# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_z4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103.25 H109 Ce2 N16 O25.25' _chemical_formula_weight 2258.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 43.484(18) _cell_length_b 26.316(11) _cell_length_c 22.430(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.713(5) _cell_angle_gamma 90.00 _cell_volume 25666(18) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5275 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 18.93 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9268 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61009 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_unetI/netI 0.2461 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 22380 _reflns_number_gt 7025 _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. Except the solvent mathanol, water, some of the solvent DMF molecules and disordered benzene ring, the other non-hydrogen atoms were refined anisotropically. Hydrogen atoms within the ligand backbones and the solvent DMF molecules were fixed geometrically at calculated distances and allowed to ride on the parent non-hydrogen atoms. To assist the stability of refinements, several restrains were applied: Four carbon atoms in one benzene ring of the salicylalzone groups were disordered into two parts with the s.o.f being fixed at 0.4 and 06, respectively. Several solvent methanol and DMF molecules were disordered with the s.o.f. being fixed at suitable value. Some of the solvent DMF molecules were restrained as idealized geometry. Thermal parameters on adjacent atoms in some of the partly occupied DMF solvent molecules were restrained to be similar. ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22380 _refine_ls_number_parameters 1412 _refine_ls_number_restraints 492 _refine_ls_R_factor_all 0.2143 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2026 _refine_ls_wR_factor_gt 0.1812 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.362372(8) 0.160745(10) 0.328643(13) 0.07784(11) Uani 1 1 d . . . Ce2 Ce 0.662589(8) 0.449124(9) 0.406370(13) 0.07248(11) Uani 1 1 d . . . N101 N 0.36114(10) 0.13836(12) 0.44311(16) 0.0842(15) Uani 1 1 d . . . O101 O 0.34209(8) 0.08623(10) 0.34609(14) 0.0949(13) Uani 1 1 d . . . C101 C 0.34005(11) 0.04638(15) 0.3812(2) 0.0753(18) Uani 1 1 d . . . N102 N 0.37028(10) 0.17745(12) 0.48009(16) 0.0967(17) Uani 1 1 d . . . H10A H 0.3715 0.1733 0.5181 0.116 Uiso 1 1 calc R . . O102 O 0.37624(8) 0.22709(9) 0.39963(14) 0.0874(12) Uani 1 1 d . . . C102 C 0.32977(13) 0.00021(18) 0.3568(2) 0.110(2) Uani 1 1 d . . . H10B H 0.3252 -0.0017 0.3163 0.132 Uiso 1 1 calc R . . N103 N 0.62369(8) 0.42179(12) 0.53255(16) 0.0754(14) Uani 1 1 d . . . H10C H 0.6179 0.4109 0.5668 0.090 Uiso 1 1 calc R . . O103 O 0.42006(8) 0.38744(11) 0.58922(14) 0.0929(13) Uani 1 1 d . . . C103 C 0.32617(15) -0.0436(2) 0.3931(3) 0.143(3) Uani 1 1 d . . . H10D H 0.3194 -0.0744 0.3774 0.172 Uiso 1 1 calc R . . N104 N 0.65389(9) 0.42206(12) 0.51901(16) 0.0689(13) Uani 1 1 d . . . O104 O 0.47941(8) 0.43550(11) 0.56460(14) 0.0955(13) Uani 1 1 d . . . C104 C 0.33326(15) -0.0380(2) 0.4533(3) 0.137(3) Uani 1 1 d . . . H10E H 0.3306 -0.0656 0.4787 0.165 Uiso 1 1 calc R . . O105 O 0.61171(8) 0.45141(10) 0.44110(12) 0.1051(13) Uani 1 1 d . . . C105 C 0.34413(15) 0.00733(16) 0.4768(2) 0.116(2) Uani 1 1 d . . . H10F H 0.3494 0.0094 0.5170 0.139 Uiso 1 1 calc R . . O106 O 0.70547(8) 0.42918(10) 0.45409(13) 0.0880(13) Uani 1 1 d . . . C106 C 0.34711(12) 0.04882(16) 0.4414(2) 0.0784(18) Uani 1 1 d . . . C107 C 0.35739(11) 0.09563(16) 0.4702(2) 0.088(2) Uani 1 1 d . . . H10G H 0.3615 0.0946 0.5110 0.106 Uiso 1 1 calc R . . C108 C 0.37710(12) 0.22185(17) 0.4551(2) 0.084(2) Uani 1 1 d . . . C109 C 0.38601(12) 0.26482(16) 0.4928(2) 0.0809(19) Uani 1 1 d . . . C110 C 0.38161(12) 0.31373(15) 0.4704(2) 0.0845(19) Uani 1 1 d . . . H11A H 0.3708 0.3182 0.4347 0.101 Uiso 1 1 calc R . . C111 C 0.39321(12) 0.35610(16) 0.5006(2) 0.093(2) Uani 1 1 d . . . H11B H 0.3909 0.3885 0.4847 0.111 Uiso 1 1 calc R . . C112 C 0.40797(13) 0.34907(16) 0.5535(2) 0.095(2) Uani 1 1 d . . . C113 C 0.41217(13) 0.30104(17) 0.5783(2) 0.094(2) Uani 1 1 d . . . H11C H 0.4222 0.2970 0.6148 0.113 Uiso 1 1 calc R . . C114 C 0.40089(14) 0.25885(17) 0.5465(2) 0.109(2) Uani 1 1 d . . . H11D H 0.4036 0.2264 0.5622 0.130 Uiso 1 1 calc R . . C115 C 0.42593(12) 0.43651(15) 0.5618(2) 0.092(2) Uani 1 1 d U . . H11E H 0.4281 0.4622 0.5925 0.111 Uiso 1 1 calc R . . H11F H 0.4086 0.4458 0.5363 0.111 Uiso 1 1 calc R . . C116 C 0.45426(12) 0.43478(17) 0.5260(2) 0.0855(19) Uani 1 1 d U . . H11G H 0.4545 0.4041 0.5021 0.103 Uiso 1 1 calc R . . H11J H 0.4550 0.4638 0.4995 0.103 Uiso 1 1 calc R . . C117 C 0.50917(11) 0.43611(16) 0.5452(2) 0.0748(18) Uani 1 1 d . . . C118 C 0.51672(12) 0.43144(15) 0.4842(2) 0.0831(19) Uani 1 1 d . . . H11H H 0.5018 0.4282 0.4543 0.100 Uiso 1 1 calc R . . C119 C 0.54669(11) 0.43200(14) 0.4727(2) 0.0728(18) Uani 1 1 d . . . H11I H 0.5520 0.4289 0.4328 0.087 Uiso 1 1 calc R . . C120 C 0.56982(12) 0.43647(14) 0.5116(2) 0.0729(18) Uani 1 1 d . . . C121 C 0.56030(11) 0.44329(15) 0.5744(2) 0.0733(17) Uani 1 1 d . . . H12A H 0.5749 0.4487 0.6044 0.088 Uiso 1 1 calc R . . C122 C 0.53104(11) 0.44156(17) 0.5867(2) 0.0817(19) Uani 1 1 d . . . H12B H 0.5252 0.4443 0.6264 0.098 Uiso 1 1 calc R . . C123 C 0.60343(11) 0.43781(15) 0.4945(2) 0.0785(17) Uani 1 1 d U . . C124 C 0.67202(11) 0.40230(17) 0.5537(2) 0.093(2) Uani 1 1 d . A . H12C H 0.6635 0.3916 0.5893 0.111 Uiso 1 1 calc R . . C125 C 0.70307(9) 0.39310(15) 0.54897(16) 0.093(2) Uani 1 1 d D . . C126 C 0.71869(11) 0.3599(3) 0.5887(3) 0.113(3) Uiso 0.40 1 d PDU A 1 H12D H 0.7077 0.3465 0.6203 0.136 Uiso 0.40 1 calc PR A 1 C127 C 0.74945(11) 0.3462(2) 0.5834(3) 0.105(3) Uiso 0.40 1 d PDU A 1 H12G H 0.7591 0.3242 0.6102 0.126 Uiso 0.40 1 calc PR A 1 C128 C 0.76490(14) 0.3673(2) 0.5355(2) 0.118(3) Uiso 0.40 1 d PDU A 1 H12K H 0.7859 0.3611 0.5326 0.141 Uiso 0.40 1 calc PR A 1 C129 C 0.75111(11) 0.3971(2) 0.4918(3) 0.106(3) Uiso 0.40 1 d PDU A 1 H29A H 0.7621 0.4106 0.4602 0.128 Uiso 0.40 1 calc PR A 1 C26' C 0.71970(10) 0.3779(3) 0.6002(2) 0.124(3) Uiso 0.60 1 d PDU A 2 H26A H 0.7096 0.3747 0.6364 0.148 Uiso 0.60 1 calc PR A 2 C27' C 0.75089(10) 0.3676(3) 0.5974(2) 0.116(3) Uiso 0.60 1 d PDU A 2 H27A H 0.7615 0.3542 0.6300 0.139 Uiso 0.60 1 calc PR A 2 C28' C 0.76589(13) 0.3778(3) 0.5444(2) 0.122(3) Uiso 0.60 1 d PDU A 2 H28A H 0.7870 0.3725 0.5430 0.146 Uiso 0.60 1 calc PR A 2 C29' C 0.75102(10) 0.3956(3) 0.4937(2) 0.102(3) Uiso 0.60 1 d PDU A 2 H12E H 0.7614 0.4006 0.4583 0.123 Uiso 0.60 1 calc PR A 2 C130 C 0.71959(8) 0.40552(16) 0.49824(19) 0.095(2) Uani 1 1 d D A . N201 N 0.35287(9) 0.24863(12) 0.28021(16) 0.0735(14) Uani 1 1 d . . . O201 O 0.31862(8) 0.18556(12) 0.35270(13) 0.1095(12) Uani 1 1 d . . . C201 C 0.30069(10) 0.23314(17) 0.3645(2) 0.1000(11) Uani 1 1 d DU . . N202 N 0.37350(9) 0.26316(12) 0.23867(16) 0.0742(14) Uani 1 1 d . . . H20A H 0.3707 0.2882 0.2145 0.089 Uiso 1 1 calc R . . O202 O 0.40180(8) 0.19680(11) 0.27468(14) 0.0894(13) Uani 1 1 d . . . C202 C 0.27687(9) 0.23298(13) 0.40518(19) 0.0982(11) Uani 1 1 d DU . . H20B H 0.2729 0.2039 0.4274 0.118 Uiso 1 1 calc R . . N203 N 0.61420(9) 0.49984(11) 0.29850(15) 0.0755(14) Uani 1 1 d . . . H20C H 0.6032 0.5199 0.2769 0.091 Uiso 1 1 calc R . . O203 O 0.49902(9) 0.29389(13) 0.1021(2) 0.1407(19) Uani 1 1 d . . . C203 C 0.25899(11) 0.27638(13) 0.4127(2) 0.1029(11) Uani 1 1 d DU . . H20D H 0.2424 0.2755 0.4385 0.123 Uiso 1 1 calc R . . N204 N 0.63313(10) 0.51822(11) 0.34320(16) 0.0759(15) Uani 1 1 d . . . O204 O 0.54934(8) 0.35715(10) 0.10086(14) 0.0932(13) Uani 1 1 d . . . C204 C 0.26545(10) 0.32070(14) 0.38246(18) 0.1018(11) Uani 1 1 d DU . . H20E H 0.2534 0.3495 0.3876 0.122 Uiso 1 1 calc R . . O205 O 0.63025(8) 0.42230(9) 0.32470(13) 0.0761(12) Uani 1 1 d . . . C205 C 0.29007(9) 0.32151(14) 0.3446(2) 0.0989(11) Uani 1 1 d DU . . H20F H 0.2951 0.3517 0.3254 0.119 Uiso 1 1 calc R . . O206 O 0.66552(9) 0.52395(10) 0.44768(13) 0.0926(13) Uani 1 1 d . . . C206 C 0.30759(11) 0.27865(15) 0.3342(2) 0.0935(11) Uani 1 1 d DU . . C207 C 0.33167(11) 0.28201(15) 0.2932(2) 0.0830(19) Uani 1 1 d . . . H20G H 0.3327 0.3124 0.2723 0.100 Uiso 1 1 calc R . . C208 C 0.39675(11) 0.23636(15) 0.2395(2) 0.0663(17) Uani 1 1 d . . . C209 C 0.42263(11) 0.24783(15) 0.2030(2) 0.0779(18) Uani 1 1 d . . . C210 C 0.45135(13) 0.22490(16) 0.2056(2) 0.101(2) Uani 1 1 d . . . H21A H 0.4528 0.1969 0.2308 0.121 Uiso 1 1 calc R . . C211 C 0.47853(14) 0.23735(18) 0.1760(3) 0.119(3) Uani 1 1 d . . . H21B H 0.4972 0.2212 0.1835 0.143 Uiso 1 1 calc R . . C212 C 0.47489(13) 0.27688(19) 0.1338(3) 0.099(2) Uani 1 1 d U . . C213 C 0.44692(12) 0.29987(19) 0.1282(2) 0.093(2) Uani 1 1 d . . . H21C H 0.4453 0.3258 0.1002 0.112 Uiso 1 1 calc R . . C214 C 0.42155(11) 0.28888(17) 0.1589(2) 0.0792(19) Uani 1 1 d . . . H21D H 0.4035 0.3071 0.1524 0.095 Uiso 1 1 calc R . . C215 C 0.52943(15) 0.27813(19) 0.1243(3) 0.129(2) Uani 1 1 d U . . H21E H 0.5322 0.2878 0.1657 0.154 Uiso 1 1 calc R . . H21F H 0.5319 0.2416 0.1208 0.154 Uiso 1 1 calc R . . C216 C 0.54955(16) 0.30240(19) 0.0898(2) 0.137(3) Uani 1 1 d U . . H21I H 0.5445 0.2961 0.0482 0.164 Uiso 1 1 calc R . . H21J H 0.5700 0.2892 0.0976 0.164 Uiso 1 1 calc R . . C217 C 0.56613(13) 0.37917(18) 0.14847(19) 0.085(2) Uani 1 1 d . . . C218 C 0.58513(12) 0.34984(16) 0.18471(19) 0.094(2) Uani 1 1 d . . . H21G H 0.5875 0.3151 0.1788 0.113 Uiso 1 1 calc R . . C219 C 0.60079(12) 0.37626(15) 0.2318(2) 0.084(2) Uani 1 1 d . . . H21H H 0.6144 0.3589 0.2569 0.101 Uiso 1 1 calc R . . C220 C 0.59589(12) 0.42650(13) 0.23979(18) 0.0638(16) Uani 1 1 d . . . C221 C 0.57679(12) 0.45276(16) 0.20243(19) 0.0788(18) Uani 1 1 d . . . H22A H 0.5739 0.4874 0.2085 0.095 Uiso 1 1 calc R . . C222 C 0.56213(12) 0.42988(15) 0.1574(2) 0.0810(19) Uani 1 1 d . . . H22B H 0.5492 0.4484 0.1322 0.097 Uiso 1 1 calc R . . C223 C 0.61368(11) 0.44909(16) 0.2900(2) 0.0671(17) Uani 1 1 d . . . C224 C 0.63795(12) 0.56626(16) 0.3415(2) 0.0798(19) Uani 1 1 d . . . H22C H 0.6287 0.5842 0.3104 0.096 Uiso 1 1 calc R . . C225 C 0.65602(13) 0.59439(16) 0.3827(2) 0.0813(19) Uani 1 1 d . . . C226 C 0.66074(14) 0.64627(16) 0.3707(3) 0.103(2) Uani 1 1 d . . . H22D H 0.6528 0.6605 0.3359 0.123 Uiso 1 1 calc R . . C227 C 0.67685(16) 0.67575(18) 0.4099(3) 0.136(3) Uani 1 1 d . . . H22E H 0.6788 0.7104 0.4025 0.163 Uiso 1 1 calc R . . C228 C 0.69068(15) 0.65503(18) 0.4614(3) 0.123(3) Uani 1 1 d . . . H22F H 0.7024 0.6756 0.4866 0.148 Uiso 1 1 calc R . . C229 C 0.68695(13) 0.60522(16) 0.4743(2) 0.102(2) Uani 1 1 d . . . H22G H 0.6956 0.5912 0.5087 0.122 Uiso 1 1 calc R . . C230 C 0.66923(13) 0.57438(16) 0.4334(2) 0.088(2) Uani 1 1 d . . . N301 N 0.39751(10) 0.09086(13) 0.28184(17) 0.0887(16) Uani 1 1 d . . . O301 O 0.34466(8) 0.13749(10) 0.23938(13) 0.0912(13) Uani 1 1 d . . . C301 C 0.34226(12) 0.09385(18) 0.2075(2) 0.0792(19) Uani 1 1 d . . . N302 N 0.42768(10) 0.08905(13) 0.30222(18) 0.0985(18) Uani 1 1 d . . . H30A H 0.4415 0.0715 0.2844 0.118 Uiso 1 1 calc R . . O302 O 0.41320(8) 0.14071(11) 0.37634(14) 0.0894(13) Uani 1 1 d . . . C302 C 0.31685(13) 0.08894(18) 0.1708(2) 0.098(2) Uani 1 1 d . . . H30B H 0.3026 0.1151 0.1669 0.117 Uiso 1 1 calc R . . N303 N 0.68060(9) 0.32637(11) 0.36363(16) 0.0788(15) Uani 1 1 d . . . H30C H 0.6893 0.2994 0.3502 0.095 Uiso 1 1 calc R . . O303 O 0.55448(8) 0.11248(13) 0.44360(17) 0.1065(15) Uani 1 1 d . . . C303 C 0.31295(14) 0.04191(19) 0.1384(2) 0.106(2) Uani 1 1 d . . . H30D H 0.2954 0.0379 0.1146 0.127 Uiso 1 1 calc R . . N304 N 0.68995(8) 0.37427(11) 0.34589(16) 0.0604(13) Uani 1 1 d . . . O304 O 0.61287(8) 0.13751(10) 0.48685(14) 0.0909(13) Uani 1 1 d . . . C304 C 0.33308(14) 0.0042(2) 0.1408(3) 0.119(3) Uani 1 1 d . . . H30E H 0.3296 -0.0259 0.1200 0.143 Uiso 1 1 calc R . . O305 O 0.64603(7) 0.36214(9) 0.42346(13) 0.0726(11) Uani 1 1 d . . . C305 C 0.35888(15) 0.0108(2) 0.1744(3) 0.126(3) Uani 1 1 d . . . H30F H 0.3738 -0.0145 0.1747 0.151 Uiso 1 1 calc R . . O306 O 0.69413(8) 0.47752(10) 0.33722(14) 0.0849(13) Uani 1 1 d . . . C306 C 0.36375(12) 0.05547(17) 0.2092(2) 0.0820(19) Uani 1 1 d . . . C307 C 0.39171(14) 0.05596(18) 0.2412(2) 0.105(2) Uani 1 1 d . . . H30G H 0.4064 0.0312 0.2336 0.127 Uiso 1 1 calc R . . C308 C 0.43419(12) 0.11684(16) 0.3525(2) 0.0791(19) Uani 1 1 d . . . C309 C 0.46557(11) 0.11636(16) 0.3722(2) 0.0753(18) Uani 1 1 d . . . C310 C 0.47344(14) 0.13029(17) 0.4327(2) 0.105(2) Uani 1 1 d . . . H31A H 0.4583 0.1405 0.4591 0.126 Uiso 1 1 calc R . . C311 C 0.50475(13) 0.12804(17) 0.4511(3) 0.112(2) Uani 1 1 d . . . H31C H 0.5095 0.1379 0.4900 0.134 Uiso 1 1 calc R . . C312 C 0.52771(13) 0.11306(18) 0.4176(3) 0.101(2) Uani 1 1 d . . . C313 C 0.52112(13) 0.10150(17) 0.3563(2) 0.093(2) Uani 1 1 d . . . H31D H 0.5364 0.0934 0.3293 0.111 Uiso 1 1 calc R . . C314 C 0.49016(11) 0.10333(18) 0.3399(2) 0.091(2) Uani 1 1 d . . . H31E H 0.4858 0.0941 0.3007 0.110 Uiso 1 1 calc R . . C315 C 0.58021(11) 0.10184(18) 0.4090(2) 0.100(2) Uani 1 1 d U . . H31B H 0.5839 0.1296 0.3816 0.120 Uiso 1 1 calc R . . H31F H 0.5767 0.0712 0.3859 0.120 Uiso 1 1 calc R . . C316 C 0.60698(12) 0.09490(16) 0.4486(2) 0.105(2) Uani 1 1 d U . . H31G H 0.6038 0.0650 0.4729 0.126 Uiso 1 1 calc R . . H31H H 0.6250 0.0888 0.4244 0.126 Uiso 1 1 calc R . . C317 C 0.62496(11) 0.18055(15) 0.4606(2) 0.0777(19) Uani 1 1 d . . . C318 C 0.61955(13) 0.22565(17) 0.4961(2) 0.099(2) Uani 1 1 d . . . H31I H 0.6088 0.2244 0.5317 0.118 Uiso 1 1 calc R . . C319 C 0.63082(14) 0.26911(16) 0.4749(2) 0.096(2) Uani 1 1 d . . . H31J H 0.6271 0.2988 0.4960 0.115 Uiso 1 1 calc R . . C320 C 0.64726(12) 0.27229(13) 0.42471(19) 0.0660(17) Uani 1 1 d . . . C321 C 0.65212(12) 0.22863(16) 0.3887(2) 0.0817(19) Uani 1 1 d . . . H32A H 0.6626 0.2312 0.3530 0.098 Uiso 1 1 calc R . . C322 C 0.64097(12) 0.18216(15) 0.4078(2) 0.0791(19) Uani 1 1 d . . . H32B H 0.6442 0.1528 0.3857 0.095 Uiso 1 1 calc R . . C323 C 0.65769(11) 0.32368(17) 0.4023(2) 0.0674(17) Uani 1 1 d . . . C324 C 0.71383(11) 0.37773(16) 0.3139(2) 0.0699(18) Uani 1 1 d . . . H32C H 0.7234 0.3473 0.3040 0.084 Uiso 1 1 calc R . . C325 C 0.72709(13) 0.42139(16) 0.2922(2) 0.083(2) Uani 1 1 d . . . C326 C 0.75219(14) 0.41728(18) 0.2581(2) 0.108(2) Uani 1 1 d . . . H32D H 0.7590 0.3844 0.2504 0.129 Uiso 1 1 calc R . . C327 C 0.76933(15) 0.4565(2) 0.2327(3) 0.128(3) Uani 1 1 d . . . H32E H 0.7862 0.4507 0.2086 0.153 Uiso 1 1 calc R . . C328 C 0.75858(14) 0.5069(2) 0.2473(3) 0.129(3) Uani 1 1 d . . . H32F H 0.7689 0.5355 0.2336 0.155 Uiso 1 1 calc R . . C329 C 0.73391(14) 0.51172(17) 0.2803(2) 0.105(2) Uani 1 1 d . . . H32G H 0.7266 0.5443 0.2881 0.126 Uiso 1 1 calc R . . C330 C 0.71794(13) 0.46978(19) 0.3047(2) 0.081(2) Uani 1 1 d . . . O11 O 0.28083(8) 0.25365(11) 0.19107(15) 0.0940(14) Uani 1 1 d . . . N11 N 0.25403(11) 0.20083(14) 0.24669(17) 0.0928(17) Uani 1 1 d . . . C11 C 0.27982(12) 0.21443(15) 0.2214(2) 0.086(2) Uani 1 1 d . . . H11K H 0.2974 0.1946 0.2263 0.103 Uiso 1 1 calc R . . C12 C 0.22608(14) 0.2284(2) 0.2442(3) 0.153(3) Uani 1 1 d . . . H12H H 0.2288 0.2584 0.2205 0.229 Uiso 1 1 calc R . . H12I H 0.2202 0.2379 0.2838 0.229 Uiso 1 1 calc R . . H12J H 0.2103 0.2076 0.2266 0.229 Uiso 1 1 calc R . . C13 C 0.25344(16) 0.15164(18) 0.2821(2) 0.137(3) Uani 1 1 d . . . H13A H 0.2733 0.1357 0.2807 0.206 Uiso 1 1 calc R . . H13B H 0.2382 0.1292 0.2652 0.206 Uiso 1 1 calc R . . H13C H 0.2484 0.1589 0.3228 0.206 Uiso 1 1 calc R . . O21 O 0.70539(8) 0.10525(17) 0.94461(9) 0.122(2) Uiso 0.50 1 d PDU B 1 N21 N 0.73244(7) 0.06639(10) 1.01408(9) 0.0995(19) Uiso 0.50 1 d PDU B 1 C21 C 0.71535(7) 0.10803(9) 0.99513(9) 0.121(2) Uiso 0.50 1 d PDU B 1 H21K H 0.7118 0.1360 1.0194 0.145 Uiso 0.50 1 calc PR B 1 C22 C 0.73918(13) 0.05738(17) 1.07543(8) 0.134(3) Uiso 0.50 1 d PDU B 1 H22H H 0.7366 0.0883 1.0975 0.201 Uiso 0.50 1 calc PR B 1 H22I H 0.7600 0.0458 1.0797 0.201 Uiso 0.50 1 calc PR B 1 H22J H 0.7255 0.0320 1.0904 0.201 Uiso 0.50 1 calc PR B 1 C23 C 0.74297(11) 0.03006(11) 0.97128(11) 0.111(3) Uiso 0.50 1 d PDU B 1 H23A H 0.7377 0.0415 0.9318 0.167 Uiso 0.50 1 calc PR B 1 H23B H 0.7334 -0.0022 0.9785 0.167 Uiso 0.50 1 calc PR B 1 H23C H 0.7649 0.0266 0.9748 0.167 Uiso 0.50 1 calc PR B 1 C423 C 0.71552(8) 0.08999(12) 0.97505(8) 0.122(2) Uiso 0.25 1 d PDU C 2 H42A H 0.7023 0.1178 0.9768 0.146 Uiso 0.25 1 calc PR C 2 C422 C 0.72689(13) 0.09561(12) 1.08209(9) 0.125(4) Uiso 0.25 1 d PDU C 2 H42D H 0.7356 0.0744 1.1128 0.188 Uiso 0.25 1 calc PR C 2 H42E H 0.7055 0.1015 1.0900 0.188 Uiso 0.25 1 calc PR C 2 H42F H 0.7376 0.1275 1.0813 0.188 Uiso 0.25 1 calc PR C 2 C421 C 0.74723(8) 0.02481(9) 1.02373(19) 0.124(3) Uiso 0.25 1 d PDU C 2 H42B H 0.7477 0.0124 0.9835 0.186 Uiso 0.25 1 calc PR C 2 H42C H 0.7378 -0.0002 1.0488 0.186 Uiso 0.25 1 calc PR C 2 H42G H 0.7678 0.0313 1.0376 0.186 Uiso 0.25 1 calc PR C 2 N421 N 0.72977(9) 0.07086(12) 1.02562(8) 0.103(2) Uiso 0.25 1 d PDU C 2 O421 O 0.7209(2) 0.0692(2) 0.92877(10) 0.093(3) Uiso 0.25 1 d PDU C 2 O31 O 0.63358(6) 0.45884(12) 0.6756(2) 0.122(2) Uiso 0.50 1 d PDU D 1 N31 N 0.66398(10) 0.51842(11) 0.64056(17) 0.1007(19) Uiso 0.50 1 d PDU D 1 C32 C 0.6439(2) 0.5380(4) 0.5923(4) 0.095(3) Uiso 0.50 1 d PU D 1 H32H H 0.6228 0.5331 0.6028 0.143 Uiso 0.50 1 calc PR D 1 H32I H 0.6481 0.5200 0.5560 0.143 Uiso 0.50 1 calc PR D 1 H32J H 0.6478 0.5736 0.5866 0.143 Uiso 0.50 1 calc PR D 1 C31 C 0.6999(2) 0.5175(4) 0.6336(5) 0.124(3) Uiso 0.50 1 d PU D 1 H31K H 0.7090 0.5000 0.6670 0.187 Uiso 0.50 1 calc PR D 1 H31L H 0.7075 0.5517 0.6323 0.187 Uiso 0.50 1 calc PR D 1 H31M H 0.7050 0.5001 0.5974 0.187 Uiso 0.50 1 calc PR D 1 C33 C 0.65740(7) 0.48093(14) 0.6809(2) 0.097(2) Uiso 0.50 1 d PDU D 1 H33A H 0.6711 0.4729 0.7115 0.117 Uiso 0.50 1 calc PR D 1 N431 N 0.67257(5) 0.51020(9) 0.63432(13) 0.104(2) Uiso 0.25 1 d PDU E 2 O431 O 0.65595(7) 0.44851(13) 0.6919(2) 0.113(3) Uiso 0.25 1 d PDU E 2 C432 C 0.64253(4) 0.53095(15) 0.6245(2) 0.115(3) Uiso 0.25 1 d PDU E 2 H43A H 0.6275 0.5091 0.6422 0.173 Uiso 0.25 1 calc PR E 2 H43B H 0.6385 0.5336 0.5825 0.173 Uiso 0.25 1 calc PR E 2 H43C H 0.6414 0.5641 0.6424 0.173 Uiso 0.25 1 calc PR E 2 C431 C 0.69696(5) 0.52937(15) 0.59816(16) 0.126(4) Uiso 0.25 1 d PDU E 2 H43D H 0.7164 0.5181 0.6141 0.190 Uiso 0.25 1 calc PR E 2 H43E H 0.6964 0.5658 0.5980 0.190 Uiso 0.25 1 calc PR E 2 H43F H 0.6944 0.5170 0.5581 0.190 Uiso 0.25 1 calc PR E 2 C433 C 0.67779(7) 0.47204(10) 0.67523(13) 0.108(2) Uiso 0.25 1 d PDU E 2 H43G H 0.6975 0.4648 0.6893 0.129 Uiso 0.25 1 calc PR E 2 N51 N 0.52737(4) 0.27477(8) 0.5644(4) 0.069(2) Uiso 0.13 1 d PDU F 1 C53 C 0.55403(4) 0.30282(10) 0.5586(2) 0.074(2) Uiso 0.13 1 d PDU F 1 H53A H 0.5556 0.3289 0.5308 0.089 Uiso 0.13 1 calc PR F 1 C51 C 0.52780(9) 0.22053(7) 0.5608(8) 0.078(4) Uiso 0.13 1 d PDU F 1 H51A H 0.5486 0.2090 0.5573 0.118 Uiso 0.13 1 calc PR F 1 H51B H 0.5161 0.2098 0.5265 0.118 Uiso 0.13 1 calc PR F 1 H51C H 0.5190 0.2064 0.5962 0.118 Uiso 0.13 1 calc PR F 1 C52 C 0.49815(5) 0.29916(12) 0.5703(7) 0.082(4) Uiso 0.13 1 d PDU F 1 H52A H 0.4992 0.3236 0.6021 0.123 Uiso 0.13 1 calc PR F 1 H52B H 0.4828 0.2742 0.5791 0.123 Uiso 0.13 1 calc PR F 1 H52C H 0.4928 0.3161 0.5337 0.123 Uiso 0.13 1 calc PR F 1 O51 O 0.57512(6) 0.2919(3) 0.5911(2) 0.093(4) Uiso 0.13 1 d PDU F 1 N51' N 0.53041(5) 0.25519(8) 0.57297(14) 0.072(2) Uiso 0.13 1 d PDU G 2 O51' O 0.53200(12) 0.32389(10) 0.5173(2) 0.089(4) Uiso 0.13 1 d PDU G 2 C51' C 0.54598(7) 0.22066(11) 0.61249(15) 0.083(4) Uiso 0.13 1 d PDU G 2 H51D H 0.5673 0.2296 0.6153 0.125 Uiso 0.13 1 calc PR G 2 H51E H 0.5440 0.1867 0.5974 0.125 Uiso 0.13 1 calc PR G 2 H51F H 0.5370 0.2226 0.6513 0.125 Uiso 0.13 1 calc PR G 2 C52' C 0.49754(4) 0.2538(2) 0.5714(3) 0.075(4) Uiso 0.13 1 d PDU G 2 H52D H 0.4900 0.2771 0.5417 0.113 Uiso 0.13 1 calc PR G 2 H52E H 0.4898 0.2634 0.6097 0.113 Uiso 0.13 1 calc PR G 2 H52F H 0.4908 0.2200 0.5619 0.113 Uiso 0.13 1 calc PR G 2 C53' C 0.54660(6) 0.29032(9) 0.54014(16) 0.074(2) Uiso 0.13 1 d PDU G 2 H53B H 0.5678 0.2881 0.5360 0.089 Uiso 0.13 1 calc PR G 2 O71 O 0.58081(5) 0.42075(14) 0.73512(15) 0.0280(15) Uiso 0.37 1 d PDU . . N71 N 0.54313(5) 0.37447(8) 0.77091(14) 0.092(3) Uiso 0.37 1 d PDU . . C72 C 0.51959(5) 0.36807(14) 0.81438(13) 0.131(4) Uiso 0.37 1 d PDU . . H72A H 0.5142 0.4006 0.8306 0.197 Uiso 0.37 1 calc PR . . H72B H 0.5270 0.3463 0.8458 0.197 Uiso 0.37 1 calc PR . . H72C H 0.5018 0.3530 0.7959 0.197 Uiso 0.37 1 calc PR . . C73 C 0.55852(6) 0.42016(7) 0.76559(18) 0.065(3) Uiso 0.37 1 d PDU . . H73A H 0.5518 0.4493 0.7850 0.079 Uiso 0.37 1 calc PR . . C71 C 0.55484(9) 0.32935(8) 0.74334(19) 0.143(4) Uiso 0.37 1 d PDU . . H71A H 0.5702 0.3385 0.7148 0.214 Uiso 0.37 1 calc PR . . H71B H 0.5383 0.3117 0.7235 0.214 Uiso 0.37 1 calc PR . . H71C H 0.5638 0.3077 0.7733 0.214 Uiso 0.37 1 calc PR . . N81 N 0.65823(5) 0.14852(16) 0.83085(9) 0.129(2) Uiso 0.25 1 d PDU H 1 O81 O 0.62134(3) 0.14876(15) 0.89711(15) 0.075(3) Uiso 0.25 1 d PDU H 1 C82 C 0.63936(6) 0.12207(14) 0.78837(12) 0.140(3) Uiso 0.25 1 d PDU H 1 H82A H 0.6230 0.1051 0.8086 0.209 Uiso 0.25 1 calc PR H 1 H82B H 0.6516 0.0975 0.7677 0.209 Uiso 0.25 1 calc PR H 1 H82C H 0.6309 0.1459 0.7602 0.209 Uiso 0.25 1 calc PR H 1 C83 C 0.64697(3) 0.16231(14) 0.88592(9) 0.136(2) Uiso 0.25 1 d PDU H 1 H83A H 0.6587 0.1811 0.9129 0.163 Uiso 0.25 1 calc PR H 1 C81 C 0.68743(5) 0.1669(2) 0.81134(16) 0.146(3) Uiso 0.25 1 d PDU H 1 H81A H 0.6972 0.1857 0.8430 0.219 Uiso 0.25 1 calc PR H 1 H81B H 0.6845 0.1886 0.7773 0.219 Uiso 0.25 1 calc PR H 1 H81C H 0.7002 0.1387 0.8006 0.219 Uiso 0.25 1 calc PR H 1 O81' O 0.65660(12) 0.1666(3) 0.90586(10) 0.126(3) Uiso 0.25 1 d PDU I 2 C83' C 0.64288(10) 0.15016(12) 0.86302(8) 0.136(2) Uiso 0.25 1 d PDU I 2 H83B H 0.6269 0.1270 0.8666 0.163 Uiso 0.25 1 calc PR I 2 C82' C 0.6484(2) 0.22026(7) 0.79222(18) 0.139(4) Uiso 0.25 1 d PDU I 2 H82D H 0.6413 0.2389 0.8261 0.208 Uiso 0.25 1 calc PR I 2 H82E H 0.6335 0.2228 0.7604 0.208 Uiso 0.25 1 calc PR I 2 H82F H 0.6676 0.2341 0.7794 0.208 Uiso 0.25 1 calc PR I 2 C81' C 0.66196(13) 0.13359(10) 0.76253(12) 0.145(4) Uiso 0.25 1 d PDU I 2 H81D H 0.6611 0.0994 0.7772 0.218 Uiso 0.25 1 calc PR I 2 H81E H 0.6827 0.1414 0.7513 0.218 Uiso 0.25 1 calc PR I 2 H81F H 0.6485 0.1370 0.7284 0.218 Uiso 0.25 1 calc PR I 2 N81' N 0.65244(14) 0.16793(9) 0.80819(9) 0.136(2) Uiso 0.25 1 d PDU I 2 N61 N 0.72045(4) 0.21136(11) 0.57241(13) 0.131(3) Uiso 0.19 1 d PDU J 1 O61 O 0.68266(5) 0.1825(3) 0.6272(2) 0.143(3) Uiso 0.19 1 d PDU J 1 C61 C 0.75281(4) 0.21843(16) 0.5643(2) 0.140(4) Uiso 0.19 1 d PDU J 1 H61A H 0.7640 0.2000 0.5944 0.210 Uiso 0.19 1 calc PR J 1 H61B H 0.7577 0.2539 0.5673 0.210 Uiso 0.19 1 calc PR J 1 H61C H 0.7584 0.2061 0.5256 0.210 Uiso 0.19 1 calc PR J 1 C62 C 0.70002(6) 0.24416(12) 0.53992(16) 0.138(4) Uiso 0.19 1 d PDU J 1 H62A H 0.6792 0.2379 0.5520 0.208 Uiso 0.19 1 calc PR J 1 H62B H 0.7018 0.2376 0.4980 0.208 Uiso 0.19 1 calc PR J 1 H62C H 0.7053 0.2789 0.5480 0.208 Uiso 0.19 1 calc PR J 1 C63 C 0.70974(5) 0.18082(12) 0.61787(14) 0.133(2) Uiso 0.19 1 d PDU J 1 H63A H 0.7229 0.1601 0.6401 0.160 Uiso 0.19 1 calc PR J 1 O61' O 0.64798(7) 0.25953(11) 0.6466(3) 0.147(4) Uiso 0.19 1 d PDU K 2 N61' N 0.68662(5) 0.21715(9) 0.60824(14) 0.127(2) Uiso 0.19 1 d PDU K 2 C62' C 0.69448(9) 0.25803(9) 0.56922(14) 0.140(3) Uiso 0.19 1 d PDU K 2 H62D H 0.6777 0.2817 0.5669 0.210 Uiso 0.19 1 calc PR K 2 H62E H 0.6985 0.2448 0.5302 0.210 Uiso 0.19 1 calc PR K 2 H62F H 0.7125 0.2750 0.5843 0.210 Uiso 0.19 1 calc PR K 2 C61' C 0.70970(6) 0.17943(10) 0.6200(3) 0.135(4) Uiso 0.19 1 d PDU K 2 H61D H 0.7035 0.1588 0.6531 0.202 Uiso 0.19 1 calc PR K 2 H61E H 0.7289 0.1958 0.6295 0.202 Uiso 0.19 1 calc PR K 2 H61F H 0.7121 0.1584 0.5854 0.202 Uiso 0.19 1 calc PR K 2 C63' C 0.66008(5) 0.21882(11) 0.64152(16) 0.134(3) Uiso 0.19 1 d PDU K 2 H63B H 0.6520 0.1898 0.6591 0.161 Uiso 0.19 1 calc PR K 2 C5 C 0.5614(4) -0.0211(11) 0.4909(6) 0.117(5) Uiso 0.20 1 d PDU L 1 O5 O 0.5390(3) -0.0231(7) 0.4379(6) 0.125(5) Uiso 0.20 1 d PDU L 1 O5' O 0.5777(3) -0.0370(6) 0.4500(8) 0.130(5) Uiso 0.20 1 d PDU M 2 C5' C 0.5531(5) -0.0649(9) 0.4128(11) 0.118(5) Uiso 0.20 1 d PDU M 2 O1W O 0.61013(15) 0.3585(2) 0.6338(3) 0.152(2) Uiso 0.70 1 d PU . . O2W O 0.6587(4) 0.3490(5) 0.7184(7) 0.118(5) Uiso 0.25 1 d PU . . O3W O 0.53451(11) -0.01071(16) 0.7505(2) 0.1345(15) Uiso 0.90 1 d PU . . O4W O 0.5634(6) 0.0459(9) 0.7582(11) 0.113(4) Uiso 0.15 1 d PU . . C91 C 0.5879(4) 0.0269(2) 0.6106(9) 0.124(8) Uiso 0.20 1 d PDU . . O91 O 0.5801(4) 0.0803(3) 0.6282(8) 0.147(7) Uiso 0.20 1 d PDU . . C6 C 0.5000 0.50856(19) 0.7500 0.148(4) Uiso 0.70 2 d SPDU N 1 O6 O 0.5000 0.56642(18) 0.7500 0.127(3) Uiso 0.70 2 d SPDU N 1 O6' O 0.5155(4) 0.5913(5) 0.7967(7) 0.151(4) Uiso 0.30 1 d PU O 2 C6' C 0.5175(2) 0.5291(7) 0.8153(3) 0.126(5) Uiso 0.30 1 d PU O 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.1207(3) 0.04612(14) 0.06643(19) 0.00117(15) -0.00823(19) -0.00091(18) Ce2 0.1146(3) 0.04324(13) 0.05955(17) -0.00073(14) -0.00190(18) 0.00177(18) N101 0.139(4) 0.0450(19) 0.068(3) -0.0045(19) -0.015(3) -0.016(2) O101 0.154(3) 0.0498(16) 0.081(2) -0.0041(17) -0.009(2) -0.034(2) C101 0.098(4) 0.044(2) 0.084(3) 0.003(3) -0.004(3) -0.009(3) N102 0.186(5) 0.047(2) 0.057(3) 0.010(2) -0.006(3) -0.016(3) O102 0.135(3) 0.0380(15) 0.088(2) -0.0014(16) -0.025(2) -0.0104(19) C102 0.154(5) 0.079(3) 0.098(4) 0.000(3) -0.026(4) -0.022(4) N103 0.095(3) 0.073(2) 0.057(2) 0.000(2) -0.004(2) 0.012(2) O103 0.139(3) 0.0641(18) 0.075(2) -0.0162(18) 0.006(2) -0.016(2) C103 0.221(7) 0.081(4) 0.127(5) 0.017(4) -0.054(5) -0.040(4) N104 0.067(3) 0.064(2) 0.075(3) -0.021(2) -0.018(2) 0.016(2) O104 0.122(3) 0.083(2) 0.081(2) -0.0154(19) -0.018(2) -0.023(2) C104 0.185(7) 0.085(4) 0.141(5) 0.046(4) -0.002(5) -0.013(4) O105 0.199(3) 0.0500(16) 0.0642(19) 0.0232(15) -0.061(2) 0.001(2) C105 0.202(6) 0.043(3) 0.102(4) -0.003(3) -0.018(4) -0.022(4) O106 0.142(3) 0.0524(16) 0.070(2) -0.0128(16) -0.009(2) -0.001(2) C106 0.103(4) 0.066(3) 0.066(3) -0.001(3) -0.004(3) -0.005(3) C107 0.133(5) 0.063(3) 0.069(3) -0.016(3) -0.020(3) -0.005(3) C108 0.116(5) 0.067(3) 0.068(3) -0.007(3) -0.016(3) -0.004(3) C109 0.125(4) 0.057(3) 0.060(3) -0.002(2) -0.022(3) -0.011(3) C110 0.120(5) 0.054(3) 0.079(3) 0.002(3) -0.018(3) -0.001(3) C111 0.147(5) 0.051(3) 0.080(4) -0.004(3) -0.010(4) -0.006(3) C112 0.135(5) 0.050(3) 0.098(4) -0.022(3) -0.006(4) -0.018(3) C113 0.143(5) 0.070(3) 0.069(3) -0.007(3) -0.015(4) -0.008(3) C114 0.202(6) 0.057(3) 0.067(4) 0.002(3) -0.007(4) -0.028(4) C115 0.099(4) 0.059(3) 0.118(4) -0.012(3) 0.017(4) -0.012(3) C116 0.112(4) 0.067(3) 0.078(3) -0.017(3) 0.005(3) -0.007(3) C117 0.061(4) 0.056(3) 0.107(4) -0.015(3) -0.005(3) -0.008(3) C118 0.121(4) 0.059(3) 0.068(3) -0.017(3) -0.028(3) 0.006(3) C119 0.101(4) 0.049(2) 0.068(3) -0.004(2) -0.017(3) 0.008(3) C120 0.115(4) 0.044(2) 0.060(3) 0.000(2) -0.007(3) 0.004(3) C121 0.086(4) 0.065(3) 0.068(3) -0.012(3) -0.006(3) -0.018(3) C122 0.074(4) 0.092(3) 0.079(4) -0.012(3) 0.012(3) -0.016(3) C123 0.065(3) 0.057(3) 0.113(4) -0.024(3) -0.042(3) 0.020(3) C124 0.090(4) 0.110(4) 0.077(4) -0.010(3) -0.027(3) 0.023(3) C125 0.143(5) 0.077(3) 0.057(3) 0.024(3) -0.042(3) 0.003(3) C130 0.156(5) 0.058(3) 0.070(3) 0.006(3) -0.035(4) -0.017(3) N201 0.103(3) 0.052(2) 0.066(3) -0.0029(19) -0.007(2) -0.012(2) O201 0.108(3) 0.134(2) 0.085(2) 0.0741(18) -0.0523(19) -0.067(2) C201 0.132(2) 0.0823(19) 0.085(2) 0.0021(19) 0.000(2) 0.015(2) N202 0.100(3) 0.047(2) 0.075(3) 0.005(2) -0.006(3) 0.006(2) O202 0.128(3) 0.0628(18) 0.077(2) -0.0060(18) 0.001(2) -0.008(2) C202 0.133(2) 0.0750(19) 0.087(2) -0.0005(19) 0.012(2) 0.0158(19) N203 0.137(4) 0.0298(17) 0.059(2) 0.0020(17) -0.018(2) 0.009(2) O203 0.106(3) 0.089(2) 0.228(5) 0.021(3) 0.020(3) -0.024(3) C203 0.137(2) 0.0867(19) 0.085(2) -0.0035(19) 0.010(2) 0.016(2) N204 0.134(4) 0.0290(17) 0.065(3) 0.0033(18) -0.002(3) -0.001(2) O204 0.131(3) 0.0649(19) 0.084(2) 0.0020(18) -0.011(2) 0.005(2) C204 0.137(2) 0.0789(19) 0.090(2) -0.0034(19) 0.008(2) 0.014(2) O205 0.121(3) 0.0372(15) 0.069(2) 0.0035(15) -0.015(2) 0.0069(17) C205 0.132(2) 0.0765(19) 0.089(2) -0.0009(19) 0.011(2) 0.013(2) O206 0.157(3) 0.0556(17) 0.064(2) -0.0091(17) -0.010(2) 0.001(2) C206 0.128(2) 0.0714(19) 0.082(2) -0.0064(18) 0.005(2) 0.0092(19) C207 0.127(5) 0.045(3) 0.076(3) 0.003(3) -0.023(3) 0.003(3) C208 0.070(4) 0.051(2) 0.077(3) -0.007(3) -0.001(3) -0.025(3) C209 0.089(4) 0.056(3) 0.087(3) -0.018(3) -0.040(3) -0.010(3) C210 0.139(5) 0.042(3) 0.122(5) -0.006(3) -0.019(4) -0.003(3) C211 0.104(5) 0.067(3) 0.187(6) -0.010(4) 0.049(5) -0.008(4) C212 0.091(4) 0.084(3) 0.123(4) -0.021(3) 0.021(4) -0.028(3) C213 0.087(4) 0.094(4) 0.099(4) -0.002(3) -0.021(4) -0.020(3) C214 0.078(4) 0.069(3) 0.090(4) -0.013(3) 0.006(3) -0.010(3) C215 0.173(5) 0.074(3) 0.141(5) 0.011(4) 0.062(5) 0.025(4) C216 0.195(6) 0.088(4) 0.128(5) 0.000(4) 0.046(5) 0.030(4) C217 0.119(5) 0.095(3) 0.042(3) -0.021(3) -0.004(3) -0.007(4) C218 0.158(5) 0.053(3) 0.070(3) 0.009(3) -0.029(4) -0.006(3) C219 0.124(5) 0.065(3) 0.064(3) 0.008(3) -0.004(3) -0.010(3) C220 0.116(4) 0.029(2) 0.047(3) -0.010(2) -0.004(3) -0.001(3) C221 0.127(4) 0.055(3) 0.054(3) -0.007(2) -0.013(3) 0.017(3) C222 0.125(5) 0.038(2) 0.080(3) 0.011(2) -0.012(3) 0.012(3) C223 0.076(4) 0.064(3) 0.062(3) 0.000(3) 0.021(3) 0.009(3) C224 0.110(4) 0.062(3) 0.067(3) 0.006(3) -0.004(3) 0.004(3) C225 0.114(5) 0.064(3) 0.065(3) -0.012(3) 0.008(3) -0.005(3) C226 0.154(6) 0.047(3) 0.106(4) -0.010(3) 0.014(4) -0.017(3) C227 0.211(7) 0.047(3) 0.151(6) -0.009(3) 0.019(6) -0.019(4) C228 0.156(6) 0.061(3) 0.152(6) -0.029(3) -0.002(5) -0.026(4) C229 0.136(5) 0.058(3) 0.111(4) -0.025(3) -0.015(4) 0.000(3) C230 0.123(5) 0.047(3) 0.093(4) -0.025(3) 0.020(4) -0.009(3) N301 0.131(4) 0.061(2) 0.074(3) 0.010(2) -0.014(3) -0.007(3) O301 0.147(3) 0.0485(16) 0.078(2) 0.0010(16) -0.030(2) -0.012(2) C301 0.079(4) 0.088(3) 0.071(3) 0.000(3) -0.006(3) -0.020(3) N302 0.135(4) 0.068(2) 0.092(3) -0.011(2) -0.008(3) 0.008(3) O302 0.122(3) 0.0674(19) 0.079(2) 0.0074(18) -0.003(2) 0.009(2) C302 0.104(5) 0.083(3) 0.106(4) 0.001(3) 0.014(4) -0.021(4) N303 0.128(4) 0.0279(18) 0.081(3) -0.0054(19) 0.025(3) 0.003(2) O303 0.076(3) 0.116(3) 0.127(3) 0.008(2) -0.005(2) -0.001(2) C303 0.145(5) 0.110(4) 0.063(3) -0.024(3) 0.020(4) -0.057(4) N304 0.063(3) 0.0357(18) 0.082(3) 0.0000(19) 0.004(2) 0.0025(19) O304 0.131(3) 0.0581(18) 0.083(2) 0.0145(18) -0.001(2) -0.010(2) C304 0.155(6) 0.092(4) 0.110(5) -0.032(4) 0.024(4) -0.048(4) O305 0.110(3) 0.0380(14) 0.069(2) -0.0012(15) 0.003(2) 0.0085(17) C305 0.159(6) 0.100(4) 0.121(5) -0.040(4) 0.015(5) -0.051(4) O306 0.121(3) 0.0533(17) 0.080(2) -0.0038(17) 0.010(2) -0.016(2) C306 0.092(4) 0.069(3) 0.085(4) -0.013(3) -0.012(3) 0.013(3) C307 0.164(6) 0.063(3) 0.090(4) -0.009(3) -0.010(4) -0.020(4) C308 0.087(4) 0.053(3) 0.097(4) 0.015(3) -0.013(3) 0.018(3) C309 0.054(3) 0.059(3) 0.113(4) 0.033(3) 0.028(3) 0.009(3) C310 0.162(6) 0.075(3) 0.078(4) -0.015(3) 0.023(4) 0.014(4) C311 0.117(5) 0.093(4) 0.124(5) 0.010(3) -0.051(4) 0.002(4) C312 0.072(4) 0.070(3) 0.162(6) 0.008(4) 0.032(4) 0.012(3) C313 0.112(5) 0.081(3) 0.086(4) 0.006(3) 0.016(4) -0.007(4) C314 0.088(4) 0.094(4) 0.091(4) 0.011(3) 0.015(4) -0.006(4) C315 0.086(4) 0.073(3) 0.139(4) 0.023(3) -0.021(4) -0.013(3) C316 0.122(4) 0.062(3) 0.130(4) 0.030(3) -0.022(4) -0.008(3) C317 0.081(4) 0.045(2) 0.107(4) 0.021(3) -0.001(3) -0.004(3) C318 0.151(5) 0.067(3) 0.078(4) 0.007(3) 0.017(4) 0.002(4) C319 0.184(6) 0.051(3) 0.054(3) 0.014(3) 0.018(4) 0.014(3) C320 0.109(4) 0.026(2) 0.062(3) 0.011(2) -0.002(3) 0.004(3) C321 0.109(4) 0.068(3) 0.069(3) 0.020(3) 0.035(3) 0.004(3) C322 0.120(5) 0.049(3) 0.069(3) 0.000(3) 0.033(3) -0.003(3) C323 0.070(4) 0.076(3) 0.056(3) 0.013(3) 0.015(3) 0.000(3) C324 0.062(4) 0.052(3) 0.096(4) -0.011(3) 0.029(3) 0.001(3) C325 0.111(5) 0.054(3) 0.086(4) -0.010(3) 0.034(4) -0.015(3) C326 0.141(5) 0.065(3) 0.117(5) 0.014(3) 0.020(4) -0.030(4) C327 0.157(6) 0.100(4) 0.127(5) -0.025(4) 0.056(5) -0.018(4) C328 0.153(6) 0.081(3) 0.156(5) -0.020(4) 0.094(5) -0.043(4) C329 0.165(6) 0.051(3) 0.100(4) 0.004(3) 0.032(4) -0.039(3) C330 0.102(4) 0.093(4) 0.048(3) 0.002(3) 0.030(3) -0.010(4) O11 0.128(3) 0.0641(19) 0.090(2) 0.0092(19) 0.017(2) -0.017(2) N11 0.143(4) 0.070(2) 0.066(3) 0.007(2) 0.004(3) -0.021(3) C11 0.129(5) 0.051(3) 0.078(4) -0.001(3) -0.003(4) -0.023(3) C12 0.115(6) 0.142(5) 0.201(7) 0.010(5) 0.003(6) 0.006(5) C13 0.231(7) 0.087(4) 0.093(4) 0.016(3) 0.008(5) -0.057(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 Ce1 O201 2.089(3) . ? Ce1 O101 2.187(3) . ? Ce1 O301 2.222(3) . ? Ce1 O202 2.314(3) . ? Ce1 O102 2.434(3) . ? Ce1 O302 2.500(3) . ? Ce1 N201 2.586(3) . ? Ce1 N301 2.619(4) . ? Ce1 N101 2.635(4) . ? Ce2 O206 2.179(3) . ? Ce2 O106 2.202(3) . ? Ce2 O306 2.213(3) . ? Ce2 O105 2.356(4) . ? Ce2 O205 2.402(3) . ? Ce2 O305 2.432(3) . ? Ce2 N204 2.629(3) . ? Ce2 N104 2.657(4) . ? Ce2 N304 2.679(3) . ? N101 C107 1.290(5) . ? N101 N102 1.377(5) . ? O101 C101 1.316(5) . ? C101 C106 1.382(6) . ? C101 C102 1.403(6) . ? N102 C108 1.331(5) . ? O102 C108 1.253(5) . ? C102 C103 1.421(7) . ? N103 C123 1.289(5) . ? N103 N104 1.352(5) . ? O103 C112 1.388(5) . ? O103 C115 1.455(5) . ? C103 C104 1.389(8) . ? N104 C124 1.217(5) . ? O104 C117 1.371(6) . ? O104 C116 1.386(6) . ? C104 C105 1.385(7) . ? O105 C123 1.305(6) . ? C105 C106 1.357(6) . ? O106 C130 1.316(5) . ? C106 C107 1.459(6) . ? C108 C109 1.460(6) . ? C109 C114 1.370(6) . ? C109 C110 1.394(6) . ? C110 C111 1.396(6) . ? C111 C112 1.356(7) . ? C112 C113 1.391(6) . ? C113 C114 1.404(6) . ? C115 C116 1.479(7) . ? C117 C122 1.331(6) . ? C117 C118 1.416(7) . ? C118 C119 1.332(7) . ? C119 C120 1.329(6) . ? C120 C121 1.483(6) . ? C120 C123 1.516(7) . ? C121 C122 1.306(7) . ? C124 C125 1.377(6) . ? C125 C130 1.392(6) . ? C125 C26' 1.409(6) . ? C125 C126 1.415(6) . ? C126 C127 1.392(6) . ? C127 C128 1.390(7) . ? C128 C129 1.386(7) . ? C129 C130 1.398(5) . ? C26' C27' 1.385(6) . ? C27' C28' 1.389(6) . ? C28' C29' 1.382(6) . ? C29' C130 1.396(5) . ? N201 C207 1.309(6) . ? N201 N202 1.356(5) . ? O201 C201 1.500(5) . ? C201 C202 1.389(5) . ? C201 C206 1.411(6) . ? N202 C208 1.233(6) . ? O202 C208 1.323(5) . ? C202 C203 1.393(5) . ? N203 C223 1.349(5) . ? N203 N204 1.377(5) . ? O203 C212 1.351(7) . ? O203 C215 1.467(7) . ? C203 C204 1.380(5) . ? N204 C224 1.282(5) . ? O204 C217 1.411(5) . ? O204 C216 1.462(6) . ? C204 C205 1.375(5) . ? O205 C223 1.268(5) . ? C205 C206 1.382(5) . ? O206 C230 1.375(5) . ? C206 C207 1.405(7) . ? C208 C209 1.432(7) . ? C209 C210 1.387(7) . ? C209 C214 1.465(6) . ? C210 C211 1.401(8) . ? C211 C212 1.415(8) . ? C212 C213 1.363(7) . ? C213 C214 1.340(7) . ? C215 C216 1.337(8) . ? C217 C222 1.361(6) . ? C217 C218 1.386(6) . ? C218 C219 1.430(6) . ? C219 C220 1.352(5) . ? C220 C221 1.361(6) . ? C220 C223 1.482(6) . ? C221 C222 1.331(6) . ? C224 C225 1.414(6) . ? C225 C230 1.373(7) . ? C225 C226 1.407(6) . ? C226 C227 1.360(8) . ? C227 C228 1.406(8) . ? C228 C229 1.352(6) . ? C229 C230 1.441(7) . ? N301 C307 1.316(6) . ? N301 N302 1.385(6) . ? O301 C301 1.357(5) . ? C301 C302 1.376(7) . ? C301 C306 1.376(7) . ? N302 C308 1.371(6) . ? O302 C308 1.235(6) . ? C302 C303 1.444(7) . ? N303 C323 1.332(6) . ? N303 N304 1.384(4) . ? O303 C312 1.296(6) . ? O303 C315 1.398(6) . ? C303 C304 1.324(8) . ? N304 C324 1.273(6) . ? O304 C317 1.383(5) . ? O304 C316 1.434(5) . ? C304 C305 1.355(8) . ? O305 C323 1.230(5) . ? C305 C306 1.425(7) . ? O306 C330 1.291(6) . ? C306 C307 1.405(7) . ? C308 C309 1.429(7) . ? C309 C314 1.342(7) . ? C309 C310 1.444(7) . ? C310 C311 1.419(8) . ? C311 C312 1.318(8) . ? C312 C313 1.434(8) . ? C313 C314 1.392(7) . ? C315 C316 1.466(7) . ? C317 C322 1.382(7) . ? C317 C318 1.450(6) . ? C318 C319 1.334(6) . ? C319 C320 1.344(7) . ? C320 C321 1.421(6) . ? C320 C323 1.514(6) . ? C321 C322 1.385(6) . ? C324 C325 1.377(6) . ? C325 C326 1.345(8) . ? C325 C330 1.364(6) . ? C326 C327 1.398(8) . ? C327 C328 1.446(8) . ? C328 C329 1.317(8) . ? C329 C330 1.417(7) . ? O11 C11 1.237(5) . ? N11 C11 1.313(7) . ? N11 C12 1.416(7) . ? N11 C13 1.519(6) . ? O21 C21 1.210(2) . ? N21 C21 1.388(3) . ? N21 C22 1.423(3) . ? N21 C23 1.434(3) . ? C423 O421 1.199(4) . ? C423 N421 1.381(3) . ? C422 N421 1.431(3) . ? C421 N421 1.431(3) . ? O31 C33 1.192(3) . ? N31 C33 1.371(4) . ? N31 C32 1.476(10) . ? N31 C31 1.570(9) . ? N431 C433 1.377(3) . ? N431 C432 1.430(3) . ? N431 C431 1.435(3) . ? O431 C433 1.198(3) . ? N51 C53 1.382(3) . ? N51 C51 1.430(3) . ? N51 C52 1.431(3) . ? C53 O51 1.200(4) . ? N51' C53' 1.380(3) . ? N51' C52' 1.430(3) . ? N51' C51' 1.433(3) . ? O51' C53' 1.199(4) . ? O71 C73 1.193(3) . ? N71 C73 1.382(3) . ? N71 C72 1.432(3) . ? N71 C71 1.435(3) . ? N81 C83 1.383(3) . ? N81 C82 1.430(3) . ? N81 C81 1.432(3) . ? O81 C83 1.1997(17) . ? O81' C83' 1.205(4) . ? C83' N81' 1.384(3) . ? C82' N81' 1.433(3) . ? C81' N81' 1.431(3) . ? N61 C63 1.384(3) . ? N61 C62 1.432(3) . ? N61 C61 1.434(2) . ? O61 C63 1.199(3) . ? O61' C63' 1.200(3) . ? N61' C63' 1.383(3) . ? N61' C62' 1.431(3) . ? N61' C61' 1.434(3) . ? C5 O5 1.529(18) . ? O5' C5' 1.53(2) . ? C91 O91 1.498(8) . ? C6 O6 1.523(6) . ? O6' C6' 1.69(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 O201 Ce1 O101 82.16(13) . . ? O201 Ce1 O301 90.70(12) . . ? O101 Ce1 O301 77.19(11) . . ? O201 Ce1 O202 133.63(11) . . ? O101 Ce1 O202 139.82(12) . . ? O301 Ce1 O202 83.82(12) . . ? O201 Ce1 O102 79.97(12) . . ? O101 Ce1 O102 128.55(11) . . ? O301 Ce1 O102 150.15(9) . . ? O202 Ce1 O102 82.46(11) . . ? O201 Ce1 O302 139.35(11) . . ? O101 Ce1 O302 95.20(11) . . ? O301 Ce1 O302 128.48(11) . . ? O202 Ce1 O302 69.73(11) . . ? O102 Ce1 O302 70.16(10) . . ? O201 Ce1 N201 71.80(12) . . ? O101 Ce1 N201 144.51(12) . . ? O301 Ce1 N201 79.40(10) . . ? O202 Ce1 N201 61.91(12) . . ? O102 Ce1 N201 70.75(10) . . ? O302 Ce1 N201 120.27(11) . . ? O201 Ce1 N301 149.43(12) . . ? O101 Ce1 N301 71.38(13) . . ? O301 Ce1 N301 69.08(12) . . ? O202 Ce1 N301 68.81(11) . . ? O102 Ce1 N301 128.67(12) . . ? O302 Ce1 N301 60.41(11) . . ? N201 Ce1 N301 123.40(12) . . ? O201 Ce1 N101 77.79(12) . . ? O101 Ce1 N101 67.18(11) . . ? O301 Ce1 N101 143.63(11) . . ? O202 Ce1 N101 128.71(12) . . ? O102 Ce1 N101 62.02(10) . . ? O302 Ce1 N101 64.18(12) . . ? N201 Ce1 N101 127.16(11) . . ? N301 Ce1 N101 104.63(11) . . ? O206 Ce2 O106 87.93(11) . . ? O206 Ce2 O306 87.67(12) . . ? O106 Ce2 O306 83.85(12) . . ? O206 Ce2 O105 83.48(12) . . ? O106 Ce2 O105 129.68(11) . . ? O306 Ce2 O105 144.68(11) . . ? O206 Ce2 O205 128.36(11) . . ? O106 Ce2 O205 141.72(10) . . ? O306 Ce2 O205 85.80(11) . . ? O105 Ce2 O205 73.52(11) . . ? O206 Ce2 O305 143.08(11) . . ? O106 Ce2 O305 87.11(10) . . ? O306 Ce2 O305 128.00(10) . . ? O105 Ce2 O305 71.98(10) . . ? O205 Ce2 O305 70.84(9) . . ? O206 Ce2 N204 68.27(11) . . ? O106 Ce2 N204 146.20(11) . . ? O306 Ce2 N204 71.99(12) . . ? O105 Ce2 N204 72.97(11) . . ? O205 Ce2 N204 61.01(10) . . ? O305 Ce2 N204 126.36(11) . . ? O206 Ce2 N104 81.15(11) . . ? O106 Ce2 N104 66.64(12) . . ? O306 Ce2 N104 148.64(12) . . ? O105 Ce2 N104 63.05(10) . . ? O205 Ce2 N104 123.89(11) . . ? O305 Ce2 N104 63.37(10) . . ? N204 Ce2 N104 128.60(11) . . ? O206 Ce2 N304 148.84(12) . . ? O106 Ce2 N304 72.07(11) . . ? O306 Ce2 N304 67.07(10) . . ? O105 Ce2 N304 127.68(10) . . ? O205 Ce2 N304 69.95(10) . . ? O305 Ce2 N304 61.43(10) . . ? N204 Ce2 N304 116.89(11) . . ? N104 Ce2 N304 110.72(10) . . ? C107 N101 N102 113.9(4) . . ? C107 N101 Ce1 131.2(3) . . ? N102 N101 Ce1 114.2(2) . . ? C101 O101 Ce1 148.5(3) . . ? O101 C101 C106 122.1(4) . . ? O101 C101 C102 118.7(4) . . ? C106 C101 C102 119.1(4) . . ? C108 N102 N101 117.8(4) . . ? C108 O102 Ce1 125.1(3) . . ? C101 C102 C103 121.1(5) . . ? C123 N103 N104 120.5(4) . . ? C112 O103 C115 118.0(4) . . ? C104 C103 C102 116.5(5) . . ? C124 N104 N103 118.5(4) . . ? C124 N104 Ce2 128.6(3) . . ? N103 N104 Ce2 111.4(2) . . ? C117 O104 C116 122.8(4) . . ? C105 C104 C103 122.1(5) . . ? C123 O105 Ce2 124.6(3) . . ? C106 C105 C104 120.3(5) . . ? C130 O106 Ce2 149.7(3) . . ? C105 C106 C101 120.8(4) . . ? C105 C106 C107 116.8(4) . . ? C101 C106 C107 122.4(4) . . ? N101 C107 C106 124.6(4) . . ? O102 C108 N102 120.7(4) . . ? O102 C108 C109 119.6(4) . . ? N102 C108 C109 119.7(4) . . ? C114 C109 C110 118.9(4) . . ? C114 C109 C108 122.6(4) . . ? C110 C109 C108 118.2(4) . . ? C109 C110 C111 121.0(4) . . ? C112 C111 C110 118.7(4) . . ? C111 C112 O103 125.3(4) . . ? C111 C112 C113 122.1(4) . . ? O103 C112 C113 112.6(4) . . ? C112 C113 C114 118.2(5) . . ? C109 C114 C113 120.9(4) . . ? O103 C115 C116 110.7(4) . . ? O104 C116 C115 108.5(4) . . ? C122 C117 O104 116.6(5) . . ? C122 C117 C118 120.9(5) . . ? O104 C117 C118 122.5(4) . . ? C119 C118 C117 115.2(4) . . ? C120 C119 C118 127.4(5) . . ? C119 C120 C121 114.6(5) . . ? C119 C120 C123 124.0(4) . . ? C121 C120 C123 121.2(4) . . ? C122 C121 C120 118.8(4) . . ? C121 C122 C117 123.0(5) . . ? N103 C123 O105 120.2(4) . . ? N103 C123 C120 118.5(4) . . ? O105 C123 C120 121.1(4) . . ? N104 C124 C125 130.9(5) . . ? C124 C125 C130 122.5(3) . . ? C124 C125 C26' 118.8(4) . . ? C130 C125 C26' 118.0(4) . . ? C124 C125 C126 121.6(4) . . ? C130 C125 C126 114.3(4) . . ? C26' C125 C126 22.0(5) . . ? C127 C126 C125 124.1(5) . . ? C128 C127 C126 115.8(5) . . ? C129 C128 C127 124.3(6) . . ? C128 C129 C130 115.6(5) . . ? C27' C26' C125 120.7(5) . . ? C26' C27' C28' 118.2(5) . . ? C29' C28' C27' 123.3(5) . . ? C28' C29' C130 116.9(5) . . ? O106 C130 C125 119.1(3) . . ? O106 C130 C29' 118.8(4) . . ? C125 C130 C29' 122.1(4) . . ? O106 C130 C129 116.5(4) . . ? C125 C130 C129 124.3(4) . . ? C29' C130 C129 2.4(4) . . ? C207 N201 N202 116.0(3) . . ? C207 N201 Ce1 128.0(3) . . ? N202 N201 Ce1 115.9(2) . . ? C201 O201 Ce1 141.6(3) . . ? C202 C201 C206 118.9(4) . . ? C202 C201 O201 120.4(4) . . ? C206 C201 O201 120.6(4) . . ? C208 N202 N201 112.2(4) . . ? C208 O202 Ce1 121.1(3) . . ? C201 C202 C203 119.9(4) . . ? C223 N203 N204 117.4(3) . . ? C212 O203 C215 115.5(5) . . ? C204 C203 C202 121.1(4) . . ? C224 N204 N203 114.9(4) . . ? C224 N204 Ce2 128.3(3) . . ? N203 N204 Ce2 115.6(2) . . ? C217 O204 C216 121.9(4) . . ? C205 C204 C203 118.8(4) . . ? C223 O205 Ce2 128.9(3) . . ? C204 C205 C206 121.7(4) . . ? C230 O206 Ce2 141.2(3) . . ? C205 C206 C207 118.4(4) . . ? C205 C206 C201 119.4(4) . . ? C207 C206 C201 122.2(4) . . ? N201 C207 C206 129.5(4) . . ? N202 C208 O202 126.1(4) . . ? N202 C208 C209 121.4(4) . . ? O202 C208 C209 112.4(4) . . ? C210 C209 C208 126.7(4) . . ? C210 C209 C214 111.7(4) . . ? C208 C209 C214 121.5(4) . . ? C209 C210 C211 130.0(5) . . ? C210 C211 C212 113.6(5) . . ? O203 C212 C213 120.2(5) . . ? O203 C212 C211 121.0(5) . . ? C213 C212 C211 118.7(5) . . ? C214 C213 C212 126.6(5) . . ? C213 C214 C209 119.1(5) . . ? C216 C215 O203 105.2(5) . . ? C215 C216 O204 111.5(5) . . ? C222 C217 C218 122.4(4) . . ? C222 C217 O204 116.7(4) . . ? C218 C217 O204 120.9(4) . . ? C217 C218 C219 115.9(4) . . ? C220 C219 C218 120.0(4) . . ? C219 C220 C221 120.7(4) . . ? C219 C220 C223 114.3(4) . . ? C221 C220 C223 124.9(4) . . ? C222 C221 C220 121.3(4) . . ? C221 C222 C217 119.6(4) . . ? O205 C223 N203 117.1(4) . . ? O205 C223 C220 122.0(4) . . ? N203 C223 C220 120.8(4) . . ? N204 C224 C225 125.9(4) . . ? C230 C225 C226 118.0(5) . . ? C230 C225 C224 124.3(4) . . ? C226 C225 C224 117.7(4) . . ? C227 C226 C225 120.4(5) . . ? C226 C227 C228 121.4(5) . . ? C229 C228 C227 120.0(5) . . ? C228 C229 C230 118.3(5) . . ? C225 C230 O206 121.0(4) . . ? C225 C230 C229 121.8(4) . . ? O206 C230 C229 117.3(4) . . ? C307 N301 N302 112.2(4) . . ? C307 N301 Ce1 131.3(4) . . ? N302 N301 Ce1 116.6(3) . . ? C301 O301 Ce1 137.1(3) . . ? O301 C301 C302 116.8(4) . . ? O301 C301 C306 124.0(4) . . ? C302 C301 C306 119.2(5) . . ? C308 N302 N301 116.0(4) . . ? C308 O302 Ce1 125.2(3) . . ? C301 C302 C303 118.0(5) . . ? C323 N303 N304 117.4(3) . . ? C312 O303 C315 118.2(5) . . ? C304 C303 C302 123.3(5) . . ? C324 N304 N303 118.2(3) . . ? C324 N304 Ce2 127.1(3) . . ? N303 N304 Ce2 113.0(3) . . ? C317 O304 C316 116.9(4) . . ? C303 C304 C305 117.9(5) . . ? C323 O305 Ce2 126.1(3) . . ? C304 C305 C306 121.8(5) . . ? C330 O306 Ce2 148.4(3) . . ? C301 C306 C307 126.2(4) . . ? C301 C306 C305 119.6(5) . . ? C307 C306 C305 114.2(5) . . ? N301 C307 C306 121.2(5) . . ? O302 C308 N302 118.8(5) . . ? O302 C308 C309 125.3(5) . . ? N302 C308 C309 115.8(4) . . ? C314 C309 C308 126.9(5) . . ? C314 C309 C310 113.0(5) . . ? C308 C309 C310 120.2(5) . . ? C311 C310 C309 118.6(5) . . ? C312 C311 C310 125.2(5) . . ? O303 C312 C311 115.4(6) . . ? O303 C312 C313 126.7(5) . . ? C311 C312 C313 117.9(5) . . ? C314 C313 C312 115.2(5) . . ? C309 C314 C313 129.9(5) . . ? O303 C315 C316 108.9(5) . . ? O304 C316 C315 113.5(4) . . ? C322 C317 O304 126.0(4) . . ? C322 C317 C318 122.2(4) . . ? O304 C317 C318 111.8(4) . . ? C319 C318 C317 116.3(5) . . ? C318 C319 C320 123.6(4) . . ? C319 C320 C321 120.6(4) . . ? C319 C320 C323 119.9(4) . . ? C321 C320 C323 119.1(4) . . ? C322 C321 C320 118.9(4) . . ? C317 C322 C321 118.3(4) . . ? O305 C323 N303 121.5(4) . . ? O305 C323 C320 118.7(4) . . ? N303 C323 C320 119.6(4) . . ? N304 C324 C325 127.4(4) . . ? C326 C325 C330 115.6(5) . . ? C326 C325 C324 118.7(4) . . ? C330 C325 C324 125.6(5) . . ? C325 C326 C327 127.8(5) . . ? C326 C327 C328 114.2(6) . . ? C329 C328 C327 118.9(5) . . ? C328 C329 C330 123.3(5) . . ? O306 C330 C325 120.1(5) . . ? O306 C330 C329 119.7(5) . . ? C325 C330 C329 120.2(5) . . ? C11 N11 C12 125.5(4) . . ? C11 N11 C13 118.6(5) . . ? C12 N11 C13 115.9(5) . . ? O11 C11 N11 120.1(5) . . ? C21 N21 C22 122.1(2) . . ? C21 N21 C23 119.7(2) . . ? C22 N21 C23 118.2(3) . . ? O21 C21 N21 115.0(3) . . ? O421 C423 N421 117.0(4) . . ? C423 N421 C421 121.2(2) . . ? C423 N421 C422 121.2(3) . . ? C421 N421 C422 117.7(3) . . ? C33 N31 C32 127.5(5) . . ? C33 N31 C31 105.6(5) . . ? C32 N31 C31 120.8(6) . . ? O31 C33 N31 118.3(4) . . ? C433 N431 C432 121.5(2) . . ? C433 N431 C431 121.1(2) . . ? C432 N431 C431 117.3(2) . . ? O431 C433 N431 117.4(3) . . ? C53 N51 C51 121.1(3) . . ? C53 N51 C52 121.1(2) . . ? C51 N51 C52 117.7(2) . . ? O51 C53 N51 116.7(4) . . ? C53' N51' C52' 121.4(3) . . ? C53' N51' C51' 121.0(2) . . ? C52' N51' C51' 117.6(3) . . ? O51' C53' N51' 116.8(3) . . ? C73 N71 C72 120.8(2) . . ? C73 N71 C71 120.5(2) . . ? C72 N71 C71 117.1(2) . . ? O71 C73 N71 117.3(3) . . ? C83 N81 C82 121.1(2) . . ? C83 N81 C81 120.6(3) . . ? C82 N81 C81 117.7(2) . . ? O81 C83 N81 116.7(3) . . ? O81' C83' N81' 115.8(4) . . ? C83' N81' C81' 121.0(2) . . ? C83' N81' C82' 120.6(3) . . ? C81' N81' C82' 117.6(2) . . ? C63 N61 C62 120.9(2) . . ? C63 N61 C61 120.6(2) . . ? C62 N61 C61 117.4(2) . . ? O61 C63 N61 116.6(3) . . ? C63' N61' C62' 120.9(2) . . ? C63' N61' C61' 120.6(3) . . ? C62' N61' C61' 117.5(2) . . ? O61' C63' N61' 116.7(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.511 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.101 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 0.500 0.151 0.750 240 20 ' ' 2 0.000 0.349 0.250 240 20 ' ' 3 0.000 0.651 0.750 240 20 ' ' 4 0.500 0.849 0.250 240 20 ' ' _database_code_depnum_ccdc_archive 'CCDC 947247' ####################################################################### # # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93.25 H92.25 Ce2 N13.75 O22.75' _chemical_formula_weight 2049.80 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1804(14) _cell_length_b 17.6680(16) _cell_length_c 19.8999(18) _cell_angle_alpha 94.536(6) _cell_angle_beta 112.377(5) _cell_angle_gamma 98.093(6) _cell_volume 4834.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6253 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.51 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36166 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_unetI/netI 0.1657 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16394 _reflns_number_gt 8543 _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. Except the solvent mathanol and water molecules, the other non-hydrogen atoms were refined anisotropically. Hydrogen atoms within the ligand backbones and the solvent DMF molecules were fixed geometrically at calculated distances and allowed to ride on the parent non-hydrogen atoms. ; _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^)+(0.0743P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16394 _refine_ls_number_parameters 1217 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1563 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2020 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce2 Ce -1.25485(2) 0.81085(2) -0.414918(16) 0.03955(11) Uani 1 1 d . . . Ce1 Ce -0.70691(3) 0.25388(2) -0.083866(16) 0.04260(11) Uani 1 1 d . . . O103 O -1.1674(3) 0.4934(2) -0.0952(2) 0.0560(13) Uani 1 1 d . . . O105 O -1.2341(3) 0.9375(2) -0.39865(17) 0.0444(12) Uani 1 1 d . . . O104 O -1.2278(3) 0.7216(2) -0.32463(17) 0.0432(12) Uani 1 1 d . . . O102 O -0.8216(3) 0.3219(2) -0.07449(19) 0.0492(13) Uani 1 1 d . . . O101 O -0.7101(3) 0.1328(2) -0.10623(19) 0.0513(13) Uani 1 1 d . . . O303 O -0.6974(3) 0.6782(3) -0.2793(2) 0.0643(14) Uani 1 1 d . . . O305 O -1.3339(3) 0.8235(2) -0.53316(18) 0.0440(12) Uani 1 1 d . . . O304 O -1.0767(3) 0.8201(2) -0.34615(17) 0.0442(12) Uani 1 1 d . . . O302 O -0.6829(3) 0.3718(2) -0.13780(18) 0.0454(12) Uani 1 1 d . . . O301 O -0.6713(3) 0.2415(2) 0.03169(18) 0.0545(14) Uani 1 1 d . . . O203 O -1.0797(3) 0.3765(2) -0.49810(19) 0.0511(13) Uani 1 1 d . . . O205 O -1.3900(3) 0.8234(2) -0.40298(19) 0.0487(12) Uani 1 1 d . . . O204 O -1.2029(3) 0.7031(2) -0.45960(17) 0.0402(12) Uani 1 1 d . . . O202 O -0.8336(3) 0.2493(2) -0.20889(18) 0.0472(12) Uani 1 1 d . . . O201 O -0.5441(3) 0.2657(2) -0.05442(19) 0.0499(13) Uani 1 1 d . . . N304 N -1.1355(3) 0.8661(3) -0.4748(2) 0.0392(14) Uani 1 1 d . . . N104 N -1.2103(3) 0.8672(3) -0.2769(2) 0.0439(15) Uani 1 1 d . . . N103 N -1.1839(3) 0.8140(3) -0.2277(2) 0.0461(16) Uani 1 1 d . . . H10A H -1.1604 0.8279 -0.1810 0.055 Uiso 1 1 calc R . . N102 N -0.9409(4) 0.2186(3) -0.0983(3) 0.0586(17) Uani 1 1 d . . . H10B H -0.9985 0.1988 -0.1030 0.070 Uiso 1 1 calc R . . N101 N -0.8736(4) 0.1741(3) -0.1008(2) 0.0480(16) Uani 1 1 d . . . N303 N -1.0415(3) 0.8519(3) -0.4405(2) 0.0428(15) Uani 1 1 d . . . H30A H -0.9991 0.8617 -0.4591 0.051 Uiso 1 1 calc R . . N302 N -0.6263(3) 0.4526(3) -0.0316(2) 0.0472(16) Uani 1 1 d . . . H30B H -0.6048 0.4988 -0.0080 0.057 Uiso 1 1 calc R . . N301 N -0.6264(3) 0.3880(3) 0.0050(2) 0.0437(15) Uani 1 1 d . . . N204 N -1.3814(3) 0.6834(3) -0.4689(2) 0.0403(14) Uani 1 1 d . . . N203 N -1.3416(4) 0.6183(3) -0.4795(2) 0.0472(16) Uani 1 1 d . . . H20A H -1.3738 0.5719 -0.4896 0.057 Uiso 1 1 calc R . . N202 N -0.7319(4) 0.2475(3) -0.2658(2) 0.0461(15) Uani 1 1 d . . . H20B H -0.7206 0.2487 -0.3049 0.055 Uiso 1 1 calc R . . N201 N -0.6643(3) 0.2311(3) -0.2019(2) 0.0388(14) Uani 1 1 d . . . C123 C -1.2507(4) 0.9928(3) -0.2924(3) 0.0447(19) Uani 1 1 d . . . C128 C -1.2618(4) 0.9913(3) -0.3654(3) 0.0420(18) Uani 1 1 d . . . C127 C -1.2995(4) 1.0510(3) -0.4040(3) 0.049(2) Uani 1 1 d . . . H12A H -1.3081 1.0501 -0.4529 0.058 Uiso 1 1 calc R . . C126 C -1.3235(5) 1.1105(4) -0.3695(3) 0.061(2) Uani 1 1 d . . . H12B H -1.3485 1.1495 -0.3953 0.073 Uiso 1 1 calc R . . C125 C -1.3104(5) 1.1125(4) -0.2956(3) 0.063(2) Uani 1 1 d . . . H12C H -1.3260 1.1532 -0.2723 0.076 Uiso 1 1 calc R . . C124 C -1.2755(5) 1.0559(4) -0.2584(3) 0.059(2) Uani 1 1 d . . . H12D H -1.2673 1.0578 -0.2095 0.071 Uiso 1 1 calc R . . C122 C -1.2221(4) 0.9318(4) -0.2516(3) 0.0441(18) Uani 1 1 d . . . H12E H -1.2109 0.9396 -0.2020 0.053 Uiso 1 1 calc R . . C121 C -1.1971(4) 0.7408(4) -0.2568(3) 0.0478(19) Uani 1 1 d . . . C118 C -1.1806(4) 0.6792(3) -0.2097(3) 0.0415(18) Uani 1 1 d . . . C119 C -1.1709(5) 0.6105(4) -0.2397(3) 0.058(2) Uani 1 1 d . . . H11A H -1.1697 0.6053 -0.2862 0.069 Uiso 1 1 calc R . . C120 C -1.1629(5) 0.5485(4) -0.2007(3) 0.058(2) Uani 1 1 d . . . H12F H -1.1546 0.5018 -0.2203 0.070 Uiso 1 1 calc R . . C115 C -1.1671(4) 0.5566(4) -0.1332(3) 0.0472(19) Uani 1 1 d . . . C116 C -1.1768(4) 0.6248(4) -0.1023(3) 0.0478(19) Uani 1 1 d . . . H11B H -1.1797 0.6290 -0.0563 0.057 Uiso 1 1 calc R . . C117 C -1.1823(4) 0.6871(4) -0.1392(3) 0.0459(19) Uani 1 1 d . . . H11C H -1.1872 0.7343 -0.1181 0.055 Uiso 1 1 calc R . . C112 C -1.1063(4) 0.4429(4) -0.0965(3) 0.053(2) Uani 1 1 d . . . C113 C -1.0096(4) 0.4718(4) -0.0847(3) 0.054(2) Uani 1 1 d . . . H11D H -0.9869 0.5247 -0.0785 0.065 Uiso 1 1 calc R . . C114 C -0.9501(4) 0.4206(4) -0.0825(3) 0.0486(19) Uani 1 1 d . . . H11E H -0.8863 0.4398 -0.0750 0.058 Uiso 1 1 calc R . . C109 C -0.9789(4) 0.3418(3) -0.0909(3) 0.0444(19) Uani 1 1 d . . . C110 C -1.0754(5) 0.3159(4) -0.1023(3) 0.058(2) Uani 1 1 d . . . H11F H -1.0982 0.2631 -0.1081 0.070 Uiso 1 1 calc R . . C111 C -1.1370(5) 0.3653(4) -0.1052(3) 0.059(2) Uani 1 1 d . . . H11G H -1.2010 0.3459 -0.1133 0.071 Uiso 1 1 calc R . . C108 C -0.9095(5) 0.2930(4) -0.0881(3) 0.0481(19) Uani 1 1 d . . . C107 C -0.9040(4) 0.1000(4) -0.1184(3) 0.054(2) Uani 1 1 d . . . H10C H -0.9661 0.0820 -0.1213 0.065 Uiso 1 1 calc R . . C106 C -0.8554(5) 0.0438(4) -0.1335(3) 0.051(2) Uani 1 1 d . . . C101 C -0.7588(5) 0.0620(4) -0.1297(3) 0.054(2) Uani 1 1 d . . . C102 C -0.7209(6) 0.0019(4) -0.1515(3) 0.073(2) Uani 1 1 d . . . H10D H -0.6602 0.0135 -0.1533 0.087 Uiso 1 1 calc R . . C103 C -0.7693(6) -0.0749(4) -0.1709(4) 0.085(3) Uani 1 1 d . . . H10E H -0.7391 -0.1134 -0.1822 0.102 Uiso 1 1 calc R . . C104 C -0.8639(6) -0.0939(4) -0.1733(4) 0.085(3) Uani 1 1 d . . . H10F H -0.8982 -0.1444 -0.1878 0.102 Uiso 1 1 calc R . . C105 C -0.9038(5) -0.0355(4) -0.1537(3) 0.066(2) Uani 1 1 d . . . H10G H -0.9653 -0.0478 -0.1535 0.079 Uiso 1 1 calc R . . C323 C -1.2445(4) 0.9221(3) -0.5715(3) 0.0436(18) Uani 1 1 d . . . C328 C -1.3337(4) 0.8831(4) -0.5703(3) 0.0471(19) Uani 1 1 d . . . C327 C -1.4175(4) 0.9071(4) -0.6139(3) 0.052(2) Uani 1 1 d . . . H32A H -1.4763 0.8823 -0.6148 0.063 Uiso 1 1 calc R . . C326 C -1.4188(5) 0.9639(4) -0.6547(3) 0.058(2) Uani 1 1 d . . . H32B H -1.4771 0.9789 -0.6812 0.070 Uiso 1 1 calc R . . C325 C -1.3342(5) 1.0004(4) -0.6578(3) 0.060(2) Uani 1 1 d . . . H32C H -1.3359 1.0388 -0.6874 0.072 Uiso 1 1 calc R . . C324 C -1.2478(5) 0.9800(4) -0.6173(3) 0.052(2) Uani 1 1 d . . . H32D H -1.1909 1.0043 -0.6198 0.063 Uiso 1 1 calc R . . C322 C -1.1493(4) 0.9063(3) -0.5272(3) 0.0433(18) Uani 1 1 d . . . H32E H -1.0966 0.9263 -0.5376 0.052 Uiso 1 1 calc R . . C321 C -1.0204(4) 0.8225(3) -0.3777(3) 0.0393(17) Uani 1 1 d . . . C318 C -0.9328(4) 0.7907(3) -0.3493(3) 0.0403(18) Uani 1 1 d . . . C319 C -0.9282(4) 0.7370(3) -0.3018(3) 0.0435(18) Uani 1 1 d . . . H31A H -0.9788 0.7262 -0.2864 0.052 Uiso 1 1 calc R . . C320 C -0.8513(4) 0.6989(4) -0.2764(3) 0.053(2) Uani 1 1 d . . . H32F H -0.8503 0.6629 -0.2446 0.063 Uiso 1 1 calc R . . C315 C -0.7753(4) 0.7148(4) -0.2986(3) 0.0469(19) Uani 1 1 d . . . C316 C -0.7757(4) 0.7701(3) -0.3442(3) 0.0453(19) Uani 1 1 d . . . H31B H -0.7234 0.7829 -0.3573 0.054 Uiso 1 1 calc R . . C317 C -0.8542(4) 0.8055(3) -0.3697(3) 0.048(2) Uani 1 1 d . . . H31C H -0.8553 0.8411 -0.4019 0.058 Uiso 1 1 calc R . . C312 C -0.6945(4) 0.6202(4) -0.2355(3) 0.0490(19) Uani 1 1 d . . . C313 C -0.6562(5) 0.6404(4) -0.1618(3) 0.060(2) Uani 1 1 d . . . H31D H -0.6397 0.6922 -0.1412 0.073 Uiso 1 1 calc R . . C314 C -0.6418(5) 0.5830(4) -0.1174(3) 0.059(2) Uani 1 1 d . . . H31E H -0.6129 0.5966 -0.0666 0.070 Uiso 1 1 calc R . . C309 C -0.6698(4) 0.5049(3) -0.1475(3) 0.0401(18) Uani 1 1 d . . . C310 C -0.7075(5) 0.4872(4) -0.2238(3) 0.063(2) Uani 1 1 d . . . H31F H -0.7244 0.4358 -0.2457 0.076 Uiso 1 1 calc R . . C311 C -0.7198(5) 0.5445(4) -0.2663(4) 0.067(2) Uani 1 1 d . . . H31G H -0.7458 0.5319 -0.3172 0.080 Uiso 1 1 calc R . . C308 C -0.6610(4) 0.4394(4) -0.1049(3) 0.0419(18) Uani 1 1 d . . . C307 C -0.5945(4) 0.4039(4) 0.0746(3) 0.0484(19) Uani 1 1 d . . . H30C H -0.5724 0.4558 0.0942 0.058 Uiso 1 1 calc R . . C306 C -0.5889(4) 0.3520(4) 0.1247(3) 0.053(2) Uani 1 1 d . . . C301 C -0.6303(4) 0.2703(4) 0.1006(3) 0.0503(19) Uani 1 1 d . . . C302 C -0.6255(5) 0.2237(4) 0.1559(3) 0.063(2) Uani 1 1 d . . . H30D H -0.6532 0.1715 0.1425 0.075 Uiso 1 1 calc R . . C303 C -0.5802(5) 0.2542(5) 0.2301(3) 0.079(3) Uani 1 1 d . . . H30E H -0.5779 0.2220 0.2653 0.095 Uiso 1 1 calc R . . C304 C -0.5385(5) 0.3317(5) 0.2521(3) 0.080(3) Uani 1 1 d . . . H30F H -0.5064 0.3509 0.3019 0.096 Uiso 1 1 calc R . . C305 C -0.5446(5) 0.3811(5) 0.1996(3) 0.071(3) Uani 1 1 d . . . H30G H -0.5190 0.4335 0.2145 0.085 Uiso 1 1 calc R . . C223 C -1.5273(4) 0.7262(3) -0.4715(3) 0.0391(17) Uani 1 1 d . . . C228 C -1.4847(4) 0.8005(3) -0.4328(3) 0.0423(18) Uani 1 1 d . . . C227 C -1.5460(4) 0.8507(4) -0.4262(3) 0.0450(18) Uani 1 1 d . . . H22A H -1.5188 0.9005 -0.4012 0.054 Uiso 1 1 calc R . . C226 C -1.6424(4) 0.8287(4) -0.4550(3) 0.051(2) Uani 1 1 d . . . H22B H -1.6810 0.8637 -0.4505 0.061 Uiso 1 1 calc R . . C225 C -1.6854(5) 0.7542(4) -0.4915(3) 0.058(2) Uani 1 1 d . . . H22C H -1.7524 0.7386 -0.5100 0.070 Uiso 1 1 calc R . . C224 C -1.6278(4) 0.7037(4) -0.4999(3) 0.0478(19) Uani 1 1 d . . . H22D H -1.6562 0.6540 -0.5249 0.057 Uiso 1 1 calc R . . C222 C -1.4709(4) 0.6687(4) -0.4822(3) 0.0444(19) Uani 1 1 d . . . H22E H -1.5032 0.6179 -0.4999 0.053 Uiso 1 1 calc R . . C221 C -1.2513(4) 0.6345(3) -0.4727(3) 0.0413(18) Uani 1 1 d . . . C218 C -1.2067(4) 0.5671(3) -0.4811(3) 0.0373(17) Uani 1 1 d . . . C219 C -1.1106(4) 0.5691(3) -0.4376(3) 0.0451(19) Uani 1 1 d . . . H21A H -1.0751 0.6138 -0.4052 0.054 Uiso 1 1 calc R . . C220 C -1.0660(4) 0.5088(3) -0.4402(3) 0.0434(19) Uani 1 1 d . . . H22F H -1.0010 0.5119 -0.4103 0.052 Uiso 1 1 calc R . . C215 C -1.1181(4) 0.4431(4) -0.4875(3) 0.0469(19) Uani 1 1 d . . . C216 C -1.2159(4) 0.4389(3) -0.5339(3) 0.049(2) Uani 1 1 d . . . H21B H -1.2513 0.3947 -0.5672 0.058 Uiso 1 1 calc R . . C217 C -1.2574(4) 0.5013(3) -0.5288(3) 0.0427(18) Uani 1 1 d . . . H21C H -1.3223 0.4991 -0.5588 0.051 Uiso 1 1 calc R . . C212 C -1.0150(4) 0.3505(3) -0.4387(3) 0.0417(18) Uani 1 1 d . . . C213 C -1.0206(5) 0.3566(4) -0.3697(3) 0.052(2) Uani 1 1 d . . . H21D H -1.0671 0.3803 -0.3614 0.062 Uiso 1 1 calc R . . C214 C -0.9553(4) 0.3263(3) -0.3155(3) 0.0464(19) Uani 1 1 d . . . H21E H -0.9577 0.3296 -0.2694 0.056 Uiso 1 1 calc R . . C209 C -0.8854(4) 0.2908(3) -0.3271(3) 0.0383(17) Uani 1 1 d . . . C210 C -0.8799(4) 0.2857(3) -0.3948(3) 0.0355(17) Uani 1 1 d . . . H21F H -0.8327 0.2627 -0.4030 0.043 Uiso 1 1 calc R . . C211 C -0.9473(4) 0.3161(3) -0.4509(3) 0.0448(19) Uani 1 1 d . . . H21G H -0.9454 0.3126 -0.4972 0.054 Uiso 1 1 calc R . . C208 C -0.8160(4) 0.2616(3) -0.2646(3) 0.0437(19) Uani 1 1 d . . . C207 C -0.5921(5) 0.2060(4) -0.2069(3) 0.050(2) Uani 1 1 d . . . H20C H -0.5920 0.1958 -0.2534 0.060 Uiso 1 1 calc R . . C206 C -0.5104(4) 0.1923(4) -0.1449(3) 0.052(2) Uani 1 1 d . . . C201 C -0.4906(4) 0.2225(4) -0.0713(3) 0.0474(19) Uani 1 1 d . . . C202 C -0.4085(5) 0.2057(4) -0.0172(3) 0.072(3) Uani 1 1 d . . . H20D H -0.3950 0.2231 0.0317 0.087 Uiso 1 1 calc R . . C203 C -0.3467(6) 0.1647(5) -0.0326(4) 0.111(3) Uani 1 1 d . . . H20E H -0.2923 0.1557 0.0057 0.134 Uiso 1 1 calc R . . C204 C -0.3634(6) 0.1368(5) -0.1030(4) 0.114(3) Uani 1 1 d . . . H20F H -0.3213 0.1088 -0.1132 0.136 Uiso 1 1 calc R . . C205 C -0.4457(5) 0.1515(5) -0.1597(4) 0.083(3) Uani 1 1 d . . . H20G H -0.4576 0.1336 -0.2081 0.100 Uiso 1 1 calc R . . N501 N -0.9538(4) 0.8877(3) -0.6459(2) 0.0563(17) Uani 1 1 d . . . O501 O -0.9395(3) 0.8953(3) -0.5277(2) 0.0608(15) Uani 1 1 d . . . C503 C -0.9250(5) 0.8680(4) -0.5805(3) 0.059(2) Uani 1 1 d . . . H50A H -0.8890 0.8287 -0.5727 0.071 Uiso 1 1 calc R . . C502 C -1.0056(6) 0.9509(4) -0.6620(4) 0.082(3) Uani 1 1 d . . . H50B H -1.0147 0.9708 -0.6192 0.123 Uiso 1 1 calc R . . H50C H -1.0676 0.9329 -0.7017 0.123 Uiso 1 1 calc R . . H50D H -0.9690 0.9911 -0.6757 0.123 Uiso 1 1 calc R . . C501 C -0.9325(5) 0.8499(4) -0.7044(3) 0.070(3) Uani 1 1 d . . . H50E H -0.8973 0.8096 -0.6868 0.106 Uiso 1 1 calc R . . H50F H -0.8941 0.8872 -0.7197 0.106 Uiso 1 1 calc R . . H50G H -0.9921 0.8282 -0.7454 0.106 Uiso 1 1 calc R . . C403 C -0.6929(9) 0.0448(7) 0.0619(5) 0.116(5) Uani 0.75 1 d P . . H40A H -0.7209 0.0468 0.0117 0.139 Uiso 0.75 1 calc PR . . C402 C -0.5233(8) 0.0876(8) 0.0605(6) 0.147(5) Uani 0.75 1 d P . . H40B H -0.5612 0.0863 0.0091 0.220 Uiso 0.75 1 calc PR . . H40C H -0.4763 0.0549 0.0666 0.220 Uiso 0.75 1 calc PR . . H40D H -0.4908 0.1397 0.0820 0.220 Uiso 0.75 1 calc PR . . C401 C -0.5337(10) 0.0607(8) 0.1784(6) 0.152(6) Uani 0.75 1 d P . . H40E H -0.4649 0.0729 0.1923 0.228 Uiso 0.75 1 calc PR . . H40F H -0.5507 0.0106 0.1902 0.228 Uiso 0.75 1 calc PR . . H40G H -0.5530 0.0987 0.2046 0.228 Uiso 0.75 1 calc PR . . O401 O -0.7473(7) 0.0297(6) 0.0899(4) 0.139(4) Uani 0.75 1 d P . . N401 N -0.5856(8) 0.0609(5) 0.0959(4) 0.113(4) Uani 0.75 1 d P . . C1 C -0.3800(6) 0.3845(5) -0.0989(5) 0.111(3) Uani 1 1 d . . . O1 O -0.4444(3) 0.4049(2) -0.0682(2) 0.0595(14) Uani 1 1 d . . . C2 C -1.2501(8) 0.3491(5) -0.3097(5) 0.117(4) Uani 1 1 d . . . O2 O -1.2102(4) 0.4109(3) -0.3385(3) 0.095(2) Uani 1 1 d . . . C3 C -1.4405(7) 0.6495(5) -0.6662(4) 0.117(4) Uani 1 1 d . . . O3 O -1.3589(3) 0.7075(3) -0.6415(2) 0.0599(14) Uani 1 1 d . . . C4 C -1.4069(5) 0.5204(5) -0.3612(4) 0.080(3) Uani 1 1 d . . . O4 O -1.3623(3) 0.4916(3) -0.4057(2) 0.0677(16) Uani 1 1 d . . . O1W O -0.8942(4) 0.1061(3) 0.0834(3) 0.102(2) Uani 1 1 d . . . O2W O -1.0353(6) 0.1556(5) -0.0082(4) 0.108(3) Uani 0.62 1 d P . . O3W O -1.1031(18) 0.3052(15) 0.0944(10) 0.129(10) Uani 0.25 1 d P . . O4W O -1.027(3) 0.473(2) 0.2386(17) 0.076(10) Uani 0.13 1 d PU . . 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 Ce2 0.0389(2) 0.0434(2) 0.03736(15) 0.00156(14) 0.01683(14) 0.00800(17) Ce1 0.0411(2) 0.0511(2) 0.03925(16) 0.00581(15) 0.01870(14) 0.01259(18) O103 0.042(2) 0.069(3) 0.079(2) 0.035(2) 0.0357(19) 0.028(2) O105 0.049(2) 0.057(3) 0.0357(17) 0.0047(16) 0.0256(16) 0.012(2) O104 0.053(2) 0.048(2) 0.0345(17) 0.0095(16) 0.0208(16) 0.015(2) O102 0.036(2) 0.068(3) 0.052(2) 0.0085(19) 0.0243(17) 0.020(2) O101 0.043(2) 0.061(3) 0.048(2) 0.0049(19) 0.0165(18) 0.010(2) O303 0.047(3) 0.087(3) 0.080(2) 0.042(2) 0.035(2) 0.035(2) O305 0.043(2) 0.047(2) 0.0400(18) 0.0093(17) 0.0135(17) 0.008(2) O304 0.048(2) 0.048(3) 0.0380(18) 0.0015(17) 0.0176(17) 0.012(2) O302 0.042(2) 0.048(3) 0.0479(19) -0.0002(17) 0.0214(17) 0.009(2) O301 0.066(3) 0.063(3) 0.0394(19) 0.0107(18) 0.0220(18) 0.019(2) O203 0.047(3) 0.059(3) 0.0419(19) 0.0059(18) 0.0088(18) 0.022(2) O205 0.035(2) 0.057(3) 0.059(2) -0.0067(19) 0.0246(17) 0.015(2) O204 0.037(2) 0.037(2) 0.0434(19) 0.0029(16) 0.0122(17) 0.0092(19) O202 0.040(2) 0.060(3) 0.0432(19) 0.0046(18) 0.0192(17) 0.007(2) O201 0.031(2) 0.065(3) 0.054(2) -0.0010(19) 0.0165(18) 0.017(2) N304 0.036(3) 0.042(3) 0.040(2) 0.006(2) 0.015(2) 0.011(2) N104 0.044(3) 0.042(3) 0.050(2) 0.006(2) 0.019(2) 0.023(2) N103 0.061(3) 0.039(3) 0.036(2) 0.000(2) 0.016(2) 0.013(3) N102 0.037(3) 0.073(4) 0.082(3) 0.028(3) 0.034(2) 0.025(3) N101 0.045(3) 0.048(3) 0.055(3) 0.012(2) 0.023(2) 0.011(3) N303 0.031(3) 0.056(3) 0.048(2) 0.010(2) 0.023(2) 0.007(2) N302 0.038(3) 0.052(3) 0.046(2) -0.003(2) 0.011(2) 0.011(3) N301 0.039(3) 0.050(3) 0.046(2) 0.013(2) 0.015(2) 0.022(2) N204 0.040(3) 0.043(3) 0.048(2) 0.002(2) 0.029(2) 0.011(2) N203 0.054(3) 0.040(3) 0.048(2) -0.001(2) 0.022(2) 0.009(3) N202 0.054(3) 0.051(3) 0.031(2) 0.003(2) 0.013(2) 0.015(3) N201 0.033(3) 0.051(3) 0.033(2) 0.001(2) 0.0129(19) 0.012(2) C123 0.034(3) 0.050(4) 0.051(3) 0.003(3) 0.017(3) 0.010(3) C128 0.029(3) 0.050(4) 0.047(3) 0.005(3) 0.016(2) 0.006(3) C127 0.047(4) 0.044(4) 0.052(3) -0.003(3) 0.019(3) 0.006(3) C126 0.049(4) 0.060(5) 0.079(4) 0.019(3) 0.029(3) 0.014(4) C125 0.070(4) 0.058(4) 0.083(4) 0.003(3) 0.047(3) 0.032(4) C124 0.074(4) 0.050(4) 0.075(4) 0.005(3) 0.048(3) 0.026(4) C122 0.039(3) 0.057(4) 0.040(3) 0.005(3) 0.018(2) 0.016(3) C121 0.042(4) 0.053(4) 0.052(3) -0.002(3) 0.027(3) 0.002(3) C118 0.034(3) 0.056(4) 0.028(3) 0.007(3) 0.005(2) 0.008(3) C119 0.070(5) 0.066(5) 0.032(3) -0.008(3) 0.021(3) 0.004(4) C120 0.068(5) 0.060(4) 0.042(3) 0.008(3) 0.013(3) 0.024(4) C115 0.028(3) 0.051(4) 0.065(3) 0.010(3) 0.016(3) 0.019(3) C116 0.046(4) 0.064(4) 0.042(3) 0.015(3) 0.023(3) 0.020(3) C117 0.038(4) 0.058(4) 0.042(3) 0.000(3) 0.018(3) 0.009(3) C112 0.044(4) 0.075(5) 0.051(3) 0.023(3) 0.023(3) 0.030(4) C113 0.040(4) 0.058(4) 0.070(4) 0.013(3) 0.025(3) 0.012(3) C114 0.028(3) 0.059(4) 0.066(3) 0.016(3) 0.022(3) 0.020(3) C109 0.047(4) 0.044(4) 0.045(3) 0.012(3) 0.018(3) 0.015(3) C110 0.046(4) 0.053(4) 0.085(4) 0.027(3) 0.030(3) 0.022(3) C111 0.050(4) 0.052(4) 0.082(4) 0.022(3) 0.032(3) 0.006(4) C108 0.063(4) 0.046(4) 0.048(3) 0.016(3) 0.030(3) 0.022(4) C107 0.034(4) 0.060(4) 0.072(3) 0.020(3) 0.028(3) -0.005(3) C106 0.056(4) 0.052(4) 0.041(3) 0.010(3) 0.012(3) 0.020(4) C101 0.068(4) 0.058(4) 0.040(3) 0.006(3) 0.020(3) 0.034(4) C102 0.087(5) 0.070(5) 0.076(4) 0.001(4) 0.046(4) 0.025(4) C103 0.094(6) 0.065(5) 0.095(5) -0.007(4) 0.035(4) 0.023(5) C104 0.108(7) 0.055(5) 0.084(5) -0.010(4) 0.033(5) 0.014(5) C105 0.063(5) 0.072(5) 0.057(4) 0.009(3) 0.018(3) 0.011(4) C323 0.039(4) 0.041(4) 0.049(3) -0.007(3) 0.018(3) 0.007(3) C328 0.031(3) 0.046(4) 0.054(3) -0.015(3) 0.010(3) 0.006(3) C327 0.026(3) 0.072(5) 0.050(3) -0.003(3) 0.006(3) 0.016(3) C326 0.053(4) 0.061(4) 0.051(3) 0.008(3) 0.005(3) 0.025(4) C325 0.059(4) 0.052(4) 0.061(4) 0.019(3) 0.009(3) 0.025(4) C324 0.045(4) 0.047(4) 0.069(4) 0.010(3) 0.025(3) 0.013(3) C322 0.036(3) 0.040(4) 0.056(3) 0.008(3) 0.019(3) 0.010(3) C321 0.045(4) 0.032(3) 0.042(3) 0.002(2) 0.019(3) 0.009(3) C318 0.035(3) 0.055(4) 0.035(3) 0.006(2) 0.019(2) 0.008(3) C319 0.032(3) 0.057(4) 0.045(3) 0.000(3) 0.021(2) 0.007(3) C320 0.046(4) 0.071(5) 0.048(3) 0.020(3) 0.022(3) 0.017(4) C315 0.037(4) 0.052(4) 0.049(3) 0.011(3) 0.014(3) 0.009(3) C316 0.040(4) 0.037(4) 0.062(3) 0.007(3) 0.023(3) 0.006(3) C317 0.055(4) 0.052(4) 0.039(3) 0.019(3) 0.014(3) 0.020(3) C312 0.036(4) 0.060(4) 0.057(3) 0.026(3) 0.019(3) 0.015(3) C313 0.080(5) 0.045(4) 0.063(3) 0.011(3) 0.035(3) 0.013(4) C314 0.072(4) 0.059(4) 0.050(3) -0.003(3) 0.030(3) 0.019(4) C309 0.024(3) 0.042(4) 0.055(3) 0.000(3) 0.015(3) 0.014(3) C310 0.073(5) 0.059(5) 0.052(3) 0.011(3) 0.019(3) 0.007(4) C311 0.061(5) 0.070(5) 0.060(4) 0.018(4) 0.013(3) 0.010(4) C308 0.009(3) 0.064(4) 0.047(3) 0.003(3) 0.006(2) 0.006(3) C307 0.042(4) 0.061(4) 0.044(3) 0.012(3) 0.016(3) 0.017(3) C306 0.039(3) 0.085(5) 0.045(3) 0.009(3) 0.021(3) 0.032(3) C301 0.042(3) 0.074(5) 0.051(3) 0.021(3) 0.026(3) 0.033(3) C302 0.061(4) 0.081(5) 0.047(3) 0.011(3) 0.024(3) 0.007(4) C303 0.081(5) 0.112(6) 0.049(3) 0.024(4) 0.023(3) 0.032(5) C304 0.064(5) 0.131(7) 0.036(3) -0.003(4) 0.011(3) 0.025(5) C305 0.056(5) 0.103(6) 0.049(3) 0.000(4) 0.017(3) 0.019(4) C223 0.022(3) 0.053(4) 0.046(3) 0.006(3) 0.018(2) 0.008(3) C228 0.040(3) 0.058(4) 0.033(3) 0.013(3) 0.016(2) 0.012(3) C227 0.040(4) 0.057(4) 0.043(3) 0.005(3) 0.023(3) 0.009(3) C226 0.040(4) 0.061(4) 0.058(3) 0.013(3) 0.022(3) 0.021(3) C225 0.037(4) 0.073(5) 0.064(4) 0.014(3) 0.018(3) 0.011(4) C224 0.031(3) 0.059(4) 0.059(3) 0.003(3) 0.023(3) 0.012(3) C222 0.035(4) 0.052(4) 0.045(3) 0.011(3) 0.016(3) 0.006(3) C221 0.042(4) 0.045(4) 0.032(3) 0.000(2) 0.013(2) 0.005(3) C218 0.036(3) 0.038(3) 0.038(3) 0.007(2) 0.013(2) 0.012(3) C219 0.057(4) 0.035(4) 0.041(3) -0.002(2) 0.020(3) 0.005(3) C220 0.037(4) 0.046(4) 0.037(3) 0.000(3) 0.004(3) 0.008(3) C215 0.056(4) 0.049(4) 0.043(3) 0.013(3) 0.021(3) 0.028(3) C216 0.050(4) 0.047(4) 0.045(3) 0.000(3) 0.014(3) 0.016(3) C217 0.038(4) 0.042(4) 0.043(3) 0.002(3) 0.010(3) 0.011(3) C212 0.034(3) 0.043(4) 0.050(3) 0.004(3) 0.015(3) 0.021(3) C213 0.048(4) 0.058(4) 0.051(3) 0.012(3) 0.021(3) 0.014(3) C214 0.050(4) 0.048(4) 0.048(3) 0.013(3) 0.025(3) 0.011(3) C209 0.038(3) 0.042(4) 0.033(3) 0.003(2) 0.011(2) 0.008(3) C210 0.020(3) 0.044(4) 0.042(3) 0.004(2) 0.011(2) 0.009(3) C211 0.046(4) 0.037(4) 0.041(3) -0.006(3) 0.010(3) 0.003(3) C208 0.031(3) 0.046(4) 0.047(3) 0.002(3) 0.012(3) -0.004(3) C207 0.059(4) 0.056(4) 0.043(3) 0.003(3) 0.029(3) 0.011(4) C206 0.043(4) 0.068(4) 0.047(3) 0.008(3) 0.013(3) 0.026(3) C201 0.040(4) 0.059(4) 0.043(3) 0.005(3) 0.014(3) 0.018(3) C202 0.063(5) 0.096(6) 0.050(4) -0.010(4) 0.010(3) 0.036(4) C203 0.093(5) 0.177(8) 0.060(4) -0.004(5) 0.006(4) 0.096(5) C204 0.094(5) 0.172(8) 0.069(5) -0.013(5) 0.006(4) 0.098(5) C205 0.065(5) 0.122(7) 0.067(4) 0.001(4) 0.021(4) 0.054(5) N501 0.039(3) 0.080(4) 0.050(3) 0.012(3) 0.020(2) 0.005(3) O501 0.049(3) 0.085(3) 0.051(2) 0.013(2) 0.0225(19) 0.011(2) C503 0.038(4) 0.073(5) 0.061(4) 0.006(3) 0.018(3) 0.002(4) C502 0.082(6) 0.084(6) 0.075(4) 0.025(4) 0.023(4) 0.014(5) C501 0.049(4) 0.095(6) 0.058(4) -0.001(4) 0.021(3) -0.009(4) C403 0.131(10) 0.108(9) 0.052(6) -0.019(6) -0.033(6) 0.062(8) C402 0.142(9) 0.254(15) 0.132(7) 0.107(8) 0.109(6) 0.108(9) C401 0.185(12) 0.215(13) 0.076(7) 0.054(8) 0.033(8) 0.136(10) O401 0.209(8) 0.152(8) 0.106(5) 0.033(5) 0.109(5) 0.055(7) N401 0.185(9) 0.108(7) 0.074(5) 0.027(4) 0.054(5) 0.100(6) C1 0.092(5) 0.093(7) 0.190(7) -0.006(5) 0.109(5) 0.008(5) O1 0.048(3) 0.059(3) 0.070(2) -0.004(2) 0.025(2) 0.010(2) C2 0.151(9) 0.106(7) 0.096(5) 0.035(5) 0.047(6) 0.025(7) O2 0.085(4) 0.106(4) 0.083(3) -0.011(3) 0.023(3) 0.030(3) C3 0.129(8) 0.111(7) 0.075(5) -0.009(5) 0.032(5) -0.051(6) O3 0.058(3) 0.066(3) 0.059(2) 0.004(2) 0.029(2) 0.008(2) C4 0.072(5) 0.085(6) 0.113(5) 0.029(4) 0.062(4) 0.030(4) O4 0.062(3) 0.058(3) 0.085(3) 0.010(2) 0.032(2) 0.009(3) O1W 0.123(5) 0.096(4) 0.068(3) -0.006(3) 0.025(3) 0.012(4) O2W 0.120(6) 0.132(7) 0.124(5) 0.067(5) 0.079(5) 0.073(6) O3W 0.16(2) 0.16(2) 0.065(11) -0.005(12) 0.065(12) -0.038(18) O4W 0.081(15) 0.084(15) 0.065(12) 0.015(11) 0.042(10) -0.014(12) _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 Ce2 O205 2.192(4) . ? Ce2 O105 2.196(4) . ? Ce2 O305 2.244(3) . ? Ce2 O204 2.392(4) . ? Ce2 O104 2.439(3) . ? Ce2 O304 2.497(4) . ? Ce2 N204 2.597(4) . ? Ce2 N104 2.637(4) . ? Ce2 N304 2.643(5) . ? Ce1 O101 2.140(4) . ? Ce1 O301 2.190(4) . ? Ce1 O201 2.286(4) . ? Ce1 O102 2.305(4) . ? Ce1 O302 2.462(4) . ? Ce1 O202 2.485(3) . ? Ce1 N101 2.603(5) . ? Ce1 N301 2.667(4) . ? Ce1 N201 2.680(5) . ? O103 C112 1.381(8) . ? O103 C115 1.398(7) . ? O105 C128 1.320(7) . ? O104 C121 1.248(6) . ? O102 C108 1.274(7) . ? O101 C101 1.310(7) . ? O303 C315 1.369(8) . ? O303 C312 1.391(7) . ? O305 C328 1.334(7) . ? O304 C321 1.237(7) . ? O302 C308 1.251(7) . ? O301 C301 1.296(6) . ? O203 C212 1.379(6) . ? O203 C215 1.420(7) . ? O205 C228 1.316(7) . ? O204 C221 1.278(7) . ? O202 C208 1.263(7) . ? O201 C201 1.303(8) . ? N304 C322 1.277(7) . ? N304 N303 1.397(6) . ? N104 C122 1.273(7) . ? N104 N103 1.399(6) . ? N103 C121 1.330(7) . ? N102 C108 1.307(8) . ? N102 N101 1.387(7) . ? N101 C107 1.298(7) . ? N303 C321 1.335(7) . ? N302 C308 1.336(7) . ? N302 N301 1.402(7) . ? N301 C307 1.273(6) . ? N204 C222 1.264(7) . ? N204 N203 1.409(7) . ? N203 C221 1.312(8) . ? N202 C208 1.345(8) . ? N202 N201 1.379(6) . ? N201 C207 1.272(8) . ? C123 C128 1.395(8) . ? C123 C122 1.418(8) . ? C123 C124 1.427(9) . ? C128 C127 1.412(8) . ? C127 C126 1.375(9) . ? C126 C125 1.405(9) . ? C125 C124 1.339(9) . ? C121 C118 1.479(8) . ? C118 C119 1.360(9) . ? C118 C117 1.408(8) . ? C119 C120 1.384(9) . ? C120 C115 1.367(9) . ? C115 C116 1.362(8) . ? C116 C117 1.365(8) . ? C112 C111 1.359(9) . ? C112 C113 1.407(9) . ? C113 C114 1.357(9) . ? C114 C109 1.376(8) . ? C109 C110 1.397(9) . ? C109 C108 1.440(9) . ? C110 C111 1.354(9) . ? C107 C106 1.395(9) . ? C106 C101 1.427(10) . ? C106 C105 1.435(9) . ? C101 C102 1.392(10) . ? C102 C103 1.397(10) . ? C103 C104 1.410(12) . ? C104 C105 1.370(11) . ? C323 C324 1.416(8) . ? C323 C328 1.440(9) . ? C323 C322 1.458(8) . ? C328 C327 1.386(8) . ? C327 C326 1.337(9) . ? C326 C325 1.378(10) . ? C325 C324 1.370(9) . ? C321 C318 1.446(8) . ? C318 C319 1.383(8) . ? C318 C317 1.397(9) . ? C319 C320 1.378(9) . ? C320 C315 1.386(9) . ? C315 C316 1.384(8) . ? C316 C317 1.368(8) . ? C312 C313 1.351(8) . ? C312 C311 1.364(9) . ? C313 C314 1.383(9) . ? C314 C309 1.397(8) . ? C309 C310 1.395(8) . ? C309 C308 1.480(8) . ? C310 C311 1.358(9) . ? C307 C306 1.393(9) . ? C306 C305 1.399(8) . ? C306 C301 1.453(9) . ? C301 C302 1.412(9) . ? C302 C303 1.392(8) . ? C303 C304 1.384(10) . ? C304 C305 1.399(10) . ? C223 C224 1.394(8) . ? C223 C228 1.398(8) . ? C223 C222 1.471(9) . ? C228 C227 1.406(9) . ? C227 C226 1.336(8) . ? C226 C225 1.391(8) . ? C225 C224 1.379(9) . ? C221 C218 1.478(9) . ? C218 C217 1.364(7) . ? C218 C219 1.378(8) . ? C219 C220 1.349(8) . ? C220 C215 1.364(7) . ? C215 C216 1.406(8) . ? C216 C217 1.360(8) . ? C212 C211 1.351(9) . ? C212 C213 1.404(8) . ? C213 C214 1.363(8) . ? C214 C209 1.387(9) . ? C209 C210 1.377(8) . ? C209 C208 1.476(8) . ? C210 C211 1.402(7) . ? C207 C206 1.444(8) . ? C206 C205 1.399(10) . ? C206 C201 1.420(8) . ? C201 C202 1.390(8) . ? C202 C203 1.370(11) . ? C203 C204 1.363(10) . ? C204 C205 1.401(10) . ? N501 C503 1.298(8) . ? N501 C502 1.443(9) . ? N501 C501 1.460(9) . ? O501 C503 1.229(8) . ? C403 O401 1.173(16) . ? C403 N401 1.480(16) . ? C402 N401 1.431(16) . ? C401 N401 1.528(12) . ? C1 O1 1.405(10) . ? C2 O2 1.438(11) . ? C3 O3 1.387(9) . ? C4 O4 1.408(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O205 Ce2 O105 81.17(15) . . ? O205 Ce2 O305 85.77(14) . . ? O105 Ce2 O305 83.35(13) . . ? O205 Ce2 O204 132.43(13) . . ? O105 Ce2 O204 143.96(14) . . ? O305 Ce2 O204 86.43(13) . . ? O205 Ce2 O104 88.58(14) . . ? O105 Ce2 O104 129.68(11) . . ? O305 Ce2 O104 145.09(12) . . ? O204 Ce2 O104 72.34(12) . . ? O205 Ce2 O304 143.96(12) . . ? O105 Ce2 O304 89.39(13) . . ? O305 Ce2 O304 127.79(14) . . ? O204 Ce2 O304 70.12(12) . . ? O104 Ce2 O304 70.98(12) . . ? O205 Ce2 N204 69.51(15) . . ? O105 Ce2 N204 145.05(14) . . ? O305 Ce2 N204 76.12(13) . . ? O204 Ce2 N204 63.06(14) . . ? O104 Ce2 N204 69.65(12) . . ? O304 Ce2 N204 125.53(14) . . ? O205 Ce2 N104 72.17(14) . . ? O105 Ce2 N104 68.21(14) . . ? O305 Ce2 N104 145.99(15) . . ? O204 Ce2 N104 127.56(13) . . ? O104 Ce2 N104 61.76(13) . . ? O304 Ce2 N104 72.03(14) . . ? N204 Ce2 N104 117.38(15) . . ? O205 Ce2 N304 143.40(15) . . ? O105 Ce2 N304 71.30(14) . . ? O305 Ce2 N304 67.85(13) . . ? O204 Ce2 N304 72.82(14) . . ? O104 Ce2 N304 127.57(14) . . ? O304 Ce2 N304 60.92(12) . . ? N204 Ce2 N304 123.81(14) . . ? N104 Ce2 N304 116.67(14) . . ? O101 Ce1 O301 88.83(15) . . ? O101 Ce1 O201 84.66(15) . . ? O301 Ce1 O201 85.57(15) . . ? O101 Ce1 O102 132.07(15) . . ? O301 Ce1 O102 86.03(15) . . ? O201 Ce1 O102 142.05(14) . . ? O101 Ce1 O302 138.37(14) . . ? O301 Ce1 O302 128.69(13) . . ? O201 Ce1 O302 81.62(14) . . ? O102 Ce1 O302 75.16(14) . . ? O101 Ce1 O202 90.03(13) . . ? O301 Ce1 O202 148.29(15) . . ? O201 Ce1 O202 125.85(14) . . ? O102 Ce1 O202 71.50(13) . . ? O302 Ce1 O202 67.59(12) . . ? O101 Ce1 N101 69.26(16) . . ? O301 Ce1 N101 82.65(15) . . ? O201 Ce1 N101 151.47(16) . . ? O102 Ce1 N101 62.82(15) . . ? O302 Ce1 N101 125.62(14) . . ? O202 Ce1 N101 67.41(14) . . ? O101 Ce1 N301 149.33(13) . . ? O301 Ce1 N301 67.53(15) . . ? O201 Ce1 N301 74.65(15) . . ? O102 Ce1 N301 67.94(14) . . ? O302 Ce1 N301 61.16(13) . . ? O202 Ce1 N301 120.42(13) . . ? N101 Ce1 N301 123.39(16) . . ? O101 Ce1 N201 72.51(15) . . ? O301 Ce1 N201 147.77(15) . . ? O201 Ce1 N201 67.11(13) . . ? O102 Ce1 N201 126.01(14) . . ? O302 Ce1 N201 65.93(14) . . ? O202 Ce1 N201 59.99(13) . . ? N101 Ce1 N201 113.17(14) . . ? N301 Ce1 N201 117.61(15) . . ? C112 O103 C115 117.8(5) . . ? C128 O105 Ce2 137.3(4) . . ? C121 O104 Ce2 125.2(4) . . ? C108 O102 Ce1 125.5(4) . . ? C101 O101 Ce1 150.2(4) . . ? C315 O303 C312 118.2(5) . . ? C328 O305 Ce2 132.5(3) . . ? C321 O304 Ce2 121.9(3) . . ? C308 O302 Ce1 125.4(4) . . ? C301 O301 Ce1 150.3(4) . . ? C212 O203 C215 120.1(4) . . ? C228 O205 Ce2 144.0(4) . . ? C221 O204 Ce2 121.7(4) . . ? C208 O202 Ce1 124.3(4) . . ? C201 O201 Ce1 134.0(3) . . ? C322 N304 N303 115.8(5) . . ? C322 N304 Ce2 130.2(4) . . ? N303 N304 Ce2 113.9(3) . . ? C122 N104 N103 116.7(5) . . ? C122 N104 Ce2 128.4(4) . . ? N103 N104 Ce2 114.2(3) . . ? C121 N103 N104 116.7(4) . . ? C108 N102 N101 114.2(5) . . ? C107 N101 N102 116.8(5) . . ? C107 N101 Ce1 128.5(5) . . ? N102 N101 Ce1 114.3(3) . . ? C321 N303 N304 117.0(5) . . ? C308 N302 N301 117.1(5) . . ? C307 N301 N302 114.6(5) . . ? C307 N301 Ce1 131.0(4) . . ? N302 N301 Ce1 114.2(3) . . ? C222 N204 N203 114.6(5) . . ? C222 N204 Ce2 131.1(4) . . ? N203 N204 Ce2 114.1(3) . . ? C221 N203 N204 114.5(5) . . ? C208 N202 N201 117.5(5) . . ? C207 N201 N202 116.6(5) . . ? C207 N201 Ce1 128.9(3) . . ? N202 N201 Ce1 114.5(4) . . ? C128 C123 C122 123.1(6) . . ? C128 C123 C124 118.7(6) . . ? C122 C123 C124 118.0(5) . . ? O105 C128 C123 121.9(5) . . ? O105 C128 C127 118.8(5) . . ? C123 C128 C127 119.2(6) . . ? C126 C127 C128 120.2(6) . . ? C127 C126 C125 120.4(6) . . ? C124 C125 C126 120.1(7) . . ? C125 C124 C123 121.3(6) . . ? N104 C122 C123 125.6(5) . . ? O104 C121 N103 121.2(6) . . ? O104 C121 C118 118.1(5) . . ? N103 C121 C118 120.7(5) . . ? C119 C118 C117 120.1(6) . . ? C119 C118 C121 116.8(5) . . ? C117 C118 C121 122.9(6) . . ? C118 C119 C120 119.8(6) . . ? C115 C120 C119 119.4(6) . . ? C116 C115 C120 121.6(6) . . ? C116 C115 O103 117.5(6) . . ? C120 C115 O103 120.8(6) . . ? C117 C116 C115 119.7(6) . . ? C116 C117 C118 119.4(6) . . ? C111 C112 O103 120.6(6) . . ? C111 C112 C113 119.4(7) . . ? O103 C112 C113 119.9(6) . . ? C114 C113 C112 118.3(6) . . ? C113 C114 C109 123.8(6) . . ? C114 C109 C110 115.8(6) . . ? C114 C109 C108 118.8(6) . . ? C110 C109 C108 125.4(6) . . ? C111 C110 C109 122.1(6) . . ? C112 C111 C110 120.6(7) . . ? O102 C108 N102 122.5(6) . . ? O102 C108 C109 121.0(6) . . ? N102 C108 C109 116.5(6) . . ? N101 C107 C106 128.4(6) . . ? C107 C106 C101 122.5(6) . . ? C107 C106 C105 119.2(7) . . ? C101 C106 C105 118.3(6) . . ? O101 C101 C102 123.0(7) . . ? O101 C101 C106 119.9(6) . . ? C102 C101 C106 117.1(6) . . ? C103 C102 C101 123.3(8) . . ? C102 C103 C104 119.9(8) . . ? C105 C104 C103 117.8(7) . . ? C104 C105 C106 123.2(8) . . ? C324 C323 C328 119.1(5) . . ? C324 C323 C322 117.2(6) . . ? C328 C323 C322 123.7(6) . . ? O305 C328 C327 123.2(6) . . ? O305 C328 C323 120.4(5) . . ? C327 C328 C323 116.3(6) . . ? C326 C327 C328 123.8(6) . . ? C327 C326 C325 120.5(6) . . ? C324 C325 C326 120.0(6) . . ? C325 C324 C323 120.3(6) . . ? N304 C322 C323 122.6(6) . . ? O304 C321 N303 120.3(5) . . ? O304 C321 C318 121.1(5) . . ? N303 C321 C318 118.5(6) . . ? C319 C318 C317 116.5(6) . . ? C319 C318 C321 117.7(6) . . ? C317 C318 C321 125.6(5) . . ? C320 C319 C318 122.1(6) . . ? C315 C320 C319 119.4(6) . . ? O303 C315 C320 124.3(6) . . ? O303 C315 C316 115.5(6) . . ? C320 C315 C316 120.1(6) . . ? C317 C316 C315 118.9(6) . . ? C316 C317 C318 122.9(6) . . ? C313 C312 C311 121.0(6) . . ? C313 C312 O303 118.5(6) . . ? C311 C312 O303 120.1(5) . . ? C312 C313 C314 119.0(6) . . ? C313 C314 C309 121.2(5) . . ? C310 C309 C314 117.5(6) . . ? C310 C309 C308 117.2(5) . . ? C314 C309 C308 125.3(5) . . ? C311 C310 C309 120.3(6) . . ? C310 C311 C312 120.9(6) . . ? O302 C308 N302 120.4(6) . . ? O302 C308 C309 119.5(5) . . ? N302 C308 C309 120.1(5) . . ? N301 C307 C306 127.2(6) . . ? C307 C306 C305 118.0(6) . . ? C307 C306 C301 121.6(5) . . ? C305 C306 C301 120.3(6) . . ? O301 C301 C302 121.2(6) . . ? O301 C301 C306 121.9(5) . . ? C302 C301 C306 116.9(5) . . ? C303 C302 C301 121.4(7) . . ? C304 C303 C302 120.9(7) . . ? C303 C304 C305 120.0(6) . . ? C306 C305 C304 120.3(7) . . ? C224 C223 C228 119.4(6) . . ? C224 C223 C222 117.4(5) . . ? C228 C223 C222 123.2(5) . . ? O205 C228 C223 121.4(6) . . ? O205 C228 C227 120.4(5) . . ? C223 C228 C227 118.1(5) . . ? C226 C227 C228 121.8(6) . . ? C227 C226 C225 120.6(7) . . ? C224 C225 C226 119.3(6) . . ? C225 C224 C223 120.7(6) . . ? N204 C222 C223 124.6(5) . . ? O204 C221 N203 123.7(6) . . ? O204 C221 C218 120.7(6) . . ? N203 C221 C218 115.6(5) . . ? C217 C218 C219 118.0(6) . . ? C217 C218 C221 122.9(5) . . ? C219 C218 C221 119.1(5) . . ? C220 C219 C218 122.5(5) . . ? C219 C220 C215 118.8(5) . . ? C220 C215 C216 120.7(6) . . ? C220 C215 O203 124.8(5) . . ? C216 C215 O203 114.4(5) . . ? C217 C216 C215 118.1(5) . . ? C216 C217 C218 122.0(5) . . ? C211 C212 O203 116.4(5) . . ? C211 C212 C213 121.3(5) . . ? O203 C212 C213 122.3(6) . . ? C214 C213 C212 117.6(6) . . ? C213 C214 C209 121.9(6) . . ? C214 C209 C210 120.2(5) . . ? C214 C209 C208 118.2(5) . . ? C210 C209 C208 121.6(6) . . ? C209 C210 C211 118.1(6) . . ? C212 C211 C210 120.9(6) . . ? O202 C208 N202 118.2(5) . . ? O202 C208 C209 121.4(6) . . ? N202 C208 C209 120.4(5) . . ? N201 C207 C206 124.2(5) . . ? C205 C206 C201 119.5(5) . . ? C205 C206 C207 117.5(6) . . ? C201 C206 C207 122.8(6) . . ? O201 C201 C202 120.8(5) . . ? O201 C201 C206 122.5(5) . . ? C202 C201 C206 116.6(6) . . ? C203 C202 C201 122.9(6) . . ? C204 C203 C202 121.2(7) . . ? C203 C204 C205 118.2(8) . . ? C206 C205 C204 121.5(7) . . ? C503 N501 C502 120.0(6) . . ? C503 N501 C501 122.4(6) . . ? C502 N501 C501 117.6(5) . . ? O501 C503 N501 127.7(7) . . ? O401 C403 N401 128.5(10) . . ? C402 N401 C403 125.7(9) . . ? C402 N401 C401 114.5(10) . . ? C403 N401 C401 119.2(10) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 2.019 _refine_diff_density_min -1.651 _refine_diff_density_rms 0.157 _database_code_depnum_ccdc_archive 'CCDC 947248' ####################################################################### # # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C177 H209 Ce2 N24 O38' _chemical_formula_weight 3560.92 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6649(8) _cell_length_b 18.3430(9) _cell_length_c 33.4669(15) _cell_angle_alpha 94.839(3) _cell_angle_beta 90.172(4) _cell_angle_gamma 93.138(3) _cell_volume 8956.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6734 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3718 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66763 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.1177 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 31380 _reflns_number_gt 20244 _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. all the non-hydrogen atoms were refined anisotropically. Several solvent DMF molecules were disordered with the s.o.f. being fixed at suitable value. Several solvent DMF molecules were restrained as idealized geometry, and thermal parameters on adjacent atoms of them were restrained to be similar. Except the water molecules and the solvent methanol, hydrogen atoms within the ligand backbones and the solvent DMF molecules were fixed geometrically at calculated distances and allowed to ride on the parent non-hydrogen atoms. ; _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^)+(0.1077P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31380 _refine_ls_number_parameters 2281 _refine_ls_number_restraints 358 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1939 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.968 _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 Ce1 Ce -0.263752(9) 0.765644(7) 0.670150(3) 0.02502(3) Uani 1 1 d . . . Ce2 Ce -0.148520(9) 0.705562(7) 1.344988(3) 0.02774(4) Uani 1 1 d . . . O305 O -0.24192(11) 0.64842(9) 1.28995(4) 0.0349(5) Uani 1 1 d . . . C101 C -0.10628(15) 0.81437(12) 0.60627(6) 0.0297(6) Uani 1 1 d . . . C104 C 0.00137(15) 0.91167(13) 0.56198(6) 0.0298(6) Uani 1 1 d . . . O101 O -0.15621(10) 0.76670(8) 0.62511(4) 0.0268(4) Uani 1 1 d . . . C246 C -0.15900(16) 0.52053(13) 1.46706(6) 0.0346(7) Uani 1 1 d . . . H24A H -0.1789 0.5183 1.4933 0.042 Uiso 1 1 calc R . . O102 O -0.26988(10) 0.83406(9) 0.73547(4) 0.0325(5) Uani 1 1 d . . . O105 O -0.18089(10) 0.79948(8) 1.30065(4) 0.0299(4) Uani 1 1 d . . . N304 N -0.32270(13) 0.72624(10) 1.34522(5) 0.0297(5) Uani 1 1 d . . . C301 C -0.36637(15) 0.90248(12) 0.63089(6) 0.0278(6) Uani 1 1 d . . . O203 O -0.07083(11) 0.58776(9) 0.87886(4) 0.0385(5) Uani 1 1 d . . . C314 C -0.36228(16) 0.65440(13) 0.79349(6) 0.0329(7) Uani 1 1 d . . . H31A H -0.3257 0.6282 0.7754 0.039 Uiso 1 1 calc R . . C310 C -0.45896(15) 0.88795(12) 0.63974(6) 0.0265(6) Uani 1 1 d . . . N302 N -0.46166(13) 0.77168(10) 0.72309(5) 0.0313(6) Uani 1 1 d . . . H30A H -0.5104 0.7859 0.7349 0.038 Uiso 1 1 calc R . . O302 O -0.35071(10) 0.69289(8) 0.71592(4) 0.0314(5) Uani 1 1 d . . . O106 O -0.02300(11) 0.69506(8) 1.38007(4) 0.0323(5) Uani 1 1 d . . . O206 O -0.20700(11) 0.62143(8) 1.38259(4) 0.0329(5) Uani 1 1 d . . . O306 O -0.18661(10) 0.77986(8) 1.39620(4) 0.0303(4) Uani 1 1 d . . . O205 O -0.05795(11) 0.68915(8) 1.28223(4) 0.0355(5) Uani 1 1 d . . . O301 O -0.30031(10) 0.86887(8) 0.64666(4) 0.0274(4) Uani 1 1 d . . . O201 O -0.34272(10) 0.70570(8) 0.62067(4) 0.0295(4) Uani 1 1 d . . . O202 O -0.15705(10) 0.71955(8) 0.71575(4) 0.0308(4) Uani 1 1 d . . . N102 N -0.12471(14) 0.87914(11) 0.73170(5) 0.0337(6) Uani 1 1 d . . . H10A H -0.0756 0.8988 0.7431 0.040 Uiso 1 1 calc R . . N201 N -0.22754(12) 0.62653(10) 0.66102(5) 0.0291(5) Uani 1 1 d . . . C341 C -0.50643(17) 0.78127(15) 1.43794(7) 0.0414(8) Uani 1 1 d . . . H34A H -0.5284 0.7635 1.4127 0.050 Uiso 1 1 calc R . . C139 C 0.05647(14) 0.80764(12) 1.40233(6) 0.0252(6) Uani 1 1 d . . . C304 C -0.50099(16) 0.98132(13) 0.59451(7) 0.0333(7) Uani 1 1 d . . . C311 C -0.48464(16) 0.84395(12) 0.67207(6) 0.0301(7) Uani 1 1 d . . . H31B H -0.5434 0.8472 0.6822 0.036 Uiso 1 1 calc R . . N202 N -0.18521(13) 0.60264(11) 0.69456(5) 0.0339(6) Uani 1 1 d . . . H20A H -0.1793 0.5568 0.6970 0.041 Uiso 1 1 calc R . . C102 C -0.09726(15) 0.80227(13) 0.56389(6) 0.0287(6) Uani 1 1 d . . . H10B H -0.1275 0.7615 0.5504 0.034 Uiso 1 1 calc R . . C140 C 0.11557(14) 0.84768(13) 1.43217(6) 0.0284(6) Uani 1 1 d . . . C201 C -0.34205(15) 0.65161(13) 0.59238(6) 0.0302(7) Uani 1 1 d . . . C138 C 0.03314(15) 0.84137(12) 1.36654(6) 0.0264(6) Uani 1 1 d . . . H13A H 0.0670 0.8834 1.3606 0.032 Uiso 1 1 calc R . . N103 N -0.04088(13) 0.85339(10) 1.30751(5) 0.0282(5) Uani 1 1 d . . . H10C H 0.0008 0.8844 1.3004 0.034 Uiso 1 1 calc R . . N301 N -0.43101(13) 0.80011(10) 0.68801(5) 0.0295(5) Uani 1 1 d . . . C239 C -0.10116(16) 0.52701(12) 1.38756(6) 0.0298(6) Uani 1 1 d . . . N104 N -0.03229(13) 0.81642(10) 1.34233(5) 0.0284(5) Uani 1 1 d . . . C337 C -0.31543(17) 0.67243(14) 1.28037(7) 0.0371(7) Uani 1 1 d . . . C109 C -0.00354(14) 0.92494(12) 0.60409(6) 0.0261(6) Uani 1 1 d . . . N203 N -0.06943(14) 0.56714(11) 1.28312(5) 0.0380(6) Uani 1 1 d . . . H20B H -0.0624 0.5239 1.2719 0.046 Uiso 1 1 calc R . . C240 C -0.06123(16) 0.47698(13) 1.41217(7) 0.0325(7) Uani 1 1 d . . . N204 N -0.08959(14) 0.57955(11) 1.32384(5) 0.0331(6) Uani 1 1 d . . . C103 C -0.04619(15) 0.84821(13) 0.54287(6) 0.0318(7) Uani 1 1 d . . . H10D H -0.0417 0.8385 0.5152 0.038 Uiso 1 1 calc R . . C209 C -0.31232(15) 0.52569(13) 0.56631(6) 0.0308(7) Uani 1 1 d . . . C108 C -0.19970(18) 0.86459(13) 0.75245(6) 0.0358(7) Uani 1 1 d . . . C248 C -0.16712(15) 0.57328(12) 1.40359(6) 0.0280(6) Uani 1 1 d . . . N101 N -0.13030(13) 0.86067(10) 0.69025(5) 0.0287(5) Uani 1 1 d . . . C347 C -0.22375(17) 0.80928(13) 1.46341(6) 0.0321(7) Uani 1 1 d . . . H34B H -0.1619 0.8134 1.4700 0.039 Uiso 1 1 calc R . . C309 C -0.52800(16) 0.92666(12) 0.62045(6) 0.0296(7) Uani 1 1 d . . . C105 C 0.05309(16) 0.96033(13) 0.53928(7) 0.0348(7) Uani 1 1 d . . . H10E H 0.0557 0.9513 0.5116 0.042 Uiso 1 1 calc R . . C147 C 0.05931(17) 0.70029(13) 1.44049(7) 0.0368(7) Uani 1 1 d . . . H14A H 0.0394 0.6521 1.4437 0.044 Uiso 1 1 calc R . . C345 C -0.38256(16) 0.81717(12) 1.48388(6) 0.0309(7) Uani 1 1 d . . . C216 C -0.08724(16) 0.60647(14) 0.84098(6) 0.0346(7) Uani 1 1 d . . . C313 C -0.42193(15) 0.70389(12) 0.77946(6) 0.0291(6) Uani 1 1 d . . . C111 C -0.06605(15) 0.88945(12) 0.66945(6) 0.0268(6) Uani 1 1 d . . . H11A H -0.0216 0.9207 0.6827 0.032 Uiso 1 1 calc R . . C339 C -0.34434(16) 0.77696(12) 1.41370(6) 0.0276(6) Uani 1 1 d . . . C302 C -0.34300(16) 0.95795(13) 0.60532(6) 0.0338(7) Uani 1 1 d . . . H30B H -0.2816 0.9689 0.6004 0.041 Uiso 1 1 calc R . . C148 C 0.02876(16) 0.73430(13) 1.40671(6) 0.0307(7) Uani 1 1 d . . . C237 C -0.06187(17) 0.62644(14) 1.26303(6) 0.0362(7) Uani 1 1 d . . . C340 C -0.41218(16) 0.78975(13) 1.44427(6) 0.0312(7) Uani 1 1 d . . . C247 C -0.19569(17) 0.56904(13) 1.44421(6) 0.0320(7) Uani 1 1 d . . . H24B H -0.2395 0.5997 1.4549 0.038 Uiso 1 1 calc R . . N303 N -0.36460(14) 0.71065(12) 1.30803(5) 0.0399(6) Uani 1 1 d . . . H30C H -0.4182 0.7244 1.3030 0.048 Uiso 1 1 calc R . . C348 C -0.25164(16) 0.78760(12) 1.42357(7) 0.0306(7) Uani 1 1 d . . . C346 C -0.28657(17) 0.82407(13) 1.49219(7) 0.0360(7) Uani 1 1 d . . . H34C H -0.2667 0.8392 1.5181 0.043 Uiso 1 1 calc R . . C134 C -0.12555(16) 0.86064(12) 1.24527(6) 0.0297(6) Uani 1 1 d . . . C110 C -0.06005(14) 0.87534(12) 0.62655(6) 0.0243(6) Uani 1 1 d . . . C141 C 0.14275(15) 0.92263(14) 1.43170(6) 0.0326(7) Uani 1 1 d . . . H14B H 0.1200 0.9493 1.4118 0.039 Uiso 1 1 calc R . . C213 C -0.12572(15) 0.63357(13) 0.76209(7) 0.0337(7) Uani 1 1 d . . . C312 C -0.62355(16) 0.91143(14) 0.62507(7) 0.0358(7) Uani 1 1 d . . . H30D H -0.6440 0.8750 0.6411 0.043 Uiso 1 1 calc R . . C204 C -0.36440(16) 0.53515(14) 0.53157(7) 0.0353(7) Uani 1 1 d . . . C112 C 0.04772(16) 0.98806(13) 0.62183(7) 0.0364(7) Uani 1 1 d . . . H10F H 0.0471 0.9981 0.6495 0.044 Uiso 1 1 calc R . . C210 C -0.30037(15) 0.58632(12) 0.59717(6) 0.0268(6) Uani 1 1 d . . . C234 C -0.05901(17) 0.61905(13) 1.21907(6) 0.0325(7) Uani 1 1 d . . . C211 C -0.25110(15) 0.57618(13) 0.63339(6) 0.0293(6) Uani 1 1 d . . . H21A H -0.2349 0.5289 0.6371 0.035 Uiso 1 1 calc R . . C241 C 0.01022(18) 0.43195(13) 1.39909(7) 0.0383(7) Uani 1 1 d . . . H24C H 0.0335 0.4353 1.3735 0.046 Uiso 1 1 calc R . . C315 C -0.35721(16) 0.64415(13) 0.83340(7) 0.0348(7) Uani 1 1 d . . . H31C H -0.3170 0.6112 0.8421 0.042 Uiso 1 1 calc R . . C146 C 0.11684(17) 0.73646(14) 1.46811(7) 0.0379(7) Uani 1 1 d . . . H14C H 0.1372 0.7120 1.4894 0.046 Uiso 1 1 calc R . . C308 C -0.41177(15) 0.72153(13) 0.73730(6) 0.0299(6) Uani 1 1 d . . . C215 C -0.08027(17) 0.67811(14) 0.82974(7) 0.0368(7) Uani 1 1 d . . . H21B H -0.0632 0.7171 0.8483 0.044 Uiso 1 1 calc R . . C208 C -0.15443(15) 0.65354(13) 0.72259(6) 0.0282(6) Uani 1 1 d . . . C142 C 0.20202(16) 0.95709(15) 1.46000(6) 0.0371(7) Uani 1 1 d . . . H14D H 0.2192 1.0064 1.4588 0.044 Uiso 1 1 calc R . . C113 C -0.19590(17) 0.88334(14) 0.79630(6) 0.0393(8) Uani 1 1 d . . . C107 C 0.09724(16) 1.03375(13) 0.59923(7) 0.0389(7) Uani 1 1 d . . . H10G H 0.1301 1.0743 0.6116 0.047 Uiso 1 1 calc R . . C143 C 0.23690(16) 0.91892(16) 1.49059(7) 0.0440(8) Uani 1 1 d . . . H14E H 0.2790 0.9420 1.5090 0.053 Uiso 1 1 calc R . . C244 C -0.05287(17) 0.42373(13) 1.47624(7) 0.0373(7) Uani 1 1 d . . . H24D H -0.0731 0.4211 1.5024 0.045 Uiso 1 1 calc R . . C214 C -0.09946(16) 0.68958(14) 0.79037(6) 0.0353(7) Uani 1 1 d . . . H21C H -0.0944 0.7372 0.7827 0.042 Uiso 1 1 calc R . . C238 C -0.07749(17) 0.52533(13) 1.34518(6) 0.0337(7) Uani 1 1 d . . . H23A H -0.0527 0.4835 1.3330 0.040 Uiso 1 1 calc R . . C217 C -0.11198(18) 0.54902(14) 0.81252(7) 0.0414(8) Uani 1 1 d . . . H21D H -0.1154 0.5011 0.8197 0.050 Uiso 1 1 calc R . . C305 C -0.56722(17) 1.01988(14) 0.57638(7) 0.0379(7) Uani 1 1 d . . . H30E H -0.5489 1.0565 0.5600 0.045 Uiso 1 1 calc R . . C243 C 0.01310(18) 0.37953(14) 1.46219(7) 0.0409(8) Uani 1 1 d . . . H24E H 0.0367 0.3464 1.4785 0.049 Uiso 1 1 calc R . . C106 C 0.09921(16) 1.02041(14) 0.55774(7) 0.0383(7) Uani 1 1 d . . . H10H H 0.1322 1.0527 0.5425 0.046 Uiso 1 1 calc R . . C334 C -0.34713(16) 0.66679(14) 1.23810(6) 0.0362(7) Uani 1 1 d . . . C212 C -0.27520(18) 0.45722(14) 0.56917(7) 0.0392(8) Uani 1 1 d . . . H20C H -0.2377 0.4504 0.5908 0.047 Uiso 1 1 calc R . . C344 C -0.44799(18) 0.83408(14) 1.51346(7) 0.0391(8) Uani 1 1 d . . . H34D H -0.4281 0.8515 1.5391 0.047 Uiso 1 1 calc R . . C332 C -0.32054(17) 0.61999(14) 1.16984(7) 0.0384(8) Uani 1 1 d . . . H33A H -0.2902 0.5889 1.1517 0.046 Uiso 1 1 calc R . . C245 C -0.09119(16) 0.47301(13) 1.45244(6) 0.0310(7) Uani 1 1 d . . . C137 C -0.11752(16) 0.83754(12) 1.28614(6) 0.0273(6) Uani 1 1 d . . . C203 C -0.39993(17) 0.60349(14) 0.52703(7) 0.0385(7) Uani 1 1 d . . . H20D H -0.4304 0.6105 0.5033 0.046 Uiso 1 1 calc R . . C242 C 0.04571(17) 0.38395(14) 1.42296(7) 0.0390(7) Uani 1 1 d . . . H24F H 0.0915 0.3541 1.4133 0.047 Uiso 1 1 calc R . . C338 C -0.37395(16) 0.75378(14) 1.37346(7) 0.0358(7) Uani 1 1 d . . . H33B H -0.4349 0.7590 1.3672 0.043 Uiso 1 1 calc R . . C144 C 0.20813(16) 0.84682(15) 1.49317(7) 0.0385(7) Uani 1 1 d . . . H14F H 0.2301 0.8217 1.5139 0.046 Uiso 1 1 calc R . . C218 C -0.13115(17) 0.56279(14) 0.77404(7) 0.0386(7) Uani 1 1 d . . . H21E H -0.1482 0.5239 0.7554 0.046 Uiso 1 1 calc R . . C343 C -0.53863(18) 0.82582(14) 1.50588(7) 0.0418(8) Uani 1 1 d . . . H34E H -0.5803 0.8383 1.5258 0.050 Uiso 1 1 calc R . . C333 C -0.30340(17) 0.61987(14) 1.21062(7) 0.0379(7) Uani 1 1 d . . . H33C H -0.2622 0.5880 1.2196 0.045 Uiso 1 1 calc R . . C235 C -0.06891(18) 0.55165(13) 1.19638(7) 0.0390(8) Uani 1 1 d . . . H23B H -0.0711 0.5085 1.2091 0.047 Uiso 1 1 calc R . . C318 C -0.47709(17) 0.74127(14) 0.80705(7) 0.0383(7) Uani 1 1 d . . . H31D H -0.5174 0.7741 0.7983 0.046 Uiso 1 1 calc R . . C145 C 0.14682(15) 0.81079(14) 1.46541(7) 0.0328(7) Uani 1 1 d . . . C202 C -0.39129(16) 0.66005(14) 0.55624(7) 0.0365(7) Uani 1 1 d . . . H20E H -0.4174 0.7041 0.5527 0.044 Uiso 1 1 calc R . . C306 C -0.65741(18) 1.00498(14) 0.58213(7) 0.0414(8) Uani 1 1 d . . . H30F H -0.7006 1.0315 0.5701 0.050 Uiso 1 1 calc R . . C233 C -0.05737(19) 0.68250(14) 1.19864(7) 0.0422(8) Uani 1 1 d . . . H23C H -0.0508 0.7281 1.2130 0.051 Uiso 1 1 calc R . . O204 O -0.08414(13) 0.61422(9) 1.09547(4) 0.0453(5) Uani 1 1 d . . . O303 O -0.39865(11) 0.67063(9) 0.90004(4) 0.0401(5) Uani 1 1 d . . . O304 O -0.40301(12) 0.67289(10) 1.11703(5) 0.0474(6) Uani 1 1 d . . . O103 O -0.19446(13) 0.92423(11) 0.91948(4) 0.0583(6) Uani 1 1 d . . . O104 O -0.15347(12) 0.89952(10) 1.12577(5) 0.0520(6) Uani 1 1 d . . . C115 C -0.25136(18) 0.85919(14) 0.86135(7) 0.0427(8) Uani 1 1 d . . . H11B H -0.2887 0.8312 0.8773 0.051 Uiso 1 1 calc R . . C232 C -0.06523(19) 0.67848(14) 1.15793(7) 0.0423(8) Uani 1 1 d . . . H23D H -0.0645 0.7213 1.1449 0.051 Uiso 1 1 calc R . . C317 C -0.47249(17) 0.73008(14) 0.84744(7) 0.0409(8) Uani 1 1 d . . . H31E H -0.5108 0.7548 0.8654 0.049 Uiso 1 1 calc R . . C231 C -0.07428(17) 0.61106(13) 1.13567(6) 0.0349(7) Uani 1 1 d . . . C303 C -0.40600(17) 0.99537(14) 0.58790(7) 0.0371(7) Uani 1 1 d . . . H30G H -0.3873 1.0312 0.5712 0.045 Uiso 1 1 calc R . . O01 O 0.30023(19) 0.73813(15) 0.55904(7) 0.0982(10) Uani 1 1 d . . . C206 C -0.34506(19) 0.40851(16) 0.50718(8) 0.0523(9) Uani 1 1 d . . . H20F H -0.3571 0.3692 0.4881 0.063 Uiso 1 1 calc R . . C331 C -0.38196(17) 0.66576(14) 1.15632(7) 0.0385(8) Uani 1 1 d . . . C236 C -0.07544(19) 0.54869(14) 1.15502(7) 0.0414(8) Uani 1 1 d . . . H23E H -0.0807 0.5034 1.1402 0.050 Uiso 1 1 calc R . . C316 C -0.41191(16) 0.68264(14) 0.86166(6) 0.0339(7) Uani 1 1 d . . . C114 C -0.25412(17) 0.84561(14) 0.82053(7) 0.0379(7) Uani 1 1 d . . . H11C H -0.2961 0.8102 0.8089 0.045 Uiso 1 1 calc R . . C120 C -0.11973(17) 0.95849(15) 0.98228(7) 0.0419(8) Uani 1 1 d . . . C324 C -0.46387(18) 0.62415(15) 1.02786(7) 0.0412(8) Uani 1 1 d . . . C205 C -0.37905(18) 0.47562(15) 0.50213(7) 0.0434(8) Uani 1 1 d . . . H20G H -0.4121 0.4819 0.4790 0.052 Uiso 1 1 calc R . . O11 O 0.27678(15) 0.80476(14) 0.69444(7) 0.0809(8) Uani 1 1 d . . . C307 C -0.68499(17) 0.94969(14) 0.60620(7) 0.0412(8) Uani 1 1 d . . . H30H H -0.7470 0.9387 0.6094 0.049 Uiso 1 1 calc R . . C133 C -0.19938(17) 0.83332(15) 1.22245(7) 0.0416(8) Uani 1 1 d . . . H13B H -0.2450 0.8051 1.2341 0.050 Uiso 1 1 calc R . . C121 C -0.07335(18) 0.90089(16) 0.99457(8) 0.0478(8) Uani 1 1 d . . . C119 C -0.1203(2) 0.97162(18) 0.93794(7) 0.0619(10) Uani 1 1 d . . . H11D H -0.1303 1.0226 0.9345 0.074 Uiso 1 1 calc R . . H11E H -0.0624 0.9596 0.9258 0.074 Uiso 1 1 calc R . . C226 C 0.0977(2) 0.66517(17) 0.96048(8) 0.0574(10) Uani 1 1 d . . . H22A H 0.1037 0.6524 0.9322 0.086 Uiso 1 1 calc R . . H22B H 0.1487 0.6485 0.9745 0.086 Uiso 1 1 calc R . . H22C H 0.0962 0.7174 0.9654 0.086 Uiso 1 1 calc R . . C322 C -0.32074(18) 0.70014(14) 1.02804(7) 0.0413(8) Uani 1 1 d . . . C125 C -0.16456(18) 1.00483(14) 1.00902(7) 0.0412(8) Uani 1 1 d . . . C323 C -0.38234(17) 0.65196(14) 1.04666(6) 0.0378(7) Uani 1 1 d . . . C222 C 0.00644(18) 0.60731(13) 1.01445(7) 0.0407(8) Uani 1 1 d . . . C336 C -0.42878(19) 0.71206(16) 1.18328(7) 0.0486(9) Uani 1 1 d . . . H33D H -0.4716 0.7423 1.1740 0.058 Uiso 1 1 calc R . . C219 C -0.0694(2) 0.64740(15) 0.91039(7) 0.0444(8) Uani 1 1 d . . . H21F H -0.1232 0.6754 0.9081 0.053 Uiso 1 1 calc R . . H21G H -0.0159 0.6800 0.9076 0.053 Uiso 1 1 calc R . . C330 C -0.35746(19) 0.62763(15) 1.08693(7) 0.0434(8) Uani 1 1 d . . . H33E H -0.3768 0.5765 1.0884 0.052 Uiso 1 1 calc R . . H33F H -0.2919 0.6330 1.0910 0.052 Uiso 1 1 calc R . . C325 C -0.48414(18) 0.64333(15) 0.98934(7) 0.0420(8) Uani 1 1 d . . . C124 C -0.15595(18) 0.99782(15) 1.05005(7) 0.0415(8) Uani 1 1 d . . . C223 C -0.07160(18) 0.56969(14) 1.02772(7) 0.0382(7) Uani 1 1 d . . . C131 C -0.14081(18) 0.89022(15) 1.16565(7) 0.0440(8) Uani 1 1 d . . . N11 N 0.13400(16) 0.75890(14) 0.67499(8) 0.0631(8) Uani 1 1 d . . . C116 C -0.19387(19) 0.91374(17) 0.87867(7) 0.0516(9) Uani 1 1 d . . . C132 C -0.20783(17) 0.84668(14) 1.18219(7) 0.0412(7) Uani 1 1 d . . . H13C H -0.2575 0.8267 1.1669 0.049 Uiso 1 1 calc R . . C329 C -0.57136(19) 0.61177(19) 0.96833(8) 0.0626(10) Uani 1 1 d . . . H32A H -0.5628 0.6091 0.9398 0.094 Uiso 1 1 calc R . . H32B H -0.6205 0.6427 0.9755 0.094 Uiso 1 1 calc R . . H32C H -0.5859 0.5635 0.9764 0.094 Uiso 1 1 calc R . . C221 C 0.01075(18) 0.62962(14) 0.97511(6) 0.0379(7) Uani 1 1 d . . . C135 C -0.06062(19) 0.90651(16) 1.22861(7) 0.0571(9) Uani 1 1 d . . . H13D H -0.0118 0.9274 1.2442 0.069 Uiso 1 1 calc R . . C224 C -0.14831(18) 0.55363(14) 1.00200(7) 0.0412(8) Uani 1 1 d . . . C320 C -0.42333(18) 0.69069(15) 0.97057(7) 0.0411(8) Uani 1 1 d . . . C220 C -0.06772(18) 0.61682(14) 0.95065(6) 0.0385(7) Uani 1 1 d . . . C207 C -0.29368(19) 0.40014(15) 0.54031(8) 0.0486(9) Uani 1 1 d . . . H20H H -0.2705 0.3548 0.5435 0.058 Uiso 1 1 calc R . . C122 C -0.06505(17) 0.89237(15) 1.03649(8) 0.0492(8) Uani 1 1 d . . . N01 N 0.35710(19) 0.66827(14) 0.60749(8) 0.0710(9) Uani 1 1 d . . . C227 C 0.0858(2) 0.62676(17) 1.04339(7) 0.0555(9) Uani 1 1 d . . . H22D H 0.0725 0.6070 1.0685 0.083 Uiso 1 1 calc R . . H22E H 0.0950 0.6791 1.0476 0.083 Uiso 1 1 calc R . . H22F H 0.1402 0.6064 1.0324 0.083 Uiso 1 1 calc R . . C342 C -0.56859(19) 0.79844(16) 1.46802(8) 0.0479(9) Uani 1 1 d . . . H34F H -0.6309 0.7915 1.4627 0.058 Uiso 1 1 calc R . . N21 N -0.45538(18) 0.53495(17) 0.35016(8) 0.0803(10) Uani 1 1 d . . . C230 C -0.0741(2) 0.54728(14) 1.06993(7) 0.0427(8) Uani 1 1 d . . . H23F H -0.1253 0.5126 1.0733 0.051 Uiso 1 1 calc R . . H23G H -0.0182 0.5248 1.0764 0.051 Uiso 1 1 calc R . . C225 C -0.14683(18) 0.57810(14) 0.96385(7) 0.0407(8) Uani 1 1 d . . . C319 C -0.44740(19) 0.71564(16) 0.93038(7) 0.0468(8) Uani 1 1 d . . . H31F H -0.5128 0.7093 0.9257 0.056 Uiso 1 1 calc R . . H31G H -0.4290 0.7670 0.9293 0.056 Uiso 1 1 calc R . . O21 O -0.37923(18) 0.49056(17) 0.29411(8) 0.1051(11) Uani 1 1 d . . . C335 C -0.41125(18) 0.71273(16) 1.22393(7) 0.0455(8) Uani 1 1 d . . . H33G H -0.4421 0.7438 1.2420 0.055 Uiso 1 1 calc R . . C321 C -0.34115(19) 0.71778(14) 0.98942(7) 0.0428(8) Uani 1 1 d . . . C13 C 0.1985(2) 0.7783(2) 0.70159(10) 0.0745(12) Uani 1 1 d . . . H13H H 0.1849 0.7719 0.7282 0.089 Uiso 1 1 calc R . . C327 C -0.2340(2) 0.73070(16) 1.04904(8) 0.0568(10) Uani 1 1 d . . . H32D H -0.2440 0.7364 1.0774 0.085 Uiso 1 1 calc R . . H32E H -0.2166 0.7775 1.0397 0.085 Uiso 1 1 calc R . . H32F H -0.1862 0.6977 1.0434 0.085 Uiso 1 1 calc R . . C23 C -0.3806(3) 0.5234(2) 0.32818(10) 0.0879(14) Uani 1 1 d . . . H23H H -0.3249 0.5414 0.3394 0.105 Uiso 1 1 calc R . . C118 C -0.1430(2) 0.94148(18) 0.81343(7) 0.0735(10) Uani 1 1 d . . . H11F H -0.1069 0.9694 0.7970 0.088 Uiso 1 1 calc R . . C229 C -0.22840(19) 0.56190(16) 0.93645(8) 0.0512(9) Uani 1 1 d . . . H22G H -0.2823 0.5781 0.9500 0.077 Uiso 1 1 calc R . . H22H H -0.2354 0.5101 0.9293 0.077 Uiso 1 1 calc R . . H22I H -0.2195 0.5872 0.9127 0.077 Uiso 1 1 calc R . . C228 C -0.2337(2) 0.51105(17) 1.01486(8) 0.0566(10) Uani 1 1 d . . . H22J H -0.2864 0.5380 1.0102 0.085 Uiso 1 1 calc R . . H22K H -0.2292 0.5040 1.0429 0.085 Uiso 1 1 calc R . . H22L H -0.2393 0.4643 0.9996 0.085 Uiso 1 1 calc R . . C123 C -0.10375(17) 0.94418(15) 1.06347(7) 0.0401(7) Uani 1 1 d . . . C328 C -0.5324(2) 0.57578(18) 1.04883(8) 0.0631(10) Uani 1 1 d . . . H32G H -0.5171 0.5775 1.0768 0.095 Uiso 1 1 calc R . . H32H H -0.5311 0.5262 1.0371 0.095 Uiso 1 1 calc R . . H32I H -0.5925 0.5930 1.0458 0.095 Uiso 1 1 calc R . . C136 C -0.0682(2) 0.92141(18) 1.18876(8) 0.0739(10) Uani 1 1 d . . . H13E H -0.0246 0.9523 1.1776 0.089 Uiso 1 1 calc R . . C03 C 0.3603(3) 0.72514(19) 0.58412(10) 0.0763(12) Uani 1 1 d . . . H03A H 0.4114 0.7575 0.5868 0.092 Uiso 1 1 calc R . . C117 C -0.1414(2) 0.95997(19) 0.85416(8) 0.0687(10) Uani 1 1 d . . . H11G H -0.1075 1.0011 0.8653 0.082 Uiso 1 1 calc R . . C126 C -0.0312(2) 0.8464(2) 0.96504(11) 0.0888(14) Uani 1 1 d . . . H12A H -0.0603 0.8469 0.9393 0.133 Uiso 1 1 calc R . . H12B H -0.0392 0.7983 0.9742 0.133 Uiso 1 1 calc R . . H12C H 0.0328 0.8592 0.9627 0.133 Uiso 1 1 calc R . . C130 C -0.08399(19) 0.94510(17) 1.10743(7) 0.0623(9) Uani 1 1 d . . . H13F H -0.0242 0.9267 1.1115 0.075 Uiso 1 1 calc R . . H13G H -0.0839 0.9949 1.1197 0.075 Uiso 1 1 calc R . . C128 C -0.2063(2) 1.05067(19) 1.07936(9) 0.0745(12) Uani 1 1 d . . . H12D H -0.2654 1.0583 1.0686 0.112 Uiso 1 1 calc R . . H12E H -0.1716 1.0967 1.0831 0.112 Uiso 1 1 calc R . . H12F H -0.2133 1.0300 1.1047 0.112 Uiso 1 1 calc R . . C129 C -0.2235(3) 1.06404(18) 0.99518(9) 0.0765(12) Uani 1 1 d . . . H12G H -0.2243 1.0615 0.9664 0.115 Uiso 1 1 calc R . . H12H H -0.1987 1.1114 1.0057 0.115 Uiso 1 1 calc R . . H12I H -0.2847 1.0565 1.0048 0.115 Uiso 1 1 calc R . . C326 C -0.2726(2) 0.76482(17) 0.96777(8) 0.0641(10) Uani 1 1 d . . . H32J H -0.2818 0.7555 0.9393 0.096 Uiso 1 1 calc R . . H32K H -0.2118 0.7532 0.9747 0.096 Uiso 1 1 calc R . . H32L H -0.2809 0.8156 0.9756 0.096 Uiso 1 1 calc R . . C127 C -0.0133(2) 0.82966(19) 1.04976(12) 0.0913(14) Uani 1 1 d . . . H12J H -0.0268 0.8231 1.0773 0.137 Uiso 1 1 calc R . . H12K H 0.0511 0.8404 1.0470 0.137 Uiso 1 1 calc R . . H12L H -0.0312 0.7856 1.0334 0.137 Uiso 1 1 calc R . . C22 C -0.4531(3) 0.5725(2) 0.38927(13) 0.1156(18) Uani 1 1 d . . . H22M H -0.3911 0.5877 0.3965 0.173 Uiso 1 1 calc R . . H22N H -0.4777 0.5403 0.4082 0.173 Uiso 1 1 calc R . . H22O H -0.4889 0.6148 0.3894 0.173 Uiso 1 1 calc R . . C02 C 0.2817(3) 0.6165(2) 0.60627(12) 0.1012(15) Uani 1 1 d . . . H02A H 0.2386 0.6280 0.5864 0.152 Uiso 1 1 calc R . . H02B H 0.2530 0.6182 0.6320 0.152 Uiso 1 1 calc R . . H02C H 0.3024 0.5683 0.5995 0.152 Uiso 1 1 calc R . . C21 C -0.5435(2) 0.5067(3) 0.33371(12) 0.137(2) Uani 1 1 d . . . H21H H -0.5352 0.4827 0.3075 0.205 Uiso 1 1 calc R . . H21I H -0.5828 0.5464 0.3319 0.205 Uiso 1 1 calc R . . H21J H -0.5706 0.4722 0.3509 0.205 Uiso 1 1 calc R . . C01 C 0.4278(3) 0.6582(2) 0.63559(12) 0.1011(16) Uani 1 1 d . . . H01A H 0.4753 0.6960 0.6341 0.152 Uiso 1 1 calc R . . H01B H 0.4525 0.6112 0.6294 0.152 Uiso 1 1 calc R . . H01C H 0.4032 0.6606 0.6622 0.152 Uiso 1 1 calc R . . C12 C 0.1454(3) 0.7726(3) 0.63359(11) 0.1171(18) Uani 1 1 d . . . H12M H 0.2055 0.7945 0.6298 0.176 Uiso 1 1 calc R . . H12N H 0.1006 0.8054 0.6262 0.176 Uiso 1 1 calc R . . H12O H 0.1379 0.7273 0.6171 0.176 Uiso 1 1 calc R . . C11 C 0.0474(2) 0.72661(18) 0.68651(12) 0.0826(13) Uani 1 1 d . . . H11H H 0.0482 0.7206 0.7147 0.124 Uiso 1 1 calc R . . H11I H 0.0364 0.6797 0.6718 0.124 Uiso 1 1 calc R . . H11J H -0.0003 0.7580 0.6807 0.124 Uiso 1 1 calc R . . N401 N -0.3386(3) 0.2219(2) -0.34428(11) 0.0977(14) Uani 0.85 1 d PU . . O401 O -0.4448(2) 0.2924(2) -0.31720(10) 0.1033(13) Uani 0.85 1 d PU . . C403 C -0.4204(3) 0.2366(2) -0.31324(13) 0.1006(14) Uani 0.85 1 d PU . . H40A H -0.4433 0.2044 -0.2952 0.121 Uiso 0.85 1 calc PR . . C402 C -0.2985(4) 0.2773(3) -0.37045(15) 0.129(2) Uani 0.85 1 d PU . . H40B H -0.2511 0.2560 -0.3865 0.194 Uiso 0.85 1 calc PR . . H40C H -0.2734 0.3190 -0.3540 0.194 Uiso 0.85 1 calc PR . . H40D H -0.3452 0.2923 -0.3876 0.194 Uiso 0.85 1 calc PR . . C401 C -0.3007(4) 0.1546(3) -0.3506(2) 0.144(2) Uani 0.85 1 d PU . . H40E H -0.2537 0.1573 -0.3705 0.216 Uiso 0.85 1 calc PR . . H40F H -0.3472 0.1181 -0.3598 0.216 Uiso 0.85 1 calc PR . . H40G H -0.2748 0.1417 -0.3260 0.216 Uiso 0.85 1 calc PR . . N31 N -0.4425(2) 0.86765(19) 0.05782(11) 0.0842(13) Uani 0.85 1 d P . . O31 O -0.5791(3) 0.8074(2) 0.03468(11) 0.1305(16) Uani 0.85 1 d P . . C32 C -0.3804(3) 0.8690(3) 0.09074(16) 0.124(2) Uani 0.85 1 d P . . H32M H -0.4028 0.8352 0.1093 0.186 Uiso 0.85 1 calc PR . . H32N H -0.3749 0.9176 0.1040 0.186 Uiso 0.85 1 calc PR . . H32O H -0.3217 0.8552 0.0811 0.186 Uiso 0.85 1 calc PR . . C33 C -0.5151(3) 0.8168(3) 0.05965(15) 0.1129(19) Uani 0.85 1 d P . . H33H H -0.5165 0.7874 0.0810 0.136 Uiso 0.85 1 calc PR . . C31 C -0.4349(5) 0.9074(3) 0.02423(16) 0.164(3) Uani 0.85 1 d P . . H31H H -0.4863 0.8945 0.0067 0.247 Uiso 0.85 1 calc PR . . H31I H -0.3796 0.8961 0.0103 0.247 Uiso 0.85 1 calc PR . . H31J H -0.4335 0.9588 0.0325 0.247 Uiso 0.85 1 calc PR . . N41 N -0.1791(2) 0.34779(17) -0.28466(10) 0.0924(12) Uani 1 1 d . . . O41 O -0.1624(2) 0.45175(13) -0.31620(8) 0.1072(10) Uani 1 1 d . . . C42 C -0.1540(3) 0.2721(2) -0.28072(16) 0.140(2) Uani 1 1 d . . . H42A H -0.1086 0.2592 -0.3002 0.210 Uiso 1 1 calc R . . H42B H -0.2071 0.2394 -0.2851 0.210 Uiso 1 1 calc R . . H42C H -0.1301 0.2684 -0.2543 0.210 Uiso 1 1 calc R . . C43 C -0.1426(3) 0.3893(2) -0.31283(12) 0.0893(15) Uani 1 1 d . . . H43A H -0.1003 0.3688 -0.3305 0.107 Uiso 1 1 calc R . . C41 C -0.2487(3) 0.3783(3) -0.25714(16) 0.158(2) Uani 1 1 d . . . H41A H -0.2591 0.4275 -0.2631 0.236 Uiso 1 1 calc R . . H41B H -0.2274 0.3786 -0.2300 0.236 Uiso 1 1 calc R . . H41C H -0.3046 0.3486 -0.2605 0.236 Uiso 1 1 calc R . . N51 N 0.25279(18) 0.95898(15) 0.26447(7) 0.0694(9) Uani 1 1 d . . . O51 O 0.11867(13) 0.94153(11) 0.29632(5) 0.0571(6) Uani 1 1 d . . . C51 C 0.2272(3) 0.9063(3) 0.23007(11) 0.1245(19) Uani 1 1 d . . . H51A H 0.1657 0.8872 0.2333 0.187 Uiso 1 1 calc R . . H51B H 0.2678 0.8669 0.2287 0.187 Uiso 1 1 calc R . . H51C H 0.2314 0.9306 0.2058 0.187 Uiso 1 1 calc R . . C52 C 0.3449(2) 0.9963(2) 0.26539(12) 0.0965(15) Uani 1 1 d . . . H52A H 0.3517 1.0293 0.2892 0.145 Uiso 1 1 calc R . . H52B H 0.3525 1.0235 0.2422 0.145 Uiso 1 1 calc R . . H52C H 0.3903 0.9605 0.2653 0.145 Uiso 1 1 calc R . . C53 C 0.19721(19) 0.97050(16) 0.29405(8) 0.0509(9) Uani 1 1 d . . . H53A H 0.2176 1.0031 0.3154 0.061 Uiso 1 1 calc R . . N61 N -0.46289(18) 0.47767(16) -0.18484(8) 0.0725(9) Uani 1 1 d . . . O61 O -0.54928(19) 0.52764(15) -0.13495(7) 0.1042(10) Uani 1 1 d . . . C61 C -0.3956(3) 0.4497(3) -0.15970(12) 0.1163(18) Uani 1 1 d . . . H61A H -0.4104 0.4612 -0.1321 0.174 Uiso 1 1 calc R . . H61B H -0.3365 0.4717 -0.1651 0.174 Uiso 1 1 calc R . . H61C H -0.3948 0.3975 -0.1652 0.174 Uiso 1 1 calc R . . C62 C -0.4546(3) 0.4671(3) -0.22824(10) 0.1137(17) Uani 1 1 d . . . H62A H -0.5039 0.4895 -0.2406 0.171 Uiso 1 1 calc R . . H62B H -0.4571 0.4156 -0.2365 0.171 Uiso 1 1 calc R . . H62C H -0.3975 0.4892 -0.2362 0.171 Uiso 1 1 calc R . . C63 C -0.5330(2) 0.5146(2) -0.17095(11) 0.0810(13) Uani 1 1 d . . . H63A H -0.5724 0.5317 -0.1894 0.097 Uiso 1 1 calc R . . O71 O 0.11001(15) 0.57577(11) 0.73717(6) 0.0675(7) Uani 1 1 d U . . N71 N 0.22307(19) 0.63370(16) 0.77289(9) 0.0805(10) Uani 1 1 d U . . C71 C 0.3218(3) 0.6504(3) 0.77874(16) 0.132(2) Uani 1 1 d U . . H71A H 0.3542 0.6276 0.7566 0.198 Uiso 1 1 calc R . . H71B H 0.3411 0.6319 0.8032 0.198 Uiso 1 1 calc R . . H71C H 0.3343 0.7024 0.7802 0.198 Uiso 1 1 calc R . . C72 C 0.1613(3) 0.6664(3) 0.80474(13) 0.1300(18) Uani 1 1 d U . . H72A H 0.0990 0.6513 0.7982 0.195 Uiso 1 1 calc R . . H72B H 0.1688 0.7189 0.8061 0.195 Uiso 1 1 calc R . . H72C H 0.1769 0.6498 0.8302 0.195 Uiso 1 1 calc R . . C73 C 0.1901(2) 0.58817(18) 0.74324(9) 0.0639(10) Uani 1 1 d U . . H73A H 0.2310 0.5644 0.7261 0.077 Uiso 1 1 calc R . . N81 N -0.2216(3) 1.2408(2) -0.11906(12) 0.1030(13) Uani 0.80 1 d PU . . O81 O -0.1591(3) 1.1349(3) -0.11547(13) 0.1575(17) Uani 0.80 1 d PU . . C82 C -0.2867(4) 1.2909(4) -0.10346(18) 0.133(2) Uani 0.80 1 d PU . . H82A H -0.2878 1.3314 -0.1198 0.199 Uiso 0.80 1 calc PR . . H82B H -0.2699 1.3087 -0.0765 0.199 Uiso 0.80 1 calc PR . . H82C H -0.3462 1.2663 -0.1036 0.199 Uiso 0.80 1 calc PR . . C83 C -0.2138(4) 1.1809(3) -0.09802(18) 0.1197(16) Uani 0.80 1 d PU . . H83A H -0.2440 1.1738 -0.0741 0.144 Uiso 0.80 1 calc PR . . C81 C -0.1817(4) 1.2599(4) -0.15492(16) 0.142(2) Uani 0.80 1 d PU . . H81A H -0.1389 1.2243 -0.1638 0.213 Uiso 0.80 1 calc PR . . H81B H -0.1504 1.3073 -0.1506 0.213 Uiso 0.80 1 calc PR . . H81C H -0.2284 1.2613 -0.1750 0.213 Uiso 0.80 1 calc PR . . N91 N -0.5511(4) 1.0170(3) 0.12435(14) 0.0941(14) Uani 0.60 1 d PDU A . C93 C -0.4804(5) 1.0739(4) 0.1072(2) 0.1131(18) Uani 0.60 1 d PDU . . H93A H -0.4268 1.0967 0.1204 0.136 Uiso 0.60 1 d PR A . C92 C -0.5185(6) 1.0244(4) 0.1640(2) 0.131(3) Uani 0.60 1 d PU . . H92A H -0.5540 0.9919 0.1797 0.197 Uiso 0.60 1 calc PR A . H92B H -0.5237 1.0740 0.1750 0.197 Uiso 0.60 1 calc PR . . H92C H -0.4557 1.0123 0.1644 0.197 Uiso 0.60 1 calc PR . . C91 C -0.6181(5) 0.9694(4) 0.1142(2) 0.144(3) Uani 0.60 1 d PU . . H91A H -0.6395 0.9467 0.1374 0.216 Uiso 0.60 1 calc PR A . H91B H -0.5971 0.9327 0.0947 0.216 Uiso 0.60 1 calc PR . . H91C H -0.6670 0.9938 0.1028 0.216 Uiso 0.60 1 calc PR . . O91 O -0.5156(7) 1.0965(4) 0.0815(2) 0.125(3) Uani 0.25 1 d PDU A 1 O91' O -0.4957(7) 1.0735(5) 0.07456(16) 0.136(3) Uani 0.35 1 d PDU A 2 O411 O -0.1607(2) 1.02821(19) 0.29156(10) 0.1164(13) Uani 0.90 1 d PU . . N411 N -0.3095(3) 0.96684(19) 0.28439(10) 0.1057(14) Uani 0.90 1 d PDU . . C412 C -0.3645(4) 0.9172(3) 0.30650(15) 0.1205(19) Uani 0.90 1 d PU B . H41D H -0.3344 0.9105 0.3313 0.181 Uiso 0.90 1 calc PR . . H41E H -0.3731 0.8708 0.2910 0.181 Uiso 0.90 1 calc PR . . H41F H -0.4228 0.9371 0.3119 0.181 Uiso 0.90 1 calc PR . . C413 C -0.2303(4) 0.9943(3) 0.29991(17) 0.1343(18) Uani 0.90 1 d PU B . H41G H -0.2271 0.9839 0.3266 0.161 Uiso 0.90 1 calc PR . . C411 C -0.3743(6) 0.9659(5) 0.2499(2) 0.130(3) Uani 0.45 1 d PDU B 1 H41H H -0.3495 0.9971 0.2306 0.195 Uiso 0.45 1 calc PR B 1 H41I H -0.4316 0.9832 0.2593 0.195 Uiso 0.45 1 calc PR B 1 H41J H -0.3834 0.9168 0.2377 0.195 Uiso 0.45 1 calc PR B 1 C41' C -0.3034(7) 0.9953(4) 0.2460(2) 0.113(3) Uani 0.45 1 d PDU B 2 H41K H -0.2448 1.0202 0.2434 0.170 Uiso 0.45 1 calc PR B 2 H41L H -0.3505 1.0290 0.2434 0.170 Uiso 0.45 1 calc PR B 2 H41M H -0.3110 0.9557 0.2253 0.170 Uiso 0.45 1 calc PR B 2 O1W O 0.39056(13) 0.84338(12) 0.75539(5) 0.0618(7) Uani 1 1 d . . . O2W O 0.05225(16) 0.90430(16) 0.75787(7) 0.0940(10) Uani 1 1 d . . . O3W O -0.72884(18) 0.57455(17) -0.11660(7) 0.1048(11) Uani 1 1 d . . . O4W O -0.68321(19) 0.8458(2) -0.16884(7) 0.1230(13) Uani 1 1 d . . . O5W O -0.72069(19) 0.73849(17) -0.10504(9) 0.1132(12) Uani 1 1 d . . . O6W O -0.6224(2) 0.8160(2) -0.04629(10) 0.1453(15) Uani 1 1 d . . . N1 N -0.5913(3) 0.8148(3) 1.21337(14) 0.0402(16) Uani 0.40 1 d P . . O1 O -0.5965(3) 0.8248(3) 1.17752(14) 0.0611(16) Uani 0.40 1 d P . . O2 O -0.6386(3) 0.7647(3) 1.22614(15) 0.0629(17) Uani 0.40 1 d P . . O3 O -0.5422(4) 0.8510(3) 1.23434(15) 0.0607(16) Uani 0.40 1 d PU . . N2 N 0.0855(2) 0.8260(3) 0.85472(12) 0.0699(14) Uani 0.60 1 d PU . . O6 O 0.0056(3) 0.8515(2) 0.85383(13) 0.0929(16) Uani 0.60 1 d P . . O5 O 0.10492(19) 0.78432(15) 0.87675(7) 0.0388(8) Uani 0.60 1 d PU . . O4 O 0.1382(2) 0.8610(2) 0.82775(8) 0.0590(11) Uani 0.60 1 d P . . 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 Ce1 0.03229(6) 0.02643(7) 0.01580(6) -0.00093(5) 0.00197(5) 0.00089(6) Ce2 0.04112(7) 0.02572(7) 0.01647(6) 0.00075(5) 0.00434(5) 0.00399(6) O305 0.0498(9) 0.0294(9) 0.0253(8) -0.0011(7) -0.0005(7) 0.0056(8) C101 0.0340(12) 0.0271(12) 0.0286(12) -0.0015(10) -0.0039(10) 0.0127(10) C104 0.0305(11) 0.0343(13) 0.0260(11) 0.0046(10) 0.0039(10) 0.0116(11) O101 0.0339(8) 0.0294(8) 0.0166(7) 0.0025(6) 0.0085(6) -0.0035(7) C246 0.0479(14) 0.0387(14) 0.0170(11) 0.0034(10) 0.0035(10) -0.0018(12) O102 0.0352(8) 0.0402(9) 0.0202(7) -0.0027(7) 0.0010(7) -0.0087(8) O105 0.0395(8) 0.0273(8) 0.0247(7) 0.0095(6) 0.0068(7) 0.0070(7) N304 0.0414(10) 0.0268(10) 0.0203(9) -0.0002(8) 0.0047(8) -0.0018(9) C301 0.0386(12) 0.0283(12) 0.0155(10) -0.0066(9) 0.0034(9) 0.0059(11) O203 0.0587(10) 0.0412(9) 0.0164(7) -0.0017(7) -0.0026(7) 0.0170(9) C314 0.0414(13) 0.0324(13) 0.0243(11) -0.0014(10) 0.0055(10) 0.0029(11) C310 0.0393(12) 0.0225(11) 0.0166(10) -0.0023(9) 0.0027(9) -0.0030(10) N302 0.0366(10) 0.0337(11) 0.0245(9) 0.0062(8) 0.0056(8) 0.0033(9) O302 0.0383(8) 0.0301(8) 0.0254(8) -0.0024(7) 0.0055(7) 0.0052(7) O106 0.0421(9) 0.0280(8) 0.0272(8) 0.0013(7) -0.0026(7) 0.0053(7) O206 0.0474(9) 0.0304(8) 0.0211(7) 0.0035(7) 0.0044(7) 0.0023(8) O306 0.0350(8) 0.0300(8) 0.0256(8) -0.0008(7) 0.0054(7) 0.0026(7) O205 0.0543(10) 0.0278(8) 0.0249(8) 0.0012(7) 0.0037(7) 0.0072(8) O301 0.0306(8) 0.0276(8) 0.0239(7) 0.0001(7) 0.0011(6) 0.0021(7) O201 0.0319(8) 0.0284(8) 0.0279(8) 0.0007(7) -0.0063(7) 0.0011(7) O202 0.0403(8) 0.0297(8) 0.0219(7) 0.0039(7) -0.0014(7) -0.0060(7) N102 0.0468(11) 0.0374(11) 0.0145(9) -0.0061(8) 0.0012(8) -0.0079(10) N201 0.0343(10) 0.0320(10) 0.0207(9) 0.0000(8) -0.0036(8) 0.0009(9) C341 0.0428(14) 0.0475(16) 0.0315(13) -0.0120(12) 0.0018(11) 0.0040(13) C139 0.0280(11) 0.0292(12) 0.0193(10) 0.0021(9) 0.0059(9) 0.0098(10) C304 0.0436(13) 0.0311(13) 0.0245(11) -0.0016(10) -0.0037(10) 0.0039(11) C311 0.0318(12) 0.0316(13) 0.0264(11) -0.0019(10) -0.0052(10) 0.0024(11) N202 0.0442(11) 0.0325(11) 0.0252(10) -0.0001(9) -0.0047(9) 0.0071(10) C102 0.0388(12) 0.0279(12) 0.0193(11) -0.0034(10) 0.0011(10) 0.0076(11) C140 0.0259(11) 0.0391(13) 0.0215(11) 0.0022(10) 0.0112(9) 0.0134(10) C201 0.0347(12) 0.0313(13) 0.0229(11) -0.0044(10) 0.0013(10) -0.0016(11) C138 0.0373(12) 0.0252(11) 0.0173(10) 0.0024(9) 0.0072(9) 0.0053(10) N103 0.0441(11) 0.0258(10) 0.0151(8) 0.0024(8) -0.0015(8) 0.0039(9) N301 0.0371(10) 0.0304(10) 0.0200(9) -0.0007(8) 0.0078(8) -0.0026(9) C239 0.0420(13) 0.0280(12) 0.0187(10) 0.0013(10) 0.0037(10) -0.0033(11) N104 0.0388(10) 0.0326(10) 0.0149(8) 0.0043(8) 0.0012(8) 0.0096(9) C337 0.0452(14) 0.0406(14) 0.0240(12) -0.0010(11) 0.0045(11) -0.0063(12) C109 0.0271(11) 0.0250(11) 0.0272(11) 0.0020(10) 0.0067(9) 0.0103(10) N203 0.0693(13) 0.0294(11) 0.0161(9) -0.0026(8) 0.0091(9) 0.0162(10) C240 0.0415(13) 0.0281(12) 0.0270(12) -0.0012(10) 0.0029(10) 0.0000(11) N204 0.0537(12) 0.0316(11) 0.0135(9) -0.0030(8) 0.0053(9) 0.0038(10) C103 0.0358(12) 0.0459(14) 0.0145(10) -0.0003(10) 0.0018(9) 0.0130(11) C209 0.0327(12) 0.0410(14) 0.0176(11) -0.0040(10) 0.0070(9) 0.0021(11) C108 0.0592(15) 0.0277(13) 0.0196(11) 0.0000(10) 0.0085(11) -0.0020(12) C248 0.0378(12) 0.0230(11) 0.0227(11) 0.0029(9) 0.0034(10) -0.0037(10) N101 0.0397(10) 0.0305(10) 0.0143(8) -0.0041(8) -0.0005(8) -0.0019(9) C347 0.0408(13) 0.0364(13) 0.0186(11) -0.0039(10) 0.0010(10) 0.0075(11) C309 0.0425(13) 0.0269(12) 0.0183(11) -0.0054(10) -0.0014(10) 0.0042(11) C105 0.0373(12) 0.0401(13) 0.0299(12) 0.0140(10) 0.0054(10) 0.0119(11) C147 0.0506(14) 0.0273(12) 0.0343(12) 0.0082(10) 0.0031(11) 0.0103(12) C345 0.0425(13) 0.0241(12) 0.0263(11) 0.0000(10) 0.0026(10) 0.0064(11) C216 0.0364(12) 0.0490(15) 0.0189(11) 0.0000(11) 0.0008(10) 0.0104(12) C313 0.0340(12) 0.0286(12) 0.0239(11) 0.0006(10) 0.0054(10) -0.0045(11) C111 0.0333(12) 0.0286(12) 0.0183(10) 0.0004(9) -0.0017(9) 0.0008(10) C339 0.0421(13) 0.0218(11) 0.0185(10) -0.0027(9) 0.0005(10) 0.0052(11) C302 0.0332(12) 0.0382(13) 0.0302(12) 0.0058(11) 0.0045(10) -0.0003(11) C148 0.0384(12) 0.0307(12) 0.0240(11) 0.0012(10) 0.0075(10) 0.0125(11) C237 0.0492(14) 0.0410(14) 0.0190(11) 0.0016(11) 0.0079(10) 0.0103(12) C340 0.0394(13) 0.0285(12) 0.0268(11) 0.0050(10) 0.0072(10) 0.0067(11) C247 0.0488(14) 0.0290(13) 0.0172(11) -0.0048(10) 0.0050(10) 0.0040(12) N303 0.0371(11) 0.0573(14) 0.0236(10) -0.0060(10) -0.0014(9) 0.0019(11) C348 0.0400(13) 0.0216(11) 0.0312(12) 0.0048(10) 0.0032(10) 0.0077(11) C346 0.0529(14) 0.0335(13) 0.0223(11) -0.0004(10) -0.0070(11) 0.0137(12) C134 0.0391(12) 0.0285(12) 0.0214(11) 0.0015(10) -0.0018(10) 0.0019(11) C110 0.0268(11) 0.0307(12) 0.0160(10) 0.0024(9) 0.0030(9) 0.0050(10) C141 0.0329(12) 0.0424(14) 0.0221(11) 0.0030(10) 0.0041(10) -0.0007(11) C213 0.0310(12) 0.0407(14) 0.0304(12) 0.0059(11) -0.0012(10) 0.0063(11) C312 0.0351(12) 0.0390(14) 0.0325(13) -0.0030(11) 0.0016(11) 0.0041(12) C204 0.0368(12) 0.0422(14) 0.0243(12) -0.0090(11) 0.0003(10) -0.0046(12) C112 0.0377(13) 0.0349(14) 0.0351(13) -0.0055(11) 0.0096(11) 0.0013(12) C210 0.0308(11) 0.0255(12) 0.0234(11) -0.0019(10) -0.0001(9) 0.0002(10) C234 0.0474(13) 0.0322(13) 0.0186(11) 0.0002(10) 0.0049(10) 0.0113(12) C211 0.0355(12) 0.0277(12) 0.0244(11) -0.0009(10) 0.0069(10) 0.0026(11) C241 0.0579(15) 0.0337(13) 0.0239(12) 0.0036(11) 0.0053(11) 0.0066(13) C315 0.0406(13) 0.0336(13) 0.0322(12) 0.0095(10) 0.0050(11) 0.0103(11) C146 0.0466(14) 0.0425(14) 0.0269(12) 0.0086(11) -0.0047(11) 0.0138(12) C308 0.0347(12) 0.0275(12) 0.0261(11) -0.0008(10) -0.0040(10) -0.0059(11) C215 0.0493(14) 0.0347(14) 0.0258(12) 0.0002(11) -0.0023(11) 0.0015(12) C208 0.0265(11) 0.0387(13) 0.0191(10) 0.0020(10) 0.0011(9) -0.0004(11) C142 0.0362(12) 0.0496(15) 0.0240(12) 0.0015(11) 0.0060(10) -0.0078(12) C113 0.0506(14) 0.0473(15) 0.0174(11) -0.0037(11) 0.0038(11) -0.0115(13) C107 0.0354(13) 0.0279(13) 0.0533(15) 0.0024(12) 0.0122(12) 0.0034(11) C143 0.0308(12) 0.078(2) 0.0208(12) -0.0108(13) -0.0033(10) 0.0088(14) C244 0.0504(14) 0.0356(14) 0.0269(12) 0.0043(11) 0.0055(11) 0.0081(12) C214 0.0433(13) 0.0374(13) 0.0257(12) 0.0069(10) -0.0032(10) 0.0000(12) C238 0.0483(14) 0.0293(13) 0.0239(11) -0.0022(10) 0.0074(11) 0.0117(11) C217 0.0561(15) 0.0325(13) 0.0368(13) 0.0039(11) -0.0086(12) 0.0117(12) C305 0.0535(15) 0.0343(14) 0.0247(12) -0.0053(11) -0.0031(11) 0.0043(13) C243 0.0558(15) 0.0394(14) 0.0286(12) 0.0069(11) -0.0039(12) 0.0080(13) C106 0.0344(12) 0.0377(13) 0.0452(13) 0.0158(11) 0.0136(11) 0.0059(11) C334 0.0417(13) 0.0437(15) 0.0218(11) -0.0004(11) -0.0031(10) -0.0058(12) C212 0.0524(15) 0.0369(14) 0.0268(12) -0.0086(11) 0.0010(11) 0.0068(13) C344 0.0554(15) 0.0415(14) 0.0206(11) -0.0009(11) 0.0059(11) 0.0110(13) C332 0.0521(15) 0.0420(15) 0.0190(11) -0.0096(11) -0.0001(11) 0.0027(13) C245 0.0475(13) 0.0268(12) 0.0176(10) -0.0010(10) 0.0016(10) -0.0023(11) C137 0.0409(12) 0.0186(11) 0.0232(11) -0.0012(9) 0.0071(10) 0.0139(10) C203 0.0464(14) 0.0453(15) 0.0233(12) -0.0041(11) -0.0116(11) 0.0094(13) C242 0.0452(14) 0.0353(14) 0.0369(13) -0.0006(12) 0.0097(12) 0.0129(12) C338 0.0287(12) 0.0442(14) 0.0339(13) 0.0032(11) -0.0009(10) -0.0033(11) C144 0.0379(13) 0.0565(16) 0.0228(12) 0.0032(11) 0.0017(10) 0.0191(12) C218 0.0532(15) 0.0377(14) 0.0252(12) -0.0035(11) -0.0054(11) 0.0137(13) C343 0.0515(15) 0.0407(15) 0.0336(13) -0.0038(12) 0.0154(12) 0.0147(13) C333 0.0415(13) 0.0468(15) 0.0233(12) -0.0025(11) 0.0002(10) -0.0085(12) C235 0.0626(16) 0.0259(12) 0.0295(12) 0.0020(11) 0.0106(12) 0.0108(12) C318 0.0414(13) 0.0497(15) 0.0256(12) 0.0081(11) 0.0004(11) 0.0114(12) C145 0.0316(12) 0.0425(14) 0.0257(11) 0.0035(11) 0.0060(10) 0.0146(11) C202 0.0408(13) 0.0398(14) 0.0292(12) 0.0022(11) -0.0073(11) 0.0070(12) C306 0.0466(14) 0.0425(15) 0.0348(13) -0.0042(12) -0.0079(12) 0.0126(13) C233 0.0747(18) 0.0302(13) 0.0214(12) -0.0044(11) 0.0094(12) 0.0110(13) O204 0.0855(12) 0.0367(9) 0.0154(8) -0.0027(7) 0.0023(8) 0.0257(9) O303 0.0531(10) 0.0485(10) 0.0206(8) 0.0050(7) 0.0017(7) 0.0171(9) O304 0.0631(11) 0.0564(11) 0.0229(8) -0.0044(8) -0.0023(8) 0.0172(10) O103 0.0702(11) 0.0822(13) 0.0156(8) -0.0059(9) 0.0034(8) -0.0411(10) O104 0.0580(10) 0.0697(12) 0.0268(8) 0.0170(8) -0.0145(8) -0.0299(9) C115 0.0563(15) 0.0471(15) 0.0222(12) 0.0024(11) 0.0020(11) -0.0201(13) C232 0.0754(18) 0.0321(13) 0.0215(11) 0.0070(10) 0.0074(12) 0.0124(13) C317 0.0462(14) 0.0485(15) 0.0289(12) 0.0024(12) 0.0135(11) 0.0119(13) C231 0.0545(14) 0.0365(13) 0.0141(11) -0.0048(10) 0.0064(10) 0.0162(12) C303 0.0459(14) 0.0342(13) 0.0321(12) 0.0073(11) 0.0031(11) 0.0026(12) O01 0.120(2) 0.1011(19) 0.0750(16) 0.0059(15) 0.0070(15) 0.0175(17) C206 0.0605(17) 0.0490(17) 0.0424(15) -0.0261(14) 0.0015(14) 0.0049(15) C331 0.0495(14) 0.0465(15) 0.0187(11) -0.0022(11) 0.0022(11) 0.0015(13) C236 0.0723(17) 0.0291(13) 0.0234(12) -0.0029(11) 0.0035(12) 0.0158(13) C316 0.0357(12) 0.0443(14) 0.0227(11) 0.0111(10) -0.0006(10) -0.0025(12) C114 0.0515(14) 0.0357(14) 0.0231(12) -0.0076(11) 0.0003(11) -0.0116(12) C120 0.0470(14) 0.0515(16) 0.0241(12) -0.0022(12) 0.0003(11) -0.0156(13) C324 0.0483(14) 0.0483(15) 0.0273(12) 0.0042(12) 0.0043(11) 0.0043(13) C205 0.0534(15) 0.0517(16) 0.0219(12) -0.0131(12) -0.0014(11) -0.0001(14) O11 0.0637(13) 0.0991(17) 0.0782(14) 0.0116(14) 0.0038(12) -0.0169(13) C307 0.0361(13) 0.0426(15) 0.0450(14) 0.0029(12) -0.0036(12) 0.0047(12) C133 0.0466(14) 0.0537(16) 0.0250(12) 0.0122(11) 0.0025(11) -0.0075(13) C121 0.0444(14) 0.0569(17) 0.0359(14) -0.0246(13) 0.0108(12) -0.0107(14) C119 0.0755(18) 0.083(2) 0.0208(13) -0.0038(14) 0.0059(13) -0.0364(17) C226 0.0596(17) 0.0671(19) 0.0470(16) 0.0107(15) -0.0005(14) 0.0079(16) C322 0.0534(15) 0.0339(14) 0.0360(13) -0.0019(12) -0.0016(12) 0.0053(13) C125 0.0588(16) 0.0351(14) 0.0278(12) -0.0004(11) -0.0018(12) -0.0089(13) C323 0.0485(14) 0.0472(15) 0.0174(11) -0.0036(11) 0.0008(11) 0.0104(13) C222 0.0584(15) 0.0302(13) 0.0336(13) -0.0088(11) -0.0095(12) 0.0213(12) C336 0.0568(16) 0.0606(18) 0.0285(13) -0.0016(13) -0.0044(12) 0.0120(15) C219 0.0653(16) 0.0459(15) 0.0232(12) -0.0020(12) 0.0003(12) 0.0206(14) C330 0.0629(16) 0.0457(15) 0.0221(12) 0.0004(11) 0.0020(12) 0.0118(14) C325 0.0486(14) 0.0546(16) 0.0224(12) -0.0005(12) 0.0001(11) 0.0041(14) C124 0.0504(15) 0.0433(15) 0.0278(13) -0.0067(12) 0.0032(11) -0.0084(13) C223 0.0613(15) 0.0362(13) 0.0180(11) -0.0034(10) 0.0000(11) 0.0198(12) C131 0.0579(15) 0.0512(15) 0.0228(11) 0.0129(11) -0.0130(11) -0.0127(13) N11 0.0445(13) 0.0619(16) 0.0845(17) 0.0113(14) 0.0080(13) 0.0097(13) C116 0.0615(16) 0.0726(19) 0.0154(11) -0.0066(12) 0.0057(11) -0.0282(15) C132 0.0424(13) 0.0512(15) 0.0292(12) 0.0106(11) -0.0057(11) -0.0141(13) C329 0.0527(16) 0.097(2) 0.0398(15) 0.0162(16) -0.0067(13) 0.0037(17) C221 0.0604(15) 0.0384(14) 0.0155(11) -0.0033(10) 0.0035(11) 0.0169(13) C135 0.0610(16) 0.0762(19) 0.0324(13) 0.0173(13) -0.0211(12) -0.0306(15) C224 0.0587(16) 0.0378(14) 0.0265(12) -0.0081(11) 0.0047(12) 0.0139(13) C320 0.0584(15) 0.0462(15) 0.0198(11) 0.0009(11) 0.0065(11) 0.0151(13) C220 0.0563(15) 0.0430(14) 0.0179(11) -0.0019(11) 0.0007(11) 0.0254(12) C207 0.0618(17) 0.0359(15) 0.0465(16) -0.0120(13) 0.0018(14) 0.0106(14) C122 0.0336(13) 0.0464(16) 0.0679(17) 0.0127(14) -0.0054(13) -0.0066(13) N01 0.0872(18) 0.0481(15) 0.0754(17) -0.0032(14) -0.0038(15) -0.0045(15) C227 0.0761(19) 0.0624(19) 0.0275(13) -0.0081(14) -0.0101(13) 0.0178(16) C342 0.0413(14) 0.0559(18) 0.0448(15) -0.0080(14) 0.0117(12) 0.0050(14) N21 0.0611(16) 0.109(2) 0.0733(16) 0.0320(16) 0.0048(14) -0.0088(16) C230 0.0670(17) 0.0388(14) 0.0224(12) -0.0068(11) -0.0032(12) 0.0170(14) C225 0.0539(15) 0.0454(15) 0.0234(12) -0.0027(11) -0.0033(11) 0.0165(13) C319 0.0606(16) 0.0595(17) 0.0231(12) 0.0041(12) 0.0070(12) 0.0268(14) O21 0.0956(18) 0.134(2) 0.0820(17) 0.0014(17) 0.0162(15) -0.0135(18) C335 0.0479(15) 0.0550(17) 0.0311(13) -0.0100(13) 0.0015(12) 0.0025(14) C321 0.0575(16) 0.0393(14) 0.0319(13) 0.0046(12) 0.0092(12) 0.0035(13) C13 0.064(2) 0.088(2) 0.073(2) 0.0169(19) 0.0144(17) 0.0011(19) C327 0.0673(18) 0.0488(17) 0.0515(16) -0.0045(15) -0.0091(15) -0.0082(16) C23 0.096(3) 0.096(3) 0.072(2) 0.025(2) 0.007(2) -0.009(2) C118 0.103(2) 0.088(2) 0.0202(13) -0.0045(13) 0.0117(13) -0.0657(16) C229 0.0603(17) 0.0553(17) 0.0375(14) -0.0061(14) -0.0023(13) 0.0160(15) C228 0.0648(18) 0.0612(19) 0.0441(16) -0.0011(15) 0.0117(14) 0.0124(16) C123 0.0437(13) 0.0505(15) 0.0255(12) 0.0087(11) -0.0060(11) -0.0124(13) C328 0.0634(18) 0.087(2) 0.0400(15) 0.0191(15) 0.0015(14) -0.0095(17) C136 0.0781(18) 0.105(2) 0.0371(14) 0.0336(14) -0.0215(13) -0.0524(17) C03 0.100(2) 0.057(2) 0.068(2) -0.0100(18) 0.0331(19) -0.005(2) C117 0.0826(19) 0.087(2) 0.0281(14) -0.0116(15) 0.0112(14) -0.0448(17) C126 0.061(2) 0.085(3) 0.112(3) -0.039(2) 0.024(2) 0.000(2) C130 0.0613(16) 0.087(2) 0.0382(14) 0.0272(14) -0.0114(13) -0.0321(16) C128 0.096(2) 0.066(2) 0.0565(19) -0.0226(17) 0.0175(18) -0.001(2) C129 0.105(3) 0.064(2) 0.0624(19) 0.0108(17) -0.0137(19) 0.017(2) C326 0.076(2) 0.065(2) 0.0506(17) 0.0134(15) 0.0116(15) -0.0088(17) C127 0.061(2) 0.073(2) 0.144(3) 0.032(2) -0.023(2) 0.0061(19) C22 0.119(3) 0.087(3) 0.141(4) 0.015(3) 0.043(3) -0.001(3) C02 0.099(3) 0.087(3) 0.112(3) 0.002(2) -0.006(2) -0.038(2) C21 0.062(2) 0.246(5) 0.107(3) 0.072(3) 0.003(2) -0.030(3) C01 0.111(3) 0.083(3) 0.106(3) -0.005(2) -0.028(2) 0.003(3) C12 0.067(2) 0.203(5) 0.088(3) 0.043(3) 0.014(2) 0.027(3) C11 0.0531(18) 0.057(2) 0.139(3) 0.023(2) -0.004(2) -0.0067(17) N401 0.099(2) 0.096(3) 0.098(2) 0.006(2) 0.007(2) 0.009(2) O401 0.0755(19) 0.124(3) 0.107(2) -0.012(2) -0.0016(17) 0.0059(19) C403 0.120(3) 0.067(2) 0.116(3) -0.009(2) -0.069(2) 0.038(2) C402 0.127(4) 0.158(4) 0.105(3) 0.044(3) -0.010(3) -0.017(4) C401 0.115(4) 0.103(4) 0.208(5) -0.038(4) 0.014(4) 0.036(3) N31 0.079(2) 0.065(2) 0.108(3) -0.007(2) 0.002(2) 0.0180(19) O31 0.134(3) 0.146(3) 0.110(3) -0.009(3) -0.005(2) 0.023(3) C32 0.096(3) 0.097(4) 0.176(5) -0.030(4) -0.060(3) 0.036(3) C33 0.098(3) 0.109(4) 0.129(4) -0.010(3) -0.061(3) 0.011(3) C31 0.259(7) 0.115(4) 0.128(4) 0.026(4) 0.105(4) 0.061(5) N41 0.0707(18) 0.082(2) 0.125(2) 0.0143(19) 0.0200(18) -0.0009(17) O41 0.172(2) 0.0479(13) 0.1023(17) -0.0044(13) -0.0445(17) 0.0315(15) C42 0.112(3) 0.076(3) 0.242(5) 0.062(3) 0.050(3) 0.022(3) C43 0.084(2) 0.066(2) 0.117(3) -0.002(2) 0.008(2) 0.008(2) C41 0.097(3) 0.134(4) 0.223(5) -0.092(4) 0.058(3) -0.004(3) N51 0.0783(17) 0.0664(17) 0.0579(15) -0.0164(14) 0.0200(13) -0.0159(15) O51 0.0566(11) 0.0654(12) 0.0484(10) 0.0110(10) 0.0027(9) -0.0159(10) C51 0.141(4) 0.150(4) 0.069(2) -0.052(3) 0.020(3) -0.028(3) C52 0.072(2) 0.100(3) 0.114(3) -0.008(3) 0.035(2) -0.009(2) C53 0.0554(16) 0.0530(17) 0.0430(15) 0.0007(14) 0.0008(13) -0.0044(15) N61 0.0623(15) 0.0797(19) 0.0744(17) 0.0084(15) 0.0191(13) -0.0115(15) O61 0.135(2) 0.0927(18) 0.0769(16) -0.0107(15) 0.0198(15) -0.0442(16) C61 0.089(3) 0.150(4) 0.114(3) 0.040(3) -0.021(2) 0.004(3) C62 0.123(3) 0.141(4) 0.068(2) -0.011(3) 0.028(2) -0.047(3) C63 0.082(2) 0.080(2) 0.076(2) 0.002(2) 0.0050(19) -0.026(2) O71 0.0895(15) 0.0451(12) 0.0657(13) -0.0048(11) -0.0063(12) -0.0003(12) N71 0.0680(16) 0.0735(18) 0.097(2) -0.0011(17) -0.0052(15) -0.0081(15) C71 0.079(3) 0.130(4) 0.184(4) 0.012(3) -0.016(3) -0.013(3) C72 0.095(3) 0.154(4) 0.125(3) -0.085(3) -0.007(3) 0.015(3) C73 0.0729(19) 0.067(2) 0.0492(17) -0.0095(16) -0.0028(15) -0.0005(18) N81 0.103(2) 0.101(2) 0.104(2) 0.010(2) -0.0466(19) -0.007(2) O81 0.135(3) 0.144(3) 0.184(3) -0.044(3) -0.070(2) 0.019(3) C82 0.126(4) 0.135(4) 0.133(4) 0.004(4) -0.034(3) -0.009(4) C83 0.107(3) 0.115(3) 0.136(3) 0.010(3) -0.046(3) 0.002(3) C81 0.123(4) 0.189(5) 0.104(4) -0.009(4) 0.008(3) -0.047(4) N91 0.121(3) 0.088(3) 0.074(2) -0.019(2) 0.034(2) 0.051(2) C93 0.144(3) 0.109(3) 0.087(3) -0.023(3) 0.026(3) 0.063(3) C92 0.154(5) 0.111(5) 0.124(5) -0.027(4) 0.024(4) 0.021(5) C91 0.146(5) 0.147(5) 0.135(5) -0.060(4) -0.015(4) 0.087(4) O91 0.149(5) 0.120(5) 0.108(5) -0.011(5) 0.014(5) 0.060(5) O91' 0.194(6) 0.133(5) 0.081(4) -0.028(4) 0.006(5) 0.071(5) O411 0.124(2) 0.114(2) 0.109(2) -0.009(2) 0.014(2) 0.015(2) N411 0.139(3) 0.076(2) 0.101(2) -0.024(2) 0.009(2) 0.043(2) C412 0.127(3) 0.092(3) 0.137(4) -0.034(3) 0.051(3) 0.014(3) C413 0.140(3) 0.087(3) 0.163(3) -0.053(3) 0.087(3) -0.026(3) C411 0.138(6) 0.080(5) 0.177(6) 0.016(5) 0.050(6) 0.036(5) C41' 0.127(5) 0.076(4) 0.140(6) -0.004(5) 0.024(5) 0.061(4) O1W 0.0598(12) 0.0789(13) 0.0511(11) 0.0172(10) 0.0156(9) 0.0259(11) O2W 0.0743(14) 0.121(2) 0.0827(15) -0.0056(16) -0.0240(12) -0.0112(15) O3W 0.0911(17) 0.147(3) 0.0708(15) -0.0078(17) -0.0068(14) -0.0165(18) O4W 0.0986(19) 0.200(3) 0.0665(16) -0.014(2) 0.0239(15) 0.013(2) O5W 0.0919(18) 0.127(2) 0.118(2) -0.012(2) -0.0019(17) 0.0213(18) O6W 0.120(2) 0.166(3) 0.149(3) -0.024(2) -0.016(2) 0.056(2) N1 0.029(2) 0.058(3) 0.033(3) -0.018(3) -0.005(2) 0.027(2) O1 0.046(2) 0.083(3) 0.058(3) 0.002(3) 0.013(2) 0.043(2) O2 0.040(3) 0.086(4) 0.064(3) 0.011(3) -0.002(2) 0.004(3) O3 0.074(3) 0.038(3) 0.070(3) -0.011(2) 0.009(3) 0.029(2) N2 0.0246(18) 0.097(3) 0.075(2) -0.063(2) 0.0045(18) -0.004(2) O6 0.096(3) 0.078(3) 0.104(3) 0.010(2) -0.004(3) -0.005(3) O5 0.0536(16) 0.0421(15) 0.0230(12) 0.0184(11) -0.0145(12) 0.0017(14) O4 0.0366(16) 0.109(3) 0.0287(15) -0.0076(18) -0.0005(13) 0.0023(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 Ce1 O101 2.1853(14) . ? Ce1 O201 2.1987(14) . ? Ce1 O301 2.2022(15) . ? Ce1 O202 2.4167(15) . ? Ce1 O102 2.4314(14) . ? Ce1 O302 2.4338(15) . ? Ce1 N101 2.5964(18) . ? Ce1 N301 2.6245(19) . ? Ce1 N201 2.6277(19) . ? Ce2 O306 2.1913(14) . ? Ce2 O106 2.2063(15) . ? Ce2 O206 2.2114(15) . ? Ce2 O305 2.4228(15) . ? Ce2 O105 2.4314(15) . ? Ce2 O205 2.4940(15) . ? Ce2 N204 2.557(2) . ? Ce2 N104 2.5884(19) . ? Ce2 N304 2.6027(19) . ? O305 C337 1.238(3) . ? C101 O101 1.313(3) . ? C101 C110 1.399(3) . ? C101 C102 1.425(3) . ? C104 C105 1.412(3) . ? C104 C109 1.413(3) . ? C104 C103 1.426(3) . ? C246 C247 1.353(3) . ? C246 C245 1.419(3) . ? O102 C108 1.255(3) . ? O105 C137 1.255(3) . ? N304 C338 1.296(3) . ? N304 N303 1.387(2) . ? C301 O301 1.309(3) . ? C301 C310 1.407(3) . ? C301 C302 1.413(3) . ? O203 C216 1.365(3) . ? O203 C219 1.454(3) . ? C314 C315 1.367(3) . ? C314 C313 1.402(3) . ? C310 C311 1.442(3) . ? C310 C309 1.449(3) . ? N302 C308 1.324(3) . ? N302 N301 1.391(2) . ? O302 C308 1.258(3) . ? O106 C148 1.310(3) . ? O206 C248 1.332(3) . ? O306 C348 1.329(3) . ? O205 C237 1.268(3) . ? O201 C201 1.313(3) . ? O202 C208 1.254(3) . ? N102 C108 1.329(3) . ? N102 N101 1.401(2) . ? N201 C211 1.283(3) . ? N201 N202 1.395(3) . ? C341 C342 1.388(4) . ? C341 C340 1.396(3) . ? C139 C148 1.404(3) . ? C139 C138 1.442(3) . ? C139 C140 1.446(3) . ? C304 C305 1.399(3) . ? C304 C309 1.422(3) . ? C304 C303 1.424(3) . ? C311 N301 1.300(3) . ? N202 C208 1.326(3) . ? C102 C103 1.342(3) . ? C140 C141 1.412(3) . ? C140 C145 1.437(3) . ? C201 C210 1.395(3) . ? C201 C202 1.430(3) . ? C138 N104 1.293(3) . ? N103 C137 1.336(3) . ? N103 N104 1.405(2) . ? C239 C248 1.400(3) . ? C239 C240 1.431(3) . ? C239 C238 1.459(3) . ? C337 N303 1.348(3) . ? C337 C334 1.481(3) . ? C109 C112 1.430(3) . ? C109 C110 1.455(3) . ? N203 C237 1.326(3) . ? N203 N204 1.398(2) . ? C240 C241 1.417(3) . ? C240 C245 1.425(3) . ? N204 C238 1.292(3) . ? C209 C212 1.406(4) . ? C209 C204 1.417(3) . ? C209 C210 1.455(3) . ? C108 C113 1.479(3) . ? C248 C247 1.431(3) . ? N101 C111 1.289(3) . ? C347 C346 1.356(3) . ? C347 C348 1.412(3) . ? C309 C312 1.425(3) . ? C105 C106 1.362(3) . ? C147 C146 1.355(3) . ? C147 C148 1.419(3) . ? C345 C344 1.408(3) . ? C345 C346 1.431(3) . ? C345 C340 1.435(3) . ? C216 C217 1.391(3) . ? C216 C215 1.396(4) . ? C313 C318 1.391(3) . ? C313 C308 1.480(3) . ? C111 C110 1.441(3) . ? C339 C348 1.397(3) . ? C339 C338 1.436(3) . ? C339 C340 1.443(3) . ? C302 C303 1.341(3) . ? C237 C234 1.467(3) . ? C134 C133 1.370(3) . ? C134 C135 1.386(4) . ? C134 C137 1.472(3) . ? C141 C142 1.373(3) . ? C213 C214 1.375(3) . ? C213 C218 1.389(4) . ? C213 C208 1.468(3) . ? C312 C307 1.358(4) . ? C204 C203 1.403(4) . ? C204 C205 1.414(3) . ? C112 C107 1.359(3) . ? C210 C211 1.440(3) . ? C234 C235 1.396(3) . ? C234 C233 1.398(3) . ? C241 C242 1.360(4) . ? C315 C316 1.411(3) . ? C146 C145 1.420(3) . ? C215 C214 1.382(3) . ? C142 C143 1.399(4) . ? C113 C118 1.368(4) . ? C113 C114 1.378(3) . ? C107 C106 1.390(3) . ? C143 C144 1.376(4) . ? C244 C243 1.356(4) . ? C244 C245 1.393(3) . ? C217 C218 1.364(3) . ? C305 C306 1.353(4) . ? C243 C242 1.406(3) . ? C334 C333 1.388(3) . ? C334 C335 1.404(4) . ? C212 C207 1.378(3) . ? C344 C343 1.350(4) . ? C332 C331 1.366(4) . ? C332 C333 1.387(3) . ? C203 C202 1.364(3) . ? C144 C145 1.391(3) . ? C343 C342 1.384(3) . ? C235 C236 1.384(3) . ? C318 C317 1.386(3) . ? C306 C307 1.391(4) . ? C233 C232 1.362(3) . ? O204 C231 1.359(3) . ? O204 C230 1.450(3) . ? O303 C316 1.337(3) . ? O303 C319 1.467(3) . ? O304 C331 1.369(3) . ? O304 C330 1.440(3) . ? O103 C116 1.363(3) . ? O103 C119 1.457(3) . ? O104 C131 1.373(3) . ? O104 C130 1.453(3) . ? C115 C116 1.362(4) . ? C115 C114 1.368(3) . ? C232 C231 1.389(3) . ? C317 C316 1.387(4) . ? C231 C236 1.361(3) . ? O01 C03 1.260(4) . ? C206 C207 1.363(4) . ? C206 C205 1.376(4) . ? C331 C336 1.395(4) . ? C120 C125 1.376(4) . ? C120 C121 1.378(4) . ? C120 C119 1.523(3) . ? C324 C325 1.400(3) . ? C324 C323 1.400(3) . ? C324 C328 1.517(4) . ? O11 C13 1.253(4) . ? C133 C132 1.396(3) . ? C121 C122 1.430(4) . ? C121 C126 1.504(4) . ? C226 C221 1.502(4) . ? C322 C321 1.394(3) . ? C322 C323 1.412(4) . ? C322 C327 1.509(4) . ? C125 C124 1.396(3) . ? C125 C129 1.525(4) . ? C323 C330 1.505(3) . ? C222 C223 1.397(4) . ? C222 C221 1.412(3) . ? C222 C227 1.520(4) . ? C336 C335 1.383(3) . ? C219 C220 1.503(3) . ? C325 C320 1.398(4) . ? C325 C329 1.520(4) . ? C124 C123 1.382(4) . ? C124 C128 1.539(4) . ? C223 C224 1.417(4) . ? C223 C230 1.504(3) . ? C131 C132 1.379(4) . ? C131 C136 1.383(4) . ? N11 C13 1.311(4) . ? N11 C12 1.437(5) . ? N11 C11 1.440(4) . ? C116 C117 1.426(4) . ? C221 C220 1.408(3) . ? C135 C136 1.389(4) . ? C224 C225 1.388(3) . ? C224 C228 1.521(4) . ? C320 C321 1.405(4) . ? C320 C319 1.504(3) . ? C220 C225 1.418(4) . ? C122 C123 1.399(4) . ? C122 C127 1.509(4) . ? N01 C03 1.354(4) . ? N01 C02 1.415(5) . ? N01 C01 1.428(5) . ? N21 C23 1.338(5) . ? N21 C22 1.426(5) . ? N21 C21 1.455(5) . ? C225 C229 1.506(4) . ? O21 C23 1.244(4) . ? C321 C326 1.515(4) . ? C118 C117 1.376(4) . ? C123 C130 1.497(3) . ? N401 C401 1.382(7) . ? N401 C402 1.494(7) . ? N401 C403 1.608(6) . ? O401 C403 1.121(6) . ? N31 C33 1.382(6) . ? N31 C31 1.392(7) . ? N31 C32 1.425(6) . ? O31 C33 1.249(6) . ? N41 C43 1.354(5) . ? N41 C42 1.472(5) . ? N41 C41 1.477(6) . ? O41 C43 1.212(4) . ? N51 C53 1.295(4) . ? N51 C51 1.473(5) . ? N51 C52 1.480(4) . ? O51 C53 1.247(3) . ? N61 C63 1.326(5) . ? N61 C61 1.438(5) . ? N61 C62 1.455(4) . ? O61 C63 1.235(4) . ? O71 C73 1.198(4) . ? N71 C73 1.315(4) . ? N71 C71 1.472(5) . ? N71 C72 1.508(5) . ? N81 C83 1.364(7) . ? N81 C81 1.399(7) . ? N81 C82 1.431(7) . ? O81 C83 1.300(7) . ? N91 C91 1.303(9) . ? N91 C92 1.401(9) . ? N91 C93 1.575(9) . ? C93 O91' 1.113(9) . ? C93 O91 1.119(10) . ? O411 C413 1.212(6) . ? N411 C413 1.327(6) . ? N411 C41' 1.429(8) . ? N411 C412 1.437(6) . ? N411 C411 1.490(8) . ? N1 O3 1.148(7) . ? N1 O2 1.227(7) . ? N1 O1 1.232(7) . ? N2 O5 1.152(5) . ? N2 O6 1.286(6) . ? N2 O4 1.368(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 O101 Ce1 O201 82.70(5) . . ? O101 Ce1 O301 84.56(5) . . ? O201 Ce1 O301 88.64(5) . . ? O101 Ce1 O202 88.78(5) . . ? O201 Ce1 O202 128.84(5) . . ? O301 Ce1 O202 140.72(5) . . ? O101 Ce1 O102 129.44(5) . . ? O201 Ce1 O102 146.08(5) . . ? O301 Ce1 O102 84.75(5) . . ? O202 Ce1 O102 70.03(5) . . ? O101 Ce1 O302 146.10(5) . . ? O201 Ce1 O302 87.85(5) . . ? O301 Ce1 O302 127.83(5) . . ? O202 Ce1 O302 72.13(5) . . ? O102 Ce1 O302 70.64(5) . . ? O101 Ce1 N101 67.41(5) . . ? O201 Ce1 N101 146.32(5) . . ? O301 Ce1 N101 73.91(6) . . ? O202 Ce1 N101 67.83(5) . . ? O102 Ce1 N101 62.13(5) . . ? O302 Ce1 N101 125.64(5) . . ? O101 Ce1 N301 145.80(5) . . ? O201 Ce1 N301 78.18(5) . . ? O301 Ce1 N301 67.02(6) . . ? O202 Ce1 N301 125.22(5) . . ? O102 Ce1 N301 68.60(5) . . ? O302 Ce1 N301 61.34(6) . . ? N101 Ce1 N301 118.51(6) . . ? O101 Ce1 N201 78.47(6) . . ? O201 Ce1 N201 67.79(5) . . ? O301 Ce1 N201 152.34(5) . . ? O202 Ce1 N201 61.08(5) . . ? O102 Ce1 N201 122.87(5) . . ? O302 Ce1 N201 67.84(5) . . ? N101 Ce1 N201 117.98(6) . . ? N301 Ce1 N201 118.75(6) . . ? O306 Ce2 O106 84.50(6) . . ? O306 Ce2 O206 82.48(6) . . ? O106 Ce2 O206 83.98(6) . . ? O306 Ce2 O305 129.58(6) . . ? O106 Ce2 O305 143.59(5) . . ? O206 Ce2 O305 88.06(5) . . ? O306 Ce2 O105 89.14(5) . . ? O106 Ce2 O105 128.11(5) . . ? O206 Ce2 O105 145.98(6) . . ? O305 Ce2 O105 72.13(5) . . ? O306 Ce2 O205 147.04(5) . . ? O106 Ce2 O205 89.12(5) . . ? O206 Ce2 O205 129.01(5) . . ? O305 Ce2 O205 68.80(5) . . ? O105 Ce2 O205 69.69(5) . . ? O306 Ce2 N204 144.68(6) . . ? O106 Ce2 N204 72.83(6) . . ? O206 Ce2 N204 68.76(6) . . ? O305 Ce2 N204 71.17(6) . . ? O105 Ce2 N204 126.16(5) . . ? O205 Ce2 N204 60.98(5) . . ? O306 Ce2 N104 76.66(6) . . ? O106 Ce2 N104 66.84(6) . . ? O206 Ce2 N104 145.31(5) . . ? O305 Ce2 N104 126.55(5) . . ? O105 Ce2 N104 61.60(5) . . ? O205 Ce2 N104 71.13(5) . . ? N204 Ce2 N104 116.34(6) . . ? O306 Ce2 N304 68.22(5) . . ? O106 Ce2 N304 147.81(5) . . ? O206 Ce2 N304 76.05(6) . . ? O305 Ce2 N304 61.44(5) . . ? O105 Ce2 N304 70.23(5) . . ? O205 Ce2 N304 123.06(5) . . ? N204 Ce2 N304 120.85(6) . . ? N104 Ce2 N304 119.66(6) . . ? C337 O305 Ce2 122.45(14) . . ? O101 C101 C110 122.18(19) . . ? O101 C101 C102 118.61(19) . . ? C110 C101 C102 119.2(2) . . ? C105 C104 C109 120.4(2) . . ? C105 C104 C103 120.6(2) . . ? C109 C104 C103 119.0(2) . . ? C101 O101 Ce1 138.97(14) . . ? C247 C246 C245 122.4(2) . . ? C108 O102 Ce1 121.95(14) . . ? C137 O105 Ce2 121.05(14) . . ? C338 N304 N303 115.68(19) . . ? C338 N304 Ce2 130.31(15) . . ? N303 N304 Ce2 113.76(13) . . ? O301 C301 C310 122.8(2) . . ? O301 C301 C302 118.3(2) . . ? C310 C301 C302 118.8(2) . . ? C216 O203 C219 115.88(19) . . ? C315 C314 C313 120.8(2) . . ? C301 C310 C311 120.5(2) . . ? C301 C310 C309 119.3(2) . . ? C311 C310 C309 119.4(2) . . ? C308 N302 N301 116.36(18) . . ? C308 O302 Ce1 119.95(14) . . ? C148 O106 Ce2 138.84(15) . . ? C248 O206 Ce2 131.15(14) . . ? C348 O306 Ce2 140.64(13) . . ? C237 O205 Ce2 117.99(14) . . ? C301 O301 Ce1 144.32(14) . . ? C201 O201 Ce1 144.69(14) . . ? C208 O202 Ce1 124.35(13) . . ? C108 N102 N101 116.12(18) . . ? C211 N201 N202 115.43(19) . . ? C211 N201 Ce1 131.01(15) . . ? N202 N201 Ce1 113.02(12) . . ? C342 C341 C340 122.3(2) . . ? C148 C139 C138 120.43(19) . . ? C148 C139 C140 119.8(2) . . ? C138 C139 C140 119.5(2) . . ? C305 C304 C309 119.9(2) . . ? C305 C304 C303 121.8(2) . . ? C309 C304 C303 118.4(2) . . ? N301 C311 C310 124.3(2) . . ? C208 N202 N201 117.23(19) . . ? C103 C102 C101 121.7(2) . . ? C141 C140 C145 116.86(19) . . ? C141 C140 C139 124.0(2) . . ? C145 C140 C139 119.1(2) . . ? O201 C201 C210 122.9(2) . . ? O201 C201 C202 117.1(2) . . ? C210 C201 C202 119.9(2) . . ? N104 C138 C139 123.6(2) . . ? C137 N103 N104 116.10(18) . . ? C311 N301 N302 116.13(19) . . ? C311 N301 Ce1 131.04(15) . . ? N302 N301 Ce1 112.45(13) . . ? C248 C239 C240 119.79(19) . . ? C248 C239 C238 120.7(2) . . ? C240 C239 C238 119.4(2) . . ? C138 N104 N103 115.59(18) . . ? C138 N104 Ce2 131.21(15) . . ? N103 N104 Ce2 113.14(12) . . ? O305 C337 N303 120.0(2) . . ? O305 C337 C334 121.5(2) . . ? N303 C337 C334 118.2(2) . . ? C104 C109 C112 116.7(2) . . ? C104 C109 C110 119.16(19) . . ? C112 C109 C110 124.17(19) . . ? C237 N203 N204 115.52(19) . . ? C241 C240 C245 117.1(2) . . ? C241 C240 C239 123.3(2) . . ? C245 C240 C239 119.6(2) . . ? C238 N204 N203 115.47(19) . . ? C238 N204 Ce2 129.36(14) . . ? N203 N204 Ce2 115.16(13) . . ? C102 C103 C104 121.4(2) . . ? C212 C209 C204 117.7(2) . . ? C212 C209 C210 123.3(2) . . ? C204 C209 C210 119.0(2) . . ? O102 C108 N102 120.95(19) . . ? O102 C108 C113 121.6(2) . . ? N102 C108 C113 117.4(2) . . ? O206 C248 C239 123.20(19) . . ? O206 C248 C247 117.0(2) . . ? C239 C248 C247 119.8(2) . . ? C111 N101 N102 115.41(17) . . ? C111 N101 Ce1 131.62(13) . . ? N102 N101 Ce1 112.79(12) . . ? C346 C347 C348 120.4(2) . . ? C304 C309 C312 117.1(2) . . ? C304 C309 C310 119.6(2) . . ? C312 C309 C310 123.3(2) . . ? C106 C105 C104 120.4(2) . . ? C146 C147 C148 121.4(2) . . ? C344 C345 C346 122.2(2) . . ? C344 C345 C340 119.5(2) . . ? C346 C345 C340 118.2(2) . . ? O203 C216 C217 116.2(2) . . ? O203 C216 C215 124.2(2) . . ? C217 C216 C215 119.6(2) . . ? C318 C313 C314 118.4(2) . . ? C318 C313 C308 123.6(2) . . ? C314 C313 C308 117.3(2) . . ? N101 C111 C110 122.91(19) . . ? C348 C339 C338 121.3(2) . . ? C348 C339 C340 119.79(19) . . ? C338 C339 C340 118.9(2) . . ? C303 C302 C301 122.5(2) . . ? O106 C148 C139 122.2(2) . . ? O106 C148 C147 118.3(2) . . ? C139 C148 C147 119.5(2) . . ? O205 C237 N203 119.25(19) . . ? O205 C237 C234 120.7(2) . . ? N203 C237 C234 120.0(2) . . ? C341 C340 C345 116.2(2) . . ? C341 C340 C339 124.9(2) . . ? C345 C340 C339 118.8(2) . . ? C246 C247 C248 120.1(2) . . ? C337 N303 N304 115.4(2) . . ? O306 C348 C339 122.14(19) . . ? O306 C348 C347 117.3(2) . . ? C339 C348 C347 120.5(2) . . ? C347 C346 C345 122.0(2) . . ? C133 C134 C135 119.0(2) . . ? C133 C134 C137 118.0(2) . . ? C135 C134 C137 123.0(2) . . ? C101 C110 C111 121.3(2) . . ? C101 C110 C109 119.54(18) . . ? C111 C110 C109 119.16(19) . . ? C142 C141 C140 121.4(2) . . ? C214 C213 C218 117.6(2) . . ? C214 C213 C208 117.5(2) . . ? C218 C213 C208 124.5(2) . . ? C307 C312 C309 120.5(2) . . ? C203 C204 C205 121.4(2) . . ? C203 C204 C209 119.3(2) . . ? C205 C204 C209 119.3(2) . . ? C107 C112 C109 121.6(2) . . ? C201 C210 C211 121.01(19) . . ? C201 C210 C209 119.4(2) . . ? C211 C210 C209 119.4(2) . . ? C235 C234 C233 117.8(2) . . ? C235 C234 C237 123.1(2) . . ? C233 C234 C237 118.7(2) . . ? N201 C211 C210 125.9(2) . . ? C242 C241 C240 121.9(2) . . ? C314 C315 C316 121.2(2) . . ? C147 C146 C145 121.7(2) . . ? O302 C308 N302 119.9(2) . . ? O302 C308 C313 119.7(2) . . ? N302 C308 C313 120.2(2) . . ? C214 C215 C216 118.3(2) . . ? O202 C208 N202 118.48(19) . . ? O202 C208 C213 120.45(19) . . ? N202 C208 C213 120.8(2) . . ? C141 C142 C143 120.8(2) . . ? C118 C113 C114 118.4(2) . . ? C118 C113 C108 122.3(2) . . ? C114 C113 C108 119.0(2) . . ? C112 C107 C106 120.6(2) . . ? C144 C143 C142 119.2(2) . . ? C243 C244 C245 121.7(2) . . ? C213 C214 C215 122.7(2) . . ? N204 C238 C239 122.7(2) . . ? C218 C217 C216 120.2(2) . . ? C306 C305 C304 121.3(2) . . ? C244 C243 C242 119.9(2) . . ? C105 C106 C107 120.3(2) . . ? C333 C334 C335 118.7(2) . . ? C333 C334 C337 118.0(2) . . ? C335 C334 C337 122.9(2) . . ? C207 C212 C209 120.9(2) . . ? C343 C344 C345 122.2(2) . . ? C331 C332 C333 120.1(2) . . ? C244 C245 C246 122.2(2) . . ? C244 C245 C240 119.5(2) . . ? C246 C245 C240 118.3(2) . . ? O105 C137 N103 118.96(19) . . ? O105 C137 C134 120.41(19) . . ? N103 C137 C134 120.5(2) . . ? C202 C203 C204 122.1(2) . . ? C241 C242 C243 119.9(2) . . ? N304 C338 C339 125.4(2) . . ? C143 C144 C145 121.3(2) . . ? C217 C218 C213 121.5(2) . . ? C344 C343 C342 119.1(2) . . ? C332 C333 C334 120.7(2) . . ? C236 C235 C234 120.4(2) . . ? C317 C318 C313 120.6(2) . . ? C144 C145 C146 121.3(2) . . ? C144 C145 C140 120.1(2) . . ? C146 C145 C140 118.5(2) . . ? C203 C202 C201 120.1(2) . . ? C305 C306 C307 119.5(2) . . ? C232 C233 C234 121.0(2) . . ? C231 O204 C230 117.58(18) . . ? C316 O303 C319 117.24(19) . . ? C331 O304 C330 117.6(2) . . ? C116 O103 C119 116.2(2) . . ? C131 O104 C130 116.12(19) . . ? C116 C115 C114 120.0(2) . . ? C233 C232 C231 120.7(2) . . ? C316 C317 C318 121.3(2) . . ? O204 C231 C236 125.6(2) . . ? O204 C231 C232 115.2(2) . . ? C236 C231 C232 119.2(2) . . ? C302 C303 C304 121.3(2) . . ? C207 C206 C205 119.5(2) . . ? C332 C331 O304 126.0(2) . . ? C332 C331 C336 120.5(2) . . ? O304 C331 C336 113.5(2) . . ? C231 C236 C235 121.0(2) . . ? O303 C316 C317 126.2(2) . . ? O303 C316 C315 116.1(2) . . ? C317 C316 C315 117.7(2) . . ? C115 C114 C113 121.3(2) . . ? C125 C120 C121 121.7(2) . . ? C125 C120 C119 119.3(2) . . ? C121 C120 C119 119.0(2) . . ? C325 C324 C323 119.3(2) . . ? C325 C324 C328 119.1(2) . . ? C323 C324 C328 121.5(2) . . ? C206 C205 C204 120.9(2) . . ? C312 C307 C306 121.6(2) . . ? C134 C133 C132 121.7(2) . . ? C120 C121 C122 119.3(2) . . ? C120 C121 C126 121.8(3) . . ? C122 C121 C126 118.9(3) . . ? O103 C119 C120 106.5(2) . . ? C321 C322 C323 118.4(2) . . ? C321 C322 C327 120.7(2) . . ? C323 C322 C327 120.9(2) . . ? C120 C125 C124 119.3(2) . . ? C120 C125 C129 121.9(2) . . ? C124 C125 C129 118.8(2) . . ? C324 C323 C322 121.6(2) . . ? C324 C323 C330 119.4(2) . . ? C322 C323 C330 118.9(2) . . ? C223 C222 C221 120.7(2) . . ? C223 C222 C227 119.2(2) . . ? C221 C222 C227 120.0(2) . . ? C335 C336 C331 119.6(3) . . ? O203 C219 C220 109.6(2) . . ? O304 C330 C323 107.6(2) . . ? C320 C325 C324 119.5(2) . . ? C320 C325 C329 120.9(2) . . ? C324 C325 C329 119.6(2) . . ? C123 C124 C125 120.1(2) . . ? C123 C124 C128 121.6(2) . . ? C125 C124 C128 118.3(2) . . ? C222 C223 C224 120.6(2) . . ? C222 C223 C230 119.3(2) . . ? C224 C223 C230 120.1(2) . . ? O104 C131 C132 114.7(2) . . ? O104 C131 C136 124.6(2) . . ? C132 C131 C136 120.7(2) . . ? C13 N11 C12 121.2(3) . . ? C13 N11 C11 121.2(3) . . ? C12 N11 C11 117.5(3) . . ? C115 C116 O103 116.9(2) . . ? C115 C116 C117 119.9(2) . . ? O103 C116 C117 123.0(2) . . ? C131 C132 C133 118.5(2) . . ? C220 C221 C222 118.0(2) . . ? C220 C221 C226 122.2(2) . . ? C222 C221 C226 119.8(2) . . ? C134 C135 C136 120.2(2) . . ? C225 C224 C223 119.4(2) . . ? C225 C224 C228 118.3(2) . . ? C223 C224 C228 122.3(2) . . ? C325 C320 C321 120.9(2) . . ? C325 C320 C319 119.9(2) . . ? C321 C320 C319 119.2(2) . . ? C221 C220 C225 121.4(2) . . ? C221 C220 C219 119.5(2) . . ? C225 C220 C219 119.1(2) . . ? C206 C207 C212 121.6(3) . . ? C123 C122 C121 118.0(2) . . ? C123 C122 C127 122.9(3) . . ? C121 C122 C127 119.1(3) . . ? C03 N01 C02 121.6(3) . . ? C03 N01 C01 122.2(3) . . ? C02 N01 C01 116.1(3) . . ? C343 C342 C341 120.5(2) . . ? C23 N21 C22 123.4(3) . . ? C23 N21 C21 118.5(3) . . ? C22 N21 C21 118.1(3) . . ? O204 C230 C223 105.7(2) . . ? C224 C225 C220 119.7(2) . . ? C224 C225 C229 119.8(2) . . ? C220 C225 C229 120.5(2) . . ? O303 C319 C320 107.1(2) . . ? C336 C335 C334 120.3(2) . . ? C322 C321 C320 120.2(2) . . ? C322 C321 C326 119.1(2) . . ? C320 C321 C326 120.6(2) . . ? O11 C13 N11 126.0(3) . . ? O21 C23 N21 125.7(4) . . ? C113 C118 C117 122.2(3) . . ? C124 C123 C122 121.0(2) . . ? C124 C123 C130 118.8(2) . . ? C122 C123 C130 120.0(2) . . ? C131 C136 C135 119.8(3) . . ? O01 C03 N01 125.9(3) . . ? C118 C117 C116 117.5(3) . . ? O104 C130 C123 109.2(2) . . ? C401 N401 C402 112.8(4) . . ? C401 N401 C403 122.6(4) . . ? C402 N401 C403 124.5(4) . . ? O401 C403 N401 107.9(4) . . ? C33 N31 C31 118.4(4) . . ? C33 N31 C32 113.6(4) . . ? C31 N31 C32 127.8(4) . . ? O31 C33 N31 124.7(5) . . ? C43 N41 C42 122.7(3) . . ? C43 N41 C41 119.4(4) . . ? C42 N41 C41 117.9(4) . . ? O41 C43 N41 123.2(4) . . ? C53 N51 C51 120.8(3) . . ? C53 N51 C52 120.5(3) . . ? C51 N51 C52 118.7(3) . . ? O51 C53 N51 125.5(3) . . ? C63 N61 C61 123.9(3) . . ? C63 N61 C62 116.5(3) . . ? C61 N61 C62 119.6(3) . . ? O61 C63 N61 124.0(4) . . ? C73 N71 C71 122.2(3) . . ? C73 N71 C72 121.1(3) . . ? C71 N71 C72 116.6(3) . . ? O71 C73 N71 123.2(3) . . ? C83 N81 C81 131.5(5) . . ? C83 N81 C82 114.8(5) . . ? C81 N81 C82 113.6(5) . . ? O81 C83 N81 111.7(5) . . ? C91 N91 C92 119.7(6) . . ? C91 N91 C93 143.1(6) . . ? C92 N91 C93 97.2(5) . . ? O91' C93 O91 29.1(7) . . ? O91' C93 N91 106.6(7) . . ? O91 C93 N91 106.3(8) . . ? C413 N411 C41' 99.2(5) . . ? C413 N411 C412 119.0(4) . . ? C41' N411 C412 141.4(5) . . ? C413 N411 C411 145.5(5) . . ? C41' N411 C411 46.6(5) . . ? C412 N411 C411 95.5(5) . . ? O411 C413 N411 142.1(5) . . ? O3 N1 O2 120.6(5) . . ? O3 N1 O1 120.6(6) . . ? O2 N1 O1 118.8(5) . . ? O5 N2 O6 122.6(4) . . ? O5 N2 O4 130.0(4) . . ? O6 N2 O4 107.3(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.064 _refine_diff_density_min -1.743 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 947249'