# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Mazzanti, M.' _publ_contact_author_email marinella.mazzanti@cea.fr _publ_section_title ; New insights into the acid mediated disproportionation of pentavalent uranyl. ; _publ_author_name 'Mazzanti, M.' # Attachment '- ciffinal.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 776755' #TrackingRef '- ciffinal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H85 N5 O32 U6' _chemical_formula_weight 3332.94 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 27.493(3) _cell_length_b 16.418(18) _cell_length_c 28.809(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13004(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2058 _cell_measurement_theta_min 3.2913 _cell_measurement_theta_max 28.9290 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6184 _exptl_absorpt_coefficient_mu 7.511 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4027 _exptl_absorpt_correction_T_max 0.7790 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16195 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.2152 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6878 _reflns_number_gt 2368 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 43.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 17.1550 -77.0000 -60.0000 92 #__ type_ start__ end____ width___ exp.time_ 2 omega -74.00 -35.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -18.7175 179.0000 90.0000 39 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6878 _refine_ls_number_parameters 407 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1822 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2245 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 0.758 _refine_ls_restrained_S_all 0.753 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.5000 1.05979(12) 0.7500 0.0459(5) Uani 1 4 d S . . U2 U 0.56970(2) 0.89288(6) 0.68322(3) 0.0497(3) Uani 1 1 d . . . U3 U 0.5000 0.72894(13) 0.7500 0.0521(5) Uani 1 4 d S . . O1U O 0.5763(6) 0.9823(13) 0.7500 0.047(5) Uani 1 2 d S . . H1U H 0.6062 1.0171 0.7500 0.057 Uiso 1 2 calc SR . . O2U O 0.5000 0.9642(14) 0.6951(7) 0.052(5) Uani 1 2 d S . . O3U O 0.5000 0.8002(14) 0.6765(7) 0.054(6) Uani 1 2 d S . . H3U H 0.5000 0.7645 0.6483 0.065 Uiso 1 2 calc SR . . O4U O 0.5592(6) 0.8235(15) 0.7500 0.054(6) Uani 1 2 d S . . O1 O 0.5548(5) 1.1226(9) 0.6922(5) 0.052(4) Uani 1 1 d . . . O2 O 0.5986(5) 1.0252(11) 0.6566(6) 0.054(4) Uani 1 1 d . . . C1 C 0.5867(7) 1.097(2) 0.6635(6) 0.058(8) Uani 1 1 d . . . C2 C 0.6126(8) 1.1656(16) 0.6367(8) 0.060(6) Uani 1 1 d . . . C3 C 0.6541(9) 1.153(2) 0.6125(9) 0.079(9) Uani 1 1 d . . . H3 H 0.6681 1.1004 0.6150 0.094 Uiso 1 1 calc R . . C4 C 0.6767(12) 1.204(2) 0.5866(9) 0.089(10) Uani 1 1 d . . . H4 H 0.7053 1.1903 0.5696 0.107 Uiso 1 1 calc R . . C5 C 0.6548(13) 1.281(3) 0.5859(13) 0.114(14) Uani 1 1 d . . . H5 H 0.6706 1.3237 0.5696 0.136 Uiso 1 1 calc R . . C6 C 0.6123(11) 1.297(2) 0.6074(13) 0.111(13) Uani 1 1 d . . . H6 H 0.5959 1.3476 0.6034 0.133 Uiso 1 1 calc R . . C7 C 0.5952(10) 1.2413(17) 0.6332(10) 0.072(7) Uani 1 1 d . . . H7 H 0.5677 1.2545 0.6516 0.086 Uiso 1 1 calc R . . N1 N 0.5000 1.239(4) 0.7500 0.10(2) Uani 1 4 d S . . C11 C 0.4607(16) 1.280(3) 0.7500 0.097(15) Uani 1 2 d S . . H11 H 0.4311 1.2505 0.7500 0.116 Uiso 1 2 calc SR . . C12 C 0.4571(19) 1.362(4) 0.7500 0.110(18) Uani 1 2 d S . . H12 H 0.4269 1.3900 0.7500 0.132 Uiso 1 2 calc SR . . C13 C 0.5000 1.399(5) 0.7500 0.11(2) Uani 1 4 d S . . H13 H 0.5000 1.4565 0.7500 0.127 Uiso 1 4 calc SR . . O21 O 0.5397(5) 0.8993(13) 0.6042(5) 0.065(4) Uani 1 1 d . . . C21 C 0.5000 0.901(2) 0.5835(9) 0.051(8) Uani 1 2 d S . . C22 C 0.5000 0.896(3) 0.5320(11) 0.078(11) Uani 1 2 d S . . C23 C 0.4611(10) 0.898(3) 0.5077(9) 0.114(13) Uani 1 1 d . . . H23 H 0.4317 0.9089 0.5238 0.137 Uiso 1 1 calc R . . C24 C 0.4577(11) 0.885(3) 0.4601(9) 0.15(2) Uani 1 1 d . . . H24 H 0.4275 0.8778 0.4447 0.186 Uiso 1 1 calc R . . C25 C 0.5000 0.885(4) 0.4380(11) 0.13(2) Uani 1 2 d S . . H25 H 0.5000 0.8838 0.4051 0.153 Uiso 1 2 calc SR . . O31 O 0.6522(4) 0.8811(12) 0.7120(5) 0.064(5) Uani 1 1 d . . . C31 C 0.6706(12) 0.866(2) 0.7500 0.053(8) Uani 1 2 d S . . C32 C 0.7245(10) 0.835(2) 0.7500 0.051(8) Uani 1 2 d S . . C33 C 0.7483(9) 0.821(2) 0.7095(10) 0.096(11) Uani 1 1 d . . . H33 H 0.7333 0.8354 0.6809 0.115 Uiso 1 1 calc R . . C34 C 0.7932(10) 0.787(2) 0.7091(11) 0.105(13) Uani 1 1 d . . . H34 H 0.8086 0.7735 0.6806 0.126 Uiso 1 1 calc R . . C35 C 0.8157(6) 0.7726(11) 0.7500 0.085(13) Uani 1 2 d S . . H35 H 0.8480 0.7520 0.7500 0.102 Uiso 1 2 calc SR . . N2 N 0.6409(6) 0.8779(11) 0.6116 0.035(8) Uani 0.50 1 d PR . . C41 C 0.6358(6) 0.8169(11) 0.5785 0.075(14) Uani 0.50 1 d PRU . . H41 H 0.6068 0.7855 0.5773 0.090 Uiso 0.50 1 calc PR . . C42 C 0.6732(6) 0.8019(11) 0.5471 0.086(17) Uani 0.50 1 d PRU . . H42 H 0.6697 0.7603 0.5245 0.103 Uiso 0.50 1 calc PR . . C43 C 0.7156(6) 0.8479(11) 0.5489 0.058(12) Uani 0.50 1 d PRU . . H43 H 0.7411 0.8377 0.5274 0.069 Uiso 0.50 1 calc PR . . C44 C 0.7207(6) 0.9089(11) 0.5820 0.098(19) Uani 0.50 1 d PRU . . H44 H 0.7497 0.9403 0.5832 0.118 Uiso 0.50 1 calc PR . . C45 C 0.6833(6) 0.9239(11) 0.6134 0.057(12) Uani 0.50 1 d PRU . . H45 H 0.6868 0.9655 0.6360 0.068 Uiso 0.50 1 calc PR . . O51 O 0.6005(6) 0.7563(14) 0.6631(6) 0.079(6) Uani 1 1 d . A . O52 O 0.5573(6) 0.6608(12) 0.7001(5) 0.069(5) Uani 1 1 d . A . C51 C 0.5922(6) 0.6857(14) 0.6772(7) 0.086(10) Uani 1 1 d . . . C52 C 0.6329(6) 0.6152(14) 0.6711(7) 0.074(15) Uani 0.50 1 d PRU A 1 C53 C 0.6788(6) 0.6347(14) 0.6542(7) 0.068(14) Uani 0.50 1 d PRU A 1 H53 H 0.6843 0.6860 0.6399 0.082 Uiso 0.50 1 calc PR A 1 C54 C 0.7167(6) 0.5791(14) 0.6583(7) 0.064(13) Uani 0.50 1 d PRU A 1 H54 H 0.7481 0.5924 0.6467 0.077 Uiso 0.50 1 calc PR A 1 C55 C 0.7087(6) 0.5040(14) 0.6792(7) 0.095(18) Uani 0.50 1 d PRU A 1 H55 H 0.7346 0.4660 0.6819 0.114 Uiso 0.50 1 calc PR A 1 C56 C 0.6628(6) 0.4845(14) 0.6961(7) 0.092(18) Uani 0.50 1 d PRU A 1 H56 H 0.6573 0.4332 0.7104 0.110 Uiso 0.50 1 calc PR A 1 C57 C 0.6249(6) 0.5401(14) 0.6920(7) 0.092(18) Uani 0.50 1 d PRU A 1 H57 H 0.5935 0.5268 0.7036 0.110 Uiso 0.50 1 calc PR A 1 N3 N 0.8259(12) 0.568(2) 0.7500 0.083(10) Uani 1 2 d S . 2 C61 C 0.7903(15) 0.581(3) 0.7341(14) 0.060(14) Uani 0.50 1 d P . 2 C62 C 0.7363(9) 0.596(2) 0.7161(11) 0.16(4) Uani 0.50 1 d P . 2 H62A H 0.7373 0.6199 0.6849 0.236 Uiso 0.50 1 calc PR . 2 H62B H 0.7195 0.6336 0.7372 0.236 Uiso 0.50 1 calc PR . 2 H62C H 0.7187 0.5442 0.7151 0.236 Uiso 0.50 1 calc PR . 2 C52B C 0.6292(9) 0.618(2) 0.6523(11) 0.11(2) Uani 0.50 1 d PRU . 2 C53B C 0.6506(9) 0.639(2) 0.6104(11) 0.11(2) Uani 0.50 1 d PRU . 2 H53B H 0.6481 0.6934 0.5993 0.134 Uiso 0.50 1 calc PR . 2 C54B C 0.6756(9) 0.581(2) 0.5846(11) 0.15(3) Uani 0.50 1 d PRU . 2 H54B H 0.6903 0.5957 0.5560 0.175 Uiso 0.50 1 calc PR . 2 C55B C 0.6793(9) 0.502(2) 0.6009(11) 0.10(2) Uani 0.50 1 d PRU . 2 H55B H 0.6964 0.4619 0.5833 0.126 Uiso 0.50 1 calc PR . 2 C56B C 0.6579(9) 0.480(2) 0.6428(11) 0.15(3) Uani 0.50 1 d PRU . 2 H56B H 0.6604 0.4257 0.6539 0.175 Uiso 0.50 1 calc PR . 2 C57B C 0.6328(9) 0.538(2) 0.6686(11) 0.12(3) Uani 0.50 1 d PRU . 2 H57B H 0.6182 0.5234 0.6972 0.142 Uiso 0.50 1 calc PR . 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 U1 0.0383(8) 0.0520(12) 0.0473(9) 0.000 0.000 0.000 U2 0.0429(4) 0.0567(5) 0.0494(4) -0.0020(6) -0.0009(3) 0.0019(5) U3 0.0450(9) 0.0557(13) 0.0556(11) 0.000 0.000 0.000 O1U 0.023(8) 0.044(13) 0.074(13) 0.000 0.000 0.005(9) O2U 0.050(11) 0.056(15) 0.051(12) 0.012(11) 0.000 0.000 O3U 0.051(10) 0.059(15) 0.052(12) -0.009(12) 0.000 0.000 O4U 0.039(10) 0.060(15) 0.062(12) 0.000 0.000 -0.004(11) O1 0.042(7) 0.046(11) 0.067(9) 0.006(8) 0.001(7) 0.007(7) O2 0.042(8) 0.052(11) 0.066(10) -0.005(10) 0.007(7) 0.002(8) C1 0.033(9) 0.12(3) 0.025(9) 0.025(16) 0.002(8) -0.004(16) C2 0.066(14) 0.050(16) 0.062(14) -0.023(14) 0.001(12) 0.006(13) C3 0.081(16) 0.09(2) 0.066(15) -0.023(17) 0.029(14) -0.031(17) C4 0.10(2) 0.11(3) 0.060(16) 0.000(19) 0.021(15) -0.04(2) C5 0.10(2) 0.11(3) 0.14(3) 0.07(3) -0.02(2) -0.05(2) C6 0.072(18) 0.10(3) 0.16(3) 0.06(3) 0.03(2) 0.00(2) C7 0.079(17) 0.049(17) 0.088(19) 0.007(16) 0.010(15) -0.008(15) N1 0.06(3) 0.18(7) 0.05(2) 0.000 0.000 0.000 C11 0.07(3) 0.09(4) 0.13(4) 0.000 0.000 0.03(3) C12 0.11(4) 0.11(5) 0.11(3) 0.000 0.000 0.06(4) C13 0.12(6) 0.05(4) 0.14(6) 0.000 0.000 0.000 O21 0.061(8) 0.083(13) 0.051(8) -0.009(11) -0.005(7) 0.000(11) C21 0.045(15) 0.07(2) 0.041(14) 0.00(2) 0.000 0.000 C22 0.060(18) 0.12(4) 0.055(18) -0.01(3) 0.000 0.000 C23 0.074(16) 0.21(4) 0.054(15) 0.00(2) 0.005(13) 0.01(3) C24 0.082(19) 0.32(7) 0.062(17) 0.03(3) -0.001(15) 0.10(3) C25 0.13(4) 0.23(7) 0.021(15) 0.04(3) 0.000 0.000 O31 0.038(7) 0.093(15) 0.062(9) -0.016(11) 0.000(7) 0.011(9) C31 0.064(19) 0.04(2) 0.057(19) 0.000 0.000 0.006(16) C32 0.041(15) 0.05(2) 0.061(19) 0.000 0.000 -0.022(16) C33 0.072(16) 0.14(3) 0.080(18) -0.03(2) 0.001(15) 0.04(2) C34 0.067(17) 0.16(4) 0.09(2) -0.02(2) -0.017(15) 0.04(2) C35 0.047(19) 0.05(3) 0.15(4) 0.000 0.000 0.014(19) N2 0.057(17) 0.02(2) 0.027(14) -0.005(14) -0.016(13) -0.003(15) C41 0.077(16) 0.073(17) 0.074(16) 0.004(10) 0.004(10) 0.005(10) C42 0.085(18) 0.087(19) 0.085(18) 0.002(10) 0.008(10) 0.002(10) C43 0.055(13) 0.056(15) 0.063(14) -0.005(10) -0.013(9) -0.001(9) C44 0.10(2) 0.10(2) 0.10(2) 0.005(10) 0.002(10) 0.007(10) C45 0.052(14) 0.059(15) 0.060(14) 0.005(9) 0.008(9) 0.001(9) O51 0.050(9) 0.102(17) 0.083(12) -0.004(13) 0.013(9) -0.016(11) O52 0.060(9) 0.089(15) 0.059(9) -0.010(10) 0.000(7) 0.015(10) C51 0.039(12) 0.10(3) 0.12(3) -0.03(2) 0.011(16) 0.002(17) C52 0.07(2) 0.07(2) 0.09(2) 0.001(18) 0.013(16) 0.006(17) C53 0.066(19) 0.06(2) 0.08(2) 0.001(17) -0.010(16) -0.015(16) C54 0.053(17) 0.07(2) 0.069(19) -0.004(17) 0.021(15) 0.014(16) C55 0.08(2) 0.10(3) 0.10(2) 0.010(19) -0.006(17) 0.001(18) C56 0.08(2) 0.10(3) 0.09(2) 0.000(18) -0.009(17) 0.006(18) C57 0.08(2) 0.09(3) 0.10(2) 0.000(18) 0.015(18) 0.007(18) N3 0.07(2) 0.07(3) 0.10(2) 0.000 0.000 0.00(2) C61 0.05(2) 0.07(4) 0.07(3) 0.00(2) -0.01(2) 0.01(2) C62 0.12(5) 0.16(7) 0.19(7) 0.12(6) 0.09(5) 0.11(5) C52B 0.11(3) 0.11(3) 0.12(3) 0.004(19) 0.028(18) -0.002(19) C53B 0.11(3) 0.10(3) 0.12(3) 0.002(19) 0.015(18) -0.008(19) C54B 0.14(3) 0.14(4) 0.15(4) -0.01(2) 0.015(19) -0.005(19) C55B 0.10(2) 0.10(3) 0.11(3) 0.000(19) -0.001(18) 0.009(19) C56B 0.15(3) 0.15(4) 0.14(3) -0.01(2) -0.006(19) 0.010(19) C57B 0.12(3) 0.12(3) 0.12(3) 0.011(19) 0.012(19) -0.002(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2U 2.23(2) 10_557 ? U1 O2U 2.23(2) . ? U1 O1U 2.453(17) . ? U1 O1U 2.453(17) 3_656 ? U1 O1 2.470(14) 10_557 ? U1 O1 2.470(14) 3_656 ? U1 O1 2.470(14) . ? U1 O1 2.470(14) 12_655 ? U1 N1 2.94(7) . ? U1 U2 3.858(3) 10_557 ? U1 U2 3.858(3) 3_656 ? U1 U2 3.858(3) 12_655 ? U2 O4U 2.255(13) . ? U2 O2U 2.271(13) . ? U2 O31 2.423(13) . ? U2 O21 2.424(13) . ? U2 O1U 2.427(13) . ? U2 O2 2.437(18) . ? U2 O3U 2.455(15) . ? U2 O51 2.47(2) . ? U2 N2 2.854(11) . ? U2 U3 3.823(3) . ? U2 U2 3.8327(15) 12_655 ? U2 U2 3.8477(16) 10_557 ? U3 O4U 2.25(2) . ? U3 O4U 2.25(2) 3_656 ? U3 O52 2.409(16) . ? U3 O52 2.409(16) 10_557 ? U3 O52 2.410(16) 3_656 ? U3 O52 2.410(16) 12_655 ? U3 O3U 2.42(2) 10_557 ? U3 O3U 2.42(2) . ? U3 U2 3.823(3) 10_557 ? U3 U2 3.823(3) 3_656 ? U3 U2 3.823(3) 12_655 ? O1U U2 2.427(13) 10_557 ? O2U U2 2.271(13) 12_655 ? O3U U2 2.455(15) 12_655 ? O4U U2 2.255(13) 10_557 ? O1 C1 1.28(3) . ? O2 C1 1.23(3) . ? C1 C2 1.55(4) . ? C2 C7 1.34(3) . ? C2 C3 1.35(3) . ? C3 C4 1.28(4) . ? C4 C5 1.41(5) . ? C5 C6 1.35(5) . ? C6 C7 1.27(4) . ? N1 C11 1.28(5) 3_656 ? N1 C11 1.28(5) . ? C11 C12 1.34(6) . ? C12 C13 1.33(7) . ? C13 C12 1.33(7) 3_656 ? O21 C21 1.244(18) . ? C21 O21 1.244(18) 12_655 ? C21 C22 1.49(4) . ? C22 C23 1.28(3) . ? C22 C23 1.28(3) 12_655 ? C23 C24 1.39(4) . ? C24 C25 1.33(3) . ? C25 C24 1.33(3) 12_655 ? O31 C31 1.232(19) . ? C31 O31 1.232(19) 10_557 ? C31 C32 1.56(4) . ? C32 C33 1.36(3) 10_557 ? C32 C33 1.36(3) . ? C33 C34 1.35(3) . ? C34 C35 1.35(3) . ? C35 C34 1.35(3) 10_557 ? N2 C41 1.3900 . ? N2 C45 1.3900 . ? C41 C42 1.3899 . ? C42 C43 1.3900 . ? C43 C44 1.3902 . ? C44 C45 1.3899 . ? O51 C51 1.25(3) . ? O52 C51 1.23(2) . ? C51 C52 1.6194 . ? C51 C52B 1.67(4) . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3902 . ? N3 C61 1.10(4) 10_557 ? N3 C61 1.10(4) . ? C61 C61 0.92(8) 10_557 ? C61 C62 1.59(5) . ? C62 C62 1.95(6) 10_557 ? C52B C53B 1.3898 . ? C52B C57B 1.3901 . ? C53B C54B 1.3901 . ? C54B C55B 1.3898 . ? C55B C56B 1.3899 . ? C56B C57B 1.3902 . ? 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 O2U U1 O2U 90.5(11) 10_557 . ? O2U U1 O1U 68.6(4) 10_557 . ? O2U U1 O1U 68.6(4) . . ? O2U U1 O1U 68.6(4) 10_557 3_656 ? O2U U1 O1U 68.6(4) . 3_656 ? O1U U1 O1U 117.5(9) . 3_656 ? O2U U1 O1 79.4(6) 10_557 10_557 ? O2U U1 O1 140.5(3) . 10_557 ? O1U U1 O1 72.2(5) . 10_557 ? O1U U1 O1 137.6(3) 3_656 10_557 ? O2U U1 O1 79.4(6) 10_557 3_656 ? O2U U1 O1 140.5(4) . 3_656 ? O1U U1 O1 137.6(3) . 3_656 ? O1U U1 O1 72.2(5) 3_656 3_656 ? O1 U1 O1 75.2(6) 10_557 3_656 ? O2U U1 O1 140.5(3) 10_557 . ? O2U U1 O1 79.4(6) . . ? O1U U1 O1 72.2(5) . . ? O1U U1 O1 137.6(3) 3_656 . ? O1 U1 O1 84.7(7) 10_557 . ? O1 U1 O1 130.7(7) 3_656 . ? O2U U1 O1 140.5(4) 10_557 12_655 ? O2U U1 O1 79.4(6) . 12_655 ? O1U U1 O1 137.6(3) . 12_655 ? O1U U1 O1 72.2(5) 3_656 12_655 ? O1 U1 O1 130.7(7) 10_557 12_655 ? O1 U1 O1 84.7(7) 3_656 12_655 ? O1 U1 O1 75.2(6) . 12_655 ? O2U U1 N1 134.8(5) 10_557 . ? O2U U1 N1 134.8(5) . . ? O1U U1 N1 121.2(5) . . ? O1U U1 N1 121.2(5) 3_656 . ? O1 U1 N1 65.3(4) 10_557 . ? O1 U1 N1 65.3(4) 3_656 . ? O1 U1 N1 65.3(4) . . ? O1 U1 N1 65.3(4) 12_655 . ? O2U U1 U2 31.32(16) 10_557 10_557 ? O2U U1 U2 81.6(5) . 10_557 ? O1U U1 U2 37.5(3) . 10_557 ? O1U U1 U2 93.2(4) 3_656 10_557 ? O1 U1 U2 70.0(4) 10_557 10_557 ? O1 U1 U2 105.3(3) 3_656 10_557 ? O1 U1 U2 109.2(3) . 10_557 ? O1 U1 U2 159.3(4) 12_655 10_557 ? N1 U1 U2 135.26(4) . 10_557 ? O2U U1 U2 31.32(16) 10_557 3_656 ? O2U U1 U2 81.6(5) . 3_656 ? O1U U1 U2 93.2(4) . 3_656 ? O1U U1 U2 37.5(3) 3_656 3_656 ? O1 U1 U2 105.3(4) 10_557 3_656 ? O1 U1 U2 70.0(4) 3_656 3_656 ? O1 U1 U2 159.3(4) . 3_656 ? O1 U1 U2 109.2(3) 12_655 3_656 ? N1 U1 U2 135.26(4) . 3_656 ? U2 U1 U2 59.57(5) 10_557 3_656 ? O2U U1 U2 81.6(5) 10_557 12_655 ? O2U U1 U2 31.32(16) . 12_655 ? O1U U1 U2 93.2(4) . 12_655 ? O1U U1 U2 37.5(3) 3_656 12_655 ? O1 U1 U2 159.3(4) 10_557 12_655 ? O1 U1 U2 109.2(3) 3_656 12_655 ? O1 U1 U2 105.3(4) . 12_655 ? O1 U1 U2 70.0(4) 12_655 12_655 ? N1 U1 U2 135.26(4) . 12_655 ? U2 U1 U2 89.47(8) 10_557 12_655 ? U2 U1 U2 59.82(5) 3_656 12_655 ? O4U U2 O2U 91.4(7) . . ? O4U U2 O31 77.7(6) . . ? O2U U2 O31 141.2(6) . . ? O4U U2 O21 141.2(6) . . ? O2U U2 O21 80.3(6) . . ? O31 U2 O21 130.1(5) . . ? O4U U2 O1U 68.8(7) . . ? O2U U2 O1U 68.4(6) . . ? O31 U2 O1U 72.9(5) . . ? O21 U2 O1U 138.0(6) . . ? O4U U2 O2 139.6(6) . . ? O2U U2 O2 82.1(6) . . ? O31 U2 O2 82.7(6) . . ? O21 U2 O2 77.1(6) . . ? O1U U2 O2 71.7(5) . . ? O4U U2 O3U 69.7(6) . . ? O2U U2 O3U 70.9(7) . . ? O31 U2 O3U 135.1(6) . . ? O21 U2 O3U 71.8(6) . . ? O1U U2 O3U 119.8(6) . . ? O2 U2 O3U 141.5(6) . . ? O4U U2 O51 77.6(7) . . ? O2U U2 O51 142.5(6) . . ? O31 U2 O51 71.7(6) . . ? O21 U2 O51 86.3(6) . . ? O1U U2 O51 135.3(6) . . ? O2 U2 O51 128.7(5) . . ? O3U U2 O51 71.7(6) . . ? O4U U2 N2 131.4(6) . . ? O2U U2 N2 137.0(6) . . ? O31 U2 N2 66.3(4) . . ? O21 U2 N2 63.8(4) . . ? O1U U2 N2 125.0(5) . . ? O2 U2 N2 68.0(5) . . ? O3U U2 N2 115.1(5) . . ? O51 U2 N2 61.1(6) . . ? O4U U2 U3 31.8(5) . . ? O2U U2 U3 82.2(5) . . ? O31 U2 U3 103.9(4) . . ? O21 U2 U3 109.4(4) . . ? O1U U2 U3 93.7(4) . . ? O2 U2 U3 161.7(4) . . ? O3U U2 U3 38.0(5) . . ? O51 U2 U3 69.5(4) . . ? N2 U2 U3 130.3(4) . . ? O4U U2 U2 82.6(4) . 12_655 ? O2U U2 U2 32.5(5) . 12_655 ? O31 U2 U2 159.4(4) . 12_655 ? O21 U2 U2 70.1(3) . 12_655 ? O1U U2 U2 94.3(4) . 12_655 ? O2 U2 U2 109.0(4) . 12_655 ? O3U U2 U2 38.7(4) . 12_655 ? O51 U2 U2 110.1(4) . 12_655 ? N2 U2 U2 133.3(2) . 12_655 ? U3 U2 U2 59.92(3) . 12_655 ? O4U U2 U2 31.4(5) . 10_557 ? O2U U2 U2 81.4(5) . 10_557 ? O31 U2 U2 70.0(3) . 10_557 ? O21 U2 U2 159.9(3) . 10_557 ? O1U U2 U2 37.6(4) . 10_557 ? O2 U2 U2 108.4(4) . 10_557 ? O3U U2 U2 94.5(5) . 10_557 ? O51 U2 U2 103.6(4) . 10_557 ? N2 U2 U2 136.3(2) . 10_557 ? U3 U2 U2 59.79(3) . 10_557 ? U2 U2 U2 89.998(1) 12_655 10_557 ? O4U U3 O4U 92.7(11) . 3_656 ? O4U U3 O52 81.2(6) . . ? O4U U3 O52 142.5(4) 3_656 . ? O4U U3 O52 81.2(6) . 10_557 ? O4U U3 O52 142.5(4) 3_656 10_557 ? O52 U3 O52 73.3(7) . 10_557 ? O4U U3 O52 142.5(4) . 3_656 ? O4U U3 O52 81.2(6) 3_656 3_656 ? O52 U3 O52 124.6(10) . 3_656 ? O52 U3 O52 81.7(8) 10_557 3_656 ? O4U U3 O52 142.5(4) . 12_655 ? O4U U3 O52 81.2(6) 3_656 12_655 ? O52 U3 O52 81.7(8) . 12_655 ? O52 U3 O52 124.6(10) 10_557 12_655 ? O52 U3 O52 73.3(7) 3_656 12_655 ? O4U U3 O3U 70.5(4) . 10_557 ? O4U U3 O3U 70.5(4) 3_656 10_557 ? O52 U3 O3U 138.4(4) . 10_557 ? O52 U3 O3U 72.7(6) 10_557 10_557 ? O52 U3 O3U 72.7(6) 3_656 10_557 ? O52 U3 O3U 138.4(4) 12_655 10_557 ? O4U U3 O3U 70.5(4) . . ? O4U U3 O3U 70.5(4) 3_656 . ? O52 U3 O3U 72.7(6) . . ? O52 U3 O3U 138.4(4) 10_557 . ? O52 U3 O3U 138.4(4) 3_656 . ? O52 U3 O3U 72.6(6) 12_655 . ? O3U U3 O3U 122.2(11) 10_557 . ? O4U U3 U2 31.94(18) . 10_557 ? O4U U3 U2 82.9(5) 3_656 10_557 ? O52 U3 U2 107.4(4) . 10_557 ? O52 U3 U2 72.5(5) 10_557 10_557 ? O52 U3 U2 110.8(4) 3_656 10_557 ? O52 U3 U2 162.8(5) 12_655 10_557 ? O3U U3 U2 38.7(3) 10_557 10_557 ? O3U U3 U2 95.7(5) . 10_557 ? O4U U3 U2 82.9(5) . 3_656 ? O4U U3 U2 31.94(18) 3_656 3_656 ? O52 U3 U2 162.8(5) . 3_656 ? O52 U3 U2 110.8(4) 10_557 3_656 ? O52 U3 U2 72.5(5) 3_656 3_656 ? O52 U3 U2 107.4(4) 12_655 3_656 ? O3U U3 U2 38.7(3) 10_557 3_656 ? O3U U3 U2 95.7(5) . 3_656 ? U2 U3 U2 60.16(5) 10_557 3_656 ? O4U U3 U2 82.9(5) . 12_655 ? O4U U3 U2 31.94(17) 3_656 12_655 ? O52 U3 U2 110.7(4) . 12_655 ? O52 U3 U2 162.8(5) 10_557 12_655 ? O52 U3 U2 107.4(4) 3_656 12_655 ? O52 U3 U2 72.5(5) 12_655 12_655 ? O3U U3 U2 95.7(5) 10_557 12_655 ? O3U U3 U2 38.7(3) . 12_655 ? U2 U3 U2 90.51(9) 10_557 12_655 ? U2 U3 U2 60.42(5) 3_656 12_655 ? O4U U3 U2 31.94(17) . . ? O4U U3 U2 82.9(5) 3_656 . ? O52 U3 U2 72.5(5) . . ? O52 U3 U2 107.4(4) 10_557 . ? O52 U3 U2 162.8(5) 3_656 . ? O52 U3 U2 110.7(4) 12_655 . ? O3U U3 U2 95.8(5) 10_557 . ? O3U U3 U2 38.7(3) . . ? U2 U3 U2 60.42(5) 10_557 . ? U2 U3 U2 90.51(9) 3_656 . ? U2 U3 U2 60.16(5) 12_655 . ? U2 O1U U2 104.9(8) 10_557 . ? U2 O1U U1 104.5(4) 10_557 . ? U2 O1U U1 104.5(4) . . ? U1 O2U U2 118.0(5) . 12_655 ? U1 O2U U2 118.0(5) . . ? U2 O2U U2 115.1(10) 12_655 . ? U3 O3U U2 103.3(6) . 12_655 ? U3 O3U U2 103.3(6) . . ? U2 O3U U2 102.6(9) 12_655 . ? U3 O4U U2 116.2(4) . 10_557 ? U3 O4U U2 116.2(4) . . ? U2 O4U U2 117.1(11) 10_557 . ? C1 O1 U1 135.7(18) . . ? C1 O2 U2 135.2(14) . . ? O2 C1 O1 127(2) . . ? O2 C1 C2 119.6(19) . . ? O1 C1 C2 113(3) . . ? C7 C2 C3 114(3) . . ? C7 C2 C1 124(2) . . ? C3 C2 C1 122(3) . . ? C4 C3 C2 128(3) . . ? C3 C4 C5 113(3) . . ? C6 C5 C4 123(3) . . ? C7 C6 C5 117(3) . . ? C6 C7 C2 126(3) . . ? C11 N1 C11 115(7) 3_656 . ? C11 N1 U1 122(4) 3_656 . ? C11 N1 U1 122(4) . . ? N1 C11 C12 127(6) . . ? C13 C12 C11 113(6) . . ? C12 C13 C12 126(8) 3_656 . ? C21 O21 U2 138.5(15) . . ? O21 C21 O21 123(3) . 12_655 ? O21 C21 C22 118.5(13) . . ? O21 C21 C22 118.5(13) 12_655 . ? C23 C22 C23 114(3) . 12_655 ? C23 C22 C21 123.0(17) . . ? C23 C22 C21 123.0(17) 12_655 . ? C22 C23 C24 126(3) . . ? C25 C24 C23 115(3) . . ? C24 C25 C24 123(3) 12_655 . ? C31 O31 U2 134.9(17) . . ? O31 C31 O31 125(3) 10_557 . ? O31 C31 C32 117.1(15) 10_557 . ? O31 C31 C32 117.1(15) . . ? C33 C32 C33 119(3) 10_557 . ? C33 C32 C31 120.7(16) 10_557 . ? C33 C32 C31 120.7(16) . . ? C34 C33 C32 121(3) . . ? C35 C34 C33 119(3) . . ? C34 C35 C34 121(3) . 10_557 ? C41 N2 C45 120.0 . . ? C41 N2 U2 119.3(3) . . ? C45 N2 U2 120.1(3) . . ? C42 C41 N2 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 N2 120.0 . . ? C51 O51 U2 134.9(14) . . ? C51 O52 U3 132.3(17) . . ? O52 C51 O51 129(2) . . ? O52 C51 C52 110.9(14) . . ? O51 C51 C52 120.1(12) . . ? O52 C51 C52B 119(2) . . ? O51 C51 C52B 112(2) . . ? C52 C51 C52B 19.2(12) . . ? C53 C52 C57 120.0 . . ? C53 C52 C51 120.1 . . ? C57 C52 C51 118.5 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C52 C57 C56 120.0 . . ? C61 N3 C61 49(5) 10_557 . ? C61 C61 N3 65(2) 10_557 . ? C61 C61 C62 109.0(19) 10_557 . ? N3 C61 C62 174(4) . . ? C61 C62 C62 71.0(19) . 10_557 ? C53B C52B C57B 120.0 . . ? C53B C52B C51 117.4(14) . . ? C57B C52B C51 121.9(14) . . ? C52B C53B C54B 120.0 . . ? C55B C54B C53B 120.0 . . ? C54B C55B C56B 120.0 . . ? C55B C56B C57B 120.0 . . ? C52B C57B C56B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.634 _refine_diff_density_min -2.019 _refine_diff_density_rms 0.334 data_2 _database_code_depnum_ccdc_archive 'CCDC 776756' #TrackingRef '- cif final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 N2 O6 U' _chemical_formula_weight 670.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3216(9) _cell_length_b 10.0554(8) _cell_length_c 10.1130(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.493(8) _cell_angle_gamma 90.00 _cell_volume 1146.00(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3800 _cell_measurement_theta_min 3.4824 _cell_measurement_theta_max 32.3968 _exptl_crystal_description bloc _exptl_crystal_colour yellow _exptl_crystal_size_max 1.06 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 7.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0494 _exptl_absorpt_correction_T_max 0.1662 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6840 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 32.52 _reflns_number_total 3712 _reflns_number_gt 2292 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 9.00 69.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 25.5614 37.0000 -90.0000 60 #__ type_ start__ end____ width___ exp.time_ 2 omega -96.00 3.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -27.4364 -77.0000 -60.0000 99 #__ type_ start__ end____ width___ exp.time_ 3 omega -52.00 36.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -27.4364 77.0000 60.0000 88 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3712 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.2078(6) -0.1215(6) 0.6301(7) 0.0346(13) Uani 1 1 d . . . U1 U 0.0000 0.0000 0.5000 0.03180(12) Uani 1 2 d S . . C1 C 0.4182(6) -0.1090(7) 0.7270(7) 0.0374(14) Uani 1 1 d . . . H1 H 0.4263 -0.0300 0.6772 0.045 Uiso 1 1 calc R . . C4 C 0.3922(7) -0.3406(8) 0.8708(8) 0.0441(16) Uani 1 1 d . . . H4 H 0.3833 -0.4198 0.9201 0.053 Uiso 1 1 calc R . . C5 C 0.2986(6) -0.2921(6) 0.7872(7) 0.0358(13) Uani 1 1 d . . . H5 H 0.2251 -0.3383 0.7788 0.043 Uiso 1 1 calc R . . O1 O 0.2143(5) -0.0082(4) 0.5771(6) 0.0395(11) Uani 1 1 d . . . O3 O -0.0369(4) 0.0512(6) 0.6583(5) 0.0383(10) Uani 1 1 d . . . O2 O 0.1122(4) -0.1858(5) 0.6129(6) 0.0435(12) Uani 1 1 d . . . C9 C 0.3110(6) -0.1764(7) 0.7156(7) 0.0343(13) Uani 1 1 d . . . N1 N 0.1113(5) 0.2246(6) 0.4909(6) 0.0380(12) Uani 1 1 d . . . C7 C 0.5131(7) -0.1551(8) 0.8095(8) 0.0445(16) Uani 1 1 d . . . H7 H 0.5863 -0.1082 0.8168 0.053 Uiso 1 1 calc R . . C13 C 0.1387(8) 0.4494(8) 0.5573(8) 0.0442(16) Uani 1 1 d . . . H13 H 0.1176 0.5212 0.6114 0.053 Uiso 1 1 calc R . . C14 C 0.0849(7) 0.3267(7) 0.5657(7) 0.0392(14) Uani 1 1 d . . . H14 H 0.0271 0.3151 0.6269 0.047 Uiso 1 1 calc R . . C8 C 0.5011(7) -0.2715(8) 0.8824(8) 0.0490(18) Uani 1 1 d . . . H8 H 0.5661 -0.3041 0.9396 0.059 Uiso 1 1 calc R . . C10 C 0.2498(7) 0.3621(8) 0.3922(8) 0.0459(17) Uani 1 1 d . . . H10 H 0.3062 0.3723 0.3292 0.055 Uiso 1 1 calc R . . C11 C 0.1936(7) 0.2409(7) 0.4064(7) 0.0397(14) Uani 1 1 d . . . H11 H 0.2144 0.1674 0.3543 0.048 Uiso 1 1 calc R . . C15 C 0.2227(9) 0.4662(10) 0.4703(9) 0.051(2) Uani 1 1 d . . . H15 H 0.2617 0.5494 0.4643 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.035(3) 0.034(3) 0.035(3) 0.000(3) 0.005(3) 0.002(2) U1 0.02871(16) 0.03310(17) 0.03379(17) 0.00190(16) 0.00406(10) 0.00086(14) C1 0.033(3) 0.039(3) 0.039(3) -0.001(3) 0.002(3) -0.001(3) C4 0.043(4) 0.047(4) 0.043(4) -0.001(3) 0.005(3) 0.001(3) C5 0.036(3) 0.035(3) 0.037(3) 0.001(3) 0.006(3) 0.000(3) O1 0.032(2) 0.039(3) 0.047(3) 0.004(2) 0.0005(19) 0.0009(19) O3 0.042(3) 0.040(2) 0.034(2) -0.002(2) 0.009(2) 0.002(2) O2 0.037(3) 0.036(2) 0.055(3) 0.009(2) -0.005(2) -0.001(2) C9 0.032(3) 0.036(3) 0.034(3) 0.001(3) 0.002(2) 0.002(2) N1 0.038(3) 0.042(3) 0.034(3) 0.001(2) -0.001(2) 0.003(2) C7 0.034(3) 0.049(4) 0.049(4) -0.002(3) -0.001(3) -0.002(3) C13 0.054(4) 0.035(3) 0.042(4) -0.002(3) -0.002(3) -0.001(4) C14 0.040(3) 0.038(3) 0.040(3) 0.000(3) 0.005(3) 0.002(3) C8 0.042(4) 0.057(4) 0.046(4) -0.001(4) -0.007(3) 0.008(3) C10 0.048(4) 0.050(4) 0.041(4) 0.002(3) 0.013(3) -0.008(3) C11 0.041(3) 0.038(3) 0.041(3) 0.006(3) 0.008(3) 0.004(3) C15 0.059(5) 0.048(4) 0.044(4) 0.005(3) -0.002(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2 O2 1.258(8) . ? C2 O1 1.265(7) . ? C2 C9 1.491(9) . ? C2 U1 2.858(7) . ? U1 O3 1.769(5) . ? U1 O3 1.769(5) 3_556 ? U1 O2 2.476(5) . ? U1 O2 2.476(5) 3_556 ? U1 O1 2.478(5) 3_556 ? U1 O1 2.478(5) . ? U1 N1 2.592(6) 3_556 ? U1 N1 2.592(6) . ? U1 C2 2.858(7) 3_556 ? C1 C7 1.377(10) . ? C1 C9 1.385(9) . ? C4 C5 1.380(10) . ? C4 C8 1.410(11) . ? C5 C9 1.385(9) . ? N1 C14 1.326(9) . ? N1 C11 1.334(9) . ? C7 C8 1.397(11) . ? C13 C15 1.366(13) . ? C13 C14 1.382(11) . ? C10 C15 1.365(12) . ? C10 C11 1.388(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C2 O1 119.3(6) . . ? O2 C2 C9 120.4(6) . . ? O1 C2 C9 120.3(6) . . ? O2 C2 U1 59.8(3) . . ? O1 C2 U1 59.9(4) . . ? C9 C2 U1 171.9(5) . . ? O3 U1 O3 180.0 . 3_556 ? O3 U1 O2 87.6(2) . . ? O3 U1 O2 92.4(2) 3_556 . ? O3 U1 O2 92.4(2) . 3_556 ? O3 U1 O2 87.6(2) 3_556 3_556 ? O2 U1 O2 180.0(2) . 3_556 ? O3 U1 O1 88.0(2) . 3_556 ? O3 U1 O1 92.0(2) 3_556 3_556 ? O2 U1 O1 127.87(15) . 3_556 ? O2 U1 O1 52.13(15) 3_556 3_556 ? O3 U1 O1 92.0(2) . . ? O3 U1 O1 88.0(2) 3_556 . ? O2 U1 O1 52.13(15) . . ? O2 U1 O1 127.87(15) 3_556 . ? O1 U1 O1 179.999(1) 3_556 . ? O3 U1 N1 93.7(2) . 3_556 ? O3 U1 N1 86.3(2) 3_556 3_556 ? O2 U1 N1 63.62(17) . 3_556 ? O2 U1 N1 116.38(17) 3_556 3_556 ? O1 U1 N1 64.89(15) 3_556 3_556 ? O1 U1 N1 115.11(15) . 3_556 ? O3 U1 N1 86.3(2) . . ? O3 U1 N1 93.7(2) 3_556 . ? O2 U1 N1 116.38(17) . . ? O2 U1 N1 63.62(17) 3_556 . ? O1 U1 N1 115.11(15) 3_556 . ? O1 U1 N1 64.89(15) . . ? N1 U1 N1 180.0 3_556 . ? O3 U1 C2 87.9(2) . . ? O3 U1 C2 92.1(2) 3_556 . ? O2 U1 C2 26.05(17) . . ? O2 U1 C2 153.95(17) 3_556 . ? O1 U1 C2 153.80(16) 3_556 . ? O1 U1 C2 26.20(16) . . ? N1 U1 C2 89.57(18) 3_556 . ? N1 U1 C2 90.43(18) . . ? O3 U1 C2 92.1(2) . 3_556 ? O3 U1 C2 87.9(2) 3_556 3_556 ? O2 U1 C2 153.95(17) . 3_556 ? O2 U1 C2 26.05(17) 3_556 3_556 ? O1 U1 C2 26.20(16) 3_556 3_556 ? O1 U1 C2 153.80(16) . 3_556 ? N1 U1 C2 90.43(18) 3_556 3_556 ? N1 U1 C2 89.57(18) . 3_556 ? C2 U1 C2 180.0 . 3_556 ? C7 C1 C9 120.8(7) . . ? C5 C4 C8 119.4(7) . . ? C4 C5 C9 120.5(7) . . ? C2 O1 U1 93.9(4) . . ? C2 O2 U1 94.2(4) . . ? C1 C9 C5 120.0(6) . . ? C1 C9 C2 119.9(6) . . ? C5 C9 C2 120.0(6) . . ? C14 N1 C11 118.7(7) . . ? C14 N1 U1 121.2(5) . . ? C11 N1 U1 120.1(5) . . ? C1 C7 C8 119.5(7) . . ? C15 C13 C14 119.2(8) . . ? N1 C14 C13 122.1(8) . . ? C7 C8 C4 119.8(7) . . ? C15 C10 C11 118.9(8) . . ? N1 C11 C10 122.0(7) . . ? C10 C15 C13 119.1(8) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 32.52 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 5.148 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.375 # Attachment '- U6O8PY6.cif' data_vm197_3 _database_code_depnum_ccdc_archive 'CCDC 793677' #TrackingRef '- U6O8PY6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C113 H95 N7 O32 U6' _chemical_formula_weight 3491.14 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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 27.4352(4) _cell_length_b 16.3250(2) _cell_length_c 28.7642(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12882.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23894 _cell_measurement_theta_min 3.3151 _cell_measurement_theta_max 32.3654 _exptl_crystal_description 'monoclinic prism' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6520 _exptl_absorpt_coefficient_mu 7.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1992 _exptl_absorpt_correction_T_max 0.4810 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _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 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9653 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66545 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8304 _reflns_number_gt 5833 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 50.00 75.50 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 30.0000 34 #__ type_ start__ end____ width___ exp.time_ 2 omega 33.00 90.75 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 -139.0000 140.0000 77 #__ type_ start__ end____ width___ exp.time_ 3 omega 34.00 89.50 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 -139.0000 -20.0000 74 #__ type_ start__ end____ width___ exp.time_ 4 omega 49.00 74.50 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - 25.2489 179.0000 -180.0000 34 #__ type_ start__ end____ width___ exp.time_ 5 omega -90.00 -32.25 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 179.0000 -90.0000 77 #__ type_ start__ end____ width___ exp.time_ 6 omega -49.00 18.50 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 37.0000 -120.0000 90 #__ type_ start__ end____ width___ exp.time_ 7 omega -54.00 -25.50 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 77.0000 -180.0000 38 #__ type_ start__ end____ width___ exp.time_ 8 omega -85.00 45.50 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 0.0000 -180.0000 174 #__ type_ start__ end____ width___ exp.time_ 9 omega -97.00 -46.00 0.7500 30.0000 omega____ theta____ kappa____ phi______ frames - -27.1239 -77.0000 120.0000 68 ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1353P)^2^+484.7964P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8304 _refine_ls_number_parameters 465 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.2725 _refine_ls_wR_factor_gt 0.2655 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.569486(18) 0.38825(3) 0.816674(18) 0.03755(19) Uani 1 1 d . . . U2 U 0.5000 0.22472(6) 0.7500 0.0380(3) Uani 1 4 d S . . U3 U 0.5000 0.55524(6) 0.7500 0.0359(3) Uani 1 4 d S . . O1U O 0.5568(5) 0.3189(8) 0.7500 0.041(3) Uani 1 2 d S . . O2U O 0.5000 0.4553(9) 0.8041(5) 0.041(3) Uani 1 2 d S . . O3U O 0.5000 0.2968(9) 0.8239(5) 0.038(3) Uani 1 2 d S . . H3O H 0.5000 0.2611 0.8522 0.045 Uiso 1 2 calc SR . . O4U O 0.4228(5) 0.4792(8) 0.7500 0.036(3) Uani 1 2 d S . . H4O H 0.3929 0.5142 0.7500 0.043 Uiso 1 2 calc SR . . O1 O 0.5545(4) 0.6166(7) 0.6925(4) 0.047(2) Uani 1 1 d . . . O2 O 0.5984(4) 0.5205(6) 0.6559(4) 0.043(2) Uani 1 1 d . . . C1 C 0.5866(5) 0.5929(12) 0.6647(5) 0.048(4) Uani 1 1 d . . . C2 C 0.6126(6) 0.6585(10) 0.6373(5) 0.049(3) Uani 1 1 d . . . C3 C 0.6546(7) 0.6416(13) 0.6122(6) 0.060(4) Uani 1 1 d . . . H3 H 0.6685 0.5883 0.6131 0.072 Uiso 1 1 calc R . . C4 C 0.6761(8) 0.7022(14) 0.5862(7) 0.071(5) Uani 1 1 d . . . H4 H 0.7050 0.6899 0.5694 0.085 Uiso 1 1 calc R . . C5 C 0.6577(10) 0.7778(17) 0.5836(9) 0.089(7) Uani 1 1 d . . . H5 H 0.6736 0.8187 0.5657 0.106 Uiso 1 1 calc R . . C6 C 0.6165(10) 0.7953(16) 0.6068(11) 0.099(9) Uani 1 1 d . . . H6 H 0.6026 0.8484 0.6042 0.119 Uiso 1 1 calc R . . C7 C 0.5936(7) 0.7359(13) 0.6349(8) 0.074(6) Uani 1 1 d . . . H7 H 0.5652 0.7495 0.6521 0.088 Uiso 1 1 calc R . . O11 O 0.4441(4) 0.1520(7) 0.7999(4) 0.052(3) Uani 1 1 d . . . O12 O 0.4008(4) 0.2506(8) 0.8371(5) 0.059(3) Uani 1 1 d . . . C11 C 0.4087(6) 0.1796(10) 0.8254(8) 0.063(5) Uani 1 1 d . A . C12 C 0.3655(15) 0.112(2) 0.8201(13) 0.057(9) Uani 0.50 1 d P A 1 C13 C 0.3713(14) 0.0361(18) 0.8027(15) 0.057(10) Uani 0.50 1 d P A 1 H13 H 0.4006 0.0227 0.7868 0.069 Uiso 0.50 1 calc PR A 1 C14 C 0.3366(16) -0.021(4) 0.8073(17) 0.090(16) Uani 0.50 1 d P A 1 H14 H 0.3429 -0.0752 0.7973 0.108 Uiso 0.50 1 calc PR A 1 C15 C 0.2923(14) -0.002(3) 0.8262(17) 0.077(13) Uani 0.50 1 d P A 1 H15 H 0.2660 -0.0404 0.8268 0.093 Uiso 0.50 1 calc PR A 1 C16 C 0.2886(14) 0.075(2) 0.8440(15) 0.066(10) Uani 0.50 1 d P A 1 H16 H 0.2591 0.0886 0.8595 0.079 Uiso 0.50 1 calc PR A 1 C17 C 0.3223(13) 0.131(3) 0.8415(14) 0.062(9) Uani 0.50 1 d P A 1 H17 H 0.3170 0.1836 0.8543 0.074 Uiso 0.50 1 calc PR A 1 C12B C 0.3780(12) 0.115(2) 0.8505(17) 0.058(9) Uani 0.50 1 d P A 2 C13B C 0.3731(9) 0.0427(13) 0.8324(10) 0.069(12) Uani 0.50 1 d P A 2 H13B H 0.3882 0.0315 0.8034 0.083 Uiso 0.50 1 calc PR A 2 C14B C 0.3465(9) -0.0189(13) 0.8541(10) 0.102(18) Uani 0.50 1 d PR A 2 H14B H 0.3449 -0.0719 0.8405 0.123 Uiso 0.50 1 calc PR A 2 C15B C 0.3223(9) -0.0031(13) 0.8956(10) 0.15(4) Uani 0.50 1 d PR A 2 H15B H 0.3042 -0.0452 0.9103 0.185 Uiso 0.50 1 calc PR A 2 C16B C 0.3247(9) 0.0745(13) 0.9154(10) 0.13(2) Uani 0.50 1 d PRU A 2 H16B H 0.3082 0.0853 0.9438 0.151 Uiso 0.50 1 calc PR A 2 C17B C 0.3513(9) 0.1361(13) 0.8938(10) 0.11(2) Uani 0.50 1 d PR A 2 H17B H 0.3523 0.1900 0.9063 0.135 Uiso 0.50 1 calc PR A 2 O21 O 0.6526(4) 0.3757(6) 0.7886(4) 0.047(2) Uani 1 1 d . . . C21 C 0.6707(7) 0.3638(13) 0.7500 0.048(5) Uani 1 2 d S . . C22 C 0.7233(8) 0.3299(15) 0.7500 0.057(6) Uani 1 2 d S . . C23 C 0.7465(8) 0.3144(16) 0.7908(8) 0.089(8) Uani 1 1 d . . . H23 H 0.7311 0.3269 0.8195 0.107 Uiso 1 1 calc R . . C24 C 0.7933(7) 0.2800(18) 0.7904(10) 0.096(9) Uani 1 1 d . . . H24 H 0.8094 0.2665 0.8187 0.115 Uiso 1 1 calc R . . C25 C 0.8144(10) 0.2667(15) 0.7500 0.078(10) Uani 1 2 d S . . H25 H 0.8468 0.2463 0.7500 0.093 Uiso 1 2 calc SR . . O31 O 0.5407(4) 0.3968(7) 0.8957(4) 0.048(2) Uani 1 1 d . . . C31 C 0.5000 0.3959(14) 0.9159(7) 0.042(4) Uani 1 2 d S . . C32 C 0.5000 0.3925(15) 0.9678(8) 0.050(5) Uani 1 2 d S . . C33 C 0.5409(8) 0.394(2) 0.9921(7) 0.104(11) Uani 1 1 d . . . H33 H 0.5710 0.3969 0.9759 0.125 Uiso 1 1 calc R . . C34 C 0.5417(9) 0.391(2) 1.0399(7) 0.107(11) Uani 1 1 d . . . H34 H 0.5718 0.3937 1.0562 0.128 Uiso 1 1 calc R . . C35 C 0.5000 0.385(2) 1.0631(10) 0.084(10) Uani 1 2 d S . . H35 H 0.5000 0.3754 1.0957 0.101 Uiso 1 2 calc SR . . N2 N 0.5000 0.726(2) 0.7500 0.061(8) Uani 1 4 d SU . 1 C51 C 0.4609(10) 0.7733(16) 0.7500 0.060(6) Uani 1 2 d SU B 1 H51 H 0.4305 0.7453 0.7500 0.072 Uiso 1 2 calc SR B 1 C52 C 0.4576(15) 0.8583(17) 0.7500 0.082(10) Uani 1 2 d S B 1 H52 H 0.4269 0.8851 0.7500 0.099 Uiso 1 2 calc SR B 1 C53 C 0.5000 0.9017(8) 0.7500 0.066(11) Uani 1 4 d S . 1 H53 H 0.5000 0.9599 0.7500 0.080 Uiso 1 4 calc SR . 1 N1 N 0.6398 0.3751(8) 0.8869 0.046(6) Uani 0.50 1 d PR . 1 C41 C 0.6840 0.4157(8) 0.8822 0.050(7) Uani 0.50 1 d PR . 1 H41 H 0.6884 0.4543 0.8579 0.060 Uiso 0.50 1 calc PR . 1 C42 C 0.7218 0.3999(8) 0.9132 0.076(13) Uani 0.50 1 d PR . 1 H42 H 0.7520 0.4277 0.9099 0.091 Uiso 0.50 1 calc PR . 1 C43 C 0.7153 0.3434(8) 0.9488 0.079(15) Uani 0.50 1 d PR . 1 H43 H 0.7411 0.3326 0.9699 0.095 Uiso 0.50 1 calc PR . 1 C44 C 0.6711 0.3028(8) 0.9535 0.068(10) Uani 0.50 1 d PR . 1 H44 H 0.6667 0.2642 0.9779 0.082 Uiso 0.50 1 calc PR . 1 C45 C 0.6333 0.3186(8) 0.9226 0.051(7) Uani 0.50 1 d PR . 1 H45 H 0.6031 0.2908 0.9258 0.062 Uiso 0.50 1 calc PR . 1 N3 N 0.1727(9) 0.0652(16) 0.7500 0.076(7) Uani 1 2 d S . 2 C61 C 0.2070(14) 0.079(3) 0.7651(13) 0.073(12) Uani 0.50 1 d P . 2 C62 C 0.2635(10) 0.0857(16) 0.7845(9) 0.12(2) Uani 0.50 1 d P . 2 N1B N 0.7367(10) 0.3543(16) 0.9734(9) 0.118(17) Uani 0.50 1 d PRU . 2 C41B C 0.7228(10) 0.4261(16) 0.9954(9) 0.102(16) Uani 0.50 1 d PR . 2 H41B H 0.7408 0.4456 1.0214 0.122 Uiso 0.50 1 calc PR . 2 C42B C 0.6824(10) 0.4695(16) 0.9797(9) 0.13(2) Uani 0.50 1 d PR . 2 C43B C 0.6560(10) 0.4411(16) 0.9418(9) 0.12(2) Uani 0.50 1 d PR . 2 H43B H 0.6284 0.4707 0.9311 0.144 Uiso 0.50 1 calc PR . 2 C44B C 0.6699(10) 0.3694(16) 0.9197(9) 0.13(3) Uani 0.50 1 d PR . 2 H44B H 0.6519 0.3499 0.8938 0.154 Uiso 0.50 1 calc PR . 2 C45B C 0.7103(10) 0.3261(16) 0.9355(9) 0.14(3) Uani 0.50 1 d PRU . 2 H45B H 0.7198 0.2770 0.9203 0.170 Uiso 0.50 1 calc PR . 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 U1 0.0365(3) 0.0388(3) 0.0374(3) 0.0009(2) 0.00097(18) 0.0009(2) U2 0.0370(5) 0.0355(5) 0.0414(6) 0.000 0.000 0.000 U3 0.0323(5) 0.0372(5) 0.0381(5) 0.000 0.000 0.000 O1U 0.039(7) 0.032(7) 0.052(8) 0.000 0.000 0.009(6) O2U 0.038(7) 0.048(8) 0.038(7) -0.009(6) 0.000 0.000 O3U 0.040(7) 0.038(7) 0.035(7) 0.000(5) 0.000 0.000 O4U 0.032(6) 0.036(7) 0.040(7) 0.000 0.000 0.004(5) O1 0.043(5) 0.046(6) 0.051(6) 0.001(5) 0.005(5) 0.008(5) O2 0.044(5) 0.036(5) 0.049(6) -0.002(4) 0.004(4) 0.000(4) C1 0.031(7) 0.077(12) 0.038(7) 0.003(7) 0.002(6) -0.003(7) C2 0.054(9) 0.046(8) 0.045(8) -0.001(7) -0.002(7) -0.003(7) C3 0.055(10) 0.068(11) 0.057(10) 0.000(8) 0.012(8) -0.017(8) C4 0.073(12) 0.081(14) 0.059(11) 0.005(10) 0.020(10) -0.011(11) C5 0.093(17) 0.094(18) 0.079(15) 0.034(13) 0.020(13) -0.011(14) C6 0.093(17) 0.076(15) 0.13(2) 0.048(16) 0.007(16) 0.000(13) C7 0.056(10) 0.064(12) 0.101(16) 0.036(11) 0.017(10) 0.002(9) O11 0.052(6) 0.051(6) 0.053(6) 0.009(5) 0.003(5) -0.010(5) O12 0.046(6) 0.060(7) 0.071(8) 0.022(6) 0.006(6) -0.004(5) C11 0.037(8) 0.036(8) 0.116(16) 0.033(9) 0.006(9) 0.001(6) C12 0.06(2) 0.07(2) 0.041(17) 0.013(17) -0.002(16) 0.030(19) C13 0.07(2) 0.026(13) 0.08(3) 0.007(15) 0.04(2) -0.007(13) C14 0.07(3) 0.12(4) 0.09(3) -0.06(3) 0.03(2) -0.01(3) C15 0.05(2) 0.08(3) 0.10(3) -0.04(2) 0.02(2) -0.03(2) C16 0.06(2) 0.06(2) 0.08(3) -0.020(19) 0.019(19) -0.021(17) C17 0.050(19) 0.07(2) 0.07(2) -0.003(18) 0.021(17) 0.000(16) C12B 0.040(16) 0.044(18) 0.09(3) 0.02(2) 0.010(18) -0.006(14) C13B 0.05(2) 0.10(4) 0.06(2) 0.03(2) -0.003(19) -0.02(2) C14B 0.13(4) 0.05(2) 0.13(5) 0.01(3) -0.02(4) -0.06(3) C15B 0.11(4) 0.08(3) 0.28(10) 0.10(5) 0.09(5) 0.01(3) C16B 0.12(2) 0.13(2) 0.13(2) 0.002(10) 0.007(10) 0.001(10) C17B 0.12(4) 0.026(15) 0.19(6) 0.02(2) 0.10(4) 0.02(2) O21 0.037(5) 0.047(6) 0.057(7) 0.004(5) 0.002(5) 0.002(4) C21 0.025(9) 0.039(10) 0.079(17) 0.000 0.000 0.003(8) C22 0.042(11) 0.040(11) 0.089(19) 0.000 0.000 0.007(10) C23 0.070(12) 0.110(19) 0.088(15) 0.050(14) 0.020(11) 0.048(13) C24 0.048(11) 0.13(2) 0.108(19) 0.052(17) 0.006(11) 0.044(13) C25 0.042(13) 0.039(12) 0.15(3) 0.000 0.000 0.024(11) O31 0.051(6) 0.056(6) 0.039(5) -0.001(5) -0.001(5) -0.004(5) C31 0.043(10) 0.050(12) 0.034(10) -0.002(9) 0.000 0.000 C32 0.048(11) 0.063(14) 0.039(11) -0.002(10) 0.000 0.000 C33 0.051(11) 0.22(3) 0.045(11) 0.005(15) 0.008(8) -0.019(15) C34 0.073(14) 0.21(3) 0.039(10) 0.004(15) -0.006(10) -0.014(17) C35 0.074(19) 0.14(3) 0.040(13) -0.007(17) 0.000 0.000 N2 0.058(10) 0.064(11) 0.062(11) 0.000 0.000 0.000 C51 0.062(9) 0.052(9) 0.067(10) 0.000 0.000 0.012(8) C52 0.11(3) 0.040(13) 0.10(2) 0.000 0.000 -0.023(16) C53 0.11(3) 0.013(12) 0.08(3) 0.000 0.000 0.000 N1 0.040(12) 0.063(16) 0.035(12) -0.003(11) 0.000(10) 0.013(12) C41 0.040(15) 0.054(18) 0.056(19) 0.002(15) -0.005(14) 0.000(13) C42 0.045(18) 0.12(4) 0.06(2) -0.02(2) -0.002(17) 0.01(2) C43 0.038(18) 0.15(4) 0.05(2) -0.01(3) -0.032(16) 0.00(2) C44 0.08(3) 0.08(3) 0.046(19) 0.004(18) -0.003(18) 0.00(2) C45 0.053(18) 0.057(19) 0.045(17) -0.007(14) -0.007(14) 0.001(15) N3 0.052(13) 0.067(15) 0.11(2) 0.000 0.000 -0.009(12) C61 0.05(2) 0.10(3) 0.06(3) 0.001(19) -0.007(15) -0.03(2) C62 0.09(4) 0.07(3) 0.18(6) -0.01(4) -0.01(4) -0.03(3) N1B 0.118(19) 0.119(19) 0.118(19) -0.002(10) 0.005(10) -0.001(10) C41B 0.11(4) 0.12(4) 0.08(3) -0.02(3) 0.01(3) 0.00(4) C42B 0.11(5) 0.13(6) 0.14(7) 0.01(4) 0.02(4) 0.00(4) C43B 0.09(4) 0.14(6) 0.13(5) 0.00(4) -0.02(4) -0.04(4) C44B 0.10(4) 0.11(5) 0.18(7) -0.06(5) -0.02(5) 0.04(4) C45B 0.14(3) 0.14(3) 0.14(3) -0.001(10) -0.003(10) -0.001(10) _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 U1 O2U 2.228(8) . ? U1 O1U 2.254(7) . ? U1 O31 2.411(11) . ? U1 O21 2.429(10) . ? U1 O3U 2.430(9) . ? U1 O2 2.432(10) 10_557 ? U1 O4U 2.435(8) 3_656 ? U1 O12 2.461(12) 12_655 ? U1 N1 2.8015(12) . ? U1 U2 3.7999(9) . ? U1 U1 3.8128(10) 12_655 ? U1 U1 3.8357(10) 10_557 ? U2 O1U 2.190(14) 3_656 ? U2 O1U 2.190(14) . ? U2 O11 2.412(11) 3_656 ? U2 O11 2.412(11) . ? U2 O11 2.412(11) 12_655 ? U2 O11 2.413(11) 10_557 ? U2 O3U 2.431(13) 10_557 ? U2 O3U 2.431(13) . ? U2 U1 3.7999(9) 12_655 ? U2 U1 3.8000(9) 3_656 ? U2 U1 3.8000(9) 10_557 ? U3 O2U 2.255(15) . ? U3 O2U 2.255(15) 10_557 ? U3 O1 2.443(11) 3_656 ? U3 O1 2.443(11) 10_557 ? U3 O1 2.443(11) 12_655 ? U3 O1 2.443(11) . ? U3 O4U 2.454(13) . ? U3 O4U 2.454(13) 3_656 ? U3 N2 2.78(3) . ? U3 U1 3.8397(9) 12_655 ? U3 U1 3.8398(9) 3_656 ? O1U U1 2.254(7) 10_557 ? O2U U1 2.228(8) 12_655 ? O3U U1 2.430(9) 12_655 ? O4U U1 2.435(8) 12_655 ? O4U U1 2.435(8) 3_656 ? O1 C1 1.253(19) . ? O2 C1 1.25(2) . ? O2 U1 2.432(10) 10_557 ? C1 C2 1.51(2) . ? C2 C7 1.37(2) . ? C2 C3 1.39(2) . ? C3 C4 1.37(3) . ? C4 C5 1.33(3) . ? C5 C6 1.34(3) . ? C6 C7 1.41(3) . ? O11 C11 1.30(2) . ? O12 C11 1.23(2) . ? O12 U1 2.461(12) 12_655 ? C11 C12B 1.53(3) . ? C11 C12 1.63(5) . ? C12 C13 1.35(5) . ? C12 C17 1.37(5) . ? C13 C14 1.34(6) . ? C14 C15 1.36(5) . ? C15 C16 1.36(6) . ? C16 C17 1.30(5) . ? C12B C13B 1.30(5) . ? C12B C17B 1.48(5) . ? C13B C14B 1.3899 . ? C14B C15B 1.3902 . ? C15B C16B 1.3899 . ? C16B C17B 1.3899 . ? O21 C21 1.232(14) . ? C21 O21 1.232(14) 10_557 ? C21 C22 1.55(3) . ? C22 C23 1.36(3) . ? C22 C23 1.36(3) 10_557 ? C23 C24 1.40(3) . ? C24 C25 1.32(3) . ? C25 C24 1.32(3) 10_557 ? O31 C31 1.259(14) . ? C31 O31 1.259(14) 12_655 ? C31 C32 1.49(3) . ? C32 C33 1.32(2) . ? C32 C33 1.32(2) 12_655 ? C33 C34 1.38(3) . ? C34 C35 1.33(3) . ? C35 C34 1.33(3) 12_655 ? N2 C51 1.33(3) . ? N2 C51 1.33(3) 3_656 ? C51 C52 1.39(4) . ? C52 C53 1.36(3) . ? C53 C52 1.36(3) 3_656 ? N1 C45 1.3900 . ? N1 C41 1.3900 . ? C41 C42 1.3901 . ? C42 C43 1.3900 . ? C43 C44 1.3899 . ? C44 C45 1.3901 . ? N3 C61 1.06(4) 10_557 ? N3 C61 1.06(4) . ? C61 C61 0.87(8) 10_557 ? C61 C62 1.65(5) . ? C62 C62 1.98(5) 10_557 ? N1B C41B 1.3860 . ? N1B C45B 1.3873 . ? C41B C42B 1.3909 . ? C42B C43B 1.3882 . ? C42B C42B 1.54(5) 4_567 ? C43B C44B 1.3849 . ? C44B C45B 1.3899 . ? 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 O2U U1 O1U 88.7(5) . . ? O2U U1 O31 81.0(4) . . ? O1U U1 O31 141.4(4) . . ? O2U U1 O21 142.3(4) . . ? O1U U1 O21 79.6(4) . . ? O31 U1 O21 128.8(4) . . ? O2U U1 O3U 69.2(4) . . ? O1U U1 O3U 69.1(5) . . ? O31 U1 O3U 72.4(4) . . ? O21 U1 O3U 135.6(4) . . ? O2U U1 O2 84.0(4) . 10_557 ? O1U U1 O2 140.6(4) . 10_557 ? O31 U1 O2 75.5(4) . 10_557 ? O21 U1 O2 82.9(4) . 10_557 ? O3U U1 O2 140.6(4) . 10_557 ? O2U U1 O4U 69.3(5) . 3_656 ? O1U U1 O4U 69.5(4) . 3_656 ? O31 U1 O4U 137.4(4) . 3_656 ? O21 U1 O4U 73.0(4) . 3_656 ? O3U U1 O4U 120.7(4) . 3_656 ? O2 U1 O4U 71.7(4) 10_557 3_656 ? O2U U1 O12 140.4(4) . 12_655 ? O1U U1 O12 78.2(4) . 12_655 ? O31 U1 O12 86.3(4) . 12_655 ? O21 U1 O12 72.1(4) . 12_655 ? O3U U1 O12 71.2(4) . 12_655 ? O2 U1 O12 128.7(4) 10_557 12_655 ? O4U U1 O12 135.8(4) 3_656 12_655 ? O2U U1 N1 138.0(4) . . ? O1U U1 N1 133.0(4) . . ? O31 U1 N1 63.2(3) . . ? O21 U1 N1 65.6(3) . . ? O3U U1 N1 115.5(4) . . ? O2 U1 N1 67.0(4) 10_557 . ? O4U U1 N1 123.8(3) 3_656 . ? O12 U1 N1 61.9(4) 12_655 . ? O2U U1 U2 80.5(3) . . ? O1U U1 U2 30.7(3) . . ? O31 U1 U2 110.6(3) . . ? O21 U1 U2 104.1(3) . . ? O3U U1 U2 38.6(3) . . ? O2 U1 U2 162.0(2) 10_557 . ? O4U U1 U2 94.3(3) 3_656 . ? O12 U1 U2 69.2(3) 12_655 . ? N1 U1 U2 130.9(3) . . ? O2U U1 U1 31.2(3) . 12_655 ? O1U U1 U1 81.1(3) . 12_655 ? O31 U1 U1 70.9(3) . 12_655 ? O21 U1 U1 160.0(3) . 12_655 ? O3U U1 U1 38.3(3) . 12_655 ? O2 U1 U1 109.0(2) 10_557 12_655 ? O4U U1 U1 95.0(3) 3_656 12_655 ? O12 U1 U1 109.3(3) 12_655 12_655 ? N1 U1 U1 133.49(2) . 12_655 ? U2 U1 U1 59.888(10) . 12_655 ? O2U U1 U1 80.7(4) . 10_557 ? O1U U1 U1 31.7(3) . 10_557 ? O31 U1 U1 160.6(3) . 10_557 ? O21 U1 U1 70.6(3) . 10_557 ? O3U U1 U1 94.9(3) . 10_557 ? O2 U1 U1 108.9(2) 10_557 10_557 ? O4U U1 U1 38.0(2) 3_656 10_557 ? O12 U1 U1 103.8(3) 12_655 10_557 ? N1 U1 U1 136.17(3) . 10_557 ? U2 U1 U1 59.690(10) . 10_557 ? U1 U1 U1 90.0 12_655 10_557 ? O1U U2 O1U 90.8(7) 3_656 . ? O1U U2 O11 143.0(3) 3_656 3_656 ? O1U U2 O11 83.9(4) . 3_656 ? O1U U2 O11 83.9(4) 3_656 . ? O1U U2 O11 143.0(3) . . ? O11 U2 O11 121.0(6) 3_656 . ? O1U U2 O11 143.0(3) 3_656 12_655 ? O1U U2 O11 83.9(4) . 12_655 ? O11 U2 O11 73.0(6) 3_656 12_655 ? O11 U2 O11 79.0(6) . 12_655 ? O1U U2 O11 83.9(4) 3_656 10_557 ? O1U U2 O11 143.0(3) . 10_557 ? O11 U2 O11 79.0(6) 3_656 10_557 ? O11 U2 O11 73.0(6) . 10_557 ? O11 U2 O11 121.0(6) 12_655 10_557 ? O1U U2 O3U 70.1(2) 3_656 10_557 ? O1U U2 O3U 70.1(3) . 10_557 ? O11 U2 O3U 73.6(4) 3_656 10_557 ? O11 U2 O3U 139.3(3) . 10_557 ? O11 U2 O3U 139.3(3) 12_655 10_557 ? O11 U2 O3U 73.6(4) 10_557 10_557 ? O1U U2 O3U 70.1(2) 3_656 . ? O1U U2 O3U 70.1(3) . . ? O11 U2 O3U 139.3(3) 3_656 . ? O11 U2 O3U 73.6(4) . . ? O11 U2 O3U 73.6(4) 12_655 . ? O11 U2 O3U 139.3(3) 10_557 . ? O3U U2 O3U 122.1(7) 10_557 . ? O1U U2 U1 82.2(3) 3_656 . ? O1U U2 U1 31.73(10) . . ? O11 U2 U1 109.1(3) 3_656 . ? O11 U2 U1 111.4(3) . . ? O11 U2 U1 74.1(3) 12_655 . ? O11 U2 U1 164.8(3) 10_557 . ? O3U U2 U1 95.8(3) 10_557 . ? O3U U2 U1 38.6(2) . . ? O1U U2 U1 31.73(10) 3_656 12_655 ? O1U U2 U1 82.2(3) . 12_655 ? O11 U2 U1 164.8(3) 3_656 12_655 ? O11 U2 U1 74.1(3) . 12_655 ? O11 U2 U1 111.4(3) 12_655 12_655 ? O11 U2 U1 109.1(3) 10_557 12_655 ? O3U U2 U1 95.8(3) 10_557 12_655 ? O3U U2 U1 38.6(2) . 12_655 ? U1 U2 U1 60.22(2) . 12_655 ? O1U U2 U1 31.72(10) 3_656 3_656 ? O1U U2 U1 82.2(3) . 3_656 ? O11 U2 U1 111.4(3) 3_656 3_656 ? O11 U2 U1 109.1(3) . 3_656 ? O11 U2 U1 164.8(3) 12_655 3_656 ? O11 U2 U1 74.1(3) 10_557 3_656 ? O3U U2 U1 38.6(2) 10_557 3_656 ? O3U U2 U1 95.8(3) . 3_656 ? U1 U2 U1 90.74(3) . 3_656 ? U1 U2 U1 60.62(2) 12_655 3_656 ? O1U U2 U1 82.2(3) 3_656 10_557 ? O1U U2 U1 31.73(10) . 10_557 ? O11 U2 U1 74.1(3) 3_656 10_557 ? O11 U2 U1 164.8(3) . 10_557 ? O11 U2 U1 109.1(3) 12_655 10_557 ? O11 U2 U1 111.4(3) 10_557 10_557 ? O3U U2 U1 38.6(2) 10_557 10_557 ? O3U U2 U1 95.8(3) . 10_557 ? U1 U2 U1 60.62(2) . 10_557 ? U1 U2 U1 90.74(3) 12_655 10_557 ? U1 U2 U1 60.22(2) 3_656 10_557 ? O2U U3 O2U 87.4(7) . 10_557 ? O2U U3 O1 80.2(4) . 3_656 ? O2U U3 O1 139.8(3) 10_557 3_656 ? O2U U3 O1 80.2(4) . 10_557 ? O2U U3 O1 139.8(3) 10_557 10_557 ? O1 U3 O1 75.4(5) 3_656 10_557 ? O2U U3 O1 139.8(3) . 12_655 ? O2U U3 O1 80.2(4) 10_557 12_655 ? O1 U3 O1 85.2(6) 3_656 12_655 ? O1 U3 O1 131.6(5) 10_557 12_655 ? O2U U3 O1 139.8(3) . . ? O2U U3 O1 80.2(4) 10_557 . ? O1 U3 O1 131.6(5) 3_656 . ? O1 U3 O1 85.2(6) 10_557 . ? O1 U3 O1 75.4(5) 12_655 . ? O2U U3 O4U 68.5(2) . . ? O2U U3 O4U 68.5(2) 10_557 . ? O1 U3 O4U 71.3(3) 3_656 . ? O1 U3 O4U 137.3(3) 10_557 . ? O1 U3 O4U 71.3(3) 12_655 . ? O1 U3 O4U 137.3(3) . . ? O2U U3 O4U 68.5(2) . 3_656 ? O2U U3 O4U 68.5(2) 10_557 3_656 ? O1 U3 O4U 137.3(3) 3_656 3_656 ? O1 U3 O4U 71.3(3) 10_557 3_656 ? O1 U3 O4U 137.3(3) 12_655 3_656 ? O1 U3 O4U 71.3(3) . 3_656 ? O4U U3 O4U 119.2(6) . 3_656 ? O2U U3 N2 136.3(3) . . ? O2U U3 N2 136.3(3) 10_557 . ? O1 U3 N2 65.8(3) 3_656 . ? O1 U3 N2 65.8(3) 10_557 . ? O1 U3 N2 65.8(3) 12_655 . ? O1 U3 N2 65.8(3) . . ? O4U U3 N2 120.4(3) . . ? O4U U3 N2 120.4(3) 3_656 . ? O2U U3 U1 30.86(9) . 12_655 ? O2U U3 U1 80.3(3) 10_557 12_655 ? O1 U3 U1 69.5(3) 3_656 12_655 ? O1 U3 U1 104.9(3) 10_557 12_655 ? O1 U3 U1 109.0(3) 12_655 12_655 ? O1 U3 U1 158.8(3) . 12_655 ? O4U U3 U1 38.06(18) . 12_655 ? O4U U3 U1 94.0(3) 3_656 12_655 ? N2 U3 U1 135.231(14) . 12_655 ? O2U U3 U1 30.86(9) . . ? O2U U3 U1 80.3(3) 10_557 . ? O1 U3 U1 104.9(3) 3_656 . ? O1 U3 U1 69.5(3) 10_557 . ? O1 U3 U1 158.8(3) 12_655 . ? O1 U3 U1 109.0(3) . . ? O4U U3 U1 94.0(3) . . ? O4U U3 U1 38.06(18) 3_656 . ? N2 U3 U1 135.231(14) . . ? U1 U3 U1 59.54(2) 12_655 . ? O2U U3 U1 80.3(3) . 3_656 ? O2U U3 U1 30.87(9) 10_557 3_656 ? O1 U3 U1 109.0(3) 3_656 3_656 ? O1 U3 U1 158.9(3) 10_557 3_656 ? O1 U3 U1 69.5(3) 12_655 3_656 ? O1 U3 U1 104.9(3) . 3_656 ? O4U U3 U1 38.06(18) . 3_656 ? O4U U3 U1 94.0(3) 3_656 3_656 ? N2 U3 U1 135.230(14) . 3_656 ? U1 U3 U1 59.93(2) 12_655 3_656 ? U1 U3 U1 89.54(3) . 3_656 ? U2 O1U U1 117.5(4) . . ? U2 O1U U1 117.5(4) . 10_557 ? U1 O1U U1 116.6(6) . 10_557 ? U1 O2U U1 117.7(7) 12_655 . ? U1 O2U U3 117.9(4) 12_655 . ? U1 O2U U3 117.9(4) . . ? U1 O3U U1 103.4(5) . 12_655 ? U1 O3U U2 102.8(4) . . ? U1 O3U U2 102.8(4) 12_655 . ? U1 O4U U1 103.9(5) 12_655 3_656 ? U1 O4U U3 103.5(4) 12_655 . ? U1 O4U U3 103.5(4) 3_656 . ? C1 O1 U3 137.5(11) . . ? C1 O2 U1 133.6(10) . 10_557 ? O2 C1 O1 127.0(15) . . ? O2 C1 C2 116.4(13) . . ? O1 C1 C2 116.6(16) . . ? C7 C2 C3 118.3(17) . . ? C7 C2 C1 120.2(16) . . ? C3 C2 C1 121.5(16) . . ? C4 C3 C2 120(2) . . ? C5 C4 C3 122(2) . . ? C4 C5 C6 119(2) . . ? C5 C6 C7 121(2) . . ? C2 C7 C6 120(2) . . ? C11 O11 U2 129.9(10) . . ? C11 O12 U1 137.7(12) . 12_655 ? O12 C11 O11 127.9(15) . . ? O12 C11 C12B 115(2) . . ? O11 C11 C12B 116(2) . . ? O12 C11 C12 122.6(18) . . ? O11 C11 C12 105.0(19) . . ? C12B C11 C12 34.5(19) . . ? C13 C12 C17 118(4) . . ? C13 C12 C11 125(3) . . ? C17 C12 C11 116(3) . . ? C14 C13 C12 121(4) . . ? C13 C14 C15 121(4) . . ? C16 C15 C14 115(4) . . ? C17 C16 C15 125(4) . . ? C16 C17 C12 119(4) . . ? C13B C12B C17B 120(3) . . ? C13B C12B C11 120(3) . . ? C17B C12B C11 120(3) . . ? C12B C13B C14B 122(2) . . ? C13B C14B C15B 120.0 . . ? C16B C15B C14B 120.0 . . ? C17B C16B C15B 120.0 . . ? C16B C17B C12B 117.7(15) . . ? C21 O21 U1 133.7(11) . . ? O21 C21 O21 129(2) . 10_557 ? O21 C21 C22 115.6(10) . . ? O21 C21 C22 115.6(10) 10_557 . ? C23 C22 C23 119(2) . 10_557 ? C23 C22 C21 120.2(12) . . ? C23 C22 C21 120.3(12) 10_557 . ? C22 C23 C24 120(2) . . ? C25 C24 C23 118(2) . . ? C24 C25 C24 124(3) . 10_557 ? C31 O31 U1 136.4(11) . . ? O31 C31 O31 125.1(19) . 12_655 ? O31 C31 C32 117.5(10) . . ? O31 C31 C32 117.5(10) 12_655 . ? C33 C32 C33 116(2) . 12_655 ? C33 C32 C31 121.9(12) . . ? C33 C32 C31 121.9(12) 12_655 . ? C32 C33 C34 123(2) . . ? C35 C34 C33 119(2) . . ? C34 C35 C34 119(3) . 12_655 ? C51 N2 C51 108(3) . 3_656 ? C51 N2 U3 126.0(17) . . ? C51 N2 U3 126.0(17) 3_656 . ? N2 C51 C52 130(3) . . ? C53 C52 C51 118(3) . . ? C52 C53 C52 117(3) 3_656 . ? C45 N1 C41 120.0 . . ? C45 N1 U1 119.7(2) . . ? C41 N1 U1 119.60(17) . . ? N1 C41 C42 120.0 . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? N1 C45 C44 120.0 . . ? C61 N3 C61 48(4) 10_557 . ? C61 C61 N3 66(2) 10_557 . ? C61 C61 C62 109.7(16) 10_557 . ? N3 C61 C62 170(5) . . ? C61 C62 C62 70.3(16) . 10_557 ? C41B N1B C45B 119.7 . . ? N1B C41B C42B 120.0 . . ? C43B C42B C41B 120.1 . . ? C43B C42B C42B 144.5(9) . 4_567 ? C41B C42B C42B 94.7(12) . 4_567 ? C44B C43B C42B 119.9 . . ? C43B C44B C45B 120.0 . . ? N1B C45B C44B 120.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 5.447 _refine_diff_density_min -5.634 _refine_diff_density_rms 0.403