data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Polly Arnold' _publ_contact_author_email POLLY.ARNOLD@ED.AC.UK _publ_section_title ; Constructing cerium supramolecular wheels and encapsulating uranium with a Schiff-base calixpyrrole ligand ; loop_ _publ_author_name 'Polly Arnold' 'Christopher D. Carmichael' 'Jason B. Love' 'Natalie A. Potter' 'Paul Roussel' 'Alexandra Slawin' # Attachment 'combinednew.cif' data_jl8025_CeHL3 _database_code_depnum_ccdc_archive 'CCDC 727811' #TrackingRef 'combinednew.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C138 H142 Ce3 N24, C60 H60' _chemical_formula_sum 'C198 H202 Ce3 N24' _chemical_formula_weight 3338.20 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' Ce Ce -0.2486 2.6331 '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' _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 19.2737(5) _cell_length_b 20.1203(6) _cell_length_c 22.5956(6) _cell_angle_alpha 75.830(2) _cell_angle_beta 86.608(2) _cell_angle_gamma 83.598(2) _cell_volume 8438.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9690 _cell_measurement_theta_min 4.9 _cell_measurement_theta_max 61.0 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4614 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details SADABS _exptl_special_details ; Grown from a saturated solution of C6D6. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 131903 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 30.55 _reflns_number_total 46583 _reflns_number_gt 36691 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure contains disordered benzene molecules and disordered ethyl groups. This leads to large anisoptropic displacemtent parameters and therefore large ratios. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+24.4632P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 46583 _refine_ls_number_parameters 1950 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 C1 C 1.4863(2) 1.0334(2) 0.8856(2) 0.0242(9) Uani 1 1 d . . . H1 H 1.5158 0.9947 0.9063 0.029 Uiso 1 1 calc R . . C2 C 1.5059(2) 1.0704(2) 0.8271(2) 0.0239(9) Uani 1 1 d . . . C3 C 1.5619(3) 1.0527(3) 0.7894(2) 0.0357(12) Uani 1 1 d . . . H3 H 1.5973 1.0154 0.7998 0.043 Uiso 1 1 calc R . . C4 C 1.5549(3) 1.1008(3) 0.7338(2) 0.0383(13) Uani 1 1 d . . . H4 H 1.5850 1.1028 0.6987 0.046 Uiso 1 1 calc R . . C5 C 1.4951(2) 1.1460(3) 0.7392(2) 0.0280(10) Uani 1 1 d . A . C6 C 1.4670(3) 1.2067(3) 0.6897(2) 0.0292(11) Uani 1 1 d . . . C7 C 1.4989(3) 1.2008(3) 0.6267(2) 0.0422(14) Uani 1 1 d . A . C8 C 1.4811(3) 1.1377(4) 0.6054(3) 0.0506(17) Uani 1 1 d . . . H8A H 1.5003 1.0954 0.6337 0.076 Uiso 1 1 calc R A . H8B H 1.5015 1.1394 0.5644 0.076 Uiso 1 1 calc R . . H8C H 1.4303 1.1381 0.6046 0.076 Uiso 1 1 calc R . . C9 C 1.4802(4) 1.2783(4) 0.7032(4) 0.032(2) Uani 0.692(11) 1 d PU A 1 H9A H 1.4673 1.3158 0.6671 0.038 Uiso 0.692(11) 1 calc PR A 1 H9B H 1.4492 1.2860 0.7379 0.038 Uiso 0.692(11) 1 calc PR A 1 C10 C 1.5558(4) 1.2822(5) 0.7182(5) 0.047(3) Uani 0.692(11) 1 d PU A 1 H10A H 1.5699 1.2439 0.7527 0.071 Uiso 0.692(11) 1 calc PR A 1 H10B H 1.5594 1.3260 0.7290 0.071 Uiso 0.692(11) 1 calc PR A 1 H10C H 1.5864 1.2794 0.6825 0.071 Uiso 0.692(11) 1 calc PR A 1 C9A C 1.5089(9) 1.2606(9) 0.7046(8) 0.031(5) Uani 0.308(11) 1 d PU A 2 H9A1 H 1.4984 1.2638 0.7473 0.038 Uiso 0.308(11) 1 calc PR A 2 H9A2 H 1.5596 1.2470 0.7002 0.038 Uiso 0.308(11) 1 calc PR A 2 C10A C 1.4895(11) 1.3302(10) 0.6611(8) 0.042(5) Uani 0.308(11) 1 d PU A 2 H10D H 1.5034 1.3277 0.6192 0.063 Uiso 0.308(11) 1 calc PR A 2 H10E H 1.5136 1.3655 0.6722 0.063 Uiso 0.308(11) 1 calc PR A 2 H10F H 1.4389 1.3421 0.6638 0.063 Uiso 0.308(11) 1 calc PR A 2 C11 C 1.3880(2) 1.2140(2) 0.6873(2) 0.0251(10) Uani 1 1 d . A . C12 C 1.3483(3) 1.2342(3) 0.6346(2) 0.0324(11) Uani 1 1 d . . . H12 H 1.3660 1.2454 0.5936 0.039 Uiso 1 1 calc R A . C13 C 1.2787(3) 1.2347(3) 0.6533(2) 0.0326(11) Uani 1 1 d . A . H13 H 1.2395 1.2455 0.6279 0.039 Uiso 1 1 calc R . . C14 C 1.2776(2) 1.2163(2) 0.7170(2) 0.0236(9) Uani 1 1 d . . . C15 C 1.2187(2) 1.2163(2) 0.7567(2) 0.0241(9) Uani 1 1 d . A . H15 H 1.1737 1.2218 0.7402 0.029 Uiso 1 1 calc R . . C16 C 1.1653(2) 1.2293(2) 0.8506(2) 0.0198(9) Uani 1 1 d . . . C17 C 1.1658(2) 1.1986(2) 0.9129(2) 0.0234(9) Uani 1 1 d . . . H17 H 1.2005 1.1616 0.9273 0.028 Uiso 1 1 calc R . . C18 C 1.1220(3) 1.1831(3) 1.0216(2) 0.0361(12) Uani 1 1 d . . . H18A H 1.1301 1.2162 1.0453 0.054 Uiso 1 1 calc R . . H18B H 1.1605 1.1463 1.0271 0.054 Uiso 1 1 calc R . . H18C H 1.0780 1.1634 1.0356 0.054 Uiso 1 1 calc R . . C19 C 1.1180(2) 1.2192(3) 0.9553(2) 0.0258(10) Uani 1 1 d . . . C20 C 1.0675(2) 1.2738(3) 0.9344(2) 0.0266(10) Uani 1 1 d . . . C21 C 1.0152(3) 1.2999(3) 0.9781(2) 0.0369(12) Uani 1 1 d . . . H21A H 0.9906 1.2617 1.0022 0.055 Uiso 1 1 calc R . . H21B H 0.9814 1.3353 0.9548 0.055 Uiso 1 1 calc R . . H21C H 1.0397 1.3198 1.0054 0.055 Uiso 1 1 calc R . . C22 C 1.0650(2) 1.3041(3) 0.8724(2) 0.0259(10) Uani 1 1 d . . . H22 H 1.0295 1.3405 0.8584 0.031 Uiso 1 1 calc R . . C23 C 1.1124(2) 1.2834(2) 0.8296(2) 0.0200(9) Uani 1 1 d . . . C24 C 1.1446(2) 1.3536(2) 0.7333(2) 0.0254(10) Uani 1 1 d . . . H24 H 1.1309 1.3723 0.6924 0.030 Uiso 1 1 calc R . . C25 C 1.2107(2) 1.3725(3) 0.7455(2) 0.0276(10) Uani 1 1 d . . . C26 C 1.2575(3) 1.4038(3) 0.7010(3) 0.0388(13) Uani 1 1 d . . . H26 H 1.2497 1.4193 0.6584 0.047 Uiso 1 1 calc R . . C27 C 1.3178(3) 1.4082(3) 0.7301(3) 0.0388(13) Uani 1 1 d . . . H27 H 1.3588 1.4270 0.7108 0.047 Uiso 1 1 calc R . . C28 C 1.3079(2) 1.3808(2) 0.7916(2) 0.0271(10) Uani 1 1 d . . . C29 C 1.3539(2) 1.3748(2) 0.8451(2) 0.0280(10) Uani 1 1 d . . . C30 C 1.3560(3) 1.4465(3) 0.8572(3) 0.0418(14) Uani 1 1 d . . . H30A H 1.3074 1.4653 0.8645 0.050 Uiso 1 1 calc R . . H30B H 1.3811 1.4406 0.8954 0.050 Uiso 1 1 calc R . . C31 C 1.3899(3) 1.5000(3) 0.8078(3) 0.0524(17) Uani 1 1 d . . . H31A H 1.4372 1.4814 0.7980 0.079 Uiso 1 1 calc R . . H31B H 1.3921 1.5417 0.8224 0.079 Uiso 1 1 calc R . . H31C H 1.3621 1.5113 0.7710 0.079 Uiso 1 1 calc R . . C32 C 1.4274(3) 1.3440(3) 0.8307(3) 0.0412(14) Uani 1 1 d . . . H32A H 1.4243 1.2978 0.8235 0.049 Uiso 1 1 calc R . . H32B H 1.4456 1.3733 0.7924 0.049 Uiso 1 1 calc R . . C33 C 1.4793(3) 1.3372(4) 0.8810(4) 0.064(2) Uani 1 1 d . . . H33A H 1.4859 1.3831 0.8860 0.096 Uiso 1 1 calc R . . H33B H 1.5242 1.3147 0.8698 0.096 Uiso 1 1 calc R . . H33C H 1.4611 1.3095 0.9195 0.096 Uiso 1 1 calc R . . C34 C 1.3242(2) 1.3276(3) 0.9018(2) 0.0281(10) Uani 1 1 d . . . C35 C 1.2901(3) 1.3480(3) 0.9525(3) 0.0353(12) Uani 1 1 d . . . H35 H 1.2773 1.3939 0.9560 0.042 Uiso 1 1 calc R . . C36 C 1.2792(3) 1.2884(3) 0.9960(2) 0.0340(12) Uani 1 1 d . . . H36 H 1.2578 1.2852 1.0354 0.041 Uiso 1 1 calc R . . C37 C 1.3058(2) 1.2336(3) 0.9707(2) 0.0276(10) Uani 1 1 d . . . C38 C 1.3133(2) 1.1633(3) 0.9999(2) 0.0244(9) Uani 1 1 d . . . H38 H 1.3026 1.1492 1.0424 0.029 Uiso 1 1 calc R . . C39 C 1.3530(2) 1.0480(2) 0.9992(2) 0.0228(9) Uani 1 1 d . . . C40 C 1.3230(2) 1.0126(3) 1.0542(2) 0.0249(10) Uani 1 1 d . . . H40 H 1.2877 1.0363 1.0748 0.030 Uiso 1 1 calc R . . C41 C 1.3435(3) 0.9441(3) 1.0792(2) 0.0292(11) Uani 1 1 d . . . C42 C 1.3067(3) 0.9067(3) 1.1369(2) 0.0386(13) Uani 1 1 d . . . H42A H 1.2731 0.9395 1.1521 0.058 Uiso 1 1 calc R . . H42B H 1.3412 0.8859 1.1680 0.058 Uiso 1 1 calc R . . H42C H 1.2819 0.8706 1.1278 0.058 Uiso 1 1 calc R . . C43 C 1.3971(3) 0.9095(2) 1.0501(2) 0.0289(10) Uani 1 1 d . . . C44 C 1.4234(3) 0.8354(3) 1.0777(3) 0.0399(13) Uani 1 1 d . . . H44A H 1.3860 0.8059 1.0784 0.060 Uiso 1 1 calc R . . H44B H 1.4378 0.8309 1.1195 0.060 Uiso 1 1 calc R . . H44C H 1.4634 0.8213 1.0531 0.060 Uiso 1 1 calc R . . C45 C 1.4266(2) 0.9447(2) 0.9952(2) 0.0256(10) Uani 1 1 d . . . H45 H 1.4628 0.9213 0.9753 0.031 Uiso 1 1 calc R . . C46 C 1.4044(2) 1.0129(2) 0.9688(2) 0.0212(9) Uani 1 1 d . . . C101 C 0.9707(2) 1.4761(2) 0.7488(2) 0.0252(10) Uani 1 1 d . . . H101 H 0.9782 1.5223 0.7476 0.030 Uiso 1 1 calc R . . C102 C 0.9276(2) 1.4400(2) 0.7953(2) 0.0257(10) Uani 1 1 d . . . C103 C 0.8971(3) 1.4599(3) 0.8461(3) 0.0367(12) Uani 1 1 d . . . H103 H 0.8974 1.5035 0.8552 0.044 Uiso 1 1 calc R . . C104 C 0.8658(3) 1.4036(3) 0.8812(2) 0.0340(12) Uani 1 1 d . . . H104 H 0.8410 1.4011 0.9192 0.041 Uiso 1 1 calc R . . C105 C 0.8780(2) 1.3510(2) 0.8497(2) 0.0234(9) Uani 1 1 d . . . C106 C 0.8551(2) 1.2787(2) 0.8675(2) 0.0229(9) Uani 1 1 d . . . C107 C 0.7992(2) 1.2732(3) 0.8229(2) 0.0269(10) Uani 1 1 d . . . H10G H 0.8204 1.2819 0.7811 0.032 Uiso 1 1 calc R . . H10H H 0.7861 1.2254 0.8336 0.032 Uiso 1 1 calc R . . C108 C 0.7329(3) 1.3224(3) 0.8227(2) 0.0385(13) Uani 1 1 d . . . H10I H 0.7101 1.3128 0.8634 0.058 Uiso 1 1 calc R . . H10J H 0.7011 1.3159 0.7928 0.058 Uiso 1 1 calc R . . H10K H 0.7450 1.3700 0.8117 0.058 Uiso 1 1 calc R . . C109 C 0.8246(2) 1.2644(3) 0.9339(2) 0.0286(10) Uani 1 1 d . . . H10L H 0.8632 1.2618 0.9617 0.034 Uiso 1 1 calc R . . H10M H 0.7911 1.3042 0.9380 0.034 Uiso 1 1 calc R . . C110 C 0.7877(3) 1.1989(3) 0.9552(2) 0.0362(12) Uani 1 1 d . . . H11A H 0.7429 1.2053 0.9351 0.054 Uiso 1 1 calc R . . H11B H 0.7795 1.1891 0.9996 0.054 Uiso 1 1 calc R . . H11C H 0.8170 1.1602 0.9446 0.054 Uiso 1 1 calc R . . C111 C 0.9169(2) 1.2272(2) 0.8619(2) 0.0225(9) Uani 1 1 d . . . C112 C 0.9502(2) 1.1751(2) 0.9069(2) 0.0269(10) Uani 1 1 d . . . H112 H 0.9379 1.1646 0.9493 0.032 Uiso 1 1 calc R . . C113 C 1.0041(3) 1.1416(3) 0.8794(2) 0.0290(10) Uani 1 1 d . . . H113 H 1.0356 1.1037 0.8986 0.035 Uiso 1 1 calc R . . C114 C 1.0030(2) 1.1747(2) 0.8170(2) 0.0229(9) Uani 1 1 d . . . C115 C 1.0449(2) 1.1590(2) 0.7683(2) 0.0232(9) Uani 1 1 d . . . H115 H 1.0784 1.1198 0.7756 0.028 Uiso 1 1 calc R . . C116 C 1.0683(2) 1.1746(2) 0.6613(2) 0.0212(9) Uani 1 1 d . . . C117 C 1.0952(2) 1.2243(2) 0.6141(2) 0.0238(9) Uani 1 1 d . . . H117 H 1.0971 1.2689 0.6206 0.029 Uiso 1 1 calc R . . C118 C 1.1197(2) 1.2128(3) 0.5579(2) 0.0259(10) Uani 1 1 d . . . C119 C 1.1491(3) 1.2691(3) 0.5106(2) 0.0392(13) Uani 1 1 d . . . H11D H 1.1450 1.3112 0.5255 0.059 Uiso 1 1 calc R . . H11E H 1.1232 1.2775 0.4730 0.059 Uiso 1 1 calc R . . H11F H 1.1984 1.2555 0.5022 0.059 Uiso 1 1 calc R . . C120 C 1.1158(2) 1.1475(3) 0.5476(2) 0.0270(10) Uani 1 1 d . . . C121 C 1.1402(3) 1.1317(3) 0.4873(2) 0.0364(12) Uani 1 1 d . . . H12A H 1.1358 1.0832 0.4892 0.055 Uiso 1 1 calc R . . H12B H 1.1892 1.1408 0.4789 0.055 Uiso 1 1 calc R . . H12C H 1.1115 1.1610 0.4547 0.055 Uiso 1 1 calc R . . C122 C 1.0900(2) 1.0969(2) 0.5946(2) 0.0254(10) Uani 1 1 d . . . H122 H 1.0885 1.0523 0.5879 0.030 Uiso 1 1 calc R . . C123 C 1.0661(2) 1.1085(2) 0.6509(2) 0.0225(9) Uani 1 1 d . . . C124 C 0.9895(2) 1.0469(2) 0.7275(2) 0.0260(10) Uani 1 1 d . . . H124 H 0.9875 1.0074 0.7605 0.031 Uiso 1 1 calc R . . C125 C 0.9268(2) 1.0922(2) 0.7212(2) 0.0241(9) Uani 1 1 d . . . C126 C 0.8692(2) 1.0874(3) 0.7613(2) 0.0298(11) Uani 1 1 d . . . H126 H 0.8649 1.0532 0.7983 0.036 Uiso 1 1 calc R . . C127 C 0.8194(2) 1.1406(2) 0.7381(2) 0.0275(10) Uani 1 1 d . . . H127 H 0.7751 1.1500 0.7567 0.033 Uiso 1 1 calc R . . C128 C 0.8453(2) 1.1783(2) 0.6825(2) 0.0216(9) Uani 1 1 d . . . C129 C 0.8115(2) 1.2364(2) 0.6344(2) 0.0210(9) Uani 1 1 d . . . C130 C 0.7655(2) 1.2057(3) 0.5958(2) 0.0242(10) Uani 1 1 d . . . H13A H 0.7456 1.2435 0.5625 0.029 Uiso 1 1 calc R . . H13B H 0.7957 1.1732 0.5766 0.029 Uiso 1 1 calc R . . C131 C 0.7058(2) 1.1682(3) 0.6310(3) 0.0350(12) Uani 1 1 d . . . H13C H 0.7248 1.1257 0.6591 0.053 Uiso 1 1 calc R . . H13D H 0.6755 1.1569 0.6023 0.053 Uiso 1 1 calc R . . H13E H 0.6786 1.1979 0.6543 0.053 Uiso 1 1 calc R . . C132 C 0.7671(2) 1.2880(2) 0.6651(2) 0.0219(9) Uani 1 1 d . . . H13F H 0.7370 1.2621 0.6977 0.026 Uiso 1 1 calc R . . H13G H 0.7989 1.3109 0.6848 0.026 Uiso 1 1 calc R . . C133 C 0.7210(3) 1.3433(3) 0.6223(2) 0.0316(11) Uani 1 1 d . . . H13H H 0.7497 1.3679 0.5885 0.047 Uiso 1 1 calc R . . H13I H 0.6978 1.3760 0.6448 0.047 Uiso 1 1 calc R . . H13J H 0.6856 1.3218 0.6060 0.047 Uiso 1 1 calc R . . C134 C 0.8688(2) 1.2719(2) 0.5928(2) 0.0198(8) Uani 1 1 d . . . C135 C 0.8801(2) 1.2747(3) 0.5308(2) 0.0281(10) Uani 1 1 d . . . H135 H 0.8558 1.2522 0.5072 0.034 Uiso 1 1 calc R . . C136 C 0.9334(3) 1.3165(3) 0.5100(2) 0.0301(11) Uani 1 1 d . . . H136 H 0.9522 1.3289 0.4695 0.036 Uiso 1 1 calc R . . C137 C 0.9538(2) 1.3367(2) 0.5609(2) 0.0219(9) Uani 1 1 d . . . C138 C 1.0015(2) 1.3839(2) 0.5613(2) 0.0226(9) Uani 1 1 d . . . H138 H 1.0214 1.4076 0.5236 0.027 Uiso 1 1 calc R . . C139 C 1.0594(2) 1.4507(2) 0.6120(2) 0.0222(9) Uani 1 1 d . . . C140 C 1.1104(2) 1.4749(2) 0.5680(2) 0.0245(9) Uani 1 1 d . . . H140 H 1.1176 1.4562 0.5331 0.029 Uiso 1 1 calc R . . C141 C 1.1509(2) 1.5259(2) 0.5739(2) 0.0270(10) Uani 1 1 d . . . C142 C 1.2074(3) 1.5488(3) 0.5267(3) 0.0397(13) Uani 1 1 d . . . H14A H 1.2064 1.5254 0.4936 0.060 Uiso 1 1 calc R . . H14B H 1.2530 1.5373 0.5457 0.060 Uiso 1 1 calc R . . H14C H 1.1996 1.5988 0.5102 0.060 Uiso 1 1 calc R . . C143 C 1.1394(3) 1.5540(2) 0.6251(2) 0.0285(10) Uani 1 1 d . . . C144 C 1.1843(3) 1.6066(3) 0.6343(3) 0.0419(14) Uani 1 1 d . . . H14D H 1.1700 1.6196 0.6726 0.063 Uiso 1 1 calc R . . H14E H 1.1791 1.6474 0.6002 0.063 Uiso 1 1 calc R . . H14F H 1.2333 1.5870 0.6362 0.063 Uiso 1 1 calc R . . C145 C 1.0879(2) 1.5305(2) 0.6684(2) 0.0261(10) Uani 1 1 d . . . H145 H 1.0800 1.5499 0.7029 0.031 Uiso 1 1 calc R . . C146 C 1.0476(2) 1.4792(2) 0.6627(2) 0.0217(9) Uani 1 1 d . . . C201 C 1.0061(2) 0.9210(2) 0.5970(2) 0.0272(10) Uani 1 1 d . . . H201 H 0.9624 0.9194 0.5803 0.033 Uiso 1 1 calc R . . C202 C 1.0668(2) 0.9243(2) 0.5592(2) 0.0251(10) Uani 1 1 d . . . C203 C 1.0745(3) 0.9296(3) 0.4965(2) 0.0307(11) Uani 1 1 d . . . H203 H 1.0386 0.9303 0.4692 0.037 Uiso 1 1 calc R . . C204 C 1.1446(3) 0.9337(3) 0.4821(2) 0.0298(11) Uani 1 1 d . . . H204 H 1.1665 0.9374 0.4428 0.036 Uiso 1 1 calc R . . C205 C 1.1780(2) 0.9312(2) 0.5365(2) 0.0251(10) Uani 1 1 d . . . C206 C 1.2546(3) 0.9314(3) 0.5470(2) 0.0279(10) Uani 1 1 d . . . C207 C 1.2952(3) 0.9452(3) 0.4850(2) 0.0377(13) Uani 1 1 d . . . H20A H 1.2813 0.9139 0.4612 0.045 Uiso 1 1 calc R . . H20B H 1.2810 0.9930 0.4622 0.045 Uiso 1 1 calc R . . C208 C 1.3753(3) 0.9357(4) 0.4891(3) 0.0531(17) Uani 1 1 d . . . H20C H 1.3891 0.9590 0.5192 0.080 Uiso 1 1 calc R . . H20D H 1.3965 0.9556 0.4491 0.080 Uiso 1 1 calc R . . H20E H 1.3912 0.8865 0.5016 0.080 Uiso 1 1 calc R . . C209 C 1.2808(3) 0.8611(3) 0.5881(2) 0.0319(11) Uani 1 1 d . . . H20F H 1.3311 0.8613 0.5947 0.038 Uiso 1 1 calc R . . H20G H 1.2560 0.8562 0.6283 0.038 Uiso 1 1 calc R . . C210 C 1.2717(3) 0.7985(3) 0.5646(3) 0.0439(14) Uani 1 1 d . . . H21D H 1.2226 0.7987 0.5556 0.066 Uiso 1 1 calc R . . H21E H 1.2861 0.7567 0.5957 0.066 Uiso 1 1 calc R . . H21F H 1.3006 0.7995 0.5273 0.066 Uiso 1 1 calc R . . C211 C 1.2618(2) 0.9878(3) 0.5797(2) 0.0255(10) Uani 1 1 d . . . C212 C 1.2932(2) 1.0490(3) 0.5586(2) 0.0310(11) Uani 1 1 d . . . H212 H 1.3167 1.0637 0.5202 0.037 Uiso 1 1 calc R . . C213 C 1.2833(2) 1.0842(3) 0.6046(2) 0.0301(11) Uani 1 1 d . . . H213 H 1.2984 1.1278 0.6038 0.036 Uiso 1 1 calc R . . C214 C 1.2466(2) 1.0428(2) 0.6523(2) 0.0221(9) Uani 1 1 d . . . C215 C 1.2271(2) 1.0516(2) 0.7106(2) 0.0221(9) Uani 1 1 d . . . H215 H 1.2380 1.0918 0.7217 0.026 Uiso 1 1 calc R . . C216 C 1.1862(2) 1.0072(2) 0.8121(2) 0.0189(8) Uani 1 1 d . . . C217 C 1.1250(2) 0.9831(2) 0.8424(2) 0.0216(9) Uani 1 1 d . . . H217 H 1.0917 0.9702 0.8190 0.026 Uiso 1 1 calc R . . C218 C 1.1097(2) 0.9769(2) 0.9035(2) 0.0219(9) Uani 1 1 d . . . C219 C 1.0414(3) 0.9507(3) 0.9302(2) 0.0315(11) Uani 1 1 d . . . H21G H 1.0184 0.9812 0.9548 0.047 Uiso 1 1 calc R . . H21H H 1.0504 0.9040 0.9560 0.047 Uiso 1 1 calc R . . H21I H 1.0112 0.9500 0.8970 0.047 Uiso 1 1 calc R . . C220 C 1.1579(2) 0.9959(2) 0.9389(2) 0.0238(9) Uani 1 1 d . . . C221 C 1.1439(3) 0.9950(3) 1.0050(2) 0.0344(12) Uani 1 1 d . . . H22A H 1.1091 1.0334 1.0086 0.052 Uiso 1 1 calc R . . H22B H 1.1873 0.9997 1.0234 0.052 Uiso 1 1 calc R . . H22C H 1.1260 0.9514 1.0261 0.052 Uiso 1 1 calc R . . C222 C 1.2193(2) 1.0196(2) 0.9095(2) 0.0233(9) Uani 1 1 d . . . H222 H 1.2521 1.0328 0.9332 0.028 Uiso 1 1 calc R . . C223 C 1.2357(2) 1.0251(2) 0.8477(2) 0.0195(8) Uani 1 1 d . . . C224 C 1.3455(2) 1.0251(2) 0.7922(2) 0.0236(9) Uani 1 1 d . . . H224 H 1.3828 1.0522 0.7767 0.028 Uiso 1 1 calc R . . C225 C 1.3513(2) 0.9619(2) 0.7743(2) 0.0229(9) Uani 1 1 d . . . C226 C 1.3938(2) 0.9454(3) 0.7272(2) 0.0293(10) Uani 1 1 d . . . H226 H 1.4257 0.9739 0.7023 0.035 Uiso 1 1 calc R . . C227 C 1.3813(2) 0.8799(3) 0.7227(2) 0.0287(10) Uani 1 1 d . . . H227 H 1.4034 0.8558 0.6943 0.034 Uiso 1 1 calc R . . C228 C 1.3313(2) 0.8562(2) 0.7670(2) 0.0230(9) Uani 1 1 d . . . C229 C 1.3044(2) 0.7861(2) 0.7891(2) 0.0228(9) Uani 1 1 d . . . C230 C 1.3578(2) 0.7398(3) 0.8349(2) 0.0292(10) Uani 1 1 d . . . H23A H 1.3639 0.7634 0.8676 0.035 Uiso 1 1 calc R . . H23B H 1.3376 0.6962 0.8543 0.035 Uiso 1 1 calc R . . C231 C 1.4293(3) 0.7223(3) 0.8076(3) 0.0380(13) Uani 1 1 d . . . H23C H 1.4246 0.6954 0.7775 0.057 Uiso 1 1 calc R . . H23D H 1.4596 0.6952 0.8401 0.057 Uiso 1 1 calc R . . H23E H 1.4498 0.7649 0.7876 0.057 Uiso 1 1 calc R . . C232 C 1.2977(2) 0.7544(2) 0.7345(2) 0.0267(10) Uani 1 1 d . . . H23F H 1.2611 0.7830 0.7079 0.032 Uiso 1 1 calc R . . H23G H 1.3424 0.7564 0.7105 0.032 Uiso 1 1 calc R . . C233 C 1.2797(3) 0.6803(3) 0.7515(3) 0.0391(13) Uani 1 1 d . . . H23H H 1.3179 0.6506 0.7745 0.059 Uiso 1 1 calc R . . H23I H 1.2732 0.6653 0.7143 0.059 Uiso 1 1 calc R . . H23J H 1.2366 0.6772 0.7768 0.059 Uiso 1 1 calc R . . C234 C 1.2333(2) 0.7934(2) 0.8213(2) 0.0215(9) Uani 1 1 d . . . C235 C 1.2171(3) 0.7603(3) 0.8823(2) 0.0285(10) Uani 1 1 d . . . H235 H 1.2487 0.7337 0.9118 0.034 Uiso 1 1 calc R . . C236 C 1.1461(3) 0.7746(3) 0.8903(2) 0.0307(11) Uani 1 1 d . . . H236 H 1.1191 0.7588 0.9266 0.037 Uiso 1 1 calc R . . C237 C 1.1210(2) 0.8161(2) 0.83586(19) 0.0213(9) Uani 1 1 d . . . C238 C 1.0504(2) 0.8368(2) 0.8222(2) 0.0237(9) Uani 1 1 d . . . H238 H 1.0154 0.8207 0.8521 0.028 Uiso 1 1 calc R . . C239 C 0.9606(2) 0.8901(2) 0.7551(2) 0.0239(9) Uani 1 1 d . . . C240 C 0.9036(2) 0.8845(3) 0.7966(2) 0.0291(10) Uani 1 1 d . . . H240 H 0.9119 0.8693 0.8391 0.035 Uiso 1 1 calc R . . C241 C 0.8354(3) 0.9006(3) 0.7776(2) 0.0336(12) Uani 1 1 d . . . C242 C 0.7761(3) 0.8938(3) 0.8244(2) 0.0431(15) Uani 1 1 d . . . H24A H 0.7500 0.8557 0.8214 0.065 Uiso 1 1 calc R . . H24B H 0.7450 0.9367 0.8170 0.065 Uiso 1 1 calc R . . H24C H 0.7948 0.8844 0.8654 0.065 Uiso 1 1 calc R . . C243 C 0.8236(3) 0.9240(3) 0.7149(3) 0.0377(13) Uani 1 1 d . . . C244 C 0.7501(3) 0.9434(4) 0.6919(3) 0.064(2) Uani 1 1 d . . . H24D H 0.7278 0.9814 0.7086 0.095 Uiso 1 1 calc R . . H24E H 0.7231 0.9035 0.7051 0.095 Uiso 1 1 calc R . . H24F H 0.7518 0.9578 0.6472 0.095 Uiso 1 1 calc R . . C245 C 0.8802(2) 0.9301(3) 0.6736(2) 0.0332(11) Uani 1 1 d . . . H245 H 0.8721 0.9458 0.6311 0.040 Uiso 1 1 calc R . . C246 C 0.9485(2) 0.9137(2) 0.6928(2) 0.0234(9) Uani 1 1 d . . . C300 C 0.1769(3) 0.4096(2) 0.3203(3) 0.082(3) Uani 1 1 d G . . H300 H 0.1829 0.3684 0.3062 0.099 Uiso 1 1 calc R . . C301 C 0.1301(3) 0.4149(2) 0.3685(2) 0.069(2) Uani 1 1 d G . . H301 H 0.1041 0.3774 0.3874 0.083 Uiso 1 1 calc R . . C302 C 0.1214(2) 0.4750(3) 0.38920(17) 0.0569(18) Uani 1 1 d G . . H302 H 0.0894 0.4787 0.4222 0.068 Uiso 1 1 calc R . . C303 C 0.1595(2) 0.52983(19) 0.36164(19) 0.0509(16) Uani 1 1 d G . . H303 H 0.1535 0.5709 0.3758 0.061 Uiso 1 1 calc R . . C304 C 0.2063(2) 0.5245(2) 0.3134(2) 0.0571(18) Uani 1 1 d G . . H304 H 0.2323 0.5619 0.2946 0.068 Uiso 1 1 calc R . . C305 C 0.2150(2) 0.4644(3) 0.2928(2) 0.078(3) Uani 1 1 d G . . H305 H 0.2470 0.4607 0.2598 0.094 Uiso 1 1 calc R . . C310 C 0.8166(6) 0.6922(4) 0.8261(4) 0.178(8) Uani 1 1 d G . . H310 H 0.8195 0.7303 0.7920 0.214 Uiso 1 1 calc R . . C311 C 0.8653(4) 0.6792(4) 0.8716(5) 0.156(8) Uani 1 1 d G . . H311 H 0.9015 0.7084 0.8685 0.188 Uiso 1 1 calc R . . C312 C 0.8611(3) 0.6234(5) 0.9216(4) 0.152(7) Uani 1 1 d G . . H312 H 0.8944 0.6145 0.9526 0.182 Uiso 1 1 calc R . . C313 C 0.8082(4) 0.5805(4) 0.9261(4) 0.144(6) Uani 1 1 d G . . H313 H 0.8054 0.5424 0.9603 0.172 Uiso 1 1 calc R . . C314 C 0.7595(3) 0.5935(5) 0.8807(5) 0.153(8) Uani 1 1 d G . . H314 H 0.7234 0.5643 0.8838 0.183 Uiso 1 1 calc R . . C315 C 0.7637(4) 0.6494(6) 0.8307(4) 0.166(8) Uani 1 1 d G . . H315 H 0.7304 0.6583 0.7996 0.200 Uiso 1 1 calc R . . C320 C 0.6529(2) 0.3493(2) 0.9902(2) 0.0517(16) Uani 1 1 d G . . H320 H 0.6772 0.3147 0.9726 0.062 Uiso 1 1 calc R . . C321 C 0.5812(2) 0.3498(2) 1.0020(2) 0.0516(16) Uani 1 1 d G . . H321 H 0.5566 0.3156 0.9925 0.062 Uiso 1 1 calc R . . C322 C 0.54559(16) 0.4003(3) 1.0278(2) 0.064(2) Uani 1 1 d G . . H322 H 0.4966 0.4007 1.0358 0.077 Uiso 1 1 calc R . . C323 C 0.5816(2) 0.4504(2) 1.0417(2) 0.075(2) Uani 1 1 d G . . H323 H 0.5572 0.4849 1.0593 0.089 Uiso 1 1 calc R . . C324 C 0.6532(2) 0.4499(2) 1.0299(2) 0.066(2) Uani 1 1 d G . . H324 H 0.6778 0.4841 1.0395 0.080 Uiso 1 1 calc R . . C325 C 0.68886(16) 0.3993(2) 1.0042(2) 0.0544(17) Uani 1 1 d G . . H325 H 0.7378 0.3990 0.9961 0.065 Uiso 1 1 calc R . . C330 C 0.5726(3) 0.6060(2) 0.7713(3) 0.088(3) Uani 1 1 d G . . H330 H 0.5626 0.6542 0.7559 0.105 Uiso 1 1 calc R . . C331 C 0.5798(3) 0.5788(3) 0.8337(3) 0.092(3) Uani 1 1 d G . . H331 H 0.5747 0.6085 0.8609 0.110 Uiso 1 1 calc R . . C332 C 0.5945(3) 0.5081(4) 0.8563(2) 0.096(3) Uani 1 1 d G . . H332 H 0.5994 0.4896 0.8989 0.116 Uiso 1 1 calc R . . C333 C 0.6019(3) 0.4647(2) 0.8166(4) 0.112(5) Uani 1 1 d G . . H333 H 0.6119 0.4164 0.8320 0.134 Uiso 1 1 calc R . . C334 C 0.5947(3) 0.4919(4) 0.7542(3) 0.121(5) Uani 1 1 d G . . H334 H 0.5998 0.4622 0.7270 0.145 Uiso 1 1 calc R . . C335 C 0.5800(3) 0.5625(4) 0.7316(2) 0.105(4) Uani 1 1 d G . . H335 H 0.5751 0.5811 0.6890 0.126 Uiso 1 1 calc R . . C340 C 0.4577(3) 0.6898(3) 0.6103(3) 0.094(3) Uani 1 1 d G . . H340 H 0.4817 0.7131 0.6334 0.113 Uiso 1 1 calc R . . C341 C 0.4253(3) 0.6316(4) 0.63956(19) 0.092(3) Uani 1 1 d G . . H341 H 0.4271 0.6152 0.6827 0.111 Uiso 1 1 calc R . . C342 C 0.3902(3) 0.5975(3) 0.6058(3) 0.093(3) Uani 1 1 d G . . H342 H 0.3680 0.5578 0.6258 0.111 Uiso 1 1 calc R . . C343 C 0.3875(3) 0.6216(3) 0.5427(3) 0.080(3) Uani 1 1 d G . . H343 H 0.3635 0.5983 0.5196 0.097 Uiso 1 1 calc R . . C344 C 0.4200(3) 0.6797(3) 0.51346(19) 0.074(2) Uani 1 1 d G . . H344 H 0.4182 0.6962 0.4704 0.089 Uiso 1 1 calc R . . C345 C 0.4551(3) 0.7138(3) 0.5473(3) 0.086(3) Uani 1 1 d G . . H345 H 0.4773 0.7535 0.5273 0.103 Uiso 1 1 calc R . . C350 C 0.0199(3) 0.6832(3) 0.7587(2) 0.078(2) Uani 1 1 d G . . H350 H 0.0103 0.6592 0.7996 0.093 Uiso 1 1 calc R . . C351 C 0.0825(3) 0.7126(3) 0.7435(2) 0.074(2) Uani 1 1 d G . . H351 H 0.1156 0.7086 0.7740 0.089 Uiso 1 1 calc R . . C352 C 0.0966(2) 0.7477(2) 0.6837(3) 0.076(3) Uani 1 1 d G . . H352 H 0.1393 0.7678 0.6733 0.091 Uiso 1 1 calc R . . C353 C 0.0481(3) 0.7534(2) 0.6391(2) 0.088(3) Uani 1 1 d G . . H353 H 0.0577 0.7774 0.5982 0.105 Uiso 1 1 calc R . . C354 C -0.0145(3) 0.7241(3) 0.6543(3) 0.094(3) Uani 1 1 d G . . H354 H -0.0476 0.7280 0.6238 0.113 Uiso 1 1 calc R . . C355 C -0.0285(2) 0.6889(3) 0.7141(3) 0.092(3) Uani 1 1 d G . . H355 H -0.0713 0.6689 0.7245 0.111 Uiso 1 1 calc R . . C360 C 0.1716(3) 0.5769(3) 0.8816(3) 0.086(3) Uani 1 1 d G . . H360 H 0.2093 0.6050 0.8741 0.104 Uiso 1 1 calc R . . C361 C 0.1233(3) 0.5812(3) 0.9290(3) 0.084(3) Uani 1 1 d G . . H361 H 0.1278 0.6122 0.9539 0.100 Uiso 1 1 calc R . . C362 C 0.0682(3) 0.5402(3) 0.9399(3) 0.107(4) Uani 1 1 d G . . H362 H 0.0352 0.5431 0.9723 0.129 Uiso 1 1 calc R . . C363 C 0.0616(3) 0.4949(3) 0.9035(3) 0.101(3) Uani 1 1 d G . . H363 H 0.0240 0.4668 0.9109 0.121 Uiso 1 1 calc R . . C364 C 0.1100(3) 0.4906(3) 0.8561(3) 0.082(3) Uani 1 1 d G . . H364 H 0.1054 0.4596 0.8312 0.098 Uiso 1 1 calc R . . C365 C 0.1650(3) 0.5316(3) 0.8452(2) 0.082(3) Uani 1 1 d G . . H365 H 0.1981 0.5286 0.8128 0.099 Uiso 1 1 calc R . . C370 C 0.3956(3) 0.1815(3) 0.1779(2) 0.097(4) Uani 1 1 d G . . H370 H 0.3609 0.1772 0.2099 0.116 Uiso 1 1 calc R . . C371 C 0.4550(3) 0.1347(2) 0.1833(2) 0.089(3) Uani 1 1 d G . . H371 H 0.4609 0.0984 0.2191 0.107 Uiso 1 1 calc R . . C372 C 0.5057(2) 0.1410(2) 0.1365(3) 0.075(3) Uani 1 1 d G . . H372 H 0.5463 0.1090 0.1402 0.090 Uiso 1 1 calc R . . C373 C 0.4971(2) 0.1941(3) 0.0842(2) 0.0620(19) Uani 1 1 d G . . H373 H 0.5317 0.1984 0.0522 0.074 Uiso 1 1 calc R . . C374 C 0.4377(2) 0.2410(2) 0.07875(18) 0.0574(18) Uani 1 1 d G . . H374 H 0.4318 0.2773 0.0430 0.069 Uiso 1 1 calc R . . C375 C 0.3870(2) 0.2347(3) 0.1256(2) 0.070(2) Uani 1 1 d G . . H375 H 0.3464 0.2667 0.1219 0.084 Uiso 1 1 calc R . . C380 C 0.4212(4) 0.1447(4) 0.4415(4) 0.127(5) Uani 1 1 d G . . H380 H 0.4393 0.1116 0.4761 0.152 Uiso 1 1 calc R . . C381 C 0.4445(4) 0.1402(4) 0.3831(5) 0.136(5) Uani 1 1 d G . . H381 H 0.4786 0.1040 0.3777 0.163 Uiso 1 1 calc R . . C382 C 0.4180(5) 0.1887(6) 0.3324(3) 0.174(9) Uani 1 1 d G . . H382 H 0.4340 0.1856 0.2925 0.209 Uiso 1 1 calc R . . C383 C 0.3682(5) 0.2416(5) 0.3402(4) 0.184(9) Uani 1 1 d G . . H383 H 0.3501 0.2747 0.3056 0.221 Uiso 1 1 calc R . . C384 C 0.3449(4) 0.2461(4) 0.3987(5) 0.153(6) Uani 1 1 d G . . H384 H 0.3108 0.2823 0.4040 0.184 Uiso 1 1 calc R . . C385 C 0.3714(5) 0.1977(5) 0.4493(3) 0.130(5) Uani 1 1 d G . . H385 H 0.3555 0.2008 0.4892 0.156 Uiso 1 1 calc R . . C390 C 0.3655(3) 0.4023(3) 0.5483(2) 0.070(2) Uani 1 1 d G . . H390 H 0.3710 0.3851 0.5910 0.084 Uiso 1 1 calc R . . C391 C 0.4148(3) 0.4418(4) 0.5133(3) 0.106(4) Uani 1 1 d G . . H391 H 0.4540 0.4516 0.5321 0.128 Uiso 1 1 calc R . . C392 C 0.4068(3) 0.4669(4) 0.4508(3) 0.149(6) Uani 1 1 d G . . H392 H 0.4405 0.4939 0.4269 0.179 Uiso 1 1 calc R . . C393 C 0.3495(4) 0.4526(4) 0.42333(19) 0.112(4) Uani 1 1 d G . . H393 H 0.3440 0.4697 0.3806 0.134 Uiso 1 1 calc R . . C394 C 0.3001(3) 0.4131(3) 0.4583(3) 0.082(3) Uani 1 1 d G . . H394 H 0.2609 0.4033 0.4395 0.099 Uiso 1 1 calc R . . C395 C 0.3081(3) 0.3879(3) 0.5208(3) 0.080(3) Uani 1 1 d G . . H395 H 0.2744 0.3609 0.5447 0.096 Uiso 1 1 calc R . . Ce1 Ce 1.351945(12) 1.159740(13) 0.851331(11) 0.01793(5) Uani 1 1 d . . . Ce2 Ce 0.973790(12) 1.320847(13) 0.714145(11) 0.01728(5) Uani 1 1 d . . . Ce3 Ce 1.130483(12) 0.930218(13) 0.696042(11) 0.01799(5) Uani 1 1 d . . . N1 N 1.42749(18) 1.0522(2) 0.91151(17) 0.0214(8) Uani 1 1 d . A . N2 N 1.46499(19) 1.1286(2) 0.79634(17) 0.0249(8) Uani 1 1 d . A . N3 N 1.34534(19) 1.2040(2) 0.73793(17) 0.0226(8) Uani 1 1 d . A . N4 N 1.22322(18) 1.20914(19) 0.81534(17) 0.0211(8) Uani 1 1 d . A . N5 N 1.09961(18) 1.31648(19) 0.76651(17) 0.0213(8) Uani 1 1 d . . . N6 N 1.24233(19) 1.3592(2) 0.80060(19) 0.0255(8) Uani 1 1 d . . . N7 N 1.3327(2) 1.2576(2) 0.91179(17) 0.0242(8) Uani 1 1 d . A . N8 N 1.3345(2) 1.1171(2) 0.96984(16) 0.0228(8) Uani 1 1 d . A . N11 N 1.00025(19) 1.4463(2) 0.70746(17) 0.0223(8) Uani 1 1 d . . . N12 N 0.91540(18) 1.3732(2) 0.79667(17) 0.0218(8) Uani 1 1 d . . . N13 N 0.94903(19) 1.22750(19) 0.80644(16) 0.0210(8) Uani 1 1 d . . . N14 N 1.03818(18) 1.19816(19) 0.71225(17) 0.0209(8) Uani 1 1 d . . . N15 N 1.04895(19) 1.04851(19) 0.69718(18) 0.0228(8) Uani 1 1 d . . . N16 N 0.91077(18) 1.14820(19) 0.67317(17) 0.0217(8) Uani 1 1 d . . . N17 N 0.91419(18) 1.30806(19) 0.61304(16) 0.0200(7) Uani 1 1 d . . . N18 N 1.01936(19) 1.3965(2) 0.61186(17) 0.0228(8) Uani 1 1 d . . . N21 N 1.00910(19) 0.92011(19) 0.65423(17) 0.0225(8) Uani 1 1 d . . . N22 N 1.1307(2) 0.9249(2) 0.58411(17) 0.0228(8) Uani 1 1 d . . . N23 N 1.23325(19) 0.9829(2) 0.63658(16) 0.0223(8) Uani 1 1 d . . . N24 N 1.19438(18) 1.00591(19) 0.75013(16) 0.0195(7) Uani 1 1 d . . . N25 N 1.29996(18) 1.05372(19) 0.82526(17) 0.0210(8) Uani 1 1 d . A . N26 N 1.31356(18) 0.9062(2) 0.79814(17) 0.0226(8) Uani 1 1 d . . . N27 N 1.17566(19) 0.82938(19) 0.79236(17) 0.0210(8) Uani 1 1 d . . . N28 N 1.03143(19) 0.8770(2) 0.77061(17) 0.0225(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(2) 0.028(2) 0.029(2) -0.0077(19) -0.0069(17) -0.0008(18) C2 0.015(2) 0.032(3) 0.024(2) -0.0057(19) -0.0005(17) -0.0040(18) C3 0.020(2) 0.049(3) 0.037(3) -0.009(2) 0.001(2) 0.000(2) C4 0.022(2) 0.063(4) 0.029(3) -0.009(3) 0.008(2) -0.010(2) C5 0.019(2) 0.040(3) 0.024(2) -0.003(2) -0.0003(18) -0.012(2) C6 0.028(2) 0.038(3) 0.021(2) -0.002(2) 0.0014(19) -0.015(2) C7 0.026(3) 0.070(4) 0.026(3) -0.002(3) 0.009(2) -0.012(3) C8 0.033(3) 0.087(5) 0.032(3) -0.026(3) 0.005(2) 0.015(3) C9 0.026(4) 0.026(4) 0.043(5) -0.005(3) 0.000(3) -0.009(3) C10 0.028(4) 0.048(5) 0.073(7) -0.023(5) 0.001(4) -0.016(4) C9A 0.019(9) 0.036(10) 0.032(9) 0.008(8) -0.009(7) -0.007(8) C10A 0.053(12) 0.046(11) 0.022(9) 0.008(8) -0.003(8) -0.016(9) C11 0.030(2) 0.023(2) 0.021(2) -0.0030(18) 0.0031(18) -0.0033(19) C12 0.034(3) 0.038(3) 0.023(2) -0.007(2) -0.001(2) 0.007(2) C13 0.035(3) 0.038(3) 0.021(2) -0.007(2) -0.004(2) 0.011(2) C14 0.025(2) 0.026(2) 0.020(2) -0.0052(18) -0.0036(17) 0.0019(18) C15 0.019(2) 0.024(2) 0.027(2) -0.0046(19) -0.0025(18) 0.0040(18) C16 0.0141(19) 0.027(2) 0.021(2) -0.0073(18) 0.0005(16) -0.0076(17) C17 0.018(2) 0.027(2) 0.025(2) -0.0045(19) -0.0021(17) -0.0073(18) C18 0.042(3) 0.044(3) 0.022(2) -0.005(2) 0.000(2) -0.012(3) C19 0.025(2) 0.033(3) 0.022(2) -0.0067(19) 0.0006(18) -0.012(2) C20 0.020(2) 0.036(3) 0.027(2) -0.011(2) 0.0001(18) -0.0076(19) C21 0.029(3) 0.055(4) 0.031(3) -0.019(3) 0.004(2) -0.003(2) C22 0.015(2) 0.035(3) 0.031(3) -0.015(2) -0.0028(18) -0.0017(19) C23 0.0154(19) 0.025(2) 0.021(2) -0.0058(17) -0.0016(16) -0.0077(17) C24 0.025(2) 0.024(2) 0.027(2) -0.0052(19) -0.0093(19) 0.0022(19) C25 0.022(2) 0.029(3) 0.031(3) -0.006(2) -0.0012(19) -0.0048(19) C26 0.033(3) 0.052(4) 0.031(3) -0.004(3) 0.002(2) -0.017(3) C27 0.029(3) 0.051(3) 0.038(3) -0.007(3) 0.004(2) -0.021(2) C28 0.021(2) 0.027(2) 0.035(3) -0.008(2) -0.0028(19) -0.0065(19) C29 0.023(2) 0.020(2) 0.041(3) -0.005(2) -0.006(2) -0.0046(18) C30 0.048(3) 0.026(3) 0.054(4) -0.010(3) -0.018(3) -0.006(2) C31 0.056(4) 0.023(3) 0.077(5) -0.003(3) -0.020(3) -0.009(3) C32 0.025(3) 0.022(3) 0.070(4) 0.003(3) 0.001(3) -0.005(2) C33 0.027(3) 0.051(4) 0.099(6) 0.017(4) -0.024(3) -0.007(3) C34 0.023(2) 0.029(3) 0.037(3) -0.015(2) -0.012(2) -0.0007(19) C35 0.035(3) 0.030(3) 0.045(3) -0.020(2) -0.009(2) 0.005(2) C36 0.034(3) 0.041(3) 0.032(3) -0.019(2) 0.000(2) -0.005(2) C37 0.023(2) 0.034(3) 0.028(2) -0.012(2) -0.0025(19) 0.000(2) C38 0.020(2) 0.036(3) 0.019(2) -0.0086(19) 0.0005(17) -0.0034(19) C39 0.019(2) 0.031(2) 0.020(2) -0.0056(18) -0.0043(17) -0.0065(18) C40 0.022(2) 0.034(3) 0.018(2) -0.0024(19) -0.0006(17) -0.0087(19) C41 0.031(3) 0.039(3) 0.019(2) -0.003(2) -0.0049(19) -0.015(2) C42 0.047(3) 0.042(3) 0.025(3) 0.004(2) -0.001(2) -0.023(3) C43 0.034(3) 0.026(2) 0.025(2) 0.0010(19) -0.009(2) -0.009(2) C44 0.053(4) 0.025(3) 0.038(3) 0.002(2) -0.009(3) -0.004(2) C45 0.023(2) 0.028(2) 0.025(2) -0.0060(19) -0.0048(18) -0.0017(19) C46 0.018(2) 0.026(2) 0.019(2) -0.0048(18) -0.0043(16) -0.0043(17) C101 0.026(2) 0.023(2) 0.028(2) -0.0085(19) -0.0024(19) -0.0019(19) C102 0.025(2) 0.025(2) 0.026(2) -0.0070(19) 0.0050(18) -0.0019(19) C103 0.040(3) 0.032(3) 0.042(3) -0.020(2) 0.014(2) -0.006(2) C104 0.036(3) 0.038(3) 0.031(3) -0.016(2) 0.013(2) -0.007(2) C105 0.019(2) 0.028(2) 0.023(2) -0.0055(19) -0.0013(17) -0.0012(18) C106 0.020(2) 0.032(2) 0.018(2) -0.0076(18) 0.0026(16) -0.0051(18) C107 0.023(2) 0.038(3) 0.021(2) -0.008(2) -0.0004(18) -0.006(2) C108 0.024(2) 0.060(4) 0.033(3) -0.016(3) -0.001(2) 0.001(2) C109 0.023(2) 0.044(3) 0.021(2) -0.011(2) 0.0041(18) -0.008(2) C110 0.035(3) 0.048(3) 0.027(3) -0.008(2) 0.007(2) -0.014(2) C111 0.020(2) 0.030(2) 0.019(2) -0.0079(18) -0.0012(17) -0.0084(18) C112 0.030(2) 0.031(3) 0.020(2) -0.0046(19) 0.0010(18) -0.008(2) C113 0.028(2) 0.026(2) 0.032(3) -0.004(2) -0.006(2) -0.002(2) C114 0.023(2) 0.020(2) 0.026(2) -0.0050(18) -0.0030(18) -0.0035(18) C115 0.017(2) 0.017(2) 0.035(3) -0.0045(19) -0.0008(18) -0.0032(17) C116 0.0146(19) 0.023(2) 0.026(2) -0.0049(18) -0.0050(17) -0.0006(17) C117 0.022(2) 0.022(2) 0.029(2) -0.0090(19) -0.0020(18) -0.0023(18) C118 0.019(2) 0.032(3) 0.027(2) -0.007(2) -0.0021(18) -0.0014(19) C119 0.044(3) 0.041(3) 0.031(3) -0.006(2) 0.009(2) -0.007(3) C120 0.022(2) 0.031(3) 0.029(2) -0.009(2) -0.0061(19) 0.0026(19) C121 0.042(3) 0.040(3) 0.029(3) -0.016(2) -0.006(2) 0.005(2) C122 0.022(2) 0.027(2) 0.031(2) -0.014(2) -0.0084(19) 0.0027(19) C123 0.0128(19) 0.025(2) 0.031(2) -0.0089(19) -0.0052(17) 0.0010(17) C124 0.023(2) 0.023(2) 0.033(3) -0.006(2) -0.0059(19) -0.0055(18) C125 0.017(2) 0.021(2) 0.035(3) -0.0058(19) -0.0021(18) -0.0040(17) C126 0.025(2) 0.030(3) 0.033(3) -0.001(2) 0.002(2) -0.007(2) C127 0.021(2) 0.027(2) 0.031(3) 0.000(2) 0.0041(19) -0.0061(19) C128 0.018(2) 0.024(2) 0.025(2) -0.0088(18) 0.0002(17) -0.0059(17) C129 0.0145(19) 0.028(2) 0.022(2) -0.0086(18) 0.0005(16) -0.0051(17) C130 0.016(2) 0.034(3) 0.029(2) -0.018(2) 0.0024(17) -0.0056(18) C131 0.021(2) 0.048(3) 0.044(3) -0.024(3) 0.005(2) -0.016(2) C132 0.021(2) 0.026(2) 0.020(2) -0.0076(18) 0.0017(17) -0.0027(18) C133 0.029(3) 0.033(3) 0.032(3) -0.008(2) -0.002(2) 0.002(2) C134 0.018(2) 0.021(2) 0.022(2) -0.0071(17) -0.0021(16) -0.0050(17) C135 0.025(2) 0.041(3) 0.023(2) -0.013(2) -0.0004(18) -0.013(2) C136 0.029(2) 0.045(3) 0.019(2) -0.012(2) 0.0067(19) -0.013(2) C137 0.023(2) 0.024(2) 0.020(2) -0.0058(18) -0.0009(17) -0.0047(18) C138 0.021(2) 0.026(2) 0.019(2) -0.0031(18) 0.0005(17) -0.0041(18) C139 0.019(2) 0.024(2) 0.023(2) -0.0024(18) -0.0010(17) -0.0060(17) C140 0.023(2) 0.026(2) 0.024(2) -0.0042(19) 0.0002(18) -0.0040(18) C141 0.020(2) 0.025(2) 0.034(3) -0.003(2) 0.0011(19) -0.0073(18) C142 0.035(3) 0.042(3) 0.045(3) -0.012(3) 0.013(2) -0.020(2) C143 0.026(2) 0.026(2) 0.034(3) -0.007(2) 0.003(2) -0.0085(19) C144 0.038(3) 0.044(3) 0.052(4) -0.023(3) 0.006(3) -0.020(3) C145 0.025(2) 0.025(2) 0.029(2) -0.009(2) 0.0025(19) -0.0048(19) C146 0.020(2) 0.020(2) 0.024(2) -0.0031(18) -0.0014(17) -0.0008(17) C201 0.024(2) 0.031(3) 0.029(2) -0.012(2) -0.0049(19) -0.005(2) C202 0.025(2) 0.030(2) 0.023(2) -0.0100(19) -0.0052(18) -0.0015(19) C203 0.033(3) 0.040(3) 0.022(2) -0.013(2) -0.009(2) 0.002(2) C204 0.042(3) 0.033(3) 0.015(2) -0.0097(19) 0.0009(19) 0.002(2) C205 0.029(2) 0.024(2) 0.021(2) -0.0076(18) 0.0009(18) 0.0020(19) C206 0.028(2) 0.036(3) 0.018(2) -0.008(2) 0.0052(18) 0.001(2) C207 0.033(3) 0.052(3) 0.028(3) -0.016(2) 0.005(2) 0.004(2) C208 0.037(3) 0.076(5) 0.046(4) -0.020(3) 0.016(3) 0.000(3) C209 0.031(3) 0.040(3) 0.025(2) -0.013(2) -0.002(2) 0.007(2) C210 0.054(4) 0.041(3) 0.037(3) -0.014(3) -0.009(3) 0.011(3) C211 0.021(2) 0.038(3) 0.018(2) -0.0083(19) 0.0045(17) -0.0016(19) C212 0.024(2) 0.045(3) 0.024(2) -0.006(2) 0.0061(19) -0.009(2) C213 0.027(2) 0.038(3) 0.025(2) -0.003(2) 0.0037(19) -0.015(2) C214 0.015(2) 0.027(2) 0.023(2) -0.0038(18) -0.0012(16) -0.0033(17) C215 0.017(2) 0.026(2) 0.024(2) -0.0075(18) -0.0044(17) -0.0013(17) C216 0.017(2) 0.018(2) 0.023(2) -0.0057(17) -0.0025(16) -0.0016(16) C217 0.018(2) 0.024(2) 0.025(2) -0.0100(18) -0.0022(17) -0.0021(17) C218 0.019(2) 0.024(2) 0.022(2) -0.0052(18) 0.0011(17) -0.0029(17) C219 0.027(2) 0.042(3) 0.027(3) -0.009(2) 0.005(2) -0.013(2) C220 0.026(2) 0.026(2) 0.021(2) -0.0069(18) -0.0012(18) -0.0040(19) C221 0.038(3) 0.048(3) 0.020(2) -0.010(2) 0.001(2) -0.012(2) C222 0.022(2) 0.025(2) 0.025(2) -0.0078(19) -0.0040(18) -0.0049(18) C223 0.018(2) 0.018(2) 0.023(2) -0.0069(17) -0.0023(16) -0.0016(16) C224 0.0133(19) 0.026(2) 0.032(2) -0.0068(19) -0.0026(17) -0.0029(17) C225 0.015(2) 0.024(2) 0.030(2) -0.0076(19) -0.0021(17) -0.0008(17) C226 0.021(2) 0.036(3) 0.030(3) -0.007(2) -0.0002(19) -0.002(2) C227 0.022(2) 0.031(3) 0.033(3) -0.011(2) 0.0026(19) 0.003(2) C228 0.019(2) 0.025(2) 0.027(2) -0.0108(19) -0.0046(17) 0.0011(18) C229 0.020(2) 0.022(2) 0.026(2) -0.0074(18) -0.0022(17) 0.0027(17) C230 0.023(2) 0.031(3) 0.033(3) -0.008(2) -0.007(2) 0.002(2) C231 0.025(3) 0.040(3) 0.048(3) -0.011(3) -0.006(2) 0.004(2) C232 0.025(2) 0.030(3) 0.028(2) -0.014(2) -0.0036(19) 0.0019(19) C233 0.042(3) 0.035(3) 0.044(3) -0.015(3) -0.006(3) -0.004(2) C234 0.023(2) 0.020(2) 0.023(2) -0.0077(17) -0.0024(17) -0.0007(17) C235 0.029(2) 0.032(3) 0.021(2) -0.0010(19) -0.0071(19) 0.002(2) C236 0.030(3) 0.035(3) 0.022(2) 0.001(2) 0.0005(19) -0.001(2) C237 0.023(2) 0.025(2) 0.016(2) -0.0045(17) 0.0010(16) -0.0037(18) C238 0.027(2) 0.023(2) 0.022(2) -0.0051(18) 0.0002(18) -0.0065(18) C239 0.018(2) 0.030(2) 0.026(2) -0.0084(19) -0.0039(17) -0.0044(18) C240 0.024(2) 0.037(3) 0.027(2) -0.007(2) -0.0046(19) -0.003(2) C241 0.020(2) 0.048(3) 0.031(3) -0.004(2) 0.000(2) -0.006(2) C242 0.017(2) 0.075(4) 0.029(3) 0.001(3) 0.004(2) -0.005(3) C243 0.023(2) 0.053(3) 0.034(3) -0.004(3) -0.005(2) -0.005(2) C244 0.025(3) 0.111(6) 0.042(4) 0.009(4) -0.006(3) -0.009(3) C245 0.020(2) 0.049(3) 0.032(3) -0.009(2) -0.006(2) -0.006(2) C246 0.021(2) 0.026(2) 0.025(2) -0.0069(19) -0.0017(17) -0.0076(18) C300 0.094(7) 0.064(5) 0.102(7) -0.042(5) -0.037(6) -0.001(5) C301 0.080(5) 0.050(4) 0.072(5) 0.012(4) -0.029(4) -0.027(4) C302 0.051(4) 0.078(5) 0.036(3) 0.000(3) -0.015(3) -0.003(4) C303 0.049(4) 0.051(4) 0.053(4) -0.012(3) -0.023(3) 0.002(3) C304 0.062(4) 0.063(4) 0.047(4) -0.007(3) -0.013(3) -0.018(4) C305 0.063(5) 0.109(7) 0.075(6) -0.048(5) -0.010(4) 0.000(5) C310 0.182(17) 0.192(16) 0.201(17) -0.148(14) 0.065(14) -0.002(14) C311 0.135(12) 0.171(15) 0.218(18) -0.152(15) 0.086(12) -0.064(11) C312 0.063(6) 0.209(16) 0.251(18) -0.191(15) 0.010(9) -0.005(8) C313 0.085(8) 0.156(11) 0.240(16) -0.157(12) 0.027(9) 0.002(8) C314 0.042(5) 0.209(16) 0.28(2) -0.203(16) -0.005(8) 0.010(7) C315 0.120(12) 0.209(19) 0.207(19) -0.145(17) -0.005(12) 0.038(12) C320 0.051(4) 0.059(4) 0.045(4) -0.019(3) -0.003(3) 0.006(3) C321 0.048(4) 0.057(4) 0.053(4) -0.019(3) -0.005(3) -0.006(3) C322 0.039(4) 0.092(6) 0.069(5) -0.037(4) 0.002(3) 0.000(4) C323 0.055(4) 0.087(6) 0.102(7) -0.064(5) 0.000(4) 0.001(4) C324 0.050(4) 0.067(5) 0.094(6) -0.043(5) -0.003(4) -0.006(4) C325 0.038(3) 0.077(5) 0.054(4) -0.029(4) 0.005(3) -0.003(3) C330 0.050(5) 0.066(5) 0.123(8) 0.012(5) 0.022(5) 0.009(4) C331 0.062(5) 0.109(8) 0.113(8) -0.046(7) 0.002(5) -0.006(5) C332 0.040(4) 0.130(9) 0.090(7) 0.021(6) -0.004(4) 0.006(5) C333 0.052(5) 0.059(5) 0.195(13) 0.007(7) 0.060(7) 0.006(4) C334 0.091(8) 0.145(11) 0.147(11) -0.079(10) 0.064(8) -0.031(8) C335 0.067(6) 0.175(12) 0.065(6) -0.031(7) 0.014(5) 0.016(7) C340 0.087(7) 0.107(8) 0.096(8) -0.038(6) -0.009(6) -0.008(6) C341 0.056(5) 0.141(9) 0.065(6) -0.005(6) 0.001(4) 0.008(6) C342 0.047(4) 0.104(7) 0.101(7) 0.029(6) 0.009(5) -0.018(5) C343 0.045(4) 0.099(7) 0.095(7) -0.011(5) -0.007(4) -0.022(4) C344 0.052(4) 0.094(6) 0.071(5) -0.005(5) 0.009(4) -0.018(4) C345 0.073(6) 0.085(6) 0.099(7) -0.011(6) -0.004(5) -0.027(5) C350 0.091(6) 0.077(6) 0.077(6) -0.045(5) -0.002(5) -0.002(5) C351 0.060(5) 0.074(5) 0.106(7) -0.062(5) -0.014(5) 0.009(4) C352 0.066(5) 0.057(5) 0.119(8) -0.050(5) -0.003(5) -0.002(4) C353 0.141(9) 0.031(4) 0.089(7) -0.017(4) -0.016(6) 0.008(5) C354 0.105(8) 0.069(6) 0.121(8) -0.035(6) -0.069(7) 0.006(5) C355 0.059(5) 0.100(7) 0.132(9) -0.048(7) -0.012(6) -0.017(5) C360 0.088(6) 0.114(8) 0.062(5) -0.010(5) -0.004(5) -0.057(6) C361 0.119(8) 0.067(5) 0.072(6) -0.020(5) -0.006(5) -0.032(5) C362 0.089(7) 0.131(9) 0.109(8) -0.039(7) 0.037(6) -0.044(7) C363 0.099(7) 0.100(8) 0.109(8) -0.015(6) 0.001(6) -0.062(6) C364 0.100(7) 0.062(5) 0.090(7) -0.026(5) -0.020(6) -0.004(5) C365 0.058(5) 0.121(8) 0.056(5) -0.007(5) -0.011(4) 0.013(5) C370 0.062(5) 0.174(11) 0.061(5) -0.012(6) -0.011(4) -0.069(6) C371 0.098(7) 0.089(6) 0.078(6) 0.013(5) -0.044(5) -0.057(6) C372 0.095(6) 0.050(4) 0.090(6) -0.027(4) -0.051(5) 0.002(4) C373 0.064(5) 0.065(5) 0.068(5) -0.033(4) -0.011(4) -0.005(4) C374 0.060(4) 0.059(4) 0.057(4) -0.018(4) -0.019(3) -0.004(4) C375 0.041(4) 0.105(7) 0.071(5) -0.031(5) -0.015(4) -0.004(4) C380 0.116(10) 0.167(13) 0.100(9) -0.008(9) 0.003(7) -0.085(9) C381 0.115(10) 0.169(13) 0.154(13) -0.082(11) 0.035(9) -0.063(9) C382 0.150(14) 0.32(3) 0.080(9) -0.054(12) 0.006(9) -0.130(16) C383 0.122(12) 0.202(18) 0.178(16) 0.076(14) -0.021(11) -0.063(12) C384 0.166(14) 0.111(10) 0.162(14) -0.003(10) 0.073(12) -0.034(9) C385 0.147(12) 0.175(14) 0.093(8) -0.060(9) 0.048(8) -0.085(11) C390 0.081(6) 0.063(5) 0.063(5) -0.011(4) -0.013(4) 0.001(4) C391 0.081(7) 0.135(9) 0.100(8) -0.002(7) -0.025(6) -0.046(7) C392 0.072(7) 0.246(17) 0.105(9) 0.016(10) 0.011(7) -0.048(9) C393 0.092(7) 0.178(12) 0.049(5) -0.018(6) 0.003(5) 0.031(8) C394 0.071(6) 0.088(6) 0.098(7) -0.046(6) -0.024(5) 0.018(5) C395 0.066(5) 0.061(5) 0.105(7) 0.003(5) -0.022(5) -0.013(4) Ce1 0.01675(11) 0.02093(12) 0.01610(11) -0.00322(9) -0.00086(8) -0.00448(9) Ce2 0.01559(11) 0.01958(12) 0.01678(11) -0.00435(9) 0.00029(8) -0.00277(9) Ce3 0.01581(11) 0.02280(12) 0.01618(11) -0.00591(9) -0.00079(8) -0.00248(9) N1 0.0155(17) 0.028(2) 0.0207(18) -0.0045(15) -0.0029(14) -0.0041(15) N2 0.0212(19) 0.032(2) 0.0211(19) -0.0020(16) -0.0026(15) -0.0123(16) N3 0.0211(18) 0.026(2) 0.0201(18) -0.0041(15) 0.0007(15) -0.0029(15) N4 0.0177(17) 0.0214(19) 0.0251(19) -0.0075(15) -0.0029(15) -0.0003(14) N5 0.0168(17) 0.0245(19) 0.0233(19) -0.0080(15) -0.0025(14) 0.0005(15) N6 0.0192(18) 0.026(2) 0.032(2) -0.0081(17) -0.0008(16) -0.0051(16) N7 0.0233(19) 0.028(2) 0.0228(19) -0.0073(16) -0.0030(15) -0.0036(16) N8 0.0242(19) 0.026(2) 0.0170(18) -0.0029(15) -0.0028(15) -0.0028(16) N11 0.0215(18) 0.026(2) 0.0195(18) -0.0049(15) 0.0013(14) -0.0045(15) N12 0.0167(17) 0.026(2) 0.0240(19) -0.0085(16) 0.0008(14) -0.0025(15) N13 0.0209(18) 0.0247(19) 0.0166(17) -0.0024(15) 0.0009(14) -0.0056(15) N14 0.0161(17) 0.0207(18) 0.027(2) -0.0084(15) 0.0022(14) -0.0033(14) N15 0.0192(18) 0.0222(19) 0.030(2) -0.0100(16) -0.0041(15) -0.0043(15) N16 0.0132(16) 0.025(2) 0.028(2) -0.0084(16) -0.0033(14) -0.0019(14) N17 0.0191(17) 0.0232(19) 0.0189(18) -0.0065(15) 0.0027(14) -0.0063(15) N18 0.0202(18) 0.025(2) 0.0237(19) -0.0054(16) 0.0008(15) -0.0074(15) N21 0.0206(18) 0.024(2) 0.0232(19) -0.0053(16) -0.0042(15) -0.0040(15) N22 0.0249(19) 0.027(2) 0.0175(18) -0.0070(15) -0.0021(15) -0.0021(16) N23 0.0188(18) 0.031(2) 0.0177(18) -0.0070(16) -0.0010(14) -0.0016(15) N24 0.0154(17) 0.0261(19) 0.0167(17) -0.0053(15) -0.0003(13) -0.0003(14) N25 0.0170(17) 0.0211(19) 0.0254(19) -0.0051(15) -0.0038(14) -0.0028(14) N26 0.0160(17) 0.026(2) 0.027(2) -0.0086(16) -0.0023(15) -0.0014(15) N27 0.0212(18) 0.0215(19) 0.0216(18) -0.0063(15) -0.0034(15) -0.0029(15) N28 0.0175(17) 0.028(2) 0.0225(19) -0.0045(16) -0.0011(14) -0.0053(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.307(6) . ? C1 C2 1.401(6) . ? C2 N2 1.390(6) . ? C2 C3 1.405(6) . ? C3 C4 1.389(8) . ? C4 C5 1.405(7) . ? C5 N2 1.364(6) . ? C5 C6 1.513(7) . ? C6 C11 1.516(7) . ? C6 C9A 1.533(18) . ? C6 C7 1.542(7) . ? C6 C9 1.593(9) . ? C7 C8 1.543(9) . ? C9 C10 1.530(11) . ? C9A C10A 1.52(2) . ? C11 N3 1.357(6) . ? C11 C12 1.404(7) . ? C12 C13 1.381(7) . ? C13 C14 1.395(6) . ? C14 N3 1.390(6) . ? C14 C15 1.406(6) . ? C15 N4 1.303(6) . ? C16 C17 1.392(6) . ? C16 N4 1.414(5) . ? C16 C23 1.417(6) . ? C17 C19 1.394(6) . ? C18 C19 1.497(7) . ? C19 C20 1.393(7) . ? C20 C22 1.387(7) . ? C20 C21 1.510(6) . ? C22 C23 1.396(6) . ? C23 N5 1.441(6) . ? C24 N5 1.290(6) . ? C24 C25 1.431(6) . ? C25 N6 1.373(6) . ? C25 C26 1.389(7) . ? C26 C27 1.391(7) . ? C27 C28 1.375(7) . ? C28 N6 1.370(6) . ? C28 C29 1.513(7) . ? C29 C34 1.519(7) . ? C29 C32 1.532(7) . ? C29 C30 1.539(7) . ? C30 C31 1.521(8) . ? C32 C33 1.531(9) . ? C34 N7 1.364(6) . ? C34 C35 1.413(7) . ? C35 C36 1.380(8) . ? C36 C37 1.398(7) . ? C37 N7 1.389(6) . ? C37 C38 1.403(7) . ? C38 N8 1.297(6) . ? C39 C46 1.398(6) . ? C39 C40 1.400(6) . ? C39 N8 1.401(6) . ? C40 C41 1.377(7) . ? C41 C43 1.403(7) . ? C41 C42 1.516(7) . ? C43 C45 1.393(7) . ? C43 C44 1.511(7) . ? C45 C46 1.385(6) . ? C46 N1 1.418(6) . ? C101 N11 1.300(6) . ? C101 C102 1.406(6) . ? C102 N12 1.381(6) . ? C102 C103 1.386(6) . ? C103 C104 1.390(7) . ? C104 C105 1.404(7) . ? C105 N12 1.365(6) . ? C105 C106 1.520(6) . ? C106 C111 1.510(6) . ? C106 C107 1.548(6) . ? C106 C109 1.549(6) . ? C107 C108 1.526(7) . ? C109 C110 1.528(7) . ? C111 N13 1.364(5) . ? C111 C112 1.398(6) . ? C112 C113 1.376(7) . ? C113 C114 1.404(6) . ? C114 N13 1.388(6) . ? C114 C115 1.404(6) . ? C115 N14 1.322(6) . ? C116 C117 1.392(6) . ? C116 C123 1.411(6) . ? C116 N14 1.420(6) . ? C117 C118 1.391(6) . ? C118 C120 1.399(7) . ? C118 C119 1.491(7) . ? C120 C122 1.391(7) . ? C120 C121 1.511(7) . ? C122 C123 1.391(6) . ? C123 N15 1.445(6) . ? C124 N15 1.299(6) . ? C124 C125 1.423(6) . ? C125 N16 1.381(6) . ? C125 C126 1.385(6) . ? C126 C127 1.378(7) . ? C127 C128 1.394(6) . ? C128 N16 1.365(5) . ? C128 C129 1.505(6) . ? C129 C134 1.529(6) . ? C129 C132 1.541(6) . ? C129 C130 1.551(6) . ? C130 C131 1.522(6) . ? C132 C133 1.523(6) . ? C134 N17 1.362(5) . ? C134 C135 1.394(6) . ? C135 C136 1.388(6) . ? C136 C137 1.401(6) . ? C137 C138 1.395(6) . ? C137 N17 1.400(5) . ? C138 N18 1.302(6) . ? C139 C140 1.395(6) . ? C139 C146 1.398(6) . ? C139 N18 1.406(6) . ? C140 C141 1.393(6) . ? C141 C143 1.403(7) . ? C141 C142 1.507(7) . ? C143 C145 1.389(6) . ? C143 C144 1.498(7) . ? C145 C146 1.394(6) . ? C146 N11 1.411(6) . ? C201 N21 1.294(6) . ? C201 C202 1.404(7) . ? C202 N22 1.386(6) . ? C202 C203 1.396(6) . ? C203 C204 1.378(7) . ? C204 C205 1.408(6) . ? C205 N22 1.358(6) . ? C205 C206 1.511(7) . ? C206 C211 1.520(7) . ? C206 C209 1.539(7) . ? C206 C207 1.542(7) . ? C207 C208 1.539(8) . ? C209 C210 1.512(7) . ? C211 N23 1.353(5) . ? C211 C212 1.398(7) . ? C212 C213 1.388(7) . ? C213 C214 1.399(6) . ? C214 N23 1.391(6) . ? C214 C215 1.396(6) . ? C215 N24 1.305(6) . ? C216 C217 1.401(6) . ? C216 N24 1.405(5) . ? C216 C223 1.414(6) . ? C217 C218 1.373(6) . ? C218 C220 1.401(6) . ? C218 C219 1.510(6) . ? C220 C222 1.395(6) . ? C220 C221 1.499(6) . ? C222 C223 1.394(6) . ? C223 N25 1.437(5) . ? C224 N25 1.297(6) . ? C224 C225 1.418(6) . ? C225 N26 1.383(6) . ? C225 C226 1.385(6) . ? C226 C227 1.394(7) . ? C227 C228 1.383(7) . ? C228 N26 1.367(6) . ? C228 C229 1.515(6) . ? C229 C234 1.523(6) . ? C229 C232 1.539(6) . ? C229 C230 1.563(6) . ? C230 C231 1.517(7) . ? C232 C233 1.519(7) . ? C234 N27 1.364(6) . ? C234 C235 1.408(6) . ? C235 C236 1.378(7) . ? C236 C237 1.387(6) . ? C237 N27 1.399(5) . ? C237 C238 1.408(6) . ? C238 N28 1.293(6) . ? C239 C240 1.396(6) . ? C239 C246 1.396(6) . ? C239 N28 1.410(6) . ? C240 C241 1.386(7) . ? C241 C243 1.403(7) . ? C241 C242 1.506(7) . ? C243 C245 1.389(7) . ? C243 C244 1.515(7) . ? C245 C246 1.390(6) . ? C246 N21 1.413(6) . ? C300 C301 1.3900 . ? C300 C305 1.3900 . ? C301 C302 1.3900 . ? C302 C303 1.3900 . ? C303 C304 1.3900 . ? C304 C305 1.3900 . ? C310 C311 1.3900 . ? C310 C315 1.3900 . ? C311 C312 1.3900 . ? C312 C313 1.3900 . ? C313 C314 1.3900 . ? C314 C315 1.3900 . ? C320 C321 1.3900 . ? C320 C325 1.3900 . ? C321 C322 1.3900 . ? C322 C323 1.3900 . ? C323 C324 1.3900 . ? C324 C325 1.3900 . ? C330 C331 1.3900 . ? C330 C335 1.3900 . ? C331 C332 1.3900 . ? C332 C333 1.3900 . ? C333 C334 1.3900 . ? C334 C335 1.3900 . ? C340 C341 1.3900 . ? C340 C345 1.3900 . ? C341 C342 1.3900 . ? C342 C343 1.3900 . ? C343 C344 1.3900 . ? C344 C345 1.3900 . ? C350 C351 1.3900 . ? C350 C355 1.3900 . ? C351 C352 1.3900 . ? C352 C353 1.3900 . ? C353 C354 1.3900 . ? C354 C355 1.3900 . ? C360 C361 1.3900 . ? C360 C365 1.3900 . ? C361 C362 1.3900 . ? C362 C363 1.3900 . ? C363 C364 1.3900 . ? C364 C365 1.3900 . ? C370 C371 1.3900 . ? C370 C375 1.3900 . ? C371 C372 1.3900 . ? C372 C373 1.3900 . ? C373 C374 1.3900 . ? C374 C375 1.3900 . ? C380 C381 1.3900 . ? C380 C385 1.3900 . ? C381 C382 1.3900 . ? C382 C383 1.3900 . ? C383 C384 1.3900 . ? C384 C385 1.3900 . ? C390 C391 1.3900 . ? C390 C395 1.3900 . ? C391 C392 1.3900 . ? C392 C393 1.3900 . ? C393 C394 1.3900 . ? C394 C395 1.3900 . ? Ce1 N3 2.504(4) . ? Ce1 N2 2.538(4) . ? Ce1 N1 2.596(4) . ? Ce1 N8 2.618(4) . ? Ce1 N7 2.640(4) . ? Ce1 N25 2.658(4) . ? Ce1 N4 2.664(4) . ? Ce2 N13 2.504(4) . ? Ce2 N12 2.511(4) . ? Ce2 N11 2.598(4) . ? Ce2 N18 2.601(4) . ? Ce2 N14 2.645(4) . ? Ce2 N17 2.696(4) . ? Ce2 N5 2.744(4) . ? Ce3 N23 2.512(4) . ? Ce3 N22 2.557(4) . ? Ce3 N28 2.612(4) . ? Ce3 N24 2.615(4) . ? Ce3 N21 2.621(4) . ? Ce3 N27 2.698(4) . ? Ce3 N15 2.707(4) . ? 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 N1 C1 C2 119.9(4) . . ? N2 C2 C1 121.5(4) . . ? N2 C2 C3 110.8(4) . . ? C1 C2 C3 127.5(5) . . ? C4 C3 C2 105.9(5) . . ? C3 C4 C5 107.2(4) . . ? N2 C5 C4 110.7(4) . . ? N2 C5 C6 123.4(4) . . ? C4 C5 C6 125.8(4) . . ? C5 C6 C11 112.9(4) . . ? C5 C6 C9A 97.4(7) . . ? C11 C6 C9A 123.8(8) . . ? C5 C6 C7 110.5(4) . . ? C11 C6 C7 109.2(4) . . ? C9A C6 C7 102.0(8) . . ? C5 C6 C9 111.9(5) . . ? C11 C6 C9 101.2(5) . . ? C9A C6 C9 22.8(6) . . ? C7 C6 C9 110.8(5) . . ? C6 C7 C8 115.1(5) . . ? C10 C9 C6 113.8(6) . . ? C10A C9A C6 109.1(12) . . ? N3 C11 C12 110.1(4) . . ? N3 C11 C6 123.2(4) . . ? C12 C11 C6 126.7(4) . . ? C13 C12 C11 107.5(4) . . ? C12 C13 C14 106.2(4) . . ? N3 C14 C13 110.3(4) . . ? N3 C14 C15 122.2(4) . . ? C13 C14 C15 127.2(4) . . ? N4 C15 C14 122.8(4) . . ? C17 C16 N4 116.0(4) . . ? C17 C16 C23 117.8(4) . . ? N4 C16 C23 125.7(4) . . ? C16 C17 C19 123.4(4) . . ? C20 C19 C17 118.4(4) . . ? C20 C19 C18 121.6(4) . . ? C17 C19 C18 120.1(5) . . ? C22 C20 C19 119.2(4) . . ? C22 C20 C21 119.6(4) . . ? C19 C20 C21 121.2(4) . . ? C20 C22 C23 122.7(4) . . ? C22 C23 C16 118.5(4) . . ? C22 C23 N5 115.9(4) . . ? C16 C23 N5 125.4(4) . . ? N5 C24 C25 133.2(4) . . ? N6 C25 C26 107.4(4) . . ? N6 C25 C24 127.9(4) . . ? C26 C25 C24 124.6(5) . . ? C25 C26 C27 107.4(5) . . ? C28 C27 C26 108.3(5) . . ? N6 C28 C27 107.6(4) . . ? N6 C28 C29 120.8(4) . . ? C27 C28 C29 131.6(4) . . ? C28 C29 C34 109.8(4) . . ? C28 C29 C32 109.3(4) . . ? C34 C29 C32 108.8(4) . . ? C28 C29 C30 109.4(4) . . ? C34 C29 C30 108.9(4) . . ? C32 C29 C30 110.7(4) . . ? C31 C30 C29 117.2(5) . . ? C33 C32 C29 114.0(5) . . ? N7 C34 C35 110.9(5) . . ? N7 C34 C29 122.6(4) . . ? C35 C34 C29 126.3(4) . . ? C36 C35 C34 106.7(4) . . ? C35 C36 C37 106.6(5) . . ? N7 C37 C36 110.9(4) . . ? N7 C37 C38 121.3(4) . . ? C36 C37 C38 127.5(5) . . ? N8 C38 C37 121.2(4) . . ? C46 C39 C40 119.2(4) . . ? C46 C39 N8 115.4(4) . . ? C40 C39 N8 125.4(4) . . ? C41 C40 C39 121.4(5) . . ? C40 C41 C43 119.6(4) . . ? C40 C41 C42 119.6(5) . . ? C43 C41 C42 120.8(5) . . ? C45 C43 C41 119.0(4) . . ? C45 C43 C44 120.0(5) . . ? C41 C43 C44 121.1(5) . . ? C46 C45 C43 121.6(5) . . ? C45 C46 C39 119.2(4) . . ? C45 C46 N1 126.4(4) . . ? C39 C46 N1 114.4(4) . . ? N11 C101 C102 120.0(4) . . ? N12 C102 C103 110.7(4) . . ? N12 C102 C101 120.3(4) . . ? C103 C102 C101 128.7(5) . . ? C102 C103 C104 106.6(4) . . ? C103 C104 C105 106.7(4) . . ? N12 C105 C104 110.2(4) . . ? N12 C105 C106 121.0(4) . . ? C104 C105 C106 128.7(4) . . ? C111 C106 C105 109.4(4) . . ? C111 C106 C107 108.2(4) . . ? C105 C106 C107 108.9(4) . . ? C111 C106 C109 110.6(4) . . ? C105 C106 C109 109.2(4) . . ? C107 C106 C109 110.4(4) . . ? C108 C107 C106 115.1(4) . . ? C110 C109 C106 115.8(4) . . ? N13 C111 C112 109.7(4) . . ? N13 C111 C106 120.5(4) . . ? C112 C111 C106 129.8(4) . . ? C113 C112 C111 108.2(4) . . ? C112 C113 C114 105.9(4) . . ? N13 C114 C115 120.6(4) . . ? N13 C114 C113 110.0(4) . . ? C115 C114 C113 129.3(4) . . ? N14 C115 C114 120.8(4) . . ? C117 C116 C123 117.3(4) . . ? C117 C116 N14 115.9(4) . . ? C123 C116 N14 126.4(4) . . ? C116 C117 C118 124.2(4) . . ? C117 C118 C120 118.1(4) . . ? C117 C118 C119 120.2(4) . . ? C120 C118 C119 121.7(4) . . ? C122 C120 C118 118.5(4) . . ? C122 C120 C121 120.5(4) . . ? C118 C120 C121 121.0(5) . . ? C123 C122 C120 123.2(4) . . ? C122 C123 C116 118.8(4) . . ? C122 C123 N15 116.1(4) . . ? C116 C123 N15 124.6(4) . . ? N15 C124 C125 133.1(5) . . ? N16 C125 C126 106.9(4) . . ? N16 C125 C124 126.5(4) . . ? C126 C125 C124 126.6(5) . . ? C127 C126 C125 108.2(4) . . ? C126 C127 C128 108.1(4) . . ? N16 C128 C127 107.0(4) . . ? N16 C128 C129 121.2(4) . . ? C127 C128 C129 131.5(4) . . ? C128 C129 C134 108.6(3) . . ? C128 C129 C132 109.7(4) . . ? C134 C129 C132 110.3(4) . . ? C128 C129 C130 108.5(4) . . ? C134 C129 C130 108.9(4) . . ? C132 C129 C130 110.8(3) . . ? C131 C130 C129 115.2(4) . . ? C133 C132 C129 115.0(4) . . ? N17 C134 C135 111.6(4) . . ? N17 C134 C129 122.2(4) . . ? C135 C134 C129 126.2(4) . . ? C136 C135 C134 107.1(4) . . ? C135 C136 C137 106.1(4) . . ? C138 C137 N17 122.3(4) . . ? C138 C137 C136 126.8(4) . . ? N17 C137 C136 110.6(4) . . ? N18 C138 C137 121.8(4) . . ? C140 C139 C146 119.4(4) . . ? C140 C139 N18 125.4(4) . . ? C146 C139 N18 115.1(4) . . ? C141 C140 C139 121.5(4) . . ? C140 C141 C143 119.0(4) . . ? C140 C141 C142 120.1(5) . . ? C143 C141 C142 120.9(4) . . ? C145 C143 C141 119.3(4) . . ? C145 C143 C144 120.3(5) . . ? C141 C143 C144 120.3(4) . . ? C143 C145 C146 121.7(4) . . ? C145 C146 C139 119.0(4) . . ? C145 C146 N11 125.7(4) . . ? C139 C146 N11 114.8(4) . . ? N21 C201 C202 120.7(4) . . ? N22 C202 C203 110.8(4) . . ? N22 C202 C201 119.5(4) . . ? C203 C202 C201 129.7(4) . . ? C204 C203 C202 106.1(4) . . ? C203 C204 C205 107.3(4) . . ? N22 C205 C204 110.3(4) . . ? N22 C205 C206 120.4(4) . . ? C204 C205 C206 129.3(4) . . ? C205 C206 C211 107.9(4) . . ? C205 C206 C209 108.4(4) . . ? C211 C206 C209 109.3(4) . . ? C205 C206 C207 109.4(4) . . ? C211 C206 C207 110.6(4) . . ? C209 C206 C207 111.2(4) . . ? C208 C207 C206 115.0(5) . . ? C210 C209 C206 116.2(4) . . ? N23 C211 C212 111.4(4) . . ? N23 C211 C206 119.6(4) . . ? C212 C211 C206 129.0(4) . . ? C213 C212 C211 106.6(4) . . ? C212 C213 C214 106.3(4) . . ? N23 C214 C215 119.5(4) . . ? N23 C214 C213 110.3(4) . . ? C215 C214 C213 130.1(4) . . ? N24 C215 C214 121.4(4) . . ? C217 C216 N24 116.3(4) . . ? C217 C216 C223 117.0(4) . . ? N24 C216 C223 126.5(4) . . ? C218 C217 C216 124.6(4) . . ? C217 C218 C220 118.7(4) . . ? C217 C218 C219 119.0(4) . . ? C220 C218 C219 122.3(4) . . ? C222 C220 C218 117.5(4) . . ? C222 C220 C221 120.0(4) . . ? C218 C220 C221 122.5(4) . . ? C223 C222 C220 124.2(4) . . ? C222 C223 C216 118.0(4) . . ? C222 C223 N25 115.9(4) . . ? C216 C223 N25 125.9(4) . . ? N25 C224 C225 133.5(4) . . ? N26 C225 C226 106.8(4) . . ? N26 C225 C224 126.9(4) . . ? C226 C225 C224 126.2(4) . . ? C225 C226 C227 108.0(4) . . ? C228 C227 C226 107.9(4) . . ? N26 C228 C227 107.5(4) . . ? N26 C228 C229 120.3(4) . . ? C227 C228 C229 131.6(4) . . ? C228 C229 C234 109.8(4) . . ? C228 C229 C232 109.8(4) . . ? C234 C229 C232 109.5(4) . . ? C228 C229 C230 107.6(4) . . ? C234 C229 C230 109.7(4) . . ? C232 C229 C230 110.4(4) . . ? C231 C230 C229 115.6(4) . . ? C233 C232 C229 114.8(4) . . ? N27 C234 C235 111.6(4) . . ? N27 C234 C229 123.0(4) . . ? C235 C234 C229 125.1(4) . . ? C236 C235 C234 105.8(4) . . ? C235 C236 C237 107.7(4) . . ? C236 C237 N27 110.4(4) . . ? C236 C237 C238 126.3(4) . . ? N27 C237 C238 123.0(4) . . ? N28 C238 C237 122.4(4) . . ? C240 C239 C246 119.1(4) . . ? C240 C239 N28 125.5(4) . . ? C246 C239 N28 115.3(4) . . ? C241 C240 C239 121.8(5) . . ? C240 C241 C243 118.8(5) . . ? C240 C241 C242 119.5(5) . . ? C243 C241 C242 121.7(5) . . ? C245 C243 C241 119.4(5) . . ? C245 C243 C244 119.8(5) . . ? C241 C243 C244 120.7(5) . . ? C243 C245 C246 121.6(5) . . ? C245 C246 C239 119.2(4) . . ? C245 C246 N21 125.4(4) . . ? C239 C246 N21 115.4(4) . . ? C301 C300 C305 120.0 . . ? C300 C301 C302 120.0 . . ? C303 C302 C301 120.0 . . ? C302 C303 C304 120.0 . . ? C305 C304 C303 120.0 . . ? C304 C305 C300 120.0 . . ? C311 C310 C315 120.0 . . ? C310 C311 C312 120.0 . . ? C313 C312 C311 120.0 . . ? C314 C313 C312 120.0 . . ? C313 C314 C315 120.0 . . ? C314 C315 C310 120.0 . . ? C321 C320 C325 120.0 . . ? C320 C321 C322 120.0 . . ? C323 C322 C321 120.0 . . ? C322 C323 C324 120.0 . . ? C325 C324 C323 120.0 . . ? C324 C325 C320 120.0 . . ? C331 C330 C335 120.0 . . ? C330 C331 C332 120.0 . . ? C333 C332 C331 120.0 . . ? C332 C333 C334 120.0 . . ? C335 C334 C333 120.0 . . ? C334 C335 C330 120.0 . . ? C341 C340 C345 120.0 . . ? C340 C341 C342 120.0 . . ? C343 C342 C341 120.0 . . ? C344 C343 C342 120.0 . . ? C343 C344 C345 120.0 . . ? C344 C345 C340 120.0 . . ? C351 C350 C355 120.0 . . ? C352 C351 C350 120.0 . . ? C351 C352 C353 120.0 . . ? C354 C353 C352 120.0 . . ? C355 C354 C353 120.0 . . ? C354 C355 C350 120.0 . . ? C361 C360 C365 120.0 . . ? C362 C361 C360 120.0 . . ? C363 C362 C361 120.0 . . ? C362 C363 C364 120.0 . . ? C365 C364 C363 120.0 . . ? C364 C365 C360 120.0 . . ? C371 C370 C375 120.0 . . ? C372 C371 C370 120.0 . . ? C373 C372 C371 120.0 . . ? C372 C373 C374 120.0 . . ? C375 C374 C373 120.0 . . ? C374 C375 C370 120.0 . . ? C381 C380 C385 120.0 . . ? C382 C381 C380 120.0 . . ? C381 C382 C383 120.0 . . ? C384 C383 C382 120.0 . . ? C383 C384 C385 120.0 . . ? C384 C385 C380 120.0 . . ? C391 C390 C395 120.0 . . ? C390 C391 C392 120.0 . . ? C393 C392 C391 120.0 . . ? C394 C393 C392 120.0 . . ? C393 C394 C395 120.0 . . ? C394 C395 C390 120.0 . . ? N3 Ce1 N2 68.06(12) . . ? N3 Ce1 N1 127.96(12) . . ? N2 Ce1 N1 65.52(12) . . ? N3 Ce1 N8 169.79(12) . . ? N2 Ce1 N8 121.63(12) . . ? N1 Ce1 N8 59.47(12) . . ? N3 Ce1 N7 113.68(12) . . ? N2 Ce1 N7 125.00(12) . . ? N1 Ce1 N7 111.50(12) . . ? N8 Ce1 N7 64.54(12) . . ? N3 Ce1 N25 81.07(12) . . ? N2 Ce1 N25 88.50(12) . . ? N1 Ce1 N25 75.56(11) . . ? N8 Ce1 N25 95.40(12) . . ? N7 Ce1 N25 146.14(12) . . ? N3 Ce1 N4 67.01(12) . . ? N2 Ce1 N4 134.07(12) . . ? N1 Ce1 N4 144.30(11) . . ? N8 Ce1 N4 102.87(12) . . ? N7 Ce1 N4 82.32(11) . . ? N25 Ce1 N4 75.77(11) . . ? N13 Ce2 N12 70.34(12) . . ? N13 Ce2 N11 129.25(12) . . ? N12 Ce2 N11 65.27(12) . . ? N13 Ce2 N18 167.16(12) . . ? N12 Ce2 N18 121.71(12) . . ? N11 Ce2 N18 59.68(12) . . ? N13 Ce2 N14 65.56(12) . . ? N12 Ce2 N14 134.08(12) . . ? N11 Ce2 N14 140.88(11) . . ? N18 Ce2 N14 101.66(12) . . ? N13 Ce2 N17 112.99(11) . . ? N12 Ce2 N17 126.46(11) . . ? N11 Ce2 N17 112.58(11) . . ? N18 Ce2 N17 64.74(11) . . ? N14 Ce2 N17 83.51(11) . . ? N13 Ce2 N5 84.58(12) . . ? N12 Ce2 N5 88.88(11) . . ? N11 Ce2 N5 71.50(11) . . ? N18 Ce2 N5 90.93(11) . . ? N14 Ce2 N5 75.13(11) . . ? N17 Ce2 N5 143.64(11) . . ? N23 Ce3 N22 68.51(12) . . ? N23 Ce3 N28 172.49(12) . . ? N22 Ce3 N28 118.91(12) . . ? N23 Ce3 N24 65.20(11) . . ? N22 Ce3 N24 131.38(12) . . ? N28 Ce3 N24 107.92(11) . . ? N23 Ce3 N21 127.47(12) . . ? N22 Ce3 N21 64.08(12) . . ? N28 Ce3 N21 59.72(12) . . ? N24 Ce3 N21 142.29(11) . . ? N23 Ce3 N27 109.63(12) . . ? N22 Ce3 N27 127.77(11) . . ? N28 Ce3 N27 65.36(11) . . ? N24 Ce3 N27 82.36(11) . . ? N21 Ce3 N27 116.55(11) . . ? N23 Ce3 N15 97.89(12) . . ? N22 Ce3 N15 102.90(12) . . ? N28 Ce3 N15 81.94(12) . . ? N24 Ce3 N15 70.26(11) . . ? N21 Ce3 N15 72.65(11) . . ? N27 Ce3 N15 128.05(11) . . ? C1 N1 C46 120.8(4) . . ? C1 N1 Ce1 117.4(3) . . ? C46 N1 Ce1 121.6(3) . . ? C5 N2 C2 105.3(4) . . ? C5 N2 Ce1 138.0(3) . . ? C2 N2 Ce1 115.7(3) . . ? C11 N3 C14 105.9(4) . . ? C11 N3 Ce1 139.8(3) . . ? C14 N3 Ce1 113.9(3) . . ? C15 N4 C16 120.7(4) . . ? C15 N4 Ce1 110.8(3) . . ? C16 N4 Ce1 128.4(3) . . ? C24 N5 C23 120.8(4) . . ? C24 N5 Ce2 115.6(3) . . ? C23 N5 Ce2 123.1(3) . . ? C28 N6 C25 109.4(4) . . ? C34 N7 C37 105.0(4) . . ? C34 N7 Ce1 140.6(3) . . ? C37 N7 Ce1 112.0(3) . . ? C38 N8 C39 122.2(4) . . ? C38 N8 Ce1 117.1(3) . . ? C39 N8 Ce1 120.5(3) . . ? C101 N11 C146 121.6(4) . . ? C101 N11 Ce2 117.2(3) . . ? C146 N11 Ce2 121.1(3) . . ? C105 N12 C102 105.7(4) . . ? C105 N12 Ce2 136.7(3) . . ? C102 N12 Ce2 117.2(3) . . ? C111 N13 C114 106.1(4) . . ? C111 N13 Ce2 133.7(3) . . ? C114 N13 Ce2 112.0(3) . . ? C115 N14 C116 120.7(4) . . ? C115 N14 Ce2 110.8(3) . . ? C116 N14 Ce2 128.4(3) . . ? C124 N15 C123 122.0(4) . . ? C124 N15 Ce3 120.3(3) . . ? C123 N15 Ce3 115.7(3) . . ? C128 N16 C125 109.7(4) . . ? C134 N17 C137 104.6(3) . . ? C134 N17 Ce2 143.2(3) . . ? C137 N17 Ce2 110.1(3) . . ? C138 N18 C139 121.8(4) . . ? C138 N18 Ce2 117.7(3) . . ? C139 N18 Ce2 120.4(3) . . ? C201 N21 C246 120.7(4) . . ? C201 N21 Ce3 118.0(3) . . ? C246 N21 Ce3 121.3(3) . . ? C205 N22 C202 105.5(4) . . ? C205 N22 Ce3 136.4(3) . . ? C202 N22 Ce3 117.5(3) . . ? C211 N23 C214 105.3(4) . . ? C211 N23 Ce3 136.1(3) . . ? C214 N23 Ce3 112.3(3) . . ? C215 N24 C216 122.0(4) . . ? C215 N24 Ce3 111.4(3) . . ? C216 N24 Ce3 125.8(3) . . ? C224 N25 C223 122.3(4) . . ? C224 N25 Ce1 109.2(3) . . ? C223 N25 Ce1 128.2(3) . . ? C228 N26 C225 109.7(4) . . ? C234 N27 C237 104.4(4) . . ? C234 N27 Ce3 144.8(3) . . ? C237 N27 Ce3 109.5(3) . . ? C238 N28 C239 121.2(4) . . ? C238 N28 Ce3 116.9(3) . . ? C239 N28 Ce3 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.462 _refine_diff_density_min -2.161 _refine_diff_density_rms 0.126 data_jl8030_CeHLTHF2 _database_code_depnum_ccdc_archive 'CCDC 727812' #TrackingRef 'combinednew.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H65 Ce N8 O2' _chemical_formula_sum 'C54 H65 Ce N8 O2' _chemical_formula_weight 998.26 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.4691(5) _cell_length_b 12.2848(2) _cell_length_c 23.6793(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.8990(10) _cell_angle_gamma 90.00 _cell_volume 6033.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 60.8 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 0.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3087 _exptl_absorpt_correction_T_max 0.4330 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; Grown from saturated THF solution at -20 C ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 69526 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 30.55 _reflns_number_total 16459 _reflns_number_gt 13157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen, 2004)' _refine_special_details ; The asymmetric unit contains one molecule of the cerium macrocycle, three and a half molecules of THF . After conventional attempts to describe the disorder failed, the disorder was modeled using the SQUEEZE routine of PLATON. SQUEEZE found two distinct voids, with a total solvent accessible volume of 1740.9 A^3^ and 550 e^-^ in the unit cell, and 138 e^-^ in the asymmetric unit. One THF requires approximately 40 e^-^ in the asymmetric unit. The refinement was much more stable after modeling with SQUEEZE. The molecules of THF, though absent from the atom list, were included in calculations of molecular formula and dependent metrics. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+0.8931P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16459 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.004 _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 0.468538(6) 0.125282(10) 0.703465(6) 0.01879(5) Uani 1 1 d . . . N1 N 0.44636(10) 0.22028(17) 0.59935(9) 0.0225(4) Uani 1 1 d . . . N2 N 0.51537(10) 0.31843(17) 0.72468(9) 0.0234(4) Uani 1 1 d . . . N3 N 0.48599(10) 0.21850(17) 0.81742(9) 0.0233(4) Uani 1 1 d . . . N5 N 0.61991(10) 0.15603(18) 0.90636(10) 0.0266(4) Uani 1 1 d . . . H5A H 0.5794 0.1402 0.8803 0.032 Uiso 1 1 calc R . . N6 N 0.54245(10) -0.01506(16) 0.79519(9) 0.0218(4) Uani 1 1 d . . . N7 N 0.40692(10) -0.04263(17) 0.71152(9) 0.0233(4) Uani 1 1 d . . . N8 N 0.36372(10) 0.06066(17) 0.60156(10) 0.0241(4) Uani 1 1 d . . . N4 N 0.54115(12) 0.30911(19) 0.95508(11) 0.0343(5) Uani 1 1 d . . . C1 C 0.35165(13) 0.1049(2) 0.54718(12) 0.0275(5) Uani 1 1 d . . . H1 H 0.3149 0.0823 0.5093 0.033 Uiso 1 1 calc R . . C2 C 0.39258(12) 0.1861(2) 0.54383(11) 0.0256(5) Uani 1 1 d . . . C3 C 0.38433(13) 0.2507(2) 0.49210(12) 0.0303(6) Uani 1 1 d . . . H3 H 0.3513 0.2441 0.4492 0.036 Uiso 1 1 calc R . . C4 C 0.43380(13) 0.3262(2) 0.51559(12) 0.0294(5) Uani 1 1 d . . . H4 H 0.4413 0.3817 0.4919 0.035 Uiso 1 1 calc R . . C5 C 0.47101(12) 0.3051(2) 0.58139(11) 0.0236(5) Uani 1 1 d . . . C6 C 0.53166(12) 0.3616(2) 0.62992(12) 0.0245(5) Uani 1 1 d . . . C7 C 0.54550(13) 0.4635(2) 0.59946(13) 0.0318(6) Uani 1 1 d . . . H7A H 0.5435 0.4419 0.5583 0.038 Uiso 1 1 calc R . . H7B H 0.5108 0.5174 0.5900 0.038 Uiso 1 1 calc R . . C8 C 0.58839(12) 0.2807(2) 0.65225(13) 0.0314(6) Uani 1 1 d . . . H8A H 0.6271 0.3150 0.6869 0.038 Uiso 1 1 calc R . . H8B H 0.5780 0.2156 0.6703 0.038 Uiso 1 1 calc R . . C9 C 0.61028(15) 0.5185(3) 0.64030(15) 0.0416(7) Uani 1 1 d . . . H9A H 0.6148 0.5816 0.6174 0.062 Uiso 1 1 calc R . . H9B H 0.6452 0.4667 0.6490 0.062 Uiso 1 1 calc R . . H9C H 0.6125 0.5424 0.6808 0.062 Uiso 1 1 calc R . . C10 C 0.60438(16) 0.2442(3) 0.59985(16) 0.0473(8) Uani 1 1 d . . . H10A H 0.6408 0.1934 0.6177 0.071 Uiso 1 1 calc R . . H10B H 0.6159 0.3078 0.5823 0.071 Uiso 1 1 calc R . . H10C H 0.5668 0.2080 0.5658 0.071 Uiso 1 1 calc R . . C11 C 0.52209(12) 0.3950(2) 0.68675(12) 0.0252(5) Uani 1 1 d . . . C12 C 0.51609(14) 0.4999(2) 0.70639(13) 0.0331(6) Uani 1 1 d . . . H12 H 0.5187 0.5666 0.6874 0.040 Uiso 1 1 calc R . . C13 C 0.50552(15) 0.4876(2) 0.75906(14) 0.0353(6) Uani 1 1 d . . . H13 H 0.4996 0.5441 0.7832 0.042 Uiso 1 1 calc R . . C14 C 0.50522(13) 0.3758(2) 0.76947(12) 0.0270(5) Uani 1 1 d . . . C15 C 0.49181(12) 0.3236(2) 0.81492(12) 0.0254(5) Uani 1 1 d . . . H15 H 0.4868 0.3673 0.8454 0.031 Uiso 1 1 calc R . . C16 C 0.47302(12) 0.1773(2) 0.86669(11) 0.0224(5) Uani 1 1 d . . . C17 C 0.43229(12) 0.0871(2) 0.85162(11) 0.0233(5) Uani 1 1 d . . . H17 H 0.4170 0.0553 0.8105 0.028 Uiso 1 1 calc R . . C18 C 0.41300(12) 0.0413(2) 0.89327(12) 0.0263(5) Uani 1 1 d . . . C19 C 0.36780(16) -0.0542(3) 0.87236(16) 0.0437(7) Uani 1 1 d . . . H19A H 0.3591 -0.0764 0.9073 0.065 Uiso 1 1 calc R . . H19B H 0.3875 -0.1149 0.8609 0.065 Uiso 1 1 calc R . . H19C H 0.3273 -0.0336 0.8352 0.065 Uiso 1 1 calc R . . C20 C 0.43509(12) 0.0876(2) 0.95380(12) 0.0269(5) Uani 1 1 d . . . C21 C 0.41322(15) 0.0457(3) 1.00064(14) 0.0386(7) Uani 1 1 d . . . H21A H 0.3839 -0.0161 0.9817 0.058 Uiso 1 1 calc R . . H21B H 0.3907 0.1038 1.0106 0.058 Uiso 1 1 calc R . . H21C H 0.4508 0.0221 1.0400 0.058 Uiso 1 1 calc R . . C22 C 0.47686(13) 0.1751(2) 0.97003(12) 0.0289(5) Uani 1 1 d . . . H22 H 0.4917 0.2066 1.0112 0.035 Uiso 1 1 calc R . . C23 C 0.49848(12) 0.2199(2) 0.92899(12) 0.0258(5) Uani 1 1 d . . . C25 C 0.60040(15) 0.3085(2) 0.96711(13) 0.0354(6) Uani 1 1 d . . . H25 H 0.6233 0.3712 0.9900 0.042 Uiso 1 1 calc R . . C26 C 0.64022(14) 0.2341(2) 0.95381(13) 0.0329(6) Uani 1 1 d . . . C27 C 0.70662(14) 0.2314(3) 0.98417(14) 0.0402(7) Uani 1 1 d . . . H27 H 0.7342 0.2761 1.0191 0.048 Uiso 1 1 calc R . . C28 C 0.72650(14) 0.1518(3) 0.95491(14) 0.0393(7) Uani 1 1 d . . . H28 H 0.7698 0.1320 0.9667 0.047 Uiso 1 1 calc R . . C29 C 0.67163(13) 0.1070(2) 0.90563(12) 0.0294(6) Uani 1 1 d . . . C30 C 0.66151(12) 0.0316(2) 0.85112(12) 0.0268(5) Uani 1 1 d . . . C31 C 0.72242(13) -0.0391(3) 0.87076(14) 0.0359(6) Uani 1 1 d . . . H31A H 0.7602 0.0095 0.8841 0.043 Uiso 1 1 calc R . . H31B H 0.7292 -0.0839 0.9082 0.043 Uiso 1 1 calc R . . C32 C 0.64923(13) 0.1026(2) 0.79226(13) 0.0315(6) Uani 1 1 d . . . H32A H 0.6324 0.0556 0.7539 0.038 Uiso 1 1 calc R . . H32B H 0.6156 0.1572 0.7856 0.038 Uiso 1 1 calc R . . C33 C 0.71935(17) -0.1142(3) 0.81830(18) 0.0483(8) Uani 1 1 d . . . H33A H 0.7595 -0.1561 0.8343 0.072 Uiso 1 1 calc R . . H33B H 0.7138 -0.0707 0.7814 0.072 Uiso 1 1 calc R . . H33C H 0.6829 -0.1643 0.8055 0.072 Uiso 1 1 calc R . . C34 C 0.70939(14) 0.1620(3) 0.79870(16) 0.0460(8) Uani 1 1 d . . . H34A H 0.6982 0.2054 0.7602 0.069 Uiso 1 1 calc R . . H34B H 0.7425 0.1085 0.8040 0.069 Uiso 1 1 calc R . . H34C H 0.7259 0.2100 0.8361 0.069 Uiso 1 1 calc R . . C35 C 0.60419(12) -0.0408(2) 0.83720(11) 0.0245(5) Uani 1 1 d . . . C36 C 0.60755(14) -0.1428(2) 0.86560(13) 0.0312(6) Uani 1 1 d . . . H36 H 0.6454 -0.1776 0.8967 0.037 Uiso 1 1 calc R . . C37 C 0.54588(14) -0.1825(2) 0.83989(12) 0.0303(6) Uani 1 1 d . . . H37 H 0.5328 -0.2502 0.8495 0.036 Uiso 1 1 calc R . . C38 C 0.50584(13) -0.10388(19) 0.79667(12) 0.0240(5) Uani 1 1 d . . . C39 C 0.44026(13) -0.1163(2) 0.75366(12) 0.0266(5) Uani 1 1 d . . . H39 H 0.4192 -0.1813 0.7553 0.032 Uiso 1 1 calc R . . C40 C 0.34242(12) -0.0654(2) 0.66551(11) 0.0241(5) Uani 1 1 d . . . C41 C 0.30175(14) -0.1377(2) 0.67531(13) 0.0301(6) Uani 1 1 d . . . H41 H 0.3167 -0.1717 0.7158 0.036 Uiso 1 1 calc R . . C42 C 0.23992(14) -0.1607(2) 0.62703(14) 0.0341(6) Uani 1 1 d . . . C43 C 0.19924(16) -0.2439(3) 0.63894(16) 0.0481(8) Uani 1 1 d . . . H43A H 0.1575 -0.2512 0.6006 0.072 Uiso 1 1 calc R . . H43B H 0.1925 -0.2202 0.6749 0.072 Uiso 1 1 calc R . . H43C H 0.2214 -0.3143 0.6491 0.072 Uiso 1 1 calc R . . C44 C 0.21744(14) -0.1081(2) 0.56784(13) 0.0320(6) Uani 1 1 d . . . C45 C 0.15174(15) -0.1337(3) 0.51344(15) 0.0425(7) Uani 1 1 d . . . H45A H 0.1302 -0.1874 0.5276 0.064 Uiso 1 1 calc R . . H45B H 0.1565 -0.1634 0.4775 0.064 Uiso 1 1 calc R . . H45C H 0.1259 -0.0670 0.5000 0.064 Uiso 1 1 calc R . . C46 C 0.25708(13) -0.0336(2) 0.55879(12) 0.0296(5) Uani 1 1 d . . . H46 H 0.2413 0.0033 0.5190 0.036 Uiso 1 1 calc R . . C47 C 0.32000(12) -0.0116(2) 0.60710(12) 0.0255(5) Uani 1 1 d . . . O1 O 0.37166(8) 0.24095(15) 0.68580(8) 0.0285(4) Uani 1 1 d . . . C100 C 0.35063(14) 0.3372(2) 0.64530(14) 0.0347(6) Uani 1 1 d . . . H10D H 0.3428 0.3196 0.6015 0.042 Uiso 1 1 calc R . . H10E H 0.3836 0.3954 0.6628 0.042 Uiso 1 1 calc R . . C101 C 0.28885(18) 0.3727(3) 0.64509(18) 0.0512(9) Uani 1 1 d . . . H10F H 0.2570 0.3983 0.6022 0.061 Uiso 1 1 calc R . . H10G H 0.2971 0.4318 0.6764 0.061 Uiso 1 1 calc R . . C102 C 0.26528(18) 0.2702(4) 0.6639(2) 0.0665(12) Uani 1 1 d . . . H10J H 0.2389 0.2883 0.6852 0.080 Uiso 1 1 calc R . . H10K H 0.2396 0.2239 0.6261 0.080 Uiso 1 1 calc R . . C103 C 0.32590(14) 0.2161(3) 0.70828(15) 0.0381(7) Uani 1 1 d . . . H10H H 0.3412 0.2439 0.7523 0.046 Uiso 1 1 calc R . . H10I H 0.3195 0.1365 0.7083 0.046 Uiso 1 1 calc R . . O2 O 0.51497(9) -0.01496(15) 0.65265(9) 0.0315(4) Uani 1 1 d . B . C200 C 0.5333(2) -0.1278(2) 0.67207(17) 0.0475(8) Uani 1 1 d . B . H20A H 0.4949 -0.1721 0.6637 0.057 Uiso 1 1 calc R . . H20B H 0.5643 -0.1320 0.7182 0.057 Uiso 1 1 calc R . . C201 C 0.5639(3) -0.1675(4) 0.6323(2) 0.0785(15) Uani 1 1 d . . . H20C H 0.6110 -0.1764 0.6590 0.094 Uiso 1 1 calc R A 1 H20D H 0.5452 -0.2383 0.6121 0.094 Uiso 1 1 calc R A 1 C202 C 0.5495(4) -0.0812(4) 0.5823(3) 0.113(2) Uani 1 1 d . B 1 H20E H 0.5899 -0.0466 0.5879 0.135 Uiso 1 1 calc R B 1 H20F H 0.5271 -0.1133 0.5390 0.135 Uiso 1 1 calc R B 1 C203 C 0.5105(3) -0.0056(3) 0.59055(19) 0.0760(15) Uani 1 1 d . . . H20G H 0.4652 -0.0170 0.5577 0.091 Uiso 1 1 calc R B 1 H20H H 0.5236 0.0685 0.5850 0.091 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ce1 0.01768(7) 0.01817(7) 0.01974(7) 0.00050(5) 0.00810(5) -0.00053(5) N1 0.0193(10) 0.0251(10) 0.0214(9) 0.0015(8) 0.0082(8) 0.0005(8) N2 0.0211(10) 0.0223(10) 0.0238(10) 0.0015(8) 0.0081(9) -0.0026(8) N3 0.0229(10) 0.0263(10) 0.0201(9) -0.0009(8) 0.0097(8) -0.0016(8) N5 0.0187(10) 0.0312(11) 0.0226(10) -0.0006(8) 0.0036(8) -0.0053(9) N6 0.0219(10) 0.0202(10) 0.0241(10) 0.0022(8) 0.0114(9) -0.0005(8) N7 0.0242(10) 0.0234(10) 0.0222(9) -0.0041(8) 0.0107(9) -0.0055(8) N8 0.0214(10) 0.0243(10) 0.0254(10) -0.0023(8) 0.0101(9) -0.0029(8) N4 0.0399(14) 0.0327(12) 0.0276(11) -0.0082(9) 0.0137(11) -0.0081(11) C1 0.0286(13) 0.0263(13) 0.0256(12) -0.0039(10) 0.0110(11) -0.0009(10) C2 0.0239(12) 0.0287(13) 0.0221(11) -0.0005(10) 0.0090(10) 0.0009(10) C3 0.0277(13) 0.0378(15) 0.0200(11) 0.0028(10) 0.0066(11) 0.0029(11) C4 0.0302(14) 0.0333(14) 0.0233(12) 0.0076(10) 0.0113(11) 0.0013(11) C5 0.0212(12) 0.0251(12) 0.0235(11) 0.0064(9) 0.0095(10) 0.0041(10) C6 0.0215(12) 0.0245(12) 0.0265(12) 0.0055(9) 0.0104(10) -0.0007(10) C7 0.0327(15) 0.0321(14) 0.0288(13) 0.0107(11) 0.0128(12) -0.0053(11) C8 0.0213(12) 0.0390(15) 0.0328(13) 0.0114(12) 0.0118(11) 0.0042(11) C9 0.0381(17) 0.0419(17) 0.0426(16) 0.0091(13) 0.0172(14) -0.0131(14) C10 0.0402(18) 0.056(2) 0.056(2) 0.0095(16) 0.0310(17) 0.0115(15) C11 0.0227(12) 0.0237(12) 0.0243(11) 0.0062(9) 0.0069(10) -0.0025(9) C12 0.0402(16) 0.0232(13) 0.0352(14) 0.0041(11) 0.0169(13) -0.0046(11) C13 0.0446(17) 0.0229(13) 0.0402(15) -0.0022(11) 0.0214(14) -0.0024(12) C14 0.0272(13) 0.0227(12) 0.0275(12) -0.0005(10) 0.0098(11) -0.0017(10) C15 0.0250(13) 0.0244(12) 0.0238(11) -0.0020(10) 0.0088(10) -0.0011(10) C16 0.0220(12) 0.0230(12) 0.0221(11) -0.0005(9) 0.0103(10) -0.0006(9) C17 0.0230(12) 0.0244(11) 0.0222(11) -0.0040(9) 0.0103(10) -0.0021(10) C18 0.0204(12) 0.0289(13) 0.0301(12) 0.0040(10) 0.0123(10) 0.0021(10) C19 0.0421(18) 0.0447(18) 0.0493(18) -0.0002(14) 0.0256(15) -0.0152(14) C20 0.0256(13) 0.0302(13) 0.0271(12) 0.0056(10) 0.0141(11) 0.0092(11) C21 0.0410(17) 0.0467(18) 0.0368(15) 0.0086(13) 0.0255(14) 0.0055(14) C22 0.0306(14) 0.0332(14) 0.0232(12) 0.0010(10) 0.0129(11) 0.0071(11) C23 0.0248(12) 0.0278(13) 0.0249(12) -0.0025(10) 0.0116(10) 0.0008(10) C25 0.0409(17) 0.0338(15) 0.0256(13) -0.0071(11) 0.0107(12) -0.0123(13) C26 0.0319(15) 0.0315(14) 0.0286(13) 0.0022(11) 0.0085(12) -0.0085(12) C27 0.0284(15) 0.0439(17) 0.0320(14) -0.0007(13) 0.0004(12) -0.0112(13) C28 0.0217(13) 0.0454(17) 0.0366(15) 0.0053(13) 0.0019(12) -0.0033(12) C29 0.0211(12) 0.0310(14) 0.0270(12) 0.0076(10) 0.0037(10) -0.0021(10) C30 0.0194(12) 0.0309(13) 0.0290(12) 0.0094(10) 0.0103(10) 0.0035(10) C31 0.0196(13) 0.0443(17) 0.0406(15) 0.0152(13) 0.0114(12) 0.0088(12) C32 0.0222(13) 0.0373(15) 0.0332(14) 0.0113(11) 0.0114(11) 0.0019(11) C33 0.0362(17) 0.050(2) 0.063(2) 0.0063(16) 0.0268(17) 0.0157(15) C34 0.0267(15) 0.056(2) 0.0500(18) 0.0266(16) 0.0137(14) 0.0023(14) C35 0.0237(12) 0.0251(12) 0.0242(11) 0.0063(9) 0.0107(10) 0.0043(10) C36 0.0341(15) 0.0265(13) 0.0315(13) 0.0112(10) 0.0140(12) 0.0074(11) C37 0.0381(15) 0.0228(13) 0.0314(13) 0.0046(10) 0.0174(12) 0.0008(11) C38 0.0294(13) 0.0194(11) 0.0259(12) 0.0006(9) 0.0153(11) -0.0018(10) C39 0.0318(14) 0.0226(12) 0.0275(12) -0.0031(10) 0.0155(11) -0.0072(10) C40 0.0228(12) 0.0237(12) 0.0247(11) -0.0081(9) 0.0103(10) -0.0082(10) C41 0.0327(14) 0.0308(14) 0.0291(13) -0.0057(10) 0.0164(12) -0.0106(11) C42 0.0324(15) 0.0367(15) 0.0346(14) -0.0117(12) 0.0169(13) -0.0147(12) C43 0.0407(18) 0.056(2) 0.0501(18) -0.0098(16) 0.0235(16) -0.0281(16) C44 0.0260(13) 0.0336(15) 0.0331(14) -0.0113(11) 0.0110(12) -0.0089(11) C45 0.0302(15) 0.0520(19) 0.0369(15) -0.0128(14) 0.0089(13) -0.0177(14) C46 0.0274(13) 0.0297(13) 0.0273(12) -0.0063(10) 0.0091(11) -0.0055(11) C47 0.0253(13) 0.0241(12) 0.0264(12) -0.0066(10) 0.0116(10) -0.0038(10) O1 0.0226(9) 0.0312(10) 0.0297(9) 0.0012(7) 0.0106(8) 0.0048(8) C100 0.0311(15) 0.0366(15) 0.0344(14) 0.0079(12) 0.0137(12) 0.0114(12) C101 0.047(2) 0.063(2) 0.0515(19) 0.0174(17) 0.0293(17) 0.0270(17) C102 0.043(2) 0.095(3) 0.068(3) 0.028(2) 0.032(2) 0.022(2) C103 0.0320(15) 0.0419(16) 0.0446(16) 0.0037(13) 0.0214(14) 0.0063(13) O2 0.0393(11) 0.0283(10) 0.0318(9) -0.0005(8) 0.0206(9) 0.0092(8) C200 0.075(3) 0.0303(15) 0.0454(18) 0.0036(13) 0.0353(19) 0.0114(16) C201 0.132(4) 0.057(2) 0.072(3) 0.017(2) 0.069(3) 0.051(3) C202 0.223(7) 0.074(3) 0.106(4) 0.040(3) 0.130(5) 0.081(4) C203 0.141(4) 0.057(2) 0.062(2) 0.0189(19) 0.074(3) 0.046(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 O1 2.5443(17) . ? Ce1 N1 2.5514(19) . ? Ce1 N2 2.564(2) . ? Ce1 N7 2.577(2) . ? Ce1 O2 2.6136(17) . ? Ce1 N8 2.636(2) . ? Ce1 N6 2.678(2) . ? Ce1 N3 2.7796(19) . ? N1 C5 1.354(3) . ? N1 C2 1.395(3) . ? N2 C11 1.359(3) . ? N2 C14 1.384(3) . ? N3 C15 1.302(3) . ? N3 C16 1.429(3) . ? N5 C29 1.362(3) . ? N5 C26 1.382(3) . ? N5 H5A 0.8800 . ? N6 C35 1.357(3) . ? N6 C38 1.399(3) . ? N7 C39 1.303(3) . ? N7 C40 1.419(3) . ? N8 C1 1.301(3) . ? N8 C47 1.409(3) . ? N4 C25 1.282(4) . ? N4 C23 1.417(3) . ? C1 C2 1.412(4) . ? C1 H1 0.9500 . ? C2 C3 1.395(3) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.409(3) . ? C4 H4 0.9500 . ? C5 C6 1.516(4) . ? C6 C11 1.521(4) . ? C6 C8 1.543(4) . ? C6 C7 1.553(3) . ? C7 C9 1.525(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.522(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.400(4) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.396(4) . ? C13 H13 0.9500 . ? C14 C15 1.409(3) . ? C15 H15 0.9500 . ? C16 C17 1.397(3) . ? C16 C23 1.408(3) . ? C17 C18 1.382(3) . ? C17 H17 0.9500 . ? C18 C20 1.396(4) . ? C18 C19 1.502(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.383(4) . ? C20 C21 1.514(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.402(3) . ? C22 H22 0.9500 . ? C25 C26 1.443(4) . ? C25 H25 0.9500 . ? C26 C27 1.378(4) . ? C27 C28 1.399(5) . ? C27 H27 0.9500 . ? C28 C29 1.384(4) . ? C28 H28 0.9500 . ? C29 C30 1.515(4) . ? C30 C35 1.515(4) . ? C30 C31 1.547(4) . ? C30 C32 1.553(3) . ? C31 C33 1.522(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.532(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.407(3) . ? C36 C37 1.371(4) . ? C36 H36 0.9500 . ? C37 C38 1.401(4) . ? C37 H37 0.9500 . ? C38 C39 1.401(4) . ? C39 H39 0.9500 . ? C40 C47 1.395(3) . ? C40 C41 1.400(3) . ? C41 C42 1.393(4) . ? C41 H41 0.9500 . ? C42 C44 1.403(4) . ? C42 C43 1.513(4) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.391(4) . ? C44 C45 1.509(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.408(4) . ? C46 H46 0.9500 . ? O1 C103 1.437(3) . ? O1 C100 1.456(3) . ? C100 C101 1.512(4) . ? C100 H10D 0.9900 . ? C100 H10E 0.9900 . ? C101 C102 1.524(5) . ? C101 H10F 0.9900 . ? C101 H10G 0.9900 . ? C102 C103 1.473(5) . ? C102 H10J 0.9900 . ? C102 H10K 0.9900 . ? C103 H10H 0.9900 . ? C103 H10I 0.9900 . ? O2 C203 1.429(4) . ? O2 C200 1.461(3) . ? C200 C201 1.508(5) . ? C200 H20A 0.9900 . ? C200 H20B 0.9900 . ? C201 C202 1.505(6) . ? C201 H20C 0.9900 . ? C201 H20D 0.9900 . ? C202 C203 1.380(5) . ? C202 H20E 0.9900 . ? C202 H20F 0.9900 . ? C203 H20G 0.9900 . ? C203 H20H 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ce1 N1 79.81(6) . . ? O1 Ce1 N2 77.50(6) . . ? N1 Ce1 N2 68.96(6) . . ? O1 Ce1 N7 88.28(6) . . ? N1 Ce1 N7 124.74(6) . . ? N2 Ce1 N7 158.47(6) . . ? O1 Ce1 O2 145.64(6) . . ? N1 Ce1 O2 78.30(6) . . ? N2 Ce1 O2 117.86(6) . . ? N7 Ce1 O2 82.86(6) . . ? O1 Ce1 N8 68.80(6) . . ? N1 Ce1 N8 64.67(6) . . ? N2 Ce1 N8 126.08(6) . . ? N7 Ce1 N8 60.73(6) . . ? O2 Ce1 N8 77.97(6) . . ? O1 Ce1 N6 133.06(6) . . ? N1 Ce1 N6 147.13(6) . . ? N2 Ce1 N6 112.41(6) . . ? N7 Ce1 N6 66.28(6) . . ? O2 Ce1 N6 72.40(6) . . ? N8 Ce1 N6 121.42(6) . . ? O1 Ce1 N3 69.14(6) . . ? N1 Ce1 N3 128.34(7) . . ? N2 Ce1 N3 64.76(6) . . ? N7 Ce1 N3 95.21(6) . . ? O2 Ce1 N3 144.56(6) . . ? N8 Ce1 N3 131.54(6) . . ? N6 Ce1 N3 74.49(6) . . ? C5 N1 C2 105.50(19) . . ? C5 N1 Ce1 137.04(16) . . ? C2 N1 Ce1 117.29(15) . . ? C11 N2 C14 105.6(2) . . ? C11 N2 Ce1 133.02(16) . . ? C14 N2 Ce1 114.18(15) . . ? C15 N3 C16 117.1(2) . . ? C15 N3 Ce1 109.58(15) . . ? C16 N3 Ce1 130.97(15) . . ? C29 N5 C26 110.3(2) . . ? C29 N5 H5A 124.9 . . ? C26 N5 H5A 124.9 . . ? C35 N6 C38 104.9(2) . . ? C35 N6 Ce1 144.02(16) . . ? C38 N6 Ce1 110.48(15) . . ? C39 N7 C40 119.6(2) . . ? C39 N7 Ce1 117.13(16) . . ? C40 N7 Ce1 122.36(15) . . ? C1 N8 C47 121.6(2) . . ? C1 N8 Ce1 117.26(17) . . ? C47 N8 Ce1 120.87(15) . . ? C25 N4 C23 124.3(2) . . ? N8 C1 C2 120.8(2) . . ? N8 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C3 C2 N1 110.4(2) . . ? C3 C2 C1 129.2(2) . . ? N1 C2 C1 119.9(2) . . ? C4 C3 C2 106.4(2) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? C3 C4 C5 106.9(2) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? N1 C5 C4 110.7(2) . . ? N1 C5 C6 120.1(2) . . ? C4 C5 C6 129.1(2) . . ? C5 C6 C11 108.6(2) . . ? C5 C6 C8 108.6(2) . . ? C11 C6 C8 109.3(2) . . ? C5 C6 C7 110.1(2) . . ? C11 C6 C7 110.1(2) . . ? C8 C6 C7 110.1(2) . . ? C9 C7 C6 115.2(2) . . ? C9 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C9 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C10 C8 C6 114.4(2) . . ? C10 C8 H8A 108.7 . . ? C6 C8 H8A 108.7 . . ? C10 C8 H8B 108.7 . . ? C6 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 110.9(2) . . ? N2 C11 C6 120.6(2) . . ? C12 C11 C6 128.4(2) . . ? C13 C12 C11 106.6(2) . . ? C13 C12 H12 126.7 . . ? C11 C12 H12 126.7 . . ? C12 C13 C14 106.5(2) . . ? C12 C13 H13 126.8 . . ? C14 C13 H13 126.8 . . ? N2 C14 C13 110.4(2) . . ? N2 C14 C15 122.3(2) . . ? C13 C14 C15 127.2(2) . . ? N3 C15 C14 123.5(2) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C17 C16 C23 117.8(2) . . ? C17 C16 N3 117.0(2) . . ? C23 C16 N3 125.2(2) . . ? C18 C17 C16 123.6(2) . . ? C18 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? C17 C18 C20 118.6(2) . . ? C17 C18 C19 119.9(2) . . ? C20 C18 C19 121.4(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C18 118.4(2) . . ? C22 C20 C21 120.0(2) . . ? C18 C20 C21 121.6(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 C23 123.5(2) . . ? C20 C22 H22 118.3 . . ? C23 C22 H22 118.3 . . ? C22 C23 C16 117.8(2) . . ? C22 C23 N4 114.4(2) . . ? C16 C23 N4 127.7(2) . . ? N4 C25 C26 134.5(3) . . ? N4 C25 H25 112.7 . . ? C26 C25 H25 112.7 . . ? C27 C26 N5 106.5(3) . . ? C27 C26 C25 126.2(3) . . ? N5 C26 C25 127.2(2) . . ? C26 C27 C28 108.4(3) . . ? C26 C27 H27 125.8 . . ? C28 C27 H27 125.8 . . ? C29 C28 C27 107.5(3) . . ? C29 C28 H28 126.2 . . ? C27 C28 H28 126.2 . . ? N5 C29 C28 107.3(3) . . ? N5 C29 C30 119.7(2) . . ? C28 C29 C30 132.4(3) . . ? C29 C30 C35 108.3(2) . . ? C29 C30 C31 109.5(2) . . ? C35 C30 C31 109.7(2) . . ? C29 C30 C32 108.1(2) . . ? C35 C30 C32 111.2(2) . . ? C31 C30 C32 110.0(2) . . ? C33 C31 C30 114.3(2) . . ? C33 C31 H31A 108.7 . . ? C30 C31 H31A 108.7 . . ? C33 C31 H31B 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C34 C32 C30 113.8(2) . . ? C34 C32 H32A 108.8 . . ? C30 C32 H32A 108.8 . . ? C34 C32 H32B 108.8 . . ? C30 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N6 C35 C36 111.1(2) . . ? N6 C35 C30 123.9(2) . . ? C36 C35 C30 125.0(2) . . ? C37 C36 C35 107.0(2) . . ? C37 C36 H36 126.5 . . ? C35 C36 H36 126.5 . . ? C36 C37 C38 106.7(2) . . ? C36 C37 H37 126.7 . . ? C38 C37 H37 126.7 . . ? N6 C38 C39 123.1(2) . . ? N6 C38 C37 110.2(2) . . ? C39 C38 C37 126.1(2) . . ? N7 C39 C38 122.9(2) . . ? N7 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? C47 C40 C41 119.6(2) . . ? C47 C40 N7 116.1(2) . . ? C41 C40 N7 124.3(2) . . ? C42 C41 C40 121.5(3) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C44 119.1(3) . . ? C41 C42 C43 119.3(3) . . ? C44 C42 C43 121.5(3) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C42 119.4(2) . . ? C46 C44 C45 119.7(3) . . ? C42 C44 C45 120.9(3) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 C47 121.6(3) . . ? C44 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? C40 C47 C46 118.7(2) . . ? C40 C47 N8 115.9(2) . . ? C46 C47 N8 125.3(2) . . ? C103 O1 C100 109.5(2) . . ? C103 O1 Ce1 125.86(16) . . ? C100 O1 Ce1 124.30(15) . . ? O1 C100 C101 105.4(2) . . ? O1 C100 H10D 110.7 . . ? C101 C100 H10D 110.7 . . ? O1 C100 H10E 110.7 . . ? C101 C100 H10E 110.7 . . ? H10D C100 H10E 108.8 . . ? C100 C101 C102 103.8(3) . . ? C100 C101 H10F 111.0 . . ? C102 C101 H10F 111.0 . . ? C100 C101 H10G 111.0 . . ? C102 C101 H10G 111.0 . . ? H10F C101 H10G 109.0 . . ? C103 C102 C101 102.7(3) . . ? C103 C102 H10J 111.2 . . ? C101 C102 H10J 111.2 . . ? C103 C102 H10K 111.2 . . ? C101 C102 H10K 111.2 . . ? H10J C102 H10K 109.1 . . ? O1 C103 C102 106.2(3) . . ? O1 C103 H10H 110.5 . . ? C102 C103 H10H 110.5 . . ? O1 C103 H10I 110.5 . . ? C102 C103 H10I 110.5 . . ? H10H C103 H10I 108.7 . . ? C203 O2 C200 105.6(2) . . ? C203 O2 Ce1 125.12(18) . . ? C200 O2 Ce1 127.25(16) . . ? O2 C200 C201 105.4(3) . . ? O2 C200 H20A 110.7 . . ? C201 C200 H20A 110.7 . . ? O2 C200 H20B 110.7 . . ? C201 C200 H20B 110.7 . . ? H20A C200 H20B 108.8 . . ? C202 C201 C200 105.4(3) . . ? C202 C201 H20C 110.7 . . ? C200 C201 H20C 110.7 . . ? C202 C201 H20D 110.7 . . ? C200 C201 H20D 110.7 . . ? H20C C201 H20D 108.8 . . ? C203 C202 C201 106.4(3) . . ? C203 C202 H20E 110.4 . . ? C201 C202 H20E 110.4 . . ? C203 C202 H20F 110.4 . . ? C201 C202 H20F 110.4 . . ? H20E C202 H20F 108.6 . . ? C202 C203 O2 110.9(3) . . ? C202 C203 H20G 109.5 . . ? O2 C203 H20G 109.5 . . ? C202 C203 H20H 109.5 . . ? O2 C203 H20H 109.5 . . ? H20G C203 H20H 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ce1 N1 C5 101.0(2) . . . . ? N2 Ce1 N1 C5 20.6(2) . . . . ? N7 Ce1 N1 C5 -178.3(2) . . . . ? O2 Ce1 N1 C5 -105.6(2) . . . . ? N8 Ce1 N1 C5 172.3(3) . . . . ? N6 Ce1 N1 C5 -78.5(3) . . . . ? N3 Ce1 N1 C5 48.1(3) . . . . ? O1 Ce1 N1 C2 -73.37(17) . . . . ? N2 Ce1 N1 C2 -153.78(18) . . . . ? N7 Ce1 N1 C2 7.3(2) . . . . ? O2 Ce1 N1 C2 79.98(17) . . . . ? N8 Ce1 N1 C2 -2.12(16) . . . . ? N6 Ce1 N1 C2 107.17(18) . . . . ? N3 Ce1 N1 C2 -126.25(16) . . . . ? O1 Ce1 N2 C11 -91.9(2) . . . . ? N1 Ce1 N2 C11 -8.2(2) . . . . ? N7 Ce1 N2 C11 -141.7(2) . . . . ? O2 Ce1 N2 C11 55.1(2) . . . . ? N8 Ce1 N2 C11 -40.2(2) . . . . ? N6 Ce1 N2 C11 136.4(2) . . . . ? N3 Ce1 N2 C11 -164.5(2) . . . . ? O1 Ce1 N2 C14 53.42(17) . . . . ? N1 Ce1 N2 C14 137.17(18) . . . . ? N7 Ce1 N2 C14 3.7(3) . . . . ? O2 Ce1 N2 C14 -159.53(16) . . . . ? N8 Ce1 N2 C14 105.11(17) . . . . ? N6 Ce1 N2 C14 -78.27(18) . . . . ? N3 Ce1 N2 C14 -19.20(16) . . . . ? O1 Ce1 N3 C15 -67.50(17) . . . . ? N1 Ce1 N3 C15 -10.4(2) . . . . ? N2 Ce1 N3 C15 18.12(16) . . . . ? N7 Ce1 N3 C15 -153.65(17) . . . . ? O2 Ce1 N3 C15 121.34(17) . . . . ? N8 Ce1 N3 C15 -98.77(18) . . . . ? N6 Ce1 N3 C15 142.74(18) . . . . ? O1 Ce1 N3 C16 94.1(2) . . . . ? N1 Ce1 N3 C16 151.21(19) . . . . ? N2 Ce1 N3 C16 179.7(2) . . . . ? N7 Ce1 N3 C16 7.9(2) . . . . ? O2 Ce1 N3 C16 -77.1(2) . . . . ? N8 Ce1 N3 C16 62.8(2) . . . . ? N6 Ce1 N3 C16 -55.68(19) . . . . ? O1 Ce1 N6 C35 -128.0(3) . . . . ? N1 Ce1 N6 C35 51.3(3) . . . . ? N2 Ce1 N6 C35 -34.3(3) . . . . ? N7 Ce1 N6 C35 169.1(3) . . . . ? O2 Ce1 N6 C35 79.3(3) . . . . ? N8 Ce1 N6 C35 142.6(3) . . . . ? N3 Ce1 N6 C35 -87.9(3) . . . . ? O1 Ce1 N6 C38 62.95(17) . . . . ? N1 Ce1 N6 C38 -117.77(16) . . . . ? N2 Ce1 N6 C38 156.67(14) . . . . ? N7 Ce1 N6 C38 0.05(14) . . . . ? O2 Ce1 N6 C38 -89.78(15) . . . . ? N8 Ce1 N6 C38 -26.52(17) . . . . ? N3 Ce1 N6 C38 103.05(16) . . . . ? O1 Ce1 N7 C39 -141.69(18) . . . . ? N1 Ce1 N7 C39 141.97(17) . . . . ? N2 Ce1 N7 C39 -93.5(2) . . . . ? O2 Ce1 N7 C39 71.58(18) . . . . ? N8 Ce1 N7 C39 151.76(19) . . . . ? N6 Ce1 N7 C39 -2.29(16) . . . . ? N3 Ce1 N7 C39 -72.82(18) . . . . ? O1 Ce1 N7 C40 49.34(17) . . . . ? N1 Ce1 N7 C40 -27.0(2) . . . . ? N2 Ce1 N7 C40 97.6(2) . . . . ? O2 Ce1 N7 C40 -97.38(17) . . . . ? N8 Ce1 N7 C40 -17.21(16) . . . . ? N6 Ce1 N7 C40 -171.26(19) . . . . ? N3 Ce1 N7 C40 118.22(17) . . . . ? O1 Ce1 N8 C1 90.39(19) . . . . ? N1 Ce1 N8 C1 1.90(17) . . . . ? N2 Ce1 N8 C1 35.1(2) . . . . ? N7 Ce1 N8 C1 -169.2(2) . . . . ? O2 Ce1 N8 C1 -80.71(18) . . . . ? N6 Ce1 N8 C1 -141.21(17) . . . . ? N3 Ce1 N8 C1 121.74(18) . . . . ? O1 Ce1 N8 C47 -84.21(18) . . . . ? N1 Ce1 N8 C47 -172.70(19) . . . . ? N2 Ce1 N8 C47 -139.46(17) . . . . ? N7 Ce1 N8 C47 16.19(16) . . . . ? O2 Ce1 N8 C47 104.69(18) . . . . ? N6 Ce1 N8 C47 44.19(19) . . . . ? N3 Ce1 N8 C47 -52.9(2) . . . . ? C47 N8 C1 C2 173.0(2) . . . . ? Ce1 N8 C1 C2 -1.5(3) . . . . ? C5 N1 C2 C3 -0.3(3) . . . . ? Ce1 N1 C2 C3 175.69(17) . . . . ? C5 N1 C2 C1 -173.6(2) . . . . ? Ce1 N1 C2 C1 2.4(3) . . . . ? N8 C1 C2 C3 -172.4(3) . . . . ? N8 C1 C2 N1 -0.6(4) . . . . ? N1 C2 C3 C4 0.2(3) . . . . ? C1 C2 C3 C4 172.7(3) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C2 N1 C5 C4 0.4(3) . . . . ? Ce1 N1 C5 C4 -174.45(18) . . . . ? C2 N1 C5 C6 -178.5(2) . . . . ? Ce1 N1 C5 C6 6.7(4) . . . . ? C3 C4 C5 N1 -0.3(3) . . . . ? C3 C4 C5 C6 178.4(2) . . . . ? N1 C5 C6 C11 -53.1(3) . . . . ? C4 C5 C6 C11 128.4(3) . . . . ? N1 C5 C6 C8 65.8(3) . . . . ? C4 C5 C6 C8 -112.8(3) . . . . ? N1 C5 C6 C7 -173.7(2) . . . . ? C4 C5 C6 C7 7.8(4) . . . . ? C5 C6 C7 C9 -171.7(2) . . . . ? C11 C6 C7 C9 68.6(3) . . . . ? C8 C6 C7 C9 -52.1(3) . . . . ? C5 C6 C8 C10 63.8(3) . . . . ? C11 C6 C8 C10 -177.9(2) . . . . ? C7 C6 C8 C10 -56.8(3) . . . . ? C14 N2 C11 C12 -0.3(3) . . . . ? Ce1 N2 C11 C12 147.1(2) . . . . ? C14 N2 C11 C6 -177.8(2) . . . . ? Ce1 N2 C11 C6 -30.4(3) . . . . ? C5 C6 C11 N2 65.6(3) . . . . ? C8 C6 C11 N2 -52.7(3) . . . . ? C7 C6 C11 N2 -173.8(2) . . . . ? C5 C6 C11 C12 -111.4(3) . . . . ? C8 C6 C11 C12 130.3(3) . . . . ? C7 C6 C11 C12 9.2(4) . . . . ? N2 C11 C12 C13 0.3(3) . . . . ? C6 C11 C12 C13 177.6(3) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C11 N2 C14 C13 0.2(3) . . . . ? Ce1 N2 C14 C13 -154.26(19) . . . . ? C11 N2 C14 C15 175.7(2) . . . . ? Ce1 N2 C14 C15 21.3(3) . . . . ? C12 C13 C14 N2 0.0(3) . . . . ? C12 C13 C14 C15 -175.3(3) . . . . ? C16 N3 C15 C14 179.3(2) . . . . ? Ce1 N3 C15 C14 -16.2(3) . . . . ? N2 C14 C15 N3 -2.1(4) . . . . ? C13 C14 C15 N3 172.7(3) . . . . ? C15 N3 C16 C17 144.1(2) . . . . ? Ce1 N3 C16 C17 -16.4(3) . . . . ? C15 N3 C16 C23 -36.5(4) . . . . ? Ce1 N3 C16 C23 162.99(18) . . . . ? C23 C16 C17 C18 3.6(4) . . . . ? N3 C16 C17 C18 -176.9(2) . . . . ? C16 C17 C18 C20 0.2(4) . . . . ? C16 C17 C18 C19 178.6(3) . . . . ? C17 C18 C20 C22 -1.9(4) . . . . ? C19 C18 C20 C22 179.7(3) . . . . ? C17 C18 C20 C21 176.7(2) . . . . ? C19 C18 C20 C21 -1.6(4) . . . . ? C18 C20 C22 C23 -0.2(4) . . . . ? C21 C20 C22 C23 -178.9(2) . . . . ? C20 C22 C23 C16 4.0(4) . . . . ? C20 C22 C23 N4 -179.9(2) . . . . ? C17 C16 C23 C22 -5.5(4) . . . . ? N3 C16 C23 C22 175.1(2) . . . . ? C17 C16 C23 N4 179.0(3) . . . . ? N3 C16 C23 N4 -0.4(4) . . . . ? C25 N4 C23 C22 115.0(3) . . . . ? C25 N4 C23 C16 -69.4(4) . . . . ? C23 N4 C25 C26 8.4(5) . . . . ? C29 N5 C26 C27 -1.3(3) . . . . ? C29 N5 C26 C25 175.5(3) . . . . ? N4 C25 C26 C27 -161.7(3) . . . . ? N4 C25 C26 N5 22.1(5) . . . . ? N5 C26 C27 C28 0.1(3) . . . . ? C25 C26 C27 C28 -176.7(3) . . . . ? C26 C27 C28 C29 1.0(3) . . . . ? C26 N5 C29 C28 2.0(3) . . . . ? C26 N5 C29 C30 -170.2(2) . . . . ? C27 C28 C29 N5 -1.8(3) . . . . ? C27 C28 C29 C30 169.0(3) . . . . ? N5 C29 C30 C35 -43.4(3) . . . . ? C28 C29 C30 C35 146.7(3) . . . . ? N5 C29 C30 C31 -163.0(2) . . . . ? C28 C29 C30 C31 27.2(4) . . . . ? N5 C29 C30 C32 77.2(3) . . . . ? C28 C29 C30 C32 -92.7(3) . . . . ? C29 C30 C31 C33 -176.9(2) . . . . ? C35 C30 C31 C33 64.4(3) . . . . ? C32 C30 C31 C33 -58.2(3) . . . . ? C29 C30 C32 C34 71.9(3) . . . . ? C35 C30 C32 C34 -169.4(3) . . . . ? C31 C30 C32 C34 -47.6(3) . . . . ? C38 N6 C35 C36 -0.6(3) . . . . ? Ce1 N6 C35 C36 -170.0(2) . . . . ? C38 N6 C35 C30 179.4(2) . . . . ? Ce1 N6 C35 C30 10.0(4) . . . . ? C29 C30 C35 N6 89.6(3) . . . . ? C31 C30 C35 N6 -151.0(2) . . . . ? C32 C30 C35 N6 -29.0(3) . . . . ? C29 C30 C35 C36 -90.4(3) . . . . ? C31 C30 C35 C36 29.0(3) . . . . ? C32 C30 C35 C36 150.9(3) . . . . ? N6 C35 C36 C37 0.7(3) . . . . ? C30 C35 C36 C37 -179.3(2) . . . . ? C35 C36 C37 C38 -0.5(3) . . . . ? C35 N6 C38 C39 -171.2(2) . . . . ? Ce1 N6 C38 C39 2.2(3) . . . . ? C35 N6 C38 C37 0.3(3) . . . . ? Ce1 N6 C38 C37 173.64(16) . . . . ? C36 C37 C38 N6 0.1(3) . . . . ? C36 C37 C38 C39 171.3(3) . . . . ? C40 N7 C39 C38 173.9(2) . . . . ? Ce1 N7 C39 C38 4.6(3) . . . . ? N6 C38 C39 N7 -4.8(4) . . . . ? C37 C38 C39 N7 -174.9(2) . . . . ? C39 N7 C40 C47 -151.2(2) . . . . ? Ce1 N7 C40 C47 17.5(3) . . . . ? C39 N7 C40 C41 28.2(4) . . . . ? Ce1 N7 C40 C41 -163.15(19) . . . . ? C47 C40 C41 C42 2.6(4) . . . . ? N7 C40 C41 C42 -176.7(2) . . . . ? C40 C41 C42 C44 -1.6(4) . . . . ? C40 C41 C42 C43 176.7(3) . . . . ? C41 C42 C44 C46 -0.5(4) . . . . ? C43 C42 C44 C46 -178.8(3) . . . . ? C41 C42 C44 C45 177.7(3) . . . . ? C43 C42 C44 C45 -0.6(4) . . . . ? C42 C44 C46 C47 1.6(4) . . . . ? C45 C44 C46 C47 -176.6(3) . . . . ? C41 C40 C47 C46 -1.4(4) . . . . ? N7 C40 C47 C46 178.0(2) . . . . ? C41 C40 C47 N8 179.2(2) . . . . ? N7 C40 C47 N8 -1.4(3) . . . . ? C44 C46 C47 C40 -0.7(4) . . . . ? C44 C46 C47 N8 178.7(2) . . . . ? C1 N8 C47 C40 171.1(2) . . . . ? Ce1 N8 C47 C40 -14.5(3) . . . . ? C1 N8 C47 C46 -8.3(4) . . . . ? Ce1 N8 C47 C46 166.1(2) . . . . ? N1 Ce1 O1 C103 152.7(2) . . . . ? N2 Ce1 O1 C103 -136.8(2) . . . . ? N7 Ce1 O1 C103 26.9(2) . . . . ? O2 Ce1 O1 C103 101.6(2) . . . . ? N8 Ce1 O1 C103 86.1(2) . . . . ? N6 Ce1 O1 C103 -27.7(2) . . . . ? N3 Ce1 O1 C103 -69.3(2) . . . . ? N1 Ce1 O1 C100 -20.53(19) . . . . ? N2 Ce1 O1 C100 49.97(19) . . . . ? N7 Ce1 O1 C100 -146.3(2) . . . . ? O2 Ce1 O1 C100 -71.6(2) . . . . ? N8 Ce1 O1 C100 -87.2(2) . . . . ? N6 Ce1 O1 C100 159.08(18) . . . . ? N3 Ce1 O1 C100 117.5(2) . . . . ? C103 O1 C100 C101 1.2(3) . . . . ? Ce1 O1 C100 C101 175.37(19) . . . . ? O1 C100 C101 C102 -21.6(4) . . . . ? C100 C101 C102 C103 33.6(4) . . . . ? C100 O1 C103 C102 20.7(4) . . . . ? Ce1 O1 C103 C102 -153.3(2) . . . . ? C101 C102 C103 O1 -33.5(4) . . . . ? O1 Ce1 O2 C203 46.4(3) . . . . ? N1 Ce1 O2 C203 -5.1(3) . . . . ? N2 Ce1 O2 C203 -63.5(3) . . . . ? N7 Ce1 O2 C203 122.7(3) . . . . ? N8 Ce1 O2 C203 61.2(3) . . . . ? N6 Ce1 O2 C203 -170.0(3) . . . . ? N3 Ce1 O2 C203 -148.4(3) . . . . ? O1 Ce1 O2 C200 -115.1(3) . . . . ? N1 Ce1 O2 C200 -166.6(3) . . . . ? N2 Ce1 O2 C200 135.0(2) . . . . ? N7 Ce1 O2 C200 -38.8(3) . . . . ? N8 Ce1 O2 C200 -100.3(3) . . . . ? N6 Ce1 O2 C200 28.5(2) . . . . ? N3 Ce1 O2 C200 50.1(3) . . . . ? C203 O2 C200 C201 21.9(4) . . . . ? Ce1 O2 C200 C201 -173.7(3) . . . . ? O2 C200 C201 C202 -11.0(6) . . . . ? C200 C201 C202 C203 -4.2(7) . . . . ? C201 C202 C203 O2 18.8(7) . . . . ? C200 O2 C203 C202 -26.2(6) . . . . ? Ce1 O2 C203 C202 169.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.190 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.094 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 871 275 ' ' 2 0.500 -0.500 1.000 870 275 ' ' _platon_squeeze_details ; ; data_UL _database_code_depnum_ccdc_archive 'CCDC 727813' #TrackingRef 'combinednew.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H48 N8 U' _chemical_formula_sum 'C46 H48 N8 U' _chemical_formula_weight 950.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 15.1086(15) _cell_length_b 33.751(4) _cell_length_c 8.3453(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.747(6) _cell_angle_gamma 90.00 _cell_volume 4180.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 9395 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 26.96 _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 3.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7354 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ;Shape and scale corrections using equivalent reflections. Shape function based on spherical harmonics. Highest even and odd order for spherical harmonics: 4 and 1 Laue group: 2/m (b) Friedel opposites are equivalent. ; _exptl_special_details ; Grown from a saturated C6D6 solution in a NMR tube ; _diffrn_ambient_temperature 93(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 'AFC8/Saturn 70' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20447 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4285 _reflns_number_gt 3510 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Farrugia, 1997)' _computing_publication_material 'enCIFer (Allen, 2004)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit contains one molecule of the uranium macrocycle, two and a half molecules of Benzene. After conventional attempts to describe the disorder failed, the disorder was modeled using the SQUEEZE routine of PLATON. SQUEEZE found two distinct voids, with a total solvent accessible volume of 448.6 A^3^ and 207 e^-^ in the unit cell, and 103 e^-^ in the asymmetric unit. One Benzene requires approximately 42 e^-^ in the asymmetric unit. The refinement was much more stable after modeling with SQUEEZE. The molecules of benzene, though absent from the atom list, were included in calculations of molecular formula and dependent metrics. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+111.4366P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00046(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4285 _refine_ls_number_parameters 275 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1676 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 1.0000 0.16792(2) 0.2500 0.0493(3) Uani 1 2 d S . . N1 N 1.0683(5) 0.1926(3) 0.0135(9) 0.043(2) Uani 1 1 d . . . N2 N 1.1054(8) 0.1225(4) 0.1475(13) 0.072(3) Uani 1 1 d . . . N3 N 1.1428(6) 0.1560(3) 0.4398(11) 0.055(3) Uani 1 1 d . B . N4 N 0.9350(5) 0.2279(3) 0.0901(8) 0.040(2) Uani 1 1 d . . . C1 C 1.1003(7) 0.1666(4) -0.0764(13) 0.059(3) Uani 1 1 d . . . H1 H 1.1104 0.1730 -0.1823 0.071 Uiso 1 1 calc R . . C2 C 1.1191(9) 0.1288(5) -0.0103(16) 0.067(4) Uani 1 1 d . . . C3 C 1.1784(10) 0.1011(5) -0.051(2) 0.084(5) Uani 1 1 d . . . H3 H 1.1967 0.0980 -0.1528 0.101 Uiso 1 1 calc R . . C4 C 1.2053(11) 0.0792(5) 0.087(2) 0.089(5) Uani 1 1 d . . . H4 H 1.2475 0.0580 0.0973 0.107 Uiso 1 1 calc R . . C5 C 1.1605(11) 0.0928(4) 0.213(2) 0.080(4) Uani 1 1 d . . . C6 C 1.1780(13) 0.0854(5) 0.394(2) 0.089(5) Uani 1 1 d . B . C7 C 1.2554(16) 0.0545(5) 0.441(2) 0.129(7) Uani 1 1 d DU . . H7A H 1.2693 0.0511 0.5607 0.155 Uiso 1 1 calc R A 1 H7B H 1.3104 0.0639 0.4044 0.155 Uiso 1 1 calc R A 1 C8A C 1.225(3) 0.0134(7) 0.357(4) 0.129(10) Uani 0.53(2) 1 d PDU B 1 H8A1 H 1.2771 -0.0040 0.3631 0.193 Uiso 0.53(2) 1 calc PR B 1 H8A2 H 1.1976 0.0179 0.2418 0.193 Uiso 0.53(2) 1 calc PR B 1 H8A3 H 1.1803 0.0010 0.4125 0.193 Uiso 0.53(2) 1 calc PR B 1 C8 C 1.293(3) 0.0450(11) 0.629(3) 0.134(11) Uani 0.47(2) 1 d PDU B 2 H8A H 1.3406 0.0252 0.6380 0.201 Uiso 0.47(2) 1 calc PR B 2 H8B H 1.2435 0.0348 0.6789 0.201 Uiso 0.47(2) 1 calc PR B 2 H8C H 1.3165 0.0694 0.6849 0.201 Uiso 0.47(2) 1 calc PR B 2 C10 C 1.081(3) 0.0279(9) 0.412(4) 0.112(9) Uani 0.54(2) 1 d PU B 3 H10A H 1.0718 0.0149 0.5125 0.168 Uiso 0.54(2) 1 calc PR B 3 H10B H 1.1358 0.0171 0.3801 0.168 Uiso 0.54(2) 1 calc PR B 3 H10C H 1.0294 0.0230 0.3249 0.168 Uiso 0.54(2) 1 calc PR B 3 C10A C 1.073(3) 0.0613(10) 0.589(4) 0.099(9) Uani 0.46(2) 1 d PU B 4 H10D H 1.0097 0.0544 0.5793 0.149 Uiso 0.46(2) 1 calc PR B 4 H10E H 1.0868 0.0851 0.6561 0.149 Uiso 0.46(2) 1 calc PR B 4 H10F H 1.1108 0.0393 0.6394 0.149 Uiso 0.46(2) 1 calc PR B 4 C9 C 1.0916(16) 0.0683(5) 0.438(3) 0.115(5) Uani 1 1 d U . . H9A H 1.0917 0.0739 0.5548 0.138 Uiso 1 1 calc R B 3 H9B H 1.0391 0.0821 0.3733 0.138 Uiso 1 1 calc R B 3 C11 C 1.1993(10) 0.1240(4) 0.4750(16) 0.066(4) Uani 1 1 d . . . C12 C 1.2781(9) 0.1358(4) 0.5809(14) 0.067(4) Uani 1 1 d . B . H12 H 1.3284 0.1194 0.6218 0.081 Uiso 1 1 calc R . . C13 C 1.2695(8) 0.1755(4) 0.6150(12) 0.058(3) Uani 1 1 d . . . H13 H 1.3118 0.1913 0.6862 0.070 Uiso 1 1 calc R B . C14 C 1.1867(7) 0.1881(4) 0.5251(12) 0.050(3) Uani 1 1 d . . . C15 C 0.8594(6) 0.2237(3) -0.0108(10) 0.040(2) Uani 1 1 d . . . H15 H 0.8351 0.2456 -0.0763 0.048 Uiso 1 1 calc R . . C16 C 0.9988(6) 0.2542(4) 0.0410(9) 0.041(3) Uani 1 1 d . . . C17 C 0.9964(6) 0.2947(4) 0.0358(10) 0.043(3) Uani 1 1 d . . . H17 H 0.9510 0.3083 0.0790 0.052 Uiso 1 1 calc R . . C18 C 1.0601(6) 0.3171(4) -0.0324(11) 0.045(3) Uani 1 1 d . . . C19 C 1.0578(7) 0.3610(4) -0.0323(13) 0.055(3) Uani 1 1 d . . . H19A H 1.1076 0.3711 0.0500 0.083 Uiso 1 1 calc R . . H19B H 1.0004 0.3701 -0.0068 0.083 Uiso 1 1 calc R . . H19C H 1.0640 0.3709 -0.1401 0.083 Uiso 1 1 calc R . . C20 C 1.1269(6) 0.2956(4) -0.0950(10) 0.046(3) Uani 1 1 d . . . C21 C 1.1945(7) 0.3174(4) -0.1745(12) 0.059(3) Uani 1 1 d . . . H21A H 1.2217 0.3389 -0.1027 0.088 Uiso 1 1 calc R . . H21B H 1.1640 0.3286 -0.2787 0.088 Uiso 1 1 calc R . . H21C H 1.2416 0.2990 -0.1937 0.088 Uiso 1 1 calc R . . C22 C 1.1299(6) 0.2555(4) -0.0825(9) 0.048(3) Uani 1 1 d . . . H22 H 1.1766 0.2417 -0.1213 0.058 Uiso 1 1 calc R . . C23 C 1.0673(6) 0.2333(3) -0.0148(9) 0.039(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0453(4) 0.0711(5) 0.0368(3) 0.000 0.0217(2) 0.000 N1 0.034(4) 0.072(6) 0.027(4) -0.013(4) 0.013(3) -0.006(4) N2 0.087(8) 0.081(8) 0.058(6) -0.007(6) 0.039(6) 0.015(6) N3 0.047(5) 0.081(7) 0.042(5) 0.012(5) 0.022(4) 0.008(5) N4 0.030(4) 0.073(6) 0.019(3) -0.004(3) 0.012(3) -0.011(4) C1 0.039(6) 0.102(10) 0.038(5) -0.032(7) 0.015(4) -0.013(6) C2 0.067(8) 0.085(10) 0.056(7) -0.026(7) 0.030(6) -0.006(7) C3 0.064(9) 0.108(13) 0.080(10) -0.059(10) 0.010(8) 0.008(8) C4 0.088(11) 0.083(11) 0.097(12) -0.045(9) 0.020(9) 0.018(9) C5 0.100(12) 0.053(8) 0.095(11) -0.010(7) 0.039(9) 0.005(8) C6 0.118(14) 0.069(10) 0.091(11) 0.002(8) 0.046(10) 0.020(9) C7 0.193(18) 0.088(11) 0.104(12) 0.011(9) 0.023(12) 0.086(12) C8A 0.20(2) 0.086(14) 0.091(17) 0.026(13) 0.010(17) 0.070(17) C8 0.19(2) 0.094(17) 0.109(15) -0.008(15) -0.006(18) 0.098(17) C10 0.17(2) 0.078(12) 0.082(16) -0.021(14) -0.002(16) 0.011(16) C10A 0.14(2) 0.071(15) 0.088(15) 0.034(14) 0.015(15) -0.040(15) C9 0.170(16) 0.078(9) 0.107(11) 0.009(9) 0.050(11) -0.010(11) C11 0.075(9) 0.074(9) 0.058(7) 0.026(6) 0.038(7) 0.024(7) C12 0.068(8) 0.097(10) 0.045(6) 0.034(6) 0.032(6) 0.049(8) C13 0.055(7) 0.101(11) 0.024(4) 0.023(5) 0.020(4) 0.029(6) C14 0.035(5) 0.092(9) 0.030(5) 0.019(5) 0.020(4) 0.013(6) C15 0.033(5) 0.069(7) 0.022(4) -0.007(4) 0.014(4) -0.007(5) C16 0.025(5) 0.084(8) 0.015(4) -0.003(4) 0.006(3) -0.012(5) C17 0.024(5) 0.083(8) 0.021(4) 0.007(4) 0.002(3) -0.001(5) C18 0.026(5) 0.079(8) 0.029(5) 0.005(5) 0.001(4) -0.011(5) C19 0.040(6) 0.084(9) 0.040(5) 0.011(6) 0.004(5) -0.015(6) C20 0.028(5) 0.087(9) 0.021(4) 0.001(5) 0.005(4) -0.020(5) C21 0.042(6) 0.107(10) 0.029(5) 0.011(5) 0.011(4) -0.021(6) C22 0.026(5) 0.107(10) 0.012(4) -0.008(5) 0.005(3) -0.022(5) C23 0.029(5) 0.075(8) 0.014(4) -0.008(4) 0.009(3) -0.010(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 U1 N3 2.459(10) . ? U1 N3 2.459(10) 2_755 ? U1 N2 2.474(10) 2_755 ? U1 N2 2.474(10) . ? U1 N4 2.520(9) 2_755 ? U1 N4 2.520(9) . ? U1 N1 2.533(8) . ? U1 N1 2.533(8) 2_755 ? N1 C1 1.306(13) . ? N1 C23 1.394(14) . ? N2 C5 1.353(18) . ? N2 C2 1.387(16) . ? N3 C11 1.374(15) . ? N3 C14 1.396(16) . ? N4 C15 1.294(12) . ? N4 C16 1.426(12) . ? C1 C2 1.398(19) . ? C1 H1 0.9500 . ? C2 C3 1.379(18) . ? C3 C4 1.36(2) . ? C3 H3 0.9500 . ? C4 C5 1.43(2) . ? C4 H4 0.9500 . ? C5 C6 1.50(2) . ? C6 C11 1.48(2) . ? C6 C9 1.53(3) . ? C6 C7 1.56(2) . ? C7 C8A 1.583(18) . ? C7 C8 1.597(18) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C9 1.39(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10A C9 1.35(4) . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.40(2) . ? C12 C13 1.382(18) . ? C12 H12 0.9500 . ? C13 C14 1.399(15) . ? C13 H13 0.9500 . ? C14 C15 1.382(15) 2_755 ? C15 C14 1.382(15) 2_755 ? C15 H15 0.9500 . ? C16 C17 1.367(16) . ? C16 C23 1.402(14) . ? C17 C18 1.423(13) . ? C17 H17 0.9500 . ? C18 C20 1.421(15) . ? C18 C19 1.482(17) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.357(16) . ? C20 C21 1.510(13) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.404(13) . ? C22 H22 0.9500 . ? 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 N3 U1 N3 161.2(5) . 2_755 ? N3 U1 N2 102.7(4) . 2_755 ? N3 U1 N2 65.0(4) 2_755 2_755 ? N3 U1 N2 65.0(4) . . ? N3 U1 N2 102.7(4) 2_755 . ? N2 U1 N2 103.5(6) 2_755 . ? N3 U1 N4 65.3(3) . 2_755 ? N3 U1 N4 132.9(3) 2_755 2_755 ? N2 U1 N4 121.7(3) 2_755 2_755 ? N2 U1 N4 117.9(3) . 2_755 ? N3 U1 N4 132.9(3) . . ? N3 U1 N4 65.3(3) 2_755 . ? N2 U1 N4 117.9(3) 2_755 . ? N2 U1 N4 121.7(3) . . ? N4 U1 N4 73.2(3) 2_755 . ? N3 U1 N1 96.9(3) . . ? N3 U1 N1 89.3(3) 2_755 . ? N2 U1 N1 148.8(3) 2_755 . ? N2 U1 N1 63.4(3) . . ? N4 U1 N1 88.5(2) 2_755 . ? N4 U1 N1 59.9(3) . . ? N3 U1 N1 89.3(3) . 2_755 ? N3 U1 N1 96.9(3) 2_755 2_755 ? N2 U1 N1 63.4(3) 2_755 2_755 ? N2 U1 N1 148.8(3) . 2_755 ? N4 U1 N1 59.9(3) 2_755 2_755 ? N4 U1 N1 88.5(2) . 2_755 ? N1 U1 N1 141.6(4) . 2_755 ? C1 N1 C23 124.0(9) . . ? C1 N1 U1 118.3(8) . . ? C23 N1 U1 117.6(5) . . ? C5 N2 C2 107.8(11) . . ? C5 N2 U1 135.1(9) . . ? C2 N2 U1 117.0(9) . . ? C11 N3 C14 106.5(11) . . ? C11 N3 U1 134.6(10) . . ? C14 N3 U1 118.5(7) . . ? C15 N4 C16 116.3(8) . . ? C15 N4 U1 117.8(7) . . ? C16 N4 U1 115.8(6) . . ? N1 C1 C2 117.2(10) . . ? N1 C1 H1 121.4 . . ? C2 C1 H1 121.4 . . ? C3 C2 N2 110.3(15) . . ? C3 C2 C1 128.0(13) . . ? N2 C2 C1 117.2(11) . . ? C4 C3 C2 105.6(13) . . ? C4 C3 H3 127.2 . . ? C2 C3 H3 127.2 . . ? C3 C4 C5 109.7(14) . . ? C3 C4 H4 125.2 . . ? C5 C4 H4 125.2 . . ? N2 C5 C4 106.5(14) . . ? N2 C5 C6 120.4(12) . . ? C4 C5 C6 131.8(16) . . ? C11 C6 C5 107.4(12) . . ? C11 C6 C9 109.9(13) . . ? C5 C6 C9 107.9(16) . . ? C11 C6 C7 112.6(16) . . ? C5 C6 C7 110.3(13) . . ? C9 C6 C7 108.6(15) . . ? C6 C7 C8A 109.2(19) . . ? C6 C7 C8 119.4(18) . . ? C8A C7 C8 106(2) . . ? C6 C7 H7A 109.8 . . ? C8A C7 H7A 109.8 . . ? C8 C7 H7A 9.8 . . ? C6 C7 H7B 109.8 . . ? C8A C7 H7B 109.8 . . ? C8 C7 H7B 101.7 . . ? H7A C7 H7B 108.3 . . ? C7 C8A H8A1 109.5 . . ? C7 C8A H8A2 109.5 . . ? C7 C8A H8A3 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? C9 C10A H10D 109.5 . . ? C9 C10A H10E 109.5 . . ? C9 C10A H10F 109.5 . . ? C10A C9 C10 86(2) . . ? C10A C9 C6 128(3) . . ? C10 C9 C6 114(2) . . ? C10A C9 H9A 24.1 . . ? C10 C9 H9A 108.8 . . ? C6 C9 H9A 108.8 . . ? C10A C9 H9B 108.1 . . ? C10 C9 H9B 108.8 . . ? C6 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N3 C11 C12 109.4(13) . . ? N3 C11 C6 121.4(14) . . ? C12 C11 C6 128.8(13) . . ? C13 C12 C11 107.7(11) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 107.1(12) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? C15 C14 N3 116.5(9) 2_755 . ? C15 C14 C13 134.1(13) 2_755 . ? N3 C14 C13 109.2(11) . . ? N4 C15 C14 121.4(10) . 2_755 ? N4 C15 H15 119.3 . . ? C14 C15 H15 119.3 2_755 . ? C17 C16 C23 120.6(9) . . ? C17 C16 N4 128.1(9) . . ? C23 C16 N4 111.2(10) . . ? C16 C17 C18 121.9(10) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C20 C18 C17 117.0(11) . . ? C20 C18 C19 122.0(9) . . ? C17 C18 C19 120.9(10) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C18 119.9(9) . . ? C22 C20 C21 120.4(10) . . ? C18 C20 C21 119.7(11) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 C23 123.1(10) . . ? C20 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? N1 C23 C16 115.1(8) . . ? N1 C23 C22 127.3(9) . . ? C16 C23 C22 117.4(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 U1 N1 C1 78.7(8) . . . . ? N3 U1 N1 C1 -83.4(8) 2_755 . . . ? N2 U1 N1 C1 -50.0(11) 2_755 . . . ? N2 U1 N1 C1 21.2(8) . . . . ? N4 U1 N1 C1 143.6(8) 2_755 . . . ? N4 U1 N1 C1 -145.0(8) . . . . ? N1 U1 N1 C1 176.3(8) 2_755 . . . ? N3 U1 N1 C23 -102.8(7) . . . . ? N3 U1 N1 C23 95.0(7) 2_755 . . . ? N2 U1 N1 C23 128.4(8) 2_755 . . . ? N2 U1 N1 C23 -160.4(8) . . . . ? N4 U1 N1 C23 -37.9(6) 2_755 . . . ? N4 U1 N1 C23 33.4(6) . . . . ? N1 U1 N1 C23 -5.2(6) 2_755 . . . ? N3 U1 N2 C5 41.2(14) . . . . ? N3 U1 N2 C5 -123.6(14) 2_755 . . . ? N2 U1 N2 C5 -56.7(14) 2_755 . . . ? N4 U1 N2 C5 81.0(15) 2_755 . . . ? N4 U1 N2 C5 167.7(13) . . . . ? N1 U1 N2 C5 153.6(16) . . . . ? N1 U1 N2 C5 3.9(19) 2_755 . . . ? N3 U1 N2 C2 -133.9(11) . . . . ? N3 U1 N2 C2 61.2(10) 2_755 . . . ? N2 U1 N2 C2 128.2(11) 2_755 . . . ? N4 U1 N2 C2 -94.1(10) 2_755 . . . ? N4 U1 N2 C2 -7.4(11) . . . . ? N1 U1 N2 C2 -21.5(9) . . . . ? N1 U1 N2 C2 -171.3(8) 2_755 . . . ? N3 U1 N3 C11 17.3(9) 2_755 . . . ? N2 U1 N3 C11 64.4(10) 2_755 . . . ? N2 U1 N3 C11 -34.8(9) . . . . ? N4 U1 N3 C11 -176.3(10) 2_755 . . . ? N4 U1 N3 C11 -145.8(9) . . . . ? N1 U1 N3 C11 -91.2(10) . . . . ? N1 U1 N3 C11 126.9(10) 2_755 . . . ? N3 U1 N3 C14 -170.8(6) 2_755 . . . ? N2 U1 N3 C14 -123.7(7) 2_755 . . . ? N2 U1 N3 C14 137.1(7) . . . . ? N4 U1 N3 C14 -4.3(6) 2_755 . . . ? N4 U1 N3 C14 26.1(8) . . . . ? N1 U1 N3 C14 80.8(7) . . . . ? N1 U1 N3 C14 -61.2(7) 2_755 . . . ? N3 U1 N4 C15 174.8(6) . . . . ? N3 U1 N4 C15 0.7(6) 2_755 . . . ? N2 U1 N4 C15 -39.0(7) 2_755 . . . ? N2 U1 N4 C15 90.7(7) . . . . ? N4 U1 N4 C15 -156.5(7) 2_755 . . . ? N1 U1 N4 C15 105.3(6) . . . . ? N1 U1 N4 C15 -97.6(6) 2_755 . . . ? N3 U1 N4 C16 30.6(7) . . . . ? N3 U1 N4 C16 -143.5(6) 2_755 . . . ? N2 U1 N4 C16 176.8(6) 2_755 . . . ? N2 U1 N4 C16 -53.5(7) . . . . ? N4 U1 N4 C16 59.3(5) 2_755 . . . ? N1 U1 N4 C16 -38.9(6) . . . . ? N1 U1 N4 C16 118.2(6) 2_755 . . . ? C23 N1 C1 C2 163.2(10) . . . . ? U1 N1 C1 C2 -18.4(13) . . . . ? C5 N2 C2 C3 4.2(17) . . . . ? U1 N2 C2 C3 -179.4(9) . . . . ? C5 N2 C2 C1 -154.1(13) . . . . ? U1 N2 C2 C1 22.3(16) . . . . ? N1 C1 C2 C3 -156.3(13) . . . . ? N1 C1 C2 N2 -2.4(18) . . . . ? N2 C2 C3 C4 -3.4(18) . . . . ? C1 C2 C3 C4 151.9(15) . . . . ? C2 C3 C4 C5 1.4(19) . . . . ? C2 N2 C5 C4 -3.2(17) . . . . ? U1 N2 C5 C4 -178.6(10) . . . . ? C2 N2 C5 C6 165.3(14) . . . . ? U1 N2 C5 C6 -10(2) . . . . ? C3 C4 C5 N2 1.1(19) . . . . ? C3 C4 C5 C6 -165.5(17) . . . . ? N2 C5 C6 C11 -47(2) . . . . ? C4 C5 C6 C11 117.7(18) . . . . ? N2 C5 C6 C9 71.0(19) . . . . ? C4 C5 C6 C9 -123.8(19) . . . . ? N2 C5 C6 C7 -170.5(15) . . . . ? C4 C5 C6 C7 -5(3) . . . . ? C11 C6 C7 C8A 176.7(19) . . . . ? C5 C6 C7 C8A -63(2) . . . . ? C9 C6 C7 C8A 55(2) . . . . ? C11 C6 C7 C8 54(3) . . . . ? C5 C6 C7 C8 174(3) . . . . ? C9 C6 C7 C8 -68(3) . . . . ? C11 C6 C9 C10A -55(3) . . . . ? C5 C6 C9 C10A -172(3) . . . . ? C7 C6 C9 C10A 68(3) . . . . ? C11 C6 C9 C10 -161(2) . . . . ? C5 C6 C9 C10 82(2) . . . . ? C7 C6 C9 C10 -37(3) . . . . ? C14 N3 C11 C12 -0.2(11) . . . . ? U1 N3 C11 C12 172.4(7) . . . . ? C14 N3 C11 C6 -174.4(11) . . . . ? U1 N3 C11 C6 -1.8(17) . . . . ? C5 C6 C11 N3 53.3(17) . . . . ? C9 C6 C11 N3 -63.8(18) . . . . ? C7 C6 C11 N3 174.9(13) . . . . ? C5 C6 C11 C12 -119.7(15) . . . . ? C9 C6 C11 C12 123.2(16) . . . . ? C7 C6 C11 C12 2(2) . . . . ? N3 C11 C12 C13 1.4(12) . . . . ? C6 C11 C12 C13 175.1(12) . . . . ? C11 C12 C13 C14 -2.1(11) . . . . ? C11 N3 C14 C15 -178.4(8) . . . 2_755 ? U1 N3 C14 C15 7.6(10) . . . 2_755 ? C11 N3 C14 C13 -1.1(10) . . . . ? U1 N3 C14 C13 -175.1(6) . . . . ? C12 C13 C14 C15 178.6(10) . . . 2_755 ? C12 C13 C14 N3 2.0(10) . . . . ? C16 N4 C15 C14 147.2(9) . . . 2_755 ? U1 N4 C15 C14 3.1(10) . . . 2_755 ? C15 N4 C16 C17 73.5(12) . . . . ? U1 N4 C16 C17 -141.7(8) . . . . ? C15 N4 C16 C23 -102.9(10) . . . . ? U1 N4 C16 C23 41.9(8) . . . . ? C23 C16 C17 C18 2.9(13) . . . . ? N4 C16 C17 C18 -173.2(8) . . . . ? C16 C17 C18 C20 -0.2(13) . . . . ? C16 C17 C18 C19 -178.2(9) . . . . ? C17 C18 C20 C22 -2.4(13) . . . . ? C19 C18 C20 C22 175.5(9) . . . . ? C17 C18 C20 C21 177.8(8) . . . . ? C19 C18 C20 C21 -4.2(14) . . . . ? C18 C20 C22 C23 2.4(13) . . . . ? C21 C20 C22 C23 -177.9(8) . . . . ? C1 N1 C23 C16 152.8(9) . . . . ? U1 N1 C23 C16 -25.6(10) . . . . ? C1 N1 C23 C22 -31.6(14) . . . . ? U1 N1 C23 C22 150.1(7) . . . . ? C17 C16 C23 N1 173.1(8) . . . . ? N4 C16 C23 N1 -10.2(10) . . . . ? C17 C16 C23 C22 -3.0(12) . . . . ? N4 C16 C23 C22 173.7(7) . . . . ? C20 C22 C23 N1 -175.2(8) . . . . ? C20 C22 C23 C16 0.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.778 _refine_diff_density_min -2.970 _refine_diff_density_rms 0.193 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 -0.007 224 103 ' ' 2 1.000 0.500 -0.028 224 103 ' ' _platon_squeeze_details ; ;