# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex05 _database_code_depnum_ccdc_archive 'CCDC 823421' #TrackingRef 'complex-05.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 N40 O28 Sm2, C6 H6 O2, 6(N O3), 11(H2 O)' _chemical_formula_sum 'C66 H104 N46 O59 Sm2' _chemical_formula_weight 2786.65 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.273(2) _cell_length_b 21.836(3) _cell_length_c 16.089(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.622(4) _cell_angle_gamma 90.00 _cell_volume 5255.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2836 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7644 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44619 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10110 _reflns_number_gt 8600 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+11.6555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10110 _refine_ls_number_parameters 744 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 5.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.1734(12) 0.1812(8) 0.6188(11) 0.041(4) Uani 1 1 d . . . O2W O 0.4545(11) 0.2374(8) 0.6402(13) 0.045(4) Uani 1 1 d . . . O3W O 0.4479(12) 0.1141(9) 0.5753(11) 0.046(4) Uani 1 1 d . . . O4W O 0.2700(13) 0.0723(8) 0.6622(13) 0.049(5) Uani 1 1 d . . . O5W O -0.324(6) 0.038(4) 0.403(7) 0.15(3) Uani 0.50 1 d P . . O6W O 0.101(3) -0.0902(17) 0.269(2) 0.130(14) Uani 1 1 d . . . C31 C -0.4085(16) 0.1916(11) 0.3869(19) 0.055(14) Uiso 0.50 1 d PD . . C32 C -0.414(3) 0.2262(14) 0.457(2) 0.044(12) Uiso 0.50 1 d PD . . H32 H -0.4070 0.2086 0.5108 0.053 Uiso 0.50 1 calc PR . . C33 C -0.429(3) 0.2885(15) 0.444(2) 0.058(15) Uiso 0.50 1 d PD . . H33 H -0.4334 0.3144 0.4896 0.069 Uiso 0.50 1 calc PR . . C34 C -0.438(2) 0.3115(11) 0.364(2) 0.065(17) Uiso 0.50 1 d PD . . C35 C -0.433(3) 0.2768(15) 0.294(3) 0.074(19) Uiso 0.50 1 d PD . . H35 H -0.4392 0.2944 0.2399 0.089 Uiso 0.50 1 calc PR . . C36 C -0.418(3) 0.2145(16) 0.307(2) 0.052(13) Uiso 0.50 1 d PD . . H36 H -0.4136 0.1887 0.2607 0.062 Uiso 0.50 1 calc PR . . O20 O -0.392(3) 0.1234(11) 0.398(3) 0.072(13) Uiso 0.50 1 d PD . . H20A H -0.3878 0.1143 0.4492 0.108 Uiso 0.50 1 calc PR . . O21 O -0.455(3) 0.3796(11) 0.350(3) 0.098(18) Uiso 0.50 1 d PD . . H21A H -0.4524 0.3888 0.3008 0.147 Uiso 0.50 1 calc PR . . N21 N -0.1317(18) 0.5193(9) 0.3406(16) 0.049(6) Uani 1 1 d . . . N22 N 0.243(2) 0.5542(10) 0.4285(18) 0.061(8) Uani 1 1 d . . . N23 N -0.306(2) 0.0870(14) 0.5982(19) 0.065(7) Uani 1 1 d . . . O17 O -0.0523(15) 0.5287(10) 0.3704(14) 0.063(5) Uani 1 1 d . . . O18 O -0.1827(17) 0.5023(11) 0.3870(18) 0.075(7) Uani 1 1 d . . . O19 O -0.158(2) 0.5241(12) 0.2610(17) 0.098(10) Uani 1 1 d . . . O14 O 0.2892(17) 0.5090(9) 0.4219(17) 0.073(7) Uani 1 1 d . . . O15 O 0.2729(16) 0.5990(10) 0.4711(15) 0.065(6) Uani 1 1 d . . . O16 O 0.164(2) 0.5556(13) 0.386(2) 0.088(8) Uani 1 1 d . . . O11 O -0.2470(16) 0.1253(12) 0.5934(17) 0.073(7) Uani 1 1 d . . . O12 O -0.300(3) 0.0538(12) 0.660(2) 0.120(14) Uani 1 1 d . . . O13 O -0.374(2) 0.083(2) 0.544(2) 0.136(15) Uani 1 1 d . . . Sm1 Sm 0.33251(7) 0.16952(4) 0.62870(6) 0.0238(5) Uani 1 1 d . . . C1 C 0.2633(14) 0.1235(9) 0.4147(13) 0.026(4) Uani 1 1 d . . . C2 C 0.2248(15) 0.0843(10) 0.2775(13) 0.029(5) Uani 1 1 d . . . H2 H 0.2514 0.0459 0.2609 0.034 Uiso 1 1 calc R . . C3 C 0.2881(15) 0.1394(10) 0.2786(13) 0.030(5) Uani 1 1 d . . . H3 H 0.3438 0.1277 0.2601 0.036 Uiso 1 1 calc R . . C4 C 0.1527(16) 0.1595(10) 0.1841(14) 0.031(5) Uani 1 1 d . . . C5 C 0.3675(14) 0.2068(10) 0.4016(14) 0.029(4) Uani 1 1 d . . . H5A H 0.3980 0.1953 0.4590 0.034 Uiso 1 1 calc R . . H5B H 0.4128 0.2106 0.3667 0.034 Uiso 1 1 calc R . . C6 C 0.2638(16) 0.2427(10) 0.2029(14) 0.031(5) Uani 1 1 d . . . H6A H 0.2329 0.2541 0.1455 0.037 Uiso 1 1 calc R . . H6B H 0.3280 0.2420 0.2034 0.037 Uiso 1 1 calc R . . C7 C 0.2900(14) 0.2850(9) 0.4716(13) 0.025(4) Uani 1 1 d . . . C8 C 0.3103(15) 0.3087(10) 0.3357(14) 0.030(5) Uani 1 1 d . . . H8 H 0.3673 0.3217 0.3208 0.036 Uiso 1 1 calc R . . C9 C 0.2628(14) 0.3626(9) 0.3706(13) 0.026(4) Uani 1 1 d . . . H9 H 0.2980 0.4009 0.3736 0.031 Uiso 1 1 calc R . . C10 C 0.1725(15) 0.3258(9) 0.2463(13) 0.026(5) Uani 1 1 d . . . C11 C 0.2185(15) 0.3773(9) 0.5150(13) 0.028(4) Uani 1 1 d . . . H11A H 0.2352 0.4202 0.5099 0.033 Uiso 1 1 calc R . . H11B H 0.2458 0.3635 0.5724 0.033 Uiso 1 1 calc R . . C12 C 0.1138(15) 0.4156(9) 0.3100(13) 0.026(4) Uani 1 1 d . . . H12A H 0.1447 0.4533 0.3323 0.032 Uiso 1 1 calc R . . H12B H 0.0832 0.4235 0.2513 0.032 Uiso 1 1 calc R . . C13 C 0.0811(16) 0.3364(9) 0.5534(13) 0.027(5) Uani 1 1 d . . . C14 C 0.0600(14) 0.4136(9) 0.4501(12) 0.025(4) Uani 1 1 d . . . H14 H 0.0740 0.4573 0.4628 0.029 Uiso 1 1 calc R . . C15 C -0.0324(15) 0.3951(9) 0.4701(13) 0.026(4) Uani 1 1 d . . . H15 H -0.0607 0.4296 0.4947 0.031 Uiso 1 1 calc R . . C16 C -0.0356(14) 0.3813(8) 0.3255(13) 0.024(4) Uani 1 1 d . . . C17 C -0.0730(16) 0.3152(10) 0.5723(14) 0.031(5) Uani 1 1 d . . . H17A H -0.0423 0.3036 0.6297 0.037 Uiso 1 1 calc R . . H17B H -0.1205 0.3442 0.5777 0.037 Uiso 1 1 calc R . . C18 C -0.1749(14) 0.3562(9) 0.3732(14) 0.027(4) Uani 1 1 d . . . H18A H -0.2048 0.3681 0.3157 0.033 Uiso 1 1 calc R . . H18B H -0.2059 0.3764 0.4133 0.033 Uiso 1 1 calc R . . C19 C -0.0749(16) 0.2046(10) 0.5459(14) 0.031(5) Uani 1 1 d . . . C20 C -0.1906(15) 0.2597(9) 0.4603(13) 0.028(4) Uani 1 1 d . . . H20 H -0.2451 0.2731 0.4797 0.033 Uiso 1 1 calc R . . C21 C -0.1963(16) 0.1906(10) 0.4333(14) 0.031(5) Uani 1 1 d . . . H21 H -0.2525 0.1718 0.4425 0.037 Uiso 1 1 calc R . . C22 C -0.1865(13) 0.2507(9) 0.3162(13) 0.024(4) Uani 1 1 d . . . C23 C -0.1044(17) 0.0986(10) 0.4960(16) 0.036(5) Uani 1 1 d . . . H23A H -0.0753 0.0894 0.5547 0.043 Uiso 1 1 calc R . . H23B H -0.1621 0.0772 0.4842 0.043 Uiso 1 1 calc R . . C24 C -0.2007(15) 0.1390(10) 0.2897(15) 0.032(5) Uani 1 1 d . . . H24A H -0.2439 0.1105 0.3060 0.039 Uiso 1 1 calc R . . H24B H -0.2239 0.1517 0.2310 0.039 Uiso 1 1 calc R . . C25 C 0.0405(16) 0.0679(9) 0.4648(14) 0.030(5) Uani 1 1 d . . . C26 C -0.0840(16) 0.0581(9) 0.3527(15) 0.033(5) Uani 1 1 d . . . H26 H -0.1287 0.0249 0.3488 0.039 Uiso 1 1 calc R . . C27 C 0.0008(16) 0.0359(10) 0.3228(14) 0.032(5) Uani 1 1 d . . . H27 H -0.0036 -0.0080 0.3069 0.038 Uiso 1 1 calc R . . C28 C -0.0695(16) 0.1124(10) 0.2305(14) 0.031(5) Uani 1 1 d . . . C29 C 0.1642(15) 0.0336(9) 0.3994(14) 0.029(5) Uani 1 1 d . . . H29A H 0.1688 -0.0043 0.3679 0.035 Uiso 1 1 calc R . . H29B H 0.1938 0.0265 0.4586 0.035 Uiso 1 1 calc R . . C30 C 0.0652(16) 0.0657(10) 0.1933(14) 0.033(5) Uani 1 1 d . . . H30A H 0.0817 0.0223 0.1934 0.040 Uiso 1 1 calc R . . H30B H 0.0347 0.0765 0.1356 0.040 Uiso 1 1 calc R . . N1 N 0.2115(13) 0.0818(8) 0.3646(11) 0.029(4) Uani 1 1 d . . . N2 N 0.3054(13) 0.1587(8) 0.3671(12) 0.031(4) Uani 1 1 d . . . N3 N 0.1459(14) 0.1021(8) 0.2159(11) 0.032(4) Uani 1 1 d . . . N4 N 0.2361(14) 0.1823(8) 0.2210(12) 0.033(4) Uani 1 1 d . . . N5 N 0.3249(13) 0.2655(8) 0.4052(12) 0.032(4) Uani 1 1 d . . . N6 N 0.2544(13) 0.3414(8) 0.4546(11) 0.027(4) Uani 1 1 d . . . N7 N 0.2462(13) 0.2895(8) 0.2619(11) 0.031(4) Uani 1 1 d . . . N8 N 0.1793(12) 0.3674(8) 0.3104(11) 0.028(4) Uani 1 1 d . . . N9 N 0.1221(12) 0.3734(7) 0.5044(11) 0.025(4) Uani 1 1 d . . . N10 N -0.0094(13) 0.3457(8) 0.5297(11) 0.029(4) Uani 1 1 d . . . N11 N 0.0481(12) 0.4007(8) 0.3597(11) 0.026(4) Uani 1 1 d . . . N12 N -0.0841(12) 0.3769(8) 0.3882(11) 0.027(4) Uani 1 1 d . . . N13 N -0.1129(13) 0.2611(8) 0.5285(11) 0.030(4) Uani 1 1 d . . . N14 N -0.1202(14) 0.1638(8) 0.4877(13) 0.032(4) Uani 1 1 d . . . N15 N -0.1817(13) 0.2901(8) 0.3822(11) 0.028(4) Uani 1 1 d . . . N16 N -0.1934(13) 0.1923(8) 0.3441(11) 0.029(4) Uani 1 1 d . . . N17 N -0.0500(14) 0.0755(8) 0.4402(12) 0.033(4) Uani 1 1 d . . . N18 N 0.0717(13) 0.0464(8) 0.3965(11) 0.029(4) Uani 1 1 d . . . N19 N -0.1167(13) 0.1077(8) 0.2940(12) 0.033(4) Uani 1 1 d . . . N20 N 0.0038(13) 0.0744(8) 0.2505(11) 0.033(4) Uani 1 1 d . . . O1 O 0.2688(10) 0.1277(7) 0.4920(9) 0.030(3) Uani 1 1 d . . . O2 O 0.2911(10) 0.2565(7) 0.5385(9) 0.031(3) Uani 1 1 d . . . O3 O 0.1195(11) 0.3026(7) 0.6099(10) 0.036(4) Uani 1 1 d . . . O4 O -0.0136(13) 0.1920(8) 0.6044(11) 0.042(4) Uani 1 1 d . . . O5 O 0.0848(12) 0.0760(7) 0.5360(10) 0.036(4) Uani 1 1 d . . . O6 O 0.0966(12) 0.1850(8) 0.1315(10) 0.040(4) Uani 1 1 d . . . O7 O 0.1108(11) 0.3228(7) 0.1844(10) 0.030(3) Uani 1 1 d . . . O8 O -0.0647(10) 0.3704(7) 0.2497(9) 0.031(3) Uani 1 1 d . . . O9 O -0.1864(11) 0.2650(7) 0.2423(9) 0.030(3) Uani 1 1 d . . . O10 O -0.0891(11) 0.1446(8) 0.1683(10) 0.037(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.036(10) 0.044(10) 0.043(10) -0.007(8) 0.005(8) 0.002(7) O2W 0.033(9) 0.033(9) 0.066(12) 0.007(8) 0.002(8) -0.008(7) O3W 0.039(10) 0.060(11) 0.036(9) -0.009(8) 0.004(8) 0.012(8) O4W 0.048(11) 0.036(9) 0.059(12) 0.005(8) 0.001(9) -0.014(8) O5W 0.15(7) 0.12(6) 0.18(8) 0.04(6) 0.02(6) 0.02(5) O6W 0.15(3) 0.11(2) 0.12(3) -0.05(2) 0.00(2) 0.05(2) N21 0.064(16) 0.024(10) 0.054(14) -0.008(10) 0.003(13) 0.010(10) N22 0.10(2) 0.033(12) 0.063(16) -0.001(11) 0.051(17) -0.002(13) N23 0.065(19) 0.072(19) 0.065(18) -0.012(15) 0.027(16) 0.020(15) O17 0.058(14) 0.062(13) 0.064(14) -0.011(11) 0.003(11) 0.000(11) O18 0.074(16) 0.053(13) 0.11(2) -0.025(13) 0.034(15) -0.007(12) O19 0.13(3) 0.066(16) 0.071(18) 0.008(13) -0.034(17) -0.004(16) O14 0.091(17) 0.034(11) 0.104(19) 0.000(11) 0.041(15) 0.006(11) O15 0.078(15) 0.048(12) 0.078(15) -0.026(11) 0.036(13) -0.010(11) O16 0.09(2) 0.063(16) 0.11(2) -0.026(15) 0.003(17) 0.001(13) O11 0.059(14) 0.084(17) 0.088(18) -0.004(14) 0.040(13) -0.005(13) O12 0.18(3) 0.061(16) 0.16(3) 0.044(18) 0.13(3) 0.055(19) O13 0.10(3) 0.18(4) 0.12(3) -0.07(3) -0.01(2) 0.01(2) Sm1 0.0274(7) 0.0236(7) 0.0180(7) 0.0001(4) -0.0012(5) -0.0010(4) C1 0.030(11) 0.025(10) 0.022(10) -0.001(8) 0.001(8) 0.003(8) C2 0.039(12) 0.027(10) 0.020(10) -0.005(8) 0.007(9) 0.006(9) C3 0.036(12) 0.029(11) 0.025(11) 0.000(9) 0.008(9) 0.010(9) C4 0.040(13) 0.030(11) 0.023(11) -0.004(9) 0.008(10) 0.007(10) C5 0.025(11) 0.034(11) 0.027(11) 0.000(9) 0.003(9) 0.001(9) C6 0.039(13) 0.035(12) 0.023(10) 0.000(9) 0.014(9) 0.004(10) C7 0.025(10) 0.023(10) 0.026(10) 0.000(8) -0.001(8) -0.004(8) C8 0.031(12) 0.030(11) 0.030(11) 0.003(9) 0.008(9) -0.004(9) C9 0.029(11) 0.021(10) 0.026(10) 0.004(8) 0.006(9) -0.005(8) C10 0.034(12) 0.025(10) 0.023(11) 0.006(8) 0.010(10) -0.003(8) C11 0.035(12) 0.024(10) 0.021(10) -0.002(8) -0.001(9) -0.002(9) C12 0.035(12) 0.021(10) 0.023(10) 0.003(8) 0.005(9) -0.003(8) C13 0.039(12) 0.019(9) 0.021(10) -0.005(8) 0.003(9) 0.002(8) C14 0.035(11) 0.019(9) 0.019(10) -0.004(7) 0.003(8) -0.002(8) C15 0.035(12) 0.020(9) 0.023(10) -0.004(8) 0.004(9) 0.001(8) C16 0.032(11) 0.017(9) 0.022(10) -0.002(7) 0.005(9) 0.000(8) C17 0.041(13) 0.031(11) 0.023(11) 0.000(9) 0.011(10) 0.002(10) C18 0.032(11) 0.022(10) 0.028(11) 0.000(8) 0.009(9) 0.004(8) C19 0.044(13) 0.025(10) 0.028(11) 0.006(9) 0.015(10) 0.001(9) C20 0.034(12) 0.025(10) 0.027(11) 0.000(8) 0.013(9) -0.002(9) C21 0.036(12) 0.024(10) 0.033(12) 0.002(9) 0.012(10) -0.004(9) C22 0.022(10) 0.022(9) 0.029(11) 0.000(8) 0.003(8) -0.001(8) C23 0.045(14) 0.028(11) 0.037(13) 0.007(9) 0.015(11) -0.002(10) C24 0.032(12) 0.029(11) 0.033(12) -0.003(9) 0.003(10) -0.002(9) C25 0.047(14) 0.015(9) 0.029(12) 0.002(8) 0.008(10) -0.006(9) C26 0.041(13) 0.018(9) 0.039(13) -0.001(9) 0.009(10) -0.005(9) C27 0.043(13) 0.020(10) 0.030(11) -0.004(8) 0.002(10) -0.001(9) C28 0.036(12) 0.025(10) 0.030(12) -0.007(9) 0.001(10) -0.002(9) C29 0.041(13) 0.018(9) 0.027(11) 0.002(8) 0.001(9) 0.002(9) C30 0.041(13) 0.032(11) 0.024(11) -0.009(9) 0.000(10) 0.000(10) N1 0.040(11) 0.025(9) 0.021(9) 0.000(7) 0.005(8) 0.001(8) N2 0.037(11) 0.030(9) 0.026(10) -0.003(7) 0.007(8) -0.004(8) N3 0.044(11) 0.028(9) 0.022(9) -0.003(7) 0.000(8) 0.002(8) N4 0.039(11) 0.029(9) 0.028(10) 0.001(8) 0.002(8) 0.005(8) N5 0.038(11) 0.029(9) 0.028(9) 0.005(8) 0.007(8) 0.004(8) N6 0.033(10) 0.023(8) 0.024(9) 0.003(7) 0.002(8) 0.001(7) N7 0.036(10) 0.030(9) 0.025(9) -0.002(7) 0.006(8) 0.003(8) N8 0.034(10) 0.027(9) 0.022(9) 0.000(7) 0.004(8) 0.001(7) N9 0.032(10) 0.021(8) 0.022(8) 0.003(7) 0.002(7) 0.002(7) N10 0.038(11) 0.024(8) 0.027(9) 0.004(7) 0.010(8) 0.001(8) N11 0.032(10) 0.027(9) 0.019(8) -0.001(7) 0.004(7) -0.005(7) N12 0.031(10) 0.025(9) 0.023(9) -0.002(7) 0.005(7) 0.001(7) N13 0.041(11) 0.025(9) 0.026(9) 0.003(7) 0.009(8) 0.001(8) N14 0.042(11) 0.022(9) 0.031(10) 0.005(7) 0.008(9) 0.001(8) N15 0.037(10) 0.023(9) 0.024(9) 0.001(7) 0.008(8) -0.001(7) N16 0.036(10) 0.022(8) 0.029(9) -0.001(7) 0.007(8) -0.003(7) N17 0.044(12) 0.025(9) 0.031(10) 0.000(7) 0.011(9) -0.002(8) N18 0.037(10) 0.023(9) 0.027(9) -0.003(7) 0.005(8) -0.001(7) N19 0.038(11) 0.024(9) 0.034(10) 0.000(8) 0.005(9) 0.001(8) N20 0.043(11) 0.030(9) 0.026(9) 0.000(7) 0.003(8) 0.006(8) O1 0.034(8) 0.031(8) 0.023(8) -0.003(6) 0.002(6) -0.003(6) O2 0.040(9) 0.028(8) 0.021(7) 0.002(6) -0.001(6) 0.003(7) O3 0.047(10) 0.038(9) 0.024(8) 0.008(7) 0.009(7) 0.009(7) O4 0.056(11) 0.035(9) 0.034(9) 0.008(7) 0.003(8) 0.006(8) O5 0.050(10) 0.032(8) 0.025(8) 0.000(6) 0.006(7) -0.002(7) O6 0.048(10) 0.036(8) 0.031(9) 0.001(7) -0.002(8) 0.008(8) O7 0.034(9) 0.030(8) 0.025(8) 0.001(6) 0.004(7) 0.000(6) O8 0.036(9) 0.033(8) 0.022(8) -0.003(6) 0.004(6) -0.003(6) O9 0.041(9) 0.026(7) 0.022(8) 0.001(6) 0.000(6) -0.001(6) O10 0.044(10) 0.035(9) 0.030(9) 0.004(7) 0.001(7) 0.006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Sm1 2.416(18) . ? O2W Sm1 2.360(16) . ? O3W Sm1 2.433(17) . ? O4W Sm1 2.433(17) . ? C31 C36 1.367(9) . ? C31 C32 1.368(9) . ? C31 O20 1.516(5) . ? C32 C33 1.390(10) . ? C32 H32 0.9400 . ? C33 C34 1.367(9) . ? C33 H33 0.9400 . ? C34 C35 1.367(9) . ? C34 O21 1.517(5) . ? C35 C36 1.387(10) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? O20 H20A 0.8300 . ? O21 H21A 0.8300 . ? N21 O17 1.23(3) . ? N21 O18 1.24(3) . ? N21 O19 1.27(3) . ? N22 O14 1.23(3) . ? N22 O15 1.23(3) . ? N22 O16 1.26(4) . ? N23 O13 1.22(4) . ? N23 O12 1.22(4) . ? N23 O11 1.24(4) . ? Sm1 O9 2.384(14) 4_666 ? Sm1 O2 2.395(14) . ? Sm1 O1 2.400(14) . ? Sm1 O8 2.405(15) 4_666 ? C1 O1 1.23(3) . ? C1 N2 1.34(3) . ? C1 N1 1.36(3) . ? C2 N3 1.45(3) . ? C2 N1 1.46(3) . ? C2 C3 1.54(3) . ? C2 H2 0.9900 . ? C3 N4 1.44(3) . ? C3 N2 1.46(3) . ? C3 H3 0.9900 . ? C4 O6 1.21(3) . ? C4 N3 1.37(3) . ? C4 N4 1.39(3) . ? C5 N5 1.44(3) . ? C5 N2 1.45(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.43(3) . ? C6 N7 1.46(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.24(2) . ? C7 N6 1.35(3) . ? C7 N5 1.36(3) . ? C8 N7 1.44(3) . ? C8 N5 1.45(3) . ? C8 C9 1.55(3) . ? C8 H8 0.9900 . ? C9 N8 1.44(3) . ? C9 N6 1.46(3) . ? C9 H9 0.9900 . ? C10 O7 1.23(3) . ? C10 N7 1.36(3) . ? C10 N8 1.36(3) . ? C11 N6 1.44(3) . ? C11 N9 1.45(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.44(3) . ? C12 N8 1.45(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.23(3) . ? C13 N9 1.36(3) . ? C13 N10 1.37(3) . ? C14 N9 1.45(3) . ? C14 N11 1.46(2) . ? C14 C15 1.56(3) . ? C14 H14 0.9900 . ? C15 N10 1.44(3) . ? C15 N12 1.45(3) . ? C15 H15 0.9900 . ? C16 O8 1.23(2) . ? C16 N11 1.36(3) . ? C16 N12 1.37(3) . ? C17 N13 1.44(3) . ? C17 N10 1.46(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.43(3) . ? C18 N15 1.46(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.22(3) . ? C19 N13 1.37(3) . ? C19 N14 1.37(3) . ? C20 N13 1.45(3) . ? C20 N15 1.45(3) . ? C20 C21 1.57(3) . ? C20 H20 0.9900 . ? C21 N14 1.43(3) . ? C21 N16 1.45(3) . ? C21 H21 0.9900 . ? C22 O9 1.23(2) . ? C22 N15 1.36(3) . ? C22 N16 1.36(3) . ? C23 N17 1.43(3) . ? C23 N14 1.45(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.44(3) . ? C24 N16 1.45(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.22(3) . ? C25 N18 1.37(3) . ? C25 N17 1.37(3) . ? C26 N17 1.45(3) . ? C26 N19 1.46(3) . ? C26 C27 1.55(3) . ? C26 H26 0.9900 . ? C27 N20 1.44(3) . ? C27 N18 1.45(3) . ? C27 H27 0.9900 . ? C28 O10 1.21(3) . ? C28 N19 1.37(3) . ? C28 N20 1.38(3) . ? C29 N18 1.43(3) . ? C29 N1 1.45(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N3 1.45(3) . ? C30 N20 1.45(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O8 Sm1 2.405(15) 4_565 ? O9 Sm1 2.384(14) 4_565 ? 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 C36 C31 C32 124.1(10) . . ? C36 C31 O20 117.3(12) . . ? C32 C31 O20 118.6(12) . . ? C31 C32 C33 117(3) . . ? C31 C32 H32 121.4 . . ? C33 C32 H32 121.4 . . ? C34 C33 C32 119(3) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C35 C34 C33 123.9(10) . . ? C35 C34 O21 117.8(12) . . ? C33 C34 O21 118.3(12) . . ? C34 C35 C36 117(3) . . ? C34 C35 H35 121.3 . . ? C36 C35 H35 121.3 . . ? C31 C36 C35 119(3) . . ? C31 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? C31 O20 H20A 109.5 . . ? C34 O21 H21A 109.5 . . ? O17 N21 O18 120(3) . . ? O17 N21 O19 118(3) . . ? O18 N21 O19 121(3) . . ? O14 N22 O15 122(3) . . ? O14 N22 O16 118(3) . . ? O15 N22 O16 119(3) . . ? O13 N23 O12 117(4) . . ? O13 N23 O11 122(4) . . ? O12 N23 O11 121(4) . . ? O2W Sm1 O9 77.2(6) . 4_666 ? O2W Sm1 O2 70.0(6) . . ? O9 Sm1 O2 86.0(5) 4_666 . ? O2W Sm1 O1 118.6(6) . . ? O9 Sm1 O1 147.3(5) 4_666 . ? O2 Sm1 O1 74.8(5) . . ? O2W Sm1 O8 77.7(6) . 4_666 ? O9 Sm1 O8 76.0(5) 4_666 4_666 ? O2 Sm1 O8 145.8(5) . 4_666 ? O1 Sm1 O8 133.0(5) . 4_666 ? O2W Sm1 O1W 135.0(6) . . ? O9 Sm1 O1W 73.2(6) 4_666 . ? O2 Sm1 O1W 74.8(6) . . ? O1 Sm1 O1W 76.3(6) . . ? O8 Sm1 O1W 125.1(6) 4_666 . ? O2W Sm1 O4W 150.5(6) . . ? O9 Sm1 O4W 103.9(6) 4_666 . ? O2 Sm1 O4W 139.3(6) . . ? O1 Sm1 O4W 76.5(6) . . ? O8 Sm1 O4W 74.1(6) 4_666 . ? O1W Sm1 O4W 70.9(6) . . ? O2W Sm1 O3W 74.0(7) . . ? O9 Sm1 O3W 141.1(6) 4_666 . ? O2 Sm1 O3W 107.6(6) . . ? O1 Sm1 O3W 71.1(6) . . ? O8 Sm1 O3W 72.8(6) 4_666 . ? O1W Sm1 O3W 145.0(6) . . ? O4W Sm1 O3W 89.3(7) . . ? O1 C1 N2 126(2) . . ? O1 C1 N1 124(2) . . ? N2 C1 N1 109.5(18) . . ? N3 C2 N1 114.2(18) . . ? N3 C2 C3 103.4(17) . . ? N1 C2 C3 103.0(16) . . ? N3 C2 H2 111.9 . . ? N1 C2 H2 111.9 . . ? C3 C2 H2 111.9 . . ? N4 C3 N2 114.2(17) . . ? N4 C3 C2 103.7(18) . . ? N2 C3 C2 103.1(17) . . ? N4 C3 H3 111.7 . . ? N2 C3 H3 111.7 . . ? C2 C3 H3 111.7 . . ? O6 C4 N3 126(2) . . ? O6 C4 N4 126(2) . . ? N3 C4 N4 107.6(19) . . ? N5 C5 N2 113.3(18) . . ? N5 C5 H5A 108.9 . . ? N2 C5 H5A 108.9 . . ? N5 C5 H5B 108.9 . . ? N2 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 114.3(17) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N6 124.6(19) . . ? O2 C7 N5 125.9(19) . . ? N6 C7 N5 109.4(18) . . ? N7 C8 N5 114.9(18) . . ? N7 C8 C9 103.3(17) . . ? N5 C8 C9 103.1(17) . . ? N7 C8 H8 111.6 . . ? N5 C8 H8 111.6 . . ? C9 C8 H8 111.6 . . ? N8 C9 N6 114.5(17) . . ? N8 C9 C8 103.2(16) . . ? N6 C9 C8 103.2(16) . . ? N8 C9 H9 111.8 . . ? N6 C9 H9 111.8 . . ? C8 C9 H9 111.8 . . ? O7 C10 N7 126(2) . . ? O7 C10 N8 125(2) . . ? N7 C10 N8 108.3(19) . . ? N6 C11 N9 113.9(17) . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? N9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N11 C12 N8 112.9(16) . . ? N11 C12 H12A 109.0 . . ? N8 C12 H12A 109.0 . . ? N11 C12 H12B 109.0 . . ? N8 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N9 125(2) . . ? O3 C13 N10 127(2) . . ? N9 C13 N10 107.8(18) . . ? N9 C14 N11 114.9(16) . . ? N9 C14 C15 103.1(16) . . ? N11 C14 C15 102.7(16) . . ? N9 C14 H14 111.8 . . ? N11 C14 H14 111.8 . . ? C15 C14 H14 111.8 . . ? N10 C15 N12 114.5(17) . . ? N10 C15 C14 102.8(17) . . ? N12 C15 C14 103.5(16) . . ? N10 C15 H15 111.8 . . ? N12 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? O8 C16 N11 125.7(19) . . ? O8 C16 N12 125.1(19) . . ? N11 C16 N12 109.2(17) . . ? N13 C17 N10 113.6(17) . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17B 108.9 . . ? N10 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N12 C18 N15 112.5(17) . . ? N12 C18 H18A 109.1 . . ? N15 C18 H18A 109.1 . . ? N12 C18 H18B 109.1 . . ? N15 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N13 126(2) . . ? O4 C19 N14 126(2) . . ? N13 C19 N14 108(2) . . ? N13 C20 N15 116.2(18) . . ? N13 C20 C21 102.9(17) . . ? N15 C20 C21 102.1(16) . . ? N13 C20 H20 111.6 . . ? N15 C20 H20 111.6 . . ? C21 C20 H20 111.6 . . ? N14 C21 N16 115.8(19) . . ? N14 C21 C20 103.4(18) . . ? N16 C21 C20 103.8(16) . . ? N14 C21 H21 111.1 . . ? N16 C21 H21 111.1 . . ? C20 C21 H21 111.1 . . ? O9 C22 N15 125.9(18) . . ? O9 C22 N16 124.8(19) . . ? N15 C22 N16 109.3(18) . . ? N17 C23 N14 113.3(18) . . ? N17 C23 H23A 108.9 . . ? N14 C23 H23A 108.9 . . ? N17 C23 H23B 108.9 . . ? N14 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N16 113.1(18) . . ? N19 C24 H24A 109.0 . . ? N16 C24 H24A 109.0 . . ? N19 C24 H24B 109.0 . . ? N16 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O5 C25 N18 126(2) . . ? O5 C25 N17 126(2) . . ? N18 C25 N17 107.7(19) . . ? N17 C26 N19 116.3(17) . . ? N17 C26 C27 103.0(19) . . ? N19 C26 C27 103.4(18) . . ? N17 C26 H26 111.2 . . ? N19 C26 H26 111.2 . . ? C27 C26 H26 111.2 . . ? N20 C27 N18 115.2(18) . . ? N20 C27 C26 103.4(18) . . ? N18 C27 C26 103.3(17) . . ? N20 C27 H27 111.5 . . ? N18 C27 H27 111.5 . . ? C26 C27 H27 111.5 . . ? O10 C28 N19 126(2) . . ? O10 C28 N20 127(2) . . ? N19 C28 N20 107.7(19) . . ? N18 C29 N1 114.2(17) . . ? N18 C29 H29A 108.7 . . ? N1 C29 H29A 108.7 . . ? N18 C29 H29B 108.7 . . ? N1 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N3 C30 N20 113.2(17) . . ? N3 C30 H30A 108.9 . . ? N20 C30 H30A 108.9 . . ? N3 C30 H30B 108.9 . . ? N20 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C1 N1 C29 122.2(17) . . ? C1 N1 C2 111.7(18) . . ? C29 N1 C2 125.0(18) . . ? C1 N2 C5 123.3(18) . . ? C1 N2 C3 112.3(18) . . ? C5 N2 C3 124.1(18) . . ? C4 N3 C30 122.2(19) . . ? C4 N3 C2 112.8(19) . . ? C30 N3 C2 124.9(18) . . ? C4 N4 C6 121.8(19) . . ? C4 N4 C3 112.5(18) . . ? C6 N4 C3 126(2) . . ? C7 N5 C5 124.3(18) . . ? C7 N5 C8 112.4(17) . . ? C5 N5 C8 123.3(18) . . ? C7 N6 C11 123.4(18) . . ? C7 N6 C9 111.8(17) . . ? C11 N6 C9 124.6(17) . . ? C10 N7 C8 112.5(18) . . ? C10 N7 C6 122.9(19) . . ? C8 N7 C6 124.0(19) . . ? C10 N8 C9 112.5(18) . . ? C10 N8 C12 122.2(18) . . ? C9 N8 C12 124.8(17) . . ? C13 N9 C14 112.8(17) . . ? C13 N9 C11 122.7(18) . . ? C14 N9 C11 124.1(17) . . ? C13 N10 C15 113.1(18) . . ? C13 N10 C17 122.1(18) . . ? C15 N10 C17 124.0(19) . . ? C16 N11 C12 123.4(17) . . ? C16 N11 C14 112.6(16) . . ? C12 N11 C14 123.4(17) . . ? C16 N12 C18 123.2(17) . . ? C16 N12 C15 112.0(17) . . ? C18 N12 C15 124.9(17) . . ? C19 N13 C17 121.1(19) . . ? C19 N13 C20 112.7(18) . . ? C17 N13 C20 126.1(18) . . ? C19 N14 C21 112.8(17) . . ? C19 N14 C23 122(2) . . ? C21 N14 C23 124(2) . . ? C22 N15 C20 112.8(17) . . ? C22 N15 C18 122.9(17) . . ? C20 N15 C18 124.1(16) . . ? C22 N16 C21 111.8(17) . . ? C22 N16 C24 123.8(18) . . ? C21 N16 C24 124.4(18) . . ? C25 N17 C23 123(2) . . ? C25 N17 C26 113.1(18) . . ? C23 N17 C26 124(2) . . ? C25 N18 C29 122.8(19) . . ? C25 N18 C27 112.8(19) . . ? C29 N18 C27 124.3(18) . . ? C28 N19 C24 121.7(19) . . ? C28 N19 C26 112.2(18) . . ? C24 N19 C26 124.7(19) . . ? C28 N20 C27 112.5(19) . . ? C28 N20 C30 121.9(19) . . ? C27 N20 C30 124.3(18) . . ? C1 O1 Sm1 152.3(14) . . ? C7 O2 Sm1 151.5(14) . . ? C16 O8 Sm1 156.3(14) . 4_565 ? C22 O9 Sm1 156.5(14) . 4_565 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.806 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.128 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 104 38 ' ' 2 0.027 0.532 0.139 45 17 ' ' 3 0.061 0.224 0.377 46 5 ' ' 4 -0.062 0.776 0.623 46 5 ' ' 5 -0.028 0.467 0.856 42 17 ' ' 6 0.500 0.500 0.500 104 38 ' ' 7 0.438 0.724 0.123 46 5 ' ' 8 0.473 0.032 0.361 44 17 ' ' 9 0.528 0.967 0.644 43 17 ' ' 10 0.561 0.276 0.877 46 5 ' ' _platon_squeeze_details ; ; data_02 _database_code_depnum_ccdc_archive 'CCDC 875765' #TrackingRef 'sbumit-06.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H64 Cl Er N22 O32' _chemical_formula_weight 1519.80 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' Er Er -0.2586 4.9576 '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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 61' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, x, z+1/6' 'y, -x+y, z+5/6' _cell_length_a 14.465(5) _cell_length_b 14.465(3) _cell_length_c 45.866(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8311(4) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4650 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6067 _exptl_absorpt_correction_T_max 0.7085 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56552 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10108 _reflns_number_gt 9756 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+24.9898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.045(8) _chemical_absolute_configuration ' R ' _refine_ls_number_reflns 10108 _refine_ls_number_parameters 743 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.4845(3) 0.3347(3) 0.56214(12) 0.0307(9) Uani 1 1 d . . . O2W O 0.4633(3) 0.0230(3) 0.56386(11) 0.0291(9) Uani 1 1 d . . . O3W O 0.6728(4) 0.1705(4) 0.57256(10) 0.0301(10) Uani 1 1 d . . . O4W O 0.6771(3) 0.3683(3) 0.54501(9) 0.0269(9) Uani 1 1 d . . . Er1 Er 0.535555(18) 0.206894(18) 0.561789(18) 0.01742(7) Uani 1 1 d . . . N21 N -0.0576(8) 0.1563(10) 0.5709(2) 0.082(2) Uani 1 1 d . . . O11 O 0.0204(6) 0.2426(7) 0.5686(3) 0.116(4) Uani 1 1 d . . . O12 O -0.1219(7) 0.1082(7) 0.55150(19) 0.099(3) Uani 1 1 d . . . O13 O -0.0750(9) 0.1176(10) 0.5959(3) 0.139(5) Uani 1 1 d . . . N22 N -0.1441(7) 0.2754(9) 0.62604(19) 0.082(2) Uani 1 1 d D . . O14 O -0.1442(8) 0.3090(8) 0.6009(2) 0.148(6) Uani 1 1 d D . . O15 O -0.0689(7) 0.3413(10) 0.6416(4) 0.331(17) Uani 1 1 d D . . O16 O -0.2136(8) 0.1839(10) 0.6342(4) 0.174(6) Uani 1 1 d D . . Cl1 Cl 0.8295(5) 0.3961(5) 0.50867(18) 0.095(2) Uani 0.50 1 d P . . Cl2 Cl 0.9602(7) 0.9459(6) 0.65065(17) 0.118(3) Uani 0.50 1 d P . . C31 C 0.9455(8) 0.7316(6) 0.5711(2) 0.092(5) Uani 1 1 d D . . C32 C 0.9705(7) 0.8267(6) 0.5845(2) 0.064(3) Uani 1 1 d D . . H32 H 1.0158 0.8511 0.6008 0.077 Uiso 1 1 calc R . . C33 C 0.9271(6) 0.8849(6) 0.57315(16) 0.053(2) Uani 1 1 d D . . H33 H 0.9438 0.9501 0.5820 0.063 Uiso 1 1 calc R . . C34 C 0.8599(5) 0.8506(6) 0.54930(16) 0.054(2) Uani 1 1 d D . . C35 C 0.8336(6) 0.7540(6) 0.5367(2) 0.077(4) Uani 1 1 d D . . H35 H 0.7869 0.7288 0.5206 0.092 Uiso 1 1 calc R . . C36 C 0.8762(8) 0.6947(7) 0.5477(2) 0.102(6) Uani 1 1 d D . . H36 H 0.8580 0.6285 0.5392 0.122 Uiso 1 1 calc R . . O17 O 0.9895(8) 0.6717(7) 0.5832(3) 0.146(6) Uani 1 1 d . . . H17 H 0.9646 0.6135 0.5746 0.220 Uiso 1 1 calc R . . O18 O 0.8145(5) 0.9045(6) 0.53677(16) 0.0695(19) Uani 1 1 d . . . H18 H 0.8347 0.9617 0.5455 0.104 Uiso 1 1 calc R . . C1 C 0.6516(4) 0.3108(4) 0.62870(11) 0.0146(10) Uani 1 1 d . . . C2 C 0.7528(5) 0.3871(5) 0.67099(13) 0.0232(12) Uani 1 1 d . . . H2 H 0.8262 0.3999 0.6737 0.028 Uiso 1 1 calc R . . C3 C 0.6674(4) 0.2686(5) 0.67646(12) 0.0202(11) Uani 1 1 d . . . H3 H 0.7005 0.2261 0.6826 0.024 Uiso 1 1 calc R . . C4 C 0.6407(4) 0.3818(4) 0.70784(12) 0.0207(11) Uani 1 1 d . . . C5 C 0.5312(5) 0.1234(4) 0.64185(13) 0.0217(12) Uani 1 1 d . . . H5A H 0.5417 0.1070 0.6218 0.026 Uiso 1 1 calc R . . H5B H 0.5385 0.0737 0.6549 0.026 Uiso 1 1 calc R . . C6 C 0.5069(6) 0.1889(5) 0.71126(14) 0.0248(13) Uani 1 1 d . . . H6A H 0.5155 0.1260 0.7123 0.030 Uiso 1 1 calc R . . H6B H 0.4959 0.2062 0.7312 0.030 Uiso 1 1 calc R . . C7 C 0.3731(5) 0.1227(4) 0.62286(12) 0.0199(11) Uani 1 1 d . . . C8 C 0.3686(5) 0.0790(5) 0.67192(14) 0.0253(13) Uani 1 1 d . . . H8 H 0.3573 0.0099 0.6794 0.030 Uiso 1 1 calc R . . C9 C 0.2610(4) 0.0736(4) 0.66367(12) 0.0186(11) Uani 1 1 d . . . H9 H 0.2002 -0.0001 0.6655 0.022 Uiso 1 1 calc R . . C10 C 0.3404(4) 0.1930(4) 0.70264(12) 0.0209(11) Uani 1 1 d . . . C11 C 0.1952(5) 0.1020(4) 0.61498(13) 0.0241(12) Uani 1 1 d . . . H11A H 0.1268 0.0412 0.6211 0.029 Uiso 1 1 calc R . . H11B H 0.2088 0.0886 0.5949 0.029 Uiso 1 1 calc R . . C12 C 0.1669(5) 0.1663(5) 0.68640(14) 0.0256(12) Uani 1 1 d . . . H12A H 0.1639 0.1902 0.7062 0.031 Uiso 1 1 calc R . . H12B H 0.0993 0.1005 0.6827 0.031 Uiso 1 1 calc R . . C13 C 0.2325(4) 0.2757(5) 0.59464(12) 0.0203(12) Uani 1 1 d . . . C14 C 0.1293(4) 0.2228(5) 0.63709(12) 0.0208(11) Uani 1 1 d . . . H14 H 0.0528 0.1676 0.6380 0.025 Uiso 1 1 calc R . . C15 C 0.1454(4) 0.3302(4) 0.62629(13) 0.0198(11) Uani 1 1 d . . . H15 H 0.0773 0.3245 0.6200 0.024 Uiso 1 1 calc R . . C16 C 0.2064(4) 0.3476(4) 0.67456(12) 0.0184(11) Uani 1 1 d . . . C17 C 0.2451(4) 0.4472(5) 0.58250(12) 0.0199(11) Uani 1 1 d . . . H17A H 0.2501 0.4256 0.5626 0.024 Uiso 1 1 calc R . . H17B H 0.1864 0.4626 0.5830 0.024 Uiso 1 1 calc R . . C18 C 0.2197(4) 0.5100(4) 0.65172(12) 0.0165(11) Uani 1 1 d . . . H18A H 0.1695 0.5192 0.6394 0.020 Uiso 1 1 calc R . . H18B H 0.2143 0.5323 0.6715 0.020 Uiso 1 1 calc R . . C19 C 0.4399(4) 0.5646(4) 0.57829(11) 0.0167(11) Uani 1 1 d . . . C20 C 0.3536(4) 0.6206(4) 0.61171(13) 0.0201(11) Uani 1 1 d . . . H20 H 0.3160 0.6592 0.6060 0.024 Uiso 1 1 calc R . . C21 C 0.4770(4) 0.6966(4) 0.61383(12) 0.0181(11) Uani 1 1 d . . . H21 H 0.4980 0.7720 0.6101 0.022 Uiso 1 1 calc R . . C22 C 0.4121(4) 0.6128(4) 0.65821(12) 0.0193(11) Uani 1 1 d . . . C23 C 0.6300(4) 0.6915(5) 0.58719(13) 0.0221(12) Uani 1 1 d . . . H23A H 0.6394 0.6700 0.5676 0.027 Uiso 1 1 calc R . . H23B H 0.6692 0.7697 0.5879 0.027 Uiso 1 1 calc R . . C24 C 0.6022(4) 0.7505(4) 0.65746(12) 0.0181(11) Uani 1 1 d . . . H24A H 0.5870 0.7633 0.6774 0.022 Uiso 1 1 calc R . . H24B H 0.6370 0.8193 0.6473 0.022 Uiso 1 1 calc R . . C25 C 0.7003(4) 0.5756(4) 0.60111(12) 0.0159(10) Uani 1 1 d . . . C26 C 0.7372(4) 0.7132(4) 0.63307(12) 0.0164(10) Uani 1 1 d . . . H26 H 0.7903 0.7874 0.6277 0.020 Uiso 1 1 calc R . . C27 C 0.7919(4) 0.6510(4) 0.64435(13) 0.0199(11) Uani 1 1 d . . . H27 H 0.8700 0.6984 0.6465 0.024 Uiso 1 1 calc R . . C28 C 0.6784(4) 0.6483(4) 0.68011(13) 0.0196(12) Uani 1 1 d . . . C29 C 0.7993(4) 0.4937(4) 0.62219(12) 0.0186(11) Uani 1 1 d . . . H29A H 0.8726 0.5265 0.6295 0.022 Uiso 1 1 calc R . . H29B H 0.7990 0.4695 0.6022 0.022 Uiso 1 1 calc R . . C30 C 0.7800(4) 0.5603(5) 0.69295(12) 0.0207(12) Uani 1 1 d . . . H30A H 0.8565 0.5890 0.6897 0.025 Uiso 1 1 calc R . . H30B H 0.7714 0.5817 0.7126 0.025 Uiso 1 1 calc R . . N1 N 0.7312(4) 0.4020(4) 0.64012(10) 0.0192(9) Uani 1 1 d . . . N2 N 0.6133(4) 0.2323(4) 0.64894(11) 0.0214(10) Uani 1 1 d . . . N3 N 0.7273(4) 0.4457(4) 0.69183(10) 0.0215(10) Uani 1 1 d . . . N4 N 0.6042(4) 0.2774(4) 0.69988(11) 0.0239(10) Uani 1 1 d . . . N5 N 0.4261(4) 0.1082(4) 0.64467(11) 0.0217(10) Uani 1 1 d . . . N6 N 0.2781(4) 0.1080(4) 0.63350(11) 0.0200(10) Uani 1 1 d . . . N7 N 0.4130(4) 0.1626(4) 0.69417(11) 0.0252(11) Uani 1 1 d . . . N8 N 0.2534(4) 0.1433(4) 0.68472(12) 0.0250(11) Uani 1 1 d . . . N9 N 0.1862(4) 0.1978(4) 0.61533(12) 0.0241(10) Uani 1 1 d . . . N10 N 0.2201(4) 0.3587(4) 0.60220(11) 0.0218(10) Uani 1 1 d . . . N11 N 0.1785(4) 0.2474(4) 0.66577(11) 0.0203(10) Uani 1 1 d . . . N12 N 0.1888(4) 0.3979(4) 0.65215(10) 0.0180(9) Uani 1 1 d . . . N13 N 0.3437(4) 0.5438(4) 0.58961(14) 0.0244(12) Uani 1 1 d . . . N14 N 0.5181(4) 0.6543(4) 0.59171(10) 0.0160(9) Uani 1 1 d . . . N15 N 0.3267(3) 0.5782(4) 0.64103(11) 0.0192(10) Uani 1 1 d . . . N16 N 0.5028(3) 0.6806(3) 0.64307(10) 0.0179(9) Uani 1 1 d . . . N17 N 0.6765(3) 0.6523(3) 0.60808(10) 0.0179(9) Uani 1 1 d . . . N18 N 0.7671(4) 0.5734(4) 0.62162(11) 0.0198(9) Uani 1 1 d . . . N19 N 0.6754(3) 0.7098(3) 0.65861(10) 0.0155(9) Uani 1 1 d . . . N20 N 0.7416(4) 0.6085(4) 0.67197(10) 0.0190(9) Uani 1 1 d . . . O1 O 0.6212(3) 0.3014(3) 0.60291(9) 0.0228(8) Uani 1 1 d . . . O2 O 0.4011(3) 0.1438(3) 0.59739(9) 0.0231(9) Uani 1 1 d . . . O3 O 0.2776(3) 0.2700(3) 0.57253(9) 0.0240(9) Uani 1 1 d . . . O4 O 0.4524(3) 0.5136(3) 0.55925(10) 0.0253(8) Uani 1 1 d . . . O5 O 0.6672(3) 0.5190(3) 0.57926(8) 0.0207(8) Uani 1 1 d . . . O6 O 0.6039(3) 0.4101(3) 0.72776(10) 0.0256(8) Uani 1 1 d . . . O7 O 0.3500(3) 0.2492(3) 0.72315(9) 0.0263(9) Uani 1 1 d . . . O8 O 0.2412(3) 0.3846(3) 0.69886(9) 0.0209(8) Uani 1 1 d . . . O9 O 0.4136(3) 0.5894(3) 0.68427(9) 0.0213(8) Uani 1 1 d . . . O10 O 0.6338(3) 0.6327(3) 0.70440(9) 0.0247(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.025(2) 0.0230(19) 0.043(3) -0.007(2) -0.003(2) 0.0111(16) O2W 0.029(2) 0.0224(19) 0.037(3) -0.0028(19) -0.001(2) 0.0135(17) O3W 0.036(2) 0.035(2) 0.029(2) -0.0132(18) -0.0086(18) 0.024(2) O4W 0.028(2) 0.026(2) 0.022(2) -0.0064(17) 0.0039(17) 0.0110(18) Er1 0.02074(12) 0.02025(12) 0.01265(10) -0.00362(9) -0.00113(9) 0.01129(10) N21 0.063(4) 0.126(6) 0.048(4) -0.015(4) -0.030(3) 0.042(4) O11 0.054(4) 0.096(6) 0.166(11) -0.045(6) -0.049(5) 0.013(4) O12 0.097(6) 0.106(6) 0.077(6) -0.047(5) -0.060(5) 0.039(5) O13 0.115(8) 0.127(9) 0.178(13) -0.059(9) -0.075(8) 0.064(7) N22 0.063(4) 0.126(6) 0.048(4) -0.015(4) -0.030(3) 0.042(4) O14 0.083(6) 0.121(8) 0.270(18) -0.069(10) -0.042(8) 0.073(7) O15 0.074(7) 0.120(9) 0.75(5) -0.203(18) 0.100(15) 0.013(7) O16 0.072(7) 0.194(14) 0.247(18) 0.045(13) 0.028(9) 0.062(8) Cl1 0.069(3) 0.080(4) 0.131(6) 0.003(4) 0.039(4) 0.033(3) Cl2 0.108(5) 0.091(5) 0.086(5) -0.010(4) 0.002(4) -0.003(4) C31 0.073(7) 0.049(6) 0.152(14) 0.033(7) 0.085(8) 0.030(6) C32 0.052(5) 0.052(5) 0.084(8) 0.011(5) 0.025(5) 0.022(4) C33 0.050(5) 0.040(4) 0.058(6) 0.008(4) 0.016(4) 0.016(4) C34 0.028(4) 0.055(5) 0.063(6) -0.008(4) 0.012(4) 0.009(4) C35 0.035(5) 0.049(5) 0.107(9) -0.020(5) 0.040(5) -0.008(4) C36 0.080(8) 0.032(5) 0.156(13) -0.007(6) 0.097(9) -0.001(5) O17 0.127(7) 0.080(5) 0.264(14) 0.095(7) 0.143(9) 0.076(6) O18 0.041(3) 0.085(5) 0.066(5) -0.015(4) -0.003(3) 0.020(3) C1 0.024(3) 0.022(3) 0.007(3) -0.0019(19) 0.0030(19) 0.018(2) C2 0.027(3) 0.027(3) 0.021(3) -0.005(2) 0.000(2) 0.018(3) C3 0.026(3) 0.027(3) 0.014(3) 0.000(2) 0.000(2) 0.018(3) C4 0.020(3) 0.028(3) 0.018(3) -0.001(2) -0.008(2) 0.014(2) C5 0.029(3) 0.014(3) 0.022(3) 0.003(2) 0.004(2) 0.011(2) C6 0.030(3) 0.029(3) 0.013(3) -0.001(2) -0.004(3) 0.014(3) C7 0.029(3) 0.015(3) 0.014(3) -0.004(2) -0.001(2) 0.010(2) C8 0.027(3) 0.019(3) 0.031(4) 0.002(2) 0.005(2) 0.011(2) C9 0.022(3) 0.015(2) 0.016(3) 0.001(2) -0.001(2) 0.007(2) C10 0.027(3) 0.024(3) 0.005(3) 0.004(2) 0.003(2) 0.008(2) C11 0.028(3) 0.015(3) 0.023(3) -0.006(2) 0.002(2) 0.007(2) C12 0.024(3) 0.023(3) 0.026(3) 0.000(2) 0.002(2) 0.009(2) C13 0.012(2) 0.027(3) 0.018(3) -0.002(2) -0.005(2) 0.006(2) C14 0.015(3) 0.028(3) 0.015(3) -0.004(2) 0.003(2) 0.007(2) C15 0.013(2) 0.022(3) 0.020(3) -0.001(2) 0.000(2) 0.006(2) C16 0.008(2) 0.027(3) 0.016(3) -0.001(2) 0.0083(19) 0.006(2) C17 0.020(3) 0.032(3) 0.007(3) 0.000(2) 0.001(2) 0.012(2) C18 0.018(3) 0.023(3) 0.012(3) -0.001(2) 0.002(2) 0.012(2) C19 0.021(3) 0.018(3) 0.011(3) 0.006(2) 0.001(2) 0.010(2) C20 0.021(3) 0.022(3) 0.025(3) -0.001(2) -0.001(2) 0.016(2) C21 0.026(3) 0.018(3) 0.015(3) 0.000(2) 0.003(2) 0.014(2) C22 0.025(3) 0.019(3) 0.017(3) -0.002(2) 0.007(2) 0.013(2) C23 0.019(3) 0.023(3) 0.024(3) 0.006(2) 0.003(2) 0.010(2) C24 0.024(3) 0.017(3) 0.011(3) -0.004(2) 0.000(2) 0.008(2) C25 0.011(2) 0.019(3) 0.014(3) 0.004(2) 0.0046(19) 0.004(2) C26 0.021(3) 0.013(2) 0.013(3) 0.0015(19) 0.002(2) 0.007(2) C27 0.013(2) 0.015(3) 0.027(3) -0.004(2) -0.002(2) 0.004(2) C28 0.011(2) 0.019(3) 0.026(3) -0.009(2) -0.007(2) 0.006(2) C29 0.013(2) 0.023(3) 0.019(3) -0.002(2) 0.001(2) 0.008(2) C30 0.021(3) 0.034(3) 0.009(3) -0.005(2) -0.008(2) 0.016(2) N1 0.019(2) 0.020(2) 0.016(2) -0.0021(18) 0.0004(18) 0.0077(19) N2 0.028(3) 0.020(2) 0.015(3) -0.0013(18) -0.0033(19) 0.011(2) N3 0.032(3) 0.034(3) 0.008(2) -0.0034(19) -0.0049(19) 0.024(2) N4 0.026(3) 0.031(3) 0.019(3) -0.005(2) 0.001(2) 0.017(2) N5 0.026(2) 0.023(2) 0.018(3) -0.0052(19) -0.001(2) 0.014(2) N6 0.020(2) 0.020(2) 0.018(3) 0.0013(18) 0.0045(18) 0.0080(19) N7 0.028(3) 0.027(3) 0.021(3) -0.004(2) -0.004(2) 0.013(2) N8 0.024(2) 0.022(2) 0.030(3) 0.002(2) 0.000(2) 0.012(2) N9 0.023(2) 0.023(2) 0.027(3) 0.003(2) 0.003(2) 0.012(2) N10 0.020(2) 0.027(2) 0.020(3) -0.0015(19) 0.0044(19) 0.013(2) N11 0.021(2) 0.018(2) 0.019(3) -0.0015(18) -0.0014(19) 0.0081(19) N12 0.020(2) 0.022(2) 0.011(2) -0.0012(17) -0.0016(17) 0.0089(19) N13 0.022(3) 0.023(3) 0.027(4) -0.002(2) 0.002(2) 0.010(2) N14 0.021(2) 0.021(2) 0.010(2) 0.0008(17) 0.0047(17) 0.0141(19) N15 0.016(2) 0.021(2) 0.019(3) 0.0030(19) 0.0012(18) 0.0090(19) N16 0.015(2) 0.014(2) 0.020(3) 0.0053(18) 0.0073(18) 0.0047(18) N17 0.016(2) 0.017(2) 0.019(2) 0.0008(18) 0.0026(18) 0.0072(18) N18 0.021(2) 0.019(2) 0.019(2) -0.0026(18) -0.0016(18) 0.0091(19) N19 0.018(2) 0.015(2) 0.012(2) -0.0031(17) -0.0002(17) 0.0075(18) N20 0.022(2) 0.025(2) 0.015(2) -0.0023(18) -0.0038(18) 0.015(2) O1 0.023(2) 0.0201(19) 0.022(2) 0.0014(15) -0.0003(16) 0.0079(16) O2 0.025(2) 0.025(2) 0.021(2) 0.0003(16) 0.0024(16) 0.0133(17) O3 0.025(2) 0.026(2) 0.021(2) 0.0018(16) 0.0044(16) 0.0129(17) O4 0.029(2) 0.0258(19) 0.024(2) -0.0019(18) 0.0032(18) 0.0166(17) O5 0.024(2) 0.025(2) 0.013(2) 0.0005(15) 0.0015(15) 0.0125(17) O6 0.032(2) 0.031(2) 0.018(2) -0.0055(18) -0.0039(19) 0.0182(17) O7 0.035(2) 0.029(2) 0.015(2) -0.0029(16) 0.0020(16) 0.0164(18) O8 0.026(2) 0.024(2) 0.013(2) -0.0035(15) 0.0013(15) 0.0124(17) O9 0.0182(19) 0.029(2) 0.017(2) 0.0001(15) 0.0013(15) 0.0116(17) O10 0.029(2) 0.029(2) 0.023(2) -0.0013(17) 0.0050(17) 0.0189(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W Er1 2.308(4) . ? O2W Er1 2.323(4) . ? O3W Er1 2.347(4) . ? O4W Er1 2.335(4) . ? Er1 O1 2.295(4) . ? Er1 O9 2.295(4) 6_554 ? Er1 O8 2.335(4) 6_554 ? Er1 O2 2.347(4) . ? N21 O11 1.198(13) . ? N21 O12 1.221(10) . ? N21 O13 1.244(16) . ? N22 O15 1.250(2) . ? N22 O14 1.252(2) . ? N22 O16 1.253(2) . ? C31 C36 1.380(2) . ? C31 C32 1.380(2) . ? C31 O17 1.419(14) . ? C32 C33 1.380(2) . ? C32 H32 0.9400 . ? C33 C34 1.380(2) . ? C33 H33 0.9400 . ? C34 O18 1.372(11) . ? C34 C35 1.379(2) . ? C35 C36 1.380(2) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? O17 H17 0.8300 . ? O18 H18 0.8300 . ? C1 O1 1.245(7) . ? C1 N1 1.349(7) . ? C1 N2 1.352(7) . ? C2 N3 1.443(7) . ? C2 N1 1.489(8) . ? C2 C3 1.553(8) . ? C2 H2 0.9900 . ? C3 N2 1.439(7) . ? C3 N4 1.457(7) . ? C3 H3 0.9900 . ? C4 O6 1.225(7) . ? C4 N3 1.343(8) . ? C4 N4 1.377(8) . ? C5 N5 1.429(7) . ? C5 N2 1.459(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.445(8) . ? C6 N4 1.445(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.224(7) . ? C7 N5 1.339(7) . ? C7 N6 1.372(7) . ? C8 N5 1.442(8) . ? C8 N7 1.463(8) . ? C8 C9 1.566(8) . ? C8 H8 0.9900 . ? C9 N8 1.439(7) . ? C9 N6 1.449(7) . ? C9 H9 0.9900 . ? C10 O7 1.205(7) . ? C10 N8 1.367(8) . ? C10 N7 1.383(8) . ? C11 N6 1.436(8) . ? C11 N9 1.455(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.449(8) . ? C12 N11 1.450(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.231(7) . ? C13 N10 1.344(8) . ? C13 N9 1.366(8) . ? C14 N9 1.449(7) . ? C14 N11 1.453(7) . ? C14 C15 1.534(8) . ? C14 H14 0.9900 . ? C15 N10 1.454(7) . ? C15 N12 1.465(7) . ? C15 H15 0.9900 . ? C16 O8 1.230(7) . ? C16 N12 1.356(7) . ? C16 N11 1.357(7) . ? C17 N13 1.450(8) . ? C17 N10 1.457(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.443(7) . ? C18 N12 1.450(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.214(7) . ? C19 N14 1.369(7) . ? C19 N13 1.370(7) . ? C20 N15 1.448(8) . ? C20 N13 1.456(8) . ? C20 C21 1.563(8) . ? C20 H20 0.9900 . ? C21 N16 1.441(7) . ? C21 N14 1.456(7) . ? C21 H21 0.9900 . ? C22 O9 1.246(7) . ? C22 N15 1.334(7) . ? C22 N16 1.370(7) . ? C23 N17 1.440(7) . ? C23 N14 1.443(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.439(7) . ? C24 N19 1.448(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.230(7) . ? C25 N17 1.354(7) . ? C25 N18 1.360(7) . ? C26 N17 1.444(7) . ? C26 N19 1.460(7) . ? C26 C27 1.554(8) . ? C26 H26 0.9900 . ? C27 N20 1.437(8) . ? C27 N18 1.439(7) . ? C27 H27 0.9900 . ? C28 O10 1.250(7) . ? C28 N19 1.343(7) . ? C28 N20 1.354(7) . ? C29 N18 1.443(7) . ? C29 N1 1.449(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N3 1.438(7) . ? C30 N20 1.452(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O8 Er1 2.335(4) 5 ? O9 Er1 2.295(4) 5 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O9 135.02(14) . 6_554 ? O1 Er1 O1W 79.10(16) . . ? O9 Er1 O1W 116.04(16) 6_554 . ? O1 Er1 O2W 116.63(15) . . ? O9 Er1 O2W 79.30(15) 6_554 . ? O1W Er1 O2W 140.86(14) . . ? O1 Er1 O8 146.35(14) . 6_554 ? O9 Er1 O8 75.64(14) 6_554 6_554 ? O1W Er1 O8 73.04(14) . 6_554 ? O2W Er1 O8 77.07(15) . 6_554 ? O1 Er1 O4W 74.52(15) . . ? O9 Er1 O4W 72.01(14) 6_554 . ? O1W Er1 O4W 70.94(15) . . ? O2W Er1 O4W 145.67(15) . . ? O8 Er1 O4W 112.45(15) 6_554 . ? O1 Er1 O2 75.84(14) . . ? O9 Er1 O2 146.60(15) 6_554 . ? O1W Er1 O2 76.80(15) . . ? O2W Er1 O2 73.46(15) . . ? O8 Er1 O2 79.69(14) 6_554 . ? O4W Er1 O2 139.45(14) . . ? O1 Er1 O3W 72.27(14) . . ? O9 Er1 O3W 74.55(14) 6_554 . ? O1W Er1 O3W 145.45(15) . . ? O2W Er1 O3W 71.41(15) . . ? O8 Er1 O3W 139.80(14) 6_554 . ? O4W Er1 O3W 82.92(16) . . ? O2 Er1 O3W 113.33(15) . . ? O11 N21 O12 125.5(11) . . ? O11 N21 O13 115.1(10) . . ? O12 N21 O13 119.3(12) . . ? O15 N22 O14 113.5(14) . . ? O15 N22 O16 124.5(14) . . ? O14 N22 O16 121.9(12) . . ? C36 C31 C32 120.6(9) . . ? C36 C31 O17 121.9(9) . . ? C32 C31 O17 117.4(10) . . ? C33 C32 C31 117.9(9) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 C34 122.2(8) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? O18 C34 C35 115.6(7) . . ? O18 C34 C33 125.3(6) . . ? C35 C34 C33 119.1(8) . . ? C34 C35 C36 119.6(9) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C31 120.6(10) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C31 O17 H17 109.5 . . ? C34 O18 H18 109.5 . . ? O1 C1 N1 123.9(5) . . ? O1 C1 N2 125.9(5) . . ? N1 C1 N2 110.2(5) . . ? N3 C2 N1 114.3(5) . . ? N3 C2 C3 104.2(5) . . ? N1 C2 C3 101.8(4) . . ? N3 C2 H2 111.9 . . ? N1 C2 H2 111.9 . . ? C3 C2 H2 111.9 . . ? N2 C3 N4 115.4(5) . . ? N2 C3 C2 104.4(4) . . ? N4 C3 C2 102.1(4) . . ? N2 C3 H3 111.5 . . ? N4 C3 H3 111.5 . . ? C2 C3 H3 111.5 . . ? O6 C4 N3 126.1(5) . . ? O6 C4 N4 124.8(5) . . ? N3 C4 N4 108.9(5) . . ? N5 C5 N2 112.0(4) . . ? N5 C5 H5A 109.2 . . ? N2 C5 H5A 109.2 . . ? N5 C5 H5B 109.2 . . ? N2 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N7 C6 N4 114.1(5) . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6B 108.7 . . ? N4 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 127.5(5) . . ? O2 C7 N6 123.9(5) . . ? N5 C7 N6 108.5(5) . . ? N5 C8 N7 114.3(5) . . ? N5 C8 C9 102.6(5) . . ? N7 C8 C9 103.0(4) . . ? N5 C8 H8 112.1 . . ? N7 C8 H8 112.1 . . ? C9 C8 H8 112.1 . . ? N8 C9 N6 117.4(4) . . ? N8 C9 C8 103.0(4) . . ? N6 C9 C8 102.6(4) . . ? N8 C9 H9 111.0 . . ? N6 C9 H9 111.0 . . ? C8 C9 H9 111.0 . . ? O7 C10 N8 126.1(6) . . ? O7 C10 N7 125.8(5) . . ? N8 C10 N7 108.0(5) . . ? N6 C11 N9 113.9(5) . . ? N6 C11 H11A 108.8 . . ? N9 C11 H11A 108.8 . . ? N6 C11 H11B 108.8 . . ? N9 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N8 C12 N11 112.8(5) . . ? N8 C12 H12A 109.0 . . ? N11 C12 H12A 109.0 . . ? N8 C12 H12B 109.0 . . ? N11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? O3 C13 N10 125.7(5) . . ? O3 C13 N9 125.1(5) . . ? N10 C13 N9 109.2(5) . . ? N9 C14 N11 114.5(5) . . ? N9 C14 C15 102.3(4) . . ? N11 C14 C15 103.7(4) . . ? N9 C14 H14 111.9 . . ? N11 C14 H14 111.9 . . ? C15 C14 H14 111.9 . . ? N10 C15 N12 114.6(4) . . ? N10 C15 C14 104.3(4) . . ? N12 C15 C14 102.3(4) . . ? N10 C15 H15 111.7 . . ? N12 C15 H15 111.7 . . ? C14 C15 H15 111.7 . . ? O8 C16 N12 126.8(5) . . ? O8 C16 N11 124.9(5) . . ? N12 C16 N11 108.3(5) . . ? N13 C17 N10 113.6(5) . . ? N13 C17 H17A 108.9 . . ? N10 C17 H17A 108.9 . . ? N13 C17 H17B 108.9 . . ? N10 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 113.2(4) . . ? N15 C18 H18A 108.9 . . ? N12 C18 H18A 108.9 . . ? N15 C18 H18B 108.9 . . ? N12 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N14 126.5(5) . . ? O4 C19 N13 125.7(5) . . ? N14 C19 N13 107.7(5) . . ? N15 C20 N13 114.8(5) . . ? N15 C20 C21 102.2(4) . . ? N13 C20 C21 102.9(4) . . ? N15 C20 H20 112.0 . . ? N13 C20 H20 112.0 . . ? C21 C20 H20 112.0 . . ? N16 C21 N14 112.8(4) . . ? N16 C21 C20 103.9(4) . . ? N14 C21 C20 102.9(4) . . ? N16 C21 H21 112.2 . . ? N14 C21 H21 112.2 . . ? C20 C21 H21 112.2 . . ? O9 C22 N15 127.1(5) . . ? O9 C22 N16 122.7(5) . . ? N15 C22 N16 110.2(5) . . ? N17 C23 N14 114.6(5) . . ? N17 C23 H23A 108.6 . . ? N14 C23 H23A 108.6 . . ? N17 C23 H23B 108.6 . . ? N14 C23 H23B 108.6 . . ? H23A C23 H23B 107.6 . . ? N16 C24 N19 114.1(4) . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N19 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N17 124.4(5) . . ? O5 C25 N18 126.4(5) . . ? N17 C25 N18 109.3(5) . . ? N17 C26 N19 116.2(4) . . ? N17 C26 C27 104.0(4) . . ? N19 C26 C27 101.2(4) . . ? N17 C26 H26 111.6 . . ? N19 C26 H26 111.6 . . ? C27 C26 H26 111.6 . . ? N20 C27 N18 115.5(4) . . ? N20 C27 C26 104.2(4) . . ? N18 C27 C26 102.1(4) . . ? N20 C27 H27 111.5 . . ? N18 C27 H27 111.5 . . ? C26 C27 H27 111.5 . . ? O10 C28 N19 126.1(5) . . ? O10 C28 N20 124.5(5) . . ? N19 C28 N20 109.3(5) . . ? N18 C29 N1 113.5(4) . . ? N18 C29 H29A 108.9 . . ? N1 C29 H29A 108.9 . . ? N18 C29 H29B 108.9 . . ? N1 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? N3 C30 N20 114.8(4) . . ? N3 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N3 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? C1 N1 C29 122.1(5) . . ? C1 N1 C2 111.5(4) . . ? C29 N1 C2 125.2(4) . . ? C1 N2 C3 112.1(5) . . ? C1 N2 C5 121.7(5) . . ? C3 N2 C5 126.1(5) . . ? C4 N3 C30 123.3(5) . . ? C4 N3 C2 112.5(5) . . ? C30 N3 C2 123.8(5) . . ? C4 N4 C6 123.0(5) . . ? C4 N4 C3 112.2(5) . . ? C6 N4 C3 124.4(5) . . ? C7 N5 C5 123.8(5) . . ? C7 N5 C8 113.7(5) . . ? C5 N5 C8 122.4(5) . . ? C7 N6 C11 122.8(5) . . ? C7 N6 C9 112.2(5) . . ? C11 N6 C9 123.4(5) . . ? C10 N7 C6 121.8(5) . . ? C10 N7 C8 111.7(5) . . ? C6 N7 C8 124.3(5) . . ? C10 N8 C9 113.6(5) . . ? C10 N8 C12 121.3(5) . . ? C9 N8 C12 125.0(5) . . ? C13 N9 C14 112.2(5) . . ? C13 N9 C11 122.6(5) . . ? C14 N9 C11 125.3(5) . . ? C13 N10 C15 110.8(5) . . ? C13 N10 C17 122.7(5) . . ? C15 N10 C17 122.9(4) . . ? C16 N11 C12 121.5(5) . . ? C16 N11 C14 112.2(5) . . ? C12 N11 C14 123.2(5) . . ? C16 N12 C18 125.1(5) . . ? C16 N12 C15 112.8(5) . . ? C18 N12 C15 121.7(4) . . ? C19 N13 C17 121.9(5) . . ? C19 N13 C20 113.2(5) . . ? C17 N13 C20 124.5(5) . . ? C19 N14 C23 122.0(4) . . ? C19 N14 C21 113.2(4) . . ? C23 N14 C21 124.1(5) . . ? C22 N15 C18 122.1(5) . . ? C22 N15 C20 112.7(4) . . ? C18 N15 C20 125.1(4) . . ? C22 N16 C24 122.2(5) . . ? C22 N16 C21 110.8(5) . . ? C24 N16 C21 124.2(4) . . ? C25 N17 C23 121.7(5) . . ? C25 N17 C26 111.2(4) . . ? C23 N17 C26 123.3(4) . . ? C25 N18 C27 112.8(4) . . ? C25 N18 C29 123.2(5) . . ? C27 N18 C29 123.7(5) . . ? C28 N19 C24 124.7(4) . . ? C28 N19 C26 112.9(4) . . ? C24 N19 C26 121.2(4) . . ? C28 N20 C27 111.5(5) . . ? C28 N20 C30 121.5(5) . . ? C27 N20 C30 123.8(4) . . ? C1 O1 Er1 154.4(4) . . ? C7 O2 Er1 150.1(4) . . ? C16 O8 Er1 147.8(4) . 5 ? C22 O9 Er1 149.4(4) . 5 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.484 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.110 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.063 0.707 0.019 59 30 ' ' 2 -0.185 0.251 0.141 95 43 ' ' 3 -0.065 0.533 0.312 45 9 ' ' 4 -0.033 0.310 0.440 34 11 ' ' 5 0.064 0.293 0.520 58 29 ' ' 6 0.185 0.749 0.641 95 43 ' ' 7 0.064 0.467 0.812 45 9 ' ' 8 0.034 0.690 0.939 33 11 ' ' 9 0.230 0.937 0.186 60 30 ' ' 10 0.049 0.511 0.597 10 8 ' ' 11 0.254 0.434 0.974 93 43 ' ' 12 0.293 0.230 0.353 59 29 ' ' 13 0.310 0.343 0.273 32 11 ' ' 14 0.336 0.032 0.106 31 11 ' ' 15 0.436 0.185 0.807 95 43 ' ' 16 0.402 0.935 0.479 45 9 ' ' 17 0.467 0.402 0.645 45 9 ' ' 18 0.533 0.598 0.145 45 9 ' ' 19 0.466 0.947 0.266 11 8 ' ' 20 0.567 0.819 0.308 93 43 ' ' 21 0.492 0.539 0.928 11 9 ' ' 22 0.519 0.467 0.432 11 8 ' ' 23 0.598 0.064 0.979 45 8 ' ' 24 0.539 0.046 0.762 11 9 ' ' 25 0.748 0.567 0.475 92 43 ' ' 26 0.773 1.064 0.685 59 29 ' ' 27 0.663 0.968 0.606 31 11 ' ' 28 0.709 0.773 0.852 59 29 ' ' 29 0.696 0.664 0.772 31 11 ' ' 30 0.951 0.489 0.097 10 8 ' ' _platon_squeeze_details ; ; data_01 _database_code_depnum_ccdc_archive 'CCDC 875766' #TrackingRef 'submit-01.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 La N21 O17, C6 H6 O2, N O3,10(H2 O)' _chemical_formula_sum 'C36 H64 Cl La N22 O32' _chemical_formula_weight 1491.45 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' La La -0.2871 2.4523 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a' _symmetry_space_group_name_Hall '-P 2a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 20.300(5) _cell_length_b 13.551(3) _cell_length_c 20.469(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5631(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8087 _exptl_absorpt_correction_T_max 0.8440 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30131 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4987 _reflns_number_gt 4225 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+10.6949P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4987 _refine_ls_number_parameters 390 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.22613(14) 0.1859(2) 0.19508(15) 0.0365(7) Uani 1 1 d . . . O2W O 0.16651(14) -0.1274(2) 0.12400(16) 0.0408(7) Uani 1 1 d . . . N11 N 0.2500 0.0000 0.0239(3) 0.0400(14) Uani 1 2 d S . . O6 O 0.2500 0.0000 -0.0351(3) 0.077(2) Uani 1 2 d S . . O7 O 0.20975(14) 0.0524(3) 0.05661(14) 0.0391(7) Uani 1 1 d . . . La1 La 0.2500 0.0000 0.172601(15) 0.02221(15) Uani 1 2 d S . . C1 C 0.08126(17) 0.0958(3) 0.20322(18) 0.0250(8) Uani 1 1 d . . . C2 C -0.01904(17) 0.1760(3) 0.21722(18) 0.0250(8) Uani 1 1 d . . . H2 H -0.0256 0.2437 0.2003 0.030 Uiso 1 1 calc R . . C3 C 0.13526(18) 0.1190(3) 0.31120(19) 0.0264(8) Uani 1 1 d . . . H3A H 0.1343 0.1744 0.3420 0.032 Uiso 1 1 calc R . . H3B H 0.1767 0.1231 0.2867 0.032 Uiso 1 1 calc R . . C4 C 0.00958(18) 0.1020(3) 0.10596(18) 0.0271(8) Uani 1 1 d . . . H4A H -0.0132 0.1598 0.0883 0.033 Uiso 1 1 calc R . . H4B H 0.0515 0.0954 0.0827 0.033 Uiso 1 1 calc R . . C5 C 0.16198(18) -0.0574(3) 0.32547(17) 0.0251(8) Uani 1 1 d . . . C6 C 0.1012(2) 0.0138(3) 0.4100(2) 0.0258(8) Uani 1 1 d . . . H6 H 0.1177 0.0602 0.4435 0.031 Uiso 1 1 calc R . . C7 C 0.11691(19) -0.0934(3) 0.42768(17) 0.0279(9) Uani 1 1 d . . . H7 H 0.1465 -0.0975 0.4661 0.033 Uiso 1 1 calc R . . C8 C 0.00272(19) -0.0694(3) 0.43095(17) 0.0266(8) Uani 1 1 d . . . C9 C 0.17797(18) -0.2289(3) 0.3627(2) 0.0296(8) Uani 1 1 d . . . H9A H 0.2168 -0.2251 0.3343 0.036 Uiso 1 1 calc R . . H9B H 0.1928 -0.2506 0.4059 0.036 Uiso 1 1 calc R . . C10 C 0.0412(2) -0.2365(3) 0.46028(18) 0.0308(9) Uani 1 1 d . . . H10A H 0.0777 -0.2588 0.4879 0.037 Uiso 1 1 calc R . . H10B H 0.0008 -0.2397 0.4865 0.037 Uiso 1 1 calc R . . C11 C 0.12848(19) -0.3230(3) 0.2719(2) 0.0312(9) Uani 1 1 d . . . C12 C 0.0885(2) -0.3581(3) 0.3767(2) 0.0313(9) Uani 1 1 d . . . H12 H 0.1124 -0.3978 0.4097 0.038 Uiso 1 1 calc R . . C13 C 0.0534(2) -0.4245(3) 0.32589(19) 0.0328(9) Uani 1 1 d . . . H13 H 0.0618 -0.4954 0.3342 0.039 Uiso 1 1 calc R . . C14 C -0.0258(2) -0.3303(3) 0.3825(2) 0.0358(10) Uani 1 1 d . . . C15 C 0.0697(2) -0.4415(3) 0.2023(2) 0.0339(9) Uani 1 1 d . . . H15A H 0.1099 -0.4373 0.1760 0.041 Uiso 1 1 calc R . . H15B H 0.0606 -0.5115 0.2102 0.041 Uiso 1 1 calc R . . N1 N 0.02290(15) 0.1184(3) 0.17495(14) 0.0253(7) Uani 1 1 d . . . N2 N 0.08092(15) 0.1293(2) 0.26604(15) 0.0257(7) Uani 1 1 d . . . N3 N 0.13459(17) 0.0274(3) 0.34793(16) 0.0280(7) Uani 1 1 d . . . N4 N 0.14898(15) -0.1311(3) 0.36838(15) 0.0281(7) Uani 1 1 d . . . N5 N 0.03003(17) 0.0151(3) 0.40631(18) 0.0275(7) Uani 1 1 d . . . N6 N 0.05269(15) -0.1356(3) 0.44151(16) 0.0287(7) Uani 1 1 d . . . N7 N 0.13326(17) -0.3008(3) 0.33667(16) 0.0318(8) Uani 1 1 d . . . N8 N 0.08109(17) -0.3931(3) 0.26437(16) 0.0327(8) Uani 1 1 d . . . N9 N 0.03492(17) -0.3024(3) 0.40584(17) 0.0328(8) Uani 1 1 d . . . N10 N -0.01593(18) -0.4000(3) 0.33440(17) 0.0350(8) Uani 1 1 d . . . O1 O 0.12731(13) 0.0532(2) 0.17598(12) 0.0301(6) Uani 1 1 d . . . O2 O 0.19429(13) -0.0666(2) 0.27501(13) 0.0319(6) Uani 1 1 d . . . O3 O 0.16171(14) -0.2865(2) 0.22817(14) 0.0362(7) Uani 1 1 d . . . O4 O -0.07875(14) -0.3010(2) 0.40156(16) 0.0414(7) Uani 1 1 d . . . O5 O -0.05530(13) -0.0827(2) 0.44365(14) 0.0335(6) Uani 1 1 d . . . O8 O 0.1540(4) 0.3616(5) 0.3151(6) 0.179(4) Uani 1 1 d . . . H8 H 0.1436 0.3480 0.2769 0.269 Uiso 1 1 calc R . . C16 C 0.2264(4) 0.4673(5) 0.3768(5) 0.084(2) Uani 1 1 d . . . H16 H 0.2082 0.4445 0.4163 0.101 Uiso 1 1 calc R . . C17 C 0.2027(4) 0.4311(5) 0.3150(6) 0.102(3) Uani 1 1 d . . . C18 C 0.2279(5) 0.4673(7) 0.2584(5) 0.105(3) Uani 1 1 d . . . H18 H 0.2120 0.4431 0.2184 0.126 Uiso 1 1 calc R . . N12 N 0.1014(6) 0.3159(7) 0.1370(6) 0.058(3) Uani 0.50 1 d PD . . O9 O 0.0468(6) 0.3486(9) 0.1188(7) 0.269(17) Uani 0.50 1 d PD . . O10 O 0.1370(7) 0.2703(9) 0.1060(8) 0.122(5) Uani 0.50 1 d P . . O11 O 0.0919(8) 0.3254(8) 0.1970(6) 0.141(6) Uani 0.50 1 d PD . . Cl1 Cl 0.0000 -0.1349(12) 0.2500 0.83(3) Uani 1 2 d S . . 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 O1W 0.0280(14) 0.0423(17) 0.0392(17) -0.0007(14) 0.0035(13) 0.0003(13) O2W 0.0275(14) 0.0490(18) 0.0460(19) -0.0057(15) -0.0114(13) 0.0003(12) N11 0.029(3) 0.075(4) 0.015(3) 0.000 0.000 0.012(2) O6 0.054(4) 0.158(7) 0.018(3) 0.000 0.000 0.046(3) O7 0.0291(14) 0.065(2) 0.0227(14) 0.0005(15) 0.0019(12) 0.0137(14) La1 0.0156(2) 0.0366(2) 0.0144(2) 0.000 0.000 0.00163(10) C1 0.0190(17) 0.034(2) 0.0217(19) 0.0014(16) 0.0024(14) -0.0056(15) C2 0.0238(18) 0.0288(19) 0.0225(19) 0.0015(15) 0.0022(15) 0.0014(14) C3 0.0220(18) 0.036(2) 0.0211(18) -0.0013(16) -0.0011(15) -0.0050(15) C4 0.0251(18) 0.037(2) 0.020(2) 0.0040(16) 0.0027(15) -0.0033(16) C5 0.0185(18) 0.038(2) 0.018(2) 0.0000(15) -0.0032(14) -0.0034(16) C6 0.022(2) 0.043(2) 0.0132(17) -0.0041(15) 0.0005(16) -0.0029(15) C7 0.0221(19) 0.045(2) 0.0164(19) -0.0011(16) -0.0024(14) -0.0015(17) C8 0.027(2) 0.042(2) 0.0108(17) -0.0027(15) -0.0013(14) -0.0024(17) C9 0.0229(18) 0.039(2) 0.026(2) 0.0017(17) -0.0016(15) 0.0026(16) C10 0.034(2) 0.040(2) 0.0174(19) 0.0034(16) 0.0022(16) -0.0026(17) C11 0.030(2) 0.035(2) 0.029(2) 0.0026(17) -0.0015(17) 0.0060(16) C12 0.032(2) 0.038(2) 0.024(2) 0.0082(17) -0.0004(16) 0.0038(17) C13 0.038(2) 0.032(2) 0.028(2) 0.0055(16) 0.0023(16) 0.0027(18) C14 0.040(2) 0.041(2) 0.027(2) 0.0018(18) 0.0041(18) -0.0018(18) C15 0.035(2) 0.036(2) 0.031(2) -0.0051(18) 0.0031(17) 0.0057(17) N1 0.0196(15) 0.0401(19) 0.0163(16) -0.0019(13) 0.0009(11) 0.0008(13) N2 0.0192(15) 0.0386(18) 0.0194(16) -0.0034(13) 0.0002(12) -0.0003(12) N3 0.0321(18) 0.0382(18) 0.0135(16) 0.0004(14) 0.0044(14) -0.0025(15) N4 0.0275(16) 0.0406(19) 0.0164(15) 0.0011(14) 0.0017(13) 0.0025(13) N5 0.0221(18) 0.043(2) 0.0181(16) 0.0015(14) 0.0008(14) -0.0001(13) N6 0.0233(16) 0.0422(19) 0.0205(16) 0.0043(14) 0.0001(13) -0.0021(14) N7 0.0295(18) 0.040(2) 0.0262(18) 0.0025(14) 0.0008(14) -0.0015(15) N8 0.0357(18) 0.0367(18) 0.0257(18) -0.0011(15) 0.0025(14) -0.0004(14) N9 0.0280(17) 0.043(2) 0.0271(18) -0.0021(15) 0.0015(14) -0.0004(15) N10 0.0330(19) 0.040(2) 0.032(2) -0.0040(15) 0.0005(14) -0.0021(15) O1 0.0217(14) 0.0456(18) 0.0229(14) -0.0050(12) 0.0020(10) 0.0021(12) O2 0.0287(14) 0.0453(16) 0.0217(14) 0.0004(12) 0.0078(11) 0.0017(12) O3 0.0355(16) 0.0463(17) 0.0266(15) 0.0026(13) 0.0050(12) -0.0030(13) O4 0.0291(16) 0.057(2) 0.0386(17) -0.0056(15) 0.0058(13) -0.0016(14) O5 0.0251(14) 0.0509(18) 0.0247(14) 0.0012(13) 0.0021(11) -0.0033(12) O8 0.112(5) 0.085(5) 0.341(14) -0.059(6) -0.043(6) -0.003(4) C16 0.079(5) 0.054(4) 0.120(7) 0.004(4) 0.009(5) 0.015(3) C17 0.058(4) 0.049(4) 0.199(11) -0.010(5) -0.005(5) 0.021(3) C18 0.091(7) 0.105(8) 0.117(7) -0.001(6) 0.001(5) 0.055(5) N12 0.068(6) 0.024(5) 0.084(8) -0.004(5) 0.001(6) 0.012(4) O9 0.59(5) 0.053(8) 0.161(17) -0.073(10) 0.18(2) -0.085(17) O10 0.108(9) 0.075(7) 0.182(13) 0.047(9) -0.060(9) 0.013(7) O11 0.202(15) 0.067(7) 0.154(13) 0.054(8) -0.068(12) -0.069(8) Cl1 1.37(8) 0.253(16) 0.86(5) 0.000 -0.66(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W La1 2.606(3) . ? O2W La1 2.616(3) . ? N11 O6 1.208(8) . ? N11 O7 1.272(4) 2 ? N11 O7 1.272(4) . ? N11 La1 3.043(5) . ? O7 La1 2.609(3) . ? La1 O2 2.547(3) 2 ? La1 O2 2.547(3) . ? La1 O1 2.594(3) 2 ? La1 O1 2.594(3) . ? La1 O1W 2.606(3) 2 ? La1 O7 2.609(3) 2 ? La1 O2W 2.616(3) 2 ? C1 O1 1.232(5) . ? C1 N1 1.353(5) . ? C1 N2 1.363(5) . ? C2 N1 1.443(5) . ? C2 N2 1.448(5) 3 ? C2 C2 1.549(7) 3 ? C2 H2 0.9900 . ? C3 N2 1.446(5) . ? C3 N3 1.451(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 N5 1.448(5) 3 ? C4 N1 1.455(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 O2 1.230(4) . ? C5 N4 1.356(5) . ? C5 N3 1.357(6) . ? C6 N5 1.446(6) . ? C6 N3 1.452(5) . ? C6 C7 1.531(6) . ? C6 H6 0.9900 . ? C7 N6 1.451(5) . ? C7 N4 1.469(5) . ? C7 H7 0.9900 . ? C8 O5 1.219(5) . ? C8 N5 1.368(6) . ? C8 N6 1.371(5) . ? C9 N7 1.434(5) . ? C9 N4 1.454(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 N9 1.434(5) . ? C10 N6 1.440(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 O3 1.226(5) . ? C11 N8 1.361(5) . ? C11 N7 1.362(5) . ? C12 N7 1.450(5) . ? C12 N9 1.451(5) . ? C12 C13 1.549(6) . ? C12 H12 0.9900 . ? C13 N8 1.443(5) . ? C13 N10 1.455(6) . ? C13 H13 0.9900 . ? C14 O4 1.210(5) . ? C14 N9 1.375(6) . ? C14 N10 1.379(6) . ? C15 N10 1.439(5) 3 ? C15 N8 1.448(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? N2 C2 1.448(5) 3 ? N5 C4 1.448(5) 3 ? N10 C15 1.439(5) 3 ? O8 C17 1.366(10) . ? O8 H8 0.8300 . ? C16 C16 1.306(16) 2_565 ? C16 C17 1.441(13) . ? C16 H16 0.9400 . ? C17 C18 1.357(13) . ? C18 C18 1.26(2) 2_565 ? C18 H18 0.9400 . ? N12 O10 1.142(18) . ? N12 O11 1.250(2) . ? N12 O9 1.251(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 O6 N11 O7 121.7(2) . 2 ? O6 N11 O7 121.7(2) . . ? O7 N11 O7 116.5(5) 2 . ? O6 N11 La1 180.0 . . ? O7 N11 La1 58.3(2) 2 . ? O7 N11 La1 58.3(2) . . ? N11 O7 La1 97.2(3) . . ? O2 La1 O2 69.23(13) 2 . ? O2 La1 O1 69.53(9) 2 2 ? O2 La1 O1 107.82(8) . 2 ? O2 La1 O1 107.81(8) 2 . ? O2 La1 O1 69.53(9) . . ? O1 La1 O1 176.95(11) 2 . ? O2 La1 O1W 96.59(9) 2 2 ? O2 La1 O1W 66.09(9) . 2 ? O1 La1 O1W 63.14(9) 2 2 ? O1 La1 O1W 116.25(9) . 2 ? O2 La1 O1W 66.09(9) 2 . ? O2 La1 O1W 96.59(9) . . ? O1 La1 O1W 116.25(9) 2 . ? O1 La1 O1W 63.14(9) . . ? O1W La1 O1W 159.66(14) 2 . ? O2 La1 O7 142.33(10) 2 . ? O2 La1 O7 134.93(9) . . ? O1 La1 O7 113.61(8) 2 . ? O1 La1 O7 69.39(8) . . ? O1W La1 O7 118.79(10) 2 . ? O1W La1 O7 80.77(10) . . ? O2 La1 O7 134.93(9) 2 2 ? O2 La1 O7 142.33(10) . 2 ? O1 La1 O7 69.39(8) 2 2 ? O1 La1 O7 113.61(8) . 2 ? O1W La1 O7 80.77(10) 2 2 ? O1W La1 O7 118.79(10) . 2 ? O7 La1 O7 49.01(13) . 2 ? O2 La1 O2W 146.57(10) 2 . ? O2 La1 O2W 77.96(10) . . ? O1 La1 O2W 116.68(9) 2 . ? O1 La1 O2W 64.61(9) . . ? O1W La1 O2W 63.24(9) 2 . ? O1W La1 O2W 125.77(9) . . ? O7 La1 O2W 68.31(11) . . ? O7 La1 O2W 71.18(10) 2 . ? O2 La1 O2W 77.96(10) 2 2 ? O2 La1 O2W 146.57(10) . 2 ? O1 La1 O2W 64.61(9) 2 2 ? O1 La1 O2W 116.68(9) . 2 ? O1W La1 O2W 125.77(9) 2 2 ? O1W La1 O2W 63.24(9) . 2 ? O7 La1 O2W 71.18(10) . 2 ? O7 La1 O2W 68.31(11) 2 2 ? O2W La1 O2W 135.30(15) . 2 ? O2 La1 N11 145.39(6) 2 . ? O2 La1 N11 145.39(6) . . ? O1 La1 N11 91.53(6) 2 . ? O1 La1 N11 91.53(6) . . ? O1W La1 N11 100.17(7) 2 . ? O1W La1 N11 100.17(7) . . ? O7 La1 N11 24.50(6) . . ? O7 La1 N11 24.50(6) 2 . ? O2W La1 N11 67.65(7) . . ? O2W La1 N11 67.65(7) 2 . ? O1 C1 N1 125.2(3) . . ? O1 C1 N2 125.9(3) . . ? N1 C1 N2 108.9(3) . . ? N1 C2 N2 114.7(3) . 3 ? N1 C2 C2 103.0(3) . 3 ? N2 C2 C2 103.2(3) 3 3 ? N1 C2 H2 111.8 . . ? N2 C2 H2 111.8 3 . ? C2 C2 H2 111.8 3 . ? N2 C3 N3 114.0(3) . . ? N2 C3 H3A 108.8 . . ? N3 C3 H3A 108.8 . . ? N2 C3 H3B 108.8 . . ? N3 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N5 C4 N1 113.3(3) 3 . ? N5 C4 H4A 108.9 3 . ? N1 C4 H4A 108.9 . . ? N5 C4 H4B 108.9 3 . ? N1 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? O2 C5 N4 124.9(4) . . ? O2 C5 N3 126.1(4) . . ? N4 C5 N3 109.0(3) . . ? N5 C6 N3 114.8(4) . . ? N5 C6 C7 103.4(3) . . ? N3 C6 C7 103.3(3) . . ? N5 C6 H6 111.6 . . ? N3 C6 H6 111.6 . . ? C7 C6 H6 111.6 . . ? N6 C7 N4 115.0(3) . . ? N6 C7 C6 103.4(3) . . ? N4 C7 C6 103.1(3) . . ? N6 C7 H7 111.6 . . ? N4 C7 H7 111.6 . . ? C6 C7 H7 111.6 . . ? O5 C8 N5 126.4(4) . . ? O5 C8 N6 125.8(4) . . ? N5 C8 N6 107.8(3) . . ? N7 C9 N4 113.1(3) . . ? N7 C9 H9A 109.0 . . ? N4 C9 H9A 109.0 . . ? N7 C9 H9B 109.0 . . ? N4 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N9 C10 N6 113.5(3) . . ? N9 C10 H10A 108.9 . . ? N6 C10 H10A 108.9 . . ? N9 C10 H10B 108.9 . . ? N6 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O3 C11 N8 126.0(4) . . ? O3 C11 N7 125.7(4) . . ? N8 C11 N7 108.3(3) . . ? N7 C12 N9 115.1(3) . . ? N7 C12 C13 102.7(3) . . ? N9 C12 C13 103.5(3) . . ? N7 C12 H12 111.6 . . ? N9 C12 H12 111.6 . . ? C13 C12 H12 111.6 . . ? N8 C13 N10 114.5(3) . . ? N8 C13 C12 103.6(3) . . ? N10 C13 C12 103.4(3) . . ? N8 C13 H13 111.6 . . ? N10 C13 H13 111.6 . . ? C12 C13 H13 111.6 . . ? O4 C14 N9 126.4(4) . . ? O4 C14 N10 125.8(4) . . ? N9 C14 N10 107.8(4) . . ? N10 C15 N8 113.7(3) 3 . ? N10 C15 H15A 108.8 3 . ? N8 C15 H15A 108.8 . . ? N10 C15 H15B 108.8 3 . ? N8 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C1 N1 C2 112.5(3) . . ? C1 N1 C4 122.9(3) . . ? C2 N1 C4 123.7(3) . . ? C1 N2 C3 124.5(3) . . ? C1 N2 C2 111.9(3) . 3 ? C3 N2 C2 123.5(3) . 3 ? C5 N3 C3 123.0(3) . . ? C5 N3 C6 112.3(3) . . ? C3 N3 C6 124.5(3) . . ? C5 N4 C9 122.7(3) . . ? C5 N4 C7 111.4(3) . . ? C9 N4 C7 124.3(3) . . ? C8 N5 C6 112.1(3) . . ? C8 N5 C4 121.3(3) . 3 ? C6 N5 C4 125.0(3) . 3 ? C8 N6 C10 122.9(3) . . ? C8 N6 C7 112.1(3) . . ? C10 N6 C7 124.9(3) . . ? C11 N7 C9 123.7(3) . . ? C11 N7 C12 112.8(3) . . ? C9 N7 C12 123.5(3) . . ? C11 N8 C13 112.5(3) . . ? C11 N8 C15 121.9(3) . . ? C13 N8 C15 124.7(3) . . ? C14 N9 C10 121.4(3) . . ? C14 N9 C12 112.7(3) . . ? C10 N9 C12 125.2(3) . . ? C14 N10 C15 122.0(4) . 3 ? C14 N10 C13 112.5(3) . . ? C15 N10 C13 125.5(4) 3 . ? C1 O1 La1 150.5(2) . . ? C5 O2 La1 153.1(3) . . ? C17 O8 H8 109.5 . . ? C16 C16 C17 118.4(5) 2_565 . ? C16 C16 H16 120.8 2_565 . ? C17 C16 H16 120.8 . . ? C18 C17 O8 121.6(11) . . ? C18 C17 C16 120.1(8) . . ? O8 C17 C16 118.3(11) . . ? C18 C18 C17 121.5(6) 2_565 . ? C18 C18 H18 119.3 2_565 . ? C17 C18 H18 119.3 . . ? O10 N12 O11 134.3(15) . . ? O10 N12 O9 126.0(14) . . ? O11 N12 O9 96.8(13) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.415 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.118 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.146 0.500 0.500 521 203 ' ' 2 0.338 0.500 1.000 521 203 ' ' _platon_squeeze_details ; ; data_03 _database_code_depnum_ccdc_archive 'CCDC 875767' #TrackingRef 'submit-03.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H159 Cl6 Eu3 N43 O76' _chemical_formula_weight 3548.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.8210(12) _cell_length_b 18.5168(13) _cell_length_c 24.5003(17) _cell_angle_alpha 106.175(2) _cell_angle_beta 100.333(2) _cell_angle_gamma 101.696(2) _cell_volume 6947.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3618 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7762 _exptl_absorpt_correction_T_max 0.8462 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74876 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.10 _reflns_number_total 24377 _reflns_number_gt 19984 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+1.0083P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24377 _refine_ls_number_parameters 1576 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl3 Cl 0.7482(4) 0.0085(6) 0.4062(3) 0.167(3) Uani 0.50 1 d P . . Cl4 Cl 0.9900(10) 0.2987(8) 0.5033(5) 0.259(6) Uani 0.50 1 d P . . Cl5 Cl 0.5506(8) -0.7476(8) 0.7640(5) 0.252(6) Uani 0.50 1 d P . . Cl6 Cl 0.4581(11) -0.3818(9) 0.5223(5) 0.282(7) Uani 0.50 1 d P . . Cl7 Cl 1.1253(5) 0.5717(4) 1.0890(3) 0.140(2) Uani 0.50 1 d P . . Cl8 Cl 0.9758(4) 0.6165(5) 0.9106(3) 0.141(2) Uani 0.50 1 d P . . Cl9 Cl 1.0892(7) 0.4837(9) 0.8068(12) 0.525(18) Uani 0.50 1 d P . . Cl10 Cl 0.9153(9) -0.4316(10) 0.6286(7) 0.286(7) Uani 0.50 1 d P . . N41 N 0.7896(3) 0.5646(3) 1.0408(2) 0.0441(11) Uani 1 1 d . . . N42 N 0.3518(3) -0.8044(3) 0.8447(2) 0.0520(12) Uani 1 1 d D . . N43 N 0.9081(5) -0.1420(4) 1.0167(3) 0.104(3) Uani 1 1 d D . . O27 O 0.7221(3) 0.5192(2) 1.03778(19) 0.0531(10) Uani 1 1 d . . . O28 O 0.8090(3) 0.6333(2) 1.0731(2) 0.0615(11) Uani 1 1 d . . . O29 O 0.8353(3) 0.5403(3) 1.0093(2) 0.0664(12) Uani 1 1 d . . . O30 O 0.3123(3) -0.7635(3) 0.8612(3) 0.0805(15) Uani 1 1 d . . . O31 O 0.4283(4) -0.7949(6) 0.8639(4) 0.193(5) Uani 1 1 d D . . O32 O 0.3277(6) -0.8699(6) 0.8062(6) 0.355(13) Uani 1 1 d D . . O33 O 0.8516(5) -0.1365(5) 1.0404(3) 0.140(4) Uani 1 1 d . . . O34 O 0.9431(4) -0.0895(5) 0.9993(3) 0.130(3) Uani 1 1 d D . . O35 O 0.9354(5) -0.2011(5) 1.0097(3) 0.139(3) Uani 1 1 d D . . O1W O 0.6781(2) -0.02487(19) 0.89467(16) 0.0414(8) Uani 1 1 d . . . O2W O 0.8601(2) -0.1175(2) 0.79133(15) 0.0391(8) Uani 1 1 d . . . O3W O 0.5939(2) -0.1555(2) 0.79627(15) 0.0406(8) Uani 1 1 d . . . O4W O 0.8646(2) -0.0443(2) 0.91076(15) 0.0469(9) Uani 1 1 d . . . O5W O 1.0181(3) 0.2100(2) 0.57509(18) 0.0543(10) Uani 1 1 d . . . O6W O 0.3571(3) -0.5985(2) 0.8805(2) 0.0663(13) Uani 1 1 d . . . O7W O 0.5084(2) -0.6384(2) 0.8619(2) 0.0596(11) Uani 1 1 d . . . O8W O 0.8491(3) 0.1365(3) 0.50624(19) 0.0598(11) Uani 1 1 d . . . O9W O 0.3690(4) -0.6719(3) 0.7689(2) 0.0831(17) Uani 1 1 d . . . O10W O 0.8931(4) 0.2722(3) 0.6072(3) 0.097(2) Uani 1 1 d . . . Eu1 Eu 0.907163(15) 0.140621(14) 0.608812(11) 0.03307(8) Uani 1 1 d . . . Eu2 Eu 0.453584(15) -0.537943(13) 0.831361(11) 0.03262(8) Uani 1 1 d . . . Eu3 Eu 0.740896(14) -0.107529(12) 0.828757(9) 0.02381(8) Uani 1 1 d . . . Cl1 Cl 0.88399(9) 0.04849(8) 0.67769(6) 0.0482(3) Uani 1 1 d . . . Cl2 Cl 0.51392(9) -0.39410(8) 0.82242(6) 0.0493(3) Uani 1 1 d . . . C1 C 0.7027(3) 0.0414(3) 0.5943(2) 0.0311(10) Uani 1 1 d . . . C2 C 0.6236(3) -0.0762(3) 0.5974(2) 0.0309(10) Uani 1 1 d . . . H2 H 0.5698 -0.1095 0.5698 0.037 Uiso 1 1 calc R . . C3 C 0.6110(3) -0.0073(3) 0.64498(19) 0.0316(10) Uani 1 1 d . . . H3 H 0.5513 -0.0069 0.6393 0.038 Uiso 1 1 calc R . . C4 C 0.6712(3) -0.0854(3) 0.69019(19) 0.0274(9) Uani 1 1 d . . . C5 C 0.6698(3) 0.1401(3) 0.6705(2) 0.0339(11) Uani 1 1 d . . . H5A H 0.6161 0.1436 0.6797 0.041 Uiso 1 1 calc R . . H5B H 0.6812 0.1730 0.6461 0.041 Uiso 1 1 calc R . . C6 C 0.6384(3) 0.0262(3) 0.75671(19) 0.0296(10) Uani 1 1 d . . . H6A H 0.6301 -0.0076 0.7808 0.036 Uiso 1 1 calc R . . H6B H 0.5894 0.0470 0.7517 0.036 Uiso 1 1 calc R . . C7 C 0.8147(3) 0.2065(3) 0.7262(2) 0.0319(10) Uani 1 1 d . . . C8 C 0.7260(3) 0.1679(3) 0.7815(2) 0.0328(10) Uani 1 1 d . . . H8 H 0.6830 0.1938 0.7937 0.039 Uiso 1 1 calc R . . C9 C 0.8137(3) 0.2106(3) 0.8225(2) 0.0295(10) Uani 1 1 d . . . H9 H 0.8126 0.2556 0.8553 0.035 Uiso 1 1 calc R . . C10 C 0.7816(3) 0.0823(2) 0.82094(18) 0.0257(9) Uani 1 1 d . . . C11 C 0.9468(3) 0.2805(3) 0.7983(2) 0.0373(11) Uani 1 1 d . . . H11A H 0.9590 0.3173 0.8382 0.045 Uiso 1 1 calc R . . H11B H 0.9537 0.3112 0.7719 0.045 Uiso 1 1 calc R . . C12 C 0.9196(3) 0.1620(3) 0.88384(19) 0.0329(10) Uani 1 1 d . . . H12A H 0.9113 0.1259 0.9062 0.039 Uiso 1 1 calc R . . H12B H 0.9365 0.2152 0.9117 0.039 Uiso 1 1 calc R . . C13 C 1.0368(3) 0.2114(3) 0.7486(2) 0.0364(11) Uani 1 1 d . . . C14 C 1.0430(3) 0.2123(3) 0.8452(2) 0.0378(11) Uani 1 1 d . . . H14 H 1.0700 0.2573 0.8814 0.045 Uiso 1 1 calc R . . C15 C 1.1075(3) 0.1710(3) 0.8205(2) 0.0416(12) Uani 1 1 d . . . H15 H 1.1655 0.1968 0.8450 0.050 Uiso 1 1 calc R . . C16 C 1.0105(3) 0.0819(3) 0.8445(2) 0.0352(11) Uani 1 1 d . . . C17 C 1.1472(3) 0.1498(3) 0.7219(2) 0.0432(13) Uani 1 1 d . . . H17A H 1.1489 0.1809 0.6955 0.052 Uiso 1 1 calc R . . H17B H 1.2048 0.1591 0.7444 0.052 Uiso 1 1 calc R . . C18 C 1.1243(3) 0.0328(4) 0.8088(2) 0.0501(14) Uani 1 1 d . . . H18A H 1.1845 0.0587 0.8210 0.060 Uiso 1 1 calc R . . H18B H 1.1133 -0.0010 0.8325 0.060 Uiso 1 1 calc R . . C19 C 1.0627(3) 0.0453(3) 0.6328(2) 0.0379(12) Uani 1 1 d . . . C20 C 1.1380(3) 0.0037(3) 0.7025(2) 0.0440(13) Uani 1 1 d . . . H20 H 1.1994 0.0106 0.7111 0.053 Uiso 1 1 calc R . . C21 C 1.0909(3) -0.0671(3) 0.6463(2) 0.0426(13) Uani 1 1 d . . . H21A H 1.1301 -0.0943 0.6291 0.051 Uiso 1 1 calc R . . C22 C 1.0440(3) -0.0853(3) 0.7278(2) 0.0414(13) Uani 1 1 d . . . C23 C 1.0008(3) -0.0745(3) 0.5485(2) 0.0405(12) Uani 1 1 d . . . H23A H 1.0216 -0.1197 0.5324 0.049 Uiso 1 1 calc R . . H23B H 1.0080 -0.0408 0.5242 0.049 Uiso 1 1 calc R . . C24 C 0.9761(3) -0.1908(3) 0.6331(2) 0.0422(13) Uani 1 1 d . . . H24A H 1.0006 -0.2172 0.6025 0.051 Uiso 1 1 calc R . . H24B H 0.9684 -0.2232 0.6583 0.051 Uiso 1 1 calc R . . C25 C 0.8576(3) -0.0577(3) 0.53845(19) 0.0323(10) Uani 1 1 d . . . C26 C 0.8720(3) -0.1764(3) 0.5481(2) 0.0361(11) Uani 1 1 d . . . H26 H 0.8795 -0.2199 0.5169 0.043 Uiso 1 1 calc R . . C27 C 0.7795(3) -0.1770(3) 0.5402(2) 0.0367(11) Uani 1 1 d . . . H27 H 0.7435 -0.2202 0.5051 0.044 Uiso 1 1 calc R . . C28 C 0.8282(3) -0.1943(3) 0.6296(2) 0.0383(12) Uani 1 1 d . . . C29 C 0.7055(3) -0.0763(3) 0.51809(19) 0.0342(11) Uani 1 1 d . . . H29A H 0.6601 -0.1218 0.4925 0.041 Uiso 1 1 calc R . . H29B H 0.7168 -0.0404 0.4958 0.041 Uiso 1 1 calc R . . C30 C 0.6794(3) -0.1916(3) 0.6064(2) 0.0348(11) Uani 1 1 d . . . H30A H 0.6358 -0.2208 0.5700 0.042 Uiso 1 1 calc R . . H30B H 0.6750 -0.2216 0.6335 0.042 Uiso 1 1 calc R . . C31 C 0.6359(3) -0.5088(3) 0.7827(2) 0.0352(11) Uani 1 1 d . . . C32 C 0.7048(4) -0.4428(3) 0.7290(2) 0.0399(12) Uani 1 1 d . . . H32 H 0.7358 -0.4625 0.6998 0.048 Uiso 1 1 calc R . . C33 C 0.7600(3) -0.4163(3) 0.7937(2) 0.0360(11) Uani 1 1 d . . . H33 H 0.8152 -0.4278 0.7953 0.043 Uiso 1 1 calc R . . C34 C 0.7238(3) -0.3098(3) 0.7731(2) 0.0318(10) Uani 1 1 d . . . C35 C 0.7329(3) -0.4589(3) 0.8819(2) 0.0377(11) Uani 1 1 d . . . H35A H 0.7084 -0.5105 0.8839 0.045 Uiso 1 1 calc R . . H35B H 0.7940 -0.4483 0.8940 0.045 Uiso 1 1 calc R . . C36 C 0.8148(3) -0.2809(3) 0.8724(2) 0.0331(10) Uani 1 1 d . . . H36A H 0.8619 -0.3005 0.8860 0.040 Uiso 1 1 calc R . . H36B H 0.8380 -0.2291 0.8702 0.040 Uiso 1 1 calc R . . C37 C 0.6326(3) -0.4175(3) 0.9371(2) 0.0312(10) Uani 1 1 d . . . C38 C 0.7559(3) -0.3208(3) 0.9532(2) 0.0330(10) Uani 1 1 d . . . H38 H 0.8108 -0.3175 0.9779 0.040 Uiso 1 1 calc R . . C39 C 0.6996(3) -0.2866(3) 0.9903(2) 0.0315(10) Uani 1 1 d . . . H39 H 0.7292 -0.2629 1.0324 0.038 Uiso 1 1 calc R . . C40 C 0.7205(3) -0.2191(3) 0.9246(2) 0.0281(10) Uani 1 1 d . . . C41 C 0.5594(3) -0.3502(3) 1.0067(2) 0.0343(11) Uani 1 1 d . . . H41A H 0.5358 -0.4024 1.0082 0.041 Uiso 1 1 calc R . . H41B H 0.5799 -0.3144 1.0472 0.041 Uiso 1 1 calc R . . C42 C 0.6333(3) -0.1723(3) 0.9899(2) 0.0311(10) Uani 1 1 d . . . H42A H 0.6455 -0.1617 1.0324 0.037 Uiso 1 1 calc R . . H42B H 0.6545 -0.1232 0.9830 0.037 Uiso 1 1 calc R . . C43 C 0.4274(3) -0.3782(3) 0.9349(2) 0.0320(10) Uani 1 1 d . . . C44 C 0.4870(3) -0.2470(3) 0.9881(2) 0.0362(11) Uani 1 1 d . . . H44 H 0.4897 -0.2218 1.0299 0.043 Uiso 1 1 calc R . . C45 C 0.3999(3) -0.2578(3) 0.9471(2) 0.0374(11) Uani 1 1 d . . . H45 H 0.3619 -0.2364 0.9697 0.045 Uiso 1 1 calc R . . C46 C 0.5039(3) -0.1803(3) 0.9200(2) 0.0317(10) Uani 1 1 d . . . C47 C 0.2890(3) -0.3825(3) 0.8796(2) 0.0384(12) Uani 1 1 d . . . H47A H 0.2477 -0.3546 0.8908 0.046 Uiso 1 1 calc R . . H47B H 0.2718 -0.4344 0.8832 0.046 Uiso 1 1 calc R . . C48 C 0.3584(3) -0.2031(3) 0.8640(2) 0.0426(13) Uani 1 1 d . . . H48A H 0.3082 -0.2000 0.8785 0.051 Uiso 1 1 calc R . . H48B H 0.3813 -0.1528 0.8592 0.051 Uiso 1 1 calc R . . C49 C 0.3018(3) -0.4530(3) 0.7825(2) 0.0383(12) Uani 1 1 d . . . C50 C 0.2683(3) -0.3353(3) 0.7902(3) 0.0432(13) Uani 1 1 d . . . H50 H 0.2134 -0.3255 0.7934 0.052 Uiso 1 1 calc R . . C51 C 0.2688(3) -0.3751(3) 0.7259(3) 0.0447(13) Uani 1 1 d . . . H51 H 0.2136 -0.3847 0.6989 0.054 Uiso 1 1 calc R . . C52 C 0.3684(3) -0.2547(3) 0.7620(2) 0.0395(12) Uani 1 1 d . . . C53 C 0.2931(3) -0.5065(3) 0.6765(2) 0.0450(13) Uani 1 1 d . . . H53A H 0.2537 -0.5061 0.6419 0.054 Uiso 1 1 calc R . . H53B H 0.2760 -0.5579 0.6810 0.054 Uiso 1 1 calc R . . C54 C 0.3564(3) -0.3303(3) 0.6592(2) 0.0450(13) Uani 1 1 d . . . H54A H 0.3065 -0.3598 0.6271 0.054 Uiso 1 1 calc R . . H54B H 0.3753 -0.2788 0.6552 0.054 Uiso 1 1 calc R . . C55 C 0.4341(4) -0.5283(3) 0.6887(2) 0.0417(12) Uani 1 1 d . . . C56 C 0.4065(4) -0.4534(3) 0.6291(2) 0.0447(13) Uani 1 1 d . . . H56 H 0.3703 -0.4747 0.5886 0.054 Uiso 1 1 calc R . . C57 C 0.4956(4) -0.4648(3) 0.6312(2) 0.0405(12) Uani 1 1 d . . . H57 H 0.5029 -0.4886 0.5916 0.049 Uiso 1 1 calc R . . C58 C 0.5035(4) -0.3320(3) 0.6682(2) 0.0389(12) Uani 1 1 d . . . C59 C 0.5689(4) -0.5503(3) 0.6774(2) 0.0441(13) Uani 1 1 d . . . H59A H 0.5925 -0.5598 0.6431 0.053 Uiso 1 1 calc R . . H59B H 0.5463 -0.6010 0.6817 0.053 Uiso 1 1 calc R . . C60 C 0.6388(4) -0.3643(3) 0.6707(2) 0.0413(12) Uani 1 1 d . . . H60A H 0.6574 -0.3101 0.6720 0.050 Uiso 1 1 calc R . . H60B H 0.6545 -0.3969 0.6376 0.050 Uiso 1 1 calc R . . N1 N 0.6781(2) -0.0377(2) 0.56855(16) 0.0319(9) Uani 1 1 d . . . N2 N 0.6622(2) 0.0608(2) 0.63716(17) 0.0298(8) Uani 1 1 d . . . N3 N 0.6633(2) -0.1181(2) 0.63174(15) 0.0289(8) Uani 1 1 d . . . N4 N 0.6431(2) -0.0202(2) 0.69982(16) 0.0293(8) Uani 1 1 d . . . N5 N 0.7353(2) 0.1704(2) 0.72475(17) 0.0309(9) Uani 1 1 d . . . N6 N 0.8612(3) 0.2352(2) 0.78220(17) 0.0338(9) Uani 1 1 d . . . N7 N 0.7126(2) 0.0907(2) 0.78757(16) 0.0281(8) Uani 1 1 d . . . N8 N 0.8405(2) 0.1508(2) 0.84281(16) 0.0304(8) Uani 1 1 d . . . N9 N 1.0071(3) 0.2355(2) 0.79651(18) 0.0387(10) Uani 1 1 d . . . N10 N 1.0979(3) 0.1764(3) 0.76220(19) 0.0405(10) Uani 1 1 d . . . N11 N 0.9868(3) 0.1497(2) 0.85538(18) 0.0362(9) Uani 1 1 d . . . N12 N 1.0789(2) 0.0918(3) 0.82133(18) 0.0383(10) Uani 1 1 d . . . N13 N 1.1157(3) 0.0684(3) 0.6872(2) 0.0424(10) Uani 1 1 d . . . N14 N 1.0500(3) -0.0324(2) 0.60708(19) 0.0385(10) Uani 1 1 d . . . N15 N 1.1035(3) -0.0148(3) 0.74859(19) 0.0422(11) Uani 1 1 d . . . N16 N 1.0346(3) -0.1165(3) 0.6680(2) 0.0448(11) Uani 1 1 d . . . N17 N 0.9127(3) -0.1014(2) 0.54455(18) 0.0372(10) Uani 1 1 d . . . N18 N 0.7796(3) -0.1012(2) 0.53371(17) 0.0351(9) Uani 1 1 d . . . N19 N 0.8949(3) -0.1856(3) 0.60564(18) 0.0401(10) Uani 1 1 d . . . N20 N 0.7611(3) -0.1860(2) 0.59311(17) 0.0354(9) Uani 1 1 d . . . N21 N 0.6353(3) -0.5038(2) 0.72888(19) 0.0378(10) Uani 1 1 d . . . N22 N 0.7089(3) -0.4604(2) 0.82155(18) 0.0328(9) Uani 1 1 d . . . N23 N 0.6839(3) -0.3717(2) 0.72472(17) 0.0327(9) Uani 1 1 d . . . N24 N 0.7679(2) -0.3329(2) 0.81379(17) 0.0317(9) Uani 1 1 d . . . N25 N 0.7069(2) -0.4014(2) 0.92280(18) 0.0315(9) Uani 1 1 d . . . N26 N 0.6297(2) -0.3520(2) 0.97998(17) 0.0306(8) Uani 1 1 d . . . N27 N 0.7649(2) -0.2736(2) 0.91469(17) 0.0297(8) Uani 1 1 d . . . N28 N 0.6782(2) -0.2281(2) 0.96481(16) 0.0287(8) Uani 1 1 d . . . N29 N 0.4937(3) -0.3260(2) 0.97602(18) 0.0343(9) Uani 1 1 d . . . N30 N 0.3693(3) -0.3413(2) 0.91992(18) 0.0349(9) Uani 1 1 d . . . N31 N 0.5436(2) -0.1986(2) 0.96620(17) 0.0313(9) Uani 1 1 d . . . N32 N 0.4200(3) -0.2157(2) 0.90767(19) 0.0361(9) Uani 1 1 d . . . N33 N 0.2875(3) -0.3913(2) 0.8189(2) 0.0406(10) Uani 1 1 d . . . N34 N 0.2876(3) -0.4483(3) 0.72715(19) 0.0426(10) Uani 1 1 d . . . N35 N 0.3343(3) -0.2630(2) 0.8073(2) 0.0391(10) Uani 1 1 d . . . N36 N 0.3332(3) -0.3202(3) 0.7148(2) 0.0416(10) Uani 1 1 d . . . N37 N 0.3759(3) -0.4952(3) 0.6665(2) 0.0446(11) Uani 1 1 d . . . N38 N 0.5012(3) -0.5153(2) 0.66675(19) 0.0422(10) Uani 1 1 d . . . N39 N 0.4213(3) -0.3698(2) 0.65292(19) 0.0431(10) Uani 1 1 d . . . N40 N 0.5498(3) -0.3857(3) 0.65974(18) 0.0412(10) Uani 1 1 d . . . O1 O 0.7514(2) 0.08676(19) 0.57957(14) 0.0339(7) Uani 1 1 d . . . O2 O 0.8398(2) 0.21543(19) 0.68334(14) 0.0332(7) Uani 1 1 d . . . O3 O 1.0139(2) 0.2214(2) 0.70023(15) 0.0392(8) Uani 1 1 d . . . O4 O 1.0337(2) 0.0890(2) 0.60969(16) 0.0412(8) Uani 1 1 d . . . O5 O 0.8742(2) 0.0081(2) 0.53438(14) 0.0374(8) Uani 1 1 d . . . O6 O 0.6982(2) -0.11280(18) 0.72810(13) 0.0298(7) Uani 1 1 d . . . O7 O 0.78882(19) 0.02196(17) 0.83077(13) 0.0287(7) Uani 1 1 d . . . O8 O 0.9793(2) 0.0238(2) 0.85522(14) 0.0383(8) Uani 1 1 d . . . O9 O 1.0074(2) -0.1168(2) 0.75703(17) 0.0477(9) Uani 1 1 d . . . O10 O 0.8263(2) -0.2100(2) 0.67532(15) 0.0408(8) Uani 1 1 d . . . O11 O 0.5821(2) -0.55267(19) 0.79584(15) 0.0383(8) Uani 1 1 d . . . O12 O 0.5789(2) -0.48011(18) 0.91769(15) 0.0342(7) Uani 1 1 d . . . O13 O 0.4187(2) -0.44906(19) 0.91595(15) 0.0374(8) Uani 1 1 d . . . O14 O 0.3215(2) -0.50853(19) 0.79559(16) 0.0405(8) Uani 1 1 d . . . O15 O 0.4245(2) -0.5672(2) 0.72234(16) 0.0429(8) Uani 1 1 d . . . O16 O 0.7222(2) -0.24171(18) 0.77856(14) 0.0344(7) Uani 1 1 d . . . O17 O 0.7208(2) -0.16890(18) 0.90035(14) 0.0314(7) Uani 1 1 d . . . O18 O 0.5366(2) -0.13746(18) 0.89568(14) 0.0336(7) Uani 1 1 d . . . O19 O 0.4203(2) -0.1976(2) 0.76348(16) 0.0433(9) Uani 1 1 d . . . O20 O 0.5349(2) -0.2612(2) 0.68566(15) 0.0404(8) Uani 1 1 d . . . C61 C 0.7465(4) 0.1935(3) 0.9563(2) 0.0430(13) Uani 1 1 d . . . C62 C 0.6731(4) 0.1845(3) 0.9173(2) 0.0421(12) Uani 1 1 d . . . H62 H 0.6413 0.1340 0.8934 0.051 Uiso 1 1 calc R . . C63 C 0.6443(4) 0.2481(3) 0.9121(2) 0.0439(12) Uani 1 1 d . . . H63 H 0.5940 0.2412 0.8848 0.053 Uiso 1 1 calc R . . C64 C 0.6920(3) 0.3229(3) 0.9486(2) 0.0409(12) Uani 1 1 d . . . C65 C 0.7660(3) 0.3317(3) 0.9867(2) 0.0403(12) Uani 1 1 d . . . H65 H 0.7985 0.3820 1.0103 0.048 Uiso 1 1 calc R . . C66 C 0.7937(3) 0.2677(3) 0.9909(2) 0.0437(12) Uani 1 1 d . . . H66 H 0.8447 0.2747 1.0174 0.052 Uiso 1 1 calc R . . C67 C 0.5335(7) 0.0793(7) 0.5228(5) 0.096(3) Uani 1 1 d . . . C68 C 0.5582(6) 0.0383(8) 0.4779(5) 0.096(3) Uani 1 1 d . . . H68 H 0.5977 0.0639 0.4621 0.116 Uiso 1 1 calc R . . C69 C 0.5250(7) -0.0436(8) 0.4540(4) 0.103(3) Uani 1 1 d . . . H69 H 0.5427 -0.0729 0.4228 0.124 Uiso 1 1 calc R . . C70 C 0.7585(5) -0.6306(4) 0.7596(4) 0.080(2) Uani 1 1 d D . . C71 C 0.6974(6) -0.6648(4) 0.7074(5) 0.108(4) Uani 1 1 d D . . H71 H 0.6455 -0.6971 0.7057 0.129 Uiso 1 1 calc R . . C72 C 0.7142(7) -0.6504(5) 0.6577(5) 0.115(4) Uani 1 1 d D . . H72 H 0.6727 -0.6734 0.6221 0.139 Uiso 1 1 calc R . . C73 C 0.7897(6) -0.6035(6) 0.6582(4) 0.105(3) Uani 1 1 d D . . C74 C 0.8498(6) -0.5683(6) 0.7108(4) 0.105(3) Uani 1 1 d D . . H74 H 0.9007 -0.5343 0.7128 0.126 Uiso 1 1 calc R . . C75 C 0.8342(5) -0.5837(4) 0.7605(4) 0.084(2) Uani 1 1 d D . . H75 H 0.8762 -0.5616 0.7959 0.101 Uiso 1 1 calc R . . O21 O 0.7689(3) 0.1271(2) 0.95885(18) 0.0535(10) Uani 1 1 d . . . H21 H 0.8140 0.1391 0.9839 0.080 Uiso 1 1 calc R . . O22 O 0.6618(3) 0.3851(2) 0.94448(18) 0.0555(10) Uani 1 1 d . . . H22 H 0.6169 0.3693 0.9188 0.083 Uiso 1 1 calc R . . O23 O 0.5641(6) 0.1615(6) 0.5478(4) 0.152(3) Uani 1 1 d . . . H23 H 0.5412 0.1773 0.5745 0.228 Uiso 1 1 calc R . . O24 O 0.7421(4) -0.6441(3) 0.8090(4) 0.108(2) Uani 1 1 d . . . H24 H 0.7833 -0.6201 0.8373 0.162 Uiso 1 1 calc R . . O25 O 0.8015(8) -0.5886(6) 0.6069(4) 0.178(4) Uani 1 1 d . . . H25 H 0.8483 -0.5579 0.6140 0.268 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl3 0.123(5) 0.256(9) 0.115(5) 0.078(5) 0.044(4) -0.006(5) Cl4 0.408(18) 0.288(13) 0.235(11) 0.195(11) 0.166(12) 0.196(13) Cl5 0.253(12) 0.354(16) 0.243(11) 0.107(11) 0.136(10) 0.203(12) Cl6 0.39(2) 0.311(16) 0.139(8) 0.058(9) 0.035(10) 0.117(14) Cl7 0.176(6) 0.124(5) 0.144(5) 0.054(4) 0.059(5) 0.063(4) Cl8 0.098(4) 0.217(7) 0.129(4) 0.115(5) -0.005(3) 0.033(4) Cl9 0.106(7) 0.308(17) 0.94(5) 0.14(2) -0.066(15) -0.157(10) Cl10 0.244(13) 0.323(17) 0.258(14) 0.071(13) 0.059(11) 0.043(12) N41 0.041(3) 0.040(3) 0.052(3) 0.022(2) 0.008(2) 0.007(2) N42 0.039(3) 0.053(3) 0.043(3) 0.006(2) -0.006(2) -0.006(2) N43 0.084(6) 0.119(7) 0.071(5) 0.060(5) -0.044(4) -0.041(5) O27 0.049(2) 0.036(2) 0.070(3) 0.0143(19) 0.020(2) 0.0001(18) O28 0.063(3) 0.035(2) 0.070(3) 0.006(2) 0.015(2) -0.006(2) O29 0.062(3) 0.066(3) 0.077(3) 0.018(2) 0.032(2) 0.023(2) O30 0.052(3) 0.058(3) 0.118(4) 0.021(3) 0.011(3) 0.006(2) O31 0.146(7) 0.215(10) 0.146(7) -0.054(7) -0.044(6) 0.121(7) O32 0.155(9) 0.47(2) 0.244(13) -0.175(16) -0.076(9) 0.189(13) O33 0.078(4) 0.207(9) 0.060(4) 0.005(4) -0.002(3) -0.055(5) O34 0.118(5) 0.162(7) 0.117(5) 0.098(5) 0.000(4) 0.001(5) O35 0.097(5) 0.155(8) 0.133(6) 0.075(6) -0.038(4) -0.010(5) O1W 0.047(2) 0.0288(18) 0.051(2) 0.0105(16) 0.0262(17) 0.0075(16) O2W 0.0363(19) 0.041(2) 0.0414(19) 0.0123(16) 0.0144(15) 0.0111(16) O3W 0.0339(19) 0.050(2) 0.0350(19) 0.0127(16) 0.0096(15) 0.0063(16) O4W 0.043(2) 0.058(2) 0.0348(19) 0.0229(18) 0.0004(16) -0.0003(18) O5W 0.060(3) 0.054(2) 0.061(3) 0.031(2) 0.030(2) 0.012(2) O6W 0.089(3) 0.038(2) 0.099(3) 0.037(2) 0.058(3) 0.024(2) O7W 0.045(2) 0.045(2) 0.102(3) 0.045(2) 0.019(2) 0.0138(19) O8W 0.056(3) 0.084(3) 0.061(3) 0.053(2) 0.019(2) 0.023(2) O9W 0.124(4) 0.040(2) 0.057(3) 0.017(2) -0.002(3) -0.020(3) O10W 0.171(6) 0.079(4) 0.115(4) 0.073(3) 0.102(4) 0.080(4) Eu1 0.03679(15) 0.03651(15) 0.03637(15) 0.02106(11) 0.01536(11) 0.01417(11) Eu2 0.03440(15) 0.02423(14) 0.04142(15) 0.01462(11) 0.01097(11) 0.00582(10) Eu3 0.02972(14) 0.02055(13) 0.02324(12) 0.01025(9) 0.00774(9) 0.00592(9) Cl1 0.0483(8) 0.0501(8) 0.0488(8) 0.0222(6) 0.0082(6) 0.0139(6) Cl2 0.0544(8) 0.0419(8) 0.0539(8) 0.0180(6) 0.0162(7) 0.0121(6) C1 0.027(2) 0.044(3) 0.029(2) 0.022(2) 0.0035(19) 0.013(2) C2 0.026(2) 0.036(3) 0.027(2) 0.013(2) -0.0012(18) 0.005(2) C3 0.026(2) 0.042(3) 0.028(2) 0.017(2) 0.0020(19) 0.010(2) C4 0.021(2) 0.028(2) 0.031(2) 0.0095(19) 0.0072(18) 0.0014(18) C5 0.030(3) 0.040(3) 0.041(3) 0.024(2) 0.009(2) 0.015(2) C6 0.029(2) 0.034(3) 0.029(2) 0.013(2) 0.0099(19) 0.008(2) C7 0.044(3) 0.023(2) 0.036(3) 0.013(2) 0.014(2) 0.015(2) C8 0.045(3) 0.023(2) 0.039(3) 0.016(2) 0.019(2) 0.014(2) C9 0.042(3) 0.018(2) 0.031(2) 0.0082(18) 0.014(2) 0.008(2) C10 0.030(2) 0.025(2) 0.024(2) 0.0098(18) 0.0109(18) 0.0056(19) C11 0.043(3) 0.026(3) 0.037(3) 0.006(2) 0.013(2) 0.000(2) C12 0.037(3) 0.033(3) 0.023(2) 0.0061(19) 0.0065(19) 0.001(2) C13 0.029(3) 0.032(3) 0.045(3) 0.013(2) 0.011(2) -0.002(2) C14 0.030(3) 0.036(3) 0.035(3) 0.010(2) 0.001(2) -0.009(2) C15 0.027(3) 0.053(3) 0.034(3) 0.010(2) 0.001(2) 0.000(2) C16 0.027(3) 0.046(3) 0.025(2) 0.010(2) -0.0033(19) 0.003(2) C17 0.022(3) 0.059(4) 0.051(3) 0.026(3) 0.010(2) 0.004(2) C18 0.036(3) 0.076(4) 0.049(3) 0.036(3) 0.006(2) 0.021(3) C19 0.030(3) 0.051(3) 0.048(3) 0.029(3) 0.020(2) 0.016(2) C20 0.032(3) 0.064(4) 0.053(3) 0.035(3) 0.018(2) 0.021(3) C21 0.041(3) 0.059(4) 0.051(3) 0.032(3) 0.027(3) 0.031(3) C22 0.040(3) 0.058(4) 0.053(3) 0.036(3) 0.023(3) 0.034(3) C23 0.053(3) 0.049(3) 0.041(3) 0.025(3) 0.029(3) 0.031(3) C24 0.055(3) 0.039(3) 0.050(3) 0.022(3) 0.024(3) 0.030(3) C25 0.039(3) 0.037(3) 0.024(2) 0.012(2) 0.009(2) 0.014(2) C26 0.053(3) 0.032(3) 0.029(2) 0.010(2) 0.017(2) 0.018(2) C27 0.055(3) 0.025(2) 0.027(2) 0.0047(19) 0.010(2) 0.009(2) C28 0.049(3) 0.030(3) 0.040(3) 0.010(2) 0.017(2) 0.016(2) C29 0.037(3) 0.043(3) 0.023(2) 0.014(2) 0.0036(19) 0.010(2) C30 0.038(3) 0.032(3) 0.031(2) 0.009(2) 0.007(2) 0.004(2) C31 0.044(3) 0.020(2) 0.050(3) 0.014(2) 0.020(2) 0.015(2) C32 0.056(3) 0.023(2) 0.049(3) 0.011(2) 0.029(3) 0.018(2) C33 0.039(3) 0.029(3) 0.050(3) 0.016(2) 0.025(2) 0.015(2) C34 0.037(3) 0.029(3) 0.038(3) 0.013(2) 0.023(2) 0.014(2) C35 0.038(3) 0.030(3) 0.055(3) 0.024(2) 0.016(2) 0.013(2) C36 0.029(2) 0.032(3) 0.044(3) 0.018(2) 0.015(2) 0.008(2) C37 0.037(3) 0.030(3) 0.032(2) 0.018(2) 0.005(2) 0.013(2) C38 0.030(3) 0.031(3) 0.037(3) 0.017(2) 0.001(2) 0.004(2) C39 0.034(3) 0.033(3) 0.028(2) 0.015(2) 0.0033(19) 0.006(2) C40 0.028(2) 0.021(2) 0.031(2) 0.0090(19) 0.0009(19) 0.0031(19) C41 0.041(3) 0.034(3) 0.031(2) 0.019(2) 0.012(2) 0.004(2) C42 0.043(3) 0.021(2) 0.028(2) 0.0049(19) 0.014(2) 0.005(2) C43 0.039(3) 0.026(3) 0.037(3) 0.015(2) 0.019(2) 0.006(2) C44 0.044(3) 0.029(3) 0.038(3) 0.009(2) 0.022(2) 0.009(2) C45 0.039(3) 0.030(3) 0.050(3) 0.012(2) 0.024(2) 0.012(2) C46 0.036(3) 0.025(2) 0.033(3) 0.002(2) 0.016(2) 0.011(2) C47 0.028(3) 0.041(3) 0.052(3) 0.021(2) 0.018(2) 0.007(2) C48 0.035(3) 0.037(3) 0.063(4) 0.018(3) 0.015(2) 0.019(2) C49 0.029(3) 0.033(3) 0.051(3) 0.018(2) 0.007(2) 0.003(2) C50 0.024(3) 0.044(3) 0.067(4) 0.028(3) 0.008(2) 0.011(2) C51 0.033(3) 0.044(3) 0.059(3) 0.029(3) 0.002(2) 0.007(2) C52 0.030(3) 0.041(3) 0.052(3) 0.023(3) 0.004(2) 0.015(2) C53 0.048(3) 0.035(3) 0.044(3) 0.015(2) 0.004(2) -0.002(2) C54 0.044(3) 0.047(3) 0.046(3) 0.026(3) 0.004(2) 0.008(3) C55 0.055(3) 0.023(3) 0.037(3) 0.003(2) 0.010(2) -0.002(2) C56 0.054(3) 0.036(3) 0.032(3) 0.009(2) 0.000(2) -0.001(2) C57 0.058(3) 0.030(3) 0.027(2) 0.004(2) 0.012(2) 0.004(2) C58 0.057(3) 0.036(3) 0.024(2) 0.012(2) 0.007(2) 0.012(3) C59 0.062(4) 0.024(3) 0.043(3) 0.005(2) 0.021(3) 0.006(2) C60 0.061(4) 0.032(3) 0.035(3) 0.012(2) 0.020(2) 0.011(2) N1 0.033(2) 0.037(2) 0.027(2) 0.0151(17) 0.0054(16) 0.0072(18) N2 0.030(2) 0.032(2) 0.034(2) 0.0170(17) 0.0099(17) 0.0125(17) N3 0.030(2) 0.033(2) 0.0229(19) 0.0111(16) 0.0025(15) 0.0072(17) N4 0.031(2) 0.031(2) 0.029(2) 0.0155(17) 0.0044(16) 0.0085(17) N5 0.036(2) 0.031(2) 0.035(2) 0.0162(17) 0.0173(17) 0.0134(18) N6 0.041(2) 0.028(2) 0.035(2) 0.0150(18) 0.0138(18) 0.0053(18) N7 0.028(2) 0.026(2) 0.033(2) 0.0137(16) 0.0074(16) 0.0067(16) N8 0.037(2) 0.023(2) 0.031(2) 0.0101(16) 0.0071(17) 0.0045(17) N9 0.037(2) 0.038(2) 0.036(2) 0.0124(19) 0.0059(18) 0.0005(19) N10 0.033(2) 0.053(3) 0.040(2) 0.024(2) 0.0122(19) 0.009(2) N11 0.034(2) 0.034(2) 0.035(2) 0.0106(18) 0.0067(18) -0.0008(18) N12 0.027(2) 0.054(3) 0.038(2) 0.023(2) 0.0087(18) 0.0078(19) N13 0.029(2) 0.049(3) 0.056(3) 0.027(2) 0.011(2) 0.010(2) N14 0.038(2) 0.041(3) 0.049(3) 0.023(2) 0.016(2) 0.020(2) N15 0.036(2) 0.064(3) 0.046(3) 0.034(2) 0.019(2) 0.026(2) N16 0.046(3) 0.053(3) 0.055(3) 0.034(2) 0.023(2) 0.025(2) N17 0.050(3) 0.037(2) 0.035(2) 0.0186(19) 0.0165(19) 0.020(2) N18 0.044(2) 0.036(2) 0.030(2) 0.0158(18) 0.0108(18) 0.0128(19) N19 0.053(3) 0.045(3) 0.041(2) 0.023(2) 0.024(2) 0.029(2) N20 0.044(2) 0.036(2) 0.030(2) 0.0143(18) 0.0103(18) 0.0122(19) N21 0.053(3) 0.020(2) 0.043(2) 0.0089(18) 0.022(2) 0.0088(19) N22 0.037(2) 0.025(2) 0.044(2) 0.0179(18) 0.0154(19) 0.0123(18) N23 0.047(2) 0.023(2) 0.032(2) 0.0091(17) 0.0167(18) 0.0115(18) N24 0.037(2) 0.024(2) 0.041(2) 0.0149(17) 0.0157(18) 0.0108(17) N25 0.031(2) 0.024(2) 0.046(2) 0.0177(18) 0.0137(18) 0.0086(17) N26 0.033(2) 0.025(2) 0.033(2) 0.0132(17) 0.0071(17) 0.0032(17) N27 0.032(2) 0.026(2) 0.035(2) 0.0176(17) 0.0096(17) 0.0067(17) N28 0.037(2) 0.027(2) 0.0245(19) 0.0138(16) 0.0078(16) 0.0076(17) N29 0.037(2) 0.025(2) 0.039(2) 0.0094(17) 0.0104(18) 0.0042(18) N30 0.035(2) 0.028(2) 0.044(2) 0.0101(18) 0.0187(19) 0.0082(18) N31 0.038(2) 0.027(2) 0.031(2) 0.0100(17) 0.0151(17) 0.0070(17) N32 0.036(2) 0.032(2) 0.047(2) 0.0183(19) 0.0178(19) 0.0099(18) N33 0.033(2) 0.036(2) 0.056(3) 0.020(2) 0.012(2) 0.0088(19) N34 0.044(3) 0.038(2) 0.043(3) 0.019(2) 0.002(2) 0.006(2) N35 0.035(2) 0.035(2) 0.051(3) 0.019(2) 0.010(2) 0.0099(19) N36 0.036(2) 0.037(2) 0.050(3) 0.019(2) 0.002(2) 0.005(2) N37 0.042(3) 0.042(3) 0.045(3) 0.019(2) 0.003(2) 0.002(2) N38 0.056(3) 0.029(2) 0.043(2) 0.0113(19) 0.018(2) 0.011(2) N39 0.045(3) 0.033(2) 0.043(3) 0.014(2) 0.004(2) -0.003(2) N40 0.048(3) 0.039(2) 0.034(2) 0.0110(19) 0.0109(19) 0.007(2) O1 0.0362(19) 0.0395(19) 0.0349(18) 0.0226(15) 0.0115(15) 0.0128(15) O2 0.0366(19) 0.0349(18) 0.0374(18) 0.0206(15) 0.0161(15) 0.0115(15) O3 0.041(2) 0.042(2) 0.040(2) 0.0215(17) 0.0160(16) 0.0063(16) O4 0.039(2) 0.043(2) 0.052(2) 0.0277(18) 0.0142(16) 0.0140(17) O5 0.044(2) 0.041(2) 0.0369(19) 0.0209(16) 0.0148(15) 0.0173(16) O6 0.0378(18) 0.0294(17) 0.0238(16) 0.0148(13) 0.0055(13) 0.0060(14) O7 0.0320(17) 0.0245(17) 0.0280(16) 0.0109(13) 0.0029(13) 0.0047(13) O8 0.039(2) 0.043(2) 0.0333(18) 0.0168(16) 0.0066(15) 0.0069(16) O9 0.056(2) 0.054(2) 0.054(2) 0.033(2) 0.0270(19) 0.030(2) O10 0.058(2) 0.043(2) 0.0333(19) 0.0209(16) 0.0182(16) 0.0234(18) O11 0.042(2) 0.0275(18) 0.049(2) 0.0163(16) 0.0164(16) 0.0078(15) O12 0.0362(19) 0.0212(17) 0.045(2) 0.0124(15) 0.0104(15) 0.0052(15) O13 0.038(2) 0.0264(19) 0.047(2) 0.0146(15) 0.0110(16) 0.0041(15) O14 0.041(2) 0.0314(19) 0.049(2) 0.0162(16) 0.0100(16) 0.0047(16) O15 0.051(2) 0.0330(19) 0.045(2) 0.0169(17) 0.0127(17) 0.0055(16) O16 0.048(2) 0.0221(17) 0.0374(18) 0.0129(14) 0.0160(15) 0.0093(15) O17 0.0409(19) 0.0270(17) 0.0351(17) 0.0167(14) 0.0174(15) 0.0120(15) O18 0.0370(19) 0.0274(17) 0.0372(18) 0.0118(15) 0.0130(15) 0.0057(14) O19 0.037(2) 0.036(2) 0.057(2) 0.0200(17) 0.0079(17) 0.0068(17) O20 0.051(2) 0.030(2) 0.0358(19) 0.0100(15) 0.0085(16) 0.0067(16) C61 0.056(3) 0.031(3) 0.048(3) 0.014(2) 0.028(3) 0.011(3) C62 0.055(3) 0.031(3) 0.036(3) 0.005(2) 0.021(3) 0.003(2) C63 0.047(3) 0.037(3) 0.043(3) 0.008(2) 0.016(2) 0.006(2) C64 0.047(3) 0.033(3) 0.046(3) 0.015(2) 0.021(3) 0.007(2) C65 0.049(3) 0.032(3) 0.039(3) 0.010(2) 0.017(2) 0.006(2) C66 0.042(3) 0.042(3) 0.049(3) 0.014(3) 0.019(2) 0.009(2) C67 0.088(7) 0.107(8) 0.075(6) 0.035(6) -0.032(5) 0.023(6) C68 0.074(6) 0.138(10) 0.081(6) 0.055(6) -0.015(5) 0.041(6) C69 0.089(7) 0.138(10) 0.079(6) 0.046(7) -0.026(6) 0.048(7) C70 0.098(6) 0.052(4) 0.122(7) 0.037(5) 0.049(6) 0.057(5) C71 0.086(6) 0.041(4) 0.192(12) 0.024(6) 0.024(8) 0.038(4) C72 0.118(10) 0.069(7) 0.147(11) 0.017(6) 0.007(8) 0.046(6) C73 0.133(9) 0.102(8) 0.103(8) 0.032(6) 0.045(7) 0.067(7) C74 0.116(8) 0.111(8) 0.105(8) 0.033(7) 0.029(7) 0.065(7) C75 0.095(6) 0.057(5) 0.110(7) 0.026(5) 0.031(5) 0.041(5) O21 0.064(3) 0.033(2) 0.063(3) 0.0110(18) 0.018(2) 0.0169(19) O22 0.065(3) 0.038(2) 0.061(3) 0.0158(19) 0.005(2) 0.019(2) O23 0.158(7) 0.150(8) 0.119(6) 0.031(5) -0.036(5) 0.056(6) O24 0.128(5) 0.061(3) 0.161(6) 0.035(4) 0.064(5) 0.056(4) O25 0.278(13) 0.179(9) 0.141(7) 0.072(7) 0.092(8) 0.131(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 N41 O28 1.236(6) . ? N41 O29 1.244(6) . ? N41 O27 1.246(6) . ? N42 O30 1.143(7) . ? N42 O32 1.246(2) . ? N42 O31 1.247(2) . ? N43 O33 1.207(10) . ? N43 O34 1.250(2) . ? N43 O35 1.250(2) . ? O1W Eu3 2.441(3) . ? O2W Eu3 2.369(3) . ? O3W Eu3 2.356(3) . ? O4W Eu3 2.437(3) . ? O5W Eu1 2.447(4) . ? O6W Eu2 2.461(4) . ? O7W Eu2 2.469(4) . ? O8W Eu1 2.501(4) . ? O9W Eu2 2.488(4) . ? O10W Eu1 2.505(4) . ? Eu1 O3 2.466(4) . ? Eu1 O1 2.498(3) . ? Eu1 O5 2.499(3) . ? Eu1 O4 2.502(3) . ? Eu1 O2 2.551(3) . ? Eu1 Cl1 2.7350(14) . ? Eu2 O14 2.462(3) . ? Eu2 O13 2.505(3) . ? Eu2 O15 2.507(4) . ? Eu2 O12 2.508(3) . ? Eu2 O11 2.508(3) . ? Eu2 Cl2 2.7352(14) . ? Eu3 O7 2.353(3) . ? Eu3 O16 2.372(3) . ? Eu3 O17 2.377(3) . ? Eu3 O6 2.410(3) . ? C1 O1 1.227(6) . ? C1 N2 1.357(6) . ? C1 N1 1.364(6) . ? C2 N1 1.448(6) . ? C2 N3 1.458(6) . ? C2 C3 1.549(7) . ? C2 H2 0.9900 . ? C3 N2 1.456(6) . ? C3 N4 1.458(5) . ? C3 H3 0.9900 . ? C4 O6 1.237(5) . ? C4 N3 1.360(6) . ? C4 N4 1.361(6) . ? C5 N2 1.434(6) . ? C5 N5 1.451(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.444(6) . ? C6 N7 1.452(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.240(6) . ? C7 N6 1.347(6) . ? C7 N5 1.356(6) . ? C8 N5 1.438(6) . ? C8 N7 1.457(6) . ? C8 C9 1.537(7) . ? C8 H8 0.9900 . ? C9 N8 1.452(6) . ? C9 N6 1.485(6) . ? C9 H9 0.9900 . ? C10 O7 1.231(5) . ? C10 N8 1.342(6) . ? C10 N7 1.358(6) . ? C11 N6 1.434(6) . ? C11 N9 1.435(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N8 1.454(6) . ? C12 N11 1.454(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.254(6) . ? C13 N9 1.356(7) . ? C13 N10 1.361(6) . ? C14 N11 1.450(6) . ? C14 N9 1.451(6) . ? C14 C15 1.562(7) . ? C14 H14 0.9900 . ? C15 N10 1.444(6) . ? C15 N12 1.454(7) . ? C15 H15 0.9900 . ? C16 O8 1.216(6) . ? C16 N11 1.364(7) . ? C16 N12 1.374(6) . ? C17 N13 1.442(7) . ? C17 N10 1.447(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.428(7) . ? C18 N12 1.450(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.237(6) . ? C19 N14 1.354(7) . ? C19 N13 1.363(7) . ? C20 N13 1.448(7) . ? C20 N15 1.449(6) . ? C20 C21 1.559(8) . ? C20 H20 0.9900 . ? C21 N14 1.447(6) . ? C21 N16 1.456(7) . ? C21 H21A 0.9900 . ? C22 O9 1.215(6) . ? C22 N15 1.373(7) . ? C22 N16 1.382(7) . ? C23 N14 1.430(7) . ? C23 N17 1.440(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.446(7) . ? C24 N16 1.444(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.229(6) . ? C25 N18 1.360(6) . ? C25 N17 1.364(6) . ? C26 N17 1.451(6) . ? C26 N19 1.460(6) . ? C26 C27 1.530(7) . ? C26 H26 0.9900 . ? C27 N20 1.432(6) . ? C27 N18 1.455(6) . ? C27 H27 0.9900 . ? C28 O10 1.237(6) . ? C28 N19 1.357(7) . ? C28 N20 1.372(6) . ? C29 N18 1.440(6) . ? C29 N1 1.448(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N3 1.434(6) . ? C30 N20 1.458(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O11 1.239(6) . ? C31 N21 1.345(6) . ? C31 N22 1.370(7) . ? C32 N21 1.450(7) . ? C32 N23 1.457(6) . ? C32 C33 1.571(8) . ? C32 H32 0.9900 . ? C33 N22 1.453(6) . ? C33 N24 1.454(6) . ? C33 H33 0.9900 . ? C34 O16 1.236(5) . ? C34 N23 1.347(6) . ? C34 N24 1.353(6) . ? C35 N25 1.442(6) . ? C35 N22 1.453(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 N27 1.442(6) . ? C36 N24 1.458(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O12 1.225(6) . ? C37 N25 1.355(6) . ? C37 N26 1.381(6) . ? C38 N25 1.457(6) . ? C38 N27 1.462(6) . ? C38 C39 1.533(7) . ? C38 H38 0.9900 . ? C39 N26 1.436(6) . ? C39 N28 1.464(6) . ? C39 H39 0.9900 . ? C40 O17 1.234(5) . ? C40 N28 1.341(6) . ? C40 N27 1.367(6) . ? C41 N29 1.441(6) . ? C41 N26 1.453(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 N31 1.441(6) . ? C42 N28 1.464(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C43 O13 1.232(6) . ? C43 N29 1.345(6) . ? C43 N30 1.355(6) . ? C44 N29 1.442(6) . ? C44 N31 1.451(6) . ? C44 C45 1.560(7) . ? C44 H44 0.9900 . ? C45 N30 1.443(6) . ? C45 N32 1.445(6) . ? C45 H45 0.9900 . ? C46 O18 1.221(6) . ? C46 N32 1.369(6) . ? C46 N31 1.370(6) . ? C47 N30 1.437(6) . ? C47 N33 1.445(7) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 N35 1.441(7) . ? C48 N32 1.453(6) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 O14 1.246(6) . ? C49 N33 1.334(7) . ? C49 N34 1.364(7) . ? C50 N35 1.455(7) . ? C50 N33 1.461(6) . ? C50 C51 1.543(8) . ? C50 H50 0.9900 . ? C51 N36 1.449(7) . ? C51 N34 1.460(7) . ? C51 H51 0.9900 . ? C52 O19 1.214(6) . ? C52 N36 1.356(7) . ? C52 N35 1.369(7) . ? C53 N34 1.431(7) . ? C53 N37 1.441(7) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 N39 1.439(7) . ? C54 N36 1.457(7) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 O15 1.248(6) . ? C55 N38 1.342(7) . ? C55 N37 1.366(7) . ? C56 N39 1.445(7) . ? C56 N37 1.452(7) . ? C56 C57 1.548(8) . ? C56 H56 0.9900 . ? C57 N38 1.451(7) . ? C57 N40 1.458(7) . ? C57 H57 0.9900 . ? C58 O20 1.228(6) . ? C58 N39 1.349(7) . ? C58 N40 1.376(7) . ? C59 N38 1.439(7) . ? C59 N21 1.442(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C60 N40 1.423(7) . ? C60 N23 1.458(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C61 C62 1.368(8) . ? C61 O21 1.371(6) . ? C61 C66 1.379(8) . ? C62 C63 1.390(8) . ? C62 H62 0.9400 . ? C63 C64 1.400(8) . ? C63 H63 0.9400 . ? C64 C65 1.365(8) . ? C64 O22 1.371(6) . ? C65 C66 1.382(7) . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? C67 C68 1.335(14) . ? C67 C69 1.371(14) 2_656 ? C67 O23 1.416(12) . ? C68 C69 1.413(14) . ? C68 H68 0.9400 . ? C69 C67 1.371(14) 2_656 ? C69 H69 0.9400 . ? C70 O24 1.366(10) . ? C70 C71 1.380(2) . ? C70 C75 1.381(2) . ? C71 C72 1.383(2) . ? C71 H71 0.9400 . ? C72 C73 1.380(2) . ? C72 H72 0.9400 . ? C73 C74 1.380(2) . ? C73 O25 1.397(12) . ? C74 C75 1.382(2) . ? C74 H74 0.9400 . ? C75 H75 0.9400 . ? O21 H21 0.8300 . ? O22 H22 0.8300 . ? O23 H23 0.8300 . ? O24 H24 0.8300 . ? O25 H25 0.8300 . ? 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 O28 N41 O29 121.0(5) . . ? O28 N41 O27 120.1(5) . . ? O29 N41 O27 118.8(5) . . ? O30 N42 O32 128.1(6) . . ? O30 N42 O31 127.2(6) . . ? O32 N42 O31 104.5(7) . . ? O33 N43 O34 122.7(10) . . ? O33 N43 O35 120.4(8) . . ? O34 N43 O35 117.0(10) . . ? O5W Eu1 O3 76.11(13) . . ? O5W Eu1 O1 139.37(12) . . ? O3 Eu1 O1 136.12(11) . . ? O5W Eu1 O5 99.34(13) . . ? O3 Eu1 O5 138.11(11) . . ? O1 Eu1 O5 72.61(11) . . ? O5W Eu1 O8W 70.77(14) . . ? O3 Eu1 O8W 142.25(13) . . ? O1 Eu1 O8W 69.60(12) . . ? O5 Eu1 O8W 66.50(13) . . ? O5W Eu1 O4 64.77(12) . . ? O3 Eu1 O4 72.37(12) . . ? O1 Eu1 O4 137.58(11) . . ? O5 Eu1 O4 68.37(12) . . ? O8W Eu1 O4 107.88(13) . . ? O5W Eu1 O10W 66.81(16) . . ? O3 Eu1 O10W 81.43(18) . . ? O1 Eu1 O10W 90.99(18) . . ? O5 Eu1 O10W 135.83(16) . . ? O8W Eu1 O10W 69.35(18) . . ? O4 Eu1 O10W 128.94(17) . . ? O5W Eu1 O2 120.68(12) . . ? O3 Eu1 O2 69.45(11) . . ? O1 Eu1 O2 69.02(11) . . ? O5 Eu1 O2 138.11(11) . . ? O8W Eu1 O2 113.21(12) . . ? O4 Eu1 O2 137.79(11) . . ? O10W Eu1 O2 61.54(13) . . ? O5W Eu1 Cl1 140.81(10) . . ? O3 Eu1 Cl1 79.39(8) . . ? O1 Eu1 Cl1 78.17(7) . . ? O5 Eu1 Cl1 79.33(8) . . ? O8W Eu1 Cl1 138.33(11) . . ? O4 Eu1 Cl1 78.92(8) . . ? O10W Eu1 Cl1 138.26(11) . . ? O2 Eu1 Cl1 77.04(7) . . ? O6W Eu2 O14 76.80(14) . . ? O6W Eu2 O7W 71.13(14) . . ? O14 Eu2 O7W 141.89(12) . . ? O6W Eu2 O9W 67.66(17) . . ? O14 Eu2 O9W 80.74(16) . . ? O7W Eu2 O9W 68.49(16) . . ? O6W Eu2 O13 62.63(12) . . ? O14 Eu2 O13 70.96(11) . . ? O7W Eu2 O13 109.99(14) . . ? O9W Eu2 O13 126.82(16) . . ? O6W Eu2 O15 123.74(15) . . ? O14 Eu2 O15 70.37(12) . . ? O7W Eu2 O15 111.70(14) . . ? O9W Eu2 O15 63.01(13) . . ? O13 Eu2 O15 137.14(11) . . ? O6W Eu2 O12 97.30(15) . . ? O14 Eu2 O12 138.05(11) . . ? O7W Eu2 O12 67.48(13) . . ? O9W Eu2 O12 135.97(14) . . ? O13 Eu2 O12 69.67(11) . . ? O15 Eu2 O12 137.18(11) . . ? O6W Eu2 O11 140.32(12) . . ? O14 Eu2 O11 136.71(11) . . ? O7W Eu2 O11 69.42(12) . . ? O9W Eu2 O11 93.74(17) . . ? O13 Eu2 O11 137.27(11) . . ? O15 Eu2 O11 69.02(12) . . ? O12 Eu2 O11 71.43(11) . . ? O6W Eu2 Cl2 138.44(10) . . ? O14 Eu2 Cl2 79.47(8) . . ? O7W Eu2 Cl2 138.62(10) . . ? O9W Eu2 Cl2 140.23(11) . . ? O13 Eu2 Cl2 77.57(8) . . ? O15 Eu2 Cl2 77.91(9) . . ? O12 Eu2 Cl2 78.53(8) . . ? O11 Eu2 Cl2 78.05(8) . . ? O7 Eu3 O3W 112.63(12) . . ? O7 Eu3 O2W 80.56(11) . . ? O3W Eu3 O2W 138.61(12) . . ? O7 Eu3 O16 146.90(11) . . ? O3W Eu3 O16 77.47(12) . . ? O2W Eu3 O16 72.95(12) . . ? O7 Eu3 O17 135.18(11) . . ? O3W Eu3 O17 82.53(12) . . ? O2W Eu3 O17 116.51(11) . . ? O16 Eu3 O17 75.84(11) . . ? O7 Eu3 O6 75.27(10) . . ? O3W Eu3 O6 71.29(11) . . ? O2W Eu3 O6 75.10(11) . . ? O16 Eu3 O6 78.96(11) . . ? O17 Eu3 O6 146.92(11) . . ? O7 Eu3 O4W 72.62(11) . . ? O3W Eu3 O4W 148.19(12) . . ? O2W Eu3 O4W 72.48(13) . . ? O16 Eu3 O4W 116.13(13) . . ? O17 Eu3 O4W 74.14(12) . . ? O6 Eu3 O4W 137.28(11) . . ? O7 Eu3 O1W 71.35(11) . . ? O3W Eu3 O1W 71.21(12) . . ? O2W Eu3 O1W 146.55(12) . . ? O16 Eu3 O1W 139.34(11) . . ? O17 Eu3 O1W 74.97(11) . . ? O6 Eu3 O1W 113.37(12) . . ? O4W Eu3 O1W 81.91(13) . . ? O1 C1 N2 126.4(5) . . ? O1 C1 N1 125.1(4) . . ? N2 C1 N1 108.5(4) . . ? N1 C2 N3 114.1(4) . . ? N1 C2 C3 103.3(4) . . ? N3 C2 C3 103.1(3) . . ? N1 C2 H2 111.9 . . ? N3 C2 H2 111.9 . . ? C3 C2 H2 111.9 . . ? N2 C3 N4 114.0(4) . . ? N2 C3 C2 102.9(4) . . ? N4 C3 C2 103.7(3) . . ? N2 C3 H3 111.9 . . ? N4 C3 H3 111.9 . . ? C2 C3 H3 111.9 . . ? O6 C4 N3 124.3(4) . . ? O6 C4 N4 125.9(4) . . ? N3 C4 N4 109.7(4) . . ? N2 C5 N5 113.9(4) . . ? N2 C5 H5A 108.8 . . ? N5 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? N5 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N7 113.5(4) . . ? N4 C6 H6A 108.9 . . ? N7 C6 H6A 108.9 . . ? N4 C6 H6B 108.9 . . ? N7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 N6 125.0(5) . . ? O2 C7 N5 125.5(4) . . ? N6 C7 N5 109.3(4) . . ? N5 C8 N7 114.7(4) . . ? N5 C8 C9 104.0(4) . . ? N7 C8 C9 102.4(4) . . ? N5 C8 H8 111.7 . . ? N7 C8 H8 111.7 . . ? C9 C8 H8 111.7 . . ? N8 C9 N6 113.4(4) . . ? N8 C9 C8 104.0(3) . . ? N6 C9 C8 102.4(4) . . ? N8 C9 H9 112.1 . . ? N6 C9 H9 112.1 . . ? C8 C9 H9 112.1 . . ? O7 C10 N8 125.0(4) . . ? O7 C10 N7 125.7(4) . . ? N8 C10 N7 109.3(4) . . ? N6 C11 N9 114.6(4) . . ? N6 C11 H11A 108.6 . . ? N9 C11 H11A 108.6 . . ? N6 C11 H11B 108.6 . . ? N9 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? N8 C12 N11 113.3(4) . . ? N8 C12 H12A 108.9 . . ? N11 C12 H12A 108.9 . . ? N8 C12 H12B 108.9 . . ? N11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 126.0(5) . . ? O3 C13 N10 125.4(5) . . ? N9 C13 N10 108.5(4) . . ? N11 C14 N9 114.6(4) . . ? N11 C14 C15 102.1(4) . . ? N9 C14 C15 102.0(4) . . ? N11 C14 H14 112.4 . . ? N9 C14 H14 112.4 . . ? C15 C14 H14 112.4 . . ? N10 C15 N12 113.7(4) . . ? N10 C15 C14 103.7(4) . . ? N12 C15 C14 103.7(4) . . ? N10 C15 H15 111.7 . . ? N12 C15 H15 111.7 . . ? C14 C15 H15 111.7 . . ? O8 C16 N11 126.7(5) . . ? O8 C16 N12 125.5(5) . . ? N11 C16 N12 107.7(4) . . ? N13 C17 N10 113.8(4) . . ? N13 C17 H17A 108.8 . . ? N10 C17 H17A 108.8 . . ? N13 C17 H17B 108.8 . . ? N10 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N15 C18 N12 114.7(4) . . ? N15 C18 H18A 108.6 . . ? N12 C18 H18A 108.6 . . ? N15 C18 H18B 108.6 . . ? N12 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N14 125.5(5) . . ? O4 C19 N13 125.3(5) . . ? N14 C19 N13 109.1(4) . . ? N13 C20 N15 114.7(4) . . ? N13 C20 C21 102.5(4) . . ? N15 C20 C21 104.3(4) . . ? N13 C20 H20 111.6 . . ? N15 C20 H20 111.6 . . ? C21 C20 H20 111.6 . . ? N14 C21 N16 115.0(4) . . ? N14 C21 C20 103.7(4) . . ? N16 C21 C20 102.8(4) . . ? N14 C21 H21A 111.6 . . ? N16 C21 H21A 111.6 . . ? C20 C21 H21A 111.6 . . ? O9 C22 N15 126.0(5) . . ? O9 C22 N16 125.3(6) . . ? N15 C22 N16 108.7(5) . . ? N14 C23 N17 113.5(4) . . ? N14 C23 H23A 108.9 . . ? N17 C23 H23A 108.9 . . ? N14 C23 H23B 108.9 . . ? N17 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N19 C24 N16 114.4(4) . . ? N19 C24 H24A 108.7 . . ? N16 C24 H24A 108.7 . . ? N19 C24 H24B 108.7 . . ? N16 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N18 125.4(4) . . ? O5 C25 N17 126.2(5) . . ? N18 C25 N17 108.3(4) . . ? N17 C26 N19 115.0(4) . . ? N17 C26 C27 104.3(4) . . ? N19 C26 C27 103.5(4) . . ? N17 C26 H26 111.2 . . ? N19 C26 H26 111.2 . . ? C27 C26 H26 111.2 . . ? N20 C27 N18 114.8(4) . . ? N20 C27 C26 103.9(4) . . ? N18 C27 C26 102.7(4) . . ? N20 C27 H27 111.6 . . ? N18 C27 H27 111.6 . . ? C26 C27 H27 111.6 . . ? O10 C28 N19 126.5(5) . . ? O10 C28 N20 125.0(5) . . ? N19 C28 N20 108.4(4) . . ? N18 C29 N1 113.0(4) . . ? N18 C29 H29A 109.0 . . ? N1 C29 H29A 109.0 . . ? N18 C29 H29B 109.0 . . ? N1 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N3 C30 N20 114.6(4) . . ? N3 C30 H30A 108.6 . . ? N20 C30 H30A 108.6 . . ? N3 C30 H30B 108.6 . . ? N20 C30 H30B 108.6 . . ? H30A C30 H30B 107.6 . . ? O11 C31 N21 126.7(5) . . ? O11 C31 N22 123.9(5) . . ? N21 C31 N22 109.3(4) . . ? N21 C32 N23 115.1(4) . . ? N21 C32 C33 102.2(4) . . ? N23 C32 C33 102.8(4) . . ? N21 C32 H32 112.0 . . ? N23 C32 H32 112.0 . . ? C33 C32 H32 112.0 . . ? N22 C33 N24 114.3(4) . . ? N22 C33 C32 103.2(4) . . ? N24 C33 C32 102.4(4) . . ? N22 C33 H33 112.1 . . ? N24 C33 H33 112.1 . . ? C32 C33 H33 112.1 . . ? O16 C34 N23 124.8(4) . . ? O16 C34 N24 125.2(5) . . ? N23 C34 N24 109.9(4) . . ? N25 C35 N22 113.8(4) . . ? N25 C35 H35A 108.8 . . ? N22 C35 H35A 108.8 . . ? N25 C35 H35B 108.8 . . ? N22 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N27 C36 N24 113.5(4) . . ? N27 C36 H36A 108.9 . . ? N24 C36 H36A 108.9 . . ? N27 C36 H36B 108.9 . . ? N24 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O12 C37 N25 126.3(4) . . ? O12 C37 N26 125.6(4) . . ? N25 C37 N26 108.1(4) . . ? N25 C38 N27 114.0(4) . . ? N25 C38 C39 103.1(4) . . ? N27 C38 C39 103.9(4) . . ? N25 C38 H38 111.8 . . ? N27 C38 H38 111.8 . . ? C39 C38 H38 111.8 . . ? N26 C39 N28 113.7(4) . . ? N26 C39 C38 104.0(4) . . ? N28 C39 C38 103.0(4) . . ? N26 C39 H39 111.8 . . ? N28 C39 H39 111.8 . . ? C38 C39 H39 111.8 . . ? O17 C40 N28 125.9(4) . . ? O17 C40 N27 124.4(4) . . ? N28 C40 N27 109.7(4) . . ? N29 C41 N26 113.6(4) . . ? N29 C41 H41A 108.8 . . ? N26 C41 H41A 108.8 . . ? N29 C41 H41B 108.8 . . ? N26 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? N31 C42 N28 114.1(4) . . ? N31 C42 H42A 108.7 . . ? N28 C42 H42A 108.7 . . ? N31 C42 H42B 108.7 . . ? N28 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? O13 C43 N29 125.4(4) . . ? O13 C43 N30 125.0(5) . . ? N29 C43 N30 109.5(4) . . ? N29 C44 N31 114.5(4) . . ? N29 C44 C45 102.6(4) . . ? N31 C44 C45 102.3(4) . . ? N29 C44 H44 112.2 . . ? N31 C44 H44 112.2 . . ? C45 C44 H44 112.2 . . ? N30 C45 N32 114.6(4) . . ? N30 C45 C44 103.2(4) . . ? N32 C45 C44 103.8(4) . . ? N30 C45 H45 111.5 . . ? N32 C45 H45 111.5 . . ? C44 C45 H45 111.5 . . ? O18 C46 N32 125.9(5) . . ? O18 C46 N31 126.3(5) . . ? N32 C46 N31 107.7(4) . . ? N30 C47 N33 114.3(4) . . ? N30 C47 H47A 108.7 . . ? N33 C47 H47A 108.7 . . ? N30 C47 H47B 108.7 . . ? N33 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N35 C48 N32 114.2(4) . . ? N35 C48 H48A 108.7 . . ? N32 C48 H48A 108.7 . . ? N35 C48 H48B 108.7 . . ? N32 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? O14 C49 N33 126.2(5) . . ? O14 C49 N34 124.4(5) . . ? N33 C49 N34 109.3(4) . . ? N35 C50 N33 114.8(4) . . ? N35 C50 C51 102.7(4) . . ? N33 C50 C51 103.1(4) . . ? N35 C50 H50 111.9 . . ? N33 C50 H50 111.9 . . ? C51 C50 H50 111.9 . . ? N36 C51 N34 115.6(4) . . ? N36 C51 C50 104.1(4) . . ? N34 C51 C50 103.0(4) . . ? N36 C51 H51 111.2 . . ? N34 C51 H51 111.2 . . ? C50 C51 H51 111.2 . . ? O19 C52 N36 125.6(5) . . ? O19 C52 N35 125.6(5) . . ? N36 C52 N35 108.7(5) . . ? N34 C53 N37 113.4(4) . . ? N34 C53 H53A 108.9 . . ? N37 C53 H53A 108.9 . . ? N34 C53 H53B 108.9 . . ? N37 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? N39 C54 N36 114.2(4) . . ? N39 C54 H54A 108.7 . . ? N36 C54 H54A 108.7 . . ? N39 C54 H54B 108.7 . . ? N36 C54 H54B 108.7 . . ? H54A C54 H54B 107.6 . . ? O15 C55 N38 125.4(5) . . ? O15 C55 N37 124.9(5) . . ? N38 C55 N37 109.6(5) . . ? N39 C56 N37 113.7(4) . . ? N39 C56 C57 103.7(4) . . ? N37 C56 C57 103.5(4) . . ? N39 C56 H56 111.8 . . ? N37 C56 H56 111.8 . . ? C57 C56 H56 111.8 . . ? N38 C57 N40 114.0(4) . . ? N38 C57 C56 102.9(4) . . ? N40 C57 C56 103.1(4) . . ? N38 C57 H57 112.0 . . ? N40 C57 H57 112.0 . . ? C56 C57 H57 112.0 . . ? O20 C58 N39 127.3(5) . . ? O20 C58 N40 123.3(5) . . ? N39 C58 N40 109.4(4) . . ? N38 C59 N21 114.1(4) . . ? N38 C59 H59A 108.7 . . ? N21 C59 H59A 108.7 . . ? N38 C59 H59B 108.7 . . ? N21 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? N40 C60 N23 115.4(4) . . ? N40 C60 H60A 108.4 . . ? N23 C60 H60A 108.4 . . ? N40 C60 H60B 108.4 . . ? N23 C60 H60B 108.4 . . ? H60A C60 H60B 107.5 . . ? C1 N1 C2 112.5(4) . . ? C1 N1 C29 121.9(4) . . ? C2 N1 C29 125.6(4) . . ? C1 N2 C5 122.8(4) . . ? C1 N2 C3 112.6(4) . . ? C5 N2 C3 124.6(4) . . ? C4 N3 C30 123.7(4) . . ? C4 N3 C2 111.9(4) . . ? C30 N3 C2 123.7(4) . . ? C4 N4 C6 124.0(4) . . ? C4 N4 C3 111.5(4) . . ? C6 N4 C3 124.2(4) . . ? C7 N5 C8 112.5(4) . . ? C7 N5 C5 121.0(4) . . ? C8 N5 C5 126.5(4) . . ? C7 N6 C11 122.5(4) . . ? C7 N6 C9 111.4(4) . . ? C11 N6 C9 126.0(4) . . ? C10 N7 C6 122.5(4) . . ? C10 N7 C8 112.2(4) . . ? C6 N7 C8 125.0(4) . . ? C10 N8 C9 111.9(4) . . ? C10 N8 C12 122.4(4) . . ? C9 N8 C12 125.7(4) . . ? C13 N9 C11 122.6(4) . . ? C13 N9 C14 113.3(4) . . ? C11 N9 C14 124.1(4) . . ? C13 N10 C15 112.3(4) . . ? C13 N10 C17 122.3(4) . . ? C15 N10 C17 125.4(4) . . ? C16 N11 C14 113.9(4) . . ? C16 N11 C12 122.8(4) . . ? C14 N11 C12 122.6(4) . . ? C16 N12 C18 122.3(5) . . ? C16 N12 C15 112.3(4) . . ? C18 N12 C15 124.7(4) . . ? C19 N13 C17 120.9(4) . . ? C19 N13 C20 112.6(5) . . ? C17 N13 C20 126.5(5) . . ? C19 N14 C23 123.4(4) . . ? C19 N14 C21 112.0(4) . . ? C23 N14 C21 124.6(4) . . ? C22 N15 C18 121.5(5) . . ? C22 N15 C20 111.9(5) . . ? C18 N15 C20 126.6(5) . . ? C22 N16 C24 122.1(5) . . ? C22 N16 C21 112.3(5) . . ? C24 N16 C21 125.6(5) . . ? C25 N17 C23 123.4(4) . . ? C25 N17 C26 111.7(4) . . ? C23 N17 C26 124.9(4) . . ? C25 N18 C29 122.1(4) . . ? C25 N18 C27 112.8(4) . . ? C29 N18 C27 124.9(4) . . ? C28 N19 C24 122.7(4) . . ? C28 N19 C26 111.7(4) . . ? C24 N19 C26 125.4(4) . . ? C28 N20 C27 112.4(4) . . ? C28 N20 C30 122.3(4) . . ? C27 N20 C30 125.2(4) . . ? C31 N21 C59 123.2(4) . . ? C31 N21 C32 113.0(4) . . ? C59 N21 C32 123.7(4) . . ? C31 N22 C33 111.7(4) . . ? C31 N22 C35 122.8(4) . . ? C33 N22 C35 125.4(4) . . ? C34 N23 C32 112.1(4) . . ? C34 N23 C60 122.9(4) . . ? C32 N23 C60 124.0(4) . . ? C34 N24 C33 112.4(4) . . ? C34 N24 C36 123.9(4) . . ? C33 N24 C36 123.6(4) . . ? C37 N25 C35 122.7(4) . . ? C37 N25 C38 112.4(4) . . ? C35 N25 C38 124.9(4) . . ? C37 N26 C39 111.9(4) . . ? C37 N26 C41 122.4(4) . . ? C39 N26 C41 125.5(4) . . ? C40 N27 C36 123.3(4) . . ? C40 N27 C38 111.0(4) . . ? C36 N27 C38 125.7(4) . . ? C40 N28 C39 112.0(4) . . ? C40 N28 C42 122.3(4) . . ? C39 N28 C42 124.0(4) . . ? C43 N29 C41 121.6(4) . . ? C43 N29 C44 112.6(4) . . ? C41 N29 C44 125.6(4) . . ? C43 N30 C47 122.5(4) . . ? C43 N30 C45 111.7(4) . . ? C47 N30 C45 125.7(4) . . ? C46 N31 C42 122.6(4) . . ? C46 N31 C44 113.5(4) . . ? C42 N31 C44 123.9(4) . . ? C46 N32 C45 112.7(4) . . ? C46 N32 C48 122.1(4) . . ? C45 N32 C48 124.7(4) . . ? C49 N33 C47 123.1(4) . . ? C49 N33 C50 112.6(5) . . ? C47 N33 C50 124.2(4) . . ? C49 N34 C53 124.6(4) . . ? C49 N34 C51 111.8(4) . . ? C53 N34 C51 123.6(4) . . ? C52 N35 C48 122.4(5) . . ? C52 N35 C50 112.4(5) . . ? C48 N35 C50 125.1(5) . . ? C52 N36 C51 112.1(5) . . ? C52 N36 C54 122.5(5) . . ? C51 N36 C54 125.4(5) . . ? C55 N37 C53 122.9(5) . . ? C55 N37 C56 111.3(5) . . ? C53 N37 C56 125.7(4) . . ? C55 N38 C59 122.1(4) . . ? C55 N38 C57 112.4(4) . . ? C59 N38 C57 125.6(4) . . ? C58 N39 C54 123.1(4) . . ? C58 N39 C56 112.3(5) . . ? C54 N39 C56 124.6(5) . . ? C58 N40 C60 123.2(4) . . ? C58 N40 C57 111.1(4) . . ? C60 N40 C57 125.2(4) . . ? C1 O1 Eu1 133.5(3) . . ? C7 O2 Eu1 136.1(3) . . ? C13 O3 Eu1 132.9(3) . . ? C19 O4 Eu1 135.5(3) . . ? C25 O5 Eu1 131.9(3) . . ? C4 O6 Eu3 152.1(3) . . ? C10 O7 Eu3 155.1(3) . . ? C31 O11 Eu2 133.8(3) . . ? C37 O12 Eu2 133.4(3) . . ? C43 O13 Eu2 134.6(3) . . ? C49 O14 Eu2 135.7(3) . . ? C55 O15 Eu2 135.7(3) . . ? C34 O16 Eu3 156.8(3) . . ? C40 O17 Eu3 157.8(3) . . ? C62 C61 O21 117.3(5) . . ? C62 C61 C66 119.2(5) . . ? O21 C61 C66 123.5(5) . . ? C61 C62 C63 121.7(5) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C62 C63 C64 118.4(5) . . ? C62 C63 H63 120.8 . . ? C64 C63 H63 120.8 . . ? C65 C64 O22 122.3(5) . . ? C65 C64 C63 119.7(5) . . ? O22 C64 C63 118.0(5) . . ? C64 C65 C66 121.0(5) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C61 C66 C65 120.0(5) . . ? C61 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C68 C67 C69 121.1(11) . 2_656 ? C68 C67 O23 122.5(14) . . ? C69 C67 O23 116.4(13) 2_656 . ? C67 C68 C69 120.2(11) . . ? C67 C68 H68 119.9 . . ? C69 C68 H68 119.9 . . ? C67 C69 C68 118.7(11) 2_656 . ? C67 C69 H69 120.7 2_656 . ? C68 C69 H69 120.7 . . ? O24 C70 C71 118.9(8) . . ? O24 C70 C75 121.8(8) . . ? C71 C70 C75 119.3(9) . . ? C70 C71 C72 118.5(10) . . ? C70 C71 H71 120.8 . . ? C72 C71 H71 120.8 . . ? C73 C72 C71 122.6(11) . . ? C73 C72 H72 118.7 . . ? C71 C72 H72 118.7 . . ? C72 C73 C74 118.5(10) . . ? C72 C73 O25 119.8(10) . . ? C74 C73 O25 121.6(10) . . ? C73 C74 C75 119.3(10) . . ? C73 C74 H74 120.4 . . ? C75 C74 H74 120.4 . . ? C70 C75 C74 121.7(9) . . ? C70 C75 H75 119.1 . . ? C74 C75 H75 119.1 . . ? C61 O21 H21 109.5 . . ? C64 O22 H22 109.5 . . ? C67 O23 H23 109.5 . . ? C70 O24 H24 109.5 . . ? C73 O25 H25 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.505 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.127 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.298 0.185 0.202 1839 612 ' ' 2 0.000 0.354 0.958 7 8 ' ' 3 0.000 0.646 0.042 7 10 ' ' _platon_squeeze_details ; ; data_04 _database_code_depnum_ccdc_archive 'CCDC 875768' #TrackingRef 'submit-04.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H80 Cl2 Gd3 N40 O30, C6 H6 O2, 7Cl, 48(H2 O)' _chemical_formula_sum 'C66 H182 Cl9 Gd3 N40 O80' _chemical_formula_weight 3607.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.065(5) _cell_length_b 18.410(5) _cell_length_c 24.350(6) _cell_angle_alpha 105.555(3) _cell_angle_beta 100.010(4) _cell_angle_gamma 102.267(4) _cell_volume 6982(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3686 _exptl_absorpt_coefficient_mu 1.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7498 _exptl_absorpt_correction_T_max 0.8353 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47426 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 23917 _reflns_number_gt 13730 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23917 _refine_ls_number_parameters 1399 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 3.015 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl3 Cl 0.6735(4) 0.2888(3) 0.1468(2) 0.103(2) Uani 1 1 d . . . Cl4 Cl 1.2078(8) 0.7666(8) 0.6195(6) 0.133(5) Uani 0.50 1 d P . . Cl5 Cl 0.7417(7) 0.5096(9) 0.3992(5) 0.156(6) Uani 0.50 1 d P . . Cl6 Cl 1.1982(7) 0.8995(11) -0.0621(6) 0.185(7) Uani 0.50 1 d P . . Cl7 Cl 1.7391(14) 1.0292(9) 0.0353(8) 0.228(9) Uani 0.50 1 d P . . Cl8 Cl 1.4724(8) 0.2957(13) 0.2445(8) 0.232(10) Uani 0.50 1 d P . . Cl9 Cl 1.0393(11) 0.8897(13) 0.0938(9) 0.380(6) Uani 0.50 1 d P . . Cl10 Cl 1.0085(19) 0.8672(12) -0.0400(8) 0.292(14) Uani 0.50 1 d P . . Cl11 Cl 1.4495(11) 0.4439(13) 0.5001(9) 0.380(6) Uani 0.50 1 d P . . Cl12 Cl 1.2932(11) 0.2781(9) 0.5162(11) 0.225(10) Uani 0.50 1 d P . . Cl13 Cl 1.3415(13) 1.0280(11) 0.4445(9) 0.239(9) Uani 0.50 1 d P . . Cl15 Cl 1.0257(14) 0.1915(9) 0.4976(7) 0.245(8) Uani 0.50 1 d P . . Cl16 Cl 1.213(2) 0.4923(19) -0.0672(14) 0.59(2) Uani 0.50 1 d P . . O1W O 1.4130(5) 0.6583(5) 0.2055(4) 0.051(3) Uani 1 1 d . . . O2W O 1.1492(5) 0.6209(5) 0.2094(4) 0.052(3) Uani 1 1 d . . . O3W O 1.3265(6) 0.5284(5) 0.1066(4) 0.063(3) Uani 1 1 d . . . O4W O 0.9767(7) 0.2901(6) 0.4234(4) 0.075(4) Uani 1 1 d . . . O5W O 1.6485(7) 1.1049(6) 0.1180(5) 0.078(4) Uani 1 1 d . . . O6W O 1.1438(7) 0.3588(6) 0.4915(5) 0.089(4) Uani 1 1 d . . . O7W O 1.1468(7) 0.5543(7) 0.0902(4) 0.076(4) Uani 1 1 d . . . O8W O 1.1007(10) 0.2287(7) 0.3931(6) 0.167(5) Uani 1 1 d . . . O9W O 1.5034(9) 1.1440(7) 0.1424(7) 0.165(5) Uani 1 1 d . . . O10W O 1.6443(16) 1.1735(8) 0.2272(7) 0.221(11) Uani 1 1 d . . . Gd1 Gd 1.08867(4) 0.35914(4) 0.38955(3) 0.0494(2) Uani 1 1 d . . . Gd2 Gd 1.26749(4) 0.61190(4) 0.17307(3) 0.04078(19) Uani 1 1 d . . . Gd3 Gd 1.55641(6) 1.04088(4) 0.16844(4) 0.0683(3) Uani 1 1 d . . . Cl1 Cl 1.1169(2) 0.4532(2) 0.32185(15) 0.0515(11) Uani 1 1 d . . . Cl2 Cl 1.4964(3) 0.8980(2) 0.17864(17) 0.0659(12) Uani 1 1 d . . . C61 C 1.2544(2) 0.3100(2) 0.04655(15) 0.148(7) Uani 1 1 d D . . C62 C 1.2037(2) 0.23291(18) 0.00985(14) 0.229(17) Uani 1 1 d D . . H62 H 1.1540 0.2262 -0.0171 0.275 Uiso 1 1 calc R . . C63 C 1.2316(2) 0.1687(2) 0.01598(19) 0.170(14) Uani 1 1 d D . . H63 H 1.1999 0.1177 -0.0071 0.204 Uiso 1 1 calc R . . C64 C 1.3042(3) 0.1789(2) 0.0550(3) 0.135(9) Uani 1 1 d D . . C65 C 1.3564(4) 0.2531(2) 0.0926(3) 0.133(9) Uani 1 1 d D . . H65 H 1.4060 0.2599 0.1197 0.159 Uiso 1 1 calc R . . C66 C 1.3255(3) 0.3140(2) 0.0846(3) 0.122(8) Uani 1 1 d D . . H66 H 1.3573 0.3646 0.1083 0.147 Uiso 1 1 calc R . . O21 O 1.2329(7) 0.3751(7) 0.0438(5) 0.133(7) Uani 1 1 d D . . H21 H 1.1904 0.3633 0.0170 0.199 Uiso 1 1 calc R . . O22 O 1.3357(12) 0.1137(8) 0.0563(7) 0.172(7) Uani 1 1 d . . . H22 H 1.3033 0.0733 0.0317 0.259 Uiso 1 1 calc R . . C1 C 0.9402(8) 0.4572(8) 0.3668(6) 0.047(4) Uani 1 1 d . . . C2 C 0.8550(8) 0.3548(9) 0.2758(7) 0.062(5) Uani 1 1 d . . . H2A H 0.7993 0.3477 0.2525 0.075 Uiso 1 1 calc R . . H2B H 0.8497 0.3232 0.3022 0.075 Uiso 1 1 calc R . . C3 C 0.9641(9) 0.2927(8) 0.2509(6) 0.052(5) Uani 1 1 d . . . C4 C 1.0523(9) 0.2216(8) 0.2011(7) 0.065(5) Uani 1 1 d . . . H4A H 1.0435 0.1897 0.2270 0.078 Uiso 1 1 calc R . . H4B H 1.0402 0.1857 0.1609 0.078 Uiso 1 1 calc R . . C5 C 1.1818(8) 0.2944(7) 0.2743(6) 0.048(4) Uani 1 1 d . . . C6 C 1.3237(8) 0.3576(7) 0.3306(6) 0.054(4) Uani 1 1 d . . . H6A H 1.3112 0.3239 0.3547 0.065 Uiso 1 1 calc R . . H6B H 1.3763 0.3532 0.3209 0.065 Uiso 1 1 calc R . . C7 C 1.2915(8) 0.4570(7) 0.4062(5) 0.044(4) Uani 1 1 d . . . C8 C 1.2909(8) 0.5745(8) 0.4836(6) 0.053(5) Uani 1 1 d . . . H8A H 1.2787 0.5386 0.5063 0.064 Uiso 1 1 calc R . . H8B H 1.3361 0.6200 0.5089 0.064 Uiso 1 1 calc R . . C9 C 1.1408(8) 0.5574(8) 0.4605(5) 0.045(4) Uani 1 1 d . . . C10 C 1.0013(8) 0.5754(8) 0.4497(5) 0.051(4) Uani 1 1 d . . . H10A H 0.9817 0.6209 0.4663 0.061 Uiso 1 1 calc R . . H10B H 0.9928 0.5406 0.4736 0.061 Uiso 1 1 calc R . . C11 C 1.1292(9) 0.6761(8) 0.4515(5) 0.050(4) Uani 1 1 d . . . H11 H 1.1215 0.7195 0.4824 0.060 Uiso 1 1 calc R . . C12 C 1.2195(9) 0.6766(7) 0.4604(6) 0.049(4) Uani 1 1 d . . . H12 H 1.2546 0.7197 0.4957 0.058 Uiso 1 1 calc R . . C13 C 1.3733(8) 0.5734(8) 0.4035(6) 0.046(4) Uani 1 1 d . . . H13 H 1.4268 0.6054 0.4313 0.055 Uiso 1 1 calc R . . C14 C 1.3841(9) 0.5043(8) 0.3560(6) 0.052(5) Uani 1 1 d . . . H14 H 1.4426 0.5029 0.3622 0.063 Uiso 1 1 calc R . . C15 C 1.2710(8) 0.3332(7) 0.2190(6) 0.046(4) Uani 1 1 d . . . H15 H 1.3131 0.3068 0.2071 0.055 Uiso 1 1 calc R . . C16 C 1.1846(8) 0.2909(7) 0.1783(6) 0.048(4) Uani 1 1 d . . . H16 H 1.1855 0.2461 0.1454 0.058 Uiso 1 1 calc R . . C17 C 0.9601(9) 0.2941(9) 0.1551(6) 0.062(5) Uani 1 1 d . . . H17 H 0.9325 0.2488 0.1192 0.075 Uiso 1 1 calc R . . C18 C 0.8978(9) 0.3350(9) 0.1783(7) 0.064(6) Uani 1 1 d . . . H18 H 0.8413 0.3094 0.1527 0.077 Uiso 1 1 calc R . . C19 C 0.8684(9) 0.4987(8) 0.2951(6) 0.061(5) Uani 1 1 d . . . H19 H 0.8079 0.4916 0.2863 0.074 Uiso 1 1 calc R . . C20 C 0.9145(8) 0.5719(8) 0.3531(6) 0.057(5) Uani 1 1 d . . . H20 H 0.8760 0.5995 0.3698 0.068 Uiso 1 1 calc R . . C21 C 0.9624(8) 0.5899(8) 0.2712(6) 0.053(4) Uani 1 1 d . . . C22 C 1.0309(9) 0.6935(7) 0.3656(6) 0.056(4) Uani 1 1 d . . . H22A H 1.0410 0.7265 0.3407 0.067 Uiso 1 1 calc R . . H22B H 1.0064 0.7203 0.3959 0.067 Uiso 1 1 calc R . . C23 C 1.1758(9) 0.6955(7) 0.3704(6) 0.046(4) Uani 1 1 d . . . C24 C 1.3207(9) 0.6933(7) 0.3950(6) 0.050(4) Uani 1 1 d . . . H24A H 1.3626 0.7227 0.4317 0.060 Uiso 1 1 calc R . . H24B H 1.3259 0.7238 0.3678 0.060 Uiso 1 1 calc R . . C25 C 1.3308(8) 0.5869(7) 0.3110(5) 0.040(4) Uani 1 1 d . . . C26 C 1.3614(8) 0.4740(8) 0.2456(5) 0.045(4) Uani 1 1 d . . . H26A H 1.4076 0.4508 0.2513 0.054 Uiso 1 1 calc R . . H26B H 1.3733 0.5083 0.2217 0.054 Uiso 1 1 calc R . . C27 C 1.2212(8) 0.4211(7) 0.1805(5) 0.040(4) Uani 1 1 d . . . C28 C 1.0841(9) 0.3423(8) 0.1168(6) 0.057(5) Uani 1 1 d . . . H28A H 1.0943 0.3786 0.0942 0.069 Uiso 1 1 calc R . . H28B H 1.0674 0.2890 0.0891 0.069 Uiso 1 1 calc R . . C29 C 0.9944(9) 0.4221(9) 0.1542(6) 0.055(5) Uani 1 1 d . . . C30 C 0.8821(9) 0.4714(10) 0.1888(6) 0.071(6) Uani 1 1 d . . . H30A H 0.8229 0.4445 0.1771 0.085 Uiso 1 1 calc R . . H30B H 0.8924 0.5046 0.1639 0.085 Uiso 1 1 calc R . . C31 C 1.2907(9) 0.7256(8) 0.0773(6) 0.053(4) Uani 1 1 d . . . C32 C 1.3739(10) 0.6777(8) 0.0109(6) 0.066(5) Uani 1 1 d . . . H32A H 1.3614 0.6674 -0.0318 0.079 Uiso 1 1 calc R . . H32B H 1.3518 0.6283 0.0179 0.079 Uiso 1 1 calc R . . C33 C 1.5013(8) 0.6826(8) 0.0789(6) 0.049(4) Uani 1 1 d . . . C34 C 1.6446(9) 0.7038(8) 0.1347(7) 0.064(5) Uani 1 1 d . . . H34A H 1.6213 0.6534 0.1400 0.076 Uiso 1 1 calc R . . H34B H 1.6936 0.7000 0.1195 0.076 Uiso 1 1 calc R . . C35 C 1.6362(9) 0.7548(8) 0.2375(7) 0.062(5) Uani 1 1 d . . . C36 C 1.6498(10) 0.8298(9) 0.3406(7) 0.074(6) Uani 1 1 d . . . H36A H 1.6295 0.7778 0.3443 0.088 Uiso 1 1 calc R . . H36B H 1.6995 0.8582 0.3724 0.088 Uiso 1 1 calc R . . C37 C 1.5049(10) 0.8337(8) 0.3324(6) 0.061(5) Uani 1 1 d . . . C38 C 1.3729(10) 0.8692(8) 0.3327(6) 0.066(5) Uani 1 1 d . . . H38A H 1.3592 0.9029 0.3662 0.080 Uiso 1 1 calc R . . H38B H 1.3537 0.8150 0.3325 0.080 Uiso 1 1 calc R . . C39 C 1.2886(8) 0.8143(8) 0.2303(6) 0.050(4) Uani 1 1 d . . . C40 C 1.1975(9) 0.7862(8) 0.1314(6) 0.060(5) Uani 1 1 d . . . H40A H 1.1509 0.8057 0.1180 0.072 Uiso 1 1 calc R . . H40B H 1.1750 0.7341 0.1341 0.072 Uiso 1 1 calc R . . C41 C 1.2529(10) 0.9211(8) 0.2086(7) 0.069(5) Uani 1 1 d . . . H41 H 1.1989 0.9332 0.2074 0.083 Uiso 1 1 calc R . . C42 C 1.3094(9) 0.9483(8) 0.2736(7) 0.072(5) Uani 1 1 d . . . H42 H 1.2800 0.9695 0.3031 0.086 Uiso 1 1 calc R . . C43 C 1.5162(12) 0.9669(8) 0.3683(6) 0.075(6) Uani 1 1 d . . . H43 H 1.5101 0.9902 0.4084 0.090 Uiso 1 1 calc R . . C44 C 1.6047(11) 0.9554(8) 0.3706(7) 0.069(6) Uani 1 1 d . . . H44 H 1.6405 0.9768 0.4110 0.082 Uiso 1 1 calc R . . C45 C 1.7371(10) 0.8771(10) 0.2724(7) 0.070(6) Uani 1 1 d . . . H45 H 1.7919 0.8866 0.2988 0.085 Uiso 1 1 calc R . . C46 C 1.7339(10) 0.8346(9) 0.2063(8) 0.076(6) Uani 1 1 d . . . H46 H 1.7875 0.8240 0.2022 0.092 Uiso 1 1 calc R . . C47 C 1.6045(10) 0.7612(8) 0.0508(6) 0.068(5) Uani 1 1 d . . . H47 H 1.6400 0.7390 0.0267 0.082 Uiso 1 1 calc R . . C48 C 1.5177(10) 0.7523(9) 0.0129(6) 0.065(5) Uani 1 1 d . . . H48 H 1.5141 0.7279 -0.0293 0.078 Uiso 1 1 calc R . . C49 C 1.3116(11) 0.7952(9) 0.0123(7) 0.073(6) Uani 1 1 d . . . H49 H 1.2821 0.7727 -0.0298 0.088 Uiso 1 1 calc R . . C50 C 1.2564(10) 0.8272(8) 0.0485(6) 0.067(5) Uani 1 1 d . . . H50 H 1.2025 0.8249 0.0242 0.081 Uiso 1 1 calc R . . C51 C 1.3784(11) 0.9222(8) 0.0632(7) 0.068(5) Uani 1 1 d . . . C52 C 1.2821(10) 0.9654(8) 0.1202(7) 0.072(5) Uani 1 1 d . . . H52A H 1.2219 0.9559 0.1082 0.086 Uiso 1 1 calc R . . H52B H 1.3078 1.0171 0.1180 0.086 Uiso 1 1 calc R . . C53 C 1.3787(10) 1.0135(7) 0.2183(7) 0.070(5) Uani 1 1 d . . . C54 C 1.4434(10) 1.0535(8) 0.3232(7) 0.073(5) Uani 1 1 d . . . H54A H 1.4196 1.0632 0.3574 0.088 Uiso 1 1 calc R . . H54B H 1.4657 1.1044 0.3183 0.088 Uiso 1 1 calc R . . C55 C 1.5778(12) 1.0329(8) 0.3118(7) 0.075(6) Uani 1 1 d . . . C56 C 1.7136(11) 1.0072(9) 0.3216(8) 0.076(6) Uani 1 1 d . . . H56A H 1.7528 1.0071 0.3561 0.092 Uiso 1 1 calc R . . H56B H 1.7308 1.0586 0.3162 0.092 Uiso 1 1 calc R . . C57 C 1.7038(10) 0.9536(8) 0.2163(8) 0.069(6) Uani 1 1 d . . . C58 C 1.7147(10) 0.8823(10) 0.1172(7) 0.078(5) Uani 1 1 d . . . H58A H 1.7340 0.9343 0.1134 0.094 Uiso 1 1 calc R . . H58B H 1.7537 0.8526 0.1054 0.094 Uiso 1 1 calc R . . C59 C 1.5784(10) 0.8813(9) 0.0633(6) 0.069(5) Uani 1 1 d . . . C60 C 1.4509(10) 0.8562(9) -0.0066(6) 0.067(5) Uani 1 1 d . . . H60A H 1.4303 0.8210 -0.0472 0.080 Uiso 1 1 calc R . . H60B H 1.4759 0.9086 -0.0078 0.080 Uiso 1 1 calc R . . N1 N 0.9513(7) 0.5344(6) 0.3906(5) 0.052(4) Uani 1 1 d . . . N2 N 0.8880(7) 0.4350(7) 0.3103(5) 0.057(4) Uani 1 1 d . . . N3 N 0.9034(7) 0.3253(7) 0.2363(5) 0.060(4) Uani 1 1 d . . . N4 N 0.9947(7) 0.2690(7) 0.2034(5) 0.057(4) Uani 1 1 d . . . N5 N 1.1372(7) 0.2656(6) 0.2179(5) 0.055(4) Uani 1 1 d . . . N6 N 1.2587(7) 0.3294(6) 0.2763(5) 0.048(3) Uani 1 1 d . . . N7 N 1.0866(7) 0.6013(6) 0.4542(4) 0.046(3) Uani 1 1 d . . . N8 N 1.2182(7) 0.6001(6) 0.4670(4) 0.044(3) Uani 1 1 d . . . N9 N 1.3177(7) 0.5350(6) 0.4326(4) 0.046(3) Uani 1 1 d . . . N10 N 1.3331(7) 0.4373(6) 0.3642(5) 0.048(3) Uani 1 1 d . . . N11 N 1.3377(6) 0.6178(6) 0.3695(4) 0.041(3) Uani 1 1 d . . . N12 N 1.3565(6) 0.5202(6) 0.3015(4) 0.041(3) Uani 1 1 d . . . N13 N 1.2874(7) 0.4124(6) 0.2140(5) 0.046(3) Uani 1 1 d . . . N14 N 1.1601(7) 0.3525(6) 0.1577(4) 0.044(3) Uani 1 1 d . . . N15 N 1.0166(7) 0.3548(7) 0.1424(5) 0.053(4) Uani 1 1 d . . . N16 N 0.9267(7) 0.4144(8) 0.1776(5) 0.059(4) Uani 1 1 d . . . N17 N 0.9029(7) 0.5217(7) 0.2501(5) 0.058(4) Uani 1 1 d . . . N18 N 0.9720(7) 0.6200(7) 0.3302(5) 0.056(4) Uani 1 1 d . . . N19 N 1.1087(7) 0.6865(6) 0.3939(4) 0.047(3) Uani 1 1 d . . . N20 N 1.2406(7) 0.6857(6) 0.4066(4) 0.042(3) Uani 1 1 d . . . N21 N 1.2481(8) 0.7798(7) 0.0878(5) 0.060(4) Uani 1 1 d . . . N22 N 1.3313(8) 0.7330(7) 0.0358(5) 0.060(4) Uani 1 1 d . . . N23 N 1.4627(7) 0.7017(6) 0.0332(5) 0.051(4) Uani 1 1 d . . . N24 N 1.5827(7) 0.7170(6) 0.0902(5) 0.056(4) Uani 1 1 d . . . N25 N 1.6696(7) 0.7632(7) 0.1906(6) 0.061(4) Uani 1 1 d . . . N26 N 1.6722(8) 0.8204(7) 0.2840(5) 0.063(4) Uani 1 1 d . . . N27 N 1.5884(9) 0.8707(7) 0.3472(5) 0.068(5) Uani 1 1 d . . . N28 N 1.4610(8) 0.8893(7) 0.3415(5) 0.061(4) Uani 1 1 d . . . N29 N 1.3281(7) 0.8763(6) 0.2794(5) 0.057(4) Uani 1 1 d . . . N30 N 1.2445(7) 0.8380(6) 0.1887(5) 0.058(4) Uani 1 1 d . . . N31 N 1.3050(8) 0.9658(7) 0.1811(6) 0.068(4) Uani 1 1 d . . . N32 N 1.3796(8) 1.0077(7) 0.2732(6) 0.070(4) Uani 1 1 d . . . N33 N 1.5115(9) 1.0192(7) 0.3354(6) 0.072(4) Uani 1 1 d . . . N34 N 1.6342(9) 0.9971(7) 0.3327(6) 0.067(5) Uani 1 1 d . . . N35 N 1.7183(8) 0.9482(7) 0.2708(6) 0.066(4) Uani 1 1 d . . . N36 N 1.7175(8) 0.8916(7) 0.1789(5) 0.064(4) Uani 1 1 d . . . N37 N 1.6357(7) 0.8439(6) 0.0772(5) 0.059(4) Uani 1 1 d . . . N38 N 1.5124(8) 0.8301(7) 0.0238(5) 0.059(4) Uani 1 1 d . . . N39 N 1.3800(8) 0.8589(7) 0.0211(5) 0.065(4) Uani 1 1 d . . . N40 N 1.3066(7) 0.9068(7) 0.0794(5) 0.066(4) Uani 1 1 d . . . O1 O 0.9668(6) 0.4121(5) 0.3878(4) 0.054(3) Uani 1 1 d . . . O2 O 0.9842(6) 0.2818(5) 0.2984(4) 0.055(3) Uani 1 1 d . . . O3 O 1.1542(6) 0.2832(5) 0.3161(4) 0.051(3) Uani 1 1 d . . . O4 O 1.2411(5) 0.4099(5) 0.4200(4) 0.046(3) Uani 1 1 d . . . O5 O 1.1216(5) 0.4899(5) 0.4649(4) 0.047(3) Uani 1 1 d . . . O6 O 1.3065(5) 0.6144(5) 0.2726(4) 0.041(3) Uani 1 1 d . . . O7 O 1.2164(5) 0.4814(5) 0.1704(4) 0.043(3) Uani 1 1 d . . . O8 O 1.0279(5) 0.4821(6) 0.1448(4) 0.055(3) Uani 1 1 d . . . O9 O 1.1789(6) 0.7110(5) 0.3240(4) 0.054(3) Uani 1 1 d . . . O10 O 1.0008(6) 0.6214(6) 0.2417(4) 0.061(3) Uani 1 1 d . . . O11 O 1.2917(6) 0.6760(5) 0.1033(4) 0.061(3) Uani 1 1 d . . . O12 O 1.2889(6) 0.7465(5) 0.2250(4) 0.048(3) Uani 1 1 d . . . O13 O 1.4732(7) 0.7626(5) 0.3147(5) 0.069(4) Uani 1 1 d . . . O14 O 1.5834(6) 0.6972(5) 0.2358(5) 0.061(3) Uani 1 1 d . . . O15 O 1.4681(6) 0.6397(5) 0.1045(4) 0.055(3) Uani 1 1 d . . . O16 O 1.5888(7) 0.9536(5) 0.0833(5) 0.069(3) Uani 1 1 d . . . O17 O 1.6861(7) 1.0095(6) 0.2029(5) 0.069(4) Uani 1 1 d . . . O18 O 1.5887(7) 1.0712(5) 0.2780(5) 0.073(4) Uani 1 1 d . . . O19 O 1.4323(7) 1.0571(5) 0.2055(5) 0.072(4) Uani 1 1 d . . . O20 O 1.4337(7) 0.9853(6) 0.0828(4) 0.072(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl3 0.103(4) 0.091(3) 0.093(3) 0.032(3) 0.010(3) -0.008(3) Cl4 0.130(9) 0.132(9) 0.145(9) 0.056(7) 0.066(7) 0.010(8) Cl5 0.085(7) 0.302(14) 0.109(6) 0.124(7) 0.043(5) 0.021(8) Cl6 0.077(7) 0.374(17) 0.164(8) 0.168(9) 0.054(6) 0.062(9) Cl7 0.41(2) 0.164(9) 0.138(13) 0.034(9) 0.032(14) 0.185(10) Cl8 0.133(8) 0.39(2) 0.189(14) 0.042(15) 0.076(9) 0.150(10) Cl9 0.132(8) 0.727(13) 0.459(10) 0.505(8) 0.020(8) 0.124(9) Cl10 0.58(4) 0.152(15) 0.136(12) 0.000(11) 0.143(17) 0.088(19) Cl11 0.132(8) 0.727(13) 0.459(10) 0.505(8) 0.020(8) 0.124(9) Cl12 0.151(12) 0.167(11) 0.41(2) 0.154(13) 0.069(15) 0.066(10) Cl13 0.321(16) 0.171(14) 0.276(16) 0.046(12) 0.209(12) 0.092(13) Cl15 0.40(2) 0.285(11) 0.239(9) 0.226(7) 0.202(11) 0.194(12) Cl16 0.55(4) 0.44(3) 0.52(3) 0.33(2) -0.39(2) -0.18(3) O1W 0.057(5) 0.049(5) 0.053(5) 0.019(4) 0.019(4) 0.017(4) O2W 0.051(5) 0.070(6) 0.042(5) 0.020(4) 0.018(4) 0.024(4) O3W 0.084(6) 0.053(5) 0.071(6) 0.024(4) 0.048(5) 0.028(5) O4W 0.101(7) 0.068(6) 0.074(6) 0.040(5) 0.045(5) 0.020(6) O5W 0.098(7) 0.062(6) 0.094(7) 0.041(5) 0.052(6) 0.019(5) O6W 0.094(8) 0.107(6) 0.106(7) 0.088(5) 0.033(6) 0.036(6) O7W 0.081(7) 0.099(7) 0.052(6) 0.031(5) 0.009(5) 0.025(6) O8W 0.330(13) 0.130(7) 0.182(8) 0.122(6) 0.196(8) 0.151(8) O9W 0.210(10) 0.108(7) 0.310(12) 0.152(7) 0.192(9) 0.102(7) O10W 0.43(3) 0.051(8) 0.121(11) 0.024(7) 0.078(15) -0.064(13) Gd1 0.0667(4) 0.0434(3) 0.0541(4) 0.0250(3) 0.0322(3) 0.0221(3) Gd2 0.0560(4) 0.0388(3) 0.0374(3) 0.0185(3) 0.0203(3) 0.0180(3) Gd3 0.1039(5) 0.0443(4) 0.0802(5) 0.0345(3) 0.0533(4) 0.0245(4) Cl1 0.0600(19) 0.0502(17) 0.0499(18) 0.0218(15) 0.0170(16) 0.0159(15) Cl2 0.088(2) 0.0517(18) 0.074(2) 0.0306(17) 0.0388(19) 0.0242(18) C61 0.220(13) 0.248(16) 0.109(10) 0.118(10) 0.129(9) 0.186(11) C62 0.23(2) 0.035(11) 0.45(4) 0.043(17) 0.21(2) 0.046(13) C63 0.16(2) 0.22(3) 0.083(14) 0.015(17) 0.062(14) -0.03(2) C64 0.25(2) 0.066(11) 0.116(12) 0.043(9) 0.117(13) 0.033(14) C65 0.23(2) 0.097(12) 0.133(13) 0.069(10) 0.114(13) 0.071(13) C66 0.207(17) 0.094(13) 0.114(12) 0.047(10) 0.112(11) 0.064(12) O21 0.166(12) 0.056(7) 0.180(13) 0.021(8) 0.078(10) 0.033(8) O22 0.297(15) 0.132(9) 0.200(12) 0.116(8) 0.159(11) 0.129(9) C1 0.049(7) 0.054(7) 0.051(7) 0.026(6) 0.026(6) 0.016(6) C2 0.035(7) 0.068(9) 0.082(10) 0.027(8) 0.018(7) 0.003(7) C3 0.059(8) 0.041(7) 0.052(8) 0.010(6) 0.020(7) 0.008(6) C4 0.087(10) 0.025(7) 0.067(9) 0.000(7) 0.037(8) -0.012(7) C5 0.067(8) 0.037(7) 0.044(7) 0.011(6) 0.029(6) 0.013(6) C6 0.068(7) 0.053(7) 0.070(8) 0.037(6) 0.037(6) 0.038(6) C7 0.049(7) 0.061(7) 0.038(7) 0.030(6) 0.013(6) 0.028(6) C8 0.059(8) 0.058(8) 0.047(8) 0.020(6) 0.014(7) 0.018(7) C9 0.058(8) 0.050(7) 0.027(6) 0.009(6) 0.018(6) 0.015(6) C10 0.064(7) 0.063(8) 0.047(7) 0.030(6) 0.037(6) 0.027(6) C11 0.077(8) 0.043(7) 0.035(7) 0.008(6) 0.029(6) 0.021(6) C12 0.069(9) 0.032(6) 0.039(7) 0.008(6) 0.008(7) 0.010(6) C13 0.041(7) 0.062(8) 0.035(7) 0.018(6) 0.005(6) 0.013(6) C14 0.046(8) 0.064(8) 0.052(8) 0.029(6) 0.009(6) 0.016(7) C15 0.062(7) 0.039(6) 0.055(7) 0.021(6) 0.033(6) 0.028(5) C16 0.070(8) 0.033(6) 0.046(7) 0.011(6) 0.027(6) 0.014(6) C17 0.067(9) 0.049(9) 0.047(8) -0.008(7) 0.014(7) -0.006(8) C18 0.039(8) 0.069(10) 0.063(10) 0.010(8) 0.001(7) -0.007(8) C19 0.056(8) 0.078(9) 0.076(9) 0.044(7) 0.036(7) 0.029(7) C20 0.053(7) 0.063(8) 0.075(9) 0.034(7) 0.032(7) 0.028(6) C21 0.049(7) 0.077(7) 0.071(8) 0.054(6) 0.030(6) 0.043(6) C22 0.082(9) 0.050(7) 0.059(8) 0.034(6) 0.029(7) 0.036(6) C23 0.063(8) 0.034(6) 0.043(7) 0.013(6) 0.014(6) 0.011(6) C24 0.063(8) 0.041(7) 0.048(7) 0.019(6) 0.018(7) 0.008(6) C25 0.041(7) 0.042(7) 0.038(6) 0.019(5) 0.014(5) 0.001(6) C26 0.052(7) 0.053(7) 0.041(7) 0.025(6) 0.021(6) 0.019(6) C27 0.056(7) 0.036(6) 0.038(7) 0.014(5) 0.019(6) 0.021(5) C28 0.077(10) 0.046(8) 0.029(7) -0.003(6) 0.015(7) -0.003(8) C29 0.052(8) 0.069(9) 0.030(7) 0.014(7) 0.000(6) -0.002(8) C30 0.051(9) 0.109(12) 0.049(9) 0.028(8) 0.005(7) 0.014(9) C31 0.070(8) 0.061(7) 0.051(7) 0.033(6) 0.031(6) 0.031(6) C32 0.106(11) 0.049(8) 0.051(8) 0.024(6) 0.039(7) 0.014(8) C33 0.064(7) 0.043(7) 0.048(7) 0.010(6) 0.031(6) 0.023(6) C34 0.072(8) 0.058(8) 0.087(10) 0.035(7) 0.045(7) 0.036(6) C35 0.061(8) 0.053(7) 0.091(10) 0.040(7) 0.021(8) 0.030(6) C36 0.086(11) 0.060(9) 0.077(10) 0.026(8) 0.023(9) 0.016(8) C37 0.096(11) 0.055(8) 0.045(7) 0.027(6) 0.026(7) 0.023(8) C38 0.115(10) 0.044(7) 0.067(8) 0.029(6) 0.061(7) 0.033(7) C39 0.063(7) 0.046(7) 0.058(8) 0.025(6) 0.032(6) 0.027(6) C40 0.078(9) 0.061(7) 0.072(8) 0.042(6) 0.036(7) 0.038(7) C41 0.093(9) 0.071(8) 0.085(9) 0.049(7) 0.055(7) 0.054(7) C42 0.087(8) 0.039(7) 0.119(11) 0.031(7) 0.073(7) 0.033(6) C43 0.144(14) 0.038(8) 0.044(8) 0.015(6) 0.042(8) 0.011(9) C44 0.111(13) 0.044(8) 0.047(8) 0.018(7) 0.023(8) 0.006(8) C45 0.052(9) 0.080(11) 0.075(10) 0.029(8) 0.016(8) 0.003(8) C46 0.059(9) 0.079(10) 0.109(12) 0.045(9) 0.034(9) 0.025(8) C47 0.094(9) 0.054(8) 0.075(8) 0.020(7) 0.063(7) 0.023(7) C48 0.087(10) 0.065(9) 0.049(8) 0.018(7) 0.036(7) 0.019(8) C49 0.099(12) 0.064(9) 0.068(9) 0.040(7) 0.033(8) 0.013(9) C50 0.086(10) 0.083(8) 0.064(8) 0.056(7) 0.024(8) 0.042(8) C51 0.106(11) 0.049(7) 0.070(9) 0.041(6) 0.021(9) 0.034(7) C52 0.090(10) 0.072(7) 0.092(9) 0.066(7) 0.035(8) 0.042(7) C53 0.121(10) 0.042(6) 0.092(9) 0.043(6) 0.073(7) 0.050(6) C54 0.124(11) 0.032(7) 0.078(9) 0.017(7) 0.061(8) 0.021(8) C55 0.110(13) 0.028(7) 0.072(10) 0.005(7) 0.025(10) 0.000(8) C56 0.080(12) 0.048(9) 0.083(11) 0.024(8) 0.003(10) -0.011(9) C57 0.076(10) 0.034(7) 0.097(11) 0.017(8) 0.036(9) 0.008(7) C58 0.090(9) 0.079(9) 0.108(10) 0.057(8) 0.067(8) 0.039(8) C59 0.096(9) 0.074(9) 0.074(8) 0.046(7) 0.061(7) 0.035(8) C60 0.097(10) 0.056(8) 0.056(8) 0.023(7) 0.046(7) 0.010(8) N1 0.065(6) 0.055(6) 0.053(6) 0.026(5) 0.022(5) 0.033(5) N2 0.060(7) 0.061(7) 0.053(7) 0.023(6) 0.017(6) 0.016(6) N3 0.057(7) 0.073(8) 0.040(6) 0.012(6) 0.020(5) -0.002(6) N4 0.065(7) 0.048(7) 0.054(7) 0.010(6) 0.021(6) 0.008(6) N5 0.082(7) 0.028(5) 0.061(7) 0.016(5) 0.037(6) 0.010(5) N6 0.068(7) 0.039(5) 0.052(6) 0.026(5) 0.027(5) 0.023(5) N7 0.069(6) 0.039(5) 0.040(6) 0.016(5) 0.021(5) 0.027(5) N8 0.050(6) 0.045(6) 0.042(6) 0.022(5) 0.015(5) 0.014(5) N9 0.054(6) 0.056(6) 0.032(5) 0.019(5) 0.014(5) 0.015(5) N10 0.052(6) 0.047(6) 0.055(6) 0.029(5) 0.019(5) 0.015(5) N11 0.049(6) 0.040(5) 0.037(5) 0.018(4) 0.013(5) 0.009(5) N12 0.052(6) 0.044(5) 0.038(5) 0.021(4) 0.018(5) 0.022(5) N13 0.060(6) 0.029(5) 0.060(6) 0.020(5) 0.027(5) 0.014(5) N14 0.055(6) 0.037(6) 0.035(5) 0.011(5) 0.014(5) 0.000(5) N15 0.055(7) 0.046(6) 0.045(6) 0.001(5) 0.015(5) 0.004(6) N16 0.054(7) 0.078(8) 0.041(6) 0.014(6) 0.007(6) 0.017(6) N17 0.058(7) 0.070(7) 0.056(7) 0.031(6) 0.018(6) 0.023(6) N18 0.057(6) 0.071(7) 0.060(7) 0.033(6) 0.030(5) 0.030(5) N19 0.064(6) 0.051(6) 0.040(6) 0.023(5) 0.020(5) 0.028(5) N20 0.057(6) 0.038(5) 0.036(5) 0.014(4) 0.018(5) 0.018(5) N21 0.082(7) 0.067(6) 0.060(6) 0.045(5) 0.036(6) 0.032(6) N22 0.085(7) 0.066(7) 0.053(6) 0.037(5) 0.036(6) 0.034(6) N23 0.067(7) 0.045(6) 0.041(6) 0.010(5) 0.031(5) 0.003(6) N24 0.084(7) 0.049(6) 0.055(6) 0.026(5) 0.044(5) 0.028(5) N25 0.068(7) 0.047(6) 0.082(8) 0.024(6) 0.037(6) 0.023(5) N26 0.073(8) 0.057(7) 0.062(7) 0.024(6) 0.025(6) 0.013(6) N27 0.089(9) 0.052(7) 0.061(7) 0.022(6) 0.026(7) 0.006(7) N28 0.081(8) 0.054(7) 0.047(7) 0.014(6) 0.021(6) 0.018(6) N29 0.081(7) 0.042(5) 0.072(7) 0.028(5) 0.044(6) 0.036(5) N30 0.088(7) 0.043(5) 0.073(7) 0.034(5) 0.049(6) 0.037(5) N31 0.088(7) 0.056(6) 0.099(8) 0.047(6) 0.057(6) 0.041(6) N32 0.109(8) 0.052(6) 0.079(7) 0.031(6) 0.060(6) 0.044(6) N33 0.116(9) 0.047(6) 0.081(7) 0.033(6) 0.061(7) 0.031(6) N34 0.087(9) 0.039(6) 0.063(8) 0.020(6) 0.013(7) -0.009(7) N35 0.076(8) 0.050(7) 0.071(8) 0.027(6) 0.018(7) 0.008(6) N36 0.072(8) 0.059(7) 0.074(7) 0.036(6) 0.030(6) 0.016(6) N37 0.068(7) 0.038(6) 0.078(8) 0.018(6) 0.034(6) 0.012(6) N38 0.071(8) 0.047(6) 0.065(7) 0.026(6) 0.021(6) 0.017(6) N39 0.090(8) 0.068(7) 0.062(6) 0.041(5) 0.045(6) 0.028(6) N40 0.077(7) 0.077(6) 0.092(7) 0.061(5) 0.054(6) 0.049(5) O1 0.058(5) 0.052(5) 0.065(5) 0.027(4) 0.027(4) 0.021(4) O2 0.069(6) 0.042(5) 0.061(5) 0.021(4) 0.034(4) 0.008(4) O3 0.071(5) 0.041(4) 0.052(5) 0.021(4) 0.030(4) 0.021(4) O4 0.061(5) 0.050(4) 0.044(4) 0.027(4) 0.023(4) 0.025(4) O5 0.058(5) 0.047(4) 0.046(5) 0.026(4) 0.016(4) 0.019(4) O6 0.048(5) 0.039(4) 0.045(5) 0.022(4) 0.015(4) 0.014(4) O7 0.046(5) 0.040(4) 0.047(5) 0.018(4) 0.015(4) 0.013(4) O8 0.044(5) 0.073(6) 0.047(5) 0.018(5) 0.013(4) 0.013(5) O9 0.078(6) 0.060(5) 0.039(5) 0.027(4) 0.023(4) 0.030(4) O10 0.071(6) 0.075(6) 0.057(5) 0.034(5) 0.028(5) 0.035(5) O11 0.097(6) 0.060(5) 0.055(5) 0.034(4) 0.047(4) 0.038(5) O12 0.073(5) 0.041(4) 0.047(5) 0.024(4) 0.030(4) 0.024(4) O13 0.091(7) 0.043(5) 0.074(6) 0.022(5) 0.024(6) 0.012(5) O14 0.058(5) 0.050(5) 0.086(7) 0.030(5) 0.026(5) 0.020(4) O15 0.067(5) 0.043(5) 0.062(5) 0.018(4) 0.032(4) 0.018(4) O16 0.093(7) 0.047(5) 0.085(6) 0.029(5) 0.047(5) 0.023(5) O17 0.086(7) 0.043(5) 0.077(6) 0.019(5) 0.038(5) 0.003(5) O18 0.100(7) 0.045(5) 0.087(7) 0.035(5) 0.042(6) 0.017(5) O19 0.115(7) 0.035(4) 0.086(6) 0.033(4) 0.051(6) 0.025(5) O20 0.115(7) 0.066(5) 0.069(6) 0.042(5) 0.045(5) 0.050(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl6 Cl7 1.41(2) 2_875 ? Cl7 Cl6 1.41(2) 2_875 ? Cl11 Cl11 2.39(4) 2_866 ? O1W Gd2 2.361(9) . ? O2W Gd2 2.360(9) . ? O3W Gd2 2.426(10) . ? O4W Gd1 2.454(11) . ? O5W Gd3 2.456(12) . ? O6W Gd1 2.500(11) . ? O7W Gd2 2.432(10) . ? O8W Gd1 2.476(14) . ? O9W Gd3 2.450(15) . ? O10W Gd3 2.467(14) . ? Gd1 O2 2.446(8) . ? Gd1 O4 2.473(9) . ? Gd1 O1 2.476(10) . ? Gd1 O5 2.485(8) . ? Gd1 O3 2.534(9) . ? Gd1 Cl1 2.721(4) . ? Gd2 O7 2.355(9) . ? Gd2 O11 2.358(10) . ? Gd2 O12 2.376(8) . ? Gd2 O6 2.383(9) . ? Gd3 O17 2.468(12) . ? Gd3 O16 2.485(11) . ? Gd3 O19 2.485(12) . ? Gd3 O20 2.491(10) . ? Gd3 O18 2.509(11) . ? Gd3 Cl2 2.707(4) . ? C61 O21 1.340(14) . ? C61 C66 1.368(5) . ? C61 C62 1.446(4) . ? C62 C63 1.398(4) . ? C62 H62 0.9400 . ? C63 C64 1.368(5) . ? C63 H63 0.9400 . ? C64 O22 1.421(17) . ? C64 C65 1.423(4) . ? C65 C66 1.380(5) . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? O21 H21 0.8300 . ? O22 H22 0.8300 . ? C1 O1 1.211(18) . ? C1 N1 1.341(17) . ? C1 N2 1.403(17) . ? C2 N2 1.422(17) . ? C2 N3 1.44(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 O2 1.229(18) . ? C3 N3 1.35(2) . ? C3 N4 1.356(19) . ? C4 N5 1.429(18) . ? C4 N4 1.45(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 O3 1.240(17) . ? C5 N6 1.320(17) . ? C5 N5 1.350(16) . ? C6 N10 1.436(16) . ? C6 N6 1.457(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O4 1.243(16) . ? C7 N9 1.343(16) . ? C7 N10 1.357(18) . ? C8 N8 1.450(18) . ? C8 N9 1.461(18) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 O5 1.256(16) . ? C9 N8 1.344(16) . ? C9 N7 1.367(19) . ? C10 N7 1.407(17) . ? C10 N1 1.444(15) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 N7 1.438(17) . ? C11 N19 1.459(18) . ? C11 C12 1.52(2) . ? C11 H11 0.9900 . ? C12 N8 1.455(17) . ? C12 N20 1.459(18) . ? C12 H12 0.9900 . ? C13 N11 1.456(18) . ? C13 N9 1.456(18) . ? C13 C14 1.542(19) . ? C13 H13 0.9900 . ? C14 N10 1.433(18) . ? C14 N12 1.456(18) . ? C14 H14 0.9900 . ? C15 N6 1.465(18) . ? C15 N13 1.468(17) . ? C15 C16 1.534(17) . ? C15 H15 0.9900 . ? C16 N14 1.464(18) . ? C16 N5 1.467(19) . ? C16 H16 0.9900 . ? C17 N15 1.45(2) . ? C17 N4 1.45(2) . ? C17 C18 1.53(2) . ? C17 H17 0.9900 . ? C18 N16 1.45(2) . ? C18 N3 1.46(2) . ? C18 H18 0.9900 . ? C19 N2 1.41(2) . ? C19 N17 1.45(2) . ? C19 C20 1.604(18) . ? C19 H19 0.9900 . ? C20 N1 1.42(2) . ? C20 N18 1.464(19) . ? C20 H20 0.9900 . ? C21 O10 1.226(18) . ? C21 N17 1.343(16) . ? C21 N18 1.360(18) . ? C22 N19 1.433(18) . ? C22 N18 1.442(16) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 O9 1.246(17) . ? C23 N20 1.364(18) . ? C23 N19 1.365(19) . ? C24 N20 1.430(18) . ? C24 N11 1.473(17) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O6 1.230(16) . ? C25 N11 1.360(16) . ? C25 N12 1.366(17) . ? C26 N12 1.426(16) . ? C26 N13 1.434(15) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 O7 1.215(16) . ? C27 N13 1.339(17) . ? C27 N14 1.362(14) . ? C28 N15 1.43(2) . ? C28 N14 1.436(18) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 O8 1.229(18) . ? C29 N15 1.34(2) . ? C29 N16 1.37(2) . ? C30 N16 1.42(2) . ? C30 N17 1.465(18) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 O11 1.245(18) . ? C31 N22 1.341(19) . ? C31 N21 1.351(19) . ? C32 N22 1.44(2) . ? C32 N23 1.444(19) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 O15 1.238(17) . ? C33 N24 1.344(17) . ? C33 N23 1.358(18) . ? C34 N25 1.425(17) . ? C34 N24 1.483(19) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 O14 1.224(17) . ? C35 N26 1.351(17) . ? C35 N25 1.39(2) . ? C36 N27 1.42(2) . ? C36 N26 1.47(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O13 1.227(16) . ? C37 N27 1.38(2) . ? C37 N28 1.39(2) . ? C38 N28 1.43(2) . ? C38 N29 1.440(19) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 O12 1.221(16) . ? C39 N29 1.360(15) . ? C39 N30 1.378(19) . ? C40 N30 1.438(16) . ? C40 N21 1.48(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 N30 1.442(18) . ? C41 N31 1.45(2) . ? C41 C42 1.59(2) . ? C41 H41 0.9900 . ? C42 N32 1.445(19) . ? C42 N29 1.462(19) . ? C42 H42 0.9900 . ? C43 N33 1.41(2) . ? C43 N28 1.438(17) . ? C43 C44 1.56(3) . ? C43 H43 0.9900 . ? C44 N34 1.44(2) . ? C44 N27 1.455(18) . ? C44 H44 0.9900 . ? C45 N35 1.42(2) . ? C45 N26 1.47(2) . ? C45 C46 1.58(2) . ? C45 H45 0.9900 . ? C46 N25 1.432(18) . ? C46 N36 1.44(2) . ? C46 H46 0.9900 . ? C47 N37 1.423(17) . ? C47 N24 1.46(2) . ? C47 C48 1.55(2) . ? C47 H47 0.9900 . ? C48 N38 1.41(2) . ? C48 N23 1.43(2) . ? C48 H48 0.9900 . ? C49 N39 1.408(19) . ? C49 N22 1.48(2) . ? C49 C50 1.50(2) . ? C49 H49 0.9900 . ? C50 N40 1.449(17) . ? C50 N21 1.46(2) . ? C50 H50 0.9900 . ? C51 O20 1.244(17) . ? C51 N39 1.340(18) . ? C51 N40 1.35(2) . ? C52 N40 1.44(2) . ? C52 N31 1.46(2) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 O19 1.225(19) . ? C53 N32 1.36(2) . ? C53 N31 1.372(18) . ? C54 N32 1.406(18) . ? C54 N33 1.46(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 O18 1.23(2) . ? C55 N33 1.36(2) . ? C55 N34 1.38(2) . ? C56 N34 1.41(2) . ? C56 N35 1.44(2) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C57 O17 1.24(2) . ? C57 N35 1.34(2) . ? C57 N36 1.35(2) . ? C58 N37 1.426(18) . ? C58 N36 1.46(2) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 O16 1.251(18) . ? C59 N38 1.330(17) . ? C59 N37 1.36(2) . ? C60 N38 1.42(2) . ? C60 N39 1.49(2) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Gd1 O4W 76.4(3) . . ? O2 Gd1 O4 136.7(3) . . ? O4W Gd1 O4 138.5(3) . . ? O2 Gd1 O1 71.7(3) . . ? O4W Gd1 O1 64.8(4) . . ? O4 Gd1 O1 138.0(3) . . ? O2 Gd1 O8W 83.1(4) . . ? O4W Gd1 O8W 67.0(5) . . ? O4 Gd1 O8W 89.7(4) . . ? O1 Gd1 O8W 129.4(4) . . ? O2 Gd1 O5 137.8(3) . . ? O4W Gd1 O5 98.2(3) . . ? O4 Gd1 O5 73.1(3) . . ? O1 Gd1 O5 68.4(3) . . ? O8W Gd1 O5 133.9(4) . . ? O2 Gd1 O6W 142.0(3) . . ? O4W Gd1 O6W 70.5(4) . . ? O4 Gd1 O6W 68.8(3) . . ? O1 Gd1 O6W 108.9(4) . . ? O8W Gd1 O6W 67.2(4) . . ? O5 Gd1 O6W 66.8(3) . . ? O2 Gd1 O3 69.9(3) . . ? O4W Gd1 O3 120.4(3) . . ? O4 Gd1 O3 69.3(3) . . ? O1 Gd1 O3 137.8(3) . . ? O8W Gd1 O3 61.5(4) . . ? O5 Gd1 O3 139.2(3) . . ? O6W Gd1 O3 111.9(4) . . ? O2 Gd1 Cl1 79.5(2) . . ? O4W Gd1 Cl1 141.3(3) . . ? O4 Gd1 Cl1 78.5(2) . . ? O1 Gd1 Cl1 79.0(3) . . ? O8W Gd1 Cl1 139.0(4) . . ? O5 Gd1 Cl1 80.0(2) . . ? O6W Gd1 Cl1 138.4(3) . . ? O3 Gd1 Cl1 77.6(2) . . ? O7 Gd2 O11 135.8(3) . . ? O7 Gd2 O2W 79.8(3) . . ? O11 Gd2 O2W 116.8(4) . . ? O7 Gd2 O1W 113.0(3) . . ? O11 Gd2 O1W 81.6(3) . . ? O2W Gd2 O1W 139.5(3) . . ? O7 Gd2 O12 146.3(3) . . ? O11 Gd2 O12 75.9(3) . . ? O2W Gd2 O12 73.6(3) . . ? O1W Gd2 O12 77.3(3) . . ? O7 Gd2 O6 75.2(3) . . ? O11 Gd2 O6 146.4(3) . . ? O2W Gd2 O6 75.2(3) . . ? O1W Gd2 O6 71.8(3) . . ? O12 Gd2 O6 78.4(3) . . ? O7 Gd2 O3W 71.1(3) . . ? O11 Gd2 O3W 75.2(4) . . ? O2W Gd2 O3W 145.2(3) . . ? O1W Gd2 O3W 71.8(3) . . ? O12 Gd2 O3W 140.1(3) . . ? O6 Gd2 O3W 113.8(3) . . ? O7 Gd2 O7W 74.0(4) . . ? O11 Gd2 O7W 73.5(4) . . ? O2W Gd2 O7W 72.1(3) . . ? O1W Gd2 O7W 147.4(4) . . ? O12 Gd2 O7W 115.5(4) . . ? O6 Gd2 O7W 138.2(3) . . ? O3W Gd2 O7W 81.6(4) . . ? O9W Gd3 O5W 70.7(5) . . ? O9W Gd3 O10W 67.5(6) . . ? O5W Gd3 O10W 64.9(5) . . ? O9W Gd3 O17 142.3(4) . . ? O5W Gd3 O17 78.7(4) . . ? O10W Gd3 O17 80.1(7) . . ? O9W Gd3 O16 111.7(5) . . ? O5W Gd3 O16 63.4(3) . . ? O10W Gd3 O16 124.3(6) . . ? O17 Gd3 O16 71.0(3) . . ? O9W Gd3 O19 67.6(5) . . ? O5W Gd3 O19 138.1(4) . . ? O10W Gd3 O19 95.3(7) . . ? O17 Gd3 O19 136.8(4) . . ? O16 Gd3 O19 137.8(3) . . ? O9W Gd3 O20 68.4(4) . . ? O5W Gd3 O20 95.9(4) . . ? O10W Gd3 O20 135.6(6) . . ? O17 Gd3 O20 137.7(3) . . ? O16 Gd3 O20 69.3(4) . . ? O19 Gd3 O20 72.2(4) . . ? O9W Gd3 O18 109.3(5) . . ? O5W Gd3 O18 122.9(3) . . ? O10W Gd3 O18 63.7(5) . . ? O17 Gd3 O18 70.0(4) . . ? O16 Gd3 O18 137.5(4) . . ? O19 Gd3 O18 69.6(4) . . ? O20 Gd3 O18 138.8(4) . . ? O9W Gd3 Cl2 138.5(3) . . ? O5W Gd3 Cl2 140.3(3) . . ? O10W Gd3 Cl2 141.2(4) . . ? O17 Gd3 Cl2 79.1(3) . . ? O16 Gd3 Cl2 78.3(3) . . ? O19 Gd3 Cl2 78.4(2) . . ? O20 Gd3 Cl2 79.4(3) . . ? O18 Gd3 Cl2 78.5(2) . . ? O21 C61 C66 121.1(5) . . ? O21 C61 C62 121.8(5) . . ? C66 C61 C62 117.1(4) . . ? C63 C62 C61 117.4(3) . . ? C63 C62 H62 121.3 . . ? C61 C62 H62 121.3 . . ? C64 C63 C62 121.0(3) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C63 C64 O22 120.1(7) . . ? C63 C64 C65 124.2(4) . . ? O22 C64 C65 115.5(7) . . ? C66 C65 C64 112.0(5) . . ? C66 C65 H65 124.0 . . ? C64 C65 H65 124.0 . . ? C61 C66 C65 128.2(4) . . ? C61 C66 H66 115.9 . . ? C65 C66 H66 115.9 . . ? C61 O21 H21 109.5 . . ? C64 O22 H22 109.5 . . ? O1 C1 N1 129.4(12) . . ? O1 C1 N2 124.0(12) . . ? N1 C1 N2 106.6(12) . . ? N2 C2 N3 114.8(12) . . ? N2 C2 H2A 108.6 . . ? N3 C2 H2A 108.6 . . ? N2 C2 H2B 108.6 . . ? N3 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? O2 C3 N3 125.1(14) . . ? O2 C3 N4 126.1(15) . . ? N3 C3 N4 108.6(13) . . ? N5 C4 N4 114.1(11) . . ? N5 C4 H4A 108.7 . . ? N4 C4 H4A 108.7 . . ? N5 C4 H4B 108.7 . . ? N4 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? O3 C5 N6 126.8(12) . . ? O3 C5 N5 123.6(12) . . ? N6 C5 N5 109.4(12) . . ? N10 C6 N6 113.4(11) . . ? N10 C6 H6A 108.9 . . ? N6 C6 H6A 108.9 . . ? N10 C6 H6B 108.9 . . ? N6 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O4 C7 N9 125.8(12) . . ? O4 C7 N10 125.3(12) . . ? N9 C7 N10 108.7(12) . . ? N8 C8 N9 112.3(11) . . ? N8 C8 H8A 109.1 . . ? N9 C8 H8A 109.1 . . ? N8 C8 H8B 109.1 . . ? N9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? O5 C9 N8 125.3(13) . . ? O5 C9 N7 124.5(12) . . ? N8 C9 N7 109.9(12) . . ? N7 C10 N1 114.8(11) . . ? N7 C10 H10A 108.6 . . ? N1 C10 H10A 108.6 . . ? N7 C10 H10B 108.6 . . ? N1 C10 H10B 108.6 . . ? H10A C10 H10B 107.5 . . ? N7 C11 N19 114.5(9) . . ? N7 C11 C12 105.3(12) . . ? N19 C11 C12 103.7(11) . . ? N7 C11 H11 111.0 . . ? N19 C11 H11 111.0 . . ? C12 C11 H11 111.0 . . ? N8 C12 N20 114.0(11) . . ? N8 C12 C11 102.8(11) . . ? N20 C12 C11 104.3(11) . . ? N8 C12 H12 111.7 . . ? N20 C12 H12 111.7 . . ? C11 C12 H12 111.7 . . ? N11 C13 N9 114.7(11) . . ? N11 C13 C14 103.3(10) . . ? N9 C13 C14 103.2(11) . . ? N11 C13 H13 111.7 . . ? N9 C13 H13 111.7 . . ? C14 C13 H13 111.7 . . ? N10 C14 N12 116.3(10) . . ? N10 C14 C13 103.0(12) . . ? N12 C14 C13 103.4(12) . . ? N10 C14 H14 111.2 . . ? N12 C14 H14 111.2 . . ? C13 C14 H14 111.2 . . ? N6 C15 N13 114.2(10) . . ? N6 C15 C16 102.3(11) . . ? N13 C15 C16 104.0(11) . . ? N6 C15 H15 111.9 . . ? N13 C15 H15 111.9 . . ? C16 C15 H15 111.9 . . ? N14 C16 N5 114.1(12) . . ? N14 C16 C15 103.2(10) . . ? N5 C16 C15 103.0(11) . . ? N14 C16 H16 111.9 . . ? N5 C16 H16 111.9 . . ? C15 C16 H16 111.9 . . ? N15 C17 N4 115.6(12) . . ? N15 C17 C18 103.5(13) . . ? N4 C17 C18 103.5(13) . . ? N15 C17 H17 111.2 . . ? N4 C17 H17 111.2 . . ? C18 C17 H17 111.2 . . ? N16 C18 N3 115.9(11) . . ? N16 C18 C17 104.4(13) . . ? N3 C18 C17 102.9(13) . . ? N16 C18 H18 111.1 . . ? N3 C18 H18 111.1 . . ? C17 C18 H18 111.1 . . ? N2 C19 N17 117.8(13) . . ? N2 C19 C20 103.2(12) . . ? N17 C19 C20 102.7(11) . . ? N2 C19 H19 110.8 . . ? N17 C19 H19 110.8 . . ? C20 C19 H19 110.8 . . ? N1 C20 N18 115.4(12) . . ? N1 C20 C19 101.1(11) . . ? N18 C20 C19 101.1(11) . . ? N1 C20 H20 112.7 . . ? N18 C20 H20 112.7 . . ? C19 C20 H20 112.7 . . ? O10 C21 N17 125.4(13) . . ? O10 C21 N18 125.1(12) . . ? N17 C21 N18 109.4(13) . . ? N19 C22 N18 114.7(11) . . ? N19 C22 H22A 108.6 . . ? N18 C22 H22A 108.6 . . ? N19 C22 H22B 108.6 . . ? N18 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? O9 C23 N20 124.8(14) . . ? O9 C23 N19 126.2(13) . . ? N20 C23 N19 109.0(12) . . ? N20 C24 N11 113.9(10) . . ? N20 C24 H24A 108.8 . . ? N11 C24 H24A 108.8 . . ? N20 C24 H24B 108.8 . . ? N11 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? O6 C25 N11 126.1(12) . . ? O6 C25 N12 125.1(11) . . ? N11 C25 N12 108.8(12) . . ? N12 C26 N13 113.6(11) . . ? N12 C26 H26A 108.8 . . ? N13 C26 H26A 108.8 . . ? N12 C26 H26B 108.8 . . ? N13 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? O7 C27 N13 125.0(11) . . ? O7 C27 N14 124.1(12) . . ? N13 C27 N14 110.9(11) . . ? N15 C28 N14 115.3(11) . . ? N15 C28 H28A 108.4 . . ? N14 C28 H28A 108.4 . . ? N15 C28 H28B 108.4 . . ? N14 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? O8 C29 N15 126.0(15) . . ? O8 C29 N16 123.9(15) . . ? N15 C29 N16 110.1(14) . . ? N16 C30 N17 114.8(13) . . ? N16 C30 H30A 108.6 . . ? N17 C30 H30A 108.6 . . ? N16 C30 H30B 108.6 . . ? N17 C30 H30B 108.6 . . ? H30A C30 H30B 107.5 . . ? O11 C31 N22 125.3(14) . . ? O11 C31 N21 123.6(14) . . ? N22 C31 N21 111.1(13) . . ? N22 C32 N23 115.4(11) . . ? N22 C32 H32A 108.4 . . ? N23 C32 H32A 108.4 . . ? N22 C32 H32B 108.4 . . ? N23 C32 H32B 108.4 . . ? H32A C32 H32B 107.5 . . ? O15 C33 N24 125.9(14) . . ? O15 C33 N23 126.4(12) . . ? N24 C33 N23 107.7(13) . . ? N25 C34 N24 114.5(12) . . ? N25 C34 H34A 108.6 . . ? N24 C34 H34A 108.6 . . ? N25 C34 H34B 108.6 . . ? N24 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? O14 C35 N26 126.9(16) . . ? O14 C35 N25 124.7(13) . . ? N26 C35 N25 108.3(12) . . ? N27 C36 N26 113.3(15) . . ? N27 C36 H36A 108.9 . . ? N26 C36 H36A 108.9 . . ? N27 C36 H36B 108.9 . . ? N26 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? O13 C37 N27 126.1(16) . . ? O13 C37 N28 124.4(15) . . ? N27 C37 N28 109.5(12) . . ? N28 C38 N29 115.0(13) . . ? N28 C38 H38A 108.5 . . ? N29 C38 H38A 108.5 . . ? N28 C38 H38B 108.5 . . ? N29 C38 H38B 108.5 . . ? H38A C38 H38B 107.5 . . ? O12 C39 N29 124.7(13) . . ? O12 C39 N30 124.7(11) . . ? N29 C39 N30 110.5(12) . . ? N30 C40 N21 112.2(11) . . ? N30 C40 H40A 109.2 . . ? N21 C40 H40A 109.2 . . ? N30 C40 H40B 109.2 . . ? N21 C40 H40B 109.2 . . ? H40A C40 H40B 107.9 . . ? N30 C41 N31 114.2(13) . . ? N30 C41 C42 102.8(12) . . ? N31 C41 C42 101.2(11) . . ? N30 C41 H41 112.6 . . ? N31 C41 H41 112.6 . . ? C42 C41 H41 112.6 . . ? N32 C42 N29 114.7(13) . . ? N32 C42 C41 103.6(13) . . ? N29 C42 C41 103.3(11) . . ? N32 C42 H42 111.5 . . ? N29 C42 H42 111.5 . . ? C41 C42 H42 111.5 . . ? N33 C43 N28 115.9(13) . . ? N33 C43 C44 103.9(14) . . ? N28 C43 C44 104.9(13) . . ? N33 C43 H43 110.6 . . ? N28 C43 H43 110.6 . . ? C44 C43 H43 110.6 . . ? N34 C44 N27 114.4(13) . . ? N34 C44 C43 102.7(14) . . ? N27 C44 C43 102.9(12) . . ? N34 C44 H44 112.0 . . ? N27 C44 H44 112.0 . . ? C43 C44 H44 112.0 . . ? N35 C45 N26 115.1(14) . . ? N35 C45 C46 103.3(14) . . ? N26 C45 C46 101.7(11) . . ? N35 C45 H45 112.0 . . ? N26 C45 H45 112.0 . . ? C46 C45 H45 112.0 . . ? N25 C46 N36 116.7(13) . . ? N25 C46 C45 104.1(14) . . ? N36 C46 C45 101.8(13) . . ? N25 C46 H46 111.2 . . ? N36 C46 H46 111.2 . . ? C45 C46 H46 111.2 . . ? N37 C47 N24 115.8(12) . . ? N37 C47 C48 102.5(13) . . ? N24 C47 C48 101.2(12) . . ? N37 C47 H47 112.1 . . ? N24 C47 H47 112.1 . . ? C48 C47 H47 112.1 . . ? N38 C48 N23 117.4(14) . . ? N38 C48 C47 103.8(11) . . ? N23 C48 C47 103.8(13) . . ? N38 C48 H48 110.4 . . ? N23 C48 H48 110.4 . . ? C47 C48 H48 110.4 . . ? N39 C49 N22 114.6(14) . . ? N39 C49 C50 106.1(12) . . ? N22 C49 C50 104.0(13) . . ? N39 C49 H49 110.6 . . ? N22 C49 H49 110.6 . . ? C50 C49 H49 110.6 . . ? N40 C50 N21 112.2(11) . . ? N40 C50 C49 101.5(13) . . ? N21 C50 C49 104.2(13) . . ? N40 C50 H50 112.7 . . ? N21 C50 H50 112.7 . . ? C49 C50 H50 112.7 . . ? O20 C51 N39 125.0(17) . . ? O20 C51 N40 126.1(15) . . ? N39 C51 N40 108.9(12) . . ? N40 C52 N31 113.3(13) . . ? N40 C52 H52A 108.9 . . ? N31 C52 H52A 108.9 . . ? N40 C52 H52B 108.9 . . ? N31 C52 H52B 108.9 . . ? H52A C52 H52B 107.7 . . ? O19 C53 N32 125.8(13) . . ? O19 C53 N31 126.0(15) . . ? N32 C53 N31 108.1(13) . . ? N32 C54 N33 115.1(12) . . ? N32 C54 H54A 108.5 . . ? N33 C54 H54A 108.5 . . ? N32 C54 H54B 108.5 . . ? N33 C54 H54B 108.5 . . ? H54A C54 H54B 107.5 . . ? O18 C55 N33 127.8(18) . . ? O18 C55 N34 123.6(18) . . ? N33 C55 N34 108.6(15) . . ? N34 C56 N35 114.1(12) . . ? N34 C56 H56A 108.7 . . ? N35 C56 H56A 108.7 . . ? N34 C56 H56B 108.7 . . ? N35 C56 H56B 108.7 . . ? H56A C56 H56B 107.6 . . ? O17 C57 N35 125.4(15) . . ? O17 C57 N36 124.8(17) . . ? N35 C57 N36 109.6(15) . . ? N37 C58 N36 115.9(14) . . ? N37 C58 H58A 108.3 . . ? N36 C58 H58A 108.3 . . ? N37 C58 H58B 108.3 . . ? N36 C58 H58B 108.3 . . ? H58A C58 H58B 107.4 . . ? O16 C59 N38 126.0(16) . . ? O16 C59 N37 124.2(13) . . ? N38 C59 N37 109.8(13) . . ? N38 C60 N39 112.9(13) . . ? N38 C60 H60A 109.0 . . ? N39 C60 H60A 109.0 . . ? N38 C60 H60B 109.0 . . ? N39 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? C1 N1 C20 115.8(11) . . ? C1 N1 C10 120.4(12) . . ? C20 N1 C10 123.8(11) . . ? C1 N2 C19 113.2(11) . . ? C1 N2 C2 121.1(13) . . ? C19 N2 C2 125.5(12) . . ? C3 N3 C2 123.9(13) . . ? C3 N3 C18 112.3(13) . . ? C2 N3 C18 123.6(14) . . ? C3 N4 C4 123.1(14) . . ? C3 N4 C17 112.1(13) . . ? C4 N4 C17 124.8(13) . . ? C5 N5 C4 122.8(13) . . ? C5 N5 C16 111.6(11) . . ? C4 N5 C16 125.4(12) . . ? C5 N6 C6 121.8(12) . . ? C5 N6 C15 113.2(10) . . ? C6 N6 C15 125.0(11) . . ? C9 N7 C10 124.2(12) . . ? C9 N7 C11 110.1(11) . . ? C10 N7 C11 125.6(12) . . ? C9 N8 C8 123.1(12) . . ? C9 N8 C12 111.6(12) . . ? C8 N8 C12 125.0(11) . . ? C7 N9 C13 111.8(11) . . ? C7 N9 C8 122.7(12) . . ? C13 N9 C8 125.5(11) . . ? C7 N10 C14 112.8(11) . . ? C7 N10 C6 122.8(12) . . ? C14 N10 C6 124.3(12) . . ? C25 N11 C13 112.3(11) . . ? C25 N11 C24 122.4(12) . . ? C13 N11 C24 124.9(10) . . ? C25 N12 C26 124.5(11) . . ? C25 N12 C14 112.1(10) . . ? C26 N12 C14 123.3(11) . . ? C27 N13 C26 124.9(11) . . ? C27 N13 C15 110.8(10) . . ? C26 N13 C15 124.0(11) . . ? C27 N14 C28 123.5(12) . . ? C27 N14 C16 111.0(10) . . ? C28 N14 C16 125.4(10) . . ? C29 N15 C28 124.6(13) . . ? C29 N15 C17 111.5(13) . . ? C28 N15 C17 123.8(13) . . ? C29 N16 C30 124.3(14) . . ? C29 N16 C18 110.4(13) . . ? C30 N16 C18 124.2(13) . . ? C21 N17 C19 113.3(11) . . ? C21 N17 C30 123.0(13) . . ? C19 N17 C30 123.3(12) . . ? C21 N18 C22 122.9(12) . . ? C21 N18 C20 113.2(10) . . ? C22 N18 C20 123.9(12) . . ? C23 N19 C22 122.0(12) . . ? C23 N19 C11 111.6(11) . . ? C22 N19 C11 126.2(12) . . ? C23 N20 C24 122.7(12) . . ? C23 N20 C12 111.2(12) . . ? C24 N20 C12 125.7(11) . . ? C31 N21 C50 110.6(13) . . ? C31 N21 C40 123.5(13) . . ? C50 N21 C40 125.9(13) . . ? C31 N22 C32 123.1(13) . . ? C31 N22 C49 110.0(13) . . ? C32 N22 C49 125.8(13) . . ? C33 N23 C48 113.3(12) . . ? C33 N23 C32 122.9(12) . . ? C48 N23 C32 123.6(13) . . ? C33 N24 C47 113.8(12) . . ? C33 N24 C34 122.2(13) . . ? C47 N24 C34 123.7(12) . . ? C35 N25 C34 122.3(12) . . ? C35 N25 C46 112.4(12) . . ? C34 N25 C46 125.1(14) . . ? C35 N26 C36 121.6(13) . . ? C35 N26 C45 113.3(13) . . ? C36 N26 C45 125.0(11) . . ? C37 N27 C36 123.3(13) . . ? C37 N27 C44 111.6(14) . . ? C36 N27 C44 125.1(13) . . ? C37 N28 C38 122.9(12) . . ? C37 N28 C43 110.8(13) . . ? C38 N28 C43 125.7(14) . . ? C39 N29 C38 123.6(12) . . ? C39 N29 C42 111.2(12) . . ? C38 N29 C42 124.7(11) . . ? C39 N30 C40 123.8(11) . . ? C39 N30 C41 112.1(11) . . ? C40 N30 C41 124.1(13) . . ? C53 N31 C41 114.0(13) . . ? C53 N31 C52 121.0(13) . . ? C41 N31 C52 125.0(12) . . ? C53 N32 C54 123.3(13) . . ? C53 N32 C42 112.7(12) . . ? C54 N32 C42 124.1(14) . . ? C55 N33 C43 112.5(15) . . ? C55 N33 C54 120.6(15) . . ? C43 N33 C54 126.8(15) . . ? C55 N34 C56 122.7(15) . . ? C55 N34 C44 111.7(15) . . ? C56 N34 C44 125.4(15) . . ? C57 N35 C45 112.5(13) . . ? C57 N35 C56 123.5(14) . . ? C45 N35 C56 124.0(14) . . ? C57 N36 C46 112.5(14) . . ? C57 N36 C58 124.2(15) . . ? C46 N36 C58 123.3(13) . . ? C59 N37 C47 111.5(12) . . ? C59 N37 C58 124.0(12) . . ? C47 N37 C58 124.3(14) . . ? C59 N38 C48 112.0(14) . . ? C59 N38 C60 120.7(13) . . ? C48 N38 C60 126.9(11) . . ? C51 N39 C49 110.9(14) . . ? C51 N39 C60 122.8(12) . . ? C49 N39 C60 125.9(12) . . ? C51 N40 C52 122.8(12) . . ? C51 N40 C50 112.0(12) . . ? C52 N40 C50 125.0(13) . . ? C1 O1 Gd1 136.9(10) . . ? C3 O2 Gd1 133.0(8) . . ? C5 O3 Gd1 134.7(9) . . ? C7 O4 Gd1 133.1(8) . . ? C9 O5 Gd1 130.5(8) . . ? C25 O6 Gd2 153.4(8) . . ? C27 O7 Gd2 154.9(8) . . ? C31 O11 Gd2 158.4(10) . . ? C39 O12 Gd2 155.7(9) . . ? C59 O16 Gd3 134.6(11) . . ? C57 O17 Gd3 135.2(10) . . ? C55 O18 Gd3 135.2(9) . . ? C53 O19 Gd3 133.7(10) . . ? C51 O20 Gd3 133.8(10) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.288 _refine_diff_density_min -1.908 _refine_diff_density_rms 0.131 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.026 -0.087 0.410 2553 960 ' ' _platon_squeeze_details ; ; data_05 _database_code_depnum_ccdc_archive 'CCDC 875769' #TrackingRef 'submit-05.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H62 Dy N23 O34' _chemical_formula_weight 1523.59 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 61' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, x, z+1/6' 'y, -x+y, z+5/6' _cell_length_a 14.4478(18) _cell_length_b 14.4478(18) _cell_length_c 46.109(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8335(3) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4662 _exptl_absorpt_coefficient_mu 1.469 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.6588 _exptl_absorpt_correction_T_max 0.7478 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58125 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10420 _reflns_number_gt 9570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+11.4862P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(9) _chemical_absolute_configuration ' R ' _refine_ls_number_reflns 10420 _refine_ls_number_parameters 706 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.33112(2) 0.54014(2) 0.596953(17) 0.01964(8) Uani 1 1 d . . . O1W O 0.3102(4) 0.6831(4) 0.58002(10) 0.0319(10) Uani 1 1 d . . . O2W O 0.1500(3) 0.4883(3) 0.59688(13) 0.0341(10) Uani 1 1 d . . . O3W O 0.4434(3) 0.4672(4) 0.59903(12) 0.0342(10) Uani 1 1 d . . . O4W O 0.5067(4) 0.6799(4) 0.60741(11) 0.0372(12) Uani 1 1 d . . . C1 C 0.4159(5) 0.6177(5) 0.52662(14) 0.0232(13) Uani 1 1 d . . . C2 C 0.2214(5) 0.5118(5) 0.51993(13) 0.0229(13) Uani 1 1 d . . . H2A H 0.2160 0.5341 0.5396 0.028 Uiso 1 1 calc R . . H2B H 0.1709 0.5206 0.5077 0.028 Uiso 1 1 calc R . . C3 C 0.2085(5) 0.3504(5) 0.54245(14) 0.0231(13) Uani 1 1 d . . . C4 C 0.1695(5) 0.1685(5) 0.55438(15) 0.0296(14) Uani 1 1 d . . . H4A H 0.1654 0.1912 0.5741 0.036 Uiso 1 1 calc R . . H4B H 0.1025 0.1022 0.5504 0.036 Uiso 1 1 calc R . . C5 C 0.3442(5) 0.1963(5) 0.57088(13) 0.0252(13) Uani 1 1 d . . . C6 C 0.5091(6) 0.1923(6) 0.57992(15) 0.0300(15) Uani 1 1 d . . . H6A H 0.5171 0.1290 0.5811 0.036 Uiso 1 1 calc R . . H6B H 0.4979 0.2101 0.5996 0.036 Uiso 1 1 calc R . . C7 C 0.6432(5) 0.3847(5) 0.57607(13) 0.0219(13) Uani 1 1 d . . . C8 C 0.7850(5) 0.5651(5) 0.56136(13) 0.0222(13) Uani 1 1 d . . . H8A H 0.8613 0.5933 0.5578 0.027 Uiso 1 1 calc R . . H8B H 0.7774 0.5868 0.5809 0.027 Uiso 1 1 calc R . . C9 C 0.6807(5) 0.6523(5) 0.54897(14) 0.0231(13) Uani 1 1 d . . . C10 C 0.6051(4) 0.7555(4) 0.52588(13) 0.0195(12) Uani 1 1 d . . . H10A H 0.5896 0.7667 0.5458 0.023 Uiso 1 1 calc R . . H10B H 0.6399 0.8250 0.5161 0.023 Uiso 1 1 calc R . . C11 C 0.4803(4) 0.7000(4) 0.48172(13) 0.0178(12) Uani 1 1 d . . . H11 H 0.5004 0.7751 0.4778 0.021 Uiso 1 1 calc R . . C12 C 0.7409(4) 0.7180(4) 0.50175(13) 0.0194(12) Uani 1 1 d . . . H12 H 0.7937 0.7924 0.4963 0.023 Uiso 1 1 calc R . . C13 C 0.7962(5) 0.6563(5) 0.51265(14) 0.0231(13) Uani 1 1 d . . . H13 H 0.8742 0.7043 0.5148 0.028 Uiso 1 1 calc R . . C14 C 0.7575(5) 0.3929(5) 0.53960(13) 0.0223(12) Uani 1 1 d . . . H14 H 0.8312 0.4066 0.5424 0.027 Uiso 1 1 calc R . . C15 C 0.6708(5) 0.2713(5) 0.54514(12) 0.0222(13) Uani 1 1 d . . . H15 H 0.7042 0.2290 0.5513 0.027 Uiso 1 1 calc R . . C16 C 0.3729(5) 0.0827(5) 0.54074(15) 0.0286(14) Uani 1 1 d . . . H16 H 0.3621 0.0138 0.5483 0.034 Uiso 1 1 calc R . . C17 C 0.2659(5) 0.0765(5) 0.53216(13) 0.0234(13) Uani 1 1 d . . . H17 H 0.2053 0.0027 0.5343 0.028 Uiso 1 1 calc R . . C18 C 0.1327(5) 0.2258(5) 0.50506(13) 0.0239(13) Uani 1 1 d . . . H18 H 0.0561 0.1703 0.5058 0.029 Uiso 1 1 calc R . . C19 C 0.1475(5) 0.3317(5) 0.49430(14) 0.0239(13) Uani 1 1 d . . . H19 H 0.0791 0.3253 0.4879 0.029 Uiso 1 1 calc R . . C20 C 0.3564(5) 0.6232(5) 0.47988(14) 0.0224(13) Uani 1 1 d . . . H20 H 0.3187 0.6618 0.4742 0.027 Uiso 1 1 calc R . . C21 C 0.4437(5) 0.5679(5) 0.44659(12) 0.0224(13) Uani 1 1 d . . . C22 C 0.2494(5) 0.4496(5) 0.45081(13) 0.0212(12) Uani 1 1 d . . . H22A H 0.2558 0.4279 0.4311 0.025 Uiso 1 1 calc R . . H22B H 0.1902 0.4644 0.4508 0.025 Uiso 1 1 calc R . . C23 C 0.2368(4) 0.2791(5) 0.46312(13) 0.0239(13) Uani 1 1 d . . . C24 C 0.1976(5) 0.1045(5) 0.48352(14) 0.0272(14) Uani 1 1 d . . . H24A H 0.1288 0.0437 0.4894 0.033 Uiso 1 1 calc R . . H24B H 0.2117 0.0914 0.4636 0.033 Uiso 1 1 calc R . . C25 C 0.5364(5) 0.1267(5) 0.51075(15) 0.0274(14) Uani 1 1 d . . . H25A H 0.5466 0.1094 0.4909 0.033 Uiso 1 1 calc R . . H25B H 0.5438 0.0776 0.5239 0.033 Uiso 1 1 calc R . . C26 C 0.8037(5) 0.4965(5) 0.49093(14) 0.0233(12) Uani 1 1 d . . . H26A H 0.8036 0.4723 0.4711 0.028 Uiso 1 1 calc R . . H26B H 0.8769 0.5289 0.4983 0.028 Uiso 1 1 calc R . . C27 C 0.7039(4) 0.5791(4) 0.46950(12) 0.0165(11) Uani 1 1 d . . . C28 C 0.6335(5) 0.6947(5) 0.45572(13) 0.0205(12) Uani 1 1 d . . . H28A H 0.6725 0.7730 0.4565 0.025 Uiso 1 1 calc R . . H28B H 0.6441 0.6738 0.4363 0.025 Uiso 1 1 calc R . . C29 C 0.6569(5) 0.3138(5) 0.49743(12) 0.0196(12) Uani 1 1 d . . . C30 C 0.3758(5) 0.1254(5) 0.49143(14) 0.0220(12) Uani 1 1 d . . . N1 N 0.5054(4) 0.6857(4) 0.51128(11) 0.0221(10) Uani 1 1 d . . . N2 N 0.3294(4) 0.5815(4) 0.50914(11) 0.0196(10) Uani 1 1 d . . . N3 N 0.1916(4) 0.4020(4) 0.52039(11) 0.0221(11) Uani 1 1 d . . . N4 N 0.1804(4) 0.2503(4) 0.53408(11) 0.0232(11) Uani 1 1 d . . . N5 N 0.2571(4) 0.1477(4) 0.55263(11) 0.0260(11) Uani 1 1 d . . . N6 N 0.4166(4) 0.1671(4) 0.56282(12) 0.0289(12) Uani 1 1 d . . . N7 N 0.6071(4) 0.2807(4) 0.56846(11) 0.0261(11) Uani 1 1 d . . . N8 N 0.7306(4) 0.4496(4) 0.56012(11) 0.0234(11) Uani 1 1 d . . . N9 N 0.7451(4) 0.6125(4) 0.54057(11) 0.0207(10) Uani 1 1 d . . . N10 N 0.6797(4) 0.7144(4) 0.52657(11) 0.0188(10) Uani 1 1 d . . . N11 N 0.6799(4) 0.6557(4) 0.47663(11) 0.0213(10) Uani 1 1 d . . . N12 N 0.7720(4) 0.5769(4) 0.49033(11) 0.0206(10) Uani 1 1 d . . . N13 N 0.7352(4) 0.4055(4) 0.50855(11) 0.0232(11) Uani 1 1 d . . . N14 N 0.6181(4) 0.2363(4) 0.51747(12) 0.0260(11) Uani 1 1 d . . . N15 N 0.4312(4) 0.1126(4) 0.51357(11) 0.0237(11) Uani 1 1 d . . . N16 N 0.2803(4) 0.1092(4) 0.50218(11) 0.0228(11) Uani 1 1 d . . . N17 N 0.1892(4) 0.2003(4) 0.48391(12) 0.0277(12) Uani 1 1 d . . . N18 N 0.2228(4) 0.3604(4) 0.47048(12) 0.0255(11) Uani 1 1 d . . . N19 N 0.3473(4) 0.5477(4) 0.45788(14) 0.0244(13) Uani 1 1 d . . . N20 N 0.5222(4) 0.6578(4) 0.45952(11) 0.0201(10) Uani 1 1 d . . . O1 O 0.4163(3) 0.5948(3) 0.55252(9) 0.0237(9) Uani 1 1 d . . . O2 O 0.2423(3) 0.3881(3) 0.56691(9) 0.0243(9) Uani 1 1 d . . . O3 O 0.3531(4) 0.2534(4) 0.59152(10) 0.0344(11) Uani 1 1 d . . . O4 O 0.6085(3) 0.4154(4) 0.59588(11) 0.0335(10) Uani 1 1 d . . . O5 O 0.6376(4) 0.6377(4) 0.57246(10) 0.0277(10) Uani 1 1 d . . . O6 O 0.4562(3) 0.5168(3) 0.42789(10) 0.0279(9) Uani 1 1 d . . . O7 O 0.2819(3) 0.2723(3) 0.44131(10) 0.0278(10) Uani 1 1 d . . . O8 O 0.6717(3) 0.5228(3) 0.44803(10) 0.0256(9) Uani 1 1 d . . . O9 O 0.4050(3) 0.1458(3) 0.46614(9) 0.0239(9) Uani 1 1 d . . . O10 O 0.6267(3) 0.3043(3) 0.47161(9) 0.0250(9) Uani 1 1 d . . . C31 C 1.0458(9) 0.9329(8) 0.6088(2) 0.065(3) Uani 1 1 d . . . H31 H 0.9961 0.9480 0.6176 0.078 Uiso 1 1 calc R . . C32 C 1.1463(8) 0.9782(8) 0.6203(3) 0.065(3) Uani 1 1 d . . . H32 H 1.1655 1.0242 0.6364 0.078 Uiso 1 1 calc R . . C33 C 1.2191(9) 0.9549(10) 0.6076(4) 0.092(5) Uani 1 1 d . . . C34 C 1.1849(13) 0.8824(11) 0.5836(3) 0.095(5) Uani 1 1 d . . . H34 H 1.2320 0.8634 0.5749 0.114 Uiso 1 1 calc R . . C35 C 1.0829(11) 0.8411(7) 0.5734(3) 0.075(4) Uani 1 1 d . . . H35 H 1.0611 0.7935 0.5576 0.090 Uiso 1 1 calc R . . C36 C 1.0133(9) 0.8652(7) 0.5848(2) 0.066(3) Uani 1 1 d . . . O11 O 0.9132(6) 0.8179(6) 0.57228(18) 0.078(2) Uiso 1 1 d . . . H11A H 0.8755 0.8374 0.5810 0.117 Uiso 1 1 calc R . . O12 O 1.3219(9) 0.9960(9) 0.6183(3) 0.123(3) Uiso 1 1 d . . . H12A H 1.3314 1.0374 0.6319 0.185 Uiso 1 1 calc R . . N21 N 0.8605(11) 0.2788(12) 0.4953(3) 0.119(5) Uiso 1 1 d D . . N22 N 0.7911(8) 0.9525(9) 0.6066(2) 0.082(3) Uiso 1 1 d . . . N23 N 0.7822(16) 0.6088(15) 0.3340(5) 0.309(16) Uiso 1 1 d D . . O13 O 0.8634(10) 0.3143(10) 0.4704(3) 0.170(6) Uani 1 1 d D . . O14 O 0.9342(9) 0.3399(11) 0.5125(3) 0.154(5) Uani 1 1 d D . . O15 O 0.7934(13) 0.1894(13) 0.5053(4) 0.201(7) Uiso 1 1 d D . . O16 O 0.7714(8) 0.8822(8) 0.5862(2) 0.105(3) Uiso 1 1 d . . . O17 O 0.7780(8) 1.0266(9) 0.6026(3) 0.119(3) Uiso 1 1 d . . . O18 O 0.8089(11) 0.9246(11) 0.6301(4) 0.156(5) Uiso 1 1 d . . . O19 O 0.8732(16) 0.623(2) 0.3371(9) 0.44(2) Uiso 1 1 d D . . O20 O 0.754(2) 0.6758(16) 0.3309(7) 0.333(15) Uiso 1 1 d D . . O21 O 0.7087(12) 0.5141(13) 0.3334(4) 0.171(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02166(14) 0.02369(14) 0.01310(12) -0.00130(11) 0.00281(11) 0.01098(11) O1W 0.038(3) 0.037(3) 0.029(3) 0.0074(19) 0.012(2) 0.024(2) O2W 0.028(2) 0.030(2) 0.044(3) -0.007(2) -0.002(2) 0.0154(19) O3W 0.031(2) 0.039(2) 0.035(3) -0.002(2) 0.004(2) 0.020(2) O4W 0.029(2) 0.041(3) 0.035(3) -0.013(2) 0.001(2) 0.013(2) C1 0.024(3) 0.022(3) 0.024(4) 0.000(2) 0.012(2) 0.012(3) C2 0.024(3) 0.033(3) 0.018(3) -0.004(2) -0.002(2) 0.019(3) C3 0.019(3) 0.026(3) 0.018(3) -0.004(2) 0.009(2) 0.007(3) C4 0.035(4) 0.024(3) 0.026(4) 0.002(3) 0.001(3) 0.012(3) C5 0.037(4) 0.024(3) 0.012(3) 0.001(2) 0.004(2) 0.014(3) C6 0.039(4) 0.032(3) 0.015(4) 0.001(3) -0.003(3) 0.015(3) C7 0.022(3) 0.036(3) 0.015(3) -0.001(2) -0.008(2) 0.019(3) C8 0.018(3) 0.035(3) 0.014(3) -0.009(2) -0.011(2) 0.013(3) C9 0.016(3) 0.027(3) 0.027(4) -0.007(3) -0.007(2) 0.012(2) C10 0.018(3) 0.016(3) 0.019(3) -0.006(2) -0.003(2) 0.004(2) C11 0.022(3) 0.015(3) 0.019(3) 0.000(2) 0.005(2) 0.011(2) C12 0.018(3) 0.018(3) 0.019(3) -0.002(2) 0.000(2) 0.007(2) C13 0.016(3) 0.026(3) 0.024(3) -0.002(2) 0.005(2) 0.009(2) C14 0.021(3) 0.026(3) 0.021(3) -0.007(2) -0.009(2) 0.013(3) C15 0.031(3) 0.031(3) 0.011(3) 0.006(2) 0.001(2) 0.021(3) C16 0.037(4) 0.024(3) 0.027(4) 0.008(3) 0.008(3) 0.016(3) C17 0.027(3) 0.020(3) 0.018(3) -0.001(2) -0.003(2) 0.007(2) C18 0.019(3) 0.029(3) 0.021(3) -0.004(2) 0.003(2) 0.010(3) C19 0.015(3) 0.027(3) 0.021(3) -0.005(2) -0.004(2) 0.004(2) C20 0.024(3) 0.026(3) 0.025(3) 0.004(2) 0.000(2) 0.019(3) C21 0.032(3) 0.026(3) 0.011(3) 0.006(2) -0.002(2) 0.016(3) C22 0.022(3) 0.030(3) 0.010(3) 0.001(2) 0.001(2) 0.012(3) C23 0.015(3) 0.029(3) 0.019(3) -0.002(2) -0.004(2) 0.005(2) C24 0.030(3) 0.024(3) 0.018(3) -0.004(2) -0.001(3) 0.006(3) C25 0.035(4) 0.020(3) 0.029(4) 0.001(3) 0.002(3) 0.015(3) C26 0.024(3) 0.025(3) 0.023(3) -0.004(2) -0.002(2) 0.013(3) C27 0.014(3) 0.022(3) 0.008(3) 0.003(2) 0.002(2) 0.005(2) C28 0.023(3) 0.023(3) 0.016(3) 0.004(2) 0.001(2) 0.013(2) C29 0.029(3) 0.026(3) 0.009(3) -0.003(2) 0.002(2) 0.017(3) C30 0.027(3) 0.018(3) 0.021(3) -0.004(2) -0.005(2) 0.011(3) N1 0.023(2) 0.026(3) 0.015(3) 0.003(2) 0.006(2) 0.010(2) N2 0.020(2) 0.024(3) 0.017(3) 0.002(2) -0.0011(19) 0.012(2) N3 0.023(3) 0.028(3) 0.014(3) -0.005(2) -0.002(2) 0.011(2) N4 0.024(3) 0.019(2) 0.015(3) -0.004(2) -0.001(2) 0.003(2) N5 0.029(3) 0.029(3) 0.020(3) -0.001(2) -0.001(2) 0.014(2) N6 0.032(3) 0.031(3) 0.020(3) 0.003(2) 0.000(2) 0.013(2) N7 0.033(3) 0.030(3) 0.017(3) -0.003(2) 0.002(2) 0.017(2) N8 0.028(3) 0.032(3) 0.012(3) -0.001(2) 0.000(2) 0.016(2) N9 0.026(3) 0.026(3) 0.015(3) -0.001(2) -0.001(2) 0.016(2) N10 0.019(2) 0.017(2) 0.017(3) -0.0035(19) 0.0015(19) 0.0060(19) N11 0.024(3) 0.022(2) 0.019(3) 0.002(2) 0.004(2) 0.013(2) N12 0.024(2) 0.026(3) 0.013(3) -0.0018(19) -0.0007(19) 0.013(2) N13 0.028(3) 0.031(3) 0.010(3) -0.002(2) -0.0009(19) 0.014(2) N14 0.036(3) 0.018(2) 0.021(3) -0.002(2) 0.002(2) 0.011(2) N15 0.031(3) 0.028(3) 0.016(3) -0.005(2) 0.003(2) 0.018(2) N16 0.027(3) 0.031(3) 0.010(3) -0.002(2) -0.0020(19) 0.015(2) N17 0.026(3) 0.028(3) 0.031(3) -0.001(2) 0.001(2) 0.015(2) N18 0.032(3) 0.029(3) 0.022(3) -0.002(2) 0.004(2) 0.020(2) N19 0.022(3) 0.026(3) 0.023(3) -0.001(2) 0.001(2) 0.010(2) N20 0.026(3) 0.021(2) 0.014(2) 0.0041(19) 0.0015(19) 0.013(2) O1 0.019(2) 0.032(2) 0.017(2) -0.0034(17) 0.0018(16) 0.0103(18) O2 0.029(2) 0.030(2) 0.013(2) -0.0038(17) 0.0005(17) 0.0137(19) O3 0.034(2) 0.035(3) 0.029(3) -0.003(2) 0.000(2) 0.013(2) O4 0.034(2) 0.040(2) 0.027(2) -0.008(2) -0.001(2) 0.019(2) O5 0.032(2) 0.033(2) 0.025(3) 0.0005(19) 0.0069(19) 0.021(2) O6 0.030(2) 0.028(2) 0.028(2) -0.005(2) 0.000(2) 0.0161(18) O7 0.028(2) 0.030(2) 0.026(2) 0.0003(18) 0.0032(18) 0.0153(19) O8 0.022(2) 0.025(2) 0.026(3) -0.0056(18) -0.0006(17) 0.0086(18) O9 0.030(2) 0.030(2) 0.011(2) -0.0029(17) -0.0015(17) 0.0152(19) O10 0.029(2) 0.024(2) 0.020(2) -0.0003(17) -0.0003(17) 0.0116(19) C31 0.078(7) 0.054(6) 0.075(7) 0.023(5) 0.018(5) 0.042(5) C32 0.066(6) 0.055(6) 0.080(8) 0.022(5) 0.008(5) 0.034(5) C33 0.057(6) 0.064(7) 0.143(13) 0.072(8) 0.009(7) 0.021(6) C34 0.128(12) 0.068(8) 0.116(12) 0.071(8) 0.078(10) 0.070(9) C35 0.101(9) 0.033(5) 0.088(8) 0.032(5) 0.054(7) 0.032(6) C36 0.108(8) 0.038(5) 0.064(6) 0.026(4) 0.034(6) 0.046(5) O13 0.136(10) 0.143(10) 0.29(2) -0.037(12) -0.008(11) 0.112(9) O14 0.102(8) 0.163(11) 0.189(14) -0.063(10) -0.008(8) 0.058(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.316(4) . ? Dy1 O10 2.317(4) 5 ? Dy1 O2W 2.335(4) . ? Dy1 O3W 2.337(4) . ? Dy1 O2 2.361(4) . ? Dy1 O1W 2.365(4) . ? Dy1 O9 2.365(4) 5 ? Dy1 O4W 2.371(5) . ? C1 O1 1.240(8) . ? C1 N2 1.353(8) . ? C1 N1 1.367(8) . ? C2 N3 1.422(8) . ? C2 N2 1.458(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 O2 1.241(8) . ? C3 N4 1.349(8) . ? C3 N3 1.353(8) . ? C4 N5 1.443(9) . ? C4 N4 1.453(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 O3 1.223(8) . ? C5 N6 1.360(8) . ? C5 N5 1.378(8) . ? C6 N6 1.433(9) . ? C6 N7 1.452(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O4 1.226(8) . ? C7 N8 1.353(8) . ? C7 N7 1.367(8) . ? C8 N8 1.447(8) . ? C8 N9 1.455(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 O5 1.214(8) . ? C9 N9 1.371(8) . ? C9 N10 1.373(8) . ? C10 N1 1.447(7) . ? C10 N10 1.467(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 N1 1.451(8) . ? C11 N20 1.468(7) . ? C11 C20 1.568(8) . ? C11 H11 0.9900 . ? C12 N10 1.431(7) . ? C12 N11 1.461(8) . ? C12 C13 1.548(8) . ? C12 H12 0.9900 . ? C13 N12 1.449(8) . ? C13 N9 1.461(8) . ? C13 H13 0.9900 . ? C14 N8 1.427(8) . ? C14 N13 1.498(8) . ? C14 C15 1.588(9) . ? C14 H14 0.9900 . ? C15 N14 1.442(8) . ? C15 N7 1.465(8) . ? C15 H15 0.9900 . ? C16 N15 1.450(8) . ? C16 N6 1.467(9) . ? C16 C17 1.554(9) . ? C16 H16 0.9900 . ? C17 N16 1.442(8) . ? C17 N5 1.448(8) . ? C17 H17 0.9900 . ? C18 N17 1.433(8) . ? C18 N4 1.466(8) . ? C18 C19 1.519(9) . ? C18 H18 0.9900 . ? C19 N18 1.453(8) . ? C19 N3 1.495(8) . ? C19 H19 0.9900 . ? C20 N19 1.447(8) . ? C20 N2 1.449(8) . ? C20 H20 0.9900 . ? C21 O6 1.206(7) . ? C21 N20 1.362(8) . ? C21 N19 1.375(8) . ? C22 N19 1.452(8) . ? C22 N18 1.462(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 O7 1.229(8) . ? C23 N18 1.332(8) . ? C23 N17 1.380(8) . ? C24 N16 1.446(8) . ? C24 N17 1.450(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 N15 1.435(8) . ? C25 N14 1.459(8) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 N13 1.438(8) . ? C26 N12 1.445(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 O8 1.216(7) . ? C27 N11 1.356(7) . ? C27 N12 1.387(7) . ? C28 N20 1.430(7) . ? C28 N11 1.439(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 O10 1.252(7) . ? C29 N14 1.339(8) . ? C29 N13 1.341(8) . ? C30 O9 1.225(8) . ? C30 N15 1.366(8) . ? C30 N16 1.371(8) . ? O9 Dy1 2.365(4) 6_554 ? O10 Dy1 2.317(4) 6_554 ? C31 C32 1.365(15) . ? C31 C36 1.396(15) . ? C31 H31 0.9400 . ? C32 C33 1.385(18) . ? C32 H32 0.9400 . ? C33 O12 1.385(16) . ? C33 C34 1.43(2) . ? C34 C35 1.368(19) . ? C34 H34 0.9400 . ? C35 C36 1.327(14) . ? C35 H35 0.9400 . ? C36 O11 1.379(14) . ? O11 H11A 0.8300 . ? O12 H12A 0.8300 . ? N21 O13 1.251(2) . ? N21 O15 1.253(2) . ? N21 O14 1.265(18) . ? N22 O17 1.191(12) . ? N22 O18 1.228(16) . ? N22 O16 1.308(13) . ? N23 O20 1.231(9) . ? N23 O19 1.233(9) . ? N23 O21 1.244(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O10 134.95(14) . 5 ? O1 Dy1 O2W 115.30(17) . . ? O10 Dy1 O2W 79.60(16) 5 . ? O1 Dy1 O3W 79.61(17) . . ? O10 Dy1 O3W 116.56(16) 5 . ? O2W Dy1 O3W 140.80(15) . . ? O1 Dy1 O2 75.35(15) . . ? O10 Dy1 O2 146.51(15) 5 . ? O2W Dy1 O2 72.56(16) . . ? O3W Dy1 O2 77.35(16) . . ? O1 Dy1 O1W 71.84(15) . . ? O10 Dy1 O1W 74.61(16) 5 . ? O2W Dy1 O1W 70.57(16) . . ? O3W Dy1 O1W 145.92(16) . . ? O2 Dy1 O1W 111.84(17) . . ? O1 Dy1 O9 147.00(15) . 5 ? O10 Dy1 O9 75.58(14) 5 5 ? O2W Dy1 O9 77.12(16) . 5 ? O3W Dy1 O9 73.52(16) . 5 ? O2 Dy1 O9 80.32(14) . 5 ? O1W Dy1 O9 139.17(15) . 5 ? O1 Dy1 O4W 74.33(16) . . ? O10 Dy1 O4W 72.36(16) 5 . ? O2W Dy1 O4W 145.48(16) . . ? O3W Dy1 O4W 71.77(17) . . ? O2 Dy1 O4W 139.81(15) . . ? O1W Dy1 O4W 82.71(18) . . ? O9 Dy1 O4W 113.69(16) 5 . ? O1 C1 N2 126.7(5) . . ? O1 C1 N1 124.2(6) . . ? N2 C1 N1 109.2(6) . . ? N3 C2 N2 113.5(5) . . ? N3 C2 H2A 108.9 . . ? N2 C2 H2A 108.9 . . ? N3 C2 H2B 108.9 . . ? N2 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O2 C3 N4 124.8(6) . . ? O2 C3 N3 125.6(6) . . ? N4 C3 N3 109.5(5) . . ? N5 C4 N4 112.6(5) . . ? N5 C4 H4A 109.1 . . ? N4 C4 H4A 109.1 . . ? N5 C4 H4B 109.1 . . ? N4 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? O3 C5 N6 125.7(6) . . ? O3 C5 N5 125.4(6) . . ? N6 C5 N5 108.8(5) . . ? N6 C6 N7 113.5(5) . . ? N6 C6 H6A 108.9 . . ? N7 C6 H6A 108.9 . . ? N6 C6 H6B 108.9 . . ? N7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O4 C7 N8 124.3(6) . . ? O4 C7 N7 126.0(6) . . ? N8 C7 N7 109.4(5) . . ? N8 C8 N9 113.8(5) . . ? N8 C8 H8A 108.8 . . ? N9 C8 H8A 108.8 . . ? N8 C8 H8B 108.8 . . ? N9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O5 C9 N9 125.2(6) . . ? O5 C9 N10 127.8(5) . . ? N9 C9 N10 107.0(5) . . ? N1 C10 N10 113.9(5) . . ? N1 C10 H10A 108.8 . . ? N10 C10 H10A 108.8 . . ? N1 C10 H10B 108.8 . . ? N10 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N1 C11 N20 114.3(4) . . ? N1 C11 C20 103.2(4) . . ? N20 C11 C20 103.4(4) . . ? N1 C11 H11 111.8 . . ? N20 C11 H11 111.8 . . ? C20 C11 H11 111.8 . . ? N10 C12 N11 116.1(5) . . ? N10 C12 C13 101.9(5) . . ? N11 C12 C13 103.2(5) . . ? N10 C12 H12 111.6 . . ? N11 C12 H12 111.6 . . ? C13 C12 H12 111.6 . . ? N12 C13 N9 114.4(5) . . ? N12 C13 C12 103.7(5) . . ? N9 C13 C12 103.9(4) . . ? N12 C13 H13 111.4 . . ? N9 C13 H13 111.4 . . ? C12 C13 H13 111.4 . . ? N8 C14 N13 115.3(5) . . ? N8 C14 C15 103.8(5) . . ? N13 C14 C15 100.9(4) . . ? N8 C14 H14 112.0 . . ? N13 C14 H14 112.0 . . ? C15 C14 H14 112.0 . . ? N14 C15 N7 115.8(5) . . ? N14 C15 C14 103.4(4) . . ? N7 C15 C14 101.5(5) . . ? N14 C15 H15 111.8 . . ? N7 C15 H15 111.8 . . ? C14 C15 H15 111.8 . . ? N15 C16 N6 114.1(5) . . ? N15 C16 C17 102.2(5) . . ? N6 C16 C17 103.1(5) . . ? N15 C16 H16 112.3 . . ? N6 C16 H16 112.3 . . ? C17 C16 H16 112.3 . . ? N16 C17 N5 116.2(5) . . ? N16 C17 C16 104.4(5) . . ? N5 C17 C16 103.4(5) . . ? N16 C17 H17 110.8 . . ? N5 C17 H17 110.8 . . ? C16 C17 H17 110.8 . . ? N17 C18 N4 115.0(5) . . ? N17 C18 C19 103.0(5) . . ? N4 C18 C19 104.1(5) . . ? N17 C18 H18 111.4 . . ? N4 C18 H18 111.4 . . ? C19 C18 H18 111.4 . . ? N18 C19 N3 114.2(5) . . ? N18 C19 C18 104.0(5) . . ? N3 C19 C18 102.6(5) . . ? N18 C19 H19 111.8 . . ? N3 C19 H19 111.8 . . ? C18 C19 H19 111.8 . . ? N19 C20 N2 115.8(5) . . ? N19 C20 C11 102.2(4) . . ? N2 C20 C11 102.6(4) . . ? N19 C20 H20 111.8 . . ? N2 C20 H20 111.8 . . ? C11 C20 H20 111.8 . . ? O6 C21 N20 126.1(6) . . ? O6 C21 N19 125.9(6) . . ? N20 C21 N19 108.0(5) . . ? N19 C22 N18 114.8(5) . . ? N19 C22 H22A 108.6 . . ? N18 C22 H22A 108.6 . . ? N19 C22 H22B 108.6 . . ? N18 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? O7 C23 N18 126.9(6) . . ? O7 C23 N17 124.6(6) . . ? N18 C23 N17 108.5(5) . . ? N16 C24 N17 114.2(5) . . ? N16 C24 H24A 108.7 . . ? N17 C24 H24A 108.7 . . ? N16 C24 H24B 108.7 . . ? N17 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? N15 C25 N14 111.1(5) . . ? N15 C25 H25A 109.4 . . ? N14 C25 H25A 109.4 . . ? N15 C25 H25B 109.4 . . ? N14 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? N13 C26 N12 113.3(5) . . ? N13 C26 H26A 108.9 . . ? N12 C26 H26A 108.9 . . ? N13 C26 H26B 108.9 . . ? N12 C26 H26B 108.9 . . ? H26A C26 H26B 107.7 . . ? O8 C27 N11 125.1(5) . . ? O8 C27 N12 125.9(5) . . ? N11 C27 N12 109.0(5) . . ? N20 C28 N11 115.4(5) . . ? N20 C28 H28A 108.4 . . ? N11 C28 H28A 108.4 . . ? N20 C28 H28B 108.4 . . ? N11 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? O10 C29 N14 126.0(6) . . ? O10 C29 N13 123.2(5) . . ? N14 C29 N13 110.9(5) . . ? O9 C30 N15 126.1(6) . . ? O9 C30 N16 125.5(5) . . ? N15 C30 N16 108.4(5) . . ? C1 N1 C10 121.0(5) . . ? C1 N1 C11 112.0(5) . . ? C10 N1 C11 124.8(5) . . ? C1 N2 C20 112.9(5) . . ? C1 N2 C2 121.8(5) . . ? C20 N2 C2 125.2(5) . . ? C3 N3 C2 126.0(5) . . ? C3 N3 C19 111.4(5) . . ? C2 N3 C19 122.3(5) . . ? C3 N4 C4 122.7(5) . . ? C3 N4 C18 111.9(5) . . ? C4 N4 C18 123.0(5) . . ? C5 N5 C4 122.2(5) . . ? C5 N5 C17 112.2(5) . . ? C4 N5 C17 125.6(5) . . ? C5 N6 C6 122.3(6) . . ? C5 N6 C16 111.7(5) . . ? C6 N6 C16 123.5(5) . . ? C7 N7 C6 122.8(5) . . ? C7 N7 C15 112.2(5) . . ? C6 N7 C15 124.5(5) . . ? C7 N8 C14 113.0(5) . . ? C7 N8 C8 123.9(5) . . ? C14 N8 C8 122.8(5) . . ? C9 N9 C8 121.5(5) . . ? C9 N9 C13 111.7(5) . . ? C8 N9 C13 123.4(5) . . ? C9 N10 C12 114.7(5) . . ? C9 N10 C10 122.0(5) . . ? C12 N10 C10 122.2(5) . . ? C27 N11 C28 121.1(5) . . ? C27 N11 C12 111.9(5) . . ? C28 N11 C12 123.0(5) . . ? C27 N12 C26 123.0(5) . . ? C27 N12 C13 111.5(5) . . ? C26 N12 C13 125.1(5) . . ? C29 N13 C26 122.8(5) . . ? C29 N13 C14 111.8(5) . . ? C26 N13 C14 124.0(5) . . ? C29 N14 C15 113.0(5) . . ? C29 N14 C25 122.3(5) . . ? C15 N14 C25 124.6(5) . . ? C30 N15 C25 124.3(5) . . ? C30 N15 C16 113.2(5) . . ? C25 N15 C16 122.5(5) . . ? C30 N16 C17 111.7(5) . . ? C30 N16 C24 122.0(5) . . ? C17 N16 C24 125.1(5) . . ? C23 N17 C18 111.9(5) . . ? C23 N17 C24 122.3(5) . . ? C18 N17 C24 125.8(5) . . ? C23 N18 C19 111.3(5) . . ? C23 N18 C22 122.0(5) . . ? C19 N18 C22 123.4(5) . . ? C21 N19 C20 113.9(5) . . ? C21 N19 C22 120.7(5) . . ? C20 N19 C22 124.8(5) . . ? C21 N20 C28 123.2(5) . . ? C21 N20 C11 112.4(5) . . ? C28 N20 C11 123.4(5) . . ? C1 O1 Dy1 150.5(4) . . ? C3 O2 Dy1 148.5(4) . . ? C30 O9 Dy1 151.2(4) . 6_554 ? C29 O10 Dy1 154.4(4) . 6_554 ? C32 C31 C36 123.2(10) . . ? C32 C31 H31 118.4 . . ? C36 C31 H31 118.4 . . ? C31 C32 C33 118.4(12) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C32 C33 O12 121.9(16) . . ? C32 C33 C34 118.5(12) . . ? O12 C33 C34 119.5(15) . . ? C35 C34 C33 119.2(11) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 C34 122.8(13) . . ? C36 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C35 C36 O11 116.6(11) . . ? C35 C36 C31 117.8(12) . . ? O11 C36 C31 125.6(9) . . ? C36 O11 H11A 109.5 . . ? C33 O12 H12A 109.5 . . ? O13 N21 O15 128(2) . . ? O13 N21 O14 116.4(17) . . ? O15 N21 O14 115.9(18) . . ? O17 N22 O18 125.9(13) . . ? O17 N22 O16 121.0(12) . . ? O18 N22 O16 112.4(12) . . ? O20 N23 O19 128.7(17) . . ? O20 N23 O21 115.3(15) . . ? O19 N23 O21 116.0(16) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.089 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.108 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.064 0.530 0.181 45 7 ' ' 2 0.121 0.090 0.199 56 25 ' ' 3 -0.030 0.319 0.309 29 10 ' ' 4 0.032 0.120 0.366 56 25 ' ' 5 -0.080 0.411 0.385 73 29 ' ' 6 0.064 0.469 0.681 45 7 ' ' 7 -0.121 0.910 0.699 57 25 ' ' 8 0.030 0.680 0.809 29 10 ' ' 9 -0.032 0.880 0.866 57 25 ' ' 10 0.080 0.588 0.885 73 29 ' ' 11 0.090 -0.031 0.033 56 25 ' ' 12 0.056 0.590 0.546 22 9 ' ' 13 0.053 0.520 0.467 13 8 ' ' 14 0.321 0.351 0.142 29 10 ' ' 15 0.351 0.030 0.976 28 10 ' ' 16 0.411 0.492 0.218 73 29 ' ' 17 0.492 0.080 0.051 74 29 ' ' 18 0.405 0.936 0.347 45 7 ' ' 19 0.410 0.467 0.879 22 9 ' ' 20 0.513 0.921 0.549 77 30 ' ' 21 0.469 0.406 0.514 46 7 ' ' 22 0.467 0.057 0.713 22 9 ' ' 23 0.530 0.594 0.014 46 7 ' ' 24 0.467 0.947 0.134 13 8 ' ' 25 0.482 0.533 0.799 13 9 ' ' 26 0.533 0.943 0.213 22 9 ' ' 27 0.520 0.467 0.300 13 8 ' ' 28 0.590 0.510 0.715 75 29 ' ' 29 0.533 0.053 0.634 13 8 ' ' 30 0.594 0.064 0.847 45 7 ' ' 31 0.590 0.533 0.379 22 9 ' ' 32 0.663 0.973 0.473 26 9 ' ' 33 0.687 0.661 0.639 26 9 ' ' 34 0.914 1.032 0.533 55 25 ' ' 35 0.943 0.410 0.046 22 9 ' ' 36 0.947 0.480 0.967 13 8 ' ' _platon_squeeze_details ; ; data_06 _database_code_depnum_ccdc_archive 'CCDC 875770' #TrackingRef 'submit-07.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 Cl3 N20 O28 Yb' _chemical_formula_weight 1508.49 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' Yb Yb -0.3850 5.5486 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 61' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, x, z+1/6' 'y, -x+y, z+5/6' _cell_length_a 14.499(4) _cell_length_b 14.499 _cell_length_c 45.818(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8341(3) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4614 _exptl_absorpt_coefficient_mu 1.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6039 _exptl_absorpt_correction_T_max 0.6868 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55123 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.10 _reflns_number_total 9508 _reflns_number_gt 9187 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+14.7435P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.060(8) _refine_ls_number_reflns 9508 _refine_ls_number_parameters 701 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.4016(6) -0.4309(5) 0.47784(18) 0.110(2) Uani 0.50 1 d P . . Cl2 Cl 0.3833(11) -0.1244(7) 0.7586(2) 0.163(4) Uani 0.50 1 d P . . Cl3 Cl 0.0165(5) -0.5928(6) 0.6702(2) 0.141(3) Uani 0.50 1 d P . . Cl4 Cl 0.9487(7) -0.0025(13) 0.6197(2) 0.183(5) Uani 0.50 1 d P . . Cl5 Cl 0.4867(10) -0.5436(7) 0.5652(2) 0.162(4) Uani 0.50 1 d P . . Cl6 Cl 0.3045(12) -0.5463(10) 0.5700(6) 0.338(15) Uani 0.50 1 d P . . C31 C 0.7151(11) -0.2100(10) 0.5333(3) 0.130(7) Uani 1 1 d D . . C32 C 0.6919(12) -0.1647(12) 0.5100(3) 0.105(5) Uani 1 1 d D . . H32 H 0.6262 -0.2056 0.5005 0.125 Uiso 1 1 calc R . . C33 C 0.7591(10) -0.0631(10) 0.4997(3) 0.136(7) Uani 1 1 d D . . H33 H 0.7434 -0.0342 0.4834 0.163 Uiso 1 1 calc R . . C34 C 0.8516(11) -0.0079(11) 0.5157(3) 0.118(6) Uani 1 1 d D . . C35 C 0.8792(12) -0.0449(12) 0.5401(3) 0.148(7) Uani 1 1 d D . . H35 H 0.9433 -0.0026 0.5501 0.178 Uiso 1 1 calc R . . C36 C 0.8073(11) -0.1473(11) 0.5488(3) 0.115(6) Uani 1 1 d D . . H36 H 0.8215 -0.1750 0.5657 0.138 Uiso 1 1 calc R . . O11 O 0.6554(11) -0.3085(8) 0.5452(4) 0.286(13) Uani 1 1 d . . . H11 H 0.6002 -0.3431 0.5355 0.430 Uiso 1 1 calc R . . O12 O 0.9165(11) 0.0957(9) 0.5034(3) 0.136(4) Uani 1 1 d . . . H12 H 0.9722 0.1286 0.5130 0.204 Uiso 1 1 calc R . . O1W O 0.0278(3) -0.4323(3) 0.53149(11) 0.0336(9) Uani 1 1 d . . . O2W O 0.3363(3) -0.1473(3) 0.53096(11) 0.0342(9) Uani 1 1 d . . . O3W O 0.1721(4) -0.4951(3) 0.54163(10) 0.0374(10) Uani 1 1 d . . . O4W O 0.3701(3) -0.3059(3) 0.51391(10) 0.0340(10) Uani 1 1 d . . . Yb1 Yb 0.209960(17) -0.323664(17) 0.530223(19) 0.02231(7) Uani 1 1 d . . . C1 C 0.3093(4) -0.3363(4) 0.59675(11) 0.0211(11) Uani 1 1 d . . . C2 C 0.3820(5) -0.3622(4) 0.63949(14) 0.0282(13) Uani 1 1 d . . . H2 H 0.3942 -0.4231 0.6421 0.034 Uiso 1 1 calc R . . C3 C 0.2659(5) -0.3943(5) 0.64481(13) 0.0273(13) Uani 1 1 d . . . H3 H 0.2238 -0.4696 0.6510 0.033 Uiso 1 1 calc R . . C4 C 0.3766(5) -0.2554(4) 0.67653(12) 0.0265(12) Uani 1 1 d . . . C5 C 0.1227(4) -0.4017(5) 0.60968(15) 0.0287(13) Uani 1 1 d . . . H5A H 0.1079 -0.4270 0.5894 0.034 Uiso 1 1 calc R . . H5B H 0.0713 -0.4593 0.6222 0.034 Uiso 1 1 calc R . . C6 C 0.1839(5) -0.3129(5) 0.67871(14) 0.0305(13) Uani 1 1 d . . . H6A H 0.1209 -0.3843 0.6791 0.037 Uiso 1 1 calc R . . H6B H 0.1988 -0.2868 0.6989 0.037 Uiso 1 1 calc R . . C7 C 0.1240(4) -0.2439(5) 0.59064(12) 0.0258(8) Uani 1 1 d . . . C8 C 0.0775(4) -0.2827(5) 0.63931(13) 0.0285(13) Uani 1 1 d . . . H8 H 0.0076 -0.3400 0.6464 0.034 Uiso 1 1 calc R . . C9 C 0.0736(4) -0.1819(5) 0.63070(12) 0.0258(12) Uani 1 1 d . . . H9 H 0.0002 -0.1939 0.6321 0.031 Uiso 1 1 calc R . . C10 C 0.1902(4) -0.1422(5) 0.67021(12) 0.0258(8) Uani 1 1 d . . . C11 C 0.1073(5) -0.0850(6) 0.58137(15) 0.0350(15) Uani 1 1 d . . . H11A H 0.0967 -0.1116 0.5613 0.042 Uiso 1 1 calc R . . H11B H 0.0460 -0.0772 0.5867 0.042 Uiso 1 1 calc R . . C12 C 0.1676(5) 0.0061(5) 0.65342(14) 0.0302(13) Uani 1 1 d . . . H12A H 0.1024 0.0083 0.6493 0.036 Uiso 1 1 calc R . . H12B H 0.1901 0.0326 0.6733 0.036 Uiso 1 1 calc R . . C13 C 0.2818(5) 0.0492(5) 0.56204(13) 0.0272(13) Uani 1 1 d . . . C14 C 0.2252(5) 0.0988(5) 0.60436(14) 0.0313(14) Uani 1 1 d . . . H14 H 0.1701 0.1200 0.6046 0.038 Uiso 1 1 calc R . . C15 C 0.3361(4) 0.1917(5) 0.59382(12) 0.0241(12) Uani 1 1 d . . . H15 H 0.3316 0.2549 0.5878 0.029 Uiso 1 1 calc R . . C16 C 0.3519(5) 0.1481(5) 0.64242(13) 0.0266(13) Uani 1 1 d . . . C17 C 0.4541(5) 0.2088(4) 0.55063(12) 0.0239(11) Uani 1 1 d . . . H17A H 0.4338 0.1821 0.5307 0.029 Uiso 1 1 calc R . . H17B H 0.4714 0.2834 0.5508 0.029 Uiso 1 1 calc R . . C18 C 0.5122(4) 0.2935(4) 0.62017(12) 0.0210(11) Uani 1 1 d . . . H18A H 0.5329 0.3210 0.6401 0.025 Uiso 1 1 calc R . . H18B H 0.5215 0.3525 0.6078 0.025 Uiso 1 1 calc R . . C19 C 0.5692(4) 0.1279(4) 0.54758(12) 0.0220(11) Uani 1 1 d . . . C20 C 0.6245(5) 0.2691(4) 0.58102(13) 0.0239(12) Uani 1 1 d . . . H20 H 0.6635 0.3450 0.5752 0.029 Uiso 1 1 calc R . . C21 C 0.7003(4) 0.2233(4) 0.58311(12) 0.0216(11) Uani 1 1 d . . . H21 H 0.7753 0.2782 0.5794 0.026 Uiso 1 1 calc R . . C22 C 0.6158(4) 0.2047(4) 0.62730(13) 0.0232(12) Uani 1 1 d . . . C23 C 0.6946(5) 0.0637(5) 0.55665(13) 0.0266(12) Uani 1 1 d . . . H23A H 0.6740 0.0327 0.5371 0.032 Uiso 1 1 calc R . . H23B H 0.7725 0.1020 0.5576 0.032 Uiso 1 1 calc R . . C24 C 0.7509(4) 0.1500(4) 0.62713(13) 0.0248(12) Uani 1 1 d . . . H24A H 0.7640 0.1777 0.6471 0.030 Uiso 1 1 calc R . . H24B H 0.8197 0.1828 0.6170 0.030 Uiso 1 1 calc R . . C25 C 0.5755(4) -0.1225(4) 0.56999(12) 0.0202(11) Uani 1 1 d . . . C26 C 0.7122(4) -0.0232(4) 0.60328(12) 0.0216(11) Uani 1 1 d . . . H26 H 0.7863 -0.0029 0.5982 0.026 Uiso 1 1 calc R . . C27 C 0.6490(4) -0.1389(5) 0.61408(13) 0.0242(12) Uani 1 1 d . . . H27 H 0.6951 -0.1707 0.6165 0.029 Uiso 1 1 calc R . . C28 C 0.6463(4) -0.0282(4) 0.65045(13) 0.0230(12) Uani 1 1 d . . . C29 C 0.4915(5) -0.3023(4) 0.59185(12) 0.0234(8) Uani 1 1 d . . . H29A H 0.5236 -0.3424 0.5998 0.028 Uiso 1 1 calc R . . H29B H 0.4683 -0.3274 0.5719 0.028 Uiso 1 1 calc R . . C30 C 0.5557(5) -0.2176(4) 0.66247(12) 0.0234(8) Uani 1 1 d . . . H30A H 0.5842 -0.2654 0.6592 0.028 Uiso 1 1 calc R . . H30B H 0.5759 -0.1886 0.6822 0.028 Uiso 1 1 calc R . . N1 N 0.4000(3) -0.3239(3) 0.60911(10) 0.0209(9) Uani 1 1 d . . . N2 N 0.2295(4) -0.3780(4) 0.61738(11) 0.0258(10) Uani 1 1 d . . . N3 N 0.4405(4) -0.2791(4) 0.66074(10) 0.0225(10) Uani 1 1 d . . . N4 N 0.2725(4) -0.3217(4) 0.66823(11) 0.0301(11) Uani 1 1 d . . . N5 N 0.1081(4) -0.3117(4) 0.61261(11) 0.0250(10) Uani 1 1 d . . . N6 N 0.1113(4) -0.1628(4) 0.60079(10) 0.0262(11) Uani 1 1 d . . . N7 N 0.1592(4) -0.2451(4) 0.66221(11) 0.0310(11) Uani 1 1 d . . . N8 N 0.1436(4) -0.1037(4) 0.65204(12) 0.0306(11) Uani 1 1 d . . . N9 N 0.2037(4) 0.0187(4) 0.58272(12) 0.0323(12) Uani 1 1 d . . . N10 N 0.3643(4) 0.1476(4) 0.56983(11) 0.0271(11) Uani 1 1 d . . . N11 N 0.2484(4) 0.0752(4) 0.63362(11) 0.0263(10) Uani 1 1 d . . . N12 N 0.4032(4) 0.2137(4) 0.62017(9) 0.0228(10) Uani 1 1 d . . . N13 N 0.5477(4) 0.2037(4) 0.55881(14) 0.0306(12) Uani 1 1 d . . . N14 N 0.6582(4) 0.1400(3) 0.56053(10) 0.0208(9) Uani 1 1 d . . . N15 N 0.5827(4) 0.2566(4) 0.60999(11) 0.0254(10) Uani 1 1 d . . . N16 N 0.6843(3) 0.1817(3) 0.61293(10) 0.0208(9) Uani 1 1 d . . . N17 N 0.6535(3) -0.0218(3) 0.57777(11) 0.0224(10) Uani 1 1 d . . . N18 N 0.5705(4) -0.1913(4) 0.59104(10) 0.0223(10) Uani 1 1 d . . . N19 N 0.7085(3) 0.0361(4) 0.62826(10) 0.0220(9) Uani 1 1 d . . . N20 N 0.6048(4) -0.1302(4) 0.64166(11) 0.0242(10) Uani 1 1 d . . . O1 O 0.3008(3) -0.3140(3) 0.57162(9) 0.0281(9) Uani 1 1 d . . . O2 O 0.1461(3) -0.2513(3) 0.56482(9) 0.0293(9) Uani 1 1 d . . . O3 O 0.2769(3) -0.0008(3) 0.54021(9) 0.0299(9) Uani 1 1 d . . . O4 O 0.5179(3) 0.0645(3) 0.52870(10) 0.0297(8) Uani 1 1 d . . . O5 O 0.5210(3) -0.1441(3) 0.54830(9) 0.0262(8) Uani 1 1 d . . . O6 O 0.4049(3) -0.1904(3) 0.69672(10) 0.0308(8) Uani 1 1 d . . . O7 O 0.2471(3) -0.0963(3) 0.69110(9) 0.0334(10) Uani 1 1 d . . . O8 O 0.3860(3) 0.1486(3) 0.66688(9) 0.0278(9) Uani 1 1 d . . . O9 O 0.5903(3) 0.1795(3) 0.65352(9) 0.0256(8) Uani 1 1 d . . . O10 O 0.6294(3) 0.0002(3) 0.67418(9) 0.0303(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.121(5) 0.099(4) 0.123(6) -0.038(4) -0.027(4) 0.066(4) Cl2 0.268(13) 0.109(6) 0.113(7) 0.011(5) 0.041(7) 0.095(7) Cl3 0.059(3) 0.115(5) 0.189(9) 0.045(6) 0.000(4) -0.001(3) Cl4 0.126(7) 0.375(17) 0.108(7) -0.030(8) -0.030(5) 0.170(10) Cl5 0.261(12) 0.099(5) 0.148(9) 0.021(5) 0.044(8) 0.106(7) Cl6 0.242(14) 0.139(9) 0.68(4) -0.146(16) -0.29(2) 0.131(10) C31 0.133(12) 0.080(8) 0.160(16) -0.039(10) 0.087(12) 0.042(9) C32 0.129(11) 0.133(13) 0.081(9) 0.021(8) 0.050(8) 0.088(11) C33 0.077(8) 0.101(10) 0.23(2) -0.067(12) 0.027(11) 0.044(8) C34 0.108(11) 0.087(9) 0.168(17) -0.029(10) 0.029(10) 0.056(9) C35 0.178(18) 0.23(2) 0.123(16) -0.004(13) 0.036(12) 0.162(19) C36 0.124(12) 0.071(8) 0.154(14) 0.006(9) 0.065(11) 0.053(8) O11 0.216(13) 0.081(7) 0.46(3) -0.089(11) 0.248(17) -0.001(7) O12 0.192(11) 0.109(7) 0.137(10) -0.002(6) 0.002(8) 0.097(8) O1W 0.028(2) 0.029(2) 0.041(3) -0.001(2) -0.003(2) 0.0125(16) O2W 0.032(2) 0.028(2) 0.038(2) 0.002(2) -0.002(2) 0.0114(17) O3W 0.040(2) 0.028(2) 0.038(3) -0.0005(18) -0.0078(19) 0.0131(19) O4W 0.036(2) 0.036(2) 0.029(2) -0.0126(18) -0.0099(18) 0.0165(19) Yb1 0.02683(12) 0.02350(12) 0.01376(10) -0.00323(9) -0.00497(10) 0.01046(10) C1 0.034(3) 0.017(3) 0.010(3) -0.005(2) 0.001(2) 0.011(2) C2 0.037(3) 0.017(3) 0.028(3) -0.003(2) -0.004(2) 0.011(2) C3 0.036(3) 0.025(3) 0.021(3) 0.003(2) -0.004(2) 0.016(3) C4 0.037(3) 0.022(3) 0.017(3) 0.003(2) -0.002(2) 0.012(3) C5 0.016(3) 0.026(3) 0.036(4) 0.002(2) -0.001(2) 0.005(2) C6 0.027(3) 0.039(3) 0.016(3) 0.003(2) 0.001(2) 0.009(3) C7 0.0227(19) 0.039(2) 0.0101(19) -0.0018(16) 0.0003(15) 0.0114(18) C8 0.021(3) 0.037(3) 0.022(3) -0.003(2) 0.003(2) 0.011(2) C9 0.018(3) 0.040(3) 0.018(3) -0.007(2) 0.000(2) 0.013(2) C10 0.0227(19) 0.039(2) 0.0101(19) -0.0018(16) 0.0003(15) 0.0114(18) C11 0.023(3) 0.057(4) 0.029(3) -0.008(3) -0.012(2) 0.024(3) C12 0.033(3) 0.043(3) 0.027(3) -0.003(3) 0.002(2) 0.028(3) C13 0.037(3) 0.034(3) 0.024(3) -0.002(2) -0.008(2) 0.027(3) C14 0.032(3) 0.038(3) 0.036(4) -0.007(3) -0.010(3) 0.027(3) C15 0.030(3) 0.031(3) 0.018(3) -0.005(2) -0.005(2) 0.020(3) C16 0.041(3) 0.035(3) 0.016(3) -0.009(2) 0.001(2) 0.027(3) C17 0.036(3) 0.030(3) 0.011(3) 0.000(2) 0.000(2) 0.020(3) C18 0.035(3) 0.019(3) 0.013(3) -0.004(2) -0.004(2) 0.017(2) C19 0.030(3) 0.022(3) 0.014(3) 0.005(2) 0.010(2) 0.013(2) C20 0.028(3) 0.014(2) 0.022(3) -0.003(2) -0.002(2) 0.005(2) C21 0.028(3) 0.016(3) 0.014(3) 0.001(2) 0.002(2) 0.006(2) C22 0.022(3) 0.022(3) 0.019(3) -0.010(2) -0.002(2) 0.007(2) C23 0.025(3) 0.028(3) 0.027(3) 0.004(2) 0.005(2) 0.014(2) C24 0.020(3) 0.028(3) 0.025(3) -0.008(2) -0.002(2) 0.011(2) C25 0.025(3) 0.028(3) 0.016(3) -0.003(2) 0.002(2) 0.020(2) C26 0.017(2) 0.027(3) 0.021(3) -0.006(2) -0.004(2) 0.011(2) C27 0.023(3) 0.036(3) 0.021(3) -0.003(2) -0.002(2) 0.020(3) C28 0.026(3) 0.026(3) 0.025(3) 0.001(2) -0.003(2) 0.019(2) C29 0.042(2) 0.025(2) 0.0123(19) 0.0009(15) -0.0019(16) 0.0225(18) C30 0.042(2) 0.025(2) 0.0123(19) 0.0009(15) -0.0019(16) 0.0225(18) N1 0.025(2) 0.022(2) 0.013(2) 0.0005(17) -0.0043(18) 0.0098(19) N2 0.025(2) 0.025(2) 0.019(3) -0.0013(19) -0.0048(19) 0.007(2) N3 0.027(2) 0.023(2) 0.016(2) 0.0011(18) -0.0025(18) 0.012(2) N4 0.031(3) 0.034(3) 0.020(3) -0.002(2) -0.002(2) 0.013(2) N5 0.023(2) 0.028(2) 0.020(3) -0.0037(19) -0.0010(19) 0.0095(19) N6 0.030(3) 0.037(3) 0.011(3) -0.0007(19) 0.0001(18) 0.017(2) N7 0.025(3) 0.038(3) 0.023(3) 0.004(2) 0.004(2) 0.011(2) N8 0.025(2) 0.033(3) 0.035(3) -0.006(2) 0.002(2) 0.015(2) N9 0.032(3) 0.032(3) 0.040(3) -0.002(2) -0.006(2) 0.022(2) N10 0.038(3) 0.028(2) 0.022(3) -0.004(2) 0.000(2) 0.022(2) N11 0.026(2) 0.040(3) 0.018(3) 0.000(2) 0.0007(19) 0.020(2) N12 0.035(3) 0.029(2) 0.006(2) -0.0040(17) -0.0052(18) 0.017(2) N13 0.036(3) 0.030(3) 0.031(3) -0.003(2) -0.002(2) 0.021(2) N14 0.029(2) 0.022(2) 0.013(2) -0.0038(17) 0.0014(18) 0.014(2) N15 0.037(3) 0.027(2) 0.021(3) 0.0076(19) 0.006(2) 0.023(2) N16 0.027(2) 0.024(2) 0.012(2) -0.0043(17) 0.0024(18) 0.0142(19) N17 0.020(2) 0.018(2) 0.028(3) -0.0009(18) -0.0008(19) 0.0093(19) N18 0.023(2) 0.024(2) 0.014(2) -0.0006(18) -0.0054(18) 0.0075(19) N19 0.023(2) 0.024(2) 0.014(2) -0.0045(18) 0.0011(18) 0.0073(19) N20 0.031(2) 0.025(2) 0.023(3) -0.0020(19) -0.0037(19) 0.018(2) O1 0.024(2) 0.035(2) 0.019(2) -0.0015(16) -0.0022(15) 0.0093(17) O2 0.034(2) 0.031(2) 0.024(2) -0.0039(17) -0.0058(17) 0.0179(19) O3 0.040(2) 0.032(2) 0.021(2) -0.0011(16) 0.0001(17) 0.0209(19) O4 0.035(2) 0.0291(19) 0.023(2) -0.0078(19) -0.0027(19) 0.0149(17) O5 0.029(2) 0.024(2) 0.023(2) -0.0036(16) -0.0042(17) 0.0124(17) O6 0.040(2) 0.037(2) 0.018(2) 0.0007(19) -0.0003(19) 0.0206(18) O7 0.033(2) 0.044(2) 0.020(3) 0.0018(18) 0.0016(17) 0.0167(19) O8 0.031(2) 0.034(2) 0.023(2) -0.0083(17) -0.0037(17) 0.0204(19) O9 0.040(2) 0.026(2) 0.017(2) -0.0009(15) -0.0019(16) 0.0210(18) O10 0.035(2) 0.033(2) 0.027(2) -0.0036(17) -0.0035(17) 0.0193(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C31 O11 1.361(17) . ? C31 C32 1.381(2) . ? C31 C36 1.381(2) . ? C32 C33 1.380(2) . ? C32 H32 0.9400 . ? C33 C34 1.379(2) . ? C33 H33 0.9400 . ? C34 C35 1.380(2) . ? C34 O12 1.432(18) . ? C35 C36 1.380(2) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? O11 H11 0.8300 . ? O12 H12 0.8300 . ? O1W Yb1 2.303(4) . ? O2W Yb1 2.282(4) . ? O3W Yb1 2.322(4) . ? O4W Yb1 2.327(4) . ? Yb1 O1 2.273(4) . ? Yb1 O9 2.277(4) 6_554 ? Yb1 O8 2.315(4) 6_554 ? Yb1 O2 2.332(4) . ? C1 O1 1.218(7) . ? C1 N1 1.360(7) . ? C1 N2 1.378(7) . ? C2 N3 1.448(7) . ? C2 N1 1.473(8) . ? C2 C3 1.525(9) . ? C2 H2 0.9900 . ? C3 N2 1.428(7) . ? C3 N4 1.472(8) . ? C3 H3 0.9900 . ? C4 O6 1.236(7) . ? C4 N3 1.349(8) . ? C4 N4 1.377(8) . ? C5 N5 1.429(7) . ? C5 N2 1.453(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N7 1.421(9) . ? C6 N4 1.435(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.244(7) . ? C7 N5 1.344(8) . ? C7 N6 1.360(8) . ? C8 N5 1.434(7) . ? C8 N7 1.469(8) . ? C8 C9 1.542(9) . ? C8 H8 0.9900 . ? C9 N6 1.450(7) . ? C9 N8 1.457(7) . ? C9 H9 0.9900 . ? C10 O7 1.221(7) . ? C10 N8 1.357(8) . ? C10 N7 1.375(8) . ? C11 N9 1.455(9) . ? C11 N6 1.460(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.423(8) . ? C12 N8 1.450(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.217(7) . ? C13 N9 1.370(8) . ? C13 N10 1.374(8) . ? C14 N9 1.437(8) . ? C14 N11 1.463(8) . ? C14 C15 1.570(9) . ? C14 H14 0.9900 . ? C15 N10 1.430(7) . ? C15 N12 1.482(7) . ? C15 H15 0.9900 . ? C16 O8 1.224(7) . ? C16 N12 1.338(8) . ? C16 N11 1.395(8) . ? C17 N13 1.446(8) . ? C17 N10 1.449(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N12 1.418(7) . ? C18 N15 1.446(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.209(7) . ? C19 N14 1.351(7) . ? C19 N13 1.382(7) . ? C20 N15 1.432(7) . ? C20 N13 1.456(8) . ? C20 C21 1.545(8) . ? C20 H20 0.9900 . ? C21 N16 1.464(7) . ? C21 N14 1.471(7) . ? C21 H21 0.9900 . ? C22 O9 1.256(7) . ? C22 N15 1.337(8) . ? C22 N16 1.365(7) . ? C23 N17 1.446(7) . ? C23 N14 1.454(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N16 1.419(7) . ? C24 N19 1.447(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.209(7) . ? C25 N18 1.363(7) . ? C25 N17 1.373(7) . ? C26 N19 1.448(7) . ? C26 N17 1.451(7) . ? C26 C27 1.537(8) . ? C26 H26 0.9900 . ? C27 N20 1.451(7) . ? C27 N18 1.457(7) . ? C27 H27 0.9900 . ? C28 O10 1.230(7) . ? C28 N20 1.350(7) . ? C28 N19 1.369(7) . ? C29 N18 1.436(7) . ? C29 N1 1.437(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N3 1.449(7) . ? C30 N20 1.456(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O8 Yb1 2.315(4) 5 ? O9 Yb1 2.277(4) 5 ? 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 O11 C31 C32 129.2(15) . . ? O11 C31 C36 112.4(15) . . ? C32 C31 C36 118.2(14) . . ? C33 C32 C31 124.1(16) . . ? C33 C32 H32 117.9 . . ? C31 C32 H32 117.9 . . ? C34 C33 C32 113.6(16) . . ? C34 C33 H33 123.2 . . ? C32 C33 H33 123.2 . . ? C33 C34 C35 126.3(16) . . ? C33 C34 O12 109.7(13) . . ? C35 C34 O12 124.1(12) . . ? C36 C35 C34 116.3(16) . . ? C36 C35 H35 121.9 . . ? C34 C35 H35 121.9 . . ? C35 C36 C31 121.3(15) . . ? C35 C36 H36 119.3 . . ? C31 C36 H36 119.3 . . ? C31 O11 H11 109.5 . . ? C34 O12 H12 109.5 . . ? O1 Yb1 O9 135.08(14) . 6_554 ? O1 Yb1 O2W 78.65(16) . . ? O9 Yb1 O2W 117.32(16) 6_554 . ? O1 Yb1 O1W 116.89(16) . . ? O9 Yb1 O1W 78.72(16) 6_554 . ? O2W Yb1 O1W 140.30(14) . . ? O1 Yb1 O8 146.06(14) . 6_554 ? O9 Yb1 O8 76.18(14) 6_554 6_554 ? O2W Yb1 O8 73.33(15) . 6_554 ? O1W Yb1 O8 76.43(15) . 6_554 ? O1 Yb1 O3W 72.40(15) . . ? O9 Yb1 O3W 74.08(15) 6_554 . ? O2W Yb1 O3W 145.48(15) . . ? O1W Yb1 O3W 71.68(15) . . ? O8 Yb1 O3W 139.76(15) 6_554 . ? O1 Yb1 O4W 75.28(15) . . ? O9 Yb1 O4W 71.77(14) 6_554 . ? O2W Yb1 O4W 71.54(15) . . ? O1W Yb1 O4W 145.45(15) . . ? O8 Yb1 O4W 112.39(16) 6_554 . ? O3W Yb1 O4W 83.09(16) . . ? O1 Yb1 O2 75.71(14) . . ? O9 Yb1 O2 146.34(14) 6_554 . ? O2W Yb1 O2 76.28(15) . . ? O1W Yb1 O2 73.32(15) . . ? O8 Yb1 O2 79.32(14) 6_554 . ? O3W Yb1 O2 113.20(16) . . ? O4W Yb1 O2 140.05(14) . . ? O1 C1 N1 125.3(5) . . ? O1 C1 N2 126.2(5) . . ? N1 C1 N2 108.5(5) . . ? N3 C2 N1 113.7(5) . . ? N3 C2 C3 104.2(5) . . ? N1 C2 C3 103.1(5) . . ? N3 C2 H2 111.8 . . ? N1 C2 H2 111.8 . . ? C3 C2 H2 111.8 . . ? N2 C3 N4 114.8(5) . . ? N2 C3 C2 104.6(5) . . ? N4 C3 C2 103.4(5) . . ? N2 C3 H3 111.2 . . ? N4 C3 H3 111.2 . . ? C2 C3 H3 111.2 . . ? O6 C4 N3 126.0(5) . . ? O6 C4 N4 124.7(5) . . ? N3 C4 N4 109.1(5) . . ? N5 C5 N2 112.8(5) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 C6 N4 115.4(5) . . ? N7 C6 H6A 108.4 . . ? N4 C6 H6A 108.4 . . ? N7 C6 H6B 108.4 . . ? N4 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? O2 C7 N5 127.4(6) . . ? O2 C7 N6 123.5(5) . . ? N5 C7 N6 109.1(5) . . ? N5 C8 N7 114.1(5) . . ? N5 C8 C9 102.9(5) . . ? N7 C8 C9 103.6(5) . . ? N5 C8 H8 111.9 . . ? N7 C8 H8 111.9 . . ? C9 C8 H8 111.9 . . ? N6 C9 N8 115.8(5) . . ? N6 C9 C8 103.5(5) . . ? N8 C9 C8 103.0(5) . . ? N6 C9 H9 111.3 . . ? N8 C9 H9 111.3 . . ? C8 C9 H9 111.3 . . ? O7 C10 N8 126.6(6) . . ? O7 C10 N7 124.5(6) . . ? N8 C10 N7 108.9(5) . . ? N9 C11 N6 112.6(5) . . ? N9 C11 H11A 109.1 . . ? N6 C11 H11A 109.1 . . ? N9 C11 H11B 109.1 . . ? N6 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N11 C12 N8 114.0(5) . . ? N11 C12 H12A 108.8 . . ? N8 C12 H12A 108.8 . . ? N11 C12 H12B 108.8 . . ? N8 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O3 C13 N9 125.7(6) . . ? O3 C13 N10 126.4(6) . . ? N9 C13 N10 107.8(5) . . ? N9 C14 N11 115.2(5) . . ? N9 C14 C15 101.3(5) . . ? N11 C14 C15 103.1(4) . . ? N9 C14 H14 112.1 . . ? N11 C14 H14 112.1 . . ? C15 C14 H14 112.1 . . ? N10 C15 N12 114.8(4) . . ? N10 C15 C14 104.6(5) . . ? N12 C15 C14 102.4(4) . . ? N10 C15 H15 111.5 . . ? N12 C15 H15 111.5 . . ? C14 C15 H15 111.5 . . ? O8 C16 N12 127.9(6) . . ? O8 C16 N11 123.2(6) . . ? N12 C16 N11 108.9(5) . . ? N13 C17 N10 113.0(5) . . ? N13 C17 H17A 109.0 . . ? N10 C17 H17A 109.0 . . ? N13 C17 H17B 109.0 . . ? N10 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N12 C18 N15 113.8(4) . . ? N12 C18 H18A 108.8 . . ? N15 C18 H18A 108.8 . . ? N12 C18 H18B 108.8 . . ? N15 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? O4 C19 N14 126.7(5) . . ? O4 C19 N13 125.0(5) . . ? N14 C19 N13 108.3(5) . . ? N15 C20 N13 115.3(5) . . ? N15 C20 C21 103.6(4) . . ? N13 C20 C21 103.9(4) . . ? N15 C20 H20 111.2 . . ? N13 C20 H20 111.2 . . ? C21 C20 H20 111.2 . . ? N16 C21 N14 113.8(4) . . ? N16 C21 C20 103.6(4) . . ? N14 C21 C20 102.6(4) . . ? N16 C21 H21 112.1 . . ? N14 C21 H21 112.1 . . ? C20 C21 H21 112.1 . . ? O9 C22 N15 126.5(5) . . ? O9 C22 N16 122.3(5) . . ? N15 C22 N16 111.2(5) . . ? N17 C23 N14 114.9(5) . . ? N17 C23 H23A 108.6 . . ? N14 C23 H23A 108.6 . . ? N17 C23 H23B 108.6 . . ? N14 C23 H23B 108.6 . . ? H23A C23 H23B 107.5 . . ? N16 C24 N19 114.6(4) . . ? N16 C24 H24A 108.6 . . ? N19 C24 H24A 108.6 . . ? N16 C24 H24B 108.6 . . ? N19 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? O5 C25 N18 127.1(5) . . ? O5 C25 N17 125.0(5) . . ? N18 C25 N17 107.9(5) . . ? N19 C26 N17 115.7(4) . . ? N19 C26 C27 102.4(4) . . ? N17 C26 C27 103.9(4) . . ? N19 C26 H26 111.4 . . ? N17 C26 H26 111.4 . . ? C27 C26 H26 111.4 . . ? N20 C27 N18 114.3(4) . . ? N20 C27 C26 103.5(4) . . ? N18 C27 C26 102.7(4) . . ? N20 C27 H27 111.9 . . ? N18 C27 H27 111.9 . . ? C26 C27 H27 111.9 . . ? O10 C28 N20 125.2(5) . . ? O10 C28 N19 127.0(5) . . ? N20 C28 N19 107.8(5) . . ? N18 C29 N1 113.0(4) . . ? N18 C29 H29A 109.0 . . ? N1 C29 H29A 109.0 . . ? N18 C29 H29B 109.0 . . ? N1 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? N3 C30 N20 114.3(4) . . ? N3 C30 H30A 108.7 . . ? N20 C30 H30A 108.7 . . ? N3 C30 H30B 108.7 . . ? N20 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C1 N1 C29 121.7(5) . . ? C1 N1 C2 111.5(5) . . ? C29 N1 C2 124.9(4) . . ? C1 N2 C3 112.2(5) . . ? C1 N2 C5 119.9(5) . . ? C3 N2 C5 127.8(5) . . ? C4 N3 C2 112.4(5) . . ? C4 N3 C30 122.7(5) . . ? C2 N3 C30 124.4(5) . . ? C4 N4 C6 124.3(5) . . ? C4 N4 C3 110.9(5) . . ? C6 N4 C3 124.5(5) . . ? C7 N5 C5 123.2(5) . . ? C7 N5 C8 113.0(5) . . ? C5 N5 C8 123.8(5) . . ? C7 N6 C9 111.0(5) . . ? C7 N6 C11 122.3(5) . . ? C9 N6 C11 124.5(5) . . ? C10 N7 C6 123.4(5) . . ? C10 N7 C8 111.0(5) . . ? C6 N7 C8 124.0(5) . . ? C10 N8 C12 122.0(5) . . ? C10 N8 C9 112.8(5) . . ? C12 N8 C9 125.1(5) . . ? C13 N9 C14 114.0(5) . . ? C13 N9 C11 121.0(5) . . ? C14 N9 C11 125.0(5) . . ? C13 N10 C15 111.6(5) . . ? C13 N10 C17 121.8(5) . . ? C15 N10 C17 124.3(5) . . ? C16 N11 C12 123.0(5) . . ? C16 N11 C14 111.9(5) . . ? C12 N11 C14 123.0(5) . . ? C16 N12 C18 125.2(5) . . ? C16 N12 C15 113.3(5) . . ? C18 N12 C15 121.4(4) . . ? C19 N13 C17 122.3(5) . . ? C19 N13 C20 112.0(5) . . ? C17 N13 C20 125.4(5) . . ? C19 N14 C23 122.3(5) . . ? C19 N14 C21 113.1(4) . . ? C23 N14 C21 123.5(5) . . ? C22 N15 C20 111.9(5) . . ? C22 N15 C18 122.3(5) . . ? C20 N15 C18 125.8(4) . . ? C22 N16 C24 123.7(5) . . ? C22 N16 C21 109.5(5) . . ? C24 N16 C21 124.6(4) . . ? C25 N17 C23 120.3(5) . . ? C25 N17 C26 111.8(4) . . ? C23 N17 C26 123.9(4) . . ? C25 N18 C29 124.0(4) . . ? C25 N18 C27 112.9(4) . . ? C29 N18 C27 122.9(4) . . ? C28 N19 C24 124.3(5) . . ? C28 N19 C26 113.0(4) . . ? C24 N19 C26 121.9(5) . . ? C28 N20 C27 112.4(5) . . ? C28 N20 C30 121.0(5) . . ? C27 N20 C30 122.7(4) . . ? C1 O1 Yb1 154.7(4) . . ? C7 O2 Yb1 149.6(4) . . ? C16 O8 Yb1 147.1(4) . 5 ? C22 O9 Yb1 149.4(4) . 5 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.135 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.098 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 1.000 0.050 1412 637 ' ' 2 -0.059 0.537 0.447 45 11 ' ' 3 0.059 0.462 0.947 45 11 ' ' 4 0.403 0.941 0.614 45 11 ' ' 5 0.462 0.403 0.781 45 11 ' ' 6 0.537 0.597 0.281 45 11 ' ' 7 0.596 0.059 0.114 45 11 ' ' _platon_squeeze_details ; ; data_08 _database_code_depnum_ccdc_archive 'CCDC 875771' #TrackingRef 'submit-08.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H74 Cl3 Lu N20 O29' _chemical_formula_weight 1532.47 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' Lu Lu -0.4720 5.8584 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 61' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, x, z+1/6' 'y, -x+y, z+5/6' _cell_length_a 14.515(4) _cell_length_b 14.515 _cell_length_c 45.826(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8361(3) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 2.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6642 _exptl_absorpt_correction_T_max 0.8079 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53064 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.10 _reflns_number_total 9487 _reflns_number_gt 9130 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+100.2557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 9487 _refine_ls_number_parameters 602 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1684 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.8287(10) -1.4315(11) 0.1473(4) 0.106(5) Uani 0.50 1 d P . . Cl2 Cl -1.0082(13) -1.5959(16) 0.1245(6) 0.160(9) Uani 0.50 1 d P . . Cl3 Cl -1.032(3) -1.555(3) 0.0600(13) 0.160(9) Uani 0.232(18) 1 d P A 1 Cl4 Cl -0.875(2) -1.5545(16) 0.0460(12) 0.53(4) Uani 0.768(18) 1 d P A 2 Cl5 Cl -0.937(3) -0.7851(13) 0.0881(10) 0.56(3) Uani 1 1 d . . . O1W O -0.4802(6) -1.1503(6) 0.0944(3) 0.0310(18) Uani 1 1 d . . . O2W O -0.4607(6) -1.4359(6) 0.0928(2) 0.0298(18) Uani 1 1 d . . . O3W O -0.6670(7) -1.4962(7) 0.0839(2) 0.030(2) Uani 1 1 d . . . O4W O -0.6716(6) -1.3067(6) 0.1110(2) 0.0279(19) Uani 1 1 d . . . Lu1 Lu -0.53219(3) -1.32578(4) 0.09496(8) 0.01907(13) Uani 1 1 d . . . C31 C -0.8593(9) -1.0073(9) 0.1073(3) 0.056(6) Uani 1 1 d D . . C32 C -0.9260(14) -1.0405(15) 0.0834(3) 0.075(7) Uani 1 1 d D . . H32 H -0.9460 -0.9954 0.0741 0.090 Uiso 1 1 calc R . . C33 C -0.9620(17) -1.1429(14) 0.0737(4) 0.082(7) Uani 1 1 d D . . H33 H -1.0045 -1.1691 0.0569 0.098 Uiso 1 1 calc R . . C34 C -0.9335(14) -1.2057(17) 0.0896(4) 0.095(10) Uani 1 1 d D . . C35 C -0.8608(14) -1.1721(10) 0.1121(4) 0.097(10) Uani 1 1 d D . . H35 H -0.8356 -1.2149 0.1201 0.117 Uiso 1 1 calc R . . C36 C -0.8283(9) -1.0705(9) 0.1219(2) 0.0256(9) Uani 1 1 d D . . H36 H -0.7850 -1.0443 0.1386 0.031 Uiso 1 1 calc R . . O11 O -0.8139(14) -0.9078(15) 0.1200(5) 0.118(5) Uani 1 1 d . . . H11 H -0.8360 -0.8718 0.1116 0.176 Uiso 1 1 calc R . . O12 O -0.9798(14) -1.3140(15) 0.0765(5) 0.118(5) Uani 1 1 d . . . H12 H -0.9580 -1.3489 0.0855 0.176 Uiso 1 1 calc R . . C1 C -0.6476(9) -1.3364(9) 0.0283(2) 0.0193(10) Uani 1 1 d . . . C2 C -0.7505(10) -1.3646(9) -0.0138(3) 0.028(3) Uani 1 1 d . . . H2 H -0.8237 -1.4251 -0.0164 0.034 Uiso 1 1 calc R . . C3 C -0.6625(9) -1.3954(8) -0.0193(3) 0.018(2) Uani 1 1 d . . . H3 H -0.6954 -1.4706 -0.0256 0.022 Uiso 1 1 calc R . . C4 C -0.6358(9) -1.2572(9) -0.0510(3) 0.0193(10) Uani 1 1 d . . . C5 C -0.5283(9) -1.4063(10) 0.0151(3) 0.0256(9) Uani 1 1 d . . . H5A H -0.5380 -1.4321 0.0352 0.031 Uiso 1 1 calc R . . H5B H -0.5357 -1.4637 0.0023 0.031 Uiso 1 1 calc R . . C6 C -0.5048(11) -1.3190(10) -0.0540(3) 0.0256(9) Uani 1 1 d . . . H6A H -0.4939 -1.2937 -0.0742 0.031 Uiso 1 1 calc R . . H6B H -0.5145 -1.3908 -0.0541 0.031 Uiso 1 1 calc R . . C7 C -0.3739(9) -1.2522(8) 0.0341(3) 0.018(2) Uani 1 1 d . . . C8 C -0.3680(9) -1.2906(9) -0.0151(3) 0.025(3) Uani 1 1 d . . . H8 H -0.3579 -1.3488 -0.0226 0.030 Uiso 1 1 calc R . . C9 C -0.2589(9) -1.1889(9) -0.0063(3) 0.018(2) Uani 1 1 d . . . H9 H -0.1990 -1.2029 -0.0080 0.022 Uiso 1 1 calc R . . C10 C -0.3384(9) -1.1481(9) -0.0457(3) 0.0193(10) Uani 1 1 d . . . C11 C -0.1918(9) -1.0898(10) 0.0425(3) 0.0256(9) Uani 1 1 d . . . H11A H -0.2071 -1.1156 0.0626 0.031 Uiso 1 1 calc R . . H11B H -0.1227 -1.0815 0.0371 0.031 Uiso 1 1 calc R . . C12 C -0.1644(10) -1.0003(11) -0.0296(3) 0.031(3) Uani 1 1 d . . . H12A H -0.0973 -0.9991 -0.0259 0.037 Uiso 1 1 calc R . . H12B H -0.1607 -0.9734 -0.0495 0.037 Uiso 1 1 calc R . . C13 C -0.2315(9) -0.9552(9) 0.0618(2) 0.023(3) Uani 1 1 d . . . C14 C -0.1258(9) -0.9081(8) 0.0191(3) 0.021(2) Uani 1 1 d . . . H14 H -0.0498 -0.8879 0.0188 0.025 Uiso 1 1 calc R . . C15 C -0.1430(9) -0.8144(9) 0.0296(3) 0.022(2) Uani 1 1 d . . . H15 H -0.0746 -0.7519 0.0355 0.026 Uiso 1 1 calc R . . C16 C -0.2040(9) -0.8567(9) -0.0178(3) 0.0193(10) Uani 1 1 d . . . C17 C -0.2411(9) -0.7944(10) 0.0737(3) 0.0256(9) Uani 1 1 d . . . H17A H -0.1831 -0.7204 0.0728 0.031 Uiso 1 1 calc R . . H17B H -0.2455 -0.8191 0.0938 0.031 Uiso 1 1 calc R . . C18 C -0.2162(9) -0.7079(10) 0.0049(3) 0.0256(9) Uani 1 1 d . . . H18A H -0.1662 -0.6502 0.0177 0.031 Uiso 1 1 calc R . . H18B H -0.2102 -0.6782 -0.0147 0.031 Uiso 1 1 calc R . . C19 C -0.4352(9) -0.8720(9) 0.0782(3) 0.020(2) Uani 1 1 d . . . C20 C -0.3509(8) -0.7325(9) 0.0445(3) 0.0170(13) Uani 1 1 d . . . H20 H -0.3139 -0.6566 0.0502 0.020 Uiso 1 1 calc R . . C21 C -0.4728(8) -0.7797(8) 0.0426(3) 0.0170(13) Uani 1 1 d . . . H21 H -0.4932 -0.7252 0.0466 0.020 Uiso 1 1 calc R . . C22 C -0.4101(9) -0.7987(9) -0.0022(2) 0.0193(10) Uani 1 1 d . . . C23 C -0.6252(9) -0.9383(9) 0.0696(3) 0.023(2) Uani 1 1 d . . . H23A H -0.6334 -0.9702 0.0889 0.027 Uiso 1 1 calc R . . H23B H -0.6645 -0.8996 0.0697 0.027 Uiso 1 1 calc R . . C24 C -0.5991(9) -0.8520(9) -0.0011(3) 0.022(2) Uani 1 1 d . . . H24A H -0.6341 -0.8184 0.0091 0.027 Uiso 1 1 calc R . . H24B H -0.5850 -0.8246 -0.0211 0.027 Uiso 1 1 calc R . . C25 C -0.6957(8) -1.1216(9) 0.0558(2) 0.018(2) Uani 1 1 d . . . C26 C -0.7338(8) -1.0219(8) 0.0234(2) 0.018(2) Uani 1 1 d . . . H26 H -0.7870 -1.0010 0.0286 0.021 Uiso 1 1 calc R . . C27 C -0.7870(8) -1.1373(8) 0.0125(3) 0.0170(13) Uani 1 1 d . . . H27 H -0.8648 -1.1681 0.0103 0.020 Uiso 1 1 calc R . . C28 C -0.6750(9) -1.0320(10) -0.0246(3) 0.025(3) Uani 1 1 d . . . C29 C -0.7942(9) -1.3039(10) 0.0345(3) 0.0256(9) Uani 1 1 d . . . H29A H -0.7936 -1.3280 0.0544 0.031 Uiso 1 1 calc R . . H29B H -0.8672 -1.3448 0.0271 0.031 Uiso 1 1 calc R . . C30 C -0.7771(10) -1.2181(10) -0.0361(3) 0.0256(9) Uani 1 1 d . . . H30A H -0.7711 -1.1902 -0.0560 0.031 Uiso 1 1 calc R . . H30B H -0.8529 -1.2656 -0.0321 0.031 Uiso 1 1 calc R . . N1 N -0.7263(7) -1.3248(6) 0.0167(2) 0.0119(17) Uani 1 1 d . . . N2 N -0.6119(7) -1.3812(7) 0.0080(2) 0.0175(19) Uani 1 1 d . . . N3 N -0.7224(8) -1.2805(7) -0.0350(2) 0.022(2) Uani 1 1 d . . . N4 N -0.6010(9) -1.3249(8) -0.0431(2) 0.029(2) Uani 1 1 d . . . N5 N -0.4230(7) -1.3169(7) 0.0120(2) 0.0181(19) Uani 1 1 d . . . N6 N -0.2743(8) -1.1692(8) 0.0232(2) 0.022(2) Uani 1 1 d . . . N7 N -0.4097(8) -1.2497(9) -0.0372(2) 0.028(2) Uani 1 1 d . . . N8 N -0.2497(7) -1.1088(7) -0.0285(2) 0.022(2) Uani 1 1 d . . . N9 N -0.1855(8) -0.9874(8) 0.0409(3) 0.028(2) Uani 1 1 d . . . N10 N -0.2153(7) -0.8585(7) 0.0547(2) 0.0200(11) Uani 1 1 d . . . N11 N -0.1727(7) -0.9299(8) -0.0097(2) 0.019(2) Uani 1 1 d . . . N12 N -0.1870(7) -0.7900(7) 0.0037(2) 0.0200(11) Uani 1 1 d . . . N13 N -0.3408(8) -0.7979(8) 0.0664(3) 0.027(2) Uani 1 1 d . . . N14 N -0.5130(7) -0.8620(7) 0.0650(2) 0.0153(18) Uani 1 1 d . . . N15 N -0.3214(7) -0.7469(7) 0.0154(2) 0.0175(19) Uani 1 1 d . . . N16 N -0.4991(7) -0.8199(7) 0.0130(2) 0.0164(18) Uani 1 1 d . . . N17 N -0.6731(7) -1.0215(7) 0.0487(2) 0.020(2) Uani 1 1 d . . . N18 N -0.7623(7) -1.1911(7) 0.0351(2) 0.0159(18) Uani 1 1 d . . . N19 N -0.6703(7) -0.9624(7) -0.0022(2) 0.0169(19) Uani 1 1 d . . . N20 N -0.7358(7) -1.1292(7) -0.0156(2) 0.0200(11) Uani 1 1 d . . . O1 O -0.6145(7) -1.3153(7) 0.0538(2) 0.0251(18) Uani 1 1 d . . . O2 O -0.3982(7) -1.2562(6) 0.05986(19) 0.0248(18) Uani 1 1 d . . . O3 O -0.2750(7) -1.0061(7) 0.0839(2) 0.030(2) Uani 1 1 d . . . O4 O -0.4491(6) -0.9356(6) 0.0971(2) 0.0226(16) Uani 1 1 d . . . O5 O -0.6635(7) -1.1445(6) 0.07773(19) 0.0253(18) Uani 1 1 d . . . O6 O -0.6015(7) -1.1949(7) -0.0710(2) 0.0323(18) Uani 1 1 d . . . O7 O -0.3486(6) -1.1007(7) -0.0664(2) 0.0284(19) Uani 1 1 d . . . O8 O -0.2394(7) -0.8548(6) -0.0432(2) 0.0233(17) Uani 1 1 d . . . O9 O -0.4106(6) -0.8244(6) -0.02811(18) 0.0191(16) Uani 1 1 d . . . O10 O -0.6298(7) -1.0001(7) -0.0480(2) 0.0278(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.072(7) 0.089(8) 0.154(14) 0.035(9) 0.036(8) 0.038(7) Cl2 0.075(9) 0.129(13) 0.25(2) -0.072(15) -0.002(11) 0.032(8) Cl3 0.075(9) 0.129(13) 0.25(2) -0.072(15) -0.002(11) 0.032(8) Cl4 0.26(3) 0.142(16) 1.18(12) 0.33(4) 0.19(4) 0.103(17) Cl5 0.60(5) 0.098(10) 0.74(7) 0.13(2) 0.08(5) -0.017(18) O1W 0.019(4) 0.026(4) 0.047(5) -0.007(4) -0.004(4) 0.012(3) O2W 0.033(4) 0.026(4) 0.037(5) -0.002(4) -0.001(4) 0.020(4) O3W 0.026(4) 0.024(4) 0.034(5) -0.002(3) -0.007(3) 0.008(4) O4W 0.023(4) 0.019(4) 0.032(5) 0.016(3) 0.000(3) 0.003(3) Lu1 0.0226(2) 0.0211(2) 0.0135(2) 0.00271(18) -0.00118(19) 0.01089(19) C31 0.016(6) 0.016(6) 0.137(19) 0.029(8) 0.042(9) 0.010(5) C32 0.088(16) 0.097(17) 0.068(14) 0.030(12) 0.049(12) 0.067(14) C33 0.092(16) 0.098(17) 0.066(15) 0.016(12) 0.044(12) 0.055(15) C34 0.044(11) 0.073(14) 0.16(3) 0.010(16) 0.058(15) 0.024(11) C35 0.061(13) 0.102(18) 0.16(3) 0.088(18) 0.082(16) 0.062(14) C36 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) O11 0.089(9) 0.098(10) 0.160(15) 0.028(9) 0.050(9) 0.042(8) O12 0.089(9) 0.098(10) 0.160(15) 0.028(9) 0.050(9) 0.042(8) C1 0.023(3) 0.021(2) 0.010(2) -0.0005(19) 0.0032(19) 0.009(2) C2 0.036(7) 0.016(6) 0.026(7) 0.010(5) 0.002(5) 0.008(5) C3 0.025(6) 0.009(5) 0.017(6) 0.002(4) -0.005(4) 0.005(4) C4 0.023(3) 0.021(2) 0.010(2) -0.0005(19) 0.0032(19) 0.009(2) C5 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) C6 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) C7 0.023(6) 0.013(5) 0.024(6) 0.004(4) 0.000(4) 0.013(5) C8 0.015(5) 0.023(6) 0.039(8) 0.003(5) 0.007(5) 0.011(5) C9 0.026(6) 0.022(6) 0.017(6) 0.009(4) 0.009(4) 0.020(5) C10 0.023(3) 0.021(2) 0.010(2) -0.0005(19) 0.0032(19) 0.009(2) C11 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) C12 0.025(6) 0.044(8) 0.029(7) 0.002(6) 0.002(5) 0.022(6) C13 0.020(6) 0.031(6) 0.005(5) 0.004(4) 0.004(4) 0.003(5) C14 0.012(5) 0.015(5) 0.025(7) 0.005(4) -0.003(4) -0.001(4) C15 0.018(5) 0.024(6) 0.022(6) 0.009(5) 0.003(4) 0.009(5) C16 0.023(3) 0.021(2) 0.010(2) -0.0005(19) 0.0032(19) 0.009(2) C17 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) C18 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) C19 0.023(6) 0.022(6) 0.018(6) -0.005(5) 0.003(4) 0.014(5) C20 0.013(3) 0.018(3) 0.023(4) 0.003(2) 0.002(2) 0.010(3) C21 0.013(3) 0.018(3) 0.023(4) 0.003(2) 0.002(2) 0.010(3) C22 0.023(3) 0.021(2) 0.010(2) -0.0005(19) 0.0032(19) 0.009(2) C23 0.019(6) 0.021(6) 0.035(7) -0.003(5) 0.001(5) 0.014(5) C24 0.027(6) 0.031(6) 0.010(6) -0.002(4) 0.000(4) 0.015(5) C25 0.006(5) 0.028(6) 0.014(6) 0.001(4) 0.004(4) 0.005(4) C26 0.017(5) 0.019(5) 0.012(5) 0.007(4) 0.004(4) 0.006(4) C27 0.013(3) 0.018(3) 0.023(4) 0.003(2) 0.002(2) 0.010(3) C28 0.018(6) 0.038(7) 0.022(7) 0.005(5) 0.000(5) 0.016(5) C29 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) C30 0.024(2) 0.031(2) 0.020(2) 0.0035(17) 0.0001(17) 0.0132(18) N1 0.019(4) 0.004(4) 0.012(4) 0.001(3) -0.002(3) 0.005(3) N2 0.016(4) 0.011(4) 0.020(5) 0.004(3) 0.003(4) 0.002(4) N3 0.037(6) 0.016(5) 0.011(5) -0.003(3) -0.001(4) 0.011(4) N4 0.046(7) 0.031(6) 0.020(6) 0.005(4) -0.003(5) 0.025(5) N5 0.022(5) 0.013(4) 0.017(5) 0.001(4) -0.001(4) 0.006(4) N6 0.024(5) 0.034(5) 0.004(5) 0.003(4) -0.002(4) 0.011(4) N7 0.032(6) 0.039(6) 0.021(6) 0.002(4) 0.005(4) 0.024(5) N8 0.022(5) 0.021(5) 0.026(6) 0.004(4) 0.001(4) 0.012(4) N9 0.017(5) 0.027(5) 0.035(6) -0.001(4) -0.002(4) 0.007(4) N10 0.019(3) 0.022(3) 0.013(3) -0.003(2) -0.002(2) 0.006(2) N11 0.015(4) 0.037(5) 0.009(5) -0.005(4) -0.006(3) 0.016(4) N12 0.019(3) 0.022(3) 0.013(3) -0.003(2) -0.002(2) 0.006(2) N13 0.019(5) 0.033(6) 0.029(7) 0.010(4) 0.005(4) 0.012(4) N14 0.020(5) 0.013(4) 0.008(4) 0.007(3) 0.004(3) 0.006(4) N15 0.012(4) 0.014(4) 0.017(5) -0.008(3) -0.003(3) 0.000(3) N16 0.018(4) 0.020(4) 0.015(5) 0.010(4) 0.012(4) 0.013(4) N17 0.019(5) 0.020(5) 0.021(5) 0.001(4) 0.005(4) 0.010(4) N18 0.018(4) 0.017(4) 0.020(5) 0.001(4) -0.005(4) 0.014(4) N19 0.030(5) 0.013(4) 0.011(5) 0.009(3) 0.010(4) 0.013(4) N20 0.019(3) 0.022(3) 0.013(3) -0.003(2) -0.002(2) 0.006(2) O1 0.034(5) 0.032(5) 0.022(4) -0.003(3) 0.002(3) 0.025(4) O2 0.030(4) 0.028(4) 0.016(5) 0.005(3) 0.001(3) 0.014(4) O3 0.039(5) 0.025(4) 0.024(5) 0.001(3) 0.001(4) 0.014(4) O4 0.021(4) 0.025(4) 0.024(4) 0.010(4) 0.005(3) 0.014(3) O5 0.039(5) 0.026(4) 0.010(4) 0.002(3) -0.005(3) 0.015(4) O6 0.040(5) 0.040(5) 0.020(4) 0.000(4) 0.000(4) 0.022(4) O7 0.028(4) 0.036(5) 0.021(5) 0.008(4) 0.005(3) 0.015(4) O8 0.028(4) 0.024(4) 0.021(4) 0.007(3) 0.004(3) 0.015(4) O9 0.016(4) 0.023(4) 0.010(4) 0.000(3) -0.003(3) 0.004(3) O10 0.031(5) 0.028(5) 0.018(4) 0.004(3) 0.001(4) 0.010(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 O1W Lu1 2.265(8) . ? O2W Lu1 2.301(7) . ? O3W Lu1 2.316(8) . ? O4W Lu1 2.296(9) . ? Lu1 O9 2.271(8) 5_445 ? Lu1 O8 2.278(8) 5_445 ? Lu1 O1 2.279(8) . ? Lu1 O2 2.329(8) . ? C31 C32 1.380(2) . ? C31 O11 1.38(2) . ? C31 C36 1.380(2) . ? C32 C33 1.380(2) . ? C32 H32 0.9400 . ? C33 C34 1.380(2) . ? C33 H33 0.9400 . ? C34 C35 1.380(2) . ? C34 O12 1.49(3) . ? C35 C36 1.380(2) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? O11 H11 0.8300 . ? O12 H12 0.8300 . ? C1 O1 1.241(14) . ? C1 N1 1.344(14) . ? C1 N2 1.377(14) . ? C2 N3 1.450(14) . ? C2 N1 1.487(16) . ? C2 C3 1.570(17) . ? C2 H2 0.9900 . ? C3 N2 1.412(14) . ? C3 N4 1.456(15) . ? C3 H3 0.9900 . ? C4 O6 1.206(14) . ? C4 N3 1.344(15) . ? C4 N4 1.359(15) . ? C5 N5 1.434(14) . ? C5 N2 1.468(15) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 N4 1.444(17) . ? C6 N7 1.456(17) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 O2 1.227(14) . ? C7 N5 1.321(15) . ? C7 N6 1.431(15) . ? C8 N5 1.420(16) . ? C8 N7 1.449(16) . ? C8 C9 1.585(16) . ? C8 H8 0.9900 . ? C9 N6 1.422(15) . ? C9 N8 1.498(14) . ? C9 H9 0.9900 . ? C10 O7 1.226(14) . ? C10 N8 1.367(15) . ? C10 N7 1.368(16) . ? C11 N9 1.445(16) . ? C11 N6 1.470(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N11 1.419(16) . ? C12 N8 1.438(16) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 O3 1.228(14) . ? C13 N10 1.341(16) . ? C13 N9 1.375(16) . ? C14 N9 1.440(15) . ? C14 N11 1.447(15) . ? C14 C15 1.575(17) . ? C14 H14 0.9900 . ? C15 N10 1.470(14) . ? C15 N12 1.471(14) . ? C15 H15 0.9900 . ? C16 O8 1.278(14) . ? C16 N12 1.316(14) . ? C16 N11 1.398(15) . ? C17 N10 1.455(15) . ? C17 N13 1.461(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 N15 1.421(15) . ? C18 N12 1.453(16) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 O4 1.207(14) . ? C19 N14 1.351(15) . ? C19 N13 1.361(15) . ? C20 N13 1.439(15) . ? C20 N15 1.446(14) . ? C20 C21 1.548(14) . ? C20 H20 0.9900 . ? C21 N16 1.453(15) . ? C21 N14 1.457(13) . ? C21 H21 0.9900 . ? C22 O9 1.244(13) . ? C22 N16 1.360(14) . ? C22 N15 1.380(14) . ? C23 N17 1.418(15) . ? C23 N14 1.456(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 N19 1.408(15) . ? C24 N16 1.436(15) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 O5 1.222(14) . ? C25 N17 1.360(15) . ? C25 N18 1.369(14) . ? C26 N17 1.458(15) . ? C26 N19 1.472(12) . ? C26 C27 1.535(15) . ? C26 H26 0.9900 . ? C27 N18 1.447(13) . ? C27 N20 1.461(14) . ? C27 H27 0.9900 . ? C28 O10 1.223(15) . ? C28 N20 1.302(16) . ? C28 N19 1.418(16) . ? C29 N1 1.425(15) . ? C29 N18 1.462(15) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 N20 1.463(15) . ? C30 N3 1.474(15) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? O8 Lu1 2.278(8) 6_654 ? O9 Lu1 2.271(8) 6_654 ? 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 O1W Lu1 O9 116.7(3) . 5_445 ? O1W Lu1 O8 72.2(3) . 5_445 ? O9 Lu1 O8 76.6(3) 5_445 5_445 ? O1W Lu1 O1 78.9(3) . . ? O9 Lu1 O1 135.6(3) 5_445 . ? O8 Lu1 O1 145.0(3) 5_445 . ? O1W Lu1 O4W 71.7(3) . . ? O9 Lu1 O4W 72.4(3) 5_445 . ? O8 Lu1 O4W 113.1(3) 5_445 . ? O1 Lu1 O4W 74.6(3) . . ? O1W Lu1 O2W 140.1(3) . . ? O9 Lu1 O2W 79.3(3) 5_445 . ? O8 Lu1 O2W 77.3(3) 5_445 . ? O1 Lu1 O2W 116.3(3) . . ? O4W Lu1 O2W 145.9(3) . . ? O1W Lu1 O3W 145.8(3) . . ? O9 Lu1 O3W 74.6(3) 5_445 . ? O8 Lu1 O3W 140.6(3) 5_445 . ? O1 Lu1 O3W 72.5(3) . . ? O4W Lu1 O3W 82.7(3) . . ? O2W Lu1 O3W 71.5(3) . . ? O1W Lu1 O2 76.6(3) . . ? O9 Lu1 O2 146.0(3) 5_445 . ? O8 Lu1 O2 78.8(3) 5_445 . ? O1 Lu1 O2 75.6(3) . . ? O4W Lu1 O2 139.8(3) . . ? O2W Lu1 O2 72.7(3) . . ? O3W Lu1 O2 112.9(3) . . ? C32 C31 O11 125.7(14) . . ? C32 C31 C36 123.9(14) . . ? O11 C31 C36 110.4(16) . . ? C31 C32 C33 117.0(18) . . ? C31 C32 H32 121.5 . . ? C33 C32 H32 121.5 . . ? C32 C33 C34 118(2) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C33 C34 C35 126(2) . . ? C33 C34 O12 111.0(18) . . ? C35 C34 O12 122.4(17) . . ? C36 C35 C34 114.5(17) . . ? C36 C35 H35 122.8 . . ? C34 C35 H35 122.8 . . ? C35 C36 C31 120.1(13) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C31 O11 H11 109.5 . . ? C34 O12 H12 109.5 . . ? O1 C1 N1 126.2(10) . . ? O1 C1 N2 124.2(10) . . ? N1 C1 N2 109.5(9) . . ? N3 C2 N1 113.0(9) . . ? N3 C2 C3 101.9(9) . . ? N1 C2 C3 101.1(9) . . ? N3 C2 H2 113.2 . . ? N1 C2 H2 113.2 . . ? C3 C2 H2 113.2 . . ? N2 C3 N4 118.0(9) . . ? N2 C3 C2 104.8(9) . . ? N4 C3 C2 102.7(8) . . ? N2 C3 H3 110.3 . . ? N4 C3 H3 110.3 . . ? C2 C3 H3 110.3 . . ? O6 C4 N3 125.8(11) . . ? O6 C4 N4 125.6(10) . . ? N3 C4 N4 108.1(10) . . ? N5 C5 N2 113.1(9) . . ? N5 C5 H5A 109.0 . . ? N2 C5 H5A 109.0 . . ? N5 C5 H5B 109.0 . . ? N2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N4 C6 N7 114.4(11) . . ? N4 C6 H6A 108.7 . . ? N7 C6 H6A 108.7 . . ? N4 C6 H6B 108.7 . . ? N7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? O2 C7 N5 131.6(11) . . ? O2 C7 N6 121.4(10) . . ? N5 C7 N6 106.9(10) . . ? N5 C8 N7 115.2(9) . . ? N5 C8 C9 101.2(9) . . ? N7 C8 C9 102.9(9) . . ? N5 C8 H8 112.2 . . ? N7 C8 H8 112.2 . . ? C9 C8 H8 112.2 . . ? N6 C9 N8 116.8(9) . . ? N6 C9 C8 104.1(9) . . ? N8 C9 C8 102.1(9) . . ? N6 C9 H9 111.0 . . ? N8 C9 H9 111.0 . . ? C8 C9 H9 111.0 . . ? O7 C10 N8 124.5(10) . . ? O7 C10 N7 125.9(11) . . ? N8 C10 N7 109.5(10) . . ? N9 C11 N6 112.6(10) . . ? N9 C11 H11A 109.1 . . ? N6 C11 H11A 109.1 . . ? N9 C11 H11B 109.1 . . ? N6 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N11 C12 N8 115.3(10) . . ? N11 C12 H12A 108.4 . . ? N8 C12 H12A 108.4 . . ? N11 C12 H12B 108.4 . . ? N8 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? O3 C13 N10 126.7(11) . . ? O3 C13 N9 124.2(12) . . ? N10 C13 N9 109.0(10) . . ? N9 C14 N11 115.4(9) . . ? N9 C14 C15 100.8(9) . . ? N11 C14 C15 102.0(9) . . ? N9 C14 H14 112.5 . . ? N11 C14 H14 112.5 . . ? C15 C14 H14 112.5 . . ? N10 C15 N12 115.7(9) . . ? N10 C15 C14 104.4(9) . . ? N12 C15 C14 103.8(9) . . ? N10 C15 H15 110.8 . . ? N12 C15 H15 110.8 . . ? C14 C15 H15 110.8 . . ? O8 C16 N12 126.6(11) . . ? O8 C16 N11 122.9(10) . . ? N12 C16 N11 110.5(10) . . ? N10 C17 N13 114.1(10) . . ? N10 C17 H17A 108.7 . . ? N13 C17 H17A 108.7 . . ? N10 C17 H17B 108.7 . . ? N13 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N15 C18 N12 112.5(10) . . ? N15 C18 H18A 109.1 . . ? N12 C18 H18A 109.1 . . ? N15 C18 H18B 109.1 . . ? N12 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? O4 C19 N14 125.0(10) . . ? O4 C19 N13 127.4(11) . . ? N14 C19 N13 107.7(10) . . ? N13 C20 N15 114.3(9) . . ? N13 C20 C21 102.6(9) . . ? N15 C20 C21 103.9(9) . . ? N13 C20 H20 111.8 . . ? N15 C20 H20 111.8 . . ? C21 C20 H20 111.8 . . ? N16 C21 N14 114.4(9) . . ? N16 C21 C20 104.0(8) . . ? N14 C21 C20 103.0(8) . . ? N16 C21 H21 111.6 . . ? N14 C21 H21 111.6 . . ? C20 C21 H21 111.6 . . ? O9 C22 N16 123.8(10) . . ? O9 C22 N15 125.9(10) . . ? N16 C22 N15 110.3(10) . . ? N17 C23 N14 115.9(9) . . ? N17 C23 H23A 108.3 . . ? N14 C23 H23A 108.3 . . ? N17 C23 H23B 108.3 . . ? N14 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? N19 C24 N16 115.6(9) . . ? N19 C24 H24A 108.4 . . ? N16 C24 H24A 108.4 . . ? N19 C24 H24B 108.4 . . ? N16 C24 H24B 108.4 . . ? H24A C24 H24B 107.4 . . ? O5 C25 N17 124.4(10) . . ? O5 C25 N18 126.5(10) . . ? N17 C25 N18 109.1(9) . . ? N17 C26 N19 115.6(9) . . ? N17 C26 C27 103.7(8) . . ? N19 C26 C27 102.0(9) . . ? N17 C26 H26 111.6 . . ? N19 C26 H26 111.6 . . ? C27 C26 H26 111.6 . . ? N18 C27 N20 114.8(9) . . ? N18 C27 C26 103.4(9) . . ? N20 C27 C26 103.8(8) . . ? N18 C27 H27 111.4 . . ? N20 C27 H27 111.4 . . ? C26 C27 H27 111.4 . . ? O10 C28 N20 129.4(12) . . ? O10 C28 N19 122.8(11) . . ? N20 C28 N19 107.8(10) . . ? N1 C29 N18 112.7(9) . . ? N1 C29 H29A 109.1 . . ? N18 C29 H29A 109.1 . . ? N1 C29 H29B 109.1 . . ? N18 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? N20 C30 N3 114.3(10) . . ? N20 C30 H30A 108.7 . . ? N3 C30 H30A 108.7 . . ? N20 C30 H30B 108.7 . . ? N3 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? C1 N1 C29 121.4(9) . . ? C1 N1 C2 112.0(9) . . ? C29 N1 C2 124.6(9) . . ? C1 N2 C3 112.2(9) . . ? C1 N2 C5 121.4(10) . . ? C3 N2 C5 126.5(10) . . ? C4 N3 C2 114.2(10) . . ? C4 N3 C30 123.4(10) . . ? C2 N3 C30 121.9(10) . . ? C4 N4 C6 124.2(10) . . ? C4 N4 C3 112.9(10) . . ? C6 N4 C3 122.3(10) . . ? C7 N5 C8 116.6(9) . . ? C7 N5 C5 121.2(10) . . ? C8 N5 C5 122.1(9) . . ? C9 N6 C7 110.9(9) . . ? C9 N6 C11 125.5(10) . . ? C7 N6 C11 122.3(9) . . ? C10 N7 C8 113.2(10) . . ? C10 N7 C6 122.7(10) . . ? C8 N7 C6 122.1(10) . . ? C10 N8 C12 123.4(10) . . ? C10 N8 C9 111.5(9) . . ? C12 N8 C9 124.7(10) . . ? C13 N9 C14 114.3(10) . . ? C13 N9 C11 121.6(10) . . ? C14 N9 C11 124.0(10) . . ? C13 N10 C17 123.9(10) . . ? C13 N10 C15 111.0(9) . . ? C17 N10 C15 123.1(9) . . ? C16 N11 C12 123.7(10) . . ? C16 N11 C14 111.7(9) . . ? C12 N11 C14 123.0(10) . . ? C16 N12 C18 127.5(10) . . ? C16 N12 C15 111.7(10) . . ? C18 N12 C15 120.5(9) . . ? C19 N13 C20 113.8(10) . . ? C19 N13 C17 121.6(10) . . ? C20 N13 C17 124.3(9) . . ? C19 N14 C23 122.1(9) . . ? C19 N14 C21 112.9(9) . . ? C23 N14 C21 124.2(9) . . ? C22 N15 C18 122.8(10) . . ? C22 N15 C20 110.8(8) . . ? C18 N15 C20 126.3(9) . . ? C22 N16 C24 122.5(10) . . ? C22 N16 C21 110.9(9) . . ? C24 N16 C21 124.7(8) . . ? C25 N17 C23 120.3(10) . . ? C25 N17 C26 111.3(9) . . ? C23 N17 C26 125.3(9) . . ? C25 N18 C27 111.9(9) . . ? C25 N18 C29 123.4(9) . . ? C27 N18 C29 124.4(9) . . ? C24 N19 C28 125.6(9) . . ? C24 N19 C26 121.9(9) . . ? C28 N19 C26 111.4(9) . . ? C28 N20 C27 114.1(9) . . ? C28 N20 C30 120.5(10) . . ? C27 N20 C30 121.9(9) . . ? C1 O1 Lu1 156.0(7) . . ? C7 O2 Lu1 147.6(8) . . ? C16 O8 Lu1 146.8(7) . 6_654 ? C22 O9 Lu1 149.3(7) . 6_654 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.458 _refine_diff_density_min -2.157 _refine_diff_density_rms 0.180 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.060 0.176 0.178 147 75 ' ' 2 -0.236 -0.060 0.344 147 75 ' ' 3 0.064 0.601 0.344 44 14 ' ' 4 -0.176 0.764 0.511 147 75 ' ' 5 0.181 0.434 0.515 91 61 ' ' 6 0.059 0.824 0.678 147 75 ' ' 7 0.235 1.059 0.844 147 75 ' ' 8 -0.064 0.399 0.844 44 14 ' ' 9 0.176 0.236 1.011 146 75 ' ' 10 -0.182 0.566 1.014 92 61 ' ' 11 0.252 0.818 0.181 92 61 ' ' 12 0.433 0.252 0.348 90 60 ' ' 13 0.399 0.463 0.678 44 14 ' ' 14 0.463 0.064 0.511 44 14 ' ' 15 0.537 0.936 0.011 44 14 ' ' 16 0.566 0.748 0.848 90 60 ' ' 17 0.601 0.537 0.178 44 14 ' ' 18 0.748 0.181 0.681 91 60 ' ' _platon_squeeze_details ; ;