# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Brian Skelton' _publ_contact_author_email brian.skelton@uwa.edu.au loop_ _publ_author_name 'Irene Ling' 'Yatimah Alias' 'Brian W. Skelton' 'Colin L. Raston' data_110713a _database_code_depnum_ccdc_archive 'CCDC 851781' #TrackingRef '7924_web_deposit_cif_file_0_BrianSkelton_1320129951.110713a.cif' _audit_creation_date 2011-08-04T16:34:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C118 H152 N4 O64 P2 S8 Y2' _chemical_formula_moiety ; 2(C28 H20 O16 S4), C12 H40 N4 O16 Y2, 2(C25 H22 O P), 14(H2 O) ; _chemical_formula_weight 3146.68 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2709(5) _cell_length_b 14.4188(4) _cell_length_c 19.2095(6) _cell_angle_alpha 98.648(2) _cell_angle_beta 95.949(3) _cell_angle_gamma 91.422(3) _cell_volume 3611.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18378 _cell_measurement_theta_min 3.567 _cell_measurement_theta_max 31.1267 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour light_brown _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.72 _exptl_crystal_size_min 0.61 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1636 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 2 -1 0.1937 -1 1 0 0.2454 -1 -1 0 0.3041 -13 -10 -8 0.2638 1 0 0 0.2523 0 -1 -2 0.3289 0 0 1 0.4472 0 0 -1 0.3493 -17 -6 12 0.3674 6 16 -18 0.2395 2 0 -1 0.2578 -13 15 4 0.2586 0 1 0 0.2763 3 -2 0 0.4185 -2 -20 5 0.4739 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_T_max 0.664 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0193073329 _diffrn_orient_matrix_ub_12 0.0424831565 _diffrn_orient_matrix_ub_13 0.0212971642 _diffrn_orient_matrix_ub_21 0.0500825548 _diffrn_orient_matrix_ub_22 -0.012533994 _diffrn_orient_matrix_ub_23 -0.0060539011 _diffrn_orient_matrix_ub_31 -0.0037009732 _diffrn_orient_matrix_ub_32 0.0227424685 _diffrn_orient_matrix_ub_33 -0.0303969783 _diffrn_measurement_device_type 'Oxford Diffraction Gemini diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.053 _diffrn_reflns_number 51016 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 16534 _reflns_number_gt 9670 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. Two phenolsulphonate groups, of the calixarene, one methylene group and the sulphonate oxygen atoms of a third phenolsulphonate group of the calixarenewere modelled as being disordered over two sets of sites with occupancies refined to 0.606(5) and its complement for the two components. Geometries and displacement parameters of the atoms of the disordered components were restrained to reasonable values. The solvent was modelled as water molecules with occupancies constrained either to 1.0 or 0.5 after trial refinement. Water molecule and phenoxyl hydrogen atoms were not located. ; _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 16534 _refine_ls_number_parameters 1077 _refine_ls_number_restraints 339 _refine_ls_R_factor_all 0.1325 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.3171 _refine_ls_wR_factor_gt 0.2929 _refine_ls_goodness_of_fit_ref 1.13 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 2.212 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 0.52051(6) 0.32895(4) 0.51642(3) 0.0636(3) Uani 1 1 d U . . O11 O 0.8259(3) 0.4923(3) 0.9417(2) 0.0577(10) Uani 1 1 d . . . C11 C 0.7438(4) 0.5120(4) 0.8967(3) 0.0424(12) Uani 1 1 d . . . C12 C 0.7418(4) 0.5986(4) 0.8734(3) 0.0469(13) Uani 1 1 d . A . C13 C 0.6568(4) 0.6209(4) 0.8322(3) 0.0511(14) Uani 1 1 d . . . H13 H 0.6542 0.6805 0.8168 0.061 Uiso 1 1 calc R . . C14 C 0.5740(4) 0.5557(5) 0.8128(3) 0.0497(14) Uani 1 1 d . A . S1 S 0.46411(13) 0.58435(15) 0.76163(8) 0.0653(5) Uani 1 1 d D . . O12 O 0.3840(6) 0.5444(10) 0.7852(6) 0.114(4) Uani 0.606(5) 1 d PDU A 1 O13 O 0.4616(7) 0.6935(5) 0.7777(4) 0.081(3) Uani 0.606(5) 1 d PDU A 1 O14 O 0.4828(8) 0.5633(6) 0.6903(4) 0.072(3) Uani 0.606(5) 1 d PDU A 1 O12' O 0.4998(13) 0.6121(11) 0.7014(7) 0.084(5) Uani 0.394(5) 1 d PDU A 2 O13' O 0.4079(11) 0.4850(8) 0.7358(9) 0.096(5) Uani 0.394(5) 1 d PDU A 2 O14' O 0.4052(13) 0.6378(14) 0.8015(7) 0.123(7) Uani 0.394(5) 1 d PDU A 2 C15 C 0.5813(5) 0.4672(5) 0.8345(3) 0.0531(15) Uani 1 1 d . . . H15 H 0.527 0.422 0.8203 0.064 Uiso 1 1 calc R A . C16 C 0.6645(4) 0.4444(4) 0.8756(3) 0.0486(14) Uani 1 1 d . A . C1 C 0.6703(5) 0.3468(4) 0.8987(3) 0.0546(15) Uani 1 1 d . . . H1A H 0.6941 0.3546 0.9499 0.065 Uiso 1 1 calc R A . H1B H 0.6013 0.3168 0.8918 0.065 Uiso 1 1 calc R . . O21 O 1.0049(14) 0.5621(13) 0.9427(5) 0.055(2) Uani 0.606(5) 1 d PD A 1 C21 C 1.0019(9) 0.5913(8) 0.8796(5) 0.036(2) Uani 0.606(5) 1 d PDU A 1 C22 C 1.0859(8) 0.5731(8) 0.8415(4) 0.034(2) Uani 0.606(5) 1 d PD A 1 C23 C 1.0868(10) 0.6085(8) 0.7778(6) 0.048(4) Uani 0.606(5) 1 d PD A 1 H23 H 1.1431 0.5968 0.7515 0.058 Uiso 0.606(5) 1 calc PR A 1 C24 C 1.0082(10) 0.6602(10) 0.7512(6) 0.041(3) Uani 0.606(5) 1 d PD A 1 S2 S 1.0191(3) 0.7079(2) 0.67203(18) 0.0469(8) Uani 0.606(5) 1 d PD A 1 O22 O 1.009(2) 0.6279(18) 0.6095(13) 0.119(8) Uani 0.606(5) 1 d PU A 1 O23 O 0.9322(7) 0.7711(6) 0.6631(4) 0.066(2) Uani 0.606(5) 1 d PU A 1 O24 O 1.1195(7) 0.7601(7) 0.6832(5) 0.074(2) Uani 0.606(5) 1 d PU A 1 C25 C 0.9269(10) 0.6787(12) 0.7911(5) 0.036(3) Uani 0.606(5) 1 d PD A 1 H25 H 0.8745 0.7169 0.7754 0.043 Uiso 0.606(5) 1 calc PR A 1 C26 C 0.9216(14) 0.6419(16) 0.8537(9) 0.037(3) Uani 0.606(5) 1 d PD A 1 O21' O 1.004(2) 0.567(2) 0.9192(10) 0.055(2) Uani 0.394(5) 1 d PD A 2 C21' C 0.9981(15) 0.5999(14) 0.8568(9) 0.036(2) Uani 0.394(5) 1 d PDU A 2 C22' C 1.0743(13) 0.5723(13) 0.8140(7) 0.034(2) Uani 0.394(5) 1 d PD A 2 C23' C 1.0632(14) 0.6021(12) 0.7483(8) 0.043(5) Uani 0.394(5) 1 d PD A 2 H23' H 1.1128 0.5848 0.7169 0.052 Uiso 0.394(5) 1 calc PR A 2 C24' C 0.9844(17) 0.6555(17) 0.7255(10) 0.050(6) Uani 0.394(5) 1 d PD A 2 S2' S 0.9788(6) 0.6972(6) 0.6411(6) 0.083(2) Uani 0.394(5) 1 d PDU A 2 O22' O 0.8878(14) 0.7169(19) 0.6227(13) 0.124(6) Uani 0.394(5) 1 d PU A 2 O23' O 1.054(2) 0.7894(17) 0.6681(14) 0.143(7) Uani 0.394(5) 1 d PU A 2 O24' O 1.035(2) 0.633(3) 0.613(2) 0.098(8) Uani 0.394(5) 1 d PU A 2 C25' C 0.9076(17) 0.676(2) 0.7684(10) 0.036(3) Uani 0.394(5) 1 d PD A 2 H25' H 0.8501 0.7077 0.7519 0.043 Uiso 0.394(5) 1 calc PR A 2 C26' C 0.915(2) 0.650(3) 0.8355(15) 0.037(3) Uani 0.394(5) 1 d PD A 2 C2 C 0.8316(4) 0.6692(4) 0.8911(3) 0.0507(14) Uani 1 1 d . . . H2A H 0.8096 0.7305 0.8792 0.061 Uiso 0.606(5) 1 calc PR A 1 H2B H 0.852 0.6775 0.9428 0.061 Uiso 0.606(5) 1 calc PR A 1 H2'A H 0.8637 0.6659 0.9395 0.061 Uiso 0.394(5) 1 d PR A 2 H2'B H 0.8071 0.7334 0.8905 0.061 Uiso 0.394(5) 1 d PR A 2 O31 O 1.050(2) 0.392(2) 0.9298(8) 0.054(3) Uani 0.606(5) 1 d PDU A 1 C31 C 1.0995(12) 0.3581(9) 0.8734(6) 0.044(3) Uani 0.606(5) 1 d PDU A 1 C32 C 1.0916(9) 0.2615(9) 0.8507(5) 0.048(3) Uani 0.606(5) 1 d PD A 1 C33 C 1.1458(7) 0.2199(8) 0.7969(5) 0.053(2) Uani 0.606(5) 1 d PD A 1 H33 H 1.1407 0.154 0.7818 0.063 Uiso 0.606(5) 1 calc PR A 1 C34 C 1.2076(8) 0.2769(6) 0.7657(6) 0.050(2) Uani 0.606(5) 1 d PD A 1 S3 S 1.2807(3) 0.2315(3) 0.69729(19) 0.0732(12) Uani 0.606(5) 1 d PD A 1 O32 O 1.2324(7) 0.2625(6) 0.6345(3) 0.077(3) Uani 0.606(5) 1 d PDU A 1 O33 O 1.3843(6) 0.2592(6) 0.7205(4) 0.106(4) Uani 0.606(5) 1 d PDU A 1 O34 O 1.2628(6) 0.1284(5) 0.6895(5) 0.082(3) Uani 0.606(5) 1 d PDU A 1 C35 C 1.2145(8) 0.3735(6) 0.7870(6) 0.049(3) Uani 0.606(5) 1 d PD A 1 H35 H 1.2551 0.4116 0.7638 0.059 Uiso 0.606(5) 1 calc PR A 1 C36 C 1.1626(8) 0.4147(7) 0.8419(6) 0.045(3) Uani 0.606(5) 1 d PD A 1 O31' O 1.055(4) 0.388(4) 0.9097(15) 0.054(3) Uani 0.394(5) 1 d PDU A 2 C31' C 1.094(2) 0.3500(15) 0.8489(10) 0.044(3) Uani 0.394(5) 1 d PDU A 2 C32' C 1.0770(15) 0.2527(15) 0.8292(8) 0.048(3) Uani 0.394(5) 1 d PD A 2 C33' C 1.1192(12) 0.2142(14) 0.7681(8) 0.053(2) Uani 0.394(5) 1 d PD A 2 H33' H 1.1129 0.1481 0.7536 0.063 Uiso 0.394(5) 1 calc PR A 2 C34' C 1.1699(13) 0.2682(10) 0.7278(11) 0.077(6) Uani 0.394(5) 1 d PDU A 2 S3' S 1.2154(6) 0.1983(6) 0.6579(5) 0.109(3) Uani 0.394(5) 1 d PDU A 2 O32' O 1.1422(9) 0.2052(11) 0.5999(7) 0.099(5) Uani 0.394(5) 1 d PDU A 2 O33' O 1.1989(14) 0.0980(10) 0.6769(11) 0.163(8) Uani 0.394(5) 1 d PDU A 2 O34' O 1.3156(8) 0.2104(11) 0.6497(6) 0.088(4) Uani 0.394(5) 1 d PDU A 2 C35' C 1.1837(12) 0.3634(11) 0.7512(8) 0.056(5) Uani 0.394(5) 1 d PD A 2 H35' H 1.2218 0.3997 0.725 0.067 Uiso 0.394(5) 1 calc PR A 2 C36' C 1.1447(13) 0.4088(12) 0.8109(7) 0.049(5) Uani 0.394(5) 1 d PD A 2 C3 C 1.1727(9) 0.5182(8) 0.8683(6) 0.049(2) Uani 0.606(5) 1 d PD A 1 H3A H 1.2363 0.5434 0.8541 0.058 Uiso 0.606(5) 1 calc PR A 1 H3B H 1.1786 0.5281 0.9208 0.058 Uiso 0.606(5) 1 calc PR A 1 C3' C 1.1631(14) 0.5140(12) 0.8342(9) 0.049(2) Uani 0.394(5) 1 d PD A 2 H3'A H 1.1793 0.5261 0.8864 0.058 Uiso 0.394(5) 1 calc PR A 2 H3'B H 1.2229 0.5349 0.813 0.058 Uiso 0.394(5) 1 calc PR A 2 O41 O 0.8709(4) 0.3145(4) 0.9546(2) 0.0685(13) Uani 1 1 d . A . C41 C 0.8394(5) 0.2700(4) 0.8871(3) 0.0490(14) Uani 1 1 d . . . C42 C 0.7405(4) 0.2820(4) 0.8583(3) 0.0460(13) Uani 1 1 d . A . C43 C 0.7058(4) 0.2320(4) 0.7931(3) 0.0417(11) Uani 1 1 d . . . H43 H 0.6383 0.239 0.7734 0.05 Uiso 1 1 calc R A . C44 C 0.7679(4) 0.1717(4) 0.7560(3) 0.0447(12) Uani 1 1 d . A . S4 S 0.72963(14) 0.11008(11) 0.67090(8) 0.0599(5) Uani 1 1 d . . . O42 O 0.7802(4) 0.1591(5) 0.6222(2) 0.0891(18) Uani 1 1 d . A . O43 O 0.7656(7) 0.0163(4) 0.6711(3) 0.127(3) Uani 1 1 d . A . O44 O 0.6215(3) 0.1152(3) 0.6592(2) 0.0555(11) Uani 1 1 d . A . C45 C 0.8682(5) 0.1621(4) 0.7843(3) 0.0499(13) Uani 1 1 d . . . H45 H 0.9117 0.1221 0.7584 0.06 Uiso 1 1 calc R A . C46 C 0.9036(5) 0.2113(4) 0.8506(3) 0.0511(14) Uani 1 1 d . A . C4 C 1.0158(5) 0.2001(4) 0.8798(4) 0.0651(18) Uani 1 1 d D . . H4A H 1.0227 0.216 0.932 0.078 Uiso 0.606(5) 1 calc PR A 1 H4B H 1.0329 0.1336 0.8678 0.078 Uiso 0.606(5) 1 calc PR A 1 H4'A H 1.0324 0.1331 0.8761 0.078 Uiso 0.394(5) 1 d PR A 2 H4'B H 1.0299 0.2303 0.9298 0.078 Uiso 0.394(5) 1 d PR A 2 N91 N 0.8948(5) 0.3849(5) 0.6564(5) 0.091(2) Uani 1 1 d U . . C92 C 0.8595(7) 0.4494(6) 0.6193(4) 0.083(2) Uani 1 1 d U . . H92 H 0.8821 0.4617 0.5761 0.099 Uiso 1 1 calc R . . N93 N 0.7866(4) 0.4945(3) 0.6523(2) 0.0548(12) Uani 1 1 d U . . C94 C 0.7824(6) 0.4563(4) 0.7123(3) 0.0604(16) Uani 1 1 d U . . H94 H 0.7388 0.4753 0.7476 0.072 Uiso 1 1 calc R . . C95 C 0.8470(5) 0.3897(5) 0.7145(4) 0.0704(19) Uani 1 1 d U . . H95 H 0.8579 0.3518 0.7508 0.085 Uiso 1 1 calc R . . C96 C 0.9748(10) 0.3187(9) 0.6398(9) 0.160(5) Uani 1 1 d U . . H96A H 0.9692 0.266 0.6662 0.24 Uiso 1 1 calc R . . H96B H 1.0414 0.3509 0.6533 0.24 Uiso 1 1 calc R . . H96C H 0.9669 0.2951 0.5889 0.24 Uiso 1 1 calc R . . C97 C 0.7286(8) 0.5711(5) 0.6301(4) 0.090(3) Uani 1 1 d U . . H97A H 0.7117 0.612 0.6731 0.108 Uiso 1 1 calc R . . H97B H 0.7728 0.6089 0.6057 0.108 Uiso 1 1 calc R . . C98 C 0.6355(7) 0.5463(5) 0.5840(3) 0.0693(19) Uani 1 1 d U . . O98 O 0.6063(5) 0.4626(3) 0.5715(2) 0.0810(15) Uani 1 1 d U . . O99 O 0.5920(5) 0.6155(4) 0.5600(3) 0.0849(16) Uani 1 1 d . . . P1 P 0.68813(10) 0.96767(8) 0.94470(7) 0.0334(3) Uani 1 1 d . . . C111 C 0.6421(4) 0.8599(3) 0.9694(3) 0.0342(10) Uani 1 1 d . . . C112 C 0.5515(4) 0.8167(3) 0.9404(2) 0.0330(10) Uani 1 1 d . . . H112 H 0.5093 0.8454 0.9075 0.04 Uiso 1 1 calc R . . C113 C 0.5199(4) 0.7312(3) 0.9583(3) 0.0381(11) Uani 1 1 d . . . H113 H 0.457 0.7016 0.9375 0.046 Uiso 1 1 calc R . . C114 C 0.5814(4) 0.6898(3) 1.0070(3) 0.0361(11) Uani 1 1 d . . . C115 C 0.6724(4) 0.7335(3) 1.0380(3) 0.0421(12) Uani 1 1 d . . . H115 H 0.7142 0.7055 1.0717 0.05 Uiso 1 1 calc R . . C116 C 0.7017(4) 0.8183(4) 1.0196(3) 0.0431(12) Uani 1 1 d . . . H116 H 0.7636 0.849 1.0414 0.052 Uiso 1 1 calc R . . O117 O 0.5450(3) 0.6069(2) 1.0206(2) 0.0439(8) Uani 1 1 d . . . C117 C 0.6133(4) 0.5552(4) 1.0635(3) 0.0454(12) Uani 1 1 d . . . H11A H 0.6755 0.5434 1.0408 0.068 Uiso 1 1 calc R . . H11B H 0.5802 0.4952 1.0681 0.068 Uiso 1 1 calc R . . H11C H 0.6302 0.5921 1.1107 0.068 Uiso 1 1 calc R . . C121 C 0.7110(4) 1.0554(3) 1.0220(3) 0.0349(10) Uani 1 1 d . . . C122 C 0.6786(4) 1.0431(4) 1.0864(3) 0.0412(11) Uani 1 1 d . . . H122 H 0.6445 0.986 1.0909 0.049 Uiso 1 1 calc R . . C123 C 0.6957(4) 1.1144(4) 1.1451(3) 0.0503(13) Uani 1 1 d . . . H123 H 0.674 1.1054 1.1893 0.06 Uiso 1 1 calc R . . C124 C 0.7448(4) 1.1990(4) 1.1381(3) 0.0478(13) Uani 1 1 d . . . H124 H 0.7565 1.248 1.1774 0.057 Uiso 1 1 calc R . . C125 C 0.7762(4) 1.2105(3) 1.0733(3) 0.0462(13) Uani 1 1 d . . . H125 H 0.8086 1.2683 1.0685 0.055 Uiso 1 1 calc R . . C126 C 0.7616(4) 1.1406(3) 1.0156(3) 0.0390(11) Uani 1 1 d . . . H126 H 0.7854 1.1494 0.972 0.047 Uiso 1 1 calc R . . C131 C 0.5976(4) 1.0062(3) 0.8807(3) 0.0356(10) Uani 1 1 d . . . C132 C 0.5561(4) 1.0945(3) 0.8930(3) 0.0366(11) Uani 1 1 d . . . H132 H 0.5742 1.1345 0.9368 0.044 Uiso 1 1 calc R . . C133 C 0.4886(4) 1.1237(4) 0.8415(3) 0.0435(12) Uani 1 1 d . . . H133 H 0.4598 1.1834 0.8504 0.052 Uiso 1 1 calc R . . C134 C 0.4630(5) 1.0670(4) 0.7777(3) 0.0519(14) Uani 1 1 d . . . H134 H 0.4171 1.0882 0.7427 0.062 Uiso 1 1 calc R . . C135 C 0.5030(5) 0.9795(5) 0.7638(3) 0.0574(16) Uani 1 1 d . . . H135 H 0.4846 0.9406 0.7195 0.069 Uiso 1 1 calc R . . C136 C 0.5720(5) 0.9479(4) 0.8159(3) 0.0494(14) Uani 1 1 d . . . H136 H 0.6003 0.888 0.8069 0.059 Uiso 1 1 calc R . . C141 C 0.8069(4) 0.9489(3) 0.9077(3) 0.0381(11) Uani 1 1 d . . . C142 C 0.8150(5) 0.9503(4) 0.8355(3) 0.0492(14) Uani 1 1 d . . . H142 H 0.7586 0.9647 0.8049 0.059 Uiso 1 1 calc R . . C143 C 0.9069(5) 0.9302(4) 0.8100(4) 0.0568(15) Uani 1 1 d . . . H143 H 0.9136 0.9321 0.7615 0.068 Uiso 1 1 calc R . . C144 C 0.9894(5) 0.9072(4) 0.8536(4) 0.0542(15) Uani 1 1 d . . . H144 H 1.0517 0.8933 0.8348 0.065 Uiso 1 1 calc R . . C145 C 0.9814(5) 0.9044(6) 0.9233(4) 0.0673(19) Uani 1 1 d . . . H145 H 1.0375 0.8873 0.9529 0.081 Uiso 1 1 calc R . . C146 C 0.8903(4) 0.9269(5) 0.9515(3) 0.0582(16) Uani 1 1 d . . . H146 H 0.8855 0.9271 1.0005 0.07 Uiso 1 1 calc R . . O1 O 0.4832(4) 0.9830(3) 0.5675(2) 0.0690(12) Uani 1 1 d . . . O2 O 0.3510(4) 0.2288(4) 0.2860(3) 0.0841(15) Uani 1 1 d . . . O3 O 0.3512(7) 0.7921(4) 0.6910(3) 0.118(2) Uani 1 1 d . . . O4 O 0.8143(6) 0.4562(6) 0.4476(4) 0.127(3) Uani 1 1 d D . . O5 O 0.7495(7) 0.8424(5) 0.5997(6) 0.171(4) Uani 1 1 d . . . O6 O 0.2687(8) 0.9898(7) 0.5686(8) 0.103(4) Uani 0.5 1 d P . . O7 O 0.8650(7) 1.0024(10) 0.5443(6) 0.095(4) Uani 0.5 1 d P . . O8 O 0.8266(10) 0.1910(9) 0.4478(7) 0.101(4) Uiso 0.5 1 d P . . O9 O 0.8923(15) 0.6396(14) 0.4886(11) 0.155(6) Uiso 0.5 1 d P . . O101 O 0.6860(5) 0.2673(4) 0.5333(3) 0.0903(17) Uani 1 1 d . . . O102 O 0.5427(5) 0.2788(4) 0.6293(3) 0.0957(19) Uani 1 1 d U . . O103 O 0.3854(6) 0.2179(4) 0.5172(3) 0.110(2) Uani 1 1 d U . . O104 O 0.5172(6) 0.2038(3) 0.4202(2) 0.0947(19) Uani 1 1 d U . . O105 O 0.6182(5) 0.3758(3) 0.4296(2) 0.0760(14) Uani 1 1 d . . . O106 O 0.4046(4) 0.4068(3) 0.5909(3) 0.0768(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.1308(7) 0.0273(3) 0.0317(3) 0.0017(2) 0.0053(3) 0.0139(3) O11 0.057(3) 0.055(2) 0.057(2) -0.0057(19) 0.010(2) -0.002(2) C11 0.044(3) 0.044(3) 0.038(3) -0.007(2) 0.017(2) -0.001(2) C12 0.041(3) 0.051(3) 0.044(3) -0.016(2) 0.018(2) 0.003(2) C13 0.053(3) 0.057(3) 0.045(3) -0.003(2) 0.025(3) 0.007(3) C14 0.044(3) 0.076(4) 0.032(3) 0.004(2) 0.023(2) -0.003(3) S1 0.0558(9) 0.1054(14) 0.0356(7) 0.0097(8) 0.0118(7) -0.0032(9) O12 0.055(5) 0.212(12) 0.092(7) 0.088(8) -0.003(5) -0.032(7) O13 0.077(6) 0.071(5) 0.074(5) -0.034(4) -0.026(4) 0.034(4) O14 0.136(8) 0.052(5) 0.025(3) -0.002(3) 0.010(4) 0.005(5) O12' 0.115(10) 0.082(10) 0.055(8) 0.024(7) -0.004(7) -0.026(9) O13' 0.069(8) 0.081(9) 0.141(12) 0.052(9) -0.024(8) -0.023(7) O14' 0.093(11) 0.167(14) 0.090(10) -0.030(10) -0.018(9) 0.058(11) C15 0.048(3) 0.068(4) 0.043(3) -0.001(3) 0.023(3) -0.009(3) C16 0.051(3) 0.058(3) 0.037(3) -0.007(2) 0.027(3) -0.006(3) C1 0.057(4) 0.056(4) 0.051(3) 0.000(3) 0.025(3) -0.011(3) O21 0.058(3) 0.075(4) 0.037(7) 0.025(6) 0.007(7) 0.011(3) C21 0.047(3) 0.031(3) 0.035(7) 0.026(5) 0.008(5) -0.003(3) C22 0.038(4) 0.037(3) 0.030(6) 0.006(5) 0.010(5) -0.008(3) C23 0.030(6) 0.034(6) 0.074(10) -0.013(7) 0.009(6) -0.010(4) C24 0.060(8) 0.025(5) 0.038(7) 0.005(5) 0.014(6) -0.007(5) S2 0.054(2) 0.0449(15) 0.0446(16) 0.0094(12) 0.0183(13) -0.0026(14) O22 0.185(16) 0.073(9) 0.094(9) -0.021(7) 0.048(11) 0.003(11) O23 0.084(6) 0.064(5) 0.057(4) 0.017(4) 0.028(4) 0.013(4) O24 0.072(5) 0.078(6) 0.079(5) 0.035(4) 0.015(4) -0.012(4) C25 0.037(6) 0.021(3) 0.046(9) 0.003(7) -0.003(5) 0.000(4) C26 0.048(4) 0.022(5) 0.044(9) 0.008(6) 0.013(6) 0.000(3) O21' 0.058(3) 0.075(4) 0.037(7) 0.025(6) 0.007(7) 0.011(3) C21' 0.047(3) 0.031(3) 0.035(7) 0.026(5) 0.008(5) -0.003(3) C22' 0.038(4) 0.037(3) 0.030(6) 0.006(5) 0.010(5) -0.008(3) C23' 0.041(12) 0.023(7) 0.066(13) -0.006(8) 0.029(10) -0.003(7) C24' 0.071(14) 0.034(9) 0.046(13) 0.008(10) 0.004(10) 0.003(9) S2' 0.073(5) 0.087(5) 0.111(6) 0.066(5) 0.033(4) 0.015(4) O22' 0.085(10) 0.180(15) 0.140(13) 0.101(12) 0.052(10) 0.028(11) O23' 0.146(15) 0.133(13) 0.167(14) 0.079(12) 0.031(13) -0.030(12) O24' 0.092(12) 0.086(14) 0.128(15) 0.041(12) 0.027(11) 0.016(10) C25' 0.037(6) 0.021(3) 0.046(9) 0.003(7) -0.003(5) 0.000(4) C26' 0.048(4) 0.022(5) 0.044(9) 0.008(6) 0.013(6) 0.000(3) C2 0.050(3) 0.037(3) 0.060(3) -0.013(2) 0.018(3) 0.004(2) O31 0.061(4) 0.051(3) 0.048(10) 0.004(9) 0.004(9) -0.011(3) C31 0.033(4) 0.045(4) 0.049(10) -0.004(6) 0.003(6) 0.008(3) C32 0.035(5) 0.045(4) 0.061(8) 0.007(5) -0.013(5) 0.002(3) C33 0.049(7) 0.049(4) 0.055(7) 0.004(6) -0.011(5) 0.024(5) C34 0.042(6) 0.051(6) 0.060(6) 0.018(5) 0.006(5) 0.018(4) S3 0.074(2) 0.080(2) 0.070(2) 0.0183(16) 0.0126(18) 0.0427(18) O32 0.111(7) 0.099(6) 0.030(3) 0.017(4) 0.016(4) 0.087(6) O33 0.129(8) 0.136(8) 0.077(6) 0.048(5) 0.053(5) 0.103(7) O34 0.068(5) 0.075(6) 0.096(6) -0.009(5) 0.003(5) 0.047(4) C35 0.037(6) 0.053(6) 0.063(7) 0.021(5) 0.010(5) 0.015(5) C36 0.031(6) 0.035(5) 0.072(8) 0.023(6) 0.001(6) 0.007(4) O31' 0.061(4) 0.051(3) 0.048(10) 0.004(9) 0.004(9) -0.011(3) C31' 0.033(4) 0.045(4) 0.049(10) -0.004(6) 0.003(6) 0.008(3) C32' 0.035(5) 0.045(4) 0.061(8) 0.007(5) -0.013(5) 0.002(3) C33' 0.049(7) 0.049(4) 0.055(7) 0.004(6) -0.011(5) 0.024(5) C34' 0.035(8) 0.109(13) 0.076(11) -0.024(10) 0.004(8) 0.018(9) S3' 0.093(5) 0.119(6) 0.109(5) -0.026(4) 0.035(4) 0.028(4) O32' 0.098(9) 0.126(10) 0.080(8) 0.016(7) 0.030(7) 0.054(8) O33' 0.168(13) 0.144(12) 0.178(13) 0.031(11) 0.015(12) 0.024(11) O34' 0.088(8) 0.130(9) 0.062(7) 0.026(6) 0.060(6) 0.037(7) C35' 0.033(9) 0.094(14) 0.037(9) -0.004(9) 0.009(7) -0.001(8) C36' 0.028(9) 0.075(12) 0.047(10) 0.021(9) -0.008(8) 0.008(8) C3 0.039(4) 0.056(4) 0.054(7) 0.014(6) 0.011(6) -0.004(3) C3' 0.039(4) 0.056(4) 0.054(7) 0.014(6) 0.011(6) -0.004(3) O41 0.073(3) 0.081(3) 0.046(2) 0.000(2) 0.001(2) -0.013(2) C41 0.058(4) 0.050(3) 0.040(3) 0.014(2) 0.005(3) -0.008(3) C42 0.051(3) 0.043(3) 0.047(3) 0.007(2) 0.022(3) -0.010(2) C43 0.043(3) 0.043(3) 0.041(3) 0.009(2) 0.012(2) 0.000(2) C44 0.055(3) 0.040(3) 0.042(3) 0.011(2) 0.010(2) 0.004(2) S4 0.0830(12) 0.0550(9) 0.0406(7) 0.0016(6) 0.0033(7) 0.0296(8) O42 0.067(3) 0.158(6) 0.048(3) 0.022(3) 0.019(2) 0.030(3) O43 0.227(8) 0.072(4) 0.063(3) -0.019(3) -0.043(4) 0.078(4) O44 0.076(3) 0.044(2) 0.043(2) 0.0007(17) 0.0047(19) -0.014(2) C45 0.052(3) 0.043(3) 0.058(3) 0.018(3) 0.008(3) 0.008(2) C46 0.054(3) 0.042(3) 0.058(3) 0.018(3) -0.002(3) -0.003(3) C4 0.056(4) 0.041(3) 0.097(5) 0.017(3) -0.007(4) 0.003(3) N91 0.079(4) 0.065(4) 0.146(6) 0.033(4) 0.067(4) 0.021(3) C92 0.119(6) 0.072(5) 0.069(4) 0.012(3) 0.064(4) 0.005(4) N93 0.092(4) 0.034(2) 0.040(2) 0.0030(18) 0.016(2) 0.010(2) C94 0.088(5) 0.054(3) 0.044(3) 0.007(3) 0.030(3) 0.001(3) C95 0.067(4) 0.063(4) 0.093(5) 0.040(4) 0.024(4) 0.005(3) C96 0.119(8) 0.126(9) 0.261(13) 0.040(9) 0.110(8) 0.052(7) C97 0.153(7) 0.037(3) 0.073(4) 0.005(3) -0.026(5) 0.017(4) C98 0.130(6) 0.044(3) 0.031(3) 0.001(2) 0.005(3) 0.004(4) O98 0.131(4) 0.054(3) 0.053(3) -0.010(2) 0.014(3) 0.001(3) O99 0.133(5) 0.065(3) 0.057(3) 0.025(2) -0.005(3) 0.006(3) P1 0.0396(7) 0.0199(5) 0.0417(7) 0.0003(5) 0.0156(5) 0.0015(5) C111 0.038(3) 0.024(2) 0.043(3) 0.0028(18) 0.018(2) 0.0021(19) C112 0.042(3) 0.021(2) 0.035(2) -0.0045(17) 0.014(2) 0.0050(18) C113 0.039(3) 0.027(2) 0.047(3) -0.002(2) 0.014(2) 0.001(2) C114 0.048(3) 0.021(2) 0.044(3) 0.0038(18) 0.025(2) 0.0053(19) C115 0.041(3) 0.030(2) 0.059(3) 0.014(2) 0.013(2) 0.006(2) C116 0.039(3) 0.032(2) 0.059(3) 0.008(2) 0.006(2) -0.001(2) O117 0.048(2) 0.0265(17) 0.061(2) 0.0084(15) 0.0214(17) 0.0021(15) C117 0.054(3) 0.031(3) 0.056(3) 0.013(2) 0.020(3) 0.008(2) C121 0.038(3) 0.024(2) 0.042(3) 0.0006(18) 0.006(2) 0.0040(18) C122 0.045(3) 0.036(3) 0.043(3) 0.001(2) 0.012(2) -0.001(2) C123 0.052(3) 0.050(3) 0.047(3) -0.002(2) 0.015(3) -0.004(3) C124 0.045(3) 0.040(3) 0.055(3) -0.008(2) 0.011(3) 0.004(2) C125 0.047(3) 0.025(2) 0.065(3) -0.003(2) 0.010(3) -0.003(2) C126 0.047(3) 0.025(2) 0.045(3) 0.0005(19) 0.011(2) 0.001(2) C131 0.041(3) 0.027(2) 0.041(2) 0.0030(19) 0.015(2) 0.0001(19) C132 0.036(3) 0.030(2) 0.044(3) -0.001(2) 0.015(2) -0.0036(19) C133 0.040(3) 0.041(3) 0.054(3) 0.015(2) 0.019(2) 0.001(2) C134 0.062(4) 0.054(3) 0.042(3) 0.017(3) 0.009(3) -0.006(3) C135 0.081(4) 0.056(4) 0.035(3) 0.007(2) 0.012(3) -0.018(3) C136 0.073(4) 0.034(3) 0.041(3) 0.002(2) 0.014(3) -0.004(3) C141 0.039(3) 0.019(2) 0.057(3) 0.001(2) 0.016(2) 0.0008(18) C142 0.055(3) 0.039(3) 0.065(4) 0.025(3) 0.034(3) 0.019(2) C143 0.066(4) 0.047(3) 0.067(4) 0.015(3) 0.031(3) 0.023(3) C144 0.047(3) 0.037(3) 0.080(4) -0.002(3) 0.032(3) 0.000(2) C145 0.032(3) 0.088(5) 0.080(5) 0.009(4) 0.005(3) 0.001(3) C146 0.038(3) 0.079(4) 0.057(3) 0.004(3) 0.009(3) -0.008(3) O1 0.103(4) 0.041(2) 0.062(3) 0.0008(19) 0.015(2) -0.005(2) O2 0.099(4) 0.073(3) 0.075(3) -0.016(3) 0.022(3) 0.013(3) O3 0.209(8) 0.080(4) 0.060(3) -0.014(3) 0.029(4) 0.006(4) O4 0.148(6) 0.147(7) 0.101(5) 0.031(5) 0.055(4) 0.019(5) O5 0.172(8) 0.084(5) 0.220(10) -0.067(6) -0.032(7) 0.038(5) O6 0.067(6) 0.049(6) 0.197(13) -0.008(7) 0.071(8) 0.004(5) O7 0.043(5) 0.161(12) 0.076(7) -0.005(7) 0.015(5) 0.005(6) O101 0.133(5) 0.084(4) 0.065(3) 0.024(3) 0.036(3) 0.036(3) O102 0.130(5) 0.114(4) 0.060(3) 0.040(3) 0.037(3) 0.062(4) O103 0.201(7) 0.057(3) 0.071(3) -0.005(3) 0.042(4) -0.025(4) O104 0.189(6) 0.042(3) 0.049(3) -0.010(2) 0.014(3) 0.019(3) O105 0.134(5) 0.048(2) 0.048(2) 0.0085(19) 0.015(3) 0.013(3) O106 0.111(4) 0.047(3) 0.067(3) -0.004(2) -0.002(3) 0.023(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Y1 O99 2.233(5) 2_666 ? Y1 O98 2.271(5) . ? Y1 O103 2.376(6) . ? Y1 O104 2.377(4) . ? Y1 O105 2.379(5) . ? Y1 O102 2.380(5) . ? Y1 O106 2.395(5) . ? Y1 O101 2.399(6) . ? O11 C11 1.382(7) . ? C11 C12 1.390(8) . ? C11 C16 1.402(8) . ? C12 C13 1.381(9) . ? C12 C2 1.524(8) . ? C13 C14 1.411(8) . ? C13 H13 0.95 . ? C14 C15 1.403(9) . ? C14 S1 1.766(6) . ? S1 O14' 1.330(11) . ? S1 O12 1.347(7) . ? S1 O12' 1.401(10) . ? S1 O14 1.407(6) . ? S1 O13 1.560(7) . ? S1 O13' 1.585(11) . ? C15 C16 1.365(9) . ? C15 H15 0.95 . ? C16 C1 1.539(9) . ? C1 C42 1.523(8) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? O21 C21 1.340(9) . ? C21 C26 1.399(9) . ? C21 C22 1.403(8) . ? C22 C23 1.395(9) . ? C22 C3 1.505(13) . ? C23 C24 1.395(9) . ? C23 H23 0.95 . ? C24 C25 1.396(9) . ? C24 S2 1.779(14) . ? S2 O24 1.492(10) . ? S2 O23 1.499(10) . ? S2 O22 1.528(19) . ? C25 C26 1.392(9) . ? C25 H25 0.95 . ? C26 C2 1.488(17) . ? O21' C21' 1.350(13) . ? C21' C26' 1.396(10) . ? C21' C22' 1.397(10) . ? C22' C23' 1.389(10) . ? C22' C3' 1.515(17) . ? C23' C24' 1.387(10) . ? C23' H23' 0.95 . ? C24' C25' 1.386(10) . ? C24' S2' 1.81(2) . ? S2' O22' 1.27(2) . ? S2' O24' 1.29(2) . ? S2' O23' 1.63(2) . ? C25' C26' 1.391(10) . ? C25' H25' 0.95 . ? C26' C2 1.61(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C2 H2'A 0.99 . ? C2 H2'B 0.99 . ? O31 C31 1.354(13) . ? C31 C32 1.394(9) . ? C31 C36 1.398(9) . ? C32 C33 1.392(9) . ? C32 C4 1.525(16) . ? C33 C34 1.386(9) . ? C33 H33 0.95 . ? C34 C35 1.388(9) . ? C34 S3 1.770(10) . ? S3 O33 1.428(9) . ? S3 O32 1.442(6) . ? S3 O34 1.482(8) . ? C35 C36 1.385(9) . ? C35 H35 0.95 . ? C36 C3 1.501(12) . ? O31' C31' 1.369(18) . ? C31' C36' 1.403(10) . ? C31' C32' 1.404(10) . ? C32' C33' 1.398(10) . ? C32' C4 1.591(17) . ? C33' C34' 1.387(10) . ? C33' H33' 0.95 . ? C34' C35' 1.380(10) . ? C34' S3' 1.725(17) . ? S3' O34' 1.365(11) . ? S3' O32' 1.418(12) . ? S3' O33' 1.558(13) . ? C35' C36' 1.388(10) . ? C35' H35' 0.95 . ? C36' C3' 1.522(17) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C3' H3'A 0.99 . ? C3' H3'B 0.99 . ? O41 C41 1.375(7) . ? C41 C46 1.385(9) . ? C41 C42 1.396(8) . ? C42 C43 1.375(8) . ? C43 C44 1.384(8) . ? C43 H43 0.95 . ? C44 C45 1.404(8) . ? C44 S4 1.757(6) . ? S4 O44 1.434(5) . ? S4 O43 1.446(5) . ? S4 O42 1.460(6) . ? C45 C46 1.390(8) . ? C45 H45 0.95 . ? C46 C4 1.557(9) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C4 H4'A 0.99 . ? C4 H4'B 0.99 . ? N91 C92 1.321(11) . ? N91 C95 1.333(10) . ? N91 C96 1.472(12) . ? C92 N93 1.340(9) . ? C92 H92 0.95 . ? N93 C94 1.355(7) . ? N93 C97 1.454(8) . ? C94 C95 1.306(9) . ? C94 H94 0.95 . ? C95 H95 0.95 . ? C96 H96A 0.98 . ? C96 H96B 0.98 . ? C96 H96C 0.98 . ? C97 C98 1.447(11) . ? C97 H97A 0.99 . ? C97 H97B 0.99 . ? C98 O98 1.238(8) . ? C98 O99 1.286(8) . ? O99 Y1 2.233(5) 2_666 ? P1 C131 1.788(5) . ? P1 C121 1.794(5) . ? P1 C111 1.803(5) . ? P1 C141 1.805(5) . ? C111 C112 1.365(7) . ? C111 C116 1.396(7) . ? C112 C113 1.396(6) . ? C112 H112 0.95 . ? C113 C114 1.389(7) . ? C113 H113 0.95 . ? C114 O117 1.349(5) . ? C114 C115 1.381(8) . ? C115 C116 1.382(7) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? O117 C117 1.458(6) . ? C117 H11A 0.98 . ? C117 H11B 0.98 . ? C117 H11C 0.98 . ? C121 C122 1.387(7) . ? C121 C126 1.412(7) . ? C122 C123 1.402(7) . ? C122 H122 0.95 . ? C123 C124 1.399(8) . ? C123 H123 0.95 . ? C124 C125 1.384(8) . ? C124 H124 0.95 . ? C125 C126 1.375(7) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.397(7) . ? C131 C136 1.398(7) . ? C132 C133 1.386(8) . ? C132 H132 0.95 . ? C133 C134 1.373(8) . ? C133 H133 0.95 . ? C134 C135 1.381(9) . ? C134 H134 0.95 . ? C135 C136 1.419(9) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C141 C146 1.393(8) . ? C141 C142 1.405(8) . ? C142 C143 1.382(8) . ? C142 H142 0.95 . ? C143 C144 1.386(9) . ? C143 H143 0.95 . ? C144 C145 1.361(10) . ? C144 H144 0.95 . ? C145 C146 1.400(9) . ? C145 H145 0.95 . ? C146 H146 0.95 . ? 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 O99 Y1 O98 101.7(2) 2_666 . ? O99 Y1 O103 82.2(2) 2_666 . ? O98 Y1 O103 147.1(2) . . ? O99 Y1 O104 81.3(2) 2_666 . ? O98 Y1 O104 144.3(2) . . ? O103 Y1 O104 68.5(2) . . ? O99 Y1 O105 75.4(2) 2_666 . ? O98 Y1 O105 75.41(17) . . ? O103 Y1 O105 135.98(18) . . ? O104 Y1 O105 71.01(19) . . ? O99 Y1 O102 143.6(2) 2_666 . ? O98 Y1 O102 85.3(2) . . ? O103 Y1 O102 73.9(2) . . ? O104 Y1 O102 113.4(2) . . ? O105 Y1 O102 140.1(2) . . ? O99 Y1 O106 76.71(19) 2_666 . ? O98 Y1 O106 75.32(19) . . ? O103 Y1 O106 73.9(2) . . ? O104 Y1 O106 138.4(2) . . ? O105 Y1 O106 133.94(17) . . ? O102 Y1 O106 70.59(17) . . ? O99 Y1 O101 145.1(2) 2_666 . ? O98 Y1 O101 81.4(2) . . ? O103 Y1 O101 114.1(2) . . ? O104 Y1 O101 77.1(2) . . ? O105 Y1 O101 71.86(18) . . ? O102 Y1 O101 70.96(18) . . ? O106 Y1 O101 136.18(17) . . ? O11 C11 C12 119.1(5) . . ? O11 C11 C16 119.5(5) . . ? C12 C11 C16 121.4(5) . . ? C13 C12 C11 119.2(5) . . ? C13 C12 C2 119.2(6) . . ? C11 C12 C2 121.6(5) . . ? C12 C13 C14 120.4(6) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 118.5(6) . . ? C15 C14 S1 120.8(5) . . ? C13 C14 S1 120.7(5) . . ? O14' S1 O12' 122.2(9) . . ? O12 S1 O14 120.9(6) . . ? O12 S1 O13 110.5(6) . . ? O14 S1 O13 105.7(5) . . ? O14' S1 O13' 108.6(8) . . ? O12' S1 O13' 106.0(7) . . ? O14' S1 C14 111.0(7) . . ? O12 S1 C14 107.2(5) . . ? O12' S1 C14 104.7(8) . . ? O14 S1 C14 106.5(5) . . ? O13 S1 C14 104.9(4) . . ? O13' S1 C14 102.5(6) . . ? C16 C15 C14 121.8(5) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C11 118.6(6) . . ? C15 C16 C1 120.6(5) . . ? C11 C16 C1 120.8(6) . . ? C42 C1 C16 113.6(4) . . ? C42 C1 H1A 108.9 . . ? C16 C1 H1A 108.9 . . ? C42 C1 H1B 108.8 . . ? C16 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O21 C21 C26 122.0(11) . . ? O21 C21 C22 117.1(10) . . ? C26 C21 C22 120.8(9) . . ? C23 C22 C21 117.7(9) . . ? C23 C22 C3 120.8(9) . . ? C21 C22 C3 121.5(8) . . ? C22 C23 C24 122.7(12) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C23 C24 C25 118.2(12) . . ? C23 C24 S2 119.5(10) . . ? C25 C24 S2 122.2(10) . . ? O24 S2 O23 112.5(6) . . ? O24 S2 O22 114.0(11) . . ? O23 S2 O22 108.5(12) . . ? O24 S2 C24 105.7(6) . . ? O23 S2 C24 107.1(5) . . ? O22 S2 C24 108.9(13) . . ? C26 C25 C24 120.8(14) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 119.7(13) . . ? C25 C26 C2 114.7(10) . . ? C21 C26 C2 125.3(10) . . ? O21' C21' C26' 120(2) . . ? O21' C21' C22' 115.6(18) . . ? C26' C21' C22' 123.8(18) . . ? C23' C22' C21' 114.5(15) . . ? C23' C22' C3' 120.4(15) . . ? C21' C22' C3' 125.1(14) . . ? C24' C23' C22' 124.2(18) . . ? C24' C23' H23' 117.9 . . ? C22' C23' H23' 117.9 . . ? C25' C24' C23' 119(2) . . ? C25' C24' S2' 119.6(15) . . ? C23' C24' S2' 121.7(16) . . ? O22' S2' O24' 130(2) . . ? O22' S2' O23' 113.4(17) . . ? O24' S2' O23' 106(2) . . ? O22' S2' C24' 109.0(11) . . ? O24' S2' C24' 95(2) . . ? O23' S2' C24' 96.3(13) . . ? C24' C25' C26' 120(2) . . ? C24' C25' H25' 120 . . ? C26' C25' H25' 120 . . ? C25' C26' C21' 118(2) . . ? C25' C26' C2 125.5(17) . . ? C21' C26' C2 116.0(17) . . ? C26 C2 C12 114.4(11) . . ? C12 C2 C26' 112.0(16) . . ? C26 C2 H2A 108.7 . . ? C12 C2 H2A 108.7 . . ? C26 C2 H2B 108.7 . . ? C12 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C12 C2 H2'A 109.3 . . ? C26' C2 H2'A 109.5 . . ? C12 C2 H2'B 109.3 . . ? C26' C2 H2'B 108.8 . . ? H2'A C2 H2'B 107.9 . . ? O31 C31 C32 117.0(17) . . ? O31 C31 C36 122.9(17) . . ? C32 C31 C36 119.9(12) . . ? C33 C32 C31 121.0(12) . . ? C33 C32 C4 118.3(10) . . ? C31 C32 C4 120.5(10) . . ? C34 C33 C32 118.5(11) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C33 C34 C35 120.9(10) . . ? C33 C34 S3 122.3(8) . . ? C35 C34 S3 116.8(7) . . ? O33 S3 O32 119.2(6) . . ? O33 S3 O34 112.0(4) . . ? O32 S3 O34 107.8(5) . . ? O33 S3 C34 107.6(5) . . ? O32 S3 C34 104.8(5) . . ? O34 S3 C34 104.2(5) . . ? C36 C35 C34 120.7(9) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 119.0(10) . . ? C35 C36 C3 121.7(9) . . ? C31 C36 C3 119.3(10) . . ? O31' C31' C36' 119(3) . . ? O31' C31' C32' 116(3) . . ? C36' C31' C32' 125(2) . . ? C33' C32' C31' 115.1(18) . . ? C33' C32' C4 128.4(16) . . ? C31' C32' C4 116.5(14) . . ? C34' C33' C32' 122.8(17) . . ? C34' C33' H33' 118.6 . . ? C32' C33' H33' 118.6 . . ? C35' C34' C33' 118.3(17) . . ? C35' C34' S3' 130.6(13) . . ? C33' C34' S3' 110.8(12) . . ? O34' S3' O32' 118.7(9) . . ? O34' S3' O33' 107.7(8) . . ? O32' S3' O33' 106.0(9) . . ? O34' S3' C34' 117.1(10) . . ? O32' S3' C34' 103.5(10) . . ? O33' S3' C34' 102.1(10) . . ? C34' C35' C36' 123.4(16) . . ? C34' C35' H35' 118.3 . . ? C36' C35' H35' 118.3 . . ? C35' C36' C31' 115.2(18) . . ? C35' C36' C3' 120.9(15) . . ? C31' C36' C3' 123.8(15) . . ? C36 C3 C22 114.3(9) . . ? C36 C3 H3A 108.7 . . ? C22 C3 H3A 108.7 . . ? C36 C3 H3B 108.7 . . ? C22 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C22' C3' C36' 114.3(15) . . ? C22' C3' H3'A 108.7 . . ? C36' C3' H3'A 108.7 . . ? C22' C3' H3'B 108.7 . . ? C36' C3' H3'B 108.7 . . ? H3'A C3' H3'B 107.6 . . ? O41 C41 C46 120.1(6) . . ? O41 C41 C42 118.5(6) . . ? C46 C41 C42 121.3(5) . . ? C43 C42 C41 118.9(5) . . ? C43 C42 C1 120.0(5) . . ? C41 C42 C1 121.1(5) . . ? C42 C43 C44 120.9(5) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 S4 122.9(4) . . ? C45 C44 S4 117.1(4) . . ? O44 S4 O43 114.8(4) . . ? O44 S4 O42 111.5(3) . . ? O43 S4 O42 111.4(4) . . ? O44 S4 C44 106.9(3) . . ? O43 S4 C44 105.9(3) . . ? O42 S4 C44 105.8(3) . . ? C46 C45 C44 119.6(6) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C41 C46 C45 119.3(5) . . ? C41 C46 C4 122.5(6) . . ? C45 C46 C4 118.1(6) . . ? C32 C4 C46 113.7(7) . . ? C46 C4 C32' 102.4(9) . . ? C32 C4 H4A 108.8 . . ? C46 C4 H4A 108.8 . . ? C32 C4 H4B 108.8 . . ? C46 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C32' C4 H4'A 111.4 . . ? C46 C4 H4'A 111.2 . . ? C46 C4 H4'B 111.2 . . ? C32' C4 H4'B 111.3 . . ? H4'A C4 H4'B 109.2 . . ? C92 N91 C95 108.5(6) . . ? C92 N91 C96 127.6(9) . . ? C95 N91 C96 123.8(9) . . ? N91 C92 N93 109.0(6) . . ? N91 C92 H92 125.5 . . ? N93 C92 H92 125.5 . . ? C92 N93 C94 105.1(6) . . ? C92 N93 C97 127.2(7) . . ? C94 N93 C97 127.6(6) . . ? C95 C94 N93 110.1(6) . . ? C95 C94 H94 124.9 . . ? N93 C94 H94 124.9 . . ? C94 C95 N91 107.2(6) . . ? C94 C95 H95 126.4 . . ? N91 C95 H95 126.4 . . ? N91 C96 H96A 109.5 . . ? N91 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? N91 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C98 C97 N93 117.1(6) . . ? C98 C97 H97A 108 . . ? N93 C97 H97A 108 . . ? C98 C97 H97B 108 . . ? N93 C97 H97B 108 . . ? H97A C97 H97B 107.3 . . ? O98 C98 O99 127.0(7) . . ? O98 C98 C97 118.1(6) . . ? O99 C98 C97 114.9(6) . . ? C98 O98 Y1 159.5(5) . . ? C98 O99 Y1 150.7(5) . 2_666 ? C131 P1 C121 110.4(2) . . ? C131 P1 C111 110.0(2) . . ? C121 P1 C111 109.5(2) . . ? C131 P1 C141 109.5(2) . . ? C121 P1 C141 107.8(2) . . ? C111 P1 C141 109.6(2) . . ? C112 C111 C116 118.7(4) . . ? C112 C111 P1 122.4(4) . . ? C116 C111 P1 118.9(4) . . ? C111 C112 C113 121.1(5) . . ? C111 C112 H112 119.5 . . ? C113 C112 H112 119.5 . . ? C114 C113 C112 119.3(4) . . ? C114 C113 H113 120.3 . . ? C112 C113 H113 120.3 . . ? O117 C114 C115 124.6(5) . . ? O117 C114 C113 115.1(4) . . ? C115 C114 C113 120.3(4) . . ? C114 C115 C116 119.1(5) . . ? C114 C115 H115 120.4 . . ? C116 C115 H115 120.4 . . ? C115 C116 C111 121.4(5) . . ? C115 C116 H116 119.3 . . ? C111 C116 H116 119.3 . . ? C114 O117 C117 116.6(4) . . ? O117 C117 H11A 109.5 . . ? O117 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? O117 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C122 C121 C126 119.5(4) . . ? C122 C121 P1 122.3(4) . . ? C126 C121 P1 118.2(4) . . ? C121 C122 C123 120.5(5) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C124 C123 C122 119.6(5) . . ? C124 C123 H123 120.2 . . ? C122 C123 H123 120.2 . . ? C125 C124 C123 119.2(5) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C126 C125 C124 121.9(5) . . ? C126 C125 H125 119.1 . . ? C124 C125 H125 119.1 . . ? C125 C126 C121 119.3(5) . . ? C125 C126 H126 120.4 . . ? C121 C126 H126 120.4 . . ? C132 C131 C136 119.9(5) . . ? C132 C131 P1 121.3(4) . . ? C136 C131 P1 118.7(4) . . ? C133 C132 C131 120.0(5) . . ? C133 C132 H132 120 . . ? C131 C132 H132 120 . . ? C134 C133 C132 120.5(5) . . ? C134 C133 H133 119.8 . . ? C132 C133 H133 119.8 . . ? C133 C134 C135 120.9(6) . . ? C133 C134 H134 119.6 . . ? C135 C134 H134 119.6 . . ? C134 C135 C136 119.6(5) . . ? C134 C135 H135 120.2 . . ? C136 C135 H135 120.2 . . ? C131 C136 C135 119.1(5) . . ? C131 C136 H136 120.5 . . ? C135 C136 H136 120.5 . . ? C146 C141 C142 119.8(5) . . ? C146 C141 P1 118.5(4) . . ? C142 C141 P1 121.6(4) . . ? C143 C142 C141 118.5(6) . . ? C143 C142 H142 120.7 . . ? C141 C142 H142 120.7 . . ? C142 C143 C144 121.5(6) . . ? C142 C143 H143 119.2 . . ? C144 C143 H143 119.2 . . ? C145 C144 C143 120.1(5) . . ? C145 C144 H144 120 . . ? C143 C144 H144 120 . . ? C144 C145 C146 120.0(6) . . ? C144 C145 H145 120 . . ? C146 C145 H145 120 . . ? C141 C146 C145 120.0(6) . . ? C141 C146 H146 120 . . ? C145 C146 H146 120 . . ? #===END # Attachment '7925_web_deposit_cif_file_1_BrianSkelton_1320129951.100907i.cif' data_100907i _database_code_depnum_ccdc_archive 'CCDC 851782' #TrackingRef '7925_web_deposit_cif_file_1_BrianSkelton_1320129951.100907i.cif' _audit_creation_date 2011-05-18T09:44:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C236 H277 Gd5 N8 O116 P4 S16' _chemical_formula_moiety ; C136 H167 Gd5 N8 O101 S16, 4(C25 H22 O P), 11(H2 O)' ; _chemical_formula_weight 6504.75 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5398(2) _cell_length_b 20.0742(4) _cell_length_c 25.4500(5) _cell_angle_alpha 75.672(2) _cell_angle_beta 88.7520(10) _cell_angle_gamma 89.7450(10) _cell_volume 6700.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 40147 _cell_measurement_theta_min 3.5158 _cell_measurement_theta_max 32.6384 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3313 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.1495 0 -1 0 0.0716 0 -1 -2 0.1739 0 1 2 0.1811 1 -1 -1 0.1831 1 1 3 0.2228 -2 -1 -2 0.2551 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.47 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.797 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0013319914 _diffrn_orient_matrix_ub_12 -0.0033546984 _diffrn_orient_matrix_ub_13 0.0283894472 _diffrn_orient_matrix_ub_21 -0.0161811947 _diffrn_orient_matrix_ub_22 -0.0345245137 _diffrn_orient_matrix_ub_23 0.0042631584 _diffrn_orient_matrix_ub_31 0.0498458213 _diffrn_orient_matrix_ub_32 -0.0112730073 _diffrn_orient_matrix_ub_33 0.0015304559 _diffrn_measurement_device_type 'Oxford Diffraction Gemini Diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_number 93408 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_full 30 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 38979 _reflns_number_gt 28362 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1563P)^2^+31.8882P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 38979 _refine_ls_number_parameters 1801 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0937 _refine_ls_wR_factor_ref 0.2841 _refine_ls_wR_factor_gt 0.2674 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.1 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 8.538 _refine_diff_density_min -6.298 _refine_diff_density_rms 0.2 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Gd1 Gd 0.43521(3) 0.32049(2) 0.662096(14) 0.04412(11) Uani 1 1 d . . . Gd2 Gd 0.33662(2) 0.122502(17) 0.880296(13) 0.03520(9) Uani 1 1 d . . . Gd3 Gd 0.94151(6) 0.48368(4) 0.48851(3) 0.04370(17) Uani 0.5 1 d P . . O11 O -0.0115(3) 0.4993(2) 0.93686(17) 0.0302(8) Uani 1 1 d . . . C11 C -0.0184(4) 0.4793(3) 0.8901(2) 0.0258(10) Uani 1 1 d . . . C12 C 0.0593(4) 0.4934(3) 0.8512(2) 0.0276(11) Uani 1 1 d . . . C13 C 0.0478(5) 0.4741(3) 0.8029(2) 0.0305(12) Uani 1 1 d . . . H13 H 0.099 0.4838 0.7759 0.037 Uiso 1 1 calc R . . C14 C -0.0376(5) 0.4408(3) 0.7934(3) 0.0330(13) Uani 1 1 d . . . S1 S -0.05608(17) 0.42116(10) 0.73063(7) 0.0463(4) Uani 1 1 d . . . O12 O 0.0322(6) 0.4394(5) 0.6989(3) 0.080(2) Uani 1 1 d . . . O13 O -0.0802(6) 0.3498(3) 0.7408(3) 0.069(2) Uani 1 1 d . . . O14 O -0.1429(5) 0.4623(4) 0.7070(2) 0.0595(16) Uani 1 1 d . . . C15 C -0.1124(5) 0.4260(3) 0.8326(2) 0.0308(12) Uani 1 1 d . . . H15 H -0.1697 0.4024 0.826 0.037 Uiso 1 1 calc R . . C16 C -0.1051(4) 0.4450(3) 0.8814(2) 0.0256(10) Uani 1 1 d . . . C1 C -0.1892(4) 0.4320(3) 0.9225(2) 0.0289(11) Uani 1 1 d . . . H1A H -0.2522 0.4364 0.9029 0.035 Uiso 1 1 calc R . . H1B H -0.1882 0.4682 0.9428 0.035 Uiso 1 1 calc R . . C21 C 0.2346(4) 0.4497(3) 0.9420(2) 0.0270(10) Uani 1 1 d . . . O21 O 0.1626(3) 0.4647(2) 0.97517(17) 0.0324(9) Uani 1 1 d . . . C22 C 0.3082(4) 0.4017(3) 0.9650(2) 0.0267(10) Uani 1 1 d . . . C23 C 0.3847(4) 0.3893(3) 0.9317(2) 0.0294(11) Uani 1 1 d . . . H23 H 0.4348 0.3571 0.9462 0.035 Uiso 1 1 calc R . . C24 C 0.3886(4) 0.4235(3) 0.8770(2) 0.0272(10) Uani 1 1 d . . . S2 S 0.49079(12) 0.40580(9) 0.83737(6) 0.0331(3) Uani 1 1 d . . . O22 O 0.5792(4) 0.4116(3) 0.8668(2) 0.0473(13) Uani 1 1 d . . . O23 O 0.4726(4) 0.3358(3) 0.8313(2) 0.0460(12) Uani 1 1 d . . . O24 O 0.4860(4) 0.4561(3) 0.78494(19) 0.0398(10) Uani 1 1 d . . . C25 C 0.3146(4) 0.4689(3) 0.8542(2) 0.0288(11) Uani 1 1 d . . . H25 H 0.3178 0.4908 0.8166 0.035 Uiso 1 1 calc R . . C26 C 0.2360(5) 0.4826(3) 0.8859(2) 0.0286(11) Uani 1 1 d . . . C2 C 0.1534(5) 0.5306(3) 0.8609(2) 0.0300(11) Uani 1 1 d . . . H2A H 0.1773 0.5601 0.8259 0.036 Uiso 1 1 calc R . . H2B H 0.1367 0.5609 0.8852 0.036 Uiso 1 1 calc R . . C31 C 0.1314(4) 0.3136(3) 1.0583(2) 0.0261(10) Uani 1 1 d . . . O31 O 0.1151(3) 0.3719(3) 1.0765(2) 0.0390(10) Uani 1 1 d . . . C32 C 0.0593(4) 0.2628(3) 1.0653(2) 0.0271(11) Uani 1 1 d . . . C33 C 0.0806(4) 0.2032(3) 1.0493(2) 0.0273(11) Uani 1 1 d . . . H33 H 0.0319 0.1682 1.0533 0.033 Uiso 1 1 calc R . . C34 C 0.1735(5) 0.1944(3) 1.0272(2) 0.0283(11) Uani 1 1 d . . . S3 S 0.19480(14) 0.11593(8) 1.00931(6) 0.0365(3) Uani 1 1 d . . . O32 O 0.2205(5) 0.0658(3) 1.0587(2) 0.0545(15) Uani 1 1 d . . . O33 O 0.1030(4) 0.0985(3) 0.9860(2) 0.0490(13) Uani 1 1 d . . . O34 O 0.2762(4) 0.1288(2) 0.96915(19) 0.0388(10) Uani 1 1 d . . . C35 C 0.2445(4) 0.2449(3) 1.0200(2) 0.0300(12) Uani 1 1 d . . . H35 H 0.3073 0.2381 1.0048 0.036 Uiso 1 1 calc R . . C36 C 0.2248(4) 0.3061(3) 1.0350(2) 0.0254(10) Uani 1 1 d . . . C3 C 0.3010(4) 0.3632(3) 1.0246(2) 0.0291(11) Uani 1 1 d . . . H3A H 0.3664 0.3434 1.0364 0.035 Uiso 1 1 calc R . . H3B H 0.2833 0.3961 1.0466 0.035 Uiso 1 1 calc R . . C41 C -0.1211(4) 0.3483(3) 1.0057(2) 0.0239(10) Uani 1 1 d . . . O41 O -0.0553(3) 0.3951(2) 1.01388(17) 0.0291(8) Uani 1 1 d . . . C42 C -0.1870(4) 0.3623(3) 0.9628(2) 0.0249(10) Uani 1 1 d . . . C43 C -0.2539(4) 0.3105(3) 0.9594(2) 0.0260(10) Uani 1 1 d . . . H43 H -0.2992 0.3186 0.9305 0.031 Uiso 1 1 calc R . . C44 C -0.2552(4) 0.2474(3) 0.9978(2) 0.0270(10) Uani 1 1 d . . . S4 S -0.34149(12) 0.18322(9) 0.99239(6) 0.0334(3) Uani 1 1 d . . . O42 O -0.4371(4) 0.2177(3) 0.9846(2) 0.0449(12) Uani 1 1 d . . . O43 O -0.3090(5) 0.1584(4) 0.9457(2) 0.0619(18) Uani 1 1 d . . . O44 O -0.3378(4) 0.1299(3) 1.0425(2) 0.0390(10) Uani 1 1 d . . . C45 C -0.1880(4) 0.2335(3) 1.0396(2) 0.0272(10) Uani 1 1 d . . . H45 H -0.1882 0.1901 1.0652 0.033 Uiso 1 1 calc R . . C46 C -0.1201(4) 0.2841(3) 1.0438(2) 0.0244(10) Uani 1 1 d . . . C4 C -0.0446(4) 0.2711(3) 1.0884(2) 0.0279(11) Uani 1 1 d . . . H4A H -0.0627 0.2289 1.1163 0.034 Uiso 1 1 calc R . . H4B H -0.0448 0.3101 1.1058 0.034 Uiso 1 1 calc R . . C51 C 0.7912(5) 0.1635(4) 0.4484(2) 0.0396(15) Uani 1 1 d . . . O51 O 0.8055(4) 0.0995(3) 0.4411(2) 0.0501(13) Uani 1 1 d . . . C52 C 0.7010(5) 0.1803(4) 0.4705(2) 0.0398(15) Uani 1 1 d . . . C53 C 0.6872(5) 0.2461(4) 0.4756(3) 0.0391(15) Uani 1 1 d . . . H53 H 0.6268 0.2581 0.4906 0.047 Uiso 1 1 calc R . . C54 C 0.7607(5) 0.2953(4) 0.4591(3) 0.0385(14) Uani 1 1 d . . . S5 S 0.73939(14) 0.37735(11) 0.46843(9) 0.0491(4) Uani 1 1 d . . . O52 O 0.7422(9) 0.4234(4) 0.4162(4) 0.107(3) Uani 1 1 d . . . O53 O 0.6450(5) 0.3761(4) 0.4955(4) 0.086(3) Uani 1 1 d . . . O54 O 0.8229(5) 0.3943(4) 0.4955(3) 0.0669(19) Uani 1 1 d . . . C55 C 0.8492(5) 0.2799(4) 0.4371(3) 0.0389(14) Uani 1 1 d . . . H55 H 0.8981 0.3145 0.4257 0.047 Uiso 1 1 calc R . . C56 C 0.8670(5) 0.2134(4) 0.4317(2) 0.0374(14) Uani 1 1 d . . . C5 C 0.9641(6) 0.1954(4) 0.4093(2) 0.0435(16) Uani 1 1 d . . . H5A H 0.9833 0.2322 0.377 0.052 Uiso 1 1 calc R . . H5B H 0.9566 0.1522 0.3975 0.052 Uiso 1 1 calc R . . C61 C 0.6959(5) 0.0644(4) 0.5799(2) 0.0339(13) Uani 1 1 d . . . O61 O 0.7637(4) 0.0403(3) 0.54946(19) 0.0387(10) Uani 1 1 d . . . C62 C 0.6997(5) 0.0470(3) 0.6366(2) 0.0318(12) Uani 1 1 d . . . C63 C 0.6243(5) 0.0691(4) 0.6656(3) 0.0377(14) Uani 1 1 d . . . H63 H 0.6259 0.0578 0.7041 0.045 Uiso 1 1 calc R . . C64 C 0.5459(5) 0.1076(4) 0.6391(3) 0.0377(14) Uani 1 1 d . . . S6 S 0.45057(13) 0.13488(11) 0.67627(8) 0.0439(4) Uani 1 1 d . . . O62 O 0.4480(4) 0.0875(4) 0.7296(2) 0.0584(16) Uani 1 1 d . . . O63 O 0.4803(4) 0.2033(3) 0.6793(3) 0.0529(14) Uani 1 1 d . . . O64 O 0.3588(4) 0.1351(4) 0.6469(3) 0.0595(16) Uani 1 1 d . . . C65 C 0.5450(5) 0.1272(4) 0.5824(3) 0.0394(14) Uani 1 1 d . . . H65 H 0.4934 0.1555 0.5644 0.047 Uiso 1 1 calc R . . C66 C 0.6194(5) 0.1054(4) 0.5526(3) 0.0361(13) Uani 1 1 d . . . C6 C 0.6213(5) 0.1264(4) 0.4913(3) 0.0425(16) Uani 1 1 d . . . H6A H 0.5561 0.1453 0.4783 0.051 Uiso 1 1 calc R . . H6B H 0.6345 0.0856 0.4769 0.051 Uiso 1 1 calc R . . C71 C 0.9546(5) 0.0301(3) 0.6248(2) 0.0309(12) Uani 1 1 d . . . O71 O 0.9308(4) -0.0024(3) 0.5865(2) 0.0489(13) Uani 1 1 d . . . C72 C 1.0487(5) 0.0582(3) 0.6255(3) 0.0365(14) Uani 1 1 d . . . C73 C 1.0716(5) 0.0909(3) 0.6667(3) 0.0361(13) Uani 1 1 d . . . H73 H 1.1354 0.11 0.6677 0.043 Uiso 1 1 calc R . . C74 C 1.0006(5) 0.0951(3) 0.7057(3) 0.0352(13) Uani 1 1 d . . . S7 S 1.02770(15) 0.13495(11) 0.75827(8) 0.0476(4) Uani 1 1 d . . . O72 O 1.1201(6) 0.1723(4) 0.7442(3) 0.074(2) Uani 1 1 d . . . O73 O 0.9475(6) 0.1832(4) 0.7599(3) 0.075(2) Uani 1 1 d . . . O74 O 1.0301(8) 0.0822(5) 0.8076(3) 0.091(3) Uani 1 1 d . . . C75 C 0.9070(5) 0.0675(3) 0.7046(2) 0.0332(12) Uani 1 1 d . . . H75 H 0.8592 0.0708 0.7317 0.04 Uiso 1 1 calc R . . C76 C 0.8826(5) 0.0353(3) 0.6643(2) 0.0294(11) Uani 1 1 d . . . C7 C 0.7814(5) 0.0024(3) 0.6654(2) 0.0340(13) Uani 1 1 d . . . H7A H 0.7885 -0.0376 0.6494 0.041 Uiso 1 1 calc R . . H7B H 0.7604 -0.0154 0.7038 0.041 Uiso 1 1 calc R . . C81 C 1.0495(5) 0.1257(4) 0.4937(2) 0.0381(14) Uani 1 1 d . . . O81 O 0.9828(4) 0.0768(3) 0.4960(2) 0.0452(12) Uani 1 1 d . . . C82 C 1.0458(5) 0.1861(4) 0.4509(2) 0.0368(14) Uani 1 1 d . . . C83 C 1.1149(5) 0.2367(4) 0.4480(2) 0.0360(13) Uani 1 1 d . . . H83 H 1.1132 0.2769 0.419 0.043 Uiso 1 1 calc R . . C84 C 1.1868(5) 0.2301(4) 0.4865(3) 0.0359(13) Uani 1 1 d . . . S8 S 1.27495(12) 0.29571(10) 0.48316(7) 0.0387(4) Uani 1 1 d . . . O82 O 1.2775(4) 0.3360(3) 0.4277(2) 0.0506(14) Uani 1 1 d . . . O83 O 1.2388(4) 0.3352(3) 0.5215(2) 0.0508(13) Uani 1 1 d . . . O84 O 1.3689(4) 0.2612(3) 0.5006(2) 0.0437(11) Uani 1 1 d . . . C85 C 1.1896(5) 0.1705(4) 0.5296(3) 0.0360(13) Uani 1 1 d . . . H85 H 1.2393 0.1659 0.5561 0.043 Uiso 1 1 calc R . . C86 C 1.1221(5) 0.1196(4) 0.5337(3) 0.0338(12) Uani 1 1 d . . . C8 C 1.1263(5) 0.0565(4) 0.5818(3) 0.0389(14) Uani 1 1 d . . . H8A H 1.1166 0.0146 0.5686 0.047 Uiso 1 1 calc R . . H8B H 1.1926 0.0537 0.5978 0.047 Uiso 1 1 calc R . . N91 N 0.0164(4) 0.2617(3) 0.8777(2) 0.0366(12) Uani 1 1 d . . . C92 C 0.0564(5) 0.2716(3) 0.8286(3) 0.0347(13) Uani 1 1 d . . . H92 H 0.0292 0.2569 0.7992 0.042 Uiso 1 1 calc R . . N93 N 0.1409(4) 0.3056(3) 0.8269(2) 0.0299(10) Uani 1 1 d . . . C94 C 0.1557(6) 0.3163(3) 0.8775(3) 0.0387(14) Uani 1 1 d . . . H94 H 0.2108 0.3386 0.8882 0.046 Uiso 1 1 calc R . . C95 C 0.0778(6) 0.2895(3) 0.9089(3) 0.0374(14) Uani 1 1 d . . . H95 H 0.0671 0.2897 0.9459 0.045 Uiso 1 1 calc R . . C96 C -0.0762(7) 0.2241(6) 0.8961(5) 0.067(3) Uani 1 1 d . . . H96A H -0.0936 0.197 0.8705 0.1 Uiso 1 1 calc R . . H96B H -0.1292 0.257 0.8978 0.1 Uiso 1 1 calc R . . H96C H -0.0674 0.1934 0.9321 0.1 Uiso 1 1 calc R . . C97 C 0.2072(6) 0.3242(4) 0.7805(3) 0.0415(15) Uani 1 1 d . . . H97A H 0.2394 0.3684 0.7804 0.05 Uiso 1 1 calc R . . H97B H 0.1682 0.3314 0.7471 0.05 Uiso 1 1 calc R . . C98 C 0.2865(5) 0.2709(3) 0.7794(3) 0.0353(13) Uani 1 1 d . . . O91 O 0.3013(3) 0.2267(2) 0.82267(19) 0.0352(9) Uani 1 1 d . . . O92 O 0.3310(5) 0.2767(3) 0.7356(2) 0.0518(14) Uani 1 1 d . . . N101 N 1.1692(6) 0.7580(4) 0.3797(3) 0.0533(17) Uani 1 1 d . . . C102 C 1.1079(6) 0.7273(5) 0.3540(3) 0.0486(18) Uani 1 1 d . . . H102 H 1.1235 0.7086 0.324 0.058 Uiso 1 1 calc R . . N103 N 1.0201(5) 0.7272(5) 0.3780(3) 0.0559(18) Uani 1 1 d . . . C104 C 1.0269(8) 0.7569(6) 0.4207(4) 0.063(3) Uani 1 1 d . . . H104 H 0.9755 0.7612 0.4457 0.076 Uiso 1 1 calc R . . C105 C 1.1193(10) 0.7784(5) 0.4204(3) 0.066(3) Uani 1 1 d . . . H105 H 1.1459 0.8034 0.444 0.08 Uiso 1 1 calc R . . C106 C 1.2752(9) 0.7633(9) 0.3679(7) 0.104(5) Uani 1 1 d . . . H10A H 1.3053 0.7177 0.3791 0.155 Uiso 1 1 calc R . . H10B H 1.305 0.794 0.3878 0.155 Uiso 1 1 calc R . . H10C H 1.2866 0.782 0.3289 0.155 Uiso 1 1 calc R . . C107 C 0.9322(12) 0.6877(9) 0.3651(7) 0.103(3) Uani 1 1 d U . . H10D H 0.9359 0.6847 0.3268 0.123 Uiso 1 1 calc R . . H10E H 0.8696 0.7106 0.3712 0.123 Uiso 1 1 calc R . . C108 C 0.9383(14) 0.6100(9) 0.4067(7) 0.110(2) Uani 1 1 d U . . O101 O 0.8568(8) 0.5723(6) 0.4102(5) 0.109(3) Uani 1 1 d U . . O102 O 1.0453(10) 0.5793(6) 0.4243(5) 0.124(3) Uani 1 1 d U . . P1 P -0.28418(10) 0.80473(7) 0.75488(5) 0.0226(3) Uani 1 1 d . . . C111 C -0.3344(4) 0.8411(3) 0.6896(2) 0.0234(10) Uani 1 1 d . . . C112 C -0.4158(4) 0.8861(3) 0.6840(2) 0.0231(10) Uani 1 1 d . . . H112 H -0.4487 0.8938 0.7153 0.028 Uiso 1 1 calc R . . C113 C -0.4478(4) 0.9190(3) 0.6329(2) 0.0244(10) Uani 1 1 d . . . H113 H -0.5043 0.9478 0.6294 0.029 Uiso 1 1 calc R . . C114 C -0.3984(4) 0.9104(3) 0.5868(2) 0.0248(10) Uani 1 1 d . . . C115 C -0.3195(4) 0.8635(3) 0.5917(2) 0.0267(10) Uani 1 1 d . . . H115 H -0.2874 0.8557 0.5602 0.032 Uiso 1 1 calc R . . C116 C -0.2887(4) 0.8287(3) 0.6428(2) 0.0275(11) Uani 1 1 d . . . H116 H -0.2365 0.7962 0.6461 0.033 Uiso 1 1 calc R . . O117 O -0.4306(3) 0.9473(2) 0.53864(17) 0.0318(9) Uani 1 1 d . . . C117 C -0.3771(5) 0.9408(4) 0.4909(2) 0.0358(13) Uani 1 1 d . . . H11A H -0.3078 0.9534 0.4933 0.054 Uiso 1 1 calc R . . H11B H -0.4061 0.9714 0.4588 0.054 Uiso 1 1 calc R . . H11C H -0.3809 0.8932 0.4879 0.054 Uiso 1 1 calc R . . C121 C -0.2801(4) 0.7132(3) 0.7657(2) 0.0235(10) Uani 1 1 d . . . C122 C -0.3236(4) 0.6798(3) 0.7303(2) 0.0293(11) Uani 1 1 d . . . H122 H -0.3552 0.7057 0.6988 0.035 Uiso 1 1 calc R . . C123 C -0.3207(4) 0.6082(3) 0.7410(3) 0.0323(12) Uani 1 1 d . . . H123 H -0.3497 0.5856 0.7165 0.039 Uiso 1 1 calc R . . C124 C -0.2756(4) 0.5699(3) 0.7873(3) 0.0308(12) Uani 1 1 d . . . H124 H -0.2747 0.5211 0.7946 0.037 Uiso 1 1 calc R . . C125 C -0.2317(4) 0.6030(3) 0.8232(2) 0.0287(11) Uani 1 1 d . . . H125 H -0.2008 0.5768 0.8548 0.034 Uiso 1 1 calc R . . C126 C -0.2335(4) 0.6748(3) 0.8123(2) 0.0266(10) Uani 1 1 d . . . H126 H -0.2033 0.6976 0.8363 0.032 Uiso 1 1 calc R . . C131 C -0.1622(4) 0.8381(3) 0.7590(2) 0.0254(10) Uani 1 1 d . . . C132 C -0.0962(4) 0.8528(4) 0.7136(3) 0.0352(13) Uani 1 1 d . . . H132 H -0.1157 0.8442 0.6803 0.042 Uiso 1 1 calc R . . C133 C -0.0036(4) 0.8797(4) 0.7175(3) 0.0349(13) Uani 1 1 d . . . H133 H 0.0404 0.8891 0.6869 0.042 Uiso 1 1 calc R . . C134 C 0.0253(4) 0.8931(3) 0.7658(3) 0.0319(12) Uani 1 1 d . . . H134 H 0.089 0.9115 0.7683 0.038 Uiso 1 1 calc R . . C135 C -0.0386(5) 0.8797(4) 0.8104(3) 0.0368(14) Uani 1 1 d . . . H135 H -0.0192 0.8895 0.8433 0.044 Uiso 1 1 calc R . . C136 C -0.1315(4) 0.8518(3) 0.8067(2) 0.0319(12) Uani 1 1 d . . . H136 H -0.1745 0.8419 0.8377 0.038 Uiso 1 1 calc R . . C141 C -0.3576(4) 0.8277(3) 0.8070(2) 0.0280(11) Uani 1 1 d . . . C142 C -0.3599(6) 0.8965(4) 0.8087(3) 0.0394(15) Uani 1 1 d . . . H142 H -0.3255 0.93 0.7816 0.047 Uiso 1 1 calc R . . C143 C -0.4129(7) 0.9165(4) 0.8503(3) 0.0506(19) Uani 1 1 d . . . H143 H -0.4136 0.9634 0.8517 0.061 Uiso 1 1 calc R . . C144 C -0.4640(6) 0.8679(4) 0.8890(3) 0.0474(18) Uani 1 1 d . . . H144 H -0.5001 0.8813 0.9171 0.057 Uiso 1 1 calc R . . C145 C -0.4627(5) 0.7981(4) 0.8869(3) 0.0406(15) Uani 1 1 d . . . H145 H -0.4985 0.7647 0.9134 0.049 Uiso 1 1 calc R . . C146 C -0.4092(4) 0.7783(3) 0.8460(2) 0.0294(11) Uani 1 1 d . . . H146 H -0.4077 0.7314 0.8447 0.035 Uiso 1 1 calc R . . P2 P 0.31533(9) 0.71455(7) 0.74432(5) 0.0209(2) Uani 1 1 d . . . C211 C 0.3611(4) 0.6731(3) 0.8098(2) 0.0215(9) Uani 1 1 d . . . C212 C 0.4491(4) 0.6346(3) 0.8146(2) 0.0241(10) Uani 1 1 d . . . H212 H 0.4855 0.6318 0.7829 0.029 Uiso 1 1 calc R . . C213 C 0.4829(4) 0.6009(3) 0.8651(2) 0.0250(10) Uani 1 1 d . . . H213 H 0.5419 0.5746 0.8681 0.03 Uiso 1 1 calc R . . C214 C 0.4296(4) 0.6057(3) 0.9117(2) 0.0233(10) Uani 1 1 d . . . C215 C 0.3426(4) 0.6434(3) 0.9078(2) 0.0271(11) Uani 1 1 d . . . H215 H 0.3064 0.6462 0.9396 0.033 Uiso 1 1 calc R . . C216 C 0.3093(4) 0.6771(3) 0.8570(2) 0.0275(11) Uani 1 1 d . . . H216 H 0.2502 0.7032 0.8542 0.033 Uiso 1 1 calc R . . O217 O 0.4677(3) 0.5701(2) 0.95881(16) 0.0297(8) Uani 1 1 d . . . C217 C 0.4086(5) 0.5666(4) 1.0069(2) 0.0346(13) Uani 1 1 d . . . H21A H 0.4065 0.6119 1.0148 0.052 Uiso 1 1 calc R . . H21B H 0.4375 0.5332 1.0374 0.052 Uiso 1 1 calc R . . H21C H 0.3414 0.5522 1.0012 0.052 Uiso 1 1 calc R . . C221 C 0.3153(4) 0.8063(3) 0.7343(2) 0.0243(10) Uani 1 1 d . . . C222 C 0.3556(4) 0.8384(3) 0.7713(3) 0.0304(11) Uani 1 1 d . . . H222 H 0.3858 0.8119 0.803 0.036 Uiso 1 1 calc R . . C223 C 0.3516(5) 0.9105(4) 0.7613(3) 0.0414(15) Uani 1 1 d . . . H223 H 0.3778 0.933 0.7867 0.05 Uiso 1 1 calc R . . C224 C 0.3093(5) 0.9482(3) 0.7146(4) 0.0429(16) Uani 1 1 d . . . H224 H 0.307 0.9969 0.7078 0.051 Uiso 1 1 calc R . . C225 C 0.2709(5) 0.9170(3) 0.6779(3) 0.0399(15) Uani 1 1 d . . . H225 H 0.2434 0.9441 0.6456 0.048 Uiso 1 1 calc R . . C226 C 0.2715(4) 0.8459(3) 0.6873(3) 0.0306(11) Uani 1 1 d . . . H226 H 0.2425 0.8242 0.6621 0.037 Uiso 1 1 calc R . . C231 C 0.1892(4) 0.6900(3) 0.7381(2) 0.0220(9) Uani 1 1 d . . . C232 C 0.1167(4) 0.7145(3) 0.7687(2) 0.0296(11) Uani 1 1 d . . . H232 H 0.1339 0.745 0.7902 0.036 Uiso 1 1 calc R . . C233 C 0.0180(4) 0.6935(4) 0.7672(3) 0.0358(13) Uani 1 1 d . . . H233 H -0.0311 0.7087 0.7887 0.043 Uiso 1 1 calc R . . C234 C -0.0079(4) 0.6508(4) 0.7346(3) 0.0342(13) Uani 1 1 d . . . H234 H -0.0744 0.636 0.7342 0.041 Uiso 1 1 calc R . . C235 C 0.0637(4) 0.6296(3) 0.7023(2) 0.0313(12) Uani 1 1 d . . . H235 H 0.0455 0.6022 0.6785 0.038 Uiso 1 1 calc R . . C236 C 0.1630(4) 0.6484(3) 0.7046(2) 0.0288(11) Uani 1 1 d . . . H236 H 0.212 0.6327 0.6832 0.035 Uiso 1 1 calc R . . C241 C 0.3903(4) 0.6889(3) 0.6937(2) 0.0226(9) Uani 1 1 d . . . C242 C 0.4398(4) 0.7382(3) 0.6531(2) 0.0239(10) Uani 1 1 d . . . H242 H 0.4336 0.7858 0.6517 0.029 Uiso 1 1 calc R . . C243 C 0.4982(4) 0.7164(3) 0.6150(2) 0.0284(11) Uani 1 1 d . . . H243 H 0.5333 0.7493 0.5878 0.034 Uiso 1 1 calc R . . C244 C 0.5057(4) 0.6468(4) 0.6162(3) 0.0335(12) Uani 1 1 d . . . H244 H 0.5439 0.6326 0.5892 0.04 Uiso 1 1 calc R . . C245 C 0.4572(4) 0.5978(3) 0.6570(3) 0.0325(12) Uani 1 1 d . . . H245 H 0.4631 0.5502 0.6582 0.039 Uiso 1 1 calc R . . C246 C 0.4002(4) 0.6193(3) 0.6960(2) 0.0289(11) Uani 1 1 d . . . H246 H 0.3679 0.5862 0.7242 0.035 Uiso 1 1 calc R . . O1 O 0.6329(4) 0.0200(3) 0.9568(2) 0.0503(13) Uani 1 1 d . . . O2 O 0.7654(6) 0.5094(3) 0.3133(3) 0.0665(18) Uani 1 1 d . . . O3 O 0.1811(11) 0.9566(6) 0.1543(6) 0.072(4) Uani 0.5 1 d P . . O4 O 0.5311(6) 0.4939(5) 0.4507(4) 0.038(2) Uani 0.5 1 d P . . O5 O 0.1292(10) 0.9579(6) 0.8625(5) 0.054(3) Uani 0.5 1 d P . . O6 O 0.6465(6) 0.4603(5) 0.7059(4) 0.0348(19) Uani 0.5 1 d P . . O7 O 0.7317(8) 0.2704(6) 0.7545(4) 0.050(3) Uani 0.5 1 d P . . O8 O 0.6784(7) 0.1518(5) 0.8392(3) 0.0338(19) Uani 0.5 1 d P . . O9 O 0.8774(7) 0.5927(4) 0.6305(5) 0.047(3) Uani 0.5 1 d P . . O111 O 0.3010(4) 0.2698(4) 0.6263(2) 0.0577(16) Uani 1 1 d . . . O112 O 0.3442(5) 0.4091(4) 0.6002(3) 0.0640(18) Uani 1 1 d . . . O113 O 0.4055(5) 0.4180(3) 0.7000(3) 0.0600(16) Uani 1 1 d . . . O114 O 0.5394(5) 0.3026(4) 0.7391(3) 0.0613(17) Uani 1 1 d . . . O115 O 0.4924(4) 0.3075(4) 0.5718(2) 0.0614(17) Uani 1 1 d . . . O116 O 0.5907(13) 0.3703(11) 0.6377(8) 0.081(4) Uani 0.5 1 d PU . . O118 O 0.5674(13) 0.4078(11) 0.6294(8) 0.081(4) Uani 0.5 1 d PU . . O211 O 0.2932(9) 0.0024(4) 0.8999(4) 0.110(4) Uani 1 1 d . . . O212 O 0.4438(5) 0.0563(4) 0.9448(3) 0.0630(17) Uani 1 1 d . . . O213 O 0.4321(4) 0.2105(3) 0.9041(2) 0.0510(14) Uani 1 1 d . . . O214 O 0.1591(4) 0.1219(3) 0.87895(19) 0.0403(11) Uani 1 1 d . . . O215 O 0.2853(4) 0.0960(3) 0.7949(2) 0.0522(14) Uani 1 1 d . . . O216 O 0.4828(4) 0.1157(4) 0.8283(3) 0.0653(19) Uani 1 1 d . . . O311 O 0.9760(9) 0.4567(6) 0.4028(5) 0.053(3) Uani 0.5 1 d P . . O312 O 1.0177(17) 0.3629(9) 0.5032(9) 0.105(6) Uani 0.5 1 d P . . O313 O 0.7926(10) 0.5304(7) 0.5175(5) 0.057(3) Uani 0.5 1 d P . . O314 O 0.9934(13) 0.5614(12) 0.5394(8) 0.104(7) Uani 0.5 1 d P . . O315 O 1.114(2) 0.4633(16) 0.5003(11) 0.164(14) Uani 0.5 1 d P . . 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 Gd1 0.04141(19) 0.0611(2) 0.03047(17) -0.01239(15) 0.00177(13) -0.01340(16) Gd2 0.04160(18) 0.03190(16) 0.03024(16) -0.00474(11) 0.00386(12) 0.00952(12) Gd3 0.0535(4) 0.0333(3) 0.0452(4) -0.0112(3) -0.0016(3) -0.0127(3) O11 0.033(2) 0.029(2) 0.031(2) -0.0126(17) -0.0055(16) -0.0019(16) C11 0.034(3) 0.018(2) 0.027(3) -0.0078(19) -0.009(2) 0.0072(19) C12 0.035(3) 0.018(2) 0.028(3) -0.0019(19) -0.011(2) 0.003(2) C13 0.043(3) 0.022(3) 0.026(3) -0.004(2) -0.009(2) 0.004(2) C14 0.048(3) 0.021(3) 0.031(3) -0.008(2) -0.017(2) 0.008(2) S1 0.0727(13) 0.0412(9) 0.0264(7) -0.0094(7) -0.0198(8) 0.0040(8) O12 0.076(5) 0.130(7) 0.051(4) -0.053(4) -0.006(3) -0.006(5) O13 0.127(6) 0.041(3) 0.045(3) -0.019(3) -0.035(4) 0.006(3) O14 0.068(4) 0.064(4) 0.041(3) -0.001(3) -0.023(3) 0.005(3) C15 0.042(3) 0.019(2) 0.031(3) -0.006(2) -0.017(2) 0.005(2) C16 0.030(3) 0.017(2) 0.030(3) -0.0056(19) -0.012(2) 0.0065(19) C1 0.030(3) 0.020(2) 0.035(3) -0.005(2) -0.012(2) 0.005(2) C21 0.031(3) 0.026(3) 0.025(2) -0.008(2) -0.007(2) -0.001(2) O21 0.034(2) 0.038(2) 0.029(2) -0.0146(18) -0.0085(16) 0.0092(18) C22 0.031(3) 0.029(3) 0.022(2) -0.009(2) -0.0081(19) -0.003(2) C23 0.028(3) 0.034(3) 0.026(3) -0.007(2) -0.006(2) 0.000(2) C24 0.028(3) 0.027(3) 0.027(3) -0.007(2) -0.0033(19) -0.004(2) S2 0.0341(7) 0.0370(8) 0.0281(7) -0.0078(6) 0.0000(5) -0.0042(6) O22 0.029(2) 0.075(4) 0.039(3) -0.016(3) -0.0042(19) -0.002(2) O23 0.066(3) 0.036(3) 0.035(2) -0.008(2) 0.012(2) -0.005(2) O24 0.044(3) 0.043(3) 0.031(2) -0.0053(19) 0.0044(19) -0.004(2) C25 0.032(3) 0.024(3) 0.028(3) -0.002(2) -0.008(2) -0.006(2) C26 0.037(3) 0.021(2) 0.027(3) -0.003(2) -0.008(2) -0.003(2) C2 0.038(3) 0.020(2) 0.030(3) -0.001(2) -0.009(2) -0.003(2) C31 0.024(2) 0.033(3) 0.022(2) -0.006(2) -0.0114(18) 0.006(2) O31 0.035(2) 0.038(3) 0.050(3) -0.023(2) -0.013(2) 0.0072(19) C32 0.026(2) 0.034(3) 0.019(2) -0.004(2) -0.0058(18) 0.008(2) C33 0.034(3) 0.028(3) 0.018(2) -0.0016(19) -0.0032(19) 0.005(2) C34 0.042(3) 0.025(3) 0.017(2) -0.0027(19) -0.001(2) 0.006(2) S3 0.0519(9) 0.0277(7) 0.0280(7) -0.0042(6) 0.0076(6) 0.0060(6) O32 0.078(4) 0.037(3) 0.040(3) 0.006(2) 0.016(3) 0.021(3) O33 0.062(3) 0.046(3) 0.045(3) -0.023(2) 0.013(2) -0.010(2) O34 0.052(3) 0.033(2) 0.030(2) -0.0049(18) 0.0078(19) 0.009(2) C35 0.031(3) 0.038(3) 0.019(2) -0.003(2) -0.0029(19) 0.010(2) C36 0.029(3) 0.031(3) 0.015(2) -0.0031(19) -0.0090(18) 0.006(2) C3 0.029(3) 0.037(3) 0.020(2) -0.004(2) -0.0097(19) 0.000(2) C41 0.024(2) 0.022(2) 0.029(3) -0.011(2) -0.0078(19) 0.0024(18) O41 0.034(2) 0.0197(18) 0.034(2) -0.0058(15) -0.0156(16) -0.0007(15) C42 0.025(2) 0.023(2) 0.028(3) -0.008(2) -0.0085(19) 0.0060(19) C43 0.021(2) 0.032(3) 0.026(2) -0.009(2) -0.0063(18) 0.0018(19) C44 0.027(2) 0.030(3) 0.026(2) -0.010(2) 0.0028(19) -0.001(2) S4 0.0345(7) 0.0353(8) 0.0306(7) -0.0087(6) 0.0044(5) -0.0114(6) O42 0.031(2) 0.056(3) 0.041(3) 0.001(2) -0.0071(19) -0.008(2) O43 0.076(4) 0.071(4) 0.048(3) -0.034(3) 0.023(3) -0.040(3) O44 0.037(2) 0.033(2) 0.044(3) -0.005(2) 0.0009(19) -0.0063(18) C45 0.031(3) 0.023(3) 0.026(2) -0.003(2) 0.002(2) 0.003(2) C46 0.024(2) 0.026(3) 0.023(2) -0.0068(19) -0.0023(18) 0.0043(19) C4 0.028(3) 0.030(3) 0.025(2) -0.005(2) -0.0034(19) 0.004(2) C51 0.050(4) 0.047(4) 0.018(2) 0.000(2) -0.004(2) -0.014(3) O51 0.060(3) 0.053(3) 0.035(3) -0.008(2) 0.004(2) -0.008(3) C52 0.041(3) 0.054(4) 0.022(3) -0.005(3) -0.004(2) -0.019(3) C53 0.033(3) 0.055(4) 0.027(3) -0.006(3) -0.005(2) -0.016(3) C54 0.039(3) 0.046(4) 0.032(3) -0.011(3) -0.006(2) -0.011(3) S5 0.0404(9) 0.0442(10) 0.0633(12) -0.0136(9) -0.0102(8) -0.0121(7) O52 0.154(9) 0.047(4) 0.116(8) -0.011(5) 0.018(7) -0.022(5) O53 0.054(4) 0.058(4) 0.147(8) -0.033(5) 0.038(4) -0.015(3) O54 0.051(3) 0.072(4) 0.092(5) -0.048(4) -0.005(3) -0.015(3) C55 0.041(3) 0.047(4) 0.028(3) -0.006(3) -0.002(2) -0.015(3) C56 0.042(3) 0.051(4) 0.019(2) -0.006(2) -0.001(2) -0.009(3) C5 0.052(4) 0.058(4) 0.017(3) -0.003(3) 0.007(2) -0.008(3) C61 0.036(3) 0.042(3) 0.025(3) -0.011(2) 0.004(2) -0.014(3) O61 0.041(2) 0.048(3) 0.028(2) -0.0105(19) 0.0060(18) -0.008(2) C62 0.036(3) 0.034(3) 0.026(3) -0.007(2) 0.000(2) -0.011(2) C63 0.046(4) 0.038(3) 0.030(3) -0.011(3) 0.006(2) -0.014(3) C64 0.034(3) 0.044(4) 0.037(3) -0.014(3) 0.001(2) -0.009(3) S6 0.0367(8) 0.0557(11) 0.0436(9) -0.0210(8) 0.0070(7) -0.0088(7) O62 0.051(3) 0.087(5) 0.039(3) -0.020(3) 0.014(2) -0.005(3) O63 0.042(3) 0.068(4) 0.060(3) -0.037(3) -0.002(2) -0.010(3) O64 0.035(3) 0.086(5) 0.068(4) -0.039(4) -0.004(2) -0.009(3) C65 0.036(3) 0.049(4) 0.032(3) -0.010(3) 0.000(2) -0.011(3) C66 0.039(3) 0.043(4) 0.026(3) -0.006(2) -0.003(2) -0.015(3) C6 0.042(4) 0.056(4) 0.027(3) -0.006(3) -0.003(2) -0.018(3) C71 0.046(3) 0.025(3) 0.021(2) -0.004(2) 0.002(2) -0.002(2) O71 0.057(3) 0.059(3) 0.036(3) -0.023(2) 0.009(2) -0.010(3) C72 0.048(4) 0.028(3) 0.027(3) 0.004(2) 0.007(2) 0.008(3) C73 0.040(3) 0.029(3) 0.036(3) -0.002(2) 0.001(2) -0.002(2) C74 0.044(3) 0.032(3) 0.031(3) -0.011(2) 0.001(2) -0.003(3) S7 0.0537(10) 0.0576(12) 0.0383(9) -0.0241(8) -0.0025(7) -0.0116(9) O72 0.088(5) 0.079(5) 0.060(4) -0.026(4) 0.002(4) -0.034(4) O73 0.071(4) 0.096(6) 0.082(5) -0.063(5) -0.010(4) 0.003(4) O74 0.146(8) 0.082(5) 0.048(4) -0.021(4) -0.022(4) -0.033(5) C75 0.042(3) 0.030(3) 0.026(3) -0.005(2) -0.001(2) -0.003(2) C76 0.039(3) 0.024(3) 0.022(2) -0.001(2) 0.003(2) -0.007(2) C7 0.044(3) 0.033(3) 0.023(3) -0.004(2) 0.005(2) -0.011(2) C81 0.042(3) 0.050(4) 0.022(3) -0.007(3) 0.009(2) 0.004(3) O81 0.056(3) 0.043(3) 0.035(2) -0.007(2) 0.004(2) -0.007(2) C82 0.038(3) 0.048(4) 0.022(3) -0.005(2) 0.007(2) 0.000(3) C83 0.035(3) 0.046(4) 0.024(3) -0.005(2) 0.009(2) 0.002(3) C84 0.032(3) 0.046(4) 0.029(3) -0.009(3) 0.011(2) -0.001(3) S8 0.0282(7) 0.0478(9) 0.0356(8) -0.0022(7) 0.0027(6) -0.0028(6) O82 0.032(2) 0.062(4) 0.044(3) 0.013(2) 0.000(2) -0.007(2) O83 0.039(3) 0.063(4) 0.054(3) -0.022(3) 0.000(2) 0.000(2) O84 0.034(2) 0.054(3) 0.038(3) -0.004(2) 0.0012(19) 0.004(2) C85 0.032(3) 0.046(4) 0.030(3) -0.009(3) 0.006(2) 0.005(3) C86 0.033(3) 0.039(3) 0.029(3) -0.009(2) 0.009(2) 0.002(2) C8 0.042(3) 0.034(3) 0.037(3) -0.003(3) 0.010(3) 0.006(3) N91 0.040(3) 0.028(3) 0.043(3) -0.013(2) 0.000(2) 0.005(2) C92 0.040(3) 0.032(3) 0.036(3) -0.015(2) -0.006(2) 0.003(2) N93 0.041(3) 0.025(2) 0.025(2) -0.0067(18) -0.0072(19) 0.0039(19) C94 0.057(4) 0.029(3) 0.032(3) -0.009(2) -0.015(3) 0.002(3) C95 0.057(4) 0.028(3) 0.027(3) -0.005(2) -0.008(3) 0.010(3) C96 0.050(5) 0.067(6) 0.093(8) -0.040(6) 0.026(5) -0.009(4) C97 0.051(4) 0.034(3) 0.032(3) 0.004(3) 0.004(3) 0.001(3) C98 0.038(3) 0.034(3) 0.033(3) -0.008(2) 0.001(2) -0.012(2) O91 0.033(2) 0.036(2) 0.034(2) -0.0033(18) -0.0072(17) -0.0028(18) O92 0.066(4) 0.050(3) 0.039(3) -0.012(2) 0.018(2) -0.010(3) N101 0.070(5) 0.046(4) 0.047(4) -0.015(3) -0.011(3) -0.005(3) C102 0.044(4) 0.062(5) 0.050(4) -0.034(4) 0.001(3) -0.010(3) N103 0.047(4) 0.083(5) 0.041(3) -0.021(3) 0.002(3) 0.001(3) C104 0.074(6) 0.080(7) 0.043(4) -0.029(4) 0.001(4) 0.022(5) C105 0.121(9) 0.044(5) 0.038(4) -0.016(3) -0.021(5) 0.010(5) C106 0.057(6) 0.126(12) 0.126(12) -0.027(10) -0.009(7) -0.036(7) C107 0.104(5) 0.113(5) 0.096(5) -0.032(5) -0.003(5) -0.021(5) C108 0.115(4) 0.111(4) 0.104(4) -0.028(4) -0.010(4) -0.021(4) O101 0.108(5) 0.109(5) 0.109(5) -0.027(4) -0.002(4) -0.010(4) O102 0.143(5) 0.118(5) 0.107(5) -0.017(4) -0.033(4) -0.031(4) P1 0.0191(6) 0.0228(6) 0.0215(6) 0.0027(5) -0.0027(4) 0.0004(5) C111 0.020(2) 0.022(2) 0.025(2) 0.0013(18) -0.0029(17) 0.0011(18) C112 0.019(2) 0.022(2) 0.024(2) 0.0015(18) -0.0023(17) 0.0012(18) C113 0.022(2) 0.022(2) 0.025(2) 0.0011(19) -0.0031(18) 0.0017(18) C114 0.022(2) 0.028(3) 0.024(2) -0.004(2) -0.0051(18) 0.0009(19) C115 0.026(2) 0.030(3) 0.024(2) -0.005(2) -0.0058(19) 0.003(2) C116 0.023(2) 0.031(3) 0.026(3) -0.002(2) -0.0046(19) 0.006(2) O117 0.028(2) 0.040(2) 0.0249(19) -0.0026(17) -0.0061(15) 0.0073(17) C117 0.031(3) 0.050(4) 0.027(3) -0.009(3) -0.013(2) 0.011(3) C121 0.018(2) 0.023(2) 0.026(2) -0.0003(19) -0.0042(17) -0.0010(17) C122 0.025(2) 0.030(3) 0.031(3) -0.003(2) -0.010(2) 0.002(2) C123 0.029(3) 0.027(3) 0.042(3) -0.009(2) -0.014(2) 0.004(2) C124 0.027(3) 0.024(3) 0.040(3) -0.005(2) -0.009(2) 0.002(2) C125 0.029(3) 0.027(3) 0.027(3) -0.001(2) -0.005(2) 0.006(2) C126 0.027(2) 0.026(3) 0.023(2) 0.0012(19) -0.0025(19) 0.002(2) C131 0.024(2) 0.022(2) 0.027(2) -0.0002(19) -0.0049(19) 0.0016(19) C132 0.025(3) 0.048(4) 0.035(3) -0.015(3) 0.002(2) -0.002(2) C133 0.020(2) 0.046(4) 0.038(3) -0.010(3) 0.000(2) 0.002(2) C134 0.023(2) 0.032(3) 0.037(3) -0.001(2) -0.004(2) -0.004(2) C135 0.036(3) 0.044(4) 0.026(3) 0.001(2) -0.007(2) -0.010(3) C136 0.031(3) 0.038(3) 0.022(2) 0.001(2) -0.002(2) -0.009(2) C141 0.023(2) 0.034(3) 0.022(2) 0.003(2) -0.0015(18) 0.004(2) C142 0.054(4) 0.033(3) 0.027(3) 0.001(2) 0.011(3) 0.004(3) C143 0.066(5) 0.047(4) 0.035(3) -0.003(3) 0.013(3) 0.018(4) C144 0.044(4) 0.060(5) 0.032(3) -0.001(3) 0.012(3) 0.014(3) C145 0.027(3) 0.054(4) 0.032(3) 0.005(3) 0.007(2) 0.001(3) C146 0.023(2) 0.034(3) 0.026(3) 0.002(2) -0.0022(19) -0.004(2) P2 0.0193(5) 0.0215(6) 0.0200(6) -0.0014(5) -0.0005(4) -0.0008(4) C211 0.018(2) 0.023(2) 0.021(2) -0.0013(18) -0.0006(16) -0.0002(17) C212 0.018(2) 0.027(3) 0.024(2) 0.0006(19) 0.0045(17) 0.0013(18) C213 0.018(2) 0.026(3) 0.029(3) -0.002(2) 0.0024(18) 0.0044(18) C214 0.019(2) 0.026(3) 0.024(2) -0.0028(19) -0.0033(17) 0.0030(18) C215 0.021(2) 0.038(3) 0.021(2) -0.005(2) -0.0015(18) 0.007(2) C216 0.022(2) 0.038(3) 0.022(2) -0.006(2) -0.0025(18) 0.009(2) O217 0.0268(19) 0.036(2) 0.0232(18) -0.0022(16) -0.0045(14) 0.0094(16) C217 0.034(3) 0.045(4) 0.024(3) -0.006(2) -0.003(2) 0.014(3) C221 0.023(2) 0.023(2) 0.026(2) -0.0031(19) 0.0023(18) -0.0014(18) C222 0.026(3) 0.028(3) 0.039(3) -0.009(2) -0.006(2) 0.000(2) C223 0.035(3) 0.033(3) 0.062(4) -0.022(3) -0.010(3) -0.003(3) C224 0.036(3) 0.023(3) 0.069(5) -0.008(3) -0.001(3) -0.001(2) C225 0.038(3) 0.027(3) 0.048(4) 0.003(3) -0.001(3) 0.000(2) C226 0.031(3) 0.025(3) 0.032(3) 0.000(2) -0.002(2) 0.001(2) C231 0.023(2) 0.022(2) 0.018(2) 0.0001(17) -0.0019(17) 0.0013(18) C232 0.019(2) 0.037(3) 0.034(3) -0.013(2) -0.008(2) 0.005(2) C233 0.018(2) 0.047(4) 0.043(3) -0.012(3) -0.004(2) 0.002(2) C234 0.021(2) 0.043(3) 0.035(3) -0.003(3) -0.005(2) 0.000(2) C235 0.029(3) 0.036(3) 0.031(3) -0.011(2) -0.004(2) -0.009(2) C236 0.025(2) 0.034(3) 0.029(3) -0.011(2) 0.002(2) -0.006(2) C241 0.023(2) 0.024(2) 0.020(2) -0.0027(18) -0.0006(17) -0.0022(18) C242 0.018(2) 0.029(3) 0.023(2) -0.0029(19) -0.0028(17) -0.0035(18) C243 0.021(2) 0.041(3) 0.021(2) -0.004(2) 0.0020(18) -0.009(2) C244 0.027(3) 0.044(4) 0.032(3) -0.014(3) 0.008(2) -0.006(2) C245 0.031(3) 0.032(3) 0.035(3) -0.009(2) 0.007(2) -0.001(2) C246 0.029(3) 0.029(3) 0.028(3) -0.006(2) 0.009(2) -0.006(2) O1 0.050(3) 0.044(3) 0.056(3) -0.011(3) 0.001(2) 0.004(2) O2 0.086(5) 0.047(4) 0.068(4) -0.016(3) -0.013(4) 0.006(3) O3 0.086(9) 0.048(7) 0.064(8) 0.013(6) 0.053(7) 0.019(6) O4 0.025(4) 0.033(5) 0.053(6) -0.007(4) 0.014(4) 0.014(3) O5 0.072(8) 0.037(6) 0.057(7) -0.015(5) -0.026(6) -0.006(5) O6 0.026(4) 0.045(5) 0.039(5) -0.021(4) 0.004(3) -0.003(3) O7 0.039(5) 0.064(7) 0.036(5) 0.011(5) -0.003(4) 0.006(5) O8 0.037(4) 0.040(5) 0.020(4) 0.002(3) -0.010(3) -0.001(4) O9 0.041(5) 0.020(4) 0.069(7) 0.014(4) -0.044(5) -0.009(3) O111 0.034(3) 0.093(5) 0.048(3) -0.022(3) 0.003(2) -0.015(3) O112 0.055(4) 0.086(5) 0.046(3) -0.005(3) -0.012(3) -0.011(3) O113 0.086(5) 0.037(3) 0.057(4) -0.010(3) -0.025(3) -0.009(3) O114 0.051(3) 0.084(5) 0.060(4) -0.038(3) -0.018(3) 0.017(3) O115 0.043(3) 0.100(5) 0.040(3) -0.017(3) 0.006(2) -0.013(3) O116 0.061(5) 0.101(7) 0.079(5) -0.020(6) 0.004(4) -0.023(5) O118 0.061(5) 0.101(7) 0.079(5) -0.020(6) 0.004(4) -0.023(5) O211 0.163(9) 0.027(3) 0.133(8) 0.001(4) -0.077(7) 0.006(4) O212 0.055(3) 0.079(5) 0.049(3) -0.002(3) -0.012(3) 0.018(3) O213 0.041(3) 0.065(4) 0.039(3) 0.006(2) -0.012(2) -0.022(2) O214 0.051(3) 0.041(3) 0.030(2) -0.0096(19) 0.0058(19) -0.012(2) O215 0.057(3) 0.059(4) 0.044(3) -0.021(3) 0.012(2) -0.018(3) O216 0.036(3) 0.118(6) 0.049(3) -0.035(4) -0.002(2) 0.011(3) O311 0.055(7) 0.051(7) 0.063(7) -0.031(6) -0.009(5) 0.009(5) O312 0.128(16) 0.059(10) 0.125(17) -0.020(10) 0.016(13) 0.022(10) O313 0.064(7) 0.055(7) 0.055(7) -0.019(6) 0.020(6) -0.002(6) O314 0.087(11) 0.151(18) 0.103(13) -0.090(14) 0.054(10) -0.058(12) O315 0.17(2) 0.21(3) 0.14(2) -0.08(2) -0.061(18) 0.15(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Gd1 O92 2.312(5) . ? Gd1 O116 2.339(17) . ? Gd1 O63 2.365(7) . ? Gd1 O111 2.389(6) . ? Gd1 O114 2.393(6) . ? Gd1 O113 2.416(6) . ? Gd1 O112 2.417(7) . ? Gd1 O115 2.483(6) . ? Gd1 O118 2.491(18) . ? Gd2 O91 2.292(5) . ? Gd2 O212 2.361(6) . ? Gd2 O216 2.380(6) . ? Gd2 O213 2.396(6) . ? Gd2 O214 2.404(5) . ? Gd2 O211 2.411(7) . ? Gd2 O34 2.420(5) . ? Gd2 O215 2.475(6) . ? Gd3 O102 2.275(12) 2_766 ? Gd3 O315 2.38(3) . ? Gd3 O314 2.377(16) . ? Gd3 O54 2.384(6) . ? Gd3 O313 2.398(12) . ? Gd3 O311 2.411(12) . ? Gd3 O312 2.575(17) . ? Gd3 O102 2.588(12) . ? Gd3 O101 2.604(12) . ? O11 C11 1.353(7) . ? C11 C12 1.408(9) . ? C11 C16 1.413(8) . ? C12 C13 1.390(8) . ? C12 C2 1.534(8) . ? C13 C14 1.394(9) . ? C13 H13 0.95 . ? C14 C15 1.385(10) . ? C14 S1 1.760(6) . ? S1 O12 1.425(8) . ? S1 O13 1.429(7) . ? S1 O14 1.483(6) . ? C15 C16 1.392(8) . ? C15 H15 0.95 . ? C16 C1 1.508(9) . ? C1 C42 1.518(8) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C21 O21 1.356(7) . ? C21 C22 1.414(8) . ? C21 C26 1.418(8) . ? C22 C23 1.385(8) . ? C22 C3 1.525(8) . ? C23 C24 1.390(8) . ? C23 H23 0.95 . ? C24 C25 1.388(8) . ? C24 S2 1.781(6) . ? S2 O22 1.445(5) . ? S2 O24 1.463(5) . ? S2 O23 1.475(6) . ? C25 C26 1.388(9) . ? C25 H25 0.95 . ? C26 C2 1.517(8) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 O31 1.377(7) . ? C31 C32 1.392(9) . ? C31 C36 1.409(8) . ? C32 C33 1.385(8) . ? C32 C4 1.536(8) . ? C33 C34 1.395(8) . ? C33 H33 0.95 . ? C34 C35 1.377(9) . ? C34 S3 1.765(6) . ? S3 O32 1.450(5) . ? S3 O34 1.466(5) . ? S3 O33 1.470(6) . ? C35 C36 1.395(8) . ? C35 H35 0.95 . ? C36 C3 1.516(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C41 O41 1.353(6) . ? C41 C42 1.398(7) . ? C41 C46 1.407(8) . ? C42 C43 1.401(8) . ? C43 C44 1.395(8) . ? C43 H43 0.95 . ? C44 C45 1.391(8) . ? C44 S4 1.775(6) . ? S4 O44 1.449(5) . ? S4 O43 1.457(6) . ? S4 O42 1.460(5) . ? C45 C46 1.398(8) . ? C45 H45 0.95 . ? C46 C4 1.517(7) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C51 O51 1.355(10) . ? C51 C52 1.408(11) . ? C51 C56 1.421(10) . ? C52 C53 1.370(11) . ? C52 C6 1.523(9) . ? C53 C54 1.388(9) . ? C53 H53 0.95 . ? C54 C55 1.377(10) . ? C54 S5 1.744(8) . ? S5 O52 1.419(10) . ? S5 O54 1.422(6) . ? S5 O53 1.437(7) . ? C55 C56 1.394(11) . ? C55 H55 0.95 . ? C56 C5 1.500(10) . ? C5 C82 1.527(10) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C61 O61 1.353(8) . ? C61 C62 1.399(8) . ? C61 C66 1.405(10) . ? C62 C63 1.381(9) . ? C62 C7 1.504(9) . ? C63 C64 1.396(10) . ? C63 H63 0.95 . ? C64 C65 1.400(10) . ? C64 S6 1.747(7) . ? S6 O62 1.452(7) . ? S6 O63 1.453(6) . ? S6 O64 1.464(6) . ? C65 C66 1.381(10) . ? C65 H65 0.95 . ? C66 C6 1.513(9) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C71 O71 1.345(8) . ? C71 C72 1.397(10) . ? C71 C76 1.408(8) . ? C72 C73 1.408(10) . ? C72 C8 1.521(9) . ? C73 C74 1.384(9) . ? C73 H73 0.95 . ? C74 C75 1.388(9) . ? C74 S7 1.765(7) . ? S7 O74 1.428(8) . ? S7 O72 1.454(8) . ? S7 O73 1.459(8) . ? C75 C76 1.387(8) . ? C75 H75 0.95 . ? C76 C7 1.521(9) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C81 O81 1.327(9) . ? C81 C86 1.415(10) . ? C81 C82 1.417(9) . ? C82 C83 1.370(10) . ? C83 C84 1.380(10) . ? C83 H83 0.95 . ? C84 C85 1.411(9) . ? C84 S8 1.766(7) . ? S8 O82 1.441(5) . ? S8 O84 1.470(5) . ? S8 O83 1.477(6) . ? C85 C86 1.358(10) . ? C85 H85 0.95 . ? C86 C8 1.530(9) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? N91 C92 1.322(9) . ? N91 C95 1.373(9) . ? N91 C96 1.472(11) . ? C92 N93 1.329(9) . ? C92 H92 0.95 . ? N93 C94 1.377(8) . ? N93 C97 1.440(9) . ? C94 C95 1.340(11) . ? C94 H94 0.95 . ? C95 H95 0.95 . ? C96 H96A 0.98 . ? C96 H96B 0.98 . ? C96 H96C 0.98 . ? C97 C98 1.519(10) . ? C97 H97A 0.99 . ? C97 H97B 0.99 . ? C98 O92 1.235(8) . ? C98 O91 1.251(8) . ? N101 C102 1.313(10) . ? N101 C105 1.370(13) . ? N101 C106 1.460(14) . ? C102 N103 1.324(10) . ? C102 H102 0.95 . ? N103 C104 1.369(11) . ? N103 C107 1.519(16) . ? C104 C105 1.325(16) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? C107 C108 1.66(2) . ? C107 H10D 0.99 . ? C107 H10E 0.99 . ? C108 O101 1.329(19) . ? C108 O102 1.60(2) . ? O102 Gd3 2.275(12) 2_766 ? P1 C111 1.789(5) . ? P1 C121 1.790(6) . ? P1 C141 1.790(6) . ? P1 C131 1.800(6) . ? C111 C116 1.407(8) . ? C111 C112 1.409(7) . ? C112 C113 1.383(7) . ? C112 H112 0.95 . ? C113 C114 1.385(8) . ? C113 H113 0.95 . ? C114 O117 1.346(6) . ? C114 C115 1.408(7) . ? C115 C116 1.387(7) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? O117 C117 1.435(8) . ? C117 H11A 0.98 . ? C117 H11B 0.98 . ? C117 H11C 0.98 . ? C121 C122 1.391(8) . ? C121 C126 1.404(7) . ? C122 C123 1.395(8) . ? C122 H122 0.95 . ? C123 C124 1.391(8) . ? C123 H123 0.95 . ? C124 C125 1.399(9) . ? C124 H124 0.95 . ? C125 C126 1.399(8) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.382(8) . ? C131 C132 1.418(8) . ? C132 C133 1.383(9) . ? C132 H132 0.95 . ? C133 C134 1.386(9) . ? C133 H133 0.95 . ? C134 C135 1.385(9) . ? C134 H134 0.95 . ? C135 C136 1.393(9) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C141 C142 1.392(9) . ? C141 C146 1.396(8) . ? C142 C143 1.404(9) . ? C142 H142 0.95 . ? C143 C144 1.379(11) . ? C143 H143 0.95 . ? C144 C145 1.416(12) . ? C144 H144 0.95 . ? C145 C146 1.390(9) . ? C145 H145 0.95 . ? C146 H146 0.95 . ? P2 C211 1.790(5) . ? P2 C241 1.794(5) . ? P2 C221 1.795(6) . ? P2 C231 1.800(5) . ? C211 C216 1.396(7) . ? C211 C212 1.409(7) . ? C212 C213 1.381(7) . ? C212 H212 0.95 . ? C213 C214 1.399(7) . ? C213 H213 0.95 . ? C214 O217 1.346(6) . ? C214 C215 1.389(7) . ? C215 C216 1.387(7) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? O217 C217 1.435(7) . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C221 C222 1.387(8) . ? C221 C226 1.405(8) . ? C222 C223 1.408(9) . ? C222 H222 0.95 . ? C223 C224 1.377(11) . ? C223 H223 0.95 . ? C224 C225 1.360(11) . ? C224 H224 0.95 . ? C225 C226 1.388(9) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C236 1.386(8) . ? C231 C232 1.401(8) . ? C232 C233 1.407(8) . ? C232 H232 0.95 . ? C233 C234 1.383(10) . ? C233 H233 0.95 . ? C234 C235 1.390(9) . ? C234 H234 0.95 . ? C235 C236 1.404(8) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C241 C246 1.392(8) . ? C241 C242 1.402(7) . ? C242 C243 1.390(8) . ? C242 H242 0.95 . ? C243 C244 1.394(9) . ? C243 H243 0.95 . ? C244 C245 1.395(9) . ? C244 H244 0.95 . ? C245 C246 1.393(8) . ? C245 H245 0.95 . ? C246 H246 0.95 . ? 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 O92 Gd1 O116 143.1(5) . . ? O92 Gd1 O63 80.9(2) . . ? O116 Gd1 O63 99.1(5) . . ? O92 Gd1 O111 74.8(2) . . ? O116 Gd1 O111 141.6(5) . . ? O63 Gd1 O111 76.8(2) . . ? O92 Gd1 O114 75.4(2) . . ? O116 Gd1 O114 69.0(5) . . ? O63 Gd1 O114 75.6(2) . . ? O111 Gd1 O114 142.0(3) . . ? O92 Gd1 O113 76.7(2) . . ? O116 Gd1 O113 84.8(6) . . ? O63 Gd1 O113 146.5(2) . . ? O111 Gd1 O113 119.8(2) . . ? O114 Gd1 O113 74.9(2) . . ? O92 Gd1 O112 106.8(2) . . ? O116 Gd1 O112 95.6(5) . . ? O63 Gd1 O112 142.5(2) . . ? O111 Gd1 O112 70.4(2) . . ? O114 Gd1 O112 141.8(2) . . ? O113 Gd1 O112 69.0(2) . . ? O92 Gd1 O115 144.6(2) . . ? O116 Gd1 O115 68.3(5) . . ? O63 Gd1 O115 76.6(2) . . ? O111 Gd1 O115 73.7(2) . . ? O114 Gd1 O115 123.5(2) . . ? O113 Gd1 O115 134.0(2) . . ? O112 Gd1 O115 77.1(2) . . ? O92 Gd1 O118 142.2(5) . . ? O63 Gd1 O118 117.6(5) . . ? O111 Gd1 O118 138.9(5) . . ? O114 Gd1 O118 77.9(5) . . ? O113 Gd1 O118 70.8(5) . . ? O112 Gd1 O118 79.1(5) . . ? O115 Gd1 O118 73.1(5) . . ? O91 Gd2 O212 148.1(2) . . ? O91 Gd2 O216 89.5(2) . . ? O212 Gd2 O216 76.9(2) . . ? O91 Gd2 O213 70.66(17) . . ? O212 Gd2 O213 78.7(2) . . ? O216 Gd2 O213 80.7(2) . . ? O91 Gd2 O214 77.28(17) . . ? O212 Gd2 O214 129.3(2) . . ? O216 Gd2 O214 144.12(18) . . ? O213 Gd2 O214 123.9(2) . . ? O91 Gd2 O211 141.8(2) . . ? O212 Gd2 O211 69.3(3) . . ? O216 Gd2 O211 97.1(4) . . ? O213 Gd2 O211 147.5(2) . . ? O214 Gd2 O211 75.6(3) . . ? O91 Gd2 O34 106.16(17) . . ? O212 Gd2 O34 72.5(2) . . ? O216 Gd2 O34 143.43(19) . . ? O213 Gd2 O34 74.09(19) . . ? O214 Gd2 O34 72.39(17) . . ? O211 Gd2 O34 90.5(3) . . ? O91 Gd2 O215 74.51(19) . . ? O212 Gd2 O215 126.4(2) . . ? O216 Gd2 O215 72.8(2) . . ? O213 Gd2 O215 135.93(18) . . ? O214 Gd2 O215 71.58(18) . . ? O211 Gd2 O215 71.8(3) . . ? O34 Gd2 O215 142.79(19) . . ? O102 Gd3 O315 75.2(8) 2_766 . ? O102 Gd3 O314 73.8(7) 2_766 . ? O315 Gd3 O314 75.0(8) . . ? O102 Gd3 O54 76.5(3) 2_766 . ? O315 Gd3 O54 123.5(9) . . ? O314 Gd3 O54 138.7(4) . . ? O102 Gd3 O313 86.9(5) 2_766 . ? O315 Gd3 O313 147.9(7) . . ? O314 Gd3 O313 74.4(6) . . ? O54 Gd3 O313 76.0(4) . . ? O102 Gd3 O311 132.1(5) 2_766 . ? O315 Gd3 O311 82.8(7) . . ? O314 Gd3 O311 139.8(5) . . ? O54 Gd3 O311 81.5(4) . . ? O313 Gd3 O311 127.9(4) . . ? O102 Gd3 O312 62.8(6) 2_766 . ? O315 Gd3 O312 57.5(10) . . ? O314 Gd3 O312 121.2(8) . . ? O54 Gd3 O312 66.1(6) . . ? O313 Gd3 O312 135.5(6) . . ? O311 Gd3 O312 69.4(6) . . ? O102 Gd3 O102 135.2(2) 2_766 . ? O315 Gd3 O102 68.5(9) . . ? O314 Gd3 O102 72.2(5) . . ? O54 Gd3 O102 146.5(3) . . ? O313 Gd3 O102 110.6(4) . . ? O311 Gd3 O102 68.6(4) . . ? O312 Gd3 O102 113.8(6) . . ? O102 Gd3 O101 154.1(5) 2_766 . ? O315 Gd3 O101 127.3(9) . . ? O314 Gd3 O101 98.1(7) . . ? O54 Gd3 O101 96.3(3) . . ? O313 Gd3 O101 67.2(4) . . ? O311 Gd3 O101 69.5(4) . . ? O312 Gd3 O101 137.1(6) . . ? O102 Gd3 O101 60.0(4) . . ? O11 C11 C12 120.0(5) . . ? O11 C11 C16 118.4(5) . . ? C12 C11 C16 121.6(5) . . ? C13 C12 C11 118.2(5) . . ? C13 C12 C2 120.4(6) . . ? C11 C12 C2 121.4(5) . . ? C12 C13 C14 121.0(6) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 120.0(6) . . ? C15 C14 S1 118.7(5) . . ? C13 C14 S1 121.2(5) . . ? O12 S1 O13 113.5(5) . . ? O12 S1 O14 113.0(5) . . ? O13 S1 O14 108.8(4) . . ? O12 S1 C14 107.2(4) . . ? O13 S1 C14 108.2(3) . . ? O14 S1 C14 105.7(3) . . ? C14 C15 C16 121.3(6) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 117.9(6) . . ? C15 C16 C1 120.8(5) . . ? C11 C16 C1 121.2(5) . . ? C16 C1 C42 114.7(4) . . ? C16 C1 H1A 108.6 . . ? C42 C1 H1A 108.6 . . ? C16 C1 H1B 108.6 . . ? C42 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? O21 C21 C22 118.5(5) . . ? O21 C21 C26 120.1(5) . . ? C22 C21 C26 121.3(5) . . ? C23 C22 C21 118.5(5) . . ? C23 C22 C3 121.2(5) . . ? C21 C22 C3 120.3(5) . . ? C22 C23 C24 120.4(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 121.0(6) . . ? C25 C24 S2 121.4(5) . . ? C23 C24 S2 117.5(4) . . ? O22 S2 O24 113.4(3) . . ? O22 S2 O23 113.7(4) . . ? O24 S2 O23 110.8(3) . . ? O22 S2 C24 107.2(3) . . ? O24 S2 C24 106.3(3) . . ? O23 S2 C24 104.8(3) . . ? C26 C25 C24 120.7(5) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 118.0(5) . . ? C25 C26 C2 120.9(5) . . ? C21 C26 C2 121.0(6) . . ? C26 C2 C12 113.9(5) . . ? C26 C2 H2A 108.8 . . ? C12 C2 H2A 108.8 . . ? C26 C2 H2B 108.8 . . ? C12 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O31 C31 C32 120.5(5) . . ? O31 C31 C36 117.6(5) . . ? C32 C31 C36 121.8(5) . . ? C33 C32 C31 118.8(5) . . ? C33 C32 C4 118.4(5) . . ? C31 C32 C4 122.8(5) . . ? C32 C33 C34 120.0(6) . . ? C32 C33 H33 120 . . ? C34 C33 H33 120 . . ? C35 C34 C33 121.0(5) . . ? C35 C34 S3 122.2(5) . . ? C33 C34 S3 116.8(5) . . ? O32 S3 O34 112.3(3) . . ? O32 S3 O33 112.7(4) . . ? O34 S3 O33 111.6(3) . . ? O32 S3 C34 106.7(3) . . ? O34 S3 C34 106.2(3) . . ? O33 S3 C34 106.8(3) . . ? S3 O34 Gd2 147.6(3) . . ? C34 C35 C36 120.4(5) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 117.9(6) . . ? C35 C36 C3 120.6(5) . . ? C31 C36 C3 121.4(5) . . ? C36 C3 C22 112.2(4) . . ? C36 C3 H3A 109.2 . . ? C22 C3 H3A 109.2 . . ? C36 C3 H3B 109.2 . . ? C22 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O41 C41 C42 122.8(5) . . ? O41 C41 C46 115.6(5) . . ? C42 C41 C46 121.6(5) . . ? C41 C42 C43 117.7(5) . . ? C41 C42 C1 121.4(5) . . ? C43 C42 C1 120.8(5) . . ? C44 C43 C42 121.1(5) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C45 C44 C43 120.6(5) . . ? C45 C44 S4 119.5(5) . . ? C43 C44 S4 119.9(4) . . ? O44 S4 O43 112.1(4) . . ? O44 S4 O42 112.7(3) . . ? O43 S4 O42 112.8(4) . . ? O44 S4 C44 106.9(3) . . ? O43 S4 C44 106.1(3) . . ? O42 S4 C44 105.7(3) . . ? C44 C45 C46 119.4(5) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C46 C41 119.5(5) . . ? C45 C46 C4 121.3(5) . . ? C41 C46 C4 119.2(5) . . ? C46 C4 C32 110.8(4) . . ? C46 C4 H4A 109.5 . . ? C32 C4 H4A 109.5 . . ? C46 C4 H4B 109.5 . . ? C32 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? O51 C51 C52 120.0(6) . . ? O51 C51 C56 119.0(7) . . ? C52 C51 C56 121.0(7) . . ? C53 C52 C51 118.8(6) . . ? C53 C52 C6 119.6(7) . . ? C51 C52 C6 121.5(7) . . ? C52 C53 C54 120.5(7) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C55 C54 C53 121.6(7) . . ? C55 C54 S5 120.4(5) . . ? C53 C54 S5 118.0(6) . . ? O52 S5 O54 105.6(6) . . ? O52 S5 O53 112.8(6) . . ? O54 S5 O53 117.0(5) . . ? O52 S5 C54 106.8(5) . . ? O54 S5 C54 106.6(4) . . ? O53 S5 C54 107.5(4) . . ? S5 O54 Gd3 140.8(5) . . ? C54 C55 C56 120.0(6) . . ? C54 C55 H55 120 . . ? C56 C55 H55 120 . . ? C55 C56 C51 118.2(7) . . ? C55 C56 C5 120.6(6) . . ? C51 C56 C5 121.2(7) . . ? C56 C5 C82 112.1(5) . . ? C56 C5 H5A 109.2 . . ? C82 C5 H5A 109.2 . . ? C56 C5 H5B 109.2 . . ? C82 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? O61 C61 C62 121.2(6) . . ? O61 C61 C66 117.5(5) . . ? C62 C61 C66 121.3(6) . . ? C63 C62 C61 118.5(6) . . ? C63 C62 C7 120.7(6) . . ? C61 C62 C7 120.8(6) . . ? C62 C63 C64 120.9(6) . . ? C62 C63 H63 119.5 . . ? C64 C63 H63 119.5 . . ? C63 C64 C65 120.1(6) . . ? C63 C64 S6 120.5(5) . . ? C65 C64 S6 119.4(6) . . ? O62 S6 O63 111.2(4) . . ? O62 S6 O64 113.0(4) . . ? O63 S6 O64 112.8(4) . . ? O62 S6 C64 106.8(4) . . ? O63 S6 C64 104.5(3) . . ? O64 S6 C64 108.0(3) . . ? S6 O63 Gd1 145.8(4) . . ? C66 C65 C64 119.9(7) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C61 119.3(6) . . ? C65 C66 C6 121.2(7) . . ? C61 C66 C6 119.5(6) . . ? C66 C6 C52 110.4(5) . . ? C66 C6 H6A 109.6 . . ? C52 C6 H6A 109.6 . . ? C66 C6 H6B 109.6 . . ? C52 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O71 C71 C72 121.0(6) . . ? O71 C71 C76 118.5(6) . . ? C72 C71 C76 120.4(6) . . ? C71 C72 C73 119.5(6) . . ? C71 C72 C8 121.6(6) . . ? C73 C72 C8 118.9(7) . . ? C74 C73 C72 119.6(6) . . ? C74 C73 H73 120.2 . . ? C72 C73 H73 120.2 . . ? C73 C74 C75 120.7(6) . . ? C73 C74 S7 120.6(5) . . ? C75 C74 S7 118.7(5) . . ? O74 S7 O72 114.1(5) . . ? O74 S7 O73 110.9(6) . . ? O72 S7 O73 109.7(5) . . ? O74 S7 C74 107.3(4) . . ? O72 S7 C74 108.1(4) . . ? O73 S7 C74 106.4(4) . . ? C76 C75 C74 120.8(6) . . ? C76 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? C75 C76 C71 119.0(6) . . ? C75 C76 C7 119.9(5) . . ? C71 C76 C7 121.0(5) . . ? C62 C7 C76 117.3(5) . . ? C62 C7 H7A 108 . . ? C76 C7 H7A 108 . . ? C62 C7 H7B 108 . . ? C76 C7 H7B 108 . . ? H7A C7 H7B 107.2 . . ? O81 C81 C86 121.4(6) . . ? O81 C81 C82 119.0(6) . . ? C86 C81 C82 119.5(7) . . ? C83 C82 C81 119.4(6) . . ? C83 C82 C5 120.5(6) . . ? C81 C82 C5 120.1(6) . . ? C82 C83 C84 121.1(6) . . ? C82 C83 H83 119.5 . . ? C84 C83 H83 119.5 . . ? C83 C84 C85 119.7(6) . . ? C83 C84 S8 121.1(5) . . ? C85 C84 S8 119.2(5) . . ? O82 S8 O84 113.6(3) . . ? O82 S8 O83 112.7(4) . . ? O84 S8 O83 111.4(3) . . ? O82 S8 C84 106.3(3) . . ? O84 S8 C84 106.6(3) . . ? O83 S8 C84 105.7(3) . . ? C86 C85 C84 120.6(6) . . ? C86 C85 H85 119.7 . . ? C84 C85 H85 119.7 . . ? C85 C86 C81 119.7(6) . . ? C85 C86 C8 119.1(6) . . ? C81 C86 C8 121.3(6) . . ? C72 C8 C86 112.7(5) . . ? C72 C8 H8A 109 . . ? C86 C8 H8A 109 . . ? C72 C8 H8B 109 . . ? C86 C8 H8B 109 . . ? H8A C8 H8B 107.8 . . ? C92 N91 C95 108.5(6) . . ? C92 N91 C96 125.1(7) . . ? C95 N91 C96 126.3(7) . . ? N91 C92 N93 108.9(6) . . ? N91 C92 H92 125.6 . . ? N93 C92 H92 125.6 . . ? C92 N93 C94 108.1(6) . . ? C92 N93 C97 125.2(6) . . ? C94 N93 C97 126.6(6) . . ? C95 C94 N93 107.2(6) . . ? C95 C94 H94 126.4 . . ? N93 C94 H94 126.4 . . ? C94 C95 N91 107.3(6) . . ? C94 C95 H95 126.3 . . ? N91 C95 H95 126.3 . . ? N91 C96 H96A 109.5 . . ? N91 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? N91 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? N93 C97 C98 113.6(5) . . ? N93 C97 H97A 108.8 . . ? C98 C97 H97A 108.8 . . ? N93 C97 H97B 108.8 . . ? C98 C97 H97B 108.8 . . ? H97A C97 H97B 107.7 . . ? O92 C98 O91 126.8(7) . . ? O92 C98 C97 116.0(6) . . ? O91 C98 C97 117.2(6) . . ? C98 O91 Gd2 159.6(5) . . ? C98 O92 Gd1 160.1(5) . . ? C102 N101 C105 109.6(8) . . ? C102 N101 C106 123.3(9) . . ? C105 N101 C106 126.9(10) . . ? N101 C102 N103 106.9(7) . . ? N101 C102 H102 126.6 . . ? N103 C102 H102 126.6 . . ? C102 N103 C104 109.8(8) . . ? C102 N103 C107 122.9(9) . . ? C104 N103 C107 126.4(10) . . ? C105 C104 N103 106.4(8) . . ? C105 C104 H104 126.8 . . ? N103 C104 H104 126.8 . . ? C104 C105 N101 107.2(8) . . ? C104 C105 H105 126.4 . . ? N101 C105 H105 126.4 . . ? N101 C106 H10A 109.5 . . ? N101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? N101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? N103 C107 C108 106.0(12) . . ? N103 C107 H10D 110.5 . . ? C108 C107 H10D 110.5 . . ? N103 C107 H10E 110.5 . . ? C108 C107 H10E 110.5 . . ? H10D C107 H10E 108.7 . . ? O101 C108 O102 124.3(15) . . ? O101 C108 C107 115.1(14) . . ? O102 C108 C107 118.0(13) . . ? O101 C108 Gd3 65.6(9) . . ? O102 C108 Gd3 63.9(7) . . ? C107 C108 Gd3 173.1(12) . . ? C108 O101 Gd3 86.8(10) . . ? C108 O102 Gd3 116.4(10) . 2_766 ? C108 O102 Gd3 82.3(8) . . ? Gd3 O102 Gd3 44.8(2) 2_766 . ? C111 P1 C121 108.8(3) . . ? C111 P1 C141 110.7(2) . . ? C121 P1 C141 110.2(3) . . ? C111 P1 C131 110.4(3) . . ? C121 P1 C131 110.2(2) . . ? C141 P1 C131 106.5(3) . . ? C116 C111 C112 119.2(5) . . ? C116 C111 P1 120.1(4) . . ? C112 C111 P1 120.6(4) . . ? C113 C112 C111 119.9(5) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C112 C113 C114 120.8(5) . . ? C112 C113 H113 119.6 . . ? C114 C113 H113 119.6 . . ? O117 C114 C113 117.1(5) . . ? O117 C114 C115 123.0(5) . . ? C113 C114 C115 119.8(5) . . ? C116 C115 C114 119.7(5) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C115 C116 C111 120.4(5) . . ? C115 C116 H116 119.8 . . ? C111 C116 H116 119.8 . . ? C114 O117 C117 117.4(4) . . ? O117 C117 H11A 109.5 . . ? O117 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? O117 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C122 C121 C126 120.0(5) . . ? C122 C121 P1 121.9(4) . . ? C126 C121 P1 118.2(4) . . ? C121 C122 C123 119.9(5) . . ? C121 C122 H122 120 . . ? C123 C122 H122 120 . . ? C124 C123 C122 120.4(6) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C123 C124 C125 120.1(5) . . ? C123 C124 H124 120 . . ? C125 C124 H124 120 . . ? C124 C125 C126 119.7(5) . . ? C124 C125 H125 120.2 . . ? C126 C125 H125 120.2 . . ? C125 C126 C121 119.9(5) . . ? C125 C126 H126 120 . . ? C121 C126 H126 120 . . ? C136 C131 C132 118.2(5) . . ? C136 C131 P1 120.3(4) . . ? C132 C131 P1 121.5(4) . . ? C133 C132 C131 120.4(6) . . ? C133 C132 H132 119.8 . . ? C131 C132 H132 119.8 . . ? C132 C133 C134 120.2(6) . . ? C132 C133 H133 119.9 . . ? C134 C133 H133 119.9 . . ? C135 C134 C133 120.2(6) . . ? C135 C134 H134 119.9 . . ? C133 C134 H134 119.9 . . ? C134 C135 C136 119.7(6) . . ? C134 C135 H135 120.2 . . ? C136 C135 H135 120.2 . . ? C131 C136 C135 121.3(6) . . ? C131 C136 H136 119.3 . . ? C135 C136 H136 119.3 . . ? C142 C141 C146 120.4(6) . . ? C142 C141 P1 118.1(4) . . ? C146 C141 P1 121.4(5) . . ? C141 C142 C143 120.2(6) . . ? C141 C142 H142 119.9 . . ? C143 C142 H142 119.9 . . ? C144 C143 C142 119.7(8) . . ? C144 C143 H143 120.2 . . ? C142 C143 H143 120.2 . . ? C143 C144 C145 120.1(7) . . ? C143 C144 H144 119.9 . . ? C145 C144 H144 119.9 . . ? C146 C145 C144 120.0(6) . . ? C146 C145 H145 120 . . ? C144 C145 H145 120 . . ? C145 C146 C141 119.5(6) . . ? C145 C146 H146 120.2 . . ? C141 C146 H146 120.2 . . ? C211 P2 C241 108.5(2) . . ? C211 P2 C221 110.8(3) . . ? C241 P2 C221 111.3(2) . . ? C211 P2 C231 110.7(2) . . ? C241 P2 C231 109.1(2) . . ? C221 P2 C231 106.4(2) . . ? C216 C211 C212 118.7(5) . . ? C216 C211 P2 120.8(4) . . ? C212 C211 P2 120.5(4) . . ? C213 C212 C211 120.6(5) . . ? C213 C212 H212 119.7 . . ? C211 C212 H212 119.7 . . ? C212 C213 C214 119.6(5) . . ? C212 C213 H213 120.2 . . ? C214 C213 H213 120.2 . . ? O217 C214 C215 124.3(5) . . ? O217 C214 C213 115.0(4) . . ? C215 C214 C213 120.7(5) . . ? C216 C215 C214 119.3(5) . . ? C216 C215 H215 120.4 . . ? C214 C215 H215 120.4 . . ? C215 C216 C211 121.2(5) . . ? C215 C216 H216 119.4 . . ? C211 C216 H216 119.4 . . ? C214 O217 C217 116.5(4) . . ? O217 C217 H21A 109.5 . . ? O217 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? O217 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C222 C221 C226 119.8(5) . . ? C222 C221 P2 122.5(4) . . ? C226 C221 P2 117.7(4) . . ? C221 C222 C223 119.5(6) . . ? C221 C222 H222 120.2 . . ? C223 C222 H222 120.2 . . ? C224 C223 C222 119.5(6) . . ? C224 C223 H223 120.2 . . ? C222 C223 H223 120.2 . . ? C225 C224 C223 121.1(6) . . ? C225 C224 H224 119.4 . . ? C223 C224 H224 119.4 . . ? C224 C225 C226 120.7(6) . . ? C224 C225 H225 119.7 . . ? C226 C225 H225 119.7 . . ? C225 C226 C221 119.3(6) . . ? C225 C226 H226 120.3 . . ? C221 C226 H226 120.3 . . ? C236 C231 C232 120.1(5) . . ? C236 C231 P2 122.2(4) . . ? C232 C231 P2 117.7(4) . . ? C231 C232 C233 119.3(6) . . ? C231 C232 H232 120.3 . . ? C233 C232 H232 120.3 . . ? C234 C233 C232 120.5(6) . . ? C234 C233 H233 119.7 . . ? C232 C233 H233 119.7 . . ? C233 C234 C235 119.7(6) . . ? C233 C234 H234 120.1 . . ? C235 C234 H234 120.1 . . ? C234 C235 C236 120.4(6) . . ? C234 C235 H235 119.8 . . ? C236 C235 H235 119.8 . . ? C231 C236 C235 119.8(5) . . ? C231 C236 H236 120.1 . . ? C235 C236 H236 120.1 . . ? C246 C241 C242 120.4(5) . . ? C246 C241 P2 119.0(4) . . ? C242 C241 P2 120.6(4) . . ? C243 C242 C241 119.0(5) . . ? C243 C242 H242 120.5 . . ? C241 C242 H242 120.5 . . ? C242 C243 C244 120.6(5) . . ? C242 C243 H243 119.7 . . ? C244 C243 H243 119.7 . . ? C243 C244 C245 120.2(5) . . ? C243 C244 H244 119.9 . . ? C245 C244 H244 119.9 . . ? C246 C245 C244 119.3(6) . . ? C246 C245 H245 120.3 . . ? C244 C245 H245 120.3 . . ? C241 C246 C245 120.4(5) . . ? C241 C246 H246 119.8 . . ? C245 C246 H246 119.8 . . ? O118 O116 Gd1 92(2) . . ? O116 O118 Gd1 70(2) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 99 18 ' ' #===END # Attachment '7926_web_deposit_cif_file_2_BrianSkelton_1320129951.110713b.cif' data_110713b _database_code_depnum_ccdc_archive 'CCDC 851783' #TrackingRef '7926_web_deposit_cif_file_2_BrianSkelton_1320129951.110713b.cif' _audit_creation_date 2011-08-09T13:41:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C236 H284 N8 O117 P4 S16 Y5' _chemical_formula_moiety ; C136 H170 Y5 N8 O100 S16, 4(C25 H22 O P), 13(H2 O)' ; _chemical_formula_weight 6186.1 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5119(3) _cell_length_b 20.0962(7) _cell_length_c 25.4359(6) _cell_angle_alpha 75.509(3) _cell_angle_beta 88.865(2) _cell_angle_gamma 89.772(2) _cell_volume 6685.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11487 _cell_measurement_theta_min 2.778 _cell_measurement_theta_max 27.8034 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3203 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 2 0.1339 0 1 -2 0.1548 -2 0 3 0.0838 1 0 -1 0.1157 -1 1 -1 0.1761 0 1 1 0.0511 0 -1 -1 0.018 1 -1 1 0.146 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.324 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.916 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0054293 _diffrn_orient_matrix_ub_12 -0.0007095 _diffrn_orient_matrix_ub_13 0.0278079 _diffrn_orient_matrix_ub_21 0.0112261 _diffrn_orient_matrix_ub_22 0.0356248 _diffrn_orient_matrix_ub_23 -0.0072528 _diffrn_orient_matrix_ub_31 -0.0510059 _diffrn_orient_matrix_ub_32 0.0077167 _diffrn_orient_matrix_ub_33 0.0019433 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur Diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_unetI/netI 0.084 _diffrn_reflns_number 43546 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 23494 _reflns_number_gt 18061 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. One Y atom, Y3, was found to be disordered about a crystallographic inversion centre with the coordinated water molecules similarly disordered. One water molecule coordinated to Y1, O116, refined with an elongated ellipsoid and was modelled as being disordered over two sites, O116, O118. Solvent molecules were modelled as three water molecules, fully weighted with a further seven which were assigned site occupancies of 0.5 from refinement and close contact considerations. Any remaining electron density that was not modelled was effectively removed by use of the program Squeeze. Water molecule and hydroxyl hydrogen atoms were not located. ; _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^)+(0.1338P)^2^+51.3580P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 23494 _refine_ls_number_parameters 1795 _refine_ls_number_restraints 165 _refine_ls_R_factor_all 0.1624 _refine_ls_R_factor_gt 0.1342 _refine_ls_wR_factor_ref 0.3229 _refine_ls_wR_factor_gt 0.3036 _refine_ls_goodness_of_fit_ref 1.16 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.02 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.089 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.15 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Y1 Y 0.43896(8) 0.31889(6) 0.66314(4) 0.0432(3) Uani 1 1 d . . . Y2 Y 0.33983(8) 0.12509(6) 0.88096(4) 0.0430(3) Uani 1 1 d . . . Y3 Y 0.93335(17) 0.48736(11) 0.48678(10) 0.0468(6) Uani 0.5 1 d P . . O11 O -0.0111(5) 0.4992(3) 0.9368(3) 0.0342(15) Uani 1 1 d . . . C11 C -0.0172(7) 0.4798(5) 0.8896(4) 0.029(2) Uani 1 1 d . . . C12 C 0.0609(7) 0.4939(4) 0.8511(4) 0.026(2) Uani 1 1 d . . . C13 C 0.0508(7) 0.4747(5) 0.8025(4) 0.031(2) Uani 1 1 d . . . H13 H 0.1026 0.4843 0.7759 0.037 Uiso 1 1 calc R . . C14 C -0.0335(8) 0.4420(5) 0.7929(4) 0.037(2) Uani 1 1 d U . . S1 S -0.0514(3) 0.42224(15) 0.72990(11) 0.0533(8) Uani 1 1 d . . . O12 O 0.0376(9) 0.4366(7) 0.7007(4) 0.100(4) Uani 1 1 d U . . O13 O -0.0781(7) 0.3523(4) 0.7400(3) 0.061(2) Uani 1 1 d U . . O14 O -0.1344(9) 0.4648(5) 0.7045(4) 0.095(4) Uani 1 1 d U . . C15 C -0.1092(8) 0.4263(4) 0.8321(4) 0.034(2) Uani 1 1 d . . . H15 H -0.166 0.4022 0.8254 0.04 Uiso 1 1 calc R . . C16 C -0.1027(7) 0.4452(5) 0.8804(4) 0.031(2) Uani 1 1 d . . . C1 C -0.1873(7) 0.4318(5) 0.9215(4) 0.033(2) Uani 1 1 d . . . H1A H -0.2502 0.4369 0.9016 0.04 Uiso 1 1 calc R . . H1B H -0.1861 0.4677 0.942 0.04 Uiso 1 1 calc R . . C21 C 0.2364(7) 0.4507(5) 0.9414(4) 0.028(2) Uani 1 1 d . . . O21 O 0.1652(5) 0.4657(3) 0.9748(3) 0.0343(15) Uani 1 1 d . . . C22 C 0.3098(6) 0.4032(5) 0.9652(4) 0.027(2) Uani 1 1 d . . . C23 C 0.3863(6) 0.3903(5) 0.9315(4) 0.027(2) Uani 1 1 d . . . H23 H 0.436 0.3577 0.9462 0.033 Uiso 1 1 calc R . . C24 C 0.3906(6) 0.4241(5) 0.8773(4) 0.031(2) Uani 1 1 d . . . S2 S 0.49198(19) 0.40618(14) 0.83729(10) 0.0374(6) Uani 1 1 d . . . O22 O 0.5803(5) 0.4103(5) 0.8666(3) 0.056(2) Uani 1 1 d . . . O23 O 0.4725(6) 0.3373(4) 0.8307(3) 0.052(2) Uani 1 1 d . . . O24 O 0.4884(5) 0.4570(4) 0.7852(3) 0.0470(19) Uani 1 1 d . . . C25 C 0.3166(7) 0.4701(5) 0.8548(4) 0.033(2) Uani 1 1 d . . . H25 H 0.3199 0.4926 0.8172 0.04 Uiso 1 1 calc R . . C26 C 0.2380(7) 0.4834(5) 0.8864(4) 0.028(2) Uani 1 1 d . . . C2 C 0.1548(8) 0.5308(5) 0.8609(4) 0.035(2) Uani 1 1 d . . . H2A H 0.1789 0.5602 0.8258 0.041 Uiso 1 1 calc R . . H2B H 0.1377 0.5614 0.8848 0.041 Uiso 1 1 calc R . . C31 C 0.1338(7) 0.3135(5) 1.0572(3) 0.030(2) Uani 1 1 d U . . O31 O 0.1155(5) 0.3715(4) 1.0755(3) 0.0396(17) Uani 1 1 d . . . C32 C 0.0608(7) 0.2623(5) 1.0646(3) 0.028(2) Uani 1 1 d . . . C33 C 0.0839(7) 0.2037(5) 1.0487(3) 0.030(2) Uani 1 1 d . . . H33 H 0.0358 0.1683 1.053 0.036 Uiso 1 1 calc R . . C34 C 0.1753(7) 0.1952(5) 1.0267(3) 0.031(2) Uani 1 1 d . . . S3 S 0.1995(2) 0.11676(14) 1.00927(10) 0.0453(7) Uani 1 1 d . . . O32 O 0.2251(8) 0.0665(4) 1.0588(3) 0.070(3) Uani 1 1 d . . . O33 O 0.1078(7) 0.0987(4) 0.9865(3) 0.062(2) Uani 1 1 d . . . O34 O 0.2792(6) 0.1304(4) 0.9692(3) 0.0454(18) Uani 1 1 d . . . C35 C 0.2458(7) 0.2461(5) 1.0198(3) 0.029(2) Uani 1 1 d . . . H35 H 0.3089 0.2395 1.0047 0.035 Uiso 1 1 calc R . . C36 C 0.2263(7) 0.3065(5) 1.0344(3) 0.029(2) Uani 1 1 d . . . C3 C 0.3032(7) 0.3638(5) 1.0241(4) 0.034(2) Uani 1 1 d . . . H3A H 0.2861 0.3961 1.0467 0.041 Uiso 1 1 calc R . . H3B H 0.3687 0.3437 1.0355 0.041 Uiso 1 1 calc R . . C41 C -0.1199(6) 0.3464(5) 1.0055(4) 0.028(2) Uani 1 1 d U . . O41 O -0.0553(5) 0.3946(3) 1.0130(3) 0.0337(15) Uani 1 1 d . . . C42 C -0.1870(6) 0.3611(4) 0.9624(3) 0.0238(19) Uani 1 1 d . . . C43 C -0.2523(6) 0.3102(5) 0.9593(4) 0.031(2) Uani 1 1 d . . . H43 H -0.2977 0.3184 0.9303 0.038 Uiso 1 1 calc R . . C44 C -0.2540(7) 0.2472(5) 0.9970(4) 0.028(2) Uani 1 1 d . . . S4 S -0.3416(2) 0.18375(15) 0.99170(11) 0.0429(7) Uani 1 1 d . . . O42 O -0.4362(5) 0.2172(5) 0.9847(3) 0.057(2) Uani 1 1 d . . . O43 O -0.3118(7) 0.1608(5) 0.9442(4) 0.078(3) Uani 1 1 d . . . O44 O -0.3368(5) 0.1299(4) 1.0410(3) 0.0468(19) Uani 1 1 d . . . C45 C -0.1873(7) 0.2337(5) 1.0384(4) 0.030(2) Uani 1 1 d . . . H45 H -0.1875 0.1901 1.0639 0.036 Uiso 1 1 calc R . . C46 C -0.1195(6) 0.2836(4) 1.0429(4) 0.026(2) Uani 1 1 d . . . C4 C -0.0426(7) 0.2699(5) 1.0870(4) 0.030(2) Uani 1 1 d . . . H4A H -0.0604 0.2273 1.1147 0.036 Uiso 1 1 calc R . . H4B H -0.0429 0.3082 1.105 0.036 Uiso 1 1 calc R . . C51 C 0.7925(7) 0.1644(5) 0.4490(3) 0.030(2) Uani 1 1 d . . . O51 O 0.8079(6) 0.0996(4) 0.4427(3) 0.0465(18) Uani 1 1 d . . . C52 C 0.7041(7) 0.1800(5) 0.4703(4) 0.033(2) Uani 1 1 d . H . C53 C 0.6894(7) 0.2459(5) 0.4750(4) 0.032(2) Uani 1 1 d . . . H53 H 0.6286 0.2577 0.4898 0.039 Uiso 1 1 calc R . . C54 C 0.7620(6) 0.2951(5) 0.4586(4) 0.028(2) Uani 1 1 d . . . S5 S 0.74224(19) 0.37819(14) 0.46696(12) 0.0430(7) Uani 1 1 d . . . O52 O 0.7436(10) 0.4230(4) 0.4143(5) 0.097(4) Uani 1 1 d . . . O53 O 0.6493(6) 0.3767(4) 0.4944(4) 0.069(3) Uani 1 1 d . . . O54 O 0.8238(6) 0.3935(4) 0.4969(4) 0.061(2) Uani 1 1 d . . . C55 C 0.8516(7) 0.2792(5) 0.4372(4) 0.033(2) Uani 1 1 d . . . H55 H 0.9012 0.3134 0.426 0.039 Uiso 1 1 calc R . . C56 C 0.8682(7) 0.2130(5) 0.4322(3) 0.030(2) Uani 1 1 d . . . C5 C 0.9679(8) 0.1950(6) 0.4102(4) 0.040(3) Uani 1 1 d U . . H5A H 0.9611 0.1519 0.3985 0.048 Uiso 1 1 calc R . . H5B H 0.9873 0.2319 0.378 0.048 Uiso 1 1 calc R . . C61 C 0.6962(7) 0.0646(5) 0.5801(4) 0.027(2) Uani 1 1 d U . . O61 O 0.7649(5) 0.0403(3) 0.5511(3) 0.0336(15) Uani 1 1 d . . . C62 C 0.7022(7) 0.0475(5) 0.6380(4) 0.030(2) Uani 1 1 d . . . C63 C 0.6255(8) 0.0695(5) 0.6664(4) 0.036(2) Uani 1 1 d . . . H63 H 0.6264 0.0579 0.705 0.043 Uiso 1 1 calc R . . C64 C 0.5472(7) 0.1082(5) 0.6399(4) 0.033(2) Uani 1 1 d . H . S6 S 0.4518(2) 0.13529(15) 0.67706(12) 0.0436(7) Uani 1 1 d . . . O62 O 0.4485(6) 0.0877(4) 0.7302(3) 0.053(2) Uani 1 1 d . H . O63 O 0.4826(5) 0.2035(4) 0.6804(3) 0.0492(19) Uani 1 1 d . H . O64 O 0.3616(5) 0.1363(5) 0.6476(3) 0.055(2) Uani 1 1 d . H . C65 C 0.5458(7) 0.1267(5) 0.5840(4) 0.032(2) Uani 1 1 d . . . H65 H 0.4929 0.1538 0.566 0.039 Uiso 1 1 calc R H . C66 C 0.6214(7) 0.1057(5) 0.5537(4) 0.033(2) Uani 1 1 d . H . C6 C 0.6239(8) 0.1267(6) 0.4920(4) 0.040(2) Uani 1 1 d . . . H6A H 0.5587 0.1458 0.4788 0.047 Uiso 1 1 calc R H . H6B H 0.6363 0.0856 0.478 0.047 Uiso 1 1 calc R . . C71 C 0.9560(7) 0.0306(5) 0.6265(3) 0.028(2) Uani 1 1 d . . . O71 O 0.9328(6) -0.0016(4) 0.5882(3) 0.0469(19) Uani 1 1 d . . . C72 C 1.0507(7) 0.0584(5) 0.6271(4) 0.032(2) Uani 1 1 d . . . C73 C 1.0744(7) 0.0914(5) 0.6675(4) 0.033(2) Uani 1 1 d . . . H73 H 1.1383 0.1106 0.6683 0.039 Uiso 1 1 calc R . . C74 C 1.0028(8) 0.0958(5) 0.7065(4) 0.037(2) Uani 1 1 d . . . S7 S 1.0314(2) 0.13639(16) 0.75829(11) 0.0492(7) Uani 1 1 d . . . O72 O 1.1237(8) 0.1731(6) 0.7441(4) 0.082(3) Uani 1 1 d . . . O73 O 0.9529(8) 0.1837(6) 0.7611(4) 0.089(3) Uani 1 1 d . . . O74 O 1.0372(11) 0.0836(6) 0.8078(4) 0.105(4) Uani 1 1 d U . . C75 C 0.9086(7) 0.0688(5) 0.7054(4) 0.031(2) Uani 1 1 d . . . H75 H 0.8603 0.0726 0.7321 0.037 Uiso 1 1 calc R . . C76 C 0.8853(7) 0.0362(5) 0.6651(3) 0.029(2) Uani 1 1 d . . . C7 C 0.7856(7) 0.0019(5) 0.6668(4) 0.033(2) Uani 1 1 d . . . H7A H 0.7653 -0.0166 0.7053 0.039 Uiso 1 1 calc R . . H7B H 0.7932 -0.0376 0.6503 0.039 Uiso 1 1 calc R . . C81 C 1.0525(7) 0.1251(5) 0.4944(3) 0.031(2) Uani 1 1 d . . . O81 O 0.9843(5) 0.0758(4) 0.4968(3) 0.0433(18) Uani 1 1 d . . . C82 C 1.0481(7) 0.1863(5) 0.4516(4) 0.032(2) Uani 1 1 d . . . C83 C 1.1174(7) 0.2361(5) 0.4496(4) 0.033(2) Uani 1 1 d . . . H83 H 1.1161 0.2763 0.4204 0.04 Uiso 1 1 calc R . . C84 C 1.1887(7) 0.2306(5) 0.4880(4) 0.033(2) Uani 1 1 d . . . S8 S 1.27609(17) 0.29598(14) 0.48468(10) 0.0388(6) Uani 1 1 d . . . O82 O 1.2770(5) 0.3376(4) 0.4294(3) 0.054(2) Uani 1 1 d . . . O83 O 1.2410(5) 0.3343(4) 0.5237(3) 0.0497(19) Uani 1 1 d . . . O84 O 1.3694(5) 0.2630(4) 0.5014(3) 0.0419(18) Uani 1 1 d . . . C85 C 1.1916(7) 0.1709(5) 0.5311(4) 0.034(2) Uani 1 1 d . . . H85 H 1.2412 0.1663 0.5577 0.041 Uiso 1 1 calc R . . C86 C 1.1237(7) 0.1197(5) 0.5348(4) 0.029(2) Uani 1 1 d . . . C8 C 1.1276(8) 0.0563(5) 0.5826(4) 0.037(2) Uani 1 1 d . . . H8A H 1.1163 0.0148 0.5692 0.044 Uiso 1 1 calc R . . H8B H 1.1945 0.0527 0.5982 0.044 Uiso 1 1 calc R . . N91 N 0.0203(6) 0.2631(4) 0.8778(3) 0.036(2) Uani 1 1 d . . . C92 C 0.0614(8) 0.2732(5) 0.8278(4) 0.037(2) Uani 1 1 d . . . H92 H 0.0341 0.2586 0.7984 0.045 Uiso 1 1 calc R . . N93 N 0.1455(6) 0.3065(4) 0.8260(3) 0.0318(18) Uani 1 1 d . . . C94 C 0.1606(9) 0.3173(5) 0.8771(4) 0.039(3) Uani 1 1 d . . . H94 H 0.2159 0.3393 0.8879 0.047 Uiso 1 1 calc R . . C95 C 0.0822(8) 0.2909(5) 0.9081(4) 0.039(3) Uani 1 1 d . . . H95 H 0.0716 0.2915 0.945 0.047 Uiso 1 1 calc R . . C96 C -0.0721(9) 0.2271(7) 0.8947(6) 0.064(4) Uani 1 1 d . . . H96A H -0.0879 0.1989 0.8697 0.096 Uiso 1 1 calc R . . H96B H -0.1252 0.2605 0.8945 0.096 Uiso 1 1 calc R . . H96C H -0.0658 0.1975 0.9315 0.096 Uiso 1 1 calc R . . C97 C 0.2123(8) 0.3248(6) 0.7793(4) 0.044(3) Uani 1 1 d . H . H97A H 0.2448 0.3691 0.7788 0.053 Uiso 1 1 calc R . . H97B H 0.1736 0.3313 0.7458 0.053 Uiso 1 1 calc R . . C98 C 0.2909(8) 0.2710(6) 0.7797(5) 0.044(3) Uani 1 1 d . . . O91 O 0.3036(5) 0.2254(4) 0.8231(3) 0.0397(17) Uani 1 1 d . H . O92 O 0.3382(7) 0.2761(5) 0.7362(3) 0.061(2) Uani 1 1 d . H . N101 N 1.1706(7) 0.7563(5) 0.3793(4) 0.051(2) Uani 1 1 d . . . C102 C 1.1062(7) 0.7266(6) 0.3546(4) 0.044(3) Uani 1 1 d . . . H102 H 1.1197 0.7073 0.3247 0.053 Uiso 1 1 calc R . . N103 N 1.0215(6) 0.7285(5) 0.3781(4) 0.050(2) Uani 1 1 d . . . C104 C 1.0283(12) 0.7577(7) 0.4203(5) 0.066(4) Uani 1 1 d . . . H104 H 0.9768 0.7629 0.4449 0.079 Uiso 1 1 calc R . . C105 C 1.1204(11) 0.7773(6) 0.4200(5) 0.056(3) Uani 1 1 d U . . H105 H 1.1479 0.8017 0.4438 0.067 Uiso 1 1 calc R . . C106 C 1.2772(11) 0.7602(9) 0.3691(7) 0.089(5) Uani 1 1 d U . . H10A H 1.3026 0.7145 0.3689 0.133 Uiso 1 1 calc R . . H10B H 1.3094 0.7765 0.3977 0.133 Uiso 1 1 calc R . . H10C H 1.2914 0.7922 0.3338 0.133 Uiso 1 1 calc R . . C107 C 0.9309(16) 0.6878(10) 0.3645(9) 0.123(3) Uani 1 1 d DU . . H10D H 0.9335 0.6866 0.3259 0.147 Uiso 1 1 calc R . . H10E H 0.868 0.7098 0.3717 0.147 Uiso 1 1 calc R . . C108 C 0.9383(13) 0.6110(10) 0.4034(9) 0.124(3) Uani 1 1 d DU . . O101 O 0.8536(11) 0.5699(8) 0.4059(6) 0.126(3) Uani 1 1 d DU . . O102 O 1.0340(11) 0.5834(8) 0.4249(6) 0.126(3) Uani 1 1 d DU . . P1 P -0.28371(15) 0.80500(11) 0.75461(9) 0.0207(5) Uani 1 1 d . . . C111 C -0.3339(6) 0.8414(4) 0.6889(3) 0.0207(18) Uani 1 1 d . . . C112 C -0.4143(6) 0.8855(4) 0.6832(3) 0.0198(17) Uani 1 1 d . . . H112 H -0.4477 0.8923 0.7147 0.024 Uiso 1 1 calc R . . C113 C -0.4466(6) 0.9197(4) 0.6324(3) 0.0211(18) Uani 1 1 d . . . H113 H -0.5023 0.9494 0.6289 0.025 Uiso 1 1 calc R . . C114 C -0.3969(6) 0.9102(4) 0.5864(3) 0.0166(17) Uani 1 1 d U . . C115 C -0.3182(6) 0.8645(4) 0.5919(3) 0.0232(18) Uani 1 1 d . . . H115 H -0.2852 0.8571 0.5605 0.028 Uiso 1 1 calc R . . C116 C -0.2879(6) 0.8299(4) 0.6429(4) 0.0239(19) Uani 1 1 d . . . H116 H -0.235 0.7978 0.6464 0.029 Uiso 1 1 calc R . . O117 O -0.4300(4) 0.9480(3) 0.5387(2) 0.0260(14) Uani 1 1 d . . . C117 C -0.3763(7) 0.9420(5) 0.4901(4) 0.030(2) Uani 1 1 d . . . H11A H -0.3071 0.9554 0.4922 0.045 Uiso 1 1 calc R . . H11B H -0.4064 0.9722 0.4581 0.045 Uiso 1 1 calc R . . H11C H -0.379 0.8943 0.4873 0.045 Uiso 1 1 calc R . . C121 C -0.2794(6) 0.7127(4) 0.7662(3) 0.0221(18) Uani 1 1 d . . . C122 C -0.3224(6) 0.6797(5) 0.7307(4) 0.026(2) Uani 1 1 d . . . H122 H -0.3547 0.7059 0.6995 0.031 Uiso 1 1 calc R . . C123 C -0.3186(6) 0.6095(5) 0.7403(4) 0.033(2) Uani 1 1 d . . . H123 H -0.3464 0.5872 0.7152 0.04 Uiso 1 1 calc R . . C124 C -0.2741(6) 0.5713(5) 0.7867(4) 0.029(2) Uani 1 1 d . . . H124 H -0.2733 0.5225 0.7942 0.034 Uiso 1 1 calc R . . C125 C -0.2307(6) 0.6044(4) 0.8222(4) 0.0247(19) Uani 1 1 d . . . H125 H -0.1991 0.5782 0.8538 0.03 Uiso 1 1 calc R . . C126 C -0.2331(6) 0.6742(5) 0.8120(3) 0.0236(19) Uani 1 1 d . . . H126 H -0.2031 0.6966 0.8364 0.028 Uiso 1 1 calc R . . C131 C -0.1603(6) 0.8388(4) 0.7595(4) 0.0242(19) Uani 1 1 d . . . C132 C -0.0950(6) 0.8530(5) 0.7147(4) 0.034(2) Uani 1 1 d . . . H132 H -0.1149 0.8448 0.6813 0.041 Uiso 1 1 calc R . . C133 C -0.0027(7) 0.8787(5) 0.7189(4) 0.036(2) Uani 1 1 d . . . H133 H 0.0422 0.8861 0.6887 0.043 Uiso 1 1 calc R . . C134 C 0.0260(6) 0.8940(5) 0.7661(4) 0.031(2) Uani 1 1 d . . . H134 H 0.0894 0.9132 0.7685 0.038 Uiso 1 1 calc R . . C135 C -0.0390(7) 0.8809(5) 0.8100(4) 0.035(2) Uani 1 1 d . . . H135 H -0.0197 0.8914 0.8427 0.042 Uiso 1 1 calc R . . C136 C -0.1311(7) 0.8531(5) 0.8076(4) 0.032(2) Uani 1 1 d . . . H136 H -0.1743 0.8436 0.8385 0.038 Uiso 1 1 calc R . . C141 C -0.3582(6) 0.8272(5) 0.8067(3) 0.027(2) Uani 1 1 d . . . C142 C -0.3628(8) 0.8957(5) 0.8087(4) 0.040(2) Uani 1 1 d . . . H142 H -0.3286 0.93 0.7821 0.048 Uiso 1 1 calc R . . C143 C -0.4169(9) 0.9140(6) 0.8495(4) 0.053(3) Uani 1 1 d . . . H143 H -0.419 0.9608 0.8508 0.063 Uiso 1 1 calc R . . C144 C -0.4666(9) 0.8667(7) 0.8872(5) 0.054(3) Uani 1 1 d . . . H144 H -0.5036 0.8802 0.915 0.065 Uiso 1 1 calc R . . C145 C -0.4641(7) 0.7964(6) 0.8858(4) 0.046(3) Uani 1 1 d . . . H145 H -0.5001 0.7628 0.9121 0.055 Uiso 1 1 calc R . . C146 C -0.4088(6) 0.7776(5) 0.8458(3) 0.029(2) Uani 1 1 d . . . H146 H -0.4053 0.7306 0.8449 0.035 Uiso 1 1 calc R . . P2 P 0.31595(15) 0.71520(11) 0.74376(8) 0.0187(5) Uani 1 1 d . . . C211 C 0.3624(6) 0.6733(4) 0.8098(3) 0.0205(18) Uani 1 1 d . . . C212 C 0.4494(6) 0.6355(4) 0.8150(3) 0.0221(18) Uani 1 1 d . . . H212 H 0.4866 0.6328 0.7835 0.027 Uiso 1 1 calc R . . C213 C 0.4818(6) 0.6020(4) 0.8655(3) 0.0213(18) Uani 1 1 d . . . H213 H 0.5415 0.5763 0.8687 0.026 Uiso 1 1 calc R . . C214 C 0.4283(6) 0.6052(4) 0.9120(3) 0.0192(17) Uani 1 1 d . . . C215 C 0.3421(6) 0.6440(5) 0.9073(3) 0.027(2) Uani 1 1 d . . . H215 H 0.3057 0.6473 0.9388 0.032 Uiso 1 1 calc R . . C216 C 0.3100(6) 0.6773(5) 0.8567(4) 0.029(2) Uani 1 1 d . . . H216 H 0.2509 0.7037 0.8536 0.035 Uiso 1 1 calc R . . O217 O 0.4660(4) 0.5698(3) 0.9590(2) 0.0299(15) Uani 1 1 d . . . C217 C 0.4079(7) 0.5665(5) 1.0071(4) 0.034(2) Uani 1 1 d . . . H21A H 0.4058 0.6119 1.0147 0.051 Uiso 1 1 calc R . . H21B H 0.4375 0.5334 1.0378 0.051 Uiso 1 1 calc R . . H21C H 0.3405 0.5518 1.002 0.051 Uiso 1 1 calc R . . C221 C 0.3149(6) 0.8070(4) 0.7342(4) 0.0247(19) Uani 1 1 d . . . C222 C 0.3553(7) 0.8383(5) 0.7705(4) 0.030(2) Uani 1 1 d . . . H222 H 0.385 0.8117 0.8025 0.036 Uiso 1 1 calc R . . C223 C 0.3525(7) 0.9099(5) 0.7602(5) 0.040(3) Uani 1 1 d . . . H223 H 0.3798 0.932 0.7855 0.048 Uiso 1 1 calc R . . C224 C 0.3100(7) 0.9492(5) 0.7129(5) 0.041(3) Uani 1 1 d . . . H224 H 0.3086 0.9979 0.7059 0.049 Uiso 1 1 calc R . . C225 C 0.2700(7) 0.9167(5) 0.6766(4) 0.036(2) Uani 1 1 d . . . H225 H 0.2404 0.9431 0.6445 0.043 Uiso 1 1 calc R . . C226 C 0.2726(6) 0.8460(5) 0.6865(4) 0.028(2) Uani 1 1 d . . . H226 H 0.2458 0.8239 0.6611 0.034 Uiso 1 1 calc R . . C231 C 0.1886(6) 0.6905(4) 0.7376(3) 0.0215(18) Uani 1 1 d . . . C232 C 0.1157(7) 0.7134(5) 0.7684(4) 0.030(2) Uani 1 1 d . . . H232 H 0.1325 0.743 0.7908 0.037 Uiso 1 1 calc R . . C233 C 0.0193(6) 0.6927(5) 0.7662(4) 0.036(2) Uani 1 1 d . . . H233 H -0.0305 0.7079 0.7874 0.043 Uiso 1 1 calc R . . C234 C -0.0059(7) 0.6510(5) 0.7341(4) 0.030(2) Uani 1 1 d . . . H234 H -0.0725 0.6363 0.7336 0.036 Uiso 1 1 calc R . . C235 C 0.0648(7) 0.6299(5) 0.7022(4) 0.030(2) Uani 1 1 d . . . H235 H 0.0464 0.6024 0.6786 0.035 Uiso 1 1 calc R . . C236 C 0.1631(6) 0.6487(5) 0.7045(3) 0.0256(19) Uani 1 1 d . . . H236 H 0.2124 0.6329 0.6834 0.031 Uiso 1 1 calc R . . C241 C 0.3917(6) 0.6898(5) 0.6937(3) 0.0228(19) Uani 1 1 d . . . C242 C 0.4405(6) 0.7381(5) 0.6528(3) 0.0219(18) Uani 1 1 d . . . H242 H 0.4341 0.7857 0.651 0.026 Uiso 1 1 calc R . . C243 C 0.4984(6) 0.7165(5) 0.6148(3) 0.025(2) Uani 1 1 d . . . H243 H 0.5326 0.7492 0.5871 0.03 Uiso 1 1 calc R . . C244 C 0.5067(6) 0.6472(5) 0.6173(4) 0.031(2) Uani 1 1 d . . . H244 H 0.5463 0.6326 0.5909 0.037 Uiso 1 1 calc R . . C245 C 0.4576(6) 0.5986(5) 0.6578(4) 0.031(2) Uani 1 1 d . . . H245 H 0.4629 0.5511 0.6592 0.037 Uiso 1 1 calc R . . C246 C 0.4009(6) 0.6205(5) 0.6963(4) 0.0244(19) Uani 1 1 d . . . H246 H 0.3681 0.5877 0.7247 0.029 Uiso 1 1 calc R . . O1 O 0.6321(8) 0.0206(5) 0.9564(4) 0.082(3) Uani 1 1 d . . . O2 O 0.7568(7) 0.5090(4) 0.3119(4) 0.065(2) Uani 1 1 d . . . O3 O 0.1796(15) 0.9575(9) 0.1515(8) 0.090(8) Uani 0.5 1 d P . . O4 O 0.5315(8) 0.4921(5) 0.4501(5) 0.090(3) Uani 1 1 d . A 1 O5 O 0.1383(15) 0.9597(8) 0.8627(7) 0.071(5) Uani 0.5 1 d PU B 1 O6 O 0.6509(10) 0.4606(7) 0.7063(5) 0.037(3) Uani 0.5 1 d P C 1 O7 O 0.7388(11) 0.2655(11) 0.7557(6) 0.065(5) Uani 0.5 1 d PU D 1 O8 O 0.6779(10) 0.1524(8) 0.8396(5) 0.041(4) Uani 0.5 1 d P E 1 O9 O 0.8808(9) 0.5916(6) 0.6251(5) 0.035(3) Uani 0.5 1 d PU F 1 O10 O 1.2421(16) 0.6112(13) 0.3854(10) 0.097(7) Uani 0.5 1 d PU G 1 O111 O 0.3040(5) 0.2705(5) 0.6287(3) 0.055(2) Uani 1 1 d . H . O112 O 0.3512(6) 0.4065(5) 0.6022(3) 0.064(2) Uani 1 1 d . H . O113 O 0.4126(7) 0.4150(4) 0.6994(4) 0.064(2) Uani 1 1 d . H . O114 O 0.5415(7) 0.3016(5) 0.7393(4) 0.069(3) Uani 1 1 d . H . O115 O 0.4932(6) 0.3074(5) 0.5725(3) 0.059(2) Uani 1 1 d . H . O116 O 0.5943(15) 0.3578(12) 0.6368(9) 0.077(4) Uani 0.5 1 d PU H 1 O118 O 0.5670(15) 0.4039(12) 0.6300(9) 0.077(4) Uani 0.5 1 d PU H 2 O211 O 0.3000(12) 0.0074(5) 0.9004(6) 0.126(5) Uani 1 1 d . . . O212 O 0.4535(10) 0.0649(7) 0.9427(4) 0.117(5) Uani 1 1 d U . . O213 O 0.4316(6) 0.2139(5) 0.9044(3) 0.061(2) Uani 1 1 d . . . O214 O 0.1654(6) 0.1230(4) 0.8792(3) 0.0447(18) Uani 1 1 d . . . O215 O 0.2885(7) 0.0966(5) 0.7978(3) 0.066(2) Uani 1 1 d . . . O216 O 0.4824(7) 0.1239(8) 0.8276(4) 0.109(5) Uani 1 1 d . . . O311 O 0.9713(12) 0.4549(8) 0.4057(8) 0.060(5) Uani 0.5 1 d P . . O313 O 0.7886(12) 0.5325(9) 0.5146(6) 0.056(4) Uani 0.5 1 d P . . O314 O 0.9926(15) 0.5619(12) 0.5371(10) 0.089(6) Uani 0.5 1 d PU . . O315 O 1.091(2) 0.4467(15) 0.5016(13) 0.129(9) Uani 0.5 1 d PU . . 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 Y1 0.0356(6) 0.0580(7) 0.0373(6) -0.0141(5) -0.0038(4) -0.0035(5) Y2 0.0531(7) 0.0403(6) 0.0355(6) -0.0096(5) 0.0019(5) 0.0210(5) Y3 0.0504(13) 0.0305(12) 0.0630(15) -0.0181(10) -0.0013(11) -0.0195(9) O11 0.039(4) 0.033(4) 0.036(4) -0.016(3) -0.009(3) 0.000(3) C11 0.031(5) 0.021(5) 0.038(5) -0.010(4) -0.012(4) 0.013(4) C12 0.031(5) 0.010(4) 0.036(5) -0.001(4) -0.012(4) 0.004(3) C13 0.043(6) 0.019(5) 0.031(5) -0.006(4) -0.009(4) 0.008(4) C14 0.059(6) 0.021(5) 0.030(5) -0.003(4) -0.016(5) 0.010(4) S1 0.089(2) 0.0426(17) 0.0293(14) -0.0083(12) -0.0250(15) 0.0016(15) O12 0.127(9) 0.143(10) 0.050(6) -0.062(6) -0.001(6) -0.026(7) O13 0.101(7) 0.054(5) 0.036(4) -0.022(4) -0.025(4) 0.009(5) O14 0.149(9) 0.064(6) 0.070(6) -0.010(5) -0.071(6) 0.019(6) C15 0.047(6) 0.013(5) 0.040(6) -0.002(4) -0.025(5) 0.008(4) C16 0.026(5) 0.022(5) 0.047(6) -0.012(4) -0.018(4) 0.010(4) C1 0.023(5) 0.039(6) 0.045(6) -0.022(5) -0.019(4) 0.008(4) C21 0.028(5) 0.032(5) 0.032(5) -0.020(4) -0.010(4) 0.004(4) O21 0.035(4) 0.034(4) 0.039(4) -0.018(3) -0.009(3) 0.008(3) C22 0.022(5) 0.029(5) 0.033(5) -0.015(4) -0.010(4) -0.001(4) C23 0.021(5) 0.033(5) 0.030(5) -0.010(4) -0.012(4) 0.001(4) C24 0.021(5) 0.041(6) 0.034(5) -0.016(4) -0.002(4) -0.003(4) S2 0.0364(14) 0.0467(16) 0.0313(13) -0.0139(12) -0.0003(11) -0.0025(11) O22 0.029(4) 0.097(7) 0.042(4) -0.019(4) -0.002(3) 0.004(4) O23 0.066(5) 0.057(5) 0.036(4) -0.019(4) 0.015(4) -0.007(4) O24 0.049(5) 0.057(5) 0.037(4) -0.018(4) 0.005(3) -0.005(4) C25 0.045(6) 0.025(5) 0.028(5) -0.005(4) -0.008(4) -0.009(4) C26 0.032(5) 0.028(5) 0.027(5) -0.011(4) -0.008(4) 0.000(4) C2 0.052(6) 0.023(5) 0.027(5) -0.003(4) -0.007(4) 0.009(4) C31 0.039(5) 0.037(5) 0.016(4) -0.012(4) -0.019(4) 0.015(4) O31 0.032(4) 0.038(4) 0.057(5) -0.026(4) -0.013(3) 0.006(3) C32 0.036(5) 0.033(5) 0.016(4) -0.006(4) -0.011(4) 0.007(4) C33 0.036(5) 0.035(6) 0.017(4) -0.002(4) -0.008(4) 0.001(4) C34 0.049(6) 0.026(5) 0.015(4) -0.002(4) -0.007(4) 0.008(4) S3 0.075(2) 0.0310(14) 0.0278(13) -0.0041(11) 0.0059(13) 0.0115(13) O32 0.121(8) 0.043(5) 0.044(5) -0.011(4) 0.009(5) 0.024(5) O33 0.089(7) 0.058(6) 0.049(5) -0.033(4) 0.014(4) -0.020(5) O34 0.054(5) 0.037(4) 0.050(5) -0.020(4) -0.007(4) 0.012(3) C35 0.026(5) 0.043(6) 0.014(4) 0.001(4) -0.007(4) 0.016(4) C36 0.033(5) 0.045(6) 0.011(4) -0.011(4) -0.008(4) 0.011(4) C3 0.032(5) 0.049(6) 0.024(5) -0.014(4) -0.018(4) 0.017(4) C41 0.021(4) 0.030(5) 0.040(5) -0.021(4) 0.002(4) 0.001(4) O41 0.032(4) 0.027(4) 0.046(4) -0.014(3) -0.016(3) 0.005(3) C42 0.019(4) 0.027(5) 0.024(5) -0.005(4) -0.002(3) 0.010(4) C43 0.019(5) 0.048(6) 0.036(5) -0.026(5) -0.008(4) 0.004(4) C44 0.034(5) 0.031(5) 0.023(5) -0.012(4) 0.000(4) 0.003(4) S4 0.0365(15) 0.0575(18) 0.0378(15) -0.0178(13) 0.0056(11) -0.0197(12) O42 0.039(4) 0.083(6) 0.043(4) -0.004(4) -0.013(3) -0.018(4) O43 0.088(7) 0.103(8) 0.059(6) -0.050(5) 0.039(5) -0.062(6) O44 0.043(4) 0.048(5) 0.043(4) -0.001(4) 0.001(3) -0.009(3) C45 0.030(5) 0.034(5) 0.027(5) -0.011(4) 0.004(4) 0.001(4) C46 0.029(5) 0.023(5) 0.029(5) -0.009(4) 0.006(4) 0.004(4) C4 0.036(5) 0.029(5) 0.022(5) -0.002(4) -0.008(4) 0.002(4) C51 0.051(6) 0.028(5) 0.008(4) 0.001(4) -0.007(4) -0.020(4) O51 0.066(5) 0.037(4) 0.039(4) -0.014(3) 0.002(4) -0.008(4) C52 0.029(5) 0.051(7) 0.017(5) -0.006(4) -0.012(4) -0.011(4) C53 0.027(5) 0.048(6) 0.024(5) -0.012(4) -0.011(4) -0.010(4) C54 0.025(5) 0.029(5) 0.033(5) -0.010(4) -0.010(4) -0.005(4) S5 0.0340(14) 0.0364(15) 0.0608(18) -0.0152(13) -0.0107(12) -0.0102(11) O52 0.168(11) 0.025(5) 0.094(8) -0.005(5) 0.003(7) -0.020(6) O53 0.037(5) 0.047(5) 0.129(9) -0.033(5) 0.013(5) -0.007(4) O54 0.042(5) 0.068(6) 0.090(7) -0.051(5) -0.013(4) -0.005(4) C55 0.037(6) 0.035(6) 0.019(5) 0.005(4) -0.005(4) -0.010(4) C56 0.042(6) 0.034(6) 0.011(4) 0.000(4) -0.007(4) -0.004(4) C5 0.063(7) 0.039(6) 0.014(4) 0.002(4) 0.007(4) -0.006(5) C61 0.031(5) 0.024(5) 0.032(5) -0.016(4) 0.005(4) -0.017(4) O61 0.042(4) 0.030(4) 0.028(3) -0.007(3) 0.002(3) -0.015(3) C62 0.032(5) 0.030(5) 0.030(5) -0.011(4) -0.003(4) -0.015(4) C63 0.047(6) 0.029(5) 0.034(5) -0.015(4) 0.000(5) -0.012(4) C64 0.034(5) 0.027(5) 0.042(6) -0.015(4) -0.006(4) -0.007(4) S6 0.0344(14) 0.0527(18) 0.0487(16) -0.0225(14) 0.0068(12) -0.0063(12) O62 0.046(5) 0.074(6) 0.037(4) -0.010(4) 0.012(3) -0.004(4) O63 0.043(4) 0.058(5) 0.056(5) -0.031(4) -0.002(4) -0.005(4) O64 0.031(4) 0.080(6) 0.063(5) -0.030(5) 0.006(4) -0.006(4) C65 0.032(5) 0.030(5) 0.036(6) -0.011(4) 0.002(4) -0.013(4) C66 0.029(5) 0.032(5) 0.038(6) -0.008(4) -0.012(4) -0.016(4) C6 0.047(6) 0.043(6) 0.030(5) -0.012(5) -0.003(5) -0.012(5) C71 0.042(6) 0.022(5) 0.018(4) -0.004(4) -0.003(4) -0.001(4) O71 0.053(5) 0.063(5) 0.034(4) -0.029(4) 0.008(3) -0.002(4) C72 0.045(6) 0.018(5) 0.029(5) 0.001(4) 0.002(4) 0.013(4) C73 0.037(5) 0.019(5) 0.041(6) -0.004(4) -0.009(4) 0.001(4) C74 0.051(6) 0.031(6) 0.028(5) -0.007(4) -0.002(5) 0.009(5) S7 0.0622(19) 0.0565(19) 0.0357(15) -0.0238(14) -0.0034(13) -0.0113(15) O72 0.102(8) 0.096(8) 0.058(6) -0.039(6) 0.004(5) -0.033(6) O73 0.100(8) 0.103(8) 0.090(8) -0.076(7) 0.002(6) 0.006(6) O74 0.191(11) 0.075(7) 0.054(6) -0.021(5) -0.042(7) -0.022(7) C75 0.042(6) 0.022(5) 0.024(5) 0.000(4) 0.004(4) -0.008(4) C76 0.042(6) 0.026(5) 0.018(4) -0.002(4) 0.002(4) -0.001(4) C7 0.045(6) 0.033(5) 0.018(5) -0.002(4) 0.010(4) -0.008(4) C81 0.029(5) 0.047(6) 0.019(5) -0.014(4) 0.009(4) 0.009(4) O81 0.055(5) 0.042(4) 0.033(4) -0.011(3) 0.003(3) -0.009(4) C82 0.035(5) 0.040(6) 0.020(5) -0.010(4) 0.013(4) 0.001(4) C83 0.031(5) 0.045(6) 0.021(5) -0.004(4) 0.013(4) 0.011(4) C84 0.025(5) 0.042(6) 0.033(5) -0.012(4) 0.007(4) 0.006(4) S8 0.0234(12) 0.0510(16) 0.0367(14) -0.0013(12) 0.0070(10) -0.0006(11) O82 0.024(4) 0.071(6) 0.050(5) 0.015(4) 0.006(3) -0.010(3) O83 0.031(4) 0.050(5) 0.067(5) -0.014(4) 0.003(4) -0.002(3) O84 0.027(4) 0.059(5) 0.035(4) -0.005(3) 0.004(3) 0.004(3) C85 0.029(5) 0.050(6) 0.020(5) -0.003(4) 0.006(4) 0.017(5) C86 0.031(5) 0.028(5) 0.029(5) -0.009(4) 0.023(4) 0.001(4) C8 0.049(6) 0.028(5) 0.029(5) -0.001(4) 0.009(4) 0.009(4) N91 0.048(5) 0.027(4) 0.037(5) -0.014(4) 0.003(4) 0.010(4) C92 0.047(6) 0.033(6) 0.040(6) -0.023(5) -0.011(5) 0.009(5) N93 0.041(5) 0.024(4) 0.028(4) -0.002(3) -0.013(4) 0.004(4) C94 0.061(7) 0.025(5) 0.034(6) -0.013(4) -0.023(5) 0.008(5) C95 0.058(7) 0.030(6) 0.036(6) -0.020(5) -0.018(5) 0.016(5) C96 0.056(8) 0.067(9) 0.078(9) -0.038(7) 0.027(7) -0.005(6) C97 0.060(7) 0.038(6) 0.031(6) -0.002(5) -0.011(5) -0.008(5) C98 0.034(6) 0.051(7) 0.052(7) -0.023(6) 0.005(5) -0.015(5) O91 0.034(4) 0.043(4) 0.041(4) -0.007(3) -0.009(3) 0.001(3) O92 0.075(6) 0.066(6) 0.047(5) -0.023(4) 0.021(4) -0.010(4) N101 0.050(6) 0.055(6) 0.052(6) -0.022(5) -0.012(5) -0.006(5) C102 0.032(6) 0.068(8) 0.040(6) -0.032(6) 0.008(5) -0.015(5) N103 0.033(5) 0.076(7) 0.040(5) -0.015(5) 0.001(4) 0.000(5) C104 0.090(11) 0.078(10) 0.035(7) -0.025(6) 0.001(6) 0.046(8) C105 0.088(8) 0.050(6) 0.036(5) -0.022(5) -0.013(5) -0.001(6) C106 0.071(8) 0.089(8) 0.099(9) -0.011(7) -0.012(7) -0.026(7) C107 0.125(5) 0.123(5) 0.121(5) -0.030(5) -0.007(5) -0.012(5) C108 0.128(5) 0.121(5) 0.123(5) -0.031(4) -0.008(4) -0.011(4) O101 0.132(5) 0.121(5) 0.124(5) -0.029(4) -0.010(4) -0.011(4) O102 0.132(5) 0.121(5) 0.124(5) -0.029(4) -0.010(4) -0.011(4) P1 0.0163(11) 0.0226(12) 0.0206(11) -0.0002(9) -0.0054(8) 0.0007(8) C111 0.019(4) 0.021(4) 0.021(4) -0.003(3) -0.005(3) -0.003(3) C112 0.012(4) 0.023(5) 0.025(4) -0.006(4) 0.000(3) 0.003(3) C113 0.013(4) 0.021(4) 0.031(5) -0.010(4) -0.008(3) 0.006(3) C114 0.019(4) 0.019(4) 0.015(4) -0.008(3) -0.010(3) -0.005(3) C115 0.021(4) 0.027(5) 0.024(5) -0.009(4) -0.004(3) 0.003(4) C116 0.014(4) 0.026(5) 0.032(5) -0.006(4) -0.001(4) 0.006(3) O117 0.022(3) 0.036(4) 0.021(3) -0.008(3) -0.007(2) 0.007(3) C117 0.026(5) 0.039(6) 0.026(5) -0.009(4) -0.012(4) 0.009(4) C121 0.014(4) 0.022(5) 0.029(5) -0.004(4) 0.000(3) 0.000(3) C122 0.019(4) 0.031(5) 0.026(5) -0.002(4) -0.012(4) 0.004(4) C123 0.018(5) 0.038(6) 0.044(6) -0.010(5) -0.010(4) 0.006(4) C124 0.029(5) 0.018(5) 0.039(5) -0.006(4) -0.011(4) 0.013(4) C125 0.020(4) 0.021(5) 0.028(5) 0.003(4) 0.000(4) 0.009(3) C126 0.013(4) 0.032(5) 0.023(4) -0.001(4) -0.002(3) 0.000(3) C131 0.015(4) 0.017(4) 0.039(5) -0.002(4) -0.007(4) 0.000(3) C132 0.020(5) 0.047(6) 0.039(6) -0.018(5) 0.000(4) -0.001(4) C133 0.027(5) 0.040(6) 0.044(6) -0.017(5) 0.002(4) 0.009(4) C134 0.018(4) 0.021(5) 0.054(6) -0.006(4) -0.010(4) -0.002(4) C135 0.041(6) 0.040(6) 0.021(5) 0.000(4) -0.007(4) -0.014(4) C136 0.035(5) 0.042(6) 0.015(4) 0.001(4) -0.004(4) -0.011(4) C141 0.027(5) 0.036(5) 0.016(4) 0.000(4) -0.005(4) 0.004(4) C142 0.057(7) 0.035(6) 0.025(5) -0.002(4) 0.007(5) 0.000(5) C143 0.075(8) 0.043(7) 0.038(6) -0.008(5) 0.018(6) 0.017(6) C144 0.060(8) 0.063(8) 0.035(6) -0.006(6) 0.020(5) 0.017(6) C145 0.029(6) 0.065(8) 0.036(6) 0.002(5) 0.002(5) -0.006(5) C146 0.024(5) 0.037(6) 0.021(5) 0.005(4) -0.005(4) 0.001(4) P2 0.0156(10) 0.0225(11) 0.0169(10) -0.0028(9) -0.0020(8) 0.0006(8) C211 0.018(4) 0.025(5) 0.018(4) -0.004(3) -0.004(3) 0.002(3) C212 0.011(4) 0.027(5) 0.027(5) -0.006(4) 0.009(3) 0.001(3) C213 0.009(4) 0.024(5) 0.031(5) -0.006(4) 0.001(3) 0.003(3) C214 0.014(4) 0.020(4) 0.022(4) -0.002(3) -0.011(3) 0.006(3) C215 0.025(5) 0.035(5) 0.021(4) -0.008(4) -0.003(4) 0.009(4) C216 0.015(4) 0.043(6) 0.028(5) -0.005(4) 0.001(4) 0.011(4) O217 0.018(3) 0.043(4) 0.026(3) -0.004(3) 0.000(3) 0.009(3) C217 0.025(5) 0.049(6) 0.025(5) -0.006(4) -0.002(4) 0.010(4) C221 0.018(4) 0.022(5) 0.032(5) -0.002(4) -0.001(4) -0.001(3) C222 0.027(5) 0.030(5) 0.035(5) -0.011(4) -0.005(4) 0.004(4) C223 0.024(5) 0.044(6) 0.061(7) -0.028(5) -0.011(5) -0.004(4) C224 0.026(5) 0.025(5) 0.072(8) -0.013(5) -0.005(5) 0.000(4) C225 0.031(5) 0.033(6) 0.041(6) 0.000(5) -0.006(4) 0.003(4) C226 0.023(5) 0.033(5) 0.026(5) -0.004(4) -0.006(4) -0.003(4) C231 0.018(4) 0.024(5) 0.020(4) -0.001(4) -0.002(3) 0.001(3) C232 0.031(5) 0.036(6) 0.028(5) -0.014(4) -0.003(4) 0.002(4) C233 0.015(5) 0.053(7) 0.042(6) -0.018(5) 0.003(4) 0.009(4) C234 0.021(5) 0.036(5) 0.031(5) -0.004(4) -0.005(4) -0.003(4) C235 0.035(5) 0.027(5) 0.025(5) -0.001(4) -0.010(4) -0.004(4) C236 0.020(4) 0.034(5) 0.022(4) -0.006(4) 0.000(4) 0.000(4) C241 0.021(4) 0.035(5) 0.012(4) -0.005(4) -0.002(3) 0.000(4) C242 0.015(4) 0.033(5) 0.018(4) -0.008(4) -0.010(3) -0.001(3) C243 0.014(4) 0.046(6) 0.014(4) -0.007(4) 0.000(3) -0.010(4) C244 0.021(5) 0.052(6) 0.024(5) -0.020(4) 0.004(4) -0.005(4) C245 0.026(5) 0.032(5) 0.036(5) -0.014(4) 0.002(4) -0.001(4) C246 0.016(4) 0.029(5) 0.029(5) -0.008(4) 0.005(4) -0.004(3) O1 0.080(7) 0.081(7) 0.080(7) -0.012(6) 0.000(5) 0.011(5) O2 0.084(6) 0.051(5) 0.063(6) -0.019(4) -0.008(5) 0.013(5) O3 0.097(15) 0.052(11) 0.095(15) 0.022(10) 0.076(12) 0.030(10) O4 0.070(7) 0.071(7) 0.120(9) -0.010(6) 0.005(6) 0.018(5) O5 0.114(13) 0.028(8) 0.072(11) -0.014(7) -0.047(10) 0.004(8) O6 0.037(8) 0.043(8) 0.041(8) -0.028(7) 0.015(6) -0.008(6) O7 0.037(8) 0.118(13) 0.038(8) -0.018(8) 0.013(6) -0.040(8) O8 0.033(8) 0.057(9) 0.024(7) 0.004(6) -0.008(6) -0.017(6) O9 0.027(6) 0.021(6) 0.048(7) 0.010(5) -0.022(5) -0.004(5) O10 0.081(10) 0.130(11) 0.095(10) -0.056(8) -0.004(8) 0.028(8) O111 0.032(4) 0.080(6) 0.057(5) -0.024(4) 0.005(4) -0.002(4) O112 0.062(5) 0.077(6) 0.051(5) -0.011(5) -0.018(4) 0.002(5) O113 0.079(6) 0.046(5) 0.067(6) -0.011(4) -0.025(5) -0.003(4) O114 0.066(6) 0.082(7) 0.076(6) -0.048(5) -0.030(5) 0.028(5) O115 0.037(4) 0.089(7) 0.047(5) -0.007(4) 0.004(4) -0.007(4) O116 0.066(6) 0.092(8) 0.075(6) -0.027(6) 0.009(5) -0.010(6) O118 0.066(6) 0.092(8) 0.075(6) -0.027(6) 0.009(5) -0.010(6) O211 0.205(15) 0.038(6) 0.129(11) -0.007(6) -0.032(10) 0.036(7) O212 0.162(10) 0.132(9) 0.069(7) -0.046(6) -0.054(7) 0.096(8) O213 0.040(5) 0.093(7) 0.046(5) -0.011(5) -0.014(4) -0.008(4) O214 0.066(5) 0.040(4) 0.030(4) -0.014(3) 0.009(3) -0.006(4) O215 0.078(6) 0.075(6) 0.051(5) -0.031(5) 0.023(4) -0.021(5) O216 0.042(5) 0.235(15) 0.071(7) -0.080(8) -0.015(5) 0.044(7) O311 0.055(10) 0.034(9) 0.102(15) -0.037(9) 0.005(9) 0.002(7) O313 0.061(10) 0.064(11) 0.043(9) -0.016(8) 0.010(8) -0.017(8) O314 0.081(12) 0.101(13) 0.110(14) -0.075(11) 0.017(10) -0.047(10) O315 0.123(16) 0.121(16) 0.148(17) -0.044(14) -0.034(14) 0.059(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Y1 O116 2.27(2) . ? Y1 O92 2.270(8) . ? Y1 O63 2.324(8) . ? Y1 O111 2.355(8) . ? Y1 O114 2.358(8) . ? Y1 O113 2.362(9) . ? Y1 O112 2.366(8) . ? Y1 O118 2.42(2) . ? Y1 O115 2.470(8) . ? Y2 O91 2.238(7) . ? Y2 O212 2.328(10) . ? Y2 O216 2.339(9) . ? Y2 O211 2.354(12) . ? Y2 O214 2.359(8) . ? Y2 O213 2.378(9) . ? Y2 O34 2.402(7) . ? Y2 O215 2.440(9) . ? Y3 O315 2.29(3) . ? Y3 O313 2.324(17) . ? Y3 O314 2.352(18) . ? Y3 O102 2.387(15) 2_766 ? Y3 O311 2.361(18) . ? Y3 O54 2.362(8) . ? Y3 O101 2.552(15) . ? Y3 O102 2.543(15) . ? O11 C11 1.355(11) . ? C11 C16 1.404(13) . ? C11 C12 1.405(14) . ? C12 C13 1.393(13) . ? C12 C2 1.528(13) . ? C13 C14 1.374(14) . ? C13 H13 0.95 . ? C14 C15 1.394(15) . ? C14 S1 1.766(10) . ? S1 O12 1.394(12) . ? S1 O13 1.411(9) . ? S1 O14 1.467(10) . ? C15 C16 1.380(14) . ? C15 H15 0.95 . ? C16 C1 1.511(14) . ? C1 C42 1.537(13) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C21 O21 1.352(11) . ? C21 C26 1.389(13) . ? C21 C22 1.410(12) . ? C22 C23 1.394(13) . ? C22 C3 1.511(13) . ? C23 C24 1.378(13) . ? C23 H23 0.95 . ? C24 C25 1.391(13) . ? C24 S2 1.778(9) . ? S2 O22 1.433(8) . ? S2 O24 1.459(8) . ? S2 O23 1.461(8) . ? C25 C26 1.386(14) . ? C25 H25 0.95 . ? C26 C2 1.518(13) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C31 O31 1.379(11) . ? C31 C36 1.388(13) . ? C31 C32 1.404(14) . ? C32 C33 1.370(13) . ? C32 C4 1.519(13) . ? C33 C34 1.373(13) . ? C33 H33 0.95 . ? C34 C35 1.377(14) . ? C34 S3 1.769(10) . ? S3 O34 1.446(8) . ? S3 O32 1.451(9) . ? S3 O33 1.462(9) . ? C35 C36 1.379(13) . ? C35 H35 0.95 . ? C36 C3 1.524(14) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C41 O41 1.357(11) . ? C41 C46 1.377(13) . ? C41 C42 1.409(12) . ? C42 C43 1.372(13) . ? C43 C44 1.384(14) . ? C43 H43 0.95 . ? C44 C45 1.373(13) . ? C44 S4 1.775(10) . ? S4 O42 1.435(9) . ? S4 O44 1.439(8) . ? S4 O43 1.448(9) . ? C45 C46 1.389(13) . ? C45 H45 0.95 . ? C46 C4 1.518(12) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C51 O51 1.366(12) . ? C51 C52 1.369(14) . ? C51 C56 1.401(13) . ? C52 C53 1.372(14) . ? C52 C6 1.523(14) . ? C53 C54 1.379(13) . ? C53 H53 0.95 . ? C54 C55 1.386(13) . ? C54 S5 1.754(10) . ? S5 O52 1.414(11) . ? S5 O53 1.421(9) . ? S5 O54 1.429(8) . ? C55 C56 1.384(14) . ? C55 H55 0.95 . ? C56 C5 1.524(14) . ? C5 C82 1.504(14) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C61 O61 1.339(11) . ? C61 C66 1.377(13) . ? C61 C62 1.429(13) . ? C62 C63 1.386(14) . ? C62 C7 1.527(14) . ? C63 C64 1.392(14) . ? C63 H63 0.95 . ? C64 C65 1.377(14) . ? C64 S6 1.748(10) . ? S6 O64 1.441(8) . ? S6 O62 1.448(8) . ? S6 O63 1.458(8) . ? C65 C66 1.393(14) . ? C65 H65 0.95 . ? C66 C6 1.520(14) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C71 O71 1.339(11) . ? C71 C76 1.381(13) . ? C71 C72 1.400(14) . ? C72 C73 1.397(14) . ? C72 C8 1.531(13) . ? C73 C74 1.390(14) . ? C73 H73 0.95 . ? C74 C75 1.389(14) . ? C74 S7 1.765(10) . ? S7 O74 1.432(11) . ? S7 O73 1.434(11) . ? S7 O72 1.445(10) . ? C75 C76 1.389(13) . ? C75 H75 0.95 . ? C76 C7 1.511(13) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C81 O81 1.344(12) . ? C81 C86 1.404(14) . ? C81 C82 1.427(13) . ? C82 C83 1.365(14) . ? C83 C84 1.371(14) . ? C83 H83 0.95 . ? C84 C85 1.407(14) . ? C84 S8 1.755(10) . ? S8 O84 1.443(7) . ? S8 O82 1.445(8) . ? S8 O83 1.471(8) . ? C85 C86 1.367(14) . ? C85 H85 0.95 . ? C86 C8 1.526(13) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? N91 C92 1.346(13) . ? N91 C95 1.360(13) . ? N91 C96 1.449(15) . ? C92 N93 1.315(13) . ? C92 H92 0.95 . ? N93 C94 1.390(12) . ? N93 C97 1.449(13) . ? C94 C95 1.336(16) . ? C94 H94 0.95 . ? C95 H95 0.95 . ? C96 H96A 0.98 . ? C96 H96B 0.98 . ? C96 H96C 0.98 . ? C97 C98 1.511(16) . ? C97 H97A 0.99 . ? C97 H97B 0.99 . ? C98 O92 1.249(13) . ? C98 O91 1.260(13) . ? N101 C102 1.312(13) . ? N101 C105 1.380(15) . ? N101 C106 1.457(17) . ? C102 N103 1.286(13) . ? C102 H102 0.95 . ? N103 C104 1.349(15) . ? N103 C107 1.57(2) . ? C104 C105 1.306(19) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C106 H10A 0.98 . ? C106 H10B 0.98 . ? C106 H10C 0.98 . ? C107 C108 1.615(17) . ? C107 H10D 0.99 . ? C107 H10E 0.99 . ? C108 O101 1.404(16) . ? C108 O102 1.466(16) . ? O102 Y3 2.387(15) 2_766 ? P1 C141 1.790(9) . ? P1 C111 1.793(8) . ? P1 C121 1.805(9) . ? P1 C131 1.821(8) . ? C111 C112 1.386(11) . ? C111 C116 1.386(12) . ? C112 C113 1.381(12) . ? C112 H112 0.95 . ? C113 C114 1.392(11) . ? C113 H113 0.95 . ? C114 O117 1.345(9) . ? C114 C115 1.389(11) . ? C115 C116 1.379(12) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? O117 C117 1.451(11) . ? C117 H11A 0.98 . ? C117 H11B 0.98 . ? C117 H11C 0.98 . ? C121 C122 1.383(12) . ? C121 C126 1.385(12) . ? C122 C123 1.372(13) . ? C122 H122 0.95 . ? C123 C124 1.384(13) . ? C123 H123 0.95 . ? C124 C125 1.388(13) . ? C124 H124 0.95 . ? C125 C126 1.363(12) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.389(13) . ? C131 C132 1.399(13) . ? C132 C133 1.369(14) . ? C132 H132 0.95 . ? C133 C134 1.376(14) . ? C133 H133 0.95 . ? C134 C135 1.379(14) . ? C134 H134 0.95 . ? C135 C136 1.375(13) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C141 C146 1.391(13) . ? C141 C142 1.393(14) . ? C142 C143 1.378(14) . ? C142 H142 0.95 . ? C143 C144 1.341(16) . ? C143 H143 0.95 . ? C144 C145 1.423(17) . ? C144 H144 0.95 . ? C145 C146 1.377(14) . ? C145 H145 0.95 . ? C146 H146 0.95 . ? P2 C241 1.789(8) . ? P2 C221 1.800(9) . ? P2 C211 1.804(8) . ? P2 C231 1.814(8) . ? C211 C212 1.387(11) . ? C211 C216 1.396(12) . ? C212 C213 1.371(12) . ? C212 H212 0.95 . ? C213 C214 1.389(12) . ? C213 H213 0.95 . ? C214 O217 1.338(10) . ? C214 C215 1.388(11) . ? C215 C216 1.371(12) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? O217 C217 1.429(11) . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C221 C222 1.364(13) . ? C221 C226 1.400(12) . ? C222 C223 1.396(14) . ? C222 H222 0.95 . ? C223 C224 1.395(15) . ? C223 H223 0.95 . ? C224 C225 1.379(15) . ? C224 H224 0.95 . ? C225 C226 1.378(13) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C236 1.379(12) . ? C231 C232 1.394(12) . ? C232 C233 1.377(13) . ? C232 H232 0.95 . ? C233 C234 1.358(14) . ? C233 H233 0.95 . ? C234 C235 1.373(13) . ? C234 H234 0.95 . ? C235 C236 1.389(12) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C241 C246 1.382(12) . ? C241 C242 1.390(12) . ? C242 C243 1.383(12) . ? C242 H242 0.95 . ? C243 C244 1.382(14) . ? C243 H243 0.95 . ? C244 C245 1.389(13) . ? C244 H244 0.95 . ? C245 C246 1.387(12) . ? C245 H245 0.95 . ? C246 H246 0.95 . ? 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 O116 Y1 O92 144.2(6) . . ? O116 Y1 O63 94.4(6) . . ? O92 Y1 O63 80.7(3) . . ? O116 Y1 O111 139.0(6) . . ? O92 Y1 O111 74.9(3) . . ? O63 Y1 O111 77.5(3) . . ? O116 Y1 O114 69.9(6) . . ? O92 Y1 O114 74.5(3) . . ? O63 Y1 O114 75.9(3) . . ? O111 Y1 O114 142.1(3) . . ? O116 Y1 O113 89.3(6) . . ? O92 Y1 O113 77.2(3) . . ? O63 Y1 O113 146.7(3) . . ? O111 Y1 O113 119.3(3) . . ? O114 Y1 O113 74.4(3) . . ? O116 Y1 O112 97.6(6) . . ? O92 Y1 O112 107.7(3) . . ? O63 Y1 O112 142.8(3) . . ? O111 Y1 O112 70.4(3) . . ? O114 Y1 O112 141.2(3) . . ? O113 Y1 O112 68.7(3) . . ? O92 Y1 O118 142.2(6) . . ? O63 Y1 O118 118.0(6) . . ? O111 Y1 O118 138.4(5) . . ? O114 Y1 O118 78.7(6) . . ? O113 Y1 O118 70.1(6) . . ? O112 Y1 O118 77.9(6) . . ? O116 Y1 O115 64.8(6) . . ? O92 Y1 O115 145.2(3) . . ? O63 Y1 O115 77.5(3) . . ? O111 Y1 O115 74.1(3) . . ? O114 Y1 O115 124.7(3) . . ? O113 Y1 O115 132.8(3) . . ? O112 Y1 O115 76.1(3) . . ? O118 Y1 O115 72.6(5) . . ? O91 Y2 O212 145.9(5) . . ? O91 Y2 O216 86.7(4) . . ? O212 Y2 O216 76.6(4) . . ? O91 Y2 O211 141.1(4) . . ? O212 Y2 O211 71.7(5) . . ? O216 Y2 O211 98.8(5) . . ? O91 Y2 O214 77.1(2) . . ? O212 Y2 O214 132.4(4) . . ? O216 Y2 O214 142.9(3) . . ? O211 Y2 O214 75.7(4) . . ? O91 Y2 O213 71.2(3) . . ? O212 Y2 O213 76.8(4) . . ? O216 Y2 O213 80.4(4) . . ? O211 Y2 O213 147.7(4) . . ? O214 Y2 O213 123.5(3) . . ? O91 Y2 O34 107.3(3) . . ? O212 Y2 O34 73.9(3) . . ? O216 Y2 O34 144.5(3) . . ? O211 Y2 O34 90.4(4) . . ? O214 Y2 O34 72.6(2) . . ? O213 Y2 O34 74.0(3) . . ? O91 Y2 O215 74.3(3) . . ? O212 Y2 O215 126.3(4) . . ? O216 Y2 O215 72.8(3) . . ? O211 Y2 O215 70.8(4) . . ? O214 Y2 O215 70.8(3) . . ? O213 Y2 O215 137.0(3) . . ? O34 Y2 O215 142.0(3) . . ? O315 Y3 O313 151.6(9) . . ? O315 Y3 O314 80.2(9) . . ? O313 Y3 O314 77.2(7) . . ? O315 Y3 O102 63.4(9) . 2_766 ? O313 Y3 O102 93.9(5) . 2_766 ? O314 Y3 O102 74.2(7) . 2_766 ? O315 Y3 O311 78.0(9) . . ? O313 Y3 O311 130.3(6) . . ? O314 Y3 O311 139.3(7) . . ? O102 Y3 O311 123.5(6) 2_766 . ? O315 Y3 O54 109.0(8) . . ? O313 Y3 O54 78.8(5) . . ? O314 Y3 O54 139.7(6) . . ? O102 Y3 O54 75.6(4) 2_766 . ? O311 Y3 O54 80.3(5) . . ? O315 Y3 O101 132.4(9) . . ? O313 Y3 O101 70.0(5) . . ? O314 Y3 O101 102.6(8) . . ? O102 Y3 O101 163.8(5) 2_766 . ? O311 Y3 O101 69.4(5) . . ? O54 Y3 O101 98.9(4) . . ? O315 Y3 O102 78.2(9) . . ? O313 Y3 O102 109.4(5) . . ? O314 Y3 O102 70.2(7) . . ? O102 Y3 O102 131.1(3) 2_766 . ? O311 Y3 O102 71.8(5) . . ? O54 Y3 O102 149.2(4) . . ? O101 Y3 O102 59.4(4) . . ? O11 C11 C16 118.5(9) . . ? O11 C11 C12 120.4(8) . . ? C16 C11 C12 121.1(9) . . ? C13 C12 C11 118.7(8) . . ? C13 C12 C2 119.7(9) . . ? C11 C12 C2 121.6(8) . . ? C14 C13 C12 120.4(10) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.4(9) . . ? C13 C14 S1 121.2(8) . . ? C15 C14 S1 118.3(8) . . ? O12 S1 O13 112.3(7) . . ? O12 S1 O14 113.8(8) . . ? O13 S1 O14 109.1(6) . . ? O12 S1 C14 106.7(6) . . ? O13 S1 C14 108.3(5) . . ? O14 S1 C14 106.3(6) . . ? C16 C15 C14 121.0(9) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 118.4(9) . . ? C15 C16 C1 120.9(8) . . ? C11 C16 C1 120.7(8) . . ? C16 C1 C42 115.7(7) . . ? C16 C1 H1A 108.4 . . ? C42 C1 H1A 108.4 . . ? C16 C1 H1B 108.4 . . ? C42 C1 H1B 108.4 . . ? H1A C1 H1B 107.4 . . ? O21 C21 C26 120.4(8) . . ? O21 C21 C22 117.4(8) . . ? C26 C21 C22 122.2(8) . . ? C23 C22 C21 117.6(8) . . ? C23 C22 C3 120.5(8) . . ? C21 C22 C3 121.7(8) . . ? C24 C23 C22 120.8(8) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.3(9) . . ? C23 C24 S2 118.2(7) . . ? C25 C24 S2 121.5(8) . . ? O22 S2 O24 113.2(5) . . ? O22 S2 O23 113.4(5) . . ? O24 S2 O23 110.8(5) . . ? O22 S2 C24 107.2(4) . . ? O24 S2 C24 106.7(5) . . ? O23 S2 C24 104.9(5) . . ? C26 C25 C24 120.8(9) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C21 118.2(8) . . ? C25 C26 C2 120.5(8) . . ? C21 C26 C2 121.4(8) . . ? C26 C2 C12 114.5(8) . . ? C26 C2 H2A 108.6 . . ? C12 C2 H2A 108.6 . . ? C26 C2 H2B 108.6 . . ? C12 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? O31 C31 C36 118.3(9) . . ? O31 C31 C32 119.3(8) . . ? C36 C31 C32 122.4(9) . . ? C33 C32 C31 117.5(9) . . ? C33 C32 C4 118.9(9) . . ? C31 C32 C4 123.5(8) . . ? C32 C33 C34 121.2(9) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C33 C34 C35 120.3(9) . . ? C33 C34 S3 118.0(8) . . ? C35 C34 S3 121.7(7) . . ? O34 S3 O32 113.2(5) . . ? O34 S3 O33 111.7(5) . . ? O32 S3 O33 111.9(6) . . ? O34 S3 C34 106.4(5) . . ? O32 S3 C34 107.3(4) . . ? O33 S3 C34 105.8(5) . . ? S3 O34 Y2 148.1(5) . . ? C34 C35 C36 121.0(9) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 117.6(9) . . ? C35 C36 C3 120.5(8) . . ? C31 C36 C3 121.9(9) . . ? C22 C3 C36 112.7(7) . . ? C22 C3 H3A 109.1 . . ? C36 C3 H3A 109.1 . . ? C22 C3 H3B 109.1 . . ? C36 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? O41 C41 C46 117.1(8) . . ? O41 C41 C42 121.2(8) . . ? C46 C41 C42 121.7(8) . . ? C43 C42 C41 117.1(8) . . ? C43 C42 C1 122.0(8) . . ? C41 C42 C1 120.9(8) . . ? C42 C43 C44 122.1(8) . . ? C42 C43 H43 119 . . ? C44 C43 H43 119 . . ? C45 C44 C43 119.8(9) . . ? C45 C44 S4 120.0(7) . . ? C43 C44 S4 120.1(7) . . ? O42 S4 O44 112.8(5) . . ? O42 S4 O43 111.5(6) . . ? O44 S4 O43 112.6(6) . . ? O42 S4 C44 106.5(5) . . ? O44 S4 C44 107.0(4) . . ? O43 S4 C44 105.9(4) . . ? C44 C45 C46 120.0(9) . . ? C44 C45 H45 120 . . ? C46 C45 H45 120 . . ? C41 C46 C45 119.3(9) . . ? C41 C46 C4 119.1(8) . . ? C45 C46 C4 121.6(8) . . ? C46 C4 C32 112.1(7) . . ? C46 C4 H4A 109.2 . . ? C32 C4 H4A 109.2 . . ? C46 C4 H4B 109.2 . . ? C32 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? O51 C51 C52 119.5(8) . . ? O51 C51 C56 118.0(9) . . ? C52 C51 C56 122.5(9) . . ? C53 C52 C51 118.5(9) . . ? C53 C52 C6 118.5(9) . . ? C51 C52 C6 123.0(10) . . ? C52 C53 C54 120.6(9) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C55 120.9(9) . . ? C53 C54 S5 119.5(8) . . ? C55 C54 S5 119.6(7) . . ? O52 S5 O53 113.1(7) . . ? O52 S5 O54 109.6(7) . . ? O53 S5 O54 113.8(6) . . ? O52 S5 C54 106.6(5) . . ? O53 S5 C54 106.4(5) . . ? O54 S5 C54 106.8(5) . . ? S5 O54 Y3 134.9(6) . . ? C54 C55 C56 119.6(9) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C51 118.0(9) . . ? C55 C56 C5 119.5(9) . . ? C51 C56 C5 122.5(9) . . ? C82 C5 C56 112.5(8) . . ? C82 C5 H5A 109.1 . . ? C56 C5 H5A 109.1 . . ? C82 C5 H5B 109.1 . . ? C56 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? O61 C61 C66 119.6(9) . . ? O61 C61 C62 119.1(8) . . ? C66 C61 C62 121.2(9) . . ? C63 C62 C61 117.1(9) . . ? C63 C62 C7 122.0(8) . . ? C61 C62 C7 120.8(8) . . ? C64 C63 C62 121.6(9) . . ? C64 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C65 C64 C63 120.0(9) . . ? C65 C64 S6 119.6(8) . . ? C63 C64 S6 120.4(8) . . ? O64 S6 O62 113.2(5) . . ? O64 S6 O63 112.8(5) . . ? O62 S6 O63 111.2(5) . . ? O64 S6 C64 107.8(5) . . ? O62 S6 C64 107.1(5) . . ? O63 S6 C64 104.2(4) . . ? S6 O63 Y1 145.5(5) . . ? C64 C65 C66 120.4(9) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C61 C66 C65 119.5(9) . . ? C61 C66 C6 118.6(9) . . ? C65 C66 C6 121.9(9) . . ? C66 C6 C52 111.4(8) . . ? C66 C6 H6A 109.4 . . ? C52 C6 H6A 109.4 . . ? C66 C6 H6B 109.4 . . ? C52 C6 H6B 109.4 . . ? H6A C6 H6B 108 . . ? O71 C71 C76 119.1(8) . . ? O71 C71 C72 120.3(8) . . ? C76 C71 C72 120.6(8) . . ? C73 C72 C71 119.8(9) . . ? C73 C72 C8 119.2(9) . . ? C71 C72 C8 120.9(9) . . ? C74 C73 C72 118.9(9) . . ? C74 C73 H73 120.6 . . ? C72 C73 H73 120.6 . . ? C75 C74 C73 121.1(9) . . ? C75 C74 S7 119.2(8) . . ? C73 C74 S7 119.7(8) . . ? O74 S7 O73 111.1(8) . . ? O74 S7 O72 112.3(7) . . ? O73 S7 O72 110.0(7) . . ? O74 S7 C74 107.1(5) . . ? O73 S7 C74 107.4(5) . . ? O72 S7 C74 108.7(5) . . ? C76 C75 C74 119.8(9) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C71 C76 C75 119.8(9) . . ? C71 C76 C7 120.5(8) . . ? C75 C76 C7 119.5(8) . . ? C76 C7 C62 115.9(8) . . ? C76 C7 H7A 108.3 . . ? C62 C7 H7A 108.3 . . ? C76 C7 H7B 108.3 . . ? C62 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? O81 C81 C86 121.8(9) . . ? O81 C81 C82 118.8(9) . . ? C86 C81 C82 119.3(9) . . ? C83 C82 C81 118.4(9) . . ? C83 C82 C5 121.5(9) . . ? C81 C82 C5 120.0(9) . . ? C82 C83 C84 122.6(9) . . ? C82 C83 H83 118.7 . . ? C84 C83 H83 118.7 . . ? C83 C84 C85 119.0(10) . . ? C83 C84 S8 121.5(8) . . ? C85 C84 S8 119.5(8) . . ? O84 S8 O82 113.9(4) . . ? O84 S8 O83 110.5(4) . . ? O82 S8 O83 112.4(5) . . ? O84 S8 C84 107.1(5) . . ? O82 S8 C84 106.6(5) . . ? O83 S8 C84 105.8(4) . . ? C86 C85 C84 120.5(9) . . ? C86 C85 H85 119.8 . . ? C84 C85 H85 119.8 . . ? C85 C86 C81 120.1(9) . . ? C85 C86 C8 119.2(9) . . ? C81 C86 C8 120.7(9) . . ? C72 C8 C86 112.7(7) . . ? C72 C8 H8A 109.1 . . ? C86 C8 H8A 109.1 . . ? C72 C8 H8B 109.1 . . ? C86 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C92 N91 C95 107.5(9) . . ? C92 N91 C96 124.4(10) . . ? C95 N91 C96 128.0(10) . . ? N93 C92 N91 109.2(9) . . ? N93 C92 H92 125.4 . . ? N91 C92 H92 125.4 . . ? C92 N93 C94 107.9(9) . . ? C92 N93 C97 125.2(8) . . ? C94 N93 C97 126.7(9) . . ? C95 C94 N93 106.9(9) . . ? C95 C94 H94 126.6 . . ? N93 C94 H94 126.6 . . ? C94 C95 N91 108.4(9) . . ? C94 C95 H95 125.8 . . ? N91 C95 H95 125.8 . . ? N91 C96 H96A 109.5 . . ? N91 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? N91 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? N93 C97 C98 112.7(9) . . ? N93 C97 H97A 109.1 . . ? C98 C97 H97A 109.1 . . ? N93 C97 H97B 109.1 . . ? C98 C97 H97B 109.1 . . ? H97A C97 H97B 107.8 . . ? O92 C98 O91 125.5(11) . . ? O92 C98 C97 116.2(11) . . ? O91 C98 C97 118.3(9) . . ? C98 O91 Y2 161.6(7) . . ? C98 O92 Y1 160.8(8) . . ? C102 N101 C105 107.4(10) . . ? C102 N101 C106 126.2(11) . . ? C105 N101 C106 126.1(11) . . ? N103 C102 N101 107.5(10) . . ? N103 C102 H102 126.2 . . ? N101 C102 H102 126.2 . . ? C102 N103 C104 111.4(11) . . ? C102 N103 C107 120.9(12) . . ? C104 N103 C107 126.7(13) . . ? C105 C104 N103 105.5(11) . . ? C105 C104 H104 127.2 . . ? N103 C104 H104 127.2 . . ? C104 C105 N101 108.0(10) . . ? C104 C105 H105 126 . . ? N101 C105 H105 126 . . ? N101 C106 H10A 109.5 . . ? N101 C106 H10B 109.5 . . ? H10A C106 H10B 109.5 . . ? N101 C106 H10C 109.5 . . ? H10A C106 H10C 109.5 . . ? H10B C106 H10C 109.5 . . ? N103 C107 C108 106.4(14) . . ? N103 C107 H10D 110.5 . . ? C108 C107 H10D 110.5 . . ? N103 C107 H10E 110.5 . . ? C108 C107 H10E 110.5 . . ? H10D C107 H10E 108.6 . . ? O101 C108 C107 115.6(15) . . ? O101 C108 O102 123.0(16) . . ? C107 C108 O102 120.3(15) . . ? C108 O101 Y3 86.4(10) . . ? C108 O102 Y3 127.6(12) . 2_766 ? C108 O102 Y3 85.5(10) . . ? C141 P1 C111 110.7(4) . . ? C141 P1 C121 109.4(4) . . ? C111 P1 C121 109.2(4) . . ? C141 P1 C131 106.6(4) . . ? C111 P1 C131 110.7(4) . . ? C121 P1 C131 110.2(4) . . ? C112 C111 C116 119.1(7) . . ? C112 C111 P1 120.6(6) . . ? C116 C111 P1 120.1(6) . . ? C111 C112 C113 121.0(8) . . ? C111 C112 H112 119.5 . . ? C113 C112 H112 119.5 . . ? C112 C113 C114 119.4(7) . . ? C112 C113 H113 120.3 . . ? C114 C113 H113 120.3 . . ? O117 C114 C115 124.5(7) . . ? O117 C114 C113 115.6(7) . . ? C115 C114 C113 119.9(7) . . ? C116 C115 C114 120.0(8) . . ? C116 C115 H115 120 . . ? C114 C115 H115 120 . . ? C115 C116 C111 120.5(8) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C114 O117 C117 116.8(6) . . ? O117 C117 H11A 109.5 . . ? O117 C117 H11B 109.5 . . ? H11A C117 H11B 109.5 . . ? O117 C117 H11C 109.5 . . ? H11A C117 H11C 109.5 . . ? H11B C117 H11C 109.5 . . ? C122 C121 C126 119.5(8) . . ? C122 C121 P1 121.3(6) . . ? C126 C121 P1 119.1(7) . . ? C123 C122 C121 120.5(8) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C122 C123 C124 119.7(9) . . ? C122 C123 H123 120.2 . . ? C124 C123 H123 120.2 . . ? C123 C124 C125 119.8(8) . . ? C123 C124 H124 120.1 . . ? C125 C124 H124 120.1 . . ? C126 C125 C124 120.3(8) . . ? C126 C125 H125 119.9 . . ? C124 C125 H125 119.9 . . ? C125 C126 C121 120.2(8) . . ? C125 C126 H126 119.9 . . ? C121 C126 H126 119.9 . . ? C136 C131 C132 119.1(8) . . ? C136 C131 P1 120.0(7) . . ? C132 C131 P1 120.9(7) . . ? C133 C132 C131 120.2(9) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C132 C133 C134 120.8(9) . . ? C132 C133 H133 119.6 . . ? C134 C133 H133 119.6 . . ? C133 C134 C135 118.7(9) . . ? C133 C134 H134 120.6 . . ? C135 C134 H134 120.6 . . ? C136 C135 C134 121.8(9) . . ? C136 C135 H135 119.1 . . ? C134 C135 H135 119.1 . . ? C135 C136 C131 119.3(9) . . ? C135 C136 H136 120.4 . . ? C131 C136 H136 120.4 . . ? C146 C141 C142 119.5(9) . . ? C146 C141 P1 121.7(8) . . ? C142 C141 P1 118.8(7) . . ? C143 C142 C141 120.0(10) . . ? C143 C142 H142 120 . . ? C141 C142 H142 120 . . ? C144 C143 C142 121.1(11) . . ? C144 C143 H143 119.5 . . ? C142 C143 H143 119.5 . . ? C143 C144 C145 120.1(10) . . ? C143 C144 H144 119.9 . . ? C145 C144 H144 119.9 . . ? C146 C145 C144 119.2(10) . . ? C146 C145 H145 120.4 . . ? C144 C145 H145 120.4 . . ? C145 C146 C141 120.1(10) . . ? C145 C146 H146 120 . . ? C141 C146 H146 120 . . ? C241 P2 C221 111.9(4) . . ? C241 P2 C211 108.0(4) . . ? C221 P2 C211 110.6(4) . . ? C241 P2 C231 109.6(4) . . ? C221 P2 C231 106.0(4) . . ? C211 P2 C231 110.7(4) . . ? C212 C211 C216 118.7(7) . . ? C212 C211 P2 121.0(6) . . ? C216 C211 P2 120.2(6) . . ? C213 C212 C211 120.2(7) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C212 C213 C214 120.7(7) . . ? C212 C213 H213 119.6 . . ? C214 C213 H213 119.6 . . ? O217 C214 C213 115.7(7) . . ? O217 C214 C215 124.8(8) . . ? C213 C214 C215 119.5(7) . . ? C216 C215 C214 119.5(8) . . ? C216 C215 H215 120.2 . . ? C214 C215 H215 120.2 . . ? C215 C216 C211 121.2(8) . . ? C215 C216 H216 119.4 . . ? C211 C216 H216 119.4 . . ? C214 O217 C217 117.0(6) . . ? O217 C217 H21A 109.5 . . ? O217 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? O217 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C222 C221 C226 120.6(8) . . ? C222 C221 P2 122.5(7) . . ? C226 C221 P2 116.9(7) . . ? C221 C222 C223 119.3(9) . . ? C221 C222 H222 120.3 . . ? C223 C222 H222 120.3 . . ? C224 C223 C222 120.5(9) . . ? C224 C223 H223 119.7 . . ? C222 C223 H223 119.7 . . ? C225 C224 C223 119.4(9) . . ? C225 C224 H224 120.3 . . ? C223 C224 H224 120.3 . . ? C224 C225 C226 120.4(9) . . ? C224 C225 H225 119.8 . . ? C226 C225 H225 119.8 . . ? C225 C226 C221 119.9(9) . . ? C225 C226 H226 120.1 . . ? C221 C226 H226 120.1 . . ? C236 C231 C232 119.9(8) . . ? C236 C231 P2 121.7(6) . . ? C232 C231 P2 118.4(7) . . ? C233 C232 C231 119.2(9) . . ? C233 C232 H232 120.4 . . ? C231 C232 H232 120.4 . . ? C234 C233 C232 121.0(9) . . ? C234 C233 H233 119.5 . . ? C232 C233 H233 119.5 . . ? C233 C234 C235 120.2(8) . . ? C233 C234 H234 119.9 . . ? C235 C234 H234 119.9 . . ? C234 C235 C236 120.1(9) . . ? C234 C235 H235 119.9 . . ? C236 C235 H235 119.9 . . ? C231 C236 C235 119.5(8) . . ? C231 C236 H236 120.3 . . ? C235 C236 H236 120.3 . . ? C246 C241 C242 120.2(8) . . ? C246 C241 P2 118.5(6) . . ? C242 C241 P2 121.3(7) . . ? C243 C242 C241 119.6(8) . . ? C243 C242 H242 120.2 . . ? C241 C242 H242 120.2 . . ? C244 C243 C242 120.1(8) . . ? C244 C243 H243 120 . . ? C242 C243 H243 120 . . ? C243 C244 C245 120.6(8) . . ? C243 C244 H244 119.7 . . ? C245 C244 H244 119.7 . . ? C246 C245 C244 119.1(9) . . ? C246 C245 H245 120.4 . . ? C244 C245 H245 120.4 . . ? C241 C246 C245 120.3(8) . . ? C241 C246 H246 119.8 . . ? C245 C246 H246 119.8 . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 104 23 ' ' #===END