data_mf619_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H42 N7 Ta' _chemical_formula_sum 'C31 H42 N7 Ta' _chemical_formula_weight 693.67 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 'C 2/c' 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 15.668(5) _cell_length_b 11.495(5) _cell_length_c 19.926(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 102.002(5) _cell_angle_gamma 90.000(5) _cell_volume 3510(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.578 _cell_measurement_theta_max 27.7765 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 3.159 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.6311 _exptl_absorpt_correction_T_max 0.8542 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 39215 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.73 _reflns_number_total 4086 _reflns_number_gt 3823 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0589P)^2^+3.8167P] 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 4086 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.020 _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 Ta1 Ta 0.5000 0.034740(14) 0.7500 0.02341(8) Uani 1 2 d S . . C1 C 0.5000 -0.1710(5) 0.7500 0.0311(10) Uani 1 2 d S . . N2 N 0.36333(19) 0.0075(3) 0.73989(15) 0.0269(6) Uani 1 1 d . . . N1 N 0.4319(2) -0.2439(3) 0.75149(16) 0.0335(6) Uani 1 1 d . . . C3 C 0.3415(2) -0.2087(3) 0.7503(2) 0.0369(8) Uani 1 1 d . . . H3A H 0.3146 -0.2648 0.7758 0.044 Uiso 1 1 calc R . . H3B H 0.3088 -0.2084 0.7033 0.044 Uiso 1 1 calc R . . C10 C 0.3103(2) 0.1439(3) 0.64596(19) 0.0352(7) Uani 1 1 d . . . H10 H 0.3648 0.1797 0.6546 0.042 Uiso 1 1 calc R . . C5 C 0.2963(2) 0.0470(3) 0.68624(19) 0.0288(7) Uani 1 1 d . . . C6 C 0.2123(3) -0.0046(4) 0.6689(2) 0.0361(8) Uani 1 1 d . . . H6 H 0.2000 -0.0697 0.6930 0.043 Uiso 1 1 calc R . . N4 N 0.5000 0.2155(4) 0.7500 0.0341(9) Uani 1 2 d S . . C8 C 0.1610(3) 0.1361(4) 0.5778(2) 0.0450(9) Uani 1 1 d . . . C7 C 0.1474(3) 0.0406(4) 0.6161(2) 0.0423(10) Uani 1 1 d . . . H7 H 0.0930 0.0047 0.6066 0.051 Uiso 1 1 calc R . . C4 C 0.3375(2) -0.0875(3) 0.78165(18) 0.0311(7) Uani 1 1 d . . . H4A H 0.2784 -0.0733 0.7874 0.037 Uiso 1 1 calc R . . H4B H 0.3754 -0.0861 0.8268 0.037 Uiso 1 1 calc R . . N3 N 0.4853(2) 0.0127(3) 0.64588(17) 0.0332(6) Uani 1 1 d . . . C11 C 0.0897(3) 0.1846(6) 0.5208(2) 0.0670(15) Uani 1 1 d . . . H11A H 0.0863 0.1389 0.4800 0.101 Uiso 1 1 calc R . . H11B H 0.1031 0.2638 0.5116 0.101 Uiso 1 1 calc R . . H11C H 0.0347 0.1817 0.5348 0.101 Uiso 1 1 calc R . . C2 C 0.4576(3) -0.3608(3) 0.7510(2) 0.0451(10) Uani 1 1 d . . . H2 H 0.4224 -0.4257 0.7518 0.054 Uiso 1 1 calc R . . C9 C 0.2449(3) 0.1868(4) 0.5940(2) 0.0443(9) Uani 1 1 d . . . H9 H 0.2567 0.2511 0.5691 0.053 Uiso 1 1 calc R . . C13 C 0.4323(3) -0.0752(5) 0.6027(2) 0.0489(10) Uani 1 1 d . . . H13A H 0.4015 -0.0395 0.5611 0.073 Uiso 1 1 calc R . . H13B H 0.3913 -0.1082 0.6269 0.073 Uiso 1 1 calc R . . H13C H 0.4696 -0.1354 0.5917 0.073 Uiso 1 1 calc R . . C14 C 0.5642(4) 0.2874(4) 0.7268(3) 0.0587(13) Uani 1 1 d . . . H14A H 0.5371 0.3274 0.6856 0.088 Uiso 1 1 calc R . . H14B H 0.6106 0.2393 0.7178 0.088 Uiso 1 1 calc R . . H14C H 0.5874 0.3432 0.7617 0.088 Uiso 1 1 calc R . . C12 C 0.5345(4) 0.0789(5) 0.6038(2) 0.0557(11) Uani 1 1 d . . . H12A H 0.5628 0.0261 0.5781 0.083 Uiso 1 1 calc R . . H12B H 0.5775 0.1260 0.6329 0.083 Uiso 1 1 calc R . . H12C H 0.4953 0.1281 0.5727 0.083 Uiso 1 1 calc R . . C27 C 0.2370(8) 0.7228(13) 0.5271(4) 0.170(6) Uani 1 1 d . . . C28 C 0.3220(7) 0.6222(8) 0.5518(5) 0.124(3) Uani 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 Ta1 0.02435(11) 0.02038(11) 0.02634(12) 0.000 0.00717(7) 0.000 C1 0.035(2) 0.031(3) 0.028(2) 0.000 0.0090(18) 0.000 N2 0.0274(14) 0.0247(13) 0.0302(15) 0.0007(12) 0.0097(11) -0.0016(11) N1 0.0388(16) 0.0210(14) 0.0431(17) 0.0003(12) 0.0136(13) -0.0039(12) C3 0.0363(18) 0.0289(18) 0.047(2) 0.0034(15) 0.0117(15) -0.0072(14) C10 0.0295(17) 0.0360(18) 0.0406(19) 0.0050(15) 0.0082(14) 0.0001(14) C5 0.0264(17) 0.0301(17) 0.0308(17) -0.0028(13) 0.0082(13) 0.0013(12) C6 0.0310(19) 0.0380(18) 0.040(2) -0.0017(17) 0.0085(15) -0.0027(16) N4 0.028(2) 0.020(2) 0.055(3) 0.000 0.0093(18) 0.000 C8 0.0337(19) 0.061(3) 0.039(2) 0.0025(18) 0.0051(15) 0.0106(18) C7 0.0270(19) 0.057(3) 0.042(2) -0.0052(17) 0.0050(16) -0.0032(15) C4 0.0300(16) 0.0320(18) 0.0336(17) 0.0032(14) 0.0116(13) -0.0026(13) N3 0.0363(17) 0.0365(16) 0.0273(15) 0.0018(13) 0.0080(12) 0.0033(13) C11 0.042(2) 0.099(4) 0.055(3) 0.019(3) -0.001(2) 0.015(3) C2 0.055(2) 0.0229(18) 0.062(3) -0.0004(16) 0.022(2) -0.0047(16) C9 0.042(2) 0.048(2) 0.044(2) 0.0136(18) 0.0093(16) 0.0079(17) C13 0.044(2) 0.067(3) 0.034(2) -0.015(2) 0.0054(16) 0.000(2) C14 0.061(3) 0.034(2) 0.084(4) 0.008(2) 0.022(3) -0.007(2) C12 0.074(3) 0.060(3) 0.036(2) 0.013(2) 0.019(2) -0.003(2) C27 0.173(10) 0.225(14) 0.105(7) -0.075(9) 0.015(7) -0.129(10) C28 0.153(9) 0.085(6) 0.116(7) -0.017(5) -0.012(6) 0.013(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 Ta1 N3 2.055(3) 2_656 ? Ta1 N3 2.055(3) . ? Ta1 N4 2.078(4) . ? Ta1 N2 2.132(3) . ? Ta1 N2 2.132(3) 2_656 ? Ta1 C1 2.365(6) . ? C1 N1 1.362(4) . ? C1 N1 1.362(4) 2_656 ? N2 C5 1.409(5) . ? N2 C4 1.479(5) . ? N1 C2 1.404(5) . ? N1 C3 1.468(5) . ? C3 C4 1.534(5) . ? C10 C9 1.387(5) . ? C10 C5 1.417(5) . ? C5 C6 1.420(5) . ? C6 C7 1.401(6) . ? N4 C14 1.449(5) 2_656 ? N4 C14 1.449(5) . ? C8 C7 1.380(6) . ? C8 C9 1.413(6) . ? C8 C11 1.523(6) . ? N3 C12 1.465(5) . ? N3 C13 1.468(6) . ? C2 C2 1.338(9) 2_656 ? C27 C27 1.38(2) 7_566 ? C27 C28 1.754(18) . ? 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 Ta1 N3 165.9(2) 2_656 . ? N3 Ta1 N4 97.07(10) 2_656 . ? N3 Ta1 N4 97.07(10) . . ? N3 Ta1 N2 88.67(12) 2_656 . ? N3 Ta1 N2 89.25(13) . . ? N4 Ta1 N2 98.46(9) . . ? N3 Ta1 N2 89.25(13) 2_656 2_656 ? N3 Ta1 N2 88.67(12) . 2_656 ? N4 Ta1 N2 98.46(9) . 2_656 ? N2 Ta1 N2 163.08(18) . 2_656 ? N3 Ta1 C1 82.93(10) 2_656 . ? N3 Ta1 C1 82.93(10) . . ? N4 Ta1 C1 180.000(2) . . ? N2 Ta1 C1 81.54(9) . . ? N2 Ta1 C1 81.54(9) 2_656 . ? N1 C1 N1 104.1(4) . 2_656 ? N1 C1 Ta1 128.0(2) . . ? N1 C1 Ta1 128.0(2) 2_656 . ? C5 N2 C4 114.6(3) . . ? C5 N2 Ta1 126.8(2) . . ? C4 N2 Ta1 116.3(2) . . ? C1 N1 C2 111.2(3) . . ? C1 N1 C3 126.0(3) . . ? C2 N1 C3 122.7(3) . . ? N1 C3 C4 111.4(3) . . ? C9 C10 C5 121.7(4) . . ? N2 C5 C10 120.3(3) . . ? N2 C5 C6 123.9(3) . . ? C10 C5 C6 115.8(3) . . ? C7 C6 C5 121.3(4) . . ? C14 N4 C14 110.5(5) 2_656 . ? C14 N4 Ta1 124.8(3) 2_656 . ? C14 N4 Ta1 124.8(3) . . ? C7 C8 C9 116.4(4) . . ? C7 C8 C11 122.0(4) . . ? C9 C8 C11 121.6(4) . . ? C8 C7 C6 122.7(4) . . ? N2 C4 C3 113.7(3) . . ? C12 N3 C13 108.8(4) . . ? C12 N3 Ta1 123.5(3) . . ? C13 N3 Ta1 127.4(3) . . ? C2 C2 N1 106.7(2) 2_656 . ? C10 C9 C8 122.2(4) . . ? C27 C27 C28 100.8(15) 7_566 . ? 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 N3 Ta1 C1 N1 82.79(19) 2_656 . . . ? N3 Ta1 C1 N1 -97.21(19) . . . . ? N4 Ta1 C1 N1 178(100) . . . . ? N2 Ta1 C1 N1 -6.92(19) . . . . ? N2 Ta1 C1 N1 173.08(19) 2_656 . . . ? N3 Ta1 C1 N1 -97.21(19) 2_656 . . 2_656 ? N3 Ta1 C1 N1 82.79(19) . . . 2_656 ? N4 Ta1 C1 N1 -2(100) . . . 2_656 ? N2 Ta1 C1 N1 173.08(19) . . . 2_656 ? N2 Ta1 C1 N1 -6.92(19) 2_656 . . 2_656 ? N3 Ta1 N2 C5 155.7(3) 2_656 . . . ? N3 Ta1 N2 C5 -38.3(3) . . . . ? N4 Ta1 N2 C5 58.8(3) . . . . ? N2 Ta1 N2 C5 -121.2(3) 2_656 . . . ? C1 Ta1 N2 C5 -121.2(3) . . . . ? N3 Ta1 N2 C4 -42.4(3) 2_656 . . . ? N3 Ta1 N2 C4 123.6(3) . . . . ? N4 Ta1 N2 C4 -139.3(2) . . . . ? N2 Ta1 N2 C4 40.7(2) 2_656 . . . ? C1 Ta1 N2 C4 40.7(2) . . . . ? N1 C1 N1 C2 0.0(2) 2_656 . . . ? Ta1 C1 N1 C2 -180.0(2) . . . . ? N1 C1 N1 C3 -177.0(4) 2_656 . . . ? Ta1 C1 N1 C3 3.0(4) . . . . ? C1 N1 C3 C4 -27.9(5) . . . . ? C2 N1 C3 C4 155.3(4) . . . . ? C4 N2 C5 C10 174.7(3) . . . . ? Ta1 N2 C5 C10 -23.1(5) . . . . ? C4 N2 C5 C6 -4.9(5) . . . . ? Ta1 N2 C5 C6 157.3(3) . . . . ? C9 C10 C5 N2 -178.2(4) . . . . ? C9 C10 C5 C6 1.5(5) . . . . ? N2 C5 C6 C7 178.2(4) . . . . ? C10 C5 C6 C7 -1.5(6) . . . . ? N3 Ta1 N4 C14 -62.0(3) 2_656 . . 2_656 ? N3 Ta1 N4 C14 118.0(3) . . . 2_656 ? N2 Ta1 N4 C14 27.7(3) . . . 2_656 ? N2 Ta1 N4 C14 -152.3(3) 2_656 . . 2_656 ? C1 Ta1 N4 C14 -158(100) . . . 2_656 ? N3 Ta1 N4 C14 118.0(3) 2_656 . . . ? N3 Ta1 N4 C14 -62.0(3) . . . . ? N2 Ta1 N4 C14 -152.3(3) . . . . ? N2 Ta1 N4 C14 27.7(3) 2_656 . . . ? C1 Ta1 N4 C14 22(100) . . . . ? C9 C8 C7 C6 0.4(6) . . . . ? C11 C8 C7 C6 -179.7(5) . . . . ? C5 C6 C7 C8 0.6(7) . . . . ? C5 N2 C4 C3 83.4(4) . . . . ? Ta1 N2 C4 C3 -80.8(3) . . . . ? N1 C3 C4 N2 68.6(4) . . . . ? N3 Ta1 N3 C12 -135.3(4) 2_656 . . . ? N4 Ta1 N3 C12 44.7(4) . . . . ? N2 Ta1 N3 C12 143.2(4) . . . . ? N2 Ta1 N3 C12 -53.6(4) 2_656 . . . ? C1 Ta1 N3 C12 -135.3(4) . . . . ? N3 Ta1 N3 C13 38.8(3) 2_656 . . . ? N4 Ta1 N3 C13 -141.2(3) . . . . ? N2 Ta1 N3 C13 -42.7(4) . . . . ? N2 Ta1 N3 C13 120.5(4) 2_656 . . . ? C1 Ta1 N3 C13 38.8(3) . . . . ? C1 N1 C2 C2 -0.1(6) . . . 2_656 ? C3 N1 C2 C2 177.1(4) . . . 2_656 ? C5 C10 C9 C8 -0.6(6) . . . . ? C7 C8 C9 C10 -0.4(6) . . . . ? C11 C8 C9 C10 179.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.276 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.144