Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Stable Analogs of the Uranyl Ion Containing 1,1,3,3-Tetramethylguanidine ; _publ_contact_author_name 'Prof. Scott Bunge' _publ_contact_author_email SBUNGE@KENT.EDU loop_ _publ_author_name 'Scott Bunge' 'Jeffrey A. Bertke' # Attachment 'BertkeBungeUranium.cif' data_bc002_mono _database_code_depnum_ccdc_archive 'CCDC 646916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(1) (UO2Cl2HTMG2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H26 Cl2 N6 O2 U' _chemical_formula_weight 571.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 P2(1)/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 7.874(2) _cell_length_b 12.918(4) _cell_length_c 9.422(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.298(4) _cell_angle_gamma 90.00 _cell_volume 915.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4309 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 30.40 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 9.173 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2268 _exptl_absorpt_correction_T_max 0.4319 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7144 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.05 _reflns_number_total 1617 _reflns_number_gt 1276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.5000P] 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 1617 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 0.685 _refine_ls_restrained_S_all 0.685 _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 U1 U 0.5000 0.5000 0.5000 0.01392(15) Uani 1 2 d S . . Cl1 Cl 0.30144(17) 0.60903(9) 0.26698(13) 0.0219(3) Uani 1 1 d . . . O1 O 0.3322(7) 0.5123(2) 0.5900(6) 0.0200(10) Uani 1 1 d . . . N1 N 0.6152(5) 0.6628(3) 0.6063(4) 0.0165(9) Uani 1 1 d . . . H1 H 0.5763 0.6851 0.6793 0.020 Uiso 1 1 calc R . . N2 N 0.8960(5) 0.6893(3) 0.5770(4) 0.0153(9) Uani 1 1 d . . . N3 N 0.6903(5) 0.8222(3) 0.5175(4) 0.0164(9) Uani 1 1 d . . . C1 C 0.7316(6) 0.7245(3) 0.5686(5) 0.0135(10) Uani 1 1 d . . . C2 C 0.9890(6) 0.7225(5) 0.4724(6) 0.0207(13) Uani 1 1 d . . . H2A H 0.9083 0.7635 0.3931 0.031 Uiso 1 1 calc R . . H2B H 1.0292 0.6616 0.4293 0.031 Uiso 1 1 calc R . . H2C H 1.0920 0.7648 0.5245 0.031 Uiso 1 1 calc R . . C3 C 0.9778(6) 0.6034(4) 0.6739(5) 0.0178(10) Uani 1 1 d . . . H3A H 0.9086 0.5884 0.7424 0.027 Uiso 1 1 calc R . . H3B H 1.0996 0.6221 0.7308 0.027 Uiso 1 1 calc R . . H3C H 0.9801 0.5420 0.6134 0.027 Uiso 1 1 calc R . . C4 C 0.8143(6) 0.9087(3) 0.5646(5) 0.0186(11) Uani 1 1 d . . . H4A H 0.7761 0.9524 0.6344 0.028 Uiso 1 1 calc R . . H4B H 0.8161 0.9497 0.4775 0.028 Uiso 1 1 calc R . . H4C H 0.9339 0.8819 0.6134 0.028 Uiso 1 1 calc R . . C5 C 0.5031(6) 0.8537(5) 0.4594(7) 0.0218(12) Uani 1 1 d . . . H5A H 0.4305 0.7937 0.4147 0.033 Uiso 1 1 calc R . . H5B H 0.4916 0.9076 0.3838 0.033 Uiso 1 1 calc R . . H5C H 0.4623 0.8808 0.5407 0.033 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 U1 0.0119(2) 0.0144(2) 0.0159(2) -0.00122(8) 0.00486(14) -0.00064(8) Cl1 0.0205(6) 0.0223(6) 0.0202(6) 0.0020(5) 0.0019(5) 0.0006(6) O1 0.014(2) 0.023(2) 0.024(2) -0.0030(14) 0.0065(19) -0.0005(14) N1 0.018(2) 0.017(2) 0.017(2) -0.0069(17) 0.0084(18) -0.0069(17) N2 0.014(2) 0.015(2) 0.018(2) 0.0034(16) 0.0056(17) 0.0026(17) N3 0.014(2) 0.0084(19) 0.023(2) 0.0001(16) -0.0003(17) -0.0011(16) C1 0.015(2) 0.016(2) 0.008(2) -0.0014(18) 0.0003(19) 0.0007(19) C2 0.018(3) 0.027(3) 0.021(2) 0.001(2) 0.011(2) -0.002(2) C3 0.017(2) 0.014(2) 0.018(2) 0.004(2) 0.000(2) 0.004(2) C4 0.018(3) 0.010(2) 0.027(3) 0.005(2) 0.005(2) -0.0005(19) C5 0.015(3) 0.019(3) 0.027(3) 0.003(2) 0.000(2) 0.0037(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 O1 1.777(5) 3_666 ? U1 O1 1.777(5) . ? U1 N1 2.390(4) 3_666 ? U1 N1 2.390(4) . ? U1 Cl1 2.6846(13) . ? U1 Cl1 2.6846(13) 3_666 ? N1 C1 1.339(6) . ? N1 H1 0.8800 . ? N2 C1 1.353(6) . ? N2 C2 1.456(6) . ? N2 C3 1.459(6) . ? N3 C1 1.355(6) . ? N3 C4 1.464(6) . ? N3 C5 1.470(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 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 O1 U1 O1 180.000(1) 3_666 . ? O1 U1 N1 87.99(15) 3_666 3_666 ? O1 U1 N1 92.01(15) . 3_666 ? O1 U1 N1 92.01(15) 3_666 . ? O1 U1 N1 87.99(15) . . ? N1 U1 N1 180.000(1) 3_666 . ? O1 U1 Cl1 89.52(15) 3_666 . ? O1 U1 Cl1 90.48(15) . . ? N1 U1 Cl1 93.60(10) 3_666 . ? N1 U1 Cl1 86.40(10) . . ? O1 U1 Cl1 90.48(15) 3_666 3_666 ? O1 U1 Cl1 89.52(15) . 3_666 ? N1 U1 Cl1 86.40(10) 3_666 3_666 ? N1 U1 Cl1 93.60(10) . 3_666 ? Cl1 U1 Cl1 180.0 . 3_666 ? C1 N1 U1 128.1(3) . . ? C1 N1 H1 116.0 . . ? U1 N1 H1 116.0 . . ? C1 N2 C2 121.8(4) . . ? C1 N2 C3 122.0(4) . . ? C2 N2 C3 115.5(4) . . ? C1 N3 C4 122.4(4) . . ? C1 N3 C5 119.9(4) . . ? C4 N3 C5 114.0(4) . . ? N1 C1 N2 120.2(4) . . ? N1 C1 N3 122.5(4) . . ? N2 C1 N3 117.3(4) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.967 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.118 #===END data_jab046_0m _database_code_depnum_ccdc_archive 'CCDC 646917' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(2) (UO2OC6H3-2,6-(C(CH3)3)2HTMG2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H68 N6 O4 U' _chemical_formula_weight 911.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.584(4) _cell_length_b 11.1983(13) _cell_length_c 23.246(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.825(2) _cell_angle_gamma 90.00 _cell_volume 8337.8(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6613 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 29.74 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 3.936 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.2436 _exptl_absorpt_correction_T_max 0.4919 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 34044 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7770 _reflns_number_gt 6553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.6695P] 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 7770 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 0.728 _refine_ls_restrained_S_all 0.728 _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 0.619051(4) 0.566636(11) 0.871340(6) 0.01428(7) Uani 1 1 d . . . O1 O 0.56764(8) 0.6242(2) 0.84172(12) 0.0196(6) Uani 1 1 d . . . O2 O 0.67008(8) 0.5055(2) 0.89932(12) 0.0207(6) Uani 1 1 d . . . O3 O 0.63584(8) 0.6969(2) 0.81217(12) 0.0167(5) Uani 1 1 d . . . O4 O 0.60785(8) 0.4423(2) 0.93823(13) 0.0157(6) Uani 1 1 d . . . N1 N 0.64595(10) 0.7332(3) 0.94894(15) 0.0206(7) Uani 1 1 d . . . H1 H 0.6724 0.7209 0.9750 0.025 Uiso 1 1 calc R . . N2 N 0.59711(11) 0.8424(3) 0.96909(17) 0.0268(8) Uani 1 1 d . . . N3 N 0.65582(12) 0.9371(3) 0.97335(18) 0.0260(8) Uani 1 1 d . . . N4 N 0.59504(10) 0.4406(2) 0.77528(16) 0.0175(7) Uani 1 1 d . . . H4 H 0.5680 0.4401 0.7507 0.021 Uiso 1 1 calc R . . N5 N 0.63930(10) 0.2788(3) 0.79263(15) 0.0213(7) Uani 1 1 d . . . N6 N 0.62204(10) 0.3941(3) 0.70185(15) 0.0193(7) Uani 1 1 d . . . C1 C 0.64677(12) 0.7808(3) 0.78164(18) 0.0178(8) Uani 1 1 d . . . C2 C 0.61678(11) 0.8696(3) 0.74387(17) 0.0178(8) Uani 1 1 d . . . C3 C 0.62964(13) 0.9572(4) 0.7133(2) 0.0228(9) Uani 1 1 d . . . H3 H 0.6103 1.0174 0.6894 0.027 Uiso 1 1 calc R . . C4 C 0.66924(14) 0.9593(4) 0.7164(2) 0.0258(9) Uani 1 1 d . . . H4A H 0.6767 1.0188 0.6942 0.031 Uiso 1 1 calc R . . C5 C 0.69792(12) 0.8738(4) 0.75239(19) 0.0224(9) Uani 1 1 d . . . H5 H 0.7253 0.8762 0.7549 0.027 Uiso 1 1 calc R . . C6 C 0.68806(12) 0.7845(3) 0.78489(17) 0.0171(8) Uani 1 1 d . . . C7 C 0.57178(12) 0.8730(3) 0.73727(18) 0.0202(8) Uani 1 1 d . . . C8 C 0.54882(12) 0.7567(4) 0.70645(19) 0.0232(8) Uani 1 1 d . . . H8A H 0.5634 0.6887 0.7336 0.035 Uiso 1 1 calc R . . H8B H 0.5483 0.7472 0.6642 0.035 Uiso 1 1 calc R . . H8C H 0.5202 0.7601 0.7020 0.035 Uiso 1 1 calc R . . C9 C 0.57238(13) 0.8935(4) 0.80330(19) 0.0224(8) Uani 1 1 d . . . H9A H 0.5910 0.8352 0.8338 0.034 Uiso 1 1 calc R . . H9B H 0.5441 0.8838 0.7998 0.034 Uiso 1 1 calc R . . H9C H 0.5824 0.9744 0.8182 0.034 Uiso 1 1 calc R . . C10 C 0.54591(13) 0.9759(4) 0.6938(2) 0.0258(9) Uani 1 1 d . . . H10A H 0.5177 0.9747 0.6912 0.039 Uiso 1 1 calc R . . H10B H 0.5444 0.9661 0.6510 0.039 Uiso 1 1 calc R . . H10C H 0.5593 1.0524 0.7118 0.039 Uiso 1 1 calc R . . C11 C 0.72209(11) 0.6932(3) 0.82443(18) 0.0187(8) Uani 1 1 d . . . C12 C 0.73253(12) 0.7049(4) 0.89574(18) 0.0235(8) Uani 1 1 d . . . H12A H 0.7071 0.6928 0.9016 0.035 Uiso 1 1 calc R . . H12B H 0.7438 0.7847 0.9109 0.035 Uiso 1 1 calc R . . H12C H 0.7533 0.6446 0.9202 0.035 Uiso 1 1 calc R . . C13 C 0.70840(13) 0.5654(3) 0.8011(2) 0.0206(9) Uani 1 1 d . . . H13A H 0.7042 0.5578 0.7567 0.031 Uiso 1 1 calc R . . H13B H 0.6822 0.5475 0.8036 0.031 Uiso 1 1 calc R . . H13C H 0.7300 0.5092 0.8280 0.031 Uiso 1 1 calc R . . C14 C 0.76310(12) 0.7140(4) 0.8191(2) 0.0259(9) Uani 1 1 d . . . H14A H 0.7838 0.6549 0.8453 0.039 Uiso 1 1 calc R . . H14B H 0.7735 0.7945 0.8343 0.039 Uiso 1 1 calc R . . H14C H 0.7582 0.7058 0.7744 0.039 Uiso 1 1 calc R . . C15 C 0.60212(11) 0.3694(3) 0.97977(17) 0.0137(7) Uani 1 1 d . . . C16 C 0.63651(11) 0.3376(3) 1.03967(17) 0.0148(7) Uani 1 1 d . . . C17 C 0.62855(12) 0.2634(3) 1.08155(18) 0.0187(8) Uani 1 1 d . . . H17 H 0.6510 0.2428 1.1213 0.022 Uiso 1 1 calc R . . C18 C 0.58917(12) 0.2188(3) 1.06726(19) 0.0220(8) Uani 1 1 d . . . H18 H 0.5846 0.1688 1.0967 0.026 Uiso 1 1 calc R . . C19 C 0.55680(12) 0.2485(4) 1.00959(18) 0.0204(8) Uani 1 1 d . . . H19 H 0.5299 0.2174 0.9998 0.024 Uiso 1 1 calc R . . C20 C 0.56146(11) 0.3218(3) 0.96470(17) 0.0160(7) Uani 1 1 d . . . C21 C 0.68139(11) 0.3815(3) 1.06003(18) 0.0188(8) Uani 1 1 d . . . C22 C 0.71121(12) 0.3409(4) 1.12794(19) 0.0274(9) Uani 1 1 d . . . H22A H 0.7005 0.3679 1.1581 0.041 Uiso 1 1 calc R . . H22B H 0.7389 0.3753 1.1399 0.041 Uiso 1 1 calc R . . H22C H 0.7132 0.2536 1.1291 0.041 Uiso 1 1 calc R . . C23 C 0.69937(12) 0.3330(3) 1.01544(19) 0.0218(8) Uani 1 1 d . . . H23A H 0.7017 0.2458 1.0193 0.033 Uiso 1 1 calc R . . H23B H 0.7271 0.3675 1.0273 0.033 Uiso 1 1 calc R . . H23C H 0.6808 0.3546 0.9712 0.033 Uiso 1 1 calc R . . C24 C 0.68274(12) 0.5184(4) 1.0615(2) 0.0234(9) Uani 1 1 d . . . H24A H 0.6639 0.5497 1.0193 0.035 Uiso 1 1 calc R . . H24B H 0.7113 0.5455 1.0728 0.035 Uiso 1 1 calc R . . H24C H 0.6738 0.5476 1.0934 0.035 Uiso 1 1 calc R . . C25 C 0.52250(11) 0.3508(4) 0.90246(18) 0.0199(8) Uani 1 1 d . . . C26 C 0.48327(13) 0.2842(4) 0.8971(2) 0.0281(9) Uani 1 1 d . . . H26A H 0.4771 0.3072 0.9327 0.042 Uiso 1 1 calc R . . H26B H 0.4882 0.1979 0.8985 0.042 Uiso 1 1 calc R . . H26C H 0.4596 0.3050 0.8566 0.042 Uiso 1 1 calc R . . C27 C 0.51300(12) 0.4842(4) 0.9009(2) 0.0284(9) Uani 1 1 d . . . H27A H 0.4887 0.5035 0.8608 0.043 Uiso 1 1 calc R . . H27B H 0.5372 0.5302 0.9036 0.043 Uiso 1 1 calc R . . H27C H 0.5071 0.5045 0.9371 0.043 Uiso 1 1 calc R . . C28 C 0.52843(12) 0.3145(4) 0.84336(19) 0.0275(9) Uani 1 1 d . . . H28A H 0.5328 0.2281 0.8439 0.041 Uiso 1 1 calc R . . H28B H 0.5528 0.3561 0.8437 0.041 Uiso 1 1 calc R . . H28C H 0.5035 0.3363 0.8047 0.041 Uiso 1 1 calc R . . C29 C 0.63328(12) 0.8341(3) 0.96362(17) 0.0217(8) Uani 1 1 d . . . C30 C 0.57580(15) 0.7354(4) 0.9752(2) 0.0328(10) Uani 1 1 d . . . H30A H 0.5534 0.7145 0.9334 0.049 Uiso 1 1 calc R . . H30B H 0.5639 0.7506 1.0055 0.049 Uiso 1 1 calc R . . H30C H 0.5958 0.6693 0.9909 0.049 Uiso 1 1 calc R . . C31 C 0.57164(16) 0.9505(4) 0.9529(3) 0.0376(12) Uani 1 1 d . . . H31A H 0.5840 1.0104 0.9356 0.056 Uiso 1 1 calc R . . H31B H 0.5705 0.9822 0.9914 0.056 Uiso 1 1 calc R . . H31C H 0.5433 0.9316 0.9209 0.056 Uiso 1 1 calc R . . C32 C 0.66037(16) 1.0212(4) 1.0248(2) 0.0400(12) Uani 1 1 d . . . H32A H 0.6466 0.9884 1.0497 0.060 Uiso 1 1 calc R . . H32B H 0.6475 1.0978 1.0061 0.060 Uiso 1 1 calc R . . H32C H 0.6901 1.0334 1.0528 0.060 Uiso 1 1 calc R . . C33 C 0.68554(14) 0.9519(4) 0.9467(2) 0.0288(10) Uani 1 1 d . . . H33A H 0.7121 0.9143 0.9750 0.043 Uiso 1 1 calc R . . H33B H 0.6900 1.0372 0.9427 0.043 Uiso 1 1 calc R . . H33C H 0.6746 0.9143 0.9045 0.043 Uiso 1 1 calc R . . C34 C 0.61809(11) 0.3737(3) 0.75644(18) 0.0183(8) Uani 1 1 d . . . C35 C 0.62486(14) 0.2233(4) 0.8361(2) 0.0286(9) Uani 1 1 d . . . H35A H 0.6362 0.2670 0.8767 0.043 Uiso 1 1 calc R . . H35B H 0.6344 0.1402 0.8438 0.043 Uiso 1 1 calc R . . H35C H 0.5943 0.2254 0.8170 0.043 Uiso 1 1 calc R . . C36 C 0.68284(13) 0.2532(4) 0.8071(2) 0.0293(9) Uani 1 1 d . . . H36A H 0.6917 0.3050 0.7813 0.044 Uiso 1 1 calc R . . H36B H 0.6855 0.1695 0.7972 0.044 Uiso 1 1 calc R . . H36C H 0.7005 0.2680 0.8525 0.044 Uiso 1 1 calc R . . C37 C 0.63030(13) 0.2989(4) 0.6665(2) 0.0265(9) Uani 1 1 d . . . H37A H 0.6299 0.2219 0.6862 0.040 Uiso 1 1 calc R . . H37B H 0.6578 0.3111 0.6673 0.040 Uiso 1 1 calc R . . H37C H 0.6088 0.2995 0.6221 0.040 Uiso 1 1 calc R . . C38 C 0.61067(12) 0.5091(3) 0.66965(19) 0.0219(8) Uani 1 1 d . . . H38A H 0.5811 0.5082 0.6391 0.033 Uiso 1 1 calc R . . H38B H 0.6277 0.5244 0.6468 0.033 Uiso 1 1 calc R . . H38C H 0.6155 0.5722 0.7013 0.033 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 U1 0.01498(10) 0.01344(10) 0.01682(10) 0.00075(5) 0.00917(7) -0.00090(5) O1 0.0188(13) 0.0174(14) 0.0251(14) 0.0026(11) 0.0119(12) -0.0012(11) O2 0.0191(13) 0.0236(15) 0.0219(14) 0.0032(11) 0.0112(11) -0.0013(11) O3 0.0168(12) 0.0152(13) 0.0202(13) 0.0004(11) 0.0099(11) -0.0029(11) O4 0.0152(13) 0.0175(14) 0.0149(13) 0.0025(10) 0.0071(11) -0.0001(9) N1 0.0192(17) 0.0165(16) 0.0225(17) -0.0008(13) 0.0057(14) 0.0013(13) N2 0.0272(18) 0.0244(18) 0.0303(19) -0.0035(15) 0.0138(16) 0.0006(15) N3 0.034(2) 0.0172(18) 0.030(2) -0.0061(14) 0.0170(18) -0.0028(13) N4 0.0105(15) 0.0201(17) 0.0201(17) -0.0021(12) 0.0048(13) -0.0037(12) N5 0.0219(17) 0.0175(17) 0.0244(17) 0.0017(13) 0.0100(14) 0.0038(13) N6 0.0174(16) 0.0182(16) 0.0243(18) -0.0013(14) 0.0110(14) -0.0008(13) C1 0.023(2) 0.0156(19) 0.0181(19) -0.0036(15) 0.0120(16) -0.0045(15) C2 0.0202(19) 0.0164(19) 0.0175(19) -0.0022(15) 0.0090(16) -0.0062(15) C3 0.032(2) 0.0176(19) 0.022(2) -0.0021(16) 0.0146(18) -0.0040(17) C4 0.036(2) 0.022(2) 0.029(2) 0.0004(17) 0.022(2) -0.0091(18) C5 0.024(2) 0.024(2) 0.029(2) -0.0083(17) 0.0202(18) -0.0099(16) C6 0.0226(19) 0.0142(19) 0.0166(18) -0.0049(15) 0.0107(16) -0.0044(15) C7 0.025(2) 0.017(2) 0.0183(19) 0.0028(15) 0.0090(16) 0.0013(16) C8 0.021(2) 0.026(2) 0.022(2) -0.0002(17) 0.0090(17) -0.0050(17) C9 0.026(2) 0.0175(19) 0.028(2) 0.0021(17) 0.0163(18) 0.0026(17) C10 0.025(2) 0.023(2) 0.029(2) 0.0051(18) 0.0106(18) 0.0031(18) C11 0.0156(18) 0.0195(19) 0.024(2) -0.0020(16) 0.0113(16) -0.0043(15) C12 0.0183(19) 0.030(2) 0.023(2) -0.0029(17) 0.0097(16) -0.0044(17) C13 0.015(2) 0.023(2) 0.023(2) -0.0016(15) 0.0088(17) 0.0000(14) C14 0.019(2) 0.032(2) 0.030(2) -0.0076(18) 0.0135(18) -0.0068(17) C15 0.0157(18) 0.0127(18) 0.0150(18) -0.0001(14) 0.0088(15) 0.0005(14) C16 0.0168(18) 0.0131(17) 0.0151(18) -0.0039(14) 0.0076(15) 0.0011(14) C17 0.024(2) 0.0150(18) 0.0158(18) 0.0007(15) 0.0073(16) 0.0028(15) C18 0.030(2) 0.019(2) 0.023(2) 0.0011(16) 0.0171(18) -0.0010(16) C19 0.020(2) 0.0224(19) 0.022(2) 0.0020(16) 0.0123(16) -0.0025(16) C20 0.0155(18) 0.0158(19) 0.0187(18) 0.0006(15) 0.0094(15) 0.0003(14) C21 0.0169(18) 0.0168(19) 0.021(2) 0.0010(16) 0.0070(16) 0.0017(15) C22 0.0182(19) 0.035(2) 0.021(2) 0.0019(18) 0.0020(16) 0.0003(17) C23 0.0201(19) 0.023(2) 0.027(2) 0.0041(16) 0.0138(17) 0.0021(15) C24 0.0177(19) 0.023(2) 0.027(2) -0.0035(17) 0.0072(17) -0.0067(16) C25 0.0168(19) 0.027(2) 0.0170(19) 0.0004(16) 0.0079(16) -0.0027(16) C26 0.023(2) 0.031(2) 0.030(2) 0.0022(18) 0.0110(18) -0.0078(17) C27 0.020(2) 0.029(2) 0.037(2) 0.009(2) 0.0133(19) 0.0039(18) C28 0.021(2) 0.041(3) 0.020(2) -0.0027(18) 0.0085(17) -0.0092(18) C29 0.029(2) 0.022(2) 0.0130(18) 0.0001(15) 0.0082(16) 0.0004(17) C30 0.038(3) 0.032(2) 0.040(3) -0.004(2) 0.027(2) -0.008(2) C31 0.032(3) 0.039(3) 0.043(3) -0.001(2) 0.017(2) 0.014(2) C32 0.044(3) 0.027(2) 0.048(3) -0.017(2) 0.019(2) -0.006(2) C33 0.030(2) 0.022(2) 0.036(3) 0.0013(18) 0.016(2) -0.0050(17) C34 0.0155(18) 0.0131(18) 0.024(2) -0.0032(15) 0.0067(16) -0.0030(14) C35 0.040(3) 0.020(2) 0.027(2) 0.0026(17) 0.015(2) -0.0032(18) C36 0.022(2) 0.023(2) 0.039(3) -0.0026(19) 0.0086(19) 0.0013(17) C37 0.027(2) 0.026(2) 0.031(2) -0.0051(18) 0.0170(18) 0.0013(18) C38 0.0202(19) 0.021(2) 0.026(2) 0.0014(17) 0.0116(17) -0.0009(16) _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 O1 1.772(3) . ? U1 O2 1.778(3) . ? U1 O4 2.248(2) . ? U1 O3 2.256(2) . ? U1 N4 2.459(3) . ? U1 N1 2.478(3) . ? O3 C1 1.334(4) . ? O4 C15 1.347(4) . ? N1 C29 1.316(5) . ? N1 H1 0.8800 . ? N2 C29 1.351(5) . ? N2 C30 1.457(5) . ? N2 C31 1.460(5) . ? N3 C29 1.366(5) . ? N3 C33 1.449(6) . ? N3 C32 1.475(5) . ? N4 C34 1.319(5) . ? N4 H4 0.8800 . ? N5 C34 1.361(5) . ? N5 C35 1.457(5) . ? N5 C36 1.464(5) . ? N6 C34 1.356(5) . ? N6 C37 1.452(5) . ? N6 C38 1.456(5) . ? C1 C6 1.439(5) . ? C1 C2 1.443(5) . ? C2 C3 1.400(5) . ? C2 C7 1.541(5) . ? C3 C4 1.379(6) . ? C3 H3 0.9500 . ? C4 C5 1.384(6) . ? C4 H4A 0.9500 . ? C5 C6 1.387(5) . ? C5 H5 0.9500 . ? C6 C11 1.546(5) . ? C7 C8 1.539(5) . ? C7 C9 1.543(5) . ? C7 C10 1.544(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.533(5) . ? C11 C14 1.535(5) . ? C11 C12 1.538(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.435(5) . ? C15 C16 1.442(5) . ? C16 C17 1.399(5) . ? C16 C21 1.536(5) . ? C17 C18 1.385(5) . ? C17 H17 0.9500 . ? C18 C19 1.374(5) . ? C18 H18 0.9500 . ? C19 C20 1.393(5) . ? C19 H19 0.9500 . ? C20 C25 1.541(5) . ? C21 C24 1.534(6) . ? C21 C23 1.535(5) . ? C21 C22 1.538(5) . ? 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 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.529(6) . ? C25 C28 1.533(5) . ? C25 C26 1.539(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 O1 U1 O2 178.31(12) . . ? O1 U1 O4 91.71(10) . . ? O2 U1 O4 88.23(10) . . ? O1 U1 O3 91.75(10) . . ? O2 U1 O3 88.43(10) . . ? O4 U1 O3 174.60(9) . . ? O1 U1 N4 87.97(11) . . ? O2 U1 N4 90.38(11) . . ? O4 U1 N4 100.17(10) . . ? O3 U1 N4 84.09(10) . . ? O1 U1 N1 90.86(11) . . ? O2 U1 N1 90.83(11) . . ? O4 U1 N1 95.23(10) . . ? O3 U1 N1 80.59(10) . . ? N4 U1 N1 164.59(10) . . ? C1 O3 U1 174.8(2) . . ? C15 O4 U1 178.3(3) . . ? C29 N1 U1 140.2(3) . . ? C29 N1 H1 109.9 . . ? U1 N1 H1 109.9 . . ? C29 N2 C30 120.7(4) . . ? C29 N2 C31 122.8(4) . . ? C30 N2 C31 114.6(4) . . ? C29 N3 C33 120.7(3) . . ? C29 N3 C32 121.5(4) . . ? C33 N3 C32 115.5(4) . . ? C34 N4 U1 127.4(3) . . ? C34 N4 H4 116.3 . . ? U1 N4 H4 116.3 . . ? C34 N5 C35 119.6(3) . . ? C34 N5 C36 122.8(3) . . ? C35 N5 C36 114.5(3) . . ? C34 N6 C37 122.4(3) . . ? C34 N6 C38 120.8(3) . . ? C37 N6 C38 116.0(3) . . ? O3 C1 C6 121.4(3) . . ? O3 C1 C2 120.0(3) . . ? C6 C1 C2 118.6(3) . . ? C3 C2 C1 118.2(3) . . ? C3 C2 C7 119.2(3) . . ? C1 C2 C7 122.6(3) . . ? C4 C3 C2 122.5(4) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C6 122.2(4) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.2(4) . . ? C5 C6 C11 118.8(3) . . ? C1 C6 C11 122.0(3) . . ? C8 C7 C2 110.1(3) . . ? C8 C7 C9 111.3(3) . . ? C2 C7 C9 110.0(3) . . ? C8 C7 C10 106.4(3) . . ? C2 C7 C10 112.4(3) . . ? C9 C7 C10 106.6(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 106.3(3) . . ? C13 C11 C12 110.6(3) . . ? C14 C11 C12 106.4(3) . . ? C13 C11 C6 111.2(3) . . ? C14 C11 C6 112.2(3) . . ? C12 C11 C6 110.1(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 C20 120.1(3) . . ? O4 C15 C16 120.8(3) . . ? C20 C15 C16 119.0(3) . . ? C17 C16 C15 118.4(3) . . ? C17 C16 C21 118.3(3) . . ? C15 C16 C21 123.3(3) . . ? C18 C17 C16 122.5(3) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.7 . . ? C19 C18 C17 118.5(4) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 123.4(4) . . ? C18 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C15 118.2(3) . . ? C19 C20 C25 118.4(3) . . ? C15 C20 C25 123.4(3) . . ? C24 C21 C23 110.6(3) . . ? C24 C21 C16 110.2(3) . . ? C23 C21 C16 111.2(3) . . ? C24 C21 C22 105.8(3) . . ? C23 C21 C22 106.5(3) . . ? C16 C21 C22 112.4(3) . . ? 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 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 110.6(3) . . ? C27 C25 C26 106.8(3) . . ? C28 C25 C26 105.9(3) . . ? C27 C25 C20 109.2(3) . . ? C28 C25 C20 111.5(3) . . ? C26 C25 C20 112.8(3) . . ? 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 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 N2 122.1(4) . . ? N1 C29 N3 121.7(4) . . ? N2 C29 N3 116.2(4) . . ? N2 C30 H30A 109.5 . . ? N2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 N6 123.2(3) . . ? N4 C34 N5 119.7(4) . . ? N6 C34 N5 117.0(3) . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 H37A 109.5 . . ? N6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 H38A 109.5 . . ? N6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.479 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.093 #===END data_jab049_mono _database_code_depnum_ccdc_archive 'CCDC 646918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(2a) (UO2OC6H3-2,6-(C(CH3)3)2HTMG2)*2TOL' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H84 N6 O4 U' _chemical_formula_weight 1095.28 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 P2(1)/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 23.403(3) _cell_length_b 11.0272(12) _cell_length_c 20.892(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.000(2) _cell_angle_gamma 90.00 _cell_volume 5253.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7804 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.07 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 3.137 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3980 _exptl_absorpt_correction_T_max 0.6337 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 41234 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 25.05 _reflns_number_total 9305 _reflns_number_gt 7040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.2498P] 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 9305 _refine_ls_number_parameters 590 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 0.788 _refine_ls_restrained_S_all 0.788 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.249754(8) 0.451246(16) 0.168201(9) 0.01066(8) Uani 1 1 d . . . O1 O 0.17967(16) 0.5958(3) 0.16214(18) 0.0140(8) Uani 1 1 d . . . O2 O 0.32096(15) 0.3101(3) 0.17868(17) 0.0118(8) Uani 1 1 d . . . O3 O 0.26232(16) 0.4991(3) 0.09107(18) 0.0148(8) Uani 1 1 d . . . O4 O 0.23672(17) 0.4014(3) 0.24431(18) 0.0164(8) Uani 1 1 d . . . N1 N 0.31473(19) 0.6122(4) 0.2243(2) 0.0156(10) Uani 1 1 d . . . H1A H 0.3190 0.6081 0.2672 0.019 Uiso 1 1 calc R . . N2 N 0.3798(2) 0.6864(4) 0.1646(2) 0.0164(10) Uani 1 1 d . . . N3 N 0.3423(2) 0.8173(4) 0.2315(2) 0.0166(10) Uani 1 1 d . . . N4 N 0.17010(19) 0.3276(4) 0.1054(2) 0.0159(10) Uani 1 1 d . . . H4 H 0.1722 0.3188 0.0641 0.019 Uiso 1 1 calc R . . N5 N 0.1315(2) 0.1829(4) 0.1652(2) 0.0165(10) Uani 1 1 d . . . N6 N 0.0674(2) 0.3003(4) 0.0884(2) 0.0178(10) Uani 1 1 d . . . C1 C 0.1383(2) 0.6809(5) 0.1597(3) 0.0119(11) Uani 1 1 d . . . C2 C 0.1048(2) 0.6848(5) 0.2101(3) 0.0149(12) Uani 1 1 d . . . C3 C 0.0597(2) 0.7695(5) 0.2033(3) 0.0175(12) Uani 1 1 d . . . H3 H 0.0365 0.7707 0.2352 0.021 Uiso 1 1 calc R . . C4 C 0.0473(2) 0.8519(5) 0.1523(3) 0.0216(13) Uani 1 1 d . . . H4A H 0.0159 0.9078 0.1489 0.026 Uiso 1 1 calc R . . C5 C 0.0812(2) 0.8516(5) 0.1064(3) 0.0178(12) Uani 1 1 d . . . H5 H 0.0733 0.9098 0.0720 0.021 Uiso 1 1 calc R . . C6 C 0.1269(2) 0.7690(5) 0.1083(3) 0.0151(12) Uani 1 1 d . . . C7 C 0.1162(2) 0.5972(5) 0.2688(3) 0.0159(12) Uani 1 1 d . . . C8 C 0.0759(3) 0.6214(5) 0.3162(3) 0.0237(14) Uani 1 1 d . . . H8A H 0.0810 0.7054 0.3319 0.036 Uiso 1 1 calc R . . H8B H 0.0861 0.5660 0.3537 0.036 Uiso 1 1 calc R . . H8C H 0.0350 0.6084 0.2934 0.036 Uiso 1 1 calc R . . C9 C 0.1044(3) 0.4657(5) 0.2444(3) 0.0189(13) Uani 1 1 d . . . H9A H 0.0629 0.4569 0.2226 0.028 Uiso 1 1 calc R . . H9B H 0.1140 0.4101 0.2819 0.028 Uiso 1 1 calc R . . H9C H 0.1288 0.4466 0.2133 0.028 Uiso 1 1 calc R . . C10 C 0.1797(2) 0.6129(5) 0.3094(3) 0.0171(12) Uani 1 1 d . . . H10A H 0.2071 0.6070 0.2803 0.026 Uiso 1 1 calc R . . H10B H 0.1884 0.5492 0.3429 0.026 Uiso 1 1 calc R . . H10C H 0.1837 0.6925 0.3308 0.026 Uiso 1 1 calc R . . C11 C 0.1633(2) 0.7754(5) 0.0550(3) 0.0173(12) Uani 1 1 d . . . C12 C 0.1523(2) 0.6599(5) 0.0118(3) 0.0187(12) Uani 1 1 d . . . H12A H 0.1632 0.5881 0.0394 0.028 Uiso 1 1 calc R . . H12B H 0.1761 0.6633 -0.0213 0.028 Uiso 1 1 calc R . . H12C H 0.1107 0.6553 -0.0102 0.028 Uiso 1 1 calc R . . C13 C 0.2290(2) 0.7915(5) 0.0870(3) 0.0197(13) Uani 1 1 d . . . H13A H 0.2349 0.8679 0.1115 0.030 Uiso 1 1 calc R . . H13B H 0.2515 0.7929 0.0527 0.030 Uiso 1 1 calc R . . H13C H 0.2424 0.7238 0.1170 0.030 Uiso 1 1 calc R . . C14 C 0.1463(3) 0.8849(5) 0.0084(3) 0.0216(13) Uani 1 1 d . . . H14A H 0.1050 0.8782 -0.0144 0.032 Uiso 1 1 calc R . . H14B H 0.1708 0.8856 -0.0239 0.032 Uiso 1 1 calc R . . H14C H 0.1524 0.9602 0.0339 0.032 Uiso 1 1 calc R . . C15 C 0.3702(2) 0.2436(5) 0.1870(3) 0.0135(11) Uani 1 1 d . . . C16 C 0.4079(2) 0.2284(5) 0.2512(3) 0.0125(11) Uani 1 1 d . . . C17 C 0.4630(2) 0.1801(5) 0.2554(3) 0.0168(12) Uani 1 1 d . . . H17 H 0.4893 0.1774 0.2973 0.020 Uiso 1 1 calc R . . C18 C 0.4820(3) 0.1355(6) 0.2020(3) 0.0239(14) Uani 1 1 d . . . H18 H 0.5208 0.1060 0.2065 0.029 Uiso 1 1 calc R . . C19 C 0.4425(3) 0.1352(5) 0.1417(3) 0.0196(12) Uani 1 1 d . . . H19 H 0.4539 0.0978 0.1055 0.024 Uiso 1 1 calc R . . C20 C 0.3870(2) 0.1870(5) 0.1317(3) 0.0126(11) Uani 1 1 d . . . C21 C 0.3890(2) 0.2620(5) 0.3151(3) 0.0137(11) Uani 1 1 d . . . C22 C 0.3295(2) 0.2030(5) 0.3154(3) 0.0158(12) Uani 1 1 d . . . H22A H 0.3153 0.2327 0.3532 0.024 Uiso 1 1 calc R . . H22B H 0.3342 0.1148 0.3184 0.024 Uiso 1 1 calc R . . H22C H 0.3012 0.2241 0.2748 0.024 Uiso 1 1 calc R . . C23 C 0.4320(2) 0.2114(5) 0.3765(3) 0.0189(12) Uani 1 1 d . . . H23A H 0.4704 0.2498 0.3808 0.028 Uiso 1 1 calc R . . H23B H 0.4359 0.1235 0.3719 0.028 Uiso 1 1 calc R . . H23C H 0.4170 0.2287 0.4157 0.028 Uiso 1 1 calc R . . C24 C 0.3871(3) 0.3989(5) 0.3242(3) 0.0187(12) Uani 1 1 d . . . H24A H 0.3588 0.4347 0.2872 0.028 Uiso 1 1 calc R . . H24B H 0.4261 0.4331 0.3259 0.028 Uiso 1 1 calc R . . H24C H 0.3753 0.4171 0.3653 0.028 Uiso 1 1 calc R . . C25 C 0.3464(2) 0.1821(5) 0.0626(3) 0.0152(12) Uani 1 1 d . . . C26 C 0.2851(3) 0.1380(5) 0.0650(3) 0.0210(13) Uani 1 1 d . . . H26A H 0.2649 0.2011 0.0846 0.032 Uiso 1 1 calc R . . H26B H 0.2882 0.0642 0.0917 0.032 Uiso 1 1 calc R . . H26C H 0.2628 0.1205 0.0204 0.032 Uiso 1 1 calc R . . C27 C 0.3440(2) 0.3074(5) 0.0304(3) 0.0166(12) Uani 1 1 d . . . H27A H 0.3199 0.3031 -0.0144 0.025 Uiso 1 1 calc R . . H27B H 0.3838 0.3332 0.0291 0.025 Uiso 1 1 calc R . . H27C H 0.3268 0.3658 0.0560 0.025 Uiso 1 1 calc R . . C28 C 0.3696(3) 0.0937(5) 0.0171(3) 0.0235(14) Uani 1 1 d . . . H28A H 0.3768 0.0143 0.0385 0.035 Uiso 1 1 calc R . . H28B H 0.4062 0.1253 0.0085 0.035 Uiso 1 1 calc R . . H28C H 0.3404 0.0854 -0.0244 0.035 Uiso 1 1 calc R . . C29 C 0.3450(2) 0.7031(5) 0.2075(3) 0.0139(12) Uani 1 1 d . . . C30 C 0.3979(3) 0.5656(5) 0.1490(3) 0.0212(13) Uani 1 1 d . . . H30A H 0.3959 0.5100 0.1850 0.032 Uiso 1 1 calc R . . H30B H 0.4382 0.5688 0.1431 0.032 Uiso 1 1 calc R . . H30C H 0.3718 0.5368 0.1084 0.032 Uiso 1 1 calc R . . C31 C 0.3889(3) 0.7829(5) 0.1190(3) 0.0215(13) Uani 1 1 d . . . H31A H 0.3623 0.8507 0.1213 0.032 Uiso 1 1 calc R . . H31B H 0.3808 0.7508 0.0741 0.032 Uiso 1 1 calc R . . H31C H 0.4296 0.8112 0.1313 0.032 Uiso 1 1 calc R . . C32 C 0.3940(3) 0.8981(5) 0.2480(3) 0.0219(13) Uani 1 1 d . . . H32A H 0.4282 0.8563 0.2387 0.033 Uiso 1 1 calc R . . H32B H 0.4017 0.9193 0.2947 0.033 Uiso 1 1 calc R . . H32C H 0.3863 0.9721 0.2214 0.033 Uiso 1 1 calc R . . C33 C 0.2925(3) 0.8550(5) 0.2580(3) 0.0204(12) Uani 1 1 d . . . H33A H 0.2581 0.8063 0.2381 0.031 Uiso 1 1 calc R . . H33B H 0.2841 0.9409 0.2480 0.031 Uiso 1 1 calc R . . H33C H 0.3019 0.8432 0.3057 0.031 Uiso 1 1 calc R . . C34 C 0.1245(2) 0.2708(5) 0.1192(3) 0.0134(11) Uani 1 1 d . . . C35 C 0.0904(2) 0.1662(5) 0.2083(3) 0.0187(12) Uani 1 1 d . . . H35A H 0.0581 0.2244 0.1962 0.028 Uiso 1 1 calc R . . H35B H 0.1110 0.1797 0.2540 0.028 Uiso 1 1 calc R . . H35C H 0.0747 0.0835 0.2033 0.028 Uiso 1 1 calc R . . C36 C 0.1867(2) 0.1199(5) 0.1869(3) 0.0227(14) Uani 1 1 d . . . H36A H 0.2104 0.1299 0.1541 0.034 Uiso 1 1 calc R . . H36B H 0.1793 0.0335 0.1923 0.034 Uiso 1 1 calc R . . H36C H 0.2078 0.1538 0.2290 0.034 Uiso 1 1 calc R . . C37 C 0.0549(3) 0.4189(5) 0.0579(3) 0.0240(14) Uani 1 1 d . . . H37A H 0.0818 0.4791 0.0829 0.036 Uiso 1 1 calc R . . H37B H 0.0144 0.4418 0.0575 0.036 Uiso 1 1 calc R . . H37C H 0.0602 0.4157 0.0127 0.036 Uiso 1 1 calc R . . C38 C 0.0223(3) 0.2089(6) 0.0693(3) 0.0243(14) Uani 1 1 d . . . H38A H 0.0381 0.1293 0.0849 0.036 Uiso 1 1 calc R . . H38B H 0.0092 0.2074 0.0214 0.036 Uiso 1 1 calc R . . H38C H -0.0110 0.2281 0.0888 0.036 Uiso 1 1 calc R . . C39 C 0.1268(3) 0.1874(6) 0.4043(3) 0.0257(14) Uani 1 1 d . . . C40 C 0.1810(3) 0.1515(6) 0.3955(3) 0.0303(15) Uani 1 1 d . . . H40 H 0.2140 0.2024 0.4107 0.036 Uiso 1 1 calc R . . C41 C 0.1885(3) 0.0424(6) 0.3649(4) 0.0362(17) Uani 1 1 d . . . H41 H 0.2262 0.0189 0.3598 0.043 Uiso 1 1 calc R . . C42 C 0.1404(3) -0.0317(6) 0.3420(3) 0.0317(16) Uani 1 1 d . . . H42 H 0.1451 -0.1066 0.3213 0.038 Uiso 1 1 calc R . . C43 C 0.0850(3) 0.0041(6) 0.3493(3) 0.0315(16) Uani 1 1 d . . . H43 H 0.0518 -0.0459 0.3333 0.038 Uiso 1 1 calc R . . C44 C 0.0787(3) 0.1127(6) 0.3800(3) 0.0252(14) Uani 1 1 d . . . H44 H 0.0409 0.1369 0.3846 0.030 Uiso 1 1 calc R . . C45 C 0.1194(3) 0.3077(6) 0.4366(3) 0.0381(18) Uani 1 1 d . . . H45A H 0.1407 0.3057 0.4827 0.057 Uiso 1 1 calc R . . H45B H 0.0776 0.3222 0.4344 0.057 Uiso 1 1 calc R . . H45C H 0.1350 0.3731 0.4137 0.057 Uiso 1 1 calc R . . C46 C 0.4146(3) 0.8240(5) 0.4335(3) 0.0213(13) Uani 1 1 d . . . C47 C 0.3919(3) 0.7102(6) 0.4108(3) 0.0271(15) Uani 1 1 d . . . H47 H 0.4161 0.6532 0.3953 0.033 Uiso 1 1 calc R . . C48 C 0.3347(3) 0.6805(6) 0.4110(3) 0.0271(15) Uani 1 1 d . . . H48 H 0.3196 0.6033 0.3954 0.033 Uiso 1 1 calc R . . C49 C 0.2990(3) 0.7626(6) 0.4337(3) 0.0257(14) Uani 1 1 d . . . H49 H 0.2595 0.7421 0.4337 0.031 Uiso 1 1 calc R . . C50 C 0.3213(3) 0.8742(6) 0.4563(3) 0.0274(15) Uani 1 1 d . . . H50 H 0.2972 0.9306 0.4723 0.033 Uiso 1 1 calc R . . C51 C 0.3782(3) 0.9046(6) 0.4559(3) 0.0235(14) Uani 1 1 d . . . H51 H 0.3927 0.9823 0.4712 0.028 Uiso 1 1 calc R . . C52 C 0.4780(3) 0.8550(6) 0.4345(3) 0.0314(15) Uani 1 1 d . . . H52A H 0.4840 0.9425 0.4409 0.047 Uiso 1 1 calc R . . H52B H 0.4870 0.8312 0.3926 0.047 Uiso 1 1 calc R . . H52C H 0.5038 0.8113 0.4705 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 U1 0.01213(12) 0.00917(12) 0.01159(12) 0.00085(8) 0.00457(8) 0.00065(8) O1 0.019(2) 0.0107(18) 0.0130(19) 0.0012(16) 0.0056(16) 0.0016(16) O2 0.0127(19) 0.0096(18) 0.0132(19) -0.0014(15) 0.0034(15) 0.0009(15) O3 0.018(2) 0.0112(18) 0.016(2) 0.0033(16) 0.0055(16) -0.0002(16) O4 0.021(2) 0.0143(19) 0.015(2) 0.0035(16) 0.0048(17) 0.0049(17) N1 0.019(3) 0.013(2) 0.014(2) -0.0013(19) 0.003(2) 0.000(2) N2 0.019(3) 0.013(2) 0.018(2) -0.003(2) 0.006(2) 0.000(2) N3 0.017(2) 0.014(2) 0.020(3) 0.000(2) 0.005(2) -0.0014(19) N4 0.019(3) 0.016(2) 0.014(2) -0.0004(19) 0.005(2) 0.000(2) N5 0.020(3) 0.011(2) 0.019(3) 0.0027(19) 0.007(2) 0.001(2) N6 0.018(3) 0.018(2) 0.016(2) 0.004(2) 0.001(2) -0.002(2) C1 0.012(3) 0.010(3) 0.014(3) -0.003(2) 0.002(2) -0.003(2) C2 0.014(3) 0.015(3) 0.015(3) -0.006(2) 0.004(2) -0.002(2) C3 0.013(3) 0.017(3) 0.023(3) -0.009(2) 0.005(2) 0.002(2) C4 0.019(3) 0.016(3) 0.027(3) -0.005(3) -0.001(3) 0.008(3) C5 0.023(3) 0.012(3) 0.015(3) 0.002(2) -0.003(2) 0.000(2) C6 0.017(3) 0.013(3) 0.013(3) -0.001(2) 0.000(2) -0.004(2) C7 0.016(3) 0.018(3) 0.015(3) 0.000(2) 0.007(2) 0.001(2) C8 0.024(3) 0.024(3) 0.026(3) -0.002(3) 0.012(3) 0.003(3) C9 0.021(3) 0.018(3) 0.020(3) -0.001(2) 0.009(2) -0.001(2) C10 0.023(3) 0.015(3) 0.011(3) 0.000(2) 0.001(2) 0.001(2) C11 0.024(3) 0.012(3) 0.016(3) 0.004(2) 0.006(2) -0.002(2) C12 0.019(3) 0.021(3) 0.014(3) 0.001(2) 0.001(2) -0.001(3) C13 0.025(3) 0.015(3) 0.020(3) 0.002(2) 0.006(3) -0.003(2) C14 0.024(3) 0.021(3) 0.017(3) 0.008(2) -0.001(2) -0.001(3) C15 0.012(3) 0.010(3) 0.020(3) -0.001(2) 0.006(2) -0.003(2) C16 0.020(3) 0.007(3) 0.012(3) -0.002(2) 0.005(2) -0.002(2) C17 0.015(3) 0.021(3) 0.014(3) 0.004(2) 0.003(2) -0.001(2) C18 0.021(3) 0.026(3) 0.028(3) 0.008(3) 0.011(3) 0.009(3) C19 0.026(3) 0.018(3) 0.018(3) 0.001(2) 0.011(3) 0.001(3) C20 0.018(3) 0.008(3) 0.012(3) 0.000(2) 0.006(2) 0.000(2) C21 0.017(3) 0.015(3) 0.011(3) -0.001(2) 0.006(2) 0.002(2) C22 0.015(3) 0.017(3) 0.016(3) -0.001(2) 0.005(2) -0.001(2) C23 0.022(3) 0.020(3) 0.015(3) 0.005(2) 0.004(2) 0.000(2) C24 0.025(3) 0.019(3) 0.012(3) 0.001(2) 0.005(2) 0.000(3) C25 0.020(3) 0.011(3) 0.015(3) -0.005(2) 0.006(2) -0.004(2) C26 0.030(3) 0.018(3) 0.017(3) -0.007(2) 0.011(3) -0.003(3) C27 0.022(3) 0.016(3) 0.014(3) 0.003(2) 0.007(2) 0.004(2) C28 0.038(4) 0.015(3) 0.019(3) -0.004(3) 0.009(3) 0.005(3) C29 0.016(3) 0.016(3) 0.009(3) -0.002(2) 0.000(2) 0.002(2) C30 0.013(3) 0.021(3) 0.031(3) -0.009(3) 0.007(3) 0.000(2) C31 0.023(3) 0.021(3) 0.023(3) 0.002(3) 0.011(3) -0.003(3) C32 0.025(3) 0.017(3) 0.025(3) -0.002(3) 0.008(3) -0.006(3) C33 0.026(3) 0.019(3) 0.019(3) -0.003(3) 0.011(3) 0.003(3) C34 0.014(3) 0.013(3) 0.015(3) -0.006(2) 0.005(2) -0.003(2) C35 0.017(3) 0.020(3) 0.021(3) 0.003(2) 0.008(2) -0.004(2) C36 0.017(3) 0.023(3) 0.029(3) 0.011(3) 0.009(3) 0.002(3) C37 0.022(3) 0.022(3) 0.026(3) 0.007(3) 0.001(3) 0.003(3) C38 0.019(3) 0.030(3) 0.022(3) 0.002(3) 0.003(3) -0.006(3) C39 0.036(4) 0.024(3) 0.016(3) 0.005(3) 0.002(3) 0.004(3) C40 0.026(3) 0.037(4) 0.024(3) 0.001(3) -0.003(3) 0.000(3) C41 0.031(4) 0.041(4) 0.036(4) 0.010(3) 0.006(3) 0.019(3) C42 0.046(4) 0.022(3) 0.027(4) 0.008(3) 0.008(3) 0.008(3) C43 0.046(4) 0.027(3) 0.019(3) 0.008(3) 0.002(3) -0.007(3) C44 0.031(4) 0.034(4) 0.011(3) 0.008(3) 0.005(3) 0.009(3) C45 0.049(5) 0.027(4) 0.035(4) 0.005(3) 0.004(3) 0.004(3) C46 0.030(3) 0.016(3) 0.017(3) 0.003(2) 0.004(3) 0.003(3) C47 0.034(4) 0.026(3) 0.024(3) 0.003(3) 0.010(3) 0.011(3) C48 0.041(4) 0.023(3) 0.019(3) 0.002(3) 0.008(3) -0.001(3) C49 0.022(3) 0.041(4) 0.014(3) 0.002(3) 0.005(3) -0.001(3) C50 0.029(4) 0.035(4) 0.019(3) -0.001(3) 0.006(3) 0.013(3) C51 0.037(4) 0.019(3) 0.015(3) -0.001(2) 0.008(3) 0.004(3) C52 0.028(4) 0.035(4) 0.033(4) -0.004(3) 0.011(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O4 1.773(4) . ? U1 O3 1.782(4) . ? U1 O2 2.255(3) . ? U1 O1 2.270(4) . ? U1 N4 2.440(4) . ? U1 N1 2.456(4) . ? O1 C1 1.341(6) . ? O2 C15 1.344(6) . ? N1 C29 1.320(7) . ? N1 H1A 0.8800 . ? N2 C29 1.352(7) . ? N2 C30 1.456(7) . ? N2 C31 1.476(7) . ? N3 C29 1.362(7) . ? N3 C33 1.459(7) . ? N3 C32 1.479(7) . ? N4 C34 1.323(7) . ? N4 H4 0.8800 . ? N5 C34 1.349(7) . ? N5 C36 1.448(7) . ? N5 C35 1.468(7) . ? N6 C34 1.385(7) . ? N6 C38 1.450(7) . ? N6 C37 1.456(7) . ? C1 C6 1.427(7) . ? C1 C2 1.448(7) . ? C2 C3 1.393(7) . ? C2 C7 1.537(8) . ? C3 C4 1.381(8) . ? C3 H3 0.9500 . ? C4 C5 1.376(8) . ? C4 H4A 0.9500 . ? C5 C6 1.398(8) . ? C5 H5 0.9500 . ? C6 C11 1.548(7) . ? C7 C8 1.538(7) . ? C7 C9 1.541(8) . ? C7 C10 1.545(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.544(8) . ? C11 C14 1.546(7) . ? C11 C12 1.549(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.440(7) . ? C15 C20 1.442(7) . ? C16 C17 1.380(7) . ? C16 C21 1.543(7) . ? C17 C18 1.381(8) . ? C17 H17 0.9500 . ? C18 C19 1.384(8) . ? C18 H18 0.9500 . ? C19 C20 1.392(8) . ? C19 H19 0.9500 . ? C20 C25 1.540(7) . ? C21 C24 1.524(8) . ? C21 C22 1.536(7) . ? C21 C23 1.546(7) . ? 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 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(8) . ? C25 C27 1.532(7) . ? C25 C28 1.541(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.381(9) . ? C39 C44 1.396(9) . ? C39 C45 1.516(9) . ? C40 C41 1.392(9) . ? C40 H40 0.9500 . ? C41 C42 1.385(10) . ? C41 H41 0.9500 . ? C42 C43 1.397(10) . ? C42 H42 0.9500 . ? C43 C44 1.381(9) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C51 1.384(8) . ? C46 C47 1.403(9) . ? C46 C52 1.516(8) . ? C47 C48 1.379(9) . ? C47 H47 0.9500 . ? C48 C49 1.386(9) . ? C48 H48 0.9500 . ? C49 C50 1.379(9) . ? C49 H49 0.9500 . ? C50 C51 1.375(9) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 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 O4 U1 O3 179.03(17) . . ? O4 U1 O2 88.36(15) . . ? O3 U1 O2 91.34(15) . . ? O4 U1 O1 89.99(15) . . ? O3 U1 O1 90.34(15) . . ? O2 U1 O1 177.56(12) . . ? O4 U1 N4 92.54(16) . . ? O3 U1 N4 86.59(16) . . ? O2 U1 N4 97.19(14) . . ? O1 U1 N4 84.68(14) . . ? O4 U1 N1 90.52(17) . . ? O3 U1 N1 90.42(16) . . ? O2 U1 N1 95.02(14) . . ? O1 U1 N1 83.19(14) . . ? N4 U1 N1 167.48(15) . . ? C1 O1 U1 179.0(3) . . ? C15 O2 U1 169.4(3) . . ? C29 N1 U1 137.2(4) . . ? C29 N1 H1A 111.4 . . ? U1 N1 H1A 111.4 . . ? C29 N2 C30 121.5(5) . . ? C29 N2 C31 121.7(5) . . ? C30 N2 C31 115.0(4) . . ? C29 N3 C33 120.6(5) . . ? C29 N3 C32 122.7(5) . . ? C33 N3 C32 114.9(4) . . ? C34 N4 U1 134.7(4) . . ? C34 N4 H4 112.7 . . ? U1 N4 H4 112.7 . . ? C34 N5 C36 121.6(5) . . ? C34 N5 C35 122.4(5) . . ? C36 N5 C35 114.1(4) . . ? C34 N6 C38 122.1(5) . . ? C34 N6 C37 119.4(5) . . ? C38 N6 C37 116.2(5) . . ? O1 C1 C6 121.1(5) . . ? O1 C1 C2 119.8(5) . . ? C6 C1 C2 119.1(5) . . ? C3 C2 C1 117.9(5) . . ? C3 C2 C7 119.6(5) . . ? C1 C2 C7 122.4(5) . . ? C4 C3 C2 122.9(5) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C5 C4 C3 118.8(5) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C4 C5 C6 122.6(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 118.5(5) . . ? C5 C6 C11 119.4(5) . . ? C1 C6 C11 122.1(5) . . ? C2 C7 C8 112.6(5) . . ? C2 C7 C9 110.0(4) . . ? C8 C7 C9 106.6(5) . . ? C2 C7 C10 110.0(4) . . ? C8 C7 C10 106.2(5) . . ? C9 C7 C10 111.5(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 105.8(4) . . ? C13 C11 C6 110.5(4) . . ? C14 C11 C6 112.6(5) . . ? C13 C11 C12 111.4(5) . . ? C14 C11 C12 106.8(4) . . ? C6 C11 C12 109.6(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 120.7(5) . . ? O2 C15 C20 120.8(5) . . ? C16 C15 C20 118.4(5) . . ? C17 C16 C15 118.1(5) . . ? C17 C16 C21 118.9(5) . . ? C15 C16 C21 122.9(5) . . ? C16 C17 C18 123.5(5) . . ? C16 C17 H17 118.2 . . ? C18 C17 H17 118.2 . . ? C17 C18 C19 117.7(5) . . ? C17 C18 H18 121.1 . . ? C19 C18 H18 121.1 . . ? C18 C19 C20 123.0(5) . . ? C18 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C19 C20 C15 118.0(5) . . ? C19 C20 C25 118.9(5) . . ? C15 C20 C25 123.0(5) . . ? C24 C21 C22 111.6(5) . . ? C24 C21 C16 111.5(4) . . ? C22 C21 C16 109.8(4) . . ? C24 C21 C23 106.6(4) . . ? C22 C21 C23 105.4(4) . . ? C16 C21 C23 111.8(4) . . ? 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 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 111.1(5) . . ? C26 C25 C20 111.5(4) . . ? C27 C25 C20 109.5(4) . . ? C26 C25 C28 106.4(4) . . ? C27 C25 C28 106.4(4) . . ? C20 C25 C28 111.9(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 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 N2 120.7(5) . . ? N1 C29 N3 122.2(5) . . ? N2 C29 N3 117.0(5) . . ? N2 C30 H30A 109.5 . . ? N2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 N5 121.4(5) . . ? N4 C34 N6 121.9(5) . . ? N5 C34 N6 116.6(5) . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 H37A 109.5 . . ? N6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 H38A 109.5 . . ? N6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 118.2(6) . . ? C40 C39 C45 120.7(6) . . ? C44 C39 C45 121.0(6) . . ? C39 C40 C41 121.5(6) . . ? C39 C40 H40 119.2 . . ? C41 C40 H40 119.2 . . ? C42 C41 C40 119.6(6) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C41 C42 C43 119.8(6) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 119.7(7) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C39 121.3(6) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 C46 C47 118.2(6) . . ? C51 C46 C52 121.7(6) . . ? C47 C46 C52 120.1(6) . . ? C48 C47 C46 120.4(6) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 120.4(6) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 119.3(6) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 120.6(6) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C46 121.1(6) . . ? C50 C51 H51 119.4 . . ? C46 C51 H51 119.4 . . ? C46 C52 H52A 109.5 . . ? C46 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C46 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.877 _refine_diff_density_min -1.136 _refine_diff_density_rms 0.117 #===END data_jab045_centro _database_code_depnum_ccdc_archive 'CCDC 646919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(3) (UO2OC6H2-2,6-(C(CH3)3)2-4-CH3HTMG2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H72 N6 O4 U' _chemical_formula_weight 939.07 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.888(3) _cell_length_b 12.046(3) _cell_length_c 16.410(4) _cell_angle_alpha 98.537(4) _cell_angle_beta 110.668(4) _cell_angle_gamma 93.634(4) _cell_volume 2157.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6683 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 3.806 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.3411 _exptl_absorpt_correction_T_max 0.5165 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 17444 _diffrn_reflns_av_R_equivalents 0.1194 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7634 _reflns_number_gt 6903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.5472P] 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 7634 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 0.718 _refine_ls_restrained_S_all 0.718 _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 0.547752(13) 0.896777(12) 0.750231(9) 0.01134(9) Uani 1 1 d . . . O1 O 0.4406(3) 0.8268(3) 0.7847(2) 0.0131(7) Uani 1 1 d . . . O2 O 0.6543(3) 0.9650(3) 0.7138(2) 0.0125(7) Uani 1 1 d . . . O3 O 0.4457(3) 1.0479(3) 0.7369(2) 0.0124(7) Uani 1 1 d . . . O4 O 0.6536(3) 0.7482(3) 0.7678(2) 0.0136(7) Uani 1 1 d . . . N1 N 0.6517(3) 1.0015(3) 0.9041(3) 0.0167(9) Uani 1 1 d . . . H1 H 0.6220 0.9770 0.9412 0.020 Uiso 1 1 calc R . . N2 N 0.7309(4) 1.1802(3) 0.9955(3) 0.0170(8) Uani 1 1 d . . . N3 N 0.8491(4) 1.0771(4) 0.9346(3) 0.0172(9) Uani 1 1 d . . . N4 N 0.4157(3) 0.8400(3) 0.5927(3) 0.0162(8) Uani 1 1 d . . . H4 H 0.4546 0.8541 0.5579 0.019 Uiso 1 1 calc R . . N5 N 0.2625(4) 0.6915(4) 0.5569(3) 0.0178(9) Uani 1 1 d . . . N6 N 0.2215(4) 0.8448(3) 0.4864(3) 0.0184(9) Uani 1 1 d . . . C1 C 0.3827(4) 1.1377(4) 0.7281(3) 0.0136(9) Uani 1 1 d . . . C2 C 0.4252(4) 1.2344(4) 0.7001(3) 0.0140(9) Uani 1 1 d . . . C3 C 0.3540(4) 1.3244(4) 0.6892(3) 0.0137(9) Uani 1 1 d . . . H3 H 0.3808 1.3881 0.6698 0.016 Uiso 1 1 calc R . . C4 C 0.2470(4) 1.3250(4) 0.7052(3) 0.0204(11) Uani 1 1 d . . . C5 C 0.2095(5) 1.2322(4) 0.7332(3) 0.0175(10) Uani 1 1 d . . . H5 H 0.1367 1.2317 0.7450 0.021 Uiso 1 1 calc R . . C6 C 0.2735(4) 1.1383(4) 0.7453(3) 0.0128(9) Uani 1 1 d . . . C7 C 0.5449(4) 1.2448(4) 0.6841(3) 0.0143(9) Uani 1 1 d . . . C8 C 0.5371(4) 1.1522(4) 0.6056(3) 0.0173(10) Uani 1 1 d . . . H8A H 0.5157 1.0778 0.6173 0.026 Uiso 1 1 calc R . . H8B H 0.6156 1.1545 0.5985 0.026 Uiso 1 1 calc R . . H8C H 0.4749 1.1656 0.5512 0.026 Uiso 1 1 calc R . . C9 C 0.6508(4) 1.2361(4) 0.7690(3) 0.0161(10) Uani 1 1 d . . . H9A H 0.6551 1.2979 0.8166 0.024 Uiso 1 1 calc R . . H9B H 0.7267 1.2413 0.7582 0.024 Uiso 1 1 calc R . . H9C H 0.6379 1.1634 0.7865 0.024 Uiso 1 1 calc R . . C10 C 0.5741(4) 1.3599(4) 0.6591(3) 0.0204(10) Uani 1 1 d . . . H10A H 0.5083 1.3699 0.6054 0.031 Uiso 1 1 calc R . . H10B H 0.6502 1.3607 0.6485 0.031 Uiso 1 1 calc R . . H10C H 0.5821 1.4216 0.7078 0.031 Uiso 1 1 calc R . . C11 C 0.1761(5) 1.4245(5) 0.6923(4) 0.0288(12) Uani 1 1 d . . . H11A H 0.2232 1.4911 0.7361 0.043 Uiso 1 1 calc R . . H11B H 0.0992 1.4072 0.7001 0.043 Uiso 1 1 calc R . . H11C H 0.1599 1.4399 0.6325 0.043 Uiso 1 1 calc R . . C12 C 0.2213(4) 1.0363(4) 0.7744(3) 0.0132(9) Uani 1 1 d . . . C13 C 0.3116(4) 1.0144(4) 0.8620(3) 0.0166(10) Uani 1 1 d . . . H13A H 0.2852 0.9414 0.8733 0.025 Uiso 1 1 calc R . . H13B H 0.3153 1.0747 0.9104 0.025 Uiso 1 1 calc R . . H13C H 0.3920 1.0129 0.8583 0.025 Uiso 1 1 calc R . . C14 C 0.1880(4) 0.9318(4) 0.7004(3) 0.0162(10) Uani 1 1 d . . . H14A H 0.2579 0.9194 0.6833 0.024 Uiso 1 1 calc R . . H14B H 0.1197 0.9441 0.6491 0.024 Uiso 1 1 calc R . . H14C H 0.1652 0.8654 0.7218 0.024 Uiso 1 1 calc R . . C15 C 0.1037(4) 1.0575(4) 0.7910(3) 0.0200(10) Uani 1 1 d . . . H15A H 0.0417 1.0701 0.7363 0.030 Uiso 1 1 calc R . . H15B H 0.1201 1.1243 0.8375 0.030 Uiso 1 1 calc R . . H15C H 0.0746 0.9915 0.8098 0.030 Uiso 1 1 calc R . . C16 C 0.7277(4) 0.6666(4) 0.7853(3) 0.0124(9) Uani 1 1 d . . . C17 C 0.7353(4) 0.6067(4) 0.8566(3) 0.0149(9) Uani 1 1 d . . . C18 C 0.8218(4) 0.5337(4) 0.8786(3) 0.0156(9) Uani 1 1 d . . . H18 H 0.8287 0.4971 0.9273 0.019 Uiso 1 1 calc R . . C19 C 0.8993(4) 0.5108(4) 0.8333(3) 0.0181(10) Uani 1 1 d . . . C20 C 0.8848(4) 0.5626(4) 0.7607(3) 0.0170(10) Uani 1 1 d . . . H20 H 0.9347 0.5456 0.7274 0.020 Uiso 1 1 calc R . . C21 C 0.8010(4) 0.6379(4) 0.7342(3) 0.0148(10) Uani 1 1 d . . . C22 C 0.6498(4) 0.6195(4) 0.9094(3) 0.0155(10) Uani 1 1 d . . . C23 C 0.6746(4) 0.7379(4) 0.9655(3) 0.0183(10) Uani 1 1 d . . . H23A H 0.6625 0.7944 0.9269 0.028 Uiso 1 1 calc R . . H23B H 0.7583 0.7508 1.0081 0.028 Uiso 1 1 calc R . . H23C H 0.6188 0.7446 0.9974 0.028 Uiso 1 1 calc R . . C24 C 0.5163(4) 0.5931(4) 0.8453(3) 0.0176(10) Uani 1 1 d . . . H24A H 0.4631 0.6099 0.8783 0.026 Uiso 1 1 calc R . . H24B H 0.4992 0.5129 0.8176 0.026 Uiso 1 1 calc R . . H24C H 0.5020 0.6397 0.7993 0.026 Uiso 1 1 calc R . . C25 C 0.6661(5) 0.5355(5) 0.9740(3) 0.0230(11) Uani 1 1 d . . . H25A H 0.7489 0.5501 1.0181 0.035 Uiso 1 1 calc R . . H25B H 0.6516 0.4579 0.9409 0.035 Uiso 1 1 calc R . . H25C H 0.6083 0.5451 1.0040 0.035 Uiso 1 1 calc R . . C26 C 0.9909(5) 0.4293(5) 0.8585(3) 0.0222(11) Uani 1 1 d . . . H26A H 1.0072 0.4202 0.9198 0.033 Uiso 1 1 calc R . . H26B H 1.0662 0.4587 0.8530 0.033 Uiso 1 1 calc R . . H26C H 0.9591 0.3558 0.8190 0.033 Uiso 1 1 calc R . . C27 C 0.7922(4) 0.6851(4) 0.6497(3) 0.0154(10) Uani 1 1 d . . . C28 C 0.6602(4) 0.6747(5) 0.5853(3) 0.0214(11) Uani 1 1 d . . . H28A H 0.6243 0.5953 0.5702 0.032 Uiso 1 1 calc R . . H28B H 0.6580 0.7014 0.5313 0.032 Uiso 1 1 calc R . . H28C H 0.6140 0.7206 0.6133 0.032 Uiso 1 1 calc R . . C29 C 0.8507(5) 0.8090(4) 0.6740(3) 0.0218(11) Uani 1 1 d . . . H29A H 0.8538 0.8344 0.6207 0.033 Uiso 1 1 calc R . . H29B H 0.9330 0.8151 0.7178 0.033 Uiso 1 1 calc R . . H29C H 0.8024 0.8565 0.6989 0.033 Uiso 1 1 calc R . . C30 C 0.8597(4) 0.6188(4) 0.5973(3) 0.0215(11) Uani 1 1 d . . . H30A H 0.8280 0.5384 0.5830 0.032 Uiso 1 1 calc R . . H30B H 0.9465 0.6284 0.6333 0.032 Uiso 1 1 calc R . . H30C H 0.8475 0.6476 0.5424 0.032 Uiso 1 1 calc R . . C31 C 0.7410(4) 1.0851(4) 0.9439(3) 0.0161(10) Uani 1 1 d . . . C32 C 0.6105(5) 1.2088(4) 0.9891(3) 0.0224(11) Uani 1 1 d . . . H32A H 0.5532 1.1840 0.9281 0.034 Uiso 1 1 calc R . . H32B H 0.6143 1.2909 1.0061 0.034 Uiso 1 1 calc R . . H32C H 0.5834 1.1708 1.0290 0.034 Uiso 1 1 calc R . . C33 C 0.8319(5) 1.2431(5) 1.0728(3) 0.0272(12) Uani 1 1 d . . . H33A H 0.9037 1.2035 1.0822 0.041 Uiso 1 1 calc R . . H33B H 0.8098 1.2485 1.1253 0.041 Uiso 1 1 calc R . . H33C H 0.8497 1.3193 1.0626 0.041 Uiso 1 1 calc R . . C34 C 0.8781(4) 0.9684(5) 0.8994(3) 0.0239(11) Uani 1 1 d . . . H34A H 0.8370 0.9070 0.9155 0.036 Uiso 1 1 calc R . . H34B H 0.9659 0.9667 0.9242 0.036 Uiso 1 1 calc R . . H34C H 0.8508 0.9587 0.8347 0.036 Uiso 1 1 calc R . . C35 C 0.9184(5) 1.1760(5) 0.9241(4) 0.0263(12) Uani 1 1 d . . . H35A H 0.8758 1.2424 0.9282 0.039 Uiso 1 1 calc R . . H35B H 0.9264 1.1614 0.8662 0.039 Uiso 1 1 calc R . . H35C H 0.9990 1.1901 0.9710 0.039 Uiso 1 1 calc R . . C36 C 0.3026(4) 0.7943(4) 0.5461(3) 0.0124(9) Uani 1 1 d . . . C37 C 0.3488(5) 0.6166(4) 0.5993(3) 0.0226(11) Uani 1 1 d . . . H37A H 0.4225 0.6285 0.5863 0.034 Uiso 1 1 calc R . . H37B H 0.3122 0.5376 0.5765 0.034 Uiso 1 1 calc R . . H37C H 0.3693 0.6335 0.6635 0.034 Uiso 1 1 calc R . . C38 C 0.1420(5) 0.6686(4) 0.5603(4) 0.0224(11) Uani 1 1 d . . . H38A H 0.1500 0.6606 0.6207 0.034 Uiso 1 1 calc R . . H38B H 0.0996 0.5984 0.5192 0.034 Uiso 1 1 calc R . . H38C H 0.0956 0.7314 0.5435 0.034 Uiso 1 1 calc R . . C39 C 0.1296(5) 0.7814(5) 0.4051(3) 0.0260(12) Uani 1 1 d . . . H39A H 0.1358 0.7003 0.4028 0.039 Uiso 1 1 calc R . . H39B H 0.1421 0.8047 0.3539 0.039 Uiso 1 1 calc R . . H39C H 0.0490 0.7964 0.4040 0.039 Uiso 1 1 calc R . . C40 C 0.2394(5) 0.9680(4) 0.4911(3) 0.0218(11) Uani 1 1 d . . . H40A H 0.2877 1.0048 0.5522 0.033 Uiso 1 1 calc R . . H40B H 0.1605 0.9964 0.4721 0.033 Uiso 1 1 calc R . . H40C H 0.2820 0.9848 0.4521 0.033 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 U1 0.01651(12) 0.00815(12) 0.01092(12) 0.00178(7) 0.00667(8) 0.00305(8) O1 0.0160(16) 0.0088(17) 0.0148(16) 0.0034(13) 0.0054(13) 0.0017(13) O2 0.0150(15) 0.0084(16) 0.0130(16) 0.0030(13) 0.0031(13) 0.0023(13) O3 0.0177(16) 0.0065(17) 0.0159(16) 0.0040(13) 0.0088(14) 0.0031(13) O4 0.0168(16) 0.0131(18) 0.0147(16) 0.0045(13) 0.0089(14) 0.0056(14) N1 0.020(2) 0.012(2) 0.017(2) 0.0061(16) 0.0046(17) -0.0007(17) N2 0.022(2) 0.014(2) 0.0149(19) -0.0006(16) 0.0090(17) 0.0017(17) N3 0.019(2) 0.016(2) 0.020(2) 0.0047(17) 0.0092(17) 0.0035(17) N4 0.0166(19) 0.013(2) 0.020(2) 0.0002(16) 0.0085(17) 0.0003(16) N5 0.0146(19) 0.018(2) 0.022(2) 0.0054(18) 0.0073(17) 0.0033(17) N6 0.020(2) 0.015(2) 0.020(2) 0.0036(17) 0.0084(17) 0.0007(17) C1 0.021(2) 0.009(2) 0.012(2) -0.0001(18) 0.0083(19) 0.002(2) C2 0.020(2) 0.014(2) 0.009(2) 0.0029(18) 0.0068(18) 0.0019(19) C3 0.015(2) 0.014(2) 0.015(2) 0.0061(18) 0.0066(18) 0.0044(19) C4 0.022(2) 0.014(3) 0.026(3) 0.004(2) 0.009(2) 0.006(2) C5 0.021(2) 0.017(3) 0.019(2) 0.005(2) 0.011(2) 0.005(2) C6 0.021(2) 0.007(2) 0.010(2) 0.0001(17) 0.0069(19) 0.0019(19) C7 0.022(2) 0.012(2) 0.012(2) 0.0007(18) 0.0100(19) 0.0050(19) C8 0.023(2) 0.016(3) 0.016(2) 0.001(2) 0.010(2) 0.003(2) C9 0.017(2) 0.013(2) 0.018(2) 0.0040(19) 0.0056(19) 0.0019(19) C10 0.023(2) 0.016(3) 0.024(3) 0.007(2) 0.011(2) 0.001(2) C11 0.031(3) 0.014(3) 0.050(4) 0.011(2) 0.022(3) 0.005(2) C12 0.017(2) 0.011(2) 0.013(2) 0.0011(18) 0.0080(19) -0.0005(19) C13 0.025(2) 0.015(3) 0.014(2) 0.0033(19) 0.013(2) 0.003(2) C14 0.021(2) 0.011(2) 0.016(2) -0.0017(19) 0.0088(19) -0.0009(19) C15 0.025(2) 0.014(2) 0.028(3) 0.004(2) 0.018(2) 0.003(2) C16 0.015(2) 0.006(2) 0.013(2) -0.0031(17) 0.0042(18) -0.0018(18) C17 0.021(2) 0.012(2) 0.011(2) -0.0001(18) 0.0067(19) -0.0017(19) C18 0.024(2) 0.010(2) 0.013(2) 0.0009(18) 0.0075(19) 0.0011(19) C19 0.023(2) 0.013(2) 0.015(2) 0.0024(19) 0.002(2) 0.001(2) C20 0.017(2) 0.016(3) 0.022(2) 0.001(2) 0.013(2) 0.003(2) C21 0.019(2) 0.010(2) 0.013(2) -0.0014(18) 0.0048(19) -0.0003(19) C22 0.022(2) 0.015(2) 0.013(2) 0.0032(19) 0.011(2) 0.005(2) C23 0.026(2) 0.017(3) 0.014(2) -0.0011(19) 0.011(2) 0.004(2) C24 0.019(2) 0.014(3) 0.022(3) 0.003(2) 0.010(2) 0.002(2) C25 0.030(3) 0.022(3) 0.025(3) 0.009(2) 0.016(2) 0.009(2) C26 0.024(2) 0.023(3) 0.023(3) 0.008(2) 0.011(2) 0.009(2) C27 0.021(2) 0.011(2) 0.018(2) 0.0023(19) 0.011(2) 0.0028(19) C28 0.023(2) 0.029(3) 0.013(2) 0.003(2) 0.008(2) 0.006(2) C29 0.029(3) 0.019(3) 0.022(3) 0.006(2) 0.015(2) 0.002(2) C30 0.027(3) 0.021(3) 0.019(2) 0.005(2) 0.012(2) 0.008(2) C31 0.022(2) 0.018(3) 0.014(2) 0.0100(19) 0.0096(19) 0.008(2) C32 0.030(3) 0.018(3) 0.024(3) 0.007(2) 0.013(2) 0.010(2) C33 0.033(3) 0.021(3) 0.024(3) -0.001(2) 0.008(2) -0.004(2) C34 0.016(2) 0.033(3) 0.017(2) -0.004(2) 0.001(2) 0.009(2) C35 0.019(2) 0.031(3) 0.033(3) 0.014(2) 0.011(2) 0.001(2) C36 0.020(2) 0.009(2) 0.012(2) 0.0008(17) 0.0109(18) 0.0012(18) C37 0.028(3) 0.011(2) 0.026(3) 0.004(2) 0.006(2) 0.004(2) C38 0.026(3) 0.015(3) 0.030(3) 0.003(2) 0.016(2) 0.002(2) C39 0.030(3) 0.025(3) 0.018(3) 0.003(2) 0.003(2) 0.002(2) C40 0.031(3) 0.015(3) 0.022(3) 0.007(2) 0.011(2) 0.009(2) _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 O1 1.780(3) . ? U1 O2 1.785(3) . ? U1 O3 2.246(3) . ? U1 O4 2.247(3) . ? U1 N4 2.467(4) . ? U1 N1 2.479(4) . ? O3 C1 1.351(6) . ? O4 C16 1.357(6) . ? N1 C31 1.322(6) . ? N1 H1 0.8800 . ? N2 C31 1.359(6) . ? N2 C32 1.465(6) . ? N2 C33 1.466(6) . ? N3 C31 1.354(6) . ? N3 C34 1.463(7) . ? N3 C35 1.471(7) . ? N4 C36 1.323(6) . ? N4 H4 0.8800 . ? N5 C36 1.357(6) . ? N5 C38 1.464(6) . ? N5 C37 1.467(6) . ? N6 C36 1.358(6) . ? N6 C39 1.456(7) . ? N6 C40 1.472(6) . ? C1 C6 1.423(7) . ? C1 C2 1.438(6) . ? C2 C3 1.412(6) . ? C2 C7 1.537(6) . ? C3 C4 1.387(7) . ? C3 H3 0.9500 . ? C4 C5 1.376(7) . ? C4 C11 1.506(7) . ? C5 C6 1.403(7) . ? C5 H5 0.9500 . ? C6 C12 1.552(6) . ? C7 C9 1.536(6) . ? C7 C8 1.545(6) . ? C7 C10 1.554(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.532(6) . ? C12 C14 1.535(6) . ? C12 C15 1.545(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.431(7) . ? C16 C17 1.444(6) . ? C17 C18 1.382(7) . ? C17 C22 1.551(6) . ? C18 C19 1.389(7) . ? C18 H18 0.9500 . ? C19 C20 1.389(7) . ? C19 C26 1.503(7) . ? C20 C21 1.390(7) . ? C20 H20 0.9500 . ? C21 C27 1.548(6) . ? C22 C23 1.528(7) . ? C22 C25 1.543(6) . ? C22 C24 1.544(6) . ? 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 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 1.536(6) . ? C27 C29 1.538(7) . ? C27 C30 1.544(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 O1 U1 O2 178.95(12) . . ? O1 U1 O3 90.96(13) . . ? O2 U1 O3 89.46(13) . . ? O1 U1 O4 89.20(13) . . ? O2 U1 O4 90.41(13) . . ? O3 U1 O4 178.23(10) . . ? O1 U1 N4 91.83(14) . . ? O2 U1 N4 87.28(14) . . ? O3 U1 N4 81.68(12) . . ? O4 U1 N4 100.08(13) . . ? O1 U1 N1 89.25(14) . . ? O2 U1 N1 91.76(14) . . ? O3 U1 N1 82.43(12) . . ? O4 U1 N1 95.81(12) . . ? N4 U1 N1 164.09(14) . . ? C1 O3 U1 179.1(3) . . ? C16 O4 U1 173.6(3) . . ? C31 N1 U1 135.5(3) . . ? C31 N1 H1 112.3 . . ? U1 N1 H1 112.3 . . ? C31 N2 C32 119.6(4) . . ? C31 N2 C33 123.6(4) . . ? C32 N2 C33 115.2(4) . . ? C31 N3 C34 120.6(4) . . ? C31 N3 C35 120.9(4) . . ? C34 N3 C35 114.0(4) . . ? C36 N4 U1 137.6(3) . . ? C36 N4 H4 111.2 . . ? U1 N4 H4 111.2 . . ? C36 N5 C38 121.2(4) . . ? C36 N5 C37 120.5(4) . . ? C38 N5 C37 114.1(4) . . ? C36 N6 C39 122.7(4) . . ? C36 N6 C40 120.5(4) . . ? C39 N6 C40 115.5(4) . . ? O3 C1 C6 121.0(4) . . ? O3 C1 C2 120.0(4) . . ? C6 C1 C2 119.0(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C7 119.1(4) . . ? C1 C2 C7 123.1(4) . . ? C4 C3 C2 123.5(4) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C5 C4 C3 117.5(4) . . ? C5 C4 C11 122.1(5) . . ? C3 C4 C11 120.4(4) . . ? C4 C5 C6 123.2(5) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C5 C6 C1 119.1(4) . . ? C5 C6 C12 119.0(4) . . ? C1 C6 C12 121.8(4) . . ? C9 C7 C2 109.7(4) . . ? C9 C7 C8 111.7(4) . . ? C2 C7 C8 109.3(4) . . ? C9 C7 C10 106.3(4) . . ? C2 C7 C10 113.3(4) . . ? C8 C7 C10 106.4(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 111.9(4) . . ? C13 C12 C15 106.1(4) . . ? C14 C12 C15 106.4(4) . . ? C13 C12 C6 110.5(4) . . ? C14 C12 C6 109.6(4) . . ? C15 C12 C6 112.4(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 C21 121.2(4) . . ? O4 C16 C17 120.7(4) . . ? C21 C16 C17 118.1(4) . . ? C18 C17 C16 118.7(4) . . ? C18 C17 C22 118.2(4) . . ? C16 C17 C22 123.1(4) . . ? C17 C18 C19 123.6(4) . . ? C17 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? C20 C19 C18 117.1(4) . . ? C20 C19 C26 121.0(4) . . ? C18 C19 C26 121.9(4) . . ? C19 C20 C21 123.3(5) . . ? C19 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C20 C21 C16 118.8(4) . . ? C20 C21 C27 117.2(4) . . ? C16 C21 C27 123.9(4) . . ? C23 C22 C25 106.5(4) . . ? C23 C22 C24 111.1(4) . . ? C25 C22 C24 105.6(4) . . ? C23 C22 C17 110.8(4) . . ? C25 C22 C17 112.7(4) . . ? C24 C22 C17 110.0(4) . . ? 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 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 110.4(4) . . ? C28 C27 C30 105.7(4) . . ? C29 C27 C30 106.7(4) . . ? C28 C27 C21 111.4(4) . . ? C29 C27 C21 110.6(4) . . ? C30 C27 C21 111.8(4) . . ? 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 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 . . ? N1 C31 N3 119.6(4) . . ? N1 C31 N2 123.2(4) . . ? N3 C31 N2 117.2(4) . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 N5 119.9(4) . . ? N4 C36 N6 123.5(4) . . ? N5 C36 N6 116.6(4) . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N6 C39 H39A 109.5 . . ? N6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.541 _refine_diff_density_min -2.013 _refine_diff_density_rms 0.167 #===END