# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '1 Dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Dy F18 O10 P' _chemical_formula_weight 1130.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.0167(18) _cell_length_b 11.8155(8) _cell_length_c 30.008(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.2930(10) _cell_angle_gamma 90.00 _cell_volume 8632.3(10) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 14434 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.30 _exptl_crystal_description blocky _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4424 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.752 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23674 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7598 _reflns_number_gt 6682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0951P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7598 _refine_ls_number_parameters 665 _refine_ls_number_restraints 630 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.597659(8) 0.435149(14) 0.320209(6) 0.04785(11) Uani 1 1 d . . . P1 P 0.56927(8) 0.39030(11) 0.43457(4) 0.0814(4) Uani 1 1 d . . . F1 F 0.7252(6) 0.6927(9) 0.4136(4) 0.144(4) Uani 0.536(10) 1 d PDU A 1 F2 F 0.6729(5) 0.8346(11) 0.3974(5) 0.157(4) Uani 0.536(10) 1 d PDU A 1 F3 F 0.7325(5) 0.8059(13) 0.3618(4) 0.146(4) Uani 0.536(10) 1 d PDU A 1 F1A F 0.6868(7) 0.7467(15) 0.4201(3) 0.149(4) Uani 0.464(10) 1 d PDU A 2 F2A F 0.7440(4) 0.6996(12) 0.3819(6) 0.153(4) Uani 0.464(10) 1 d PDU A 2 F3A F 0.7052(7) 0.8550(7) 0.3679(5) 0.138(5) Uani 0.464(10) 1 d PDU A 2 F4 F 0.5860(8) 0.8548(5) 0.2250(7) 0.106(4) Uani 0.58(3) 1 d PDU A 1 F5 F 0.6155(7) 0.7137(16) 0.1950(5) 0.124(4) Uani 0.58(3) 1 d PDU A 1 F6 F 0.5321(5) 0.7195(14) 0.1961(6) 0.122(4) Uani 0.58(3) 1 d PDU A 1 F4A F 0.6029(11) 0.8439(12) 0.2179(10) 0.118(6) Uani 0.42(3) 1 d PDU A 2 F5A F 0.5908(12) 0.6776(13) 0.1882(5) 0.121(4) Uani 0.42(3) 1 d PDU A 2 F6A F 0.5274(4) 0.756(2) 0.2135(8) 0.116(5) Uani 0.42(3) 1 d PDU A 2 F7 F 0.7682(6) 0.5767(9) 0.2758(6) 0.156(4) Uani 0.547(9) 1 d PDU B 1 F8 F 0.7943(5) 0.4244(12) 0.2532(6) 0.163(4) Uani 0.547(9) 1 d PDU B 1 F9 F 0.7181(4) 0.4974(13) 0.2172(3) 0.146(4) Uani 0.547(9) 1 d PDU B 1 F7A F 0.7369(7) 0.5783(10) 0.2444(7) 0.143(4) Uani 0.453(9) 1 d PDU B 2 F8A F 0.7599(7) 0.4014(11) 0.2281(5) 0.139(4) Uani 0.453(9) 1 d PDU B 2 F9A F 0.8019(4) 0.4889(15) 0.2815(5) 0.151(4) Uani 0.453(9) 1 d PDU B 2 F10 F 0.7851(2) 0.1490(5) 0.3687(2) 0.173(2) Uani 1 1 d . B . F11 F 0.7087(3) 0.0776(4) 0.3446(3) 0.161(2) Uani 1 1 d . B . F12 F 0.7255(3) 0.1608(6) 0.4082(2) 0.180(3) Uani 1 1 d . B . F13 F 0.65547(17) 0.2712(4) 0.19361(14) 0.1225(14) Uani 1 1 d . . . F14 F 0.60624(19) 0.1261(3) 0.17757(13) 0.1175(13) Uani 1 1 d . . . F15 F 0.57081(18) 0.2878(4) 0.15980(11) 0.1177(14) Uani 1 1 d . . . F16 F 0.5588(7) -0.0417(5) 0.3043(4) 0.115(3) Uani 0.592(18) 1 d PDU C 1 F17 F 0.5877(4) 0.0457(8) 0.3666(3) 0.099(3) Uani 0.592(18) 1 d PDU C 1 F18 F 0.5026(4) 0.0491(15) 0.3342(6) 0.119(4) Uani 0.592(18) 1 d PDU C 1 F16A F 0.5961(5) 0.0036(14) 0.3504(8) 0.127(4) Uani 0.408(18) 1 d PDU C 2 F17A F 0.5150(7) 0.0693(18) 0.3502(7) 0.099(4) Uani 0.408(18) 1 d PDU C 2 F18A F 0.5238(8) -0.0218(12) 0.2954(4) 0.110(4) Uani 0.408(18) 1 d PDU C 2 O1W O 0.50168(13) 0.4756(3) 0.30590(11) 0.0640(7) Uani 1 1 d . . . H1WB H 0.4851 0.4414 0.2817 0.096 Uiso 1 1 d R . . H1WC H 0.4892 0.4531 0.3284 0.096 Uiso 1 1 d R . . O1 O 0.58185(18) 0.4260(3) 0.39118(12) 0.0730(10) Uani 1 1 d . . . O2 O 0.6164(4) 0.4229(4) 0.47633(16) 0.149(3) Uani 1 1 d D . . O3 O 0.5156(3) 0.4429(3) 0.4425(2) 0.122(2) Uani 1 1 d . . . O4 O 0.63935(16) 0.5965(3) 0.35803(12) 0.0736(9) Uani 1 1 d . . . O5 O 0.57469(13) 0.5911(2) 0.26864(11) 0.0573(7) Uani 1 1 d . . . O6 O 0.67623(14) 0.4747(3) 0.29195(12) 0.0712(8) Uani 1 1 d . . . O7 O 0.66587(15) 0.3057(3) 0.35127(12) 0.0734(9) Uani 1 1 d . . . O8 O 0.58565(14) 0.3461(3) 0.24849(10) 0.0656(8) Uani 1 1 d . . . O9 O 0.55512(13) 0.2494(2) 0.32187(10) 0.0627(7) Uani 1 1 d . . . C1 C 0.5595(4) 0.2414(4) 0.43714(19) 0.0977(19) Uani 1 1 d U . . H1A H 0.5279 0.2210 0.4131 0.117 Uiso 1 1 calc R . . H1B H 0.5912 0.2043 0.4303 0.117 Uiso 1 1 calc R . . C2 C 0.5509(4) 0.1934(4) 0.48187(19) 0.1101(17) Uani 1 1 d U . . C3 C 0.5989(3) 0.1514(4) 0.51566(15) 0.134(2) Uani 1 1 d GU . . C4 C 0.6518(4) 0.1555(5) 0.50856(19) 0.166(3) Uani 1 1 d GU . . H4A H 0.6580 0.1868 0.4818 0.199 Uiso 1 1 calc R . . C5 C 0.6956(3) 0.1127(6) 0.5415(3) 0.193(4) Uani 1 1 d GU . . H5A H 0.7310 0.1154 0.5368 0.232 Uiso 1 1 calc R . . C6 C 0.6863(4) 0.0659(5) 0.5816(2) 0.191(4) Uani 1 1 d GU . . H6A H 0.7156 0.0373 0.6036 0.229 Uiso 1 1 calc R . . C7 C 0.6334(4) 0.0618(4) 0.58867(15) 0.179(4) Uani 1 1 d GU . . H7A H 0.6272 0.0305 0.6155 0.214 Uiso 1 1 calc R . . C8 C 0.5897(3) 0.1046(5) 0.55572(19) 0.152(3) Uani 1 1 d GU . . C9 C 0.5352(6) 0.0975(6) 0.5607(3) 0.150(3) Uani 1 1 d U . . H9A H 0.5297 0.0650 0.5875 0.180 Uiso 1 1 calc R . . C10 C 0.4889(3) 0.1348(4) 0.52902(16) 0.144(2) Uani 1 1 d GU . . C11 C 0.4365(3) 0.1223(5) 0.5367(2) 0.167(3) Uani 1 1 d GU . . H11A H 0.4318 0.0900 0.5638 0.200 Uiso 1 1 calc R . . C12 C 0.3910(3) 0.1581(5) 0.5038(3) 0.173(3) Uani 1 1 d GU . . H12A H 0.3559 0.1497 0.5089 0.208 Uiso 1 1 calc R . . C13 C 0.3979(3) 0.2064(5) 0.4632(2) 0.162(3) Uani 1 1 d GU . . H13A H 0.3675 0.2303 0.4412 0.194 Uiso 1 1 calc R . . C14 C 0.4503(3) 0.2189(4) 0.45557(15) 0.135(2) Uani 1 1 d GU . . H14A H 0.4550 0.2511 0.4285 0.162 Uiso 1 1 calc R . . C15 C 0.4958(2) 0.1831(4) 0.48848(18) 0.1238(19) Uani 1 1 d GU . . C16 C 0.6502(5) 0.5167(11) 0.4790(3) 0.185(5) Uani 1 1 d DU . . H16A H 0.6268 0.5820 0.4759 0.222 Uiso 1 1 d R . . H16B H 0.6678 0.5172 0.4538 0.222 Uiso 1 1 d R . . C17 C 0.6922(5) 0.5308(11) 0.5197(4) 0.187(5) Uani 1 1 d DU . . H17C H 0.7118 0.5998 0.5178 0.280 Uiso 1 1 calc R . . H17D H 0.7172 0.4680 0.5230 0.280 Uiso 1 1 calc R . . H17E H 0.6759 0.5339 0.5457 0.280 Uiso 1 1 calc R . . C18 C 0.4990(5) 0.5599(6) 0.4325(4) 0.137(3) Uani 1 1 d U . . H18D H 0.5123 0.6059 0.4596 0.164 Uiso 1 1 calc R . . H18E H 0.5152 0.5883 0.4083 0.164 Uiso 1 1 calc R . . C19 C 0.4391(6) 0.5685(8) 0.4184(5) 0.159(4) Uani 1 1 d U . . H19A H 0.4289 0.6462 0.4121 0.238 Uiso 1 1 calc R . . H19B H 0.4231 0.5410 0.4425 0.238 Uiso 1 1 calc R . . H19C H 0.4261 0.5241 0.3913 0.238 Uiso 1 1 calc R . . C20 C 0.6969(3) 0.7519(5) 0.3796(2) 0.1037(17) Uani 1 1 d DU . . C21 C 0.6548(2) 0.6873(4) 0.34416(18) 0.0714(12) Uani 1 1 d U A . C22 C 0.6374(2) 0.7356(4) 0.30138(17) 0.0708(12) Uani 1 1 d U . . H22A H 0.6522 0.8047 0.2954 0.085 Uiso 1 1 calc R A . C23 C 0.59815(19) 0.6833(4) 0.26682(17) 0.0625(10) Uani 1 1 d U A . C24 C 0.5813(2) 0.7439(4) 0.2207(2) 0.0855(14) Uani 1 1 d DU . . C25 C 0.7507(2) 0.4767(6) 0.2581(3) 0.1078(17) Uani 1 1 d DU . . C26 C 0.7178(2) 0.4217(4) 0.2896(2) 0.0732(13) Uani 1 1 d U B . C27 C 0.7371(2) 0.3229(5) 0.3121(2) 0.0861(14) Uani 1 1 d U . . H27A H 0.7690 0.2900 0.3071 0.103 Uiso 1 1 calc R B . C28 C 0.7099(2) 0.2722(5) 0.3418(2) 0.0806(14) Uani 1 1 d U B . C29 C 0.7330(3) 0.1650(7) 0.3661(3) 0.109(2) Uani 1 1 d U . . C30 C 0.6061(2) 0.2307(5) 0.19176(18) 0.0755(13) Uani 1 1 d U . . C31 C 0.59098(19) 0.2440(4) 0.23766(15) 0.0602(10) Uani 1 1 d U . . C32 C 0.5829(2) 0.1503(4) 0.26260(17) 0.0699(12) Uani 1 1 d U . . H32A H 0.5905 0.0788 0.2527 0.084 Uiso 1 1 calc R . . C33 C 0.5638(2) 0.1606(4) 0.30216(17) 0.0662(11) Uani 1 1 d U C . C34 C 0.5519(2) 0.0512(4) 0.32588(18) 0.0820(14) Uani 1 1 d DU . . 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 Dy1 0.06265(17) 0.03796(16) 0.04744(16) 0.00181(6) 0.02191(10) 0.00223(7) P1 0.1497(14) 0.0532(7) 0.0528(7) 0.0016(5) 0.0472(8) 0.0063(8) F1 0.151(8) 0.117(6) 0.126(7) 0.012(6) -0.049(6) -0.042(6) F2 0.192(8) 0.136(8) 0.130(7) -0.070(6) 0.011(6) -0.008(6) F3 0.141(8) 0.142(9) 0.144(7) -0.010(7) 0.013(6) -0.075(7) F1A 0.200(10) 0.146(9) 0.093(6) -0.039(6) 0.020(6) -0.064(8) F2A 0.121(7) 0.139(8) 0.171(9) -0.023(8) -0.025(7) -0.016(6) F3A 0.184(10) 0.060(5) 0.149(8) -0.007(5) -0.004(8) -0.046(6) F4 0.148(9) 0.051(3) 0.120(7) 0.027(4) 0.037(6) -0.001(4) F5 0.161(9) 0.129(8) 0.094(5) 0.018(5) 0.057(6) 0.011(7) F6 0.134(6) 0.103(7) 0.104(7) 0.046(5) -0.021(5) -0.036(5) F4A 0.145(12) 0.095(7) 0.112(9) 0.047(7) 0.022(9) -0.049(8) F5A 0.175(10) 0.107(7) 0.081(6) 0.022(5) 0.028(7) -0.017(7) F6A 0.094(5) 0.112(10) 0.120(11) 0.037(8) -0.018(6) 0.007(5) F7 0.133(8) 0.131(7) 0.218(10) 0.011(7) 0.073(7) -0.040(6) F8 0.116(7) 0.191(9) 0.213(11) 0.015(8) 0.103(7) 0.031(7) F9 0.137(7) 0.183(9) 0.135(6) 0.051(6) 0.068(5) -0.025(7) F7A 0.140(9) 0.128(7) 0.189(10) 0.075(7) 0.095(8) 0.029(7) F8A 0.140(8) 0.168(8) 0.139(8) -0.025(6) 0.095(6) -0.028(7) F9A 0.098(6) 0.160(10) 0.206(10) 0.015(8) 0.059(6) -0.036(6) F10 0.117(4) 0.151(4) 0.246(6) 0.073(4) 0.034(4) 0.072(3) F11 0.185(6) 0.070(3) 0.229(7) 0.030(3) 0.051(5) 0.024(3) F12 0.219(6) 0.184(6) 0.145(5) 0.087(4) 0.056(4) 0.114(5) F13 0.122(3) 0.152(4) 0.116(3) -0.029(3) 0.074(2) -0.020(3) F14 0.176(4) 0.094(3) 0.096(2) -0.038(2) 0.062(2) 0.009(3) F15 0.155(3) 0.144(3) 0.0592(18) 0.0041(19) 0.035(2) 0.047(3) F16 0.192(10) 0.044(3) 0.114(5) 0.002(3) 0.048(6) 0.006(5) F17 0.151(6) 0.052(4) 0.090(4) 0.017(3) 0.018(4) 0.010(4) F18 0.133(6) 0.086(7) 0.145(10) 0.027(6) 0.046(6) -0.025(5) F16A 0.147(7) 0.064(7) 0.159(10) 0.032(7) 0.010(7) 0.012(6) F17A 0.141(8) 0.064(6) 0.108(9) 0.004(6) 0.063(7) -0.029(6) F18A 0.161(10) 0.054(6) 0.113(7) 0.004(5) 0.028(6) -0.022(6) O1W 0.0684(19) 0.0659(18) 0.0638(18) -0.0001(15) 0.0280(14) -0.0022(15) O1 0.111(3) 0.064(2) 0.0519(18) 0.0026(13) 0.0353(18) -0.0015(16) O2 0.303(9) 0.073(3) 0.057(3) 0.0009(19) 0.013(4) -0.028(4) O3 0.198(6) 0.064(3) 0.146(5) 0.017(2) 0.123(5) 0.020(2) O4 0.106(3) 0.0523(17) 0.0646(19) -0.0028(15) 0.0235(18) -0.0161(18) O5 0.0622(18) 0.0402(14) 0.0715(19) 0.0069(14) 0.0197(14) -0.0027(13) O6 0.069(2) 0.0630(19) 0.089(2) 0.0127(18) 0.0330(17) 0.0085(16) O7 0.083(2) 0.064(2) 0.076(2) 0.0119(16) 0.0251(17) 0.0165(17) O8 0.098(2) 0.0479(17) 0.0572(17) -0.0001(13) 0.0312(15) 0.0021(15) O9 0.084(2) 0.0454(16) 0.0631(17) -0.0038(13) 0.0262(15) -0.0018(14) C1 0.192(6) 0.050(3) 0.066(3) -0.001(2) 0.062(3) 0.008(3) C2 0.239(5) 0.042(2) 0.062(3) 0.001(2) 0.059(3) 0.001(3) C3 0.274(6) 0.050(3) 0.080(3) 0.005(3) 0.042(4) 0.012(4) C4 0.275(8) 0.094(5) 0.120(5) 0.000(4) 0.028(5) 0.019(6) C5 0.290(9) 0.127(6) 0.140(6) 0.000(5) 0.002(6) 0.015(7) C6 0.313(9) 0.111(6) 0.119(6) -0.005(4) -0.012(7) 0.013(6) C7 0.329(9) 0.089(5) 0.097(5) 0.022(4) 0.007(6) 0.000(6) C8 0.307(7) 0.061(3) 0.080(4) 0.011(3) 0.029(5) 0.007(5) C9 0.323(8) 0.059(3) 0.085(4) 0.002(3) 0.080(5) -0.018(5) C10 0.294(7) 0.060(3) 0.107(4) -0.001(3) 0.108(4) -0.024(4) C11 0.308(8) 0.079(4) 0.156(6) -0.004(4) 0.140(6) -0.030(6) C12 0.276(8) 0.092(5) 0.193(7) -0.019(5) 0.140(6) -0.019(6) C13 0.253(7) 0.085(4) 0.178(6) -0.020(4) 0.112(6) -0.016(5) C14 0.242(7) 0.065(3) 0.124(5) -0.006(3) 0.097(5) -0.018(4) C15 0.261(6) 0.048(3) 0.089(3) -0.006(2) 0.097(4) -0.008(4) C16 0.202(11) 0.207(11) 0.127(7) 0.014(8) -0.001(7) -0.043(10) C17 0.184(11) 0.183(10) 0.162(9) 0.010(8) -0.026(7) -0.006(9) C18 0.188(8) 0.079(5) 0.169(9) 0.005(4) 0.095(8) 0.030(5) C19 0.190(9) 0.130(8) 0.171(10) 0.013(6) 0.070(8) 0.033(6) C20 0.125(4) 0.078(3) 0.101(4) -0.008(3) 0.011(3) -0.032(3) C21 0.091(3) 0.051(2) 0.076(3) -0.006(2) 0.027(2) -0.009(2) C22 0.084(3) 0.052(2) 0.079(3) 0.009(2) 0.024(2) -0.010(2) C23 0.069(2) 0.048(2) 0.076(3) 0.008(2) 0.029(2) 0.005(2) C24 0.101(3) 0.066(3) 0.090(3) 0.021(3) 0.023(3) -0.014(3) C25 0.090(4) 0.110(4) 0.144(5) 0.008(4) 0.069(3) -0.001(3) C26 0.064(3) 0.074(3) 0.089(3) -0.005(2) 0.032(3) 0.001(2) C27 0.073(3) 0.084(3) 0.106(4) 0.004(3) 0.031(3) 0.021(3) C28 0.079(3) 0.068(3) 0.092(3) 0.005(3) 0.013(3) 0.022(2) C29 0.111(5) 0.081(4) 0.134(6) 0.025(4) 0.024(4) 0.035(4) C30 0.092(4) 0.072(3) 0.068(3) -0.010(2) 0.030(3) 0.004(3) C31 0.070(3) 0.055(2) 0.056(2) -0.0075(19) 0.0170(19) 0.008(2) C32 0.097(3) 0.045(2) 0.071(3) -0.0079(19) 0.026(2) 0.011(2) C33 0.088(3) 0.047(2) 0.066(3) 0.001(2) 0.022(2) 0.003(2) C34 0.119(4) 0.048(2) 0.082(3) 0.003(2) 0.031(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.256(3) . ? Dy1 O7 2.322(3) . ? Dy1 O4 2.338(3) . ? Dy1 O8 2.352(3) . ? Dy1 O6 2.360(3) . ? Dy1 O5 2.390(3) . ? Dy1 O1W 2.388(3) . ? Dy1 O9 2.445(3) . ? P1 O1 1.470(4) . ? P1 O3 1.547(6) . ? P1 O2 1.559(7) . ? P1 C1 1.781(6) . ? F1 C20 1.304(7) . ? F2 C20 1.323(7) . ? F3 C20 1.305(7) . ? F1A C20 1.300(8) . ? F2A C20 1.318(8) . ? F3A C20 1.298(7) . ? F4 C24 1.320(7) . ? F5 C24 1.325(7) . ? F6 C24 1.312(7) . ? F4A C24 1.310(8) . ? F5A C24 1.314(8) . ? F6A C24 1.322(8) . ? F7 C25 1.327(7) . ? F8 C25 1.291(7) . ? F9 C25 1.333(7) . ? F7A C25 1.291(8) . ? F8A C25 1.324(8) . ? F9A C25 1.318(8) . ? F10 C29 1.303(9) . ? F11 C29 1.293(10) . ? F12 C29 1.318(9) . ? F13 C30 1.313(7) . ? F14 C30 1.308(6) . ? F15 C30 1.329(7) . ? F16 C34 1.306(6) . ? F17 C34 1.341(7) . ? F18 C34 1.313(7) . ? F16A C34 1.307(8) . ? F17A C34 1.318(8) . ? F18A C34 1.333(7) . ? O1W H1WB 0.8501 . ? O1W H1WC 0.8501 . ? O2 C16 1.385(9) . ? O3 C18 1.454(8) . ? O4 C21 1.244(6) . ? O5 C23 1.244(5) . ? O6 C26 1.230(6) . ? O7 C28 1.264(7) . ? O8 C31 1.265(5) . ? O9 C33 1.248(5) . ? C1 C2 1.517(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C15 1.442(10) . ? C2 C3 1.468(9) . ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.3900 . ? C5 H5A 0.9300 . ? C6 C7 1.3900 . ? C6 H6A 0.9300 . ? C7 C8 1.3900 . ? C7 H7A 0.9300 . ? C8 C9 1.407(14) . ? C9 C10 1.390(13) . ? C9 H9A 0.9300 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11A 0.9300 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C16 C17 1.426(9) . ? C16 H16A 0.9599 . ? C16 H16B 0.9599 . ? C17 H17C 0.9600 . ? C17 H17D 0.9600 . ? C17 H17E 0.9600 . ? C18 C19 1.463(16) . ? C18 H18D 0.9700 . ? C18 H18E 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.518(8) . ? C21 C22 1.381(7) . ? C22 C23 1.398(7) . ? C22 H22A 0.9300 . ? C23 C24 1.530(7) . ? C25 C26 1.532(9) . ? C26 C27 1.379(8) . ? C27 C28 1.376(9) . ? C27 H27A 0.9300 . ? C28 C29 1.510(8) . ? C30 C31 1.518(7) . ? C31 C32 1.376(7) . ? C32 C33 1.384(7) . ? C32 H32A 0.9300 . ? C33 C34 1.537(7) . ? 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 O1 Dy1 O7 82.04(13) . . ? O1 Dy1 O4 74.72(12) . . ? O7 Dy1 O4 97.92(14) . . ? O1 Dy1 O8 145.99(11) . . ? O7 Dy1 O8 90.00(12) . . ? O4 Dy1 O8 139.28(11) . . ? O1 Dy1 O6 133.63(14) . . ? O7 Dy1 O6 71.25(12) . . ? O4 Dy1 O6 72.39(13) . . ? O8 Dy1 O6 72.63(12) . . ? O1 Dy1 O5 125.45(12) . . ? O7 Dy1 O5 144.41(11) . . ? O4 Dy1 O5 72.52(12) . . ? O8 Dy1 O5 77.96(10) . . ? O6 Dy1 O5 73.19(11) . . ? O1 Dy1 O1W 78.00(13) . . ? O7 Dy1 O1W 145.06(12) . . ? O4 Dy1 O1W 104.01(13) . . ? O8 Dy1 O1W 90.76(11) . . ? O6 Dy1 O1W 141.44(11) . . ? O5 Dy1 O1W 69.35(11) . . ? O1 Dy1 O9 76.47(11) . . ? O7 Dy1 O9 71.54(12) . . ? O4 Dy1 O9 150.45(11) . . ? O8 Dy1 O9 69.65(10) . . ? O6 Dy1 O9 125.99(11) . . ? O5 Dy1 O9 131.64(10) . . ? O1W Dy1 O9 76.05(11) . . ? O1 P1 O3 113.0(3) . . ? O1 P1 O2 111.4(3) . . ? O3 P1 O2 107.5(4) . . ? O1 P1 C1 112.4(2) . . ? O3 P1 C1 104.9(3) . . ? O2 P1 C1 107.2(3) . . ? Dy1 O1W H1WB 109.4 . . ? Dy1 O1W H1WC 109.5 . . ? H1WB O1W H1WC 109.5 . . ? P1 O1 Dy1 165.8(2) . . ? C16 O2 P1 125.7(5) . . ? C18 O3 P1 124.6(5) . . ? C21 O4 Dy1 132.8(3) . . ? C23 O5 Dy1 131.1(3) . . ? C26 O6 Dy1 134.9(3) . . ? C28 O7 Dy1 135.6(3) . . ? C31 O8 Dy1 131.5(3) . . ? C33 O9 Dy1 128.4(3) . . ? C2 C1 P1 117.2(4) . . ? C2 C1 H1A 108.0 . . ? P1 C1 H1A 108.0 . . ? C2 C1 H1B 108.0 . . ? P1 C1 H1B 108.0 . . ? H1A C1 H1B 107.3 . . ? C15 C2 C3 122.2(5) . . ? C15 C2 C1 119.2(7) . . ? C3 C2 C1 118.5(7) . . ? C4 C3 C8 120.0 . . ? C4 C3 C2 122.6(5) . . ? C8 C3 C2 117.4(5) . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C3 120.0 . . ? C7 C8 C9 121.7(6) . . ? C3 C8 C9 118.2(6) . . ? C10 C9 C8 125.8(7) . . ? C10 C9 H9A 117.1 . . ? C8 C9 H9A 117.1 . . ? C9 C10 C11 121.6(6) . . ? C9 C10 C15 118.4(6) . . ? C11 C10 C15 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 C2 121.9(5) . . ? C10 C15 C2 118.1(5) . . ? C17 C16 O2 117.6(10) . . ? C17 C16 H16A 107.6 . . ? O2 C16 H16A 106.6 . . ? C17 C16 H16B 107.1 . . ? O2 C16 H16B 110.0 . . ? H16A C16 H16B 107.5 . . ? C16 C17 H17C 109.5 . . ? C16 C17 H17D 109.5 . . ? H17C C17 H17D 109.5 . . ? C16 C17 H17E 109.5 . . ? H17C C17 H17E 109.5 . . ? H17D C17 H17E 109.5 . . ? C19 C18 O3 110.6(8) . . ? C19 C18 H18D 109.5 . . ? O3 C18 H18D 109.5 . . ? C19 C18 H18E 109.5 . . ? O3 C18 H18E 109.5 . . ? H18D C18 H18E 108.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F3A C20 F1 128.6(9) . . ? F3A C20 F1A 112.0(11) . . ? F1 C20 F1A 55.2(9) . . ? F3A C20 F3 42.6(8) . . ? F1 C20 F3 106.5(10) . . ? F1A C20 F3 134.7(9) . . ? F3A C20 F2A 104.9(11) . . ? F1 C20 F2A 52.5(8) . . ? F1A C20 F2A 107.1(11) . . ? F3 C20 F2A 64.2(10) . . ? F3A C20 F2 62.0(9) . . ? F1 C20 F2 107.2(10) . . ? F1A C20 F2 56.8(9) . . ? F3 C20 F2 102.7(9) . . ? F2A C20 F2 144.0(9) . . ? F3A C20 C21 114.2(8) . . ? F1 C20 C21 116.3(6) . . ? F1A C20 C21 112.2(7) . . ? F3 C20 C21 112.8(7) . . ? F2A C20 C21 105.6(7) . . ? F2 C20 C21 110.3(7) . . ? O4 C21 C22 127.7(5) . . ? O4 C21 C20 114.7(5) . . ? C22 C21 C20 117.6(4) . . ? C21 C22 C23 121.7(4) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? O5 C23 C22 127.8(4) . . ? O5 C23 C24 114.5(4) . . ? C22 C23 C24 117.7(4) . . ? F4A C24 F6 120.7(14) . . ? F4A C24 F5A 110.0(13) . . ? F6 C24 F5A 76.0(9) . . ? F4A C24 F4 23.3(14) . . ? F6 C24 F4 109.0(11) . . ? F5A C24 F4 129.7(11) . . ? F4A C24 F6A 108.1(14) . . ? F6 C24 F6A 31.3(9) . . ? F5A C24 F6A 107.3(11) . . ? F4 C24 F6A 88.3(11) . . ? F4A C24 F5 82.8(11) . . ? F6 C24 F5 105.2(9) . . ? F5A C24 F5 32.6(7) . . ? F4 C24 F5 105.6(9) . . ? F6A C24 F5 134.9(11) . . ? F4A C24 C23 116.6(14) . . ? F6 C24 C23 115.7(7) . . ? F5A C24 C23 109.5(8) . . ? F4 C24 C23 112.0(10) . . ? F6A C24 C23 104.9(9) . . ? F5 C24 C23 108.6(7) . . ? F8 C25 F7A 125.5(10) . . ? F8 C25 F9A 51.0(9) . . ? F7A C25 F9A 103.0(12) . . ? F8 C25 F8A 46.9(8) . . ? F7A C25 F8A 118.9(12) . . ? F9A C25 F8A 97.8(10) . . ? F8 C25 F7 105.2(11) . . ? F7A C25 F7 48.6(9) . . ? F9A C25 F7 60.0(9) . . ? F8A C25 F7 141.1(9) . . ? F8 C25 F9 109.7(11) . . ? F7A C25 F9 58.1(10) . . ? F9A C25 F9 141.6(9) . . ? F8A C25 F9 70.2(10) . . ? F7 C25 F9 106.3(10) . . ? F8 C25 C26 117.1(8) . . ? F7A C25 C26 116.6(7) . . ? F9A C25 C26 108.3(8) . . ? F8A C25 C26 109.6(7) . . ? F7 C25 C26 107.8(7) . . ? F9 C25 C26 110.1(6) . . ? O6 C26 C27 127.4(5) . . ? O6 C26 C25 113.7(5) . . ? C27 C26 C25 118.9(5) . . ? C28 C27 C26 121.1(5) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? O7 C28 C27 126.6(5) . . ? O7 C28 C29 114.1(6) . . ? C27 C28 C29 119.2(6) . . ? F10 C29 F12 107.3(7) . . ? F10 C29 F11 105.3(7) . . ? F12 C29 F11 107.2(8) . . ? F10 C29 C28 114.6(7) . . ? F12 C29 C28 111.9(6) . . ? F11 C29 C28 110.1(7) . . ? F14 C30 F13 106.6(5) . . ? F14 C30 F15 107.2(5) . . ? F13 C30 F15 107.9(5) . . ? F14 C30 C31 114.4(5) . . ? F13 C30 C31 110.6(4) . . ? F15 C30 C31 109.8(4) . . ? O8 C31 C32 126.1(4) . . ? O8 C31 C30 113.2(4) . . ? C32 C31 C30 120.6(4) . . ? C31 C32 C33 121.3(4) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 119.4 . . ? O9 C33 C32 127.8(4) . . ? O9 C33 C34 114.4(4) . . ? C32 C33 C34 117.8(4) . . ? F16 C34 F16A 74.1(9) . . ? F16 C34 F18 108.4(9) . . ? F16A C34 F18 126.5(12) . . ? F16 C34 F17A 126.8(10) . . ? F16A C34 F17A 111.5(14) . . ? F18 C34 F17A 24.6(10) . . ? F16 C34 F18A 39.2(6) . . ? F16A C34 F18A 110.6(9) . . ? F18 C34 F18A 75.5(9) . . ? F17A C34 F18A 99.2(10) . . ? F16 C34 F17 105.9(7) . . ? F16A C34 F17 33.3(9) . . ? F18 C34 F17 106.5(9) . . ? F17A C34 F17 84.7(10) . . ? F18A C34 F17 136.8(8) . . ? F16 C34 C33 114.6(6) . . ? F16A C34 C33 113.2(8) . . ? F18 C34 C33 113.3(9) . . ? F17A C34 C33 110.8(10) . . ? F18A C34 C33 110.7(7) . . ? F17 C34 C33 107.7(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.852 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.069 _database_code_depnum_ccdc_archive 'CCDC 925929' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '2 Gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 F18 Gd O10 P' _chemical_formula_weight 1124.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.4266(15) _cell_length_b 11.7278(7) _cell_length_c 29.6653(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.8430(10) _cell_angle_gamma 90.00 _cell_volume 8214.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9117 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.52 _exptl_crystal_description blocky _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4408 _exptl_absorpt_coefficient_mu 1.789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.657 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32353 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8057 _reflns_number_gt 7230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+36.1805P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8057 _refine_ls_number_parameters 577 _refine_ls_number_restraints 508 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.205 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.402215(8) 0.947909(16) 0.178912(7) 0.02136(10) Uani 1 1 d . . . P1 P 0.42710(8) 0.89365(11) 0.06224(4) 0.0446(4) Uani 1 1 d U . . F1 F 0.2751(2) 1.2116(4) 0.0818(2) 0.1162(19) Uani 1 1 d U . . F2 F 0.3229(2) 1.3571(5) 0.0994(2) 0.1081(17) Uani 1 1 d U . . F3 F 0.2632(2) 1.3229(5) 0.1324(2) 0.1089(16) Uani 1 1 d U . . F4 F 0.40716(17) 1.3730(3) 0.27820(13) 0.0571(9) Uani 1 1 d U . . F5 F 0.3935(2) 1.2152(4) 0.30906(13) 0.0723(12) Uani 1 1 d U . . F6 F 0.47439(15) 1.2534(3) 0.29899(15) 0.0686(12) Uani 1 1 d U . . F7 F 0.2220(3) 1.0696(7) 0.2267(3) 0.149(3) Uani 1 1 d U . . F8 F 0.2203(3) 0.9117(6) 0.2612(3) 0.136(2) Uani 1 1 d U . . F9 F 0.2861(2) 1.0236(6) 0.2820(2) 0.1074(18) Uani 1 1 d U . . F10 F 0.20995(16) 0.6516(4) 0.13103(19) 0.0812(14) Uani 1 1 d U . . F11 F 0.29155(18) 0.5755(3) 0.16070(18) 0.0711(12) Uani 1 1 d U . . F12 F 0.2745(2) 0.6554(4) 0.09301(18) 0.0867(15) Uani 1 1 d U . . F13 F 0.34203(14) 0.7831(3) 0.30718(12) 0.0497(8) Uani 1 1 d U . . F14 F 0.39283(15) 0.6322(3) 0.32359(11) 0.0469(8) Uani 1 1 d U . . F15 F 0.43013(15) 0.7968(3) 0.34306(10) 0.0477(8) Uani 1 1 d U . . F16 F 0.4559(2) 0.4701(3) 0.20105(13) 0.0704(13) Uani 1 1 d U . . F17 F 0.49385(15) 0.5695(3) 0.15746(12) 0.0478(8) Uani 1 1 d U . . F18 F 0.40551(16) 0.5410(3) 0.13729(14) 0.0591(10) Uani 1 1 d U . . O1W O 0.50098(13) 0.9933(3) 0.19270(11) 0.0272(6) Uani 1 1 d U . . H1WC H 0.5148 0.9662 0.1671 0.033 Uiso 1 1 d R . . H1WB H 0.5216 0.9572 0.2210 0.033 Uiso 1 1 d R . . O1 O 0.41503(16) 0.9329(3) 0.10569(11) 0.0336(8) Uani 1 1 d U . . O2 O 0.3745(3) 0.9257(4) 0.01899(14) 0.0860(18) Uani 1 1 d U . . O3 O 0.4826(3) 0.9445(3) 0.05459(17) 0.0634(14) Uani 1 1 d U . . O4 O 0.35956(15) 1.1127(3) 0.13909(12) 0.0370(8) Uani 1 1 d U . . O5 O 0.42611(13) 1.1068(2) 0.23197(11) 0.0269(6) Uani 1 1 d U . . O6 O 0.32033(14) 0.9886(3) 0.20447(13) 0.0356(8) Uani 1 1 d U . . O7 O 0.33191(14) 0.8113(3) 0.14783(13) 0.0367(8) Uani 1 1 d U . . O8 O 0.41260(13) 0.8567(2) 0.25238(10) 0.0265(6) Uani 1 1 d U . . O9 O 0.44755(13) 0.7606(2) 0.17964(10) 0.0268(6) Uani 1 1 d U . . C1 C 0.4363(3) 0.7427(4) 0.06132(18) 0.0510(16) Uani 1 1 d U . . H1A H 0.4696 0.7229 0.0858 0.061 Uiso 1 1 calc R . . H1B H 0.4040 0.7070 0.0691 0.061 Uiso 1 1 calc R . . C2 C 0.4425(3) 0.6916(4) 0.01610(18) 0.0539(17) Uani 1 1 d U . . C3 C 0.3937(4) 0.6493(5) -0.0171(2) 0.0621(19) Uani 1 1 d U . . C4 C 0.3379(4) 0.6542(6) -0.0113(3) 0.074(2) Uani 1 1 d U . . H4A H 0.3316 0.6897 0.0149 0.089 Uiso 1 1 calc R . . C5 C 0.2934(5) 0.6079(7) -0.0435(3) 0.087(3) Uani 1 1 d U . . H5A H 0.2574 0.6123 -0.0385 0.104 Uiso 1 1 calc R . . C6 C 0.3001(5) 0.5540(6) -0.0837(3) 0.085(2) Uani 1 1 d U . . H6A H 0.2691 0.5217 -0.1048 0.102 Uiso 1 1 calc R . . C7 C 0.3519(5) 0.5492(5) -0.0916(2) 0.0734(17) Uani 1 1 d U . . H7A H 0.3561 0.5150 -0.1188 0.088 Uiso 1 1 calc R . . C8 C 0.4013(4) 0.5960(5) -0.0588(2) 0.0634(13) Uani 1 1 d U . . C9 C 0.4548(4) 0.5898(5) -0.0658(2) 0.0639(13) Uani 1 1 d U . . H9A H 0.4590 0.5574 -0.0933 0.077 Uiso 1 1 calc R . . C10 C 0.5033(4) 0.6296(5) -0.0335(2) 0.0611(13) Uani 1 1 d U . . C11 C 0.5586(4) 0.6196(6) -0.0406(3) 0.0739(16) Uani 1 1 d U . . H11A H 0.5626 0.5879 -0.0683 0.089 Uiso 1 1 calc R . . C12 C 0.6054(4) 0.6546(6) -0.0087(3) 0.076(2) Uani 1 1 d U . . H12A H 0.6411 0.6453 -0.0139 0.091 Uiso 1 1 calc R . . C13 C 0.5991(4) 0.7066(5) 0.0336(3) 0.073(2) Uani 1 1 d U . . H13A H 0.6310 0.7318 0.0558 0.088 Uiso 1 1 calc R . . C14 C 0.5478(4) 0.7193(5) 0.0414(2) 0.0604(18) Uani 1 1 d U . . H14A H 0.5449 0.7537 0.0690 0.072 Uiso 1 1 calc R . . C15 C 0.4977(4) 0.6818(4) 0.00884(19) 0.0574(18) Uani 1 1 d U . . C16 C 0.3453(4) 1.0380(7) 0.0182(3) 0.084(3) Uani 1 1 d DU . . H16A H 0.3288 1.0437 0.0445 0.100 Uiso 1 1 calc R . . H16B H 0.3723 1.0997 0.0202 0.100 Uiso 1 1 calc R . . C17 C 0.3016(4) 1.0459(6) -0.0250(3) 0.083(3) Uani 1 1 d DU . . H17A H 0.2828 1.1183 -0.0265 0.125 Uiso 1 1 calc R . . H17B H 0.2746 0.9857 -0.0263 0.125 Uiso 1 1 calc R . . H17C H 0.3183 1.0391 -0.0508 0.125 Uiso 1 1 calc R . . C18 C 0.5004(3) 1.0636(4) 0.0642(2) 0.0495(15) Uani 1 1 d U . . H18A H 0.4880 1.1087 0.0360 0.059 Uiso 1 1 calc R . . H18B H 0.4832 1.0950 0.0876 0.059 Uiso 1 1 calc R . . C19 C 0.5624(4) 1.0687(6) 0.0812(2) 0.067(2) Uani 1 1 d U . . H19A H 0.5740 1.1465 0.0875 0.101 Uiso 1 1 calc R . . H19B H 0.5792 1.0382 0.0578 0.101 Uiso 1 1 calc R . . H19C H 0.5743 1.0246 0.1092 0.101 Uiso 1 1 calc R . . C20 C 0.3004(3) 1.2718(5) 0.1163(2) 0.0539(12) Uani 1 1 d U . . C21 C 0.3441(2) 1.2058(4) 0.1530(2) 0.0410(10) Uani 1 1 d U . . C22 C 0.3629(2) 1.2547(4) 0.19688(19) 0.0355(10) Uani 1 1 d U . . H22A H 0.3484 1.3252 0.2024 0.043 Uiso 1 1 calc R . . C23 C 0.40215(19) 1.2025(4) 0.23255(18) 0.0300(10) Uani 1 1 d U . . C24 C 0.4193(2) 1.2627(4) 0.27986(19) 0.0379(11) Uani 1 1 d U . . C25 C 0.2501(3) 0.9815(6) 0.2440(3) 0.0614(16) Uani 1 1 d U . . C26 C 0.2812(2) 0.9293(5) 0.2110(2) 0.0431(12) Uani 1 1 d U . . C27 C 0.2633(2) 0.8237(5) 0.1912(2) 0.0487(14) Uani 1 1 d U . . H27A H 0.2341 0.7853 0.1996 0.058 Uiso 1 1 calc R . . C28 C 0.2887(2) 0.7760(4) 0.1593(2) 0.0422(12) Uani 1 1 d U . . C29 C 0.2656(3) 0.6639(6) 0.1354(3) 0.0622(18) Uani 1 1 d U . . C30 C 0.3929(2) 0.7400(4) 0.30961(17) 0.0329(10) Uani 1 1 d U . . C31 C 0.40862(18) 0.7540(4) 0.26302(15) 0.0249(9) Uani 1 1 d U . . C32 C 0.41774(19) 0.6586(4) 0.23858(16) 0.0273(9) Uani 1 1 d U . . H32A H 0.4106 0.5863 0.2487 0.033 Uiso 1 1 calc R . . C33 C 0.43775(19) 0.6707(4) 0.19867(15) 0.0258(9) Uani 1 1 d U . . C34 C 0.4486(2) 0.5605(4) 0.17395(18) 0.0346(11) Uani 1 1 d U . . 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 0.02123(14) 0.01797(13) 0.02396(14) 0.00265(7) 0.00412(9) -0.00061(7) P1 0.0928(12) 0.0219(6) 0.0171(5) 0.0006(4) 0.0102(6) -0.0105(6) F1 0.116(3) 0.064(3) 0.117(3) -0.006(2) -0.065(3) 0.037(2) F2 0.098(3) 0.093(3) 0.108(3) 0.060(3) -0.019(3) -0.004(3) F3 0.090(3) 0.126(4) 0.101(3) 0.023(3) 0.007(2) 0.073(3) F4 0.085(3) 0.0295(16) 0.057(2) -0.0059(14) 0.0192(19) 0.0184(16) F5 0.109(3) 0.065(2) 0.048(2) -0.0023(18) 0.030(2) -0.023(2) F6 0.047(2) 0.062(2) 0.083(3) -0.042(2) -0.0090(19) 0.0089(17) F7 0.148(5) 0.169(5) 0.149(5) 0.031(4) 0.074(4) 0.118(4) F8 0.139(5) 0.133(4) 0.181(5) -0.046(4) 0.125(4) -0.066(4) F9 0.084(3) 0.140(4) 0.113(4) -0.051(4) 0.053(3) -0.009(3) F10 0.045(2) 0.060(2) 0.130(4) -0.018(2) 0.008(2) -0.0293(19) F11 0.067(3) 0.0361(18) 0.114(4) -0.008(2) 0.032(3) -0.0122(18) F12 0.099(3) 0.074(3) 0.087(3) -0.035(2) 0.025(3) -0.049(3) F13 0.0481(19) 0.058(2) 0.0536(19) 0.0075(16) 0.0326(16) 0.0093(15) F14 0.068(2) 0.0385(16) 0.0430(17) 0.0151(13) 0.0295(16) -0.0011(15) F15 0.062(2) 0.0570(19) 0.0260(14) -0.0032(13) 0.0150(14) -0.0144(16) F16 0.145(4) 0.0246(15) 0.057(2) 0.0112(15) 0.055(3) 0.019(2) F17 0.056(2) 0.0388(16) 0.056(2) -0.0130(14) 0.0269(17) 0.0042(14) F18 0.050(2) 0.055(2) 0.067(2) -0.0339(17) 0.0042(18) -0.0064(15) O1W 0.0246(16) 0.0278(16) 0.0295(15) 0.0015(13) 0.0076(13) 0.0013(12) O1 0.045(2) 0.0296(16) 0.0238(16) 0.0045(12) 0.0053(15) -0.0002(14) O2 0.177(5) 0.0287(19) 0.027(2) 0.0019(16) -0.020(2) -0.001(3) O3 0.119(4) 0.027(2) 0.065(3) -0.0080(17) 0.061(3) -0.014(2) O4 0.043(2) 0.0256(16) 0.0393(18) 0.0052(14) 0.0050(16) 0.0088(14) O5 0.0219(15) 0.0208(15) 0.0372(17) -0.0010(13) 0.0065(13) 0.0016(12) O6 0.0266(17) 0.0312(17) 0.050(2) 0.0031(15) 0.0120(15) 0.0000(14) O7 0.0286(18) 0.0309(17) 0.047(2) 0.0003(15) 0.0029(15) -0.0064(14) O8 0.0324(17) 0.0228(15) 0.0255(15) 0.0023(12) 0.0094(13) -0.0011(12) O9 0.0329(17) 0.0228(15) 0.0257(15) 0.0036(12) 0.0092(13) 0.0008(12) C1 0.105(5) 0.025(2) 0.025(2) -0.0024(19) 0.019(3) -0.013(3) C2 0.119(5) 0.019(2) 0.024(2) -0.0004(19) 0.019(3) -0.012(3) C3 0.126(6) 0.027(3) 0.032(3) -0.003(2) 0.018(3) -0.013(3) C4 0.121(6) 0.051(4) 0.052(4) -0.004(3) 0.024(4) -0.028(4) C5 0.120(7) 0.065(5) 0.075(5) -0.012(4) 0.025(5) -0.030(5) C6 0.129(4) 0.052(4) 0.061(4) -0.007(3) -0.002(4) -0.015(4) C7 0.135(4) 0.037(3) 0.036(3) -0.010(2) 0.000(3) -0.003(3) C8 0.125(3) 0.029(3) 0.031(3) -0.003(2) 0.010(3) -0.005(3) C9 0.134(3) 0.027(3) 0.030(3) -0.004(2) 0.019(3) 0.000(3) C10 0.122(3) 0.026(3) 0.037(3) 0.002(2) 0.025(2) -0.001(3) C11 0.131(3) 0.037(3) 0.061(4) 0.001(3) 0.038(4) 0.004(4) C12 0.111(6) 0.044(3) 0.081(5) 0.011(3) 0.041(5) 0.007(4) C13 0.121(6) 0.032(3) 0.066(4) 0.011(3) 0.022(4) 0.000(4) C14 0.111(6) 0.031(3) 0.043(3) 0.006(2) 0.027(4) 0.001(3) C15 0.122(6) 0.020(2) 0.031(3) 0.003(2) 0.021(3) -0.004(3) C16 0.104(6) 0.067(5) 0.070(5) -0.001(4) 0.003(4) 0.001(4) C17 0.120(8) 0.050(4) 0.069(5) 0.009(3) 0.005(5) -0.010(4) C18 0.078(4) 0.025(2) 0.051(3) 0.003(2) 0.025(3) -0.005(2) C19 0.095(6) 0.058(4) 0.045(4) 0.001(3) 0.010(4) 0.003(4) C20 0.054(3) 0.034(2) 0.063(3) 0.011(2) -0.005(2) 0.011(2) C21 0.039(2) 0.030(2) 0.050(2) 0.0100(18) 0.005(2) 0.0066(17) C22 0.030(2) 0.024(2) 0.052(2) 0.0025(19) 0.0100(19) 0.0060(18) C23 0.024(2) 0.023(2) 0.045(3) 0.0026(19) 0.011(2) -0.0012(17) C24 0.038(3) 0.028(2) 0.049(3) -0.005(2) 0.012(2) 0.005(2) C25 0.039(3) 0.058(3) 0.097(4) -0.002(3) 0.036(3) -0.003(3) C26 0.027(2) 0.040(3) 0.064(3) 0.006(2) 0.015(2) 0.001(2) C27 0.033(3) 0.045(3) 0.069(4) 0.004(3) 0.015(3) -0.014(2) C28 0.033(3) 0.032(3) 0.057(3) 0.002(2) 0.003(2) -0.008(2) C29 0.052(4) 0.049(3) 0.085(5) -0.010(3) 0.015(3) -0.022(3) C30 0.039(3) 0.033(2) 0.031(2) 0.0041(19) 0.015(2) -0.002(2) C31 0.023(2) 0.027(2) 0.025(2) 0.0038(17) 0.0062(17) -0.0023(16) C32 0.030(2) 0.021(2) 0.030(2) 0.0036(17) 0.0065(18) -0.0023(17) C33 0.027(2) 0.024(2) 0.023(2) 0.0004(16) 0.0026(17) 0.0012(17) C34 0.048(3) 0.027(2) 0.031(2) 0.0009(18) 0.014(2) 0.0003(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O1 2.279(3) . ? Gd1 O7 2.357(3) . ? Gd1 O6 2.362(3) . ? Gd1 O4 2.364(3) . ? Gd1 O8 2.382(3) . ? Gd1 O1W 2.401(3) . ? Gd1 O5 2.412(3) . ? Gd1 O9 2.458(3) . ? P1 O1 1.468(4) . ? P1 O3 1.550(5) . ? P1 O2 1.611(5) . ? P1 C1 1.786(5) . ? F1 C20 1.269(8) . ? F2 C20 1.303(8) . ? F3 C20 1.280(8) . ? F4 C24 1.326(6) . ? F5 C24 1.317(6) . ? F6 C24 1.324(6) . ? F7 C25 1.273(9) . ? F8 C25 1.285(8) . ? F9 C25 1.334(10) . ? F10 C29 1.340(8) . ? F11 C29 1.339(9) . ? F12 C29 1.335(9) . ? F13 C30 1.325(6) . ? F14 C30 1.331(6) . ? F15 C30 1.339(6) . ? F16 C34 1.315(6) . ? F17 C34 1.322(6) . ? F18 C34 1.325(7) . ? O1W H1WC 0.9600 . ? O1W H1WB 0.9600 . ? O2 C16 1.494(10) . ? O3 C18 1.470(6) . ? O4 C21 1.257(6) . ? O5 C23 1.268(5) . ? O6 C26 1.237(6) . ? O7 C28 1.260(6) . ? O8 C31 1.255(5) . ? O9 C33 1.247(5) . ? C1 C2 1.512(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C15 1.423(11) . ? C2 C3 1.427(10) . ? C3 C4 1.416(12) . ? C3 C8 1.442(9) . ? C4 C5 1.364(11) . ? C4 H4A 0.9300 . ? C5 C6 1.397(13) . ? C5 H5A 0.9300 . ? C6 C7 1.345(14) . ? C6 H6A 0.9300 . ? C7 C8 1.450(11) . ? C7 H7A 0.9300 . ? C8 C9 1.376(11) . ? C9 C10 1.399(11) . ? C9 H9A 0.9300 . ? C10 C11 1.425(12) . ? C10 C15 1.434(8) . ? C11 C12 1.349(12) . ? C11 H11A 0.9300 . ? C12 C13 1.438(11) . ? C12 H12A 0.9300 . ? C13 C14 1.339(11) . ? C13 H13A 0.9300 . ? C14 C15 1.421(10) . ? C14 H14A 0.9300 . ? C16 C17 1.446(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.469(11) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.526(7) . ? C21 C22 1.389(8) . ? C22 C23 1.376(7) . ? C22 H22A 0.9300 . ? C23 C24 1.530(7) . ? C25 C26 1.512(9) . ? C26 C27 1.392(8) . ? C27 C28 1.376(8) . ? C27 H27A 0.9300 . ? C28 C29 1.531(8) . ? C30 C31 1.536(6) . ? C31 C32 1.382(6) . ? C32 C33 1.399(6) . ? C32 H32A 0.9300 . ? C33 C34 1.543(6) . ? 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 O1 Gd1 O7 80.73(13) . . ? O1 Gd1 O6 130.98(13) . . ? O7 Gd1 O6 70.79(12) . . ? O1 Gd1 O4 74.78(12) . . ? O7 Gd1 O4 100.18(12) . . ? O6 Gd1 O4 72.19(12) . . ? O1 Gd1 O8 145.97(11) . . ? O7 Gd1 O8 87.07(12) . . ? O6 Gd1 O8 72.39(11) . . ? O4 Gd1 O8 138.97(11) . . ? O1 Gd1 O1W 78.59(12) . . ? O7 Gd1 O1W 144.77(11) . . ? O6 Gd1 O1W 142.84(12) . . ? O4 Gd1 O1W 101.48(12) . . ? O8 Gd1 O1W 94.40(11) . . ? O1 Gd1 O5 127.75(11) . . ? O7 Gd1 O5 144.15(11) . . ? O6 Gd1 O5 73.60(11) . . ? O4 Gd1 O5 72.33(12) . . ? O8 Gd1 O5 78.37(10) . . ? O1W Gd1 O5 69.70(10) . . ? O1 Gd1 O9 76.57(11) . . ? O7 Gd1 O9 71.17(11) . . ? O6 Gd1 O9 126.47(11) . . ? O4 Gd1 O9 151.08(11) . . ? O8 Gd1 O9 69.43(10) . . ? O1W Gd1 O9 76.45(10) . . ? O5 Gd1 O9 130.65(10) . . ? O1 P1 O3 112.8(2) . . ? O1 P1 O2 109.1(3) . . ? O3 P1 O2 110.1(3) . . ? O1 P1 C1 112.2(2) . . ? O3 P1 C1 105.1(3) . . ? O2 P1 C1 107.3(3) . . ? Gd1 O1W H1WC 109.5 . . ? Gd1 O1W H1WB 109.4 . . ? H1WC O1W H1WB 109.5 . . ? P1 O1 Gd1 165.6(2) . . ? C16 O2 P1 119.9(4) . . ? C18 O3 P1 124.3(4) . . ? C21 O4 Gd1 132.6(3) . . ? C23 O5 Gd1 131.1(3) . . ? C26 O6 Gd1 133.6(3) . . ? C28 O7 Gd1 134.0(4) . . ? C31 O8 Gd1 131.6(3) . . ? C33 O9 Gd1 128.4(3) . . ? C2 C1 P1 116.6(4) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C15 C2 C3 121.7(5) . . ? C15 C2 C1 118.7(6) . . ? C3 C2 C1 119.5(7) . . ? C4 C3 C2 124.3(6) . . ? C4 C3 C8 117.5(7) . . ? C2 C3 C8 118.2(8) . . ? C5 C4 C3 121.2(8) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 122.1(10) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C7 C6 C5 119.3(9) . . ? C7 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? C6 C7 C8 121.8(7) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C9 C8 C7 122.6(6) . . ? C9 C8 C3 119.3(7) . . ? C7 C8 C3 118.1(8) . . ? C8 C9 C10 123.3(6) . . ? C8 C9 H9A 118.3 . . ? C10 C9 H9A 118.3 . . ? C9 C10 C11 122.6(6) . . ? C9 C10 C15 119.2(7) . . ? C11 C10 C15 118.1(7) . . ? C12 C11 C10 122.4(7) . . ? C12 C11 H11A 118.8 . . ? C10 C11 H11A 118.8 . . ? C11 C12 C13 118.7(8) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C14 C13 C12 120.9(8) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 121.9(7) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C2 C15 C14 123.8(5) . . ? C2 C15 C10 118.2(7) . . ? C14 C15 C10 118.0(7) . . ? C17 C16 O2 108.2(7) . . ? C17 C16 H16A 110.1 . . ? O2 C16 H16A 110.1 . . ? C17 C16 H16B 110.1 . . ? O2 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O3 109.4(5) . . ? C19 C18 H18A 109.8 . . ? O3 C18 H18A 109.8 . . ? C19 C18 H18B 109.8 . . ? O3 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F1 C20 F3 108.4(7) . . ? F1 C20 F2 106.3(7) . . ? F3 C20 F2 101.3(6) . . ? F1 C20 C21 113.6(5) . . ? F3 C20 C21 114.0(6) . . ? F2 C20 C21 112.2(5) . . ? O4 C21 C22 127.7(5) . . ? O4 C21 C20 114.9(5) . . ? C22 C21 C20 117.4(5) . . ? C23 C22 C21 122.3(4) . . ? C23 C22 H22A 118.8 . . ? C21 C22 H22A 118.8 . . ? O5 C23 C22 128.1(5) . . ? O5 C23 C24 113.7(4) . . ? C22 C23 C24 118.2(4) . . ? F5 C24 F6 106.7(5) . . ? F5 C24 F4 107.3(4) . . ? F6 C24 F4 106.8(4) . . ? F5 C24 C23 110.1(4) . . ? F6 C24 C23 111.4(4) . . ? F4 C24 C23 114.2(4) . . ? F7 C25 F8 112.1(7) . . ? F7 C25 F9 102.2(7) . . ? F8 C25 F9 102.6(7) . . ? F7 C25 C26 112.0(7) . . ? F8 C25 C26 115.4(6) . . ? F9 C25 C26 111.4(5) . . ? O6 C26 C27 127.2(6) . . ? O6 C26 C25 114.2(5) . . ? C27 C26 C25 118.5(5) . . ? C28 C27 C26 120.3(5) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? O7 C28 C27 127.5(5) . . ? O7 C28 C29 113.1(5) . . ? C27 C28 C29 119.4(5) . . ? F10 C29 F12 107.8(6) . . ? F10 C29 F11 107.1(5) . . ? F12 C29 F11 107.6(6) . . ? F10 C29 C28 112.4(6) . . ? F12 C29 C28 111.7(5) . . ? F11 C29 C28 109.9(6) . . ? F13 C30 F14 107.7(4) . . ? F13 C30 F15 107.5(4) . . ? F14 C30 F15 107.2(4) . . ? F13 C30 C31 111.0(4) . . ? F14 C30 C31 113.7(4) . . ? F15 C30 C31 109.5(4) . . ? O8 C31 C32 127.7(4) . . ? O8 C31 C30 112.5(4) . . ? C32 C31 C30 119.8(4) . . ? C31 C32 C33 120.0(4) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? O9 C33 C32 128.2(4) . . ? O9 C33 C34 114.6(4) . . ? C32 C33 C34 117.2(4) . . ? F17 C34 F16 107.2(5) . . ? F17 C34 F18 105.9(4) . . ? F16 C34 F18 108.5(5) . . ? F17 C34 C33 111.7(4) . . ? F16 C34 C33 113.5(4) . . ? F18 C34 C33 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.721 _refine_diff_density_min -1.547 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 925930' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_20120312a #TrackingRef '3 Dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H92 Dy2 F36 O25 P4' _chemical_formula_weight 2898.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8118(6) _cell_length_b 39.565(2) _cell_length_c 26.3821(11) _cell_angle_alpha 90.00 _cell_angle_beta 112.919(2) _cell_angle_gamma 90.00 _cell_volume 12317.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 23.34 _exptl_crystal_description blocky _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5776 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86032 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 24219 _reflns_number_gt 12882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24219 _refine_ls_number_parameters 1566 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.96877(3) 0.267296(8) 0.739079(12) 0.05026(10) Uani 1 1 d . . . Dy2 Dy 0.49927(3) 0.484739(8) 0.746816(12) 0.05133(10) Uani 1 1 d . . . P1 P 0.89700(14) 0.24992(4) 0.59299(6) 0.0498(4) Uani 1 1 d D . . P2 P 1.06271(14) 0.24457(4) 0.88393(6) 0.0468(4) Uani 1 1 d . . . P3 P 0.57715(14) 0.50234(4) 0.89325(7) 0.0509(4) Uani 1 1 d . . . P4 P 0.40958(14) 0.50661(4) 0.60059(7) 0.0523(4) Uani 1 1 d . . . F1 F 1.2968(3) 0.18040(9) 0.80538(14) 0.0580(9) Uani 1 1 d . . . F2 F 1.2020(3) 0.17297(9) 0.71799(14) 0.0575(9) Uani 1 1 d . . . F3 F 1.3605(3) 0.19442(9) 0.74536(15) 0.0610(9) Uani 1 1 d . . . F4 F 1.3054(3) 0.28872(10) 0.67463(15) 0.0624(10) Uani 1 1 d . . . F5 F 1.2241(3) 0.33866(10) 0.69341(15) 0.0642(10) Uani 1 1 d . . . F6 F 1.3752(3) 0.31779(10) 0.74538(18) 0.0742(12) Uani 1 1 d . . . F7 F 0.9012(3) 0.35739(10) 0.61000(15) 0.0668(10) Uani 1 1 d . . . F8 F 0.8529(3) 0.40131(9) 0.64940(14) 0.0592(9) Uani 1 1 d . . . F9 F 0.7332(3) 0.36037(10) 0.61709(14) 0.0660(10) Uani 1 1 d . . . F10 F 1.0267(3) 0.39770(9) 0.84409(14) 0.0639(10) Uani 1 1 d . . . F11 F 1.0008(3) 0.35356(9) 0.88401(14) 0.0563(9) Uani 1 1 d . . . F12 F 1.1426(3) 0.35589(8) 0.86993(13) 0.0557(9) Uani 1 1 d . . . F13 F 0.5764(3) 0.29899(8) 0.70952(13) 0.0508(8) Uani 1 1 d . . . F14 F 0.6464(3) 0.28598(9) 0.79585(13) 0.0550(9) Uani 1 1 d . . . F15 F 0.5310(3) 0.25235(8) 0.73931(13) 0.0509(8) Uani 1 1 d . . . F16 F 0.7007(3) 0.15381(10) 0.73631(16) 0.0680(10) Uani 1 1 d . . . F17 F 0.8598(3) 0.14762(9) 0.72777(16) 0.0634(10) Uani 1 1 d . . . F18 F 0.7070(3) 0.15962(9) 0.65905(15) 0.0640(10) Uani 1 1 d . . . F19 F 0.8287(3) 0.46619(9) 0.69398(14) 0.0579(9) Uani 1 1 d . . . F20 F 0.8948(3) 0.45347(9) 0.78063(14) 0.0588(9) Uani 1 1 d . . . F21 F 0.9473(3) 0.49783(9) 0.75324(15) 0.0608(9) Uani 1 1 d . . . F22 F 0.7408(3) 0.60157(9) 0.73925(15) 0.0688(11) Uani 1 1 d . . . F23 F 0.7701(3) 0.59484(8) 0.82456(14) 0.0551(9) Uani 1 1 d . . . F24 F 0.6071(3) 0.60374(9) 0.77041(16) 0.0726(12) Uani 1 1 d . . . F25 F 0.2752(3) 0.58096(9) 0.76695(14) 0.0559(9) Uani 1 1 d . . . F26 F 0.1145(3) 0.55909(8) 0.74205(15) 0.0573(9) Uani 1 1 d . . . F27 F 0.1776(3) 0.57321(9) 0.68070(14) 0.0600(9) Uani 1 1 d . . . F28 F 0.1313(3) 0.44607(11) 0.79371(16) 0.0712(11) Uani 1 1 d . . . F29 F 0.2423(3) 0.40704(9) 0.78571(15) 0.0680(11) Uani 1 1 d . . . F30 F 0.1164(3) 0.42136(11) 0.71689(15) 0.0735(11) Uani 1 1 d . . . F31 F 0.5526(3) 0.38693(10) 0.86626(16) 0.0701(11) Uani 1 1 d . . . F32 F 0.7316(3) 0.39636(9) 0.88255(14) 0.0660(10) Uani 1 1 d . . . F33 F 0.6398(3) 0.35075(9) 0.84259(14) 0.0609(9) Uani 1 1 d . . . F34 F 0.3944(3) 0.35566(9) 0.64432(14) 0.0595(9) Uani 1 1 d . . . F35 F 0.5076(3) 0.38367(9) 0.61727(14) 0.0617(10) Uani 1 1 d . . . F36 F 0.3452(3) 0.40246(10) 0.60831(15) 0.0650(10) Uani 1 1 d . . . O1 O 0.9581(3) 0.25437(10) 0.65277(15) 0.0507(10) Uani 1 1 d D . . O1W O 0.0442(4) 0.38915(10) 0.23796(17) 0.0593(12) Uani 1 1 d . . . H1X H -0.0171 0.3786 0.2206 0.071 Uiso 1 1 d R . . H1Y H 0.0693 0.3974 0.2151 0.071 Uiso 1 1 d R . . O2 O 0.8867(4) 0.21214(11) 0.57531(18) 0.0584(11) Uani 1 1 d . . . O3 O 0.9556(4) 0.26919(10) 0.55967(16) 0.0514(10) Uani 1 1 d . . . O4 O 0.9951(3) 0.24690(10) 0.82401(15) 0.0472(9) Uani 1 1 d . . . O5 O 1.0088(3) 0.26236(11) 0.91788(17) 0.0537(11) Uani 1 1 d . . . O6 O 1.0794(3) 0.20682(10) 0.90507(15) 0.0494(10) Uani 1 1 d . . . O7 O 0.4703(4) 0.50536(10) 0.66151(16) 0.0539(11) Uani 1 1 d . . . O8 O 0.4684(4) 0.48774(10) 0.56895(16) 0.0505(10) Uani 1 1 d . . . O9 O 0.3959(4) 0.54321(11) 0.57761(17) 0.0563(11) Uani 1 1 d . . . O10 O 0.5107(3) 0.49885(10) 0.83373(16) 0.0491(10) Uani 1 1 d . . . O11 O 0.5896(3) 0.53968(10) 0.91338(17) 0.0531(11) Uani 1 1 d . . . O12 O 0.5209(4) 0.48230(10) 0.92797(17) 0.0557(11) Uani 1 1 d . . . O13 O 1.1168(3) 0.22853(10) 0.75897(16) 0.0477(10) Uani 1 1 d . . . O14 O 1.1270(3) 0.29895(10) 0.74362(16) 0.0480(10) Uani 1 1 d . . . O15 O 0.8917(3) 0.31595(10) 0.68314(14) 0.0450(9) Uani 1 1 d . . . O16 O 0.9974(3) 0.31353(10) 0.79937(15) 0.0505(10) Uani 1 1 d . . . O17 O 0.7838(4) 0.27385(10) 0.73441(16) 0.0507(10) Uani 1 1 d . . . O18 O 0.8721(3) 0.21465(10) 0.71717(16) 0.0482(10) Uani 1 1 d . . . O19 O 0.6845(3) 0.47851(10) 0.75297(16) 0.0485(10) Uani 1 1 d . . . O20 O 0.5955(3) 0.53907(10) 0.76722(16) 0.0504(10) Uani 1 1 d . . . O21 O 0.3456(3) 0.52374(10) 0.72663(16) 0.0529(10) Uani 1 1 d . . . O22 O 0.3391(3) 0.45645(10) 0.74703(16) 0.0494(10) Uani 1 1 d . . . O23 O 0.5774(3) 0.43738(10) 0.80326(16) 0.0478(9) Uani 1 1 d . . . O24 O 0.4693(3) 0.43831(9) 0.68741(15) 0.0457(9) Uani 1 1 d . . . C1 C 0.6159(6) 0.22986(16) 0.4921(3) 0.0612(19) Uani 1 1 d . . . C2 C 0.6084(6) 0.20624(15) 0.5310(3) 0.0607(18) Uani 1 1 d . . . H2 H 0.6534 0.2093 0.5690 0.073 Uiso 1 1 calc R . . C3 C 0.5377(6) 0.17938(16) 0.5145(3) 0.0644(19) Uani 1 1 d . . . H3 H 0.5314 0.1642 0.5411 0.077 Uiso 1 1 calc R . . C4 C 0.4768(6) 0.17399(17) 0.4612(3) 0.0603(17) Uani 1 1 d . . . H4 H 0.4290 0.1547 0.4507 0.072 Uiso 1 1 calc R . . C5 C 0.4812(6) 0.19631(18) 0.4194(3) 0.070(2) Uani 1 1 d . . . H5 H 0.4379 0.1922 0.3815 0.084 Uiso 1 1 calc R . . C6 C 0.5513(5) 0.22409(18) 0.4368(2) 0.0539(16) Uani 1 1 d . . . C7 C 0.5542(5) 0.24723(17) 0.3963(2) 0.0552(17) Uani 1 1 d . . . H7 H 0.5069 0.2431 0.3589 0.066 Uiso 1 1 calc R . . C8 C 0.6240(6) 0.27599(15) 0.4092(2) 0.0510(16) Uani 1 1 d . . . C9 C 0.6233(5) 0.29827(17) 0.3681(2) 0.0605(18) Uani 1 1 d . . . H9 H 0.5790 0.2940 0.3303 0.073 Uiso 1 1 calc R . . C10 C 0.6891(6) 0.32642(18) 0.3846(2) 0.0577(17) Uani 1 1 d . . . H10 H 0.6867 0.3420 0.3567 0.069 Uiso 1 1 calc R . . C11 C 0.7591(6) 0.33439(16) 0.4381(2) 0.0553(16) Uani 1 1 d . . . H11 H 0.8061 0.3539 0.4470 0.066 Uiso 1 1 calc R . . C12 C 0.7562(6) 0.31216(17) 0.4780(3) 0.0639(18) Uani 1 1 d . . . H12 H 0.8014 0.3169 0.5154 0.077 Uiso 1 1 calc R . . C13 C 0.6887(6) 0.28267(18) 0.4652(3) 0.0601(17) Uani 1 1 d . . . C14 C 0.6857(6) 0.26085(15) 0.5049(2) 0.0540(16) Uani 1 1 d . . . C15 C 0.7563(5) 0.26777(14) 0.5686(2) 0.0478(14) Uani 1 1 d . . . H15A H 0.7151 0.2581 0.5900 0.057 Uiso 1 1 calc R . . H15B H 0.7623 0.2925 0.5750 0.057 Uiso 1 1 calc R . . C16 C 0.9577(6) 0.18613(16) 0.6030(3) 0.0587(16) Uani 1 1 d . . . H16A H 0.9531 0.1842 0.6395 0.070 Uiso 1 1 calc R . . H16B H 1.0361 0.1932 0.6096 0.070 Uiso 1 1 calc R . . C17 C 0.9408(6) 0.15098(15) 0.5780(2) 0.0609(19) Uani 1 1 d . . . H17A H 0.8666 0.1497 0.5475 0.091 Uiso 1 1 calc R . . H17B H 0.9446 0.1343 0.6061 0.091 Uiso 1 1 calc R . . H17C H 1.0004 0.1463 0.5644 0.091 Uiso 1 1 calc R . . C18 C 1.0745(5) 0.27279(19) 0.5749(3) 0.0634(19) Uani 1 1 d . . . H18A H 1.1039 0.2510 0.5676 0.076 Uiso 1 1 calc R . . H18B H 1.1094 0.2766 0.6151 0.076 Uiso 1 1 calc R . . C19 C 1.1168(5) 0.30096(17) 0.5470(2) 0.0563(16) Uani 1 1 d . . . H19A H 1.0688 0.3017 0.5077 0.084 Uiso 1 1 calc R . . H19B H 1.1953 0.2963 0.5519 0.084 Uiso 1 1 calc R . . H19C H 1.1132 0.3228 0.5638 0.084 Uiso 1 1 calc R . . C20 C 1.3492(6) 0.22694(15) 0.9804(2) 0.0504(15) Uani 1 1 d . . . C21 C 1.3553(5) 0.20323(13) 0.9409(2) 0.0479(15) Uani 1 1 d . . . H21 H 1.3081 0.2064 0.9032 0.057 Uiso 1 1 calc R . . C22 C 1.4246(5) 0.17702(15) 0.9553(3) 0.0557(16) Uani 1 1 d . . . H22 H 1.4285 0.1621 0.9278 0.067 Uiso 1 1 calc R . . C23 C 1.4922(5) 0.17113(17) 1.0107(3) 0.0549(16) Uani 1 1 d . . . H23 H 1.5434 0.1526 1.0211 0.066 Uiso 1 1 calc R . . C24 C 1.4833(6) 0.19296(15) 1.0506(3) 0.0552(16) Uani 1 1 d . . . H24 H 1.5253 0.1885 1.0885 0.066 Uiso 1 1 calc R . . C25 C 1.4154(5) 0.22025(19) 1.0353(3) 0.0611(17) Uani 1 1 d . . . C26 C 1.4159(6) 0.24301(17) 1.0770(3) 0.0619(18) Uani 1 1 d . . . H26 H 1.4633 0.2386 1.1143 0.074 Uiso 1 1 calc R . . C27 C 1.3479(5) 0.27161(15) 1.0638(2) 0.0492(15) Uani 1 1 d . . . C28 C 1.3482(5) 0.29419(15) 1.1041(2) 0.0498(15) Uani 1 1 d . . . H28 H 1.3960 0.2896 1.1413 0.060 Uiso 1 1 calc R . . C29 C 1.2848(5) 0.32181(15) 1.0930(3) 0.0540(16) Uani 1 1 d . . . H29 H 1.2869 0.3362 1.1222 0.065 Uiso 1 1 calc R . . C30 C 1.2133(5) 0.33032(17) 1.0378(3) 0.0566(16) Uani 1 1 d . . . H30 H 1.1682 0.3502 1.0295 0.068 Uiso 1 1 calc R . . C31 C 1.2128(5) 0.30829(14) 0.9971(2) 0.0516(15) Uani 1 1 d . . . H31 H 1.1659 0.3134 0.9600 0.062 Uiso 1 1 calc R . . C32 C 1.2779(6) 0.27883(17) 1.0079(3) 0.0614(18) Uani 1 1 d . . . C33 C 1.2791(6) 0.25654(15) 0.9673(2) 0.0540(16) Uani 1 1 d . . . C34 C 1.2011(5) 0.26342(15) 0.9043(2) 0.0450(13) Uani 1 1 d . . . H34A H 1.2389 0.2543 0.8809 0.054 Uiso 1 1 calc R . . H34B H 1.1925 0.2881 0.8980 0.054 Uiso 1 1 calc R . . C35 C 0.8875(6) 0.26238(18) 0.9075(3) 0.0601(17) Uani 1 1 d . . . H35A H 0.8697 0.2420 0.9244 0.072 Uiso 1 1 calc R . . H35B H 0.8428 0.2613 0.8673 0.072 Uiso 1 1 calc R . . C36 C 0.8527(5) 0.29404(13) 0.9309(3) 0.0480(14) Uani 1 1 d . . . H36A H 0.8665 0.2903 0.9697 0.072 Uiso 1 1 calc R . . H36B H 0.7720 0.2986 0.9101 0.072 Uiso 1 1 calc R . . H36C H 0.8975 0.3134 0.9277 0.072 Uiso 1 1 calc R . . C37 C 1.0420(6) 0.17797(15) 0.8705(2) 0.0550(16) Uani 1 1 d . . . H37A H 1.0975 0.1735 0.8537 0.066 Uiso 1 1 calc R . . H37B H 0.9690 0.1837 0.8403 0.066 Uiso 1 1 calc R . . C38 C 1.0259(5) 0.14601(15) 0.8968(3) 0.0588(17) Uani 1 1 d . . . H38A H 1.0926 0.1420 0.9307 0.088 Uiso 1 1 calc R . . H38B H 1.0160 0.1271 0.8714 0.088 Uiso 1 1 calc R . . H38C H 0.9585 0.1481 0.9056 0.088 Uiso 1 1 calc R . . C39 C 1.2651(5) 0.19303(19) 0.7564(3) 0.0610(18) Uani 1 1 d . . . C40 C 1.2046(5) 0.22681(16) 0.7500(3) 0.0562(17) Uani 1 1 d . . . C41 C 1.2576(6) 0.25621(18) 0.7371(3) 0.0615(18) Uani 1 1 d . . . H41 H 1.3264 0.2537 0.7318 0.074 Uiso 1 1 calc R . . C42 C 1.2101(5) 0.28703(15) 0.7328(3) 0.0492(14) Uani 1 1 d . . . C43 C 1.2747(5) 0.30808(18) 0.7068(3) 0.0640(19) Uani 1 1 d . . . C44 C 0.8428(5) 0.36792(17) 0.6429(3) 0.0556(16) Uani 1 1 d . . . C45 C 0.8972(5) 0.34705(15) 0.6940(2) 0.0516(15) Uani 1 1 d . . . C46 C 0.9346(5) 0.36319(15) 0.7442(2) 0.0487(14) Uani 1 1 d . . . H46 H 0.9286 0.3871 0.7457 0.058 Uiso 1 1 calc R . . C47 C 0.9818(5) 0.34449(16) 0.7930(3) 0.0547(16) Uani 1 1 d . . . C48 C 1.0319(6) 0.36514(16) 0.8460(3) 0.0569(16) Uani 1 1 d . . . C49 C 0.6120(5) 0.27457(18) 0.7461(3) 0.0536(16) Uani 1 1 d . . . C50 C 0.7047(5) 0.25528(15) 0.7357(2) 0.0442(13) Uani 1 1 d . . . C51 C 0.6990(5) 0.22046(16) 0.7312(2) 0.0496(14) Uani 1 1 d . . . H51 H 0.6386 0.2084 0.7351 0.060 Uiso 1 1 calc R . . C52 C 0.7844(6) 0.20336(17) 0.7207(3) 0.0589(17) Uani 1 1 d . . . C53 C 0.7638(6) 0.16567(17) 0.7121(3) 0.0612(18) Uani 1 1 d . . . C54 C 0.2023(5) 0.47036(14) 0.4766(2) 0.0517(16) Uani 1 1 d . . . C55 C 0.2692(6) 0.44170(16) 0.4894(3) 0.0578(17) Uani 1 1 d . . . H55 H 0.3131 0.4367 0.5269 0.069 Uiso 1 1 calc R . . C56 C 0.2739(6) 0.42089(17) 0.4505(3) 0.0572(16) Uani 1 1 d . . . H56 H 0.3238 0.4021 0.4601 0.069 Uiso 1 1 calc R . . C57 C 0.2037(5) 0.42726(17) 0.3950(2) 0.0519(15) Uani 1 1 d . . . H57 H 0.2023 0.4117 0.3673 0.062 Uiso 1 1 calc R . . C58 C 0.1383(6) 0.45537(18) 0.3810(3) 0.0599(17) Uani 1 1 d . . . H58 H 0.0957 0.4603 0.3433 0.072 Uiso 1 1 calc R . . C59 C 0.1332(6) 0.47730(16) 0.4221(2) 0.0599(18) Uani 1 1 d . . . C60 C 0.0676(6) 0.50560(17) 0.4073(3) 0.0646(18) Uani 1 1 d . . . H60 H 0.0285 0.5103 0.3692 0.078 Uiso 1 1 calc R . . C61 C 0.0542(5) 0.52907(16) 0.4468(3) 0.0546(16) Uani 1 1 d . . . C62 C -0.0130(6) 0.55618(16) 0.4315(3) 0.0612(18) Uani 1 1 d . . . H62 H -0.0583 0.5601 0.3937 0.073 Uiso 1 1 calc R . . C63 C -0.0156(5) 0.57824(17) 0.4710(3) 0.0605(18) Uani 1 1 d . . . H63 H -0.0600 0.5982 0.4604 0.073 Uiso 1 1 calc R . . C64 C 0.0469(5) 0.57168(15) 0.5273(3) 0.0568(17) Uani 1 1 d . . . H64 H 0.0380 0.5856 0.5547 0.068 Uiso 1 1 calc R . . C65 C 0.1167(6) 0.54638(18) 0.5413(3) 0.070(2) Uani 1 1 d . . . H65 H 0.1623 0.5432 0.5792 0.084 Uiso 1 1 calc R . . C66 C 0.1283(6) 0.52280(16) 0.5021(3) 0.0642(19) Uani 1 1 d . . . C67 C 0.1961(5) 0.49422(15) 0.5171(2) 0.0488(14) Uani 1 1 d . . . C68 C 0.2717(6) 0.48730(15) 0.5793(2) 0.0544(16) Uani 1 1 d . . . H68A H 0.2810 0.4626 0.5854 0.065 Uiso 1 1 calc R . . H68B H 0.2327 0.4961 0.6024 0.065 Uiso 1 1 calc R . . C69 C 0.5895(5) 0.48819(18) 0.5817(3) 0.0565(16) Uani 1 1 d . . . H69A H 0.6314 0.4895 0.6221 0.068 Uiso 1 1 calc R . . H69B H 0.6086 0.5085 0.5652 0.068 Uiso 1 1 calc R . . C70 C 0.6254(5) 0.45725(16) 0.5602(2) 0.0513(15) Uani 1 1 d . . . H70A H 0.6007 0.4371 0.5741 0.077 Uiso 1 1 calc R . . H70B H 0.7081 0.4570 0.5726 0.077 Uiso 1 1 calc R . . H70C H 0.5909 0.4573 0.5199 0.077 Uiso 1 1 calc R . . C71 C 0.4151(5) 0.57269(15) 0.6121(3) 0.0589(16) Uani 1 1 d . . . H71A H 0.4569 0.5661 0.6510 0.071 Uiso 1 1 calc R . . H71B H 0.3412 0.5822 0.6087 0.071 Uiso 1 1 calc R . . C72 C 0.4841(6) 0.60028(16) 0.5961(3) 0.0608(16) Uani 1 1 d . . . H72A H 0.5581 0.5911 0.6004 0.091 Uiso 1 1 calc R . . H72B H 0.4950 0.6200 0.6201 0.091 Uiso 1 1 calc R . . H72C H 0.4425 0.6071 0.5577 0.091 Uiso 1 1 calc R . . C73 C 0.8675(6) 0.52279(16) 0.9890(3) 0.0625(17) Uani 1 1 d . . . C74 C 0.8655(6) 0.54623(14) 0.9487(3) 0.0603(17) Uani 1 1 d . . . H74 H 0.8166 0.5425 0.9114 0.072 Uiso 1 1 calc R . . C75 C 0.9311(6) 0.57358(17) 0.9621(3) 0.0646(18) Uani 1 1 d . . . H75 H 0.9316 0.5885 0.9339 0.078 Uiso 1 1 calc R . . C76 C 1.0000(5) 0.58070(16) 1.0174(2) 0.0612(17) Uani 1 1 d . . . H76 H 1.0449 0.6006 1.0273 0.073 Uiso 1 1 calc R . . C77 C 0.9999(5) 0.55768(15) 1.0571(3) 0.0591(17) Uani 1 1 d . . . H77 H 1.0476 0.5616 1.0945 0.071 Uiso 1 1 calc R . . C78 C 0.9343(6) 0.52997(15) 1.0440(3) 0.0607(17) Uani 1 1 d . . . C79 C 0.9341(5) 0.50762(16) 1.0855(3) 0.0565(15) Uani 1 1 d . . . H79 H 0.9830 0.5120 1.1226 0.068 Uiso 1 1 calc R . . C80 C 0.8631(5) 0.47888(14) 1.0735(3) 0.0569(16) Uani 1 1 d . . . C81 C 0.8712(5) 0.45599(14) 1.1149(2) 0.0565(17) Uani 1 1 d . . . H81 H 0.9218 0.4604 1.1517 0.068 Uiso 1 1 calc R . . C82 C 0.8068(5) 0.42707(16) 1.1031(3) 0.0644(18) Uani 1 1 d . . . H82 H 0.8094 0.4125 1.1322 0.077 Uiso 1 1 calc R . . C83 C 0.7363(5) 0.41872(15) 1.0480(2) 0.0517(14) Uani 1 1 d . . . H83 H 0.6950 0.3981 1.0394 0.062 Uiso 1 1 calc R . . C84 C 0.7298(5) 0.44134(15) 1.0075(3) 0.0572(16) Uani 1 1 d . . . H84 H 0.6779 0.4370 0.9710 0.069 Uiso 1 1 calc R . . C85 C 0.7960(6) 0.47027(16) 1.0180(3) 0.0637(18) Uani 1 1 d . . . C86 C 0.7958(6) 0.49436(15) 0.9755(3) 0.0620(18) Uani 1 1 d . . . C87 C 0.7187(5) 0.48481(14) 0.9143(2) 0.0509(14) Uani 1 1 d . . . H87A H 0.7135 0.4599 0.9106 0.061 Uiso 1 1 calc R . . H87B H 0.7542 0.4934 0.8895 0.061 Uiso 1 1 calc R . . C88 C 0.5182(5) 0.56767(15) 0.8871(3) 0.0557(15) Uani 1 1 d . . . H88A H 0.4401 0.5617 0.8827 0.067 Uiso 1 1 calc R . . H88B H 0.5180 0.5697 0.8497 0.067 Uiso 1 1 calc R . . C89 C 0.5435(7) 0.60196(16) 0.9131(3) 0.082(3) Uani 1 1 d . . . H89A H 0.5944 0.5997 0.9519 0.123 Uiso 1 1 calc R . . H89B H 0.4728 0.6127 0.9105 0.123 Uiso 1 1 calc R . . H89C H 0.5799 0.6158 0.8939 0.123 Uiso 1 1 calc R . . C90 C 0.4020(5) 0.48222(15) 0.9161(2) 0.0496(14) Uani 1 1 d . . . H90A H 0.3585 0.4826 0.8758 0.060 Uiso 1 1 calc R . . H90B H 0.3817 0.5026 0.9322 0.060 Uiso 1 1 calc R . . C91 C 0.3729(5) 0.45059(17) 0.9405(3) 0.0641(17) Uani 1 1 d . . . H91A H 0.4352 0.4343 0.9495 0.096 Uiso 1 1 calc R . . H91B H 0.3034 0.4405 0.9136 0.096 Uiso 1 1 calc R . . H91C H 0.3612 0.4565 0.9739 0.096 Uiso 1 1 calc R . . C92 C 0.8597(5) 0.47759(16) 0.7447(3) 0.0574(15) Uani 1 1 d . . . C93 C 0.7619(5) 0.49772(16) 0.7526(3) 0.0581(16) Uani 1 1 d . . . C94 C 0.7680(5) 0.53128(15) 0.7563(2) 0.0466(13) Uani 1 1 d . . . H94 H 0.8292 0.5429 0.7524 0.056 Uiso 1 1 calc R . . C95 C 0.6868(5) 0.54871(14) 0.7658(2) 0.0467(13) Uani 1 1 d . . . C96 C 0.7007(6) 0.58755(16) 0.7742(3) 0.0626(17) Uani 1 1 d . . . C97 C 0.2071(5) 0.55992(14) 0.7302(2) 0.0508(14) Uani 1 1 d . . . C98 C 0.2588(5) 0.52418(16) 0.7365(3) 0.0557(15) Uani 1 1 d . . . C99 C 0.2054(5) 0.49731(15) 0.7482(2) 0.0534(15) Uani 1 1 d . . . H99 H 0.1376 0.5004 0.7542 0.064 Uiso 1 1 calc R . . C100 C 0.2519(5) 0.46546(14) 0.7513(2) 0.0494(13) Uani 1 1 d . . . C101 C 0.1867(5) 0.43548(16) 0.7650(3) 0.0570(15) Uani 1 1 d . . . C102 C 0.6347(5) 0.38496(17) 0.8470(3) 0.0625(17) Uani 1 1 d . . . C103 C 0.5766(5) 0.40665(15) 0.7949(2) 0.0498(13) Uani 1 1 d . . . C104 C 0.5341(5) 0.38957(15) 0.7429(2) 0.0499(14) Uani 1 1 d . . . H104 H 0.5390 0.3656 0.7415 0.060 Uiso 1 1 calc R . . C105 C 0.4864(5) 0.40773(15) 0.6948(2) 0.0511(14) Uani 1 1 d . . . C106 C 0.4330(5) 0.38645(15) 0.6411(2) 0.0549(15) 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 Dy1 0.04486(17) 0.05015(18) 0.04944(17) 0.00547(12) 0.01148(13) 0.00793(13) Dy2 0.04742(18) 0.04785(18) 0.05022(18) -0.00027(12) 0.00976(14) 0.00660(12) P1 0.0460(9) 0.0535(9) 0.0467(8) -0.0091(7) 0.0146(7) 0.0109(7) P2 0.0461(9) 0.0462(9) 0.0404(8) -0.0031(6) 0.0085(7) -0.0138(7) P3 0.0443(9) 0.0544(10) 0.0509(9) -0.0153(7) 0.0151(7) 0.0146(7) P4 0.0477(9) 0.0497(9) 0.0489(9) -0.0013(7) 0.0074(8) 0.0061(7) F1 0.064(2) 0.049(2) 0.054(2) 0.0140(15) 0.0153(18) 0.0229(17) F2 0.0385(19) 0.067(2) 0.056(2) 0.0081(17) 0.0065(17) 0.0193(16) F3 0.058(2) 0.058(2) 0.060(2) -0.0144(17) 0.0153(19) 0.0053(17) F4 0.049(2) 0.078(3) 0.054(2) -0.0050(18) 0.0140(18) 0.0050(18) F5 0.061(2) 0.065(2) 0.064(2) 0.0047(18) 0.0205(19) -0.0024(19) F6 0.058(2) 0.056(2) 0.091(3) -0.018(2) 0.009(2) -0.0206(18) F7 0.064(2) 0.069(3) 0.059(2) 0.0132(18) 0.015(2) 0.0127(19) F8 0.061(2) 0.051(2) 0.059(2) 0.0175(16) 0.0154(18) 0.0111(17) F9 0.052(2) 0.082(3) 0.047(2) -0.0126(18) 0.0016(18) -0.0038(19) F10 0.065(2) 0.057(2) 0.057(2) 0.0097(17) 0.0095(19) 0.0042(18) F11 0.056(2) 0.057(2) 0.051(2) -0.0014(16) 0.0159(18) 0.0128(17) F12 0.065(2) 0.048(2) 0.0368(17) -0.0014(14) 0.0013(16) 0.0032(17) F13 0.0452(19) 0.058(2) 0.0442(18) -0.0010(15) 0.0117(16) 0.0162(16) F14 0.048(2) 0.063(2) 0.0446(19) 0.0051(16) 0.0074(16) 0.0192(17) F15 0.049(2) 0.0452(19) 0.054(2) 0.0017(15) 0.0160(16) 0.0170(16) F16 0.061(2) 0.070(3) 0.071(3) -0.014(2) 0.024(2) 0.004(2) F17 0.052(2) 0.058(2) 0.069(2) -0.0084(18) 0.0118(19) -0.0091(18) F18 0.062(2) 0.058(2) 0.060(2) -0.0133(17) 0.011(2) 0.0038(18) F19 0.052(2) 0.060(2) 0.052(2) 0.0089(16) 0.0104(17) 0.0101(17) F20 0.049(2) 0.063(2) 0.057(2) 0.0162(17) 0.0125(17) 0.0040(17) F21 0.0416(19) 0.053(2) 0.076(2) 0.0028(17) 0.0101(18) -0.0031(16) F22 0.076(3) 0.044(2) 0.062(2) -0.0011(16) 0.001(2) -0.0101(18) F23 0.052(2) 0.048(2) 0.054(2) -0.0089(15) 0.0076(17) -0.0050(16) F24 0.064(2) 0.055(2) 0.068(2) -0.0145(18) -0.008(2) -0.0100(18) F25 0.0350(17) 0.058(2) 0.063(2) -0.0161(17) 0.0057(16) 0.0055(15) F26 0.0439(19) 0.044(2) 0.078(2) -0.0002(16) 0.0172(18) -0.0021(15) F27 0.051(2) 0.061(2) 0.061(2) 0.0027(17) 0.0141(18) -0.0014(17) F28 0.057(2) 0.083(3) 0.067(2) 0.004(2) 0.017(2) -0.011(2) F29 0.058(2) 0.053(2) 0.068(2) -0.0001(17) -0.0035(19) -0.0135(18) F30 0.054(2) 0.091(3) 0.055(2) 0.003(2) -0.0011(18) -0.021(2) F31 0.060(2) 0.070(3) 0.074(3) 0.023(2) 0.019(2) 0.018(2) F32 0.063(2) 0.060(2) 0.055(2) 0.0057(17) 0.0009(19) -0.0038(18) F33 0.064(2) 0.054(2) 0.055(2) -0.0038(16) 0.0128(19) -0.0013(18) F34 0.065(2) 0.052(2) 0.053(2) 0.0027(16) 0.0145(18) 0.0015(17) F35 0.056(2) 0.066(2) 0.050(2) -0.0048(17) 0.0059(18) -0.0028(18) F36 0.050(2) 0.072(2) 0.059(2) -0.0089(18) 0.0058(18) 0.0031(18) O1 0.043(2) 0.054(2) 0.042(2) -0.0024(18) 0.0022(18) 0.0058(19) O1W 0.044(2) 0.045(2) 0.066(3) 0.0024(19) -0.004(2) 0.0005(18) O2 0.062(3) 0.053(3) 0.058(3) -0.009(2) 0.020(2) 0.008(2) O3 0.048(2) 0.048(2) 0.049(2) -0.0118(18) 0.009(2) 0.0062(18) O4 0.048(2) 0.046(2) 0.037(2) 0.0006(17) 0.0053(18) 0.0052(18) O5 0.038(2) 0.065(3) 0.051(2) -0.015(2) 0.0094(19) -0.0082(19) O6 0.054(2) 0.048(2) 0.040(2) 0.0059(17) 0.0114(19) -0.0074(19) O7 0.052(3) 0.050(2) 0.047(2) -0.0066(18) 0.007(2) -0.0081(19) O8 0.051(2) 0.056(3) 0.042(2) 0.0022(18) 0.0153(19) -0.0076(19) O9 0.043(2) 0.057(3) 0.052(2) 0.009(2) 0.000(2) -0.0001(19) O10 0.042(2) 0.049(2) 0.045(2) 0.0019(17) 0.0046(18) -0.0009(18) O11 0.044(2) 0.046(2) 0.058(2) -0.0130(19) 0.008(2) 0.0096(18) O12 0.049(2) 0.051(3) 0.048(2) 0.0006(18) -0.002(2) 0.0105(19) O13 0.029(2) 0.044(2) 0.056(2) 0.0003(17) 0.0001(18) 0.0021(16) O14 0.041(2) 0.045(2) 0.048(2) 0.0065(17) 0.0067(19) 0.0031(17) O15 0.034(2) 0.055(2) 0.0367(19) -0.0003(17) 0.0032(17) 0.0057(17) O16 0.043(2) 0.049(2) 0.042(2) 0.0015(17) -0.0024(18) 0.0096(18) O17 0.049(3) 0.051(2) 0.045(2) 0.0105(18) 0.0105(19) 0.0132(19) O18 0.036(2) 0.047(2) 0.053(2) 0.0061(18) 0.0082(19) 0.0070(18) O19 0.041(2) 0.043(2) 0.055(2) -0.0013(17) 0.0109(19) -0.0034(17) O20 0.040(2) 0.057(3) 0.049(2) -0.0050(19) 0.0110(19) 0.0037(18) O21 0.047(2) 0.045(2) 0.050(2) 0.0062(18) -0.0003(19) 0.0071(18) O22 0.039(2) 0.042(2) 0.051(2) -0.0001(17) 0.0015(18) 0.0068(17) O23 0.034(2) 0.049(2) 0.053(2) 0.0013(18) 0.0092(18) 0.0054(17) O24 0.042(2) 0.044(2) 0.039(2) 0.0003(16) 0.0031(18) 0.0061(17) C1 0.053(4) 0.053(4) 0.047(3) 0.017(3) -0.015(3) -0.004(3) C2 0.070(4) 0.042(3) 0.053(4) 0.001(3) 0.006(3) 0.012(3) C3 0.082(5) 0.046(4) 0.052(4) -0.010(3) 0.012(4) 0.003(3) C4 0.058(4) 0.059(4) 0.063(4) -0.022(3) 0.023(4) 0.001(3) C5 0.048(4) 0.074(5) 0.050(4) -0.002(3) -0.022(3) 0.009(3) C6 0.031(3) 0.085(5) 0.041(3) -0.009(3) 0.009(3) -0.001(3) C7 0.045(4) 0.063(4) 0.033(3) -0.009(3) -0.012(3) 0.010(3) C8 0.063(4) 0.039(3) 0.045(3) -0.007(3) 0.015(3) 0.027(3) C9 0.047(4) 0.071(5) 0.039(3) -0.010(3) -0.010(3) 0.006(3) C10 0.056(4) 0.079(5) 0.040(3) -0.007(3) 0.021(3) 0.012(3) C11 0.061(4) 0.054(4) 0.046(3) -0.012(3) 0.017(3) -0.005(3) C12 0.064(4) 0.057(4) 0.051(4) -0.006(3) 0.001(3) 0.000(3) C13 0.056(4) 0.070(5) 0.046(3) -0.018(3) 0.011(3) -0.002(3) C14 0.060(4) 0.044(3) 0.040(3) 0.000(3) -0.001(3) 0.014(3) C15 0.042(3) 0.041(3) 0.046(3) -0.006(2) 0.001(3) 0.004(3) C16 0.062(4) 0.053(4) 0.061(4) -0.004(3) 0.023(3) 0.001(3) C17 0.067(4) 0.048(4) 0.037(3) -0.004(3) -0.014(3) 0.015(3) C18 0.039(3) 0.091(5) 0.047(3) 0.012(3) 0.002(3) -0.010(3) C19 0.046(4) 0.066(4) 0.048(4) 0.007(3) 0.009(3) 0.006(3) C20 0.057(4) 0.046(3) 0.046(3) 0.006(3) 0.017(3) -0.004(3) C21 0.065(4) 0.034(3) 0.035(3) 0.008(2) 0.008(3) -0.009(3) C22 0.051(4) 0.044(4) 0.063(4) 0.009(3) 0.012(3) 0.006(3) C23 0.029(3) 0.067(4) 0.060(4) 0.006(3) 0.008(3) 0.006(3) C24 0.060(4) 0.044(4) 0.047(3) 0.014(3) 0.006(3) 0.003(3) C25 0.043(4) 0.072(5) 0.057(4) 0.003(3) 0.007(3) 0.019(3) C26 0.046(4) 0.056(4) 0.058(4) -0.007(3) -0.007(3) 0.009(3) C27 0.056(4) 0.056(4) 0.027(3) 0.003(2) 0.007(3) -0.008(3) C28 0.049(3) 0.048(3) 0.043(3) 0.001(3) 0.007(3) -0.009(3) C29 0.034(3) 0.050(4) 0.056(4) -0.007(3) -0.008(3) -0.009(3) C30 0.032(3) 0.061(4) 0.062(4) -0.005(3) 0.002(3) 0.006(3) C31 0.059(4) 0.038(3) 0.045(3) 0.005(2) 0.006(3) -0.009(3) C32 0.058(4) 0.058(4) 0.048(4) -0.002(3) -0.001(3) 0.005(3) C33 0.067(4) 0.041(3) 0.036(3) -0.001(2) 0.001(3) -0.005(3) C34 0.042(3) 0.058(4) 0.029(3) 0.000(2) 0.006(2) -0.015(3) C35 0.049(4) 0.075(5) 0.045(3) -0.010(3) 0.006(3) -0.004(3) C36 0.037(3) 0.028(3) 0.074(4) -0.002(3) 0.015(3) -0.009(2) C37 0.049(4) 0.050(4) 0.052(4) 0.010(3) 0.004(3) 0.012(3) C38 0.039(3) 0.043(3) 0.087(5) -0.003(3) 0.016(3) -0.009(3) C39 0.032(3) 0.087(5) 0.051(4) 0.017(3) 0.002(3) 0.022(3) C40 0.040(4) 0.058(4) 0.051(4) 0.015(3) -0.004(3) 0.012(3) C41 0.043(4) 0.076(5) 0.067(4) 0.008(3) 0.024(3) 0.023(3) C42 0.042(3) 0.049(4) 0.055(4) -0.015(3) 0.016(3) -0.007(3) C43 0.038(3) 0.057(4) 0.091(5) -0.012(4) 0.020(4) -0.013(3) C44 0.043(4) 0.056(4) 0.066(4) 0.010(3) 0.020(3) 0.006(3) C45 0.056(4) 0.038(3) 0.047(3) -0.002(2) 0.005(3) -0.007(3) C46 0.039(3) 0.042(3) 0.058(3) -0.003(3) 0.011(3) 0.002(2) C47 0.045(3) 0.056(4) 0.055(4) 0.000(3) 0.011(3) 0.025(3) C48 0.053(4) 0.049(4) 0.060(4) -0.001(3) 0.012(3) 0.012(3) C49 0.023(3) 0.081(5) 0.045(3) -0.003(3) 0.000(3) 0.005(3) C50 0.028(3) 0.051(3) 0.041(3) -0.012(2) 0.001(2) 0.001(2) C51 0.037(3) 0.055(4) 0.056(4) -0.001(3) 0.018(3) -0.011(3) C52 0.048(4) 0.061(4) 0.054(4) -0.017(3) 0.005(3) 0.000(3) C53 0.040(4) 0.056(4) 0.079(5) -0.005(3) 0.013(4) -0.010(3) C54 0.049(4) 0.034(3) 0.049(3) -0.006(2) -0.006(3) -0.011(3) C55 0.051(4) 0.049(4) 0.062(4) 0.006(3) 0.010(3) 0.013(3) C56 0.056(4) 0.055(4) 0.067(4) 0.005(3) 0.031(4) -0.002(3) C57 0.042(3) 0.071(4) 0.051(4) -0.004(3) 0.026(3) -0.001(3) C58 0.056(4) 0.074(5) 0.042(3) 0.002(3) 0.010(3) -0.013(3) C59 0.063(4) 0.050(4) 0.039(3) -0.003(3) -0.010(3) -0.001(3) C60 0.061(4) 0.059(4) 0.058(4) -0.012(3) 0.006(3) -0.001(3) C61 0.036(3) 0.049(4) 0.064(4) 0.005(3) 0.004(3) -0.004(3) C62 0.070(5) 0.044(4) 0.050(4) 0.008(3) 0.002(3) -0.007(3) C63 0.035(3) 0.051(4) 0.078(5) 0.004(3) 0.003(3) 0.008(3) C64 0.047(4) 0.041(3) 0.066(4) -0.006(3) 0.004(3) -0.012(3) C65 0.054(4) 0.066(5) 0.069(4) -0.006(4) 0.002(4) 0.016(3) C66 0.058(4) 0.046(4) 0.058(4) -0.003(3) -0.010(3) -0.003(3) C67 0.045(3) 0.047(3) 0.052(3) 0.007(3) 0.016(3) -0.001(3) C68 0.059(4) 0.040(3) 0.047(3) 0.016(3) 0.004(3) 0.002(3) C69 0.037(3) 0.072(4) 0.059(4) 0.005(3) 0.017(3) -0.007(3) C70 0.043(3) 0.063(4) 0.053(3) 0.010(3) 0.025(3) -0.011(3) C71 0.039(3) 0.053(4) 0.077(4) 0.017(3) 0.014(3) 0.015(3) C72 0.057(4) 0.049(4) 0.075(4) 0.008(3) 0.025(3) -0.001(3) C73 0.058(4) 0.060(4) 0.048(3) -0.017(3) -0.002(3) -0.002(3) C74 0.076(5) 0.037(3) 0.053(4) -0.010(3) 0.009(3) -0.006(3) C75 0.062(4) 0.061(4) 0.051(3) 0.007(3) 0.000(3) 0.007(3) C76 0.053(4) 0.051(3) 0.055(4) 0.006(3) -0.007(3) 0.007(3) C77 0.044(3) 0.051(4) 0.057(4) -0.007(3) -0.009(3) 0.002(3) C78 0.063(4) 0.042(3) 0.055(4) -0.005(3) -0.001(3) 0.016(3) C79 0.042(3) 0.067(4) 0.049(3) -0.003(3) 0.006(3) 0.000(3) C80 0.059(4) 0.038(3) 0.056(4) -0.003(3) 0.003(3) 0.008(3) C81 0.038(3) 0.048(3) 0.050(3) -0.001(3) -0.019(3) 0.014(3) C82 0.043(3) 0.053(4) 0.074(4) -0.009(3) -0.002(3) -0.001(3) C83 0.049(3) 0.045(3) 0.064(4) -0.014(3) 0.025(3) 0.004(3) C84 0.053(4) 0.045(3) 0.055(4) -0.006(3) 0.002(3) 0.007(3) C85 0.059(4) 0.047(4) 0.061(4) 0.000(3) -0.002(3) 0.006(3) C86 0.063(4) 0.040(3) 0.054(4) -0.011(3) -0.009(3) 0.002(3) C87 0.034(3) 0.044(3) 0.058(4) -0.005(3) 0.000(3) 0.007(2) C88 0.044(3) 0.057(4) 0.061(4) -0.012(3) 0.016(3) 0.002(3) C89 0.089(6) 0.046(4) 0.069(4) -0.003(3) -0.015(4) 0.014(4) C90 0.045(3) 0.055(4) 0.048(3) -0.006(2) 0.017(3) 0.023(3) C91 0.047(4) 0.076(5) 0.062(4) -0.006(3) 0.013(3) -0.011(3) C92 0.054(4) 0.052(4) 0.061(4) -0.001(3) 0.017(3) -0.001(3) C93 0.050(4) 0.047(3) 0.063(4) -0.003(3) 0.007(3) -0.011(3) C94 0.044(3) 0.053(3) 0.043(3) 0.005(2) 0.018(3) -0.004(3) C95 0.062(4) 0.051(3) 0.029(3) -0.011(2) 0.020(3) -0.014(3) C96 0.068(4) 0.055(4) 0.051(3) -0.001(3) 0.008(3) -0.009(3) C97 0.046(3) 0.043(3) 0.051(3) -0.002(2) 0.005(3) -0.006(2) C98 0.043(3) 0.050(4) 0.065(4) -0.004(3) 0.011(3) 0.003(3) C99 0.048(3) 0.057(4) 0.037(3) -0.005(2) -0.003(3) -0.002(3) C100 0.044(3) 0.047(3) 0.054(3) 0.003(2) 0.015(3) 0.007(3) C101 0.047(3) 0.060(4) 0.057(4) 0.009(3) 0.013(3) 0.011(3) C102 0.046(4) 0.059(4) 0.059(4) 0.004(3) -0.005(3) -0.012(3) C103 0.042(3) 0.057(4) 0.039(3) 0.009(2) 0.004(2) 0.006(3) C104 0.041(3) 0.049(3) 0.054(3) -0.002(3) 0.012(3) 0.013(3) C105 0.033(3) 0.056(4) 0.057(3) -0.003(3) 0.008(3) 0.006(2) C106 0.056(4) 0.046(3) 0.055(3) -0.002(3) 0.013(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O4 2.280(4) . ? Dy1 O1 2.285(4) . ? Dy1 O13 2.334(4) . ? Dy1 O17 2.339(4) . ? Dy1 O14 2.346(4) . ? Dy1 O16 2.357(4) . ? Dy1 O18 2.377(4) . ? Dy1 O15 2.392(4) . ? Dy2 O7 2.284(4) . ? Dy2 O10 2.308(4) . ? Dy2 O19 2.328(4) . ? Dy2 O22 2.340(4) . ? Dy2 O24 2.347(4) . ? Dy2 O23 2.360(4) . ? Dy2 O21 2.392(4) . ? Dy2 O20 2.432(4) . ? P1 O1 1.473(4) . ? P1 O2 1.556(5) . ? P1 O3 1.559(5) . ? P1 C15 1.805(6) . ? P2 O4 1.480(4) . ? P2 O5 1.503(4) . ? P2 O6 1.579(4) . ? P2 C34 1.802(6) . ? P3 O10 1.473(4) . ? P3 O11 1.557(4) . ? P3 O12 1.582(5) . ? P3 C87 1.815(5) . ? P4 O7 1.489(4) . ? P4 O8 1.521(5) . ? P4 O9 1.553(4) . ? P4 C68 1.802(7) . ? F1 C39 1.295(7) . ? F2 C39 1.293(8) . ? F3 C39 1.363(7) . ? F4 C43 1.312(8) . ? F5 C43 1.353(8) . ? F6 C43 1.350(7) . ? F7 C44 1.412(7) . ? F8 C44 1.332(7) . ? F9 C44 1.335(7) . ? F10 C48 1.290(7) . ? F11 C48 1.298(8) . ? F12 C48 1.359(7) . ? F13 C49 1.315(7) . ? F14 C49 1.293(7) . ? F15 C49 1.318(7) . ? F16 C53 1.298(8) . ? F17 C53 1.341(8) . ? F18 C53 1.323(8) . ? F19 C92 1.319(6) . ? F20 C92 1.295(6) . ? F21 C92 1.324(6) . ? F22 C96 1.338(7) . ? F23 C96 1.311(6) . ? F24 C96 1.329(7) . ? F25 C97 1.317(5) . ? F26 C97 1.339(6) . ? F27 C97 1.320(6) . ? F28 C101 1.293(7) . ? F29 C101 1.330(6) . ? F30 C101 1.357(6) . ? F31 C102 1.338(7) . ? F32 C102 1.310(6) . ? F33 C102 1.362(7) . ? F34 C106 1.329(6) . ? F35 C106 1.338(7) . ? F36 C106 1.288(6) . ? O1W H1X 0.8500 . ? O1W H1Y 0.8499 . ? O2 C16 1.379(8) . ? O3 C18 1.423(8) . ? O5 C35 1.469(8) . ? O6 C37 1.423(7) . ? O8 C69 1.453(7) . ? O9 C71 1.441(7) . ? O11 C88 1.431(6) . ? O12 C90 1.430(6) . ? O13 C40 1.239(8) . ? O14 C42 1.294(7) . ? O15 C45 1.259(7) . ? O16 C47 1.242(7) . ? O17 C50 1.263(7) . ? O18 C52 1.245(8) . ? O19 C93 1.253(6) . ? O20 C95 1.245(6) . ? O21 C98 1.238(6) . ? O22 C100 1.218(6) . ? O23 C103 1.235(6) . ? O24 C105 1.232(6) . ? C1 C6 1.387(8) . ? C1 C2 1.419(9) . ? C1 C14 1.478(9) . ? C2 C3 1.354(10) . ? C2 H2 0.9500 . ? C3 C4 1.332(9) . ? C3 H3 0.9500 . ? C4 C5 1.431(10) . ? C4 H4 0.9500 . ? C5 C6 1.380(10) . ? C5 H5 0.9500 . ? C6 C7 1.418(9) . ? C7 C8 1.405(9) . ? C7 H7 0.9500 . ? C8 C9 1.395(9) . ? C8 C13 1.410(8) . ? C9 C10 1.362(10) . ? C9 H9 0.9500 . ? C10 C11 1.383(8) . ? C10 H10 0.9500 . ? C11 C12 1.382(9) . ? C11 H11 0.9500 . ? C12 C13 1.413(10) . ? C12 H12 0.9500 . ? C13 C14 1.370(9) . ? C14 C15 1.590(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.518(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.545(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.391(9) . ? C20 C21 1.425(8) . ? C20 C33 1.434(9) . ? C21 C22 1.321(8) . ? C21 H21 0.9500 . ? C22 C23 1.399(8) . ? C22 H22 0.9500 . ? C23 C24 1.399(9) . ? C23 H23 0.9500 . ? C24 C25 1.346(9) . ? C24 H24 0.9500 . ? C25 C26 1.419(9) . ? C26 C27 1.388(9) . ? C26 H26 0.9500 . ? C27 C28 1.389(8) . ? C27 C32 1.425(8) . ? C28 C29 1.325(8) . ? C28 H28 0.9500 . ? C29 C30 1.425(9) . ? C29 H29 0.9500 . ? C30 C31 1.381(9) . ? C30 H30 0.9500 . ? C31 C32 1.397(9) . ? C31 H31 0.9500 . ? C32 C33 1.392(9) . ? C33 C34 1.595(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.536(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.495(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.521(9) . ? C40 C41 1.452(10) . ? C41 C42 1.348(9) . ? C41 H41 0.9500 . ? C42 C43 1.513(9) . ? C44 C45 1.501(8) . ? C45 C46 1.377(8) . ? C46 C47 1.403(8) . ? C46 H46 0.9500 . ? C47 C48 1.528(9) . ? C49 C50 1.524(8) . ? C50 C51 1.382(8) . ? C51 C52 1.403(9) . ? C51 H51 0.9500 . ? C52 C53 1.516(9) . ? C54 C55 1.382(8) . ? C54 C59 1.392(8) . ? C54 C67 1.451(9) . ? C55 C56 1.335(9) . ? C55 H55 0.9500 . ? C56 C57 1.410(9) . ? C56 H56 0.9500 . ? C57 C58 1.354(9) . ? C57 H57 0.9500 . ? C58 C59 1.410(9) . ? C58 H58 0.9500 . ? C59 C60 1.363(9) . ? C60 C61 1.455(9) . ? C60 H60 0.9500 . ? C61 C62 1.336(9) . ? C61 C66 1.418(9) . ? C62 C63 1.371(9) . ? C62 H62 0.9500 . ? C63 C64 1.410(9) . ? C63 H63 0.9500 . ? C64 C65 1.296(9) . ? C64 H64 0.9500 . ? C65 C66 1.444(10) . ? C65 H65 0.9500 . ? C66 C67 1.386(9) . ? C67 C68 1.571(8) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.495(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.564(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C78 1.397(8) . ? C73 C74 1.403(9) . ? C73 C86 1.407(9) . ? C74 C75 1.331(9) . ? C74 H74 0.9500 . ? C75 C76 1.410(8) . ? C75 H75 0.9500 . ? C76 C77 1.387(9) . ? C76 H76 0.9500 . ? C77 C78 1.342(9) . ? C77 H77 0.9500 . ? C78 C79 1.409(9) . ? C79 C80 1.413(9) . ? C79 H79 0.9500 . ? C80 C81 1.392(9) . ? C80 C85 1.421(8) . ? C81 C82 1.374(9) . ? C81 H81 0.9500 . ? C82 C83 1.420(8) . ? C82 H82 0.9500 . ? C83 C84 1.370(8) . ? C83 H83 0.9500 . ? C84 C85 1.387(9) . ? C84 H84 0.9500 . ? C85 C86 1.469(9) . ? C86 C87 1.577(8) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.497(8) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 C91 1.518(9) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 C93 1.566(9) . ? C93 C94 1.331(8) . ? C94 C95 1.349(8) . ? C94 H94 0.9500 . ? C95 C96 1.553(8) . ? C97 C98 1.543(8) . ? C98 C99 1.363(9) . ? C99 C100 1.383(8) . ? C99 H99 0.9500 . ? C100 C101 1.573(9) . ? C102 C103 1.543(8) . ? C103 C104 1.434(8) . ? C104 C105 1.376(8) . ? C104 H104 0.9500 . ? C105 C106 1.559(8) . ? 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 O4 Dy1 O1 145.96(15) . . ? O4 Dy1 O13 75.54(15) . . ? O1 Dy1 O13 78.75(14) . . ? O4 Dy1 O17 81.37(14) . . ? O1 Dy1 O17 107.84(14) . . ? O13 Dy1 O17 143.36(14) . . ? O4 Dy1 O14 110.17(14) . . ? O1 Dy1 O14 83.42(15) . . ? O13 Dy1 O14 74.29(14) . . ? O17 Dy1 O14 141.35(14) . . ? O4 Dy1 O16 71.75(14) . . ? O1 Dy1 O16 141.19(15) . . ? O13 Dy1 O16 117.31(13) . . ? O17 Dy1 O16 80.67(15) . . ? O14 Dy1 O16 69.31(15) . . ? O4 Dy1 O18 78.02(14) . . ? O1 Dy1 O18 74.83(15) . . ? O13 Dy1 O18 77.27(13) . . ? O17 Dy1 O18 70.31(14) . . ? O14 Dy1 O18 146.98(14) . . ? O16 Dy1 O18 140.69(15) . . ? O4 Dy1 O15 139.34(14) . . ? O1 Dy1 O15 73.46(13) . . ? O13 Dy1 O15 140.48(14) . . ? O17 Dy1 O15 73.26(13) . . ? O14 Dy1 O15 75.09(13) . . ? O16 Dy1 O15 73.16(13) . . ? O18 Dy1 O15 120.29(13) . . ? O7 Dy2 O10 144.62(15) . . ? O7 Dy2 O19 82.91(15) . . ? O10 Dy2 O19 106.73(14) . . ? O7 Dy2 O22 111.54(14) . . ? O10 Dy2 O22 80.19(14) . . ? O19 Dy2 O22 145.14(13) . . ? O7 Dy2 O24 72.55(14) . . ? O10 Dy2 O24 141.54(14) . . ? O19 Dy2 O24 82.02(14) . . ? O22 Dy2 O24 73.22(14) . . ? O7 Dy2 O23 140.48(15) . . ? O10 Dy2 O23 73.63(14) . . ? O19 Dy2 O23 72.62(14) . . ? O22 Dy2 O23 77.04(13) . . ? O24 Dy2 O23 73.67(13) . . ? O7 Dy2 O21 75.31(15) . . ? O10 Dy2 O21 78.08(14) . . ? O19 Dy2 O21 144.28(14) . . ? O22 Dy2 O21 70.29(14) . . ? O24 Dy2 O21 116.72(13) . . ? O23 Dy2 O21 139.71(15) . . ? O7 Dy2 O20 77.07(14) . . ? O10 Dy2 O20 74.68(14) . . ? O19 Dy2 O20 70.31(13) . . ? O22 Dy2 O20 142.36(14) . . ? O24 Dy2 O20 140.97(14) . . ? O23 Dy2 O20 120.55(13) . . ? O21 Dy2 O20 77.36(13) . . ? O1 P1 O2 112.5(2) . . ? O1 P1 O3 111.9(3) . . ? O2 P1 O3 107.7(2) . . ? O1 P1 C15 112.1(3) . . ? O2 P1 C15 108.2(3) . . ? O3 P1 C15 103.9(3) . . ? O4 P2 O5 113.2(2) . . ? O4 P2 O6 112.2(2) . . ? O5 P2 O6 105.2(2) . . ? O4 P2 C34 113.0(3) . . ? O5 P2 C34 104.8(3) . . ? O6 P2 C34 107.7(3) . . ? O10 P3 O11 113.1(2) . . ? O10 P3 O12 111.5(2) . . ? O11 P3 O12 106.7(2) . . ? O10 P3 C87 112.58(19) . . ? O11 P3 C87 107.53(18) . . ? O12 P3 C87 105.0(2) . . ? O7 P4 O8 114.4(3) . . ? O7 P4 O9 112.6(2) . . ? O8 P4 O9 104.4(3) . . ? O7 P4 C68 111.0(3) . . ? O8 P4 C68 104.8(3) . . ? O9 P4 C68 109.0(3) . . ? P1 O1 Dy1 153.4(3) . . ? H1X O1W H1Y 109.5 . . ? C16 O2 P1 126.6(4) . . ? C18 O3 P1 125.9(4) . . ? P2 O4 Dy1 150.8(3) . . ? C35 O5 P2 126.0(4) . . ? C37 O6 P2 124.5(3) . . ? P4 O7 Dy2 153.1(3) . . ? C69 O8 P4 125.4(4) . . ? C71 O9 P4 122.9(3) . . ? P3 O10 Dy2 150.3(3) . . ? C88 O11 P3 127.5(3) . . ? C90 O12 P3 124.1(3) . . ? C40 O13 Dy1 135.4(4) . . ? C42 O14 Dy1 124.3(4) . . ? C45 O15 Dy1 132.3(3) . . ? C47 O16 Dy1 134.4(4) . . ? C50 O17 Dy1 137.8(4) . . ? C52 O18 Dy1 134.1(4) . . ? C93 O19 Dy2 136.4(3) . . ? C95 O20 Dy2 131.7(3) . . ? C98 O21 Dy2 133.7(3) . . ? C100 O22 Dy2 134.1(3) . . ? C103 O23 Dy2 134.2(3) . . ? C105 O24 Dy2 133.6(3) . . ? C6 C1 C2 118.2(6) . . ? C6 C1 C14 116.0(6) . . ? C2 C1 C14 125.9(6) . . ? C3 C2 C1 120.6(6) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 120.6(7) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 122.1(7) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 116.8(6) . . ? C6 C5 H5 121.6 . . ? C4 C5 H5 121.6 . . ? C5 C6 C1 121.7(6) . . ? C5 C6 C7 117.9(6) . . ? C1 C6 C7 120.4(6) . . ? C8 C7 C6 122.9(5) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C9 C8 C7 120.9(6) . . ? C9 C8 C13 121.3(6) . . ? C7 C8 C13 117.6(6) . . ? C10 C9 C8 116.9(6) . . ? C10 C9 H9 121.6 . . ? C8 C9 H9 121.6 . . ? C9 C10 C11 126.0(7) . . ? C9 C10 H10 117.0 . . ? C11 C10 H10 117.0 . . ? C12 C11 C10 115.7(6) . . ? C12 C11 H11 122.2 . . ? C10 C11 H11 122.2 . . ? C11 C12 C13 122.7(6) . . ? C11 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C14 C13 C8 120.3(6) . . ? C14 C13 C12 122.4(6) . . ? C8 C13 C12 117.4(7) . . ? C13 C14 C1 122.8(6) . . ? C13 C14 C15 121.7(6) . . ? C1 C14 C15 115.5(5) . . ? C14 C15 P1 112.8(4) . . ? C14 C15 H15A 109.0 . . ? P1 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? P1 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? O2 C16 C17 120.0(5) . . ? O2 C16 H16A 107.3 . . ? C17 C16 H16A 107.3 . . ? O2 C16 H16B 107.3 . . ? C17 C16 H16B 107.3 . . ? H16A C16 H16B 106.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 C19 118.2(5) . . ? O3 C18 H18A 107.8 . . ? C19 C18 H18A 107.8 . . ? O3 C18 H18B 107.8 . . ? C19 C18 H18B 107.8 . . ? H18A C18 H18B 107.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 116.8(6) . . ? C25 C20 C33 118.5(6) . . ? C21 C20 C33 124.7(5) . . ? C22 C21 C20 122.0(6) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C25 C24 C23 120.2(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 121.7(6) . . ? C24 C25 C26 118.0(6) . . ? C20 C25 C26 120.2(6) . . ? C27 C26 C25 120.7(6) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 121.2(5) . . ? C26 C27 C32 120.3(6) . . ? C28 C27 C32 118.5(6) . . ? C29 C28 C27 122.8(6) . . ? C29 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C28 C29 C30 121.1(6) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 116.8(6) . . ? C31 C30 H30 121.6 . . ? C29 C30 H30 121.6 . . ? C30 C31 C32 123.2(6) . . ? C30 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C33 C32 C31 123.9(6) . . ? C33 C32 C27 118.5(6) . . ? C31 C32 C27 117.6(6) . . ? C32 C33 C20 121.7(5) . . ? C32 C33 C34 120.2(6) . . ? C20 C33 C34 118.0(5) . . ? C33 C34 P2 112.6(4) . . ? C33 C34 H34A 109.1 . . ? P2 C34 H34A 109.1 . . ? C33 C34 H34B 109.1 . . ? P2 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? O5 C35 C36 112.1(5) . . ? O5 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? O5 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6 C37 C38 117.0(5) . . ? O6 C37 H37A 108.1 . . ? C38 C37 H37A 108.1 . . ? O6 C37 H37B 108.1 . . ? C38 C37 H37B 108.1 . . ? H37A C37 H37B 107.3 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F2 C39 F1 113.7(6) . . ? F2 C39 F3 101.4(5) . . ? F1 C39 F3 105.6(5) . . ? F2 C39 C40 108.5(5) . . ? F1 C39 C40 113.5(6) . . ? F3 C39 C40 113.7(6) . . ? O13 C40 C41 122.9(6) . . ? O13 C40 C39 119.2(6) . . ? C41 C40 C39 117.8(6) . . ? C42 C41 C40 120.5(6) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? O14 C42 C41 134.0(6) . . ? O14 C42 C43 122.8(6) . . ? C41 C42 C43 103.2(6) . . ? F4 C43 F6 102.4(5) . . ? F4 C43 F5 126.0(7) . . ? F6 C43 F5 99.3(5) . . ? F4 C43 C42 109.0(5) . . ? F6 C43 C42 110.2(6) . . ? F5 C43 C42 108.6(5) . . ? F8 C44 F9 108.5(5) . . ? F8 C44 F7 108.9(5) . . ? F9 C44 F7 109.0(5) . . ? F8 C44 C45 116.3(6) . . ? F9 C44 C45 111.3(5) . . ? F7 C44 C45 102.6(5) . . ? O15 C45 C46 129.7(6) . . ? O15 C45 C44 111.6(5) . . ? C46 C45 C44 118.3(6) . . ? C45 C46 C47 120.2(6) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? O16 C47 C46 129.3(6) . . ? O16 C47 C48 114.6(5) . . ? C46 C47 C48 115.9(6) . . ? F10 C48 F11 110.9(5) . . ? F10 C48 F12 108.4(5) . . ? F11 C48 F12 97.2(5) . . ? F10 C48 C47 120.1(6) . . ? F11 C48 C47 111.8(6) . . ? F12 C48 C47 105.8(5) . . ? F14 C49 F13 111.9(6) . . ? F14 C49 F15 108.0(5) . . ? F13 C49 F15 111.1(5) . . ? F14 C49 C50 112.1(5) . . ? F13 C49 C50 107.9(5) . . ? F15 C49 C50 105.6(5) . . ? O17 C50 C51 126.4(6) . . ? O17 C50 C49 113.8(5) . . ? C51 C50 C49 119.7(6) . . ? C50 C51 C52 118.6(6) . . ? C50 C51 H51 120.7 . . ? C52 C51 H51 120.7 . . ? O18 C52 C51 129.6(6) . . ? O18 C52 C53 116.8(6) . . ? C51 C52 C53 113.6(6) . . ? F16 C53 F18 105.3(5) . . ? F16 C53 F17 109.1(6) . . ? F18 C53 F17 106.9(6) . . ? F16 C53 C52 112.8(6) . . ? F18 C53 C52 109.1(6) . . ? F17 C53 C52 113.1(5) . . ? C55 C54 C59 119.9(6) . . ? C55 C54 C67 124.1(6) . . ? C59 C54 C67 115.9(6) . . ? C56 C55 C54 121.8(6) . . ? C56 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? C55 C56 C57 119.1(6) . . ? C55 C56 H56 120.5 . . ? C57 C56 H56 120.5 . . ? C58 C57 C56 120.5(6) . . ? C58 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C57 C58 C59 120.3(6) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C60 C59 C54 122.1(6) . . ? C60 C59 C58 119.6(6) . . ? C54 C59 C58 118.2(6) . . ? C59 C60 C61 123.4(6) . . ? C59 C60 H60 118.3 . . ? C61 C60 H60 118.3 . . ? C62 C61 C66 123.1(7) . . ? C62 C61 C60 122.5(6) . . ? C66 C61 C60 114.0(6) . . ? C61 C62 C63 119.0(6) . . ? C61 C62 H62 120.5 . . ? C63 C62 H62 120.5 . . ? C62 C63 C64 120.8(6) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C65 C64 C63 119.2(7) . . ? C65 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C64 C65 C66 123.2(7) . . ? C64 C65 H65 118.4 . . ? C66 C65 H65 118.4 . . ? C67 C66 C61 122.1(6) . . ? C67 C66 C65 123.4(6) . . ? C61 C66 C65 114.2(6) . . ? C66 C67 C54 121.9(6) . . ? C66 C67 C68 120.3(6) . . ? C54 C67 C68 117.8(5) . . ? C67 C68 P4 112.5(4) . . ? C67 C68 H68A 109.1 . . ? P4 C68 H68A 109.1 . . ? C67 C68 H68B 109.1 . . ? P4 C68 H68B 109.1 . . ? H68A C68 H68B 107.8 . . ? O8 C69 C70 111.1(5) . . ? O8 C69 H69A 109.4 . . ? C70 C69 H69A 109.4 . . ? O8 C69 H69B 109.4 . . ? C70 C69 H69B 109.4 . . ? H69A C69 H69B 108.0 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O9 C71 C72 111.6(5) . . ? O9 C71 H71A 109.3 . . ? C72 C71 H71A 109.3 . . ? O9 C71 H71B 109.3 . . ? C72 C71 H71B 109.3 . . ? H71A C71 H71B 108.0 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C78 C73 C74 118.4(6) . . ? C78 C73 C86 120.0(7) . . ? C74 C73 C86 121.3(6) . . ? C75 C74 C73 120.9(6) . . ? C75 C74 H74 119.5 . . ? C73 C74 H74 119.5 . . ? C74 C75 C76 120.8(6) . . ? C74 C75 H75 119.6 . . ? C76 C75 H75 119.6 . . ? C77 C76 C75 117.8(6) . . ? C77 C76 H76 121.1 . . ? C75 C76 H76 121.1 . . ? C78 C77 C76 121.8(6) . . ? C78 C77 H77 119.1 . . ? C76 C77 H77 119.1 . . ? C77 C78 C73 120.1(6) . . ? C77 C78 C79 120.3(6) . . ? C73 C78 C79 119.6(6) . . ? C78 C79 C80 121.8(6) . . ? C78 C79 H79 119.1 . . ? C80 C79 H79 119.1 . . ? C81 C80 C79 120.2(6) . . ? C81 C80 C85 118.9(6) . . ? C79 C80 C85 120.1(6) . . ? C82 C81 C80 120.6(6) . . ? C82 C81 H81 119.7 . . ? C80 C81 H81 119.7 . . ? C81 C82 C83 120.8(7) . . ? C81 C82 H82 119.6 . . ? C83 C82 H82 119.6 . . ? C84 C83 C82 117.9(6) . . ? C84 C83 H83 121.1 . . ? C82 C83 H83 121.1 . . ? C83 C84 C85 122.5(6) . . ? C83 C84 H84 118.7 . . ? C85 C84 H84 118.7 . . ? C84 C85 C80 118.7(6) . . ? C84 C85 C86 124.4(6) . . ? C80 C85 C86 116.8(6) . . ? C73 C86 C85 121.2(5) . . ? C73 C86 C87 122.5(6) . . ? C85 C86 C87 116.1(5) . . ? C86 C87 P3 112.0(4) . . ? C86 C87 H87A 109.2 . . ? P3 C87 H87A 109.2 . . ? C86 C87 H87B 109.2 . . ? P3 C87 H87B 109.2 . . ? H87A C87 H87B 107.9 . . ? O11 C88 C89 119.7(5) . . ? O11 C88 H88A 107.4 . . ? C89 C88 H88A 107.4 . . ? O11 C88 H88B 107.4 . . ? C89 C88 H88B 107.4 . . ? H88A C88 H88B 106.9 . . ? C88 C89 H89A 109.5 . . ? C88 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? O12 C90 C91 109.0(4) . . ? O12 C90 H90A 109.9 . . ? C91 C90 H90A 109.9 . . ? O12 C90 H90B 109.9 . . ? C91 C90 H90B 109.9 . . ? H90A C90 H90B 108.3 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? F20 C92 F19 111.9(5) . . ? F20 C92 F21 107.0(4) . . ? F19 C92 F21 106.3(5) . . ? F20 C92 C93 110.2(5) . . ? F19 C92 C93 111.6(5) . . ? F21 C92 C93 109.8(5) . . ? O19 C93 C94 128.9(6) . . ? O19 C93 C92 111.7(5) . . ? C94 C93 C92 119.4(6) . . ? C93 C94 C95 119.8(6) . . ? C93 C94 H94 120.1 . . ? C95 C94 H94 120.1 . . ? O20 C95 C94 130.5(5) . . ? O20 C95 C96 110.8(5) . . ? C94 C95 C96 118.6(5) . . ? F23 C96 F24 101.9(5) . . ? F23 C96 F22 108.5(5) . . ? F24 C96 F22 109.0(4) . . ? F23 C96 C95 111.0(5) . . ? F24 C96 C95 114.6(5) . . ? F22 C96 C95 111.4(5) . . ? F25 C97 F27 109.2(4) . . ? F25 C97 F26 103.8(4) . . ? F27 C97 F26 107.6(4) . . ? F25 C97 C98 111.5(4) . . ? F27 C97 C98 114.6(5) . . ? F26 C97 C98 109.6(5) . . ? O21 C98 C99 127.5(6) . . ? O21 C98 C97 111.9(5) . . ? C99 C98 C97 120.5(6) . . ? C98 C99 C100 118.7(6) . . ? C98 C99 H99 120.6 . . ? C100 C99 H99 120.6 . . ? O22 C100 C99 130.7(6) . . ? O22 C100 C101 112.9(5) . . ? C99 C100 C101 116.4(5) . . ? F28 C101 F29 111.2(5) . . ? F28 C101 F30 111.5(5) . . ? F29 C101 F30 95.2(4) . . ? F28 C101 C100 110.7(5) . . ? F29 C101 C100 119.0(5) . . ? F30 C101 C100 108.3(5) . . ? F32 C102 F31 111.9(5) . . ? F32 C102 F33 109.8(5) . . ? F31 C102 F33 99.3(4) . . ? F32 C102 C103 116.1(5) . . ? F31 C102 C103 97.3(5) . . ? F33 C102 C103 120.0(5) . . ? O23 C103 C104 127.5(5) . . ? O23 C103 C102 114.9(5) . . ? C104 C103 C102 117.5(5) . . ? C105 C104 C103 120.2(5) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? O24 C105 C104 130.4(5) . . ? O24 C105 C106 113.5(5) . . ? C104 C105 C106 115.8(5) . . ? F36 C106 F34 104.1(4) . . ? F36 C106 F35 108.7(4) . . ? F34 C106 F35 107.8(4) . . ? F36 C106 C105 107.8(5) . . ? F34 C106 C105 118.7(5) . . ? F35 C106 C105 109.3(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.337 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.093 _database_code_depnum_ccdc_archive 'CCDC 925931' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_20121107x #TrackingRef '4 Gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H47 F18 Gd O13 P2' _chemical_formula_weight 1453.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-c 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.322(4) _cell_length_b 19.736(3) _cell_length_c 12.824(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.600(3) _cell_angle_gamma 90.00 _cell_volume 6126.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6948 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 22.38 _exptl_crystal_description blocky _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2900 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24257 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5995 _reflns_number_gt 4685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5995 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.5000 0.218010(16) 0.7500 0.04691(14) Uani 1 2 d S . . P1 P 0.35374(5) 0.25834(7) 0.68528(10) 0.0490(3) Uani 1 1 d . . . F1 F 0.43521(13) 0.41772(17) 0.9703(2) 0.0660(8) Uani 1 1 d . . . F2 F 0.49925(13) 0.44149(17) 0.8690(2) 0.0637(8) Uani 1 1 d . . . F3 F 0.52207(13) 0.42328(19) 1.0237(3) 0.0675(9) Uani 1 1 d . . . F4 F 0.54675(14) 0.20782(17) 1.1661(3) 0.0644(8) Uani 1 1 d . . . F5 F 0.56378(13) 0.12053(17) 1.0588(2) 0.0613(8) Uani 1 1 d . . . F6 F 0.48552(12) 0.13229(16) 1.1142(2) 0.0576(7) Uani 1 1 d . . . F7 F 0.37631(12) 0.03468(17) 0.8414(2) 0.0634(8) Uani 1 1 d . . . F8 F 0.35801(12) 0.05460(17) 0.6784(3) 0.0622(8) Uani 1 1 d . . . F9 F 0.40369(12) -0.03804(17) 0.7362(3) 0.0642(8) Uani 1 1 d . . . O1 O 0.31926(15) 0.22007(17) 0.5953(3) 0.0519(8) Uani 1 1 d . . . O1W O 0.5000 0.4177(5) 0.2500 0.058(2) Uani 0.50 2 d SP . . H1WD H 0.4810 0.4027 0.2973 0.069 Uiso 0.25 1 d PR . . H1WC H 0.5101 0.3848 0.2136 0.087 Uiso 0.25 1 d PR . . O2 O 0.33177(14) 0.33251(18) 0.6755(3) 0.0517(8) Uani 1 1 d . . . O2W O 0.5000 0.0000 0.0000 0.066(3) Uani 0.50 2 d SP . . H2WD H 0.5000 0.0401 0.0241 0.079 Uiso 0.25 1 d PR . . H2WC H 0.4669 -0.0127 -0.0169 0.099 Uiso 0.25 1 d PR . . O3 O 0.41501(13) 0.25448(19) 0.6804(3) 0.0500(8) Uani 1 1 d . . . O4 O 0.47523(15) 0.31743(19) 0.8321(3) 0.0559(9) Uani 1 1 d . . . O5 O 0.50096(15) 0.1752(2) 0.9120(3) 0.0656(10) Uani 1 1 d . . . O6 O 0.43823(14) 0.12904(19) 0.7485(3) 0.0589(9) Uani 1 1 d . . . C1 C 0.2300(2) 0.1893(3) 0.7748(4) 0.0501(11) Uani 1 1 d . . . C2 C 0.2413(2) 0.1310(3) 0.7185(4) 0.0551(12) Uani 1 1 d . . . H2 H 0.2776 0.1200 0.7083 0.066 Uiso 1 1 calc R . . C3 C 0.1982(2) 0.0896(3) 0.6779(4) 0.0559(12) Uani 1 1 d . . . H3 H 0.2058 0.0512 0.6397 0.067 Uiso 1 1 calc R . . C4 C 0.1441(2) 0.1051(3) 0.6938(4) 0.0569(13) Uani 1 1 d . . . H4 H 0.1155 0.0769 0.6669 0.068 Uiso 1 1 calc R . . C5 C 0.1324(2) 0.1624(3) 0.7495(4) 0.0580(13) Uani 1 1 d . . . H5 H 0.0960 0.1722 0.7604 0.070 Uiso 1 1 calc R . . C6 C 0.1747(2) 0.2058(3) 0.7898(5) 0.0546(13) Uani 1 1 d . . . C7 C 0.1610(2) 0.2618(3) 0.8449(4) 0.0527(12) Uani 1 1 d . . . H7 H 0.1242 0.2706 0.8532 0.063 Uiso 1 1 calc R . . C8 C 0.2020(2) 0.3056(3) 0.8888(4) 0.0522(12) Uani 1 1 d . . . C9 C 0.1871(2) 0.3612(3) 0.9447(4) 0.0536(12) Uani 1 1 d . . . H9 H 0.1501 0.3691 0.9537 0.064 Uiso 1 1 calc R . . C10 C 0.2284(2) 0.4060(3) 0.9880(4) 0.0570(12) Uani 1 1 d . . . H10 H 0.2188 0.4440 1.0250 0.068 Uiso 1 1 calc R . . C11 C 0.2828(2) 0.3930(3) 0.9753(4) 0.0571(13) Uani 1 1 d . . . H11 H 0.3101 0.4222 1.0049 0.069 Uiso 1 1 calc R . . C12 C 0.2977(2) 0.3375(3) 0.9192(4) 0.0556(12) Uani 1 1 d . . . H12 H 0.3346 0.3298 0.9103 0.067 Uiso 1 1 calc R . . C13 C 0.2573(2) 0.2931(2) 0.8759(4) 0.0482(11) Uani 1 1 d . . . C14 C 0.2724(2) 0.2358(3) 0.8195(4) 0.0498(11) Uani 1 1 d . . . C15 C 0.3304(2) 0.2209(2) 0.7987(4) 0.0490(11) Uani 1 1 d . . . H15A H 0.3343 0.1722 0.7932 0.059 Uiso 1 1 calc R . . H15B H 0.3546 0.2356 0.8590 0.059 Uiso 1 1 calc R . . C16 C 0.3300(2) 0.2222(3) 0.4830(4) 0.0537(13) Uani 1 1 d . . . H16A H 0.3695 0.2251 0.4785 0.064 Uiso 1 1 calc R . . H16B H 0.3131 0.2625 0.4507 0.064 Uiso 1 1 calc R . . C17 C 0.3077(2) 0.1605(3) 0.4230(4) 0.0582(13) Uani 1 1 d . . . H17A H 0.3348 0.1250 0.4309 0.087 Uiso 1 1 d R . . H17B H 0.3000 0.1714 0.3500 0.087 Uiso 1 1 d R . . H17C H 0.2743 0.1455 0.4502 0.087 Uiso 1 1 d R . . C18 C 0.3579(2) 0.3855(3) 0.6167(4) 0.0589(13) Uani 1 1 d . . . H18A H 0.3541 0.3733 0.5431 0.071 Uiso 1 1 calc R . . H18B H 0.3970 0.3866 0.6399 0.071 Uiso 1 1 calc R . . C19 C 0.3336(2) 0.4583(3) 0.6281(4) 0.0630(14) Uani 1 1 d . . . H19D H 0.3035 0.4563 0.6711 0.094 Uiso 1 1 calc R . . H19E H 0.3206 0.4754 0.5601 0.094 Uiso 1 1 calc R . . H19F H 0.3619 0.4876 0.6600 0.094 Uiso 1 1 calc R . . C20 C 0.4851(2) 0.4053(3) 0.9495(5) 0.0641(15) Uani 1 1 d . . . C21 C 0.4823(2) 0.3300(3) 0.9271(5) 0.0646(15) Uani 1 1 d . . . C22 C 0.4978(3) 0.2807(3) 1.0067(6) 0.0681(17) Uani 1 1 d . . . H22 H 0.5006 0.2967 1.0752 0.082 Uiso 1 1 calc R . . C23 C 0.5096(3) 0.2091(3) 0.9950(5) 0.0680(17) Uani 1 1 d . . . C24 C 0.5302(2) 0.1678(3) 1.0878(5) 0.0615(14) Uani 1 1 d . . . C25 C 0.3955(2) 0.0267(3) 0.7486(4) 0.0581(13) Uani 1 1 d . . . C26 C 0.4480(2) 0.0679(3) 0.7436(4) 0.0588(13) Uani 1 1 d . . . C27 C 0.5000 0.0365(4) 0.7500 0.071(2) Uani 1 2 d S . . H27 H 0.5000 -0.0106 0.7500 0.085 Uiso 1 2 calc SR . . 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 0.0492(2) 0.0372(2) 0.0504(2) 0.000 -0.01544(14) 0.000 P1 0.0496(6) 0.0472(7) 0.0465(7) -0.0056(5) -0.0134(5) -0.0056(5) F1 0.0669(18) 0.076(2) 0.0568(18) 0.0110(16) 0.0143(15) 0.0110(17) F2 0.0685(18) 0.0668(19) 0.0584(17) -0.0135(15) 0.0187(15) -0.0170(16) F3 0.0602(17) 0.077(2) 0.066(2) -0.0113(17) 0.0116(16) 0.0152(16) F4 0.0644(19) 0.074(2) 0.0568(18) 0.0094(16) 0.0142(16) 0.0127(15) F5 0.0614(17) 0.070(2) 0.0517(16) -0.0094(15) 0.0011(14) -0.0116(15) F6 0.0559(15) 0.0598(17) 0.0558(17) -0.0057(14) -0.0016(13) -0.0144(14) F7 0.0596(16) 0.0676(19) 0.0656(19) -0.0077(15) 0.0186(15) 0.0094(15) F8 0.0564(16) 0.0654(19) 0.0659(19) 0.0068(16) 0.0117(14) 0.0126(15) F9 0.0521(16) 0.066(2) 0.072(2) -0.0086(16) -0.0082(14) 0.0111(14) O1 0.0529(19) 0.058(2) 0.0417(18) -0.0071(15) -0.0123(15) -0.0115(15) O1W 0.067(6) 0.054(6) 0.053(6) 0.000 0.010(5) 0.000 O2 0.0511(18) 0.0499(19) 0.054(2) -0.0086(16) 0.0040(15) -0.0049(15) O2W 0.055(5) 0.095(9) 0.045(5) -0.014(5) -0.016(4) -0.018(6) O3 0.0486(17) 0.0515(19) 0.0453(18) -0.0053(15) -0.0186(14) -0.0021(15) O4 0.058(2) 0.056(2) 0.055(2) 0.0031(17) 0.0150(17) 0.0058(17) O5 0.055(2) 0.088(3) 0.052(2) -0.002(2) -0.0046(17) 0.007(2) O6 0.0481(18) 0.052(2) 0.072(2) 0.0126(18) -0.0178(16) -0.0010(16) C1 0.049(3) 0.054(3) 0.044(3) -0.009(2) -0.010(2) -0.005(2) C2 0.059(3) 0.054(3) 0.054(3) -0.009(2) 0.015(2) -0.014(2) C3 0.064(3) 0.061(3) 0.042(3) -0.008(2) 0.005(2) -0.006(3) C4 0.047(3) 0.069(3) 0.052(3) -0.010(3) -0.007(2) 0.005(2) C5 0.056(3) 0.057(3) 0.059(3) -0.009(3) -0.002(2) -0.010(2) C6 0.051(3) 0.057(3) 0.057(3) -0.014(2) 0.012(2) -0.010(2) C7 0.050(3) 0.057(3) 0.054(3) -0.007(2) 0.017(2) -0.004(2) C8 0.059(3) 0.051(3) 0.048(3) -0.009(2) 0.012(2) -0.010(2) C9 0.057(3) 0.054(3) 0.052(3) 0.000(2) 0.012(2) -0.004(2) C10 0.067(3) 0.055(3) 0.051(3) -0.010(2) 0.016(2) -0.006(2) C11 0.066(3) 0.050(3) 0.051(3) -0.007(2) -0.017(2) 0.009(2) C12 0.066(3) 0.056(3) 0.043(3) -0.007(2) -0.007(2) -0.002(2) C13 0.054(3) 0.043(3) 0.045(3) -0.008(2) -0.008(2) -0.002(2) C14 0.052(3) 0.046(2) 0.049(3) -0.009(2) -0.006(2) -0.003(2) C15 0.050(2) 0.048(3) 0.046(3) -0.006(2) -0.010(2) -0.008(2) C16 0.053(3) 0.065(3) 0.044(3) 0.013(2) 0.010(2) 0.012(2) C17 0.054(3) 0.065(3) 0.053(3) 0.014(3) -0.009(2) -0.010(2) C18 0.053(3) 0.071(4) 0.054(3) -0.007(3) 0.016(2) -0.012(3) C19 0.063(3) 0.068(4) 0.054(3) 0.006(3) -0.008(2) -0.016(3) C20 0.064(3) 0.078(4) 0.051(3) -0.003(3) 0.014(3) 0.010(3) C21 0.053(3) 0.081(4) 0.064(4) 0.007(3) 0.022(3) 0.005(3) C22 0.058(3) 0.085(5) 0.065(4) 0.004(3) 0.025(3) 0.008(3) C23 0.066(3) 0.087(4) 0.054(3) 0.000(3) 0.019(3) 0.025(3) C24 0.068(3) 0.063(3) 0.057(3) -0.001(3) 0.022(3) -0.005(3) C25 0.058(3) 0.051(3) 0.067(3) 0.006(3) 0.013(3) 0.010(2) C26 0.070(3) 0.043(3) 0.065(3) 0.008(2) 0.021(3) 0.000(2) C27 0.051(4) 0.057(5) 0.110(7) 0.000 0.033(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O5 2.241(4) . ? Gd1 O5 2.241(4) 2_656 ? Gd1 O3 2.286(3) 2_656 ? Gd1 O3 2.286(3) . ? Gd1 O6 2.310(4) 2_656 ? Gd1 O6 2.310(4) . ? Gd1 O4 2.333(4) 2_656 ? Gd1 O4 2.334(4) . ? P1 O3 1.500(4) . ? P1 O1 1.554(3) . ? P1 O2 1.559(4) . ? P1 C15 1.774(5) . ? F1 C20 1.292(6) . ? F2 C20 1.328(7) . ? F3 C20 1.293(7) . ? F4 C24 1.309(7) . ? F5 C24 1.317(7) . ? F6 C24 1.365(6) . ? F7 C25 1.329(6) . ? F8 C25 1.337(6) . ? F9 C25 1.304(6) . ? O1 C16 1.490(6) . ? O1W H1WD 0.8500 . ? O1W H1WC 0.8499 . ? O2 C18 1.470(6) . ? O2W H2WD 0.8500 . ? O2W H2WC 0.8500 . ? O4 C21 1.239(7) . ? O5 C23 1.257(8) . ? O6 C26 1.232(6) . ? C1 C2 1.399(7) . ? C1 C6 1.416(7) . ? C1 C14 1.455(7) . ? C2 C3 1.389(7) . ? C2 H2 0.9300 . ? C3 C4 1.387(7) . ? C3 H3 0.9300 . ? C4 C5 1.382(8) . ? C4 H4 0.9300 . ? C5 C6 1.397(7) . ? C5 H5 0.9300 . ? C6 C7 1.370(7) . ? C7 C8 1.397(8) . ? C7 H7 0.9300 . ? C8 C9 1.378(7) . ? C8 C13 1.391(7) . ? C9 C10 1.411(8) . ? C9 H9 0.9300 . ? C10 C11 1.374(8) . ? C10 H10 0.9300 . ? C11 C12 1.377(7) . ? C11 H11 0.9300 . ? C12 C13 1.391(7) . ? C12 H12 0.9300 . ? C13 C14 1.411(7) . ? C14 C15 1.489(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.513(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9599 . ? C17 H17B 0.9600 . ? C17 H17C 0.9601 . ? C18 C19 1.564(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19D 0.9600 . ? C19 H19E 0.9600 . ? C19 H19F 0.9600 . ? C20 C21 1.513(9) . ? C21 C22 1.435(9) . ? C22 C23 1.452(8) . ? C22 H22 0.9300 . ? C23 C24 1.489(9) . ? C25 C26 1.521(7) . ? C26 C27 1.404(7) . ? C27 C26 1.404(7) 2_656 ? C27 H27 0.9300 . ? 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 O5 Gd1 O5 135.7(2) . 2_656 ? O5 Gd1 O3 80.18(13) . 2_656 ? O5 Gd1 O3 114.07(13) 2_656 2_656 ? O5 Gd1 O3 114.08(13) . . ? O5 Gd1 O3 80.18(13) 2_656 . ? O3 Gd1 O3 143.30(18) 2_656 . ? O5 Gd1 O6 76.00(15) . 2_656 ? O5 Gd1 O6 70.66(15) 2_656 2_656 ? O3 Gd1 O6 70.95(12) 2_656 2_656 ? O3 Gd1 O6 143.61(12) . 2_656 ? O5 Gd1 O6 70.66(15) . . ? O5 Gd1 O6 76.00(15) 2_656 . ? O3 Gd1 O6 143.61(12) 2_656 . ? O3 Gd1 O6 70.95(12) . . ? O6 Gd1 O6 81.04(18) 2_656 . ? O5 Gd1 O4 139.07(15) . 2_656 ? O5 Gd1 O4 83.02(15) 2_656 2_656 ? O3 Gd1 O4 69.40(13) 2_656 2_656 ? O3 Gd1 O4 79.78(13) . 2_656 ? O6 Gd1 O4 116.52(13) 2_656 2_656 ? O6 Gd1 O4 146.30(13) . 2_656 ? O5 Gd1 O4 83.02(15) . . ? O5 Gd1 O4 139.07(15) 2_656 . ? O3 Gd1 O4 79.78(13) 2_656 . ? O3 Gd1 O4 69.40(13) . . ? O6 Gd1 O4 146.30(13) 2_656 . ? O6 Gd1 O4 116.52(13) . . ? O4 Gd1 O4 65.54(17) 2_656 . ? O3 P1 O1 114.2(2) . . ? O3 P1 O2 112.2(2) . . ? O1 P1 O2 103.9(2) . . ? O3 P1 C15 114.4(2) . . ? O1 P1 C15 102.3(2) . . ? O2 P1 C15 108.8(2) . . ? C16 O1 P1 124.8(3) . . ? H1WD O1W H1WC 109.5 . . ? C18 O2 P1 123.2(3) . . ? H2WD O2W H2WC 109.5 . . ? P1 O3 Gd1 149.8(2) . . ? C21 O4 Gd1 126.5(4) . . ? C23 O5 Gd1 124.7(4) . . ? C26 O6 Gd1 128.0(4) . . ? C2 C1 C6 119.7(5) . . ? C2 C1 C14 123.7(5) . . ? C6 C1 C14 116.6(5) . . ? C3 C2 C1 119.9(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 118.6(5) . . ? C7 C6 C1 122.5(5) . . ? C5 C6 C1 118.9(5) . . ? C6 C7 C8 120.6(5) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C13 120.7(5) . . ? C9 C8 C7 119.2(5) . . ? C13 C8 C7 120.1(5) . . ? C8 C9 C10 119.3(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.0(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C8 119.5(5) . . ? C12 C13 C14 120.0(5) . . ? C8 C13 C14 120.4(4) . . ? C13 C14 C1 119.8(5) . . ? C13 C14 C15 123.3(4) . . ? C1 C14 C15 116.9(4) . . ? C14 C15 P1 116.7(4) . . ? C14 C15 H15A 108.1 . . ? P1 C15 H15A 108.1 . . ? C14 C15 H15B 108.1 . . ? P1 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? O1 C16 C17 112.4(4) . . ? O1 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? O1 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C17 H17A 108.8 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.7 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O2 C18 C19 114.8(4) . . ? O2 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? O2 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.5 . . ? C18 C19 H19D 109.5 . . ? C18 C19 H19E 109.5 . . ? H19D C19 H19E 109.5 . . ? C18 C19 H19F 109.5 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? F1 C20 F3 113.3(4) . . ? F1 C20 F2 112.2(5) . . ? F3 C20 F2 102.1(5) . . ? F1 C20 C21 101.5(5) . . ? F3 C20 C21 115.1(5) . . ? F2 C20 C21 113.0(5) . . ? O4 C21 C22 124.4(6) . . ? O4 C21 C20 112.5(5) . . ? C22 C21 C20 121.9(6) . . ? C21 C22 C23 128.9(6) . . ? C21 C22 H22 115.6 . . ? C23 C22 H22 115.6 . . ? O5 C23 C22 126.0(6) . . ? O5 C23 C24 113.6(6) . . ? C22 C23 C24 120.3(6) . . ? F4 C24 F5 119.5(5) . . ? F4 C24 F6 108.2(4) . . ? F5 C24 F6 103.7(5) . . ? F4 C24 C23 109.7(5) . . ? F5 C24 C23 109.4(4) . . ? F6 C24 C23 105.4(5) . . ? F9 C25 F7 107.3(4) . . ? F9 C25 F8 115.1(5) . . ? F7 C25 F8 106.1(4) . . ? F9 C25 C26 112.4(4) . . ? F7 C25 C26 110.1(5) . . ? F8 C25 C26 105.7(4) . . ? O6 C26 C27 127.3(6) . . ? O6 C26 C25 110.8(5) . . ? C27 C26 C25 121.1(5) . . ? C26 C27 C26 127.6(8) 2_656 . ? C26 C27 H27 116.2 2_656 . ? C26 C27 H27 116.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 C16 -43.5(4) . . . . ? O2 P1 O1 C16 79.1(4) . . . . ? C15 P1 O1 C16 -167.7(4) . . . . ? O3 P1 O2 C18 29.6(4) . . . . ? O1 P1 O2 C18 -94.4(4) . . . . ? C15 P1 O2 C18 157.2(4) . . . . ? O1 P1 O3 Gd1 -113.6(4) . . . . ? O2 P1 O3 Gd1 128.4(4) . . . . ? C15 P1 O3 Gd1 3.8(5) . . . . ? O5 Gd1 O3 P1 -10.9(5) . . . . ? O5 Gd1 O3 P1 125.0(5) 2_656 . . . ? O3 Gd1 O3 P1 -117.6(4) 2_656 . . . ? O6 Gd1 O3 P1 88.3(5) 2_656 . . . ? O6 Gd1 O3 P1 46.6(4) . . . . ? O4 Gd1 O3 P1 -150.4(4) 2_656 . . . ? O4 Gd1 O3 P1 -82.8(4) . . . . ? O5 Gd1 O4 C21 19.6(4) . . . . ? O5 Gd1 O4 C21 -176.8(4) 2_656 . . . ? O3 Gd1 O4 C21 -61.7(4) 2_656 . . . ? O3 Gd1 O4 C21 138.6(4) . . . . ? O6 Gd1 O4 C21 -31.9(5) 2_656 . . . ? O6 Gd1 O4 C21 83.8(4) . . . . ? O4 Gd1 O4 C21 -133.6(5) 2_656 . . . ? O5 Gd1 O5 C23 169.0(5) 2_656 . . . ? O3 Gd1 O5 C23 54.4(4) 2_656 . . . ? O3 Gd1 O5 C23 -90.0(4) . . . . ? O6 Gd1 O5 C23 127.1(4) 2_656 . . . ? O6 Gd1 O5 C23 -147.7(5) . . . . ? O4 Gd1 O5 C23 12.6(5) 2_656 . . . ? O4 Gd1 O5 C23 -26.3(4) . . . . ? O5 Gd1 O6 C26 -82.1(5) . . . . ? O5 Gd1 O6 C26 68.2(5) 2_656 . . . ? O3 Gd1 O6 C26 -43.5(6) 2_656 . . . ? O3 Gd1 O6 C26 152.5(5) . . . . ? O6 Gd1 O6 C26 -3.9(4) 2_656 . . . ? O4 Gd1 O6 C26 121.4(4) 2_656 . . . ? O4 Gd1 O6 C26 -153.5(5) . . . . ? C6 C1 C2 C3 -0.2(8) . . . . ? C14 C1 C2 C3 -179.5(5) . . . . ? C1 C2 C3 C4 -0.8(8) . . . . ? C2 C3 C4 C5 0.6(8) . . . . ? C3 C4 C5 C6 0.6(9) . . . . ? C4 C5 C6 C7 -179.7(5) . . . . ? C4 C5 C6 C1 -1.6(9) . . . . ? C2 C1 C6 C7 179.4(6) . . . . ? C14 C1 C6 C7 -1.2(8) . . . . ? C2 C1 C6 C5 1.4(8) . . . . ? C14 C1 C6 C5 -179.3(5) . . . . ? C5 C6 C7 C8 178.4(5) . . . . ? C1 C6 C7 C8 0.4(9) . . . . ? C6 C7 C8 C9 -179.4(5) . . . . ? C6 C7 C8 C13 0.6(9) . . . . ? C13 C8 C9 C10 0.7(8) . . . . ? C7 C8 C9 C10 -179.3(5) . . . . ? C8 C9 C10 C11 -0.9(8) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C10 C11 C12 C13 -1.0(8) . . . . ? C11 C12 C13 C8 0.7(8) . . . . ? C11 C12 C13 C14 -179.3(5) . . . . ? C9 C8 C13 C12 -0.5(8) . . . . ? C7 C8 C13 C12 179.4(5) . . . . ? C9 C8 C13 C14 179.4(5) . . . . ? C7 C8 C13 C14 -0.6(8) . . . . ? C12 C13 C14 C1 179.7(5) . . . . ? C8 C13 C14 C1 -0.3(8) . . . . ? C12 C13 C14 C15 -2.8(8) . . . . ? C8 C13 C14 C15 177.2(5) . . . . ? C2 C1 C14 C13 -179.5(5) . . . . ? C6 C1 C14 C13 1.2(8) . . . . ? C2 C1 C14 C15 2.9(8) . . . . ? C6 C1 C14 C15 -176.5(5) . . . . ? C13 C14 C15 P1 -87.0(6) . . . . ? C1 C14 C15 P1 90.6(5) . . . . ? O3 P1 C15 C14 167.4(3) . . . . ? O1 P1 C15 C14 -68.6(4) . . . . ? O2 P1 C15 C14 41.0(4) . . . . ? P1 O1 C16 C17 155.8(4) . . . . ? P1 O2 C18 C19 -172.9(4) . . . . ? Gd1 O4 C21 C22 -12.4(8) . . . . ? Gd1 O4 C21 C20 155.3(4) . . . . ? F1 C20 C21 O4 97.7(5) . . . . ? F3 C20 C21 O4 -139.5(5) . . . . ? F2 C20 C21 O4 -22.7(7) . . . . ? F1 C20 C21 C22 -94.3(6) . . . . ? F3 C20 C21 C22 28.5(7) . . . . ? F2 C20 C21 C22 145.3(5) . . . . ? O4 C21 C22 C23 2.0(10) . . . . ? C20 C21 C22 C23 -164.6(6) . . . . ? Gd1 O5 C23 C22 27.7(8) . . . . ? Gd1 O5 C23 C24 -156.7(4) . . . . ? C21 C22 C23 O5 -10.5(10) . . . . ? C21 C22 C23 C24 174.1(6) . . . . ? O5 C23 C24 F4 169.6(5) . . . . ? C22 C23 C24 F4 -14.5(8) . . . . ? O5 C23 C24 F5 36.7(7) . . . . ? C22 C23 C24 F5 -147.4(5) . . . . ? O5 C23 C24 F6 -74.1(6) . . . . ? C22 C23 C24 F6 101.8(6) . . . . ? Gd1 O6 C26 C27 8.2(8) . . . . ? Gd1 O6 C26 C25 178.0(3) . . . . ? F9 C25 C26 O6 175.5(5) . . . . ? F7 C25 C26 O6 -64.9(6) . . . . ? F8 C25 C26 O6 49.2(6) . . . . ? F9 C25 C26 C27 -14.0(7) . . . . ? F7 C25 C26 C27 105.6(5) . . . . ? F8 C25 C26 C27 -140.3(4) . . . . ? O6 C26 C27 C26 -4.6(5) . . . 2_656 ? C25 C26 C27 C26 -173.5(6) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.696 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 925932'