# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2260 data_global # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr \^Angela Domingos' _publ_contact_author_address ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; _publ_contact_author_phone '00351 21 994 60 00' _publ_contact_author_fax '00351 21 994 14 55' _publ_contact_author_email 'angela@itn1.itn.pt' _publ_requested_journal 'J. Chem. Soc, Dalton Trans.' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Hydrotris(mesitylpyrazol-1-yl)borate U(IV) Compounds: Synthesis, Structure, and Ligand Isomerization. ; loop_ _publ_author_name _publ_author_address 'Silva, Manuela' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Domingos, \^Angela' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Pires de Matos, Antonio' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Marques, Noemia' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Trofimenko, Swiatoslaw' ; University of Delaware Newark, DE 19716-2522 USA ; # 4. TEXT _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_acknowledgements ; M. S. thanks PRAXIS XXI for a PhD grant. ; # data_ucl3msa _audit_creation_method SHELXL _chemical_name_systematic ; Hydrobis(3-mesitylpyrazolyl)(5-mesitylpyrazolyl)borato trichloro uranium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural UCl3[HB(3-Mspz)2(5-Mspz)] _chemical_formula_analytical ? _chemical_formula_sum 'C36 H40 B Cl3 N6 U' _chemical_formula_weight 911.93 _chemical_melting_point ? _chemical_compound_source ? 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' '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)/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 12.132(2) _cell_length_b 15.286(2) _cell_length_c 21.327(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.040(10) _cell_angle_gamma 90.00 _cell_volume 3894.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.8 _cell_measurement_theta_max 15.6 _exptl_crystal_description irregular _exptl_crystal_colour light-green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method ? _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 4.406 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; Crystals were grown from a concentrated dichlorometane 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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 8.5 _diffrn_reflns_number 6487 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5857 _reflns_number_observed 3473 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1196 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+1.1320P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4661 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_obs 0.0514 _refine_ls_wR_factor_all 0.2169 _refine_ls_wR_factor_obs 0.1137 _refine_ls_goodness_of_fit_all 1.094 _refine_ls_goodness_of_fit_obs 1.112 _refine_ls_restrained_S_all 1.597 _refine_ls_restrained_S_obs 1.112 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group U1 U 0.12619(4) 0.04098(3) 0.21713(2) 0.0428(2) Uani 1 d . . Cl1 Cl 0.0269(3) 0.1491(2) 0.2781(2) 0.0766(11) Uani 1 d . . Cl2 Cl 0.3252(3) 0.0906(2) 0.2558(2) 0.0704(11) Uani 1 d . . Cl3 Cl 0.0783(4) 0.1297(3) 0.1156(2) 0.0977(15) Uani 1 d . . N1 N -0.0471(8) -0.0424(6) 0.1842(5) 0.047(2) Uani 1 d . . N2 N 0.1322(8) -0.0758(6) 0.2994(5) 0.041(2) Uani 1 d . . N3 N 0.1938(8) -0.0878(5) 0.1646(4) 0.036(2) Uani 1 d . . N11 N -0.0509(7) -0.1313(5) 0.1852(5) 0.041(2) Uani 1 d . . N21 N 0.0947(7) -0.1589(6) 0.2824(5) 0.043(3) Uani 1 d . . N31 N 0.1501(8) -0.1706(6) 0.1733(5) 0.045(3) Uani 1 d . . C11 C -0.1535(9) -0.1598(8) 0.1619(5) 0.039(3) Uani 1 d . . C12 C -0.2224(10) -0.0871(8) 0.1454(6) 0.049(3) Uani 1 d . . H12 H -0.2983(10) -0.0863(8) 0.1284(6) 0.059 Uiso 1 calc R . C13 C -0.1508(12) -0.0165(8) 0.1604(6) 0.053(4) Uani 1 d . . H13 H -0.1726(12) 0.0417(8) 0.1545(6) 0.063 Uiso 1 calc R . C21 C 0.1070(11) -0.2112(8) 0.3325(7) 0.057(4) Uani 1 d . . H21 H 0.0898(11) -0.2705(8) 0.3321(7) 0.068 Uiso 1 calc R . C22 C 0.1500(12) -0.1623(9) 0.3854(7) 0.069(4) Uani 1 d . . H22 H 0.1663(12) -0.1819(9) 0.4272(7) 0.083 Uiso 1 calc R . C23 C 0.1640(10) -0.0789(8) 0.3642(6) 0.045(3) Uani 1 d . . C31 C 0.2045(11) -0.2291(8) 0.1462(6) 0.053(4) Uani 1 d . . H31 H 0.1889(11) -0.2887(8) 0.1448(6) 0.064 Uiso 1 calc R . C32 C 0.2870(11) -0.1908(8) 0.1203(6) 0.052(3) Uani 1 d . . H32 H 0.3385(11) -0.2181(8) 0.0992(6) 0.062 Uiso 1 calc R . C33 C 0.2774(10) -0.1007(7) 0.1325(5) 0.040(3) Uani 1 d . . C111 C -0.1803(8) -0.2546(7) 0.1562(6) 0.037(3) Uani 1 d . . C112 C -0.1668(9) -0.2983(8) 0.1016(6) 0.042(3) Uani 1 d . . C113 C -0.1858(10) -0.3895(8) 0.0991(6) 0.051(3) Uani 1 d . . H113 H -0.1754(10) -0.4199(8) 0.0627(6) 0.061 Uiso 1 calc R . C114 C -0.2185(10) -0.4345(8) 0.1473(7) 0.053(4) Uani 1 d . . C115 C -0.2345(10) -0.3871(9) 0.2013(7) 0.059(4) Uani 1 d . . H115 H -0.2592(10) -0.4159(9) 0.2347(7) 0.070 Uiso 1 calc R . C116 C -0.2140(9) -0.2985(8) 0.2056(6) 0.046(3) Uani 1 d . . C117 C -0.1263(12) -0.2531(9) 0.0477(6) 0.065(4) Uani 1 d . . H11A H -0.1226(12) -0.2943(9) 0.0142(6) 0.098 Uiso 1 calc R . H11B H -0.0533(12) -0.2291(9) 0.0624(6) 0.098 Uiso 1 calc R . H11C H -0.1772(12) -0.2068(9) 0.0318(6) 0.098 Uiso 1 calc R . C118 C -0.2366(13) -0.5319(8) 0.1438(8) 0.074(4) Uani 1 d . . H11D H -0.2594(13) -0.5518(8) 0.1822(8) 0.111 Uiso 1 calc R . H11E H -0.1682(13) -0.5604(8) 0.1388(8) 0.111 Uiso 1 calc R . H11F H -0.2939(13) -0.5455(8) 0.1080(8) 0.111 Uiso 1 calc R . C119 C -0.2283(13) -0.2526(10) 0.2667(7) 0.075(5) Uani 1 d . . H11G H -0.2522(13) -0.2942(10) 0.2953(7) 0.112 Uiso 1 calc R . H11H H -0.2835(13) -0.2073(10) 0.2573(7) 0.112 Uiso 1 calc R . H11I H -0.1582(13) -0.2274(10) 0.2862(7) 0.112 Uiso 1 calc R . C233 C 0.2109(10) -0.0023(8) 0.4042(6) 0.045(3) Uani 1 d . . C234 C 0.1374(11) 0.0518(9) 0.4325(6) 0.055(3) Uani 1 d . . C235 C 0.1825(13) 0.1161(9) 0.4713(7) 0.062(4) Uani 1 d . . H235 H 0.1346(13) 0.1521(9) 0.4893(7) 0.074 Uiso 1 calc R . C236 C 0.2970(13) 0.1320(8) 0.4863(6) 0.058(4) Uani 1 d . . C237 C 0.3677(11) 0.0765(9) 0.4575(6) 0.056(4) Uani 1 d . . H237 H 0.4447(11) 0.0851(9) 0.4667(6) 0.067 Uiso 1 calc R . C238 C 0.3256(11) 0.0093(9) 0.4157(6) 0.050(3) Uani 1 d . . C239 C 0.0126(11) 0.0348(11) 0.4197(7) 0.076(4) Uani 1 d . . H23A H -0.0034(11) -0.0136(11) 0.3909(7) 0.115 Uiso 1 calc R . H23B H -0.0258(11) 0.0859(11) 0.4011(7) 0.115 Uiso 1 calc R . H23C H -0.0120(11) 0.0212(11) 0.4590(7) 0.115 Uiso 1 calc R . C240 C 0.4059(11) -0.0492(10) 0.3910(7) 0.071(4) Uani 1 d . . H24A H 0.4808(11) -0.0284(10) 0.4051(7) 0.107 Uiso 1 calc R . H24B H 0.3898(11) -0.0497(10) 0.3453(7) 0.107 Uiso 1 calc R . H24C H 0.3991(11) -0.1075(10) 0.4067(7) 0.107 Uiso 1 calc R . C241 C 0.3483(13) 0.2052(9) 0.5281(7) 0.075(5) Uani 1 d . . H24D H 0.4282(13) 0.2033(9) 0.5316(7) 0.113 Uiso 1 calc R . H24E H 0.3288(13) 0.1991(9) 0.5697(7) 0.113 Uiso 1 calc R . H24F H 0.3208(13) 0.2601(9) 0.5100(7) 0.113 Uiso 1 calc R . C333 C 0.3421(10) -0.0305(8) 0.1101(6) 0.043(3) Uani 1 d . . C334 C 0.3025(13) 0.0124(9) 0.0535(7) 0.058(4) Uani 1 d . . C335 C 0.3700(15) 0.0776(9) 0.0327(7) 0.070(5) Uani 1 d . . H335 H 0.3436(15) 0.1089(9) -0.0042(7) 0.084 Uiso 1 calc R . C336 C 0.4782(16) 0.0959(10) 0.0680(10) 0.077(5) Uani 1 d . . C337 C 0.5163(12) 0.0519(9) 0.1230(8) 0.067(4) Uani 1 d . . H337 H 0.5868(12) 0.0649(9) 0.1459(8) 0.080 Uiso 1 calc R . C338 C 0.4522(12) -0.0117(9) 0.1455(7) 0.058(4) Uani 1 d . . C339 C 0.1943(14) -0.0114(10) 0.0136(8) 0.081(5) Uani 1 d . . H33A H 0.1811(14) 0.0253(10) -0.0234(8) 0.121 Uiso 1 calc R . H33B H 0.1351(14) -0.0034(10) 0.0377(8) 0.121 Uiso 1 calc R . H33C H 0.1964(14) -0.0714(10) 0.0008(8) 0.121 Uiso 1 calc R . C340 C 0.5463(15) 0.1656(10) 0.0414(10) 0.116(8) Uani 1 d . . H34A H 0.5041(15) 0.1882(10) 0.0024(10) 0.174 Uiso 1 calc R . H34B H 0.6148(15) 0.1404(10) 0.0331(10) 0.174 Uiso 1 calc R . H34C H 0.5629(15) 0.2122(10) 0.0717(10) 0.174 Uiso 1 calc R . C341 C 0.4998(12) -0.0615(9) 0.2044(8) 0.076(5) Uani 1 d . . H34D H 0.4456(12) -0.1031(9) 0.2138(8) 0.114 Uiso 1 calc R . H34E H 0.5182(12) -0.0216(9) 0.2394(8) 0.114 Uiso 1 calc R . H34F H 0.5661(12) -0.0919(9) 0.1978(8) 0.114 Uiso 1 calc R . B B 0.0579(11) -0.1855(9) 0.2112(6) 0.037(3) Uiso 1 d . . H0 H 0.0387(11) -0.2478(9) 0.2094(6) 0.044 Uiso 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 0.0492(3) 0.0271(2) 0.0512(3) 0.0008(3) 0.0064(2) -0.0034(3) Cl1 0.083(3) 0.059(2) 0.093(3) -0.014(2) 0.030(2) 0.011(2) Cl2 0.058(2) 0.053(2) 0.102(3) -0.021(2) 0.019(2) -0.016(2) Cl3 0.143(4) 0.072(3) 0.080(3) 0.034(2) 0.021(3) 0.017(3) N1 0.047(6) 0.034(5) 0.056(7) 0.011(5) -0.001(5) 0.006(5) N2 0.035(6) 0.044(6) 0.043(7) -0.008(5) 0.011(5) -0.004(4) N3 0.046(6) 0.026(5) 0.039(6) 0.000(4) 0.012(5) -0.009(4) N11 0.036(6) 0.026(5) 0.057(7) -0.001(5) -0.001(5) 0.002(4) N21 0.037(6) 0.034(6) 0.059(7) 0.004(5) 0.013(5) -0.007(4) N31 0.039(6) 0.037(6) 0.063(8) -0.014(5) 0.022(5) 0.000(5) C11 0.032(7) 0.053(8) 0.027(7) -0.002(5) -0.011(5) -0.002(6) C12 0.032(7) 0.055(8) 0.058(9) 0.003(7) 0.002(6) 0.001(6) C13 0.071(10) 0.048(8) 0.035(8) 0.003(6) -0.002(7) 0.018(7) C21 0.061(9) 0.041(7) 0.061(10) 0.008(7) -0.008(7) -0.017(6) C22 0.082(11) 0.064(10) 0.053(10) 0.033(8) -0.007(8) -0.017(8) C23 0.038(7) 0.057(8) 0.039(8) 0.001(6) 0.003(6) -0.003(6) C31 0.072(10) 0.029(7) 0.064(9) 0.002(6) 0.025(8) -0.002(6) C32 0.067(9) 0.047(8) 0.048(9) -0.008(6) 0.027(7) 0.014(7) C33 0.049(8) 0.036(7) 0.033(7) 0.001(5) 0.003(6) -0.002(5) C111 0.021(6) 0.048(7) 0.040(8) -0.008(6) 0.003(5) -0.009(5) C112 0.030(7) 0.057(8) 0.038(8) 0.000(6) 0.008(6) -0.003(6) C113 0.049(8) 0.044(8) 0.058(9) -0.023(7) 0.008(7) 0.002(6) C114 0.037(8) 0.052(9) 0.069(10) 0.005(7) 0.009(7) 0.006(6) C115 0.047(8) 0.070(10) 0.065(10) 0.006(8) 0.031(7) -0.009(7) C116 0.035(7) 0.040(7) 0.065(9) -0.009(7) 0.013(7) -0.005(6) C117 0.075(10) 0.061(9) 0.060(10) -0.014(8) 0.012(8) 0.001(7) C118 0.085(11) 0.039(8) 0.091(12) 0.002(8) -0.003(9) -0.008(7) C119 0.094(12) 0.064(9) 0.074(11) -0.007(8) 0.035(9) -0.014(8) C233 0.035(8) 0.063(8) 0.033(8) 0.022(6) -0.006(6) -0.015(6) C234 0.041(8) 0.075(10) 0.046(8) 0.012(8) 0.003(6) 0.010(7) C235 0.074(11) 0.060(9) 0.052(9) -0.001(8) 0.017(8) 0.005(8) C236 0.078(11) 0.041(8) 0.047(9) 0.000(7) -0.006(8) -0.008(7) C237 0.049(8) 0.061(9) 0.055(9) 0.010(7) 0.000(7) -0.009(7) C238 0.048(8) 0.062(8) 0.038(8) 0.007(6) 0.002(7) -0.003(6) C239 0.048(9) 0.113(13) 0.068(10) 0.004(10) 0.010(7) 0.005(9) C240 0.049(8) 0.091(11) 0.070(10) -0.020(9) 0.000(7) 0.003(8) C241 0.089(12) 0.060(9) 0.077(12) -0.011(8) 0.015(9) -0.008(8) C333 0.041(7) 0.051(8) 0.042(7) -0.009(7) 0.022(6) 0.000(6) C334 0.080(11) 0.055(9) 0.044(9) 0.007(7) 0.023(8) 0.004(7) C335 0.107(14) 0.055(9) 0.058(10) 0.017(7) 0.043(10) 0.010(9) C336 0.089(13) 0.058(10) 0.103(15) -0.019(10) 0.068(12) -0.003(9) C337 0.057(9) 0.058(9) 0.091(12) 0.010(9) 0.032(9) 0.011(8) C338 0.062(10) 0.049(8) 0.066(10) -0.006(7) 0.021(8) 0.002(7) C339 0.103(14) 0.072(11) 0.064(11) 0.009(8) 0.008(10) 0.002(9) C340 0.112(15) 0.070(11) 0.187(22) 0.033(12) 0.086(15) -0.026(10) C341 0.043(8) 0.079(11) 0.102(13) -0.001(9) 0.002(8) -0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N1 2.454(10) . ? U1 N3 2.475(9) . ? U1 N2 2.495(10) . ? U1 Cl2 2.527(4) . ? U1 Cl3 2.534(4) . ? U1 Cl1 2.535(4) . ? N1 C13 1.33(2) . ? N1 N11 1.360(12) . ? N2 C23 1.370(15) . ? N2 N21 1.377(12) . ? N3 C33 1.333(14) . ? N3 N31 1.397(12) . ? N11 C11 1.330(13) . ? N11 B 1.575(15) . ? N21 C21 1.322(15) . ? N21 B 1.56(2) . ? N31 C31 1.305(14) . ? N31 B 1.51(2) . ? C11 C12 1.40(2) . ? C11 C111 1.48(2) . ? C12 C13 1.39(2) . ? C21 C22 1.38(2) . ? C22 C23 1.37(2) . ? C23 C233 1.50(2) . ? C31 C32 1.36(2) . ? C32 C33 1.41(2) . ? C33 C333 1.46(2) . ? C111 C116 1.37(2) . ? C111 C112 1.38(2) . ? C112 C113 1.41(2) . ? C112 C117 1.50(2) . ? C113 C114 1.35(2) . ? C114 C115 1.40(2) . ? C114 C118 1.51(2) . ? C115 C116 1.38(2) . ? C116 C119 1.52(2) . ? C233 C238 1.38(2) . ? C233 C234 1.43(2) . ? C234 C235 1.34(2) . ? C234 C239 1.51(2) . ? C235 C236 1.39(2) . ? C236 C237 1.42(2) . ? C236 C241 1.50(2) . ? C237 C238 1.40(2) . ? C238 C240 1.48(2) . ? C333 C334 1.38(2) . ? C333 C338 1.44(2) . ? C334 C335 1.41(2) . ? C334 C339 1.48(2) . ? C335 C336 1.42(2) . ? C336 C337 1.36(2) . ? C336 C340 1.52(2) . ? C337 C338 1.38(2) . ? C338 C341 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 N1 U1 N3 78.0(3) . . ? N1 U1 N2 75.4(3) . . ? N3 U1 N2 77.2(3) . . ? N1 U1 Cl2 166.1(2) . . ? N3 U1 Cl2 90.7(2) . . ? N2 U1 Cl2 94.4(2) . . ? N1 U1 Cl3 88.6(2) . . ? N3 U1 Cl3 94.8(2) . . ? N2 U1 Cl3 163.3(2) . . ? Cl2 U1 Cl3 100.5(2) . . ? N1 U1 Cl1 91.5(2) . . ? N3 U1 Cl1 167.4(2) . . ? N2 U1 Cl1 93.7(2) . . ? Cl2 U1 Cl1 98.61(13) . . ? Cl3 U1 Cl1 91.75(15) . . ? C13 N1 N11 105.6(9) . . ? C13 N1 U1 131.3(8) . . ? N11 N1 U1 123.0(7) . . ? C23 N2 N21 104.8(10) . . ? C23 N2 U1 134.7(8) . . ? N21 N2 U1 120.5(7) . . ? C33 N3 N31 106.0(8) . . ? C33 N3 U1 133.7(7) . . ? N31 N3 U1 119.8(6) . . ? C11 N11 N1 110.8(9) . . ? C11 N11 B 129.1(9) . . ? N1 N11 B 120.1(9) . . ? C21 N21 N2 111.1(10) . . ? C21 N21 B 127.0(10) . . ? N2 N21 B 121.5(9) . . ? C31 N31 N3 109.2(9) . . ? C31 N31 B 127.9(10) . . ? N3 N31 B 122.9(9) . . ? N11 C11 C12 108.2(10) . . ? N11 C11 C111 121.8(10) . . ? C12 C11 C111 129.9(10) . . ? C13 C12 C11 103.8(10) . . ? N1 C13 C12 111.6(11) . . ? N21 C21 C22 107.9(11) . . ? C23 C22 C21 106.6(12) . . ? C22 C23 N2 109.5(11) . . ? C22 C23 C233 126.5(12) . . ? N2 C23 C233 124.0(11) . . ? N31 C31 C32 110.5(10) . . ? C31 C32 C33 104.9(11) . . ? N3 C33 C32 109.4(10) . . ? N3 C33 C333 124.1(10) . . ? C32 C33 C333 126.3(11) . . ? C116 C111 C112 120.5(11) . . ? C116 C111 C11 120.3(10) . . ? C112 C111 C11 119.1(11) . . ? C111 C112 C113 117.9(11) . . ? C111 C112 C117 121.9(11) . . ? C113 C112 C117 120.0(11) . . ? C114 C113 C112 122.7(12) . . ? C113 C114 C115 117.6(12) . . ? C113 C114 C118 121.7(13) . . ? C115 C114 C118 120.8(13) . . ? C116 C115 C114 120.9(12) . . ? C111 C116 C115 120.3(12) . . ? C111 C116 C119 121.9(11) . . ? C115 C116 C119 117.8(12) . . ? C238 C233 C234 122.4(12) . . ? C238 C233 C23 118.1(12) . . ? C234 C233 C23 119.3(11) . . ? C235 C234 C233 118.0(12) . . ? C235 C234 C239 121.8(13) . . ? C233 C234 C239 120.2(13) . . ? C234 C235 C236 123.7(13) . . ? C235 C236 C237 116.7(12) . . ? C235 C236 C241 124.2(14) . . ? C237 C236 C241 119.0(13) . . ? C238 C237 C236 122.3(12) . . ? C233 C238 C237 116.9(13) . . ? C233 C238 C240 124.2(13) . . ? C237 C238 C240 118.6(12) . . ? C334 C333 C338 120.7(12) . . ? C334 C333 C33 120.6(12) . . ? C338 C333 C33 118.5(11) . . ? C333 C334 C335 118.5(14) . . ? C333 C334 C339 121.5(13) . . ? C335 C334 C339 119.9(14) . . ? C334 C335 C336 120.4(14) . . ? C337 C336 C335 120.1(14) . . ? C337 C336 C340 122.9(18) . . ? C335 C336 C340 116.9(18) . . ? C336 C337 C338 121.3(15) . . ? C337 C338 C333 118.9(14) . . ? C337 C338 C341 119.4(14) . . ? C333 C338 C341 121.6(12) . . ? N31 B N21 111.7(10) . . ? N31 B N11 112.7(10) . . ? N21 B N11 106.6(9) . . ? _refine_diff_density_max 1.129 _refine_diff_density_min -1.559 _refine_diff_density_rms 0.160 # = = = END data_ucl3mss _audit_creation_method SHELXL _chemical_name_systematic ; Hydrotris(3-mesitylpyrazolyl)borato trichloro uranium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural UCl3[HB(3-Mspz)3].C7H8 _chemical_formula_analytical ? _chemical_formula_sum 'C43 H48 B Cl3 N6 U' _chemical_formula_weight 1004.06 _chemical_melting_point ? _chemical_compound_source ? 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' '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 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.413(3) _cell_length_b 15.7480(10) _cell_length_c 19.492(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4424.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.7 _cell_measurement_theta_max 12.7 _exptl_crystal_description 'irregular needle' _exptl_crystal_colour 'bright-green' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method ? _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 3.886 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.998 _exptl_special_details ; Crystals were obtained during one attempted recrystallization of UCl2[N(SiMe3)2][HB(3-Mspz)2(5-Mspz)] from a toluene 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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 31.0 _diffrn_reflns_number 3445 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1820 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 22.98 _reflns_number_total 3445 _reflns_number_observed 1949 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 493 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+37.1792P] 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 riding _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 -0.01(3) _refine_ls_number_reflns 2952 _refine_ls_number_parameters 317 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1874 _refine_ls_R_factor_obs 0.0864 _refine_ls_wR_factor_all 0.1976 _refine_ls_wR_factor_obs 0.1271 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_all 1.266 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group U1 U 0.77191(9) 0.04730(8) 0.84686(6) 0.0413(3) Uani 1 d . . Cl1 Cl 0.7876(8) 0.2033(5) 0.8708(4) 0.067(3) Uani 1 d . . Cl2 Cl 0.6317(7) 0.0300(7) 0.9251(5) 0.068(3) Uani 1 d . . Cl3 Cl 0.8865(8) 0.0020(7) 0.9385(5) 0.078(4) Uani 1 d . . N1 N 0.7583(19) -0.0934(14) 0.7965(11) 0.044(7) Uani 1 d U . N2 N 0.6797(16) 0.0717(15) 0.7397(11) 0.034(7) Uani 1 d U . N3 N 0.8946(21) 0.0505(19) 0.7552(12) 0.053(8) Uani 1 d . . N11 N 0.7656(21) -0.1064(15) 0.7232(11) 0.049(7) Uani 1 d . . N21 N 0.7063(17) 0.0331(17) 0.6797(11) 0.045(7) Uani 1 d U . N31 N 0.8749(20) 0.0124(16) 0.6899(13) 0.051(8) Uani 1 d U . C11 C 0.7533(23) -0.1866(19) 0.7096(15) 0.052(10) Uani 1 d U . H11 H 0.7555(23) -0.2091(19) 0.6655(15) 0.063 Uiso 1 calc R . C12 C 0.7365(26) -0.2345(20) 0.7673(14) 0.060(10) Uani 1 d U . H12 H 0.7259(26) -0.2926(20) 0.7706(14) 0.072 Uiso 1 calc R . C13 C 0.7394(24) -0.1736(17) 0.8202(13) 0.040(8) Uani 1 d U . C21 C 0.6484(21) 0.0570(24) 0.6300(13) 0.051(9) Uani 1 d . . H21 H 0.6495(21) 0.0384(24) 0.5848(13) 0.061 Uiso 1 calc R . C22 C 0.5865(25) 0.1145(21) 0.6580(19) 0.065(11) Uani 1 d . . H22 H 0.5389(25) 0.1415(21) 0.6343(19) 0.079 Uiso 1 calc R . C23 C 0.6067(23) 0.1254(20) 0.7266(15) 0.039(9) Uani 1 d U . C31 C 0.9557(21) 0.0226(17) 0.6538(19) 0.050(9) Uani 1 d U . H31 H 0.9640(21) 0.0016(17) 0.6096(19) 0.061 Uiso 1 calc R . C32 C 1.0212(24) 0.0649(21) 0.6874(15) 0.058(10) Uani 1 d U . H32 H 1.0797(24) 0.0796(21) 0.6710(15) 0.070 Uiso 1 calc R . C33 C 0.9843(24) 0.0830(20) 0.7525(16) 0.042(10) Uani 1 d . . C131 C 0.7198(28) -0.1860(18) 0.8951(14) 0.041(9) Uiso 1 d . . C132 C 0.6301(28) -0.1865(23) 0.9134(18) 0.056(11) Uiso 1 d . . C133 C 0.6146(23) -0.1969(18) 0.9829(15) 0.043(9) Uiso 1 d . . H133 H 0.5540(23) -0.1927(18) 0.9990(15) 0.051 Uiso 1 calc R . C134 C 0.6844(27) -0.2133(24) 1.0298(18) 0.061(11) Uiso 1 d . . C135 C 0.7754(28) -0.2140(18) 1.0073(14) 0.043(9) Uiso 1 d . . H135 H 0.8237(28) -0.2204(18) 1.0385(14) 0.052 Uiso 1 calc R . C136 C 0.7938(23) -0.2050(18) 0.9383(14) 0.036(8) Uiso 1 d . . C137 C 0.5524(23) -0.1675(20) 0.8691(16) 0.066(12) Uiso 1 d . . H13A H 0.4957(23) -0.1725(20) 0.8946(16) 0.100 Uiso 1 calc R . H13B H 0.5516(23) -0.2067(20) 0.8314(16) 0.100 Uiso 1 calc R . H13C H 0.5583(23) -0.1107(20) 0.8518(16) 0.100 Uiso 1 calc R . C138 C 0.8896(25) -0.2152(25) 0.9129(19) 0.083(14) Uiso 1 d . . H13D H 0.8907(25) -0.2072(25) 0.8641(19) 0.124 Uiso 1 calc R . H13E H 0.9115(25) -0.2711(25) 0.9238(19) 0.124 Uiso 1 calc R . H13F H 0.9290(25) -0.1738(25) 0.9344(19) 0.124 Uiso 1 calc R . C139 C 0.6687(24) -0.2279(21) 1.1077(15) 0.067(11) Uiso 1 d . . H13G H 0.7272(24) -0.2380(21) 1.1297(15) 0.101 Uiso 1 calc R . H13H H 0.6290(24) -0.2762(21) 1.1142(15) 0.101 Uiso 1 calc R . H13I H 0.6400(24) -0.1785(21) 1.1274(15) 0.101 Uiso 1 calc R . C231 C 0.5591(23) 0.1792(20) 0.7758(15) 0.044(9) Uiso 1 d . . C232 C 0.5797(28) 0.2675(26) 0.7854(20) 0.071(13) Uiso 1 d . . C233 C 0.5344(24) 0.3090(22) 0.8391(19) 0.069(11) Uiso 1 d . . H233 H 0.5530(24) 0.3635(22) 0.8513(19) 0.083 Uiso 1 calc R . C234 C 0.4654(27) 0.2725(26) 0.8731(20) 0.068(13) Uiso 1 d . . C235 C 0.4415(22) 0.1898(20) 0.8583(17) 0.052(10) Uiso 1 d . . H235 H 0.3928(22) 0.1649(20) 0.8824(17) 0.063 Uiso 1 calc R . C236 C 0.4868(26) 0.1429(24) 0.8096(18) 0.060(11) Uiso 1 d . . C237 C 0.6558(24) 0.3027(21) 0.7444(17) 0.064(11) Uiso 1 d . . H23A H 0.6747(24) 0.2618(21) 0.7106(17) 0.096 Uiso 1 calc R . H23B H 0.7073(24) 0.3157(21) 0.7738(17) 0.096 Uiso 1 calc R . H23C H 0.6352(24) 0.3535(21) 0.7219(17) 0.096 Uiso 1 calc R . C238 C 0.4197(30) 0.3250(25) 0.9260(21) 0.109(17) Uiso 1 d . . H23D H 0.3710(30) 0.2928(25) 0.9473(21) 0.163 Uiso 1 calc R . H23E H 0.3939(30) 0.3748(25) 0.9050(21) 0.163 Uiso 1 calc R . H23F H 0.4644(30) 0.3414(25) 0.9599(21) 0.163 Uiso 1 calc R . C239 C 0.4467(23) 0.0507(25) 0.7982(16) 0.074(11) Uiso 1 d . . H23G H 0.3952(23) 0.0417(25) 0.8285(16) 0.111 Uiso 1 calc R . H23H H 0.4942(23) 0.0095(25) 0.8076(16) 0.111 Uiso 1 calc R . H23I H 0.4264(23) 0.0448(25) 0.7515(16) 0.111 Uiso 1 calc R . C331 C 1.0268(24) 0.1239(23) 0.8141(17) 0.049(10) Uiso 1 d . . C332 C 1.0870(25) 0.0800(22) 0.8559(22) 0.071(11) Uiso 1 d . . C333 C 1.1212(24) 0.1210(21) 0.9097(16) 0.055(10) Uiso 1 d . . H333 H 1.1555(24) 0.0905(21) 0.9418(16) 0.066 Uiso 1 calc R . C334 C 1.1084(24) 0.2066(22) 0.9203(17) 0.053(10) Uiso 1 d . . C335 C 1.0542(23) 0.2487(24) 0.8759(17) 0.057(11) Uiso 1 d . . H335 H 1.0402(23) 0.3052(24) 0.8853(17) 0.068 Uiso 1 calc R . C336 C 1.0172(24) 0.2122(22) 0.8155(16) 0.047(9) Uiso 1 d . . C337 C 1.0999(24) -0.0165(19) 0.8465(21) 0.084(12) Uiso 1 d . . H33A H 1.0707(24) -0.0342(19) 0.8046(21) 0.126 Uiso 1 calc R . H33B H 1.0721(24) -0.0459(19) 0.8845(21) 0.126 Uiso 1 calc R . H33C H 1.1649(24) -0.0296(19) 0.8447(21) 0.126 Uiso 1 calc R . C338 C 1.1510(26) 0.2488(24) 0.9862(18) 0.083(13) Uiso 1 d . . H33D H 1.1872(26) 0.2075(24) 1.0107(18) 0.125 Uiso 1 calc R . H33E H 1.1019(26) 0.2691(24) 1.0152(18) 0.125 Uiso 1 calc R . H33F H 1.1900(26) 0.2954(24) 0.9731(18) 0.125 Uiso 1 calc R . C339 C 0.9631(25) 0.2650(22) 0.7666(18) 0.067(12) Uiso 1 d . . H33G H 0.9680(25) 0.3237(22) 0.7794(18) 0.100 Uiso 1 calc R . H33H H 0.8991(25) 0.2480(22) 0.7678(18) 0.100 Uiso 1 calc R . H33I H 0.9871(25) 0.2574(22) 0.7211(18) 0.100 Uiso 1 calc R . B1 B 0.7831(27) -0.0321(22) 0.6789(16) 0.045(10) Uani 1 d U . H1 H 0.7850(27) -0.0541(22) 0.6319(16) 0.054 Uiso 1 calc R . C1S C 1.3401(40) 0.0529(44) 0.5884(27) 0.214(29) Uiso 1 d . . H1S1 H 1.3508(40) 0.1071(44) 0.5673(27) 0.321 Uiso 1 calc R . H1S2 H 1.3893(40) 0.0147(44) 0.5763(27) 0.321 Uiso 1 calc R . H1S3 H 1.3383(40) 0.0596(44) 0.6373(27) 0.321 Uiso 1 calc R . C2S C 1.2499(36) 0.0177(28) 0.5641(22) 0.111(16) Uiso 1 d . . C3S C 1.2088(34) 0.0634(29) 0.5112(21) 0.113(16) Uiso 1 d . . H3S H 1.2324(34) 0.1132(29) 0.4924(21) 0.136 Uiso 1 calc R . C4S C 1.1328(36) 0.0264(33) 0.4922(23) 0.126(19) Uiso 1 d . . H4S H 1.0971(36) 0.0559(33) 0.4604(23) 0.151 Uiso 1 calc R . C5S C 1.0987(32) -0.0496(35) 0.5125(23) 0.118(16) Uiso 1 d . . H5S H 1.0460(32) -0.0721(35) 0.4918(23) 0.141 Uiso 1 calc R . C6S C 1.1405(37) -0.0910(32) 0.5617(25) 0.130(20) Uiso 1 d . . H6S H 1.1168(37) -0.1416(32) 0.5790(25) 0.156 Uiso 1 calc R . C7S C 1.2191(36) -0.0573(32) 0.5860(21) 0.127(16) Uiso 1 d . . H7S H 1.2529(36) -0.0868(32) 0.6188(21) 0.152 Uiso 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 0.0459(7) 0.0494(6) 0.0287(5) -0.0081(8) 0.0007(8) -0.0022(9) Cl1 0.091(8) 0.048(5) 0.062(6) -0.012(4) 0.008(6) -0.005(6) Cl2 0.066(7) 0.068(8) 0.071(6) -0.022(6) 0.021(5) -0.024(6) Cl3 0.083(9) 0.091(9) 0.059(6) 0.011(6) -0.027(6) -0.006(7) N1 0.041(8) 0.045(8) 0.045(8) 0.002(5) -0.001(5) -0.001(5) N2 0.037(8) 0.032(8) 0.033(8) -0.004(5) 0.000(5) -0.003(5) N3 0.079(24) 0.039(17) 0.040(15) 0.011(18) 0.009(17) 0.040(24) N11 0.043(19) 0.053(17) 0.050(15) -0.025(13) 0.007(17) -0.002(18) N21 0.046(9) 0.047(9) 0.042(8) -0.002(5) 0.000(5) -0.002(5) N31 0.049(9) 0.053(9) 0.050(9) -0.004(5) 0.002(5) 0.000(5) C11 0.053(11) 0.052(10) 0.051(10) -0.003(5) 0.000(5) 0.001(5) C12 0.061(11) 0.059(10) 0.059(10) 0.001(5) 0.001(5) 0.000(5) C13 0.040(10) 0.040(9) 0.041(9) -0.003(5) 0.000(5) -0.002(5) C21 0.049(22) 0.077(26) 0.027(16) 0.016(20) -0.021(16) 0.017(27) C22 0.078(29) 0.069(25) 0.049(22) -0.008(25) 0.017(27) 0.026(24) C23 0.040(10) 0.040(10) 0.038(9) -0.002(5) -0.001(5) 0.000(5) C31 0.051(10) 0.051(10) 0.050(10) -0.003(5) 0.002(5) -0.002(5) C32 0.057(11) 0.060(11) 0.057(11) -0.002(5) 0.005(5) 0.000(5) C33 0.028(23) 0.056(25) 0.042(19) -0.008(17) 0.012(19) 0.016(20) B1 0.045(11) 0.044(11) 0.045(10) 0.001(5) 0.000(5) 0.000(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 N1 2.43(2) . ? U1 N2 2.51(2) . ? U1 Cl1 2.510(8) . ? U1 N3 2.51(3) . ? U1 Cl3 2.534(10) . ? U1 Cl2 2.546(9) . ? N1 C13 1.37(3) . ? N1 N11 1.45(3) . ? N2 C23 1.37(4) . ? N2 N21 1.37(3) . ? N3 C33 1.39(4) . ? N3 N31 1.44(3) . ? N11 C11 1.30(3) . ? N11 B1 1.48(4) . ? N21 C21 1.33(3) . ? N21 B1 1.51(4) . ? N31 C31 1.37(3) . ? N31 B1 1.51(4) . ? C11 C12 1.38(3) . ? C12 C13 1.41(3) . ? C13 C131 1.50(3) . ? C21 C22 1.38(4) . ? C22 C23 1.38(4) . ? C23 C231 1.45(4) . ? C31 C32 1.33(4) . ? C32 C33 1.41(4) . ? C33 C331 1.49(4) . ? C131 C132 1.34(5) . ? C131 C136 1.39(4) . ? C132 C133 1.38(4) . ? C132 C137 1.45(4) . ? C133 C134 1.38(4) . ? C134 C135 1.38(4) . ? C134 C139 1.55(4) . ? C135 C136 1.38(4) . ? C136 C138 1.48(4) . ? C231 C236 1.36(4) . ? C231 C232 1.43(4) . ? C232 C233 1.40(5) . ? C232 C237 1.47(5) . ? C233 C234 1.33(4) . ? C234 C235 1.38(5) . ? C234 C238 1.48(5) . ? C235 C236 1.37(4) . ? C236 C239 1.58(5) . ? C331 C332 1.38(4) . ? C331 C336 1.40(4) . ? C332 C333 1.33(4) . ? C332 C337 1.54(4) . ? C333 C334 1.38(4) . ? C334 C335 1.34(4) . ? C334 C338 1.57(4) . ? C335 C336 1.41(4) . ? C336 C339 1.49(4) . ? C1S C2S 1.49(6) . ? C2S C7S 1.33(6) . ? C2S C3S 1.39(5) . ? C3S C4S 1.30(5) . ? C4S C5S 1.35(6) . ? C5S C6S 1.31(5) . ? C6S C7S 1.34(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 U1 N2 76.1(7) . . ? N1 U1 Cl1 166.9(5) . . ? N2 U1 Cl1 93.0(6) . . ? N1 U1 N3 77.8(9) . . ? N2 U1 N3 77.1(8) . . ? Cl1 U1 N3 92.8(8) . . ? N1 U1 Cl3 94.6(6) . . ? N2 U1 Cl3 167.4(6) . . ? Cl1 U1 Cl3 94.9(3) . . ? N3 U1 Cl3 92.8(6) . . ? N1 U1 Cl2 94.6(7) . . ? N2 U1 Cl2 95.4(6) . . ? Cl1 U1 Cl2 93.7(3) . . ? N3 U1 Cl2 170.4(7) . . ? Cl3 U1 Cl2 93.7(3) . . ? C13 N1 N11 102.6(21) . . ? C13 N1 U1 135.9(18) . . ? N11 N1 U1 121.5(16) . . ? C23 N2 N21 109.2(24) . . ? C23 N2 U1 130.9(19) . . ? N21 N2 U1 119.6(18) . . ? C33 N3 N31 107.7(25) . . ? C33 N3 U1 133.4(22) . . ? N31 N3 U1 118.9(22) . . ? C11 N11 N1 109.2(24) . . ? C11 N11 B1 132.3(24) . . ? N1 N11 B1 118.5(22) . . ? C21 N21 N2 108.6(25) . . ? C21 N21 B1 130.0(26) . . ? N2 N21 B1 121.0(24) . . ? C31 N31 N3 103.8(27) . . ? C31 N31 B1 136.5(28) . . ? N3 N31 B1 119.5(27) . . ? N11 C11 C12 112.9(28) . . ? C11 C12 C13 102.7(27) . . ? N1 C13 C12 112.7(24) . . ? N1 C13 C131 119.1(25) . . ? C12 C13 C131 128.1(28) . . ? N21 C21 C22 107.6(28) . . ? C21 C22 C23 109.1(33) . . ? N2 C23 C22 105.3(28) . . ? N2 C23 C231 126.7(28) . . ? C22 C23 C231 127.9(32) . . ? C32 C31 N31 114.3(32) . . ? C31 C32 C33 106.1(32) . . ? N3 C33 C32 108.1(30) . . ? N3 C33 C331 120.6(28) . . ? C32 C33 C331 131.2(32) . . ? C132 C131 C136 125.3(32) . . ? C132 C131 C13 116.1(35) . . ? C136 C131 C13 118.2(35) . . ? C131 C132 C133 114.6(36) . . ? C131 C132 C137 126.0(34) . . ? C133 C132 C137 119.0(36) . . ? C132 C133 C134 123.4(37) . . ? C133 C134 C135 118.8(33) . . ? C133 C134 C139 124.6(34) . . ? C135 C134 C139 116.5(32) . . ? C136 C135 C134 119.4(35) . . ? C135 C136 C131 117.7(34) . . ? C135 C136 C138 119.7(33) . . ? C131 C136 C138 122.6(29) . . ? C236 C231 C232 120.2(35) . . ? C236 C231 C23 116.0(32) . . ? C232 C231 C23 123.6(34) . . ? C233 C232 C231 117.1(38) . . ? C233 C232 C237 125.6(38) . . ? C231 C232 C237 116.8(36) . . ? C234 C233 C232 121.5(38) . . ? C233 C234 C235 119.5(40) . . ? C233 C234 C238 116.1(39) . . ? C235 C234 C238 124.3(39) . . ? C236 C235 C234 122.4(37) . . ? C231 C236 C235 118.4(36) . . ? C231 C236 C239 126.9(34) . . ? C235 C236 C239 114.7(33) . . ? C332 C331 C336 123.4(35) . . ? C332 C331 C33 121.2(33) . . ? C336 C331 C33 113.9(32) . . ? C333 C332 C331 117.3(34) . . ? C333 C332 C337 121.9(40) . . ? C331 C332 C337 120.0(39) . . ? C332 C333 C334 123.0(36) . . ? C335 C334 C333 117.8(35) . . ? C335 C334 C338 123.1(32) . . ? C333 C334 C338 118.9(33) . . ? C334 C335 C336 123.8(36) . . ? C331 C336 C335 112.6(33) . . ? C331 C336 C339 126.6(33) . . ? C335 C336 C339 120.3(33) . . ? N11 B1 N21 114.0(29) . . ? N11 B1 N31 115.7(28) . . ? N21 B1 N31 109.0(24) . . ? C7S C2S C3S 123.7(54) . . ? C7S C2S C1S 121.2(56) . . ? C3S C2S C1S 114.5(49) . . ? C4S C3S C2S 109.9(48) . . ? C3S C4S C5S 128.4(53) . . ? C6S C5S C4S 119.2(54) . . ? C5S C6S C7S 116.9(55) . . ? C2S C7S C6S 121.4(55) . . ? _refine_diff_density_max 1.054 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.183 # = = = END data_umsamide _audit_creation_method SHELXL _chemical_name_systematic ; Hydrobis(3-mesitylpyrazolyl)(5-mesitylpyrazolyl)borato dichloro hexamethyldisilyamide uranium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural UCl2[N(SiMe3)2][HB(3-Mspz)2(5-Mspz)] _chemical_formula_analytical ? _chemical_formula_sum 'C42 H58 B Cl2 N7 Si2 U' _chemical_formula_weight 1036.87 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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 12.538(2) _cell_length_b 14.137(2) _cell_length_c 16.016(3) _cell_angle_alpha 112.530(10) _cell_angle_beta 95.660(10) _cell_angle_gamma 92.700(10) _cell_volume 2598.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.3 _cell_measurement_theta_max 14.9 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method ? _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 3.305 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; Crystals were grown from a toluene 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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 31.6 _diffrn_reflns_number 9514 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9106 _reflns_number_observed 7343 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 629 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+2.0283P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8477 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_obs 0.0402 _refine_ls_wR_factor_all 0.0970 _refine_ls_wR_factor_obs 0.0811 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.154 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group U U 0.14197(2) 0.17169(2) 0.26680(2) 0.04385(8) Uani 1 d . . Cl1 Cl 0.00678(13) 0.01927(11) 0.16205(13) 0.0729(5) Uani 1 d . . Cl2 Cl 0.1630(2) 0.1351(2) 0.41096(14) 0.0933(6) Uani 1 d . . Si1 Si 0.3256(2) 0.1497(2) 0.11146(14) 0.0879(7) Uani 1 d . . Si2 Si 0.3173(2) -0.0109(2) 0.1901(2) 0.1074(10) Uani 1 d . . N1 N 0.0635(4) 0.2522(3) 0.1653(3) 0.0518(12) Uani 1 d . . N2 N -0.0017(3) 0.2912(3) 0.3441(3) 0.0437(11) Uani 1 d . . N3 N 0.2384(3) 0.3504(3) 0.3522(3) 0.0441(11) Uani 1 d . . N4 N 0.2749(4) 0.1067(4) 0.1910(4) 0.070(2) Uani 1 d . . N11 N 0.0516(4) 0.3548(3) 0.1933(3) 0.0476(11) Uani 1 d . . N21 N 0.0069(3) 0.3906(3) 0.3500(3) 0.0435(11) Uani 1 d . . N31 N 0.1989(3) 0.4279(3) 0.3307(3) 0.0443(11) Uani 1 d . . C1 C 0.3178(6) 0.2905(6) 0.1424(5) 0.092(2) Uani 1 d . . H1A H 0.2447(6) 0.3063(6) 0.1489(5) 0.138 Uiso 1 calc R . H1B H 0.3420(6) 0.3092(6) 0.0953(5) 0.138 Uiso 1 calc R . H1C H 0.3626(6) 0.3284(6) 0.1989(5) 0.138 Uiso 1 calc R . C2 C 0.4712(6) 0.1299(7) 0.1009(7) 0.129(4) Uani 1 d . . H2A H 0.4812(6) 0.0584(7) 0.0849(7) 0.194 Uiso 1 calc R . H2B H 0.5139(6) 0.1701(7) 0.1579(7) 0.194 Uiso 1 calc R . H2C H 0.4931(6) 0.1509(7) 0.0543(7) 0.194 Uiso 1 calc R . C3 C 0.2482(8) 0.0819(9) -0.0056(6) 0.150(5) Uani 1 d . . H3A H 0.2502(8) 0.0090(9) -0.0243(6) 0.226 Uiso 1 calc R . H3B H 0.2802(8) 0.1039(9) -0.0481(6) 0.226 Uiso 1 calc R . H3C H 0.1748(8) 0.0985(9) -0.0042(6) 0.226 Uiso 1 calc R . C4 C 0.2310(9) -0.0775(8) 0.2415(9) 0.152(5) Uani 1 d . . H4A H 0.1585(9) -0.0886(8) 0.2118(9) 0.228 Uiso 1 calc R . H4B H 0.2324(9) -0.0360(8) 0.3052(9) 0.228 Uiso 1 calc R . H4C H 0.2573(9) -0.1425(8) 0.2344(9) 0.228 Uiso 1 calc R . C5 C 0.3110(10) -0.1100(7) 0.0703(9) 0.184(6) Uani 1 d . . H5A H 0.2395(10) -0.1184(7) 0.0393(9) 0.277 Uiso 1 calc R . H5B H 0.3292(10) -0.1744(7) 0.0722(9) 0.277 Uiso 1 calc R . H5C H 0.3611(10) -0.0877(7) 0.0384(9) 0.277 Uiso 1 calc R . C6 C 0.4539(8) 0.0072(8) 0.2520(11) 0.226(9) Uani 1 d . . H6A H 0.5023(8) 0.0417(8) 0.2277(11) 0.339 Uiso 1 calc R . H6B H 0.4778(8) -0.0586(8) 0.2450(11) 0.339 Uiso 1 calc R . H6C H 0.4525(8) 0.0480(8) 0.3155(11) 0.339 Uiso 1 calc R . C11 C -0.0010(5) 0.3746(5) 0.1258(4) 0.060(2) Uani 1 d . . C12 C -0.0220(6) 0.2828(5) 0.0516(5) 0.076(2) Uani 1 d . . H12 H -0.0566(6) 0.2725(5) -0.0057(5) 0.091 Uiso 1 calc R . C13 C 0.0180(6) 0.2099(5) 0.0791(4) 0.068(2) Uani 1 d . . H13 H 0.0139(6) 0.1401(5) 0.0426(4) 0.081 Uiso 1 calc R . C21 C -0.0671(5) 0.4415(4) 0.3977(4) 0.0524(15) Uani 1 d . . H21 H -0.0773(5) 0.5102(4) 0.4106(4) 0.063 Uiso 1 calc R . C22 C -0.1257(5) 0.3781(5) 0.4250(4) 0.058(2) Uani 1 d . . H22 H -0.1825(5) 0.3943(5) 0.4597(4) 0.070 Uiso 1 calc R . C23 C -0.0833(4) 0.2845(4) 0.3903(4) 0.0441(13) Uani 1 d . . C31 C 0.2732(5) 0.5087(4) 0.3610(4) 0.055(2) Uani 1 d . . H31 H 0.2654(5) 0.5708(4) 0.3546(4) 0.066 Uiso 1 calc R . C32 C 0.3620(5) 0.4853(4) 0.4025(4) 0.059(2) Uani 1 d . . H32 H 0.4260(5) 0.5270(4) 0.4282(4) 0.070 Uiso 1 calc R . C33 C 0.3386(4) 0.3875(4) 0.3989(4) 0.0468(13) Uani 1 d . . C111 C -0.0305(6) 0.4792(5) 0.1388(4) 0.065(2) Uani 1 d . . C112 C -0.1337(7) 0.5036(6) 0.1598(5) 0.081(2) Uani 1 d . . C113 C -0.1581(9) 0.6044(7) 0.1760(6) 0.109(3) Uani 1 d . . H113 H -0.2261(9) 0.6228(7) 0.1909(6) 0.131 Uiso 1 calc R . C114 C -0.0859(11) 0.6765(7) 0.1707(7) 0.114(3) Uani 1 d . . C115 C 0.0134(9) 0.6494(6) 0.1507(6) 0.101(3) Uani 1 d . . H115 H 0.0633(9) 0.6989(6) 0.1485(6) 0.122 Uiso 1 calc R . C116 C 0.0441(7) 0.5520(5) 0.1335(5) 0.076(2) Uani 1 d . . C117 C -0.2153(7) 0.4266(7) 0.1669(7) 0.106(3) Uani 1 d . . H11A H -0.2809(7) 0.4578(7) 0.1818(7) 0.159 Uiso 1 calc R . H11B H -0.1880(7) 0.4042(7) 0.2137(7) 0.159 Uiso 1 calc R . H11C H -0.2290(7) 0.3686(7) 0.1097(7) 0.159 Uiso 1 calc R . C118 C -0.1157(12) 0.7851(8) 0.1889(10) 0.192(7) Uani 1 d . . H11D H -0.1889(12) 0.7902(8) 0.2018(10) 0.287 Uiso 1 calc R . H11E H -0.1083(12) 0.8004(8) 0.1363(10) 0.287 Uiso 1 calc R . H11F H -0.0689(12) 0.8332(8) 0.2403(10) 0.287 Uiso 1 calc R . C119 C 0.1545(7) 0.5242(7) 0.1100(6) 0.107(3) Uani 1 d . . H11G H 0.1606(7) 0.4534(7) 0.1004(6) 0.160 Uiso 1 calc R . H11H H 0.2075(7) 0.5672(7) 0.1591(6) 0.160 Uiso 1 calc R . H11I H 0.1661(7) 0.5342(7) 0.0554(6) 0.160 Uiso 1 calc R . C231 C -0.1279(4) 0.1844(4) 0.3897(4) 0.0470(13) Uani 1 d . . C232 C -0.1978(4) 0.1201(4) 0.3129(4) 0.0491(14) Uani 1 d . . C233 C -0.2448(5) 0.0299(5) 0.3136(5) 0.064(2) Uani 1 d . . H233 H -0.2889(5) -0.0148(5) 0.2620(5) 0.077 Uiso 1 calc R . C234 C -0.2283(6) 0.0045(6) 0.3879(6) 0.078(2) Uani 1 d . . C235 C -0.1597(6) 0.0690(6) 0.4626(5) 0.081(2) Uani 1 d . . H235 H -0.1464(6) 0.0510(6) 0.5125(5) 0.097 Uiso 1 calc R . C236 C -0.1098(5) 0.1602(5) 0.4656(4) 0.065(2) Uani 1 d . . C237 C -0.2243(5) 0.1472(5) 0.2317(4) 0.060(2) Uani 1 d . . H23A H -0.1855(5) 0.2115(5) 0.2417(4) 0.090 Uiso 1 calc R . H23B H -0.3002(5) 0.1530(5) 0.2231(4) 0.090 Uiso 1 calc R . H23C H -0.2043(5) 0.0943(5) 0.1784(4) 0.090 Uiso 1 calc R . C238 C -0.2842(8) -0.0943(6) 0.3871(7) 0.119(3) Uani 1 d . . H23D H -0.2638(8) -0.1000(6) 0.4442(7) 0.178 Uiso 1 calc R . H23E H -0.2632(8) -0.1524(6) 0.3385(7) 0.178 Uiso 1 calc R . H23F H -0.3608(8) -0.0925(6) 0.3781(7) 0.178 Uiso 1 calc R . C239 C -0.0407(7) 0.2322(6) 0.5524(5) 0.093(3) Uani 1 d . . H23G H -0.0378(7) 0.2020(6) 0.5969(5) 0.140 Uiso 1 calc R . H23H H -0.0714(7) 0.2968(6) 0.5759(5) 0.140 Uiso 1 calc R . H23I H 0.0308(7) 0.2433(6) 0.5392(5) 0.140 Uiso 1 calc R . C331 C 0.4039(4) 0.3323(4) 0.4446(4) 0.052(2) Uani 1 d . . C332 C 0.5004(5) 0.2960(5) 0.4144(5) 0.070(2) Uani 1 d . . C333 C 0.5615(6) 0.2488(5) 0.4621(6) 0.085(2) Uani 1 d . . H333 H 0.6243(6) 0.2218(5) 0.4406(6) 0.102 Uiso 1 calc R . C334 C 0.5328(6) 0.2405(6) 0.5391(8) 0.090(3) Uani 1 d . . C335 C 0.4409(6) 0.2814(5) 0.5693(6) 0.080(2) Uani 1 d . . H335 H 0.4212(6) 0.2778(5) 0.6226(6) 0.096 Uiso 1 calc R . C336 C 0.3753(5) 0.3280(4) 0.5250(5) 0.056(2) Uani 1 d . . C337 C 0.5413(6) 0.3122(7) 0.3355(5) 0.109(3) Uani 1 d . . H33A H 0.4897(6) 0.3455(7) 0.3105(5) 0.164 Uiso 1 calc R . H33B H 0.5520(6) 0.2469(7) 0.2896(5) 0.164 Uiso 1 calc R . H33C H 0.6084(6) 0.3546(7) 0.3560(5) 0.164 Uiso 1 calc R . C338 C 0.6014(8) 0.1870(8) 0.5868(9) 0.147(5) Uani 1 d . . H33D H 0.6621(8) 0.1639(8) 0.5547(9) 0.220 Uiso 1 calc R . H33E H 0.5596(8) 0.1290(8) 0.5881(9) 0.220 Uiso 1 calc R . H33F H 0.6262(8) 0.2340(8) 0.6480(9) 0.220 Uiso 1 calc R . C339 C 0.2785(5) 0.3767(5) 0.5656(5) 0.071(2) Uani 1 d . . H33G H 0.2420(5) 0.4054(5) 0.5265(5) 0.107 Uiso 1 calc R . H33H H 0.3011(5) 0.4303(5) 0.6244(5) 0.107 Uiso 1 calc R . H33I H 0.2305(5) 0.3256(5) 0.5719(5) 0.107 Uiso 1 calc R . B B 0.0800(5) 0.4271(5) 0.2950(4) 0.048(2) Uani 1 d . . H0 H 0.0654(5) 0.4972(5) 0.3023(4) 0.058 Uiso 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 0.03633(12) 0.03304(11) 0.05209(14) 0.00796(8) -0.00326(8) 0.00039(7) Cl1 0.0547(10) 0.0463(8) 0.0946(13) 0.0109(8) -0.0200(9) -0.0109(7) Cl2 0.122(2) 0.0836(13) 0.0839(14) 0.0494(11) -0.0071(12) -0.0047(12) Si1 0.0533(12) 0.111(2) 0.0580(13) -0.0124(12) 0.0075(10) 0.0004(11) Si2 0.0524(12) 0.0590(12) 0.162(3) -0.0065(14) -0.0077(14) 0.0164(10) N1 0.055(3) 0.042(3) 0.050(3) 0.010(2) 0.000(2) 0.001(2) N2 0.042(3) 0.037(2) 0.049(3) 0.014(2) 0.002(2) 0.001(2) N3 0.036(2) 0.037(2) 0.048(3) 0.006(2) 0.001(2) -0.003(2) N4 0.036(3) 0.065(3) 0.079(4) -0.005(3) 0.002(3) 0.008(2) N11 0.049(3) 0.045(3) 0.045(3) 0.016(2) -0.001(2) 0.001(2) N21 0.041(3) 0.036(2) 0.048(3) 0.012(2) 0.004(2) 0.004(2) N31 0.045(3) 0.038(2) 0.042(3) 0.009(2) -0.002(2) -0.008(2) C1 0.076(5) 0.136(7) 0.069(5) 0.044(5) 0.020(4) 0.009(5) C2 0.064(5) 0.126(8) 0.138(9) -0.019(6) 0.038(6) 0.004(5) C3 0.117(8) 0.199(12) 0.063(6) -0.024(6) 0.002(5) -0.011(8) C4 0.125(9) 0.115(8) 0.238(14) 0.084(9) 0.033(9) 0.064(7) C5 0.173(12) 0.076(7) 0.221(14) -0.041(8) 0.055(10) 0.005(7) C6 0.094(8) 0.089(7) 0.426(24) 0.061(11) -0.117(11) 0.004(6) C11 0.070(4) 0.061(4) 0.054(4) 0.030(3) -0.003(3) 0.002(3) C12 0.099(6) 0.066(4) 0.054(4) 0.023(4) -0.020(4) -0.002(4) C13 0.082(5) 0.056(4) 0.049(4) 0.008(3) -0.010(3) 0.001(3) C21 0.052(4) 0.041(3) 0.051(4) 0.003(3) 0.006(3) 0.010(3) C22 0.048(4) 0.058(4) 0.060(4) 0.011(3) 0.018(3) 0.004(3) C23 0.035(3) 0.047(3) 0.045(3) 0.014(3) 0.000(3) -0.002(2) C31 0.060(4) 0.041(3) 0.062(4) 0.021(3) 0.005(3) -0.011(3) C32 0.048(4) 0.051(3) 0.061(4) 0.008(3) 0.000(3) -0.014(3) C33 0.036(3) 0.045(3) 0.045(3) 0.003(3) 0.004(3) -0.006(2) C111 0.083(5) 0.065(4) 0.051(4) 0.030(3) -0.003(3) 0.009(4) C112 0.094(6) 0.080(5) 0.083(5) 0.047(4) 0.006(5) 0.016(4) C113 0.137(8) 0.108(7) 0.112(7) 0.066(6) 0.034(6) 0.053(6) C114 0.178(11) 0.080(6) 0.113(8) 0.062(6) 0.043(8) 0.033(7) C115 0.150(9) 0.074(5) 0.098(7) 0.053(5) 0.020(6) 0.001(6) C116 0.100(6) 0.068(5) 0.070(5) 0.042(4) 0.004(4) 0.005(4) C117 0.083(6) 0.108(7) 0.140(8) 0.062(6) 0.015(6) 0.012(5) C118 0.295(18) 0.094(7) 0.248(15) 0.110(9) 0.108(14) 0.089(10) C119 0.106(7) 0.108(7) 0.120(8) 0.065(6) 0.013(6) -0.015(6) C231 0.036(3) 0.050(3) 0.051(4) 0.015(3) 0.005(3) -0.004(2) C232 0.036(3) 0.050(3) 0.058(4) 0.018(3) 0.004(3) 0.003(3) C233 0.055(4) 0.057(4) 0.071(5) 0.020(3) -0.003(3) -0.012(3) C234 0.070(5) 0.073(5) 0.099(6) 0.045(4) 0.002(4) -0.018(4) C235 0.081(5) 0.090(5) 0.080(5) 0.048(4) -0.002(4) -0.015(4) C236 0.060(4) 0.078(5) 0.056(4) 0.027(4) 0.007(3) -0.009(3) C237 0.045(3) 0.061(4) 0.062(4) 0.013(3) -0.004(3) 0.002(3) C238 0.134(8) 0.094(6) 0.137(8) 0.069(6) -0.016(7) -0.047(6) C239 0.100(6) 0.109(6) 0.058(5) 0.029(4) -0.013(4) -0.026(5) C331 0.035(3) 0.039(3) 0.063(4) 0.002(3) -0.010(3) -0.008(2) C332 0.043(4) 0.062(4) 0.072(5) -0.008(3) -0.005(3) -0.001(3) C333 0.042(4) 0.063(4) 0.117(7) 0.003(5) -0.006(4) 0.012(3) C334 0.059(5) 0.061(4) 0.146(9) 0.043(5) -0.018(5) 0.005(4) C335 0.062(5) 0.067(4) 0.119(7) 0.050(5) 0.001(4) -0.005(4) C336 0.046(3) 0.041(3) 0.074(5) 0.018(3) 0.002(3) -0.006(3) C337 0.054(5) 0.166(9) 0.071(5) 0.004(5) 0.013(4) 0.021(5) C338 0.088(7) 0.136(9) 0.253(14) 0.119(10) 0.002(8) 0.036(6) C339 0.057(4) 0.081(5) 0.073(5) 0.028(4) 0.006(3) 0.003(3) B 0.049(4) 0.041(3) 0.051(4) 0.016(3) 0.000(3) 0.003(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 U N4 2.188(5) . ? U N1 2.474(5) . ? U N3 2.541(4) . ? U Cl2 2.545(2) . ? U Cl1 2.5799(15) . ? U N2 2.599(4) . ? U Si2 3.412(2) . ? Si1 N4 1.764(7) . ? Si1 C1 1.868(9) . ? Si1 C2 1.874(8) . ? Si1 C3 1.885(8) . ? Si2 N4 1.764(6) . ? Si2 C6 1.847(9) . ? Si2 C4 1.847(11) . ? Si2 C5 1.884(11) . ? N1 C13 1.330(7) . ? N1 N11 1.364(6) . ? N2 C23 1.340(7) . ? N2 N21 1.370(6) . ? N3 C33 1.365(6) . ? N3 N31 1.368(6) . ? N11 C11 1.339(7) . ? N11 B 1.549(8) . ? N21 C21 1.320(7) . ? N21 B 1.531(8) . ? N31 C31 1.340(7) . ? N31 B 1.541(8) . ? C11 C12 1.374(9) . ? C11 C111 1.483(9) . ? C12 C13 1.364(9) . ? C21 C22 1.354(8) . ? C22 C23 1.380(8) . ? C23 C231 1.493(7) . ? C31 C32 1.359(8) . ? C32 C33 1.377(8) . ? C33 C331 1.482(8) . ? C111 C116 1.390(10) . ? C111 C112 1.395(10) . ? C112 C113 1.401(11) . ? C112 C117 1.503(11) . ? C113 C114 1.363(13) . ? C114 C115 1.352(13) . ? C114 C118 1.522(12) . ? C115 C116 1.379(11) . ? C116 C119 1.501(11) . ? C231 C236 1.385(8) . ? C231 C232 1.402(8) . ? C232 C233 1.383(8) . ? C232 C237 1.502(8) . ? C233 C234 1.369(9) . ? C234 C235 1.374(10) . ? C234 C238 1.528(9) . ? C235 C236 1.388(9) . ? C236 C239 1.522(9) . ? C331 C336 1.392(9) . ? C331 C332 1.395(8) . ? C332 C333 1.393(11) . ? C332 C337 1.499(11) . ? C333 C334 1.364(11) . ? C334 C335 1.361(11) . ? C334 C338 1.506(11) . ? C335 C336 1.382(9) . ? C336 C339 1.504(9) . ? 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 N1 97.8(2) . . ? N4 U N3 95.5(2) . . ? N1 U N3 82.52(14) . . ? N4 U Cl2 106.8(2) . . ? N1 U Cl2 155.00(12) . . ? N3 U Cl2 90.94(11) . . ? N4 U Cl1 92.37(14) . . ? N1 U Cl1 82.00(11) . . ? N3 U Cl1 163.44(10) . . ? Cl2 U Cl1 100.68(7) . . ? N4 U N2 164.0(2) . . ? N1 U N2 69.98(15) . . ? N3 U N2 73.16(13) . . ? Cl2 U N2 85.02(11) . . ? Cl1 U N2 95.94(10) . . ? N4 U Si2 26.9(2) . . ? N1 U Si2 119.68(13) . . ? N3 U Si2 112.13(10) . . ? Cl2 U Si2 85.15(8) . . ? Cl1 U Si2 80.86(5) . . ? N2 U Si2 168.92(11) . . ? N4 Si1 C1 112.7(3) . . ? N4 Si1 C2 113.2(4) . . ? C1 Si1 C2 104.9(4) . . ? N4 Si1 C3 111.4(4) . . ? C1 Si1 C3 106.7(5) . . ? C2 Si1 C3 107.4(4) . . ? N4 Si2 C6 111.3(4) . . ? N4 Si2 C4 115.3(3) . . ? C6 Si2 C4 106.0(6) . . ? N4 Si2 C5 111.4(5) . . ? C6 Si2 C5 110.7(6) . . ? C4 Si2 C5 101.6(6) . . ? N4 Si2 U 34.1(2) . . ? C6 Si2 U 120.1(4) . . ? C4 Si2 U 81.5(3) . . ? C5 Si2 U 126.1(4) . . ? C13 N1 N11 105.8(5) . . ? C13 N1 U 130.4(4) . . ? N11 N1 U 123.6(3) . . ? C23 N2 N21 105.8(4) . . ? C23 N2 U 135.7(3) . . ? N21 N2 U 118.2(3) . . ? C33 N3 N31 106.3(4) . . ? C33 N3 U 134.5(3) . . ? N31 N3 U 116.7(3) . . ? Si1 N4 Si2 115.9(3) . . ? Si1 N4 U 123.8(3) . . ? Si2 N4 U 119.0(3) . . ? C11 N11 N1 110.2(5) . . ? C11 N11 B 128.5(5) . . ? N1 N11 B 120.5(4) . . ? C21 N21 N2 109.5(4) . . ? C21 N21 B 127.1(5) . . ? N2 N21 B 122.7(4) . . ? C31 N31 N3 109.2(4) . . ? C31 N31 B 126.3(5) . . ? N3 N31 B 123.4(4) . . ? N11 C11 C12 107.2(5) . . ? N11 C11 C111 121.9(5) . . ? C12 C11 C111 130.9(6) . . ? C13 C12 C11 106.1(6) . . ? N1 C13 C12 110.7(6) . . ? N21 C21 C22 109.4(5) . . ? C21 C22 C23 105.4(5) . . ? N2 C23 C22 109.9(5) . . ? N2 C23 C231 122.3(5) . . ? C22 C23 C231 127.2(5) . . ? N31 C31 C32 109.0(5) . . ? C31 C32 C33 106.5(5) . . ? N3 C33 C32 109.0(5) . . ? N3 C33 C331 123.6(5) . . ? C32 C33 C331 127.2(5) . . ? C116 C111 C112 121.0(7) . . ? C116 C111 C11 120.8(7) . . ? C112 C111 C11 118.1(6) . . ? C111 C112 C113 117.1(8) . . ? C111 C112 C117 122.0(7) . . ? C113 C112 C117 120.9(8) . . ? C114 C113 C112 122.5(9) . . ? C115 C114 C113 118.2(9) . . ? C115 C114 C118 121.0(10) . . ? C113 C114 C118 120.7(11) . . ? C114 C115 C116 123.1(9) . . ? C115 C116 C111 117.9(8) . . ? C115 C116 C119 121.7(8) . . ? C111 C116 C119 120.4(7) . . ? C236 C231 C232 120.8(5) . . ? C236 C231 C23 121.4(5) . . ? C232 C231 C23 117.5(5) . . ? C233 C232 C231 118.2(6) . . ? C233 C232 C237 119.7(5) . . ? C231 C232 C237 122.1(5) . . ? C234 C233 C232 122.0(6) . . ? C233 C234 C235 118.7(6) . . ? C233 C234 C238 120.5(7) . . ? C235 C234 C238 120.9(7) . . ? C234 C235 C236 121.8(7) . . ? C231 C236 C235 118.4(6) . . ? C231 C236 C239 121.9(6) . . ? C235 C236 C239 119.6(6) . . ? C336 C331 C332 119.7(6) . . ? C336 C331 C33 119.2(5) . . ? C332 C331 C33 120.6(6) . . ? C333 C332 C331 118.5(7) . . ? C333 C332 C337 120.2(7) . . ? C331 C332 C337 121.2(7) . . ? C334 C333 C332 122.6(7) . . ? C335 C334 C333 117.3(7) . . ? C335 C334 C338 122.7(10) . . ? C333 C334 C338 120.0(9) . . ? C334 C335 C336 123.5(8) . . ? C335 C336 C331 118.3(6) . . ? C335 C336 C339 120.2(7) . . ? C331 C336 C339 121.5(6) . . ? N21 B N31 109.8(5) . . ? N21 B N11 107.8(4) . . ? N31 B N11 112.4(5) . . ? _refine_diff_density_max 1.511 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.090 # = = = END data_umsaldol _audit_creation_method SHELXL _chemical_name_systematic ; Hydrobis(3-mesitylpyrazolyl)(5-mesitylpyrazolyl)borato dichloro (1-mesitylpyrazlyl)(1-methyl) ethoxide uranium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural UCl2[n2-OC(Me)2pzMs][HB(3-Mspz)2(5-Mspz)].C7H8 _chemical_formula_analytical ? _chemical_formula_sum 'C58 H67 B Cl2 N8 O U' _chemical_formula_weight 1211.94 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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)/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 12.776(3) _cell_length_b 28.661(5) _cell_length_c 16.447(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.310(10) _cell_angle_gamma 90.00 _cell_volume 5683.6(22) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.8 _cell_measurement_theta_max 13.8 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method ? _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 2.995 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; Crystal were obtained during an attempted recrystallization of UCl2[n2-OC(Me)2CH2C(=O)Me][HB(3-Mspz)2(5-Mspz)] in toluene ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3.9 _diffrn_reflns_number 10338 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.1153 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.98 _reflns_number_total 9972 _reflns_number_observed 5760 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1638 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+84.7494P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8334 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1723 _refine_ls_R_factor_obs 0.0877 _refine_ls_wR_factor_all 0.3810 _refine_ls_wR_factor_obs 0.1898 _refine_ls_goodness_of_fit_all 1.074 _refine_ls_goodness_of_fit_obs 1.139 _refine_ls_restrained_S_all 1.769 _refine_ls_restrained_S_obs 1.139 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group U1 U 0.07539(5) 0.13597(2) 0.29086(4) 0.0383(2) Uani 1 d . . Cl1 Cl 0.1189(4) 0.1833(2) 0.4318(3) 0.0708(15) Uani 1 d . . Cl2 Cl -0.0095(4) 0.0662(2) 0.3534(4) 0.079(2) Uani 1 d . . O1 O 0.2289(8) 0.1542(4) 0.2818(7) 0.044(3) Uani 1 d . . N1 N 0.0130(10) 0.2056(5) 0.1840(8) 0.038(3) Uani 1 d . . N2 N -0.0171(10) 0.1005(4) 0.1438(8) 0.040(3) Uani 1 d . . N3 N -0.1251(10) 0.1565(6) 0.2714(9) 0.053(4) Uani 1 d . . N4 N 0.2330(10) 0.0780(5) 0.3526(9) 0.051(4) Uani 1 d . . N5 N 0.3353(9) 0.0969(4) 0.3677(8) 0.039(3) Uani 1 d . . N11 N -0.0901(10) 0.2012(5) 0.1167(8) 0.047(4) Uani 1 d . . N21 N -0.1236(10) 0.1152(5) 0.0984(8) 0.038(3) Uani 1 d . . N31 N -0.2041(10) 0.1629(6) 0.1927(7) 0.050(4) Uani 1 d . . C1 C 0.3412(12) 0.1433(6) 0.3263(10) 0.042(4) Uani 1 d . . C1A C 0.4019(13) 0.1373(8) 0.2619(12) 0.072(6) Uani 1 d . . H1A1 H 0.3662(13) 0.1135(8) 0.2211(12) 0.107 Uiso 1 calc R . H1A2 H 0.4774(13) 0.1285(8) 0.2916(12) 0.107 Uiso 1 calc R . H1A3 H 0.4005(13) 0.1662(8) 0.2320(12) 0.107 Uiso 1 calc R . C1B C 0.3896(14) 0.1797(6) 0.3933(12) 0.059(5) Uani 1 d . . H1B1 H 0.4659(14) 0.1725(6) 0.4237(12) 0.088 Uiso 1 calc R . H1B2 H 0.3490(14) 0.1804(6) 0.4332(12) 0.088 Uiso 1 calc R . H1B3 H 0.3848(14) 0.2097(6) 0.3662(12) 0.088 Uiso 1 calc R . C11 C -0.1029(16) 0.2389(6) 0.0672(11) 0.061(5) Uani 1 d . . H11 H -0.1641(16) 0.2448(6) 0.0186(11) 0.073 Uiso 1 calc R . C12 C -0.0134(16) 0.2678(7) 0.0980(13) 0.073(6) Uani 1 d . . H12 H -0.0015(16) 0.2963(7) 0.0757(13) 0.087 Uiso 1 calc R . C13 C 0.0566(14) 0.2447(6) 0.1708(10) 0.045(4) Uani 1 d . . C21 C -0.1716(16) 0.0849(7) 0.0351(12) 0.065(5) Uani 1 d . . H21 H -0.2428(16) 0.0874(7) -0.0045(12) 0.078 Uiso 1 calc R . C22 C -0.0978(14) 0.0494(8) 0.0386(12) 0.063(6) Uani 1 d . . H22 H -0.1090(14) 0.0237(8) 0.0022(12) 0.076 Uiso 1 calc R . C23 C 0.0000(13) 0.0602(6) 0.1097(10) 0.043(4) Uani 1 d . . C31 C -0.3025(13) 0.1709(6) 0.2001(10) 0.047(4) Uani 1 d . . C32 C -0.2890(13) 0.1711(8) 0.2887(11) 0.062(6) Uani 1 d . . H32 H -0.3427(13) 0.1766(8) 0.3143(11) 0.074 Uiso 1 calc R . C33 C -0.1785(13) 0.1612(8) 0.3287(11) 0.059(5) Uani 1 d . . H33 H -0.1450(13) 0.1581(8) 0.3880(11) 0.071 Uiso 1 calc R . C51 C 0.4131(15) 0.0693(7) 0.4188(11) 0.056(5) Uani 1 d . . C52 C 0.3594(14) 0.0302(6) 0.4340(13) 0.061(5) Uani 1 d . . H52 H 0.3922(14) 0.0043(6) 0.4666(13) 0.073 Uiso 1 calc R . C53 C 0.2479(17) 0.0369(7) 0.3916(13) 0.075(6) Uani 1 d . . H53 H 0.1920(17) 0.0159(7) 0.3904(13) 0.090 Uiso 1 calc R . C131 C 0.1603(12) 0.2644(6) 0.2270(9) 0.039(4) Uani 1 d . . C132 C 0.1649(14) 0.2906(6) 0.2991(11) 0.051(5) Uani 1 d . . C133 C 0.2651(16) 0.3119(7) 0.3467(12) 0.061(5) Uani 1 d . . H133 H 0.2682(16) 0.3284(7) 0.3961(12) 0.074 Uiso 1 calc R . C134 C 0.3589(17) 0.3094(8) 0.3238(15) 0.073(7) Uani 1 d . . C135 C 0.3529(15) 0.2861(9) 0.2539(16) 0.083(8) Uani 1 d . . H135 H 0.4160(15) 0.2851(9) 0.2377(16) 0.099 Uiso 1 calc R . C136 C 0.2566(16) 0.2622(7) 0.2007(11) 0.058(5) Uani 1 d . . C137 C 0.0671(15) 0.2974(8) 0.3275(13) 0.074(6) Uani 1 d . . H13A H 0.0875(15) 0.3165(8) 0.3783(13) 0.112 Uiso 1 calc R . H13B H 0.0417(15) 0.2676(8) 0.3402(13) 0.112 Uiso 1 calc R . H13C H 0.0089(15) 0.3123(8) 0.2825(13) 0.112 Uiso 1 calc R . C138 C 0.4675(22) 0.3307(12) 0.3765(20) 0.155(14) Uani 1 d . . H13D H 0.4588(22) 0.3465(12) 0.4253(20) 0.233 Uiso 1 calc R . H13E H 0.4909(22) 0.3526(12) 0.3418(20) 0.233 Uiso 1 calc R . H13F H 0.5222(22) 0.3065(12) 0.3960(20) 0.233 Uiso 1 calc R . C139 C 0.2467(20) 0.2357(9) 0.1177(15) 0.096(8) Uani 1 d . . H13G H 0.1735(20) 0.2228(9) 0.0942(15) 0.144 Uiso 1 calc R . H13H H 0.3004(20) 0.2110(9) 0.1302(15) 0.144 Uiso 1 calc R . H13I H 0.2599(20) 0.2567(9) 0.0767(15) 0.144 Uiso 1 calc R . C231 C 0.1028(14) 0.0340(7) 0.1373(10) 0.049(4) Uani 1 d . . C232 C 0.1871(14) 0.0512(7) 0.1087(11) 0.053(5) Uani 1 d . . C233 C 0.2862(15) 0.0244(9) 0.1278(13) 0.076(7) Uani 1 d . . H233 H 0.3456(15) 0.0358(9) 0.1128(13) 0.091 Uiso 1 calc R . C234 C 0.2952(17) -0.0191(8) 0.1689(13) 0.065(6) Uani 1 d . . C235 C 0.2086(21) -0.0342(7) 0.1955(13) 0.077(7) Uani 1 d . . H235 H 0.2160(21) -0.0621(7) 0.2258(13) 0.092 Uiso 1 calc R . C236 C 0.1127(18) -0.0091(7) 0.1785(13) 0.067(6) Uani 1 d . . C237 C 0.1807(15) 0.0948(7) 0.0606(12) 0.063(5) Uani 1 d . . H23A H 0.2484(15) 0.0992(7) 0.0482(12) 0.095 Uiso 1 calc R . H23B H 0.1701(15) 0.1205(7) 0.0945(12) 0.095 Uiso 1 calc R . H23C H 0.1195(15) 0.0933(7) 0.0076(12) 0.095 Uiso 1 calc R . C238 C 0.3985(18) -0.0481(9) 0.1834(18) 0.127(12) Uani 1 d . . H23D H 0.4486(18) -0.0320(9) 0.1607(18) 0.190 Uiso 1 calc R . H23E H 0.3787(18) -0.0776(9) 0.1546(18) 0.190 Uiso 1 calc R . H23F H 0.4337(18) -0.0533(9) 0.2440(18) 0.190 Uiso 1 calc R . C239 C 0.0184(21) -0.0293(9) 0.2049(14) 0.093(8) Uani 1 d . . H23G H -0.0431(21) -0.0080(9) 0.1889(14) 0.140 Uiso 1 calc R . H23H H 0.0433(21) -0.0340(9) 0.2661(14) 0.140 Uiso 1 calc R . H23I H -0.0045(21) -0.0586(9) 0.1763(14) 0.140 Uiso 1 calc R . C311 C -0.4071(12) 0.1814(8) 0.1272(10) 0.052(5) Uani 1 d . . C312 C -0.4661(13) 0.1449(7) 0.0800(11) 0.049(5) Uani 1 d . . C313 C -0.5627(14) 0.1545(10) 0.0126(12) 0.072(7) Uani 1 d . . H313 H -0.6087(14) 0.1298(10) -0.0139(12) 0.087 Uiso 1 calc R . C314 C -0.5926(14) 0.1983(10) -0.0161(14) 0.074(7) Uani 1 d . . C315 C -0.5301(15) 0.2357(8) 0.0290(13) 0.068(6) Uani 1 d . . H315 H -0.5517(15) 0.2661(8) 0.0117(13) 0.081 Uiso 1 calc R . C316 C -0.4338(14) 0.2276(8) 0.1010(12) 0.059(5) Uani 1 d . . C317 C -0.4342(15) 0.0941(7) 0.1039(13) 0.069(6) Uani 1 d . . H31A H -0.4854(15) 0.0739(7) 0.0633(13) 0.104 Uiso 1 calc R . H31B H -0.4367(15) 0.0880(7) 0.1607(13) 0.104 Uiso 1 calc R . H31C H -0.3606(15) 0.0886(7) 0.1029(13) 0.104 Uiso 1 calc R . C318 C -0.6939(16) 0.2075(11) -0.0917(14) 0.117(11) Uani 1 d . . H31D H -0.7014(16) 0.2405(11) -0.1023(14) 0.176 Uiso 1 calc R . H31E H -0.7580(16) 0.1961(11) -0.0798(14) 0.176 Uiso 1 calc R . H31F H -0.6874(16) 0.1920(11) -0.1415(14) 0.176 Uiso 1 calc R . C319 C -0.3705(17) 0.2677(8) 0.1448(13) 0.074(6) Uani 1 d . . H31G H -0.4038(17) 0.2958(8) 0.1157(13) 0.112 Uiso 1 calc R . H31H H -0.2957(17) 0.2654(8) 0.1444(13) 0.112 Uiso 1 calc R . H31I H -0.3702(17) 0.2685(8) 0.2032(13) 0.112 Uiso 1 calc R . C511 C 0.5334(13) 0.0799(6) 0.4546(11) 0.046(4) Uani 1 d . . C512 C 0.5686(15) 0.1003(7) 0.5359(11) 0.057(5) Uani 1 d . . C513 C 0.6808(19) 0.1108(8) 0.5738(13) 0.076(6) Uani 1 d . . H513 H 0.7045(19) 0.1246(8) 0.6279(13) 0.091 Uiso 1 calc R . C514 C 0.7605(17) 0.1011(9) 0.5327(16) 0.083(7) Uani 1 d . . C515 C 0.7212(14) 0.0808(8) 0.4576(16) 0.075(7) Uani 1 d . . H515 H 0.7716(14) 0.0744(8) 0.4293(16) 0.090 Uiso 1 calc R . C516 C 0.6081(13) 0.0675(7) 0.4141(12) 0.054(5) Uani 1 d . . C517 C 0.4921(19) 0.1061(9) 0.5875(13) 0.087(7) Uani 1 d . . H51A H 0.5313(19) 0.1208(9) 0.6415(13) 0.130 Uiso 1 calc R . H51B H 0.4660(19) 0.0760(9) 0.5980(13) 0.130 Uiso 1 calc R . H51C H 0.4302(19) 0.1251(9) 0.5560(13) 0.130 Uiso 1 calc R . C519 C 0.5750(17) 0.0394(9) 0.3346(15) 0.098(9) Uani 1 d . . H51D H 0.6382(17) 0.0344(9) 0.3164(15) 0.147 Uiso 1 calc R . H51E H 0.5185(17) 0.0556(9) 0.2902(15) 0.147 Uiso 1 calc R . H51F H 0.5467(17) 0.0098(9) 0.3454(15) 0.147 Uiso 1 calc R . C518 C 0.8802(18) 0.1142(13) 0.5731(18) 0.158(16) Uani 1 d . . H51G H 0.8910(18) 0.1286(13) 0.6280(18) 0.237 Uiso 1 calc R . H51H H 0.9008(18) 0.1357(13) 0.5363(18) 0.237 Uiso 1 calc R . H51I H 0.9254(18) 0.0867(13) 0.5810(18) 0.237 Uiso 1 calc R . B1 B -0.1687(14) 0.1630(9) 0.1098(12) 0.054(6) Uani 1 d . . H1 H -0.2349(14) 0.1690(9) 0.0598(12) 0.065 Uiso 1 calc R . C1S C 0.2787(23) 0.0533(9) 0.7773(21) 0.087(7) Uani 1 d . . C2S C 0.3136(24) 0.0952(12) 0.7661(24) 0.117(10) Uani 1 d . . H2S H 0.3614(24) 0.1106(12) 0.8136(24) 0.140 Uiso 1 calc R . C3S C 0.2832(39) 0.1169(12) 0.6887(41) 0.156(18) Uani 1 d . . H3S H 0.3121(39) 0.1459(12) 0.6825(41) 0.187 Uiso 1 calc R . C4S C 0.2049(36) 0.0937(21) 0.6161(26) 0.146(17) Uani 1 d . . H4S H 0.1760(36) 0.1086(21) 0.5631(26) 0.176 Uiso 1 calc R . C5S C 0.1751(28) 0.0497(18) 0.6276(40) 0.176(26) Uani 1 d . . H5S H 0.1319(28) 0.0323(18) 0.5807(40) 0.212 Uiso 1 calc R . C6S C 0.2091(26) 0.0305(13) 0.7098(27) 0.122(12) Uani 1 d . . H6S H 0.1832(26) 0.0011(13) 0.7181(27) 0.146 Uiso 1 calc R . C11S C 0.3149(32) 0.0306(15) 0.8624(23) 0.184(18) Uani 1 d . . H11A H 0.2810(32) 0.0004(15) 0.8580(23) 0.276 Uiso 1 calc R . H11B H 0.2933(32) 0.0494(15) 0.9025(23) 0.276 Uiso 1 calc R . H11C H 0.3942(32) 0.0272(15) 0.8823(23) 0.276 Uiso 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 0.0285(3) 0.0477(4) 0.0331(3) 0.0021(4) 0.0026(2) 0.0013(3) Cl1 0.060(3) 0.096(4) 0.050(3) -0.022(3) 0.009(2) 0.007(3) Cl2 0.054(3) 0.079(4) 0.106(4) 0.028(3) 0.031(3) -0.006(3) O1 0.020(5) 0.065(8) 0.042(6) 0.007(5) 0.004(4) 0.005(5) N1 0.031(7) 0.041(8) 0.036(7) 0.008(6) 0.006(6) 0.001(6) N2 0.040(7) 0.034(8) 0.042(7) 0.010(6) 0.010(6) 0.004(6) N3 0.018(6) 0.089(12) 0.046(8) -0.003(8) 0.004(6) 0.017(7) N4 0.033(7) 0.036(8) 0.070(10) 0.003(7) -0.002(7) 0.005(6) N5 0.023(6) 0.034(8) 0.049(8) 0.004(6) -0.003(6) 0.007(6) N11 0.037(8) 0.074(11) 0.022(7) 0.014(7) -0.002(6) 0.001(7) N21 0.035(7) 0.040(8) 0.032(7) -0.007(6) 0.004(6) -0.005(6) N31 0.027(7) 0.101(12) 0.020(6) 0.000(7) 0.006(5) 0.008(7) C1 0.025(7) 0.041(11) 0.050(9) -0.001(8) 0.000(7) 0.005(7) C1A 0.031(9) 0.113(18) 0.066(12) 0.025(13) 0.010(8) 0.000(11) C1B 0.047(11) 0.036(11) 0.075(13) -0.019(10) -0.004(9) 0.004(8) C11 0.064(12) 0.050(12) 0.047(11) -0.001(9) -0.013(9) -0.013(10) C12 0.066(13) 0.048(12) 0.080(14) 0.025(11) -0.009(11) -0.016(10) C13 0.049(10) 0.052(11) 0.034(9) 0.010(8) 0.015(8) -0.005(8) C21 0.049(11) 0.076(15) 0.065(13) -0.020(11) 0.013(10) 0.000(10) C22 0.033(9) 0.086(16) 0.067(13) -0.028(11) 0.011(9) -0.008(10) C23 0.042(9) 0.050(11) 0.041(9) -0.011(8) 0.020(8) 0.011(8) C31 0.037(9) 0.066(13) 0.037(9) 0.009(9) 0.010(7) -0.011(8) C32 0.032(9) 0.105(17) 0.052(11) -0.014(11) 0.020(8) 0.007(10) C33 0.029(9) 0.107(16) 0.043(10) -0.004(10) 0.014(8) 0.002(9) C51 0.055(11) 0.057(13) 0.048(10) 0.024(9) 0.005(9) 0.012(9) C52 0.038(10) 0.049(12) 0.085(14) 0.030(10) 0.006(9) 0.019(9) C53 0.062(13) 0.049(13) 0.090(16) 0.030(11) -0.007(11) 0.006(10) C131 0.037(9) 0.048(10) 0.028(8) 0.007(7) 0.007(7) 0.006(7) C132 0.040(9) 0.059(12) 0.051(11) 0.015(9) 0.011(8) 0.002(8) C133 0.058(12) 0.056(13) 0.055(12) -0.004(10) -0.001(10) -0.009(10) C134 0.054(13) 0.085(17) 0.063(14) 0.014(12) -0.005(11) -0.025(11) C135 0.028(10) 0.126(22) 0.092(17) 0.046(16) 0.015(11) -0.012(11) C136 0.067(13) 0.067(13) 0.044(10) 0.013(10) 0.025(10) 0.010(10) C137 0.058(12) 0.115(19) 0.062(12) -0.023(13) 0.035(10) -0.002(12) C138 0.082(19) 0.184(34) 0.149(28) -0.037(25) -0.030(18) -0.071(21) C139 0.103(19) 0.114(21) 0.093(18) 0.023(16) 0.062(16) 0.040(16) C231 0.042(10) 0.063(13) 0.039(9) -0.018(9) 0.011(8) 0.000(9) C232 0.036(9) 0.059(13) 0.055(11) -0.017(10) 0.003(8) 0.004(8) C233 0.031(10) 0.113(20) 0.069(14) -0.046(14) -0.003(9) 0.000(11) C234 0.053(12) 0.070(15) 0.052(12) -0.023(11) -0.010(10) 0.006(11) C235 0.101(18) 0.052(13) 0.057(13) 0.011(10) -0.002(12) 0.017(13) C236 0.084(15) 0.055(14) 0.057(12) -0.002(10) 0.016(11) 0.009(11) C237 0.058(12) 0.063(14) 0.067(13) -0.011(11) 0.018(10) -0.005(10) C238 0.064(15) 0.097(20) 0.159(25) -0.048(18) -0.045(16) 0.047(14) C239 0.130(22) 0.100(20) 0.078(16) 0.017(14) 0.074(16) -0.002(16) C311 0.017(8) 0.097(16) 0.038(9) 0.003(10) 0.005(7) -0.008(9) C312 0.035(9) 0.062(14) 0.057(11) -0.008(9) 0.023(8) -0.012(8) C313 0.023(9) 0.136(23) 0.048(11) 0.004(12) -0.002(8) -0.019(11) C314 0.023(9) 0.126(22) 0.068(14) 0.022(15) 0.009(9) 0.008(12) C315 0.041(11) 0.095(17) 0.074(14) 0.039(13) 0.029(10) 0.026(11) C316 0.042(10) 0.074(15) 0.058(12) 0.005(11) 0.015(9) 0.016(10) C317 0.048(11) 0.070(15) 0.078(14) 0.002(12) 0.004(10) -0.025(10) C318 0.040(12) 0.229(35) 0.061(14) -0.003(18) -0.013(10) 0.025(16) C319 0.072(14) 0.082(17) 0.062(13) -0.006(12) 0.013(11) 0.014(12) C511 0.032(9) 0.043(11) 0.051(10) 0.007(8) -0.001(8) 0.005(7) C512 0.052(11) 0.070(14) 0.040(10) 0.005(10) 0.002(9) 0.001(10) C513 0.076(15) 0.078(16) 0.054(12) 0.016(11) -0.003(11) -0.013(12) C514 0.051(13) 0.087(18) 0.084(17) 0.027(14) -0.015(12) -0.008(12) C515 0.028(9) 0.094(18) 0.101(17) 0.026(14) 0.018(11) 0.018(10) C516 0.032(9) 0.061(12) 0.061(12) 0.019(10) 0.003(8) 0.012(8) C517 0.099(18) 0.107(20) 0.049(12) -0.009(13) 0.017(12) -0.005(15) C519 0.054(13) 0.132(23) 0.097(17) -0.032(17) 0.012(12) 0.040(14) C518 0.040(13) 0.279(45) 0.119(22) 0.063(26) -0.023(14) -0.052(19) B1 0.015(8) 0.104(19) 0.038(11) 0.000(11) 0.002(8) 0.011(10) C1S 0.091(18) 0.047(15) 0.131(24) -0.003(15) 0.048(18) -0.004(13) C2S 0.096(21) 0.097(26) 0.159(32) 0.008(23) 0.045(21) 0.007(19) C3S 0.172(41) 0.076(24) 0.279(60) 0.024(33) 0.154(44) 0.023(25) C4S 0.129(34) 0.197(49) 0.123(29) 0.014(33) 0.054(26) 0.089(35) C5S 0.071(21) 0.154(42) 0.253(60) -0.102(44) -0.015(28) 0.042(25) C6S 0.066(19) 0.138(32) 0.170(33) -0.054(30) 0.049(21) 0.000(20) C11S 0.195(41) 0.226(48) 0.160(35) 0.055(34) 0.099(31) 0.083(35) _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 2.082(10) . ? U1 N2 2.528(13) . ? U1 N3 2.542(12) . ? U1 N4 2.547(13) . ? U1 Cl1 2.582(5) . ? U1 N1 2.604(12) . ? U1 Cl2 2.639(5) . ? O1 C1 1.41(2) . ? N1 C13 1.30(2) . ? N1 N11 1.42(2) . ? N2 C23 1.33(2) . ? N2 N21 1.38(2) . ? N3 C33 1.34(2) . ? N3 N31 1.36(2) . ? N4 C53 1.32(2) . ? N4 N5 1.36(2) . ? N5 C51 1.33(2) . ? N5 C1 1.51(2) . ? N11 C11 1.33(2) . ? N11 B1 1.47(3) . ? N21 C21 1.34(2) . ? N21 B1 1.52(3) . ? N31 C31 1.32(2) . ? N31 B1 1.57(2) . ? C1 C1B 1.50(2) . ? C1 C1A 1.51(2) . ? C11 C12 1.37(2) . ? C12 C13 1.40(2) . ? C13 C131 1.46(2) . ? C21 C22 1.38(3) . ? C22 C23 1.43(2) . ? C23 C231 1.45(2) . ? C31 C32 1.41(2) . ? C31 C311 1.50(2) . ? C32 C33 1.38(2) . ? C51 C52 1.38(2) . ? C51 C511 1.48(2) . ? C52 C53 1.38(2) . ? C131 C132 1.39(2) . ? C131 C136 1.43(2) . ? C132 C133 1.40(2) . ? C132 C137 1.48(2) . ? C133 C134 1.37(3) . ? C134 C135 1.31(3) . ? C134 C138 1.50(3) . ? C135 C136 1.43(3) . ? C136 C139 1.53(3) . ? C231 C236 1.39(3) . ? C231 C232 1.40(2) . ? C232 C233 1.42(2) . ? C232 C237 1.47(3) . ? C233 C234 1.40(3) . ? C234 C235 1.39(3) . ? C234 C238 1.51(3) . ? C235 C236 1.37(3) . ? C236 C239 1.52(3) . ? C311 C312 1.37(2) . ? C311 C316 1.40(3) . ? C312 C313 1.39(2) . ? C312 C317 1.53(3) . ? C313 C314 1.35(3) . ? C314 C315 1.39(3) . ? C314 C318 1.49(2) . ? C315 C316 1.42(2) . ? C316 C319 1.45(3) . ? C511 C516 1.38(2) . ? C511 C512 1.39(2) . ? C512 C513 1.39(3) . ? C512 C517 1.50(3) . ? C513 C514 1.42(3) . ? C514 C515 1.30(3) . ? C514 C518 1.50(3) . ? C515 C516 1.44(2) . ? C516 C519 1.47(3) . ? C1S C2S 1.31(4) . ? C1S C6S 1.34(4) . ? C1S C11S 1.47(4) . ? C2S C3S 1.35(5) . ? C3S C4S 1.44(5) . ? C4S C5S 1.35(6) . ? C5S C6S 1.39(6) . ? 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 N2 100.7(4) . . ? O1 U1 N3 150.0(5) . . ? N2 U1 N3 80.8(4) . . ? O1 U1 N4 63.5(4) . . ? N2 U1 N4 100.2(4) . . ? N3 U1 N4 146.2(5) . . ? O1 U1 Cl1 90.2(3) . . ? N2 U1 Cl1 164.5(3) . . ? N3 U1 Cl1 84.3(3) . . ? N4 U1 Cl1 94.4(3) . . ? O1 U1 N1 81.1(4) . . ? N2 U1 N1 73.8(4) . . ? N3 U1 N1 70.5(4) . . ? N4 U1 N1 142.5(4) . . ? Cl1 U1 N1 97.5(3) . . ? O1 U1 Cl2 137.4(3) . . ? N2 U1 Cl2 86.9(3) . . ? N3 U1 Cl2 72.4(4) . . ? N4 U1 Cl2 74.0(3) . . ? Cl1 U1 Cl2 92.4(2) . . ? N1 U1 Cl2 140.3(3) . . ? C1 O1 U1 136.6(10) . . ? C13 N1 N11 106.5(12) . . ? C13 N1 U1 136.1(10) . . ? N11 N1 U1 117.2(9) . . ? C23 N2 N21 107.8(12) . . ? C23 N2 U1 131.4(10) . . ? N21 N2 U1 117.3(9) . . ? C33 N3 N31 105.3(12) . . ? C33 N3 U1 131.3(11) . . ? N31 N3 U1 123.3(9) . . ? C53 N4 N5 106.8(13) . . ? C53 N4 U1 137.8(13) . . ? N5 N4 U1 113.6(9) . . ? C51 N5 N4 110.6(14) . . ? C51 N5 C1 132.2(13) . . ? N4 N5 C1 117.2(11) . . ? C11 N11 N1 107.5(13) . . ? C11 N11 B1 128.1(14) . . ? N1 N11 B1 124.2(13) . . ? C21 N21 N2 109.7(14) . . ? C21 N21 B1 125.8(14) . . ? N2 N21 B1 123.6(12) . . ? C31 N31 N3 111.4(12) . . ? C31 N31 B1 129.3(13) . . ? N3 N31 B1 119.2(12) . . ? O1 C1 C1B 109.1(13) . . ? O1 C1 N5 103.6(11) . . ? C1B C1 N5 110.6(13) . . ? O1 C1 C1A 109.3(13) . . ? C1B C1 C1A 114.3(15) . . ? N5 C1 C1A 109.3(14) . . ? N11 C11 C12 110.2(16) . . ? C11 C12 C13 104.6(16) . . ? N1 C13 C12 111.2(15) . . ? N1 C13 C131 125.2(14) . . ? C12 C13 C131 123.4(16) . . ? N21 C21 C22 108.4(16) . . ? C21 C22 C23 106.0(16) . . ? N2 C23 C22 108.0(14) . . ? N2 C23 C231 125.1(15) . . ? C22 C23 C231 126.8(15) . . ? N31 C31 C32 107.4(14) . . ? N31 C31 C311 125.8(14) . . ? C32 C31 C311 126.6(15) . . ? C33 C32 C31 104.4(15) . . ? N3 C33 C32 111.4(15) . . ? N5 C51 C52 106.5(15) . . ? N5 C51 C511 126.1(16) . . ? C52 C51 C511 127.3(15) . . ? C53 C52 C51 106.7(16) . . ? N4 C53 C52 109.2(18) . . ? C132 C131 C136 118.8(15) . . ? C132 C131 C13 121.7(14) . . ? C136 C131 C13 118.9(15) . . ? C131 C132 C133 119.1(17) . . ? C131 C132 C137 122.5(16) . . ? C133 C132 C137 118.4(18) . . ? C134 C133 C132 123.0(19) . . ? C135 C134 C133 117.7(18) . . ? C135 C134 C138 119.2(25) . . ? C133 C134 C138 123.1(25) . . ? C134 C135 C136 124.8(20) . . ? C135 C136 C131 116.5(18) . . ? C135 C136 C139 125.8(20) . . ? C131 C136 C139 117.7(18) . . ? C236 C231 C232 121.3(17) . . ? C236 C231 C23 122.6(17) . . ? C232 C231 C23 115.5(17) . . ? C231 C232 C233 117.5(20) . . ? C231 C232 C237 124.7(16) . . ? C233 C232 C237 117.7(19) . . ? C234 C233 C232 120.7(21) . . ? C235 C234 C233 118.9(19) . . ? C235 C234 C238 121.6(24) . . ? C233 C234 C238 119.5(23) . . ? C236 C235 C234 121.7(21) . . ? C235 C236 C231 119.8(21) . . ? C235 C236 C239 118.8(21) . . ? C231 C236 C239 121.4(19) . . ? C312 C311 C316 121.0(16) . . ? C312 C311 C31 118.5(18) . . ? C316 C311 C31 119.9(16) . . ? C311 C312 C313 118.6(19) . . ? C311 C312 C317 122.1(16) . . ? C313 C312 C317 119.1(17) . . ? C314 C313 C312 122.5(20) . . ? C313 C314 C315 118.8(18) . . ? C313 C314 C318 121.5(24) . . ? C315 C314 C318 119.6(24) . . ? C314 C315 C316 120.5(20) . . ? C311 C316 C315 117.9(19) . . ? C311 C316 C319 123.8(17) . . ? C315 C316 C319 118.3(20) . . ? C516 C511 C512 121.2(16) . . ? C516 C511 C51 123.2(16) . . ? C512 C511 C51 115.5(16) . . ? C511 C512 C513 118.5(19) . . ? C511 C512 C517 121.8(17) . . ? C513 C512 C517 119.4(18) . . ? C512 C513 C514 122.6(20) . . ? C515 C514 C513 115.1(19) . . ? C515 C514 C518 123.3(27) . . ? C513 C514 C518 121.6(25) . . ? C514 C515 C516 126.8(21) . . ? C511 C516 C515 115.7(18) . . ? C511 C516 C519 121.9(16) . . ? C515 C516 C519 122.3(18) . . ? N11 B1 N21 113.8(13) . . ? N11 B1 N31 108.7(15) . . ? N21 B1 N31 109.5(16) . . ? C2S C1S C6S 119.4(33) . . ? C2S C1S C11S 121.5(34) . . ? C6S C1S C11S 119.1(33) . . ? C1S C2S C3S 123.2(38) . . ? C2S C3S C4S 118.2(38) . . ? C5S C4S C3S 117.7(43) . . ? C4S C5S C6S 119.7(45) . . ? C1S C6S C5S 121.4(40) . . ? _refine_diff_density_max 2.809 _refine_diff_density_min -1.896 _refine_diff_density_rms 0.180 # = = = END data_ualquilo _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural UCl2[o-C6H4CH2NMe2][HB(3-Mspz)2(5-Mspz)].C7H8 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H60 B Cl2 N7 U' _chemical_formula_weight 1102.81 _chemical_melting_point ? _chemical_compound_source ? 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' '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 10.1460(10) _cell_length_b 23.404(2) _cell_length_c 24.374(3) _cell_angle_alpha 115.560(10) _cell_angle_beta 95.120(10) _cell_angle_gamma 95.950(10) _cell_volume 5135.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 10.2 _exptl_crystal_description irregular _exptl_crystal_colour 'golden-yellow' _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method ? _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 3.306 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.5780 _exptl_absorpt_correction_T_max 0.9972 _exptl_special_details ; Crystals were grown from a concentrated toluene 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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7.6 _diffrn_reflns_number 16609 _diffrn_reflns_av_R_equivalents 0.1565 _diffrn_reflns_av_sigmaI/netI 0.3625 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.13 _reflns_number_total 16158 _reflns_number_observed 5512 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4190 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+117.1237P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11968 _refine_ls_number_parameters 1135 _refine_ls_number_restraints 720 _refine_ls_R_factor_all 0.3511 _refine_ls_R_factor_obs 0.1458 _refine_ls_wR_factor_all 0.4350 _refine_ls_wR_factor_obs 0.2486 _refine_ls_goodness_of_fit_all 1.098 _refine_ls_goodness_of_fit_obs 1.341 _refine_ls_restrained_S_all 1.307 _refine_ls_restrained_S_obs 1.252 _refine_ls_shift/esd_max 0.057 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group U1 U 0.56403(14) 0.21442(7) 0.00839(7) 0.0397(5) Uani 1 d . . U2 U 0.15282(14) 0.71863(7) 0.47967(7) 0.0379(5) Uani 1 d . . Cl11 Cl 0.6963(11) 0.3266(5) 0.0774(5) 0.065(3) Uani 1 d . . Cl12 Cl 0.7517(10) 0.1567(6) -0.0474(5) 0.074(3) Uani 1 d . . Cl21 Cl -0.0508(10) 0.7258(6) 0.5387(5) 0.076(4) Uani 1 d . . Cl22 Cl 0.0612(11) 0.7483(5) 0.3948(5) 0.071(3) Uani 1 d . . N1 N 0.4279(32) 0.1322(15) -0.0896(14) 0.057(9) Uani 1 d U . N2 N 0.5095(29) 0.2621(14) -0.0657(13) 0.048(8) Uani 1 d U . N3 N 0.3401(25) 0.2526(12) 0.0250(12) 0.035(7) Uani 1 d U . N4 N 0.2770(24) 0.7475(11) 0.5838(11) 0.026(6) Uani 1 d U . N5 N 0.3884(26) 0.7343(12) 0.4567(12) 0.035(7) Uani 1 d U . N6 N 0.2478(34) 0.8371(15) 0.5380(15) 0.062(10) Uani 1 d U . N10 N 0.7018(28) 0.1964(13) 0.0968(13) 0.042(8) Uani 1 d U . N11 N 0.3022(28) 0.1367(13) -0.1128(13) 0.036(7) Uani 1 d U . C2 C 0.2195(30) 0.6211(15) 0.4748(14) 0.031(8) Uani 1 d U . N21 N 0.3779(26) 0.2472(12) -0.0981(12) 0.034(7) Uani 1 d U . N31 N 0.2342(24) 0.2307(12) -0.0231(12) 0.033(7) Uani 1 d U . N41 N 0.4070(27) 0.7781(12) 0.6045(12) 0.032(7) Uani 1 d U . N51 N 0.4917(25) 0.7672(12) 0.5049(11) 0.031(7) Uani 1 d U . N61 N 0.3765(29) 0.8605(14) 0.5676(13) 0.044(8) Uani 1 d U . C1 C 0.4634(36) 0.1312(16) 0.0313(16) 0.045(10) Uani 1 d U . N20 N -0.0167(27) 0.6132(12) 0.4032(13) 0.035(7) Uani 1 d U . C11 C 0.2349(41) 0.0788(19) -0.1573(18) 0.058(11) Uani 1 d U . C12 C 0.3240(36) 0.0394(18) -0.1645(17) 0.050(10) Uani 1 d U . H12 H 0.3101(36) -0.0030(18) -0.1944(17) 0.060 Uiso 1 calc R . C13 C 0.4347(41) 0.0673(18) -0.1244(18) 0.061(12) Uani 1 d U . H13 H 0.5060(41) 0.0469(18) -0.1200(18) 0.073 Uiso 1 calc R . C21 C 0.3665(40) 0.2802(17) -0.1343(18) 0.058(11) Uani 1 d U . H21 H 0.2905(40) 0.2811(17) -0.1581(18) 0.069 Uiso 1 calc R . C22 C 0.4918(37) 0.3102(17) -0.1260(17) 0.051(10) Uani 1 d U . H22 H 0.5203(37) 0.3360(17) -0.1443(17) 0.061 Uiso 1 calc R . C23 C 0.5649(34) 0.2975(15) -0.0892(15) 0.036(9) Uani 1 d U . C31 C 0.1226(40) 0.2447(17) 0.0016(18) 0.057(11) Uani 1 d U . H31 H 0.0370(40) 0.2331(17) -0.0208(18) 0.068 Uiso 1 calc R . C32 C 0.1485(32) 0.2758(15) 0.0594(15) 0.037(9) Uani 1 d U . H32 H 0.0863(32) 0.2911(15) 0.0859(15) 0.044 Uiso 1 calc R . C33 C 0.2790(32) 0.2830(14) 0.0757(15) 0.034(8) Uani 1 d U . C41 C 0.4572(38) 0.7688(17) 0.6502(17) 0.049(10) Uani 1 d U . C42 C 0.3609(30) 0.7391(14) 0.6667(14) 0.030(8) Uani 1 d U . H42 H 0.3685(30) 0.7276(14) 0.6988(14) 0.036 Uiso 1 calc R . C43 C 0.2464(36) 0.7290(16) 0.6258(16) 0.042(10) Uani 1 d U . H43 H 0.1611(36) 0.7118(16) 0.6277(16) 0.050 Uiso 1 calc R . C51 C 0.5972(41) 0.7561(17) 0.4831(18) 0.058(11) Uani 1 d U . H51 H 0.6792(41) 0.7709(17) 0.5088(18) 0.069 Uiso 1 calc R . C52 C 0.5924(39) 0.7225(17) 0.4219(17) 0.052(11) Uani 1 d U . H52 H 0.6598(39) 0.7127(17) 0.3974(17) 0.063 Uiso 1 calc R . C53 C 0.4540(31) 0.7073(14) 0.4075(14) 0.028(8) Uani 1 d U . C61 C 0.4101(37) 0.9228(16) 0.5921(16) 0.046(10) Uani 1 d U . H61 H 0.4947(37) 0.9456(16) 0.6122(16) 0.055 Uiso 1 calc R . C62 C 0.3035(41) 0.9485(20) 0.5833(18) 0.066(12) Uani 1 d U . H62 H 0.2972(41) 0.9917(20) 0.5972(18) 0.079 Uiso 1 calc R . C63 C 0.2024(38) 0.8952(18) 0.5483(18) 0.055(11) Uani 1 d U . C10 C 0.6753(36) 0.1294(17) 0.0816(18) 0.059(11) Uani 1 d U . H10A H 0.7078(36) 0.1229(17) 0.1168(18) 0.071 Uiso 1 calc R . H10B H 0.7221(36) 0.1054(17) 0.0480(18) 0.071 Uiso 1 calc R . C10A C 0.8538(37) 0.2205(18) 0.1092(17) 0.056(11) Uani 1 d U . H10C H 0.8692(37) 0.2653(18) 0.1192(17) 0.084 Uiso 1 calc R . H10D H 0.8928(37) 0.1968(18) 0.0732(17) 0.084 Uiso 1 calc R . H10E H 0.8942(37) 0.2142(18) 0.1430(17) 0.084 Uiso 1 calc R . C10B C 0.6573(37) 0.2334(17) 0.1576(17) 0.059(12) Uani 1 d U . H10F H 0.6742(37) 0.2784(17) 0.1685(17) 0.088 Uiso 1 calc R . H10G H 0.7061(37) 0.2253(17) 0.1884(17) 0.088 Uiso 1 calc R . H10H H 0.5631(37) 0.2202(17) 0.1547(17) 0.088 Uiso 1 calc R . C101 C 0.5334(34) 0.1066(15) 0.0642(15) 0.035(9) Uani 1 d U . C102 C 0.4874(56) 0.0555(24) 0.0728(23) 0.106(18) Uani 1 d U . H102 H 0.5454(56) 0.0374(24) 0.0900(23) 0.127 Uiso 1 calc R . C103 C 0.3548(53) 0.0308(23) 0.0559(22) 0.094(16) Uani 1 d U . H103 H 0.3239(53) -0.0037(23) 0.0633(22) 0.112 Uiso 1 calc R . C104 C 0.2675(40) 0.0528(17) 0.0296(17) 0.055(11) Uani 1 d U . H104 H 0.1769(40) 0.0357(17) 0.0198(17) 0.066 Uiso 1 calc R . C105 C 0.3213(37) 0.1058(17) 0.0164(16) 0.049(10) Uani 1 d U . H105 H 0.2633(37) 0.1232(17) -0.0017(16) 0.059 Uiso 1 calc R . C111 C 0.1071(42) 0.0724(18) -0.1894(19) 0.060(12) Uani 1 d U . C112 C -0.0069(36) 0.0610(16) -0.1659(16) 0.041(9) Uani 1 d U . C113 C -0.1288(43) 0.0560(17) -0.2004(19) 0.063(12) Uani 1 d U . H113 H -0.2076(43) 0.0485(17) -0.1861(19) 0.075 Uiso 1 calc R . C114 C -0.1378(47) 0.0612(20) -0.2508(22) 0.072(13) Uani 1 d U . C115 C -0.0261(49) 0.0715(19) -0.2763(22) 0.079(14) Uani 1 d U . H115 H -0.0333(49) 0.0720(19) -0.3144(22) 0.095 Uiso 1 calc R . C116 C 0.0968(53) 0.0808(22) -0.2414(24) 0.083(15) Uani 1 d U . C117 C -0.0035(34) 0.0551(17) -0.1074(17) 0.058(11) Uani 1 d U . H11A H -0.0934(34) 0.0473(17) -0.1000(17) 0.087 Uiso 1 calc R . H11B H 0.0434(34) 0.0942(17) -0.0741(17) 0.087 Uiso 1 calc R . H11C H 0.0418(34) 0.0201(17) -0.1105(17) 0.087 Uiso 1 calc R . C118 C -0.2758(45) 0.0510(21) -0.2891(22) 0.098(17) Uani 1 d U . H11D H -0.2632(45) 0.0568(21) -0.3250(22) 0.146 Uiso 1 calc R . H11E H -0.3287(45) 0.0816(21) -0.2647(22) 0.146 Uiso 1 calc R . H11F H -0.3211(45) 0.0083(21) -0.3012(22) 0.146 Uiso 1 calc R . C119 C 0.2171(50) 0.0913(23) -0.2705(23) 0.109(19) Uani 1 d U . H11G H 0.1877(50) 0.0961(23) -0.3065(23) 0.164 Uiso 1 calc R . H11H H 0.2635(50) 0.0550(23) -0.2817(23) 0.164 Uiso 1 calc R . H11I H 0.2764(50) 0.1293(23) -0.2416(23) 0.164 Uiso 1 calc R . C20A C -0.1469(42) 0.6235(20) 0.3862(19) 0.080(14) Uani 1 d U . H20A H -0.1391(42) 0.6529(20) 0.3683(19) 0.120 Uiso 1 calc R . H20B H -0.1903(42) 0.6412(20) 0.4220(19) 0.120 Uiso 1 calc R . H20C H -0.1990(42) 0.5835(20) 0.3568(19) 0.120 Uiso 1 calc R . C20B C 0.0459(41) 0.5830(19) 0.3463(19) 0.077(14) Uani 1 d U . H20D H 0.0486(41) 0.6102(19) 0.3260(19) 0.115 Uiso 1 calc R . H20E H -0.0062(41) 0.5420(19) 0.3192(19) 0.115 Uiso 1 calc R . H20F H 0.1354(41) 0.5775(19) 0.3570(19) 0.115 Uiso 1 calc R . C201 C 0.1193(41) 0.5647(19) 0.4554(18) 0.062(12) Uani 1 d U . C202 C 0.1541(46) 0.5088(21) 0.4578(20) 0.075(14) Uani 1 d U . H202 H 0.0918(46) 0.4713(21) 0.4402(20) 0.090 Uiso 1 calc R . C203 C 0.2784(52) 0.5084(24) 0.4857(22) 0.095(16) Uani 1 d U . H203 H 0.2981(52) 0.4747(24) 0.4939(22) 0.114 Uiso 1 calc R . C204 C 0.3659(43) 0.5591(20) 0.4995(18) 0.065(12) Uani 1 d U . H204 H 0.4543(43) 0.5567(20) 0.5108(18) 0.078 Uiso 1 calc R . C205 C 0.3452(40) 0.6103(19) 0.4992(17) 0.057(11) Uani 1 d U . H205 H 0.4158(40) 0.6445(19) 0.5160(17) 0.068 Uiso 1 calc R . C20 C -0.0170(37) 0.5711(18) 0.4298(18) 0.057(11) Uani 1 d U . H20G H -0.0606(37) 0.5290(18) 0.3991(18) 0.069 Uiso 1 calc R . H20H H -0.0708(37) 0.5851(18) 0.4628(18) 0.069 Uiso 1 calc R . C231 C 0.7176(33) 0.3229(15) -0.0708(15) 0.038(9) Uani 1 d U . C232 C 0.8167(36) 0.2883(16) -0.0999(16) 0.041(9) Uani 1 d U . C233 C 0.9467(43) 0.3134(19) -0.0847(19) 0.064(12) Uani 1 d U . H233 H 1.0073(43) 0.2886(19) -0.1067(19) 0.076 Uiso 1 calc R . C234 C 0.9927(47) 0.3696(22) -0.0416(21) 0.075(14) Uani 1 d U . C235 C 0.9090(38) 0.4093(18) -0.0091(18) 0.057(11) Uani 1 d U . H235 H 0.9444(38) 0.4500(18) 0.0218(18) 0.068 Uiso 1 calc R . C236 C 0.7554(38) 0.3871(17) -0.0232(17) 0.050(10) Uani 1 d U . C237 C 0.7677(39) 0.2244(16) -0.1526(16) 0.058(11) Uani 1 d U . H23A H 0.6721(39) 0.2147(16) -0.1562(16) 0.087 Uiso 1 calc R . H23B H 0.8086(39) 0.1923(16) -0.1458(16) 0.087 Uiso 1 calc R . H23C H 0.7907(39) 0.2249(16) -0.1897(16) 0.087 Uiso 1 calc R . C238 C 1.1398(43) 0.3990(19) -0.0189(21) 0.082(14) Uani 1 d U . H23D H 1.1467(43) 0.4416(19) 0.0137(21) 0.123 Uiso 1 calc R . H23E H 1.1811(43) 0.4008(19) -0.0522(21) 0.123 Uiso 1 calc R . H23F H 1.1844(43) 0.3731(19) -0.0040(21) 0.123 Uiso 1 calc R . C239 C 0.6769(41) 0.4301(17) 0.0108(18) 0.068(13) Uani 1 d U . H23G H 0.7330(41) 0.4694(17) 0.0392(18) 0.103 Uiso 1 calc R . H23H H 0.6272(41) 0.4123(17) 0.0331(18) 0.103 Uiso 1 calc R . H23I H 0.6158(41) 0.4384(17) -0.0163(18) 0.103 Uiso 1 calc R . C331 C 0.3568(36) 0.3154(17) 0.1418(17) 0.046(10) Uani 1 d U . C332 C 0.4277(33) 0.3779(16) 0.1607(16) 0.038(9) Uani 1 d U . C333 C 0.4977(35) 0.4103(17) 0.2195(17) 0.050(10) Uani 1 d U . H333 H 0.5495(35) 0.4498(17) 0.2302(17) 0.060 Uiso 1 calc R . C334 C 0.4959(36) 0.3868(17) 0.2660(17) 0.048(10) Uani 1 d U . C335 C 0.4222(37) 0.3255(18) 0.2421(18) 0.054(11) Uani 1 d U . H335 H 0.4235(37) 0.3058(18) 0.2680(18) 0.064 Uiso 1 calc R . C336 C 0.3466(37) 0.2899(18) 0.1839(18) 0.050(10) Uani 1 d U . C337 C 0.4287(39) 0.4133(16) 0.1210(17) 0.057(11) Uani 1 d U . H33A H 0.3771(39) 0.3863(16) 0.0814(17) 0.086 Uiso 1 calc R . H33B H 0.5192(39) 0.4244(16) 0.1162(17) 0.086 Uiso 1 calc R . H33C H 0.3902(39) 0.4517(16) 0.1404(17) 0.086 Uiso 1 calc R . C338 C 0.5584(35) 0.4247(16) 0.3319(14) 0.049(10) Uani 1 d U . H33D H 0.6041(35) 0.4654(16) 0.3379(14) 0.074 Uiso 1 calc R . H33E H 0.6213(35) 0.4016(16) 0.3422(14) 0.074 Uiso 1 calc R . H33F H 0.4899(35) 0.4313(16) 0.3578(14) 0.074 Uiso 1 calc R . C339 C 0.2710(36) 0.2279(15) 0.1670(16) 0.048(10) Uani 1 d U . H33G H 0.2258(36) 0.2108(15) 0.1256(16) 0.071 Uiso 1 calc R . H33H H 0.2062(36) 0.2318(15) 0.1943(16) 0.071 Uiso 1 calc R . H33I H 0.3305(36) 0.1996(15) 0.1698(16) 0.071 Uiso 1 calc R . C411 C 0.6008(33) 0.7983(15) 0.6849(15) 0.037(9) Uani 1 d U . C412 C 0.6362(34) 0.8619(15) 0.7332(15) 0.034(9) Uani 1 d U . C413 C 0.7658(42) 0.8821(20) 0.7594(19) 0.066(13) Uani 1 d U . H413 H 0.7859(42) 0.9215(20) 0.7942(19) 0.080 Uiso 1 calc R . C414 C 0.8746(42) 0.8483(19) 0.7383(19) 0.061(12) Uani 1 d U . C415 C 0.8327(33) 0.7878(15) 0.6923(14) 0.037(9) Uani 1 d U . H415 H 0.8989(33) 0.7623(15) 0.6795(14) 0.044 Uiso 1 calc R . C416 C 0.6957(33) 0.7581(15) 0.6606(15) 0.037(9) Uani 1 d U . C417 C 0.5210(47) 0.8999(22) 0.7541(21) 0.096(17) Uani 1 d U . H41A H 0.4386(47) 0.8753(22) 0.7282(21) 0.143 Uiso 1 calc R . H41B H 0.5384(47) 0.9396(22) 0.7513(21) 0.143 Uiso 1 calc R . H41C H 0.5139(47) 0.9087(22) 0.7959(21) 0.143 Uiso 1 calc R . C418 C 1.0094(40) 0.8754(19) 0.7692(19) 0.073(14) Uani 1 d U . H41D H 1.0114(40) 0.9187(19) 0.7996(19) 0.110 Uiso 1 calc R . H41E H 1.0666(40) 0.8752(19) 0.7399(19) 0.110 Uiso 1 calc R . H41F H 1.0401(40) 0.8504(19) 0.7889(19) 0.110 Uiso 1 calc R . C419 C 0.6717(36) 0.6950(15) 0.6105(14) 0.049(10) Uani 1 d U . H41G H 0.7550(36) 0.6788(15) 0.6037(14) 0.074 Uiso 1 calc R . H41H H 0.6323(36) 0.6967(15) 0.5740(14) 0.074 Uiso 1 calc R . H41I H 0.6118(36) 0.6673(15) 0.6201(14) 0.074 Uiso 1 calc R . C531 C 0.3794(34) 0.6730(16) 0.3433(16) 0.043(9) Uani 1 d U . C532 C 0.3363(33) 0.7017(16) 0.3054(16) 0.039(9) Uani 1 d U . C533 C 0.2842(34) 0.6669(16) 0.2461(17) 0.048(10) Uani 1 d U . H533 H 0.2520(34) 0.6878(16) 0.2240(17) 0.057 Uiso 1 calc R . C534 C 0.2765(30) 0.6009(14) 0.2166(14) 0.026(8) Uani 1 d U . C535 C 0.3093(34) 0.5709(17) 0.2500(16) 0.044(10) Uani 1 d U . H535 H 0.2953(34) 0.5263(17) 0.2323(16) 0.052 Uiso 1 calc R . C536 C 0.3650(29) 0.6066(14) 0.3117(13) 0.022(7) Uani 1 d U . C537 C 0.3494(39) 0.7752(17) 0.3362(18) 0.068(13) Uani 1 d U . H53A H 0.3887(39) 0.7920(17) 0.3785(18) 0.102 Uiso 1 calc R . H53B H 0.2622(39) 0.7873(17) 0.3340(18) 0.102 Uiso 1 calc R . H53C H 0.4053(39) 0.7924(17) 0.3153(18) 0.102 Uiso 1 calc R . C538 C 0.2117(37) 0.5660(17) 0.1468(16) 0.057(11) Uani 1 d U . H53D H 0.1969(37) 0.5974(17) 0.1324(16) 0.086 Uiso 1 calc R . H53E H 0.1278(37) 0.5402(17) 0.1424(16) 0.086 Uiso 1 calc R . H53F H 0.2711(37) 0.5391(17) 0.1230(16) 0.086 Uiso 1 calc R . C539 C 0.4135(34) 0.5675(15) 0.3444(15) 0.045(10) Uani 1 d U . H53G H 0.3961(34) 0.5227(15) 0.3162(15) 0.067 Uiso 1 calc R . H53H H 0.3666(34) 0.5748(15) 0.3788(15) 0.067 Uiso 1 calc R . H53I H 0.5079(34) 0.5806(15) 0.3587(15) 0.067 Uiso 1 calc R . C631 C 0.0579(33) 0.8990(15) 0.5276(15) 0.036(9) Uani 1 d U . C632 C -0.0373(39) 0.9006(17) 0.5651(18) 0.051(10) Uani 1 d U . C633 C -0.1604(42) 0.9050(18) 0.5466(19) 0.063(12) Uani 1 d U . H633 H -0.2265(42) 0.9033(18) 0.5701(19) 0.075 Uiso 1 calc R . C634 C -0.1962(42) 0.9119(18) 0.4944(20) 0.059(12) Uani 1 d U . C635 C -0.1101(42) 0.9101(18) 0.4595(19) 0.065(12) Uani 1 d U . H635 H -0.1359(42) 0.9115(18) 0.4225(19) 0.078 Uiso 1 calc R . C636 C 0.0246(36) 0.9060(16) 0.4756(16) 0.045(10) Uani 1 d U . C637 C -0.0040(40) 0.8977(17) 0.6268(18) 0.062(12) Uani 1 d U . H63A H 0.0892(40) 0.8946(17) 0.6333(18) 0.093 Uiso 1 calc R . H63B H -0.0576(40) 0.8609(17) 0.6257(18) 0.093 Uiso 1 calc R . H63C H -0.0229(40) 0.9359(17) 0.6597(18) 0.093 Uiso 1 calc R . C638 C -0.3475(51) 0.9129(23) 0.4764(24) 0.117(19) Uani 1 d U . H63D H -0.3959(51) 0.9143(23) 0.5089(24) 0.175 Uiso 1 calc R . H63E H -0.3836(51) 0.8749(23) 0.4393(24) 0.175 Uiso 1 calc R . H63F H -0.3559(51) 0.9501(23) 0.4699(24) 0.175 Uiso 1 calc R . C639 C 0.1342(43) 0.9094(20) 0.4386(19) 0.081(14) Uani 1 d U . H63G H 0.0972(43) 0.9143(20) 0.4035(19) 0.122 Uiso 1 calc R . H63H H 0.1728(43) 0.8707(20) 0.4251(19) 0.122 Uiso 1 calc R . H63I H 0.2023(43) 0.9455(20) 0.4637(19) 0.122 Uiso 1 calc R . B1 B 0.2767(44) 0.2040(20) -0.0901(19) 0.043(11) Uani 1 d U . H1 H 0.1961(44) 0.2012(20) -0.1170(19) 0.052 Uiso 1 calc R . B2 B 0.4662(47) 0.8170(21) 0.5700(21) 0.052(13) Uani 1 d U . H2 H 0.5526(47) 0.8425(21) 0.5937(21) 0.062 Uiso 1 calc R . C1S C 0.8826(49) 0.3997(21) 0.2378(22) 0.084(15) Uani 1 d U . H1S H 0.8014(49) 0.4048(21) 0.2210(22) 0.101 Uiso 1 calc R . C2S C 0.8886(57) 0.3829(23) 0.2842(25) 0.098(17) Uani 1 d U . H2S H 0.8114(57) 0.3841(23) 0.3023(25) 0.118 Uiso 1 calc R . C3S C 0.9833(57) 0.3661(23) 0.3059(24) 0.102(18) Uani 1 d U . H3S H 0.9694(57) 0.3483(23) 0.3329(24) 0.123 Uiso 1 calc R . C4S C 1.1170(62) 0.3737(25) 0.2896(26) 0.121(21) Uani 1 d U . H4S H 1.1941(62) 0.3656(25) 0.3068(26) 0.146 Uiso 1 calc R . C5S C 1.1101(39) 0.3966(16) 0.2411(17) 0.050(11) Uani 1 d U . H5S H 1.1913(39) 0.4025(16) 0.2278(17) 0.060 Uiso 1 calc R . C6S C 1.0078(50) 0.4098(21) 0.2143(22) 0.079(14) Uani 1 d U . C60S C 1.0039(48) 0.4370(21) 0.1756(22) 0.095(16) Uani 1 d U . H60A H 0.9128(48) 0.4399(21) 0.1641(22) 0.143 Uiso 1 calc R . H60B H 1.0404(48) 0.4113(21) 0.1395(22) 0.143 Uiso 1 calc R . H60C H 1.0558(48) 0.4792(21) 0.1956(22) 0.143 Uiso 1 calc R . C7S C 0.3319(50) 0.3530(24) -0.2472(22) 0.087(15) Uani 1 d U . C8S C 0.2451(50) 0.3013(25) -0.2647(22) 0.083(15) Uani 1 d U . C9S C 0.0876(70) 0.2747(33) -0.2484(32) 0.155(26) Uani 1 d U . C10S C 0.1070(48) 0.3484(25) -0.2135(23) 0.089(15) Uani 1 d U . C11S C 0.3092(66) 0.4213(28) -0.2057(28) 0.129(22) Uani 1 d U . C12S C 0.1703(79) 0.4168(35) -0.1868(34) 0.167(28) Uani 1 d U . C13S C 0.2087(95) 0.2324(44) -0.3015(43) 0.236(40) Uani 1 d U . 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 0.0284(10) 0.0568(12) 0.0382(11) 0.0251(9) 0.0033(8) 0.0079(8) U2 0.0315(10) 0.0429(10) 0.0365(10) 0.0150(8) 0.0075(8) 0.0038(8) Cl11 0.058(7) 0.067(8) 0.064(8) 0.028(6) 0.001(6) -0.006(6) Cl12 0.042(6) 0.122(10) 0.070(8) 0.046(8) 0.035(6) 0.030(6) Cl21 0.034(6) 0.110(10) 0.070(8) 0.021(7) 0.032(6) 0.024(6) Cl22 0.072(8) 0.079(8) 0.057(7) 0.027(6) -0.012(6) 0.020(7) N1 0.057(12) 0.058(12) 0.059(12) 0.029(9) 0.016(9) -0.001(9) N2 0.042(11) 0.057(12) 0.043(11) 0.021(8) 0.015(9) 0.008(8) N3 0.033(10) 0.039(10) 0.033(10) 0.017(8) 0.004(8) 0.007(8) N4 0.026(10) 0.024(10) 0.029(10) 0.015(8) -0.002(8) 0.005(8) N5 0.039(10) 0.039(10) 0.026(10) 0.013(8) 0.013(8) 0.003(8) N6 0.061(13) 0.064(12) 0.059(13) 0.026(9) 0.007(9) 0.018(9) N10 0.042(11) 0.039(11) 0.046(11) 0.020(8) 0.006(8) 0.006(8) N11 0.044(11) 0.033(10) 0.038(11) 0.023(8) 0.002(8) -0.001(8) C2 0.023(11) 0.035(11) 0.029(11) 0.011(8) 0.001(8) -0.008(8) N21 0.032(10) 0.033(10) 0.039(10) 0.020(8) 0.003(8) 0.003(8) N31 0.015(9) 0.036(10) 0.037(10) 0.007(8) 0.010(8) -0.003(8) N41 0.037(11) 0.032(10) 0.028(10) 0.016(8) -0.004(8) 0.006(8) N51 0.022(10) 0.037(10) 0.026(10) 0.005(8) 0.011(8) 0.004(8) N61 0.042(11) 0.048(11) 0.035(11) 0.010(8) 0.013(8) 0.011(8) C1 0.049(13) 0.040(12) 0.042(13) 0.017(9) 0.002(9) 0.000(9) N20 0.029(10) 0.035(10) 0.039(11) 0.012(8) 0.004(8) 0.008(8) C11 0.059(14) 0.060(14) 0.055(14) 0.025(10) 0.003(9) 0.015(9) C12 0.050(13) 0.052(13) 0.051(13) 0.027(9) 0.003(9) 0.004(9) C13 0.060(15) 0.058(14) 0.065(15) 0.028(10) 0.005(9) 0.016(9) C21 0.053(14) 0.059(14) 0.061(14) 0.027(10) 0.009(9) 0.003(9) C22 0.050(13) 0.050(13) 0.054(13) 0.025(9) 0.009(9) 0.003(9) C23 0.041(12) 0.033(12) 0.034(12) 0.017(9) 0.000(9) 0.004(9) C31 0.053(14) 0.058(14) 0.058(14) 0.025(9) 0.013(9) 0.008(9) C32 0.028(12) 0.038(12) 0.038(12) 0.012(9) 0.001(9) -0.001(8) C33 0.029(11) 0.030(11) 0.039(12) 0.008(8) 0.012(9) 0.013(8) C41 0.051(13) 0.052(13) 0.044(13) 0.021(9) 0.014(9) 0.004(9) C42 0.032(11) 0.034(11) 0.027(11) 0.017(8) 0.001(8) 0.000(8) C43 0.039(13) 0.045(13) 0.037(13) 0.014(9) 0.005(9) 0.002(9) C51 0.057(14) 0.058(14) 0.054(14) 0.023(10) 0.004(9) 0.007(9) C52 0.055(14) 0.054(14) 0.048(14) 0.022(9) 0.009(9) 0.008(9) C53 0.032(11) 0.027(11) 0.028(11) 0.016(8) 0.010(8) -0.002(8) C61 0.046(13) 0.041(12) 0.050(13) 0.021(9) 0.012(9) 0.005(9) C62 0.065(15) 0.063(15) 0.067(15) 0.028(10) 0.007(9) 0.009(9) C63 0.049(13) 0.053(13) 0.058(14) 0.020(9) 0.000(9) 0.013(9) C10 0.056(14) 0.058(14) 0.062(14) 0.026(10) 0.007(9) 0.009(9) C10A 0.067(19) 0.073(19) 0.048(18) 0.044(15) 0.008(14) 0.016(15) C10B 0.050(18) 0.066(19) 0.059(19) 0.023(14) 0.025(15) 0.010(14) C101 0.041(12) 0.031(11) 0.035(12) 0.017(9) -0.001(9) 0.005(9) C102 0.106(20) 0.106(20) 0.105(20) 0.047(12) 0.016(10) 0.017(10) C103 0.098(19) 0.093(18) 0.094(18) 0.046(11) 0.012(10) 0.015(10) C104 0.052(14) 0.054(13) 0.054(14) 0.022(9) 0.009(9) 0.000(9) C105 0.052(13) 0.056(13) 0.043(13) 0.026(9) 0.005(9) 0.005(9) C111 0.059(14) 0.060(14) 0.060(14) 0.025(10) 0.006(9) 0.008(9) C112 0.038(12) 0.046(12) 0.039(12) 0.021(9) 0.010(9) -0.004(9) C113 0.063(15) 0.059(14) 0.065(15) 0.026(10) 0.014(10) 0.004(9) C114 0.071(16) 0.070(16) 0.073(16) 0.030(10) 0.003(10) 0.014(10) C115 0.085(17) 0.076(16) 0.075(17) 0.033(11) 0.015(10) 0.010(10) C116 0.083(18) 0.082(17) 0.083(18) 0.036(11) 0.015(10) 0.012(10) C117 0.036(16) 0.056(17) 0.062(18) 0.006(14) -0.002(14) 0.026(14) C118 0.083(23) 0.094(22) 0.101(23) 0.033(17) 0.000(17) 0.011(17) C119 0.109(25) 0.113(24) 0.106(25) 0.045(18) 0.014(18) 0.037(18) C20A 0.079(21) 0.084(21) 0.069(20) 0.027(16) -0.002(16) 0.017(16) C20B 0.069(20) 0.071(20) 0.075(20) 0.017(15) 0.032(16) 0.001(15) C201 0.062(15) 0.063(14) 0.063(14) 0.030(10) 0.004(9) 0.013(9) C202 0.076(16) 0.072(16) 0.080(16) 0.037(10) 0.015(10) 0.007(10) C203 0.099(19) 0.093(18) 0.096(19) 0.043(11) 0.015(10) 0.015(10) C204 0.061(15) 0.065(15) 0.070(15) 0.030(10) 0.007(9) 0.015(10) C205 0.059(14) 0.056(14) 0.057(14) 0.026(10) 0.012(9) 0.009(9) C20 0.056(14) 0.054(14) 0.062(14) 0.025(10) 0.014(9) 0.009(9) C231 0.039(12) 0.036(12) 0.039(12) 0.017(9) 0.009(9) 0.001(9) C232 0.042(13) 0.043(12) 0.040(12) 0.021(9) 0.011(9) 0.000(9) C233 0.068(15) 0.063(15) 0.062(15) 0.032(10) 0.005(9) 0.006(9) C234 0.075(16) 0.078(16) 0.071(16) 0.033(10) 0.009(10) 0.011(10) C235 0.056(14) 0.051(13) 0.060(14) 0.021(9) 0.007(9) 0.014(9) C236 0.052(13) 0.049(13) 0.050(13) 0.024(9) 0.009(9) 0.004(9) C237 0.075(19) 0.048(17) 0.053(18) 0.022(14) -0.003(15) 0.030(15) C238 0.083(22) 0.077(20) 0.094(22) 0.049(16) 0.000(16) 0.005(16) C239 0.077(20) 0.059(19) 0.065(19) 0.025(15) 0.021(16) -0.006(15) C331 0.048(13) 0.048(13) 0.042(13) 0.020(9) 0.009(9) 0.014(9) C332 0.037(12) 0.037(12) 0.039(12) 0.018(9) 0.009(9) -0.001(9) C333 0.043(13) 0.046(13) 0.056(13) 0.017(9) 0.010(9) 0.012(9) C334 0.046(13) 0.050(13) 0.049(13) 0.023(9) -0.002(9) 0.018(9) C335 0.056(14) 0.058(14) 0.052(14) 0.028(9) 0.013(9) 0.013(9) C336 0.049(13) 0.052(13) 0.050(13) 0.024(9) 0.005(9) 0.008(9) C337 0.072(19) 0.048(17) 0.067(19) 0.039(15) 0.016(15) 0.005(14) C338 0.054(17) 0.055(17) 0.029(16) 0.007(13) 0.012(14) 0.017(14) C339 0.062(18) 0.045(17) 0.043(17) 0.025(13) 0.006(14) 0.019(14) C411 0.036(12) 0.038(12) 0.033(12) 0.012(9) 0.005(9) 0.002(9) C412 0.035(12) 0.034(12) 0.035(12) 0.016(9) 0.010(9) 0.002(8) C413 0.070(15) 0.070(15) 0.059(15) 0.031(10) 0.008(9) 0.002(9) C414 0.063(15) 0.062(14) 0.061(14) 0.033(10) -0.003(9) 0.010(9) C415 0.036(12) 0.041(12) 0.033(12) 0.016(9) 0.006(9) 0.005(9) C416 0.040(12) 0.037(12) 0.031(12) 0.013(9) 0.006(9) 0.008(9) C417 0.097(24) 0.108(23) 0.078(22) 0.038(17) 0.006(17) 0.021(17) C418 0.066(20) 0.078(20) 0.078(20) 0.036(16) 0.012(16) 0.012(16) C419 0.057(18) 0.055(17) 0.028(16) 0.010(13) 0.003(13) 0.019(14) C531 0.043(13) 0.044(12) 0.040(12) 0.018(9) 0.001(9) 0.008(9) C532 0.035(12) 0.042(12) 0.042(12) 0.018(9) 0.021(9) 0.004(9) C533 0.047(13) 0.050(13) 0.052(13) 0.027(9) 0.005(9) 0.015(9) C534 0.032(11) 0.022(11) 0.024(11) 0.011(8) 0.005(8) 0.003(8) C535 0.044(13) 0.044(12) 0.045(13) 0.022(9) 0.006(9) 0.007(9) C536 0.028(11) 0.032(11) 0.010(10) 0.014(8) 0.003(8) -0.005(8) C537 0.063(19) 0.072(19) 0.062(19) 0.020(15) 0.021(15) 0.016(15) C538 0.064(19) 0.059(18) 0.053(18) 0.030(14) 0.013(15) 0.004(14) C539 0.047(17) 0.035(16) 0.040(17) 0.005(13) 0.006(14) 0.010(13) C631 0.036(12) 0.036(12) 0.035(12) 0.013(9) 0.010(9) 0.011(9) C632 0.052(14) 0.048(13) 0.055(13) 0.027(9) 0.002(9) 0.004(9) C633 0.061(15) 0.066(14) 0.062(14) 0.029(10) 0.011(9) 0.008(9) C634 0.061(14) 0.053(14) 0.067(14) 0.030(10) 0.007(9) 0.013(9) C635 0.066(15) 0.068(15) 0.061(15) 0.031(10) 0.009(10) 0.006(9) C636 0.045(13) 0.046(13) 0.043(13) 0.018(9) 0.010(9) 0.005(9) C637 0.068(19) 0.044(17) 0.069(20) 0.018(14) 0.011(15) 0.019(15) C638 0.108(25) 0.116(25) 0.117(25) 0.041(18) 0.020(18) 0.032(18) C639 0.085(21) 0.087(21) 0.069(20) 0.035(16) 0.011(16) 0.002(16) B1 0.047(14) 0.051(14) 0.037(14) 0.024(10) 0.016(9) 0.003(9) B2 0.050(15) 0.049(15) 0.055(15) 0.022(10) 0.005(9) 0.006(9) C1S 0.080(17) 0.085(17) 0.085(17) 0.034(11) 0.013(10) 0.015(10) C2S 0.096(20) 0.099(19) 0.100(19) 0.044(12) 0.017(10) 0.015(10) C3S 0.104(20) 0.103(20) 0.102(20) 0.047(12) 0.022(10) 0.014(10) C4S 0.119(22) 0.125(22) 0.122(22) 0.055(13) 0.019(10) 0.024(10) C5S 0.048(13) 0.049(13) 0.054(13) 0.024(9) 0.009(9) 0.007(9) C6S 0.077(17) 0.079(16) 0.080(16) 0.035(11) 0.011(10) 0.011(10) C60S 0.096(23) 0.101(23) 0.097(23) 0.055(18) 0.006(17) 0.003(17) C7S 0.090(18) 0.089(17) 0.087(17) 0.044(11) 0.011(10) 0.015(10) C8S 0.086(17) 0.087(17) 0.078(17) 0.041(11) 0.003(10) 0.011(10) C9S 0.154(27) 0.161(27) 0.152(27) 0.072(14) 0.020(11) 0.026(11) C10S 0.086(18) 0.092(18) 0.091(18) 0.043(11) 0.013(10) 0.011(10) C11S 0.133(24) 0.130(24) 0.128(24) 0.061(13) 0.015(10) 0.017(10) C12S 0.167(30) 0.169(30) 0.166(30) 0.074(15) 0.024(11) 0.032(11) C13S 0.236(41) 0.234(41) 0.236(41) 0.104(20) 0.032(12) 0.039(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 C1 2.40(3) . ? U1 N1 2.49(3) . ? U1 N3 2.53(3) . ? U1 N2 2.55(3) . ? U1 Cl11 2.565(11) . ? U1 Cl12 2.590(9) . ? U1 N10 2.67(3) . ? U2 C2 2.41(3) . ? U2 N4 2.50(2) . ? U2 N5 2.53(3) . ? U2 N6 2.54(3) . ? U2 Cl22 2.581(11) . ? U2 Cl21 2.600(10) . ? U2 N20 2.67(3) . ? N1 N11 1.38(4) . ? N1 C13 1.40(4) . ? N2 C23 1.31(4) . ? N2 N21 1.42(3) . ? N3 C33 1.37(4) . ? N3 N31 1.39(3) . ? N4 C43 1.32(4) . ? N4 N41 1.37(3) . ? N5 C53 1.36(4) . ? N5 N51 1.38(3) . ? N6 N61 1.37(4) . ? N6 C63 1.41(4) . ? N10 C10 1.44(4) . ? N10 C10B 1.50(4) . ? N10 C10A 1.54(4) . ? N11 C11 1.37(4) . ? N11 B1 1.49(4) . ? C2 C201 1.45(5) . ? C2 C205 1.45(5) . ? N21 C21 1.41(4) . ? N21 B1 1.45(4) . ? N31 C31 1.33(4) . ? N31 B1 1.59(4) . ? N41 C41 1.30(4) . ? N41 B2 1.59(5) . ? N51 C51 1.24(4) . ? N51 B2 1.58(5) . ? N61 C61 1.31(4) . ? N61 B2 1.45(5) . ? C1 C101 1.36(4) . ? C1 C105 1.45(5) . ? N20 C20 1.39(4) . ? N20 C20A 1.43(4) . ? N20 C20B 1.49(4) . ? C11 C12 1.33(5) . ? C11 C111 1.41(5) . ? C12 C13 1.32(5) . ? C21 C22 1.34(5) . ? C22 C23 1.27(4) . ? C23 C231 1.55(4) . ? C31 C32 1.26(4) . ? C32 C33 1.32(4) . ? C33 C331 1.55(5) . ? C41 C42 1.33(4) . ? C41 C411 1.54(5) . ? C42 C43 1.39(4) . ? C51 C52 1.35(5) . ? C52 C53 1.39(4) . ? C53 C531 1.50(4) . ? C61 C62 1.33(5) . ? C62 C63 1.41(5) . ? C63 C631 1.53(5) . ? C10 C101 1.44(4) . ? C101 C102 1.35(5) . ? C102 C103 1.36(6) . ? C103 C104 1.32(5) . ? C104 C105 1.48(5) . ? C111 C116 1.36(6) . ? C111 C112 1.39(5) . ? C112 C113 1.40(5) . ? C112 C117 1.49(5) . ? C113 C114 1.28(5) . ? C114 C115 1.39(6) . ? C114 C118 1.55(5) . ? C115 C116 1.39(6) . ? C116 C119 1.52(6) . ? C201 C202 1.41(5) . ? C201 C20 1.51(5) . ? C202 C203 1.38(6) . ? C203 C204 1.30(5) . ? C204 C205 1.24(5) . ? C231 C232 1.40(4) . ? C231 C236 1.43(4) . ? C232 C233 1.34(5) . ? C232 C237 1.48(4) . ? C233 C234 1.28(5) . ? C234 C235 1.36(5) . ? C234 C238 1.52(5) . ? C235 C236 1.55(5) . ? C236 C239 1.38(5) . ? C331 C336 1.40(5) . ? C331 C332 1.42(4) . ? C332 C333 1.38(4) . ? C332 C337 1.52(4) . ? C333 C334 1.46(5) . ? C334 C335 1.39(5) . ? C334 C338 1.50(4) . ? C335 C336 1.39(5) . ? C336 C339 1.44(4) . ? C411 C416 1.40(4) . ? C411 C412 1.42(4) . ? C412 C413 1.35(5) . ? C412 C417 1.53(5) . ? C413 C414 1.43(5) . ? C414 C415 1.36(4) . ? C414 C418 1.44(5) . ? C415 C416 1.47(4) . ? C416 C419 1.43(4) . ? C531 C536 1.39(4) . ? C531 C532 1.42(4) . ? C532 C533 1.34(4) . ? C532 C537 1.54(4) . ? C533 C534 1.39(4) . ? C534 C535 1.33(4) . ? C534 C538 1.58(4) . ? C535 C536 1.40(4) . ? C536 C539 1.54(4) . ? C631 C636 1.36(4) . ? C631 C632 1.38(5) . ? C632 C633 1.32(5) . ? C632 C637 1.54(5) . ? C633 C634 1.37(5) . ? C634 C635 1.26(5) . ? C634 C638 1.56(6) . ? C635 C636 1.41(5) . ? C636 C639 1.51(5) . ? C1S C2S 1.35(6) . ? C1S C6S 1.48(6) . ? C2S C3S 1.23(6) . ? C3S C4S 1.46(7) . ? C4S C5S 1.49(6) . ? C5S C6S 1.31(5) . ? C6S C60S 1.35(5) . ? C7S C8S 1.30(6) . ? C7S C11S 1.54(6) . ? C8S C13S 1.45(9) . ? C8S C9S 1.79(8) . ? C9S C10S 1.54(7) . ? C9S C13S 1.90(10) . ? C10S C12S 1.49(7) . ? C11S C12S 1.53(8) . ? 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 C1 U1 N1 74.0(11) . . ? C1 U1 N3 83.2(10) . . ? N1 U1 N3 81.4(9) . . ? C1 U1 N2 137.7(11) . . ? N1 U1 N2 68.9(10) . . ? N3 U1 N2 72.0(9) . . ? C1 U1 Cl11 132.0(9) . . ? N1 U1 Cl11 152.8(8) . . ? N3 U1 Cl11 93.0(6) . . ? N2 U1 Cl11 84.1(7) . . ? C1 U1 Cl12 98.0(9) . . ? N1 U1 Cl12 80.0(8) . . ? N3 U1 Cl12 160.2(6) . . ? N2 U1 Cl12 94.9(7) . . ? Cl11 U1 Cl12 100.5(4) . . ? C1 U1 N10 63.4(10) . . ? N1 U1 N10 128.3(9) . . ? N3 U1 N10 119.0(8) . . ? N2 U1 N10 158.9(9) . . ? Cl11 U1 N10 77.6(6) . . ? Cl12 U1 N10 78.4(7) . . ? C2 U2 N4 74.1(9) . . ? C2 U2 N5 81.4(9) . . ? N4 U2 N5 81.7(8) . . ? C2 U2 N6 135.4(10) . . ? N4 U2 N6 67.4(9) . . ? N5 U2 N6 71.9(9) . . ? C2 U2 Cl22 131.7(8) . . ? N4 U2 Cl22 151.8(6) . . ? N5 U2 Cl22 90.5(7) . . ? N6 U2 Cl22 84.5(8) . . ? C2 U2 Cl21 100.4(8) . . ? N4 U2 Cl21 81.3(6) . . ? N5 U2 Cl21 161.7(6) . . ? N6 U2 Cl21 95.1(8) . . ? Cl22 U2 Cl21 101.3(4) . . ? C2 U2 N20 66.1(9) . . ? N4 U2 N20 129.9(8) . . ? N5 U2 N20 119.2(8) . . ? N6 U2 N20 158.4(10) . . ? Cl22 U2 N20 77.4(7) . . ? Cl21 U2 N20 77.4(6) . . ? N11 N1 C13 101.8(29) . . ? N11 N1 U1 124.9(22) . . ? C13 N1 U1 131.1(26) . . ? C23 N2 N21 98.8(28) . . ? C23 N2 U1 141.8(25) . . ? N21 N2 U1 119.3(20) . . ? C33 N3 N31 102.5(24) . . ? C33 N3 U1 134.7(21) . . ? N31 N3 U1 121.4(18) . . ? C43 N4 N41 104.3(26) . . ? C43 N4 U2 130.0(22) . . ? N41 N4 U2 124.8(19) . . ? C53 N5 N51 103.0(24) . . ? C53 N5 U2 136.2(21) . . ? N51 N5 U2 119.2(17) . . ? N61 N6 C63 99.4(30) . . ? N61 N6 U2 124.1(23) . . ? C63 N6 U2 136.4(26) . . ? C10 N10 C10B 108.2(29) . . ? C10 N10 C10A 110.9(27) . . ? C10B N10 C10A 103.4(27) . . ? C10 N10 U1 108.1(22) . . ? C10B N10 U1 110.8(21) . . ? C10A N10 U1 115.2(20) . . ? C11 N11 N1 112.6(29) . . ? C11 N11 B1 133.8(33) . . ? N1 N11 B1 113.0(29) . . ? C201 C2 C205 109.6(32) . . ? C201 C2 U2 119.6(24) . . ? C205 C2 U2 129.8(24) . . ? C21 N21 N2 110.7(27) . . ? C21 N21 B1 129.4(32) . . ? N2 N21 B1 119.9(30) . . ? C31 N31 N3 107.5(27) . . ? C31 N31 B1 137.1(32) . . ? N3 N31 B1 114.9(25) . . ? C41 N41 N4 110.4(29) . . ? C41 N41 B2 132.8(32) . . ? N4 N41 B2 116.8(27) . . ? C51 N51 N5 106.5(28) . . ? C51 N51 B2 130.8(33) . . ? N5 N51 B2 121.8(27) . . ? C61 N61 N6 115.5(31) . . ? C61 N61 B2 124.2(34) . . ? N6 N61 B2 120.2(32) . . ? C101 C1 C105 113.1(33) . . ? C101 C1 U1 122.8(26) . . ? C105 C1 U1 124.0(26) . . ? C20 N20 C20A 114.0(31) . . ? C20 N20 C20B 105.9(29) . . ? C20A N20 C20B 108.2(31) . . ? C20 N20 U2 106.5(22) . . ? C20A N20 U2 115.3(22) . . ? C20B N20 U2 106.3(21) . . ? C12 C11 N11 103.5(35) . . ? C12 C11 C111 133.4(40) . . ? N11 C11 C111 122.5(36) . . ? C13 C12 C11 112.3(38) . . ? C12 C13 N1 109.4(36) . . ? C22 C21 N21 103.1(35) . . ? C23 C22 C21 108.5(38) . . ? C22 C23 N2 118.7(35) . . ? C22 C23 C231 122.3(34) . . ? N2 C23 C231 119.0(31) . . ? C32 C31 N31 111.1(37) . . ? C31 C32 C33 108.3(35) . . ? C32 C33 N3 110.4(30) . . ? C32 C33 C331 127.1(31) . . ? N3 C33 C331 122.3(28) . . ? N41 C41 C42 109.2(34) . . ? N41 C41 C411 123.2(33) . . ? C42 C41 C411 127.0(34) . . ? C41 C42 C43 105.3(32) . . ? N4 C43 C42 109.8(31) . . ? N51 C51 C52 119.6(39) . . ? C51 C52 C53 96.8(35) . . ? N5 C53 C52 113.8(30) . . ? N5 C53 C531 121.2(29) . . ? C52 C53 C531 124.4(30) . . ? N61 C61 C62 108.9(36) . . ? C61 C62 C63 104.5(36) . . ? N6 C63 C62 111.5(35) . . ? N6 C63 C631 123.2(33) . . ? C62 C63 C631 125.2(34) . . ? N10 C10 C101 109.8(30) . . ? C102 C101 C1 125.7(39) . . ? C102 C101 C10 116.1(38) . . ? C1 C101 C10 117.2(33) . . ? C101 C102 C103 119.0(52) . . ? C104 C103 C102 123.8(53) . . ? C103 C104 C105 116.5(41) . . ? C1 C105 C104 120.9(35) . . ? C116 C111 C112 120.5(43) . . ? C116 C111 C11 119.7(44) . . ? C112 C111 C11 119.7(40) . . ? C111 C112 C113 115.7(36) . . ? C111 C112 C117 123.5(36) . . ? C113 C112 C117 120.7(34) . . ? C114 C113 C112 123.4(43) . . ? C113 C114 C115 122.5(47) . . ? C113 C114 C118 121.0(47) . . ? C115 C114 C118 116.3(45) . . ? C116 C115 C114 115.6(47) . . ? C111 C116 C115 121.8(50) . . ? C111 C116 C119 123.0(48) . . ? C115 C116 C119 114.6(47) . . ? C202 C201 C2 120.4(38) . . ? C202 C201 C20 125.5(39) . . ? C2 C201 C20 113.9(34) . . ? C203 C202 C201 121.7(45) . . ? C204 C203 C202 114.4(49) . . ? C205 C204 C203 127.7(49) . . ? C204 C205 C2 125.0(41) . . ? N20 C20 C201 115.8(33) . . ? C232 C231 C236 119.7(32) . . ? C232 C231 C23 124.1(30) . . ? C236 C231 C23 116.2(29) . . ? C233 C232 C231 122.0(35) . . ? C233 C232 C237 121.7(36) . . ? C231 C232 C237 116.0(32) . . ? C234 C233 C232 123.8(45) . . ? C233 C234 C235 121.2(46) . . ? C233 C234 C238 126.3(45) . . ? C235 C234 C238 112.5(41) . . ? C234 C235 C236 120.4(38) . . ? C239 C236 C231 129.9(36) . . ? C239 C236 C235 117.2(34) . . ? C231 C236 C235 112.8(32) . . ? C336 C331 C332 120.5(34) . . ? C336 C331 C33 123.7(33) . . ? C332 C331 C33 115.3(32) . . ? C333 C332 C331 118.7(34) . . ? C333 C332 C337 116.9(31) . . ? C331 C332 C337 124.4(33) . . ? C332 C333 C334 124.3(35) . . ? C335 C334 C333 111.2(34) . . ? C335 C334 C338 124.0(36) . . ? C333 C334 C338 124.7(34) . . ? C334 C335 C336 128.0(38) . . ? C335 C336 C331 116.6(36) . . ? C335 C336 C339 121.3(36) . . ? C331 C336 C339 122.0(35) . . ? C416 C411 C412 123.0(31) . . ? C416 C411 C41 113.0(29) . . ? C412 C411 C41 123.7(30) . . ? C413 C412 C411 117.9(34) . . ? C413 C412 C417 125.3(36) . . ? C411 C412 C417 116.7(32) . . ? C412 C413 C414 125.6(40) . . ? C415 C414 C413 112.6(38) . . ? C415 C414 C418 126.3(39) . . ? C413 C414 C418 120.7(39) . . ? C414 C415 C416 127.9(34) . . ? C411 C416 C419 127.5(32) . . ? C411 C416 C415 112.5(29) . . ? C419 C416 C415 120.1(30) . . ? C536 C531 C532 112.9(31) . . ? C536 C531 C53 120.1(30) . . ? C532 C531 C53 126.3(31) . . ? C533 C532 C531 122.2(34) . . ? C533 C532 C537 121.0(35) . . ? C531 C532 C537 116.8(32) . . ? C532 C533 C534 122.2(35) . . ? C535 C534 C533 118.4(32) . . ? C535 C534 C538 124.4(29) . . ? C533 C534 C538 116.7(29) . . ? C534 C535 C536 119.6(32) . . ? C531 C536 C535 124.3(31) . . ? C531 C536 C539 120.2(27) . . ? C535 C536 C539 115.5(28) . . ? C636 C631 C632 119.7(34) . . ? C636 C631 C63 121.2(33) . . ? C632 C631 C63 118.9(33) . . ? C633 C632 C631 117.6(38) . . ? C633 C632 C637 120.0(38) . . ? C631 C632 C637 122.4(35) . . ? C632 C633 C634 123.5(43) . . ? C635 C634 C633 119.4(43) . . ? C635 C634 C638 122.4(44) . . ? C633 C634 C638 117.8(42) . . ? C634 C635 C636 121.1(42) . . ? C631 C636 C635 118.4(36) . . ? C631 C636 C639 118.1(35) . . ? C635 C636 C639 123.5(36) . . ? N21 B1 N11 115.0(31) . . ? N21 B1 N31 114.7(30) . . ? N11 B1 N31 112.0(29) . . ? N61 B2 N51 113.9(33) . . ? N61 B2 N41 109.7(32) . . ? N51 B2 N41 108.1(29) . . ? C2S C1S C6S 118.6(50) . . ? C3S C2S C1S 128.5(62) . . ? C2S C3S C4S 120.7(61) . . ? C3S C4S C5S 109.3(50) . . ? C6S C5S C4S 130.2(46) . . ? C5S C6S C60S 130.2(50) . . ? C5S C6S C1S 111.8(46) . . ? C60S C6S C1S 117.5(48) . . ? C8S C7S C11S 125.4(52) . . ? C7S C8S C13S 148.9(64) . . ? C7S C8S C9S 140.4(51) . . ? C13S C8S C9S 70.5(46) . . ? C10S C9S C8S 75.2(39) . . ? C10S C9S C13S 121.2(56) . . ? C8S C9S C13S 46.3(33) . . ? C12S C10S C9S 160.7(56) . . ? C12S C11S C7S 107.8(52) . . ? C10S C12S C11S 109.7(56) . . ? C8S C13S C9S 63.2(45) . . ? _refine_diff_density_max 2.009 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.228 _eof # End of Crystallographic Information File