) 0.002(3) -0.018(3) O9 0.137(5) 0.148(5) 0.072(3) 0.047(3) -0.026(3) -0.022(4) Co4 0.0642(5) 0.0779(5) 0.0354(3) -0.0037(3) 0.0164(3) -0.0103(4) C10 0.097(5) 0.100(5) 0.052(3) 0.007(3) 0.031(3) -0.014(4) O10 0.150(5) 0.157(5) 0.069(3) 0.047(3) 0.039(3) -0.003(4) C11 0.084(4) 0.088(5) 0.064(4) -0.011(4) 0.016(3) 0.005(4) O11 0.142(5) 0.098(4) 0.137(5) -0.026(4) 0.024(4) 0.026(4) C12 0.081(5) 0.153(7) 0.061(4) -0.017(4) 0.030(4) -0.040(5) O12 0.086(4) 0.295(9) 0.102(4) -0.021(5) 0.005(3) -0.074(5) C13 0.051(3) 0.057(3) 0.035(2) 0.002(2) 0.001(2) 0.005(2) C14 0.047(3) 0.056(3) 0.028(2) 0.002(2) 0.0038(19) 0.006(2) C15 0.056(3) 0.054(3) 0.032(2) -0.002(2) 0.002(2) -0.001(2) C16 0.060(3) 0.049(3) 0.029(2) 0.000(2) 0.003(2) -0.001(2) C17 0.053(3) 0.073(3) 0.036(2) 0.005(2) 0.008(2) 0.000(3) C18 0.054(3) 0.065(3) 0.031(2) 0.000(2) 0.011(2) -0.011(2) C19 0.058(3) 0.061(3) 0.032(2) -0.001(2) 0.011(2) -0.015(2) C20 0.097(4) 0.062(3) 0.049(3) 0.007(3) 0.015(3) -0.014(3) C21 0.079(4) 0.038(3) 0.045(3) 0.004(2) 0.008(3) -0.008(3) C22 0.097(5) 0.066(4) 0.058(4) 0.011(3) -0.006(3) 0.008(3) C23 0.073(4) 0.074(4) 0.088(5) 0.012(4) 0.002(4) 0.023(3) C24 0.091(4) 0.052(3) 0.064(4) 0.002(3) 0.024(3) 0.012(3) C25 0.072(4) 0.035(2) 0.047(3) -0.005(2) 0.006(3) -0.007(2) C26 0.063(3) 0.038(3) 0.055(3) -0.002(2) 0.005(3) -0.002(2) C27 0.084(4) 0.059(3) 0.043(3) -0.005(2) -0.001(3) -0.014(3) C28 0.117(5) 0.053(3) 0.033(3) -0.002(2) -0.004(3) 0.000(3) C29 0.145(6) 0.064(4) 0.077(5) 0.022(3) -0.011(4) -0.042(4) C30 0.202(9) 0.066(4) 0.075(5) -0.009(4) 0.013(5) 0.042(5) _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 C3 1.786(7) . ? Co1 C1 1.803(7) . ? Co1 C2 1.810(6) . ? Co1 C14 1.978(4) . ? Co1 C13 1.978(5) . ? Co1 Co2 2.4618(12) . ? C1 O1 1.139(7) . ? C2 O2 1.116(6) . ? C3 O3 1.120(7) . ? Co2 C5 1.783(6) . ? Co2 C4 1.812(7) . ? Co2 C6 1.834(6) . ? Co2 C13 1.954(5) . ? Co2 C14 1.977(4) . ? C4 O4 1.127(7) . ? C5 O5 1.129(7) . ? C6 O6 1.114(7) . ? Co3 C7 1.797(6) . ? Co3 C9 1.817(6) . ? Co3 C8 1.820(7) . ? Co3 C19 1.964(5) . ? Co3 C18 1.966(5) . ? Co3 Co4 2.4651(12) . ? C7 O7 1.135(7) . ? C8 O8 1.122(7) . ? C9 O9 1.127(7) . ? Co4 C12 1.780(8) . ? Co4 C10 1.813(6) . ? Co4 C11 1.816(8) . ? Co4 C19 1.965(5) . ? Co4 C18 1.986(4) . ? C10 O10 1.125(7) . ? C11 O11 1.116(7) . ? C12 O12 1.123(8) . ? C13 C14 1.338(6) . ? C13 C27 1.506(7) . ? C14 C15 1.501(6) . ? C15 C16 1.523(6) . ? C16 C28 1.337(7) . ? C16 C17 1.495(6) . ? C17 C18 1.517(6) . ? C18 C19 1.327(7) . ? C19 C20 1.506(7) . ? C20 C21 1.503(7) . ? C21 C22 1.371(8) . ? C21 C26 1.391(7) . ? C22 C23 1.370(8) . ? C23 C24 1.366(8) . ? C24 C25 1.379(7) . ? C25 C26 1.380(7) . ? C25 C27 1.514(7) . ? C28 C30 1.500(8) . ? C28 C29 1.523(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Co1 C1 98.7(3) . . ? C3 Co1 C2 98.7(3) . . ? C1 Co1 C2 106.2(3) . . ? C3 Co1 C14 100.2(2) . . ? C1 Co1 C14 104.5(2) . . ? C2 Co1 C14 140.7(2) . . ? C3 Co1 C13 102.4(2) . . ? C1 Co1 C13 140.8(2) . . ? C2 Co1 C13 102.7(2) . . ? C14 Co1 C13 39.54(19) . . ? C3 Co1 Co2 150.19(19) . . ? C1 Co1 Co2 97.93(19) . . ? C2 Co1 Co2 100.1(2) . . ? C14 Co1 Co2 51.48(13) . . ? C13 Co1 Co2 50.81(14) . . ? O1 C1 Co1 178.9(6) . . ? O2 C2 Co1 178.8(7) . . ? O3 C3 Co1 178.9(6) . . ? C5 Co2 C4 100.8(3) . . ? C5 Co2 C6 99.7(3) . . ? C4 Co2 C6 103.7(3) . . ? C5 Co2 C13 99.7(2) . . ? C4 Co2 C13 143.5(3) . . ? C6 Co2 C13 102.2(2) . . ? C5 Co2 C14 98.5(2) . . ? C4 Co2 C14 107.1(2) . . ? C6 Co2 C14 140.3(2) . . ? C13 Co2 C14 39.80(19) . . ? C5 Co2 Co1 148.31(19) . . ? C4 Co2 Co1 98.5(2) . . ? C6 Co2 Co1 99.8(2) . . ? C13 Co2 Co1 51.68(14) . . ? C14 Co2 Co1 51.52(13) . . ? O4 C4 Co2 177.4(6) . . ? O5 C5 Co2 177.5(6) . . ? O6 C6 Co2 177.7(6) . . ? C7 Co3 C9 98.1(3) . . ? C7 Co3 C8 99.1(3) . . ? C9 Co3 C8 107.1(3) . . ? C7 Co3 C19 104.1(2) . . ? C9 Co3 C19 101.0(2) . . ? C8 Co3 C19 140.3(3) . . ? C7 Co3 C18 103.0(2) . . ? C9 Co3 C18 138.6(2) . . ? C8 Co3 C18 104.2(3) . . ? C19 Co3 C18 39.5(2) . . ? C7 Co3 Co4 152.96(19) . . ? C9 Co3 Co4 97.6(2) . . ? C8 Co3 Co4 97.0(2) . . ? C19 Co3 Co4 51.15(15) . . ? C18 Co3 Co4 51.76(13) . . ? O7 C7 Co3 177.8(5) . . ? O8 C8 Co3 178.9(6) . . ? O9 C9 Co3 177.3(7) . . ? C12 Co4 C10 102.5(3) . . ? C12 Co4 C11 97.3(4) . . ? C10 Co4 C11 106.2(3) . . ? C12 Co4 C19 100.0(3) . . ? C10 Co4 C19 101.0(3) . . ? C11 Co4 C19 143.6(2) . . ? C12 Co4 C18 96.2(2) . . ? C10 Co4 C18 139.0(3) . . ? C11 Co4 C18 107.2(3) . . ? C19 Co4 C18 39.26(19) . . ? C12 Co4 Co3 146.4(2) . . ? C10 Co4 Co3 100.2(2) . . ? C11 Co4 Co3 99.8(2) . . ? C19 Co4 Co3 51.12(14) . . ? C18 Co4 Co3 51.04(14) . . ? O10 C10 Co4 178.9(7) . . ? O11 C11 Co4 177.9(7) . . ? O12 C12 Co4 176.3(6) . . ? C14 C13 C27 141.2(4) . . ? C14 C13 Co2 71.0(3) . . ? C27 C13 Co2 135.0(4) . . ? C14 C13 Co1 70.2(3) . . ? C27 C13 Co1 133.9(4) . . ? Co2 C13 Co1 77.51(18) . . ? C13 C14 C15 140.9(4) . . ? C13 C14 Co2 69.2(3) . . ? C15 C14 Co2 140.6(3) . . ? C13 C14 Co1 70.2(3) . . ? C15 C14 Co1 129.7(3) . . ? Co2 C14 Co1 76.99(15) . . ? C14 C15 C16 117.1(4) . . ? C28 C16 C17 123.3(5) . . ? C28 C16 C15 122.4(5) . . ? C17 C16 C15 114.2(4) . . ? C16 C17 C18 116.2(4) . . ? C19 C18 C17 142.0(5) . . ? C19 C18 Co3 70.2(3) . . ? C17 C18 Co3 138.6(4) . . ? C19 C18 Co4 69.5(3) . . ? C17 C18 Co4 130.3(4) . . ? Co3 C18 Co4 77.19(16) . . ? C18 C19 C20 143.6(5) . . ? C18 C19 Co3 70.3(3) . . ? C20 C19 Co3 134.8(4) . . ? C18 C19 Co4 71.2(3) . . ? C20 C19 Co4 131.5(4) . . ? Co3 C19 Co4 77.72(18) . . ? C21 C20 C19 111.4(4) . . ? C22 C21 C26 118.0(5) . . ? C22 C21 C20 122.4(5) . . ? C26 C21 C20 119.6(5) . . ? C21 C22 C23 120.7(6) . . ? C24 C23 C22 120.9(6) . . ? C23 C24 C25 120.2(5) . . ? C24 C25 C26 118.4(5) . . ? C24 C25 C27 121.6(5) . . ? C26 C25 C27 119.8(5) . . ? C25 C26 C21 121.8(5) . . ? C13 C27 C25 109.4(4) . . ? C16 C28 C30 123.2(6) . . ? C16 C28 C29 121.9(6) . . ? C30 C28 C29 114.9(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.364 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.102 #===END data_br13_20 _database_code_CSD 168778 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H14 Co4 O12 S' _chemical_formula_weight 750.12 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.4898(2) _cell_length_b 27.3932(4) _cell_length_c 16.8607(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.6450(10) _cell_angle_gamma 90.00 _cell_volume 5669.37(14) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max .36 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 2.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 38439 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 21.98 _reflns_number_total 6925 _reflns_number_gt 5137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0219P)^2^+8.1250P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6925 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.175 _refine_ls_shift/su_mean 0.007 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_1 Co -0.27140(5) 0.77108(3) 0.17013(4) 0.0370(2) Uani 1 1 d . . . Co2_1 Co -0.17506(5) 0.73848(2) 0.06665(4) 0.02791(18) Uani 1 1 d . . . Co3_1 Co 0.26456(5) 0.73983(3) 0.45856(4) 0.0361(2) Uani 1 1 d . . . Co4_1 Co 0.37389(5) 0.78224(3) 0.37166(4) 0.03446(19) Uani 1 1 d . . . S1_1 S -0.00760(10) 0.80263(5) 0.31453(7) 0.0346(3) Uani 1 1 d . . . C1_1 C -0.1586(4) 0.72010(19) 0.1809(3) 0.0320(13) Uani 1 1 d . . . C2_1 C -0.1136(4) 0.76362(18) 0.1742(3) 0.0284(12) Uani 1 1 d . . . C3_1 C -0.0165(4) 0.79368(18) 0.2060(3) 0.0328(13) Uani 1 1 d . . . H3A_1 H -0.0223 0.8257 0.1783 0.039 Uiso 1 1 calc R . . H3B_1 H 0.0500 0.7771 0.1957 0.039 Uiso 1 1 calc R . . C4_1 C 0.1341(4) 0.82101(17) 0.3430(3) 0.0351(13) Uani 1 1 d . . . H4A_1 H 0.1539 0.8403 0.2981 0.042 Uiso 1 1 calc R . . H4B_1 H 0.1409 0.8428 0.3905 0.042 Uiso 1 1 calc R . . C5_1 C 0.2140(4) 0.78045(19) 0.3627(3) 0.0319(13) Uani 1 1 d . . . C6_1 C 0.2505(4) 0.73706(19) 0.3411(3) 0.0341(13) Uani 1 1 d . . . C7_1 C 0.2239(5) 0.6972(2) 0.2803(3) 0.0596(19) Uani 1 1 d . . . H7A_1 H 0.2797 0.6712 0.2918 0.072 Uiso 1 1 calc R . . H7B_1 H 0.2256 0.7103 0.2258 0.072 Uiso 1 1 calc R . . C8_1 C 0.1070(7) 0.6747(2) 0.2818(4) 0.097(3) Uani 1 1 d . . . H8A_1 H 0.1157 0.6479 0.3219 0.117 Uiso 1 1 calc R . . H8B_1 H 0.0617 0.7003 0.3009 0.117 Uiso 1 1 calc R . . C9_1 C 0.0509(6) 0.6567(3) 0.2094(5) 0.089(2) Uani 1 1 d . . . H9A_1 H 0.0943 0.6297 0.1925 0.107 Uiso 1 1 calc R . . H9B_1 H 0.0474 0.6828 0.1685 0.107 Uiso 1 1 calc R . . C10_1 C -0.0605(5) 0.6386(2) 0.2072(4) 0.074(2) Uani 1 1 d . . . H10A_1 H -0.0558 0.6108 0.2451 0.089 Uiso 1 1 calc R . . H10B_1 H -0.0872 0.6255 0.1524 0.089 Uiso 1 1 calc R . . C11_1 C -0.1468(4) 0.67339(19) 0.2269(3) 0.0433(15) Uani 1 1 d . . . H11A_1 H -0.2179 0.6563 0.2167 0.052 Uiso 1 1 calc R . . H11B_1 H -0.1293 0.6811 0.2853 0.052 Uiso 1 1 calc R . . C15_1 C -0.3936(5) 0.7343(3) 0.1475(4) 0.0617(19) Uani 1 1 d . . . O15_1 O -0.4675(4) 0.7098(2) 0.1355(4) 0.111(2) Uani 1 1 d . . . C16_1 C -0.3058(5) 0.8302(2) 0.1249(4) 0.0577(17) Uani 1 1 d . . . O16_1 O -0.3262(4) 0.86734(18) 0.0970(3) 0.1015(19) Uani 1 1 d . . . C17_1 C -0.2754(4) 0.7852(2) 0.2726(4) 0.0543(17) Uani 1 1 d . . . O17_1 O -0.2809(4) 0.7942(2) 0.3376(3) 0.0867(16) Uani 1 1 d . . . C25_1 C -0.2749(4) 0.6943(2) 0.0200(3) 0.0354(13) Uani 1 1 d . . . O25_1 O -0.3372(3) 0.66554(14) -0.0057(2) 0.0542(11) Uani 1 1 d . . . C26_1 C -0.1890(4) 0.7905(2) -0.0013(3) 0.0410(14) Uani 1 1 d . . . O26_1 O -0.1961(3) 0.82305(16) -0.0434(3) 0.0693(13) Uani 1 1 d . . . C27_1 C -0.0552(5) 0.71495(19) 0.0374(3) 0.0378(14) Uani 1 1 d . . . O27_1 O 0.0220(3) 0.70104(14) 0.0178(3) 0.0585(12) Uani 1 1 d . . . C35_1 C 0.2774(4) 0.7849(2) 0.5397(4) 0.0469(16) Uani 1 1 d . . . O35_1 O 0.2839(4) 0.81427(18) 0.5870(3) 0.0738(14) Uani 1 1 d . . . C36_1 C 0.3575(5) 0.6909(2) 0.4970(3) 0.0532(17) Uani 1 1 d . . . O36_1 O 0.4147(4) 0.65962(17) 0.5199(3) 0.0789(15) Uani 1 1 d . . . C37_1 C 0.1410(5) 0.7097(2) 0.4706(4) 0.0488(16) Uani 1 1 d . . . O37_1 O 0.0624(3) 0.69069(15) 0.4779(3) 0.0702(13) Uani 1 1 d . . . C45_1 C 0.4036(4) 0.8388(2) 0.4265(3) 0.0409(14) Uani 1 1 d . . . O45_1 O 0.4151(3) 0.87515(16) 0.4600(3) 0.0659(13) Uani 1 1 d . . . C46_1 C 0.4919(5) 0.7438(2) 0.3955(4) 0.0544(17) Uani 1 1 d . . . O46_1 O 0.5642(4) 0.71783(16) 0.4116(3) 0.0849(16) Uani 1 1 d . . . C47_1 C 0.3894(5) 0.8004(2) 0.2728(4) 0.0595(18) Uani 1 1 d . . . O47_1 O 0.3967(5) 0.80953(19) 0.2081(3) 0.1008(19) Uani 1 1 d . . . Co1_2 Co 0.28607(5) 0.50183(2) 0.07705(4) 0.03166(18) Uani 1 1 d . . . Co2_2 Co 0.16034(5) 0.46192(2) 0.15395(4) 0.03088(19) Uani 1 1 d . . . Co3_2 Co 0.80775(5) 0.47186(3) 0.32579(4) 0.03467(19) Uani 1 1 d . . . Co4_2 Co 0.74711(5) 0.50100(2) 0.44864(4) 0.03254(19) Uani 1 1 d . . . S1_2 S 0.54055(10) 0.43556(5) 0.21480(7) 0.0314(3) Uani 1 1 d . . . C1_2 C 0.2890(4) 0.50246(18) 0.1943(3) 0.0291(12) Uani 1 1 d . . . C2_2 C 0.3208(4) 0.45874(18) 0.1710(3) 0.0279(12) Uani 1 1 d . . . C3_2 C 0.3974(4) 0.41784(17) 0.1938(3) 0.0329(13) Uani 1 1 d . . . H3A_2 H 0.3863 0.3936 0.1495 0.039 Uiso 1 1 calc R . . H3B_2 H 0.3796 0.4017 0.2423 0.039 Uiso 1 1 calc R . . C4_2 C 0.5585(4) 0.44914(18) 0.3225(3) 0.0307(13) Uani 1 1 d . . . H4A_2 H 0.4941 0.4669 0.3340 0.037 Uiso 1 1 calc R . . H4B_2 H 0.5662 0.4184 0.3539 0.037 Uiso 1 1 calc R . . C5_2 C 0.6579(4) 0.47962(18) 0.3461(3) 0.0271(12) Uani 1 1 d . . . C6_2 C 0.6996(4) 0.52351(19) 0.3366(3) 0.0297(12) Uani 1 1 d . . . C7_2 C 0.6794(4) 0.57252(18) 0.2979(3) 0.0419(15) Uani 1 1 d . . . H7A_2 H 0.6514 0.5679 0.2395 0.050 Uiso 1 1 calc R . . H7B_2 H 0.7497 0.5901 0.3035 0.050 Uiso 1 1 calc R . . C8_2 C 0.5981(4) 0.60461(19) 0.3333(4) 0.0506(16) Uani 1 1 d . . . H8A_2 H 0.6323 0.6136 0.3891 0.061 Uiso 1 1 calc R . . H8B_2 H 0.5866 0.6352 0.3015 0.061 Uiso 1 1 calc R . . C9_2 C 0.4879(4) 0.5823(2) 0.3355(3) 0.0475(15) Uani 1 1 d . . . H9A_2 H 0.4976 0.5552 0.3749 0.057 Uiso 1 1 calc R . . H9B_2 H 0.4415 0.6073 0.3548 0.057 Uiso 1 1 calc R . . C10_2 C 0.4299(4) 0.56327(19) 0.2556(3) 0.0464(15) Uani 1 1 d . . . H10A_2 H 0.4767 0.5387 0.2357 0.056 Uiso 1 1 calc R . . H10B_2 H 0.4189 0.5905 0.2163 0.056 Uiso 1 1 calc R . . C11_2 C 0.3181(4) 0.53979(19) 0.2588(3) 0.0410(14) Uani 1 1 d . . . H11A_2 H 0.3206 0.5243 0.3121 0.049 Uiso 1 1 calc R . . H11B_2 H 0.2614 0.5655 0.2521 0.049 Uiso 1 1 calc R . . C15_2 C 0.2062(4) 0.5555(2) 0.0400(3) 0.0431(15) Uani 1 1 d . . . O15_2 O 0.1555(4) 0.58875(16) 0.0178(3) 0.0711(14) Uani 1 1 d . . . C16_2 C 0.2710(4) 0.4610(2) -0.0107(3) 0.0393(14) Uani 1 1 d . . . O16_2 O 0.2617(3) 0.43573(15) -0.0641(2) 0.0558(11) Uani 1 1 d . . . C17_2 C 0.4188(5) 0.5251(2) 0.0726(3) 0.0433(15) Uani 1 1 d . . . O17_2 O 0.5030(3) 0.53998(15) 0.0697(2) 0.0585(12) Uani 1 1 d . . . C25_2 C 0.0489(4) 0.5054(2) 0.1326(4) 0.0466(15) Uani 1 1 d . . . O25_2 O -0.0194(4) 0.53266(16) 0.1178(3) 0.0850(16) Uani 1 1 d . . . C26_2 C 0.1215(4) 0.4120(2) 0.0843(4) 0.0412(14) Uani 1 1 d . . . O26_2 O 0.1018(4) 0.38149(16) 0.0388(3) 0.0720(14) Uani 1 1 d . . . C27_2 C 0.1348(4) 0.4355(2) 0.2455(4) 0.0467(15) Uani 1 1 d . . . O27_2 O 0.1189(4) 0.41897(18) 0.3041(3) 0.0836(15) Uani 1 1 d . . . C35_2 C 0.8330(5) 0.4085(2) 0.3538(3) 0.0489(16) Uani 1 1 d . . . O35_2 O 0.8414(4) 0.36840(18) 0.3702(3) 0.0822(16) Uani 1 1 d . . . C36_2 C 0.9368(5) 0.5040(2) 0.3397(3) 0.0479(15) Uani 1 1 d . . . O36_2 O 1.0160(3) 0.52502(17) 0.3478(3) 0.0706(13) Uani 1 1 d . . . C37_2 C 0.7908(4) 0.4646(2) 0.2191(4) 0.0439(15) Uani 1 1 d . . . O37_2 O 0.7841(3) 0.45905(17) 0.1510(3) 0.0703(13) Uani 1 1 d . . . C45_2 C 0.7768(4) 0.4462(2) 0.5088(3) 0.0431(15) Uani 1 1 d . . . O45_2 O 0.7917(4) 0.41127(16) 0.5453(3) 0.0743(14) Uani 1 1 d . . . C46_2 C 0.8569(5) 0.5438(2) 0.4847(3) 0.0447(15) Uani 1 1 d . . . O46_2 O 0.9248(3) 0.57080(16) 0.5058(3) 0.0684(13) Uani 1 1 d . . . C47_2 C 0.6463(5) 0.5254(2) 0.4999(3) 0.0421(15) Uani 1 1 d . . . O47_2 O 0.5825(3) 0.53973(16) 0.5341(3) 0.0676(13) 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_1 0.0288(4) 0.0448(5) 0.0364(4) -0.0040(4) 0.0033(3) 0.0008(3) Co2_1 0.0259(4) 0.0293(4) 0.0259(4) 0.0009(3) -0.0021(3) -0.0026(3) Co3_1 0.0252(4) 0.0447(5) 0.0365(4) 0.0075(4) 0.0006(3) 0.0055(3) Co4_1 0.0264(4) 0.0414(5) 0.0349(4) -0.0069(4) 0.0041(3) -0.0011(3) S1_1 0.0278(8) 0.0430(9) 0.0299(8) -0.0068(6) -0.0027(6) 0.0057(6) C1_1 0.028(3) 0.038(4) 0.027(3) 0.004(3) -0.003(2) -0.004(3) C2_1 0.026(3) 0.032(3) 0.026(3) 0.002(2) 0.002(2) 0.000(3) C3_1 0.032(3) 0.034(3) 0.029(3) -0.002(2) -0.002(2) -0.003(3) C4_1 0.033(3) 0.028(3) 0.038(3) -0.009(3) -0.011(3) 0.002(2) C5_1 0.022(3) 0.039(4) 0.031(3) 0.002(3) -0.006(2) -0.006(3) C6_1 0.029(3) 0.033(3) 0.035(3) 0.001(3) -0.007(2) 0.000(3) C7_1 0.086(5) 0.038(4) 0.043(4) -0.010(3) -0.020(3) 0.012(3) C8_1 0.158(8) 0.069(5) 0.051(4) -0.002(4) -0.016(5) -0.093(5) C9_1 0.060(5) 0.094(6) 0.106(7) 0.038(5) -0.005(5) 0.006(4) C10_1 0.055(5) 0.066(5) 0.100(6) 0.044(4) 0.008(4) 0.014(4) C11_1 0.039(3) 0.041(4) 0.044(4) 0.019(3) -0.006(3) -0.006(3) C15_1 0.033(4) 0.084(5) 0.070(5) -0.019(4) 0.015(3) -0.006(4) O15_1 0.044(3) 0.138(5) 0.153(5) -0.048(4) 0.025(3) -0.041(3) C16_1 0.056(4) 0.049(4) 0.064(5) -0.005(4) 0.000(3) 0.012(3) O16_1 0.116(4) 0.056(3) 0.126(5) 0.013(3) 0.008(4) 0.041(3) C17_1 0.035(4) 0.076(5) 0.053(4) -0.003(4) 0.012(3) 0.003(3) O17_1 0.078(4) 0.141(5) 0.048(3) -0.017(3) 0.029(3) 0.005(3) C25_1 0.030(3) 0.040(4) 0.032(3) -0.002(3) -0.005(3) 0.001(3) O25_1 0.047(3) 0.048(3) 0.063(3) -0.011(2) -0.001(2) -0.016(2) C26_1 0.027(3) 0.050(4) 0.042(4) 0.007(3) -0.003(3) -0.003(3) O26_1 0.055(3) 0.068(3) 0.080(3) 0.046(3) -0.002(2) -0.002(2) C27_1 0.037(4) 0.035(3) 0.038(3) -0.006(3) -0.001(3) -0.011(3) O27_1 0.041(3) 0.050(3) 0.088(3) -0.017(2) 0.020(2) -0.005(2) C35_1 0.031(4) 0.071(5) 0.036(4) 0.010(3) -0.001(3) 0.011(3) O35_1 0.070(3) 0.100(4) 0.051(3) -0.026(3) 0.011(2) 0.011(3) C36_1 0.041(4) 0.069(5) 0.046(4) 0.009(3) -0.002(3) 0.005(3) O36_1 0.062(3) 0.080(4) 0.087(4) 0.025(3) -0.004(3) 0.033(3) C37_1 0.040(4) 0.042(4) 0.063(4) 0.013(3) 0.006(3) 0.009(3) O37_1 0.048(3) 0.057(3) 0.110(4) 0.024(3) 0.025(3) -0.001(2) C45_1 0.030(3) 0.046(4) 0.045(4) 0.000(3) 0.003(3) 0.000(3) O45_1 0.070(3) 0.054(3) 0.071(3) -0.019(3) 0.005(2) -0.008(2) C46_1 0.038(4) 0.049(4) 0.078(5) -0.014(4) 0.014(3) -0.009(3) O46_1 0.038(3) 0.061(3) 0.151(5) -0.014(3) 0.005(3) 0.011(2) C47_1 0.063(5) 0.057(4) 0.063(5) -0.015(4) 0.024(4) -0.008(3) O47_1 0.150(5) 0.109(4) 0.055(3) 0.002(3) 0.050(3) -0.009(4) Co1_2 0.0265(4) 0.0358(4) 0.0314(4) 0.0039(3) 0.0022(3) -0.0007(3) Co2_2 0.0247(4) 0.0317(4) 0.0360(4) -0.0016(3) 0.0051(3) -0.0009(3) Co3_2 0.0317(4) 0.0425(5) 0.0286(4) 0.0024(4) 0.0022(3) 0.0008(3) Co4_2 0.0372(4) 0.0336(4) 0.0245(4) 0.0005(3) -0.0003(3) -0.0044(3) S1_2 0.0280(8) 0.0351(8) 0.0296(8) -0.0047(6) 0.0009(6) 0.0042(6) C1_2 0.025(3) 0.032(3) 0.029(3) 0.004(3) 0.002(2) -0.004(2) C2_2 0.022(3) 0.030(3) 0.031(3) -0.002(2) 0.002(2) 0.001(2) C3_2 0.032(3) 0.027(3) 0.036(3) -0.005(2) -0.003(3) -0.004(2) C4_2 0.036(3) 0.030(3) 0.026(3) -0.001(2) 0.003(2) -0.001(2) C5_2 0.030(3) 0.025(3) 0.024(3) -0.001(2) 0.001(2) -0.003(2) C6_2 0.028(3) 0.032(3) 0.027(3) 0.003(3) 0.000(2) -0.001(2) C7_2 0.045(4) 0.031(3) 0.046(4) 0.014(3) -0.001(3) -0.010(3) C8_2 0.054(4) 0.028(3) 0.063(4) 0.003(3) -0.006(3) 0.003(3) C9_2 0.044(4) 0.041(4) 0.054(4) -0.009(3) 0.000(3) 0.001(3) C10_2 0.063(4) 0.028(3) 0.047(4) 0.001(3) 0.006(3) -0.008(3) C11_2 0.043(4) 0.039(4) 0.038(3) -0.011(3) 0.000(3) 0.003(3) C15_2 0.035(4) 0.053(4) 0.040(4) 0.007(3) 0.005(3) -0.006(3) O15_2 0.068(3) 0.059(3) 0.086(3) 0.027(3) 0.012(3) 0.026(3) C16_2 0.031(3) 0.044(4) 0.042(4) 0.008(3) 0.007(3) 0.003(3) O16_2 0.053(3) 0.065(3) 0.050(3) -0.019(2) 0.013(2) -0.007(2) C17_2 0.039(4) 0.050(4) 0.040(3) 0.006(3) 0.007(3) -0.001(3) O17_2 0.036(3) 0.075(3) 0.065(3) 0.015(2) 0.011(2) -0.011(2) C25_2 0.029(3) 0.043(4) 0.070(4) 0.003(3) 0.014(3) -0.004(3) O25_2 0.046(3) 0.063(3) 0.147(5) 0.015(3) 0.021(3) 0.025(3) C26_2 0.031(3) 0.039(4) 0.054(4) -0.004(3) 0.011(3) -0.007(3) O26_2 0.086(3) 0.053(3) 0.081(3) -0.030(3) 0.027(3) -0.030(3) C27_2 0.040(4) 0.049(4) 0.053(4) -0.007(3) 0.013(3) 0.001(3) O27_2 0.107(4) 0.090(4) 0.064(3) 0.019(3) 0.043(3) 0.003(3) C35_2 0.052(4) 0.056(5) 0.040(4) -0.003(3) 0.012(3) 0.011(3) O35_2 0.126(4) 0.051(3) 0.075(3) 0.010(3) 0.033(3) 0.035(3) C36_2 0.039(4) 0.061(4) 0.042(4) 0.000(3) 0.001(3) 0.008(3) O36_2 0.041(3) 0.093(4) 0.076(3) -0.005(3) 0.007(2) -0.019(3) C37_2 0.042(4) 0.050(4) 0.041(4) 0.009(3) 0.009(3) -0.003(3) O37_2 0.070(3) 0.106(4) 0.037(3) 0.001(3) 0.017(2) -0.011(3) C45_2 0.051(4) 0.043(4) 0.032(3) -0.005(3) -0.001(3) -0.004(3) O45_2 0.119(4) 0.044(3) 0.053(3) 0.019(2) -0.003(3) -0.004(3) C46_2 0.043(4) 0.049(4) 0.039(4) -0.003(3) -0.002(3) 0.000(3) O46_2 0.057(3) 0.069(3) 0.070(3) -0.007(2) -0.011(2) -0.027(3) C47_2 0.049(4) 0.042(4) 0.033(3) -0.013(3) 0.000(3) -0.019(3) O47_2 0.067(3) 0.081(3) 0.061(3) -0.026(3) 0.031(3) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1_1 C17_1 1.780(7) . ? Co1_1 C16_1 1.808(7) . ? Co1_1 C15_1 1.810(7) . ? Co1_1 C1_1 1.968(5) . ? Co1_1 C2_1 1.970(5) . ? Co1_1 Co2_1 2.4627(9) . ? Co2_1 C27_1 1.781(6) . ? Co2_1 C25_1 1.811(6) . ? Co2_1 C26_1 1.816(6) . ? Co2_1 C2_1 1.960(5) . ? Co2_1 C1_1 1.966(5) . ? Co3_1 C37_1 1.794(6) . ? Co3_1 C36_1 1.813(7) . ? Co3_1 C35_1 1.828(7) . ? Co3_1 C6_1 1.958(5) . ? Co3_1 C5_1 1.968(5) . ? Co3_1 Co4_1 2.4699(10) . ? Co4_1 C47_1 1.784(7) . ? Co4_1 C46_1 1.795(7) . ? Co4_1 C45_1 1.806(6) . ? Co4_1 C6_1 1.970(5) . ? Co4_1 C5_1 1.975(5) . ? S1_1 C4_1 1.817(5) . ? S1_1 C3_1 1.829(5) . ? C1_1 C2_1 1.332(6) . ? C1_1 C11_1 1.489(7) . ? C2_1 C3_1 1.481(6) . ? C4_1 C5_1 1.490(7) . ? C5_1 C6_1 1.347(7) . ? C6_1 C7_1 1.492(7) . ? C7_1 C8_1 1.590(9) . ? C8_1 C9_1 1.381(8) . ? C9_1 C10_1 1.470(8) . ? C10_1 C11_1 1.522(8) . ? C15_1 O15_1 1.128(7) . ? C16_1 O16_1 1.130(7) . ? C17_1 O17_1 1.138(6) . ? C25_1 O25_1 1.135(5) . ? C26_1 O26_1 1.134(6) . ? C27_1 O27_1 1.141(6) . ? C35_1 O35_1 1.125(6) . ? C36_1 O36_1 1.136(6) . ? C37_1 O37_1 1.138(6) . ? C45_1 O45_1 1.142(6) . ? C46_1 O46_1 1.143(6) . ? C47_1 O47_1 1.139(7) . ? Co1_2 C17_2 1.791(6) . ? Co1_2 C15_2 1.820(6) . ? Co1_2 C16_2 1.835(6) . ? Co1_2 C2_2 1.959(5) . ? Co1_2 C1_2 1.971(5) . ? Co1_2 Co2_2 2.4688(9) . ? Co2_2 C27_2 1.785(7) . ? Co2_2 C26_2 1.810(6) . ? Co2_2 C25_2 1.817(6) . ? Co2_2 C1_2 1.968(5) . ? Co2_2 C2_2 1.974(4) . ? Co3_2 C37_2 1.784(6) . ? Co3_2 C35_2 1.811(7) . ? Co3_2 C36_2 1.814(7) . ? Co3_2 C5_2 1.975(5) . ? Co3_2 C6_2 1.987(5) . ? Co3_2 Co4_2 2.4659(9) . ? Co4_2 C47_2 1.784(6) . ? Co4_2 C45_2 1.812(6) . ? Co4_2 C46_2 1.821(6) . ? Co4_2 C5_2 1.965(5) . ? Co4_2 C6_2 1.972(5) . ? S1_2 C3_2 1.824(5) . ? S1_2 C4_2 1.826(4) . ? C1_2 C2_2 1.343(6) . ? C1_2 C11_2 1.488(7) . ? C2_2 C3_2 1.477(6) . ? C4_2 C5_2 1.488(6) . ? C5_2 C6_2 1.332(6) . ? C6_2 C7_2 1.493(7) . ? C7_2 C8_2 1.544(7) . ? C8_2 C9_2 1.512(7) . ? C9_2 C10_2 1.501(7) . ? C10_2 C11_2 1.547(7) . ? C15_2 O15_2 1.134(6) . ? C16_2 O16_2 1.125(6) . ? C17_2 O17_2 1.137(6) . ? C25_2 O25_2 1.127(6) . ? C26_2 O26_2 1.130(6) . ? C27_2 O27_2 1.139(6) . ? C35_2 O35_2 1.133(6) . ? C36_2 O36_2 1.131(6) . ? C37_2 O37_2 1.145(6) . ? C45_2 O45_2 1.134(6) . ? C46_2 O46_2 1.133(6) . ? C47_2 O47_2 1.136(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17_1 Co1_1 C16_1 99.6(3) . . ? C17_1 Co1_1 C15_1 98.7(3) . . ? C16_1 Co1_1 C15_1 106.6(3) . . ? C17_1 Co1_1 C1_1 102.2(2) . . ? C16_1 Co1_1 C1_1 141.7(2) . . ? C15_1 Co1_1 C1_1 100.7(3) . . ? C17_1 Co1_1 C2_1 101.3(2) . . ? C16_1 Co1_1 C2_1 105.4(2) . . ? C15_1 Co1_1 C2_1 138.5(2) . . ? C1_1 Co1_1 C2_1 39.54(18) . . ? C17_1 Co1_1 Co2_1 150.60(19) . . ? C16_1 Co1_1 Co2_1 97.8(2) . . ? C15_1 Co1_1 Co2_1 98.77(19) . . ? C1_1 Co1_1 Co2_1 51.19(14) . . ? C2_1 Co1_1 Co2_1 51.00(14) . . ? C27_1 Co2_1 C25_1 100.6(2) . . ? C27_1 Co2_1 C26_1 95.6(2) . . ? C25_1 Co2_1 C26_1 105.8(2) . . ? C27_1 Co2_1 C2_1 100.2(2) . . ? C25_1 Co2_1 C2_1 139.3(2) . . ? C26_1 Co2_1 C2_1 106.5(2) . . ? C27_1 Co2_1 C1_1 103.8(2) . . ? C25_1 Co2_1 C1_1 101.2(2) . . ? C26_1 Co2_1 C1_1 143.1(2) . . ? C2_1 Co2_1 C1_1 39.68(19) . . ? C27_1 Co2_1 Co1_1 150.82(17) . . ? C25_1 Co2_1 Co1_1 99.39(16) . . ? C26_1 Co2_1 Co1_1 99.19(17) . . ? C2_1 Co2_1 Co1_1 51.39(14) . . ? C1_1 Co2_1 Co1_1 51.28(15) . . ? C37_1 Co3_1 C36_1 97.3(3) . . ? C37_1 Co3_1 C35_1 100.6(3) . . ? C36_1 Co3_1 C35_1 105.7(3) . . ? C37_1 Co3_1 C6_1 100.2(2) . . ? C36_1 Co3_1 C6_1 105.4(2) . . ? C35_1 Co3_1 C6_1 139.7(2) . . ? C37_1 Co3_1 C5_1 101.6(2) . . ? C36_1 Co3_1 C5_1 143.0(2) . . ? C35_1 Co3_1 C5_1 101.7(2) . . ? C6_1 Co3_1 C5_1 40.13(19) . . ? C37_1 Co3_1 Co4_1 149.84(19) . . ? C36_1 Co3_1 Co4_1 99.94(19) . . ? C35_1 Co3_1 Co4_1 98.31(18) . . ? C6_1 Co3_1 Co4_1 51.26(15) . . ? C5_1 Co3_1 Co4_1 51.33(14) . . ? C47_1 Co4_1 C46_1 98.4(3) . . ? C47_1 Co4_1 C45_1 101.1(3) . . ? C46_1 Co4_1 C45_1 107.8(2) . . ? C47_1 Co4_1 C6_1 98.3(2) . . ? C46_1 Co4_1 C6_1 105.1(2) . . ? C45_1 Co4_1 C6_1 138.5(2) . . ? C47_1 Co4_1 C5_1 102.6(2) . . ? C46_1 Co4_1 C5_1 141.1(2) . . ? C45_1 Co4_1 C5_1 99.8(2) . . ? C6_1 Co4_1 C5_1 39.93(19) . . ? C47_1 Co4_1 Co3_1 148.5(2) . . ? C46_1 Co4_1 Co3_1 96.41(19) . . ? C45_1 Co4_1 Co3_1 100.57(17) . . ? C6_1 Co4_1 Co3_1 50.81(15) . . ? C5_1 Co4_1 Co3_1 51.09(14) . . ? C4_1 S1_1 C3_1 100.2(2) . . ? C2_1 C1_1 C11_1 144.1(5) . . ? C2_1 C1_1 Co2_1 69.9(3) . . ? C11_1 C1_1 Co2_1 135.5(4) . . ? C2_1 C1_1 Co1_1 70.3(3) . . ? C11_1 C1_1 Co1_1 131.2(4) . . ? Co2_1 C1_1 Co1_1 77.53(18) . . ? C1_1 C2_1 C3_1 142.9(5) . . ? C1_1 C2_1 Co2_1 70.4(3) . . ? C3_1 C2_1 Co2_1 133.2(3) . . ? C1_1 C2_1 Co1_1 70.1(3) . . ? C3_1 C2_1 Co1_1 134.6(4) . . ? Co2_1 C2_1 Co1_1 77.60(17) . . ? C2_1 C3_1 S1_1 109.3(3) . . ? C5_1 C4_1 S1_1 115.6(3) . . ? C6_1 C5_1 C4_1 147.5(5) . . ? C6_1 C5_1 Co3_1 69.5(3) . . ? C4_1 C5_1 Co3_1 134.8(4) . . ? C6_1 C5_1 Co4_1 69.9(3) . . ? C4_1 C5_1 Co4_1 128.7(4) . . ? Co3_1 C5_1 Co4_1 77.58(17) . . ? C5_1 C6_1 C7_1 142.0(5) . . ? C5_1 C6_1 Co3_1 70.3(3) . . ? C7_1 C6_1 Co3_1 133.7(4) . . ? C5_1 C6_1 Co4_1 70.2(3) . . ? C7_1 C6_1 Co4_1 134.7(4) . . ? Co3_1 C6_1 Co4_1 77.92(18) . . ? C6_1 C7_1 C8_1 111.1(5) . . ? C9_1 C8_1 C7_1 116.3(6) . . ? C8_1 C9_1 C10_1 117.8(7) . . ? C9_1 C10_1 C11_1 119.2(6) . . ? C1_1 C11_1 C10_1 115.5(5) . . ? O15_1 C15_1 Co1_1 177.1(7) . . ? O16_1 C16_1 Co1_1 179.2(7) . . ? O17_1 C17_1 Co1_1 178.2(5) . . ? O25_1 C25_1 Co2_1 176.7(5) . . ? O26_1 C26_1 Co2_1 179.0(5) . . ? O27_1 C27_1 Co2_1 178.2(5) . . ? O35_1 C35_1 Co3_1 176.8(5) . . ? O36_1 C36_1 Co3_1 178.6(6) . . ? O37_1 C37_1 Co3_1 179.7(6) . . ? O45_1 C45_1 Co4_1 175.4(5) . . ? O46_1 C46_1 Co4_1 177.2(6) . . ? O47_1 C47_1 Co4_1 176.2(6) . . ? C17_2 Co1_2 C15_2 98.7(2) . . ? C17_2 Co1_2 C16_2 98.1(2) . . ? C15_2 Co1_2 C16_2 104.3(2) . . ? C17_2 Co1_2 C2_2 100.4(2) . . ? C15_2 Co1_2 C2_2 142.1(2) . . ? C16_2 Co1_2 C2_2 105.0(2) . . ? C17_2 Co1_2 C1_2 101.1(2) . . ? C15_2 Co1_2 C1_2 104.1(2) . . ? C16_2 Co1_2 C1_2 142.5(2) . . ? C2_2 Co1_2 C1_2 39.98(18) . . ? C17_2 Co1_2 Co2_2 149.69(17) . . ? C15_2 Co1_2 Co2_2 100.14(17) . . ? C16_2 Co1_2 Co2_2 99.95(16) . . ? C2_2 Co1_2 Co2_2 51.38(13) . . ? C1_2 Co1_2 Co2_2 51.14(13) . . ? C27_2 Co2_2 C26_2 100.7(2) . . ? C27_2 Co2_2 C25_2 100.6(3) . . ? C26_2 Co2_2 C25_2 105.3(2) . . ? C27_2 Co2_2 C1_2 101.2(2) . . ? C26_2 Co2_2 C1_2 139.0(2) . . ? C25_2 Co2_2 C1_2 104.2(2) . . ? C27_2 Co2_2 C2_2 101.2(2) . . ? C26_2 Co2_2 C2_2 101.8(2) . . ? C25_2 Co2_2 C2_2 141.1(2) . . ? C1_2 Co2_2 C2_2 39.86(18) . . ? C27_2 Co2_2 Co1_2 149.98(18) . . ? C26_2 Co2_2 Co1_2 96.57(17) . . ? C25_2 Co2_2 Co1_2 98.28(17) . . ? C1_2 Co2_2 Co1_2 51.23(13) . . ? C2_2 Co2_2 Co1_2 50.86(14) . . ? C37_2 Co3_2 C35_2 97.9(2) . . ? C37_2 Co3_2 C36_2 97.0(2) . . ? C35_2 Co3_2 C36_2 108.9(3) . . ? C37_2 Co3_2 C5_2 104.3(2) . . ? C35_2 Co3_2 C5_2 100.5(2) . . ? C36_2 Co3_2 C5_2 140.6(2) . . ? C37_2 Co3_2 C6_2 102.5(2) . . ? C35_2 Co3_2 C6_2 138.3(2) . . ? C36_2 Co3_2 C6_2 104.2(2) . . ? C5_2 Co3_2 C6_2 39.27(18) . . ? C37_2 Co3_2 Co4_2 152.39(18) . . ? C35_2 Co3_2 Co4_2 99.04(17) . . ? C36_2 Co3_2 Co4_2 97.92(18) . . ? C5_2 Co3_2 Co4_2 51.06(13) . . ? C6_2 Co3_2 Co4_2 51.21(13) . . ? C47_2 Co4_2 C45_2 97.4(3) . . ? C47_2 Co4_2 C46_2 98.8(2) . . ? C45_2 Co4_2 C46_2 106.4(2) . . ? C47_2 Co4_2 C5_2 101.6(2) . . ? C45_2 Co4_2 C5_2 105.6(2) . . ? C46_2 Co4_2 C5_2 139.1(2) . . ? C47_2 Co4_2 C6_2 103.5(2) . . ? C45_2 Co4_2 C6_2 142.2(2) . . ? C46_2 Co4_2 C6_2 101.2(2) . . ? C5_2 Co4_2 C6_2 39.54(18) . . ? C47_2 Co4_2 Co3_2 151.91(17) . . ? C45_2 Co4_2 Co3_2 98.00(17) . . ? C46_2 Co4_2 Co3_2 99.17(17) . . ? C5_2 Co4_2 Co3_2 51.45(14) . . ? C6_2 Co4_2 Co3_2 51.76(14) . . ? C3_2 S1_2 C4_2 100.6(2) . . ? C2_2 C1_2 C11_2 141.3(5) . . ? C2_2 C1_2 Co2_2 70.3(3) . . ? C11_2 C1_2 Co2_2 135.6(4) . . ? C2_2 C1_2 Co1_2 69.6(3) . . ? C11_2 C1_2 Co1_2 134.1(4) . . ? Co2_2 C1_2 Co1_2 77.63(17) . . ? C1_2 C2_2 C3_2 144.4(5) . . ? C1_2 C2_2 Co1_2 70.5(3) . . ? C3_2 C2_2 Co1_2 134.7(4) . . ? C1_2 C2_2 Co2_2 69.8(3) . . ? C3_2 C2_2 Co2_2 131.5(3) . . ? Co1_2 C2_2 Co2_2 77.76(17) . . ? C2_2 C3_2 S1_2 114.4(3) . . ? C5_2 C4_2 S1_2 108.9(3) . . ? C6_2 C5_2 C4_2 143.1(5) . . ? C6_2 C5_2 Co4_2 70.5(3) . . ? C4_2 C5_2 Co4_2 135.5(3) . . ? C6_2 C5_2 Co3_2 70.9(3) . . ? C4_2 C5_2 Co3_2 131.5(3) . . ? Co4_2 C5_2 Co3_2 77.50(17) . . ? C5_2 C6_2 C7_2 145.7(5) . . ? C5_2 C6_2 Co4_2 69.9(3) . . ? C7_2 C6_2 Co4_2 134.1(4) . . ? C5_2 C6_2 Co3_2 69.9(3) . . ? C7_2 C6_2 Co3_2 131.5(4) . . ? Co4_2 C6_2 Co3_2 77.03(17) . . ? C6_2 C7_2 C8_2 114.4(4) . . ? C9_2 C8_2 C7_2 116.5(4) . . ? C10_2 C9_2 C8_2 114.2(5) . . ? C9_2 C10_2 C11_2 113.8(4) . . ? C1_2 C11_2 C10_2 111.2(4) . . ? O15_2 C15_2 Co1_2 179.0(5) . . ? O16_2 C16_2 Co1_2 179.5(5) . . ? O17_2 C17_2 Co1_2 179.8(6) . . ? O25_2 C25_2 Co2_2 178.4(6) . . ? O26_2 C26_2 Co2_2 176.2(5) . . ? O27_2 C27_2 Co2_2 179.5(6) . . ? O35_2 C35_2 Co3_2 175.4(6) . . ? O36_2 C36_2 Co3_2 178.4(6) . . ? O37_2 C37_2 Co3_2 177.2(5) . . ? O45_2 C45_2 Co4_2 177.6(5) . . ? O46_2 C46_2 Co4_2 178.7(5) . . ? O47_2 C47_2 Co4_2 177.9(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.888 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.077 #===END data_br21_22 _database_code_CSD 168779 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Co4 N O12' _chemical_formula_weight 747.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/c 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 16.2075(5) _cell_length_b 7.67660(10) _cell_length_c 24.2396(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.5940(10) _cell_angle_gamma 90.00 _cell_volume 2858.43(14) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max .50 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 2.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 'CCD area detector' _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 10055 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5772 _reflns_number_gt 3594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1101P)^2^+1.6017P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5772 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1634 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.35381(5) 0.09554(10) 0.06897(3) 0.0302(2) Uani 0.934(2) 1 d P A 1 Co2 Co 0.28018(5) 0.37931(10) 0.04191(3) 0.0290(2) Uani 0.934(2) 1 d P A 1 Co3 Co 0.19303(5) 0.09120(10) 0.27400(4) 0.0299(2) Uani 0.934(2) 1 d P A 1 Co4 Co 0.27153(5) 0.36932(10) 0.30248(3) 0.0287(2) Uani 0.934(2) 1 d P A 1 C1 C 0.3362(4) 0.2797(7) 0.1205(2) 0.0313(13) Uani 1 1 d . A 1 C2 C 0.2609(4) 0.2026(7) 0.0947(2) 0.0309(13) Uani 1 1 d . A 1 C3 C 0.1827(4) 0.1260(8) 0.1040(3) 0.0400(15) Uani 1 1 d . A 1 H3A H 0.1496 0.0626 0.0687 0.048 Uiso 1 1 calc R A 1 H3B H 0.2012 0.0415 0.1359 0.048 Uiso 1 1 calc R A 1 N4 N 0.1253(3) 0.2550(7) 0.1178(2) 0.0405(13) Uani 1 1 d . A 1 C5 C 0.1660(4) 0.3644(7) 0.1676(2) 0.0326(13) Uani 1 1 d . A 1 H5A H 0.1207 0.4355 0.1753 0.039 Uiso 1 1 calc R A 1 H5B H 0.2060 0.4441 0.1573 0.039 Uiso 1 1 calc R A 1 C6 C 0.2160(3) 0.2715(7) 0.2234(2) 0.0276(12) Uani 1 1 d . A 1 C7 C 0.2886(4) 0.1884(7) 0.2500(2) 0.0330(13) Uani 1 1 d . A 1 C8 C 0.3661(4) 0.1039(7) 0.2401(3) 0.0335(14) Uani 1 1 d . A 1 H8A H 0.3456 0.0209 0.2079 0.040 Uiso 1 1 calc R A 1 H8B H 0.3977 0.0377 0.2751 0.040 Uiso 1 1 calc R A 1 C9 C 0.4299(3) 0.2319(8) 0.2260(2) 0.0349(14) Uani 1 1 d . A 1 H9A H 0.4587 0.2992 0.2613 0.042 Uiso 1 1 calc R A 1 H9B H 0.4749 0.1636 0.2169 0.042 Uiso 1 1 calc R A 1 C10 C 0.3914(4) 0.3602(7) 0.1762(2) 0.0344(14) Uani 1 1 d . A 1 H10A H 0.3562 0.4459 0.1887 0.041 Uiso 1 1 calc R A 1 H10B H 0.4393 0.4232 0.1686 0.041 Uiso 1 1 calc R A 1 C11 C 0.0358(5) 0.2188(14) 0.1052(6) 0.127(5) Uani 1 1 d . A 1 H11 H 0.0358 0.1767 0.1438 0.152 Uiso 1 1 calc R A 1 C12 C -0.0042(6) 0.0781(17) 0.0710(6) 0.135(5) Uani 1 1 d . A 1 H12A H 0.0358 -0.0194 0.0783 0.203 Uiso 1 1 calc R A 1 H12B H -0.0207 0.1105 0.0303 0.203 Uiso 1 1 calc R A 1 H12C H -0.0558 0.0452 0.0806 0.203 Uiso 1 1 calc R A 1 C13 C -0.0205(6) 0.3735(16) 0.0992(7) 0.155(6) Uani 1 1 d . A 1 H13A H 0.0107 0.4637 0.1257 0.232 Uiso 1 1 calc R A 1 H13B H -0.0726 0.3422 0.1083 0.232 Uiso 1 1 calc R A 1 H13C H -0.0365 0.4164 0.0595 0.232 Uiso 1 1 calc R A 1 C15 C 0.3826(4) -0.0920(8) 0.1143(3) 0.0434(16) Uani 1 1 d . A 1 O15 O 0.4004(4) -0.2154(7) 0.1421(2) 0.0708(16) Uani 1 1 d . A 1 C16 C 0.4614(5) 0.1517(10) 0.0669(3) 0.0559(19) Uani 1 1 d . A 1 O16 O 0.5299(4) 0.1859(10) 0.0663(4) 0.109(3) Uani 1 1 d . A 1 C17 C 0.2973(5) -0.0172(9) 0.0023(3) 0.0507(18) Uani 1 1 d . A 1 O17 O 0.2609(4) -0.0933(7) -0.0389(2) 0.084(2) Uani 1 1 d . A 1 C25 C 0.2219(5) 0.5607(9) 0.0570(3) 0.0456(16) Uani 1 1 d . A 1 O25 O 0.1858(4) 0.6790(7) 0.0661(2) 0.0722(16) Uani 1 1 d . A 1 C26 C 0.3671(5) 0.4984(8) 0.0278(3) 0.0474(17) Uani 1 1 d . A 1 O26 O 0.4237(4) 0.5746(8) 0.0214(3) 0.0812(19) Uani 1 1 d . A 1 C27 C 0.2041(4) 0.3189(9) -0.0285(3) 0.0465(16) Uani 1 1 d . A 1 O27 O 0.1555(4) 0.2750(8) -0.0707(2) 0.0763(17) Uani 1 1 d . A 1 C35 C 0.1640(4) -0.0919(9) 0.2271(3) 0.0433(16) Uani 1 1 d . A 1 O35 O 0.1479(4) -0.2123(7) 0.1979(2) 0.0688(15) Uani 1 1 d . A 1 C36 C 0.0865(5) 0.1552(11) 0.2767(3) 0.057(2) Uani 1 1 d . A 1 O36 O 0.0210(4) 0.1978(11) 0.2793(3) 0.102(2) Uani 1 1 d . A 1 C37 C 0.2460(5) -0.0278(9) 0.3411(3) 0.0531(18) Uani 1 1 d . A 1 O37 O 0.2807(4) -0.0997(8) 0.3821(2) 0.087(2) Uani 1 1 d . A 1 C45 C 0.3267(4) 0.5583(9) 0.2874(3) 0.0460(16) Uani 1 1 d . A 1 O45 O 0.3598(4) 0.6784(6) 0.2786(3) 0.0705(16) Uani 1 1 d . A 1 C46 C 0.1873(5) 0.4838(9) 0.3200(3) 0.0450(16) Uani 1 1 d . A 1 O46 O 0.1307(4) 0.5601(8) 0.3285(2) 0.0762(17) Uani 1 1 d . A 1 C47 C 0.3503(5) 0.3044(9) 0.3716(3) 0.0539(18) Uani 1 1 d . A 1 O47 O 0.3997(4) 0.2622(8) 0.4139(2) 0.085(2) Uani 1 1 d . A 1 Co1B Co 0.2800(9) 0.1126(17) 0.0483(6) 0.042(4) Uiso 0.066(2) 1 d P A 2 Co2B Co 0.3603(9) 0.3894(16) 0.0747(6) 0.040(4) Uiso 0.066(2) 1 d P A 2 Co3B Co 0.2771(8) 0.1287(15) 0.3067(5) 0.035(4) Uiso 0.066(2) 1 d P A 2 Co4B Co 0.1945(9) 0.4053(17) 0.2782(6) 0.043(4) Uiso 0.066(2) 1 d P A 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 0.0338(5) 0.0286(4) 0.0288(5) 0.0013(3) 0.0108(4) 0.0049(3) Co2 0.0350(5) 0.0255(4) 0.0255(4) 0.0037(3) 0.0081(4) 0.0012(3) Co3 0.0321(5) 0.0284(4) 0.0316(5) 0.0017(3) 0.0134(4) -0.0030(3) Co4 0.0314(5) 0.0278(4) 0.0256(4) -0.0019(3) 0.0073(3) 0.0001(3) C1 0.032(3) 0.036(3) 0.028(3) 0.002(2) 0.011(2) 0.002(2) C2 0.034(3) 0.032(3) 0.023(3) 0.005(2) 0.004(2) 0.005(2) C3 0.039(4) 0.040(3) 0.039(3) -0.008(3) 0.010(3) -0.008(3) N4 0.021(2) 0.060(3) 0.039(3) -0.020(2) 0.006(2) 0.005(2) C5 0.029(3) 0.034(3) 0.033(3) -0.002(2) 0.009(2) 0.007(2) C6 0.029(3) 0.032(3) 0.025(3) -0.003(2) 0.014(2) -0.002(2) C7 0.035(3) 0.029(3) 0.035(3) 0.000(2) 0.009(3) -0.003(2) C8 0.031(3) 0.030(3) 0.037(3) 0.005(2) 0.008(3) 0.004(2) C9 0.016(3) 0.056(4) 0.031(3) 0.000(3) 0.006(2) 0.001(3) C10 0.036(3) 0.036(3) 0.030(3) -0.003(2) 0.008(3) -0.009(2) C11 0.026(4) 0.102(8) 0.212(13) -0.077(8) -0.017(6) 0.009(5) C12 0.051(6) 0.147(11) 0.190(13) -0.068(10) 0.013(7) -0.044(7) C13 0.054(6) 0.130(11) 0.230(15) -0.057(10) -0.025(7) 0.046(6) C15 0.052(4) 0.038(3) 0.039(4) -0.007(3) 0.012(3) 0.006(3) O15 0.112(4) 0.044(3) 0.044(3) 0.007(2) 0.009(3) 0.021(3) C16 0.049(5) 0.054(4) 0.072(5) 0.015(4) 0.029(4) 0.012(4) O16 0.046(4) 0.127(6) 0.165(7) 0.058(5) 0.049(4) 0.011(4) C17 0.066(5) 0.046(4) 0.040(4) 0.000(3) 0.018(3) 0.017(3) O17 0.115(5) 0.070(4) 0.047(3) -0.022(3) -0.002(3) 0.018(3) C25 0.058(4) 0.038(4) 0.040(4) 0.010(3) 0.013(3) 0.006(3) O25 0.098(4) 0.050(3) 0.081(4) 0.009(3) 0.046(3) 0.026(3) C26 0.064(5) 0.039(4) 0.041(4) 0.003(3) 0.020(3) -0.003(3) O26 0.075(4) 0.075(4) 0.107(5) 0.009(3) 0.048(4) -0.027(3) C27 0.056(4) 0.045(4) 0.037(4) 0.003(3) 0.011(3) 0.009(3) O27 0.085(4) 0.079(4) 0.042(3) -0.014(3) -0.011(3) 0.006(3) C35 0.043(4) 0.046(4) 0.045(4) 0.002(3) 0.020(3) -0.013(3) O35 0.093(4) 0.051(3) 0.069(4) -0.017(3) 0.034(3) -0.025(3) C36 0.046(4) 0.069(5) 0.060(5) -0.004(4) 0.020(4) -0.005(4) O36 0.043(3) 0.154(7) 0.118(6) -0.036(5) 0.041(4) -0.002(4) C37 0.075(5) 0.041(4) 0.048(4) 0.000(3) 0.026(4) -0.012(3) O37 0.122(5) 0.073(4) 0.052(3) 0.029(3) 0.007(3) 0.003(4) C45 0.049(4) 0.038(4) 0.049(4) -0.014(3) 0.012(3) -0.009(3) O45 0.082(4) 0.038(3) 0.103(4) -0.011(3) 0.046(3) -0.015(3) C46 0.053(4) 0.049(4) 0.037(4) -0.005(3) 0.020(3) 0.000(3) O46 0.067(4) 0.090(4) 0.079(4) -0.011(3) 0.034(3) 0.027(3) C47 0.066(5) 0.046(4) 0.045(4) 0.003(3) 0.012(4) -0.010(3) O47 0.090(4) 0.086(4) 0.048(3) 0.017(3) -0.024(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C15 1.781(7) . ? Co1 C17 1.805(7) . ? Co1 C16 1.812(8) . ? Co1 C1 1.967(6) . ? Co1 C2 1.982(6) . ? Co1 Co2 2.4700(11) . ? Co2 C25 1.785(7) . ? Co2 C26 1.801(7) . ? Co2 C27 1.818(7) . ? Co2 C2 1.956(6) . ? Co2 C1 1.985(5) . ? Co3 C35 1.775(7) . ? Co3 C36 1.817(8) . ? Co3 C37 1.823(8) . ? Co3 C6 1.962(5) . ? Co3 C7 1.967(6) . ? Co3 Co4 2.4685(11) . ? Co4 C46 1.785(7) . ? Co4 C45 1.802(7) . ? Co4 C47 1.823(7) . ? Co4 C7 1.962(6) . ? Co4 C6 1.987(5) . ? C1 C2 1.321(7) . ? C1 C10 1.494(7) . ? C2 C3 1.478(8) . ? C3 N4 1.469(7) . ? N4 C11 1.412(9) . ? N4 C5 1.446(7) . ? C5 C6 1.516(7) . ? C6 C7 1.312(7) . ? C7 C8 1.499(8) . ? C8 C9 1.541(8) . ? C9 C10 1.530(8) . ? C11 C12 1.390(12) . ? C11 C13 1.476(13) . ? C15 O15 1.146(7) . ? C16 O16 1.146(9) . ? C17 O17 1.144(8) . ? C25 O25 1.139(8) . ? C26 O26 1.140(8) . ? C27 O27 1.126(7) . ? C35 O35 1.143(8) . ? C36 O36 1.131(9) . ? C37 O37 1.120(8) . ? C45 O45 1.120(8) . ? C46 O46 1.161(8) . ? C47 O47 1.128(8) . ? Co1B Co2B 2.468(18) . ? Co3B Co4B 2.488(18) . ? 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 C15 Co1 C17 97.1(3) . . ? C15 Co1 C16 98.3(3) . . ? C17 Co1 C16 107.9(3) . . ? C15 Co1 C1 104.6(3) . . ? C17 Co1 C1 141.1(3) . . ? C16 Co1 C1 100.5(3) . . ? C15 Co1 C2 102.5(3) . . ? C17 Co1 C2 105.1(3) . . ? C16 Co1 C2 138.1(3) . . ? C1 Co1 C2 39.1(2) . . ? C15 Co1 Co2 152.4(2) . . ? C17 Co1 Co2 96.9(2) . . ? C16 Co1 Co2 99.8(2) . . ? C1 Co1 Co2 51.63(16) . . ? C2 Co1 Co2 50.70(16) . . ? C25 Co2 C26 98.0(3) . . ? C25 Co2 C27 98.4(3) . . ? C26 Co2 C27 106.8(3) . . ? C25 Co2 C2 101.7(3) . . ? C26 Co2 C2 140.7(3) . . ? C27 Co2 C2 103.6(3) . . ? C25 Co2 C1 102.4(3) . . ? C26 Co2 C1 103.4(3) . . ? C27 Co2 C1 140.2(3) . . ? C2 Co2 C1 39.2(2) . . ? C25 Co2 Co1 151.2(2) . . ? C26 Co2 Co1 99.0(2) . . ? C27 Co2 Co1 98.6(2) . . ? C2 Co2 Co1 51.63(17) . . ? C1 Co2 Co1 50.99(17) . . ? C35 Co3 C36 100.1(3) . . ? C35 Co3 C37 97.3(3) . . ? C36 Co3 C37 106.6(3) . . ? C35 Co3 C6 102.9(3) . . ? C36 Co3 C6 101.8(3) . . ? C37 Co3 C6 141.4(3) . . ? C35 Co3 C7 100.6(3) . . ? C36 Co3 C7 139.1(3) . . ? C37 Co3 C7 105.2(3) . . ? C6 Co3 C7 39.0(2) . . ? C35 Co3 Co4 150.7(2) . . ? C36 Co3 Co4 99.6(3) . . ? C37 Co3 Co4 97.5(2) . . ? C6 Co3 Co4 51.76(15) . . ? C7 Co3 Co4 50.98(17) . . ? C46 Co4 C45 96.8(3) . . ? C46 Co4 C47 106.3(3) . . ? C45 Co4 C47 99.2(3) . . ? C46 Co4 C7 141.2(3) . . ? C45 Co4 C7 104.9(3) . . ? C47 Co4 C7 101.6(3) . . ? C46 Co4 C6 105.6(3) . . ? C45 Co4 C6 102.1(3) . . ? C47 Co4 C6 138.8(3) . . ? C7 Co4 C6 38.8(2) . . ? C46 Co4 Co3 97.3(2) . . ? C45 Co4 Co3 152.2(2) . . ? C47 Co4 Co3 99.7(2) . . ? C7 Co4 Co3 51.16(17) . . ? C6 Co4 Co3 50.86(16) . . ? C2 C1 C10 144.2(6) . . ? C2 C1 Co1 71.1(4) . . ? C10 C1 Co1 134.8(4) . . ? C2 C1 Co2 69.3(3) . . ? C10 C1 Co2 131.8(4) . . ? Co1 C1 Co2 77.4(2) . . ? C1 C2 C3 144.4(5) . . ? C1 C2 Co2 71.6(4) . . ? C3 C2 Co2 134.4(4) . . ? C1 C2 Co1 69.8(4) . . ? C3 C2 Co1 131.1(4) . . ? Co2 C2 Co1 77.7(2) . . ? N4 C3 C2 113.7(5) . . ? C11 N4 C5 117.3(6) . . ? C11 N4 C3 120.0(6) . . ? C5 N4 C3 115.4(4) . . ? N4 C5 C6 116.3(5) . . ? C7 C6 C5 143.9(5) . . ? C7 C6 Co3 70.7(4) . . ? C5 C6 Co3 137.4(4) . . ? C7 C6 Co4 69.6(3) . . ? C5 C6 Co4 129.2(4) . . ? Co3 C6 Co4 77.4(2) . . ? C6 C7 C8 142.9(6) . . ? C6 C7 Co4 71.6(3) . . ? C8 C7 Co4 135.1(4) . . ? C6 C7 Co3 70.3(3) . . ? C8 C7 Co3 131.5(4) . . ? Co4 C7 Co3 77.9(2) . . ? C7 C8 C9 114.5(5) . . ? C10 C9 C8 116.9(4) . . ? C1 C10 C9 115.0(5) . . ? C12 C11 N4 122.3(9) . . ? C12 C11 C13 114.2(8) . . ? N4 C11 C13 115.0(9) . . ? O15 C15 Co1 178.2(6) . . ? O16 C16 Co1 179.0(7) . . ? O17 C17 Co1 177.6(7) . . ? O25 C25 Co2 178.4(7) . . ? O26 C26 Co2 177.1(6) . . ? O27 C27 Co2 176.5(7) . . ? O35 C35 Co3 177.7(7) . . ? O36 C36 Co3 178.5(8) . . ? O37 C37 Co3 178.1(7) . . ? O45 C45 Co4 178.2(7) . . ? O46 C46 Co4 176.7(6) . . ? O47 C47 Co4 178.7(8) . . ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.883 _refine_diff_density_max 0.923 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.133 #===END data_br24_23 _database_code_CSD 168780 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H15 Co4 N O12 S' _chemical_formula_weight 765.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.81340(10) _cell_length_b 7.68310(10) _cell_length_c 23.14790(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.5060(10) _cell_angle_gamma 90.00 _cell_volume 2867.00(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 2.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.38 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 28495 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6548 _reflns_number_gt 5455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0349P)^2^+1.0769P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6548 _refine_ls_number_parameters 383 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.305 _refine_ls_shift/su_mean 0.007 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 0.750333(17) 0.37484(4) 0.109655(12) 0.02965(8) Uani 1 1 d . . . Co2 Co 0.818682(17) 0.09915(4) 0.096208(12) 0.02834(8) Uani 1 1 d . . . Co3 Co 0.633890(17) 0.41767(3) -0.177563(12) 0.02589(7) Uani 1 1 d . A . Co4 Co 0.560528(16) 0.14461(3) -0.169188(12) 0.02495(7) Uani 1 1 d . A . C1 C 0.71087(12) 0.1956(2) 0.04794(8) 0.0242(4) Uani 1 1 d . A . C2 C 0.77377(12) 0.2816(2) 0.03647(8) 0.0242(4) Uani 1 1 d . . . C3 C 0.80288(13) 0.3659(3) -0.01231(9) 0.0287(4) Uani 1 1 d D A . H3A H 0.7605 0.4505 -0.0340 0.034 Uiso 1 1 calc R . . H3B H 0.8546 0.4311 0.0063 0.034 Uiso 1 1 calc R . . N4 N 0.81843(11) 0.2413(3) -0.05569(8) 0.0361(4) Uani 1 1 d D . . C44 C 0.86923(19) 0.2937(4) -0.09503(16) 0.0431(9) Uani 0.781(4) 1 d PD A 1 H44 H 0.8309 0.3477 -0.1318 0.052 Uiso 0.781(4) 1 calc PR A 1 C45 C 0.9342(2) 0.4240(6) -0.0684(2) 0.0723(14) Uani 0.781(4) 1 d PD A 1 H45A H 0.9090 0.5240 -0.0540 0.087 Uiso 0.781(4) 1 calc PR A 1 H45B H 0.9603 0.4627 -0.0990 0.087 Uiso 0.781(4) 1 calc PR A 1 H45C H 0.9762 0.3715 -0.0346 0.087 Uiso 0.781(4) 1 calc PR A 1 C46 C 0.9088(3) 0.1380(7) -0.1157(2) 0.0755(15) Uani 0.781(4) 1 d PD A 1 H46A H 0.8660 0.0519 -0.1337 0.091 Uiso 0.781(4) 1 calc PR A 1 H46B H 0.9496 0.0860 -0.0810 0.091 Uiso 0.781(4) 1 calc PR A 1 H46C H 0.9365 0.1751 -0.1456 0.091 Uiso 0.781(4) 1 calc PR A 1 C5 C 0.74761(12) 0.1358(3) -0.08645(9) 0.0268(4) Uani 1 1 d D A . H5A H 0.7359 0.0544 -0.0567 0.032 Uiso 1 1 calc R . . H5B H 0.7634 0.0648 -0.1171 0.032 Uiso 1 1 calc R . . C6 C 0.66828(12) 0.2309(2) -0.11721(8) 0.0229(4) Uani 1 1 d . . . C7 C 0.60534(12) 0.3199(2) -0.10705(8) 0.0234(4) Uani 1 1 d . A . C8 C 0.57595(13) 0.4051(3) -0.05907(9) 0.0271(4) Uani 1 1 d . . . H8A H 0.5291 0.4831 -0.0786 0.033 Uiso 1 1 calc R A . H8B H 0.6214 0.4789 -0.0345 0.033 Uiso 1 1 calc R . . S9 S 0.54233(3) 0.25894(7) -0.00867(2) 0.02983(12) Uani 1 1 d . A . C10 C 0.62916(12) 0.1120(3) 0.02020(9) 0.0263(4) Uani 1 1 d . . . H10A H 0.6161 0.0354 0.0507 0.032 Uiso 1 1 calc R A . H10B H 0.6343 0.0370 -0.0133 0.032 Uiso 1 1 calc R . . C11 C 0.69092(18) 0.3006(4) 0.16032(12) 0.0536(7) Uani 1 1 d . . . O11 O 0.65041(17) 0.2460(4) 0.18705(11) 0.0908(8) Uani 1 1 d . . . C12 C 0.84250(16) 0.4863(3) 0.15355(12) 0.0469(6) Uani 1 1 d . . . O12 O 0.90037(13) 0.5576(3) 0.17971(12) 0.0825(8) Uani 1 1 d . . . C13 C 0.69347(14) 0.5674(3) 0.08044(11) 0.0437(6) Uani 1 1 d . . . O13 O 0.66015(12) 0.6930(3) 0.06302(11) 0.0734(7) Uani 1 1 d . . . C21 C 0.79225(15) -0.0241(3) 0.15500(11) 0.0461(6) Uani 1 1 d . . . O21 O 0.77283(15) -0.1000(3) 0.19050(10) 0.0791(7) Uani 1 1 d . . . C22 C 0.92629(14) 0.1665(3) 0.12674(11) 0.0389(5) Uani 1 1 d . . . O22 O 0.99269(11) 0.2127(3) 0.14494(10) 0.0644(6) Uani 1 1 d . . . C23 C 0.83331(16) -0.0793(3) 0.05019(12) 0.0454(6) Uani 1 1 d . . . O23 O 0.84256(15) -0.1936(3) 0.02219(10) 0.0770(7) Uani 1 1 d . . . C31 C 0.68707(15) 0.3531(3) -0.23279(11) 0.0414(5) Uani 1 1 d . . . O31 O 0.72028(14) 0.3096(3) -0.26592(10) 0.0788(7) Uani 1 1 d . A . C32 C 0.54342(15) 0.5388(3) -0.22053(10) 0.0391(5) Uani 1 1 d . . . O32 O 0.48651(13) 0.6127(3) -0.24751(9) 0.0634(6) Uani 1 1 d . A . C33 C 0.69624(16) 0.5985(3) -0.14247(10) 0.0386(5) Uani 1 1 d . . . O33 O 0.73410(14) 0.7140(2) -0.11929(9) 0.0626(5) Uani 1 1 d . A . C41 C 0.58415(14) 0.0324(3) -0.23136(10) 0.0368(5) Uani 1 1 d . . . O41 O 0.60107(13) -0.0373(3) -0.26925(9) 0.0634(5) Uani 1 1 d . A . C42 C 0.45305(15) 0.2192(3) -0.19591(11) 0.0420(5) Uani 1 1 d . . . O42 O 0.38750(12) 0.2694(3) -0.21050(11) 0.0754(7) Uani 1 1 d . A . C43 C 0.54635(14) -0.0455(3) -0.12818(10) 0.0356(5) Uani 1 1 d . . . O43 O 0.53871(13) -0.1681(2) -0.10365(8) 0.0579(5) Uani 1 1 d . A . C44B C 0.9025(5) 0.2356(13) -0.0553(5) 0.033(2) Uiso 0.219(4) 1 d PD A 2 H44B H 0.9338 0.3334 -0.0305 0.039 Uiso 0.219(4) 1 calc PR A 2 C45B C 0.9398(14) 0.070(3) -0.0319(11) 0.144(10) Uiso 0.219(4) 1 d PD A 2 H45D H 0.9292 0.0458 0.0069 0.173 Uiso 0.219(4) 1 calc PR A 2 H45E H 0.9997 0.0746 -0.0263 0.173 Uiso 0.219(4) 1 calc PR A 2 H45F H 0.9155 -0.0232 -0.0605 0.173 Uiso 0.219(4) 1 calc PR A 2 C46B C 0.911(3) 0.245(5) -0.1193(12) 0.26(3) Uiso 0.219(4) 1 d PD A 2 H46D H 0.8888 0.3555 -0.1378 0.309 Uiso 0.219(4) 1 calc PR A 2 H46E H 0.8802 0.1483 -0.1433 0.309 Uiso 0.219(4) 1 calc PR A 2 H46F H 0.9698 0.2355 -0.1178 0.309 Uiso 0.219(4) 1 calc PR A 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 0.02988(15) 0.03136(15) 0.02445(15) -0.00760(11) 0.00242(11) 0.00208(11) Co2 0.02667(14) 0.02686(14) 0.02679(15) 0.00099(11) -0.00001(11) 0.00249(11) Co3 0.03321(15) 0.02473(14) 0.02087(13) 0.00233(10) 0.00951(11) -0.00057(11) Co4 0.02670(14) 0.02607(14) 0.02149(13) -0.00221(10) 0.00589(11) -0.00206(10) C1 0.0276(10) 0.0232(9) 0.0198(9) -0.0014(7) 0.0034(8) 0.0033(7) C2 0.0263(10) 0.0217(9) 0.0228(9) -0.0023(7) 0.0040(8) 0.0037(7) C3 0.0268(10) 0.0302(10) 0.0291(10) -0.0024(8) 0.0081(8) -0.0063(8) N4 0.0260(9) 0.0530(12) 0.0320(10) -0.0119(9) 0.0125(8) -0.0093(8) C44 0.0365(17) 0.0516(19) 0.049(2) -0.0009(15) 0.0256(15) -0.0012(14) C45 0.063(2) 0.092(3) 0.079(3) -0.018(2) 0.047(2) -0.041(2) C46 0.065(3) 0.082(3) 0.104(4) -0.027(3) 0.063(3) -0.002(2) C5 0.0282(10) 0.0271(10) 0.0259(10) -0.0032(8) 0.0088(8) 0.0030(8) C6 0.0276(10) 0.0215(9) 0.0197(9) -0.0005(7) 0.0070(8) -0.0026(7) C7 0.0272(10) 0.0218(9) 0.0209(9) 0.0005(7) 0.0065(8) -0.0019(7) C8 0.0320(10) 0.0268(10) 0.0237(10) 0.0007(8) 0.0098(8) 0.0048(8) S9 0.0229(2) 0.0437(3) 0.0246(2) 0.0053(2) 0.0095(2) 0.0046(2) C10 0.0247(10) 0.0282(10) 0.0248(10) 0.0016(8) 0.0050(8) -0.0011(8) C11 0.0623(17) 0.0672(18) 0.0352(14) -0.0180(13) 0.0204(13) -0.0073(14) O11 0.1046(18) 0.122(2) 0.0653(15) -0.0207(14) 0.0560(15) -0.0293(17) C12 0.0448(14) 0.0351(13) 0.0485(14) -0.0137(11) -0.0066(11) 0.0075(11) O12 0.0512(12) 0.0582(13) 0.1068(18) -0.0339(13) -0.0281(12) 0.0017(10) C13 0.0332(12) 0.0432(14) 0.0451(14) -0.0197(11) -0.0045(10) 0.0060(10) O13 0.0554(12) 0.0438(11) 0.0944(16) -0.0196(11) -0.0220(11) 0.0205(10) C21 0.0417(13) 0.0503(15) 0.0404(13) 0.0118(12) 0.0020(11) 0.0005(11) O21 0.0791(15) 0.0913(17) 0.0656(14) 0.0370(13) 0.0186(12) -0.0120(13) C22 0.0337(12) 0.0341(12) 0.0442(13) -0.0022(10) 0.0035(10) 0.0067(9) O22 0.0319(10) 0.0605(12) 0.0909(16) -0.0149(11) 0.0013(10) -0.0027(9) C23 0.0432(13) 0.0345(13) 0.0480(14) -0.0023(11) -0.0041(11) 0.0105(10) O23 0.0935(16) 0.0506(12) 0.0718(14) -0.0234(11) -0.0010(12) 0.0270(12) C31 0.0454(13) 0.0481(14) 0.0356(12) -0.0028(11) 0.0192(11) -0.0066(11) O31 0.0839(16) 0.1054(18) 0.0676(14) -0.0245(13) 0.0545(13) -0.0127(14) C32 0.0492(14) 0.0341(12) 0.0345(12) 0.0054(10) 0.0126(11) 0.0007(10) O32 0.0580(12) 0.0582(12) 0.0645(13) 0.0202(10) 0.0021(10) 0.0172(10) C33 0.0549(15) 0.0327(12) 0.0296(11) 0.0070(9) 0.0141(11) -0.0051(10) O33 0.0910(15) 0.0411(10) 0.0496(11) -0.0008(9) 0.0103(10) -0.0285(10) C41 0.0365(12) 0.0390(12) 0.0324(12) -0.0068(10) 0.0057(9) -0.0027(10) O41 0.0706(13) 0.0739(14) 0.0511(11) -0.0280(10) 0.0260(10) -0.0007(11) C42 0.0341(13) 0.0429(13) 0.0463(14) 0.0009(11) 0.0070(11) -0.0029(10) O42 0.0344(11) 0.0798(15) 0.1054(18) 0.0138(13) 0.0093(11) 0.0108(10) C43 0.0417(12) 0.0340(12) 0.0299(11) -0.0059(9) 0.0083(9) -0.0091(10) O43 0.0894(15) 0.0393(10) 0.0478(11) 0.0040(8) 0.0240(10) -0.0195(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 C13 1.787(2) . ? Co1 C12 1.809(2) . ? Co1 C11 1.834(3) . ? Co1 C1 1.9595(19) . ? Co1 C2 1.9792(19) . ? Co1 Co2 2.4713(4) . ? Co2 C23 1.796(3) . ? Co2 C21 1.814(3) . ? Co2 C22 1.821(2) . ? Co2 C2 1.9633(19) . ? Co2 C1 1.9829(19) . ? Co3 C33 1.790(2) . ? Co3 C32 1.819(2) . ? Co3 C31 1.825(2) . ? Co3 C6 1.9716(18) . ? Co3 C7 1.9759(18) . ? Co3 Co4 2.4691(4) . ? Co4 C43 1.794(2) . ? Co4 C41 1.816(2) . ? Co4 C42 1.828(2) . ? Co4 C7 1.9580(19) . ? Co4 C6 1.9825(19) . ? C1 C2 1.336(3) . ? C1 C10 1.487(3) . ? C2 C3 1.499(3) . ? C3 N4 1.463(3) . ? N4 C44B 1.411(9) . ? N4 C5 1.449(3) . ? N4 C44 1.471(3) . ? C44 C45 1.480(5) . ? C44 C46 1.511(5) . ? C5 C6 1.510(3) . ? C6 C7 1.336(3) . ? C7 C8 1.489(3) . ? C8 S9 1.821(2) . ? S9 C10 1.816(2) . ? C11 O11 1.124(3) . ? C12 O12 1.131(3) . ? C13 O13 1.131(3) . ? C21 O21 1.129(3) . ? C22 O22 1.132(3) . ? C23 O23 1.128(3) . ? C31 O31 1.120(3) . ? C32 O32 1.135(3) . ? C33 O33 1.135(3) . ? C41 O41 1.131(3) . ? C42 O42 1.125(3) . ? C43 O43 1.126(3) . ? C44B C45B 1.456(16) . ? C44B C46B 1.530(18) . ? 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 C13 Co1 C12 95.82(10) . . ? C13 Co1 C11 99.76(13) . . ? C12 Co1 C11 108.86(12) . . ? C13 Co1 C1 105.80(9) . . ? C12 Co1 C1 143.21(10) . . ? C11 Co1 C1 96.57(10) . . ? C13 Co1 C2 101.01(10) . . ? C12 Co1 C2 107.76(10) . . ? C11 Co1 C2 135.38(10) . . ? C1 Co1 C2 39.66(8) . . ? C13 Co1 Co2 151.64(8) . . ? C12 Co1 Co2 96.99(7) . . ? C11 Co1 Co2 99.86(10) . . ? C1 Co1 Co2 51.61(5) . . ? C2 Co1 Co2 50.90(5) . . ? C23 Co2 C21 98.66(12) . . ? C23 Co2 C22 99.15(11) . . ? C21 Co2 C22 106.59(11) . . ? C23 Co2 C2 102.57(10) . . ? C21 Co2 C2 140.72(10) . . ? C22 Co2 C2 102.19(9) . . ? C23 Co2 C1 102.03(9) . . ? C21 Co2 C1 103.78(10) . . ? C22 Co2 C1 139.55(9) . . ? C2 Co2 C1 39.58(8) . . ? C23 Co2 Co1 151.19(8) . . ? C21 Co2 Co1 97.53(9) . . ? C22 Co2 Co1 98.84(7) . . ? C2 Co2 Co1 51.47(5) . . ? C1 Co2 Co1 50.76(5) . . ? C33 Co3 C32 98.17(11) . . ? C33 Co3 C31 100.87(11) . . ? C32 Co3 C31 104.84(11) . . ? C33 Co3 C6 103.13(9) . . ? C32 Co3 C6 142.29(9) . . ? C31 Co3 C6 101.25(10) . . ? C33 Co3 C7 99.71(9) . . ? C32 Co3 C7 106.53(9) . . ? C31 Co3 C7 139.26(10) . . ? C6 Co3 C7 39.55(8) . . ? C33 Co3 Co4 149.87(7) . . ? C32 Co3 Co4 96.82(7) . . ? C31 Co3 Co4 100.31(8) . . ? C6 Co3 Co4 51.56(5) . . ? C7 Co3 Co4 50.80(5) . . ? C43 Co4 C41 97.16(10) . . ? C43 Co4 C42 99.63(11) . . ? C41 Co4 C42 107.37(11) . . ? C43 Co4 C7 104.62(9) . . ? C41 Co4 C7 141.59(9) . . ? C42 Co4 C7 99.78(10) . . ? C43 Co4 C6 100.77(9) . . ? C41 Co4 C6 105.77(9) . . ? C42 Co4 C6 138.20(10) . . ? C7 Co4 C6 39.62(8) . . ? C43 Co4 Co3 151.35(7) . . ? C41 Co4 Co3 96.58(7) . . ? C42 Co4 Co3 100.06(8) . . ? C7 Co4 Co3 51.45(5) . . ? C6 Co4 Co3 51.16(5) . . ? C2 C1 C10 144.50(18) . . ? C2 C1 Co1 70.97(11) . . ? C10 C1 Co1 134.29(14) . . ? C2 C1 Co2 69.42(11) . . ? C10 C1 Co2 131.81(14) . . ? Co1 C1 Co2 77.64(7) . . ? C1 C2 C3 144.04(18) . . ? C1 C2 Co2 71.00(11) . . ? C3 C2 Co2 134.12(14) . . ? C1 C2 Co1 69.37(11) . . ? C3 C2 Co1 132.49(14) . . ? Co2 C2 Co1 77.63(7) . . ? N4 C3 C2 113.26(17) . . ? C44B N4 C5 131.9(4) . . ? C44B N4 C3 112.9(4) . . ? C5 N4 C3 114.88(16) . . ? C44B N4 C44 41.9(4) . . ? C5 N4 C44 112.92(19) . . ? C3 N4 C44 119.6(2) . . ? N4 C44 C45 114.6(3) . . ? N4 C44 C46 111.4(3) . . ? C45 C44 C46 109.1(3) . . ? N4 C5 C6 116.98(16) . . ? C7 C6 C5 143.37(18) . . ? C7 C6 Co3 70.40(11) . . ? C5 C6 Co3 136.73(14) . . ? C7 C6 Co4 69.20(11) . . ? C5 C6 Co4 131.08(13) . . ? Co3 C6 Co4 77.28(7) . . ? C6 C7 C8 143.47(18) . . ? C6 C7 Co4 71.18(11) . . ? C8 C7 Co4 135.26(14) . . ? C6 C7 Co3 70.05(11) . . ? C8 C7 Co3 131.19(14) . . ? Co4 C7 Co3 77.75(7) . . ? C7 C8 S9 115.82(14) . . ? C10 S9 C8 104.81(9) . . ? C1 C10 S9 115.98(14) . . ? O11 C11 Co1 173.6(3) . . ? O12 C12 Co1 178.3(3) . . ? O13 C13 Co1 177.3(2) . . ? O21 C21 Co2 177.5(2) . . ? O22 C22 Co2 178.1(2) . . ? O23 C23 Co2 178.7(3) . . ? O31 C31 Co3 178.2(3) . . ? O32 C32 Co3 179.3(3) . . ? O33 C33 Co3 178.0(2) . . ? O41 C41 Co4 178.1(2) . . ? O42 C42 Co4 177.3(3) . . ? O43 C43 Co4 177.6(2) . . ? N4 C44B C45B 110.8(12) . . ? N4 C44B C46B 111.2(17) . . ? C45B C44B C46B 104.5(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.418 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.065 #===END data_br19_24 _database_code_CSD 168781 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Co4 N2 O12' _chemical_formula_weight 790.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6251(4) _cell_length_b 7.7115(2) _cell_length_c 16.0675(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.8410(10) _cell_angle_gamma 90.00 _cell_volume 1558.73(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max .265 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 15325 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3561 _reflns_number_gt 2720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3561 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.78192(2) 0.12954(4) -0.001534(18) 0.02188(9) Uani 1 1 d . . . Co2 Co 0.73870(2) -0.15140(4) -0.070820(18) 0.02293(9) Uani 1 1 d . . . C1 C 0.67627(16) -0.0460(3) 0.02492(13) 0.0200(5) Uani 1 1 d . . . C2 C 0.64246(16) 0.0372(3) -0.04502(13) 0.0199(4) Uani 1 1 d . . . C3 C 0.54914(16) 0.1362(3) -0.08429(14) 0.0228(5) Uani 1 1 d . . . H3A H 0.5209 0.2111 -0.0412 0.027 Uiso 1 1 calc R . . H3B H 0.5740 0.2130 -0.1280 0.027 Uiso 1 1 calc R . . N4 N 0.46193(13) 0.0274(2) -0.12200(10) 0.0197(4) Uani 1 1 d . . . C5 C 0.35877(16) 0.1051(3) -0.10736(13) 0.0227(5) Uani 1 1 d . . . H5A H 0.3050 0.0710 -0.1528 0.027 Uiso 1 1 calc R . . H5B H 0.3649 0.2331 -0.1076 0.027 Uiso 1 1 calc R . . C6 C 0.47410(18) -0.0107(3) -0.21133(13) 0.0273(5) Uani 1 1 d . . . H6 H 0.5496 -0.0471 -0.2151 0.033 Uiso 1 1 calc R . . C7 C 0.4538(2) 0.1437(3) -0.27044(16) 0.0420(7) Uani 1 1 d . . . H7A H 0.3784 0.1754 -0.2732 0.063 Uiso 1 1 calc R . . H7B H 0.4729 0.1120 -0.3263 0.063 Uiso 1 1 calc R . . H7C H 0.4971 0.2425 -0.2496 0.063 Uiso 1 1 calc R . . C8 C 0.4041(2) -0.1646(3) -0.24100(16) 0.0415(7) Uani 1 1 d . . . H8A H 0.4194 -0.2635 -0.2036 0.062 Uiso 1 1 calc R . . H8B H 0.4190 -0.1964 -0.2979 0.062 Uiso 1 1 calc R . . H8C H 0.3291 -0.1323 -0.2405 0.062 Uiso 1 1 calc R . . C11 C 0.73487(19) 0.3127(3) 0.05304(16) 0.0304(5) Uani 1 1 d . . . O11 O 0.70369(16) 0.4286(2) 0.08687(13) 0.0513(5) Uani 1 1 d . . . C12 C 0.83604(18) 0.2446(3) -0.08736(16) 0.0331(6) Uani 1 1 d . . . O12 O 0.86958(16) 0.3186(3) -0.14027(13) 0.0556(6) Uani 1 1 d . . . C13 C 0.89563(19) 0.0605(3) 0.06780(15) 0.0285(5) Uani 1 1 d . . . O13 O 0.96389(14) 0.0118(2) 0.11169(11) 0.0449(5) Uani 1 1 d . . . C21 C 0.6410(2) -0.3180(3) -0.09383(16) 0.0330(6) Uani 1 1 d . . . O21 O 0.57761(16) -0.4213(2) -0.10464(13) 0.0538(5) Uani 1 1 d . . . C22 C 0.77947(19) -0.0976(3) -0.17385(16) 0.0363(6) Uani 1 1 d . . . O22 O 0.80550(17) -0.0584(3) -0.23675(12) 0.0643(6) Uani 1 1 d . . . C23 C 0.8471(2) -0.2813(3) -0.02207(16) 0.0324(6) Uani 1 1 d . . . O23 O 0.91415(15) -0.3598(2) 0.01046(14) 0.0535(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 0.01635(16) 0.02356(16) 0.02588(18) -0.00016(12) 0.00263(12) -0.00252(12) Co2 0.01810(17) 0.02511(16) 0.02601(18) -0.00392(13) 0.00442(12) 0.00224(13) C1 0.0158(11) 0.0186(10) 0.0259(12) -0.0037(9) 0.0042(9) 0.0001(8) C2 0.0168(11) 0.0207(10) 0.0227(11) -0.0039(9) 0.0044(9) -0.0016(9) C3 0.0190(11) 0.0224(11) 0.0268(12) 0.0002(9) 0.0006(9) 0.0010(9) N4 0.0143(9) 0.0250(9) 0.0199(9) -0.0004(7) 0.0024(7) 0.0008(7) C5 0.0173(11) 0.0270(11) 0.0242(12) 0.0046(9) 0.0043(9) 0.0023(9) C6 0.0240(12) 0.0376(13) 0.0208(11) -0.0008(10) 0.0040(9) 0.0038(10) C7 0.0410(16) 0.0595(18) 0.0256(13) 0.0109(12) 0.0044(11) -0.0011(14) C8 0.0436(16) 0.0487(16) 0.0315(14) -0.0121(12) -0.0013(12) -0.0036(13) C11 0.0258(13) 0.0276(12) 0.0376(14) 0.0041(11) 0.0013(11) -0.0050(10) O11 0.0614(13) 0.0307(10) 0.0632(13) -0.0109(9) 0.0147(11) 0.0066(9) C12 0.0220(13) 0.0390(14) 0.0382(15) 0.0031(12) 0.0014(11) -0.0046(11) O12 0.0507(13) 0.0678(14) 0.0499(13) 0.0242(11) 0.0134(10) -0.0087(11) C13 0.0248(13) 0.0279(12) 0.0331(14) -0.0057(10) 0.0042(11) -0.0044(10) O13 0.0341(11) 0.0470(11) 0.0508(11) -0.0036(10) -0.0129(9) 0.0081(9) C21 0.0319(14) 0.0274(12) 0.0398(15) -0.0059(11) 0.0035(11) 0.0050(11) O21 0.0459(12) 0.0326(10) 0.0814(16) -0.0088(10) -0.0029(11) -0.0110(9) C22 0.0253(13) 0.0518(16) 0.0321(14) -0.0072(12) 0.0039(11) 0.0003(12) O22 0.0559(14) 0.1072(18) 0.0319(11) 0.0000(12) 0.0154(10) -0.0106(13) C23 0.0265(13) 0.0282(13) 0.0429(15) -0.0095(11) 0.0044(11) 0.0037(11) O23 0.0381(11) 0.0436(11) 0.0763(15) -0.0040(10) -0.0097(11) 0.0148(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 Co1 C11 1.790(3) . ? Co1 C12 1.821(3) . ? Co1 C13 1.821(3) . ? Co1 C2 1.972(2) . ? Co1 C1 1.972(2) . ? Co1 Co2 2.4755(4) . ? Co2 C21 1.798(3) . ? Co2 C23 1.819(3) . ? Co2 C22 1.822(3) . ? Co2 C2 1.962(2) . ? Co2 C1 1.963(2) . ? C1 C2 1.333(3) . ? C1 C5 1.502(3) 3_655 ? C2 C3 1.498(3) . ? C3 N4 1.474(3) . ? N4 C5 1.471(3) . ? N4 C6 1.486(3) . ? C5 C1 1.502(3) 3_655 ? C6 C7 1.531(3) . ? C6 C8 1.531(3) . ? C11 O11 1.134(3) . ? C12 O12 1.135(3) . ? C13 O13 1.131(3) . ? C21 O21 1.132(3) . ? C22 O22 1.130(3) . ? C23 O23 1.132(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 C11 Co1 C12 98.50(11) . . ? C11 Co1 C13 102.00(11) . . ? C12 Co1 C13 106.20(10) . . ? C11 Co1 C2 97.76(10) . . ? C12 Co1 C2 106.77(10) . . ? C13 Co1 C2 138.22(9) . . ? C11 Co1 C1 100.23(9) . . ? C12 Co1 C1 143.30(10) . . ? C13 Co1 C1 100.38(9) . . ? C2 Co1 C1 39.51(8) . . ? C11 Co1 Co2 147.26(8) . . ? C12 Co1 Co2 99.70(8) . . ? C13 Co1 Co2 98.74(7) . . ? C2 Co1 Co2 50.83(6) . . ? C1 Co1 Co2 50.85(6) . . ? C21 Co2 C23 99.95(11) . . ? C21 Co2 C22 102.55(11) . . ? C23 Co2 C22 104.88(11) . . ? C21 Co2 C2 98.45(9) . . ? C23 Co2 C2 140.73(10) . . ? C22 Co2 C2 104.51(10) . . ? C21 Co2 C1 98.23(10) . . ? C23 Co2 C1 103.16(10) . . ? C22 Co2 C1 141.31(10) . . ? C2 Co2 C1 39.70(8) . . ? C21 Co2 Co1 147.07(8) . . ? C23 Co2 Co1 99.17(7) . . ? C22 Co2 Co1 98.10(8) . . ? C2 Co2 Co1 51.17(6) . . ? C1 Co2 Co1 51.17(6) . . ? C2 C1 C5 142.41(19) . 3_655 ? C2 C1 Co2 70.12(12) . . ? C5 C1 Co2 137.13(15) 3_655 . ? C2 C1 Co1 70.24(12) . . ? C5 C1 Co1 130.79(15) 3_655 . ? Co2 C1 Co1 77.97(7) . . ? C1 C2 C3 141.8(2) . . ? C1 C2 Co2 70.18(13) . . ? C3 C2 Co2 140.17(15) . . ? C1 C2 Co1 70.26(12) . . ? C3 C2 Co1 127.76(15) . . ? Co2 C2 Co1 78.00(8) . . ? N4 C3 C2 114.62(17) . . ? C5 N4 C3 110.05(16) . . ? C5 N4 C6 113.60(16) . . ? C3 N4 C6 112.03(17) . . ? N4 C5 C1 110.36(16) . 3_655 ? N4 C6 C7 114.84(19) . . ? N4 C6 C8 110.47(19) . . ? C7 C6 C8 110.3(2) . . ? O11 C11 Co1 179.0(2) . . ? O12 C12 Co1 179.0(2) . . ? O13 C13 Co1 177.1(2) . . ? O21 C21 Co2 176.6(2) . . ? O22 C22 Co2 177.5(3) . . ? O23 C23 Co2 178.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.454 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.078 #===END data_br16_25 _database_code_CSD 168782 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H10 Co2 O6 S' _chemical_formula_weight 436.15 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7265(1) _cell_length_b 14.0345(2) _cell_length_c 16.1067(2) _cell_angle_alpha 92.7570(10) _cell_angle_beta 96.672(1) _cell_angle_gamma 90.3120(10) _cell_volume 1732.63(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour red _exptl_crystal_size_max .32 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 2.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 17772 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7845 _reflns_number_gt 6694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0241P)^2^+2.2452P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7845 _refine_ls_number_parameters 452 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.195 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.005 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_1 Co -0.20626(5) 0.00320(3) 0.33545(3) 0.03039(10) Uani 1 1 d . . . Co2_1 Co 0.04233(5) 0.09755(3) 0.29838(3) 0.03037(10) Uani 1 1 d . . . C1_1 C -0.1706(4) 0.0549(2) 0.22598(19) 0.0301(6) Uani 1 1 d D . . C2_1 C -0.0674(3) -0.0194(2) 0.24206(18) 0.0274(6) Uani 1 1 d D . . C3_1 C 0.0158(4) -0.1071(2) 0.2102(2) 0.0313(6) Uani 1 1 d D . . H3A_1 H 0.1086 -0.1268 0.2534 0.038 Uiso 1 1 calc R . . H3B_1 H 0.0717 -0.0918 0.1601 0.038 Uiso 1 1 calc R . . S4_1 S -0.13481(11) -0.20667(6) 0.18287(5) 0.03704(18) Uani 1 1 d D . . C5_1 C -0.1616(5) -0.2069(2) 0.0694(2) 0.0457(8) Uani 1 1 d D . . H5A_1 H -0.0521 -0.2280 0.0482 0.055 Uiso 1 1 calc R . . H5B_1 H -0.2550 -0.2528 0.0468 0.055 Uiso 1 1 calc R . . C6_1 C -0.2056(5) -0.1128(3) 0.0398(2) 0.0419(8) Uani 1 1 d D . . C7_1 C -0.2333(5) -0.0329(3) 0.0229(2) 0.0432(8) Uani 1 1 d D . . C8_1 C -0.2690(5) 0.0675(3) 0.0069(2) 0.0465(9) Uani 1 1 d D . . H8A_1 H -0.3957 0.0754 -0.0088 0.056 Uiso 1 1 calc R . . H8B_1 H -0.2080 0.0864 -0.0406 0.056 Uiso 1 1 calc R . . C9_1 C -0.2092(5) 0.1327(2) 0.0839(2) 0.0456(8) Uani 1 1 d D . . H9A_1 H -0.2403 0.1992 0.0714 0.055 Uiso 1 1 calc R . . H9B_1 H -0.0807 0.1299 0.0955 0.055 Uiso 1 1 calc R . . C10_1 C -0.2911(4) 0.1054(3) 0.1635(2) 0.0433(8) Uani 1 1 d D . . H10A_1 H -0.3318 0.1643 0.1911 0.052 Uiso 1 1 calc R . . H10B_1 H -0.3945 0.0641 0.1460 0.052 Uiso 1 1 calc R . . C11_1 C -0.2913(4) 0.0957(2) 0.4024(2) 0.0375(7) Uani 1 1 d . . . O11_1 O -0.3411(4) 0.15334(19) 0.44459(18) 0.0532(7) Uani 1 1 d . . . C12_1 C -0.1036(4) -0.0810(2) 0.4079(2) 0.0383(7) Uani 1 1 d . . . O12_1 O -0.0403(4) -0.1358(2) 0.45062(18) 0.0591(7) Uani 1 1 d . . . C13_1 C -0.4065(4) -0.0591(3) 0.3001(2) 0.0480(9) Uani 1 1 d . . . O13_1 O -0.5335(4) -0.0968(3) 0.2775(2) 0.0812(11) Uani 1 1 d . . . C21_1 C -0.0270(4) 0.2166(2) 0.3305(2) 0.0388(7) Uani 1 1 d . . . O21_1 O -0.0774(4) 0.28947(18) 0.34771(19) 0.0574(7) Uani 1 1 d . . . C22_1 C 0.2027(4) 0.0557(3) 0.3792(2) 0.0425(8) Uani 1 1 d . . . O22_1 O 0.3023(3) 0.0267(2) 0.42927(18) 0.0638(8) Uani 1 1 d . . . C23_1 C 0.1873(4) 0.1277(3) 0.2237(2) 0.0425(8) Uani 1 1 d . . . O23_1 O 0.2802(4) 0.1460(2) 0.17737(19) 0.0667(8) Uani 1 1 d . . . Co1_2 Co 0.50051(5) 0.60060(3) 0.21101(2) 0.02329(9) Uani 1 1 d . . . Co2_2 Co 0.29661(5) 0.47383(3) 0.14836(2) 0.02437(9) Uani 1 1 d . . . C1_2 C 0.2924(3) 0.54974(19) 0.25490(16) 0.0241(5) Uani 1 1 d D A . C2_2 C 0.4200(3) 0.48635(19) 0.26314(16) 0.0236(5) Uani 1 1 d D A . C3_2 C 0.5208(4) 0.4190(2) 0.31852(19) 0.0326(6) Uani 1 1 d D . . H3A_2 H 0.5597 0.4531 0.3728 0.039 Uiso 0.525(5) 1 calc PR A 1 H3B_2 H 0.6263 0.3998 0.2927 0.039 Uiso 0.525(5) 1 calc PR A 1 H3C_2 H 0.5831 0.4557 0.3670 0.039 Uiso 0.475(5) 1 calc PR A 2 H3D_2 H 0.6093 0.3874 0.2872 0.039 Uiso 0.475(5) 1 calc PR A 2 S4_2 S 0.4039(6) 0.3138(3) 0.3381(3) 0.0385(8) Uani 0.525(5) 1 d PD A 1 C5_2 C 0.3629(5) 0.3485(3) 0.4434(2) 0.0489(9) Uani 1 1 d D . . H5A_2 H 0.2872 0.2991 0.4629 0.059 Uiso 0.525(5) 1 calc PR A 1 H5B_2 H 0.4752 0.3485 0.4799 0.059 Uiso 0.525(5) 1 calc PR A 1 H4C_2 H 0.2825 0.2965 0.4540 0.059 Uiso 0.475(5) 1 calc PR A 2 H4D_2 H 0.4712 0.3441 0.4824 0.059 Uiso 0.475(5) 1 calc PR A 2 C6_2 C 0.2820(5) 0.4410(3) 0.4551(2) 0.0449(9) Uani 1 1 d D A . C7_2 C 0.2220(5) 0.5184(3) 0.4599(2) 0.0466(9) Uani 1 1 d D . . C8_2 C 0.1454(5) 0.6138(3) 0.4560(2) 0.0529(10) Uani 1 1 d D A . H8A_2 H 0.1958 0.6553 0.5044 0.064 Uiso 0.525(5) 1 calc PR A 1 H8B_2 H 0.0177 0.6098 0.4569 0.064 Uiso 0.525(5) 1 calc PR A 1 H8C_2 H 0.1786 0.6488 0.5104 0.064 Uiso 0.475(5) 1 calc PR A 2 H8D_2 H 0.0170 0.6066 0.4487 0.064 Uiso 0.475(5) 1 calc PR A 2 C9_2 C 0.188(2) 0.6546(8) 0.3733(8) 0.044(3) Uani 0.525(5) 1 d PD A 1 H9A_2 H 0.1301 0.7170 0.3680 0.053 Uiso 0.525(5) 1 calc PR A 1 H9B_2 H 0.3154 0.6674 0.3792 0.053 Uiso 0.525(5) 1 calc PR A 1 C10_2 C 0.1412(4) 0.5967(2) 0.28966(19) 0.0324(6) Uani 1 1 d D . . H10A_2 H 0.0544 0.5470 0.2980 0.039 Uiso 0.525(5) 1 calc PR A 1 H10B_2 H 0.0855 0.6399 0.2479 0.039 Uiso 0.525(5) 1 calc PR A 1 H10C_2 H 0.0686 0.5474 0.3113 0.039 Uiso 0.475(5) 1 calc PR A 2 H10D_2 H 0.0687 0.6276 0.2440 0.039 Uiso 0.475(5) 1 calc PR A 2 C11_2 C 0.4084(4) 0.7041(2) 0.1582(2) 0.0341(7) Uani 1 1 d . . . O11_2 O 0.3467(4) 0.76693(18) 0.12664(18) 0.0590(7) Uani 1 1 d . . . C12_2 C 0.6808(4) 0.5618(2) 0.1566(2) 0.0356(7) Uani 1 1 d . . . O12_2 O 0.7919(3) 0.5360(2) 0.12117(19) 0.0606(8) Uani 1 1 d . . . C13_2 C 0.6215(4) 0.6571(2) 0.30216(19) 0.0350(7) Uani 1 1 d . . . O13_2 O 0.7005(4) 0.6909(2) 0.36027(16) 0.0596(8) Uani 1 1 d . . . C21_2 C 0.1809(4) 0.5489(2) 0.07142(17) 0.0287(6) Uani 1 1 d . . . O21_2 O 0.1107(3) 0.59927(17) 0.02666(14) 0.0433(6) Uani 1 1 d . . . C22_2 C 0.4381(5) 0.3959(3) 0.0938(2) 0.0432(8) Uani 1 1 d . . . O22_2 O 0.5250(4) 0.3469(2) 0.0599(2) 0.0783(10) Uani 1 1 d . . . C23_2 C 0.1229(5) 0.3914(2) 0.1589(2) 0.0380(7) Uani 1 1 d . . . O23_2 O 0.0107(4) 0.3415(2) 0.16583(19) 0.0633(8) Uani 1 1 d . . . C4_2 C 0.404(3) 0.3405(10) 0.3513(9) 0.049(5) Uani 0.475(5) 1 d PD A 2 H4A_2 H 0.2919 0.3381 0.3149 0.058 Uiso 0.475(5) 1 calc PR A 2 H4B_2 H 0.4613 0.2783 0.3429 0.058 Uiso 0.475(5) 1 calc PR A 2 S9_2 S 0.2078(7) 0.6860(3) 0.3737(2) 0.0409(9) Uani 0.475(5) 1 d PD A 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_1 0.02246(19) 0.0335(2) 0.0354(2) -0.00585(17) 0.00752(16) -0.00134(15) Co2_1 0.0234(2) 0.0318(2) 0.0358(2) -0.00603(17) 0.00631(16) -0.00331(15) C1_1 0.0212(13) 0.0327(15) 0.0360(16) -0.0050(12) 0.0039(11) -0.0001(11) C2_1 0.0198(13) 0.0314(15) 0.0303(14) -0.0042(11) 0.0029(11) -0.0026(11) C3_1 0.0227(14) 0.0322(15) 0.0385(16) -0.0055(12) 0.0041(12) 0.0023(11) S4_1 0.0424(4) 0.0273(4) 0.0413(4) 0.0022(3) 0.0047(3) -0.0033(3) C5_1 0.059(2) 0.0356(18) 0.0394(19) -0.0088(14) -0.0019(16) -0.0010(16) C6_1 0.0452(19) 0.049(2) 0.0300(16) 0.0014(14) -0.0017(14) 0.0039(16) C7_1 0.044(2) 0.054(2) 0.0319(17) 0.0051(15) 0.0039(14) 0.0023(16) C8_1 0.046(2) 0.054(2) 0.0417(19) 0.0207(16) 0.0044(16) 0.0070(17) C9_1 0.0426(19) 0.0376(18) 0.056(2) 0.0164(16) -0.0035(16) 0.0017(15) C10_1 0.0327(17) 0.046(2) 0.049(2) -0.0010(16) -0.0013(15) 0.0130(14) C11_1 0.0296(16) 0.0395(18) 0.0446(18) 0.0017(14) 0.0097(14) 0.0002(13) O11_1 0.0550(16) 0.0458(15) 0.0612(17) -0.0104(13) 0.0225(13) 0.0102(12) C12_1 0.0372(17) 0.0369(17) 0.0412(18) -0.0073(15) 0.0100(14) 0.0001(14) O12_1 0.0689(19) 0.0510(16) 0.0562(17) 0.0031(13) 0.0023(14) 0.0149(14) C13_1 0.0299(17) 0.058(2) 0.056(2) -0.0194(18) 0.0129(16) -0.0058(16) O13_1 0.0343(15) 0.093(2) 0.113(3) -0.046(2) 0.0166(16) -0.0216(15) C21_1 0.0344(17) 0.0422(19) 0.0406(18) -0.0040(14) 0.0106(14) -0.0073(14) O21_1 0.0665(18) 0.0368(14) 0.0720(19) -0.0111(13) 0.0268(15) 0.0036(12) C22_1 0.0289(16) 0.054(2) 0.0450(19) -0.0075(16) 0.0097(15) -0.0055(15) O22_1 0.0335(14) 0.103(2) 0.0541(17) 0.0109(16) -0.0028(12) 0.0041(14) C23_1 0.0314(17) 0.048(2) 0.048(2) -0.0115(16) 0.0075(15) -0.0057(14) O23_1 0.0442(15) 0.099(2) 0.0603(18) -0.0070(16) 0.0276(14) -0.0127(15) Co1_2 0.02373(19) 0.02375(19) 0.02238(18) 0.00227(14) 0.00225(14) -0.00148(14) Co2_2 0.02555(19) 0.02451(19) 0.02219(18) 0.00072(14) -0.00071(14) -0.00030(14) C1_2 0.0265(14) 0.0253(13) 0.0203(13) 0.0010(10) 0.0027(10) -0.0025(10) C2_2 0.0243(13) 0.0236(13) 0.0224(13) 0.0020(10) 0.0004(10) -0.0026(10) C3_2 0.0314(15) 0.0310(15) 0.0347(16) 0.0103(12) -0.0034(12) 0.0033(12) S4_2 0.0505(14) 0.0279(17) 0.0362(13) 0.0098(11) -0.0023(11) -0.0059(11) C5_2 0.053(2) 0.057(2) 0.0366(19) 0.0119(16) -0.0020(16) -0.0113(18) C6_2 0.0415(19) 0.068(3) 0.0260(16) 0.0079(16) 0.0037(14) -0.0111(18) C7_2 0.0401(19) 0.074(3) 0.0271(17) 0.0070(17) 0.0077(14) -0.0111(18) C8_2 0.047(2) 0.071(3) 0.042(2) 0.0006(18) 0.0146(17) 0.0019(19) C9_2 0.041(6) 0.041(8) 0.051(5) -0.013(5) 0.016(4) 0.005(6) C10_2 0.0246(14) 0.0422(17) 0.0305(15) -0.0017(13) 0.0046(12) 0.0063(12) C11_2 0.0382(17) 0.0289(16) 0.0340(16) 0.0008(13) -0.0008(13) -0.0042(13) O11_2 0.0751(19) 0.0356(14) 0.0627(18) 0.0149(13) -0.0122(15) 0.0056(13) C12_2 0.0335(16) 0.0354(17) 0.0370(17) -0.0021(13) 0.0031(13) -0.0050(13) O12_2 0.0377(14) 0.0730(19) 0.0729(19) -0.0200(15) 0.0236(14) -0.0025(13) C13_2 0.0361(16) 0.0408(17) 0.0288(15) 0.0057(13) 0.0052(13) -0.0099(13) O13_2 0.0652(18) 0.0748(19) 0.0346(13) -0.0024(13) -0.0081(12) -0.0299(15) C21_2 0.0286(14) 0.0345(16) 0.0220(13) -0.0009(12) 0.0004(11) -0.0035(12) O21_2 0.0469(14) 0.0446(13) 0.0357(12) 0.0077(10) -0.0096(10) 0.0038(11) C22_2 0.0395(18) 0.0427(19) 0.0452(19) -0.0139(15) 0.0015(15) 0.0009(15) O22_2 0.067(2) 0.070(2) 0.097(3) -0.0372(19) 0.0199(18) 0.0151(16) C23_2 0.0454(19) 0.0356(17) 0.0310(16) 0.0082(13) -0.0068(14) -0.0082(14) O23_2 0.0590(17) 0.0626(18) 0.0655(18) 0.0213(14) -0.0105(14) -0.0321(15) C4_2 0.068(8) 0.033(9) 0.039(7) 0.013(6) -0.021(5) -0.016(7) S9_2 0.0476(17) 0.037(2) 0.0395(12) -0.0092(11) 0.0144(10) 0.0041(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1_1 C13_1 1.793(3) . ? Co1_1 C12_1 1.821(4) . ? Co1_1 C11_1 1.822(3) . ? Co1_1 C2_1 1.962(3) . ? Co1_1 C1_1 1.986(3) . ? Co1_1 Co2_1 2.4727(6) . ? Co2_1 C23_1 1.799(4) . ? Co2_1 C22_1 1.811(4) . ? Co2_1 C21_1 1.827(4) . ? Co2_1 C2_1 1.975(3) . ? Co2_1 C1_1 1.975(3) . ? C1_1 C2_1 1.334(4) . ? C1_1 C10_1 1.497(4) . ? C2_1 C3_1 1.488(4) . ? C3_1 S4_1 1.818(3) . ? S4_1 C5_1 1.816(3) . ? C5_1 C6_1 1.453(5) . ? C6_1 C7_1 1.182(5) . ? C7_1 C8_1 1.466(5) . ? C8_1 C9_1 1.530(5) . ? C9_1 C10_1 1.556(5) . ? C11_1 O11_1 1.130(4) . ? C12_1 O12_1 1.132(4) . ? C13_1 O13_1 1.126(4) . ? C21_1 O21_1 1.130(4) . ? C22_1 O22_1 1.140(4) . ? C23_1 O23_1 1.131(4) . ? Co1_2 C13_2 1.795(3) . ? Co1_2 C12_2 1.804(3) . ? Co1_2 C11_2 1.824(3) . ? Co1_2 C1_2 1.973(3) . ? Co1_2 C2_2 1.976(3) . ? Co1_2 Co2_2 2.4684(5) . ? Co2_2 C23_2 1.795(3) . ? Co2_2 C22_2 1.819(3) . ? Co2_2 C21_2 1.823(3) . ? Co2_2 C2_2 1.979(3) . ? Co2_2 C1_2 1.979(3) . ? C1_2 C2_2 1.331(4) . ? C1_2 C10_2 1.496(4) . ? C2_2 C3_2 1.491(4) . ? C3_2 C4_2 1.567(13) . ? C3_2 S4_2 1.787(4) . ? S4_2 C5_2 1.806(5) . ? C5_2 C6_2 1.458(5) . ? C5_2 C4_2 1.552(13) . ? C6_2 C7_2 1.186(5) . ? C7_2 C8_2 1.468(6) . ? C8_2 C9_2 1.545(12) . ? C8_2 S9_2 1.814(5) . ? C9_2 C10_2 1.543(11) . ? C10_2 S9_2 1.826(5) . ? C11_2 O11_2 1.121(4) . ? C12_2 O12_2 1.136(4) . ? C13_2 O13_2 1.138(4) . ? C21_2 O21_2 1.130(4) . ? C22_2 O22_2 1.130(4) . ? C23_2 O23_2 1.131(4) . ? 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 C13_1 Co1_1 C12_1 100.35(18) . . ? C13_1 Co1_1 C11_1 98.71(15) . . ? C12_1 Co1_1 C11_1 104.46(15) . . ? C13_1 Co1_1 C2_1 103.03(14) . . ? C12_1 Co1_1 C2_1 99.61(13) . . ? C11_1 Co1_1 C2_1 143.87(14) . . ? C13_1 Co1_1 C1_1 96.45(16) . . ? C12_1 Co1_1 C1_1 138.64(13) . . ? C11_1 Co1_1 C1_1 109.97(14) . . ? C2_1 Co1_1 C1_1 39.48(12) . . ? C13_1 Co1_1 Co2_1 147.45(13) . . ? C12_1 Co1_1 Co2_1 103.42(11) . . ? C11_1 Co1_1 Co2_1 96.53(10) . . ? C2_1 Co1_1 Co2_1 51.33(8) . . ? C1_1 Co1_1 Co2_1 51.19(8) . . ? C23_1 Co2_1 C22_1 98.53(16) . . ? C23_1 Co2_1 C21_1 100.16(15) . . ? C22_1 Co2_1 C21_1 108.81(16) . . ? C23_1 Co2_1 C2_1 100.01(14) . . ? C22_1 Co2_1 C2_1 104.95(14) . . ? C21_1 Co2_1 C2_1 137.22(13) . . ? C23_1 Co2_1 C1_1 102.59(14) . . ? C22_1 Co2_1 C1_1 141.11(15) . . ? C21_1 Co2_1 C1_1 99.17(14) . . ? C2_1 Co2_1 C1_1 39.46(12) . . ? C23_1 Co2_1 Co1_1 149.98(11) . . ? C22_1 Co2_1 Co1_1 96.64(11) . . ? C21_1 Co2_1 Co1_1 99.23(10) . . ? C2_1 Co2_1 Co1_1 50.85(8) . . ? C1_1 Co2_1 Co1_1 51.57(9) . . ? C2_1 C1_1 C10_1 147.8(3) . . ? C2_1 C1_1 Co2_1 70.25(17) . . ? C10_1 C1_1 Co2_1 131.9(2) . . ? C2_1 C1_1 Co1_1 69.28(18) . . ? C10_1 C1_1 Co1_1 131.6(2) . . ? Co2_1 C1_1 Co1_1 77.24(11) . . ? C1_1 C2_1 C3_1 148.4(3) . . ? C1_1 C2_1 Co1_1 71.24(18) . . ? C3_1 C2_1 Co1_1 131.7(2) . . ? C1_1 C2_1 Co2_1 70.29(17) . . ? C3_1 C2_1 Co2_1 129.4(2) . . ? Co1_1 C2_1 Co2_1 77.82(10) . . ? C2_1 C3_1 S4_1 113.9(2) . . ? C5_1 S4_1 C3_1 101.64(16) . . ? C6_1 C5_1 S4_1 111.6(2) . . ? C7_1 C6_1 C5_1 173.7(4) . . ? C6_1 C7_1 C8_1 176.7(4) . . ? C7_1 C8_1 C9_1 111.5(3) . . ? C8_1 C9_1 C10_1 113.2(3) . . ? C1_1 C10_1 C9_1 114.6(3) . . ? O11_1 C11_1 Co1_1 178.8(3) . . ? O12_1 C12_1 Co1_1 177.4(3) . . ? O13_1 C13_1 Co1_1 178.8(4) . . ? O21_1 C21_1 Co2_1 176.5(3) . . ? O22_1 C22_1 Co2_1 178.0(4) . . ? O23_1 C23_1 Co2_1 179.1(4) . . ? C13_2 Co1_2 C12_2 98.72(14) . . ? C13_2 Co1_2 C11_2 100.95(14) . . ? C12_2 Co1_2 C11_2 106.73(15) . . ? C13_2 Co1_2 C1_2 103.07(12) . . ? C12_2 Co1_2 C1_2 140.84(13) . . ? C11_2 Co1_2 C1_2 100.60(13) . . ? C13_2 Co1_2 C2_2 98.34(12) . . ? C12_2 Co1_2 C2_2 105.69(13) . . ? C11_2 Co1_2 C2_2 138.92(13) . . ? C1_2 Co1_2 C2_2 39.38(11) . . ? C13_2 Co1_2 Co2_2 149.28(10) . . ? C12_2 Co1_2 Co2_2 95.54(10) . . ? C11_2 Co1_2 Co2_2 100.76(10) . . ? C1_2 Co1_2 Co2_2 51.46(8) . . ? C2_2 Co1_2 Co2_2 51.43(8) . . ? C23_2 Co2_2 C22_2 99.73(16) . . ? C23_2 Co2_2 C21_2 98.42(14) . . ? C22_2 Co2_2 C21_2 107.66(15) . . ? C23_2 Co2_2 C2_2 102.87(13) . . ? C22_2 Co2_2 C2_2 102.90(14) . . ? C21_2 Co2_2 C2_2 138.88(12) . . ? C23_2 Co2_2 C1_2 98.67(13) . . ? C22_2 Co2_2 C1_2 141.09(14) . . ? C21_2 Co2_2 C1_2 103.14(12) . . ? C2_2 Co2_2 C1_2 39.29(11) . . ? C23_2 Co2_2 Co1_2 149.31(11) . . ? C22_2 Co2_2 Co1_2 102.21(11) . . ? C21_2 Co2_2 Co1_2 95.09(9) . . ? C2_2 Co2_2 Co1_2 51.32(8) . . ? C1_2 Co2_2 Co1_2 51.25(8) . . ? C2_2 C1_2 C10_2 148.6(3) . . ? C2_2 C1_2 Co1_2 70.40(16) . . ? C10_2 C1_2 Co1_2 132.7(2) . . ? C2_2 C1_2 Co2_2 70.32(16) . . ? C10_2 C1_2 Co2_2 128.9(2) . . ? Co1_2 C1_2 Co2_2 77.29(10) . . ? C1_2 C2_2 C3_2 147.1(3) . . ? C1_2 C2_2 Co1_2 70.21(16) . . ? C3_2 C2_2 Co1_2 129.6(2) . . ? C1_2 C2_2 Co2_2 70.38(16) . . ? C3_2 C2_2 Co2_2 133.7(2) . . ? Co1_2 C2_2 Co2_2 77.25(9) . . ? C2_2 C3_2 C4_2 113.4(9) . . ? C2_2 C3_2 S4_2 114.8(3) . . ? C4_2 C3_2 S4_2 12.4(5) . . ? C3_2 S4_2 C5_2 97.2(2) . . ? C6_2 C5_2 C4_2 106.7(7) . . ? C6_2 C5_2 S4_2 116.5(3) . . ? C4_2 C5_2 S4_2 11.6(5) . . ? C7_2 C6_2 C5_2 175.2(4) . . ? C6_2 C7_2 C8_2 173.9(4) . . ? C7_2 C8_2 C9_2 106.7(6) . . ? C7_2 C8_2 S9_2 115.7(3) . . ? C9_2 C8_2 S9_2 13.0(4) . . ? C10_2 C9_2 C8_2 120.0(7) . . ? C1_2 C10_2 C9_2 114.6(8) . . ? C1_2 C10_2 S9_2 112.9(3) . . ? C9_2 C10_2 S9_2 12.6(5) . . ? O11_2 C11_2 Co1_2 177.7(3) . . ? O12_2 C12_2 Co1_2 178.5(3) . . ? O13_2 C13_2 Co1_2 178.3(3) . . ? O21_2 C21_2 Co2_2 176.4(3) . . ? O22_2 C22_2 Co2_2 179.4(4) . . ? O23_2 C23_2 Co2_2 178.1(4) . . ? C5_2 C4_2 C3_2 119.5(8) . . ? C8_2 S9_2 C10_2 94.6(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.383 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.072 #===END data_br10_2 _database_code_CSD 168783 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H18 S' _chemical_formula_weight 206.33 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.0282(9) _cell_length_b 9.4287(9) _cell_length_c 13.6170(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1159.14(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .29 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _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 2431 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1187 _reflns_number_gt 865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0520P)^2^+0.2385P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1187 _refine_ls_number_parameters 73 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.076 _refine_ls_shift/su_mean 0.010 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 0.46127(19) 0.95313(18) 0.67425(12) 0.0273(4) Uani 1 1 d . . . C2 C 0.37754(19) 0.87534(18) 0.63386(12) 0.0276(4) Uani 1 1 d . . . C3 C 0.27674(19) 0.77866(19) 0.58195(13) 0.0318(5) Uani 1 1 d D B . H3A H 0.2180 0.7255 0.6311 0.038 Uiso 1 1 calc R . . H3B H 0.3365 0.7090 0.5447 0.038 Uiso 1 1 calc R . . C4 C 0.1704(2) 0.8525(2) 0.51107(13) 0.0352(5) Uani 1 1 d DU . . H4A H 0.0958 0.9032 0.5512 0.042 Uiso 1 1 calc R A 1 H4B H 0.1170 0.7776 0.4744 0.042 Uiso 1 1 calc R A 1 S5 S 0.2373(4) 0.9689(3) 0.42787(17) 0.0274(4) Uani 0.50 1 d PDU B 1 C5 C 0.2543(16) 0.9490(14) 0.4307(8) 0.056(4) Uani 0.50 1 d PDU B 2 H5A H 0.1800 1.0060 0.3946 0.067 Uiso 0.50 1 calc PR B 2 H5B H 0.3214 1.0155 0.4650 0.067 Uiso 0.50 1 calc PR B 2 C6 C 0.3480(2) 0.85864(18) 0.35383(12) 0.0306(5) Uani 1 1 d DU . . H6A H 0.4189 0.8056 0.3954 0.037 Uiso 1 1 calc R B 1 H6B H 0.2848 0.7892 0.3190 0.037 Uiso 1 1 calc R B 1 C7 C 0.4328(2) 0.94928(19) 0.27907(12) 0.0315(5) Uani 1 1 d D . . H7A H 0.4870 0.8860 0.2335 0.038 Uiso 1 1 calc R . . H7B H 0.3610 1.0050 0.2399 0.038 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 C1 0.0261(9) 0.0305(9) 0.0254(9) 0.0029(8) 0.0012(7) 0.0004(8) C2 0.0252(9) 0.0290(9) 0.0287(9) 0.0034(8) 0.0033(8) 0.0001(8) C3 0.0289(9) 0.0318(10) 0.0347(10) 0.0020(8) -0.0004(8) -0.0089(8) C4 0.0268(9) 0.0406(12) 0.0382(10) -0.0086(9) -0.0032(8) 0.0002(8) S5 0.0327(8) 0.0229(7) 0.0267(8) -0.0010(6) 0.0038(6) 0.0014(7) C5 0.068(8) 0.044(6) 0.055(5) 0.011(4) -0.017(4) -0.007(4) C6 0.0305(10) 0.0277(10) 0.0336(10) -0.0037(8) 0.0013(8) -0.0032(8) C7 0.0310(10) 0.0376(11) 0.0258(9) -0.0029(8) -0.0024(7) -0.0048(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 C1 C2 1.188(2) . ? C1 C7 1.471(2) 5_676 ? C2 C3 1.469(2) . ? C3 C4 1.529(2) . ? C4 C5 1.613(10) . ? C4 S5 1.689(3) . ? S5 C6 1.760(3) . ? C5 C6 1.592(10) . ? C6 C7 1.534(2) . ? C7 C1 1.471(2) 5_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C7 178.01(17) . 5_676 ? C1 C2 C3 178.56(18) . . ? C2 C3 C4 114.22(15) . . ? C3 C4 C5 113.0(6) . . ? C3 C4 S5 119.64(18) . . ? C5 C4 S5 8.1(6) . . ? C4 S5 C6 101.73(19) . . ? C6 C5 C4 113.2(8) . . ? C7 C6 C5 113.8(5) . . ? C7 C6 S5 109.55(14) . . ? C5 C6 S5 6.2(6) . . ? C1 C7 C6 112.70(13) 5_676 . ? _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.892 _refine_diff_density_max 0.222 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.040 #===END _eof # End of Crystallographic Information File