Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email COSTES@LCC-TOULOUSE.FR _publ_contact_author_name 'Dr Jean-Pierre Costes' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Laboratoire de Chimie de Coordination CNRS 205, route de Narbonne Toulouse 31077 FRANCE ; _publ_section_title ; Hetero Di- and Trinuclear Cu-Gd Complexes with Trifluoroacetate Bridges: Synthesis, Structural and Magnetic Studies ; loop_ _publ_author_name _publ_author_address G.Novitchi ; Department of Chemistry Moldova State University A. Mateevici str.60.2009 Chisinau Moldova ; S.Shova ; Institute of Applied Physics Academy of Sciences of Moldova Academiei str. 3.2028 Chisinau Moldova ; 'Andrea Caneschi' ; Dipartimento di Chimica, Universita di Firenze, 50019 S. Fiorentino, Italy. ; J.-P.Costes ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Maria Gdaniec' ; Faculty of Chemistry, A. Mickiewicz University, Grunwaldzka 6, 60-780, Poznan, Poland ; 'Nicolae Stanica' ; Institute of Physical Chemistry, Splaiul Independentei 202, 70208 Bucuresti, Romania ; data_1 _database_code_depnum_ccdc_archive 'CCDC 215829' _chemical_name_common 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 Cu F9 Gd N2 O12' _chemical_formula_weight 1034.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.582(5) _cell_length_b 19.872(5) _cell_length_c 21.060(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 94.040(5) _cell_angle_gamma 90.000(5) _cell_volume 4000(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180 _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.5 _exptl_crystal_description prism _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 2.276 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.540 _exptl_absorpt_process_details 'R. H. Blessing, Acta Cryst., 1995, a51, 33' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4CCD' _diffrn_measurement_method omega-phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30006 _diffrn_reflns_av_R_equivalents 0.0884 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7417 _reflns_number_gt 4506 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++) (compiled Jun 6 2003,13:53:32 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1244P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7417 _refine_ls_number_parameters 546 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1853 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 1.025 _refine_ls_shift/su_mean 0.032 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 0.51144(4) 0.22677(2) -0.09336(2) 0.05053(17) Uani 1 1 d . A . Cu1 Cu 0.63645(10) 0.34152(5) 0.01543(5) 0.0509(3) Uani 1 1 d . A . O2A O 0.4598(6) 0.3221(3) -0.0314(3) 0.0567(16) Uani 1 1 d . . . O1A O 0.6927(6) 0.2539(3) -0.0155(3) 0.0535(15) Uani 1 1 d . . . O5A O 0.6894(7) 0.1309(3) -0.0528(3) 0.0635(17) Uani 1 1 d . A . N2A N 0.5645(8) 0.4169(5) 0.0594(5) 0.084(3) Uani 1 1 d D . . N1A N 0.7897(10) 0.3478(4) 0.0775(4) 0.073(2) Uani 1 1 d D . . C15A C 0.6818(16) 0.4537(7) 0.0966(11) 0.126(16) Uani 0.558(19) 1 d PD A 1 H15A H 0.7395 0.4778 0.0681 0.151 Uiso 0.558(19) 1 calc PR A 1 H15B H 0.6447 0.4856 0.1259 0.151 Uiso 0.558(19) 1 calc PR A 1 C17A C 0.7621(13) 0.4016(8) 0.1308(6) 0.082(8) Uani 0.558(19) 1 d PD A 1 C25A C 0.8922(16) 0.4371(12) 0.1530(10) 0.084(8) Uani 0.558(19) 1 d PD A 1 H25A H 0.9391 0.4525 0.1169 0.126 Uiso 0.558(19) 1 calc PR A 1 H25B H 0.9522 0.4069 0.1778 0.126 Uiso 0.558(19) 1 calc PR A 1 H25C H 0.8695 0.4749 0.1787 0.126 Uiso 0.558(19) 1 calc PR A 1 C25* C 0.665(2) 0.5011(9) 0.1451(12) 0.063(7) Uani 0.442(19) 1 d PD A 2 H25D H 0.7437 0.5062 0.1758 0.095 Uiso 0.442(19) 1 calc PR A 2 H25E H 0.5809 0.5131 0.1642 0.095 Uiso 0.442(19) 1 calc PR A 2 H25F H 0.6777 0.5298 0.1093 0.095 Uiso 0.442(19) 1 calc PR A 2 C15* C 0.6565(19) 0.4305(7) 0.1236(6) 0.090(11) Uani 0.442(19) 1 d PD A 2 C17* C 0.8011(15) 0.4197(10) 0.1033(13) 0.076(9) Uiso 0.442(19) 1 d PD A 2 H17A H 0.8705 0.4232 0.1389 0.091 Uiso 0.442(19) 1 calc PR A 2 H17B H 0.8234 0.4514 0.0705 0.091 Uiso 0.442(19) 1 calc PR A 2 C24A C 0.6589(12) 0.3817(6) 0.1811(5) 0.074(3) Uani 1 1 d D . . H24A H 0.6501 0.4179 0.2107 0.111 Uiso 0.558(19) 1 d PR A . H24B H 0.5689 0.3719 0.1602 0.111 Uiso 0.558(19) 1 d PR . . H24C H 0.6942 0.3425 0.2034 0.111 Uiso 0.558(19) 1 d PR . . H24A' H 0.7210 0.3978 0.2155 0.111 Uiso 0.442(19) 1 d PR . . H24B' H 0.5657 0.3786 0.1948 0.111 Uiso 0.442(19) 1 d PR . . H24C' H 0.6890 0.3381 0.1680 0.111 Uiso 0.442(19) 1 d PR . . C7A C 0.8784(12) 0.3006(6) 0.0941(6) 0.080(3) Uani 1 1 d . A . H7A H 0.9470 0.3104 0.1262 0.096 Uiso 1 1 calc R . . C6A C 0.8787(10) 0.2348(5) 0.0668(5) 0.064(3) Uani 1 1 d . . . C5A C 0.9705(12) 0.1877(6) 0.0941(6) 0.084(4) Uani 1 1 d . A . H5A H 1.0375 0.2015 0.1255 0.101 Uiso 1 1 calc R . . C4A C 0.9659(13) 0.1229(7) 0.0767(7) 0.101(5) Uani 1 1 d . . . H4A H 1.0268 0.0923 0.0974 0.121 Uiso 1 1 calc R A . C3A C 0.8733(12) 0.1012(6) 0.0291(6) 0.085(4) Uani 1 1 d . A . H3A H 0.8691 0.0559 0.0181 0.102 Uiso 1 1 calc R . . C2A C 0.7870(10) 0.1463(5) -0.0024(5) 0.061(2) Uani 1 1 d . . . C1A C 0.7832(9) 0.2128(5) 0.0156(4) 0.055(2) Uani 1 1 d . A . C8A C 0.3371(9) 0.3515(4) -0.0193(5) 0.054(2) Uani 1 1 d . A . C9A C 0.2175(9) 0.3227(5) -0.0507(5) 0.064(3) Uani 1 1 d . A . C10A C 0.0891(11) 0.3519(5) -0.0449(6) 0.075(3) Uani 1 1 d . . . H10A H 0.0100 0.3327 -0.0656 0.090 Uiso 1 1 calc R . . C11A C 0.0751(9) 0.4088(5) -0.0092(6) 0.072(3) Uani 1 1 d . . . H11A H -0.0125 0.4283 -0.0066 0.086 Uiso 1 1 calc R . . C12A C 0.1892(10) 0.4365(5) 0.0223(6) 0.074(3) Uani 1 1 d . A . H12A H 0.1792 0.4743 0.0475 0.088 Uiso 1 1 d R . . C13A C 0.3231(9) 0.4085(5) 0.0177(5) 0.062(3) Uani 1 1 d . . . C14A C 0.4385(11) 0.4378(6) 0.0579(7) 0.092(4) Uani 1 1 d . A . H14A H 0.4184 0.4750 0.0824 0.110 Uiso 1 1 d R . . O6A O 0.2450(7) 0.2651(4) -0.0841(4) 0.086(3) Uani 1 1 d D . . C22A C 0.1279(14) 0.2355(9) -0.1266(7) 0.071(6) Uani 0.70(3) 1 d PD B 1 H22A H 0.0673 0.2701 -0.1458 0.085 Uiso 0.70(3) 1 d PR B 1 H22B H 0.1624 0.2074 -0.1597 0.085 Uiso 0.70(3) 1 d PR B 1 C23A C 0.0434(19) 0.1964(10) -0.0834(10) 0.097(7) Uani 0.73(3) 1 d PD B 1 H23A H 0.1038 0.1607 -0.0675 0.146 Uiso 0.73(3) 1 d PR B 1 H23B H -0.0406 0.1776 -0.1036 0.146 Uiso 0.73(3) 1 d PR B 1 H23C H 0.0202 0.2247 -0.0487 0.146 Uiso 0.73(3) 1 d PR B 1 C22* C 0.121(3) 0.2165(15) -0.0771(13) 0.057(11) Uiso 0.30(3) 1 d PD B 2 H22C H 0.1544 0.1710 -0.0688 0.068 Uiso 0.30(3) 1 calc PR B 2 H22D H 0.0662 0.2305 -0.0424 0.068 Uiso 0.30(3) 1 calc PR B 2 C23* C 0.037(3) 0.2199(17) -0.1382(13) 0.048(10) Uiso 0.27(3) 1 d PD B 2 H23D H -0.0263 0.2574 -0.1377 0.072 Uiso 0.27(3) 1 calc PR B 2 H23E H -0.0155 0.1790 -0.1446 0.072 Uiso 0.27(3) 1 calc PR B 2 H23F H 0.0977 0.2256 -0.1721 0.072 Uiso 0.27(3) 1 calc PR B 2 C20A C 0.6873(13) 0.0617(6) -0.0755(7) 0.090(4) Uani 1 1 d . . . H20A H 0.6006 0.0540 -0.1011 0.108 Uiso 1 1 d R A . H20B H 0.6884 0.0317 -0.0391 0.108 Uiso 1 1 d R . . C21A C 0.8052(18) 0.0435(7) -0.1137(8) 0.121(6) Uani 1 1 d . A . H21A H 0.8276 0.0815 -0.1391 0.181 Uiso 1 1 d R . . H21B H 0.7801 0.0060 -0.1409 0.181 Uiso 1 1 d R . . H21C H 0.8851 0.0317 -0.0858 0.181 Uiso 1 1 d R . . C3C C 0.3320(11) 0.0771(5) -0.1019(6) 0.067(3) Uani 1 1 d . B . O3C O 0.3848(6) 0.1294(3) -0.1246(3) 0.0585(16) Uani 1 1 d . . . O4C O 0.3082(11) 0.0649(5) -0.0460(4) 0.102(3) Uani 1 1 d . . . C4C C 0.2944(12) 0.0223(5) -0.1501(6) 0.090(4) Uani 1 1 d D . . F7C F 0.345(2) 0.0298(10) -0.2062(7) 0.090(6) Uiso 0.47(4) 1 d PD B 1 F8C F 0.346(2) -0.0380(6) -0.1260(7) 0.077(6) Uiso 0.47(4) 1 d PD B 1 F9C F 0.1604(13) 0.0135(14) -0.1608(12) 0.111(8) Uiso 0.47(4) 1 d PD B 1 F7C* F 0.387(2) 0.0180(11) -0.1943(10) 0.106(6) Uiso 0.53(4) 1 d PD B 2 F8C* F 0.272(3) -0.0370(9) -0.1229(9) 0.140(9) Uiso 0.53(4) 1 d PD B 2 F9C* F 0.1691(17) 0.0381(15) -0.1785(11) 0.134(8) Uiso 0.53(4) 1 d PD B 2 C1C C 0.6401(12) 0.1888(6) -0.2364(5) 0.071(3) Uani 1 1 d . B . O1C O 0.6460(6) 0.1831(3) -0.1778(3) 0.0593(16) Uani 1 1 d . . . O2C O 0.5459(11) 0.2076(7) -0.2716(4) 0.125(4) Uani 1 1 d . . . C2C C 0.7735(14) 0.1691(6) -0.2683(5) 0.096(4) Uani 1 1 d D . . F4C F 0.8882(16) 0.1797(10) -0.2302(8) 0.119(7) Uiso 0.54(2) 1 d PD B 1 F5C F 0.785(2) 0.1950(11) -0.3250(7) 0.127(7) Uiso 0.54(2) 1 d PD B 1 F6C F 0.770(2) 0.1026(8) -0.2752(9) 0.131(7) Uiso 0.54(2) 1 d PD B 1 F4C* F 0.866(2) 0.2194(10) -0.2663(12) 0.144(10) Uiso 0.46(2) 1 d PD B 2 F5C* F 0.747(2) 0.1544(13) -0.3303(7) 0.133(8) Uiso 0.46(2) 1 d PD B 2 F6C* F 0.845(2) 0.1183(10) -0.2438(9) 0.117(8) Uiso 0.46(2) 1 d PD B 2 C18A C 0.7015(9) 0.3715(5) -0.1208(5) 0.056(2) Uani 1 1 d . A . O3A O 0.7201(6) 0.3970(3) -0.0678(3) 0.0561(15) Uani 1 1 d . . . O4A O 0.6389(7) 0.3180(3) -0.1376(3) 0.0663(17) Uani 1 1 d . . . C19A C 0.7638(11) 0.4077(5) -0.1768(5) 0.072(3) Uani 1 1 d D . . F1A F 0.8807(13) 0.4413(8) -0.1588(6) 0.099(5) Uiso 0.545(17) 1 d PD A 1 F2A F 0.782(2) 0.3720(9) -0.2283(8) 0.135(7) Uiso 0.545(17) 1 d PD A 1 F3A F 0.6759(16) 0.4561(8) -0.1975(8) 0.123(6) Uiso 0.545(17) 1 d PD A 1 F1A* F 0.797(2) 0.4716(7) -0.1662(9) 0.113(7) Uiso 0.455(17) 1 d PD A 2 F2A* F 0.8746(17) 0.3726(9) -0.1957(9) 0.109(7) Uiso 0.455(17) 1 d PD A 2 F3A* F 0.6825(17) 0.4087(10) -0.2303(7) 0.103(6) Uiso 0.455(17) 1 d PD A 2 O2D O 0.3837(7) 0.2632(4) -0.1922(4) 0.073(2) Uani 1 1 d . . . H2 H 0.4193 0.2353 -0.2179 0.088 Uiso 1 1 d R A . C3D C 0.3448(15) 0.3311(7) -0.2119(7) 0.102(4) Uani 1 1 d . A . H3D1 H 0.4259 0.3542 -0.2264 0.122 Uiso 1 1 calc R . . H3D2 H 0.3128 0.3558 -0.1760 0.122 Uiso 1 1 calc R . . C4D C 0.2301(14) 0.3293(9) -0.2649(8) 0.119(6) Uani 1 1 d . . . H4D1 H 0.2677 0.3135 -0.3033 0.178 Uiso 1 1 calc R A . H4D2 H 0.1927 0.3738 -0.2717 0.178 Uiso 1 1 calc R . . H4D3 H 0.1571 0.2995 -0.2535 0.178 Uiso 1 1 calc R . . O1D O 0.4308(7) 0.1773(4) 0.0045(3) 0.0685(18) Uani 1 1 d . . . H1 H 0.3783 0.1422 0.0000 0.082 Uiso 1 1 d R A . C1D C 0.408(2) 0.2017(9) 0.0663(6) 0.121(6) Uani 1 1 d . A . H1D1 H 0.4857 0.2304 0.0805 0.145 Uiso 1 1 calc R . . H1D2 H 0.3241 0.2293 0.0635 0.145 Uiso 1 1 calc R . . C2D C 0.393(3) 0.1525(11) 0.1120(9) 0.150(7) Uani 1 1 d . . . H2D1 H 0.3096 0.1269 0.1012 0.226 Uiso 1 1 calc R A . H2D2 H 0.3862 0.1733 0.1528 0.226 Uiso 1 1 calc R . . H2D3 H 0.4726 0.1231 0.1137 0.226 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0509(2) 0.0348(3) 0.0643(3) -0.0037(2) -0.00728(17) 0.00141(18) Cu1 0.0462(5) 0.0397(6) 0.0655(7) -0.0063(5) -0.0046(4) -0.0002(4) O2A 0.048(3) 0.037(3) 0.085(4) -0.017(3) 0.000(3) 0.005(2) O1A 0.047(3) 0.045(3) 0.065(4) 0.004(3) -0.020(3) 0.005(2) O5A 0.073(4) 0.040(4) 0.075(4) -0.010(3) -0.016(3) 0.018(3) N2A 0.048(4) 0.070(6) 0.135(9) -0.047(6) 0.014(5) -0.013(4) N1A 0.100(6) 0.044(5) 0.071(5) 0.000(4) -0.028(5) -0.001(4) C15A 0.052(13) 0.11(2) 0.23(4) -0.11(3) 0.073(19) -0.062(15) C17A 0.103(19) 0.050(12) 0.089(17) -0.005(11) -0.015(15) -0.028(12) C25A 0.052(10) 0.114(18) 0.083(14) -0.056(13) -0.011(9) -0.006(10) C25* 0.061(12) 0.044(13) 0.082(16) -0.005(11) -0.011(11) 0.000(9) C15* 0.058(17) 0.08(2) 0.13(3) -0.043(19) 0.025(17) -0.036(15) C24A 0.098(8) 0.065(7) 0.061(6) -0.006(5) 0.024(6) -0.022(6) C7A 0.088(7) 0.061(7) 0.085(8) 0.007(6) -0.032(6) -0.003(6) C6A 0.060(5) 0.067(7) 0.062(6) 0.009(5) -0.019(4) 0.007(5) C5A 0.092(8) 0.064(8) 0.089(8) 0.010(6) -0.035(6) 0.016(6) C4A 0.095(9) 0.076(10) 0.126(11) 0.021(8) -0.033(8) 0.038(7) C3A 0.082(7) 0.064(7) 0.103(9) 0.014(6) -0.030(7) 0.026(6) C2A 0.059(5) 0.042(6) 0.079(7) 0.003(5) -0.005(5) 0.017(4) C1A 0.051(5) 0.058(6) 0.054(5) 0.006(4) -0.008(4) 0.009(4) C8A 0.045(4) 0.039(5) 0.079(6) 0.004(4) 0.007(4) 0.002(4) C9A 0.045(4) 0.050(6) 0.094(7) -0.008(5) -0.005(4) 0.008(4) C10A 0.056(5) 0.051(6) 0.116(9) -0.001(6) -0.003(6) 0.009(4) C11A 0.043(5) 0.061(7) 0.113(9) 0.003(6) 0.010(5) 0.014(4) C12A 0.055(5) 0.044(6) 0.123(10) -0.005(6) 0.017(6) 0.006(4) C13A 0.053(5) 0.041(5) 0.094(7) -0.013(5) 0.018(5) 0.002(4) C14A 0.065(6) 0.071(8) 0.142(12) -0.046(8) 0.027(7) -0.012(6) O6A 0.051(4) 0.073(5) 0.129(7) -0.039(5) -0.017(4) 0.007(3) C22A 0.047(8) 0.084(12) 0.079(12) -0.019(9) -0.009(6) -0.018(7) C23A 0.082(12) 0.080(13) 0.130(19) 0.006(11) 0.005(11) -0.028(9) C20A 0.091(8) 0.053(7) 0.118(10) -0.021(7) -0.042(7) 0.019(6) C21A 0.156(14) 0.061(9) 0.144(14) -0.013(8) -0.005(11) 0.054(9) C3C 0.084(7) 0.042(6) 0.073(7) -0.006(5) -0.001(5) -0.005(5) O3C 0.067(4) 0.035(4) 0.072(4) -0.005(3) -0.006(3) -0.009(3) O4C 0.157(8) 0.072(6) 0.078(6) -0.006(5) 0.012(5) -0.043(6) C4C 0.113(10) 0.042(6) 0.111(10) 0.021(6) -0.024(8) -0.029(6) C1C 0.085(7) 0.066(7) 0.060(7) -0.004(5) -0.002(5) 0.009(5) O1C 0.059(3) 0.048(4) 0.070(5) -0.001(3) 0.002(3) 0.008(3) O2C 0.107(7) 0.189(12) 0.074(6) 0.000(6) -0.027(5) 0.054(7) C2C 0.149(13) 0.088(10) 0.055(7) 0.007(6) 0.033(7) 0.025(9) C18A 0.049(5) 0.039(5) 0.079(7) 0.002(5) 0.004(4) 0.004(4) O3A 0.059(3) 0.042(4) 0.067(4) -0.005(3) 0.001(3) -0.008(3) O4A 0.076(4) 0.043(4) 0.079(5) 0.002(3) -0.001(3) -0.014(3) C19A 0.088(7) 0.049(6) 0.077(7) -0.003(5) -0.005(6) -0.011(5) O2D 0.070(4) 0.071(5) 0.076(5) 0.008(4) -0.016(3) 0.022(3) C3D 0.112(10) 0.070(9) 0.120(11) 0.040(8) -0.017(8) 0.010(7) C4D 0.083(8) 0.136(14) 0.134(13) 0.056(11) -0.016(8) 0.024(9) O1D 0.086(5) 0.056(4) 0.064(4) -0.003(3) 0.008(3) -0.013(3) C1D 0.193(17) 0.116(13) 0.060(8) -0.006(8) 0.045(9) -0.045(12) C2D 0.21(2) 0.136(17) 0.102(13) -0.012(12) 0.017(13) -0.003(15) _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 O3C 2.353(6) . ? Gd1 O1A 2.364(5) . ? Gd1 O2A 2.373(6) . ? Gd1 O4A 2.410(7) . ? Gd1 O1C 2.430(7) . ? Gd1 O2D 2.448(7) . ? Gd1 O1D 2.456(7) . ? Gd1 O5A 2.658(6) . ? Gd1 O6A 2.685(7) . ? Gd1 Cu1 3.3908(13) . ? Cu1 N1A 1.899(8) . ? Cu1 N2A 1.914(9) . ? Cu1 O2A 1.936(6) . ? Cu1 O1A 1.949(6) . ? Cu1 O3A 2.265(7) . ? O2A C8A 1.353(10) . ? O1A C1A 1.330(10) . ? O5A C2A 1.398(11) . ? O5A C20A 1.456(13) . ? N2A C14A 1.275(14) . ? N2A C15* 1.585(16) . ? N2A C15A 1.512(15) . ? N1A C7A 1.297(14) . ? N1A C17A 1.586(15) . ? N1A C17* 1.531(17) . ? C15A C17A 1.452(18) . ? C17A C25A 1.479(15) . ? C17A C24A 1.550(10) . ? C25* C15* 1.474(17) . ? C15* C17* 1.494(17) . ? C17* C24A 2.33(3) . ? C7A C6A 1.430(16) . ? C6A C5A 1.381(14) . ? C6A C1A 1.431(13) . ? C5A C4A 1.339(19) . ? C4A C3A 1.361(18) . ? C3A C2A 1.360(13) . ? C2A C1A 1.376(14) . ? C8A C13A 1.387(13) . ? C8A C9A 1.404(13) . ? C9A C10A 1.374(13) . ? C9A O6A 1.378(12) . ? C10A C11A 1.368(16) . ? C11A C12A 1.355(15) . ? C12A C13A 1.408(13) . ? C13A C14A 1.464(16) . ? O6A C22A 1.504(13) . ? O6A C22* 1.55(2) . ? C22A C23A 1.48(2) . ? C22* C23* 1.47(2) . ? C20A C21A 1.48(2) . ? C3C O4C 1.240(13) . ? C3C O3C 1.263(12) . ? C3C C4C 1.515(15) . ? C4C F9C 1.299(14) . ? C4C F7C 1.315(14) . ? C4C F7C* 1.333(14) . ? C4C F8C* 1.334(14) . ? C4C F9C* 1.340(14) . ? C4C F8C 1.380(13) . ? C1C O2C 1.187(13) . ? C1C O1C 1.236(12) . ? C1C C2C 1.537(17) . ? C2C F6C* 1.308(14) . ? C2C F5C 1.311(14) . ? C2C F6C 1.330(14) . ? C2C F4C 1.331(14) . ? C2C F4C* 1.336(15) . ? C2C F5C* 1.343(14) . ? C18A O3A 1.227(12) . ? C18A O4A 1.259(11) . ? C18A C19A 1.538(15) . ? C19A F2A 1.317(14) . ? C19A F3A* 1.323(14) . ? C19A F1A* 1.324(14) . ? C19A F3A 1.333(14) . ? C19A F1A 1.336(13) . ? C19A F2A* 1.352(14) . ? O2D C3D 1.453(14) . ? C3D C4D 1.511(18) . ? O1D C1D 1.422(14) . ? C1D C2D 1.39(2) . ? 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 O3C Gd1 O1A 136.1(2) . . ? O3C Gd1 O2A 133.4(2) . . ? O1A Gd1 O2A 66.9(2) . . ? O3C Gd1 O4A 140.9(2) . . ? O1A Gd1 O4A 74.3(2) . . ? O2A Gd1 O4A 75.1(2) . . ? O3C Gd1 O1C 77.9(2) . . ? O1A Gd1 O1C 100.8(2) . . ? O2A Gd1 O1C 146.1(2) . . ? O4A Gd1 O1C 71.1(2) . . ? O3C Gd1 O2D 77.8(2) . . ? O1A Gd1 O2D 145.2(2) . . ? O2A Gd1 O2D 96.9(2) . . ? O4A Gd1 O2D 71.7(3) . . ? O1C Gd1 O2D 75.1(2) . . ? O3C Gd1 O1D 73.7(2) . . ? O1A Gd1 O1D 76.6(2) . . ? O2A Gd1 O1D 76.6(2) . . ? O4A Gd1 O1D 145.4(2) . . ? O1C Gd1 O1D 133.3(2) . . ? O2D Gd1 O1D 131.6(3) . . ? O3C Gd1 O5A 78.9(2) . . ? O1A Gd1 O5A 61.1(2) . . ? O2A Gd1 O5A 123.3(2) . . ? O4A Gd1 O5A 109.4(2) . . ? O1C Gd1 O5A 67.5(2) . . ? O2D Gd1 O5A 139.1(2) . . ? O1D Gd1 O5A 71.1(2) . . ? O3C Gd1 O6A 77.3(2) . . ? O1A Gd1 O6A 122.7(2) . . ? O2A Gd1 O6A 59.8(2) . . ? O4A Gd1 O6A 109.0(3) . . ? O1C Gd1 O6A 135.3(2) . . ? O2D Gd1 O6A 63.7(3) . . ? O1D Gd1 O6A 72.3(3) . . ? O5A Gd1 O6A 140.5(3) . . ? O3C Gd1 Cu1 153.22(17) . . ? O1A Gd1 Cu1 34.03(15) . . ? O2A Gd1 Cu1 33.76(14) . . ? O4A Gd1 Cu1 65.83(17) . . ? O1C Gd1 Cu1 123.68(16) . . ? O2D Gd1 Cu1 120.49(19) . . ? O1D Gd1 Cu1 79.60(16) . . ? O5A Gd1 Cu1 94.40(14) . . ? O6A Gd1 Cu1 93.01(16) . . ? N1A Cu1 N2A 84.5(4) . . ? N1A Cu1 O2A 165.6(4) . . ? N2A Cu1 O2A 94.0(3) . . ? N1A Cu1 O1A 94.0(3) . . ? N2A Cu1 O1A 168.0(4) . . ? O2A Cu1 O1A 84.5(2) . . ? N1A Cu1 O3A 101.7(3) . . ? N2A Cu1 O3A 98.8(4) . . ? O2A Cu1 O3A 92.7(3) . . ? O1A Cu1 O3A 93.2(3) . . ? N1A Cu1 Gd1 136.7(3) . . ? N2A Cu1 Gd1 137.0(2) . . ? O2A Cu1 Gd1 42.92(17) . . ? O1A Cu1 Gd1 42.75(15) . . ? O3A Cu1 Gd1 86.09(16) . . ? C8A O2A Cu1 124.0(6) . . ? C8A O2A Gd1 131.7(5) . . ? Cu1 O2A Gd1 103.3(2) . . ? C1A O1A Cu1 124.7(6) . . ? C1A O1A Gd1 128.6(6) . . ? Cu1 O1A Gd1 103.2(2) . . ? C2A O5A C20A 116.7(7) . . ? C2A O5A Gd1 117.8(5) . . ? C20A O5A Gd1 125.3(6) . . ? C14A N2A C15* 115.7(11) . . ? C14A N2A C15A 121.5(10) . . ? C15* N2A C15A 29.2(10) . . ? C14A N2A Cu1 127.9(8) . . ? C15* N2A Cu1 110.4(6) . . ? C15A N2A Cu1 110.5(7) . . ? C7A N1A C17A 115.8(9) . . ? C7A N1A C17* 123.4(11) . . ? C17A N1A C17* 29.6(11) . . ? C7A N1A Cu1 126.8(7) . . ? C17A N1A Cu1 111.8(6) . . ? C17* N1A Cu1 109.7(8) . . ? C17A C15A N2A 105.0(10) . . ? C15A C17A C25A 102.8(14) . . ? C15A C17A N1A 103.8(9) . . ? C25A C17A N1A 111.5(11) . . ? C15A C17A C24A 100.3(13) . . ? C25A C17A C24A 118.0(12) . . ? N1A C17A C24A 117.3(11) . . ? C17* C15* C25* 100.9(14) . . ? C17* C15* N2A 101.6(10) . . ? C25* C15* N2A 116.2(13) . . ? C15* C17* N1A 101.0(10) . . ? C15* C17* C24A 40.9(8) . . ? N1A C17* C24A 85.2(11) . . ? C17A C24A C17* 5.1(7) . . ? N1A C7A C6A 124.9(9) . . ? C5A C6A C7A 118.1(9) . . ? C5A C6A C1A 117.5(10) . . ? C7A C6A C1A 124.2(9) . . ? C4A C5A C6A 121.9(11) . . ? C5A C4A C3A 120.9(10) . . ? C2A C3A C4A 119.5(12) . . ? C3A C2A C1A 121.7(10) . . ? C3A C2A O5A 125.2(10) . . ? C1A C2A O5A 113.0(7) . . ? O1A C1A C2A 118.8(8) . . ? O1A C1A C6A 123.0(9) . . ? C2A C1A C6A 118.2(8) . . ? O2A C8A C13A 125.2(8) . . ? O2A C8A C9A 115.3(8) . . ? C13A C8A C9A 119.4(8) . . ? C10A C9A O6A 127.0(9) . . ? C10A C9A C8A 119.4(10) . . ? O6A C9A C8A 113.6(7) . . ? C11A C10A C9A 121.5(10) . . ? C12A C11A C10A 119.8(9) . . ? C11A C12A C13A 120.9(10) . . ? C8A C13A C12A 119.0(9) . . ? C8A C13A C14A 123.4(9) . . ? C12A C13A C14A 117.3(9) . . ? N2A C14A C13A 124.1(10) . . ? C9A O6A C22A 117.8(9) . . ? C9A O6A C22* 107.1(14) . . ? C22A O6A C22* 42.9(12) . . ? C9A O6A Gd1 119.3(5) . . ? C22A O6A Gd1 121.2(7) . . ? C22* O6A Gd1 124.8(13) . . ? C23A C22A O6A 104.9(11) . . ? C23* C22* O6A 105.4(18) . . ? O5A C20A C21A 114.6(12) . . ? O4C C3C O3C 128.8(10) . . ? O4C C3C C4C 116.4(10) . . ? O3C C3C C4C 114.8(10) . . ? C3C O3C Gd1 141.4(7) . . ? F9C C4C F7C 106.2(14) . . ? F9C C4C F7C* 124.6(16) . . ? F7C C4C F7C* 22.5(11) . . ? F9C C4C F8C* 76.5(14) . . ? F7C C4C F8C* 124.6(16) . . ? F7C* C4C F8C* 112.4(15) . . ? F9C C4C F9C* 27.3(12) . . ? F7C C4C F9C* 86.9(14) . . ? F7C* C4C F9C* 108.8(15) . . ? F8C* C4C F9C* 103.3(14) . . ? F9C C4C F8C 105.9(13) . . ? F7C C4C F8C 106.5(13) . . ? F7C* C4C F8C 87.8(13) . . ? F8C* C4C F8C 30.9(11) . . ? F9C* C4C F8C 131.0(15) . . ? F9C C4C C3C 113.5(14) . . ? F7C C4C C3C 115.8(12) . . ? F7C* C4C C3C 112.0(12) . . ? F8C* C4C C3C 112.7(13) . . ? F9C* C4C C3C 107.1(14) . . ? F8C C4C C3C 108.4(10) . . ? O2C C1C O1C 129.2(12) . . ? O2C C1C C2C 115.2(11) . . ? O1C C1C C2C 115.6(10) . . ? C1C O1C Gd1 135.1(7) . . ? F6C* C2C F5C 126.0(15) . . ? F6C* C2C F6C 44.1(10) . . ? F5C C2C F6C 107.0(14) . . ? F6C* C2C F4C 59.6(12) . . ? F5C C2C F4C 111.7(14) . . ? F6C C2C F4C 103.5(13) . . ? F6C* C2C F4C* 103.6(15) . . ? F5C C2C F4C* 68.8(14) . . ? F6C C2C F4C* 139.2(17) . . ? F4C C2C F4C* 49.0(12) . . ? F6C* C2C F5C* 105.8(15) . . ? F5C C2C F5C* 39.0(11) . . ? F6C C2C F5C* 71.1(14) . . ? F4C C2C F5C* 135.3(16) . . ? F4C* C2C F5C* 105.8(15) . . ? F6C* C2C C1C 117.0(12) . . ? F5C C2C C1C 115.1(13) . . ? F6C C2C C1C 106.7(13) . . ? F4C C2C C1C 111.9(11) . . ? F4C* C2C C1C 111.6(14) . . ? F5C* C2C C1C 112.1(14) . . ? O3A C18A O4A 129.8(9) . . ? O3A C18A C19A 117.7(8) . . ? O4A C18A C19A 112.5(9) . . ? C18A O3A Cu1 117.8(6) . . ? C18A O4A Gd1 140.5(7) . . ? F2A C19A F3A* 53.8(10) . . ? F2A C19A F1A* 127.8(15) . . ? F3A* C19A F1A* 104.4(13) . . ? F2A C19A F3A 103.6(12) . . ? F3A* C19A F3A 52.4(10) . . ? F1A* C19A F3A 60.0(11) . . ? F2A C19A F1A 110.5(13) . . ? F3A* C19A F1A 131.7(13) . . ? F1A* C19A F1A 44.5(9) . . ? F3A C19A F1A 103.3(12) . . ? F2A C19A F2A* 48.1(10) . . ? F3A* C19A F2A* 100.7(12) . . ? F1A* C19A F2A* 111.1(13) . . ? F3A C19A F2A* 140.1(14) . . ? F1A C19A F2A* 71.4(11) . . ? F2A C19A C18A 117.4(11) . . ? F3A* C19A C18A 115.0(11) . . ? F1A* C19A C18A 114.8(12) . . ? F3A C19A C18A 108.6(11) . . ? F1A C19A C18A 112.2(10) . . ? F2A* C19A C18A 109.9(11) . . ? C3D O2D Gd1 128.3(8) . . ? O2D C3D C4D 110.4(12) . . ? C1D O1D Gd1 135.3(8) . . ? C2D C1D O1D 115.2(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2D H2 O2C 0.86 1.80 2.607(13) 154.9 . O1D H1 O4C 0.86 1.91 2.706(11) 152.6 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.032 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.147 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 215830' _chemical_name_common 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H38 Cu2 Dy F9 N4 O11' _chemical_formula_weight 1247.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 'P 1 21/c 1' _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 18.034(4) _cell_length_b 11.701(2) _cell_length_c 22.351(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.13(3) _cell_angle_gamma 90.00 _cell_volume 4689.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 130 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2468 _exptl_absorpt_coefficient_mu 2.574 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 0.627 _exptl_absorpt_process_details 'XEMP ver. 4.2. Siemens Analytical X-ray Inst. Inc. 1990' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM4CCD' _diffrn_measurement_method omega-phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24990 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9562 _reflns_number_gt 8439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD' _computing_cell_refinement '(Version 1.168 (release 08.03.2001 CrysAlis168 BETA))' _computing_data_reduction '(Version 1.168 (release 08.03.2001 CrysAlis168 BETA))' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0274P)^2^+12.9188P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9562 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.007 _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 0.254750(8) -0.000172(13) 0.181762(6) 0.01452(5) Uani 1 1 d . . . Cu1A Cu 0.08187(2) -0.07645(4) 0.19712(2) 0.02399(10) Uani 1 1 d . . . Cu1B Cu 0.41961(2) 0.03229(4) 0.259804(18) 0.01781(9) Uani 1 1 d . . . F1A F 0.2073(3) -0.4380(3) 0.11756(18) 0.0873(13) Uani 1 1 d . . . F2A F 0.14050(18) -0.3488(4) 0.04859(18) 0.0905(15) Uani 1 1 d . . . F3A F 0.25722(16) -0.3267(2) 0.05979(12) 0.0503(7) Uani 1 1 d . . . F1B F 0.22110(15) 0.3975(2) 0.22132(14) 0.0497(7) Uani 1 1 d . . . F2B F 0.2788(2) 0.3918(3) 0.30907(13) 0.0650(9) Uani 1 1 d . . . F3B F 0.33510(16) 0.4465(2) 0.23532(17) 0.0593(8) Uani 1 1 d . . . F1C F 0.30951(15) 0.1185(4) -0.02002(14) 0.0817(13) Uani 1 1 d . . . F2C F 0.2179(2) 0.0357(3) -0.07135(11) 0.0579(9) Uani 1 1 d . . . F3C F 0.20056(16) 0.1840(2) -0.02137(11) 0.0443(6) Uani 1 1 d . . . O1A O 0.16985(13) -0.0362(2) 0.25242(10) 0.0213(5) Uani 1 1 d . . . O2A O 0.12769(13) 0.0382(2) 0.15023(11) 0.0237(5) Uani 1 1 d . . . O3A O 0.12592(15) -0.2366(2) 0.15206(13) 0.0339(7) Uani 1 1 d . . . O4A O 0.24535(14) -0.1848(2) 0.14997(11) 0.0225(5) Uani 1 1 d . . . O1B O 0.33300(13) -0.0658(2) 0.26675(10) 0.0193(5) Uani 1 1 d . . . O2B O 0.38418(12) 0.0076(2) 0.17482(10) 0.0179(5) Uani 1 1 d . . . O3B O 0.37282(15) 0.2223(2) 0.26651(13) 0.0324(6) Uani 1 1 d . . . O4B O 0.26409(14) 0.1863(2) 0.21192(11) 0.0235(5) Uani 1 1 d . . . O1C O 0.25792(14) 0.0567(2) 0.08447(11) 0.0228(5) Uani 1 1 d . . . O2C O 0.1855(2) -0.0669(3) 0.02756(14) 0.0444(8) Uani 1 1 d . . . O1S O 0.4362(2) 0.1065(4) 0.52390(16) 0.0618(11) Uani 1 1 d . . . N1A N 0.0396(2) -0.1628(3) 0.26114(18) 0.0413(9) Uani 1 1 d . . . N2A N -0.00421(18) -0.0912(3) 0.13522(19) 0.0388(9) Uani 1 1 d . . . N1B N 0.44340(17) 0.0406(3) 0.34757(13) 0.0212(6) Uani 1 1 d . . . N2B N 0.51357(16) 0.0992(2) 0.23836(13) 0.0210(6) Uani 1 1 d . . . C1A C 0.1660(2) -0.0107(3) 0.31018(16) 0.0206(7) Uani 1 1 d . . . C2A C 0.2183(2) 0.0637(3) 0.34061(16) 0.0214(7) Uani 1 1 d . . . H42A H 0.2555 0.0987 0.3190 0.026 Uiso 1 1 d R . . C3A C 0.2167(2) 0.0885(4) 0.40049(18) 0.0324(9) Uani 1 1 d . . . H50A H 0.2536 0.1387 0.4202 0.039 Uiso 1 1 d R . . C4A C 0.1631(3) 0.0412(5) 0.4328(2) 0.0477(12) Uani 1 1 d . . . H68A H 0.1630 0.0576 0.4749 0.057 Uiso 1 1 d R . . C5A C 0.1117(3) -0.0319(5) 0.4043(2) 0.0534(14) Uani 1 1 d . . . H72A H 0.0732 -0.0630 0.4261 0.064 Uiso 1 1 d R . . C6A C 0.1112(3) -0.0592(4) 0.34301(18) 0.0348(10) Uani 1 1 d . . . C7A C 0.0567(3) -0.1401(4) 0.3170(2) 0.0475(13) Uani 1 1 d . . . H20A H 0.0296 -0.1810 0.3448 0.057 Uiso 1 1 d R . . C8A C 0.0903(2) 0.1121(3) 0.11236(15) 0.0239(8) Uani 1 1 d . . . C9A C 0.1207(2) 0.2188(4) 0.10244(17) 0.0286(8) Uani 1 1 d . . . H39A H 0.1676 0.2402 0.1240 0.034 Uiso 1 1 d R . . C10A C 0.0843(2) 0.2944(4) 0.06153(19) 0.0376(10) Uani 1 1 d . . . H53A H 0.1059 0.3681 0.0559 0.045 Uiso 1 1 d R . . C11A C 0.0175(3) 0.2666(4) 0.02910(19) 0.0425(12) Uani 1 1 d . . . H56A H -0.0058 0.3187 -0.0003 0.051 Uiso 1 1 d R . . C12A C -0.0144(3) 0.1634(5) 0.0394(2) 0.0448(12) Uani 1 1 d . . . H47A H -0.0613 0.1443 0.0172 0.054 Uiso 1 1 d R . . C13A C 0.0200(2) 0.0842(4) 0.08200(18) 0.0335(9) Uani 1 1 d . . . C14A C -0.0195(2) -0.0198(4) 0.0920(2) 0.0422(12) Uani 1 1 d . . . H64A H -0.0617 -0.0372 0.0636 0.051 Uiso 1 1 d R . . C15A C -0.0505(3) -0.1949(5) 0.1362(3) 0.0536(14) Uani 1 1 d . . . H78A H -0.0225 -0.2601 0.1255 0.064 Uiso 1 1 d R . . H78B H -0.0928 -0.1868 0.1066 0.064 Uiso 1 1 d R . . C16A C -0.0763(3) -0.2144(5) 0.1978(3) 0.071(2) Uani 1 1 d . . . H76A H -0.0971 -0.1445 0.2111 0.085 Uiso 1 1 d R . . H76B H -0.1153 -0.2706 0.1940 0.085 Uiso 1 1 d R . . C17A C -0.0152(3) -0.2540(5) 0.2447(3) 0.0592(16) Uani 1 1 d . . . H73A H -0.0370 -0.2769 0.2802 0.071 Uiso 1 1 d R . . H73B H 0.0092 -0.3194 0.2298 0.071 Uiso 1 1 d R . . C18A C 0.1882(2) -0.2434(3) 0.13448(16) 0.0233(8) Uani 1 1 d . . . C19A C 0.1985(2) -0.3400(4) 0.0893(2) 0.0333(9) Uani 1 1 d . . . C1B C 0.32401(19) -0.1347(3) 0.31292(15) 0.0200(7) Uani 1 1 d . . . C2B C 0.2753(2) -0.2282(3) 0.30475(17) 0.0235(7) Uani 1 1 d . . . H51A H 0.2518 -0.2451 0.2652 0.028 Uiso 1 1 d R . . C3B C 0.2606(2) -0.2959(3) 0.35274(19) 0.0321(9) Uani 1 1 d . . . H71A H 0.2275 -0.3599 0.3458 0.039 Uiso 1 1 d R . . C4B C 0.2936(3) -0.2724(4) 0.41079(19) 0.0376(10) Uani 1 1 d . . . H69A H 0.2823 -0.3182 0.4443 0.045 Uiso 1 1 d R . . C5B C 0.3428(2) -0.1832(4) 0.41921(17) 0.0328(9) Uani 1 1 d . . . H36A H 0.3657 -0.1668 0.4590 0.039 Uiso 1 1 d R . . C6B C 0.3607(2) -0.1146(3) 0.37094(16) 0.0230(7) Uani 1 1 d . . . C7B C 0.4140(2) -0.0234(3) 0.38505(16) 0.0233(8) Uani 1 1 d . . . H16A H 0.4297 -0.0107 0.4269 0.028 Uiso 1 1 d R . . C8B C 0.42969(19) -0.0282(3) 0.13512(15) 0.0172(7) Uani 1 1 d . . . C9B C 0.40237(19) -0.0959(3) 0.08605(15) 0.0193(7) Uani 1 1 d . . . H49A H 0.3507 -0.1177 0.0814 0.023 Uiso 1 1 d R . . C10B C 0.4485(2) -0.1312(3) 0.04420(16) 0.0229(7) Uani 1 1 d . . . H30A H 0.4281 -0.1768 0.0107 0.028 Uiso 1 1 d R . . C11B C 0.5239(2) -0.1021(3) 0.04994(17) 0.0264(8) Uani 1 1 d . . . H43A H 0.5557 -0.1274 0.0207 0.032 Uiso 1 1 d R . . C12B C 0.5515(2) -0.0359(3) 0.09785(17) 0.0244(8) Uani 1 1 d . . . H25A H 0.6032 -0.0149 0.1020 0.029 Uiso 1 1 d R . . C13B C 0.50653(19) 0.0015(3) 0.14121(15) 0.0182(7) Uani 1 1 d . . . C14B C 0.54022(19) 0.0738(3) 0.18942(16) 0.0211(7) Uani 1 1 d . . . H15A H 0.5880 0.1060 0.1839 0.025 Uiso 1 1 d R . . C15B C 0.5567(2) 0.1784(3) 0.27977(18) 0.0283(8) Uani 1 1 d . . . H44A H 0.5311 0.2503 0.2796 0.034 Uiso 1 1 d R . . H44B H 0.6045 0.1915 0.2658 0.034 Uiso 1 1 d R . . C16B C 0.5668(2) 0.1328(3) 0.34366(17) 0.0278(8) Uani 1 1 d . . . H54A H 0.6027 0.1794 0.3672 0.033 Uiso 1 1 d R . . H54B H 0.5866 0.0567 0.3429 0.033 Uiso 1 1 d R . . C17B C 0.4950(2) 0.1304(3) 0.37339(18) 0.0284(8) Uani 1 1 d . . . H62A H 0.5067 0.1167 0.4157 0.034 Uiso 1 1 d R . . H62B H 0.4710 0.2035 0.3686 0.034 Uiso 1 1 d R . . C18B C 0.3111(2) 0.2479(3) 0.24270(16) 0.0204(7) Uani 1 1 d . . . C19B C 0.2854(2) 0.3717(3) 0.25190(18) 0.0264(8) Uani 1 1 d . . . C1C C 0.2253(2) 0.0157(3) 0.03592(16) 0.0228(8) Uani 1 1 d . . . C2C C 0.2394(2) 0.0876(4) -0.01958(16) 0.0267(8) Uani 1 1 d . . . C1S C 0.3176(3) 0.1167(5) 0.5650(3) 0.0595(16) Uani 1 1 d . . . H1AA H 0.3003 0.0639 0.5337 0.071 Uiso 1 1 d R . . H1AB H 0.3132 0.0824 0.6035 0.071 Uiso 1 1 d R . . H1AC H 0.2881 0.1850 0.5610 0.071 Uiso 1 1 d R . . C2S C 0.4326(3) 0.2284(5) 0.6070(3) 0.0605(16) Uani 1 1 d . . . H2AA H 0.4837 0.2424 0.6006 0.073 Uiso 1 1 d R . . H2AB H 0.4054 0.2990 0.6038 0.073 Uiso 1 1 d R . . H2AC H 0.4306 0.1964 0.6463 0.073 Uiso 1 1 d R . . C3S C 0.3996(3) 0.1467(4) 0.56028(19) 0.0353(9) 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 0.01152(8) 0.01805(8) 0.01372(8) 0.00017(6) 0.00011(5) -0.00172(6) Cu1A 0.0154(2) 0.0267(2) 0.0302(2) -0.00655(19) 0.00408(17) -0.00685(17) Cu1B 0.01338(19) 0.0223(2) 0.0172(2) -0.00107(16) -0.00110(15) -0.00141(16) F1A 0.145(4) 0.0265(16) 0.101(3) 0.0068(17) 0.063(3) 0.0259(19) F2A 0.0496(19) 0.118(3) 0.096(3) -0.084(3) -0.0262(18) 0.015(2) F3A 0.0541(17) 0.0539(17) 0.0459(16) -0.0219(13) 0.0195(13) -0.0011(14) F1B 0.0349(14) 0.0298(13) 0.080(2) -0.0042(13) -0.0161(14) 0.0106(11) F2B 0.101(3) 0.0538(19) 0.0413(16) -0.0168(14) 0.0112(16) 0.0297(18) F3B 0.0475(17) 0.0241(13) 0.108(3) 0.0040(15) 0.0181(17) -0.0132(12) F1C 0.0218(13) 0.176(4) 0.0492(18) 0.043(2) 0.0119(12) -0.0057(19) F2C 0.107(3) 0.0497(16) 0.0163(12) -0.0042(11) 0.0021(14) 0.0129(17) F3C 0.0676(18) 0.0329(14) 0.0338(14) 0.0107(11) 0.0126(12) 0.0147(13) O1A 0.0196(12) 0.0285(13) 0.0166(12) -0.0025(10) 0.0049(9) -0.0065(10) O2A 0.0143(12) 0.0323(14) 0.0232(13) 0.0053(11) -0.0036(10) 0.0013(10) O3A 0.0275(15) 0.0331(15) 0.0422(17) -0.0114(13) 0.0092(13) -0.0035(12) O4A 0.0228(13) 0.0201(12) 0.0238(13) -0.0007(10) -0.0010(10) -0.0021(10) O1B 0.0198(12) 0.0225(13) 0.0154(11) 0.0038(9) 0.0015(9) -0.0023(10) O2B 0.0122(11) 0.0260(13) 0.0150(11) -0.0004(9) -0.0006(9) -0.0013(9) O3B 0.0255(14) 0.0308(15) 0.0387(16) -0.0053(12) -0.0070(12) 0.0047(12) O4B 0.0231(13) 0.0182(12) 0.0285(14) -0.0017(10) -0.0001(10) -0.0052(10) O1C 0.0220(13) 0.0286(14) 0.0174(12) 0.0003(10) -0.0001(10) 0.0027(10) O2C 0.064(2) 0.0351(17) 0.0316(16) 0.0003(13) -0.0076(15) -0.0145(16) O1S 0.069(3) 0.080(3) 0.0363(19) -0.0176(19) 0.0048(17) 0.012(2) N1A 0.042(2) 0.039(2) 0.047(2) -0.0119(17) 0.0242(18) -0.0230(17) N2A 0.0180(16) 0.036(2) 0.061(3) -0.0178(18) -0.0034(16) -0.0040(14) N1B 0.0224(15) 0.0225(15) 0.0174(14) -0.0047(12) -0.0038(11) 0.0045(12) N2B 0.0157(14) 0.0198(15) 0.0265(16) -0.0008(12) -0.0027(12) 0.0002(11) C1A 0.0233(17) 0.0208(17) 0.0186(16) -0.0001(13) 0.0064(13) 0.0038(14) C2A 0.0229(18) 0.0210(18) 0.0206(17) 0.0026(14) 0.0039(14) 0.0074(14) C3A 0.040(2) 0.029(2) 0.027(2) -0.0062(17) 0.0044(17) 0.0048(18) C4A 0.069(3) 0.053(3) 0.025(2) -0.012(2) 0.019(2) -0.009(3) C5A 0.068(4) 0.061(3) 0.037(3) -0.006(2) 0.034(3) -0.018(3) C6A 0.044(2) 0.036(2) 0.028(2) -0.0039(17) 0.0200(18) -0.0095(19) C7A 0.061(3) 0.042(3) 0.046(3) -0.008(2) 0.035(2) -0.024(2) C8A 0.0203(17) 0.038(2) 0.0134(16) -0.0043(15) 0.0022(13) 0.0102(15) C9A 0.0244(19) 0.040(2) 0.0229(18) 0.0067(16) 0.0087(15) 0.0101(17) C10A 0.037(2) 0.049(3) 0.029(2) 0.0104(19) 0.0138(18) 0.021(2) C11A 0.047(3) 0.058(3) 0.023(2) 0.004(2) 0.0018(18) 0.031(2) C12A 0.034(2) 0.064(3) 0.032(2) -0.017(2) -0.0149(19) 0.025(2) C13A 0.027(2) 0.043(2) 0.029(2) -0.0150(18) -0.0069(16) 0.0128(18) C14A 0.020(2) 0.049(3) 0.053(3) -0.023(2) -0.0141(19) 0.0078(19) C15A 0.029(2) 0.047(3) 0.080(4) -0.020(3) -0.013(2) -0.010(2) C16A 0.030(3) 0.059(4) 0.128(6) -0.032(4) 0.024(3) -0.027(3) C17A 0.069(4) 0.051(3) 0.064(3) -0.016(3) 0.032(3) -0.041(3) C18A 0.0266(19) 0.0202(18) 0.0218(17) -0.0004(14) -0.0030(15) 0.0001(14) C19A 0.028(2) 0.029(2) 0.042(2) -0.0115(18) 0.0011(18) -0.0005(17) C1B 0.0184(16) 0.0223(17) 0.0196(17) 0.0029(14) 0.0038(13) 0.0079(14) C2B 0.0227(18) 0.0228(18) 0.0249(18) 0.0031(15) 0.0023(14) 0.0015(14) C3B 0.036(2) 0.025(2) 0.036(2) 0.0100(17) 0.0065(18) 0.0006(17) C4B 0.048(3) 0.034(2) 0.031(2) 0.0144(18) 0.0045(19) 0.0030(19) C5B 0.044(2) 0.034(2) 0.0194(18) 0.0072(16) -0.0033(17) 0.0060(18) C6B 0.0251(18) 0.0234(18) 0.0204(17) 0.0034(14) 0.0022(14) 0.0066(14) C7B 0.0262(18) 0.0270(19) 0.0157(16) -0.0009(14) -0.0023(14) 0.0088(15) C8B 0.0173(16) 0.0187(16) 0.0156(15) 0.0079(13) 0.0014(12) 0.0020(13) C9B 0.0166(16) 0.0176(17) 0.0236(17) 0.0039(13) 0.0017(13) 0.0009(13) C10B 0.0269(19) 0.0191(17) 0.0226(17) 0.0012(14) 0.0020(14) 0.0003(14) C11B 0.0222(18) 0.030(2) 0.0278(19) 0.0023(16) 0.0076(15) 0.0030(15) C12B 0.0148(16) 0.0295(19) 0.0293(19) 0.0043(16) 0.0045(14) 0.0006(14) C13B 0.0151(15) 0.0192(16) 0.0202(16) 0.0029(13) 0.0011(13) 0.0012(13) C14B 0.0135(15) 0.0227(17) 0.0268(18) 0.0035(14) 0.0002(13) 0.0011(13) C15B 0.0229(19) 0.0238(19) 0.037(2) -0.0057(16) -0.0026(16) -0.0040(15) C16B 0.0226(18) 0.0247(19) 0.033(2) -0.0094(16) -0.0103(16) 0.0015(15) C17B 0.028(2) 0.029(2) 0.0268(19) -0.0097(16) -0.0043(16) -0.0017(16) C18B 0.0228(18) 0.0168(16) 0.0222(17) 0.0003(13) 0.0048(14) -0.0014(14) C19B 0.0247(19) 0.0208(18) 0.033(2) -0.0040(15) -0.0001(15) -0.0030(15) C1C 0.0202(17) 0.030(2) 0.0175(17) 0.0000(14) 0.0002(13) 0.0077(15) C2C 0.0221(18) 0.039(2) 0.0191(17) 0.0021(16) 0.0033(14) 0.0073(16) C1S 0.051(3) 0.047(3) 0.072(4) 0.023(3) -0.030(3) -0.015(2) C2S 0.045(3) 0.041(3) 0.097(5) -0.037(3) 0.015(3) -0.006(2) C3S 0.045(3) 0.026(2) 0.033(2) 0.0035(17) -0.0012(19) -0.0008(18) _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 O4A 2.275(2) . ? Dy1 O1C 2.281(2) . ? Dy1 O4B 2.285(2) . ? Dy1 O1A 2.352(2) . ? Dy1 O2B 2.357(2) . ? Dy1 O2A 2.367(2) . ? Dy1 O1B 2.370(2) . ? Dy1 Cu1A 3.2959(8) . ? Dy1 Cu1B 3.3043(11) . ? Cu1A O2A 1.941(3) . ? Cu1A O1A 1.962(2) . ? Cu1A N1A 1.970(4) . ? Cu1A N2A 1.974(4) . ? Cu1A O3A 2.308(3) . ? Cu1B O1B 1.958(2) . ? Cu1B O2B 1.960(2) . ? Cu1B N1B 1.965(3) . ? Cu1B N2B 1.972(3) . ? Cu1B O3B 2.389(3) . ? F1A C19A 1.310(5) . ? F2A C19A 1.316(5) . ? F3A C19A 1.315(5) . ? F1B C19B 1.318(4) . ? F2B C19B 1.317(5) . ? F3B C19B 1.333(5) . ? F1C C2C 1.316(5) . ? F2C C2C 1.327(5) . ? F3C C2C 1.326(5) . ? O1A C1A 1.334(4) . ? O2A C8A 1.341(4) . ? O3A C18A 1.232(5) . ? O4A C18A 1.255(4) . ? O1B C1B 1.333(4) . ? O2B C8B 1.339(4) . ? O3B C18B 1.218(4) . ? O4B C18B 1.260(4) . ? O1C C1C 1.272(4) . ? O2C C1C 1.206(5) . ? O1S C3S 1.196(6) . ? N1A C7A 1.281(6) . ? N1A C17A 1.475(5) . ? N2A C14A 1.284(6) . ? N2A C15A 1.475(6) . ? N1B C7B 1.280(5) . ? N1B C17B 1.480(5) . ? N2B C14B 1.276(5) . ? N2B C15B 1.472(5) . ? C1A C2A 1.404(5) . ? C1A C6A 1.411(5) . ? C2A C3A 1.373(5) . ? C3A C4A 1.382(6) . ? C4A C5A 1.368(7) . ? C5A C6A 1.406(6) . ? C6A C7A 1.441(6) . ? C8A C9A 1.391(6) . ? C8A C13A 1.410(5) . ? C9A C10A 1.386(5) . ? C10A C11A 1.377(7) . ? C11A C12A 1.368(7) . ? C12A C13A 1.422(6) . ? C13A C14A 1.440(7) . ? C15A C16A 1.516(9) . ? C16A C17A 1.510(9) . ? C18A C19A 1.540(5) . ? C1B C2B 1.402(5) . ? C1B C6B 1.411(5) . ? C2B C3B 1.382(5) . ? C3B C4B 1.396(6) . ? C4B C5B 1.369(6) . ? C5B C6B 1.410(5) . ? C6B C7B 1.448(5) . ? C8B C9B 1.399(5) . ? C8B C13B 1.421(5) . ? C9B C10B 1.380(5) . ? C10B C11B 1.395(5) . ? C11B C12B 1.371(5) . ? C12B C13B 1.399(5) . ? C13B C14B 1.451(5) . ? C15B C16B 1.517(6) . ? C16B C17B 1.517(6) . ? C18B C19B 1.541(5) . ? C1C C2C 1.542(5) . ? C1S C3S 1.534(7) . ? C2S C3S 1.491(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 O4A Dy1 O1C 89.30(9) . . ? O4A Dy1 O4B 178.96(9) . . ? O1C Dy1 O4B 89.66(9) . . ? O4A Dy1 O1A 90.44(9) . . ? O1C Dy1 O1A 140.97(9) . . ? O4B Dy1 O1A 90.32(9) . . ? O4A Dy1 O2B 93.28(9) . . ? O1C Dy1 O2B 78.48(9) . . ? O4B Dy1 O2B 86.58(9) . . ? O1A Dy1 O2B 140.46(8) . . ? O4A Dy1 O2A 92.84(9) . . ? O1C Dy1 O2A 77.46(9) . . ? O4B Dy1 O2A 86.86(9) . . ? O1A Dy1 O2A 63.58(9) . . ? O2B Dy1 O2A 155.07(8) . . ? O4A Dy1 O1B 87.75(8) . . ? O1C Dy1 O1B 141.75(8) . . ? O4B Dy1 O1B 93.12(9) . . ? O1A Dy1 O1B 77.20(8) . . ? O2B Dy1 O1B 63.66(8) . . ? O2A Dy1 O1B 140.77(8) . . ? O4A Dy1 Cu1A 74.67(6) . . ? O1C Dy1 Cu1A 107.37(7) . . ? O4B Dy1 Cu1A 105.58(6) . . ? O1A Dy1 Cu1A 35.98(6) . . ? O2B Dy1 Cu1A 166.28(6) . . ? O2A Dy1 Cu1A 35.52(6) . . ? O1B Dy1 Cu1A 108.52(6) . . ? O4A Dy1 Cu1B 107.87(6) . . ? O1C Dy1 Cu1B 110.92(7) . . ? O4B Dy1 Cu1B 72.58(6) . . ? O1A Dy1 Cu1B 106.24(6) . . ? O2B Dy1 Cu1B 35.80(6) . . ? O2A Dy1 Cu1B 157.39(7) . . ? O1B Dy1 Cu1B 35.81(6) . . ? Cu1A Dy1 Cu1B 141.623(16) . . ? O2A Cu1A O1A 79.15(10) . . ? O2A Cu1A N1A 165.17(13) . . ? O1A Cu1A N1A 90.85(14) . . ? O2A Cu1A N2A 91.75(14) . . ? O1A Cu1A N2A 170.20(14) . . ? N1A Cu1A N2A 97.37(17) . . ? O2A Cu1A O3A 98.01(11) . . ? O1A Cu1A O3A 100.21(10) . . ? N1A Cu1A O3A 94.50(14) . . ? N2A Cu1A O3A 84.52(13) . . ? O2A Cu1A Dy1 45.13(7) . . ? O1A Cu1A Dy1 44.78(7) . . ? N1A Cu1A Dy1 131.13(13) . . ? N2A Cu1A Dy1 129.25(12) . . ? O3A Cu1A Dy1 78.52(7) . . ? O1B Cu1B O2B 79.05(10) . . ? O1B Cu1B N1B 92.34(12) . . ? O2B Cu1B N1B 171.35(12) . . ? O1B Cu1B N2B 164.95(11) . . ? O2B Cu1B N2B 91.30(11) . . ? N1B Cu1B N2B 96.97(13) . . ? O1B Cu1B O3B 104.52(10) . . ? O2B Cu1B O3B 96.74(10) . . ? N1B Cu1B O3B 86.12(11) . . ? N2B Cu1B O3B 87.94(11) . . ? O1B Cu1B Dy1 45.10(7) . . ? O2B Cu1B Dy1 44.73(7) . . ? N1B Cu1B Dy1 128.38(9) . . ? N2B Cu1B Dy1 131.72(9) . . ? O3B Cu1B Dy1 80.57(6) . . ? C1A O1A Cu1A 122.8(2) . . ? C1A O1A Dy1 135.6(2) . . ? Cu1A O1A Dy1 99.25(10) . . ? C8A O2A Cu1A 124.9(2) . . ? C8A O2A Dy1 135.7(2) . . ? Cu1A O2A Dy1 99.36(10) . . ? C18A O3A Cu1A 124.1(2) . . ? C18A O4A Dy1 129.5(2) . . ? C1B O1B Cu1B 125.5(2) . . ? C1B O1B Dy1 134.8(2) . . ? Cu1B O1B Dy1 99.09(10) . . ? C8B O2B Cu1B 121.9(2) . . ? C8B O2B Dy1 135.5(2) . . ? Cu1B O2B Dy1 99.47(10) . . ? C18B O3B Cu1B 120.9(2) . . ? C18B O4B Dy1 137.0(2) . . ? C1C O1C Dy1 130.3(2) . . ? C7A N1A C17A 118.5(4) . . ? C7A N1A Cu1A 122.0(3) . . ? C17A N1A Cu1A 119.4(3) . . ? C14A N2A C15A 118.1(4) . . ? C14A N2A Cu1A 124.0(3) . . ? C15A N2A Cu1A 117.8(3) . . ? C7B N1B C17B 116.6(3) . . ? C7B N1B Cu1B 124.3(3) . . ? C17B N1B Cu1B 119.1(2) . . ? C14B N2B C15B 117.6(3) . . ? C14B N2B Cu1B 121.9(2) . . ? C15B N2B Cu1B 120.5(2) . . ? O1A C1A C2A 120.3(3) . . ? O1A C1A C6A 121.7(3) . . ? C2A C1A C6A 117.9(3) . . ? C3A C2A C1A 121.4(4) . . ? C2A C3A C4A 120.9(4) . . ? C5A C4A C3A 119.0(4) . . ? C4A C5A C6A 121.9(4) . . ? C5A C6A C1A 118.9(4) . . ? C5A C6A C7A 118.4(4) . . ? C1A C6A C7A 122.6(4) . . ? N1A C7A C6A 127.7(4) . . ? O2A C8A C9A 119.9(3) . . ? O2A C8A C13A 121.4(4) . . ? C9A C8A C13A 118.7(4) . . ? C10A C9A C8A 120.7(4) . . ? C11A C10A C9A 121.5(5) . . ? C12A C11A C10A 118.7(4) . . ? C11A C12A C13A 121.8(4) . . ? C8A C13A C12A 118.5(4) . . ? C8A C13A C14A 123.7(4) . . ? C12A C13A C14A 117.8(4) . . ? N2A C14A C13A 126.6(4) . . ? N2A C15A C16A 111.5(4) . . ? C17A C16A C15A 113.9(4) . . ? N1A C17A C16A 111.8(5) . . ? O3A C18A O4A 128.8(4) . . ? O3A C18A C19A 115.8(3) . . ? O4A C18A C19A 115.4(3) . . ? F1A C19A F2A 108.1(4) . . ? F1A C19A F3A 106.5(4) . . ? F2A C19A F3A 106.6(4) . . ? F1A C19A C18A 110.1(4) . . ? F2A C19A C18A 111.6(3) . . ? F3A C19A C18A 113.7(3) . . ? O1B C1B C2B 119.8(3) . . ? O1B C1B C6B 121.8(3) . . ? C2B C1B C6B 118.4(3) . . ? C3B C2B C1B 121.0(4) . . ? C2B C3B C4B 120.7(4) . . ? C5B C4B C3B 118.9(4) . . ? C4B C5B C6B 121.8(4) . . ? C5B C6B C1B 119.0(4) . . ? C5B C6B C7B 117.0(3) . . ? C1B C6B C7B 124.0(3) . . ? N1B C7B C6B 126.9(3) . . ? O2B C8B C9B 120.5(3) . . ? O2B C8B C13B 121.3(3) . . ? C9B C8B C13B 118.2(3) . . ? C10B C9B C8B 120.9(3) . . ? C9B C10B C11B 121.1(3) . . ? C12B C11B C10B 118.6(3) . . ? C11B C12B C13B 122.0(3) . . ? C12B C13B C8B 119.2(3) . . ? C12B C13B C14B 118.0(3) . . ? C8B C13B C14B 122.7(3) . . ? N2B C14B C13B 127.3(3) . . ? N2B C15B C16B 111.9(3) . . ? C17B C16B C15B 113.4(3) . . ? N1B C17B C16B 111.9(3) . . ? O3B C18B O4B 128.9(3) . . ? O3B C18B C19B 116.5(3) . . ? O4B C18B C19B 114.6(3) . . ? F2B C19B F1B 107.2(3) . . ? F2B C19B F3B 106.6(3) . . ? F1B C19B F3B 106.6(3) . . ? F2B C19B C18B 110.9(3) . . ? F1B C19B C18B 114.0(3) . . ? F3B C19B C18B 111.1(3) . . ? O2C C1C O1C 130.4(4) . . ? O2C C1C C2C 117.3(3) . . ? O1C C1C C2C 112.3(3) . . ? F1C C2C F2C 108.1(3) . . ? F1C C2C F3C 105.7(4) . . ? F2C C2C F3C 105.0(3) . . ? F1C C2C C1C 113.4(3) . . ? F2C C2C C1C 113.2(3) . . ? F3C C2C C1C 110.9(3) . . ? O1S C3S C2S 121.3(5) . . ? O1S C3S C1S 124.2(5) . . ? C2S C3S C1S 114.5(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.559 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.101 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 215831' _chemical_name_common 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H32.34 Cu2 F9 Gd N4 O10.17' _chemical_formula_weight 1187.09 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' Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 12.528(3) _cell_length_b 25.531(5) _cell_length_c 14.391(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.48(3) _cell_angle_gamma 90.00 _cell_volume 4598.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 5961 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description prism _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2339 _exptl_absorpt_coefficient_mu 2.437 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.529 _exptl_absorpt_correction_T_max 0.641 _exptl_absorpt_process_details 'XEMP ver. 4.2. Siemens Analytical X-ray Inst. Inc. 1990' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16579 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0740 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7653 _reflns_number_gt 6195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (2201) COLLECT Nonius BV, Delft, The Netherlands' _computing_cell_refinement 'Nonius Software' _computing_data_reduction 'Nonius Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0183P)^2^+66.1385P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7653 _refine_ls_number_parameters 624 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0879 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.001 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 0.28661(4) 0.60706(2) 0.21665(4) 0.02880(16) Uani 1 1 d . . . Cu1A Cu 0.44829(10) 0.64890(5) 0.38930(10) 0.0298(3) Uani 1 1 d . . . Cu1B Cu 0.10163(10) 0.63551(5) 0.04961(9) 0.0292(3) Uani 1 1 d . . . F1A F 0.6123(7) 0.7092(3) 0.1153(7) 0.080(3) Uani 1 1 d . . . F2A F 0.6166(6) 0.6386(4) 0.0395(6) 0.073(3) Uani 1 1 d . . . F3A F 0.7189(5) 0.6485(4) 0.1596(6) 0.079(3) Uani 1 1 d . . . F1B F -0.0659(9) 0.6715(4) 0.3551(8) 0.132(5) Uani 1 1 d D . . F2B F -0.0268(7) 0.5977(6) 0.4073(7) 0.138(6) Uani 1 1 d D . . F3B F -0.1512(5) 0.6060(3) 0.3057(5) 0.066(2) Uani 1 1 d D . . F1C F 0.4389(9) 0.4264(3) 0.2543(8) 0.079(4) Uani 0.809(8) 1 d P . . F2C F 0.3515(7) 0.4220(3) 0.1255(6) 0.052(3) Uani 0.809(8) 1 d P . . F3C F 0.2708(9) 0.4099(4) 0.2493(8) 0.073(3) Uani 0.809(8) 1 d P . . O1W O -0.166(3) 0.7639(15) 0.220(3) 0.035(10) Uiso 0.17 1 d PD . . H1W1 H -0.1744 0.7475 0.2712 0.042 Uiso 0.17 1 d PRD . . H2W1 H -0.1049 0.7595 0.1961 0.042 Uiso 0.17 1 d PRD . . O1A O 0.3562(6) 0.5880(3) 0.3710(5) 0.0311(18) Uani 1 1 d . . . O2A O 0.3324(6) 0.6815(3) 0.3144(5) 0.0321(18) Uani 1 1 d . . . O3A O 0.5616(6) 0.6298(3) 0.2693(6) 0.046(2) Uani 1 1 d . . . O4A O 0.4430(6) 0.6330(3) 0.1460(6) 0.041(2) Uani 1 1 d . . . O1B O 0.2102(5) 0.6766(3) 0.1189(5) 0.0297(17) Uani 1 1 d . . . O2B O 0.2132(6) 0.5825(3) 0.0676(5) 0.0330(18) Uani 1 1 d . . . O3B O -0.0108(6) 0.6163(3) 0.1738(6) 0.044(2) Uani 1 1 d . . . O4B O 0.1204(6) 0.6160(3) 0.2845(6) 0.045(2) Uani 1 1 d . . . O1C O 0.2237(8) 0.5131(3) 0.2304(6) 0.064(3) Uani 1 1 d D . . O2C O 0.4020(6) 0.5286(3) 0.2043(6) 0.022(2) Uani 0.809(8) 1 d P . . N1A N 0.5436(7) 0.6103(3) 0.4766(7) 0.035(2) Uani 1 1 d . . . N2A N 0.5224(7) 0.7161(4) 0.4047(7) 0.036(2) Uani 1 1 d . . . N1B N 0.0117(7) 0.6977(3) 0.0249(6) 0.030(2) Uani 1 1 d . . . N2B N 0.0122(7) 0.5865(3) -0.0258(7) 0.034(2) Uani 1 1 d . . . C1A C 0.3327(8) 0.5587(4) 0.4443(8) 0.031(3) Uani 1 1 d . . . C2A C 0.2313(10) 0.5355(5) 0.4475(9) 0.043(3) Uani 1 1 d . . . H2A H 0.1820 0.5400 0.3979 0.052 Uiso 1 1 calc R . . C3A C 0.2048(10) 0.5068(5) 0.5215(10) 0.052(4) Uani 1 1 d . . . H3A H 0.1365 0.4925 0.5221 0.062 Uiso 1 1 calc R . . C4A C 0.2751(12) 0.4976(5) 0.5972(9) 0.057(4) Uani 1 1 d . . . H4A H 0.2550 0.4778 0.6477 0.068 Uiso 1 1 calc R . . C5A C 0.3746(11) 0.5189(5) 0.5943(9) 0.048(3) Uani 1 1 d . . . H5A H 0.4236 0.5128 0.6435 0.057 Uiso 1 1 calc R . . C6A C 0.4052(9) 0.5497(4) 0.5194(8) 0.032(3) Uani 1 1 d . . . C7A C 0.5121(9) 0.5717(4) 0.5218(8) 0.040(3) Uani 1 1 d . . . H7A H 0.5628 0.5553 0.5610 0.048 Uiso 1 1 calc R . . C8A C 0.2959(9) 0.7296(4) 0.3323(7) 0.029(2) Uani 1 1 d . . . C9A C 0.1903(8) 0.7428(4) 0.3082(8) 0.031(3) Uani 1 1 d . . . H9A H 0.1433 0.7171 0.2858 0.037 Uiso 1 1 calc R . . C10A C 0.1557(9) 0.7928(5) 0.3173(9) 0.041(3) Uani 1 1 d . . . H10A H 0.0856 0.8009 0.2986 0.049 Uiso 1 1 calc R . . C11A C 0.2215(11) 0.8326(5) 0.3538(9) 0.048(3) Uani 1 1 d . . . H11A H 0.1962 0.8666 0.3598 0.058 Uiso 1 1 calc R . . C12A C 0.3259(10) 0.8197(4) 0.3808(8) 0.039(3) Uani 1 1 d . . . H12A H 0.3709 0.8455 0.4059 0.047 Uiso 1 1 calc R . . C13A C 0.3647(8) 0.7690(4) 0.3710(8) 0.032(3) Uani 1 1 d . . . C14A C 0.4746(9) 0.7602(4) 0.3975(7) 0.031(3) Uani 1 1 d . . . H14A H 0.5157 0.7898 0.4109 0.038 Uiso 1 1 calc R . . C15A C 0.6389(9) 0.7174(5) 0.4252(9) 0.041(3) Uani 1 1 d . . . H17A H 0.6606 0.7531 0.4392 0.049 Uiso 1 1 calc R . . H17B H 0.6755 0.7062 0.3706 0.049 Uiso 1 1 calc R . . C16A C 0.6720(9) 0.6825(5) 0.5064(9) 0.047(3) Uani 1 1 d . . . H16C H 0.7465 0.6891 0.5234 0.057 Uiso 1 1 calc R . . H16D H 0.6304 0.6919 0.5592 0.057 Uiso 1 1 calc R . . C17A C 0.6580(9) 0.6247(5) 0.4876(10) 0.045(3) Uani 1 1 d . . . H15A H 0.6938 0.6155 0.4314 0.054 Uiso 1 1 calc R . . H15B H 0.6910 0.6049 0.5387 0.054 Uiso 1 1 calc R . . C18A C 0.5337(9) 0.6369(4) 0.1883(9) 0.034(3) Uani 1 1 d . . . C19A C 0.6216(10) 0.6574(5) 0.1245(9) 0.046(3) Uani 1 1 d . . . C1B C 0.2331(8) 0.7263(4) 0.0982(7) 0.028(2) Uani 1 1 d . . . C2B C 0.3330(8) 0.7472(4) 0.1226(8) 0.032(3) Uani 1 1 d . . . H2B H 0.3863 0.7251 0.1468 0.039 Uiso 1 1 calc R . . C3B C 0.3554(10) 0.7993(5) 0.1119(8) 0.042(3) Uani 1 1 d . . . H3B H 0.4229 0.8120 0.1294 0.050 Uiso 1 1 calc R . . C4B C 0.2785(11) 0.8331(5) 0.0754(9) 0.052(4) Uani 1 1 d . . . H4B H 0.2928 0.8687 0.0698 0.062 Uiso 1 1 calc R . . C5B C 0.1808(11) 0.8133(4) 0.0475(8) 0.045(3) Uani 1 1 d . . . H5B H 0.1301 0.8358 0.0203 0.054 Uiso 1 1 calc R . . C6B C 0.1542(8) 0.7601(4) 0.0584(7) 0.029(2) Uani 1 1 d . . . C7B C 0.0482(9) 0.7439(4) 0.0295(8) 0.035(3) Uani 1 1 d . . . H7B H 0.0007 0.7705 0.0122 0.042 Uiso 1 1 calc R . . C8B C 0.2408(10) 0.5514(4) -0.0032(8) 0.035(3) Uani 1 1 d . . . C9B C 0.3484(9) 0.5387(4) -0.0139(8) 0.038(3) Uani 1 1 d . . . H9B H 0.4005 0.5522 0.0274 0.045 Uiso 1 1 calc R . . C10B C 0.3778(10) 0.5063(5) -0.0855(8) 0.045(3) Uani 1 1 d . . . H10B H 0.4496 0.4992 -0.0937 0.054 Uiso 1 1 calc R . . C11B C 0.2994(11) 0.4842(5) -0.1453(9) 0.051(4) Uani 1 1 d . . . H11B H 0.3188 0.4609 -0.1913 0.061 Uiso 1 1 calc R . . C12B C 0.1944(10) 0.4967(4) -0.1367(8) 0.043(3) Uani 1 1 d . . . H12B H 0.1431 0.4819 -0.1774 0.051 Uiso 1 1 calc R . . C13B C 0.1618(9) 0.5317(4) -0.0671(8) 0.030(3) Uani 1 1 d . . . C14B C 0.0519(9) 0.5467(4) -0.0676(8) 0.035(3) Uani 1 1 d . . . H14B H 0.0040 0.5255 -0.1014 0.042 Uiso 1 1 calc R . . C15B C -0.1038(8) 0.5948(4) -0.0374(9) 0.043(3) Uani 1 1 d . . . H17C H -0.1366 0.5887 0.0215 0.051 Uiso 1 1 calc R . . H17D H -0.1337 0.5699 -0.0823 0.051 Uiso 1 1 calc R . . C16B C -0.1290(10) 0.6499(5) -0.0701(9) 0.044(3) Uani 1 1 d . . . H16A H -0.0886 0.6572 -0.1246 0.053 Uiso 1 1 calc R . . H16B H -0.2043 0.6519 -0.0886 0.053 Uiso 1 1 calc R . . C17B C -0.1043(9) 0.6916(5) 0.0018(9) 0.046(3) Uani 1 1 d . . . H15C H -0.1325 0.7248 -0.0210 0.055 Uiso 1 1 calc R . . H15D H -0.1404 0.6830 0.0581 0.055 Uiso 1 1 calc R . . C18B C 0.0268(9) 0.6174(4) 0.2536(8) 0.030(3) Uani 1 1 d . . . C19B C -0.0528(10) 0.6210(6) 0.3309(10) 0.056(4) Uani 1 1 d . . . C1C C 0.3287(14) 0.4994(6) 0.2140(10) 0.045(5) Uani 0.809(8) 1 d P . . C2C C 0.3475(12) 0.4383(5) 0.2116(11) 0.041(4) Uani 0.809(8) 1 d P . . F1* F 0.036(2) 0.4833(14) 0.328(3) 0.078(14) Uiso 0.191(8) 1 d PD . . F2* F 0.111(3) 0.4202(15) 0.378(2) 0.083(15) Uiso 0.191(8) 1 d PD . . F3* F 0.067(3) 0.4167(17) 0.251(3) 0.098(17) Uiso 0.191(8) 1 d PD . . O1* O 0.289(3) 0.4440(19) 0.310(5) 0.11(2) Uiso 0.191(8) 1 d PD . . C1* C 0.2186(15) 0.4732(13) 0.282(3) 0.057(19) Uiso 0.191(8) 1 d PD . . C2* C 0.1121(19) 0.4519(10) 0.306(2) 0.07(2) Uiso 0.191(8) 1 d PD . . 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 0.0296(3) 0.0297(3) 0.0268(3) -0.0016(2) -0.0023(2) 0.0017(2) Cu1A 0.0274(7) 0.0319(7) 0.0297(9) -0.0024(6) -0.0015(6) 0.0019(6) Cu1B 0.0253(7) 0.0318(7) 0.0303(9) 0.0007(6) -0.0004(6) -0.0001(5) F1A 0.074(6) 0.055(5) 0.113(8) 0.026(5) 0.021(5) -0.011(4) F2A 0.067(6) 0.116(7) 0.038(6) 0.003(5) 0.020(5) -0.010(5) F3A 0.021(4) 0.137(8) 0.078(7) 0.046(6) 0.002(4) -0.005(4) F1B 0.113(9) 0.131(10) 0.159(12) -0.086(9) 0.080(8) -0.049(8) F2B 0.046(6) 0.300(18) 0.067(8) 0.071(9) 0.004(5) -0.010(8) F3B 0.030(4) 0.114(7) 0.056(6) -0.011(5) 0.016(4) -0.026(4) F1C 0.092(8) 0.043(5) 0.096(9) -0.007(5) -0.056(7) 0.013(5) F2C 0.067(6) 0.042(5) 0.047(6) -0.019(4) -0.009(5) 0.009(4) F3C 0.101(9) 0.042(5) 0.078(9) 0.004(5) 0.039(7) -0.006(5) O1A 0.031(4) 0.033(4) 0.028(5) 0.001(3) -0.004(4) 0.001(3) O2A 0.037(4) 0.033(4) 0.027(5) -0.001(3) 0.003(4) 0.001(3) O3A 0.038(5) 0.079(6) 0.022(5) 0.007(4) 0.012(4) 0.021(4) O4A 0.028(4) 0.044(5) 0.050(6) -0.002(4) 0.011(4) 0.005(4) O1B 0.025(4) 0.033(4) 0.031(5) 0.004(3) -0.002(3) 0.000(3) O2B 0.030(4) 0.033(4) 0.036(5) -0.003(3) -0.002(4) 0.008(3) O3B 0.040(5) 0.064(6) 0.030(6) 0.007(4) 0.008(4) -0.008(4) O4B 0.023(4) 0.051(5) 0.061(6) 0.014(4) -0.019(4) -0.009(4) O1C 0.088(8) 0.052(6) 0.049(6) 0.009(4) -0.020(6) -0.024(5) O2C 0.016(4) 0.019(4) 0.031(6) 0.001(4) 0.007(4) -0.003(3) N1A 0.030(5) 0.032(5) 0.043(6) 0.002(4) -0.005(4) 0.002(4) N2A 0.032(5) 0.039(5) 0.037(6) -0.003(4) -0.005(5) -0.007(4) N1B 0.023(5) 0.037(5) 0.030(6) -0.003(4) 0.002(4) 0.001(4) N2B 0.023(5) 0.035(5) 0.043(7) 0.006(4) -0.005(4) 0.000(4) C1A 0.026(6) 0.027(5) 0.040(8) -0.006(5) 0.004(5) 0.003(4) C2A 0.053(8) 0.045(7) 0.032(8) 0.011(5) -0.006(6) -0.001(6) C3A 0.045(8) 0.057(8) 0.053(10) 0.001(7) 0.006(7) -0.022(6) C4A 0.091(12) 0.047(8) 0.032(9) 0.011(6) -0.007(8) -0.006(8) C5A 0.062(9) 0.046(7) 0.034(8) 0.000(6) -0.008(7) -0.007(7) C6A 0.043(7) 0.028(5) 0.026(7) -0.001(5) -0.003(6) 0.008(5) C7A 0.035(7) 0.039(6) 0.044(8) -0.003(6) -0.010(6) 0.008(5) C8A 0.033(6) 0.031(6) 0.022(7) -0.005(4) 0.008(5) -0.001(5) C9A 0.026(6) 0.036(6) 0.031(8) 0.002(5) 0.011(5) 0.005(5) C10A 0.031(7) 0.050(7) 0.043(9) 0.005(6) 0.009(6) 0.010(5) C11A 0.065(9) 0.034(6) 0.044(9) -0.006(5) -0.002(7) 0.011(6) C12A 0.056(8) 0.027(6) 0.034(8) -0.003(5) -0.006(6) -0.002(5) C13A 0.027(6) 0.039(6) 0.031(7) -0.004(5) 0.010(5) 0.004(5) C14A 0.041(7) 0.032(6) 0.023(7) -0.004(5) 0.006(5) -0.008(5) C15A 0.026(6) 0.060(8) 0.038(8) 0.000(6) 0.006(6) -0.003(6) C16A 0.019(6) 0.061(8) 0.061(10) -0.005(7) -0.008(6) -0.007(6) C17A 0.028(6) 0.053(7) 0.055(9) 0.000(6) 0.001(6) 0.009(5) C18A 0.034(7) 0.026(6) 0.045(9) -0.004(5) 0.020(6) 0.006(5) C19A 0.051(8) 0.058(8) 0.031(9) 0.008(6) 0.005(7) 0.000(6) C1B 0.028(6) 0.034(6) 0.023(7) -0.004(4) 0.009(5) 0.001(5) C2B 0.022(6) 0.043(6) 0.034(8) 0.003(5) 0.008(5) -0.002(5) C3B 0.042(7) 0.054(8) 0.030(8) 0.011(6) 0.005(6) -0.015(6) C4B 0.078(10) 0.044(7) 0.034(8) 0.012(6) 0.005(7) -0.028(7) C5B 0.061(8) 0.034(6) 0.038(8) 0.003(5) -0.008(7) -0.002(6) C6B 0.025(6) 0.037(6) 0.024(7) 0.001(5) 0.004(5) 0.002(5) C7B 0.032(6) 0.037(6) 0.036(8) 0.001(5) -0.003(5) 0.018(5) C8B 0.054(8) 0.029(6) 0.023(7) 0.006(5) 0.004(6) 0.001(5) C9B 0.031(6) 0.047(7) 0.035(8) -0.003(5) 0.000(6) 0.016(5) C10B 0.049(8) 0.064(8) 0.023(8) -0.006(6) 0.004(6) 0.027(6) C11B 0.063(9) 0.060(8) 0.029(8) -0.008(6) 0.000(7) 0.025(7) C12B 0.056(8) 0.038(6) 0.032(8) -0.004(5) -0.015(6) -0.005(6) C13B 0.036(6) 0.029(5) 0.026(7) 0.001(4) 0.006(5) 0.002(5) C14B 0.050(7) 0.028(6) 0.027(7) 0.005(5) -0.002(6) -0.007(5) C15B 0.024(6) 0.051(7) 0.052(9) 0.004(6) -0.003(6) -0.004(5) C16B 0.035(7) 0.054(8) 0.042(9) 0.009(6) -0.003(6) -0.002(6) C17B 0.029(6) 0.049(7) 0.059(10) -0.001(6) -0.009(6) 0.005(5) C18B 0.036(6) 0.030(6) 0.023(7) 0.008(4) 0.017(6) -0.010(5) C19B 0.032(7) 0.096(12) 0.041(10) 0.000(8) 0.005(7) -0.015(7) C1C 0.062(11) 0.053(10) 0.019(9) -0.016(7) -0.008(8) 0.041(9) C2C 0.046(9) 0.027(7) 0.049(11) 0.000(7) -0.016(8) -0.007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O4A 2.341(8) . ? Gd1 O4B 2.349(8) . ? Gd1 O2B 2.381(7) . ? Gd1 O1A 2.400(7) . ? Gd1 O2A 2.419(7) . ? Gd1 O1B 2.436(7) . ? Gd1 O2C 2.480(8) . ? Gd1 O1C 2.536(8) . ? Gd1 C1C 2.800(14) . ? Gd1 Cu1A 3.3139(16) . ? Gd1 Cu1B 3.3459(17) . ? Cu1A O1A 1.947(7) . ? Cu1A O2A 1.956(7) . ? Cu1A N2A 1.958(9) . ? Cu1A N1A 1.961(9) . ? Cu1A O3A 2.334(8) . ? Cu1B O2B 1.954(7) . ? Cu1B O1B 1.957(7) . ? Cu1B N1B 1.971(8) . ? Cu1B N2B 1.973(9) . ? Cu1B O3B 2.374(8) . ? F1A C19A 1.335(14) . ? F2A C19A 1.313(14) . ? F3A C19A 1.318(14) . ? F1B C19B 1.348(18) . ? F2B C19B 1.279(16) . ? F3B C19B 1.326(13) . ? F1C C2C 1.312(16) . ? F2C C2C 1.311(17) . ? F3C O1* 1.25(8) . ? F3C C2C 1.337(17) . ? F3C C1* 1.81(4) . ? O1A C1A 1.337(13) . ? O2A C8A 1.340(12) . ? O3A C18A 1.217(13) . ? O4A C18A 1.269(13) . ? O1B C1B 1.337(12) . ? O2B C8B 1.350(13) . ? O3B C18B 1.222(13) . ? O4B C18B 1.237(12) . ? O1C C1* 1.266(10) . ? O1C C1C 1.391(18) . ? O2C C1C 1.20(2) . ? N1A C7A 1.254(14) . ? N1A C17A 1.482(13) . ? N2A C14A 1.279(13) . ? N2A C15A 1.478(13) . ? N1B C7B 1.266(13) . ? N1B C17B 1.484(13) . ? N2B C14B 1.292(14) . ? N2B C15B 1.471(13) . ? C1A C6A 1.400(14) . ? C1A C2A 1.404(15) . ? C2A C3A 1.347(16) . ? C3A C4A 1.391(17) . ? C4A C5A 1.361(18) . ? C5A C6A 1.402(16) . ? C6A C7A 1.451(15) . ? C8A C9A 1.394(14) . ? C8A C13A 1.421(14) . ? C9A C10A 1.358(15) . ? C10A C11A 1.395(16) . ? C11A C12A 1.388(16) . ? C12A C13A 1.392(15) . ? C13A C14A 1.431(14) . ? C15A C16A 1.513(16) . ? C16A C17A 1.509(16) . ? C18A C19A 1.554(17) . ? C1B C2B 1.392(14) . ? C1B C6B 1.414(14) . ? C2B C3B 1.369(15) . ? C3B C4B 1.381(17) . ? C4B C5B 1.368(17) . ? C5B C6B 1.409(15) . ? C6B C7B 1.436(14) . ? C8B C9B 1.402(15) . ? C8B C13B 1.413(15) . ? C9B C10B 1.383(15) . ? C10B C11B 1.397(17) . ? C11B C12B 1.365(17) . ? C12B C13B 1.416(15) . ? C13B C14B 1.428(15) . ? C15B C16B 1.512(15) . ? C16B C17B 1.507(16) . ? C18B C19B 1.529(18) . ? C1C C2C 1.578(19) . ? C1C C1* 1.85(3) . ? C2C O1* 1.63(7) . ? F1* C2* 1.295(10) . ? F2* C2* 1.322(10) . ? F3* C2* 1.305(10) . ? O1* C1* 1.207(10) . ? C1* C2* 1.494(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4A Gd1 O4B 157.9(3) . . ? O4A Gd1 O2B 88.9(3) . . ? O4B Gd1 O2B 94.9(3) . . ? O4A Gd1 O1A 100.5(3) . . ? O4B Gd1 O1A 85.9(3) . . ? O2B Gd1 O1A 153.0(2) . . ? O4A Gd1 O2A 81.3(3) . . ? O4B Gd1 O2A 82.8(3) . . ? O2B Gd1 O2A 143.5(2) . . ? O1A Gd1 O2A 63.5(2) . . ? O4A Gd1 O1B 81.9(3) . . ? O4B Gd1 O1B 80.6(2) . . ? O2B Gd1 O1B 62.9(2) . . ? O1A Gd1 O1B 143.1(2) . . ? O2A Gd1 O1B 80.8(2) . . ? O4A Gd1 O2C 72.3(3) . . ? O4B Gd1 O2C 129.7(3) . . ? O2B Gd1 O2C 85.8(3) . . ? O1A Gd1 O2C 73.4(3) . . ? O2A Gd1 O2C 123.5(3) . . ? O1B Gd1 O2C 139.7(3) . . ? O4A Gd1 O1C 124.7(3) . . ? O4B Gd1 O1C 77.0(3) . . ? O2B Gd1 O1C 73.2(3) . . ? O1A Gd1 O1C 80.7(3) . . ? O2A Gd1 O1C 139.9(3) . . ? O1B Gd1 O1C 128.2(3) . . ? O2C Gd1 O1C 55.0(3) . . ? O4A Gd1 C1C 96.3(4) . . ? O4B Gd1 C1C 105.8(4) . . ? O2B Gd1 C1C 78.2(3) . . ? O1A Gd1 C1C 75.7(3) . . ? O2A Gd1 C1C 137.7(3) . . ? O1B Gd1 C1C 141.1(3) . . ? O2C Gd1 C1C 25.3(4) . . ? O1C Gd1 C1C 29.7(4) . . ? O4A Gd1 Cu1A 74.9(2) . . ? O4B Gd1 Cu1A 100.43(19) . . ? O2B Gd1 Cu1A 163.77(19) . . ? O1A Gd1 Cu1A 35.50(17) . . ? O2A Gd1 Cu1A 35.78(16) . . ? O1B Gd1 Cu1A 114.22(16) . . ? O2C Gd1 Cu1A 88.56(19) . . ? O1C Gd1 Cu1A 115.4(2) . . ? C1C Gd1 Cu1A 102.5(3) . . ? O4A Gd1 Cu1B 101.1(2) . . ? O4B Gd1 Cu1B 71.26(19) . . ? O2B Gd1 Cu1B 35.04(16) . . ? O1A Gd1 Cu1B 157.11(18) . . ? O2A Gd1 Cu1B 112.75(17) . . ? O1B Gd1 Cu1B 35.32(16) . . ? O2C Gd1 Cu1B 120.8(2) . . ? O1C Gd1 Cu1B 93.1(2) . . ? C1C Gd1 Cu1B 109.2(3) . . ? Cu1A Gd1 Cu1B 148.28(4) . . ? O1A Cu1A O2A 81.0(3) . . ? O1A Cu1A N2A 171.8(3) . . ? O2A Cu1A N2A 91.5(3) . . ? O1A Cu1A N1A 91.5(3) . . ? O2A Cu1A N1A 169.6(4) . . ? N2A Cu1A N1A 95.5(4) . . ? O1A Cu1A O3A 96.2(3) . . ? O2A Cu1A O3A 98.2(3) . . ? N2A Cu1A O3A 88.1(4) . . ? N1A Cu1A O3A 89.8(3) . . ? O1A Cu1A Gd1 45.7(2) . . ? O2A Cu1A Gd1 46.3(2) . . ? N2A Cu1A Gd1 129.7(3) . . ? N1A Cu1A Gd1 130.8(3) . . ? O3A Cu1A Gd1 75.5(2) . . ? O2B Cu1B O1B 80.0(3) . . ? O2B Cu1B N1B 169.1(3) . . ? O1B Cu1B N1B 92.3(3) . . ? O2B Cu1B N2B 91.1(3) . . ? O1B Cu1B N2B 170.4(3) . . ? N1B Cu1B N2B 96.0(3) . . ? O2B Cu1B O3B 101.6(3) . . ? O1B Cu1B O3B 98.6(3) . . ? N1B Cu1B O3B 87.1(3) . . ? N2B Cu1B O3B 86.7(3) . . ? O2B Cu1B Gd1 44.4(2) . . ? O1B Cu1B Gd1 46.0(2) . . ? N1B Cu1B Gd1 132.7(3) . . ? N2B Cu1B Gd1 128.1(3) . . ? O3B Cu1B Gd1 80.2(2) . . ? O1* F3C C2C 78(2) . . ? O1* F3C C1* 41.5(16) . . ? C2C F3C C1* 84.0(9) . . ? C1A O1A Cu1A 119.3(6) . . ? C1A O1A Gd1 139.5(6) . . ? Cu1A O1A Gd1 98.8(3) . . ? C8A O2A Cu1A 122.4(6) . . ? C8A O2A Gd1 139.3(6) . . ? Cu1A O2A Gd1 97.9(3) . . ? C18A O3A Cu1A 121.3(7) . . ? C18A O4A Gd1 124.2(8) . . ? C1B O1B Cu1B 123.1(6) . . ? C1B O1B Gd1 137.5(6) . . ? Cu1B O1B Gd1 98.7(3) . . ? C8B O2B Cu1B 120.8(6) . . ? C8B O2B Gd1 137.2(7) . . ? Cu1B O2B Gd1 100.6(3) . . ? C18B O3B Cu1B 119.1(7) . . ? C18B O4B Gd1 134.2(8) . . ? C1* O1C C1C 88.2(14) . . ? C1* O1C Gd1 146(2) . . ? C1C O1C Gd1 85.7(8) . . ? C1C O2C Gd1 92.4(8) . . ? C7A N1A C17A 117.6(9) . . ? C7A N1A Cu1A 122.1(8) . . ? C17A N1A Cu1A 120.2(7) . . ? C14A N2A C15A 116.8(9) . . ? C14A N2A Cu1A 123.1(8) . . ? C15A N2A Cu1A 120.1(7) . . ? C7B N1B C17B 117.2(9) . . ? C7B N1B Cu1B 122.6(7) . . ? C17B N1B Cu1B 120.2(7) . . ? C14B N2B C15B 117.4(10) . . ? C14B N2B Cu1B 122.3(8) . . ? C15B N2B Cu1B 120.3(7) . . ? O1A C1A C6A 123.0(10) . . ? O1A C1A C2A 119.4(10) . . ? C6A C1A C2A 117.6(11) . . ? C3A C2A C1A 120.7(11) . . ? C2A C3A C4A 122.8(13) . . ? C5A C4A C3A 117.3(12) . . ? C4A C5A C6A 121.9(12) . . ? C1A C6A C5A 119.8(11) . . ? C1A C6A C7A 121.4(11) . . ? C5A C6A C7A 118.9(10) . . ? N1A C7A C6A 127.1(10) . . ? O2A C8A C9A 120.1(9) . . ? O2A C8A C13A 121.2(9) . . ? C9A C8A C13A 118.6(10) . . ? C10A C9A C8A 120.5(11) . . ? C9A C10A C11A 122.3(11) . . ? C12A C11A C10A 117.9(11) . . ? C11A C12A C13A 121.3(11) . . ? C12A C13A C8A 119.3(10) . . ? C12A C13A C14A 117.0(10) . . ? C8A C13A C14A 123.6(10) . . ? N2A C14A C13A 127.0(10) . . ? N2A C15A C16A 112.1(10) . . ? C17A C16A C15A 114.3(11) . . ? N1A C17A C16A 111.5(9) . . ? O3A C18A O4A 131.4(12) . . ? O3A C18A C19A 115.8(11) . . ? O4A C18A C19A 112.7(11) . . ? F2A C19A F3A 107.5(12) . . ? F2A C19A F1A 105.6(11) . . ? F3A C19A F1A 106.4(11) . . ? F2A C19A C18A 114.9(11) . . ? F3A C19A C18A 112.5(10) . . ? F1A C19A C18A 109.3(11) . . ? O1B C1B C2B 120.4(9) . . ? O1B C1B C6B 121.1(9) . . ? C2B C1B C6B 118.2(9) . . ? C3B C2B C1B 122.0(10) . . ? C2B C3B C4B 120.5(11) . . ? C5B C4B C3B 118.8(11) . . ? C4B C5B C6B 122.4(11) . . ? C5B C6B C1B 118.0(10) . . ? C5B C6B C7B 117.8(10) . . ? C1B C6B C7B 124.2(9) . . ? N1B C7B C6B 127.7(10) . . ? O2B C8B C9B 119.9(10) . . ? O2B C8B C13B 120.4(11) . . ? C9B C8B C13B 119.8(11) . . ? C10B C9B C8B 120.5(11) . . ? C9B C10B C11B 119.8(12) . . ? C12B C11B C10B 120.3(12) . . ? C11B C12B C13B 121.3(11) . . ? C8B C13B C12B 118.0(10) . . ? C8B C13B C14B 123.8(10) . . ? C12B C13B C14B 118.2(10) . . ? N2B C14B C13B 126.8(10) . . ? N2B C15B C16B 111.2(9) . . ? C17B C16B C15B 114.2(10) . . ? N1B C17B C16B 113.4(10) . . ? O3B C18B O4B 131.1(11) . . ? O3B C18B C19B 116.7(11) . . ? O4B C18B C19B 112.2(11) . . ? F2B C19B F3B 107.5(12) . . ? F2B C19B F1B 104.7(13) . . ? F3B C19B F1B 103.0(12) . . ? F2B C19B C18B 116.5(12) . . ? F3B C19B C18B 114.2(11) . . ? F1B C19B C18B 109.6(12) . . ? O2C C1C O1C 126.8(13) . . ? O2C C1C C2C 119.9(13) . . ? O1C C1C C2C 113.3(15) . . ? O2C C1C C1* 152(2) . . ? O1C C1C C1* 43.1(8) . . ? C2C C1C C1* 76.7(16) . . ? O2C C1C Gd1 62.3(7) . . ? O1C C1C Gd1 64.6(6) . . ? C2C C1C Gd1 177.7(12) . . ? C1* C1C Gd1 101.7(13) . . ? F2C C2C F1C 107.5(14) . . ? F2C C2C F3C 105.7(11) . . ? F1C C2C F3C 108.2(13) . . ? F2C C2C C1C 110.3(12) . . ? F1C C2C C1C 110.3(11) . . ? F3C C2C C1C 114.6(14) . . ? F2C C2C O1* 153(3) . . ? F1C C2C O1* 91.8(17) . . ? F3C C2C O1* 48(2) . . ? C1C C2C O1* 79.6(17) . . ? C1* O1* F3C 95(5) . . ? C1* O1* C2C 97(4) . . ? F3C O1* C2C 53(3) . . ? O1* C1* O1C 129.7(17) . . ? O1* C1* C2* 110(2) . . ? O1C C1* C2* 119.6(11) . . ? O1* C1* F3C 43(4) . . ? O1C C1* F3C 122(3) . . ? C2* C1* F3C 94.0(16) . . ? O1* C1* C1C 81.4(18) . . ? O1C C1* C1C 48.7(8) . . ? C2* C1* C1C 161(2) . . ? F3C C1* C1C 84.2(17) . . ? F1* C2* F3* 106(3) . . ? F1* C2* F2* 99(3) . . ? F3* C2* F2* 92(3) . . ? F1* C2* C1* 120.2(12) . . ? F3* C2* C1* 118.8(12) . . ? F2* C2* C1* 116.4(12) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.893 _refine_diff_density_max 1.777 _refine_diff_density_min -1.370 _refine_diff_density_rms 0.146 #===END