data_asb259 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H68 Ca Cl2 Co F3 N4 O15 S4' _chemical_formula_weight 1260.18 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 '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 11.2366(6) _cell_length_b 15.2439(7) _cell_length_c 17.5369(9) _cell_angle_alpha 71.8050(6) _cell_angle_beta 84.3928(6) _cell_angle_gamma 77.3591(6) _cell_volume 2783.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9271 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.48 _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.7895 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33463 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.63 _reflns_number_total 13276 _reflns_number_gt 11430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0534P)^2^+2.3073P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap & geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13276 _refine_ls_number_parameters 937 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL asb259 in P-1 CELL 0.71073 11.2366 15.2439 17.5369 71.8050 84.3928 77.3591 ZERR 2.00 0.0006 0.0007 0.0009 0.0006 0.0006 0.0006 LATT 1 SFAC C H N O F S CL CA CO UNIT 90 136 8 30 6 8 4 2 2 TEMP -185.000 SIZE 0.092 0.242 0.343 rem David Lacy 25s sphere ccd1 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 OMIT 0 1 0 OMIT 0 0 1 CONN 8 CA1 DFIX 0.85 0.001 O7 H7 L.S. 12 ACTA 51 WGHT 0.053400 2.307300 FVAR 0.13027 CO1 9 0.875216 0.811066 0.722949 11.00000 0.01501 0.01239 = 0.00923 -0.00175 0.00059 -0.00316 CA1 8 1.108816 0.592717 0.712362 11.00000 0.01704 0.01341 = 0.00994 -0.00291 -0.00046 -0.00261 S1 6 1.157280 0.833777 0.664253 11.00000 0.01571 0.01504 = 0.01153 -0.00368 0.00010 -0.00427 S2 6 0.819079 0.698338 0.608209 11.00000 0.01893 0.01629 = 0.01029 -0.00277 -0.00115 -0.00441 S3 6 0.800631 0.744227 0.916029 11.00000 0.01751 0.01874 = 0.00979 -0.00271 0.00100 -0.00436 O1 4 1.184150 0.731382 0.692601 11.00000 0.01788 0.01541 = 0.01810 -0.00587 -0.00061 -0.00347 O2 4 1.193665 0.874137 0.581531 11.00000 0.02123 0.02406 = 0.01201 -0.00486 0.00267 -0.00881 O3 4 0.944547 0.647869 0.622456 11.00000 0.02157 0.01711 = 0.01415 -0.00526 -0.00385 -0.00017 O4 4 0.728682 0.641723 0.642401 11.00000 0.02734 0.02400 = 0.01497 -0.00271 0.00228 -0.01191 O5 4 0.874382 0.653821 0.915107 11.00000 0.02247 0.02047 = 0.01267 0.00006 0.00189 0.00094 O6 4 0.838269 0.786069 0.970371 11.00000 0.02333 0.03418 = 0.01636 -0.00962 -0.00027 -0.01089 O7 4 0.960218 0.688193 0.762676 11.00000 0.02116 0.01499 = 0.01086 -0.00232 0.00158 -0.00115 H7 2 0.930832 0.665615 0.809506 11.00000 0.04126 O8 4 1.210707 0.534696 0.845533 11.00000 0.01985 0.01667 = 0.01241 -0.00167 -0.00085 0.00074 O9 4 1.332852 0.529895 0.710238 11.00000 0.01767 0.02300 = 0.01375 -0.00420 0.00089 -0.00270 O10 4 1.209191 0.580174 0.579172 11.00000 0.02268 0.01811 = 0.01585 -0.00536 0.00253 -0.00564 O11 4 1.079768 0.452346 0.675874 11.00000 0.02218 0.01958 = 0.01195 -0.00442 0.00189 -0.00748 O12 4 1.016360 0.471738 0.819888 11.00000 0.02483 0.01802 = 0.01208 -0.00146 -0.00077 -0.00504 N1 3 0.776808 0.941521 0.682792 11.00000 0.01633 0.01594 = 0.01372 -0.00186 0.00147 -0.00329 N2 3 1.015259 0.872016 0.679456 11.00000 0.01581 0.01342 = 0.01477 -0.00113 0.00004 -0.00358 N3 3 0.800725 0.791062 0.635475 11.00000 0.01804 0.01672 = 0.01407 -0.00400 -0.00377 0.00005 N4 3 0.792150 0.814314 0.826091 11.00000 0.02097 0.01440 = 0.01081 -0.00184 0.00240 -0.00295 C1 1 0.858383 1.009113 0.675618 11.00000 0.02224 0.01495 = 0.01995 -0.00285 0.00133 -0.00526 C2 1 0.979824 0.974352 0.638256 11.00000 0.01886 0.01500 = 0.01754 0.00138 -0.00008 -0.00427 C3 1 1.237006 0.874351 0.726233 11.00000 0.01455 0.01488 = 0.01512 -0.00450 -0.00281 -0.00077 C4 1 1.306857 0.944991 0.692711 11.00000 0.01530 0.01668 = 0.01724 -0.00407 -0.00205 -0.00062 C5 1 1.358035 0.977729 0.745733 11.00000 0.01738 0.01607 = 0.02384 -0.00483 -0.00334 -0.00334 C6 1 1.343703 0.943760 0.828474 11.00000 0.01871 0.01697 = 0.02291 -0.00763 -0.00777 0.00147 C7 1 1.277070 0.872837 0.859117 11.00000 0.02213 0.01774 = 0.01466 -0.00451 -0.00424 0.00073 C8 1 1.222132 0.837652 0.810682 11.00000 0.01795 0.01477 = 0.01627 -0.00335 -0.00178 -0.00135 C9 1 1.331354 0.989646 0.604346 11.00000 0.02325 0.02258 = 0.01823 -0.00308 0.00118 -0.01086 C10 1 1.392370 0.984646 0.883815 11.00000 0.02972 0.02112 = 0.02498 -0.00710 -0.01111 -0.00349 C11 1 1.149347 0.762879 0.852040 11.00000 0.03233 0.02409 = 0.01275 -0.00290 -0.00141 -0.01165 C12 1 0.724746 0.955388 0.603678 11.00000 0.02100 0.01924 = 0.01582 -0.00162 -0.00286 -0.00095 C13 1 0.690674 0.863421 0.606489 11.00000 0.01696 0.02186 = 0.01703 -0.00427 -0.00321 -0.00026 C14 1 0.805427 0.738551 0.501361 11.00000 0.01960 0.01646 = 0.01045 -0.00248 -0.00077 -0.00482 C15 1 0.903578 0.773593 0.453800 11.00000 0.01982 0.01286 = 0.01730 -0.00289 0.00036 -0.00186 C16 1 0.898349 0.796134 0.370357 11.00000 0.02663 0.01587 = 0.01768 -0.00166 0.00588 -0.00120 C17 1 0.800291 0.785465 0.333646 11.00000 0.03648 0.01788 = 0.01232 -0.00330 -0.00305 0.00338 C18 1 0.702993 0.756721 0.381548 11.00000 0.02876 0.02453 = 0.01990 -0.00703 -0.00950 -0.00260 C19 1 0.700987 0.733435 0.465299 11.00000 0.02112 0.02134 = 0.01705 -0.00464 -0.00311 -0.00550 C20 1 1.014193 0.788205 0.486734 11.00000 0.01976 0.01970 = 0.02750 -0.00301 0.00022 -0.00676 C21 1 0.799867 0.804406 0.243858 11.00000 0.05803 0.03104 = 0.01441 -0.00632 -0.00482 0.01328 AFIX 137 H21A 2 0.781373 0.750093 0.232165 11.00000 -1.50000 H21B 2 0.880232 0.814919 0.220353 11.00000 -1.50000 H21C 2 0.737721 0.860501 0.220779 11.00000 -1.50000 AFIX 0 C22 1 0.586673 0.704855 0.509006 11.00000 0.02378 0.03635 = 0.02908 -0.00463 -0.00511 -0.01234 C23 1 0.674350 0.954732 0.742220 11.00000 0.02053 0.01718 = 0.02003 -0.00415 0.00498 -0.00119 C24 1 0.721740 0.909150 0.825006 11.00000 0.02641 0.01531 = 0.01770 -0.00530 0.00661 -0.00221 C25 1 0.650212 0.722221 0.947212 11.00000 0.01772 0.01587 = 0.01082 -0.00099 0.00082 -0.00409 C26 1 0.604012 0.665794 0.911357 11.00000 0.02528 0.01794 = 0.01287 -0.00419 0.00186 -0.00642 C27 1 0.495729 0.636704 0.942709 11.00000 0.02434 0.02127 = 0.01669 -0.00574 -0.00085 -0.00892 C28 1 0.430871 0.662416 1.006622 11.00000 0.01768 0.01846 = 0.01573 -0.00003 -0.00130 -0.00303 C29 1 0.474241 0.722532 1.037407 11.00000 0.01955 0.01870 = 0.01239 -0.00260 0.00085 -0.00038 C30 1 0.582916 0.753587 1.009753 11.00000 0.02064 0.01540 = 0.01028 -0.00156 -0.00153 -0.00219 C31 1 0.664258 0.635590 0.840075 11.00000 0.03709 0.03286 = 0.02091 -0.01607 0.00911 -0.01902 C32 1 0.316908 0.625729 1.041947 11.00000 0.02130 0.03157 = 0.02220 -0.00559 0.00182 -0.00972 C33 1 0.618816 0.818095 1.049759 11.00000 0.02714 0.02449 = 0.01695 -0.01023 0.00443 -0.00883 C34 1 1.317755 0.462708 0.849997 11.00000 0.02168 0.01892 = 0.01795 -0.00351 -0.00414 0.00150 C35 1 1.401529 0.500109 0.781389 11.00000 0.01915 0.02550 = 0.01897 -0.00644 -0.00374 -0.00211 C36 1 1.407935 0.543753 0.638320 11.00000 0.01988 0.03250 = 0.01815 -0.00519 0.00513 -0.00629 C37 1 1.325939 0.606429 0.570092 11.00000 0.02423 0.02575 = 0.01619 -0.00356 0.00422 -0.00850 C38 1 1.211885 0.492903 0.563397 11.00000 0.03111 0.02284 = 0.01684 -0.00941 0.00515 -0.00700 C39 1 1.090670 0.465517 0.591036 11.00000 0.03057 0.01955 = 0.01426 -0.00773 -0.00049 -0.00569 C40 1 0.966053 0.427487 0.709968 11.00000 0.02419 0.02024 = 0.01941 -0.00578 0.00093 -0.00994 C41 1 0.975367 0.399312 0.800157 11.00000 0.02732 0.02143 = 0.01836 -0.00339 0.00442 -0.01079 C42 1 1.056552 0.440533 0.901097 11.00000 0.02557 0.02583 = 0.01014 0.00043 0.00093 -0.00417 C43 1 1.124269 0.511198 0.910840 11.00000 0.02306 0.02447 = 0.01080 -0.00280 0.00041 -0.00066 C44 1 1.287244 0.702920 0.288570 11.00000 0.02713 0.03228 = 0.03093 -0.01332 0.00573 -0.00889 S4 6 1.405972 0.772049 0.266628 11.00000 0.01948 0.02293 = 0.02446 -0.01011 -0.00255 -0.00193 O13 4 1.514744 0.703890 0.260282 11.00000 0.02206 0.03257 = 0.04763 -0.02127 -0.00322 0.00087 O14 4 1.397253 0.806282 0.335433 11.00000 0.03700 0.02934 = 0.03032 -0.01532 -0.01064 0.00155 O15 4 1.367753 0.843148 0.192300 11.00000 0.03535 0.03083 = 0.02407 -0.00517 0.00038 -0.00565 F1 5 1.303499 0.633840 0.358373 11.00000 0.07423 0.04332 = 0.03800 0.00003 0.00704 -0.02686 F2 5 1.176990 0.756516 0.291973 11.00000 0.02173 0.05560 = 0.08170 -0.03474 0.01314 -0.00935 F3 5 1.284891 0.661317 0.231918 11.00000 0.03884 0.05206 = 0.05152 -0.03204 0.00304 -0.02006 C45 1 1.113335 0.928896 1.086072 11.00000 0.03268 0.04852 = 0.03933 -0.01296 -0.00414 0.00039 CL1 7 1.057546 0.842974 1.059844 11.00000 0.08426 0.04449 = 0.04354 -0.02002 0.01596 -0.01443 CL2 7 1.000154 0.986532 1.141302 11.00000 0.03877 0.04745 = 0.05131 -0.02403 -0.00266 -0.00469 H1A 2 0.869503 1.010108 0.727971 11.00000 0.01865 H1B 2 0.821603 1.073156 0.643752 11.00000 0.01591 H2A 2 0.977115 0.985239 0.579916 11.00000 0.01927 H2B 2 1.038349 1.009864 0.646285 11.00000 0.01662 H5A 2 1.402479 1.026969 0.723113 11.00000 0.01969 H7A 2 1.265063 0.850672 0.911422 11.00000 0.02387 H9A 2 1.380951 1.035343 0.597415 11.00000 0.02274 H9B 2 1.256245 1.021992 0.575402 11.00000 0.02628 H9C 2 1.375513 0.946648 0.578288 11.00000 0.03065 H10A 2 1.451483 1.024867 0.854439 11.00000 0.02994 H10B 2 1.432999 0.934020 0.926063 11.00000 0.02971 H10C 2 1.329116 1.024598 0.903760 11.00000 0.03548 H11A 2 1.137290 0.763693 0.906029 11.00000 0.03502 H11B 2 1.195535 0.704270 0.852072 11.00000 0.03618 H11C 2 1.081607 0.769873 0.827284 11.00000 0.04514 H12A 2 0.788155 0.970024 0.560833 11.00000 0.01634 H12B 2 0.654949 1.009112 0.594583 11.00000 0.02780 H13A 2 0.620844 0.853816 0.642697 11.00000 0.02247 H13B 2 0.674695 0.863500 0.553467 11.00000 0.01912 H16A 2 0.964426 0.822241 0.337701 11.00000 0.02636 H18A 2 0.633811 0.754026 0.360753 11.00000 0.03705 H20A 2 1.059602 0.828999 0.442930 11.00000 0.02812 H20B 2 1.064684 0.733447 0.508667 11.00000 0.02481 H20C 2 0.990905 0.813664 0.526561 11.00000 0.02926 H22A 2 0.525197 0.720442 0.470970 11.00000 0.03592 H22B 2 0.557876 0.733518 0.551915 11.00000 0.03017 H22C 2 0.600271 0.641847 0.530367 11.00000 0.03024 H23A 2 0.638842 1.021836 0.730628 11.00000 0.01959 H23B 2 0.611970 0.924043 0.733651 11.00000 0.01962 H24A 2 0.775621 0.945806 0.839642 11.00000 0.01907 H24B 2 0.652553 0.906398 0.862334 11.00000 0.02979 H27A 2 0.467106 0.600000 0.919563 11.00000 0.02530 H29A 2 0.426423 0.744427 1.079526 11.00000 0.02080 H31A 2 0.607974 0.608262 0.819125 11.00000 0.02912 H31B 2 0.735508 0.587214 0.856807 11.00000 0.04169 H31C 2 0.682967 0.684733 0.798538 11.00000 0.04232 H32A 2 0.250503 0.675528 1.042570 11.00000 0.04879 H32B 2 0.325637 0.586480 1.093550 11.00000 0.05961 H32C 2 0.289917 0.595293 1.015415 11.00000 0.07303 H33A 2 0.548860 0.835790 1.082451 11.00000 0.02562 H33B 2 0.642452 0.873714 1.012580 11.00000 0.03034 H33C 2 0.680952 0.791870 1.078376 11.00000 0.02679 H34A 2 1.295566 0.409579 0.845074 11.00000 0.01960 H34B 2 1.356103 0.451086 0.899119 11.00000 0.02329 H35A 2 1.426816 0.551012 0.787193 11.00000 0.02265 H35B 2 1.467111 0.450838 0.777947 11.00000 0.02232 H36A 2 1.443574 0.485259 0.631827 11.00000 0.03194 H36B 2 1.470044 0.572171 0.640103 11.00000 0.02681 H37A 2 1.305361 0.670373 0.572053 11.00000 0.01919 H37B 2 1.364500 0.604025 0.517009 11.00000 0.02923 H38A 2 1.278400 0.445507 0.592988 11.00000 0.02898 H38B 2 1.225135 0.501508 0.507846 11.00000 0.02712 H39A 2 1.025149 0.514124 0.566025 11.00000 0.01048 H39B 2 1.086988 0.410533 0.582674 11.00000 0.01774 H40A 2 0.958089 0.371893 0.697570 11.00000 0.01945 H40B 2 0.897375 0.481345 0.689701 11.00000 0.01687 H41A 2 0.898811 0.389889 0.826354 11.00000 0.02979 H41B 2 1.035645 0.339413 0.819319 11.00000 0.02187 H42A 2 1.106776 0.381491 0.907957 11.00000 0.01869 H42B 2 0.990580 0.437868 0.934525 11.00000 0.02296 H43A 2 1.070129 0.568818 0.909656 11.00000 0.01511 H43B 2 1.165191 0.485350 0.961854 11.00000 0.03371 H45A 2 1.125835 0.979724 1.028080 11.00000 0.06430 H45B 2 1.181848 0.898387 1.118605 11.00000 0.05660 HKLF 4 REM asb259 in P-1 REM R1 = 0.0346 for 11430 Fo > 4sig(Fo) and 0.0423 for all 13276 data REM 937 parameters refined using 1 restraints END WGHT 0.0534 2.3065 REM Highest difference peak 0.747, deepest hole -0.983, 1-sigma level 0.073 Q1 1 1.3429 0.7388 0.2814 11.00000 0.05 0.75 Q2 1 1.1914 0.8549 0.6878 11.00000 0.05 0.48 Q3 1 0.8566 0.7653 0.7202 11.00000 0.05 0.47 Q4 1 1.0788 0.8590 0.6711 11.00000 0.05 0.47 Q5 1 0.4122 0.8458 0.4852 11.00000 0.05 0.46 Q6 1 0.4594 0.6929 1.0187 11.00000 0.05 0.44 Q7 1 0.7236 0.7394 0.9307 11.00000 0.05 0.44 Q8 1 0.7433 0.8268 0.6169 11.00000 0.05 0.42 Q9 1 0.9474 0.7957 0.7235 11.00000 0.05 0.41 Q10 1 0.9359 0.8428 0.7074 11.00000 0.05 0.41 Q11 1 0.8432 0.7955 0.3610 11.00000 0.05 0.41 Q12 1 0.7688 0.6726 0.6219 11.00000 0.05 0.41 Q13 1 0.8167 0.9701 0.6780 11.00000 0.05 0.40 Q14 1 0.5404 0.6620 0.9207 11.00000 0.05 0.40 Q15 1 0.8036 0.8365 0.7217 11.00000 0.05 0.39 Q16 1 1.1479 0.4860 0.5813 11.00000 0.05 0.38 Q17 1 0.3806 0.6427 1.0247 11.00000 0.05 0.38 Q18 1 1.3018 0.7312 0.3392 11.00000 0.05 0.38 Q19 1 0.6099 0.7840 1.0322 11.00000 0.05 0.38 Q20 1 1.3248 0.9630 0.7242 11.00000 0.05 0.37 ; 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 0.87522(2) 0.811066(17) 0.722949(14) 0.01256(6) Uani 1 1 d . . . Ca1 Ca 1.10882(3) 0.59272(2) 0.71236(2) 0.01367(8) Uani 1 1 d . . . S1 S 1.15728(4) 0.83378(3) 0.66425(3) 0.01401(9) Uani 1 1 d . . . S2 S 0.81908(4) 0.69834(3) 0.60821(3) 0.01526(9) Uani 1 1 d . . . S3 S 0.80063(4) 0.74423(3) 0.91603(3) 0.01569(9) Uani 1 1 d . . . O1 O 1.18415(12) 0.73138(9) 0.69260(8) 0.0169(3) Uani 1 1 d . . . O2 O 1.19367(12) 0.87414(10) 0.58153(8) 0.0188(3) Uani 1 1 d . . . O3 O 0.94455(12) 0.64787(9) 0.62246(8) 0.0178(3) Uani 1 1 d . . . O4 O 0.72868(13) 0.64172(10) 0.64240(8) 0.0220(3) Uani 1 1 d . . . O5 O 0.87438(13) 0.65382(10) 0.91511(8) 0.0207(3) Uani 1 1 d . . . O6 O 0.83827(13) 0.78607(11) 0.97037(8) 0.0233(3) Uani 1 1 d . . . O7 O 0.96022(12) 0.68819(9) 0.76268(8) 0.0166(3) Uani 1 1 d D . . H7 H 0.931(2) 0.6656(19) 0.8095(7) 0.041(8) Uiso 1 1 d D . . O8 O 1.21071(12) 0.53470(9) 0.84553(8) 0.0176(3) Uani 1 1 d . . . O9 O 1.33285(12) 0.52990(10) 0.71024(8) 0.0188(3) Uani 1 1 d . . . O10 O 1.20919(13) 0.58017(9) 0.57917(8) 0.0188(3) Uani 1 1 d . . . O11 O 1.07977(12) 0.45235(9) 0.67587(8) 0.0176(3) Uani 1 1 d . . . O12 O 1.01636(13) 0.47174(9) 0.81989(8) 0.0189(3) Uani 1 1 d . . . N1 N 0.77681(14) 0.94152(11) 0.68279(9) 0.0161(3) Uani 1 1 d . . . N2 N 1.01526(14) 0.87202(11) 0.67946(9) 0.0153(3) Uani 1 1 d . . . N3 N 0.80073(14) 0.79106(11) 0.63548(9) 0.0168(3) Uani 1 1 d . . . N4 N 0.79215(15) 0.81431(11) 0.82609(9) 0.0161(3) Uani 1 1 d . . . C1 C 0.85838(18) 1.00911(14) 0.67562(12) 0.0195(4) Uani 1 1 d . . . C2 C 0.97982(18) 0.97435(13) 0.63826(12) 0.0185(4) Uani 1 1 d . . . C3 C 1.23701(16) 0.87435(13) 0.72623(11) 0.0150(3) Uani 1 1 d . . . C4 C 1.30686(17) 0.94499(13) 0.69271(11) 0.0169(4) Uani 1 1 d . . . C5 C 1.35803(18) 0.97773(14) 0.74573(12) 0.0192(4) Uani 1 1 d . . . C6 C 1.34370(18) 0.94376(14) 0.82847(12) 0.0194(4) Uani 1 1 d . . . C7 C 1.27707(18) 0.87284(14) 0.85912(12) 0.0188(4) Uani 1 1 d . . . C8 C 1.22213(17) 0.83765(13) 0.81068(11) 0.0169(4) Uani 1 1 d . . . C9 C 1.3314(2) 0.98965(15) 0.60435(12) 0.0212(4) Uani 1 1 d . . . C10 C 1.3924(2) 0.98465(16) 0.88382(13) 0.0248(4) Uani 1 1 d . . . C11 C 1.1493(2) 0.76288(16) 0.85204(12) 0.0227(4) Uani 1 1 d . . . C12 C 0.72475(19) 0.95539(14) 0.60368(12) 0.0199(4) Uani 1 1 d . . . C13 C 0.69067(18) 0.86342(14) 0.60649(12) 0.0194(4) Uani 1 1 d . . . C14 C 0.80543(17) 0.73855(13) 0.50136(10) 0.0157(3) Uani 1 1 d . . . C15 C 0.90358(17) 0.77359(13) 0.45380(11) 0.0173(4) Uani 1 1 d . . . C16 C 0.89835(19) 0.79613(14) 0.37036(12) 0.0218(4) Uani 1 1 d . . . C17 C 0.8003(2) 0.78547(14) 0.33365(11) 0.0238(4) Uani 1 1 d . . . C18 C 0.7030(2) 0.75672(15) 0.38155(12) 0.0241(4) Uani 1 1 d . . . C19 C 0.70099(18) 0.73343(14) 0.46530(12) 0.0197(4) Uani 1 1 d . . . C20 C 1.01419(19) 0.78820(15) 0.48673(14) 0.0229(4) Uani 1 1 d . . . C21 C 0.7999(3) 0.80441(18) 0.24386(13) 0.0379(6) Uani 1 1 d . . . H21A H 0.7814 0.7501 0.2322 0.057 Uiso 1 1 calc R . . H21B H 0.8802 0.8149 0.2204 0.057 Uiso 1 1 calc R . . H21C H 0.7377 0.8605 0.2208 0.057 Uiso 1 1 calc R . . C22 C 0.5867(2) 0.70486(19) 0.50901(15) 0.0296(5) Uani 1 1 d . . . C23 C 0.67435(19) 0.95473(14) 0.74222(12) 0.0204(4) Uani 1 1 d . . . C24 C 0.72174(19) 0.90915(14) 0.82501(12) 0.0205(4) Uani 1 1 d . . . C25 C 0.65021(17) 0.72222(13) 0.94721(10) 0.0155(3) Uani 1 1 d . . . C26 C 0.60401(18) 0.66579(13) 0.91136(11) 0.0186(4) Uani 1 1 d . . . C27 C 0.49573(19) 0.63670(14) 0.94271(12) 0.0200(4) Uani 1 1 d . . . C28 C 0.43087(17) 0.66242(14) 1.00662(11) 0.0185(4) Uani 1 1 d . . . C29 C 0.47424(18) 0.72253(14) 1.03741(11) 0.0180(4) Uani 1 1 d . . . C30 C 0.58292(17) 0.75359(13) 1.00975(10) 0.0161(4) Uani 1 1 d . . . C31 C 0.6643(2) 0.63559(18) 0.84008(13) 0.0272(5) Uani 1 1 d . . . C32 C 0.3169(2) 0.62573(17) 1.04195(14) 0.0251(4) Uani 1 1 d . . . C33 C 0.6188(2) 0.81810(15) 1.04976(12) 0.0217(4) Uani 1 1 d . . . C34 C 1.31775(19) 0.46271(14) 0.85000(12) 0.0206(4) Uani 1 1 d . . . C35 C 1.40153(19) 0.50011(16) 0.78139(12) 0.0214(4) Uani 1 1 d . . . C36 C 1.40793(19) 0.54375(17) 0.63832(12) 0.0243(4) Uani 1 1 d . . . C37 C 1.32594(19) 0.60643(15) 0.57009(12) 0.0225(4) Uani 1 1 d . . . C38 C 1.2119(2) 0.49290(15) 0.56340(12) 0.0229(4) Uani 1 1 d . . . C39 C 1.0907(2) 0.46552(15) 0.59104(11) 0.0207(4) Uani 1 1 d . . . C40 C 0.96605(19) 0.42749(15) 0.70997(12) 0.0205(4) Uani 1 1 d . . . C41 C 0.9754(2) 0.39931(15) 0.80016(12) 0.0224(4) Uani 1 1 d . . . C42 C 1.0566(2) 0.44053(15) 0.90110(11) 0.0221(4) Uani 1 1 d . . . C43 C 1.12427(19) 0.51120(15) 0.91084(11) 0.0207(4) Uani 1 1 d . . . C44 C 1.2872(2) 0.70292(17) 0.28857(14) 0.0292(5) Uani 1 1 d . . . S4 S 1.40597(5) 0.77205(4) 0.26663(3) 0.02182(11) Uani 1 1 d . . . O13 O 1.51474(14) 0.70389(12) 0.26028(11) 0.0328(4) Uani 1 1 d . . . O14 O 1.39725(15) 0.80628(11) 0.33543(10) 0.0314(4) Uani 1 1 d . . . O15 O 1.36775(15) 0.84315(12) 0.19230(9) 0.0310(3) Uani 1 1 d . . . F1 F 1.30350(18) 0.63384(12) 0.35837(10) 0.0529(4) Uani 1 1 d . . . F2 F 1.17699(13) 0.75652(12) 0.29197(12) 0.0504(4) Uani 1 1 d . . . F3 F 1.28489(14) 0.66132(11) 0.23192(10) 0.0421(4) Uani 1 1 d . . . C45 C 1.1133(3) 0.9289(2) 1.08607(18) 0.0414(6) Uani 1 1 d . . . Cl1 Cl 1.05755(9) 0.84297(5) 1.05984(5) 0.0568(2) Uani 1 1 d . . . Cl2 Cl 1.00015(6) 0.98653(5) 1.14130(4) 0.04421(16) Uani 1 1 d . . . H1A H 0.870(2) 1.0101(16) 0.7280(15) 0.019(6) Uiso 1 1 d . . . H1B H 0.822(2) 1.0732(17) 0.6438(14) 0.016(5) Uiso 1 1 d . . . H2A H 0.977(2) 0.9852(16) 0.5799(15) 0.019(6) Uiso 1 1 d . . . H2B H 1.038(2) 1.0099(16) 0.6463(14) 0.017(5) Uiso 1 1 d . . . H5A H 1.402(2) 1.0270(17) 0.7231(14) 0.020(6) Uiso 1 1 d . . . H7A H 1.265(2) 0.8507(18) 0.9114(16) 0.024(6) Uiso 1 1 d . . . H9A H 1.381(2) 1.0353(18) 0.5974(14) 0.023(6) Uiso 1 1 d . . . H9B H 1.256(2) 1.0220(18) 0.5754(15) 0.026(6) Uiso 1 1 d . . . H9C H 1.376(2) 0.9466(19) 0.5783(16) 0.031(7) Uiso 1 1 d . . . H10A H 1.451(2) 1.0249(19) 0.8544(16) 0.030(7) Uiso 1 1 d . . . H10B H 1.433(2) 0.9340(19) 0.9261(16) 0.030(7) Uiso 1 1 d . . . H10C H 1.329(3) 1.025(2) 0.9038(17) 0.035(7) Uiso 1 1 d . . . H11A H 1.137(2) 0.7637(19) 0.9060(17) 0.035(7) Uiso 1 1 d . . . H11B H 1.196(3) 0.704(2) 0.8521(17) 0.036(7) Uiso 1 1 d . . . H11C H 1.082(3) 0.770(2) 0.8273(19) 0.045(8) Uiso 1 1 d . . . H12A H 0.788(2) 0.9700(16) 0.5608(14) 0.016(5) Uiso 1 1 d . . . H12B H 0.655(2) 1.0091(18) 0.5946(15) 0.028(6) Uiso 1 1 d . . . H13A H 0.621(2) 0.8538(17) 0.6427(15) 0.022(6) Uiso 1 1 d . . . H13B H 0.675(2) 0.8635(16) 0.5535(15) 0.019(6) Uiso 1 1 d . . . H16A H 0.964(2) 0.8222(18) 0.3377(15) 0.026(6) Uiso 1 1 d . . . H18A H 0.634(3) 0.754(2) 0.3608(17) 0.037(7) Uiso 1 1 d . . . H20A H 1.060(2) 0.8290(18) 0.4429(16) 0.028(6) Uiso 1 1 d . . . H20B H 1.065(2) 0.7334(19) 0.5087(15) 0.025(6) Uiso 1 1 d . . . H20C H 0.991(2) 0.8137(19) 0.5266(16) 0.029(7) Uiso 1 1 d . . . H22A H 0.525(3) 0.720(2) 0.4710(17) 0.036(7) Uiso 1 1 d . . . H22B H 0.558(2) 0.7335(19) 0.5519(17) 0.030(7) Uiso 1 1 d . . . H22C H 0.600(2) 0.642(2) 0.5304(16) 0.030(7) Uiso 1 1 d . . . H23A H 0.639(2) 1.0218(17) 0.7306(14) 0.020(6) Uiso 1 1 d . . . H23B H 0.612(2) 0.9240(17) 0.7337(14) 0.020(6) Uiso 1 1 d . . . H24A H 0.776(2) 0.9458(17) 0.8396(14) 0.019(6) Uiso 1 1 d . . . H24B H 0.653(2) 0.9064(18) 0.8623(16) 0.030(7) Uiso 1 1 d . . . H27A H 0.467(2) 0.6000(18) 0.9196(15) 0.025(6) Uiso 1 1 d . . . H29A H 0.426(2) 0.7444(17) 1.0795(14) 0.021(6) Uiso 1 1 d . . . H31A H 0.608(2) 0.6083(18) 0.8191(16) 0.029(7) Uiso 1 1 d . . . H31B H 0.736(3) 0.587(2) 0.8568(18) 0.042(8) Uiso 1 1 d . . . H31C H 0.683(3) 0.685(2) 0.7985(19) 0.042(8) Uiso 1 1 d . . . H32A H 0.251(3) 0.676(2) 1.0426(19) 0.049(9) Uiso 1 1 d . . . H32B H 0.326(3) 0.586(2) 1.094(2) 0.060(10) Uiso 1 1 d . . . H32C H 0.290(4) 0.595(3) 1.015(2) 0.073(12) Uiso 1 1 d . . . H33A H 0.549(2) 0.8358(18) 1.0825(15) 0.026(6) Uiso 1 1 d . . . H33B H 0.642(2) 0.8737(19) 1.0126(16) 0.030(7) Uiso 1 1 d . . . H33C H 0.681(3) 0.7919(19) 1.0784(16) 0.027(7) Uiso 1 1 d . . . H34A H 1.296(2) 0.4096(17) 0.8451(14) 0.020(6) Uiso 1 1 d . . . H34B H 1.356(2) 0.4511(17) 0.8991(15) 0.023(6) Uiso 1 1 d . . . H35A H 1.427(2) 0.5510(18) 0.7872(15) 0.023(6) Uiso 1 1 d . . . H35B H 1.467(2) 0.4508(18) 0.7779(14) 0.022(6) Uiso 1 1 d . . . H36A H 1.444(2) 0.485(2) 0.6318(16) 0.032(7) Uiso 1 1 d . . . H36B H 1.470(2) 0.5722(18) 0.6401(15) 0.027(6) Uiso 1 1 d . . . H37A H 1.305(2) 0.6704(17) 0.5721(14) 0.019(6) Uiso 1 1 d . . . H37B H 1.365(2) 0.6040(18) 0.5170(16) 0.029(7) Uiso 1 1 d . . . H38A H 1.278(2) 0.4455(19) 0.5930(16) 0.029(7) Uiso 1 1 d . . . H38B H 1.225(2) 0.5015(18) 0.5078(16) 0.027(6) Uiso 1 1 d . . . H39A H 1.025(2) 0.5141(16) 0.5660(13) 0.010(5) Uiso 1 1 d . . . H39B H 1.087(2) 0.4105(17) 0.5827(14) 0.018(6) Uiso 1 1 d . . . H40A H 0.958(2) 0.3719(17) 0.6976(14) 0.019(6) Uiso 1 1 d . . . H40B H 0.897(2) 0.4813(17) 0.6897(14) 0.017(5) Uiso 1 1 d . . . H41A H 0.899(2) 0.3899(18) 0.8264(16) 0.030(7) Uiso 1 1 d . . . H41B H 1.036(2) 0.3394(18) 0.8193(14) 0.022(6) Uiso 1 1 d . . . H42A H 1.107(2) 0.3815(17) 0.9080(14) 0.019(6) Uiso 1 1 d . . . H42B H 0.991(2) 0.4379(17) 0.9345(15) 0.023(6) Uiso 1 1 d . . . H43A H 1.070(2) 0.5688(16) 0.9097(13) 0.015(5) Uiso 1 1 d . . . H43B H 1.165(2) 0.4854(19) 0.9619(17) 0.034(7) Uiso 1 1 d . . . H45A H 1.126(3) 0.980(3) 1.028(2) 0.064(10) Uiso 1 1 d . . . H45B H 1.182(3) 0.898(2) 1.119(2) 0.057(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01501(12) 0.01239(12) 0.00923(11) -0.00175(9) 0.00059(9) -0.00316(9) Ca1 0.01704(17) 0.01341(17) 0.00994(16) -0.00291(13) -0.00046(13) -0.00261(13) S1 0.0157(2) 0.0150(2) 0.01153(19) -0.00368(16) 0.00010(15) -0.00427(16) S2 0.0189(2) 0.0163(2) 0.01029(19) -0.00277(16) -0.00115(16) -0.00441(17) S3 0.0175(2) 0.0187(2) 0.00979(19) -0.00271(16) 0.00100(16) -0.00436(17) O1 0.0179(6) 0.0154(6) 0.0181(6) -0.0059(5) -0.0006(5) -0.0035(5) O2 0.0212(7) 0.0241(7) 0.0120(6) -0.0049(5) 0.0027(5) -0.0088(6) O3 0.0216(7) 0.0171(6) 0.0141(6) -0.0053(5) -0.0039(5) -0.0002(5) O4 0.0273(7) 0.0240(7) 0.0150(6) -0.0027(5) 0.0023(5) -0.0119(6) O5 0.0225(7) 0.0205(7) 0.0127(6) 0.0001(5) 0.0019(5) 0.0009(6) O6 0.0233(7) 0.0342(8) 0.0164(7) -0.0096(6) -0.0003(5) -0.0109(6) O7 0.0212(7) 0.0150(6) 0.0109(6) -0.0023(5) 0.0016(5) -0.0011(5) O8 0.0198(7) 0.0167(6) 0.0124(6) -0.0017(5) -0.0008(5) 0.0007(5) O9 0.0177(6) 0.0230(7) 0.0137(6) -0.0042(5) 0.0009(5) -0.0027(5) O10 0.0227(7) 0.0181(7) 0.0158(6) -0.0054(5) 0.0025(5) -0.0056(5) O11 0.0222(7) 0.0196(7) 0.0120(6) -0.0044(5) 0.0019(5) -0.0075(5) O12 0.0248(7) 0.0180(6) 0.0121(6) -0.0015(5) -0.0008(5) -0.0050(5) N1 0.0163(7) 0.0159(7) 0.0137(7) -0.0019(6) 0.0015(6) -0.0033(6) N2 0.0158(7) 0.0134(7) 0.0148(7) -0.0011(6) 0.0000(6) -0.0036(6) N3 0.0180(8) 0.0167(8) 0.0141(7) -0.0040(6) -0.0038(6) 0.0000(6) N4 0.0210(8) 0.0144(7) 0.0108(7) -0.0018(6) 0.0024(6) -0.0029(6) C1 0.0222(9) 0.0149(9) 0.0200(9) -0.0029(7) 0.0013(7) -0.0053(7) C2 0.0189(9) 0.0150(9) 0.0175(9) 0.0014(7) -0.0001(7) -0.0043(7) C3 0.0145(8) 0.0149(8) 0.0151(8) -0.0045(7) -0.0028(7) -0.0008(7) C4 0.0153(8) 0.0167(9) 0.0172(9) -0.0041(7) -0.0020(7) -0.0006(7) C5 0.0174(9) 0.0161(9) 0.0238(10) -0.0048(7) -0.0033(7) -0.0033(7) C6 0.0187(9) 0.0170(9) 0.0229(9) -0.0076(7) -0.0078(7) 0.0015(7) C7 0.0221(9) 0.0177(9) 0.0147(9) -0.0045(7) -0.0042(7) 0.0007(7) C8 0.0179(9) 0.0148(8) 0.0163(8) -0.0033(7) -0.0018(7) -0.0013(7) C9 0.0233(10) 0.0226(10) 0.0182(9) -0.0031(8) 0.0012(8) -0.0109(8) C10 0.0297(11) 0.0211(10) 0.0250(10) -0.0071(8) -0.0111(9) -0.0035(9) C11 0.0323(11) 0.0241(10) 0.0128(9) -0.0029(8) -0.0014(8) -0.0116(9) C12 0.0210(9) 0.0192(9) 0.0158(9) -0.0016(7) -0.0029(7) -0.0010(8) C13 0.0170(9) 0.0219(10) 0.0170(9) -0.0043(7) -0.0032(7) -0.0003(7) C14 0.0196(9) 0.0165(8) 0.0104(8) -0.0025(7) -0.0008(7) -0.0048(7) C15 0.0198(9) 0.0129(8) 0.0173(9) -0.0029(7) 0.0004(7) -0.0019(7) C16 0.0266(10) 0.0159(9) 0.0177(9) -0.0017(7) 0.0059(8) -0.0012(8) C17 0.0365(12) 0.0179(9) 0.0123(8) -0.0033(7) -0.0030(8) 0.0034(8) C18 0.0288(11) 0.0245(10) 0.0199(9) -0.0070(8) -0.0095(8) -0.0026(8) C19 0.0211(9) 0.0213(9) 0.0170(9) -0.0046(7) -0.0031(7) -0.0055(8) C20 0.0198(10) 0.0197(10) 0.0275(11) -0.0030(8) 0.0002(8) -0.0068(8) C21 0.0580(16) 0.0310(12) 0.0144(10) -0.0063(9) -0.0048(10) 0.0133(11) C22 0.0238(11) 0.0363(13) 0.0291(11) -0.0046(10) -0.0051(9) -0.0123(10) C23 0.0205(9) 0.0172(9) 0.0200(9) -0.0042(7) 0.0050(7) -0.0012(8) C24 0.0264(10) 0.0153(9) 0.0177(9) -0.0053(7) 0.0066(8) -0.0022(8) C25 0.0177(9) 0.0159(8) 0.0108(8) -0.0010(7) 0.0008(7) -0.0041(7) C26 0.0253(10) 0.0179(9) 0.0129(8) -0.0042(7) 0.0019(7) -0.0064(8) C27 0.0243(10) 0.0213(9) 0.0167(9) -0.0057(7) -0.0009(7) -0.0089(8) C28 0.0177(9) 0.0185(9) 0.0157(8) 0.0000(7) -0.0013(7) -0.0030(7) C29 0.0196(9) 0.0187(9) 0.0124(8) -0.0026(7) 0.0008(7) -0.0004(7) C30 0.0206(9) 0.0154(8) 0.0103(8) -0.0016(6) -0.0015(7) -0.0022(7) C31 0.0371(12) 0.0329(12) 0.0209(10) -0.0161(9) 0.0091(9) -0.0190(10) C32 0.0213(10) 0.0316(12) 0.0222(10) -0.0056(9) 0.0018(8) -0.0097(9) C33 0.0271(11) 0.0245(10) 0.0169(9) -0.0102(8) 0.0044(8) -0.0088(9) C34 0.0217(10) 0.0189(9) 0.0179(9) -0.0035(7) -0.0041(7) 0.0015(8) C35 0.0191(9) 0.0255(10) 0.0190(9) -0.0064(8) -0.0037(7) -0.0021(8) C36 0.0199(10) 0.0325(12) 0.0181(9) -0.0052(8) 0.0051(8) -0.0063(9) C37 0.0242(10) 0.0257(10) 0.0162(9) -0.0036(8) 0.0042(8) -0.0085(8) C38 0.0311(11) 0.0228(10) 0.0168(9) -0.0094(8) 0.0051(8) -0.0070(9) C39 0.0306(11) 0.0196(10) 0.0143(9) -0.0077(7) -0.0005(8) -0.0057(8) C40 0.0242(10) 0.0202(10) 0.0194(9) -0.0058(8) 0.0009(8) -0.0099(8) C41 0.0273(10) 0.0214(10) 0.0184(9) -0.0034(8) 0.0044(8) -0.0108(8) C42 0.0256(10) 0.0258(11) 0.0101(8) 0.0004(7) 0.0009(7) -0.0042(8) C43 0.0231(10) 0.0245(10) 0.0108(8) -0.0028(7) 0.0004(7) -0.0007(8) C44 0.0271(11) 0.0323(12) 0.0309(11) -0.0133(9) 0.0057(9) -0.0089(9) S4 0.0195(2) 0.0229(2) 0.0245(2) -0.0101(2) -0.00255(19) -0.00193(19) O13 0.0221(8) 0.0326(9) 0.0476(10) -0.0213(8) -0.0032(7) 0.0009(7) O14 0.0370(9) 0.0293(8) 0.0303(8) -0.0153(7) -0.0106(7) 0.0016(7) O15 0.0354(9) 0.0308(8) 0.0241(8) -0.0052(7) 0.0004(7) -0.0056(7) F1 0.0742(12) 0.0433(9) 0.0380(9) 0.0000(7) 0.0070(8) -0.0269(9) F2 0.0217(7) 0.0556(10) 0.0817(13) -0.0347(9) 0.0131(7) -0.0093(7) F3 0.0388(8) 0.0521(9) 0.0515(9) -0.0320(8) 0.0030(7) -0.0201(7) C45 0.0327(13) 0.0485(16) 0.0393(14) -0.0130(12) -0.0041(11) 0.0004(12) Cl1 0.0843(6) 0.0445(4) 0.0435(4) -0.0200(3) 0.0160(4) -0.0144(4) Cl2 0.0388(3) 0.0474(4) 0.0513(4) -0.0240(3) -0.0027(3) -0.0047(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 O7 1.8542(13) . ? Co1 N3 1.9498(16) . ? Co1 N4 1.9624(15) . ? Co1 N2 1.9708(16) . ? Co1 N1 1.9971(16) . ? Ca1 O7 2.2661(13) . ? Ca1 O1 2.3607(14) . ? Ca1 O3 2.3794(13) . ? Ca1 O9 2.4909(14) . ? Ca1 O11 2.5092(14) . ? Ca1 O12 2.5140(14) . ? Ca1 O8 2.5173(13) . ? Ca1 O10 2.5365(14) . ? S1 O2 1.4446(13) . ? S1 O1 1.4537(14) . ? S1 N2 1.6014(16) . ? S1 C3 1.7942(18) . ? S2 O4 1.4414(14) . ? S2 O3 1.4546(14) . ? S2 N3 1.5951(16) . ? S2 C14 1.7911(18) . ? S3 O6 1.4389(14) . ? S3 O5 1.4484(14) . ? S3 N4 1.6033(15) . ? S3 C25 1.7948(19) . ? O8 C34 1.430(2) . ? O8 C43 1.436(2) . ? O9 C35 1.428(2) . ? O9 C36 1.432(2) . ? O10 C37 1.434(2) . ? O10 C38 1.435(2) . ? O11 C40 1.434(2) . ? O11 C39 1.434(2) . ? O12 C41 1.429(2) . ? O12 C42 1.438(2) . ? N1 C1 1.493(2) . ? N1 C12 1.494(2) . ? N1 C23 1.499(2) . ? N2 C2 1.481(2) . ? N3 C13 1.476(2) . ? N4 C24 1.484(2) . ? C1 C2 1.516(3) . ? C3 C4 1.416(3) . ? C3 C8 1.418(3) . ? C4 C5 1.402(3) . ? C4 C9 1.510(3) . ? C5 C6 1.386(3) . ? C6 C7 1.390(3) . ? C6 C10 1.503(3) . ? C7 C8 1.386(3) . ? C8 C11 1.507(3) . ? C12 C13 1.517(3) . ? C14 C15 1.413(3) . ? C14 C19 1.414(3) . ? C15 C16 1.399(3) . ? C15 C20 1.507(3) . ? C16 C17 1.392(3) . ? C17 C18 1.376(3) . ? C17 C21 1.510(3) . ? C18 C19 1.398(3) . ? C19 C22 1.507(3) . ? C23 C24 1.494(3) . ? C25 C26 1.415(3) . ? C25 C30 1.418(2) . ? C26 C27 1.390(3) . ? C26 C31 1.513(3) . ? C27 C28 1.390(3) . ? C28 C29 1.387(3) . ? C28 C32 1.509(3) . ? C29 C30 1.394(3) . ? C30 C33 1.511(3) . ? C34 C35 1.498(3) . ? C36 C37 1.520(3) . ? C38 C39 1.503(3) . ? C40 C41 1.512(3) . ? C42 C43 1.506(3) . ? C44 F2 1.334(3) . ? C44 F1 1.340(3) . ? C44 F3 1.340(3) . ? C44 S4 1.817(2) . ? S4 O13 1.4407(16) . ? S4 O15 1.4428(16) . ? S4 O14 1.4442(16) . ? C45 Cl1 1.764(3) . ? C45 Cl2 1.769(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 O7 Co1 N3 96.14(6) . . ? O7 Co1 N4 94.30(6) . . ? N3 Co1 N4 124.36(7) . . ? O7 Co1 N2 98.42(6) . . ? N3 Co1 N2 109.01(7) . . ? N4 Co1 N2 123.14(7) . . ? O7 Co1 N1 177.38(6) . . ? N3 Co1 N1 83.41(7) . . ? N4 Co1 N1 83.85(6) . . ? N2 Co1 N1 84.15(6) . . ? O7 Ca1 O1 74.73(5) . . ? O7 Ca1 O3 72.38(5) . . ? O1 Ca1 O3 101.67(5) . . ? O7 Ca1 O9 143.47(5) . . ? O1 Ca1 O9 79.24(5) . . ? O3 Ca1 O9 138.85(5) . . ? O7 Ca1 O11 124.98(5) . . ? O1 Ca1 O11 154.75(5) . . ? O3 Ca1 O11 73.78(5) . . ? O9 Ca1 O11 88.16(5) . . ? O7 Ca1 O12 79.80(5) . . ? O1 Ca1 O12 141.09(5) . . ? O3 Ca1 O12 97.97(5) . . ? O9 Ca1 O12 106.63(5) . . ? O11 Ca1 O12 63.54(4) . . ? O7 Ca1 O8 89.15(5) . . ? O1 Ca1 O8 85.68(5) . . ? O3 Ca1 O8 157.17(5) . . ? O9 Ca1 O8 63.51(4) . . ? O11 Ca1 O8 108.25(4) . . ? O12 Ca1 O8 64.82(4) . . ? O7 Ca1 O10 140.40(5) . . ? O1 Ca1 O10 89.10(5) . . ? O3 Ca1 O10 76.07(5) . . ? O9 Ca1 O10 62.78(4) . . ? O11 Ca1 O10 65.65(4) . . ? O12 Ca1 O10 128.37(5) . . ? O8 Ca1 O10 126.07(5) . . ? O2 S1 O1 114.70(8) . . ? O2 S1 N2 110.74(8) . . ? O1 S1 N2 109.70(8) . . ? O2 S1 C3 108.19(8) . . ? O1 S1 C3 107.35(8) . . ? N2 S1 C3 105.71(8) . . ? O4 S2 O3 114.43(9) . . ? O4 S2 N3 113.66(9) . . ? O3 S2 N3 108.38(8) . . ? O4 S2 C14 108.22(8) . . ? O3 S2 C14 105.70(8) . . ? N3 S2 C14 105.80(8) . . ? O6 S3 O5 115.36(9) . . ? O6 S3 N4 111.53(9) . . ? O5 S3 N4 109.04(8) . . ? O6 S3 C25 108.05(9) . . ? O5 S3 C25 105.28(9) . . ? N4 S3 C25 107.08(8) . . ? S1 O1 Ca1 145.78(8) . . ? S2 O3 Ca1 146.64(8) . . ? Co1 O7 Ca1 134.56(7) . . ? C34 O8 C43 113.56(14) . . ? C34 O8 Ca1 114.35(11) . . ? C43 O8 Ca1 111.19(11) . . ? C35 O9 C36 112.96(15) . . ? C35 O9 Ca1 121.44(11) . . ? C36 O9 Ca1 123.51(11) . . ? C37 O10 C38 113.87(16) . . ? C37 O10 Ca1 109.59(11) . . ? C38 O10 Ca1 115.29(11) . . ? C40 O11 C39 112.35(15) . . ? C40 O11 Ca1 109.62(11) . . ? C39 O11 Ca1 112.97(11) . . ? C41 O12 C42 111.58(15) . . ? C41 O12 Ca1 120.03(11) . . ? C42 O12 Ca1 120.93(12) . . ? C1 N1 C12 111.16(15) . . ? C1 N1 C23 109.94(15) . . ? C12 N1 C23 109.04(15) . . ? C1 N1 Co1 107.97(11) . . ? C12 N1 Co1 110.00(12) . . ? C23 N1 Co1 108.69(11) . . ? C2 N2 S1 111.18(12) . . ? C2 N2 Co1 113.57(12) . . ? S1 N2 Co1 134.15(9) . . ? C13 N3 S2 115.98(13) . . ? C13 N3 Co1 112.59(12) . . ? S2 N3 Co1 129.25(9) . . ? C24 N4 S3 110.64(12) . . ? C24 N4 Co1 113.26(11) . . ? S3 N4 Co1 134.98(10) . . ? N1 C1 C2 108.64(16) . . ? N2 C2 C1 106.96(15) . . ? C4 C3 C8 120.40(17) . . ? C4 C3 S1 121.60(14) . . ? C8 C3 S1 117.89(14) . . ? C5 C4 C3 117.70(17) . . ? C5 C4 C9 116.16(17) . . ? C3 C4 C9 126.14(17) . . ? C6 C5 C4 123.00(18) . . ? C5 C6 C7 117.58(18) . . ? C5 C6 C10 121.90(19) . . ? C7 C6 C10 120.45(18) . . ? C8 C7 C6 122.88(18) . . ? C7 C8 C3 118.40(18) . . ? C7 C8 C11 117.21(17) . . ? C3 C8 C11 124.39(17) . . ? N1 C12 C13 107.47(15) . . ? N3 C13 C12 104.43(16) . . ? C15 C14 C19 120.77(17) . . ? C15 C14 S2 118.03(14) . . ? C19 C14 S2 121.19(14) . . ? C16 C15 C14 118.03(18) . . ? C16 C15 C20 117.46(18) . . ? C14 C15 C20 124.51(17) . . ? C17 C16 C15 122.17(19) . . ? C18 C17 C16 118.14(18) . . ? C18 C17 C21 120.5(2) . . ? C16 C17 C21 121.4(2) . . ? C17 C18 C19 123.01(19) . . ? C18 C19 C14 117.60(18) . . ? C18 C19 C22 116.51(18) . . ? C14 C19 C22 125.89(18) . . ? C24 C23 N1 108.60(16) . . ? N4 C24 C23 106.19(15) . . ? C26 C25 C30 120.49(17) . . ? C26 C25 S3 117.52(14) . . ? C30 C25 S3 121.81(14) . . ? C27 C26 C25 118.32(17) . . ? C27 C26 C31 117.48(18) . . ? C25 C26 C31 124.20(18) . . ? C28 C27 C26 122.41(18) . . ? C29 C28 C27 118.05(18) . . ? C29 C28 C32 120.84(18) . . ? C27 C28 C32 121.10(19) . . ? C28 C29 C30 122.69(17) . . ? C29 C30 C25 117.83(17) . . ? C29 C30 C33 116.56(17) . . ? C25 C30 C33 125.61(17) . . ? O8 C34 C35 107.06(16) . . ? O9 C35 C34 106.68(16) . . ? O9 C36 C37 106.75(16) . . ? O10 C37 C36 110.93(16) . . ? O10 C38 C39 107.46(16) . . ? O11 C39 C38 106.57(16) . . ? O11 C40 C41 106.83(16) . . ? O12 C41 C40 108.25(16) . . ? O12 C42 C43 108.00(16) . . ? O8 C43 C42 111.22(16) . . ? F2 C44 F1 107.92(19) . . ? F2 C44 F3 107.00(19) . . ? F1 C44 F3 106.47(19) . . ? F2 C44 S4 111.45(16) . . ? F1 C44 S4 112.22(17) . . ? F3 C44 S4 111.49(15) . . ? O13 S4 O15 115.17(10) . . ? O13 S4 O14 115.59(10) . . ? O15 S4 O14 114.97(10) . . ? O13 S4 C44 102.91(10) . . ? O15 S4 C44 102.68(11) . . ? O14 S4 C44 102.77(10) . . ? Cl1 C45 Cl2 110.24(16) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.747 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.073