Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'John Arnold' _publ_contact_author_address ; Department of Chemistry University of California Berkeley Berkeley CA 94720 UNITED STATES OF AMERICA ; _publ_contact_author_email ARNOLD@BERKELEY.EDU _publ_section_title ; Olefination and Group Transfer Reactions of an Electron Deficient Tantalum Methylidene Complex ; loop_ _publ_author_name 'John Arnold' 'Robert Bergman' 'Mullins Sarah' #------------------------------------------------------------------------------ # Attachment 'tathiof.cif' data_Ta_Me_thioformaldehyde _database_code_depnum_ccdc_archive 'CCDC 283319' _audit_creation_date 'Wed Sep 28 16:46:04 2005' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H46 N4 S Si4 Ta ' _chemical_formula_moiety 'C30 H46 N4 S Si4 Ta ' _chemical_formula_weight 788.07 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.9195(3) _cell_length_b 18.8911(4) _cell_length_c 16.7243(2) _cell_angle_alpha 90 _cell_angle_beta 103.423(1) _cell_angle_gamma 90 _cell_volume 3970.3(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5016 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 22.5 _cell_measurement_temperature 168.2 #------------------------------------------------------------------------------ _exptl_crystal_description needlelike _exptl_crystal_colour yellow _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596.00 _exptl_absorpt_coefficient_mu 2.960 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.820 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scans _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9490 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 24.40 _diffrn_measured_fraction_theta_max 0.9966 _diffrn_reflns_theta_full 24.40 _diffrn_measured_fraction_theta_full 0.9966 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). The complex has a crystallographic two-fold axis. This causes the thioformaldehyde and the methyl group to be disordered. There is also disorder in the methyl groups of one of the SiMe3 moieties. The possibility of an ordered structure in Cc was investigated, but did not reach a stable refinement. The refinement of the disordered model in C2/c proceeded cleanly. Hydrogen atoms were calculated for all except the disordered SiMe3, hence the discrepancy between the observed and calculated formulae. ; _reflns_number_total 3257 _reflns_number_gt 2689 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0416 _refine_ls_R_factor_all 0.0433 _refine_ls_wR_factor_all 0.0438 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2689 _refine_ls_number_parameters 182 _refine_ls_goodness_of_fit_ref 1.676 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0025 _refine_diff_density_max 0.83 _refine_diff_density_min -0.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ta Ta -0.705 6.523 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si Si 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-AXS SMART v5.054' _computing_cell_refinement 'Bruker-AXS SAINT v6.40' _computing_data_reduction 'Bruker-AXS SAINT v6.40' _computing_structure_solution ? _computing_structure_refinement teXsan _computing_publication_material teXsan _computing_molecular_graphics ? #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.0000 0.24411(2) 0.2500 0.0441(1) Uani 1.00 d S . . S1 S -0.0097(4) 0.3618(2) 0.2149(2) 0.085(1) Uani 0.50 d P . . Si1 Si 0.2545(1) 0.26321(9) 0.1978(1) 0.0560(5) Uani 1.00 d . . . Si2 Si 0.0725(1) 0.09097(10) 0.3997(1) 0.0619(5) Uani 1.00 d . . . N1 N 0.1562(3) 0.2177(2) 0.2364(3) 0.043(1) Uani 1.00 d . . . N2 N 0.0857(3) 0.1510(2) 0.3222(3) 0.044(1) Uani 1.00 d . . . C1 C 0.1709(4) 0.1657(3) 0.2940(3) 0.043(2) Uani 1.00 d . . . C2 C 0.2757(4) 0.1292(3) 0.3238(3) 0.048(2) Uani 1.00 d . . . C3 C 0.3000(5) 0.0666(3) 0.2891(4) 0.082(2) Uani 1.00 d . . . C4 C 0.3963(5) 0.0332(3) 0.3192(5) 0.085(2) Uani 1.00 d . . . C5 C 0.4719(4) 0.0605(3) 0.3835(4) 0.058(2) Uani 1.00 d . . . C6 C 0.4467(4) 0.1226(3) 0.4180(3) 0.059(2) Uani 1.00 d . . . C7 C 0.3506(4) 0.1569(3) 0.3883(3) 0.051(2) Uani 1.00 d . . . C8 C 0.5762(5) 0.0235(4) 0.4182(4) 0.081(3) Uani 1.00 d . . . C9 C 0.3248(6) 0.3278(4) 0.2741(5) 0.097(3) Uani 1.00 d . . . C10 C 0.3536(5) 0.2025(4) 0.1698(5) 0.086(3) Uani 1.00 d . . . C11 C 0.1904(5) 0.3128(5) 0.1039(5) 0.096(3) Uani 1.00 d . . . C12 C 0.151(1) 0.1305(9) 0.5046(10) 0.089(4) Uiso 0.50 d P . . C13 C 0.155(1) 0.0055(10) 0.395(1) 0.106(5) Uiso 0.50 d P . . C14 C -0.063(1) 0.0739(8) 0.3924(9) 0.079(4) Uiso 0.50 d P . . C15 C 0.177(1) 0.0845(7) 0.4919(8) 0.064(3) Uiso 0.50 d P . . C16 C 0.034(1) -0.0010(9) 0.350(1) 0.095(5) Uiso 0.50 d P . . C17 C -0.062(1) 0.1177(7) 0.4325(8) 0.074(4) Uiso 0.50 d P . . C18 C 0.066(1) 0.3033(9) 0.359(1) 0.067(5) Uiso 0.50 d P . . C19 C -0.053(1) 0.2880(8) 0.1191(10) 0.059(4) Uiso 0.50 d P . . H1 H 0.2500 0.0464 0.2441 0.0983 Uiso 1.00 calc . . . H2 H 0.4107 -0.0099 0.2947 0.1016 Uiso 1.00 calc . . . H3 H 0.4966 0.1425 0.4633 0.0704 Uiso 1.00 calc . . . H4 H 0.3364 0.2000 0.4129 0.0618 Uiso 1.00 calc . . . H5 H 0.6254 0.0562 0.4492 0.0971 Uiso 1.00 calc . . . H6 H 0.6038 0.0053 0.3744 0.0971 Uiso 1.00 calc . . . H7 H 0.5650 -0.0143 0.4527 0.0971 Uiso 1.00 calc . . . H8 H 0.3586 0.3037 0.3231 0.1165 Uiso 1.00 calc . . . H9 H 0.3768 0.3519 0.2525 0.1165 Uiso 1.00 calc . . . H10 H 0.2752 0.3610 0.2860 0.1165 Uiso 1.00 calc . . . H11 H 0.3887 0.1765 0.2169 0.1037 Uiso 1.00 calc . . . H12 H 0.3184 0.1707 0.1284 0.1037 Uiso 1.00 calc . . . H13 H 0.4044 0.2293 0.1497 0.1037 Uiso 1.00 calc . . . H14 H 0.2433 0.3366 0.0830 0.1150 Uiso 1.00 calc . . . H15 H 0.1530 0.2807 0.0636 0.1150 Uiso 1.00 calc . . . H16 H 0.1420 0.3464 0.1168 0.1150 Uiso 1.00 calc . . . H17 H 0.0886 0.2716 0.4042 0.0805 Uiso 0.50 calc P . . H18 H 0.1244 0.3303 0.3517 0.0805 Uiso 0.50 calc P . . H19 H 0.0128 0.3341 0.3711 0.0805 Uiso 0.50 calc P . . H20 H -0.0081 0.2817 0.0817 0.0709 Uiso 0.50 calc P . . H21 H -0.1250 0.2841 0.0904 0.0709 Uiso 0.50 calc 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta1 0.0357(2) 0.0385(2) 0.0583(2) 0.0000 0.0115(1) 0.0000 S1 0.081(3) 0.049(2) 0.135(4) 0.002(2) 0.042(4) 0.017(2) Si1 0.0449(9) 0.067(1) 0.060(1) 0.0048(7) 0.0195(8) 0.0098(8) Si2 0.066(1) 0.070(1) 0.0475(10) 0.0007(9) 0.0081(9) 0.0152(8) N1 0.039(2) 0.043(2) 0.047(3) 0.003(2) 0.010(2) 0.003(2) N2 0.042(3) 0.049(3) 0.038(2) -0.001(2) 0.002(2) 0.003(2) C1 0.044(3) 0.043(3) 0.038(3) -0.001(2) -0.000(2) -0.007(2) C2 0.043(3) 0.048(3) 0.050(3) 0.002(2) 0.006(3) 0.002(2) C3 0.060(4) 0.067(4) 0.098(6) 0.019(3) -0.025(4) -0.021(4) C4 0.072(5) 0.056(4) 0.109(6) 0.026(3) -0.011(4) -0.009(4) C5 0.044(4) 0.066(4) 0.061(4) 0.006(3) 0.005(3) 0.020(3) C6 0.036(3) 0.086(5) 0.050(4) -0.007(3) 0.002(3) 0.003(3) C7 0.045(3) 0.060(4) 0.047(3) -0.003(3) 0.007(3) -0.005(3) C8 0.047(4) 0.097(5) 0.093(6) 0.013(3) 0.006(4) 0.031(4) C9 0.097(6) 0.081(5) 0.121(7) -0.041(4) 0.043(5) -0.007(5) C10 0.055(4) 0.111(6) 0.101(6) 0.014(4) 0.034(4) 0.001(5) C11 0.062(5) 0.137(7) 0.093(6) 0.020(4) 0.027(4) 0.053(5) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TA1 S1 2.296(3) . . yes TA1 S1 2.296(3) . 2_555 yes TA1 N1 2.141(4) . . yes TA1 N1 2.141(4) . 2_555 yes TA1 N2 2.271(4) . . yes TA1 N2 2.271(4) . 2_555 yes TA1 C18 2.14(2) . . yes TA1 C18 2.14(2) . 2_555 yes TA1 C19 2.29(2) . . yes TA1 C19 2.29(2) . 2_555 yes S1 S1 1.143(8) . 2_555 yes S1 C18 1.70(2) . 2_555 yes S1 C19 2.10(2) . . yes SI1 N1 1.774(4) . . yes SI1 C9 1.845(8) . . yes SI1 C10 1.859(7) . . yes SI1 C11 1.851(7) . . yes SI2 N2 1.760(4) . . yes SI2 C12 1.96(2) . . yes SI2 C13 1.94(2) . . yes SI2 C14 1.76(1) . . yes SI2 C15 1.81(1) . . yes SI2 C16 1.94(2) . . yes SI2 C17 2.01(1) . . yes N1 C1 1.358(6) . . yes N2 C1 1.325(6) . . yes C1 C2 1.497(7) . . yes C2 C3 1.385(8) . . yes C2 C7 1.375(7) . . yes C3 C4 1.381(8) . . yes C4 C5 1.374(8) . . yes C5 C6 1.379(8) . . yes C5 C8 1.508(8) . . yes C6 C7 1.386(7) . . yes C12 C15 0.98(2) . . yes C13 C16 1.57(2) . . yes C14 C17 1.06(2) . . yes C18 C19 0.52(2) . 2_555 yes S1 H19 1.521 . 2_555 no C3 H1 0.950 . . no C4 H2 0.950 . . no C6 H3 0.950 . . no C7 H4 0.950 . . no C8 H5 0.950 . . no C8 H6 0.950 . . no C8 H7 0.950 . . no C9 H8 0.950 . . no C9 H9 0.950 . . no C9 H10 0.950 . . no C10 H11 0.950 . . no C10 H12 0.950 . . no C10 H13 0.950 . . no C11 H14 0.950 . . no C11 H15 0.950 . . no C11 H16 0.950 . . no C18 H17 0.950 . . no C18 H18 0.950 . . no C18 H19 0.950 . . no C18 H21 1.061 . 2_555 no C19 H17 0.617 . 2_555 no C19 H19 1.004 . 2_555 no C19 H20 0.950 . . no C19 H21 0.950 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 TA1 S1 28.8(2) . 1_555 2_555 ? S1 TA1 N1 101.3(2) . . . ? S1 TA1 N1 104.8(2) . 1_555 2_555 ? S1 TA1 N2 151.3(2) . . . ? S1 TA1 N2 128.6(1) . 1_555 2_555 ? S1 TA1 C18 72.6(5) . . . ? S1 TA1 C18 44.7(4) . 1_555 2_555 ? S1 TA1 C19 54.4(4) . . . ? S1 TA1 C19 83.1(4) . 1_555 2_555 ? N1 TA1 N1 153.0(2) . 1_555 2_555 ? N1 TA1 N2 61.4(2) . . . ? N1 TA1 N2 96.8(2) . 1_555 2_555 ? N1 TA1 C18 91.0(5) . . . ? N1 TA1 C18 103.1(5) . 1_555 2_555 ? N1 TA1 C19 93.5(4) . . . ? N1 TA1 C19 96.2(4) . 1_555 2_555 ? N2 TA1 N2 78.5(2) . 1_555 2_555 ? N2 TA1 C18 84.4(4) . . . ? N2 TA1 C18 154.8(5) . 1_555 2_555 ? N2 TA1 C19 142.0(4) . . . ? N2 TA1 C19 76.9(4) . 1_555 2_555 ? C18 TA1 C18 117.2(9) . 1_555 2_555 ? C18 TA1 C19 126.7(6) . . . ? C18 TA1 C19 12.8(6) . 1_555 2_555 ? C19 TA1 C19 137.6(8) . 1_555 2_555 ? TA1 S1 S1 75.6(1) . 1_555 2_555 ? TA1 S1 C18 62.9(6) . 1_555 2_555 ? TA1 S1 C19 62.7(4) . . . ? N1 SI1 C9 110.4(3) . . . ? N1 SI1 C10 112.7(3) . . . ? N1 SI1 C11 109.7(3) . . . ? C9 SI1 C10 108.9(4) . . . ? C9 SI1 C11 107.7(4) . . . ? C10 SI1 C11 107.2(4) . . . ? N2 SI2 C12 107.2(5) . . . ? N2 SI2 C13 110.8(6) . . . ? N2 SI2 C14 109.4(5) . . . ? N2 SI2 C15 119.4(4) . . . ? N2 SI2 C16 108.8(5) . . . ? N2 SI2 C17 106.1(4) . . . ? C12 SI2 C13 100.5(7) . . . ? C12 SI2 C14 115.6(7) . . . ? C12 SI2 C15 29.7(5) . . . ? C12 SI2 C16 138.8(7) . . . ? C12 SI2 C17 87.8(6) . . . ? C13 SI2 C14 112.9(7) . . . ? C13 SI2 C15 70.8(6) . . . ? C13 SI2 C16 47.7(6) . . . ? C13 SI2 C17 137.5(7) . . . ? C14 SI2 C15 125.9(6) . . . ? C14 SI2 C16 69.6(7) . . . ? C14 SI2 C17 31.9(5) . . . ? C15 SI2 C16 111.8(6) . . . ? C15 SI2 C17 108.1(6) . . . ? C16 SI2 C17 100.8(6) . . . ? TA1 N1 SI1 134.2(2) . . . ? TA1 N1 C1 94.2(3) . . . ? SI1 N1 C1 127.9(4) . . . ? TA1 N2 SI2 140.6(2) . . . ? TA1 N2 C1 89.5(3) . . . ? SI2 N2 C1 128.9(4) . . . ? N1 C1 N2 114.4(4) . . . ? N1 C1 C2 122.4(5) . . . ? N2 C1 C2 123.2(5) . . . ? C1 C2 C3 121.9(5) . . . ? C1 C2 C7 120.2(5) . . . ? C3 C2 C7 117.8(5) . . . ? C2 C3 C4 120.6(6) . . . ? C3 C4 C5 122.1(6) . . . ? C4 C5 C6 116.9(5) . . . ? C4 C5 C8 122.4(6) . . . ? C6 C5 C8 120.7(6) . . . ? C5 C6 C7 121.8(5) . . . ? C2 C7 C6 120.8(5) . . . ? SI2 C12 C15 66(1) . . . ? SI2 C13 C16 66.0(9) . . . ? SI2 C14 C17 87(1) . . . ? SI2 C15 C12 83(1) . . . ? SI2 C16 C13 66.4(9) . . . ? SI2 C17 C14 60(1) . . . ? TA1 C18 S1 72.4(6) . 1_555 2_555 ? TA1 C18 C19 100(3) . 1_555 2_555 ? TA1 C19 S1 62.9(4) . . . ? TA1 C19 C18 67(2) . 1_555 2_555 ? S1 C19 C18 34(2) . 1_555 2_555 ? TA1 S1 H19 84.028 . 1_555 2_555 no C19 S1 H19 26.592 . 1_555 2_555 no C2 C3 H1 119.682 . . . no C4 C3 H1 119.685 . . . no C3 C4 H2 118.960 . . . no C5 C4 H2 118.965 . . . no C5 C6 H3 119.110 . . . no C7 C6 H3 119.108 . . . no C2 C7 H4 119.585 . . . no C6 C7 H4 119.585 . . . no C5 C8 H5 109.468 . . . no C5 C8 H6 109.474 . . . no C5 C8 H7 109.473 . . . no H5 C8 H6 109.469 . . . no H5 C8 H7 109.468 . . . no H6 C8 H7 109.476 . . . no SI1 C9 H8 109.467 . . . no SI1 C9 H9 109.461 . . . no SI1 C9 H10 109.464 . . . no H8 C9 H9 109.479 . . . no H8 C9 H10 109.483 . . . no H9 C9 H10 109.473 . . . no SI1 C10 H11 109.473 . . . no SI1 C10 H12 109.473 . . . no SI1 C10 H13 109.472 . . . no H11 C10 H12 109.471 . . . no H11 C10 H13 109.470 . . . no H12 C10 H13 109.468 . . . no SI1 C11 H14 109.462 . . . no SI1 C11 H15 109.470 . . . no SI1 C11 H16 109.462 . . . no H14 C11 H15 109.480 . . . no H14 C11 H16 109.470 . . . no H15 C11 H16 109.482 . . . no TA1 C18 H17 109.466 . . . no TA1 C18 H18 109.476 . . . no TA1 C18 H19 109.472 . . . no TA1 C18 H21 124.494 . 1_555 2_555 no H17 C18 H18 109.469 . . . no H17 C18 H19 109.464 . . . no H17 C18 H21 29.008 . 1_555 2_555 no H18 C18 H19 109.481 . . . no H18 C18 H21 80.657 . 1_555 2_555 no H19 C18 H21 118.062 . 1_555 2_555 no TA1 C19 H17 115.735 . 1_555 2_555 no TA1 C19 H19 97.469 . 1_555 2_555 no TA1 C19 H20 119.516 . . . no TA1 C19 H21 119.512 . . . no S1 C19 H17 147.487 . 1_555 2_555 no S1 C19 H19 42.688 . 1_555 2_555 no S1 C19 H20 119.510 . . . no S1 C19 H21 119.507 . . . no H20 C19 H21 109.469 . . . no #------------------------------------------------------------------------------ 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 TA1 S1 S1 C18 22(1) 1_555 1_555 2_555 1_555 yes TA1 S1 S1 C19 8.7(9) 1_555 1_555 2_555 2_555 yes TA1 S1 C18 C19 -86(4) 1_555 1_555 2_555 1_555 yes TA1 S1 C19 C18 88(4) 1_555 1_555 1_555 2_555 yes TA1 S1 S1 C18 22(1) 1_555 2_555 1_555 2_555 yes TA1 S1 S1 C19 8.7(9) 1_555 2_555 1_555 1_555 yes TA1 S1 C18 C19 -86(4) 1_555 2_555 1_555 2_555 yes TA1 S1 C19 C18 88(4) 1_555 2_555 2_555 1_555 yes TA1 N1 SI1 C9 77.5(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C10 -160.4(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C11 -41.0(5) 1_555 1_555 1_555 1_555 yes TA1 N1 C1 N2 7.0(4) 1_555 1_555 1_555 1_555 yes TA1 N1 C1 C2 -172.0(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C9 77.5(4) 1_555 2_555 2_555 2_555 yes TA1 N1 SI1 C10 -160.4(4) 1_555 2_555 2_555 2_555 yes TA1 N1 SI1 C11 -41.0(5) 1_555 2_555 2_555 2_555 yes TA1 N1 C1 N2 7.0(4) 1_555 2_555 2_555 2_555 yes TA1 N1 C1 C2 -172.0(4) 1_555 2_555 2_555 2_555 yes TA1 N2 SI2 C12 -93.7(6) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C13 157.5(6) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C14 32.3(7) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C15 -123.4(6) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C16 106.7(6) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C17 -1.1(6) 1_555 1_555 1_555 1_555 yes TA1 N2 C1 N1 -6.5(4) 1_555 1_555 1_555 1_555 yes TA1 N2 C1 C2 172.4(4) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C12 -93.7(6) 1_555 2_555 2_555 2_555 yes TA1 N2 SI2 C13 157.5(6) 1_555 2_555 2_555 2_555 yes TA1 N2 SI2 C14 32.3(7) 1_555 2_555 2_555 2_555 yes TA1 N2 SI2 C15 -123.4(6) 1_555 2_555 2_555 2_555 yes TA1 N2 SI2 C16 106.7(6) 1_555 2_555 2_555 2_555 yes TA1 N2 SI2 C17 -1.1(6) 1_555 2_555 2_555 2_555 yes TA1 N2 C1 N1 -6.5(4) 1_555 2_555 2_555 2_555 yes TA1 N2 C1 C2 172.4(4) 1_555 2_555 2_555 2_555 yes TA1 C18 S1 S1 -24(1) 1_555 1_555 2_555 1_555 yes TA1 C18 S1 C19 86(4) 1_555 1_555 2_555 2_555 yes TA1 C18 C19 S1 -74(3) 1_555 1_555 2_555 2_555 yes TA1 C18 S1 S1 -24(1) 1_555 2_555 1_555 2_555 yes TA1 C18 S1 C19 86(4) 1_555 2_555 1_555 1_555 yes TA1 C18 C19 S1 -74(3) 1_555 2_555 1_555 1_555 yes TA1 C19 S1 S1 -9(1) 1_555 1_555 1_555 2_555 yes TA1 C19 S1 C18 -88(4) 1_555 1_555 1_555 2_555 yes TA1 C19 C18 S1 74(3) 1_555 1_555 2_555 1_555 yes TA1 C19 S1 S1 -9(1) 1_555 2_555 2_555 1_555 yes TA1 C19 S1 C18 -88(4) 1_555 2_555 2_555 1_555 yes TA1 C19 C18 S1 74(3) 1_555 2_555 1_555 2_555 yes S1 TA1 S1 C18 -162.3(9) 1_555 1_555 2_555 1_555 yes S1 TA1 S1 C19 -173.4(7) 1_555 1_555 2_555 2_555 yes S1 TA1 N1 SI1 -7.2(3) 1_555 1_555 1_555 1_555 yes S1 TA1 N1 C1 151.3(3) 1_555 1_555 1_555 1_555 yes S1 TA1 N1 SI1 -36.6(4) 1_555 1_555 2_555 2_555 yes S1 TA1 N1 C1 122.0(3) 1_555 1_555 2_555 2_555 yes S1 TA1 N2 SI2 114.4(4) 1_555 1_555 1_555 1_555 yes S1 TA1 N2 C1 -53.5(4) 1_555 1_555 1_555 1_555 yes S1 TA1 N2 SI2 85.7(4) 1_555 1_555 2_555 2_555 yes S1 TA1 N2 C1 -82.2(3) 1_555 1_555 2_555 2_555 yes S1 TA1 C18 C19 144(3) 1_555 1_555 1_555 2_555 yes S1 TA1 C18 C19 135(3) 1_555 1_555 2_555 1_555 yes S1 TA1 C19 C18 -37(3) 1_555 1_555 1_555 2_555 yes S1 TA1 C19 C18 -34(3) 1_555 1_555 2_555 1_555 yes S1 S1 TA1 N1 86.4(5) 1_555 2_555 1_555 1_555 yes S1 S1 TA1 N1 -100.4(5) 1_555 2_555 1_555 2_555 yes S1 S1 TA1 N2 151.4(4) 1_555 2_555 1_555 1_555 yes S1 S1 TA1 N2 -51.2(6) 1_555 2_555 1_555 2_555 yes S1 S1 TA1 C18 162.3(9) 1_555 2_555 1_555 1_555 yes S1 S1 TA1 C18 -12.9(6) 1_555 2_555 1_555 2_555 yes S1 S1 TA1 C19 -5.4(6) 1_555 2_555 1_555 1_555 yes S1 S1 TA1 C19 173.4(7) 1_555 2_555 1_555 2_555 yes S1 S1 C18 C19 -110(4) 1_555 2_555 1_555 2_555 yes S1 S1 C19 C18 79(5) 1_555 2_555 2_555 1_555 yes S1 C18 TA1 N1 -92.9(5) 1_555 2_555 1_555 1_555 yes S1 C18 TA1 N1 110.3(5) 1_555 2_555 1_555 2_555 yes S1 C18 TA1 N2 -141.5(7) 1_555 2_555 1_555 1_555 yes S1 C18 TA1 N2 171.4(5) 1_555 2_555 1_555 2_555 yes S1 C18 TA1 C18 5.1(2) 1_555 2_555 1_555 1_555 yes S1 C18 TA1 C19 -135(3) 1_555 2_555 1_555 1_555 yes S1 C18 TA1 C19 15(1) 1_555 2_555 1_555 2_555 yes S1 C19 TA1 N1 -101.4(3) 1_555 1_555 1_555 1_555 yes S1 C19 TA1 N1 103.8(3) 1_555 1_555 1_555 2_555 yes S1 C19 TA1 N2 -146.8(4) 1_555 1_555 1_555 1_555 yes S1 C19 TA1 N2 162.5(4) 1_555 1_555 1_555 2_555 yes S1 C19 TA1 C18 -7.6(9) 1_555 1_555 1_555 1_555 yes S1 C19 TA1 C18 37(3) 1_555 1_555 1_555 2_555 yes S1 C19 TA1 C19 1.8(2) 1_555 1_555 1_555 2_555 yes SI1 N1 TA1 N1 158.2(3) 1_555 1_555 1_555 2_555 yes SI1 N1 TA1 N2 -162.8(4) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 N2 124.3(3) 1_555 1_555 1_555 2_555 yes SI1 N1 TA1 C18 -79.7(6) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 C18 38.5(6) 1_555 1_555 1_555 2_555 yes SI1 N1 TA1 C19 47.2(5) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 C19 -91.4(5) 1_555 1_555 1_555 2_555 yes SI1 N1 C1 N2 167.6(4) 1_555 1_555 1_555 1_555 yes SI1 N1 C1 C2 -11.4(7) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N1 172.2(4) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N1 -24.5(4) 1_555 1_555 1_555 2_555 yes SI2 N2 TA1 N2 -83.4(4) 1_555 1_555 1_555 2_555 yes SI2 N2 TA1 C18 78.0(6) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 C18 -131(1) 1_555 1_555 1_555 2_555 yes SI2 N2 TA1 C19 -133.7(7) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 C19 67.5(5) 1_555 1_555 1_555 2_555 yes SI2 N2 C1 N1 -176.7(4) 1_555 1_555 1_555 1_555 yes SI2 N2 C1 C2 2.3(7) 1_555 1_555 1_555 1_555 yes N1 TA1 S1 C18 97.3(7) 1_555 1_555 1_555 2_555 yes N1 TA1 S1 C19 86.2(5) 1_555 1_555 1_555 1_555 yes N1 TA1 S1 C18 -75.9(7) 1_555 1_555 2_555 1_555 yes N1 TA1 S1 C19 -87.0(5) 1_555 1_555 2_555 2_555 yes N1 TA1 N1 C1 -43.2(3) 1_555 1_555 2_555 2_555 yes N1 TA1 N2 C1 4.3(3) 1_555 1_555 1_555 1_555 yes N1 TA1 N2 C1 167.6(3) 1_555 1_555 2_555 2_555 yes N1 TA1 C18 C19 -114(3) 1_555 1_555 1_555 2_555 yes N1 TA1 C18 C19 42(3) 1_555 1_555 2_555 1_555 yes N1 TA1 C19 C18 -138(3) 1_555 1_555 1_555 2_555 yes N1 TA1 C19 C18 66(3) 1_555 1_555 2_555 1_555 yes N1 C1 C2 C3 -93.6(7) 1_555 1_555 1_555 1_555 yes N1 C1 C2 C7 87.5(7) 1_555 1_555 1_555 1_555 yes N2 TA1 S1 C18 146.5(7) 1_555 1_555 1_555 2_555 yes N2 TA1 S1 C19 135.4(6) 1_555 1_555 1_555 1_555 yes N2 TA1 S1 C18 -10.9(7) 1_555 1_555 2_555 1_555 yes N2 TA1 S1 C19 -22.0(5) 1_555 1_555 2_555 2_555 yes N2 TA1 N1 C1 -4.2(3) 1_555 1_555 1_555 1_555 yes N2 TA1 N1 C1 -77.1(3) 1_555 1_555 2_555 2_555 yes N2 TA1 N2 C1 108.7(3) 1_555 1_555 2_555 2_555 yes N2 TA1 C18 C19 -53(3) 1_555 1_555 1_555 2_555 yes N2 TA1 C18 C19 -6(4) 1_555 1_555 2_555 1_555 yes N2 TA1 C19 C18 175(2) 1_555 1_555 1_555 2_555 yes N2 TA1 C19 C18 125(3) 1_555 1_555 2_555 1_555 yes N2 SI2 C12 C15 -119(1) 1_555 1_555 1_555 1_555 yes N2 SI2 C13 C16 -96.9(9) 1_555 1_555 1_555 1_555 yes N2 SI2 C14 C17 -89(1) 1_555 1_555 1_555 1_555 yes N2 SI2 C15 C12 72(1) 1_555 1_555 1_555 1_555 yes N2 SI2 C16 C13 101.4(9) 1_555 1_555 1_555 1_555 yes N2 SI2 C17 C14 100(1) 1_555 1_555 1_555 1_555 yes N2 C1 C2 C3 87.5(8) 1_555 1_555 1_555 1_555 yes N2 C1 C2 C7 -91.3(7) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C18 78.9(5) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C18 -162.9(5) 1_555 1_555 1_555 2_555 yes C1 N1 TA1 C19 -154.3(5) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C19 67.1(5) 1_555 1_555 1_555 2_555 yes C1 N1 SI1 C9 -75.0(5) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C10 47.1(5) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C11 166.5(5) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C18 -89.9(5) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C18 60(1) 1_555 1_555 1_555 2_555 yes C1 N2 TA1 C19 58.4(7) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C19 -100.4(5) 1_555 1_555 1_555 2_555 yes C1 N2 SI2 C12 70.6(7) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C13 -38.1(7) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C14 -163.3(6) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C15 41.0(7) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C16 -89.0(7) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C17 163.3(6) 1_555 1_555 1_555 1_555 yes C1 C2 C3 C4 -178.4(7) 1_555 1_555 1_555 1_555 yes C1 C2 C7 C6 178.2(5) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C5 0(1) 1_555 1_555 1_555 1_555 yes C2 C7 C6 C5 1.1(9) 1_555 1_555 1_555 1_555 yes C3 C2 C7 C6 -0.7(9) 1_555 1_555 1_555 1_555 yes C3 C4 C5 C6 1(1) 1_555 1_555 1_555 1_555 yes C3 C4 C5 C8 178.5(7) 1_555 1_555 1_555 1_555 yes C4 C3 C2 C7 0(1) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C7 -1.2(9) 1_555 1_555 1_555 1_555 yes C7 C6 C5 C8 -178.7(6) 1_555 1_555 1_555 1_555 yes C12 SI2 C13 C16 150.0(9) 1_555 1_555 1_555 1_555 yes C12 SI2 C14 C17 31(1) 1_555 1_555 1_555 1_555 yes C12 SI2 C16 C13 -48(1) 1_555 1_555 1_555 1_555 yes C12 SI2 C17 C14 -151(1) 1_555 1_555 1_555 1_555 yes C12 C15 SI2 C13 176(1) 1_555 1_555 1_555 1_555 yes C12 C15 SI2 C14 -79(1) 1_555 1_555 1_555 1_555 yes C12 C15 SI2 C16 -159(1) 1_555 1_555 1_555 1_555 yes C12 C15 SI2 C17 -48(1) 1_555 1_555 1_555 1_555 yes C13 SI2 C12 C15 -3(1) 1_555 1_555 1_555 1_555 yes C13 SI2 C14 C17 146(1) 1_555 1_555 1_555 1_555 yes C13 SI2 C17 C14 -48(1) 1_555 1_555 1_555 1_555 yes C13 C16 SI2 C14 -154(1) 1_555 1_555 1_555 1_555 yes C13 C16 SI2 C15 -32(1) 1_555 1_555 1_555 1_555 yes C13 C16 SI2 C17 -147.3(9) 1_555 1_555 1_555 1_555 yes C14 SI2 C12 C15 118(1) 1_555 1_555 1_555 1_555 yes C14 SI2 C13 C16 26(1) 1_555 1_555 1_555 1_555 yes C14 C17 SI2 C15 -129(1) 1_555 1_555 1_555 1_555 yes C14 C17 SI2 C16 -12(1) 1_555 1_555 1_555 1_555 yes C15 SI2 C13 C16 148(1) 1_555 1_555 1_555 1_555 yes C15 SI2 C14 C17 64(1) 1_555 1_555 1_555 1_555 yes C15 C12 SI2 C16 30(1) 1_555 1_555 1_555 1_555 yes C15 C12 SI2 C17 134(1) 1_555 1_555 1_555 1_555 yes C16 SI2 C14 C17 166(1) 1_555 1_555 1_555 1_555 yes C16 C13 SI2 C17 51(1) 1_555 1_555 1_555 1_555 yes C18 TA1 S1 C19 173.7(8) 1_555 1_555 1_555 1_555 yes C18 TA1 S1 C19 -11.1(9) 1_555 1_555 2_555 2_555 yes C18 TA1 C18 C19 140(3) 1_555 1_555 2_555 1_555 yes C18 S1 TA1 C19 -167.7(9) 1_555 2_555 1_555 1_555 yes C18 S1 TA1 C19 11.1(9) 1_555 2_555 1_555 2_555 yes C18 S1 S1 C18 44(2) 1_555 2_555 1_555 2_555 yes C18 S1 S1 C19 31(1) 1_555 2_555 1_555 1_555 yes C18 C19 TA1 C19 -35(3) 1_555 2_555 1_555 1_555 yes C19 S1 S1 C19 17(1) 1_555 1_555 2_555 2_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C6 C10 3.583(9) . 2_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # Attachment 'methy.cif' data_a_tantalum_methyl_methylid _database_code_depnum_ccdc_archive 'CCDC 283320' _audit_creation_date 'Tue Oct 4 11:14:39 2005' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Blessing, R. H., (1995), Acta Crystallogr, A51, 33-38. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C30 H55 N4 Si4 Ta ' _chemical_formula_moiety 'C30 H55 N4 Si4 Ta ' _chemical_formula_weight 765.08 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 28.2182(1) _cell_length_b 8.7227(1) _cell_length_c 19.8359(1) _cell_angle_alpha 90 _cell_angle_beta 128.625(1) _cell_angle_gamma 90 _cell_volume 3814.35(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8042 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.0 _cell_measurement_temperature 155.2 #------------------------------------------------------------------------------ _exptl_crystal_description blocklike _exptl_crystal_colour orange _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568.00 _exptl_absorpt_coefficient_mu 3.026 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.450 _exptl_absorpt_correction_T_max 0.640 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scans _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10633 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 26.17 _diffrn_measured_fraction_theta_max 0.8981 _diffrn_reflns_theta_full 24.7 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). The tantalum atoms sits on a crystallographioc two-fold axis which makes discrimination of the methyl and methyene carbons impossible. A single full-occupancy carbon atom was refined. No attempt was made to locate the disordered hydrogen atoms on this carbon. ; _reflns_number_total 3429 _reflns_number_gt 2922 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0378 _refine_ls_R_factor_all 0.0365 _refine_ls_wR_factor_all 0.0406 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2922 _refine_ls_number_parameters 177 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0008 _refine_diff_density_max 1.60 _refine_diff_density_min -0.96 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si Si 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ta Ta -0.705 6.523 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-AXS SMART v5.054' _computing_cell_refinement 'Bruker-AXS SAINT v6.40' _computing_data_reduction 'Bruker-AXS SAINT v6.40' _computing_structure_solution SIR92 _computing_structure_refinement teXsan _computing_publication_material teXsan _computing_molecular_graphics ? #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.000 0.02908(3) 0.250 0.03353(7) Uani 1.00 d S . . Si2 Si -0.03809(5) 0.3427(1) 0.33689(7) 0.0354(3) Uani 1.00 d . . . Si3 Si 0.15826(5) -0.0240(2) 0.43272(8) 0.0367(3) Uani 1.00 d . . . N1 N 0.0104(1) 0.2188(4) 0.3360(2) 0.0299(9) Uani 1.00 d . . . N2 N 0.0892(1) 0.0746(4) 0.3736(2) 0.0288(8) Uani 1.00 d . . . C1 C -0.0386(2) -0.1167(6) 0.2845(4) 0.062(2) Uani 1.00 d . . . C2 C -0.0952(2) 0.4088(7) 0.2231(3) 0.057(2) Uani 1.00 d . . . C3 C 0.0008(2) 0.5144(6) 0.4053(4) 0.048(1) Uani 1.00 d . . . C4 C -0.0742(3) 0.2387(7) 0.3755(4) 0.067(2) Uani 1.00 d . . . C5 C 0.2210(2) 0.0690(7) 0.5363(3) 0.055(1) Uani 1.00 d . . . C6 C 0.1466(3) -0.2194(7) 0.4545(5) 0.080(2) Uani 1.00 d . . . C7 C 0.1851(2) -0.0294(8) 0.3672(4) 0.067(2) Uani 1.00 d . . . C8 C 0.0669(2) 0.1787(5) 0.3973(2) 0.028(1) Uani 1.00 d . . . C9 C 0.1040(2) 0.2381(5) 0.4881(2) 0.031(1) Uani 1.00 d . . . C10 C 0.1396(2) 0.3679(5) 0.5135(3) 0.041(1) Uani 1.00 d . . . C11 C 0.1743(2) 0.4166(7) 0.5986(3) 0.050(1) Uani 1.00 d . . . C12 C 0.1752(2) 0.3368(6) 0.6595(3) 0.048(1) Uani 1.00 d . . . C13 C 0.1389(2) 0.2099(7) 0.6331(3) 0.053(2) Uani 1.00 d . . . C14 C 0.1030(2) 0.1604(6) 0.5485(3) 0.044(1) Uani 1.00 d . . . C15 C 0.2163(3) 0.3893(9) 0.7534(3) 0.077(2) Uani 1.00 d . . . H1 H -0.115 0.323 0.186 0.069 Uiso 1.00 calc . . . H2 H -0.075 0.464 0.206 0.069 Uiso 1.00 calc . . . H3 H -0.124 0.473 0.219 0.069 Uiso 1.00 calc . . . H4 H -0.029 0.587 0.394 0.058 Uiso 1.00 calc . . . H5 H 0.025 0.559 0.393 0.058 Uiso 1.00 calc . . . H6 H 0.026 0.486 0.464 0.058 Uiso 1.00 calc . . . H7 H -0.099 0.307 0.379 0.081 Uiso 1.00 calc . . . H8 H -0.099 0.158 0.337 0.081 Uiso 1.00 calc . . . H9 H -0.044 0.197 0.431 0.081 Uiso 1.00 calc . . . H10 H 0.229 0.168 0.525 0.066 Uiso 1.00 calc . . . H11 H 0.210 0.079 0.572 0.066 Uiso 1.00 calc . . . H12 H 0.257 0.008 0.565 0.066 Uiso 1.00 calc . . . H13 H 0.137 -0.215 0.492 0.096 Uiso 1.00 calc . . . H14 H 0.183 -0.277 0.480 0.096 Uiso 1.00 calc . . . H15 H 0.114 -0.267 0.402 0.096 Uiso 1.00 calc . . . H16 H 0.219 -0.095 0.394 0.080 Uiso 1.00 calc . . . H17 H 0.153 -0.067 0.311 0.080 Uiso 1.00 calc . . . H18 H 0.196 0.071 0.363 0.080 Uiso 1.00 calc . . . H19 H 0.140 0.423 0.473 0.049 Uiso 1.00 calc . . . H20 H 0.198 0.507 0.615 0.060 Uiso 1.00 calc . . . H21 H 0.138 0.155 0.674 0.064 Uiso 1.00 calc . . . H22 H 0.078 0.073 0.532 0.053 Uiso 1.00 calc . . . H23 H 0.257 0.358 0.781 0.092 Uiso 1.00 calc . . . H24 H 0.215 0.498 0.756 0.092 Uiso 1.00 calc . . . H25 H 0.203 0.344 0.783 0.092 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta1 0.0314(1) 0.0290(2) 0.0247(1) -0.000 0.0100(1) 0.001 Si2 0.0332(6) 0.0396(7) 0.0315(6) 0.0042(5) 0.0192(5) 0.0003(5) Si3 0.0249(5) 0.0396(7) 0.0326(6) 0.0043(5) 0.0117(5) 0.0038(5) N1 0.028(2) 0.032(2) 0.024(2) -0.000(1) 0.013(1) 0.001(1) N2 0.027(2) 0.032(2) 0.021(2) 0.002(1) 0.011(1) 0.002(1) C1 0.039(3) 0.046(3) 0.066(3) -0.010(2) 0.016(3) 0.019(3) C2 0.051(3) 0.067(4) 0.038(3) 0.027(3) 0.020(2) 0.002(3) C3 0.053(3) 0.046(3) 0.048(3) 0.008(2) 0.032(3) 0.001(2) C4 0.066(3) 0.066(4) 0.096(5) -0.008(3) 0.064(4) -0.011(3) C5 0.025(2) 0.080(4) 0.038(3) 0.006(2) 0.008(2) -0.002(3) C6 0.047(3) 0.050(4) 0.102(5) 0.015(3) 0.026(3) 0.034(3) C7 0.038(3) 0.105(5) 0.053(3) 0.013(3) 0.026(3) -0.014(3) C8 0.026(2) 0.028(2) 0.025(2) -0.005(2) 0.013(2) 0.005(2) C9 0.028(2) 0.035(2) 0.025(2) -0.001(2) 0.015(2) 0.000(2) C10 0.041(2) 0.042(3) 0.030(2) -0.007(2) 0.017(2) 0.002(2) C11 0.043(3) 0.054(3) 0.041(3) -0.015(2) 0.020(2) -0.014(2) C12 0.039(2) 0.069(4) 0.030(2) -0.002(2) 0.017(2) -0.008(2) C13 0.050(3) 0.080(4) 0.026(2) -0.006(3) 0.022(2) 0.002(2) C14 0.042(2) 0.052(3) 0.034(2) -0.013(2) 0.021(2) -0.001(2) C15 0.062(4) 0.118(6) 0.033(3) -0.018(4) 0.021(3) -0.032(3) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TA1 N1 2.261(3) . . yes TA1 N1 2.261(3) . 2_555 yes TA1 N2 2.191(3) . . yes TA1 N2 2.191(3) . 2_555 yes TA1 C1 2.050(5) . . yes TA1 C1 2.050(5) . 2_555 yes SI2 N1 1.752(4) . . yes SI2 C2 1.867(5) . . yes SI2 C3 1.851(6) . . yes SI2 C4 1.851(6) . . yes SI3 N2 1.749(3) . . yes SI3 C5 1.863(5) . . yes SI3 C6 1.837(6) . . yes SI3 C7 1.869(6) . . yes N1 C8 1.312(5) . . yes N2 C8 1.348(5) . . yes C8 C9 1.500(5) . . yes C9 C10 1.384(6) . . yes C9 C14 1.393(6) . . yes C10 C11 1.387(6) . . yes C11 C12 1.380(7) . . yes C12 C13 1.372(8) . . yes C12 C15 1.527(6) . . yes C13 C14 1.380(6) . . yes C2 H1 0.950 . . no C2 H2 0.950 . . no C2 H3 0.950 . . no C3 H4 0.950 . . no C3 H5 0.950 . . no C3 H6 0.950 . . no C4 H7 0.950 . . no C4 H8 0.950 . . no C4 H9 0.950 . . no C5 H10 0.950 . . no C5 H11 0.950 . . no C5 H12 0.950 . . no C6 H13 0.950 . . no C6 H14 0.950 . . no C6 H15 0.950 . . no C7 H16 0.950 . . no C7 H17 0.950 . . no C7 H18 0.950 . . no C10 H19 0.950 . . no C11 H20 0.950 . . no C13 H21 0.950 . . no C14 H22 0.950 . . no C15 H23 0.950 . . no C15 H24 0.950 . . no C15 H25 0.950 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 TA1 N1 85.9(2) . 1_555 2_555 ? N1 TA1 N2 60.4(1) . . . ? N1 TA1 N2 103.2(1) . 1_555 2_555 ? N1 TA1 C1 92.7(2) . . . ? N1 TA1 C1 149.4(2) . 1_555 2_555 ? N2 TA1 N2 159.1(2) . 1_555 2_555 ? N2 TA1 C1 102.6(2) . . . ? N2 TA1 C1 90.4(2) . 1_555 2_555 ? C1 TA1 C1 103.3(4) . 1_555 2_555 ? N1 SI2 C2 105.6(2) . . . ? N1 SI2 C3 113.4(2) . . . ? N1 SI2 C4 109.7(2) . . . ? C2 SI2 C3 107.8(3) . . . ? C2 SI2 C4 111.7(3) . . . ? C3 SI2 C4 108.7(3) . . . ? N2 SI3 C5 114.8(2) . . . ? N2 SI3 C6 109.1(2) . . . ? N2 SI3 C7 108.1(2) . . . ? C5 SI3 C6 109.3(3) . . . ? C5 SI3 C7 105.1(3) . . . ? C6 SI3 C7 110.4(3) . . . ? TA1 N1 SI2 136.5(2) . . . ? TA1 N1 C8 90.9(3) . . . ? SI2 N1 C8 131.2(3) . . . ? TA1 N2 SI3 133.0(2) . . . ? TA1 N2 C8 93.0(2) . . . ? SI3 N2 C8 131.7(3) . . . ? N1 C8 N2 114.7(3) . . . ? N1 C8 C9 123.7(4) . . . ? N2 C8 C9 121.6(3) . . . ? C8 C9 C10 121.6(4) . . . ? C8 C9 C14 119.4(4) . . . ? C10 C9 C14 119.0(4) . . . ? C9 C10 C11 119.6(4) . . . ? C10 C11 C12 121.6(5) . . . ? C11 C12 C13 118.2(4) . . . ? C11 C12 C15 120.2(5) . . . ? C13 C12 C15 121.6(5) . . . ? C12 C13 C14 121.5(4) . . . ? C9 C14 C13 120.0(4) . . . ? SI2 C2 H1 109.480 . . . no SI2 C2 H2 109.471 . . . no SI2 C2 H3 109.467 . . . no H1 C2 H2 109.479 . . . no H1 C2 H3 109.473 . . . no H2 C2 H3 109.456 . . . no SI2 C3 H4 109.473 . . . no SI2 C3 H5 109.468 . . . no SI2 C3 H6 109.469 . . . no H4 C3 H5 109.473 . . . no H4 C3 H6 109.476 . . . no H5 C3 H6 109.468 . . . no SI2 C4 H7 109.471 . . . no SI2 C4 H8 109.479 . . . no SI2 C4 H9 109.476 . . . no H7 C4 H8 109.468 . . . no H7 C4 H9 109.462 . . . no H8 C4 H9 109.472 . . . no SI3 C5 H10 109.475 . . . no SI3 C5 H11 109.466 . . . no SI3 C5 H12 109.467 . . . no H10 C5 H11 109.476 . . . no H10 C5 H12 109.478 . . . no H11 C5 H12 109.465 . . . no SI3 C6 H13 109.465 . . . no SI3 C6 H14 109.458 . . . no SI3 C6 H15 109.465 . . . no H13 C6 H14 109.476 . . . no H13 C6 H15 109.487 . . . no H14 C6 H15 109.477 . . . no SI3 C7 H16 109.477 . . . no SI3 C7 H17 109.469 . . . no SI3 C7 H18 109.467 . . . no H16 C7 H17 109.478 . . . no H16 C7 H18 109.475 . . . no H17 C7 H18 109.462 . . . no C9 C10 H19 120.207 . . . no C11 C10 H19 120.203 . . . no C10 C11 H20 119.184 . . . no C12 C11 H20 119.181 . . . no C12 C13 H21 119.239 . . . no C14 C13 H21 119.243 . . . no C9 C14 H22 120.004 . . . no C13 C14 H22 120.001 . . . no C12 C15 H23 109.466 . . . no C12 C15 H24 109.464 . . . no C12 C15 H25 109.465 . . . no H23 C15 H24 109.480 . . . no H23 C15 H25 109.478 . . . no H24 C15 H25 109.475 . . . no #------------------------------------------------------------------------------ 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 TA1 N1 SI2 C2 -42.6(3) 1_555 1_555 1_555 1_555 yes TA1 N1 SI2 C3 -160.4(3) 1_555 1_555 1_555 1_555 yes TA1 N1 SI2 C4 77.9(3) 1_555 1_555 1_555 1_555 yes TA1 N1 C8 N2 9.8(3) 1_555 1_555 1_555 1_555 yes TA1 N1 C8 C9 -168.1(3) 1_555 1_555 1_555 1_555 yes TA1 N1 SI2 C2 -42.6(3) 1_555 2_555 2_555 2_555 yes TA1 N1 SI2 C3 -160.4(3) 1_555 2_555 2_555 2_555 yes TA1 N1 SI2 C4 77.9(3) 1_555 2_555 2_555 2_555 yes TA1 N1 C8 N2 9.8(3) 1_555 2_555 2_555 2_555 yes TA1 N1 C8 C9 -168.1(3) 1_555 2_555 2_555 2_555 yes TA1 N2 SI3 C5 -179.9(3) 1_555 1_555 1_555 1_555 yes TA1 N2 SI3 C6 -56.9(4) 1_555 1_555 1_555 1_555 yes TA1 N2 SI3 C7 63.2(3) 1_555 1_555 1_555 1_555 yes TA1 N2 C8 N1 -10.1(3) 1_555 1_555 1_555 1_555 yes TA1 N2 C8 C9 167.8(3) 1_555 1_555 1_555 1_555 yes TA1 N2 SI3 C5 -179.9(3) 1_555 2_555 2_555 2_555 yes TA1 N2 SI3 C6 -56.9(4) 1_555 2_555 2_555 2_555 yes TA1 N2 SI3 C7 63.2(3) 1_555 2_555 2_555 2_555 yes TA1 N2 C8 N1 -10.1(3) 1_555 2_555 2_555 2_555 yes TA1 N2 C8 C9 167.8(3) 1_555 2_555 2_555 2_555 yes SI2 N1 TA1 N1 79.4(2) 1_555 1_555 1_555 2_555 yes SI2 N1 TA1 N2 -172.9(3) 1_555 1_555 1_555 1_555 yes SI2 N1 TA1 N2 21.1(3) 1_555 1_555 1_555 2_555 yes SI2 N1 TA1 C1 -69.9(3) 1_555 1_555 1_555 1_555 yes SI2 N1 TA1 C1 167.8(4) 1_555 1_555 1_555 2_555 yes SI2 N1 C8 N2 177.5(3) 1_555 1_555 1_555 1_555 yes SI2 N1 C8 C9 -0.4(6) 1_555 1_555 1_555 1_555 yes SI3 N2 TA1 N1 169.8(3) 1_555 1_555 1_555 1_555 yes SI3 N2 TA1 N1 -112.8(2) 1_555 1_555 1_555 2_555 yes SI3 N2 TA1 N2 -148.9(2) 1_555 1_555 1_555 2_555 yes SI3 N2 TA1 C1 83.8(3) 1_555 1_555 1_555 1_555 yes SI3 N2 TA1 C1 -19.9(3) 1_555 1_555 1_555 2_555 yes SI3 N2 C8 N1 -174.1(3) 1_555 1_555 1_555 1_555 yes SI3 N2 C8 C9 3.8(6) 1_555 1_555 1_555 1_555 yes N1 TA1 N1 C8 -114.0(3) 1_555 1_555 2_555 2_555 yes N1 TA1 N2 C8 6.1(2) 1_555 1_555 1_555 1_555 yes N1 TA1 N2 C8 83.5(2) 1_555 1_555 2_555 2_555 yes N1 C8 C9 C10 -91.3(5) 1_555 1_555 1_555 1_555 yes N1 C8 C9 C14 89.2(5) 1_555 1_555 1_555 1_555 yes N2 TA1 N1 C8 -6.3(2) 1_555 1_555 1_555 1_555 yes N2 TA1 N1 C8 -172.3(2) 1_555 1_555 2_555 2_555 yes N2 TA1 N2 C8 47.4(2) 1_555 1_555 2_555 2_555 yes N2 C8 C9 C10 91.0(5) 1_555 1_555 1_555 1_555 yes N2 C8 C9 C14 -88.6(5) 1_555 1_555 1_555 1_555 yes C1 TA1 N1 C8 96.7(3) 1_555 1_555 1_555 1_555 yes C1 TA1 N1 C8 -25.5(5) 1_555 1_555 2_555 2_555 yes C1 TA1 N2 C8 -79.8(3) 1_555 1_555 1_555 1_555 yes C1 TA1 N2 C8 176.4(3) 1_555 1_555 2_555 2_555 yes C2 SI2 N1 C8 155.4(4) 1_555 1_555 1_555 1_555 yes C3 SI2 N1 C8 37.6(4) 1_555 1_555 1_555 1_555 yes C4 SI2 N1 C8 -84.2(4) 1_555 1_555 1_555 1_555 yes C5 SI3 N2 C8 -22.0(5) 1_555 1_555 1_555 1_555 yes C6 SI3 N2 C8 101.0(4) 1_555 1_555 1_555 1_555 yes C7 SI3 N2 C8 -138.9(4) 1_555 1_555 1_555 1_555 yes C8 C9 C10 C11 -178.5(4) 1_555 1_555 1_555 1_555 yes C8 C9 C14 C13 177.2(5) 1_555 1_555 1_555 1_555 yes C9 C10 C11 C12 1.4(8) 1_555 1_555 1_555 1_555 yes C9 C14 C13 C12 1.2(8) 1_555 1_555 1_555 1_555 yes C10 C9 C14 C13 -2.3(7) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C13 -2.5(8) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C15 177.0(5) 1_555 1_555 1_555 1_555 yes C11 C10 C9 C14 1.0(7) 1_555 1_555 1_555 1_555 yes C11 C12 C13 C14 1.2(8) 1_555 1_555 1_555 1_555 yes C14 C13 C12 C15 -178.3(5) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C1 C3 3.742(7) . 1_545 ? C3 C3 3.794(10) . 3_566 ? C5 C15 3.711(7) . 6_546 ? C6 C10 3.828(7) . 1_545 ? C7 C11 3.718(8) . 7_556 ? #------------------------------------------------------------------------------ # Attachment 'tasulf.cif' data_bis_amidinate_tantalum_sul _database_code_depnum_ccdc_archive 'CCDC 283321' _audit_creation_date 'Tue Oct 4 10:27:11 2005' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Blessing, R. H., (1995), Acta Crystallogr, A51, 33-38. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C29 H53 N4 S Si4 Ta ' _chemical_formula_moiety 'C29 H53 N4 S Si4 Ta ' _chemical_formula_weight 783.11 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 28.2627(4) _cell_length_b 8.7781(2) _cell_length_c 19.8801(3) _cell_angle_alpha 90 _cell_angle_beta 129.253(1) _cell_angle_gamma 90 _cell_volume 3819.2(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6047 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24.5 _cell_measurement_temperature 166.2 #------------------------------------------------------------------------------ _exptl_crystal_description blocklike _exptl_crystal_colour yellow _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600.00 _exptl_absorpt_coefficient_mu 3.077 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_T_max 0.500 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scans _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8561 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 24.68 _diffrn_measured_fraction_theta_max 0.9644 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.9644 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). The tantalum lies on the crystallographic two-fold axis, causing the methyl group and the sulfido group to be disordered. They were refined at half-occupancy. No hydrogen atom positions were calculated for the methyl carbon. ; _reflns_number_total 3139 _reflns_number_gt 2646 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0402 _refine_ls_R_factor_all 0.0400 _refine_ls_wR_factor_all 0.0421 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2646 _refine_ls_number_parameters 181 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0051 _refine_diff_density_max 0.70 _refine_diff_density_min -2.37 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si Si 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ta Ta -0.705 6.523 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-AXS SMART v5.054' _computing_cell_refinement 'Bruker-AXS SAINT v6.40' _computing_data_reduction 'Bruker-AXS SAINT v6.40' _computing_structure_solution SIR92 _computing_structure_refinement teXsan _computing_publication_material teXsan _computing_molecular_graphics ? #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 1.000 0.97105(3) 0.250 0.04081(9) Uani 1.00 d S . . S1 S 0.9624(4) 1.145(1) 0.2860(5) 0.073(1) Uani 0.50 d P . . Si1 Si 0.96048(6) 0.6578(2) 0.33507(8) 0.0392(3) Uani 1.00 d . . . Si2 Si 1.15817(6) 1.0210(2) 0.43333(8) 0.0414(3) Uani 1.00 d . . . N1 N 1.0082(2) 0.7829(4) 0.3338(2) 0.0320(9) Uani 1.00 d . . . N2 N 1.0881(2) 0.9209(5) 0.3710(2) 0.0332(9) Uani 1.00 d . . . C1 C 1.0658(2) 0.8206(5) 0.3955(3) 0.032(1) Uani 1.00 d . . . C2 C 0.9220(3) 0.7623(8) 0.3700(4) 0.072(2) Uani 1.00 d . . . C3 C 0.9043(3) 0.5868(8) 0.2211(3) 0.059(2) Uani 1.00 d . . . C4 C 1.0017(3) 0.4902(6) 0.4072(4) 0.055(2) Uani 1.00 d . . . C5 C 1.2210(2) 0.9285(8) 0.5376(3) 0.062(2) Uani 1.00 d . . . C6 C 1.1858(3) 1.0297(9) 0.3698(4) 0.073(2) Uani 1.00 d . . . C7 C 1.1449(3) 1.2133(7) 0.4561(5) 0.084(2) Uani 1.00 d . . . C8 C 1.1030(2) 0.7631(5) 0.4866(3) 0.035(1) Uani 1.00 d . . . C9 C 1.1403(2) 0.6348(6) 0.5145(3) 0.045(1) Uani 1.00 d . . . C10 C 1.1749(2) 0.5888(7) 0.5996(3) 0.054(1) Uani 1.00 d . . . C11 C 1.1745(2) 0.6648(7) 0.6590(3) 0.053(2) Uani 1.00 d . . . C12 C 1.1367(3) 0.7891(7) 0.6314(3) 0.058(2) Uani 1.00 d . . . C13 C 1.1009(2) 0.8389(7) 0.5460(3) 0.047(1) Uani 1.00 d . . . C14 C 1.2155(3) 0.6142(10) 0.7537(3) 0.078(2) Uani 1.00 d . . . C15 C 1.035(2) 1.141(5) 0.204(2) 0.061(9) Uiso 0.50 d P . . H1 H 0.898 0.842 0.330 0.086 Uiso 1.00 calc . . . H3 H 0.897 0.694 0.372 0.086 Uiso 1.00 calc . . . H6 H 1.031 0.524 0.466 0.065 Uiso 1.00 calc . . . H7 H 1.021 0.437 0.390 0.065 Uiso 1.00 calc . . . H8 H 1.210 0.924 0.574 0.074 Uiso 1.00 calc . . . H9 H 1.227 0.828 0.527 0.074 Uiso 1.00 calc . . . H10 H 1.155 1.071 0.314 0.088 Uiso 1.00 calc . . . H11 H 1.221 1.092 0.399 0.088 Uiso 1.00 calc . . . H12 H 1.180 1.274 0.482 0.101 Uiso 1.00 calc . . . H13 H 1.111 1.259 0.403 0.101 Uiso 1.00 calc . . . H14 H 1.142 0.579 0.475 0.053 Uiso 1.00 calc . . . H15 H 1.200 0.501 0.618 0.065 Uiso 1.00 calc . . . H16 H 1.135 0.842 0.672 0.070 Uiso 1.00 calc . . . H17 H 1.075 0.925 0.528 0.057 Uiso 1.00 calc . . . H18 H 1.256 0.647 0.782 0.094 Uiso 1.00 calc . . . H19 H 1.215 0.506 0.756 0.094 Uiso 1.00 calc . . . H20 H 1.201 0.657 0.782 0.094 Uiso 1.00 calc . . . H21 H 1.257 0.986 0.565 0.074 Uiso 1.00 calc . . . H22 H 1.196 0.930 0.364 0.088 Uiso 1.00 calc . . . H23 H 1.136 1.206 0.495 0.101 Uiso 1.00 calc . . . H25 H 0.973 0.424 0.403 0.065 Uiso 1.00 calc . . . H26 H 0.878 0.514 0.218 0.071 Uiso 1.00 calc . . . H27 H 0.926 0.540 0.204 0.071 Uiso 1.00 calc . . . H28 H 0.881 0.670 0.184 0.071 Uiso 1.00 calc . . . H29 H 0.952 0.805 0.426 0.086 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta1 0.0473(2) 0.0250(2) 0.0270(2) -0.003 0.0126(1) -0.005 S1 0.042(2) 0.079(4) 0.056(3) 0.012(2) 0.010(2) -0.032(3) Si1 0.0409(7) 0.0405(8) 0.0361(6) -0.0038(5) 0.0244(6) -0.0002(6) Si2 0.0292(6) 0.0436(8) 0.0361(7) -0.0063(5) 0.0133(5) -0.0081(6) N1 0.034(2) 0.030(2) 0.028(2) -0.002(2) 0.018(2) -0.003(2) N2 0.030(2) 0.032(2) 0.030(2) 0.001(2) 0.015(2) -0.000(2) C1 0.036(2) 0.028(2) 0.030(2) 0.004(2) 0.020(2) -0.006(2) C2 0.075(4) 0.070(4) 0.095(5) 0.013(3) 0.066(4) 0.011(4) C3 0.058(3) 0.065(4) 0.042(3) -0.025(3) 0.026(3) -0.004(3) C4 0.063(3) 0.049(3) 0.053(3) -0.000(3) 0.038(3) 0.010(3) C5 0.037(3) 0.079(4) 0.038(3) -0.006(3) 0.009(2) -0.004(3) C6 0.043(3) 0.110(6) 0.052(3) -0.019(3) 0.023(3) 0.002(3) C7 0.063(4) 0.042(4) 0.109(5) -0.013(3) 0.036(4) -0.031(4) C8 0.039(2) 0.034(3) 0.029(2) 0.003(2) 0.019(2) -0.001(2) C9 0.051(3) 0.043(3) 0.034(2) 0.013(2) 0.025(2) 0.001(2) C10 0.051(3) 0.056(3) 0.046(3) 0.020(3) 0.026(2) 0.020(3) C11 0.047(3) 0.074(4) 0.032(2) 0.003(3) 0.022(2) 0.010(3) C12 0.065(3) 0.079(4) 0.033(2) 0.006(3) 0.032(3) -0.006(3) C13 0.049(3) 0.058(3) 0.035(2) 0.012(2) 0.026(2) -0.003(2) C14 0.072(4) 0.114(6) 0.032(3) 0.007(4) 0.025(3) 0.015(3) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TA1 S1 2.223(9) . . yes TA1 S1 2.223(9) . 2_755 yes TA1 N1 2.251(4) . . yes TA1 N1 2.251(4) . 2_755 yes TA1 N2 2.144(3) . . yes TA1 N2 2.144(3) . 2_755 yes TA1 C15 2.27(4) . . yes TA1 C15 2.27(4) . 2_755 yes S1 C15 0.17(4) . 2_755 yes SI1 N1 1.753(4) . . yes SI1 C2 1.862(6) . . yes SI1 C3 1.868(5) . . yes SI1 C4 1.861(6) . . yes SI2 N2 1.768(4) . . yes SI2 C5 1.858(6) . . yes SI2 C6 1.861(7) . . yes SI2 C7 1.847(7) . . yes N1 C1 1.318(5) . . yes N2 C1 1.339(6) . . yes C1 C8 1.494(6) . . yes C8 C9 1.395(7) . . yes C8 C13 1.388(6) . . yes C9 C10 1.375(7) . . yes C10 C11 1.362(8) . . yes C11 C12 1.374(8) . . yes C11 C14 1.524(7) . . yes C12 C13 1.386(7) . . yes C2 H1 0.950 . . no C2 H3 0.950 . . no C2 H29 0.950 . . no C3 H26 0.950 . . no C3 H27 0.950 . . no C3 H28 0.950 . . no C4 H6 0.950 . . no C4 H7 0.950 . . no C4 H25 0.950 . . no C5 H8 0.950 . . no C5 H9 0.950 . . no C5 H21 0.950 . . no C6 H10 0.950 . . no C6 H11 0.950 . . no C6 H22 0.950 . . no C7 H12 0.950 . . no C7 H13 0.950 . . no C7 H23 0.950 . . no C9 H14 0.950 . . no C10 H15 0.950 . . no C12 H16 0.950 . . no C13 H17 0.950 . . no C14 H18 0.950 . . no C14 H19 0.950 . . no C14 H20 0.950 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 TA1 S1 93.0(6) . 1_555 2_755 ? S1 TA1 N1 96.5(3) . . . ? S1 TA1 N1 153.7(2) . 1_555 2_755 ? S1 TA1 N2 103.4(2) . . . ? S1 TA1 N2 92.9(2) . 1_555 2_755 ? S1 TA1 C15 95.4(7) . . . ? S1 TA1 C15 4(1) . 1_555 2_755 ? N1 TA1 N1 85.6(2) . 1_555 2_755 ? N1 TA1 N2 61.1(1) . . . ? N1 TA1 N2 100.5(1) . 1_555 2_755 ? N1 TA1 C15 155.7(9) . . . ? N1 TA1 C15 93.0(9) . 1_555 2_755 ? N2 TA1 N2 156.3(2) . 1_555 2_755 ? N2 TA1 C15 95.6(9) . . . ? N2 TA1 C15 99.9(9) . 1_555 2_755 ? C15 TA1 C15 97(1) . 1_555 2_755 ? TA1 S1 C15 104(17) . 1_555 2_755 ? N1 SI1 C2 109.5(2) . . . ? N1 SI1 C3 105.3(2) . . . ? N1 SI1 C4 113.2(2) . . . ? C2 SI1 C3 111.6(3) . . . ? C2 SI1 C4 109.3(3) . . . ? C3 SI1 C4 108.0(3) . . . ? N2 SI2 C5 114.8(2) . . . ? N2 SI2 C6 108.1(2) . . . ? N2 SI2 C7 108.4(2) . . . ? C5 SI2 C6 105.1(3) . . . ? C5 SI2 C7 108.9(3) . . . ? C6 SI2 C7 111.5(4) . . . ? TA1 N1 SI1 138.6(2) . . . ? TA1 N1 C1 89.5(3) . . . ? SI1 N1 C1 130.8(3) . . . ? TA1 N2 SI2 132.4(2) . . . ? TA1 N2 C1 93.7(2) . . . ? SI2 N2 C1 130.4(3) . . . ? N1 C1 N2 114.5(4) . . . ? N1 C1 C8 123.3(4) . . . ? N2 C1 C8 122.1(4) . . . ? C1 C8 C9 121.9(4) . . . ? C1 C8 C13 119.6(4) . . . ? C9 C8 C13 118.5(4) . . . ? C8 C9 C10 119.8(4) . . . ? C9 C10 C11 122.2(5) . . . ? C10 C11 C12 118.2(4) . . . ? C10 C11 C14 120.7(5) . . . ? C12 C11 C14 121.1(5) . . . ? C11 C12 C13 121.3(5) . . . ? C8 C13 C12 120.0(5) . . . ? TA1 C15 S1 71(17) . 1_555 2_755 ? SI1 C2 H1 109.471 . . . no SI1 C2 H3 109.471 . . . no SI1 C2 H29 109.471 . . . no H1 C2 H3 109.470 . . . no H1 C2 H29 109.473 . . . no H3 C2 H29 109.473 . . . no SI1 C3 H26 109.469 . . . no SI1 C3 H27 109.470 . . . no SI1 C3 H28 109.470 . . . no H26 C3 H27 109.471 . . . no H26 C3 H28 109.473 . . . no H27 C3 H28 109.474 . . . no SI1 C4 H6 109.469 . . . no SI1 C4 H7 109.469 . . . no SI1 C4 H25 109.470 . . . no H6 C4 H7 109.472 . . . no H6 C4 H25 109.474 . . . no H7 C4 H25 109.472 . . . no SI2 C5 H8 109.470 . . . no SI2 C5 H9 109.471 . . . no SI2 C5 H21 109.469 . . . no H8 C5 H9 109.473 . . . no H8 C5 H21 109.470 . . . no H9 C5 H21 109.474 . . . no SI2 C6 H10 109.468 . . . no SI2 C6 H11 109.467 . . . no SI2 C6 H22 109.470 . . . no H10 C6 H11 109.471 . . . no H10 C6 H22 109.475 . . . no H11 C6 H22 109.475 . . . no SI2 C7 H12 109.468 . . . no SI2 C7 H13 109.469 . . . no SI2 C7 H23 109.466 . . . no H12 C7 H13 109.477 . . . no H12 C7 H23 109.474 . . . no H13 C7 H23 109.474 . . . no C8 C9 H14 120.115 . . . no C10 C9 H14 120.117 . . . no C9 C10 H15 118.902 . . . no C11 C10 H15 118.902 . . . no C11 C12 H16 119.338 . . . no C13 C12 H16 119.337 . . . no C8 C13 H17 120.015 . . . no C12 C13 H17 120.016 . . . no C11 C14 H18 109.470 . . . no C11 C14 H19 109.470 . . . no C11 C14 H20 109.470 . . . no H18 C14 H19 109.473 . . . no H18 C14 H20 109.471 . . . no H19 C14 H20 109.473 . . . no #------------------------------------------------------------------------------ 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 TA1 N1 SI1 C2 -76.4(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C3 43.7(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C4 161.4(3) 1_555 1_555 1_555 1_555 yes TA1 N1 C1 N2 -10.2(4) 1_555 1_555 1_555 1_555 yes TA1 N1 C1 C8 166.9(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C2 -76.4(4) 1_555 2_755 2_755 2_755 yes TA1 N1 SI1 C3 43.7(4) 1_555 2_755 2_755 2_755 yes TA1 N1 SI1 C4 161.4(3) 1_555 2_755 2_755 2_755 yes TA1 N1 C1 N2 -10.2(4) 1_555 2_755 2_755 2_755 yes TA1 N1 C1 C8 166.9(4) 1_555 2_755 2_755 2_755 yes TA1 N2 SI2 C5 177.5(3) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C6 -65.5(4) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C7 55.5(4) 1_555 1_555 1_555 1_555 yes TA1 N2 C1 N1 10.7(4) 1_555 1_555 1_555 1_555 yes TA1 N2 C1 C8 -166.4(3) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C5 177.5(3) 1_555 2_755 2_755 2_755 yes TA1 N2 SI2 C6 -65.5(4) 1_555 2_755 2_755 2_755 yes TA1 N2 SI2 C7 55.5(4) 1_555 2_755 2_755 2_755 yes TA1 N2 C1 N1 10.7(4) 1_555 2_755 2_755 2_755 yes TA1 N2 C1 C8 -166.4(3) 1_555 2_755 2_755 2_755 yes S1 TA1 S1 C15 -124(15) 1_555 1_555 2_755 1_555 yes S1 TA1 N1 SI1 73.5(3) 1_555 1_555 1_555 1_555 yes S1 TA1 N1 C1 -95.2(3) 1_555 1_555 1_555 1_555 yes S1 TA1 N1 SI1 -176.0(7) 1_555 1_555 2_755 2_755 yes S1 TA1 N1 C1 15.3(8) 1_555 1_555 2_755 2_755 yes S1 TA1 N2 SI2 -76.1(4) 1_555 1_555 1_555 1_555 yes S1 TA1 N2 C1 83.6(4) 1_555 1_555 1_555 1_555 yes S1 TA1 N2 SI2 17.7(4) 1_555 1_555 2_755 2_755 yes S1 TA1 N2 C1 177.4(4) 1_555 1_555 2_755 2_755 yes S1 C15 TA1 N1 -149(15) 1_555 2_755 1_555 1_555 yes S1 C15 TA1 N1 -63(16) 1_555 2_755 1_555 2_755 yes S1 C15 TA1 N2 149(15) 1_555 2_755 1_555 1_555 yes S1 C15 TA1 N2 -48(15) 1_555 2_755 1_555 2_755 yes S1 C15 TA1 C15 52(15) 1_555 2_755 1_555 1_555 yes SI1 N1 TA1 N1 -80.2(3) 1_555 1_555 1_555 2_755 yes SI1 N1 TA1 N2 175.2(3) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 N2 -20.7(3) 1_555 1_555 1_555 2_755 yes SI1 N1 TA1 C15 -167(2) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 C15 75.5(9) 1_555 1_555 1_555 2_755 yes SI1 N1 C1 N2 179.7(3) 1_555 1_555 1_555 1_555 yes SI1 N1 C1 C8 -3.2(6) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N1 -166.1(3) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N1 114.9(3) 1_555 1_555 1_555 2_755 yes SI2 N2 TA1 N2 151.6(3) 1_555 1_555 1_555 2_755 yes SI2 N2 TA1 C15 20.8(10) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 C15 -78.2(10) 1_555 1_555 1_555 2_755 yes SI2 N2 C1 N1 171.0(3) 1_555 1_555 1_555 1_555 yes SI2 N2 C1 C8 -6.1(6) 1_555 1_555 1_555 1_555 yes N1 TA1 S1 C15 30(15) 1_555 1_555 1_555 2_755 yes N1 TA1 S1 C15 123(15) 1_555 1_555 2_755 1_555 yes N1 TA1 N1 C1 111.1(3) 1_555 1_555 2_755 2_755 yes N1 TA1 N2 C1 -6.5(2) 1_555 1_555 1_555 1_555 yes N1 TA1 N2 C1 -85.5(3) 1_555 1_555 2_755 2_755 yes N1 C1 C8 C9 94.4(5) 1_555 1_555 1_555 1_555 yes N1 C1 C8 C13 -85.9(6) 1_555 1_555 1_555 1_555 yes N2 TA1 S1 C15 -31(15) 1_555 1_555 1_555 2_755 yes N2 TA1 S1 C15 131(15) 1_555 1_555 2_755 1_555 yes N2 TA1 N1 C1 6.6(2) 1_555 1_555 1_555 1_555 yes N2 TA1 N1 C1 170.6(2) 1_555 1_555 2_755 2_755 yes N2 TA1 N2 C1 -48.7(2) 1_555 1_555 2_755 2_755 yes N2 C1 C8 C9 -88.7(6) 1_555 1_555 1_555 1_555 yes N2 C1 C8 C13 91.0(6) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C15 23(2) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C15 -93.1(9) 1_555 1_555 1_555 2_755 yes C1 N1 SI1 C2 88.5(4) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C3 -151.4(4) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C4 -33.7(5) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C15 -179.6(9) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C15 81.4(10) 1_555 1_555 1_555 2_755 yes C1 N2 SI2 C5 24.6(5) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C6 141.6(4) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C7 -97.4(5) 1_555 1_555 1_555 1_555 yes C1 C8 C9 C10 178.2(5) 1_555 1_555 1_555 1_555 yes C1 C8 C13 C12 -178.0(5) 1_555 1_555 1_555 1_555 yes C8 C9 C10 C11 -0.2(9) 1_555 1_555 1_555 1_555 yes C8 C13 C12 C11 -0.2(9) 1_555 1_555 1_555 1_555 yes C9 C8 C13 C12 1.7(8) 1_555 1_555 1_555 1_555 yes C9 C10 C11 C12 1.7(9) 1_555 1_555 1_555 1_555 yes C9 C10 C11 C14 -177.5(6) 1_555 1_555 1_555 1_555 yes C10 C9 C8 C13 -1.5(8) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C13 -1.5(9) 1_555 1_555 1_555 1_555 yes C13 C12 C11 C14 177.7(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S1 C4 3.58(1) . 1_565 ? C4 C15 3.53(4) . 2_745 ? data_tantalum_ketenimine _database_code_depnum_ccdc_archive 'CCDC 283322' _audit_creation_date 'Wed Sep 28 15:49:12 2005' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C39 H64 N5 Si4 Ta ' _chemical_formula_moiety 'C39 H64 N5 Si4 Ta ' _chemical_formula_weight 896.26 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? #------------------------------------------------------------------------------ loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 17.9014(4) _cell_length_b 11.6015(2) _cell_length_c 23.0038(5) _cell_angle_alpha 90 _cell_angle_beta 111.041(1) _cell_angle_gamma 90 _cell_volume 4459.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7933 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 22.5 _cell_measurement_temperature 170.2 #------------------------------------------------------------------------------ _exptl_crystal_description blocklike _exptl_crystal_colour orange _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.120 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848.00 _exptl_absorpt_coefficient_mu 2.600 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.517 _exptl_absorpt_correction_T_max 0.636 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scans _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21557 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_max 26.02 _diffrn_measured_fraction_theta_max 0.8969 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.8969 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7890 _reflns_number_gt 4578 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0316 _refine_ls_R_factor_all 0.0645 _refine_ls_wR_factor_all 0.0430 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4578 _refine_ls_number_parameters 442 _refine_ls_goodness_of_fit_ref 0.838 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0023 _refine_diff_density_max 0.69 _refine_diff_density_min -0.65 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Si Si 0.082 0.070 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ta Ta -0.705 6.523 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ _computing_data_collection 'Bruker-AXS SMART v5.054' _computing_cell_refinement 'Bruker-AXS SAINT v6.40' _computing_data_reduction 'Bruker-AXS SAINT v6.40' _computing_structure_solution SAPI91 _computing_structure_refinement teXsan _computing_publication_material teXsan _computing_molecular_graphics ? #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.27735(1) 0.49397(2) 0.742845(9) 0.02368(5) Uani 1.00 d . . . Si1 Si 0.3635(1) 0.7409(1) 0.83718(7) 0.0328(4) Uani 1.00 d . . . Si2 Si 0.2686(1) 0.2969(1) 0.87609(8) 0.0415(5) Uani 1.00 d . . . Si3 Si 0.06974(9) 0.5087(2) 0.71534(8) 0.0418(5) Uani 1.00 d . . . Si4 Si 0.2879(1) 0.1953(1) 0.67682(8) 0.0349(5) Uani 1.00 d . . . N1 N 0.3190(3) 0.6021(3) 0.8225(2) 0.027(1) Uani 1.00 d . . . N2 N 0.2842(3) 0.4210(4) 0.8374(2) 0.031(1) Uani 1.00 d . . . N3 N 0.1543(3) 0.4367(4) 0.7129(2) 0.028(1) Uani 1.00 d . . . N4 N 0.2441(3) 0.3169(3) 0.6976(2) 0.025(1) Uani 1.00 d . . . N5 N 0.2779(3) 0.5520(4) 0.6612(2) 0.026(1) Uani 1.00 d . . . C1 C 0.3099(3) 0.5234(4) 0.8626(2) 0.027(1) Uani 1.00 d . . . C2 C 0.2845(4) 0.8529(5) 0.8242(3) 0.045(2) Uani 1.00 d . . . C3 C 0.4187(4) 0.7621(5) 0.7832(3) 0.042(2) Uani 1.00 d . . . C4 C 0.4388(4) 0.7585(5) 0.9175(3) 0.039(2) Uani 1.00 d . . . C5 C 0.3668(5) 0.2199(5) 0.9141(3) 0.066(2) Uani 1.00 d . . . C6 C 0.2194(5) 0.3283(6) 0.9333(3) 0.061(3) Uani 1.00 d . . . C7 C 0.1999(4) 0.1985(5) 0.8178(3) 0.051(2) Uani 1.00 d . . . C8 C 0.3285(3) 0.5515(4) 0.9298(2) 0.028(1) Uani 1.00 d . . . C9 C 0.2835(3) 0.6325(5) 0.9478(2) 0.031(2) Uani 1.00 d . . . C10 C 0.3931(3) 0.4993(5) 0.9753(2) 0.031(1) Uani 1.00 d . . . C11 C 0.3029(4) 0.6610(5) 1.0101(3) 0.033(2) Uani 1.00 d . . . C12 C 0.4119(3) 0.5276(4) 1.0380(2) 0.030(1) Uani 1.00 d . . . C13 C 0.3661(3) 0.6087(5) 1.0556(2) 0.032(2) Uani 1.00 d . . . C14 C 0.3891(4) 0.6399(5) 1.1237(3) 0.043(2) Uani 1.00 d . . . C15 C 0.1678(4) 0.3417(5) 0.6834(2) 0.030(2) Uani 1.00 d . . . C16 C -0.0007(5) 0.555(1) 0.6381(4) 0.139(4) Uani 1.00 d . . . C17 C 0.1082(4) 0.6366(6) 0.7638(3) 0.059(2) Uani 1.00 d . . . C18 C 0.0142(7) 0.4255(7) 0.7552(6) 0.122(5) Uani 1.00 d . . . C19 C 0.3287(4) 0.2345(5) 0.6155(3) 0.051(2) Uani 1.00 d . . . C20 C 0.2182(4) 0.0706(5) 0.6503(3) 0.062(2) Uani 1.00 d . . . C21 C 0.3707(4) 0.1417(5) 0.7470(3) 0.048(2) Uani 1.00 d . . . C22 C 0.0996(3) 0.2785(4) 0.6349(3) 0.029(1) Uani 1.00 d . . . C23 C 0.0422(4) 0.2202(5) 0.6501(3) 0.042(2) Uani 1.00 d . . . C24 C 0.0965(4) 0.2783(5) 0.5735(3) 0.036(2) Uani 1.00 d . . . C25 C -0.0180(4) 0.1615(5) 0.6044(3) 0.045(2) Uani 1.00 d . . . C26 C 0.0358(4) 0.2200(5) 0.5285(3) 0.041(2) Uani 1.00 d . . . C27 C -0.0228(4) 0.1607(5) 0.5430(3) 0.041(2) Uani 1.00 d . . . C28 C -0.0889(4) 0.0956(6) 0.4934(3) 0.053(2) Uani 1.00 d . . . C29 C 0.2463(3) 0.6407(4) 0.6852(2) 0.027(2) Uani 1.00 d . . . C30 C 0.2162(4) 0.7451(4) 0.6602(3) 0.035(2) Uani 1.00 d . . . C31 C 0.2801(4) 0.5462(4) 0.5996(3) 0.030(2) Uani 1.00 d . . . C32 C 0.2085(4) 0.5470(5) 0.5478(3) 0.037(2) Uani 1.00 d . . . C33 C 0.3539(4) 0.5409(5) 0.5918(3) 0.038(2) Uani 1.00 d . . . C34 C 0.2134(5) 0.5368(5) 0.4879(3) 0.049(2) Uani 1.00 d . . . C35 C 0.3563(5) 0.5320(5) 0.5317(3) 0.049(2) Uani 1.00 d . . . C36 C 0.2853(5) 0.5288(6) 0.4805(3) 0.059(2) Uani 1.00 d . . . C37 C 0.1289(4) 0.5572(5) 0.5536(3) 0.044(2) Uani 1.00 d . . . C38 C 0.4335(4) 0.5480(6) 0.6454(3) 0.047(2) Uani 1.00 d . . . C39 C 0.4008(3) 0.4325(5) 0.7692(3) 0.034(2) Uani 1.00 d . . . H1 H 0.191 0.797 0.684 0.041 Uiso 1.00 calc . . . H2 H 0.220 0.778 0.619 0.041 Uiso 1.00 calc . . . H3 H 0.239 0.669 0.917 0.037 Uiso 1.00 calc . . . H4 H 0.425 0.444 0.964 0.037 Uiso 1.00 calc . . . H5 H 0.456 0.492 1.069 0.036 Uiso 1.00 calc . . . H6 H 0.044 0.220 0.692 0.051 Uiso 1.00 calc . . . H7 H -0.057 0.121 0.616 0.054 Uiso 1.00 calc . . . H8 H 0.034 0.220 0.487 0.049 Uiso 1.00 calc . . . H9 H 0.136 0.318 0.563 0.043 Uiso 1.00 calc . . . H10 H 0.272 0.717 1.021 0.040 Uiso 1.00 calc . . . H11 H 0.166 0.536 0.452 0.059 Uiso 1.00 calc . . . H12 H 0.287 0.521 0.440 0.071 Uiso 1.00 calc . . . H13 H 0.406 0.528 0.526 0.059 Uiso 1.00 calc . . . H14 H -0.139 0.126 0.490 0.064 Uiso 1.00 calc . . . H15 H -0.082 0.104 0.454 0.064 Uiso 1.00 calc . . . H16 H -0.086 0.016 0.504 0.064 Uiso 1.00 calc . . . H17 H 0.387 0.573 1.147 0.051 Uiso 1.00 calc . . . H18 H 0.442 0.670 1.139 0.051 Uiso 1.00 calc . . . H19 H 0.353 0.696 1.128 0.051 Uiso 1.00 calc . . . H20 H 0.253 0.378 0.965 0.074 Uiso 1.00 calc . . . H21 H 0.169 0.365 0.913 0.074 Uiso 1.00 calc . . . H22 H 0.211 0.258 0.952 0.074 Uiso 1.00 calc . . . H23 H 0.150 0.236 0.798 0.061 Uiso 1.00 calc . . . H24 H 0.223 0.178 0.788 0.061 Uiso 1.00 calc . . . H25 H 0.192 0.131 0.838 0.061 Uiso 1.00 calc . . . H26 H 0.413 0.750 0.947 0.047 Uiso 1.00 calc . . . H27 H 0.479 0.702 0.925 0.047 Uiso 1.00 calc . . . H28 H 0.462 0.833 0.922 0.047 Uiso 1.00 calc . . . H29 H 0.309 0.927 0.832 0.055 Uiso 1.00 calc . . . H30 H 0.249 0.850 0.782 0.055 Uiso 1.00 calc . . . H31 H 0.256 0.839 0.851 0.055 Uiso 1.00 calc . . . H32 H 0.459 0.704 0.791 0.050 Uiso 1.00 calc . . . H33 H 0.382 0.757 0.741 0.050 Uiso 1.00 calc . . . H34 H 0.443 0.836 0.790 0.050 Uiso 1.00 calc . . . H35 H 0.135 0.563 0.596 0.053 Uiso 1.00 calc . . . H36 H 0.102 0.624 0.532 0.053 Uiso 1.00 calc . . . H37 H 0.098 0.491 0.536 0.053 Uiso 1.00 calc . . . H38 H 0.359 0.153 0.935 0.079 Uiso 1.00 calc . . . H39 H 0.388 0.197 0.883 0.079 Uiso 1.00 calc . . . H40 H 0.404 0.270 0.943 0.079 Uiso 1.00 calc . . . H41 H 0.464 0.481 0.646 0.057 Uiso 1.00 calc . . . H42 H 0.462 0.614 0.640 0.057 Uiso 1.00 calc . . . H43 H 0.425 0.554 0.684 0.057 Uiso 1.00 calc . . . H44 H 0.142 0.613 0.804 0.071 Uiso 1.00 calc . . . H45 H 0.138 0.682 0.746 0.071 Uiso 1.00 calc . . . H46 H 0.065 0.680 0.766 0.071 Uiso 1.00 calc . . . H47 H -0.027 0.472 0.759 0.147 Uiso 1.00 calc . . . H48 H -0.009 0.359 0.731 0.147 Uiso 1.00 calc . . . H49 H 0.050 0.403 0.795 0.147 Uiso 1.00 calc . . . H50 H -0.045 0.593 0.643 0.167 Uiso 1.00 calc . . . H51 H 0.026 0.606 0.620 0.167 Uiso 1.00 calc . . . H52 H -0.019 0.489 0.612 0.167 Uiso 1.00 calc . . . H53 H 0.352 0.168 0.605 0.062 Uiso 1.00 calc . . . H54 H 0.287 0.262 0.580 0.062 Uiso 1.00 calc . . . H55 H 0.368 0.293 0.631 0.062 Uiso 1.00 calc . . . H56 H 0.199 0.049 0.682 0.074 Uiso 1.00 calc . . . H57 H 0.174 0.092 0.614 0.074 Uiso 1.00 calc . . . H58 H 0.246 0.007 0.641 0.074 Uiso 1.00 calc . . . H59 H 0.350 0.121 0.778 0.058 Uiso 1.00 calc . . . H60 H 0.395 0.076 0.736 0.058 Uiso 1.00 calc . . . H61 H 0.410 0.201 0.763 0.058 Uiso 1.00 calc . . . H62 H 0.417 0.399 0.810 0.041 Uiso 1.00 calc . . . H63 H 0.404 0.376 0.740 0.041 Uiso 1.00 calc . . . H64 H 0.435 0.495 0.770 0.041 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta1 0.0263(1) 0.0208(1) 0.0223(1) -0.0023(1) 0.00666(8) -0.0012(1) Si1 0.046(1) 0.0240(8) 0.0277(8) -0.0062(7) 0.0122(8) -0.0024(7) Si2 0.058(1) 0.0337(9) 0.0316(9) -0.0165(9) 0.0138(9) 0.0028(7) Si3 0.0271(8) 0.051(1) 0.0497(9) -0.0022(10) 0.0168(7) -0.012(1) Si4 0.0339(10) 0.0245(8) 0.0398(9) 0.0028(7) 0.0053(8) -0.0056(7) N1 0.040(3) 0.019(2) 0.023(2) -0.006(2) 0.013(2) -0.007(2) N2 0.037(3) 0.028(2) 0.028(3) -0.008(2) 0.010(2) -0.001(2) N3 0.023(3) 0.029(2) 0.036(3) -0.005(2) 0.015(2) -0.011(2) N4 0.025(3) 0.022(2) 0.024(2) -0.001(2) 0.005(2) -0.000(2) N5 0.025(3) 0.028(2) 0.018(2) 0.002(2) 0.001(2) -0.001(2) C1 0.020(3) 0.029(3) 0.028(3) -0.003(2) 0.004(2) -0.004(2) C2 0.059(5) 0.029(3) 0.045(4) 0.002(3) 0.014(3) -0.002(3) C3 0.044(4) 0.040(3) 0.041(4) -0.015(3) 0.014(3) -0.005(3) C4 0.045(4) 0.034(3) 0.036(3) -0.009(3) 0.012(3) -0.003(3) C5 0.092(6) 0.033(4) 0.051(4) -0.012(4) -0.000(4) 0.013(3) C6 0.081(6) 0.067(5) 0.045(4) -0.034(4) 0.033(4) -0.007(4) C7 0.066(5) 0.038(4) 0.048(4) -0.017(3) 0.020(4) 0.004(3) C8 0.030(3) 0.028(3) 0.027(3) -0.004(2) 0.010(3) 0.000(2) C9 0.027(3) 0.033(3) 0.031(3) 0.004(3) 0.008(3) 0.005(3) C10 0.032(3) 0.030(3) 0.034(3) -0.000(3) 0.015(2) -0.005(3) C11 0.036(4) 0.033(3) 0.033(3) 0.003(3) 0.016(3) -0.003(3) C12 0.029(3) 0.034(3) 0.026(3) 0.000(2) 0.009(2) 0.003(2) C13 0.035(4) 0.039(3) 0.024(3) -0.005(3) 0.013(3) -0.005(3) C14 0.043(4) 0.057(4) 0.029(3) 0.004(3) 0.013(3) -0.004(3) C15 0.038(4) 0.030(3) 0.020(3) -0.006(3) 0.007(3) -0.000(2) C16 0.061(6) 0.26(1) 0.070(6) 0.094(8) -0.008(5) -0.043(7) C17 0.062(5) 0.046(4) 0.085(6) -0.002(4) 0.046(5) -0.019(4) C18 0.140(10) 0.066(6) 0.24(1) -0.033(6) 0.163(10) -0.050(7) C19 0.067(5) 0.049(4) 0.039(4) 0.016(4) 0.021(4) -0.007(3) C20 0.055(5) 0.025(3) 0.087(6) 0.002(3) 0.003(4) -0.015(3) C21 0.056(5) 0.030(3) 0.049(4) 0.010(3) 0.008(3) 0.004(3) C22 0.027(3) 0.021(3) 0.034(3) -0.002(2) 0.007(3) -0.005(2) C23 0.039(4) 0.046(4) 0.043(4) -0.013(3) 0.017(3) -0.007(3) C24 0.043(4) 0.029(3) 0.036(3) 0.000(3) 0.014(3) -0.001(3) C25 0.033(4) 0.048(4) 0.054(4) -0.007(3) 0.013(3) -0.010(3) C26 0.040(4) 0.041(4) 0.027(3) 0.004(3) -0.004(3) -0.006(3) C27 0.027(4) 0.032(3) 0.049(4) 0.005(3) -0.002(3) -0.009(3) C28 0.038(4) 0.054(4) 0.051(4) -0.003(3) -0.005(3) -0.012(3) C29 0.026(3) 0.026(3) 0.028(3) -0.007(3) 0.009(3) -0.004(2) C30 0.044(4) 0.029(3) 0.035(3) -0.002(3) 0.017(3) -0.000(3) C31 0.034(3) 0.022(3) 0.032(3) -0.002(2) 0.008(3) -0.001(2) C32 0.044(4) 0.026(3) 0.035(3) -0.002(3) 0.008(3) 0.002(3) C33 0.052(4) 0.028(3) 0.039(3) 0.006(3) 0.021(3) 0.003(3) C34 0.079(6) 0.039(4) 0.019(3) -0.002(3) 0.004(3) -0.004(2) C35 0.073(5) 0.040(4) 0.049(4) 0.014(3) 0.039(4) 0.009(3) C36 0.100(7) 0.049(4) 0.040(4) 0.007(4) 0.039(4) -0.002(3) C37 0.045(4) 0.032(3) 0.040(4) -0.008(3) -0.005(3) 0.003(3) C38 0.042(4) 0.055(4) 0.054(4) 0.006(3) 0.028(3) 0.005(3) C39 0.028(3) 0.037(3) 0.031(3) -0.006(3) 0.005(3) 0.001(3) #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TA1 N1 2.123(4) . . yes TA1 N2 2.296(4) . . yes TA1 N3 2.163(4) . . yes TA1 N4 2.283(4) . . yes TA1 N5 1.998(4) . . yes TA1 C29 2.106(5) . . yes TA1 C39 2.189(6) . . yes SI1 N1 1.775(4) . . yes SI1 C2 1.863(6) . . yes SI1 C3 1.860(6) . . yes SI1 C4 1.865(6) . . yes SI2 N2 1.767(4) . . yes SI2 C5 1.884(8) . . yes SI2 C6 1.863(7) . . yes SI2 C7 1.851(6) . . yes SI3 N3 1.748(4) . . yes SI3 C16 1.851(9) . . yes SI3 C17 1.835(7) . . yes SI3 C18 1.849(9) . . yes SI4 N4 1.761(4) . . yes SI4 C19 1.861(7) . . yes SI4 C20 1.865(6) . . yes SI4 C21 1.864(6) . . yes N1 C1 1.350(6) . . yes N2 C1 1.329(6) . . yes N3 C15 1.360(6) . . yes N4 C15 1.318(7) . . yes N5 C29 1.380(7) . . yes N5 C31 1.435(7) . . yes C1 C8 1.494(7) . . yes C8 C9 1.395(8) . . yes C8 C10 1.389(7) . . yes C9 C11 1.387(7) . . yes C10 C12 1.398(7) . . yes C11 C13 1.376(8) . . yes C12 C13 1.400(7) . . yes C13 C14 1.514(7) . . yes C15 C22 1.514(7) . . yes C22 C23 1.375(8) . . yes C22 C24 1.394(8) . . yes C23 C25 1.384(8) . . yes C24 C26 1.379(8) . . yes C25 C27 1.385(8) . . yes C26 C27 1.391(9) . . yes C27 C28 1.518(8) . . yes C29 C30 1.366(7) . . yes C31 C32 1.401(8) . . yes C31 C33 1.398(8) . . yes C32 C34 1.417(8) . . yes C32 C37 1.483(9) . . yes C33 C35 1.402(8) . . yes C33 C38 1.516(9) . . yes C34 C36 1.36(1) . . yes C35 C36 1.39(1) . . yes C2 H29 0.950 . . no C2 H30 0.950 . . no C2 H31 0.950 . . no C3 H32 0.950 . . no C3 H33 0.950 . . no C3 H34 0.950 . . no C4 H26 0.950 . . no C4 H27 0.950 . . no C4 H28 0.950 . . no C5 H38 0.950 . . no C5 H39 0.950 . . no C5 H40 0.950 . . no C6 H20 0.950 . . no C6 H21 0.950 . . no C6 H22 0.950 . . no C7 H23 0.950 . . no C7 H24 0.950 . . no C7 H25 0.950 . . no C9 H3 0.950 . . no C10 H4 0.950 . . no C11 H10 0.950 . . no C12 H5 0.950 . . no C14 H17 0.950 . . no C14 H18 0.950 . . no C14 H19 0.950 . . no C16 H50 0.950 . . no C16 H51 0.952 . . no C16 H52 0.949 . . no C17 H44 0.950 . . no C17 H45 0.950 . . no C17 H46 0.950 . . no C18 H47 0.950 . . no C18 H48 0.950 . . no C18 H49 0.951 . . no C19 H53 0.950 . . no C19 H54 0.950 . . no C19 H55 0.950 . . no C20 H56 0.951 . . no C20 H57 0.950 . . no C20 H58 0.950 . . no C21 H59 0.950 . . no C21 H60 0.950 . . no C21 H61 0.950 . . no C23 H6 0.950 . . no C24 H9 0.950 . . no C25 H7 0.950 . . no C26 H8 0.950 . . no C28 H14 0.950 . . no C28 H15 0.950 . . no C28 H16 0.950 . . no C30 H1 1.020 . . no C30 H2 1.049 . . no C34 H11 0.950 . . no C35 H13 0.950 . . no C36 H12 0.950 . . no C37 H35 0.950 . . no C37 H36 0.950 . . no C37 H37 0.950 . . no C38 H41 0.950 . . no C38 H42 0.950 . . no C38 H43 0.950 . . no C39 H62 0.950 . . no C39 H63 0.950 . . no C39 H64 0.950 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 TA1 N2 61.1(2) . . . ? N1 TA1 N3 117.3(2) . . . ? N1 TA1 N4 151.5(2) . . . ? N1 TA1 N5 119.5(2) . . . ? N1 TA1 C29 89.8(2) . . . ? N1 TA1 C39 86.9(2) . . . ? N2 TA1 N3 83.7(2) . . . ? N2 TA1 N4 91.0(2) . . . ? N2 TA1 N5 176.4(2) . . . ? N2 TA1 C29 143.7(2) . . . ? N2 TA1 C39 85.0(2) . . . ? N3 TA1 N4 60.6(2) . . . ? N3 TA1 N5 98.7(2) . . . ? N3 TA1 C29 92.3(2) . . . ? N3 TA1 C39 143.0(2) . . . ? N4 TA1 N5 87.9(2) . . . ? N4 TA1 C29 118.3(2) . . . ? N4 TA1 C39 84.6(2) . . . ? N5 TA1 C29 39.2(2) . . . ? N5 TA1 C39 91.5(2) . . . ? C29 TA1 C39 116.7(2) . . . ? N1 SI1 C2 109.8(3) . . . ? N1 SI1 C3 107.6(2) . . . ? N1 SI1 C4 113.7(2) . . . ? C2 SI1 C3 110.8(3) . . . ? C2 SI1 C4 108.6(3) . . . ? C3 SI1 C4 106.2(3) . . . ? N2 SI2 C5 109.2(3) . . . ? N2 SI2 C6 113.3(3) . . . ? N2 SI2 C7 108.8(2) . . . ? C5 SI2 C6 111.3(3) . . . ? C5 SI2 C7 108.1(3) . . . ? C6 SI2 C7 105.8(3) . . . ? N3 SI3 C16 114.0(3) . . . ? N3 SI3 C17 105.4(3) . . . ? N3 SI3 C18 113.1(4) . . . ? C16 SI3 C17 109.1(5) . . . ? C16 SI3 C18 108.9(6) . . . ? C17 SI3 C18 105.8(4) . . . ? N4 SI4 C19 110.1(3) . . . ? N4 SI4 C20 113.6(3) . . . ? N4 SI4 C21 109.0(2) . . . ? C19 SI4 C20 109.9(3) . . . ? C19 SI4 C21 109.4(3) . . . ? C20 SI4 C21 104.8(3) . . . ? TA1 N1 SI1 134.1(2) . . . ? TA1 N1 C1 95.7(3) . . . ? SI1 N1 C1 129.8(3) . . . ? TA1 N2 SI2 144.4(2) . . . ? TA1 N2 C1 88.6(3) . . . ? SI2 N2 C1 127.0(4) . . . ? TA1 N3 SI3 129.6(2) . . . ? TA1 N3 C15 93.7(3) . . . ? SI3 N3 C15 135.6(4) . . . ? TA1 N4 SI4 140.9(3) . . . ? TA1 N4 C15 89.6(3) . . . ? SI4 N4 C15 129.1(4) . . . ? TA1 N5 C29 74.6(3) . . . ? TA1 N5 C31 157.5(4) . . . ? C29 N5 C31 126.2(4) . . . ? N1 C1 N2 114.5(4) . . . ? N1 C1 C8 121.5(4) . . . ? N2 C1 C8 124.0(5) . . . ? C1 C8 C9 121.1(5) . . . ? C1 C8 C10 120.1(5) . . . ? C9 C8 C10 118.9(5) . . . ? C8 C9 C11 120.7(5) . . . ? C8 C10 C12 120.2(5) . . . ? C9 C11 C13 120.9(5) . . . ? C10 C12 C13 120.5(5) . . . ? C11 C13 C12 118.9(5) . . . ? C11 C13 C14 121.7(5) . . . ? C12 C13 C14 119.4(5) . . . ? N3 C15 N4 114.0(5) . . . ? N3 C15 C22 121.2(5) . . . ? N4 C15 C22 124.6(5) . . . ? C15 C22 C23 122.0(5) . . . ? C15 C22 C24 118.3(5) . . . ? C23 C22 C24 119.6(5) . . . ? C22 C23 C25 119.9(6) . . . ? C22 C24 C26 119.7(6) . . . ? C23 C25 C27 121.6(6) . . . ? C24 C26 C27 121.4(6) . . . ? C25 C27 C26 117.7(5) . . . ? C25 C27 C28 121.1(6) . . . ? C26 C27 C28 121.2(6) . . . ? TA1 C29 N5 66.2(3) . . . ? TA1 C29 C30 163.1(5) . . . ? N5 C29 C30 130.4(5) . . . ? N5 C31 C32 119.9(5) . . . ? N5 C31 C33 119.5(5) . . . ? C32 C31 C33 120.6(5) . . . ? C31 C32 C34 118.0(6) . . . ? C31 C32 C37 122.6(5) . . . ? C34 C32 C37 119.4(6) . . . ? C31 C33 C35 119.7(6) . . . ? C31 C33 C38 123.3(5) . . . ? C35 C33 C38 117.0(6) . . . ? C32 C34 C36 121.3(6) . . . ? C33 C35 C36 119.7(7) . . . ? C34 C36 C35 120.7(6) . . . ? SI1 C2 H29 109.489 . . . no SI1 C2 H30 109.490 . . . no SI1 C2 H31 109.481 . . . no H29 C2 H30 109.465 . . . no H29 C2 H31 109.451 . . . no H30 C2 H31 109.451 . . . no SI1 C3 H32 109.484 . . . no SI1 C3 H33 109.494 . . . no SI1 C3 H34 109.499 . . . no H32 C3 H33 109.440 . . . no H32 C3 H34 109.447 . . . no H33 C3 H34 109.464 . . . no SI1 C4 H26 109.477 . . . no SI1 C4 H27 109.474 . . . no SI1 C4 H28 109.471 . . . no H26 C4 H27 109.471 . . . no H26 C4 H28 109.468 . . . no H27 C4 H28 109.466 . . . no SI2 C5 H38 109.505 . . . no SI2 C5 H39 109.492 . . . no SI2 C5 H40 109.511 . . . no H38 C5 H39 109.427 . . . no H38 C5 H40 109.457 . . . no H39 C5 H40 109.435 . . . no SI2 C6 H20 109.477 . . . no SI2 C6 H21 109.495 . . . no SI2 C6 H22 109.481 . . . no H20 C6 H21 109.462 . . . no H20 C6 H22 109.442 . . . no H21 C6 H22 109.470 . . . no SI2 C7 H23 109.472 . . . no SI2 C7 H24 109.495 . . . no SI2 C7 H25 109.477 . . . no H23 C7 H24 109.468 . . . no H23 C7 H25 109.440 . . . no H24 C7 H25 109.475 . . . no C8 C9 H3 119.636 . . . no C11 C9 H3 119.635 . . . no C8 C10 H4 119.923 . . . no C12 C10 H4 119.918 . . . no C9 C11 H10 119.579 . . . no C13 C11 H10 119.552 . . . no C10 C12 H5 119.743 . . . no C13 C12 H5 119.752 . . . no C13 C14 H17 109.468 . . . no C13 C14 H18 109.483 . . . no C13 C14 H19 109.490 . . . no H17 C14 H18 109.457 . . . no H17 C14 H19 109.460 . . . no H18 C14 H19 109.469 . . . no SI3 C16 H50 109.575 . . . no SI3 C16 H51 109.463 . . . no SI3 C16 H52 109.605 . . . no H50 C16 H51 109.305 . . . no H50 C16 H52 109.528 . . . no H51 C16 H52 109.351 . . . no SI3 C17 H44 109.494 . . . no SI3 C17 H45 109.487 . . . no SI3 C17 H46 109.517 . . . no H44 C17 H45 109.415 . . . no H44 C17 H46 109.464 . . . no H45 C17 H46 109.451 . . . no SI3 C18 H47 109.566 . . . no SI3 C18 H48 109.557 . . . no SI3 C18 H49 109.492 . . . no H47 C18 H48 109.476 . . . no H47 C18 H49 109.376 . . . no H48 C18 H49 109.359 . . . no SI4 C19 H53 109.484 . . . no SI4 C19 H54 109.479 . . . no SI4 C19 H55 109.481 . . . no H53 C19 H54 109.463 . . . no H53 C19 H55 109.463 . . . no H54 C19 H55 109.457 . . . no SI4 C20 H56 109.475 . . . no SI4 C20 H57 109.503 . . . no SI4 C20 H58 109.504 . . . no H56 C20 H57 109.432 . . . no H56 C20 H58 109.436 . . . no H57 C20 H58 109.478 . . . no SI4 C21 H59 109.502 . . . no SI4 C21 H60 109.504 . . . no SI4 C21 H61 109.492 . . . no H59 C21 H60 109.455 . . . no H59 C21 H61 109.435 . . . no H60 C21 H61 109.439 . . . no C22 C23 H6 120.024 . . . no C25 C23 H6 120.027 . . . no C22 C24 H9 120.136 . . . no C26 C24 H9 120.158 . . . no C23 C25 H7 119.227 . . . no C27 C25 H7 119.219 . . . no C24 C26 H8 119.297 . . . no C27 C26 H8 119.279 . . . no C27 C28 H14 109.464 . . . no C27 C28 H15 109.455 . . . no C27 C28 H16 109.472 . . . no H14 C28 H15 109.478 . . . no H14 C28 H16 109.480 . . . no H15 C28 H16 109.479 . . . no C29 C30 H1 119.219 . . . no C29 C30 H2 124.298 . . . no H1 C30 H2 116.409 . . . no C32 C34 H11 119.376 . . . no C36 C34 H11 119.353 . . . no C33 C35 H13 120.170 . . . no C36 C35 H13 120.168 . . . no C34 C36 H12 119.645 . . . no C35 C36 H12 119.609 . . . no C32 C37 H35 109.487 . . . no C32 C37 H36 109.487 . . . no C32 C37 H37 109.495 . . . no H35 C37 H36 109.448 . . . no H35 C37 H37 109.451 . . . no H36 C37 H37 109.459 . . . no C33 C38 H41 109.488 . . . no C33 C38 H42 109.487 . . . no C33 C38 H43 109.471 . . . no H41 C38 H42 109.469 . . . no H41 C38 H43 109.459 . . . no H42 C38 H43 109.454 . . . no TA1 C39 H62 109.481 . . . no TA1 C39 H63 109.476 . . . no TA1 C39 H64 109.475 . . . no H62 C39 H63 109.469 . . . no H62 C39 H64 109.466 . . . no H63 C39 H64 109.459 . . . no #------------------------------------------------------------------------------ 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 TA1 N1 SI1 C2 92.2(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C3 -28.5(4) 1_555 1_555 1_555 1_555 yes TA1 N1 SI1 C4 -145.8(3) 1_555 1_555 1_555 1_555 yes TA1 N1 C1 N2 2.3(5) 1_555 1_555 1_555 1_555 yes TA1 N1 C1 C8 -178.4(4) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C5 97.2(5) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C6 -138.0(5) 1_555 1_555 1_555 1_555 yes TA1 N2 SI2 C7 -20.5(6) 1_555 1_555 1_555 1_555 yes TA1 N2 C1 N1 -2.1(5) 1_555 1_555 1_555 1_555 yes TA1 N2 C1 C8 178.6(5) 1_555 1_555 1_555 1_555 yes TA1 N3 SI3 C16 108.5(5) 1_555 1_555 1_555 1_555 yes TA1 N3 SI3 C17 -11.2(4) 1_555 1_555 1_555 1_555 yes TA1 N3 SI3 C18 -126.4(5) 1_555 1_555 1_555 1_555 yes TA1 N3 C15 N4 13.8(5) 1_555 1_555 1_555 1_555 yes TA1 N3 C15 C22 -161.6(4) 1_555 1_555 1_555 1_555 yes TA1 N4 SI4 C19 -65.1(4) 1_555 1_555 1_555 1_555 yes TA1 N4 SI4 C20 171.2(4) 1_555 1_555 1_555 1_555 yes TA1 N4 SI4 C21 54.9(5) 1_555 1_555 1_555 1_555 yes TA1 N4 C15 N3 -13.0(4) 1_555 1_555 1_555 1_555 yes TA1 N4 C15 C22 162.2(5) 1_555 1_555 1_555 1_555 yes TA1 N5 C29 C30 -176.3(6) 1_555 1_555 1_555 1_555 yes TA1 N5 C31 C32 94(1) 1_555 1_555 1_555 1_555 yes TA1 N5 C31 C33 -85(1) 1_555 1_555 1_555 1_555 yes TA1 C29 N5 C31 170.7(5) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 N2 171.2(4) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 N3 -124.0(3) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 N4 157.9(3) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 N5 -4.7(4) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 C29 -31.5(4) 1_555 1_555 1_555 1_555 yes SI1 N1 TA1 C39 85.3(4) 1_555 1_555 1_555 1_555 yes SI1 N1 C1 N2 -170.8(4) 1_555 1_555 1_555 1_555 yes SI1 N1 C1 C8 8.6(8) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N1 -178.5(5) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N3 55.5(5) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N4 -4.8(5) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 N5 -76(2) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 C29 140.7(4) 1_555 1_555 1_555 1_555 yes SI2 N2 TA1 C39 -89.3(5) 1_555 1_555 1_555 1_555 yes SI2 N2 C1 N1 177.8(4) 1_555 1_555 1_555 1_555 yes SI2 N2 C1 C8 -1.5(8) 1_555 1_555 1_555 1_555 yes SI3 N3 TA1 N1 34.7(4) 1_555 1_555 1_555 1_555 yes SI3 N3 TA1 N2 87.6(3) 1_555 1_555 1_555 1_555 yes SI3 N3 TA1 N4 -177.7(4) 1_555 1_555 1_555 1_555 yes SI3 N3 TA1 N5 -95.1(3) 1_555 1_555 1_555 1_555 yes SI3 N3 TA1 C29 -56.3(3) 1_555 1_555 1_555 1_555 yes SI3 N3 TA1 C39 160.5(3) 1_555 1_555 1_555 1_555 yes SI3 N3 C15 N4 -177.9(4) 1_555 1_555 1_555 1_555 yes SI3 N3 C15 C22 6.7(8) 1_555 1_555 1_555 1_555 yes SI4 N4 TA1 N1 -84.8(5) 1_555 1_555 1_555 1_555 yes SI4 N4 TA1 N2 -96.4(4) 1_555 1_555 1_555 1_555 yes SI4 N4 TA1 N3 -178.6(5) 1_555 1_555 1_555 1_555 yes SI4 N4 TA1 N5 80.1(4) 1_555 1_555 1_555 1_555 yes SI4 N4 TA1 C29 105.9(4) 1_555 1_555 1_555 1_555 yes SI4 N4 TA1 C39 -11.6(4) 1_555 1_555 1_555 1_555 yes SI4 N4 C15 N3 172.8(4) 1_555 1_555 1_555 1_555 yes SI4 N4 C15 C22 -12.0(8) 1_555 1_555 1_555 1_555 yes N1 TA1 N2 C1 1.4(3) 1_555 1_555 1_555 1_555 yes N1 TA1 N3 C15 -155.9(3) 1_555 1_555 1_555 1_555 yes N1 TA1 N4 C15 102.4(4) 1_555 1_555 1_555 1_555 yes N1 TA1 N5 C29 -45.5(4) 1_555 1_555 1_555 1_555 yes N1 TA1 N5 C31 154.5(9) 1_555 1_555 1_555 1_555 yes N1 TA1 C29 N5 141.6(3) 1_555 1_555 1_555 1_555 yes N1 TA1 C29 C30 -48(1) 1_555 1_555 1_555 1_555 yes N1 C1 C8 C9 66.0(8) 1_555 1_555 1_555 1_555 yes N1 C1 C8 C10 -112.0(6) 1_555 1_555 1_555 1_555 yes N2 TA1 N1 C1 -1.4(3) 1_555 1_555 1_555 1_555 yes N2 TA1 N3 C15 -103.0(3) 1_555 1_555 1_555 1_555 yes N2 TA1 N4 C15 90.7(3) 1_555 1_555 1_555 1_555 yes N2 TA1 N5 C29 -145(2) 1_555 1_555 1_555 1_555 yes N2 TA1 N5 C31 54(2) 1_555 1_555 1_555 1_555 yes N2 TA1 C29 N5 176.5(3) 1_555 1_555 1_555 1_555 yes N2 TA1 C29 C30 -13(1) 1_555 1_555 1_555 1_555 yes N2 C1 C8 C9 -114.7(6) 1_555 1_555 1_555 1_555 yes N2 C1 C8 C10 67.3(8) 1_555 1_555 1_555 1_555 yes N3 TA1 N1 C1 63.5(4) 1_555 1_555 1_555 1_555 yes N3 TA1 N2 C1 -124.6(3) 1_555 1_555 1_555 1_555 yes N3 TA1 N4 C15 8.5(3) 1_555 1_555 1_555 1_555 yes N3 TA1 N5 C29 82.8(3) 1_555 1_555 1_555 1_555 yes N3 TA1 N5 C31 -77.2(10) 1_555 1_555 1_555 1_555 yes N3 TA1 C29 N5 -101.1(3) 1_555 1_555 1_555 1_555 yes N3 TA1 C29 C30 69(1) 1_555 1_555 1_555 1_555 yes N3 C15 C22 C23 -66.8(7) 1_555 1_555 1_555 1_555 yes N3 C15 C22 C24 114.5(6) 1_555 1_555 1_555 1_555 yes N4 TA1 N1 C1 -14.6(6) 1_555 1_555 1_555 1_555 yes N4 TA1 N2 C1 175.1(3) 1_555 1_555 1_555 1_555 yes N4 TA1 N3 C15 -8.3(3) 1_555 1_555 1_555 1_555 yes N4 TA1 N5 C29 142.7(3) 1_555 1_555 1_555 1_555 yes N4 TA1 N5 C31 -17.3(10) 1_555 1_555 1_555 1_555 yes N4 TA1 C29 N5 -43.5(3) 1_555 1_555 1_555 1_555 yes N4 TA1 C29 C30 126(1) 1_555 1_555 1_555 1_555 yes N4 C15 C22 C23 118.3(7) 1_555 1_555 1_555 1_555 yes N4 C15 C22 C24 -60.3(7) 1_555 1_555 1_555 1_555 yes N5 TA1 N1 C1 -177.3(3) 1_555 1_555 1_555 1_555 yes N5 TA1 N2 C1 103(2) 1_555 1_555 1_555 1_555 yes N5 TA1 N3 C15 74.3(3) 1_555 1_555 1_555 1_555 yes N5 TA1 N4 C15 -92.7(3) 1_555 1_555 1_555 1_555 yes N5 TA1 C29 C30 170(1) 1_555 1_555 1_555 1_555 yes N5 C29 TA1 C39 55.1(3) 1_555 1_555 1_555 1_555 yes N5 C31 C32 C34 -177.7(5) 1_555 1_555 1_555 1_555 yes N5 C31 C32 C37 1.8(8) 1_555 1_555 1_555 1_555 yes N5 C31 C33 C35 178.3(5) 1_555 1_555 1_555 1_555 yes N5 C31 C33 C38 -3.7(8) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C29 155.9(4) 1_555 1_555 1_555 1_555 yes C1 N1 TA1 C39 -87.3(4) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C2 -97.4(5) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C3 141.9(5) 1_555 1_555 1_555 1_555 yes C1 N1 SI1 C4 24.6(6) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C29 -39.4(5) 1_555 1_555 1_555 1_555 yes C1 N2 TA1 C39 90.6(3) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C5 -82.6(5) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C6 42.2(6) 1_555 1_555 1_555 1_555 yes C1 N2 SI2 C7 159.6(5) 1_555 1_555 1_555 1_555 yes C1 C8 C9 C11 -177.8(5) 1_555 1_555 1_555 1_555 yes C1 C8 C10 C12 178.3(5) 1_555 1_555 1_555 1_555 yes C8 C9 C11 C13 -1.0(9) 1_555 1_555 1_555 1_555 yes C8 C10 C12 C13 -0.1(9) 1_555 1_555 1_555 1_555 yes C9 C8 C10 C12 0.3(8) 1_555 1_555 1_555 1_555 yes C9 C11 C13 C12 1.3(9) 1_555 1_555 1_555 1_555 yes C9 C11 C13 C14 179.0(5) 1_555 1_555 1_555 1_555 yes C10 C8 C9 C11 0.2(9) 1_555 1_555 1_555 1_555 yes C10 C12 C13 C11 -0.8(9) 1_555 1_555 1_555 1_555 yes C10 C12 C13 C14 -178.5(5) 1_555 1_555 1_555 1_555 yes C15 N3 TA1 C29 113.1(3) 1_555 1_555 1_555 1_555 yes C15 N3 TA1 C39 -30.1(5) 1_555 1_555 1_555 1_555 yes C15 N3 SI3 C16 -56.3(7) 1_555 1_555 1_555 1_555 yes C15 N3 SI3 C17 -176.0(6) 1_555 1_555 1_555 1_555 yes C15 N3 SI3 C18 68.8(7) 1_555 1_555 1_555 1_555 yes C15 N4 TA1 C29 -66.9(4) 1_555 1_555 1_555 1_555 yes C15 N4 TA1 C39 175.6(3) 1_555 1_555 1_555 1_555 yes C15 N4 SI4 C19 105.6(5) 1_555 1_555 1_555 1_555 yes C15 N4 SI4 C20 -18.0(6) 1_555 1_555 1_555 1_555 yes C15 N4 SI4 C21 -134.4(5) 1_555 1_555 1_555 1_555 yes C15 C22 C23 C25 -178.6(6) 1_555 1_555 1_555 1_555 yes C15 C22 C24 C26 179.0(5) 1_555 1_555 1_555 1_555 yes C22 C23 C25 C27 0(1) 1_555 1_555 1_555 1_555 yes C22 C24 C26 C27 -0.2(9) 1_555 1_555 1_555 1_555 yes C23 C22 C24 C26 0.3(9) 1_555 1_555 1_555 1_555 yes C23 C25 C27 C26 0.8(9) 1_555 1_555 1_555 1_555 yes C23 C25 C27 C28 179.7(6) 1_555 1_555 1_555 1_555 yes C24 C22 C23 C25 0.1(9) 1_555 1_555 1_555 1_555 yes C24 C26 C27 C25 -0.3(9) 1_555 1_555 1_555 1_555 yes C24 C26 C27 C28 -179.2(6) 1_555 1_555 1_555 1_555 yes C29 TA1 N5 C31 -159(1) 1_555 1_555 1_555 1_555 yes C29 N5 TA1 C39 -132.8(3) 1_555 1_555 1_555 1_555 yes C29 N5 C31 C32 -60.8(7) 1_555 1_555 1_555 1_555 yes C29 N5 C31 C33 118.4(6) 1_555 1_555 1_555 1_555 yes C30 C29 TA1 C39 -134(1) 1_555 1_555 1_555 1_555 yes C30 C29 N5 C31 -5.7(9) 1_555 1_555 1_555 1_555 yes C31 N5 TA1 C39 67.2(10) 1_555 1_555 1_555 1_555 yes C31 C32 C34 C36 -1.3(9) 1_555 1_555 1_555 1_555 yes C31 C33 C35 C36 0.2(9) 1_555 1_555 1_555 1_555 yes C32 C31 C33 C35 -2.4(8) 1_555 1_555 1_555 1_555 yes C32 C31 C33 C38 175.6(5) 1_555 1_555 1_555 1_555 yes C32 C34 C36 C35 -0.9(10) 1_555 1_555 1_555 1_555 yes C33 C31 C32 C34 3.0(8) 1_555 1_555 1_555 1_555 yes C33 C31 C32 C37 -177.5(5) 1_555 1_555 1_555 1_555 yes C33 C35 C36 C34 1.5(10) 1_555 1_555 1_555 1_555 yes C36 C34 C32 C37 179.1(6) 1_555 1_555 1_555 1_555 yes C36 C35 C33 C38 -178.0(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag C10 C10 3.58(1) . 3_667 ?