Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Xue, Ziling' 'Cai, Hu' 'Chen, Tianniu' 'Koetzie, Thomas E.' 'Schultz, Arthur J.' 'Wang, Xiao-ping' _publ_contact_author_name ; Dr Ziling `Xue ; _publ_contact_author_address ; Department of Chemistry The University of Tennessee Knoxville TN 37996 UNITED STATES OF AMERICA ; _publ_contact_author_email 'XUE@NOVELL.CHEM.UTK.EDU' _publ_section_title ; Direct observation of n2-imine of formation through B-H abstraction between amide ligands. Neutron and X-ray diffraction structure of a dihydride imine ditantatalum complex ; data_ta2patt2 _database_code_CSD 173742 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H43 N7 Ta2' _chemical_formula_weight 671.45 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' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.004(4) _cell_length_b 11.211(4) _cell_length_c 15.801(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.866(5) _cell_angle_gamma 90.00 _cell_volume 2287.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 172(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 9.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3278 _exptl_absorpt_correction_T_max 0.4796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 172(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13943 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0479 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.36 _reflns_number_total 3306 _reflns_number_gt 2516 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0344P)^2^+4.8081P] 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 3306 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.713 _refine_ls_shift/su_mean 0.005 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 Ta2 Ta 0.79782(2) 0.12446(2) 0.196283(16) 0.01829(11) Uani 1 1 d . . . Ta1 Ta 0.723843(19) -0.12776(2) 0.219048(16) 0.01832(11) Uani 1 1 d . . . N2 N 0.6964(4) -0.1148(5) 0.3429(4) 0.0228(13) Uani 1 1 d . . . N7 N 0.7899(4) -0.0277(5) 0.1162(3) 0.0188(12) Uani 1 1 d . . . N4 N 0.9186(4) 0.1769(5) 0.1392(3) 0.0209(13) Uani 1 1 d . . . N1 N 0.5873(4) -0.1545(5) 0.1472(4) 0.0245(14) Uani 1 1 d . . . C8 C 0.9735(5) 0.1207(6) 0.0740(4) 0.0295(17) Uani 1 1 d . . . H8A H 0.9635 0.1683 0.0216 0.044 Uiso 1 1 calc R . . H8B H 0.9462 0.0402 0.0622 0.044 Uiso 1 1 calc R . . H8C H 1.0476 0.1161 0.0944 0.044 Uiso 1 1 calc R . . N3 N 0.7526(4) -0.3051(5) 0.2393(4) 0.0265(14) Uani 1 1 d . . . C14 C 0.8455(5) -0.1385(6) 0.1334(4) 0.0228(16) Uani 1 1 d . . . H14A H 0.9179 -0.1318 0.1606 0.027 Uiso 1 1 calc R . . H14B H 0.8359 -0.1999 0.0881 0.027 Uiso 1 1 calc R . . N6 N 0.8383(4) 0.1914(5) 0.3127(4) 0.0225(13) Uani 1 1 d . . . N5 N 0.6881(4) 0.2390(5) 0.1492(4) 0.0249(14) Uani 1 1 d . . . C13 C 0.9075(6) 0.1386(7) 0.3821(5) 0.0324(18) Uani 1 1 d . . . H13A H 0.9677 0.1907 0.3962 0.049 Uiso 1 1 calc R . . H13B H 0.9309 0.0603 0.3644 0.049 Uiso 1 1 calc R . . H13C H 0.8707 0.1294 0.4323 0.049 Uiso 1 1 calc R . . C2 C 0.7633(6) -0.1664(7) 0.4142(5) 0.0350(19) Uani 1 1 d . . . H2A H 0.8113 -0.1054 0.4398 0.053 Uiso 1 1 calc R . . H2B H 0.8027 -0.2327 0.3937 0.053 Uiso 1 1 calc R . . H2C H 0.7208 -0.1958 0.4570 0.053 Uiso 1 1 calc R . . C3 C 0.6803(6) -0.3775(7) 0.2816(6) 0.042(2) Uani 1 1 d . . . H3A H 0.6399 -0.4284 0.2395 0.063 Uiso 1 1 calc R . . H3B H 0.6333 -0.3251 0.3085 0.063 Uiso 1 1 calc R . . H3C H 0.7191 -0.4276 0.3252 0.063 Uiso 1 1 calc R . . C4 C 0.8290(6) -0.3838(7) 0.2097(5) 0.0362(19) Uani 1 1 d . . . H4A H 0.8620 -0.4310 0.2576 0.054 Uiso 1 1 calc R . . H4B H 0.8815 -0.3364 0.1854 0.054 Uiso 1 1 calc R . . H4C H 0.7950 -0.4374 0.1660 0.054 Uiso 1 1 calc R . . C9 C 0.9654(6) 0.2942(6) 0.1612(5) 0.0327(18) Uani 1 1 d . . . H9A H 1.0376 0.2835 0.1857 0.049 Uiso 1 1 calc R . . H9B H 0.9268 0.3339 0.2028 0.049 Uiso 1 1 calc R . . H9C H 0.9629 0.3433 0.1096 0.049 Uiso 1 1 calc R . . C10 C 0.6965(6) 0.3166(6) 0.0770(5) 0.0324(18) Uani 1 1 d . . . H10A H 0.6464 0.2917 0.0290 0.049 Uiso 1 1 calc R . . H10B H 0.7667 0.3114 0.0606 0.049 Uiso 1 1 calc R . . H10C H 0.6822 0.3990 0.0926 0.049 Uiso 1 1 calc R . . C1 C 0.6315(6) -0.0241(6) 0.3760(5) 0.0314(18) Uani 1 1 d . . . H1A H 0.5982 -0.0575 0.4231 0.047 Uiso 1 1 calc R . . H1B H 0.5783 0.0019 0.3305 0.047 Uiso 1 1 calc R . . H1C H 0.6744 0.0443 0.3965 0.047 Uiso 1 1 calc R . . C6 C 0.5003(6) -0.0719(7) 0.1342(5) 0.039(2) Uani 1 1 d . . . H6A H 0.4971 -0.0367 0.0772 0.058 Uiso 1 1 calc R . . H6B H 0.5097 -0.0085 0.1772 0.058 Uiso 1 1 calc R . . H6C H 0.4358 -0.1149 0.1395 0.058 Uiso 1 1 calc R . . C12 C 0.8011(6) 0.3072(6) 0.3413(5) 0.038(2) Uani 1 1 d . . . H12A H 0.7646 0.2951 0.3914 0.057 Uiso 1 1 calc R . . H12B H 0.7537 0.3430 0.2953 0.057 Uiso 1 1 calc R . . H12C H 0.8602 0.3605 0.3561 0.057 Uiso 1 1 calc R . . C7 C 0.7307(5) -0.0162(6) 0.0299(4) 0.0278(17) Uani 1 1 d . . . H7A H 0.7782 0.0053 -0.0114 0.042 Uiso 1 1 calc R . . H7B H 0.6780 0.0461 0.0309 0.042 Uiso 1 1 calc R . . H7C H 0.6971 -0.0923 0.0134 0.042 Uiso 1 1 calc R . . C11 C 0.5864(6) 0.2548(7) 0.1775(5) 0.039(2) Uani 1 1 d . . . H11A H 0.5740 0.3398 0.1863 0.059 Uiso 1 1 calc R . . H11B H 0.5837 0.2116 0.2311 0.059 Uiso 1 1 calc R . . H11C H 0.5332 0.2235 0.1340 0.059 Uiso 1 1 calc R . . C5 C 0.5660(6) -0.2572(7) 0.0912(5) 0.042(2) Uani 1 1 d . . . H5A H 0.5005 -0.2941 0.1019 0.063 Uiso 1 1 calc R . . H5B H 0.6222 -0.3154 0.1023 0.063 Uiso 1 1 calc R . . H5C H 0.5611 -0.2311 0.0316 0.063 Uiso 1 1 calc R . . H30 H 0.831(4) -0.020(5) 0.267(3) 0.006(14) Uiso 1 1 d . . . H20 H 0.665(4) 0.033(5) 0.223(3) 0.000(13) Uiso 1 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 Ta2 0.02271(18) 0.01646(17) 0.01565(17) -0.00021(12) 0.00203(12) -0.00058(12) Ta1 0.02136(18) 0.01652(17) 0.01712(18) 0.00009(12) 0.00245(12) -0.00010(12) N2 0.027(3) 0.020(3) 0.022(3) 0.002(3) 0.008(2) 0.002(3) N7 0.024(3) 0.014(3) 0.018(3) -0.001(2) 0.005(2) -0.001(2) N4 0.026(3) 0.021(3) 0.016(3) -0.004(2) 0.003(2) -0.005(3) N1 0.022(3) 0.023(3) 0.028(3) -0.005(3) 0.004(3) -0.005(3) C8 0.032(4) 0.037(4) 0.022(4) 0.005(3) 0.010(3) 0.000(4) N3 0.027(3) 0.022(3) 0.033(4) 0.000(3) 0.013(3) 0.002(3) C14 0.020(4) 0.023(4) 0.026(4) -0.013(3) 0.003(3) -0.002(3) N6 0.027(3) 0.020(3) 0.022(3) 0.000(2) 0.009(3) 0.000(3) N5 0.025(3) 0.018(3) 0.031(4) 0.006(3) 0.001(3) 0.001(3) C13 0.040(5) 0.033(4) 0.023(4) -0.002(3) -0.002(3) 0.002(4) C2 0.050(5) 0.034(4) 0.021(4) 0.009(3) 0.007(4) 0.008(4) C3 0.046(5) 0.031(4) 0.051(5) 0.008(4) 0.019(4) -0.002(4) C4 0.034(4) 0.024(4) 0.050(5) -0.005(4) 0.002(4) -0.005(4) C9 0.034(5) 0.031(4) 0.033(5) -0.002(3) 0.008(4) -0.009(4) C10 0.044(5) 0.028(4) 0.026(4) 0.010(3) 0.004(4) 0.000(4) C1 0.037(4) 0.029(4) 0.029(4) 0.000(3) 0.011(3) 0.004(4) C6 0.026(4) 0.037(5) 0.050(5) 0.009(4) -0.008(4) -0.001(4) C12 0.053(5) 0.022(4) 0.036(5) -0.010(4) -0.003(4) -0.002(4) C7 0.040(4) 0.023(4) 0.020(4) 0.004(3) -0.001(3) -0.004(3) C11 0.033(5) 0.033(4) 0.052(6) 0.006(4) 0.006(4) 0.012(4) C5 0.037(5) 0.047(5) 0.039(5) -0.013(4) -0.005(4) -0.008(4) _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 Ta2 N4 1.991(6) . ? Ta2 N6 1.998(6) . ? Ta2 N5 1.996(5) . ? Ta2 N7 2.120(5) . ? Ta2 Ta1 3.0221(10) . ? Ta2 H30 1.99(5) . ? Ta2 H20 2.09(5) . ? Ta1 N1 2.013(5) . ? Ta1 N2 2.036(6) . ? Ta1 N3 2.041(6) . ? Ta1 C14 2.205(7) . ? Ta1 N7 2.229(5) . ? Ta1 H30 1.93(5) . ? Ta1 H20 1.96(5) . ? N2 C1 1.457(8) . ? N2 C2 1.458(9) . ? N7 C14 1.446(8) . ? N7 C7 1.489(8) . ? N4 C8 1.465(8) . ? N4 C9 1.473(8) . ? N1 C5 1.458(9) . ? N1 C6 1.457(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? N3 C4 1.448(9) . ? N3 C3 1.464(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? N6 C13 1.458(9) . ? N6 C12 1.476(9) . ? N5 C10 1.448(8) . ? N5 C11 1.457(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ta2 N6 99.8(2) . . ? N4 Ta2 N5 102.0(2) . . ? N6 Ta2 N5 101.5(2) . . ? N4 Ta2 N7 87.2(2) . . ? N6 Ta2 N7 147.2(2) . . ? N5 Ta2 N7 108.3(2) . . ? N4 Ta2 Ta1 127.57(15) . . ? N6 Ta2 Ta1 107.12(15) . . ? N5 Ta2 Ta1 115.03(16) . . ? N7 Ta2 Ta1 47.50(14) . . ? N4 Ta2 H30 111.4(14) . . ? N6 Ta2 H30 77.0(16) . . ? N5 Ta2 H30 146.4(14) . . ? N7 Ta2 H30 70.6(16) . . ? Ta1 Ta2 H30 38.7(15) . . ? N4 Ta2 H20 161.6(14) . . ? N6 Ta2 H20 97.7(14) . . ? N5 Ta2 H20 79.7(14) . . ? N7 Ta2 H20 74.9(14) . . ? Ta1 Ta2 H20 40.0(14) . . ? H30 Ta2 H20 67(2) . . ? N1 Ta1 N2 108.0(2) . . ? N1 Ta1 N3 94.4(2) . . ? N2 Ta1 N3 88.2(2) . . ? N1 Ta1 C14 107.2(2) . . ? N2 Ta1 C14 144.6(2) . . ? N3 Ta1 C14 84.9(2) . . ? N1 Ta1 N7 93.1(2) . . ? N2 Ta1 N7 142.4(2) . . ? N3 Ta1 N7 121.7(2) . . ? C14 Ta1 N7 38.1(2) . . ? N1 Ta1 Ta2 110.13(16) . . ? N2 Ta1 Ta2 98.18(15) . . ? N3 Ta1 Ta2 151.04(16) . . ? C14 Ta1 Ta2 73.50(17) . . ? N7 Ta1 Ta2 44.51(13) . . ? N1 Ta1 H30 149.6(16) . . ? N2 Ta1 H30 77.4(16) . . ? N3 Ta1 H30 115.9(15) . . ? C14 Ta1 H30 74.6(15) . . ? N7 Ta1 H30 69.3(16) . . ? Ta2 Ta1 H30 40.2(16) . . ? N1 Ta1 H20 80.3(14) . . ? N2 Ta1 H20 78.1(15) . . ? N3 Ta1 H20 162.8(14) . . ? C14 Ta1 H20 112.2(14) . . ? N7 Ta1 H20 75.2(15) . . ? Ta2 Ta1 H20 43.5(14) . . ? H30 Ta1 H20 71(2) . . ? C1 N2 C2 108.5(6) . . ? C1 N2 Ta1 124.7(4) . . ? C2 N2 Ta1 123.9(4) . . ? C14 N7 C7 116.0(5) . . ? C14 N7 Ta2 126.3(4) . . ? C7 N7 Ta2 117.4(4) . . ? C14 N7 Ta1 70.0(3) . . ? C7 N7 Ta1 120.6(4) . . ? Ta2 N7 Ta1 88.00(19) . . ? C8 N4 C9 109.1(5) . . ? C8 N4 Ta2 132.0(4) . . ? C9 N4 Ta2 118.9(4) . . ? C5 N1 C6 109.2(6) . . ? C5 N1 Ta1 123.4(5) . . ? C6 N1 Ta1 127.0(5) . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 N3 C3 108.2(6) . . ? C4 N3 Ta1 131.5(5) . . ? C3 N3 Ta1 119.7(5) . . ? N7 C14 Ta1 71.9(3) . . ? N7 C14 H14A 116.4 . . ? Ta1 C14 H14A 116.4 . . ? N7 C14 H14B 116.4 . . ? Ta1 C14 H14B 116.4 . . ? H14A C14 H14B 113.4 . . ? C13 N6 C12 108.8(6) . . ? C13 N6 Ta2 127.7(4) . . ? C12 N6 Ta2 123.5(5) . . ? C10 N5 C11 109.0(6) . . ? C10 N5 Ta2 124.2(5) . . ? C11 N5 Ta2 126.7(5) . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N5 C11 H11A 109.5 . . ? N5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.36 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.002 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.154 #========================================================================== data_taa _database_code_CSD 173743 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H43 N7 Ta2' _chemical_formula_weight 671.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ta' 'Ta' -0.7052 6.5227 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorombic _symmetry_space_group_name_H-M Pbca 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' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.8544(6) _cell_length_b 16.5918(7) _cell_length_c 19.2122(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4735.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 9.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1158 _exptl_absorpt_correction_T_max 0.4033 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44653 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4858 _reflns_number_gt 4032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+50.9797P] 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 4858 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.003 _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 N6 N 0.1252(5) 0.7167(4) 0.2389(3) 0.0403(17) Uani 1 1 d . . . Ta1 Ta 0.225995(16) 0.864893(15) 0.083967(13) 0.01750(7) Uani 1 1 d . . . Ta2 Ta 0.105838(18) 0.830350(16) 0.207713(14) 0.02283(8) Uani 1 1 d . . . N7 N 0.1453(3) 0.9388(3) 0.1582(3) 0.0200(11) Uani 1 1 d . . . N4 N 0.1220(4) 0.8846(4) 0.3000(3) 0.0351(15) Uani 1 1 d . . . N3 N 0.3432(4) 0.9065(4) 0.0446(3) 0.0304(13) Uani 1 1 d . . . N2 N 0.2732(4) 0.7516(4) 0.0685(3) 0.0333(14) Uani 1 1 d . . . N1 N 0.1544(4) 0.8981(3) -0.0009(3) 0.0267(12) Uani 1 1 d . . . N5 N -0.0248(4) 0.8334(4) 0.1874(3) 0.0377(16) Uani 1 1 d . . . C14 C 0.2373(4) 0.9678(4) 0.1548(4) 0.0245(14) Uani 1 1 d . . . H14A H 0.2738 0.9597 0.1961 0.029 Uiso 1 1 calc R . . H14B H 0.2462 1.0201 0.1333 0.029 Uiso 1 1 calc R . . C5 C 0.1734(6) 0.9710(5) -0.0398(4) 0.0404(19) Uani 1 1 d . . . H5A H 0.1668 0.9605 -0.0886 0.061 Uiso 1 1 calc R . . H5B H 0.2339 0.9882 -0.0304 0.061 Uiso 1 1 calc R . . H5C H 0.1321 1.0126 -0.0261 0.061 Uiso 1 1 calc R . . C6 C 0.0709(5) 0.8616(5) -0.0252(4) 0.0368(18) Uani 1 1 d . . . H6A H 0.0206 0.8907 -0.0064 0.055 Uiso 1 1 calc R . . H6B H 0.0682 0.8065 -0.0101 0.055 Uiso 1 1 calc R . . H6C H 0.0688 0.8636 -0.0751 0.055 Uiso 1 1 calc R . . C7 C 0.0780(5) 0.9954(4) 0.1310(4) 0.0342(17) Uani 1 1 d . . . H7A H 0.0583 1.0304 0.1678 0.051 Uiso 1 1 calc R . . H7B H 0.0275 0.9659 0.1131 0.051 Uiso 1 1 calc R . . H7C H 0.1043 1.0270 0.0944 0.051 Uiso 1 1 calc R . . C1 C 0.2161(6) 0.6824(4) 0.0543(5) 0.042(2) Uani 1 1 d . . . H1A H 0.2480 0.6448 0.0253 0.063 Uiso 1 1 calc R . . H1B H 0.1625 0.6999 0.0308 0.063 Uiso 1 1 calc R . . H1C H 0.2001 0.6567 0.0973 0.063 Uiso 1 1 calc R . . C4 C 0.4005(5) 0.9741(5) 0.0642(5) 0.041(2) Uani 1 1 d . . . H4A H 0.4625 0.9591 0.0585 0.061 Uiso 1 1 calc R . . H4B H 0.3896 0.9881 0.1119 0.061 Uiso 1 1 calc R . . H4C H 0.3873 1.0195 0.0350 0.061 Uiso 1 1 calc R . . C3 C 0.3766(6) 0.8731(5) -0.0229(5) 0.051(2) Uani 1 1 d . . . H3A H 0.3737 0.9140 -0.0581 0.076 Uiso 1 1 calc R . . H3B H 0.3398 0.8282 -0.0364 0.076 Uiso 1 1 calc R . . H3C H 0.4378 0.8555 -0.0175 0.076 Uiso 1 1 calc R . . C2 C 0.3611(5) 0.7255(5) 0.0925(5) 0.046(2) Uani 1 1 d . . . H2A H 0.3539 0.6852 0.1279 0.070 Uiso 1 1 calc R . . H2B H 0.3932 0.7708 0.1113 0.070 Uiso 1 1 calc R . . H2C H 0.3943 0.7034 0.0542 0.070 Uiso 1 1 calc R . . C13 C 0.2111(7) 0.6809(5) 0.2599(5) 0.055(3) Uani 1 1 d . . . H13A H 0.2068 0.6622 0.3071 0.083 Uiso 1 1 calc R . . H13B H 0.2579 0.7206 0.2565 0.083 Uiso 1 1 calc R . . H13C H 0.2249 0.6363 0.2299 0.083 Uiso 1 1 calc R . . C11 C -0.0718(6) 0.8004(6) 0.1273(5) 0.053(2) Uani 1 1 d . . . H11A H -0.1245 0.7720 0.1426 0.080 Uiso 1 1 calc R . . H11B H -0.0327 0.7640 0.1030 0.080 Uiso 1 1 calc R . . H11C H -0.0891 0.8435 0.0968 0.080 Uiso 1 1 calc R . . C8 C 0.1334(7) 0.9705(5) 0.3142(4) 0.049(2) Uani 1 1 d . . . H8A H 0.0867 0.9884 0.3450 0.074 Uiso 1 1 calc R . . H8B H 0.1301 1.0001 0.2714 0.074 Uiso 1 1 calc R . . H8C H 0.1910 0.9794 0.3355 0.074 Uiso 1 1 calc R . . C12 C 0.0554(8) 0.6547(5) 0.2399(6) 0.068(3) Uani 1 1 d . . . H12A H 0.0527 0.6289 0.1952 0.102 Uiso 1 1 calc R . . H12B H -0.0017 0.6791 0.2501 0.102 Uiso 1 1 calc R . . H12C H 0.0694 0.6155 0.2749 0.102 Uiso 1 1 calc R . . C10 C -0.0897(6) 0.8803(7) 0.2291(6) 0.066(3) Uani 1 1 d . . . H10A H -0.1027 0.9302 0.2059 0.098 Uiso 1 1 calc R . . H10B H -0.0644 0.8913 0.2741 0.098 Uiso 1 1 calc R . . H10C H -0.1443 0.8499 0.2344 0.098 Uiso 1 1 calc R . . C9 C 0.1285(9) 0.8396(7) 0.3646(5) 0.072(3) Uani 1 1 d . . . H9A H 0.1866 0.8145 0.3676 0.107 Uiso 1 1 calc R . . H9B H 0.0825 0.7990 0.3658 0.107 Uiso 1 1 calc R . . H9C H 0.1207 0.8756 0.4033 0.107 Uiso 1 1 calc R . . H20 H 0.130(4) 0.804(4) 0.128(3) 0.010(15) Uiso 1 1 d . . . H30 H 0.224(4) 0.822(3) 0.167(3) 0.009(15) Uiso 1 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 N6 0.062(5) 0.024(3) 0.035(4) 0.006(3) 0.015(3) -0.010(3) Ta1 0.01636(12) 0.01551(13) 0.02063(13) 0.00081(10) 0.00206(10) 0.00120(10) Ta2 0.02468(14) 0.02305(14) 0.02076(14) -0.00223(11) 0.00483(11) -0.00593(11) N7 0.020(3) 0.018(3) 0.021(3) -0.004(2) -0.002(2) 0.001(2) N4 0.045(4) 0.039(4) 0.021(3) -0.009(3) 0.003(3) -0.004(3) N3 0.026(3) 0.033(3) 0.033(3) 0.007(3) 0.008(3) 0.002(3) N2 0.042(4) 0.021(3) 0.038(4) -0.002(3) 0.009(3) 0.009(3) N1 0.026(3) 0.027(3) 0.027(3) 0.004(3) -0.001(2) 0.001(2) N5 0.027(3) 0.051(4) 0.034(4) -0.011(3) 0.009(3) -0.011(3) C14 0.020(3) 0.023(3) 0.030(4) -0.001(3) -0.001(3) -0.002(3) C5 0.045(5) 0.045(5) 0.031(4) 0.019(4) -0.007(4) -0.004(4) C6 0.033(4) 0.046(5) 0.031(4) -0.006(3) -0.007(3) -0.004(4) C7 0.033(4) 0.026(4) 0.044(4) -0.001(3) 0.004(3) 0.014(3) C1 0.054(5) 0.022(4) 0.050(5) -0.008(3) 0.000(4) 0.007(4) C4 0.024(4) 0.033(4) 0.065(6) 0.006(4) 0.009(4) -0.005(3) C3 0.052(5) 0.038(5) 0.062(6) -0.002(4) 0.035(5) 0.003(4) C2 0.038(4) 0.039(5) 0.063(6) 0.008(4) 0.006(4) 0.020(4) C13 0.080(7) 0.030(4) 0.056(6) 0.017(4) -0.006(5) 0.007(5) C11 0.034(4) 0.080(7) 0.046(5) -0.014(5) 0.000(4) -0.018(5) C8 0.067(6) 0.046(5) 0.035(5) -0.013(4) 0.008(4) -0.012(5) C12 0.078(7) 0.036(5) 0.089(8) 0.014(5) 0.015(6) -0.019(5) C10 0.038(5) 0.080(7) 0.079(8) -0.030(6) 0.034(5) -0.010(5) C9 0.122(10) 0.065(7) 0.027(5) -0.001(5) 0.000(6) -0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N6 C12 1.460(11) . ? N6 C13 1.465(11) . ? N6 Ta2 1.999(6) . ? Ta1 N3 2.019(6) . ? Ta1 N1 2.022(6) . ? Ta1 N2 2.029(6) . ? Ta1 C14 2.190(7) . ? Ta1 N7 2.229(5) . ? Ta1 Ta2 3.0276(4) . ? Ta1 H20 1.94(6) . ? Ta1 H30 1.74(6) . ? Ta2 N5 1.981(6) . ? Ta2 N4 2.003(6) . ? Ta2 N7 2.118(5) . ? Ta2 H20 1.63(6) . ? Ta2 H30 1.92(6) . ? N7 C14 1.451(8) . ? N7 C7 1.468(8) . ? N4 C9 1.452(11) . ? N4 C8 1.461(10) . ? N3 C4 1.457(10) . ? N3 C3 1.496(10) . ? N2 C2 1.450(10) . ? N2 C1 1.453(10) . ? N1 C5 1.450(9) . ? N1 C6 1.458(9) . ? N5 C11 1.454(10) . ? N5 C10 1.475(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 C12 N6 C13 109.2(7) . . ? C12 N6 Ta2 124.5(6) . . ? C13 N6 Ta2 126.2(5) . . ? N3 Ta1 N1 93.3(2) . . ? N3 Ta1 N2 88.0(2) . . ? N1 Ta1 N2 108.4(2) . . ? N3 Ta1 C14 84.2(2) . . ? N1 Ta1 C14 109.2(2) . . ? N2 Ta1 C14 141.9(3) . . ? N3 Ta1 N7 121.0(2) . . ? N1 Ta1 N7 94.8(2) . . ? N2 Ta1 N7 142.1(2) . . ? C14 Ta1 N7 38.3(2) . . ? N3 Ta1 Ta2 150.09(18) . . ? N1 Ta1 Ta2 111.99(16) . . ? N2 Ta1 Ta2 98.25(17) . . ? C14 Ta1 Ta2 72.84(17) . . ? N7 Ta1 Ta2 44.37(14) . . ? N3 Ta1 H20 167.1(18) . . ? N1 Ta1 H20 96.1(18) . . ? N2 Ta1 H20 80.7(18) . . ? C14 Ta1 H20 100.9(18) . . ? N7 Ta1 H20 67.1(18) . . ? Ta2 Ta1 H20 29.0(18) . . ? N3 Ta1 H30 119.8(19) . . ? N1 Ta1 H30 146.9(19) . . ? N2 Ta1 H30 76.4(19) . . ? C14 Ta1 H30 75.5(19) . . ? N7 Ta1 H30 68.2(19) . . ? Ta2 Ta1 H30 36.4(19) . . ? H20 Ta1 H30 52(3) . . ? N5 Ta2 N6 102.9(3) . . ? N5 Ta2 N4 106.3(3) . . ? N6 Ta2 N4 98.1(3) . . ? N5 Ta2 N7 99.3(2) . . ? N6 Ta2 N7 153.6(2) . . ? N4 Ta2 N7 89.0(2) . . ? N5 Ta2 Ta1 114.71(19) . . ? N6 Ta2 Ta1 109.23(19) . . ? N4 Ta2 Ta1 122.65(19) . . ? N7 Ta2 Ta1 47.39(14) . . ? N5 Ta2 H20 92(2) . . ? N6 Ta2 H20 90(2) . . ? N4 Ta2 H20 157(2) . . ? N7 Ta2 H20 75(2) . . ? Ta1 Ta2 H20 35(2) . . ? N5 Ta2 H30 144.5(18) . . ? N6 Ta2 H30 85.7(17) . . ? N4 Ta2 H30 106.4(18) . . ? N7 Ta2 H30 67.9(17) . . ? Ta1 Ta2 H30 32.5(17) . . ? H20 Ta2 H30 53(3) . . ? C14 N7 C7 114.4(5) . . ? C14 N7 Ta2 124.2(4) . . ? C7 N7 Ta2 121.0(4) . . ? C14 N7 Ta1 69.4(3) . . ? C7 N7 Ta1 119.4(4) . . ? Ta2 N7 Ta1 88.23(19) . . ? C9 N4 C8 109.5(7) . . ? C9 N4 Ta2 122.3(6) . . ? C8 N4 Ta2 128.2(5) . . ? C4 N3 C3 108.4(6) . . ? C4 N3 Ta1 132.1(5) . . ? C3 N3 Ta1 118.9(5) . . ? C2 N2 C1 110.5(6) . . ? C2 N2 Ta1 122.7(5) . . ? C1 N2 Ta1 123.9(5) . . ? C5 N1 C6 110.3(6) . . ? C5 N1 Ta1 122.7(5) . . ? C6 N1 Ta1 126.4(5) . . ? C11 N5 C10 108.4(7) . . ? C11 N5 Ta2 128.1(5) . . ? C10 N5 Ta2 123.1(6) . . ? N7 C14 Ta1 72.3(3) . . ? N7 C14 H14A 116.3 . . ? Ta1 C14 H14A 116.3 . . ? N7 C14 H14B 116.3 . . ? Ta1 C14 H14B 116.3 . . ? H14A C14 H14B 113.3 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C1 H1A 109.5 . . ? N2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N6 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C11 H11A 109.5 . . ? N5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C10 H10A 109.5 . . ? N5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C9 H9A 109.5 . . ? N4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.812 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.197 #============================================================================ data_TaHneutron _database_code_CSD 173744 _audit_creation_method 'manual' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H43 N7 Ta2' _chemical_formula_weight 671.44 _cell_length_a 14.811(3) _cell_length_b 16.555(3) _cell_length_c 18.985(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 4655.0(16) _cell_formula_units_Z 8 _cell_measurement_temperature 20(2) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 2.8 _exptl_crystal_size_mid 1.3 _exptl_crystal_size_min 1.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method ? _exptl_absorpt_coefficient_mu '1.838 + 1.490(\l) cm^-1^' _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.3990 _exptl_absorpt_correction_T_max 0.4396 _exptl_absorpt_process_details 'IPNS ANVRED program' _exptl_special_details ; The atomic and magnetic scattering factors for 4 types of atoms are: Atom b-len a(1) b(1) a(2) b(2) a(3) b(3) a(4) b(4) c H -.374 .4930 10.5109 .3229 26.1257 .1402 3.1424 .0408 57.7997 .0030 N .930 12.2126 .0057 3.1322 9.8933 2.0125 28.9975 1.1663 .5826 -11.5290 C .665 2.3100 20.8439 1.0200 10.2075 1.5886 .5687 .8650 51.6512 .2156 TA .691 29.2024 1.7733 15.2293 9.3705 14.5135 .2960 4.7649 63.3644 9.2435 ; _diffrn_ambient_temperature 20(2) _diffrn_radiation_wavelength '0.7-4.2' _diffrn_radiation_type neutrons _diffrn_radiation_source 'pulsed spallation source at IPNS' _diffrn_measurement_device_type 'IPNS Single Crystal Diffractometer' _diffrn_measurement_method 'time of flight Laue' _diffrn_reflns_number 2775 _diffrn_reflns_av_R_equivalents 0.1324 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 30 _reflns_number_total 2775 _reflns_number_gt 2775 _reflns_threshold_expression >3sigma(I) _computing_data_collection 'IPNS data aquisition software' _computing_cell_refinement 'LATCON (Argonne Programs)' _computing_data_reduction 'ANVRED (Argonne Programs)' _computing_structure_solution 'from x-ray structure' _computing_structure_refinement 'GSAS(Larson & Von Dreele, 2000)' _computing_molecular_graphics 'ORTEP (Burnett & Johnson 1996)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; SigmaFoSq = SigmaFoSq + (.002*FoSq)^2^ Wght = 1.0/(SigmaFoSq)^2^ All single crystal weights were scaled by Min(Fo/Fc,Fc/Fo)^4^ ; _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 2775 _refine_ls_number_parameters 461 _refine_ls_number_restraints 6 _refine_ls_R_factor 0.101 _refine_ls_wR_factor 0.057 _refine_ls_goodness_of_fit 1.90 _refine_ls_shift/esd_max 0.01 _refine_ls_shift/esd_mean 0.00 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity TA1 .22797(27) .86470(25) .08447(20) 1.0 Uiso .0025(5) 8 TA2 .10400(24) .83093(24) .20808(20) 1.0 Uiso .0004(5) 8 H20 .1169(7) .8019(5) .1076(5) 1.0 Uani .01772 8 H30 .2285(7) .8217(7) .1805(5) 1.0 Uani .02888 8 N1 .15647(21) .89724(20) -.00217(18) 1.0 Uiso .0100(7) 8 N2 .27680(22) .75144(21) .06944(17) 1.0 Uiso .0117(7) 8 N3 .34773(22) .90754(20) .04476(17) 1.0 Uiso .0093(7) 8 N4 .12123(23) .88762(20) .30147(17) 1.0 Uiso .0128(7) 8 N5 -.02784(21) .83475(21) .18751(18) 1.0 Uiso .0117(7) 8 N6 .12422(22) .71792(20) .24084(17) 1.0 Uiso .0114(7) 8 N7 .14422(21) .94038(19) .15589(17) 1.0 Uiso .0078(7) 8 C1 .22025(28) .68146(26) .05505(21) 1.0 Uiso .0122(10) 8 H1A .2562(6) .6379(5) .0224(5) 1.0 Uani .03817 8 H1B .1590(6) .6996(6) .0275(7) 1.0 Uani .04484 8 H1C .1978(8) .6526(6) .10360(34) 1.0 Uani .03784 8 C2 .36441(30) .72473(25) .09740(22) 1.0 Uiso .0164(12) 8 H2A .3969(7) .6856(7) .0588(5) 1.0 Uani .0409 8 H2B .3563(7) .6913(7) .1465(4) 1.0 Uani .03712 8 H2C .4085(6) .7766(4) .1054(7) 1.0 Uani .03651 8 C3 .38393(26) .87191(25) -.01931(22) 1.0 Uiso .0110(10) 8 H3A .4537(4) .8525(7) -.0121(6) 1.0 Uani .03429 8 H3B .3876(8) .9151(6) -.0626(4) 1.0 Uani .04122 8 H3C .3454(7) .8187(5) -.0349(5) 1.0 Uani .03338 8 C4 .40181(28) .97747(28) .06405(22) 1.0 Uiso .0145(11) 8 H4A .47395(31) .9646(7) .0623(6) 1.0 Uani .03732 8 H4B .3887(8) 1.0004(6) .11689(34) 1.0 Uani .04041 8 H4C .3920(9) 1.0274(5) .0274(5) 1.0 Uani .04545 8 C5 .17493(25) .97143(29) -.04261(21) 1.0 Uiso .0118(10) 8 H5A .1768(8) .9598(7) -.09910(23) 1.0 Uani .03668 8 H5B .2397(4) .9976(6) -.0279(6) 1.0 Uani .03634 8 H5C .1220(6) 1.0166(5) -.0364(6) 1.0 Uani .03371 8 C6 .07251(30) .86149(26) -.02677(21) 1.0 Uiso .0154(12) 8 H6A .0728(7) .8516(6) -.08354(23) 1.0 Uani .02568 8 H6B .0148(5) .9003(6) -.0156(6) 1.0 Uani .03771 8 H6C .0611(7) .8019(4) -.0040(6) 1.0 Uani .03371 8 C7 .07602(28) .99588(25) .12717(21) 1.0 Uiso .0107(10) 8 H7A .0502(7) 1.0357(6) .1682(4) 1.0 Uani .03985 8 H7B .0165(6) .9644(7) .1076(6) 1.0 Uani .04665 8 H7C .1048(7) 1.0309(7) .0840(5) 1.0 Uani .0418 8 C8 .13005(26) .97448(27) .31344(20) 1.0 Uiso .0132(10) 8 H8A .1933(5) .9866(6) .3409(6) 1.0 Uani .0401 8 H8B .0752(7) .9971(6) .3462(6) 1.0 Uani .04214 8 H8C .1278(8) 1.0075(5) .26382(31) 1.0 Uani .03139 8 C9 .12963(28) .84526(26) .36857(25) 1.0 Uiso .0168(11) 8 H9A .0777(6) .8636(7) .4060(4) 1.0 Uani .04366 8 H9B .1944(5) .8603(7) .3924(6) 1.0 Uani .04043 8 H9C .1208(9) .78031(28) .3621(6) 1.0 Uani .04616 8 C10 -.09007(27) .88218(27) .23022(22) 1.0 Uiso .0171(12) 8 H10A -.1184(8) .9318(6) .1997(6) 1.0 Uani .05236 8 H10B -.0576(6) .9097(6) .2758(4) 1.0 Uani .03431 8 H10C -.1474(5) .8461(6) .2478(7) 1.0 Uani .04435 8 C11 -.07438(29) .80114(25) .12730(24) 1.0 Uiso .0168(12) 8 H11A -.1320(5) .7650(6) .1441(6) 1.0 Uani .03876 8 H11B -.0294(5) .7648(6) .0947(5) 1.0 Uani .03254 8 H11C -.1024(7) .8485(5) .0939(5) 1.0 Uani .04077 8 C12 .05523(30) .65597(28) .23926(23) 1.0 Uiso .0197(12) 8 H12A .0525(8) .6278(7) .2911(4) 1.0 Uani .04192 8 H12B .0756(9) .6082(6) .2030(6) 1.0 Uani .05137 8 H12C -.0105(4) .6811(5) .2256(6) 1.0 Uani .03766 8 C13 .21098(30) .68161(25) .26263(21) 1.0 Uiso .0161(11) 8 H13A .2295(8) .6307(5) .2292(5) 1.0 Uani .04337 8 H13B .2078(8) .6567(7) .31572(33) 1.0 Uani .04204 8 H13C .2609(6) .7300(5) .2616(6) 1.0 Uani .04917 8 C14 .23611(29) .97108(25) .15563(21) 1.0 Uiso .0128(11) 8 H14A .2725(5) .9681(6) .20548(29) 1.0 Uani .02062 8 H14B .2406(6) 1.02938(35) .1292(5) 1.0 Uani .02062 8 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 H20 .024(5) .011(5) .019(5) -.004(4) .000(4) -.004(4) H30 .035(6) .035(6) .017(5) -.002(5) -.008(5) .008(5) H1A .038(6) .025(6) .052(7) -.006(5) -.002(6) -.013(6) H1B .028(6) .023(6) .084(10) .011(5) -.033(6) -.006(7) H1C .066(8) .031(7) .016(5) -.025(6) .000(6) .004(5) H2A .031(6) .043(7) .049(7) .018(6) .007(6) -.007(7) H2B .025(5) .055(7) .031(6) .009(5) -.002(5) .035(6) H2C .030(6) .019(6) .061(8) .012(5) -.003(6) .005(6) H3A .017(5) .054(8) .032(6) .021(5) .007(5) -.001(6) H3B .048(7) .045(7) .031(6) -.002(6) .029(6) .006(6) H3C .033(6) .046(7) .021(6) -.009(6) .005(5) -.009(6) H4A .024(6) .037(7) .051(7) .005(5) .004(5) -.034(6) H4B .051(7) .021(6) .049(8) .001(5) .030(6) -.024(6) H4C .067(8) .034(7) .036(7) -.009(7) .003(6) .017(6) H5A .043(7) .043(7) .024(6) .006(6) -.007(5) .011(6) H5B .032(6) .033(6) .045(7) -.015(5) -.008(5) -.004(6) H5C .039(6) .025(6) .037(7) .007(5) .002(6) .007(5) H6A .029(5) .024(6) .024(6) -.013(5) -.015(5) .004(5) H6B .021(6) .039(7) .054(8) .002(5) -.006(5) -.022(7) H6C .058(7) .010(6) .033(6) .007(5) -.014(6) .012(5) H7A .038(6) .049(8) .033(6) .033(6) .002(5) .000(6) H7B .049(7) .064(9) .027(6) -.019(7) -.034(6) .012(7) H7C .023(6) .048(7) .054(8) .000(6) -.001(6) .014(7) H8A .037(6) .028(6) .055(8) -.007(5) -.021(6) -.005(6) H8B .065(8) .009(5) .053(8) .006(5) .038(7) -.005(6) H8C .065(7) .026(6) .003(4) -.012(5) -.005(5) .006(4) H9A .089(10) .036(7) .006(5) .004(7) -.002(6) -.003(5) H9B .031(6) .051(8) .039(7) -.005(6) -.028(5) -.006(6) H9C .081(9) .016(5) .041(7) -.002(6) -.004(7) .005(6) H10A .0331(34) .047(4) .077(4) .0323(31) .0067(29) -.015(4) H10B .0256(34) .048(4) .030(4) -.0074(31) -.0230(29) -.001(4) H10C .0359(34) .044(4) .053(4) -.0012(31) .0335(29) -.007(4) H11A .011(5) .058(8) .047(7) -.007(5) -.004(5) -.011(7) H11B .028(6) .055(8) .014(5) .001(6) .006(5) -.012(6) H11C .026(6) .058(8) .039(7) -.007(6) -.014(5) .011(7) H12A .043(4) .038(4) .045(5) -.0059(31) .0077(34) .008(4) H12B .054(4) .042(4) .058(5) .0052(31) .0145(34) -.009(4) H12C .030(4) .014(4) .068(5) -.0117(31) .0041(34) .001(4) H13A .067(8) .034(7) .029(6) .005(6) -.010(6) -.012(6) H13B .061(8) .047(8) .018(5) .006(7) .003(6) .022(6) H13C .042(7) .058(9) .047(8) .010(7) -.012(6) .015(7) H14A .0066(29) .026(4) .029(4) -.0027(30) .0036(28) .004(5) H14B .0066(29) .026(4) .029(4) -.0027(30) .0036(28) .014(5) 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 Ta1 N1 2.022(5) . ? Ta1 N2 2.030(5) . ? Ta1 N3 2.054(5) . ? Ta1 C14 2.223(6) . ? Ta1 N7 2.224(5) . ? Ta1 Ta2 3.032(5) . ? Ta2 N5 1.992(5) . ? Ta2 N6 1.994(5) . ? Ta2 N4 2.022(5) . ? Ta2 N7 2.149(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 H20 Ta1 H30 67.0(4) . . ? H20 Ta2 H30 68.0(4) . . ? Ta1 H20 Ta2 99.5(4) . . ? Ta1 H30 Ta2 102.8(5) . . ? N1 Ta1 N2 108.5(2) . . ? N1 Ta1 N3 93.5(2) . . ? N2 Ta1 N3 87.8(3) . . ? N1 Ta1 C14 108.1(2) . . ? N2 Ta1 C14 142.9(3) . . ? N3 Ta1 C14 84.4(2) . . ? N1 Ta1 N7 93.1(2) . . ? N2 Ta1 N7 143.6(2) . . ? N3 Ta1 N7 120.7(2) . . ? C14 Ta1 N7 38.1(2) . . ? N5 Ta2 N6 103.8(2) . . ? N5 Ta2 N4 106.3(2) . . ? N6 Ta2 N4 98.2(2) . . ? N5 Ta2 N7 98.9(2) . . ? N6 Ta2 N7 153.3(2) . . ? N4 Ta2 N7 88.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag H20 Ta1 Ta2 N7 31.0(7) . . . . ? H30 Ta1 Ta2 N7 -121.8(7) . . . . ? C14 Ta1 Ta2 N7 31.0(2) . . . . ? #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--