data_1 _audit_creation_date 2012-02-17 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C88 H112 Ga2 N4 O4 Sm' _chemical_formula_sum 'C88 H112 Ga2 N4 O4 Sm' _chemical_formula_weight 1579.61 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' 'Ga' 'Ga' 0.2307 1.6083 '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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _symmetry_space_group_name_H-M 'P 21/n' _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 13.7822(4) _cell_length_b 14.3724(4) _cell_length_c 20.1608(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.656(2) _cell_angle_gamma 90.00 _cell_volume 3993.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41591 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.34 _exptl_crystal_description 'prism' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.397 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.205 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 1.447 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7537 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34618 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7239 _reflns_number_gt 6179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; Diamond 2.1e/3 O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. Microsoft Word ; _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^)+(0.0320P)^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 7239 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0501 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 Sm Sm 0.5000 0.0000 0.5000 0.02143(4) Uani 1 2 d S . . Ga Ga 0.684515(13) 0.139213(13) 0.502962(9) 0.02223(5) Uani 1 1 d . . . O1 O 0.55407(10) -0.04486(9) 0.38407(6) 0.0338(3) Uani 1 1 d . . . O2 O 0.38608(11) 0.12344(11) 0.45791(9) 0.0571(5) Uani 1 1 d . B . N1 N 0.74998(10) 0.20331(10) 0.57512(7) 0.0216(3) Uani 1 1 d . . . N2 N 0.78953(10) 0.18854(10) 0.44874(7) 0.0209(3) Uani 1 1 d . . . C1 C 0.83213(11) 0.24840(11) 0.55339(8) 0.0207(3) Uani 1 1 d . . . C2 C 0.85367(11) 0.23988(11) 0.48695(8) 0.0199(3) Uani 1 1 d . . . C3 C 0.94036(11) 0.29605(12) 0.47329(8) 0.0213(3) Uani 1 1 d . . . C4 C 0.99194(12) 0.32304(12) 0.41820(9) 0.0250(4) Uani 1 1 d . . . H4 H 0.9747 0.3007 0.3753 0.030 Uiso 1 1 calc R . . C5 C 1.07154(13) 0.38512(13) 0.42722(10) 0.0301(4) Uani 1 1 d . . . H5 H 1.1063 0.4046 0.3892 0.036 Uiso 1 1 calc R . . C6 C 1.10029(13) 0.41796(13) 0.48789(10) 0.0314(4) Uani 1 1 d . . . H6 H 1.1547 0.4583 0.4915 0.038 Uiso 1 1 calc R . . C7 C 1.04864(12) 0.39164(13) 0.54558(9) 0.0274(4) Uani 1 1 d . . . C8 C 1.06658(14) 0.42126(14) 0.61209(10) 0.0356(4) Uani 1 1 d . . . H8 H 1.1209 0.4597 0.6220 0.043 Uiso 1 1 calc R . . C9 C 1.00571(15) 0.39439(15) 0.66150(10) 0.0379(5) Uani 1 1 d . . . H9 H 1.0191 0.4148 0.7055 0.046 Uiso 1 1 calc R . . C10 C 0.92305(13) 0.33716(13) 0.64984(9) 0.0305(4) Uani 1 1 d . . . H10 H 0.8811 0.3212 0.6851 0.037 Uiso 1 1 calc R . . C11 C 0.90506(12) 0.30548(12) 0.58684(8) 0.0231(4) Uani 1 1 d . . . C12 C 0.96996(12) 0.33299(12) 0.53565(8) 0.0223(3) Uani 1 1 d . . . C13 C 0.70672(11) 0.23201(11) 0.63545(8) 0.0202(3) Uani 1 1 d . . . C14 C 0.71763(12) 0.17732(12) 0.69265(8) 0.0239(4) Uani 1 1 d . . . C15 C 0.67042(13) 0.20523(13) 0.75012(9) 0.0289(4) Uani 1 1 d . . . H15 H 0.6776 0.1692 0.7894 0.035 Uiso 1 1 calc R . . C16 C 0.61354(14) 0.28401(13) 0.75119(9) 0.0320(4) Uani 1 1 d . . . H16 H 0.5820 0.3019 0.7908 0.038 Uiso 1 1 calc R . . C17 C 0.60260(13) 0.33689(13) 0.69446(9) 0.0300(4) Uani 1 1 d . . . H17 H 0.5627 0.3907 0.6953 0.036 Uiso 1 1 calc R . . C18 C 0.64902(12) 0.31276(12) 0.63599(8) 0.0243(4) Uani 1 1 d . . . C19 C 0.77755(13) 0.08896(14) 0.69252(9) 0.0309(4) Uani 1 1 d . . . H19 H 0.8045 0.0814 0.6470 0.037 Uiso 1 1 calc R . . C20 C 0.86307(16) 0.09612(17) 0.74072(11) 0.0460(5) Uani 1 1 d . . . H20A H 0.9046 0.1483 0.7279 0.069 Uiso 1 1 calc R . . H20B H 0.9006 0.0383 0.7396 0.069 Uiso 1 1 calc R . . H20C H 0.8390 0.1064 0.7857 0.069 Uiso 1 1 calc R . . C21 C 0.71571(18) 0.00389(15) 0.70679(16) 0.0561(7) Uani 1 1 d . . . H21A H 0.6885 0.0091 0.7513 0.084 Uiso 1 1 calc R . . H21B H 0.7559 -0.0522 0.7043 0.084 Uiso 1 1 calc R . . H21C H 0.6628 -0.0001 0.6740 0.084 Uiso 1 1 calc R . . C22 C 0.63346(14) 0.37111(13) 0.57394(10) 0.0318(4) Uani 1 1 d . . . H22 H 0.6758 0.3445 0.5387 0.038 Uiso 1 1 calc R . . C23 C 0.6642(2) 0.47172(16) 0.58401(13) 0.0527(6) Uani 1 1 d . . . H23A H 0.6222 0.5010 0.6169 0.079 Uiso 1 1 calc R . . H23B H 0.6586 0.5053 0.5418 0.079 Uiso 1 1 calc R . . H23C H 0.7317 0.4737 0.5998 0.079 Uiso 1 1 calc R . . C24 C 0.52941(17) 0.36540(19) 0.54850(13) 0.0564(6) Uani 1 1 d . . . H24A H 0.5119 0.3001 0.5411 0.085 Uiso 1 1 calc R . . H24B H 0.5234 0.3998 0.5067 0.085 Uiso 1 1 calc R . . H24C H 0.4859 0.3926 0.5813 0.085 Uiso 1 1 calc R . . C25 C 0.80501(11) 0.17331(12) 0.38000(8) 0.0206(3) Uani 1 1 d . . . C26 C 0.87048(12) 0.10432(12) 0.35914(8) 0.0243(4) Uani 1 1 d . . . C27 C 0.88136(13) 0.08959(14) 0.29116(9) 0.0305(4) Uani 1 1 d . . . H27 H 0.9267 0.0445 0.2764 0.037 Uiso 1 1 calc R . . C28 C 0.82778(14) 0.13895(14) 0.24514(9) 0.0333(4) Uani 1 1 d . . . H28 H 0.8367 0.1283 0.1991 0.040 Uiso 1 1 calc R . . C29 C 0.76105(13) 0.20398(14) 0.26590(9) 0.0305(4) Uani 1 1 d . . . H29 H 0.7230 0.2364 0.2338 0.037 Uiso 1 1 calc R . . C30 C 0.74848(12) 0.22300(12) 0.33314(8) 0.0237(4) Uani 1 1 d . . . C31 C 0.92612(13) 0.04409(14) 0.40847(9) 0.0299(4) Uani 1 1 d . . . H31 H 0.9010 0.0585 0.4537 0.036 Uiso 1 1 calc R . . C32 C 0.90961(16) -0.05974(15) 0.39587(11) 0.0420(5) Uani 1 1 d . . . H32A H 0.9413 -0.0960 0.4311 0.063 Uiso 1 1 calc R . . H32B H 0.9371 -0.0769 0.3530 0.063 Uiso 1 1 calc R . . H32C H 0.8398 -0.0729 0.3954 0.063 Uiso 1 1 calc R . . C33 C 1.03440(14) 0.06539(15) 0.40901(11) 0.0375(5) Uani 1 1 d . . . H33A H 1.0607 0.0543 0.3647 0.056 Uiso 1 1 calc R . . H33B H 1.0674 0.0250 0.4412 0.056 Uiso 1 1 calc R . . H33C H 1.0447 0.1306 0.4214 0.056 Uiso 1 1 calc R . . C34 C 0.67428(12) 0.29434(13) 0.35615(9) 0.0288(4) Uani 1 1 d . . . H34 H 0.6424 0.2677 0.3962 0.035 Uiso 1 1 calc R . . C35 C 0.59379(15) 0.31446(16) 0.30538(11) 0.0431(5) Uani 1 1 d . . . H35A H 0.6211 0.3472 0.2673 0.065 Uiso 1 1 calc R . . H35B H 0.5439 0.3533 0.3258 0.065 Uiso 1 1 calc R . . H35C H 0.5647 0.2557 0.2905 0.065 Uiso 1 1 calc R . . C36 C 0.72249(15) 0.38516(14) 0.37771(11) 0.0384(5) Uani 1 1 d . . . H36A H 0.7713 0.3723 0.4122 0.058 Uiso 1 1 calc R . . H36B H 0.6733 0.4275 0.3952 0.058 Uiso 1 1 calc R . . H36C H 0.7539 0.4141 0.3395 0.058 Uiso 1 1 calc R . . C37 C 0.61167(18) 0.01641(15) 0.34318(11) 0.0448(6) Uani 1 1 d . . . H37A H 0.6676 0.0411 0.3689 0.054 Uiso 1 1 calc R . . H37B H 0.5720 0.0694 0.3272 0.054 Uiso 1 1 calc R . . C38 C 0.64603(14) -0.04078(15) 0.28584(10) 0.0353(4) Uani 1 1 d . . . H38A H 0.7087 -0.0715 0.2963 0.042 Uiso 1 1 calc R . . H38B H 0.6532 -0.0023 0.2455 0.042 Uiso 1 1 calc R . . C39 C 0.56557(14) -0.11107(14) 0.27749(10) 0.0335(4) Uani 1 1 d . . . H39A H 0.5885 -0.1676 0.2543 0.040 Uiso 1 1 calc R . . H39B H 0.5097 -0.0844 0.2527 0.040 Uiso 1 1 calc R . . C40 C 0.53955(15) -0.13203(14) 0.34849(10) 0.0349(4) Uani 1 1 d . . . H40A H 0.4712 -0.1527 0.3515 0.042 Uiso 1 1 calc R . . H40B H 0.5821 -0.1814 0.3670 0.042 Uiso 1 1 calc R . . C41 C 0.39815(19) 0.19876(17) 0.41219(13) 0.0552(6) Uani 1 1 d . B . H41A H 0.4009 0.1754 0.3660 0.066 Uiso 1 1 calc R . . H41B H 0.4584 0.2337 0.4223 0.066 Uiso 1 1 calc R . . C42 C 0.3111(3) 0.2588(2) 0.4216(2) 0.1006(13) Uani 1 1 d . . . H42A H 0.2661 0.2526 0.3832 0.121 Uiso 0.70 1 calc PR A 1 H42B H 0.3306 0.3248 0.4257 0.121 Uiso 0.70 1 calc PR A 1 H42C H 0.3235 0.3064 0.4561 0.121 Uiso 0.30 1 calc PR A 2 H42D H 0.2925 0.2902 0.3797 0.121 Uiso 0.30 1 calc PR A 2 C43A C 0.2621(4) 0.2260(3) 0.4850(3) 0.0681(11) Uani 0.70 1 d P B 1 H43A H 0.2875 0.2592 0.5245 0.082 Uiso 0.70 1 calc PR B 1 H43B H 0.1908 0.2334 0.4823 0.082 Uiso 0.70 1 calc PR B 1 C43B C 0.2450(6) 0.2020(7) 0.4398(6) 0.062(3) Uani 0.30 1 d P B 2 H43C H 0.2158 0.1711 0.4005 0.074 Uiso 0.30 1 calc PR B 2 H43D H 0.1932 0.2360 0.4632 0.074 Uiso 0.30 1 calc PR B 2 C44 C 0.28991(19) 0.1303(2) 0.48530(19) 0.0813(11) Uani 1 1 d . . . H44A H 0.2435 0.0934 0.4583 0.098 Uiso 0.70 1 calc PR B 1 H44B H 0.2899 0.1059 0.5312 0.098 Uiso 0.70 1 calc PR B 1 H44C H 0.2919 0.1521 0.5319 0.098 Uiso 0.30 1 calc PR B 2 H44D H 0.2550 0.0702 0.4828 0.098 Uiso 0.30 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.01780(6) 0.02438(7) 0.02210(7) 0.00150(5) 0.00028(4) -0.00454(5) Ga 0.02132(9) 0.02782(10) 0.01759(10) -0.00370(7) 0.00269(7) -0.00949(8) O1 0.0424(8) 0.0341(7) 0.0251(7) -0.0045(6) 0.0074(6) -0.0154(6) O2 0.0341(8) 0.0519(10) 0.0853(13) 0.0357(9) 0.0075(8) 0.0099(7) N1 0.0214(7) 0.0265(8) 0.0170(7) -0.0038(6) 0.0030(5) -0.0067(6) N2 0.0199(7) 0.0276(7) 0.0152(7) -0.0016(6) 0.0009(5) -0.0053(6) C1 0.0182(7) 0.0238(8) 0.0202(8) -0.0013(6) 0.0010(6) -0.0027(7) C2 0.0172(7) 0.0236(8) 0.0190(8) -0.0014(6) 0.0006(6) -0.0022(6) C3 0.0170(7) 0.0229(8) 0.0240(9) 0.0003(7) 0.0008(6) -0.0002(7) C4 0.0230(8) 0.0280(9) 0.0243(9) 0.0001(7) 0.0042(7) -0.0016(7) C5 0.0242(9) 0.0310(10) 0.0353(11) 0.0035(8) 0.0103(8) -0.0028(8) C6 0.0211(8) 0.0296(10) 0.0437(12) 0.0006(8) 0.0055(8) -0.0082(7) C7 0.0220(8) 0.0263(9) 0.0341(10) -0.0022(8) -0.0012(7) -0.0040(7) C8 0.0296(10) 0.0379(11) 0.0393(11) -0.0067(9) -0.0052(8) -0.0147(8) C9 0.0408(11) 0.0433(12) 0.0296(11) -0.0089(9) -0.0063(8) -0.0140(9) C10 0.0317(9) 0.0368(10) 0.0230(9) -0.0045(8) 0.0007(7) -0.0103(8) C11 0.0216(8) 0.0242(9) 0.0235(9) -0.0019(7) -0.0009(7) -0.0030(7) C12 0.0189(8) 0.0240(9) 0.0241(9) -0.0006(7) 0.0010(6) -0.0016(7) C13 0.0179(7) 0.0244(8) 0.0183(8) -0.0043(7) 0.0026(6) -0.0067(7) C14 0.0216(8) 0.0295(9) 0.0204(8) -0.0023(7) -0.0006(6) -0.0044(7) C15 0.0320(9) 0.0368(10) 0.0179(9) 0.0005(7) 0.0024(7) -0.0085(8) C16 0.0346(10) 0.0358(10) 0.0260(9) -0.0111(8) 0.0114(8) -0.0085(9) C17 0.0318(9) 0.0252(9) 0.0332(10) -0.0079(8) 0.0072(8) -0.0033(8) C18 0.0247(8) 0.0241(9) 0.0240(9) -0.0033(7) 0.0028(7) -0.0068(7) C19 0.0320(9) 0.0373(11) 0.0234(9) 0.0020(8) -0.0015(7) 0.0059(8) C20 0.0393(12) 0.0518(14) 0.0468(13) 0.0026(11) -0.0122(10) 0.0050(10) C21 0.0461(13) 0.0306(11) 0.091(2) -0.0025(12) -0.0132(13) 0.0042(10) C22 0.0364(10) 0.0266(9) 0.0324(10) 0.0029(8) 0.0030(8) 0.0010(8) C23 0.0740(17) 0.0356(12) 0.0484(14) 0.0105(10) 0.0002(12) -0.0168(12) C24 0.0506(14) 0.0563(15) 0.0617(16) 0.0224(13) -0.0163(12) -0.0069(12) C25 0.0191(8) 0.0266(9) 0.0162(8) -0.0009(7) 0.0020(6) -0.0092(7) C26 0.0225(8) 0.0303(9) 0.0202(8) -0.0013(7) 0.0023(7) -0.0062(7) C27 0.0305(9) 0.0372(10) 0.0240(9) -0.0049(8) 0.0070(7) -0.0044(8) C28 0.0392(10) 0.0441(11) 0.0166(9) -0.0027(8) 0.0043(7) -0.0107(9) C29 0.0328(10) 0.0382(11) 0.0203(9) 0.0055(8) -0.0030(7) -0.0108(8) C30 0.0225(8) 0.0277(9) 0.0210(8) 0.0027(7) 0.0000(6) -0.0090(7) C31 0.0313(9) 0.0350(10) 0.0234(9) 0.0001(8) 0.0055(7) 0.0043(8) C32 0.0441(12) 0.0378(12) 0.0443(13) 0.0080(9) 0.0015(10) -0.0028(10) C33 0.0341(10) 0.0385(11) 0.0397(12) 0.0032(9) -0.0069(9) 0.0034(9) C34 0.0252(9) 0.0327(10) 0.0284(10) 0.0072(8) -0.0002(7) -0.0019(8) C35 0.0350(11) 0.0481(13) 0.0461(13) 0.0082(10) -0.0099(9) 0.0037(10) C36 0.0425(11) 0.0316(11) 0.0411(12) -0.0013(9) 0.0001(9) 0.0024(9) C37 0.0646(14) 0.0413(13) 0.0287(11) -0.0046(9) 0.0121(10) -0.0271(11) C38 0.0305(10) 0.0455(11) 0.0298(10) 0.0029(9) 0.0027(8) -0.0036(9) C39 0.0350(10) 0.0328(10) 0.0326(11) -0.0075(8) 0.0011(8) 0.0019(8) C40 0.0379(10) 0.0286(10) 0.0381(11) -0.0033(8) 0.0017(8) -0.0092(8) C41 0.0637(15) 0.0459(14) 0.0558(15) 0.0198(11) -0.0076(12) -0.0082(12) C42 0.120(3) 0.064(2) 0.118(3) 0.044(2) 0.005(2) 0.037(2) C43A 0.070(3) 0.059(3) 0.075(3) 0.009(2) 0.001(2) 0.016(2) C43B 0.039(4) 0.053(6) 0.093(8) -0.001(6) -0.021(5) 0.005(4) C44 0.0358(13) 0.079(2) 0.130(3) 0.045(2) 0.0229(15) 0.0225(14) _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 Sm O2 2.5105(15) . ? Sm O2 2.5105(15) 3_656 ? Sm O1 2.5443(12) 3_656 ? Sm O1 2.5444(12) . ? Sm Ga 3.23579(18) 3_656 ? Sm Ga 3.23580(18) . ? Ga N1 1.9362(14) . ? Ga N2 1.9567(13) . ? O1 C37 1.449(2) . ? O1 C40 1.456(2) . ? O2 C41 1.433(3) . ? O2 C44 1.445(3) . ? N1 C1 1.380(2) . ? N1 C13 1.422(2) . ? N2 C2 1.380(2) . ? N2 C25 1.422(2) . ? C1 C2 1.381(2) . ? C1 C11 1.457(2) . ? C2 C3 1.471(2) . ? C3 C4 1.381(2) . ? C3 C12 1.420(2) . ? C4 C5 1.424(3) . ? C5 C6 1.366(3) . ? C6 C7 1.422(3) . ? C7 C12 1.386(2) . ? C7 C8 1.426(3) . ? C8 C9 1.366(3) . ? C9 C10 1.422(3) . ? C10 C11 1.369(2) . ? C11 C12 1.429(2) . ? C13 C14 1.402(2) . ? C13 C18 1.407(2) . ? C14 C15 1.394(2) . ? C14 C19 1.515(3) . ? C15 C16 1.377(3) . ? C16 C17 1.380(3) . ? C17 C18 1.392(2) . ? C18 C22 1.519(3) . ? C19 C21 1.520(3) . ? C19 C20 1.523(3) . ? C22 C24 1.520(3) . ? C22 C23 1.520(3) . ? C25 C26 1.408(2) . ? C25 C30 1.412(2) . ? C26 C27 1.397(2) . ? C26 C31 1.519(3) . ? C27 C28 1.376(3) . ? C28 C29 1.380(3) . ? C29 C30 1.396(2) . ? C30 C34 1.524(2) . ? C31 C33 1.523(3) . ? C31 C32 1.530(3) . ? C34 C36 1.526(3) . ? C34 C35 1.528(3) . ? C37 C38 1.500(3) . ? C38 C39 1.508(3) . ? C39 C40 1.510(3) . ? C41 C42 1.491(4) . ? C42 C43B 1.280(10) . ? C42 C43A 1.527(6) . ? C43A C44 1.427(5) . ? C43B C44 1.507(10) . ? 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 O2 Sm O2 180.0 . 3_656 ? O2 Sm O1 86.72(5) . 3_656 ? O2 Sm O1 93.28(5) 3_656 3_656 ? O2 Sm O1 93.28(5) . . ? O2 Sm O1 86.72(5) 3_656 . ? O1 Sm O1 180.00(6) 3_656 . ? O2 Sm Ga 86.70(4) . 3_656 ? O2 Sm Ga 93.30(4) 3_656 3_656 ? O1 Sm Ga 86.29(3) 3_656 3_656 ? O1 Sm Ga 93.71(3) . 3_656 ? O2 Sm Ga 93.30(4) . . ? O2 Sm Ga 86.70(4) 3_656 . ? O1 Sm Ga 93.71(3) 3_656 . ? O1 Sm Ga 86.29(3) . . ? Ga Sm Ga 180.0 3_656 . ? N1 Ga N2 84.61(5) . . ? N1 Ga Sm 131.87(4) . . ? N2 Ga Sm 143.12(4) . . ? C37 O1 C40 108.40(14) . . ? C37 O1 Sm 122.45(11) . . ? C40 O1 Sm 129.09(10) . . ? C41 O2 C44 107.93(18) . . ? C41 O2 Sm 132.43(14) . . ? C44 O2 Sm 119.48(14) . . ? C1 N1 C13 119.26(13) . . ? C1 N1 Ga 111.22(10) . . ? C13 N1 Ga 125.76(10) . . ? C2 N2 C25 121.62(13) . . ? C2 N2 Ga 110.80(10) . . ? C25 N2 Ga 127.53(10) . . ? N1 C1 C2 116.90(15) . . ? N1 C1 C11 132.97(15) . . ? C2 C1 C11 110.13(14) . . ? N2 C2 C1 116.46(14) . . ? N2 C2 C3 134.88(15) . . ? C1 C2 C3 108.49(14) . . ? C4 C3 C12 117.48(15) . . ? C4 C3 C2 137.02(16) . . ? C12 C3 C2 105.38(14) . . ? C3 C4 C5 118.44(17) . . ? C6 C5 C4 123.10(16) . . ? C5 C6 C7 119.87(16) . . ? C12 C7 C6 116.21(17) . . ? C12 C7 C8 116.39(16) . . ? C6 C7 C8 127.36(17) . . ? C9 C8 C7 120.01(17) . . ? C8 C9 C10 122.72(18) . . ? C11 C10 C9 118.80(16) . . ? C10 C11 C12 118.02(16) . . ? C10 C11 C1 137.16(16) . . ? C12 C11 C1 104.81(14) . . ? C7 C12 C3 124.86(15) . . ? C7 C12 C11 123.98(16) . . ? C3 C12 C11 111.10(14) . . ? C14 C13 C18 120.75(14) . . ? C14 C13 N1 119.93(15) . . ? C18 C13 N1 119.24(15) . . ? C15 C14 C13 118.39(16) . . ? C15 C14 C19 120.14(16) . . ? C13 C14 C19 121.45(15) . . ? C16 C15 C14 121.37(17) . . ? C15 C16 C17 119.77(16) . . ? C16 C17 C18 121.19(17) . . ? C17 C18 C13 118.52(16) . . ? C17 C18 C22 119.87(16) . . ? C13 C18 C22 121.56(15) . . ? C14 C19 C21 111.55(16) . . ? C14 C19 C20 111.12(17) . . ? C21 C19 C20 111.41(18) . . ? C18 C22 C24 111.83(16) . . ? C18 C22 C23 112.26(17) . . ? C24 C22 C23 110.92(19) . . ? C26 C25 C30 120.47(15) . . ? C26 C25 N2 120.23(15) . . ? C30 C25 N2 119.12(15) . . ? C27 C26 C25 118.44(17) . . ? C27 C26 C31 119.79(16) . . ? C25 C26 C31 121.73(15) . . ? C28 C27 C26 121.38(18) . . ? C27 C28 C29 119.94(17) . . ? C28 C29 C30 121.19(18) . . ? C29 C30 C25 118.51(16) . . ? C29 C30 C34 121.23(16) . . ? C25 C30 C34 120.25(15) . . ? C26 C31 C33 112.16(15) . . ? C26 C31 C32 111.96(16) . . ? C33 C31 C32 109.94(16) . . ? C30 C34 C36 111.77(15) . . ? C30 C34 C35 114.07(16) . . ? C36 C34 C35 109.83(16) . . ? O1 C37 C38 106.57(16) . . ? C37 C38 C39 102.42(15) . . ? C38 C39 C40 102.13(15) . . ? O1 C40 C39 105.22(15) . . ? O2 C41 C42 104.8(2) . . ? C43B C42 C41 104.1(5) . . ? C41 C42 C43A 107.0(3) . . ? C44 C43A C42 100.3(3) . . ? C42 C43B C44 108.8(6) . . ? C43A C44 O2 108.2(3) . . ? O2 C44 C43B 100.7(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.498 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.046 #============================================================================== data_1' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H112 Ga2 N4 O4 Sm, 2(C4 H8 O), C7 H8' _chemical_formula_sum 'C103 H136 Ga2 N4 O6 Sm' _chemical_formula_weight 1815.95 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' 'Ga' 'Ga' 0.2307 1.6083 '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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 _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 12.7406(7) _cell_length_b 15.4964(5) _cell_length_c 24.3631(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.393(4) _cell_angle_gamma 90.00 _cell_volume 4745.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14943 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 29.51 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.302 _exptl_crystal_size_mid 0.247 _exptl_crystal_size_min 0.202 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7332 _exptl_absorpt_correction_T_max 0.8714 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18069 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8536 _reflns_number_gt 6215 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; Diamond 2.1e/3 O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. Microsoft Word ; _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^)+(0.0413P)^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 8536 _refine_ls_number_parameters 541 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.911 _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 Sm Sm 0.5000 0.5000 1.0000 0.03839(7) Uani 1 2 d S . . Ga Ga 0.49023(3) 0.37683(2) 0.886446(14) 0.04184(9) Uani 1 1 d . . . O1 O 0.40343(18) 0.62475(14) 0.94741(9) 0.0519(5) Uani 1 1 d . . . O2 O 0.67796(18) 0.55896(16) 0.98558(12) 0.0663(7) Uani 1 1 d . . . O3 O 0.8142(4) 0.2762(2) 0.6340(2) 0.1281(15) Uani 1 1 d . . . N1 N 0.54585(17) 0.26733(14) 0.86204(10) 0.0366(5) Uani 1 1 d . . . N2 N 0.42942(17) 0.38920(14) 0.80794(10) 0.0362(5) Uani 1 1 d . . . C1 C 0.51533(19) 0.25544(18) 0.80555(12) 0.0341(6) Uani 1 1 d . . . C2 C 0.45513(19) 0.32050(17) 0.77681(12) 0.0334(6) Uani 1 1 d . . . C3 C 0.43433(19) 0.29939(18) 0.71777(12) 0.0347(6) Uani 1 1 d . . . C4 C 0.3835(2) 0.3366(2) 0.66931(13) 0.0435(7) Uani 1 1 d . . . H4 H 0.3484 0.3906 0.6701 0.052 Uiso 1 1 calc R . . C5 C 0.3843(2) 0.2928(2) 0.61788(14) 0.0514(8) Uani 1 1 d . . . H5 H 0.3491 0.3186 0.5845 0.062 Uiso 1 1 calc R . . C6 C 0.4340(3) 0.2146(2) 0.61456(14) 0.0517(8) Uani 1 1 d . . . H6 H 0.4331 0.1877 0.5795 0.062 Uiso 1 1 calc R . . C7 C 0.4869(2) 0.1742(2) 0.66391(13) 0.0429(7) Uani 1 1 d . . . C8 C 0.5437(2) 0.0939(2) 0.66793(15) 0.0489(8) Uani 1 1 d . . . H8 H 0.5462 0.0605 0.6355 0.059 Uiso 1 1 calc R . . C9 C 0.5936(2) 0.0660(2) 0.71828(15) 0.0472(8) Uani 1 1 d . . . H9 H 0.6316 0.0130 0.7200 0.057 Uiso 1 1 calc R . . C10 C 0.5919(2) 0.11204(19) 0.76857(14) 0.0422(7) Uani 1 1 d . . . H10 H 0.6279 0.0904 0.8030 0.051 Uiso 1 1 calc R . . C11 C 0.5368(2) 0.18887(18) 0.76628(12) 0.0355(6) Uani 1 1 d . . . C12 C 0.4856(2) 0.21758(18) 0.71315(12) 0.0358(6) Uani 1 1 d . . . C13 C 0.6033(2) 0.20126(19) 0.89538(12) 0.0384(7) Uani 1 1 d . . . C14 C 0.5491(2) 0.12871(19) 0.91111(13) 0.0429(7) Uani 1 1 d . . . C15 C 0.6065(3) 0.0680(2) 0.94649(15) 0.0571(9) Uani 1 1 d . . . H15 H 0.5710 0.0189 0.9580 0.069 Uiso 1 1 calc R . . C16 C 0.7144(3) 0.0787(3) 0.96497(16) 0.0666(11) Uani 1 1 d . . . H16 H 0.7521 0.0372 0.9893 0.080 Uiso 1 1 calc R . . C17 C 0.7672(3) 0.1485(2) 0.94859(16) 0.0600(10) Uani 1 1 d . . . H17 H 0.8415 0.1540 0.9611 0.072 Uiso 1 1 calc R . . C18 C 0.7140(2) 0.2118(2) 0.91381(13) 0.0435(7) Uani 1 1 d . . . C19 C 0.4301(2) 0.1171(2) 0.89211(15) 0.0505(8) Uani 1 1 d . . . H19 H 0.4110 0.1469 0.8554 0.061 Uiso 1 1 calc R . . C20 C 0.3953(3) 0.0232(2) 0.88412(19) 0.0711(11) Uani 1 1 d . . . H20A H 0.4395 -0.0060 0.8604 0.107 Uiso 1 1 calc R . . H20B H 0.3206 0.0208 0.8664 0.107 Uiso 1 1 calc R . . H20C H 0.4036 -0.0056 0.9204 0.107 Uiso 1 1 calc R . . C21 C 0.3678(3) 0.1611(3) 0.9332(2) 0.0851(14) Uani 1 1 d . . . H21A H 0.3876 0.1352 0.9701 0.128 Uiso 1 1 calc R . . H21B H 0.2914 0.1535 0.9205 0.128 Uiso 1 1 calc R . . H21C H 0.3847 0.2229 0.9351 0.128 Uiso 1 1 calc R . . C22 C 0.7730(2) 0.2897(2) 0.89642(15) 0.0505(8) Uani 1 1 d . . . H22 H 0.7248 0.3405 0.8968 0.061 Uiso 1 1 calc R . . C23 C 0.8761(3) 0.3108(3) 0.9358(2) 0.0786(13) Uani 1 1 d . . . H23A H 0.8616 0.3149 0.9740 0.118 Uiso 1 1 calc R . . H23B H 0.9043 0.3660 0.9250 0.118 Uiso 1 1 calc R . . H23C H 0.9284 0.2651 0.9337 0.118 Uiso 1 1 calc R . . C24 C 0.7959(3) 0.2811(3) 0.83767(19) 0.0846(14) Uani 1 1 d . . . H24A H 0.8437 0.2321 0.8356 0.127 Uiso 1 1 calc R . . H24B H 0.8297 0.3341 0.8272 0.127 Uiso 1 1 calc R . . H24C H 0.7291 0.2716 0.8121 0.127 Uiso 1 1 calc R . . C25 C 0.3702(2) 0.46120(18) 0.78231(12) 0.0366(6) Uani 1 1 d . . . C26 C 0.2602(2) 0.46495(19) 0.78187(13) 0.0407(7) Uani 1 1 d . . . C27 C 0.2066(2) 0.5411(2) 0.76363(14) 0.0482(8) Uani 1 1 d . . . H27 H 0.1323 0.5455 0.7641 0.058 Uiso 1 1 calc R . . C28 C 0.2593(3) 0.6097(2) 0.74500(15) 0.0540(9) Uani 1 1 d . . . H28 H 0.2219 0.6614 0.7336 0.065 Uiso 1 1 calc R . . C29 C 0.3664(3) 0.6037(2) 0.74277(15) 0.0513(8) Uani 1 1 d . . . H29 H 0.4014 0.6507 0.7284 0.062 Uiso 1 1 calc R . . C30 C 0.4246(2) 0.52978(19) 0.76132(14) 0.0430(7) Uani 1 1 d . . . C31 C 0.2002(2) 0.3887(2) 0.80104(16) 0.0529(9) Uani 1 1 d . . . H31 H 0.2477 0.3371 0.8029 0.063 Uiso 1 1 calc R . . C32 C 0.1743(3) 0.4045(3) 0.85945(19) 0.0765(12) Uani 1 1 d . . . H32A H 0.2405 0.4125 0.8857 0.115 Uiso 1 1 calc R . . H32B H 0.1357 0.3546 0.8709 0.115 Uiso 1 1 calc R . . H32C H 0.1301 0.4563 0.8591 0.115 Uiso 1 1 calc R . . C33 C 0.0986(3) 0.3681(3) 0.7607(2) 0.0713(11) Uani 1 1 d . . . H33A H 0.0481 0.4159 0.7603 0.107 Uiso 1 1 calc R . . H33B H 0.0667 0.3152 0.7726 0.107 Uiso 1 1 calc R . . H33C H 0.1156 0.3600 0.7232 0.107 Uiso 1 1 calc R . . C34 C 0.5448(3) 0.5250(2) 0.76192(17) 0.0593(9) Uani 1 1 d . . . H34 H 0.5649 0.4626 0.7627 0.071 Uiso 1 1 calc R . . C35 C 0.5780(4) 0.5645(4) 0.7105(2) 0.1020(17) Uani 1 1 d . . . H35A H 0.5343 0.5403 0.6772 0.153 Uiso 1 1 calc R . . H35B H 0.6531 0.5514 0.7099 0.153 Uiso 1 1 calc R . . H35C H 0.5681 0.6271 0.7111 0.153 Uiso 1 1 calc R . . C36 C 0.6051(3) 0.5664(4) 0.8144(2) 0.0946(16) Uani 1 1 d . . . H36A H 0.5915 0.6287 0.8135 0.142 Uiso 1 1 calc R . . H36B H 0.6815 0.5560 0.8164 0.142 Uiso 1 1 calc R . . H36C H 0.5811 0.5412 0.8471 0.142 Uiso 1 1 calc R . . C37 C 0.3618(3) 0.6295(2) 0.88910(16) 0.0653(10) Uani 1 1 d . . . H37A H 0.2840 0.6198 0.8825 0.078 Uiso 1 1 calc R . . H37B H 0.3956 0.5855 0.8682 0.078 Uiso 1 1 calc R . . C38 C 0.3875(3) 0.7195(2) 0.87099(17) 0.0668(10) Uani 1 1 d . . . H38A H 0.4518 0.7190 0.8531 0.080 Uiso 1 1 calc R . . H38B H 0.3274 0.7436 0.8445 0.080 Uiso 1 1 calc R . . C39 C 0.4063(3) 0.7712(2) 0.92421(19) 0.0690(11) Uani 1 1 d . . . H39A H 0.4807 0.7920 0.9323 0.083 Uiso 1 1 calc R . . H39B H 0.3578 0.8215 0.9217 0.083 Uiso 1 1 calc R . . C40 C 0.3836(4) 0.7093(2) 0.96803(17) 0.0706(11) Uani 1 1 d . . . H40A H 0.4309 0.7207 1.0038 0.085 Uiso 1 1 calc R . . H40B H 0.3088 0.7146 0.9739 0.085 Uiso 1 1 calc R . . C41 C 0.7067(4) 0.6452(3) 0.9750(2) 0.0886(14) Uani 1 1 d D . . H41A H 0.6933 0.6836 1.0056 0.106 Uiso 1 1 calc R . . H41B H 0.6647 0.6663 0.9398 0.106 Uiso 1 1 calc R . . C42 C 0.8205(4) 0.6445(4) 0.9711(3) 0.129(2) Uani 1 1 d D . . H42A H 0.8314 0.6632 0.9336 0.155 Uiso 1 1 calc R . . H42B H 0.8598 0.6843 0.9989 0.155 Uiso 1 1 calc R . . C43 C 0.8573(4) 0.5598(4) 0.9813(3) 0.141(3) Uani 1 1 d D . . H43A H 0.9055 0.5567 1.0175 0.169 Uiso 1 1 calc R . . H43B H 0.8972 0.5410 0.9518 0.169 Uiso 1 1 calc R . . C44 C 0.7681(3) 0.5056(3) 0.9821(3) 0.114(2) Uani 1 1 d D . . H44A H 0.7813 0.4662 1.0145 0.136 Uiso 1 1 calc R . . H44B H 0.7549 0.4703 0.9478 0.136 Uiso 1 1 calc R . . C45 C 0.8294(5) 0.3606(3) 0.6190(3) 0.110(2) Uani 1 1 d . A 1 H45A H 0.8041 0.3686 0.5787 0.132 Uiso 1 1 calc R A 1 H45B H 0.9060 0.3754 0.6270 0.132 Uiso 1 1 calc R A 1 C46 C 0.7698(5) 0.4157(3) 0.6510(3) 0.1072(18) Uani 1 1 d . . . H46A H 0.7225 0.4550 0.6263 0.129 Uiso 1 1 calc R A 1 H46B H 0.8184 0.4505 0.6782 0.129 Uiso 1 1 calc R A 1 C47 C 0.7063(5) 0.3546(3) 0.6801(3) 0.114(2) Uani 1 1 d . A . H47A H 0.7031 0.3744 0.7185 0.137 Uiso 1 1 calc R . . H47B H 0.6329 0.3486 0.6596 0.137 Uiso 1 1 calc R . . C48 C 0.7628(5) 0.2756(3) 0.6806(3) 0.1068(18) Uani 1 1 d . A . H48A H 0.8156 0.2705 0.7151 0.128 Uiso 1 1 calc R . . H48B H 0.7132 0.2261 0.6787 0.128 Uiso 1 1 calc R . . C49 C 0.4274(14) 0.5952(11) 0.5159(9) 0.147(5) Uani 0.50 1 d PD B -1 H49A H 0.3550 0.5958 0.4947 0.220 Uiso 0.50 1 calc PR B -1 H49B H 0.4644 0.6482 0.5083 0.220 Uiso 0.50 1 calc PR B -1 H49C H 0.4242 0.5916 0.5557 0.220 Uiso 0.50 1 calc PR B -1 C55 C 0.5036(7) 0.4574(7) 0.5381(4) 0.100(4) Uani 0.50 1 d PGD B -1 H55 H 0.4815 0.4611 0.5734 0.120 Uiso 0.50 1 calc PR B -1 C50 C 0.4818(7) 0.5246(6) 0.5002(5) 0.111(5) Uani 0.50 1 d PG B -1 C51 C 0.5142(7) 0.5191(8) 0.4485(4) 0.116(4) Uani 0.50 1 d PGD B -1 H51 H 0.4993 0.5651 0.4226 0.139 Uiso 0.50 1 calc PR B -1 C52 C 0.5684(7) 0.4465(10) 0.4348(4) 0.111(4) Uani 0.50 1 d PG B -1 H52 H 0.5906 0.4428 0.3995 0.133 Uiso 0.50 1 calc PR B -1 C53 C 0.5903(8) 0.3793(7) 0.4727(6) 0.147(5) Uani 0.50 1 d PG B -1 H53 H 0.6273 0.3296 0.4633 0.176 Uiso 0.50 1 calc PR B -1 C54 C 0.5578(8) 0.3847(6) 0.5244(5) 0.116(4) Uani 0.50 1 d PG B -1 H54 H 0.5727 0.3388 0.5503 0.139 Uiso 0.50 1 calc PR B -1 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 Sm 0.04471(11) 0.03536(11) 0.03428(12) -0.00233(11) 0.00405(8) 0.00469(10) Ga 0.05203(18) 0.03950(18) 0.03161(19) -0.00485(15) -0.00028(14) 0.01380(14) O1 0.0711(13) 0.0429(12) 0.0394(13) -0.0003(10) 0.0017(10) 0.0150(11) O2 0.0596(14) 0.0528(14) 0.090(2) -0.0110(14) 0.0235(13) -0.0057(12) O3 0.195(4) 0.067(2) 0.147(4) -0.007(2) 0.104(3) 0.004(2) N1 0.0406(11) 0.0345(12) 0.0327(14) -0.0022(11) -0.0001(10) 0.0093(10) N2 0.0419(12) 0.0334(12) 0.0317(13) -0.0010(10) 0.0011(10) 0.0088(10) C1 0.0343(13) 0.0352(14) 0.0328(16) -0.0022(12) 0.0055(11) 0.0008(11) C2 0.0325(12) 0.0337(14) 0.0327(16) -0.0006(12) 0.0018(11) 0.0013(11) C3 0.0322(13) 0.0365(15) 0.0350(16) 0.0008(13) 0.0046(11) -0.0049(11) C4 0.0457(15) 0.0456(17) 0.0381(18) 0.0017(14) 0.0038(13) -0.0039(13) C5 0.0537(18) 0.063(2) 0.0345(18) 0.0045(16) -0.0007(14) -0.0085(16) C6 0.0607(18) 0.061(2) 0.0333(18) -0.0094(16) 0.0071(14) -0.0120(17) C7 0.0451(15) 0.0488(18) 0.0365(18) -0.0083(14) 0.0117(13) -0.0120(13) C8 0.0550(17) 0.0484(18) 0.047(2) -0.0174(16) 0.0187(15) -0.0089(15) C9 0.0495(16) 0.0377(16) 0.057(2) -0.0111(16) 0.0163(15) -0.0006(14) C10 0.0435(15) 0.0381(16) 0.0457(19) -0.0059(14) 0.0089(13) 0.0014(13) C11 0.0345(13) 0.0358(15) 0.0366(17) -0.0037(13) 0.0071(11) -0.0017(11) C12 0.0359(13) 0.0376(15) 0.0347(17) -0.0027(13) 0.0080(11) -0.0065(11) C13 0.0450(15) 0.0386(15) 0.0300(16) -0.0055(13) 0.0016(12) 0.0139(12) C14 0.0549(16) 0.0414(16) 0.0323(17) -0.0028(14) 0.0070(13) 0.0094(14) C15 0.079(2) 0.0436(18) 0.048(2) 0.0081(16) 0.0069(17) 0.0149(17) C16 0.080(2) 0.065(2) 0.050(2) 0.0084(19) -0.0035(19) 0.031(2) C17 0.0538(18) 0.066(2) 0.055(2) -0.0025(19) -0.0067(16) 0.0237(18) C18 0.0426(15) 0.0475(17) 0.0386(18) -0.0096(14) 0.0015(13) 0.0149(13) C19 0.0566(18) 0.0451(18) 0.048(2) 0.0031(15) 0.0036(15) -0.0010(15) C20 0.088(3) 0.051(2) 0.070(3) 0.0014(18) -0.001(2) -0.0144(18) C21 0.064(2) 0.086(3) 0.110(4) -0.023(3) 0.029(2) -0.005(2) C22 0.0418(15) 0.0523(19) 0.055(2) -0.0106(16) 0.0009(14) 0.0061(14) C23 0.053(2) 0.080(3) 0.094(3) -0.018(2) -0.015(2) 0.0037(19) C24 0.090(3) 0.099(3) 0.069(3) -0.015(3) 0.025(2) -0.039(3) C25 0.0436(15) 0.0341(14) 0.0304(16) -0.0025(12) 0.0010(12) 0.0058(12) C26 0.0409(15) 0.0382(15) 0.0401(18) -0.0018(13) -0.0019(13) 0.0037(12) C27 0.0414(15) 0.0445(17) 0.054(2) 0.0008(16) -0.0060(14) 0.0090(14) C28 0.0634(19) 0.0380(18) 0.054(2) 0.0034(16) -0.0091(16) 0.0131(15) C29 0.070(2) 0.0365(17) 0.046(2) 0.0066(15) 0.0045(16) -0.0018(15) C30 0.0498(16) 0.0383(15) 0.0411(18) -0.0037(13) 0.0082(14) 0.0014(13) C31 0.0434(16) 0.0436(18) 0.072(3) 0.0085(17) 0.0109(15) 0.0044(14) C32 0.072(2) 0.084(3) 0.075(3) 0.020(2) 0.017(2) -0.006(2) C33 0.059(2) 0.057(2) 0.095(3) -0.010(2) 0.006(2) -0.0083(18) C34 0.0570(19) 0.0475(19) 0.079(3) -0.0016(18) 0.0277(18) -0.0040(15) C35 0.101(3) 0.104(4) 0.117(5) 0.020(3) 0.065(3) -0.003(3) C36 0.050(2) 0.120(4) 0.113(4) -0.031(3) 0.011(2) -0.016(2) C37 0.094(3) 0.052(2) 0.047(2) -0.0025(17) 0.0030(19) 0.0098(19) C38 0.088(3) 0.062(2) 0.053(2) 0.0130(19) 0.0219(19) 0.017(2) C39 0.076(2) 0.048(2) 0.082(3) 0.000(2) 0.008(2) -0.0014(18) C40 0.107(3) 0.056(2) 0.046(2) -0.0032(18) 0.004(2) 0.021(2) C41 0.096(3) 0.062(3) 0.116(4) 0.005(3) 0.043(3) -0.007(2) C42 0.083(3) 0.107(4) 0.202(8) 0.034(5) 0.038(4) -0.026(3) C43 0.077(3) 0.145(6) 0.215(8) 0.062(6) 0.071(4) 0.017(4) C44 0.068(2) 0.084(3) 0.194(7) -0.034(4) 0.035(3) 0.008(3) C45 0.115(4) 0.079(3) 0.155(6) 0.022(3) 0.079(4) 0.008(3) C46 0.148(5) 0.060(3) 0.125(5) -0.011(3) 0.057(4) -0.009(3) C47 0.126(4) 0.090(4) 0.146(6) 0.029(4) 0.079(4) 0.023(3) C48 0.142(4) 0.075(3) 0.122(5) 0.000(3) 0.078(4) -0.003(3) C49 0.072(5) 0.095(9) 0.261(14) -0.016(8) -0.011(7) -0.019(5) C55 0.085(7) 0.112(10) 0.097(11) 0.029(8) -0.006(7) -0.050(7) C50 0.034(7) 0.077(9) 0.211(16) -0.013(11) -0.011(8) -0.018(5) C51 0.087(6) 0.133(9) 0.117(9) 0.041(7) -0.018(5) -0.047(6) C52 0.074(6) 0.172(13) 0.083(8) -0.009(9) -0.001(5) -0.049(8) C53 0.072(5) 0.095(9) 0.261(14) -0.016(8) -0.011(7) -0.019(5) C54 0.087(6) 0.133(9) 0.117(9) 0.041(7) -0.018(5) -0.047(6) _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 Sm O2 2.522(2) 3_667 ? Sm O2 2.522(2) . ? Sm O1 2.525(2) . ? Sm O1 2.526(2) 3_667 ? Sm Ga 3.3467(3) . ? Sm Ga 3.3467(3) 3_667 ? Ga N2 1.952(2) . ? Ga N1 1.968(2) . ? O1 C37 1.435(4) . ? O1 C40 1.441(4) . ? O2 C41 1.421(5) . ? O2 C44 1.429(5) . ? O3 C45 1.379(6) . ? O3 C48 1.400(6) . ? N1 C1 1.380(4) . ? N1 C13 1.432(3) . ? N2 C2 1.377(4) . ? N2 C25 1.432(3) . ? C1 C2 1.386(4) . ? C1 C11 1.463(4) . ? C2 C3 1.457(4) . ? C3 C4 1.377(4) . ? C3 C12 1.439(4) . ? C4 C5 1.427(5) . ? C5 C6 1.375(5) . ? C6 C7 1.424(5) . ? C7 C12 1.378(4) . ? C7 C8 1.434(4) . ? C8 C9 1.357(5) . ? C9 C10 1.421(4) . ? C10 C11 1.379(4) . ? C11 C12 1.423(4) . ? C13 C14 1.405(4) . ? C13 C18 1.419(4) . ? C14 C15 1.398(4) . ? C14 C19 1.522(4) . ? C15 C16 1.385(5) . ? C16 C17 1.366(5) . ? C17 C18 1.398(5) . ? C18 C22 1.518(5) . ? C19 C20 1.526(5) . ? C19 C21 1.534(5) . ? C22 C24 1.513(5) . ? C22 C23 1.531(4) . ? C25 C26 1.402(4) . ? C25 C30 1.409(4) . ? C26 C27 1.399(4) . ? C26 C31 1.521(4) . ? C27 C28 1.374(5) . ? C28 C29 1.378(5) . ? C29 C30 1.399(4) . ? C30 C34 1.530(4) . ? C31 C33 1.526(5) . ? C31 C32 1.532(6) . ? C34 C35 1.516(6) . ? C34 C36 1.522(6) . ? C37 C38 1.514(5) . ? C38 C39 1.510(6) . ? C39 C40 1.498(6) . ? C41 C42 1.468(6) . ? C42 C43 1.402(7) . ? C43 C44 1.415(6) . ? C45 C46 1.452(7) . ? C46 C47 1.497(7) . ? C47 C48 1.419(7) . ? C49 C50 1.382(17) . ? C55 C50 1.3900 . ? C55 C54 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? 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 O2 Sm O2 180.0 3_667 . ? O2 Sm O1 88.47(8) 3_667 . ? O2 Sm O1 91.53(8) . . ? O2 Sm O1 91.52(8) 3_667 3_667 ? O2 Sm O1 88.47(8) . 3_667 ? O1 Sm O1 180.000(1) . 3_667 ? O2 Sm Ga 89.75(6) 3_667 . ? O2 Sm Ga 90.25(6) . . ? O1 Sm Ga 93.89(5) . . ? O1 Sm Ga 86.11(5) 3_667 . ? O2 Sm Ga 90.25(6) 3_667 3_667 ? O2 Sm Ga 89.75(6) . 3_667 ? O1 Sm Ga 86.11(5) . 3_667 ? O1 Sm Ga 93.89(5) 3_667 3_667 ? Ga Sm Ga 180.0 . 3_667 ? N2 Ga N1 83.89(9) . . ? N2 Ga Sm 135.16(7) . . ? N1 Ga Sm 140.80(7) . . ? C37 O1 C40 103.9(3) . . ? C37 O1 Sm 127.76(19) . . ? C40 O1 Sm 128.2(2) . . ? C41 O2 C44 107.5(3) . . ? C41 O2 Sm 129.1(2) . . ? C44 O2 Sm 123.2(2) . . ? C45 O3 C48 109.0(4) . . ? C1 N1 C13 120.3(2) . . ? C1 N1 Ga 111.08(17) . . ? C13 N1 Ga 128.41(19) . . ? C2 N2 C25 121.2(2) . . ? C2 N2 Ga 111.81(17) . . ? C25 N2 Ga 126.90(18) . . ? N1 C1 C2 116.7(2) . . ? N1 C1 C11 134.0(2) . . ? C2 C1 C11 109.3(2) . . ? N2 C2 C1 116.5(2) . . ? N2 C2 C3 134.1(2) . . ? C1 C2 C3 109.4(2) . . ? C4 C3 C12 117.2(3) . . ? C4 C3 C2 137.5(3) . . ? C12 C3 C2 105.3(2) . . ? C3 C4 C5 118.9(3) . . ? C6 C5 C4 122.7(3) . . ? C5 C6 C7 119.8(3) . . ? C12 C7 C6 116.7(3) . . ? C12 C7 C8 116.2(3) . . ? C6 C7 C8 127.1(3) . . ? C9 C8 C7 119.7(3) . . ? C8 C9 C10 123.2(3) . . ? C11 C10 C9 118.6(3) . . ? C10 C11 C12 117.5(3) . . ? C10 C11 C1 137.0(3) . . ? C12 C11 C1 105.5(2) . . ? C7 C12 C11 124.8(3) . . ? C7 C12 C3 124.6(3) . . ? C11 C12 C3 110.5(2) . . ? C14 C13 C18 120.9(3) . . ? C14 C13 N1 119.9(2) . . ? C18 C13 N1 119.1(3) . . ? C15 C14 C13 118.4(3) . . ? C15 C14 C19 120.2(3) . . ? C13 C14 C19 121.4(3) . . ? C16 C15 C14 120.7(3) . . ? C17 C16 C15 120.6(3) . . ? C16 C17 C18 121.3(3) . . ? C17 C18 C13 118.0(3) . . ? C17 C18 C22 121.0(3) . . ? C13 C18 C22 121.0(3) . . ? C14 C19 C20 113.9(3) . . ? C14 C19 C21 110.2(3) . . ? C20 C19 C21 109.7(3) . . ? C24 C22 C18 112.0(3) . . ? C24 C22 C23 109.5(3) . . ? C18 C22 C23 114.1(3) . . ? C26 C25 C30 121.1(3) . . ? C26 C25 N2 119.4(3) . . ? C30 C25 N2 119.4(2) . . ? C27 C26 C25 118.3(3) . . ? C27 C26 C31 120.6(3) . . ? C25 C26 C31 121.2(3) . . ? C28 C27 C26 121.2(3) . . ? C27 C28 C29 120.2(3) . . ? C28 C29 C30 121.2(3) . . ? C29 C30 C25 118.0(3) . . ? C29 C30 C34 121.3(3) . . ? C25 C30 C34 120.7(3) . . ? C26 C31 C33 112.4(3) . . ? C26 C31 C32 110.9(3) . . ? C33 C31 C32 110.1(3) . . ? C35 C34 C36 110.7(4) . . ? C35 C34 C30 112.7(4) . . ? C36 C34 C30 110.8(3) . . ? O1 C37 C38 105.9(3) . . ? C39 C38 C37 104.5(3) . . ? C40 C39 C38 104.5(3) . . ? O1 C40 C39 105.6(3) . . ? O2 C41 C42 106.9(4) . . ? C43 C42 C41 107.5(4) . . ? C42 C43 C44 108.2(4) . . ? C43 C44 O2 108.2(4) . . ? O3 C45 C46 107.8(4) . . ? C45 C46 C47 104.7(4) . . ? C48 C47 C46 103.7(4) . . ? O3 C48 C47 106.9(5) . . ? C50 C55 C54 120.0 . . ? C49 C50 C55 117.7(7) . . ? C49 C50 C51 122.3(7) . . ? C55 C50 C51 120.0 . . ? C50 C51 C52 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C55 120.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.580 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.055 #============================================================================== data_2 _audit_creation_date 2012-02-17 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name 'Peter Roesky' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.5(C176 H224 Eu2 Ga4 N8 O8), 2(C4 H8 O), 0.5(C14 H16)' _chemical_formula_sum 'C103 H136 Eu Ga2 N4 O6' _chemical_formula_weight 1817.56 _chemical_melting_point ? 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' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.611(3) _cell_length_b 15.433(3) _cell_length_c 24.211(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.49(3) _cell_angle_gamma 90.00 _cell_volume 4647.3(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 28483 _cell_measurement_temperature 150 _cell_measurement_theta_max 27.24 _cell_measurement_theta_min 1.32 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_T_max 0.8841 _exptl_absorpt_correction_T_min 0.6967 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'prism' _exptl_crystal_F_000 1910 _exptl_crystal_size_max 0.363 _exptl_crystal_size_mid 0.232 _exptl_crystal_size_min 0.106 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 35152 _diffrn_reflns_theta_full 26.74 _diffrn_reflns_theta_max 26.74 _diffrn_reflns_theta_min 1.57 _diffrn_ambient_temperature 150 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7744 _reflns_number_total 9858 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. 2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.822 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 518 _refine_ls_number_reflns 9858 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0359 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.0786 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Eu Eu 0.5000 0.5000 1.0000 0.02416(6) Uani 1 2 d S . . Ga Ga 0.48822(2) 0.37669(2) 0.886587(11) 0.02662(8) Uani 1 1 d . . . O1 O 0.40196(17) 0.62442(13) 0.94718(8) 0.0337(5) Uani 1 1 d . . . C2 C 0.45393(19) 0.32083(16) 0.77637(10) 0.0211(5) Uani 1 1 d . . . C1 C 0.51527(19) 0.25591(17) 0.80507(10) 0.0207(5) Uani 1 1 d . . . C14 C 0.5505(2) 0.12813(18) 0.91145(11) 0.0280(6) Uani 1 1 d . . . C25 C 0.3667(2) 0.46088(17) 0.78185(10) 0.0223(5) Uani 1 1 d . . . C10 C 0.5944(2) 0.11291(17) 0.76818(11) 0.0255(5) Uani 1 1 d . . . H10 H 0.6309 0.0914 0.8030 0.031 Uiso 1 1 calc R . . C4 C 0.3823(2) 0.33754(19) 0.66794(11) 0.0280(6) Uani 1 1 d . . . H4 H 0.3460 0.3914 0.6688 0.034 Uiso 1 1 calc R . . C12 C 0.4861(2) 0.21854(17) 0.71221(10) 0.0218(5) Uani 1 1 d . . . C13 C 0.6048(2) 0.20172(17) 0.89538(10) 0.0235(5) Uani 1 1 d . . . C11 C 0.5379(2) 0.18937(17) 0.76571(10) 0.0218(5) Uani 1 1 d . . . C29 C 0.3633(3) 0.60415(19) 0.74260(12) 0.0330(6) Uani 1 1 d . . . H29 H 0.3988 0.6512 0.7281 0.040 Uiso 1 1 calc R . . C31 C 0.1957(2) 0.38851(19) 0.80122(13) 0.0339(6) Uani 1 1 d . . . H31 H 0.2436 0.3366 0.8028 0.041 Uiso 1 1 calc R . . C26 C 0.2562(2) 0.46497(18) 0.78167(11) 0.0257(5) Uani 1 1 d . . . C7 C 0.4886(2) 0.17510(18) 0.66237(11) 0.0275(6) Uani 1 1 d . . . C8 C 0.5465(2) 0.09514(19) 0.66656(12) 0.0315(6) Uani 1 1 d . . . H8 H 0.5497 0.0618 0.6339 0.038 Uiso 1 1 calc R . . C27 C 0.2014(2) 0.54110(19) 0.76372(12) 0.0305(6) Uani 1 1 d . . . H27 H 0.1264 0.5452 0.7644 0.037 Uiso 1 1 calc R . . C6 C 0.4348(2) 0.2160(2) 0.61275(11) 0.0336(6) Uani 1 1 d . . . H6 H 0.4337 0.1890 0.5774 0.040 Uiso 1 1 calc R . . C5 C 0.3847(2) 0.2939(2) 0.61604(11) 0.0329(6) Uani 1 1 d . . . H5 H 0.3499 0.3203 0.5824 0.039 Uiso 1 1 calc R . . C3 C 0.4338(2) 0.29972(17) 0.71659(10) 0.0220(5) Uani 1 1 d . . . C19 C 0.4310(2) 0.11656(19) 0.89250(12) 0.0331(6) Uani 1 1 d . . . H19 H 0.4119 0.1464 0.8555 0.040 Uiso 1 1 calc R . . C18 C 0.7160(2) 0.21312(19) 0.91404(11) 0.0283(6) Uani 1 1 d . . . C30 C 0.4215(2) 0.53001(18) 0.76116(11) 0.0273(6) Uani 1 1 d . . . C34 C 0.5423(3) 0.5250(2) 0.76194(14) 0.0394(7) Uani 1 1 d . . . H34 H 0.5623 0.4623 0.7618 0.047 Uiso 1 1 calc R . . C28 C 0.2546(3) 0.61031(19) 0.74497(12) 0.0342(7) Uani 1 1 d . . . H28 H 0.2167 0.6623 0.7337 0.041 Uiso 1 1 calc R . . O3 O 0.8173(3) 0.27511(18) 0.63485(13) 0.0720(9) Uani 1 1 d . . . C22 C 0.7745(2) 0.2919(2) 0.89697(12) 0.0320(6) Uani 1 1 d . . . H22 H 0.7259 0.3428 0.8983 0.038 Uiso 1 1 calc R . . C17 C 0.7710(2) 0.1498(2) 0.94905(12) 0.0364(7) Uani 1 1 d . . . H17 H 0.8460 0.1562 0.9618 0.044 Uiso 1 1 calc R . . C20 C 0.3960(3) 0.0221(2) 0.88402(15) 0.0465(8) Uani 1 1 d . . . H20A H 0.4404 -0.0067 0.8599 0.070 Uiso 1 1 calc R . . H20B H 0.3204 0.0197 0.8664 0.070 Uiso 1 1 calc R . . H20C H 0.4049 -0.0073 0.9204 0.070 Uiso 1 1 calc R . . C9 C 0.5972(2) 0.06663(19) 0.71777(12) 0.0302(6) Uani 1 1 d . . . H9 H 0.6360 0.0136 0.7196 0.036 Uiso 1 1 calc R . . C16 C 0.7181(3) 0.0782(2) 0.96544(13) 0.0417(8) Uani 1 1 d . . . H16 H 0.7565 0.0361 0.9895 0.050 Uiso 1 1 calc R . . C23 C 0.8796(3) 0.3123(3) 0.93553(15) 0.0484(8) Uani 1 1 d . . . H23A H 0.8667 0.3159 0.9743 0.073 Uiso 1 1 calc R . . H23B H 0.9078 0.3678 0.9246 0.073 Uiso 1 1 calc R . . H23C H 0.9320 0.2664 0.9325 0.073 Uiso 1 1 calc R . . C36 C 0.6036(3) 0.5653(3) 0.81599(18) 0.0596(10) Uani 1 1 d . . . H36A H 0.5861 0.6271 0.8171 0.089 Uiso 1 1 calc R . . H36B H 0.6811 0.5585 0.8168 0.089 Uiso 1 1 calc R . . H36C H 0.5828 0.5361 0.8485 0.089 Uiso 1 1 calc R . . C21 C 0.3677(3) 0.1606(3) 0.93314(18) 0.0606(11) Uani 1 1 d . . . H21A H 0.3851 0.1332 0.9700 0.091 Uiso 1 1 calc R . . H21B H 0.2905 0.1547 0.9193 0.091 Uiso 1 1 calc R . . H21C H 0.3868 0.2222 0.9362 0.091 Uiso 1 1 calc R . . C32 C 0.1714(3) 0.4043(3) 0.86037(14) 0.0497(9) Uani 1 1 d . . . H32A H 0.2387 0.4151 0.8860 0.075 Uiso 1 1 calc R . . H32B H 0.1359 0.3532 0.8729 0.075 Uiso 1 1 calc R . . H32C H 0.1240 0.4547 0.8600 0.075 Uiso 1 1 calc R . . C46 C 0.7692(4) 0.4177(2) 0.65174(18) 0.0583(10) Uani 1 1 d . . . H46A H 0.7223 0.4582 0.6271 0.070 Uiso 1 1 calc R . . H46B H 0.8186 0.4517 0.6796 0.070 Uiso 1 1 calc R . . C33 C 0.0922(3) 0.3678(2) 0.76097(16) 0.0463(8) Uani 1 1 d . . . H33A H 0.0407 0.4152 0.7615 0.069 Uiso 1 1 calc R . . H33B H 0.0612 0.3139 0.7726 0.069 Uiso 1 1 calc R . . H33C H 0.1083 0.3610 0.7230 0.069 Uiso 1 1 calc R . . C35 C 0.5775(4) 0.5670(3) 0.71116(19) 0.0689(12) Uani 1 1 d . . . H35A H 0.5341 0.5441 0.6769 0.103 Uiso 1 1 calc R . . H35B H 0.6535 0.5540 0.7110 0.103 Uiso 1 1 calc R . . H35C H 0.5676 0.6299 0.7128 0.103 Uiso 1 1 calc R . . C24 C 0.7956(3) 0.2844(3) 0.83691(14) 0.0510(9) Uani 1 1 d . . . H24A H 0.8453 0.2363 0.8343 0.076 Uiso 1 1 calc R . . H24B H 0.8274 0.3385 0.8261 0.076 Uiso 1 1 calc R . . H24C H 0.7277 0.2735 0.8118 0.076 Uiso 1 1 calc R . . C45 C 0.8304(4) 0.3607(3) 0.61843(18) 0.0591(10) Uani 1 1 d . . . H45A H 0.8028 0.3676 0.5780 0.071 Uiso 1 1 calc R . . H45B H 0.9075 0.3766 0.6254 0.071 Uiso 1 1 calc R . . C47 C 0.7036(4) 0.3561(3) 0.68001(18) 0.0595(10) Uani 1 1 d . . . H47A H 0.6955 0.3771 0.7177 0.071 Uiso 1 1 calc R . . H47B H 0.6315 0.3473 0.6575 0.071 Uiso 1 1 calc R . . C48 C 0.7681(3) 0.2752(2) 0.68352(16) 0.0519(9) Uani 1 1 d . . . H48A H 0.8232 0.2750 0.7178 0.062 Uiso 1 1 calc R . . H48B H 0.7214 0.2238 0.6841 0.062 Uiso 1 1 calc R . . C15 C 0.6096(3) 0.0678(2) 0.94680(12) 0.0366(7) Uani 1 1 d . . . H15 H 0.5741 0.0184 0.9583 0.044 Uiso 1 1 calc R . . N1 N 0.54596(17) 0.26727(14) 0.86217(8) 0.0229(4) Uani 1 1 d . . . N2 N 0.42676(17) 0.38908(14) 0.80727(8) 0.0229(4) Uani 1 1 d . . . C37 C 0.3585(3) 0.6295(2) 0.88826(12) 0.0421(8) Uani 1 1 d . . . H37A H 0.2797 0.6210 0.8819 0.050 Uiso 1 1 calc R . . H37B H 0.3913 0.5849 0.8670 0.050 Uiso 1 1 calc R . . C38 C 0.3867(3) 0.7200(2) 0.87040(13) 0.0425(8) Uani 1 1 d . . . H38A H 0.3267 0.7451 0.8437 0.051 Uiso 1 1 calc R . . H38B H 0.4520 0.7188 0.8526 0.051 Uiso 1 1 calc R . . C40 C 0.3807(3) 0.7090(2) 0.96834(12) 0.0418(8) Uani 1 1 d . . . H40A H 0.4267 0.7198 1.0049 0.050 Uiso 1 1 calc R . . H40B H 0.3044 0.7142 0.9730 0.050 Uiso 1 1 calc R . . C39 C 0.4064(3) 0.7719(2) 0.92502(14) 0.0429(8) Uani 1 1 d . . . H39A H 0.4821 0.7914 0.9338 0.052 Uiso 1 1 calc R . . H39B H 0.3587 0.8232 0.9226 0.052 Uiso 1 1 calc R . . O2 O 0.67778(18) 0.55926(15) 0.98473(10) 0.0449(6) Uani 1 1 d . . . C41 C 0.7050(3) 0.6472(2) 0.97412(19) 0.0565(10) Uani 1 1 d . . . H41A H 0.6950 0.6848 1.0060 0.068 Uiso 1 1 calc R . . H41B H 0.6590 0.6691 0.9399 0.068 Uiso 1 1 calc R . . C44 C 0.7694(3) 0.5065(3) 0.9810(3) 0.0835(16) Uani 1 1 d . . . H44A H 0.7587 0.4743 0.9451 0.100 Uiso 1 1 calc R . . H44B H 0.7809 0.4641 1.0121 0.100 Uiso 1 1 calc R . . C42 C 0.8195(4) 0.6465(4) 0.9668(3) 0.0876(16) Uani 1 1 d . . . H42A H 0.8255 0.6567 0.9271 0.105 Uiso 1 1 calc R . . H42B H 0.8598 0.6926 0.9898 0.105 Uiso 1 1 calc R . . C43 C 0.8612(4) 0.5637(4) 0.9843(2) 0.0855(16) Uani 1 1 d . . . H43A H 0.9008 0.5663 1.0231 0.103 Uiso 1 1 calc R . . H43B H 0.9109 0.5430 0.9594 0.103 Uiso 1 1 calc R . . C49 C 0.4285(11) 0.6001(8) 0.5070(5) 0.100(4) Uiso 0.50 1 d PD A -1 H49A H 0.3560 0.5997 0.4849 0.150 Uiso 0.50 1 calc PR A -1 H49B H 0.4674 0.6513 0.4973 0.150 Uiso 0.50 1 calc PR A -1 H49C H 0.4235 0.6017 0.5470 0.150 Uiso 0.50 1 calc PR A -1 C55 C 0.5092(4) 0.4576(3) 0.53591(15) 0.0423(15) Uiso 0.50 1 d PGD A -1 H55 H 0.4871 0.4654 0.5712 0.051 Uiso 0.50 1 calc PR A -1 C50 C 0.4866(5) 0.5208(3) 0.4948(2) 0.074(3) Uiso 0.50 1 d PG A -1 C51 C 0.5190(5) 0.5094(3) 0.44307(17) 0.063(2) Uiso 0.50 1 d PGD A -1 H51 H 0.5035 0.5526 0.4149 0.076 Uiso 0.50 1 calc PR A -1 C52 C 0.5739(5) 0.4347(4) 0.43253(17) 0.062(2) Uiso 0.50 1 d PG A -1 H52 H 0.5961 0.4269 0.3972 0.075 Uiso 0.50 1 calc PR A -1 C53 C 0.5966(5) 0.3715(3) 0.4737(2) 0.063(2) Uiso 0.50 1 d PG A -1 H53 H 0.6342 0.3204 0.4665 0.076 Uiso 0.50 1 calc PR A -1 C54 C 0.5642(4) 0.3829(3) 0.52537(19) 0.0523(18) Uiso 0.50 1 d PG A -1 H54 H 0.5797 0.3397 0.5535 0.063 Uiso 0.50 1 calc PR A -1 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 Eu 0.02727(9) 0.02208(9) 0.02235(9) -0.00249(8) 0.00175(6) 0.00283(9) Ga 0.03247(16) 0.02501(15) 0.02045(13) -0.00404(11) -0.00135(11) 0.00964(12) O1 0.0466(12) 0.0280(11) 0.0254(9) -0.0015(8) 0.0021(8) 0.0092(9) C2 0.0189(12) 0.0212(13) 0.0228(12) -0.0003(10) 0.0024(9) 0.0001(10) C1 0.0199(12) 0.0222(12) 0.0199(11) -0.0018(10) 0.0026(9) 0.0014(10) C14 0.0358(15) 0.0243(14) 0.0237(12) -0.0003(11) 0.0044(11) 0.0066(11) C25 0.0278(13) 0.0214(12) 0.0171(11) 0.0000(10) 0.0015(10) 0.0055(10) C10 0.0248(13) 0.0228(13) 0.0286(13) -0.0017(11) 0.0040(10) -0.0017(10) C4 0.0289(14) 0.0271(14) 0.0269(13) 0.0023(11) 0.0010(11) -0.0023(11) C12 0.0220(12) 0.0220(13) 0.0215(11) -0.0019(10) 0.0040(9) -0.0033(10) C13 0.0289(13) 0.0229(13) 0.0181(11) -0.0031(10) 0.0017(10) 0.0102(11) C11 0.0207(12) 0.0203(12) 0.0245(12) -0.0023(10) 0.0036(9) -0.0010(10) C29 0.0472(18) 0.0222(14) 0.0292(14) 0.0025(11) 0.0052(12) -0.0007(12) C31 0.0287(15) 0.0262(15) 0.0473(17) 0.0052(13) 0.0076(12) 0.0026(12) C26 0.0270(14) 0.0235(12) 0.0252(12) -0.0007(11) -0.0002(10) 0.0027(11) C7 0.0297(14) 0.0295(14) 0.0244(12) -0.0060(11) 0.0074(10) -0.0076(11) C8 0.0349(15) 0.0305(15) 0.0307(14) -0.0120(12) 0.0102(12) -0.0070(12) C27 0.0259(14) 0.0278(15) 0.0345(14) -0.0006(12) -0.0043(11) 0.0052(12) C6 0.0407(16) 0.0393(17) 0.0204(12) -0.0056(12) 0.0038(11) -0.0085(13) C5 0.0376(16) 0.0387(17) 0.0208(12) 0.0052(12) 0.0005(11) -0.0069(13) C3 0.0196(12) 0.0220(13) 0.0241(12) 0.0004(10) 0.0027(9) -0.0032(10) C19 0.0396(16) 0.0271(15) 0.0315(14) 0.0029(12) 0.0027(12) -0.0014(12) C18 0.0296(14) 0.0297(14) 0.0250(12) -0.0045(11) 0.0023(10) 0.0107(11) C30 0.0342(15) 0.0244(13) 0.0241(12) -0.0020(10) 0.0073(11) 0.0009(11) C34 0.0382(17) 0.0257(15) 0.0585(19) -0.0036(13) 0.0205(15) -0.0008(12) C28 0.0434(17) 0.0222(14) 0.0335(14) 0.0026(12) -0.0041(12) 0.0108(12) O3 0.116(3) 0.0398(15) 0.0744(19) -0.0015(14) 0.0568(18) 0.0086(16) C22 0.0260(14) 0.0346(16) 0.0337(14) -0.0053(12) -0.0004(11) 0.0067(12) C17 0.0313(15) 0.0420(18) 0.0329(14) -0.0006(13) -0.0038(12) 0.0156(13) C20 0.057(2) 0.0315(18) 0.0479(18) 0.0026(14) 0.0005(16) -0.0093(14) C9 0.0327(15) 0.0223(14) 0.0373(15) -0.0068(12) 0.0112(12) -0.0004(11) C16 0.0479(19) 0.0398(18) 0.0348(15) 0.0079(14) -0.0010(14) 0.0199(15) C23 0.0341(18) 0.053(2) 0.053(2) -0.0104(17) -0.0070(15) 0.0012(15) C36 0.0332(18) 0.066(3) 0.080(3) -0.017(2) 0.0089(18) -0.0089(17) C21 0.040(2) 0.064(3) 0.082(3) -0.021(2) 0.0205(19) -0.0068(18) C32 0.045(2) 0.056(2) 0.0487(19) 0.0123(17) 0.0114(15) -0.0073(17) C46 0.075(3) 0.0354(19) 0.070(2) -0.0031(18) 0.028(2) -0.0023(18) C33 0.0361(17) 0.0353(18) 0.066(2) -0.0083(16) 0.0044(15) -0.0052(14) C35 0.075(3) 0.062(3) 0.083(3) 0.011(2) 0.052(2) -0.001(2) C24 0.054(2) 0.059(2) 0.0410(17) -0.0090(17) 0.0125(15) -0.0234(18) C45 0.066(3) 0.048(2) 0.071(3) 0.0082(19) 0.035(2) 0.0027(19) C47 0.064(3) 0.052(2) 0.070(3) 0.011(2) 0.034(2) 0.0118(19) C48 0.064(2) 0.041(2) 0.058(2) 0.0038(17) 0.0294(18) 0.0018(17) C15 0.0495(19) 0.0293(16) 0.0308(14) 0.0060(12) 0.0063(13) 0.0090(14) N1 0.0262(11) 0.0215(11) 0.0193(10) -0.0012(8) -0.0015(8) 0.0051(9) N2 0.0249(11) 0.0224(11) 0.0204(10) -0.0002(8) 0.0008(8) 0.0051(9) C37 0.064(2) 0.0353(17) 0.0249(14) -0.0018(13) 0.0010(14) 0.0060(16) C38 0.056(2) 0.0387(18) 0.0353(16) 0.0097(14) 0.0151(14) 0.0123(15) C40 0.064(2) 0.0309(16) 0.0291(14) -0.0037(12) 0.0027(14) 0.0136(15) C39 0.0465(19) 0.0295(17) 0.0516(19) 0.0006(14) 0.0043(15) -0.0016(14) O2 0.0350(12) 0.0349(12) 0.0672(15) -0.0081(11) 0.0151(11) -0.0015(10) C41 0.062(2) 0.0359(19) 0.078(3) 0.0021(18) 0.031(2) -0.0037(17) C44 0.041(2) 0.052(3) 0.159(5) -0.032(3) 0.022(3) 0.007(2) C42 0.053(3) 0.078(3) 0.137(5) 0.024(3) 0.029(3) -0.015(2) C43 0.053(3) 0.103(4) 0.108(4) 0.036(3) 0.036(3) 0.008(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 Eu Ga 3.3239(6) . ? Eu Ga 3.3239(6) 3_667 ? Eu O1 2.516(2) . ? Eu O1 2.516(2) 3_667 ? Eu O2 2.505(2) 3_667 ? Eu O2 2.505(2) . ? Ga N1 1.968(2) . ? Ga N2 1.958(2) . ? O1 C37 1.443(3) . ? O1 C40 1.444(4) . ? C2 C1 1.381(3) . ? C2 C3 1.464(3) . ? C2 N2 1.368(3) . ? C1 C11 1.461(3) . ? C1 N1 1.384(3) . ? C14 C13 1.413(4) . ? C14 C19 1.512(4) . ? C14 C15 1.394(4) . ? C25 C26 1.395(4) . ? C25 C30 1.407(4) . ? C25 N2 1.423(3) . ? C10 C11 1.374(4) . ? C10 C9 1.420(4) . ? C4 C5 1.430(4) . ? C4 C3 1.377(4) . ? C12 C11 1.424(3) . ? C12 C7 1.386(3) . ? C12 C3 1.428(4) . ? C13 C18 1.412(4) . ? C13 N1 1.422(3) . ? C29 C30 1.393(4) . ? C29 C28 1.385(4) . ? C31 C26 1.522(4) . ? C31 C32 1.533(5) . ? C31 C33 1.528(4) . ? C26 C27 1.396(4) . ? C7 C8 1.428(4) . ? C7 C6 1.426(4) . ? C8 C9 1.371(4) . ? C27 C28 1.378(4) . ? C6 C5 1.368(4) . ? C19 C20 1.527(4) . ? C19 C21 1.525(5) . ? C18 C22 1.515(4) . ? C18 C17 1.400(4) . ? C30 C34 1.522(4) . ? C34 C36 1.537(5) . ? C34 C35 1.519(5) . ? O3 C45 1.397(5) . ? O3 C48 1.420(4) . ? C22 C23 1.523(4) . ? C22 C24 1.525(4) . ? C17 C16 1.383(5) . ? C16 C15 1.378(5) . ? C46 C45 1.492(5) . ? C46 C47 1.498(5) . ? C47 C48 1.484(5) . ? C37 C38 1.521(5) . ? C38 C39 1.531(5) . ? C40 C39 1.503(5) . ? O2 C41 1.433(4) . ? O2 C44 1.429(4) . ? C41 C42 1.483(6) . ? C44 C43 1.448(7) . ? C42 C43 1.420(7) . ? C49 C50 1.481(13) . ? C55 C50 1.3900 . ? C55 C54 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? 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 Ga Eu Ga 180.0 3_667 . ? O1 Eu Ga 93.77(5) . . ? O1 Eu Ga 86.23(5) 3_667 . ? O1 Eu Ga 86.23(5) . 3_667 ? O1 Eu Ga 93.77(5) 3_667 3_667 ? O1 Eu O1 179.998(1) . 3_667 ? O2 Eu Ga 90.36(6) 3_667 3_667 ? O2 Eu Ga 89.64(6) . 3_667 ? O2 Eu Ga 90.36(6) . . ? O2 Eu Ga 89.64(6) 3_667 . ? O2 Eu O1 88.67(8) . 3_667 ? O2 Eu O1 91.33(8) 3_667 3_667 ? O2 Eu O1 91.33(8) . . ? O2 Eu O1 88.67(8) 3_667 . ? O2 Eu O2 180.0 . 3_667 ? N1 Ga Eu 140.44(6) . . ? N2 Ga Eu 135.30(6) . . ? N2 Ga N1 84.00(9) . . ? C37 O1 Eu 128.18(17) . . ? C37 O1 C40 103.8(2) . . ? C40 O1 Eu 127.92(16) . . ? C1 C2 C3 109.1(2) . . ? N2 C2 C1 117.0(2) . . ? N2 C2 C3 133.9(2) . . ? C2 C1 C11 109.6(2) . . ? C2 C1 N1 116.9(2) . . ? N1 C1 C11 133.5(2) . . ? C13 C14 C19 121.0(2) . . ? C15 C14 C13 118.1(3) . . ? C15 C14 C19 120.8(3) . . ? C26 C25 C30 120.9(2) . . ? C26 C25 N2 119.8(2) . . ? C30 C25 N2 119.1(2) . . ? C11 C10 C9 118.7(2) . . ? C3 C4 C5 118.5(3) . . ? C11 C12 C3 111.0(2) . . ? C7 C12 C11 124.5(2) . . ? C7 C12 C3 124.5(2) . . ? C14 C13 N1 119.8(2) . . ? C18 C13 C14 120.8(2) . . ? C18 C13 N1 119.3(2) . . ? C10 C11 C1 137.0(2) . . ? C10 C11 C12 117.9(2) . . ? C12 C11 C1 105.1(2) . . ? C28 C29 C30 121.0(3) . . ? C26 C31 C32 110.8(3) . . ? C26 C31 C33 112.5(3) . . ? C33 C31 C32 110.3(3) . . ? C25 C26 C31 121.0(2) . . ? C25 C26 C27 118.8(3) . . ? C27 C26 C31 120.1(2) . . ? C12 C7 C8 116.2(2) . . ? C12 C7 C6 116.3(3) . . ? C6 C7 C8 127.5(2) . . ? C9 C8 C7 119.9(2) . . ? C28 C27 C26 120.8(3) . . ? C5 C6 C7 120.0(3) . . ? C6 C5 C4 122.8(3) . . ? C4 C3 C2 137.0(3) . . ? C4 C3 C12 117.8(2) . . ? C12 C3 C2 105.2(2) . . ? C14 C19 C20 113.9(3) . . ? C14 C19 C21 110.7(3) . . ? C21 C19 C20 110.0(3) . . ? C13 C18 C22 121.0(2) . . ? C17 C18 C13 118.3(3) . . ? C17 C18 C22 120.7(3) . . ? C25 C30 C34 120.4(2) . . ? C29 C30 C25 118.3(3) . . ? C29 C30 C34 121.2(3) . . ? C30 C34 C36 110.6(3) . . ? C35 C34 C30 113.2(3) . . ? C35 C34 C36 110.1(3) . . ? C27 C28 C29 120.0(3) . . ? C45 O3 C48 108.8(3) . . ? C18 C22 C23 114.4(3) . . ? C18 C22 C24 111.6(2) . . ? C23 C22 C24 109.2(3) . . ? C16 C17 C18 121.2(3) . . ? C8 C9 C10 122.8(3) . . ? C15 C16 C17 119.9(3) . . ? C45 C46 C47 104.2(3) . . ? O3 C45 C46 108.0(3) . . ? C48 C47 C46 102.8(3) . . ? O3 C48 C47 105.3(3) . . ? C16 C15 C14 121.7(3) . . ? C1 N1 Ga 110.63(16) . . ? C1 N1 C13 120.6(2) . . ? C13 N1 Ga 128.66(16) . . ? C2 N2 Ga 111.51(16) . . ? C2 N2 C25 121.8(2) . . ? C25 N2 Ga 126.61(16) . . ? O1 C37 C38 105.2(3) . . ? C37 C38 C39 104.3(2) . . ? O1 C40 C39 105.2(2) . . ? C40 C39 C38 104.0(3) . . ? C41 O2 Eu 128.2(2) . . ? C44 O2 Eu 123.7(2) . . ? C44 O2 C41 107.9(3) . . ? O2 C41 C42 106.4(3) . . ? O2 C44 C43 107.3(4) . . ? C43 C42 C41 106.9(4) . . ? C42 C43 C44 106.2(4) . . ? C50 C55 C54 120.0 . . ? C55 C50 C49 119.1(5) . . ? C55 C50 C51 120.0 . . ? C51 C50 C49 120.9(5) . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? #============================================================================== data_3 _audit_creation_date 2012-02-17 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C88 H112 Ga2 N4 O4 Yb' _chemical_formula_sum 'C88 H112 Ga2 N4 O4 Yb' _chemical_formula_weight 1602.30 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' 'Ga' 'Ga' 0.2307 1.6083 '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' 'Yb' 'Yb' -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _symmetry_space_group_name_H-M 'P 21/n' _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 13.6617(5) _cell_length_b 14.3216(4) _cell_length_c 20.1983(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.575(3) _cell_angle_gamma 90.00 _cell_volume 3951.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15063 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 29.44 _exptl_crystal_description 'rhombus' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.168 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.021 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.902 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8958 _exptl_absorpt_correction_T_max 0.9801 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24572 _diffrn_reflns_av_R_equivalents 0.0889 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7022 _reflns_number_gt 4635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; Diamond 2.1e/3 O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. Microsoft Word ; _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^)+(0.0249P)^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 7022 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _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 Yb Yb 0.5000 0.0000 0.5000 0.02587(8) Uani 1 2 d S . . Ga Ga 0.67862(4) 0.13680(3) 0.50299(3) 0.02361(12) Uani 1 1 d . . . O1 O 0.5482(3) -0.0410(2) 0.38831(17) 0.0379(8) Uani 1 1 d . . . O2 O 0.3888(3) 0.1184(2) 0.4615(2) 0.0460(10) Uani 1 1 d . B . N1 N 0.7451(3) 0.2016(2) 0.57435(19) 0.0237(9) Uani 1 1 d . . . N2 N 0.7859(3) 0.1847(2) 0.44856(17) 0.0223(8) Uani 1 1 d . . . C1 C 0.8282(3) 0.2454(3) 0.5525(2) 0.0226(9) Uani 1 1 d . . . C2 C 0.8506(3) 0.2362(3) 0.4863(2) 0.0229(9) Uani 1 1 d . . . C3 C 0.9383(3) 0.2927(3) 0.4723(2) 0.0240(9) Uani 1 1 d . . . C4 C 0.9899(3) 0.3197(3) 0.4175(2) 0.0296(10) Uani 1 1 d . . . H4 H 0.9723 0.2973 0.3747 0.036 Uiso 1 1 calc R . . C5 C 1.0705(4) 0.3820(3) 0.4262(3) 0.0330(11) Uani 1 1 d . . . H5 H 1.1054 0.4014 0.3882 0.040 Uiso 1 1 calc R . . C6 C 1.0994(4) 0.4148(3) 0.4862(3) 0.0351(12) Uani 1 1 d . . . H6 H 1.1548 0.4548 0.4894 0.042 Uiso 1 1 calc R . . C7 C 1.0476(4) 0.3900(3) 0.5443(2) 0.0313(11) Uani 1 1 d . . . C8 C 1.0670(4) 0.4200(3) 0.6100(3) 0.0388(12) Uani 1 1 d . . . H8 H 1.1219 0.4586 0.6195 0.047 Uiso 1 1 calc R . . C9 C 1.0052(4) 0.3922(3) 0.6603(3) 0.0425(13) Uani 1 1 d . . . H9 H 1.0196 0.4115 0.7043 0.051 Uiso 1 1 calc R . . C10 C 0.9206(4) 0.3358(3) 0.6484(3) 0.0377(12) Uani 1 1 d . . . H10 H 0.8773 0.3212 0.6834 0.045 Uiso 1 1 calc R . . C11 C 0.9026(3) 0.3030(3) 0.5855(2) 0.0245(10) Uani 1 1 d . . . C12 C 0.9689(3) 0.3304(3) 0.5344(2) 0.0253(10) Uani 1 1 d . . . C13 C 0.7031(3) 0.2316(3) 0.6349(2) 0.0226(9) Uani 1 1 d . . . C14 C 0.7145(3) 0.1779(3) 0.6923(2) 0.0283(10) Uani 1 1 d . . . C15 C 0.6684(4) 0.2065(3) 0.7501(2) 0.0347(11) Uani 1 1 d . . . H15 H 0.6761 0.1708 0.7895 0.042 Uiso 1 1 calc R . . C16 C 0.6114(4) 0.2865(3) 0.7506(3) 0.0387(13) Uani 1 1 d . . . H16 H 0.5800 0.3054 0.7902 0.046 Uiso 1 1 calc R . . C17 C 0.6002(4) 0.3388(3) 0.6938(2) 0.0352(12) Uani 1 1 d . . . H17 H 0.5601 0.3930 0.6943 0.042 Uiso 1 1 calc R . . C18 C 0.6465(3) 0.3133(3) 0.6356(2) 0.0273(10) Uani 1 1 d . . . C19 C 0.7762(4) 0.0897(3) 0.6929(2) 0.0326(11) Uani 1 1 d . . . H19 H 0.8052 0.0830 0.6479 0.039 Uiso 1 1 calc R . . C20 C 0.8599(5) 0.0955(4) 0.7419(3) 0.0529(15) Uani 1 1 d . . . H20A H 0.9038 0.1465 0.7293 0.079 Uiso 1 1 calc R . . H20B H 0.8962 0.0364 0.7420 0.079 Uiso 1 1 calc R . . H20C H 0.8343 0.1073 0.7863 0.079 Uiso 1 1 calc R . . C21 C 0.7134(4) 0.0030(4) 0.7051(3) 0.0601(15) Uani 1 1 d . . . H21A H 0.6850 0.0064 0.7494 0.090 Uiso 1 1 calc R . . H21B H 0.7542 -0.0531 0.7018 0.090 Uiso 1 1 calc R . . H21C H 0.6607 0.0001 0.6718 0.090 Uiso 1 1 calc R . . C22 C 0.6306(4) 0.3721(3) 0.5732(3) 0.0362(12) Uani 1 1 d . . . H22 H 0.6726 0.3447 0.5379 0.043 Uiso 1 1 calc R . . C23 C 0.6641(5) 0.4727(3) 0.5835(3) 0.0541(17) Uani 1 1 d . . . H23A H 0.6210 0.5035 0.6153 0.081 Uiso 1 1 calc R . . H23B H 0.6615 0.5061 0.5412 0.081 Uiso 1 1 calc R . . H23C H 0.7315 0.4730 0.6008 0.081 Uiso 1 1 calc R . . C24 C 0.5266(5) 0.3674(4) 0.5485(4) 0.0634(18) Uani 1 1 d . . . H24A H 0.5078 0.3020 0.5419 0.095 Uiso 1 1 calc R . . H24B H 0.5208 0.4010 0.5064 0.095 Uiso 1 1 calc R . . H24C H 0.4833 0.3961 0.5811 0.095 Uiso 1 1 calc R . . C25 C 0.8011(3) 0.1696(3) 0.3796(2) 0.0253(10) Uani 1 1 d . . . C26 C 0.8673(3) 0.0995(3) 0.3587(2) 0.0262(10) Uani 1 1 d . . . C27 C 0.8776(4) 0.0850(3) 0.2913(2) 0.0365(12) Uani 1 1 d . . . H27 H 0.9223 0.0388 0.2766 0.044 Uiso 1 1 calc R . . C28 C 0.8254(4) 0.1352(3) 0.2455(2) 0.0392(12) Uani 1 1 d . . . H28 H 0.8346 0.1245 0.1995 0.047 Uiso 1 1 calc R . . C29 C 0.7590(4) 0.2017(3) 0.2665(2) 0.0352(11) Uani 1 1 d . . . H29 H 0.7216 0.2352 0.2345 0.042 Uiso 1 1 calc R . . C30 C 0.7461(3) 0.2203(3) 0.3331(2) 0.0268(10) Uani 1 1 d . . . C31 C 0.9237(4) 0.0386(3) 0.4077(2) 0.0319(12) Uani 1 1 d . . . H31 H 0.8964 0.0514 0.4526 0.038 Uiso 1 1 calc R . . C32 C 0.9102(5) -0.0658(3) 0.3945(3) 0.0445(15) Uani 1 1 d . . . H32A H 0.9406 -0.1017 0.4305 0.067 Uiso 1 1 calc R . . H32B H 0.9413 -0.0822 0.3525 0.067 Uiso 1 1 calc R . . H32C H 0.8402 -0.0804 0.3919 0.067 Uiso 1 1 calc R . . C33 C 1.0323(4) 0.0631(3) 0.4107(3) 0.0405(13) Uani 1 1 d . . . H33A H 1.0603 0.0576 0.3664 0.061 Uiso 1 1 calc R . . H33B H 1.0662 0.0201 0.4410 0.061 Uiso 1 1 calc R . . H33C H 1.0403 0.1273 0.4267 0.061 Uiso 1 1 calc R . . C34 C 0.6722(4) 0.2934(3) 0.3559(2) 0.0315(11) Uani 1 1 d . . . H34 H 0.6408 0.2682 0.3967 0.038 Uiso 1 1 calc R . . C35 C 0.5906(4) 0.3136(4) 0.3065(3) 0.0469(14) Uani 1 1 d . . . H35A H 0.6183 0.3414 0.2665 0.070 Uiso 1 1 calc R . . H35B H 0.5439 0.3572 0.3261 0.070 Uiso 1 1 calc R . . H35C H 0.5570 0.2553 0.2949 0.070 Uiso 1 1 calc R . . C36 C 0.7230(4) 0.3843(3) 0.3756(3) 0.0431(13) Uani 1 1 d . . . H36A H 0.7720 0.3717 0.4102 0.065 Uiso 1 1 calc R . . H36B H 0.6744 0.4285 0.3924 0.065 Uiso 1 1 calc R . . H36C H 0.7551 0.4112 0.3369 0.065 Uiso 1 1 calc R . . C37 C 0.6002(5) 0.0192(3) 0.3440(3) 0.0559(18) Uani 1 1 d . . . H37A H 0.6550 0.0501 0.3678 0.067 Uiso 1 1 calc R . . H37B H 0.5558 0.0680 0.3264 0.067 Uiso 1 1 calc R . . C38 C 0.6386(5) -0.0392(4) 0.2886(3) 0.0524(15) Uani 1 1 d . . . H38A H 0.6428 -0.0026 0.2471 0.063 Uiso 1 1 calc R . . H38B H 0.7040 -0.0649 0.2996 0.063 Uiso 1 1 calc R . . C39 C 0.5668(5) -0.1123(4) 0.2827(3) 0.0592(17) Uani 1 1 d . . . H39A H 0.5947 -0.1686 0.2616 0.071 Uiso 1 1 calc R . . H39B H 0.5090 -0.0913 0.2567 0.071 Uiso 1 1 calc R . . C40 C 0.5395(5) -0.1316(3) 0.3562(3) 0.0515(15) Uani 1 1 d . . . H40A H 0.4719 -0.1559 0.3594 0.062 Uiso 1 1 calc R . . H40B H 0.5851 -0.1773 0.3765 0.062 Uiso 1 1 calc R . . C41 C 0.4021(5) 0.1937(3) 0.4155(3) 0.0550(16) Uani 1 1 d . B . H41A H 0.4077 0.1694 0.3698 0.066 Uiso 1 1 calc R . . H41B H 0.4621 0.2294 0.4267 0.066 Uiso 1 1 calc R . . C42 C 0.3122(6) 0.2551(5) 0.4217(4) 0.085(3) Uani 1 1 d . . . H42A H 0.2695 0.2488 0.3820 0.102 Uiso 0.70 1 calc PR A 1 H42B H 0.3314 0.3214 0.4266 0.102 Uiso 0.70 1 calc PR A 1 H42C H 0.3220 0.3037 0.4560 0.102 Uiso 0.30 1 calc PR A 2 H42D H 0.2957 0.2856 0.3790 0.102 Uiso 0.30 1 calc PR A 2 C43A C 0.2595(8) 0.2212(6) 0.4832(7) 0.065(3) Uani 0.70 1 d P B 1 H43A H 0.2819 0.2554 0.5232 0.078 Uiso 0.70 1 calc PR B 1 H43B H 0.1877 0.2279 0.4783 0.078 Uiso 0.70 1 calc PR B 1 C43B C 0.2421(19) 0.194(2) 0.4394(15) 0.068(8) Uani 0.30 1 d P B 2 H43C H 0.2148 0.1622 0.3997 0.082 Uiso 0.30 1 calc PR B 2 H43D H 0.1882 0.2268 0.4621 0.082 Uiso 0.30 1 calc PR B 2 C44 C 0.2887(5) 0.1226(5) 0.4858(5) 0.089(3) Uani 1 1 d . . . H44A H 0.2857 0.0989 0.5317 0.107 Uiso 0.70 1 calc PR B 1 H44B H 0.2447 0.0843 0.4575 0.107 Uiso 0.70 1 calc PR B 1 H44C H 0.2869 0.1439 0.5323 0.107 Uiso 0.30 1 calc PR B 2 H44D H 0.2559 0.0611 0.4821 0.107 Uiso 0.30 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb 0.02275(15) 0.02440(12) 0.03043(15) 0.00510(15) -0.00122(10) -0.00424(15) Ga 0.0241(3) 0.0260(2) 0.0208(3) -0.0029(2) 0.0027(2) -0.0066(2) O1 0.044(2) 0.0324(15) 0.037(2) -0.0008(14) 0.0069(16) -0.0152(15) O2 0.030(2) 0.0430(19) 0.065(3) 0.0276(18) 0.0038(19) 0.0074(15) N1 0.026(2) 0.0236(18) 0.021(2) -0.0026(15) 0.0035(17) -0.0050(16) N2 0.022(2) 0.0255(17) 0.0191(19) -0.0017(14) 0.0040(15) -0.0043(14) C1 0.026(3) 0.0224(19) 0.019(2) -0.0016(16) 0.0033(19) -0.0046(17) C2 0.024(3) 0.026(2) 0.019(2) 0.0009(16) 0.0007(18) -0.0032(17) C3 0.021(3) 0.0206(19) 0.030(2) -0.0011(17) 0.0033(19) -0.0014(16) C4 0.026(3) 0.029(2) 0.034(3) -0.0051(19) 0.006(2) -0.0009(18) C5 0.024(3) 0.034(2) 0.041(3) 0.000(2) 0.011(2) -0.0005(19) C6 0.026(3) 0.029(2) 0.051(3) 0.002(2) 0.006(2) -0.0070(19) C7 0.026(3) 0.030(2) 0.038(3) -0.0030(19) 0.002(2) -0.0048(18) C8 0.034(3) 0.040(3) 0.042(3) -0.006(2) -0.003(2) -0.018(2) C9 0.042(3) 0.049(3) 0.037(3) -0.011(2) -0.009(2) -0.016(2) C10 0.040(3) 0.036(2) 0.037(3) -0.005(2) 0.001(2) -0.012(2) C11 0.021(3) 0.027(2) 0.025(2) -0.0004(17) 0.0009(19) 0.0022(17) C12 0.022(3) 0.023(2) 0.030(3) -0.0026(18) 0.000(2) -0.0027(17) C13 0.021(3) 0.026(2) 0.020(2) -0.0028(17) 0.0000(18) -0.0095(17) C14 0.027(3) 0.031(2) 0.027(2) -0.0029(18) 0.006(2) -0.0063(18) C15 0.041(3) 0.038(3) 0.025(3) 0.001(2) 0.005(2) -0.008(2) C16 0.046(4) 0.040(3) 0.030(3) -0.009(2) 0.017(2) -0.006(2) C17 0.042(3) 0.029(2) 0.035(3) -0.008(2) 0.011(2) 0.001(2) C18 0.027(3) 0.022(2) 0.032(3) 0.0007(17) -0.001(2) -0.0078(17) C19 0.034(3) 0.039(3) 0.024(2) 0.0014(19) 0.000(2) 0.008(2) C20 0.050(4) 0.054(3) 0.055(4) 0.005(3) -0.012(3) 0.005(3) C21 0.047(3) 0.030(2) 0.102(5) -0.005(4) -0.008(3) 0.002(3) C22 0.044(3) 0.027(2) 0.038(3) 0.001(2) 0.009(2) 0.006(2) C23 0.070(5) 0.038(3) 0.055(4) 0.008(2) 0.013(3) -0.020(2) C24 0.060(4) 0.052(3) 0.078(5) 0.027(3) -0.025(4) -0.011(3) C25 0.026(3) 0.028(2) 0.022(2) 0.0001(17) 0.0064(19) -0.0090(18) C26 0.028(3) 0.029(2) 0.022(2) -0.0009(17) 0.0043(19) -0.0038(18) C27 0.045(3) 0.038(2) 0.027(3) -0.002(2) 0.012(2) 0.000(2) C28 0.050(4) 0.049(3) 0.020(2) -0.003(2) 0.003(2) -0.001(2) C29 0.038(3) 0.043(3) 0.025(3) 0.008(2) -0.002(2) -0.005(2) C30 0.027(3) 0.031(2) 0.022(2) 0.0020(18) 0.0019(19) -0.0096(18) C31 0.036(3) 0.034(2) 0.025(3) -0.0007(19) 0.006(2) 0.006(2) C32 0.045(4) 0.038(3) 0.050(4) 0.005(3) 0.000(3) -0.002(2) C33 0.040(3) 0.039(3) 0.043(3) 0.000(2) -0.011(2) 0.002(2) C34 0.025(3) 0.038(2) 0.032(3) 0.007(2) 0.002(2) -0.0003(19) C35 0.039(4) 0.053(3) 0.049(3) 0.011(3) -0.010(3) 0.006(2) C36 0.045(4) 0.034(3) 0.051(3) 0.001(2) 0.000(3) 0.003(2) C37 0.093(5) 0.040(4) 0.034(3) -0.007(2) 0.014(3) -0.028(3) C38 0.054(4) 0.062(3) 0.041(3) 0.009(3) 0.000(3) -0.001(3) C39 0.063(5) 0.062(4) 0.053(4) -0.014(3) 0.023(3) 0.003(3) C40 0.054(4) 0.028(2) 0.072(4) -0.007(3) 0.008(3) -0.014(2) C41 0.068(5) 0.035(3) 0.061(4) 0.017(3) -0.009(3) -0.007(3) C42 0.089(7) 0.059(4) 0.107(7) 0.039(4) 0.005(5) 0.027(4) C43A 0.055(7) 0.045(5) 0.095(9) 0.022(5) 0.002(6) 0.015(4) C43B 0.033(15) 0.10(2) 0.067(19) 0.006(16) -0.017(13) -0.005(13) C44 0.038(5) 0.074(5) 0.156(9) 0.043(5) 0.029(5) 0.021(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 Yb O2 2.402(3) 3_656 ? Yb O2 2.402(3) . ? Yb O1 2.428(3) 3_656 ? Yb O1 2.428(3) . ? Yb Ga 3.1295(5) . ? Yb Ga 3.1296(5) 3_656 ? Ga N1 1.933(4) . ? Ga N2 1.965(3) . ? O1 C37 1.435(6) . ? O1 C40 1.454(6) . ? O2 C41 1.435(6) . ? O2 C44 1.458(7) . ? N1 C1 1.374(6) . ? N1 C13 1.422(6) . ? N2 C2 1.375(5) . ? N2 C25 1.427(5) . ? C1 C2 1.382(6) . ? C1 C11 1.463(6) . ? C2 C3 1.477(6) . ? C3 C4 1.373(6) . ? C3 C12 1.425(6) . ? C4 C5 1.427(6) . ? C5 C6 1.355(7) . ? C6 C7 1.422(7) . ? C7 C12 1.386(6) . ? C7 C8 1.418(7) . ? C8 C9 1.385(7) . ? C9 C10 1.429(7) . ? C10 C11 1.374(7) . ? C11 C12 1.435(6) . ? C13 C14 1.399(6) . ? C13 C18 1.403(6) . ? C14 C15 1.394(6) . ? C14 C19 1.519(6) . ? C15 C16 1.386(7) . ? C16 C17 1.377(7) . ? C17 C18 1.388(6) . ? C18 C22 1.530(6) . ? C19 C20 1.508(8) . ? C19 C21 1.530(8) . ? C22 C24 1.503(8) . ? C22 C23 1.526(6) . ? C25 C30 1.400(7) . ? C25 C26 1.418(6) . ? C26 C27 1.385(6) . ? C26 C31 1.524(7) . ? C27 C28 1.368(7) . ? C28 C29 1.384(7) . ? C29 C30 1.386(6) . ? C30 C34 1.528(6) . ? C31 C33 1.525(8) . ? C31 C32 1.529(7) . ? C34 C35 1.517(7) . ? C34 C36 1.526(7) . ? C37 C38 1.497(7) . ? C38 C39 1.438(8) . ? C39 C40 1.559(8) . ? C41 C42 1.516(9) . ? C42 C43B 1.35(3) . ? C42 C43A 1.521(13) . ? C43A C44 1.469(11) . ? C43B C44 1.52(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Yb O2 179.999(1) 3_656 . ? O2 Yb O1 92.65(13) 3_656 3_656 ? O2 Yb O1 87.35(13) . 3_656 ? O2 Yb O1 87.35(13) 3_656 . ? O2 Yb O1 92.65(13) . . ? O1 Yb O1 180.0 3_656 . ? O2 Yb Ga 86.85(9) 3_656 . ? O2 Yb Ga 93.15(9) . . ? O1 Yb Ga 92.82(8) 3_656 . ? O1 Yb Ga 87.18(8) . . ? O2 Yb Ga 93.15(9) 3_656 3_656 ? O2 Yb Ga 86.85(9) . 3_656 ? O1 Yb Ga 87.18(8) 3_656 3_656 ? O1 Yb Ga 92.82(8) . 3_656 ? Ga Yb Ga 180.000(1) . 3_656 ? N1 Ga N2 84.37(15) . . ? N1 Ga Yb 132.49(11) . . ? N2 Ga Yb 142.54(10) . . ? C37 O1 C40 107.2(4) . . ? C37 O1 Yb 125.0(3) . . ? C40 O1 Yb 127.5(3) . . ? C41 O2 C44 108.2(4) . . ? C41 O2 Yb 131.0(3) . . ? C44 O2 Yb 120.8(3) . . ? C1 N1 C13 118.7(4) . . ? C1 N1 Ga 111.3(3) . . ? C13 N1 Ga 126.5(3) . . ? C2 N2 C25 121.6(3) . . ? C2 N2 Ga 110.9(3) . . ? C25 N2 Ga 127.6(3) . . ? N1 C1 C2 117.3(4) . . ? N1 C1 C11 133.1(4) . . ? C2 C1 C11 109.6(4) . . ? N2 C2 C1 116.2(4) . . ? N2 C2 C3 135.0(4) . . ? C1 C2 C3 108.7(4) . . ? C4 C3 C12 117.1(4) . . ? C4 C3 C2 137.1(4) . . ? C12 C3 C2 105.7(4) . . ? C3 C4 C5 118.5(5) . . ? C6 C5 C4 123.1(4) . . ? C5 C6 C7 120.5(4) . . ? C12 C7 C8 117.3(4) . . ? C12 C7 C6 115.3(4) . . ? C8 C7 C6 127.4(4) . . ? C9 C8 C7 119.4(4) . . ? C8 C9 C10 122.5(5) . . ? C11 C10 C9 119.1(5) . . ? C10 C11 C12 117.5(4) . . ? C10 C11 C1 136.9(4) . . ? C12 C11 C1 105.5(4) . . ? C7 C12 C3 125.4(4) . . ? C7 C12 C11 124.1(4) . . ? C3 C12 C11 110.4(4) . . ? C14 C13 C18 120.4(4) . . ? C14 C13 N1 120.3(4) . . ? C18 C13 N1 119.2(4) . . ? C15 C14 C13 119.1(4) . . ? C15 C14 C19 119.5(4) . . ? C13 C14 C19 121.4(4) . . ? C16 C15 C14 120.5(4) . . ? C17 C16 C15 120.1(4) . . ? C16 C17 C18 120.9(4) . . ? C17 C18 C13 119.0(4) . . ? C17 C18 C22 119.3(4) . . ? C13 C18 C22 121.6(4) . . ? C20 C19 C14 112.1(4) . . ? C20 C19 C21 111.3(4) . . ? C14 C19 C21 111.4(4) . . ? C24 C22 C23 111.7(5) . . ? C24 C22 C18 112.0(4) . . ? C23 C22 C18 111.5(4) . . ? C30 C25 C26 120.5(4) . . ? C30 C25 N2 119.6(4) . . ? C26 C25 N2 119.9(4) . . ? C27 C26 C25 118.1(4) . . ? C27 C26 C31 119.8(4) . . ? C25 C26 C31 122.1(4) . . ? C28 C27 C26 121.9(5) . . ? C27 C28 C29 119.5(4) . . ? C28 C29 C30 121.3(5) . . ? C29 C30 C25 118.6(4) . . ? C29 C30 C34 121.0(4) . . ? C25 C30 C34 120.3(4) . . ? C26 C31 C33 112.3(4) . . ? C26 C31 C32 112.8(5) . . ? C33 C31 C32 110.3(4) . . ? C35 C34 C36 109.7(4) . . ? C35 C34 C30 114.6(4) . . ? C36 C34 C30 111.3(4) . . ? O1 C37 C38 108.1(4) . . ? C39 C38 C37 102.9(5) . . ? C38 C39 C40 102.7(5) . . ? O1 C40 C39 104.3(4) . . ? O2 C41 C42 106.0(5) . . ? C43B C42 C41 102.8(13) . . ? C41 C42 C43A 105.8(6) . . ? C44 C43A C42 101.9(8) . . ? C42 C43B C44 107.8(17) . . ? O2 C44 C43A 106.4(6) . . ? O2 C44 C43B 102.0(12) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.928 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.089 #============================================================================== data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H128 Ga2 I N4 O6 Tm, (C4 H8 O)' _chemical_formula_sum 'C100 H136 Ga2 I N4 O7 Tm' _chemical_formula_weight 1941.40 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' 'Tm' 'Tm' -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 _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 46.0961(15) _cell_length_b 20.8634(9) _cell_length_c 25.2675(8) _cell_angle_alpha 90.00 _cell_angle_beta 122.319(2) _cell_angle_gamma 90.00 _cell_volume 20535.8(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44241 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 26.49 _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.423 _exptl_crystal_size_mid 0.242 _exptl_crystal_size_min 0.079 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8032 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7178 _exptl_absorpt_correction_T_max 0.7954 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91276 _diffrn_reflns_av_R_equivalents 0.1066 _diffrn_reflns_av_sigmaI/netI 0.1087 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.25 _reflns_number_total 18592 _reflns_number_gt 9083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_molecular_graphics ; Diamond 2.1e/3 O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. Microsoft Word ; _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^)+(0.0112P)^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 18592 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.004 _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 Tm Tm 0.071117(7) 0.160670(13) 0.071731(13) 0.05062(8) Uani 1 1 d . . . I I 0.037224(11) 0.05606(2) 0.10310(2) 0.07186(14) Uani 1 1 d . . . Ga1 Ga 0.201727(14) 0.48558(3) 0.06762(3) 0.03786(15) Uani 1 1 d . . . Ga2 Ga 0.139712(14) 0.51007(3) 0.02870(3) 0.03874(15) Uani 1 1 d . . . O1 O 0.09110(10) 0.23076(18) 0.04945(19) 0.0592(11) Uani 1 1 d U . . O2 O 0.04504(9) 0.24220(19) 0.09841(19) 0.0646(12) Uani 1 1 d . . . O3 O 0.01634(9) 0.18263(18) -0.01891(18) 0.0647(12) Uani 1 1 d . . . O4 O 0.06548(9) 0.09572(18) -0.00984(17) 0.0564(11) Uani 1 1 d . . . O5 O 0.12343(9) 0.10475(18) 0.11119(17) 0.0535(10) Uani 1 1 d . . . O6 O 0.10663(9) 0.17874(18) 0.18197(17) 0.0574(11) Uani 1 1 d . . . O7 O 0.13690(17) 0.0527(3) 0.5031(3) 0.132(2) Uani 1 1 d . . . N1 N 0.24347(10) 0.51330(19) 0.07555(18) 0.0372(10) Uani 1 1 d . . . N2 N 0.22947(10) 0.43152(17) 0.13903(18) 0.0327(10) Uani 1 1 d . . . N3 N 0.11120(10) 0.5498(2) -0.05195(19) 0.0444(11) Uani 1 1 d . . . N4 N 0.13301(10) 0.58688(18) 0.06345(19) 0.0350(10) Uani 1 1 d . . . C1 C 0.27107(13) 0.4851(2) 0.1281(2) 0.0365(12) Uani 1 1 d . . . C2 C 0.26409(13) 0.4420(2) 0.1609(2) 0.0363(12) Uani 1 1 d . . . C3 C 0.29624(13) 0.4166(2) 0.2134(2) 0.0378(13) Uani 1 1 d . . . C4 C 0.30565(14) 0.3738(3) 0.2611(3) 0.0476(15) Uani 1 1 d . . . H4 H 0.2889 0.3530 0.2660 0.057 Uiso 1 1 calc R . . C5 C 0.34075(15) 0.3616(3) 0.3023(3) 0.0601(17) Uani 1 1 d . . . H5 H 0.3473 0.3311 0.3347 0.072 Uiso 1 1 calc R . . C6 C 0.36624(15) 0.3910(3) 0.2989(3) 0.0592(17) Uani 1 1 d . . . H6 H 0.3897 0.3816 0.3288 0.071 Uiso 1 1 calc R . . C7 C 0.35711(14) 0.4360(3) 0.2498(3) 0.0504(15) Uani 1 1 d . . . C8 C 0.37983(15) 0.4708(3) 0.2393(3) 0.0592(17) Uani 1 1 d . . . H8 H 0.4039 0.4645 0.2654 0.071 Uiso 1 1 calc R . . C9 C 0.36652(15) 0.5142(3) 0.1903(3) 0.0576(16) Uani 1 1 d . . . H9 H 0.3820 0.5382 0.1840 0.069 Uiso 1 1 calc R . . C10 C 0.33072(14) 0.5243(3) 0.1490(2) 0.0461(14) Uani 1 1 d . . . H10 H 0.3225 0.5540 0.1155 0.055 Uiso 1 1 calc R . . C11 C 0.30817(13) 0.4905(2) 0.1581(2) 0.0387(13) Uani 1 1 d . . . C12 C 0.32214(14) 0.4470(3) 0.2085(2) 0.0403(13) Uani 1 1 d . . . C13 C 0.24830(12) 0.5430(2) 0.0295(2) 0.0358(13) Uani 1 1 d . . . C14 C 0.25925(13) 0.5057(3) -0.0037(2) 0.0417(13) Uani 1 1 d . . . C15 C 0.26195(14) 0.5367(3) -0.0500(3) 0.0505(15) Uani 1 1 d . . . H15 H 0.2694 0.5129 -0.0727 0.061 Uiso 1 1 calc R . . C16 C 0.25414(14) 0.6004(3) -0.0635(3) 0.0548(16) Uani 1 1 d . . . H16 H 0.2557 0.6201 -0.0958 0.066 Uiso 1 1 calc R . . C17 C 0.24400(14) 0.6358(3) -0.0298(3) 0.0526(16) Uani 1 1 d . . . H17 H 0.2393 0.6802 -0.0385 0.063 Uiso 1 1 calc R . . C18 C 0.24058(13) 0.6080(3) 0.0162(2) 0.0424(14) Uani 1 1 d . . . C19 C 0.26655(15) 0.4344(3) 0.0067(3) 0.0543(16) Uani 1 1 d . . . H19 H 0.2669 0.4223 0.0453 0.065 Uiso 1 1 calc R . . C20 C 0.23793(17) 0.3960(3) -0.0478(3) 0.084(2) Uani 1 1 d . . . H20A H 0.2162 0.4038 -0.0505 0.126 Uiso 1 1 calc R . . H20B H 0.2435 0.3502 -0.0408 0.126 Uiso 1 1 calc R . . H20C H 0.2358 0.4092 -0.0869 0.126 Uiso 1 1 calc R . . C21 C 0.30116(15) 0.4154(3) 0.0168(3) 0.074(2) Uani 1 1 d . . . H21A H 0.3010 0.4239 -0.0215 0.112 Uiso 1 1 calc R . . H21B H 0.3052 0.3697 0.0269 0.112 Uiso 1 1 calc R . . H21C H 0.3194 0.4405 0.0514 0.112 Uiso 1 1 calc R . . C22 C 0.23131(14) 0.6501(3) 0.0545(3) 0.0499(15) Uani 1 1 d . . . H22 H 0.2245 0.6213 0.0777 0.060 Uiso 1 1 calc R . . C23 C 0.26340(15) 0.6870(3) 0.1028(3) 0.0665(18) Uani 1 1 d . . . H23A H 0.2808 0.6568 0.1325 0.100 Uiso 1 1 calc R . . H23B H 0.2574 0.7169 0.1255 0.100 Uiso 1 1 calc R . . H23C H 0.2725 0.7110 0.0815 0.100 Uiso 1 1 calc R . . C24 C 0.20120(15) 0.6952(3) 0.0140(3) 0.0697(19) Uani 1 1 d . . . H24A H 0.2072 0.7242 -0.0092 0.105 Uiso 1 1 calc R . . H24B H 0.1961 0.7204 0.0409 0.105 Uiso 1 1 calc R . . H24C H 0.1810 0.6700 -0.0155 0.105 Uiso 1 1 calc R . . C25 C 0.22188(12) 0.3743(2) 0.1605(2) 0.0355(13) Uani 1 1 d . . . C26 C 0.22739(12) 0.3147(2) 0.1416(2) 0.0392(13) Uani 1 1 d . . . C27 C 0.22247(13) 0.2591(3) 0.1671(3) 0.0487(15) Uani 1 1 d . . . H27 H 0.2259 0.2183 0.1546 0.058 Uiso 1 1 calc R . . C28 C 0.21265(13) 0.2626(3) 0.2099(3) 0.0480(15) Uani 1 1 d . . . H28 H 0.2104 0.2246 0.2282 0.058 Uiso 1 1 calc R . . C29 C 0.20621(13) 0.3213(3) 0.2260(2) 0.0461(15) Uani 1 1 d . . . H29 H 0.1985 0.3233 0.2541 0.055 Uiso 1 1 calc R . . C30 C 0.21061(13) 0.3784(2) 0.2020(2) 0.0379(13) Uani 1 1 d . . . C31 C 0.23730(14) 0.3076(3) 0.0936(3) 0.0481(15) Uani 1 1 d . . . H31 H 0.2389 0.3515 0.0796 0.058 Uiso 1 1 calc R . . C32 C 0.20960(14) 0.2699(3) 0.0353(3) 0.0632(18) Uani 1 1 d . . . H32A H 0.2075 0.2265 0.0478 0.095 Uiso 1 1 calc R . . H32B H 0.2163 0.2674 0.0045 0.095 Uiso 1 1 calc R . . H32C H 0.1875 0.2920 0.0167 0.095 Uiso 1 1 calc R . . C33 C 0.27219(15) 0.2751(3) 0.1208(3) 0.0686(19) Uani 1 1 d . . . H33A H 0.2893 0.2969 0.1595 0.103 Uiso 1 1 calc R . . H33B H 0.2792 0.2774 0.0904 0.103 Uiso 1 1 calc R . . H33C H 0.2705 0.2301 0.1299 0.103 Uiso 1 1 calc R . . C34 C 0.20503(14) 0.4427(3) 0.2231(3) 0.0491(15) Uani 1 1 d . . . H34 H 0.1978 0.4738 0.1880 0.059 Uiso 1 1 calc R . . C35 C 0.17723(17) 0.4413(3) 0.2377(3) 0.072(2) Uani 1 1 d . . . H35A H 0.1563 0.4226 0.2024 0.109 Uiso 1 1 calc R . . H35B H 0.1725 0.4851 0.2451 0.109 Uiso 1 1 calc R . . H35C H 0.1849 0.4153 0.2753 0.109 Uiso 1 1 calc R . . C36 C 0.23934(16) 0.4669(3) 0.2800(3) 0.0655(18) Uani 1 1 d . . . H36A H 0.2480 0.4356 0.3141 0.098 Uiso 1 1 calc R . . H36B H 0.2356 0.5081 0.2941 0.098 Uiso 1 1 calc R . . H36C H 0.2561 0.4723 0.2678 0.098 Uiso 1 1 calc R . . C37 C 0.10218(13) 0.6101(3) -0.0445(3) 0.0431(14) Uani 1 1 d . . . C38 C 0.11325(12) 0.6291(2) 0.0152(2) 0.0370(13) Uani 1 1 d . . . C39 C 0.10178(13) 0.6952(3) 0.0146(3) 0.0411(14) Uani 1 1 d . . . C40 C 0.10250(12) 0.7379(2) 0.0561(3) 0.0420(14) Uani 1 1 d . . . H40 H 0.1137 0.7271 0.0992 0.050 Uiso 1 1 calc R . . C41 C 0.08650(13) 0.7986(3) 0.0346(3) 0.0500(15) Uani 1 1 d . . . H41 H 0.0872 0.8278 0.0641 0.060 Uiso 1 1 calc R . . C42 C 0.07003(15) 0.8169(3) -0.0270(3) 0.0618(17) Uani 1 1 d . . . H42 H 0.0598 0.8581 -0.0398 0.074 Uiso 1 1 calc R . . C43 C 0.06867(14) 0.7733(3) -0.0710(3) 0.0550(16) Uani 1 1 d . . . C44 C 0.05176(16) 0.7835(3) -0.1370(3) 0.0704(19) Uani 1 1 d . . . H44 H 0.0411 0.8235 -0.1548 0.084 Uiso 1 1 calc R . . C45 C 0.05113(15) 0.7346(3) -0.1747(3) 0.0698(19) Uani 1 1 d . . . H45 H 0.0397 0.7421 -0.2184 0.084 Uiso 1 1 calc R . . C46 C 0.06655(14) 0.6738(3) -0.1515(3) 0.0563(16) Uani 1 1 d . . . H46 H 0.0653 0.6415 -0.1791 0.068 Uiso 1 1 calc R . . C47 C 0.08349(12) 0.6624(3) -0.0875(2) 0.0473(14) Uani 1 1 d . . . C48 C 0.08420(13) 0.7137(3) -0.0489(3) 0.0445(14) Uani 1 1 d . . . C49 C 0.09431(9) 0.52109(19) -0.11299(14) 0.0498(15) Uani 1 1 d G . . C50 C 0.06351(10) 0.4885(2) -0.13626(18) 0.075(2) Uani 1 1 d G . . C51 C 0.04716(9) 0.4610(2) -0.1955(2) 0.0909(18) Uani 1 1 d G . . H51 H 0.0261 0.4388 -0.2114 0.109 Uiso 1 1 calc R . . C52 C 0.06162(11) 0.4662(2) -0.23154(15) 0.098(3) Uani 1 1 d G . . H52 H 0.0504 0.4475 -0.2721 0.117 Uiso 1 1 calc R . . C53 C 0.09242(11) 0.4988(2) -0.20828(18) 0.0909(18) Uani 1 1 d G . . H53 H 0.1023 0.5023 -0.2329 0.109 Uiso 1 1 calc R . . C54 C 0.10877(8) 0.52626(19) -0.14900(18) 0.0542(16) Uani 1 1 d G . . C55 C 0.04620(18) 0.4827(5) -0.0995(3) 0.100(3) Uani 1 1 d . . . H55 H 0.0643 0.4901 -0.0545 0.120 Uiso 1 1 calc R . . C56 C 0.0194(2) 0.5356(4) -0.1186(4) 0.122(3) Uani 1 1 d . . . H56A H 0.0307 0.5776 -0.1093 0.183 Uiso 1 1 calc R . . H56B H 0.0082 0.5307 -0.0952 0.183 Uiso 1 1 calc R . . H56C H 0.0023 0.5325 -0.1636 0.183 Uiso 1 1 calc R . . C57 C 0.03044(19) 0.4180(4) -0.1033(4) 0.111(3) Uani 1 1 d . . . H57A H 0.0100 0.4120 -0.1454 0.167 Uiso 1 1 calc R . . H57B H 0.0239 0.4159 -0.0723 0.167 Uiso 1 1 calc R . . H57C H 0.0472 0.3843 -0.0948 0.167 Uiso 1 1 calc R . . C58 C 0.14312(16) 0.5576(3) -0.1244(3) 0.0636(18) Uani 1 1 d . . . H58 H 0.1519 0.5722 -0.0807 0.076 Uiso 1 1 calc R . . C59 C 0.16892(16) 0.5102(3) -0.1214(3) 0.084(2) Uani 1 1 d . . . H59A H 0.1710 0.4735 -0.0954 0.126 Uiso 1 1 calc R . . H59B H 0.1913 0.5312 -0.1032 0.126 Uiso 1 1 calc R . . H59C H 0.1612 0.4953 -0.1638 0.126 Uiso 1 1 calc R . . C60 C 0.14105(19) 0.6160(3) -0.1621(3) 0.092(2) Uani 1 1 d . . . H60A H 0.1339 0.6028 -0.2047 0.139 Uiso 1 1 calc R . . H60B H 0.1636 0.6365 -0.1421 0.139 Uiso 1 1 calc R . . H60C H 0.1243 0.6464 -0.1640 0.139 Uiso 1 1 calc R . . C61 C 0.13796(13) 0.5976(2) 0.1238(2) 0.0369(13) Uani 1 1 d . . . C62 C 0.11180(14) 0.5830(3) 0.1342(3) 0.0474(15) Uani 1 1 d . . . C63 C 0.11741(17) 0.5955(3) 0.1933(3) 0.0590(17) Uani 1 1 d . . . H63 H 0.0997 0.5867 0.2009 0.071 Uiso 1 1 calc R . . C64 C 0.14815(19) 0.6203(3) 0.2408(3) 0.0658(18) Uani 1 1 d . . . H64 H 0.1517 0.6275 0.2809 0.079 Uiso 1 1 calc R . . C65 C 0.17358(16) 0.6344(3) 0.2303(3) 0.0611(17) Uani 1 1 d . . . H65 H 0.1947 0.6514 0.2635 0.073 Uiso 1 1 calc R . . C66 C 0.16931(14) 0.6245(3) 0.1721(3) 0.0440(14) Uani 1 1 d . . . C67 C 0.07818(14) 0.5546(3) 0.0834(3) 0.0555(16) Uani 1 1 d . . . H67 H 0.0802 0.5449 0.0467 0.067 Uiso 1 1 calc R . . C68 C 0.04805(15) 0.6015(3) 0.0612(3) 0.072(2) Uani 1 1 d . . . H68A H 0.0443 0.6091 0.0954 0.108 Uiso 1 1 calc R . . H68B H 0.0272 0.5831 0.0253 0.108 Uiso 1 1 calc R . . H68C H 0.0534 0.6422 0.0489 0.108 Uiso 1 1 calc R . . C69 C 0.06960(16) 0.4912(3) 0.1039(3) 0.0691(18) Uani 1 1 d . . . H69A H 0.0885 0.4608 0.1175 0.104 Uiso 1 1 calc R . . H69B H 0.0484 0.4731 0.0686 0.104 Uiso 1 1 calc R . . H69C H 0.0664 0.4997 0.1387 0.104 Uiso 1 1 calc R . . C70 C 0.19649(13) 0.6469(2) 0.1606(2) 0.0427(14) Uani 1 1 d . . . H70 H 0.1887 0.6350 0.1166 0.051 Uiso 1 1 calc R . . C71 C 0.23145(13) 0.6146(3) 0.2037(3) 0.0541(16) Uani 1 1 d . . . H71A H 0.2393 0.6234 0.2475 0.081 Uiso 1 1 calc R . . H71B H 0.2482 0.6316 0.1947 0.081 Uiso 1 1 calc R . . H71C H 0.2292 0.5682 0.1965 0.081 Uiso 1 1 calc R . . C72 C 0.19975(14) 0.7199(2) 0.1655(3) 0.0575(17) Uani 1 1 d . . . H72A H 0.1780 0.7394 0.1334 0.086 Uiso 1 1 calc R . . H72B H 0.2180 0.7336 0.1591 0.086 Uiso 1 1 calc R . . H72C H 0.2054 0.7335 0.2070 0.086 Uiso 1 1 calc R . . C73 C 0.12558(14) 0.4270(2) 0.0463(3) 0.0509(15) Uani 1 1 d . B . H73A H 0.1385 0.4202 0.0922 0.061 Uiso 1 1 calc R . . H73B H 0.1009 0.4292 0.0314 0.061 Uiso 1 1 calc R . . C74 C 0.13149(17) 0.3693(3) 0.0156(3) 0.0663(19) Uani 1 1 d U . . H74A H 0.1554 0.3542 0.0434 0.080 Uiso 0.30 1 calc PR A 1 H74B H 0.1287 0.3833 -0.0243 0.080 Uiso 0.30 1 calc PR A 1 H74C H 0.1541 0.3739 0.0201 0.080 Uiso 0.70 1 calc PR A 2 H74D H 0.1137 0.3691 -0.0297 0.080 Uiso 0.70 1 calc PR A 2 C75A C 0.1058(8) 0.3101(10) 0.0015(12) 0.065(7) Uani 0.30 1 d PU B 1 H75A H 0.0818 0.3252 -0.0178 0.078 Uiso 0.30 1 calc PR B 1 H75B H 0.1068 0.2783 -0.0266 0.078 Uiso 0.30 1 calc PR B 1 C75B C 0.1304(3) 0.3027(4) 0.0452(6) 0.055(3) Uani 0.70 1 d PU B 2 H75C H 0.1411 0.2687 0.0338 0.066 Uiso 0.70 1 calc PR B 2 H75D H 0.1432 0.3060 0.0914 0.066 Uiso 0.70 1 calc PR B 2 C76A C 0.1186(8) 0.2836(12) 0.0624(13) 0.070(7) Uani 0.30 1 d PU B 1 H76A H 0.1198 0.3166 0.0917 0.084 Uiso 0.30 1 calc PR B 1 H76B H 0.1416 0.2645 0.0798 0.084 Uiso 0.30 1 calc PR B 1 C76B C 0.0931(3) 0.2870(5) 0.0193(5) 0.053(3) Uani 0.70 1 d PU B 2 H76C H 0.0819 0.3233 0.0266 0.064 Uiso 0.70 1 calc PR B 2 H76D H 0.0811 0.2796 -0.0264 0.064 Uiso 0.70 1 calc PR B 2 C77 C 0.06007(16) 0.3055(3) 0.1186(3) 0.0684(19) Uani 1 1 d . B . H77A H 0.0550 0.3321 0.0822 0.082 Uiso 1 1 calc R . . H77B H 0.0853 0.3025 0.1476 0.082 Uiso 1 1 calc R . . C78 C 0.04371(19) 0.3335(4) 0.1512(4) 0.099(2) Uani 1 1 d . . . H78A H 0.0569 0.3221 0.1962 0.119 Uiso 1 1 calc R B . H78B H 0.0422 0.3808 0.1470 0.119 Uiso 1 1 calc R . . C79 C 0.00863(19) 0.3039(4) 0.1180(4) 0.097(3) Uani 1 1 d . B . H79A H 0.0004 0.2995 0.1468 0.116 Uiso 1 1 calc R . . H79B H -0.0079 0.3306 0.0819 0.116 Uiso 1 1 calc R . . C80 C 0.01240(16) 0.2397(4) 0.0965(3) 0.081(2) Uani 1 1 d . B . H80A H 0.0132 0.2057 0.1245 0.097 Uiso 1 1 calc R . . H80B H -0.0071 0.2310 0.0534 0.097 Uiso 1 1 calc R . . C81 C 0.14069(15) 0.2065(3) 0.2109(3) 0.0674(18) Uani 1 1 d . B . H81A H 0.1418 0.2366 0.1817 0.081 Uiso 1 1 calc R . . H81B H 0.1581 0.1726 0.2227 0.081 Uiso 1 1 calc R . . C82 C 0.14671(17) 0.2409(3) 0.2671(3) 0.078(2) Uani 1 1 d . . . H82A H 0.1368 0.2845 0.2563 0.094 Uiso 1 1 calc R B . H82B H 0.1715 0.2440 0.2992 0.094 Uiso 1 1 calc R . . C83 C 0.12839(17) 0.1992(3) 0.2895(3) 0.0704(19) Uani 1 1 d . B . H83A H 0.1209 0.2249 0.3130 0.084 Uiso 1 1 calc R . . H83B H 0.1435 0.1641 0.3167 0.084 Uiso 1 1 calc R . . C84 C 0.09764(15) 0.1727(3) 0.2292(3) 0.0647(18) Uani 1 1 d . B . H84A H 0.0935 0.1273 0.2346 0.078 Uiso 1 1 calc R . . H84B H 0.0767 0.1978 0.2169 0.078 Uiso 1 1 calc R . . C85 C 0.14656(16) 0.1147(4) 0.0894(3) 0.080(2) Uani 1 1 d . B . H85A H 0.1359 0.0988 0.0460 0.096 Uiso 1 1 calc R . . H85B H 0.1514 0.1610 0.0899 0.096 Uiso 1 1 calc R . . C86 C 0.17808(16) 0.0802(3) 0.1306(3) 0.080(2) Uani 1 1 d . . . H86A H 0.1976 0.1105 0.1511 0.096 Uiso 1 1 calc R B . H86B H 0.1825 0.0488 0.1064 0.096 Uiso 1 1 calc R . . C87 C 0.17439(16) 0.0469(3) 0.1783(3) 0.076(2) Uani 1 1 d . B . H87A H 0.1888 0.0676 0.2197 0.092 Uiso 1 1 calc R . . H87B H 0.1813 0.0014 0.1818 0.092 Uiso 1 1 calc R . . C88 C 0.13671(15) 0.0521(3) 0.1557(3) 0.0601(17) Uani 1 1 d . B . H88A H 0.1245 0.0118 0.1352 0.072 Uiso 1 1 calc R . . H88B H 0.1339 0.0611 0.1911 0.072 Uiso 1 1 calc R . . C89 C 0.06512(17) 0.0258(3) -0.0145(3) 0.0714(19) Uani 1 1 d . B . H89A H 0.0470 0.0073 -0.0093 0.086 Uiso 1 1 calc R . . H89B H 0.0876 0.0076 0.0181 0.086 Uiso 1 1 calc R . . C90 C 0.05797(17) 0.0118(3) -0.0783(3) 0.077(2) Uani 1 1 d . . . H90A H 0.0330 0.0097 -0.1096 0.093 Uiso 1 1 calc R B . H90B H 0.0687 -0.0290 -0.0789 0.093 Uiso 1 1 calc R . . C91 C 0.07416(18) 0.0684(3) -0.0901(3) 0.078(2) Uani 1 1 d . B . H91A H 0.0994 0.0632 -0.0685 0.093 Uiso 1 1 calc R . . H91B H 0.0644 0.0744 -0.1355 0.093 Uiso 1 1 calc R . . C92 C 0.06506(17) 0.1232(3) -0.0633(3) 0.0708(19) Uani 1 1 d . B . H92A H 0.0821 0.1582 -0.0498 0.085 Uiso 1 1 calc R . . H92B H 0.0420 0.1403 -0.0945 0.085 Uiso 1 1 calc R . . C93 C -0.01149(15) 0.1360(3) -0.0557(3) 0.082(2) Uani 1 1 d DU B . H93A H -0.0250 0.1287 -0.0362 0.099 Uiso 1 1 calc R . . H93B H -0.0021 0.0946 -0.0588 0.099 Uiso 1 1 calc R . . C94 C -0.03329(17) 0.1661(4) -0.1190(3) 0.106(3) Uani 1 1 d DU . . H94A H -0.0259 0.1520 -0.1474 0.128 Uiso 1 1 calc R B . H94B H -0.0577 0.1546 -0.1379 0.128 Uiso 1 1 calc R . . C95 C -0.02818(18) 0.2367(4) -0.1075(3) 0.136(4) Uani 1 1 d DU B . H95A H -0.0456 0.2548 -0.1002 0.163 Uiso 1 1 calc R . . H95B H -0.0300 0.2588 -0.1439 0.163 Uiso 1 1 calc R . . C96 C 0.00716(16) 0.2446(3) -0.0505(3) 0.089(2) Uani 1 1 d DU B . H96A H 0.0236 0.2568 -0.0626 0.107 Uiso 1 1 calc R . . H96B H 0.0073 0.2782 -0.0227 0.107 Uiso 1 1 calc R . . C97 C 0.1352(2) 0.0762(5) 0.4485(4) 0.137(4) Uani 1 1 d . . . H97A H 0.1109 0.0788 0.4135 0.165 Uiso 1 1 calc R . . H97B H 0.1472 0.0462 0.4363 0.165 Uiso 1 1 calc R . . C98 C 0.1510(2) 0.1395(5) 0.4608(4) 0.116(3) Uani 1 1 d . . . H98A H 0.1345 0.1714 0.4308 0.140 Uiso 1 1 calc R . . H98B H 0.1714 0.1386 0.4574 0.140 Uiso 1 1 calc R . . C99 C 0.16092(17) 0.1551(3) 0.5259(4) 0.079(2) Uani 1 1 d . . . H99A H 0.1457 0.1885 0.5260 0.095 Uiso 1 1 calc R . . H99B H 0.1850 0.1703 0.5511 0.095 Uiso 1 1 calc R . . C100 C 0.1567(2) 0.0924(4) 0.5510(4) 0.089(2) Uani 1 1 d . . . H10A H 0.1795 0.0726 0.5791 0.107 Uiso 1 1 calc R . . H10B H 0.1460 0.1002 0.5755 0.107 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 Tm 0.04696(15) 0.04792(16) 0.05619(17) 0.00372(16) 0.02705(13) -0.00276(15) I 0.0656(3) 0.0721(3) 0.0748(3) 0.0056(3) 0.0355(3) -0.0211(2) Ga1 0.0450(4) 0.0363(3) 0.0379(4) 0.0030(3) 0.0259(3) 0.0029(3) Ga2 0.0439(3) 0.0379(4) 0.0385(4) -0.0024(3) 0.0248(3) 0.0001(3) O1 0.072(3) 0.039(2) 0.075(3) 0.002(2) 0.045(2) -0.007(2) O2 0.049(3) 0.066(3) 0.075(3) -0.003(2) 0.031(2) -0.003(2) O3 0.055(3) 0.058(3) 0.067(3) -0.001(2) 0.023(2) 0.000(2) O4 0.069(3) 0.045(3) 0.053(3) 0.000(2) 0.032(2) -0.002(2) O5 0.051(2) 0.061(3) 0.056(3) 0.014(2) 0.033(2) 0.004(2) O6 0.049(2) 0.067(3) 0.063(3) -0.008(2) 0.035(2) -0.009(2) O7 0.179(6) 0.116(5) 0.122(5) -0.042(4) 0.095(5) -0.056(4) N1 0.044(3) 0.036(3) 0.032(2) 0.005(2) 0.020(2) 0.003(2) N2 0.040(3) 0.027(2) 0.038(3) 0.004(2) 0.025(2) 0.0000(19) N3 0.045(3) 0.056(3) 0.030(3) -0.008(2) 0.019(2) 0.008(2) N4 0.040(3) 0.031(2) 0.036(3) -0.003(2) 0.021(2) -0.002(2) C1 0.044(3) 0.037(3) 0.034(3) -0.003(3) 0.025(3) -0.003(3) C2 0.041(3) 0.033(3) 0.034(3) -0.002(3) 0.020(3) -0.001(3) C3 0.044(3) 0.040(3) 0.028(3) -0.004(3) 0.018(3) -0.004(3) C4 0.048(4) 0.049(4) 0.046(4) 0.004(3) 0.024(3) 0.002(3) C5 0.059(4) 0.053(4) 0.057(4) 0.014(3) 0.024(4) 0.002(3) C6 0.049(4) 0.066(4) 0.049(4) 0.011(3) 0.017(3) 0.005(3) C7 0.049(4) 0.057(4) 0.046(4) 0.001(3) 0.026(3) 0.000(3) C8 0.044(4) 0.072(5) 0.055(4) 0.000(4) 0.022(3) -0.003(3) C9 0.059(4) 0.064(4) 0.061(4) -0.011(4) 0.039(4) -0.011(3) C10 0.051(4) 0.052(4) 0.039(3) 0.005(3) 0.027(3) 0.002(3) C11 0.047(3) 0.041(3) 0.037(3) -0.005(3) 0.028(3) -0.005(3) C12 0.047(4) 0.046(3) 0.031(3) -0.003(3) 0.023(3) 0.000(3) C13 0.044(3) 0.035(3) 0.031(3) 0.005(3) 0.021(3) 0.000(2) C14 0.052(3) 0.043(4) 0.040(3) 0.002(3) 0.031(3) -0.001(3) C15 0.059(4) 0.053(4) 0.055(4) -0.003(3) 0.041(3) 0.000(3) C16 0.064(4) 0.066(5) 0.047(4) 0.015(3) 0.038(3) 0.000(3) C17 0.068(4) 0.038(4) 0.060(4) 0.007(3) 0.039(4) 0.001(3) C18 0.052(4) 0.038(3) 0.038(3) 0.004(3) 0.025(3) 0.001(3) C19 0.083(5) 0.041(4) 0.052(4) -0.003(3) 0.045(4) 0.008(3) C20 0.105(6) 0.054(4) 0.101(6) -0.024(4) 0.060(5) -0.009(4) C21 0.075(5) 0.063(4) 0.084(5) -0.008(4) 0.042(4) 0.020(4) C22 0.064(4) 0.039(4) 0.055(4) 0.005(3) 0.038(3) 0.001(3) C23 0.084(5) 0.055(4) 0.072(5) -0.010(3) 0.049(4) -0.004(3) C24 0.073(4) 0.057(4) 0.082(5) 0.002(4) 0.043(4) 0.018(3) C25 0.040(3) 0.029(3) 0.035(3) 0.002(3) 0.019(3) -0.004(2) C26 0.043(3) 0.036(3) 0.042(3) 0.004(3) 0.025(3) 0.000(3) C27 0.044(3) 0.037(4) 0.056(4) -0.002(3) 0.020(3) 0.002(3) C28 0.039(3) 0.043(4) 0.055(4) 0.016(3) 0.020(3) 0.000(3) C29 0.045(3) 0.056(4) 0.039(3) 0.012(3) 0.024(3) 0.004(3) C30 0.044(3) 0.042(3) 0.027(3) 0.002(3) 0.018(3) -0.003(3) C31 0.065(4) 0.032(3) 0.057(4) -0.006(3) 0.040(3) 0.000(3) C32 0.064(4) 0.065(4) 0.061(4) -0.019(4) 0.034(4) 0.007(3) C33 0.069(4) 0.075(5) 0.077(5) -0.021(4) 0.049(4) -0.004(4) C34 0.069(4) 0.050(4) 0.044(4) 0.007(3) 0.040(3) 0.003(3) C35 0.110(5) 0.062(4) 0.097(5) 0.006(4) 0.089(5) 0.009(4) C36 0.086(5) 0.064(4) 0.040(4) -0.001(3) 0.029(4) -0.002(4) C37 0.042(3) 0.051(4) 0.042(4) 0.000(3) 0.026(3) 0.006(3) C38 0.041(3) 0.034(3) 0.039(3) 0.005(3) 0.023(3) 0.003(3) C39 0.038(3) 0.048(4) 0.037(4) 0.001(3) 0.020(3) 0.001(3) C40 0.042(3) 0.036(3) 0.049(4) 0.003(3) 0.025(3) 0.002(3) C41 0.045(3) 0.038(4) 0.064(4) -0.009(3) 0.028(3) -0.001(3) C42 0.057(4) 0.053(4) 0.077(5) 0.012(4) 0.037(4) 0.011(3) C43 0.051(4) 0.060(4) 0.055(4) 0.009(4) 0.029(3) 0.004(3) C44 0.074(5) 0.069(5) 0.067(5) 0.023(4) 0.036(4) 0.033(4) C45 0.072(5) 0.092(6) 0.046(4) 0.027(4) 0.032(4) 0.030(4) C46 0.061(4) 0.065(4) 0.040(4) 0.002(3) 0.025(3) 0.017(3) C47 0.043(3) 0.062(4) 0.041(3) 0.004(3) 0.025(3) 0.008(3) C48 0.045(3) 0.046(4) 0.045(4) 0.007(3) 0.026(3) 0.003(3) C49 0.047(4) 0.058(4) 0.044(4) -0.009(3) 0.024(3) 0.000(3) C50 0.050(4) 0.126(6) 0.051(4) -0.038(4) 0.028(3) -0.022(4) C51 0.057(3) 0.156(5) 0.060(3) -0.044(3) 0.031(3) -0.026(3) C52 0.069(5) 0.161(8) 0.053(4) -0.049(5) 0.026(4) -0.009(5) C53 0.057(3) 0.156(5) 0.060(3) -0.044(3) 0.031(3) -0.026(3) C54 0.053(4) 0.072(4) 0.035(3) -0.002(3) 0.021(3) 0.004(3) C55 0.051(4) 0.184(9) 0.068(5) -0.027(6) 0.033(4) -0.021(6) C56 0.098(6) 0.142(8) 0.176(9) -0.083(7) 0.107(7) -0.051(6) C57 0.078(6) 0.160(9) 0.111(7) 0.017(6) 0.061(5) 0.014(6) C58 0.075(5) 0.089(5) 0.038(4) -0.006(4) 0.038(4) -0.028(4) C59 0.066(5) 0.107(6) 0.070(5) 0.023(4) 0.030(4) -0.008(4) C60 0.121(6) 0.083(5) 0.110(6) 0.015(5) 0.086(5) 0.001(5) C61 0.046(3) 0.035(3) 0.036(3) 0.003(3) 0.026(3) 0.002(3) C62 0.050(4) 0.053(4) 0.047(4) 0.000(3) 0.031(3) 0.006(3) C63 0.079(5) 0.067(4) 0.055(4) -0.002(4) 0.052(4) 0.004(4) C64 0.093(5) 0.077(5) 0.041(4) -0.010(4) 0.044(4) 0.004(4) C65 0.068(4) 0.073(5) 0.044(4) -0.007(3) 0.031(4) 0.000(3) C66 0.048(4) 0.043(3) 0.046(4) -0.002(3) 0.028(3) 0.002(3) C67 0.051(4) 0.066(4) 0.064(4) 0.000(4) 0.040(4) 0.000(3) C68 0.055(4) 0.084(5) 0.090(5) 0.001(4) 0.047(4) -0.004(4) C69 0.076(4) 0.067(5) 0.082(5) -0.002(4) 0.053(4) -0.011(4) C70 0.045(3) 0.038(4) 0.039(3) -0.007(3) 0.018(3) -0.002(3) C71 0.059(4) 0.040(3) 0.053(4) 0.001(3) 0.023(3) -0.004(3) C72 0.054(4) 0.046(4) 0.063(4) 0.000(3) 0.025(3) 0.004(3) C73 0.053(4) 0.053(4) 0.058(4) -0.006(3) 0.037(3) -0.005(3) C74 0.090(5) 0.044(4) 0.105(5) -0.012(4) 0.078(4) -0.013(3) C75A 0.087(15) 0.029(11) 0.065(14) 0.003(10) 0.031(12) 0.008(11) C75B 0.054(7) 0.034(5) 0.080(8) 0.006(5) 0.038(6) -0.005(5) C76A 0.063(14) 0.055(13) 0.076(15) -0.006(12) 0.028(12) -0.011(12) C76B 0.052(6) 0.050(6) 0.062(7) -0.003(5) 0.034(6) -0.008(5) C77 0.072(4) 0.056(4) 0.084(5) -0.002(4) 0.046(4) -0.006(4) C78 0.102(6) 0.102(6) 0.121(6) -0.036(6) 0.079(5) -0.004(5) C79 0.078(6) 0.117(7) 0.109(7) -0.017(5) 0.060(5) -0.004(5) C80 0.057(4) 0.093(6) 0.095(6) -0.004(5) 0.043(4) 0.003(4) C81 0.061(4) 0.077(5) 0.066(5) -0.014(4) 0.035(4) -0.019(4) C82 0.085(5) 0.083(5) 0.067(5) -0.011(4) 0.042(4) -0.028(4) C83 0.097(5) 0.059(4) 0.056(4) -0.005(4) 0.041(4) -0.012(4) C84 0.068(4) 0.071(5) 0.064(4) 0.005(4) 0.041(4) -0.003(4) C85 0.060(4) 0.118(6) 0.074(5) 0.036(5) 0.044(4) 0.023(4) C86 0.065(5) 0.080(5) 0.098(6) 0.032(4) 0.046(4) 0.014(4) C87 0.065(5) 0.096(6) 0.068(5) 0.019(4) 0.035(4) 0.019(4) C88 0.064(4) 0.056(4) 0.058(4) 0.018(3) 0.031(4) 0.005(3) C89 0.085(5) 0.046(4) 0.078(5) -0.004(4) 0.040(4) -0.003(3) C90 0.075(5) 0.075(5) 0.071(5) -0.012(4) 0.032(4) 0.002(4) C91 0.099(5) 0.063(5) 0.074(5) -0.008(4) 0.048(4) -0.010(4) C92 0.087(5) 0.069(5) 0.054(4) 0.005(4) 0.036(4) 0.007(4) C93 0.049(4) 0.093(6) 0.086(6) -0.009(4) 0.023(4) -0.012(4) C94 0.060(5) 0.170(8) 0.075(5) 0.011(6) 0.027(4) -0.022(6) C95 0.132(8) 0.106(7) 0.076(6) 0.009(5) -0.007(6) 0.044(6) C96 0.082(5) 0.069(5) 0.087(6) 0.026(4) 0.026(5) 0.032(4) C97 0.174(9) 0.182(10) 0.130(8) -0.101(8) 0.131(8) -0.116(8) C98 0.125(7) 0.143(9) 0.115(7) 0.022(7) 0.086(6) 0.026(6) C99 0.088(5) 0.055(4) 0.123(7) -0.012(5) 0.074(5) -0.006(4) C100 0.093(6) 0.091(6) 0.094(6) -0.016(5) 0.057(5) -0.007(5) _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 Tm O1 1.964(4) . ? Tm O4 2.362(4) . ? Tm O5 2.366(3) . ? Tm O3 2.377(4) . ? Tm O2 2.379(4) . ? Tm O6 2.389(4) . ? Tm I 3.0259(5) . ? Ga1 N1 1.914(4) . ? Ga1 N2 1.923(4) . ? Ga1 Ga2 2.5287(8) . ? Ga2 N3 1.924(4) . ? Ga2 N4 1.930(4) . ? Ga2 C73 1.985(5) . ? O1 C76B 1.429(11) . ? O1 C76A 1.58(3) . ? O2 C77 1.451(6) . ? O2 C80 1.480(7) . ? O3 C96 1.458(7) . ? O3 C93 1.477(6) . ? O4 C92 1.458(7) . ? O4 C89 1.463(6) . ? O5 C88 1.452(6) . ? O5 C85 1.453(6) . ? O6 C81 1.452(6) . ? O6 C84 1.463(6) . ? O7 C100 1.344(8) . ? O7 C97 1.423(9) . ? N1 C1 1.387(6) . ? N1 C13 1.436(6) . ? N2 C2 1.399(6) . ? N2 C25 1.431(6) . ? N3 C37 1.370(6) . ? N3 C49 1.435(5) . ? N4 C38 1.380(6) . ? N4 C61 1.432(6) . ? C1 C2 1.371(6) . ? C1 C11 1.458(7) . ? C2 C3 1.461(7) . ? C3 C4 1.371(7) . ? C3 C12 1.414(7) . ? C4 C5 1.402(7) . ? C5 C6 1.368(7) . ? C6 C7 1.428(7) . ? C7 C12 1.393(7) . ? C7 C8 1.411(7) . ? C8 C9 1.385(8) . ? C9 C10 1.419(7) . ? C10 C11 1.372(7) . ? C11 C12 1.410(7) . ? C13 C18 1.397(7) . ? C13 C14 1.419(7) . ? C14 C15 1.400(7) . ? C14 C19 1.516(7) . ? C15 C16 1.372(7) . ? C16 C17 1.383(7) . ? C17 C18 1.382(7) . ? C18 C22 1.527(7) . ? C19 C21 1.527(7) . ? C19 C20 1.529(8) . ? C22 C24 1.529(7) . ? C22 C23 1.530(7) . ? C25 C30 1.399(7) . ? C25 C26 1.403(6) . ? C26 C27 1.403(7) . ? C26 C31 1.514(7) . ? C27 C28 1.381(7) . ? C28 C29 1.373(7) . ? C29 C30 1.399(7) . ? C30 C34 1.514(7) . ? C31 C33 1.529(7) . ? C31 C32 1.552(7) . ? C34 C35 1.513(7) . ? C34 C36 1.547(7) . ? C37 C38 1.368(7) . ? C37 C47 1.453(7) . ? C38 C39 1.474(7) . ? C39 C40 1.363(7) . ? C39 C48 1.411(7) . ? C40 C41 1.418(7) . ? C41 C42 1.372(7) . ? C42 C43 1.411(8) . ? C43 C48 1.393(7) . ? C43 C44 1.430(8) . ? C44 C45 1.386(8) . ? C45 C46 1.418(8) . ? C46 C47 1.389(7) . ? C47 C48 1.438(7) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 C55 1.519(7) . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C58 1.506(6) . ? C55 C57 1.511(10) . ? C55 C56 1.529(10) . ? C58 C59 1.517(8) . ? C58 C60 1.518(8) . ? C61 C62 1.400(7) . ? C61 C66 1.417(7) . ? C62 C63 1.397(7) . ? C62 C67 1.509(7) . ? C63 C64 1.377(8) . ? C64 C65 1.364(8) . ? C65 C66 1.391(7) . ? C66 C70 1.504(7) . ? C67 C68 1.540(7) . ? C67 C69 1.546(7) . ? C70 C72 1.529(7) . ? C70 C71 1.537(7) . ? C73 C74 1.534(7) . ? C74 C75B 1.589(11) . ? C74 C75A 1.61(3) . ? C75A C76A 1.43(4) . ? C75B C76B 1.513(13) . ? C77 C78 1.501(8) . ? C78 C79 1.500(9) . ? C79 C80 1.490(9) . ? C81 C82 1.478(8) . ? C82 C83 1.517(8) . ? C83 C84 1.525(7) . ? C85 C86 1.447(8) . ? C86 C87 1.476(8) . ? C87 C88 1.515(7) . ? C89 C90 1.491(8) . ? C90 C91 1.510(8) . ? C91 C92 1.499(8) . ? C93 C94 1.498(2) . ? C94 C95 1.496(2) . ? C95 C96 1.499(2) . ? C97 C98 1.460(10) . ? C98 C99 1.489(9) . ? C99 C100 1.510(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 O1 Tm O4 91.53(15) . . ? O1 Tm O5 87.68(14) . . ? O4 Tm O5 72.34(13) . . ? O1 Tm O3 89.99(15) . . ? O4 Tm O3 72.86(13) . . ? O5 Tm O3 145.04(13) . . ? O1 Tm O2 86.23(14) . . ? O4 Tm O2 145.18(13) . . ? O5 Tm O2 142.06(13) . . ? O3 Tm O2 72.40(13) . . ? O1 Tm O6 94.74(15) . . ? O4 Tm O6 142.67(12) . . ? O5 Tm O6 71.20(12) . . ? O3 Tm O6 143.71(13) . . ? O2 Tm O6 72.05(13) . . ? O1 Tm I 177.35(11) . . ? O4 Tm I 89.05(9) . . ? O5 Tm I 94.96(9) . . ? O3 Tm I 87.71(10) . . ? O2 Tm I 91.81(10) . . ? O6 Tm I 86.35(9) . . ? N1 Ga1 N2 87.25(16) . . ? N1 Ga1 Ga2 147.54(12) . . ? N2 Ga1 Ga2 122.00(12) . . ? N3 Ga2 N4 86.54(18) . . ? N3 Ga2 C73 119.6(2) . . ? N4 Ga2 C73 118.13(19) . . ? N3 Ga2 Ga1 119.27(12) . . ? N4 Ga2 Ga1 114.43(12) . . ? C73 Ga2 Ga1 100.07(16) . . ? C76B O1 Tm 159.8(5) . . ? C76A O1 Tm 155.4(11) . . ? C77 O2 C80 109.2(5) . . ? C77 O2 Tm 122.1(3) . . ? C80 O2 Tm 128.6(4) . . ? C96 O3 C93 109.8(4) . . ? C96 O3 Tm 123.1(3) . . ? C93 O3 Tm 126.7(3) . . ? C92 O4 C89 108.9(4) . . ? C92 O4 Tm 121.6(3) . . ? C89 O4 Tm 129.3(4) . . ? C88 O5 C85 108.1(4) . . ? C88 O5 Tm 127.7(3) . . ? C85 O5 Tm 124.0(3) . . ? C81 O6 C84 109.0(4) . . ? C81 O6 Tm 122.2(3) . . ? C84 O6 Tm 128.4(3) . . ? C100 O7 C97 108.6(6) . . ? C1 N1 C13 119.9(4) . . ? C1 N1 Ga1 109.1(3) . . ? C13 N1 Ga1 128.9(3) . . ? C2 N2 C25 116.1(4) . . ? C2 N2 Ga1 108.9(3) . . ? C25 N2 Ga1 132.2(3) . . ? C37 N3 C49 120.0(4) . . ? C37 N3 Ga2 109.6(3) . . ? C49 N3 Ga2 129.0(3) . . ? C38 N4 C61 119.7(4) . . ? C38 N4 Ga2 108.6(3) . . ? C61 N4 Ga2 129.8(3) . . ? C2 C1 N1 117.7(4) . . ? C2 C1 C11 109.1(4) . . ? N1 C1 C11 133.2(5) . . ? C1 C2 N2 116.8(4) . . ? C1 C2 C3 109.5(4) . . ? N2 C2 C3 133.7(5) . . ? C4 C3 C12 118.9(5) . . ? C4 C3 C2 136.5(5) . . ? C12 C3 C2 104.6(4) . . ? C3 C4 C5 117.9(5) . . ? C6 C5 C4 124.1(6) . . ? C5 C6 C7 119.0(5) . . ? C12 C7 C8 116.9(5) . . ? C12 C7 C6 116.3(5) . . ? C8 C7 C6 126.7(6) . . ? C9 C8 C7 119.1(5) . . ? C8 C9 C10 122.6(5) . . ? C11 C10 C9 119.2(5) . . ? C10 C11 C12 117.5(5) . . ? C10 C11 C1 137.4(5) . . ? C12 C11 C1 105.1(4) . . ? C7 C12 C11 124.7(5) . . ? C7 C12 C3 123.7(5) . . ? C11 C12 C3 111.6(5) . . ? C18 C13 C14 121.0(5) . . ? C18 C13 N1 118.9(5) . . ? C14 C13 N1 120.0(4) . . ? C15 C14 C13 117.4(5) . . ? C15 C14 C19 119.0(5) . . ? C13 C14 C19 123.5(5) . . ? C16 C15 C14 121.7(5) . . ? C15 C16 C17 119.7(5) . . ? C18 C17 C16 121.5(5) . . ? C17 C18 C13 118.8(5) . . ? C17 C18 C22 119.2(5) . . ? C13 C18 C22 121.9(5) . . ? C14 C19 C21 113.6(5) . . ? C14 C19 C20 110.8(5) . . ? C21 C19 C20 109.6(5) . . ? C18 C22 C24 113.1(5) . . ? C18 C22 C23 108.5(4) . . ? C24 C22 C23 111.6(5) . . ? C30 C25 C26 121.2(5) . . ? C30 C25 N2 119.8(5) . . ? C26 C25 N2 118.9(4) . . ? C25 C26 C27 118.2(5) . . ? C25 C26 C31 123.2(5) . . ? C27 C26 C31 118.5(5) . . ? C28 C27 C26 121.1(5) . . ? C29 C28 C27 119.5(5) . . ? C28 C29 C30 121.9(5) . . ? C25 C30 C29 117.9(5) . . ? C25 C30 C34 121.3(5) . . ? C29 C30 C34 120.7(5) . . ? C26 C31 C33 112.3(5) . . ? C26 C31 C32 111.3(5) . . ? C33 C31 C32 109.6(4) . . ? C35 C34 C30 113.2(5) . . ? C35 C34 C36 111.0(5) . . ? C30 C34 C36 109.5(5) . . ? C38 C37 N3 117.1(5) . . ? C38 C37 C47 109.2(5) . . ? N3 C37 C47 133.6(5) . . ? C37 C38 N4 118.0(5) . . ? C37 C38 C39 109.9(5) . . ? N4 C38 C39 132.1(5) . . ? C40 C39 C48 117.3(5) . . ? C40 C39 C38 138.0(5) . . ? C48 C39 C38 104.7(5) . . ? C39 C40 C41 119.7(5) . . ? C42 C41 C40 122.8(6) . . ? C41 C42 C43 118.6(6) . . ? C48 C43 C42 117.5(6) . . ? C48 C43 C44 116.3(6) . . ? C42 C43 C44 126.1(6) . . ? C45 C44 C43 119.3(6) . . ? C44 C45 C46 123.6(6) . . ? C47 C46 C45 118.7(6) . . ? C46 C47 C48 117.1(5) . . ? C46 C47 C37 137.6(6) . . ? C48 C47 C37 105.3(5) . . ? C43 C48 C39 124.1(6) . . ? C43 C48 C47 124.9(5) . . ? C39 C48 C47 110.9(5) . . ? C50 C49 C54 120.0 . . ? C50 C49 N3 120.2(3) . . ? C54 C49 N3 119.8(3) . . ? C49 C50 C51 120.0 . . ? C49 C50 C55 122.1(4) . . ? C51 C50 C55 117.8(4) . . ? C52 C51 C50 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 C58 117.9(3) . . ? C49 C54 C58 122.0(3) . . ? C57 C55 C50 115.0(7) . . ? C57 C55 C56 110.2(6) . . ? C50 C55 C56 110.4(7) . . ? C54 C58 C59 111.2(5) . . ? C54 C58 C60 113.0(5) . . ? C59 C58 C60 109.8(5) . . ? C62 C61 C66 120.5(5) . . ? C62 C61 N4 120.3(5) . . ? C66 C61 N4 119.2(5) . . ? C63 C62 C61 118.4(5) . . ? C63 C62 C67 120.2(5) . . ? C61 C62 C67 121.4(5) . . ? C64 C63 C62 121.1(6) . . ? C65 C64 C63 120.3(6) . . ? C64 C65 C66 121.4(6) . . ? C65 C66 C61 118.3(5) . . ? C65 C66 C70 119.8(5) . . ? C61 C66 C70 121.8(5) . . ? C62 C67 C68 112.1(5) . . ? C62 C67 C69 112.4(5) . . ? C68 C67 C69 108.8(5) . . ? C66 C70 C72 110.5(4) . . ? C66 C70 C71 113.1(4) . . ? C72 C70 C71 111.0(4) . . ? C74 C73 Ga2 113.8(4) . . ? C73 C74 C75B 112.9(6) . . ? C73 C74 C75A 113.8(10) . . ? C76A C75A C74 103(2) . . ? C76B C75B C74 107.5(9) . . ? C75A C76A O1 103(2) . . ? O1 C76B C75B 109.4(10) . . ? O2 C77 C78 105.2(5) . . ? C79 C78 C77 103.9(6) . . ? C80 C79 C78 105.8(6) . . ? O2 C80 C79 105.8(5) . . ? O6 C81 C82 105.9(5) . . ? C81 C82 C83 103.0(5) . . ? C82 C83 C84 103.9(5) . . ? O6 C84 C83 105.4(5) . . ? C86 C85 O5 108.3(5) . . ? C85 C86 C87 108.1(5) . . ? C86 C87 C88 105.5(5) . . ? O5 C88 C87 105.7(5) . . ? O4 C89 C90 105.6(5) . . ? C89 C90 C91 102.4(5) . . ? C92 C91 C90 102.6(6) . . ? O4 C92 C91 104.5(5) . . ? O3 C93 C94 104.9(5) . . ? C95 C94 C93 105.0(6) . . ? C94 C95 C96 105.7(6) . . ? O3 C96 C95 106.1(5) . . ? O7 C97 C98 110.0(7) . . ? C97 C98 C99 104.9(7) . . ? C98 C99 C100 104.0(6) . . ? O7 C100 C99 109.5(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.912 _refine_diff_density_min -2.530 _refine_diff_density_rms 0.095 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.174 0.250 656 119 ' ' 2 0.000 0.173 0.750 656 119 ' ' 3 0.500 0.115 0.750 18 1 ' ' 4 0.500 0.326 0.250 656 119 ' ' 5 0.500 0.673 0.750 656 119 ' ' 6 0.000 0.385 0.250 18 1 ' ' 7 0.000 0.615 0.750 18 1 ' ' 8 0.500 0.885 0.250 18 1 ' ' _platon_squeeze_details ; ; #============================================================================== data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H152 Dy Ga2 I N4 O9' _chemical_formula_weight 2079.18 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' 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 45.875(7) _cell_length_b 20.805(3) _cell_length_c 25.246(4) _cell_angle_alpha 90.00 _cell_angle_beta 122.187(2) _cell_angle_gamma 90.00 _cell_volume 20392(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8648 _exptl_absorpt_coefficient_mu 1.610 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7084 _exptl_absorpt_correction_T_max 0.8428 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 85256 _diffrn_reflns_av_R_equivalents 0.2862 _diffrn_reflns_av_sigmaI/netI 0.2646 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 19935 _reflns_number_gt 8757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^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 19935 _refine_ls_number_parameters 1097 _refine_ls_number_restraints 107 _refine_ls_R_factor_all 0.2018 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.867 _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 Dy1 Dy -0.070834(7) -0.160522(15) -0.073843(14) 0.02701(8) Uani 1 1 d . . . Ga1 Ga -0.140160(15) -0.51040(3) -0.02851(3) 0.02258(18) Uani 1 1 d . . . Ga2 Ga -0.202455(15) -0.48595(3) -0.06741(3) 0.02412(18) Uani 1 1 d . . . I1 I -0.036534(11) -0.05418(2) -0.10503(2) 0.03913(13) Uani 1 1 d . . . N1 N -0.13317(10) -0.5880(2) -0.06273(19) 0.0203(13) Uani 1 1 d . . . N2 N -0.11149(10) -0.5476(2) 0.0522(2) 0.0240(13) Uani 1 1 d . . . N3 N -0.23003(10) -0.4320(2) -0.13941(19) 0.0212(13) Uani 1 1 d . . . N4 N -0.24468(11) -0.5132(2) -0.0762(2) 0.0256(14) Uani 1 1 d . . . O1 O -0.08989(10) -0.2333(2) -0.04933(19) 0.0424(13) Uani 1 1 d U . . O2 O -0.12472(9) -0.1058(2) -0.11326(17) 0.0321(12) Uani 1 1 d . . . O3 O -0.06582(9) -0.09706(19) 0.00978(17) 0.0325(12) Uani 1 1 d . . . O4 O -0.01455(9) -0.18139(19) 0.01694(18) 0.0354(13) Uani 1 1 d . . . O5 O -0.04432(9) -0.2446(2) -0.10112(19) 0.0363(13) Uani 1 1 d . . . O6 O -0.10706(9) -0.1778(2) -0.18679(17) 0.0352(13) Uani 1 1 d . . . C1 C -0.11328(13) -0.6299(3) -0.0138(3) 0.0234(17) Uani 1 1 d . . . C2 C -0.10240(12) -0.6092(3) 0.0460(2) 0.0225(16) Uani 1 1 d . . . C3 C -0.08306(13) -0.6618(3) 0.0908(3) 0.0292(17) Uani 1 1 d . . . C4 C -0.08408(13) -0.7140(3) 0.0520(3) 0.0222(16) Uani 1 1 d . . . C5 C -0.10172(14) -0.6957(3) -0.0127(3) 0.0274(18) Uani 1 1 d . . . C6 C -0.10233(13) -0.7390(3) -0.0537(3) 0.0251(17) Uani 1 1 d . . . H6A H -0.1133 -0.7288 -0.0969 0.030 Uiso 1 1 calc R . . C7 C -0.08601(13) -0.8005(3) -0.0304(3) 0.0254(17) Uani 1 1 d . . . H7A H -0.0867 -0.8306 -0.0594 0.031 Uiso 1 1 calc R . . C8 C -0.06981(14) -0.8175(3) 0.0302(3) 0.0329(19) Uani 1 1 d . . . H8A H -0.0594 -0.8586 0.0433 0.039 Uiso 1 1 calc R . . C9 C -0.06841(14) -0.7733(3) 0.0747(3) 0.0340(18) Uani 1 1 d . . . C10 C -0.05127(15) -0.7829(3) 0.1413(3) 0.038(2) Uani 1 1 d . . . H10C H -0.0403 -0.8226 0.1596 0.046 Uiso 1 1 calc R . . C11 C -0.05104(15) -0.7345(4) 0.1776(3) 0.045(2) Uani 1 1 d . . . H11C H -0.0401 -0.7419 0.2213 0.055 Uiso 1 1 calc R . . C12 C -0.06672(14) -0.6717(3) 0.1532(3) 0.0345(19) Uani 1 1 d . . . H12C H -0.0655 -0.6388 0.1804 0.041 Uiso 1 1 calc R . . C13 C -0.13773(13) -0.5996(3) -0.1225(3) 0.0229(16) Uani 1 1 d . . . C14 C -0.11180(13) -0.5856(3) -0.1334(3) 0.0261(17) Uani 1 1 d . . . C15 C -0.11728(16) -0.5986(3) -0.1930(3) 0.0376(18) Uani 1 1 d . . . H15A H -0.0996 -0.5900 -0.2010 0.045 Uiso 1 1 calc R . . C16 C -0.14815(16) -0.6236(3) -0.2394(3) 0.045(2) Uani 1 1 d . . . H16A H -0.1518 -0.6310 -0.2796 0.053 Uiso 1 1 calc R . . C17 C -0.17402(16) -0.6382(3) -0.2293(3) 0.042(2) Uani 1 1 d . . . H17A H -0.1950 -0.6562 -0.2621 0.051 Uiso 1 1 calc R . . C18 C -0.16960(14) -0.6265(3) -0.1705(3) 0.0259(17) Uani 1 1 d . . . C19 C -0.07803(14) -0.5557(3) -0.0829(3) 0.0322(17) Uani 1 1 d . . . H19A H -0.0800 -0.5451 -0.0463 0.039 Uiso 1 1 calc R . . C20 C -0.06998(15) -0.4935(3) -0.1053(3) 0.045(2) Uani 1 1 d . . . H20A H -0.0898 -0.4644 -0.1222 0.067 Uiso 1 1 calc R . . H20B H -0.0653 -0.5036 -0.1380 0.067 Uiso 1 1 calc R . . H20C H -0.0497 -0.4728 -0.0700 0.067 Uiso 1 1 calc R . . C21 C -0.04740(15) -0.6032(3) -0.0603(3) 0.047(2) Uani 1 1 d . . . H21A H -0.0518 -0.6424 -0.0441 0.071 Uiso 1 1 calc R . . H21B H -0.0261 -0.5829 -0.0271 0.071 Uiso 1 1 calc R . . H21C H -0.0450 -0.6141 -0.0955 0.071 Uiso 1 1 calc R . . C22 C -0.19702(13) -0.6473(3) -0.1586(3) 0.0254(17) Uani 1 1 d . . . H22A H -0.1890 -0.6350 -0.1146 0.030 Uiso 1 1 calc R . . C23 C -0.23197(14) -0.6152(3) -0.2014(3) 0.0310(19) Uani 1 1 d . . . H23A H -0.2297 -0.5686 -0.1945 0.046 Uiso 1 1 calc R . . H23B H -0.2486 -0.6320 -0.1918 0.046 Uiso 1 1 calc R . . H23C H -0.2400 -0.6244 -0.2451 0.046 Uiso 1 1 calc R . . C24 C -0.20032(14) -0.7218(3) -0.1630(3) 0.0327(19) Uani 1 1 d . . . H24A H -0.1785 -0.7412 -0.1305 0.049 Uiso 1 1 calc R . . H24B H -0.2057 -0.7359 -0.2043 0.049 Uiso 1 1 calc R . . H24C H -0.2188 -0.7353 -0.1569 0.049 Uiso 1 1 calc R . . C25 C -0.09438(13) -0.5190(3) 0.1133(3) 0.0302(18) Uani 1 1 d . . . C26 C -0.06345(15) -0.4857(4) 0.1352(3) 0.045(2) Uani 1 1 d . . . C27 C -0.04873(17) -0.4565(4) 0.1938(3) 0.068(3) Uani 1 1 d . . . H27A H -0.0280 -0.4329 0.2092 0.082 Uiso 1 1 calc R . . C28 C -0.06259(17) -0.4601(4) 0.2301(3) 0.062(3) Uani 1 1 d . . . H28A H -0.0513 -0.4406 0.2703 0.075 Uiso 1 1 calc R . . C29 C -0.09248(16) -0.4917(3) 0.2078(3) 0.046(2) Uani 1 1 d . . . H29A H -0.1024 -0.4935 0.2326 0.055 Uiso 1 1 calc R . . C30 C -0.10964(15) -0.5223(3) 0.1487(3) 0.0342(19) Uani 1 1 d . . . C31 C -0.04636(16) -0.4817(4) 0.0993(3) 0.065(3) Uani 1 1 d . . . H31A H -0.0645 -0.4910 0.0546 0.078 Uiso 1 1 calc R . . C32 C -0.01895(17) -0.5342(4) 0.1199(4) 0.087(3) Uani 1 1 d . . . H32A H -0.0100 -0.5340 0.0922 0.131 Uiso 1 1 calc R . . H32B H -0.0292 -0.5762 0.1177 0.131 Uiso 1 1 calc R . . H32C H 0.0000 -0.5260 0.1630 0.131 Uiso 1 1 calc R . . C33 C -0.03142(16) -0.4190(3) 0.0998(3) 0.074(3) Uani 1 1 d . . . H33A H -0.0486 -0.3852 0.0888 0.112 Uiso 1 1 calc R . . H33B H -0.0244 -0.4193 0.0692 0.112 Uiso 1 1 calc R . . H33C H -0.0113 -0.4107 0.1416 0.112 Uiso 1 1 calc RD . . C34 C -0.14423(14) -0.5534(3) 0.1243(3) 0.0367(19) Uani 1 1 d . . . H34A H -0.1528 -0.5687 0.0808 0.044 Uiso 1 1 calc R . . C35 C -0.14018(16) -0.6127(3) 0.1642(3) 0.052(2) Uani 1 1 d . . . H35A H -0.1239 -0.6428 0.1638 0.078 Uiso 1 1 calc R . . H35B H -0.1626 -0.6338 0.1467 0.078 Uiso 1 1 calc R . . H35C H -0.1315 -0.5993 0.2073 0.078 Uiso 1 1 calc R . . C36 C -0.16976(15) -0.5076(4) 0.1206(3) 0.055(3) Uani 1 1 d . . . H36A H -0.1727 -0.4720 0.0926 0.082 Uiso 1 1 calc R . . H36B H -0.1617 -0.4907 0.1624 0.082 Uiso 1 1 calc R . . H36C H -0.1919 -0.5295 0.1042 0.082 Uiso 1 1 calc R . . C37 C -0.26395(14) -0.4417(3) -0.1610(3) 0.0268(17) Uani 1 1 d . . . C38 C -0.27211(14) -0.4843(3) -0.1281(3) 0.0254(16) Uani 1 1 d . . . C39 C -0.30962(13) -0.4900(3) -0.1583(2) 0.0216(15) Uani 1 1 d . . . C40 C -0.32324(13) -0.4460(3) -0.2107(3) 0.0243(16) Uani 1 1 d . . . C41 C -0.29668(14) -0.4162(3) -0.2134(3) 0.0250(17) Uani 1 1 d . . . C42 C -0.30555(14) -0.3735(3) -0.2611(3) 0.0295(18) Uani 1 1 d . . . H42A H -0.2886 -0.3531 -0.2659 0.035 Uiso 1 1 calc R . . C43 C -0.34092(15) -0.3614(3) -0.3026(3) 0.039(2) Uani 1 1 d . . . H43A H -0.3472 -0.3310 -0.3351 0.047 Uiso 1 1 calc R . . C44 C -0.36654(15) -0.3895(3) -0.2999(3) 0.039(2) Uani 1 1 d . . . H44A H -0.3899 -0.3795 -0.3300 0.047 Uiso 1 1 calc R . . C45 C -0.35797(14) -0.4354(3) -0.2502(3) 0.0304(18) Uani 1 1 d . . . C46 C -0.38073(16) -0.4701(3) -0.2401(3) 0.041(2) Uani 1 1 d . . . H46A H -0.4049 -0.4641 -0.2672 0.049 Uiso 1 1 calc R . . C47 C -0.36840(14) -0.5129(3) -0.1913(3) 0.0340(18) Uani 1 1 d . . . H47A H -0.3842 -0.5359 -0.1849 0.041 Uiso 1 1 calc R . . C48 C -0.33269(14) -0.5234(3) -0.1505(3) 0.0330(18) Uani 1 1 d . . . H48A H -0.3247 -0.5538 -0.1176 0.040 Uiso 1 1 calc R . . C49 C -0.22201(14) -0.3747(3) -0.1606(3) 0.0269(17) Uani 1 1 d . . . C50 C -0.22755(14) -0.3147(3) -0.1428(3) 0.0289(18) Uani 1 1 d . . . C51 C -0.22253(14) -0.2596(3) -0.1685(3) 0.0339(19) Uani 1 1 d . . . H51A H -0.2260 -0.2183 -0.1567 0.041 Uiso 1 1 calc R . . C52 C -0.21264(14) -0.2649(3) -0.2108(3) 0.035(2) Uani 1 1 d . . . H52A H -0.2103 -0.2269 -0.2291 0.042 Uiso 1 1 calc R . . C53 C -0.20597(14) -0.3233(3) -0.2277(3) 0.0297(18) Uani 1 1 d . . . H53A H -0.1984 -0.3257 -0.2560 0.036 Uiso 1 1 calc R . . C54 C -0.21066(13) -0.3785(3) -0.2023(3) 0.0223(16) Uani 1 1 d . . . C55 C -0.23742(14) -0.3073(3) -0.0931(3) 0.0329(18) Uani 1 1 d . . . H55A H -0.2392 -0.3514 -0.0791 0.039 Uiso 1 1 calc R . . C56 C -0.27298(15) -0.2746(4) -0.1220(3) 0.053(2) Uani 1 1 d . . . H56A H -0.2787 -0.2701 -0.0899 0.080 Uiso 1 1 calc R . . H56B H -0.2905 -0.3008 -0.1565 0.080 Uiso 1 1 calc R . . H56C H -0.2722 -0.2319 -0.1377 0.080 Uiso 1 1 calc R . . C57 C -0.21104(14) -0.2699(3) -0.0360(3) 0.0376(19) Uani 1 1 d . . . H57A H -0.1893 -0.2937 -0.0143 0.056 Uiso 1 1 calc R . . H57B H -0.2194 -0.2641 -0.0078 0.056 Uiso 1 1 calc R . . H57C H -0.2074 -0.2278 -0.0489 0.056 Uiso 1 1 calc R . . C58 C -0.20484(14) -0.4442(3) -0.2232(3) 0.0285(17) Uani 1 1 d . . . H58A H -0.1975 -0.4747 -0.1876 0.034 Uiso 1 1 calc R . . C59 C -0.17687(15) -0.4447(3) -0.2380(3) 0.044(2) Uani 1 1 d . . . H59A H -0.1566 -0.4219 -0.2050 0.066 Uiso 1 1 calc R . . H59B H -0.1853 -0.4232 -0.2782 0.066 Uiso 1 1 calc R . . H59C H -0.1707 -0.4892 -0.2404 0.066 Uiso 1 1 calc R . . C60 C -0.23882(17) -0.4697(3) -0.2784(3) 0.046(2) Uani 1 1 d . . . H60A H -0.2351 -0.5124 -0.2902 0.069 Uiso 1 1 calc R . . H60B H -0.2473 -0.4404 -0.3141 0.069 Uiso 1 1 calc R . . H60C H -0.2559 -0.4727 -0.2664 0.069 Uiso 1 1 calc R . . C61 C -0.24921(13) -0.5418(3) -0.0279(2) 0.0225(16) Uani 1 1 d . . . C62 C -0.26073(13) -0.5050(3) 0.0032(2) 0.0219(16) Uani 1 1 d . . . C63 C -0.26312(14) -0.5343(3) 0.0496(3) 0.0352(19) Uani 1 1 d . . . H63A H -0.2709 -0.5098 0.0716 0.042 Uiso 1 1 calc R . . C64 C -0.25465(15) -0.5977(3) 0.0651(3) 0.0363(19) Uani 1 1 d . . . H64A H -0.2562 -0.6170 0.0977 0.044 Uiso 1 1 calc R . . C65 C -0.24396(15) -0.6327(3) 0.0325(3) 0.040(2) Uani 1 1 d . . . H65A H -0.2385 -0.6768 0.0426 0.048 Uiso 1 1 calc R . . C66 C -0.24077(14) -0.6069(3) -0.0143(3) 0.0249(17) Uani 1 1 d . . . C67 C -0.26861(15) -0.4324(3) -0.0085(3) 0.0343(18) Uani 1 1 d . . . H67A H -0.2697 -0.4212 -0.0480 0.041 Uiso 1 1 calc R . . C68 C -0.30341(15) -0.4156(3) -0.0179(3) 0.045(2) Uani 1 1 d . . . H68A H -0.3082 -0.3698 -0.0282 0.067 Uiso 1 1 calc R . . H68B H -0.3030 -0.4247 0.0206 0.067 Uiso 1 1 calc R . . H68C H -0.3215 -0.4414 -0.0523 0.067 Uiso 1 1 calc R . . C69 C -0.23981(16) -0.3929(3) 0.0439(3) 0.049(2) Uani 1 1 d . . . H69A H -0.2449 -0.3470 0.0347 0.073 Uiso 1 1 calc R . . H69B H -0.2180 -0.4030 0.0473 0.073 Uiso 1 1 calc R . . H69C H -0.2379 -0.4031 0.0835 0.073 Uiso 1 1 calc R . . C70 C -0.23172(14) -0.6495(3) -0.0511(3) 0.0329(18) Uani 1 1 d . . . H70A H -0.2247 -0.6206 -0.0741 0.039 Uiso 1 1 calc R . . C71 C -0.26366(16) -0.6861(3) -0.1009(3) 0.044(2) Uani 1 1 d . . . H71A H -0.2809 -0.6556 -0.1306 0.066 Uiso 1 1 calc R . . H71B H -0.2734 -0.7107 -0.0807 0.066 Uiso 1 1 calc R . . H71C H -0.2572 -0.7157 -0.1232 0.066 Uiso 1 1 calc R . . C72 C -0.20133(15) -0.6945(3) -0.0113(3) 0.040(2) Uani 1 1 d . . . H72A H -0.1821 -0.6699 0.0223 0.061 Uiso 1 1 calc R . . H72B H -0.1941 -0.7143 -0.0377 0.061 Uiso 1 1 calc R . . H72C H -0.2083 -0.7281 0.0069 0.061 Uiso 1 1 calc R . . C73 C -0.12601(14) -0.4271(3) -0.0470(3) 0.0309(18) Uani 1 1 d . . . H73A H -0.1010 -0.4285 -0.0304 0.037 Uiso 1 1 calc R . . H73B H -0.1382 -0.4215 -0.0929 0.037 Uiso 1 1 calc R . . C74 C -0.13356(16) -0.3693(3) -0.0189(3) 0.044(2) Uani 1 1 d . . . H74A H -0.1178 -0.3700 0.0272 0.053 Uiso 1 1 calc R . . H74B H -0.1574 -0.3725 -0.0284 0.053 Uiso 1 1 calc R . . C75 C -0.12912(16) -0.3036(3) -0.0454(3) 0.051(2) Uani 1 1 d . . . H75A H -0.1412 -0.3064 -0.0915 0.062 Uiso 1 1 calc R . . H75B H -0.1399 -0.2686 -0.0350 0.062 Uiso 1 1 calc R . . C76 C -0.09464(16) -0.2888(3) -0.0209(3) 0.053(2) Uani 1 1 d U . . H76A H -0.0833 -0.3262 -0.0267 0.064 Uiso 1 1 calc R . . H76B H -0.0832 -0.2812 0.0247 0.064 Uiso 1 1 calc R . . C77 C -0.13841(14) -0.0511(3) -0.1577(3) 0.0380(19) Uani 1 1 d . . . H77A H -0.1262 -0.0109 -0.1367 0.046 Uiso 1 1 calc R . . H77B H -0.1357 -0.0592 -0.1935 0.046 Uiso 1 1 calc R . . C78 C -0.17506(15) -0.0466(4) -0.1790(3) 0.050(2) Uani 1 1 d . . . H78A H -0.1895 -0.0670 -0.2206 0.060 Uiso 1 1 calc R . . H78B H -0.1820 -0.0011 -0.1823 0.060 Uiso 1 1 calc R . . C79 C -0.17937(15) -0.0810(4) -0.1314(3) 0.051(2) Uani 1 1 d . . . H79A H -0.1841 -0.0498 -0.1072 0.062 Uiso 1 1 calc R . . H79B H -0.1989 -0.1116 -0.1522 0.062 Uiso 1 1 calc R . . C80 C -0.14720(15) -0.1154(4) -0.0899(3) 0.056(2) Uani 1 1 d . . . H80A H -0.1362 -0.0986 -0.0467 0.068 Uiso 1 1 calc R . . H80B H -0.1518 -0.1618 -0.0894 0.068 Uiso 1 1 calc R . . C81 C -0.06564(16) -0.0275(3) 0.0164(3) 0.041(2) Uani 1 1 d . . . H81A H -0.0887 -0.0094 -0.0137 0.049 Uiso 1 1 calc R . . H81B H -0.0486 -0.0076 0.0088 0.049 Uiso 1 1 calc R . . C82 C -0.05613(17) -0.0158(3) 0.0819(3) 0.049(2) Uani 1 1 d . . . H82A H -0.0658 0.0253 0.0855 0.059 Uiso 1 1 calc R . . H82B H -0.0308 -0.0154 0.1112 0.059 Uiso 1 1 calc R . . C83 C -0.07220(16) -0.0719(3) 0.0938(3) 0.048(2) Uani 1 1 d . . . H83A H -0.0971 -0.0650 0.0755 0.057 Uiso 1 1 calc R . . H83B H -0.0609 -0.0806 0.1391 0.057 Uiso 1 1 calc R . . C84 C -0.06594(15) -0.1252(2) 0.0613(2) 0.042(2) Uani 1 1 d . . . H84A H -0.0435 -0.1461 0.0903 0.050 Uiso 1 1 calc RD . . H84B H -0.0844 -0.1579 0.0462 0.050 Uiso 1 1 calc R . . C85 C -0.00446(17) -0.2422(3) 0.0495(3) 0.046(2) Uani 1 1 d . . . H85A H -0.0044 -0.2762 0.0222 0.056 Uiso 1 1 calc R . . H85B H -0.0207 -0.2548 0.0622 0.056 Uiso 1 1 calc R . . C86 C 0.03220(17) -0.2328(3) 0.1079(3) 0.052(2) Uani 1 1 d . . . H86A H 0.0356 -0.2580 0.1441 0.063 Uiso 1 1 calc R . . H86B H 0.0502 -0.2447 0.0993 0.063 Uiso 1 1 calc R . . C87 C 0.03202(16) -0.1613(4) 0.1186(3) 0.057(3) Uani 1 1 d . . . H87A H 0.0206 -0.1517 0.1417 0.068 Uiso 1 1 calc R . . H87B H 0.0558 -0.1440 0.1423 0.068 Uiso 1 1 calc R . . C88 C 0.01212(15) -0.1339(3) 0.0541(3) 0.045(2) Uani 1 1 d . . . H88A H 0.0017 -0.0921 0.0540 0.054 Uiso 1 1 calc R . . H88B H 0.0272 -0.1274 0.0375 0.054 Uiso 1 1 calc R . . C89 C -0.01284(15) -0.2422(3) -0.1000(3) 0.047(2) Uani 1 1 d . . . H89A H 0.0067 -0.2318 -0.0574 0.056 Uiso 1 1 calc R . . H89B H -0.0142 -0.2091 -0.1294 0.056 Uiso 1 1 calc R . . C90 C -0.00834(16) -0.3071(3) -0.1192(3) 0.053(2) Uani 1 1 d . . . H90A H 0.0071 -0.3338 -0.0822 0.063 Uiso 1 1 calc R . . H90B H 0.0015 -0.3039 -0.1458 0.063 Uiso 1 1 calc R . . C91 C -0.04403(15) -0.3354(4) -0.1556(3) 0.048(2) Uani 1 1 d . . . H91A H -0.0567 -0.3213 -0.1998 0.057 Uiso 1 1 calc R . . H91B H -0.0434 -0.3830 -0.1539 0.057 Uiso 1 1 calc R . . C92 C -0.05965(15) -0.3081(3) -0.1210(3) 0.041(2) Uani 1 1 d . . . H92A H -0.0850 -0.3050 -0.1488 0.049 Uiso 1 1 calc R . . H92B H -0.0540 -0.3351 -0.0844 0.049 Uiso 1 1 calc R . . C93 C -0.09780(15) -0.1741(3) -0.2332(3) 0.039(2) Uani 1 1 d . . . H93A H -0.0771 -0.2003 -0.2204 0.046 Uiso 1 1 calc R . . H93B H -0.0931 -0.1291 -0.2391 0.046 Uiso 1 1 calc R . . C94 C -0.12886(17) -0.2004(3) -0.2932(3) 0.045(2) Uani 1 1 d . . . H94A H -0.1439 -0.1651 -0.3203 0.054 Uiso 1 1 calc R . . H94B H -0.1216 -0.2267 -0.3168 0.054 Uiso 1 1 calc R . . C95 C -0.14712(16) -0.2411(3) -0.2698(3) 0.043(2) Uani 1 1 d . . . H95A H -0.1720 -0.2446 -0.3020 0.052 Uiso 1 1 calc R . . H95B H -0.1371 -0.2848 -0.2585 0.052 Uiso 1 1 calc R . . C96 C -0.14140(14) -0.2061(3) -0.2143(3) 0.0359(19) Uani 1 1 d . . . H96A H -0.1590 -0.1722 -0.2265 0.043 Uiso 1 1 calc R . . H96B H -0.1422 -0.2358 -0.1845 0.043 Uiso 1 1 calc R . . O1S O -0.13499(19) 0.0517(4) 0.0000(3) 0.135(2) Uani 1 1 d U . . O2S O -0.09762(10) -0.8022(2) -0.3586(2) 0.135(2) Uani 1 1 d DU . . O3S O 0.0000 -0.0304(6) 0.2500 0.153(3) Uani 1 2 d SU . . O4S O 0.0000 -0.1944(3) 0.2500 0.153(3) Uani 1 2 d SDU . . C1S C -0.1563(2) 0.0919(5) -0.0494(4) 0.103(2) Uani 1 1 d U . . H1SA H -0.1789 0.0709 -0.0766 0.124 Uiso 1 1 calc R . . H1SB H -0.1460 0.1001 -0.0747 0.124 Uiso 1 1 calc R . . C2S C -0.1611(2) 0.1548(5) -0.0249(4) 0.085(2) Uani 1 1 d U . . H2SA H -0.1451 0.1880 -0.0228 0.102 Uiso 1 1 calc R . . H2SB H -0.1850 0.1706 -0.0518 0.102 Uiso 1 1 calc R . . C3S C -0.1533(2) 0.1383(5) 0.0385(5) 0.119(3) Uani 1 1 d U . . H3SA H -0.1395 0.1725 0.0689 0.143 Uiso 1 1 calc R . . H3SB H -0.1747 0.1317 0.0383 0.143 Uiso 1 1 calc R . . C4S C -0.1334(3) 0.0780(6) 0.0538(5) 0.122(3) Uani 1 1 d U . . H4SA H -0.1090 0.0866 0.0867 0.146 Uiso 1 1 calc R . . H4SB H -0.1426 0.0464 0.0705 0.146 Uiso 1 1 calc R . . C5S C -0.11474(15) -0.8192(2) -0.3283(3) 0.103(2) Uani 1 1 d DU . . H5SA H -0.1034 -0.8574 -0.3018 0.124 Uiso 1 1 calc R . . H5SB H -0.1388 -0.8312 -0.3602 0.124 Uiso 1 1 calc R . . C6S C -0.1152(2) -0.7663(4) -0.2878(4) 0.085(2) Uani 1 1 d DU . . H6SA H -0.0922 -0.7540 -0.2521 0.102 Uiso 1 1 calc R . . H6SB H -0.1317 -0.7735 -0.2743 0.102 Uiso 1 1 calc R . . C7S C -0.12912(13) -0.7220(2) -0.3458(3) 0.119(3) Uani 1 1 d DU . . H7SA H -0.1546 -0.7225 -0.3703 0.143 Uiso 1 1 calc R . . H7SB H -0.1213 -0.6773 -0.3322 0.143 Uiso 1 1 calc R . . C8S C -0.11582(17) -0.7459(3) -0.3865(3) 0.122(3) Uani 1 1 d DU . . H8SA H -0.1353 -0.7545 -0.4297 0.146 Uiso 1 1 calc R . . H8SB H -0.1006 -0.7133 -0.3882 0.146 Uiso 1 1 calc R . . C9S C -0.0246(2) 0.0105(5) 0.2512(4) 0.106(2) Uani 1 1 d U . . H9SA H -0.0288 -0.0043 0.2839 0.127 Uiso 1 1 calc R . . H9SB H -0.0467 0.0088 0.2103 0.127 Uiso 1 1 calc R . . C10S C -0.0113(3) 0.0780(6) 0.2648(6) 0.173(4) Uani 1 1 d U . . H10A H 0.0026 0.0866 0.3103 0.207 Uiso 1 1 calc R . . H10B H -0.0303 0.1097 0.2442 0.207 Uiso 1 1 calc R . . C11S C -0.01138(19) -0.22855(17) 0.19450(16) 0.106(2) Uani 1 1 d DU . . H11A H 0.0057 -0.2272 0.1819 0.127 Uiso 1 1 calc R . . H11B H -0.0338 -0.2123 0.1598 0.127 Uiso 1 1 calc RD . . C12S C -0.01458(14) -0.2960(2) 0.21513(11) 0.173(4) Uani 1 1 d DU . . H12A H -0.0109 -0.3296 0.1915 0.207 Uiso 1 1 calc RD . . H12B H -0.0374 -0.3024 0.2099 0.207 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 Dy1 0.02781(13) 0.02547(15) 0.02934(14) 0.00056(15) 0.01628(11) -0.00290(15) Ga1 0.0255(3) 0.0200(3) 0.0230(3) -0.0011(3) 0.0135(3) 0.0012(3) Ga2 0.0284(3) 0.0216(4) 0.0240(3) 0.0032(3) 0.0151(3) 0.0025(3) I1 0.0415(2) 0.0386(3) 0.0382(2) 0.0006(2) 0.02181(18) -0.0136(2) N1 0.024(2) 0.021(3) 0.016(2) -0.002(2) 0.0104(19) -0.002(2) N2 0.025(2) 0.027(3) 0.021(2) -0.010(2) 0.0132(19) 0.004(2) N3 0.026(2) 0.022(3) 0.017(2) 0.003(2) 0.0129(19) 0.006(2) N4 0.035(2) 0.022(3) 0.019(2) 0.006(2) 0.014(2) 0.010(2) O1 0.063(2) 0.031(3) 0.049(2) -0.004(2) 0.0412(19) -0.001(2) O2 0.0293(19) 0.040(3) 0.033(2) 0.001(2) 0.0211(17) 0.000(2) O3 0.045(2) 0.031(2) 0.026(2) 0.0024(19) 0.0224(17) 0.001(2) O4 0.033(2) 0.033(3) 0.028(2) 0.0058(19) 0.0079(18) 0.005(2) O5 0.033(2) 0.033(3) 0.048(2) -0.004(2) 0.0249(18) -0.005(2) O6 0.040(2) 0.043(3) 0.027(2) -0.0046(19) 0.0203(17) -0.009(2) C1 0.029(3) 0.018(3) 0.019(3) 0.008(3) 0.010(2) 0.003(3) C2 0.015(2) 0.037(4) 0.020(3) -0.003(3) 0.012(2) -0.003(3) C3 0.027(3) 0.038(4) 0.022(3) 0.003(3) 0.012(2) -0.005(3) C4 0.020(3) 0.023(3) 0.017(3) 0.006(3) 0.005(2) -0.001(3) C5 0.022(3) 0.026(3) 0.028(3) -0.003(3) 0.009(3) -0.008(3) C6 0.029(3) 0.022(3) 0.026(3) 0.004(3) 0.016(2) -0.001(3) C7 0.019(3) 0.022(3) 0.031(3) -0.008(3) 0.010(2) -0.005(3) C8 0.025(3) 0.023(3) 0.042(4) 0.006(3) 0.012(3) 0.012(3) C9 0.035(3) 0.036(4) 0.036(3) 0.004(3) 0.022(3) -0.002(3) C10 0.039(3) 0.041(4) 0.034(4) 0.009(3) 0.020(3) 0.006(3) C11 0.040(3) 0.068(5) 0.029(4) 0.018(4) 0.019(3) 0.022(4) C12 0.038(3) 0.038(4) 0.027(3) 0.001(3) 0.017(3) 0.010(3) C13 0.026(3) 0.016(3) 0.026(3) 0.008(3) 0.013(2) 0.005(3) C14 0.022(3) 0.015(3) 0.041(4) 0.006(3) 0.017(3) 0.004(3) C15 0.069(3) 0.029(4) 0.038(3) 0.006(3) 0.044(3) 0.010(3) C16 0.060(4) 0.047(5) 0.036(4) -0.002(3) 0.032(3) 0.003(4) C17 0.049(4) 0.038(4) 0.035(4) -0.008(3) 0.020(3) 0.001(3) C18 0.031(3) 0.020(3) 0.026(3) -0.001(3) 0.015(3) 0.008(3) C19 0.040(3) 0.033(4) 0.033(3) 0.008(3) 0.026(3) 0.007(3) C20 0.048(3) 0.038(4) 0.063(4) -0.008(3) 0.040(3) -0.008(3) C21 0.041(4) 0.049(5) 0.050(4) 0.007(4) 0.023(3) -0.003(4) C22 0.026(3) 0.026(4) 0.020(3) -0.007(3) 0.010(2) -0.005(3) C23 0.030(3) 0.025(3) 0.028(3) -0.006(3) 0.009(3) -0.006(3) C24 0.033(3) 0.029(4) 0.034(3) -0.002(3) 0.016(3) 0.002(3) C25 0.019(3) 0.038(4) 0.030(3) 0.000(3) 0.010(3) 0.004(3) C26 0.023(3) 0.082(6) 0.027(3) -0.021(4) 0.011(3) -0.006(4) C27 0.034(4) 0.114(7) 0.049(4) -0.049(5) 0.017(3) -0.028(4) C28 0.043(4) 0.104(7) 0.038(4) -0.040(4) 0.020(3) -0.016(4) C29 0.047(4) 0.063(5) 0.032(4) 0.001(4) 0.023(3) 0.010(4) C30 0.045(3) 0.031(4) 0.025(3) 0.001(3) 0.018(3) 0.005(3) C31 0.029(3) 0.127(8) 0.051(4) -0.032(5) 0.029(3) -0.018(4) C32 0.077(4) 0.106(7) 0.129(5) -0.064(5) 0.089(4) -0.051(5) C33 0.043(4) 0.115(8) 0.057(5) 0.023(5) 0.021(4) 0.019(5) C34 0.042(3) 0.060(5) 0.013(3) -0.011(3) 0.018(2) -0.022(3) C35 0.067(4) 0.042(4) 0.065(4) 0.008(4) 0.047(3) -0.005(4) C36 0.025(3) 0.079(6) 0.043(4) 0.020(4) 0.007(3) -0.001(4) C37 0.038(3) 0.016(3) 0.027(3) -0.003(3) 0.017(3) 0.002(3) C38 0.036(3) 0.022(3) 0.021(3) 0.000(3) 0.017(2) 0.007(3) C39 0.032(3) 0.019(3) 0.018(3) -0.002(2) 0.015(2) 0.005(3) C40 0.028(3) 0.018(3) 0.033(3) -0.002(3) 0.020(2) -0.002(3) C41 0.033(3) 0.016(3) 0.021(3) 0.003(3) 0.011(3) 0.007(3) C42 0.034(3) 0.022(3) 0.031(3) 0.003(3) 0.017(3) -0.001(3) C43 0.038(3) 0.039(4) 0.029(4) 0.011(3) 0.012(3) 0.003(3) C44 0.021(3) 0.048(4) 0.037(4) 0.005(3) 0.008(3) 0.009(3) C45 0.031(3) 0.028(4) 0.033(3) -0.002(3) 0.017(3) 0.000(3) C46 0.032(3) 0.043(4) 0.043(4) 0.003(3) 0.016(3) 0.006(3) C47 0.030(3) 0.044(4) 0.037(3) -0.006(3) 0.023(3) -0.009(3) C48 0.049(3) 0.033(4) 0.027(3) 0.009(3) 0.027(3) 0.003(3) C49 0.028(3) 0.029(4) 0.025(3) 0.008(3) 0.014(2) 0.006(3) C50 0.032(3) 0.022(3) 0.036(3) 0.000(3) 0.020(3) -0.003(3) C51 0.033(3) 0.016(3) 0.050(4) -0.003(3) 0.020(3) 0.004(3) C52 0.020(3) 0.032(4) 0.038(4) 0.018(3) 0.006(3) 0.002(3) C53 0.026(3) 0.035(4) 0.029(3) 0.003(3) 0.015(2) 0.004(3) C54 0.024(3) 0.021(3) 0.019(3) 0.001(3) 0.010(2) 0.000(3) C55 0.042(3) 0.026(4) 0.038(3) -0.009(3) 0.026(3) -0.007(3) C56 0.053(4) 0.053(5) 0.061(4) -0.004(4) 0.035(3) 0.015(4) C57 0.037(3) 0.036(4) 0.042(4) -0.001(3) 0.023(3) 0.014(3) C58 0.036(3) 0.032(4) 0.019(3) 0.005(3) 0.015(2) 0.000(3) C59 0.065(4) 0.039(4) 0.049(4) 0.010(3) 0.043(3) 0.011(4) C60 0.073(4) 0.032(4) 0.034(4) -0.008(3) 0.029(3) -0.004(4) C61 0.020(3) 0.032(4) 0.017(3) 0.001(3) 0.010(2) -0.006(3) C62 0.021(3) 0.028(3) 0.015(3) 0.002(3) 0.009(2) 0.002(3) C63 0.035(3) 0.037(4) 0.040(4) -0.001(3) 0.024(3) 0.001(3) C64 0.045(3) 0.034(4) 0.033(3) 0.009(3) 0.023(3) -0.007(3) C65 0.049(3) 0.024(4) 0.053(4) 0.004(3) 0.032(3) 0.002(3) C66 0.024(3) 0.023(3) 0.023(3) -0.006(3) 0.010(2) -0.002(3) C67 0.063(4) 0.028(4) 0.023(3) -0.002(3) 0.030(3) 0.007(3) C68 0.050(4) 0.032(4) 0.046(4) -0.006(3) 0.021(3) 0.009(3) C69 0.050(4) 0.037(4) 0.066(4) -0.002(4) 0.035(3) 0.005(3) C70 0.037(3) 0.020(4) 0.045(4) 0.006(3) 0.025(3) 0.001(3) C71 0.051(4) 0.023(4) 0.053(4) -0.004(3) 0.024(3) 0.001(3) C72 0.057(4) 0.028(4) 0.034(4) -0.005(3) 0.023(3) 0.008(3) C73 0.040(3) 0.021(3) 0.034(3) 0.002(3) 0.021(3) 0.002(3) C74 0.054(4) 0.029(4) 0.063(4) -0.006(3) 0.041(3) -0.003(3) C75 0.053(4) 0.024(4) 0.073(5) -0.022(4) 0.031(4) -0.002(3) C76 0.056(4) 0.038(4) 0.080(5) -0.035(3) 0.046(3) -0.019(3) C77 0.047(3) 0.029(4) 0.041(4) 0.016(3) 0.025(3) 0.011(3) C78 0.045(4) 0.060(5) 0.043(4) 0.013(4) 0.022(3) 0.008(4) C79 0.032(3) 0.052(5) 0.068(5) 0.020(4) 0.025(3) 0.010(4) C80 0.036(3) 0.099(6) 0.041(4) 0.025(4) 0.026(3) 0.017(4) C81 0.047(3) 0.028(4) 0.052(4) -0.009(3) 0.030(3) -0.005(3) C82 0.057(4) 0.044(4) 0.039(4) -0.019(4) 0.021(3) -0.005(4) C83 0.062(4) 0.046(5) 0.047(4) -0.016(3) 0.036(3) -0.024(4) C84 0.048(4) 0.047(4) 0.030(4) 0.000(3) 0.020(3) -0.002(4) C85 0.043(4) 0.038(4) 0.031(4) 0.005(3) 0.002(3) 0.009(4) C86 0.044(4) 0.055(5) 0.052(4) 0.026(4) 0.021(3) 0.017(4) C87 0.025(3) 0.089(6) 0.034(4) 0.008(4) 0.000(3) -0.018(4) C88 0.023(3) 0.051(5) 0.044(4) 0.017(4) 0.006(3) 0.003(3) C89 0.040(3) 0.049(5) 0.058(4) -0.009(4) 0.030(3) 0.000(4) C90 0.054(4) 0.057(5) 0.055(4) 0.001(4) 0.034(3) 0.013(4) C91 0.047(3) 0.053(5) 0.042(4) -0.020(4) 0.024(3) 0.000(4) C92 0.044(3) 0.028(4) 0.054(4) -0.006(3) 0.028(3) -0.005(3) C93 0.046(3) 0.045(5) 0.026(3) 0.000(3) 0.020(3) -0.005(3) C94 0.068(4) 0.037(4) 0.025(4) -0.006(3) 0.021(3) -0.007(4) C95 0.040(4) 0.046(4) 0.032(4) -0.005(3) 0.010(3) -0.007(4) C96 0.035(3) 0.026(4) 0.046(4) -0.007(3) 0.021(3) -0.008(3) O1S 0.163(3) 0.124(4) 0.124(3) 0.004(3) 0.080(2) 0.029(3) O2S 0.163(3) 0.124(4) 0.124(3) 0.004(3) 0.080(2) 0.029(3) O3S 0.165(4) 0.133(5) 0.136(4) 0.000 0.064(3) 0.000 O4S 0.165(4) 0.133(5) 0.136(4) 0.000 0.064(3) 0.000 C1S 0.114(3) 0.109(4) 0.109(4) -0.003(3) 0.073(3) -0.031(3) C2S 0.099(3) 0.088(4) 0.082(3) 0.003(3) 0.058(2) 0.001(3) C3S 0.127(4) 0.139(5) 0.111(4) -0.004(4) 0.076(3) 0.020(4) C4S 0.126(4) 0.135(5) 0.110(4) 0.030(4) 0.067(3) 0.038(4) C5S 0.114(3) 0.109(4) 0.109(4) -0.003(3) 0.073(3) -0.031(3) C6S 0.099(3) 0.088(4) 0.082(3) 0.003(3) 0.058(2) 0.001(3) C7S 0.127(4) 0.139(5) 0.111(4) -0.004(4) 0.076(3) 0.020(4) C8S 0.126(4) 0.135(5) 0.110(4) 0.030(4) 0.067(3) 0.038(4) C9S 0.118(4) 0.115(4) 0.091(3) -0.020(3) 0.060(3) 0.004(4) C10S 0.182(5) 0.147(5) 0.167(5) 0.003(4) 0.078(3) 0.000(4) C11S 0.118(4) 0.115(4) 0.091(3) -0.020(3) 0.060(3) 0.004(4) C12S 0.182(5) 0.147(5) 0.167(5) 0.003(4) 0.078(3) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.005(5) . ? Dy1 O3 2.395(4) . ? Dy1 O2 2.404(4) . ? Dy1 O4 2.409(3) . ? Dy1 O5 2.430(4) . ? Dy1 O6 2.444(4) . ? Dy1 I1 3.0513(6) . ? Ga1 N2 1.904(4) . ? Ga1 N1 1.936(5) . ? Ga1 C73 1.992(6) . ? Ga1 Ga2 2.5298(10) . ? Ga2 N4 1.915(5) . ? Ga2 N3 1.927(4) . ? N1 C1 1.386(7) . ? N1 C13 1.428(8) . ? N2 C2 1.381(7) . ? N2 C25 1.435(7) . ? N3 C37 1.362(7) . ? N3 C49 1.433(8) . ? N4 C38 1.381(6) . ? N4 C61 1.466(8) . ? O1 C76 1.437(8) . ? O2 C80 1.449(8) . ? O2 C77 1.481(7) . ? O3 C84 1.429(6) . ? O3 C81 1.456(7) . ? O4 C85 1.445(7) . ? O4 C88 1.460(7) . ? O5 C89 1.430(8) . ? O5 C92 1.453(7) . ? O6 C93 1.445(8) . ? O6 C96 1.464(7) . ? C1 C2 1.382(8) . ? C1 C5 1.463(8) . ? C2 C3 1.481(8) . ? C3 C12 1.353(8) . ? C3 C4 1.447(9) . ? C4 C9 1.388(8) . ? C4 C5 1.435(8) . ? C5 C6 1.360(8) . ? C6 C7 1.441(8) . ? C7 C8 1.345(8) . ? C8 C9 1.425(9) . ? C9 C10 1.442(8) . ? C10 C11 1.358(9) . ? C11 C12 1.459(9) . ? C13 C14 1.388(8) . ? C13 C18 1.426(7) . ? C14 C15 1.414(9) . ? C14 C19 1.520(7) . ? C15 C16 1.371(8) . ? C16 C17 1.375(10) . ? C17 C18 1.408(9) . ? C18 C22 1.503(9) . ? C19 C20 1.535(9) . ? C19 C21 1.556(8) . ? C22 C23 1.529(7) . ? C22 C24 1.557(8) . ? C25 C26 1.401(8) . ? C25 C30 1.402(9) . ? C26 C27 1.395(9) . ? C26 C31 1.483(10) . ? C27 C28 1.369(11) . ? C28 C29 1.344(9) . ? C29 C30 1.413(9) . ? C30 C34 1.508(8) . ? C31 C33 1.472(10) . ? C31 C32 1.532(11) . ? C34 C36 1.473(9) . ? C34 C35 1.541(9) . ? C37 C38 1.396(9) . ? C37 C41 1.473(7) . ? C38 C39 1.469(7) . ? C39 C48 1.365(8) . ? C39 C40 1.447(8) . ? C40 C45 1.374(7) . ? C40 C41 1.401(8) . ? C41 C42 1.371(8) . ? C42 C43 1.409(8) . ? C43 C44 1.347(9) . ? C44 C45 1.454(9) . ? C45 C46 1.400(9) . ? C46 C47 1.375(9) . ? C47 C48 1.412(7) . ? C49 C50 1.394(8) . ? C49 C54 1.403(9) . ? C50 C51 1.395(9) . ? C50 C55 1.552(9) . ? C51 C52 1.368(10) . ? C52 C53 1.375(9) . ? C53 C54 1.388(8) . ? C54 C58 1.539(8) . ? C55 C57 1.514(8) . ? C55 C56 1.546(8) . ? C58 C59 1.515(9) . ? C58 C60 1.530(8) . ? C61 C62 1.389(8) . ? C61 C66 1.400(8) . ? C62 C63 1.375(9) . ? C62 C67 1.544(8) . ? C63 C64 1.373(8) . ? C64 C65 1.371(9) . ? C65 C66 1.373(9) . ? C66 C70 1.494(9) . ? C67 C69 1.520(8) . ? C67 C68 1.524(9) . ? C70 C72 1.529(8) . ? C70 C71 1.532(8) . ? C73 C74 1.526(9) . ? C74 C75 1.582(9) . ? C75 C76 1.391(9) . ? C77 C78 1.470(8) . ? C78 C79 1.500(10) . ? C79 C80 1.463(8) . ? C81 C82 1.489(9) . ? C82 C83 1.494(9) . ? C83 C84 1.495(9) . ? C85 C86 1.548(8) . ? C86 C87 1.513(10) . ? C87 C88 1.491(9) . ? C89 C90 1.487(9) . ? C90 C91 1.506(9) . ? C91 C92 1.505(10) . ? C93 C94 1.524(8) . ? C94 C95 1.513(10) . ? C95 C96 1.473(9) . ? O1S C1S 1.382(11) . ? O1S C4S 1.429(12) . ? O2S C8S 1.392(4) . ? O2S C5S 1.404(5) . ? O3S C9S 1.428(11) . ? O3S C9S 1.428(11) 2 ? O4S C11S 1.400(4) 2 ? O4S C11S 1.400(4) . ? C1S C2S 1.513(13) . ? C2S C3S 1.483(13) . ? C3S C4S 1.476(14) . ? C5S C6S 1.510(10) . ? C6S C7S 1.549(10) . ? C7S C8S 1.531(5) . ? C9S C10S 1.496(14) . ? C10S C10S 1.57(3) 2 ? C11S C12S 1.530(4) . ? C12S C12S 1.543(4) 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 O1 Dy1 O3 89.86(16) . . ? O1 Dy1 O2 87.97(15) . . ? O3 Dy1 O2 72.44(13) . . ? O1 Dy1 O4 89.59(15) . . ? O3 Dy1 O4 73.13(14) . . ? O2 Dy1 O4 145.49(14) . . ? O1 Dy1 O5 84.82(16) . . ? O3 Dy1 O5 144.99(12) . . ? O2 Dy1 O5 141.57(12) . . ? O4 Dy1 O5 72.26(13) . . ? O1 Dy1 O6 96.39(15) . . ? O3 Dy1 O6 142.75(13) . . ? O2 Dy1 O6 71.14(14) . . ? O4 Dy1 O6 143.26(15) . . ? O5 Dy1 O6 72.25(13) . . ? O1 Dy1 I1 175.73(11) . . ? O3 Dy1 I1 90.40(10) . . ? O2 Dy1 I1 96.17(10) . . ? O4 Dy1 I1 86.41(10) . . ? O5 Dy1 I1 92.53(10) . . ? O6 Dy1 I1 85.96(10) . . ? N2 Ga1 N1 87.36(19) . . ? N2 Ga1 C73 118.6(2) . . ? N1 Ga1 C73 118.0(2) . . ? N2 Ga1 Ga2 119.40(15) . . ? N1 Ga1 Ga2 114.56(12) . . ? C73 Ga1 Ga2 100.12(17) . . ? N4 Ga2 N3 87.02(19) . . ? N4 Ga2 Ga1 148.13(14) . . ? N3 Ga2 Ga1 121.43(15) . . ? C1 N1 C13 119.4(5) . . ? C1 N1 Ga1 108.3(4) . . ? C13 N1 Ga1 130.2(4) . . ? C2 N2 C25 118.8(4) . . ? C2 N2 Ga1 109.5(3) . . ? C25 N2 Ga1 130.6(4) . . ? C37 N3 C49 116.0(4) . . ? C37 N3 Ga2 109.2(4) . . ? C49 N3 Ga2 131.8(3) . . ? C38 N4 C61 120.3(5) . . ? C38 N4 Ga2 109.6(4) . . ? C61 N4 Ga2 127.3(3) . . ? C76 O1 Dy1 165.7(4) . . ? C80 O2 C77 107.9(5) . . ? C80 O2 Dy1 124.3(4) . . ? C77 O2 Dy1 127.2(4) . . ? C84 O3 C81 107.7(5) . . ? C84 O3 Dy1 122.1(3) . . ? C81 O3 Dy1 129.9(4) . . ? C85 O4 C88 108.8(4) . . ? C85 O4 Dy1 123.7(3) . . ? C88 O4 Dy1 126.6(3) . . ? C89 O5 C92 109.7(5) . . ? C89 O5 Dy1 128.4(4) . . ? C92 O5 Dy1 121.9(4) . . ? C93 O6 C96 110.1(4) . . ? C93 O6 Dy1 128.8(3) . . ? C96 O6 Dy1 120.3(4) . . ? C2 C1 N1 117.4(5) . . ? C2 C1 C5 110.8(5) . . ? N1 C1 C5 131.7(5) . . ? N2 C2 C1 117.2(5) . . ? N2 C2 C3 133.9(5) . . ? C1 C2 C3 108.9(5) . . ? C12 C3 C4 118.2(6) . . ? C12 C3 C2 137.5(6) . . ? C4 C3 C2 104.4(5) . . ? C9 C4 C5 124.0(6) . . ? C9 C4 C3 124.4(5) . . ? C5 C4 C3 111.5(5) . . ? C6 C5 C4 117.4(5) . . ? C6 C5 C1 138.1(6) . . ? C4 C5 C1 104.4(5) . . ? C5 C6 C7 118.9(5) . . ? C8 C7 C6 123.2(6) . . ? C7 C8 C9 119.6(6) . . ? C4 C9 C8 116.9(6) . . ? C4 C9 C10 116.4(6) . . ? C8 C9 C10 126.7(6) . . ? C11 C10 C9 119.2(6) . . ? C10 C11 C12 123.6(6) . . ? C3 C12 C11 118.1(6) . . ? C14 C13 C18 120.8(6) . . ? C14 C13 N1 121.1(5) . . ? C18 C13 N1 118.1(5) . . ? C13 C14 C15 119.2(5) . . ? C13 C14 C19 121.1(6) . . ? C15 C14 C19 119.7(6) . . ? C16 C15 C14 119.9(7) . . ? C15 C16 C17 121.8(7) . . ? C16 C17 C18 120.3(6) . . ? C17 C18 C13 118.1(6) . . ? C17 C18 C22 119.6(5) . . ? C13 C18 C22 122.1(5) . . ? C14 C19 C20 111.9(5) . . ? C14 C19 C21 111.4(5) . . ? C20 C19 C21 108.8(5) . . ? C18 C22 C23 114.1(5) . . ? C18 C22 C24 109.4(5) . . ? C23 C22 C24 111.1(4) . . ? C26 C25 C30 121.1(6) . . ? C26 C25 N2 119.3(6) . . ? C30 C25 N2 119.5(5) . . ? C27 C26 C25 116.7(7) . . ? C27 C26 C31 120.6(6) . . ? C25 C26 C31 122.7(6) . . ? C28 C27 C26 123.5(7) . . ? C29 C28 C27 118.7(7) . . ? C28 C29 C30 122.2(7) . . ? C25 C30 C29 117.7(6) . . ? C25 C30 C34 122.3(5) . . ? C29 C30 C34 119.9(6) . . ? C33 C31 C26 116.0(7) . . ? C33 C31 C32 109.6(6) . . ? C26 C31 C32 111.0(7) . . ? C36 C34 C30 112.1(6) . . ? C36 C34 C35 112.0(6) . . ? C30 C34 C35 110.0(5) . . ? N3 C37 C38 117.8(5) . . ? N3 C37 C41 135.0(6) . . ? C38 C37 C41 107.2(5) . . ? N4 C38 C37 116.4(5) . . ? N4 C38 C39 132.9(6) . . ? C37 C38 C39 110.7(5) . . ? C48 C39 C40 117.6(5) . . ? C48 C39 C38 138.5(5) . . ? C40 C39 C38 103.9(5) . . ? C45 C40 C41 126.5(6) . . ? C45 C40 C39 122.3(6) . . ? C41 C40 C39 111.2(5) . . ? C42 C41 C40 118.1(5) . . ? C42 C41 C37 134.8(6) . . ? C40 C41 C37 107.1(5) . . ? C41 C42 C43 117.1(6) . . ? C44 C43 C42 125.0(6) . . ? C43 C44 C45 119.2(5) . . ? C40 C45 C46 118.3(6) . . ? C40 C45 C44 114.1(6) . . ? C46 C45 C44 127.6(5) . . ? C47 C46 C45 120.5(5) . . ? C46 C47 C48 121.1(6) . . ? C39 C48 C47 120.3(6) . . ? C50 C49 C54 119.7(6) . . ? C50 C49 N3 120.0(6) . . ? C54 C49 N3 120.2(5) . . ? C49 C50 C51 118.9(6) . . ? C49 C50 C55 121.9(6) . . ? C51 C50 C55 119.1(6) . . ? C52 C51 C50 120.1(6) . . ? C51 C52 C53 122.3(6) . . ? C52 C53 C54 118.2(6) . . ? C53 C54 C49 120.7(6) . . ? C53 C54 C58 118.6(6) . . ? C49 C54 C58 120.7(5) . . ? C57 C55 C56 109.2(5) . . ? C57 C55 C50 113.1(5) . . ? C56 C55 C50 110.6(5) . . ? C59 C58 C60 111.0(5) . . ? C59 C58 C54 114.5(5) . . ? C60 C58 C54 110.0(5) . . ? C62 C61 C66 122.2(6) . . ? C62 C61 N4 120.9(5) . . ? C66 C61 N4 116.9(6) . . ? C63 C62 C61 117.7(6) . . ? C63 C62 C67 118.7(6) . . ? C61 C62 C67 123.5(6) . . ? C64 C63 C62 122.1(7) . . ? C65 C64 C63 118.4(7) . . ? C64 C65 C66 123.1(6) . . ? C65 C66 C61 116.6(6) . . ? C65 C66 C70 119.6(6) . . ? C61 C66 C70 123.6(6) . . ? C69 C67 C68 111.4(5) . . ? C69 C67 C62 110.9(5) . . ? C68 C67 C62 111.9(5) . . ? C66 C70 C72 114.4(5) . . ? C66 C70 C71 110.2(5) . . ? C72 C70 C71 111.9(5) . . ? C74 C73 Ga1 113.2(5) . . ? C73 C74 C75 111.8(6) . . ? C76 C75 C74 112.0(6) . . ? C75 C76 O1 113.2(6) . . ? C78 C77 O2 105.5(5) . . ? C77 C78 C79 106.9(5) . . ? C80 C79 C78 107.0(6) . . ? O2 C80 C79 107.9(6) . . ? O3 C81 C82 105.8(5) . . ? C81 C82 C83 102.1(5) . . ? C82 C83 C84 102.1(6) . . ? O3 C84 C83 106.9(4) . . ? O4 C85 C86 106.7(5) . . ? C87 C86 C85 100.8(5) . . ? C88 C87 C86 103.9(6) . . ? O4 C88 C87 105.0(5) . . ? O5 C89 C90 106.0(5) . . ? C89 C90 C91 105.0(6) . . ? C92 C91 C90 101.4(5) . . ? O5 C92 C91 104.6(6) . . ? O6 C93 C94 105.2(5) . . ? C95 C94 C93 103.4(5) . . ? C96 C95 C94 103.8(5) . . ? O6 C96 C95 104.6(5) . . ? C1S O1S C4S 106.3(8) . . ? C8S O2S C5S 97.4(5) . . ? C9S O3S C9S 106.8(12) . 2 ? C11S O4S C11S 119.1(6) 2 . ? O1S C1S C2S 110.0(8) . . ? C3S C2S C1S 103.7(8) . . ? C4S C3S C2S 103.8(9) . . ? O1S C4S C3S 111.4(9) . . ? O2S C5S C6S 113.5(5) . . ? C5S C6S C7S 86.6(5) . . ? C8S C7S C6S 109.4(5) . . ? O2S C8S C7S 106.2(5) . . ? O3S C9S C10S 109.5(10) . . ? C9S C10S C10S 100.6(8) . 2 ? O4S C11S C12S 100.2(4) . . ? C11S C12S C12S 101.9(3) . 2 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.083 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.133 _publ_section_references ; Bruker (2003) SAINTPlus Data Reduction and Correction Program v. 6.45a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005) SMART. Bruker Molecular Analysis Research Tool, v. 5.632 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker|Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; #==============================================================================