data_asb228 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H69 Ca Co F3 N4 O16 S4' _chemical_formula_weight 1194.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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 9.4438(4) _cell_length_b 17.4810(7) _cell_length_c 17.5309(7) _cell_angle_alpha 73.4591(4) _cell_angle_beta 88.5336(4) _cell_angle_gamma 85.2907(5) _cell_volume 2765.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9896 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.71 _exptl_crystal_description rod _exptl_crystal_colour pink _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1254 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7569 _exptl_absorpt_correction_T_max 0.9281 _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 33604 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.86 _reflns_number_total 13265 _reflns_number_gt 11313 _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^)+(0.0800P)^2^+2.4148P] 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 13265 _refine_ls_number_parameters 683 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.49313(3) 1.296641(17) -0.293110(17) 0.01603(8) Uani 1 1 d . . . Ca1 Ca -0.60418(4) 1.31500(3) -0.05832(2) 0.01579(10) Uani 1 1 d . . . S1 S -0.38581(5) 1.43104(3) -0.21370(3) 0.01712(12) Uani 1 1 d . . . S2 S -0.44125(6) 1.09884(3) -0.23142(3) 0.02044(12) Uani 1 1 d . . . S3 S -0.81923(6) 1.34522(3) -0.35718(3) 0.01903(12) Uani 1 1 d . . . O1 O -0.51871(16) 1.41497(9) -0.17025(9) 0.0180(3) Uani 1 1 d . . . O2 O -0.26384(17) 1.42065(10) -0.16139(10) 0.0231(3) Uani 1 1 d . . . O3 O -0.52129(18) 1.11185(10) -0.16324(10) 0.0235(3) Uani 1 1 d . . . O4 O -0.49964(19) 1.04322(11) -0.26672(11) 0.0280(4) Uani 1 1 d . . . O5 O -0.84355(17) 1.30878(11) -0.27261(10) 0.0253(4) Uani 1 1 d . . . O6 O -0.89286(19) 1.42299(11) -0.38923(11) 0.0265(4) Uani 1 1 d . . . O7 O -0.61219(17) 1.26342(10) -0.17905(9) 0.0191(3) Uani 1 1 d D . . H1 H -0.595(3) 1.2132(3) -0.1710(18) 0.026(8) Uiso 1 1 d D . . H2 H -0.6960(12) 1.2706(18) -0.1977(17) 0.027(8) Uiso 1 1 d D . . N1 N -0.3736(2) 1.32437(11) -0.40061(11) 0.0199(4) Uani 1 1 d . . . N2 N -0.36811(19) 1.37819(12) -0.27249(11) 0.0184(4) Uani 1 1 d . . . N3 N -0.4227(2) 1.18356(12) -0.29261(12) 0.0227(4) Uani 1 1 d . . . N4 N -0.65295(19) 1.34487(11) -0.36996(11) 0.0182(4) Uani 1 1 d . . . C1 C -0.2323(3) 1.34021(16) -0.37869(15) 0.0264(5) Uani 1 1 d . . . H1A H -0.1784 1.3647 -0.4275 0.032 Uiso 1 1 calc R . . H1B H -0.1798 1.2890 -0.3503 0.032 Uiso 1 1 calc R . . C2 C -0.2428(2) 1.39596(15) -0.32582(14) 0.0238(5) Uani 1 1 d . . . H2A H -0.1553 1.3881 -0.2937 0.029 Uiso 1 1 calc R . . H2B H -0.2530 1.4523 -0.3590 0.029 Uiso 1 1 calc R . . C3 C -0.3988(2) 1.53469(14) -0.27034(13) 0.0202(4) Uani 1 1 d . . . C4 C -0.2807(3) 1.58143(15) -0.27922(13) 0.0232(5) Uani 1 1 d . . . C5 C -0.3002(3) 1.66205(15) -0.32239(14) 0.0278(5) Uani 1 1 d . . . H5A H -0.2215 1.6939 -0.3285 0.033 Uiso 1 1 calc R . . C6 C -0.4277(3) 1.69776(15) -0.35656(14) 0.0301(6) Uani 1 1 d . . . C7 C -0.5410(3) 1.64979(15) -0.34882(14) 0.0261(5) Uani 1 1 d . . . H7A H -0.6294 1.6734 -0.3724 0.031 Uiso 1 1 calc R . . C8 C -0.5300(3) 1.56836(14) -0.30775(13) 0.0211(4) Uani 1 1 d . . . C9 C -0.1338(3) 1.55267(16) -0.24481(15) 0.0280(5) Uani 1 1 d . . . H9A H -0.0674 1.5933 -0.2683 0.042 Uiso 1 1 calc R . . H9B H -0.1019 1.5026 -0.2569 0.042 Uiso 1 1 calc R . . H9C H -0.1370 1.5435 -0.1870 0.042 Uiso 1 1 calc R . . C10 C -0.4422(4) 1.78584(17) -0.39996(19) 0.0429(7) Uani 1 1 d . . . H10A H -0.4125 1.8164 -0.3650 0.064 Uiso 1 1 calc R . . H10B H -0.5416 1.8022 -0.4155 0.064 Uiso 1 1 calc R . . H10C H -0.3821 1.7962 -0.4477 0.064 Uiso 1 1 calc R . . C11 C -0.6577(3) 1.52228(15) -0.30809(14) 0.0235(5) Uani 1 1 d . . . H11A H -0.6285 1.4736 -0.3235 0.035 Uiso 1 1 calc R . . H11B H -0.7277 1.5556 -0.3462 0.035 Uiso 1 1 calc R . . H11C H -0.7000 1.5077 -0.2548 0.035 Uiso 1 1 calc R . . C12 C -0.3718(3) 1.25432(15) -0.43096(15) 0.0261(5) Uani 1 1 d . . . H12A H -0.2981 1.2581 -0.4728 0.031 Uiso 1 1 calc R . . H12B H -0.4649 1.2531 -0.4551 0.031 Uiso 1 1 calc R . . C13 C -0.3408(3) 1.17757(15) -0.36390(15) 0.0282(5) Uani 1 1 d . . . H13A H -0.3681 1.1311 -0.3803 0.034 Uiso 1 1 calc R . . H13B H -0.2380 1.1697 -0.3517 0.034 Uiso 1 1 calc R . . C14 C -0.2659(2) 1.05662(14) -0.19793(14) 0.0214(4) Uani 1 1 d . . . C15 C -0.1915(3) 0.99926(14) -0.23043(15) 0.0240(5) Uani 1 1 d . . . C16 C -0.0526(3) 0.97138(15) -0.20320(16) 0.0280(5) Uani 1 1 d . . . H16A H -0.0009 0.9339 -0.2254 0.034 Uiso 1 1 calc R . . C17 C 0.0114(3) 0.99631(15) -0.14564(17) 0.0291(5) Uani 1 1 d . . . C18 C -0.0641(3) 1.05259(15) -0.11529(17) 0.0282(5) Uani 1 1 d . . . H18A H -0.0213 1.0696 -0.0751 0.034 Uiso 1 1 calc R . . C19 C -0.2001(3) 1.08533(14) -0.14118(15) 0.0246(5) Uani 1 1 d . . . C20 C -0.2471(3) 0.96469(16) -0.29290(16) 0.0315(6) Uani 1 1 d . . . H20A H -0.1772 0.9234 -0.3018 0.047 Uiso 1 1 calc R . . H20B H -0.2632 1.0074 -0.3427 0.047 Uiso 1 1 calc R . . H20C H -0.3367 0.9409 -0.2745 0.047 Uiso 1 1 calc R . . C21 C 0.1609(3) 0.96456(17) -0.1179(2) 0.0366(6) Uani 1 1 d . . . H21A H 0.1794 0.9768 -0.0680 0.055 Uiso 1 1 calc R . . H21B H 0.2290 0.9899 -0.1585 0.055 Uiso 1 1 calc R . . H21C H 0.1712 0.9065 -0.1092 0.055 Uiso 1 1 calc R . . C22 C -0.2659(3) 1.15072(16) -0.10751(17) 0.0304(5) Uani 1 1 d . . . H22A H -0.1974 1.1632 -0.0726 0.046 Uiso 1 1 calc R . . H22B H -0.3513 1.1326 -0.0770 0.046 Uiso 1 1 calc R . . H22C H -0.2916 1.1988 -0.1512 0.046 Uiso 1 1 calc R . . C23 C -0.4520(2) 1.39555(14) -0.45284(14) 0.0228(5) Uani 1 1 d . . . H23A H -0.4146 1.4056 -0.5078 0.027 Uiso 1 1 calc R . . H23B H -0.4377 1.4429 -0.4344 0.027 Uiso 1 1 calc R . . C24 C -0.6096(2) 1.38387(14) -0.45251(13) 0.0219(5) Uani 1 1 d . . . H24A H -0.6645 1.4363 -0.4729 0.026 Uiso 1 1 calc R . . H24B H -0.6284 1.3500 -0.4872 0.026 Uiso 1 1 calc R . . C25 C -0.8850(2) 1.28124(14) -0.41069(14) 0.0201(4) Uani 1 1 d . . . C26 C -0.8826(3) 1.19801(15) -0.37293(15) 0.0261(5) Uani 1 1 d . . . C27 C -0.9407(3) 1.14982(16) -0.41232(17) 0.0319(6) Uani 1 1 d . . . H27A H -0.9423 1.0942 -0.3863 0.038 Uiso 1 1 calc R . . C28 C -0.9970(3) 1.18001(18) -0.48899(18) 0.0341(6) Uani 1 1 d . . . C29 C -0.9921(3) 1.26116(17) -0.52594(15) 0.0284(5) Uani 1 1 d . . . H29A H -1.0269 1.2820 -0.5788 0.034 Uiso 1 1 calc R . . C30 C -0.9383(2) 1.31362(15) -0.48894(14) 0.0216(5) Uani 1 1 d . . . C31 C -0.8207(3) 1.15645(16) -0.29170(17) 0.0329(6) Uani 1 1 d . . . H31A H -0.8101 1.0985 -0.2842 0.049 Uiso 1 1 calc R . . H31B H -0.8842 1.1681 -0.2507 0.049 Uiso 1 1 calc R . . H31C H -0.7275 1.1758 -0.2875 0.049 Uiso 1 1 calc R . . C32 C -1.0620(4) 1.1255(2) -0.5291(2) 0.0528(9) Uani 1 1 d . . . H32A H -1.0921 1.0782 -0.4887 0.079 Uiso 1 1 calc R . . H32B H -0.9917 1.1087 -0.5644 0.079 Uiso 1 1 calc R . . H32C H -1.1446 1.1542 -0.5604 0.079 Uiso 1 1 calc R . . C33 C -0.9486(3) 1.40087(15) -0.53612(14) 0.0255(5) Uani 1 1 d . . . H33A H -0.9842 1.4064 -0.5896 0.038 Uiso 1 1 calc R . . H33B H -0.8544 1.4214 -0.5401 0.038 Uiso 1 1 calc R . . H33C H -1.0140 1.4314 -0.5093 0.038 Uiso 1 1 calc R . . O8 O -0.59910(19) 1.16559(10) 0.01011(10) 0.0268(4) Uani 1 1 d . . . O9 O -0.56178(19) 1.27334(11) 0.08971(10) 0.0250(4) Uani 1 1 d . . . O10 O -0.61948(18) 1.42615(10) 0.00500(10) 0.0227(3) Uani 1 1 d . . . O11 O -0.81042(17) 1.41401(10) -0.10477(10) 0.0223(3) Uani 1 1 d . . . O12 O -0.83511(17) 1.25808(10) -0.04390(10) 0.0232(3) Uani 1 1 d . . . C34 C -0.5095(3) 1.14310(16) 0.07970(16) 0.0327(6) Uani 1 1 d . . . H34A H -0.4096 1.1520 0.0635 0.039 Uiso 1 1 calc R . . H34B H -0.5149 1.0855 0.1072 0.039 Uiso 1 1 calc R . . C35 C -0.5559(3) 1.19168(17) 0.13544(15) 0.0335(6) Uani 1 1 d . . . H35A H -0.6505 1.1775 0.1582 0.040 Uiso 1 1 calc R . . H35B H -0.4872 1.1816 0.1796 0.040 Uiso 1 1 calc R . . C36 C -0.6017(3) 1.32879(17) 0.13424(14) 0.0284(5) Uani 1 1 d . . . H36A H -0.5514 1.3131 0.1859 0.034 Uiso 1 1 calc R . . H36B H -0.7054 1.3308 0.1444 0.034 Uiso 1 1 calc R . . C37 C -0.5597(3) 1.40863(17) 0.08362(15) 0.0284(5) Uani 1 1 d . . . H37A H -0.5941 1.4509 0.1085 0.034 Uiso 1 1 calc R . . H37B H -0.4548 1.4078 0.0798 0.034 Uiso 1 1 calc R . . C38 C -0.7497(3) 1.47708(15) -0.00548(15) 0.0258(5) Uani 1 1 d . . . H38A H -0.7342 1.5288 0.0043 0.031 Uiso 1 1 calc R . . H38B H -0.8239 1.4511 0.0315 0.031 Uiso 1 1 calc R . . C39 C -0.7929(3) 1.48966(15) -0.09042(15) 0.0262(5) Uani 1 1 d . . . H39A H -0.8833 1.5238 -0.1014 0.031 Uiso 1 1 calc R . . H39B H -0.7193 1.5175 -0.1267 0.031 Uiso 1 1 calc R . . C40 C -0.9502(2) 1.38780(16) -0.08170(16) 0.0280(5) Uani 1 1 d . . . H40A H -1.0230 1.4240 -0.1167 0.034 Uiso 1 1 calc R . . H40B H -0.9708 1.3881 -0.0261 0.034 Uiso 1 1 calc R . . C41 C -0.9524(2) 1.30489(17) -0.08915(15) 0.0267(5) Uani 1 1 d . . . H41A H -1.0429 1.2822 -0.0682 0.032 Uiso 1 1 calc R . . H41B H -0.9428 1.3054 -0.1456 0.032 Uiso 1 1 calc R . . C42 C -0.8376(3) 1.17513(16) -0.03641(17) 0.0313(6) Uani 1 1 d . . . H42A H -0.8106 1.1643 -0.0875 0.038 Uiso 1 1 calc R . . H42B H -0.9342 1.1577 -0.0217 0.038 Uiso 1 1 calc R . . C43 C -0.7344(3) 1.13114(17) 0.02675(18) 0.0355(6) Uani 1 1 d . . . H43A H -0.7702 1.1349 0.0793 0.043 Uiso 1 1 calc R . . H43B H -0.7231 1.0739 0.0283 0.043 Uiso 1 1 calc R . . O13 O -0.35613(17) 1.30089(11) -0.03513(10) 0.0226(3) Uani 1 1 d D . . H13C H -0.320(3) 1.300(2) 0.0092(9) 0.033(8) Uiso 1 1 d D . . H13D H -0.311(3) 1.3366(14) -0.0672(15) 0.033(8) Uiso 1 1 d D . . S4 S -0.07472(7) 1.28332(4) 0.12791(4) 0.02729(14) Uani 1 1 d . . . O14 O 0.0248(2) 1.34151(13) 0.12043(13) 0.0430(5) Uani 1 1 d . . . O15 O -0.2130(3) 1.32229(16) 0.09247(16) 0.0537(6) Uani 1 1 d . . . O16 O -0.0354(3) 1.21182(14) 0.10918(15) 0.0515(6) Uani 1 1 d . . . C44 C -0.1246(4) 1.2561(2) 0.2313(2) 0.0487(8) Uani 1 1 d . . . F1 F -0.2214(3) 1.20437(16) 0.24910(13) 0.0700(7) Uani 1 1 d . . . F2 F -0.0058(3) 1.21737(16) 0.27548(13) 0.0733(7) Uani 1 1 d . . . F3 F -0.1549(2) 1.31568(15) 0.26071(13) 0.0606(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 0.01476(15) 0.01743(15) 0.01372(15) -0.00147(11) 0.00146(10) 0.00027(11) Ca1 0.0140(2) 0.0189(2) 0.0132(2) -0.00229(16) 0.00098(15) -0.00254(15) S1 0.0141(2) 0.0218(3) 0.0139(2) -0.00204(19) 0.00130(18) -0.00360(19) S2 0.0211(3) 0.0185(3) 0.0190(3) -0.0010(2) -0.0005(2) -0.0013(2) S3 0.0159(2) 0.0243(3) 0.0154(2) -0.0040(2) 0.00071(19) 0.0009(2) O1 0.0156(7) 0.0219(8) 0.0142(7) -0.0017(6) 0.0033(6) -0.0022(6) O2 0.0183(8) 0.0303(9) 0.0183(8) -0.0014(7) -0.0015(6) -0.0073(7) O3 0.0235(8) 0.0237(8) 0.0201(8) -0.0009(6) 0.0023(6) -0.0022(6) O4 0.0276(9) 0.0276(9) 0.0291(9) -0.0077(7) -0.0029(7) -0.0044(7) O5 0.0165(8) 0.0398(10) 0.0174(8) -0.0052(7) 0.0023(6) 0.0000(7) O6 0.0251(9) 0.0281(9) 0.0258(9) -0.0088(7) -0.0032(7) 0.0063(7) O7 0.0183(8) 0.0215(8) 0.0158(7) -0.0029(6) 0.0014(6) -0.0017(6) N1 0.0201(9) 0.0194(9) 0.0178(9) -0.0028(7) 0.0032(7) 0.0015(7) N2 0.0129(8) 0.0242(9) 0.0179(9) -0.0054(7) 0.0046(7) -0.0034(7) N3 0.0251(10) 0.0199(9) 0.0184(9) 0.0004(7) 0.0039(8) 0.0034(8) N4 0.0150(8) 0.0215(9) 0.0150(9) -0.0004(7) 0.0011(7) -0.0015(7) C1 0.0194(11) 0.0335(13) 0.0245(12) -0.0065(10) 0.0054(9) 0.0004(9) C2 0.0147(10) 0.0321(12) 0.0241(12) -0.0071(10) 0.0074(9) -0.0039(9) C3 0.0245(11) 0.0213(11) 0.0141(10) -0.0032(8) 0.0048(8) -0.0058(9) C4 0.0288(12) 0.0272(12) 0.0144(10) -0.0057(9) 0.0044(9) -0.0088(9) C5 0.0396(14) 0.0265(12) 0.0184(11) -0.0058(9) 0.0077(10) -0.0135(11) C6 0.0528(17) 0.0226(12) 0.0149(11) -0.0045(9) 0.0051(10) -0.0062(11) C7 0.0357(13) 0.0251(12) 0.0160(11) -0.0047(9) -0.0001(9) 0.0022(10) C8 0.0250(11) 0.0230(11) 0.0148(10) -0.0052(8) 0.0033(8) -0.0014(9) C9 0.0253(12) 0.0352(13) 0.0240(12) -0.0064(10) 0.0038(9) -0.0146(10) C10 0.070(2) 0.0240(13) 0.0322(15) -0.0020(11) -0.0030(14) -0.0081(13) C11 0.0221(11) 0.0263(12) 0.0193(11) -0.0028(9) -0.0012(9) 0.0018(9) C12 0.0311(13) 0.0247(12) 0.0205(11) -0.0053(9) 0.0061(9) 0.0028(10) C13 0.0352(14) 0.0222(11) 0.0229(12) -0.0024(9) 0.0093(10) 0.0039(10) C14 0.0204(11) 0.0174(10) 0.0227(11) 0.0002(8) -0.0020(8) -0.0004(8) C15 0.0265(12) 0.0177(10) 0.0240(12) -0.0002(9) -0.0002(9) -0.0005(9) C16 0.0284(13) 0.0188(11) 0.0316(13) -0.0002(10) 0.0018(10) 0.0023(9) C17 0.0238(12) 0.0187(11) 0.0384(14) 0.0028(10) -0.0024(10) -0.0022(9) C18 0.0266(12) 0.0217(11) 0.0343(14) -0.0033(10) -0.0055(10) -0.0045(9) C19 0.0244(12) 0.0197(11) 0.0280(12) -0.0034(9) -0.0012(9) -0.0030(9) C20 0.0401(15) 0.0242(12) 0.0293(13) -0.0084(10) -0.0042(11) 0.0062(11) C21 0.0242(13) 0.0302(14) 0.0501(17) -0.0036(12) -0.0079(12) 0.0020(10) C22 0.0304(13) 0.0269(12) 0.0360(14) -0.0131(11) -0.0071(11) 0.0024(10) C23 0.0217(11) 0.0232(11) 0.0196(11) -0.0006(9) 0.0035(8) 0.0005(9) C24 0.0223(11) 0.0234(11) 0.0152(10) 0.0023(8) 0.0008(8) -0.0015(9) C25 0.0150(10) 0.0240(11) 0.0196(11) -0.0038(9) 0.0008(8) 0.0002(8) C26 0.0186(11) 0.0285(12) 0.0273(12) -0.0016(10) 0.0000(9) -0.0028(9) C27 0.0301(13) 0.0267(13) 0.0364(14) -0.0040(11) -0.0034(11) -0.0037(10) C28 0.0321(14) 0.0349(14) 0.0381(15) -0.0148(12) -0.0051(11) -0.0011(11) C29 0.0258(12) 0.0374(14) 0.0223(12) -0.0093(10) -0.0014(9) -0.0013(10) C30 0.0168(10) 0.0281(12) 0.0185(11) -0.0050(9) 0.0039(8) -0.0001(9) C31 0.0344(14) 0.0262(13) 0.0313(14) 0.0040(10) -0.0073(11) -0.0043(11) C32 0.066(2) 0.0430(18) 0.054(2) -0.0190(16) -0.0150(18) -0.0086(16) C33 0.0248(12) 0.0303(13) 0.0172(11) -0.0005(9) -0.0008(9) 0.0002(9) O8 0.0298(9) 0.0223(8) 0.0239(9) 0.0004(7) 0.0032(7) -0.0028(7) O9 0.0258(9) 0.0310(9) 0.0154(8) -0.0020(7) 0.0018(6) -0.0030(7) O10 0.0217(8) 0.0286(9) 0.0196(8) -0.0100(7) 0.0005(6) -0.0004(7) O11 0.0154(7) 0.0275(9) 0.0222(8) -0.0040(7) 0.0012(6) -0.0021(6) O12 0.0195(8) 0.0264(9) 0.0247(8) -0.0073(7) 0.0017(6) -0.0079(6) C34 0.0305(13) 0.0281(13) 0.0301(13) 0.0055(10) -0.0005(11) 0.0026(10) C35 0.0354(14) 0.0380(15) 0.0186(12) 0.0061(10) -0.0007(10) -0.0044(11) C36 0.0271(12) 0.0423(15) 0.0167(11) -0.0087(10) 0.0022(9) -0.0060(11) C37 0.0299(13) 0.0392(14) 0.0203(11) -0.0139(10) -0.0005(9) -0.0064(11) C38 0.0246(12) 0.0243(12) 0.0292(13) -0.0093(10) 0.0059(10) -0.0012(9) C39 0.0228(11) 0.0234(12) 0.0296(13) -0.0036(10) 0.0025(9) -0.0003(9) C40 0.0137(10) 0.0363(14) 0.0320(13) -0.0068(11) 0.0016(9) -0.0021(9) C41 0.0163(11) 0.0425(14) 0.0227(11) -0.0098(10) 0.0007(9) -0.0086(10) C42 0.0322(14) 0.0292(13) 0.0358(14) -0.0116(11) 0.0070(11) -0.0143(11) C43 0.0385(15) 0.0275(13) 0.0364(15) 0.0004(11) 0.0051(12) -0.0144(11) O13 0.0168(8) 0.0306(9) 0.0165(8) -0.0001(7) 0.0000(6) -0.0027(7) S4 0.0348(3) 0.0275(3) 0.0206(3) -0.0070(2) 0.0017(2) -0.0087(3) O14 0.0500(13) 0.0422(12) 0.0418(12) -0.0169(10) 0.0166(10) -0.0204(10) O15 0.0519(14) 0.0528(14) 0.0578(15) -0.0187(12) -0.0228(12) 0.0058(11) O16 0.0686(17) 0.0397(12) 0.0467(13) -0.0142(10) 0.0128(12) -0.0038(11) C44 0.058(2) 0.057(2) 0.0372(17) -0.0210(15) 0.0197(15) -0.0216(17) F1 0.0750(16) 0.0973(18) 0.0442(12) -0.0189(12) 0.0264(11) -0.0572(14) F2 0.097(2) 0.0732(16) 0.0383(12) 0.0002(11) -0.0185(12) 0.0062(14) F3 0.0659(14) 0.0840(16) 0.0473(12) -0.0422(12) 0.0205(10) -0.0171(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 N4 2.0131(19) . ? Co1 N3 2.031(2) . ? Co1 N2 2.0368(19) . ? Co1 N1 2.1262(19) . ? Co1 O7 2.2205(16) . ? Ca1 O13 2.3687(17) . ? Ca1 O1 2.3987(15) . ? Ca1 O12 2.4485(17) . ? Ca1 O11 2.4854(17) . ? Ca1 O10 2.4905(17) . ? Ca1 O9 2.5209(17) . ? Ca1 O7 2.5306(17) . ? Ca1 O8 2.5418(18) . ? S1 O1 1.4565(16) . ? S1 O2 1.4579(17) . ? S1 N2 1.566(2) . ? S1 C3 1.797(2) . ? S2 O4 1.4425(19) . ? S2 O3 1.4602(18) . ? S2 N3 1.582(2) . ? S2 C14 1.798(2) . ? S3 O6 1.4413(18) . ? S3 O5 1.4579(17) . ? S3 N4 1.5803(19) . ? S3 C25 1.805(2) . ? O3 H1 1.820(7) . ? O5 H2 1.885(12) . ? O7 H1 0.8499(10) . ? O7 H2 0.8500(10) . ? N1 C12 1.466(3) . ? N1 C1 1.468(3) . ? N1 C23 1.473(3) . ? N2 C2 1.486(3) . ? N3 C13 1.477(3) . ? N4 C24 1.477(3) . ? C1 C2 1.521(4) . ? C3 C4 1.416(3) . ? C3 C8 1.418(3) . ? C4 C5 1.396(3) . ? C4 C9 1.516(4) . ? C5 C6 1.378(4) . ? C6 C7 1.394(4) . ? C6 C10 1.507(4) . ? C7 C8 1.397(3) . ? C8 C11 1.505(3) . ? C12 C13 1.524(3) . ? C14 C19 1.413(3) . ? C14 C15 1.419(3) . ? C15 C16 1.407(4) . ? C15 C20 1.516(4) . ? C16 C17 1.378(4) . ? C17 C18 1.387(4) . ? C17 C21 1.514(4) . ? C18 C19 1.394(4) . ? C19 C22 1.513(4) . ? C23 C24 1.518(3) . ? C25 C30 1.415(3) . ? C25 C26 1.415(3) . ? C26 C27 1.383(4) . ? C26 C31 1.511(4) . ? C27 C28 1.398(4) . ? C28 C29 1.386(4) . ? C28 C32 1.511(4) . ? C29 C30 1.397(4) . ? C30 C33 1.510(3) . ? O8 C34 1.443(3) . ? O8 C43 1.445(3) . ? O9 C35 1.422(3) . ? O9 C36 1.431(3) . ? O10 C38 1.441(3) . ? O10 C37 1.443(3) . ? O11 C39 1.438(3) . ? O11 C40 1.443(3) . ? O12 C42 1.420(3) . ? O12 C41 1.432(3) . ? C34 C35 1.503(4) . ? C36 C37 1.504(4) . ? C38 C39 1.504(4) . ? C40 C41 1.494(4) . ? C42 C43 1.488(4) . ? S4 O16 1.400(2) . ? S4 O14 1.418(2) . ? S4 O15 1.487(2) . ? S4 C44 1.799(3) . ? C44 F3 1.297(4) . ? C44 F1 1.308(4) . ? C44 F2 1.392(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 N4 Co1 N3 113.87(8) . . ? N4 Co1 N2 114.14(8) . . ? N3 Co1 N2 124.38(8) . . ? N4 Co1 N1 81.15(7) . . ? N3 Co1 N1 81.35(8) . . ? N2 Co1 N1 79.89(8) . . ? N4 Co1 O7 100.68(7) . . ? N3 Co1 O7 96.69(7) . . ? N2 Co1 O7 100.43(7) . . ? N1 Co1 O7 177.76(7) . . ? O13 Ca1 O1 77.68(6) . . ? O13 Ca1 O12 150.51(6) . . ? O1 Ca1 O12 127.53(6) . . ? O13 Ca1 O11 143.95(6) . . ? O1 Ca1 O11 74.49(5) . . ? O12 Ca1 O11 65.16(6) . . ? O13 Ca1 O10 87.84(6) . . ? O1 Ca1 O10 83.22(6) . . ? O12 Ca1 O10 108.27(6) . . ? O11 Ca1 O10 66.65(6) . . ? O13 Ca1 O9 71.26(6) . . ? O1 Ca1 O9 135.34(6) . . ? O12 Ca1 O9 93.01(6) . . ? O11 Ca1 O9 115.23(6) . . ? O10 Ca1 O9 64.65(6) . . ? O13 Ca1 O7 100.29(6) . . ? O1 Ca1 O7 72.19(5) . . ? O12 Ca1 O7 77.45(6) . . ? O11 Ca1 O7 92.58(6) . . ? O10 Ca1 O7 151.56(6) . . ? O9 Ca1 O7 143.76(6) . . ? O13 Ca1 O8 85.93(6) . . ? O1 Ca1 O8 144.56(6) . . ? O12 Ca1 O8 64.63(6) . . ? O11 Ca1 O8 129.64(6) . . ? O10 Ca1 O8 127.75(6) . . ? O9 Ca1 O8 64.26(6) . . ? O7 Ca1 O8 80.29(6) . . ? O1 S1 O2 112.82(9) . . ? O1 S1 N2 108.55(10) . . ? O2 S1 N2 112.92(11) . . ? O1 S1 C3 107.64(10) . . ? O2 S1 C3 105.86(10) . . ? N2 S1 C3 108.84(10) . . ? O4 S2 O3 114.40(11) . . ? O4 S2 N3 113.38(11) . . ? O3 S2 N3 107.79(10) . . ? O4 S2 C14 106.22(11) . . ? O3 S2 C14 108.08(11) . . ? N3 S2 C14 106.57(11) . . ? O6 S3 O5 114.64(11) . . ? O6 S3 N4 113.36(11) . . ? O5 S3 N4 106.96(10) . . ? O6 S3 C25 106.20(11) . . ? O5 S3 C25 107.75(11) . . ? N4 S3 C25 107.61(10) . . ? S1 O1 Ca1 137.67(9) . . ? S2 O3 H1 117.4(10) . . ? S3 O5 H2 123.5(9) . . ? H1 O7 H2 101(3) . . ? H1 O7 Co1 95(2) . . ? H2 O7 Co1 99(2) . . ? H1 O7 Ca1 116(2) . . ? H2 O7 Ca1 110(2) . . ? Co1 O7 Ca1 130.41(7) . . ? C12 N1 C1 113.21(19) . . ? C12 N1 C23 112.68(19) . . ? C1 N1 C23 113.18(19) . . ? C12 N1 Co1 106.46(14) . . ? C1 N1 Co1 105.74(14) . . ? C23 N1 Co1 104.69(14) . . ? C2 N2 S1 112.97(16) . . ? C2 N2 Co1 115.56(15) . . ? S1 N2 Co1 131.31(11) . . ? C13 N3 S2 112.44(16) . . ? C13 N3 Co1 114.86(15) . . ? S2 N3 Co1 132.68(12) . . ? C24 N4 S3 113.99(15) . . ? C24 N4 Co1 115.59(14) . . ? S3 N4 Co1 130.38(11) . . ? N1 C1 C2 111.23(19) . . ? N2 C2 C1 109.00(19) . . ? C4 C3 C8 120.5(2) . . ? C4 C3 S1 121.14(18) . . ? C8 C3 S1 118.31(17) . . ? C5 C4 C3 117.8(2) . . ? C5 C4 C9 116.1(2) . . ? C3 C4 C9 126.1(2) . . ? C6 C5 C4 123.3(2) . . ? C5 C6 C7 117.6(2) . . ? C5 C6 C10 120.4(3) . . ? C7 C6 C10 121.9(3) . . ? C6 C7 C8 122.7(2) . . ? C7 C8 C3 117.9(2) . . ? C7 C8 C11 117.3(2) . . ? C3 C8 C11 124.7(2) . . ? N1 C12 C13 110.5(2) . . ? N3 C13 C12 109.04(19) . . ? C19 C14 C15 120.3(2) . . ? C19 C14 S2 118.20(18) . . ? C15 C14 S2 121.39(18) . . ? C16 C15 C14 117.9(2) . . ? C16 C15 C20 116.0(2) . . ? C14 C15 C20 126.1(2) . . ? C17 C16 C15 122.6(2) . . ? C16 C17 C18 118.0(2) . . ? C16 C17 C21 120.9(3) . . ? C18 C17 C21 121.1(3) . . ? C17 C18 C19 122.9(2) . . ? C18 C19 C14 118.2(2) . . ? C18 C19 C22 117.4(2) . . ? C14 C19 C22 124.4(2) . . ? N1 C23 C24 110.77(19) . . ? N4 C24 C23 108.36(18) . . ? C30 C25 C26 120.5(2) . . ? C30 C25 S3 120.68(18) . . ? C26 C25 S3 118.82(18) . . ? C27 C26 C25 118.6(2) . . ? C27 C26 C31 116.4(2) . . ? C25 C26 C31 125.0(2) . . ? C26 C27 C28 122.4(3) . . ? C29 C28 C27 117.8(2) . . ? C29 C28 C32 121.7(3) . . ? C27 C28 C32 120.6(3) . . ? C28 C29 C30 122.9(2) . . ? C29 C30 C25 117.8(2) . . ? C29 C30 C33 115.9(2) . . ? C25 C30 C33 126.3(2) . . ? C34 O8 C43 111.5(2) . . ? C34 O8 Ca1 111.33(15) . . ? C43 O8 Ca1 117.07(15) . . ? C35 O9 C36 114.2(2) . . ? C35 O9 Ca1 121.70(15) . . ? C36 O9 Ca1 119.22(14) . . ? C38 O10 C37 113.48(19) . . ? C38 O10 Ca1 117.23(14) . . ? C37 O10 Ca1 116.85(15) . . ? C39 O11 C40 111.47(19) . . ? C39 O11 Ca1 112.63(13) . . ? C40 O11 Ca1 117.34(14) . . ? C42 O12 C41 112.54(19) . . ? C42 O12 Ca1 118.13(15) . . ? C41 O12 Ca1 118.34(14) . . ? O8 C34 C35 110.3(2) . . ? O9 C35 C34 106.6(2) . . ? O9 C36 C37 105.64(19) . . ? O10 C37 C36 110.1(2) . . ? O10 C38 C39 105.49(19) . . ? O11 C39 C38 110.2(2) . . ? O11 C40 C41 107.6(2) . . ? O12 C41 C40 107.08(19) . . ? O12 C42 C43 107.6(2) . . ? O8 C43 C42 109.3(2) . . ? O16 S4 O14 120.32(15) . . ? O16 S4 O15 113.07(16) . . ? O14 S4 O15 110.15(15) . . ? O16 S4 C44 106.63(16) . . ? O14 S4 C44 104.84(15) . . ? O15 S4 C44 99.20(18) . . ? F3 C44 F1 111.9(3) . . ? F3 C44 F2 102.0(3) . . ? F1 C44 F2 105.1(3) . . ? F3 C44 S4 115.1(3) . . ? F1 C44 S4 113.6(2) . . ? F2 C44 S4 107.8(2) . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.350 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.087 _iucr_refine_instructions_details ; TITL asb228 in P-1 CELL 0.71073 9.4438 17.4810 17.5309 73.4591 88.5336 85.2907 ZERR 2.00 0.0004 0.0007 0.0007 0.0004 0.0004 0.0005 LATT 1 SFAC C H N O F S CA CO UNIT 88 138 8 32 6 8 2 2 TEMP -185.000 SIZE 0.12 0.17 0.467 rem Squeezed files rem David Lacy 20s sphere CCD1 rem APEX2 2010.9-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 BOND H1 BOND H2 BIND H1 O3 H2 O5 BIND O7 H1 O7 H2 DFIX 0.850 0.001 h1 o7 h2 o7 h13c o13 h13d o13 CONN 8 CA1 L.S. 12 ACTA 51 WGHT 0.080000 2.414800 FVAR 1.50164 CO1 8 -0.493132 1.296641 -0.293110 11.00000 0.01476 0.01743 = 0.01372 -0.00147 0.00146 0.00027 CA1 7 -0.604184 1.314998 -0.058324 11.00000 0.01402 0.01892 = 0.01318 -0.00229 0.00098 -0.00254 S1 6 -0.385815 1.431039 -0.213698 11.00000 0.01412 0.02181 = 0.01387 -0.00204 0.00130 -0.00360 S2 6 -0.441253 1.098841 -0.231421 11.00000 0.02106 0.01850 = 0.01903 -0.00100 -0.00048 -0.00126 S3 6 -0.819231 1.345219 -0.357180 11.00000 0.01594 0.02425 = 0.01540 -0.00395 0.00071 0.00085 O1 4 -0.518708 1.414966 -0.170249 11.00000 0.01562 0.02195 = 0.01420 -0.00168 0.00325 -0.00215 O2 4 -0.263842 1.420650 -0.161390 11.00000 0.01830 0.03034 = 0.01834 -0.00139 -0.00150 -0.00732 O3 4 -0.521287 1.111855 -0.163240 11.00000 0.02348 0.02372 = 0.02008 -0.00091 0.00228 -0.00223 O4 4 -0.499641 1.043219 -0.266725 11.00000 0.02765 0.02757 = 0.02915 -0.00769 -0.00292 -0.00445 O5 4 -0.843551 1.308778 -0.272610 11.00000 0.01650 0.03976 = 0.01737 -0.00519 0.00227 -0.00004 O6 4 -0.892861 1.422988 -0.389226 11.00000 0.02507 0.02808 = 0.02581 -0.00880 -0.00315 0.00633 O7 4 -0.612190 1.263424 -0.179050 11.00000 0.01832 0.02148 = 0.01584 -0.00290 0.00137 -0.00166 H1 2 -0.595440 1.213240 -0.170989 11.00000 0.02565 H2 2 -0.695985 1.270644 -0.197709 11.00000 0.02681 N1 3 -0.373640 1.324371 -0.400606 11.00000 0.02009 0.01941 = 0.01779 -0.00276 0.00317 0.00150 N2 3 -0.368106 1.378185 -0.272489 11.00000 0.01285 0.02419 = 0.01792 -0.00538 0.00458 -0.00336 N3 3 -0.422658 1.183560 -0.292611 11.00000 0.02510 0.01992 = 0.01838 0.00045 0.00389 0.00345 N4 3 -0.652952 1.344869 -0.369962 11.00000 0.01502 0.02154 = 0.01500 -0.00038 0.00108 -0.00154 C1 1 -0.232281 1.340207 -0.378686 11.00000 0.01937 0.03351 = 0.02448 -0.00648 0.00540 0.00037 AFIX 23 H1A 2 -0.178416 1.364712 -0.427530 11.00000 -1.20000 H1B 2 -0.179778 1.289041 -0.350273 11.00000 -1.20000 AFIX 0 C2 1 -0.242795 1.395962 -0.325823 11.00000 0.01474 0.03205 = 0.02415 -0.00707 0.00736 -0.00386 AFIX 23 H2A 2 -0.155280 1.388144 -0.293711 11.00000 -1.20000 H2B 2 -0.253037 1.452333 -0.359049 11.00000 -1.20000 AFIX 0 C3 1 -0.398849 1.534689 -0.270336 11.00000 0.02451 0.02125 = 0.01408 -0.00316 0.00483 -0.00577 C4 1 -0.280676 1.581426 -0.279224 11.00000 0.02880 0.02724 = 0.01441 -0.00567 0.00438 -0.00884 C5 1 -0.300171 1.662050 -0.322394 11.00000 0.03964 0.02648 = 0.01840 -0.00581 0.00769 -0.01354 AFIX 43 H5A 2 -0.221543 1.693891 -0.328514 11.00000 -1.20000 AFIX 0 C6 1 -0.427651 1.697761 -0.356564 11.00000 0.05277 0.02256 = 0.01492 -0.00455 0.00510 -0.00625 C7 1 -0.541002 1.649788 -0.348816 11.00000 0.03567 0.02510 = 0.01604 -0.00471 -0.00005 0.00223 AFIX 43 H7A 2 -0.629382 1.673436 -0.372430 11.00000 -1.20000 AFIX 0 C8 1 -0.529969 1.568358 -0.307749 11.00000 0.02496 0.02302 = 0.01481 -0.00515 0.00330 -0.00141 C9 1 -0.133751 1.552672 -0.244806 11.00000 0.02526 0.03523 = 0.02401 -0.00638 0.00376 -0.01461 AFIX 137 H9A 2 -0.067378 1.593302 -0.268312 11.00000 -1.50000 H9B 2 -0.101875 1.502591 -0.256852 11.00000 -1.50000 H9C 2 -0.137010 1.543533 -0.187002 11.00000 -1.50000 AFIX 0 C10 1 -0.442220 1.785840 -0.399962 11.00000 0.06981 0.02398 = 0.03224 -0.00198 -0.00305 -0.00806 AFIX 137 H10A 2 -0.412457 1.816403 -0.364988 11.00000 -1.50000 H10B 2 -0.541557 1.802196 -0.415459 11.00000 -1.50000 H10C 2 -0.382119 1.796185 -0.447655 11.00000 -1.50000 AFIX 0 C11 1 -0.657679 1.522284 -0.308093 11.00000 0.02207 0.02630 = 0.01934 -0.00280 -0.00118 0.00176 AFIX 137 H11A 2 -0.628491 1.473636 -0.323489 11.00000 -1.50000 H11B 2 -0.727665 1.555565 -0.346235 11.00000 -1.50000 H11C 2 -0.700022 1.507654 -0.254780 11.00000 -1.50000 AFIX 0 C12 1 -0.371797 1.254320 -0.430960 11.00000 0.03114 0.02468 = 0.02047 -0.00527 0.00605 0.00278 AFIX 23 H12A 2 -0.298072 1.258144 -0.472770 11.00000 -1.20000 H12B 2 -0.464941 1.253131 -0.455085 11.00000 -1.20000 AFIX 0 C13 1 -0.340844 1.177574 -0.363902 11.00000 0.03521 0.02225 = 0.02294 -0.00238 0.00930 0.00391 AFIX 23 H13A 2 -0.368078 1.131113 -0.380335 11.00000 -1.20000 H13B 2 -0.237979 1.169674 -0.351728 11.00000 -1.20000 AFIX 0 C14 1 -0.265913 1.056615 -0.197927 11.00000 0.02042 0.01743 = 0.02274 0.00018 -0.00198 -0.00040 C15 1 -0.191482 0.999260 -0.230430 11.00000 0.02647 0.01772 = 0.02403 -0.00022 -0.00015 -0.00054 C16 1 -0.052592 0.971377 -0.203202 11.00000 0.02840 0.01877 = 0.03162 -0.00021 0.00175 0.00234 AFIX 43 H16A 2 -0.000904 0.933868 -0.225392 11.00000 -1.20000 AFIX 0 C17 1 0.011419 0.996311 -0.145641 11.00000 0.02379 0.01871 = 0.03837 0.00278 -0.00239 -0.00217 C18 1 -0.064112 1.052587 -0.115285 11.00000 0.02655 0.02171 = 0.03430 -0.00332 -0.00546 -0.00450 AFIX 43 H18A 2 -0.021308 1.069576 -0.075058 11.00000 -1.20000 AFIX 0 C19 1 -0.200054 1.085331 -0.141182 11.00000 0.02439 0.01969 = 0.02796 -0.00339 -0.00121 -0.00304 C20 1 -0.247059 0.964686 -0.292904 11.00000 0.04012 0.02423 = 0.02929 -0.00843 -0.00425 0.00618 AFIX 137 H20A 2 -0.177235 0.923436 -0.301849 11.00000 -1.50000 H20B 2 -0.263202 1.007367 -0.342749 11.00000 -1.50000 H20C 2 -0.336664 0.940908 -0.274495 11.00000 -1.50000 AFIX 0 C21 1 0.160927 0.964559 -0.117893 11.00000 0.02424 0.03019 = 0.05011 -0.00357 -0.00786 0.00205 AFIX 137 H21A 2 0.179363 0.976789 -0.068032 11.00000 -1.50000 H21B 2 0.229047 0.989867 -0.158504 11.00000 -1.50000 H21C 2 0.171172 0.906462 -0.109177 11.00000 -1.50000 AFIX 0 C22 1 -0.265878 1.150725 -0.107511 11.00000 0.03040 0.02691 = 0.03595 -0.01310 -0.00705 0.00237 AFIX 137 H22A 2 -0.197413 1.163182 -0.072554 11.00000 -1.50000 H22B 2 -0.351265 1.132555 -0.077004 11.00000 -1.50000 H22C 2 -0.291579 1.198783 -0.151170 11.00000 -1.50000 AFIX 0 C23 1 -0.452049 1.395552 -0.452837 11.00000 0.02169 0.02319 = 0.01955 -0.00057 0.00345 0.00052 AFIX 23 H23A 2 -0.414622 1.405557 -0.507781 11.00000 -1.20000 H23B 2 -0.437724 1.442883 -0.434408 11.00000 -1.20000 AFIX 0 C24 1 -0.609623 1.383874 -0.452513 11.00000 0.02232 0.02335 = 0.01520 0.00227 0.00078 -0.00147 AFIX 23 H24A 2 -0.664487 1.436261 -0.472918 11.00000 -1.20000 H24B 2 -0.628442 1.350019 -0.487228 11.00000 -1.20000 AFIX 0 C25 1 -0.884984 1.281237 -0.410693 11.00000 0.01499 0.02396 = 0.01958 -0.00377 0.00081 0.00022 C26 1 -0.882636 1.198008 -0.372933 11.00000 0.01860 0.02850 = 0.02730 -0.00156 0.00003 -0.00278 C27 1 -0.940652 1.149820 -0.412316 11.00000 0.03012 0.02668 = 0.03641 -0.00404 -0.00339 -0.00367 AFIX 43 H27A 2 -0.942293 1.094216 -0.386342 11.00000 -1.20000 AFIX 0 C28 1 -0.996971 1.180015 -0.488987 11.00000 0.03207 0.03489 = 0.03810 -0.01478 -0.00515 -0.00114 C29 1 -0.992102 1.261157 -0.525941 11.00000 0.02583 0.03739 = 0.02235 -0.00930 -0.00135 -0.00133 AFIX 43 H29A 2 -1.026879 1.282046 -0.578778 11.00000 -1.20000 AFIX 0 C30 1 -0.938311 1.313619 -0.488936 11.00000 0.01677 0.02814 = 0.01849 -0.00501 0.00389 -0.00010 C31 1 -0.820673 1.156445 -0.291695 11.00000 0.03439 0.02616 = 0.03133 0.00401 -0.00732 -0.00432 AFIX 137 H31A 2 -0.810101 1.098541 -0.284243 11.00000 -1.50000 H31B 2 -0.884248 1.168078 -0.250663 11.00000 -1.50000 H31C 2 -0.727472 1.175755 -0.287481 11.00000 -1.50000 AFIX 0 C32 1 -1.062040 1.125500 -0.529148 11.00000 0.06617 0.04301 = 0.05390 -0.01899 -0.01498 -0.00857 AFIX 137 H32A 2 -1.092060 1.078235 -0.488702 11.00000 -1.50000 H32B 2 -0.991659 1.108729 -0.564425 11.00000 -1.50000 H32C 2 -1.144616 1.154169 -0.560371 11.00000 -1.50000 AFIX 0 C33 1 -0.948629 1.400873 -0.536123 11.00000 0.02478 0.03026 = 0.01722 -0.00045 -0.00081 0.00016 AFIX 137 H33A 2 -0.984213 1.406444 -0.589610 11.00000 -1.50000 H33B 2 -0.854412 1.421405 -0.540089 11.00000 -1.50000 H33C 2 -1.013958 1.431381 -0.509284 11.00000 -1.50000 AFIX 0 O8 4 -0.599098 1.165595 0.010112 11.00000 0.02981 0.02234 = 0.02385 0.00037 0.00316 -0.00279 O9 4 -0.561780 1.273336 0.089709 11.00000 0.02576 0.03098 = 0.01542 -0.00203 0.00176 -0.00300 O10 4 -0.619477 1.426148 0.005000 11.00000 0.02168 0.02862 = 0.01957 -0.01002 0.00047 -0.00043 O11 4 -0.810422 1.414006 -0.104768 11.00000 0.01544 0.02754 = 0.02217 -0.00398 0.00115 -0.00211 O12 4 -0.835115 1.258077 -0.043900 11.00000 0.01949 0.02639 = 0.02468 -0.00728 0.00167 -0.00794 C34 1 -0.509521 1.143097 0.079696 11.00000 0.03046 0.02815 = 0.03010 0.00550 -0.00049 0.00260 AFIX 23 H34A 2 -0.409632 1.151969 0.063457 11.00000 -1.20000 H34B 2 -0.514860 1.085486 0.107234 11.00000 -1.20000 AFIX 0 C35 1 -0.555944 1.191676 0.135442 11.00000 0.03537 0.03803 = 0.01856 0.00612 -0.00069 -0.00435 AFIX 23 H35A 2 -0.650528 1.177525 0.158203 11.00000 -1.20000 H35B 2 -0.487236 1.181575 0.179583 11.00000 -1.20000 AFIX 0 C36 1 -0.601736 1.328786 0.134245 11.00000 0.02706 0.04226 = 0.01665 -0.00867 0.00215 -0.00596 AFIX 23 H36A 2 -0.551443 1.313131 0.185901 11.00000 -1.20000 H36B 2 -0.705381 1.330755 0.144422 11.00000 -1.20000 AFIX 0 C37 1 -0.559660 1.408629 0.083618 11.00000 0.02986 0.03917 = 0.02030 -0.01391 -0.00054 -0.00643 AFIX 23 H37A 2 -0.594146 1.450926 0.108511 11.00000 -1.20000 H37B 2 -0.454805 1.407849 0.079808 11.00000 -1.20000 AFIX 0 C38 1 -0.749684 1.477084 -0.005483 11.00000 0.02463 0.02432 = 0.02918 -0.00929 0.00594 -0.00120 AFIX 23 H38A 2 -0.734185 1.528800 0.004344 11.00000 -1.20000 H38B 2 -0.823866 1.451061 0.031549 11.00000 -1.20000 AFIX 0 C39 1 -0.792884 1.489663 -0.090415 11.00000 0.02285 0.02344 = 0.02960 -0.00363 0.00249 -0.00033 AFIX 23 H39A 2 -0.883252 1.523755 -0.101378 11.00000 -1.20000 H39B 2 -0.719296 1.517485 -0.126656 11.00000 -1.20000 AFIX 0 C40 1 -0.950205 1.387799 -0.081696 11.00000 0.01374 0.03625 = 0.03204 -0.00678 0.00159 -0.00213 AFIX 23 H40A 2 -1.023039 1.424034 -0.116730 11.00000 -1.20000 H40B 2 -0.970785 1.388130 -0.026129 11.00000 -1.20000 AFIX 0 C41 1 -0.952362 1.304886 -0.089146 11.00000 0.01628 0.04246 = 0.02269 -0.00985 0.00073 -0.00858 AFIX 23 H41A 2 -1.042918 1.282190 -0.068223 11.00000 -1.20000 H41B 2 -0.942842 1.305375 -0.145649 11.00000 -1.20000 AFIX 0 C42 1 -0.837596 1.175133 -0.036411 11.00000 0.03216 0.02922 = 0.03577 -0.01162 0.00701 -0.01430 AFIX 23 H42A 2 -0.810643 1.164300 -0.087509 11.00000 -1.20000 H42B 2 -0.934193 1.157711 -0.021743 11.00000 -1.20000 AFIX 0 C43 1 -0.734438 1.131145 0.026754 11.00000 0.03851 0.02751 = 0.03640 0.00043 0.00509 -0.01438 AFIX 23 H43A 2 -0.770155 1.134867 0.079266 11.00000 -1.20000 H43B 2 -0.723089 1.073913 0.028318 11.00000 -1.20000 AFIX 0 O13 4 -0.356130 1.300893 -0.035125 11.00000 0.01678 0.03065 = 0.01653 -0.00013 -0.00005 -0.00273 H13C 2 -0.320122 1.299716 0.009168 11.00000 0.03296 H13D 2 -0.310631 1.336633 -0.067169 11.00000 0.03253 S4 6 -0.074723 1.283323 0.127909 11.00000 0.03484 0.02749 = 0.02063 -0.00696 0.00172 -0.00870 O14 4 0.024847 1.341507 0.120429 11.00000 0.05003 0.04223 = 0.04179 -0.01687 0.01657 -0.02037 O15 4 -0.213032 1.322288 0.092473 11.00000 0.05191 0.05281 = 0.05778 -0.01873 -0.02280 0.00576 O16 4 -0.035379 1.211821 0.109182 11.00000 0.06857 0.03970 = 0.04668 -0.01421 0.01280 -0.00379 C44 1 -0.124624 1.256075 0.231341 11.00000 0.05817 0.05728 = 0.03718 -0.02098 0.01968 -0.02163 F1 5 -0.221406 1.204369 0.249098 11.00000 0.07496 0.09730 = 0.04417 -0.01885 0.02640 -0.05715 F2 5 -0.005827 1.217371 0.275483 11.00000 0.09723 0.07321 = 0.03832 0.00021 -0.01849 0.00621 F3 5 -0.154883 1.315682 0.260705 11.00000 0.06592 0.08398 = 0.04730 -0.04217 0.02048 -0.01707 HKLF 4 REM asb228 in P-1 REM R1 = 0.0461 for 11313 Fo > 4sig(Fo) and 0.0526 for all 13265 data REM 683 parameters refined using 4 restraints END WGHT 0.0800 2.4146 REM Highest difference peak 2.350, deepest hole -0.783, 1-sigma level 0.087 Q1 1 0.0693 1.2186 0.1708 11.00000 0.05 2.35 Q2 1 -0.1319 1.2442 0.0786 11.00000 0.05 2.30 Q3 1 -0.2857 1.3270 0.1836 11.00000 0.05 2.22 Q4 1 -0.0420 1.3602 0.0907 11.00000 0.05 0.94 Q5 1 -0.0818 1.2824 0.2705 11.00000 0.05 0.76 Q6 1 -0.0083 1.2584 0.1398 11.00000 0.05 0.75 Q7 1 -0.1841 1.2876 0.2038 11.00000 0.05 0.73 Q8 1 -0.7370 1.3486 -0.3637 11.00000 0.05 0.59 Q9 1 -0.0955 1.2677 0.1759 11.00000 0.05 0.57 Q10 1 -0.3626 1.3916 -0.2281 11.00000 0.05 0.53 Q11 1 -0.4860 1.2578 -0.3033 11.00000 0.05 0.51 Q12 1 -0.8515 1.3122 -0.3819 11.00000 0.05 0.47 Q13 1 -0.5866 1.2725 -0.0604 11.00000 0.05 0.45 Q14 1 -0.2842 1.3967 -0.4035 11.00000 0.05 0.45 Q15 1 -0.9269 1.1610 -0.4568 11.00000 0.05 0.44 Q16 1 -0.5760 1.2959 -0.2880 11.00000 0.05 0.44 Q17 1 -0.5396 1.3850 -0.4540 11.00000 0.05 0.42 Q18 1 -0.9360 1.3475 -0.0865 11.00000 0.05 0.42 Q19 1 -0.3307 1.4185 -0.1786 11.00000 0.05 0.41 Q20 1 -0.5924 1.5466 -0.3017 11.00000 0.05 0.41 ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 1.000 0.500 171 47 ' ' 2 0.500 0.000 1.000 11 0 ' ' _platon_squeeze_details ; There were several high residuals present in the final difference-Fourier map. It was not possible to determine the nature of the residuals although it is probable that dichloromethane solvent was present. ;