# 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 'Paula L Diaconescu' _publ_contact_author_email PLD@CHEM.UCLA.EDU _publ_section_title ; In situ generation of uranium alkyl complexes ; loop_ _publ_author_name 'Paula L Diaconescu' 'Selma Duhoviscu' # Attachment 'uranium_insitu_cif.txt' data_1py2-U _database_code_depnum_ccdc_archive 'CCDC 756840' #TrackingRef 'uranium_insitu_cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H82 N6 U, 0.8(C6 H14)' _chemical_formula_sum 'C66.80 H93.20 N6 U' _chemical_formula_weight 1218.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.828(2) _cell_length_b 22.158(2) _cell_length_c 14.7466(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.9640(10) _cell_angle_gamma 90.00 _cell_volume 6127.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 29.81 _exptl_crystal_description block _exptl_crystal_colour gold _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 2.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7464 _exptl_absorpt_correction_T_max 0.8772 _exptl_absorpt_process_details 'Sadabs (Bruker)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30421 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 30.79 _reflns_number_total 9049 _reflns_number_gt 8262 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+5.0346P] 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 9049 _refine_ls_number_parameters 336 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.5000 0.675365(5) 0.7500 0.01147(4) Uani 1 2 d S . . N2 N 0.59232(9) 0.63164(8) 0.89549(12) 0.0137(3) Uani 1 1 d . . . N3 N 0.60553(10) 0.73282(8) 0.80826(13) 0.0172(3) Uani 1 1 d . . . N1 N 0.54629(9) 0.60551(8) 0.66850(13) 0.0167(3) Uani 1 1 d . . . C8 C 0.66093(12) 0.81611(10) 0.74211(17) 0.0205(4) Uani 1 1 d . . . C7 C 0.61718(11) 0.79589(10) 0.79524(16) 0.0175(4) Uani 1 1 d . . . C1 C 0.65839(11) 0.65463(10) 0.92923(15) 0.0157(4) Uani 1 1 d . . . C12 C 0.58692(12) 0.83893(10) 0.84220(16) 0.0193(4) Uani 1 1 d . . . C5 C 0.57679(11) 0.57962(10) 0.93206(15) 0.0156(4) Uani 1 1 d . . . C2 C 0.71008(12) 0.62898(10) 1.00751(16) 0.0195(4) Uani 1 1 d . . . H2A H 0.7554 0.6476 1.0344 0.023 Uiso 1 1 calc R . . C9 C 0.67116(13) 0.87837(11) 0.73458(17) 0.0234(5) Uani 1 1 d . . . H9A H 0.7008 0.8921 0.6996 0.028 Uiso 1 1 calc R . . C4 C 0.62724(12) 0.54965(11) 1.00586(16) 0.0202(4) Uani 1 1 d . . . H4A H 0.6163 0.5121 1.0289 0.024 Uiso 1 1 calc R . . C6 C 0.67215(12) 0.70511(10) 0.86995(17) 0.0199(4) Uani 1 1 d . . . H6A H 0.7016 0.7363 0.9129 0.024 Uiso 1 1 calc R . . H6B H 0.6994 0.6894 0.8294 0.024 Uiso 1 1 calc R . . C3 C 0.69408(12) 0.57555(11) 1.04547(16) 0.0211(4) Uani 1 1 d . . . H3A H 0.7287 0.5569 1.0983 0.025 Uiso 1 1 calc R . . C10 C 0.63930(13) 0.91997(11) 0.77657(18) 0.0253(5) Uani 1 1 d . . . H10A H 0.6459 0.9619 0.7691 0.030 Uiso 1 1 calc R . . C11 C 0.59739(13) 0.90021(11) 0.83006(17) 0.0239(5) Uani 1 1 d . . . H11A H 0.5754 0.9291 0.8590 0.029 Uiso 1 1 calc RD . . C13 C 0.55001(13) 0.81951(10) 0.91361(17) 0.0211(4) Uani 1 1 d . . . H13A H 0.5188 0.7841 0.8858 0.025 Uiso 1 1 calc R . . C16 C 0.69960(13) 0.77337(12) 0.69509(18) 0.0250(5) Uani 1 1 d . . . H16A H 0.6767 0.7327 0.6892 0.030 Uiso 1 1 calc R . . C14 C 0.60581(13) 0.79920(12) 1.00750(18) 0.0260(5) Uani 1 1 d . . . H14A H 0.6308 0.7635 0.9955 0.039 Uiso 1 1 calc R . . H14B H 0.5821 0.7893 1.0545 0.039 Uiso 1 1 calc R . . H14C H 0.6402 0.8318 1.0325 0.039 Uiso 1 1 calc R . . C15 C 0.50361(14) 0.86843(12) 0.93556(19) 0.0287(5) Uani 1 1 d . . . H15A H 0.4708 0.8844 0.8754 0.043 Uiso 1 1 calc R . . H15B H 0.5340 0.9011 0.9715 0.043 Uiso 1 1 calc R . . H15C H 0.4762 0.8513 0.9739 0.043 Uiso 1 1 calc R . . C17 C 0.77885(14) 0.76712(14) 0.7560(2) 0.0338(6) Uani 1 1 d . . . H17A H 0.7826 0.7554 0.8215 0.051 Uiso 1 1 calc R . . H17B H 0.8031 0.8058 0.7573 0.051 Uiso 1 1 calc R . . H17C H 0.8013 0.7362 0.7278 0.051 Uiso 1 1 calc R . . C18 C 0.69686(16) 0.79460(14) 0.5941(2) 0.0350(6) Uani 1 1 d . . . H18A H 0.6477 0.8050 0.5565 0.052 Uiso 1 1 calc R . . H18B H 0.7138 0.7621 0.5619 0.052 Uiso 1 1 calc R . . H18C H 0.7274 0.8302 0.5999 0.052 Uiso 1 1 calc R . . C19 C 0.60776(12) 0.60673(10) 0.63632(16) 0.0191(4) Uani 1 1 d . . . C27 C 0.68093(12) 0.54476(12) 0.78315(17) 0.0238(5) Uani 1 1 d . . . H27A H 0.6518 0.5664 0.8170 0.029 Uiso 1 1 calc R . . C25 C 0.53225(13) 0.65810(11) 0.47871(18) 0.0241(5) Uani 1 1 d . . . H25A H 0.4976 0.6610 0.5150 0.029 Uiso 1 1 calc R . . C24 C 0.60197(13) 0.63265(11) 0.54644(18) 0.0226(5) Uani 1 1 d . . . C20 C 0.67299(12) 0.57907(11) 0.69097(17) 0.0222(5) Uani 1 1 d . . . C21 C 0.73056(13) 0.58093(13) 0.6559(2) 0.0308(6) Uani 1 1 d . . . H21A H 0.7748 0.5638 0.6932 0.037 Uiso 1 1 calc R . . C23 C 0.66115(15) 0.63218(12) 0.5145(2) 0.0314(6) Uani 1 1 d . . . H23A H 0.6572 0.6496 0.4542 0.038 Uiso 1 1 calc R . . C28 C 0.75766(14) 0.54169(14) 0.8525(2) 0.0347(6) Uani 1 1 d . . . H28A H 0.7775 0.5825 0.8645 0.052 Uiso 1 1 calc R . . H28B H 0.7867 0.5171 0.8241 0.052 Uiso 1 1 calc R . . H28C H 0.7578 0.5235 0.9131 0.052 Uiso 1 1 calc R . . C26 C 0.54010(16) 0.72089(13) 0.4406(2) 0.0365(6) Uani 1 1 d . . . H26A H 0.4951 0.7327 0.3921 0.055 Uiso 1 1 calc R . . H26B H 0.5782 0.7203 0.4117 0.055 Uiso 1 1 calc R . . H26C H 0.5521 0.7500 0.4935 0.055 Uiso 1 1 calc R . . C22 C 0.72490(15) 0.60699(13) 0.5687(2) 0.0359(6) Uani 1 1 d . . . H22A H 0.7647 0.6075 0.5463 0.043 Uiso 1 1 calc R . . C29 C 0.49697(11) 0.55680(10) 0.61953(16) 0.0175(4) Uani 1 1 d . . . H29A H 0.4946 0.5263 0.6675 0.021 Uiso 1 1 calc R . . H29B H 0.5159 0.5367 0.5729 0.021 Uiso 1 1 calc R . . C30 C 0.65142(14) 0.48022(12) 0.76323(18) 0.0280(5) Uani 1 1 d . . . H30A H 0.6018 0.4816 0.7207 0.042 Uiso 1 1 calc R . . H30B H 0.6535 0.4608 0.8238 0.042 Uiso 1 1 calc R . . H30C H 0.6801 0.4571 0.7325 0.042 Uiso 1 1 calc R . . C31 C 0.50027(16) 0.61595(13) 0.39316(19) 0.0348(6) Uani 1 1 d . . . H31A H 0.4923 0.5760 0.4164 0.052 Uiso 1 1 calc R . . H31B H 0.5333 0.6124 0.3563 0.052 Uiso 1 1 calc R . . H31C H 0.4548 0.6325 0.3520 0.052 Uiso 1 1 calc R . . C1S C 0.5956(6) 1.0538(4) 0.9541(7) 0.158(3) Uiso 0.80 1 d PD . . H1S1 H 0.5944 1.0100 0.9444 0.237 Uiso 0.40 1 calc PRD A 1 H1S2 H 0.5613 1.0650 0.9863 0.237 Uiso 0.40 1 calc PR A 1 H1S3 H 0.6436 1.0661 0.9937 0.237 Uiso 0.40 1 calc PR A 1 H1S4 H 0.6206 1.0153 0.9573 0.237 Uiso 0.40 1 calc PR A 2 H1S5 H 0.5805 1.0581 1.0108 0.237 Uiso 0.40 1 calc PR A 2 H1S6 H 0.6276 1.0871 0.9520 0.237 Uiso 0.40 1 calc PR A 2 C2S C 0.5764(9) 1.0849(9) 0.8592(10) 0.158(3) Uiso 0.40 1 d PD B 1 H2S1 H 0.6097 1.0727 0.8250 0.189 Uiso 0.40 1 calc PR B 1 H2S2 H 0.5797 1.1292 0.8685 0.189 Uiso 0.40 1 calc PR B 1 C3S C 0.5012(6) 1.0674(11) 0.8015(4) 0.158(3) Uiso 0.40 1 d PD . 1 H3S1 H 0.4896 1.0268 0.8205 0.189 Uiso 0.40 1 calc PR . 1 H3S2 H 0.4667 1.0968 0.8114 0.189 Uiso 0.40 1 calc PR . 1 C4S C 0.5312(9) 1.0551(9) 0.8652(12) 0.158(3) Uiso 0.40 1 d PD B 2 H4S1 H 0.4884 1.0625 0.8842 0.189 Uiso 0.40 1 calc PR B 2 H4S2 H 0.5257 1.0150 0.8342 0.189 Uiso 0.40 1 calc PR B 2 C5S C 0.5342(6) 1.1022(9) 0.7931(7) 0.158(3) Uiso 0.40 1 d PD . 2 H5S1 H 0.5755 1.0941 0.7712 0.189 Uiso 0.40 1 calc PR . 2 H5S2 H 0.5410 1.1425 0.8238 0.189 Uiso 0.40 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 0.01062(5) 0.01267(5) 0.01120(5) 0.000 0.00365(3) 0.000 N2 0.0133(8) 0.0158(8) 0.0121(8) 0.0000(6) 0.0043(6) -0.0010(6) N3 0.0133(8) 0.0169(8) 0.0200(9) 0.0031(7) 0.0036(7) -0.0019(7) N1 0.0127(8) 0.0203(9) 0.0172(8) -0.0037(7) 0.0050(7) 0.0013(7) C8 0.0144(10) 0.0237(11) 0.0205(11) 0.0034(8) 0.0018(8) -0.0026(8) C7 0.0134(9) 0.0176(10) 0.0182(10) 0.0033(8) 0.0004(7) -0.0031(8) C1 0.0140(9) 0.0166(9) 0.0159(10) -0.0009(8) 0.0040(7) -0.0016(8) C12 0.0143(10) 0.0199(10) 0.0199(11) 0.0019(8) 0.0003(8) -0.0026(8) C5 0.0148(9) 0.0180(10) 0.0143(9) 0.0004(8) 0.0050(7) -0.0014(8) C2 0.0141(9) 0.0231(11) 0.0186(10) -0.0004(8) 0.0018(8) -0.0021(8) C9 0.0199(11) 0.0239(11) 0.0235(11) 0.0053(9) 0.0031(9) -0.0072(9) C4 0.0184(10) 0.0224(10) 0.0184(10) 0.0052(8) 0.0042(8) -0.0027(8) C6 0.0146(10) 0.0199(10) 0.0240(11) 0.0040(9) 0.0043(8) -0.0021(8) C3 0.0176(10) 0.0273(11) 0.0157(10) 0.0043(9) 0.0018(8) 0.0015(9) C10 0.0241(12) 0.0184(11) 0.0278(12) 0.0041(9) 0.0008(9) -0.0054(9) C11 0.0229(11) 0.0199(11) 0.0250(12) 0.0007(9) 0.0024(9) -0.0011(9) C13 0.0172(10) 0.0231(11) 0.0219(11) 0.0001(9) 0.0047(8) -0.0021(8) C16 0.0218(11) 0.0269(12) 0.0280(12) 0.0048(10) 0.0104(9) -0.0020(9) C14 0.0228(12) 0.0327(13) 0.0225(12) 0.0029(10) 0.0072(9) 0.0011(10) C15 0.0229(12) 0.0319(13) 0.0309(13) -0.0013(10) 0.0082(10) 0.0022(10) C17 0.0214(12) 0.0403(15) 0.0419(16) 0.0128(12) 0.0132(11) 0.0007(11) C18 0.0387(15) 0.0416(16) 0.0289(14) 0.0045(12) 0.0171(12) -0.0018(13) C19 0.0152(10) 0.0205(10) 0.0230(11) -0.0047(8) 0.0080(8) 0.0009(8) C27 0.0182(11) 0.0317(12) 0.0205(11) -0.0049(9) 0.0049(8) 0.0079(9) C25 0.0246(12) 0.0238(11) 0.0269(12) 0.0026(9) 0.0128(10) 0.0041(9) C24 0.0215(11) 0.0207(11) 0.0280(12) -0.0003(9) 0.0114(9) 0.0026(9) C20 0.0173(10) 0.0245(11) 0.0242(11) -0.0052(9) 0.0060(9) 0.0030(9) C21 0.0176(11) 0.0341(14) 0.0425(15) 0.0010(12) 0.0124(10) 0.0070(10) C23 0.0299(13) 0.0325(14) 0.0389(15) 0.0077(11) 0.0208(11) 0.0072(11) C28 0.0214(12) 0.0499(17) 0.0283(13) -0.0080(12) 0.0019(10) 0.0113(11) C26 0.0349(15) 0.0274(13) 0.0512(18) 0.0085(12) 0.0195(13) 0.0053(11) C22 0.0252(13) 0.0398(16) 0.0507(17) 0.0074(13) 0.0235(12) 0.0086(11) C29 0.0160(10) 0.0171(10) 0.0181(10) -0.0036(8) 0.0035(8) 0.0034(8) C30 0.0305(13) 0.0281(12) 0.0225(12) 0.0014(10) 0.0047(9) 0.0066(10) C31 0.0409(16) 0.0364(15) 0.0237(13) 0.0016(11) 0.0058(11) 0.0064(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 2.3238(18) . ? U1 N1 2.3238(18) 2_656 ? U1 N3 2.3599(18) . ? U1 N3 2.3599(18) 2_656 ? U1 N2 2.5179(17) 2_656 ? U1 N2 2.5179(17) . ? N2 C1 1.341(3) . ? N2 C5 1.350(3) . ? N3 C7 1.439(3) . ? N3 C6 1.473(3) . ? N1 C19 1.445(3) . ? N1 C29 1.478(3) . ? C8 C9 1.404(3) . ? C8 C7 1.417(3) . ? C8 C16 1.520(4) . ? C7 C12 1.421(3) . ? C1 C2 1.392(3) . ? C1 C6 1.498(3) . ? C12 C11 1.394(3) . ? C12 C13 1.527(3) . ? C5 C4 1.385(3) . ? C5 C29 1.500(3) 2_656 ? C2 C3 1.390(3) . ? C2 H2A 0.9500 . ? C9 C10 1.374(4) . ? C9 H9A 0.9500 . ? C4 C3 1.387(3) . ? C4 H4A 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C3 H3A 0.9500 . ? C10 C11 1.389(4) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C13 C15 1.523(3) . ? C13 C14 1.532(3) . ? C13 H13A 1.0000 . ? C16 C17 1.542(4) . ? C16 C18 1.546(4) . ? C16 H16A 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.415(3) . ? C19 C20 1.421(3) . ? C27 C20 1.520(3) . ? C27 C28 1.534(3) . ? C27 C30 1.537(4) . ? C27 H27A 1.0000 . ? C25 C24 1.526(3) . ? C25 C26 1.527(4) . ? C25 C31 1.532(4) . ? C25 H25A 1.0000 . ? C24 C23 1.399(3) . ? C20 C21 1.398(3) . ? C21 C22 1.381(4) . ? C21 H21A 0.9500 . ? C23 C22 1.375(4) . ? C23 H23A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C22 H22A 0.9500 . ? C29 C5 1.500(3) 2_656 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C1S C2S 1.493(9) . ? C1S C4S 1.503(9) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C1S H1S4 0.9800 . ? C1S H1S5 0.9800 . ? C1S H1S6 0.9800 . ? C2S C3S 1.507(10) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C3S 1.505(10) 2_656 ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.504(10) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S C5S 1.529(10) 2_656 ? C5S H5S1 0.9900 . ? C5S H5S2 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 N1 U1 N1 96.46(9) . 2_656 ? N1 U1 N3 95.46(6) . . ? N1 U1 N3 128.58(6) 2_656 . ? N1 U1 N3 128.58(6) . 2_656 ? N1 U1 N3 95.46(6) 2_656 2_656 ? N3 U1 N3 114.70(9) . 2_656 ? N1 U1 N2 66.61(6) . 2_656 ? N1 U1 N2 83.36(6) 2_656 2_656 ? N3 U1 N2 146.19(6) . 2_656 ? N3 U1 N2 65.44(6) 2_656 2_656 ? N1 U1 N2 83.36(6) . . ? N1 U1 N2 66.61(6) 2_656 . ? N3 U1 N2 65.44(6) . . ? N3 U1 N2 146.19(6) 2_656 . ? N2 U1 N2 134.74(8) 2_656 . ? C1 N2 C5 119.88(18) . . ? C1 N2 U1 121.46(14) . . ? C5 N2 U1 118.16(13) . . ? C7 N3 C6 109.68(17) . . ? C7 N3 U1 129.56(13) . . ? C6 N3 U1 120.74(13) . . ? C19 N1 C29 110.38(17) . . ? C19 N1 U1 132.41(14) . . ? C29 N1 U1 115.43(13) . . ? C9 C8 C7 119.0(2) . . ? C9 C8 C16 118.0(2) . . ? C7 C8 C16 123.0(2) . . ? C8 C7 C12 119.2(2) . . ? C8 C7 N3 122.3(2) . . ? C12 C7 N3 118.4(2) . . ? N2 C1 C2 121.3(2) . . ? N2 C1 C6 114.09(18) . . ? C2 C1 C6 124.34(19) . . ? C11 C12 C7 119.1(2) . . ? C11 C12 C13 119.2(2) . . ? C7 C12 C13 121.3(2) . . ? N2 C5 C4 121.5(2) . . ? N2 C5 C29 113.37(18) . 2_656 ? C4 C5 C29 124.96(19) . 2_656 ? C3 C2 C1 118.6(2) . . ? C3 C2 H2A 120.7 . . ? C1 C2 H2A 120.7 . . ? C10 C9 C8 121.6(2) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C5 C4 C3 118.7(2) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N3 C6 C1 112.02(18) . . ? N3 C6 H6A 109.2 . . ? C1 C6 H6A 109.2 . . ? N3 C6 H6B 109.2 . . ? C1 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C4 C3 C2 119.7(2) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C9 C10 C11 119.5(2) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C10 C11 C12 121.4(2) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C15 C13 C12 113.8(2) . . ? C15 C13 C14 109.0(2) . . ? C12 C13 C14 109.80(19) . . ? C15 C13 H13A 108.0 . . ? C12 C13 H13A 108.0 . . ? C14 C13 H13A 108.0 . . ? C8 C16 C17 111.1(2) . . ? C8 C16 C18 112.6(2) . . ? C17 C16 C18 107.4(2) . . ? C8 C16 H16A 108.5 . . ? C17 C16 H16A 108.5 . . ? C18 C16 H16A 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 119.2(2) . . ? C24 C19 N1 119.7(2) . . ? C20 C19 N1 121.0(2) . . ? C20 C27 C28 114.2(2) . . ? C20 C27 C30 111.85(19) . . ? C28 C27 C30 108.6(2) . . ? C20 C27 H27A 107.3 . . ? C28 C27 H27A 107.3 . . ? C30 C27 H27A 107.3 . . ? C24 C25 C26 113.5(2) . . ? C24 C25 C31 111.0(2) . . ? C26 C25 C31 108.5(2) . . ? C24 C25 H25A 107.9 . . ? C26 C25 H25A 107.9 . . ? C31 C25 H25A 107.9 . . ? C23 C24 C19 119.4(2) . . ? C23 C24 C25 117.6(2) . . ? C19 C24 C25 122.9(2) . . ? C21 C20 C19 118.6(2) . . ? C21 C20 C27 119.0(2) . . ? C19 C20 C27 122.2(2) . . ? C22 C21 C20 121.8(2) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C22 C23 C24 121.4(3) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C22 C21 119.5(2) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? N1 C29 C5 112.51(17) . 2_656 ? N1 C29 H29A 109.1 . . ? C5 C29 H29A 109.1 2_656 . ? N1 C29 H29B 109.1 . . ? C5 C29 H29B 109.1 2_656 . ? H29A C29 H29B 107.8 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C2S C1S H1S1 109.5 . . ? C4S C1S H1S1 85.4 . . ? C2S C1S H1S2 109.5 . . ? C4S C1S H1S2 83.8 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? C4S C1S H1S3 154.1 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C2S C1S H1S4 114.7 . . ? C4S C1S H1S4 109.5 . . ? H1S2 C1S H1S4 128.0 . . ? H1S3 C1S H1S4 80.4 . . ? C2S C1S H1S5 134.3 . . ? C4S C1S H1S5 109.5 . . ? H1S1 C1S H1S5 102.8 . . ? H1S3 C1S H1S5 88.3 . . ? H1S4 C1S H1S5 109.5 . . ? C2S C1S H1S6 66.1 . . ? C4S C1S H1S6 109.5 . . ? H1S1 C1S H1S6 136.5 . . ? H1S2 C1S H1S6 112.6 . . ? H1S4 C1S H1S6 109.5 . . ? H1S5 C1S H1S6 109.5 . . ? C1S C2S C3S 108.3(10) . . ? C1S C2S H2S1 110.0 . . ? C3S C2S H2S1 110.0 . . ? C1S C2S H2S2 110.0 . . ? C3S C2S H2S2 110.0 . . ? H2S1 C2S H2S2 108.4 . . ? C3S C3S C2S 105.8(11) 2_656 . ? C3S C3S H3S1 110.6 2_656 . ? C2S C3S H3S1 110.6 . . ? C3S C3S H3S2 110.6 2_656 . ? C2S C3S H3S2 110.6 . . ? H3S1 C3S H3S2 108.7 . . ? C1S C4S C5S 114.3(11) . . ? C1S C4S H4S1 108.7 . . ? C5S C4S H4S1 108.7 . . ? C1S C4S H4S2 108.7 . . ? C5S C4S H4S2 108.7 . . ? H4S1 C4S H4S2 107.6 . . ? C4S C5S C5S 111.1(11) . 2_656 ? C4S C5S H5S1 109.4 . . ? C5S C5S H5S1 109.4 2_656 . ? C4S C5S H5S2 109.4 . . ? C5S C5S H5S2 109.4 2_656 . ? H5S1 C5S H5S2 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 U1 N2 C1 90.20(16) . . . . ? N1 U1 N2 C1 -169.79(18) 2_656 . . . ? N3 U1 N2 C1 -8.92(15) . . . . ? N3 U1 N2 C1 -107.16(17) 2_656 . . . ? N2 U1 N2 C1 137.51(16) 2_656 . . . ? N1 U1 N2 C5 -81.61(15) . . . . ? N1 U1 N2 C5 18.40(14) 2_656 . . . ? N3 U1 N2 C5 179.27(17) . . . . ? N3 U1 N2 C5 81.04(18) 2_656 . . . ? N2 U1 N2 C5 -34.30(14) 2_656 . . . ? N1 U1 N3 C7 122.26(19) . . . . ? N1 U1 N3 C7 -134.98(17) 2_656 . . . ? N3 U1 N3 C7 -14.92(16) 2_656 . . . ? N2 U1 N3 C7 67.3(2) 2_656 . . . ? N2 U1 N3 C7 -157.6(2) . . . . ? N1 U1 N3 C6 -59.62(17) . . . . ? N1 U1 N3 C6 43.14(19) 2_656 . . . ? N3 U1 N3 C6 163.20(18) 2_656 . . . ? N2 U1 N3 C6 -114.59(16) 2_656 . . . ? N2 U1 N3 C6 20.51(15) . . . . ? N1 U1 N1 C19 -148.2(2) 2_656 . . . ? N3 U1 N1 C19 -18.33(19) . . . . ? N3 U1 N1 C19 109.49(19) 2_656 . . . ? N2 U1 N1 C19 131.9(2) 2_656 . . . ? N2 U1 N1 C19 -82.77(19) . . . . ? N1 U1 N1 C29 48.72(13) 2_656 . . . ? N3 U1 N1 C29 178.61(14) . . . . ? N3 U1 N1 C29 -53.57(17) 2_656 . . . ? N2 U1 N1 C29 -31.15(14) 2_656 . . . ? N2 U1 N1 C29 114.17(15) . . . . ? C9 C8 C7 C12 -2.2(3) . . . . ? C16 C8 C7 C12 175.8(2) . . . . ? C9 C8 C7 N3 -178.4(2) . . . . ? C16 C8 C7 N3 -0.5(3) . . . . ? C6 N3 C7 C8 68.3(3) . . . . ? U1 N3 C7 C8 -113.4(2) . . . . ? C6 N3 C7 C12 -107.9(2) . . . . ? U1 N3 C7 C12 70.4(2) . . . . ? C5 N2 C1 C2 -5.9(3) . . . . ? U1 N2 C1 C2 -177.59(16) . . . . ? C5 N2 C1 C6 168.50(19) . . . . ? U1 N2 C1 C6 -3.2(3) . . . . ? C8 C7 C12 C11 3.9(3) . . . . ? N3 C7 C12 C11 -179.7(2) . . . . ? C8 C7 C12 C13 -169.6(2) . . . . ? N3 C7 C12 C13 6.8(3) . . . . ? C1 N2 C5 C4 1.5(3) . . . . ? U1 N2 C5 C4 173.48(16) . . . . ? C1 N2 C5 C29 -174.39(19) . . . 2_656 ? U1 N2 C5 C29 -2.5(2) . . . 2_656 ? N2 C1 C2 C3 5.6(3) . . . . ? C6 C1 C2 C3 -168.2(2) . . . . ? C7 C8 C9 C10 -0.6(3) . . . . ? C16 C8 C9 C10 -178.7(2) . . . . ? N2 C5 C4 C3 3.0(3) . . . . ? C29 C5 C4 C3 178.4(2) 2_656 . . . ? C7 N3 C6 C1 148.45(19) . . . . ? U1 N3 C6 C1 -30.0(2) . . . . ? N2 C1 C6 N3 20.0(3) . . . . ? C2 C1 C6 N3 -165.8(2) . . . . ? C5 C4 C3 C2 -3.2(3) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C8 C9 C10 C11 1.8(4) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C7 C12 C11 C10 -2.9(3) . . . . ? C13 C12 C11 C10 170.8(2) . . . . ? C11 C12 C13 C15 22.5(3) . . . . ? C7 C12 C13 C15 -164.0(2) . . . . ? C11 C12 C13 C14 -100.0(2) . . . . ? C7 C12 C13 C14 73.5(3) . . . . ? C9 C8 C16 C17 77.3(3) . . . . ? C7 C8 C16 C17 -100.6(3) . . . . ? C9 C8 C16 C18 -43.2(3) . . . . ? C7 C8 C16 C18 138.9(2) . . . . ? C29 N1 C19 C24 77.7(2) . . . . ? U1 N1 C19 C24 -86.0(2) . . . . ? C29 N1 C19 C20 -98.5(2) . . . . ? U1 N1 C19 C20 97.8(2) . . . . ? C20 C19 C24 C23 -2.0(3) . . . . ? N1 C19 C24 C23 -178.2(2) . . . . ? C20 C19 C24 C25 174.2(2) . . . . ? N1 C19 C24 C25 -2.1(3) . . . . ? C26 C25 C24 C23 -52.2(3) . . . . ? C31 C25 C24 C23 70.3(3) . . . . ? C26 C25 C24 C19 131.6(3) . . . . ? C31 C25 C24 C19 -106.0(3) . . . . ? C24 C19 C20 C21 3.0(3) . . . . ? N1 C19 C20 C21 179.2(2) . . . . ? C24 C19 C20 C27 -173.6(2) . . . . ? N1 C19 C20 C27 2.6(3) . . . . ? C28 C27 C20 C21 28.1(3) . . . . ? C30 C27 C20 C21 -95.8(3) . . . . ? C28 C27 C20 C19 -155.3(2) . . . . ? C30 C27 C20 C19 80.8(3) . . . . ? C19 C20 C21 C22 -2.2(4) . . . . ? C27 C20 C21 C22 174.5(3) . . . . ? C19 C24 C23 C22 0.1(4) . . . . ? C25 C24 C23 C22 -176.3(3) . . . . ? C24 C23 C22 C21 0.8(5) . . . . ? C20 C21 C22 C23 0.3(5) . . . . ? C19 N1 C29 C5 -123.8(2) . . . 2_656 ? U1 N1 C29 C5 43.0(2) . . . 2_656 ? C4S C1S C2S C3S 1.1(18) . . . . ? C1S C2S C3S C3S -148.1(12) . . . 2_656 ? C2S C1S C4S C5S -9.3(17) . . . . ? C1S C4S C5S C5S -177.8(16) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.308 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.099 #===END data_1py-U(CH2Ph)2 _database_code_depnum_ccdc_archive 'CCDC 756841' #TrackingRef 'uranium_insitu_cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H55 N3 U, C4 H10 O' _chemical_formula_sum 'C49 H65 N3 O U' _chemical_formula_weight 950.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5281(10) _cell_length_b 12.7043(12) _cell_length_c 17.9213(16) _cell_angle_alpha 103.8250(10) _cell_angle_beta 105.2050(10) _cell_angle_gamma 95.6000(10) _cell_volume 2213.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 3.68 _cell_measurement_theta_max 30.25 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 3.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6145 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details 'sadabs (Bruker)' _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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22255 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 30.86 _reflns_number_total 12383 _reflns_number_gt 11086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+1.3697P] 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 12383 _refine_ls_number_parameters 487 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.874509(10) 0.825290(9) 0.720000(6) 0.02123(4) Uani 1 1 d . . . N1 N 0.9646(2) 0.6834(2) 0.66744(16) 0.0247(5) Uani 1 1 d . . . N2 N 1.0931(2) 0.8796(2) 0.69945(15) 0.0213(5) Uani 1 1 d . . . N3 N 0.9220(2) 1.0048(2) 0.73008(15) 0.0229(5) Uani 1 1 d . . . C1 C 0.6365(3) 0.7839(3) 0.6299(2) 0.0297(7) Uani 1 1 d . . . H1A H 0.5972 0.8498 0.6226 0.036 Uiso 1 1 calc R . . H1B H 0.6208 0.7281 0.5779 0.036 Uiso 1 1 calc R . . C2 C 0.6055(3) 0.7410(3) 0.6919(2) 0.0309(7) Uani 1 1 d . . . C3 C 0.6159(3) 0.8126(4) 0.7680(2) 0.0423(10) Uani 1 1 d . . . H3A H 0.5710 0.8776 0.7637 0.051 Uiso 1 1 calc R . . C4 C 0.5979(4) 0.7714(5) 0.8302(3) 0.0597(15) Uani 1 1 d . . . H4A H 0.6035 0.8206 0.8805 0.072 Uiso 1 1 calc R . . C5 C 0.5718(4) 0.6592(6) 0.8196(3) 0.0667(16) Uani 1 1 d . . . H5A H 0.5578 0.6313 0.8621 0.080 Uiso 1 1 calc R . . C6 C 0.5663(4) 0.5876(5) 0.7466(3) 0.0564(12) Uani 1 1 d . . . H6A H 0.5492 0.5105 0.7396 0.068 Uiso 1 1 calc R . . C7 C 0.5849(3) 0.6259(4) 0.6845(2) 0.0392(8) Uani 1 1 d . . . H7A H 0.5840 0.5752 0.6358 0.047 Uiso 1 1 calc R . . C8 C 0.9342(3) 0.8268(3) 0.8653(2) 0.0330(7) Uani 1 1 d . . . H8A H 0.8812 0.8713 0.8945 0.040 Uiso 1 1 calc R . . H8B H 0.9244 0.7516 0.8719 0.040 Uiso 1 1 calc R . . C9 C 1.0754(3) 0.8795(3) 0.89008(19) 0.0310(7) Uani 1 1 d . . . C10 C 1.1759(4) 0.8195(4) 0.8746(2) 0.0476(11) Uani 1 1 d . . . H10A H 1.1549 0.7417 0.8539 0.057 Uiso 1 1 calc R . . C11 C 1.3042(4) 0.8722(6) 0.8889(3) 0.0701(19) Uani 1 1 d . . . H11A H 1.3699 0.8303 0.8772 0.084 Uiso 1 1 calc R . . C12 C 1.3390(4) 0.9851(6) 0.9201(3) 0.0707(19) Uani 1 1 d . . . H12A H 1.4272 1.0211 0.9287 0.085 Uiso 1 1 calc R . . C13 C 1.2445(5) 1.0437(5) 0.9384(3) 0.0624(15) Uani 1 1 d . . . H13A H 1.2682 1.1211 0.9612 0.075 Uiso 1 1 calc R . . C14 C 1.1141(4) 0.9931(3) 0.9243(2) 0.0410(9) Uani 1 1 d . . . H14A H 1.0505 1.0362 0.9381 0.049 Uiso 1 1 calc R . . C15 C 0.8795(3) 0.5785(2) 0.62765(19) 0.0236(6) Uani 1 1 d . . . C16 C 0.8001(3) 0.5576(2) 0.54655(19) 0.0231(6) Uani 1 1 d . . . C17 C 0.7154(3) 0.4557(3) 0.5098(2) 0.0281(6) Uani 1 1 d . . . H17A H 0.6608 0.4409 0.4558 0.034 Uiso 1 1 calc R . . C18 C 0.7094(3) 0.3760(3) 0.5503(2) 0.0329(7) Uani 1 1 d . . . H18A H 0.6510 0.3076 0.5242 0.040 Uiso 1 1 calc R . . C19 C 0.7888(4) 0.3964(3) 0.6287(2) 0.0339(7) Uani 1 1 d . . . H19A H 0.7851 0.3414 0.6562 0.041 Uiso 1 1 calc R . . C20 C 0.8743(3) 0.4968(3) 0.6682(2) 0.0282(6) Uani 1 1 d . . . C21 C 0.8072(3) 0.6401(2) 0.49794(19) 0.0258(6) Uani 1 1 d . . . H21A H 0.8211 0.7153 0.5354 0.031 Uiso 1 1 calc R . . C22 C 0.9257(4) 0.6339(4) 0.4645(3) 0.0450(9) Uani 1 1 d . . . H22A H 1.0089 0.6605 0.5088 0.067 Uiso 1 1 calc R . . H22B H 0.9207 0.6797 0.4273 0.067 Uiso 1 1 calc R . . H22C H 0.9241 0.5574 0.4359 0.067 Uiso 1 1 calc R . . C23 C 0.6810(4) 0.6277(3) 0.4293(2) 0.0374(8) Uani 1 1 d . . . H23A H 0.6029 0.6223 0.4491 0.056 Uiso 1 1 calc R . . H23B H 0.6739 0.5610 0.3865 0.056 Uiso 1 1 calc R . . H23C H 0.6849 0.6919 0.4081 0.056 Uiso 1 1 calc R . . C24 C 0.9626(4) 0.5125(3) 0.7534(2) 0.0371(8) Uani 1 1 d . . . H24A H 1.0108 0.5903 0.7735 0.045 Uiso 1 1 calc R . . C25 C 0.8836(5) 0.4958(4) 0.8110(3) 0.0495(10) Uani 1 1 d . . . H25A H 0.8167 0.5443 0.8097 0.074 Uiso 1 1 calc R . . H25B H 0.9446 0.5132 0.8657 0.074 Uiso 1 1 calc R . . H25C H 0.8388 0.4190 0.7947 0.074 Uiso 1 1 calc R . . C26 C 1.0682(5) 0.4381(4) 0.7546(3) 0.0558(12) Uani 1 1 d . . . H26A H 1.1235 0.4550 0.7213 0.084 Uiso 1 1 calc R . . H26B H 1.0242 0.3610 0.7332 0.084 Uiso 1 1 calc R . . H26C H 1.1247 0.4507 0.8100 0.084 Uiso 1 1 calc R . . C27 C 1.1035(3) 0.6862(3) 0.6681(2) 0.0298(7) Uani 1 1 d . . . H27A H 1.1082 0.6382 0.6169 0.036 Uiso 1 1 calc R . . H27B H 1.1526 0.6585 0.7126 0.036 Uiso 1 1 calc R . . C28 C 1.1668(3) 0.8021(2) 0.67893(18) 0.0225(6) Uani 1 1 d . . . C29 C 1.2923(3) 0.8303(3) 0.67124(19) 0.0270(6) Uani 1 1 d . . . H29A H 1.3424 0.7750 0.6561 0.032 Uiso 1 1 calc R . . C30 C 1.3435(3) 0.9407(3) 0.6860(2) 0.0280(6) Uani 1 1 d . . . H30A H 1.4293 0.9619 0.6811 0.034 Uiso 1 1 calc R . . C31 C 1.2684(3) 1.0193(3) 0.7078(2) 0.0279(6) Uani 1 1 d . . . H31A H 1.3025 1.0951 0.7185 0.033 Uiso 1 1 calc RD . . C32 C 1.1429(3) 0.9869(3) 0.71418(18) 0.0229(6) Uani 1 1 d . . . C33 C 1.0530(3) 1.0652(3) 0.73822(19) 0.0262(6) Uani 1 1 d . . . H33A H 1.0944 1.1096 0.7947 0.031 Uiso 1 1 calc R . . H33B H 1.0419 1.1160 0.7037 0.031 Uiso 1 1 calc R . . C34 C 0.8124(3) 1.0628(2) 0.70873(18) 0.0213(5) Uani 1 1 d . . . C35 C 0.7618(3) 1.0661(2) 0.62821(18) 0.0227(6) Uani 1 1 d . . . C36 C 0.6518(3) 1.1168(3) 0.6067(2) 0.0256(6) Uani 1 1 d . . . H36A H 0.6163 1.1175 0.5523 0.031 Uiso 1 1 calc R . . C37 C 0.5934(3) 1.1665(3) 0.6640(2) 0.0267(6) Uani 1 1 d . . . H37A H 0.5188 1.2015 0.6490 0.032 Uiso 1 1 calc R . . C38 C 0.6437(3) 1.1649(3) 0.7428(2) 0.0273(6) Uani 1 1 d . . . H38A H 0.6039 1.2001 0.7817 0.033 Uiso 1 1 calc R . . C39 C 0.7522(3) 1.1126(2) 0.76688(18) 0.0237(6) Uani 1 1 d . . . C40 C 0.8258(3) 1.0162(3) 0.56272(19) 0.0270(6) Uani 1 1 d . . . H40A H 0.8964 0.9765 0.5866 0.032 Uiso 1 1 calc R . . C41 C 0.7241(4) 0.9333(3) 0.4906(2) 0.0328(7) Uani 1 1 d . . . H41A H 0.7695 0.8993 0.4522 0.049 Uiso 1 1 calc R . . H41B H 0.6561 0.9712 0.4644 0.049 Uiso 1 1 calc R . . H41C H 0.6812 0.8763 0.5088 0.049 Uiso 1 1 calc R . . C42 C 0.8933(4) 1.1079(3) 0.5362(2) 0.0349(7) Uani 1 1 d . . . H42A H 0.9339 1.0750 0.4948 0.052 Uiso 1 1 calc R . . H42B H 0.9627 1.1572 0.5826 0.052 Uiso 1 1 calc R . . H42C H 0.8264 1.1497 0.5143 0.052 Uiso 1 1 calc R . . C43 C 0.8062(3) 1.1146(3) 0.85502(19) 0.0287(7) Uani 1 1 d . . . H43A H 0.8496 1.0483 0.8571 0.034 Uiso 1 1 calc R . . C44 C 0.9131(4) 1.2166(3) 0.9007(2) 0.0417(9) Uani 1 1 d . . . H44A H 0.9831 1.2185 0.8739 0.062 Uiso 1 1 calc R . . H44B H 0.9524 1.2137 0.9560 0.062 Uiso 1 1 calc R . . H44C H 0.8724 1.2828 0.9014 0.062 Uiso 1 1 calc R . . C45 C 0.6975(4) 1.1100(3) 0.8968(2) 0.0396(8) Uani 1 1 d . . . H45A H 0.6250 1.0488 0.8643 0.059 Uiso 1 1 calc R . . H45B H 0.6625 1.1792 0.9030 0.059 Uiso 1 1 calc R . . H45C H 0.7353 1.0989 0.9499 0.059 Uiso 1 1 calc R . . O1S O 0.5150(9) 0.3582(9) 0.9140(5) 0.120(4) Uiso 0.596(8) 1 d PD A 1 C1S C 0.3816(8) 0.3043(8) 0.8682(5) 0.059(2) Uiso 0.596(8) 1 d PD A 1 H1S1 H 0.3144 0.3306 0.8945 0.070 Uiso 0.596(8) 1 calc PR A 1 H1S2 H 0.3718 0.2232 0.8562 0.070 Uiso 0.596(8) 1 calc PR A 1 C3S C 0.5270(11) 0.3387(10) 0.9889(6) 0.091(4) Uiso 0.596(8) 1 d PD A 1 H3S1 H 0.5199 0.2594 0.9857 0.109 Uiso 0.596(8) 1 calc PR A 1 H3S2 H 0.4607 0.3702 1.0139 0.109 Uiso 0.596(8) 1 calc PR A 1 C4S C 0.6681(13) 0.4011(14) 1.0322(9) 0.133(6) Uiso 0.596(8) 1 d PD A 1 H4S1 H 0.6941 0.3959 1.0877 0.199 Uiso 0.596(8) 1 calc PR A 1 H4S2 H 0.6713 0.4786 1.0325 0.199 Uiso 0.596(8) 1 calc PR A 1 H4S3 H 0.7298 0.3691 1.0044 0.199 Uiso 0.596(8) 1 calc PR A 1 O2S O 0.5805(12) 0.4142(10) 0.8892(6) 0.092(4) Uiso 0.404(8) 1 d PD A 2 C1SA C 0.456(2) 0.351(3) 0.8770(12) 0.190(15) Uiso 0.404(8) 1 d PD A 2 H1S3 H 0.4120 0.3868 0.9163 0.228 Uiso 0.404(8) 1 calc PR A 2 H1S4 H 0.4670 0.2767 0.8830 0.228 Uiso 0.404(8) 1 calc PR A 2 C3SA C 0.6541(11) 0.4284(11) 0.9682(7) 0.064(4) Uiso 0.404(8) 1 d PD A 2 H3S3 H 0.6687 0.3551 0.9752 0.077 Uiso 0.404(8) 1 calc PR A 2 H3S4 H 0.5993 0.4575 1.0031 0.077 Uiso 0.404(8) 1 calc PR A 2 C4SA C 0.7891(10) 0.5037(9) 0.9986(7) 0.048(3) Uiso 0.404(8) 1 d PD A 2 H4S4 H 0.8308 0.5076 1.0551 0.072 Uiso 0.404(8) 1 calc PR A 2 H4S5 H 0.7768 0.5776 0.9938 0.072 Uiso 0.404(8) 1 calc PR A 2 H4S6 H 0.8467 0.4746 0.9665 0.072 Uiso 0.404(8) 1 calc PR A 2 C2S C 0.3768(12) 0.3444(5) 0.7941(6) 0.166(5) Uiso 1 1 d D . . H2S1 H 0.4608 0.3931 0.8033 0.249 Uiso 0.596(8) 1 calc PR A 1 H2S2 H 0.3023 0.3847 0.7838 0.249 Uiso 0.596(8) 1 calc PR A 1 H2S3 H 0.3642 0.2811 0.7476 0.249 Uiso 0.596(8) 1 calc PR A 1 H2S4 H 0.4324 0.3804 0.7682 0.249 Uiso 0.404(8) 1 calc PR A 2 H2S5 H 0.2997 0.3813 0.7958 0.249 Uiso 0.404(8) 1 calc PR A 2 H2S6 H 0.3457 0.2670 0.7635 0.249 Uiso 0.404(8) 1 calc PR A 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 0.01359(5) 0.02298(6) 0.02538(6) 0.00407(4) 0.00462(4) 0.00468(4) N1 0.0155(11) 0.0212(12) 0.0329(14) 0.0030(10) 0.0040(10) 0.0023(9) N2 0.0129(10) 0.0247(12) 0.0225(12) 0.0041(9) 0.0009(9) 0.0039(9) N3 0.0189(11) 0.0245(12) 0.0250(12) 0.0063(10) 0.0047(10) 0.0083(9) C1 0.0195(14) 0.0349(17) 0.0288(16) 0.0012(13) 0.0031(12) 0.0073(12) C2 0.0108(12) 0.0436(19) 0.0324(17) 0.0042(14) 0.0022(12) 0.0041(12) C3 0.0176(14) 0.071(3) 0.0317(18) 0.0028(17) 0.0041(13) 0.0138(16) C4 0.0248(18) 0.117(5) 0.032(2) 0.007(2) 0.0122(16) 0.009(2) C5 0.033(2) 0.128(5) 0.047(3) 0.042(3) 0.014(2) -0.001(3) C6 0.037(2) 0.077(3) 0.061(3) 0.035(3) 0.014(2) -0.003(2) C7 0.0231(16) 0.053(2) 0.040(2) 0.0143(17) 0.0071(14) 0.0007(15) C8 0.0250(15) 0.0403(19) 0.0298(16) 0.0096(14) 0.0019(13) 0.0056(14) C9 0.0223(14) 0.049(2) 0.0194(14) 0.0113(13) 0.0003(12) 0.0087(14) C10 0.0310(18) 0.077(3) 0.0249(17) -0.0012(18) 0.0001(14) 0.0228(19) C11 0.028(2) 0.154(6) 0.028(2) 0.018(3) 0.0080(16) 0.035(3) C12 0.024(2) 0.143(6) 0.046(3) 0.049(3) -0.0016(18) -0.012(3) C13 0.044(2) 0.073(3) 0.056(3) 0.041(2) -0.019(2) -0.019(2) C14 0.0323(18) 0.046(2) 0.0358(19) 0.0157(16) -0.0068(15) 0.0034(16) C15 0.0175(13) 0.0198(13) 0.0308(15) 0.0018(11) 0.0075(11) 0.0022(10) C16 0.0205(13) 0.0192(13) 0.0299(15) 0.0048(11) 0.0087(11) 0.0061(11) C17 0.0215(14) 0.0240(15) 0.0340(17) 0.0036(12) 0.0046(12) 0.0028(12) C18 0.0254(15) 0.0215(15) 0.045(2) 0.0042(13) 0.0059(14) -0.0021(12) C19 0.0304(17) 0.0291(17) 0.044(2) 0.0147(14) 0.0100(15) 0.0031(13) C20 0.0220(14) 0.0277(15) 0.0329(16) 0.0077(12) 0.0059(12) 0.0023(12) C21 0.0270(15) 0.0190(13) 0.0296(15) 0.0038(11) 0.0069(12) 0.0064(11) C22 0.046(2) 0.047(2) 0.057(2) 0.0254(19) 0.027(2) 0.0147(18) C23 0.0394(19) 0.0339(18) 0.0336(18) 0.0084(14) 0.0024(15) 0.0070(15) C24 0.0350(18) 0.0392(19) 0.0346(18) 0.0116(15) 0.0051(15) 0.0052(15) C25 0.047(2) 0.061(3) 0.040(2) 0.0206(19) 0.0103(18) 0.001(2) C26 0.054(3) 0.066(3) 0.044(2) 0.016(2) 0.004(2) 0.027(2) C27 0.0190(13) 0.0233(15) 0.0444(19) 0.0032(13) 0.0094(13) 0.0065(11) C28 0.0159(12) 0.0238(14) 0.0234(14) 0.0031(11) 0.0014(10) 0.0031(10) C29 0.0168(13) 0.0330(16) 0.0286(15) 0.0043(12) 0.0048(11) 0.0076(12) C30 0.0163(13) 0.0356(17) 0.0318(16) 0.0106(13) 0.0067(12) 0.0008(12) C31 0.0232(14) 0.0271(15) 0.0321(16) 0.0109(12) 0.0051(12) 0.0001(12) C32 0.0195(13) 0.0252(14) 0.0223(14) 0.0078(11) 0.0019(11) 0.0050(11) C33 0.0226(14) 0.0225(14) 0.0293(15) 0.0045(11) 0.0023(12) 0.0065(11) C34 0.0193(13) 0.0164(12) 0.0269(14) 0.0056(10) 0.0038(11) 0.0062(10) C35 0.0218(13) 0.0207(13) 0.0256(14) 0.0060(11) 0.0065(11) 0.0054(11) C36 0.0237(14) 0.0231(14) 0.0299(15) 0.0101(12) 0.0047(12) 0.0059(11) C37 0.0186(13) 0.0259(15) 0.0365(17) 0.0118(12) 0.0054(12) 0.0068(11) C38 0.0256(15) 0.0242(15) 0.0352(17) 0.0084(12) 0.0121(13) 0.0095(12) C39 0.0225(14) 0.0218(14) 0.0260(14) 0.0055(11) 0.0055(11) 0.0072(11) C40 0.0288(15) 0.0289(15) 0.0254(15) 0.0086(12) 0.0086(12) 0.0102(12) C41 0.0410(19) 0.0325(17) 0.0236(15) 0.0068(12) 0.0077(14) 0.0071(14) C42 0.0364(18) 0.0375(19) 0.0375(18) 0.0146(15) 0.0170(15) 0.0103(15) C43 0.0335(16) 0.0288(16) 0.0238(15) 0.0055(12) 0.0067(13) 0.0143(13) C44 0.041(2) 0.041(2) 0.0313(18) -0.0004(15) -0.0001(15) 0.0077(16) C45 0.049(2) 0.044(2) 0.0304(18) 0.0094(15) 0.0164(16) 0.0183(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N3 2.239(3) . ? U1 N1 2.242(3) . ? U1 N2 2.482(2) . ? U1 C8 2.508(3) . ? U1 C1 2.525(3) . ? U1 C2 2.797(3) . ? U1 C3 3.064(4) . ? N1 C15 1.436(4) . ? N1 C27 1.457(4) . ? N2 C32 1.349(4) . ? N2 C28 1.354(4) . ? N3 C34 1.446(4) . ? N3 C33 1.465(4) . ? C1 C2 1.443(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.417(5) . ? C2 C7 1.426(6) . ? C3 C4 1.387(7) . ? C3 H3A 1.0000 . ? C4 C5 1.382(8) . ? C4 H4A 0.9500 . ? C5 C6 1.387(8) . ? C5 H5A 0.9500 . ? C6 C7 1.366(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.474(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C14 1.399(6) . ? C9 C10 1.410(5) . ? C10 C11 1.378(7) . ? C10 H10A 0.9500 . ? C11 C12 1.382(9) . ? C11 H11A 0.9500 . ? C12 C13 1.360(8) . ? C12 H12A 0.9500 . ? C13 C14 1.389(6) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.407(5) . ? C15 C16 1.420(4) . ? C16 C17 1.401(4) . ? C16 C21 1.523(4) . ? C17 C18 1.385(5) . ? C17 H17A 0.9500 . ? C18 C19 1.381(5) . ? C18 H18A 0.9500 . ? C19 C20 1.396(5) . ? C19 H19A 0.9500 . ? C20 C24 1.520(5) . ? C21 C23 1.520(5) . ? C21 C22 1.521(5) . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.525(6) . ? C24 C26 1.527(6) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.501(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.385(4) . ? C29 C30 1.388(5) . ? C29 H29A 0.9500 . ? C30 C31 1.381(5) . ? C30 H30A 0.9500 . ? C31 C32 1.386(4) . ? C31 H31A 0.9500 . ? C32 C33 1.504(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.413(4) . ? C34 C35 1.414(4) . ? C35 C36 1.391(4) . ? C35 C40 1.541(4) . ? C36 C37 1.390(5) . ? C36 H36A 0.9500 . ? C37 C38 1.377(5) . ? C37 H37A 0.9500 . ? C38 C39 1.399(4) . ? C38 H38A 0.9500 . ? C39 C43 1.525(4) . ? C40 C41 1.527(5) . ? C40 C42 1.539(5) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C45 1.526(5) . ? C43 C44 1.531(5) . ? C43 H43A 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O1S C3S 1.398(8) . ? O1S C1S 1.433(8) . ? C1S C2S 1.523(8) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C3S C4S 1.519(9) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9800 . ? C4S H4S2 0.9800 . ? C4S H4S3 0.9800 . ? O2S C3SA 1.383(8) . ? O2S C1SA 1.401(9) . ? C1SA C2S 1.479(10) . ? C1SA H1S3 0.9900 . ? C1SA H1S4 0.9900 . ? C3SA C4SA 1.521(9) . ? C3SA H3S3 0.9900 . ? C3SA H3S4 0.9900 . ? C4SA H4S4 0.9800 . ? C4SA H4S5 0.9800 . ? C4SA H4S6 0.9800 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 0.9800 . ? C2S H2S4 0.9800 . ? C2S H2S5 0.9800 . ? C2S H2S6 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 U1 N1 130.48(9) . . ? N3 U1 N2 66.44(9) . . ? N1 U1 N2 65.78(9) . . ? N3 U1 C8 101.32(11) . . ? N1 U1 C8 101.79(11) . . ? N2 U1 C8 103.78(10) . . ? N3 U1 C1 99.44(10) . . ? N1 U1 C1 103.61(10) . . ? N2 U1 C1 133.25(10) . . ? C8 U1 C1 122.90(11) . . ? N3 U1 C2 116.00(10) . . ? N1 U1 C2 105.85(10) . . ? N2 U1 C2 162.45(9) . . ? C8 U1 C2 92.90(11) . . ? C1 U1 C2 30.94(11) . . ? N3 U1 C3 101.82(11) . . ? N1 U1 C3 126.83(11) . . ? N2 U1 C3 167.01(11) . . ? C8 U1 C3 72.16(11) . . ? C1 U1 C3 51.69(10) . . ? C2 U1 C3 27.50(10) . . ? C15 N1 C27 115.1(2) . . ? C15 N1 U1 118.56(18) . . ? C27 N1 U1 126.37(19) . . ? C32 N2 C28 119.7(3) . . ? C32 N2 U1 120.06(19) . . ? C28 N2 U1 120.1(2) . . ? C34 N3 C33 114.2(2) . . ? C34 N3 U1 118.32(19) . . ? C33 N3 U1 125.91(18) . . ? C2 C1 U1 84.98(18) . . ? C2 C1 H1A 114.5 . . ? U1 C1 H1A 114.5 . . ? C2 C1 H1B 114.5 . . ? U1 C1 H1B 114.5 . . ? H1A C1 H1B 111.6 . . ? C3 C2 C7 116.9(4) . . ? C3 C2 C1 120.5(4) . . ? C7 C2 C1 121.8(3) . . ? C3 C2 U1 86.8(2) . . ? C7 C2 U1 111.9(2) . . ? C1 C2 U1 64.08(17) . . ? C4 C3 C2 120.9(5) . . ? C4 C3 U1 124.5(3) . . ? C2 C3 U1 65.70(18) . . ? C4 C3 H3A 112.6 . . ? C2 C3 H3A 112.6 . . ? U1 C3 H3A 112.6 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 119.5(4) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C7 C6 C5 121.2(5) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C6 C7 C2 120.8(4) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? C9 C8 U1 98.6(2) . . ? C9 C8 H8A 112.0 . . ? U1 C8 H8A 112.0 . . ? C9 C8 H8B 112.0 . . ? U1 C8 H8B 112.0 . . ? H8A C8 H8B 109.7 . . ? C14 C9 C10 116.9(4) . . ? C14 C9 C8 121.3(3) . . ? C10 C9 C8 121.6(4) . . ? C11 C10 C9 120.8(5) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C10 C11 C12 121.2(5) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C13 C12 C11 118.6(4) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? C12 C13 C14 121.6(5) . . ? C12 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C13 C14 C9 120.7(4) . . ? C13 C14 H14A 119.6 . . ? C9 C14 H14A 119.6 . . ? C20 C15 C16 119.9(3) . . ? C20 C15 N1 120.7(3) . . ? C16 C15 N1 119.4(3) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 C21 119.3(3) . . ? C15 C16 C21 122.4(3) . . ? C18 C17 C16 121.6(3) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 121.0(3) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C19 C20 C15 119.6(3) . . ? C19 C20 C24 118.3(3) . . ? C15 C20 C24 122.1(3) . . ? C23 C21 C22 109.0(3) . . ? C23 C21 C16 114.0(3) . . ? C22 C21 C16 111.1(3) . . ? C23 C21 H21A 107.5 . . ? C22 C21 H21A 107.5 . . ? C16 C21 H21A 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 C25 113.1(3) . . ? C20 C24 C26 111.1(3) . . ? C25 C24 C26 110.6(4) . . ? C20 C24 H24A 107.3 . . ? C25 C24 H24A 107.3 . . ? C26 C24 H24A 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 C27 C28 109.6(2) . . ? N1 C27 H27A 109.7 . . ? C28 C27 H27A 109.7 . . ? N1 C27 H27B 109.7 . . ? C28 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? N2 C28 C29 121.5(3) . . ? N2 C28 C27 114.7(3) . . ? C29 C28 C27 123.8(3) . . ? C28 C29 C30 118.9(3) . . ? C28 C29 H29A 120.5 . . ? C30 C29 H29A 120.6 . . ? C31 C30 C29 119.3(3) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C30 C31 C32 119.6(3) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? N2 C32 C31 121.0(3) . . ? N2 C32 C33 114.8(3) . . ? C31 C32 C33 124.2(3) . . ? N3 C33 C32 110.6(3) . . ? N3 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C39 C34 C35 119.7(3) . . ? C39 C34 N3 120.7(3) . . ? C35 C34 N3 119.6(3) . . ? C36 C35 C34 119.7(3) . . ? C36 C35 C40 118.2(3) . . ? C34 C35 C40 122.1(3) . . ? C37 C36 C35 120.5(3) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C38 C37 C36 119.9(3) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C39 121.6(3) . . ? C37 C38 H38A 119.2 . . ? C39 C38 H38A 119.2 . . ? C38 C39 C34 118.6(3) . . ? C38 C39 C43 119.7(3) . . ? C34 C39 C43 121.6(3) . . ? C41 C40 C42 110.7(3) . . ? C41 C40 C35 111.8(3) . . ? C42 C40 C35 110.4(3) . . ? C41 C40 H40A 107.9 . . ? C42 C40 H40A 107.9 . . ? C35 C40 H40A 107.9 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C43 C45 113.2(3) . . ? C39 C43 C44 110.3(3) . . ? C45 C43 C44 109.9(3) . . ? C39 C43 H43A 107.8 . . ? C45 C43 H43A 107.8 . . ? C44 C43 H43A 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C3S O1S C1S 102.8(8) . . ? O1S C1S C2S 96.9(7) . . ? O1S C1S H1S1 112.4 . . ? C2S C1S H1S1 112.4 . . ? O1S C1S H1S2 112.4 . . ? C2S C1S H1S2 112.4 . . ? H1S1 C1S H1S2 109.9 . . ? O1S C3S C4S 98.2(9) . . ? O1S C3S H3S1 112.1 . . ? C4S C3S H3S1 112.1 . . ? O1S C3S H3S2 112.1 . . ? C4S C3S H3S2 112.1 . . ? H3S1 C3S H3S2 109.8 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? C3SA O2S C1SA 107.2(10) . . ? O2S C1SA C2S 105.8(13) . . ? O2S C1SA H1S3 110.6 . . ? C2S C1SA H1S3 110.6 . . ? O2S C1SA H1S4 110.6 . . ? C2S C1SA H1S4 110.6 . . ? H1S3 C1SA H1S4 108.7 . . ? O2S C3SA C4SA 117.2(11) . . ? O2S C3SA H3S3 108.0 . . ? C4SA C3SA H3S3 108.0 . . ? O2S C3SA H3S4 108.0 . . ? C4SA C3SA H3S4 108.0 . . ? H3S3 C3SA H3S4 107.2 . . ? C3SA C4SA H4S4 109.5 . . ? C3SA C4SA H4S5 109.5 . . ? H4S4 C4SA H4S5 109.5 . . ? C3SA C4SA H4S6 109.5 . . ? H4S4 C4SA H4S6 109.5 . . ? H4S5 C4SA H4S6 109.5 . . ? C1SA C2S H2S1 75.0 . . ? C1S C2S H2S1 109.5 . . ? C1SA C2S H2S2 121.4 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1SA C2S H2S3 124.2 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C1SA C2S H2S4 109.5 . . ? C1S C2S H2S4 143.1 . . ? H2S2 C2S H2S4 97.4 . . ? H2S3 C2S H2S4 83.5 . . ? C1SA C2S H2S5 109.5 . . ? C1S C2S H2S5 95.6 . . ? H2S1 C2S H2S5 115.2 . . ? H2S3 C2S H2S5 116.5 . . ? H2S4 C2S H2S5 109.5 . . ? C1SA C2S H2S6 109.5 . . ? C1S C2S H2S6 85.8 . . ? H2S1 C2S H2S6 130.4 . . ? H2S2 C2S H2S6 108.8 . . ? H2S4 C2S H2S6 109.5 . . ? H2S5 C2S H2S6 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 U1 N1 C15 -145.4(2) . . . . ? N2 U1 N1 C15 -161.7(3) . . . . ? C8 U1 N1 C15 98.3(2) . . . . ? C1 U1 N1 C15 -30.1(3) . . . . ? C2 U1 N1 C15 1.8(3) . . . . ? C3 U1 N1 C15 21.9(3) . . . . ? N3 U1 N1 C27 33.5(3) . . . . ? N2 U1 N1 C27 17.3(2) . . . . ? C8 U1 N1 C27 -82.7(3) . . . . ? C1 U1 N1 C27 148.9(3) . . . . ? C2 U1 N1 C27 -179.2(3) . . . . ? C3 U1 N1 C27 -159.1(2) . . . . ? N3 U1 N2 C32 8.8(2) . . . . ? N1 U1 N2 C32 175.3(2) . . . . ? C8 U1 N2 C32 -87.8(2) . . . . ? C1 U1 N2 C32 89.3(2) . . . . ? C2 U1 N2 C32 110.7(3) . . . . ? C3 U1 N2 C32 -17.6(5) . . . . ? N3 U1 N2 C28 -175.9(2) . . . . ? N1 U1 N2 C28 -9.3(2) . . . . ? C8 U1 N2 C28 87.6(2) . . . . ? C1 U1 N2 C28 -95.4(2) . . . . ? C2 U1 N2 C28 -73.9(4) . . . . ? C3 U1 N2 C28 157.7(4) . . . . ? N1 U1 N3 C34 134.6(2) . . . . ? N2 U1 N3 C34 150.8(2) . . . . ? C8 U1 N3 C34 -109.0(2) . . . . ? C1 U1 N3 C34 17.5(2) . . . . ? C2 U1 N3 C34 -10.1(2) . . . . ? C3 U1 N3 C34 -35.1(2) . . . . ? N1 U1 N3 C33 -30.2(3) . . . . ? N2 U1 N3 C33 -14.0(2) . . . . ? C8 U1 N3 C33 86.2(2) . . . . ? C1 U1 N3 C33 -147.3(2) . . . . ? C2 U1 N3 C33 -174.8(2) . . . . ? C3 U1 N3 C33 160.1(2) . . . . ? N3 U1 C1 C2 -126.0(2) . . . . ? N1 U1 C1 C2 98.2(2) . . . . ? N2 U1 C1 C2 167.61(17) . . . . ? C8 U1 C1 C2 -15.8(3) . . . . ? C3 U1 C1 C2 -28.3(2) . . . . ? U1 C1 C2 C3 69.0(3) . . . . ? U1 C1 C2 C7 -100.7(3) . . . . ? N3 U1 C2 C3 -63.7(3) . . . . ? N1 U1 C2 C3 143.5(2) . . . . ? N2 U1 C2 C3 -157.6(3) . . . . ? C8 U1 C2 C3 40.4(3) . . . . ? C1 U1 C2 C3 -126.4(3) . . . . ? N3 U1 C2 C7 178.6(2) . . . . ? N1 U1 C2 C7 25.8(3) . . . . ? N2 U1 C2 C7 84.7(4) . . . . ? C8 U1 C2 C7 -77.3(3) . . . . ? C1 U1 C2 C7 115.9(3) . . . . ? C3 U1 C2 C7 -117.7(4) . . . . ? N3 U1 C2 C1 62.7(2) . . . . ? N1 U1 C2 C1 -90.1(2) . . . . ? N2 U1 C2 C1 -31.2(4) . . . . ? C8 U1 C2 C1 166.8(2) . . . . ? C3 U1 C2 C1 126.4(3) . . . . ? C7 C2 C3 C4 -4.1(5) . . . . ? C1 C2 C3 C4 -174.3(3) . . . . ? U1 C2 C3 C4 -117.0(3) . . . . ? C7 C2 C3 U1 112.9(3) . . . . ? C1 C2 C3 U1 -57.2(2) . . . . ? N3 U1 C3 C4 -123.5(4) . . . . ? N1 U1 C3 C4 66.3(4) . . . . ? N2 U1 C3 C4 -98.9(6) . . . . ? C8 U1 C3 C4 -25.3(4) . . . . ? C1 U1 C3 C4 143.8(5) . . . . ? C2 U1 C3 C4 111.9(5) . . . . ? N3 U1 C3 C2 124.6(2) . . . . ? N1 U1 C3 C2 -45.6(3) . . . . ? N2 U1 C3 C2 149.2(4) . . . . ? C8 U1 C3 C2 -137.2(3) . . . . ? C1 U1 C3 C2 31.8(2) . . . . ? C2 C3 C4 C5 1.2(6) . . . . ? U1 C3 C4 C5 -78.9(5) . . . . ? C3 C4 C5 C6 1.2(7) . . . . ? C4 C5 C6 C7 -0.6(7) . . . . ? C5 C6 C7 C2 -2.4(6) . . . . ? C3 C2 C7 C6 4.7(5) . . . . ? C1 C2 C7 C6 174.7(3) . . . . ? U1 C2 C7 C6 102.5(4) . . . . ? N3 U1 C8 C9 -58.2(2) . . . . ? N1 U1 C8 C9 77.7(2) . . . . ? N2 U1 C8 C9 10.0(2) . . . . ? C1 U1 C8 C9 -167.4(2) . . . . ? C2 U1 C8 C9 -175.5(2) . . . . ? C3 U1 C8 C9 -157.2(3) . . . . ? U1 C8 C9 C14 94.6(3) . . . . ? U1 C8 C9 C10 -80.2(3) . . . . ? C14 C9 C10 C11 -3.2(6) . . . . ? C8 C9 C10 C11 171.8(4) . . . . ? C9 C10 C11 C12 1.1(7) . . . . ? C10 C11 C12 C13 1.5(7) . . . . ? C11 C12 C13 C14 -1.7(7) . . . . ? C12 C13 C14 C9 -0.5(6) . . . . ? C10 C9 C14 C13 3.0(5) . . . . ? C8 C9 C14 C13 -172.0(3) . . . . ? C27 N1 C15 C20 82.8(4) . . . . ? U1 N1 C15 C20 -98.1(3) . . . . ? C27 N1 C15 C16 -97.2(3) . . . . ? U1 N1 C15 C16 81.9(3) . . . . ? C20 C15 C16 C17 1.7(4) . . . . ? N1 C15 C16 C17 -178.3(3) . . . . ? C20 C15 C16 C21 -176.5(3) . . . . ? N1 C15 C16 C21 3.5(4) . . . . ? C15 C16 C17 C18 -0.9(5) . . . . ? C21 C16 C17 C18 177.3(3) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 0.6(5) . . . . ? C18 C19 C20 C15 0.2(5) . . . . ? C18 C19 C20 C24 -177.8(3) . . . . ? C16 C15 C20 C19 -1.3(5) . . . . ? N1 C15 C20 C19 178.7(3) . . . . ? C16 C15 C20 C24 176.6(3) . . . . ? N1 C15 C20 C24 -3.4(5) . . . . ? C17 C16 C21 C23 26.6(4) . . . . ? C15 C16 C21 C23 -155.3(3) . . . . ? C17 C16 C21 C22 -97.0(4) . . . . ? C15 C16 C21 C22 81.1(4) . . . . ? C19 C20 C24 C25 -57.3(5) . . . . ? C15 C20 C24 C25 124.7(4) . . . . ? C19 C20 C24 C26 67.7(5) . . . . ? C15 C20 C24 C26 -110.3(4) . . . . ? C15 N1 C27 C28 156.8(3) . . . . ? U1 N1 C27 C28 -22.2(4) . . . . ? C32 N2 C28 C29 -1.1(4) . . . . ? U1 N2 C28 C29 -176.5(2) . . . . ? C32 N2 C28 C27 177.1(3) . . . . ? U1 N2 C28 C27 1.7(3) . . . . ? N1 C27 C28 N2 10.9(4) . . . . ? N1 C27 C28 C29 -170.9(3) . . . . ? N2 C28 C29 C30 0.8(5) . . . . ? C27 C28 C29 C30 -177.2(3) . . . . ? C28 C29 C30 C31 0.0(5) . . . . ? C29 C30 C31 C32 -0.4(5) . . . . ? C28 N2 C32 C31 0.7(4) . . . . ? U1 N2 C32 C31 176.0(2) . . . . ? C28 N2 C32 C33 -178.7(3) . . . . ? U1 N2 C32 C33 -3.3(3) . . . . ? C30 C31 C32 N2 0.1(5) . . . . ? C30 C31 C32 C33 179.4(3) . . . . ? C34 N3 C33 C32 -148.1(3) . . . . ? U1 N3 C33 C32 17.2(4) . . . . ? N2 C32 C33 N3 -7.3(4) . . . . ? C31 C32 C33 N3 173.4(3) . . . . ? C33 N3 C34 C39 -104.5(3) . . . . ? U1 N3 C34 C39 89.0(3) . . . . ? C33 N3 C34 C35 77.9(3) . . . . ? U1 N3 C34 C35 -88.6(3) . . . . ? C39 C34 C35 C36 -1.0(4) . . . . ? N3 C34 C35 C36 176.6(3) . . . . ? C39 C34 C35 C40 178.2(3) . . . . ? N3 C34 C35 C40 -4.2(4) . . . . ? C34 C35 C36 C37 1.5(5) . . . . ? C40 C35 C36 C37 -177.7(3) . . . . ? C35 C36 C37 C38 -0.5(5) . . . . ? C36 C37 C38 C39 -1.0(5) . . . . ? C37 C38 C39 C34 1.5(5) . . . . ? C37 C38 C39 C43 179.0(3) . . . . ? C35 C34 C39 C38 -0.4(4) . . . . ? N3 C34 C39 C38 -178.0(3) . . . . ? C35 C34 C39 C43 -177.9(3) . . . . ? N3 C34 C39 C43 4.5(4) . . . . ? C36 C35 C40 C41 -55.5(4) . . . . ? C34 C35 C40 C41 125.3(3) . . . . ? C36 C35 C40 C42 68.2(4) . . . . ? C34 C35 C40 C42 -111.1(3) . . . . ? C38 C39 C43 C45 34.8(4) . . . . ? C34 C39 C43 C45 -147.8(3) . . . . ? C38 C39 C43 C44 -88.8(4) . . . . ? C34 C39 C43 C44 88.6(4) . . . . ? C3S O1S C1S C2S 173.0(9) . . . . ? C1S O1S C3S C4S -178.5(10) . . . . ? C3SA O2S C1SA C2S 176.0(19) . . . . ? C1SA O2S C3SA C4SA -174(2) . . . . ? O2S C1SA C2S C1S 173(5) . . . . ? O1S C1S C2S C1SA -5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.378 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.115 #===END data_1py-UI(CH2Ph) _database_code_depnum_ccdc_archive 'CCDC 756842' #TrackingRef 'uranium_insitu_cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H48 I N3 U, 0.5(C14 H12)' _chemical_formula_sum 'C45 H54 I N3 U' _chemical_formula_weight 1001.84 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.3927(15) _cell_length_b 13.9847(19) _cell_length_c 25.077(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.235(2) _cell_angle_gamma 90.00 _cell_volume 3978.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2841 _cell_measurement_theta_min 3.72 _cell_measurement_theta_max 20.68 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 4.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6157 _exptl_absorpt_correction_T_max 0.8284 _exptl_absorpt_process_details 'Sadabs (Bruker)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25937 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0747 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 24.43 _reflns_number_total 6513 _reflns_number_gt 4748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+5.6329P] 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 6513 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 C1S C 0.9882(10) 0.3730(8) 0.5288(4) 0.064(3) Uani 1 1 d . . . C2S C 0.9746(10) 0.2918(8) 0.4981(5) 0.076(3) Uani 1 1 d . . . H2S H 0.9978 0.2919 0.4627 0.091 Uiso 1 1 calc R . . C3S C 0.9262(9) 0.2077(7) 0.5189(4) 0.059(3) Uani 1 1 d . . . H3S H 0.9144 0.1521 0.4973 0.071 Uiso 1 1 calc R . . C4S C 0.8972(9) 0.2081(7) 0.5701(4) 0.058(3) Uani 1 1 d . . . H4S H 0.8659 0.1519 0.5847 0.070 Uiso 1 1 calc R . . C5S C 0.9127(10) 0.2893(8) 0.6012(5) 0.068(3) Uani 1 1 d . . . H5S H 0.8901 0.2891 0.6367 0.082 Uiso 1 1 calc R . . C6S C 0.9597(10) 0.3692(9) 0.5815(5) 0.080(3) Uani 1 1 d . . . H6S H 0.9735 0.4235 0.6039 0.095 Uiso 1 1 calc R . . C7S C 1.0414(10) 0.4661(8) 0.5089(6) 0.098(5) Uani 1 1 d . . . H7S1 H 1.1239 0.4760 0.5089 0.147 Uiso 1 1 calc R . . U1 U 0.29276(2) 0.260249(17) 0.370459(10) 0.01793(9) Uani 1 1 d . . . I1 I 0.06660(5) 0.36837(4) 0.33920(2) 0.03337(15) Uani 1 1 d . . . N1 N 0.2448(5) 0.1286(4) 0.4129(2) 0.0166(13) Uani 1 1 d . . . N2 N 0.2896(5) 0.2781(4) 0.4689(2) 0.0181(13) Uani 1 1 d . . . N3 N 0.3836(5) 0.3887(4) 0.4031(2) 0.0178(13) Uani 1 1 d . . . C6 C 0.4307(6) 0.1977(5) 0.3065(3) 0.0230(18) Uani 1 1 d . . . H6A H 0.5058 0.2334 0.3067 0.028 Uiso 1 1 calc R . . H6B H 0.4442 0.1279 0.3086 0.028 Uiso 1 1 calc R . . C7 C 0.3414(6) 0.2269(5) 0.2649(3) 0.0215(17) Uani 1 1 d . . . C8 C 0.3398(7) 0.3199(5) 0.2416(3) 0.0267(19) Uani 1 1 d . . . H8A H 0.4033 0.3626 0.2508 0.032 Uiso 1 1 calc R . . C9 C 0.2475(7) 0.3489(5) 0.2060(3) 0.0282(19) Uani 1 1 d . . . H9A H 0.2492 0.4108 0.1904 0.034 Uiso 1 1 calc R . . C10 C 0.1524(7) 0.2895(6) 0.1924(3) 0.030(2) Uani 1 1 d . . . H10A H 0.0905 0.3101 0.1671 0.036 Uiso 1 1 calc R . . C11 C 0.1475(7) 0.1998(5) 0.2159(3) 0.0279(19) Uani 1 1 d . . . H11A H 0.0817 0.1591 0.2074 0.034 Uiso 1 1 calc R . . C12 C 0.2398(7) 0.1709(5) 0.2517(3) 0.0237(18) Uani 1 1 d . . . H12A H 0.2347 0.1101 0.2683 0.028 Uiso 1 1 calc R . . C13 C 0.2258(6) 0.0457(5) 0.3785(3) 0.0185(16) Uani 1 1 d . . . C14 C 0.1131(6) 0.0312(5) 0.3517(3) 0.0190(17) Uani 1 1 d . . . C15 C 0.1004(7) -0.0410(5) 0.3115(3) 0.0277(19) Uani 1 1 d . . . H15A H 0.0259 -0.0510 0.2921 0.033 Uiso 1 1 calc R . . C16 C 0.1945(7) -0.0962(5) 0.3006(3) 0.0286(19) Uani 1 1 d . . . H16A H 0.1852 -0.1428 0.2730 0.034 Uiso 1 1 calc R . . C17 C 0.3014(7) -0.0848(5) 0.3291(3) 0.0261(18) Uani 1 1 d . . . H17A H 0.3645 -0.1257 0.3218 0.031 Uiso 1 1 calc R . . C18 C 0.3210(6) -0.0145(5) 0.3688(3) 0.0203(17) Uani 1 1 d . . . C19 C 0.0036(6) 0.0852(5) 0.3654(3) 0.0222(17) Uani 1 1 d . . . H19A H 0.0300 0.1435 0.3862 0.027 Uiso 1 1 calc R . . C20 C -0.0736(7) 0.1174(5) 0.3159(3) 0.034(2) Uani 1 1 d . . . H20A H -0.0264 0.1553 0.2929 0.051 Uiso 1 1 calc R . . H20B H -0.1386 0.1566 0.3269 0.051 Uiso 1 1 calc R . . H20C H -0.1055 0.0613 0.2962 0.051 Uiso 1 1 calc R . . C21 C -0.0661(6) 0.0225(5) 0.4013(3) 0.0290(19) Uani 1 1 d . . . H21A H -0.0154 0.0044 0.4335 0.044 Uiso 1 1 calc R . . H21B H -0.0930 -0.0353 0.3818 0.044 Uiso 1 1 calc R . . H21C H -0.1344 0.0581 0.4118 0.044 Uiso 1 1 calc R . . C22 C 0.4372(6) -0.0112(5) 0.4034(3) 0.0263(19) Uani 1 1 d . . . H22A H 0.4463 0.0540 0.4197 0.032 Uiso 1 1 calc R . . C23 C 0.4346(7) -0.0855(5) 0.4496(3) 0.032(2) Uani 1 1 d . . . H23A H 0.3656 -0.0737 0.4693 0.049 Uiso 1 1 calc R . . H23B H 0.5065 -0.0792 0.4740 0.049 Uiso 1 1 calc R . . H23C H 0.4302 -0.1502 0.4345 0.049 Uiso 1 1 calc R . . C24 C 0.5451(6) -0.0315(5) 0.3731(3) 0.032(2) Uani 1 1 d . . . H24A H 0.5444 0.0111 0.3420 0.048 Uiso 1 1 calc R . . H24B H 0.5431 -0.0982 0.3610 0.048 Uiso 1 1 calc R . . H24C H 0.6170 -0.0204 0.3969 0.048 Uiso 1 1 calc R . . C25 C 0.2229(6) 0.1162(5) 0.4694(3) 0.0210(17) Uani 1 1 d . . . H25A H 0.2711 0.0626 0.4852 0.025 Uiso 1 1 calc R . . H25B H 0.1388 0.1007 0.4720 0.025 Uiso 1 1 calc R . . C26 C 0.2483(7) 0.2179(5) 0.5538(3) 0.0260(19) Uani 1 1 d . . . H26A H 0.2231 0.1667 0.5749 0.031 Uiso 1 1 calc R . . C27 C 0.2793(7) 0.3039(5) 0.5768(3) 0.0286(19) Uani 1 1 d . . . H27A H 0.2758 0.3126 0.6142 0.034 Uiso 1 1 calc R . . C28 C 0.3156(6) 0.3778(5) 0.5461(3) 0.0290(19) Uani 1 1 d . . . H28A H 0.3371 0.4377 0.5620 0.035 Uiso 1 1 calc R . . C29 C 0.3202(6) 0.3637(5) 0.4919(3) 0.0226(17) Uani 1 1 d . . . C30 C 0.3589(7) 0.4365(5) 0.4530(3) 0.0287(19) Uani 1 1 d . . . H30A H 0.2962 0.4849 0.4454 0.034 Uiso 1 1 calc R . . H30B H 0.4307 0.4696 0.4688 0.034 Uiso 1 1 calc R . . C31 C 0.4878(6) 0.4205(5) 0.3786(3) 0.0192(17) Uani 1 1 d . . . C32 C 0.4792(7) 0.5026(5) 0.3451(3) 0.0230(17) Uani 1 1 d . . . C33 C 0.5794(7) 0.5275(5) 0.3196(3) 0.0233(18) Uani 1 1 d . . . H33A H 0.5768 0.5825 0.2973 0.028 Uiso 1 1 calc R . . C34 C 0.6802(7) 0.4750(5) 0.3261(3) 0.0257(18) Uani 1 1 d . . . H34A H 0.7457 0.4925 0.3073 0.031 Uiso 1 1 calc R . . C35 C 0.6884(7) 0.3962(5) 0.3598(3) 0.0270(18) Uani 1 1 d . . . H35A H 0.7604 0.3618 0.3652 0.032 Uiso 1 1 calc R . . C36 C 0.3710(7) 0.5674(5) 0.3400(3) 0.0250(18) Uani 1 1 d . . . H36A H 0.3069 0.5343 0.3575 0.030 Uiso 1 1 calc R . . C37 C 0.3258(7) 0.5867(6) 0.2819(3) 0.038(2) Uani 1 1 d . . . H37A H 0.2535 0.6248 0.2808 0.057 Uiso 1 1 calc R . . H37B H 0.3091 0.5258 0.2634 0.057 Uiso 1 1 calc R . . H37C H 0.3858 0.6217 0.2642 0.057 Uiso 1 1 calc R . . C38 C 0.3990(7) 0.6599(5) 0.3700(3) 0.037(2) Uani 1 1 d . . . H38A H 0.4190 0.6460 0.4081 0.056 Uiso 1 1 calc R . . H38B H 0.3302 0.7022 0.3660 0.056 Uiso 1 1 calc R . . H38C H 0.4660 0.6914 0.3554 0.056 Uiso 1 1 calc R . . C39 C 0.2540(6) 0.2065(5) 0.4995(3) 0.0188(17) Uani 1 1 d . . . C40 C 0.5916(6) 0.3675(5) 0.3856(3) 0.0221(17) Uani 1 1 d . . . C41 C 0.6018(7) 0.2832(5) 0.4250(3) 0.0257(18) Uani 1 1 d . . . H41A H 0.5217 0.2542 0.4255 0.031 Uiso 1 1 calc R . . C42 C 0.6394(8) 0.3190(5) 0.4809(3) 0.042(2) Uani 1 1 d . . . H42A H 0.6444 0.2651 0.5059 0.063 Uiso 1 1 calc R . . H42B H 0.5815 0.3654 0.4916 0.063 Uiso 1 1 calc R . . H42C H 0.7168 0.3499 0.4813 0.063 Uiso 1 1 calc R . . C43 C 0.6852(7) 0.2052(5) 0.4091(3) 0.032(2) Uani 1 1 d . . . H43A H 0.6637 0.1865 0.3718 0.047 Uiso 1 1 calc R . . H43B H 0.6792 0.1496 0.4325 0.047 Uiso 1 1 calc R . . H43C H 0.7663 0.2294 0.4128 0.047 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 C1S 0.074(8) 0.064(8) 0.057(7) 0.006(6) 0.019(6) 0.014(6) C2S 0.077(9) 0.067(8) 0.083(9) 0.011(7) 0.004(7) 0.013(7) C3S 0.060(7) 0.049(7) 0.065(8) 0.002(5) -0.011(6) 0.000(5) C4S 0.066(8) 0.051(7) 0.058(7) 0.009(5) 0.001(6) 0.007(5) C5S 0.072(8) 0.062(7) 0.073(8) 0.005(6) 0.016(7) 0.003(6) C6S 0.082(9) 0.084(9) 0.075(9) 0.020(7) 0.021(7) 0.007(7) C7S 0.071(9) 0.056(8) 0.160(13) 0.047(8) -0.026(9) -0.016(6) U1 0.02529(15) 0.01502(14) 0.01388(13) -0.00087(13) 0.00408(10) -0.00016(14) I1 0.0339(3) 0.0328(3) 0.0331(3) -0.0010(2) 0.0013(2) 0.0060(2) N1 0.017(3) 0.020(3) 0.014(3) -0.004(3) 0.004(3) 0.002(3) N2 0.013(3) 0.024(3) 0.018(3) 0.002(3) 0.002(3) -0.002(3) N3 0.021(3) 0.018(3) 0.016(3) 0.000(3) 0.011(3) 0.000(3) C6 0.029(5) 0.016(4) 0.026(4) -0.003(3) 0.008(4) 0.001(3) C7 0.033(5) 0.020(4) 0.013(4) -0.009(3) 0.009(3) 0.008(3) C8 0.044(5) 0.019(4) 0.019(4) -0.004(3) 0.011(4) 0.005(4) C9 0.038(5) 0.026(4) 0.020(4) -0.001(3) 0.002(4) 0.007(4) C10 0.034(5) 0.043(5) 0.014(4) 0.002(4) 0.005(4) 0.013(4) C11 0.031(5) 0.033(5) 0.021(4) -0.004(4) 0.007(4) -0.001(4) C12 0.036(5) 0.018(4) 0.019(4) 0.000(3) 0.010(4) 0.002(4) C13 0.023(5) 0.014(4) 0.018(4) 0.002(3) -0.001(3) -0.004(3) C14 0.026(4) 0.011(4) 0.020(4) 0.006(3) 0.001(3) -0.003(3) C15 0.033(5) 0.028(4) 0.021(4) 0.001(3) 0.000(4) -0.010(4) C16 0.044(6) 0.026(4) 0.015(4) -0.002(3) 0.001(4) -0.014(4) C17 0.036(5) 0.015(4) 0.028(4) -0.003(3) 0.009(4) 0.006(3) C18 0.025(5) 0.012(4) 0.024(4) 0.003(3) 0.004(4) -0.005(3) C19 0.022(4) 0.027(4) 0.018(4) 0.004(3) 0.003(3) -0.007(3) C20 0.037(5) 0.032(5) 0.033(5) 0.005(4) 0.000(4) -0.001(4) C21 0.029(5) 0.027(4) 0.032(5) -0.003(4) 0.006(4) -0.007(4) C22 0.036(5) 0.016(4) 0.027(4) 0.001(3) 0.000(4) 0.007(3) C23 0.043(5) 0.034(5) 0.020(4) 0.004(4) 0.001(4) -0.002(4) C24 0.027(5) 0.023(4) 0.047(5) 0.000(4) 0.008(4) 0.015(4) C25 0.024(4) 0.017(4) 0.022(4) -0.002(3) 0.003(3) -0.001(3) C26 0.037(5) 0.029(5) 0.013(4) 0.002(3) 0.002(3) -0.009(4) C27 0.037(5) 0.036(5) 0.013(4) -0.005(4) 0.007(4) -0.002(4) C28 0.033(5) 0.029(5) 0.026(5) -0.009(4) 0.009(4) -0.005(4) C29 0.023(4) 0.021(4) 0.024(4) -0.007(3) 0.006(3) -0.005(3) C30 0.031(5) 0.030(4) 0.028(5) -0.007(4) 0.017(4) -0.003(4) C31 0.034(5) 0.018(4) 0.006(4) -0.001(3) 0.004(3) -0.010(3) C32 0.035(5) 0.016(4) 0.017(4) 0.000(3) -0.002(4) -0.003(3) C33 0.036(5) 0.019(4) 0.015(4) 0.006(3) 0.004(4) -0.004(4) C34 0.032(5) 0.030(4) 0.018(4) 0.001(3) 0.018(4) -0.011(4) C35 0.029(5) 0.026(4) 0.027(4) -0.002(4) 0.008(4) 0.004(4) C36 0.029(5) 0.019(4) 0.028(5) 0.003(3) 0.007(4) 0.000(3) C37 0.043(6) 0.043(5) 0.025(5) -0.009(4) -0.017(4) 0.006(4) C38 0.044(6) 0.029(5) 0.039(5) -0.006(4) 0.000(4) 0.004(4) C39 0.016(4) 0.020(4) 0.020(4) 0.002(3) -0.001(3) -0.001(3) C40 0.031(5) 0.015(4) 0.023(4) -0.004(3) 0.011(4) 0.004(3) C41 0.033(5) 0.015(4) 0.031(5) 0.004(3) 0.010(4) 0.002(3) C42 0.075(7) 0.020(4) 0.033(5) 0.002(4) 0.014(5) 0.010(4) C43 0.036(5) 0.024(4) 0.033(5) 0.005(4) -0.003(4) 0.006(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 C1S C2S 1.372(14) . ? C1S C6S 1.390(14) . ? C1S C7S 1.538(14) . ? C2S C3S 1.417(14) . ? C2S H2S 0.9500 . ? C3S C4S 1.355(13) . ? C3S H3S 0.9500 . ? C4S C5S 1.380(13) . ? C4S H4S 0.9500 . ? C5S C6S 1.352(14) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S C7S 1.38(2) 3_766 ? C7S H7S1 0.9500 . ? U1 N3 2.194(5) . ? U1 N1 2.220(5) . ? U1 N2 2.485(5) . ? U1 C6 2.504(7) . ? U1 C7 2.793(6) . ? U1 I1 3.0284(7) . ? N1 C13 1.450(8) . ? N1 C25 1.471(8) . ? N2 C39 1.347(8) . ? N2 C29 1.360(8) . ? N3 C31 1.456(8) . ? N3 C30 1.468(8) . ? C6 C7 1.447(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C12 1.412(10) . ? C7 C8 1.425(9) . ? C8 C9 1.377(10) . ? C8 H8A 0.9500 . ? C9 C10 1.383(10) . ? C9 H9A 0.9500 . ? C10 C11 1.388(10) . ? C10 H10A 0.9500 . ? C11 C12 1.379(10) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.409(9) . ? C13 C18 1.412(9) . ? C14 C15 1.424(10) . ? C14 C19 1.525(10) . ? C15 C16 1.368(10) . ? C15 H15A 0.9500 . ? C16 C17 1.364(10) . ? C16 H16A 0.9500 . ? C17 C18 1.402(9) . ? C17 H17A 0.9500 . ? C18 C22 1.517(9) . ? C19 C20 1.521(9) . ? C19 C21 1.530(9) . ? C19 H19A 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.530(10) . ? C22 C23 1.558(9) . ? C22 H22A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C39 1.497(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.367(10) . ? C26 C39 1.377(9) . ? C26 H26A 0.9500 . ? C27 C28 1.374(10) . ? C27 H27A 0.9500 . ? C28 C29 1.380(9) . ? C28 H28A 0.9500 . ? C29 C30 1.504(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C40 1.393(10) . ? C31 C32 1.420(9) . ? C32 C33 1.402(10) . ? C32 C36 1.526(10) . ? C33 C34 1.361(10) . ? C33 H33A 0.9500 . ? C34 C35 1.386(10) . ? C34 H34A 0.9500 . ? C35 C40 1.388(10) . ? C35 H35A 0.9500 . ? C36 C38 1.517(10) . ? C36 C37 1.525(10) . ? C36 H36A 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C40 C41 1.535(9) . ? C41 C42 1.513(10) . ? C41 C43 1.523(9) . ? C41 H41A 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2S C1S C6S 118.5(11) . . ? C2S C1S C7S 123.1(11) . . ? C6S C1S C7S 118.2(11) . . ? C1S C2S C3S 120.6(11) . . ? C1S C2S H2S 119.7 . . ? C3S C2S H2S 119.7 . . ? C4S C3S C2S 118.8(10) . . ? C4S C3S H3S 120.6 . . ? C2S C3S H3S 120.6 . . ? C3S C4S C5S 120.6(10) . . ? C3S C4S H4S 119.7 . . ? C5S C4S H4S 119.7 . . ? C6S C5S C4S 120.5(11) . . ? C6S C5S H5S 119.7 . . ? C4S C5S H5S 119.7 . . ? C5S C6S C1S 120.9(12) . . ? C5S C6S H6S 119.5 . . ? C1S C6S H6S 119.5 . . ? C7S C7S C1S 114.1(13) 3_766 . ? C7S C7S H7S1 123.0 3_766 . ? C1S C7S H7S1 123.0 . . ? N3 U1 N1 128.95(19) . . ? N3 U1 N2 66.20(18) . . ? N1 U1 N2 65.17(18) . . ? N3 U1 C6 102.9(2) . . ? N1 U1 C6 102.4(2) . . ? N2 U1 C6 137.6(2) . . ? N3 U1 C7 111.3(2) . . ? N1 U1 C7 113.27(19) . . ? N2 U1 C7 168.69(19) . . ? C6 U1 C7 31.1(2) . . ? N3 U1 I1 92.79(14) . . ? N1 U1 I1 107.29(14) . . ? N2 U1 I1 96.78(12) . . ? C6 U1 I1 125.27(16) . . ? C7 U1 I1 94.34(15) . . ? C13 N1 C25 116.7(5) . . ? C13 N1 U1 114.0(4) . . ? C25 N1 U1 129.1(4) . . ? C39 N2 C29 119.4(6) . . ? C39 N2 U1 121.6(4) . . ? C29 N2 U1 118.9(4) . . ? C31 N3 C30 116.6(5) . . ? C31 N3 U1 117.9(4) . . ? C30 N3 U1 124.7(4) . . ? C7 C6 U1 85.5(4) . . ? C7 C6 H6A 114.4 . . ? U1 C6 H6A 114.4 . . ? C7 C6 H6B 114.4 . . ? U1 C6 H6B 114.4 . . ? H6A C6 H6B 111.5 . . ? C12 C7 C8 115.5(7) . . ? C12 C7 C6 121.4(6) . . ? C8 C7 C6 122.3(7) . . ? C12 C7 U1 94.9(4) . . ? C8 C7 U1 103.9(4) . . ? C6 C7 U1 63.4(3) . . ? C9 C8 C7 121.0(7) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 121.1(7) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C11 120.0(7) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 118.9(7) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C7 123.3(7) . . ? C11 C12 H12A 118.3 . . ? C7 C12 H12A 118.3 . . ? C14 C13 C18 120.8(6) . . ? C14 C13 N1 118.6(6) . . ? C18 C13 N1 120.3(6) . . ? C13 C14 C15 118.0(7) . . ? C13 C14 C19 123.4(6) . . ? C15 C14 C19 118.6(7) . . ? C16 C15 C14 120.7(7) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C17 C16 C15 120.5(7) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 122.1(7) . . ? C16 C17 H17A 119.0 . . ? C18 C17 H17A 119.0 . . ? C17 C18 C13 117.7(7) . . ? C17 C18 C22 120.2(6) . . ? C13 C18 C22 121.8(6) . . ? C20 C19 C14 112.8(6) . . ? C20 C19 C21 111.0(6) . . ? C14 C19 C21 109.2(6) . . ? C20 C19 H19A 107.9 . . ? C14 C19 H19A 107.9 . . ? C21 C19 H19A 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 114.1(6) . . ? C18 C22 C23 109.3(6) . . ? C24 C22 C23 108.4(6) . . ? C18 C22 H22A 108.3 . . ? C24 C22 H22A 108.3 . . ? C23 C22 H22A 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C39 109.5(5) . . ? N1 C25 H25A 109.8 . . ? C39 C25 H25A 109.8 . . ? N1 C25 H25B 109.8 . . ? C39 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? C27 C26 C39 119.1(7) . . ? C27 C26 H26A 120.5 . . ? C39 C26 H26A 120.5 . . ? C26 C27 C28 120.3(7) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C27 C28 C29 118.9(7) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? N2 C29 C28 120.9(7) . . ? N2 C29 C30 113.5(6) . . ? C28 C29 C30 125.6(6) . . ? N3 C30 C29 109.6(6) . . ? N3 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? N3 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C40 C31 C32 121.2(7) . . ? C40 C31 N3 120.0(6) . . ? C32 C31 N3 118.7(7) . . ? C33 C32 C31 117.1(7) . . ? C33 C32 C36 119.9(6) . . ? C31 C32 C36 122.8(7) . . ? C34 C33 C32 121.6(7) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 120.7(7) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C34 C35 C40 120.1(7) . . ? C34 C35 H35A 119.9 . . ? C40 C35 H35A 119.9 . . ? C38 C36 C37 111.2(6) . . ? C38 C36 C32 109.5(6) . . ? C37 C36 C32 112.6(6) . . ? C38 C36 H36A 107.8 . . ? C37 C36 H36A 107.8 . . ? C32 C36 H36A 107.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 C26 121.4(6) . . ? N2 C39 C25 114.1(6) . . ? C26 C39 C25 124.5(6) . . ? C35 C40 C31 119.2(6) . . ? C35 C40 C41 120.3(6) . . ? C31 C40 C41 120.3(6) . . ? C42 C41 C43 110.4(6) . . ? C42 C41 C40 109.9(6) . . ? C43 C41 C40 113.2(6) . . ? C42 C41 H41A 107.7 . . ? C43 C41 H41A 107.7 . . ? C40 C41 H41A 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.765 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.150 #===END