# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c: _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Dinitro{(+-)-2,7,12-Trimethoxy-3,8,13-tris(2-N-oxide-pyridylmethoxy)-10,15-dihydro-5H- tribenzo[a,d,g]cyclononatriene}]gadolinium(III) dimethylformamide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H46 Gd N7 O19' _chemical_formula_weight 1146.14 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 44.860(4) _cell_length_b 15.1635(14) _cell_length_c 15.6748(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.550(4) _cell_angle_gamma 90.00 _cell_volume 10570.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4648 _exptl_absorpt_coefficient_mu 1.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8783 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER X8 CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34505 _diffrn_reflns_av_R_equivalents 0.0958 _diffrn_reflns_av_sigmaI/netI 0.1242 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.73 _reflns_number_total 10908 _reflns_number_gt 6048 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The solvent DMF molecule was refined isotropically and modelled as disordered across two positions, each at 50% occupancy. C-O bond lengths of the disordered DMF were restrained to be chemically reasonable. ; _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^)+(0.1170P)^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 10908 _refine_ls_number_parameters 633 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1437 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2194 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.099611(10) 0.16107(3) 0.06720(2) 0.04213(17) Uani 1 1 d . . . O1 O 0.27941(14) 0.4050(4) 0.0901(4) 0.0543(16) Uani 1 1 d . . . N1 N 0.15022(19) 0.2929(5) -0.0324(5) 0.058(2) Uani 1 1 d . . . C1 C 0.2841(2) 0.2673(6) 0.2925(5) 0.048(2) Uani 1 1 d . . . O2 O 0.22938(14) 0.3088(4) 0.0543(4) 0.0513(15) Uani 1 1 d . . . N2 N 0.38566(18) -0.2924(5) 0.2244(4) 0.0482(18) Uani 1 1 d . . . C2 C 0.2910(2) 0.3324(5) 0.2321(6) 0.046(2) Uani 1 1 d . . . H2 H 0.3079 0.3695 0.2470 0.055 Uiso 1 1 calc R . . O3 O 0.26672(14) -0.1074(4) 0.1150(4) 0.0555(16) Uani 1 1 d . . . N3 N 0.44531(18) 0.4998(5) 0.3617(4) 0.0485(18) Uani 1 1 d . . . C3 C 0.2736(2) 0.3435(6) 0.1521(6) 0.048(2) Uani 1 1 d . . . O4 O 0.31631(15) -0.1662(4) 0.2065(4) 0.0559(16) Uani 1 1 d . . . C4 C 0.2478(2) 0.2900(6) 0.1309(5) 0.047(2) Uani 1 1 d . . . O5 O 0.42219(16) 0.1125(4) 0.4053(5) 0.071(2) Uani 1 1 d . . . N4 N 0.15359(19) 0.0485(5) 0.1127(5) 0.0530(19) Uani 1 1 d . . . C5 C 0.2415(2) 0.2238(5) 0.1891(5) 0.047(2) Uani 1 1 d . . . H5 H 0.2246 0.1867 0.1740 0.056 Uiso 1 1 calc R . . O6 O 0.41409(15) 0.2801(4) 0.3681(4) 0.0620(18) Uani 1 1 d . . . N5 N 0.07709(18) 0.0889(6) -0.1045(5) 0.055(2) Uani 1 1 d . . . C6 C 0.2595(2) 0.2105(6) 0.2689(5) 0.049(2) Uani 1 1 d . . . O7 O 0.14095(16) 0.2447(5) 0.0322(4) 0.078(2) Uani 1 1 d . . . N6 N 0.0500(2) 0.2889(6) 0.0336(5) 0.067(2) Uani 1 1 d . . . C7 C 0.2522(2) 0.1313(6) 0.3243(6) 0.053(2) Uani 1 1 d . . . H7A H 0.2304 0.1184 0.3136 0.063 Uiso 1 1 calc R . . H7B H 0.2574 0.1459 0.3860 0.063 Uiso 1 1 calc R . . O8 O 0.39923(14) -0.2624(4) 0.3014(3) 0.0508(15) Uani 1 1 d . . . C8 C 0.2703(2) 0.0487(6) 0.3022(5) 0.046(2) Uani 1 1 d . . . O9 O 0.42000(14) 0.5487(4) 0.3488(3) 0.0502(15) Uani 1 1 d . . . C9 C 0.2596(2) 0.0059(5) 0.2227(5) 0.045(2) Uani 1 1 d . . . H9 H 0.2414 0.0257 0.1901 0.054 Uiso 1 1 calc R . . C10 C 0.2754(2) -0.0652(6) 0.1919(5) 0.049(2) Uani 1 1 d . . . O10 O 0.14616(14) 0.1081(4) 0.1647(4) 0.0516(15) Uani 1 1 d . . . C11 C 0.3018(2) -0.0944(6) 0.2426(5) 0.047(2) Uani 1 1 d . . . O11 O 0.17631(18) 0.0017(5) 0.1296(5) 0.083(2) Uani 1 1 d . . . C12 C 0.3124(2) -0.0536(5) 0.3207(5) 0.048(2) Uani 1 1 d . . . H12 H 0.3301 -0.0751 0.3539 0.057 Uiso 1 1 calc R . . O12 O 0.13599(15) 0.0385(4) 0.0418(4) 0.0588(17) Uani 1 1 d . . . C13 C 0.2971(2) 0.0184(6) 0.3506(5) 0.052(2) Uani 1 1 d . . . O13 O 0.07186(14) 0.0492(4) -0.0346(4) 0.0536(16) Uani 1 1 d . . . C14 C 0.3127(2) 0.0657(6) 0.4318(5) 0.052(2) Uani 1 1 d . . . H14A H 0.2976 0.1012 0.4576 0.063 Uiso 1 1 calc R . . H14B H 0.3209 0.0211 0.4747 0.063 Uiso 1 1 calc R . . O14 O 0.06837(16) 0.0553(5) -0.1757(4) 0.071(2) Uani 1 1 d . . . C15 C 0.3383(2) 0.1264(6) 0.4110(5) 0.051(2) Uani 1 1 d . . . O15 O 0.09136(18) 0.1618(5) -0.0944(4) 0.0676(19) Uani 1 1 d . . . C16 C 0.3676(2) 0.0904(6) 0.4179(5) 0.052(2) Uani 1 1 d . . . H16 H 0.3705 0.0304 0.4342 0.063 Uiso 1 1 calc R . . O18 O 0.07803(17) 0.3117(4) 0.0307(4) 0.0640(18) Uani 1 1 d . . . C17 C 0.3925(2) 0.1414(6) 0.4012(6) 0.052(2) Uani 1 1 d . . . O17 O 0.0291(2) 0.3438(5) 0.0239(7) 0.103(3) Uani 1 1 d . . . C18 C 0.3882(2) 0.2320(6) 0.3799(6) 0.054(2) Uani 1 1 d . . . O16 O 0.04558(14) 0.2077(4) 0.0477(4) 0.0565(16) Uani 1 1 d . . . C19 C 0.3589(2) 0.2667(6) 0.3705(5) 0.050(2) Uani 1 1 d . . . H19 H 0.3558 0.3261 0.3522 0.060 Uiso 1 1 calc R . . C20 C 0.3340(2) 0.2162(6) 0.3874(5) 0.050(2) Uani 1 1 d . . . C21 C 0.3034(2) 0.2654(6) 0.3810(5) 0.050(2) Uani 1 1 d . . . H21A H 0.2914 0.2381 0.4225 0.060 Uiso 1 1 calc R . . H21B H 0.3075 0.3271 0.3996 0.060 Uiso 1 1 calc R . . C22 C 0.3074(2) 0.4537(7) 0.1074(7) 0.065(3) Uani 1 1 d . . . H22A H 0.3071 0.4895 0.1594 0.098 Uiso 1 1 calc R . . H22B H 0.3096 0.4924 0.0586 0.098 Uiso 1 1 calc R . . H22C H 0.3243 0.4123 0.1160 0.098 Uiso 1 1 calc R . . C23 C 0.2006(2) 0.2633(6) 0.0439(6) 0.051(2) Uani 1 1 d . . . H23A H 0.1910 0.2687 0.0970 0.061 Uiso 1 1 calc R . . H23B H 0.2036 0.1999 0.0324 0.061 Uiso 1 1 calc R . . C24 C 0.1809(2) 0.3050(6) -0.0310(5) 0.046(2) Uani 1 1 d . . . C25 C 0.1911(2) 0.3563(5) -0.0967(6) 0.050(2) Uani 1 1 d . . . H25 H 0.2119 0.3674 -0.0963 0.060 Uiso 1 1 calc R . . C26 C 0.1703(2) 0.3905(6) -0.1617(6) 0.054(2) Uani 1 1 d . . . H26 H 0.1772 0.4225 -0.2074 0.065 Uiso 1 1 calc R . . C27 C 0.1396(3) 0.3784(7) -0.1610(6) 0.072(3) Uani 1 1 d . . . H27 H 0.1255 0.4030 -0.2050 0.086 Uiso 1 1 calc R . . C28 C 0.1300(3) 0.3297(7) -0.0943(7) 0.074(3) Uani 1 1 d . . . H28 H 0.1091 0.3221 -0.0922 0.088 Uiso 1 1 calc R . . C29 C 0.2433(2) -0.0622(7) 0.0556(6) 0.066(3) Uani 1 1 d . . . H29A H 0.2247 -0.0590 0.0819 0.098 Uiso 1 1 calc R . . H29B H 0.2396 -0.0951 0.0015 0.098 Uiso 1 1 calc R . . H29C H 0.2500 -0.0024 0.0441 0.098 Uiso 1 1 calc R . . C30 C 0.3459(2) -0.1878(6) 0.2470(6) 0.051(2) Uani 1 1 d . . . H30A H 0.3452 -0.2096 0.3063 0.061 Uiso 1 1 calc R . . H30B H 0.3591 -0.1353 0.2498 0.061 Uiso 1 1 calc R . . C31 C 0.3574(2) -0.2586(6) 0.1922(5) 0.052(2) Uani 1 1 d . . . C32 C 0.3427(2) -0.2902(6) 0.1139(6) 0.057(3) Uani 1 1 d . . . H32 H 0.3235 -0.2678 0.0914 0.068 Uiso 1 1 calc R . . C33 C 0.3564(2) -0.3548(6) 0.0694(6) 0.059(3) Uani 1 1 d . . . H33 H 0.3465 -0.3769 0.0163 0.071 Uiso 1 1 calc R . . C34 C 0.3847(2) -0.3872(6) 0.1030(6) 0.059(3) Uani 1 1 d . . . H34 H 0.3941 -0.4311 0.0725 0.071 Uiso 1 1 calc R . . C35 C 0.3992(2) -0.3552(6) 0.1811(6) 0.052(2) Uani 1 1 d . . . H35 H 0.4184 -0.3774 0.2039 0.063 Uiso 1 1 calc R . . C36 C 0.4273(3) 0.0191(7) 0.4217(8) 0.082(3) Uani 1 1 d . . . H36A H 0.4221 0.0043 0.4787 0.123 Uiso 1 1 calc R . . H36B H 0.4486 0.0054 0.4195 0.123 Uiso 1 1 calc R . . H36C H 0.4148 -0.0154 0.3778 0.123 Uiso 1 1 calc R . . C37 C 0.4112(2) 0.3750(6) 0.3605(6) 0.052(2) Uani 1 1 d . . . H37A H 0.4003 0.3989 0.4064 0.062 Uiso 1 1 calc R . . H37B H 0.4001 0.3913 0.3039 0.062 Uiso 1 1 calc R . . C38 C 0.4429(2) 0.4104(6) 0.3692(5) 0.047(2) Uani 1 1 d . . . C39 C 0.4688(2) 0.3607(7) 0.3809(7) 0.066(3) Uani 1 1 d . . . H39 H 0.4675 0.2986 0.3871 0.079 Uiso 1 1 calc R . . C40 C 0.4970(3) 0.4002(7) 0.3838(8) 0.079(3) Uani 1 1 d . . . H40 H 0.5148 0.3654 0.3921 0.095 Uiso 1 1 calc R . . C41 C 0.4989(2) 0.4900(7) 0.3745(7) 0.070(3) Uani 1 1 d . . . H41 H 0.5180 0.5177 0.3767 0.083 Uiso 1 1 calc R . . C42 C 0.4732(2) 0.5397(6) 0.3622(5) 0.059(3) Uani 1 1 d . . . H42 H 0.4745 0.6015 0.3539 0.071 Uiso 1 1 calc R . . N7A N 0.4436(2) -0.1631(6) 0.1630(5) 0.107(8) Uiso 0.50 1 d PR A 2 N7B N 0.4535(2) -0.1936(6) 0.1506(5) 0.105(8) Uiso 0.50 1 d PR B 1 O19A O 0.4046(5) -0.0750(15) 0.1803(14) 0.133(7) Uiso 0.50 1 d PD A 2 C44A C 0.4578(5) -0.2288(16) 0.0922(15) 0.188(9) Uiso 0.50 1 d P A 2 H44A H 0.4418 -0.2654 0.0623 0.282 Uiso 0.50 1 calc PR A 2 H44B H 0.4734 -0.2667 0.1228 0.282 Uiso 0.50 1 calc PR A 2 H44C H 0.4667 -0.1925 0.0502 0.282 Uiso 0.50 1 calc PR A 2 C45B C 0.4684(6) -0.2419(16) 0.2268(17) 0.096(8) Uiso 0.50 1 d PD B 1 H45B H 0.4657 -0.2174 0.2810 0.116 Uiso 0.50 1 calc PR B 1 C45A C 0.4623(8) -0.141(2) 0.240(2) 0.128(11) Uiso 0.50 1 d P A 2 H45A H 0.4512 -0.1033 0.2756 0.192 Uiso 0.50 1 calc PR A 2 H45C H 0.4801 -0.1092 0.2258 0.192 Uiso 0.50 1 calc PR A 2 H45D H 0.4687 -0.1949 0.2716 0.192 Uiso 0.50 1 calc PR A 2 C43A C 0.4227(6) -0.1235(17) 0.1425(16) 0.206(10) Uiso 0.50 1 d PD A 2 H43A H 0.4169 -0.1262 0.0820 0.248 Uiso 0.50 1 calc PR A 2 O19B O 0.4837(4) -0.3082(12) 0.2298(10) 0.085(5) Uiso 0.50 1 d PD . 1 C43B C 0.4227(6) -0.1235(17) 0.1425(16) 0.206(10) Uiso 0.50 1 d P B 1 H43B H 0.4128 -0.1229 0.0829 0.310 Uiso 0.50 1 calc PR B 1 H43C H 0.4295 -0.0638 0.1594 0.310 Uiso 0.50 1 calc PR B 1 H43D H 0.4085 -0.1442 0.1805 0.310 Uiso 0.50 1 calc PR B 1 C44B C 0.4578(5) -0.2288(16) 0.0922(15) 0.188(9) Uiso 0.50 1 d P B 1 H44D H 0.4785 -0.2173 0.0814 0.282 Uiso 0.50 1 calc PR B 1 H44E H 0.4438 -0.2081 0.0431 0.282 Uiso 0.50 1 calc PR B 1 H44F H 0.4551 -0.2922 0.1000 0.282 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 Gd1 0.0511(3) 0.0393(2) 0.0348(2) 0.0007(2) 0.00093(17) -0.0018(2) O1 0.059(4) 0.042(4) 0.060(4) 0.004(3) 0.001(3) -0.004(3) N1 0.062(6) 0.062(5) 0.050(4) 0.013(4) 0.004(4) -0.011(4) C1 0.059(6) 0.037(5) 0.047(5) -0.004(4) 0.003(4) 0.000(4) O2 0.059(4) 0.044(3) 0.052(4) 0.001(3) 0.009(3) -0.002(3) N2 0.071(5) 0.038(4) 0.037(4) 0.005(3) 0.009(4) -0.001(4) C2 0.051(5) 0.035(5) 0.053(5) -0.008(4) 0.006(4) -0.001(4) O3 0.067(4) 0.052(4) 0.046(3) -0.005(3) 0.003(3) 0.004(3) N3 0.062(5) 0.046(5) 0.036(4) -0.002(3) -0.001(3) 0.006(4) C3 0.058(6) 0.037(5) 0.051(5) 0.003(4) 0.017(4) 0.003(4) O4 0.064(4) 0.049(4) 0.053(4) -0.010(3) 0.001(3) 0.008(3) C4 0.057(6) 0.043(5) 0.041(5) -0.002(4) 0.002(4) 0.004(4) O5 0.069(5) 0.038(4) 0.105(6) 0.000(4) 0.005(4) 0.007(3) N4 0.063(6) 0.044(5) 0.052(5) 0.000(4) 0.005(4) -0.002(4) C5 0.053(6) 0.035(5) 0.053(5) -0.003(4) 0.007(4) -0.003(4) O6 0.066(5) 0.035(4) 0.086(5) -0.005(3) 0.013(4) 0.000(3) N5 0.060(5) 0.064(6) 0.042(4) 0.003(4) 0.005(4) 0.007(4) C6 0.060(6) 0.041(5) 0.045(5) -0.001(4) 0.002(4) 0.010(4) O7 0.074(5) 0.096(6) 0.060(4) 0.037(4) -0.003(4) -0.033(4) N6 0.083(7) 0.047(5) 0.069(6) -0.002(4) 0.002(5) 0.000(5) C7 0.064(7) 0.052(6) 0.043(5) 0.000(4) 0.012(4) -0.001(5) O8 0.068(4) 0.041(3) 0.041(3) 0.002(3) -0.001(3) 0.005(3) C8 0.057(6) 0.041(5) 0.042(5) 0.011(4) 0.010(4) 0.000(4) O9 0.059(4) 0.045(4) 0.045(3) -0.001(3) 0.000(3) 0.008(3) C9 0.058(6) 0.036(5) 0.044(5) 0.007(4) 0.011(4) -0.005(4) C10 0.069(7) 0.041(5) 0.038(5) 0.003(4) 0.008(4) -0.008(5) O10 0.060(4) 0.050(4) 0.043(3) -0.005(3) 0.002(3) 0.006(3) C11 0.057(6) 0.034(5) 0.050(5) 0.004(4) 0.012(4) 0.001(4) O11 0.077(5) 0.093(6) 0.075(5) 0.003(4) -0.004(4) 0.041(5) C12 0.067(6) 0.034(5) 0.042(5) 0.006(4) 0.005(4) -0.008(4) O12 0.062(4) 0.064(4) 0.049(4) -0.013(3) 0.002(3) 0.007(3) C13 0.069(7) 0.040(5) 0.046(5) -0.003(4) 0.007(4) -0.010(5) O13 0.063(4) 0.048(4) 0.047(3) -0.005(3) -0.001(3) -0.001(3) C14 0.070(7) 0.042(5) 0.043(5) 0.008(4) 0.001(4) -0.003(5) O14 0.080(5) 0.093(6) 0.037(3) -0.018(4) 0.000(3) -0.002(4) C15 0.072(7) 0.041(5) 0.038(5) -0.004(4) 0.003(4) -0.005(5) O15 0.092(6) 0.065(5) 0.046(4) 0.010(3) 0.009(3) -0.014(4) C16 0.063(7) 0.040(5) 0.052(5) 0.000(4) 0.004(5) 0.006(5) O18 0.067(5) 0.051(4) 0.072(5) 0.003(3) -0.001(4) -0.007(3) C17 0.059(6) 0.037(5) 0.056(5) -0.001(4) -0.003(5) 0.001(4) O17 0.089(7) 0.056(5) 0.164(9) 0.014(5) 0.017(6) 0.023(4) C18 0.068(7) 0.040(5) 0.052(5) -0.003(4) 0.004(5) 0.006(5) O16 0.067(4) 0.032(3) 0.068(4) -0.002(3) -0.001(3) -0.003(3) C19 0.063(6) 0.038(5) 0.048(5) -0.009(4) 0.003(4) 0.009(4) C20 0.063(6) 0.047(6) 0.039(5) -0.004(4) 0.003(4) -0.001(5) C21 0.063(6) 0.043(5) 0.043(5) -0.008(4) 0.007(4) -0.001(4) C22 0.061(7) 0.054(6) 0.079(7) 0.023(5) 0.006(5) -0.006(5) C23 0.055(6) 0.038(5) 0.058(6) 0.005(4) 0.006(4) 0.002(4) C24 0.048(6) 0.043(5) 0.048(5) -0.008(4) 0.005(4) -0.001(4) C25 0.063(6) 0.041(5) 0.047(5) 0.006(4) 0.013(5) -0.004(4) C26 0.068(7) 0.045(6) 0.051(5) 0.007(4) 0.014(5) -0.006(5) C27 0.084(9) 0.070(7) 0.055(6) 0.027(6) -0.010(5) -0.008(6) C28 0.064(7) 0.081(8) 0.072(7) 0.027(6) -0.006(5) -0.014(6) C29 0.064(7) 0.075(7) 0.054(6) -0.002(5) -0.005(5) 0.014(5) C30 0.062(6) 0.046(5) 0.043(5) 0.001(4) 0.004(4) 0.007(4) C31 0.066(6) 0.044(5) 0.042(5) 0.007(4) -0.004(4) 0.010(5) C32 0.071(7) 0.053(6) 0.045(5) 0.007(5) 0.000(5) 0.002(5) C33 0.076(7) 0.057(6) 0.044(5) 0.007(4) 0.004(5) 0.010(5) C34 0.082(8) 0.053(6) 0.045(5) -0.005(5) 0.014(5) 0.015(5) C35 0.061(6) 0.048(6) 0.047(5) -0.001(4) 0.004(4) 0.013(4) C36 0.101(9) 0.043(6) 0.104(9) 0.014(6) 0.017(7) 0.022(6) C37 0.059(6) 0.041(5) 0.056(5) -0.001(4) 0.013(5) 0.004(4) C38 0.059(6) 0.041(5) 0.041(5) 0.006(4) 0.005(4) 0.008(4) C39 0.065(7) 0.046(6) 0.085(7) 0.006(5) 0.008(6) 0.008(5) C40 0.059(7) 0.053(7) 0.122(10) 0.007(7) -0.002(6) 0.001(5) C41 0.055(7) 0.061(7) 0.091(8) 0.003(6) 0.003(5) -0.001(5) C42 0.069(7) 0.047(6) 0.061(6) 0.002(5) 0.008(5) -0.001(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 Gd1 O8 2.358(5) 4 ? Gd1 O7 2.370(6) . ? Gd1 O9 2.390(6) 4_545 ? Gd1 O16 2.505(6) . ? Gd1 O15 2.511(6) . ? Gd1 O18 2.517(7) . ? Gd1 O12 2.539(6) . ? Gd1 O13 2.539(6) . ? Gd1 O10 2.550(6) . ? Gd1 N6 2.946(10) . ? Gd1 N5 2.958(8) . ? Gd1 N4 2.972(8) . ? O1 C3 1.395(10) . ? O1 C22 1.452(11) . ? N1 O7 1.357(9) . ? N1 C28 1.359(13) . ? N1 C24 1.388(11) . ? C1 C6 1.411(13) . ? C1 C2 1.430(12) . ? C1 C21 1.536(11) . ? O2 C4 1.394(10) . ? O2 C23 1.453(11) . ? N2 C35 1.359(11) . ? N2 O8 1.357(9) . ? N2 C31 1.397(11) . ? C2 C3 1.397(12) . ? C2 H2 0.9500 . ? O3 C10 1.375(10) . ? O3 C29 1.478(11) . ? N3 O9 1.349(9) . ? N3 C38 1.367(11) . ? N3 C42 1.389(11) . ? C3 C4 1.419(13) . ? O4 C11 1.424(10) . ? O4 C30 1.434(11) . ? C4 C5 1.410(12) . ? O5 C17 1.395(11) . ? O5 C36 1.452(11) . ? N4 O11 1.241(10) . ? N4 O12 1.284(9) . ? N4 O10 1.291(9) . ? C5 C6 1.410(12) . ? C5 H5 0.9500 . ? O6 C18 1.406(11) . ? O6 C37 1.448(11) . ? N5 O14 1.242(9) . ? N5 O15 1.277(10) . ? N5 O13 1.299(9) . ? C6 C7 1.543(13) . ? N6 O17 1.247(11) . ? N6 O16 1.272(10) . ? N6 O18 1.310(11) . ? C7 C8 1.555(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O8 Gd1 2.358(5) 4_545 ? C8 C13 1.414(13) . ? C8 C9 1.431(12) . ? O9 Gd1 2.390(6) 4 ? C9 C10 1.410(12) . ? C9 H9 0.9500 . ? C10 C11 1.409(12) . ? C11 C12 1.397(12) . ? C12 C13 1.403(12) . ? C12 H12 0.9500 . ? C13 C14 1.545(12) . ? C14 C15 1.541(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.412(13) . ? C15 C20 1.418(13) . ? C16 C17 1.414(13) . ? C16 H16 0.9500 . ? C17 C18 1.422(12) . ? C18 C19 1.403(13) . ? C19 C20 1.410(13) . ? C19 H19 0.9500 . ? C20 C21 1.551(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.511(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.412(12) . ? C25 C26 1.388(13) . ? C25 H25 0.9500 . ? C26 C27 1.391(14) . ? C26 H26 0.9500 . ? C27 C28 1.393(14) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.508(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.400(12) . ? C32 C33 1.392(13) . ? C32 H32 0.9500 . ? C33 C34 1.398(13) . ? C33 H33 0.9500 . ? C34 C35 1.395(13) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.508(13) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.379(13) . ? C39 C40 1.395(15) . ? C39 H39 0.9500 . ? C40 C41 1.373(14) . ? C40 H40 0.9500 . ? C41 C42 1.368(13) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? N7A C43A 1.12(3) . ? N7A C45A 1.42(3) . ? N7A C44A 1.68(2) . ? N7B C45B 1.48(3) . ? O19A C43A 1.296(17) . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C45B O19B 1.214(17) . ? C45B H45B 0.9500 . ? C45A H45A 0.9800 . ? C45A H45C 0.9800 . ? C45A H45D 0.9800 . ? C43A H43A 0.9500 . ? O19B O19B 1.52(3) 2_655 ? 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 O8 Gd1 O7 90.6(2) 4 . ? O8 Gd1 O9 80.63(19) 4 4_545 ? O7 Gd1 O9 149.9(2) . 4_545 ? O8 Gd1 O16 83.0(2) 4 . ? O7 Gd1 O16 126.5(2) . . ? O9 Gd1 O16 81.3(2) 4_545 . ? O8 Gd1 O15 149.6(2) 4 . ? O7 Gd1 O15 77.3(2) . . ? O9 Gd1 O15 122.8(2) 4_545 . ? O16 Gd1 O15 82.2(2) . . ? O8 Gd1 O18 73.5(2) 4 . ? O7 Gd1 O18 75.6(3) . . ? O9 Gd1 O18 127.9(2) 4_545 . ? O16 Gd1 O18 51.6(2) . . ? O15 Gd1 O18 76.4(2) . . ? O8 Gd1 O12 123.8(2) 4 . ? O7 Gd1 O12 79.5(3) . . ? O9 Gd1 O12 81.7(2) 4_545 . ? O16 Gd1 O12 145.0(2) . . ? O15 Gd1 O12 81.8(2) . . ? O18 Gd1 O12 149.8(2) . . ? O8 Gd1 O13 146.1(2) 4 . ? O7 Gd1 O13 123.1(2) . . ? O9 Gd1 O13 71.61(19) 4_545 . ? O16 Gd1 O13 74.04(19) . . ? O15 Gd1 O13 51.2(2) . . ? O18 Gd1 O13 108.7(2) . . ? O12 Gd1 O13 71.6(2) . . ? O8 Gd1 O10 73.09(19) 4 . ? O7 Gd1 O10 72.7(2) . . ? O9 Gd1 O10 77.1(2) 4_545 . ? O16 Gd1 O10 149.88(19) . . ? O15 Gd1 O10 127.3(2) . . ? O18 Gd1 O10 133.0(2) . . ? O12 Gd1 O10 51.01(19) . . ? O13 Gd1 O10 117.48(19) . . ? O8 Gd1 N6 76.2(2) 4 . ? O7 Gd1 N6 101.7(3) . . ? O9 Gd1 N6 104.1(2) 4_545 . ? O16 Gd1 N6 25.4(2) . . ? O15 Gd1 N6 79.0(2) . . ? O18 Gd1 N6 26.3(2) . . ? O12 Gd1 N6 160.0(2) . . ? O13 Gd1 N6 91.8(2) . . ? O10 Gd1 N6 148.7(2) . . ? O8 Gd1 N5 160.5(2) 4 . ? O7 Gd1 N5 99.9(2) . . ? O9 Gd1 N5 97.5(2) 4_545 . ? O16 Gd1 N5 77.5(2) . . ? O15 Gd1 N5 25.3(2) . . ? O18 Gd1 N5 93.1(2) . . ? O12 Gd1 N5 74.7(2) . . ? O13 Gd1 N5 25.9(2) . . ? O10 Gd1 N5 125.7(2) . . ? N6 Gd1 N5 85.5(2) . . ? O8 Gd1 N4 98.6(2) 4 . ? O7 Gd1 N4 74.1(2) . . ? O9 Gd1 N4 78.8(2) 4_545 . ? O16 Gd1 N4 159.4(2) . . ? O15 Gd1 N4 104.6(2) . . ? O18 Gd1 N4 148.5(2) . . ? O12 Gd1 N4 25.42(18) . . ? O13 Gd1 N4 94.8(2) . . ? O10 Gd1 N4 25.60(18) . . ? N6 Gd1 N4 173.4(2) . . ? N5 Gd1 N4 100.1(2) . . ? C3 O1 C22 116.4(7) . . ? O7 N1 C28 120.8(8) . . ? O7 N1 C24 117.4(7) . . ? C28 N1 C24 121.8(8) . . ? C6 C1 C2 118.5(8) . . ? C6 C1 C21 123.8(8) . . ? C2 C1 C21 117.7(8) . . ? C4 O2 C23 114.6(6) . . ? C35 N2 O8 120.1(7) . . ? C35 N2 C31 121.4(7) . . ? O8 N2 C31 118.5(7) . . ? C3 C2 C1 122.4(8) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C10 O3 C29 115.5(7) . . ? O9 N3 C38 118.9(7) . . ? O9 N3 C42 120.1(7) . . ? C38 N3 C42 120.9(8) . . ? O1 C3 C2 125.0(8) . . ? O1 C3 C4 116.1(8) . . ? C2 C3 C4 118.9(8) . . ? C11 O4 C30 116.4(6) . . ? O2 C4 C5 123.9(8) . . ? O2 C4 C3 117.2(7) . . ? C5 C4 C3 118.8(8) . . ? C17 O5 C36 116.3(8) . . ? O11 N4 O12 120.8(8) . . ? O11 N4 O10 122.5(8) . . ? O12 N4 O10 116.7(7) . . ? O11 N4 Gd1 178.5(6) . . ? O12 N4 Gd1 58.1(4) . . ? O10 N4 Gd1 58.6(4) . . ? C6 C5 C4 122.5(8) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C18 O6 C37 117.3(7) . . ? O14 N5 O15 124.1(8) . . ? O14 N5 O13 119.9(8) . . ? O15 N5 O13 116.0(7) . . ? O14 N5 Gd1 177.2(7) . . ? O15 N5 Gd1 57.4(4) . . ? O13 N5 Gd1 58.7(4) . . ? C5 C6 C1 118.8(8) . . ? C5 C6 C7 118.2(8) . . ? C1 C6 C7 122.9(8) . . ? N1 O7 Gd1 141.9(5) . . ? O17 N6 O16 122.4(10) . . ? O17 N6 O18 121.9(9) . . ? O16 N6 O18 115.7(9) . . ? O17 N6 Gd1 176.8(8) . . ? O16 N6 Gd1 57.5(5) . . ? O18 N6 Gd1 58.2(5) . . ? C6 C7 C8 110.2(7) . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N2 O8 Gd1 124.6(5) . 4_545 ? C13 C8 C9 119.0(8) . . ? C13 C8 C7 125.1(8) . . ? C9 C8 C7 115.8(8) . . ? N3 O9 Gd1 132.3(5) . 4 ? C10 C9 C8 121.3(8) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? O3 C10 C11 117.9(8) . . ? O3 C10 C9 124.0(8) . . ? C11 C10 C9 118.0(8) . . ? N4 O10 Gd1 95.8(5) . . ? C12 C11 C10 121.3(8) . . ? C12 C11 O4 124.4(8) . . ? C10 C11 O4 114.2(7) . . ? C11 C12 C13 120.8(9) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N4 O12 Gd1 96.5(5) . . ? C12 C13 C8 119.5(8) . . ? C12 C13 C14 116.7(8) . . ? C8 C13 C14 123.5(8) . . ? N5 O13 Gd1 95.4(5) . . ? C15 C14 C13 111.8(7) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 119.0(9) . . ? C16 C15 C14 117.7(8) . . ? C20 C15 C14 123.2(9) . . ? N5 O15 Gd1 97.3(5) . . ? C15 C16 C17 121.7(9) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? N6 O18 Gd1 95.5(5) . . ? O5 C17 C16 126.5(8) . . ? O5 C17 C18 114.6(8) . . ? C16 C17 C18 118.9(9) . . ? O6 C18 C19 124.8(8) . . ? O6 C18 C17 116.2(8) . . ? C19 C18 C17 119.1(9) . . ? N6 O16 Gd1 97.1(6) . . ? C18 C19 C20 122.1(9) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 119.1(9) . . ? C19 C20 C21 116.3(8) . . ? C15 C20 C21 124.7(8) . . ? C1 C21 C20 117.2(7) . . ? C1 C21 H21A 108.0 . . ? C20 C21 H21A 108.0 . . ? C1 C21 H21B 108.0 . . ? C20 C21 H21B 108.0 . . ? H21A C21 H21B 107.2 . . ? O1 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O2 C23 C24 108.0(7) . . ? O2 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O2 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? N1 C24 C25 118.3(8) . . ? N1 C24 C23 115.8(8) . . ? C25 C24 C23 125.8(8) . . ? C26 C25 C24 119.5(9) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.9(9) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 118.7(9) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? N1 C28 C27 120.6(10) . . ? N1 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? O3 C29 H29A 109.5 . . ? O3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O4 C30 C31 106.0(7) . . ? O4 C30 H30A 110.5 . . ? C31 C30 H30A 110.5 . . ? O4 C30 H30B 110.5 . . ? C31 C30 H30B 110.5 . . ? H30A C30 H30B 108.7 . . ? N2 C31 C32 119.5(8) . . ? N2 C31 C30 114.6(7) . . ? C32 C31 C30 125.9(8) . . ? C33 C32 C31 119.5(9) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 119.8(9) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 120.3(9) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? N2 C35 C34 119.6(9) . . ? N2 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? O5 C36 H36A 109.5 . . ? O5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6 C37 C38 105.8(7) . . ? O6 C37 H37A 110.6 . . ? C38 C37 H37A 110.6 . . ? O6 C37 H37B 110.6 . . ? C38 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? N3 C38 C39 118.5(9) . . ? N3 C38 C37 115.5(8) . . ? C39 C38 C37 125.9(9) . . ? C38 C39 C40 121.1(10) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 119.3(10) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C40 C41 C42 119.9(10) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 N3 120.2(9) . . ? C41 C42 H42 119.9 . . ? N3 C42 H42 119.9 . . ? C43A N7A C45A 120(2) . . ? C43A N7A C44A 120.2(16) . . ? C45A N7A C44A 117.9(17) . . ? N7A C44A H44A 109.5 . . ? N7A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? N7A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? O19B C45B N7B 129(2) . . ? O19B C45B H45B 115.4 . . ? N7B C45B H45B 115.4 . . ? N7A C45A H45A 109.5 . . ? N7A C45A H45C 109.5 . . ? H45A C45A H45C 109.5 . . ? N7A C45A H45D 109.5 . . ? H45A C45A H45D 109.5 . . ? H45C C45A H45D 109.5 . . ? O19A C43A N7A 136(3) . . ? O19A C43A H43A 111.9 . . ? N7A C43A H43A 111.9 . . ? C45B O19B O19B 121.6(16) . 2_655 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.280 _refine_diff_density_min -1.536 _refine_diff_density_rms 0.232 _database_code_depnum_ccdc_archive 'CCDC 936737' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c: _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Chlorotrisdimethylformamide{(+-)-2,7,12-trimethoxy- 3,8,13-tris(4-N-oxide-pyridyloxy)-10,15-dihydro-5H- tribenzo[a,d,g]cyclononatriene}samarium(III) pentachlorodimethylformamidesamariumate(III) dimethylformamide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61.50 H78.50 Cl6 N9.50 O18.50 Sm2' _chemical_formula_weight 1760.24 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' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7326(12) _cell_length_b 16.1047(13) _cell_length_c 19.7002(17) _cell_angle_alpha 103.648(2) _cell_angle_beta 91.582(3) _cell_angle_gamma 94.159(3) _cell_volume 3911.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 1.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6774 _exptl_absorpt_correction_T_max 0.8035 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER X8 CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61774 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.28 _reflns_number_total 17431 _reflns_number_gt 12627 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Two methyl groups of ligand 2 were refined as being disordered across two positions, one with OMe in two positions each at 50% occupancy, and the other with the CH3 group across two positions at 75:25 occupancy. The coordinated DMF of the [SmCl5.(DMF)] was refined as disordered across two positions each at 50% occupancy. Two uncoordinated solvent DMF molecules were refined isotropically and one shows a symmetry-related disorder and was refined at 50% occupancy. Some bond lengths of this DMF were restrained to be chemically reasonable ; _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^)+(0.0748P)^2^+8.2961P] 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 17431 _refine_ls_number_parameters 933 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.038 _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 Sm1 Sm 0.35522(2) 0.413374(16) 0.687637(14) 0.03056(8) Uani 1 1 d . . . Cl1 Cl 0.30778(17) 0.43211(12) 0.55413(10) 0.0647(5) Uani 1 1 d . A 1 O1 O 0.4239(3) 0.1284(3) 1.0907(2) 0.0458(10) Uani 1 1 d . . . N1 N 0.3642(4) 0.3032(3) 0.8187(3) 0.0465(12) Uani 1 1 d . . . C1 C 0.7173(4) -0.0251(4) 1.1613(3) 0.0378(12) Uani 1 1 d . . . H1A H 0.7612 -0.0687 1.1346 0.045 Uiso 1 1 calc R . . H1B H 0.6585 -0.0558 1.1796 0.045 Uiso 1 1 calc R . . Sm2 Sm 0.73750(2) 0.083148(18) 0.717584(15) 0.03585(9) Uani 1 1 d . . . Cl2 Cl 0.69437(17) 0.24823(11) 0.73647(10) 0.0626(5) Uani 1 1 d . B 1 O2 O 0.5283(3) 0.1496(3) 0.9747(2) 0.0408(9) Uani 1 1 d . . . N2 N 1.4419(4) 0.5011(3) 1.1962(3) 0.0415(11) Uani 1 1 d . . . C2 C 0.6720(4) 0.0237(3) 1.1118(3) 0.0342(12) Uani 1 1 d . . . Cl3 Cl 0.78720(16) 0.12184(13) 0.85463(9) 0.0635(5) Uani 1 1 d . B 1 O3 O 0.5382(4) 0.2822(3) 1.0462(2) 0.0595(13) Uani 1 1 d . . . N3 N 0.5758(4) 0.3664(3) 1.5898(3) 0.0434(12) Uani 1 1 d . . . C3 C 0.5716(4) 0.0547(4) 1.1254(3) 0.0366(12) Uani 1 1 d . . . H3 H 0.5362 0.0446 1.1648 0.044 Uiso 1 1 calc R . . Cl4 Cl 0.53031(12) 0.03693(12) 0.71892(9) 0.0528(4) Uani 1 1 d . B . O4 O 0.3127(4) 0.3236(3) 0.7660(2) 0.0510(11) Uani 1 1 d . A . N4 N 0.2075(4) 0.6492(3) 0.8193(3) 0.0501(13) Uani 1 1 d . A . C4 C 0.5235(4) 0.0994(4) 1.0825(3) 0.0377(13) Uani 1 1 d . . . Cl5 Cl 0.77000(13) -0.08303(10) 0.70349(9) 0.0504(4) Uani 1 1 d . B 1 O5 O 1.0676(4) 0.2565(3) 1.0122(3) 0.0631(13) Uani 1 1 d . . . N5 N 0.0014(5) 0.3182(5) 0.6390(5) 0.079(2) Uani 1 1 d . A . C5 C 0.5773(4) 0.1143(4) 1.0255(3) 0.0370(12) Uani 1 1 d . . . Cl6 Cl 0.74904(14) 0.06857(11) 0.57721(8) 0.0513(4) Uani 1 1 d . B . O6 O 1.1817(3) 0.2507(3) 1.1280(2) 0.0485(11) Uani 1 1 d . D . N6 N 0.4048(5) 0.1568(3) 0.5287(3) 0.0539(14) Uani 1 1 d . A . C6 C 0.6761(4) 0.0853(3) 1.0111(3) 0.0344(12) Uani 1 1 d . . . H6 H 0.7113 0.0972 0.9722 0.041 Uiso 1 1 calc R . . O7 O 1.0752(3) 0.3566(3) 1.1677(3) 0.0670(15) Uani 1 1 d . D . N7 N 0.5507(7) 0.6765(5) 0.6939(4) 0.092(3) Uani 1 1 d . A . C7 C 0.7246(4) 0.0390(3) 1.0532(3) 0.0336(12) Uani 1 1 d . . . O8 O 1.5277(3) 0.5543(3) 1.2084(2) 0.0411(9) Uani 1 1 d . . . C8 C 0.8297(4) 0.0043(4) 1.0302(3) 0.0379(13) Uani 1 1 d . . . H8A H 0.8295 -0.0106 0.9785 0.045 Uiso 1 1 calc R . . H8B H 0.8374 -0.0489 1.0462 0.045 Uiso 1 1 calc R . . N9 N 0.9509(9) 0.5509(9) 0.6017(6) 0.070(4) Uiso 0.50 1 d PD . . C9 C 0.9252(4) 0.0691(4) 1.0594(3) 0.0362(12) Uani 1 1 d . D . O10 O 0.7306(4) 0.1673(3) 1.3969(2) 0.0494(11) Uani 1 1 d . . . N10 N 0.8108(9) 0.4261(7) 0.9305(6) 0.116(3) Uiso 1 1 d . . . C10 C 0.9512(4) 0.1316(4) 1.0222(3) 0.0396(13) Uani 1 1 d . . . H10 H 0.9109 0.1319 0.9809 0.048 Uiso 1 1 calc R D . O11 O 0.7587(4) 0.2932(3) 1.3649(3) 0.0667(14) Uani 1 1 d . . . C11 C 1.0356(5) 0.1936(4) 1.0450(3) 0.0435(14) Uani 1 1 d . D . O12 O 0.5314(3) 0.4051(3) 1.6479(2) 0.0500(11) Uani 1 1 d . . . C12 C 1.0919(4) 0.1905(4) 1.1062(3) 0.0441(15) Uani 1 1 d . . . O13 O 0.2551(4) 0.5191(3) 0.7622(3) 0.0592(13) Uani 1 1 d . A . C13 C 1.0692(4) 0.1299(4) 1.1425(3) 0.0395(13) Uani 1 1 d . D . H13 H 1.1106 0.1300 1.1834 0.047 Uiso 1 1 calc R . . O14 O 0.1716(4) 0.3611(3) 0.6699(3) 0.0593(13) Uani 1 1 d . A . C14 C 0.9843(4) 0.0665(4) 1.1199(3) 0.0350(12) Uani 1 1 d . . . O15 O 0.3643(4) 0.2661(3) 0.6186(2) 0.0496(11) Uani 1 1 d . A . C15 C 0.9613(5) 0.0030(4) 1.1641(3) 0.0415(14) Uani 1 1 d . D . H15A H 1.0285 -0.0129 1.1821 0.050 Uiso 1 1 calc R . . H15B H 0.9232 -0.0497 1.1349 0.050 Uiso 1 1 calc R . . O16 O 0.4364(4) 0.5621(3) 0.6951(3) 0.0531(11) Uani 1 1 d . A . C16 C 0.8942(5) 0.0414(4) 1.2258(3) 0.0418(13) Uani 1 1 d . . . O17 O 0.9241(4) 0.1121(4) 0.7092(3) 0.0662(16) Uani 1 1 d . B . C17 C 0.9481(5) 0.0926(5) 1.2860(4) 0.063(2) Uani 1 1 d . C . H17 H 1.0230 0.0982 1.2879 0.076 Uiso 1 1 calc R . . O18 O 0.8025(9) 0.4869(7) 0.6316(6) 0.068(3) Uiso 0.50 1 d PD . . C18 C 0.8954(6) 0.1352(6) 1.3426(4) 0.069(2) Uani 1 1 d . . . O19 O 0.7987(13) 0.5416(10) 1.0085(9) 0.230(6) Uiso 1 1 d . . . C19 C 0.7863(5) 0.1254(4) 1.3382(3) 0.0482(15) Uani 1 1 d . C . C20 C 0.7317(5) 0.0748(4) 1.2812(3) 0.0416(13) Uani 1 1 d . . . H20 H 0.6569 0.0687 1.2805 0.050 Uiso 1 1 calc R C . C21 C 0.7846(4) 0.0313(4) 1.2234(3) 0.0367(12) Uani 1 1 d . C . C22 C 0.3588(5) 0.0931(4) 1.1371(3) 0.0454(14) Uani 1 1 d . . . H22A H 0.3569 0.0304 1.1238 0.068 Uiso 1 1 calc R . . H22B H 0.2872 0.1109 1.1340 0.068 Uiso 1 1 calc R . . H22C H 0.3879 0.1140 1.1852 0.068 Uiso 1 1 calc R . . C23 C 0.5132(5) 0.2329(4) 0.9908(3) 0.0422(14) Uani 1 1 d . . . C24 C 0.4612(5) 0.2571(4) 0.9293(3) 0.0432(14) Uani 1 1 d . A . C25 C 0.3968(8) 0.3251(5) 0.9400(4) 0.077(3) Uani 1 1 d . . . H25 H 0.3872 0.3571 0.9862 0.093 Uiso 1 1 calc R A . C26 C 0.3475(7) 0.3459(6) 0.8846(4) 0.076(3) Uani 1 1 d . A . H26 H 0.3014 0.3907 0.8925 0.091 Uiso 1 1 calc R . . C27 C 0.4284(5) 0.2412(4) 0.8066(3) 0.0496(15) Uani 1 1 d . A . H27 H 0.4413 0.2137 0.7597 0.060 Uiso 1 1 calc R . . C28 C 0.4773(5) 0.2154(4) 0.8609(3) 0.0454(14) Uani 1 1 d . . . H28 H 0.5217 0.1695 0.8514 0.055 Uiso 1 1 calc R A . C30 C 1.1625(5) 0.3330(4) 1.1555(3) 0.0484(16) Uani 1 1 d . . . C31 C 1.2614(5) 0.3899(4) 1.1691(3) 0.0426(14) Uani 1 1 d . D . C32 C 1.2573(5) 0.4747(4) 1.2056(4) 0.0515(16) Uani 1 1 d . . . H32 H 1.1919 0.4947 1.2217 0.062 Uiso 1 1 calc R D . C33 C 1.3479(5) 0.5304(4) 1.2187(3) 0.0484(15) Uani 1 1 d . D . H33 H 1.3446 0.5885 1.2432 0.058 Uiso 1 1 calc R . . C34 C 1.4478(5) 0.4191(4) 1.1594(3) 0.0421(14) Uani 1 1 d . D . H34 H 1.5136 0.4004 1.1431 0.051 Uiso 1 1 calc R . . C35 C 1.3580(4) 0.3623(4) 1.1454(3) 0.0406(13) Uani 1 1 d . . . H35 H 1.3625 0.3049 1.1197 0.049 Uiso 1 1 calc R D . C37 C 0.7251(5) 0.2526(4) 1.4050(3) 0.0470(15) Uani 1 1 d . . . C38 C 0.6727(4) 0.2910(4) 1.4709(3) 0.0395(13) Uani 1 1 d . . . C39 C 0.6322(6) 0.3706(4) 1.4767(3) 0.0512(16) Uani 1 1 d . . . H39 H 0.6391 0.3991 1.4399 0.061 Uiso 1 1 calc R . . C40 C 0.5829(6) 0.4071(4) 1.5357(4) 0.0516(16) Uani 1 1 d . . . H40 H 0.5534 0.4604 1.5395 0.062 Uiso 1 1 calc R . . C41 C 0.6139(5) 0.2916(4) 1.5853(3) 0.0432(14) Uani 1 1 d . . . H41 H 0.6081 0.2650 1.6234 0.052 Uiso 1 1 calc R . . C42 C 0.6629(5) 0.2506(4) 1.5251(3) 0.0421(13) Uani 1 1 d . . . H42 H 0.6889 0.1961 1.5217 0.050 Uiso 1 1 calc R . . C43 C 0.2391(5) 0.5946(4) 0.7647(4) 0.0525(16) Uani 1 1 d . . . H43 H 0.2507 0.6147 0.7237 0.063 Uiso 1 1 calc R A . C44 C 0.1887(8) 0.6261(6) 0.8847(4) 0.081(3) Uani 1 1 d . . . H44A H 0.2072 0.5673 0.8813 0.122 Uiso 1 1 calc R A . H44B H 0.1141 0.6300 0.8949 0.122 Uiso 1 1 calc R . . H44C H 0.2321 0.6654 0.9224 0.122 Uiso 1 1 calc R . . C45 C 0.1906(7) 0.7384(4) 0.8182(4) 0.068(2) Uani 1 1 d . . . H45A H 0.2086 0.7485 0.7726 0.102 Uiso 1 1 calc R A . H45B H 0.2354 0.7777 0.8551 0.102 Uiso 1 1 calc R . . H45C H 0.1165 0.7485 0.8263 0.102 Uiso 1 1 calc R . . C46 C 0.1034(7) 0.3333(6) 0.6288(6) 0.079(2) Uani 1 1 d . . . H46 H 0.1228 0.3193 0.5815 0.095 Uiso 1 1 calc R A . C47 C -0.0348(10) 0.3375(7) 0.7077(8) 0.124(5) Uani 1 1 d . . . H47A H -0.0608 0.2843 0.7199 0.186 Uiso 1 1 calc R A . H47B H -0.0919 0.3755 0.7104 0.186 Uiso 1 1 calc R . . H47C H 0.0234 0.3659 0.7405 0.186 Uiso 1 1 calc R . . C48 C -0.0725(9) 0.2782(8) 0.5822(8) 0.139(5) Uani 1 1 d . . . H48A H -0.0998 0.3221 0.5611 0.209 Uiso 1 1 calc R A . H48B H -0.1309 0.2475 0.5998 0.209 Uiso 1 1 calc R . . H48C H -0.0370 0.2376 0.5469 0.209 Uiso 1 1 calc R . . C49 C 0.3717(6) 0.2338(5) 0.5537(4) 0.0587(18) Uani 1 1 d . . . H49 H 0.3525 0.2663 0.5215 0.070 Uiso 1 1 calc R A . C50 C 0.4204(8) 0.1257(6) 0.4514(4) 0.085(3) Uani 1 1 d . . . H50A H 0.4100 0.1721 0.4281 0.127 Uiso 1 1 calc R A . H50B H 0.3693 0.0769 0.4316 0.127 Uiso 1 1 calc R . . H50C H 0.4921 0.1078 0.4444 0.127 Uiso 1 1 calc R . . C51 C 0.4366(7) 0.1013(5) 0.5704(4) 0.070(2) Uani 1 1 d . . . H51A H 0.4292 0.1285 0.6199 0.105 Uiso 1 1 calc R A . H51B H 0.5104 0.0899 0.5625 0.105 Uiso 1 1 calc R . . H51C H 0.3922 0.0472 0.5577 0.105 Uiso 1 1 calc R . . C52 C 0.5228(8) 0.5930(5) 0.6810(4) 0.072(2) Uani 1 1 d . . . H52 H 0.5721 0.5545 0.6597 0.087 Uiso 1 1 calc R A . C53 C 0.6649(11) 0.7052(8) 0.6822(8) 0.150(6) Uani 1 1 d . . . H53A H 0.7072 0.7145 0.7260 0.225 Uiso 1 1 calc R A . H53B H 0.6664 0.7588 0.6666 0.225 Uiso 1 1 calc R . . H53C H 0.6939 0.6608 0.6464 0.225 Uiso 1 1 calc R . . C54 C 0.4833(10) 0.7397(6) 0.7272(9) 0.149(7) Uani 1 1 d . . . H54A H 0.4109 0.7235 0.7079 0.224 Uiso 1 1 calc R A . H54B H 0.5075 0.7955 0.7190 0.224 Uiso 1 1 calc R . . H54C H 0.4852 0.7433 0.7776 0.224 Uiso 1 1 calc R . . C58 C 0.8433(9) 0.5206(7) 0.5966(6) 0.041(3) Uiso 0.50 1 d PD . . H58 H 0.8020 0.5307 0.5589 0.049 Uiso 0.50 1 calc PR . . C59 C 1.0089(9) 0.5630(7) 0.6672(6) 0.038(3) Uiso 0.50 1 d PD . . H59A H 1.0813 0.5854 0.6627 0.058 Uiso 0.50 1 calc PR . . H59B H 1.0097 0.5080 0.6803 0.058 Uiso 0.50 1 calc PR . . H59C H 0.9752 0.6039 0.7033 0.058 Uiso 0.50 1 calc PR . . C60 C 1.0208(18) 0.5483(15) 0.5397(10) 0.109(7) Uiso 0.50 1 d PD . . H60A H 1.0920 0.5729 0.5567 0.164 Uiso 0.50 1 calc PR . . H60B H 0.9914 0.5816 0.5090 0.164 Uiso 0.50 1 calc PR . . H60C H 1.0237 0.4888 0.5135 0.164 Uiso 0.50 1 calc PR . . C61 C 0.8550(14) 0.5041(11) 0.9679(9) 0.150(6) Uiso 1 1 d . . . H61 H 0.9245 0.5259 0.9616 0.180 Uiso 1 1 calc R . . C62 C 0.8880(16) 0.3869(13) 0.8765(11) 0.209(8) Uiso 1 1 d . . . H62A H 0.8576 0.3823 0.8294 0.314 Uiso 1 1 calc R . . H62B H 0.9016 0.3297 0.8821 0.314 Uiso 1 1 calc R . . H62C H 0.9542 0.4234 0.8834 0.314 Uiso 1 1 calc R . . C63 C 0.7090(14) 0.3924(11) 0.9352(9) 0.177(7) Uiso 1 1 d . . . H63A H 0.7101 0.3482 0.9618 0.265 Uiso 1 1 calc R . . H63B H 0.6781 0.3669 0.8881 0.265 Uiso 1 1 calc R . . H63C H 0.6666 0.4381 0.9588 0.265 Uiso 1 1 calc R . . N8A N 1.0855(14) 0.0909(11) 0.6489(8) 0.058(4) Uani 0.50 1 d P B 1 O9A O 0.9472(10) 0.2060(9) 1.3976(6) 0.053(3) Uani 0.50 1 d P C 1 C29A C 1.0120(12) 0.2586(8) 0.9539(7) 0.082(4) Uani 0.75 1 d P D 1 H29A H 1.0205 0.2064 0.9177 0.123 Uiso 0.75 1 calc PR D 1 H29B H 1.0376 0.3089 0.9373 0.123 Uiso 0.75 1 calc PR D 1 H29C H 0.9373 0.2620 0.9640 0.123 Uiso 0.75 1 calc PR D 1 C36A C 1.0628(11) 0.2261(13) 1.3960(9) 0.080(6) Uani 0.50 1 d P C 1 H36A H 1.0906 0.1863 1.3563 0.120 Uiso 0.50 1 calc PR C 1 H36B H 1.0971 0.2204 1.4396 0.120 Uiso 0.50 1 calc PR C 1 H36C H 1.0768 0.2850 1.3910 0.120 Uiso 0.50 1 calc PR C 1 C55A C 0.9843(15) 0.0757(13) 0.6555(11) 0.048(4) Uani 0.50 1 d P B 1 H55A H 0.9482 0.0341 0.6182 0.057 Uiso 0.50 1 calc PR B 1 C56A C 1.1417(18) 0.0473(18) 0.5891(12) 0.099(8) Uani 0.50 1 d P B 1 H56A H 1.1868 0.0070 0.6034 0.148 Uiso 0.50 1 calc PR B 1 H56B H 1.1854 0.0896 0.5715 0.148 Uiso 0.50 1 calc PR B 1 H56C H 1.0908 0.0158 0.5520 0.148 Uiso 0.50 1 calc PR B 1 C57A C 1.1425(18) 0.1484(13) 0.7092(14) 0.069(6) Uani 0.50 1 d P B 1 H57D H 1.0997 0.1536 0.7504 0.103 Uiso 0.50 1 calc PR B 1 H57E H 1.1570 0.2050 0.6996 0.103 Uiso 0.50 1 calc PR B 1 H57F H 1.2092 0.1252 0.7182 0.103 Uiso 0.50 1 calc PR B 1 N8B N 1.0893(13) 0.1348(14) 0.6900(15) 0.078(7) Uani 0.50 1 d P B 2 O9B O 0.9381(11) 0.1659(9) 1.4103(7) 0.055(3) Uani 0.50 1 d P C 2 C29B C 1.088(3) 0.239(2) 0.9372(18) 0.080(12) Uani 0.25 1 d P D 2 H29D H 1.1524 0.2098 0.9284 0.119 Uiso 0.25 1 calc PR D 2 H29E H 1.0962 0.2938 0.9230 0.119 Uiso 0.25 1 calc PR D 2 H29F H 1.0283 0.2034 0.9102 0.119 Uiso 0.25 1 calc PR D 2 C36B C 1.041(2) 0.1397(17) 1.4262(11) 0.149(13) Uani 0.50 1 d P C 2 H36D H 1.0410 0.0774 1.4094 0.224 Uiso 0.50 1 calc PR C 2 H36E H 1.0556 0.1560 1.4769 0.224 Uiso 0.50 1 calc PR C 2 H36F H 1.0947 0.1680 1.4030 0.224 Uiso 0.50 1 calc PR C 2 C55B C 0.994(3) 0.1101(14) 0.6758(18) 0.086(10) Uani 0.50 1 d P B 2 H55B H 0.9774 0.0850 0.6276 0.103 Uiso 0.50 1 calc PR B 2 C56B C 1.1708(18) 0.111(2) 0.643(2) 0.145(16) Uani 0.50 1 d P B 2 H56D H 1.2027 0.0613 0.6522 0.217 Uiso 0.50 1 calc PR B 2 H56E H 1.2249 0.1592 0.6486 0.217 Uiso 0.50 1 calc PR B 2 H56F H 1.1410 0.0968 0.5945 0.217 Uiso 0.50 1 calc PR B 2 C57B C 1.1175(18) 0.1875(15) 0.7656(14) 0.100(8) Uani 0.50 1 d P B 2 H57A H 1.0547 0.1890 0.7933 0.150 Uiso 0.50 1 calc PR B 2 H57B H 1.1432 0.2460 0.7647 0.150 Uiso 0.50 1 calc PR B 2 H57C H 1.1726 0.1607 0.7866 0.150 Uiso 0.50 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 Sm1 0.03061(15) 0.02564(14) 0.03373(15) 0.00437(11) 0.00052(11) 0.00047(10) Cl1 0.0877(13) 0.0525(10) 0.0563(10) 0.0275(8) -0.0260(9) -0.0157(9) O1 0.034(2) 0.054(3) 0.054(3) 0.019(2) 0.0089(19) 0.0113(19) N1 0.052(3) 0.045(3) 0.044(3) 0.015(2) -0.002(2) -0.004(2) C1 0.036(3) 0.034(3) 0.044(3) 0.011(2) 0.004(2) 0.003(2) Sm2 0.03542(17) 0.03663(17) 0.03613(17) 0.01140(12) -0.00315(12) -0.00020(12) Cl2 0.0901(14) 0.0418(9) 0.0557(10) 0.0092(7) -0.0037(9) 0.0145(9) O2 0.041(2) 0.043(2) 0.037(2) 0.0075(18) -0.0010(17) 0.0077(18) N2 0.043(3) 0.040(3) 0.038(3) 0.006(2) -0.009(2) -0.004(2) C2 0.031(3) 0.029(3) 0.038(3) -0.001(2) -0.001(2) -0.001(2) Cl3 0.0771(12) 0.0746(12) 0.0383(8) 0.0181(8) -0.0100(8) -0.0078(10) O3 0.097(4) 0.045(3) 0.034(2) 0.001(2) 0.002(2) 0.018(2) N3 0.034(3) 0.049(3) 0.038(3) -0.006(2) 0.003(2) -0.004(2) C3 0.034(3) 0.040(3) 0.035(3) 0.009(2) 0.002(2) -0.001(2) Cl4 0.0374(8) 0.0657(10) 0.0545(9) 0.0145(8) 0.0043(7) -0.0019(7) O4 0.057(3) 0.049(3) 0.049(3) 0.024(2) -0.008(2) -0.013(2) N4 0.050(3) 0.049(3) 0.048(3) 0.001(2) 0.010(3) 0.013(2) C4 0.031(3) 0.038(3) 0.042(3) 0.002(2) 0.003(2) 0.005(2) Cl5 0.0463(9) 0.0399(8) 0.0660(10) 0.0161(7) -0.0098(7) 0.0027(6) O5 0.063(3) 0.061(3) 0.063(3) 0.017(3) 0.000(3) -0.012(2) N5 0.036(3) 0.083(5) 0.120(6) 0.035(5) -0.004(4) -0.005(3) C5 0.034(3) 0.038(3) 0.034(3) 0.000(2) -0.004(2) 0.002(2) Cl6 0.0612(10) 0.0545(9) 0.0414(8) 0.0180(7) 0.0035(7) 0.0036(8) O6 0.028(2) 0.041(2) 0.067(3) -0.004(2) -0.0034(19) -0.0002(17) N6 0.060(4) 0.039(3) 0.054(3) -0.006(3) -0.004(3) 0.005(3) C6 0.032(3) 0.038(3) 0.030(3) 0.002(2) 0.002(2) 0.000(2) O7 0.034(2) 0.061(3) 0.089(4) -0.016(3) 0.000(2) 0.006(2) N7 0.138(7) 0.054(4) 0.077(5) 0.021(4) -0.027(5) -0.048(5) C7 0.029(3) 0.033(3) 0.031(3) -0.005(2) -0.002(2) 0.000(2) O8 0.040(2) 0.043(2) 0.036(2) 0.0037(17) -0.0005(17) -0.0069(18) C8 0.029(3) 0.039(3) 0.040(3) -0.001(2) 0.002(2) 0.004(2) C9 0.025(3) 0.036(3) 0.042(3) -0.005(2) 0.006(2) 0.003(2) O10 0.057(3) 0.053(3) 0.039(2) 0.008(2) 0.014(2) 0.014(2) C10 0.027(3) 0.047(3) 0.038(3) -0.004(3) 0.002(2) 0.009(2) O11 0.089(4) 0.058(3) 0.054(3) 0.014(2) 0.028(3) -0.001(3) C11 0.037(3) 0.038(3) 0.049(4) -0.002(3) 0.006(3) 0.001(2) O12 0.040(2) 0.065(3) 0.038(2) -0.001(2) 0.0090(18) 0.002(2) C12 0.024(3) 0.042(3) 0.056(4) -0.009(3) -0.004(3) 0.005(2) O13 0.064(3) 0.040(2) 0.074(3) 0.009(2) 0.022(3) 0.018(2) C13 0.031(3) 0.043(3) 0.039(3) -0.002(3) -0.001(2) 0.010(2) O14 0.036(2) 0.062(3) 0.078(3) 0.019(3) -0.017(2) -0.008(2) C14 0.027(3) 0.038(3) 0.035(3) -0.002(2) 0.000(2) 0.007(2) O15 0.065(3) 0.034(2) 0.044(2) -0.0017(19) 0.005(2) 0.003(2) C15 0.034(3) 0.049(3) 0.039(3) 0.003(3) 0.001(2) 0.014(3) O16 0.056(3) 0.034(2) 0.065(3) 0.008(2) -0.010(2) -0.008(2) C16 0.038(3) 0.047(3) 0.042(3) 0.010(3) 0.004(3) 0.012(3) O17 0.046(3) 0.083(4) 0.074(4) 0.034(3) -0.004(3) -0.012(3) C17 0.036(3) 0.098(6) 0.047(4) 0.000(4) -0.005(3) 0.014(4) C18 0.049(4) 0.108(7) 0.037(4) -0.012(4) -0.002(3) 0.020(4) C19 0.045(4) 0.059(4) 0.039(3) 0.004(3) 0.006(3) 0.017(3) C20 0.042(3) 0.038(3) 0.047(3) 0.012(3) 0.004(3) 0.009(3) C21 0.035(3) 0.038(3) 0.038(3) 0.010(2) 0.002(2) 0.005(2) C22 0.031(3) 0.051(4) 0.052(4) 0.008(3) 0.004(3) 0.002(3) C23 0.047(3) 0.041(3) 0.040(3) 0.008(3) 0.009(3) 0.008(3) C24 0.045(3) 0.043(3) 0.044(3) 0.013(3) 0.008(3) 0.007(3) C25 0.117(7) 0.079(6) 0.044(4) 0.016(4) 0.019(4) 0.054(5) C26 0.104(7) 0.086(6) 0.050(4) 0.027(4) 0.020(4) 0.051(5) C27 0.054(4) 0.049(4) 0.041(3) 0.000(3) 0.002(3) 0.005(3) C28 0.050(4) 0.044(3) 0.040(3) 0.005(3) 0.001(3) 0.005(3) C30 0.031(3) 0.054(4) 0.052(4) -0.005(3) -0.003(3) 0.007(3) C31 0.038(3) 0.041(3) 0.044(3) -0.001(3) -0.004(3) 0.003(3) C32 0.037(3) 0.046(4) 0.065(4) -0.003(3) -0.004(3) 0.008(3) C33 0.047(4) 0.041(3) 0.053(4) 0.000(3) -0.007(3) 0.010(3) C34 0.038(3) 0.043(3) 0.040(3) -0.001(3) 0.002(3) 0.001(3) C35 0.037(3) 0.039(3) 0.040(3) -0.002(2) -0.002(2) 0.003(2) C37 0.046(4) 0.058(4) 0.037(3) 0.009(3) 0.006(3) 0.007(3) C38 0.034(3) 0.047(3) 0.035(3) 0.005(3) 0.002(2) 0.000(2) C39 0.063(4) 0.044(4) 0.044(4) 0.008(3) 0.011(3) -0.003(3) C40 0.059(4) 0.042(4) 0.051(4) 0.006(3) 0.010(3) 0.002(3) C41 0.037(3) 0.055(4) 0.039(3) 0.013(3) 0.002(3) 0.002(3) C42 0.034(3) 0.052(4) 0.041(3) 0.012(3) 0.002(2) 0.006(3) C43 0.057(4) 0.050(4) 0.051(4) 0.009(3) 0.011(3) 0.013(3) C44 0.099(7) 0.093(7) 0.061(5) 0.027(5) 0.021(5) 0.028(5) C45 0.081(5) 0.041(4) 0.075(5) -0.005(4) 0.022(4) 0.018(4) C46 0.056(5) 0.078(6) 0.107(7) 0.037(5) -0.006(5) -0.005(4) C47 0.111(9) 0.080(7) 0.186(14) 0.034(8) 0.065(9) 0.014(6) C48 0.093(8) 0.133(11) 0.191(14) 0.058(10) -0.061(9) -0.042(8) C49 0.058(4) 0.046(4) 0.068(5) 0.010(4) -0.009(4) -0.006(3) C50 0.110(8) 0.075(6) 0.055(5) -0.010(4) 0.005(5) -0.002(5) C51 0.078(6) 0.054(4) 0.077(5) 0.011(4) 0.003(4) 0.008(4) C52 0.109(7) 0.052(4) 0.048(4) 0.007(3) -0.002(4) -0.026(4) C53 0.167(13) 0.124(10) 0.163(13) 0.072(10) -0.009(10) -0.082(10) C54 0.126(10) 0.043(5) 0.258(17) 0.010(8) -0.104(11) -0.001(6) N8A 0.035(9) 0.078(11) 0.060(9) 0.012(7) 0.004(6) 0.005(7) O9A 0.044(6) 0.073(9) 0.034(6) -0.001(6) 0.001(4) 0.005(7) C29A 0.112(11) 0.068(7) 0.074(8) 0.037(6) -0.001(8) -0.009(7) C36A 0.043(8) 0.115(15) 0.057(9) -0.031(10) -0.008(7) 0.014(9) C55A 0.024(7) 0.058(13) 0.061(11) 0.017(9) 0.007(7) -0.011(8) C56A 0.072(14) 0.15(2) 0.089(15) 0.051(14) 0.042(12) 0.027(15) C57A 0.033(10) 0.071(12) 0.113(18) 0.054(12) -0.018(13) -0.020(10) N8B 0.023(8) 0.086(14) 0.15(2) 0.092(15) -0.007(12) -0.011(9) O9B 0.053(7) 0.068(9) 0.040(6) 0.008(6) -0.010(5) 0.001(7) C29B 0.11(3) 0.051(18) 0.09(2) 0.022(16) 0.08(2) 0.011(18) C36B 0.18(2) 0.15(2) 0.088(15) -0.050(15) -0.100(17) 0.09(2) C55B 0.10(2) 0.040(12) 0.12(2) 0.020(13) -0.042(18) -0.009(14) C56B 0.053(15) 0.15(3) 0.29(5) 0.16(3) 0.07(2) 0.046(16) C57B 0.074(14) 0.105(18) 0.14(2) 0.086(17) -0.046(15) -0.038(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O12 2.398(4) 1_554 ? Sm1 O4 2.399(4) . ? Sm1 O14 2.414(4) . ? Sm1 O8 2.430(4) 2_767 ? Sm1 O13 2.433(4) . ? Sm1 O15 2.453(4) . ? Sm1 O16 2.508(4) . ? Sm1 Cl1 2.7724(17) . ? O1 C4 1.384(7) . ? O1 C22 1.436(7) . ? N1 C27 1.319(8) . ? N1 O4 1.331(7) . ? N1 C26 1.348(9) . ? C1 C2 1.517(8) . ? C1 C21 1.536(8) . ? Sm2 O17 2.406(6) . ? Sm2 Cl3 2.6707(17) . ? Sm2 Cl5 2.6883(16) . ? Sm2 Cl4 2.6912(16) . ? Sm2 Cl2 2.6952(17) . ? Sm2 Cl6 2.7286(16) . ? O2 C23 1.334(7) . ? O2 C5 1.413(7) . ? N2 O8 1.319(6) . ? N2 C34 1.356(7) . ? N2 C33 1.365(8) . ? C2 C7 1.412(8) . ? C2 C3 1.416(8) . ? O3 C23 1.207(7) . ? N3 C41 1.317(8) . ? N3 O12 1.330(6) . ? N3 C40 1.377(8) . ? C3 C4 1.388(8) . ? N4 C43 1.311(8) . ? N4 C44 1.445(9) . ? N4 C45 1.473(9) . ? C4 C5 1.392(8) . ? O5 C29A 1.343(13) . ? O5 C11 1.368(8) . ? O5 C29B 1.47(3) . ? N5 C46 1.333(10) . ? N5 C47 1.413(14) . ? N5 C48 1.438(13) . ? C5 C6 1.386(8) . ? O6 C30 1.351(7) . ? O6 C12 1.432(7) . ? N6 C49 1.325(9) . ? N6 C51 1.422(10) . ? N6 C50 1.509(9) . ? C6 C7 1.399(8) . ? O7 C30 1.212(7) . ? N7 C52 1.328(9) . ? N7 C54 1.431(15) . ? N7 C53 1.533(14) . ? C7 C8 1.527(7) . ? O8 Sm1 2.430(4) 2_767 ? C8 C9 1.547(8) . ? N9 C58 1.413(13) . ? N9 C59 1.434(13) . ? N9 C60 1.527(16) . ? C9 C14 1.404(8) . ? C9 C10 1.405(9) . ? O10 C37 1.353(8) . ? O10 C19 1.428(7) . ? N10 C61 1.369(17) . ? N10 C63 1.383(17) . ? N10 C62 1.525(19) . ? C10 C11 1.400(8) . ? O11 C37 1.207(8) . ? C11 C12 1.398(9) . ? O12 Sm1 2.398(4) 1_556 ? C12 C13 1.359(9) . ? O13 C43 1.237(8) . ? C13 C14 1.416(8) . ? O14 C46 1.159(10) . ? C14 C15 1.510(8) . ? O15 C49 1.271(8) . ? C15 C16 1.540(8) . ? O16 C52 1.240(9) . ? C16 C21 1.392(8) . ? C16 C17 1.402(9) . ? O17 C55B 1.11(4) . ? O17 C55A 1.37(2) . ? C17 C18 1.383(9) . ? O18 C58 1.093(12) . ? C18 C19 1.385(10) . ? C18 O9B 1.388(15) . ? C18 O9A 1.475(15) . ? O19 C61 1.177(19) . ? C19 C20 1.361(9) . ? C20 C21 1.405(8) . ? C23 C24 1.509(9) . ? C24 C28 1.383(8) . ? C24 C25 1.395(9) . ? C25 C26 1.365(11) . ? C27 C28 1.384(9) . ? C30 C31 1.481(9) . ? C31 C32 1.391(8) . ? C31 C35 1.394(8) . ? C32 C33 1.388(9) . ? C34 C35 1.390(8) . ? C37 C38 1.497(8) . ? C38 C42 1.381(8) . ? C38 C39 1.396(9) . ? C39 C40 1.365(9) . ? C41 C42 1.400(8) . ? C60 C60 1.96(4) 2_766 ? N8A C55A 1.31(3) . ? N8A C56A 1.46(3) . ? N8A C57A 1.46(3) . ? O9A C36A 1.49(2) . ? N8B C55B 1.26(4) . ? N8B C56B 1.43(4) . ? N8B C57B 1.55(3) . ? O9B C36B 1.45(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 O12 Sm1 O4 113.86(16) 1_554 . ? O12 Sm1 O14 148.56(16) 1_554 . ? O4 Sm1 O14 70.35(16) . . ? O12 Sm1 O8 73.39(14) 1_554 2_767 ? O4 Sm1 O8 67.22(14) . 2_767 ? O14 Sm1 O8 131.18(16) . 2_767 ? O12 Sm1 O13 137.21(16) 1_554 . ? O4 Sm1 O13 86.19(17) . . ? O14 Sm1 O13 72.57(17) . . ? O8 Sm1 O13 81.56(16) 2_767 . ? O12 Sm1 O15 73.89(15) 1_554 . ? O4 Sm1 O15 74.62(15) . . ? O14 Sm1 O15 77.78(17) . . ? O8 Sm1 O15 112.01(15) 2_767 . ? O13 Sm1 O15 148.75(16) . . ? O12 Sm1 O16 70.93(16) 1_554 . ? O4 Sm1 O16 137.79(15) . . ? O14 Sm1 O16 128.49(16) . . ? O8 Sm1 O16 75.27(14) 2_767 . ? O13 Sm1 O16 69.43(16) . . ? O15 Sm1 O16 140.02(16) . . ? O12 Sm1 Cl1 83.69(12) 1_554 . ? O4 Sm1 Cl1 142.03(11) . . ? O14 Sm1 Cl1 77.77(13) . . ? O8 Sm1 Cl1 149.79(10) 2_767 . ? O13 Sm1 Cl1 103.66(13) . . ? O15 Sm1 Cl1 79.02(12) . . ? O16 Sm1 Cl1 78.83(11) . . ? C4 O1 C22 115.8(5) . . ? C27 N1 O4 120.5(5) . . ? C27 N1 C26 120.9(6) . . ? O4 N1 C26 118.6(6) . . ? C2 C1 C21 114.3(5) . . ? O17 Sm2 Cl3 83.11(15) . . ? O17 Sm2 Cl5 88.44(15) . . ? Cl3 Sm2 Cl5 92.65(6) . . ? O17 Sm2 Cl4 174.80(16) . . ? Cl3 Sm2 Cl4 99.95(6) . . ? Cl5 Sm2 Cl4 87.22(5) . . ? O17 Sm2 Cl2 94.70(15) . . ? Cl3 Sm2 Cl2 85.99(6) . . ? Cl5 Sm2 Cl2 176.40(6) . . ? Cl4 Sm2 Cl2 89.72(6) . . ? O17 Sm2 Cl6 79.37(15) . . ? Cl3 Sm2 Cl6 161.78(6) . . ? Cl5 Sm2 Cl6 91.85(5) . . ? Cl4 Sm2 Cl6 97.89(5) . . ? Cl2 Sm2 Cl6 90.46(5) . . ? C23 O2 C5 118.9(5) . . ? O8 N2 C34 119.5(5) . . ? O8 N2 C33 119.3(5) . . ? C34 N2 C33 121.1(5) . . ? C7 C2 C3 119.0(5) . . ? C7 C2 C1 123.3(5) . . ? C3 C2 C1 117.7(5) . . ? C41 N3 O12 120.0(5) . . ? C41 N3 C40 121.3(5) . . ? O12 N3 C40 118.7(5) . . ? C4 C3 C2 121.7(5) . . ? N1 O4 Sm1 134.6(4) . . ? C43 N4 C44 122.1(6) . . ? C43 N4 C45 122.2(6) . . ? C44 N4 C45 115.7(6) . . ? O1 C4 C3 125.1(5) . . ? O1 C4 C5 116.7(5) . . ? C3 C4 C5 118.2(5) . . ? C29A O5 C11 116.5(7) . . ? C29A O5 C29B 44.4(17) . . ? C11 O5 C29B 123.3(13) . . ? C46 N5 C47 119.5(9) . . ? C46 N5 C48 121.7(10) . . ? C47 N5 C48 118.6(9) . . ? C6 C5 C4 121.4(5) . . ? C6 C5 O2 116.8(5) . . ? C4 C5 O2 121.4(5) . . ? C30 O6 C12 116.9(4) . . ? C49 N6 C51 124.6(6) . . ? C49 N6 C50 120.2(7) . . ? C51 N6 C50 115.0(6) . . ? C5 C6 C7 121.0(5) . . ? C52 N7 C54 122.4(9) . . ? C52 N7 C53 118.3(10) . . ? C54 N7 C53 118.7(9) . . ? C6 C7 C2 118.7(5) . . ? C6 C7 C8 117.1(5) . . ? C2 C7 C8 124.2(5) . . ? N2 O8 Sm1 126.8(3) . 2_767 ? C7 C8 C9 112.7(4) . . ? C58 N9 C59 119.2(11) . . ? C58 N9 C60 124.9(13) . . ? C59 N9 C60 113.6(13) . . ? C14 C9 C10 120.7(5) . . ? C14 C9 C8 122.4(5) . . ? C10 C9 C8 116.9(5) . . ? C37 O10 C19 115.8(5) . . ? C61 N10 C63 126.0(14) . . ? C61 N10 C62 108.6(14) . . ? C63 N10 C62 125.0(14) . . ? C11 C10 C9 121.0(6) . . ? O5 C11 C12 117.6(6) . . ? O5 C11 C10 125.3(6) . . ? C12 C11 C10 117.1(6) . . ? N3 O12 Sm1 135.8(3) . 1_556 ? C13 C12 C11 123.0(6) . . ? C13 C12 O6 119.3(6) . . ? C11 C12 O6 117.5(6) . . ? C43 O13 Sm1 134.5(4) . . ? C12 C13 C14 120.6(6) . . ? C46 O14 Sm1 145.4(6) . . ? C9 C14 C13 117.6(6) . . ? C9 C14 C15 124.6(5) . . ? C13 C14 C15 117.8(5) . . ? C49 O15 Sm1 133.1(4) . . ? C14 C15 C16 110.7(5) . . ? C52 O16 Sm1 135.1(5) . . ? C21 C16 C17 119.3(6) . . ? C21 C16 C15 123.6(5) . . ? C17 C16 C15 117.0(5) . . ? C55B O17 C55A 25.7(11) . . ? C55B O17 Sm2 148.6(16) . . ? C55A O17 Sm2 126.7(9) . . ? C18 C17 C16 121.9(6) . . ? C17 C18 C19 117.5(6) . . ? C17 C18 O9B 125.8(9) . . ? C19 C18 O9B 113.9(8) . . ? C17 C18 O9A 122.5(8) . . ? C19 C18 O9A 118.0(7) . . ? O9B C18 O9A 30.1(5) . . ? C20 C19 C18 121.9(6) . . ? C20 C19 O10 119.7(6) . . ? C18 C19 O10 118.3(6) . . ? C19 C20 C21 120.9(6) . . ? C16 C21 C20 118.3(5) . . ? C16 C21 C1 124.0(5) . . ? C20 C21 C1 117.7(5) . . ? O3 C23 O2 125.2(6) . . ? O3 C23 C24 124.7(6) . . ? O2 C23 C24 110.1(5) . . ? C28 C24 C25 117.6(6) . . ? C28 C24 C23 122.1(5) . . ? C25 C24 C23 120.2(6) . . ? C26 C25 C24 120.5(7) . . ? N1 C26 C25 120.1(7) . . ? N1 C27 C28 121.2(6) . . ? C27 C28 C24 119.5(6) . . ? O7 C30 O6 123.9(6) . . ? O7 C30 C31 124.8(6) . . ? O6 C30 C31 111.3(5) . . ? C32 C31 C35 118.7(6) . . ? C32 C31 C30 118.7(5) . . ? C35 C31 C30 122.6(5) . . ? C33 C32 C31 120.6(6) . . ? N2 C33 C32 119.5(6) . . ? N2 C34 C35 120.4(5) . . ? C34 C35 C31 119.7(5) . . ? O11 C37 O10 124.7(6) . . ? O11 C37 C38 124.0(6) . . ? O10 C37 C38 111.3(5) . . ? C42 C38 C39 119.5(6) . . ? C42 C38 C37 122.5(6) . . ? C39 C38 C37 118.1(6) . . ? C40 C39 C38 119.7(6) . . ? C39 C40 N3 119.9(6) . . ? N3 C41 C42 120.9(6) . . ? C38 C42 C41 118.8(6) . . ? O13 C43 N4 125.4(7) . . ? O14 C46 N5 128.8(10) . . ? O15 C49 N6 123.1(7) . . ? O16 C52 N7 124.1(9) . . ? O18 C58 N9 126.8(13) . . ? N9 C60 C60 112.8(18) . 2_766 ? O19 C61 N10 113.6(18) . . ? C55A N8A C56A 123.2(19) . . ? C55A N8A C57A 115.7(17) . . ? C56A N8A C57A 120.7(17) . . ? C18 O9A C36A 118.6(11) . . ? N8A C55A O17 128.1(18) . . ? C55B N8B C56B 124(4) . . ? C55B N8B C57B 116(3) . . ? C56B N8B C57B 120(3) . . ? C18 O9B C36B 117.5(13) . . ? O17 C55B N8B 132(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.920 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.133 _database_code_depnum_ccdc_archive 'CCDC 936738' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c: _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Aquodimethylformamide{(+-)-2,7,12-Trimethoxy-3,8,13-tris(4- phenylcarboxylic acid methoxy)-10,15-dihydro-5H- tribenzo[a,d,g] cyclononatriene}europium(III) dimethylformamide hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.50 H60.50 Eu N2.50 O16.50' _chemical_formula_weight 1178.52 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2284(10) _cell_length_b 14.7501(11) _cell_length_c 16.4083(12) _cell_angle_alpha 76.082(4) _cell_angle_beta 70.013(3) _cell_angle_gamma 61.718(3) _cell_volume 2837.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5392 _exptl_absorpt_correction_T_max 0.8528 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER X8 CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73244 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0235 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9928 _reflns_number_gt 9299 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. DMF ligand and DMF and water solvent were refined isotropically and the DMF ligand was refined with group displacement parameters for C/N atoms. A disordered water molecule was refined across two positions each at 50% occupancy. One C-N bond was restrained to be chemically reasonable. ; _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^)+(0.0792P)^2^+19.9926P] 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 9928 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.168 _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 Eu1 Eu 0.88309(3) -0.06623(3) 0.52273(2) 0.03844(15) Uani 1 1 d . . . O1 O 0.6832(4) -0.0243(4) 0.5341(3) 0.0477(13) Uani 1 1 d . . . O2 O 0.7639(5) -0.1346(5) 0.6355(4) 0.0566(15) Uani 1 1 d . . . O3 O -0.0733(4) 0.0914(4) 0.5489(3) 0.0444(12) Uani 1 1 d . . . O4 O -0.2336(4) 0.0820(4) 0.6063(4) 0.0481(13) Uani 1 1 d . . . O5 O -0.0224(4) 0.8694(4) 0.6390(3) 0.0396(11) Uani 1 1 d . . . O6 O 0.0009(5) 0.7489(4) 0.5671(4) 0.0513(13) Uani 1 1 d . . . O7 O 0.1939(4) -0.1008(4) 0.7657(4) 0.0446(12) Uani 1 1 d . . . O8 O -0.0183(4) -0.0244(4) 0.7909(4) 0.0469(13) Uani 1 1 d . . . O9 O -0.2924(5) 0.5135(5) 0.7987(5) 0.0694(19) Uani 1 1 d . . . O10 O -0.1876(5) 0.6124(4) 0.8008(4) 0.0594(15) Uani 1 1 d . . . O11 O 0.3728(5) 0.3675(4) 0.8042(6) 0.075(2) Uani 1 1 d . . . O12 O 0.4734(5) 0.1732(5) 0.7856(6) 0.082(2) Uani 1 1 d . . . O13 O 0.8646(4) 0.0624(4) 0.3966(3) 0.0470(12) Uani 1 1 d . . . O14 O 0.8907(5) -0.1586(5) 0.4174(4) 0.0557(14) Uiso 1 1 d . . . C1 C 0.1560(7) 0.1082(6) 0.9790(5) 0.0448(17) Uani 1 1 d . . . H1A H 0.1001 0.1373 1.0330 0.054 Uiso 1 1 calc R . . H1B H 0.2154 0.0433 0.9965 0.054 Uiso 1 1 calc R . . C2 C 0.1018(6) 0.0816(5) 0.9289(5) 0.0400(16) Uani 1 1 d . . . C3 C 0.1721(6) 0.0037(5) 0.8714(5) 0.0395(16) Uani 1 1 d . . . H3 H 0.2496 -0.0279 0.8653 0.047 Uiso 1 1 calc R . . C4 C 0.1311(6) -0.0272(5) 0.8245(5) 0.0386(15) Uani 1 1 d . . . C5 C 0.0156(6) 0.0167(5) 0.8355(5) 0.0403(16) Uani 1 1 d . . . C6 C -0.0541(6) 0.0945(5) 0.8906(5) 0.0416(16) Uani 1 1 d . . . H6 H -0.1316 0.1252 0.8973 0.050 Uiso 1 1 calc R . . C7 C -0.0115(6) 0.1285(6) 0.9368(5) 0.0419(16) Uani 1 1 d . . . C8 C -0.0953(7) 0.2168(6) 0.9938(5) 0.0467(18) Uani 1 1 d . . . H8A H -0.1663 0.2108 1.0169 0.056 Uiso 1 1 calc R . . H8B H -0.0680 0.2096 1.0441 0.056 Uiso 1 1 calc R . . C9 C -0.1157(6) 0.3226(5) 0.9456(5) 0.0408(16) Uani 1 1 d . . . C10 C -0.1956(6) 0.3670(6) 0.8985(6) 0.0476(19) Uani 1 1 d . . . H10 H -0.2362 0.3305 0.9000 0.057 Uiso 1 1 calc R . . C11 C -0.2173(6) 0.4617(6) 0.8501(6) 0.0492(19) Uani 1 1 d . . . C12 C -0.1590(6) 0.5167(6) 0.8490(5) 0.0440(17) Uani 1 1 d . . . C13 C -0.0808(6) 0.4747(5) 0.8947(5) 0.0413(16) Uani 1 1 d . . . H13 H -0.0411 0.5121 0.8930 0.050 Uiso 1 1 calc R . . C14 C -0.0573(6) 0.3780(5) 0.9440(5) 0.0382(15) Uani 1 1 d . . . C15 C 0.0287(6) 0.3404(6) 0.9941(5) 0.0438(17) Uani 1 1 d . . . H15A H 0.0149 0.2900 1.0431 0.053 Uiso 1 1 calc R . . H15B H 0.0187 0.4000 1.0193 0.053 Uiso 1 1 calc R . . C16 C 0.1482(6) 0.2900(5) 0.9401(5) 0.0428(17) Uani 1 1 d . . . C17 C 0.2028(7) 0.3526(6) 0.8963(6) 0.052(2) Uani 1 1 d . . . H17 H 0.1641 0.4248 0.9019 0.062 Uiso 1 1 calc R . . C18 C 0.3097(7) 0.3144(6) 0.8457(7) 0.055(2) Uani 1 1 d . . . C19 C 0.3683(7) 0.2061(6) 0.8357(7) 0.059(2) Uani 1 1 d . . . C20 C 0.3130(7) 0.1441(6) 0.8802(6) 0.0503(19) Uani 1 1 d . . . H20 H 0.3514 0.0718 0.8748 0.060 Uiso 1 1 calc R . . C21 C 0.2051(7) 0.1832(6) 0.9316(5) 0.0439(17) Uani 1 1 d . . . C22 C 0.3014(6) -0.1785(6) 0.7769(5) 0.0428(17) Uani 1 1 d . . . H22A H 0.3189 -0.2429 0.7546 0.051 Uiso 1 1 calc R . . H22B H 0.2966 -0.1939 0.8400 0.051 Uiso 1 1 calc R . . C23 C 0.3948(6) -0.1475(5) 0.7318(5) 0.0378(15) Uani 1 1 d . . . C24 C 0.3916(7) -0.0693(6) 0.6638(5) 0.0485(18) Uani 1 1 d . . . H24 H 0.3254 -0.0287 0.6460 0.058 Uiso 1 1 calc R . . C25 C 0.4828(6) -0.0500(6) 0.6224(5) 0.0464(18) Uani 1 1 d . . . H25 H 0.4788 0.0035 0.5761 0.056 Uiso 1 1 calc R . . C26 C 0.5803(6) -0.1071(6) 0.6466(5) 0.0396(15) Uani 1 1 d . . . C27 C 0.5847(6) -0.1860(6) 0.7151(6) 0.0478(18) Uani 1 1 d . . . H27 H 0.6510 -0.2263 0.7329 0.057 Uiso 1 1 calc R . . C28 C 0.4928(7) -0.2049(6) 0.7565(6) 0.0472(18) Uani 1 1 d . . . H28 H 0.4966 -0.2583 0.8028 0.057 Uiso 1 1 calc R . . C29 C 0.6813(6) -0.0864(6) 0.6031(5) 0.0440(17) Uani 1 1 d . . . C30 C -0.3622(7) 0.4712(8) 0.8016(8) 0.071(3) Uani 1 1 d . . . H30A H -0.4281 0.5267 0.7837 0.085 Uiso 1 1 calc R . . H30B H -0.3880 0.4454 0.8627 0.085 Uiso 1 1 calc R . . C31 C -0.3106(7) 0.3829(7) 0.7442(6) 0.058(2) Uani 1 1 d . . . C32 C -0.2117(8) 0.3627(8) 0.6788(7) 0.069(3) Uani 1 1 d . . . H32 H -0.1742 0.4049 0.6687 0.082 Uiso 1 1 calc R . . C33 C -0.1679(8) 0.2818(7) 0.6288(6) 0.061(2) Uani 1 1 d . . . H33 H -0.0995 0.2673 0.5854 0.073 Uiso 1 1 calc R . . C34 C -0.2230(6) 0.2226(6) 0.6415(5) 0.0438(17) Uani 1 1 d . . . C35 C -0.3240(7) 0.2465(7) 0.7038(6) 0.056(2) Uani 1 1 d . . . H35 H -0.3648 0.2083 0.7106 0.067 Uiso 1 1 calc R . . C36 C -0.3659(7) 0.3249(8) 0.7562(7) 0.068(3) Uani 1 1 d . . . H36 H -0.4335 0.3383 0.8005 0.081 Uiso 1 1 calc R . . C37 C -0.1738(6) 0.1275(6) 0.5948(5) 0.0410(16) Uani 1 1 d . . . C38 C 0.3263(8) 0.4742(6) 0.8231(9) 0.070(3) Uani 1 1 d . . . H38A H 0.3873 0.4947 0.8102 0.084 Uiso 1 1 calc R . . H38B H 0.2881 0.4791 0.8860 0.084 Uiso 1 1 calc R . . C39 C 0.2460(7) 0.5481(6) 0.7715(7) 0.055(2) Uani 1 1 d . . . C40 C 0.2380(8) 0.5229(7) 0.6969(8) 0.069(3) Uani 1 1 d . . . H40 H 0.2828 0.4550 0.6791 0.083 Uiso 1 1 calc R . . C41 C 0.1661(7) 0.5956(6) 0.6496(7) 0.058(2) Uani 1 1 d . . . H41 H 0.1610 0.5772 0.6002 0.070 Uiso 1 1 calc R . . C42 C 0.1006(6) 0.6965(6) 0.6741(5) 0.0423(16) Uani 1 1 d . . . C43 C 0.1097(6) 0.7210(6) 0.7470(5) 0.0417(16) Uani 1 1 d . . . H43 H 0.0661 0.7891 0.7644 0.050 Uiso 1 1 calc R . . C44 C 0.1816(6) 0.6471(6) 0.7943(6) 0.0450(17) Uani 1 1 d . . . H44 H 0.1863 0.6656 0.8438 0.054 Uiso 1 1 calc R . . C45 C 0.0222(6) 0.7745(6) 0.6238(5) 0.0389(15) Uani 1 1 d . . . C46 C -0.1351(6) 0.0229(6) 0.7961(5) 0.0471(18) Uani 1 1 d . . . H46A H -0.1593 0.0969 0.7771 0.071 Uiso 1 1 calc R . . H46B H -0.1768 0.0137 0.8564 0.071 Uiso 1 1 calc R . . H46C H -0.1482 -0.0098 0.7584 0.071 Uiso 1 1 calc R . . C47 C -0.1300(8) 0.6704(8) 0.7982(9) 0.083(4) Uani 1 1 d . . . H47A H -0.0501 0.6288 0.7770 0.125 Uiso 1 1 calc R . . H47B H -0.1470 0.6886 0.8568 0.125 Uiso 1 1 calc R . . H47C H -0.1533 0.7337 0.7589 0.125 Uiso 1 1 calc R . . C48 C 0.5337(12) 0.0665(10) 0.7761(12) 0.128(7) Uani 1 1 d . . . H48A H 0.4946 0.0441 0.7520 0.192 Uiso 1 1 calc R . . H48B H 0.5409 0.0282 0.8331 0.192 Uiso 1 1 calc R . . H48C H 0.6075 0.0528 0.7366 0.192 Uiso 1 1 calc R . . C50 C 0.8415(15) -0.2040(13) 0.4160(12) 0.117(2) Uiso 1 1 d . . . H50 H 0.7882 -0.2115 0.4678 0.141 Uiso 1 1 calc R . . N50 N 0.8566(11) -0.2454(11) 0.3455(9) 0.117(2) Uiso 1 1 d D . . C52 C 0.9403(13) -0.2505(13) 0.2655(10) 0.117(2) Uiso 1 1 d D . . H52A H 0.9932 -0.2305 0.2731 0.176 Uiso 1 1 calc R . . H52B H 0.9060 -0.2033 0.2199 0.176 Uiso 1 1 calc R . . H52C H 0.9792 -0.3213 0.2486 0.176 Uiso 1 1 calc R . . C53 C 0.7696(14) -0.2555(13) 0.3229(11) 0.117(2) Uiso 1 1 d . . . H53A H 0.7091 -0.2526 0.3754 0.176 Uiso 1 1 calc R . . H53B H 0.8013 -0.3217 0.2988 0.176 Uiso 1 1 calc R . . H53C H 0.7409 -0.1987 0.2796 0.176 Uiso 1 1 calc R . . N60 N 0.4884(9) 0.2331(8) 0.0131(7) 0.082(3) Uiso 1 1 d . . . C61 C 0.4389(17) 0.3394(15) 0.0191(14) 0.147(7) Uiso 1 1 d . . . H61A H 0.3903 0.3747 -0.0199 0.220 Uiso 1 1 calc R . . H61B H 0.4963 0.3642 0.0023 0.220 Uiso 1 1 calc R . . H61C H 0.3952 0.3538 0.0792 0.220 Uiso 1 1 calc R . . O60 O 0.6529(18) 0.2152(16) -0.0168(14) 0.218(8) Uiso 1 1 d . . . C60 C 0.591(3) 0.171(2) -0.0217(19) 0.201(11) Uiso 1 1 d . . . H60 H 0.6164 0.1077 -0.0453 0.241 Uiso 1 1 calc R . . C62 C 0.4065(19) 0.1923(18) 0.0434(15) 0.166(8) Uiso 1 1 d . . . H62A H 0.3849 0.1841 0.1073 0.249 Uiso 1 1 calc R . . H62B H 0.4378 0.1250 0.0212 0.249 Uiso 1 1 calc R . . H62C H 0.3413 0.2403 0.0223 0.249 Uiso 1 1 calc R . . O80 O 0.798(2) 0.2917(19) 0.4790(16) 0.130(7) Uiso 0.50 1 d P . . O70 O 0.5329(8) 0.3957(7) 0.3239(6) 0.039(2) Uiso 0.50 1 d P A 1 N70 N 0.5195(15) 0.3154(14) 0.4569(13) 0.073(5) Uiso 0.50 1 d P A 1 C72 C 0.6291(19) 0.2777(19) 0.4521(16) 0.079(6) Uiso 0.50 1 d P A 1 H72A H 0.6614 0.2020 0.4608 0.119 Uiso 0.50 1 calc PR A 1 H72B H 0.6371 0.3045 0.4973 0.119 Uiso 0.50 1 calc PR A 1 H72C H 0.6676 0.2996 0.3946 0.119 Uiso 0.50 1 calc PR A 1 C70 C 0.485(3) 0.362(2) 0.394(2) 0.111(9) Uiso 0.50 1 d P A 1 H70 H 0.4117 0.3743 0.3994 0.133 Uiso 0.50 1 calc PR A 1 C71 C 0.485(5) 0.274(4) 0.535(3) 0.20(2) Uiso 0.50 1 d P A 1 H71A H 0.4397 0.3275 0.5754 0.293 Uiso 0.50 1 calc PR A 1 H71B H 0.5491 0.2216 0.5559 0.293 Uiso 0.50 1 calc PR A 1 H71C H 0.4407 0.2407 0.5320 0.293 Uiso 0.50 1 calc PR A 1 O71 O 0.5597(19) 0.1599(17) 0.5229(14) 0.114(6) Uiso 0.50 1 d P 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 Eu1 0.0366(2) 0.0451(2) 0.0350(2) -0.00647(15) -0.00530(15) -0.02035(17) O1 0.042(3) 0.055(3) 0.039(3) 0.002(2) -0.006(2) -0.021(3) O2 0.045(3) 0.067(4) 0.060(4) 0.016(3) -0.019(3) -0.032(3) O3 0.039(3) 0.051(3) 0.039(3) -0.008(2) -0.006(2) -0.018(2) O4 0.041(3) 0.048(3) 0.054(3) -0.012(2) -0.002(2) -0.022(2) O5 0.037(3) 0.039(3) 0.042(3) -0.008(2) -0.007(2) -0.015(2) O6 0.054(3) 0.047(3) 0.055(3) -0.013(3) -0.015(3) -0.019(3) O7 0.030(2) 0.045(3) 0.053(3) -0.018(2) -0.006(2) -0.009(2) O8 0.032(3) 0.043(3) 0.064(3) -0.022(3) -0.007(2) -0.011(2) O9 0.058(4) 0.041(3) 0.116(6) -0.019(3) -0.047(4) -0.005(3) O10 0.054(3) 0.039(3) 0.081(4) 0.005(3) -0.035(3) -0.009(3) O11 0.041(3) 0.034(3) 0.142(7) 0.006(3) -0.029(4) -0.013(3) O12 0.050(4) 0.042(3) 0.123(6) -0.007(4) 0.006(4) -0.014(3) O13 0.047(3) 0.054(3) 0.043(3) 0.001(2) -0.014(2) -0.025(3) C1 0.049(4) 0.033(4) 0.041(4) 0.000(3) -0.011(3) -0.012(3) C2 0.043(4) 0.033(4) 0.038(4) -0.003(3) -0.002(3) -0.018(3) C3 0.037(4) 0.034(4) 0.041(4) -0.002(3) -0.006(3) -0.014(3) C4 0.039(4) 0.030(3) 0.041(4) -0.005(3) -0.006(3) -0.013(3) C5 0.038(4) 0.033(4) 0.045(4) -0.003(3) -0.004(3) -0.017(3) C6 0.039(4) 0.034(4) 0.042(4) -0.003(3) -0.001(3) -0.015(3) C7 0.045(4) 0.035(4) 0.036(4) -0.003(3) 0.000(3) -0.017(3) C8 0.042(4) 0.041(4) 0.044(4) -0.012(3) 0.004(3) -0.015(3) C9 0.038(4) 0.036(4) 0.040(4) -0.014(3) -0.002(3) -0.010(3) C10 0.035(4) 0.034(4) 0.073(5) -0.021(4) -0.015(4) -0.006(3) C11 0.040(4) 0.036(4) 0.070(5) -0.017(4) -0.026(4) -0.001(3) C12 0.037(4) 0.034(4) 0.053(4) -0.010(3) -0.016(3) -0.004(3) C13 0.039(4) 0.033(4) 0.052(4) -0.008(3) -0.013(3) -0.013(3) C14 0.035(4) 0.035(4) 0.040(4) -0.012(3) -0.008(3) -0.008(3) C15 0.049(4) 0.034(4) 0.050(4) -0.012(3) -0.018(3) -0.012(3) C16 0.044(4) 0.033(4) 0.052(4) -0.005(3) -0.023(3) -0.010(3) C17 0.041(4) 0.029(4) 0.086(6) -0.009(4) -0.030(4) -0.006(3) C18 0.044(4) 0.029(4) 0.093(7) 0.006(4) -0.028(4) -0.016(3) C19 0.036(4) 0.036(4) 0.087(7) -0.008(4) -0.006(4) -0.008(3) C20 0.046(4) 0.028(4) 0.070(5) -0.006(3) -0.012(4) -0.012(3) C21 0.047(4) 0.036(4) 0.048(4) -0.002(3) -0.019(3) -0.015(3) C22 0.031(4) 0.035(4) 0.054(4) -0.008(3) -0.006(3) -0.009(3) C23 0.033(3) 0.032(3) 0.046(4) -0.011(3) -0.007(3) -0.011(3) C24 0.039(4) 0.046(4) 0.053(5) 0.002(3) -0.015(3) -0.014(3) C25 0.043(4) 0.046(4) 0.043(4) 0.006(3) -0.009(3) -0.020(3) C26 0.037(4) 0.039(4) 0.040(4) -0.008(3) -0.004(3) -0.016(3) C27 0.038(4) 0.043(4) 0.064(5) 0.005(4) -0.022(4) -0.017(3) C28 0.047(4) 0.040(4) 0.056(5) 0.008(3) -0.019(4) -0.022(3) C29 0.035(4) 0.047(4) 0.050(4) -0.009(3) -0.006(3) -0.019(3) C30 0.040(5) 0.065(6) 0.112(8) -0.042(6) -0.033(5) -0.001(4) C31 0.032(4) 0.060(5) 0.070(6) -0.026(4) -0.023(4) 0.005(4) C32 0.057(6) 0.073(6) 0.091(7) -0.035(6) -0.023(5) -0.025(5) C33 0.053(5) 0.062(5) 0.068(6) -0.027(5) -0.007(4) -0.023(4) C34 0.041(4) 0.048(4) 0.042(4) -0.010(3) -0.017(3) -0.012(3) C35 0.040(4) 0.050(5) 0.066(5) -0.021(4) -0.011(4) -0.005(4) C36 0.036(4) 0.073(6) 0.083(7) -0.039(5) -0.010(4) -0.003(4) C37 0.039(4) 0.039(4) 0.037(4) -0.005(3) -0.010(3) -0.009(3) C38 0.049(5) 0.032(4) 0.139(10) 0.003(5) -0.046(6) -0.016(4) C39 0.038(4) 0.038(4) 0.093(7) 0.000(4) -0.021(4) -0.021(3) C40 0.056(5) 0.035(4) 0.120(9) -0.021(5) -0.032(6) -0.010(4) C41 0.051(5) 0.034(4) 0.085(6) -0.021(4) -0.018(4) -0.008(4) C42 0.035(4) 0.035(4) 0.053(4) -0.008(3) -0.004(3) -0.015(3) C43 0.038(4) 0.035(4) 0.047(4) -0.005(3) -0.005(3) -0.015(3) C44 0.038(4) 0.038(4) 0.058(5) 0.000(3) -0.009(3) -0.020(3) C45 0.034(4) 0.039(4) 0.041(4) -0.009(3) -0.003(3) -0.017(3) C46 0.039(4) 0.046(4) 0.048(4) -0.005(3) -0.016(3) -0.008(3) C47 0.052(5) 0.059(6) 0.138(10) 0.041(6) -0.046(6) -0.034(5) C48 0.093(10) 0.079(8) 0.165(15) -0.065(9) 0.057(10) -0.038(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O14 2.392(6) . ? Eu1 O4 2.421(5) 1_655 ? Eu1 O2 2.428(5) . ? Eu1 O3 2.434(5) 2_656 ? Eu1 O13 2.442(5) . ? Eu1 O5 2.454(5) 1_645 ? Eu1 O6 2.515(6) 1_645 ? Eu1 O1 2.556(5) . ? Eu1 O3 2.829(5) 1_655 ? Eu1 C29 2.847(7) . ? Eu1 C45 2.855(7) 1_645 ? Eu1 C37 3.000(7) 1_655 ? O1 C29 1.275(10) . ? O2 C29 1.274(10) . ? O3 C37 1.278(9) . ? O3 Eu1 2.434(5) 2_656 ? O3 Eu1 2.829(5) 1_455 ? O4 C37 1.257(9) . ? O4 Eu1 2.421(5) 1_455 ? O5 C45 1.281(9) . ? O5 Eu1 2.453(5) 1_465 ? O6 C45 1.253(9) . ? O6 Eu1 2.515(6) 1_465 ? O7 C4 1.380(8) . ? O7 C22 1.455(9) . ? O8 C5 1.366(9) . ? O8 C46 1.445(9) . ? O9 C30 1.386(12) . ? O9 C11 1.403(10) . ? O10 C12 1.386(9) . ? O10 C47 1.425(11) . ? O11 C18 1.370(10) . ? O11 C38 1.456(11) . ? O12 C19 1.347(11) . ? O12 C48 1.409(13) . ? O14 C50 1.184(17) . ? C1 C21 1.504(11) . ? C1 C2 1.516(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.392(11) . ? C2 C3 1.414(10) . ? C3 C4 1.367(11) . ? C3 H3 0.9500 . ? C4 C5 1.413(10) . ? C5 C6 1.388(10) . ? C6 C7 1.407(11) . ? C6 H6 0.9500 . ? C7 C8 1.531(10) . ? C8 C9 1.510(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.404(11) . ? C9 C14 1.405(11) . ? C10 C11 1.378(12) . ? C10 H10 0.9500 . ? C11 C12 1.404(11) . ? C12 C13 1.370(11) . ? C13 C14 1.407(10) . ? C13 H13 0.9500 . ? C14 C15 1.518(10) . ? C15 C16 1.523(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.397(12) . ? C16 C21 1.406(10) . ? C17 C18 1.367(12) . ? C17 H17 0.9500 . ? C18 C19 1.430(11) . ? C19 C20 1.398(12) . ? C20 C21 1.383(11) . ? C20 H20 0.9500 . ? C22 C23 1.504(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.389(11) . ? C23 C24 1.395(11) . ? C24 C25 1.371(11) . ? C24 H24 0.9500 . ? C25 C26 1.379(11) . ? C25 H25 0.9500 . ? C26 C27 1.404(11) . ? C26 C29 1.508(10) . ? C27 C28 1.376(11) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C30 C31 1.528(12) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.356(14) . ? C31 C32 1.395(14) . ? C32 C33 1.380(12) . ? C32 H32 0.9500 . ? C33 C34 1.367(12) . ? C33 H33 0.9500 . ? C34 C35 1.387(12) . ? C34 C37 1.505(10) . ? C35 C36 1.381(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 Eu1 3.000(7) 1_455 ? C38 C39 1.499(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.368(11) . ? C39 C40 1.416(15) . ? C40 C41 1.378(14) . ? C40 H40 0.9500 . ? C41 C42 1.400(10) . ? C41 H41 0.9500 . ? C42 C43 1.391(11) . ? C42 C45 1.485(11) . ? C43 C44 1.384(11) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 Eu1 2.855(8) 1_465 ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 N50 1.34(2) . ? C50 H50 0.9500 . ? N50 C52 1.429(14) . ? N50 C53 1.49(2) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? N60 C60 1.31(3) . ? N60 C61 1.39(2) . ? N60 C62 1.45(2) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? O60 C60 1.36(3) . ? C60 H60 0.9500 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O70 C70 1.25(3) . ? N70 C70 1.20(3) . ? N70 C71 1.32(5) . ? N70 C72 1.36(3) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C70 H70 0.9500 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Eu1 O4 143.8(2) . 1_655 ? O14 Eu1 O2 90.8(2) . . ? O4 Eu1 O2 80.4(2) 1_655 . ? O14 Eu1 O3 90.37(19) . 2_656 ? O4 Eu1 O3 116.44(18) 1_655 2_656 ? O2 Eu1 O3 145.51(19) . 2_656 ? O14 Eu1 O13 78.14(19) . . ? O4 Eu1 O13 84.47(19) 1_655 . ? O2 Eu1 O13 136.71(18) . . ? O3 Eu1 O13 77.04(18) 2_656 . ? O14 Eu1 O5 129.44(18) . 1_645 ? O4 Eu1 O5 83.37(18) 1_655 1_645 ? O2 Eu1 O5 78.51(18) . 1_645 ? O3 Eu1 O5 74.29(17) 2_656 1_645 ? O13 Eu1 O5 139.52(17) . 1_645 ? O14 Eu1 O6 77.04(19) . 1_645 ? O4 Eu1 O6 131.17(19) 1_655 1_645 ? O2 Eu1 O6 71.9(2) . 1_645 ? O3 Eu1 O6 74.78(19) 2_656 1_645 ? O13 Eu1 O6 141.97(19) . 1_645 ? O5 Eu1 O6 52.56(17) 1_645 1_645 ? O14 Eu1 O1 73.26(19) . . ? O4 Eu1 O1 73.47(18) 1_655 . ? O2 Eu1 O1 53.04(18) . . ? O3 Eu1 O1 157.06(17) 2_656 . ? O13 Eu1 O1 83.80(17) . . ? O5 Eu1 O1 128.54(16) 1_645 . ? O6 Eu1 O1 115.49(18) 1_645 . ? O14 Eu1 O3 145.55(18) . 1_655 ? O4 Eu1 O3 48.99(16) 1_655 1_655 ? O2 Eu1 O3 122.55(19) . 1_655 ? O3 Eu1 O3 67.48(19) 2_656 1_655 ? O13 Eu1 O3 71.54(17) . 1_655 ? O5 Eu1 O3 71.38(16) 1_645 1_655 ? O6 Eu1 O3 118.70(17) 1_645 1_655 ? O1 Eu1 O3 118.12(17) . 1_655 ? O14 Eu1 C29 80.8(2) . . ? O4 Eu1 C29 75.9(2) 1_655 . ? O2 Eu1 C29 26.5(2) . . ? O3 Eu1 C29 166.8(2) 2_656 . ? O13 Eu1 C29 110.4(2) . . ? O5 Eu1 C29 103.8(2) 1_645 . ? O6 Eu1 C29 93.5(2) 1_645 . ? O1 Eu1 C29 26.6(2) . . ? O3 Eu1 C29 124.79(19) 1_655 . ? O14 Eu1 C45 102.9(2) . 1_645 ? O4 Eu1 C45 108.2(2) 1_655 1_645 ? O2 Eu1 C45 74.40(19) . 1_645 ? O3 Eu1 C45 71.75(19) 2_656 1_645 ? O13 Eu1 C45 148.77(19) . 1_645 ? O5 Eu1 C45 26.57(18) 1_645 1_645 ? O6 Eu1 C45 26.02(19) 1_645 1_645 ? O1 Eu1 C45 126.82(18) . 1_645 ? O3 Eu1 C45 94.99(18) 1_655 1_645 ? C29 Eu1 C45 100.5(2) . 1_645 ? O14 Eu1 C37 153.3(2) . 1_655 ? O4 Eu1 C37 23.89(19) 1_655 1_655 ? O2 Eu1 C37 101.4(2) . 1_655 ? O3 Eu1 C37 92.58(19) 2_656 1_655 ? O13 Eu1 C37 76.70(19) . 1_655 ? O5 Eu1 C37 76.68(18) 1_645 1_655 ? O6 Eu1 C37 129.24(18) 1_645 1_655 ? O1 Eu1 C37 95.19(19) . 1_655 ? O3 Eu1 C37 25.11(18) 1_655 1_655 ? C29 Eu1 C37 99.7(2) . 1_655 ? C45 Eu1 C37 103.2(2) 1_645 1_655 ? C29 O1 Eu1 89.6(4) . . ? C29 O2 Eu1 95.4(5) . . ? C37 O3 Eu1 162.5(5) . 2_656 ? C37 O3 Eu1 84.9(4) . 1_455 ? Eu1 O3 Eu1 112.52(19) 2_656 1_455 ? C37 O4 Eu1 104.8(4) . 1_455 ? C45 O5 Eu1 94.5(4) . 1_465 ? C45 O6 Eu1 92.3(4) . 1_465 ? C4 O7 C22 117.6(6) . . ? C5 O8 C46 117.1(6) . . ? C30 O9 C11 117.7(8) . . ? C12 O10 C47 117.0(6) . . ? C18 O11 C38 116.9(7) . . ? C19 O12 C48 117.3(8) . . ? C50 O14 Eu1 134.7(10) . . ? C21 C1 C2 116.1(6) . . ? C21 C1 H1A 108.3 . . ? C2 C1 H1A 108.3 . . ? C21 C1 H1B 108.3 . . ? C2 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C7 C2 C3 118.9(7) . . ? C7 C2 C1 124.0(7) . . ? C3 C2 C1 117.0(7) . . ? C4 C3 C2 121.5(7) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 O7 125.2(7) . . ? C3 C4 C5 119.7(7) . . ? O7 C4 C5 115.1(6) . . ? O8 C5 C6 125.2(7) . . ? O8 C5 C4 115.6(6) . . ? C6 C5 C4 119.2(7) . . ? C5 C6 C7 121.0(7) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 119.5(7) . . ? C2 C7 C8 123.9(7) . . ? C6 C7 C8 116.6(7) . . ? C9 C8 C7 113.2(6) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C14 118.3(7) . . ? C10 C9 C8 118.2(7) . . ? C14 C9 C8 123.5(7) . . ? C11 C10 C9 122.4(7) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 O9 128.3(7) . . ? C10 C11 C12 119.0(7) . . ? O9 C11 C12 112.7(7) . . ? C13 C12 O10 125.1(7) . . ? C13 C12 C11 119.4(7) . . ? O10 C12 C11 115.5(7) . . ? C12 C13 C14 122.2(7) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C9 C14 C13 118.6(7) . . ? C9 C14 C15 123.7(7) . . ? C13 C14 C15 117.6(7) . . ? C14 C15 C16 114.7(6) . . ? C14 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? C14 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C21 118.8(7) . . ? C17 C16 C15 118.7(6) . . ? C21 C16 C15 122.5(7) . . ? C18 C17 C16 122.8(7) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 O11 127.6(7) . . ? C17 C18 C19 119.1(7) . . ? O11 C18 C19 113.3(8) . . ? O12 C19 C20 126.1(7) . . ? O12 C19 C18 116.2(8) . . ? C20 C19 C18 117.7(8) . . ? C21 C20 C19 122.9(7) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C20 C21 C16 118.7(7) . . ? C20 C21 C1 118.0(7) . . ? C16 C21 C1 123.2(7) . . ? O7 C22 C23 114.4(6) . . ? O7 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? O7 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C28 C23 C24 118.0(7) . . ? C28 C23 C22 117.5(7) . . ? C24 C23 C22 124.5(7) . . ? C25 C24 C23 120.9(7) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 121.2(7) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 118.6(7) . . ? C25 C26 C29 122.3(7) . . ? C27 C26 C29 119.2(7) . . ? C28 C27 C26 120.0(7) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 121.4(7) . . ? C27 C28 H28 119.3 . . ? C23 C28 H28 119.3 . . ? O2 C29 O1 121.9(7) . . ? O2 C29 C26 118.4(7) . . ? O1 C29 C26 119.7(7) . . ? O2 C29 Eu1 58.1(4) . . ? O1 C29 Eu1 63.9(4) . . ? C26 C29 Eu1 175.1(5) . . ? O9 C30 C31 115.0(8) . . ? O9 C30 H30A 108.5 . . ? C31 C30 H30A 108.5 . . ? O9 C30 H30B 108.5 . . ? C31 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? C36 C31 C32 119.6(8) . . ? C36 C31 C30 118.0(8) . . ? C32 C31 C30 122.3(9) . . ? C33 C32 C31 120.3(9) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.1(9) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.2(8) . . ? C33 C34 C37 122.1(7) . . ? C35 C34 C37 118.6(7) . . ? C36 C35 C34 120.8(9) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C31 C36 C35 119.9(9) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? O4 C37 O3 121.2(7) . . ? O4 C37 C34 117.5(6) . . ? O3 C37 C34 121.2(7) . . ? O4 C37 Eu1 51.3(4) . 1_455 ? O3 C37 Eu1 69.9(4) . 1_455 ? C34 C37 Eu1 168.7(5) . 1_455 ? O11 C38 C39 112.8(8) . . ? O11 C38 H38A 109.0 . . ? C39 C38 H38A 109.0 . . ? O11 C38 H38B 109.0 . . ? C39 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C44 C39 C40 117.9(8) . . ? C44 C39 C38 118.5(9) . . ? C40 C39 C38 123.4(8) . . ? C41 C40 C39 120.8(8) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C42 120.4(9) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C43 C42 C41 118.4(8) . . ? C43 C42 C45 121.1(6) . . ? C41 C42 C45 120.4(8) . . ? C44 C43 C42 120.6(7) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C39 C44 C43 121.7(8) . . ? C39 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? O6 C45 O5 120.5(7) . . ? O6 C45 C42 121.1(7) . . ? O5 C45 C42 118.3(6) . . ? O6 C45 Eu1 61.7(4) . 1_465 ? O5 C45 Eu1 59.0(4) . 1_465 ? C42 C45 Eu1 175.1(5) . 1_465 ? O8 C46 H46A 109.5 . . ? O8 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O8 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O10 C47 H47A 109.5 . . ? O10 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O10 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O12 C48 H48A 109.5 . . ? O12 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O12 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O14 C50 N50 123.8(17) . . ? O14 C50 H50 118.1 . . ? N50 C50 H50 118.1 . . ? C50 N50 C52 125.6(15) . . ? C50 N50 C53 125.4(14) . . ? C52 N50 C53 105.2(13) . . ? N50 C52 H52A 109.5 . . ? N50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N50 C53 H53A 109.5 . . ? N50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C60 N60 C61 130.6(19) . . ? C60 N60 C62 118.1(19) . . ? C61 N60 C62 111.0(15) . . ? N60 C61 H61A 109.5 . . ? N60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N60 C60 O60 105(3) . . ? N60 C60 H60 127.4 . . ? O60 C60 H60 127.4 . . ? N60 C62 H62A 109.5 . . ? N60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C70 N70 C71 139(3) . . ? C70 N70 C72 121(3) . . ? C71 N70 C72 100(3) . . ? N70 C70 O70 129(3) . . ? N70 C70 H70 115.5 . . ? O70 C70 H70 115.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.976 _refine_diff_density_min -1.936 _refine_diff_density_rms 0.148 _database_code_depnum_ccdc_archive 'CCDC 936739'