# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1561 data_LB59 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [methyltris(3,5-dimethylpyrazol-1-yl)boratothallium(I)] ; _chemical_name_common ? _chemical_melting_point 232 _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B N6 Tl' _chemical_formula_weight 515.59 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' 'Tl' 'Tl' -2.8358 9.6688 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 11.46560(10) _cell_length_b 9.96760(10) _cell_length_c 17.0414(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.1250(10) _cell_angle_gamma 90.00 _cell_volume 1936.45(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7222 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour 'colourless, transparent' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 8.350 _exptl_absorpt_correction_type 'empirical (SADABS)' _exptl_absorpt_correction_T_min 0.1229 _exptl_absorpt_correction_T_max 0.2528 _exptl_absorpt_process_details ? _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_type 'Siemens SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14261 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4432 _reflns_number_gt 3304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00185(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4432 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.270054(16) 0.269618(17) 0.226951(10) 0.04835(8) Uani 1 1 d . . . B B 0.4913(4) 0.5167(5) 0.2902(3) 0.0385(11) Uani 1 1 d . . . N1 N 0.3924(3) 0.5335(3) 0.34628(19) 0.0331(7) Uani 1 1 d . . . N2 N 0.2881(3) 0.4669(3) 0.3308(2) 0.0395(8) Uani 1 1 d . . . C1 C 0.2244(4) 0.4941(4) 0.3899(3) 0.0467(11) Uani 1 1 d . . . C2 C 0.2851(4) 0.5771(5) 0.4437(3) 0.0502(12) Uani 1 1 d . . . H2 H 0.2590 0.6117 0.4894 0.080 Uiso 1 1 calc R . . C3 C 0.3922(4) 0.5990(4) 0.4168(2) 0.0399(10) Uani 1 1 d . . . C4 C 0.1010(4) 0.4410(6) 0.3900(3) 0.0738(16) Uani 1 1 d . . . H4A H 0.0460 0.5125 0.3776 0.080 Uiso 1 1 calc R . . H4B H 0.0910 0.4057 0.4413 0.080 Uiso 1 1 calc R . . H4C H 0.0876 0.3713 0.3513 0.080 Uiso 1 1 calc R . . C5 C 0.4911(4) 0.6775(5) 0.4571(3) 0.0613(14) Uani 1 1 d . . . H5A H 0.5610 0.6239 0.4617 0.080 Uiso 1 1 calc R . . H5B H 0.4729 0.7028 0.5088 0.080 Uiso 1 1 calc R . . H5C H 0.5033 0.7567 0.4270 0.080 Uiso 1 1 calc R . . N3 N 0.5562(3) 0.3835(3) 0.3146(2) 0.0387(8) Uani 1 1 d . . . N4 N 0.4878(3) 0.2697(3) 0.3134(2) 0.0439(9) Uani 1 1 d . . . C6 C 0.5606(5) 0.1691(5) 0.3350(3) 0.0516(12) Uani 1 1 d . . . C7 C 0.6740(4) 0.2155(5) 0.3517(3) 0.0593(13) Uani 1 1 d . . . H7 H 0.7399 0.1648 0.3688 0.080 Uiso 1 1 calc R . . C8 C 0.6701(4) 0.3511(5) 0.3380(3) 0.0461(11) Uani 1 1 d . . . C9 C 0.5149(5) 0.0275(5) 0.3388(3) 0.0807(18) Uani 1 1 d . . . H9A H 0.5046 0.0055 0.3925 0.080 Uiso 1 1 calc R . . H9B H 0.5700 -0.0336 0.3196 0.080 Uiso 1 1 calc R . . H9C H 0.4410 0.0204 0.3068 0.080 Uiso 1 1 calc R . . C10 C 0.7710(4) 0.4447(6) 0.3443(3) 0.0738(17) Uani 1 1 d . . . H10A H 0.8418 0.3962 0.3607 0.080 Uiso 1 1 calc R . . H10B H 0.7595 0.5131 0.3823 0.080 Uiso 1 1 calc R . . H10C H 0.7772 0.4854 0.2938 0.080 Uiso 1 1 calc R . . N5 N 0.4318(3) 0.4974(3) 0.20318(19) 0.0387(8) Uani 1 1 d . . . N6 N 0.3380(3) 0.5799(3) 0.1762(2) 0.0446(9) Uani 1 1 d . . . C11 C 0.3187(4) 0.5602(5) 0.0979(3) 0.0521(12) Uani 1 1 d . . . C12 C 0.3986(5) 0.4685(5) 0.0747(3) 0.0593(13) Uani 1 1 d . . . H12 H 0.4026 0.4374 0.0236 0.080 Uiso 1 1 calc R . . C13 C 0.4710(4) 0.4314(5) 0.1406(3) 0.0487(11) Uani 1 1 d . . . C14 C 0.2233(5) 0.6345(6) 0.0494(3) 0.0769(17) Uani 1 1 d . . . H14A H 0.1842 0.6930 0.0829 0.080 Uiso 1 1 calc R . . H14B H 0.1680 0.5717 0.0242 0.080 Uiso 1 1 calc R . . H14C H 0.2566 0.6867 0.0100 0.080 Uiso 1 1 calc R . . C15 C 0.5738(5) 0.3393(6) 0.1440(3) 0.0691(15) Uani 1 1 d . . . H15A H 0.6426 0.3853 0.1671 0.080 Uiso 1 1 calc R . . H15B H 0.5854 0.3108 0.0916 0.080 Uiso 1 1 calc R . . H15C H 0.5596 0.2624 0.1755 0.080 Uiso 1 1 calc R . . C16 C 0.5729(4) 0.6469(5) 0.2881(3) 0.0558(13) Uani 1 1 d . . . H16A H 0.6193 0.6569 0.3381 0.080 Uiso 1 1 calc R . . H16B H 0.5246 0.7249 0.2777 0.080 Uiso 1 1 calc R . . H16C H 0.6238 0.6368 0.2472 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl 0.05232(12) 0.04780(12) 0.04390(11) -0.00603(9) 0.00040(8) -0.01393(9) B 0.039(3) 0.036(3) 0.040(3) 0.001(2) 0.004(2) -0.003(2) N1 0.0314(18) 0.0322(18) 0.0350(18) 0.0007(14) 0.0003(16) -0.0016(14) N2 0.0332(19) 0.043(2) 0.042(2) -0.0023(16) 0.0035(18) -0.0035(16) C1 0.039(3) 0.054(3) 0.049(3) 0.007(2) 0.011(2) 0.009(2) C2 0.056(3) 0.060(3) 0.036(3) 0.001(2) 0.007(2) 0.008(2) C3 0.048(3) 0.034(2) 0.035(2) 0.0016(18) -0.007(2) 0.0068(19) C4 0.050(3) 0.097(4) 0.077(4) -0.004(3) 0.024(3) -0.004(3) C5 0.070(3) 0.063(3) 0.047(3) -0.008(3) -0.010(3) -0.005(3) N3 0.033(2) 0.041(2) 0.042(2) 0.0016(16) 0.0016(17) -0.0001(16) N4 0.048(2) 0.0361(19) 0.047(2) 0.0026(17) 0.0050(19) 0.0017(17) C6 0.063(3) 0.045(3) 0.048(3) 0.004(2) 0.008(3) 0.008(2) C7 0.052(3) 0.073(4) 0.053(3) 0.008(3) 0.007(3) 0.024(3) C8 0.036(3) 0.061(3) 0.042(3) 0.002(2) 0.006(2) 0.008(2) C9 0.110(5) 0.046(3) 0.086(4) 0.005(3) 0.012(4) 0.010(3) C10 0.034(3) 0.108(5) 0.078(4) 0.010(3) 0.001(3) -0.004(3) N5 0.038(2) 0.044(2) 0.0354(18) 0.0057(16) 0.0070(17) 0.0007(16) N6 0.042(2) 0.054(2) 0.038(2) 0.0042(17) 0.0038(19) 0.0030(17) C11 0.056(3) 0.062(3) 0.038(3) 0.006(2) 0.001(3) 0.004(2) C12 0.066(4) 0.076(4) 0.037(3) -0.004(2) 0.013(3) 0.001(3) C13 0.052(3) 0.055(3) 0.041(3) 0.003(2) 0.014(2) 0.002(2) C14 0.079(4) 0.100(5) 0.048(3) 0.009(3) -0.008(3) 0.018(3) C15 0.077(4) 0.082(4) 0.052(3) -0.002(3) 0.021(3) 0.027(3) C16 0.053(3) 0.054(3) 0.061(3) 0.002(2) 0.007(3) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl N2 2.638(3) . ? Tl N4 2.760(4) . ? Tl N6 2.876(4) 2_545 ? B N3 1.557(6) . ? B N1 1.568(6) . ? B N5 1.577(6) . ? B C16 1.602(6) . ? N1 C3 1.367(5) . ? N1 N2 1.368(4) . ? N2 C1 1.334(5) . ? C1 C2 1.369(6) . ? C1 C4 1.510(6) . ? C2 C3 1.374(6) . ? C3 C5 1.484(6) . ? N3 C8 1.362(5) . ? N3 N4 1.378(4) . ? N4 C6 1.331(5) . ? C6 C7 1.380(7) . ? C6 C9 1.510(7) . ? C7 C8 1.372(7) . ? C8 C10 1.482(6) . ? N5 C13 1.369(5) . ? N5 N6 1.393(5) . ? N6 C11 1.343(6) . ? N6 Tl 2.876(4) 2 ? C11 C12 1.380(7) . ? C11 C14 1.496(6) . ? C12 C13 1.373(6) . ? C13 C15 1.490(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 N2 Tl N4 68.89(10) . . ? N2 Tl N6 96.49(10) . 2_545 ? N4 Tl N6 96.57(10) . 2_545 ? N3 B N1 106.5(3) . . ? N3 B N5 107.0(3) . . ? N1 B N5 108.5(3) . . ? N3 B C16 115.7(4) . . ? N1 B C16 112.9(4) . . ? N5 B C16 105.8(4) . . ? C3 N1 N2 108.6(3) . . ? C3 N1 B 130.9(3) . . ? N2 N1 B 120.3(3) . . ? C1 N2 N1 107.0(3) . . ? C1 N2 Tl 130.3(3) . . ? N1 N2 Tl 119.7(2) . . ? N2 C1 C2 110.4(4) . . ? N2 C1 C4 121.3(4) . . ? C2 C1 C4 128.3(4) . . ? C1 C2 C3 106.3(4) . . ? N1 C3 C2 107.6(4) . . ? N1 C3 C5 125.9(4) . . ? C2 C3 C5 126.5(4) . . ? C8 N3 N4 109.6(3) . . ? C8 N3 B 134.1(4) . . ? N4 N3 B 116.3(3) . . ? C6 N4 N3 106.0(4) . . ? C6 N4 Tl 130.7(3) . . ? N3 N4 Tl 119.3(2) . . ? N4 C6 C7 110.7(4) . . ? N4 C6 C9 120.4(5) . . ? C7 C6 C9 128.9(5) . . ? C8 C7 C6 106.3(4) . . ? N3 C8 C7 107.2(4) . . ? N3 C8 C10 126.0(4) . . ? C7 C8 C10 126.7(4) . . ? C13 N5 N6 109.4(3) . . ? C13 N5 B 130.3(4) . . ? N6 N5 B 118.7(3) . . ? C11 N6 N5 106.3(4) . . ? C11 N6 Tl 129.1(3) . 2 ? N5 N6 Tl 124.3(2) . 2 ? N6 C11 C12 109.7(4) . . ? N6 C11 C14 120.6(5) . . ? C12 C11 C14 129.7(5) . . ? C13 C12 C11 107.8(4) . . ? N5 C13 C12 106.7(4) . . ? N5 C13 C15 126.1(4) . . ? C12 C13 C15 127.2(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.651 _refine_diff_density_min -1.211 _refine_diff_density_rms 0.173 #=END data_LB112 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [methyltris(3-methylpyrazol-1-yl)boratothallium(I)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H18 B N6 Tl' _chemical_formula_weight 473.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 8.17560(10) _cell_length_b 14.19210(10) _cell_length_c 13.97460(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.7710(10) _cell_angle_gamma 90.00 _cell_volume 1610.15(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7011 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour 'colorless, transparent' _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.62 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 10.033 _exptl_absorpt_correction_type 'empirical (SADABS)' _exptl_absorpt_correction_T_min 0.0154 _exptl_absorpt_correction_T_max 0.0483 _exptl_absorpt_process_details ? _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_type 'Siemens SMART CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12008 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3685 _reflns_number_gt 2800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3685 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.24906(2) 0.190079(15) 0.180212(13) 0.04630(8) Uani 1 1 d . . . B B 0.1827(7) 0.3386(4) 0.3885(4) 0.0382(12) Uani 1 1 d . . . N1 N 0.0934(4) 0.3828(3) 0.2947(3) 0.0361(8) Uani 1 1 d . . . N2 N 0.0947(5) 0.3423(3) 0.2054(3) 0.0410(9) Uani 1 1 d . . . C1 C 0.0061(6) 0.3962(4) 0.1419(4) 0.0467(12) Uani 1 1 d . . . C2 C -0.0523(7) 0.4731(4) 0.1885(4) 0.0559(14) Uani 1 1 d . . . H2 H -0.1169 0.5221 0.1606 0.080 Uiso 1 1 calc R . . C3 C 0.0039(6) 0.4626(4) 0.2836(4) 0.0475(12) Uani 1 1 d . . . H3 H -0.0161 0.5036 0.3327 0.080 Uiso 1 1 calc R . . C4 C -0.0183(9) 0.3709(5) 0.0375(4) 0.0658(17) Uani 1 1 d . . . H4A H 0.0804 0.3845 0.0091 0.080 Uiso 1 1 calc R . . H4B H -0.1080 0.4069 0.0055 0.080 Uiso 1 1 calc R . . H4C H -0.0430 0.3049 0.0308 0.080 Uiso 1 1 calc R . . N3 N 0.3695(5) 0.3307(3) 0.3776(3) 0.0406(9) Uani 1 1 d . . . N4 N 0.4291(5) 0.2801(3) 0.3058(3) 0.0422(10) Uani 1 1 d . . . C5 C 0.5917(6) 0.2917(4) 0.3156(4) 0.0462(12) Uani 1 1 d . . . C6 C 0.6396(7) 0.3488(4) 0.3946(4) 0.0563(14) Uani 1 1 d . . . H6 H 0.7459 0.3674 0.4181 0.080 Uiso 1 1 calc R . . C7 C 0.4962(6) 0.3718(4) 0.4303(4) 0.0480(13) Uani 1 1 d . . . H7 H 0.4883 0.4103 0.4833 0.080 Uiso 1 1 calc R . . C8 C 0.6945(7) 0.2452(5) 0.2479(4) 0.0628(16) Uani 1 1 d . . . H8A H 0.6479 0.1849 0.2291 0.080 Uiso 1 1 calc R . . H8B H 0.8045 0.2367 0.2792 0.080 Uiso 1 1 calc R . . H8C H 0.6972 0.2840 0.1918 0.080 Uiso 1 1 calc R . . N5 N 0.1100(5) 0.2377(3) 0.3990(3) 0.0363(9) Uani 1 1 d . . . N6 N 0.1264(5) 0.1681(3) 0.3343(3) 0.0394(9) Uani 1 1 d . . . C9 C 0.0444(6) 0.0925(3) 0.3619(3) 0.0430(11) Uani 1 1 d . . . C10 C -0.0253(7) 0.1148(4) 0.4454(4) 0.0529(14) Uani 1 1 d . . . H10 H -0.0887 0.0759 0.4800 0.080 Uiso 1 1 calc R . . C11 C 0.0190(7) 0.2051(4) 0.4653(4) 0.0473(13) Uani 1 1 d . . . H11 H -0.0096 0.2396 0.5174 0.080 Uiso 1 1 calc R . . C12 C 0.0372(8) 0.0039(4) 0.3057(5) 0.0656(16) Uani 1 1 d . . . H12A H -0.0630 0.0023 0.2624 0.080 Uiso 1 1 calc R . . H12B H 0.0400 -0.0488 0.3489 0.080 Uiso 1 1 calc R . . H12C H 0.1298 0.0009 0.2696 0.080 Uiso 1 1 calc R . . C13 C 0.1562(7) 0.4009(4) 0.4796(4) 0.0508(13) Uani 1 1 d . . . H13A H 0.2122 0.3723 0.5366 0.080 Uiso 1 1 calc R . . H13B H 0.0406 0.4051 0.4856 0.080 Uiso 1 1 calc R . . H13C H 0.1996 0.4629 0.4719 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl 0.04876(13) 0.05418(13) 0.03704(11) -0.00866(10) 0.00959(7) 0.00387(10) B 0.042(3) 0.035(3) 0.038(3) -0.003(2) 0.005(2) 0.001(2) N1 0.034(2) 0.033(2) 0.041(2) -0.0019(17) 0.0054(16) 0.0017(15) N2 0.045(2) 0.041(2) 0.037(2) -0.0023(18) 0.0032(17) 0.0033(17) C1 0.046(3) 0.046(3) 0.047(3) 0.010(2) 0.001(2) 0.000(2) C2 0.059(4) 0.048(3) 0.061(4) 0.012(3) 0.008(3) 0.013(2) C3 0.049(3) 0.045(3) 0.049(3) 0.000(2) 0.011(2) 0.008(2) C4 0.081(5) 0.062(4) 0.052(3) 0.007(3) -0.006(3) 0.004(3) N3 0.037(2) 0.046(3) 0.038(2) -0.0025(18) 0.0025(16) -0.0014(16) N4 0.034(2) 0.049(3) 0.044(2) -0.0029(19) 0.0054(17) -0.0001(16) C5 0.036(3) 0.051(3) 0.051(3) 0.015(2) 0.005(2) 0.003(2) C6 0.042(3) 0.064(4) 0.058(3) 0.005(3) -0.011(3) -0.013(3) C7 0.041(3) 0.052(3) 0.048(3) -0.003(3) -0.008(2) -0.006(2) C8 0.044(3) 0.079(5) 0.068(4) 0.007(3) 0.018(3) 0.004(3) N5 0.038(2) 0.038(2) 0.034(2) -0.0020(17) 0.0070(16) 0.0024(16) N6 0.043(2) 0.036(2) 0.041(2) -0.0045(17) 0.0096(17) -0.0001(16) C9 0.044(3) 0.040(3) 0.046(3) 0.001(2) 0.007(2) -0.002(2) C10 0.055(3) 0.052(3) 0.055(3) 0.010(3) 0.021(3) -0.002(2) C11 0.051(3) 0.055(4) 0.038(3) 0.003(2) 0.017(2) 0.003(2) C12 0.070(4) 0.047(4) 0.082(4) -0.012(3) 0.022(3) -0.013(3) C13 0.059(3) 0.051(3) 0.043(3) -0.010(2) 0.007(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl N6 2.499(4) . ? Tl N4 2.504(4) . ? Tl N2 2.547(4) . ? B N1 1.555(7) . ? B N3 1.557(7) . ? B N5 1.564(7) . ? B C13 1.587(7) . ? N1 C3 1.347(6) . ? N1 N2 1.374(5) . ? N2 C1 1.322(6) . ? C1 C2 1.384(7) . ? C1 C4 1.493(7) . ? C2 C3 1.362(7) . ? N3 C7 1.332(6) . ? N3 N4 1.370(6) . ? N4 C5 1.330(6) . ? C5 C6 1.387(8) . ? C5 C8 1.492(8) . ? C6 C7 1.366(8) . ? N5 C11 1.337(6) . ? N5 N6 1.356(5) . ? N6 C9 1.345(6) . ? C9 C10 1.395(7) . ? C9 C12 1.479(7) . ? C10 C11 1.352(7) . ? 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 N6 Tl N4 73.87(13) . . ? N6 Tl N2 74.39(13) . . ? N4 Tl N2 74.35(13) . . ? N1 B N3 108.4(4) . . ? N1 B N5 107.6(4) . . ? N3 B N5 109.4(4) . . ? N1 B C13 110.9(4) . . ? N3 B C13 110.3(4) . . ? N5 B C13 110.2(4) . . ? C3 N1 N2 108.0(4) . . ? C3 N1 B 129.1(4) . . ? N2 N1 B 122.9(4) . . ? C1 N2 N1 107.8(4) . . ? C1 N2 Tl 129.7(3) . . ? N1 N2 Tl 122.5(3) . . ? N2 C1 C2 109.4(5) . . ? N2 C1 C4 121.1(5) . . ? C2 C1 C4 129.5(5) . . ? C3 C2 C1 106.1(5) . . ? N1 C3 C2 108.7(5) . . ? C7 N3 N4 108.3(4) . . ? C7 N3 B 128.5(4) . . ? N4 N3 B 123.1(4) . . ? C5 N4 N3 107.2(4) . . ? C5 N4 Tl 129.3(4) . . ? N3 N4 Tl 123.4(3) . . ? N4 C5 C6 109.8(5) . . ? N4 C5 C8 120.7(5) . . ? C6 C5 C8 129.5(5) . . ? C7 C6 C5 104.8(5) . . ? N3 C7 C6 109.8(5) . . ? C11 N5 N6 108.5(4) . . ? C11 N5 B 129.0(4) . . ? N6 N5 B 122.4(4) . . ? C9 N6 N5 107.3(4) . . ? C9 N6 Tl 127.6(3) . . ? N5 N6 Tl 124.4(3) . . ? N6 C9 C10 109.0(4) . . ? N6 C9 C12 121.0(5) . . ? C10 C9 C12 129.9(5) . . ? C11 C10 C9 105.1(5) . . ? N5 C11 C10 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.661 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.146 #=END data_LB95 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [hydrotris(3,5-dimethylpyrazol-1-yl)boratothallium(I)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H22 B N6 Tl' _chemical_formula_weight 501.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.6275(5) _cell_length_b 8.61680(10) _cell_length_c 15.6585(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.8120(10) _cell_angle_gamma 90.00 _cell_volume 3585.57(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6521 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour 'colourless, transparent' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 9.016 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4236 _exptl_absorpt_correction_T_max 0.8000 _exptl_absorpt_process_details ? _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_type 'Siemens SMART CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13372 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4110 _reflns_number_gt 2909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4110 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.373115(12) 0.65393(3) 0.37733(2) 0.03761(12) Uani 1 1 d . . . B B 0.3702(3) 0.2344(10) 0.3815(7) 0.0337(19) Uani 1 1 d . . . H0 H 0.3691 0.1208 0.3815 0.080 Uiso 1 1 calc R . . N1 N 0.4188(2) 0.2887(7) 0.4753(4) 0.0294(13) Uani 1 1 d . . . N2 N 0.4299(2) 0.4434(7) 0.4915(4) 0.0318(13) Uani 1 1 d . . . C1 C 0.4727(3) 0.4546(10) 0.5763(5) 0.0354(17) Uani 1 1 d . . . C2 C 0.4892(3) 0.3079(10) 0.6161(5) 0.043(2) Uani 1 1 d . . . H2 H 0.5178 0.2843 0.6756 0.080 Uiso 1 1 calc R . . C3 C 0.4547(3) 0.2041(10) 0.5497(6) 0.0404(19) Uani 1 1 d . . . C4 C 0.4947(3) 0.6095(11) 0.6166(6) 0.052(2) Uani 1 1 d . . . H4A H 0.4778 0.6541 0.6485 0.080 Uiso 1 1 calc R . . H4B H 0.4905 0.6761 0.5639 0.080 Uiso 1 1 calc R . . H4C H 0.5298 0.5985 0.6634 0.080 Uiso 1 1 calc R . . C5 C 0.4536(4) 0.0348(12) 0.5557(7) 0.064(3) Uani 1 1 d . . . H5A H 0.4556 -0.0104 0.5018 0.080 Uiso 1 1 calc R . . H5B H 0.4227 0.0033 0.5526 0.080 Uiso 1 1 calc R . . H5C H 0.4816 0.0004 0.6168 0.080 Uiso 1 1 calc R . . N3 N 0.3721(2) 0.2888(7) 0.2880(4) 0.0293(13) Uani 1 1 d . . . N4 N 0.3688(2) 0.4421(7) 0.2644(4) 0.0307(13) Uani 1 1 d . . . C6 C 0.3722(2) 0.4523(9) 0.1832(4) 0.0303(15) Uani 1 1 d . . . C7 C 0.3789(3) 0.3044(9) 0.1548(5) 0.0357(18) Uani 1 1 d . . . H7 H 0.3825 0.2795 0.1009 0.080 Uiso 1 1 calc R . . C8 C 0.3789(3) 0.2015(9) 0.2237(5) 0.0328(17) Uani 1 1 d . . . C9 C 0.3706(4) 0.6034(10) 0.1391(6) 0.047(2) Uani 1 1 d . . . H9A H 0.4003 0.6168 0.1341 0.080 Uiso 1 1 calc R . . H9B H 0.3688 0.6841 0.1796 0.080 Uiso 1 1 calc R . . H9C H 0.3414 0.6086 0.0746 0.080 Uiso 1 1 calc R . . C10 C 0.3857(4) 0.0293(10) 0.2310(7) 0.053(2) Uani 1 1 d . . . H10A H 0.3568 -0.0187 0.2283 0.080 Uiso 1 1 calc R . . H10B H 0.4152 0.0034 0.2922 0.080 Uiso 1 1 calc R . . H10C H 0.3896 -0.0075 0.1773 0.080 Uiso 1 1 calc R . . N5 N 0.3233(2) 0.2963(7) 0.3801(4) 0.0283(13) Uani 1 1 d . . . N6 N 0.3151(2) 0.4514(8) 0.3815(4) 0.0342(13) Uani 1 1 d . . . C11 C 0.2734(3) 0.4681(10) 0.3869(5) 0.0369(17) Uani 1 1 d . . . C12 C 0.2536(3) 0.3247(10) 0.3873(6) 0.042(2) Uani 1 1 d . . . H12 H 0.2242 0.3044 0.3889 0.080 Uiso 1 1 calc R . . C13 C 0.2860(3) 0.2186(10) 0.3847(5) 0.0370(18) Uani 1 1 d . . . C14 C 0.2555(4) 0.6267(11) 0.3903(7) 0.055(2) Uani 1 1 d . . . H14A H 0.2500 0.6837 0.3331 0.080 Uiso 1 1 calc R . . H14B H 0.2803 0.6790 0.4484 0.080 Uiso 1 1 calc R . . H14C H 0.2245 0.6202 0.3915 0.080 Uiso 1 1 calc R . . C15 C 0.2825(4) 0.0454(11) 0.3859(7) 0.059(3) Uani 1 1 d . . . H15A H 0.3076 0.0068 0.4490 0.080 Uiso 1 1 calc R . . H15B H 0.2879 0.0021 0.3355 0.080 Uiso 1 1 calc R . . H15C H 0.2497 0.0163 0.3742 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl 0.04321(19) 0.03477(16) 0.04042(17) -0.00197(15) 0.02501(13) -0.00535(16) B 0.025(4) 0.036(4) 0.048(5) -0.004(4) 0.023(4) -0.004(4) N1 0.030(3) 0.036(3) 0.030(3) 0.002(3) 0.021(3) -0.002(3) N2 0.030(3) 0.038(3) 0.027(3) -0.002(3) 0.014(2) -0.007(3) C1 0.025(4) 0.053(5) 0.032(4) -0.001(4) 0.017(3) -0.001(4) C2 0.034(5) 0.060(6) 0.027(4) -0.004(4) 0.008(3) -0.003(4) C3 0.035(5) 0.048(5) 0.043(4) 0.005(4) 0.023(4) 0.003(4) C4 0.032(5) 0.077(6) 0.044(5) -0.010(4) 0.016(4) -0.015(4) C5 0.053(6) 0.068(6) 0.061(6) 0.013(5) 0.023(5) 0.004(5) N3 0.029(3) 0.035(3) 0.029(3) -0.005(3) 0.018(3) -0.002(3) N4 0.033(3) 0.039(3) 0.023(3) 0.000(3) 0.016(2) -0.001(3) C6 0.020(4) 0.049(4) 0.019(3) 0.001(3) 0.008(3) 0.001(3) C7 0.036(4) 0.051(5) 0.026(4) -0.005(3) 0.020(3) -0.007(4) C8 0.024(4) 0.043(4) 0.033(4) -0.012(3) 0.016(3) -0.008(3) C9 0.054(6) 0.060(5) 0.033(4) 0.003(4) 0.025(4) 0.000(4) C10 0.070(6) 0.047(5) 0.065(5) -0.010(5) 0.050(5) -0.003(5) N5 0.021(3) 0.034(3) 0.036(3) 0.003(3) 0.019(3) -0.002(2) N6 0.025(3) 0.041(3) 0.038(3) 0.005(3) 0.017(3) 0.002(3) C11 0.021(4) 0.055(5) 0.036(4) 0.004(4) 0.015(3) -0.001(4) C12 0.020(4) 0.063(6) 0.045(4) -0.003(4) 0.018(3) -0.008(4) C13 0.023(4) 0.047(4) 0.039(4) 0.003(4) 0.014(3) -0.011(4) C14 0.047(6) 0.063(6) 0.061(6) 0.004(5) 0.033(5) 0.011(5) C15 0.050(6) 0.058(6) 0.073(6) -0.001(5) 0.033(5) -0.023(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 Tl N4 2.499(6) . ? Tl N6 2.515(6) . ? Tl N2 2.534(6) . ? B N5 1.522(10) . ? B N1 1.555(10) . ? B N3 1.565(10) . ? N1 C3 1.351(9) . ? N1 N2 1.368(9) . ? N2 C1 1.327(9) . ? C1 C2 1.389(12) . ? C1 C4 1.487(12) . ? C2 C3 1.381(11) . ? C3 C5 1.463(13) . ? N3 C8 1.353(9) . ? N3 N4 1.361(9) . ? N4 C6 1.330(8) . ? C6 C7 1.397(11) . ? C6 C9 1.463(11) . ? C7 C8 1.396(11) . ? C8 C10 1.495(11) . ? N5 C13 1.357(9) . ? N5 N6 1.362(9) . ? N6 C11 1.330(9) . ? C11 C12 1.378(11) . ? C11 C14 1.484(12) . ? C12 C13 1.366(12) . ? C13 C15 1.497(13) . ? 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 Tl N6 73.9(2) . . ? N4 Tl N2 75.67(18) . . ? N6 Tl N2 74.39(19) . . ? N5 B N1 111.2(6) . . ? N5 B N3 110.8(6) . . ? N1 B N3 109.2(6) . . ? C3 N1 N2 110.2(6) . . ? C3 N1 B 129.7(7) . . ? N2 N1 B 120.0(6) . . ? C1 N2 N1 106.7(6) . . ? C1 N2 Tl 130.1(5) . . ? N1 N2 Tl 123.2(4) . . ? N2 C1 C2 109.9(7) . . ? N2 C1 C4 120.2(8) . . ? C2 C1 C4 129.8(7) . . ? C3 C2 C1 106.3(7) . . ? N1 C3 C2 106.9(7) . . ? N1 C3 C5 123.9(7) . . ? C2 C3 C5 129.1(8) . . ? C8 N3 N4 110.8(6) . . ? C8 N3 B 128.3(7) . . ? N4 N3 B 120.8(5) . . ? C6 N4 N3 107.1(6) . . ? C6 N4 Tl 128.8(5) . . ? N3 N4 Tl 123.0(4) . . ? N4 C6 C7 109.7(7) . . ? N4 C6 C9 120.6(7) . . ? C7 C6 C9 129.7(6) . . ? C8 C7 C6 106.1(6) . . ? N3 C8 C7 106.3(7) . . ? N3 C8 C10 124.2(7) . . ? C7 C8 C10 129.5(7) . . ? C13 N5 N6 108.4(6) . . ? C13 N5 B 129.8(7) . . ? N6 N5 B 121.6(6) . . ? C11 N6 N5 107.4(6) . . ? C11 N6 Tl 129.8(6) . . ? N5 N6 Tl 122.8(4) . . ? N6 C11 C12 110.0(8) . . ? N6 C11 C14 119.1(8) . . ? C12 C11 C14 130.9(8) . . ? C13 C12 C11 105.8(7) . . ? N5 C13 C12 108.4(7) . . ? N5 C13 C15 124.1(8) . . ? C12 C13 C15 127.5(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.350 _refine_diff_density_min -2.862 _refine_diff_density_rms 0.190 #=END