# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_asb189 _database_code_depnum_ccdc_archive 'CCDC 895607' #TrackingRef '13191_web_deposit_cif_file_0_NathanielS.Sickerman_1344538304.SuperCif.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H68 Ca Cl2 F3 Fe N4 O15 S4' _chemical_formula_weight 1257.10 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' 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' Fe Fe 0.3463 0.8444 '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 14.2376(5) _cell_length_b 14.5557(5) _cell_length_c 16.0245(6) _cell_angle_alpha 112.0349(4) _cell_angle_beta 96.1392(4) _cell_angle_gamma 107.9824(4) _cell_volume 2832.94(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.23 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1314 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8077 _exptl_absorpt_correction_T_max 0.8895 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33973 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.88 _reflns_number_total 13241 _reflns_number_gt 11334 _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. Hydrogen atom H(7) was located from a difference-Fourier map and refined (x,y,z and Uiso) with d(O-H) fixed at 0.85 ang. The remaining hydrogen atoms were included using a riding model. The fluorine atoms, oxygen atoms O(14) and O(15) and carbon atoms C(37), C(38) and C(40) were disordered and included using multiple components and partial site-occupancy-factors. Equivalent anisotropic thermal parameters were used for the fluorine atoms. There was one molecule of dichloromethane solvent present. ; _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^)+(0.0564P)^2^+2.8693P] 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 13241 _refine_ls_number_parameters 733 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.19919(2) 0.45178(2) 0.716377(19) 0.01999(8) Uani 1 1 d . . . Ca1 Ca 0.08624(3) 0.22996(3) 0.78210(3) 0.02256(9) Uani 1 1 d . B . S1 S 0.26735(5) 0.25215(5) 0.63219(4) 0.03117(13) Uani 1 1 d . . . S2 S -0.03346(4) 0.28740(4) 0.60737(4) 0.02520(11) Uani 1 1 d . . . S3 S 0.21650(4) 0.66897(4) 0.89343(4) 0.02692(12) Uani 1 1 d . . . O1 O 0.19848(13) 0.21899(13) 0.68519(13) 0.0361(4) Uani 1 1 d . . . O2 O 0.23368(17) 0.18770(18) 0.53360(13) 0.0524(5) Uani 1 1 d . . . O3 O -0.02360(12) 0.26871(14) 0.69004(12) 0.0344(4) Uani 1 1 d . . . O4 O -0.04655(14) 0.19874(14) 0.52182(13) 0.0438(5) Uani 1 1 d . . . O5 O 0.18922(13) 0.59586(12) 0.93623(11) 0.0321(3) Uani 1 1 d . . . O6 O 0.13910(13) 0.70915(14) 0.87647(13) 0.0392(4) Uani 1 1 d . . . O7 O 0.17639(12) 0.40484(12) 0.80857(10) 0.0246(3) Uani 1 1 d D . . H7 H 0.175(2) 0.4570(16) 0.8554(14) 0.049(9) Uiso 1 1 d D . . O8 O 0.23556(14) 0.26549(15) 0.90547(13) 0.0411(4) Uani 1 1 d . B . O9 O 0.12012(14) 0.07041(14) 0.77293(13) 0.0381(4) Uani 1 1 d . B . O10 O -0.04484(14) 0.05102(13) 0.66614(12) 0.0350(4) Uani 1 1 d . . . O11 O -0.07574(14) 0.17175(14) 0.82886(12) 0.0389(4) Uani 1 1 d . . . O12 O 0.08771(13) 0.34395(15) 0.94705(11) 0.0396(4) Uani 1 1 d . . . N1 N 0.24260(13) 0.52219(15) 0.61756(12) 0.0255(4) Uani 1 1 d . . . N2 N 0.28774(14) 0.37383(16) 0.65781(14) 0.0286(4) Uani 1 1 d . . . N3 N 0.06246(13) 0.39089(15) 0.62517(12) 0.0243(4) Uani 1 1 d . . . N4 N 0.24800(15) 0.61231(15) 0.80007(13) 0.0293(4) Uani 1 1 d . . . C1 C 0.2862(2) 0.4555(2) 0.55155(17) 0.0358(5) Uani 1 1 d . . . H1B H 0.3295 0.4980 0.5241 0.043 Uiso 1 1 calc R . . H1C H 0.2306 0.3932 0.5005 0.043 Uiso 1 1 calc R . . C2 C 0.3496(2) 0.4174(2) 0.6031(2) 0.0403(6) Uani 1 1 d . . . H2A H 0.3678 0.3613 0.5583 0.048 Uiso 1 1 calc R . . H2B H 0.4133 0.4778 0.6448 0.048 Uiso 1 1 calc R . . C3 C 0.3862(2) 0.2432(2) 0.6728(2) 0.0384(6) Uani 1 1 d . . . C4 C 0.4136(3) 0.1595(3) 0.6164(3) 0.0576(9) Uani 1 1 d . . . C5 C 0.5101(3) 0.1604(3) 0.6538(3) 0.0723(12) Uani 1 1 d . . . H5B H 0.5299 0.1042 0.6180 0.087 Uiso 1 1 calc R . . C6 C 0.5752(3) 0.2359(4) 0.7368(3) 0.0634(10) Uani 1 1 d . . . C7 C 0.5437(2) 0.3133(3) 0.7889(3) 0.0568(9) Uani 1 1 d . . . H7B H 0.5874 0.3662 0.8477 0.068 Uiso 1 1 calc R . . C8 C 0.4499(2) 0.3187(2) 0.7600(2) 0.0406(6) Uani 1 1 d . . . C9 C 0.3508(4) 0.0722(4) 0.5218(3) 0.0962(16) Uani 1 1 d . . . H9A H 0.2798 0.0424 0.5241 0.144 Uiso 1 1 calc R . . H9B H 0.3782 0.0155 0.5037 0.144 Uiso 1 1 calc R . . H9C H 0.3537 0.1020 0.4760 0.144 Uiso 1 1 calc R . . C10 C 0.6755(3) 0.2301(5) 0.7689(4) 0.0977(18) Uani 1 1 d . . . H10A H 0.7102 0.2188 0.7184 0.147 Uiso 1 1 calc R . . H10B H 0.6633 0.1704 0.7863 0.147 Uiso 1 1 calc R . . H10C H 0.7183 0.2972 0.8229 0.147 Uiso 1 1 calc R . . C11 C 0.4264(2) 0.4084(3) 0.82669(19) 0.0460(7) Uani 1 1 d . . . H11A H 0.4682 0.4342 0.8896 0.069 Uiso 1 1 calc R . . H11B H 0.3540 0.3824 0.8261 0.069 Uiso 1 1 calc R . . H11C H 0.4417 0.4671 0.8079 0.069 Uiso 1 1 calc R . . C12 C 0.14719(18) 0.5202(2) 0.56969(18) 0.0347(5) Uani 1 1 d . . . H12A H 0.1565 0.5310 0.5132 0.042 Uiso 1 1 calc R . . H12B H 0.1295 0.5790 0.6112 0.042 Uiso 1 1 calc R . . C13 C 0.06180(19) 0.4138(2) 0.54288(17) 0.0388(6) Uani 1 1 d . . . H13A H -0.0046 0.4168 0.5216 0.047 Uiso 1 1 calc R . . H13B H 0.0719 0.3565 0.4914 0.047 Uiso 1 1 calc R . . C14 C -0.14399(15) 0.32057(16) 0.59928(14) 0.0226(4) Uani 1 1 d . . . C15 C -0.22713(17) 0.26075(18) 0.52036(15) 0.0289(4) Uani 1 1 d . . . C16 C -0.31360(17) 0.2869(2) 0.52281(17) 0.0318(5) Uani 1 1 d . . . H16A H -0.3714 0.2449 0.4710 0.038 Uiso 1 1 calc R . . C17 C -0.31904(17) 0.3709(2) 0.59690(18) 0.0320(5) Uani 1 1 d . . . C18 C -0.23460(18) 0.4308(2) 0.67203(18) 0.0349(5) Uani 1 1 d . . . H18A H -0.2362 0.4905 0.7228 0.042 Uiso 1 1 calc R . . C19 C -0.14744(17) 0.40692(19) 0.67603(16) 0.0298(5) Uani 1 1 d . . . C20 C -0.2303(2) 0.1726(3) 0.4307(2) 0.0589(9) Uani 1 1 d . . . H20A H -0.1749 0.2008 0.4048 0.088 Uiso 1 1 calc R . . H20B H -0.2960 0.1457 0.3861 0.088 Uiso 1 1 calc R . . H20C H -0.2220 0.1141 0.4430 0.088 Uiso 1 1 calc R . . C21 C -0.41410(19) 0.3963(3) 0.5959(2) 0.0447(7) Uani 1 1 d . . . H21A H -0.4480 0.3768 0.5318 0.067 Uiso 1 1 calc R . . H21B H -0.3955 0.4731 0.6335 0.067 Uiso 1 1 calc R . . H21C H -0.4605 0.3555 0.6217 0.067 Uiso 1 1 calc R . . C22 C -0.0618(2) 0.4762(2) 0.76280(19) 0.0503(8) Uani 1 1 d . . . H22A H -0.0847 0.5246 0.8095 0.075 Uiso 1 1 calc R . . H22B H -0.0033 0.5184 0.7480 0.075 Uiso 1 1 calc R . . H22C H -0.0416 0.4309 0.7874 0.075 Uiso 1 1 calc R . . C23 C 0.3185(2) 0.6317(2) 0.67365(18) 0.0391(6) Uani 1 1 d . . . H23A H 0.3266 0.6724 0.6356 0.047 Uiso 1 1 calc R . . H23B H 0.3854 0.6289 0.6938 0.047 Uiso 1 1 calc R . . C24 C 0.2843(3) 0.6877(2) 0.75826(19) 0.0470(7) Uani 1 1 d . . . H24A H 0.3418 0.7530 0.8039 0.056 Uiso 1 1 calc R . . H24B H 0.2285 0.7088 0.7398 0.056 Uiso 1 1 calc R . . C25 C 0.32676(17) 0.78152(17) 0.97332(15) 0.0270(4) Uani 1 1 d . . . C26 C 0.40846(17) 0.76050(18) 1.00987(16) 0.0303(5) Uani 1 1 d . . . C27 C 0.48534(18) 0.8442(2) 1.08502(18) 0.0359(5) Uani 1 1 d . . . H27A H 0.5402 0.8307 1.1107 0.043 Uiso 1 1 calc R . . C28 C 0.48505(19) 0.9468(2) 1.12407(18) 0.0382(5) Uani 1 1 d . . . C29 C 0.4095(2) 0.96718(19) 1.08168(18) 0.0383(5) Uani 1 1 d . . . H29A H 0.4118 1.0385 1.1050 0.046 Uiso 1 1 calc R . . C30 C 0.32934(19) 0.88688(19) 1.00552(17) 0.0335(5) Uani 1 1 d . . . C31 C 0.4191(2) 0.6536(2) 0.96974(19) 0.0403(6) Uani 1 1 d . . . H31A H 0.3598 0.5988 0.9717 0.060 Uiso 1 1 calc R . . H31B H 0.4814 0.6579 1.0063 0.060 Uiso 1 1 calc R . . H31C H 0.4231 0.6348 0.9051 0.060 Uiso 1 1 calc R . . C32 C 0.5656(2) 1.0328(2) 1.2103(2) 0.0573(8) Uani 1 1 d . . . H32A H 0.5741 1.0042 1.2559 0.086 Uiso 1 1 calc R . . H32B H 0.5448 1.0936 1.2371 0.086 Uiso 1 1 calc R . . H32C H 0.6305 1.0566 1.1942 0.086 Uiso 1 1 calc R . . C33 C 0.2549(2) 0.9232(2) 0.9650(2) 0.0515(8) Uani 1 1 d . . . H33A H 0.2855 1.0009 0.9860 0.077 Uiso 1 1 calc R . . H33B H 0.1922 0.9049 0.9857 0.077 Uiso 1 1 calc R . . H33C H 0.2387 0.8873 0.8969 0.077 Uiso 1 1 calc R . . C34 C 0.2400(2) 0.1737(3) 0.9167(2) 0.0489(7) Uani 1 1 d . . . H34A H 0.1885 0.1505 0.9491 0.059 Uiso 1 1 calc R . . H34B H 0.3084 0.1905 0.9536 0.059 Uiso 1 1 calc R . . C35 C 0.2185(2) 0.0885(2) 0.8218(2) 0.0471(7) Uani 1 1 d . . . H35A H 0.2706 0.1114 0.7898 0.057 Uiso 1 1 calc R . . H35B H 0.2194 0.0220 0.8248 0.057 Uiso 1 1 calc R . . C36 C 0.0864(2) -0.0144(2) 0.6804(2) 0.0456(6) Uani 1 1 d . . . H36A H 0.1033 -0.0757 0.6796 0.055 Uiso 0.50 1 calc PR A 1 H36B H 0.1192 0.0108 0.6374 0.055 Uiso 0.50 1 calc PR A 1 H36C H 0.1453 -0.0199 0.6581 0.055 Uiso 0.50 1 d PR A 2 H36D H 0.0512 -0.0803 0.6837 0.055 Uiso 0.50 1 d PR A 2 C37 C -0.0297(3) -0.0470(3) 0.6519(3) 0.0408(9) Uani 0.746(5) 1 d P B 1 H37A H -0.0580 -0.0997 0.5859 0.049 Uiso 0.746(5) 1 calc PR B 1 H37B H -0.0633 -0.0788 0.6909 0.049 Uiso 0.746(5) 1 calc PR B 1 C38 C -0.1502(2) 0.0371(3) 0.6757(2) 0.0346(8) Uani 0.746(5) 1 d P B 1 H38A H -0.1750 0.0812 0.6517 0.042 Uiso 0.746(5) 1 calc PR B 1 H38B H -0.1961 -0.0388 0.6386 0.042 Uiso 0.746(5) 1 calc PR B 1 C40 C -0.0815(3) 0.2192(3) 0.9232(3) 0.0396(9) Uani 0.746(5) 1 d P B 1 H40A H -0.0626 0.1808 0.9575 0.048 Uiso 0.746(5) 1 calc PR B 1 H40B H -0.1519 0.2151 0.9251 0.048 Uiso 0.746(5) 1 calc PR B 1 C37B C 0.0206(8) -0.0031(9) 0.6149(7) 0.044(3) Uani 0.254(5) 1 d P B 2 H37C H -0.0230 -0.0742 0.5643 0.053 Uiso 0.254(5) 1 calc PR B 2 H37D H 0.0612 0.0408 0.5872 0.053 Uiso 0.254(5) 1 calc PR B 2 C38B C -0.1072(8) 0.0024(7) 0.7014(7) 0.036(3) Uani 0.254(5) 1 d P B 2 H38C H -0.0719 -0.0299 0.7320 0.043 Uiso 0.254(5) 1 calc PR B 2 H38D H -0.1645 -0.0571 0.6499 0.043 Uiso 0.254(5) 1 calc PR B 2 C40B C -0.0875(8) 0.2526(11) 0.8916(9) 0.041(3) Uani 0.254(5) 1 d P B 2 H40C H -0.1431 0.2221 0.9172 0.050 Uiso 0.254(5) 1 calc PR B 2 H40D H -0.1134 0.2883 0.8582 0.050 Uiso 0.254(5) 1 calc PR B 2 C39 C -0.1518(2) 0.0690(2) 0.7718(2) 0.0468(7) Uani 1 1 d . B . H39A H -0.2197 0.0700 0.7789 0.056 Uiso 0.50 1 calc PR C 1 H39B H -0.1401 0.0161 0.7921 0.056 Uiso 0.50 1 calc PR C 1 H39C H -0.1764 0.0336 0.8096 0.056 Uiso 0.50 1 d PR C 2 H39D H -0.2082 0.0758 0.7395 0.056 Uiso 0.50 1 d PR C 2 C41 C -0.0106(2) 0.3313(3) 0.9658(2) 0.0530(8) Uani 1 1 d . B . H41A H -0.0402 0.3727 0.9421 0.064 Uiso 0.50 1 calc PR D 1 H41B H -0.0023 0.3611 1.0340 0.064 Uiso 0.50 1 calc PR D 1 H41C H -0.0129 0.3142 1.0181 0.064 Uiso 0.50 1 d PR D 2 H41D H -0.0204 0.3976 0.9821 0.064 Uiso 0.50 1 d PR D 2 C42 C 0.1633(3) 0.3565(3) 1.02208(19) 0.0573(8) Uani 1 1 d . B . H42A H 0.1387 0.2962 1.0392 0.069 Uiso 1 1 calc R . . H42B H 0.1774 0.4241 1.0775 0.069 Uiso 1 1 calc R . . C43 C 0.2573(2) 0.3585(3) 0.98942(19) 0.0509(7) Uani 1 1 d . . . H43A H 0.2854 0.4233 0.9787 0.061 Uiso 1 1 calc R B . H43B H 0.3094 0.3618 1.0378 0.061 Uiso 1 1 calc R . . S4 S 0.64158(6) 0.71573(7) 0.80170(5) 0.05206(19) Uani 1 1 d . . . O13 O 0.7069(2) 0.6598(3) 0.7980(2) 0.0900(9) Uani 1 1 d . E . O14 O 0.5494(6) 0.7019(11) 0.8080(7) 0.137(5) Uani 0.50 1 d P E 1 O15 O 0.7176(7) 0.8294(8) 0.8656(6) 0.108(3) Uani 0.50 1 d P E 1 O14B O 0.5390(6) 0.6271(6) 0.7709(6) 0.080(2) Uani 0.50 1 d P E 2 O15B O 0.6492(10) 0.8034(6) 0.8794(5) 0.114(4) Uani 0.50 1 d P E 2 F1 F 0.5769(4) 0.6497(5) 0.6213(4) 0.0896(7) Uani 0.589(4) 1 d P E 1 F2 F 0.6105(4) 0.8138(5) 0.6936(4) 0.0896(7) Uani 0.589(4) 1 d P E 1 F3 F 0.7314(4) 0.7638(4) 0.6742(3) 0.0896(7) Uani 0.589(4) 1 d P E 1 F1B F 0.6311(6) 0.6639(7) 0.6258(6) 0.0896(7) Uani 0.411(4) 1 d P E 2 F2B F 0.5661(6) 0.7820(7) 0.6957(5) 0.0896(7) Uani 0.411(4) 1 d P E 2 F3B F 0.7321(6) 0.8251(6) 0.7267(5) 0.0896(7) Uani 0.411(4) 1 d P E 2 C45 C 0.6440(3) 0.7425(3) 0.7008(3) 0.0597(8) Uani 1 1 d . E . C44 C 0.9507(2) 0.7577(3) 0.8108(2) 0.0489(7) Uani 1 1 d . . . H44A H 0.8766 0.7228 0.8031 0.059 Uiso 1 1 calc R . . H44B H 0.9868 0.7288 0.8447 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.98930(8) 0.89597(8) 0.87702(7) 0.0728(3) Uani 1 1 d . . . Cl2 Cl 0.97575(10) 0.72573(9) 0.70037(6) 0.0813(3) 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 Fe1 0.02002(14) 0.02552(15) 0.01955(14) 0.01198(11) 0.00656(10) 0.01186(11) Ca1 0.0271(2) 0.0243(2) 0.02184(19) 0.01139(16) 0.00941(16) 0.01403(16) S1 0.0355(3) 0.0378(3) 0.0311(3) 0.0161(2) 0.0189(2) 0.0228(2) S2 0.0227(2) 0.0252(2) 0.0274(3) 0.0087(2) 0.00391(19) 0.0128(2) S3 0.0260(3) 0.0241(2) 0.0263(3) 0.0077(2) 0.0049(2) 0.0085(2) O1 0.0398(9) 0.0317(9) 0.0445(10) 0.0161(7) 0.0257(8) 0.0191(7) O2 0.0604(13) 0.0599(13) 0.0337(10) 0.0084(9) 0.0193(9) 0.0307(11) O3 0.0264(8) 0.0370(9) 0.0461(10) 0.0269(8) 0.0039(7) 0.0108(7) O4 0.0378(10) 0.0352(9) 0.0445(10) -0.0016(8) 0.0046(8) 0.0213(8) O5 0.0376(9) 0.0263(8) 0.0287(8) 0.0093(6) 0.0139(7) 0.0085(7) O6 0.0300(9) 0.0345(9) 0.0440(10) 0.0086(8) 0.0005(7) 0.0136(7) O7 0.0326(8) 0.0255(7) 0.0201(7) 0.0112(6) 0.0099(6) 0.0140(6) O8 0.0439(10) 0.0454(10) 0.0349(9) 0.0181(8) 0.0022(8) 0.0194(8) O9 0.0402(10) 0.0346(9) 0.0460(10) 0.0172(8) 0.0092(8) 0.0234(8) O10 0.0445(10) 0.0287(8) 0.0316(8) 0.0082(7) 0.0108(7) 0.0192(7) O11 0.0414(10) 0.0349(9) 0.0293(8) 0.0076(7) 0.0166(7) 0.0058(8) O12 0.0356(9) 0.0494(11) 0.0251(8) 0.0097(8) 0.0124(7) 0.0114(8) N1 0.0238(9) 0.0360(10) 0.0263(9) 0.0188(8) 0.0093(7) 0.0161(8) N2 0.0287(9) 0.0411(11) 0.0346(10) 0.0250(9) 0.0173(8) 0.0230(8) N3 0.0204(8) 0.0342(10) 0.0236(8) 0.0153(7) 0.0060(7) 0.0135(7) N4 0.0371(10) 0.0249(9) 0.0248(9) 0.0111(7) 0.0095(8) 0.0091(8) C1 0.0428(13) 0.0550(15) 0.0350(12) 0.0306(12) 0.0248(11) 0.0322(12) C2 0.0375(13) 0.0647(17) 0.0545(16) 0.0448(14) 0.0315(12) 0.0349(13) C3 0.0447(14) 0.0507(15) 0.0561(16) 0.0391(13) 0.0343(13) 0.0373(13) C4 0.076(2) 0.0612(19) 0.077(2) 0.0432(18) 0.0499(19) 0.0533(18) C5 0.092(3) 0.088(3) 0.114(3) 0.072(3) 0.074(3) 0.081(3) C6 0.061(2) 0.103(3) 0.087(3) 0.072(2) 0.044(2) 0.061(2) C7 0.0496(17) 0.098(3) 0.071(2) 0.063(2) 0.0337(16) 0.0510(18) C8 0.0398(14) 0.0649(18) 0.0497(15) 0.0420(14) 0.0250(12) 0.0354(13) C9 0.123(4) 0.073(3) 0.101(3) 0.013(2) 0.043(3) 0.073(3) C10 0.077(3) 0.169(5) 0.157(5) 0.129(4) 0.074(3) 0.098(3) C11 0.0414(14) 0.0694(19) 0.0392(14) 0.0258(14) 0.0100(11) 0.0334(14) C12 0.0311(12) 0.0550(15) 0.0401(13) 0.0352(12) 0.0138(10) 0.0247(11) C13 0.0285(12) 0.0636(17) 0.0317(12) 0.0310(12) 0.0049(9) 0.0147(11) C14 0.0189(9) 0.0258(10) 0.0246(10) 0.0114(8) 0.0050(7) 0.0097(8) C15 0.0244(10) 0.0309(11) 0.0265(11) 0.0103(9) 0.0018(8) 0.0083(9) C16 0.0195(10) 0.0417(13) 0.0334(12) 0.0204(10) 0.0004(8) 0.0074(9) C17 0.0224(10) 0.0455(13) 0.0442(13) 0.0308(11) 0.0147(9) 0.0170(10) C18 0.0302(12) 0.0384(13) 0.0380(13) 0.0121(10) 0.0136(10) 0.0193(10) C19 0.0232(10) 0.0327(11) 0.0293(11) 0.0079(9) 0.0051(8) 0.0125(9) C20 0.0475(17) 0.063(2) 0.0334(14) -0.0107(13) -0.0126(12) 0.0259(15) C21 0.0278(12) 0.0668(18) 0.0638(18) 0.0429(16) 0.0200(12) 0.0279(13) C22 0.0384(14) 0.0540(17) 0.0338(13) -0.0089(12) -0.0021(11) 0.0245(13) C23 0.0410(14) 0.0401(13) 0.0356(13) 0.0234(11) 0.0112(11) 0.0055(11) C24 0.071(2) 0.0310(13) 0.0373(14) 0.0186(11) 0.0185(13) 0.0101(13) C25 0.0275(11) 0.0239(10) 0.0261(10) 0.0095(8) 0.0039(8) 0.0077(8) C26 0.0293(11) 0.0302(11) 0.0319(11) 0.0145(9) 0.0069(9) 0.0110(9) C27 0.0273(11) 0.0369(13) 0.0403(13) 0.0175(11) 0.0021(10) 0.0090(10) C28 0.0307(12) 0.0322(12) 0.0399(13) 0.0129(10) 0.0015(10) 0.0024(10) C29 0.0416(14) 0.0227(11) 0.0412(14) 0.0096(10) 0.0038(11) 0.0074(10) C30 0.0362(12) 0.0276(11) 0.0349(12) 0.0131(10) 0.0044(10) 0.0118(10) C31 0.0403(14) 0.0360(13) 0.0441(14) 0.0136(11) 0.0033(11) 0.0207(11) C32 0.0438(16) 0.0370(15) 0.0581(19) 0.0075(13) -0.0142(14) -0.0016(12) C33 0.0597(18) 0.0308(13) 0.0552(17) 0.0124(12) -0.0083(14) 0.0209(13) C34 0.0456(15) 0.0650(19) 0.0527(17) 0.0387(15) 0.0069(13) 0.0276(14) C35 0.0436(15) 0.0527(16) 0.0639(18) 0.0336(15) 0.0135(13) 0.0317(13) C36 0.0542(17) 0.0290(12) 0.0538(16) 0.0100(12) 0.0200(13) 0.0237(12) C37 0.048(2) 0.0269(16) 0.0434(19) 0.0080(14) 0.0138(16) 0.0172(15) C38 0.0290(16) 0.0291(16) 0.0375(17) 0.0089(13) 0.0026(13) 0.0092(13) C40 0.0372(19) 0.053(2) 0.0313(19) 0.0183(17) 0.0193(15) 0.0171(17) C37B 0.043(6) 0.034(5) 0.040(6) -0.001(4) 0.017(5) 0.016(5) C38B 0.035(5) 0.025(4) 0.034(5) 0.006(4) 0.006(4) 0.004(4) C40B 0.033(5) 0.054(7) 0.035(6) 0.010(5) 0.014(4) 0.023(5) C39 0.0316(13) 0.0391(14) 0.0546(17) 0.0070(12) 0.0086(12) 0.0114(11) C41 0.0454(16) 0.0586(18) 0.0368(14) 0.0013(13) 0.0218(12) 0.0166(14) C42 0.0573(18) 0.077(2) 0.0231(12) 0.0125(13) 0.0068(12) 0.0201(16) C43 0.0466(16) 0.0596(18) 0.0334(14) 0.0136(13) -0.0001(12) 0.0150(14) S4 0.0507(4) 0.0675(5) 0.0346(3) 0.0127(3) 0.0035(3) 0.0322(4) O13 0.095(2) 0.109(2) 0.116(3) 0.072(2) 0.0434(19) 0.066(2) O14 0.049(5) 0.314(16) 0.100(8) 0.132(10) 0.042(5) 0.073(8) O15 0.106(6) 0.105(6) 0.054(4) -0.008(4) -0.008(4) 0.025(5) O14B 0.043(3) 0.108(5) 0.087(6) 0.066(5) 0.004(3) 0.000(4) O15B 0.230(12) 0.077(5) 0.041(3) 0.008(3) 0.008(6) 0.095(7) F1 0.1026(19) 0.1049(19) 0.0803(13) 0.0549(13) 0.0341(17) 0.0412(18) F2 0.1026(19) 0.1049(19) 0.0803(13) 0.0549(13) 0.0341(17) 0.0412(18) F3 0.1026(19) 0.1049(19) 0.0803(13) 0.0549(13) 0.0341(17) 0.0412(18) F1B 0.1026(19) 0.1049(19) 0.0803(13) 0.0549(13) 0.0341(17) 0.0412(18) F2B 0.1026(19) 0.1049(19) 0.0803(13) 0.0549(13) 0.0341(17) 0.0412(18) F3B 0.1026(19) 0.1049(19) 0.0803(13) 0.0549(13) 0.0341(17) 0.0412(18) C45 0.060(2) 0.0506(18) 0.072(2) 0.0314(17) 0.0180(17) 0.0186(16) C44 0.0465(16) 0.070(2) 0.0448(15) 0.0351(15) 0.0136(12) 0.0269(15) Cl1 0.0727(6) 0.0736(6) 0.0667(5) 0.0233(5) 0.0028(4) 0.0344(5) Cl2 0.1215(9) 0.0937(7) 0.0491(5) 0.0420(5) 0.0322(5) 0.0492(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 Fe1 O7 1.8649(14) . ? Fe1 N3 2.0163(17) . ? Fe1 N2 2.0236(18) . ? Fe1 N4 2.0464(19) . ? Fe1 N1 2.2306(18) . ? Ca1 O7 2.3158(15) . ? Ca1 O1 2.3437(16) . ? Ca1 O3 2.3697(16) . ? Ca1 O9 2.4696(17) . ? Ca1 O11 2.4976(17) . ? Ca1 O10 2.5190(18) . ? Ca1 O8 2.5201(18) . ? Ca1 O12 2.5331(17) . ? S1 O2 1.433(2) . ? S1 O1 1.4523(17) . ? S1 N2 1.582(2) . ? S1 C3 1.807(3) . ? S2 O4 1.4314(18) . ? S2 O3 1.4502(17) . ? S2 N3 1.5935(19) . ? S2 C14 1.788(2) . ? S3 O6 1.4434(18) . ? S3 O5 1.4502(17) . ? S3 N4 1.6017(19) . ? S3 C25 1.788(2) . ? O5 H7 1.880(10) . ? O8 C43 1.423(3) . ? O8 C34 1.433(3) . ? O9 C35 1.423(3) . ? O9 C36 1.435(3) . ? O10 C38B 1.276(10) . ? O10 C37 1.445(4) . ? O10 C38 1.483(4) . ? O10 C37B 1.515(10) . ? O11 C40B 1.301(11) . ? O11 C39 1.417(3) . ? O11 C40 1.431(4) . ? O12 C41 1.434(3) . ? O12 C42 1.440(4) . ? N1 C23 1.473(3) . ? N1 C12 1.473(3) . ? N1 C1 1.479(3) . ? N2 C2 1.478(3) . ? N3 C13 1.476(3) . ? N4 C24 1.481(3) . ? C1 C2 1.516(3) . ? C3 C8 1.395(4) . ? C3 C4 1.412(4) . ? C4 C5 1.433(5) . ? C4 C9 1.509(6) . ? C5 C6 1.360(6) . ? C6 C7 1.361(5) . ? C6 C10 1.504(4) . ? C7 C8 1.401(4) . ? C8 C11 1.503(4) . ? C12 C13 1.513(4) . ? C14 C15 1.406(3) . ? C14 C19 1.409(3) . ? C15 C16 1.397(3) . ? C15 C20 1.510(3) . ? C16 C17 1.378(4) . ? C17 C18 1.382(3) . ? C17 C21 1.509(3) . ? C18 C19 1.390(3) . ? C19 C22 1.504(3) . ? C23 C24 1.515(4) . ? C25 C30 1.409(3) . ? C25 C26 1.414(3) . ? C26 C27 1.388(3) . ? C26 C31 1.507(3) . ? C27 C28 1.388(4) . ? C28 C29 1.378(4) . ? C28 C32 1.507(4) . ? C29 C30 1.402(3) . ? C30 C33 1.510(3) . ? C34 C35 1.482(4) . ? C36 C37B 1.421(12) . ? C36 C37 1.535(5) . ? C38 C39 1.437(5) . ? C40 C41 1.465(5) . ? C38B C39 1.526(10) . ? C40B C41 1.360(12) . ? C42 C43 1.484(4) . ? S4 O14 1.286(8) . ? S4 O15B 1.373(7) . ? S4 O13 1.405(3) . ? S4 O14B 1.499(7) . ? S4 O15 1.531(9) . ? S4 C45 1.802(4) . ? F1 C45 1.418(7) . ? F2 C45 1.304(6) . ? F3 C45 1.341(6) . ? F1B C45 1.257(9) . ? F2B C45 1.407(9) . ? F3B C45 1.332(8) . ? C44 Cl1 1.752(3) . ? C44 Cl2 1.759(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 Fe1 N3 106.18(7) . . ? O7 Fe1 N2 100.87(7) . . ? N3 Fe1 N2 109.27(8) . . ? O7 Fe1 N4 97.14(7) . . ? N3 Fe1 N4 113.94(8) . . ? N2 Fe1 N4 125.71(8) . . ? O7 Fe1 N1 173.58(7) . . ? N3 Fe1 N1 79.88(7) . . ? N2 Fe1 N1 78.73(7) . . ? N4 Fe1 N1 78.17(7) . . ? O7 Ca1 O1 74.59(6) . . ? O7 Ca1 O3 75.21(6) . . ? O1 Ca1 O3 94.35(6) . . ? O7 Ca1 O9 138.83(6) . . ? O1 Ca1 O9 77.20(6) . . ? O3 Ca1 O9 136.65(6) . . ? O7 Ca1 O11 123.95(6) . . ? O1 Ca1 O11 156.53(6) . . ? O3 Ca1 O11 78.80(6) . . ? O9 Ca1 O11 92.33(6) . . ? O7 Ca1 O10 145.13(6) . . ? O1 Ca1 O10 91.06(6) . . ? O3 Ca1 O10 74.41(6) . . ? O9 Ca1 O10 63.50(6) . . ? O11 Ca1 O10 65.50(6) . . ? O7 Ca1 O8 83.41(6) . . ? O1 Ca1 O8 84.86(7) . . ? O3 Ca1 O8 157.98(6) . . ? O9 Ca1 O8 64.66(6) . . ? O11 Ca1 O8 109.83(6) . . ? O10 Ca1 O8 127.58(6) . . ? O7 Ca1 O12 74.73(6) . . ? O1 Ca1 O12 138.95(6) . . ? O3 Ca1 O12 103.44(6) . . ? O9 Ca1 O12 110.64(6) . . ? O11 Ca1 O12 64.36(6) . . ? O10 Ca1 O12 129.15(6) . . ? O8 Ca1 O12 65.10(6) . . ? O2 S1 O1 115.12(12) . . ? O2 S1 N2 111.72(12) . . ? O1 S1 N2 107.34(10) . . ? O2 S1 C3 107.40(13) . . ? O1 S1 C3 106.76(11) . . ? N2 S1 C3 108.21(12) . . ? O4 S2 O3 115.76(12) . . ? O4 S2 N3 111.62(11) . . ? O3 S2 N3 107.84(10) . . ? O4 S2 C14 108.19(10) . . ? O3 S2 C14 105.78(10) . . ? N3 S2 C14 107.19(9) . . ? O6 S3 O5 114.32(11) . . ? O6 S3 N4 111.58(11) . . ? O5 S3 N4 108.95(10) . . ? O6 S3 C25 107.20(10) . . ? O5 S3 C25 106.48(10) . . ? N4 S3 C25 107.99(11) . . ? S1 O1 Ca1 158.06(11) . . ? S2 O3 Ca1 140.99(11) . . ? S3 O5 H7 111.4(9) . . ? Fe1 O7 Ca1 125.27(7) . . ? C43 O8 C34 115.5(2) . . ? C43 O8 Ca1 113.74(16) . . ? C34 O8 Ca1 115.74(16) . . ? C35 O9 C36 113.5(2) . . ? C35 O9 Ca1 116.94(16) . . ? C36 O9 Ca1 113.29(15) . . ? C38B O10 C37 72.6(5) . . ? C38B O10 C38 43.8(5) . . ? C37 O10 C38 108.9(2) . . ? C38B O10 C37B 118.8(7) . . ? C37 O10 C37B 46.4(5) . . ? C38 O10 C37B 144.8(5) . . ? C38B O10 Ca1 114.3(4) . . ? C37 O10 Ca1 120.86(18) . . ? C38 O10 Ca1 113.00(15) . . ? C37B O10 Ca1 102.1(4) . . ? C40B O11 C39 127.2(5) . . ? C40B O11 C40 35.3(6) . . ? C39 O11 C40 115.8(2) . . ? C40B O11 Ca1 111.4(6) . . ? C39 O11 Ca1 119.13(15) . . ? C40 O11 Ca1 121.60(18) . . ? C41 O12 C42 113.7(2) . . ? C41 O12 Ca1 115.58(15) . . ? C42 O12 Ca1 118.03(16) . . ? C23 N1 C12 112.69(19) . . ? C23 N1 C1 111.15(19) . . ? C12 N1 C1 111.49(19) . . ? C23 N1 Fe1 106.93(13) . . ? C12 N1 Fe1 105.53(13) . . ? C1 N1 Fe1 108.71(13) . . ? C2 N2 S1 114.10(16) . . ? C2 N2 Fe1 116.43(14) . . ? S1 N2 Fe1 125.19(11) . . ? C13 N3 S2 111.94(15) . . ? C13 N3 Fe1 116.24(14) . . ? S2 N3 Fe1 127.10(10) . . ? C24 N4 S3 110.53(16) . . ? C24 N4 Fe1 118.07(15) . . ? S3 N4 Fe1 127.50(11) . . ? N1 C1 C2 108.99(19) . . ? N2 C2 C1 107.65(18) . . ? C8 C3 C4 120.4(3) . . ? C8 C3 S1 119.64(18) . . ? C4 C3 S1 119.9(3) . . ? C3 C4 C5 115.8(4) . . ? C3 C4 C9 125.5(3) . . ? C5 C4 C9 118.7(3) . . ? C6 C5 C4 124.6(3) . . ? C5 C6 C7 116.9(3) . . ? C5 C6 C10 120.2(4) . . ? C7 C6 C10 122.8(4) . . ? C6 C7 C8 123.2(4) . . ? C3 C8 C7 119.0(3) . . ? C3 C8 C11 124.7(2) . . ? C7 C8 C11 116.3(3) . . ? N1 C12 C13 109.72(19) . . ? N3 C13 C12 108.33(19) . . ? C15 C14 C19 120.26(19) . . ? C15 C14 S2 121.60(16) . . ? C19 C14 S2 118.10(15) . . ? C16 C15 C14 117.8(2) . . ? C16 C15 C20 116.4(2) . . ? C14 C15 C20 125.8(2) . . ? C17 C16 C15 123.1(2) . . ? C16 C17 C18 117.7(2) . . ? C16 C17 C21 121.0(2) . . ? C18 C17 C21 121.2(2) . . ? C17 C18 C19 122.4(2) . . ? C18 C19 C14 118.6(2) . . ? C18 C19 C22 117.3(2) . . ? C14 C19 C22 124.0(2) . . ? N1 C23 C24 110.0(2) . . ? N4 C24 C23 108.0(2) . . ? C30 C25 C26 120.7(2) . . ? C30 C25 S3 121.69(17) . . ? C26 C25 S3 117.42(16) . . ? C27 C26 C25 118.1(2) . . ? C27 C26 C31 118.0(2) . . ? C25 C26 C31 123.9(2) . . ? C28 C27 C26 122.4(2) . . ? C29 C28 C27 118.1(2) . . ? C29 C28 C32 121.5(3) . . ? C27 C28 C32 120.4(2) . . ? C28 C29 C30 122.6(2) . . ? C29 C30 C25 117.6(2) . . ? C29 C30 C33 116.0(2) . . ? C25 C30 C33 126.4(2) . . ? O8 C34 C35 106.4(2) . . ? O9 C35 C34 107.0(2) . . ? C37B C36 O9 115.3(4) . . ? C37B C36 C37 46.3(5) . . ? O9 C36 C37 105.7(2) . . ? O10 C37 C36 105.3(3) . . ? C39 C38 O10 109.9(2) . . ? O11 C40 C41 107.9(3) . . ? C36 C37B O10 107.7(7) . . ? C36 C37B Ca1 81.8(4) . . ? O10 C37B Ca1 50.3(3) . . ? O10 C38B C39 116.9(7) . . ? O11 C40B C41 123.2(8) . . ? O11 C40B Ca1 46.4(4) . . ? C41 C40B Ca1 86.5(5) . . ? O11 C39 C38 111.1(3) . . ? O11 C39 C38B 109.7(4) . . ? C38 C39 C38B 41.2(4) . . ? C40B C41 O12 112.0(5) . . ? C40B C41 C40 34.2(6) . . ? O12 C41 C40 112.8(3) . . ? O12 C42 C43 107.5(2) . . ? O8 C43 C42 110.4(2) . . ? O14 S4 O15B 74.6(7) . . ? O14 S4 O13 137.3(6) . . ? O15B S4 O13 123.5(4) . . ? O14 S4 O14B 40.2(6) . . ? O15B S4 O14B 111.7(6) . . ? O13 S4 O14B 101.4(4) . . ? O14 S4 O15 112.9(7) . . ? O15B S4 O15 40.3(5) . . ? O13 S4 O15 99.3(4) . . ? O14B S4 O15 151.9(5) . . ? O14 S4 C45 102.3(4) . . ? O15B S4 C45 112.2(4) . . ? O13 S4 C45 104.06(18) . . ? O14B S4 C45 101.3(4) . . ? O15 S4 C45 91.8(4) . . ? F1B C45 F2 116.0(5) . . ? F1B C45 F3B 114.9(5) . . ? F2 C45 F3B 80.0(4) . . ? F1B C45 F3 73.0(4) . . ? F2 C45 F3 103.3(4) . . ? F3B C45 F3 42.4(3) . . ? F1B C45 F2B 111.1(6) . . ? F2 C45 F2B 28.3(3) . . ? F3B C45 F2B 106.7(5) . . ? F3 C45 F2B 130.3(4) . . ? F1B C45 F1 30.6(4) . . ? F2 C45 F1 100.4(4) . . ? F3B C45 F1 141.4(5) . . ? F3 C45 F1 102.0(4) . . ? F2B C45 F1 85.2(4) . . ? F1B C45 S4 115.6(4) . . ? F2 C45 S4 120.2(3) . . ? F3B C45 S4 103.5(4) . . ? F3 C45 S4 118.9(3) . . ? F2B C45 S4 104.0(4) . . ? F1 C45 S4 109.1(3) . . ? Cl1 C44 Cl2 112.43(17) . . ? _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.056 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.065 _iucr_refine_instructions_details ; TITL asb189 in P-1 CELL 0.71073 14.2376 14.5557 16.0245 112.0349 96.1392 107.9824 ZERR 2.00 0.0005 0.0005 0.0006 0.0004 0.0004 0.0004 LATT 1 SFAC C H N O F S CL CA FE UNIT 90 136 8 30 6 8 4 2 2 TEMP -100.000 SIZE 0.178 0.227 0.331 rem Young Jun Park 20s CCD1 rem APEX2 2010.9-0, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 CONN 8 CA1 CONN 5 FE1 EADP F1 > F3B OMIT 0 -1 1 OMIT 0 0 1 SHEL 100 0.76 DFIX 0.85 0.001 O7 H7 BIND O5 H7 L.S. 12 ACTA 51 WGHT 0.056400 2.869300 FVAR 0.10246 0.74636 0.58941 FE1 9 0.199194 0.451784 0.716377 11.00000 0.02002 0.02552 = 0.01955 0.01198 0.00656 0.01186 CA1 8 0.086241 0.229961 0.782095 11.00000 0.02712 0.02432 = 0.02184 0.01139 0.00941 0.01403 S1 6 0.267354 0.252152 0.632185 11.00000 0.03548 0.03783 = 0.03107 0.01612 0.01887 0.02275 S2 6 -0.033458 0.287404 0.607365 11.00000 0.02269 0.02521 = 0.02742 0.00870 0.00391 0.01282 S3 6 0.216505 0.668971 0.893433 11.00000 0.02604 0.02415 = 0.02625 0.00771 0.00486 0.00852 O1 4 0.198485 0.218994 0.685188 11.00000 0.03976 0.03175 = 0.04454 0.01606 0.02566 0.01909 O2 4 0.233679 0.187701 0.533605 11.00000 0.06040 0.05989 = 0.03366 0.00843 0.01934 0.03071 O3 4 -0.023599 0.268714 0.690036 11.00000 0.02639 0.03702 = 0.04613 0.02695 0.00391 0.01082 O4 4 -0.046551 0.198737 0.521823 11.00000 0.03783 0.03523 = 0.04445 -0.00159 0.00459 0.02128 O5 4 0.189217 0.595861 0.936228 11.00000 0.03763 0.02629 = 0.02868 0.00929 0.01393 0.00854 O6 4 0.139105 0.709153 0.876470 11.00000 0.02996 0.03446 = 0.04405 0.00863 0.00052 0.01362 O7 4 0.176395 0.404836 0.808568 11.00000 0.03264 0.02548 = 0.02010 0.01120 0.00994 0.01399 H7 2 0.175302 0.457021 0.855389 11.00000 0.04927 O8 4 0.235565 0.265491 0.905468 11.00000 0.04386 0.04536 = 0.03489 0.01809 0.00216 0.01942 O9 4 0.120124 0.070410 0.772934 11.00000 0.04024 0.03462 = 0.04601 0.01715 0.00919 0.02340 O10 4 -0.044840 0.051021 0.666137 11.00000 0.04451 0.02871 = 0.03164 0.00818 0.01076 0.01918 O11 4 -0.075741 0.171751 0.828862 11.00000 0.04143 0.03490 = 0.02935 0.00758 0.01658 0.00584 O12 4 0.087714 0.343945 0.947055 11.00000 0.03556 0.04943 = 0.02511 0.00975 0.01238 0.01137 N1 3 0.242599 0.522192 0.617559 11.00000 0.02383 0.03597 = 0.02632 0.01875 0.00934 0.01606 N2 3 0.287742 0.373834 0.657809 11.00000 0.02875 0.04109 = 0.03458 0.02504 0.01727 0.02302 N3 3 0.062462 0.390889 0.625172 11.00000 0.02045 0.03421 = 0.02357 0.01532 0.00605 0.01346 N4 3 0.247998 0.612306 0.800070 11.00000 0.03706 0.02494 = 0.02483 0.01115 0.00955 0.00910 C1 1 0.286192 0.455544 0.551549 11.00000 0.04283 0.05501 = 0.03503 0.03056 0.02479 0.03219 AFIX 23 H1B 2 0.329451 0.497966 0.524139 11.00000 -1.20000 H1C 2 0.230600 0.393241 0.500471 11.00000 -1.20000 AFIX 0 C2 1 0.349589 0.417426 0.603058 11.00000 0.03751 0.06474 = 0.05453 0.04477 0.03150 0.03495 AFIX 23 H2A 2 0.367841 0.361327 0.558304 11.00000 -1.20000 H2B 2 0.413344 0.477776 0.644821 11.00000 -1.20000 AFIX 0 C3 1 0.386173 0.243159 0.672760 11.00000 0.04473 0.05068 = 0.05615 0.03907 0.03430 0.03728 C4 1 0.413622 0.159519 0.616395 11.00000 0.07621 0.06124 = 0.07745 0.04316 0.04994 0.05328 C5 1 0.510058 0.160365 0.653764 11.00000 0.09209 0.08753 = 0.11443 0.07249 0.07443 0.08055 AFIX 43 H5B 2 0.529900 0.104182 0.618015 11.00000 -1.20000 AFIX 0 C6 1 0.575184 0.235945 0.736812 11.00000 0.06115 0.10259 = 0.08680 0.07158 0.04439 0.06129 C7 1 0.543663 0.313277 0.788874 11.00000 0.04964 0.09849 = 0.07096 0.06335 0.03367 0.05098 AFIX 43 H7B 2 0.587376 0.366169 0.847685 11.00000 -1.20000 AFIX 0 C8 1 0.449922 0.318715 0.760001 11.00000 0.03980 0.06495 = 0.04971 0.04201 0.02498 0.03536 C9 1 0.350822 0.072187 0.521779 11.00000 0.12305 0.07284 = 0.10073 0.01311 0.04296 0.07289 AFIX 137 H9A 2 0.279832 0.042415 0.524099 11.00000 -1.50000 H9B 2 0.378155 0.015450 0.503732 11.00000 -1.50000 H9C 2 0.353686 0.101968 0.476050 11.00000 -1.50000 AFIX 0 C10 1 0.675490 0.230076 0.768900 11.00000 0.07687 0.16862 = 0.15700 0.12910 0.07353 0.09832 AFIX 137 H10A 2 0.710178 0.218773 0.718447 11.00000 -1.50000 H10B 2 0.663305 0.170411 0.786266 11.00000 -1.50000 H10C 2 0.718339 0.297218 0.822894 11.00000 -1.50000 AFIX 0 C11 1 0.426412 0.408427 0.826688 11.00000 0.04135 0.06937 = 0.03918 0.02579 0.00999 0.03336 AFIX 137 H11A 2 0.468202 0.434229 0.889576 11.00000 -1.50000 H11B 2 0.353999 0.382422 0.826079 11.00000 -1.50000 H11C 2 0.441703 0.467130 0.807897 11.00000 -1.50000 AFIX 0 C12 1 0.147193 0.520221 0.569686 11.00000 0.03110 0.05500 = 0.04006 0.03515 0.01379 0.02469 AFIX 23 H12A 2 0.156463 0.531028 0.513230 11.00000 -1.20000 H12B 2 0.129540 0.579020 0.611242 11.00000 -1.20000 AFIX 0 C13 1 0.061804 0.413774 0.542881 11.00000 0.02855 0.06362 = 0.03167 0.03104 0.00493 0.01470 AFIX 23 H13A 2 -0.004605 0.416816 0.521642 11.00000 -1.20000 H13B 2 0.071933 0.356460 0.491432 11.00000 -1.20000 AFIX 0 C14 1 -0.143987 0.320566 0.599276 11.00000 0.01888 0.02580 = 0.02457 0.01143 0.00499 0.00966 C15 1 -0.227127 0.260753 0.520355 11.00000 0.02441 0.03088 = 0.02645 0.01027 0.00179 0.00830 C16 1 -0.313597 0.286916 0.522815 11.00000 0.01951 0.04169 = 0.03342 0.02043 0.00039 0.00735 AFIX 43 H16A 2 -0.371359 0.244857 0.470982 11.00000 -1.20000 AFIX 0 C17 1 -0.319038 0.370869 0.596900 11.00000 0.02240 0.04548 = 0.04423 0.03077 0.01475 0.01696 C18 1 -0.234601 0.430804 0.672032 11.00000 0.03016 0.03841 = 0.03801 0.01209 0.01361 0.01935 AFIX 43 H18A 2 -0.236213 0.490482 0.722769 11.00000 -1.20000 AFIX 0 C19 1 -0.147440 0.406921 0.676033 11.00000 0.02324 0.03265 = 0.02929 0.00789 0.00512 0.01253 C20 1 -0.230281 0.172625 0.430689 11.00000 0.04753 0.06296 = 0.03340 -0.01068 -0.01260 0.02586 AFIX 137 H20A 2 -0.174877 0.200804 0.404804 11.00000 -1.50000 H20B 2 -0.295985 0.145741 0.386070 11.00000 -1.50000 H20C 2 -0.222029 0.114131 0.442994 11.00000 -1.50000 AFIX 0 C21 1 -0.414100 0.396302 0.595892 11.00000 0.02783 0.06677 = 0.06377 0.04287 0.02004 0.02789 AFIX 137 H21A 2 -0.448025 0.376783 0.531752 11.00000 -1.50000 H21B 2 -0.395499 0.473087 0.633544 11.00000 -1.50000 H21C 2 -0.460495 0.355549 0.621727 11.00000 -1.50000 AFIX 0 C22 1 -0.061812 0.476246 0.762796 11.00000 0.03844 0.05400 = 0.03384 -0.00894 -0.00214 0.02448 AFIX 137 H22A 2 -0.084655 0.524637 0.809525 11.00000 -1.50000 H22B 2 -0.003346 0.518358 0.748038 11.00000 -1.50000 H22C 2 -0.041648 0.430908 0.787351 11.00000 -1.50000 AFIX 0 C23 1 0.318497 0.631719 0.673654 11.00000 0.04098 0.04011 = 0.03565 0.02338 0.01121 0.00549 AFIX 23 H23A 2 0.326638 0.672399 0.635582 11.00000 -1.20000 H23B 2 0.385371 0.628925 0.693758 11.00000 -1.20000 AFIX 0 C24 1 0.284264 0.687661 0.758257 11.00000 0.07064 0.03101 = 0.03727 0.01856 0.01846 0.01012 AFIX 23 H24A 2 0.341848 0.753013 0.803897 11.00000 -1.20000 H24B 2 0.228546 0.708795 0.739809 11.00000 -1.20000 AFIX 0 C25 1 0.326759 0.781525 0.973323 11.00000 0.02745 0.02391 = 0.02611 0.00952 0.00390 0.00765 C26 1 0.408458 0.760502 1.009870 11.00000 0.02929 0.03024 = 0.03191 0.01447 0.00695 0.01097 C27 1 0.485342 0.844200 1.085018 11.00000 0.02729 0.03693 = 0.04026 0.01755 0.00210 0.00903 AFIX 43 H27A 2 0.540164 0.830747 1.110655 11.00000 -1.20000 AFIX 0 C28 1 0.485048 0.946818 1.124071 11.00000 0.03069 0.03216 = 0.03987 0.01291 0.00147 0.00245 C29 1 0.409469 0.967185 1.081675 11.00000 0.04160 0.02265 = 0.04120 0.00958 0.00381 0.00744 AFIX 43 H29A 2 0.411753 1.038452 1.104968 11.00000 -1.20000 AFIX 0 C30 1 0.329340 0.886875 1.005524 11.00000 0.03616 0.02756 = 0.03491 0.01309 0.00437 0.01184 C31 1 0.419110 0.653637 0.969744 11.00000 0.04028 0.03597 = 0.04414 0.01362 0.00327 0.02074 AFIX 137 H31A 2 0.359783 0.598789 0.971738 11.00000 -1.50000 H31B 2 0.481361 0.657891 1.006303 11.00000 -1.50000 H31C 2 0.423112 0.634752 0.905104 11.00000 -1.50000 AFIX 0 C32 1 0.565645 1.032829 1.210340 11.00000 0.04384 0.03695 = 0.05807 0.00747 -0.01421 -0.00162 AFIX 137 H32A 2 0.574120 1.004199 1.255852 11.00000 -1.50000 H32B 2 0.544760 1.093620 1.237128 11.00000 -1.50000 H32C 2 0.630474 1.056610 1.194151 11.00000 -1.50000 AFIX 0 C33 1 0.254914 0.923178 0.964989 11.00000 0.05967 0.03081 = 0.05521 0.01240 -0.00828 0.02095 AFIX 137 H33A 2 0.285483 1.000866 0.986046 11.00000 -1.50000 H33B 2 0.192232 0.904916 0.985704 11.00000 -1.50000 H33C 2 0.238725 0.887313 0.896909 11.00000 -1.50000 AFIX 0 C34 1 0.239994 0.173674 0.916709 11.00000 0.04556 0.06502 = 0.05268 0.03867 0.00686 0.02758 AFIX 23 H34A 2 0.188518 0.150507 0.949089 11.00000 -1.20000 H34B 2 0.308429 0.190476 0.953622 11.00000 -1.20000 AFIX 0 C35 1 0.218487 0.088477 0.821751 11.00000 0.04357 0.05268 = 0.06394 0.03357 0.01351 0.03172 AFIX 23 H35A 2 0.270609 0.111396 0.789827 11.00000 -1.20000 H35B 2 0.219405 0.022043 0.824753 11.00000 -1.20000 AFIX 0 C36 1 0.086398 -0.014390 0.680432 11.00000 0.05422 0.02895 = 0.05383 0.01005 0.02003 0.02369 AFIX 23 PART 1 H36A 2 0.103306 -0.075733 0.679623 10.50000 -1.20000 H36B 2 0.119242 0.010806 0.637450 10.50000 -1.20000 PART 2 H36C 2 0.145267 -0.019940 0.658072 10.50000 -1.20000 H36D 2 0.051168 -0.080350 0.683662 10.50000 -1.20000 AFIX 0 PART 1 C37 1 -0.029673 -0.046962 0.651911 21.00000 0.04796 0.02687 = 0.04342 0.00801 0.01385 0.01721 AFIX 23 H37A 2 -0.057985 -0.099693 0.585856 21.00000 -1.20000 H37B 2 -0.063262 -0.078840 0.690949 21.00000 -1.20000 AFIX 0 C38 1 -0.150208 0.037131 0.675705 21.00000 0.02902 0.02910 = 0.03749 0.00887 0.00258 0.00915 AFIX 23 H38A 2 -0.175031 0.081184 0.651693 21.00000 -1.20000 H38B 2 -0.196140 -0.038795 0.638596 21.00000 -1.20000 AFIX 0 C40 1 -0.081481 0.219212 0.923202 21.00000 0.03723 0.05313 = 0.03125 0.01825 0.01932 0.01711 AFIX 23 H40A 2 -0.062601 0.180757 0.957514 21.00000 -1.20000 H40B 2 -0.151891 0.215062 0.925112 21.00000 -1.20000 AFIX 0 PART 2 C37B 1 0.020630 -0.003072 0.614927 -21.00000 0.04294 0.03447 = 0.03958 -0.00149 0.01691 0.01574 AFIX 23 H37C 2 -0.022956 -0.074197 0.564333 -21.00000 -1.20000 H37D 2 0.061232 0.040847 0.587202 -21.00000 -1.20000 AFIX 0 C38B 1 -0.107183 0.002386 0.701379 -21.00000 0.03467 0.02506 = 0.03449 0.00623 0.00604 0.00427 AFIX 23 H38C 2 -0.071910 -0.029877 0.732040 -21.00000 -1.20000 H38D 2 -0.164516 -0.057107 0.649909 -21.00000 -1.20000 AFIX 0 C40B 1 -0.087451 0.252550 0.891613 -21.00000 0.03286 0.05374 = 0.03526 0.01022 0.01434 0.02315 AFIX 23 H40C 2 -0.143074 0.222098 0.917165 -21.00000 -1.20000 H40D 2 -0.113430 0.288292 0.858178 -21.00000 -1.20000 AFIX 0 PART 0 C39 1 -0.151772 0.068963 0.771837 11.00000 0.03158 0.03913 = 0.05459 0.00697 0.00860 0.01137 AFIX 23 PART 1 H39A 2 -0.219712 0.070007 0.778927 10.50000 -1.20000 H39B 2 -0.140114 0.016109 0.792125 10.50000 -1.20000 PART 2 H39C 2 -0.176392 0.033633 0.809607 10.50000 -1.20000 H39D 2 -0.208182 0.075763 0.739517 10.50000 -1.20000 AFIX 0 PART 0 C41 1 -0.010607 0.331252 0.965826 11.00000 0.04543 0.05857 = 0.03679 0.00129 0.02183 0.01664 AFIX 23 PART 1 H41A 2 -0.040197 0.372690 0.942124 10.50000 -1.20000 H41B 2 -0.002272 0.361089 1.033983 10.50000 -1.20000 PART 2 H41C 2 -0.012907 0.314222 1.018126 10.50000 -1.20000 H41D 2 -0.020387 0.397572 0.982066 10.50000 -1.20000 AFIX 0 PART 0 C42 1 0.163345 0.356512 1.022083 11.00000 0.05734 0.07747 = 0.02307 0.01252 0.00677 0.02013 AFIX 23 H42A 2 0.138659 0.296168 1.039155 11.00000 -1.20000 H42B 2 0.177441 0.424053 1.077484 11.00000 -1.20000 AFIX 0 C43 1 0.257340 0.358539 0.989422 11.00000 0.04662 0.05961 = 0.03341 0.01357 -0.00012 0.01497 AFIX 23 H43A 2 0.285359 0.423271 0.978721 11.00000 -1.20000 H43B 2 0.309378 0.361772 1.037788 11.00000 -1.20000 AFIX 0 S4 6 0.641580 0.715730 0.801702 11.00000 0.05071 0.06752 = 0.03462 0.01265 0.00350 0.03224 O13 4 0.706918 0.659832 0.797968 11.00000 0.09456 0.10862 = 0.11623 0.07238 0.04340 0.06628 PART 1 O14 4 0.549363 0.701884 0.808016 10.50000 0.04910 0.31421 = 0.09971 0.13236 0.04163 0.07257 O15 4 0.717612 0.829412 0.865623 10.50000 0.10569 0.10468 = 0.05393 -0.00786 -0.00790 0.02544 PART 2 O14B 4 0.538961 0.627053 0.770897 10.50000 0.04340 0.10751 = 0.08667 0.06555 0.00421 0.00000 O15B 4 0.649203 0.803389 0.879449 10.50000 0.23037 0.07701 = 0.04060 0.00812 0.00766 0.09528 PART 1 F1 5 0.576902 0.649714 0.621309 31.00000 0.10263 0.10486 = 0.08031 0.05486 0.03406 0.04121 F2 5 0.610512 0.813825 0.693646 31.00000 0.10263 0.10486 = 0.08031 0.05486 0.03406 0.04121 F3 5 0.731387 0.763806 0.674182 31.00000 0.10263 0.10486 = 0.08031 0.05486 0.03406 0.04121 PART 2 F1B 5 0.631075 0.663858 0.625756 -31.00000 0.10263 0.10486 = 0.08031 0.05486 0.03406 0.04121 F2B 5 0.566056 0.782032 0.695656 -31.00000 0.10263 0.10486 = 0.08031 0.05486 0.03406 0.04121 F3B 5 0.732139 0.825057 0.726718 -31.00000 0.10263 0.10486 = 0.08031 0.05486 0.03406 0.04121 PART 0 C45 1 0.644024 0.742513 0.700758 11.00000 0.05988 0.05056 = 0.07206 0.03138 0.01799 0.01865 C44 1 0.950703 0.757673 0.810779 11.00000 0.04646 0.06999 = 0.04477 0.03510 0.01359 0.02693 AFIX 23 H44A 2 0.876607 0.722826 0.803059 11.00000 -1.20000 H44B 2 0.986779 0.728810 0.844674 11.00000 -1.20000 AFIX 0 CL1 7 0.989302 0.895975 0.877020 11.00000 0.07271 0.07359 = 0.06672 0.02330 0.00281 0.03443 CL2 7 0.975747 0.725731 0.700365 11.00000 0.12154 0.09365 = 0.04910 0.04201 0.03220 0.04923 HKLF 4 REM asb189 in P-1 REM R1 = 0.0443 for 11334 Fo > 4sig(Fo) and 0.0520 for all 13241 data REM 733 parameters refined using 1 restraints END WGHT 0.0564 2.8703 REM Highest difference peak 1.056, deepest hole -0.803, 1-sigma level 0.065 Q1 1 0.6993 0.6885 0.6548 11.00000 0.05 1.06 Q2 1 0.6664 0.7775 0.8054 11.00000 0.05 0.69 Q3 1 0.7203 0.8622 0.7679 11.00000 0.05 0.64 Q4 1 0.6209 0.6177 0.7808 11.00000 0.05 0.63 Q5 1 0.7151 0.8063 0.6767 11.00000 0.05 0.61 Q6 1 0.2197 0.3210 1.0192 11.00000 0.05 0.58 Q7 1 0.6646 0.8358 0.6863 11.00000 0.05 0.56 Q8 1 0.7624 0.7987 0.7183 11.00000 0.05 0.53 Q9 1 0.4622 0.1142 0.6015 11.00000 0.05 0.50 Q10 1 0.6380 0.7376 0.7561 11.00000 0.05 0.47 Q11 1 0.6358 0.1632 0.7107 11.00000 0.05 0.47 Q12 1 0.1892 0.4159 1.0102 11.00000 0.05 0.46 Q13 1 0.5143 0.2585 0.7447 11.00000 0.05 0.45 Q14 1 0.3630 0.1182 0.5695 11.00000 0.05 0.45 Q15 1 0.7228 0.7320 0.8506 11.00000 0.05 0.43 Q16 1 0.2267 0.2266 0.5863 11.00000 0.05 0.42 Q17 1 0.2805 0.3182 0.6498 11.00000 0.05 0.40 Q18 1 0.3001 0.0491 0.4756 11.00000 0.05 0.37 Q19 1 0.4212 0.3549 0.7886 11.00000 0.05 0.35 Q20 1 0.1973 0.1910 0.5113 11.00000 0.05 0.34 ; data_asb247 _database_code_depnum_ccdc_archive 'CCDC 895608' #TrackingRef '13191_web_deposit_cif_file_0_NathanielS.Sickerman_1344538304.SuperCif.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H68 Cl2 F3 Fe N4 O15 S4 Sr' _chemical_formula_weight 1304.64 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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 8.7949(3) _cell_length_b 28.7099(11) _cell_length_c 22.4440(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.6131(5) _cell_angle_gamma 90.00 _cell_volume 5603.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9843 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.53 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2700 _exptl_absorpt_coefficient_mu 1.532 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6440 _exptl_absorpt_correction_T_max 0.8257 _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 64317 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.10 _reflns_number_total 12345 _reflns_number_gt 10487 _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^)+(0.0649P)^2^+13.2397P] 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 12345 _refine_ls_number_parameters 675 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.45000(5) 0.089917(14) 0.849387(19) 0.01526(10) Uani 1 1 d . . . Sr1 Sr 0.49841(3) 0.079020(10) 0.682789(12) 0.01875(8) Uani 1 1 d . A . O1 O 0.3351(3) 0.14250(8) 0.71999(10) 0.0248(5) Uani 1 1 d . A . O2 O 0.0954(3) 0.16119(8) 0.75701(13) 0.0319(6) Uani 1 1 d . A . O3 O 0.4200(3) 0.00790(8) 0.73884(10) 0.0258(5) Uani 1 1 d . A . O4 O 0.1414(3) 0.00590(8) 0.73371(11) 0.0283(5) Uani 1 1 d . A . O5 O 0.8376(2) 0.08490(8) 0.87438(10) 0.0216(5) Uani 1 1 d . . . O6 O 0.8321(3) 0.03464(8) 0.96189(10) 0.0237(5) Uani 1 1 d . . . O7 O 0.5834(2) 0.08885(8) 0.79176(10) 0.0216(5) Uani 1 1 d D A . H7 H 0.6770(15) 0.0898(15) 0.8081(18) 0.040(12) Uiso 1 1 d D . . N1 N 0.3002(3) 0.09420(9) 0.92380(11) 0.0174(5) Uani 1 1 d . . . N2 N 0.3422(3) 0.15085(9) 0.82913(12) 0.0200(5) Uani 1 1 d . A . N3 N 0.3056(3) 0.03643(9) 0.82642(11) 0.0186(5) Uani 1 1 d . A . N4 N 0.6054(3) 0.08568(9) 0.92544(11) 0.0177(5) Uani 1 1 d . . . S1 S 0.25970(9) 0.16670(3) 0.76446(4) 0.02049(16) Uani 1 1 d . . . S2 S 0.28909(9) 0.00157(3) 0.77068(3) 0.02046(16) Uani 1 1 d . . . S3 S 0.78845(8) 0.07822(3) 0.93262(3) 0.01697(15) Uani 1 1 d . . . C1 C 0.1922(4) 0.13389(11) 0.90939(15) 0.0219(6) Uani 1 1 d . A . H1A H 0.1591 0.1460 0.9467 0.026 Uiso 1 1 calc R . . H1B H 0.0998 0.1235 0.8818 0.026 Uiso 1 1 calc R . . C2 C 0.2743(4) 0.17135(11) 0.87990(15) 0.0243(7) Uani 1 1 d . . . H2A H 0.2011 0.1964 0.8648 0.029 Uiso 1 1 calc R A . H2B H 0.3565 0.1851 0.9097 0.029 Uiso 1 1 calc R . . C3 C 0.3000(4) 0.22789(10) 0.76163(14) 0.0193(6) Uani 1 1 d . A . C4 C 0.1849(4) 0.26125(11) 0.76672(15) 0.0236(7) Uani 1 1 d . . . C5 C 0.2313(4) 0.30785(12) 0.77427(15) 0.0271(7) Uani 1 1 d . A . H5A H 0.1554 0.3308 0.7780 0.033 Uiso 1 1 calc R . . C6 C 0.3820(4) 0.32201(11) 0.77650(15) 0.0282(7) Uani 1 1 d . . . C7 C 0.4907(4) 0.28866(12) 0.76834(14) 0.0255(7) Uani 1 1 d . A . H7A H 0.5938 0.2982 0.7677 0.031 Uiso 1 1 calc R . . C8 C 0.4542(4) 0.24153(11) 0.76106(14) 0.0218(6) Uani 1 1 d . . . C9 C 0.0152(4) 0.25172(13) 0.76522(18) 0.0321(8) Uani 1 1 d . A . H9A H 0.0007 0.2311 0.7987 0.048 Uiso 1 1 calc R . . H9B H -0.0260 0.2367 0.7270 0.048 Uiso 1 1 calc R . . H9C H -0.0390 0.2811 0.7690 0.048 Uiso 1 1 calc R . . C10 C 0.4285(5) 0.37190(12) 0.79072(19) 0.0392(9) Uani 1 1 d . A . H10A H 0.3469 0.3928 0.7721 0.059 Uiso 1 1 calc R . . H10B H 0.5239 0.3788 0.7748 0.059 Uiso 1 1 calc R . . H10C H 0.4448 0.3765 0.8345 0.059 Uiso 1 1 calc R . . C11 C 0.5820(4) 0.20838(12) 0.75336(16) 0.0267(7) Uani 1 1 d . A . H11A H 0.6810 0.2245 0.7626 0.040 Uiso 1 1 calc R . . H11B H 0.5685 0.1971 0.7117 0.040 Uiso 1 1 calc R . . H11C H 0.5798 0.1819 0.7808 0.040 Uiso 1 1 calc R . . C12 C 0.2179(4) 0.04905(11) 0.92260(14) 0.0203(6) Uani 1 1 d . A . H12A H 0.1267 0.0522 0.9434 0.024 Uiso 1 1 calc R . . H12B H 0.2864 0.0250 0.9438 0.024 Uiso 1 1 calc R . . C13 C 0.1683(3) 0.03468(11) 0.85786(14) 0.0207(6) Uani 1 1 d . . . H13A H 0.1255 0.0027 0.8562 0.025 Uiso 1 1 calc R A . H13B H 0.0878 0.0561 0.8382 0.025 Uiso 1 1 calc R . . C14 C 0.3037(4) -0.05581(10) 0.80193(14) 0.0215(6) Uani 1 1 d . A . C15 C 0.1749(4) -0.08586(11) 0.79544(15) 0.0250(7) Uani 1 1 d . . . C16 C 0.1972(4) -0.13074(12) 0.81954(15) 0.0287(7) Uani 1 1 d . A . H16A H 0.1125 -0.1516 0.8150 0.034 Uiso 1 1 calc R . . C17 C 0.3357(5) -0.14600(12) 0.84941(15) 0.0302(8) Uani 1 1 d . . . C18 C 0.4583(4) -0.11516(12) 0.85657(15) 0.0298(8) Uani 1 1 d . A . H18A H 0.5541 -0.1252 0.8779 0.036 Uiso 1 1 calc R . . C19 C 0.4465(4) -0.06994(12) 0.83373(15) 0.0255(7) Uani 1 1 d . . . C20 C 0.0129(4) -0.07400(13) 0.76620(17) 0.0326(8) Uani 1 1 d . A . H20A H -0.0569 -0.0993 0.7734 0.049 Uiso 1 1 calc R . . H20B H 0.0109 -0.0700 0.7227 0.049 Uiso 1 1 calc R . . H20C H -0.0200 -0.0450 0.7835 0.049 Uiso 1 1 calc R . . C21 C 0.3522(6) -0.19453(13) 0.87574(19) 0.0448(11) Uani 1 1 d . A . H21A H 0.3035 -0.2170 0.8460 0.067 Uiso 1 1 calc R . . H21B H 0.3024 -0.1959 0.9119 0.067 Uiso 1 1 calc R . . H21C H 0.4616 -0.2021 0.8864 0.067 Uiso 1 1 calc R . . C22 C 0.5880(4) -0.03927(13) 0.84488(18) 0.0335(8) Uani 1 1 d . A . H22A H 0.6163 -0.0294 0.8062 0.050 Uiso 1 1 calc R . . H22B H 0.6733 -0.0568 0.8676 0.050 Uiso 1 1 calc R . . H22C H 0.5661 -0.0118 0.8681 0.050 Uiso 1 1 calc R . . C23 C 0.3988(4) 0.10171(12) 0.98198(14) 0.0233(7) Uani 1 1 d . . . H23A H 0.3456 0.0906 1.0152 0.028 Uiso 1 1 calc R . . H23B H 0.4200 0.1354 0.9880 0.028 Uiso 1 1 calc R . . C24 C 0.5486(4) 0.07552(12) 0.98293(14) 0.0227(7) Uani 1 1 d . . . H24A H 0.6246 0.0859 1.0174 0.027 Uiso 1 1 calc R . . H24B H 0.5316 0.0416 0.9869 0.027 Uiso 1 1 calc R . . C25 C 0.8747(3) 0.12449(10) 0.98013(13) 0.0165(6) Uani 1 1 d . . . C26 C 0.8594(3) 0.17066(11) 0.95740(14) 0.0197(6) Uani 1 1 d . . . C27 C 0.9323(4) 0.20660(11) 0.99248(15) 0.0241(7) Uani 1 1 d . . . H27A H 0.9202 0.2377 0.9781 0.029 Uiso 1 1 calc R . . C28 C 1.0221(4) 0.19823(12) 1.04785(15) 0.0255(7) Uani 1 1 d . . . C29 C 1.0353(4) 0.15308(12) 1.06873(14) 0.0242(7) Uani 1 1 d . . . H29A H 1.0972 0.1473 1.1064 0.029 Uiso 1 1 calc R . . C30 C 0.9617(3) 0.11521(11) 1.03697(14) 0.0197(6) Uani 1 1 d . . . C31 C 0.7735(4) 0.18355(12) 0.89633(15) 0.0247(7) Uani 1 1 d . . . H31A H 0.7671 0.2175 0.8928 0.037 Uiso 1 1 calc R . . H31B H 0.6695 0.1704 0.8918 0.037 Uiso 1 1 calc R . . H31C H 0.8280 0.1711 0.8648 0.037 Uiso 1 1 calc R . . C32 C 1.1026(5) 0.23805(14) 1.08394(18) 0.0388(9) Uani 1 1 d . . . H32A H 1.1153 0.2304 1.1270 0.058 Uiso 1 1 calc R . . H32B H 1.0407 0.2664 1.0765 0.058 Uiso 1 1 calc R . . H32C H 1.2037 0.2431 1.0717 0.058 Uiso 1 1 calc R . . C33 C 0.9817(4) 0.06821(12) 1.06723(15) 0.0244(7) Uani 1 1 d . . . H33A H 0.8805 0.0545 1.0692 0.037 Uiso 1 1 calc R . . H33B H 1.0378 0.0719 1.1081 0.037 Uiso 1 1 calc R . . H33C H 1.0398 0.0477 1.0440 0.037 Uiso 1 1 calc R . . O8 O 0.7837(4) 0.05019(14) 0.68235(18) 0.0178(9) Uiso 0.526(3) 1 d P A 1 O9 O 0.6945(5) 0.13834(15) 0.64375(19) 0.0226(10) Uiso 0.526(3) 1 d P A 1 O10 O 0.4066(5) 0.12788(17) 0.5850(2) 0.0280(11) Uiso 0.526(3) 1 d P A 1 O11 O 0.2663(6) 0.04782(18) 0.6096(2) 0.0342(12) Uiso 0.526(3) 1 d P A 1 O12 O 0.5452(5) 0.00921(16) 0.6096(2) 0.0273(10) Uiso 0.526(3) 1 d P A 1 C34 C 0.8896(8) 0.0887(3) 0.6931(3) 0.0209(17) Uiso 0.526(3) 1 d P A 1 H34A H 0.9960 0.0772 0.6936 0.025 Uiso 0.526(3) 1 calc PR A 1 H34B H 0.8826 0.1025 0.7330 0.025 Uiso 0.526(3) 1 calc PR A 1 C35 C 0.8553(7) 0.1255(2) 0.6452(3) 0.0238(13) Uiso 0.526(3) 1 d P A 1 H35A H 0.9225 0.1530 0.6551 0.029 Uiso 0.526(3) 1 calc PR A 1 H35B H 0.8726 0.1132 0.6055 0.029 Uiso 0.526(3) 1 calc PR A 1 C36 C 0.6639(12) 0.1496(4) 0.5890(4) 0.054(2) Uiso 0.526(3) 1 d P A 1 H36A H 0.7435 0.1341 0.5693 0.065 Uiso 0.526(3) 1 calc PR A 1 H36B H 0.6865 0.1834 0.5880 0.065 Uiso 0.526(3) 1 calc PR A 1 C37 C 0.5286(14) 0.1439(5) 0.5498(6) 0.075(3) Uiso 0.526(3) 1 d P A 1 H37A H 0.5430 0.1205 0.5186 0.090 Uiso 0.526(3) 1 calc PR A 1 H37B H 0.4978 0.1737 0.5293 0.090 Uiso 0.526(3) 1 calc PR A 1 C38 C 0.2637(13) 0.1182(4) 0.5521(6) 0.072(3) Uiso 0.526(3) 1 d P A 1 H38A H 0.2777 0.1072 0.5115 0.086 Uiso 0.526(3) 1 calc PR A 1 H38B H 0.2024 0.1472 0.5472 0.086 Uiso 0.526(3) 1 calc PR A 1 C39 C 0.1822(17) 0.0846(5) 0.5792(7) 0.082(4) Uiso 0.526(3) 1 d P A 1 H39A H 0.1042 0.0710 0.5477 0.099 Uiso 0.526(3) 1 calc PR A 1 H39B H 0.1261 0.1007 0.6084 0.099 Uiso 0.526(3) 1 calc PR A 1 C40 C 0.281(2) 0.0068(6) 0.5774(9) 0.097(6) Uiso 0.526(3) 1 d P A 1 H40A H 0.2721 0.0149 0.5341 0.116 Uiso 0.526(3) 1 calc PR A 1 H40B H 0.1925 -0.0136 0.5821 0.116 Uiso 0.526(3) 1 calc PR A 1 C41 C 0.4157(12) -0.0191(4) 0.5931(5) 0.055(2) Uiso 0.526(3) 1 d P A 1 H41A H 0.4326 -0.0388 0.5585 0.066 Uiso 0.526(3) 1 calc PR A 1 H41B H 0.4032 -0.0400 0.6271 0.066 Uiso 0.526(3) 1 calc PR A 1 C42 C 0.6857(9) -0.0165(3) 0.6267(4) 0.0299(17) Uiso 0.526(3) 1 d P A 1 H42A H 0.7013 -0.0392 0.5950 0.036 Uiso 0.526(3) 1 calc PR A 1 H42B H 0.6827 -0.0335 0.6649 0.036 Uiso 0.526(3) 1 calc PR A 1 C43 C 0.8131(9) 0.0193(3) 0.6345(3) 0.0306(15) Uiso 0.526(3) 1 d P A 1 H43A H 0.9142 0.0039 0.6452 0.037 Uiso 0.526(3) 1 calc PR A 1 H43B H 0.8135 0.0370 0.5967 0.037 Uiso 0.526(3) 1 calc PR A 1 O13 O 0.7671(6) 0.11103(17) 0.6830(2) 0.0256(11) Uiso 0.474(3) 1 d P A 2 O14 O 0.5195(6) 0.14609(18) 0.6090(2) 0.0282(12) Uiso 0.474(3) 1 d P A 2 O15 O 0.2426(6) 0.09689(19) 0.6046(3) 0.0298(12) Uiso 0.474(3) 1 d P A 2 O16 O 0.4132(6) 0.01982(17) 0.5929(2) 0.0238(11) Uiso 0.474(3) 1 d P A 2 O17 O 0.6997(6) 0.01974(18) 0.6507(2) 0.0288(12) Uiso 0.474(3) 1 d P A 2 C44 C 0.7868(13) 0.1451(4) 0.6403(5) 0.047(2) Uiso 0.474(3) 1 d P A 2 H44A H 0.8528 0.1310 0.6130 0.057 Uiso 0.474(3) 1 calc PR A 2 H44B H 0.8477 0.1704 0.6623 0.057 Uiso 0.474(3) 1 calc PR A 2 C45 C 0.6442(8) 0.1701(3) 0.5972(3) 0.0212(14) Uiso 0.474(3) 1 d P A 2 H45A H 0.6365 0.2034 0.6077 0.025 Uiso 0.474(3) 1 calc PR A 2 H45B H 0.6563 0.1675 0.5542 0.025 Uiso 0.474(3) 1 calc PR A 2 C46 C 0.3985(9) 0.1548(3) 0.5633(4) 0.0305(16) Uiso 0.474(3) 1 d P A 2 H46A H 0.4126 0.1365 0.5272 0.037 Uiso 0.474(3) 1 calc PR A 2 H46B H 0.3981 0.1883 0.5524 0.037 Uiso 0.474(3) 1 calc PR A 2 C47 C 0.2441(8) 0.1421(3) 0.5828(3) 0.0274(15) Uiso 0.474(3) 1 d P A 2 H47A H 0.2225 0.1640 0.6146 0.033 Uiso 0.474(3) 1 calc PR A 2 H47B H 0.1614 0.1455 0.5480 0.033 Uiso 0.474(3) 1 calc PR A 2 C48 C 0.1998(8) 0.0655(2) 0.5557(3) 0.0200(13) Uiso 0.474(3) 1 d P A 2 H48A H 0.2507 0.0745 0.5209 0.024 Uiso 0.474(3) 1 calc PR A 2 H48B H 0.0871 0.0663 0.5429 0.024 Uiso 0.474(3) 1 calc PR A 2 C49 C 0.2508(11) 0.0169(3) 0.5776(4) 0.0276(19) Uiso 0.474(3) 1 d P A 2 H49A H 0.2030 0.0081 0.6133 0.033 Uiso 0.474(3) 1 calc PR A 2 H49B H 0.2220 -0.0065 0.5455 0.033 Uiso 0.474(3) 1 calc PR A 2 C50 C 0.4879(9) -0.0256(3) 0.6038(4) 0.0276(16) Uiso 0.474(3) 1 d P A 2 H50A H 0.4522 -0.0477 0.5708 0.033 Uiso 0.474(3) 1 calc PR A 2 H50B H 0.4683 -0.0390 0.6425 0.033 Uiso 0.474(3) 1 calc PR A 2 C51 C 0.6567(10) -0.0138(3) 0.6056(5) 0.0309(19) Uiso 0.474(3) 1 d P A 2 H51A H 0.7198 -0.0422 0.6143 0.037 Uiso 0.474(3) 1 calc PR A 2 H51B H 0.6743 -0.0015 0.5660 0.037 Uiso 0.474(3) 1 calc PR A 2 C52 C 0.8500(10) 0.0365(3) 0.6485(4) 0.038(2) Uiso 0.474(3) 1 d P A 2 H52A H 0.8579 0.0486 0.6078 0.045 Uiso 0.474(3) 1 calc PR A 2 H52B H 0.9260 0.0111 0.6579 0.045 Uiso 0.474(3) 1 calc PR A 2 C53 C 0.8804(10) 0.0750(4) 0.6949(4) 0.029(2) Uiso 0.474(3) 1 d P A 2 H53A H 0.8781 0.0621 0.7357 0.035 Uiso 0.474(3) 1 calc PR A 2 H53B H 0.9840 0.0883 0.6940 0.035 Uiso 0.474(3) 1 calc PR A 2 S4 S 0.17737(11) -0.36897(3) 1.04274(4) 0.0316(2) Uani 1 1 d . . . F1 F 0.1000(5) -0.34314(13) 1.14565(15) 0.0899(12) Uani 1 1 d . . . F2 F -0.0510(3) -0.39358(13) 1.09720(16) 0.0749(10) Uani 1 1 d . . . F3 F 0.1749(4) -0.41368(12) 1.14347(13) 0.0750(10) Uani 1 1 d . . . O18 O 0.1591(4) -0.41212(11) 1.01133(14) 0.0468(7) Uani 1 1 d . . . O19 O 0.3368(4) -0.35924(13) 1.06579(17) 0.0619(10) Uani 1 1 d . . . O20 O 0.0873(3) -0.33121(10) 1.01382(14) 0.0443(7) Uani 1 1 d . . . C54 C 0.0968(6) -0.38012(18) 1.1105(2) 0.0495(11) Uani 1 1 d . . . C55 C 0.4236(5) 0.27921(14) 0.92265(17) 0.0349(8) Uani 1 1 d . . . H55A H 0.4735 0.3099 0.9204 0.042 Uiso 1 1 calc R . . H55B H 0.4242 0.2632 0.8836 0.042 Uiso 1 1 calc R . . Cl1 Cl 0.23134(11) 0.28739(4) 0.93495(4) 0.0404(2) Uani 1 1 d . . . Cl2 Cl 0.53002(11) 0.24576(3) 0.98111(4) 0.0384(2) 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 Fe1 0.0139(2) 0.0162(2) 0.0159(2) -0.00066(15) 0.00290(15) 0.00091(15) Sr1 0.02052(15) 0.02003(15) 0.01547(14) -0.00008(10) 0.00189(10) 0.00064(11) O1 0.0289(12) 0.0197(11) 0.0241(11) -0.0036(9) -0.0017(9) 0.0032(9) O2 0.0184(12) 0.0212(12) 0.0543(16) -0.0041(11) -0.0009(11) -0.0015(9) O3 0.0368(13) 0.0205(11) 0.0223(11) -0.0023(9) 0.0122(10) -0.0010(10) O4 0.0332(13) 0.0259(12) 0.0233(12) 0.0006(9) -0.0040(10) 0.0004(10) O5 0.0144(10) 0.0310(12) 0.0200(11) -0.0033(9) 0.0045(8) 0.0009(9) O6 0.0221(11) 0.0196(11) 0.0278(12) -0.0005(9) -0.0016(9) 0.0029(9) O7 0.0157(11) 0.0318(12) 0.0173(11) -0.0009(9) 0.0028(8) 0.0013(9) N1 0.0143(12) 0.0183(12) 0.0200(13) -0.0007(10) 0.0037(10) -0.0001(9) N2 0.0216(13) 0.0167(12) 0.0231(13) 0.0010(10) 0.0082(10) 0.0020(10) N3 0.0196(13) 0.0165(12) 0.0202(13) -0.0038(10) 0.0049(10) -0.0012(10) N4 0.0131(12) 0.0238(13) 0.0169(12) 0.0005(10) 0.0037(9) 0.0008(10) S1 0.0180(4) 0.0146(3) 0.0279(4) -0.0018(3) 0.0002(3) 0.0005(3) S2 0.0270(4) 0.0159(3) 0.0187(4) -0.0006(3) 0.0042(3) -0.0004(3) S3 0.0129(3) 0.0197(4) 0.0184(3) -0.0016(3) 0.0023(3) 0.0018(3) C1 0.0182(15) 0.0209(15) 0.0280(16) -0.0008(12) 0.0080(12) 0.0030(12) C2 0.0275(17) 0.0185(15) 0.0287(17) -0.0034(13) 0.0101(14) 0.0021(12) C3 0.0245(15) 0.0137(14) 0.0193(14) 0.0001(11) 0.0019(12) -0.0009(11) C4 0.0273(17) 0.0205(16) 0.0231(16) 0.0029(12) 0.0036(13) 0.0028(12) C5 0.0380(19) 0.0192(16) 0.0249(17) 0.0033(13) 0.0071(14) 0.0052(14) C6 0.046(2) 0.0179(15) 0.0217(16) 0.0015(12) 0.0076(15) -0.0040(14) C7 0.0316(18) 0.0236(16) 0.0220(16) 0.0024(12) 0.0065(13) -0.0073(13) C8 0.0272(17) 0.0219(16) 0.0168(14) -0.0001(12) 0.0053(12) -0.0017(12) C9 0.0254(18) 0.0247(17) 0.046(2) 0.0028(15) 0.0055(15) 0.0083(14) C10 0.063(3) 0.0172(17) 0.039(2) -0.0011(15) 0.0115(19) -0.0069(17) C11 0.0232(16) 0.0278(17) 0.0308(18) 0.0042(14) 0.0092(14) 0.0001(13) C12 0.0182(15) 0.0208(15) 0.0232(15) 0.0035(12) 0.0069(12) -0.0006(12) C13 0.0182(15) 0.0193(15) 0.0256(16) -0.0014(12) 0.0062(12) -0.0014(11) C14 0.0339(18) 0.0136(14) 0.0179(15) -0.0009(11) 0.0068(13) -0.0010(12) C15 0.0350(19) 0.0206(16) 0.0209(16) -0.0044(12) 0.0094(14) -0.0030(13) C16 0.043(2) 0.0196(16) 0.0263(17) -0.0044(13) 0.0146(15) -0.0047(14) C17 0.054(2) 0.0187(16) 0.0219(16) -0.0005(13) 0.0182(16) 0.0028(15) C18 0.041(2) 0.0274(18) 0.0208(16) -0.0010(13) 0.0052(14) 0.0094(15) C19 0.0336(18) 0.0223(16) 0.0209(16) -0.0040(12) 0.0057(13) 0.0030(13) C20 0.035(2) 0.0303(19) 0.0318(19) -0.0039(15) 0.0045(15) -0.0073(15) C21 0.077(3) 0.0239(19) 0.037(2) 0.0083(16) 0.018(2) 0.0058(19) C22 0.0293(18) 0.0265(18) 0.042(2) -0.0009(15) -0.0026(16) 0.0048(14) C23 0.0181(15) 0.0351(18) 0.0174(15) -0.0047(13) 0.0053(12) -0.0015(13) C24 0.0159(15) 0.0340(18) 0.0180(15) 0.0014(13) 0.0016(12) -0.0008(12) C25 0.0135(13) 0.0184(14) 0.0180(14) -0.0027(11) 0.0040(11) 0.0004(11) C26 0.0164(14) 0.0222(15) 0.0217(15) 0.0010(12) 0.0065(12) 0.0027(11) C27 0.0248(16) 0.0198(15) 0.0290(17) -0.0014(13) 0.0088(13) -0.0004(12) C28 0.0251(16) 0.0258(17) 0.0265(17) -0.0064(13) 0.0071(13) -0.0040(13) C29 0.0204(15) 0.0331(18) 0.0186(15) -0.0013(13) 0.0014(12) -0.0020(13) C30 0.0176(14) 0.0224(15) 0.0195(15) -0.0006(12) 0.0046(11) 0.0014(11) C31 0.0244(16) 0.0227(16) 0.0263(17) 0.0062(13) 0.0015(13) 0.0022(13) C32 0.047(2) 0.032(2) 0.035(2) -0.0100(16) 0.0000(17) -0.0111(17) C33 0.0260(17) 0.0260(16) 0.0201(15) 0.0031(13) -0.0001(13) 0.0027(13) S4 0.0329(5) 0.0349(5) 0.0259(4) 0.0078(4) 0.0011(3) -0.0026(4) F1 0.130(3) 0.089(3) 0.0501(18) -0.0210(17) 0.0148(19) 0.041(2) F2 0.0484(17) 0.088(2) 0.095(2) 0.026(2) 0.0329(17) 0.0014(16) F3 0.090(2) 0.094(2) 0.0481(17) 0.0376(16) 0.0335(16) 0.0425(19) O18 0.0528(19) 0.0470(18) 0.0380(16) -0.0031(13) -0.0012(14) 0.0088(14) O19 0.0331(16) 0.076(2) 0.073(2) 0.036(2) -0.0045(15) -0.0129(16) O20 0.0427(16) 0.0405(16) 0.0484(17) 0.0181(13) 0.0023(13) 0.0031(13) C54 0.056(3) 0.056(3) 0.040(2) 0.008(2) 0.020(2) 0.013(2) C55 0.041(2) 0.034(2) 0.0296(19) 0.0020(15) 0.0046(16) -0.0018(16) Cl1 0.0383(5) 0.0441(5) 0.0370(5) -0.0093(4) 0.0003(4) 0.0106(4) Cl2 0.0407(5) 0.0336(5) 0.0370(5) -0.0079(4) -0.0065(4) 0.0077(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 Fe1 O7 1.872(2) . ? Fe1 N2 2.009(3) . ? Fe1 N3 2.010(3) . ? Fe1 N4 2.024(3) . ? Fe1 N1 2.280(3) . ? Sr1 O7 2.464(2) . ? Sr1 O13 2.535(5) . ? Sr1 O1 2.538(2) . ? Sr1 O3 2.547(2) . ? Sr1 O14 2.565(5) . ? Sr1 O11 2.581(5) . ? Sr1 O10 2.629(5) . ? Sr1 O17 2.633(5) . ? Sr1 O8 2.644(4) . ? Sr1 O16 2.659(5) . ? Sr1 O12 2.662(5) . ? Sr1 O9 2.664(5) . ? Sr1 O15 2.687(6) . ? O1 S1 1.455(2) . ? O2 S1 1.438(2) . ? O3 S2 1.455(2) . ? O4 S2 1.438(2) . ? O5 S3 1.450(2) . ? O5 H7 1.90(2) . ? O6 S3 1.438(2) . ? N1 C23 1.472(4) . ? N1 C12 1.483(4) . ? N1 C1 1.488(4) . ? N2 C2 1.485(4) . ? N2 S1 1.589(3) . ? N3 C13 1.488(4) . ? N3 S2 1.592(3) . ? N4 C24 1.481(4) . ? N4 S3 1.608(3) . ? S1 C3 1.795(3) . ? S2 C14 1.788(3) . ? S3 C25 1.798(3) . ? C1 C2 1.503(4) . ? C3 C4 1.410(4) . ? C3 C8 1.414(4) . ? C4 C5 1.402(5) . ? C4 C9 1.512(5) . ? C5 C6 1.380(5) . ? C6 C7 1.385(5) . ? C6 C10 1.510(5) . ? C7 C8 1.395(5) . ? C8 C11 1.502(5) . ? C12 C13 1.511(4) . ? C14 C19 1.408(5) . ? C14 C15 1.414(5) . ? C15 C16 1.400(5) . ? C15 C20 1.515(5) . ? C16 C17 1.371(5) . ? C17 C18 1.385(5) . ? C17 C21 1.512(5) . ? C18 C19 1.394(5) . ? C19 C22 1.515(5) . ? C23 C24 1.514(4) . ? C25 C30 1.412(4) . ? C25 C26 1.419(4) . ? C26 C27 1.394(5) . ? C26 C31 1.509(4) . ? C27 C28 1.390(5) . ? C28 C29 1.377(5) . ? C28 C32 1.514(5) . ? C29 C30 1.404(4) . ? C30 C33 1.509(4) . ? O8 C34 1.442(8) . ? O8 C43 1.445(8) . ? O9 C36 1.259(10) . ? O9 C35 1.457(8) . ? O10 C38 1.387(12) . ? O10 C37 1.497(13) . ? O11 C40 1.398(18) . ? O11 C39 1.407(14) . ? O12 C41 1.403(11) . ? O12 C42 1.441(9) . ? C34 C35 1.506(10) . ? C36 C37 1.381(15) . ? C38 C39 1.393(17) . ? C40 C41 1.40(2) . ? C42 C43 1.512(11) . ? O13 C44 1.398(11) . ? O13 C53 1.433(10) . ? O14 C45 1.355(9) . ? O14 C46 1.386(9) . ? O15 C47 1.387(9) . ? O15 C48 1.427(9) . ? O16 C49 1.421(11) . ? O16 C50 1.463(9) . ? O17 C51 1.407(10) . ? O17 C52 1.414(10) . ? C44 C45 1.631(12) . ? C46 C47 1.533(10) . ? C48 C49 1.526(12) . ? C50 C51 1.517(12) . ? C52 C53 1.517(13) . ? S4 O18 1.423(3) . ? S4 O20 1.439(3) . ? S4 O19 1.447(3) . ? S4 C54 1.801(4) . ? F1 C54 1.320(6) . ? F2 C54 1.346(6) . ? F3 C54 1.340(5) . ? C55 Cl1 1.769(4) . ? C55 Cl2 1.775(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 O7 Fe1 N2 100.45(10) . . ? O7 Fe1 N3 104.33(10) . . ? N2 Fe1 N3 110.40(11) . . ? O7 Fe1 N4 99.67(10) . . ? N2 Fe1 N4 118.64(11) . . ? N3 Fe1 N4 119.41(11) . . ? O7 Fe1 N1 175.99(10) . . ? N2 Fe1 N1 79.27(10) . . ? N3 Fe1 N1 79.45(10) . . ? N4 Fe1 N1 77.10(10) . . ? O7 Sr1 O13 79.21(12) . . ? O7 Sr1 O1 72.17(7) . . ? O13 Sr1 O1 108.22(12) . . ? O7 Sr1 O3 70.48(8) . . ? O13 Sr1 O3 127.66(12) . . ? O1 Sr1 O3 101.82(8) . . ? O7 Sr1 O14 120.97(13) . . ? O13 Sr1 O14 64.62(16) . . ? O1 Sr1 O14 76.86(13) . . ? O3 Sr1 O14 166.41(13) . . ? O7 Sr1 O11 139.89(13) . . ? O13 Sr1 O11 140.80(16) . . ? O1 Sr1 O11 91.49(12) . . ? O3 Sr1 O11 77.84(13) . . ? O14 Sr1 O11 88.64(16) . . ? O7 Sr1 O10 141.03(12) . . ? O13 Sr1 O10 88.71(15) . . ? O1 Sr1 O10 76.90(11) . . ? O3 Sr1 O10 140.22(12) . . ? O14 Sr1 O10 26.19(15) . . ? O11 Sr1 O10 62.55(15) . . ? O7 Sr1 O17 103.25(12) . . ? O13 Sr1 O17 64.52(16) . . ? O1 Sr1 O17 172.36(13) . . ? O3 Sr1 O17 81.94(12) . . ? O14 Sr1 O17 101.06(16) . . ? O11 Sr1 O17 95.83(16) . . ? O10 Sr1 O17 104.56(15) . . ? O7 Sr1 O8 83.83(10) . . ? O13 Sr1 O8 39.50(14) . . ? O1 Sr1 O8 144.13(10) . . ? O3 Sr1 O8 94.48(10) . . ? O14 Sr1 O8 94.14(14) . . ? O11 Sr1 O8 123.33(14) . . ? O10 Sr1 O8 109.69(13) . . ? O17 Sr1 O8 28.24(14) . . ? O7 Sr1 O16 146.67(12) . . ? O13 Sr1 O16 112.94(15) . . ? O1 Sr1 O16 126.84(12) . . ? O3 Sr1 O16 78.23(12) . . ? O14 Sr1 O16 91.67(15) . . ? O11 Sr1 O16 35.81(15) . . ? O10 Sr1 O16 71.99(15) . . ? O17 Sr1 O16 60.25(15) . . ? O8 Sr1 O16 87.53(14) . . ? O7 Sr1 O12 130.29(11) . . ? O13 Sr1 O12 92.50(15) . . ? O1 Sr1 O12 153.00(11) . . ? O3 Sr1 O12 77.26(11) . . ? O14 Sr1 O12 97.69(15) . . ? O11 Sr1 O12 61.75(15) . . ? O10 Sr1 O12 86.72(14) . . ? O17 Sr1 O12 34.11(15) . . ? O8 Sr1 O12 61.80(13) . . ? O16 Sr1 O12 26.17(14) . . ? O7 Sr1 O9 97.94(11) . . ? O13 Sr1 O9 28.29(14) . . ? O1 Sr1 O9 94.32(11) . . ? O3 Sr1 O9 155.72(11) . . ? O14 Sr1 O9 36.35(15) . . ? O11 Sr1 O9 120.12(15) . . ? O10 Sr1 O9 61.11(14) . . ? O17 Sr1 O9 80.11(15) . . ? O8 Sr1 O9 62.44(13) . . ? O16 Sr1 O9 106.38(14) . . ? O12 Sr1 O9 96.36(14) . . ? O7 Sr1 O15 136.55(13) . . ? O13 Sr1 O15 128.39(16) . . ? O1 Sr1 O15 67.53(13) . . ? O3 Sr1 O15 102.33(13) . . ? O14 Sr1 O15 64.49(16) . . ? O11 Sr1 O15 31.33(16) . . ? O10 Sr1 O15 39.69(15) . . ? O17 Sr1 O15 118.45(16) . . ? O8 Sr1 O15 139.44(14) . . ? O16 Sr1 O15 60.88(16) . . ? O12 Sr1 O15 86.13(15) . . ? O9 Sr1 O15 100.56(15) . . ? S1 O1 Sr1 155.10(14) . . ? S2 O3 Sr1 129.46(13) . . ? S3 O5 H7 115.4(12) . . ? Fe1 O7 Sr1 124.01(10) . . ? C23 N1 C12 111.4(2) . . ? C23 N1 C1 110.7(2) . . ? C12 N1 C1 111.8(2) . . ? C23 N1 Fe1 109.22(18) . . ? C12 N1 Fe1 105.88(18) . . ? C1 N1 Fe1 107.59(18) . . ? C2 N2 S1 114.0(2) . . ? C2 N2 Fe1 113.7(2) . . ? S1 N2 Fe1 126.26(15) . . ? C13 N3 S2 111.5(2) . . ? C13 N3 Fe1 115.51(19) . . ? S2 N3 Fe1 131.43(15) . . ? C24 N4 S3 110.5(2) . . ? C24 N4 Fe1 118.27(19) . . ? S3 N4 Fe1 129.18(15) . . ? O2 S1 O1 114.89(15) . . ? O2 S1 N2 112.83(15) . . ? O1 S1 N2 107.31(13) . . ? O2 S1 C3 107.67(14) . . ? O1 S1 C3 109.30(14) . . ? N2 S1 C3 104.30(14) . . ? O4 S2 O3 114.76(15) . . ? O4 S2 N3 111.56(14) . . ? O3 S2 N3 108.76(14) . . ? O4 S2 C14 108.16(15) . . ? O3 S2 C14 107.00(15) . . ? N3 S2 C14 106.15(14) . . ? O4 S2 Sr1 96.93(10) . . ? O3 S2 Sr1 32.61(9) . . ? N3 S2 Sr1 92.73(10) . . ? C14 S2 Sr1 139.59(11) . . ? O6 S3 O5 115.57(14) . . ? O6 S3 N4 110.88(14) . . ? O5 S3 N4 108.74(13) . . ? O6 S3 C25 108.17(14) . . ? O5 S3 C25 106.30(14) . . ? N4 S3 C25 106.73(13) . . ? N1 C1 C2 108.1(2) . . ? N2 C2 C1 109.2(3) . . ? C4 C3 C8 120.9(3) . . ? C4 C3 S1 120.9(2) . . ? C8 C3 S1 117.8(2) . . ? C5 C4 C3 117.3(3) . . ? C5 C4 C9 116.3(3) . . ? C3 C4 C9 126.4(3) . . ? C6 C5 C4 123.1(3) . . ? C5 C6 C7 118.0(3) . . ? C5 C6 C10 121.0(3) . . ? C7 C6 C10 120.9(3) . . ? C6 C7 C8 122.3(3) . . ? C7 C8 C3 118.2(3) . . ? C7 C8 C11 117.7(3) . . ? C3 C8 C11 124.1(3) . . ? N1 C12 C13 109.0(2) . . ? N3 C13 C12 108.0(2) . . ? C19 C14 C15 121.1(3) . . ? C19 C14 S2 118.1(2) . . ? C15 C14 S2 120.8(3) . . ? C16 C15 C14 117.2(3) . . ? C16 C15 C20 116.3(3) . . ? C14 C15 C20 126.5(3) . . ? C17 C16 C15 123.1(3) . . ? C16 C17 C18 118.1(3) . . ? C16 C17 C21 120.8(4) . . ? C18 C17 C21 121.1(4) . . ? C17 C18 C19 122.6(3) . . ? C18 C19 C14 117.8(3) . . ? C18 C19 C22 117.8(3) . . ? C14 C19 C22 124.4(3) . . ? N1 C23 C24 109.6(3) . . ? N4 C24 C23 107.2(3) . . ? C30 C25 C26 120.7(3) . . ? C30 C25 S3 121.3(2) . . ? C26 C25 S3 117.9(2) . . ? C27 C26 C25 118.5(3) . . ? C27 C26 C31 117.2(3) . . ? C25 C26 C31 124.3(3) . . ? C28 C27 C26 121.9(3) . . ? C29 C28 C27 118.3(3) . . ? C29 C28 C32 121.3(3) . . ? C27 C28 C32 120.4(3) . . ? C28 C29 C30 123.2(3) . . ? C29 C30 C25 117.3(3) . . ? C29 C30 C33 116.8(3) . . ? C25 C30 C33 125.9(3) . . ? C34 O8 C43 114.3(5) . . ? C34 O8 Sr1 110.4(4) . . ? C43 O8 Sr1 118.0(4) . . ? C36 O9 C35 98.7(6) . . ? C36 O9 Sr1 115.5(5) . . ? C35 O9 Sr1 120.4(3) . . ? C38 O10 C37 116.5(8) . . ? C38 O10 Sr1 118.5(6) . . ? C37 O10 Sr1 116.8(5) . . ? C40 O11 C39 117.7(11) . . ? C40 O11 Sr1 119.8(8) . . ? C39 O11 Sr1 110.8(7) . . ? C41 O12 C42 113.8(6) . . ? C41 O12 Sr1 113.9(5) . . ? C42 O12 Sr1 115.2(4) . . ? O8 C34 C35 111.3(5) . . ? O9 C35 C34 106.4(5) . . ? O9 C36 C37 129.1(10) . . ? O9 C36 Sr1 45.0(4) . . ? C37 C36 Sr1 85.2(7) . . ? C36 C37 O10 108.5(9) . . ? O10 C38 C39 113.1(11) . . ? C38 C39 O11 117.6(12) . . ? C38 C39 Sr1 84.7(8) . . ? O11 C39 Sr1 46.1(5) . . ? O11 C40 C41 117.1(14) . . ? C40 C41 O12 112.6(11) . . ? O12 C42 C43 105.8(6) . . ? O8 C43 C42 106.9(6) . . ? C44 O13 C53 118.6(7) . . ? C44 O13 Sr1 117.6(5) . . ? C53 O13 Sr1 111.1(5) . . ? C45 O14 C46 108.6(6) . . ? C45 O14 Sr1 130.3(4) . . ? C46 O14 Sr1 119.5(4) . . ? C47 O15 C48 109.5(6) . . ? C47 O15 Sr1 110.9(4) . . ? C48 O15 Sr1 118.8(4) . . ? C49 O16 C50 113.4(6) . . ? C49 O16 Sr1 112.3(5) . . ? C50 O16 Sr1 112.0(4) . . ? C51 O17 C52 111.0(6) . . ? C51 O17 Sr1 121.3(5) . . ? C52 O17 Sr1 117.4(5) . . ? O13 C44 C45 123.5(8) . . ? O13 C44 Sr1 41.1(4) . . ? C45 C44 Sr1 82.7(5) . . ? O14 C45 C44 103.5(6) . . ? O14 C46 C47 111.1(6) . . ? O15 C47 C46 112.4(6) . . ? O15 C48 C49 107.3(6) . . ? O16 C49 C48 105.1(7) . . ? O16 C50 C51 102.7(6) . . ? O17 C51 C50 109.1(7) . . ? O17 C52 C53 107.0(7) . . ? O13 C53 C52 110.6(7) . . ? O13 C53 Sr1 45.2(4) . . ? C52 C53 Sr1 84.1(5) . . ? O18 S4 O20 114.78(19) . . ? O18 S4 O19 112.1(2) . . ? O20 S4 O19 117.0(2) . . ? O18 S4 C54 103.5(2) . . ? O20 S4 C54 104.8(2) . . ? O19 S4 C54 102.4(2) . . ? F1 C54 F3 106.5(4) . . ? F1 C54 F2 107.3(4) . . ? F3 C54 F2 108.3(4) . . ? F1 C54 S4 112.7(4) . . ? F3 C54 S4 111.1(3) . . ? F2 C54 S4 110.7(3) . . ? Cl1 C55 Cl2 111.5(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.001 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.095 _iucr_refine_instructions_details ; TITL asb247 in P2(1)/c CELL 0.71073 8.7949 28.7099 22.4440 90.000 98.6131 90.000 ZERR 4.00 0.0003 0.0011 0.0009 0.000 0.0005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F S CL FE SR UNIT 180 272 16 60 12 16 8 4 4 TEMP -185.000 SIZE 0.13 0.184 0.315 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 rem Young Jun Park 25s sphere ccd1 SHEL 100 0.78 OMIT 0 2 0 OMIT 0 1 1 CONN 13 SR1 CONN 5 FE1 DFIX 0.85 0.001 O7 H7 BIND O5 H7 L.S. 12 ACTA 51 WGHT 0.064900 13.239697 FVAR 0.06311 0.52626 FE1 8 0.450002 0.089917 0.849387 11.00000 0.01389 0.01620 = 0.01590 -0.00066 0.00290 0.00091 SR1 9 0.498410 0.079020 0.682789 11.00000 0.02052 0.02003 = 0.01547 -0.00008 0.00189 0.00064 O1 4 0.335061 0.142502 0.719988 11.00000 0.02889 0.01966 = 0.02406 -0.00355 -0.00169 0.00315 O2 4 0.095385 0.161190 0.757014 11.00000 0.01843 0.02118 = 0.05426 -0.00405 -0.00087 -0.00149 O3 4 0.420045 0.007904 0.738837 11.00000 0.03682 0.02052 = 0.02233 -0.00230 0.01219 -0.00103 O4 4 0.141444 0.005896 0.733709 11.00000 0.03324 0.02586 = 0.02326 0.00058 -0.00402 0.00040 O5 4 0.837592 0.084899 0.874384 11.00000 0.01443 0.03101 = 0.02004 -0.00335 0.00446 0.00094 O6 4 0.832105 0.034636 0.961885 11.00000 0.02207 0.01963 = 0.02784 -0.00048 -0.00156 0.00292 O7 4 0.583392 0.088847 0.791757 11.00000 0.01570 0.03183 = 0.01730 -0.00094 0.00276 0.00128 H7 2 0.676989 0.089811 0.808086 11.00000 0.03991 N1 3 0.300171 0.094199 0.923802 11.00000 0.01432 0.01828 = 0.01995 -0.00069 0.00371 -0.00014 N2 3 0.342177 0.150851 0.829130 11.00000 0.02159 0.01670 = 0.02314 0.00098 0.00821 0.00198 N3 3 0.305621 0.036428 0.826421 11.00000 0.01956 0.01655 = 0.02021 -0.00382 0.00492 -0.00121 N4 3 0.605354 0.085676 0.925444 11.00000 0.01306 0.02377 = 0.01686 0.00048 0.00373 0.00076 S1 6 0.259701 0.166696 0.764461 11.00000 0.01797 0.01465 = 0.02788 -0.00182 0.00022 0.00054 S2 6 0.289093 0.001568 0.770675 11.00000 0.02705 0.01586 = 0.01870 -0.00058 0.00417 -0.00038 S3 6 0.788445 0.078218 0.932623 11.00000 0.01287 0.01967 = 0.01836 -0.00155 0.00235 0.00184 C1 1 0.192155 0.133895 0.909390 11.00000 0.01818 0.02093 = 0.02796 -0.00076 0.00802 0.00301 AFIX 23 H1A 2 0.159078 0.145981 0.946722 11.00000 -1.20000 H1B 2 0.099776 0.123547 0.881846 11.00000 -1.20000 AFIX 0 C2 1 0.274326 0.171349 0.879904 11.00000 0.02748 0.01849 = 0.02875 -0.00340 0.01014 0.00214 AFIX 23 H2A 2 0.201129 0.196360 0.864755 11.00000 -1.20000 H2B 2 0.356504 0.185121 0.909658 11.00000 -1.20000 AFIX 0 C3 1 0.299972 0.227895 0.761630 11.00000 0.02445 0.01369 = 0.01926 0.00008 0.00195 -0.00088 C4 1 0.184873 0.261249 0.766715 11.00000 0.02734 0.02048 = 0.02307 0.00291 0.00361 0.00285 C5 1 0.231265 0.307850 0.774266 11.00000 0.03796 0.01923 = 0.02489 0.00330 0.00710 0.00524 AFIX 43 H5A 2 0.155378 0.330772 0.778026 11.00000 -1.20000 AFIX 0 C6 1 0.381957 0.322014 0.776499 11.00000 0.04576 0.01787 = 0.02166 0.00148 0.00762 -0.00403 C7 1 0.490703 0.288664 0.768343 11.00000 0.03160 0.02360 = 0.02197 0.00244 0.00645 -0.00727 AFIX 43 H7A 2 0.593843 0.298230 0.767687 11.00000 -1.20000 AFIX 0 C8 1 0.454213 0.241534 0.761058 11.00000 0.02721 0.02194 = 0.01677 -0.00011 0.00534 -0.00168 C9 1 0.015208 0.251716 0.765217 11.00000 0.02544 0.02466 = 0.04638 0.00277 0.00548 0.00834 AFIX 137 H9A 2 0.000725 0.231118 0.798730 11.00000 -1.50000 H9B 2 -0.026010 0.236711 0.726978 11.00000 -1.50000 H9C 2 -0.039022 0.281144 0.768972 11.00000 -1.50000 AFIX 0 C10 1 0.428479 0.371896 0.790718 11.00000 0.06264 0.01724 = 0.03895 -0.00113 0.01147 -0.00687 AFIX 137 H10A 2 0.346943 0.392823 0.772075 11.00000 -1.50000 H10B 2 0.523929 0.378755 0.774826 11.00000 -1.50000 H10C 2 0.444752 0.376478 0.834481 11.00000 -1.50000 AFIX 0 C11 1 0.581959 0.208383 0.753361 11.00000 0.02323 0.02776 = 0.03075 0.00417 0.00920 0.00015 AFIX 137 H11A 2 0.680962 0.224476 0.762560 11.00000 -1.50000 H11B 2 0.568485 0.197115 0.711686 11.00000 -1.50000 H11C 2 0.579778 0.181930 0.780815 11.00000 -1.50000 AFIX 0 C12 1 0.217888 0.049053 0.922603 11.00000 0.01820 0.02078 = 0.02317 0.00348 0.00689 -0.00056 AFIX 23 H12A 2 0.126730 0.052167 0.943377 11.00000 -1.20000 H12B 2 0.286423 0.025028 0.943834 11.00000 -1.20000 AFIX 0 C13 1 0.168262 0.034677 0.857861 11.00000 0.01819 0.01928 = 0.02555 -0.00136 0.00617 -0.00142 AFIX 23 H13A 2 0.125469 0.002729 0.856152 11.00000 -1.20000 H13B 2 0.087841 0.056097 0.838173 11.00000 -1.20000 AFIX 0 C14 1 0.303705 -0.055809 0.801932 11.00000 0.03388 0.01359 = 0.01788 -0.00092 0.00676 -0.00100 C15 1 0.174878 -0.085865 0.795437 11.00000 0.03497 0.02058 = 0.02094 -0.00438 0.00935 -0.00295 C16 1 0.197232 -0.130736 0.819544 11.00000 0.04305 0.01958 = 0.02630 -0.00437 0.01457 -0.00473 AFIX 43 H16A 2 0.112450 -0.151602 0.815004 11.00000 -1.20000 AFIX 0 C17 1 0.335740 -0.146000 0.849409 11.00000 0.05393 0.01871 = 0.02189 -0.00052 0.01823 0.00280 C18 1 0.458272 -0.115158 0.856567 11.00000 0.04124 0.02743 = 0.02076 -0.00101 0.00516 0.00938 AFIX 43 H18A 2 0.554135 -0.125226 0.877887 11.00000 -1.20000 AFIX 0 C19 1 0.446472 -0.069940 0.833726 11.00000 0.03363 0.02228 = 0.02094 -0.00402 0.00568 0.00301 C20 1 0.012928 -0.073998 0.766201 11.00000 0.03532 0.03032 = 0.03184 -0.00388 0.00446 -0.00728 AFIX 137 H20A 2 -0.056880 -0.099292 0.773427 11.00000 -1.50000 H20B 2 0.010903 -0.069990 0.722727 11.00000 -1.50000 H20C 2 -0.019994 -0.045036 0.783539 11.00000 -1.50000 AFIX 0 C21 1 0.352244 -0.194526 0.875741 11.00000 0.07669 0.02385 = 0.03680 0.00833 0.01817 0.00584 AFIX 137 H21A 2 0.303486 -0.216990 0.845973 11.00000 -1.50000 H21B 2 0.302363 -0.195936 0.911927 11.00000 -1.50000 H21C 2 0.461583 -0.202109 0.886394 11.00000 -1.50000 AFIX 0 C22 1 0.588022 -0.039269 0.844879 11.00000 0.02932 0.02654 = 0.04207 -0.00089 -0.00262 0.00478 AFIX 137 H22A 2 0.616257 -0.029363 0.806208 11.00000 -1.50000 H22B 2 0.673289 -0.056798 0.867558 11.00000 -1.50000 H22C 2 0.566097 -0.011803 0.868087 11.00000 -1.50000 AFIX 0 C23 1 0.398850 0.101709 0.981984 11.00000 0.01808 0.03514 = 0.01737 -0.00470 0.00533 -0.00155 AFIX 23 H23A 2 0.345611 0.090598 1.015167 11.00000 -1.20000 H23B 2 0.420003 0.135385 0.987994 11.00000 -1.20000 AFIX 0 C24 1 0.548579 0.075520 0.982933 11.00000 0.01593 0.03397 = 0.01801 0.00137 0.00162 -0.00076 AFIX 23 H24A 2 0.624615 0.085851 1.017448 11.00000 -1.20000 H24B 2 0.531571 0.041644 0.986871 11.00000 -1.20000 AFIX 0 C25 1 0.874657 0.124490 0.980126 11.00000 0.01348 0.01843 = 0.01805 -0.00266 0.00396 0.00043 C26 1 0.859411 0.170659 0.957398 11.00000 0.01636 0.02222 = 0.02171 0.00100 0.00647 0.00266 C27 1 0.932275 0.206604 0.992481 11.00000 0.02483 0.01984 = 0.02902 -0.00143 0.00884 -0.00042 AFIX 43 H27A 2 0.920187 0.237711 0.978124 11.00000 -1.20000 AFIX 0 C28 1 1.022074 0.198233 1.047847 11.00000 0.02513 0.02576 = 0.02645 -0.00643 0.00706 -0.00401 C29 1 1.035302 0.153083 1.068727 11.00000 0.02036 0.03314 = 0.01862 -0.00133 0.00137 -0.00203 AFIX 43 H29A 2 1.097209 0.147290 1.106440 11.00000 -1.20000 AFIX 0 C30 1 0.961729 0.115211 1.036975 11.00000 0.01756 0.02245 = 0.01955 -0.00056 0.00459 0.00139 C31 1 0.773466 0.183551 0.896334 11.00000 0.02439 0.02268 = 0.02634 0.00624 0.00148 0.00215 AFIX 137 H31A 2 0.767077 0.217539 0.892763 11.00000 -1.50000 H31B 2 0.669516 0.170419 0.891762 11.00000 -1.50000 H31C 2 0.827982 0.171069 0.864812 11.00000 -1.50000 AFIX 0 C32 1 1.102562 0.238047 1.083935 11.00000 0.04725 0.03179 = 0.03533 -0.01002 0.00002 -0.01109 AFIX 137 H32A 2 1.115326 0.230402 1.126951 11.00000 -1.50000 H32B 2 1.040734 0.266429 1.076474 11.00000 -1.50000 H32C 2 1.203728 0.243084 1.071741 11.00000 -1.50000 AFIX 0 C33 1 0.981726 0.068206 1.067227 11.00000 0.02596 0.02598 = 0.02009 0.00308 -0.00012 0.00273 AFIX 137 H33A 2 0.880515 0.054535 1.069231 11.00000 -1.50000 H33B 2 1.037799 0.071879 1.108101 11.00000 -1.50000 H33C 2 1.039850 0.047677 1.043995 11.00000 -1.50000 AFIX 0 PART 1 O8 4 0.783714 0.050189 0.682354 21.00000 0.01782 O9 4 0.694487 0.138343 0.643754 21.00000 0.02264 O10 4 0.406635 0.127882 0.584960 21.00000 0.02800 O11 4 0.266320 0.047818 0.609594 21.00000 0.03419 O12 4 0.545220 0.009206 0.609590 21.00000 0.02729 C34 1 0.889643 0.088691 0.693066 21.00000 0.02091 AFIX 23 H34A 2 0.995957 0.077180 0.693629 21.00000 -1.20000 H34B 2 0.882629 0.102500 0.732982 21.00000 -1.20000 AFIX 0 C35 1 0.855332 0.125541 0.645177 21.00000 0.02385 AFIX 23 H35A 2 0.922550 0.152977 0.655101 21.00000 -1.20000 H35B 2 0.872580 0.113228 0.605533 21.00000 -1.20000 AFIX 0 C36 1 0.663877 0.149615 0.589048 21.00000 0.05407 AFIX 23 H36A 2 0.743469 0.134051 0.569257 21.00000 -1.20000 H36B 2 0.686530 0.183359 0.588049 21.00000 -1.20000 AFIX 0 C37 1 0.528601 0.143886 0.549752 21.00000 0.07501 AFIX 23 H37A 2 0.543025 0.120524 0.518640 21.00000 -1.20000 H37B 2 0.497834 0.173733 0.529348 21.00000 -1.20000 AFIX 0 C38 1 0.263668 0.118170 0.552147 21.00000 0.07175 AFIX 23 H38A 2 0.277699 0.107182 0.511514 21.00000 -1.20000 H38B 2 0.202449 0.147223 0.547166 21.00000 -1.20000 AFIX 0 C39 1 0.182227 0.084646 0.579226 21.00000 0.08209 AFIX 23 H39A 2 0.104235 0.071016 0.547656 21.00000 -1.20000 H39B 2 0.126054 0.100668 0.608364 21.00000 -1.20000 AFIX 0 C40 1 0.280753 0.006759 0.577388 21.00000 0.09688 AFIX 23 H40A 2 0.272070 0.014855 0.534134 21.00000 -1.20000 H40B 2 0.192482 -0.013603 0.582091 21.00000 -1.20000 AFIX 0 C41 1 0.415727 -0.019082 0.593086 21.00000 0.05461 AFIX 23 H41A 2 0.432620 -0.038794 0.558482 21.00000 -1.20000 H41B 2 0.403174 -0.039963 0.627113 21.00000 -1.20000 AFIX 0 C42 1 0.685694 -0.016510 0.626742 21.00000 0.02989 AFIX 23 H42A 2 0.701310 -0.039238 0.595042 21.00000 -1.20000 H42B 2 0.682717 -0.033534 0.664909 21.00000 -1.20000 AFIX 0 C43 1 0.813073 0.019324 0.634514 21.00000 0.03063 AFIX 23 H43A 2 0.914201 0.003930 0.645217 21.00000 -1.20000 H43B 2 0.813471 0.036994 0.596658 21.00000 -1.20000 AFIX 0 PART 2 O13 4 0.767136 0.111033 0.682970 -21.00000 0.02563 O14 4 0.519483 0.146088 0.608971 -21.00000 0.02820 O15 4 0.242625 0.096885 0.604631 -21.00000 0.02983 O16 4 0.413207 0.019820 0.592894 -21.00000 0.02382 O17 4 0.699718 0.019744 0.650687 -21.00000 0.02880 C44 1 0.786796 0.145073 0.640268 -21.00000 0.04734 AFIX 23 H44A 2 0.852808 0.131038 0.613009 -21.00000 -1.20000 H44B 2 0.847728 0.170368 0.662320 -21.00000 -1.20000 AFIX 0 C45 1 0.644239 0.170107 0.597235 -21.00000 0.02115 AFIX 23 H45A 2 0.636512 0.203432 0.607716 -21.00000 -1.20000 H45B 2 0.656291 0.167498 0.554207 -21.00000 -1.20000 AFIX 0 C46 1 0.398480 0.154843 0.563270 -21.00000 0.03053 AFIX 23 H46A 2 0.412628 0.136488 0.527163 -21.00000 -1.20000 H46B 2 0.398105 0.188258 0.552358 -21.00000 -1.20000 AFIX 0 C47 1 0.244118 0.142065 0.582848 -21.00000 0.02741 AFIX 23 H47A 2 0.222542 0.163980 0.614596 -21.00000 -1.20000 H47B 2 0.161354 0.145535 0.548029 -21.00000 -1.20000 AFIX 0 C48 1 0.199822 0.065544 0.555672 -21.00000 0.02003 AFIX 23 H48A 2 0.250673 0.074465 0.520877 -21.00000 -1.20000 H48B 2 0.087103 0.066290 0.542931 -21.00000 -1.20000 AFIX 0 C49 1 0.250800 0.016891 0.577646 -21.00000 0.02758 AFIX 23 H49A 2 0.202970 0.008116 0.613261 -21.00000 -1.20000 H49B 2 0.221992 -0.006478 0.545500 -21.00000 -1.20000 AFIX 0 C50 1 0.487873 -0.025551 0.603777 -21.00000 0.02762 AFIX 23 H50A 2 0.452164 -0.047669 0.570798 -21.00000 -1.20000 H50B 2 0.468263 -0.039042 0.642503 -21.00000 -1.20000 AFIX 0 C51 1 0.656705 -0.013796 0.605574 -21.00000 0.03090 AFIX 23 H51A 2 0.719843 -0.042223 0.614283 -21.00000 -1.20000 H51B 2 0.674303 -0.001460 0.565985 -21.00000 -1.20000 AFIX 0 C52 1 0.850030 0.036453 0.648487 -21.00000 0.03778 AFIX 23 H52A 2 0.857941 0.048615 0.607790 -21.00000 -1.20000 H52B 2 0.925977 0.011058 0.657901 -21.00000 -1.20000 AFIX 0 C53 1 0.880443 0.075036 0.694949 -21.00000 0.02877 AFIX 23 H53A 2 0.878117 0.062077 0.735679 -21.00000 -1.20000 H53B 2 0.983953 0.088307 0.694010 -21.00000 -1.20000 AFIX 0 PART 0 S4 6 0.177368 -0.368968 1.042735 11.00000 0.03289 0.03489 = 0.02589 0.00784 0.00110 -0.00257 F1 5 0.100013 -0.343145 1.145650 11.00000 0.13047 0.08947 = 0.05008 -0.02105 0.01484 0.04099 F2 5 -0.051001 -0.393575 1.097198 11.00000 0.04838 0.08787 = 0.09518 0.02590 0.03287 0.00137 F3 5 0.174857 -0.413676 1.143474 11.00000 0.08980 0.09412 = 0.04813 0.03762 0.03351 0.04250 O18 4 0.159133 -0.412120 1.011331 11.00000 0.05284 0.04703 = 0.03799 -0.00309 -0.00122 0.00878 O19 4 0.336765 -0.359239 1.065791 11.00000 0.03312 0.07626 = 0.07258 0.03568 -0.00450 -0.01286 O20 4 0.087329 -0.331207 1.013819 11.00000 0.04271 0.04052 = 0.04841 0.01812 0.00234 0.00314 C54 1 0.096750 -0.380121 1.110510 11.00000 0.05636 0.05620 = 0.03985 0.00837 0.02007 0.01330 C55 1 0.423628 0.279214 0.922655 11.00000 0.04050 0.03446 = 0.02959 0.00204 0.00463 -0.00181 AFIX 23 H55A 2 0.473518 0.309947 0.920430 11.00000 -1.20000 H55B 2 0.424160 0.263197 0.883624 11.00000 -1.20000 AFIX 0 CL1 7 0.231344 0.287385 0.934951 11.00000 0.03829 0.04414 = 0.03701 -0.00926 0.00033 0.01058 CL2 7 0.530022 0.245763 0.981114 11.00000 0.04074 0.03365 = 0.03703 -0.00794 -0.00645 0.00769 HKLF 4 REM asb247 in P2(1)/c REM R1 = 0.0472 for 10487 Fo > 4sig(Fo) and 0.0578 for all 12345 data REM 675 parameters refined using 1 restraints END WGHT 0.0648 13.2487 REM Highest difference peak 2.001, deepest hole -0.896, 1-sigma level 0.095 Q1 1 0.4589 0.1734 0.5929 11.00000 0.05 2.00 Q2 1 0.0870 -0.3766 1.0480 11.00000 0.05 1.78 Q3 1 0.1963 -0.3152 1.1348 11.00000 0.05 1.14 Q4 1 0.5775 0.0695 0.6902 11.00000 0.05 1.04 Q5 1 0.2263 0.1214 0.5746 11.00000 0.05 0.90 Q6 1 0.5211 0.1000 0.6705 11.00000 0.05 0.87 Q7 1 0.2458 -0.3814 1.1538 11.00000 0.05 0.86 Q8 1 0.2671 -0.0032 0.6044 11.00000 0.05 0.85 Q9 1 0.2969 0.0114 0.5611 11.00000 0.05 0.75 Q10 1 0.2280 0.0796 0.5471 11.00000 0.05 0.75 Q11 1 -0.0081 -0.3640 1.1190 11.00000 0.05 0.68 Q12 1 0.0838 -0.4171 1.0373 11.00000 0.05 0.67 Q13 1 0.7928 0.1251 0.6195 11.00000 0.05 0.63 Q14 1 0.0127 -0.4052 1.0605 11.00000 0.05 0.61 Q15 1 0.1704 0.0549 0.5654 11.00000 0.05 0.61 Q16 1 0.6830 0.0789 0.9281 11.00000 0.05 0.58 Q17 1 0.1772 -0.3526 1.1174 11.00000 0.05 0.57 Q18 1 0.3100 0.3026 0.9240 11.00000 0.05 0.54 Q19 1 0.2862 0.1111 0.5372 11.00000 0.05 0.52 Q20 1 0.6956 0.1662 0.6136 11.00000 0.05 0.50 ; data_asb232 _database_code_depnum_ccdc_archive 'CCDC 895609' #TrackingRef '13191_web_deposit_cif_file_0_NathanielS.Sickerman_1344538304.SuperCif.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H78 Ba F3 Fe N4 O17 S4' _chemical_formula_weight 1385.59 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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 12.9433(6) _cell_length_b 14.8169(7) _cell_length_c 18.2751(8) _cell_angle_alpha 110.9912(5) _cell_angle_beta 91.9057(5) _cell_angle_gamma 105.8683(5) _cell_volume 3113.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.24 _exptl_crystal_description rectangle _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1430 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7528 _exptl_absorpt_correction_T_max 0.8456 _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 37859 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.80 _reflns_number_total 14927 _reflns_number_gt 12832 _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. Hydrogen atoms were included using a riding model. There was one molecule of THF solvent present. The solvent molecule was disordered and included using multiple components, partial site-occupancy-factors, geometric restraints (DFIX) and thermal constraints (EADP). ; _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^)+(0.0571P)^2^+2.2067P] 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 14927 _refine_ls_number_parameters 720 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.035 _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 Fe1 Fe 0.25130(3) 1.21484(3) 0.26514(2) 0.03148(8) Uani 1 1 d . . . Ba1 Ba 0.195151(12) 0.917966(11) 0.252098(9) 0.03671(6) Uani 1 1 d . . . S1 S 0.01433(5) 1.11803(6) 0.30642(4) 0.04168(15) Uani 1 1 d . . . S2 S 0.41441(5) 1.19391(5) 0.39037(4) 0.03649(13) Uani 1 1 d . . . S3 S 0.31296(6) 1.20236(5) 0.08766(4) 0.04135(15) Uani 1 1 d . . . S4 S 0.18703(7) 0.62650(6) 0.21594(5) 0.0555(2) Uani 1 1 d . . . O1 O 0.05019(15) 1.02960(16) 0.27340(13) 0.0468(5) Uani 1 1 d . . . O2 O -0.01085(17) 1.1396(2) 0.38588(12) 0.0570(6) Uani 1 1 d . . . O3 O 0.33498(17) 1.09447(14) 0.36314(12) 0.0485(5) Uani 1 1 d . . . O4 O 0.52035(16) 1.19634(17) 0.36836(12) 0.0503(5) Uani 1 1 d . . . O5 O 0.3262(2) 1.10698(16) 0.08342(12) 0.0553(5) Uani 1 1 d . . . O6 O 0.23073(17) 1.19490(18) 0.02885(13) 0.0559(5) Uani 1 1 d . . . O7 O 0.24847(15) 1.08103(13) 0.21163(10) 0.0359(4) Uani 1 1 d D . . H7 H 0.278(3) 1.079(3) 0.1704(15) 0.088(14) Uiso 1 1 d D . . O8 O -0.0195(3) 0.8222(3) 0.2752(3) 0.1183(15) Uani 1 1 d . . . O9 O 0.0184(3) 0.8195(2) 0.1247(2) 0.1097(14) Uani 1 1 d . . . O10 O 0.2254(4) 0.8314(2) 0.09205(19) 0.1126(14) Uani 1 1 d . . . O11 O 0.4023(3) 0.8961(2) 0.2103(3) 0.1225(16) Uani 1 1 d . . . O12 O 0.3512(3) 0.8931(2) 0.3546(3) 0.1118(15) Uani 1 1 d . . . O13 O 0.1507(4) 0.9041(3) 0.40020(19) 0.1140(14) Uani 1 1 d . . . O14 O 0.1725(2) 0.71692(18) 0.21251(19) 0.0832(9) Uani 1 1 d . . . O15 O 0.1814(2) 0.6175(2) 0.29078(16) 0.0769(8) Uani 1 1 d . . . O16 O 0.2721(2) 0.5957(3) 0.1768(2) 0.0920(9) Uani 1 1 d . . . N1 N 0.2680(2) 1.38390(17) 0.31986(14) 0.0434(5) Uani 1 1 d . . . N2 N 0.10497(18) 1.21203(18) 0.30046(14) 0.0413(5) Uani 1 1 d . . . N3 N 0.36265(18) 1.26389(15) 0.36217(13) 0.0365(4) Uani 1 1 d . . . N4 N 0.29412(19) 1.26305(16) 0.17533(13) 0.0389(5) Uani 1 1 d . . . F1 F 0.0605(3) 0.43889(17) 0.1493(2) 0.1202(12) Uani 1 1 d . . . F2 F -0.0234(2) 0.5488(3) 0.1854(2) 0.1094(10) Uani 1 1 d . . . F3 F 0.0523(2) 0.5307(2) 0.08310(15) 0.0972(8) Uani 1 1 d . . . C1 C 0.1563(3) 1.3909(3) 0.3232(2) 0.0587(8) Uani 1 1 d . . . H1A H 0.1240 1.3826 0.2705 0.070 Uiso 1 1 calc R . . H1B H 0.1585 1.4588 0.3615 0.070 Uiso 1 1 calc R . . C2 C 0.0872(3) 1.3102(3) 0.3481(2) 0.0574(8) Uani 1 1 d . . . H2B H 0.1078 1.3275 0.4052 0.069 Uiso 1 1 calc R . . H2C H 0.0097 1.3051 0.3387 0.069 Uiso 1 1 calc R . . C3 C -0.1066(2) 1.0981(2) 0.24417(15) 0.0398(6) Uani 1 1 d . . . C4 C -0.2028(2) 1.1087(3) 0.27517(17) 0.0513(7) Uani 1 1 d . . . C5 C -0.2939(2) 1.0896(3) 0.22323(18) 0.0527(7) Uani 1 1 d . . . H5A H -0.3583 1.0985 0.2440 0.063 Uiso 1 1 calc R . . C6 C -0.2944(2) 1.0582(3) 0.14268(18) 0.0498(7) Uani 1 1 d . . . C7 C -0.1993(2) 1.0476(2) 0.11354(16) 0.0463(6) Uani 1 1 d . . . H7B H -0.1992 1.0250 0.0579 0.056 Uiso 1 1 calc R . . C8 C -0.1042(2) 1.0684(2) 0.16210(16) 0.0402(6) Uani 1 1 d . . . C9 C -0.2172(3) 1.1388(5) 0.3619(2) 0.105(2) Uani 1 1 d . . . H9A H -0.2902 1.1451 0.3681 0.157 Uiso 1 1 calc R . . H9B H -0.1630 1.2041 0.3932 0.157 Uiso 1 1 calc R . . H9C H -0.2078 1.0868 0.3805 0.157 Uiso 1 1 calc R . . C10 C -0.3956(3) 1.0363(4) 0.0872(2) 0.0743(11) Uani 1 1 d . . . H10A H -0.4590 1.0282 0.1148 0.111 Uiso 1 1 calc R . . H10B H -0.4048 0.9737 0.0409 0.111 Uiso 1 1 calc R . . H10C H -0.3886 1.0928 0.0699 0.111 Uiso 1 1 calc R . . C11 C -0.0053(3) 1.0577(3) 0.12240(18) 0.0550(8) Uani 1 1 d . . . H11A H -0.0281 1.0159 0.0658 0.083 Uiso 1 1 calc R . . H11B H 0.0341 1.0251 0.1466 0.083 Uiso 1 1 calc R . . H11C H 0.0421 1.1250 0.1290 0.083 Uiso 1 1 calc R . . C12 C 0.3333(3) 1.4262(2) 0.39911(18) 0.0544(8) Uani 1 1 d . . . H12A H 0.2854 1.4164 0.4386 0.065 Uiso 1 1 calc R . . H12B H 0.3687 1.5000 0.4147 0.065 Uiso 1 1 calc R . . C13 C 0.4190(3) 1.3737(2) 0.39790(18) 0.0460(6) Uani 1 1 d . . . H13A H 0.4751 1.3931 0.3661 0.055 Uiso 1 1 calc R . . H13B H 0.4547 1.3930 0.4524 0.055 Uiso 1 1 calc R . . C14 C 0.4280(2) 1.2433(2) 0.49672(15) 0.0376(5) Uani 1 1 d . . . C15 C 0.5295(2) 1.27963(18) 0.54451(15) 0.0363(5) Uani 1 1 d . . . C16 C 0.5316(2) 1.3124(2) 0.62712(16) 0.0415(6) Uani 1 1 d . . . H16B H 0.5993 1.3337 0.6598 0.050 Uiso 1 1 calc R . . C17 C 0.4402(3) 1.3147(2) 0.66231(17) 0.0499(7) Uani 1 1 d . . . C18 C 0.3411(3) 1.2791(3) 0.61369(19) 0.0582(8) Uani 1 1 d . . . H18A H 0.2771 1.2805 0.6375 0.070 Uiso 1 1 calc R . . C19 C 0.3320(2) 1.2415(3) 0.53123(18) 0.0496(7) Uani 1 1 d . . . C20 C 0.6383(2) 1.2893(2) 0.51583(18) 0.0481(7) Uani 1 1 d . . . H20A H 0.6476 1.3315 0.4843 0.072 Uiso 1 1 calc R . . H20B H 0.6421 1.2218 0.4831 0.072 Uiso 1 1 calc R . . H20C H 0.6961 1.3210 0.5615 0.072 Uiso 1 1 calc R . . C21 C 0.4462(3) 1.3565(3) 0.75146(19) 0.0667(10) Uani 1 1 d . . . H21A H 0.5210 1.3733 0.7760 0.100 Uiso 1 1 calc R . . H21B H 0.3982 1.3054 0.7676 0.100 Uiso 1 1 calc R . . H21C H 0.4233 1.4177 0.7685 0.100 Uiso 1 1 calc R . . C22 C 0.2191(2) 1.2007(3) 0.4849(2) 0.0675(10) Uani 1 1 d . . . H22A H 0.2187 1.2265 0.4425 0.101 Uiso 1 1 calc R . . H22B H 0.1679 1.2227 0.5204 0.101 Uiso 1 1 calc R . . H22C H 0.1974 1.1263 0.4618 0.101 Uiso 1 1 calc R . . C23 C 0.3219(3) 1.4329(2) 0.26774(19) 0.0520(7) Uani 1 1 d . . . H23A H 0.4016 1.4496 0.2796 0.062 Uiso 1 1 calc R . . H23B H 0.3045 1.4969 0.2774 0.062 Uiso 1 1 calc R . . C24 C 0.2837(3) 1.3628(2) 0.18288(18) 0.0483(7) Uani 1 1 d . . . H24A H 0.2072 1.3564 0.1676 0.058 Uiso 1 1 calc R . . H24B H 0.3286 1.3893 0.1479 0.058 Uiso 1 1 calc R . . C25 C 0.4415(2) 1.2775(2) 0.07507(16) 0.0431(6) Uani 1 1 d . . . C26 C 0.4503(2) 1.3183(3) 0.01614(18) 0.0515(7) Uani 1 1 d . . . C27 C 0.5518(3) 1.3752(3) 0.0100(2) 0.0635(9) Uani 1 1 d . . . H27A H 0.5579 1.4041 -0.0290 0.076 Uiso 1 1 calc R . . C28 C 0.6440(3) 1.3915(3) 0.0588(2) 0.0716(10) Uani 1 1 d . . . C29 C 0.6333(3) 1.3508(3) 0.1160(2) 0.0676(10) Uani 1 1 d . . . H29A H 0.6967 1.3616 0.1497 0.081 Uiso 1 1 calc R . . C30 C 0.5347(3) 1.2950(3) 0.12667(18) 0.0513(7) Uani 1 1 d . . . C31 C 0.3571(3) 1.3055(4) -0.0422(2) 0.0772(12) Uani 1 1 d . . . H31A H 0.3841 1.3412 -0.0770 0.116 Uiso 1 1 calc R . . H31B H 0.3034 1.3338 -0.0134 0.116 Uiso 1 1 calc R . . H31C H 0.3230 1.2331 -0.0742 0.116 Uiso 1 1 calc R . . C32 C 0.7553(4) 1.4510(5) 0.0470(4) 0.115(2) Uani 1 1 d . . . H32A H 0.8007 1.4061 0.0310 0.173 Uiso 1 1 calc R . . H32B H 0.7906 1.5080 0.0967 0.173 Uiso 1 1 calc R . . H32C H 0.7455 1.4768 0.0056 0.173 Uiso 1 1 calc R . . C33 C 0.5323(3) 1.2579(3) 0.1943(2) 0.0661(10) Uani 1 1 d . . . H33A H 0.4876 1.1866 0.1753 0.099 Uiso 1 1 calc R . . H33B H 0.5013 1.2989 0.2373 0.099 Uiso 1 1 calc R . . H33C H 0.6063 1.2641 0.2139 0.099 Uiso 1 1 calc R . . C34 C -0.1044(4) 0.8095(6) 0.2136(7) 0.180(5) Uani 1 1 d . . . H34A H -0.1102 0.8766 0.2185 0.216 Uiso 1 1 calc R . . H34B H -0.1754 0.7684 0.2199 0.216 Uiso 1 1 calc R . . C35 C -0.0759(6) 0.7578(5) 0.1345(7) 0.203(6) Uani 1 1 d . . . H35A H -0.0661 0.6924 0.1306 0.244 Uiso 1 1 calc R . . H35B H -0.1351 0.7438 0.0925 0.244 Uiso 1 1 calc R . . C36 C 0.0462(7) 0.7803(5) 0.0439(3) 0.145(4) Uani 1 1 d . . . H36A H -0.0073 0.7838 0.0058 0.174 Uiso 1 1 calc R . . H36B H 0.0432 0.7084 0.0288 0.174 Uiso 1 1 calc R . . C37 C 0.1567(9) 0.8411(5) 0.0406(3) 0.164(4) Uani 1 1 d . . . H37A H 0.1754 0.8155 -0.0137 0.197 Uiso 1 1 calc R . . H37B H 0.1607 0.9133 0.0555 0.197 Uiso 1 1 calc R . . C38 C 0.3345(8) 0.8627(5) 0.0788(5) 0.164(4) Uani 1 1 d . . . H38A H 0.3591 0.9367 0.0912 0.196 Uiso 1 1 calc R . . H38B H 0.3409 0.8269 0.0227 0.196 Uiso 1 1 calc R . . C39 C 0.4029(7) 0.8367(5) 0.1327(7) 0.193(5) Uani 1 1 d . . . H39A H 0.3730 0.7640 0.1239 0.232 Uiso 1 1 calc R . . H39B H 0.4783 0.8492 0.1206 0.232 Uiso 1 1 calc R . . C40 C 0.4663(4) 0.8719(5) 0.2644(7) 0.165(5) Uani 1 1 d . . . H40A H 0.4389 0.7984 0.2535 0.198 Uiso 1 1 calc R . . H40B H 0.5432 0.8882 0.2557 0.198 Uiso 1 1 calc R . . C41 C 0.4593(5) 0.9279(4) 0.3436(7) 0.178(5) Uani 1 1 d . . . H41A H 0.5084 0.9171 0.3802 0.214 Uiso 1 1 calc R . . H41B H 0.4801 1.0012 0.3539 0.214 Uiso 1 1 calc R . . C42 C 0.3378(7) 0.9324(4) 0.4346(4) 0.171(5) Uani 1 1 d . . . H42A H 0.3486 1.0063 0.4527 0.206 Uiso 1 1 calc R . . H42B H 0.3914 0.9214 0.4677 0.206 Uiso 1 1 calc R . . C43 C 0.2274(8) 0.8794(5) 0.4413(3) 0.159(4) Uani 1 1 d . . . H43A H 0.2152 0.8052 0.4186 0.190 Uiso 1 1 calc R . . H43B H 0.2178 0.8995 0.4978 0.190 Uiso 1 1 calc R . . C44 C 0.0440(9) 0.8508(7) 0.4055(6) 0.188(5) Uani 1 1 d . . . H44A H 0.0304 0.8748 0.4612 0.226 Uiso 1 1 calc R . . H44B H 0.0349 0.7772 0.3870 0.226 Uiso 1 1 calc R . . C45 C -0.0337(7) 0.8695(7) 0.3552(7) 0.187(5) Uani 1 1 d . . . H45A H -0.1091 0.8404 0.3629 0.225 Uiso 1 1 calc R . . H45B H -0.0192 0.9433 0.3695 0.225 Uiso 1 1 calc R . . C46 C 0.0651(3) 0.5307(3) 0.1545(2) 0.0665(10) Uani 1 1 d . . . O17 O 0.1723(14) 1.5031(12) 0.5474(8) 0.223(3) Uiso 0.50 1 d PD A 1 C47 C 0.0606(13) 1.4816(18) 0.5603(10) 0.223(3) Uiso 0.50 1 d PD A 1 H47A H 0.0147 1.4180 0.5180 0.267 Uiso 0.50 1 calc PR A 1 H47B H 0.0320 1.5378 0.5623 0.267 Uiso 0.50 1 calc PR A 1 C48 C 0.0647(14) 1.4708(18) 0.6405(12) 0.223(3) Uiso 0.50 1 d PD A 1 H48A H 0.0030 1.4860 0.6676 0.267 Uiso 0.50 1 calc PR A 1 H48B H 0.0656 1.4021 0.6349 0.267 Uiso 0.50 1 calc PR A 1 C49 C 0.1690(16) 1.5487(17) 0.6826(7) 0.223(3) Uiso 0.50 1 d PD A 1 H49A H 0.1957 1.5387 0.7297 0.267 Uiso 0.50 1 calc PR A 1 H49B H 0.1632 1.6182 0.6988 0.267 Uiso 0.50 1 calc PR A 1 C50 C 0.2412(11) 1.5274(18) 0.6180(12) 0.223(3) Uiso 0.50 1 d PD A 1 H50A H 0.3043 1.5879 0.6276 0.267 Uiso 0.50 1 calc PR A 1 H50B H 0.2677 1.4699 0.6155 0.267 Uiso 0.50 1 calc PR A 1 O18 O 0.0711(11) 1.4240(11) 0.5868(10) 0.223(3) Uiso 0.50 1 d PD B 2 C51 C 0.1532(16) 1.4251(13) 0.6427(13) 0.223(3) Uiso 0.50 1 d PD B 2 H51A H 0.1647 1.3578 0.6275 0.267 Uiso 0.50 1 calc PR B 2 H51B H 0.1336 1.4456 0.6969 0.267 Uiso 0.50 1 calc PR B 2 C52 C 0.2512(11) 1.5024(15) 0.6374(14) 0.223(3) Uiso 0.50 1 d PD B 2 H52A H 0.2814 1.4756 0.5879 0.267 Uiso 0.50 1 calc PR B 2 H52B H 0.3083 1.5264 0.6834 0.267 Uiso 0.50 1 calc PR B 2 C53 C 0.2040(16) 1.5857(10) 0.6379(15) 0.223(3) Uiso 0.50 1 d PD B 2 H53A H 0.2035 1.6313 0.6928 0.267 Uiso 0.50 1 calc PR B 2 H53B H 0.2462 1.6265 0.6101 0.267 Uiso 0.50 1 calc PR B 2 C54 C 0.0937(15) 1.5314(14) 0.5963(14) 0.223(3) Uiso 0.50 1 d PD B 2 H54A H 0.0871 1.5362 0.5438 0.267 Uiso 0.50 1 calc PR B 2 H54B H 0.0414 1.5610 0.6271 0.267 Uiso 0.50 1 calc PR B 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 Fe1 0.03481(18) 0.03157(17) 0.03120(17) 0.01293(14) 0.00487(13) 0.01370(14) Ba1 0.03516(9) 0.03367(8) 0.04205(9) 0.01955(7) -0.00439(6) 0.00600(6) S1 0.0327(3) 0.0633(4) 0.0365(3) 0.0238(3) 0.0069(2) 0.0195(3) S2 0.0386(3) 0.0343(3) 0.0346(3) 0.0117(2) -0.0027(2) 0.0110(2) S3 0.0466(4) 0.0425(3) 0.0336(3) 0.0171(3) 0.0057(3) 0.0081(3) S4 0.0536(4) 0.0386(4) 0.0695(5) 0.0247(4) -0.0193(4) 0.0045(3) O1 0.0350(9) 0.0566(12) 0.0598(12) 0.0334(10) 0.0080(9) 0.0157(9) O2 0.0404(11) 0.1004(18) 0.0373(10) 0.0321(11) 0.0075(8) 0.0245(11) O3 0.0602(12) 0.0338(9) 0.0454(11) 0.0160(8) -0.0146(9) 0.0062(9) O4 0.0452(11) 0.0647(13) 0.0404(10) 0.0126(9) 0.0040(8) 0.0259(10) O5 0.0845(16) 0.0422(11) 0.0414(11) 0.0157(9) 0.0221(11) 0.0217(11) O6 0.0469(11) 0.0671(14) 0.0454(11) 0.0261(11) -0.0025(9) -0.0007(10) O7 0.0440(10) 0.0325(9) 0.0348(9) 0.0149(7) 0.0094(8) 0.0141(7) O8 0.0608(19) 0.093(2) 0.231(5) 0.102(3) 0.042(3) 0.0133(17) O9 0.114(3) 0.0556(16) 0.123(3) 0.0102(17) -0.082(2) 0.0137(17) O10 0.221(5) 0.0597(18) 0.0629(18) 0.0258(15) 0.044(2) 0.047(2) O11 0.073(2) 0.0576(17) 0.259(5) 0.070(3) 0.064(3) 0.0371(16) O12 0.104(2) 0.0474(14) 0.160(3) 0.0408(19) -0.084(2) -0.0031(15) O13 0.203(4) 0.089(2) 0.076(2) 0.0616(19) 0.040(2) 0.043(3) O14 0.094(2) 0.0404(12) 0.109(2) 0.0336(14) -0.0310(17) 0.0098(12) O15 0.0846(18) 0.0723(17) 0.0695(16) 0.0343(14) -0.0228(14) 0.0119(14) O16 0.0574(16) 0.105(2) 0.117(3) 0.045(2) 0.0031(16) 0.0277(16) N1 0.0535(14) 0.0366(11) 0.0432(12) 0.0127(10) 0.0073(10) 0.0220(10) N2 0.0371(11) 0.0470(13) 0.0418(12) 0.0140(10) 0.0084(9) 0.0194(10) N3 0.0415(11) 0.0308(10) 0.0361(11) 0.0126(9) -0.0012(9) 0.0104(9) N4 0.0499(13) 0.0357(11) 0.0375(11) 0.0188(9) 0.0087(9) 0.0163(10) F1 0.117(2) 0.0450(12) 0.164(3) 0.0316(15) -0.068(2) -0.0073(13) F2 0.0564(14) 0.135(3) 0.129(2) 0.059(2) -0.0064(15) 0.0078(15) F3 0.0969(18) 0.107(2) 0.0669(15) 0.0271(14) -0.0276(13) 0.0114(15) C1 0.067(2) 0.0529(18) 0.065(2) 0.0174(16) 0.0126(16) 0.0383(16) C2 0.0578(19) 0.0604(19) 0.0573(19) 0.0146(15) 0.0165(15) 0.0329(16) C3 0.0329(12) 0.0569(16) 0.0331(12) 0.0181(12) 0.0050(10) 0.0183(11) C4 0.0395(14) 0.086(2) 0.0348(13) 0.0234(14) 0.0102(11) 0.0275(15) C5 0.0362(14) 0.084(2) 0.0472(16) 0.0276(16) 0.0119(12) 0.0286(15) C6 0.0386(14) 0.0671(19) 0.0442(15) 0.0201(14) 0.0005(12) 0.0193(14) C7 0.0453(15) 0.0618(18) 0.0326(13) 0.0153(12) 0.0032(11) 0.0216(13) C8 0.0391(13) 0.0503(15) 0.0356(13) 0.0181(12) 0.0078(10) 0.0179(12) C9 0.057(2) 0.230(6) 0.0415(19) 0.044(3) 0.0219(16) 0.075(3) C10 0.0456(18) 0.119(3) 0.0523(19) 0.024(2) -0.0049(15) 0.030(2) C11 0.0495(16) 0.089(2) 0.0393(15) 0.0276(16) 0.0162(13) 0.0363(17) C12 0.078(2) 0.0377(15) 0.0444(16) 0.0087(12) 0.0012(15) 0.0226(15) C13 0.0555(17) 0.0322(13) 0.0444(15) 0.0131(11) -0.0037(13) 0.0076(12) C14 0.0381(13) 0.0397(13) 0.0350(12) 0.0169(11) -0.0007(10) 0.0089(10) C15 0.0385(13) 0.0308(12) 0.0393(13) 0.0135(10) -0.0013(10) 0.0109(10) C16 0.0428(14) 0.0405(14) 0.0393(13) 0.0160(11) -0.0061(11) 0.0102(11) C17 0.0527(17) 0.0589(18) 0.0385(14) 0.0222(13) 0.0021(12) 0.0133(14) C18 0.0424(16) 0.088(2) 0.0447(16) 0.0310(17) 0.0082(13) 0.0127(16) C19 0.0388(14) 0.0657(19) 0.0427(15) 0.0255(14) 0.0028(12) 0.0075(13) C20 0.0394(14) 0.0558(17) 0.0444(15) 0.0114(13) -0.0023(12) 0.0186(13) C21 0.067(2) 0.094(3) 0.0394(16) 0.0258(17) 0.0053(15) 0.025(2) C22 0.0343(15) 0.112(3) 0.0499(18) 0.036(2) 0.0020(13) 0.0070(17) C23 0.070(2) 0.0345(14) 0.0570(18) 0.0214(13) 0.0044(15) 0.0206(13) C24 0.0648(19) 0.0435(15) 0.0503(16) 0.0271(13) 0.0109(14) 0.0249(14) C25 0.0405(14) 0.0524(16) 0.0387(14) 0.0214(12) 0.0053(11) 0.0126(12) C26 0.0441(15) 0.067(2) 0.0463(16) 0.0296(15) 0.0053(12) 0.0110(14) C27 0.0525(18) 0.078(2) 0.062(2) 0.0396(19) 0.0098(16) 0.0056(17) C28 0.0434(18) 0.084(3) 0.077(3) 0.034(2) 0.0072(17) 0.0001(17) C29 0.0445(17) 0.086(3) 0.061(2) 0.0193(19) -0.0083(15) 0.0162(17) C30 0.0474(16) 0.0653(19) 0.0415(15) 0.0178(14) 0.0022(12) 0.0215(14) C31 0.054(2) 0.125(4) 0.070(2) 0.071(3) 0.0028(17) 0.010(2) C32 0.048(2) 0.148(5) 0.133(5) 0.067(4) 0.007(3) -0.012(3) C33 0.066(2) 0.099(3) 0.0495(18) 0.0353(19) 0.0021(16) 0.041(2) C34 0.031(2) 0.113(5) 0.394(16) 0.123(8) -0.012(5) -0.012(3) C35 0.093(5) 0.077(4) 0.358(15) 0.024(6) -0.134(8) 0.002(3) C36 0.240(9) 0.073(3) 0.083(4) -0.007(3) -0.094(5) 0.049(4) C37 0.365(14) 0.071(3) 0.050(3) 0.018(3) 0.009(5) 0.067(6) C38 0.279(10) 0.102(4) 0.174(7) 0.080(5) 0.175(8) 0.104(6) C39 0.223(9) 0.104(4) 0.361(13) 0.144(7) 0.224(10) 0.122(6) C40 0.054(3) 0.068(3) 0.380(15) 0.093(6) 0.003(5) 0.024(3) C41 0.086(4) 0.056(3) 0.360(14) 0.071(5) -0.111(6) 0.001(3) C42 0.241(9) 0.075(3) 0.151(6) 0.062(4) -0.145(6) -0.029(4) C43 0.299(11) 0.094(4) 0.069(3) 0.050(3) -0.053(5) 0.023(5) C44 0.280(12) 0.175(7) 0.205(9) 0.157(7) 0.146(9) 0.090(8) C45 0.161(7) 0.190(8) 0.317(13) 0.187(9) 0.174(9) 0.079(6) C46 0.060(2) 0.0539(19) 0.079(2) 0.0292(18) -0.0224(18) 0.0061(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 Fe1 O7 1.8594(17) . ? Fe1 N2 2.016(2) . ? Fe1 N3 2.021(2) . ? Fe1 N4 2.048(2) . ? Fe1 N1 2.284(2) . ? Ba1 O7 2.6951(17) . ? Ba1 O14 2.729(2) . ? Ba1 O3 2.7565(19) . ? Ba1 O1 2.7734(19) . ? Ba1 O10 2.831(3) . ? Ba1 O13 2.853(3) . ? Ba1 O9 2.858(3) . ? Ba1 O8 2.874(3) . ? Ba1 O11 2.883(3) . ? Ba1 O12 2.894(3) . ? S1 O2 1.440(2) . ? S1 O1 1.443(2) . ? S1 N2 1.597(3) . ? S1 C3 1.795(3) . ? S2 O4 1.436(2) . ? S2 O3 1.445(2) . ? S2 N3 1.590(2) . ? S2 C14 1.798(3) . ? S3 O6 1.440(2) . ? S3 O5 1.445(2) . ? S3 N4 1.596(2) . ? S3 C25 1.804(3) . ? S4 O15 1.423(3) . ? S4 O16 1.423(3) . ? S4 O14 1.425(2) . ? S4 C46 1.812(3) . ? O5 H7 1.868(13) . ? O8 C45 1.421(11) . ? O8 C34 1.471(9) . ? O9 C35 1.371(11) . ? O9 C36 1.478(9) . ? O10 C37 1.344(9) . ? O10 C38 1.419(9) . ? O11 C39 1.378(10) . ? O11 C40 1.468(9) . ? O12 C41 1.401(9) . ? O12 C42 1.403(10) . ? O13 C44 1.416(10) . ? O13 C43 1.424(8) . ? N1 C12 1.477(4) . ? N1 C23 1.478(4) . ? N1 C1 1.479(4) . ? N2 C2 1.488(4) . ? N3 C13 1.471(3) . ? N4 C24 1.478(3) . ? F1 C46 1.315(4) . ? F2 C46 1.344(5) . ? F3 C46 1.308(4) . ? C1 C2 1.507(5) . ? C3 C8 1.408(4) . ? C3 C4 1.409(4) . ? C4 C5 1.386(4) . ? C4 C9 1.518(4) . ? C5 C6 1.375(4) . ? C6 C7 1.383(4) . ? C6 C10 1.514(4) . ? C7 C8 1.386(4) . ? C8 C11 1.510(4) . ? C12 C13 1.516(4) . ? C14 C15 1.407(3) . ? C14 C19 1.410(4) . ? C15 C16 1.407(4) . ? C15 C20 1.507(4) . ? C16 C17 1.369(4) . ? C17 C18 1.389(4) . ? C17 C21 1.512(4) . ? C18 C19 1.395(4) . ? C19 C22 1.513(4) . ? C23 C24 1.498(4) . ? C25 C26 1.405(4) . ? C25 C30 1.411(4) . ? C26 C27 1.386(4) . ? C26 C31 1.508(4) . ? C27 C28 1.377(5) . ? C28 C29 1.375(6) . ? C28 C32 1.536(5) . ? C29 C30 1.380(5) . ? C30 C33 1.521(5) . ? C34 C35 1.485(14) . ? C36 C37 1.484(12) . ? C38 C39 1.518(13) . ? C40 C41 1.406(13) . ? C42 C43 1.463(11) . ? C44 C45 1.485(13) . ? O17 C50 1.415(9) . ? O17 C47 1.439(9) . ? C47 C48 1.531(9) . ? C48 C49 1.479(10) . ? C49 C50 1.527(9) . ? O18 C51 1.441(9) . ? O18 C54 1.481(9) . ? C51 C52 1.491(9) . ? C52 C53 1.517(9) . ? C53 C54 1.457(9) . ? 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 Fe1 N2 107.44(9) . . ? O7 Fe1 N3 103.49(8) . . ? N2 Fe1 N3 108.37(9) . . ? O7 Fe1 N4 96.38(8) . . ? N2 Fe1 N4 120.05(9) . . ? N3 Fe1 N4 118.34(9) . . ? O7 Fe1 N1 172.87(8) . . ? N2 Fe1 N1 78.41(9) . . ? N3 Fe1 N1 77.95(8) . . ? N4 Fe1 N1 76.95(9) . . ? O7 Ba1 O14 148.37(8) . . ? O7 Ba1 O3 63.52(6) . . ? O14 Ba1 O3 133.71(7) . . ? O7 Ba1 O1 63.05(5) . . ? O14 Ba1 O1 133.94(8) . . ? O3 Ba1 O1 84.15(6) . . ? O7 Ba1 O10 77.99(7) . . ? O14 Ba1 O10 70.62(9) . . ? O3 Ba1 O10 124.35(10) . . ? O1 Ba1 O10 113.29(10) . . ? O7 Ba1 O13 130.09(8) . . ? O14 Ba1 O13 81.24(10) . . ? O3 Ba1 O13 75.90(9) . . ? O1 Ba1 O13 86.02(10) . . ? O10 Ba1 O13 151.85(9) . . ? O7 Ba1 O9 89.77(8) . . ? O14 Ba1 O9 76.81(8) . . ? O3 Ba1 O9 149.48(7) . . ? O1 Ba1 O9 69.89(8) . . ? O10 Ba1 O9 57.49(14) . . ? O13 Ba1 O9 116.50(14) . . ? O7 Ba1 O8 124.37(8) . . ? O14 Ba1 O8 72.36(10) . . ? O3 Ba1 O8 123.70(12) . . ? O1 Ba1 O8 63.40(8) . . ? O10 Ba1 O8 110.83(15) . . ? O13 Ba1 O8 58.22(14) . . ? O9 Ba1 O8 58.42(15) . . ? O7 Ba1 O11 85.73(8) . . ? O14 Ba1 O11 74.90(9) . . ? O3 Ba1 O11 79.01(10) . . ? O1 Ba1 O11 148.65(7) . . ? O10 Ba1 O11 58.59(15) . . ? O13 Ba1 O11 114.73(14) . . ? O9 Ba1 O11 115.41(14) . . ? O8 Ba1 O11 147.20(9) . . ? O7 Ba1 O12 119.66(7) . . ? O14 Ba1 O12 69.71(8) . . ? O3 Ba1 O12 64.02(7) . . ? O1 Ba1 O12 135.67(10) . . ? O10 Ba1 O12 110.13(14) . . ? O13 Ba1 O12 57.89(14) . . ? O9 Ba1 O12 146.50(8) . . ? O8 Ba1 O12 108.53(12) . . ? O11 Ba1 O12 56.89(14) . . ? O2 S1 O1 115.10(14) . . ? O2 S1 N2 111.54(14) . . ? O1 S1 N2 107.58(12) . . ? O2 S1 C3 107.54(12) . . ? O1 S1 C3 107.73(13) . . ? N2 S1 C3 107.00(13) . . ? O4 S2 O3 115.60(13) . . ? O4 S2 N3 112.81(13) . . ? O3 S2 N3 107.14(12) . . ? O4 S2 C14 107.96(12) . . ? O3 S2 C14 106.17(12) . . ? N3 S2 C14 106.61(12) . . ? O6 S3 O5 115.40(14) . . ? O6 S3 N4 111.69(13) . . ? O5 S3 N4 108.89(12) . . ? O6 S3 C25 107.96(13) . . ? O5 S3 C25 106.93(14) . . ? N4 S3 C25 105.38(13) . . ? O15 S4 O16 114.21(19) . . ? O15 S4 O14 115.75(19) . . ? O16 S4 O14 115.3(2) . . ? O15 S4 C46 103.64(18) . . ? O16 S4 C46 103.4(2) . . ? O14 S4 C46 101.88(16) . . ? S1 O1 Ba1 156.12(12) . . ? S2 O3 Ba1 155.45(12) . . ? S3 O5 H7 109.9(13) . . ? Fe1 O7 Ba1 131.97(8) . . ? C45 O8 C34 117.0(6) . . ? C45 O8 Ba1 109.6(4) . . ? C34 O8 Ba1 112.9(4) . . ? C35 O9 C36 112.8(6) . . ? C35 O9 Ba1 119.0(5) . . ? C36 O9 Ba1 116.8(4) . . ? C37 O10 C38 111.5(6) . . ? C37 O10 Ba1 113.8(4) . . ? C38 O10 Ba1 113.9(4) . . ? C39 O11 C40 110.6(5) . . ? C39 O11 Ba1 116.3(5) . . ? C40 O11 Ba1 116.2(4) . . ? C41 O12 C42 111.9(5) . . ? C41 O12 Ba1 114.3(4) . . ? C42 O12 Ba1 112.4(4) . . ? C44 O13 C43 109.6(5) . . ? C44 O13 Ba1 118.3(5) . . ? C43 O13 Ba1 117.4(4) . . ? S4 O14 Ba1 160.27(17) . . ? C12 N1 C23 111.3(3) . . ? C12 N1 C1 112.7(2) . . ? C23 N1 C1 110.1(2) . . ? C12 N1 Fe1 107.65(16) . . ? C23 N1 Fe1 108.61(17) . . ? C1 N1 Fe1 106.31(18) . . ? C2 N2 S1 111.5(2) . . ? C2 N2 Fe1 118.3(2) . . ? S1 N2 Fe1 127.76(13) . . ? C13 N3 S2 116.33(18) . . ? C13 N3 Fe1 116.53(16) . . ? S2 N3 Fe1 125.40(12) . . ? C24 N4 S3 110.59(17) . . ? C24 N4 Fe1 117.13(17) . . ? S3 N4 Fe1 130.77(12) . . ? N1 C1 C2 110.5(3) . . ? N2 C2 C1 108.0(2) . . ? C8 C3 C4 120.2(2) . . ? C8 C3 S1 117.99(19) . . ? C4 C3 S1 121.8(2) . . ? C5 C4 C3 118.5(3) . . ? C5 C4 C9 115.7(3) . . ? C3 C4 C9 125.7(3) . . ? C6 C5 C4 122.4(3) . . ? C5 C6 C7 118.0(3) . . ? C5 C6 C10 121.3(3) . . ? C7 C6 C10 120.7(3) . . ? C6 C7 C8 122.8(3) . . ? C7 C8 C3 118.0(2) . . ? C7 C8 C11 117.0(2) . . ? C3 C8 C11 125.0(2) . . ? N1 C12 C13 109.9(2) . . ? N3 C13 C12 106.6(2) . . ? C15 C14 C19 120.6(2) . . ? C15 C14 S2 122.0(2) . . ? C19 C14 S2 117.4(2) . . ? C14 C15 C16 117.9(2) . . ? C14 C15 C20 126.1(2) . . ? C16 C15 C20 116.0(2) . . ? C17 C16 C15 122.7(3) . . ? C16 C17 C18 118.1(3) . . ? C16 C17 C21 121.3(3) . . ? C18 C17 C21 120.6(3) . . ? C17 C18 C19 122.5(3) . . ? C18 C19 C14 118.2(3) . . ? C18 C19 C22 117.4(3) . . ? C14 C19 C22 124.5(3) . . ? N1 C23 C24 109.6(2) . . ? N4 C24 C23 107.2(2) . . ? C26 C25 C30 120.0(3) . . ? C26 C25 S3 121.9(2) . . ? C30 C25 S3 118.0(2) . . ? C27 C26 C25 118.7(3) . . ? C27 C26 C31 116.2(3) . . ? C25 C26 C31 125.2(3) . . ? C28 C27 C26 122.1(3) . . ? C29 C28 C27 118.1(3) . . ? C29 C28 C32 121.9(4) . . ? C27 C28 C32 120.0(4) . . ? C28 C29 C30 123.0(3) . . ? C29 C30 C25 118.0(3) . . ? C29 C30 C33 118.3(3) . . ? C25 C30 C33 123.7(3) . . ? O8 C34 C35 109.0(6) . . ? O9 C35 C34 108.9(5) . . ? O9 C36 C37 110.1(4) . . ? O10 C37 C36 106.7(5) . . ? O10 C38 C39 107.1(5) . . ? O11 C39 C38 109.0(4) . . ? C41 C40 O11 110.3(5) . . ? O12 C41 C40 106.8(5) . . ? O12 C42 C43 107.5(4) . . ? O13 C43 C42 110.0(4) . . ? O13 C44 C45 108.3(5) . . ? O8 C45 C44 107.3(7) . . ? F3 C46 F1 109.2(4) . . ? F3 C46 F2 105.1(3) . . ? F1 C46 F2 106.1(4) . . ? F3 C46 S4 113.0(3) . . ? F1 C46 S4 112.6(2) . . ? F2 C46 S4 110.3(3) . . ? C50 O17 C47 110.4(6) . . ? O17 C47 C48 103.4(6) . . ? C49 C48 C47 100.9(7) . . ? C48 C49 C50 100.6(7) . . ? O17 C50 C49 104.0(7) . . ? C51 O18 C54 104.9(7) . . ? O18 C51 C52 102.7(8) . . ? C51 C52 C53 101.1(7) . . ? C54 C53 C52 104.2(6) . . ? C53 C54 O18 107.4(5) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.837 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.070 _iucr_refine_instructions_details ; TITL asb232 in P-1 CELL 0.71073 12.9433 14.8169 18.2751 110.9912 91.9057 105.8683 ZERR 2.00 0.0006 0.0007 0.0008 0.0005 0.0005 0.0005 LATT 1 SFAC C H N O F S FE BA UNIT 100 156 8 34 6 8 2 2 TEMP -185.000 SIZE 0.162 0.279 0.281 EADP O17 > C54 DFIX 1.453 0.01 O17 C47 O17 C50 DFIX 1.520 0.01 C47 C48 C48 C49 C49 C50 DFIX 2.320 0.01 C47 C49 C48 C50 C50 C47 DFIX 2.320 0.01 O17 C48 O17 C49 DFIX 1.453 0.01 O18 C51 O18 C54 DFIX 1.520 0.01 C51 C52 C52 C53 C53 C54 DFIX 2.320 0.01 C51 C53 C52 C54 C54 C51 DFIX 2.320 0.01 O18 C52 O18 C53 DFIX 0.85 0.001 O7 H7 BIND O5 H7 CONN 10 BA1 CONN 5 FE1 L.S. 12 ACTA 51 WGHT 0.057100 2.206700 FVAR 0.07920 FE1 7 0.251303 1.214845 0.265143 11.00000 0.03481 0.03157 = 0.03120 0.01293 0.00487 0.01370 BA1 8 0.195151 0.917966 0.252098 11.00000 0.03516 0.03367 = 0.04205 0.01955 -0.00439 0.00600 S1 6 0.014330 1.118034 0.306421 11.00000 0.03266 0.06329 = 0.03650 0.02377 0.00689 0.01955 S2 6 0.414408 1.193910 0.390366 11.00000 0.03863 0.03429 = 0.03463 0.01175 -0.00267 0.01101 S3 6 0.312959 1.202364 0.087661 11.00000 0.04663 0.04247 = 0.03355 0.01706 0.00571 0.00808 S4 6 0.187033 0.626504 0.215944 11.00000 0.05359 0.03857 = 0.06953 0.02469 -0.01931 0.00454 O1 4 0.050194 1.029596 0.273401 11.00000 0.03501 0.05658 = 0.05985 0.03341 0.00799 0.01567 O2 4 -0.010852 1.139566 0.385880 11.00000 0.04041 0.10042 = 0.03734 0.03208 0.00749 0.02446 O3 4 0.334984 1.094467 0.363142 11.00000 0.06023 0.03377 = 0.04539 0.01596 -0.01458 0.00617 O4 4 0.520351 1.196338 0.368356 11.00000 0.04519 0.06465 = 0.04038 0.01263 0.00399 0.02586 O5 4 0.326195 1.106984 0.083418 11.00000 0.08450 0.04223 = 0.04139 0.01569 0.02214 0.02166 O6 4 0.230730 1.194905 0.028846 11.00000 0.04692 0.06713 = 0.04535 0.02614 -0.00254 -0.00070 O7 4 0.248468 1.081031 0.211627 11.00000 0.04399 0.03247 = 0.03485 0.01494 0.00943 0.01409 H7 2 0.277839 1.078796 0.170360 11.00000 0.08758 O8 4 -0.019471 0.822239 0.275175 11.00000 0.06083 0.09320 = 0.23088 0.10224 0.04209 0.01329 O9 4 0.018409 0.819482 0.124678 11.00000 0.11385 0.05564 = 0.12334 0.01024 -0.08206 0.01370 O10 4 0.225418 0.831444 0.092047 11.00000 0.22135 0.05967 = 0.06292 0.02582 0.04381 0.04659 O11 4 0.402307 0.896072 0.210331 11.00000 0.07315 0.05756 = 0.25943 0.07019 0.06397 0.03714 O12 4 0.351210 0.893059 0.354573 11.00000 0.10414 0.04740 = 0.16018 0.04081 -0.08446 -0.00309 O13 4 0.150666 0.904058 0.400198 11.00000 0.20346 0.08904 = 0.07635 0.06165 0.04010 0.04329 O14 4 0.172531 0.716923 0.212506 11.00000 0.09367 0.04037 = 0.10938 0.03360 -0.03099 0.00979 O15 4 0.181391 0.617544 0.290776 11.00000 0.08463 0.07233 = 0.06953 0.03429 -0.02284 0.01188 O16 4 0.272104 0.595720 0.176770 11.00000 0.05742 0.10527 = 0.11698 0.04549 0.00311 0.02766 N1 3 0.268038 1.383904 0.319859 11.00000 0.05349 0.03664 = 0.04319 0.01268 0.00730 0.02201 N2 3 0.104975 1.212031 0.300456 11.00000 0.03711 0.04697 = 0.04180 0.01403 0.00843 0.01935 N3 3 0.362648 1.263888 0.362174 11.00000 0.04149 0.03075 = 0.03613 0.01260 -0.00122 0.01044 N4 3 0.294115 1.263051 0.175331 11.00000 0.04991 0.03567 = 0.03747 0.01885 0.00873 0.01626 F1 5 0.060544 0.438886 0.149338 11.00000 0.11713 0.04496 = 0.16381 0.03160 -0.06769 -0.00734 F2 5 -0.023432 0.548827 0.185433 11.00000 0.05635 0.13528 = 0.12854 0.05895 -0.00641 0.00785 F3 5 0.052335 0.530656 0.083100 11.00000 0.09692 0.10676 = 0.06693 0.02713 -0.02762 0.01141 C1 1 0.156349 1.390945 0.323216 11.00000 0.06729 0.05285 = 0.06475 0.01741 0.01264 0.03834 AFIX 23 H1A 2 0.124001 1.382640 0.270456 11.00000 -1.20000 H1B 2 0.158482 1.458799 0.361456 11.00000 -1.20000 AFIX 0 C2 1 0.087202 1.310184 0.348078 11.00000 0.05778 0.06037 = 0.05727 0.01457 0.01649 0.03293 AFIX 23 H2B 2 0.107789 1.327459 0.405231 11.00000 -1.20000 H2C 2 0.009663 1.305073 0.338686 11.00000 -1.20000 AFIX 0 C3 1 -0.106649 1.098109 0.244167 11.00000 0.03291 0.05689 = 0.03315 0.01806 0.00496 0.01829 C4 1 -0.202830 1.108739 0.275168 11.00000 0.03945 0.08566 = 0.03482 0.02342 0.01018 0.02750 C5 1 -0.293898 1.089606 0.223227 11.00000 0.03615 0.08405 = 0.04724 0.02756 0.01186 0.02860 AFIX 43 H5A 2 -0.358321 1.098483 0.244038 11.00000 -1.20000 AFIX 0 C6 1 -0.294411 1.058245 0.142675 11.00000 0.03858 0.06709 = 0.04417 0.02006 0.00048 0.01930 C7 1 -0.199313 1.047570 0.113538 11.00000 0.04530 0.06179 = 0.03260 0.01531 0.00317 0.02164 AFIX 43 H7B 2 -0.199175 1.025013 0.057901 11.00000 -1.20000 AFIX 0 C8 1 -0.104209 1.068399 0.162097 11.00000 0.03913 0.05027 = 0.03559 0.01809 0.00775 0.01787 C9 1 -0.217209 1.138841 0.361901 11.00000 0.05654 0.23010 = 0.04148 0.04393 0.02195 0.07453 AFIX 137 H9A 2 -0.290173 1.145065 0.368083 11.00000 -1.50000 H9B 2 -0.162963 1.204089 0.393160 11.00000 -1.50000 H9C 2 -0.207773 1.086802 0.380452 11.00000 -1.50000 AFIX 0 C10 1 -0.395646 1.036305 0.087180 11.00000 0.04559 0.11940 = 0.05226 0.02424 -0.00495 0.02956 AFIX 137 H10A 2 -0.459033 1.028151 0.114842 11.00000 -1.50000 H10B 2 -0.404770 0.973721 0.040918 11.00000 -1.50000 H10C 2 -0.388643 1.092846 0.069871 11.00000 -1.50000 AFIX 0 C11 1 -0.005346 1.057666 0.122396 11.00000 0.04954 0.08938 = 0.03928 0.02759 0.01621 0.03634 AFIX 137 H11A 2 -0.028067 1.015904 0.065816 11.00000 -1.50000 H11B 2 0.034089 1.025144 0.146592 11.00000 -1.50000 H11C 2 0.042110 1.124982 0.129010 11.00000 -1.50000 AFIX 0 C12 1 0.333306 1.426220 0.399113 11.00000 0.07752 0.03770 = 0.04439 0.00867 0.00123 0.02257 AFIX 23 H12A 2 0.285447 1.416425 0.438564 11.00000 -1.20000 H12B 2 0.368650 1.499997 0.414714 11.00000 -1.20000 AFIX 0 C13 1 0.419042 1.373718 0.397903 11.00000 0.05551 0.03222 = 0.04439 0.01310 -0.00372 0.00762 AFIX 23 H13A 2 0.475079 1.393134 0.366110 11.00000 -1.20000 H13B 2 0.454714 1.392982 0.452396 11.00000 -1.20000 AFIX 0 C14 1 0.427986 1.243268 0.496721 11.00000 0.03807 0.03967 = 0.03496 0.01685 -0.00065 0.00894 C15 1 0.529528 1.279626 0.544508 11.00000 0.03845 0.03080 = 0.03930 0.01349 -0.00130 0.01085 C16 1 0.531611 1.312353 0.627121 11.00000 0.04278 0.04047 = 0.03935 0.01598 -0.00610 0.01018 AFIX 43 H16B 2 0.599288 1.333685 0.659804 11.00000 -1.20000 AFIX 0 C17 1 0.440156 1.314714 0.662314 11.00000 0.05269 0.05886 = 0.03851 0.02216 0.00208 0.01335 C18 1 0.341111 1.279147 0.613693 11.00000 0.04237 0.08805 = 0.04465 0.03103 0.00820 0.01271 AFIX 43 H18A 2 0.277125 1.280506 0.637506 11.00000 -1.20000 AFIX 0 C19 1 0.332039 1.241513 0.531230 11.00000 0.03879 0.06566 = 0.04273 0.02546 0.00284 0.00750 C20 1 0.638339 1.289320 0.515834 11.00000 0.03942 0.05581 = 0.04444 0.01142 -0.00225 0.01859 AFIX 137 H20A 2 0.647632 1.331517 0.484257 11.00000 -1.50000 H20B 2 0.642059 1.221789 0.483145 11.00000 -1.50000 H20C 2 0.696085 1.320958 0.561454 11.00000 -1.50000 AFIX 0 C21 1 0.446191 1.356457 0.751462 11.00000 0.06717 0.09367 = 0.03940 0.02581 0.00533 0.02463 AFIX 137 H21A 2 0.521011 1.373317 0.776042 11.00000 -1.50000 H21B 2 0.398206 1.305370 0.767585 11.00000 -1.50000 H21C 2 0.423267 1.417740 0.768542 11.00000 -1.50000 AFIX 0 C22 1 0.219059 1.200659 0.484918 11.00000 0.03428 0.11248 = 0.04987 0.03625 0.00197 0.00699 AFIX 137 H22A 2 0.218658 1.226504 0.442521 11.00000 -1.50000 H22B 2 0.167950 1.222692 0.520437 11.00000 -1.50000 H22C 2 0.197369 1.126311 0.461788 11.00000 -1.50000 AFIX 0 C23 1 0.321854 1.432946 0.267745 11.00000 0.07044 0.03454 = 0.05698 0.02136 0.00442 0.02059 AFIX 23 H23A 2 0.401566 1.449569 0.279622 11.00000 -1.20000 H23B 2 0.304468 1.496938 0.277421 11.00000 -1.20000 AFIX 0 C24 1 0.283728 1.362792 0.182876 11.00000 0.06480 0.04347 = 0.05034 0.02714 0.01091 0.02494 AFIX 23 H24A 2 0.207167 1.356384 0.167601 11.00000 -1.20000 H24B 2 0.328641 1.389304 0.147915 11.00000 -1.20000 AFIX 0 C25 1 0.441481 1.277469 0.075066 11.00000 0.04049 0.05239 = 0.03871 0.02139 0.00529 0.01258 C26 1 0.450292 1.318263 0.016139 11.00000 0.04410 0.06705 = 0.04626 0.02955 0.00534 0.01095 C27 1 0.551773 1.375250 0.010041 11.00000 0.05247 0.07802 = 0.06205 0.03955 0.00983 0.00564 AFIX 43 H27A 2 0.557887 1.404064 -0.029044 11.00000 -1.20000 AFIX 0 C28 1 0.644029 1.391455 0.058807 11.00000 0.04337 0.08410 = 0.07715 0.03367 0.00724 0.00009 C29 1 0.633296 1.350772 0.115988 11.00000 0.04450 0.08599 = 0.06092 0.01932 -0.00832 0.01621 AFIX 43 H29A 2 0.696676 1.361553 0.149713 11.00000 -1.20000 AFIX 0 C30 1 0.534741 1.295005 0.126671 11.00000 0.04742 0.06529 = 0.04146 0.01780 0.00223 0.02145 C31 1 0.357054 1.305483 -0.042214 11.00000 0.05417 0.12486 = 0.07007 0.07109 0.00276 0.00962 AFIX 137 H31A 2 0.384143 1.341219 -0.076950 11.00000 -1.50000 H31B 2 0.303398 1.333790 -0.013434 11.00000 -1.50000 H31C 2 0.323032 1.233134 -0.074178 11.00000 -1.50000 AFIX 0 C32 1 0.755261 1.450979 0.046977 11.00000 0.04848 0.14779 = 0.13336 0.06741 0.00705 -0.01212 AFIX 137 H32A 2 0.800707 1.406063 0.031021 11.00000 -1.50000 H32B 2 0.790557 1.508036 0.096721 11.00000 -1.50000 H32C 2 0.745471 1.476807 0.005643 11.00000 -1.50000 AFIX 0 C33 1 0.532251 1.257856 0.194312 11.00000 0.06628 0.09857 = 0.04950 0.03533 0.00212 0.04118 AFIX 137 H33A 2 0.487574 1.186572 0.175299 11.00000 -1.50000 H33B 2 0.501273 1.298942 0.237303 11.00000 -1.50000 H33C 2 0.606300 1.264115 0.213923 11.00000 -1.50000 AFIX 0 C34 1 -0.104389 0.809490 0.213555 11.00000 0.03094 0.11327 = 0.39397 0.12275 -0.01222 -0.01174 AFIX 23 H34A 2 -0.110152 0.876632 0.218493 11.00000 -1.20000 H34B 2 -0.175367 0.768407 0.219921 11.00000 -1.20000 AFIX 0 C35 1 -0.075909 0.757830 0.134506 11.00000 0.09294 0.07723 = 0.35849 0.02376 -0.13412 0.00156 AFIX 23 H35A 2 -0.066133 0.692379 0.130643 11.00000 -1.20000 H35B 2 -0.135135 0.743809 0.092481 11.00000 -1.20000 AFIX 0 C36 1 0.046223 0.780312 0.043863 11.00000 0.23994 0.07274 = 0.08281 -0.00668 -0.09439 0.04939 AFIX 23 H36A 2 -0.007251 0.783801 0.005752 11.00000 -1.20000 H36B 2 0.043229 0.708360 0.028751 11.00000 -1.20000 AFIX 0 C37 1 0.156732 0.841104 0.040552 11.00000 0.36465 0.07073 = 0.05037 0.01790 0.00946 0.06688 AFIX 23 H37A 2 0.175368 0.815544 -0.013658 11.00000 -1.20000 H37B 2 0.160729 0.913271 0.055528 11.00000 -1.20000 AFIX 0 C38 1 0.334535 0.862722 0.078771 11.00000 0.27885 0.10206 = 0.17432 0.08002 0.17530 0.10434 AFIX 23 H38A 2 0.359090 0.936697 0.091233 11.00000 -1.20000 H38B 2 0.340946 0.826880 0.022658 11.00000 -1.20000 AFIX 0 C39 1 0.402934 0.836691 0.132664 11.00000 0.22301 0.10371 = 0.36121 0.14362 0.22389 0.12204 AFIX 23 H39A 2 0.373023 0.764004 0.123944 11.00000 -1.20000 H39B 2 0.478314 0.849202 0.120555 11.00000 -1.20000 AFIX 0 C40 1 0.466328 0.871869 0.264444 11.00000 0.05415 0.06849 = 0.37958 0.09261 0.00301 0.02395 AFIX 23 H40A 2 0.438882 0.798359 0.253491 11.00000 -1.20000 H40B 2 0.543168 0.888161 0.255678 11.00000 -1.20000 AFIX 0 C41 1 0.459308 0.927851 0.343552 11.00000 0.08577 0.05638 = 0.36015 0.07109 -0.11100 0.00069 AFIX 23 H41A 2 0.508442 0.917132 0.380152 11.00000 -1.20000 H41B 2 0.480136 1.001239 0.353864 11.00000 -1.20000 AFIX 0 C42 1 0.337795 0.932403 0.434566 11.00000 0.24101 0.07519 = 0.15099 0.06177 -0.14535 -0.02947 AFIX 23 H42A 2 0.348610 1.006251 0.452678 11.00000 -1.20000 H42B 2 0.391420 0.921379 0.467705 11.00000 -1.20000 AFIX 0 C43 1 0.227422 0.879445 0.441296 11.00000 0.29924 0.09372 = 0.06922 0.05018 -0.05292 0.02260 AFIX 23 H43A 2 0.215189 0.805224 0.418608 11.00000 -1.20000 H43B 2 0.217827 0.899541 0.497837 11.00000 -1.20000 AFIX 0 C44 1 0.043996 0.850811 0.405497 11.00000 0.27982 0.17500 = 0.20472 0.15676 0.14566 0.09044 AFIX 23 H44A 2 0.030378 0.874778 0.461184 11.00000 -1.20000 H44B 2 0.034883 0.777219 0.386989 11.00000 -1.20000 AFIX 0 C45 1 -0.033728 0.869496 0.355223 11.00000 0.16112 0.19008 = 0.31705 0.18698 0.17448 0.07942 AFIX 23 H45A 2 -0.109139 0.840399 0.362859 11.00000 -1.20000 H45B 2 -0.019199 0.943340 0.369537 11.00000 -1.20000 AFIX 0 C46 1 0.065093 0.530740 0.154455 11.00000 0.06009 0.05385 = 0.07920 0.02922 -0.02244 0.00608 PART 1 O17 4 0.172273 1.503125 0.547448 10.50000 0.22268 C47 1 0.060567 1.481579 0.560293 10.50000 0.22268 AFIX 23 H47A 2 0.014654 1.417955 0.518013 10.50000 -1.20000 H47B 2 0.032022 1.537833 0.562289 10.50000 -1.20000 AFIX 0 C48 1 0.064748 1.470833 0.640514 10.50000 0.22268 AFIX 23 H48A 2 0.002958 1.485964 0.667619 10.50000 -1.20000 H48B 2 0.065624 1.402086 0.634936 10.50000 -1.20000 AFIX 0 C49 1 0.169035 1.548688 0.682585 10.50000 0.22268 AFIX 23 H49A 2 0.195688 1.538744 0.729672 10.50000 -1.20000 H49B 2 0.163202 1.618216 0.698808 10.50000 -1.20000 AFIX 0 C50 1 0.241194 1.527401 0.617990 10.50000 0.22268 AFIX 23 H50A 2 0.304317 1.587946 0.627568 10.50000 -1.20000 H50B 2 0.267738 1.469863 0.615472 10.50000 -1.20000 AFIX 0 PART 2 O18 4 0.071115 1.423988 0.586842 10.50000 0.22268 C51 1 0.153182 1.425136 0.642732 10.50000 0.22268 AFIX 23 H51A 2 0.164686 1.357796 0.627457 10.50000 -1.20000 H51B 2 0.133596 1.445618 0.696908 10.50000 -1.20000 AFIX 0 C52 1 0.251201 1.502391 0.637402 10.50000 0.22268 AFIX 23 H52A 2 0.281391 1.475642 0.587878 10.50000 -1.20000 H52B 2 0.308289 1.526355 0.683401 10.50000 -1.20000 AFIX 0 C53 1 0.203970 1.585686 0.637911 10.50000 0.22268 AFIX 23 H53A 2 0.203494 1.631258 0.692817 10.50000 -1.20000 H53B 2 0.246171 1.626460 0.610083 10.50000 -1.20000 AFIX 0 C54 1 0.093708 1.531413 0.596286 10.50000 0.22268 AFIX 23 H54A 2 0.087079 1.536246 0.543787 10.50000 -1.20000 H54B 2 0.041359 1.561030 0.627125 10.50000 -1.20000 PART 0 HKLF 4 REM asb232 in P-1 REM R1 = 0.0370 for 12832 Fo > 4sig(Fo) and 0.0444 for all 14927 data REM 720 parameters refined using 21 restraints END WGHT 0.0571 2.2066 REM Highest difference peak 0.837, deepest hole -0.605, 1-sigma level 0.070 Q1 1 0.1955 1.4929 0.6778 11.00000 0.05 0.84 Q2 1 0.1954 1.4370 0.5713 11.00000 0.05 0.77 Q3 1 0.1801 0.9455 0.2920 11.00000 0.05 0.66 Q4 1 0.3675 0.8762 0.1709 11.00000 0.05 0.64 Q5 1 0.1362 1.5660 0.6781 11.00000 0.05 0.57 Q6 1 0.1399 1.5645 0.5750 11.00000 0.05 0.57 Q7 1 0.1411 1.3998 0.6090 11.00000 0.05 0.56 Q8 1 0.2173 0.8765 0.2525 11.00000 0.05 0.55 Q9 1 0.1177 0.6298 0.2354 11.00000 0.05 0.53 Q10 1 0.4420 0.8675 0.2173 11.00000 0.05 0.52 Q11 1 0.1627 0.8041 0.0808 11.00000 0.05 0.48 Q12 1 0.1242 0.4515 0.1056 11.00000 0.05 0.48 Q13 1 0.3559 0.8256 0.0939 11.00000 0.05 0.46 Q14 1 0.2633 0.8354 0.0608 11.00000 0.05 0.46 Q15 1 0.0843 1.5197 0.6505 11.00000 0.05 0.44 Q16 1 0.4365 0.9259 0.3720 11.00000 0.05 0.42 Q17 1 0.3609 0.8814 0.3195 11.00000 0.05 0.42 Q18 1 0.3020 0.8855 0.3711 11.00000 0.05 0.41 Q19 1 0.4614 0.9112 0.2985 11.00000 0.05 0.40 Q20 1 -0.0159 0.7516 0.0574 11.00000 0.05 0.39 ; data_asb241 _database_code_depnum_ccdc_archive 'CCDC 895610' #TrackingRef '13191_web_deposit_cif_file_0_NathanielS.Sickerman_1344538304.SuperCif.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H70 Cl4 F3 Mn N4 O15 S4 Sr' _chemical_formula_weight 1388.66 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 '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 13.9061(7) _cell_length_b 15.1055(8) _cell_length_c 16.2620(9) _cell_angle_alpha 68.7445(6) _cell_angle_beta 75.3429(6) _cell_angle_gamma 74.3805(6) _cell_volume 3019.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9853 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.35 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5806 _exptl_absorpt_correction_T_max 0.7443 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 32819 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _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 1.36 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12276 _reflns_number_gt 11026 _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. Hydrogen atom H(7) was located from a difference-Fourier map and refined (x,y,z and Uiso) with d(O-H) fixed at 0.85 ang. The remaining hydrogen atoms were included using a riding model. There were two molecules of dichloromethane solvent present. The triflate anion and the solvent chlorine atoms were disordered and included using multiple components and partial site-occupancy-factors. The triflate anion was refined as a rigid group. Isotropic thermal parameters were used for the carbon, fluorine and oxygen atoms associated with the triflate anion and for the chlorine atoms. ; _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^)+(0.0738P)^2^+8.9969P] 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 12276 _refine_ls_number_parameters 674 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sr1 Sr 0.51905(2) 0.96054(2) 0.230891(19) 0.01569(9) Uani 1 1 d . . . Mn1 Mn 0.63460(4) 0.69003(3) 0.34448(3) 0.01674(12) Uani 1 1 d . . . S1 S 0.45120(6) 0.72794(6) 0.23581(6) 0.02016(17) Uani 1 1 d . . . S3 S 0.69858(7) 0.70080(6) 0.52202(6) 0.02171(18) Uani 1 1 d . . . S2 S 0.75889(6) 0.80186(6) 0.14194(5) 0.01892(17) Uani 1 1 d . . . O1 O 0.44490(19) 0.82867(17) 0.22705(17) 0.0233(5) Uani 1 1 d . . . O2 O 0.4889(2) 0.70514(19) 0.15328(17) 0.0307(6) Uani 1 1 d . . . O3 O 0.68125(18) 0.88503(17) 0.15441(16) 0.0224(5) Uani 1 1 d . . . O4 O 0.76013(19) 0.77940(19) 0.06275(17) 0.0261(5) Uani 1 1 d . . . O5 O 0.65597(19) 0.80282(17) 0.48346(16) 0.0237(5) Uani 1 1 d . . . O6 O 0.8044(2) 0.6784(2) 0.52664(19) 0.0328(6) Uani 1 1 d . . . O7 O 0.57659(18) 0.81315(16) 0.34659(16) 0.0196(5) Uani 1 1 d D . . H7 H 0.594(4) 0.820(4) 0.390(2) 0.042(14) Uiso 1 1 d D . . O8 O 0.58284(18) 1.11346(18) 0.10437(16) 0.0223(5) Uani 1 1 d . . . O9 O 0.64352(19) 1.04217(18) 0.26453(16) 0.0230(5) Uani 1 1 d . . . O10 O 0.46080(19) 1.01237(18) 0.37922(16) 0.0241(5) Uani 1 1 d . . . O11 O 0.33107(18) 1.05625(18) 0.25939(16) 0.0234(5) Uani 1 1 d . . . O12 O 0.42966(18) 1.04234(18) 0.09211(15) 0.0215(5) Uani 1 1 d . . . N1 N 0.6965(2) 0.5486(2) 0.35158(19) 0.0202(6) Uani 1 1 d . . . N2 N 0.5152(2) 0.6608(2) 0.3122(2) 0.0202(6) Uani 1 1 d . . . N3 N 0.7467(2) 0.7125(2) 0.22997(19) 0.0201(6) Uani 1 1 d . . . N4 N 0.6740(2) 0.6418(2) 0.4684(2) 0.0223(6) Uani 1 1 d . . . C1 C 0.6412(3) 0.5167(3) 0.3032(2) 0.0239(7) Uani 1 1 d . . . H1A H 0.6540 0.4451 0.3221 0.029 Uiso 1 1 calc R . . H1B H 0.6653 0.5410 0.2378 0.029 Uiso 1 1 calc R . . C2 C 0.5289(3) 0.5563(2) 0.3246(3) 0.0246(7) Uani 1 1 d . . . H2B H 0.4923 0.5472 0.2843 0.030 Uiso 1 1 calc R . . H2C H 0.5015 0.5216 0.3872 0.030 Uiso 1 1 calc R . . C3 C 0.3257(3) 0.7036(3) 0.2769(3) 0.0244(7) Uani 1 1 d . . . C4 C 0.2706(3) 0.7294(3) 0.3528(3) 0.0276(8) Uani 1 1 d . . . C5 C 0.1741(3) 0.7071(3) 0.3872(3) 0.0396(10) Uani 1 1 d . . . H5A H 0.1359 0.7237 0.4387 0.048 Uiso 1 1 calc R . . C6 C 0.1325(3) 0.6615(3) 0.3483(4) 0.0473(13) Uani 1 1 d . . . C7 C 0.1877(3) 0.6393(3) 0.2728(4) 0.0432(12) Uani 1 1 d . . . H7B H 0.1585 0.6096 0.2454 0.052 Uiso 1 1 calc R . . C8 C 0.2841(3) 0.6584(3) 0.2350(3) 0.0338(9) Uani 1 1 d . . . C9 C 0.3082(3) 0.7806(3) 0.3988(3) 0.0329(9) Uani 1 1 d . . . H9A H 0.2676 0.7739 0.4587 0.049 Uiso 1 1 calc R . . H9B H 0.3021 0.8494 0.3637 0.049 Uiso 1 1 calc R . . H9C H 0.3794 0.7518 0.4038 0.049 Uiso 1 1 calc R . . C10 C 0.0284(4) 0.6362(4) 0.3882(5) 0.072(2) Uani 1 1 d . . . H10A H -0.0100 0.6770 0.4254 0.107 Uiso 1 1 calc R . . H10B H 0.0359 0.5679 0.4251 0.107 Uiso 1 1 calc R . . H10C H -0.0079 0.6474 0.3398 0.107 Uiso 1 1 calc R . . C11 C 0.3346(4) 0.6285(3) 0.1522(3) 0.0478(12) Uani 1 1 d . . . H11A H 0.2910 0.5950 0.1401 0.072 Uiso 1 1 calc R . . H11B H 0.4000 0.5850 0.1621 0.072 Uiso 1 1 calc R . . H11C H 0.3455 0.6862 0.1008 0.072 Uiso 1 1 calc R . . C12 C 0.8057(3) 0.5444(3) 0.3094(3) 0.0268(8) Uani 1 1 d . . . H12A H 0.8357 0.4799 0.3018 0.032 Uiso 1 1 calc R . . H12B H 0.8432 0.5540 0.3488 0.032 Uiso 1 1 calc R . . C13 C 0.8155(3) 0.6223(3) 0.2192(3) 0.0254(7) Uani 1 1 d . . . H13A H 0.8863 0.6322 0.1986 0.030 Uiso 1 1 calc R . . H13B H 0.7965 0.6031 0.1742 0.030 Uiso 1 1 calc R . . C14 C 0.8787(2) 0.8318(2) 0.1319(2) 0.0204(7) Uani 1 1 d . . . C15 C 0.9539(3) 0.8350(3) 0.0538(2) 0.0278(8) Uani 1 1 d . . . C16 C 1.0427(3) 0.8630(3) 0.0517(3) 0.0331(9) Uani 1 1 d . . . H16A H 1.0935 0.8672 -0.0004 0.040 Uiso 1 1 calc R . . C17 C 1.0607(3) 0.8847(3) 0.1211(3) 0.0316(8) Uani 1 1 d . . . C18 C 0.9867(3) 0.8786(3) 0.1971(3) 0.0277(8) Uani 1 1 d . . . H18A H 0.9985 0.8926 0.2458 0.033 Uiso 1 1 calc R . . C19 C 0.8955(3) 0.8526(3) 0.2042(2) 0.0227(7) Uani 1 1 d . . . C20 C 0.9476(3) 0.8105(4) -0.0262(3) 0.0415(11) Uani 1 1 d . . . H20A H 1.0113 0.8155 -0.0690 0.062 Uiso 1 1 calc R . . H20B H 0.8914 0.8558 -0.0549 0.062 Uiso 1 1 calc R . . H20C H 0.9359 0.7443 -0.0068 0.062 Uiso 1 1 calc R . . C21 C 1.1578(3) 0.9135(4) 0.1163(3) 0.0443(11) Uani 1 1 d . . . H21A H 1.1515 0.9368 0.1668 0.066 Uiso 1 1 calc R . . H21B H 1.1715 0.9652 0.0599 0.066 Uiso 1 1 calc R . . H21C H 1.2137 0.8574 0.1192 0.066 Uiso 1 1 calc R . . C22 C 0.8226(3) 0.8458(3) 0.2916(2) 0.0273(8) Uani 1 1 d . . . H22A H 0.8402 0.8818 0.3234 0.041 Uiso 1 1 calc R . . H22B H 0.8271 0.7777 0.3286 0.041 Uiso 1 1 calc R . . H22C H 0.7534 0.8735 0.2795 0.041 Uiso 1 1 calc R . . C23 C 0.6869(3) 0.4881(3) 0.4480(2) 0.0265(8) Uani 1 1 d . . . H23A H 0.7299 0.4229 0.4539 0.032 Uiso 1 1 calc R . . H23B H 0.6157 0.4805 0.4723 0.032 Uiso 1 1 calc R . . C24 C 0.7197(3) 0.5365(3) 0.5004(2) 0.0266(8) Uani 1 1 d . . . H24A H 0.6956 0.5086 0.5653 0.032 Uiso 1 1 calc R . . H24B H 0.7946 0.5269 0.4897 0.032 Uiso 1 1 calc R . . C25 C 0.6290(3) 0.6657(2) 0.6339(2) 0.0241(7) Uani 1 1 d . . . C26 C 0.5232(3) 0.6757(2) 0.6454(2) 0.0252(7) Uani 1 1 d . . . C27 C 0.4666(3) 0.6568(3) 0.7324(3) 0.0315(8) Uani 1 1 d . . . H27A H 0.3955 0.6621 0.7404 0.038 Uiso 1 1 calc R . . C28 C 0.5114(4) 0.6307(3) 0.8068(3) 0.0391(10) Uani 1 1 d . . . C29 C 0.6152(4) 0.6221(3) 0.7933(3) 0.0403(10) Uani 1 1 d . . . H29A H 0.6463 0.6048 0.8442 0.048 Uiso 1 1 calc R . . C30 C 0.6774(3) 0.6374(3) 0.7087(3) 0.0321(9) Uani 1 1 d . . . C31 C 0.4637(3) 0.7086(3) 0.5701(3) 0.0267(8) Uani 1 1 d . . . H31A H 0.3909 0.7185 0.5944 0.040 Uiso 1 1 calc R . . H31B H 0.4811 0.6590 0.5402 0.040 Uiso 1 1 calc R . . H31C H 0.4804 0.7695 0.5267 0.040 Uiso 1 1 calc R . . C32 C 0.4489(5) 0.6118(4) 0.8997(3) 0.0608(16) Uani 1 1 d . . . H32A H 0.4727 0.6405 0.9342 0.091 Uiso 1 1 calc R . . H32B H 0.4558 0.5418 0.9296 0.091 Uiso 1 1 calc R . . H32C H 0.3775 0.6409 0.8956 0.091 Uiso 1 1 calc R . . C33 C 0.7892(4) 0.6242(3) 0.7059(3) 0.0424(10) Uani 1 1 d . . . H33A H 0.8030 0.6015 0.7671 0.064 Uiso 1 1 calc R . . H33B H 0.8109 0.6861 0.6730 0.064 Uiso 1 1 calc R . . H33C H 0.8265 0.5762 0.6757 0.064 Uiso 1 1 calc R . . C34 C 0.6833(3) 1.1170(3) 0.1086(2) 0.0254(7) Uani 1 1 d . . . H34A H 0.7059 1.1737 0.0604 0.031 Uiso 1 1 calc R . . H34B H 0.7312 1.0575 0.1013 0.031 Uiso 1 1 calc R . . C35 C 0.6793(3) 1.1249(3) 0.1984(2) 0.0273(8) Uani 1 1 d . . . H35A H 0.7475 1.1259 0.2056 0.033 Uiso 1 1 calc R . . H35B H 0.6327 1.1853 0.2049 0.033 Uiso 1 1 calc R . . C36 C 0.6240(3) 1.0457(3) 0.3546(2) 0.0264(8) Uani 1 1 d . . . H36A H 0.6632 1.0898 0.3580 0.032 Uiso 1 1 calc R . . H36B H 0.6460 0.9803 0.3959 0.032 Uiso 1 1 calc R . . C37 C 0.5132(3) 1.0809(3) 0.3824(2) 0.0266(8) Uani 1 1 d . . . H37A H 0.4996 1.0850 0.4439 0.032 Uiso 1 1 calc R . . H37B H 0.4903 1.1461 0.3412 0.032 Uiso 1 1 calc R . . C38 C 0.3524(3) 1.0366(3) 0.4050(2) 0.0281(8) Uani 1 1 d . . . H38A H 0.3366 1.0681 0.4520 0.034 Uiso 1 1 calc R . . H38B H 0.3248 0.9764 0.4308 0.034 Uiso 1 1 calc R . . C39 C 0.3024(3) 1.1031(3) 0.3271(3) 0.0287(8) Uani 1 1 d . . . H39A H 0.2278 1.1154 0.3457 0.034 Uiso 1 1 calc R . . H39B H 0.3250 1.1658 0.3037 0.034 Uiso 1 1 calc R . . C40 C 0.2819(3) 1.1094(3) 0.1836(2) 0.0277(8) Uani 1 1 d . . . H40A H 0.2973 1.1753 0.1566 0.033 Uiso 1 1 calc R . . H40B H 0.2075 1.1152 0.2017 0.033 Uiso 1 1 calc R . . C41 C 0.3217(3) 1.0538(3) 0.1175(2) 0.0260(8) Uani 1 1 d . . . H41A H 0.3031 0.9892 0.1445 0.031 Uiso 1 1 calc R . . H41B H 0.2899 1.0887 0.0635 0.031 Uiso 1 1 calc R . . C42 C 0.4627(3) 1.1236(3) 0.0198(2) 0.0265(8) Uani 1 1 d . . . H42A H 0.4244 1.1854 0.0298 0.032 Uiso 1 1 calc R . . H42B H 0.4519 1.1232 -0.0380 0.032 Uiso 1 1 calc R . . C43 C 0.5732(3) 1.1123(3) 0.0190(2) 0.0251(7) Uani 1 1 d . . . H43A H 0.6112 1.0503 0.0091 0.030 Uiso 1 1 calc R . . H43B H 0.6006 1.1660 -0.0297 0.030 Uiso 1 1 calc R . . C45 C -0.0403(4) 1.0010(5) 0.3993(4) 0.0662(16) Uani 1 1 d . . . H45A H -0.0809 1.0329 0.3507 0.079 Uiso 1 1 calc R A 1 H45B H -0.0514 1.0450 0.4349 0.079 Uiso 1 1 calc R A 1 Cl1 Cl 0.0897(3) 0.9734(3) 0.3542(2) 0.0420(10) Uiso 0.50 1 d P B 1 Cl2 Cl -0.0791(2) 0.8800(2) 0.47444(17) 0.0438(6) Uiso 0.50 1 d P B 1 Cl1B Cl 0.0931(3) 0.9645(3) 0.3735(3) 0.0463(11) Uiso 0.50 1 d P B 2 Cl2B Cl -0.1016(2) 0.9177(3) 0.4631(2) 0.0564(7) Uiso 0.50 1 d P B 2 C46 C 1.1527(11) 0.4830(10) -0.0100(9) 0.158(5) Uiso 1 1 d . . . H46A H 1.1025 0.4452 -0.0060 0.190 Uiso 1 1 calc R C 1 H46B H 1.1594 0.5308 -0.0708 0.190 Uiso 1 1 calc R C 1 Cl3 Cl 1.1061(4) 0.5447(4) 0.0671(4) 0.1084(15) Uiso 0.50 1 d P D 1 Cl4 Cl 1.2515(5) 0.4165(5) 0.0010(4) 0.1223(19) Uiso 0.50 1 d P D 1 Cl3B Cl 1.1441(7) 0.5812(6) 0.0483(6) 0.162(3) Uiso 0.50 1 d P D 2 Cl4B Cl 1.2997(4) 0.4172(3) -0.0264(3) 0.0901(12) Uiso 0.50 1 d P D 2 S4 S 0.85210(19) 0.27988(19) 0.2694(2) 0.0395(8) Uani 0.553(7) 1 d PG E 1 O13 O 0.8076(2) 0.3665(3) 0.2076(3) 0.0406(14) Uiso 0.553(7) 1 d PG E 1 O14 O 0.8580(3) 0.1900(2) 0.2550(4) 0.0546(19) Uiso 0.553(7) 1 d PG E 1 O15 O 0.8171(3) 0.2755(3) 0.3631(2) 0.0586(19) Uiso 0.553(7) 1 d PG E 1 C44 C 0.98334(19) 0.2917(2) 0.2511(2) 0.0351(17) Uiso 0.553(7) 1 d PG E 1 F1 F 0.9900(3) 0.3675(2) 0.2712(3) 0.0567(16) Uiso 0.553(7) 1 d PG E 1 F2 F 1.0396(2) 0.2135(3) 0.2976(3) 0.0600(17) Uiso 0.553(7) 1 d PG E 1 F3 F 1.0232(2) 0.3067(4) 0.1638(2) 0.078(2) Uiso 0.553(7) 1 d PG E 1 S4B S 0.8343(3) 0.2649(3) 0.2965(4) 0.0564(15) Uani 0.447(7) 1 d PG E 2 O13B O 0.7984(4) 0.3226(6) 0.2149(4) 0.106(4) Uiso 0.447(7) 1 d PG E 2 O14B O 0.8294(4) 0.1639(3) 0.3283(7) 0.104(4) Uiso 0.447(7) 1 d PG E 2 O15B O 0.7996(3) 0.3099(4) 0.3673(4) 0.054(2) Uiso 0.447(7) 1 d PG E 2 C44B C 0.9692(3) 0.2669(3) 0.2687(3) 0.056(3) Uiso 0.447(7) 1 d PG E 2 F1B F 0.9852(4) 0.3563(4) 0.2468(4) 0.093(3) Uiso 0.447(7) 1 d PG E 2 F2B F 1.0179(3) 0.2098(4) 0.3346(4) 0.0427(16) Uiso 0.447(7) 1 d PG E 2 F3B F 1.0103(4) 0.2363(6) 0.1971(4) 0.114(4) Uiso 0.447(7) 1 d PG E 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 Sr1 0.01523(15) 0.01517(15) 0.01756(15) -0.00591(11) -0.00269(11) -0.00356(11) Mn1 0.0164(2) 0.0145(2) 0.0191(2) -0.00611(19) -0.00278(18) -0.00174(18) S1 0.0214(4) 0.0175(4) 0.0227(4) -0.0047(3) -0.0049(3) -0.0069(3) S3 0.0233(4) 0.0212(4) 0.0217(4) -0.0069(3) -0.0056(3) -0.0042(3) S2 0.0143(4) 0.0228(4) 0.0202(4) -0.0086(3) -0.0006(3) -0.0043(3) O1 0.0243(12) 0.0182(12) 0.0291(13) -0.0039(10) -0.0091(10) -0.0076(10) O2 0.0424(16) 0.0284(14) 0.0237(13) -0.0086(11) -0.0037(11) -0.0125(12) O3 0.0172(11) 0.0229(12) 0.0239(12) -0.0063(10) -0.0013(9) -0.0024(9) O4 0.0240(13) 0.0348(14) 0.0230(12) -0.0126(11) -0.0013(10) -0.0092(11) O5 0.0317(14) 0.0201(12) 0.0210(12) -0.0057(10) -0.0059(10) -0.0074(10) O6 0.0254(14) 0.0407(16) 0.0351(15) -0.0128(13) -0.0087(11) -0.0068(12) O7 0.0226(12) 0.0167(11) 0.0200(12) -0.0075(9) -0.0051(9) -0.0010(9) O8 0.0205(12) 0.0277(13) 0.0197(12) -0.0064(10) -0.0010(9) -0.0101(10) O9 0.0277(13) 0.0240(12) 0.0211(12) -0.0081(10) -0.0046(10) -0.0095(10) O10 0.0262(13) 0.0256(13) 0.0252(12) -0.0131(10) -0.0025(10) -0.0073(10) O11 0.0212(12) 0.0245(12) 0.0230(12) -0.0095(10) -0.0035(10) 0.0003(10) O12 0.0180(12) 0.0265(13) 0.0193(11) -0.0044(10) -0.0020(9) -0.0085(10) N1 0.0194(14) 0.0175(13) 0.0240(14) -0.0079(11) -0.0034(11) -0.0022(11) N2 0.0176(14) 0.0162(13) 0.0275(15) -0.0055(11) -0.0056(11) -0.0044(11) N3 0.0159(13) 0.0197(14) 0.0243(14) -0.0098(12) 0.0001(11) -0.0024(11) N4 0.0254(15) 0.0171(14) 0.0232(14) -0.0060(12) -0.0079(12) 0.0009(11) C1 0.0253(18) 0.0198(17) 0.0286(18) -0.0093(14) -0.0048(14) -0.0053(14) C2 0.0236(18) 0.0172(16) 0.0333(19) -0.0065(14) -0.0058(14) -0.0058(13) C3 0.0205(17) 0.0195(16) 0.0322(19) -0.0015(14) -0.0089(14) -0.0074(13) C4 0.0200(17) 0.0188(17) 0.036(2) 0.0017(15) -0.0084(15) -0.0014(13) C5 0.0218(19) 0.027(2) 0.054(3) 0.0001(19) -0.0037(18) -0.0005(16) C6 0.024(2) 0.026(2) 0.079(4) 0.010(2) -0.020(2) -0.0091(16) C7 0.037(2) 0.026(2) 0.069(3) 0.001(2) -0.029(2) -0.0139(18) C8 0.036(2) 0.0205(18) 0.046(2) 0.0011(17) -0.0218(18) -0.0106(16) C9 0.0246(19) 0.035(2) 0.034(2) -0.0111(17) -0.0018(16) 0.0002(16) C10 0.025(2) 0.049(3) 0.120(6) 0.003(3) -0.013(3) -0.016(2) C11 0.070(3) 0.037(2) 0.053(3) -0.014(2) -0.024(2) -0.024(2) C12 0.0207(17) 0.0227(18) 0.037(2) -0.0128(16) -0.0026(15) -0.0017(14) C13 0.0200(17) 0.0222(17) 0.0332(19) -0.0135(15) 0.0012(14) -0.0016(14) C14 0.0146(15) 0.0227(17) 0.0240(17) -0.0075(14) -0.0004(13) -0.0063(13) C15 0.0210(17) 0.037(2) 0.0250(18) -0.0114(16) 0.0002(14) -0.0062(15) C16 0.0222(18) 0.047(2) 0.029(2) -0.0113(18) 0.0049(15) -0.0140(17) C17 0.0219(18) 0.037(2) 0.035(2) -0.0067(17) -0.0040(15) -0.0119(16) C18 0.0243(18) 0.031(2) 0.0310(19) -0.0108(16) -0.0051(15) -0.0095(15) C19 0.0178(16) 0.0238(17) 0.0263(18) -0.0093(14) -0.0024(13) -0.0032(13) C20 0.025(2) 0.075(3) 0.031(2) -0.028(2) 0.0096(16) -0.017(2) C21 0.029(2) 0.063(3) 0.046(3) -0.015(2) -0.0015(19) -0.025(2) C22 0.0214(17) 0.040(2) 0.0263(18) -0.0171(16) -0.0023(14) -0.0077(15) C23 0.0321(19) 0.0176(16) 0.0261(18) -0.0043(14) -0.0046(15) -0.0027(14) C24 0.0319(19) 0.0181(17) 0.0263(18) -0.0052(14) -0.0098(15) 0.0027(14) C25 0.036(2) 0.0160(16) 0.0207(17) -0.0054(13) -0.0062(14) -0.0049(14) C26 0.034(2) 0.0173(16) 0.0264(18) -0.0082(14) -0.0033(15) -0.0076(14) C27 0.040(2) 0.0187(17) 0.032(2) -0.0080(15) 0.0028(17) -0.0076(15) C28 0.059(3) 0.024(2) 0.0239(19) -0.0045(16) 0.0012(18) -0.0048(19) C29 0.066(3) 0.028(2) 0.0234(19) -0.0033(16) -0.0164(19) -0.002(2) C30 0.045(2) 0.0227(18) 0.029(2) -0.0070(15) -0.0143(17) -0.0021(16) C31 0.0267(18) 0.0262(18) 0.0305(19) -0.0106(15) -0.0032(15) -0.0100(15) C32 0.081(4) 0.052(3) 0.027(2) -0.003(2) 0.005(2) -0.003(3) C33 0.050(3) 0.042(2) 0.036(2) -0.0094(19) -0.023(2) 0.001(2) C34 0.0216(17) 0.0315(19) 0.0251(18) -0.0062(15) -0.0002(14) -0.0156(15) C35 0.0295(19) 0.0294(19) 0.0290(19) -0.0098(15) -0.0041(15) -0.0154(15) C36 0.033(2) 0.0281(19) 0.0244(18) -0.0104(15) -0.0101(15) -0.0093(15) C37 0.035(2) 0.0267(18) 0.0250(18) -0.0141(15) -0.0031(15) -0.0111(15) C38 0.0285(19) 0.035(2) 0.0240(18) -0.0164(16) 0.0032(14) -0.0091(16) C39 0.0243(18) 0.031(2) 0.032(2) -0.0185(16) 0.0014(15) -0.0025(15) C40 0.0176(17) 0.0290(19) 0.0281(19) -0.0023(15) -0.0056(14) 0.0011(14) C41 0.0169(16) 0.036(2) 0.0239(17) -0.0045(15) -0.0060(13) -0.0087(14) C42 0.0267(19) 0.0306(19) 0.0195(17) 0.0000(15) -0.0047(14) -0.0118(15) C43 0.0255(18) 0.0324(19) 0.0175(16) -0.0041(14) -0.0015(13) -0.0129(15) C45 0.042(3) 0.099(5) 0.067(4) -0.044(4) -0.005(3) -0.007(3) S4 0.0260(13) 0.0494(16) 0.0499(16) -0.0241(12) -0.0145(11) 0.0010(11) S4B 0.0332(19) 0.060(2) 0.094(4) -0.047(2) -0.027(2) 0.0065(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 Sr1 O7 2.430(2) . ? Sr1 O3 2.482(2) . ? Sr1 O1 2.503(2) . ? Sr1 O12 2.595(2) . ? Sr1 O9 2.633(2) . ? Sr1 O11 2.641(2) . ? Sr1 O8 2.663(2) . ? Sr1 O10 2.670(2) . ? Mn1 O7 1.826(2) . ? Mn1 N4 2.042(3) . ? Mn1 N1 2.049(3) . ? Mn1 N2 2.057(3) . ? Mn1 N3 2.090(3) . ? S1 O2 1.441(3) . ? S1 O1 1.456(2) . ? S1 N2 1.588(3) . ? S1 C3 1.790(4) . ? S3 O6 1.434(3) . ? S3 O5 1.454(3) . ? S3 N4 1.597(3) . ? S3 C25 1.793(4) . ? S2 O4 1.441(3) . ? S2 O3 1.459(2) . ? S2 N3 1.581(3) . ? S2 C14 1.795(3) . ? O5 H7 1.836(14) . ? O8 C34 1.431(4) . ? O8 C43 1.435(4) . ? O9 C35 1.433(4) . ? O9 C36 1.439(4) . ? O10 C37 1.439(4) . ? O10 C38 1.441(4) . ? O11 C40 1.430(4) . ? O11 C39 1.436(4) . ? O12 C41 1.432(4) . ? O12 C42 1.444(4) . ? N1 C1 1.492(4) . ? N1 C23 1.495(5) . ? N1 C12 1.495(4) . ? N2 C2 1.482(4) . ? N3 C13 1.479(4) . ? N4 C24 1.493(4) . ? C1 C2 1.512(5) . ? C3 C4 1.404(6) . ? C3 C8 1.419(5) . ? C4 C5 1.397(5) . ? C4 C9 1.505(6) . ? C5 C6 1.387(7) . ? C6 C7 1.375(8) . ? C6 C10 1.518(6) . ? C7 C8 1.386(6) . ? C8 C11 1.517(7) . ? C12 C13 1.513(5) . ? C14 C19 1.408(5) . ? C14 C15 1.421(5) . ? C15 C16 1.398(5) . ? C15 C20 1.504(5) . ? C16 C17 1.378(6) . ? C17 C18 1.387(5) . ? C17 C21 1.502(5) . ? C18 C19 1.392(5) . ? C19 C22 1.510(5) . ? C23 C24 1.514(5) . ? C25 C26 1.410(5) . ? C25 C30 1.413(5) . ? C26 C27 1.402(5) . ? C26 C31 1.511(5) . ? C27 C28 1.382(6) . ? C28 C29 1.382(7) . ? C28 C32 1.508(6) . ? C29 C30 1.403(6) . ? C30 C33 1.504(6) . ? C34 C35 1.495(5) . ? C36 C37 1.497(5) . ? C38 C39 1.499(6) . ? C40 C41 1.507(5) . ? C42 C43 1.497(5) . ? C45 Cl2B 1.602(7) . ? C45 Cl1 1.768(6) . ? C45 Cl1B 1.774(7) . ? C45 Cl2 1.924(8) . ? C46 Cl4 1.477(14) . ? C46 Cl3 1.724(14) . ? C46 Cl3B 1.995(16) . ? C46 Cl4B 2.016(14) . ? S4 O13 1.4251 . ? S4 O14 1.4372 . ? S4 O15 1.4601 . ? S4 C44 1.8201 . ? C44 F2 1.3169 . ? C44 F1 1.3313 . ? C44 F3 1.3450 . ? S4B O13B 1.4251 . ? S4B O14B 1.4373 . ? S4B O15B 1.4600 . ? S4B C44B 1.8202 . ? C44B F2B 1.3170 . ? C44B F1B 1.3312 . ? C44B F3B 1.3449 . ? 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 Sr1 O3 76.04(8) . . ? O7 Sr1 O1 72.10(8) . . ? O3 Sr1 O1 86.83(8) . . ? O7 Sr1 O12 148.30(8) . . ? O3 Sr1 O12 97.09(8) . . ? O1 Sr1 O12 76.69(8) . . ? O7 Sr1 O9 87.92(8) . . ? O3 Sr1 O9 81.02(8) . . ? O1 Sr1 O9 158.67(8) . . ? O12 Sr1 O9 122.02(7) . . ? O7 Sr1 O11 118.88(8) . . ? O3 Sr1 O11 160.99(8) . . ? O1 Sr1 O11 87.05(8) . . ? O12 Sr1 O11 63.97(8) . . ? O9 Sr1 O11 109.73(8) . . ? O7 Sr1 O8 141.98(8) . . ? O3 Sr1 O8 77.67(8) . . ? O1 Sr1 O8 133.04(8) . . ? O12 Sr1 O8 61.98(7) . . ? O9 Sr1 O8 61.09(7) . . ? O11 Sr1 O8 93.58(8) . . ? O7 Sr1 O10 76.71(8) . . ? O3 Sr1 O10 135.37(8) . . ? O1 Sr1 O10 117.01(8) . . ? O12 Sr1 O10 123.83(8) . . ? O9 Sr1 O10 63.31(7) . . ? O11 Sr1 O10 62.95(8) . . ? O8 Sr1 O10 104.59(7) . . ? O7 Mn1 N4 95.43(11) . . ? O7 Mn1 N1 176.02(11) . . ? N4 Mn1 N1 81.18(11) . . ? O7 Mn1 N2 97.68(11) . . ? N4 Mn1 N2 126.32(12) . . ? N1 Mn1 N2 82.76(11) . . ? O7 Mn1 N3 102.74(11) . . ? N4 Mn1 N3 119.87(12) . . ? N1 Mn1 N3 80.84(11) . . ? N2 Mn1 N3 107.40(12) . . ? O2 S1 O1 114.43(15) . . ? O2 S1 N2 112.51(16) . . ? O1 S1 N2 108.45(15) . . ? O2 S1 C3 108.00(17) . . ? O1 S1 C3 107.22(16) . . ? N2 S1 C3 105.75(16) . . ? O6 S3 O5 115.65(16) . . ? O6 S3 N4 111.44(17) . . ? O5 S3 N4 108.16(15) . . ? O6 S3 C25 108.32(17) . . ? O5 S3 C25 105.23(16) . . ? N4 S3 C25 107.60(16) . . ? O4 S2 O3 114.16(15) . . ? O4 S2 N3 112.26(15) . . ? O3 S2 N3 108.57(14) . . ? O4 S2 C14 107.98(16) . . ? O3 S2 C14 106.48(15) . . ? N3 S2 C14 107.00(16) . . ? S1 O1 Sr1 151.41(15) . . ? S2 O3 Sr1 152.81(15) . . ? S3 O5 H7 110.0(15) . . ? Mn1 O7 Sr1 132.09(12) . . ? C34 O8 C43 113.3(3) . . ? C34 O8 Sr1 111.69(19) . . ? C43 O8 Sr1 108.57(19) . . ? C35 O9 C36 113.6(3) . . ? C35 O9 Sr1 120.68(19) . . ? C36 O9 Sr1 115.0(2) . . ? C37 O10 C38 113.4(3) . . ? C37 O10 Sr1 115.1(2) . . ? C38 O10 Sr1 113.86(19) . . ? C40 O11 C39 112.8(3) . . ? C40 O11 Sr1 117.9(2) . . ? C39 O11 Sr1 119.1(2) . . ? C41 O12 C42 113.7(3) . . ? C41 O12 Sr1 111.50(19) . . ? C42 O12 Sr1 120.82(19) . . ? C1 N1 C23 110.4(3) . . ? C1 N1 C12 111.4(3) . . ? C23 N1 C12 110.3(3) . . ? C1 N1 Mn1 109.1(2) . . ? C23 N1 Mn1 108.4(2) . . ? C12 N1 Mn1 107.1(2) . . ? C2 N2 S1 112.8(2) . . ? C2 N2 Mn1 111.4(2) . . ? S1 N2 Mn1 127.30(16) . . ? C13 N3 S2 111.9(2) . . ? C13 N3 Mn1 113.8(2) . . ? S2 N3 Mn1 132.62(16) . . ? C24 N4 S3 111.9(2) . . ? C24 N4 Mn1 115.1(2) . . ? S3 N4 Mn1 129.50(17) . . ? N1 C1 C2 108.9(3) . . ? N2 C2 C1 108.1(3) . . ? C4 C3 C8 121.3(3) . . ? C4 C3 S1 117.7(3) . . ? C8 C3 S1 121.1(3) . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C9 117.9(4) . . ? C3 C4 C9 124.2(3) . . ? C6 C5 C4 122.0(5) . . ? C7 C6 C5 118.6(4) . . ? C7 C6 C10 120.6(5) . . ? C5 C6 C10 120.9(6) . . ? C6 C7 C8 123.0(4) . . ? C7 C8 C3 117.4(4) . . ? C7 C8 C11 116.1(4) . . ? C3 C8 C11 126.6(4) . . ? N1 C12 C13 109.9(3) . . ? N3 C13 C12 107.5(3) . . ? C19 C14 C15 120.9(3) . . ? C19 C14 S2 117.6(3) . . ? C15 C14 S2 121.5(3) . . ? C16 C15 C14 116.7(3) . . ? C16 C15 C20 117.0(3) . . ? C14 C15 C20 126.4(3) . . ? C17 C16 C15 123.6(4) . . ? C16 C17 C18 118.2(3) . . ? C16 C17 C21 121.8(4) . . ? C18 C17 C21 119.9(4) . . ? C17 C18 C19 121.8(4) . . ? C18 C19 C14 118.8(3) . . ? C18 C19 C22 116.5(3) . . ? C14 C19 C22 124.7(3) . . ? N1 C23 C24 109.4(3) . . ? N4 C24 C23 106.9(3) . . ? C26 C25 C30 120.6(3) . . ? C26 C25 S3 118.2(3) . . ? C30 C25 S3 120.9(3) . . ? C27 C26 C25 118.8(4) . . ? C27 C26 C31 116.3(4) . . ? C25 C26 C31 124.9(3) . . ? C28 C27 C26 122.0(4) . . ? C29 C28 C27 117.8(4) . . ? C29 C28 C32 121.2(5) . . ? C27 C28 C32 121.0(5) . . ? C28 C29 C30 123.7(4) . . ? C29 C30 C25 117.1(4) . . ? C29 C30 C33 116.9(4) . . ? C25 C30 C33 126.0(4) . . ? O8 C34 C35 106.8(3) . . ? O9 C35 C34 107.3(3) . . ? O9 C36 C37 110.0(3) . . ? O10 C37 C36 107.0(3) . . ? O10 C38 C39 111.8(3) . . ? O11 C39 C38 107.2(3) . . ? O11 C40 C41 106.8(3) . . ? O12 C41 C40 111.3(3) . . ? O12 C41 Sr1 45.38(14) . . ? C40 C41 Sr1 83.13(19) . . ? O12 C42 C43 106.3(3) . . ? O8 C43 C42 107.3(3) . . ? O8 C43 Sr1 47.87(14) . . ? C42 C43 Sr1 83.43(19) . . ? Cl2B C45 Cl1 121.6(4) . . ? Cl2B C45 Cl1B 116.4(4) . . ? Cl1 C45 Cl1B 9.86(17) . . ? Cl2B C45 Cl2 15.01(15) . . ? Cl1 C45 Cl2 106.7(4) . . ? Cl1B C45 Cl2 101.4(4) . . ? Cl4 C46 Cl3 114.9(9) . . ? Cl4 C46 Cl3B 106.3(9) . . ? Cl3 C46 Cl3B 23.2(3) . . ? Cl4 C46 Cl4B 15.2(4) . . ? Cl3 C46 Cl4B 120.2(8) . . ? Cl3B C46 Cl4B 106.0(7) . . ? O13 S4 O14 117.2 . . ? O13 S4 O15 114.0 . . ? O14 S4 O15 112.9 . . ? O13 S4 C44 103.5 . . ? O14 S4 C44 104.8 . . ? O15 S4 C44 102.3 . . ? F2 C44 F1 108.8 . . ? F2 C44 F3 107.8 . . ? F1 C44 F3 107.2 . . ? F2 C44 S4 112.4 . . ? F1 C44 S4 111.4 . . ? F3 C44 S4 109.1 . . ? O13B S4B O14B 117.2 . . ? O13B S4B O15B 114.0 . . ? O14B S4B O15B 112.8 . . ? O13B S4B C44B 103.5 . . ? O14B S4B C44B 104.8 . . ? O15B S4B C44B 102.3 . . ? F2B C44B F1B 108.8 . . ? F2B C44B F3B 107.7 . . ? F1B C44B F3B 107.2 . . ? F2B C44B S4B 112.4 . . ? F1B C44B S4B 111.4 . . ? F3B C44B S4B 109.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.949 _refine_diff_density_min -1.455 _refine_diff_density_rms 0.103 _iucr_refine_instructions_details ; TITL asb241 in P-1 CELL 0.71073 13.9061 15.1055 16.2620 68.7445 75.3429 74.3805 ZERR 2.00 0.0007 0.0008 0.0009 0.0006 0.0006 0.0006 LATT 1 SFAC C H N O F S CL MN SR UNIT 92 140 8 30 6 8 8 2 2 TEMP -130.000 SIZE 0.212 0.312 0.412 rem SADABS 2008/1 on 11/1/11 rem Same numbering scheme as asb189 rem Hydrogens added with Riding Model rem H7a located on the diff. map rem FRAG instruction used for disordered triflate CONN 8 SR1 CONN 5 MN1 SHEL 100 0.80 DFIX 0.85 0.001 h7 o7 BIND O5 H7 L.S. 12 ACTA 51 FMAP 2 PLAN 10 WGHT 0.073800 8.996900 FVAR 0.10338 0.55310 SR1 9 0.519045 0.960541 0.230891 11.00000 0.01523 0.01517 = 0.01756 -0.00591 -0.00269 -0.00356 MN1 8 0.634604 0.690032 0.344485 11.00000 0.01636 0.01446 = 0.01911 -0.00611 -0.00278 -0.00174 S1 6 0.451204 0.727940 0.235806 11.00000 0.02143 0.01747 = 0.02274 -0.00472 -0.00493 -0.00693 S3 6 0.698577 0.700802 0.522018 11.00000 0.02327 0.02121 = 0.02167 -0.00694 -0.00561 -0.00419 S2 6 0.758888 0.801861 0.141935 11.00000 0.01433 0.02277 = 0.02023 -0.00862 -0.00058 -0.00430 O1 4 0.444899 0.828669 0.227046 11.00000 0.02429 0.01820 = 0.02910 -0.00390 -0.00907 -0.00761 O2 4 0.488851 0.705137 0.153276 11.00000 0.04241 0.02840 = 0.02368 -0.00856 -0.00370 -0.01249 O3 4 0.681245 0.885028 0.154410 11.00000 0.01717 0.02288 = 0.02386 -0.00626 -0.00134 -0.00243 O4 4 0.760132 0.779404 0.062754 11.00000 0.02398 0.03476 = 0.02302 -0.01264 -0.00126 -0.00920 O5 4 0.655965 0.802822 0.483461 11.00000 0.03169 0.02005 = 0.02101 -0.00568 -0.00589 -0.00743 O6 4 0.804448 0.678353 0.526636 11.00000 0.02537 0.04067 = 0.03513 -0.01283 -0.00868 -0.00677 O7 4 0.576593 0.813146 0.346590 11.00000 0.02260 0.01668 = 0.02004 -0.00752 -0.00506 -0.00099 H7 2 0.593511 0.819600 0.390494 11.00000 0.04171 O8 4 0.582839 1.113457 0.104366 11.00000 0.02047 0.02766 = 0.01973 -0.00640 -0.00098 -0.01012 O9 4 0.643516 1.042165 0.264534 11.00000 0.02769 0.02396 = 0.02111 -0.00813 -0.00461 -0.00946 O10 4 0.460797 1.012370 0.379221 11.00000 0.02619 0.02562 = 0.02515 -0.01311 -0.00254 -0.00731 O11 4 0.331074 1.056250 0.259392 11.00000 0.02116 0.02451 = 0.02303 -0.00949 -0.00353 0.00028 O12 4 0.429662 1.042341 0.092110 11.00000 0.01801 0.02646 = 0.01929 -0.00441 -0.00201 -0.00846 N1 3 0.696531 0.548611 0.351581 11.00000 0.01938 0.01747 = 0.02398 -0.00794 -0.00335 -0.00220 N2 3 0.515206 0.660793 0.312177 11.00000 0.01758 0.01617 = 0.02748 -0.00554 -0.00564 -0.00442 N3 3 0.746658 0.712458 0.229966 11.00000 0.01594 0.01970 = 0.02434 -0.00979 0.00012 -0.00240 N4 3 0.673982 0.641771 0.468408 11.00000 0.02540 0.01709 = 0.02320 -0.00603 -0.00790 0.00091 C1 1 0.641155 0.516714 0.303191 11.00000 0.02525 0.01985 = 0.02862 -0.00928 -0.00481 -0.00530 AFIX 23 H1A 2 0.653963 0.445070 0.322105 11.00000 -1.20000 H1B 2 0.665292 0.540986 0.237827 11.00000 -1.20000 AFIX 0 C2 1 0.528947 0.556279 0.324638 11.00000 0.02359 0.01722 = 0.03335 -0.00648 -0.00578 -0.00581 AFIX 23 H2B 2 0.492326 0.547174 0.284324 11.00000 -1.20000 H2C 2 0.501549 0.521620 0.387230 11.00000 -1.20000 AFIX 0 C3 1 0.325692 0.703627 0.276875 11.00000 0.02054 0.01946 = 0.03222 -0.00146 -0.00895 -0.00743 C4 1 0.270595 0.729364 0.352816 11.00000 0.01997 0.01881 = 0.03574 0.00168 -0.00844 -0.00137 C5 1 0.174121 0.707096 0.387165 11.00000 0.02182 0.02711 = 0.05432 0.00008 -0.00373 -0.00047 AFIX 43 H5A 2 0.135887 0.723665 0.438696 11.00000 -1.20000 AFIX 0 C6 1 0.132492 0.661510 0.348269 11.00000 0.02398 0.02551 = 0.07864 0.01028 -0.02022 -0.00910 C7 1 0.187709 0.639337 0.272806 11.00000 0.03665 0.02578 = 0.06943 0.00113 -0.02880 -0.01388 AFIX 43 H7B 2 0.158463 0.609577 0.245360 11.00000 -1.20000 AFIX 0 C8 1 0.284131 0.658443 0.234953 11.00000 0.03636 0.02047 = 0.04615 0.00110 -0.02182 -0.01060 C9 1 0.308209 0.780580 0.398753 11.00000 0.02455 0.03520 = 0.03354 -0.01111 -0.00181 0.00016 AFIX 137 H9A 2 0.267613 0.773893 0.458713 11.00000 -1.50000 H9B 2 0.302065 0.849401 0.363658 11.00000 -1.50000 H9C 2 0.379444 0.751798 0.403801 11.00000 -1.50000 AFIX 0 C10 1 0.028386 0.636229 0.388182 11.00000 0.02526 0.04944 = 0.11959 0.00311 -0.01322 -0.01560 AFIX 137 H10A 2 -0.009967 0.677041 0.425376 11.00000 -1.50000 H10B 2 0.035857 0.567928 0.425098 11.00000 -1.50000 H10C 2 -0.007924 0.647401 0.339835 11.00000 -1.50000 AFIX 0 C11 1 0.334631 0.628502 0.152161 11.00000 0.06968 0.03685 = 0.05294 -0.01378 -0.02433 -0.02417 AFIX 137 H11A 2 0.290975 0.595008 0.140111 11.00000 -1.50000 H11B 2 0.399987 0.584955 0.162149 11.00000 -1.50000 H11C 2 0.345545 0.686205 0.100751 11.00000 -1.50000 AFIX 0 C12 1 0.805749 0.544408 0.309405 11.00000 0.02066 0.02272 = 0.03691 -0.01279 -0.00257 -0.00169 AFIX 23 H12A 2 0.835652 0.479947 0.301757 11.00000 -1.20000 H12B 2 0.843239 0.553973 0.348812 11.00000 -1.20000 AFIX 0 C13 1 0.815456 0.622296 0.219194 11.00000 0.01998 0.02223 = 0.03317 -0.01354 0.00115 -0.00161 AFIX 23 H13A 2 0.886269 0.632177 0.198649 11.00000 -1.20000 H13B 2 0.796451 0.603142 0.174247 11.00000 -1.20000 AFIX 0 C14 1 0.878681 0.831817 0.131858 11.00000 0.01464 0.02274 = 0.02400 -0.00754 -0.00043 -0.00627 C15 1 0.953928 0.835019 0.053824 11.00000 0.02103 0.03675 = 0.02496 -0.01138 0.00024 -0.00622 C16 1 1.042738 0.862959 0.051702 11.00000 0.02222 0.04686 = 0.02874 -0.01127 0.00488 -0.01399 AFIX 43 H16A 2 1.093482 0.867180 -0.000406 11.00000 -1.20000 AFIX 0 C17 1 1.060726 0.884730 0.121091 11.00000 0.02195 0.03680 = 0.03533 -0.00670 -0.00401 -0.01194 C18 1 0.986674 0.878649 0.197148 11.00000 0.02431 0.03127 = 0.03099 -0.01077 -0.00508 -0.00950 AFIX 43 H18A 2 0.998459 0.892648 0.245779 11.00000 -1.20000 AFIX 0 C19 1 0.895529 0.852581 0.204155 11.00000 0.01783 0.02376 = 0.02627 -0.00935 -0.00237 -0.00323 C20 1 0.947579 0.810520 -0.026198 11.00000 0.02457 0.07462 = 0.03124 -0.02824 0.00960 -0.01661 AFIX 137 H20A 2 1.011254 0.815532 -0.069009 11.00000 -1.50000 H20B 2 0.891433 0.855812 -0.054873 11.00000 -1.50000 H20C 2 0.935913 0.744258 -0.006842 11.00000 -1.50000 AFIX 0 C21 1 1.157815 0.913541 0.116337 11.00000 0.02863 0.06283 = 0.04633 -0.01492 -0.00150 -0.02475 AFIX 137 H21A 2 1.151535 0.936822 0.166774 11.00000 -1.50000 H21B 2 1.171550 0.965225 0.059898 11.00000 -1.50000 H21C 2 1.213687 0.857368 0.119237 11.00000 -1.50000 AFIX 0 C22 1 0.822636 0.845796 0.291569 11.00000 0.02143 0.03973 = 0.02633 -0.01707 -0.00229 -0.00770 AFIX 137 H22A 2 0.840154 0.881752 0.323369 11.00000 -1.50000 H22B 2 0.827057 0.777683 0.328594 11.00000 -1.50000 H22C 2 0.753387 0.873549 0.279479 11.00000 -1.50000 AFIX 0 C23 1 0.686922 0.488105 0.448029 11.00000 0.03208 0.01758 = 0.02606 -0.00430 -0.00458 -0.00272 AFIX 23 H23A 2 0.729918 0.422909 0.453907 11.00000 -1.20000 H23B 2 0.615699 0.480541 0.472266 11.00000 -1.20000 AFIX 0 C24 1 0.719734 0.536473 0.500364 11.00000 0.03190 0.01813 = 0.02628 -0.00523 -0.00983 0.00272 AFIX 23 H24A 2 0.695632 0.508630 0.565336 11.00000 -1.20000 H24B 2 0.794584 0.526870 0.489678 11.00000 -1.20000 AFIX 0 C25 1 0.629030 0.665656 0.633907 11.00000 0.03581 0.01597 = 0.02066 -0.00537 -0.00622 -0.00488 C26 1 0.523154 0.675690 0.645387 11.00000 0.03364 0.01726 = 0.02636 -0.00821 -0.00328 -0.00756 C27 1 0.466638 0.656804 0.732405 11.00000 0.04016 0.01867 = 0.03168 -0.00803 0.00284 -0.00758 AFIX 43 H27A 2 0.395461 0.662145 0.740436 11.00000 -1.20000 AFIX 0 C28 1 0.511383 0.630655 0.806831 11.00000 0.05909 0.02443 = 0.02393 -0.00447 0.00123 -0.00484 C29 1 0.615214 0.622062 0.793338 11.00000 0.06608 0.02783 = 0.02343 -0.00333 -0.01638 -0.00223 AFIX 43 H29A 2 0.646268 0.604787 0.844208 11.00000 -1.20000 AFIX 0 C30 1 0.677351 0.637410 0.708750 11.00000 0.04521 0.02266 = 0.02913 -0.00702 -0.01428 -0.00212 C31 1 0.463667 0.708552 0.570052 11.00000 0.02671 0.02621 = 0.03053 -0.01058 -0.00319 -0.01004 AFIX 137 H31A 2 0.390946 0.718457 0.594359 11.00000 -1.50000 H31B 2 0.481065 0.659012 0.540212 11.00000 -1.50000 H31C 2 0.480402 0.769503 0.526718 11.00000 -1.50000 AFIX 0 C32 1 0.448887 0.611827 0.899676 11.00000 0.08106 0.05193 = 0.02676 -0.00324 0.00532 -0.00291 AFIX 137 H32A 2 0.472707 0.640486 0.934220 11.00000 -1.50000 H32B 2 0.455826 0.541809 0.929601 11.00000 -1.50000 H32C 2 0.377510 0.640950 0.895551 11.00000 -1.50000 AFIX 0 C33 1 0.789173 0.624173 0.705907 11.00000 0.05009 0.04173 = 0.03565 -0.00935 -0.02273 0.00106 AFIX 137 H33A 2 0.803025 0.601526 0.767144 11.00000 -1.50000 H33B 2 0.810875 0.686122 0.672992 11.00000 -1.50000 H33C 2 0.826467 0.576248 0.675734 11.00000 -1.50000 AFIX 0 C34 1 0.683254 1.116973 0.108560 11.00000 0.02155 0.03147 = 0.02510 -0.00620 -0.00024 -0.01561 AFIX 23 H34A 2 0.705881 1.173683 0.060409 11.00000 -1.20000 H34B 2 0.731228 1.057518 0.101285 11.00000 -1.20000 AFIX 0 C35 1 0.679263 1.124878 0.198428 11.00000 0.02945 0.02939 = 0.02895 -0.00984 -0.00406 -0.01538 AFIX 23 H35A 2 0.747520 1.125935 0.205579 11.00000 -1.20000 H35B 2 0.632740 1.185300 0.204926 11.00000 -1.20000 AFIX 0 C36 1 0.623969 1.045733 0.354634 11.00000 0.03334 0.02810 = 0.02444 -0.01036 -0.01012 -0.00927 AFIX 23 H36A 2 0.663167 1.089819 0.357962 11.00000 -1.20000 H36B 2 0.645957 0.980343 0.395902 11.00000 -1.20000 AFIX 0 C37 1 0.513225 1.080922 0.382418 11.00000 0.03496 0.02674 = 0.02499 -0.01407 -0.00308 -0.01110 AFIX 23 H37A 2 0.499628 1.084961 0.443857 11.00000 -1.20000 H37B 2 0.490294 1.146050 0.341188 11.00000 -1.20000 AFIX 0 C38 1 0.352424 1.036586 0.405045 11.00000 0.02850 0.03510 = 0.02400 -0.01640 0.00323 -0.00912 AFIX 23 H38A 2 0.336616 1.068137 0.451968 11.00000 -1.20000 H38B 2 0.324765 0.976419 0.430759 11.00000 -1.20000 AFIX 0 C39 1 0.302393 1.103090 0.327074 11.00000 0.02434 0.03127 = 0.03229 -0.01845 0.00144 -0.00247 AFIX 23 H39A 2 0.227800 1.115391 0.345651 11.00000 -1.20000 H39B 2 0.324983 1.165830 0.303746 11.00000 -1.20000 AFIX 0 C40 1 0.281912 1.109367 0.183592 11.00000 0.01760 0.02900 = 0.02808 -0.00230 -0.00558 0.00109 AFIX 23 H40A 2 0.297346 1.175263 0.156609 11.00000 -1.20000 H40B 2 0.207527 1.115213 0.201741 11.00000 -1.20000 AFIX 0 C41 1 0.321741 1.053823 0.117460 11.00000 0.01692 0.03633 = 0.02390 -0.00446 -0.00597 -0.00868 AFIX 23 H41A 2 0.303128 0.989214 0.144469 11.00000 -1.20000 H41B 2 0.289933 1.088699 0.063456 11.00000 -1.20000 AFIX 0 C42 1 0.462668 1.123580 0.019772 11.00000 0.02669 0.03056 = 0.01948 0.00004 -0.00466 -0.01182 AFIX 23 H42A 2 0.424372 1.185354 0.029832 11.00000 -1.20000 H42B 2 0.451935 1.123232 -0.038006 11.00000 -1.20000 AFIX 0 C43 1 0.573172 1.112266 0.018991 11.00000 0.02545 0.03242 = 0.01747 -0.00414 -0.00147 -0.01288 AFIX 23 H43A 2 0.611180 1.050330 0.009120 11.00000 -1.20000 H43B 2 0.600645 1.166014 -0.029714 11.00000 -1.20000 AFIX 0 C45 1 -0.040305 1.000963 0.399335 11.00000 0.04179 0.09856 = 0.06660 -0.04367 -0.00475 -0.00709 AFIX 23 H45A 2 -0.080930 1.032860 0.350698 11.00000 -1.20000 H45B 2 -0.051368 1.045034 0.434890 11.00000 -1.20000 AFIX 0 PART 1 CL1 7 0.089703 0.973405 0.354215 10.50000 0.04197 CL2 7 -0.079074 0.879961 0.474442 10.50000 0.04376 PART 2 CL1B 7 0.093148 0.964497 0.373546 10.50000 0.04629 CL2B 7 -0.101578 0.917695 0.463085 10.50000 0.05635 PART 0 C46 1 1.152651 0.482991 -0.010030 11.00000 0.15814 AFIX 23 H46A 2 1.102532 0.445182 -0.005978 11.00000 -1.20000 H46B 2 1.159392 0.530833 -0.070828 11.00000 -1.20000 AFIX 0 PART 1 CL3 7 1.106087 0.544693 0.067051 10.50000 0.10838 CL4 7 1.251521 0.416466 0.001025 10.50000 0.12228 PART 2 CL3B 7 1.144129 0.581171 0.048265 10.50000 0.16159 CL4B 7 1.299731 0.417213 -0.026411 10.50000 0.09012 AFIX 6 PART 1 S4 6 0.852100 0.279881 0.269432 21.00000 0.02599 0.04942 = 0.04988 -0.02407 -0.01454 0.00100 O13 4 0.807640 0.366481 0.207553 21.00000 0.04062 O14 4 0.857992 0.190011 0.255021 21.00000 0.05461 O15 4 0.817111 0.275519 0.363123 21.00000 0.05856 C44 1 0.983341 0.291701 0.251073 21.00000 0.03512 F1 5 0.989960 0.367521 0.271244 21.00000 0.05672 F2 5 1.039590 0.213451 0.297573 21.00000 0.05995 F3 5 1.023220 0.306672 0.163813 21.00000 0.07753 AFIX 6 PART 2 S4B 6 0.834341 0.264928 0.296474 -21.00000 0.03321 0.06035 = 0.09403 -0.04652 -0.02668 0.00646 O13B 4 0.798409 0.322554 0.214903 -21.00000 0.10629 O14B 4 0.829443 0.163927 0.328258 -21.00000 0.10445 O15B 4 0.799581 0.309882 0.367341 -21.00000 0.05389 C44B 1 0.969191 0.266890 0.268711 -21.00000 0.05618 F1B 5 0.985249 0.356251 0.246776 -21.00000 0.09295 F2B 5 1.017901 0.209764 0.334622 -21.00000 0.04266 F3B 5 1.010290 0.236307 0.197063 -21.00000 0.11388 PART 0 HKLF 4 REM asb241 in P-1 REM R1 = 0.0530 for 11026 Fo > 4sig(Fo) and 0.0585 for all 12276 data REM 674 parameters refined using 1 restraints END WGHT 0.0738 8.9899 REM Highest difference peak 1.949, deepest hole -1.455, 1-sigma level 0.103 Q1 1 0.8770 0.2013 0.2193 11.00000 0.05 1.95 Q2 1 1.0398 0.2728 0.1841 11.00000 0.05 1.51 Q3 1 1.1553 0.5382 0.0498 11.00000 0.05 1.39 Q4 1 0.8358 0.1791 0.2943 11.00000 0.05 1.39 Q5 1 0.8279 0.2242 0.3648 11.00000 0.05 1.28 Q6 1 0.9887 0.3259 0.2214 11.00000 0.05 1.28 Q7 1 1.1041 0.4393 0.0470 11.00000 0.05 1.13 Q8 1 -0.1248 0.9705 0.4435 11.00000 0.05 1.08 Q9 1 1.1011 0.5854 0.0842 11.00000 0.05 1.07 Q10 1 0.7854 0.3448 0.2415 11.00000 0.05 1.02 ; data_asb265 _database_code_depnum_ccdc_archive 'CCDC 895611' #TrackingRef '13191_web_deposit_cif_file_0_NathanielS.Sickerman_1344538304.SuperCif.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H68 Ca Cl2 F3 Ga N4 O15 S4' _chemical_formula_weight 1270.97 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' Ga Ga 0.2307 1.6083 '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 14.3885(5) _cell_length_b 14.7196(5) _cell_length_c 15.8403(6) _cell_angle_alpha 112.8012(4) _cell_angle_beta 97.8526(4) _cell_angle_gamma 106.3846(4) _cell_volume 2850.07(18) _cell_formula_units_Z 2 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.74 _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7239 _exptl_absorpt_correction_T_max 0.7916 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 33065 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _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 1.61 _diffrn_reflns_theta_max 27.10 _reflns_number_total 12505 _reflns_number_gt 11177 _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. Hydrogen atom H(7) was located from a difference-Fourier map and refined (x,y,z and Uiso) with d(O-H) fixed at 0.85 ang. The remaining hydrogen atoms were included using a riding model. The fluorine atoms, carbon C(45) and oxygen atoms O(13), O(14) and O(15) were disordered and included using multiple components and partial site-occupancy-factors. Equivalent isotropic thermal parameters were used for the fluorine atoms and oxygen atoms associated with the triflate anion. There was one molecule of dichloromethane solvent present. ; _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^)+(0.0648P)^2^+3.8509P] 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 12505 _refine_ls_number_parameters 672 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.181383(19) 0.44563(2) 0.707407(18) 0.02265(8) Uani 1 1 d . . . Ca1 Ca 0.08938(4) 0.23793(4) 0.78617(3) 0.02526(11) Uani 1 1 d . . . S1 S 0.24947(5) 0.25278(5) 0.62282(5) 0.02955(14) Uani 1 1 d . . . S2 S -0.04895(4) 0.27712(5) 0.60810(4) 0.02492(13) Uani 1 1 d . . . S3 S 0.19627(5) 0.66164(5) 0.88633(5) 0.03106(14) Uani 1 1 d . . . O1 O 0.18185(15) 0.21812(15) 0.67371(15) 0.0361(4) Uani 1 1 d . . . O2 O 0.21274(17) 0.19552(19) 0.52060(15) 0.0462(5) Uani 1 1 d . . . O3 O -0.03350(13) 0.27236(15) 0.69860(13) 0.0305(4) Uani 1 1 d . . . O4 O -0.06739(15) 0.18050(15) 0.52536(15) 0.0380(4) Uani 1 1 d . . . O5 O 0.18053(16) 0.59363(15) 0.93311(14) 0.0388(5) Uani 1 1 d . . . O6 O 0.11597(15) 0.69927(16) 0.87253(16) 0.0434(5) Uani 1 1 d . . . O7 O 0.17106(14) 0.40518(14) 0.80356(12) 0.0266(4) Uani 1 1 d D . . H7 H 0.172(3) 0.4612(19) 0.848(2) 0.069(13) Uiso 1 1 d D . . O8 O 0.2357(2) 0.2835(3) 0.9189(2) 0.0779(9) Uani 1 1 d . . . O9 O 0.1370(2) 0.0896(2) 0.7819(2) 0.0547(6) Uani 1 1 d . . . O10 O -0.03274(17) 0.05643(16) 0.67313(16) 0.0425(5) Uani 1 1 d . . . O11 O -0.06286(14) 0.17744(16) 0.83771(14) 0.0351(4) Uani 1 1 d . . . O12 O 0.08757(17) 0.3605(2) 0.94796(15) 0.0525(6) Uani 1 1 d . . . N1 N 0.21275(17) 0.50365(18) 0.60098(16) 0.0298(5) Uani 1 1 d . . . N2 N 0.27584(16) 0.37594(18) 0.65929(16) 0.0295(5) Uani 1 1 d . . . N3 N 0.04471(15) 0.37211(17) 0.61590(14) 0.0256(4) Uani 1 1 d . . . N4 N 0.21821(17) 0.60186(17) 0.78703(16) 0.0307(5) Uani 1 1 d . . . C1 C 0.2685(2) 0.4450(3) 0.5431(2) 0.0387(6) Uani 1 1 d . . . H1B H 0.3093 0.4884 0.5171 0.046 Uiso 1 1 calc R . . H1C H 0.2204 0.3782 0.4891 0.046 Uiso 1 1 calc R . . C2 C 0.3366(2) 0.4212(3) 0.6071(2) 0.0399(7) Uani 1 1 d . . . H2A H 0.3643 0.3702 0.5683 0.048 Uiso 1 1 calc R . . H2B H 0.3936 0.4871 0.6527 0.048 Uiso 1 1 calc R . . C3 C 0.3634(2) 0.2331(2) 0.6583(2) 0.0340(6) Uani 1 1 d . . . C4 C 0.3839(3) 0.1474(3) 0.5949(3) 0.0504(8) Uani 1 1 d . . . C5 C 0.4732(3) 0.1354(4) 0.6267(3) 0.0655(11) Uani 1 1 d . . . H5B H 0.4884 0.0784 0.5850 0.079 Uiso 1 1 calc R . . C6 C 0.5395(3) 0.2015(4) 0.7147(3) 0.0638(11) Uani 1 1 d . . . C7 C 0.5169(3) 0.2832(3) 0.7754(3) 0.0541(9) Uani 1 1 d . . . H7B H 0.5624 0.3291 0.8371 0.065 Uiso 1 1 calc R . . C8 C 0.4294(2) 0.3013(3) 0.7498(2) 0.0400(7) Uani 1 1 d . . . C9 C 0.3183(4) 0.0678(4) 0.4951(3) 0.0810(15) Uani 1 1 d . . . H9A H 0.2478 0.0431 0.4960 0.121 Uiso 1 1 calc R . . H9B H 0.3402 0.0074 0.4723 0.121 Uiso 1 1 calc R . . H9C H 0.3243 0.1014 0.4524 0.121 Uiso 1 1 calc R . . C10 C 0.6378(4) 0.1874(5) 0.7451(4) 0.0966(19) Uani 1 1 d . . . H10A H 0.6227 0.1167 0.7420 0.145 Uiso 1 1 calc R . . H10B H 0.6746 0.2413 0.8106 0.145 Uiso 1 1 calc R . . H10C H 0.6793 0.1952 0.7023 0.145 Uiso 1 1 calc R . . C11 C 0.4153(3) 0.3951(3) 0.8229(2) 0.0526(9) Uani 1 1 d . . . H11A H 0.4554 0.4137 0.8865 0.079 Uiso 1 1 calc R . . H11B H 0.3439 0.3772 0.8212 0.079 Uiso 1 1 calc R . . H11C H 0.4376 0.4555 0.8085 0.079 Uiso 1 1 calc R . . C12 C 0.1130(2) 0.4818(2) 0.5419(2) 0.0340(6) Uani 1 1 d . . . H12A H 0.1191 0.4829 0.4808 0.041 Uiso 1 1 calc R . . H12B H 0.0868 0.5372 0.5755 0.041 Uiso 1 1 calc R . . C13 C 0.0411(2) 0.3743(2) 0.52320(19) 0.0336(6) Uani 1 1 d . . . H13A H -0.0282 0.3625 0.4911 0.040 Uiso 1 1 calc R . . H13B H 0.0615 0.3177 0.4815 0.040 Uiso 1 1 calc R . . C14 C -0.15806(18) 0.31206(19) 0.59622(17) 0.0250(5) Uani 1 1 d . . . C15 C -0.2439(2) 0.2483(2) 0.51725(19) 0.0327(6) Uani 1 1 d . . . C16 C -0.3290(2) 0.2764(2) 0.5193(2) 0.0376(6) Uani 1 1 d . . . H16A H -0.3879 0.2329 0.4672 0.045 Uiso 1 1 calc R . . C17 C -0.3317(2) 0.3637(2) 0.5928(2) 0.0367(6) Uani 1 1 d . . . C18 C -0.2451(2) 0.4272(2) 0.6677(2) 0.0376(6) Uani 1 1 d . . . H18A H -0.2451 0.4889 0.7182 0.045 Uiso 1 1 calc R . . C19 C -0.1580(2) 0.4036(2) 0.67155(19) 0.0308(5) Uani 1 1 d . . . C20 C -0.2514(3) 0.1537(3) 0.4282(2) 0.0610(11) Uani 1 1 d . . . H20A H -0.2007 0.1761 0.3976 0.092 Uiso 1 1 calc R . . H20B H -0.3188 0.1239 0.3839 0.092 Uiso 1 1 calc R . . H20C H -0.2396 0.0999 0.4453 0.092 Uiso 1 1 calc R . . C21 C -0.4261(2) 0.3901(3) 0.5921(3) 0.0539(9) Uani 1 1 d . . . H21A H -0.4634 0.3666 0.5261 0.081 Uiso 1 1 calc R . . H21B H -0.4074 0.4669 0.6281 0.081 Uiso 1 1 calc R . . H21C H -0.4686 0.3540 0.6215 0.081 Uiso 1 1 calc R . . C22 C -0.0684(2) 0.4788(3) 0.7563(2) 0.0477(8) Uani 1 1 d . . . H22A H -0.0874 0.5329 0.8018 0.072 Uiso 1 1 calc R . . H22B H -0.0137 0.5129 0.7353 0.072 Uiso 1 1 calc R . . H22C H -0.0457 0.4395 0.7871 0.072 Uiso 1 1 calc R . . C23 C 0.2735(2) 0.6181(2) 0.6541(2) 0.0403(7) Uani 1 1 d . . . H23A H 0.2706 0.6519 0.6112 0.048 Uiso 1 1 calc R . . H23B H 0.3448 0.6288 0.6786 0.048 Uiso 1 1 calc R . . C24 C 0.2329(3) 0.6683(2) 0.7366(2) 0.0417(7) Uani 1 1 d . . . H24A H 0.2812 0.7408 0.7805 0.050 Uiso 1 1 calc R . . H24B H 0.1680 0.6728 0.7125 0.050 Uiso 1 1 calc R . . C25 C 0.3073(2) 0.7757(2) 0.96210(19) 0.0313(5) Uani 1 1 d . . . C26 C 0.3960(2) 0.7587(2) 0.9886(2) 0.0386(6) Uani 1 1 d . . . C27 C 0.4795(2) 0.8453(3) 1.0546(2) 0.0480(8) Uani 1 1 d . . . H27A H 0.5396 0.8345 1.0730 0.058 Uiso 1 1 calc R . . C28 C 0.4784(3) 0.9470(3) 1.0949(2) 0.0492(8) Uani 1 1 d . . . C29 C 0.3914(3) 0.9620(2) 1.0664(2) 0.0467(7) Uani 1 1 d . . . H29A H 0.3906 1.0317 1.0930 0.056 Uiso 1 1 calc R . . C30 C 0.3042(2) 0.8785(2) 0.9998(2) 0.0383(6) Uani 1 1 d . . . C31 C 0.4073(3) 0.6522(3) 0.9476(3) 0.0506(8) Uani 1 1 d . . . H31A H 0.3525 0.6000 0.9539 0.076 Uiso 1 1 calc R . . H31B H 0.4723 0.6582 0.9824 0.076 Uiso 1 1 calc R . . H31C H 0.4044 0.6296 0.8801 0.076 Uiso 1 1 calc R . . C32 C 0.5702(3) 1.0396(4) 1.1681(3) 0.0775(14) Uani 1 1 d . . . H32A H 0.5816 1.0325 1.2273 0.116 Uiso 1 1 calc R . . H32B H 0.5592 1.1058 1.1807 0.116 Uiso 1 1 calc R . . H32C H 0.6293 1.0404 1.1438 0.116 Uiso 1 1 calc R . . C33 C 0.2155(3) 0.9090(3) 0.9754(3) 0.0595(10) Uani 1 1 d . . . H33A H 0.2350 0.9860 1.0102 0.089 Uiso 1 1 calc R . . H33B H 0.1587 0.8738 0.9936 0.089 Uiso 1 1 calc R . . H33C H 0.1956 0.8869 0.9067 0.089 Uiso 1 1 calc R . . C34 C 0.2425(4) 0.1953(5) 0.9344(4) 0.0904(17) Uani 1 1 d . . . H34A H 0.3097 0.2156 0.9768 0.108 Uiso 1 1 calc R . . H34B H 0.1907 0.1740 0.9653 0.108 Uiso 1 1 calc R . . C35 C 0.2269(4) 0.1088(4) 0.8439(4) 0.0812(15) Uani 1 1 d . . . H35A H 0.2840 0.1266 0.8172 0.097 Uiso 1 1 calc R . . H35B H 0.2233 0.0446 0.8520 0.097 Uiso 1 1 calc R . . C36 C 0.0979(4) -0.0095(3) 0.6992(5) 0.0923(19) Uani 1 1 d . . . H36A H 0.0672 -0.0668 0.7163 0.111 Uiso 1 1 calc R . . H36B H 0.1532 -0.0235 0.6719 0.111 Uiso 1 1 calc R . . C37 C 0.0203(3) -0.0081(3) 0.6271(3) 0.0706(13) Uani 1 1 d . . . H37A H 0.0535 0.0199 0.5869 0.085 Uiso 1 1 calc R . . H37B H -0.0280 -0.0812 0.5852 0.085 Uiso 1 1 calc R . . C38 C -0.1041(2) 0.0082(2) 0.7113(2) 0.0441(7) Uani 1 1 d . . . H38A H -0.0712 -0.0131 0.7556 0.053 Uiso 1 1 calc R . . H38B H -0.1586 -0.0555 0.6595 0.053 Uiso 1 1 calc R . . C40 C -0.0886(2) 0.2657(3) 0.8911(2) 0.0439(7) Uani 1 1 d . . . H40A H -0.1508 0.2414 0.9093 0.053 Uiso 1 1 calc R . . H40B H -0.1002 0.3029 0.8528 0.053 Uiso 1 1 calc R . . C39 C -0.1459(2) 0.0898(3) 0.7631(2) 0.0437(7) Uani 1 1 d . . . H39A H -0.1770 0.1126 0.7191 0.052 Uiso 1 1 calc R . . H39B H -0.1979 0.0602 0.7902 0.052 Uiso 1 1 calc R . . C41 C -0.0019(2) 0.3379(3) 0.9782(2) 0.0478(8) Uani 1 1 d . . . H41A H -0.0126 0.4043 1.0141 0.057 Uiso 1 1 calc R . . H41B H 0.0044 0.3034 1.0202 0.057 Uiso 1 1 calc R . . C42 C 0.1780(3) 0.4008(5) 1.0253(3) 0.098(2) Uani 1 1 d . . . H42A H 0.1979 0.4785 1.0615 0.117 Uiso 1 1 calc R . . H42B H 0.1619 0.3696 1.0693 0.117 Uiso 1 1 calc R . . C43 C 0.2578(6) 0.3800(6) 0.9970(5) 0.157(4) Uani 1 1 d . . . H43A H 0.3041 0.3834 1.0514 0.188 Uiso 1 1 calc R . . H43B H 0.2947 0.4370 0.9819 0.188 Uiso 1 1 calc R . . C44 C 0.9266(3) 0.7596(3) 0.8167(3) 0.0544(9) Uani 1 1 d . . . H44A H 0.9666 0.7298 0.8469 0.065 Uiso 1 1 calc R . . H44B H 0.8544 0.7208 0.8068 0.065 Uiso 1 1 calc R . . Cl1 Cl 0.95802(11) 0.89287(11) 0.89338(8) 0.0882(4) Uani 1 1 d . . . Cl2 Cl 0.94817(12) 0.73933(11) 0.70656(8) 0.0877(4) Uani 1 1 d . . . S4 S 0.61847(7) 0.71055(7) 0.79210(7) 0.0532(2) Uani 1 1 d . . . O13 O 0.6934(8) 0.6647(8) 0.8021(7) 0.0827(8) Uiso 0.50 1 d P A 1 O14 O 0.6206(6) 0.7950(6) 0.8765(5) 0.0827(8) Uiso 0.50 1 d P A 1 O15 O 0.5186(6) 0.6240(6) 0.7471(5) 0.0827(8) Uiso 0.50 1 d P A 1 C45 C 0.6210(8) 0.7326(9) 0.6936(7) 0.060(2) Uiso 0.50 1 d P A 1 F1 F 0.5963(6) 0.8230(6) 0.6949(6) 0.1122(10) Uiso 0.50 1 d P A 1 F2 F 0.5734(6) 0.6396(6) 0.6108(6) 0.1122(10) Uiso 0.50 1 d P A 1 F3 F 0.7123(6) 0.7692(7) 0.6754(6) 0.1122(10) Uiso 0.50 1 d P A 1 O13B O 0.6787(8) 0.6468(8) 0.7800(6) 0.0827(8) Uiso 0.50 1 d P A 2 O14B O 0.6745(6) 0.8141(6) 0.8688(5) 0.0827(8) Uiso 0.50 1 d P A 2 O15B O 0.5169(6) 0.6708(6) 0.7816(5) 0.0827(8) Uiso 0.50 1 d P A 2 C45B C 0.6468(11) 0.7740(12) 0.7122(10) 0.088(4) Uiso 0.50 1 d P A 2 F1B F 0.5567(6) 0.7814(7) 0.6820(6) 0.1122(10) Uiso 0.50 1 d P A 2 F2B F 0.6394(7) 0.6882(7) 0.6255(6) 0.1122(10) Uiso 0.50 1 d P A 2 F3B F 0.7292(6) 0.8408(7) 0.7438(6) 0.1122(10) Uiso 0.50 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 Ga1 0.02220(13) 0.02584(14) 0.02415(14) 0.01275(11) 0.00808(10) 0.01181(10) Ca1 0.0279(2) 0.0282(2) 0.0267(2) 0.0148(2) 0.01049(19) 0.0150(2) S1 0.0275(3) 0.0361(3) 0.0316(3) 0.0151(3) 0.0142(2) 0.0182(3) S2 0.0240(3) 0.0264(3) 0.0259(3) 0.0102(2) 0.0065(2) 0.0137(2) S3 0.0285(3) 0.0243(3) 0.0343(3) 0.0077(3) 0.0111(3) 0.0078(2) O1 0.0353(10) 0.0326(10) 0.0466(11) 0.0168(9) 0.0240(9) 0.0167(8) O2 0.0474(12) 0.0558(14) 0.0331(11) 0.0110(10) 0.0120(9) 0.0279(11) O3 0.0270(9) 0.0366(10) 0.0349(10) 0.0214(8) 0.0085(7) 0.0139(8) O4 0.0386(11) 0.0313(10) 0.0385(11) 0.0057(8) 0.0092(8) 0.0200(8) O5 0.0486(12) 0.0281(10) 0.0364(10) 0.0105(8) 0.0227(9) 0.0102(9) O6 0.0293(10) 0.0348(11) 0.0535(13) 0.0080(9) 0.0093(9) 0.0121(8) O7 0.0324(9) 0.0269(9) 0.0231(8) 0.0115(7) 0.0094(7) 0.0133(7) O8 0.079(2) 0.080(2) 0.0626(18) 0.0224(15) -0.0174(15) 0.0436(17) O9 0.0653(16) 0.0524(14) 0.0766(17) 0.0398(13) 0.0340(14) 0.0416(13) O10 0.0510(13) 0.0289(10) 0.0468(12) 0.0121(9) 0.0236(10) 0.0158(9) O11 0.0298(9) 0.0393(10) 0.0351(10) 0.0140(8) 0.0125(8) 0.0133(8) O12 0.0404(12) 0.0602(15) 0.0312(11) 0.0046(10) 0.0166(9) 0.0021(10) N1 0.0306(11) 0.0369(12) 0.0330(11) 0.0204(10) 0.0146(9) 0.0183(9) N2 0.0274(10) 0.0372(12) 0.0368(12) 0.0221(10) 0.0161(9) 0.0189(9) N3 0.0230(10) 0.0334(11) 0.0244(10) 0.0144(9) 0.0078(8) 0.0132(8) N4 0.0360(12) 0.0251(10) 0.0310(11) 0.0128(9) 0.0120(9) 0.0096(9) C1 0.0420(15) 0.0573(18) 0.0428(16) 0.0332(15) 0.0280(13) 0.0317(14) C2 0.0329(14) 0.0573(18) 0.0556(18) 0.0394(16) 0.0256(13) 0.0265(13) C3 0.0338(14) 0.0444(15) 0.0425(15) 0.0267(13) 0.0201(12) 0.0259(12) C4 0.058(2) 0.057(2) 0.056(2) 0.0279(17) 0.0270(17) 0.0410(18) C5 0.074(3) 0.080(3) 0.077(3) 0.039(2) 0.036(2) 0.064(2) C6 0.057(2) 0.095(3) 0.083(3) 0.057(3) 0.034(2) 0.058(2) C7 0.0416(18) 0.082(3) 0.059(2) 0.040(2) 0.0165(16) 0.0371(18) C8 0.0354(15) 0.0543(18) 0.0459(17) 0.0281(15) 0.0169(13) 0.0278(14) C9 0.100(4) 0.073(3) 0.066(3) 0.006(2) 0.019(2) 0.064(3) C10 0.080(3) 0.149(5) 0.111(4) 0.070(4) 0.035(3) 0.091(4) C11 0.0467(18) 0.068(2) 0.0395(17) 0.0140(16) 0.0029(14) 0.0341(17) C12 0.0374(14) 0.0465(16) 0.0335(14) 0.0259(12) 0.0137(11) 0.0235(12) C13 0.0338(14) 0.0489(16) 0.0256(12) 0.0210(12) 0.0087(10) 0.0191(12) C14 0.0223(11) 0.0286(12) 0.0270(12) 0.0128(10) 0.0075(9) 0.0128(9) C15 0.0287(13) 0.0361(14) 0.0303(13) 0.0128(11) 0.0043(10) 0.0125(11) C16 0.0246(13) 0.0471(16) 0.0410(15) 0.0232(13) 0.0037(11) 0.0107(12) C17 0.0263(13) 0.0474(16) 0.0531(17) 0.0318(14) 0.0181(12) 0.0202(12) C18 0.0338(14) 0.0375(15) 0.0464(16) 0.0163(13) 0.0176(12) 0.0205(12) C19 0.0279(12) 0.0323(13) 0.0316(13) 0.0107(11) 0.0103(10) 0.0144(10) C20 0.0484(19) 0.060(2) 0.0398(18) -0.0079(16) -0.0115(15) 0.0258(17) C21 0.0311(15) 0.068(2) 0.083(3) 0.043(2) 0.0237(16) 0.0298(16) C22 0.0384(16) 0.0414(17) 0.0405(16) -0.0049(13) 0.0029(13) 0.0198(13) C23 0.0445(16) 0.0393(16) 0.0448(16) 0.0274(14) 0.0171(13) 0.0120(13) C24 0.0585(19) 0.0283(14) 0.0404(16) 0.0181(12) 0.0159(14) 0.0138(13) C25 0.0302(13) 0.0257(12) 0.0312(13) 0.0087(10) 0.0081(10) 0.0068(10) C26 0.0341(14) 0.0353(15) 0.0412(16) 0.0126(12) 0.0109(12) 0.0115(12) C27 0.0330(15) 0.0478(18) 0.0497(18) 0.0135(15) 0.0048(13) 0.0110(13) C28 0.0386(16) 0.0414(17) 0.0431(17) 0.0065(14) 0.0029(13) 0.0020(13) C29 0.0501(18) 0.0273(14) 0.0453(17) 0.0071(13) 0.0066(14) 0.0059(13) C30 0.0398(15) 0.0290(14) 0.0381(15) 0.0099(12) 0.0066(12) 0.0107(12) C31 0.0415(17) 0.0428(17) 0.064(2) 0.0168(16) 0.0099(15) 0.0221(14) C32 0.052(2) 0.059(2) 0.067(3) 0.000(2) -0.008(2) -0.0029(19) C33 0.059(2) 0.0293(16) 0.072(2) 0.0108(16) -0.0052(18) 0.0188(15) C34 0.098(4) 0.149(5) 0.074(3) 0.072(4) 0.023(3) 0.084(4) C35 0.071(3) 0.083(3) 0.126(4) 0.065(3) 0.027(3) 0.054(3) C36 0.067(3) 0.038(2) 0.159(5) 0.020(3) 0.038(3) 0.033(2) C37 0.064(2) 0.0356(18) 0.088(3) -0.0005(18) 0.041(2) 0.0161(17) C38 0.0433(17) 0.0337(15) 0.0504(18) 0.0172(13) 0.0148(14) 0.0086(13) C40 0.0377(15) 0.0529(18) 0.0394(16) 0.0131(14) 0.0177(13) 0.0219(14) C39 0.0309(14) 0.0458(17) 0.0453(17) 0.0148(14) 0.0104(12) 0.0092(13) C41 0.0430(17) 0.057(2) 0.0348(15) 0.0111(14) 0.0214(13) 0.0159(15) C42 0.044(2) 0.127(4) 0.038(2) -0.014(2) 0.0071(17) -0.010(2) C43 0.127(6) 0.162(7) 0.089(4) -0.035(4) -0.063(4) 0.098(5) C44 0.059(2) 0.068(2) 0.0474(19) 0.0325(18) 0.0170(16) 0.0286(18) Cl1 0.0992(9) 0.0890(8) 0.0549(6) 0.0063(6) 0.0007(6) 0.0513(7) Cl2 0.1268(11) 0.0859(8) 0.0427(5) 0.0270(5) 0.0284(6) 0.0286(8) S4 0.0473(5) 0.0466(5) 0.0526(5) 0.0132(4) 0.0087(4) 0.0142(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 Ga1 O7 1.8469(17) . ? Ga1 N2 1.986(2) . ? Ga1 N3 1.986(2) . ? Ga1 N4 2.010(2) . ? Ga1 N1 2.209(2) . ? Ca1 O7 2.2959(18) . ? Ca1 O1 2.3437(19) . ? Ca1 O3 2.3847(18) . ? Ca1 O9 2.446(2) . ? Ca1 O8 2.491(3) . ? Ca1 O11 2.492(2) . ? Ca1 O10 2.493(2) . ? Ca1 O12 2.507(2) . ? S1 O2 1.438(2) . ? S1 O1 1.452(2) . ? S1 N2 1.583(2) . ? S1 C3 1.798(3) . ? S2 O4 1.4347(19) . ? S2 O3 1.4522(19) . ? S2 N3 1.595(2) . ? S2 C14 1.793(2) . ? S3 O6 1.441(2) . ? S3 O5 1.448(2) . ? S3 N4 1.602(2) . ? S3 C25 1.792(3) . ? O5 H7 1.846(8) . ? O8 C43 1.388(6) . ? O8 C34 1.437(6) . ? O9 C35 1.397(5) . ? O9 C36 1.419(5) . ? O10 C38 1.418(4) . ? O10 C37 1.428(4) . ? O11 C40 1.430(4) . ? O11 C39 1.432(4) . ? O12 C41 1.431(4) . ? O12 C42 1.454(5) . ? N1 C23 1.476(4) . ? N1 C12 1.476(3) . ? N1 C1 1.485(3) . ? N2 C2 1.479(3) . ? N3 C13 1.475(3) . ? N4 C24 1.474(4) . ? C1 C2 1.520(4) . ? C3 C8 1.404(4) . ? C3 C4 1.412(4) . ? C4 C5 1.398(5) . ? C4 C9 1.516(6) . ? C5 C6 1.364(6) . ? C6 C7 1.375(6) . ? C6 C10 1.527(5) . ? C7 C8 1.398(4) . ? C8 C11 1.507(5) . ? C12 C13 1.514(4) . ? C14 C15 1.409(4) . ? C14 C19 1.411(3) . ? C15 C16 1.399(4) . ? C15 C20 1.514(4) . ? C16 C17 1.375(4) . ? C17 C18 1.383(4) . ? C17 C21 1.514(4) . ? C18 C19 1.391(4) . ? C19 C22 1.503(4) . ? C23 C24 1.516(4) . ? C25 C26 1.407(4) . ? C25 C30 1.413(4) . ? C26 C27 1.385(4) . ? C26 C31 1.513(4) . ? C27 C28 1.387(5) . ? C28 C29 1.377(5) . ? C28 C32 1.513(5) . ? C29 C30 1.401(4) . ? C30 C33 1.517(5) . ? C34 C35 1.437(7) . ? C36 C37 1.495(8) . ? C38 C39 1.502(5) . ? C40 C41 1.494(5) . ? C42 C43 1.360(8) . ? C44 Cl2 1.739(4) . ? C44 Cl1 1.741(4) . ? S4 O15B 1.371(8) . ? S4 O14 1.418(8) . ? S4 O13B 1.426(12) . ? S4 O14B 1.433(8) . ? S4 O13 1.445(12) . ? S4 O15 1.477(8) . ? S4 C45 1.715(10) . ? S4 C45B 1.866(14) . ? C45 F2 1.377(13) . ? C45 F3 1.387(13) . ? C45 F1 1.465(14) . ? C45B F3B 1.193(15) . ? C45B F1B 1.368(16) . ? C45B F2B 1.425(16) . ? 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 Ga1 N2 96.82(8) . . ? O7 Ga1 N3 105.22(8) . . ? N2 Ga1 N3 111.47(9) . . ? O7 Ga1 N4 97.62(8) . . ? N2 Ga1 N4 125.65(10) . . ? N3 Ga1 N4 114.51(9) . . ? O7 Ga1 N1 173.31(8) . . ? N2 Ga1 N1 79.93(8) . . ? N3 Ga1 N1 81.44(8) . . ? N4 Ga1 N1 79.81(9) . . ? O7 Ca1 O1 73.88(7) . . ? O7 Ca1 O3 75.12(6) . . ? O1 Ca1 O3 93.59(7) . . ? O7 Ca1 O9 136.26(8) . . ? O1 Ca1 O9 77.81(8) . . ? O3 Ca1 O9 139.83(9) . . ? O7 Ca1 O8 84.73(9) . . ? O1 Ca1 O8 93.79(10) . . ? O3 Ca1 O8 155.65(9) . . ? O9 Ca1 O8 64.50(10) . . ? O7 Ca1 O11 127.18(7) . . ? O1 Ca1 O11 152.06(7) . . ? O3 Ca1 O11 77.35(7) . . ? O9 Ca1 O11 92.06(8) . . ? O8 Ca1 O11 105.34(10) . . ? O7 Ca1 O10 144.89(7) . . ? O1 Ca1 O10 86.66(7) . . ? O3 Ca1 O10 77.32(7) . . ? O9 Ca1 O10 63.18(9) . . ? O8 Ca1 O10 126.27(9) . . ? O11 Ca1 O10 65.65(7) . . ? O7 Ca1 O12 75.00(7) . . ? O1 Ca1 O12 143.82(8) . . ? O3 Ca1 O12 95.85(8) . . ? O9 Ca1 O12 114.28(9) . . ? O8 Ca1 O12 65.30(10) . . ? O11 Ca1 O12 64.05(7) . . ? O10 Ca1 O12 129.49(7) . . ? O2 S1 O1 114.98(14) . . ? O2 S1 N2 111.96(14) . . ? O1 S1 N2 107.56(11) . . ? O2 S1 C3 107.57(13) . . ? O1 S1 C3 106.51(12) . . ? N2 S1 C3 107.92(13) . . ? O4 S2 O3 115.84(12) . . ? O4 S2 N3 111.50(12) . . ? O3 S2 N3 108.20(11) . . ? O4 S2 C14 107.89(12) . . ? O3 S2 C14 105.50(11) . . ? N3 S2 C14 107.45(11) . . ? O6 S3 O5 114.94(14) . . ? O6 S3 N4 110.81(13) . . ? O5 S3 N4 109.16(12) . . ? O6 S3 C25 107.11(13) . . ? O5 S3 C25 106.46(13) . . ? N4 S3 C25 108.04(12) . . ? S1 O1 Ca1 156.20(12) . . ? S2 O3 Ca1 134.21(11) . . ? S3 O5 H7 108.2(14) . . ? Ga1 O7 Ca1 126.94(9) . . ? C43 O8 C34 119.1(5) . . ? C43 O8 Ca1 113.8(3) . . ? C34 O8 Ca1 114.8(3) . . ? C35 O9 C36 115.1(3) . . ? C35 O9 Ca1 119.9(3) . . ? C36 O9 Ca1 121.2(3) . . ? C38 O10 C37 113.8(3) . . ? C38 O10 Ca1 115.44(18) . . ? C37 O10 Ca1 109.8(2) . . ? C40 O11 C39 114.0(2) . . ? C40 O11 Ca1 110.20(17) . . ? C39 O11 Ca1 114.59(17) . . ? C41 O12 C42 111.7(3) . . ? C41 O12 Ca1 119.39(18) . . ? C42 O12 Ca1 116.4(2) . . ? C23 N1 C12 112.4(2) . . ? C23 N1 C1 111.3(2) . . ? C12 N1 C1 111.3(2) . . ? C23 N1 Ga1 107.10(16) . . ? C12 N1 Ga1 105.44(15) . . ? C1 N1 Ga1 108.99(16) . . ? C2 N2 S1 113.94(19) . . ? C2 N2 Ga1 115.06(17) . . ? S1 N2 Ga1 122.14(12) . . ? C13 N3 S2 111.63(17) . . ? C13 N3 Ga1 114.07(16) . . ? S2 N3 Ga1 129.57(12) . . ? C24 N4 S3 110.63(18) . . ? C24 N4 Ga1 116.54(18) . . ? S3 N4 Ga1 128.88(13) . . ? N1 C1 C2 108.1(2) . . ? N2 C2 C1 108.1(2) . . ? C8 C3 C4 120.9(3) . . ? C8 C3 S1 119.4(2) . . ? C4 C3 S1 119.7(2) . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C9 117.0(3) . . ? C3 C4 C9 125.8(3) . . ? C6 C5 C4 123.3(3) . . ? C5 C6 C7 118.3(3) . . ? C5 C6 C10 121.4(4) . . ? C7 C6 C10 120.3(4) . . ? C6 C7 C8 122.4(4) . . ? C7 C8 C3 118.0(3) . . ? C7 C8 C11 116.6(3) . . ? C3 C8 C11 125.4(3) . . ? N1 C12 C13 109.2(2) . . ? N3 C13 C12 107.8(2) . . ? C15 C14 C19 120.2(2) . . ? C15 C14 S2 121.93(19) . . ? C19 C14 S2 117.79(19) . . ? C16 C15 C14 117.6(3) . . ? C16 C15 C20 116.6(3) . . ? C14 C15 C20 125.8(3) . . ? C17 C16 C15 123.3(3) . . ? C16 C17 C18 117.8(2) . . ? C16 C17 C21 121.3(3) . . ? C18 C17 C21 120.9(3) . . ? C17 C18 C19 122.2(3) . . ? C18 C19 C14 118.8(2) . . ? C18 C19 C22 117.4(2) . . ? C14 C19 C22 123.8(2) . . ? N1 C23 C24 109.5(2) . . ? N4 C24 C23 108.1(2) . . ? C26 C25 C30 120.9(3) . . ? C26 C25 S3 117.8(2) . . ? C30 C25 S3 121.1(2) . . ? C27 C26 C25 118.3(3) . . ? C27 C26 C31 117.5(3) . . ? C25 C26 C31 124.2(3) . . ? C26 C27 C28 122.4(3) . . ? C29 C28 C27 118.4(3) . . ? C29 C28 C32 120.5(3) . . ? C27 C28 C32 121.2(4) . . ? C28 C29 C30 122.5(3) . . ? C29 C30 C25 117.5(3) . . ? C29 C30 C33 115.8(3) . . ? C25 C30 C33 126.7(3) . . ? C35 C34 O8 108.6(4) . . ? O9 C35 C34 108.9(4) . . ? O9 C36 C37 109.6(3) . . ? O10 C37 C36 110.6(4) . . ? O10 C38 C39 106.4(2) . . ? O11 C40 C41 106.9(3) . . ? O11 C39 C38 106.7(2) . . ? O12 C41 C40 107.8(2) . . ? C43 C42 O12 114.5(4) . . ? C42 C43 O8 116.4(6) . . ? Cl2 C44 Cl1 112.8(2) . . ? O15B S4 O14 84.9(5) . . ? O15B S4 O13B 122.5(5) . . ? O14 S4 O13B 128.9(5) . . ? O15B S4 O14B 116.5(5) . . ? O14 S4 O14B 32.2(3) . . ? O13B S4 O14B 109.8(5) . . ? O15B S4 O13 129.4(6) . . ? O14 S4 O13 115.8(5) . . ? O13B S4 O13 13.4(6) . . ? O14B S4 O13 96.9(5) . . ? O15B S4 O15 28.3(4) . . ? O14 S4 O15 112.4(4) . . ? O13B S4 O15 97.9(5) . . ? O14B S4 O15 144.4(4) . . ? O13 S4 O15 108.0(5) . . ? O15B S4 C45 101.9(5) . . ? O14 S4 C45 117.2(5) . . ? O13B S4 C45 99.4(6) . . ? O14B S4 C45 102.4(5) . . ? O13 S4 C45 106.8(6) . . ? O15 S4 C45 94.4(5) . . ? O15B S4 C45B 111.8(6) . . ? O14 S4 C45B 103.4(6) . . ? O13B S4 C45B 103.7(6) . . ? O14B S4 C45B 85.6(6) . . ? O13 S4 C45B 107.4(6) . . ? O15 S4 C45B 109.6(6) . . ? C45 S4 C45B 16.9(5) . . ? F2 C45 F3 99.6(8) . . ? F2 C45 F1 115.2(8) . . ? F3 C45 F1 91.9(8) . . ? F2 C45 S4 111.2(7) . . ? F3 C45 S4 120.0(7) . . ? F1 C45 S4 116.8(7) . . ? F3B C45B F1B 128.6(14) . . ? F3B C45B F2B 110.9(12) . . ? F1B C45B F2B 96.7(10) . . ? F3B C45B S4 111.7(10) . . ? F1B C45B S4 102.1(9) . . ? F2B C45B S4 103.6(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.172 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.075 _iucr_refine_instructions_details ; TITL asb265 in P-1 CELL 0.71073 14.3885 14.7196 15.8403 112.8012 97.8526 106.3846 ZERR 2.00 0.0005 0.0005 0.0006 0.0004 0.0004 0.0004 LATT 1 SFAC C H N O F S CL CA GA UNIT 90 136 8 30 6 8 4 2 2 TEMP -75.000 SIZE 0.276 0.327 0.389 rem SADABS data 7/1/12 CONN 8 CA1 CONN 5 GA1 EADP F1 F2 F3 F1B F2B F3B EADP O13 O14 O15 O13B O14B O15B OMIT 0 -1 1 OMIT 0 0 1 OMIT 1 0 0 SHEL 100 0.78 DFIX 0.85 0.001 O7 H7 BIND O5 H7 L.S. 12 FMAP 2 PLAN 10 ACTA 51 WGHT 0.064800 3.850900 FVAR 0.10941 GA1 9 0.181383 0.445626 0.707407 11.00000 0.02220 0.02584 = 0.02415 0.01275 0.00808 0.01181 CA1 8 0.089378 0.237933 0.786167 11.00000 0.02787 0.02816 = 0.02667 0.01482 0.01049 0.01496 S1 6 0.249472 0.252779 0.622821 11.00000 0.02754 0.03612 = 0.03157 0.01511 0.01415 0.01820 S2 6 -0.048952 0.277122 0.608103 11.00000 0.02403 0.02636 = 0.02587 0.01021 0.00646 0.01372 S3 6 0.196268 0.661638 0.886332 11.00000 0.02853 0.02425 = 0.03428 0.00767 0.01111 0.00780 O1 4 0.181849 0.218115 0.673706 11.00000 0.03527 0.03262 = 0.04655 0.01675 0.02396 0.01674 O2 4 0.212735 0.195524 0.520596 11.00000 0.04741 0.05579 = 0.03311 0.01105 0.01196 0.02786 O3 4 -0.033502 0.272356 0.698597 11.00000 0.02702 0.03660 = 0.03494 0.02142 0.00852 0.01391 O4 4 -0.067390 0.180505 0.525358 11.00000 0.03859 0.03133 = 0.03847 0.00569 0.00916 0.01997 O5 4 0.180533 0.593630 0.933114 11.00000 0.04862 0.02815 = 0.03637 0.01045 0.02271 0.01023 O6 4 0.115970 0.699269 0.872534 11.00000 0.02926 0.03484 = 0.05347 0.00796 0.00932 0.01209 O7 4 0.171059 0.405181 0.803563 11.00000 0.03243 0.02690 = 0.02314 0.01147 0.00939 0.01327 H7 2 0.171898 0.461191 0.848394 11.00000 0.06879 O8 4 0.235719 0.283461 0.918872 11.00000 0.07931 0.07998 = 0.06256 0.02236 -0.01740 0.04360 O9 4 0.136992 0.089621 0.781859 11.00000 0.06527 0.05236 = 0.07665 0.03982 0.03404 0.04158 O10 4 -0.032745 0.056426 0.673128 11.00000 0.05097 0.02891 = 0.04677 0.01208 0.02365 0.01579 O11 4 -0.062857 0.177435 0.837706 11.00000 0.02983 0.03929 = 0.03508 0.01405 0.01249 0.01330 O12 4 0.087570 0.360543 0.947962 11.00000 0.04041 0.06017 = 0.03118 0.00459 0.01658 0.00208 N1 3 0.212751 0.503654 0.600984 11.00000 0.03061 0.03692 = 0.03299 0.02045 0.01459 0.01827 N2 3 0.275840 0.375938 0.659293 11.00000 0.02743 0.03722 = 0.03684 0.02214 0.01609 0.01893 N3 3 0.044712 0.372113 0.615897 11.00000 0.02296 0.03343 = 0.02438 0.01442 0.00777 0.01324 N4 3 0.218206 0.601855 0.787031 11.00000 0.03596 0.02511 = 0.03099 0.01280 0.01199 0.00959 C1 1 0.268486 0.445026 0.543099 11.00000 0.04202 0.05726 = 0.04282 0.03321 0.02795 0.03174 AFIX 23 H1B 2 0.309325 0.488362 0.517098 11.00000 -1.20000 H1C 2 0.220440 0.378193 0.489081 11.00000 -1.20000 AFIX 0 C2 1 0.336605 0.421244 0.607135 11.00000 0.03292 0.05727 = 0.05562 0.03945 0.02561 0.02650 AFIX 23 H2A 2 0.364338 0.370193 0.568318 11.00000 -1.20000 H2B 2 0.393574 0.487069 0.652728 11.00000 -1.20000 AFIX 0 C3 1 0.363419 0.233061 0.658288 11.00000 0.03375 0.04444 = 0.04254 0.02674 0.02009 0.02587 C4 1 0.383926 0.147427 0.594918 11.00000 0.05805 0.05717 = 0.05629 0.02788 0.02698 0.04104 C5 1 0.473199 0.135395 0.626711 11.00000 0.07393 0.07952 = 0.07722 0.03869 0.03627 0.06359 AFIX 43 H5B 2 0.488409 0.078383 0.584962 11.00000 -1.20000 AFIX 0 C6 1 0.539548 0.201454 0.714703 11.00000 0.05706 0.09504 = 0.08294 0.05653 0.03444 0.05844 C7 1 0.516888 0.283195 0.775443 11.00000 0.04156 0.08158 = 0.05920 0.04035 0.01650 0.03710 AFIX 43 H7B 2 0.562362 0.329073 0.837078 11.00000 -1.20000 AFIX 0 C8 1 0.429400 0.301279 0.749844 11.00000 0.03545 0.05428 = 0.04588 0.02815 0.01687 0.02776 C9 1 0.318267 0.067812 0.495073 11.00000 0.10015 0.07276 = 0.06586 0.00569 0.01950 0.06381 AFIX 137 H9A 2 0.247815 0.043090 0.496008 11.00000 -1.50000 H9B 2 0.340198 0.007437 0.472256 11.00000 -1.50000 H9C 2 0.324341 0.101437 0.452406 11.00000 -1.50000 AFIX 0 C10 1 0.637846 0.187389 0.745127 11.00000 0.07955 0.14875 = 0.11115 0.07011 0.03461 0.09079 AFIX 137 H10A 2 0.622671 0.116726 0.741952 11.00000 -1.50000 H10B 2 0.674633 0.241251 0.810606 11.00000 -1.50000 H10C 2 0.679318 0.195164 0.702350 11.00000 -1.50000 AFIX 0 C11 1 0.415341 0.395096 0.822884 11.00000 0.04674 0.06761 = 0.03953 0.01399 0.00291 0.03410 AFIX 137 H11A 2 0.455399 0.413652 0.886461 11.00000 -1.50000 H11B 2 0.343918 0.377179 0.821182 11.00000 -1.50000 H11C 2 0.437562 0.455483 0.808520 11.00000 -1.50000 AFIX 0 C12 1 0.112993 0.481850 0.541941 11.00000 0.03735 0.04647 = 0.03346 0.02595 0.01369 0.02347 AFIX 23 H12A 2 0.119057 0.482854 0.480774 11.00000 -1.20000 H12B 2 0.086783 0.537171 0.575462 11.00000 -1.20000 AFIX 0 C13 1 0.041133 0.374274 0.523197 11.00000 0.03381 0.04889 = 0.02561 0.02104 0.00871 0.01913 AFIX 23 H13A 2 -0.028223 0.362507 0.491085 11.00000 -1.20000 H13B 2 0.061510 0.317722 0.481458 11.00000 -1.20000 AFIX 0 C14 1 -0.158062 0.312061 0.596220 11.00000 0.02231 0.02864 = 0.02696 0.01279 0.00746 0.01276 C15 1 -0.243866 0.248324 0.517247 11.00000 0.02870 0.03608 = 0.03026 0.01275 0.00434 0.01253 C16 1 -0.329007 0.276394 0.519282 11.00000 0.02456 0.04707 = 0.04099 0.02315 0.00369 0.01074 AFIX 43 H16A 2 -0.387946 0.232885 0.467224 11.00000 -1.20000 AFIX 0 C17 1 -0.331688 0.363748 0.592801 11.00000 0.02630 0.04741 = 0.05312 0.03179 0.01814 0.02022 C18 1 -0.245100 0.427198 0.667701 11.00000 0.03385 0.03753 = 0.04641 0.01634 0.01760 0.02052 AFIX 43 H18A 2 -0.245095 0.488948 0.718204 11.00000 -1.20000 AFIX 0 C19 1 -0.157993 0.403605 0.671553 11.00000 0.02789 0.03230 = 0.03155 0.01072 0.01028 0.01443 C20 1 -0.251396 0.153684 0.428151 11.00000 0.04839 0.06024 = 0.03975 -0.00793 -0.01147 0.02584 AFIX 137 H20A 2 -0.200652 0.176057 0.397589 11.00000 -1.50000 H20B 2 -0.318815 0.123896 0.383917 11.00000 -1.50000 H20C 2 -0.239595 0.099855 0.445291 11.00000 -1.50000 AFIX 0 C21 1 -0.426102 0.390133 0.592061 11.00000 0.03114 0.06809 = 0.08266 0.04297 0.02374 0.02981 AFIX 137 H21A 2 -0.463439 0.366612 0.526141 11.00000 -1.50000 H21B 2 -0.407375 0.466855 0.628076 11.00000 -1.50000 H21C 2 -0.468591 0.354006 0.621488 11.00000 -1.50000 AFIX 0 C22 1 -0.068407 0.478764 0.756324 11.00000 0.03845 0.04138 = 0.04049 -0.00493 0.00293 0.01975 AFIX 137 H22A 2 -0.087433 0.532905 0.801759 11.00000 -1.50000 H22B 2 -0.013685 0.512873 0.735337 11.00000 -1.50000 H22C 2 -0.045698 0.439512 0.787140 11.00000 -1.50000 AFIX 0 C23 1 0.273525 0.618056 0.654150 11.00000 0.04453 0.03935 = 0.04482 0.02742 0.01713 0.01201 AFIX 23 H23A 2 0.270568 0.651946 0.611219 11.00000 -1.20000 H23B 2 0.344824 0.628789 0.678623 11.00000 -1.20000 AFIX 0 C24 1 0.232887 0.668253 0.736576 11.00000 0.05847 0.02831 = 0.04039 0.01813 0.01595 0.01384 AFIX 23 H24A 2 0.281162 0.740767 0.780528 11.00000 -1.20000 H24B 2 0.167985 0.672835 0.712511 11.00000 -1.20000 AFIX 0 C25 1 0.307318 0.775664 0.962100 11.00000 0.03022 0.02573 = 0.03122 0.00875 0.00811 0.00682 C26 1 0.395963 0.758747 0.988627 11.00000 0.03415 0.03525 = 0.04115 0.01257 0.01094 0.01148 C27 1 0.479452 0.845250 1.054624 11.00000 0.03298 0.04783 = 0.04968 0.01354 0.00484 0.01097 AFIX 43 H27A 2 0.539603 0.834519 1.072977 11.00000 -1.20000 AFIX 0 C28 1 0.478381 0.946950 1.094864 11.00000 0.03860 0.04139 = 0.04311 0.00652 0.00287 0.00195 C29 1 0.391439 0.961992 1.066427 11.00000 0.05006 0.02731 = 0.04527 0.00707 0.00663 0.00594 AFIX 43 H29A 2 0.390611 1.031654 1.093009 11.00000 -1.20000 AFIX 0 C30 1 0.304161 0.878513 0.999801 11.00000 0.03982 0.02904 = 0.03808 0.00993 0.00656 0.01072 C31 1 0.407270 0.652243 0.947642 11.00000 0.04147 0.04278 = 0.06358 0.01679 0.00988 0.02210 AFIX 137 H31A 2 0.352513 0.600014 0.953907 11.00000 -1.50000 H31B 2 0.472253 0.658184 0.982358 11.00000 -1.50000 H31C 2 0.404366 0.629552 0.880117 11.00000 -1.50000 AFIX 0 C32 1 0.570209 1.039602 1.168132 11.00000 0.05238 0.05876 = 0.06741 -0.00022 -0.00828 -0.00288 AFIX 137 H32A 2 0.581571 1.032536 1.227338 11.00000 -1.50000 H32B 2 0.559181 1.105827 1.180732 11.00000 -1.50000 H32C 2 0.629340 1.040440 1.143771 11.00000 -1.50000 AFIX 0 C33 1 0.215508 0.908992 0.975421 11.00000 0.05881 0.02929 = 0.07226 0.01081 -0.00519 0.01883 AFIX 137 H33A 2 0.234964 0.985956 1.010159 11.00000 -1.50000 H33B 2 0.158720 0.873837 0.993643 11.00000 -1.50000 H33C 2 0.195554 0.886877 0.906706 11.00000 -1.50000 AFIX 0 C34 1 0.242505 0.195331 0.934424 11.00000 0.09847 0.14876 = 0.07411 0.07225 0.02277 0.08440 AFIX 23 H34A 2 0.309738 0.215604 0.976814 11.00000 -1.20000 H34B 2 0.190722 0.173979 0.965317 11.00000 -1.20000 AFIX 0 C35 1 0.226922 0.108777 0.843885 11.00000 0.07079 0.08327 = 0.12564 0.06450 0.02725 0.05369 AFIX 23 H35A 2 0.283969 0.126589 0.817217 11.00000 -1.20000 H35B 2 0.223255 0.044585 0.852006 11.00000 -1.20000 AFIX 0 C36 1 0.097929 -0.009505 0.699191 11.00000 0.06709 0.03803 = 0.15928 0.01999 0.03779 0.03340 AFIX 23 H36A 2 0.067204 -0.066776 0.716348 11.00000 -1.20000 H36B 2 0.153242 -0.023550 0.671935 11.00000 -1.20000 AFIX 0 C37 1 0.020281 -0.008077 0.627096 11.00000 0.06397 0.03564 = 0.08814 -0.00052 0.04056 0.01605 AFIX 23 H37A 2 0.053470 0.019933 0.586857 11.00000 -1.20000 H37B 2 -0.028006 -0.081209 0.585238 11.00000 -1.20000 AFIX 0 C38 1 -0.104078 0.008248 0.711256 11.00000 0.04328 0.03374 = 0.05041 0.01720 0.01484 0.00865 AFIX 23 H38A 2 -0.071171 -0.013062 0.755618 11.00000 -1.20000 H38B 2 -0.158602 -0.055455 0.659513 11.00000 -1.20000 AFIX 0 C40 1 -0.088597 0.265689 0.891146 11.00000 0.03772 0.05288 = 0.03942 0.01311 0.01767 0.02194 AFIX 23 H40A 2 -0.150802 0.241443 0.909257 11.00000 -1.20000 H40B 2 -0.100180 0.302922 0.852755 11.00000 -1.20000 AFIX 0 C39 1 -0.145912 0.089752 0.763129 11.00000 0.03093 0.04576 = 0.04527 0.01477 0.01038 0.00923 AFIX 23 H39A 2 -0.177007 0.112574 0.719119 11.00000 -1.20000 H39B 2 -0.197862 0.060215 0.790188 11.00000 -1.20000 AFIX 0 C41 1 -0.001895 0.337899 0.978195 11.00000 0.04303 0.05741 = 0.03485 0.01107 0.02135 0.01585 AFIX 23 H41A 2 -0.012583 0.404280 1.014143 11.00000 -1.20000 H41B 2 0.004367 0.303449 1.020245 11.00000 -1.20000 AFIX 0 C42 1 0.177998 0.400811 1.025349 11.00000 0.04378 0.12682 = 0.03841 -0.01448 0.00713 -0.01023 AFIX 23 H42A 2 0.197855 0.478475 1.061522 11.00000 -1.20000 H42B 2 0.161904 0.369608 1.069263 11.00000 -1.20000 AFIX 0 C43 1 0.257849 0.380022 0.996972 11.00000 0.12703 0.16159 = 0.08906 -0.03521 -0.06316 0.09774 AFIX 23 H43A 2 0.304131 0.383404 1.051388 11.00000 -1.20000 H43B 2 0.294662 0.437044 0.981950 11.00000 -1.20000 AFIX 0 C44 1 0.926553 0.759555 0.816669 11.00000 0.05901 0.06798 = 0.04742 0.03251 0.01697 0.02856 AFIX 23 H44A 2 0.966565 0.729848 0.846852 11.00000 -1.20000 H44B 2 0.854388 0.720820 0.806778 11.00000 -1.20000 AFIX 0 CL1 7 0.958022 0.892870 0.893383 11.00000 0.09917 0.08900 = 0.05489 0.00629 0.00067 0.05128 CL2 7 0.948174 0.739327 0.706562 11.00000 0.12683 0.08593 = 0.04265 0.02704 0.02843 0.02857 S4 6 0.618468 0.710552 0.792098 11.00000 0.04731 0.04659 = 0.05258 0.01316 0.00869 0.01419 PART 1 O13 4 0.693384 0.664688 0.802074 10.50000 0.08272 O14 4 0.620599 0.795006 0.876458 10.50000 0.08272 O15 4 0.518552 0.623993 0.747099 10.50000 0.08272 C45 1 0.621002 0.732569 0.693584 10.50000 0.05992 F1 5 0.596311 0.823047 0.694913 10.50000 0.11222 F2 5 0.573390 0.639613 0.610799 10.50000 0.11222 F3 5 0.712288 0.769216 0.675370 10.50000 0.11222 PART 2 O13B 4 0.678703 0.646807 0.780024 10.50000 0.08272 O14B 4 0.674531 0.814138 0.868807 10.50000 0.08272 O15B 4 0.516936 0.670784 0.781573 10.50000 0.08272 C45B 1 0.646814 0.773975 0.712189 10.50000 0.08794 F1B 5 0.556725 0.781402 0.681973 10.50000 0.11222 F2B 5 0.639378 0.688248 0.625491 10.50000 0.11222 F3B 5 0.729223 0.840850 0.743780 10.50000 0.11222 PART 0 HKLF 4 REM asb265 in P-1 REM R1 = 0.0469 for 11177 Fo > 4sig(Fo) and 0.0516 for all 12505 data REM 672 parameters refined using 1 restraints END WGHT 0.0648 3.8497 REM Highest difference peak 1.172, deepest hole -1.399, 1-sigma level 0.075 Q1 1 0.2176 0.3407 1.0294 11.00000 0.05 0.96 Q2 1 0.7409 0.8079 0.7210 11.00000 0.05 0.83 Q3 1 0.5963 0.7021 0.7358 11.00000 0.05 0.81 Q4 1 0.5266 0.7415 0.8070 11.00000 0.05 0.76 Q5 1 0.7346 0.8820 0.7941 11.00000 0.05 0.75 Q6 1 0.7125 0.8268 0.8534 11.00000 0.05 0.75 Q7 1 0.5142 0.6451 0.7077 11.00000 0.05 0.72 Q8 1 0.6611 0.7448 0.6326 11.00000 0.05 0.69 Q9 1 0.5171 0.6229 0.6150 11.00000 0.05 0.67 Q10 1 0.6174 0.6244 0.7895 11.00000 0.05 0.60 ;