Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Noemia Marques' _publ_contact_author_address ; Departamento de Quimica ITN Estrada Nacional 10, 2686-953 Sacavem PORTUGAL ; _publ_contact_author_email NMARQUES@ITN.PT _publ_section_title ; The Uranium-Nitrogen Bond in U(IV) Complexes Supported by the Hydrotris(3,5-dimethylpyrazolyl)borate Ligand ; loop_ _publ_author_name 'Noemia Marques' 'Maria Augusta Antunes' 'I.C.dos Santos' 'Marta Dias' 'Angela Domingos' ; J.Marcalo ; 'Manuela Silva' data_unitrilo _database_code_depnum_ccdc_archive 'CCDC 276941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety {UCl2[(N=C-(Ph))(CH2SiMe3)]TpMe2} _chemical_formula_sum 'C26 H38 B Cl2 N7 Si U' _chemical_formula_weight 796.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 20.948(3) _cell_length_b 10.5300(10) _cell_length_c 15.0120(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3311.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.2 _cell_measurement_theta_max 14.6 _exptl_crystal_description irregular _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 5.126 _exptl_absorpt_correction_type 'empirical via \y-scan North et al (1968)' _exptl_absorpt_correction_T_min 0.4894 _exptl_absorpt_correction_T_max 0.9994 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were obtained from a concentrated toluene/hexane solution ; _diffrn_ambient_temperature 293(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 CAD4-Enraf-Nonius _diffrn_measurement_method \w/2\qscans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_reflns_number 3185 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.1265 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3014 _reflns_number_gt 1687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction process-MOLEN(Fair,1990) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(18) _refine_ls_number_reflns 3014 _refine_ls_number_parameters 343 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1539 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.015 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 0.91201(4) 0.93542(6) 0.72586(4) 0.0416(2) Uani 1 1 d . . . Cl1 Cl 0.9260(4) 1.1071(6) 0.6029(5) 0.080(3) Uani 1 1 d . . . Cl2 Cl 0.8395(3) 1.0604(7) 0.8378(5) 0.072(2) Uani 1 1 d . . . Si1 Si 1.0982(5) 1.2280(6) 0.8142(5) 0.061(2) Uani 1 1 d . . . N4 N 0.9985(9) 0.9571(17) 0.7872(14) 0.064(7) Uani 1 1 d . . . N11 N 0.8918(11) 0.7312(18) 0.8061(13) 0.051(6) Uani 1 1 d . . . N12 N 0.8703(11) 0.6217(19) 0.7668(13) 0.038(6) Uani 1 1 d U . . N21 N 0.8182(10) 0.8428(16) 0.6495(12) 0.041(5) Uani 1 1 d . . . N22 N 0.8121(10) 0.711(2) 0.6350(12) 0.046(5) Uani 1 1 d . . . N31 N 0.9583(11) 0.7648(18) 0.6258(13) 0.049(6) Uani 1 1 d . . . N32 N 0.9303(10) 0.6459(18) 0.6236(15) 0.054(7) Uani 1 1 d . . . C4 C 1.0517(13) 0.976(2) 0.8341(16) 0.040(6) Uani 1 1 d U . . C5 C 1.0589(14) 1.096(2) 0.8830(13) 0.067(9) Uani 1 1 d . . . H5A H 1.0844 1.0812 0.9359 0.080 Uiso 1 1 calc R . . H5B H 1.0171 1.1249 0.9023 0.080 Uiso 1 1 calc R . . C6 C 1.1374(15) 1.158(2) 0.717(3) 0.105(13) Uani 1 1 d . . . H6A H 1.1065 1.1126 0.6818 0.157 Uiso 1 1 calc R . . H6B H 1.1702 1.1008 0.7359 0.157 Uiso 1 1 calc R . . H6C H 1.1559 1.2244 0.6811 0.157 Uiso 1 1 calc R . . C7 C 1.0310(14) 1.338(2) 0.779(2) 0.127(16) Uani 1 1 d . . . H7A H 1.0008 1.2920 0.7429 0.190 Uiso 1 1 calc R . . H7B H 1.0482 1.4072 0.7444 0.190 Uiso 1 1 calc R . . H7C H 1.0099 1.3713 0.8304 0.190 Uiso 1 1 calc R . . C8 C 1.1552(13) 1.315(3) 0.8816(18) 0.090(10) Uani 1 1 d . . . H8A H 1.1338 1.3514 0.9322 0.136 Uiso 1 1 calc R . . H8B H 1.1738 1.3821 0.8467 0.136 Uiso 1 1 calc R . . H8C H 1.1881 1.2588 0.9017 0.136 Uiso 1 1 calc R . . C11 C 0.8955(10) 0.7133(19) 0.8963(13) 0.029(5) Uani 1 1 d U . . C12 C 0.8767(12) 0.586(2) 0.9105(16) 0.052(7) Uani 1 1 d . . . H12 H 0.8756 0.5454 0.9653 0.062 Uiso 1 1 calc R . . C13 C 0.8608(12) 0.5344(19) 0.8325(17) 0.045(7) Uani 1 1 d U . . C14 C 0.9196(13) 0.802(2) 0.9611(15) 0.069(9) Uani 1 1 d . . . H14A H 0.9300 0.8806 0.9322 0.103 Uiso 1 1 calc R . . H14B H 0.9572 0.7674 0.9885 0.103 Uiso 1 1 calc R . . H14C H 0.8877 0.8168 1.0058 0.103 Uiso 1 1 calc R . . C15 C 0.8431(11) 0.3997(17) 0.8076(18) 0.057(8) Uani 1 1 d . . . H15A H 0.8368 0.3943 0.7443 0.085 Uiso 1 1 calc R . . H15B H 0.8045 0.3760 0.8376 0.085 Uiso 1 1 calc R . . H15C H 0.8769 0.3432 0.8249 0.085 Uiso 1 1 calc R . . C21 C 0.7630(16) 0.892(3) 0.612(2) 0.070(10) Uani 1 1 d . . . C22 C 0.7288(15) 0.801(3) 0.576(2) 0.078(12) Uani 1 1 d . . . H22 H 0.6897 0.8116 0.5471 0.094 Uiso 1 1 calc R . . C23 C 0.7615(14) 0.686(2) 0.5870(18) 0.051(7) Uani 1 1 d U . . C24 C 0.7573(16) 1.036(3) 0.6189(18) 0.091(11) Uani 1 1 d . . . H24A H 0.7932 1.0687 0.6514 0.137 Uiso 1 1 calc R . . H24B H 0.7186 1.0572 0.6496 0.137 Uiso 1 1 calc R . . H24C H 0.7566 1.0721 0.5603 0.137 Uiso 1 1 calc R . . C25 C 0.7399(13) 0.557(2) 0.5622(14) 0.067(8) Uani 1 1 d . . . H25A H 0.7713 0.4957 0.5808 0.100 Uiso 1 1 calc R . . H25B H 0.7345 0.5518 0.4988 0.100 Uiso 1 1 calc R . . H25C H 0.7000 0.5387 0.5910 0.100 Uiso 1 1 calc R . . C31 C 1.0137(11) 0.761(2) 0.5781(17) 0.050(7) Uani 1 1 d . . . C32 C 1.0167(15) 0.644(3) 0.540(2) 0.073(9) Uani 1 1 d U . . H32 H 1.0495 0.6147 0.5036 0.087 Uiso 1 1 calc R . . C33 C 0.9650(15) 0.579(2) 0.563(2) 0.068(9) Uani 1 1 d . . . C34 C 1.0562(13) 0.876(3) 0.5765(19) 0.067(9) Uani 1 1 d . . . H34A H 1.0389 0.9398 0.6151 0.100 Uiso 1 1 calc R . . H34B H 1.0587 0.9082 0.5169 0.100 Uiso 1 1 calc R . . H34C H 1.0981 0.8527 0.5966 0.100 Uiso 1 1 calc R . . C35 C 0.9477(14) 0.4472(19) 0.539(2) 0.083(10) Uani 1 1 d . . . H35A H 0.9076 0.4260 0.5663 0.124 Uiso 1 1 calc R . . H35B H 0.9801 0.3904 0.5609 0.124 Uiso 1 1 calc R . . H35C H 0.9443 0.4395 0.4759 0.124 Uiso 1 1 calc R . . C40 C 1.1011(12) 0.876(2) 0.8335(18) 0.046(7) Uani 1 1 d . . . C41 C 1.0903(15) 0.759(2) 0.8028(17) 0.071(8) Uani 1 1 d . . . H41 H 1.0495 0.7404 0.7823 0.085 Uiso 1 1 calc R . . C42 C 1.1352(17) 0.665(2) 0.799(2) 0.084(11) Uani 1 1 d . . . H42 H 1.1259 0.5865 0.7738 0.101 Uiso 1 1 calc R . . C43 C 1.1941(16) 0.690(3) 0.834(3) 0.087(12) Uani 1 1 d . . . H43 H 1.2243 0.6252 0.8353 0.104 Uiso 1 1 calc R . . C44 C 1.2098(19) 0.803(4) 0.867(2) 0.096(12) Uani 1 1 d U . . H44 H 1.2506 0.8195 0.8878 0.115 Uiso 1 1 calc R . . C45 C 1.1629(14) 0.894(3) 0.867(2) 0.084(11) Uani 1 1 d . . . H45 H 1.1727 0.9724 0.8920 0.101 Uiso 1 1 calc R . . B1 B 0.8720(19) 0.619(4) 0.665(2) 0.040(9) Uani 1 1 d U . . H1 H 0.8604 0.5322 0.6472 0.048 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 0.0422(4) 0.0349(3) 0.0477(4) -0.0004(13) 0.0006(14) 0.0012(5) Cl1 0.113(8) 0.053(4) 0.073(5) 0.020(4) 0.016(6) -0.002(4) Cl2 0.079(5) 0.059(4) 0.078(5) -0.014(5) 0.018(5) 0.024(5) Si1 0.080(7) 0.051(4) 0.051(4) -0.007(4) -0.017(5) -0.012(5) N4 0.047(13) 0.062(14) 0.082(15) 0.008(13) 0.037(13) -0.023(12) N11 0.070(18) 0.047(12) 0.037(13) 0.000(11) 0.005(13) -0.015(12) N12 0.040(8) 0.036(7) 0.038(8) -0.004(5) -0.003(5) -0.002(5) N21 0.037(13) 0.041(12) 0.045(13) -0.015(10) 0.000(12) 0.013(11) N22 0.042(14) 0.071(14) 0.026(11) -0.005(11) 0.007(11) 0.010(12) N31 0.069(18) 0.045(12) 0.035(12) 0.007(11) 0.018(13) 0.005(13) N32 0.052(18) 0.037(11) 0.074(17) -0.010(12) 0.018(14) 0.012(12) C4 0.039(8) 0.040(7) 0.039(8) -0.005(5) -0.003(5) -0.005(5) C5 0.12(3) 0.075(19) 0.009(10) -0.016(13) -0.010(15) -0.015(17) C6 0.16(3) 0.080(17) 0.08(3) 0.01(3) 0.02(4) -0.072(19) C7 0.09(3) 0.10(2) 0.18(4) 0.02(2) -0.10(3) 0.01(2) C8 0.10(3) 0.09(2) 0.09(2) 0.02(2) -0.01(2) -0.02(2) C11 0.030(7) 0.031(6) 0.026(7) 0.000(5) 0.004(5) 0.002(5) C12 0.038(15) 0.072(19) 0.044(15) 0.030(15) 0.011(14) -0.003(15) C13 0.044(8) 0.044(8) 0.046(8) 0.002(5) 0.006(5) -0.004(5) C14 0.08(2) 0.094(18) 0.034(13) 0.001(14) -0.026(17) -0.04(2) C15 0.054(18) 0.038(14) 0.079(19) 0.013(13) -0.032(17) -0.021(12) C21 0.05(2) 0.09(2) 0.07(2) 0.041(19) 0.02(2) 0.018(19) C22 0.04(2) 0.11(3) 0.09(3) 0.04(2) 0.04(2) 0.00(2) C23 0.047(8) 0.053(8) 0.053(8) 0.002(5) -0.006(5) -0.001(5) C24 0.10(3) 0.13(3) 0.048(18) 0.00(2) -0.01(2) 0.05(2) C25 0.08(2) 0.085(19) 0.033(13) 0.016(17) 0.011(15) -0.04(2) C31 0.025(15) 0.062(16) 0.063(19) 0.013(15) 0.022(15) 0.013(14) C32 0.073(10) 0.070(9) 0.075(10) -0.002(5) 0.001(5) 0.004(5) C33 0.08(2) 0.040(15) 0.09(2) 0.013(17) 0.034(19) -0.009(17) C34 0.037(18) 0.10(2) 0.06(2) -0.004(19) 0.027(17) -0.024(18) C35 0.10(2) 0.016(11) 0.13(3) -0.028(16) 0.02(2) -0.004(15) C40 0.027(18) 0.058(15) 0.054(18) 0.010(15) 0.024(15) 0.017(13) C41 0.09(2) 0.050(15) 0.071(19) -0.014(15) -0.02(2) 0.028(19) C42 0.12(3) 0.018(13) 0.11(3) 0.006(15) 0.01(3) -0.016(17) C43 0.05(2) 0.10(3) 0.11(3) 0.03(3) 0.03(2) 0.01(2) C44 0.093(13) 0.097(12) 0.097(13) -0.001(5) -0.002(5) 0.000(5) C45 0.06(2) 0.08(2) 0.11(3) -0.01(2) 0.02(2) 0.001(18) B1 0.042(10) 0.036(10) 0.041(10) 0.000(5) 0.000(5) -0.002(5) _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 N4 2.04(2) . ? U1 N21 2.48(2) . ? U1 N11 2.501(19) . ? U1 N31 2.536(19) . ? U1 Cl1 2.600(6) . ? U1 Cl2 2.620(7) . ? Si1 C8 1.82(3) . ? Si1 C6 1.83(4) . ? Si1 C7 1.90(3) . ? Si1 C5 1.91(2) . ? N4 C4 1.33(3) . ? N11 N12 1.37(3) . ? N11 C11 1.37(3) . ? N12 C13 1.36(3) . ? N12 B1 1.53(4) . ? N21 C21 1.39(3) . ? N21 N22 1.41(2) . ? N22 C23 1.31(3) . ? N22 B1 1.65(4) . ? N31 C31 1.36(3) . ? N31 N32 1.38(2) . ? N32 C33 1.36(3) . ? N32 B1 1.40(4) . ? C4 C5 1.47(3) . ? C4 C40 1.48(3) . ? C11 C12 1.41(3) . ? C11 C14 1.44(3) . ? C12 C13 1.33(3) . ? C13 C15 1.51(3) . ? C21 C22 1.31(4) . ? C21 C24 1.53(4) . ? C22 C23 1.40(4) . ? C23 C25 1.49(3) . ? C31 C32 1.36(3) . ? C31 C34 1.50(3) . ? C32 C33 1.33(4) . ? C33 C35 1.48(3) . ? C40 C41 1.33(3) . ? C40 C45 1.41(3) . ? C41 C42 1.37(3) . ? C42 C43 1.37(4) . ? C43 C44 1.33(4) . ? C44 C45 1.37(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 U1 N21 162.9(7) . . ? N4 U1 N11 91.7(7) . . ? N21 U1 N11 75.5(6) . . ? N4 U1 N31 90.4(8) . . ? N21 U1 N31 75.5(7) . . ? N11 U1 N31 75.0(7) . . ? N4 U1 Cl1 98.2(6) . . ? N21 U1 Cl1 92.0(5) . . ? N11 U1 Cl1 163.5(5) . . ? N31 U1 Cl1 91.7(5) . . ? N4 U1 Cl2 99.7(6) . . ? N21 U1 Cl2 92.0(5) . . ? N11 U1 Cl2 91.4(5) . . ? N31 U1 Cl2 163.3(5) . . ? Cl1 U1 Cl2 99.9(2) . . ? C8 Si1 C6 110.7(14) . . ? C8 Si1 C7 109.6(13) . . ? C6 Si1 C7 110.6(16) . . ? C8 Si1 C5 110.4(11) . . ? C6 Si1 C5 109.4(10) . . ? C7 Si1 C5 106.0(14) . . ? C4 N4 U1 174.4(18) . . ? N12 N11 C11 109.1(19) . . ? N12 N11 U1 124.9(14) . . ? C11 N11 U1 125.8(15) . . ? N11 N12 C13 107.7(18) . . ? N11 N12 B1 116(3) . . ? C13 N12 B1 135(3) . . ? C21 N21 N22 103(2) . . ? C21 N21 U1 134.8(19) . . ? N22 N21 U1 122.1(15) . . ? C23 N22 N21 111(2) . . ? C23 N22 B1 131(2) . . ? N21 N22 B1 118(2) . . ? C31 N31 N32 109(2) . . ? C31 N31 U1 131.2(17) . . ? N32 N31 U1 119.5(16) . . ? C33 N32 N31 105(2) . . ? C33 N32 B1 131(3) . . ? N31 N32 B1 123(2) . . ? N4 C4 C5 118(2) . . ? N4 C4 C40 119(2) . . ? C5 C4 C40 123(2) . . ? C4 C5 Si1 113.5(15) . . ? N11 C11 C12 105(2) . . ? N11 C11 C14 127(2) . . ? C12 C11 C14 128(2) . . ? C13 C12 C11 109(2) . . ? C12 C13 N12 109(2) . . ? C12 C13 C15 131(2) . . ? N12 C13 C15 119(2) . . ? C22 C21 N21 111(3) . . ? C22 C21 C24 135(3) . . ? N21 C21 C24 114(3) . . ? C21 C22 C23 108(3) . . ? N22 C23 C22 107(3) . . ? N22 C23 C25 124(2) . . ? C22 C23 C25 128(3) . . ? C32 C31 N31 107(2) . . ? C32 C31 C34 134(3) . . ? N31 C31 C34 119(2) . . ? C33 C32 C31 109(3) . . ? C32 C33 N32 110(3) . . ? C32 C33 C35 129(3) . . ? N32 C33 C35 121(3) . . ? C41 C40 C45 114(3) . . ? C41 C40 C4 123(3) . . ? C45 C40 C4 123(3) . . ? C40 C41 C42 125(3) . . ? C43 C42 C41 118(3) . . ? C44 C43 C42 122(3) . . ? C43 C44 C45 117(4) . . ? C44 C45 C40 124(3) . . ? N32 B1 N12 117(3) . . ? N32 B1 N22 115(3) . . ? N12 B1 N22 104(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.880 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.191 # ===END data_utpclnet _database_code_depnum_ccdc_archive 'CCDC 276942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H32 B Cl2 N7 U' _chemical_formula_sum 'C19 H32 B Cl2 N7 U' _chemical_formula_weight 678.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.942(5) _cell_length_b 17.310(3) _cell_length_c 14.541(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 109.01(3) _cell_angle_gamma 90.000(5) _cell_volume 2603.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 6.458 _exptl_absorpt_correction_type 'psi-scan (North,1968)' _exptl_absorpt_correction_T_min 0.1402 _exptl_absorpt_correction_T_max 0.2710 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type cad4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 4780 _diffrn_reflns_av_R_equivalents 0.1275 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4526 _reflns_number_gt 2834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0684P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4526 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 U U 0.11461(4) 0.16379(3) 0.29761(3) 0.03025(17) Uani 1 1 d . . . Cl1 Cl 0.3426(4) 0.1771(3) 0.2751(3) 0.0648(12) Uani 1 1 d . . . Cl2 Cl 0.0516(5) 0.3107(2) 0.2760(3) 0.0655(12) Uani 1 1 d . . . B B -0.1163(14) 0.0248(9) 0.1668(11) 0.037(4) Uani 1 1 d . . . H H -0.1785 -0.0145 0.1315 0.07(5) Uiso 1 1 calc R . . N11 N -0.1120(9) 0.1287(6) 0.2894(7) 0.033(3) Uani 1 1 d . . . N12 N -0.1822(9) 0.0751(6) 0.2233(8) 0.034(3) Uani 1 1 d . . . N21 N 0.0052(10) 0.1344(6) 0.1226(8) 0.034(3) Uani 1 1 d . . . N22 N -0.0799(10) 0.0722(6) 0.0933(8) 0.036(3) Uani 1 1 d . . . N31 N 0.1147(11) 0.0210(6) 0.2810(8) 0.041(3) Uani 1 1 d . . . N32 N 0.0002(10) -0.0171(5) 0.2372(7) 0.033(3) Uani 1 1 d . . . C11 C -0.1939(12) 0.1649(8) 0.3295(10) 0.040(3) Uani 1 1 d . . . C12 C -0.3131(15) 0.1355(9) 0.2881(11) 0.048(4) Uani 1 1 d . . . H12 H -0.3881 0.1499 0.3006 0.058 Uiso 1 1 calc R . . C13 C -0.3022(13) 0.0806(9) 0.2246(12) 0.051(4) Uani 1 1 d . . . C14 C -0.1489(17) 0.2248(9) 0.4057(13) 0.073(5) Uani 1 1 d . . . H14A H -0.0574 0.2320 0.4211 0.110 Uiso 1 1 calc R . . H14B H -0.1673 0.2086 0.4630 0.110 Uiso 1 1 calc R . . H14C H -0.1928 0.2725 0.3825 0.110 Uiso 1 1 calc R . . C15 C -0.4117(14) 0.0310(11) 0.1557(14) 0.088(7) Uani 1 1 d . . . H15A H -0.3759 -0.0035 0.1194 0.131 Uiso 1 1 calc R . . H15B H -0.4741 0.0642 0.1116 0.131 Uiso 1 1 calc R . . H15C H -0.4529 0.0016 0.1932 0.131 Uiso 1 1 calc R . . C21 C 0.0099(12) 0.1683(8) 0.0426(10) 0.043(3) Uani 1 1 d . . . C22 C -0.0691(15) 0.1314(9) -0.0364(11) 0.052(4) Uani 1 1 d . . . H22 H -0.0825 0.1445 -0.1010 0.063 Uiso 1 1 calc R . . C23 C -0.1245(12) 0.0727(8) -0.0051(9) 0.040(3) Uani 1 1 d . . . C24 C 0.0950(16) 0.2373(8) 0.0451(12) 0.062(5) Uani 1 1 d . . . H24A H 0.1401 0.2511 0.1114 0.092 Uiso 1 1 calc R . . H24B H 0.0427 0.2799 0.0124 0.092 Uiso 1 1 calc R . . H24C H 0.1564 0.2247 0.0129 0.092 Uiso 1 1 calc R . . C25 C -0.2222(14) 0.0115(10) -0.0630(10) 0.062(4) Uani 1 1 d . . . H25A H -0.2446 -0.0222 -0.0187 0.093 Uiso 1 1 calc R . . H25B H -0.1840 -0.0180 -0.1025 0.093 Uiso 1 1 calc R . . H25C H -0.2986 0.0369 -0.1040 0.093 Uiso 1 1 calc R . . C31 C 0.1993(15) -0.0340(8) 0.3263(11) 0.053(4) Uani 1 1 d . . . C32 C 0.1422(14) -0.1040(8) 0.3161(10) 0.051(4) Uani 1 1 d . . . H32 H 0.1806 -0.1506 0.3419 0.061 Uiso 1 1 calc R . . C33 C 0.0175(14) -0.0925(7) 0.2608(9) 0.038(3) Uani 1 1 d . . . C34 C 0.3384(15) -0.0137(10) 0.3795(13) 0.076(5) Uani 1 1 d . . . H34A H 0.3506 0.0409 0.3749 0.114 Uiso 1 1 calc R . . H34B H 0.3934 -0.0410 0.3509 0.114 Uiso 1 1 calc R . . H34C H 0.3598 -0.0281 0.4467 0.114 Uiso 1 1 calc R . . C35 C -0.0895(14) -0.1508(8) 0.2227(12) 0.060(5) Uani 1 1 d . . . H35A H -0.1675 -0.1247 0.1858 0.091 Uiso 1 1 calc R . . H35B H -0.1034 -0.1775 0.2763 0.091 Uiso 1 1 calc R . . H35C H -0.0657 -0.1873 0.1818 0.091 Uiso 1 1 calc R . . N4 N 0.1600(11) 0.1452(6) 0.4512(7) 0.041(3) Uani 1 1 d . . . C40 C 0.2518(14) 0.2061(9) 0.5011(10) 0.052(4) Uani 1 1 d . . . H40A H 0.2759 0.2354 0.4528 0.063 Uiso 1 1 calc R . . H40B H 0.3294 0.1819 0.5439 0.063 Uiso 1 1 calc R . . C41 C 0.2006(19) 0.2614(10) 0.5601(13) 0.079(6) Uani 1 1 d . . . H41A H 0.2659 0.2988 0.5908 0.119 Uiso 1 1 calc R . . H41B H 0.1777 0.2332 0.6089 0.119 Uiso 1 1 calc R . . H41C H 0.1255 0.2873 0.5181 0.119 Uiso 1 1 calc R . . C42 C 0.1135(16) 0.0942(9) 0.5091(11) 0.059(4) Uani 1 1 d . . . H42A H 0.0511 0.0592 0.4665 0.070 Uiso 1 1 calc R . . H42B H 0.0688 0.1243 0.5446 0.070 Uiso 1 1 calc R . . C43 C 0.217(2) 0.0473(11) 0.5805(14) 0.102(8) Uani 1 1 d . . . H43A H 0.1791 0.0144 0.6168 0.153 Uiso 1 1 calc R . . H43B H 0.2784 0.0813 0.6242 0.153 Uiso 1 1 calc R . . H43C H 0.2608 0.0163 0.5460 0.153 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 U 0.0239(2) 0.0309(2) 0.0330(3) -0.0021(3) 0.00525(17) -0.0030(3) Cl1 0.038(2) 0.081(3) 0.078(3) 0.005(2) 0.023(2) -0.006(2) Cl2 0.087(3) 0.038(2) 0.071(3) 0.0089(19) 0.025(3) 0.010(2) B 0.027(8) 0.044(9) 0.029(8) -0.011(7) -0.007(7) -0.011(7) N11 0.021(6) 0.035(6) 0.034(6) 0.016(5) -0.003(5) 0.003(5) N12 0.014(5) 0.039(6) 0.044(7) 0.011(5) 0.003(5) 0.001(5) N21 0.031(6) 0.037(6) 0.032(6) -0.001(5) 0.008(5) -0.011(5) N22 0.032(6) 0.034(6) 0.036(7) 0.004(5) 0.004(5) 0.004(5) N31 0.036(6) 0.030(6) 0.044(7) 0.001(5) -0.003(6) 0.010(6) N32 0.040(7) 0.020(6) 0.034(6) -0.010(5) 0.006(5) -0.006(5) C11 0.025(7) 0.035(7) 0.061(9) -0.002(8) 0.016(6) 0.010(7) C12 0.049(10) 0.048(9) 0.051(10) 0.021(7) 0.020(8) 0.023(7) C13 0.025(7) 0.059(10) 0.062(10) 0.026(9) 0.007(7) -0.001(7) C14 0.064(12) 0.066(11) 0.091(14) -0.027(10) 0.028(11) 0.022(9) C15 0.021(8) 0.106(16) 0.122(18) -0.016(13) 0.006(10) -0.028(9) C21 0.034(7) 0.050(8) 0.044(8) -0.008(8) 0.009(6) -0.006(7) C22 0.064(11) 0.067(10) 0.033(8) 0.005(8) 0.027(8) 0.010(9) C23 0.030(7) 0.054(9) 0.028(8) -0.001(7) -0.005(6) 0.012(7) C24 0.074(12) 0.060(10) 0.061(11) 0.010(9) 0.036(10) -0.018(9) C25 0.056(10) 0.075(11) 0.036(8) -0.014(8) -0.011(7) -0.002(9) C31 0.057(10) 0.043(9) 0.049(10) -0.005(7) 0.002(8) 0.010(8) C32 0.062(11) 0.038(8) 0.049(10) 0.006(7) 0.014(9) 0.021(7) C33 0.056(9) 0.033(8) 0.032(8) -0.016(6) 0.022(7) 0.002(7) C34 0.055(11) 0.076(12) 0.073(12) 0.000(10) -0.012(9) 0.032(10) C35 0.055(10) 0.037(9) 0.097(14) -0.003(8) 0.036(10) -0.005(7) N4 0.046(7) 0.046(7) 0.026(6) 0.002(5) 0.002(5) -0.010(5) C40 0.045(9) 0.068(10) 0.032(8) -0.009(8) -0.002(7) -0.007(8) C41 0.097(15) 0.083(13) 0.065(12) -0.037(10) 0.036(11) -0.045(11) C42 0.072(11) 0.057(10) 0.040(9) 0.015(8) 0.008(8) -0.005(9) C43 0.15(2) 0.087(15) 0.059(13) 0.018(11) 0.028(14) 0.007(14) _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 U N4 2.148(10) . ? U N31 2.483(10) . ? U N21 2.487(10) . ? U N11 2.518(10) . ? U Cl2 2.627(4) . ? U Cl1 2.629(4) . ? U C40 2.942(13) . ? B N22 1.500(18) . ? B N12 1.530(18) . ? B N32 1.533(17) . ? N11 C11 1.370(16) . ? N11 N12 1.376(14) . ? N12 C13 1.323(17) . ? N21 C21 1.318(17) . ? N21 N22 1.396(14) . ? N22 C23 1.352(15) . ? N31 C31 1.341(17) . ? N31 N32 1.376(14) . ? N32 C33 1.346(16) . ? C11 C12 1.346(19) . ? C11 C14 1.48(2) . ? C12 C13 1.36(2) . ? C13 C15 1.55(2) . ? C21 C22 1.353(19) . ? C21 C24 1.508(18) . ? C22 C23 1.337(19) . ? C23 C25 1.544(19) . ? C31 C32 1.35(2) . ? C31 C34 1.51(2) . ? C32 C33 1.354(19) . ? C33 C35 1.508(18) . ? N4 C42 1.424(17) . ? N4 C40 1.475(17) . ? C40 C41 1.51(2) . ? C42 C43 1.50(2) . ? 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 N4 U N31 86.8(4) . . ? N4 U N21 154.7(4) . . ? N31 U N21 73.3(3) . . ? N4 U N11 84.5(4) . . ? N31 U N11 77.7(4) . . ? N21 U N11 76.3(3) . . ? N4 U Cl2 103.4(3) . . ? N31 U Cl2 163.8(3) . . ? N21 U Cl2 93.2(3) . . ? N11 U Cl2 90.7(3) . . ? N4 U Cl1 103.6(3) . . ? N31 U Cl1 92.5(3) . . ? N21 U Cl1 92.9(3) . . ? N11 U Cl1 167.1(3) . . ? Cl2 U Cl1 97.08(14) . . ? N4 U C40 28.6(4) . . ? N31 U C40 109.2(4) . . ? N21 U C40 176.6(4) . . ? N11 U C40 106.3(4) . . ? Cl2 U C40 84.7(3) . . ? Cl1 U C40 84.8(3) . . ? N22 B N12 110.6(11) . . ? N22 B N32 112.3(11) . . ? N12 B N32 110.2(10) . . ? C11 N11 N12 108.2(10) . . ? C11 N11 U 129.8(9) . . ? N12 N11 U 120.9(8) . . ? C13 N12 N11 105.8(12) . . ? C13 N12 B 133.9(13) . . ? N11 N12 B 120.4(9) . . ? C21 N21 N22 106.7(10) . . ? C21 N21 U 131.9(8) . . ? N22 N21 U 121.4(7) . . ? C23 N22 N21 107.0(10) . . ? C23 N22 B 131.9(11) . . ? N21 N22 B 120.7(10) . . ? C31 N31 N32 105.4(10) . . ? C31 N31 U 132.9(9) . . ? N32 N31 U 119.6(7) . . ? C33 N32 N31 108.4(10) . . ? C33 N32 B 130.2(11) . . ? N31 N32 B 121.1(10) . . ? C12 C11 N11 108.0(13) . . ? C12 C11 C14 129.6(14) . . ? N11 C11 C14 122.4(12) . . ? C11 C12 C13 106.4(14) . . ? N12 C13 C12 111.6(14) . . ? N12 C13 C15 120.8(15) . . ? C12 C13 C15 127.5(15) . . ? N21 C21 C22 110.0(13) . . ? N21 C21 C24 122.2(12) . . ? C22 C21 C24 127.8(14) . . ? C23 C22 C21 107.7(13) . . ? C22 C23 N22 108.5(12) . . ? C22 C23 C25 130.1(13) . . ? N22 C23 C25 121.3(13) . . ? N31 C31 C32 111.3(13) . . ? N31 C31 C34 120.4(14) . . ? C32 C31 C34 128.2(14) . . ? C31 C32 C33 105.9(13) . . ? N32 C33 C32 108.9(12) . . ? N32 C33 C35 121.8(13) . . ? C32 C33 C35 129.1(13) . . ? C42 N4 C40 118.0(11) . . ? C42 N4 U 134.6(9) . . ? C40 N4 U 107.1(8) . . ? N4 C40 C41 114.5(13) . . ? N4 C40 U 44.3(6) . . ? C41 C40 U 124.6(11) . . ? N4 C42 C43 114.1(15) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.229 _refine_diff_density_min -2.069 _refine_diff_density_rms 0.198 # ===END data_utpclnph _database_code_depnum_ccdc_archive 'CCDC 276943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H32 B Cl2 N7 U' _chemical_formula_sum 'C27 H32 B Cl2 N7 U' _chemical_formula_weight 774.34 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' B B 0.0013 0.0007 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1647(11) _cell_length_b 10.2881(11) _cell_length_c 18.947(2) _cell_angle_alpha 75.667(9) _cell_angle_beta 88.415(11) _cell_angle_gamma 78.416(10) _cell_volume 1510.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description plate _exptl_crystal_colour 'golden brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 5.580 _exptl_absorpt_correction_type 'psi-scan (North,1968)' _exptl_absorpt_correction_T_min 0.3314 _exptl_absorpt_correction_T_max 0.4941 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type cad4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 5697 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.2274 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5297 _reflns_number_gt 2849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5297 _refine_ls_number_parameters 347 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1762 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _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 U U 0.51066(9) 0.40175(6) 0.76331(4) 0.03462(18) Uani 1 1 d . . . Cl1 Cl 0.7967(5) 0.2700(4) 0.7288(2) 0.0526(12) Uani 1 1 d . . . Cl2 Cl 0.4010(5) 0.1976(4) 0.8476(2) 0.0613(13) Uani 1 1 d . . . N11 N 0.2997(14) 0.5647(11) 0.8115(6) 0.035(3) Uani 1 1 d . . . N12 N 0.3360(15) 0.6761(11) 0.8286(6) 0.041(3) Uani 1 1 d . . . N21 N 0.6487(14) 0.4320(13) 0.8723(7) 0.045(4) Uani 1 1 d . . . N22 N 0.6167(14) 0.5592(11) 0.8883(6) 0.038(3) Uani 1 1 d . . . N31 N 0.6072(13) 0.6197(10) 0.7215(6) 0.032(3) Uani 1 1 d . . . N32 N 0.5962(14) 0.7135(12) 0.7622(6) 0.044(3) Uani 1 1 d . . . B B 0.522(2) 0.6903(18) 0.8377(10) 0.042(5) Uani 1 1 d . . . H H 0.509(11) 0.766(8) 0.865(5) 0.01(3) Uiso 1 1 d . . . C11 C 0.1311(17) 0.5830(16) 0.8084(8) 0.047(4) Uani 1 1 d . . . C12 C 0.0626(17) 0.7005(14) 0.8255(7) 0.041(4) Uani 1 1 d . . . H12 H -0.0509 0.7337 0.8297 0.049 Uiso 1 1 calc R . . C13 C 0.192(2) 0.7635(14) 0.8358(7) 0.043(4) Uani 1 1 d . . . C14 C 0.0399(16) 0.4811(11) 0.7887(7) 0.048(4) Uani 1 1 d U . . H14A H 0.1201 0.4059 0.7790 0.072 Uiso 1 1 calc R . . H14B H -0.0299 0.5255 0.7462 0.072 Uiso 1 1 calc R . . H14C H -0.0279 0.4476 0.8286 0.072 Uiso 1 1 calc R . . C15 C 0.1867(17) 0.8963(13) 0.8561(8) 0.072(6) Uani 1 1 d . . . H15A H 0.2986 0.9106 0.8594 0.108 Uiso 1 1 calc R . . H15B H 0.1342 0.8932 0.9022 0.108 Uiso 1 1 calc R . . H15C H 0.1241 0.9701 0.8195 0.108 Uiso 1 1 calc R . . C21 C 0.747(2) 0.3431(16) 0.9235(9) 0.056(5) Uani 1 1 d . . . C22 C 0.7853(18) 0.4123(15) 0.9725(8) 0.054(5) Uani 1 1 d . . . H22 H 0.8564 0.3739 1.0131 0.065 Uiso 1 1 calc R . . C23 C 0.7031(18) 0.5454(17) 0.9526(8) 0.048(4) Uani 1 1 d . . . C24 C 0.803(2) 0.1971(13) 0.9248(8) 0.076(6) Uani 1 1 d . . . H24A H 0.7568 0.1787 0.8832 0.114 Uiso 1 1 calc R . . H24B H 0.7659 0.1421 0.9685 0.114 Uiso 1 1 calc R . . H24C H 0.9230 0.1755 0.9236 0.114 Uiso 1 1 calc R . . C25 C 0.6970(18) 0.6649(14) 0.9864(7) 0.072(6) Uani 1 1 d . . . H25A H 0.6264 0.7449 0.9569 0.107 Uiso 1 1 calc R . . H25B H 0.8078 0.6817 0.9893 0.107 Uiso 1 1 calc R . . H25C H 0.6529 0.6439 1.0345 0.107 Uiso 1 1 calc R . . C31 C 0.6819(18) 0.6720(14) 0.6582(9) 0.038(4) Uani 1 1 d . . . C32 C 0.7174(17) 0.7989(12) 0.6578(8) 0.047(4) Uani 1 1 d . . . H32 H 0.7671 0.8558 0.6213 0.056 Uiso 1 1 calc R . . C33 C 0.6613(17) 0.8207(13) 0.7247(8) 0.037(4) Uani 1 1 d . . . C34 C 0.7135(17) 0.5979(12) 0.5994(7) 0.053(5) Uani 1 1 d . . . H34A H 0.6763 0.5126 0.6143 0.080 Uiso 1 1 calc R . . H34B H 0.8311 0.5804 0.5901 0.080 Uiso 1 1 calc R . . H34C H 0.6535 0.6528 0.5558 0.080 Uiso 1 1 calc R . . C35 C 0.6654(18) 0.9457(12) 0.7529(8) 0.065(5) Uani 1 1 d . . . H35A H 0.6188 0.9342 0.8006 0.098 Uiso 1 1 calc R . . H35B H 0.6010 1.0255 0.7205 0.098 Uiso 1 1 calc R . . H35C H 0.7790 0.9567 0.7554 0.098 Uiso 1 1 calc R . . N4 N 0.3590(13) 0.4565(10) 0.6605(6) 0.030(3) Uani 1 1 d . . . C40 C 0.369(2) 0.3308(14) 0.6397(8) 0.040(4) Uani 1 1 d . . . C41 C 0.2536(17) 0.2487(13) 0.6634(7) 0.042(4) Uani 1 1 d . . . H41 H 0.1700 0.2764 0.6940 0.051 Uiso 1 1 calc R . . C42 C 0.2564(19) 0.1275(15) 0.6440(9) 0.059(5) Uani 1 1 d . . . H42 H 0.1768 0.0744 0.6606 0.071 Uiso 1 1 calc R . . C43 C 0.380(2) 0.0892(15) 0.5997(9) 0.061(5) Uani 1 1 d . . . H43 H 0.3827 0.0080 0.5860 0.073 Uiso 1 1 calc R . . C44 C 0.501(2) 0.1625(16) 0.5738(9) 0.073(6) Uani 1 1 d . . . H44 H 0.5839 0.1339 0.5432 0.088 Uiso 1 1 calc R . . C45 C 0.4915(18) 0.2826(14) 0.5964(8) 0.053(5) Uani 1 1 d . . . H45 H 0.5739 0.3335 0.5811 0.064 Uiso 1 1 calc R . . C46 C 0.2610(18) 0.5720(14) 0.6124(8) 0.040(4) Uani 1 1 d . . . C47 C 0.2339(16) 0.6987(12) 0.6295(8) 0.039(4) Uani 1 1 d . . . H47 H 0.2785 0.7061 0.6726 0.047 Uiso 1 1 calc R . . C48 C 0.141(2) 0.8132(13) 0.5830(8) 0.056(5) Uani 1 1 d . . . H48 H 0.1225 0.8965 0.5958 0.067 Uiso 1 1 calc R . . C49 C 0.0749(19) 0.8065(14) 0.5161(8) 0.056(5) Uani 1 1 d . . . H49 H 0.0171 0.8850 0.4840 0.067 Uiso 1 1 calc R . . C410 C 0.0972(18) 0.6829(15) 0.5000(8) 0.053(5) Uani 1 1 d . . . H410 H 0.0501 0.6749 0.4575 0.064 Uiso 1 1 calc R . . C411 C 0.1899(17) 0.5691(14) 0.5468(7) 0.040(4) Uani 1 1 d . . . H411 H 0.2060 0.4859 0.5341 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 U 0.0355(3) 0.0361(3) 0.0359(3) -0.0139(2) -0.0029(3) -0.0087(2) Cl1 0.035(3) 0.056(3) 0.072(3) -0.029(2) 0.006(2) -0.007(2) Cl2 0.082(4) 0.048(3) 0.061(3) -0.015(2) 0.006(3) -0.029(2) N11 0.026(8) 0.044(8) 0.044(9) -0.020(7) 0.003(7) -0.016(6) N12 0.043(9) 0.050(8) 0.044(9) -0.026(7) -0.001(7) -0.020(7) N21 0.029(8) 0.063(9) 0.046(9) -0.027(8) 0.003(7) -0.002(7) N22 0.035(8) 0.049(8) 0.036(9) -0.022(7) 0.007(7) -0.009(7) N31 0.027(7) 0.045(7) 0.026(8) -0.016(6) 0.001(6) -0.004(6) N32 0.044(9) 0.061(9) 0.030(8) -0.022(7) -0.011(7) 0.000(7) B 0.032(12) 0.052(13) 0.042(13) -0.012(11) -0.003(10) -0.007(10) C11 0.013(9) 0.088(13) 0.037(11) -0.016(9) 0.002(8) -0.006(9) C12 0.025(9) 0.061(11) 0.039(10) -0.027(9) 0.019(8) 0.003(8) C13 0.053(12) 0.048(10) 0.029(10) -0.019(8) 0.017(9) 0.000(9) C14 0.041(6) 0.054(6) 0.050(6) -0.006(4) -0.004(4) -0.018(4) C15 0.048(12) 0.070(12) 0.094(15) -0.038(11) 0.013(11) 0.020(9) C21 0.071(14) 0.053(12) 0.046(12) -0.008(10) -0.023(10) -0.014(10) C22 0.052(12) 0.068(12) 0.038(11) -0.012(10) -0.022(9) 0.002(10) C23 0.039(11) 0.087(13) 0.030(10) -0.024(10) 0.008(9) -0.027(10) C24 0.098(16) 0.042(11) 0.072(14) -0.008(10) -0.009(12) 0.015(10) C25 0.069(13) 0.110(14) 0.057(13) -0.057(11) -0.013(10) -0.018(11) C31 0.035(10) 0.035(9) 0.046(12) -0.011(8) 0.002(9) -0.006(8) C32 0.058(12) 0.017(8) 0.061(12) -0.005(8) 0.007(10) -0.005(8) C33 0.026(9) 0.031(9) 0.045(11) 0.002(8) -0.001(8) -0.001(7) C34 0.074(13) 0.055(10) 0.035(10) -0.017(8) 0.017(9) -0.021(9) C35 0.085(14) 0.028(9) 0.088(14) -0.025(9) -0.013(11) -0.008(9) N4 0.032(8) 0.027(7) 0.029(8) -0.007(6) -0.002(6) -0.003(6) C40 0.052(12) 0.045(10) 0.029(10) -0.009(8) -0.010(9) -0.018(9) C41 0.039(10) 0.045(10) 0.046(11) -0.024(8) 0.000(9) 0.001(8) C42 0.050(12) 0.060(11) 0.078(14) -0.027(10) 0.011(11) -0.024(10) C43 0.042(12) 0.054(11) 0.091(16) -0.037(11) 0.003(11) 0.002(10) C44 0.055(14) 0.077(14) 0.088(16) -0.036(12) -0.011(12) 0.008(11) C45 0.035(11) 0.053(11) 0.080(14) -0.035(10) 0.000(10) -0.008(9) C46 0.037(10) 0.044(10) 0.046(11) -0.011(9) 0.000(9) -0.021(8) C47 0.046(10) 0.032(9) 0.045(11) -0.020(8) -0.010(9) -0.010(8) C48 0.089(14) 0.027(9) 0.050(12) -0.007(8) -0.019(11) -0.008(9) C49 0.064(13) 0.043(10) 0.061(13) -0.004(9) -0.004(11) -0.021(9) C410 0.047(11) 0.085(13) 0.029(10) -0.024(10) -0.008(9) -0.003(10) C411 0.050(11) 0.045(10) 0.020(9) -0.001(8) 0.002(8) -0.011(8) _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 U N4 2.225(10) . ? U N31 2.465(11) . ? U N11 2.474(11) . ? U N21 2.493(12) . ? U Cl2 2.603(4) . ? U Cl1 2.608(4) . ? U C40 2.949(13) . ? N11 C11 1.352(15) . ? N11 N12 1.354(12) . ? N12 C13 1.355(15) . ? N12 B 1.575(19) . ? N21 C21 1.317(16) . ? N21 N22 1.389(13) . ? N22 C23 1.388(15) . ? N22 B 1.522(19) . ? N31 N32 1.365(12) . ? N31 C31 1.369(16) . ? N32 C33 1.354(15) . ? N32 B 1.52(2) . ? C11 C12 1.338(16) . ? C11 C14 1.521(16) . ? C12 C13 1.387(17) . ? C13 C15 1.500(16) . ? C21 C22 1.378(17) . ? C21 C24 1.473(16) . ? C22 C23 1.363(17) . ? C23 C25 1.512(16) . ? C31 C32 1.391(16) . ? C31 C34 1.488(16) . ? C32 C33 1.391(17) . ? C33 C35 1.516(15) . ? N4 C46 1.417(15) . ? N4 C40 1.430(14) . ? C40 C45 1.372(18) . ? C40 C41 1.380(18) . ? C41 C42 1.381(15) . ? C42 C43 1.354(18) . ? C43 C44 1.369(19) . ? C44 C45 1.393(16) . ? C46 C47 1.393(15) . ? C46 C411 1.395(17) . ? C47 C48 1.378(16) . ? C48 C49 1.414(17) . ? C49 C410 1.357(15) . ? C410 C411 1.377(16) . ? 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 N4 U N31 88.4(4) . . ? N4 U N11 89.3(4) . . ? N31 U N11 76.7(4) . . ? N4 U N21 159.1(4) . . ? N31 U N21 74.8(4) . . ? N11 U N21 75.0(4) . . ? N4 U Cl2 105.3(3) . . ? N31 U Cl2 160.9(3) . . ? N11 U Cl2 90.0(3) . . ? N21 U Cl2 88.7(3) . . ? N4 U Cl1 103.2(3) . . ? N31 U Cl1 90.1(3) . . ? N11 U Cl1 161.6(3) . . ? N21 U Cl1 89.4(3) . . ? Cl2 U Cl1 99.37(13) . . ? N4 U C40 27.8(3) . . ? N31 U C40 110.3(4) . . ? N11 U C40 110.5(4) . . ? N21 U C40 173.0(4) . . ? Cl2 U C40 87.1(3) . . ? Cl1 U C40 85.8(3) . . ? C11 N11 N12 106.9(11) . . ? C11 N11 U 128.7(10) . . ? N12 N11 U 122.4(9) . . ? N11 N12 C13 109.4(12) . . ? N11 N12 B 121.3(12) . . ? C13 N12 B 129.2(13) . . ? C21 N21 N22 109.4(12) . . ? C21 N21 U 131.0(10) . . ? N22 N21 U 119.5(9) . . ? C23 N22 N21 107.3(12) . . ? C23 N22 B 127.8(13) . . ? N21 N22 B 124.4(12) . . ? N32 N31 C31 106.2(11) . . ? N32 N31 U 123.4(9) . . ? C31 N31 U 130.4(9) . . ? C33 N32 N31 109.1(12) . . ? C33 N32 B 129.0(13) . . ? N31 N32 B 121.9(13) . . ? N32 B N22 111.2(13) . . ? N32 B N12 106.9(13) . . ? N22 B N12 108.8(13) . . ? C12 C11 N11 109.7(13) . . ? C12 C11 C14 127.2(13) . . ? N11 C11 C14 123.1(13) . . ? C11 C12 C13 107.5(13) . . ? N12 C13 C12 106.4(12) . . ? N12 C13 C15 123.4(14) . . ? C12 C13 C15 130.0(14) . . ? N21 C21 C22 107.6(14) . . ? N21 C21 C24 124.0(15) . . ? C22 C21 C24 128.4(16) . . ? C23 C22 C21 109.8(14) . . ? C22 C23 N22 105.9(13) . . ? C22 C23 C25 132.3(15) . . ? N22 C23 C25 121.8(14) . . ? N31 C31 C32 110.9(13) . . ? N31 C31 C34 121.7(13) . . ? C32 C31 C34 127.4(15) . . ? C33 C32 C31 103.9(13) . . ? N32 C33 C32 109.9(12) . . ? N32 C33 C35 123.3(14) . . ? C32 C33 C35 126.8(13) . . ? C46 N4 C40 114.2(11) . . ? C46 N4 U 140.2(8) . . ? C40 N4 U 105.5(8) . . ? C45 C40 C41 115.6(13) . . ? C45 C40 N4 123.2(14) . . ? C41 C40 N4 121.2(14) . . ? C45 C40 U 111.5(10) . . ? C41 C40 U 110.8(10) . . ? N4 C40 U 46.6(6) . . ? C40 C41 C42 123.3(14) . . ? C43 C42 C41 117.1(15) . . ? C42 C43 C44 124.2(16) . . ? C43 C44 C45 115.5(16) . . ? C40 C45 C44 124.2(16) . . ? C47 C46 C411 116.4(14) . . ? C47 C46 N4 119.4(13) . . ? C411 C46 N4 124.2(13) . . ? C48 C47 C46 120.6(14) . . ? C47 C48 C49 121.3(13) . . ? C410 C49 C48 118.4(14) . . ? C49 C410 C411 119.8(14) . . ? C410 C411 C46 123.5(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.985 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.221 #_eof # End of Crystallographic Information