# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Michael F. Lappert' 'Yanxiang Cheng' 'Peter B. Hitchcock' 'Meisu Zhou' _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; Chemistry Department University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis and characterisation of thallium(I) b-diketiminates; structures of the crystalline monomers TlL and TlL' [ L = {N(SiMe3)C(Ph)}2CH, L' = {N(C6H3Pri2 2,6)C(H)}2CPh] ; _publ_requested_category FM data_(1)-jun2904 _database_code_depnum_ccdc_archive 'CCDC 249920' _audit_creation_date 2004-06-25T17:59:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H29 N2 Si2 Tl1' _chemical_formula_sum 'C21 H29 N2 Si2 Tl1' _chemical_formula_weight 570.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9885(2) _cell_length_b 19.6876(3) _cell_length_c 12.2915(3) _cell_angle_alpha 90 _cell_angle_beta 107.184(1) _cell_angle_gamma 90 _cell_volume 2309.22(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16692 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.2644 _exptl_absorpt_correction_T_max 0.4088 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.126984E-1 _diffrn_orient_matrix_ub_12 0.24857E-2 _diffrn_orient_matrix_ub_13 0.776107E-1 _diffrn_orient_matrix_ub_21 -0.104019 _diffrn_orient_matrix_ub_22 -0.166E-4 _diffrn_orient_matrix_ub_23 -0.34842E-1 _diffrn_orient_matrix_ub_31 -0.588E-3 _diffrn_orient_matrix_ub_32 -0.507325E-1 _diffrn_orient_matrix_ub_33 0.3814E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_unetI/netI 0.0282 _diffrn_reflns_number 28873 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 4043 _reflns_number_gt 3658 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+6.6567P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 4043 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.886 _refine_diff_density_min -1.449 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.697076(16) 0.544932(8) 0.520247(14) 0.03246(8) Uani 1 1 d . . . Si1 Si 0.68842(12) 0.72321(6) 0.52627(10) 0.0320(3) Uani 1 1 d . . . Si2 Si 0.65661(11) 0.48486(6) 0.24720(10) 0.0286(2) Uani 1 1 d . . . N1 N 0.7940(3) 0.65783(16) 0.5039(3) 0.0263(7) Uani 1 1 d . . . N2 N 0.7780(3) 0.53145(16) 0.3518(3) 0.0246(7) Uani 1 1 d . . . C1 C 0.9175(4) 0.65939(19) 0.4836(3) 0.0243(8) Uani 1 1 d . . . C2 C 0.9735(4) 0.60877(19) 0.4288(3) 0.0245(8) Uani 1 1 d . . . H2 H 1.0718 0.6111 0.4406 0.029 Uiso 1 1 calc R . . C3 C 0.9034(4) 0.55485(18) 0.3586(3) 0.0216(8) Uani 1 1 d . . . C4 C 1.0151(4) 0.71901(19) 0.5240(3) 0.0264(8) Uani 1 1 d . . . C5 C 1.0733(5) 0.7529(2) 0.4486(4) 0.0385(11) Uani 1 1 d . . . H5 H 1.0485 0.7396 0.3708 0.046 Uiso 1 1 calc R . . C6 C 1.1672(6) 0.8058(3) 0.4875(5) 0.0501(13) Uani 1 1 d . . . H6 H 1.2043 0.8295 0.4356 0.06 Uiso 1 1 calc R . . C7 C 1.2070(5) 0.8242(2) 0.6009(5) 0.0464(12) Uani 1 1 d . . . H7 H 1.2735 0.8595 0.6273 0.056 Uiso 1 1 calc R . . C8 C 1.1503(5) 0.7913(2) 0.6755(4) 0.0402(11) Uani 1 1 d . . . H8 H 1.1768 0.8043 0.7535 0.048 Uiso 1 1 calc R . . C9 C 1.0542(4) 0.7391(2) 0.6372(4) 0.0301(9) Uani 1 1 d . . . H9 H 1.0147 0.7169 0.6891 0.036 Uiso 1 1 calc R . . C10 C 0.9835(4) 0.52355(19) 0.2853(3) 0.0213(8) Uani 1 1 d . . . C11 C 1.0457(4) 0.5627(2) 0.2198(4) 0.0267(8) Uani 1 1 d . . . H11 H 1.0427 0.6108 0.2241 0.032 Uiso 1 1 calc R . . C12 C 1.1120(5) 0.5324(2) 0.1482(4) 0.0341(10) Uani 1 1 d . . . H12 H 1.1514 0.5598 0.102 0.041 Uiso 1 1 calc R . . C13 C 1.1213(4) 0.4630(2) 0.1434(4) 0.0332(10) Uani 1 1 d . . . H13 H 1.1664 0.4425 0.0936 0.04 Uiso 1 1 calc R . . C14 C 1.0652(4) 0.4230(2) 0.2111(4) 0.0306(9) Uani 1 1 d . . . H14 H 1.0739 0.375 0.2094 0.037 Uiso 1 1 calc R . . C15 C 0.9962(4) 0.45272(18) 0.2814(4) 0.0250(8) Uani 1 1 d . . . H15 H 0.9571 0.4249 0.3273 0.03 Uiso 1 1 calc R . . C16 C 0.5057(5) 0.6998(3) 0.4423(4) 0.0451(12) Uani 1 1 d . . . H16A H 0.4995 0.6969 0.3614 0.068 Uiso 1 1 calc R . . H16B H 0.4404 0.7345 0.4532 0.068 Uiso 1 1 calc R . . H16C H 0.4814 0.6557 0.4684 0.068 Uiso 1 1 calc R . . C17 C 0.6868(6) 0.7272(3) 0.6771(4) 0.0507(13) Uani 1 1 d . . . H17A H 0.7803 0.7395 0.726 0.076 Uiso 1 1 calc R . . H17B H 0.6604 0.6827 0.7002 0.076 Uiso 1 1 calc R . . H17C H 0.6188 0.7614 0.6847 0.076 Uiso 1 1 calc R . . C18 C 0.7291(6) 0.8086(2) 0.4782(5) 0.0516(13) Uani 1 1 d . . . H18A H 0.73 0.8059 0.3988 0.077 Uiso 1 1 calc R . . H18B H 0.8211 0.8236 0.5262 0.077 Uiso 1 1 calc R . . H18C H 0.6574 0.8412 0.4842 0.077 Uiso 1 1 calc R . . C19 C 0.4866(5) 0.5301(3) 0.2273(5) 0.0460(12) Uani 1 1 d . . . H19A H 0.4675 0.5339 0.3008 0.069 Uiso 1 1 calc R . . H19B H 0.4111 0.5044 0.1741 0.069 Uiso 1 1 calc R . . H19C H 0.4921 0.5755 0.1965 0.069 Uiso 1 1 calc R . . C20 C 0.6414(6) 0.3975(2) 0.3016(5) 0.0501(13) Uani 1 1 d . . . H20A H 0.627 0.4005 0.3769 0.075 Uiso 1 1 calc R . . H20B H 0.7276 0.3721 0.3073 0.075 Uiso 1 1 calc R . . H20C H 0.5616 0.3741 0.249 0.075 Uiso 1 1 calc R . . C21 C 0.6840(5) 0.4800(3) 0.1037(4) 0.0387(10) Uani 1 1 d . . . H21A H 0.6911 0.526 0.0755 0.058 Uiso 1 1 calc R . . H21B H 0.6047 0.4564 0.051 0.058 Uiso 1 1 calc R . . H21C H 0.7707 0.4551 0.1093 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl 0.03265(11) 0.04071(12) 0.02713(12) -0.00183(7) 0.01363(8) -0.00978(6) Si1 0.0363(6) 0.0354(6) 0.0251(6) -0.0012(5) 0.0105(5) 0.0115(5) Si2 0.0232(5) 0.0347(6) 0.0269(6) -0.0041(5) 0.0059(5) -0.0049(4) N1 0.0318(18) 0.0246(16) 0.0251(18) -0.0003(14) 0.0124(15) 0.0012(13) N2 0.0230(16) 0.0298(17) 0.0216(18) -0.0013(13) 0.0076(14) -0.0006(13) C1 0.028(2) 0.0265(19) 0.0170(19) 0.0039(15) 0.0051(16) 0.0003(15) C2 0.0204(18) 0.0283(19) 0.023(2) -0.0017(16) 0.0043(15) -0.0011(15) C3 0.0241(19) 0.0261(19) 0.0144(19) 0.0016(15) 0.0053(15) 0.0025(15) C4 0.034(2) 0.0230(18) 0.026(2) -0.0018(16) 0.0132(17) -0.0016(16) C5 0.055(3) 0.036(2) 0.031(3) -0.0049(19) 0.024(2) -0.011(2) C6 0.071(3) 0.039(3) 0.054(3) -0.006(2) 0.039(3) -0.022(2) C7 0.051(3) 0.033(2) 0.058(3) -0.013(2) 0.020(2) -0.016(2) C8 0.048(3) 0.037(2) 0.032(3) -0.007(2) 0.007(2) -0.005(2) C9 0.040(2) 0.027(2) 0.025(2) -0.0038(17) 0.0127(18) -0.0058(17) C10 0.0165(17) 0.0249(18) 0.021(2) -0.0013(15) 0.0029(15) -0.0009(14) C11 0.025(2) 0.0261(19) 0.031(2) 0.0014(17) 0.0120(17) 0.0019(15) C12 0.034(2) 0.038(2) 0.036(3) 0.0079(19) 0.020(2) 0.0026(18) C13 0.029(2) 0.043(2) 0.031(3) -0.0056(18) 0.0151(19) 0.0059(18) C14 0.030(2) 0.023(2) 0.037(2) -0.0026(17) 0.0065(18) 0.0049(16) C15 0.025(2) 0.0239(19) 0.026(2) 0.0027(15) 0.0078(17) -0.0004(14) C16 0.035(2) 0.064(3) 0.037(3) 0.002(2) 0.011(2) 0.014(2) C17 0.052(3) 0.071(3) 0.032(3) -0.009(2) 0.017(2) 0.014(3) C18 0.063(3) 0.034(3) 0.056(3) 0.002(2) 0.015(3) 0.018(2) C19 0.022(2) 0.075(3) 0.041(3) -0.008(2) 0.007(2) 0.000(2) C20 0.055(3) 0.040(3) 0.052(3) 0.000(2) 0.011(2) -0.018(2) C21 0.033(2) 0.053(3) 0.026(2) -0.008(2) 0.0032(19) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl N2 2.449(3) . ? Tl N1 2.456(3) . ? Si1 N1 1.736(3) . ? Si1 C17 1.861(5) . ? Si1 C18 1.866(5) . ? Si1 C16 1.869(5) . ? Si2 N2 1.744(3) . ? Si2 C21 1.865(5) . ? Si2 C20 1.867(5) . ? Si2 C19 1.868(5) . ? N1 C1 1.330(5) . ? N2 C3 1.314(5) . ? C1 C2 1.408(6) . ? C1 C4 1.513(5) . ? C2 C3 1.416(5) . ? C3 C10 1.502(5) . ? C4 C9 1.387(6) . ? C4 C5 1.399(6) . ? C5 C6 1.389(7) . ? C6 C7 1.380(8) . ? C7 C8 1.374(7) . ? C8 C9 1.391(6) . ? C10 C11 1.388(6) . ? C10 C15 1.402(5) . ? C11 C12 1.384(6) . ? C12 C13 1.371(6) . ? C13 C14 1.378(6) . ? C14 C15 1.384(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Tl N1 78.04(11) . . ? N1 Si1 C17 111.9(2) . . ? N1 Si1 C18 114.7(2) . . ? C17 Si1 C18 110.2(3) . . ? N1 Si1 C16 105.6(2) . . ? C17 Si1 C16 105.4(2) . . ? C18 Si1 C16 108.4(2) . . ? N2 Si2 C21 117.36(19) . . ? N2 Si2 C20 109.4(2) . . ? C21 Si2 C20 110.0(2) . . ? N2 Si2 C19 104.7(2) . . ? C21 Si2 C19 106.4(2) . . ? C20 Si2 C19 108.6(3) . . ? C1 N1 Si1 130.8(3) . . ? C1 N1 Tl 116.5(2) . . ? Si1 N1 Tl 112.69(16) . . ? C3 N2 Si2 132.3(3) . . ? C3 N2 Tl 117.0(3) . . ? Si2 N2 Tl 110.44(15) . . ? N1 C1 C2 126.6(4) . . ? N1 C1 C4 120.0(3) . . ? C2 C1 C4 113.4(3) . . ? C1 C2 C3 128.8(3) . . ? N2 C3 C2 126.3(4) . . ? N2 C3 C10 119.0(3) . . ? C2 C3 C10 114.7(3) . . ? C9 C4 C5 118.7(4) . . ? C9 C4 C1 120.9(3) . . ? C5 C4 C1 120.3(4) . . ? C6 C5 C4 119.9(4) . . ? C7 C6 C5 120.6(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 120.1(4) . . ? C4 C9 C8 120.8(4) . . ? C11 C10 C15 118.1(4) . . ? C11 C10 C3 122.0(3) . . ? C15 C10 C3 119.9(3) . . ? C12 C11 C10 120.7(4) . . ? C13 C12 C11 120.6(4) . . ? C12 C13 C14 119.9(4) . . ? C13 C14 C15 120.1(4) . . ? C14 C15 C10 120.6(4) . . ? #===END data_(2)-mar904 _database_code_depnum_ccdc_archive 'CCDC 249921' _audit_creation_date 2004-03-15T14:46:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C33 H41 N2 Tl1' _chemical_formula_sum 'C33 H41 N2 Tl1' _chemical_formula_weight 670.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3632(2) _cell_length_b 12.0547(3) _cell_length_c 13.6277(3) _cell_angle_alpha 72.045(1) _cell_angle_beta 84.102(1) _cell_angle_gamma 88.813(1) _cell_volume 1455.41(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15536 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.572 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4015 _exptl_absorpt_correction_T_max 0.6154 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.391204E-1 _diffrn_orient_matrix_ub_12 -0.577083E-1 _diffrn_orient_matrix_ub_13 0.668899E-1 _diffrn_orient_matrix_ub_21 -0.973063E-1 _diffrn_orient_matrix_ub_22 0.66861E-2 _diffrn_orient_matrix_ub_23 -0.253129E-1 _diffrn_orient_matrix_ub_31 0.02304 _diffrn_orient_matrix_ub_32 -0.650408E-1 _diffrn_orient_matrix_ub_33 -0.299469E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_number 23257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 25.69 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.955 _reflns_number_total 5294 _reflns_number_gt 4919 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+4.4956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0033(3) _refine_ls_number_reflns 5294 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.293 _refine_diff_density_min -1.547 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tl Tl 0.579753(17) 0.422356(13) 0.623946(11) 0.02674(8) Uani 1 1 d . . . N1 N 0.7020(3) 0.2988(2) 0.5270(2) 0.0164(6) Uani 1 1 d . . . N2 N 0.6207(3) 0.2416(3) 0.7576(2) 0.0199(6) Uani 1 1 d . . . C1 C 0.7729(3) 0.2022(3) 0.5627(3) 0.0158(7) Uani 1 1 d . . . H1 H 0.8185 0.1705 0.512 0.019 Uiso 1 1 calc R . . C2 C 0.7902(4) 0.1392(3) 0.6670(3) 0.0170(7) Uani 1 1 d . . . C3 C 0.7150(4) 0.1608(3) 0.7543(3) 0.0188(7) Uani 1 1 d . . . H3 H 0.7356 0.1097 0.8197 0.023 Uiso 1 1 calc R . . C4 C 0.8899(4) 0.0389(3) 0.6855(3) 0.0176(7) Uani 1 1 d . . . C5 C 0.8596(4) -0.0648(3) 0.7660(3) 0.0231(8) Uani 1 1 d . . . H5 H 0.7718 -0.0721 0.8093 0.028 Uiso 1 1 calc R . . C6 C 0.9537(4) -0.1568(3) 0.7843(3) 0.0306(9) Uani 1 1 d . . . H6 H 0.9304 -0.2256 0.8405 0.037 Uiso 1 1 calc R . . C7 C 1.0817(4) -0.1502(3) 0.7218(3) 0.0294(9) Uani 1 1 d . . . H7 H 1.1462 -0.2137 0.7345 0.035 Uiso 1 1 calc R . . C8 C 1.1135(4) -0.0489(3) 0.6405(3) 0.0265(8) Uani 1 1 d . . . H8 H 1.2 -0.0433 0.5961 0.032 Uiso 1 1 calc R . . C9 C 1.0200(4) 0.0443(3) 0.6233(3) 0.0210(8) Uani 1 1 d . . . H9 H 1.0448 0.1136 0.568 0.025 Uiso 1 1 calc R . . C10 C 0.6859(4) 0.3419(3) 0.4186(2) 0.0161(7) Uani 1 1 d . . . C11 C 0.7708(4) 0.4381(3) 0.3557(3) 0.0201(7) Uani 1 1 d . . . C12 C 0.7410(4) 0.4888(3) 0.2531(3) 0.0257(8) Uani 1 1 d . . . H12 H 0.7964 0.5542 0.2101 0.031 Uiso 1 1 calc R . . C13 C 0.6328(4) 0.4459(4) 0.2131(3) 0.0276(9) Uani 1 1 d . . . H13 H 0.6119 0.4831 0.1439 0.033 Uiso 1 1 calc R . . C14 C 0.5553(4) 0.3490(3) 0.2739(3) 0.0236(8) Uani 1 1 d . . . H14 H 0.4842 0.3178 0.2446 0.028 Uiso 1 1 calc R . . C15 C 0.5780(4) 0.2956(3) 0.3770(3) 0.0192(7) Uani 1 1 d . . . C16 C 0.8959(4) 0.4800(3) 0.3972(3) 0.0261(8) Uani 1 1 d . . . H16 H 0.8711 0.465 0.4733 0.031 Uiso 1 1 calc R . . C17 C 1.0283(4) 0.4076(4) 0.3828(4) 0.0366(10) Uani 1 1 d . . . H17A H 1.1097 0.4343 0.4098 0.055 Uiso 1 1 calc R . . H17B H 1.0519 0.4172 0.3089 0.055 Uiso 1 1 calc R . . H17C H 1.0081 0.3252 0.4205 0.055 Uiso 1 1 calc R . . C18 C 0.9295(5) 0.6103(4) 0.3486(3) 0.0345(10) Uani 1 1 d . . . H18A H 1.0113 0.6312 0.3791 0.052 Uiso 1 1 calc R . . H18B H 0.8455 0.6553 0.3621 0.052 Uiso 1 1 calc R . . H18C H 0.9531 0.6278 0.2736 0.052 Uiso 1 1 calc R . . C19 C 0.4846(4) 0.1930(3) 0.4446(3) 0.0241(8) Uani 1 1 d . . . H19 H 0.5461 0.1421 0.4958 0.029 Uiso 1 1 calc R . . C20 C 0.3614(5) 0.2339(4) 0.5063(4) 0.0475(12) Uiso 1 1 d . . . H20A H 0.3995 0.2819 0.5443 0.071 Uiso 1 1 calc R . . H20B H 0.3102 0.1661 0.5555 0.071 Uiso 1 1 calc R . . H20C H 0.2951 0.2802 0.4588 0.071 Uiso 1 1 calc R . . C21 C 0.4291(5) 0.1183(5) 0.3852(4) 0.0483(12) Uiso 1 1 d . . . H21A H 0.3703 0.0541 0.4331 0.072 Uiso 1 1 calc R . . H21B H 0.5104 0.0865 0.3516 0.072 Uiso 1 1 calc R . . H21C H 0.3706 0.1659 0.3323 0.072 Uiso 1 1 calc R . . C22 C 0.5507(4) 0.2424(3) 0.8564(3) 0.0191(7) Uani 1 1 d . . . C23 C 0.6145(4) 0.3001(3) 0.9161(3) 0.0220(8) Uani 1 1 d . . . C24 C 0.5365(4) 0.3084(3) 1.0066(3) 0.0273(9) Uani 1 1 d . . . H24 H 0.5791 0.3453 1.0489 0.033 Uiso 1 1 calc R . . C25 C 0.3990(4) 0.2639(3) 1.0354(3) 0.0283(9) Uani 1 1 d . . . H25 H 0.3462 0.2726 1.096 0.034 Uiso 1 1 calc R . . C26 C 0.3377(4) 0.2067(3) 0.9761(3) 0.0268(8) Uani 1 1 d . . . H26 H 0.2431 0.1756 0.9971 0.032 Uiso 1 1 calc R . . C27 C 0.4111(4) 0.1935(3) 0.8868(3) 0.0214(8) Uani 1 1 d . . . C28 C 0.7667(4) 0.3493(4) 0.8883(3) 0.0296(9) Uani 1 1 d . . . H28 H 0.7981 0.3499 0.8158 0.035 Uiso 1 1 calc R . . C29 C 0.8688(5) 0.2717(5) 0.9591(4) 0.0580(14) Uani 1 1 d . . . H29A H 0.9663 0.3045 0.9398 0.087 Uiso 1 1 calc R . . H29B H 0.8676 0.1933 0.952 0.087 Uiso 1 1 calc R . . H29C H 0.8383 0.2674 1.0312 0.087 Uiso 1 1 calc R . . C30 C 0.7758(6) 0.4743(4) 0.8917(4) 0.0483(12) Uiso 1 1 d . . . H30A H 0.7102 0.5234 0.8453 0.072 Uiso 1 1 calc R . . H30B H 0.8743 0.504 0.8692 0.072 Uiso 1 1 calc R . . H30C H 0.7488 0.4758 0.9627 0.072 Uiso 1 1 calc R . . C31 C 0.3454(4) 0.1236(4) 0.8269(3) 0.0273(9) Uani 1 1 d . . . H31 H 0.3733 0.1628 0.7515 0.033 Uiso 1 1 calc R . . C32 C 0.4055(5) -0.0001(4) 0.8543(4) 0.0396(11) Uani 1 1 d . . . H32A H 0.3618 -0.0437 0.8149 0.059 Uiso 1 1 calc R . . H32B H 0.3833 -0.0395 0.9287 0.059 Uiso 1 1 calc R . . H32C H 0.5098 0.0038 0.8368 0.059 Uiso 1 1 calc R . . C33 C 0.1813(5) 0.1154(4) 0.8437(4) 0.0403(11) Uani 1 1 d . . . H33A H 0.1469 0.0691 0.8029 0.06 Uiso 1 1 calc R . . H33B H 0.1412 0.1939 0.8215 0.06 Uiso 1 1 calc R . . H33C H 0.1508 0.078 0.9174 0.06 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tl 0.03907(11) 0.02229(10) 0.01685(9) -0.00449(6) -0.00031(6) 0.00969(6) N1 0.0176(14) 0.0194(15) 0.0124(14) -0.0057(12) -0.0001(11) -0.0006(12) N2 0.0278(16) 0.0189(15) 0.0115(14) -0.0034(12) 0.0003(12) 0.0039(13) C1 0.0153(16) 0.0187(18) 0.0141(17) -0.0069(14) 0.0014(13) -0.0021(13) C2 0.0181(17) 0.0169(17) 0.0162(17) -0.0055(14) -0.0009(14) -0.0003(14) C3 0.0229(18) 0.0195(18) 0.0135(17) -0.0040(14) -0.0030(14) 0.0001(14) C4 0.0205(18) 0.0204(18) 0.0140(17) -0.0074(14) -0.0037(14) -0.0002(14) C5 0.0245(19) 0.024(2) 0.0187(18) -0.0034(15) -0.0015(15) 0.0037(15) C6 0.035(2) 0.024(2) 0.027(2) -0.0005(17) 0.0001(17) 0.0052(17) C7 0.032(2) 0.027(2) 0.032(2) -0.0122(18) -0.0079(17) 0.0105(17) C8 0.0227(19) 0.032(2) 0.027(2) -0.0148(18) 0.0022(16) 0.0019(16) C9 0.0218(18) 0.0227(19) 0.0178(18) -0.0058(15) 0.0009(14) -0.0009(15) C10 0.0184(17) 0.0191(18) 0.0103(16) -0.0050(14) 0.0014(13) 0.0034(14) C11 0.0213(18) 0.0242(19) 0.0153(17) -0.0068(15) -0.0011(14) -0.0003(15) C12 0.030(2) 0.028(2) 0.0155(18) -0.0030(16) 0.0035(15) -0.0020(16) C13 0.036(2) 0.034(2) 0.0135(18) -0.0075(16) -0.0058(16) 0.0042(17) C14 0.028(2) 0.024(2) 0.0217(19) -0.0108(16) -0.0070(16) 0.0030(16) C15 0.0216(18) 0.0205(18) 0.0168(18) -0.0079(15) -0.0012(14) 0.0037(14) C16 0.027(2) 0.031(2) 0.0172(19) -0.0025(16) 0.0001(15) -0.0076(16) C17 0.027(2) 0.040(3) 0.040(3) -0.008(2) -0.0051(19) -0.0039(18) C18 0.037(2) 0.034(2) 0.028(2) -0.0040(18) -0.0006(18) -0.0109(19) C19 0.0260(19) 0.0231(19) 0.0233(19) -0.0057(16) -0.0077(16) -0.0007(15) C22 0.0236(18) 0.0195(18) 0.0130(17) -0.0042(14) -0.0001(14) 0.0066(14) C23 0.027(2) 0.0215(19) 0.0160(18) -0.0049(15) 0.0010(15) 0.0014(15) C24 0.039(2) 0.026(2) 0.0178(19) -0.0095(16) 0.0022(17) -0.0038(17) C25 0.038(2) 0.029(2) 0.0160(19) -0.0073(16) 0.0087(16) 0.0002(17) C26 0.029(2) 0.027(2) 0.0212(19) -0.0044(16) 0.0030(16) -0.0005(16) C27 0.031(2) 0.0183(18) 0.0119(17) -0.0011(14) -0.0010(15) 0.0059(15) C28 0.032(2) 0.037(2) 0.021(2) -0.0128(18) 0.0021(17) -0.0039(18) C29 0.035(3) 0.068(4) 0.062(4) -0.007(3) -0.009(2) -0.001(2) C31 0.030(2) 0.035(2) 0.0174(19) -0.0082(17) -0.0024(16) -0.0039(17) C32 0.038(2) 0.033(2) 0.054(3) -0.022(2) -0.003(2) -0.0018(19) C33 0.036(2) 0.050(3) 0.039(3) -0.017(2) -0.012(2) 0.000(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl N2 2.423(3) . ? Tl N1 2.471(3) . ? Tl Tl 3.7642(3) 2_666 ? N1 C1 1.311(4) . ? N1 C10 1.430(4) . ? N2 C3 1.309(5) . ? N2 C22 1.439(4) . ? C1 C2 1.413(5) . ? C2 C3 1.411(5) . ? C2 C4 1.487(5) . ? C4 C5 1.397(5) . ? C4 C9 1.401(5) . ? C5 C6 1.379(5) . ? C6 C7 1.386(6) . ? C7 C8 1.386(6) . ? C8 C9 1.387(5) . ? C10 C15 1.411(5) . ? C10 C11 1.413(5) . ? C11 C12 1.398(5) . ? C11 C16 1.511(5) . ? C12 C13 1.378(6) . ? C13 C14 1.376(6) . ? C14 C15 1.389(5) . ? C15 C19 1.523(5) . ? C16 C18 1.530(6) . ? C16 C17 1.532(6) . ? C19 C21 1.514(6) . ? C19 C20 1.521(6) . ? C22 C23 1.403(5) . ? C22 C27 1.413(5) . ? C23 C24 1.396(5) . ? C23 C28 1.520(5) . ? C24 C25 1.377(6) . ? C25 C26 1.384(6) . ? C26 C27 1.386(5) . ? C27 C31 1.518(5) . ? C28 C29 1.522(6) . ? C28 C30 1.526(6) . ? C31 C33 1.531(6) . ? C31 C32 1.531(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Tl N1 76.20(9) . . ? N2 Tl Tl 148.94(7) . 2_666 ? N1 Tl Tl 86.00(6) . 2_666 ? C1 N1 C10 119.2(3) . . ? C1 N1 Tl 128.6(2) . . ? C10 N1 Tl 112.2(2) . . ? C3 N2 C22 119.0(3) . . ? C3 N2 Tl 128.6(2) . . ? C22 N2 Tl 110.9(2) . . ? N1 C1 C2 128.4(3) . . ? C3 C2 C1 125.0(3) . . ? C3 C2 C4 117.7(3) . . ? C1 C2 C4 117.2(3) . . ? N2 C3 C2 128.8(3) . . ? C5 C4 C9 116.7(3) . . ? C5 C4 C2 121.9(3) . . ? C9 C4 C2 121.4(3) . . ? C6 C5 C4 121.8(3) . . ? C5 C6 C7 120.8(4) . . ? C6 C7 C8 118.6(4) . . ? C7 C8 C9 120.5(3) . . ? C8 C9 C4 121.6(3) . . ? C15 C10 C11 120.4(3) . . ? C15 C10 N1 120.3(3) . . ? C11 C10 N1 119.1(3) . . ? C12 C11 C10 118.4(3) . . ? C12 C11 C16 121.1(3) . . ? C10 C11 C16 120.4(3) . . ? C13 C12 C11 121.3(4) . . ? C14 C13 C12 119.7(3) . . ? C13 C14 C15 121.9(3) . . ? C14 C15 C10 118.2(3) . . ? C14 C15 C19 120.9(3) . . ? C10 C15 C19 120.8(3) . . ? C11 C16 C18 113.9(3) . . ? C11 C16 C17 109.2(3) . . ? C18 C16 C17 110.6(3) . . ? C21 C19 C20 110.7(4) . . ? C21 C19 C15 113.7(3) . . ? C20 C19 C15 111.0(3) . . ? C23 C22 C27 121.1(3) . . ? C23 C22 N2 120.4(3) . . ? C27 C22 N2 118.3(3) . . ? C24 C23 C22 118.4(3) . . ? C24 C23 C28 119.1(3) . . ? C22 C23 C28 122.5(3) . . ? C25 C24 C23 121.1(4) . . ? C24 C25 C26 119.9(3) . . ? C25 C26 C27 121.5(4) . . ? C26 C27 C22 118.0(3) . . ? C26 C27 C31 120.5(3) . . ? C22 C27 C31 121.4(3) . . ? C23 C28 C29 110.6(4) . . ? C23 C28 C30 112.3(3) . . ? C29 C28 C30 110.3(4) . . ? C27 C31 C33 114.2(3) . . ? C27 C31 C32 110.7(3) . . ? C33 C31 C32 108.6(3) . . ? #===END data_(3)-oct497 _database_code_depnum_ccdc_archive 'CCDC 249922' _audit_creation_date 2004-09-03T15:07:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C29 H45 N2 Na O2 Si2' _chemical_formula_weight 532.84 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 13.049(2) _cell_length_b 10.632(4) _cell_length_c 23.466(9) _cell_angle_alpha 90 _cell_angle_beta 107.95(2) _cell_angle_gamma 90 _cell_volume 3097.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.1353 _diffrn_reflns_number 2828 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2710 _reflns_number_gt 1313 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The tfh group is disordered and its C atoms were left isotropic and SADI bond constraints applied. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1502P)^2^+10.0632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 2710 _refine_ls_number_parameters 161 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2061 _refine_ls_R_factor_gt 0.1073 _refine_ls_wR_factor_ref 0.3185 _refine_ls_wR_factor_gt 0.2532 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.652 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.43713(19) 0.10358(19) 0.60626(9) 0.0464(7) Uani 1 1 d . A . Na Na 0.5 0.2012(3) 0.75 0.0425(11) Uani 1 2 d S . . O O 0.6141(6) 0.3609(5) 0.7367(3) 0.087(2) Uani 1 1 d D . . N N 0.4709(4) 0.0412(5) 0.6771(2) 0.0362(14) Uani 1 1 d . . . C1 C 0.5 -0.1318(8) 0.75 0.031(2) Uani 1 2 d S . . H1 H 0.5 -0.2211 0.75 0.037 Uiso 1 2 calc SR A . C2 C 0.4808(5) -0.0806(6) 0.6926(3) 0.0286(15) Uani 1 1 d . A . C3 C 0.4679(6) -0.1790(6) 0.6449(3) 0.0345(16) Uani 1 1 d . . . C4 C 0.3789(6) -0.2590(7) 0.6273(3) 0.0481(19) Uani 1 1 d . A . H4 H 0.3246 -0.2524 0.6464 0.058 Uiso 1 1 calc R . . C5 C 0.3680(7) -0.3469(8) 0.5831(4) 0.060(2) Uani 1 1 d . . . H5 H 0.3067 -0.4003 0.572 0.073 Uiso 1 1 calc R A . C6 C 0.4450(8) -0.3584(8) 0.5547(4) 0.062(2) Uani 1 1 d . A . H6 H 0.4364 -0.4177 0.5233 0.075 Uiso 1 1 calc R . . C7 C 0.5341(7) -0.2835(8) 0.5723(4) 0.062(2) Uani 1 1 d . . . H7 H 0.5891 -0.2942 0.554 0.074 Uiso 1 1 calc R A . C8 C 0.5464(6) -0.1926(7) 0.6159(3) 0.0461(19) Uani 1 1 d . A . H8 H 0.6078 -0.1394 0.6262 0.055 Uiso 1 1 calc R . . C9 C 0.3766(9) 0.2615(8) 0.6115(4) 0.078(3) Uani 1 1 d . . . H9A H 0.36 0.3045 0.5728 0.116 Uiso 1 1 calc R A . H9B H 0.4279 0.3121 0.6423 0.116 Uiso 1 1 calc R . . H9C H 0.3103 0.2505 0.6222 0.116 Uiso 1 1 calc R . . C10 C 0.5582(8) 0.1248(9) 0.5805(4) 0.079(3) Uani 1 1 d . . . H10A H 0.5846 0.0423 0.5727 0.118 Uiso 1 1 calc R A . H10B H 0.6148 0.1682 0.6117 0.118 Uiso 1 1 calc R . . H10C H 0.5386 0.1749 0.5437 0.118 Uiso 1 1 calc R . . C11 C 0.3308(8) 0.0215(8) 0.5473(4) 0.066(3) Uani 1 1 d . . . H11A H 0.3114 0.0716 0.5105 0.1 Uiso 1 1 calc R A . H11B H 0.2672 0.0102 0.5606 0.1 Uiso 1 1 calc R . . H11C H 0.3575 -0.0609 0.5396 0.1 Uiso 1 1 calc R . . C12 C 0.6939(13) 0.3538(15) 0.7110(8) 0.064(5) Uiso 0.543(15) 1 d PD A 1 H12B H 0.6752 0.294 0.6771 0.076 Uiso 0.543(15) 1 calc PR A 1 H12A H 0.7628 0.3275 0.7405 0.076 Uiso 0.543(15) 1 calc PR A 1 C13 C 0.7008(18) 0.4851(15) 0.6901(8) 0.088(7) Uiso 0.543(15) 1 d PD A 1 H13B H 0.6439 0.5015 0.6518 0.106 Uiso 0.543(15) 1 calc PR A 1 H13A H 0.7721 0.5015 0.6849 0.106 Uiso 0.543(15) 1 calc PR A 1 C14 C 0.6846(15) 0.5639(14) 0.7395(8) 0.062(5) Uiso 0.543(15) 1 d PD A 1 H14B H 0.7536 0.5999 0.7648 0.075 Uiso 0.543(15) 1 calc PR A 1 H14A H 0.6331 0.6331 0.7234 0.075 Uiso 0.543(15) 1 calc PR A 1 C15 C 0.6405(18) 0.4734(15) 0.7738(8) 0.098(7) Uiso 0.543(15) 1 d PD A 1 H15B H 0.6946 0.4541 0.8128 0.117 Uiso 0.543(15) 1 calc PR A 1 H15A H 0.5753 0.508 0.7811 0.117 Uiso 0.543(15) 1 calc PR A 1 C12A C 0.608(3) 0.434(3) 0.6837(11) 0.154(14) Uiso 0.457(15) 1 d PD A 2 H12D H 0.5334 0.4629 0.6646 0.184 Uiso 0.457(15) 1 calc PR A 2 H12C H 0.6299 0.3813 0.6546 0.184 Uiso 0.457(15) 1 calc PR A 2 C13A C 0.682(2) 0.545(3) 0.7010(11) 0.110(10) Uiso 0.457(15) 1 d PD A 2 H13D H 0.7312 0.5506 0.6765 0.132 Uiso 0.457(15) 1 calc PR A 2 H13C H 0.6409 0.6245 0.6977 0.132 Uiso 0.457(15) 1 calc PR A 2 C14A C 0.7400(18) 0.5135(17) 0.7642(8) 0.069(6) Uiso 0.457(15) 1 d PD A 2 H14D H 0.7083 0.5569 0.7921 0.083 Uiso 0.457(15) 1 calc PR A 2 H14C H 0.8174 0.535 0.7747 0.083 Uiso 0.457(15) 1 calc PR A 2 C15A C 0.7232(13) 0.3743(18) 0.7644(11) 0.091(8) Uiso 0.457(15) 1 d PD A 2 H15D H 0.7651 0.3303 0.7418 0.109 Uiso 0.457(15) 1 calc PR A 2 H15C H 0.7442 0.341 0.8058 0.109 Uiso 0.457(15) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0641(15) 0.0348(11) 0.0385(12) 0.0016(10) 0.0133(10) -0.0031(10) Na 0.056(3) 0.0228(19) 0.049(2) 0 0.017(2) 0 O 0.086(5) 0.033(3) 0.136(6) 0.008(4) 0.026(4) -0.023(3) N 0.036(3) 0.028(3) 0.044(4) -0.005(3) 0.013(3) -0.004(3) C1 0.033(5) 0.024(5) 0.039(6) 0 0.015(4) 0 C2 0.020(3) 0.031(3) 0.037(4) -0.005(3) 0.011(3) -0.001(3) C3 0.045(4) 0.027(3) 0.030(4) 0.002(3) 0.009(3) 0.003(3) C4 0.047(5) 0.044(4) 0.054(5) -0.012(4) 0.016(4) -0.011(4) C5 0.067(6) 0.047(5) 0.060(6) -0.011(4) 0.010(5) -0.014(4) C6 0.089(7) 0.042(5) 0.054(5) -0.019(4) 0.020(5) 0.011(5) C7 0.063(6) 0.066(6) 0.060(5) -0.016(5) 0.025(4) 0.014(5) C8 0.048(5) 0.047(4) 0.050(5) -0.006(4) 0.024(4) 0.004(4) C9 0.120(8) 0.039(5) 0.058(6) 0.007(4) 0.004(5) 0.021(5) C10 0.095(8) 0.085(7) 0.067(6) 0.017(5) 0.041(5) -0.017(6) C11 0.094(7) 0.045(5) 0.047(5) -0.001(4) 0.003(5) 0.005(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si N 1.717(6) . ? Si C11 1.848(8) . ? Si C10 1.871(9) . ? Si C9 1.876(8) . ? Na O 2.341(6) . ? Na N 2.358(6) . ? O C12 1.357(13) . ? O C15A 1.378(15) . ? O C12A 1.449(17) . ? O C15 1.456(14) . ? N C2 1.341(8) . ? C1 C2 1.402(7) 6_657 ? C1 C2 1.402(7) . ? C2 C3 1.503(9) . ? C3 C4 1.396(9) . ? C3 C8 1.400(10) . ? C4 C5 1.372(10) . ? C5 C6 1.370(12) . ? C6 C7 1.364(12) . ? C7 C8 1.381(10) . ? C12 C13 1.491(15) . ? C13 C14 1.498(14) . ? C14 C15 1.478(15) . ? C12A C13A 1.494(17) . ? C13A C14A 1.481(16) . ? C14A C15A 1.497(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Si C11 116.9(3) . . ? N Si C10 111.6(4) . . ? C11 Si C10 109.2(5) . . ? N Si C9 105.6(3) . . ? C11 Si C9 103.8(4) . . ? C10 Si C9 109.1(5) . . ? O Na O 87.1(4) . 6_657 ? O Na N 113.2(2) . . ? O Na N 130.7(2) 6_657 . ? O Na N 130.7(2) . 6_657 ? O Na N 113.2(2) 6_657 6_657 ? N Na N 87.6(3) . 6_657 ? C12 O C15A 52.6(12) . . ? C12 O C12A 59.5(17) . . ? C15A O C12A 97.0(18) . . ? C12 O C15 103.8(11) . . ? C15A O C15 67.3(13) . . ? C12A O C15 90.7(15) . . ? C12 O Na 128.7(8) . . ? C15A O Na 128.3(10) . . ? C12A O Na 129.5(13) . . ? C15 O Na 124.0(8) . . ? C2 N Si 127.6(4) . . ? C2 N Na 121.4(4) . . ? Si N Na 111.1(3) . . ? C2 C1 C2 134.3(8) 6_657 . ? N C2 C1 127.5(6) . . ? N C2 C3 119.4(6) . . ? C1 C2 C3 113.1(6) . . ? C4 C3 C8 117.4(6) . . ? C4 C3 C2 122.4(6) . . ? C8 C3 C2 120.2(6) . . ? C5 C4 C3 121.4(7) . . ? C6 C5 C4 120.6(8) . . ? C7 C6 C5 119.0(8) . . ? C6 C7 C8 121.7(8) . . ? C7 C8 C3 119.8(7) . . ? O C12 C13 103.1(12) . . ? C12 C13 C14 103.4(14) . . ? C15 C14 C13 103.2(13) . . ? O C15 C14 105.7(12) . . ? O C12A C13A 109(2) . . ? C14A C13A C12A 101(2) . . ? C13A C14A C15A 101.3(19) . . ? O C15A C14A 103.4(14) . . ? #===END