data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 N8 O12 Sm, C5 H6 N' _chemical_formula_sum 'C33 H30 N9 O12 Sm' _chemical_formula_weight 895.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 23.473(8) _cell_length_b 8.794(3) _cell_length_c 36.244(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7482(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3592 _exptl_absorpt_coefficient_mu 1.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7347 _exptl_absorpt_correction_T_max 0.8529 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 155952 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.36 _reflns_number_total 13706 _reflns_number_gt 13111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-2004' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-32' _computing_publication_material 'WinGX' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+8.0800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.290(6) _refine_ls_number_reflns 13706 _refine_ls_number_parameters 991 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Sm1 Sm 0.928747(7) 0.654911(18) 0.749167(5) 0.02792(4) Uani 1 1 d . . . C4 C 1.14823(18) 0.4017(5) 0.75249(17) 0.0536(12) Uani 1 1 d . . . H4 H 1.1833 0.3728 0.7636 0.064 Uiso 1 1 calc R . . O2 O 1.02397(12) 0.6275(3) 0.77115(7) 0.0441(7) Uani 1 1 d . . . N8 N 0.84037(13) 0.3859(3) 0.72296(8) 0.0292(6) Uani 1 1 d . . . O1 O 0.99558(13) 0.5243(3) 0.70877(8) 0.0435(7) Uani 1 1 d . . . C10 C 0.91521(19) 0.8489(4) 0.86654(11) 0.0376(9) Uani 1 1 d . . . C25 C 0.78468(17) 0.1658(5) 0.71251(13) 0.0401(10) Uani 1 1 d . . . H25 H 0.7576 0.1109 0.6983 0.048 Uiso 1 1 calc R . . O8 O 0.90198(11) 0.4050(3) 0.77083(7) 0.0372(6) Uani 1 1 d . . . C9 C 0.9725(2) 0.8366(5) 0.88442(12) 0.0494(11) Uani 1 1 d . . . C28 C 0.86555(14) 0.3251(4) 0.75449(11) 0.0327(8) Uani 1 1 d . . . N5 N 0.91211(13) 0.9251(3) 0.68681(8) 0.0315(7) Uani 1 1 d . . . O4 O 0.84730(11) 0.7536(3) 0.78246(7) 0.0378(6) Uani 1 1 d . . . C19 C 0.89386(16) 0.9940(5) 0.65481(10) 0.0361(8) Uani 1 1 d . . . O12 O 0.72556(15) 0.3449(4) 0.65973(9) 0.0613(9) Uani 1 1 d . . . N1 N 1.06166(12) 0.5371(3) 0.75411(10) 0.0365(7) Uani 1 1 d . . . O6 O 0.89464(12) 0.7837(3) 0.69559(7) 0.0410(7) Uani 1 1 d . . . O7 O 0.85760(11) 0.5266(3) 0.71380(7) 0.0339(6) Uani 1 1 d . . . C24 C 0.80020(15) 0.3113(4) 0.70211(10) 0.0327(8) Uani 1 1 d . . . C13 C 0.8080(2) 0.8736(5) 0.83548(13) 0.0453(10) Uani 1 1 d . . . H13 H 0.7710 0.8822 0.8251 0.054 Uiso 1 1 calc R . . O3 O 0.94468(11) 0.7217(3) 0.81238(7) 0.0355(6) Uani 1 1 d . . . C1 C 1.04473(17) 0.4816(4) 0.72047(11) 0.0388(9) Uani 1 1 d . . . N4 N 0.90346(13) 0.7931(4) 0.83203(8) 0.0347(7) Uani 1 1 d . . . C26 C 0.80894(18) 0.0993(5) 0.74393(14) 0.0481(11) Uani 1 1 d . . . H26 H 0.7980 -0.0004 0.7511 0.058 Uiso 1 1 calc R . . C23 C 0.7734(2) 0.3856(5) 0.66887(11) 0.0449(10) Uani 1 1 d . C . C18 C 0.9135(2) 1.1376(5) 0.64759(13) 0.0496(11) Uani 1 1 d . . . H18 H 0.9025 1.1873 0.6254 0.060 Uiso 1 1 calc R . . O10 O 0.98115(18) 0.9034(5) 0.91348(10) 0.0829(12) Uani 1 1 d . . . C5 C 1.11257(18) 0.5026(5) 0.77010(13) 0.0463(10) Uani 1 1 d . . . C12 C 0.8177(2) 0.9280(5) 0.87029(14) 0.0548(12) Uani 1 1 d . . . H12 H 0.7875 0.9726 0.8840 0.066 Uiso 1 1 calc R . . C3 C 1.1327(2) 0.3426(5) 0.71851(17) 0.0604(14) Uani 1 1 d . . . H3 H 1.1572 0.2724 0.7064 0.072 Uiso 1 1 calc R . . C14 C 0.85147(16) 0.8056(4) 0.81499(10) 0.0354(8) Uani 1 1 d . . . C2 C 1.0830(2) 0.3839(5) 0.70241(13) 0.0490(11) Uani 1 1 d . . . H2 H 1.0739 0.3462 0.6786 0.059 Uiso 1 1 calc R . . Sm2 Sm 0.792030(7) 0.133428(18) 0.990021(5) 0.02604(4) Uani 1 1 d . . . N16 N 0.65622(12) 0.0399(3) 0.99070(11) 0.0354(6) Uani 1 1 d . . . N9 N 0.87450(12) -0.1530(3) 1.01372(8) 0.0279(6) Uani 1 1 d . . . C53 C 0.56557(18) -0.0661(6) 0.99697(15) 0.0587(13) Uani 1 1 d . . . H53 H 0.5274 -0.0776 0.9887 0.070 Uiso 1 1 calc R . . O20 O 0.72848(12) -0.0143(3) 1.02991(7) 0.0391(6) Uani 1 1 d . . . O14 O 0.86002(11) -0.0121(3) 1.02467(7) 0.0346(6) Uani 1 1 d . . . O15 O 0.83047(12) 0.2495(3) 1.04312(7) 0.0392(6) Uani 1 1 d . . . C48 C 0.7378(2) 0.3389(5) 0.85758(12) 0.0479(11) Uani 1 1 d . . . C47 C 0.79773(19) 0.3407(5) 0.87281(11) 0.0395(10) Uani 1 1 d . . . O19 O 0.69477(11) 0.1281(3) 0.97365(8) 0.0423(7) Uani 1 1 d . . . O18 O 0.77126(10) 0.2119(3) 0.92808(7) 0.0337(6) Uani 1 1 d . . . C52 C 0.60207(17) 0.0285(5) 0.97805(12) 0.0421(10) Uani 1 1 d . . . O13 O 0.81819(11) -0.1078(3) 0.96419(7) 0.0337(6) Uani 1 1 d . . . N12 N 0.81409(13) 0.3889(3) 1.05439(8) 0.0314(7) Uani 1 1 d . . . C38 C 0.83154(17) 0.4450(4) 1.08820(10) 0.0350(8) Uani 1 1 d . . . N13 N 0.81114(13) 0.2804(3) 0.90699(8) 0.0310(7) Uani 1 1 d . . . C42 C 0.77869(16) 0.4666(4) 1.03090(10) 0.0314(8) Uani 1 1 d . . . C34 C 0.92831(17) -0.1924(5) 1.07289(11) 0.0401(9) Uani 1 1 d . . . C33 C 0.90853(15) -0.2426(4) 1.03553(10) 0.0321(8) Uani 1 1 d . . . C43 C 0.86510(16) 0.2840(4) 0.92184(10) 0.0309(8) Uani 1 1 d . . . C29 C 0.85212(15) -0.1991(4) 0.98053(9) 0.0303(8) Uani 1 1 d . . . O21 O 0.96845(16) -0.2576(5) 1.08723(10) 0.0748(12) Uani 1 1 d . . . C44 C 0.90846(18) 0.3508(4) 0.90004(11) 0.0391(9) Uani 1 1 d . . . H44 H 0.9465 0.3551 0.9090 0.047 Uiso 1 1 calc R . . C51 C 0.58080(17) 0.1149(6) 0.94553(14) 0.0503(11) Uani 1 1 d . . . C37 C 0.8691(2) 0.3549(5) 1.11386(10) 0.0398(10) Uani 1 1 d . . . O22 O 0.87729(16) 0.4056(4) 1.14500(8) 0.0607(9) Uani 1 1 d . . . C39 C 0.81294(19) 0.5868(5) 1.09880(11) 0.0425(10) Uani 1 1 d . . . H39 H 0.8236 0.6271 1.1221 0.051 Uiso 1 1 calc R . . O23 O 0.72926(17) 0.3964(6) 0.82716(11) 0.0876(14) Uani 1 1 d . . . C40 C 0.7785(2) 0.6707(5) 1.07512(12) 0.0465(10) Uani 1 1 d . . . H40 H 0.7664 0.7695 1.0822 0.056 Uiso 1 1 calc R . . C45 C 0.8955(2) 0.4093(5) 0.86591(12) 0.0463(10) Uani 1 1 d . . . H45 H 0.9248 0.4534 0.8514 0.056 Uiso 1 1 calc R . . C41 C 0.76193(17) 0.6128(5) 1.04184(12) 0.0413(9) Uani 1 1 d . . . H41 H 0.7388 0.6723 1.0259 0.050 Uiso 1 1 calc R . . O16 O 0.76431(11) 0.3977(3) 1.00116(7) 0.0379(6) Uani 1 1 d . . . O5 O 0.96356(12) 0.9131(3) 0.73940(7) 0.0415(7) Uani 1 1 d . . . C30 C 0.86910(17) -0.3435(4) 0.96724(11) 0.0375(9) Uani 1 1 d . . . H30 H 0.8564 -0.3782 0.9438 0.045 Uiso 1 1 calc R . . C27 C 0.84791(19) 0.1768(5) 0.76407(12) 0.0448(10) Uani 1 1 d . . . H27 H 0.8639 0.1299 0.7853 0.054 Uiso 1 1 calc R . . C15 C 0.94884(17) 0.9921(4) 0.71163(11) 0.0356(8) Uani 1 1 d . . . C31 C 0.90442(16) -0.4339(4) 0.98861(14) 0.0437(9) Uani 1 1 d . . . H31 H 0.9154 -0.5315 0.9799 0.052 Uiso 1 1 calc R . . O11 O 0.84736(16) 0.9718(4) 0.59804(9) 0.0682(10) Uani 1 1 d . . . C20 C 0.85275(19) 0.9187(5) 0.62874(11) 0.0439(10) Uani 1 1 d . C . C46 C 0.8403(2) 0.4049(6) 0.85234(12) 0.0487(11) Uani 1 1 d . . . H46 H 0.8321 0.4467 0.8288 0.058 Uiso 1 1 calc R . . O17 O 0.87138(11) 0.2257(3) 0.95379(6) 0.0325(6) Uani 1 1 d . . . C16 C 0.9670(2) 1.1397(5) 0.70323(13) 0.0514(12) Uani 1 1 d . . . H16 H 0.9922 1.1905 0.7196 0.062 Uiso 1 1 calc R . . C32 C 0.92388(17) -0.3840(5) 1.02242(13) 0.0399(10) Uani 1 1 d . . . H32 H 0.9480 -0.4474 1.0368 0.048 Uiso 1 1 calc R . . C56 C 0.67724(17) -0.0361(5) 1.02174(11) 0.0391(9) Uani 1 1 d . . . O9 O 1.17618(14) 0.5334(5) 0.82013(12) 0.0822(12) Uani 1 1 d . . . C11 C 0.8717(2) 0.9180(5) 0.88552(13) 0.0499(11) Uani 1 1 d . . . H11 H 0.8786 0.9593 0.9093 0.060 Uiso 1 1 calc R . . C6 C 1.13237(18) 0.5755(6) 0.80541(14) 0.0529(11) Uani 1 1 d . . . O24 O 0.53387(14) 0.0840(5) 0.93252(12) 0.0816(12) Uani 1 1 d . . . C17 C 0.9494(2) 1.2115(5) 0.67219(13) 0.0569(12) Uani 1 1 d . . . H17 H 0.9615 1.3125 0.6673 0.068 Uiso 1 1 calc R . . C55 C 0.6372(2) -0.1308(5) 1.03991(14) 0.0547(12) Uani 1 1 d . . . H55 H 0.6486 -0.1861 1.0612 0.066 Uiso 1 1 calc R . . C54 C 0.5835(2) -0.1439(6) 1.02759(15) 0.0580(13) Uani 1 1 d . . . H54 H 0.5575 -0.2082 1.0403 0.070 Uiso 1 1 calc R . . N14 N 0.69744(15) 0.2744(5) 0.87748(10) 0.0504(10) Uani 1 1 d . . . H14 H 0.7075 0.2333 0.8986 0.061 Uiso 1 1 calc R . . N11 N 0.89374(16) 0.2308(4) 1.10100(9) 0.0462(9) Uani 1 1 d . . . H11A H 0.8864 0.2044 1.0781 0.055 Uiso 1 1 calc R . . N3 N 1.01119(16) 0.7514(5) 0.86843(10) 0.0562(10) Uani 1 1 d . . . H3A H 1.0012 0.7050 0.8479 0.067 Uiso 1 1 calc R . . C62 C 0.98419(19) 0.1160(6) 0.99327(17) 0.0596(12) Uani 1 1 d . . . H18A H 0.9473 0.1325 0.9833 0.071 Uiso 1 1 calc R . . N10 N 0.89650(16) -0.0889(4) 1.08997(9) 0.0445(9) Uani 1 1 d . . . H10 H 0.8654 -0.0579 1.0787 0.053 Uiso 1 1 calc R . . N15 N 0.61331(15) 0.2266(5) 0.93257(11) 0.0553(10) Uani 1 1 d . . . H15 H 0.6448 0.2478 0.9447 0.066 Uiso 1 1 calc R . . N17 N 0.69374(17) 0.5387(5) 0.76859(10) 0.0516(10) Uani 1 1 d . . . H17A H 0.7046 0.4799 0.7869 0.062 Uiso 1 1 calc R . . N18 N 1.02072(19) 0.0250(5) 0.97686(10) 0.0602(11) Uani 1 1 d . . . H66 H 1.0103 -0.0215 0.9564 0.072 Uiso 1 1 calc R . . N2 N 1.10072(17) 0.6892(6) 0.81831(11) 0.0696(13) Uani 1 1 d . . . H2A H 1.0712 0.7173 0.8050 0.083 Uiso 1 1 calc R . . N6 N 0.8220(2) 0.8029(5) 0.64163(13) 0.0700(14) Uani 1 1 d . . . H6 H 0.8317 0.7715 0.6638 0.084 Uiso 1 1 calc R A 1 C61 C 0.7319(2) 0.6273(6) 0.75273(16) 0.0601(13) Uani 1 1 d . . . H61 H 0.7703 0.6286 0.7610 0.072 Uiso 1 1 calc R . . C57 C 0.6396(2) 0.5346(6) 0.75807(14) 0.0608(14) Uani 1 1 d . . . H57 H 0.6139 0.4687 0.7705 0.073 Uiso 1 1 calc R . . C60 C 0.7146(3) 0.7176(6) 0.72384(15) 0.0738(18) Uani 1 1 d . . . H60 H 0.7409 0.7815 0.7113 0.089 Uiso 1 1 calc R . . C65 C 1.0894(2) 0.0641(7) 1.02040(16) 0.0736(16) Uani 1 1 d . . . H64 H 1.1268 0.0444 1.0292 0.088 Uiso 1 1 calc R . . C66 C 1.0722(2) 0.0008(7) 0.98983(16) 0.0731(15) Uani 1 1 d . . . H65 H 1.0973 -0.0641 0.9767 0.088 Uiso 1 1 calc R . . C64 C 1.0544(3) 0.1578(7) 1.03965(15) 0.0707(15) Uani 1 1 d . . . H63 H 1.0666 0.2016 1.0623 0.085 Uiso 1 1 calc R . . C58 C 0.6206(2) 0.6203(8) 0.73064(15) 0.0700(16) Uani 1 1 d . . . H58 H 0.5818 0.6168 0.7232 0.084 Uiso 1 1 calc R . . C63 C 1.0015(3) 0.1881(7) 1.02597(15) 0.0699(16) Uani 1 1 d . . . H62 H 0.9767 0.2567 1.0384 0.084 Uiso 1 1 calc R . . C36 C 0.93224(19) 0.1347(5) 1.12223(12) 0.0461(11) Uani 1 1 d . . . H36A H 0.9380 0.1797 1.1470 0.055 Uiso 1 1 calc R . . H36B H 0.9697 0.1302 1.1097 0.055 Uiso 1 1 calc R . . C35 C 0.9091(2) -0.0222(5) 1.12627(11) 0.0459(10) Uani 1 1 d . . . H35A H 0.9373 -0.0865 1.1393 0.055 Uiso 1 1 calc R . . H35B H 0.8739 -0.0192 1.1413 0.055 Uiso 1 1 calc R . . C49 C 0.63810(19) 0.2660(6) 0.86727(13) 0.0561(12) Uani 1 1 d . . . H49A H 0.6284 0.1603 0.8603 0.067 Uiso 1 1 calc R . . H49B H 0.6309 0.3324 0.8457 0.067 Uiso 1 1 calc R . . C50 C 0.60084(19) 0.3165(7) 0.89978(13) 0.0585(13) Uani 1 1 d . . . H50A H 0.6079 0.4254 0.9051 0.070 Uiso 1 1 calc R . . H50B H 0.5602 0.3046 0.8932 0.070 Uiso 1 1 calc R . . N7 N 0.8044(2) 0.4860(5) 0.65103(11) 0.0732(14) Uani 1 1 d . . . H7 H 0.8360 0.5131 0.6623 0.088 Uiso 1 1 calc R B 1 C59 C 0.6582(3) 0.7130(7) 0.71356(14) 0.0752(19) Uani 1 1 d . . . H59 H 0.6454 0.7763 0.6940 0.090 Uiso 1 1 calc R . . C8 C 1.0694(2) 0.7266(8) 0.88150(14) 0.0695(16) Uani 1 1 d . . . H8A H 1.0747 0.6178 0.8876 0.083 Uiso 1 1 calc R . . H8B H 1.0760 0.7868 0.9042 0.083 Uiso 1 1 calc R . . C7 C 1.1109(2) 0.7718(9) 0.85294(15) 0.0828(19) Uani 1 1 d . . . H7A H 1.1078 0.8825 0.8484 0.099 Uiso 1 1 calc R . . H7B H 1.1499 0.7503 0.8618 0.099 Uiso 1 1 calc R . . C21A C 0.7739(3) 0.7180(8) 0.6245(2) 0.035(2) Uiso 0.531(11) 1 d P C 1 H21A H 0.7616 0.7686 0.6015 0.043 Uiso 0.531(11) 1 calc PR C 1 H21B H 0.7410 0.7144 0.6417 0.043 Uiso 0.531(11) 1 calc PR C 1 C22A C 0.7951(3) 0.5578(8) 0.6164(2) 0.035(2) Uiso 0.531(11) 1 d P C 1 H22A H 0.7664 0.5008 0.6019 0.042 Uiso 0.531(11) 1 calc PR C 1 H22B H 0.8310 0.5617 0.6021 0.042 Uiso 0.531(11) 1 calc PR C 1 C22B C 0.7639(5) 0.6019(11) 0.6252(3) 0.048(3) Uiso 0.469(11) 1 d P C 2 H22C H 0.7433 0.5429 0.6062 0.057 Uiso 0.469(11) 1 calc PR C 2 H22D H 0.7357 0.6552 0.6408 0.057 Uiso 0.469(11) 1 calc PR C 2 C21B C 0.8018(5) 0.7096(12) 0.6081(3) 0.053(3) Uiso 0.469(11) 1 d P C 2 H21C H 0.7816 0.7742 0.5900 0.064 Uiso 0.469(11) 1 calc PR C 2 H21D H 0.8341 0.6580 0.5958 0.064 Uiso 0.469(11) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02991(9) 0.02960(8) 0.02426(8) -0.00138(8) -0.00403(8) -0.00410(7) C4 0.036(2) 0.039(2) 0.086(4) 0.012(3) 0.009(3) 0.0030(17) O2 0.0343(15) 0.0589(19) 0.0390(16) -0.0187(13) -0.0054(12) 0.0097(13) N8 0.0304(16) 0.0265(15) 0.0306(16) 0.0008(12) -0.0015(13) -0.0048(12) O1 0.0460(17) 0.0457(17) 0.0387(16) -0.0126(13) 0.0038(13) -0.0040(13) C10 0.052(2) 0.035(2) 0.025(2) -0.0037(15) 0.0010(18) -0.0071(17) C25 0.033(2) 0.033(2) 0.054(3) -0.0069(19) 0.0035(18) -0.0084(17) O8 0.0349(14) 0.0383(15) 0.0384(15) 0.0083(12) -0.0069(12) -0.0072(12) C9 0.061(3) 0.059(3) 0.028(2) 0.0006(19) -0.004(2) -0.009(2) C28 0.0281(17) 0.0332(18) 0.037(2) 0.0048(16) 0.0042(16) 0.0008(14) N5 0.0350(16) 0.0261(15) 0.0335(16) 0.0037(13) 0.0036(13) -0.0033(13) O4 0.0324(14) 0.0450(16) 0.0360(14) -0.0021(12) -0.0047(11) 0.0032(12) C19 0.042(2) 0.039(2) 0.0276(18) -0.0008(16) 0.0041(16) 0.0054(17) O12 0.058(2) 0.072(2) 0.054(2) 0.0083(17) -0.0262(17) -0.0227(17) N1 0.0301(16) 0.0334(15) 0.046(2) -0.0012(15) 0.0065(15) -0.0013(12) O6 0.0570(18) 0.0280(14) 0.0379(15) 0.0041(11) -0.0177(13) -0.0119(13) O7 0.0413(15) 0.0289(14) 0.0317(13) 0.0051(11) -0.0075(11) -0.0137(12) C24 0.0309(19) 0.0308(19) 0.036(2) -0.0013(16) 0.0011(15) -0.0069(15) C13 0.044(2) 0.043(2) 0.049(3) -0.0055(19) 0.009(2) 0.0027(19) O3 0.0304(14) 0.0478(16) 0.0282(13) -0.0062(11) -0.0013(11) 0.0046(12) C1 0.040(2) 0.030(2) 0.047(2) -0.0010(17) 0.0163(19) -0.0093(17) N4 0.0352(17) 0.0393(18) 0.0298(16) -0.0020(13) 0.0055(14) 0.0002(14) C26 0.041(2) 0.0332(19) 0.070(3) 0.011(2) 0.004(2) -0.0109(17) C23 0.065(3) 0.036(2) 0.034(2) -0.0043(17) -0.013(2) -0.011(2) C18 0.062(3) 0.049(3) 0.038(2) 0.0122(19) 0.007(2) -0.002(2) O10 0.094(3) 0.108(3) 0.047(2) -0.040(2) -0.0197(19) 0.001(3) C5 0.034(2) 0.040(2) 0.065(3) 0.008(2) -0.001(2) -0.0061(18) C12 0.065(3) 0.043(3) 0.057(3) -0.005(2) 0.021(2) 0.001(2) C3 0.047(3) 0.040(3) 0.094(4) 0.002(3) 0.032(3) 0.002(2) C14 0.037(2) 0.0319(19) 0.037(2) 0.0003(16) 0.0036(16) -0.0018(16) C2 0.058(3) 0.037(2) 0.053(3) -0.0101(19) 0.026(2) -0.011(2) Sm2 0.02757(8) 0.02734(8) 0.02319(8) -0.00041(8) -0.00271(8) 0.00201(7) N16 0.0278(14) 0.0376(15) 0.0410(16) 0.0016(17) 0.0063(16) 0.0006(12) N9 0.0298(15) 0.0253(15) 0.0287(16) -0.0034(12) 0.0040(12) 0.0018(12) C53 0.037(2) 0.057(3) 0.083(4) -0.008(3) 0.012(2) -0.006(2) O20 0.0377(15) 0.0432(16) 0.0362(14) 0.0083(12) 0.0043(12) 0.0023(12) O14 0.0412(15) 0.0255(13) 0.0372(14) -0.0076(11) -0.0081(12) 0.0113(11) O15 0.0581(18) 0.0232(13) 0.0363(14) -0.0084(11) -0.0122(13) 0.0075(12) C48 0.054(3) 0.056(3) 0.033(2) 0.0114(19) -0.007(2) 0.007(2) C47 0.053(3) 0.042(2) 0.024(2) 0.0037(16) -0.0011(17) 0.0037(18) O19 0.0262(14) 0.0553(17) 0.0455(15) 0.0188(13) -0.0019(11) -0.0063(12) O18 0.0285(13) 0.0428(15) 0.0297(13) 0.0094(11) -0.0017(11) -0.0025(11) C52 0.030(2) 0.044(2) 0.053(3) -0.0075(18) 0.0022(17) -0.0012(17) O13 0.0392(14) 0.0329(14) 0.0291(13) -0.0072(11) -0.0030(11) 0.0036(11) N12 0.0394(17) 0.0268(16) 0.0281(16) -0.0034(12) 0.0034(13) 0.0021(13) C38 0.044(2) 0.032(2) 0.0288(18) -0.0027(15) 0.0052(16) -0.0071(17) N13 0.0336(16) 0.0330(17) 0.0263(16) 0.0015(13) 0.0005(13) 0.0008(13) C42 0.032(2) 0.0291(19) 0.033(2) -0.0007(15) 0.0017(16) -0.0005(15) C34 0.042(2) 0.038(2) 0.040(2) -0.0022(18) -0.0054(18) 0.0079(18) C33 0.0285(18) 0.0329(19) 0.0349(19) 0.0008(16) -0.0005(15) 0.0031(15) C43 0.032(2) 0.0283(18) 0.032(2) -0.0051(15) -0.0006(15) -0.0017(15) C29 0.0278(17) 0.0275(17) 0.036(2) 0.0018(14) 0.0020(14) -0.0005(14) O21 0.070(2) 0.092(3) 0.062(2) -0.023(2) -0.0311(18) 0.043(2) C44 0.036(2) 0.040(2) 0.042(2) -0.0029(17) 0.0090(18) -0.0044(17) C51 0.029(2) 0.059(3) 0.062(3) -0.009(2) -0.003(2) 0.008(2) C37 0.056(3) 0.040(2) 0.0240(19) -0.0005(16) 0.0006(17) -0.0070(19) O22 0.099(3) 0.0554(19) 0.0273(15) -0.0085(14) -0.0063(16) 0.0058(19) C39 0.055(2) 0.031(2) 0.042(2) -0.0102(17) 0.0105(19) -0.0044(19) O23 0.074(3) 0.130(4) 0.059(2) 0.053(2) -0.022(2) -0.010(2) C40 0.062(3) 0.032(2) 0.046(2) -0.0096(18) 0.013(2) 0.0072(19) C45 0.051(3) 0.052(3) 0.035(2) 0.0045(19) 0.0143(19) -0.005(2) C41 0.036(2) 0.036(2) 0.053(3) -0.0008(19) 0.0038(19) 0.0074(17) O16 0.0411(15) 0.0331(13) 0.0397(16) -0.0001(11) -0.0049(11) 0.0085(11) O5 0.0467(16) 0.0369(14) 0.0409(17) 0.0023(12) -0.0126(12) -0.0134(12) C30 0.040(2) 0.033(2) 0.040(2) -0.0073(16) 0.0009(17) 0.0010(16) C27 0.046(2) 0.038(2) 0.050(2) 0.0151(19) -0.0114(19) -0.0026(19) C15 0.037(2) 0.034(2) 0.036(2) -0.0028(17) 0.0035(17) -0.0084(16) C31 0.043(2) 0.0263(17) 0.061(2) -0.006(2) 0.003(2) 0.0038(15) O11 0.080(2) 0.090(3) 0.0344(17) 0.0082(17) -0.0112(16) 0.013(2) C20 0.054(3) 0.046(2) 0.032(2) -0.0038(18) -0.0076(19) 0.012(2) C46 0.060(3) 0.055(3) 0.031(2) 0.008(2) 0.006(2) -0.004(2) O17 0.0317(13) 0.0373(14) 0.0287(13) -0.0005(11) -0.0028(10) -0.0013(11) C16 0.068(3) 0.040(2) 0.047(3) 0.0058(19) -0.005(2) -0.017(2) C32 0.036(2) 0.030(2) 0.053(3) -0.0006(18) 0.0025(18) 0.0066(17) C56 0.041(2) 0.038(2) 0.038(2) 0.0028(17) 0.0083(18) 0.0019(17) O9 0.0392(19) 0.092(3) 0.115(3) 0.008(3) -0.032(2) 0.0012(19) C11 0.068(3) 0.043(2) 0.039(2) -0.008(2) 0.012(2) -0.002(2) C6 0.032(2) 0.063(3) 0.063(3) 0.007(2) -0.005(2) 0.000(2) O24 0.042(2) 0.087(3) 0.116(3) 0.014(2) -0.033(2) -0.0161(19) C17 0.079(3) 0.041(2) 0.051(3) 0.010(2) 0.003(2) -0.015(2) C55 0.051(3) 0.049(3) 0.064(3) 0.011(2) 0.024(2) 0.003(2) C54 0.042(3) 0.057(3) 0.075(3) 0.010(2) 0.021(2) -0.004(2) N14 0.041(2) 0.074(3) 0.0361(19) 0.0144(19) -0.0112(16) 0.0075(19) N11 0.068(2) 0.039(2) 0.0322(17) -0.0075(15) -0.0179(17) 0.0044(17) N3 0.049(2) 0.085(3) 0.0349(19) -0.0148(19) -0.0137(17) 0.002(2) C62 0.039(2) 0.080(3) 0.059(3) 0.024(3) -0.007(2) -0.002(2) N10 0.050(2) 0.047(2) 0.0367(19) -0.0073(16) -0.0094(16) 0.0140(18) N15 0.037(2) 0.076(3) 0.053(2) 0.008(2) -0.0116(17) -0.0022(19) N17 0.055(2) 0.067(3) 0.0328(18) 0.0065(18) -0.0073(17) 0.013(2) N18 0.081(3) 0.061(3) 0.039(2) -0.0056(17) -0.004(2) -0.004(2) N2 0.043(2) 0.113(4) 0.054(2) -0.022(2) -0.0180(19) 0.005(2) N6 0.094(3) 0.044(2) 0.072(3) 0.010(2) -0.057(3) -0.009(2) C61 0.039(2) 0.085(4) 0.056(3) -0.019(3) 0.001(3) -0.004(2) C57 0.049(3) 0.072(3) 0.062(3) 0.001(3) 0.005(2) -0.007(2) C60 0.111(5) 0.050(3) 0.060(3) -0.012(3) 0.039(3) -0.027(3) C65 0.057(3) 0.094(4) 0.070(4) 0.000(3) -0.011(3) 0.015(3) C66 0.076(4) 0.086(4) 0.057(3) -0.002(3) 0.014(4) 0.034(3) C64 0.079(4) 0.083(4) 0.050(3) -0.016(3) -0.021(3) 0.007(3) C58 0.054(3) 0.099(4) 0.057(3) -0.014(3) -0.020(3) 0.024(3) C63 0.079(4) 0.073(4) 0.057(3) -0.002(3) 0.024(3) 0.028(3) C36 0.052(3) 0.057(3) 0.029(2) -0.0015(18) -0.0177(19) 0.002(2) C35 0.059(3) 0.052(3) 0.0264(19) -0.0002(18) -0.0078(18) 0.005(2) C49 0.043(3) 0.076(3) 0.050(3) 0.008(2) -0.019(2) 0.007(2) C50 0.037(2) 0.079(4) 0.059(3) 0.009(3) -0.015(2) 0.007(2) N7 0.109(4) 0.062(3) 0.048(2) 0.018(2) -0.037(2) -0.047(3) C59 0.122(5) 0.065(4) 0.038(3) 0.000(2) -0.013(3) 0.037(4) C8 0.056(3) 0.105(5) 0.048(3) -0.010(3) -0.022(2) 0.004(3) C7 0.055(3) 0.124(6) 0.069(4) -0.027(4) -0.027(3) -0.021(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 Sm1 O6 2.386(3) . ? Sm1 O7 2.389(2) . ? Sm1 O2 2.385(3) . ? Sm1 O3 2.395(3) . ? Sm1 O8 2.417(3) . ? Sm1 O4 2.422(3) . ? Sm1 O1 2.434(3) . ? Sm1 O5 2.439(3) . ? C4 C5 1.377(6) . ? C4 C3 1.386(8) . ? C4 H4 0.9500 . ? O2 N1 1.340(4) . ? N8 O7 1.344(4) . ? N8 C24 1.375(5) . ? N8 C28 1.393(5) . ? O1 C1 1.285(5) . ? C10 N4 1.371(5) . ? C10 C11 1.374(6) . ? C10 C9 1.497(6) . ? C25 C24 1.382(5) . ? C25 C26 1.401(6) . ? C25 H25 0.9500 . ? O8 C28 1.255(4) . ? C9 O10 1.223(5) . ? C9 N3 1.312(6) . ? C28 C27 1.412(5) . ? N5 O6 1.347(4) . ? N5 C19 1.377(5) . ? N5 C15 1.378(5) . ? O4 C14 1.268(4) . ? C19 C18 1.370(6) . ? C19 C20 1.504(6) . ? O12 C23 1.224(5) . ? N1 C5 1.362(5) . ? N1 C1 1.372(5) . ? C24 C23 1.509(6) . ? C13 C12 1.369(7) . ? C13 C14 1.397(6) . ? C13 H13 0.9500 . ? O3 N4 1.356(4) . ? C1 C2 1.406(6) . ? N4 C14 1.372(5) . ? C26 C27 1.354(6) . ? C26 H26 0.9500 . ? C23 N7 1.315(6) . ? C18 C17 1.387(7) . ? C18 H18 0.9500 . ? C5 C6 1.505(7) . ? C12 C11 1.385(7) . ? C12 H12 0.9500 . ? C3 C2 1.353(7) . ? C3 H3 0.9500 . ? C2 H2 0.9500 . ? Sm2 O19 2.359(3) . ? Sm2 O15 2.358(3) . ? Sm2 O18 2.399(2) . ? Sm2 O13 2.398(3) . ? Sm2 O14 2.400(2) . ? Sm2 O17 2.419(3) . ? Sm2 O16 2.447(3) . ? Sm2 O20 2.450(3) . ? N16 O19 1.342(4) . ? N16 C52 1.355(5) . ? N16 C56 1.399(5) . ? N9 O14 1.345(4) . ? N9 C33 1.372(5) . ? N9 C29 1.374(5) . ? C53 C52 1.377(6) . ? C53 C54 1.370(7) . ? C53 H53 0.9500 . ? O20 C56 1.253(5) . ? O15 N12 1.348(4) . ? C48 O23 1.229(5) . ? C48 N14 1.319(6) . ? C48 C47 1.511(6) . ? C47 C46 1.367(6) . ? C47 N13 1.384(5) . ? O18 N13 1.350(4) . ? C52 C51 1.489(6) . ? O13 C29 1.277(4) . ? N12 C42 1.371(5) . ? N12 C38 1.383(5) . ? C38 C39 1.376(5) . ? C38 C37 1.507(6) . ? N13 C43 1.377(5) . ? C42 O16 1.282(4) . ? C42 C41 1.402(5) . ? C34 O21 1.220(5) . ? C34 N10 1.330(5) . ? C34 C33 1.498(5) . ? C33 C32 1.379(5) . ? C43 O17 1.275(4) . ? C43 C44 1.416(5) . ? C29 C30 1.415(5) . ? C44 C45 1.374(6) . ? C44 H44 0.9500 . ? C51 O24 1.229(5) . ? C51 N15 1.329(6) . ? C37 O22 1.228(5) . ? C37 N11 1.320(5) . ? C39 C40 1.391(6) . ? C39 H39 0.9500 . ? C40 C41 1.366(6) . ? C40 H40 0.9500 . ? C45 C46 1.386(6) . ? C45 H45 0.9500 . ? C41 H41 0.9500 . ? O5 C15 1.271(5) . ? C30 C31 1.386(6) . ? C30 H30 0.9500 . ? C27 H27 0.9500 . ? C15 C16 1.400(6) . ? C31 C32 1.380(7) . ? C31 H31 0.9500 . ? O11 C20 1.213(5) . ? C20 N6 1.334(6) . ? C46 H46 0.9500 . ? C16 C17 1.355(6) . ? C16 H16 0.9500 . ? C32 H32 0.9500 . ? C56 C55 1.419(6) . ? O9 C6 1.216(5) . ? C11 H11 0.9500 . ? C6 N2 1.330(6) . ? C17 H17 0.9500 . ? C55 C54 1.342(7) . ? C55 H55 0.9500 . ? C54 H54 0.9500 . ? N14 C49 1.443(5) . ? N14 H14 0.8800 . ? N11 C36 1.457(5) . ? N11 H11A 0.8800 . ? N3 C8 1.462(6) . ? N3 H3A 0.8800 . ? C62 N18 1.316(6) . ? C62 C63 1.404(8) . ? C62 H18A 0.9500 . ? N10 C35 1.471(5) . ? N10 H10 0.8800 . ? N15 C50 1.457(6) . ? N15 H15 0.8800 . ? N17 C57 1.328(6) . ? N17 C61 1.319(6) . ? N17 H17A 0.8800 . ? N18 C66 1.313(6) . ? N18 H66 0.8800 . ? N2 C7 1.469(6) . ? N2 H2A 0.8800 . ? N6 C21A 1.488(8) . ? N6 C21B 1.539(11) . ? N6 H6 0.8800 . ? C61 C60 1.376(8) . ? C61 H61 0.9500 . ? C57 C58 1.325(7) . ? C57 H57 0.9500 . ? C60 C59 1.376(9) . ? C60 H60 0.9500 . ? C65 C66 1.304(8) . ? C65 C64 1.357(8) . ? C65 H64 0.9500 . ? C66 H65 0.9500 . ? C64 C63 1.365(8) . ? C64 H63 0.9500 . ? C58 C59 1.351(9) . ? C58 H58 0.9500 . ? C63 H62 0.9500 . ? C36 C35 1.489(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C49 C50 1.533(7) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C22A 1.422(8) . ? N7 C22B 1.679(10) . ? N7 H7 0.8800 . ? C59 H59 0.9500 . ? C8 C7 1.476(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C21A C22A 1.524(11) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C22B C21B 1.440(16) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C21B H21C 0.9900 . ? C21B H21D 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 O6 Sm1 O7 63.45(9) . . ? O6 Sm1 O2 129.35(10) . . ? O7 Sm1 O2 141.89(10) . . ? O6 Sm1 O3 135.60(10) . . ? O7 Sm1 O3 137.60(9) . . ? O2 Sm1 O3 63.82(9) . . ? O6 Sm1 O8 127.50(9) . . ? O7 Sm1 O8 64.09(8) . . ? O2 Sm1 O8 92.48(10) . . ? O3 Sm1 O8 87.29(9) . . ? O6 Sm1 O4 88.30(10) . . ? O7 Sm1 O4 83.38(10) . . ? O2 Sm1 O4 127.56(9) . . ? O3 Sm1 O4 63.81(9) . . ? O8 Sm1 O4 87.64(10) . . ? O6 Sm1 O1 87.18(10) . . ? O7 Sm1 O1 84.54(10) . . ? O2 Sm1 O1 63.21(9) . . ? O3 Sm1 O1 126.21(9) . . ? O8 Sm1 O1 86.20(10) . . ? O4 Sm1 O1 167.88(9) . . ? O6 Sm1 O5 63.40(9) . . ? O7 Sm1 O5 126.59(9) . . ? O2 Sm1 O5 80.13(10) . . ? O3 Sm1 O5 81.86(9) . . ? O8 Sm1 O5 168.76(9) . . ? O4 Sm1 O5 90.18(10) . . ? O1 Sm1 O5 97.83(10) . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 O2 Sm1 121.6(2) . . ? O7 N8 C24 120.7(3) . . ? O7 N8 C28 115.4(3) . . ? C24 N8 C28 124.0(3) . . ? C1 O1 Sm1 121.2(2) . . ? N4 C10 C11 117.7(4) . . ? N4 C10 C9 123.3(4) . . ? C11 C10 C9 118.9(4) . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C28 O8 Sm1 122.2(2) . . ? O10 C9 N3 122.7(5) . . ? O10 C9 C10 119.1(5) . . ? N3 C9 C10 118.2(4) . . ? O8 C28 N8 117.5(3) . . ? O8 C28 C27 126.9(4) . . ? N8 C28 C27 115.6(3) . . ? O6 N5 C19 120.7(3) . . ? O6 N5 C15 115.5(3) . . ? C19 N5 C15 123.8(3) . . ? C14 O4 Sm1 122.1(2) . . ? C18 C19 N5 117.5(4) . . ? C18 C19 C20 120.1(4) . . ? N5 C19 C20 122.4(4) . . ? O2 N1 C5 121.0(3) . . ? O2 N1 C1 115.4(3) . . ? C5 N1 C1 123.5(3) . . ? N5 O6 Sm1 121.9(2) . . ? N8 O7 Sm1 120.86(19) . . ? N8 C24 C25 118.2(4) . . ? N8 C24 C23 121.2(3) . . ? C25 C24 C23 120.6(4) . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? N4 O3 Sm1 120.3(2) . . ? O1 C1 N1 116.7(3) . . ? O1 C1 C2 126.8(4) . . ? N1 C1 C2 116.5(4) . . ? O3 N4 C10 120.1(3) . . ? O3 N4 C14 115.8(3) . . ? C10 N4 C14 124.1(3) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? O12 C23 N7 124.9(4) . . ? O12 C23 C24 118.2(4) . . ? N7 C23 C24 116.9(4) . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? N1 C5 C4 118.7(4) . . ? N1 C5 C6 122.5(4) . . ? C4 C5 C6 118.8(4) . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? O4 C14 N4 117.3(3) . . ? O4 C14 C13 126.3(4) . . ? N4 C14 C13 116.4(4) . . ? C3 C2 C1 120.9(5) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? O19 Sm2 O15 125.74(10) . . ? O19 Sm2 O18 64.76(9) . . ? O15 Sm2 O18 135.81(9) . . ? O19 Sm2 O13 97.59(10) . . ? O15 Sm2 O13 127.13(9) . . ? O18 Sm2 O13 86.63(9) . . ? O19 Sm2 O14 139.86(9) . . ? O15 Sm2 O14 63.22(8) . . ? O18 Sm2 O14 141.10(9) . . ? O13 Sm2 O14 64.06(8) . . ? O19 Sm2 O17 127.96(9) . . ? O15 Sm2 O17 90.19(9) . . ? O18 Sm2 O17 63.38(8) . . ? O13 Sm2 O17 83.55(9) . . ? O14 Sm2 O17 87.19(9) . . ? O19 Sm2 O16 78.64(10) . . ? O15 Sm2 O16 63.63(8) . . ? O18 Sm2 O16 80.04(9) . . ? O13 Sm2 O16 166.51(8) . . ? O14 Sm2 O16 126.64(8) . . ? O17 Sm2 O16 88.60(9) . . ? O19 Sm2 O20 63.18(9) . . ? O15 Sm2 O20 88.91(10) . . ? O18 Sm2 O20 125.52(9) . . ? O13 Sm2 O20 85.25(9) . . ? O14 Sm2 O20 79.24(10) . . ? O17 Sm2 O20 165.23(9) . . ? O16 Sm2 O20 104.15(9) . . ? O19 N16 C52 121.3(3) . . ? O19 N16 C56 114.1(3) . . ? C52 N16 C56 124.6(3) . . ? O14 N9 C33 120.4(3) . . ? O14 N9 C29 115.7(3) . . ? C33 N9 C29 123.9(3) . . ? C52 C53 C54 120.9(4) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C56 O20 Sm2 121.7(2) . . ? N9 O14 Sm2 120.3(2) . . ? N12 O15 Sm2 122.1(2) . . ? O23 C48 N14 123.3(5) . . ? O23 C48 C47 118.4(4) . . ? N14 C48 C47 118.2(4) . . ? C46 C47 N13 118.5(4) . . ? C46 C47 C48 119.1(4) . . ? N13 C47 C48 122.3(4) . . ? N16 O19 Sm2 123.2(2) . . ? N13 O18 Sm2 121.15(19) . . ? N16 C52 C53 117.4(4) . . ? N16 C52 C51 123.0(4) . . ? C53 C52 C51 119.6(4) . . ? C29 O13 Sm2 122.3(2) . . ? O15 N12 C42 115.9(3) . . ? O15 N12 C38 120.5(3) . . ? C42 N12 C38 123.5(3) . . ? C39 C38 N12 118.4(4) . . ? C39 C38 C37 119.4(3) . . ? N12 C38 C37 122.2(3) . . ? O18 N13 C43 115.3(3) . . ? O18 N13 C47 121.3(3) . . ? C43 N13 C47 123.4(3) . . ? O16 C42 N12 116.5(3) . . ? O16 C42 C41 126.7(4) . . ? N12 C42 C41 116.8(3) . . ? O21 C34 N10 123.9(4) . . ? O21 C34 C33 119.1(4) . . ? N10 C34 C33 116.6(3) . . ? N9 C33 C32 118.1(4) . . ? N9 C33 C34 122.1(3) . . ? C32 C33 C34 119.7(4) . . ? O17 C43 N13 116.9(3) . . ? O17 C43 C44 126.2(4) . . ? N13 C43 C44 116.9(3) . . ? O13 C29 N9 117.3(3) . . ? O13 C29 C30 125.6(3) . . ? N9 C29 C30 117.1(3) . . ? C45 C44 C43 119.9(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? O24 C51 N15 122.9(5) . . ? O24 C51 C52 119.4(5) . . ? N15 C51 C52 117.7(4) . . ? O22 C37 N11 123.8(4) . . ? O22 C37 C38 117.9(4) . . ? N11 C37 C38 118.2(3) . . ? C38 C39 C40 119.5(4) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? C41 C40 C39 120.9(4) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C44 C45 C46 121.1(4) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C40 C41 C42 120.7(4) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C42 O16 Sm2 121.2(2) . . ? C15 O5 Sm1 122.2(2) . . ? C31 C30 C29 119.5(4) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C26 C27 C28 122.0(4) . . ? C26 C27 H27 119.0 . . ? C28 C27 H27 119.0 . . ? O5 C15 N5 117.0(3) . . ? O5 C15 C16 126.6(4) . . ? N5 C15 C16 116.4(4) . . ? C30 C31 C32 120.8(4) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? O11 C20 N6 124.0(4) . . ? O11 C20 C19 118.3(4) . . ? N6 C20 C19 117.6(4) . . ? C47 C46 C45 120.1(4) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C43 O17 Sm2 122.6(2) . . ? C17 C16 C15 121.3(4) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? O20 C56 N16 117.1(3) . . ? O20 C56 C55 128.0(4) . . ? N16 C56 C55 114.8(4) . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? O9 C6 N2 123.1(5) . . ? O9 C6 C5 120.3(5) . . ? N2 C6 C5 116.5(4) . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C54 C55 C56 121.2(5) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C55 C54 C53 121.0(4) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C48 N14 C49 125.1(4) . . ? C48 N14 H14 117.4 . . ? C49 N14 H14 117.4 . . ? C37 N11 C36 124.4(3) . . ? C37 N11 H11A 117.8 . . ? C36 N11 H11A 117.8 . . ? C9 N3 C8 126.1(4) . . ? C9 N3 H3A 117.0 . . ? C8 N3 H3A 117.0 . . ? N18 C62 C63 117.9(5) . . ? N18 C62 H18A 121.0 . . ? C63 C62 H18A 121.0 . . ? C34 N10 C35 125.2(4) . . ? C34 N10 H10 117.4 . . ? C35 N10 H10 117.4 . . ? C51 N15 C50 125.0(4) . . ? C51 N15 H15 117.5 . . ? C50 N15 H15 117.5 . . ? C57 N17 C61 122.8(4) . . ? C57 N17 H17A 118.6 . . ? C61 N17 H17A 118.6 . . ? C66 N18 C62 122.4(5) . . ? C66 N18 H66 118.8 . . ? C62 N18 H66 118.8 . . ? C6 N2 C7 125.5(5) . . ? C6 N2 H2A 117.2 . . ? C7 N2 H2A 117.2 . . ? C20 N6 C21A 130.4(5) . . ? C20 N6 C21B 107.3(6) . . ? C20 N6 H6 114.8 . . ? C21A N6 H6 114.8 . . ? C21B N6 H6 129.3 . . ? N17 C61 C60 118.2(5) . . ? N17 C61 H61 120.9 . . ? C60 C61 H61 120.9 . . ? N17 C57 C58 121.5(5) . . ? N17 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C59 C60 C61 118.2(5) . . ? C59 C60 H60 120.9 . . ? C61 C60 H60 120.9 . . ? C66 C65 C64 120.5(5) . . ? C66 C65 H64 119.7 . . ? C64 C65 H64 119.7 . . ? C65 C66 N18 121.4(5) . . ? C65 C66 H65 119.3 . . ? N18 C66 H65 119.3 . . ? C63 C64 C65 118.9(5) . . ? C63 C64 H63 120.6 . . ? C65 C64 H63 120.6 . . ? C57 C58 C59 117.8(5) . . ? C57 C58 H58 121.1 . . ? C59 C58 H58 121.1 . . ? C64 C63 C62 118.8(5) . . ? C64 C63 H62 120.6 . . ? C62 C63 H62 120.6 . . ? N11 C36 C35 111.3(4) . . ? N11 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? N11 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? N10 C35 C36 110.8(4) . . ? N10 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? N10 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? N14 C49 C50 109.8(4) . . ? N14 C49 H49A 109.7 . . ? C50 C49 H49A 109.7 . . ? N14 C49 H49B 109.7 . . ? C50 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? N15 C50 C49 110.8(4) . . ? N15 C50 H50A 109.5 . . ? C49 C50 H50A 109.5 . . ? N15 C50 H50B 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? C23 N7 C22A 130.3(5) . . ? C23 N7 C22B 111.5(5) . . ? C23 N7 H7 114.9 . . ? C22A N7 H7 114.9 . . ? C22B N7 H7 124.9 . . ? C58 C59 C60 121.5(5) . . ? C58 C59 H59 119.3 . . ? C60 C59 H59 119.3 . . ? N3 C8 C7 110.4(4) . . ? N3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? N2 C7 C8 111.0(5) . . ? N2 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N6 C21A C22A 107.2(6) . . ? N6 C21A H21A 110.3 . . ? C22A C21A H21A 110.3 . . ? N6 C21A H21B 110.3 . . ? C22A C21A H21B 110.3 . . ? H21A C21A H21B 108.5 . . ? N7 C22A C21A 106.8(6) . . ? N7 C22A H22A 110.4 . . ? C21A C22A H22A 110.4 . . ? N7 C22A H22B 110.4 . . ? C21A C22A H22B 110.4 . . ? H22A C22A H22B 108.6 . . ? C21B C22B N7 106.8(8) . . ? C21B C22B H22C 110.4 . . ? N7 C22B H22C 110.4 . . ? C21B C22B H22D 110.4 . . ? N7 C22B H22D 110.4 . . ? H22C C22B H22D 108.6 . . ? C22B C21B N6 101.6(9) . . ? C22B C21B H21C 111.4 . . ? N6 C21B H21C 111.4 . . ? C22B C21B H21D 111.4 . . ? N6 C21B H21D 111.4 . . ? H21C C21B H21D 109.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.782 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.054 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 0.537 0.070 0.115 45 17 ' ' 2 0.993 -0.195 0.317 66 20 ' ' 3 0.790 0.197 0.428 68 18 ' ' 4 0.463 -0.070 0.615 45 17 ' ' 5 0.007 0.195 0.817 66 19 ' ' 6 0.210 -0.197 0.928 68 18 ' ' 7 0.290 0.303 0.428 68 18 ' ' 8 0.507 0.305 0.817 66 20 ' ' 9 0.037 0.430 0.115 45 17 ' ' 10 0.963 0.570 0.615 45 17 ' ' 11 0.493 0.695 0.317 66 19 ' ' 12 0.710 0.697 0.928 68 18 ' ' _platon_squeeze_details ; ;