# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1425 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [U{H2B(3tBu,5Me-pz)2}I2(THF)2].THF _chemical_formula_analytical ? _chemical_formula_sum 'C28 H52 B I2 N4 O3 U' _chemical_formula_weight 995.38 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 10.3860(10) _cell_length_b 13.1150(10) _cell_length_c 26.556(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3617.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 14.6 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method ? _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 6.225 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.7705 _exptl_absorpt_correction_T_max 0.9996 _exptl_special_details ; ? ; _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\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count '100 reflections' _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% none _diffrn_reflns_number 5512 _diffrn_reflns_av_R_equivalents 0.1496 _diffrn_reflns_av_sigmaI/netI 0.1350 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.96 _reflns_number_total 5247 _reflns_number_observed 2961 _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 792 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^)+(0.0237P)^2^+35.9195P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 4455 _refine_ls_number_parameters 330 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1689 _refine_ls_R_factor_obs 0.0724 _refine_ls_wR_factor_all 0.1997 _refine_ls_wR_factor_obs 0.1003 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.656 _refine_ls_restrained_S_obs 1.125 _refine_ls_shift/esd_max 0.002 _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 0.23952(8) 0.69021(6) 0.16331(3) 0.0334(2) Uani 1 d . . I1 I 0.2674(2) 0.67804(12) 0.27952(5) 0.0517(4) Uani 1 d . . I2 I -0.05847(15) 0.72280(14) 0.17180(8) 0.0666(6) Uani 1 d . . O1 O 0.1510(15) 0.5120(11) 0.1625(7) 0.054(4) Uani 1 d . . O2 O 0.4680(12) 0.7677(10) 0.1679(6) 0.041(4) Uani 1 d . . N1 N 0.3732(16) 0.5941(14) 0.0982(6) 0.036(5) Uani 1 d . . N2 N 0.2335(22) 0.8458(11) 0.1089(6) 0.043(5) Uani 1 d . . N11 N 0.3492(17) 0.6330(14) 0.0512(6) 0.036(5) Uani 1 d . . N21 N 0.2567(20) 0.8185(12) 0.0598(5) 0.042(4) Uani 1 d . . C11 C 0.4276(22) 0.5913(17) 0.0172(6) 0.031(6) Uani 1 d . . C12 C 0.5056(24) 0.5246(19) 0.0408(10) 0.057(8) Uani 1 d . . H12 H 0.5697(24) 0.4849(19) 0.0262(10) 0.068 Uiso 1 calc R . C13 C 0.4707(21) 0.5269(17) 0.0924(8) 0.034(6) Uani 1 d . . C21 C 0.2994(24) 0.9008(20) 0.0350(10) 0.055(7) Uani 1 d . . C22 C 0.2893(24) 0.9823(17) 0.0637(11) 0.058(9) Uani 1 d . . H22 H 0.3067(24) 1.0492(17) 0.0543(11) 0.069 Uiso 1 calc R . C23 C 0.2478(34) 0.9491(16) 0.1107(8) 0.051(7) Uani 1 d . . C111 C 0.4268(25) 0.6184(20) -0.0379(8) 0.057(8) Uani 1 d . . H11A H 0.3609(25) 0.6681(20) -0.0441(8) 0.085 Uiso 1 calc R . H11B H 0.4098(25) 0.5583(20) -0.0574(8) 0.085 Uiso 1 calc R . H11C H 0.5090(25) 0.6460(20) -0.0472(8) 0.085 Uiso 1 calc R . C122 C 0.1011(34) 0.4682(21) 0.1182(12) 0.079(10) Uani 1 d . . H12A H 0.1681(34) 0.4619(21) 0.0929(12) 0.097(34) Uiso 1 calc R . H12B H 0.0324(34) 0.5102(21) 0.1046(12) 0.097(34) Uiso 1 calc R . C123 C 0.0505(38) 0.3650(24) 0.1324(11) 0.095(14) Uani 1 d . . H12C H -0.0333(38) 0.3534(24) 0.1173(11) 0.097(34) Uiso 1 calc R . H12D H 0.1089(38) 0.3119(24) 0.1213(11) 0.097(34) Uiso 1 calc R . C124 C 0.0414(38) 0.3659(27) 0.1851(12) 0.125(15) Uani 1 d U . H12E H -0.0479(38) 0.3589(27) 0.1952(12) 0.097(34) Uiso 1 calc R . H12F H 0.0893(38) 0.3090(27) 0.1990(12) 0.097(34) Uiso 1 calc R . C125 C 0.0930(32) 0.4608(22) 0.2041(11) 0.077(10) Uani 1 d U . H12G H 0.1566(32) 0.4477(22) 0.2301(11) 0.097(34) Uiso 1 calc R . H12H H 0.0248(32) 0.5022(22) 0.2184(11) 0.097(34) Uiso 1 calc R . C131 C 0.5173(23) 0.4643(19) 0.1333(9) 0.039(6) Uani 1 d . . C132 C 0.4843(28) 0.5078(19) 0.1865(9) 0.069(9) Uani 1 d . . H13A H 0.5181(28) 0.4632(19) 0.2120(9) 0.103 Uiso 1 calc R . H13B H 0.3925(28) 0.5127(19) 0.1902(9) 0.103 Uiso 1 calc R . H13C H 0.5219(28) 0.5743(19) 0.1902(9) 0.103 Uiso 1 calc R . C133 C 0.4676(27) 0.3565(20) 0.1300(10) 0.071(10) Uani 1 d . . H13D H 0.5009(27) 0.3174(20) 0.1577(10) 0.107 Uiso 1 calc R . H13E H 0.4949(27) 0.3264(20) 0.0988(10) 0.107 Uiso 1 calc R . H13F H 0.3752(27) 0.3570(20) 0.1315(10) 0.107 Uiso 1 calc R . C134 C 0.6642(23) 0.4618(27) 0.1326(11) 0.086(11) Uani 1 d . . H13G H 0.6948(23) 0.4202(27) 0.1598(11) 0.129 Uiso 1 calc R . H13H H 0.6970(23) 0.5298(27) 0.1363(11) 0.129 Uiso 1 calc R . H13I H 0.6932(23) 0.4338(27) 0.1011(11) 0.129 Uiso 1 calc R . C211 C 0.3326(30) 0.8915(20) -0.0208(10) 0.093(12) Uani 1 d . . H21A H 0.3319(30) 0.8209(20) -0.0304(10) 0.140 Uiso 1 calc R . H21B H 0.4166(30) 0.9196(20) -0.0267(10) 0.140 Uiso 1 calc R . H21C H 0.2701(30) 0.9281(20) -0.0404(10) 0.140 Uiso 1 calc R . C222 C 0.5483(25) 0.7955(22) 0.2088(9) 0.067(8) Uani 1 d . . H22A H 0.6055(25) 0.7397(22) 0.2175(9) 0.093(31) Uiso 1 calc R . H22B H 0.4966(25) 0.8122(22) 0.2381(9) 0.093(31) Uiso 1 calc R . C223 C 0.6265(28) 0.8891(22) 0.1918(11) 0.077(10) Uani 1 d . . H22C H 0.5874(28) 0.9519(22) 0.2035(11) 0.093(31) Uiso 1 calc R . H22D H 0.7145(28) 0.8856(22) 0.2040(11) 0.093(31) Uiso 1 calc R . C224 C 0.6213(28) 0.8812(24) 0.1355(12) 0.085(11) Uani 1 d . . H22E H 0.5802(28) 0.9414(24) 0.1217(12) 0.093(31) Uiso 1 calc R . H22F H 0.7080(28) 0.8773(24) 0.1220(12) 0.093(31) Uiso 1 calc R . C225 C 0.5483(24) 0.7896(21) 0.1208(8) 0.060(8) Uani 1 d . . H22G H 0.6054(24) 0.7332(21) 0.1131(8) 0.093(31) Uiso 1 calc R . H22H H 0.4938(24) 0.8030(21) 0.0919(8) 0.093(31) Uiso 1 calc R . C231 C 0.2190(22) 1.0082(15) 0.1596(9) 0.043(6) Uani 1 d . . C232 C 0.3126(25) 1.0996(16) 0.1635(11) 0.081(9) Uani 1 d . . H23A H 0.3074(25) 1.1396(16) 0.1333(11) 0.122 Uiso 1 calc R . H23B H 0.3989(25) 1.0749(16) 0.1677(11) 0.122 Uiso 1 calc R . H23C H 0.2895(25) 1.1410(16) 0.1919(11) 0.122 Uiso 1 calc R . C233 C 0.2220(29) 0.9436(16) 0.2056(6) 0.055(8) Uani 1 d . . H23D H 0.2037(29) 0.9849(16) 0.2346(6) 0.083 Uiso 1 calc R . H23E H 0.3058(29) 0.9135(16) 0.2091(6) 0.083 Uiso 1 calc R . H23F H 0.1585(29) 0.8907(16) 0.2028(6) 0.083 Uiso 1 calc R . C234 C 0.0777(29) 1.0505(22) 0.1513(9) 0.083(10) Uani 1 d . . H23G H 0.0758(29) 1.0923(22) 0.1217(9) 0.124 Uiso 1 calc R . H23H H 0.0525(29) 1.0905(22) 0.1800(9) 0.124 Uiso 1 calc R . H23I H 0.0192(29) 0.9944(22) 0.1474(9) 0.124 Uiso 1 calc R . B1 B 0.2304(25) 0.7038(20) 0.0435(8) 0.042(7) Uani 1 d D . H1A H 0.1558(25) 0.6763(20) 0.0637(8) 0.050 Uiso 1 calc RD . H1B H 0.2049(25) 0.7024(20) 0.0068(8) 0.050 Uiso 1 calc RD . O1S O 0.6154(40) 0.1551(34) 0.0029(17) 0.247(19) Uiso 1 d . . C1S C 0.6466(56) 0.1073(43) 0.0446(22) 0.233(30) Uiso 1 d . . H1S1 H 0.6573(56) 0.0347(43) 0.0391(22) 0.279 Uiso 1 calc R . H1S2 H 0.5832(56) 0.1183(43) 0.0709(22) 0.279 Uiso 1 calc R . C2S C 0.7825(51) 0.1623(37) 0.0578(17) 0.186(20) Uiso 1 d . . H2S1 H 0.7895(51) 0.1734(37) 0.0938(17) 0.224 Uiso 1 calc R . H2S2 H 0.8538(51) 0.1197(37) 0.0472(17) 0.224 Uiso 1 calc R . C3S C 0.7858(54) 0.2588(39) 0.0314(18) 0.200(23) Uiso 1 d . . H3S1 H 0.7622(54) 0.3148(39) 0.0534(18) 0.240 Uiso 1 calc R . H3S2 H 0.8703(54) 0.2718(39) 0.0172(18) 0.240 Uiso 1 calc R . C4S C 0.7004(43) 0.2453(35) -0.0037(17) 0.160(18) Uiso 1 d . . H4S1 H 0.7447(43) 0.2389(35) -0.0357(17) 0.193 Uiso 1 calc R . H4S2 H 0.6468(43) 0.3058(35) -0.0055(17) 0.193 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 0.0365(4) 0.0342(3) 0.0295(3) 0.0007(5) 0.0014(5) -0.0002(5) I1 0.0653(11) 0.0565(9) 0.0333(6) 0.0000(8) 0.0020(9) -0.0051(13) I2 0.0409(10) 0.0793(13) 0.0795(13) -0.0003(13) 0.0034(10) 0.0076(10) O1 0.047(10) 0.053(10) 0.061(11) 0.011(11) 0.004(11) -0.006(9) O2 0.031(7) 0.042(8) 0.048(9) -0.021(9) -0.013(8) 0.002(7) N1 0.028(10) 0.046(12) 0.034(11) -0.012(10) 0.002(8) 0.015(10) N2 0.061(13) 0.017(8) 0.052(10) 0.004(7) 0.018(12) 0.011(12) N11 0.041(11) 0.040(11) 0.027(10) 0.010(9) -0.015(9) -0.004(10) N21 0.050(11) 0.028(8) 0.048(9) -0.005(9) 0.020(12) 0.022(14) C11 0.038(13) 0.047(15) 0.006(10) -0.013(10) -0.003(10) 0.003(13) C12 0.046(16) 0.055(18) 0.070(21) 0.004(16) 0.021(15) 0.007(15) C13 0.029(12) 0.042(15) 0.031(13) 0.011(12) 0.007(11) -0.004(12) C21 0.045(17) 0.048(16) 0.071(19) 0.010(15) 0.002(15) -0.006(14) C22 0.051(19) 0.016(11) 0.106(23) -0.001(13) -0.033(18) 0.003(12) C23 0.075(19) 0.042(14) 0.036(12) 0.003(10) -0.022(19) 0.019(21) C111 0.057(17) 0.078(20) 0.036(14) 0.004(14) -0.001(14) 0.000(18) C122 0.091(26) 0.055(20) 0.091(25) 0.018(19) 0.012(23) -0.008(21) C123 0.152(35) 0.075(25) 0.056(23) -0.035(19) 0.048(23) -0.081(25) C124 0.126(15) 0.125(15) 0.123(15) 0.000(5) 0.002(5) -0.002(5) C125 0.079(10) 0.076(10) 0.078(10) 0.003(5) 0.003(5) -0.002(5) C131 0.041(15) 0.044(16) 0.032(14) -0.001(13) 0.003(12) 0.022(13) C132 0.088(23) 0.066(20) 0.051(18) 0.020(15) -0.004(17) 0.014(19) C133 0.080(22) 0.060(21) 0.074(23) 0.014(19) -0.009(19) -0.005(20) C134 0.029(16) 0.134(30) 0.095(24) 0.036(23) -0.008(16) 0.033(18) C211 0.143(32) 0.054(18) 0.082(23) 0.038(17) 0.003(22) 0.024(21) C222 0.064(18) 0.075(21) 0.064(18) -0.006(19) -0.006(15) 0.000(21) C223 0.068(22) 0.068(21) 0.094(25) -0.049(19) 0.000(19) -0.030(19) C224 0.061(23) 0.070(23) 0.123(30) -0.017(22) 0.041(22) -0.037(20) C225 0.063(18) 0.067(20) 0.049(15) 0.006(16) 0.023(14) 0.040(19) C231 0.046(15) 0.045(12) 0.038(12) -0.020(12) -0.009(14) -0.002(12) C232 0.105(23) 0.034(13) 0.104(22) 0.018(19) -0.002(23) -0.046(15) C233 0.094(23) 0.064(15) 0.008(9) -0.012(10) 0.008(13) -0.034(19) C234 0.100(25) 0.102(25) 0.045(19) -0.015(17) 0.019(19) 0.016(23) B1 0.038(16) 0.071(19) 0.018(10) 0.010(13) 0.001(12) -0.010(20) _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 N2 2.502(15) . ? U1 O1 2.512(15) . ? U1 N1 2.55(2) . ? U1 O2 2.584(12) . ? U1 I1 3.104(2) . ? U1 I2 3.132(2) . ? O1 C122 1.41(3) . ? O1 C125 1.43(3) . ? O2 C222 1.42(2) . ? O2 C225 1.53(2) . ? N1 C13 1.35(2) . ? N1 N11 1.37(2) . ? N2 C23 1.36(2) . ? N2 N21 1.37(2) . ? N11 C11 1.33(2) . ? N11 B1 1.56(3) . ? N21 C21 1.34(3) . ? N21 B1 1.59(3) . ? C11 C12 1.35(3) . ? C11 C111 1.51(3) . ? C12 C13 1.42(3) . ? C13 C131 1.45(3) . ? C21 C22 1.32(3) . ? C21 C211 1.53(3) . ? C22 C23 1.39(3) . ? C23 C231 1.54(3) . ? C122 C123 1.50(3) . ? C123 C124 1.40(4) . ? C124 C125 1.45(4) . ? C131 C133 1.51(3) . ? C131 C134 1.53(3) . ? C131 C132 1.56(3) . ? C222 C223 1.54(3) . ? C223 C224 1.50(3) . ? C224 C225 1.47(3) . ? C231 C233 1.49(3) . ? C231 C232 1.55(3) . ? C231 C234 1.58(3) . ? O1S C1S 1.31(6) . ? O1S C4S 1.49(5) . ? C1S C2S 1.62(7) . ? C2S C3S 1.45(5) . ? C3S C4S 1.30(5) . ? 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 N2 U1 O1 138.2(6) . . ? N2 U1 N1 91.4(6) . . ? O1 U1 N1 74.6(6) . . ? N2 U1 O2 74.3(6) . . ? O1 U1 O2 134.6(5) . . ? N1 U1 O2 74.1(5) . . ? N2 U1 I1 128.2(4) . . ? O1 U1 I1 89.7(4) . . ? N1 U1 I1 126.7(4) . . ? O2 U1 I1 83.6(4) . . ? N2 U1 I2 84.6(5) . . ? O1 U1 I2 76.5(3) . . ? N1 U1 I2 130.8(4) . . ? O2 U1 I2 148.2(3) . . ? I1 U1 I2 91.59(6) . . ? C122 O1 C125 107.5(19) . . ? C122 O1 U1 121.4(15) . . ? C125 O1 U1 125.9(17) . . ? C222 O2 C225 104.9(15) . . ? C222 O2 U1 132.6(14) . . ? C225 O2 U1 122.4(13) . . ? C13 N1 N11 106.0(17) . . ? C13 N1 U1 143.8(15) . . ? N11 N1 U1 109.5(12) . . ? C23 N2 N21 105.9(16) . . ? C23 N2 U1 141.9(14) . . ? N21 N2 U1 109.3(10) . . ? C11 N11 N1 110.6(17) . . ? C11 N11 B1 129.7(17) . . ? N1 N11 B1 119.1(17) . . ? C21 N21 N2 108.3(18) . . ? C21 N21 B1 133.3(18) . . ? N2 N21 B1 118.4(16) . . ? N11 C11 C12 108.6(18) . . ? N11 C11 C111 123.9(21) . . ? C12 C11 C111 127.5(22) . . ? C11 C12 C13 106.3(21) . . ? N1 C13 C12 108.4(20) . . ? N1 C13 C131 122.5(20) . . ? C12 C13 C131 128.9(22) . . ? C22 C21 N21 110.1(23) . . ? C22 C21 C211 130.1(26) . . ? N21 C21 C211 119.2(24) . . ? C21 C22 C23 106.9(22) . . ? N2 C23 C22 108.2(19) . . ? N2 C23 C231 120.6(20) . . ? C22 C23 C231 131.3(21) . . ? O1 C122 C123 106.6(24) . . ? C124 C123 C122 105.6(28) . . ? C125 C124 C123 109.3(32) . . ? C124 C125 O1 106.9(26) . . ? C13 C131 C133 112.0(22) . . ? C13 C131 C134 109.7(23) . . ? C133 C131 C134 108.8(24) . . ? C13 C131 C132 113.4(19) . . ? C133 C131 C132 108.6(22) . . ? C134 C131 C132 103.8(23) . . ? O2 C222 C223 106.9(20) . . ? C224 C223 C222 102.6(23) . . ? C225 C224 C223 109.8(25) . . ? C224 C225 O2 102.5(19) . . ? C233 C231 C23 113.7(16) . . ? C233 C231 C232 112.0(20) . . ? C23 C231 C232 108.8(22) . . ? C233 C231 C234 109.5(21) . . ? C23 C231 C234 103.8(21) . . ? C232 C231 C234 108.7(20) . . ? N11 B1 N21 113.1(19) . . ? C1S O1S C4S 109.4(47) . . ? O1S C1S C2S 100.6(48) . . ? C3S C2S C1S 107.7(49) . . ? C4S C3S C2S 102.3(48) . . ? C3S C4S O1S 115.5(42) . . ? _refine_diff_density_max 0.981 _refine_diff_density_min -1.158 _refine_diff_density_rms 0.222 # = = = END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [U{H2B(3tBu,5Me-pz)2}I2(OPPh3)2].2C7H8 _chemical_formula_analytical ? _chemical_formula_sum 'C66 H74 B I2 N4 O2 P2 U' _chemical_formula_weight 1519.87 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 17.950(3) _cell_length_b 19.866(3) _cell_length_c 18.793(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.894(12) _cell_angle_gamma 90.00 _cell_volume 6653.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.6 _cell_measurement_theta_max 13.5 _exptl_crystal_description 'irregular' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method ? _exptl_crystal_F_000 2988 _exptl_absorpt_coefficient_mu 3.459 _exptl_absorpt_correction_type 'empirical via \y-scan North et al (1968)' _exptl_absorpt_correction_T_min 0.7385 _exptl_absorpt_correction_T_max 0.9989 _exptl_special_details ; ? ; _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\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 1800 _diffrn_standards_decay_% 61.0 _diffrn_reflns_number 9576 _diffrn_reflns_av_R_equivalents 0.1342 _diffrn_reflns_av_sigmaI/netI 0.1867 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.97 _reflns_number_total 9070 _reflns_number_observed 4395 _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 1676 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^)+(0.0749P)^2^+141.6814P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7394 _refine_ls_number_parameters 454 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.2191 _refine_ls_R_factor_obs 0.1004 _refine_ls_wR_factor_all 0.2977 _refine_ls_wR_factor_obs 0.1902 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.143 _refine_ls_restrained_S_all 1.233 _refine_ls_restrained_S_obs 1.140 _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 U1 U 0.31299(5) 0.18987(5) 0.10595(5) 0.0343(3) Uani 1 d . . I1 I 0.31205(11) 0.21114(10) -0.06099(9) 0.0560(6) Uani 1 d . . I2 I 0.19464(11) 0.23995(10) 0.20893(11) 0.0572(6) Uani 1 d . . P1 P 0.3490(4) 0.3784(3) 0.0979(4) 0.043(2) Uani 1 d . . P2 P 0.5269(4) 0.1673(4) 0.1108(4) 0.048(2) Uani 1 d . . O1 O 0.3448(9) 0.3052(8) 0.1166(9) 0.048(5) Uani 1 d . . O2 O 0.4436(7) 0.1839(7) 0.1040(7) 0.029(4) Uani 1 d . . N1 N 0.2094(10) 0.1029(11) 0.0596(10) 0.037(5) Uani 1 d . . N2 N 0.3499(10) 0.1034(10) 0.2066(11) 0.038(5) Uani 1 d . . N11 N 0.2440(13) 0.0400(11) 0.0595(12) 0.056(7) Uani 1 d . . N21 N 0.3367(13) 0.0429(12) 0.1764(12) 0.054(6) Uani 1 d . . C11 C 0.1964(20) -0.0055(16) 0.0316(16) 0.072(11) Uani 1 d . . C131 C 0.0774(17) 0.1479(16) 0.0137(16) 0.068(10) Uani 1 d . . C13 C 0.1386(16) 0.0938(14) 0.0267(14) 0.050(8) Uani 1 d . . C21 C 0.3492(17) -0.0068(13) 0.2260(16) 0.056(8) Uani 1 d . . C22 C 0.3686(16) 0.0263(14) 0.2885(16) 0.054(8) Uani 1 d U . H22 H 0.3814(16) 0.0055(14) 0.3325(16) 0.064 Uiso 1 calc R . C23 C 0.3668(15) 0.0942(15) 0.2783(14) 0.049(8) Uani 1 d . . C1 C 0.2765(15) 0.4009(13) 0.0308(14) 0.044(7) Uiso 1 d . . C100 C 0.2047(19) 0.3910(16) 0.0454(19) 0.082(11) Uiso 1 d . . H100 H 0.1952(19) 0.3749(16) 0.0899(19) 0.098 Uiso 1 calc R . C101 C 0.1434(23) 0.4061(19) -0.0098(21) 0.102(13) Uiso 1 d . . H101 H 0.0947(23) 0.3925(19) -0.0051(21) 0.123 Uiso 1 calc R . C102 C 0.1588(23) 0.4398(19) -0.0673(21) 0.097(12) Uiso 1 d . . H102 H 0.1189(23) 0.4582(19) -0.0971(21) 0.116 Uiso 1 calc R . C103 C 0.2293(29) 0.4493(24) -0.0853(27) 0.144(18) Uiso 1 d . . H103 H 0.2380(29) 0.4648(24) -0.1302(27) 0.173 Uiso 1 calc R . C104 C 0.2897(23) 0.4335(18) -0.0299(20) 0.098(13) Uiso 1 d . . H104 H 0.3385(23) 0.4458(18) -0.0360(20) 0.118 Uiso 1 calc R . C111 C 0.2148(20) -0.0770(18) 0.0185(21) 0.119(16) Uani 1 d . . H11A H 0.2649(20) -0.0865(18) 0.0401(21) 0.178 Uiso 1 calc R . H11B H 0.2114(20) -0.0849(18) -0.0322(21) 0.178 Uiso 1 calc R . H11C H 0.1800(20) -0.1057(18) 0.0390(21) 0.178 Uiso 1 calc R . C12 C 0.1261(18) 0.0269(17) 0.0072(17) 0.083(12) Uani 1 d . . H12 H 0.0827(18) 0.0076(17) -0.0162(17) 0.100 Uiso 1 calc R . C132 C 0.0254(17) 0.1351(19) -0.0532(16) 0.094(13) Uani 1 d . . H13A H 0.0039(17) 0.0910(19) -0.0510(16) 0.140 Uiso 1 calc R . H13B H 0.0527(17) 0.1378(19) -0.0940(16) 0.140 Uiso 1 calc R . H13C H -0.0139(17) 0.1681(19) -0.0575(16) 0.140 Uiso 1 calc R . C133 C 0.1106(15) 0.2172(15) 0.0094(16) 0.069(10) Uani 1 d . . H13D H 0.1442(15) 0.2260(15) 0.0521(16) 0.104 Uiso 1 calc R . H13E H 0.0711(15) 0.2501(15) 0.0048(16) 0.104 Uiso 1 calc R . H13F H 0.1378(15) 0.2197(15) -0.0316(16) 0.104 Uiso 1 calc R . C211 C 0.3406(20) -0.0781(12) 0.2078(17) 0.086(12) Uani 1 d . . H21A H 0.3260(20) -0.0827(12) 0.1571(17) 0.129 Uiso 1 calc R . H21B H 0.3028(20) -0.0975(12) 0.2334(17) 0.129 Uiso 1 calc R . H21C H 0.3874(20) -0.1009(12) 0.2207(17) 0.129 Uiso 1 calc R . C134 C 0.0289(16) 0.1471(17) 0.0803(15) 0.076(10) Uani 1 d . . H13G H 0.0613(16) 0.1553(17) 0.1239(15) 0.114 Uiso 1 calc R . H13H H 0.0053(16) 0.1040(17) 0.0829(15) 0.114 Uiso 1 calc R . H13I H -0.0088(16) 0.1815(17) 0.0738(15) 0.114 Uiso 1 calc R . C2 C 0.4389(14) 0.3956(12) 0.0692(13) 0.040(7) Uiso 1 d . . C200 C 0.4617(15) 0.3614(13) 0.0121(14) 0.048(7) Uiso 1 d . . H200 H 0.4287(15) 0.3313(13) -0.0130(14) 0.058 Uiso 1 calc R . C201 C 0.5320(19) 0.3703(17) -0.0090(19) 0.082(11) Uiso 1 d . . H201 H 0.5465(19) 0.3459(17) -0.0472(19) 0.098 Uiso 1 calc R . C202 C 0.5811(20) 0.4166(17) 0.0280(18) 0.083(11) Uiso 1 d . . H202 H 0.6296(20) 0.4228(17) 0.0165(18) 0.100 Uiso 1 calc R . C203 C 0.5546(17) 0.4519(15) 0.0810(16) 0.062(9) Uiso 1 d . . H203 H 0.5854(17) 0.4854(15) 0.1030(16) 0.074 Uiso 1 calc R . C204 C 0.4858(17) 0.4424(15) 0.1053(16) 0.067(9) Uiso 1 d . . H204 H 0.4719(17) 0.4663(15) 0.1441(16) 0.080 Uiso 1 calc R . C231 C 0.3892(18) 0.1481(17) 0.3299(14) 0.062(9) Uani 1 d . . C232 C 0.3274(18) 0.1562(16) 0.3792(15) 0.077(11) Uani 1 d . . H23A H 0.3412(18) 0.1914(16) 0.4134(15) 0.116 Uiso 1 calc R . H23B H 0.3215(18) 0.1147(16) 0.4041(15) 0.116 Uiso 1 calc R . H23C H 0.2810(18) 0.1677(16) 0.3510(15) 0.116 Uiso 1 calc R . C233 C 0.4014(14) 0.2135(14) 0.2921(16) 0.062(9) Uani 1 d . . H23D H 0.4160(14) 0.2479(14) 0.3269(16) 0.093 Uiso 1 calc R . H23E H 0.3557(14) 0.2266(14) 0.2636(16) 0.093 Uiso 1 calc R . H23F H 0.4402(14) 0.2077(14) 0.2617(16) 0.093 Uiso 1 calc R . C234 C 0.4659(17) 0.1290(16) 0.3763(16) 0.083(11) Uani 1 d . . H23G H 0.4803(17) 0.1645(16) 0.4099(16) 0.124 Uiso 1 calc R . H23H H 0.5042(17) 0.1232(16) 0.3453(16) 0.124 Uiso 1 calc R . H23I H 0.4598(17) 0.0879(16) 0.4018(16) 0.124 Uiso 1 calc R . C3 C 0.3440(15) 0.4318(13) 0.1759(14) 0.045(7) Uiso 1 d . . C300 C 0.3237(17) 0.4967(16) 0.1707(18) 0.069(9) Uiso 1 d . . H300 H 0.3063(17) 0.5148(16) 0.1262(18) 0.082 Uiso 1 calc R . C301 C 0.3284(19) 0.5356(19) 0.2292(19) 0.086(11) Uiso 1 d . . H301 H 0.3160(19) 0.5810(19) 0.2244(19) 0.104 Uiso 1 calc R . C302 C 0.3500(18) 0.5112(17) 0.2929(19) 0.077(10) Uiso 1 d . . H302 H 0.3498(18) 0.5390(17) 0.3326(19) 0.092 Uiso 1 calc R . C303 C 0.3726(19) 0.4468(17) 0.3028(19) 0.085(11) Uiso 1 d . . H303 H 0.3914(19) 0.4305(17) 0.3478(19) 0.102 Uiso 1 calc R . C304 C 0.3663(16) 0.4053(16) 0.2409(16) 0.061(9) Uiso 1 d . . H304 H 0.3775(16) 0.3597(16) 0.2453(16) 0.073 Uiso 1 calc R . C4 C 0.5467(13) 0.0797(12) 0.1241(13) 0.035(6) Uiso 1 d . . C400 C 0.5820(16) 0.0425(15) 0.0765(16) 0.060(8) Uiso 1 d . . H400 H 0.5943(16) 0.0624(15) 0.0347(16) 0.072 Uiso 1 calc R . C401 C 0.6001(19) -0.0267(17) 0.0908(18) 0.082(11) Uiso 1 d . . H401 H 0.6262(19) -0.0524(17) 0.0607(18) 0.098 Uiso 1 calc R . C402 C 0.5761(19) -0.0531(18) 0.1528(18) 0.084(11) Uiso 1 d . . H402 H 0.5841(19) -0.0985(18) 0.1631(18) 0.101 Uiso 1 calc R . C403 C 0.5418(19) -0.0152(17) 0.1982(19) 0.084(11) Uiso 1 d . . H403 H 0.5272(19) -0.0343(17) 0.2395(19) 0.101 Uiso 1 calc R . C404 C 0.5284(16) 0.0510(15) 0.1839(16) 0.064(9) Uiso 1 d . . H404 H 0.5059(16) 0.0770(15) 0.2166(16) 0.076 Uiso 1 calc R . C5 C 0.5706(13) 0.2139(12) 0.1827(12) 0.035(6) Uiso 1 d . . C500 C 0.6222(17) 0.1833(17) 0.2357(16) 0.071(9) Uiso 1 d . . H500 H 0.6341(17) 0.1378(17) 0.2335(16) 0.085 Uiso 1 calc R . C501 C 0.6557(20) 0.2253(17) 0.2930(19) 0.085(11) Uiso 1 d . . H501 H 0.6891(20) 0.2065(17) 0.3293(19) 0.102 Uiso 1 calc R . C502 C 0.6391(20) 0.2940(18) 0.2952(20) 0.091(11) Uiso 1 d . . H502 H 0.6631(20) 0.3210(18) 0.3313(20) 0.110 Uiso 1 calc R . C503 C 0.5862(18) 0.3215(18) 0.2428(17) 0.081(10) Uiso 1 d . . H503 H 0.5746(18) 0.3670(18) 0.2451(17) 0.097 Uiso 1 calc R . C504 C 0.5498(17) 0.2820(15) 0.1864(16) 0.063(9) Uiso 1 d . . H504 H 0.5133(17) 0.3005(15) 0.1528(16) 0.076 Uiso 1 calc R . C6 C 0.5695(15) 0.1916(14) 0.0339(14) 0.053(7) Uiso 1 d . . C600 C 0.6423(18) 0.2158(15) 0.0401(18) 0.074(10) Uiso 1 d . . H600 H 0.6700(18) 0.2206(15) 0.0849(18) 0.089 Uiso 1 calc R . C601 C 0.6728(21) 0.2326(17) -0.0212(20) 0.089(11) Uiso 1 d . . H601 H 0.7213(21) 0.2499(17) -0.0156(20) 0.107 Uiso 1 calc R . C602 C 0.6399(21) 0.2266(17) -0.0861(20) 0.089(11) Uiso 1 d . . H602 H 0.6651(21) 0.2366(17) -0.1253(20) 0.106 Uiso 1 calc R . C603 C 0.5642(21) 0.2043(17) -0.0957(20) 0.092(12) Uiso 1 d . . H603 H 0.5381(21) 0.2008(17) -0.1413(20) 0.111 Uiso 1 calc R . C604 C 0.5287(20) 0.1871(17) -0.0333(18) 0.084(10) Uiso 1 d . . H604 H 0.4789(20) 0.1731(17) -0.0382(18) 0.101 Uiso 1 calc R . B1 B 0.3251(17) 0.0342(16) 0.0925(15) 0.041(8) Uani 1 d DU . H1A H 0.3556(17) 0.0696(16) 0.0705(16) 0.049 Uiso 1 calc RD . H1B H 0.3450(17) -0.0113(16) 0.0801(16) 0.049 Uiso 1 calc RD . C1S C 0.8108(37) 0.0851(32) 0.2535(36) 0.215(29) Uiso 1 d D . C2S C 0.8753(32) 0.1213(36) 0.2854(39) 0.242(33) Uiso 1 d D . C3S C 0.9555(32) 0.1209(28) 0.2886(31) 0.203(27) Uiso 1 d D . C4S C 0.9422(27) 0.0649(24) 0.2398(26) 0.142(18) Uiso 1 d D . C5S C 0.9015(27) 0.0131(26) 0.2000(28) 0.165(21) Uiso 1 d D . C6S C 0.8280(30) 0.0348(27) 0.2121(40) 0.236(33) Uiso 1 d D . C7S C 0.7717(30) -0.0115(37) 0.1849(45) 0.319(46) Uiso 1 d D . C8S C 0.4939(35) 0.1585(33) 0.6309(37) 0.176(23) Uiso 1 d . . C9S C 0.4577(40) 0.1892(31) 0.6848(35) 0.183(23) Uiso 1 d . . C10S C 0.3803(49) 0.1928(37) 0.7062(42) 0.225(31) Uiso 1 d . . C11S C 0.3438(68) 0.1639(59) 0.6412(67) 0.317(56) Uiso 1 d . . C12S C 0.3631(41) 0.1244(34) 0.6002(35) 0.176(25) Uiso 1 d . . C13S C 0.4480(63) 0.1124(46) 0.5888(47) 0.292(42) Uiso 1 d . . C14S C 0.2780(40) 0.1578(33) 0.6705(35) 0.197(27) Uiso 1 d . . 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 0.0325(5) 0.0332(5) 0.0346(6) -0.0009(6) -0.0060(4) -0.0041(5) I1 0.0516(12) 0.0740(14) 0.0385(11) 0.0052(10) -0.0107(9) -0.0050(10) I2 0.0491(12) 0.0641(14) 0.0579(13) -0.0025(11) 0.0047(10) 0.0087(10) P1 0.035(4) 0.038(4) 0.053(5) -0.003(4) -0.005(4) -0.011(3) P2 0.033(4) 0.061(5) 0.049(5) 0.001(4) 0.004(4) 0.004(4) O1 0.045(10) 0.038(11) 0.058(11) 0.011(10) -0.007(9) -0.036(9) O2 0.029(8) 0.030(9) 0.022(8) 0.011(8) -0.024(7) -0.011(8) N1 0.018(11) 0.057(15) 0.037(13) -0.006(11) 0.004(9) -0.005(10) N2 0.029(12) 0.031(13) 0.053(15) -0.004(11) 0.004(11) 0.001(10) N11 0.056(16) 0.038(14) 0.066(17) -0.014(13) -0.019(13) 0.002(12) N21 0.056(16) 0.050(16) 0.057(17) 0.003(14) 0.017(13) 0.010(13) C11 0.106(29) 0.051(21) 0.055(21) -0.031(17) -0.013(20) -0.031(20) C131 0.065(22) 0.082(24) 0.048(20) 0.004(18) -0.029(17) -0.044(19) C13 0.055(19) 0.047(18) 0.046(18) 0.029(15) -0.009(15) -0.030(15) C21 0.072(22) 0.030(17) 0.062(21) 0.013(16) -0.005(17) -0.008(15) C22 0.053(9) 0.053(9) 0.054(9) 0.005(5) 0.006(5) 0.001(5) C23 0.043(17) 0.076(22) 0.029(17) 0.001(16) 0.010(14) -0.002(16) C111 0.082(28) 0.116(34) 0.152(40) -0.065(30) -0.013(27) -0.045(26) C12 0.069(24) 0.091(28) 0.077(25) 0.003(21) -0.043(20) -0.046(20) C132 0.064(23) 0.149(35) 0.063(23) 0.013(23) -0.012(18) -0.054(24) C133 0.034(17) 0.090(24) 0.080(23) 0.032(19) -0.007(16) 0.003(17) C211 0.137(34) 0.022(17) 0.096(28) 0.023(17) 0.000(24) -0.020(19) C134 0.051(19) 0.120(29) 0.052(21) 0.029(20) -0.013(17) -0.019(20) C231 0.075(23) 0.094(26) 0.019(16) -0.001(17) 0.005(15) 0.042(20) C232 0.104(29) 0.091(25) 0.047(20) -0.009(18) 0.051(20) -0.029(22) C233 0.028(15) 0.075(22) 0.077(22) -0.005(19) -0.021(15) 0.012(15) C234 0.077(24) 0.093(26) 0.067(23) -0.010(20) -0.039(19) 0.022(20) B1 0.041(9) 0.041(9) 0.042(9) -0.001(5) 0.008(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O2 2.351(14) . ? U1 O1 2.36(2) . ? U1 N2 2.58(2) . ? U1 N1 2.61(2) . ? U1 B1 3.11(3) . ? U1 I1 3.164(2) . ? U1 I2 3.199(2) . ? P1 O1 1.50(2) . ? P1 C1 1.76(3) . ? P1 C2 1.79(3) . ? P1 C3 1.82(3) . ? P2 O2 1.523(15) . ? P2 C5 1.75(2) . ? P2 C6 1.78(3) . ? P2 C4 1.79(2) . ? N1 C13 1.36(3) . ? N1 N11 1.40(3) . ? N2 N21 1.34(3) . ? N2 C23 1.36(3) . ? N11 C11 1.31(3) . ? N11 B1 1.52(3) . ? N21 C21 1.36(3) . ? N21 B1 1.57(3) . ? C11 C12 1.44(4) . ? C11 C111 1.48(4) . ? C131 C132 1.50(3) . ? C131 C133 1.51(4) . ? C131 C13 1.54(4) . ? C131 C134 1.61(4) . ? C13 C12 1.39(4) . ? C21 C22 1.35(4) . ? C21 C211 1.46(3) . ? C22 C23 1.36(4) . ? C23 C231 1.47(4) . ? C1 C104 1.36(4) . ? C1 C100 1.36(4) . ? C100 C101 1.45(4) . ? C101 C102 1.33(4) . ? C102 C103 1.36(5) . ? C103 C104 1.44(5) . ? C2 C200 1.37(3) . ? C2 C204 1.38(4) . ? C200 C201 1.38(4) . ? C201 C202 1.40(4) . ? C202 C203 1.35(4) . ? C203 C204 1.38(4) . ? C231 C233 1.51(4) . ? C231 C232 1.54(4) . ? C231 C234 1.58(3) . ? C3 C300 1.34(4) . ? C3 C304 1.35(3) . ? C300 C301 1.34(4) . ? C301 C302 1.31(4) . ? C302 C303 1.35(4) . ? C303 C304 1.42(4) . ? C4 C404 1.34(3) . ? C4 C400 1.37(3) . ? C400 C401 1.43(4) . ? C401 C402 1.39(4) . ? C402 C403 1.34(4) . ? C403 C404 1.36(4) . ? C5 C504 1.41(3) . ? C5 C500 1.41(3) . ? C500 C501 1.44(4) . ? C501 C502 1.40(4) . ? C502 C503 1.39(4) . ? C503 C504 1.41(4) . ? C6 C600 1.38(4) . ? C6 C604 1.39(4) . ? C600 C601 1.38(4) . ? C601 C602 1.30(4) . ? C602 C603 1.42(4) . ? C603 C604 1.44(4) . ? C1S C6S 1.33(6) . ? C1S C2S 1.43(2) . ? C2S C3S 1.43(2) . ? C2S C4S 1.92(8) . ? C3S C4S 1.44(2) . ? C4S C5S 1.42(2) . ? C5S C6S 1.43(2) . ? C6S C7S 1.42(2) . ? C8S C9S 1.41(7) . ? C8S C13S 1.41(9) . ? C9S C10S 1.49(9) . ? C10S C11S 1.44(12) . ? C10S C14S 2.00(11) . ? C11S C12S 1.18(12) . ? C11S C14S 1.37(11) . ? C12S C13S 1.58(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 O2 U1 O1 79.6(5) . . ? O2 U1 N2 79.0(5) . . ? O1 U1 N2 123.0(6) . . ? O2 U1 N1 129.3(6) . . ? O1 U1 N1 145.6(6) . . ? N2 U1 N1 85.1(6) . . ? O2 U1 B1 82.5(7) . . ? O1 U1 B1 162.1(7) . . ? N2 U1 B1 52.0(7) . . ? N1 U1 B1 50.9(7) . . ? O2 U1 I1 83.0(3) . . ? O1 U1 I1 85.8(4) . . ? N2 U1 I1 141.8(5) . . ? N1 U1 I1 80.7(4) . . ? B1 U1 I1 92.5(5) . . ? O2 U1 I2 139.5(3) . . ? O1 U1 I2 79.5(4) . . ? N2 U1 I2 83.9(5) . . ? N1 U1 I2 84.8(4) . . ? B1 U1 I2 114.6(6) . . ? I1 U1 I2 129.31(6) . . ? O1 P1 C1 111.1(11) . . ? O1 P1 C2 109.1(11) . . ? C1 P1 C2 110.5(13) . . ? O1 P1 C3 111.6(12) . . ? C1 P1 C3 109.1(13) . . ? C2 P1 C3 105.4(12) . . ? O2 P2 C5 107.2(10) . . ? O2 P2 C6 112.6(11) . . ? C5 P2 C6 106.7(13) . . ? O2 P2 C4 113.5(10) . . ? C5 P2 C4 110.2(11) . . ? C6 P2 C4 106.3(13) . . ? P1 O1 U1 159.8(10) . . ? P2 O2 U1 168.7(9) . . ? C13 N1 N11 105.7(20) . . ? C13 N1 U1 146.3(18) . . ? N11 N1 U1 107.1(13) . . ? N21 N2 C23 107.9(21) . . ? N21 N2 U1 105.6(15) . . ? C23 N2 U1 145.5(18) . . ? C11 N11 N1 110.5(24) . . ? C11 N11 B1 131.3(27) . . ? N1 N11 B1 118.1(20) . . ? N2 N21 C21 110.8(22) . . ? N2 N21 B1 121.2(22) . . ? C21 N21 B1 126.8(24) . . ? N11 C11 C12 108.9(27) . . ? N11 C11 C111 125.4(33) . . ? C12 C11 C111 125.3(27) . . ? C132 C131 C133 108.8(26) . . ? C132 C131 C13 112.1(28) . . ? C133 C131 C13 111.7(23) . . ? C132 C131 C134 108.1(24) . . ? C133 C131 C134 107.8(27) . . ? C13 C131 C134 108.2(24) . . ? N1 C13 C12 111.2(27) . . ? N1 C13 C131 126.2(24) . . ? C12 C13 C131 122.6(25) . . ? C22 C21 N21 104.2(24) . . ? C22 C21 C211 133.2(28) . . ? N21 C21 C211 122.6(27) . . ? C21 C22 C23 111.2(27) . . ? N2 C23 C22 105.7(25) . . ? N2 C23 C231 124.6(26) . . ? C22 C23 C231 129.0(27) . . ? C104 C1 C100 120.2(31) . . ? C104 C1 P1 122.4(26) . . ? C100 C1 P1 117.0(24) . . ? C1 C100 C101 118.7(34) . . ? C102 C101 C100 118.2(40) . . ? C101 C102 C103 124.2(46) . . ? C102 C103 C104 115.5(47) . . ? C1 C104 C103 121.2(40) . . ? C13 C12 C11 103.6(24) . . ? C200 C2 C204 119.8(27) . . ? C200 C2 P1 120.3(20) . . ? C204 C2 P1 119.9(22) . . ? C2 C200 C201 122.0(28) . . ? C200 C201 C202 119.0(34) . . ? C203 C202 C201 116.8(35) . . ? C202 C203 C204 125.6(33) . . ? C2 C204 C203 116.6(30) . . ? C23 C231 C233 111.1(22) . . ? C23 C231 C232 108.3(28) . . ? C233 C231 C232 110.4(25) . . ? C23 C231 C234 109.9(24) . . ? C233 C231 C234 107.4(27) . . ? C232 C231 C234 109.6(23) . . ? C300 C3 C304 119.4(29) . . ? C300 C3 P1 122.7(24) . . ? C304 C3 P1 117.8(22) . . ? C301 C300 C3 120.5(34) . . ? C302 C301 C300 121.2(38) . . ? C301 C302 C303 122.1(38) . . ? C302 C303 C304 116.4(34) . . ? C3 C304 C303 120.2(30) . . ? C404 C4 C400 119.9(26) . . ? C404 C4 P2 118.0(21) . . ? C400 C4 P2 122.1(21) . . ? C4 C400 C401 120.5(30) . . ? C402 C401 C400 115.6(34) . . ? C403 C402 C401 122.2(36) . . ? C402 C403 C404 120.1(37) . . ? C4 C404 C403 121.6(32) . . ? C504 C5 C500 122.3(25) . . ? C504 C5 P2 116.8(20) . . ? C500 C5 P2 120.8(20) . . ? C5 C500 C501 117.2(30) . . ? C502 C501 C500 121.2(35) . . ? C503 C502 C501 119.4(36) . . ? C502 C503 C504 121.7(34) . . ? C5 C504 C503 118.0(28) . . ? C600 C6 C604 119.3(30) . . ? C600 C6 P2 121.2(23) . . ? C604 C6 P2 119.5(24) . . ? C601 C600 C6 118.7(33) . . ? C602 C601 C600 125.8(39) . . ? C601 C602 C603 118.0(39) . . ? C602 C603 C604 118.8(35) . . ? C6 C604 C603 119.4(33) . . ? N11 B1 N21 114.0(22) . . ? N11 B1 U1 83.4(15) . . ? N21 B1 U1 79.2(14) . . ? C6S C1S C2S 113.1(70) . . ? C1S C2S C3S 140.4(70) . . ? C1S C2S C4S 92.1(53) . . ? C3S C2S C4S 48.3(24) . . ? C2S C3S C4S 83.7(45) . . ? C5S C4S C3S 158.1(52) . . ? C5S C4S C2S 110.4(42) . . ? C3S C4S C2S 48.0(23) . . ? C4S C5S C6S 97.1(43) . . ? C1S C6S C7S 119.7(43) . . ? C1S C6S C5S 127.2(47) . . ? C7S C6S C5S 112.2(22) . . ? C9S C8S C13S 113.3(71) . . ? C8S C9S C10S 137.7(68) . . ? C11S C10S C9S 95.5(76) . . ? C11S C10S C14S 43.1(57) . . ? C9S C10S C14S 137.6(64) . . ? C12S C11S C14S 122.6(100) . . ? C12S C11S C10S 133.0(100) . . ? C14S C11S C10S 91.2(99) . . ? C11S C12S C13S 123.4(98) . . ? C8S C13S C12S 109.6(74) . . ? C11S C14S C10S 45.8(62) . . ? _refine_diff_density_max 1.958 _refine_diff_density_min -2.139 _refine_diff_density_rms 0.217 # = = = END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [U{Ph2B(pz)2}3].1.5C7H8 _chemical_formula_analytical ? _chemical_formula_sum 'C64.50 H60 B3 N12 U' _chemical_formula_weight 1273.71 _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' '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 13.5650(10) _cell_length_b 15.715(2) _cell_length_c 15.929(2) _cell_angle_alpha 118.957(9) _cell_angle_beta 92.650(11) _cell_angle_gamma 97.356(15) _cell_volume 2923.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 13.9 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'pink-red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method ? _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 2.828 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.8372 _exptl_absorpt_correction_T_max 0.9998 _exptl_special_details ; ? ; _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\qscan' _diffrn_standards_number 3 _diffrn_standards_interval_count 'every 100 reflections' _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 4.4 _diffrn_reflns_number 9397 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 24.98 _reflns_number_total 8202 _reflns_number_observed 6559 _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 545 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^)+(0.0728P)^2^+2.4718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7657 _refine_ls_number_parameters 677 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_obs 0.0501 _refine_ls_wR_factor_all 0.1401 _refine_ls_wR_factor_obs 0.1161 _refine_ls_goodness_of_fit_all 1.087 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.178 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max -0.114 _refine_ls_shift/esd_mean 0.002 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 0.24373(2) 0.15658(2) 0.33499(2) 0.03785(13) Uani 1 d . . N1 N 0.1361(5) 0.0001(5) 0.3071(5) 0.042(2) Uani 1 d . . N2 N 0.3621(5) 0.0395(5) 0.3209(5) 0.046(2) Uani 1 d . . N3 N 0.3403(5) 0.3006(5) 0.4830(5) 0.042(2) Uani 1 d . . N4 N 0.1144(5) 0.2426(5) 0.4457(5) 0.041(2) Uani 1 d . . N5 N 0.1383(5) 0.1567(5) 0.2024(5) 0.042(2) Uani 1 d . . N6 N 0.3641(5) 0.1996(5) 0.2368(5) 0.046(2) Uani 1 d . . N11 N 0.1563(5) -0.0581(5) 0.3447(5) 0.043(2) Uani 1 d . . N21 N 0.3457(5) -0.0324(5) 0.3443(5) 0.041(2) Uani 1 d . . N31 N 0.3185(5) 0.3918(5) 0.5387(5) 0.046(2) Uani 1 d . . N41 N 0.1272(5) 0.3392(5) 0.5156(5) 0.042(2) Uani 1 d . . N51 N 0.1587(5) 0.1302(5) 0.1109(5) 0.042(2) Uani 1 d . . N61 N 0.3507(5) 0.1706(5) 0.1410(5) 0.048(2) Uani 1 d . . C11 C 0.0738(7) -0.1245(7) 0.3273(8) 0.062(3) Uani 1 d . . H11 H 0.0681(7) -0.1721(7) 0.3463(8) 0.063(7) Uiso 1 calc R . C12 C -0.0004(7) -0.1100(8) 0.2770(8) 0.064(3) Uani 1 d . . H12 H -0.0655(7) -0.1449(8) 0.2558(8) 0.063(7) Uiso 1 calc R . C13 C 0.0405(6) -0.0344(7) 0.2642(7) 0.049(2) Uani 1 d . . H13 H 0.0073(6) -0.0097(7) 0.2306(7) 0.063(7) Uiso 1 calc R . C14 C 0.2719(7) 0.0673(6) 0.5024(7) 0.047(2) Uani 1 d . . C15 C 0.1920(7) 0.1129(7) 0.5417(7) 0.051(2) Uani 1 d . . H15 H 0.1277(7) 0.0823(7) 0.5099(7) 0.065(5) Uiso 1 calc R . C16 C 0.2044(10) 0.2032(8) 0.6276(8) 0.072(3) Uani 1 d . . H16 H 0.1489(10) 0.2320(8) 0.6517(8) 0.065(5) Uiso 1 calc R . C17 C 0.2972(11) 0.2490(8) 0.6760(8) 0.071(3) Uani 1 d . . H17 H 0.3053(11) 0.3090(8) 0.7333(8) 0.065(5) Uiso 1 calc R . C18 C 0.3795(9) 0.2067(8) 0.6403(8) 0.070(3) Uani 1 d . . H18 H 0.4433(9) 0.2376(8) 0.6734(8) 0.065(5) Uiso 1 calc R . C19 C 0.3664(8) 0.1178(7) 0.5547(7) 0.059(3) Uani 1 d . . H19 H 0.4226(8) 0.0903(7) 0.5309(7) 0.065(5) Uiso 1 calc R . C21 C 0.4221(7) -0.0820(7) 0.3213(8) 0.058(3) Uani 1 d . . H21 H 0.4289(7) -0.1346(7) 0.3315(8) 0.063(7) Uiso 1 calc R . C22 C 0.4884(8) -0.0450(8) 0.2812(8) 0.067(3) Uani 1 d . . H22 H 0.5472(8) -0.0667(8) 0.2579(8) 0.063(7) Uiso 1 calc R . C23 C 0.4488(7) 0.0318(7) 0.2828(7) 0.057(3) Uani 1 d . . H23 H 0.4779(7) 0.0728(7) 0.2605(7) 0.063(7) Uiso 1 calc R . C24 C 0.2681(7) -0.1315(7) 0.4217(7) 0.049(2) Uani 1 d . . C25 C 0.2977(7) -0.1189(7) 0.5126(7) 0.055(2) Uani 1 d . . H25 H 0.3087(7) -0.0556(7) 0.5659(7) 0.065(5) Uiso 1 calc R . C26 C 0.3110(8) -0.1970(9) 0.5256(9) 0.069(3) Uani 1 d . . H26 H 0.3324(8) -0.1864(9) 0.5868(9) 0.065(5) Uiso 1 calc R . C27 C 0.2926(8) -0.2900(9) 0.4485(10) 0.072(3) Uani 1 d . . H27 H 0.3005(8) -0.3429(9) 0.4577(10) 0.065(5) Uiso 1 calc R . C28 C 0.2631(9) -0.3070(8) 0.3588(9) 0.073(3) Uani 1 d . . H28 H 0.2502(9) -0.3711(8) 0.3068(9) 0.065(5) Uiso 1 calc R . C29 C 0.2521(7) -0.2282(7) 0.3451(8) 0.060(3) Uani 1 d . . H29 H 0.2334(7) -0.2400(7) 0.2830(8) 0.065(5) Uiso 1 calc R . C31 C 0.4003(7) 0.4518(7) 0.5961(8) 0.060(3) Uani 1 d . . H31 H 0.4042(7) 0.5185(7) 0.6404(8) 0.063(7) Uiso 1 calc R . C32 C 0.4775(7) 0.4012(7) 0.5803(8) 0.067(3) Uani 1 d . . H32 H 0.5432(7) 0.4253(7) 0.6102(8) 0.063(7) Uiso 1 calc R . C33 C 0.4376(7) 0.3067(7) 0.5107(7) 0.055(3) Uani 1 d . . H33 H 0.4726(7) 0.2542(7) 0.4859(7) 0.063(7) Uiso 1 calc R . C34 C 0.2029(7) 0.4173(6) 0.4201(6) 0.045(2) Uani 1 d . . C35 C 0.2825(7) 0.4159(6) 0.3684(7) 0.049(2) Uani 1 d . . H35 H 0.3465(7) 0.4180(6) 0.3937(7) 0.065(5) Uiso 1 calc R . C36 C 0.2683(9) 0.4115(7) 0.2792(8) 0.068(3) Uani 1 d . . H36 H 0.3224(9) 0.4088(7) 0.2447(8) 0.065(5) Uiso 1 calc R . C37 C 0.1740(11) 0.4110(7) 0.2412(8) 0.076(3) Uani 1 d . . H37 H 0.1652(11) 0.4085(7) 0.1818(8) 0.065(5) Uiso 1 calc R . C38 C 0.0947(9) 0.4143(7) 0.2906(8) 0.068(3) Uani 1 d . . H38 H 0.0313(9) 0.4143(7) 0.2657(8) 0.065(5) Uiso 1 calc R . C39 C 0.1097(7) 0.4175(7) 0.3784(7) 0.055(2) Uani 1 d . . H39 H 0.0548(7) 0.4201(7) 0.4119(7) 0.065(5) Uiso 1 calc R . C41 C 0.0445(7) 0.3538(7) 0.5604(7) 0.057(3) Uani 1 d . . H41 H 0.0341(7) 0.4140(7) 0.6104(7) 0.063(7) Uiso 1 calc R . C42 C -0.0219(7) 0.2679(7) 0.5222(7) 0.054(2) Uani 1 d . . H42 H -0.0847(7) 0.2573(7) 0.5399(7) 0.063(7) Uiso 1 calc R . C43 C 0.0252(6) 0.1999(7) 0.4511(7) 0.049(2) Uani 1 d . . H43 H -0.0016(6) 0.1333(7) 0.4121(7) 0.063(7) Uiso 1 calc R . C44 C 0.2068(7) 0.5242(6) 0.6161(7) 0.049(2) Uani 1 d . . C45 C 0.1915(7) 0.6079(7) 0.6117(8) 0.057(3) Uani 1 d . . H45 H 0.1819(7) 0.6045(7) 0.5519(8) 0.065(5) Uiso 1 calc R . C46 C 0.1905(9) 0.6973(7) 0.6963(10) 0.077(3) Uani 1 d . . H46 H 0.1801(9) 0.7524(7) 0.6919(10) 0.065(5) Uiso 1 calc R . C47 C 0.2041(8) 0.7043(8) 0.7832(10) 0.079(4) Uani 1 d . . H47 H 0.2048(8) 0.7645(8) 0.8388(10) 0.065(5) Uiso 1 calc R . C48 C 0.2171(8) 0.6226(8) 0.7904(8) 0.069(3) Uani 1 d . . H48 H 0.2249(8) 0.6267(8) 0.8507(8) 0.065(5) Uiso 1 calc R . C49 C 0.2183(8) 0.5342(7) 0.7072(8) 0.065(3) Uani 1 d . . H49 H 0.2273(8) 0.4794(7) 0.7128(8) 0.065(5) Uiso 1 calc R . C51 C 0.0758(8) 0.1272(8) 0.0605(7) 0.061(3) Uani 1 d . . H51 H 0.0691(8) 0.1090(8) -0.0047(7) 0.063(7) Uiso 1 calc R . C52 C 0.0035(8) 0.1542(8) 0.1180(8) 0.068(3) Uani 1 d . . H52 H -0.0611(8) 0.1596(8) 0.1013(8) 0.063(7) Uiso 1 calc R . C53 C 0.0438(7) 0.1720(7) 0.2060(7) 0.053(2) Uani 1 d . . H53 H 0.0105(7) 0.1919(7) 0.2605(7) 0.063(7) Uiso 1 calc R . C54 C 0.2621(6) -0.0112(6) 0.0686(6) 0.044(2) Uani 1 d . . C55 C 0.1829(8) -0.0654(7) 0.0818(7) 0.056(2) Uani 1 d . . H55 H 0.1229(8) -0.0413(7) 0.0937(7) 0.065(5) Uiso 1 calc R . C56 C 0.1885(9) -0.1534(8) 0.0781(8) 0.071(3) Uani 1 d . . H56 H 0.1325(9) -0.1881(8) 0.0863(8) 0.065(5) Uiso 1 calc R . C57 C 0.2750(11) -0.1904(9) 0.0626(8) 0.082(4) Uani 1 d . . H57 H 0.2793(11) -0.2492(9) 0.0622(8) 0.065(5) Uiso 1 calc R . C58 C 0.3542(10) -0.1409(9) 0.0479(9) 0.083(4) Uani 1 d . . H58 H 0.4131(10) -0.1670(9) 0.0348(9) 0.065(5) Uiso 1 calc R . C59 C 0.3493(8) -0.0516(8) 0.0521(8) 0.068(3) Uani 1 d . . H59 H 0.4059(8) -0.0176(8) 0.0437(8) 0.065(5) Uiso 1 calc R . C61 C 0.4347(8) 0.2044(8) 0.1188(8) 0.072(3) Uani 1 d . . H61 H 0.4452(8) 0.1925(8) 0.0570(8) 0.063(7) Uiso 1 calc R . C62 C 0.5016(8) 0.2578(9) 0.1975(8) 0.077(3) Uani 1 d . . H62 H 0.5655(8) 0.2903(9) 0.2015(8) 0.063(7) Uiso 1 calc R . C63 C 0.4556(7) 0.2544(7) 0.2713(7) 0.056(2) Uani 1 d . . H63 H 0.4839(7) 0.2856(7) 0.3355(7) 0.063(7) Uiso 1 calc R . C64 C 0.2587(7) 0.0872(7) -0.0330(7) 0.051(2) Uani 1 d . . C65 C 0.2538(7) 0.0008(7) -0.1188(7) 0.060(3) Uani 1 d . . H65 H 0.2536(7) -0.0579(7) -0.1176(7) 0.065(5) Uiso 1 calc R . C66 C 0.2492(8) -0.0015(9) -0.2066(8) 0.074(3) Uani 1 d . . H66 H 0.2460(8) -0.0618(9) -0.2628(8) 0.065(5) Uiso 1 calc R . C67 C 0.2492(8) 0.0816(11) -0.2138(9) 0.075(3) Uani 1 d . . H67 H 0.2455(8) 0.0793(11) -0.2733(9) 0.065(5) Uiso 1 calc R . C68 C 0.2549(9) 0.1683(9) -0.1290(9) 0.075(3) Uani 1 d . . H68 H 0.2561(9) 0.2268(9) -0.1307(9) 0.065(5) Uiso 1 calc R . C69 C 0.2588(8) 0.1709(8) -0.0423(8) 0.062(3) Uani 1 d . . H69 H 0.2616(8) 0.2315(8) 0.0135(8) 0.065(5) Uiso 1 calc R . B1 B 0.2605(7) -0.0380(8) 0.4059(7) 0.042(2) Uani 1 d . . B2 B 0.2143(8) 0.4193(7) 0.5211(8) 0.049(3) Uani 1 d . . B3 B 0.2580(8) 0.0917(8) 0.0700(7) 0.046(3) Uani 1 d . . C1S C 0.3357(19) 0.5129(18) -0.0587(17) 0.182(9) Uiso 1 d D . C2S C 0.2712(30) 0.4956(34) 0.0052(30) 0.367(24) Uiso 1 d D . C3S C 0.3308(32) 0.5595(32) 0.0951(33) 0.362(23) Uiso 1 d D . C4S C 0.4189(24) 0.6271(23) 0.1019(21) 0.231(12) Uiso 1 d D . C5S C 0.4924(22) 0.6500(21) 0.0479(21) 0.240(13) Uiso 1 d D . C6S C 0.4320(22) 0.5799(23) -0.0432(22) 0.258(14) Uiso 1 d D . C7S C 0.4827(31) 0.5473(35) -0.1234(25) 0.449(31) Uiso 1 d D . C8S C 0.0044(32) 0.6144(23) 0.0882(26) 0.323(19) Uiso 1 d D . C9S C 0.0173(20) 0.5731(25) -0.0101(25) 0.194(9) Uiso 1 d D . C10S C -0.0053(32) 0.5237(39) 0.0898(30) 0.301(18) Uiso 1 d D . C11S C -0.0133(32) 0.5704(30) 0.1758(32) 0.158(15) Uiso 0.50 d P . 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 0.0301(2) 0.0382(2) 0.0419(2) 0.0163(2) 0.00827(14) 0.00858(13) N1 0.036(4) 0.047(4) 0.044(4) 0.024(4) 0.001(4) 0.012(3) N2 0.036(4) 0.048(4) 0.057(5) 0.026(4) 0.007(4) 0.016(3) N3 0.031(4) 0.038(4) 0.050(5) 0.014(4) 0.010(3) 0.017(3) N4 0.035(4) 0.037(4) 0.048(5) 0.018(4) 0.010(3) 0.008(3) N5 0.038(4) 0.045(4) 0.040(5) 0.019(4) 0.004(3) 0.009(3) N6 0.033(4) 0.044(4) 0.050(5) 0.018(4) 0.005(4) -0.002(3) N11 0.038(4) 0.042(4) 0.051(5) 0.024(4) 0.001(4) 0.005(3) N21 0.030(4) 0.039(4) 0.055(5) 0.022(4) 0.004(3) 0.013(3) N31 0.039(5) 0.037(4) 0.050(5) 0.012(4) 0.009(4) 0.007(4) N41 0.033(4) 0.042(4) 0.053(5) 0.023(4) 0.012(4) 0.015(3) N51 0.032(4) 0.051(4) 0.038(4) 0.017(4) 0.004(4) 0.010(3) N61 0.042(5) 0.058(5) 0.042(5) 0.022(4) 0.012(4) 0.008(4) C11 0.050(6) 0.067(6) 0.086(8) 0.054(6) 0.005(6) -0.002(5) C12 0.039(6) 0.077(7) 0.082(8) 0.046(7) -0.002(5) -0.002(5) C13 0.038(6) 0.056(6) 0.051(6) 0.026(5) -0.003(5) 0.006(4) C14 0.045(6) 0.053(5) 0.054(6) 0.033(5) 0.005(5) 0.019(5) C15 0.053(6) 0.059(6) 0.043(6) 0.026(6) 0.007(5) 0.019(5) C16 0.101(10) 0.072(8) 0.055(8) 0.033(7) 0.032(7) 0.047(7) C17 0.112(11) 0.048(6) 0.050(7) 0.021(6) 0.007(8) 0.020(7) C18 0.071(8) 0.059(7) 0.066(8) 0.024(7) -0.016(6) 0.000(6) C19 0.053(7) 0.050(6) 0.066(7) 0.024(6) -0.006(6) 0.012(5) C21 0.039(6) 0.055(6) 0.087(8) 0.039(6) 0.007(5) 0.016(5) C22 0.044(6) 0.074(7) 0.093(8) 0.044(7) 0.020(6) 0.028(5) C23 0.036(6) 0.069(6) 0.074(7) 0.038(6) 0.020(5) 0.019(5) C24 0.043(5) 0.052(6) 0.057(6) 0.030(5) 0.016(5) 0.017(4) C25 0.060(6) 0.054(6) 0.059(7) 0.031(5) 0.018(5) 0.022(5) C26 0.070(7) 0.088(9) 0.076(8) 0.056(8) 0.018(6) 0.031(6) C27 0.064(7) 0.074(8) 0.114(11) 0.068(9) 0.036(7) 0.036(6) C28 0.091(9) 0.043(6) 0.087(9) 0.029(6) 0.032(7) 0.023(6) C29 0.064(7) 0.051(6) 0.065(7) 0.028(6) 0.018(6) 0.012(5) C31 0.038(6) 0.040(5) 0.072(7) 0.008(5) 0.006(5) -0.003(5) C32 0.035(6) 0.064(7) 0.079(8) 0.020(6) -0.003(6) 0.002(5) C33 0.032(5) 0.056(6) 0.074(7) 0.027(6) 0.010(5) 0.014(5) C34 0.044(6) 0.032(4) 0.051(6) 0.015(4) 0.009(5) 0.005(4) C35 0.041(5) 0.051(5) 0.061(7) 0.030(5) 0.016(5) 0.014(4) C36 0.072(8) 0.061(7) 0.071(8) 0.031(6) 0.027(7) 0.010(6) C37 0.125(12) 0.055(7) 0.046(7) 0.027(6) 0.000(7) 0.004(7) C38 0.069(8) 0.065(7) 0.072(8) 0.034(6) 0.004(6) 0.015(6) C39 0.048(6) 0.052(6) 0.066(7) 0.027(5) 0.013(5) 0.013(5) C41 0.051(6) 0.053(6) 0.066(7) 0.023(5) 0.030(6) 0.028(5) C42 0.039(5) 0.055(6) 0.076(7) 0.036(6) 0.024(5) 0.013(5) C43 0.037(5) 0.045(5) 0.060(6) 0.022(5) 0.011(5) 0.003(4) C44 0.047(6) 0.039(5) 0.054(7) 0.016(5) 0.015(5) 0.007(4) C45 0.054(6) 0.047(6) 0.068(7) 0.024(6) 0.020(5) 0.014(5) C46 0.085(9) 0.039(6) 0.094(10) 0.019(7) 0.025(8) 0.022(6) C47 0.049(7) 0.059(7) 0.087(10) 0.002(7) 0.017(7) 0.014(5) C48 0.059(7) 0.067(7) 0.062(7) 0.015(7) 0.014(6) 0.016(6) C49 0.075(8) 0.042(6) 0.059(7) 0.008(6) 0.018(6) 0.023(5) C51 0.057(7) 0.079(7) 0.042(6) 0.025(6) -0.002(6) 0.017(6) C52 0.040(6) 0.090(8) 0.059(7) 0.022(6) 0.007(6) 0.026(6) C53 0.038(6) 0.063(6) 0.047(6) 0.016(5) 0.014(5) 0.019(5) C54 0.043(5) 0.051(5) 0.037(5) 0.019(5) 0.006(4) 0.009(4) C55 0.060(7) 0.050(6) 0.048(6) 0.016(5) 0.012(5) 0.009(5) C56 0.080(8) 0.061(7) 0.065(8) 0.027(6) 0.010(6) 0.006(6) C57 0.121(12) 0.072(8) 0.054(7) 0.029(7) 0.015(8) 0.032(8) C58 0.086(9) 0.091(9) 0.078(9) 0.034(8) 0.032(7) 0.058(8) C59 0.056(7) 0.073(7) 0.074(8) 0.032(6) 0.021(6) 0.022(6) C61 0.054(7) 0.098(8) 0.059(7) 0.038(7) 0.021(6) -0.005(6) C62 0.041(6) 0.095(9) 0.073(8) 0.029(7) 0.012(6) -0.010(6) C63 0.044(6) 0.061(6) 0.054(6) 0.025(5) 0.003(5) 0.002(5) C64 0.051(6) 0.055(6) 0.047(6) 0.024(6) 0.011(5) 0.012(5) C65 0.066(7) 0.055(6) 0.057(7) 0.024(6) 0.025(5) 0.013(5) C66 0.083(8) 0.089(8) 0.043(7) 0.024(6) 0.022(6) 0.020(7) C67 0.055(7) 0.129(11) 0.075(9) 0.072(9) 0.027(6) 0.028(7) C68 0.087(9) 0.077(8) 0.071(8) 0.041(8) 0.016(7) 0.022(7) C69 0.067(7) 0.067(7) 0.051(7) 0.028(6) 0.012(5) 0.015(5) B1 0.038(6) 0.052(6) 0.040(6) 0.026(6) -0.002(5) 0.010(5) B2 0.050(7) 0.032(5) 0.063(8) 0.019(6) 0.019(6) 0.012(5) B3 0.040(6) 0.050(6) 0.038(6) 0.016(5) 0.010(5) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N3 2.487(7) . ? U1 N5 2.497(7) . ? U1 N1 2.518(7) . ? U1 N2 2.531(6) . ? U1 N6 2.558(7) . ? U1 N4 2.569(7) . ? N1 C13 1.350(11) . ? N1 N11 1.361(9) . ? N2 C23 1.340(11) . ? N2 N21 1.347(9) . ? N3 C33 1.348(11) . ? N3 N31 1.353(9) . ? N4 C43 1.334(10) . ? N4 N41 1.362(9) . ? N5 C53 1.333(11) . ? N5 N51 1.362(9) . ? N6 C63 1.338(11) . ? N6 N61 1.359(10) . ? N11 C11 1.346(11) . ? N11 B1 1.583(12) . ? N21 C21 1.336(11) . ? N21 B1 1.572(12) . ? N31 C31 1.328(11) . ? N31 B2 1.581(13) . ? N41 C41 1.342(11) . ? N41 B2 1.579(12) . ? N51 C51 1.333(11) . ? N51 B3 1.587(12) . ? N61 C61 1.329(11) . ? N61 B3 1.585(13) . ? C11 C12 1.367(13) . ? C12 C13 1.355(12) . ? C14 C15 1.381(12) . ? C14 C19 1.402(13) . ? C14 B1 1.604(14) . ? C15 C16 1.398(14) . ? C16 C17 1.36(2) . ? C17 C18 1.38(2) . ? C18 C19 1.383(14) . ? C21 C22 1.354(13) . ? C22 C23 1.374(13) . ? C24 C29 1.392(13) . ? C24 C25 1.393(13) . ? C24 B1 1.622(12) . ? C25 C26 1.373(13) . ? C26 C27 1.36(2) . ? C27 C28 1.35(2) . ? C28 C29 1.382(13) . ? C31 C32 1.355(13) . ? C32 C33 1.368(13) . ? C34 C35 1.385(12) . ? C34 C39 1.402(12) . ? C34 B2 1.593(14) . ? C35 C36 1.392(14) . ? C36 C37 1.39(2) . ? C37 C38 1.35(2) . ? C38 C39 1.379(14) . ? C41 C42 1.359(12) . ? C42 C43 1.379(13) . ? C44 C49 1.382(13) . ? C44 C45 1.391(12) . ? C44 B2 1.630(14) . ? C45 C46 1.401(14) . ? C46 C47 1.34(2) . ? C47 C48 1.38(2) . ? C48 C49 1.382(14) . ? C51 C52 1.340(14) . ? C52 C53 1.361(13) . ? C54 C55 1.371(12) . ? C54 C59 1.390(13) . ? C54 B3 1.615(13) . ? C55 C56 1.368(13) . ? C56 C57 1.35(2) . ? C57 C58 1.34(2) . ? C58 C59 1.384(15) . ? C61 C62 1.335(15) . ? C62 C63 1.376(14) . ? C64 C65 1.374(13) . ? C64 C69 1.393(13) . ? C64 B3 1.609(14) . ? C65 C66 1.380(14) . ? C66 C67 1.366(15) . ? C67 C68 1.37(2) . ? C68 C69 1.361(14) . ? C1S C2S 1.47(2) . ? C1S C6S 1.50(3) . ? C2S C3S 1.42(2) . ? C3S C4S 1.46(2) . ? C4S C5S 1.47(2) . ? C5S C6S 1.45(2) . ? C6S C7S 1.38(2) . ? C8S C9S 1.41(2) . ? C8S C10S 1.43(2) . ? C8S C11S 1.85(7) . ? C9S C10S 1.41(4) 2_565 ? C10S C11S 1.22(5) . ? C10S C9S 1.41(4) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 U1 N5 128.2(2) . . ? N3 U1 N1 132.3(2) . . ? N5 U1 N1 91.0(2) . . ? N3 U1 N2 95.1(2) . . ? N5 U1 N2 128.2(2) . . ? N1 U1 N2 73.6(2) . . ? N3 U1 N6 87.7(2) . . ? N5 U1 N6 73.2(2) . . ? N1 U1 N6 134.3(2) . . ? N2 U1 N6 83.0(2) . . ? N3 U1 N4 73.6(2) . . ? N5 U1 N4 86.7(2) . . ? N1 U1 N4 84.4(2) . . ? N2 U1 N4 137.9(2) . . ? N6 U1 N4 135.1(2) . . ? C13 N1 N11 105.9(7) . . ? C13 N1 U1 126.4(5) . . ? N11 N1 U1 127.0(5) . . ? C23 N2 N21 106.8(7) . . ? C23 N2 U1 127.2(6) . . ? N21 N2 U1 125.8(5) . . ? C33 N3 N31 105.8(7) . . ? C33 N3 U1 123.0(6) . . ? N31 N3 U1 130.0(5) . . ? C43 N4 N41 106.7(7) . . ? C43 N4 U1 126.7(6) . . ? N41 N4 U1 126.4(5) . . ? C53 N5 N51 106.7(7) . . ? C53 N5 U1 124.4(6) . . ? N51 N5 U1 128.4(5) . . ? C63 N6 N61 106.4(7) . . ? C63 N6 U1 125.4(6) . . ? N61 N6 U1 128.2(5) . . ? C11 N11 N1 109.1(7) . . ? C11 N11 B1 129.2(7) . . ? N1 N11 B1 121.5(6) . . ? C21 N21 N2 108.1(7) . . ? C21 N21 B1 128.4(7) . . ? N2 N21 B1 122.5(6) . . ? C31 N31 N3 109.3(7) . . ? C31 N31 B2 128.2(7) . . ? N3 N31 B2 121.9(7) . . ? C41 N41 N4 108.0(7) . . ? C41 N41 B2 128.2(7) . . ? N4 N41 B2 122.4(7) . . ? C51 N51 N5 108.0(7) . . ? C51 N51 B3 127.1(8) . . ? N5 N51 B3 124.0(7) . . ? C61 N61 N6 108.2(8) . . ? C61 N61 B3 128.3(8) . . ? N6 N61 B3 122.3(7) . . ? N11 C11 C12 108.4(8) . . ? C13 C12 C11 105.9(8) . . ? N1 C13 C12 110.6(8) . . ? C15 C14 C19 115.4(9) . . ? C15 C14 B1 123.8(8) . . ? C19 C14 B1 120.8(8) . . ? C14 C15 C16 122.3(10) . . ? C17 C16 C15 120.1(11) . . ? C16 C17 C18 120.0(10) . . ? C17 C18 C19 119.3(10) . . ? C18 C19 C14 122.8(10) . . ? N21 C21 C22 110.5(8) . . ? C21 C22 C23 104.1(9) . . ? N2 C23 C22 110.4(9) . . ? C29 C24 C25 116.1(8) . . ? C29 C24 B1 122.3(8) . . ? C25 C24 B1 121.5(8) . . ? C26 C25 C24 121.9(10) . . ? C27 C26 C25 119.4(10) . . ? C28 C27 C26 121.4(10) . . ? C27 C28 C29 119.2(11) . . ? C28 C29 C24 121.9(10) . . ? N31 C31 C32 109.6(8) . . ? C31 C32 C33 104.9(8) . . ? N3 C33 C32 110.3(8) . . ? C35 C34 C39 115.7(9) . . ? C35 C34 B2 123.1(8) . . ? C39 C34 B2 121.1(8) . . ? C34 C35 C36 121.0(9) . . ? C37 C36 C35 120.5(10) . . ? C38 C37 C36 120.1(10) . . ? C37 C38 C39 118.8(11) . . ? C38 C39 C34 123.8(9) . . ? N41 C41 C42 110.3(8) . . ? C41 C42 C43 104.2(8) . . ? N4 C43 C42 110.8(8) . . ? C49 C44 C45 116.3(9) . . ? C49 C44 B2 120.2(8) . . ? C45 C44 B2 123.5(9) . . ? C44 C45 C46 120.8(10) . . ? C47 C46 C45 120.9(11) . . ? C46 C47 C48 120.0(11) . . ? C47 C48 C49 119.3(11) . . ? C44 C49 C48 122.6(10) . . ? N51 C51 C52 109.6(9) . . ? C51 C52 C53 105.9(9) . . ? N5 C53 C52 109.8(8) . . ? C55 C54 C59 115.3(9) . . ? C55 C54 B3 124.4(8) . . ? C59 C54 B3 120.4(8) . . ? C56 C55 C54 122.7(10) . . ? C57 C56 C55 120.6(11) . . ? C58 C57 C56 119.0(11) . . ? C57 C58 C59 120.7(11) . . ? C58 C59 C54 121.7(10) . . ? N61 C61 C62 110.6(9) . . ? C61 C62 C63 105.0(9) . . ? N6 C63 C62 109.9(9) . . ? C65 C64 C69 114.8(9) . . ? C65 C64 B3 123.1(8) . . ? C69 C64 B3 122.0(9) . . ? C64 C65 C66 121.8(10) . . ? C67 C66 C65 122.3(11) . . ? C66 C67 C68 116.5(10) . . ? C69 C68 C67 121.4(10) . . ? C68 C69 C64 123.1(10) . . ? N21 B1 N11 107.8(7) . . ? N21 B1 C14 108.1(7) . . ? N11 B1 C14 108.7(7) . . ? N21 B1 C24 107.3(7) . . ? N11 B1 C24 108.7(7) . . ? C14 B1 C24 115.9(7) . . ? N41 B2 N31 109.0(7) . . ? N41 B2 C34 107.0(8) . . ? N31 B2 C34 110.6(7) . . ? N41 B2 C44 107.6(7) . . ? N31 B2 C44 106.7(8) . . ? C34 B2 C44 115.8(7) . . ? N61 B3 N51 108.1(7) . . ? N61 B3 C64 108.4(7) . . ? N51 B3 C64 106.7(8) . . ? N61 B3 C54 108.5(7) . . ? N51 B3 C54 109.1(7) . . ? C64 B3 C54 115.8(8) . . ? C2S C1S C6S 134.8(29) . . ? C3S C2S C1S 99.1(33) . . ? C2S C3S C4S 120.8(38) . . ? C3S C4S C5S 145.3(35) . . ? C6S C5S C4S 91.1(25) . . ? C7S C6S C5S 115.2(24) . . ? C7S C6S C1S 113.3(24) . . ? C5S C6S C1S 127.6(27) . . ? C9S C8S C10S 95.7(16) . . ? C9S C8S C11S 137.0(30) . . ? C10S C8S C11S 41.3(28) . . ? C10S C9S C8S 135.4(28) 2_565 . ? C11S C10S C9S 143.1(42) . 2_565 ? C11S C10S C8S 88.1(47) . . ? C9S C10S C8S 127.8(31) 2_565 . ? C10S C11S C8S 50.6(25) . . ? _refine_diff_density_max 2.133 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.118