# Copyright The Royal Society of Chemistry, 1999 # CCDC Number :182/1127 data_La(ntb)2(ClO4)3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C64 H78 Cl3 La N16 O15' _chemical_formula_weight 1556.68 _chemical_melting_point ? _chemical_compound_source ? 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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.4451(4) _cell_length_b 25.0336(6) _cell_length_c 16.9564(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.7940(10) _cell_angle_gamma 90.00 _cell_volume 7269.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method ? _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19052 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.1221 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.06 _reflns_number_total 9937 _reflns_number_observed 5936 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+43.0143P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9937 _refine_ls_number_parameters 892 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_obs 0.0767 _refine_ls_wR_factor_all 0.2264 _refine_ls_wR_factor_obs 0.1827 _refine_ls_goodness_of_fit_all 1.100 _refine_ls_goodness_of_fit_obs 1.178 _refine_ls_restrained_S_all 1.100 _refine_ls_restrained_S_obs 1.178 _refine_ls_shift/esd_max 0.072 _refine_ls_shift/esd_mean 0.010 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group La La 0.71357(3) 0.63506(3) 0.71406(4) 0.0307(2) Uani 1 d . . Cl1 Cl 0.2572(2) 0.6243(2) 0.3446(2) 0.0705(12) Uani 1 d . . Cl2 Cl 0.8483(2) 0.6223(2) 0.2089(2) 0.0620(10) Uani 1 d . . Cl3 Cl 0.5358(2) 0.6067(2) 0.2880(2) 0.0580(10) Uani 1 d . . O1 O 0.1810(5) 0.5150(4) 0.5873(6) 0.061(3) Uani 1 d . . O2 O 0.2585(8) 0.8537(6) 0.3019(9) 0.114(4) Uani 1 d . . O3 O 1.0819(8) 0.7568(7) 0.9068(12) 0.150(7) Uani 1 d . . O11 O 0.2273(8) 0.6591(6) 0.2767(12) 0.182(9) Uani 1 d . . O12 O 0.2484(9) 0.6481(10) 0.4128(13) 0.250(14) Uani 1 d . . O13 O 0.2156(6) 0.5760(5) 0.3217(8) 0.099(4) Uani 1 d . . O14 O 0.3386(5) 0.6159(5) 0.3639(8) 0.116(5) Uani 1 d . . O21 O 0.9186(8) 0.5954(7) 0.2372(11) 0.158(7) Uani 1 d . . O22 O 0.8447(8) 0.6664(6) 0.1536(9) 0.124(5) Uani 1 d . . O23 O 0.8354(9) 0.6425(6) 0.2801(7) 0.123(5) Uani 1 d . . O24 O 0.7833(8) 0.5884(6) 0.1605(6) 0.124(5) Uani 1 d . . O31 O 0.5505(7) 0.5548(5) 0.3232(7) 0.089(4) Uani 1 d . . O32 O 0.5989(6) 0.6425(4) 0.3349(6) 0.077(3) Uani 1 d . . O33 O 0.4683(6) 0.6247(5) 0.3007(8) 0.092(4) Uani 1 d . . O34 O 0.5293(8) 0.6059(5) 0.2018(6) 0.101(4) Uani 1 d . . N1 N 0.6442(5) 0.5578(4) 0.5904(5) 0.038(2) Uani 1 d . . N2 N 0.7811(4) 0.7128(4) 0.8389(5) 0.034(2) Uani 1 d . . N3 N 0.4162(7) 0.5566(5) 0.5831(8) 0.062(3) Uani 1 d . . N4 N 0.9705(9) 0.6384(9) 1.0121(9) 0.145(8) Uani 1 d . . N11 N 0.5650(4) 0.6438(4) 0.6280(6) 0.035(2) Uani 1 d . . N12 N 0.4747(5) 0.6518(4) 0.4970(6) 0.050(3) Uani 1 d . . H12 H 0.4492(5) 0.6462(4) 0.4424(6) 0.060 Uiso 1 calc R . N21 N 0.7209(5) 0.5358(4) 0.7596(5) 0.035(2) Uani 1 d . . N22 N 0.6551(5) 0.4626(4) 0.7617(6) 0.046(3) Uani 1 d . . H22 H 0.6197(5) 0.4373(4) 0.7431(6) 0.055 Uiso 1 calc R . N31 N 0.7666(5) 0.6253(4) 0.5929(6) 0.041(3) Uani 1 d . . N32 N 0.8045(5) 0.5721(4) 0.5081(6) 0.047(3) Uani 1 d . . H32 H 0.8065(5) 0.5441(4) 0.4776(6) 0.057 Uiso 1 calc R . N41 N 0.6985(5) 0.7346(4) 0.6684(5) 0.035(2) Uani 1 d . . N42 N 0.6426(5) 0.8094(4) 0.6888(6) 0.040(3) Uani 1 d . . H42 H 0.6314(5) 0.8363(4) 0.7158(6) 0.048 Uiso 1 calc R . N51 N 0.6709(5) 0.6385(4) 0.8439(5) 0.039(2) Uani 1 d . . N52 N 0.7203(6) 0.6259(5) 0.9828(6) 0.055(3) Uani 1 d . . H52 H 0.7511(6) 0.6297(5) 1.0363(6) 0.066 Uiso 1 calc R . N61 N 0.8638(4) 0.6337(4) 0.7915(5) 0.036(2) Uani 1 d . . N62 N 0.9762(5) 0.6781(5) 0.8343(6) 0.049(3) Uani 1 d . . H62 H 1.0096(5) 0.7044(5) 0.8546(6) 0.059 Uiso 1 calc R . C11 C 0.5810(7) 0.5856(5) 0.5172(7) 0.046(3) Uani 1 d . . H11A H 0.6050(7) 0.6031(5) 0.4805(7) 0.055 Uiso 1 calc R . H11B H 0.5433(7) 0.5586(5) 0.4826(7) 0.055 Uiso 1 calc R . C12 C 0.5391(5) 0.6258(5) 0.5469(7) 0.036(3) Uani 1 d . . C13 C 0.5109(6) 0.6838(5) 0.6268(8) 0.042(3) Uani 1 d . . C14 C 0.5089(6) 0.7153(6) 0.6955(9) 0.053(4) Uani 1 d . . H14 H 0.5467(6) 0.7107(6) 0.7513(9) 0.063 Uiso 1 calc R . C15 C 0.4506(7) 0.7527(6) 0.6786(10) 0.065(4) Uani 1 d . . H15 H 0.4481(7) 0.7752(6) 0.7228(10) 0.078 Uiso 1 calc R . C16 C 0.3941(8) 0.7577(7) 0.5949(11) 0.075(5) Uani 1 d . . H16 H 0.3538(8) 0.7835(7) 0.5845(11) 0.090 Uiso 1 calc R . C17 C 0.3950(7) 0.7264(7) 0.5271(10) 0.066(4) Uani 1 d . . H17 H 0.3573(7) 0.7302(7) 0.4712(10) 0.079 Uiso 1 calc R . C18 C 0.4552(6) 0.6893(6) 0.5473(8) 0.047(3) Uani 1 d . . C21 C 0.6102(6) 0.5157(5) 0.6271(7) 0.039(3) Uani 1 d . . H21A H 0.6020(6) 0.4829(5) 0.5923(7) 0.046 Uiso 1 calc R . H21B H 0.5588(6) 0.5276(5) 0.6266(7) 0.046 Uiso 1 calc R . C22 C 0.6631(6) 0.5039(5) 0.7158(8) 0.041(3) Uani 1 d . . C23 C 0.7544(6) 0.5119(5) 0.8435(7) 0.041(3) Uani 1 d . . C24 C 0.8152(6) 0.5281(5) 0.9156(7) 0.044(3) Uani 1 d . . H24 H 0.8441(6) 0.5594(5) 0.9154(7) 0.052 Uiso 1 calc R . C25 C 0.8325(8) 0.4983(7) 0.9865(8) 0.069(5) Uani 1 d . . H25 H 0.8742(8) 0.5086(7) 1.0370(8) 0.083 Uiso 1 calc R . C26 C 0.7888(9) 0.4515(7) 0.9860(9) 0.076(5) Uani 1 d . . H26 H 0.8021(9) 0.4317(7) 1.0372(9) 0.091 Uiso 1 calc R . C27 C 0.7279(8) 0.4332(7) 0.9152(9) 0.069(4) Uani 1 d . . H27 H 0.6997(8) 0.4015(7) 0.9150(9) 0.083 Uiso 1 calc R . C28 C 0.7118(7) 0.4659(6) 0.8443(7) 0.046(3) Uani 1 d . . C31 C 0.7029(6) 0.5356(6) 0.5595(7) 0.047(3) Uani 1 d . . H31A H 0.6762(6) 0.5188(6) 0.5032(7) 0.057 Uiso 1 calc R . H31B H 0.7336(6) 0.5077(6) 0.5992(7) 0.057 Uiso 1 calc R . C32 C 0.7562(6) 0.5786(5) 0.5524(7) 0.039(3) Uani 1 d . . C33 C 0.8496(6) 0.6179(5) 0.5203(8) 0.044(3) Uani 1 d . . C34 C 0.9097(7) 0.6330(7) 0.4931(8) 0.055(4) Uani 1 d . . H34 H 0.9252(7) 0.6107(7) 0.4568(8) 0.066 Uiso 1 calc R . C35 C 0.9453(7) 0.6813(7) 0.5207(8) 0.055(4) Uani 1 d . . H35 H 0.9869(7) 0.6923(7) 0.5043(8) 0.066 Uiso 1 calc R . C36 C 0.9216(6) 0.7141(6) 0.5724(8) 0.054(4) Uani 1 d . . H36 H 0.9475(6) 0.7473(6) 0.5902(8) 0.065 Uiso 1 calc R . C37 C 0.8598(6) 0.7001(6) 0.5998(7) 0.048(4) Uani 1 d . . H37 H 0.8421(6) 0.7235(6) 0.6329(7) 0.057 Uiso 1 calc R . C38 C 0.8272(6) 0.6502(6) 0.5753(7) 0.044(3) Uani 1 d . . C41 C 0.7289(6) 0.7612(5) 0.8197(7) 0.041(3) Uani 1 d . . H41A H 0.7600(6) 0.7931(5) 0.8465(7) 0.049 Uiso 1 calc R . H41B H 0.6880(6) 0.7563(5) 0.8438(7) 0.049 Uiso 1 calc R . C42 C 0.6909(6) 0.7695(5) 0.7237(7) 0.036(3) Uani 1 d . . C43 C 0.6493(6) 0.7550(5) 0.5885(7) 0.036(3) Uani 1 d . . C44 C 0.6313(6) 0.7344(5) 0.5071(7) 0.045(3) Uani 1 d . . H44 H 0.6557(6) 0.7029(5) 0.4974(7) 0.054 Uiso 1 calc R . C45 C 0.5765(6) 0.7616(6) 0.4413(7) 0.049(4) Uani 1 d . . H45 H 0.5645(6) 0.7493(6) 0.3848(7) 0.059 Uiso 1 calc R . C46 C 0.5386(7) 0.8060(6) 0.4540(9) 0.060(4) Uani 1 d . . H46 H 0.4990(7) 0.8219(6) 0.4065(9) 0.072 Uiso 1 calc R . C47 C 0.5560(7) 0.8287(5) 0.5344(8) 0.047(3) Uani 1 d . . H47 H 0.5316(7) 0.8603(5) 0.5433(8) 0.056 Uiso 1 calc R . C48 C 0.6124(6) 0.8008(5) 0.6003(7) 0.040(3) Uani 1 d . . C51 C 0.7906(6) 0.6905(5) 0.9230(7) 0.042(3) Uani 1 d . . H51A H 0.7919(6) 0.7201(5) 0.9623(7) 0.051 Uiso 1 calc R . H51B H 0.8409(6) 0.6711(5) 0.9466(7) 0.051 Uiso 1 calc R . C52 C 0.7254(6) 0.6533(5) 0.9166(7) 0.042(3) Uani 1 d . . C53 C 0.6574(7) 0.5903(5) 0.9518(7) 0.040(3) Uani 1 d . . C54 C 0.6259(8) 0.5524(6) 0.9888(8) 0.060(4) Uani 1 d . . H54 H 0.6470(8) 0.5458(6) 1.0482(8) 0.072 Uiso 1 calc R . C55 C 0.5629(9) 0.5247(6) 0.9358(11) 0.067(4) Uani 1 d . . H55 H 0.5409(9) 0.4978(6) 0.9597(11) 0.080 Uiso 1 calc R . C56 C 0.5296(7) 0.5335(6) 0.8501(9) 0.062(4) Uani 1 d . . H56 H 0.4855(7) 0.5130(6) 0.8167(9) 0.074 Uiso 1 calc R . C57 C 0.5593(6) 0.5719(6) 0.8111(8) 0.050(4) Uani 1 d . . H57 H 0.5370(6) 0.5784(6) 0.7517(8) 0.061 Uiso 1 calc R . C58 C 0.6245(6) 0.6007(5) 0.8650(7) 0.041(3) Uani 1 d . . C61 C 0.8579(6) 0.7270(6) 0.8348(8) 0.048(4) Uani 1 d . . H61A H 0.8499(6) 0.7527(6) 0.7879(8) 0.058 Uiso 1 calc R . H61B H 0.8908(6) 0.7445(6) 0.8885(8) 0.058 Uiso 1 calc R . C62 C 0.8987(6) 0.6788(5) 0.8208(7) 0.038(3) Uani 1 d . . C63 C 0.9212(5) 0.5994(6) 0.7831(6) 0.037(3) Uani 1 d . . C64 C 0.9173(7) 0.5464(6) 0.7554(7) 0.051(4) Uani 1 d . . H64 H 0.8695(7) 0.5272(6) 0.7376(7) 0.061 Uiso 1 calc R . C65 C 0.9855(8) 0.5227(6) 0.7548(9) 0.061(4) Uani 1 d . . H65 H 0.9843(8) 0.4871(6) 0.7349(9) 0.073 Uiso 1 calc R . C66 C 1.0565(8) 0.5515(7) 0.7838(9) 0.067(5) Uani 1 d . . H66 H 1.1027(8) 0.5342(7) 0.7849(9) 0.080 Uiso 1 calc R . C67 C 1.0610(7) 0.6030(8) 0.8101(9) 0.069(5) Uani 1 d . . H67 H 1.1090(7) 0.6221(8) 0.8282(9) 0.083 Uiso 1 calc R . C68 C 0.9926(6) 0.6269(6) 0.8095(8) 0.045(3) Uani 1 d . . C70 C 0.0857(10) 0.5489(8) 0.4576(12) 0.106(7) Uani 1 d . . H70A H 0.0379(10) 0.5702(8) 0.4340(12) 0.159 Uiso 1 calc R . H70B H 0.0759(10) 0.5127(8) 0.4341(12) 0.159 Uiso 1 calc R . H70C H 0.1271(10) 0.5655(8) 0.4429(12) 0.159 Uiso 1 calc R . C71 C 0.1109(9) 0.5462(7) 0.5535(12) 0.088(6) Uani 1 d . . H71A H 0.1205(9) 0.5827(7) 0.5777(12) 0.105 Uiso 1 calc R . H71B H 0.0691(9) 0.5297(7) 0.5688(12) 0.105 Uiso 1 calc R . C72 C 0.2055(9) 0.5074(7) 0.6762(10) 0.077(5) Uani 1 d . . H72A H 0.1654(9) 0.4868(7) 0.6891(10) 0.092 Uiso 1 calc R . H72B H 0.2115(9) 0.5425(7) 0.7048(10) 0.092 Uiso 1 calc R . C73 C 0.2827(10) 0.4776(8) 0.7099(11) 0.096(6) Uani 1 d . . H73A H 0.2988(10) 0.4726(8) 0.7714(11) 0.145 Uiso 1 calc R . H73B H 0.3226(10) 0.4982(8) 0.6978(11) 0.145 Uiso 1 calc R . H73C H 0.2766(10) 0.4426(8) 0.6821(11) 0.145 Uiso 1 calc R . C74 C 0.3246(11) 0.6198(8) 0.6263(15) 0.114(8) Uani 1 d . . C75 C 0.3774(9) 0.5832(7) 0.6013(10) 0.066(4) Uani 1 d . . C76 C 0.1664(23) 0.8008(13) 0.1906(18) 0.228(18) Uani 1 d . . H76A H 0.1471(23) 0.7647(13) 0.1717(18) 0.342 Uiso 1 calc R . H76B H 0.1860(23) 0.8169(13) 0.1497(18) 0.342 Uiso 1 calc R . H76C H 0.1238(23) 0.8226(13) 0.1945(18) 0.342 Uiso 1 calc R . C77 C 0.2338(16) 0.7977(10) 0.2795(18) 0.141(9) Uani 1 d . . H77A H 0.2151(16) 0.7817(10) 0.3218(18) 0.169 Uiso 1 calc R . H77B H 0.2776(16) 0.7760(10) 0.2768(18) 0.169 Uiso 1 calc R . C78 C 0.3181(11) 0.8561(11) 0.3801(18) 0.158(12) Uani 1 d . . H78A H 0.3603(11) 0.8312(11) 0.3814(18) 0.190 Uiso 1 calc R . H78B H 0.2985(11) 0.8447(11) 0.4245(18) 0.190 Uiso 1 calc R . C79 C 0.3494(12) 0.9107(11) 0.3981(14) 0.140(9) Uani 1 d . . H79A H 0.3917(12) 0.9116(11) 0.4541(14) 0.210 Uiso 1 calc R . H79B H 0.3078(12) 0.9352(11) 0.3977(14) 0.210 Uiso 1 calc R . H79C H 0.3695(12) 0.9217(11) 0.3546(14) 0.210 Uiso 1 calc R . C80 C 1.0453(15) 0.7973(11) 0.7719(19) 0.174(11) Uani 1 d . . H80A H 1.0314(15) 0.8309(11) 0.7403(19) 0.260 Uiso 1 calc R . H80B H 1.0018(15) 0.7720(11) 0.7497(19) 0.260 Uiso 1 calc R . H80C H 1.0918(15) 0.7822(11) 0.7655(19) 0.260 Uiso 1 calc R . C81 C 1.0613(11) 0.8072(10) 0.8606(13) 0.099(7) Uani 1 d . . H81A H 1.0146(11) 0.8228(10) 0.8675(13) 0.119 Uiso 1 calc R . H81B H 1.1049(11) 0.8329(10) 0.8834(13) 0.119 Uiso 1 calc R . C82 C 1.1413(11) 0.7571(11) 0.9762(14) 0.127(9) Uani 1 d . . H82A H 1.1309(11) 0.7815(11) 1.0166(14) 0.153 Uiso 1 calc R . H82B H 1.1866(11) 0.7714(11) 0.9649(14) 0.153 Uiso 1 calc R . C83 C 1.1631(12) 0.7022(11) 1.0179(15) 0.143(9) Uani 1 d . . H83A H 1.2090(12) 0.7057(11) 1.0706(15) 0.214 Uiso 1 calc R . H83B H 1.1751(12) 0.6779(11) 0.9791(15) 0.214 Uiso 1 calc R . H83C H 1.1193(12) 0.6880(11) 1.0309(15) 0.214 Uiso 1 calc R . C84 C 1.0725(10) 0.5842(8) 1.1334(11) 0.095(6) Uani 1 d . . C85 C 1.0154(9) 0.6150(8) 1.0656(10) 0.080(6) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La 0.0318(3) 0.0348(5) 0.0249(3) -0.0037(4) 0.0097(2) -0.0004(3) Cl1 0.054(2) 0.078(4) 0.063(2) -0.023(2) 0.002(2) 0.013(2) Cl2 0.078(2) 0.055(3) 0.044(2) 0.003(2) 0.012(2) 0.015(2) Cl3 0.080(2) 0.051(3) 0.055(2) 0.000(2) 0.039(2) -0.016(2) O1 0.076(6) 0.056(8) 0.066(6) -0.004(5) 0.045(5) 0.002(5) O2 0.113(10) 0.115(14) 0.106(10) -0.003(10) 0.033(8) -0.013(9) O3 0.097(9) 0.098(14) 0.182(16) 0.008(12) -0.033(10) -0.040(8) O11 0.129(11) 0.099(14) 0.219(19) 0.084(13) -0.049(11) -0.018(9) O12 0.134(13) 0.400(34) 0.220(20) -0.241(23) 0.073(13) -0.030(16) O13 0.090(7) 0.074(11) 0.109(9) -0.001(7) 0.011(7) -0.017(7) O14 0.057(6) 0.134(13) 0.130(10) -0.076(9) 0.003(6) -0.001(6) O21 0.110(10) 0.141(16) 0.216(17) 0.013(13) 0.055(11) 0.071(10) O22 0.152(11) 0.095(13) 0.111(10) 0.056(9) 0.030(9) 0.010(9) O23 0.180(13) 0.123(13) 0.068(8) -0.029(8) 0.047(8) 0.027(10) O24 0.167(11) 0.127(13) 0.042(7) -0.008(7) -0.003(7) -0.076(10) O31 0.165(11) 0.048(9) 0.067(7) 0.013(6) 0.059(7) 0.004(7) O32 0.094(7) 0.079(9) 0.059(6) -0.016(6) 0.032(5) -0.041(6) O33 0.085(7) 0.089(10) 0.114(9) -0.015(7) 0.051(7) -0.023(6) O34 0.178(11) 0.092(11) 0.046(6) -0.004(6) 0.056(7) -0.048(8) N1 0.042(5) 0.051(8) 0.019(5) -0.003(5) 0.011(4) -0.002(4) N2 0.033(4) 0.043(8) 0.021(5) -0.003(4) 0.006(4) -0.003(4) N3 0.074(8) 0.038(10) 0.070(9) 0.003(7) 0.021(7) -0.013(6) N4 0.089(10) 0.266(26) 0.067(10) 0.047(13) 0.013(8) 0.073(13) N11 0.034(4) 0.029(7) 0.038(6) -0.005(5) 0.007(4) -0.008(4) N12 0.058(6) 0.043(9) 0.034(6) 0.004(5) -0.002(5) -0.013(5) N21 0.042(5) 0.031(7) 0.029(5) -0.002(5) 0.012(4) 0.000(4) N22 0.049(5) 0.051(9) 0.032(6) 0.013(5) 0.009(4) -0.011(5) N31 0.058(6) 0.031(8) 0.044(6) -0.009(5) 0.031(5) -0.006(5) N32 0.066(6) 0.043(9) 0.046(6) -0.015(6) 0.036(5) 0.003(5) N41 0.039(5) 0.036(7) 0.030(5) -0.006(5) 0.015(4) 0.001(4) N42 0.052(6) 0.031(8) 0.043(6) -0.002(5) 0.023(5) 0.004(5) N51 0.041(5) 0.044(8) 0.034(5) -0.010(5) 0.018(4) 0.002(5) N52 0.067(7) 0.070(10) 0.029(6) 0.003(6) 0.017(5) 0.003(6) N61 0.023(4) 0.050(8) 0.031(5) -0.019(5) 0.005(3) 0.003(4) N62 0.039(5) 0.063(10) 0.043(6) -0.005(6) 0.012(4) -0.005(5) C11 0.059(7) 0.049(11) 0.021(6) -0.006(6) 0.005(5) -0.005(6) C12 0.030(5) 0.035(9) 0.031(6) 0.009(6) -0.005(4) -0.007(5) C13 0.035(6) 0.040(10) 0.049(8) 0.007(7) 0.013(5) -0.008(5) C14 0.033(6) 0.062(11) 0.064(9) 0.005(8) 0.019(6) 0.006(6) C15 0.045(7) 0.061(12) 0.091(11) -0.029(9) 0.026(8) 0.000(7) C16 0.050(8) 0.063(13) 0.099(13) -0.001(10) 0.013(8) 0.016(7) C17 0.045(7) 0.063(13) 0.069(10) 0.023(9) -0.004(7) -0.002(7) C18 0.046(7) 0.034(10) 0.052(8) -0.002(7) 0.007(6) -0.015(6) C21 0.043(6) 0.037(9) 0.033(7) -0.001(6) 0.011(5) -0.009(5) C22 0.044(6) 0.034(10) 0.046(7) -0.002(7) 0.018(6) -0.006(5) C23 0.045(6) 0.045(10) 0.029(7) 0.010(6) 0.010(5) 0.008(6) C24 0.050(7) 0.048(10) 0.027(7) -0.003(6) 0.009(5) 0.001(6) C25 0.068(9) 0.088(15) 0.033(8) -0.009(8) -0.002(6) -0.006(8) C26 0.090(11) 0.088(16) 0.043(9) 0.020(9) 0.016(8) -0.002(9) C27 0.086(10) 0.066(13) 0.046(9) 0.018(8) 0.013(7) -0.004(8) C28 0.054(7) 0.043(11) 0.035(7) -0.001(7) 0.009(6) 0.003(6) C31 0.055(7) 0.055(11) 0.032(7) -0.010(6) 0.016(5) -0.008(6) C32 0.046(6) 0.036(10) 0.040(7) -0.003(6) 0.022(5) 0.003(5) C33 0.042(6) 0.042(11) 0.047(7) 0.008(6) 0.018(5) 0.012(5) C34 0.055(7) 0.069(13) 0.054(8) 0.012(8) 0.035(6) 0.023(8) C35 0.040(7) 0.075(13) 0.059(9) 0.029(8) 0.029(6) 0.017(7) C36 0.045(7) 0.062(11) 0.050(8) 0.027(8) 0.012(6) 0.003(6) C37 0.045(7) 0.068(12) 0.033(7) 0.014(7) 0.018(5) 0.012(6) C38 0.048(6) 0.054(12) 0.037(7) -0.004(7) 0.023(5) 0.008(6) C41 0.046(6) 0.030(9) 0.050(8) -0.007(6) 0.023(6) -0.005(5) C42 0.043(6) 0.028(9) 0.037(7) 0.004(6) 0.014(5) 0.000(5) C43 0.038(6) 0.030(9) 0.043(7) -0.001(6) 0.020(5) 0.008(5) C44 0.048(7) 0.047(10) 0.045(8) 0.006(7) 0.022(6) 0.004(6) C45 0.051(7) 0.069(12) 0.030(7) 0.013(7) 0.018(6) 0.002(7) C46 0.040(7) 0.074(13) 0.068(10) 0.023(9) 0.024(6) 0.009(7) C47 0.056(7) 0.033(10) 0.052(9) 0.003(7) 0.020(6) -0.002(6) C48 0.044(6) 0.040(10) 0.043(7) 0.011(6) 0.025(5) -0.003(5) C51 0.052(7) 0.039(10) 0.030(7) -0.012(6) 0.008(5) 0.001(6) C52 0.037(6) 0.055(10) 0.031(7) -0.003(6) 0.010(5) 0.000(5) C53 0.060(7) 0.035(10) 0.031(7) 0.008(6) 0.024(6) 0.009(6) C54 0.085(10) 0.073(13) 0.031(7) 0.002(8) 0.031(7) 0.003(8) C55 0.082(10) 0.053(13) 0.083(12) -0.009(9) 0.052(9) -0.007(8) C56 0.055(7) 0.076(13) 0.071(10) -0.016(9) 0.043(8) -0.019(7) C57 0.038(6) 0.070(12) 0.044(8) -0.012(7) 0.016(6) -0.005(6) C58 0.052(7) 0.035(9) 0.045(8) 0.000(6) 0.030(6) 0.009(6) C61 0.036(6) 0.063(11) 0.045(8) -0.001(7) 0.013(5) -0.009(6) C62 0.029(6) 0.046(10) 0.028(6) 0.001(6) -0.002(5) 0.008(5) C63 0.030(5) 0.055(11) 0.018(6) -0.002(6) -0.001(4) 0.008(5) C64 0.047(7) 0.066(12) 0.034(7) -0.001(7) 0.009(5) 0.012(6) C65 0.079(10) 0.044(12) 0.058(9) 0.002(8) 0.024(8) 0.014(7) C66 0.071(10) 0.077(15) 0.057(9) 0.007(9) 0.028(7) 0.033(9) C67 0.043(7) 0.109(16) 0.060(10) 0.018(10) 0.026(7) 0.013(8) C68 0.034(6) 0.050(11) 0.052(8) 0.004(7) 0.017(5) 0.019(6) C70 0.100(13) 0.103(19) 0.118(17) 0.017(13) 0.045(12) 0.028(11) C71 0.073(10) 0.091(16) 0.103(14) -0.019(12) 0.037(10) 0.017(9) C72 0.102(12) 0.081(15) 0.074(11) -0.007(10) 0.063(10) -0.016(10) C73 0.103(13) 0.108(18) 0.080(13) 0.005(12) 0.037(10) 0.000(11) C74 0.119(14) 0.084(18) 0.185(21) -0.012(14) 0.110(15) -0.004(11) C75 0.076(10) 0.054(14) 0.070(11) 0.003(9) 0.030(8) -0.012(8) C76 0.384(51) 0.186(38) 0.140(27) -0.057(24) 0.128(32) -0.132(34) C77 0.187(24) 0.091(24) 0.149(24) -0.014(19) 0.067(20) -0.033(17) C78 0.066(11) 0.162(29) 0.200(27) 0.088(22) -0.006(14) -0.013(13) C79 0.118(16) 0.174(28) 0.118(18) -0.025(18) 0.031(14) -0.053(17) C80 0.183(25) 0.144(29) 0.211(33) 0.042(24) 0.094(24) -0.030(19) C81 0.098(13) 0.123(22) 0.080(14) -0.002(14) 0.037(11) -0.021(12) C82 0.085(13) 0.155(27) 0.117(18) -0.059(17) 0.010(13) -0.008(14) C83 0.097(15) 0.162(28) 0.152(22) 0.034(20) 0.025(14) 0.021(16) C84 0.098(12) 0.099(17) 0.073(12) 0.020(11) 0.013(9) 0.037(10) C85 0.067(9) 0.130(18) 0.047(9) 0.012(10) 0.028(8) 0.026(9) _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 La N61 2.589(7) . ? La N21 2.590(10) . ? La N11 2.591(8) . ? La N41 2.594(10) . ? La N31 2.595(8) . ? La N51 2.601(8) . ? La N1 2.791(9) . ? La N2 2.803(9) . ? Cl1 O12 1.364(14) . ? Cl1 O11 1.385(14) . ? Cl1 O13 1.407(12) . ? Cl1 O14 1.427(10) . ? Cl2 O21 1.379(12) . ? Cl2 O23 1.408(11) . ? Cl2 O22 1.435(12) . ? Cl2 O24 1.450(11) . ? Cl3 O33 1.414(10) . ? Cl3 O31 1.414(11) . ? Cl3 O34 1.421(9) . ? Cl3 O32 1.450(9) . ? O1 C72 1.42(2) . ? O1 C71 1.44(2) . ? O2 C78 1.37(2) . ? O2 C77 1.48(2) . ? O3 C82 1.28(2) . ? O3 C81 1.46(2) . ? N1 C31 1.475(13) . ? N1 C21 1.477(13) . ? N1 C11 1.519(14) . ? N2 C51 1.479(13) . ? N2 C61 1.487(12) . ? N2 C41 1.506(14) . ? N3 C75 1.10(2) . ? N4 C85 1.14(2) . ? N11 C12 1.355(13) . ? N11 C13 1.409(15) . ? N12 C12 1.342(14) . ? N12 C18 1.40(2) . ? N21 C22 1.319(14) . ? N21 C23 1.453(13) . ? N22 C22 1.333(14) . ? N22 C28 1.406(14) . ? N31 C32 1.333(14) . ? N31 C38 1.405(14) . ? N32 C32 1.372(12) . ? N32 C33 1.39(2) . ? N41 C42 1.325(14) . ? N41 C43 1.417(13) . ? N42 C42 1.323(14) . ? N42 C48 1.410(14) . ? N51 C52 1.323(13) . ? N51 C58 1.409(15) . ? N52 C52 1.348(14) . ? N52 C53 1.40(2) . ? N61 C62 1.303(14) . ? N61 C63 1.411(14) . ? N62 C62 1.361(13) . ? N62 C68 1.42(2) . ? C11 C12 1.47(2) . ? C18 C13 1.36(2) . ? C18 C17 1.39(2) . ? C13 C14 1.42(2) . ? C14 C15 1.37(2) . ? C15 C16 1.42(2) . ? C16 C17 1.40(2) . ? C21 C22 1.49(2) . ? C23 C24 1.378(15) . ? C23 C28 1.40(2) . ? C24 C25 1.35(2) . ? C25 C26 1.42(2) . ? C26 C27 1.38(2) . ? C27 C28 1.39(2) . ? C31 C32 1.49(2) . ? C33 C34 1.40(2) . ? C33 C38 1.41(2) . ? C34 C35 1.37(2) . ? C35 C36 1.39(2) . ? C36 C37 1.426(15) . ? C37 C38 1.38(2) . ? C41 C42 1.53(2) . ? C43 C48 1.39(2) . ? C43 C44 1.39(2) . ? C44 C45 1.38(2) . ? C45 C46 1.37(2) . ? C46 C47 1.40(2) . ? C47 C48 1.40(2) . ? C51 C52 1.49(2) . ? C53 C54 1.38(2) . ? C53 C58 1.391(15) . ? C54 C55 1.36(2) . ? C55 C56 1.37(2) . ? C56 C57 1.39(2) . ? C57 C58 1.41(2) . ? C61 C62 1.49(2) . ? C63 C64 1.40(2) . ? C63 C68 1.40(2) . ? C64 C65 1.40(2) . ? C65 C66 1.41(2) . ? C66 C67 1.36(2) . ? C67 C68 1.39(2) . ? C70 C71 1.52(2) . ? C72 C73 1.52(2) . ? C74 C75 1.51(2) . ? C76 C77 1.56(4) . ? C78 C79 1.47(3) . ? C80 C81 1.44(3) . ? C82 C83 1.53(3) . ? C84 C85 1.46(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 N61 La N21 84.8(3) . . ? N61 La N11 174.6(3) . . ? N21 La N11 100.1(3) . . ? N61 La N41 98.1(3) . . ? N21 La N41 176.8(2) . . ? N11 La N41 77.1(3) . . ? N61 La N31 75.7(3) . . ? N21 La N31 98.8(3) . . ? N11 La N31 101.1(3) . . ? N41 La N31 83.4(3) . . ? N61 La N51 100.1(3) . . ? N21 La N51 77.2(3) . . ? N11 La N51 83.4(3) . . ? N41 La N51 100.8(3) . . ? N31 La N51 174.5(3) . . ? N61 La N1 118.5(3) . . ? N21 La N1 61.2(3) . . ? N11 La N1 62.7(3) . . ? N41 La N1 118.3(3) . . ? N31 La N1 62.7(3) . . ? N51 La N1 117.4(3) . . ? N61 La N2 62.2(3) . . ? N21 La N2 118.8(3) . . ? N11 La N2 116.6(3) . . ? N41 La N2 61.8(3) . . ? N31 La N2 118.1(3) . . ? N51 La N2 61.8(3) . . ? N1 La N2 179.1(2) . . ? O12 Cl1 O11 107.0(15) . . ? O12 Cl1 O13 112.6(12) . . ? O11 Cl1 O13 107.7(9) . . ? O12 Cl1 O14 108.4(9) . . ? O11 Cl1 O14 110.1(10) . . ? O13 Cl1 O14 110.9(7) . . ? O21 Cl2 O23 108.2(10) . . ? O21 Cl2 O22 114.3(10) . . ? O23 Cl2 O22 107.6(9) . . ? O21 Cl2 O24 112.6(11) . . ? O23 Cl2 O24 109.1(9) . . ? O22 Cl2 O24 104.7(8) . . ? O33 Cl3 O31 105.7(7) . . ? O33 Cl3 O34 114.8(8) . . ? O31 Cl3 O34 110.6(7) . . ? O33 Cl3 O32 107.0(7) . . ? O31 Cl3 O32 110.3(7) . . ? O34 Cl3 O32 108.5(6) . . ? C72 O1 C71 112.6(11) . . ? C78 O2 C77 110.4(19) . . ? C82 O3 C81 117.0(18) . . ? C31 N1 C21 111.3(10) . . ? C31 N1 C11 108.9(8) . . ? C21 N1 C11 110.7(8) . . ? C31 N1 La 109.6(6) . . ? C21 N1 La 109.0(6) . . ? C11 N1 La 107.1(7) . . ? C51 N2 C61 111.2(8) . . ? C51 N2 C41 110.4(8) . . ? C61 N2 C41 109.9(9) . . ? C51 N2 La 109.1(7) . . ? C61 N2 La 107.2(6) . . ? C41 N2 La 109.0(6) . . ? C12 N11 C13 103.9(9) . . ? C12 N11 La 116.4(6) . . ? C13 N11 La 131.6(7) . . ? C12 N12 C18 107.9(10) . . ? C22 N21 C23 105.2(10) . . ? C22 N21 La 118.2(8) . . ? C23 N21 La 130.1(8) . . ? C22 N22 C28 109.5(10) . . ? C32 N31 C38 104.7(9) . . ? C32 N31 La 117.7(7) . . ? C38 N31 La 133.6(8) . . ? C32 N32 C33 107.3(10) . . ? C42 N41 C43 104.0(9) . . ? C42 N41 La 116.7(7) . . ? C43 N41 La 126.2(7) . . ? C42 N42 C48 107.1(10) . . ? C52 N51 C58 105.9(9) . . ? C52 N51 La 115.7(6) . . ? C58 N51 La 126.6(7) . . ? C52 N52 C53 108.4(10) . . ? C62 N61 C63 106.4(9) . . ? C62 N61 La 117.8(7) . . ? C63 N61 La 131.3(7) . . ? C62 N62 C68 106.8(10) . . ? C12 C11 N1 112.2(8) . . ? N12 C12 N11 112.1(11) . . ? N12 C12 C11 124.9(10) . . ? N11 C12 C11 122.9(9) . . ? C13 C18 C17 123.5(14) . . ? C13 C18 N12 105.3(11) . . ? C17 C18 N12 131.2(12) . . ? C18 C13 N11 110.9(11) . . ? C18 C13 C14 121.0(12) . . ? N11 C13 C14 128.1(10) . . ? C15 C14 C13 117.7(12) . . ? C14 C15 C16 119.7(14) . . ? C17 C16 C15 123.0(13) . . ? C18 C17 C16 115.1(13) . . ? N1 C21 C22 110.3(8) . . ? N21 C22 N22 112.5(10) . . ? N21 C22 C21 122.5(11) . . ? N22 C22 C21 124.8(10) . . ? C24 C23 C28 120.6(11) . . ? C24 C23 N21 131.1(12) . . ? C28 C23 N21 108.3(10) . . ? C25 C24 C23 118.3(13) . . ? C24 C25 C26 120.2(13) . . ? C27 C26 C25 123.7(14) . . ? C26 C27 C28 113.6(14) . . ? C27 C28 C23 123.5(12) . . ? C27 C28 N22 131.9(13) . . ? C23 C28 N22 104.6(10) . . ? N1 C31 C32 110.4(11) . . ? N31 C32 N32 112.7(10) . . ? N31 C32 C31 124.4(10) . . ? N32 C32 C31 122.7(11) . . ? N32 C33 C34 132.8(12) . . ? N32 C33 C38 105.4(10) . . ? C34 C33 C38 121.7(13) . . ? C35 C34 C33 117.6(12) . . ? C34 C35 C36 121.0(11) . . ? C35 C36 C37 122.5(14) . . ? C38 C37 C36 115.9(12) . . ? C37 C38 N31 128.9(10) . . ? C37 C38 C33 121.1(11) . . ? N31 C38 C33 109.8(12) . . ? N2 C41 C42 110.0(9) . . ? N42 C42 N41 114.3(10) . . ? N42 C42 C41 123.0(11) . . ? N41 C42 C41 122.4(10) . . ? C48 C43 C44 120.1(11) . . ? C48 C43 N41 109.4(10) . . ? C44 C43 N41 130.3(11) . . ? C45 C44 C43 116.9(12) . . ? C46 C45 C44 122.5(12) . . ? C45 C46 C47 122.4(12) . . ? C46 C47 C48 114.2(12) . . ? C43 C48 C47 123.8(11) . . ? C43 C48 N42 105.1(10) . . ? C47 C48 N42 131.1(12) . . ? N2 C51 C52 111.2(9) . . ? N51 C52 N52 111.7(11) . . ? N51 C52 C51 123.8(10) . . ? N52 C52 C51 124.1(10) . . ? C54 C53 C58 121.2(12) . . ? C54 C53 N52 134.2(11) . . ? C58 C53 N52 104.7(10) . . ? C55 C54 C53 116.7(12) . . ? C54 C55 C56 123.6(14) . . ? C55 C56 C57 121.1(13) . . ? C56 C57 C58 115.9(12) . . ? C53 C58 N51 109.1(10) . . ? C53 C58 C57 121.6(12) . . ? N51 C58 C57 129.1(11) . . ? C62 C61 N2 111.1(10) . . ? N61 C62 N62 113.1(10) . . ? N61 C62 C61 123.8(9) . . ? N62 C62 C61 123.0(11) . . ? C64 C63 C68 119.8(10) . . ? C64 C63 N61 131.5(10) . . ? C68 C63 N61 108.7(12) . . ? C65 C64 C63 118.1(12) . . ? C64 C65 C66 120.1(15) . . ? C67 C66 C65 122.4(13) . . ? C66 C67 C68 117.4(14) . . ? C67 C68 C63 122.2(14) . . ? C67 C68 N62 132.8(13) . . ? C63 C68 N62 105.0(9) . . ? O1 C71 C70 108.9(12) . . ? O1 C72 C73 110.6(12) . . ? N3 C75 C74 179.7(15) . . ? O2 C77 C76 105.2(21) . . ? O2 C78 C79 110.6(19) . . ? C80 C81 O3 108.8(21) . . ? O3 C82 C83 114.3(20) . . ? N4 C85 C84 179.1(24) . . ? _refine_diff_density_max 1.776 _refine_diff_density_min -1.239 _refine_diff_density_rms 0.141 #=END data_Nd(ntb)(ClO4)3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C64 H78 Cl3 N16 Nd O15' _chemical_formula_weight 1562.01 _chemical_melting_point ? _chemical_compound_source ? 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' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2235(7) _cell_length_b 24.8434(10) _cell_length_c 16.8575(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.7930(10) _cell_angle_gamma 90.00 _cell_volume 7086.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method ? _exptl_crystal_F_000 3220 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30589 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.06 _reflns_number_total 12398 _reflns_number_observed 7610 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+1.6750P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00128(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12398 _refine_ls_number_parameters 893 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_obs 0.0618 _refine_ls_wR_factor_all 0.1592 _refine_ls_wR_factor_obs 0.1250 _refine_ls_goodness_of_fit_all 1.120 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max -0.098 _refine_ls_shift/esd_mean 0.009 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.712209(14) 0.634908(10) 0.712481(15) 0.02696(6) Uani 1 d . . Cl1 Cl 0.25716(9) 0.62382(6) 0.34350(10) 0.0626(5) Uani 1 d . . Cl2 Cl 0.84356(9) 0.62222(5) 0.20379(8) 0.0542(4) Uani 1 d . . Cl3 Cl 0.53549(9) 0.60727(6) 0.28733(9) 0.0554(4) Uani 1 d . . O1 O 0.1799(2) 0.51300(14) 0.5863(2) 0.0535(11) Uani 1 d . . O2 O 0.2570(3) 0.8534(2) 0.3012(3) 0.098(2) Uani 1 d . . O3 O 1.0804(3) 0.7558(2) 0.9051(4) 0.123(2) Uani 1 d . . O11 O 0.2277(4) 0.6570(2) 0.2746(5) 0.178(3) Uani 1 d . . O12 O 0.2486(4) 0.6472(3) 0.4122(5) 0.216(3) Uani 1 d . . O13 O 0.2153(3) 0.5748(2) 0.3217(3) 0.085(2) Uani 1 d . . O14 O 0.3385(2) 0.6147(2) 0.3640(3) 0.094(2) Uani 1 d . . O21 O 0.9119(3) 0.5914(2) 0.2283(4) 0.127(2) Uani 1 d . . O22 O 0.8416(3) 0.6653(2) 0.1489(3) 0.109(2) Uani 1 d . . O23 O 0.8346(3) 0.6425(2) 0.2774(3) 0.102(2) Uani 1 d . . O24 O 0.7775(3) 0.5887(2) 0.1584(3) 0.106(2) Uani 1 d . . O31 O 0.5485(3) 0.5553(2) 0.3235(2) 0.082(2) Uani 1 d . . O32 O 0.5973(3) 0.6442(2) 0.3341(2) 0.0749(14) Uani 1 d . . O33 O 0.4656(3) 0.6258(2) 0.2964(4) 0.109(2) Uani 1 d . . O34 O 0.5322(3) 0.6052(2) 0.2033(2) 0.086(2) Uani 1 d . . N1 N 0.6439(2) 0.55935(15) 0.5906(2) 0.0326(11) Uani 1 d . . N2 N 0.7784(2) 0.71165(15) 0.8357(2) 0.0298(10) Uani 1 d . . N3 N 0.4140(3) 0.5557(2) 0.5810(3) 0.060(2) Uani 1 d . . N4 N 0.9704(3) 0.6404(3) 1.0105(4) 0.121(3) Uani 1 d . . N11 N 0.5657(2) 0.64398(14) 0.6284(2) 0.0305(10) Uani 1 d . . N12 N 0.4737(2) 0.6526(2) 0.4985(3) 0.0443(13) Uani 1 d . . H12A H 0.4484(2) 0.6472(2) 0.4448(3) 0.053 Uiso 1 calc R . N21 N 0.7221(2) 0.5385(2) 0.7610(2) 0.0308(10) Uani 1 d . . N22 N 0.6569(2) 0.4638(2) 0.7629(2) 0.0398(12) Uani 1 d . . H22A H 0.6228(2) 0.4383(2) 0.7452(2) 0.048 Uiso 1 calc R . N31 N 0.7660(2) 0.62644(14) 0.5944(2) 0.0336(11) Uani 1 d . . N32 N 0.8052(2) 0.5748(2) 0.5106(2) 0.0408(12) Uani 1 d . . H32A H 0.8073(2) 0.5476(2) 0.4799(2) 0.049 Uiso 1 calc R . N41 N 0.6951(2) 0.73231(15) 0.6657(2) 0.0308(10) Uani 1 d . . N42 N 0.6405(2) 0.80828(15) 0.6862(2) 0.0337(11) Uani 1 d . . H42A H 0.6298(2) 0.83494(15) 0.7127(2) 0.040 Uiso 1 calc R . N51 N 0.6676(2) 0.6371(2) 0.8382(2) 0.0355(11) Uani 1 d . . N52 N 0.7150(2) 0.6250(2) 0.9776(2) 0.0423(12) Uani 1 d . . H52A H 0.7442(2) 0.6293(2) 1.0306(2) 0.051 Uiso 1 calc R . N61 N 0.8595(2) 0.6319(2) 0.7879(2) 0.0353(11) Uani 1 d . . N62 N 0.9728(2) 0.6760(2) 0.8300(2) 0.0396(12) Uani 1 d . . H62A H 1.0058(2) 0.7020(2) 0.8494(2) 0.048 Uiso 1 calc R . C11 C 0.5806(3) 0.5853(2) 0.5176(3) 0.0367(14) Uani 1 d . . H11A H 0.6036(3) 0.6017(2) 0.4800(3) 0.044 Uiso 1 calc R . H11B H 0.5431(3) 0.5582(2) 0.4853(3) 0.044 Uiso 1 calc R . C12 C 0.5389(3) 0.6269(2) 0.5479(3) 0.0347(14) Uani 1 d . . C13 C 0.5121(3) 0.6839(2) 0.6297(3) 0.0350(14) Uani 1 d . . C14 C 0.5091(3) 0.7141(2) 0.6975(3) 0.043(2) Uani 1 d . . H14A H 0.5459(3) 0.7094(2) 0.7527(3) 0.052 Uiso 1 calc R . C15 C 0.4487(3) 0.7518(2) 0.6794(4) 0.052(2) Uani 1 d . . H15A H 0.4456(3) 0.7734(2) 0.7230(4) 0.062 Uiso 1 calc R . C16 C 0.3932(3) 0.7577(3) 0.5974(4) 0.065(2) Uani 1 d . . H16A H 0.3536(3) 0.7833(3) 0.5878(4) 0.078 Uiso 1 calc R . C17 C 0.3941(3) 0.7272(2) 0.5298(4) 0.057(2) Uani 1 d . . H17A H 0.3569(3) 0.7318(2) 0.4748(4) 0.068 Uiso 1 calc R . C18 C 0.4536(3) 0.6895(2) 0.5487(3) 0.0385(14) Uani 1 d . . C21 C 0.6096(3) 0.5160(2) 0.6274(3) 0.0353(14) Uani 1 d . . H21A H 0.5582(3) 0.5270(2) 0.6264(3) 0.042 Uiso 1 calc R . H21B H 0.6029(3) 0.4834(2) 0.5935(3) 0.042 Uiso 1 calc R . C22 C 0.6637(3) 0.5052(2) 0.7170(3) 0.0331(13) Uani 1 d . . C23 C 0.7554(3) 0.5150(2) 0.8424(3) 0.0346(13) Uani 1 d . . C24 C 0.8172(3) 0.5320(2) 0.9155(3) 0.0398(15) Uani 1 d . . H24A H 0.8457(3) 0.5630(2) 0.9152(3) 0.048 Uiso 1 calc R . C25 C 0.8344(3) 0.5018(2) 0.9876(3) 0.054(2) Uani 1 d . . H25A H 0.8746(3) 0.5128(2) 1.0377(3) 0.065 Uiso 1 calc R . C26 C 0.7933(4) 0.4553(3) 0.9874(3) 0.068(2) Uani 1 d . . H26A H 0.8078(4) 0.4354(3) 1.0376(3) 0.082 Uiso 1 calc R . C27 C 0.7316(3) 0.4368(2) 0.9167(3) 0.056(2) Uani 1 d . . H27A H 0.7040(3) 0.4054(2) 0.9176(3) 0.067 Uiso 1 calc R . C28 C 0.7141(3) 0.4682(2) 0.8444(3) 0.0382(14) Uani 1 d . . C31 C 0.7041(3) 0.5361(2) 0.5615(3) 0.0409(14) Uani 1 d . . H31A H 0.6786(3) 0.5189(2) 0.5064(3) 0.049 Uiso 1 calc R . H31B H 0.7345(3) 0.5091(2) 0.6019(3) 0.049 Uiso 1 calc R . C32 C 0.7571(3) 0.5795(2) 0.5547(3) 0.0353(14) Uani 1 d . . C33 C 0.8508(3) 0.6208(2) 0.5228(3) 0.0407(15) Uani 1 d . . C34 C 0.9095(3) 0.6362(2) 0.4944(3) 0.052(2) Uani 1 d . . H34A H 0.9254(3) 0.6146(2) 0.4587(3) 0.062 Uiso 1 calc R . C35 C 0.9433(3) 0.6860(2) 0.5226(3) 0.051(2) Uani 1 d . . H35A H 0.9841(3) 0.6978(2) 0.5064(3) 0.062 Uiso 1 calc R . C36 C 0.9181(3) 0.7192(2) 0.5747(3) 0.045(2) Uani 1 d . . H36A H 0.9424(3) 0.7524(2) 0.5921(3) 0.054 Uiso 1 calc R . C37 C 0.8580(3) 0.7037(2) 0.6007(3) 0.0402(15) Uani 1 d . . H37A H 0.8398(3) 0.7264(2) 0.6334(3) 0.048 Uiso 1 calc R . C38 C 0.8256(3) 0.6531(2) 0.5762(3) 0.0309(12) Uani 1 d . . C41 C 0.7265(3) 0.7590(2) 0.8171(3) 0.0371(14) Uani 1 d . . H41A H 0.7571(3) 0.7906(2) 0.8435(3) 0.045 Uiso 1 calc R . H41B H 0.6861(3) 0.7539(2) 0.8410(3) 0.045 Uiso 1 calc R . C42 C 0.6882(3) 0.7674(2) 0.7222(3) 0.0310(13) Uani 1 d . . C43 C 0.6463(3) 0.7525(2) 0.5861(3) 0.0311(13) Uani 1 d . . C44 C 0.6286(3) 0.7328(2) 0.5039(3) 0.0338(13) Uani 1 d . . H44A H 0.6534(3) 0.7022(2) 0.4940(3) 0.041 Uiso 1 calc R . C45 C 0.5733(3) 0.7600(2) 0.4380(3) 0.044(2) Uani 1 d . . H45A H 0.5594(3) 0.7466(2) 0.3828(3) 0.053 Uiso 1 calc R . C46 C 0.5374(3) 0.8066(2) 0.4505(3) 0.050(2) Uani 1 d . . H46A H 0.5007(3) 0.8241(2) 0.4038(3) 0.061 Uiso 1 calc R . C47 C 0.5553(3) 0.8273(2) 0.5312(3) 0.0406(15) Uani 1 d . . H47A H 0.5308(3) 0.8583(2) 0.5401(3) 0.049 Uiso 1 calc R . C48 C 0.6107(3) 0.8005(2) 0.5983(3) 0.0366(14) Uani 1 d . . C51 C 0.7880(3) 0.6894(2) 0.9202(3) 0.0403(15) Uani 1 d . . H51A H 0.8380(3) 0.6705(2) 0.9441(3) 0.048 Uiso 1 calc R . H51B H 0.7881(3) 0.7184(2) 0.9588(3) 0.048 Uiso 1 calc R . C52 C 0.7226(3) 0.6520(2) 0.9113(3) 0.0314(13) Uani 1 d . . C53 C 0.6527(3) 0.5899(2) 0.9462(3) 0.0368(14) Uani 1 d . . C54 C 0.6210(3) 0.5518(2) 0.9836(3) 0.053(2) Uani 1 d . . H54A H 0.6417(3) 0.5459(2) 1.0423(3) 0.063 Uiso 1 calc R . C55 C 0.5575(3) 0.5232(2) 0.9307(3) 0.059(2) Uani 1 d . . H55A H 0.5360(3) 0.4963(2) 0.9538(3) 0.070 Uiso 1 calc R . C56 C 0.5243(3) 0.5331(2) 0.8434(3) 0.051(2) Uani 1 d . . H56A H 0.4800(3) 0.5136(2) 0.8101(3) 0.061 Uiso 1 calc R . C57 C 0.5552(3) 0.5711(2) 0.8047(3) 0.0427(15) Uani 1 d . . H57A H 0.5332(3) 0.5777(2) 0.7463(3) 0.051 Uiso 1 calc R . C58 C 0.6211(3) 0.5986(2) 0.8585(3) 0.0354(13) Uani 1 d . . C61 C 0.8564(3) 0.7262(2) 0.8330(3) 0.0368(14) Uani 1 d . . H61A H 0.8892(3) 0.7424(2) 0.8868(3) 0.044 Uiso 1 calc R . H61B H 0.8493(3) 0.7524(2) 0.7880(3) 0.044 Uiso 1 calc R . C62 C 0.8965(3) 0.6772(2) 0.8168(3) 0.0323(13) Uani 1 d . . C63 C 0.9189(3) 0.5981(2) 0.7799(3) 0.0326(13) Uani 1 d . . C64 C 0.9144(3) 0.5449(2) 0.7528(3) 0.0418(15) Uani 1 d . . H64A H 0.8669(3) 0.5262(2) 0.7351(3) 0.050 Uiso 1 calc R . C65 C 0.9828(3) 0.5207(2) 0.7530(3) 0.050(2) Uani 1 d . . H65A H 0.9815(3) 0.4851(2) 0.7351(3) 0.060 Uiso 1 calc R . C66 C 1.0528(3) 0.5490(2) 0.7794(3) 0.058(2) Uani 1 d . . H66A H 1.0979(3) 0.5319(2) 0.7787(3) 0.070 Uiso 1 calc R . C67 C 1.0586(3) 0.6009(2) 0.8065(3) 0.051(2) Uani 1 d . . H67A H 1.1064(3) 0.6193(2) 0.8238(3) 0.062 Uiso 1 calc R . C68 C 0.9897(3) 0.6257(2) 0.8073(3) 0.0360(14) Uani 1 d . . C70 C 0.0848(4) 0.5472(3) 0.4572(5) 0.101(3) Uani 1 d . . H70A H 0.0378(4) 0.5686(3) 0.4342(5) 0.151 Uiso 1 calc R . H70B H 0.0742(4) 0.5114(3) 0.4340(5) 0.151 Uiso 1 calc R . H70C H 0.1260(4) 0.5631(3) 0.4424(5) 0.151 Uiso 1 calc R . C71 C 0.1105(4) 0.5447(3) 0.5528(4) 0.077(2) Uani 1 d . . H71A H 0.1209(4) 0.5807(3) 0.5766(4) 0.093 Uiso 1 calc R . H71B H 0.0689(4) 0.5289(3) 0.5682(4) 0.093 Uiso 1 calc R . C72 C 0.2049(4) 0.5058(3) 0.6762(4) 0.071(2) Uani 1 d . . H72A H 0.1655(4) 0.4856(3) 0.6897(4) 0.085 Uiso 1 calc R . H72B H 0.2118(4) 0.5404(3) 0.7045(4) 0.085 Uiso 1 calc R . C73 C 0.2816(4) 0.4757(3) 0.7062(4) 0.082(2) Uani 1 d . . H73A H 0.2995(4) 0.4704(3) 0.7669(4) 0.124 Uiso 1 calc R . H73B H 0.3203(4) 0.4961(3) 0.6928(4) 0.124 Uiso 1 calc R . H73C H 0.2742(4) 0.4414(3) 0.6781(4) 0.124 Uiso 1 calc R . C74 C 0.3206(4) 0.6181(3) 0.6239(5) 0.102(3) Uani 1 d . . C75 C 0.3739(4) 0.5822(2) 0.6006(4) 0.059(2) Uani 1 d . . C76 C 0.1648(8) 0.8005(5) 0.1920(6) 0.205(6) Uani 1 d . . H76A H 0.1476(8) 0.7643(5) 0.1757(6) 0.307 Uiso 1 calc R . H76B H 0.1825(8) 0.8162(5) 0.1501(6) 0.307 Uiso 1 calc R . H76C H 0.1217(8) 0.8213(5) 0.1955(6) 0.307 Uiso 1 calc R . C77 C 0.2320(6) 0.8003(3) 0.2778(7) 0.145(4) Uani 1 d . . H77A H 0.2146(6) 0.7843(3) 0.3203(7) 0.174 Uiso 1 calc R . H77B H 0.2755(6) 0.7791(3) 0.2747(7) 0.174 Uiso 1 calc R . C78 C 0.3171(5) 0.8575(4) 0.3832(6) 0.136(4) Uani 1 d . . H78A H 0.3599(5) 0.8331(4) 0.3874(6) 0.163 Uiso 1 calc R . H78B H 0.2963(5) 0.8475(4) 0.4263(6) 0.163 Uiso 1 calc R . C79 C 0.3472(5) 0.9133(4) 0.3981(6) 0.131(4) Uani 1 d . . H79A H 0.3880(5) 0.9159(4) 0.4539(6) 0.196 Uiso 1 calc R . H79B H 0.3048(5) 0.9373(4) 0.3945(6) 0.196 Uiso 1 calc R . H79C H 0.3683(5) 0.9229(4) 0.3557(6) 0.196 Uiso 1 calc R . C80 C 1.0403(5) 0.8000(4) 0.7725(6) 0.140(4) Uani 1 d . . H80A H 1.0280(5) 0.8344(4) 0.7447(6) 0.210 Uiso 1 calc R . H80B H 0.9949(5) 0.7769(4) 0.7509(6) 0.210 Uiso 1 calc R . H80C H 1.0835(5) 0.7840(4) 0.7615(6) 0.210 Uiso 1 calc R . C81 C 1.0610(5) 0.8067(3) 0.8591(5) 0.091(3) Uani 1 d . . H81A H 1.0176(5) 0.8235(3) 0.8698(5) 0.110 Uiso 1 calc R . H81B H 1.1062(5) 0.8306(3) 0.8804(5) 0.110 Uiso 1 calc R . C82 C 1.1413(5) 0.7534(3) 0.9758(5) 0.109(3) Uani 1 d . . H82A H 1.1331(5) 0.7784(3) 1.0159(5) 0.131 Uiso 1 calc R . H82B H 1.1870(5) 0.7659(3) 0.9646(5) 0.131 Uiso 1 calc R . C83 C 1.1603(5) 0.7008(3) 1.0171(5) 0.120(4) Uani 1 d . . H83A H 1.2063(5) 0.7039(3) 1.0686(5) 0.179 Uiso 1 calc R . H83B H 1.1706(5) 0.6757(3) 0.9791(5) 0.179 Uiso 1 calc R . H83C H 1.1165(5) 0.6883(3) 1.0306(5) 0.179 Uiso 1 calc R . C84 C 1.0713(4) 0.5842(3) 1.1315(4) 0.091(3) Uani 1 d . . C85 C 1.0145(3) 0.6149(3) 1.0625(4) 0.068(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.02682(11) 0.02794(12) 0.02454(11) -0.00357(12) 0.00770(9) -0.00066(13) Cl1 0.0451(8) 0.0593(10) 0.0651(9) -0.0205(7) -0.0010(7) 0.0120(7) Cl2 0.0660(9) 0.0457(8) 0.0434(7) 0.0031(6) 0.0116(7) 0.0115(7) Cl3 0.0796(9) 0.0420(8) 0.0573(7) -0.0027(6) 0.0404(7) -0.0156(7) O1 0.065(2) 0.047(2) 0.060(2) -0.008(2) 0.037(2) 0.005(2) O2 0.105(4) 0.100(4) 0.084(3) -0.009(3) 0.031(3) -0.009(3) O3 0.097(4) 0.089(4) 0.124(4) 0.012(3) -0.028(3) -0.039(3) O11 0.119(5) 0.103(4) 0.216(6) 0.087(4) -0.048(5) -0.028(4) O12 0.112(4) 0.318(7) 0.212(5) -0.196(5) 0.052(4) -0.003(5) O13 0.069(3) 0.060(3) 0.112(4) -0.001(3) 0.016(3) -0.010(2) O14 0.046(3) 0.105(3) 0.103(3) -0.060(3) -0.004(2) 0.003(3) O21 0.096(3) 0.085(4) 0.197(5) 0.025(4) 0.052(4) 0.050(3) O22 0.134(4) 0.073(3) 0.102(3) 0.043(3) 0.022(3) -0.010(3) O23 0.138(4) 0.107(4) 0.057(2) -0.034(2) 0.032(3) 0.005(3) O24 0.129(4) 0.110(4) 0.053(3) -0.008(3) 0.002(3) -0.061(3) O31 0.152(4) 0.045(2) 0.051(2) 0.003(2) 0.039(2) -0.013(3) O32 0.097(3) 0.065(3) 0.065(2) -0.022(2) 0.033(2) -0.047(2) O33 0.078(3) 0.082(4) 0.188(5) -0.016(3) 0.073(3) -0.020(3) O34 0.151(4) 0.071(3) 0.043(2) -0.004(2) 0.044(2) -0.044(3) N1 0.041(2) 0.024(2) 0.031(2) -0.001(2) 0.012(2) -0.001(2) N2 0.028(2) 0.027(2) 0.030(2) -0.006(2) 0.006(2) 0.001(2) N3 0.061(3) 0.054(3) 0.064(3) 0.003(2) 0.020(2) -0.014(3) N4 0.066(4) 0.211(7) 0.077(4) 0.052(4) 0.014(3) 0.069(4) N11 0.029(2) 0.030(2) 0.029(2) 0.001(2) 0.007(2) -0.004(2) N12 0.037(2) 0.044(3) 0.033(2) 0.007(2) -0.009(2) -0.007(2) N21 0.030(2) 0.033(2) 0.028(2) -0.006(2) 0.009(2) 0.002(2) N22 0.047(2) 0.031(2) 0.039(2) 0.002(2) 0.012(2) -0.011(2) N31 0.045(2) 0.025(2) 0.038(2) -0.004(2) 0.023(2) 0.001(2) N32 0.054(2) 0.038(2) 0.036(2) -0.012(2) 0.024(2) 0.005(2) N41 0.031(2) 0.031(2) 0.030(2) -0.005(2) 0.011(2) -0.002(2) N42 0.039(2) 0.023(2) 0.042(2) -0.001(2) 0.019(2) 0.007(2) N51 0.031(2) 0.042(2) 0.030(2) -0.007(2) 0.006(2) -0.002(2) N52 0.056(2) 0.046(3) 0.025(2) 0.000(2) 0.016(2) 0.008(2) N61 0.028(2) 0.041(2) 0.033(2) -0.008(2) 0.007(2) -0.001(2) N62 0.026(2) 0.044(3) 0.046(2) -0.006(2) 0.010(2) -0.009(2) C11 0.043(3) 0.041(3) 0.018(2) -0.003(2) 0.002(2) -0.016(2) C12 0.033(3) 0.034(3) 0.026(2) 0.002(2) -0.002(2) -0.010(2) C13 0.020(2) 0.035(3) 0.046(3) 0.009(2) 0.007(2) 0.001(2) C14 0.032(3) 0.045(3) 0.054(3) -0.005(3) 0.016(2) 0.004(2) C15 0.037(3) 0.040(3) 0.083(4) -0.007(3) 0.027(3) -0.002(3) C16 0.039(3) 0.061(4) 0.085(4) 0.001(3) 0.010(3) 0.012(3) C17 0.034(3) 0.052(4) 0.066(4) 0.015(3) -0.002(3) 0.001(3) C18 0.028(3) 0.029(3) 0.052(3) 0.010(2) 0.008(2) -0.006(2) C21 0.037(3) 0.030(3) 0.034(2) -0.001(2) 0.008(2) -0.004(2) C22 0.043(3) 0.026(3) 0.031(2) -0.001(2) 0.014(2) 0.000(2) C23 0.042(3) 0.026(3) 0.034(2) 0.003(2) 0.012(2) 0.011(2) C24 0.041(3) 0.036(3) 0.036(3) -0.001(2) 0.007(2) 0.002(2) C25 0.054(3) 0.061(4) 0.034(3) 0.002(3) -0.001(3) -0.005(3) C26 0.085(5) 0.069(4) 0.036(3) 0.017(3) 0.005(3) -0.002(4) C27 0.061(3) 0.045(3) 0.058(3) 0.022(3) 0.019(3) 0.007(3) C28 0.034(3) 0.041(3) 0.035(3) 0.006(2) 0.008(2) 0.000(2) C31 0.053(3) 0.034(3) 0.037(3) -0.008(2) 0.019(2) -0.002(3) C32 0.042(3) 0.037(3) 0.028(2) 0.003(2) 0.014(2) 0.003(2) C33 0.048(3) 0.040(3) 0.033(2) 0.005(2) 0.014(2) 0.011(2) C34 0.050(3) 0.062(4) 0.054(3) 0.013(3) 0.033(2) 0.020(3) C35 0.037(3) 0.066(4) 0.055(3) 0.016(3) 0.021(2) 0.009(3) C36 0.034(3) 0.053(3) 0.044(3) 0.010(3) 0.012(2) -0.009(3) C37 0.043(3) 0.044(3) 0.033(3) 0.004(2) 0.013(2) 0.002(3) C38 0.035(2) 0.034(3) 0.029(2) 0.005(2) 0.018(2) 0.005(2) C41 0.050(3) 0.035(3) 0.028(2) -0.008(2) 0.016(2) 0.001(2) C42 0.032(2) 0.027(3) 0.036(3) -0.001(2) 0.015(2) -0.002(2) C43 0.034(2) 0.023(2) 0.040(3) 0.005(2) 0.018(2) -0.002(2) C44 0.041(3) 0.031(3) 0.033(2) -0.003(2) 0.018(2) 0.001(2) C45 0.049(3) 0.047(3) 0.036(3) 0.011(2) 0.015(2) -0.004(3) C46 0.040(3) 0.052(3) 0.055(3) 0.034(3) 0.013(2) 0.000(3) C47 0.039(3) 0.032(3) 0.049(3) 0.011(2) 0.015(2) 0.003(2) C48 0.037(3) 0.033(3) 0.044(3) 0.009(2) 0.019(2) 0.001(2) C51 0.043(3) 0.046(3) 0.026(2) -0.003(2) 0.006(2) 0.004(3) C52 0.031(2) 0.035(3) 0.026(2) -0.004(2) 0.008(2) 0.006(2) C53 0.044(3) 0.036(3) 0.035(2) 0.003(2) 0.019(2) 0.004(2) C54 0.069(3) 0.056(4) 0.040(3) 0.004(3) 0.028(3) 0.008(3) C55 0.080(3) 0.053(4) 0.065(3) -0.003(3) 0.053(3) -0.004(3) C56 0.053(3) 0.056(4) 0.054(3) -0.011(3) 0.031(3) -0.012(3) C57 0.045(3) 0.050(3) 0.036(3) -0.011(2) 0.018(2) -0.006(3) C58 0.041(2) 0.036(3) 0.038(2) 0.001(2) 0.024(2) 0.002(2) C61 0.032(3) 0.034(3) 0.042(3) -0.006(2) 0.010(2) -0.005(2) C62 0.025(2) 0.040(3) 0.026(2) -0.001(2) 0.002(2) 0.001(2) C63 0.028(2) 0.039(3) 0.029(2) 0.005(2) 0.008(2) 0.009(2) C64 0.041(3) 0.040(3) 0.045(3) 0.002(2) 0.017(2) 0.010(2) C65 0.045(3) 0.048(3) 0.055(3) -0.007(3) 0.015(3) 0.020(3) C66 0.057(3) 0.067(4) 0.056(3) 0.009(3) 0.027(3) 0.030(3) C67 0.024(3) 0.073(4) 0.055(3) 0.001(3) 0.012(2) 0.009(3) C68 0.032(2) 0.041(3) 0.035(2) 0.004(2) 0.011(2) 0.010(2) C70 0.088(5) 0.100(6) 0.118(6) 0.021(5) 0.041(4) 0.034(5) C71 0.068(4) 0.062(4) 0.116(5) -0.017(4) 0.050(4) 0.008(3) C72 0.094(4) 0.076(5) 0.065(3) -0.015(3) 0.054(3) -0.013(4) C73 0.078(4) 0.099(6) 0.070(4) 0.004(4) 0.028(4) 0.002(4) C74 0.107(4) 0.073(5) 0.167(6) -0.022(4) 0.099(4) -0.011(4) C75 0.063(3) 0.054(4) 0.061(4) -0.002(3) 0.024(3) -0.030(3) C76 0.294(13) 0.191(11) 0.136(8) -0.063(8) 0.088(9) -0.111(11) C77 0.179(8) 0.070(6) 0.204(9) -0.018(6) 0.093(7) -0.042(6) C78 0.070(5) 0.129(8) 0.174(9) 0.058(7) 0.004(6) -0.003(6) C79 0.125(7) 0.125(8) 0.144(7) -0.017(6) 0.051(6) -0.044(6) C80 0.128(7) 0.141(8) 0.146(8) 0.025(7) 0.044(6) -0.028(7) C81 0.111(5) 0.074(5) 0.097(5) 0.002(4) 0.048(4) -0.015(5) C82 0.084(6) 0.120(7) 0.105(6) -0.027(5) 0.015(5) -0.025(5) C83 0.108(7) 0.107(7) 0.103(6) 0.030(5) -0.008(5) -0.015(6) C84 0.091(5) 0.087(5) 0.071(4) 0.025(4) 0.003(4) 0.038(4) C85 0.050(3) 0.099(5) 0.060(4) -0.003(3) 0.025(3) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 N61 2.508(4) . ? Nd1 N21 2.516(4) . ? Nd1 N11 2.526(3) . ? Nd1 N41 2.528(4) . ? Nd1 N31 2.534(4) . ? Nd1 N51 2.537(4) . ? Nd1 N1 2.720(3) . ? Nd1 N2 2.746(3) . ? Cl1 O12 1.356(7) . ? Cl1 O11 1.361(6) . ? Cl1 O14 1.410(4) . ? Cl1 O13 1.411(4) . ? Cl2 O21 1.388(5) . ? Cl2 O23 1.404(5) . ? Cl2 O22 1.408(5) . ? Cl2 O24 1.429(5) . ? Cl3 O34 1.396(4) . ? Cl3 O31 1.410(4) . ? Cl3 O33 1.415(5) . ? Cl3 O32 1.440(4) . ? O1 C71 1.416(7) . ? O1 C72 1.423(6) . ? O2 C77 1.404(9) . ? O2 C78 1.412(9) . ? O3 C82 1.294(8) . ? O3 C81 1.458(9) . ? N1 C31 1.475(6) . ? N1 C11 1.484(5) . ? N1 C21 1.491(6) . ? N2 C41 1.469(6) . ? N2 C51 1.478(6) . ? N2 C61 1.484(6) . ? N3 C75 1.121(8) . ? N4 C85 1.136(8) . ? N11 C12 1.328(5) . ? N11 C13 1.398(6) . ? N12 C12 1.333(6) . ? N12 C18 1.384(7) . ? N21 C22 1.334(6) . ? N21 C23 1.405(5) . ? N22 C22 1.321(6) . ? N22 C28 1.386(5) . ? N31 C32 1.325(6) . ? N31 C38 1.399(6) . ? N32 C32 1.348(6) . ? N32 C33 1.381(6) . ? N41 C42 1.330(6) . ? N41 C43 1.398(5) . ? N42 C42 1.330(6) . ? N42 C48 1.389(6) . ? N51 C52 1.321(5) . ? N51 C58 1.402(6) . ? N52 C52 1.355(6) . ? N52 C53 1.372(6) . ? N61 C62 1.309(6) . ? N61 C63 1.416(6) . ? N62 C62 1.325(6) . ? N62 C68 1.377(6) . ? C11 C12 1.483(7) . ? C18 C17 1.380(7) . ? C18 C13 1.392(6) . ? C13 C14 1.385(7) . ? C14 C15 1.391(7) . ? C15 C16 1.384(7) . ? C16 C17 1.373(9) . ? C21 C22 1.490(6) . ? C23 C24 1.391(6) . ? C23 C28 1.394(7) . ? C24 C25 1.361(7) . ? C25 C26 1.377(8) . ? C26 C27 1.378(7) . ? C27 C28 1.381(7) . ? C31 C32 1.480(7) . ? C33 C34 1.378(8) . ? C33 C38 1.404(7) . ? C34 C35 1.385(8) . ? C35 C36 1.401(8) . ? C36 C37 1.377(7) . ? C37 C38 1.387(7) . ? C41 C42 1.503(6) . ? C43 C44 1.390(6) . ? C43 C48 1.410(7) . ? C44 C45 1.369(6) . ? C45 C46 1.385(7) . ? C46 C47 1.376(7) . ? C47 C48 1.375(6) . ? C51 C52 1.473(7) . ? C53 C54 1.378(7) . ? C53 C58 1.389(6) . ? C54 C55 1.368(7) . ? C55 C56 1.390(7) . ? C56 C57 1.379(7) . ? C57 C58 1.387(6) . ? C61 C62 1.497(7) . ? C63 C68 1.380(6) . ? C63 C64 1.390(7) . ? C64 C65 1.383(7) . ? C65 C66 1.378(8) . ? C66 C67 1.359(8) . ? C67 C68 1.403(7) . ? C70 C71 1.504(9) . ? C72 C73 1.497(9) . ? C74 C75 1.475(10) . ? C76 C77 1.508(13) . ? C78 C79 1.477(12) . ? C80 C81 1.374(11) . ? C82 C83 1.460(11) . ? C84 C85 1.454(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N61 Nd1 N21 82.68(12) . . ? N61 Nd1 N11 175.14(13) . . ? N21 Nd1 N11 101.58(11) . . ? N61 Nd1 N41 99.90(12) . . ? N21 Nd1 N41 176.66(13) . . ? N11 Nd1 N41 75.93(11) . . ? N61 Nd1 N31 75.05(12) . . ? N21 Nd1 N31 100.02(12) . . ? N11 Nd1 N31 101.72(12) . . ? N41 Nd1 N31 82.75(12) . . ? N61 Nd1 N51 101.08(12) . . ? N21 Nd1 N51 75.87(13) . . ? N11 Nd1 N51 82.36(12) . . ? N41 Nd1 N51 101.46(13) . . ? N31 Nd1 N51 174.81(11) . . ? N61 Nd1 N1 117.77(12) . . ? N21 Nd1 N1 62.99(11) . . ? N11 Nd1 N1 62.95(12) . . ? N41 Nd1 N1 117.13(11) . . ? N31 Nd1 N1 63.34(12) . . ? N51 Nd1 N1 116.56(12) . . ? N61 Nd1 N2 63.30(12) . . ? N21 Nd1 N2 117.20(11) . . ? N11 Nd1 N2 116.01(11) . . ? N41 Nd1 N2 62.61(11) . . ? N31 Nd1 N2 117.54(12) . . ? N51 Nd1 N2 62.64(12) . . ? N1 Nd1 N2 178.88(12) . . ? O12 Cl1 O11 109.6(5) . . ? O12 Cl1 O14 107.7(3) . . ? O11 Cl1 O14 110.6(4) . . ? O12 Cl1 O13 111.7(4) . . ? O11 Cl1 O13 107.2(3) . . ? O14 Cl1 O13 110.1(3) . . ? O21 Cl2 O23 108.8(4) . . ? O21 Cl2 O22 114.6(4) . . ? O23 Cl2 O22 108.9(3) . . ? O21 Cl2 O24 108.8(3) . . ? O23 Cl2 O24 109.4(3) . . ? O22 Cl2 O24 106.2(3) . . ? O34 Cl3 O31 110.0(3) . . ? O34 Cl3 O33 114.9(3) . . ? O31 Cl3 O33 105.4(3) . . ? O34 Cl3 O32 108.1(3) . . ? O31 Cl3 O32 112.0(3) . . ? O33 Cl3 O32 106.6(3) . . ? C71 O1 C72 112.4(5) . . ? C77 O2 C78 113.3(6) . . ? C82 O3 C81 119.1(6) . . ? C31 N1 C11 109.9(4) . . ? C31 N1 C21 109.4(4) . . ? C11 N1 C21 110.0(3) . . ? C31 N1 Nd1 109.4(3) . . ? C11 N1 Nd1 108.9(3) . . ? C21 N1 Nd1 109.2(3) . . ? C41 N2 C51 110.0(4) . . ? C41 N2 C61 110.3(4) . . ? C51 N2 C61 110.5(3) . . ? C41 N2 Nd1 109.1(2) . . ? C51 N2 Nd1 109.3(3) . . ? C61 N2 Nd1 107.6(3) . . ? C12 N11 C13 104.3(4) . . ? C12 N11 Nd1 117.2(3) . . ? C13 N11 Nd1 130.8(3) . . ? C12 N12 C18 108.1(4) . . ? C22 N21 C23 104.6(4) . . ? C22 N21 Nd1 117.6(3) . . ? C23 N21 Nd1 131.7(3) . . ? C22 N22 C28 108.7(4) . . ? C32 N31 C38 105.4(4) . . ? C32 N31 Nd1 117.3(3) . . ? C38 N31 Nd1 133.7(3) . . ? C32 N32 C33 109.0(4) . . ? C42 N41 C43 105.0(4) . . ? C42 N41 Nd1 115.9(3) . . ? C43 N41 Nd1 127.1(3) . . ? C42 N42 C48 108.2(4) . . ? C52 N51 C58 106.3(4) . . ? C52 N51 Nd1 114.7(3) . . ? C58 N51 Nd1 126.8(3) . . ? C52 N52 C53 108.6(4) . . ? C62 N61 C63 103.8(4) . . ? C62 N61 Nd1 118.0(3) . . ? C63 N61 Nd1 133.0(3) . . ? C62 N62 C68 107.5(4) . . ? C12 C11 N1 110.9(4) . . ? N11 C12 N12 113.0(4) . . ? N11 C12 C11 122.2(4) . . ? N12 C12 C11 124.8(4) . . ? C17 C18 N12 132.2(5) . . ? C17 C18 C13 122.9(5) . . ? N12 C18 C13 104.7(4) . . ? C14 C13 C18 120.4(5) . . ? C14 C13 N11 129.7(4) . . ? C18 C13 N11 109.8(4) . . ? C13 C14 C15 117.0(5) . . ? C16 C15 C14 121.1(6) . . ? C17 C16 C15 122.8(6) . . ? C16 C17 C18 115.7(5) . . ? C22 C21 N1 109.3(4) . . ? N22 C22 N21 112.7(4) . . ? N22 C22 C21 124.3(4) . . ? N21 C22 C21 122.9(4) . . ? C24 C23 C28 119.9(4) . . ? C24 C23 N21 130.9(4) . . ? C28 C23 N21 109.2(4) . . ? C25 C24 C23 117.8(5) . . ? C24 C25 C26 121.0(5) . . ? C25 C26 C27 123.4(5) . . ? C26 C27 C28 114.9(5) . . ? C27 C28 N22 132.3(5) . . ? C27 C28 C23 122.9(4) . . ? N22 C28 C23 104.8(4) . . ? N1 C31 C32 109.2(4) . . ? N31 C32 N32 111.7(4) . . ? N31 C32 C31 124.3(5) . . ? N32 C32 C31 123.9(4) . . ? C34 C33 N32 132.8(5) . . ? C34 C33 C38 122.9(5) . . ? N32 C33 C38 104.2(4) . . ? C33 C34 C35 115.7(5) . . ? C34 C35 C36 122.2(5) . . ? C37 C36 C35 121.3(5) . . ? C36 C37 C38 117.4(5) . . ? C37 C38 N31 130.0(5) . . ? C37 C38 C33 120.4(5) . . ? N31 C38 C33 109.6(4) . . ? N2 C41 C42 110.1(4) . . ? N41 C42 N42 113.1(4) . . ? N41 C42 C41 122.8(4) . . ? N42 C42 C41 123.9(4) . . ? C44 C43 N41 131.4(4) . . ? C44 C43 C48 119.6(4) . . ? N41 C43 C48 109.0(4) . . ? C45 C44 C43 117.7(5) . . ? C44 C45 C46 122.4(5) . . ? C47 C46 C45 120.8(4) . . ? C48 C47 C46 117.7(5) . . ? C47 C48 N42 133.4(5) . . ? C47 C48 C43 121.8(5) . . ? N42 C48 C43 104.7(4) . . ? C52 C51 N2 109.6(3) . . ? N51 C52 N52 110.9(4) . . ? N51 C52 C51 125.3(4) . . ? N52 C52 C51 123.7(4) . . ? N52 C53 C54 133.4(4) . . ? N52 C53 C58 105.6(4) . . ? C54 C53 C58 121.0(4) . . ? C55 C54 C53 117.1(5) . . ? C54 C55 C56 121.9(5) . . ? C57 C56 C55 121.9(5) . . ? C56 C57 C58 115.7(4) . . ? C57 C58 C53 122.4(5) . . ? C57 C58 N51 129.2(4) . . ? C53 C58 N51 108.5(4) . . ? N2 C61 C62 110.2(4) . . ? N61 C62 N62 114.1(4) . . ? N61 C62 C61 123.3(4) . . ? N62 C62 C61 122.6(4) . . ? C68 C63 C64 121.0(5) . . ? C68 C63 N61 109.1(4) . . ? C64 C63 N61 129.9(4) . . ? C65 C64 C63 118.1(5) . . ? C66 C65 C64 120.2(5) . . ? C67 C66 C65 122.8(5) . . ? C66 C67 C68 117.4(5) . . ? N62 C68 C63 105.5(4) . . ? N62 C68 C67 134.0(5) . . ? C63 C68 C67 120.5(5) . . ? O1 C71 C70 109.1(5) . . ? O1 C72 C73 108.2(5) . . ? N3 C75 C74 178.3(7) . . ? O2 C77 C76 109.3(8) . . ? O2 C78 C79 109.8(7) . . ? C80 C81 O3 112.1(7) . . ? O3 C82 C83 116.8(7) . . ? N4 C85 C84 177.7(8) . . ? _refine_diff_density_max 1.527 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.127 #=END data_Eu(ntb)2(ClO4)3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C64 H78 Cl3 Eu N16 O15' _chemical_formula_weight 1569.73 _chemical_melting_point ? _chemical_compound_source ? 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' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1861(4) _cell_length_b 24.8563(6) _cell_length_c 16.9481(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.9290(10) _cell_angle_gamma 90.00 _cell_volume 7106.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method ? _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32598 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.02 _reflns_number_total 12490 _reflns_number_observed 7546 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12484 _refine_ls_number_parameters 892 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1115 _refine_ls_R_factor_obs 0.0481 _refine_ls_wR_factor_all 0.1076 _refine_ls_wR_factor_obs 0.0865 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_restrained_S_all 1.033 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max 0.248 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Eu1 Eu 0.71136(2) 0.635233(11) 0.71168(2) 0.02270(9) Uani 1 d . . Cl1 Cl 0.25699(10) 0.62392(7) 0.34243(12) 0.0562(5) Uani 1 d . . Cl2 Cl 0.84005(10) 0.62118(6) 0.20051(10) 0.0481(4) Uani 1 d . . Cl3 Cl 0.53529(11) 0.60696(7) 0.28674(11) 0.0500(4) Uani 1 d . . O1 O 0.1785(2) 0.5122(2) 0.5834(3) 0.0477(11) Uani 1 d . . O2 O 0.2556(3) 0.8536(2) 0.3014(3) 0.081(2) Uani 1 d . . O3 O 1.0824(3) 0.7555(2) 0.9036(4) 0.103(2) Uani 1 d . . O11 O 0.2279(4) 0.6567(3) 0.2715(5) 0.166(4) Uani 1 d . . O12 O 0.2494(4) 0.6474(4) 0.4135(5) 0.191(4) Uani 1 d . . O13 O 0.2149(3) 0.5742(2) 0.3215(3) 0.075(2) Uani 1 d . . O14 O 0.3392(2) 0.6149(2) 0.3626(3) 0.082(2) Uani 1 d . . O21 O 0.9080(3) 0.5902(2) 0.2222(4) 0.109(2) Uani 1 d . . O22 O 0.8393(3) 0.6640(2) 0.1448(3) 0.092(2) Uani 1 d . . O23 O 0.8340(3) 0.6422(2) 0.2756(3) 0.088(2) Uani 1 d . . O24 O 0.7712(3) 0.5887(2) 0.1564(3) 0.089(2) Uani 1 d . . O31 O 0.5487(3) 0.5551(2) 0.3242(3) 0.073(2) Uani 1 d . . O32 O 0.5973(3) 0.6445(2) 0.3340(3) 0.0693(15) Uani 1 d . . O33 O 0.4622(3) 0.6258(2) 0.2893(5) 0.116(2) Uani 1 d . . O34 O 0.5350(3) 0.6039(2) 0.2031(3) 0.080(2) Uani 1 d . . N1 N 0.6433(2) 0.5598(2) 0.5907(3) 0.0273(11) Uani 1 d . . N2 N 0.7767(2) 0.7118(2) 0.8328(3) 0.0265(11) Uani 1 d . . N3 N 0.4123(3) 0.5556(2) 0.5791(4) 0.050(2) Uani 1 d . . N4 N 0.9716(4) 0.6417(3) 1.0107(4) 0.106(3) Uani 1 d . . N11 N 0.5656(2) 0.6443(2) 0.6288(3) 0.0242(11) Uani 1 d . . N12 N 0.4724(3) 0.6526(2) 0.5000(3) 0.0346(13) Uani 1 d . . H12A H 0.4458(3) 0.6469(2) 0.4455(3) 0.042 Uiso 1 calc R . N21 N 0.7227(2) 0.5400(2) 0.7613(3) 0.0261(11) Uani 1 d . . N22 N 0.6577(3) 0.4647(2) 0.7646(3) 0.0345(12) Uani 1 d . . H22A H 0.6226(3) 0.4386(2) 0.7472(3) 0.041 Uiso 1 calc R . N31 N 0.7653(2) 0.6270(2) 0.5960(3) 0.0253(11) Uani 1 d . . N32 N 0.8067(3) 0.5757(2) 0.5129(3) 0.0371(13) Uani 1 d . . H32A H 0.8099(3) 0.5479(2) 0.4822(3) 0.045 Uiso 1 calc R . N41 N 0.6927(2) 0.7313(2) 0.6645(3) 0.0245(11) Uani 1 d . . N42 N 0.6378(2) 0.8086(2) 0.6826(3) 0.0312(12) Uani 1 d . . H42A H 0.6268(2) 0.8362(2) 0.7088(3) 0.037 Uiso 1 calc R . N51 N 0.6665(2) 0.6372(2) 0.8345(3) 0.0262(10) Uani 1 d . . N52 N 0.7123(3) 0.6251(2) 0.9748(3) 0.0331(12) Uani 1 d . . H52A H 0.7415(3) 0.6297(2) 1.0290(3) 0.040 Uiso 1 calc R . N61 N 0.8575(2) 0.6322(2) 0.7844(3) 0.0278(11) Uani 1 d . . N62 N 0.9722(3) 0.6761(2) 0.8275(3) 0.0318(12) Uani 1 d . . H62A H 1.0065(3) 0.7025(2) 0.8469(3) 0.038 Uiso 1 calc R . C11 C 0.5793(3) 0.5854(2) 0.5179(3) 0.0303(14) Uani 1 d . . H11A H 0.6023(3) 0.6022(2) 0.4793(3) 0.036 Uiso 1 calc R . H11B H 0.5407(3) 0.5577(2) 0.4854(3) 0.036 Uiso 1 calc R . C12 C 0.5380(3) 0.6270(2) 0.5489(3) 0.0284(14) Uani 1 d . . C13 C 0.5115(3) 0.6838(2) 0.6314(4) 0.0296(14) Uani 1 d . . C14 C 0.5087(3) 0.7143(2) 0.6989(4) 0.0338(15) Uani 1 d . . H14A H 0.5468(3) 0.7096(2) 0.7548(4) 0.041 Uiso 1 calc R . C15 C 0.4485(3) 0.7519(2) 0.6818(4) 0.046(2) Uani 1 d . . H15A H 0.4458(3) 0.7739(2) 0.7265(4) 0.055 Uiso 1 calc R . C16 C 0.3914(4) 0.7578(3) 0.5992(5) 0.054(2) Uani 1 d . . H16A H 0.3505(4) 0.7837(3) 0.5894(5) 0.065 Uiso 1 calc R . C17 C 0.3926(3) 0.7275(3) 0.5327(4) 0.049(2) Uani 1 d . . H17A H 0.3538(3) 0.7319(3) 0.4771(4) 0.058 Uiso 1 calc R . C18 C 0.4535(3) 0.6896(2) 0.5498(4) 0.034(2) Uani 1 d . . C21 C 0.6097(3) 0.5167(2) 0.6278(3) 0.0299(14) Uani 1 d . . H21A H 0.6034(3) 0.4832(2) 0.5943(3) 0.036 Uiso 1 calc R . H21B H 0.5569(3) 0.5276(2) 0.6265(3) 0.036 Uiso 1 calc R . C22 C 0.6646(3) 0.5070(2) 0.7178(3) 0.0279(14) Uani 1 d . . C23 C 0.7561(3) 0.5174(2) 0.8430(3) 0.0287(14) Uani 1 d . . C24 C 0.8185(3) 0.5343(2) 0.9154(4) 0.037(2) Uani 1 d . . H24A H 0.8478(3) 0.5658(2) 0.9148(4) 0.045 Uiso 1 calc R . C25 C 0.8363(4) 0.5040(3) 0.9882(4) 0.048(2) Uani 1 d . . H25A H 0.8778(4) 0.5152(3) 1.0390(4) 0.058 Uiso 1 calc R . C26 C 0.7948(4) 0.4574(3) 0.9886(4) 0.057(2) Uani 1 d . . H26A H 0.8092(4) 0.4375(3) 1.0399(4) 0.068 Uiso 1 calc R . C27 C 0.7331(4) 0.4386(3) 0.9172(4) 0.050(2) Uani 1 d . . H27A H 0.7049(4) 0.4065(3) 0.9179(4) 0.060 Uiso 1 calc R . C28 C 0.7156(3) 0.4699(2) 0.8449(4) 0.0344(15) Uani 1 d . . C31 C 0.7044(3) 0.5369(2) 0.5617(4) 0.0343(15) Uani 1 d . . H31A H 0.7352(3) 0.5090(2) 0.6022(4) 0.041 Uiso 1 calc R . H31B H 0.6786(3) 0.5200(2) 0.5052(4) 0.041 Uiso 1 calc R . C32 C 0.7577(3) 0.5802(2) 0.5567(3) 0.0286(14) Uani 1 d . . C33 C 0.8505(3) 0.6224(2) 0.5249(4) 0.035(2) Uani 1 d . . C34 C 0.9106(3) 0.6388(3) 0.4985(4) 0.044(2) Uani 1 d . . H34A H 0.9283(3) 0.6166(3) 0.4635(4) 0.052 Uiso 1 calc R . C35 C 0.9431(3) 0.6886(3) 0.5253(4) 0.044(2) Uani 1 d . . H35A H 0.9846(3) 0.7010(3) 0.5086(4) 0.052 Uiso 1 calc R . C36 C 0.9168(3) 0.7217(2) 0.5765(3) 0.037(2) Uani 1 d . . H36A H 0.9407(3) 0.7560(2) 0.5934(3) 0.044 Uiso 1 calc R . C37 C 0.8568(3) 0.7055(2) 0.6028(3) 0.0318(14) Uani 1 d . . H37A H 0.8385(3) 0.7282(2) 0.6367(3) 0.038 Uiso 1 calc R . C38 C 0.8242(3) 0.6545(2) 0.5776(3) 0.0270(14) Uani 1 d . . C41 C 0.7241(3) 0.7593(2) 0.8145(3) 0.0314(15) Uani 1 d . . H41A H 0.7553(3) 0.7917(2) 0.8410(3) 0.038 Uiso 1 calc R . H41B H 0.6828(3) 0.7541(2) 0.8387(3) 0.038 Uiso 1 calc R . C42 C 0.6858(3) 0.7670(2) 0.7196(3) 0.0266(14) Uani 1 d . . C43 C 0.6444(3) 0.7517(2) 0.5838(4) 0.0274(14) Uani 1 d . . C44 C 0.6279(3) 0.7310(2) 0.5028(3) 0.0304(14) Uani 1 d . . H44A H 0.6536(3) 0.6996(2) 0.4940(3) 0.036 Uiso 1 calc R . C45 C 0.5718(3) 0.7583(2) 0.4352(4) 0.036(2) Uani 1 d . . H45A H 0.5575(3) 0.7447(2) 0.3791(4) 0.043 Uiso 1 calc R . C46 C 0.5360(3) 0.8058(2) 0.4489(4) 0.039(2) Uani 1 d . . H46A H 0.4984(3) 0.8237(2) 0.4014(4) 0.047 Uiso 1 calc R . C47 C 0.5537(3) 0.8270(2) 0.5287(4) 0.036(2) Uani 1 d . . H47A H 0.5291(3) 0.8589(2) 0.5376(4) 0.043 Uiso 1 calc R . C48 C 0.6088(3) 0.7998(2) 0.5949(4) 0.0284(14) Uani 1 d . . C51 C 0.7874(3) 0.6893(2) 0.9179(3) 0.0308(14) Uani 1 d . . H51A H 0.7875(3) 0.7188(2) 0.9572(3) 0.037 Uiso 1 calc R . H51B H 0.8389(3) 0.6703(2) 0.9419(3) 0.037 Uiso 1 calc R . C52 C 0.7213(3) 0.6511(2) 0.9089(3) 0.0278(14) Uani 1 d . . C53 C 0.6487(3) 0.5900(2) 0.9419(3) 0.0300(14) Uani 1 d . . C54 C 0.6165(4) 0.5521(2) 0.9803(4) 0.043(2) Uani 1 d . . H54A H 0.6371(4) 0.5467(2) 1.0401(4) 0.052 Uiso 1 calc R . C55 C 0.5528(4) 0.5230(3) 0.9266(4) 0.047(2) Uani 1 d . . H55A H 0.5302(4) 0.4957(3) 0.9497(4) 0.056 Uiso 1 calc R . C56 C 0.5211(3) 0.5327(2) 0.8393(4) 0.041(2) Uani 1 d . . H56A H 0.4763(3) 0.5125(2) 0.8047(4) 0.049 Uiso 1 calc R . C57 C 0.5525(3) 0.5708(2) 0.8012(4) 0.034(2) Uani 1 d . . H57A H 0.5299(3) 0.5774(2) 0.7417(4) 0.041 Uiso 1 calc R . C58 C 0.6190(3) 0.5989(2) 0.8541(3) 0.0301(14) Uani 1 d . . C61 C 0.8546(3) 0.7269(2) 0.8300(3) 0.0332(15) Uani 1 d . . H61A H 0.8880(3) 0.7439(2) 0.8845(3) 0.040 Uiso 1 calc R . H61B H 0.8470(3) 0.7532(2) 0.7837(3) 0.040 Uiso 1 calc R . C62 C 0.8949(3) 0.6777(2) 0.8150(3) 0.0279(14) Uani 1 d . . C63 C 0.9164(3) 0.5980(2) 0.7775(3) 0.0285(14) Uani 1 d . . C64 C 0.9121(3) 0.5442(2) 0.7512(3) 0.036(2) Uani 1 d . . H64A H 0.8636(3) 0.5248(2) 0.7334(3) 0.043 Uiso 1 calc R . C65 C 0.9811(4) 0.5203(3) 0.7519(4) 0.044(2) Uani 1 d . . H65A H 0.9798(4) 0.4839(3) 0.7340(4) 0.053 Uiso 1 calc R . C66 C 1.0522(4) 0.5483(3) 0.7783(4) 0.048(2) Uani 1 d . . H66A H 1.0983(4) 0.5306(3) 0.7775(4) 0.058 Uiso 1 calc R . C67 C 1.0579(3) 0.6008(3) 0.8054(4) 0.041(2) Uani 1 d . . H67A H 1.1069(3) 0.6196(3) 0.8240(4) 0.050 Uiso 1 calc R . C68 C 0.9882(3) 0.6253(2) 0.8044(3) 0.0333(15) Uani 1 d . . C70 C 0.0844(4) 0.5471(3) 0.4555(5) 0.085(3) Uani 1 d . . H70A H 0.0365(4) 0.5692(3) 0.4315(5) 0.127 Uiso 1 calc R . H70B H 0.0734(4) 0.5107(3) 0.4317(5) 0.127 Uiso 1 calc R . H70C H 0.1272(4) 0.5632(3) 0.4414(5) 0.127 Uiso 1 calc R . C71 C 0.1092(4) 0.5444(3) 0.5509(5) 0.065(2) Uani 1 d . . H71A H 0.1202(4) 0.5810(3) 0.5756(5) 0.078 Uiso 1 calc R . H71B H 0.0663(4) 0.5284(3) 0.5659(5) 0.078 Uiso 1 calc R . C72 C 0.2041(4) 0.5045(3) 0.6732(5) 0.064(2) Uani 1 d . . H72A H 0.1641(4) 0.4833(3) 0.6865(5) 0.077 Uiso 1 calc R . H72B H 0.2100(4) 0.5398(3) 0.7020(5) 0.077 Uiso 1 calc R . C73 C 0.2817(4) 0.4755(3) 0.7043(5) 0.078(2) Uani 1 d . . H73A H 0.2995(4) 0.4701(3) 0.7659(5) 0.117 Uiso 1 calc R . H73B H 0.3211(4) 0.4969(3) 0.6914(5) 0.117 Uiso 1 calc R . H73C H 0.2754(4) 0.4405(3) 0.6759(5) 0.117 Uiso 1 calc R . C74 C 0.3190(5) 0.6182(3) 0.6256(6) 0.085(3) Uani 1 d . . C75 C 0.3715(4) 0.5829(3) 0.5990(5) 0.051(2) Uani 1 d . . C76 C 0.1672(8) 0.7977(4) 0.1951(6) 0.170(5) Uani 1 d . . H76A H 0.1509(8) 0.7602(4) 0.1807(6) 0.255 Uiso 1 calc R . H76B H 0.1860(8) 0.8127(4) 0.1526(6) 0.255 Uiso 1 calc R . H76C H 0.1219(8) 0.8187(4) 0.1960(6) 0.255 Uiso 1 calc R . C77 C 0.2330(6) 0.7999(4) 0.2815(7) 0.117(4) Uani 1 d . . H77A H 0.2145(6) 0.7845(4) 0.3248(7) 0.141 Uiso 1 calc R . H77B H 0.2788(6) 0.7785(4) 0.2812(7) 0.141 Uiso 1 calc R . C78 C 0.3151(5) 0.8592(4) 0.3829(7) 0.121(4) Uani 1 d . . H78A H 0.3596(5) 0.8346(4) 0.3884(7) 0.145 Uiso 1 calc R . H78B H 0.2935(5) 0.8489(4) 0.4264(7) 0.145 Uiso 1 calc R . C79 C 0.3444(5) 0.9152(4) 0.3978(6) 0.112(3) Uani 1 d . . H79A H 0.3856(5) 0.9181(4) 0.4549(6) 0.168 Uiso 1 calc R . H79B H 0.3004(5) 0.9394(4) 0.3933(6) 0.168 Uiso 1 calc R . H79C H 0.3665(5) 0.9252(4) 0.3553(6) 0.168 Uiso 1 calc R . C80 C 1.0390(6) 0.8034(4) 0.7736(6) 0.134(4) Uani 1 d . . H80A H 1.0249(6) 0.8392(4) 0.7483(6) 0.201 Uiso 1 calc R . H80B H 0.9933(6) 0.7793(4) 0.7501(6) 0.201 Uiso 1 calc R . H80C H 1.0835(6) 0.7892(4) 0.7608(6) 0.201 Uiso 1 calc R . C81 C 1.0609(5) 0.8070(3) 0.8625(6) 0.084(3) Uani 1 d . . H81A H 1.0161(5) 0.8221(3) 0.8752(6) 0.100 Uiso 1 calc R . H81B H 1.1064(5) 0.8320(3) 0.8859(6) 0.100 Uiso 1 calc R . C82 C 1.1425(5) 0.7525(4) 0.9780(5) 0.093(3) Uani 1 d . . H82A H 1.1305(5) 0.7760(4) 1.0188(5) 0.112 Uiso 1 calc R . H82B H 1.1903(5) 0.7672(4) 0.9709(5) 0.112 Uiso 1 calc R . C83 C 1.1615(5) 0.6989(4) 1.0152(5) 0.107(4) Uani 1 d . . H83A H 1.2064(5) 0.7013(4) 1.0697(5) 0.160 Uiso 1 calc R . H83B H 1.1753(5) 0.6754(4) 0.9765(5) 0.160 Uiso 1 calc R . H83C H 1.1154(5) 0.6842(4) 1.0245(5) 0.160 Uiso 1 calc R . C84 C 1.0708(4) 0.5832(3) 1.1303(5) 0.078(3) Uani 1 d . . C85 C 1.0152(4) 0.6160(3) 1.0624(4) 0.058(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02489(15) 0.0225(2) 0.02033(15) -0.0031(2) 0.00802(11) -0.00012(15) Cl1 0.0440(10) 0.0510(13) 0.0584(12) -0.0183(10) 0.0014(9) 0.0093(9) Cl2 0.0630(11) 0.0383(11) 0.0381(10) 0.0027(8) 0.0131(9) 0.0089(9) Cl3 0.0745(13) 0.0340(10) 0.0549(11) -0.0035(9) 0.0395(9) -0.0149(9) O1 0.061(3) 0.041(3) 0.055(3) -0.011(2) 0.037(2) 0.001(2) O2 0.089(4) 0.074(4) 0.079(4) -0.002(3) 0.030(3) -0.006(3) O3 0.097(4) 0.071(4) 0.089(4) 0.005(4) -0.025(4) -0.032(3) O11 0.111(5) 0.104(5) 0.194(7) 0.092(5) -0.045(5) -0.026(4) O12 0.093(5) 0.283(10) 0.194(8) -0.188(8) 0.048(5) -0.015(5) O13 0.068(3) 0.056(4) 0.088(4) -0.003(3) 0.015(3) -0.013(3) O14 0.039(3) 0.095(4) 0.088(4) -0.048(3) -0.006(3) 0.003(3) O21 0.093(4) 0.082(4) 0.153(6) 0.019(4) 0.048(4) 0.054(4) O22 0.124(5) 0.063(4) 0.074(4) 0.035(3) 0.021(3) -0.011(3) O23 0.115(4) 0.092(4) 0.050(3) -0.033(3) 0.024(3) 0.005(3) O24 0.106(4) 0.098(4) 0.044(3) -0.006(3) 0.006(3) -0.049(4) O31 0.150(5) 0.033(3) 0.044(3) -0.002(2) 0.047(3) -0.020(3) O32 0.097(4) 0.056(3) 0.061(3) -0.019(3) 0.037(3) -0.039(3) O33 0.079(4) 0.067(4) 0.231(7) -0.006(4) 0.093(4) -0.013(3) O34 0.155(5) 0.063(4) 0.029(3) -0.005(3) 0.042(3) -0.043(3) N1 0.034(3) 0.027(3) 0.019(3) -0.001(2) 0.007(2) -0.002(2) N2 0.023(3) 0.030(3) 0.023(3) -0.004(2) 0.006(2) -0.002(2) N3 0.052(4) 0.042(4) 0.054(4) 0.009(3) 0.016(3) -0.010(3) N4 0.076(5) 0.179(8) 0.056(5) 0.031(5) 0.016(4) 0.058(5) N11 0.024(2) 0.023(3) 0.022(3) 0.000(2) 0.005(2) -0.002(2) N12 0.038(3) 0.031(3) 0.021(3) 0.005(2) -0.005(2) -0.007(2) N21 0.031(3) 0.022(3) 0.025(3) -0.003(2) 0.010(2) 0.001(2) N22 0.042(3) 0.029(3) 0.033(3) 0.001(3) 0.014(2) -0.009(2) N31 0.029(3) 0.023(3) 0.028(3) -0.004(2) 0.015(2) -0.001(2) N32 0.052(3) 0.029(3) 0.039(3) -0.007(3) 0.027(3) 0.000(3) N41 0.030(3) 0.023(3) 0.025(3) -0.005(2) 0.015(2) 0.002(2) N42 0.042(3) 0.019(3) 0.039(3) 0.000(2) 0.022(2) 0.004(2) N51 0.028(2) 0.030(3) 0.021(2) -0.002(2) 0.010(2) 0.001(2) N52 0.042(3) 0.042(3) 0.014(2) 0.002(2) 0.009(2) 0.010(3) N61 0.025(2) 0.028(3) 0.029(3) -0.005(2) 0.008(2) -0.004(2) N62 0.029(3) 0.033(3) 0.030(3) 0.000(2) 0.006(2) -0.008(2) C11 0.040(4) 0.029(4) 0.018(3) 0.003(3) 0.007(3) -0.009(3) C12 0.031(3) 0.027(4) 0.020(3) 0.004(3) 0.001(3) -0.010(3) C13 0.025(3) 0.029(4) 0.030(4) 0.002(3) 0.005(3) -0.005(3) C14 0.027(3) 0.036(4) 0.037(4) -0.003(3) 0.011(3) -0.004(3) C15 0.038(4) 0.039(4) 0.063(5) -0.007(4) 0.021(4) 0.000(3) C16 0.034(4) 0.041(5) 0.082(6) 0.000(4) 0.015(4) 0.008(3) C17 0.031(4) 0.043(5) 0.057(5) 0.014(4) 0.000(3) 0.007(3) C18 0.028(4) 0.029(4) 0.037(4) 0.008(3) 0.002(3) -0.008(3) C21 0.037(3) 0.026(3) 0.024(3) -0.003(3) 0.009(3) -0.005(3) C22 0.033(3) 0.026(4) 0.026(3) -0.002(3) 0.013(3) 0.003(3) C23 0.029(3) 0.030(4) 0.027(3) 0.003(3) 0.011(3) 0.007(3) C24 0.041(4) 0.028(4) 0.040(4) 0.003(3) 0.011(3) 0.005(3) C25 0.048(4) 0.048(5) 0.034(4) 0.011(4) -0.001(3) 0.000(4) C26 0.069(5) 0.058(5) 0.034(4) 0.020(4) 0.008(4) 0.005(4) C27 0.058(4) 0.043(4) 0.043(4) 0.009(4) 0.013(4) -0.001(4) C28 0.042(4) 0.032(4) 0.028(4) 0.003(3) 0.012(3) 0.008(3) C31 0.044(4) 0.027(4) 0.034(4) -0.004(3) 0.017(3) -0.001(3) C32 0.038(4) 0.025(4) 0.026(3) -0.002(3) 0.015(3) 0.005(3) C33 0.040(4) 0.036(4) 0.034(4) 0.003(3) 0.018(3) 0.006(3) C34 0.042(4) 0.053(5) 0.043(4) 0.009(4) 0.025(3) 0.012(4) C35 0.034(4) 0.049(5) 0.047(4) 0.015(4) 0.014(3) 0.001(3) C36 0.037(4) 0.041(4) 0.033(4) 0.008(3) 0.013(3) -0.003(3) C37 0.036(4) 0.036(4) 0.026(3) 0.002(3) 0.015(3) -0.001(3) C38 0.025(3) 0.027(4) 0.028(3) 0.004(3) 0.009(3) 0.006(3) C41 0.039(4) 0.024(4) 0.031(4) -0.005(3) 0.014(3) -0.001(3) C42 0.031(3) 0.020(3) 0.033(4) 0.000(3) 0.018(3) -0.007(3) C43 0.028(3) 0.023(3) 0.033(4) 0.004(3) 0.013(3) 0.001(3) C44 0.038(4) 0.029(4) 0.027(4) 0.002(3) 0.015(3) 0.001(3) C45 0.041(4) 0.042(4) 0.026(4) 0.006(3) 0.015(3) -0.009(3) C46 0.036(4) 0.038(4) 0.042(4) 0.015(3) 0.013(3) 0.002(3) C47 0.042(4) 0.026(4) 0.045(4) 0.008(3) 0.022(3) 0.006(3) C48 0.028(3) 0.027(4) 0.033(4) 0.002(3) 0.015(3) -0.003(3) C51 0.032(3) 0.034(4) 0.025(3) -0.005(3) 0.010(3) 0.001(3) C52 0.031(3) 0.024(4) 0.026(3) -0.002(3) 0.008(3) 0.006(3) C53 0.038(4) 0.028(4) 0.026(3) 0.000(3) 0.015(3) 0.004(3) C54 0.063(5) 0.049(5) 0.029(4) 0.011(3) 0.030(3) 0.006(4) C55 0.065(5) 0.036(4) 0.055(5) 0.001(4) 0.040(4) -0.008(4) C56 0.043(4) 0.036(4) 0.050(4) -0.009(3) 0.026(3) -0.013(3) C57 0.036(4) 0.035(4) 0.034(4) -0.010(3) 0.015(3) -0.003(3) C58 0.037(4) 0.029(4) 0.031(4) 0.003(3) 0.020(3) 0.006(3) C61 0.032(3) 0.037(4) 0.026(3) -0.008(3) 0.005(3) 0.001(3) C62 0.024(3) 0.035(4) 0.021(3) 0.001(3) 0.004(3) 0.004(3) C63 0.027(3) 0.034(4) 0.022(3) 0.004(3) 0.006(3) 0.004(3) C64 0.035(4) 0.037(4) 0.036(4) 0.000(3) 0.014(3) 0.004(3) C65 0.041(4) 0.037(4) 0.053(4) -0.003(3) 0.017(3) 0.009(3) C66 0.041(4) 0.061(5) 0.044(4) 0.003(4) 0.019(3) 0.024(4) C67 0.031(4) 0.057(5) 0.036(4) 0.004(4) 0.012(3) 0.006(3) C68 0.029(3) 0.035(4) 0.034(4) 0.005(3) 0.010(3) 0.009(3) C70 0.079(6) 0.088(7) 0.098(7) 0.023(6) 0.045(5) 0.031(5) C71 0.060(5) 0.061(5) 0.083(6) -0.023(5) 0.038(4) 0.004(4) C72 0.082(6) 0.065(6) 0.068(5) -0.018(4) 0.054(5) -0.014(4) C73 0.081(6) 0.092(7) 0.070(6) 0.010(5) 0.039(5) 0.003(5) C74 0.103(6) 0.047(5) 0.138(8) -0.012(5) 0.085(6) -0.006(5) C75 0.053(5) 0.039(5) 0.056(5) 0.004(4) 0.015(4) -0.025(4) C76 0.283(16) 0.130(11) 0.108(9) -0.041(8) 0.088(10) -0.064(11) C77 0.158(10) 0.072(8) 0.137(10) -0.012(7) 0.072(8) -0.033(7) C78 0.056(5) 0.126(10) 0.139(10) 0.021(8) -0.012(6) -0.010(6) C79 0.108(8) 0.131(9) 0.106(8) -0.030(7) 0.050(6) -0.047(7) C80 0.128(9) 0.127(10) 0.131(10) 0.035(8) 0.029(8) -0.031(7) C81 0.105(7) 0.063(6) 0.094(7) 0.000(6) 0.050(6) -0.015(5) C82 0.063(6) 0.132(9) 0.079(7) -0.021(6) 0.020(5) -0.012(6) C83 0.083(7) 0.104(8) 0.103(8) 0.033(7) 0.000(5) -0.020(6) C84 0.085(6) 0.070(6) 0.058(5) 0.028(4) 0.001(4) 0.032(5) C85 0.043(4) 0.087(6) 0.043(5) -0.011(4) 0.016(4) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 N61 2.479(4) . ? Eu1 N21 2.496(4) . ? Eu1 N41 2.500(4) . ? Eu1 N51 2.503(4) . ? Eu1 N11 2.504(4) . ? Eu1 N31 2.507(4) . ? Eu1 N1 2.713(4) . ? Eu1 N2 2.725(4) . ? Cl1 O11 1.383(6) . ? Cl1 O12 1.390(6) . ? Cl1 O14 1.421(4) . ? Cl1 O13 1.428(5) . ? Cl2 O21 1.385(5) . ? Cl2 O23 1.416(5) . ? Cl2 O22 1.419(5) . ? Cl2 O24 1.442(5) . ? Cl3 O34 1.418(4) . ? Cl3 O31 1.418(4) . ? Cl3 O33 1.426(5) . ? Cl3 O32 1.453(4) . ? O1 C71 1.420(7) . ? O1 C72 1.429(7) . ? O2 C77 1.400(9) . ? O2 C78 1.408(9) . ? O3 C82 1.326(8) . ? O3 C81 1.441(9) . ? N1 C31 1.485(6) . ? N1 C21 1.486(6) . ? N1 C11 1.487(6) . ? N2 C41 1.477(6) . ? N2 C61 1.485(6) . ? N2 C51 1.491(6) . ? N3 C75 1.144(8) . ? N4 C85 1.134(8) . ? N11 C12 1.328(6) . ? N11 C13 1.401(6) . ? N12 C12 1.334(6) . ? N12 C18 1.376(7) . ? N21 C22 1.323(6) . ? N21 C23 1.404(6) . ? N22 C22 1.352(6) . ? N22 C28 1.381(6) . ? N31 C32 1.323(6) . ? N31 C38 1.401(6) . ? N32 C32 1.361(6) . ? N32 C33 1.379(7) . ? N41 C42 1.329(6) . ? N41 C43 1.415(6) . ? N42 C42 1.348(6) . ? N42 C48 1.397(6) . ? N51 C52 1.329(6) . ? N51 C58 1.406(7) . ? N52 C52 1.352(7) . ? N52 C53 1.388(6) . ? N61 C62 1.322(6) . ? N61 C63 1.406(6) . ? N62 C62 1.342(6) . ? N62 C68 1.384(7) . ? C11 C12 1.484(7) . ? C18 C17 1.398(8) . ? C18 C13 1.398(7) . ? C13 C14 1.389(7) . ? C14 C15 1.385(7) . ? C15 C16 1.405(8) . ? C16 C17 1.363(8) . ? C21 C22 1.497(7) . ? C23 C24 1.389(7) . ? C23 C28 1.400(7) . ? C24 C25 1.377(7) . ? C25 C26 1.382(8) . ? C26 C27 1.389(8) . ? C27 C28 1.384(8) . ? C31 C32 1.472(7) . ? C33 C34 1.387(8) . ? C33 C38 1.408(7) . ? C34 C35 1.375(8) . ? C35 C36 1.402(8) . ? C36 C37 1.384(7) . ? C37 C38 1.395(7) . ? C41 C42 1.507(7) . ? C43 C44 1.390(7) . ? C43 C48 1.404(7) . ? C44 C45 1.393(7) . ? C45 C46 1.409(7) . ? C46 C47 1.374(7) . ? C47 C48 1.372(7) . ? C51 C52 1.494(7) . ? C53 C54 1.392(7) . ? C53 C58 1.399(7) . ? C54 C55 1.380(8) . ? C55 C56 1.395(8) . ? C56 C57 1.384(7) . ? C57 C58 1.394(7) . ? C61 C62 1.496(7) . ? C63 C68 1.388(7) . ? C63 C64 1.403(7) . ? C64 C65 1.384(7) . ? C65 C66 1.386(8) . ? C66 C67 1.375(8) . ? C67 C68 1.401(7) . ? C70 C71 1.509(9) . ? C72 C73 1.495(9) . ? C74 C75 1.486(10) . ? C76 C77 1.506(12) . ? C78 C79 1.479(10) . ? C80 C81 1.410(10) . ? C82 C83 1.458(10) . ? C84 C85 1.463(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N61 Eu1 N21 82.23(14) . . ? N61 Eu1 N41 100.40(14) . . ? N21 Eu1 N41 176.46(14) . . ? N61 Eu1 N51 102.07(13) . . ? N21 Eu1 N51 75.49(14) . . ? N41 Eu1 N51 101.56(14) . . ? N61 Eu1 N11 174.73(14) . . ? N21 Eu1 N11 102.23(13) . . ? N41 Eu1 N11 75.27(13) . . ? N51 Eu1 N11 81.91(13) . . ? N61 Eu1 N31 74.11(13) . . ? N21 Eu1 N31 100.33(14) . . ? N41 Eu1 N31 82.72(13) . . ? N51 Eu1 N31 174.83(13) . . ? N11 Eu1 N31 102.13(13) . . ? N61 Eu1 N1 117.15(14) . . ? N21 Eu1 N1 63.63(13) . . ? N41 Eu1 N1 116.69(13) . . ? N51 Eu1 N1 116.32(14) . . ? N11 Eu1 N1 63.25(13) . . ? N31 Eu1 N1 63.50(13) . . ? N61 Eu1 N2 64.04(14) . . ? N21 Eu1 N2 116.81(13) . . ? N41 Eu1 N2 62.80(13) . . ? N51 Eu1 N2 63.01(14) . . ? N11 Eu1 N2 115.57(13) . . ? N31 Eu1 N2 117.26(13) . . ? N1 Eu1 N2 178.81(13) . . ? O11 Cl1 O12 112.1(6) . . ? O11 Cl1 O14 109.2(4) . . ? O12 Cl1 O14 107.0(3) . . ? O11 Cl1 O13 107.4(3) . . ? O12 Cl1 O13 111.2(5) . . ? O14 Cl1 O13 109.9(3) . . ? O21 Cl2 O23 109.1(3) . . ? O21 Cl2 O22 112.3(4) . . ? O23 Cl2 O22 109.7(3) . . ? O21 Cl2 O24 110.0(4) . . ? O23 Cl2 O24 109.1(3) . . ? O22 Cl2 O24 106.5(3) . . ? O34 Cl3 O31 109.6(3) . . ? O34 Cl3 O33 113.1(4) . . ? O31 Cl3 O33 107.0(3) . . ? O34 Cl3 O32 107.3(3) . . ? O31 Cl3 O32 111.7(3) . . ? O33 Cl3 O32 108.2(3) . . ? C71 O1 C72 112.1(5) . . ? C77 O2 C78 112.3(7) . . ? C82 O3 C81 119.2(7) . . ? C31 N1 C21 110.0(4) . . ? C31 N1 C11 109.9(4) . . ? C21 N1 C11 110.0(4) . . ? C31 N1 Eu1 109.1(3) . . ? C21 N1 Eu1 108.8(3) . . ? C11 N1 Eu1 109.0(3) . . ? C41 N2 C61 110.0(4) . . ? C41 N2 C51 110.1(4) . . ? C61 N2 C51 110.1(4) . . ? C41 N2 Eu1 109.5(3) . . ? C61 N2 Eu1 107.8(3) . . ? C51 N2 Eu1 109.2(3) . . ? C12 N11 C13 104.9(4) . . ? C12 N11 Eu1 117.4(3) . . ? C13 N11 Eu1 130.9(3) . . ? C12 N12 C18 107.9(5) . . ? C22 N21 C23 105.3(4) . . ? C22 N21 Eu1 116.9(3) . . ? C23 N21 Eu1 131.5(3) . . ? C22 N22 C28 107.6(5) . . ? C32 N31 C38 105.2(4) . . ? C32 N31 Eu1 117.9(3) . . ? C38 N31 Eu1 133.6(3) . . ? C32 N32 C33 108.1(5) . . ? C42 N41 C43 104.6(4) . . ? C42 N41 Eu1 116.8(3) . . ? C43 N41 Eu1 127.8(3) . . ? C42 N42 C48 107.2(5) . . ? C52 N51 C58 105.2(4) . . ? C52 N51 Eu1 115.6(3) . . ? C58 N51 Eu1 127.1(3) . . ? C52 N52 C53 108.0(4) . . ? C62 N61 C63 104.7(4) . . ? C62 N61 Eu1 117.9(4) . . ? C63 N61 Eu1 133.3(3) . . ? C62 N62 C68 107.5(5) . . ? C12 C11 N1 110.4(4) . . ? N11 C12 N12 112.9(5) . . ? N11 C12 C11 122.6(5) . . ? N12 C12 C11 124.5(5) . . ? N12 C18 C17 133.0(6) . . ? N12 C18 C13 105.6(5) . . ? C17 C18 C13 121.4(6) . . ? C14 C13 C18 120.8(6) . . ? C14 C13 N11 130.6(5) . . ? C18 C13 N11 108.7(5) . . ? C15 C14 C13 117.8(6) . . ? C14 C15 C16 120.7(6) . . ? C17 C16 C15 122.1(6) . . ? C16 C17 C18 117.2(6) . . ? N1 C21 C22 108.9(4) . . ? N21 C22 N22 112.6(5) . . ? N21 C22 C21 124.0(5) . . ? N22 C22 C21 123.4(5) . . ? C24 C23 C28 119.9(5) . . ? C24 C23 N21 131.3(5) . . ? C28 C23 N21 108.8(5) . . ? C25 C24 C23 117.8(6) . . ? C24 C25 C26 121.1(6) . . ? C25 C26 C27 122.9(6) . . ? C28 C27 C26 115.1(6) . . ? N22 C28 C27 131.1(6) . . ? N22 C28 C23 105.7(5) . . ? C27 C28 C23 123.1(5) . . ? C32 C31 N1 109.3(4) . . ? N31 C32 N32 112.3(5) . . ? N31 C32 C31 124.1(5) . . ? N32 C32 C31 123.5(5) . . ? N32 C33 C34 132.8(6) . . ? N32 C33 C38 104.9(5) . . ? C34 C33 C38 122.2(6) . . ? C35 C34 C33 116.8(6) . . ? C34 C35 C36 121.9(6) . . ? C37 C36 C35 121.3(6) . . ? C36 C37 C38 117.6(5) . . ? C37 C38 N31 130.4(5) . . ? C37 C38 C33 120.1(5) . . ? N31 C38 C33 109.5(5) . . ? N2 C41 C42 109.3(4) . . ? N41 C42 N42 113.6(5) . . ? N41 C42 C41 122.5(5) . . ? N42 C42 C41 123.7(5) . . ? C44 C43 C48 120.4(5) . . ? C44 C43 N41 130.4(5) . . ? C48 C43 N41 109.1(5) . . ? C43 C44 C45 117.0(5) . . ? C44 C45 C46 120.9(5) . . ? C47 C46 C45 122.1(5) . . ? C48 C47 C46 116.5(5) . . ? C47 C48 N42 131.5(5) . . ? C47 C48 C43 122.9(5) . . ? N42 C48 C43 105.4(5) . . ? N2 C51 C52 109.3(4) . . ? N51 C52 N52 112.3(5) . . ? N51 C52 C51 123.5(5) . . ? N52 C52 C51 124.1(5) . . ? N52 C53 C54 132.1(5) . . ? N52 C53 C58 105.1(5) . . ? C54 C53 C58 122.8(5) . . ? C55 C54 C53 116.3(5) . . ? C54 C55 C56 121.4(6) . . ? C57 C56 C55 122.3(6) . . ? C56 C57 C58 116.9(5) . . ? C57 C58 C53 120.2(5) . . ? C57 C58 N51 130.5(5) . . ? C53 C58 N51 109.3(5) . . ? N2 C61 C62 109.4(5) . . ? N61 C62 N62 113.0(5) . . ? N61 C62 C61 123.7(5) . . ? N62 C62 C61 123.2(5) . . ? C68 C63 C64 120.3(5) . . ? C68 C63 N61 109.2(5) . . ? C64 C63 N61 130.5(5) . . ? C65 C64 C63 117.6(5) . . ? C64 C65 C66 121.4(6) . . ? C67 C66 C65 122.0(6) . . ? C66 C67 C68 117.0(6) . . ? N62 C68 C63 105.6(5) . . ? N62 C68 C67 132.6(5) . . ? C63 C68 C67 121.8(6) . . ? O1 C71 C70 107.9(6) . . ? O1 C72 C73 109.1(6) . . ? N3 C75 C74 179.5(8) . . ? O2 C77 C76 108.9(9) . . ? O2 C78 C79 110.9(8) . . ? C80 C81 O3 112.1(8) . . ? O3 C82 C83 116.2(8) . . ? N4 C85 C84 178.9(8) . . ? _refine_diff_density_max 0.949 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.107 #=END data_Lu(ntb)2Cl3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48.50 H58 Cl3 Lu N14 O7.50' _chemical_formula_weight 1238.41 _chemical_melting_point ? _chemical_compound_source ? 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' 'Lu' 'Lu' -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 28.03400(10) _cell_length_b 14.87580(10) _cell_length_c 27.7355(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11566.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method ? _exptl_crystal_F_000 5032 _exptl_absorpt_coefficient_mu 1.905 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51787 _diffrn_reflns_av_R_equivalents 0.1442 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10926 _reflns_number_observed 6063 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1381P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10926 _refine_ls_number_parameters 720 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1555 _refine_ls_R_factor_obs 0.0867 _refine_ls_wR_factor_all 0.2566 _refine_ls_wR_factor_obs 0.2266 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.272 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.272 _refine_ls_shift/esd_max -0.365 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Lu Lu 0.127320(4) 0.376410(11) 0.369230(5) 0.02831(4) Uani 1 d . . N1 N 0.19504(9) 0.2710(2) 0.33205(10) 0.0358(9) Uani 1 d . . N2 N 0.06027(8) 0.4809(2) 0.40592(9) 0.0320(8) Uani 1 d . . N11 N 0.18039(8) 0.4490(2) 0.31258(9) 0.0271(8) Uani 1 d . . N12 N 0.21435(10) 0.4447(2) 0.24088(10) 0.0395(9) Uani 1 d . . H12A H 0.22826(10) 0.4239(2) 0.21560(10) 0.047 Uiso 1 calc R . N21 N 0.09985(9) 0.2464(2) 0.32421(10) 0.0336(8) Uani 1 d . . N22 N 0.10358(10) 0.0991(2) 0.31969(11) 0.0383(9) Uani 1 d . . H22A H 0.11584(10) 0.0462(2) 0.31824(11) 0.046 Uiso 1 calc R . N31 N 0.18313(8) 0.3099(2) 0.42617(9) 0.0282(8) Uani 1 d . . N32 N 0.25869(10) 0.2954(2) 0.44615(10) 0.0401(9) Uani 1 d . . H32A H 0.28869(10) 0.2855(2) 0.44245(10) 0.048 Uiso 1 calc R . N41 N 0.07815(8) 0.4548(2) 0.31059(9) 0.0283(8) Uani 1 d . . N42 N 0.05206(8) 0.5899(2) 0.28757(10) 0.0348(9) Uani 1 d . . H42A H 0.04054(8) 0.6434(2) 0.28928(10) 0.042 Uiso 1 calc R . N51 N 0.07026(8) 0.3044(2) 0.42023(10) 0.0319(8) Uani 1 d . . N52 N -0.00556(10) 0.2724(2) 0.43112(10) 0.0400(9) Uani 1 d . . H52A H -0.03593(10) 0.2799(2) 0.43275(10) 0.048 Uiso 1 calc R . N61 N 0.15465(8) 0.4962(2) 0.41874(9) 0.0332(8) Uani 1 d . . N62 N 0.14962(10) 0.5676(2) 0.48835(11) 0.0434(10) Uani 1 d . . H62A H 0.13688(10) 0.5910(2) 0.51363(11) 0.052 Uiso 1 calc R . C11 C 0.20269(11) 0.2982(2) 0.28246(12) 0.0378(11) Uani 1 d . . H11A H 0.17843(11) 0.2717(2) 0.26199(12) 0.045 Uiso 1 calc R . H11B H 0.23361(11) 0.2772(2) 0.27155(12) 0.045 Uiso 1 calc R . C12 C 0.20052(11) 0.3970(2) 0.27893(11) 0.0343(11) Uani 1 d . . C13 C 0.18186(10) 0.5372(2) 0.29558(12) 0.0351(10) Uani 1 d . . C14 C 0.16688(10) 0.6138(2) 0.31319(13) 0.0326(10) Uani 1 d . . H14A H 0.15442(10) 0.6165(2) 0.34423(13) 0.039 Uiso 1 calc R . C15 C 0.16973(11) 0.6919(3) 0.28499(15) 0.0529(13) Uani 1 d . . H15A H 0.15896(11) 0.7465(3) 0.29724(15) 0.064 Uiso 1 calc R . C16 C 0.18819(13) 0.6879(3) 0.23989(14) 0.0497(13) Uani 1 d . . H16A H 0.18857(13) 0.7399(3) 0.22131(14) 0.060 Uiso 1 calc R . C17 C 0.20614(12) 0.6111(3) 0.22068(15) 0.0536(13) Uani 1 d . . H17A H 0.22013(12) 0.6102(3) 0.19028(15) 0.064 Uiso 1 calc R . C18 C 0.20257(11) 0.5329(2) 0.24897(13) 0.0402(11) Uani 1 d . . C21 C 0.17947(11) 0.1779(2) 0.33364(13) 0.0384(11) Uani 1 d . . H21A H 0.18732(11) 0.1517(2) 0.36465(13) 0.046 Uiso 1 calc R . H21B H 0.19544(11) 0.1435(2) 0.30869(13) 0.046 Uiso 1 calc R . C22 C 0.12768(10) 0.1757(3) 0.32606(12) 0.0352(11) Uani 1 d . . C23 C 0.05326(11) 0.2122(2) 0.31882(12) 0.0354(10) Uani 1 d . . C24 C 0.01072(11) 0.2550(2) 0.31425(12) 0.0365(11) Uani 1 d . . H24A H 0.00882(11) 0.3174(2) 0.31337(12) 0.044 Uiso 1 calc R . C25 C -0.02879(13) 0.2031(3) 0.31103(13) 0.0461(12) Uani 1 d . . H25A H -0.05839(13) 0.2310(3) 0.30872(13) 0.055 Uiso 1 calc R . C26 C -0.02686(14) 0.1105(3) 0.31104(15) 0.0527(13) Uani 1 d . . H26A H -0.05515(14) 0.0778(3) 0.31009(15) 0.063 Uiso 1 calc R . C27 C 0.01595(13) 0.0650(3) 0.3124(2) 0.0588(14) Uani 1 d . . H27A H 0.01808(13) 0.0027(3) 0.3112(2) 0.071 Uiso 1 calc R . C28 C 0.05499(11) 0.1196(3) 0.31578(13) 0.0404(11) Uani 1 d . . C31 C 0.23920(12) 0.2823(2) 0.36107(12) 0.0372(11) Uani 1 d . . H31A H 0.25907(12) 0.2292(2) 0.35819(12) 0.045 Uiso 1 calc R . H31B H 0.25719(12) 0.3336(2) 0.34946(12) 0.045 Uiso 1 calc R . C32 C 0.22569(10) 0.2960(2) 0.41127(12) 0.0306(10) Uani 1 d . . C33 C 0.18736(11) 0.3214(2) 0.47506(12) 0.0345(10) Uani 1 d . . C34 C 0.15406(13) 0.3356(3) 0.51040(12) 0.0436(12) Uani 1 d . . H34A H 0.12178(13) 0.3374(3) 0.50272(12) 0.052 Uiso 1 calc R . C35 C 0.16827(14) 0.3468(3) 0.55592(14) 0.0545(14) Uani 1 d . . H35A H 0.14612(14) 0.3590(3) 0.58000(14) 0.065 Uiso 1 calc R . C36 C 0.2162(2) 0.3400(3) 0.5669(2) 0.067(2) Uani 1 d . . H36A H 0.2252(2) 0.3479(3) 0.5990(2) 0.081 Uiso 1 calc R . C37 C 0.25093(14) 0.3227(3) 0.53454(15) 0.0540(14) Uani 1 d . . H37A H 0.28281(14) 0.3177(3) 0.54343(15) 0.065 Uiso 1 calc R . C38 C 0.23635(11) 0.3130(3) 0.48812(12) 0.0373(11) Uani 1 d . . C41 C 0.05386(13) 0.5607(2) 0.37576(11) 0.0394(11) Uani 1 d . . H41A H 0.07689(13) 0.6064(2) 0.38470(11) 0.047 Uiso 1 calc R . H41B H 0.02211(13) 0.5851(2) 0.38039(11) 0.047 Uiso 1 calc R . C42 C 0.06053(11) 0.5353(2) 0.32518(13) 0.0358(11) Uani 1 d . . C43 C 0.08066(10) 0.4607(2) 0.26061(12) 0.0326(10) Uani 1 d . . C44 C 0.09630(11) 0.3998(3) 0.22747(13) 0.0413(12) Uani 1 d . . H44A H 0.10714(11) 0.3433(3) 0.23670(13) 0.050 Uiso 1 calc R . C45 C 0.09540(12) 0.4256(3) 0.17938(13) 0.0426(12) Uani 1 d . . H45A H 0.10410(12) 0.3847(3) 0.15557(13) 0.051 Uiso 1 calc R . C46 C 0.08154(11) 0.5123(3) 0.16657(14) 0.0452(12) Uani 1 d . . H46A H 0.08285(11) 0.5284(3) 0.13420(14) 0.054 Uiso 1 calc R . C47 C 0.06611(12) 0.5749(3) 0.19907(14) 0.0501(13) Uani 1 d . . H47A H 0.05714(12) 0.6327(3) 0.19003(14) 0.060 Uiso 1 calc R . C48 C 0.06487(11) 0.5461(2) 0.24594(12) 0.0354(10) Uani 1 d . . C51 C 0.01563(10) 0.4287(2) 0.40822(13) 0.0353(11) Uani 1 d . . H51A H -0.00551(10) 0.4543(2) 0.43226(13) 0.042 Uiso 1 calc R . H51B H -0.00042(10) 0.4305(2) 0.37725(13) 0.042 Uiso 1 calc R . C52 C 0.02701(10) 0.3375(2) 0.42068(11) 0.0313(10) Uani 1 d . . C53 C 0.06545(10) 0.2121(2) 0.43160(12) 0.0326(10) Uani 1 d . . C54 C 0.09813(13) 0.1444(3) 0.43688(14) 0.0491(13) Uani 1 d . . H54A H 0.13058(13) 0.1562(3) 0.43399(14) 0.059 Uiso 1 calc R . C55 C 0.08255(13) 0.0596(3) 0.4464(2) 0.0548(13) Uani 1 d . . H55A H 0.10479(13) 0.0136(3) 0.4493(2) 0.066 Uiso 1 calc R . C56 C 0.03465(12) 0.0399(3) 0.45183(14) 0.0552(13) Uani 1 d . . H56A H 0.02497(12) -0.0188(3) 0.45789(14) 0.066 Uiso 1 calc R . C57 C 0.00249(13) 0.1053(3) 0.44835(14) 0.0523(13) Uani 1 d . . H57A H -0.02976(13) 0.0927(3) 0.45238(14) 0.063 Uiso 1 calc R . C58 C 0.01763(11) 0.1941(2) 0.43848(12) 0.0382(11) Uani 1 d . . C61 C 0.07437(10) 0.5069(3) 0.45474(11) 0.0349(10) Uani 1 d . . H61A H 0.06749(10) 0.4588(3) 0.47734(11) 0.042 Uiso 1 calc R . H61B H 0.05729(10) 0.5604(3) 0.46482(11) 0.042 Uiso 1 calc R . C62 C 0.12725(10) 0.5249(2) 0.45276(12) 0.0330(10) Uani 1 d . . C63 C 0.20057(10) 0.5228(2) 0.43338(11) 0.0297(9) Uani 1 d . . C64 C 0.24431(11) 0.5097(2) 0.41222(12) 0.0357(11) Uani 1 d . . H64A H 0.24654(11) 0.4815(2) 0.38237(12) 0.043 Uiso 1 calc R . C65 C 0.28462(12) 0.5384(2) 0.43548(13) 0.0444(12) Uani 1 d . . H65A H 0.31447(12) 0.5287(2) 0.42180(13) 0.053 Uiso 1 calc R . C66 C 0.28078(14) 0.5818(3) 0.47930(14) 0.0525(13) Uani 1 d . . H66A H 0.30834(14) 0.6016(3) 0.49466(14) 0.063 Uiso 1 calc R . C67 C 0.23742(13) 0.5965(3) 0.50079(15) 0.0492(13) Uani 1 d . . H67A H 0.23467(13) 0.6251(3) 0.53048(15) 0.059 Uiso 1 calc R . C68 C 0.19885(11) 0.5668(3) 0.47609(13) 0.0436(12) Uani 1 d . . Cl1 Cl -0.11730(3) 0.29317(8) 0.43450(4) 0.0547(3) Uani 1 d . . Cl2 Cl 0.16646(4) 0.92930(8) 0.32592(5) 0.0745(4) Uani 1 d . . Cl3 Cl -0.03031(4) 0.64093(9) 0.45495(4) 0.0739(4) Uani 1 d . . C1 C 0.0922(3) 0.8761(7) 0.2206(5) 0.114(4) Uani 0.50 d P 1 O1 O 0.1418(4) 0.9379(6) 0.2191(3) 0.193(4) Uani 0.50 d P 1 O2A O 0.0137(2) 0.7560(3) 0.3175(2) 0.069(2) Uani 0.50 d P . O2B O 0.0324(3) 0.7845(6) 0.3117(5) 0.329(5) Uani 0.50 d P . O3A O 0.2198(3) 0.8974(6) 0.1723(2) 0.129(4) Uani 0.50 d P . O3B O 0.2486(2) 0.8470(4) 0.1646(2) 0.075(2) Uani 0.50 d P . O3C O 0.2289(5) 0.8841(6) 0.1273(2) 0.217(5) Uani 0.50 d P . O4A O 0.1709(2) 0.2235(4) 0.1600(2) 0.093(2) Uani 0.50 d P . O4B O 0.1657(2) 0.1456(5) 0.1724(4) 0.152(4) Uani 0.50 d P . O5B O 0.0480(3) 0.7813(4) 0.1124(2) 0.120(3) Uani 0.50 d P . O5A O 0.0700(3) 0.8383(5) 0.0937(3) 0.114(3) Uani 0.50 d P . O6 O -0.07044(14) 0.2407(5) 0.5362(2) 0.193(3) Uani 1 d . . O7 O -0.14896(10) 0.2223(3) 0.58961(13) 0.100(2) Uani 1 d . . O8A O 0.1372(8) 0.9009(17) 0.2012(9) 0.169(9) Uiso 0.25 d P 2 O8B O 0.1428(12) 0.8770(22) 0.1370(10) 0.235(14) Uiso 0.25 d P 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 Lu 0.01352(6) 0.03753(7) 0.03388(7) 0.00193(7) 0.00203(6) 0.00238(6) N1 0.0200(13) 0.051(2) 0.037(2) -0.0046(14) 0.0041(12) -0.0005(13) N2 0.0148(12) 0.043(2) 0.038(2) 0.0000(14) 0.0052(11) 0.0052(12) N11 0.0175(12) 0.0288(14) 0.0350(15) 0.0029(13) 0.0030(11) 0.0028(11) N12 0.037(2) 0.048(2) 0.033(2) 0.0056(14) 0.0011(13) -0.0025(14) N21 0.0268(13) 0.035(2) 0.039(2) -0.0042(13) 0.0020(12) 0.0095(13) N22 0.042(2) 0.0206(15) 0.052(2) -0.0018(13) 0.0004(14) 0.0010(13) N31 0.0113(11) 0.040(2) 0.0336(15) 0.0021(13) -0.0009(11) 0.0088(12) N32 0.0276(14) 0.043(2) 0.050(2) 0.008(2) -0.0037(13) 0.0041(14) N41 0.0173(12) 0.0293(14) 0.038(2) 0.0054(13) -0.0040(11) -0.0004(11) N42 0.0143(12) 0.049(2) 0.041(2) 0.0045(14) -0.0028(12) 0.0076(12) N51 0.0143(12) 0.046(2) 0.0353(15) 0.0081(14) 0.0039(11) -0.0018(12) N52 0.0240(14) 0.052(2) 0.044(2) 0.009(2) -0.0024(13) 0.0005(14) N61 0.0181(12) 0.046(2) 0.0359(15) -0.0022(14) 0.0069(11) 0.0041(13) N62 0.033(2) 0.051(2) 0.046(2) 0.001(2) -0.0007(14) 0.0072(15) C11 0.024(2) 0.046(2) 0.044(2) -0.008(2) 0.007(2) 0.007(2) C12 0.020(2) 0.059(2) 0.023(2) -0.002(2) -0.0004(13) -0.004(2) C13 0.0124(14) 0.048(2) 0.045(2) 0.009(2) -0.0046(14) -0.0143(15) C14 0.0163(14) 0.026(2) 0.055(2) 0.005(2) -0.0033(14) 0.0018(14) C15 0.020(2) 0.057(2) 0.082(3) 0.003(2) -0.025(2) -0.009(2) C16 0.047(2) 0.044(2) 0.058(3) 0.008(2) -0.010(2) -0.011(2) C17 0.035(2) 0.068(3) 0.058(2) 0.022(2) -0.013(2) -0.021(2) C18 0.022(2) 0.057(2) 0.042(2) 0.015(2) -0.0026(15) -0.005(2) C21 0.026(2) 0.051(2) 0.039(2) -0.010(2) 0.0007(15) 0.012(2) C22 0.0156(15) 0.054(2) 0.036(2) -0.002(2) 0.0076(14) -0.002(2) C23 0.023(2) 0.045(2) 0.039(2) 0.008(2) 0.0054(14) 0.003(2) C24 0.020(2) 0.041(2) 0.048(2) -0.001(2) 0.0054(15) 0.001(2) C25 0.033(2) 0.049(2) 0.057(2) -0.004(2) 0.002(2) 0.006(2) C26 0.038(2) 0.050(2) 0.070(3) 0.003(2) -0.009(2) -0.002(2) C27 0.034(2) 0.057(2) 0.085(3) 0.019(2) 0.001(2) -0.003(2) C28 0.025(2) 0.055(2) 0.041(2) 0.003(2) -0.0011(15) 0.000(2) C31 0.023(2) 0.031(2) 0.058(2) -0.003(2) 0.000(2) 0.000(2) C32 0.0174(14) 0.036(2) 0.038(2) 0.004(2) -0.0083(13) 0.0054(14) C33 0.021(2) 0.046(2) 0.036(2) 0.011(2) -0.0037(14) 0.009(2) C34 0.037(2) 0.060(2) 0.034(2) -0.002(2) 0.006(2) 0.009(2) C35 0.042(2) 0.071(3) 0.051(2) 0.008(2) 0.006(2) 0.013(2) C36 0.062(3) 0.091(3) 0.050(3) 0.001(2) -0.016(2) 0.000(3) C37 0.039(2) 0.060(3) 0.063(3) 0.008(2) 0.007(2) 0.004(2) C38 0.024(2) 0.055(2) 0.033(2) 0.008(2) 0.0010(15) -0.003(2) C41 0.036(2) 0.044(2) 0.037(2) 0.005(2) 0.010(2) 0.007(2) C42 0.023(2) 0.032(2) 0.052(2) 0.007(2) -0.001(2) -0.0010(15) C43 0.0132(14) 0.051(2) 0.034(2) -0.006(2) 0.0018(13) -0.0036(15) C44 0.017(2) 0.064(3) 0.043(2) -0.004(2) -0.0033(15) -0.005(2) C45 0.032(2) 0.060(2) 0.036(2) -0.009(2) -0.001(2) -0.013(2) C46 0.029(2) 0.058(2) 0.049(2) 0.008(2) -0.016(2) -0.004(2) C47 0.027(2) 0.069(3) 0.055(2) 0.008(2) 0.001(2) -0.011(2) C48 0.0188(15) 0.050(2) 0.037(2) 0.006(2) -0.0050(14) -0.008(2) C51 0.0057(13) 0.046(2) 0.054(2) 0.007(2) 0.0080(13) 0.0072(14) C52 0.0084(13) 0.057(2) 0.028(2) 0.009(2) 0.0021(12) -0.0061(14) C53 0.0135(14) 0.053(2) 0.032(2) 0.009(2) -0.0012(13) 0.0089(15) C54 0.028(2) 0.063(3) 0.056(2) 0.016(2) 0.008(2) 0.007(2) C55 0.036(2) 0.048(2) 0.080(3) 0.020(2) 0.006(2) 0.018(2) C56 0.033(2) 0.062(3) 0.070(3) 0.028(2) 0.016(2) -0.002(2) C57 0.028(2) 0.062(3) 0.066(3) 0.011(2) 0.009(2) -0.013(2) C58 0.024(2) 0.046(2) 0.044(2) 0.022(2) 0.0045(15) -0.004(2) C61 0.021(2) 0.050(2) 0.033(2) 0.001(2) 0.0018(14) 0.009(2) C62 0.026(2) 0.035(2) 0.037(2) 0.005(2) -0.0070(14) 0.003(2) C63 0.024(2) 0.030(2) 0.035(2) -0.001(2) -0.0033(14) 0.0129(14) C64 0.033(2) 0.040(2) 0.034(2) -0.003(2) 0.0012(15) -0.005(2) C65 0.027(2) 0.048(2) 0.058(2) 0.014(2) 0.005(2) -0.009(2) C66 0.047(2) 0.063(3) 0.048(2) 0.004(2) -0.016(2) -0.014(2) C67 0.039(2) 0.053(2) 0.056(2) -0.006(2) -0.008(2) -0.003(2) C68 0.021(2) 0.066(3) 0.044(2) 0.013(2) -0.006(2) -0.007(2) Cl1 0.0249(4) 0.0842(7) 0.0550(6) -0.0151(6) 0.0043(4) 0.0047(5) Cl2 0.0612(6) 0.0588(7) 0.1034(9) -0.0248(6) -0.0308(6) 0.0246(5) Cl3 0.0443(5) 0.1121(9) 0.0653(7) 0.0041(7) 0.0215(5) 0.0311(6) C1 0.052(5) 0.085(7) 0.206(10) -0.063(7) -0.067(5) 0.005(5) O1 0.346(9) 0.199(7) 0.035(4) 0.025(4) 0.040(5) 0.188(6) O2A 0.035(3) 0.034(3) 0.136(5) 0.011(3) -0.014(3) -0.004(3) O2B 0.207(5) 0.195(6) 0.585(14) 0.254(7) 0.273(6) 0.182(4) O3A 0.187(8) 0.143(7) 0.058(4) -0.027(5) -0.038(5) 0.023(6) O3B 0.082(4) 0.092(5) 0.053(4) -0.025(3) -0.004(3) -0.029(3) O3C 0.485(13) 0.140(6) 0.025(3) -0.034(4) -0.076(5) 0.182(6) O4A 0.120(4) 0.078(4) 0.082(4) -0.013(3) -0.074(3) -0.001(4) O4B 0.042(3) 0.075(5) 0.338(12) 0.018(6) -0.065(5) 0.009(4) O5B 0.271(9) 0.060(4) 0.028(3) -0.014(3) -0.011(5) -0.052(5) O5A 0.122(6) 0.135(6) 0.086(5) -0.067(4) 0.023(4) -0.041(5) O6 0.052(2) 0.353(8) 0.174(5) 0.033(5) 0.004(3) 0.001(4) O7 0.036(2) 0.154(3) 0.110(3) 0.007(3) -0.012(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu N61 2.377(3) . ? Lu N51 2.389(3) . ? Lu N11 2.418(2) . ? Lu N21 2.428(3) . ? Lu N41 2.430(2) . ? Lu N31 2.433(2) . ? Lu N2 2.643(3) . ? Lu N1 2.669(3) . ? N1 C11 1.450(4) . ? N1 C21 1.453(4) . ? N1 C31 1.486(4) . ? N2 C61 1.463(4) . ? N2 C41 1.463(4) . ? N2 C51 1.474(4) . ? N11 C12 1.337(4) . ? N11 C13 1.395(4) . ? N12 C12 1.330(4) . ? N12 C18 1.372(5) . ? N21 C22 1.310(4) . ? N21 C23 1.410(4) . ? N22 C22 1.337(5) . ? N22 C28 1.400(4) . ? N31 C32 1.279(4) . ? N31 C33 1.372(4) . ? N32 C32 1.339(4) . ? N32 C38 1.348(4) . ? N41 C42 1.357(4) . ? N41 C43 1.391(4) . ? N42 C42 1.344(4) . ? N42 C48 1.373(4) . ? N51 C52 1.308(4) . ? N51 C53 1.416(4) . ? N52 C58 1.349(4) . ? N52 C52 1.363(4) . ? N61 C62 1.289(4) . ? N61 C63 1.407(4) . ? N62 C62 1.331(4) . ? N62 C68 1.421(4) . ? C11 C12 1.473(5) . ? C13 C14 1.309(5) . ? C13 C18 1.419(5) . ? C14 C15 1.403(5) . ? C15 C16 1.355(5) . ? C16 C17 1.356(5) . ? C17 C18 1.406(5) . ? C21 C22 1.467(4) . ? C23 C24 1.358(4) . ? C23 C28 1.380(5) . ? C24 C25 1.353(5) . ? C25 C26 1.379(5) . ? C26 C27 1.378(5) . ? C27 C28 1.366(5) . ? C31 C32 1.457(5) . ? C33 C34 1.370(5) . ? C33 C38 1.426(4) . ? C34 C35 1.334(5) . ? C35 C36 1.382(6) . ? C36 C37 1.350(6) . ? C37 C38 1.358(5) . ? C41 C42 1.465(5) . ? C43 C44 1.363(5) . ? C43 C48 1.406(5) . ? C44 C45 1.388(5) . ? C45 C46 1.393(5) . ? C46 C47 1.367(5) . ? C47 C48 1.369(5) . ? C51 C52 1.436(5) . ? C53 C54 1.370(5) . ? C53 C58 1.380(4) . ? C54 C55 1.360(5) . ? C55 C56 1.383(5) . ? C56 C57 1.330(5) . ? C57 C58 1.415(5) . ? C61 C62 1.508(4) . ? C63 C68 1.354(5) . ? C63 C64 1.373(4) . ? C64 C65 1.370(5) . ? C65 C66 1.380(5) . ? C66 C67 1.371(5) . ? C67 C68 1.354(5) . ? O2A O2B 0.694(10) . ? O3A O3B 1.123(11) . ? O3A O3C 1.290(10) . ? O3B O3C 1.297(10) . ? O4A O4B 1.218(10) . ? O5B O5A 1.170(10) . ? O1 C1 1.666(14) . ? 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 N61 Lu N51 102.11(9) . . ? N61 Lu N11 80.92(9) . . ? N51 Lu N11 175.46(8) . . ? N61 Lu N21 175.46(9) . . ? N51 Lu N21 74.63(9) . . ? N11 Lu N21 102.52(9) . . ? N61 Lu N41 102.11(9) . . ? N51 Lu N41 103.39(8) . . ? N11 Lu N41 72.53(8) . . ? N21 Lu N41 81.84(9) . . ? N61 Lu N31 73.90(9) . . ? N51 Lu N31 82.18(8) . . ? N11 Lu N31 101.99(8) . . ? N21 Lu N31 102.34(9) . . ? N41 Lu N31 173.86(8) . . ? N61 Lu N2 64.26(8) . . ? N51 Lu N2 63.85(9) . . ? N11 Lu N2 115.15(8) . . ? N21 Lu N2 116.17(8) . . ? N41 Lu N2 64.66(8) . . ? N31 Lu N2 116.53(8) . . ? N61 Lu N1 115.74(8) . . ? N51 Lu N1 116.22(9) . . ? N11 Lu N1 64.77(8) . . ? N21 Lu N1 63.83(8) . . ? N41 Lu N1 115.25(8) . . ? N31 Lu N1 63.55(8) . . ? N2 Lu N1 179.91(7) . . ? C11 N1 C21 109.8(3) . . ? C11 N1 C31 111.0(2) . . ? C21 N1 C31 110.0(3) . . ? C11 N1 Lu 107.9(2) . . ? C21 N1 Lu 109.5(2) . . ? C31 N1 Lu 108.5(2) . . ? C61 N2 C41 110.4(3) . . ? C61 N2 C51 109.2(2) . . ? C41 N2 C51 110.3(2) . . ? C61 N2 Lu 108.6(2) . . ? C41 N2 Lu 110.1(2) . . ? C51 N2 Lu 108.1(2) . . ? C12 N11 C13 107.2(3) . . ? C12 N11 Lu 117.0(2) . . ? C13 N11 Lu 131.1(2) . . ? C12 N12 C18 108.1(3) . . ? C22 N21 C23 105.4(3) . . ? C22 N21 Lu 115.5(2) . . ? C23 N21 Lu 129.5(2) . . ? C22 N22 C28 108.4(3) . . ? C32 N31 C33 105.0(3) . . ? C32 N31 Lu 117.1(2) . . ? C33 N31 Lu 130.3(2) . . ? C32 N32 C38 107.6(3) . . ? C42 N41 C43 105.1(3) . . ? C42 N41 Lu 115.5(2) . . ? C43 N41 Lu 132.0(2) . . ? C42 N42 C48 108.6(3) . . ? C52 N51 C53 105.9(3) . . ? C52 N51 Lu 117.2(2) . . ? C53 N51 Lu 129.1(2) . . ? C58 N52 C52 108.8(3) . . ? C62 N61 C63 103.9(3) . . ? C62 N61 Lu 118.6(2) . . ? C63 N61 Lu 132.3(2) . . ? C62 N62 C68 106.0(3) . . ? N1 C11 C12 109.6(3) . . ? N12 C12 N11 111.6(3) . . ? N12 C12 C11 125.0(3) . . ? N11 C12 C11 123.2(3) . . ? C14 C13 N11 133.1(3) . . ? C14 C13 C18 120.7(3) . . ? N11 C13 C18 106.1(3) . . ? C13 C14 C15 119.7(3) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 122.8(4) . . ? C16 C17 C18 116.8(4) . . ? N12 C18 C17 133.1(3) . . ? N12 C18 C13 106.9(3) . . ? C17 C18 C13 120.0(3) . . ? N1 C21 C22 108.3(3) . . ? N21 C22 N22 112.2(3) . . ? N21 C22 C21 125.2(3) . . ? N22 C22 C21 122.6(3) . . ? C24 C23 C28 119.5(3) . . ? C24 C23 N21 130.9(3) . . ? C28 C23 N21 109.5(3) . . ? C25 C24 C23 117.2(3) . . ? C24 C25 C26 122.5(3) . . ? C27 C26 C25 121.6(4) . . ? C28 C27 C26 114.1(4) . . ? C27 C28 C23 124.7(3) . . ? C27 C28 N22 130.9(4) . . ? C23 C28 N22 104.3(3) . . ? C32 C31 N1 108.5(3) . . ? N31 C32 N32 114.3(3) . . ? N31 C32 C31 125.0(3) . . ? N32 C32 C31 120.7(3) . . ? C34 C33 N31 131.9(3) . . ? C34 C33 C38 119.2(3) . . ? N31 C33 C38 108.9(3) . . ? C35 C34 C33 119.5(3) . . ? C34 C35 C36 119.4(4) . . ? C37 C36 C35 124.6(4) . . ? C36 C37 C38 115.7(4) . . ? N32 C38 C37 134.4(3) . . ? N32 C38 C33 104.2(3) . . ? C37 C38 C33 121.4(3) . . ? N2 C41 C42 108.8(3) . . ? N42 C42 N41 111.5(3) . . ? N42 C42 C41 124.4(3) . . ? N41 C42 C41 124.1(3) . . ? C44 C43 N41 130.3(3) . . ? C44 C43 C48 120.4(3) . . ? N41 C43 C48 109.2(3) . . ? C43 C44 C45 117.3(3) . . ? C44 C45 C46 120.4(3) . . ? C47 C46 C45 123.5(4) . . ? C46 C47 C48 114.9(4) . . ? C47 C48 N42 131.0(3) . . ? C47 C48 C43 123.3(3) . . ? N42 C48 C43 105.5(3) . . ? C52 C51 N2 108.6(2) . . ? N51 C52 N52 110.8(3) . . ? N51 C52 C51 124.0(3) . . ? N52 C52 C51 125.0(3) . . ? C54 C53 C58 119.5(3) . . ? C54 C53 N51 132.4(3) . . ? C58 C53 N51 108.2(3) . . ? C55 C54 C53 119.2(3) . . ? C54 C55 C56 122.0(4) . . ? C57 C56 C55 119.7(4) . . ? C56 C57 C58 119.6(3) . . ? N52 C58 C53 106.2(3) . . ? N52 C58 C57 133.7(3) . . ? C53 C58 C57 120.0(3) . . ? N2 C61 C62 106.2(2) . . ? N61 C62 N62 114.8(3) . . ? N61 C62 C61 123.6(3) . . ? N62 C62 C61 121.4(3) . . ? C68 C63 C64 118.3(3) . . ? C68 C63 N61 110.8(3) . . ? C64 C63 N61 130.8(3) . . ? C65 C64 C63 119.4(3) . . ? C64 C65 C66 119.8(3) . . ? C67 C66 C65 121.8(4) . . ? C68 C67 C66 115.8(4) . . ? C63 C68 C67 124.9(3) . . ? C63 C68 N62 104.4(3) . . ? C67 C68 N62 130.6(3) . . ? O3B O3A O3C 64.6(7) . . ? O3A O3B O3C 64.0(6) . . ? O3A O3C O3B 51.5(5) . . ? _refine_diff_density_max 3.932 _refine_diff_density_min -3.348 _refine_diff_density_rms 0.233 #=END