# 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_? #============================================================================== _audit_creation_method 'form.cif (version 2.0)' #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_[La(1)(Otf)3] #TrackingRef 'complexes_ChemSci.cif' _chemical_name_systematic ; ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 F9 La N9 O9 P S4, C4 H8 O' _chemical_formula_sum 'C28 H32 F9 La N9 O10 P S4' _chemical_formula_weight 1123.75 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.106(2) _cell_length_b 16.930(3) _cell_length_c 22.000(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.61(3) _cell_angle_gamma 90.00 _cell_volume 4134.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 19618 _cell_measurement_theta_min 3.86 _cell_measurement_theta_max 25.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.805 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19618 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.1233 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7235 _reflns_number_gt 4523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep32 _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^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7235 _refine_ls_number_parameters 635 _refine_ls_number_restraints 238 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.932 _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 La1 La 0.33528(3) 0.25985(2) 0.571437(16) 0.02667(13) Uani 1 1 d . . . P1 P 0.65323(15) 0.26220(10) 0.49518(8) 0.0308(4) Uani 1 1 d . A . S1 S 0.80557(16) 0.27126(11) 0.45801(9) 0.0453(5) Uani 1 1 d . . . C1 C 0.7310(6) 0.1188(4) 0.5382(3) 0.046(2) Uani 1 1 d . A . H19D H 0.7356 0.1113 0.5824 0.070 Uiso 1 1 calc R . . H19E H 0.8064 0.1421 0.5246 0.070 Uiso 1 1 calc R . . H19F H 0.7182 0.0676 0.5182 0.070 Uiso 1 1 calc R . . S2 S 0.35080(19) 0.48061(11) 0.61280(9) 0.0460(5) Uani 1 1 d . . . C200 C 0.3102(10) 0.4959(5) 0.6908(4) 0.069(3) Uani 1 1 d . A . C2 C 0.5499(7) 0.2645(5) 0.3817(3) 0.053(2) Uani 1 1 d . A . H5A H 0.4752 0.2405 0.3657 0.079 Uiso 1 1 calc R . . H5B H 0.6173 0.2283 0.3755 0.079 Uiso 1 1 calc R . . H5C H 0.5645 0.3142 0.3603 0.079 Uiso 1 1 calc R . . S3 S 0.24922(16) 0.13533(10) 0.43257(8) 0.0344(4) Uani 1 1 d . . . C300 C 0.1100(7) 0.0787(5) 0.4397(4) 0.050(2) Uani 1 1 d . A . C3 C 0.7047(6) 0.3960(4) 0.5606(3) 0.0429(19) Uani 1 1 d . A . H19A H 0.6555 0.4370 0.5792 0.064 Uiso 1 1 calc R . . H19B H 0.7310 0.4142 0.5209 0.064 Uiso 1 1 calc R . . H19C H 0.7754 0.3852 0.5870 0.064 Uiso 1 1 calc R . . N10 N 0.6304(5) 0.1717(3) 0.5223(2) 0.0313(13) Uani 1 1 d . . . C10 C 0.5021(6) 0.0830(4) 0.5644(3) 0.0301(16) Uani 1 1 d . . . H14 H 0.5676 0.0470 0.5625 0.036 Uiso 1 1 calc R A . N11 N 0.5160(4) 0.1526(3) 0.5436(2) 0.0273(12) Uani 1 1 d . A . C11 C 0.3897(6) 0.0558(4) 0.5912(3) 0.0344(17) Uani 1 1 d . A . N12 N 0.3035(5) 0.1089(3) 0.6013(2) 0.0297(13) Uani 1 1 d . A . C12 C 0.3791(6) -0.0224(4) 0.6044(3) 0.0445(19) Uani 1 1 d . . . H181 H 0.4431 -0.0579 0.5967 0.053 Uiso 1 1 calc R A . C13 C 0.2740(7) -0.0492(4) 0.6292(4) 0.055(2) Uani 1 1 d . A . H171 H 0.2649 -0.1034 0.6393 0.066 Uiso 1 1 calc R . . C14 C 0.1843(6) 0.0026(4) 0.6390(3) 0.0385(18) Uani 1 1 d . . . H141 H 0.1106 -0.0144 0.6555 0.046 Uiso 1 1 calc R A . C15 C 0.2021(6) 0.0800(4) 0.6245(3) 0.0331(16) Uani 1 1 d . A . H113 H 0.1382 0.1159 0.6314 0.040 Uiso 1 1 calc R . . O20 O 0.3460(4) 0.3958(2) 0.6076(2) 0.0427(12) Uani 1 1 d . A . N20 N 0.5389(5) 0.2802(3) 0.4471(2) 0.0345(14) Uani 1 1 d . . . C20 C 0.3661(6) 0.3490(4) 0.4302(3) 0.0349(17) Uani 1 1 d . . . H17 H 0.3964 0.3598 0.3911 0.042 Uiso 1 1 calc R A . F20 F 0.3248(6) 0.5696(3) 0.7070(3) 0.108(2) Uani 1 1 d . . . N21 N 0.4339(5) 0.3113(3) 0.4685(2) 0.0313(13) Uani 1 1 d . A . C21 C 0.2462(6) 0.3760(4) 0.4434(3) 0.0311(16) Uani 1 1 d . A . O21 O 0.4681(5) 0.5111(4) 0.6117(3) 0.094(2) Uani 1 1 d . A . F21 F 0.1979(7) 0.4784(4) 0.6991(3) 0.134(3) Uani 1 1 d . . . N22 N 0.2007(5) 0.3515(3) 0.4959(2) 0.0309(13) Uani 1 1 d . A . O22 O 0.2578(6) 0.5199(3) 0.5784(3) 0.089(2) Uani 1 1 d . A . C22 C 0.1842(6) 0.4221(4) 0.4031(3) 0.0459(19) Uani 1 1 d . . . H20 H 0.2215 0.4400 0.3673 0.055 Uiso 1 1 calc R A . F22 F 0.3744(7) 0.4505(4) 0.7278(2) 0.130(3) Uani 1 1 d . . . C23 C 0.0674(7) 0.4431(4) 0.4140(3) 0.046(2) Uani 1 1 d . A . H10 H 0.0228 0.4748 0.3857 0.055 Uiso 1 1 calc R . . C24 C 0.0166(6) 0.4176(4) 0.4662(3) 0.0427(18) Uani 1 1 d . . . H11 H -0.0649 0.4296 0.4745 0.051 Uiso 1 1 calc R A . C25 C 0.0868(6) 0.3738(4) 0.5069(3) 0.0452(19) Uani 1 1 d . A . H117 H 0.0531 0.3587 0.5444 0.054 Uiso 1 1 calc R . . O30 O 0.2476(4) 0.1833(3) 0.48606(19) 0.0400(12) Uani 1 1 d . A . N30 N 0.6338(5) 0.3242(3) 0.5531(2) 0.0324(13) Uani 1 1 d . . . C30 C 0.5892(6) 0.3187(4) 0.6542(3) 0.0346(17) Uani 1 1 d . . . H116 H 0.6494 0.3575 0.6623 0.041 Uiso 1 1 calc R A . F30 F 0.1094(4) 0.0415(3) 0.4916(2) 0.0736(14) Uani 1 1 d . . . N31 N 0.5674(5) 0.2951(3) 0.6009(3) 0.0319(13) Uani 1 1 d . A . C31 C 0.5202(6) 0.2853(4) 0.7038(3) 0.0369(17) Uani 1 1 d . A . F31 F 0.0155(4) 0.1266(3) 0.4364(2) 0.0799(16) Uani 1 1 d . . . O31 O 0.2363(5) 0.1786(3) 0.3778(2) 0.0567(15) Uani 1 1 d . A . N32 N 0.4195(5) 0.2447(3) 0.6868(2) 0.0333(12) Uani 1 1 d . A . C32 C 0.5590(7) 0.2927(5) 0.7634(3) 0.049(2) Uani 1 1 d . . . H200 H 0.6279 0.3233 0.7743 0.059 Uiso 1 1 calc R A . O32 O 0.3397(4) 0.0757(3) 0.4349(2) 0.0514(14) Uani 1 1 d . A . F32 F 0.0992(4) 0.0266(3) 0.3960(2) 0.0897(17) Uani 1 1 d . . . C33 C 0.4941(6) 0.2540(5) 0.8063(3) 0.051(2) Uani 1 1 d . A . H111 H 0.5208 0.2561 0.8476 0.061 Uiso 1 1 calc R . . C34 C 0.3937(7) 0.2130(4) 0.7916(3) 0.049(2) Uani 1 1 d . . . H100 H 0.3480 0.1875 0.8217 0.059 Uiso 1 1 calc R A . C35 C 0.3603(6) 0.2097(4) 0.7315(3) 0.0400(18) Uani 1 1 d . A . H13 H 0.2900 0.1803 0.7206 0.048 Uiso 1 1 calc R . . S4 S 0.0181(4) 0.2693(3) 0.6444(2) 0.0432(17) Uani 0.415(6) 1 d PDU A 1 O40 O 0.1377(14) 0.256(3) 0.6251(17) 0.026(5) Uani 0.415(6) 1 d PDU A 1 O41 O -0.0519(15) 0.2028(11) 0.6255(11) 0.077(6) Uani 0.415(6) 1 d PDU A 1 O42 O -0.028(2) 0.3474(8) 0.6363(13) 0.071(7) Uani 0.415(6) 1 d PDU A 1 C40 C 0.0263(12) 0.2597(8) 0.7267(4) 0.047(3) Uani 0.415(6) 1 d PDU A 1 F40 F 0.0640(15) 0.1884(8) 0.7409(6) 0.074(4) Uani 0.415(6) 1 d PDU A 1 F41 F 0.0951(14) 0.3137(14) 0.7525(7) 0.066(5) Uani 0.415(6) 1 d PDU A 1 F42 F -0.0822(12) 0.2737(13) 0.7475(7) 0.067(5) Uani 0.415(6) 1 d PDU A 1 S4' S 0.0750(3) 0.3050(2) 0.67614(16) 0.0387(12) Uani 0.585(6) 1 d PDU A 2 O40' O 0.1549(12) 0.2684(19) 0.6349(12) 0.027(4) Uani 0.585(6) 1 d PDU A 2 O41' O 0.1306(10) 0.3120(11) 0.7345(4) 0.051(3) Uani 0.585(6) 1 d PDU A 2 O42' O 0.0142(15) 0.3724(6) 0.6514(9) 0.060(4) Uani 0.585(6) 1 d PDU A 2 C40' C -0.0453(9) 0.2338(6) 0.6859(6) 0.059(3) Uani 0.585(6) 1 d PDU A 2 F40' F -0.0036(10) 0.1681(6) 0.7096(6) 0.099(4) Uani 0.585(6) 1 d PDU A 2 F41' F -0.1001(10) 0.2211(9) 0.6332(7) 0.105(5) Uani 0.585(6) 1 d PDU A 2 F42' F -0.1272(9) 0.2595(10) 0.7230(7) 0.091(5) Uani 0.585(6) 1 d PDU A 2 O99 O 0.7447(8) 0.4682(4) 0.7241(3) 0.092(2) Uani 1 1 d . . . C999 C 0.6815(11) 0.5309(9) 0.7501(5) 0.109(4) Uani 1 1 d . . . H99A H 0.6373 0.5122 0.7858 0.131 Uiso 1 1 calc R . . H99B H 0.6227 0.5533 0.7201 0.131 Uiso 1 1 calc R . . C998 C 0.7700(16) 0.5905(8) 0.7684(5) 0.130(5) Uani 1 1 d . . . H99C H 0.7507 0.6133 0.8084 0.156 Uiso 1 1 calc R . . H99D H 0.7724 0.6336 0.7381 0.156 Uiso 1 1 calc R . . C997 C 0.8855(13) 0.5482(9) 0.7719(6) 0.132(5) Uani 1 1 d . . . H99E H 0.9423 0.5700 0.7423 0.158 Uiso 1 1 calc R . . H99F H 0.9225 0.5520 0.8132 0.158 Uiso 1 1 calc R . . C996 C 0.8550(11) 0.4668(6) 0.7571(5) 0.087(3) Uani 1 1 d . . . H99G H 0.9185 0.4428 0.7324 0.104 Uiso 1 1 calc R . . H99H H 0.8472 0.4354 0.7947 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0253(2) 0.0292(2) 0.0257(2) 0.0006(2) 0.00207(15) 0.0015(2) P1 0.0265(9) 0.0315(10) 0.0349(9) 0.0007(9) 0.0085(8) 0.0004(8) S1 0.0329(10) 0.0486(12) 0.0554(12) 0.0002(10) 0.0184(9) -0.0008(9) C1 0.025(4) 0.045(4) 0.070(5) 0.024(4) 0.009(4) 0.013(4) S2 0.0562(14) 0.0311(10) 0.0509(13) -0.0035(9) 0.0047(11) 0.0032(10) C200 0.094(8) 0.051(6) 0.062(6) -0.021(5) 0.016(6) 0.023(6) C2 0.057(5) 0.061(5) 0.040(4) 0.001(4) 0.001(4) 0.011(4) S3 0.0332(11) 0.0369(10) 0.0327(10) -0.0048(8) -0.0062(8) 0.0042(9) C300 0.029(4) 0.061(5) 0.058(5) -0.030(5) -0.009(4) 0.003(4) C3 0.032(4) 0.035(4) 0.062(5) -0.007(4) 0.011(4) -0.015(3) N10 0.022(3) 0.031(3) 0.041(3) -0.002(3) 0.003(3) -0.001(3) C10 0.025(4) 0.029(4) 0.036(4) 0.000(3) -0.001(3) 0.011(3) N11 0.021(3) 0.026(3) 0.034(3) -0.001(3) -0.003(3) 0.001(2) C11 0.035(4) 0.036(4) 0.032(4) 0.000(3) -0.006(3) 0.002(3) N12 0.031(3) 0.033(3) 0.025(3) 0.002(3) 0.002(3) -0.001(3) C12 0.033(4) 0.035(4) 0.066(5) 0.009(4) 0.016(4) 0.001(3) C13 0.048(5) 0.033(4) 0.083(6) 0.004(4) 0.020(5) -0.005(4) C14 0.031(4) 0.046(5) 0.039(4) 0.003(4) 0.012(3) -0.014(4) C15 0.026(4) 0.039(4) 0.034(4) -0.001(3) -0.002(3) -0.003(3) O20 0.054(3) 0.027(3) 0.046(3) -0.004(2) -0.003(3) 0.009(2) N20 0.028(3) 0.044(4) 0.031(3) 0.007(3) 0.006(3) 0.010(3) C20 0.033(4) 0.040(4) 0.032(4) 0.008(3) 0.010(3) 0.002(3) F20 0.152(6) 0.064(4) 0.108(4) -0.048(3) 0.019(4) 0.019(4) N21 0.026(3) 0.037(3) 0.031(3) 0.002(3) 0.002(3) 0.005(3) C21 0.028(4) 0.036(4) 0.029(4) 0.005(3) 0.000(3) -0.003(3) O21 0.068(4) 0.079(5) 0.136(6) -0.040(4) 0.037(4) -0.033(4) F21 0.124(6) 0.155(6) 0.129(6) -0.023(5) 0.084(5) 0.001(5) N22 0.029(3) 0.032(3) 0.031(3) -0.001(3) 0.001(3) 0.003(3) O22 0.119(5) 0.060(4) 0.085(4) 0.019(3) -0.026(4) 0.049(4) C22 0.042(5) 0.051(5) 0.044(5) 0.009(4) 0.007(4) 0.007(4) F22 0.230(8) 0.115(5) 0.044(3) -0.010(3) -0.003(4) 0.080(5) C23 0.037(5) 0.052(5) 0.048(5) 0.006(4) -0.017(4) 0.012(4) C24 0.029(4) 0.041(4) 0.058(5) -0.001(4) -0.001(4) 0.001(4) C25 0.041(5) 0.050(5) 0.045(5) 0.003(4) 0.010(4) 0.009(4) O30 0.048(3) 0.041(3) 0.031(3) -0.011(2) -0.007(2) 0.001(2) N30 0.021(3) 0.039(3) 0.037(3) -0.002(3) 0.006(3) -0.005(3) C30 0.029(4) 0.034(4) 0.040(4) 0.001(3) -0.005(3) -0.010(3) F30 0.063(3) 0.068(3) 0.089(4) 0.016(3) 0.005(3) -0.021(3) N31 0.027(3) 0.030(3) 0.039(3) -0.002(3) 0.000(3) -0.003(3) C31 0.032(4) 0.041(4) 0.037(4) -0.002(3) -0.003(3) 0.002(3) F31 0.031(3) 0.085(4) 0.123(4) -0.005(3) -0.003(3) 0.016(3) O31 0.060(4) 0.076(4) 0.034(3) 0.008(3) -0.008(3) 0.007(3) N32 0.030(3) 0.039(3) 0.031(3) -0.001(3) 0.005(2) 0.000(3) C32 0.048(5) 0.063(5) 0.035(4) -0.009(4) -0.010(4) -0.014(4) O32 0.030(3) 0.043(3) 0.081(4) -0.009(3) 0.003(3) 0.008(2) F32 0.056(3) 0.102(4) 0.110(4) -0.054(4) -0.016(3) -0.018(3) C33 0.044(4) 0.071(6) 0.037(4) 0.006(4) -0.002(4) -0.014(5) C34 0.048(5) 0.063(5) 0.036(4) 0.004(4) 0.001(4) -0.018(4) C35 0.039(4) 0.043(4) 0.038(4) -0.001(4) -0.004(4) 0.003(4) S4 0.029(3) 0.064(3) 0.037(3) 0.002(3) 0.009(2) 0.006(3) O40 0.022(6) 0.037(15) 0.019(9) -0.009(7) -0.003(7) 0.000(8) O41 0.028(11) 0.121(12) 0.083(11) -0.022(11) -0.013(10) -0.019(10) O42 0.062(16) 0.094(9) 0.057(14) 0.041(12) 0.017(10) 0.045(11) C40 0.046(9) 0.054(9) 0.040(6) 0.010(7) 0.009(7) 0.009(8) F40 0.102(13) 0.066(7) 0.055(8) 0.026(6) 0.029(8) 0.024(7) F41 0.061(9) 0.096(9) 0.042(8) -0.023(8) 0.021(7) -0.009(9) F42 0.054(8) 0.085(13) 0.065(9) 0.003(8) 0.041(8) 0.003(8) S4' 0.032(2) 0.048(2) 0.036(2) 0.0034(17) 0.0066(17) 0.0024(16) O40' 0.026(5) 0.026(8) 0.029(9) -0.009(5) 0.003(6) -0.011(5) O41' 0.041(7) 0.077(7) 0.036(6) -0.014(6) 0.019(5) 0.018(6) O42' 0.061(11) 0.048(6) 0.072(11) 0.022(6) 0.025(7) 0.018(6) C40' 0.045(7) 0.066(8) 0.068(8) 0.014(7) 0.022(5) -0.003(6) F40' 0.087(9) 0.053(6) 0.159(12) 0.034(7) 0.055(7) 0.009(5) F41' 0.047(8) 0.156(11) 0.111(8) -0.027(7) -0.007(7) -0.035(8) F42' 0.053(7) 0.075(7) 0.149(12) -0.019(9) 0.060(7) -0.016(6) O99 0.100(6) 0.088(5) 0.089(5) -0.008(4) -0.002(5) -0.035(5) C999 0.116(11) 0.152(13) 0.060(7) -0.005(8) 0.013(7) 0.040(10) C998 0.209(17) 0.106(10) 0.074(8) -0.047(8) -0.003(10) 0.003(12) C997 0.130(12) 0.135(13) 0.127(11) -0.022(10) -0.052(9) -0.012(11) C996 0.111(10) 0.083(8) 0.067(7) 0.003(6) 0.007(7) 0.002(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 La1 O20 2.437(4) . ? La1 O30 2.461(4) . ? La1 O40' 2.477(12) . ? La1 O40 2.521(17) . ? La1 N12 2.664(5) . ? La1 N21 2.688(5) . ? La1 N32 2.693(5) . ? La1 N22 2.695(5) . ? La1 N31 2.707(5) . ? La1 N11 2.787(5) . ? P1 N20 1.658(5) . ? P1 N10 1.667(5) . ? P1 N30 1.669(5) . ? P1 S1 1.906(2) . ? C1 N10 1.466(7) . ? C1 H19D 0.9800 . ? C1 H19E 0.9800 . ? C1 H19F 0.9800 . ? S2 O21 1.402(6) . ? S2 O22 1.429(5) . ? S2 O20 1.441(5) . ? S2 C200 1.805(9) . ? C200 F21 1.301(11) . ? C200 F20 1.307(9) . ? C200 F22 1.314(10) . ? C2 N20 1.472(8) . ? C2 H5A 0.9800 . ? C2 H5B 0.9800 . ? C2 H5C 0.9800 . ? S3 O31 1.414(5) . ? S3 O32 1.424(5) . ? S3 O30 1.430(4) . ? S3 C300 1.829(8) . ? C300 F30 1.305(9) . ? C300 F32 1.307(8) . ? C300 F31 1.326(8) . ? C3 N30 1.456(7) . ? C3 H19A 0.9800 . ? C3 H19B 0.9800 . ? C3 H19C 0.9800 . ? N10 N11 1.405(7) . ? C10 N11 1.275(7) . ? C10 C11 1.469(8) . ? C10 H14 0.9500 . ? C11 N12 1.337(8) . ? C11 C12 1.361(9) . ? N12 C15 1.342(7) . ? C12 C13 1.379(9) . ? C12 H181 0.9500 . ? C13 C14 1.349(9) . ? C13 H171 0.9500 . ? C14 C15 1.364(9) . ? C14 H141 0.9500 . ? C15 H113 0.9500 . ? N20 N21 1.375(6) . ? C20 N21 1.285(7) . ? C20 C21 1.445(9) . ? C20 H17 0.9500 . ? C21 N22 1.339(7) . ? C21 C22 1.354(9) . ? N22 C25 1.349(8) . ? C22 C23 1.372(9) . ? C22 H20 0.9500 . ? C23 C24 1.364(9) . ? C23 H10 0.9500 . ? C24 C25 1.387(9) . ? C24 H11 0.9500 . ? C25 H117 0.9500 . ? N30 N31 1.392(7) . ? C30 N31 1.258(7) . ? C30 C31 1.463(9) . ? C30 H116 0.9500 . ? C31 N32 1.356(8) . ? C31 C32 1.374(9) . ? N32 C35 1.336(8) . ? C32 C33 1.370(9) . ? C32 H200 0.9500 . ? C33 C34 1.345(9) . ? C33 H111 0.9500 . ? C34 C35 1.364(9) . ? C34 H100 0.9500 . ? C35 H13 0.9500 . ? S4 O41 1.423(10) . ? S4 O40 1.424(9) . ? S4 O42 1.427(9) . ? S4 C40 1.819(9) . ? C40 F41 1.309(10) . ? C40 F40 1.312(9) . ? C40 F42 1.323(9) . ? S4' O41' 1.413(9) . ? S4' O42' 1.427(8) . ? S4' O40' 1.429(9) . ? S4' C40' 1.817(8) . ? C40' F40' 1.308(9) . ? C40' F41' 1.312(9) . ? C40' F42' 1.313(9) . ? O99 C999 1.403(12) . ? O99 C996 1.406(11) . ? C999 C998 1.457(15) . ? C999 H99A 0.9900 . ? C999 H99B 0.9900 . ? C998 C997 1.469(15) . ? C998 H99C 0.9900 . ? C998 H99D 0.9900 . ? C997 C996 1.454(14) . ? C997 H99E 0.9900 . ? C997 H99F 0.9900 . ? C996 H99G 0.9900 . ? C996 H99H 0.9900 . ? 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 O20 La1 O30 139.60(15) . . ? O20 La1 O40' 78.1(6) . . ? O30 La1 O40' 98.7(4) . . ? O20 La1 O40 84.8(8) . . ? O30 La1 O40 90.6(6) . . ? O40' La1 O40 8.1(9) . . ? O20 La1 N12 146.19(15) . . ? O30 La1 N12 68.30(15) . . ? O40' La1 N12 78.6(8) . . ? O40 La1 N12 74.6(11) . . ? O20 La1 N21 87.23(16) . . ? O30 La1 N21 71.93(15) . . ? O40' La1 N21 144.2(9) . . ? O40 La1 N21 141.6(11) . . ? N12 La1 N21 125.34(16) . . ? O20 La1 N32 76.68(16) . . ? O30 La1 N32 142.09(16) . . ? O40' La1 N32 74.9(7) . . ? O40 La1 N32 80.8(9) . . ? N12 La1 N32 73.82(16) . . ? N21 La1 N32 133.32(16) . . ? O20 La1 N22 71.28(15) . . ? O30 La1 N22 68.39(15) . . ? O40' La1 N22 82.6(9) . . ? O40 La1 N22 80.2(12) . . ? N12 La1 N22 128.97(16) . . ? N21 La1 N22 61.70(16) . . ? N32 La1 N22 143.91(15) . . ? O20 La1 N31 71.13(15) . . ? O30 La1 N31 130.73(16) . . ? O40' La1 N31 129.2(5) . . ? O40 La1 N31 136.9(7) . . ? N12 La1 N31 106.52(16) . . ? N21 La1 N31 73.86(16) . . ? N32 La1 N31 59.50(16) . . ? N22 La1 N31 121.91(16) . . ? O20 La1 N11 131.17(15) . . ? O30 La1 N11 76.18(14) . . ? O40' La1 N11 139.5(9) . . ? O40 La1 N11 136.5(11) . . ? N12 La1 N11 61.98(15) . . ? N21 La1 N11 73.35(16) . . ? N32 La1 N11 84.94(15) . . ? N22 La1 N11 129.04(15) . . ? N31 La1 N11 60.61(15) . . ? N20 P1 N10 106.0(3) . . ? N20 P1 N30 105.0(3) . . ? N10 P1 N30 106.3(3) . . ? N20 P1 S1 112.6(2) . . ? N10 P1 S1 111.9(2) . . ? N30 P1 S1 114.3(2) . . ? N10 C1 H19D 109.5 . . ? N10 C1 H19E 109.5 . . ? H19D C1 H19E 109.5 . . ? N10 C1 H19F 109.5 . . ? H19D C1 H19F 109.5 . . ? H19E C1 H19F 109.5 . . ? O21 S2 O22 118.5(4) . . ? O21 S2 O20 113.5(4) . . ? O22 S2 O20 113.4(3) . . ? O21 S2 C200 102.7(5) . . ? O22 S2 C200 103.9(4) . . ? O20 S2 C200 102.0(4) . . ? F21 C200 F20 106.9(8) . . ? F21 C200 F22 106.5(9) . . ? F20 C200 F22 109.2(9) . . ? F21 C200 S2 111.5(7) . . ? F20 C200 S2 111.4(7) . . ? F22 C200 S2 111.0(6) . . ? N20 C2 H5A 109.5 . . ? N20 C2 H5B 109.5 . . ? H5A C2 H5B 109.5 . . ? N20 C2 H5C 109.5 . . ? H5A C2 H5C 109.5 . . ? H5B C2 H5C 109.5 . . ? O31 S3 O32 116.9(3) . . ? O31 S3 O30 113.9(3) . . ? O32 S3 O30 113.5(3) . . ? O31 S3 C300 106.2(4) . . ? O32 S3 C300 102.9(3) . . ? O30 S3 C300 101.3(3) . . ? F30 C300 F32 108.3(7) . . ? F30 C300 F31 108.6(7) . . ? F32 C300 F31 108.4(6) . . ? F30 C300 S3 110.7(5) . . ? F32 C300 S3 110.5(6) . . ? F31 C300 S3 110.2(6) . . ? N30 C3 H19A 109.5 . . ? N30 C3 H19B 109.5 . . ? H19A C3 H19B 109.5 . . ? N30 C3 H19C 109.5 . . ? H19A C3 H19C 109.5 . . ? H19B C3 H19C 109.5 . . ? N11 N10 C1 118.1(5) . . ? N11 N10 P1 118.6(4) . . ? C1 N10 P1 121.6(4) . . ? N11 C10 C11 123.1(6) . . ? N11 C10 H14 118.5 . . ? C11 C10 H14 118.5 . . ? C10 N11 N10 116.9(5) . . ? C10 N11 La1 115.4(4) . . ? N10 N11 La1 125.9(3) . . ? N12 C11 C12 123.5(7) . . ? N12 C11 C10 118.5(6) . . ? C12 C11 C10 118.0(6) . . ? C11 N12 C15 115.5(6) . . ? C11 N12 La1 120.3(4) . . ? C15 N12 La1 124.2(4) . . ? C11 C12 C13 119.0(7) . . ? C11 C12 H181 120.5 . . ? C13 C12 H181 120.5 . . ? C14 C13 C12 119.0(7) . . ? C14 C13 H171 120.5 . . ? C12 C13 H171 120.5 . . ? C13 C14 C15 118.4(6) . . ? C13 C14 H141 120.8 . . ? C15 C14 H141 120.8 . . ? N12 C15 C14 124.6(6) . . ? N12 C15 H113 117.7 . . ? C14 C15 H113 117.7 . . ? S2 O20 La1 165.5(3) . . ? N21 N20 C2 119.9(5) . . ? N21 N20 P1 119.6(4) . . ? C2 N20 P1 120.5(4) . . ? N21 C20 C21 123.5(6) . . ? N21 C20 H17 118.2 . . ? C21 C20 H17 118.2 . . ? C20 N21 N20 116.9(5) . . ? C20 N21 La1 117.9(4) . . ? N20 N21 La1 122.3(4) . . ? N22 C21 C22 123.1(6) . . ? N22 C21 C20 116.5(6) . . ? C22 C21 C20 120.4(6) . . ? C21 N22 C25 116.5(6) . . ? C21 N22 La1 119.6(4) . . ? C25 N22 La1 123.8(4) . . ? C21 C22 C23 120.1(7) . . ? C21 C22 H20 120.0 . . ? C23 C22 H20 120.0 . . ? C24 C23 C22 118.7(7) . . ? C24 C23 H10 120.7 . . ? C22 C23 H10 120.7 . . ? C23 C24 C25 118.4(7) . . ? C23 C24 H11 120.8 . . ? C25 C24 H11 120.8 . . ? N22 C25 C24 123.1(7) . . ? N22 C25 H117 118.4 . . ? C24 C25 H117 118.4 . . ? S3 O30 La1 156.0(3) . . ? N31 N30 C3 120.4(5) . . ? N31 N30 P1 115.9(4) . . ? C3 N30 P1 122.1(4) . . ? N31 C30 C31 118.8(6) . . ? N31 C30 H116 120.6 . . ? C31 C30 H116 120.6 . . ? C30 N31 N30 120.1(5) . . ? C30 N31 La1 116.8(4) . . ? N30 N31 La1 114.8(4) . . ? N32 C31 C32 122.8(6) . . ? N32 C31 C30 115.9(6) . . ? C32 C31 C30 121.2(6) . . ? C35 N32 C31 116.3(5) . . ? C35 N32 La1 124.8(4) . . ? C31 N32 La1 118.2(4) . . ? C33 C32 C31 117.2(7) . . ? C33 C32 H200 121.4 . . ? C31 C32 H200 121.4 . . ? C34 C33 C32 122.0(7) . . ? C34 C33 H111 119.0 . . ? C32 C33 H111 119.0 . . ? C33 C34 C35 117.1(7) . . ? C33 C34 H100 121.4 . . ? C35 C34 H100 121.4 . . ? N32 C35 C34 124.6(7) . . ? N32 C35 H13 117.7 . . ? C34 C35 H13 117.7 . . ? O41 S4 O40 106.9(16) . . ? O41 S4 O42 120.4(13) . . ? O40 S4 O42 117(2) . . ? O41 S4 C40 103.4(12) . . ? O40 S4 C40 105.2(18) . . ? O42 S4 C40 102.4(12) . . ? S4 O40 La1 165(3) . . ? F41 C40 F40 111.2(16) . . ? F41 C40 F42 104.6(14) . . ? F40 C40 F42 111.7(15) . . ? F41 C40 S4 112.4(11) . . ? F40 C40 S4 109.0(9) . . ? F42 C40 S4 107.9(10) . . ? O41' S4' O42' 118.0(11) . . ? O41' S4' O40' 110.5(12) . . ? O42' S4' O40' 113.6(18) . . ? O41' S4' C40' 104.6(8) . . ? O42' S4' C40' 103.5(8) . . ? O40' S4' C40' 105.0(11) . . ? S4' O40' La1 155.4(16) . . ? F40' C40' F41' 111.3(13) . . ? F40' C40' F42' 106.1(12) . . ? F41' C40' F42' 106.9(12) . . ? F40' C40' S4' 111.0(8) . . ? F41' C40' S4' 109.2(9) . . ? F42' C40' S4' 112.2(9) . . ? C999 O99 C996 103.9(8) . . ? O99 C999 C998 107.1(10) . . ? O99 C999 H99A 110.3 . . ? C998 C999 H99A 110.3 . . ? O99 C999 H99B 110.3 . . ? C998 C999 H99B 110.3 . . ? H99A C999 H99B 108.5 . . ? C999 C998 C997 105.0(11) . . ? C999 C998 H99C 110.8 . . ? C997 C998 H99C 110.8 . . ? C999 C998 H99D 110.8 . . ? C997 C998 H99D 110.8 . . ? H99C C998 H99D 108.8 . . ? C996 C997 C998 104.7(11) . . ? C996 C997 H99E 110.8 . . ? C998 C997 H99E 110.8 . . ? C996 C997 H99F 110.8 . . ? C998 C997 H99F 110.8 . . ? H99E C997 H99F 108.9 . . ? O99 C996 C997 107.0(9) . . ? O99 C996 H99G 110.3 . . ? C997 C996 H99G 110.3 . . ? O99 C996 H99H 110.3 . . ? C997 C996 H99H 110.3 . . ? H99G C996 H99H 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O21 S2 C200 F21 173.3(7) . . . . ? O22 S2 C200 F21 49.2(8) . . . . ? O20 S2 C200 F21 -69.0(7) . . . . ? O21 S2 C200 F20 53.9(9) . . . . ? O22 S2 C200 F20 -70.2(9) . . . . ? O20 S2 C200 F20 171.7(7) . . . . ? O21 S2 C200 F22 -68.0(8) . . . . ? O22 S2 C200 F22 167.9(7) . . . . ? O20 S2 C200 F22 49.7(8) . . . . ? O31 S3 C300 F30 -174.9(5) . . . . ? O32 S3 C300 F30 61.8(6) . . . . ? O30 S3 C300 F30 -55.8(6) . . . . ? O31 S3 C300 F32 65.0(7) . . . . ? O32 S3 C300 F32 -58.3(7) . . . . ? O30 S3 C300 F32 -175.8(6) . . . . ? O31 S3 C300 F31 -54.8(6) . . . . ? O32 S3 C300 F31 -178.1(5) . . . . ? O30 S3 C300 F31 64.4(6) . . . . ? N20 P1 N10 N11 -48.3(5) . . . . ? N30 P1 N10 N11 63.0(5) . . . . ? S1 P1 N10 N11 -171.5(4) . . . . ? N20 P1 N10 C1 146.7(5) . . . . ? N30 P1 N10 C1 -101.9(5) . . . . ? S1 P1 N10 C1 23.6(6) . . . . ? C11 C10 N11 N10 176.7(5) . . . . ? C11 C10 N11 La1 11.1(8) . . . . ? C1 N10 N11 C10 -14.1(8) . . . . ? P1 N10 N11 C10 -179.5(4) . . . . ? C1 N10 N11 La1 149.9(5) . . . . ? P1 N10 N11 La1 -15.6(6) . . . . ? O20 La1 N11 C10 134.7(4) . . . . ? O30 La1 N11 C10 -79.5(4) . . . . ? O40' La1 N11 C10 7.8(9) . . . . ? O40 La1 N11 C10 -3.5(12) . . . . ? N12 La1 N11 C10 -7.0(4) . . . . ? N21 La1 N11 C10 -154.4(5) . . . . ? N32 La1 N11 C10 67.4(4) . . . . ? N22 La1 N11 C10 -126.0(4) . . . . ? N31 La1 N11 C10 125.0(5) . . . . ? O20 La1 N11 N10 -29.4(5) . . . . ? O30 La1 N11 N10 116.4(4) . . . . ? O40' La1 N11 N10 -156.4(8) . . . . ? O40 La1 N11 N10 -167.7(11) . . . . ? N12 La1 N11 N10 -171.1(5) . . . . ? N21 La1 N11 N10 41.4(4) . . . . ? N32 La1 N11 N10 -96.8(4) . . . . ? N22 La1 N11 N10 69.8(5) . . . . ? N31 La1 N11 N10 -39.1(4) . . . . ? N11 C10 C11 N12 -8.8(9) . . . . ? N11 C10 C11 C12 171.3(6) . . . . ? C12 C11 N12 C15 -1.5(10) . . . . ? C10 C11 N12 C15 178.6(5) . . . . ? C12 C11 N12 La1 -179.0(5) . . . . ? C10 C11 N12 La1 1.1(7) . . . . ? O20 La1 N12 C11 -120.3(5) . . . . ? O30 La1 N12 C11 88.2(5) . . . . ? O40' La1 N12 C11 -167.5(7) . . . . ? O40 La1 N12 C11 -174.8(9) . . . . ? N21 La1 N12 C11 41.9(5) . . . . ? N32 La1 N12 C11 -90.1(5) . . . . ? N22 La1 N12 C11 121.9(4) . . . . ? N31 La1 N12 C11 -39.7(5) . . . . ? N11 La1 N12 C11 2.8(4) . . . . ? O20 La1 N12 C15 62.4(6) . . . . ? O30 La1 N12 C15 -89.1(5) . . . . ? O40' La1 N12 C15 15.2(7) . . . . ? O40 La1 N12 C15 7.9(9) . . . . ? N21 La1 N12 C15 -135.4(4) . . . . ? N32 La1 N12 C15 92.6(5) . . . . ? N22 La1 N12 C15 -55.4(5) . . . . ? N31 La1 N12 C15 143.0(5) . . . . ? N11 La1 N12 C15 -174.6(5) . . . . ? N12 C11 C12 C13 0.5(11) . . . . ? C10 C11 C12 C13 -179.6(6) . . . . ? C11 C12 C13 C14 0.7(11) . . . . ? C12 C13 C14 C15 -0.8(11) . . . . ? C11 N12 C15 C14 1.4(9) . . . . ? La1 N12 C15 C14 178.9(5) . . . . ? C13 C14 C15 N12 -0.3(11) . . . . ? O21 S2 O20 La1 -88.5(13) . . . . ? O22 S2 O20 La1 50.6(13) . . . . ? C200 S2 O20 La1 161.8(12) . . . . ? O30 La1 O20 S2 -31.3(13) . . . . ? O40' La1 O20 S2 -120.8(15) . . . . ? O40 La1 O20 S2 -116.2(16) . . . . ? N12 La1 O20 S2 -168.2(11) . . . . ? N21 La1 O20 S2 26.3(12) . . . . ? N32 La1 O20 S2 162.1(13) . . . . ? N22 La1 O20 S2 -34.7(12) . . . . ? N31 La1 O20 S2 100.2(12) . . . . ? N11 La1 O20 S2 91.2(12) . . . . ? N10 P1 N20 N21 86.8(5) . . . . ? N30 P1 N20 N21 -25.5(5) . . . . ? S1 P1 N20 N21 -150.4(4) . . . . ? N10 P1 N20 C2 -94.2(5) . . . . ? N30 P1 N20 C2 153.4(5) . . . . ? S1 P1 N20 C2 28.5(6) . . . . ? C21 C20 N21 N20 171.5(6) . . . . ? C21 C20 N21 La1 10.1(8) . . . . ? C2 N20 N21 C20 -22.4(8) . . . . ? P1 N20 N21 C20 156.5(5) . . . . ? C2 N20 N21 La1 138.1(5) . . . . ? P1 N20 N21 La1 -43.0(6) . . . . ? O20 La1 N21 C20 -76.2(5) . . . . ? O30 La1 N21 C20 68.7(5) . . . . ? O40' La1 N21 C20 -11.0(9) . . . . ? O40 La1 N21 C20 1.8(13) . . . . ? N12 La1 N21 C20 113.6(5) . . . . ? N32 La1 N21 C20 -144.9(4) . . . . ? N22 La1 N21 C20 -6.0(4) . . . . ? N31 La1 N21 C20 -147.4(5) . . . . ? N11 La1 N21 C20 149.2(5) . . . . ? O20 La1 N21 N20 123.4(4) . . . . ? O30 La1 N21 N20 -91.7(4) . . . . ? O40' La1 N21 N20 -171.4(8) . . . . ? O40 La1 N21 N20 -158.6(12) . . . . ? N12 La1 N21 N20 -46.8(5) . . . . ? N32 La1 N21 N20 54.7(5) . . . . ? N22 La1 N21 N20 -166.4(5) . . . . ? N31 La1 N21 N20 52.3(4) . . . . ? N11 La1 N21 N20 -11.2(4) . . . . ? N21 C20 C21 N22 -8.0(10) . . . . ? N21 C20 C21 C22 173.5(7) . . . . ? C22 C21 N22 C25 1.3(10) . . . . ? C20 C21 N22 C25 -177.2(6) . . . . ? C22 C21 N22 La1 -180.0(5) . . . . ? C20 C21 N22 La1 1.5(7) . . . . ? O20 La1 N22 C21 99.2(5) . . . . ? O30 La1 N22 C21 -78.4(5) . . . . ? O40' La1 N22 C21 179.1(7) . . . . ? O40 La1 N22 C21 -173.1(8) . . . . ? N12 La1 N22 C21 -112.1(5) . . . . ? N21 La1 N22 C21 2.0(4) . . . . ? N32 La1 N22 C21 127.8(4) . . . . ? N31 La1 N22 C21 47.0(5) . . . . ? N11 La1 N22 C21 -29.1(5) . . . . ? O20 La1 N22 C25 -82.2(5) . . . . ? O30 La1 N22 C25 100.2(5) . . . . ? O40' La1 N22 C25 -2.3(7) . . . . ? O40 La1 N22 C25 5.6(8) . . . . ? N12 La1 N22 C25 66.5(5) . . . . ? N21 La1 N22 C25 -179.3(6) . . . . ? N32 La1 N22 C25 -53.6(6) . . . . ? N31 La1 N22 C25 -134.3(5) . . . . ? N11 La1 N22 C25 149.5(5) . . . . ? N22 C21 C22 C23 -2.8(11) . . . . ? C20 C21 C22 C23 175.6(7) . . . . ? C21 C22 C23 C24 1.0(11) . . . . ? C22 C23 C24 C25 2.2(11) . . . . ? C21 N22 C25 C24 2.1(10) . . . . ? La1 N22 C25 C24 -176.6(5) . . . . ? C23 C24 C25 N22 -3.8(11) . . . . ? O31 S3 O30 La1 -95.7(7) . . . . ? O32 S3 O30 La1 41.2(8) . . . . ? C300 S3 O30 La1 150.8(7) . . . . ? O20 La1 O30 S3 114.0(7) . . . . ? O40' La1 O30 S3 -164.1(11) . . . . ? O40 La1 O30 S3 -163.3(14) . . . . ? N12 La1 O30 S3 -90.2(7) . . . . ? N21 La1 O30 S3 51.5(7) . . . . ? N32 La1 O30 S3 -87.5(7) . . . . ? N22 La1 O30 S3 117.5(7) . . . . ? N31 La1 O30 S3 3.3(8) . . . . ? N11 La1 O30 S3 -25.2(7) . . . . ? N20 P1 N30 N31 91.5(5) . . . . ? N10 P1 N30 N31 -20.6(5) . . . . ? S1 P1 N30 N31 -144.6(4) . . . . ? N20 P1 N30 C3 -103.0(5) . . . . ? N10 P1 N30 C3 144.9(5) . . . . ? S1 P1 N30 C3 20.9(6) . . . . ? C31 C30 N31 N30 -178.3(5) . . . . ? C31 C30 N31 La1 35.2(7) . . . . ? C3 N30 N31 C30 -16.7(9) . . . . ? P1 N30 N31 C30 149.1(5) . . . . ? C3 N30 N31 La1 130.4(5) . . . . ? P1 N30 N31 La1 -63.8(5) . . . . ? O20 La1 N31 C30 56.5(5) . . . . ? O30 La1 N31 C30 -163.3(4) . . . . ? O40' La1 N31 C30 0.6(12) . . . . ? O40 La1 N31 C30 -3.1(18) . . . . ? N12 La1 N31 C30 -88.0(5) . . . . ? N21 La1 N31 C30 149.2(5) . . . . ? N32 La1 N31 C30 -28.8(5) . . . . ? N22 La1 N31 C30 108.8(5) . . . . ? N11 La1 N31 C30 -131.2(5) . . . . ? O20 La1 N31 N30 -91.7(4) . . . . ? O30 La1 N31 N30 48.5(4) . . . . ? O40' La1 N31 N30 -147.6(11) . . . . ? O40 La1 N31 N30 -151.3(17) . . . . ? N12 La1 N31 N30 123.8(4) . . . . ? N21 La1 N31 N30 0.9(4) . . . . ? N32 La1 N31 N30 -177.0(4) . . . . ? N22 La1 N31 N30 -39.5(4) . . . . ? N11 La1 N31 N30 80.6(4) . . . . ? N31 C30 C31 N32 -14.5(9) . . . . ? N31 C30 C31 C32 163.1(7) . . . . ? C32 C31 N32 C35 -1.9(10) . . . . ? C30 C31 N32 C35 175.8(6) . . . . ? C32 C31 N32 La1 168.6(5) . . . . ? C30 C31 N32 La1 -13.8(7) . . . . ? O20 La1 N32 C35 114.5(5) . . . . ? O30 La1 N32 C35 -51.3(6) . . . . ? O40' La1 N32 C35 33.4(9) . . . . ? O40 La1 N32 C35 27.7(11) . . . . ? N12 La1 N32 C35 -48.8(5) . . . . ? N21 La1 N32 C35 -172.5(5) . . . . ? N22 La1 N32 C35 86.7(6) . . . . ? N31 La1 N32 C35 -169.8(6) . . . . ? N11 La1 N32 C35 -111.1(5) . . . . ? O20 La1 N32 C31 -55.0(5) . . . . ? O30 La1 N32 C31 139.1(4) . . . . ? O40' La1 N32 C31 -136.1(9) . . . . ? O40 La1 N32 C31 -141.8(11) . . . . ? N12 La1 N32 C31 141.7(5) . . . . ? N21 La1 N32 C31 18.0(6) . . . . ? N22 La1 N32 C31 -82.8(5) . . . . ? N31 La1 N32 C31 20.7(4) . . . . ? N11 La1 N32 C31 79.4(5) . . . . ? N32 C31 C32 C33 2.8(11) . . . . ? C30 C31 C32 C33 -174.7(7) . . . . ? C31 C32 C33 C34 -2.7(12) . . . . ? C32 C33 C34 C35 1.7(12) . . . . ? C31 N32 C35 C34 0.8(10) . . . . ? La1 N32 C35 C34 -168.9(5) . . . . ? C33 C34 C35 N32 -0.7(11) . . . . ? O41 S4 O40 La1 109(6) . . . . ? O42 S4 O40 La1 -29(7) . . . . ? C40 S4 O40 La1 -142(6) . . . . ? O20 La1 O40 S4 61(6) . . . . ? O30 La1 O40 S4 -79(6) . . . . ? O40' La1 O40 S4 95(17) . . . . ? N12 La1 O40 S4 -146(6) . . . . ? N21 La1 O40 S4 -18(7) . . . . ? N32 La1 O40 S4 138(6) . . . . ? N22 La1 O40 S4 -11(6) . . . . ? N31 La1 O40 S4 116(6) . . . . ? N11 La1 O40 S4 -149(6) . . . . ? O41 S4 C40 F41 175.7(15) . . . . ? O40 S4 C40 F41 64(2) . . . . ? O42 S4 C40 F41 -58.5(16) . . . . ? O41 S4 C40 F40 52.0(14) . . . . ? O40 S4 C40 F40 -60(2) . . . . ? O42 S4 C40 F40 177.8(15) . . . . ? O41 S4 C40 F42 -69.5(16) . . . . ? O40 S4 C40 F42 179(2) . . . . ? O42 S4 C40 F42 56.3(17) . . . . ? O41' S4' O40' La1 -69(5) . . . . ? O42' S4' O40' La1 67(5) . . . . ? C40' S4' O40' La1 179(5) . . . . ? O20 La1 O40' S4' -6(5) . . . . ? O30 La1 O40' S4' -145(5) . . . . ? O40 La1 O40' S4' -151(19) . . . . ? N12 La1 O40' S4' 149(5) . . . . ? N21 La1 O40' S4' -74(5) . . . . ? N32 La1 O40' S4' 73(5) . . . . ? N22 La1 O40' S4' -78(5) . . . . ? N31 La1 O40' S4' 47(6) . . . . ? N11 La1 O40' S4' 136(5) . . . . ? O41' S4' C40' F40' -54.7(12) . . . . ? O42' S4' C40' F40' -178.9(12) . . . . ? O40' S4' C40' F40' 61.7(18) . . . . ? O41' S4' C40' F41' -177.8(11) . . . . ? O42' S4' C40' F41' 58.0(13) . . . . ? O40' S4' C40' F41' -61.4(17) . . . . ? O41' S4' C40' F42' 63.9(13) . . . . ? O42' S4' C40' F42' -60.4(14) . . . . ? O40' S4' C40' F42' -179.7(18) . . . . ? C996 O99 C999 C998 33.6(11) . . . . ? O99 C999 C998 C997 -19.6(14) . . . . ? C999 C998 C997 C996 -1.7(14) . . . . ? C999 O99 C996 C997 -34.7(12) . . . . ? C998 C997 C996 O99 22.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.640 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.114 _database_code_depnum_ccdc_archive 'CCDC 929143' ####################################################################### # # 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_? #============================================================================== _audit_creation_method 'form.cif (version 2.0)' #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_[Sm(1)(Otf)3] #TrackingRef 'complexes_ChemSci.cif' _chemical_name_systematic ; ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C24 H24 F9 N9 O9 P S4 Sm), C4 H10 O, C2 H3 N' _chemical_formula_sum 'C54 H61 F18 N19 O19 P2 S8 Sm2' _chemical_formula_weight 2241.44 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' P P 0.1023 0.0942 '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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.764(2) _cell_length_b 19.857(4) _cell_length_c 22.899(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.37(3) _cell_angle_gamma 90.00 _cell_volume 4403.2(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 29512 _cell_measurement_theta_min 3.90 _cell_measurement_theta_max 24.73 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 1.656 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi with CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29512 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 24.73 _reflns_number_total 7495 _reflns_number_gt 4973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement 'CrysAlis Red' _computing_data_reduction 'CrysAlis Red' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep32 _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^)+(0.0880P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7495 _refine_ls_number_parameters 665 _refine_ls_number_restraints 304 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 0.995 _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 Sm1 Sm 0.56546(4) 0.629155(19) 0.329836(17) 0.02839(16) Uani 1 1 d . . . S1 S 0.8509(2) 0.37299(10) 0.34767(10) 0.0396(5) Uani 1 1 d . . . P1 P 0.7586(2) 0.45776(10) 0.33819(9) 0.0302(5) Uani 1 1 d . A . N10 N 0.6033(6) 0.4572(3) 0.3597(3) 0.0340(16) Uani 1 1 d . . . C1 C 0.5227(8) 0.3948(4) 0.3576(4) 0.040(2) Uani 1 1 d . A . H1A H 0.5311 0.3747 0.3970 0.060 Uiso 1 1 calc R . . H1B H 0.5576 0.3632 0.3301 0.060 Uiso 1 1 calc R . . H1C H 0.4255 0.4049 0.3442 0.060 Uiso 1 1 calc R . . O20 O 0.4769(5) 0.7401(3) 0.3301(2) 0.0379(13) Uani 1 1 d . A . F20 F 0.4965(7) 0.9172(3) 0.3836(3) 0.0785(19) Uani 1 1 d . . . S2 S 0.4231(2) 0.80885(10) 0.32560(10) 0.0392(5) Uani 1 1 d . . . C2 C 0.8354(9) 0.4638(4) 0.2285(4) 0.043(2) Uani 1 1 d . A . H2A H 0.7860 0.4420 0.1935 0.064 Uiso 1 1 calc R . . H2B H 0.9019 0.4321 0.2490 0.064 Uiso 1 1 calc R . . H2C H 0.8845 0.5035 0.2165 0.064 Uiso 1 1 calc R . . N11 N 0.5517(6) 0.5145(3) 0.3822(3) 0.0302(15) Uani 1 1 d . A . O22 O 0.4507(6) 0.8426(3) 0.2735(3) 0.0495(16) Uani 1 1 d . A . F21 F 0.6613(6) 0.8472(3) 0.3788(3) 0.0757(18) Uani 1 1 d . . . S3 S 0.2261(2) 0.53962(11) 0.27771(10) 0.0393(5) Uani 1 1 d . . . N20 N 0.7369(6) 0.4844(3) 0.2678(3) 0.0316(15) Uani 1 1 d . . . F22 F 0.5118(6) 0.8274(3) 0.4364(3) 0.0715(17) Uani 1 1 d . . . O21 O 0.2869(6) 0.8137(3) 0.3410(3) 0.0574(18) Uani 1 1 d . A . C3 C 0.9745(8) 0.5083(4) 0.4140(4) 0.039(2) Uani 1 1 d . A . H3A H 1.0493 0.5087 0.3892 0.058 Uiso 1 1 calc R . . H3B H 0.9725 0.4646 0.4337 0.058 Uiso 1 1 calc R . . H3C H 0.9903 0.5440 0.4436 0.058 Uiso 1 1 calc R . . N21 N 0.6509(6) 0.5389(3) 0.2537(3) 0.0319(15) Uani 1 1 d . A . N30 N 0.8429(6) 0.5197(3) 0.3774(3) 0.0319(15) Uani 1 1 d . . . N31 N 0.8175(6) 0.5827(3) 0.3510(3) 0.0297(15) Uani 1 1 d . A . O30 O 0.3519(5) 0.5781(3) 0.2916(3) 0.0437(14) Uani 1 1 d . A . F31 F 0.2684(7) 0.5434(3) 0.1685(3) 0.0786(19) Uani 1 1 d . . . F30 F 0.1443(6) 0.4616(3) 0.1895(3) 0.0754(18) Uani 1 1 d . . . O31 O 0.1089(6) 0.5803(3) 0.2638(3) 0.0595(18) Uani 1 1 d . A . F32 F 0.3623(7) 0.4606(3) 0.2171(3) 0.097(2) Uani 1 1 d . . . O32 O 0.2141(6) 0.4853(3) 0.3169(3) 0.0609(18) Uani 1 1 d . A . N12 N 0.4051(6) 0.6253(3) 0.4111(3) 0.0323(15) Uani 1 1 d . A . C10 C 0.4552(7) 0.5072(4) 0.4147(3) 0.0293(17) Uani 1 1 d . . . H10 H 0.4291 0.4633 0.4254 0.035 Uiso 1 1 calc R A . C11 C 0.3849(7) 0.5656(4) 0.4355(3) 0.0276(17) Uani 1 1 d . A . C12 C 0.3000(8) 0.5573(4) 0.4788(3) 0.0338(18) Uani 1 1 d . . . H12 H 0.2879 0.5141 0.4952 0.041 Uiso 1 1 calc R A . C13 C 0.2332(8) 0.6128(4) 0.4977(4) 0.041(2) Uani 1 1 d . A . H13 H 0.1723 0.6082 0.5267 0.049 Uiso 1 1 calc R . . C14 C 0.2553(9) 0.6735(4) 0.4746(4) 0.047(2) Uani 1 1 d . . . H14 H 0.2123 0.7125 0.4878 0.056 Uiso 1 1 calc R A . C15 C 0.3416(8) 0.6782(4) 0.4315(4) 0.043(2) Uani 1 1 d . A . H15 H 0.3564 0.7213 0.4155 0.052 Uiso 1 1 calc R . . N22 N 0.4945(7) 0.6528(3) 0.2187(3) 0.0373(16) Uani 1 1 d . A . C20 C 0.6442(8) 0.5614(4) 0.2005(4) 0.041(2) Uani 1 1 d . . . H20 H 0.6991 0.5408 0.1741 0.049 Uiso 1 1 calc R A . C21 C 0.5554(8) 0.6173(4) 0.1799(4) 0.039(2) Uani 1 1 d . A . C22 C 0.5312(11) 0.6292(5) 0.1202(4) 0.064(3) Uani 1 1 d . . . H22 H 0.5781 0.6037 0.0938 0.077 Uiso 1 1 calc R A . C23 C 0.4391(12) 0.6782(6) 0.0992(5) 0.073(3) Uani 1 1 d . A . H23 H 0.4220 0.6875 0.0582 0.088 Uiso 1 1 calc R . . C24 C 0.3730(10) 0.7129(5) 0.1380(5) 0.059(3) Uani 1 1 d . . . H24 H 0.3068 0.7464 0.1245 0.071 Uiso 1 1 calc R A . C25 C 0.4024(9) 0.6995(4) 0.1969(4) 0.046(2) Uani 1 1 d . A . H25 H 0.3554 0.7245 0.2236 0.056 Uiso 1 1 calc R . . N32 N 0.7607(6) 0.7020(3) 0.2957(3) 0.0350(16) Uani 1 1 d . A . C30 C 0.9174(8) 0.6252(4) 0.3517(4) 0.0354(19) Uani 1 1 d . . . H30 H 1.0053 0.6160 0.3731 0.043 Uiso 1 1 calc R A . C31 C 0.8923(8) 0.6875(4) 0.3192(3) 0.0333(18) Uani 1 1 d . A . C32 C 1.0021(9) 0.7273(5) 0.3100(4) 0.053(2) Uani 1 1 d . . . H32 H 1.0931 0.7160 0.3270 0.063 Uiso 1 1 calc R A . C33 C 0.9775(10) 0.7841(5) 0.2756(5) 0.059(3) Uani 1 1 d . A . H33 H 1.0521 0.8125 0.2686 0.070 Uiso 1 1 calc R . . C34 C 0.8445(9) 0.7998(4) 0.2513(5) 0.053(3) Uani 1 1 d . . . H34 H 0.8254 0.8386 0.2274 0.063 Uiso 1 1 calc R A . C35 C 0.7415(9) 0.7572(4) 0.2629(4) 0.043(2) Uani 1 1 d . A . H35 H 0.6498 0.7677 0.2463 0.051 Uiso 1 1 calc R . . C300 C 0.2505(9) 0.4996(5) 0.2097(5) 0.054(3) Uani 1 1 d . A . C200 C 0.5280(11) 0.8518(5) 0.3844(5) 0.058(3) Uani 1 1 d . A . S4 S 0.7613(9) 0.6570(5) 0.4776(6) 0.049(2) Uani 0.588(9) 1 d PDU A 1 O40 O 0.693(3) 0.675(2) 0.4205(10) 0.032(4) Uani 0.588(9) 1 d PDU A 1 O41 O 0.9072(10) 0.6605(10) 0.4799(6) 0.090(5) Uani 0.588(9) 1 d PDU A 1 O42 O 0.7036(17) 0.5992(5) 0.5008(5) 0.072(4) Uani 0.588(9) 1 d PDU A 1 C40 C 0.7161(13) 0.7211(7) 0.5279(5) 0.065(4) Uani 0.588(9) 1 d PDU A 1 F40 F 0.749(2) 0.7792(7) 0.5066(10) 0.115(6) Uani 0.588(9) 1 d PDU A 1 F41 F 0.5815(12) 0.7210(9) 0.5268(5) 0.114(5) Uani 0.588(9) 1 d PDU A 1 F42 F 0.7802(16) 0.7090(6) 0.5808(4) 0.092(4) Uani 0.588(9) 1 d PDU A 1 S4' S 0.7199(13) 0.6563(7) 0.4827(8) 0.047(3) Uani 0.412(9) 1 d PDU A 2 O40' O 0.664(4) 0.675(4) 0.4242(13) 0.035(6) Uani 0.412(9) 1 d PDU A 2 O41' O 0.6180(17) 0.6536(15) 0.5213(7) 0.093(7) Uani 0.412(9) 1 d PDU A 2 O42' O 0.813(2) 0.6014(9) 0.4896(9) 0.073(5) Uani 0.412(9) 1 d PDU A 2 C40' C 0.8359(18) 0.7249(9) 0.5071(7) 0.060(4) Uani 0.412(9) 1 d PDU A 2 F40' F 0.775(3) 0.7819(11) 0.5164(17) 0.098(7) Uani 0.412(9) 1 d PDU A 2 F41' F 0.9277(16) 0.7268(13) 0.4707(9) 0.117(7) Uani 0.412(9) 1 d PDU A 2 F42' F 0.8928(18) 0.7131(8) 0.5609(7) 0.088(5) Uani 0.412(9) 1 d PDU A 2 C98 C 0.956(3) 0.6569(14) 0.1435(10) 0.095(8) Uani 0.50 1 d PDU . . H98A H 0.8719 0.6840 0.1425 0.143 Uiso 0.50 1 calc PR . . H98B H 1.0304 0.6848 0.1314 0.143 Uiso 0.50 1 calc PR . . H98C H 0.9834 0.6403 0.1836 0.143 Uiso 0.50 1 calc PR . . O99 O 0.8393(17) 0.5648(9) 0.0886(7) 0.092(5) Uani 0.50 1 d PDU . . C99 C 0.934(2) 0.6080(14) 0.1090(12) 0.082(7) Uani 0.50 1 d PDU . . H99A H 1.0116 0.5778 0.1235 0.099 Uiso 0.50 1 calc PR . . H99B H 0.9602 0.6272 0.0721 0.099 Uiso 0.50 1 calc PR . . C96 C 0.708(5) 0.4949(19) 0.015(2) 0.203(19) Uani 0.50 1 d PDU . . H96A H 0.7147 0.4494 0.0313 0.304 Uiso 0.50 1 calc PR . . H96B H 0.7021 0.4923 -0.0283 0.304 Uiso 0.50 1 calc PR . . H96C H 0.6243 0.5168 0.0253 0.304 Uiso 0.50 1 calc PR . . C97 C 0.812(3) 0.5285(18) 0.0347(18) 0.140(10) Uani 0.50 1 d PDU . . H97A H 0.8234 0.5620 0.0037 0.168 Uiso 0.50 1 calc PR . . H97B H 0.8903 0.4969 0.0350 0.168 Uiso 0.50 1 calc PR . . N88 N 0.016(3) 0.8733(16) 0.4133(10) 0.153(12) Uani 0.50 1 d PU . . C88 C 0.095(2) 0.8512(13) 0.4665(12) 0.083(8) Uani 0.50 1 d PU . . C87 C 0.160(2) 0.8378(11) 0.5024(11) 0.075(7) Uani 0.50 1 d PU . . H87A H 0.1774 0.7893 0.5013 0.112 Uiso 0.50 1 calc PR . . H87B H 0.1182 0.8488 0.5380 0.112 Uiso 0.50 1 calc PR . . H87C H 0.2470 0.8623 0.5028 0.112 Uiso 0.50 1 calc PR . . 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 Sm1 0.0276(2) 0.0286(2) 0.0297(2) 0.00060(18) 0.00657(17) -0.00180(17) S1 0.0436(12) 0.0315(11) 0.0454(13) 0.0013(10) 0.0132(10) 0.0079(9) P1 0.0305(11) 0.0293(11) 0.0316(12) -0.0007(9) 0.0070(9) 0.0005(8) N10 0.037(4) 0.027(3) 0.040(4) -0.002(3) 0.015(3) -0.004(3) C1 0.035(4) 0.035(5) 0.052(6) -0.005(4) 0.012(4) -0.006(4) O20 0.041(3) 0.036(3) 0.039(3) 0.005(3) 0.014(3) 0.004(2) F20 0.110(5) 0.035(3) 0.092(5) -0.014(3) 0.017(4) -0.008(3) S2 0.0412(12) 0.0307(11) 0.0454(13) 0.0058(9) 0.0052(10) 0.0033(9) C2 0.041(5) 0.042(5) 0.049(6) 0.004(4) 0.022(4) 0.006(4) N11 0.035(4) 0.030(4) 0.026(4) 0.001(3) 0.004(3) 0.001(3) O22 0.062(4) 0.037(3) 0.048(4) 0.014(3) 0.003(3) 0.006(3) F21 0.058(4) 0.084(4) 0.082(5) -0.004(3) -0.004(3) -0.020(3) S3 0.0289(11) 0.0466(13) 0.0423(13) -0.0054(10) 0.0048(10) -0.0058(9) N20 0.037(4) 0.027(3) 0.033(4) -0.002(3) 0.011(3) -0.002(3) F22 0.097(5) 0.067(4) 0.051(4) -0.007(3) 0.010(3) -0.014(3) O21 0.039(3) 0.052(4) 0.084(5) 0.010(3) 0.016(3) 0.011(3) C3 0.029(4) 0.051(5) 0.036(5) 0.002(4) 0.003(4) 0.002(4) N21 0.029(3) 0.034(4) 0.032(4) 0.005(3) 0.004(3) -0.009(3) N30 0.034(4) 0.029(4) 0.033(4) 0.001(3) 0.007(3) 0.009(3) N31 0.029(3) 0.026(3) 0.034(4) -0.008(3) 0.004(3) -0.002(3) O30 0.037(3) 0.050(4) 0.042(4) -0.001(3) -0.003(3) -0.015(3) F31 0.095(5) 0.098(5) 0.045(4) -0.009(3) 0.018(3) -0.032(4) F30 0.061(4) 0.088(4) 0.078(4) -0.035(3) 0.011(3) -0.029(3) O31 0.041(4) 0.065(4) 0.071(5) -0.017(4) 0.002(3) 0.016(3) F32 0.067(4) 0.099(5) 0.128(6) -0.055(5) 0.021(4) 0.019(4) O32 0.053(4) 0.060(4) 0.071(5) 0.013(4) 0.012(4) -0.022(3) N12 0.030(3) 0.030(4) 0.038(4) -0.007(3) 0.012(3) -0.007(3) C10 0.021(4) 0.037(4) 0.030(4) 0.005(3) 0.000(3) -0.004(3) C11 0.016(3) 0.031(4) 0.036(5) 0.003(3) 0.002(3) -0.010(3) C12 0.033(4) 0.039(5) 0.030(4) 0.009(4) 0.007(4) -0.003(4) C13 0.038(5) 0.059(6) 0.028(5) -0.003(4) 0.013(4) -0.011(4) C14 0.055(6) 0.041(5) 0.049(6) -0.001(4) 0.027(5) 0.011(4) C15 0.038(5) 0.038(5) 0.058(6) 0.004(4) 0.017(4) 0.003(4) N22 0.039(4) 0.038(4) 0.033(4) 0.002(3) -0.005(3) -0.004(3) C20 0.039(5) 0.051(5) 0.034(5) -0.008(4) 0.011(4) -0.002(4) C21 0.036(5) 0.047(5) 0.034(5) 0.008(4) 0.006(4) 0.000(4) C22 0.072(7) 0.087(8) 0.034(5) 0.009(5) 0.004(5) 0.029(6) C23 0.084(8) 0.101(9) 0.034(6) 0.019(6) 0.005(6) 0.027(7) C24 0.064(6) 0.056(6) 0.054(7) 0.011(5) -0.005(5) 0.021(5) C25 0.047(5) 0.052(6) 0.036(5) -0.004(4) -0.006(4) 0.008(4) N32 0.037(4) 0.034(4) 0.035(4) 0.006(3) 0.011(3) -0.002(3) C30 0.033(4) 0.035(5) 0.037(5) 0.000(4) 0.000(4) 0.000(4) C31 0.037(4) 0.030(4) 0.033(5) -0.004(3) 0.007(4) -0.002(4) C32 0.038(5) 0.049(6) 0.072(7) 0.011(5) 0.009(5) -0.011(4) C33 0.058(6) 0.042(6) 0.079(8) 0.015(5) 0.022(6) -0.015(5) C34 0.053(6) 0.039(5) 0.069(7) 0.023(5) 0.018(5) 0.001(4) C35 0.038(5) 0.044(5) 0.045(5) 0.013(4) 0.006(4) -0.001(4) C300 0.039(5) 0.065(7) 0.060(7) -0.020(5) 0.009(5) -0.012(5) C200 0.059(7) 0.063(7) 0.053(7) 0.003(5) 0.012(5) -0.002(5) S4 0.055(4) 0.045(3) 0.045(4) -0.012(3) -0.007(4) 0.012(3) O40 0.028(11) 0.038(7) 0.033(5) -0.005(5) 0.016(6) -0.001(10) O41 0.047(6) 0.154(14) 0.064(9) -0.020(9) -0.008(6) 0.023(7) O42 0.119(11) 0.031(6) 0.054(8) 0.006(5) -0.037(8) -0.021(7) C40 0.077(8) 0.067(7) 0.044(7) -0.029(6) -0.015(8) 0.000(8) F40 0.185(14) 0.035(6) 0.099(11) -0.020(6) -0.084(10) 0.002(7) F41 0.089(7) 0.195(14) 0.062(8) -0.014(9) 0.017(6) 0.060(8) F42 0.129(10) 0.099(9) 0.042(5) -0.023(5) -0.013(6) 0.025(8) S4' 0.055(6) 0.048(5) 0.036(4) -0.006(4) 0.000(4) -0.015(4) O40' 0.012(12) 0.054(11) 0.038(8) -0.018(10) 0.003(8) -0.006(11) O41' 0.060(11) 0.17(2) 0.052(10) -0.002(13) 0.013(8) -0.033(10) O42' 0.104(9) 0.046(7) 0.064(9) 0.004(6) -0.004(7) 0.012(7) C40' 0.049(11) 0.062(9) 0.061(10) -0.018(10) -0.022(7) -0.003(7) F40' 0.119(10) 0.066(7) 0.098(11) -0.021(7) -0.026(8) -0.002(7) F41' 0.051(9) 0.180(19) 0.118(12) -0.001(14) 0.004(8) -0.054(10) F42' 0.072(11) 0.100(11) 0.077(9) -0.027(9) -0.046(8) 0.000(9) C98 0.106(18) 0.134(19) 0.042(14) 0.052(11) -0.006(13) 0.060(15) O99 0.088(11) 0.117(14) 0.079(11) 0.029(9) 0.044(10) 0.037(9) C99 0.050(12) 0.117(18) 0.077(16) 0.063(10) -0.001(12) 0.049(10) C96 0.26(4) 0.09(3) 0.27(4) -0.10(3) 0.07(3) -0.02(3) C97 0.16(2) 0.12(2) 0.16(2) -0.036(17) 0.09(2) 0.021(17) N88 0.16(2) 0.24(3) 0.052(13) -0.026(16) -0.021(14) 0.08(2) C88 0.056(13) 0.105(18) 0.077(15) -0.053(13) -0.034(11) 0.029(12) C87 0.052(13) 0.074(15) 0.084(16) -0.045(12) -0.043(11) 0.015(11) _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 Sm1 O20 2.368(5) . ? Sm1 O30 2.382(5) . ? Sm1 O40' 2.43(5) . ? Sm1 O40 2.45(3) . ? Sm1 N12 2.582(6) . ? Sm1 N11 2.585(6) . ? Sm1 N22 2.592(7) . ? Sm1 N32 2.592(6) . ? Sm1 N31 2.614(6) . ? Sm1 N21 2.706(6) . ? S1 P1 1.909(3) . ? P1 N10 1.653(6) . ? P1 N30 1.676(7) . ? P1 N20 1.684(7) . ? N10 N11 1.372(8) . ? N10 C1 1.465(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O20 S2 1.461(5) . ? F20 C200 1.334(11) . ? S2 O21 1.422(6) . ? S2 O22 1.425(6) . ? S2 C200 1.798(11) . ? C2 N20 1.457(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N11 C10 1.282(9) . ? F21 C200 1.327(11) . ? S3 O31 1.403(6) . ? S3 O32 1.417(6) . ? S3 O30 1.447(5) . ? S3 C300 1.791(10) . ? N20 N21 1.383(8) . ? F22 C200 1.314(11) . ? C3 N30 1.459(10) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N21 C20 1.291(10) . ? N30 N31 1.398(8) . ? N31 C30 1.288(9) . ? F31 C300 1.310(12) . ? F30 C300 1.318(10) . ? F32 C300 1.331(11) . ? N12 C15 1.334(10) . ? N12 C11 1.337(9) . ? C10 C11 1.458(10) . ? C10 H10 0.9500 . ? C11 C12 1.380(10) . ? C12 C13 1.378(11) . ? C12 H12 0.9500 . ? C13 C14 1.345(11) . ? C13 H13 0.9500 . ? C14 C15 1.381(11) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? N22 C21 1.333(10) . ? N22 C25 1.344(10) . ? C20 C21 1.450(11) . ? C20 H20 0.9500 . ? C21 C22 1.378(12) . ? C22 C23 1.369(13) . ? C22 H22 0.9500 . ? C23 C24 1.353(14) . ? C23 H23 0.9500 . ? C24 C25 1.368(13) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N32 C35 1.328(10) . ? N32 C31 1.359(10) . ? C30 C31 1.448(11) . ? C30 H30 0.9500 . ? C31 C32 1.370(11) . ? C32 C33 1.381(12) . ? C32 H32 0.9500 . ? C33 C34 1.381(13) . ? C33 H33 0.9500 . ? C34 C35 1.366(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? S4 O42 1.411(9) . ? S4 O41 1.421(9) . ? S4 O40 1.432(8) . ? S4 C40 1.809(9) . ? C40 F40 1.310(10) . ? C40 F41 1.311(9) . ? C40 F42 1.312(9) . ? S4' O41' 1.414(10) . ? S4' O42' 1.418(9) . ? S4' O40' 1.430(10) . ? S4' C40' 1.814(10) . ? C40' F41' 1.301(10) . ? C40' F42' 1.305(10) . ? C40' F40' 1.310(10) . ? C98 C99 1.25(3) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? O99 C99 1.30(3) . ? O99 C97 1.42(3) . ? C99 H99A 0.9900 . ? C99 H99B 0.9900 . ? C96 C97 1.26(3) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? N88 C88 1.42(3) . ? C88 C87 1.01(3) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? 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 O20 Sm1 O30 95.40(19) . . ? O20 Sm1 O40' 75.5(15) . . ? O30 Sm1 O40' 135.7(10) . . ? O20 Sm1 O40 78.5(10) . . ? O30 Sm1 O40 142.5(7) . . ? O40' Sm1 O40 7.2(17) . . ? O20 Sm1 N12 76.71(18) . . ? O30 Sm1 N12 70.7(2) . . ? O40' Sm1 N12 65.0(10) . . ? O40 Sm1 N12 71.9(7) . . ? O20 Sm1 N11 141.07(19) . . ? O30 Sm1 N11 72.6(2) . . ? O40' Sm1 N11 87.5(14) . . ? O40 Sm1 N11 89.0(9) . . ? N12 Sm1 N11 64.36(19) . . ? O20 Sm1 N22 77.4(2) . . ? O30 Sm1 N22 66.7(2) . . ? O40' Sm1 N22 146.2(14) . . ? O40 Sm1 N22 143.8(9) . . ? N12 Sm1 N22 127.0(2) . . ? N11 Sm1 N22 126.3(2) . . ? O20 Sm1 N32 76.36(18) . . ? O30 Sm1 N32 140.3(2) . . ? O40' Sm1 N32 80.5(11) . . ? O40 Sm1 N32 74.8(7) . . ? N12 Sm1 N32 140.5(2) . . ? N11 Sm1 N32 135.7(2) . . ? N22 Sm1 N32 73.6(2) . . ? O20 Sm1 N31 131.53(18) . . ? O30 Sm1 N31 132.62(19) . . ? O40' Sm1 N31 73.2(12) . . ? O40 Sm1 N31 67.0(9) . . ? N12 Sm1 N31 120.0(2) . . ? N11 Sm1 N31 72.96(19) . . ? N22 Sm1 N31 111.9(2) . . ? N32 Sm1 N31 62.7(2) . . ? O20 Sm1 N21 139.57(18) . . ? O30 Sm1 N21 78.97(19) . . ? O40' Sm1 N21 134.7(13) . . ? O40 Sm1 N21 128.6(9) . . ? N12 Sm1 N21 135.25(18) . . ? N11 Sm1 N21 75.76(18) . . ? N22 Sm1 N21 63.5(2) . . ? N32 Sm1 N21 82.89(19) . . ? N31 Sm1 N21 61.68(19) . . ? N10 P1 N30 104.6(3) . . ? N10 P1 N20 106.3(3) . . ? N30 P1 N20 106.0(3) . . ? N10 P1 S1 113.4(2) . . ? N30 P1 S1 113.2(2) . . ? N20 P1 S1 112.6(2) . . ? N11 N10 C1 119.5(6) . . ? N11 N10 P1 120.1(5) . . ? C1 N10 P1 120.4(5) . . ? N10 C1 H1A 109.5 . . ? N10 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N10 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S2 O20 Sm1 175.7(3) . . ? O21 S2 O22 117.4(4) . . ? O21 S2 O20 112.6(3) . . ? O22 S2 O20 113.2(3) . . ? O21 S2 C200 104.1(5) . . ? O22 S2 C200 104.7(4) . . ? O20 S2 C200 103.0(4) . . ? N20 C2 H2A 109.5 . . ? N20 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N20 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C10 N11 N10 117.3(6) . . ? C10 N11 Sm1 117.0(5) . . ? N10 N11 Sm1 120.9(4) . . ? O31 S3 O32 116.8(4) . . ? O31 S3 O30 113.0(4) . . ? O32 S3 O30 113.6(4) . . ? O31 S3 C300 104.7(5) . . ? O32 S3 C300 104.2(5) . . ? O30 S3 C300 102.8(4) . . ? N21 N20 C2 120.3(6) . . ? N21 N20 P1 117.8(5) . . ? C2 N20 P1 119.4(5) . . ? N30 C3 H3A 109.5 . . ? N30 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N30 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C20 N21 N20 116.5(7) . . ? C20 N21 Sm1 113.3(5) . . ? N20 N21 Sm1 126.6(5) . . ? N31 N30 C3 118.8(6) . . ? N31 N30 P1 112.2(5) . . ? C3 N30 P1 121.9(5) . . ? C30 N31 N30 119.3(6) . . ? C30 N31 Sm1 117.7(5) . . ? N30 N31 Sm1 120.4(4) . . ? S3 O30 Sm1 169.7(4) . . ? C15 N12 C11 116.8(7) . . ? C15 N12 Sm1 125.5(5) . . ? C11 N12 Sm1 117.6(5) . . ? N11 C10 C11 120.8(7) . . ? N11 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? N12 C11 C12 122.7(7) . . ? N12 C11 C10 117.8(6) . . ? C12 C11 C10 119.4(7) . . ? C13 C12 C11 118.9(7) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 119.1(8) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 119.1(8) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N12 C15 C14 123.4(8) . . ? N12 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C21 N22 C25 116.8(7) . . ? C21 N22 Sm1 118.2(5) . . ? C25 N22 Sm1 124.9(6) . . ? N21 C20 C21 121.9(8) . . ? N21 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? N22 C21 C22 122.5(8) . . ? N22 C21 C20 119.1(7) . . ? C22 C21 C20 118.3(8) . . ? C23 C22 C21 119.4(10) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 118.6(10) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 119.4(9) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N22 C25 C24 123.1(9) . . ? N22 C25 H25 118.4 . . ? C24 C25 H25 118.4 . . ? C35 N32 C31 117.2(7) . . ? C35 N32 Sm1 125.1(5) . . ? C31 N32 Sm1 117.2(5) . . ? N31 C30 C31 118.3(7) . . ? N31 C30 H30 120.8 . . ? C31 C30 H30 120.8 . . ? N32 C31 C32 122.4(8) . . ? N32 C31 C30 118.3(7) . . ? C32 C31 C30 119.2(8) . . ? C31 C32 C33 118.5(9) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 120.0(8) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 117.4(8) . . ? C35 C34 H34 121.3 . . ? C33 C34 H34 121.3 . . ? N32 C35 C34 124.6(8) . . ? N32 C35 H35 117.7 . . ? C34 C35 H35 117.7 . . ? F31 C300 F30 107.4(9) . . ? F31 C300 F32 107.2(8) . . ? F30 C300 F32 107.9(8) . . ? F31 C300 S3 112.2(7) . . ? F30 C300 S3 111.9(7) . . ? F32 C300 S3 110.2(7) . . ? F22 C200 F21 107.1(9) . . ? F22 C200 F20 108.4(8) . . ? F21 C200 F20 107.0(8) . . ? F22 C200 S2 112.4(7) . . ? F21 C200 S2 111.6(7) . . ? F20 C200 S2 110.1(7) . . ? O42 S4 O41 118.2(13) . . ? O42 S4 O40 112.3(18) . . ? O41 S4 O40 111.7(15) . . ? O42 S4 C40 101.0(10) . . ? O41 S4 C40 105.5(10) . . ? O40 S4 C40 107(2) . . ? S4 O40 Sm1 144(3) . . ? F40 C40 F41 106.8(16) . . ? F40 C40 F42 113.2(15) . . ? F41 C40 F42 112.0(14) . . ? F40 C40 S4 106.9(11) . . ? F41 C40 S4 108.3(10) . . ? F42 C40 S4 109.4(10) . . ? O41' S4' O42' 113.3(19) . . ? O41' S4' O40' 112(2) . . ? O42' S4' O40' 118(3) . . ? O41' S4' C40' 107.3(14) . . ? O42' S4' C40' 100.1(14) . . ? O40' S4' C40' 104(3) . . ? S4' O40' Sm1 143(5) . . ? F41' C40' F42' 111.4(19) . . ? F41' C40' F40' 116(2) . . ? F42' C40' F40' 99(2) . . ? F41' C40' S4' 106.2(13) . . ? F42' C40' S4' 109.3(14) . . ? F40' C40' S4' 114.8(19) . . ? C99 C98 H98A 109.5 . . ? C99 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C99 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C99 O99 C97 134(2) . . ? C98 C99 O99 142(3) . . ? C98 C99 H99A 101.4 . . ? O99 C99 H99A 101.4 . . ? C98 C99 H99B 101.4 . . ? O99 C99 H99B 101.4 . . ? H99A C99 H99B 104.6 . . ? C97 C96 H96A 109.5 . . ? C97 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C97 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C96 C97 O99 130(3) . . ? C96 C97 H97A 104.8 . . ? O99 C97 H97A 104.8 . . ? C96 C97 H97B 104.8 . . ? O99 C97 H97B 104.8 . . ? H97A C97 H97B 105.8 . . ? C87 C88 N88 174(4) . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N30 P1 N10 N11 25.2(6) . . . . ? N20 P1 N10 N11 -86.7(6) . . . . ? S1 P1 N10 N11 149.0(5) . . . . ? N30 P1 N10 C1 -151.8(6) . . . . ? N20 P1 N10 C1 96.3(7) . . . . ? S1 P1 N10 C1 -28.0(7) . . . . ? O30 Sm1 O20 S2 -80(5) . . . . ? O40' Sm1 O20 S2 144(5) . . . . ? O40 Sm1 O20 S2 137(5) . . . . ? N12 Sm1 O20 S2 -149(5) . . . . ? N11 Sm1 O20 S2 -149(4) . . . . ? N22 Sm1 O20 S2 -15(5) . . . . ? N32 Sm1 O20 S2 61(5) . . . . ? N31 Sm1 O20 S2 93(5) . . . . ? N21 Sm1 O20 S2 -1(5) . . . . ? Sm1 O20 S2 O21 119(5) . . . . ? Sm1 O20 S2 O22 -17(5) . . . . ? Sm1 O20 S2 C200 -130(5) . . . . ? C1 N10 N11 C10 18.7(10) . . . . ? P1 N10 N11 C10 -158.4(6) . . . . ? C1 N10 N11 Sm1 -135.9(6) . . . . ? P1 N10 N11 Sm1 47.1(7) . . . . ? O20 Sm1 N11 C10 12.6(7) . . . . ? O30 Sm1 N11 C10 -64.0(5) . . . . ? O40' Sm1 N11 C10 75.8(12) . . . . ? O40 Sm1 N11 C10 82.8(9) . . . . ? N12 Sm1 N11 C10 12.5(5) . . . . ? N22 Sm1 N11 C10 -106.0(5) . . . . ? N32 Sm1 N11 C10 149.6(5) . . . . ? N31 Sm1 N11 C10 149.0(6) . . . . ? N21 Sm1 N11 C10 -146.7(6) . . . . ? O20 Sm1 N11 N10 167.3(4) . . . . ? O30 Sm1 N11 N10 90.6(5) . . . . ? O40' Sm1 N11 N10 -129.6(12) . . . . ? O40 Sm1 N11 N10 -122.5(9) . . . . ? N12 Sm1 N11 N10 167.1(6) . . . . ? N22 Sm1 N11 N10 48.7(6) . . . . ? N32 Sm1 N11 N10 -55.8(6) . . . . ? N31 Sm1 N11 N10 -56.3(5) . . . . ? N21 Sm1 N11 N10 7.9(5) . . . . ? N10 P1 N20 N21 44.2(6) . . . . ? N30 P1 N20 N21 -66.7(6) . . . . ? S1 P1 N20 N21 169.0(4) . . . . ? N10 P1 N20 C2 -153.4(6) . . . . ? N30 P1 N20 C2 95.7(6) . . . . ? S1 P1 N20 C2 -28.6(6) . . . . ? C2 N20 N21 C20 12.7(10) . . . . ? P1 N20 N21 C20 174.9(6) . . . . ? C2 N20 N21 Sm1 -144.6(6) . . . . ? P1 N20 N21 Sm1 17.6(7) . . . . ? O20 Sm1 N21 C20 0.8(7) . . . . ? O30 Sm1 N21 C20 86.2(6) . . . . ? O40' Sm1 N21 C20 -127.4(18) . . . . ? O40 Sm1 N21 C20 -122.3(11) . . . . ? N12 Sm1 N21 C20 133.7(5) . . . . ? N11 Sm1 N21 C20 160.8(6) . . . . ? N22 Sm1 N21 C20 16.9(5) . . . . ? N32 Sm1 N21 C20 -58.3(5) . . . . ? N31 Sm1 N21 C20 -121.1(6) . . . . ? O20 Sm1 N21 N20 158.8(4) . . . . ? O30 Sm1 N21 N20 -115.9(5) . . . . ? O40' Sm1 N21 N20 30.5(19) . . . . ? O40 Sm1 N21 N20 35.7(12) . . . . ? N12 Sm1 N21 N20 -68.3(6) . . . . ? N11 Sm1 N21 N20 -41.2(5) . . . . ? N22 Sm1 N21 N20 174.8(6) . . . . ? N32 Sm1 N21 N20 99.6(5) . . . . ? N31 Sm1 N21 N20 36.8(5) . . . . ? N10 P1 N30 N31 -85.0(5) . . . . ? N20 P1 N30 N31 27.1(5) . . . . ? S1 P1 N30 N31 151.1(4) . . . . ? N10 P1 N30 C3 124.8(6) . . . . ? N20 P1 N30 C3 -123.1(6) . . . . ? S1 P1 N30 C3 0.9(6) . . . . ? C3 N30 N31 C30 10.8(10) . . . . ? P1 N30 N31 C30 -140.4(6) . . . . ? C3 N30 N31 Sm1 -150.3(5) . . . . ? P1 N30 N31 Sm1 58.5(6) . . . . ? O20 Sm1 N31 C30 -14.6(7) . . . . ? O30 Sm1 N31 C30 155.8(5) . . . . ? O40' Sm1 N31 C30 -66.6(15) . . . . ? O40 Sm1 N31 C30 -62.9(10) . . . . ? N12 Sm1 N31 C30 -113.5(6) . . . . ? N11 Sm1 N31 C30 -159.2(6) . . . . ? N22 Sm1 N31 C30 77.9(6) . . . . ? N32 Sm1 N31 C30 21.2(5) . . . . ? N21 Sm1 N31 C30 118.1(6) . . . . ? O20 Sm1 N31 N30 146.9(4) . . . . ? O30 Sm1 N31 N30 -42.8(6) . . . . ? O40' Sm1 N31 N30 94.8(14) . . . . ? O40 Sm1 N31 N30 98.6(10) . . . . ? N12 Sm1 N31 N30 47.9(5) . . . . ? N11 Sm1 N31 N30 2.3(5) . . . . ? N22 Sm1 N31 N30 -120.7(5) . . . . ? N32 Sm1 N31 N30 -177.3(5) . . . . ? N21 Sm1 N31 N30 -80.4(5) . . . . ? O31 S3 O30 Sm1 129(2) . . . . ? O32 S3 O30 Sm1 -7(2) . . . . ? C300 S3 O30 Sm1 -118(2) . . . . ? O20 Sm1 O30 S3 -124(2) . . . . ? O40' Sm1 O30 S3 -49(3) . . . . ? O40 Sm1 O30 S3 -46(3) . . . . ? N12 Sm1 O30 S3 -50(2) . . . . ? N11 Sm1 O30 S3 18(2) . . . . ? N22 Sm1 O30 S3 162(2) . . . . ? N32 Sm1 O30 S3 161(2) . . . . ? N31 Sm1 O30 S3 63(2) . . . . ? N21 Sm1 O30 S3 97(2) . . . . ? O20 Sm1 N12 C15 -6.8(6) . . . . ? O30 Sm1 N12 C15 -107.5(7) . . . . ? O40' Sm1 N12 C15 73.2(18) . . . . ? O40 Sm1 N12 C15 75.2(12) . . . . ? N11 Sm1 N12 C15 173.0(7) . . . . ? N22 Sm1 N12 C15 -69.6(7) . . . . ? N32 Sm1 N12 C15 41.3(8) . . . . ? N31 Sm1 N12 C15 123.7(6) . . . . ? N21 Sm1 N12 C15 -157.6(6) . . . . ? O20 Sm1 N12 C11 174.1(6) . . . . ? O30 Sm1 N12 C11 73.4(5) . . . . ? O40' Sm1 N12 C11 -105.9(18) . . . . ? O40 Sm1 N12 C11 -103.8(12) . . . . ? N11 Sm1 N12 C11 -6.1(5) . . . . ? N22 Sm1 N12 C11 111.3(5) . . . . ? N32 Sm1 N12 C11 -137.8(5) . . . . ? N31 Sm1 N12 C11 -55.4(6) . . . . ? N21 Sm1 N12 C11 23.3(7) . . . . ? N10 N11 C10 C11 -173.7(6) . . . . ? Sm1 N11 C10 C11 -18.2(9) . . . . ? C15 N12 C11 C12 1.6(11) . . . . ? Sm1 N12 C11 C12 -179.2(5) . . . . ? C15 N12 C11 C10 -178.9(7) . . . . ? Sm1 N12 C11 C10 0.2(8) . . . . ? N11 C10 C11 N12 12.4(10) . . . . ? N11 C10 C11 C12 -168.2(7) . . . . ? N12 C11 C12 C13 0.0(11) . . . . ? C10 C11 C12 C13 -179.4(7) . . . . ? C11 C12 C13 C14 -1.7(12) . . . . ? C12 C13 C14 C15 1.7(13) . . . . ? C11 N12 C15 C14 -1.7(12) . . . . ? Sm1 N12 C15 C14 179.2(7) . . . . ? C13 C14 C15 N12 0.0(14) . . . . ? O20 Sm1 N22 C21 156.9(6) . . . . ? O30 Sm1 N22 C21 -101.5(6) . . . . ? O40' Sm1 N22 C21 119(2) . . . . ? O40 Sm1 N22 C21 107.5(15) . . . . ? N12 Sm1 N22 C21 -140.6(6) . . . . ? N11 Sm1 N22 C21 -57.5(7) . . . . ? N32 Sm1 N22 C21 77.7(6) . . . . ? N31 Sm1 N22 C21 27.0(6) . . . . ? N21 Sm1 N22 C21 -12.5(5) . . . . ? O20 Sm1 N22 C25 -21.5(6) . . . . ? O30 Sm1 N22 C25 80.1(7) . . . . ? O40' Sm1 N22 C25 -59(2) . . . . ? O40 Sm1 N22 C25 -71.0(16) . . . . ? N12 Sm1 N22 C25 40.9(7) . . . . ? N11 Sm1 N22 C25 124.1(6) . . . . ? N32 Sm1 N22 C25 -100.8(7) . . . . ? N31 Sm1 N22 C25 -151.5(6) . . . . ? N21 Sm1 N22 C25 169.1(7) . . . . ? N20 N21 C20 C21 178.6(7) . . . . ? Sm1 N21 C20 C21 -21.2(10) . . . . ? C25 N22 C21 C22 2.9(13) . . . . ? Sm1 N22 C21 C22 -175.7(7) . . . . ? C25 N22 C21 C20 -173.4(7) . . . . ? Sm1 N22 C21 C20 8.1(10) . . . . ? N21 C20 C21 N22 10.0(12) . . . . ? N21 C20 C21 C22 -166.4(9) . . . . ? N22 C21 C22 C23 -1.5(16) . . . . ? C20 C21 C22 C23 174.8(9) . . . . ? C21 C22 C23 C24 -0.8(17) . . . . ? C22 C23 C24 C25 1.7(17) . . . . ? C21 N22 C25 C24 -2.0(13) . . . . ? Sm1 N22 C25 C24 176.5(7) . . . . ? C23 C24 C25 N22 -0.2(15) . . . . ? O20 Sm1 N32 C35 -34.5(6) . . . . ? O30 Sm1 N32 C35 47.5(8) . . . . ? O40' Sm1 N32 C35 -111.7(16) . . . . ? O40 Sm1 N32 C35 -116.1(12) . . . . ? N12 Sm1 N32 C35 -82.7(7) . . . . ? N11 Sm1 N32 C35 171.7(6) . . . . ? N22 Sm1 N32 C35 46.2(6) . . . . ? N31 Sm1 N32 C35 172.3(7) . . . . ? N21 Sm1 N32 C35 110.6(7) . . . . ? O20 Sm1 N32 C31 136.9(6) . . . . ? O30 Sm1 N32 C31 -141.1(5) . . . . ? O40' Sm1 N32 C31 59.7(16) . . . . ? O40 Sm1 N32 C31 55.3(11) . . . . ? N12 Sm1 N32 C31 88.7(6) . . . . ? N11 Sm1 N32 C31 -16.9(7) . . . . ? N22 Sm1 N32 C31 -142.4(6) . . . . ? N31 Sm1 N32 C31 -16.3(5) . . . . ? N21 Sm1 N32 C31 -78.0(5) . . . . ? N30 N31 C30 C31 174.0(6) . . . . ? Sm1 N31 C30 C31 -24.4(9) . . . . ? C35 N32 C31 C32 0.1(12) . . . . ? Sm1 N32 C31 C32 -172.0(7) . . . . ? C35 N32 C31 C30 -175.8(7) . . . . ? Sm1 N32 C31 C30 12.1(9) . . . . ? N31 C30 C31 N32 8.3(11) . . . . ? N31 C30 C31 C32 -167.7(8) . . . . ? N32 C31 C32 C33 -0.1(14) . . . . ? C30 C31 C32 C33 175.7(9) . . . . ? C31 C32 C33 C34 0.0(15) . . . . ? C32 C33 C34 C35 0.1(15) . . . . ? C31 N32 C35 C34 0.0(13) . . . . ? Sm1 N32 C35 C34 171.4(7) . . . . ? C33 C34 C35 N32 -0.1(15) . . . . ? O31 S3 C300 F31 59.1(8) . . . . ? O32 S3 C300 F31 -177.8(7) . . . . ? O30 S3 C300 F31 -59.1(7) . . . . ? O31 S3 C300 F30 -61.6(9) . . . . ? O32 S3 C300 F30 61.4(8) . . . . ? O30 S3 C300 F30 -179.9(7) . . . . ? O31 S3 C300 F32 178.4(7) . . . . ? O32 S3 C300 F32 -58.5(8) . . . . ? O30 S3 C300 F32 60.2(8) . . . . ? O21 S2 C200 F22 54.8(8) . . . . ? O22 S2 C200 F22 178.5(7) . . . . ? O20 S2 C200 F22 -62.9(8) . . . . ? O21 S2 C200 F21 175.1(7) . . . . ? O22 S2 C200 F21 -61.2(8) . . . . ? O20 S2 C200 F21 57.4(8) . . . . ? O21 S2 C200 F20 -66.3(8) . . . . ? O22 S2 C200 F20 57.5(8) . . . . ? O20 S2 C200 F20 176.1(6) . . . . ? O42 S4 O40 Sm1 -30(4) . . . . ? O41 S4 O40 Sm1 106(3) . . . . ? C40 S4 O40 Sm1 -139(3) . . . . ? O20 Sm1 O40 S4 153(3) . . . . ? O30 Sm1 O40 S4 69(4) . . . . ? O40' Sm1 O40 S4 89(19) . . . . ? N12 Sm1 O40 S4 73(3) . . . . ? N11 Sm1 O40 S4 10(3) . . . . ? N22 Sm1 O40 S4 -158(2) . . . . ? N32 Sm1 O40 S4 -128(3) . . . . ? N31 Sm1 O40 S4 -62(3) . . . . ? N21 Sm1 O40 S4 -61(3) . . . . ? O42 S4 C40 F40 -172.2(14) . . . . ? O41 S4 C40 F40 64.2(16) . . . . ? O40 S4 C40 F40 -54.7(19) . . . . ? O42 S4 C40 F41 -57.5(14) . . . . ? O41 S4 C40 F41 178.9(13) . . . . ? O40 S4 C40 F41 60.0(18) . . . . ? O42 S4 C40 F42 64.9(14) . . . . ? O41 S4 C40 F42 -58.7(15) . . . . ? O40 S4 C40 F42 -177.6(18) . . . . ? O41' S4' O40' Sm1 -91(5) . . . . ? O42' S4' O40' Sm1 44(5) . . . . ? C40' S4' O40' Sm1 153(4) . . . . ? O20 Sm1 O40' S4' 156(4) . . . . ? O30 Sm1 O40' S4' 73(5) . . . . ? O40 Sm1 O40' S4' -90(21) . . . . ? N12 Sm1 O40' S4' 74(4) . . . . ? N11 Sm1 O40' S4' 11(4) . . . . ? N22 Sm1 O40' S4' -166(3) . . . . ? N32 Sm1 O40' S4' -126(4) . . . . ? N31 Sm1 O40' S4' -62(4) . . . . ? N21 Sm1 O40' S4' -56(5) . . . . ? O41' S4' C40' F41' -179.4(18) . . . . ? O42' S4' C40' F41' 62(2) . . . . ? O40' S4' C40' F41' -60(3) . . . . ? O41' S4' C40' F42' 60(2) . . . . ? O42' S4' C40' F42' -58.1(19) . . . . ? O40' S4' C40' F42' 180(3) . . . . ? O41' S4' C40' F40' -49(3) . . . . ? O42' S4' C40' F40' -168(2) . . . . ? O40' S4' C40' F40' 70(3) . . . . ? C97 O99 C99 C98 152(4) . . . . ? C99 O99 C97 C96 -169(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.104 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.145 _database_code_depnum_ccdc_archive 'CCDC 929144' ####################################################################### # # 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_? #============================================================================== _audit_creation_method 'form.cif (version 2.0)' #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== data_compound_[Pu(1)(Otf)3] #TrackingRef 'complexes_ChemSci.cif' _chemical_name_systematic ; 1,2-bis(2,2,4,4,5,5-hexakis(2,4,6-trimethylphenyl)- 3-methyl-2,4,5-trisila-1,3- distannabicylo[1.1.1]pentan)ethyne ; _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H24 N9 P S, C3 F9 O9 Pu S3, 3(C2 H3 N)' _chemical_formula_sum 'C30 H33 F9 N12 O9 P Pu S4' _chemical_formula_weight 1277.89 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' P P 0.1023 0.0942 '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' Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2866(4) _cell_length_b 13.3751(5) _cell_length_c 13.8490(5) _cell_angle_alpha 83.93 _cell_angle_beta 70.1560(10) _cell_angle_gamma 80.1230(10) _cell_volume 2277.64(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7875 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour green _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1246 _exptl_absorpt_coefficient_mu 1.765 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7875 _diffrn_reflns_av_R_equivalents 0.0079 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7093 _reflns_number_gt 6834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II (Bruker 2007)' _computing_cell_refinement 'APEX II (Bruker 2007)' _computing_data_reduction 'SAINT (Bruker 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep32 (Farrugia, 1997)' _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^)+(0.0250P)^2^+3.3899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7093 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Pu1 Pu 0.314107(7) 0.253935(8) 0.313337(8) 0.01353(4) Uani 1 1 d . . . S1 S 0.21052(6) -0.15911(6) 0.36752(7) 0.02456(18) Uani 1 1 d . . . S2 S 0.58257(7) 0.22091(9) 0.10062(8) 0.0449(3) Uani 1 1 d . . . S3 S 0.23681(6) 0.23370(6) 0.60079(6) 0.02312(17) Uani 1 1 d . . . S4 S 0.34003(5) 0.53403(6) 0.32288(6) 0.02214(17) Uani 1 1 d . . . P1 P 0.24043(5) -0.02175(6) 0.34539(6) 0.01736(17) Uani 1 1 d . . . F21 F 0.4908(3) 0.2023(3) -0.0337(2) 0.0970(13) Uani 1 1 d . . . F22 F 0.6626(3) 0.1784(3) -0.0917(2) 0.1018(13) Uani 1 1 d . . . F23 F 0.5791(5) 0.0687(3) 0.0062(4) 0.150(2) Uani 1 1 d . . . F31 F 0.23321(19) 0.40137(18) 0.6853(2) 0.0499(6) Uani 1 1 d . . . F32 F 0.39065(17) 0.3145(2) 0.62730(19) 0.0523(7) Uani 1 1 d . . . F33 F 0.2759(2) 0.2640(2) 0.76586(18) 0.0559(7) Uani 1 1 d . . . F41 F 0.47369(19) 0.5654(2) 0.13842(18) 0.0522(7) Uani 1 1 d . . . F42 F 0.47287(18) 0.66654(16) 0.24914(19) 0.0453(6) Uani 1 1 d . . . F43 F 0.55169(16) 0.51339(18) 0.2517(2) 0.0512(6) Uani 1 1 d . . . O21 O 0.48015(17) 0.2095(2) 0.17496(18) 0.0365(6) Uani 1 1 d . . . O22 O 0.5855(4) 0.3275(3) 0.0654(3) 0.1161(19) Uani 1 1 d . . . O23 O 0.6715(3) 0.1725(5) 0.1207(3) 0.146(3) Uani 1 1 d . . . O31 O 0.25382(16) 0.29115(17) 0.50231(17) 0.0230(5) Uani 1 1 d . . . O32 O 0.12478(18) 0.2341(2) 0.66083(19) 0.0347(6) Uani 1 1 d . . . O33 O 0.3050(2) 0.13690(19) 0.5952(2) 0.0373(6) Uani 1 1 d . . . O41 O 0.35033(16) 0.42777(16) 0.29946(17) 0.0222(5) Uani 1 1 d . . . O42 O 0.25833(18) 0.59915(18) 0.2911(2) 0.0352(6) Uani 1 1 d . . . O43 O 0.34261(19) 0.5455(2) 0.42326(19) 0.0361(6) Uani 1 1 d . . . N1 N 0.21273(19) 0.03593(19) 0.2418(2) 0.0197(6) Uani 1 1 d . . . N2 N 0.24265(18) 0.13234(19) 0.2091(2) 0.0189(6) Uani 1 1 d . . . N3 N 0.28926(18) 0.3293(2) 0.1384(2) 0.0200(6) Uani 1 1 d . . . N4 N 0.17165(18) 0.05212(19) 0.4443(2) 0.0192(6) Uani 1 1 d . . . N5 N 0.15146(18) 0.15508(19) 0.41761(19) 0.0172(5) Uani 1 1 d . . . N6 N 0.11748(17) 0.35353(19) 0.3565(2) 0.0187(6) Uani 1 1 d . . . N7 N 0.37082(18) -0.0155(2) 0.3248(2) 0.0209(6) Uani 1 1 d . . . N8 N 0.40003(17) 0.06766(19) 0.35458(19) 0.0179(5) Uani 1 1 d . . . N9 N 0.47725(18) 0.2362(2) 0.3817(2) 0.0208(6) Uani 1 1 d . . . C1 C 0.1391(3) -0.0010(3) 0.1998(3) 0.0325(9) Uani 1 1 d . . . H1A H 0.0718 0.0469 0.2136 0.037(3) Uiso 1 1 calc R . . H1B H 0.1230 -0.0677 0.2324 0.037(3) Uiso 1 1 calc R . . H1C H 0.1733 -0.0069 0.1255 0.037(3) Uiso 1 1 calc R . . C2 C 0.2074(2) 0.1804(2) 0.1393(2) 0.0227(7) Uani 1 1 d . . . H2 H 0.1627 0.1493 0.1142 0.019(5) Uiso 1 1 calc R . . C3 C 0.2333(2) 0.2811(2) 0.0969(2) 0.0215(7) Uani 1 1 d . . . C4 C 0.1998(3) 0.3236(3) 0.0157(3) 0.0318(8) Uani 1 1 d . . . H4 H 0.1578 0.2890 -0.0095 0.033(3) Uiso 1 1 calc R . . C5 C 0.2276(3) 0.4166(3) -0.0287(3) 0.0349(9) Uani 1 1 d . . . H5 H 0.2047 0.4471 -0.0843 0.033(3) Uiso 1 1 calc R . . C6 C 0.2892(2) 0.4643(3) 0.0095(3) 0.0275(8) Uani 1 1 d . . . H6 H 0.3113 0.5275 -0.0206 0.033(3) Uiso 1 1 calc R . . C7 C 0.3181(2) 0.4184(2) 0.0922(2) 0.0236(7) Uani 1 1 d . . . H7 H 0.3607 0.4517 0.1179 0.033(3) Uiso 1 1 calc R . . C8 C 0.1128(2) 0.0123(2) 0.5472(2) 0.0224(7) Uani 1 1 d . . . H8A H 0.1201 0.0524 0.5991 0.037(3) Uiso 1 1 calc R . . H8B H 0.1429 -0.0588 0.5566 0.037(3) Uiso 1 1 calc R . . H8C H 0.0362 0.0167 0.5546 0.037(3) Uiso 1 1 calc R . . C9 C 0.0623(2) 0.2082(2) 0.4677(2) 0.0192(7) Uani 1 1 d . . . H9 H 0.0123 0.1788 0.5258 0.019(5) Uiso 1 1 calc R . . C10 C 0.0389(2) 0.3133(2) 0.4347(2) 0.0192(7) Uani 1 1 d . . . C11 C -0.0634(2) 0.3684(2) 0.4767(3) 0.0246(7) Uani 1 1 d . . . H11 H -0.1165 0.3392 0.5320 0.033(3) Uiso 1 1 calc R . . C12 C -0.0875(2) 0.4649(3) 0.4381(3) 0.0276(8) Uani 1 1 d . . . H12 H -0.1569 0.5032 0.4665 0.033(3) Uiso 1 1 calc R . . C13 C -0.0088(2) 0.5052(3) 0.3572(3) 0.0263(8) Uani 1 1 d . . . H13 H -0.0235 0.5712 0.3277 0.033(3) Uiso 1 1 calc R . . C14 C 0.0922(2) 0.4470(2) 0.3199(2) 0.0220(7) Uani 1 1 d . . . H14 H 0.1464 0.4756 0.2651 0.033(3) Uiso 1 1 calc R . . C15 C 0.4547(2) -0.0959(3) 0.2714(3) 0.0330(9) Uani 1 1 d . . . H15A H 0.5142 -0.0654 0.2205 0.037(3) Uiso 1 1 calc R . . H15B H 0.4241 -0.1368 0.2367 0.037(3) Uiso 1 1 calc R . . H15C H 0.4820 -0.1395 0.3213 0.037(3) Uiso 1 1 calc R . . C16 C 0.4945(2) 0.0571(2) 0.3636(2) 0.0208(7) Uani 1 1 d . . . H16 H 0.5385 -0.0074 0.3553 0.019(5) Uiso 1 1 calc R . . C17 C 0.5343(2) 0.1435(2) 0.3866(2) 0.0199(7) Uani 1 1 d . . . C18 C 0.6284(2) 0.1280(3) 0.4121(3) 0.0272(8) Uani 1 1 d . . . H18 H 0.6671 0.0616 0.4146 0.033(3) Uiso 1 1 calc R . . C19 C 0.6651(2) 0.2111(3) 0.4338(3) 0.0313(8) Uani 1 1 d . . . H19 H 0.7301 0.2028 0.4499 0.033(3) Uiso 1 1 calc R . . C20 C 0.6059(3) 0.3056(3) 0.4318(3) 0.0309(8) Uani 1 1 d . . . H20 H 0.6285 0.3636 0.4477 0.033(3) Uiso 1 1 calc R . . C21 C 0.5124(2) 0.3147(3) 0.4060(3) 0.0268(8) Uani 1 1 d . . . H21 H 0.4712 0.3801 0.4056 0.033(3) Uiso 1 1 calc R . . C22 C 0.5757(4) 0.1683(4) -0.0099(4) 0.0612(14) Uani 1 1 d . . . C23 C 0.2871(3) 0.3083(3) 0.6734(3) 0.0320(8) Uani 1 1 d . . . C24 C 0.4670(3) 0.5715(3) 0.2354(3) 0.0310(8) Uani 1 1 d . . . N100 N 0.0029(4) 0.4018(4) 0.8967(4) 0.0689(12) Uani 1 1 d . . . C100 C -0.0479(3) 0.3480(4) 0.8834(3) 0.0481(11) Uani 1 1 d . . . C101 C -0.1130(4) 0.2803(4) 0.8650(4) 0.0644(14) Uani 1 1 d . . . H10A H -0.1750 0.3204 0.8490 0.132(16) Uiso 1 1 calc R . . H10B H -0.1390 0.2359 0.9265 0.132(16) Uiso 1 1 calc R . . H10C H -0.0691 0.2387 0.8069 0.132(16) Uiso 1 1 calc R . . N200 N 0.0644(4) 0.1182(4) 0.9918(4) 0.0695(13) Uani 1 1 d . . . C200 C 0.1021(4) 0.0706(4) 0.9213(4) 0.0518(12) Uani 1 1 d . . . C201 C 0.1498(4) 0.0103(4) 0.8310(4) 0.0657(14) Uani 1 1 d . . . H20A H 0.2160 -0.0327 0.8350 0.135(16) Uiso 1 1 calc R . . H20B H 0.1672 0.0556 0.7690 0.135(16) Uiso 1 1 calc R . . H20C H 0.0982 -0.0327 0.8280 0.135(16) Uiso 1 1 calc R . . N300 N 0.9376(3) 0.2039(3) 0.2873(3) 0.0574(10) Uani 1 1 d . . . C300 C 0.9073(4) 0.2664(4) 0.2384(4) 0.0519(12) Uani 1 1 d . . . C301 C 0.8660(6) 0.3478(5) 0.1773(5) 0.103(2) Uani 1 1 d . . . H30A H 0.8336 0.4074 0.2186 0.20(3) Uiso 1 1 calc R . . H30B H 0.8111 0.3250 0.1555 0.20(3) Uiso 1 1 calc R . . H30C H 0.9255 0.3657 0.1165 0.20(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pu1 0.01280(5) 0.01121(7) 0.01654(7) 0.00003(4) -0.00506(4) -0.00155(4) S1 0.0260(3) 0.0131(4) 0.0335(5) 0.0013(3) -0.0077(3) -0.0057(3) S2 0.0242(4) 0.0738(8) 0.0331(5) -0.0129(5) 0.0010(3) -0.0126(4) S3 0.0274(4) 0.0208(5) 0.0204(4) -0.0027(3) -0.0075(3) -0.0013(3) S4 0.0211(3) 0.0170(4) 0.0277(5) -0.0041(3) -0.0059(3) -0.0037(3) P1 0.0167(3) 0.0120(4) 0.0226(4) -0.0001(3) -0.0055(3) -0.0023(3) F21 0.0641(19) 0.178(4) 0.052(2) -0.040(2) -0.0198(15) -0.005(2) F22 0.0647(19) 0.174(4) 0.0467(18) -0.044(2) 0.0189(14) -0.016(2) F23 0.219(6) 0.070(3) 0.145(4) -0.048(3) -0.017(4) -0.038(3) F31 0.0649(15) 0.0314(15) 0.0644(18) -0.0226(13) -0.0367(13) 0.0082(11) F32 0.0365(11) 0.0797(19) 0.0504(15) -0.0185(13) -0.0205(10) -0.0125(11) F33 0.0795(18) 0.0670(19) 0.0291(15) -0.0019(13) -0.0310(12) -0.0045(13) F41 0.0552(14) 0.0661(18) 0.0340(14) -0.0017(12) 0.0002(10) -0.0367(12) F42 0.0519(13) 0.0249(13) 0.0657(16) 0.0025(11) -0.0217(11) -0.0208(10) F43 0.0241(10) 0.0415(15) 0.0805(18) 0.0081(13) -0.0101(10) -0.0065(9) O21 0.0245(11) 0.0553(18) 0.0228(13) 0.0034(12) -0.0034(9) 0.0000(10) O22 0.160(5) 0.090(3) 0.094(3) -0.002(3) 0.000(3) -0.095(3) O23 0.043(2) 0.302(8) 0.075(3) -0.050(4) -0.0263(19) 0.061(3) O31 0.0256(10) 0.0232(13) 0.0218(12) -0.0014(10) -0.0100(8) -0.0032(8) O32 0.0307(12) 0.0426(17) 0.0275(14) -0.0033(12) -0.0032(9) -0.0088(10) O33 0.0510(15) 0.0217(15) 0.0336(15) -0.0031(12) -0.0117(11) 0.0062(10) O41 0.0251(10) 0.0152(13) 0.0271(13) -0.0014(10) -0.0085(8) -0.0055(8) O42 0.0320(12) 0.0211(14) 0.0545(17) -0.0051(12) -0.0187(11) 0.0019(9) O43 0.0408(13) 0.0405(17) 0.0292(15) -0.0103(12) -0.0086(10) -0.0122(11) N1 0.0265(12) 0.0113(14) 0.0245(15) 0.0001(11) -0.0113(10) -0.0056(9) N2 0.0209(11) 0.0141(15) 0.0214(15) -0.0002(11) -0.0059(9) -0.0044(9) N3 0.0194(11) 0.0179(15) 0.0219(15) -0.0004(12) -0.0060(9) -0.0030(9) N4 0.0211(11) 0.0119(15) 0.0205(14) 0.0026(11) -0.0032(9) -0.0010(9) N5 0.0197(11) 0.0113(15) 0.0207(14) 0.0007(11) -0.0071(9) -0.0021(9) N6 0.0183(11) 0.0151(15) 0.0221(15) 0.0008(11) -0.0071(9) -0.0015(9) N7 0.0170(11) 0.0159(15) 0.0293(16) -0.0045(12) -0.0070(9) -0.0003(9) N8 0.0176(11) 0.0151(15) 0.0204(14) 0.0000(11) -0.0057(9) -0.0022(9) N9 0.0207(11) 0.0205(16) 0.0230(15) -0.0021(12) -0.0105(9) -0.0005(9) C1 0.0439(18) 0.024(2) 0.043(2) 0.0066(17) -0.0289(16) -0.0148(15) C2 0.0287(14) 0.0215(19) 0.0227(18) 0.0010(15) -0.0134(12) -0.0073(12) C3 0.0235(14) 0.0189(18) 0.0219(18) -0.0003(14) -0.0074(11) -0.0032(11) C4 0.0448(19) 0.030(2) 0.030(2) 0.0059(17) -0.0244(15) -0.0127(15) C5 0.048(2) 0.033(2) 0.030(2) 0.0106(18) -0.0230(16) -0.0103(16) C6 0.0333(16) 0.022(2) 0.0246(19) 0.0064(15) -0.0077(13) -0.0056(13) C7 0.0271(14) 0.0204(19) 0.0236(18) 0.0011(15) -0.0082(12) -0.0059(12) C8 0.0251(14) 0.0190(19) 0.0211(18) 0.0045(14) -0.0064(11) -0.0036(11) C9 0.0179(12) 0.0155(18) 0.0223(17) 0.0000(13) -0.0044(10) -0.0025(11) C10 0.0178(12) 0.0159(18) 0.0229(17) -0.0018(13) -0.0051(11) -0.0030(11) C11 0.0197(13) 0.0185(19) 0.0294(19) -0.0004(15) -0.0016(11) 0.0004(11) C12 0.0205(14) 0.021(2) 0.036(2) -0.0023(16) -0.0051(12) 0.0048(11) C13 0.0247(14) 0.0153(19) 0.036(2) 0.0028(15) -0.0103(13) 0.0020(11) C14 0.0233(14) 0.0160(19) 0.0261(18) 0.0038(14) -0.0088(11) -0.0032(11) C15 0.0221(15) 0.028(2) 0.046(2) -0.0176(17) -0.0047(13) -0.0003(12) C16 0.0182(13) 0.0152(18) 0.0276(18) 0.0006(14) -0.0077(11) 0.0013(10) C17 0.0190(13) 0.0188(18) 0.0218(17) -0.0001(14) -0.0071(11) -0.0020(11) C18 0.0235(14) 0.022(2) 0.038(2) 0.0006(16) -0.0153(13) 0.0009(12) C19 0.0248(15) 0.035(2) 0.041(2) -0.0017(17) -0.0196(14) -0.0041(13) C20 0.0343(17) 0.027(2) 0.040(2) -0.0048(17) -0.0209(15) -0.0069(14) C21 0.0273(15) 0.021(2) 0.036(2) -0.0041(16) -0.0162(13) -0.0004(12) C22 0.051(3) 0.073(4) 0.050(3) -0.025(3) 0.000(2) -0.005(2) C23 0.0352(17) 0.033(2) 0.030(2) -0.0073(18) -0.0158(14) 0.0032(14) C24 0.0297(16) 0.026(2) 0.038(2) 0.0010(16) -0.0084(14) -0.0128(13) N100 0.065(3) 0.084(4) 0.063(3) -0.006(3) -0.028(2) -0.011(2) C100 0.042(2) 0.060(3) 0.038(3) 0.004(2) -0.0136(17) 0.0021(19) C101 0.055(3) 0.068(4) 0.074(4) 0.007(3) -0.027(2) -0.014(2) N200 0.102(4) 0.068(3) 0.060(3) 0.005(3) -0.045(3) -0.038(3) C200 0.068(3) 0.052(3) 0.054(3) 0.020(3) -0.041(2) -0.030(2) C201 0.078(3) 0.071(4) 0.055(3) 0.009(3) -0.030(3) -0.018(3) N300 0.053(2) 0.057(3) 0.058(3) 0.002(2) -0.0170(18) -0.0015(18) C300 0.057(3) 0.051(3) 0.042(3) -0.003(2) -0.011(2) -0.005(2) C301 0.134(6) 0.086(5) 0.077(5) 0.026(4) -0.045(4) 0.017(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 Pu1 O21 2.411(2) . ? Pu1 O41 2.429(2) . ? Pu1 O31 2.541(2) . ? Pu1 N9 2.611(2) . ? Pu1 N6 2.621(2) . ? Pu1 N3 2.629(3) . ? Pu1 N5 2.638(2) . ? Pu1 N8 2.646(3) . ? Pu1 N2 2.754(2) . ? S1 P1 1.9173(11) . ? S2 O23 1.347(4) . ? S2 O21 1.422(2) . ? S2 O22 1.460(4) . ? S2 C22 1.787(5) . ? S3 O32 1.437(2) . ? S3 O33 1.440(3) . ? S3 O31 1.459(2) . ? S3 C23 1.830(4) . ? S4 O43 1.427(3) . ? S4 O42 1.432(2) . ? S4 O41 1.464(2) . ? S4 C24 1.827(3) . ? P1 N7 1.673(2) . ? P1 N4 1.678(3) . ? P1 N1 1.678(3) . ? F21 C22 1.277(6) . ? F22 C22 1.329(5) . ? F23 C22 1.323(7) . ? F31 C23 1.322(4) . ? F32 C23 1.319(4) . ? F33 C23 1.324(4) . ? F41 C24 1.326(4) . ? F42 C24 1.324(4) . ? F43 C24 1.325(4) . ? N1 N2 1.398(3) . ? N1 C1 1.466(4) . ? N2 C2 1.281(4) . ? N3 C7 1.343(4) . ? N3 C3 1.353(4) . ? N4 N5 1.392(4) . ? N4 C8 1.466(4) . ? N5 C9 1.283(4) . ? N6 C14 1.331(4) . ? N6 C10 1.362(3) . ? N7 N8 1.382(3) . ? N7 C15 1.465(4) . ? N8 C16 1.285(4) . ? N9 C21 1.335(4) . ? N9 C17 1.347(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.461(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(5) . ? C4 C5 1.380(5) . ? C4 H4 0.9500 . ? C5 C6 1.378(5) . ? C5 H5 0.9500 . ? C6 C7 1.381(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.447(4) . ? C9 H9 0.9500 . ? C10 C11 1.393(4) . ? C11 C12 1.371(5) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 C14 1.390(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.455(4) . ? C16 H16 0.9500 . ? C17 C18 1.388(4) . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.372(5) . ? C19 H19 0.9500 . ? C20 C21 1.388(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? N100 C100 1.134(6) . ? C100 C101 1.450(7) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? N200 C200 1.140(7) . ? C200 C201 1.455(8) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? N300 C300 1.127(6) . ? C300 C301 1.455(8) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? 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 O21 Pu1 O41 90.37(8) . . ? O21 Pu1 O31 138.57(7) . . ? O41 Pu1 O31 79.70(7) . . ? O21 Pu1 N9 70.65(8) . . ? O41 Pu1 N9 77.19(8) . . ? O31 Pu1 N9 67.93(7) . . ? O21 Pu1 N6 143.65(8) . . ? O41 Pu1 N6 79.31(7) . . ? O31 Pu1 N6 74.04(7) . . ? N9 Pu1 N6 138.07(8) . . ? O21 Pu1 N3 70.85(8) . . ? O41 Pu1 N3 75.38(8) . . ? O31 Pu1 N3 141.48(7) . . ? N9 Pu1 N3 131.92(7) . . ? N6 Pu1 N3 72.83(8) . . ? O21 Pu1 N5 133.32(9) . . ? O41 Pu1 N5 135.92(7) . . ? O31 Pu1 N5 70.42(7) . . ? N9 Pu1 N5 117.76(8) . . ? N6 Pu1 N5 62.00(8) . . ? N3 Pu1 N5 109.45(7) . . ? O21 Pu1 N8 71.73(8) . . ? O41 Pu1 N8 139.57(7) . . ? O31 Pu1 N8 90.18(7) . . ? N9 Pu1 N8 62.83(8) . . ? N6 Pu1 N8 135.35(7) . . ? N3 Pu1 N8 127.54(8) . . ? N5 Pu1 N8 73.38(7) . . ? O21 Pu1 N2 80.67(8) . . ? O41 Pu1 N2 137.97(8) . . ? O31 Pu1 N2 131.77(7) . . ? N9 Pu1 N2 135.14(8) . . ? N6 Pu1 N2 84.08(7) . . ? N3 Pu1 N2 62.85(8) . . ? N5 Pu1 N2 61.36(7) . . ? N8 Pu1 N2 75.95(8) . . ? O23 S2 O21 117.8(3) . . ? O23 S2 O22 115.4(4) . . ? O21 S2 O22 109.8(2) . . ? O23 S2 C22 108.2(3) . . ? O21 S2 C22 102.60(19) . . ? O22 S2 C22 100.7(3) . . ? O32 S3 O33 116.03(16) . . ? O32 S3 O31 113.68(14) . . ? O33 S3 O31 114.13(14) . . ? O32 S3 C23 104.03(16) . . ? O33 S3 C23 103.42(16) . . ? O31 S3 C23 103.48(15) . . ? O43 S4 O42 117.25(16) . . ? O43 S4 O41 113.18(15) . . ? O42 S4 O41 113.12(14) . . ? O43 S4 C24 104.78(16) . . ? O42 S4 C24 104.24(16) . . ? O41 S4 C24 102.19(15) . . ? N7 P1 N4 105.14(13) . . ? N7 P1 N1 106.23(13) . . ? N4 P1 N1 106.84(13) . . ? N7 P1 S1 112.05(10) . . ? N4 P1 S1 114.34(9) . . ? N1 P1 S1 111.67(10) . . ? S2 O21 Pu1 158.09(19) . . ? S3 O31 Pu1 137.68(13) . . ? S4 O41 Pu1 160.43(13) . . ? N2 N1 C1 119.1(2) . . ? N2 N1 P1 117.91(19) . . ? C1 N1 P1 121.6(2) . . ? C2 N2 N1 116.5(2) . . ? C2 N2 Pu1 113.9(2) . . ? N1 N2 Pu1 126.88(18) . . ? C7 N3 C3 116.9(3) . . ? C7 N3 Pu1 124.6(2) . . ? C3 N3 Pu1 118.08(19) . . ? N5 N4 C8 119.8(2) . . ? N5 N4 P1 115.02(19) . . ? C8 N4 P1 123.5(2) . . ? C9 N5 N4 119.7(2) . . ? C9 N5 Pu1 117.23(19) . . ? N4 N5 Pu1 119.76(15) . . ? C14 N6 C10 117.5(2) . . ? C14 N6 Pu1 124.80(17) . . ? C10 N6 Pu1 116.77(19) . . ? N8 N7 C15 119.7(2) . . ? N8 N7 P1 120.08(19) . . ? C15 N7 P1 120.2(2) . . ? C16 N8 N7 117.2(3) . . ? C16 N8 Pu1 116.9(2) . . ? N7 N8 Pu1 120.33(17) . . ? C21 N9 C17 117.4(3) . . ? C21 N9 Pu1 124.0(2) . . ? C17 N9 Pu1 118.51(19) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C3 122.5(3) . . ? N2 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? N3 C3 C4 122.4(3) . . ? N3 C3 C2 119.0(3) . . ? C4 C3 C2 118.6(3) . . ? C5 C4 C3 119.6(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 118.6(3) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 118.7(3) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? N3 C7 C6 123.6(3) . . ? N3 C7 H7 118.2 . . ? C6 C7 H7 118.2 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 C10 119.2(3) . . ? N5 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N6 C10 C11 121.5(3) . . ? N6 C10 C9 117.7(2) . . ? C11 C10 C9 120.6(3) . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 118.7(3) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C12 C13 C14 118.5(3) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? N6 C14 C13 123.8(3) . . ? N6 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? N7 C15 H15A 109.5 . . ? N7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 C17 120.4(3) . . ? N8 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? N9 C17 C18 122.6(3) . . ? N9 C17 C16 117.7(3) . . ? C18 C17 C16 119.7(3) . . ? C19 C18 C17 118.8(3) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 C18 119.0(3) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 118.7(3) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? N9 C21 C20 123.4(3) . . ? N9 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? F21 C22 F23 107.3(5) . . ? F21 C22 F22 109.2(5) . . ? F23 C22 F22 103.5(4) . . ? F21 C22 S2 115.0(3) . . ? F23 C22 S2 109.1(4) . . ? F22 C22 S2 112.0(4) . . ? F32 C23 F31 108.5(3) . . ? F32 C23 F33 107.7(3) . . ? F31 C23 F33 108.0(3) . . ? F32 C23 S3 111.1(2) . . ? F31 C23 S3 111.7(2) . . ? F33 C23 S3 109.7(3) . . ? F42 C24 F43 107.6(3) . . ? F42 C24 F41 108.1(3) . . ? F43 C24 F41 108.7(3) . . ? F42 C24 S4 110.2(2) . . ? F43 C24 S4 111.5(2) . . ? F41 C24 S4 110.6(2) . . ? N100 C100 C101 179.1(5) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N200 C200 C201 179.6(6) . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? N300 C300 C301 178.7(6) . . ? C300 C301 H30A 109.5 . . ? C300 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C300 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O23 S2 O21 Pu1 103.0(5) . . . . ? O22 S2 O21 Pu1 -31.9(5) . . . . ? C22 S2 O21 Pu1 -138.4(4) . . . . ? O41 Pu1 O21 S2 9.7(4) . . . . ? O31 Pu1 O21 S2 -65.0(5) . . . . ? N9 Pu1 O21 S2 -66.5(4) . . . . ? N6 Pu1 O21 S2 82.0(5) . . . . ? N3 Pu1 O21 S2 84.1(4) . . . . ? N5 Pu1 O21 S2 -176.9(4) . . . . ? N8 Pu1 O21 S2 -133.4(4) . . . . ? N2 Pu1 O21 S2 148.5(4) . . . . ? O32 S3 O31 Pu1 -106.94(19) . . . . ? O33 S3 O31 Pu1 29.3(2) . . . . ? C23 S3 O31 Pu1 140.89(18) . . . . ? O21 Pu1 O31 S3 -80.2(2) . . . . ? O41 Pu1 O31 S3 -158.91(18) . . . . ? N9 Pu1 O31 S3 -78.67(18) . . . . ? N6 Pu1 O31 S3 119.37(18) . . . . ? N3 Pu1 O31 S3 150.91(15) . . . . ? N5 Pu1 O31 S3 53.99(17) . . . . ? N8 Pu1 O31 S3 -18.27(17) . . . . ? N2 Pu1 O31 S3 52.9(2) . . . . ? O43 S4 O41 Pu1 56.5(4) . . . . ? O42 S4 O41 Pu1 -79.9(4) . . . . ? C24 S4 O41 Pu1 168.6(4) . . . . ? O21 Pu1 O41 S4 -172.2(4) . . . . ? O31 Pu1 O41 S4 -32.6(4) . . . . ? N9 Pu1 O41 S4 -102.1(4) . . . . ? N6 Pu1 O41 S4 42.9(4) . . . . ? N3 Pu1 O41 S4 117.7(4) . . . . ? N5 Pu1 O41 S4 14.7(5) . . . . ? N8 Pu1 O41 S4 -110.6(4) . . . . ? N2 Pu1 O41 S4 111.4(4) . . . . ? N7 P1 N1 N2 -50.1(2) . . . . ? N4 P1 N1 N2 61.7(2) . . . . ? S1 P1 N1 N2 -172.55(17) . . . . ? N7 P1 N1 C1 143.4(3) . . . . ? N4 P1 N1 C1 -104.8(3) . . . . ? S1 P1 N1 C1 20.9(3) . . . . ? C1 N1 N2 C2 -3.7(4) . . . . ? P1 N1 N2 C2 -170.6(2) . . . . ? C1 N1 N2 Pu1 156.4(2) . . . . ? P1 N1 N2 Pu1 -10.5(3) . . . . ? O21 Pu1 N2 C2 -89.2(2) . . . . ? O41 Pu1 N2 C2 -9.2(2) . . . . ? O31 Pu1 N2 C2 120.1(2) . . . . ? N9 Pu1 N2 C2 -139.4(2) . . . . ? N6 Pu1 N2 C2 57.6(2) . . . . ? N3 Pu1 N2 C2 -16.07(19) . . . . ? N5 Pu1 N2 C2 118.9(2) . . . . ? N8 Pu1 N2 C2 -162.6(2) . . . . ? O21 Pu1 N2 N1 110.3(2) . . . . ? O41 Pu1 N2 N1 -169.67(18) . . . . ? O31 Pu1 N2 N1 -40.4(2) . . . . ? N9 Pu1 N2 N1 60.1(2) . . . . ? N6 Pu1 N2 N1 -102.8(2) . . . . ? N3 Pu1 N2 N1 -176.6(2) . . . . ? N5 Pu1 N2 N1 -41.60(19) . . . . ? N8 Pu1 N2 N1 36.9(2) . . . . ? O21 Pu1 N3 C7 -84.5(2) . . . . ? O41 Pu1 N3 C7 11.1(2) . . . . ? O31 Pu1 N3 C7 62.4(3) . . . . ? N9 Pu1 N3 C7 -46.1(3) . . . . ? N6 Pu1 N3 C7 94.2(2) . . . . ? N5 Pu1 N3 C7 145.1(2) . . . . ? N8 Pu1 N3 C7 -131.2(2) . . . . ? N2 Pu1 N3 C7 -173.7(2) . . . . ? O21 Pu1 N3 C3 102.9(2) . . . . ? O41 Pu1 N3 C3 -161.5(2) . . . . ? O31 Pu1 N3 C3 -110.2(2) . . . . ? N9 Pu1 N3 C3 141.3(2) . . . . ? N6 Pu1 N3 C3 -78.4(2) . . . . ? N5 Pu1 N3 C3 -27.5(2) . . . . ? N8 Pu1 N3 C3 56.2(2) . . . . ? N2 Pu1 N3 C3 13.74(19) . . . . ? N7 P1 N4 N5 84.9(2) . . . . ? N1 P1 N4 N5 -27.7(2) . . . . ? S1 P1 N4 N5 -151.81(15) . . . . ? N7 P1 N4 C8 -110.1(2) . . . . ? N1 P1 N4 C8 137.3(2) . . . . ? S1 P1 N4 C8 13.2(3) . . . . ? C8 N4 N5 C9 -21.1(4) . . . . ? P1 N4 N5 C9 144.6(2) . . . . ? C8 N4 N5 Pu1 137.9(2) . . . . ? P1 N4 N5 Pu1 -56.5(2) . . . . ? O21 Pu1 N5 C9 -161.8(2) . . . . ? O41 Pu1 N5 C9 8.7(3) . . . . ? O31 Pu1 N5 C9 58.9(2) . . . . ? N9 Pu1 N5 C9 109.2(2) . . . . ? N6 Pu1 N5 C9 -23.0(2) . . . . ? N3 Pu1 N5 C9 -80.2(2) . . . . ? N8 Pu1 N5 C9 155.2(2) . . . . ? N2 Pu1 N5 C9 -122.1(2) . . . . ? O21 Pu1 N5 N4 38.7(2) . . . . ? O41 Pu1 N5 N4 -150.78(18) . . . . ? O31 Pu1 N5 N4 -100.6(2) . . . . ? N9 Pu1 N5 N4 -50.2(2) . . . . ? N6 Pu1 N5 N4 177.5(2) . . . . ? N3 Pu1 N5 N4 120.4(2) . . . . ? N8 Pu1 N5 N4 -4.3(2) . . . . ? N2 Pu1 N5 N4 78.5(2) . . . . ? O21 Pu1 N6 C14 -45.8(3) . . . . ? O41 Pu1 N6 C14 30.0(2) . . . . ? O31 Pu1 N6 C14 112.2(3) . . . . ? N9 Pu1 N6 C14 86.8(3) . . . . ? N3 Pu1 N6 C14 -47.9(2) . . . . ? N5 Pu1 N6 C14 -171.9(3) . . . . ? N8 Pu1 N6 C14 -174.4(2) . . . . ? N2 Pu1 N6 C14 -111.2(3) . . . . ? O21 Pu1 N6 C10 145.6(2) . . . . ? O41 Pu1 N6 C10 -138.6(2) . . . . ? O31 Pu1 N6 C10 -56.4(2) . . . . ? N9 Pu1 N6 C10 -81.8(2) . . . . ? N3 Pu1 N6 C10 143.6(2) . . . . ? N5 Pu1 N6 C10 19.6(2) . . . . ? N8 Pu1 N6 C10 17.1(3) . . . . ? N2 Pu1 N6 C10 80.2(2) . . . . ? N4 P1 N7 N8 -24.7(3) . . . . ? N1 P1 N7 N8 88.4(2) . . . . ? S1 P1 N7 N8 -149.4(2) . . . . ? N4 P1 N7 C15 157.9(3) . . . . ? N1 P1 N7 C15 -89.0(3) . . . . ? S1 P1 N7 C15 33.2(3) . . . . ? C15 N7 N8 C16 -21.3(4) . . . . ? P1 N7 N8 C16 161.3(2) . . . . ? C15 N7 N8 Pu1 131.7(3) . . . . ? P1 N7 N8 Pu1 -45.7(3) . . . . ? O21 Pu1 N8 C16 60.6(2) . . . . ? O41 Pu1 N8 C16 -7.3(3) . . . . ? O31 Pu1 N8 C16 -81.5(2) . . . . ? N9 Pu1 N8 C16 -16.5(2) . . . . ? N6 Pu1 N8 C16 -148.6(2) . . . . ? N3 Pu1 N8 C16 107.0(2) . . . . ? N5 Pu1 N8 C16 -150.9(2) . . . . ? N2 Pu1 N8 C16 145.2(2) . . . . ? O21 Pu1 N8 N7 -92.5(2) . . . . ? O41 Pu1 N8 N7 -160.35(17) . . . . ? O31 Pu1 N8 N7 125.45(19) . . . . ? N9 Pu1 N8 N7 -169.6(2) . . . . ? N6 Pu1 N8 N7 58.3(2) . . . . ? N3 Pu1 N8 N7 -46.1(2) . . . . ? N5 Pu1 N8 N7 55.98(19) . . . . ? N2 Pu1 N8 N7 -7.86(18) . . . . ? O21 Pu1 N9 C21 107.8(3) . . . . ? O41 Pu1 N9 C21 12.8(2) . . . . ? O31 Pu1 N9 C21 -71.1(2) . . . . ? N6 Pu1 N9 C21 -44.6(3) . . . . ? N3 Pu1 N9 C21 69.3(3) . . . . ? N5 Pu1 N9 C21 -122.6(2) . . . . ? N8 Pu1 N9 C21 -173.3(3) . . . . ? N2 Pu1 N9 C21 161.2(2) . . . . ? O21 Pu1 N9 C17 -67.6(2) . . . . ? O41 Pu1 N9 C17 -162.6(2) . . . . ? O31 Pu1 N9 C17 113.5(2) . . . . ? N6 Pu1 N9 C17 139.9(2) . . . . ? N3 Pu1 N9 C17 -106.1(2) . . . . ? N5 Pu1 N9 C17 61.9(2) . . . . ? N8 Pu1 N9 C17 11.2(2) . . . . ? N2 Pu1 N9 C17 -14.2(3) . . . . ? N1 N2 C2 C3 -179.2(3) . . . . ? Pu1 N2 C2 C3 18.2(4) . . . . ? C7 N3 C3 C4 -4.7(4) . . . . ? Pu1 N3 C3 C4 168.5(3) . . . . ? C7 N3 C3 C2 175.3(3) . . . . ? Pu1 N3 C3 C2 -11.5(3) . . . . ? N2 C2 C3 N3 -5.5(5) . . . . ? N2 C2 C3 C4 174.4(3) . . . . ? N3 C3 C4 C5 2.9(5) . . . . ? C2 C3 C4 C5 -177.1(3) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? C4 C5 C6 C7 -1.7(5) . . . . ? C3 N3 C7 C6 3.3(4) . . . . ? Pu1 N3 C7 C6 -169.3(2) . . . . ? C5 C6 C7 N3 -0.2(5) . . . . ? N4 N5 C9 C10 -175.7(3) . . . . ? Pu1 N5 C9 C10 24.9(4) . . . . ? C14 N6 C10 C11 -1.5(5) . . . . ? Pu1 N6 C10 C11 168.0(2) . . . . ? C14 N6 C10 C9 173.8(3) . . . . ? Pu1 N6 C10 C9 -16.7(3) . . . . ? N5 C9 C10 N6 -5.5(4) . . . . ? N5 C9 C10 C11 169.8(3) . . . . ? N6 C10 C11 C12 1.1(5) . . . . ? C9 C10 C11 C12 -174.0(3) . . . . ? C10 C11 C12 C13 0.4(5) . . . . ? C11 C12 C13 C14 -1.5(5) . . . . ? C10 N6 C14 C13 0.3(5) . . . . ? Pu1 N6 C14 C13 -168.2(2) . . . . ? C12 C13 C14 N6 1.1(5) . . . . ? N7 N8 C16 C17 175.1(3) . . . . ? Pu1 N8 C16 C17 21.1(4) . . . . ? C21 N9 C17 C18 -2.3(5) . . . . ? Pu1 N9 C17 C18 173.5(2) . . . . ? C21 N9 C17 C16 177.9(3) . . . . ? Pu1 N9 C17 C16 -6.3(3) . . . . ? N8 C16 C17 N9 -10.3(4) . . . . ? N8 C16 C17 C18 169.9(3) . . . . ? N9 C17 C18 C19 0.3(5) . . . . ? C16 C17 C18 C19 -179.9(3) . . . . ? C17 C18 C19 C20 1.5(5) . . . . ? C18 C19 C20 C21 -1.2(5) . . . . ? C17 N9 C21 C20 2.6(5) . . . . ? Pu1 N9 C21 C20 -172.9(3) . . . . ? C19 C20 C21 N9 -0.9(6) . . . . ? O23 S2 C22 F21 175.3(5) . . . . ? O21 S2 C22 F21 50.1(5) . . . . ? O22 S2 C22 F21 -63.3(5) . . . . ? O23 S2 C22 F23 54.7(5) . . . . ? O21 S2 C22 F23 -70.5(4) . . . . ? O22 S2 C22 F23 176.2(4) . . . . ? O23 S2 C22 F22 -59.3(6) . . . . ? O21 S2 C22 F22 175.6(4) . . . . ? O22 S2 C22 F22 62.2(5) . . . . ? O32 S3 C23 F32 179.8(3) . . . . ? O33 S3 C23 F32 58.2(3) . . . . ? O31 S3 C23 F32 -61.1(3) . . . . ? O32 S3 C23 F31 -58.9(3) . . . . ? O33 S3 C23 F31 179.5(3) . . . . ? O31 S3 C23 F31 60.2(3) . . . . ? O32 S3 C23 F33 60.8(3) . . . . ? O33 S3 C23 F33 -60.9(3) . . . . ? O31 S3 C23 F33 179.8(2) . . . . ? O43 S4 C24 F42 -59.6(3) . . . . ? O42 S4 C24 F42 64.1(3) . . . . ? O41 S4 C24 F42 -177.9(2) . . . . ? O43 S4 C24 F43 59.8(3) . . . . ? O42 S4 C24 F43 -176.5(3) . . . . ? O41 S4 C24 F43 -58.5(3) . . . . ? O43 S4 C24 F41 -179.1(3) . . . . ? O42 S4 C24 F41 -55.4(3) . . . . ? O41 S4 C24 F41 62.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.715 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.715 _refine_diff_density_max 1.025 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.072 _database_code_depnum_ccdc_archive 'CCDC 929145'