Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name M.Lappert _publ_contact_author_address ; Department of Chemistry University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_section_title ; Researches on selected benzamidinates of Li, Na, Al, Zr and Sn(II) using the C1-symmetric ligands [N(SiMe3)C(C6H4Me-4 or Ph)NPh](-) ; _publ_requested_category FM _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK loop_ _publ_author_name M.Lappert P.B.Hitchcock P.G.Merle # Attachment 'mfl2-jun-2005.cif' data_(1)-apr799 _database_code_depnum_ccdc_archive 'CCDC 622818' _audit_creation_date 1999-04-12T13:28:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H31 Li1 N2 O1 Si1' _chemical_formula_structural 'C21 H31 LI1 N2 O1 SI1' _chemical_formula_sum 'C42 H62 Li2 N4 O2 Si2' _chemical_formula_weight 725.02 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.861(7) _cell_length_b 9.412(4) _cell_length_c 23.889(10) _cell_angle_alpha 90 _cell_angle_beta 94.97(6) _cell_angle_gamma 90 _cell_volume 2209(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.3 _cell_measurement_theta_max 8.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.09 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.24976E-1 _diffrn_orient_matrix_ub_12 0.00667 _diffrn_orient_matrix_ub_13 0.41391E-1 _diffrn_orient_matrix_ub_21 0.6839E-2 _diffrn_orient_matrix_ub_22 0.105664 _diffrn_orient_matrix_ub_23 -0.3143E-2 _diffrn_orient_matrix_ub_31 -0.98447E-1 _diffrn_orient_matrix_ub_32 0.8839E-2 _diffrn_orient_matrix_ub_33 0.6515E-2 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 7 _diffrn_standards_decay_corr_max 1.073 _diffrn_standards_decay_corr_min 0.996 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -2 6 -2 3 5 _diffrn_reflns_number 4096 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 3866 _reflns_number_gt 2671 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin,Pearce & Prout, 1993)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # 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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 0.002(2) _refine_ls_number_reflns 3866 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2272 _refine_ls_wR_factor_gt 0.199 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.512 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 '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' 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 Li Li 0.0853(6) 0.0208(5) -0.03721(19) 0.0364(12) Uani 1 1 d . . . Si Si 0.03853(10) -0.23878(9) -0.14290(3) 0.0401(3) Uani 1 1 d . A . O O 0.1835(3) 0.1711(2) -0.07294(10) 0.0528(7) Uani 1 1 d . . . N1 N -0.1377(3) 0.0323(3) -0.04543(9) 0.0333(6) Uani 1 1 d . . . N2 N -0.0049(3) -0.1113(3) -0.09621(10) 0.0354(6) Uani 1 1 d . . . C1 C -0.1187(3) -0.0414(3) -0.09298(11) 0.0315(7) Uani 1 1 d . A . C2 C -0.2325(3) -0.0451(3) -0.13941(11) 0.0333(7) Uani 1 1 d . . . C3 C -0.3515(4) -0.1166(4) -0.13366(14) 0.0520(10) Uani 1 1 d . A . H3 H -0.3647 -0.1606 -0.0988 0.062 Uiso 1 1 calc R . . C4 C -0.4529(4) -0.1264(5) -0.17716(15) 0.0571(10) Uani 1 1 d . . . H4 H -0.5335 -0.1782 -0.1719 0.068 Uiso 1 1 calc R A . C5 C -0.4387(4) -0.0617(4) -0.22850(14) 0.0488(9) Uani 1 1 d . A . C6 C -0.3210(4) 0.0120(4) -0.23369(14) 0.0529(10) Uani 1 1 d . . . H6 H -0.3095 0.059 -0.2681 0.064 Uiso 1 1 calc R A . C7 C -0.2179(4) 0.0207(4) -0.19059(13) 0.0456(9) Uani 1 1 d . A . H7 H -0.137 0.0718 -0.1961 0.055 Uiso 1 1 calc R . . C8 C -0.5488(4) -0.0719(6) -0.27654(17) 0.0741(14) Uani 1 1 d . . . H8A H -0.6329 -0.0294 -0.2652 0.111 Uiso 0.5 1 calc PR A . H8B H -0.565 -0.172 -0.2863 0.111 Uiso 0.5 1 calc PR . . H8C H -0.5197 -0.0211 -0.3092 0.111 Uiso 0.5 1 calc PR . . H8D H -0.5122 -0.1189 -0.3086 0.111 Uiso 0.5 1 calc PR . . H8E H -0.58 0.0237 -0.2875 0.111 Uiso 0.5 1 calc PR . . H8F H -0.6254 -0.1272 -0.2646 0.111 Uiso 0.5 1 calc PR . . C9 C -0.2410(3) 0.1368(3) -0.04675(12) 0.0344(7) Uani 1 1 d . A . C10 C -0.3471(4) 0.1255(4) -0.01277(14) 0.0513(9) Uani 1 1 d . . . H10 H -0.3548 0.043 0.0096 0.062 Uiso 1 1 calc R A . C11 C -0.4429(4) 0.2341(5) -0.01108(17) 0.0671(12) Uani 1 1 d . A . H11 H -0.515 0.225 0.0126 0.081 Uiso 1 1 calc R . . C12 C -0.4339(4) 0.3544(4) -0.04331(17) 0.0590(11) Uani 1 1 d . . . H12 H -0.4993 0.4282 -0.042 0.071 Uiso 1 1 calc R A . C13 C -0.3302(4) 0.3665(4) -0.07714(16) 0.0509(9) Uani 1 1 d . A . H13 H -0.3232 0.4491 -0.0995 0.061 Uiso 1 1 calc R . . C14 C -0.2352(4) 0.2594(3) -0.07911(14) 0.0419(8) Uani 1 1 d . . . H14 H -0.164 0.2695 -0.1032 0.05 Uiso 1 1 calc R A . C15 C -0.0890(4) -0.3850(4) -0.15385(17) 0.0647(12) Uani 1 1 d . . . H15A H -0.0522 -0.4604 -0.1764 0.097 Uiso 1 1 calc R A . H15B H -0.1729 -0.3477 -0.1735 0.097 Uiso 1 1 calc R . . H15C H -0.1089 -0.4236 -0.1174 0.097 Uiso 1 1 calc R . . C16 C 0.0737(5) -0.1687(4) -0.21367(14) 0.0621(11) Uani 1 1 d . . . H16A H -0.011 -0.1328 -0.2332 0.093 Uiso 1 1 calc R A . H16B H 0.1101 -0.2452 -0.2358 0.093 Uiso 1 1 calc R . . H16C H 0.1403 -0.0915 -0.209 0.093 Uiso 1 1 calc R . . C17 C 0.2012(4) -0.3174(4) -0.11147(16) 0.0542(10) Uani 1 1 d . . . H17A H 0.2343 -0.3872 -0.1375 0.081 Uiso 1 1 calc R A . H17B H 0.1856 -0.3643 -0.076 0.081 Uiso 1 1 calc R . . H17C H 0.2691 -0.2421 -0.1044 0.081 Uiso 1 1 calc R . . C18 C 0.1767(5) 0.3182(4) -0.06071(19) 0.0630(11) Uani 1 1 d . A . H18A H 0.1128 0.3656 -0.0891 0.076 Uiso 1 1 calc R . . H18B H 0.2677 0.3618 -0.0623 0.076 Uiso 1 1 calc R . . C19 C 0.1306(5) 0.3379(4) -0.00505(18) 0.0747(14) Uani 1 1 d . . . H19A H 0.1967 0.2953 0.0231 0.112 Uiso 1 1 calc R A . H19B H 0.0419 0.2919 -0.0033 0.112 Uiso 1 1 calc R . . H19C H 0.1222 0.4396 0.0026 0.112 Uiso 1 1 calc R . . C20 C 0.2697(7) 0.1367(6) -0.1189(3) 0.052(2) Uani 0.745(16) 1 d P A 1 H20A H 0.2768 0.0323 -0.1226 0.063 Uiso 0.745(16) 1 calc PR A 1 H20B H 0.3624 0.175 -0.1097 0.063 Uiso 0.745(16) 1 calc PR A 1 C21 C 0.2114(12) 0.1982(8) -0.1734(3) 0.085(3) Uani 0.745(16) 1 d P A 1 H21A H 0.2705 0.1746 -0.203 0.128 Uiso 0.745(16) 1 calc PR A 1 H21B H 0.205 0.3017 -0.1699 0.128 Uiso 0.745(16) 1 calc PR A 1 H21C H 0.1205 0.1586 -0.1831 0.128 Uiso 0.745(16) 1 calc PR A 1 C20A C 0.162(4) 0.184(3) -0.1350(9) 0.110(11) Uani 0.255(16) 1 d P A 2 H20C H 0.1122 0.2725 -0.1463 0.132 Uiso 0.255(16) 1 calc PR A 2 H20D H 0.1121 0.1015 -0.152 0.132 Uiso 0.255(16) 1 calc PR A 2 C21A C 0.305(3) 0.189(4) -0.1507(12) 0.102(10) Uani 0.255(16) 1 d P A 2 H21D H 0.3049 0.2065 -0.1912 0.153 Uiso 0.255(16) 1 calc PR A 2 H21E H 0.3495 0.0977 -0.1415 0.153 Uiso 0.255(16) 1 calc PR A 2 H21F H 0.3545 0.2651 -0.1299 0.153 Uiso 0.255(16) 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 Li 0.060(3) 0.029(3) 0.021(2) 0.001(2) 0.008(2) -0.001(2) Si 0.0664(7) 0.0277(5) 0.0274(5) -0.0060(3) 0.0111(4) -0.0009(4) O 0.0857(18) 0.0307(13) 0.0439(14) 0.0043(10) 0.0164(13) -0.0118(12) N1 0.0551(16) 0.0269(13) 0.0183(12) -0.0011(10) 0.0048(11) -0.0001(12) N2 0.0588(17) 0.0249(13) 0.0234(12) -0.0049(10) 0.0092(11) -0.0016(12) C1 0.0526(19) 0.0206(14) 0.0222(14) -0.0001(11) 0.0085(13) -0.0067(14) C2 0.0525(19) 0.0270(15) 0.0209(14) -0.0023(12) 0.0054(13) -0.0025(14) C3 0.066(2) 0.060(2) 0.0315(17) 0.0016(16) 0.0110(16) -0.016(2) C4 0.054(2) 0.075(3) 0.042(2) -0.0057(19) 0.0051(17) -0.021(2) C5 0.056(2) 0.055(2) 0.0345(18) -0.0086(16) -0.0007(16) -0.0006(18) C6 0.075(3) 0.056(2) 0.0268(17) 0.0074(15) -0.0026(17) -0.002(2) C7 0.064(2) 0.0417(19) 0.0302(16) 0.0061(14) 0.0015(15) -0.0140(17) C8 0.072(3) 0.097(4) 0.051(2) -0.012(2) -0.011(2) -0.006(3) C9 0.0503(18) 0.0294(16) 0.0226(14) -0.0052(12) -0.0017(13) -0.0010(14) C10 0.060(2) 0.057(2) 0.0380(18) 0.0069(16) 0.0131(17) 0.0072(19) C11 0.067(3) 0.089(3) 0.047(2) -0.003(2) 0.0162(19) 0.018(2) C12 0.068(3) 0.051(2) 0.056(2) -0.0186(19) -0.008(2) 0.016(2) C13 0.066(2) 0.0304(18) 0.054(2) -0.0030(16) -0.0112(19) 0.0002(17) C14 0.055(2) 0.0311(17) 0.0393(17) 0.0004(14) 0.0014(15) -0.0007(15) C15 0.089(3) 0.046(2) 0.061(2) -0.0277(19) 0.015(2) -0.016(2) C16 0.103(3) 0.050(2) 0.0354(19) -0.0039(17) 0.018(2) 0.012(2) C17 0.082(3) 0.0334(19) 0.049(2) -0.0053(16) 0.0189(19) 0.0056(18) C18 0.077(3) 0.032(2) 0.082(3) 0.004(2) 0.017(2) -0.0078(19) C19 0.124(4) 0.043(2) 0.060(3) -0.009(2) 0.018(3) -0.024(2) C20 0.069(4) 0.047(3) 0.043(4) 0.003(2) 0.019(3) -0.007(3) C21 0.153(9) 0.062(4) 0.042(4) 0.013(3) 0.015(5) -0.017(5) C20A 0.15(3) 0.12(2) 0.062(15) 0.048(14) 0.017(15) -0.018(19) C21A 0.084(17) 0.17(3) 0.058(16) -0.032(17) 0.016(13) -0.046(17) #----------------------------------------------------------------------------# # 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 Li O 1.953(5) . ? Li N2 2.026(6) . ? Li N1 2.058(5) 3 ? Li N1 2.193(6) . ? Li C1 2.387(6) . ? Li Li 2.581(10) 3 ? Si N2 1.718(3) . ? Si C17 1.864(4) . ? Si C15 1.867(4) . ? Si C16 1.875(4) . ? O C18 1.418(4) . ? O C20 1.482(6) . ? O C20A 1.48(2) . ? N1 C1 1.357(4) . ? N1 C9 1.415(4) . ? N1 Li 2.058(5) 3 ? N2 C1 1.309(4) . ? C1 C2 1.508(4) . ? C2 C3 1.370(5) . ? C2 C7 1.389(4) . ? C3 C4 1.381(5) . ? C4 C5 1.387(5) . ? C5 C6 1.367(5) . ? C5 C8 1.513(5) . ? C6 C7 1.385(5) . ? C9 C10 1.383(5) . ? C9 C14 1.392(4) . ? C10 C11 1.395(6) . ? C11 C12 1.377(6) . ? C12 C13 1.362(5) . ? C13 C14 1.379(5) . ? C18 C19 1.454(6) . ? C20 C21 1.492(12) . ? C20A C21A 1.49(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Li N2 110.2(2) . . ? O Li N1 120.2(3) . 3 ? N2 Li N1 125.3(3) . 3 ? O Li N1 117.2(3) . . ? N2 Li N1 65.92(19) . . ? N1 Li N1 105.3(2) 3 . ? O Li C1 111.1(2) . . ? N2 Li C1 33.24(13) . . ? N1 Li C1 127.2(3) 3 . ? N1 Li C1 34.15(12) . . ? O Li Li 142.0(4) . 3 ? N2 Li Li 96.5(3) . 3 ? N1 Li Li 55.04(19) 3 3 ? N1 Li Li 50.3(2) . 3 ? C1 Li Li 77.3(3) . 3 ? N2 Si C17 105.66(15) . . ? N2 Si C15 113.77(16) . . ? C17 Si C15 108.0(2) . . ? N2 Si C16 114.56(15) . . ? C17 Si C16 106.45(19) . . ? C15 Si C16 107.9(2) . . ? C18 O C20 114.0(3) . . ? C18 O C20A 96.8(12) . . ? C20 O C20A 47.1(13) . . ? C18 O Li 125.7(3) . . ? C20 O Li 120.3(3) . . ? C20A O Li 117.7(11) . . ? C1 N1 C9 119.2(2) . . ? C1 N1 Li 129.6(2) . 3 ? C9 N1 Li 108.1(2) . 3 ? C1 N1 Li 80.8(2) . . ? C9 N1 Li 138.6(2) . . ? Li N1 Li 74.7(2) 3 . ? C1 N2 Si 130.7(2) . . ? C1 N2 Li 88.7(2) . . ? Si N2 Li 139.6(2) . . ? N2 C1 N1 119.1(3) . . ? N2 C1 C2 122.1(2) . . ? N1 C1 C2 118.7(3) . . ? N2 C1 Li 58.0(2) . . ? N1 C1 Li 65.1(2) . . ? C2 C1 Li 162.4(2) . . ? C3 C2 C7 117.5(3) . . ? C3 C2 C1 121.8(3) . . ? C7 C2 C1 120.7(3) . . ? C2 C3 C4 121.9(3) . . ? C3 C4 C5 120.9(3) . . ? C6 C5 C4 117.0(3) . . ? C6 C5 C8 121.5(3) . . ? C4 C5 C8 121.5(4) . . ? C5 C6 C7 122.5(3) . . ? C6 C7 C2 120.2(3) . . ? C10 C9 C14 117.3(3) . . ? C10 C9 N1 120.9(3) . . ? C14 C9 N1 121.6(3) . . ? C9 C10 C11 120.6(4) . . ? C12 C11 C10 120.7(4) . . ? C13 C12 C11 119.2(4) . . ? C12 C13 C14 120.4(4) . . ? C13 C14 C9 121.7(3) . . ? O C18 C19 109.7(3) . . ? O C20 C21 111.1(7) . . ? O C20A C21A 101(3) . . ? #===END data_(2)-may3700 _database_code_depnum_ccdc_archive 'CCDC 622819' _audit_creation_date 2000-05-24T17:14:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[MeAl{Me3SiNC(C6H4Me)NPh}2]' _chemical_formula_moiety 'C35 H45 Al1 N4 Si2' _chemical_formula_sum 'C35 H45 Al N4 Si2' _chemical_formula_weight 604.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _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 11.6469(4) _cell_length_b 14.5539(3) _cell_length_c 20.9017(6) _cell_angle_alpha 90 _cell_angle_beta 90.0160(10) _cell_angle_gamma 90 _cell_volume 3543.00(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15620 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.153 _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_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 24368 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_unetI/netI 0.0645 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.86 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 8240 _reflns_number_gt 5752 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.0548P)^2^+1.2836P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8240 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.27 _refine_diff_density_min -0.25 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # 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' Al Al 0.0645 0.0514 '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' 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 Si1 Si 0.34735(5) 0.34486(4) 0.24004(3) 0.03319(15) Uani 1 1 d . . . Si2 Si 0.17563(5) 0.39399(4) -0.08748(3) 0.03505(15) Uani 1 1 d . . . Al Al 0.26907(5) 0.38579(4) 0.07784(3) 0.02743(15) Uani 1 1 d . . . N1 N 0.38867(14) 0.29781(10) 0.05822(7) 0.0285(4) Uani 1 1 d . . . N2 N 0.33964(14) 0.32567(10) 0.15815(7) 0.0287(4) Uani 1 1 d . . . N3 N 0.12044(14) 0.32850(10) 0.09028(7) 0.0281(4) Uani 1 1 d . . . N4 N 0.18141(14) 0.36544(10) -0.00654(7) 0.0296(4) Uani 1 1 d . . . C1 C 0.40583(16) 0.27612(12) 0.12002(9) 0.0271(4) Uani 1 1 d . . . C2 C 0.49007(17) 0.20562(12) 0.14055(8) 0.0282(4) Uani 1 1 d . . . C3 C 0.60542(18) 0.21366(14) 0.12420(10) 0.0363(5) Uani 1 1 d . . . H3 H 0.6311 0.2655 0.1005 0.044 Uiso 1 1 calc R . . C4 C 0.68317(19) 0.14607(15) 0.14238(10) 0.0419(5) Uani 1 1 d . . . H4 H 0.762 0.1531 0.1318 0.05 Uiso 1 1 calc R . . C5 C 0.64801(19) 0.06865(14) 0.17571(10) 0.0385(5) Uani 1 1 d . . . C6 C 0.53303(19) 0.06175(14) 0.19206(10) 0.0380(5) Uani 1 1 d . . . H6 H 0.5075 0.0099 0.2157 0.046 Uiso 1 1 calc R . . C7 C 0.45464(18) 0.12867(13) 0.17469(9) 0.0325(5) Uani 1 1 d . . . H7 H 0.3762 0.122 0.1861 0.039 Uiso 1 1 calc R . . C8 C 0.7322(2) -0.00641(17) 0.19293(14) 0.0587(7) Uani 1 1 d . . . H8A H 0.8088 0.0102 0.1773 0.088 Uiso 0.5 1 calc PR . . H8B H 0.708 -0.0643 0.1731 0.088 Uiso 0.5 1 calc PR . . H8C H 0.7345 -0.0138 0.2395 0.088 Uiso 0.5 1 calc PR . . H8D H 0.692 -0.0554 0.216 0.088 Uiso 0.5 1 calc PR . . H8E H 0.7929 0.019 0.2202 0.088 Uiso 0.5 1 calc PR . . H8F H 0.7663 -0.0315 0.1538 0.088 Uiso 0.5 1 calc PR . . C9 C 0.43323(16) 0.24866(13) 0.00509(8) 0.0278(4) Uani 1 1 d . . . C10 C 0.49243(18) 0.29673(14) -0.04158(9) 0.0365(5) Uani 1 1 d . . . H10 H 0.5057 0.3607 -0.0364 0.044 Uiso 1 1 calc R . . C11 C 0.5324(2) 0.25239(16) -0.09575(10) 0.0456(6) Uani 1 1 d . . . H11 H 0.5728 0.286 -0.1275 0.055 Uiso 1 1 calc R . . C12 C 0.5137(2) 0.15974(17) -0.10365(10) 0.0474(6) Uani 1 1 d . . . H12 H 0.5406 0.1294 -0.141 0.057 Uiso 1 1 calc R . . C13 C 0.4558(2) 0.11108(15) -0.05710(10) 0.0448(6) Uani 1 1 d . . . H13 H 0.4436 0.047 -0.0623 0.054 Uiso 1 1 calc R . . C14 C 0.41517(19) 0.15508(14) -0.00276(9) 0.0358(5) Uani 1 1 d . . . H14 H 0.3751 0.1212 0.029 0.043 Uiso 1 1 calc R . . C15 C 0.4972(2) 0.37446(17) 0.26262(11) 0.0505(6) Uani 1 1 d . . . H15A H 0.5239 0.426 0.2364 0.076 Uiso 1 1 calc R . . H15B H 0.547 0.3211 0.2555 0.076 Uiso 1 1 calc R . . H15C H 0.4997 0.3919 0.3079 0.076 Uiso 1 1 calc R . . C16 C 0.2966(3) 0.24677(17) 0.28984(11) 0.0607(8) Uani 1 1 d . . . H16A H 0.2176 0.2311 0.2779 0.091 Uiso 1 1 calc R . . H16B H 0.299 0.2641 0.3351 0.091 Uiso 1 1 calc R . . H16C H 0.3465 0.1935 0.2827 0.091 Uiso 1 1 calc R . . C17 C 0.2487(2) 0.44336(17) 0.25356(12) 0.0532(6) Uani 1 1 d . . . H17A H 0.1704 0.4257 0.2414 0.08 Uiso 1 1 calc R . . H17B H 0.2734 0.4957 0.2275 0.08 Uiso 1 1 calc R . . H17C H 0.2501 0.4606 0.2989 0.08 Uiso 1 1 calc R . . C18 C 0.10569(17) 0.31769(12) 0.02713(9) 0.0275(4) Uani 1 1 d . . . C19 C 0.01830(17) 0.25303(12) 0.00116(8) 0.0278(4) Uani 1 1 d . . . C20 C 0.05565(18) 0.17236(13) -0.02780(9) 0.0337(4) Uani 1 1 d . . . H20 H 0.1351 0.1633 -0.0357 0.04 Uiso 1 1 calc R . . C21 C -0.0229(2) 0.10519(13) -0.04512(10) 0.0379(5) Uani 1 1 d . . . H21 H 0.0038 0.0498 -0.064 0.046 Uiso 1 1 calc R . . C22 C -0.13899(19) 0.11748(14) -0.03537(9) 0.0366(5) Uani 1 1 d . . . C23 C -0.17638(19) 0.20002(15) -0.00949(10) 0.0401(5) Uani 1 1 d . . . H23 H -0.2564 0.211 -0.005 0.048 Uiso 1 1 calc R . . C24 C -0.09874(18) 0.26663(14) 0.00993(10) 0.0365(5) Uani 1 1 d . . . H24 H -0.1256 0.3217 0.0293 0.044 Uiso 1 1 calc R . . C25 C -0.2233(2) 0.04155(17) -0.05068(13) 0.0554(7) Uani 1 1 d . . . H25A H -0.1819 -0.0113 -0.0683 0.083 Uiso 0.5 1 calc PR . . H25B H -0.2793 0.0637 -0.0821 0.083 Uiso 0.5 1 calc PR . . H25C H -0.2634 0.023 -0.0115 0.083 Uiso 0.5 1 calc PR . . H25D H -0.3012 0.0616 -0.0396 0.083 Uiso 0.5 1 calc PR . . H25E H -0.2038 -0.0134 -0.0259 0.083 Uiso 0.5 1 calc PR . . H25F H -0.2197 0.0273 -0.0965 0.083 Uiso 0.5 1 calc PR . . C26 C 0.06574(17) 0.27281(12) 0.13738(8) 0.0284(4) Uani 1 1 d . . . C27 C 0.0912(2) 0.18050(14) 0.14291(11) 0.0434(5) Uani 1 1 d . . . H27 H 0.1434 0.1526 0.1139 0.052 Uiso 1 1 calc R . . C28 C 0.0405(2) 0.12830(16) 0.19084(12) 0.0511(6) Uani 1 1 d . . . H28 H 0.0576 0.0646 0.1941 0.061 Uiso 1 1 calc R . . C29 C -0.0342(2) 0.16790(16) 0.23364(11) 0.0497(6) Uani 1 1 d . . . H29 H -0.068 0.1321 0.2666 0.06 Uiso 1 1 calc R . . C30 C -0.0592(2) 0.25946(17) 0.22818(11) 0.0538(7) Uani 1 1 d . . . H30 H -0.1107 0.2873 0.2576 0.065 Uiso 1 1 calc R . . C31 C -0.0102(2) 0.31192(15) 0.18004(10) 0.0426(6) Uani 1 1 d . . . H31 H -0.029 0.3752 0.1764 0.051 Uiso 1 1 calc R . . C32 C 0.0292(2) 0.43367(18) -0.10922(12) 0.0558(7) Uani 1 1 d . . . H32A H 0.0068 0.4847 -0.0813 0.084 Uiso 1 1 calc R . . H32B H -0.0253 0.3829 -0.104 0.084 Uiso 1 1 calc R . . H32C H 0.0287 0.4544 -0.1538 0.084 Uiso 1 1 calc R . . C33 C 0.2147(2) 0.29701(17) -0.14114(10) 0.0505(6) Uani 1 1 d . . . H33A H 0.292 0.2752 -0.1305 0.076 Uiso 1 1 calc R . . H33B H 0.2132 0.3179 -0.1857 0.076 Uiso 1 1 calc R . . H33C H 0.1596 0.2468 -0.1355 0.076 Uiso 1 1 calc R . . C34 C 0.2799(2) 0.48991(17) -0.09890(12) 0.0560(7) Uani 1 1 d . . . H34A H 0.2593 0.5412 -0.0708 0.084 Uiso 1 1 calc R . . H34B H 0.2778 0.5104 -0.1435 0.084 Uiso 1 1 calc R . . H34C H 0.3575 0.4685 -0.0884 0.084 Uiso 1 1 calc R . . C35 C 0.3040(2) 0.51666(14) 0.08555(12) 0.0469(6) Uani 1 1 d . . . H35A H 0.2336 0.5505 0.0957 0.07 Uiso 1 1 calc R . . H35B H 0.3356 0.5392 0.045 0.07 Uiso 1 1 calc R . . H35C H 0.3604 0.5259 0.1198 0.07 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 Si1 0.0336(3) 0.0390(3) 0.0270(3) -0.0085(2) 0.0036(2) 0.0005(2) Si2 0.0377(4) 0.0381(3) 0.0294(3) 0.0078(2) 0.0052(2) 0.0000(2) Al 0.0257(3) 0.0259(3) 0.0306(3) -0.0015(2) 0.0053(2) -0.0020(2) N1 0.0289(9) 0.0311(8) 0.0253(7) -0.0003(6) 0.0059(7) 0.0015(7) N2 0.0245(9) 0.0339(8) 0.0277(8) -0.0063(7) 0.0038(7) 0.0002(7) N3 0.0282(9) 0.0293(8) 0.0267(8) 0.0009(6) 0.0056(7) -0.0037(6) N4 0.0285(9) 0.0305(8) 0.0299(8) 0.0034(6) 0.0044(7) -0.0005(7) C1 0.0251(11) 0.0277(9) 0.0286(9) -0.0025(7) 0.0038(8) -0.0056(7) C2 0.0276(11) 0.0322(10) 0.0248(9) -0.0048(7) 0.0023(8) -0.0009(8) C3 0.0308(12) 0.0392(11) 0.0389(11) 0.0042(9) 0.0048(9) -0.0026(9) C4 0.0278(12) 0.0517(13) 0.0463(12) -0.0002(10) 0.0010(10) 0.0025(10) C5 0.0391(14) 0.0381(11) 0.0383(11) -0.0048(9) -0.0066(10) 0.0045(9) C6 0.0452(14) 0.0324(11) 0.0363(11) 0.0018(9) 0.0004(10) -0.0024(9) C7 0.0324(12) 0.0340(10) 0.0311(10) -0.0023(8) 0.0060(9) -0.0020(8) C8 0.0533(17) 0.0498(14) 0.0731(18) 0.0041(13) -0.0129(14) 0.0126(12) C9 0.0247(11) 0.0344(10) 0.0243(9) -0.0017(8) 0.0041(8) 0.0007(8) C10 0.0371(13) 0.0383(11) 0.0340(10) 0.0018(9) 0.0096(9) 0.0008(9) C11 0.0428(14) 0.0604(15) 0.0336(11) 0.0030(10) 0.0157(10) 0.0053(11) C12 0.0506(15) 0.0603(15) 0.0312(11) -0.0120(10) 0.0078(10) 0.0142(12) C13 0.0564(16) 0.0386(12) 0.0395(12) -0.0115(10) -0.0006(11) 0.0033(10) C14 0.0403(13) 0.0353(11) 0.0317(10) -0.0014(8) 0.0039(9) -0.0042(9) C15 0.0437(15) 0.0638(15) 0.0441(13) -0.0204(11) -0.0078(11) 0.0028(12) C16 0.087(2) 0.0608(16) 0.0341(12) -0.0046(11) 0.0216(13) -0.0113(14) C17 0.0459(15) 0.0658(15) 0.0479(13) -0.0247(12) 0.0023(11) 0.0129(12) C18 0.0264(11) 0.0266(9) 0.0294(9) 0.0021(7) 0.0044(8) 0.0052(8) C19 0.0287(11) 0.0304(9) 0.0242(9) 0.0038(7) 0.0009(8) -0.0012(8) C20 0.0308(12) 0.0336(10) 0.0366(10) 0.0011(8) 0.0026(9) 0.0022(8) C21 0.0466(14) 0.0292(10) 0.0380(11) -0.0011(9) -0.0007(10) 0.0002(9) C22 0.0393(13) 0.0384(11) 0.0321(10) 0.0050(9) -0.0057(9) -0.0093(9) C23 0.0273(12) 0.0527(13) 0.0404(11) -0.0020(10) 0.0022(9) -0.0029(10) C24 0.0320(12) 0.0408(11) 0.0367(11) -0.0058(9) 0.0038(9) 0.0015(9) C25 0.0508(17) 0.0515(14) 0.0640(16) 0.0012(12) -0.0110(13) -0.0163(12) C26 0.0286(11) 0.0324(10) 0.0241(9) 0.0011(7) -0.0001(8) -0.0055(8) C27 0.0468(14) 0.0360(11) 0.0473(12) 0.0066(10) 0.0108(11) 0.0039(10) C28 0.0573(17) 0.0373(12) 0.0588(15) 0.0153(11) 0.0029(13) -0.0047(11) C29 0.0599(17) 0.0540(14) 0.0354(11) 0.0106(10) 0.0063(11) -0.0214(12) C30 0.0658(18) 0.0534(14) 0.0423(12) -0.0043(11) 0.0268(12) -0.0119(12) C31 0.0509(15) 0.0360(11) 0.0409(12) -0.0010(9) 0.0170(11) -0.0030(10) C32 0.0555(17) 0.0611(16) 0.0509(14) 0.0207(12) -0.0029(12) 0.0094(12) C33 0.0587(17) 0.0591(14) 0.0336(11) -0.0018(10) 0.0101(11) -0.0038(12) C34 0.0656(18) 0.0549(14) 0.0477(13) 0.0171(11) 0.0110(13) -0.0132(12) C35 0.0500(15) 0.0337(11) 0.0570(14) -0.0013(10) 0.0021(12) -0.0081(10) #----------------------------------------------------------------------------# # 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 Si1 N2 1.7366(16) . ? Si1 C15 1.858(3) . ? Si1 C17 1.859(2) . ? Si1 C16 1.863(2) . ? Si2 N4 1.7435(16) . ? Si2 C33 1.859(2) . ? Si2 C32 1.857(3) . ? Si2 C34 1.866(2) . ? Al N1 1.9361(16) . ? Al N3 1.9390(16) . ? Al C35 1.954(2) . ? Al N4 2.0589(18) . ? Al N2 2.0635(17) . ? Al C18 2.393(2) . ? Al C1 2.421(2) . ? N1 C1 1.344(2) . ? N1 C9 1.419(2) . ? N2 C1 1.323(2) . ? N3 C18 1.340(2) . ? N3 C26 1.425(2) . ? N4 C18 1.325(2) . ? C1 C2 1.483(3) . ? C2 C3 1.391(3) . ? C2 C7 1.391(3) . ? C3 C4 1.390(3) . ? C4 C5 1.387(3) . ? C5 C6 1.386(3) . ? C5 C8 1.511(3) . ? C6 C7 1.383(3) . ? C9 C10 1.384(2) . ? C9 C14 1.388(3) . ? C10 C11 1.384(3) . ? C11 C12 1.376(3) . ? C12 C13 1.380(3) . ? C13 C14 1.387(3) . ? C18 C19 1.489(3) . ? C19 C24 1.390(3) . ? C19 C20 1.391(3) . ? C20 C21 1.387(3) . ? C21 C22 1.379(3) . ? C22 C23 1.388(3) . ? C22 C25 1.513(3) . ? C23 C24 1.386(3) . ? C26 C27 1.381(3) . ? C26 C31 1.379(3) . ? C27 C28 1.389(3) . ? C28 C29 1.374(3) . ? C29 C30 1.369(3) . ? C30 C31 1.386(3) . ? 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 Si1 C15 109.63(9) . . ? N2 Si1 C17 104.01(10) . . ? C15 Si1 C17 111.30(11) . . ? N2 Si1 C16 114.28(10) . . ? C15 Si1 C16 109.50(13) . . ? C17 Si1 C16 108.04(12) . . ? N4 Si2 C33 113.27(9) . . ? N4 Si2 C32 110.29(10) . . ? C33 Si2 C32 108.28(13) . . ? N4 Si2 C34 106.11(10) . . ? C33 Si2 C34 109.34(11) . . ? C32 Si2 C34 109.51(12) . . ? N1 Al N3 112.74(7) . . ? N1 Al C35 120.80(9) . . ? N3 Al C35 126.44(9) . . ? N1 Al N4 94.60(7) . . ? N3 Al N4 67.08(6) . . ? C35 Al N4 108.31(9) . . ? N1 Al N2 66.76(6) . . ? N3 Al N2 93.67(7) . . ? C35 Al N2 105.26(9) . . ? N4 Al N2 146.42(7) . . ? N1 Al C18 101.79(7) . . ? N3 Al C18 34.05(6) . . ? C35 Al C18 127.29(9) . . ? N4 Al C18 33.58(6) . . ? N2 Al C18 120.08(6) . . ? N1 Al C1 33.67(6) . . ? N3 Al C1 104.77(7) . . ? C35 Al C1 118.39(9) . . ? N4 Al C1 122.90(6) . . ? N2 Al C1 33.11(6) . . ? C18 Al C1 114.29(6) . . ? C1 N1 C9 125.39(16) . . ? C1 N1 Al 93.36(11) . . ? C9 N1 Al 139.66(13) . . ? C1 N2 Si1 130.66(15) . . ? C1 N2 Al 88.46(12) . . ? Si1 N2 Al 138.95(9) . . ? C18 N3 C26 123.79(16) . . ? C18 N3 Al 91.86(11) . . ? C26 N3 Al 137.41(13) . . ? C18 N4 Si2 127.93(15) . . ? C18 N4 Al 87.17(12) . . ? Si2 N4 Al 144.68(9) . . ? N2 C1 N1 111.37(17) . . ? N2 C1 C2 126.04(17) . . ? N1 C1 C2 122.59(15) . . ? N2 C1 Al 58.44(10) . . ? N1 C1 Al 52.97(9) . . ? C2 C1 Al 175.32(13) . . ? C3 C2 C7 118.72(18) . . ? C3 C2 C1 120.63(17) . . ? C7 C2 C1 120.62(17) . . ? C2 C3 C4 120.15(19) . . ? C5 C4 C3 121.3(2) . . ? C4 C5 C6 117.9(2) . . ? C4 C5 C8 121.0(2) . . ? C6 C5 C8 121.1(2) . . ? C5 C6 C7 121.47(19) . . ? C6 C7 C2 120.38(19) . . ? C10 C9 C14 119.21(17) . . ? C10 C9 N1 118.62(17) . . ? C14 C9 N1 122.11(16) . . ? C11 C10 C9 120.57(19) . . ? C12 C11 C10 120.1(2) . . ? C13 C12 C11 119.73(19) . . ? C12 C13 C14 120.5(2) . . ? C13 C14 C9 119.88(18) . . ? N4 C18 N3 112.10(17) . . ? N4 C18 C19 126.37(17) . . ? N3 C18 C19 121.38(15) . . ? N4 C18 Al 59.25(11) . . ? N3 C18 Al 54.09(10) . . ? C19 C18 Al 165.23(13) . . ? C24 C19 C20 118.99(18) . . ? C24 C19 C18 122.18(17) . . ? C20 C19 C18 118.58(17) . . ? C21 C20 C19 120.16(19) . . ? C22 C21 C20 121.10(19) . . ? C21 C22 C23 118.53(19) . . ? C21 C22 C25 120.7(2) . . ? C23 C22 C25 120.7(2) . . ? C22 C23 C24 121.0(2) . . ? C23 C24 C19 120.10(19) . . ? C27 C26 C31 119.02(18) . . ? C27 C26 N3 121.01(17) . . ? C31 C26 N3 119.91(17) . . ? C26 C27 C28 120.1(2) . . ? C29 C28 C27 120.6(2) . . ? C30 C29 C28 119.3(2) . . ? C29 C30 C31 120.6(2) . . ? C26 C31 C30 120.4(2) . . ? #===END data_(3)-oct2499 _database_code_depnum_ccdc_archive 'CCDC 622820' _audit_creation_date 1999-10-22T16:38:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Al{Me3SiNC(PhMe)NPh}2(Cl/Me)]' _chemical_formula_moiety 'C34.52 H43.56 Al Cl0.48 N4 Si2' _chemical_formula_sum 'C34.52 H43.56 Al Cl0.48 N4 Si2' _chemical_formula_weight 615.12 _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 10.2505(3) _cell_length_b 12.4069(3) _cell_length_c 14.8217(3) _cell_angle_alpha 105.102(1) _cell_angle_beta 101.050(1) _cell_angle_gamma 93.509(1) _cell_volume 1773.81(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12633 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.191 _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_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 22571 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 27.92 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 8390 _reflns_number_gt 6914 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 ; The crystal contains a mixture of the chloride and methyl aluminium compounds. The disorder between Cl and C35 could not be resolved and a single position was refined together with site occupancy factors for Cl and C which refined to 0.52:0.48. The C35 methyl H atoms were omitted. 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^)+(0.0527P)^2^+0.6867P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8390 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.117 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.268 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # 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' Al Al 0.0645 0.0514 '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' Cl Cl 0.1484 0.1585 '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 Al Al 0.28006(4) 0.82155(3) 0.19397(3) 0.02412(11) Uani 1 1 d . . . Si1 Si 0.22288(5) 1.10204(4) 0.22344(3) 0.03211(12) Uani 1 1 d . . . Si2 Si 0.29537(5) 0.53089(3) 0.13829(3) 0.03170(12) Uani 1 1 d . . . N1 N 0.31508(12) 0.98750(10) 0.21482(9) 0.0269(3) Uani 1 1 d . . . N2 N 0.46285(12) 0.86746(10) 0.19152(9) 0.0250(3) Uani 1 1 d . . . N3 N 0.28531(13) 0.66526(10) 0.20948(9) 0.0276(3) Uani 1 1 d . . . N4 N 0.25584(14) 0.81464(10) 0.31854(9) 0.0289(3) Uani 1 1 d . . . C1 C 0.43822(15) 0.97523(12) 0.20342(10) 0.0244(3) Uani 1 1 d . . . C2 C 0.53612(15) 1.06940(12) 0.20317(11) 0.0257(3) Uani 1 1 d . . . C3 C 0.52932(17) 1.10622(13) 0.12188(11) 0.0325(3) Uani 1 1 d . . . H3 H 0.4619 1.0714 0.0663 0.039 Uiso 1 1 calc R . . C4 C 0.62010(18) 1.19346(14) 0.12112(12) 0.0376(4) Uani 1 1 d . . . H4 H 0.6149 1.2173 0.0647 0.045 Uiso 1 1 calc R . . C5 C 0.71874(18) 1.24647(14) 0.20205(13) 0.0371(4) Uani 1 1 d . . . C6 C 0.72245(18) 1.21065(15) 0.28315(13) 0.0397(4) Uani 1 1 d . . . H6 H 0.7881 1.2469 0.3394 0.048 Uiso 1 1 calc R . . C7 C 0.63263(17) 1.12282(14) 0.28461(12) 0.0345(4) Uani 1 1 d . . . H7 H 0.6374 1.0995 0.3412 0.041 Uiso 1 1 calc R . . C8 C 0.8187(2) 1.34028(18) 0.20051(17) 0.0582(6) Uani 1 1 d . . . H8A H 0.8002 1.3538 0.1373 0.087 Uiso 0.5 1 calc PR . . H8B H 0.9094 1.319 0.214 0.087 Uiso 0.5 1 calc PR . . H8C H 0.8114 1.4089 0.2492 0.087 Uiso 0.5 1 calc PR . . H8D H 0.8805 1.3673 0.2631 0.087 Uiso 0.5 1 calc PR . . H8E H 0.7713 1.4021 0.1863 0.087 Uiso 0.5 1 calc PR . . H8F H 0.8693 1.3122 0.1511 0.087 Uiso 0.5 1 calc PR . . C9 C 0.0694(2) 1.05963(18) 0.26062(17) 0.0518(5) Uani 1 1 d . . . H9A H 0.0941 1.0444 0.323 0.078 Uiso 1 1 calc R . . H9B H 0.0209 0.9917 0.2131 0.078 Uiso 1 1 calc R . . H9C H 0.0122 1.1204 0.2655 0.078 Uiso 1 1 calc R . . C10 C 0.3178(2) 1.22868(16) 0.31506(17) 0.0578(6) Uani 1 1 d . . . H10A H 0.3415 1.2119 0.3768 0.087 Uiso 1 1 calc R . . H10B H 0.2623 1.2907 0.321 0.087 Uiso 1 1 calc R . . H10C H 0.3995 1.2502 0.2957 0.087 Uiso 1 1 calc R . . C11 C 0.1761(2) 1.13096(19) 0.10526(15) 0.0541(5) Uani 1 1 d . . . H11A H 0.2573 1.1536 0.0857 0.081 Uiso 1 1 calc R . . H11B H 0.1187 1.1916 0.1101 0.081 Uiso 1 1 calc R . . H11C H 0.1278 1.0629 0.0576 0.081 Uiso 1 1 calc R . . C12 C 0.58614(14) 0.82386(12) 0.18408(10) 0.0246(3) Uani 1 1 d . . . C13 C 0.67241(16) 0.85425(14) 0.13033(11) 0.0323(3) Uani 1 1 d . . . H13 H 0.6499 0.9079 0.0961 0.039 Uiso 1 1 calc R . . C14 C 0.79060(17) 0.80669(15) 0.12653(13) 0.0373(4) Uani 1 1 d . . . H14 H 0.849 0.829 0.0904 0.045 Uiso 1 1 calc R . . C15 C 0.82525(17) 0.72746(15) 0.17428(13) 0.0376(4) Uani 1 1 d . . . H15 H 0.9071 0.6959 0.1718 0.045 Uiso 1 1 calc R . . C16 C 0.73862(17) 0.69474(14) 0.22575(12) 0.0362(4) Uani 1 1 d . . . H16 H 0.7603 0.6391 0.2579 0.043 Uiso 1 1 calc R . . C17 C 0.62058(16) 0.74230(12) 0.23079(11) 0.0299(3) Uani 1 1 d . . . H17 H 0.5622 0.719 0.2666 0.036 Uiso 1 1 calc R . . C18 C 0.26425(15) 0.70367(12) 0.29678(11) 0.0267(3) Uani 1 1 d . . . C19 C 0.25686(16) 0.63529(12) 0.36538(11) 0.0291(3) Uani 1 1 d . . . C20 C 0.14703(18) 0.55790(14) 0.35259(13) 0.0376(4) Uani 1 1 d . . . H20 H 0.0739 0.5482 0.2999 0.045 Uiso 1 1 calc R . . C21 C 0.1439(2) 0.49431(15) 0.41707(14) 0.0431(4) Uani 1 1 d . . . H21 H 0.0676 0.4422 0.4081 0.052 Uiso 1 1 calc R . . C22 C 0.2490(2) 0.50521(15) 0.49354(13) 0.0427(4) Uani 1 1 d . . . C23 C 0.3580(2) 0.58361(17) 0.50643(13) 0.0467(4) Uani 1 1 d . . . H23 H 0.431 0.593 0.5591 0.056 Uiso 1 1 calc R . . C24 C 0.36200(18) 0.64866(15) 0.44341(13) 0.0404(4) Uani 1 1 d . . . H24 H 0.4371 0.7026 0.4538 0.048 Uiso 1 1 calc R . . C25 C 0.2458(3) 0.4337(2) 0.56205(17) 0.0644(6) Uani 1 1 d . . . H25A H 0.1612 0.3842 0.5426 0.097 Uiso 0.5 1 calc PR . . H25B H 0.2536 0.4826 0.627 0.097 Uiso 0.5 1 calc PR . . H25C H 0.3207 0.3883 0.5609 0.097 Uiso 0.5 1 calc PR . . H25D H 0.3291 0.4525 0.6111 0.097 Uiso 0.5 1 calc PR . . H25E H 0.2367 0.3541 0.5267 0.097 Uiso 0.5 1 calc PR . . H25F H 0.1697 0.4484 0.5927 0.097 Uiso 0.5 1 calc PR . . C26 C 0.3402(2) 0.55400(16) 0.02890(13) 0.0472(5) Uani 1 1 d . . . H26A H 0.2713 0.5921 -0.0019 0.071 Uiso 1 1 calc R . . H26B H 0.3464 0.4814 -0.0154 0.071 Uiso 1 1 calc R . . H26C H 0.4267 0.6007 0.0462 0.071 Uiso 1 1 calc R . . C27 C 0.1307(2) 0.44337(16) 0.10517(16) 0.0544(5) Uani 1 1 d . . . H27A H 0.1067 0.4309 0.1629 0.082 Uiso 1 1 calc R . . H27B H 0.1361 0.3709 0.0605 0.082 Uiso 1 1 calc R . . H27C H 0.0623 0.4822 0.0747 0.082 Uiso 1 1 calc R . . C28 C 0.4250(2) 0.45989(16) 0.19937(16) 0.0531(5) Uani 1 1 d . . . H28A H 0.3993 0.448 0.2568 0.08 Uiso 1 1 calc R . . H28B H 0.5113 0.507 0.2177 0.08 Uiso 1 1 calc R . . H28C H 0.4326 0.3872 0.1559 0.08 Uiso 1 1 calc R . . C29 C 0.23557(16) 0.88247(13) 0.40681(11) 0.0302(3) Uani 1 1 d . . . C30 C 0.31862(19) 0.98293(14) 0.45056(12) 0.0377(4) Uani 1 1 d . . . H30 H 0.3894 1.0029 0.4228 0.045 Uiso 1 1 calc R . . C31 C 0.2981(2) 1.05414(16) 0.53498(13) 0.0467(5) Uani 1 1 d . . . H31 H 0.3546 1.1229 0.5643 0.056 Uiso 1 1 calc R . . C32 C 0.1965(2) 1.02578(18) 0.57626(13) 0.0492(5) Uani 1 1 d . . . H32 H 0.1828 1.0746 0.6339 0.059 Uiso 1 1 calc R . . C33 C 0.1149(2) 0.92612(18) 0.53332(13) 0.0456(4) Uani 1 1 d . . . H33 H 0.0455 0.906 0.5622 0.055 Uiso 1 1 calc R . . C34 C 0.13251(18) 0.85429(15) 0.44827(12) 0.0373(4) Uani 1 1 d . . . H34 H 0.0744 0.7864 0.4187 0.045 Uiso 1 1 calc R . . Cl Cl 0.12739(7) 0.78623(6) 0.06902(5) 0.0374(3) Uani 0.479(3) 1 d P . . C35 C 0.12739(7) 0.78623(6) 0.06902(5) 0.0374(3) Uani 0.521(3) 1 d 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.0264(2) 0.0206(2) 0.0268(2) 0.00719(17) 0.00905(17) 0.00064(16) Si1 0.0372(2) 0.0262(2) 0.0376(3) 0.01217(18) 0.01256(19) 0.01008(18) Si2 0.0391(3) 0.0198(2) 0.0340(2) 0.00417(16) 0.00821(19) 0.00029(17) N1 0.0289(6) 0.0220(6) 0.0323(7) 0.0096(5) 0.0099(5) 0.0030(5) N2 0.0261(6) 0.0210(6) 0.0298(6) 0.0089(5) 0.0083(5) 0.0020(5) N3 0.0340(7) 0.0209(6) 0.0285(6) 0.0066(5) 0.0097(5) -0.0001(5) N4 0.0388(7) 0.0230(6) 0.0274(7) 0.0076(5) 0.0126(5) 0.0037(5) C1 0.0281(7) 0.0227(7) 0.0226(7) 0.0073(5) 0.0052(5) 0.0006(6) C2 0.0287(7) 0.0202(6) 0.0296(8) 0.0082(6) 0.0083(6) 0.0019(5) C3 0.0385(9) 0.0306(8) 0.0273(8) 0.0086(6) 0.0060(6) -0.0029(7) C4 0.0488(10) 0.0337(8) 0.0343(9) 0.0149(7) 0.0135(7) -0.0025(7) C5 0.0399(9) 0.0292(8) 0.0430(10) 0.0103(7) 0.0129(7) -0.0041(7) C6 0.0367(9) 0.0393(9) 0.0371(9) 0.0095(7) -0.0006(7) -0.0102(7) C7 0.0352(8) 0.0372(8) 0.0321(8) 0.0163(7) 0.0027(7) -0.0027(7) C8 0.0615(13) 0.0494(11) 0.0605(13) 0.0167(10) 0.0130(10) -0.0237(10) C9 0.0455(11) 0.0554(12) 0.0694(14) 0.0265(10) 0.0303(10) 0.0222(9) C10 0.0682(14) 0.0301(9) 0.0667(14) 0.0015(9) 0.0091(11) 0.0126(9) C11 0.0610(13) 0.0606(13) 0.0546(12) 0.0348(10) 0.0148(10) 0.0226(10) C12 0.0260(7) 0.0222(6) 0.0236(7) 0.0036(5) 0.0050(5) 0.0014(5) C13 0.0339(8) 0.0356(8) 0.0329(8) 0.0153(7) 0.0113(7) 0.0070(7) C14 0.0339(9) 0.0441(9) 0.0406(9) 0.0156(7) 0.0179(7) 0.0077(7) C15 0.0330(8) 0.0403(9) 0.0422(10) 0.0112(7) 0.0117(7) 0.0143(7) C16 0.0409(9) 0.0331(8) 0.0394(9) 0.0158(7) 0.0099(7) 0.0127(7) C17 0.0344(8) 0.0271(7) 0.0305(8) 0.0095(6) 0.0103(6) 0.0034(6) C18 0.0265(7) 0.0255(7) 0.0291(7) 0.0094(6) 0.0070(6) -0.0004(6) C19 0.0351(8) 0.0260(7) 0.0291(8) 0.0101(6) 0.0101(6) 0.0045(6) C20 0.0400(9) 0.0384(9) 0.0368(9) 0.0188(7) 0.0044(7) -0.0027(7) C21 0.0509(11) 0.0384(9) 0.0456(10) 0.0210(8) 0.0134(8) -0.0022(8) C22 0.0612(12) 0.0414(9) 0.0350(9) 0.0204(8) 0.0165(8) 0.0149(9) C23 0.0520(11) 0.0527(11) 0.0361(10) 0.0198(8) 0.0000(8) 0.0099(9) C24 0.0395(9) 0.0426(9) 0.0380(9) 0.0152(8) 0.0025(7) -0.0010(8) C25 0.0925(18) 0.0650(14) 0.0534(13) 0.0404(11) 0.0224(12) 0.0177(13) C26 0.0653(13) 0.0376(9) 0.0394(10) 0.0039(8) 0.0215(9) 0.0091(9) C27 0.0528(12) 0.0383(10) 0.0594(13) -0.0014(9) 0.0078(10) -0.0128(9) C28 0.0624(13) 0.0310(9) 0.0634(13) 0.0132(9) 0.0052(10) 0.0131(9) C29 0.0371(8) 0.0298(7) 0.0260(8) 0.0091(6) 0.0085(6) 0.0095(6) C30 0.0461(10) 0.0350(8) 0.0312(9) 0.0082(7) 0.0076(7) 0.0047(7) C31 0.0602(12) 0.0401(10) 0.0310(9) 0.0002(7) 0.0003(8) 0.0095(9) C32 0.0601(12) 0.0584(12) 0.0259(9) 0.0036(8) 0.0068(8) 0.0251(10) C33 0.0476(11) 0.0638(12) 0.0333(9) 0.0174(9) 0.0172(8) 0.0237(9) C34 0.0382(9) 0.0430(9) 0.0338(9) 0.0122(7) 0.0121(7) 0.0088(7) Cl 0.0341(4) 0.0397(4) 0.0349(4) 0.0076(3) 0.0028(3) 0.0050(3) C35 0.0341(4) 0.0397(4) 0.0349(4) 0.0076(3) 0.0028(3) 0.0050(3) #----------------------------------------------------------------------------# # 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 Al N4 1.9322(13) . ? Al N2 1.9346(13) . ? Al N1 1.9998(12) . ? Al N3 2.0140(13) . ? Al Cl 2.1101(8) . ? Al C1 2.3831(14) . ? Al C18 2.3904(15) . ? Si1 N1 1.7450(13) . ? Si1 C9 1.854(2) . ? Si1 C11 1.858(2) . ? Si1 C10 1.859(2) . ? Si2 N3 1.7463(13) . ? Si2 C26 1.8533(19) . ? Si2 C27 1.858(2) . ? Si2 C28 1.859(2) . ? N1 C1 1.3179(19) . ? N2 C1 1.3485(18) . ? N2 C12 1.4169(19) . ? N3 C18 1.3214(19) . ? N4 C18 1.3419(19) . ? N4 C29 1.4196(19) . ? C1 C2 1.4940(19) . ? C2 C7 1.386(2) . ? C2 C3 1.387(2) . ? C3 C4 1.387(2) . ? C4 C5 1.391(2) . ? C5 C6 1.381(2) . ? C5 C8 1.511(2) . ? C6 C7 1.390(2) . ? C12 C17 1.394(2) . ? C12 C13 1.394(2) . ? C13 C14 1.384(2) . ? C14 C15 1.379(2) . ? C15 C16 1.383(2) . ? C16 C17 1.385(2) . ? C18 C19 1.494(2) . ? C19 C20 1.384(2) . ? C19 C24 1.388(2) . ? C20 C21 1.392(2) . ? C21 C22 1.377(3) . ? C22 C23 1.386(3) . ? C22 C25 1.515(2) . ? C23 C24 1.389(2) . ? C29 C34 1.390(2) . ? C29 C30 1.391(2) . ? C30 C31 1.392(2) . ? C31 C32 1.376(3) . ? C32 C33 1.376(3) . ? C33 C34 1.392(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Al N2 113.69(6) . . ? N4 Al N1 101.31(5) . . ? N2 Al N1 67.98(5) . . ? N4 Al N3 67.68(5) . . ? N2 Al N3 103.75(5) . . ? N1 Al N3 163.04(6) . . ? N4 Al Cl 125.59(5) . . ? N2 Al Cl 120.71(5) . . ? N1 Al Cl 97.91(5) . . ? N3 Al Cl 99.02(5) . . ? N4 Al C1 112.35(5) . . ? N2 Al C1 34.45(5) . . ? N1 Al C1 33.57(5) . . ? N3 Al C1 136.96(6) . . ? Cl Al C1 111.61(4) . . ? N4 Al C18 34.13(5) . . ? N2 Al C18 113.00(5) . . ? N1 Al C18 134.34(6) . . ? N3 Al C18 33.55(5) . . ? Cl Al C18 115.91(4) . . ? C1 Al C18 132.47(5) . . ? N1 Si1 C9 105.56(8) . . ? N1 Si1 C11 110.44(8) . . ? C9 Si1 C11 109.51(11) . . ? N1 Si1 C10 110.96(8) . . ? C9 Si1 C10 109.65(11) . . ? C11 Si1 C10 110.59(11) . . ? N3 Si2 C26 104.77(7) . . ? N3 Si2 C27 110.67(8) . . ? C26 Si2 C27 109.25(10) . . ? N3 Si2 C28 111.56(8) . . ? C26 Si2 C28 110.64(10) . . ? C27 Si2 C28 109.83(10) . . ? C1 N1 Si1 132.15(10) . . ? C1 N1 Al 89.38(9) . . ? Si1 N1 Al 137.63(7) . . ? C1 N2 C12 127.32(12) . . ? C1 N2 Al 91.30(9) . . ? C12 N2 Al 141.37(10) . . ? C18 N3 Si2 133.32(11) . . ? C18 N3 Al 89.05(9) . . ? Si2 N3 Al 137.34(7) . . ? C18 N4 C29 125.83(13) . . ? C18 N4 Al 91.99(9) . . ? C29 N4 Al 142.19(10) . . ? N1 C1 N2 111.20(12) . . ? N1 C1 C2 123.73(13) . . ? N2 C1 C2 125.07(13) . . ? N1 C1 Al 57.05(7) . . ? N2 C1 Al 54.25(7) . . ? C2 C1 Al 176.68(10) . . ? C7 C2 C3 119.16(14) . . ? C7 C2 C1 120.57(13) . . ? C3 C2 C1 120.25(13) . . ? C2 C3 C4 120.53(15) . . ? C3 C4 C5 120.75(15) . . ? C6 C5 C4 118.10(15) . . ? C6 C5 C8 121.29(17) . . ? C4 C5 C8 120.61(16) . . ? C5 C6 C7 121.70(15) . . ? C2 C7 C6 119.74(15) . . ? C17 C12 C13 118.10(14) . . ? C17 C12 N2 117.60(13) . . ? C13 C12 N2 124.25(13) . . ? C14 C13 C12 120.36(15) . . ? C15 C14 C13 121.25(15) . . ? C14 C15 C16 118.76(15) . . ? C15 C16 C17 120.58(15) . . ? C16 C17 C12 120.91(14) . . ? N3 C18 N4 111.27(13) . . ? N3 C18 C19 125.26(13) . . ? N4 C18 C19 123.41(13) . . ? N3 C18 Al 57.39(8) . . ? N4 C18 Al 53.89(7) . . ? C19 C18 Al 177.01(11) . . ? C20 C19 C24 118.97(15) . . ? C20 C19 C18 121.28(14) . . ? C24 C19 C18 119.75(14) . . ? C19 C20 C21 119.91(16) . . ? C22 C21 C20 121.56(17) . . ? C21 C22 C23 118.20(16) . . ? C21 C22 C25 121.13(19) . . ? C23 C22 C25 120.68(19) . . ? C22 C23 C24 120.96(17) . . ? C19 C24 C23 120.36(17) . . ? C34 C29 C30 119.33(15) . . ? C34 C29 N4 122.26(15) . . ? C30 C29 N4 118.35(14) . . ? C29 C30 C31 120.04(17) . . ? C32 C31 C30 120.56(18) . . ? C33 C32 C31 119.39(17) . . ? C32 C33 C34 121.07(18) . . ? C29 C34 C33 119.60(17) . . ? #===END data_(4)-apr399 _database_code_depnum_ccdc_archive 'CCDC 622821' _audit_creation_date 2000-05-26T09:34:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Sn{Me3SiNC(C6H4-Me)NPh}2]' _chemical_formula_moiety 'C34 H42 N4 Si2 Sn' _chemical_formula_sum 'C34 H42 N4 Si2 Sn' _chemical_formula_weight 681.59 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.945(4) _cell_length_b 11.592(3) _cell_length_c 14.515(5) _cell_angle_alpha 90.22(2) _cell_angle_beta 111.95(3) _cell_angle_gamma 91.32(3) _cell_volume 1707.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details Psi-scans #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5982 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0385 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5982 _reflns_number_gt 5517 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material SHELXL-93 #----------------------------------------------------------------------------# # 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^)+(0.0268P)^2^+1.5912P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 5982 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.884 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.064 #----------------------------------------------------------------------------# # 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' #Sn Sn -0.6537 1.4246 '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 Sn Sn 0.508962(16) 0.762327(14) 0.593345(12) 0.02459(7) Uani 1 1 d . . . Si1 Si 0.75951(7) 0.84660(6) 0.47953(5) 0.02505(15) Uani 1 1 d . . . Si2 Si 0.41912(7) 0.66043(6) 0.81313(5) 0.02565(15) Uani 1 1 d . . . N1 N 0.6418(2) 0.88957(18) 0.70061(15) 0.0256(4) Uani 1 1 d . . . N2 N 0.7009(2) 0.83845(17) 0.57518(15) 0.0248(4) Uani 1 1 d . . . N3 N 0.6351(2) 0.61344(18) 0.65494(16) 0.0253(4) Uani 1 1 d . . . N4 N 0.5149(2) 0.67029(17) 0.74121(16) 0.0257(4) Uani 1 1 d . . . C1 C 0.7267(2) 0.9037(2) 0.65545(17) 0.0232(5) Uani 1 1 d . . . C2 C 0.8384(2) 0.9894(2) 0.69244(17) 0.0234(5) Uani 1 1 d . . . C3 C 0.9677(3) 0.9553(2) 0.72351(18) 0.0270(5) Uani 1 1 d . . . H3 H 0.9861 0.8761 0.7196 0.032 Uiso 1 1 calc R . . C4 C 1.0704(3) 1.0352(2) 0.76009(19) 0.0304(6) Uani 1 1 d . . . H4 H 1.1585 1.0098 0.7816 0.036 Uiso 1 1 calc R . . C5 C 1.0479(3) 1.1518(2) 0.7661(2) 0.0321(6) Uani 1 1 d . . . C6 C 0.9175(3) 1.1862(2) 0.7326(2) 0.0346(6) Uani 1 1 d . . . H6 H 0.8993 1.2658 0.7343 0.041 Uiso 1 1 calc R . . C7 C 0.8143(3) 1.1067(2) 0.6970(2) 0.0308(6) Uani 1 1 d . . . H7 H 0.7262 1.132 0.6754 0.037 Uiso 1 1 calc R . . C8 C 1.1601(3) 1.2382(3) 0.8087(3) 0.0483(8) Uani 1 1 d . . . H8A H 1.1249 1.3156 0.8066 0.072 Uiso 0.5 1 calc PR . . H8B H 1.216 1.2368 0.7694 0.072 Uiso 0.5 1 calc PR . . H8C H 1.2124 1.2187 0.8776 0.072 Uiso 0.5 1 calc PR . . H8D H 1.244 1.1984 0.8292 0.072 Uiso 0.5 1 calc PR . . H8E H 1.1528 1.2773 0.8663 0.072 Uiso 0.5 1 calc PR . . H8F H 1.1565 1.2953 0.7581 0.072 Uiso 0.5 1 calc PR . . C9 C 0.6574(3) 0.9353(2) 0.79471(18) 0.0253(5) Uani 1 1 d . . . C10 C 0.5544(3) 0.9937(2) 0.8059(2) 0.0306(6) Uani 1 1 d . . . H10 H 0.4753 1.0041 0.75 0.037 Uiso 1 1 calc R . . C11 C 0.5663(3) 1.0370(2) 0.8979(2) 0.0390(7) Uani 1 1 d . . . H11 H 0.4952 1.0768 0.9048 0.047 Uiso 1 1 calc R . . C12 C 0.6805(3) 1.0227(3) 0.9797(2) 0.0414(7) Uani 1 1 d . . . H12 H 0.6884 1.0529 1.0427 0.05 Uiso 1 1 calc R . . C13 C 0.7831(3) 0.9644(3) 0.9695(2) 0.0390(7) Uani 1 1 d . . . H13 H 0.8619 0.9544 1.0257 0.047 Uiso 1 1 calc R . . C14 C 0.7720(3) 0.9201(2) 0.8777(2) 0.0319(6) Uani 1 1 d . . . H14 H 0.8428 0.8793 0.8715 0.038 Uiso 1 1 calc R . . C15 C 0.9183(3) 0.7729(2) 0.5075(2) 0.0345(6) Uani 1 1 d . . . H15C H 0.942 0.7741 0.4487 0.052 Uiso 1 1 calc R . . H15B H 0.9092 0.6928 0.5258 0.052 Uiso 1 1 calc R . . H15A H 0.9876 0.813 0.5628 0.052 Uiso 1 1 calc R . . C16 C 0.7799(3) 0.9981(2) 0.4451(2) 0.0364(6) Uani 1 1 d . . . H16C H 0.8496 1.0375 0.5005 0.055 Uiso 1 1 calc R . . H16B H 0.697 1.0382 0.43 0.055 Uiso 1 1 calc R . . H16A H 0.804 0.9985 0.3865 0.055 Uiso 1 1 calc R . . C17 C 0.6283(3) 0.7688(3) 0.3749(2) 0.0422(7) Uani 1 1 d . . . H17C H 0.5446 0.8078 0.3592 0.063 Uiso 1 1 calc R . . H17B H 0.6189 0.6891 0.3942 0.063 Uiso 1 1 calc R . . H17A H 0.6525 0.7686 0.3163 0.063 Uiso 1 1 calc R . . C18 C 0.6068(2) 0.6012(2) 0.73643(19) 0.0245(5) Uani 1 1 d . . . C19 C 0.6764(2) 0.5174(2) 0.81408(19) 0.0250(5) Uani 1 1 d . . . C20 C 0.7540(3) 0.5556(2) 0.90940(19) 0.0287(6) Uani 1 1 d . . . H20 H 0.7571 0.6353 0.9258 0.034 Uiso 1 1 calc R . . C21 C 0.8264(3) 0.4795(2) 0.9803(2) 0.0326(6) Uani 1 1 d . . . H21 H 0.8806 0.5078 1.0444 0.039 Uiso 1 1 calc R . . C22 C 0.8216(3) 0.3614(2) 0.9596(2) 0.0322(6) Uani 1 1 d . . . C23 C 0.7407(3) 0.3233(2) 0.8654(2) 0.0321(6) Uani 1 1 d . . . H23 H 0.7331 0.243 0.8504 0.039 Uiso 1 1 calc R . . C24 C 0.6708(3) 0.3995(2) 0.7929(2) 0.0294(6) Uani 1 1 d . . . H24 H 0.6186 0.3714 0.7282 0.035 Uiso 1 1 calc R . . C25 C 0.9038(3) 0.2786(3) 1.0359(3) 0.0480(8) Uani 1 1 d . . . H25A H 0.9543 0.3208 1.0975 0.072 Uiso 0.5 1 calc PR . . H25B H 0.9646 0.2406 1.0109 0.072 Uiso 0.5 1 calc PR . . H25C H 0.8462 0.2203 1.0489 0.072 Uiso 0.5 1 calc PR . . H25D H 0.8891 0.2003 1.0073 0.072 Uiso 0.5 1 calc PR . . H25E H 0.8788 0.2806 1.094 0.072 Uiso 0.5 1 calc PR . . H25F H 0.9972 0.3008 1.0559 0.072 Uiso 0.5 1 calc PR . . C26 C 0.7445(3) 0.5638(2) 0.6416(2) 0.0264(5) Uani 1 1 d . . . C27 C 0.8720(3) 0.5829(2) 0.7099(2) 0.0325(6) Uani 1 1 d . . . H27 H 0.8868 0.63 0.767 0.039 Uiso 1 1 calc R . . C28 C 0.9773(3) 0.5342(3) 0.6955(2) 0.0398(7) Uani 1 1 d . . . H28 H 1.0638 0.5466 0.7436 0.048 Uiso 1 1 calc R . . C29 C 0.9584(3) 0.4679(3) 0.6122(3) 0.0437(8) Uani 1 1 d . . . H29 H 1.0313 0.4347 0.6024 0.052 Uiso 1 1 calc R . . C30 C 0.8331(4) 0.4504(3) 0.5436(3) 0.0462(8) Uani 1 1 d . . . H30 H 0.8196 0.4047 0.4859 0.055 Uiso 1 1 calc R . . C31 C 0.7254(3) 0.4982(2) 0.5569(2) 0.0361(6) Uani 1 1 d . . . H31 H 0.6393 0.4861 0.5083 0.043 Uiso 1 1 calc R . . C32 C 0.2778(3) 0.7557(3) 0.7510(2) 0.0395(7) Uani 1 1 d . . . H32C H 0.2306 0.7289 0.6824 0.059 Uiso 1 1 calc R . . H32B H 0.3106 0.8351 0.751 0.059 Uiso 1 1 calc R . . H32A H 0.2177 0.7533 0.7869 0.059 Uiso 1 1 calc R . . C33 C 0.5053(3) 0.7131(3) 0.9438(2) 0.0405(7) Uani 1 1 d . . . H33C H 0.5373 0.7927 0.9436 0.061 Uiso 1 1 calc R . . H33B H 0.5801 0.6639 0.9778 0.061 Uiso 1 1 calc R . . H33A H 0.4439 0.7104 0.9785 0.061 Uiso 1 1 calc R . . C34 C 0.3584(3) 0.5089(2) 0.8141(3) 0.0415(7) Uani 1 1 d . . . H34C H 0.2986 0.5061 0.8502 0.062 Uiso 1 1 calc R . . H34B H 0.4334 0.4595 0.8468 0.062 Uiso 1 1 calc R . . H34A H 0.3113 0.4815 0.7456 0.062 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 Sn 0.02227(10) 0.02300(10) 0.02747(10) -0.00411(7) 0.00821(7) -0.00009(6) Si1 0.0298(4) 0.0245(3) 0.0229(3) -0.0034(3) 0.0122(3) 0.0001(3) Si2 0.0251(4) 0.0222(3) 0.0350(4) 0.0007(3) 0.0173(3) 0.0023(3) N1 0.0278(11) 0.0246(11) 0.0266(11) -0.0050(8) 0.0131(9) -0.0058(9) N2 0.0290(11) 0.0205(10) 0.0265(11) -0.0036(8) 0.0123(9) -0.0004(8) N3 0.0247(11) 0.0227(11) 0.0328(11) 0.0000(9) 0.0158(9) 0.0015(8) N4 0.0260(11) 0.0214(10) 0.0335(12) -0.0017(9) 0.0158(9) -0.0006(8) C1 0.0280(13) 0.0200(12) 0.0226(12) 0.0008(9) 0.0105(10) 0.0022(10) C2 0.0300(13) 0.0233(12) 0.0192(12) -0.0016(9) 0.0120(10) -0.0025(10) C3 0.0321(14) 0.0264(13) 0.0229(12) -0.0032(10) 0.0109(11) 0.0009(11) C4 0.0277(14) 0.0380(15) 0.0252(13) -0.0019(11) 0.0096(11) 0.0002(11) C5 0.0354(15) 0.0352(15) 0.0289(14) -0.0047(11) 0.0164(12) -0.0107(12) C6 0.0435(16) 0.0225(13) 0.0433(16) -0.0039(11) 0.0232(13) -0.0064(12) C7 0.0309(14) 0.0249(13) 0.0393(15) -0.0020(11) 0.0164(12) 0.0006(11) C8 0.0481(19) 0.0460(18) 0.0508(19) -0.0090(15) 0.0199(15) -0.0203(15) C9 0.0332(14) 0.0208(12) 0.0253(12) -0.0034(10) 0.0152(11) -0.0048(10) C10 0.0328(14) 0.0306(14) 0.0323(14) 0.0014(11) 0.0166(12) -0.0003(11) C11 0.0487(18) 0.0342(15) 0.0441(17) -0.0086(13) 0.0290(15) -0.0003(13) C12 0.060(2) 0.0400(17) 0.0308(15) -0.0124(12) 0.0260(15) -0.0124(14) C13 0.0437(17) 0.0468(17) 0.0252(14) -0.0009(12) 0.0121(12) -0.0097(14) C14 0.0351(15) 0.0323(14) 0.0315(14) -0.0006(11) 0.0163(12) -0.0014(11) C15 0.0401(16) 0.0323(15) 0.0377(15) -0.0006(12) 0.0219(13) 0.0059(12) C16 0.0501(18) 0.0317(15) 0.0344(15) 0.0054(12) 0.0235(13) 0.0044(13) C17 0.0465(18) 0.0499(18) 0.0284(14) -0.0110(13) 0.0125(13) -0.0077(14) C18 0.0228(12) 0.0188(12) 0.0340(14) -0.0056(10) 0.0134(11) -0.0046(9) C19 0.0210(12) 0.0255(13) 0.0328(13) -0.0037(10) 0.0149(10) -0.0006(10) C20 0.0300(14) 0.0250(13) 0.0342(14) -0.0054(11) 0.0157(11) -0.0008(10) C21 0.0301(14) 0.0350(15) 0.0307(14) -0.0030(11) 0.0093(11) -0.0039(11) C22 0.0289(14) 0.0306(14) 0.0397(15) 0.0049(12) 0.0159(12) 0.0014(11) C23 0.0363(15) 0.0214(13) 0.0408(15) -0.0013(11) 0.0170(12) -0.0001(11) C24 0.0306(14) 0.0249(13) 0.0328(14) -0.0053(11) 0.0121(11) -0.0026(11) C25 0.0435(18) 0.0412(18) 0.0507(19) 0.0075(15) 0.0078(15) 0.0030(14) C26 0.0296(13) 0.0188(12) 0.0354(14) -0.0005(10) 0.0174(11) 0.0017(10) C27 0.0322(14) 0.0348(15) 0.0356(15) -0.0027(12) 0.0183(12) 0.0023(12) C28 0.0311(15) 0.0450(17) 0.0487(18) 0.0089(14) 0.0205(13) 0.0064(13) C29 0.0478(19) 0.0348(16) 0.065(2) 0.0070(15) 0.0395(17) 0.0141(14) C30 0.066(2) 0.0316(16) 0.056(2) -0.0125(14) 0.0407(18) 0.0006(14) C31 0.0395(16) 0.0311(15) 0.0420(16) -0.0100(12) 0.0208(13) -0.0054(12) C32 0.0348(16) 0.0384(16) 0.0533(18) 0.0051(14) 0.0250(14) 0.0092(13) C33 0.0442(17) 0.0464(18) 0.0385(16) -0.0020(13) 0.0240(14) 0.0030(14) C34 0.0375(16) 0.0294(15) 0.067(2) 0.0080(14) 0.0301(15) 0.0009(12) #----------------------------------------------------------------------------# # 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 Sn N3 2.210(2) . ? Sn N1 2.215(2) . ? Sn N2 2.365(2) . ? Sn N4 2.380(2) . ? Si1 N2 1.736(2) . ? Si1 C16 1.859(3) . ? Si1 C15 1.860(3) . ? Si1 C17 1.866(3) . ? Si2 N4 1.736(2) . ? Si2 C32 1.863(3) . ? Si2 C34 1.866(3) . ? Si2 C33 1.867(3) . ? N1 C1 1.330(3) . ? N1 C9 1.411(3) . ? N2 C1 1.322(3) . ? N3 C18 1.338(3) . ? N3 C26 1.417(3) . ? N4 C18 1.321(3) . ? C1 C2 1.489(3) . ? C2 C3 1.383(4) . ? C2 C7 1.397(4) . ? C3 C4 1.380(4) . ? C4 C5 1.388(4) . ? C5 C6 1.394(4) . ? C5 C8 1.505(4) . ? C6 C7 1.379(4) . ? C9 C10 1.389(4) . ? C9 C14 1.392(4) . ? C10 C11 1.383(4) . ? C11 C12 1.379(5) . ? C12 C13 1.377(4) . ? C13 C14 1.387(4) . ? C18 C19 1.482(4) . ? C19 C20 1.390(4) . ? C19 C24 1.394(4) . ? C20 C21 1.377(4) . ? C21 C22 1.396(4) . ? C22 C23 1.386(4) . ? C22 C25 1.504(4) . ? C23 C24 1.382(4) . ? C26 C31 1.388(4) . ? C26 C27 1.389(4) . ? C27 C28 1.378(4) . ? C28 C29 1.377(4) . ? C29 C30 1.371(5) . ? C30 C31 1.391(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Sn N1 94.92(8) . . ? N3 Sn N2 83.12(8) . . ? N1 Sn N2 58.17(8) . . ? N3 Sn N4 58.15(8) . . ? N1 Sn N4 82.53(8) . . ? N2 Sn N4 122.30(8) . . ? N2 Si1 C16 112.27(12) . . ? N2 Si1 C15 113.34(12) . . ? C16 Si1 C15 108.44(14) . . ? N2 Si1 C17 103.08(13) . . ? C16 Si1 C17 110.51(15) . . ? C15 Si1 C17 109.07(14) . . ? N4 Si2 C32 104.73(12) . . ? N4 Si2 C34 110.58(12) . . ? C32 Si2 C34 110.07(14) . . ? N4 Si2 C33 113.86(13) . . ? C32 Si2 C33 108.24(14) . . ? C34 Si2 C33 109.23(15) . . ? C1 N1 C9 125.6(2) . . ? C1 N1 Sn 96.91(15) . . ? C9 N1 Sn 136.86(16) . . ? C1 N2 Si1 131.01(18) . . ? C1 N2 Sn 90.41(15) . . ? Si1 N2 Sn 135.71(11) . . ? C18 N3 C26 124.3(2) . . ? C18 N3 Sn 97.17(15) . . ? C26 N3 Sn 135.68(16) . . ? C18 N4 Si2 129.77(18) . . ? C18 N4 Sn 89.97(15) . . ? Si2 N4 Sn 138.38(12) . . ? N2 C1 N1 114.5(2) . . ? N2 C1 C2 124.0(2) . . ? N1 C1 C2 121.5(2) . . ? C3 C2 C7 118.5(2) . . ? C3 C2 C1 121.2(2) . . ? C7 C2 C1 120.4(2) . . ? C4 C3 C2 120.6(2) . . ? C3 C4 C5 121.5(3) . . ? C4 C5 C6 117.7(2) . . ? C4 C5 C8 121.4(3) . . ? C6 C5 C8 120.9(3) . . ? C7 C6 C5 121.1(3) . . ? C6 C7 C2 120.6(3) . . ? C10 C9 C14 118.9(2) . . ? C10 C9 N1 119.3(2) . . ? C14 C9 N1 121.8(2) . . ? C11 C10 C9 120.4(3) . . ? C12 C11 C10 120.5(3) . . ? C13 C12 C11 119.5(3) . . ? C12 C13 C14 120.4(3) . . ? C13 C14 C9 120.3(3) . . ? N4 C18 N3 114.4(2) . . ? N4 C18 C19 124.3(2) . . ? N3 C18 C19 121.3(2) . . ? C20 C19 C24 118.3(2) . . ? C20 C19 C18 120.3(2) . . ? C24 C19 C18 121.4(2) . . ? C21 C20 C19 120.8(2) . . ? C20 C21 C22 121.2(3) . . ? C23 C22 C21 117.7(3) . . ? C23 C22 C25 121.0(3) . . ? C21 C22 C25 121.3(3) . . ? C24 C23 C22 121.4(2) . . ? C23 C24 C19 120.4(2) . . ? C31 C26 C27 118.9(2) . . ? C31 C26 N3 119.7(2) . . ? C27 C26 N3 121.3(2) . . ? C28 C27 C26 120.5(3) . . ? C29 C28 C27 120.7(3) . . ? C30 C29 C28 119.1(3) . . ? C29 C30 C31 121.1(3) . . ? C26 C31 C30 119.6(3) . . ? #===END data_(6)-dec599 _database_code_depnum_ccdc_archive 'CCDC 622822' _audit_creation_date 1999-12-07T10:21:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[ZrCl{Me3SiNC(C6H4Me)NPh}3].3(toluene)' _chemical_formula_moiety 'C51 H63 Cl1 N6 Si3 Zr1, 3(C7 H8)' _chemical_formula_sum 'C72 H87 Cl N6 Si3 Zr' _chemical_formula_weight 1247.42 _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 14.1992(5) _cell_length_b 16.9004(7) _cell_length_c 17.7967(7) _cell_angle_alpha 114.887(2) _cell_angle_beta 98.208(2) _cell_angle_gamma 105.088(2) _cell_volume 3582.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 68640 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.284 _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 0.738 _exptl_absorpt_correction_T_max 0.927 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _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_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 32825 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_av_sigmaI/netI 0.0634 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 12331 _reflns_number_gt 9899 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 ; One of the three toluene solvate molecules is disordered over two partially overlapping sites and H atoms were omittted for this molecule. 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^)+(0.0789P)^2^+14.9844P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 12331 _refine_ls_number_parameters 655 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2258 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.087 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' Zr Zr -2.9673 0.5597 '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 Zr Zr 0.81501(4) 0.77452(3) 0.68675(3) 0.02955(17) Uani 1 1 d . . . Cl Cl 0.72048(12) 0.66784(10) 0.53311(9) 0.0490(4) Uani 1 1 d . . . Si1 Si 0.92074(12) 0.58913(10) 0.60856(10) 0.0372(4) Uani 1 1 d . . . Si2 Si 0.85823(13) 0.90586(12) 0.56868(11) 0.0427(4) Uani 1 1 d . . . Si3 Si 0.54685(13) 0.67728(12) 0.67393(14) 0.0546(5) Uani 1 1 d . . . N1 N 0.8307(3) 0.7427(3) 0.7996(3) 0.0315(9) Uani 1 1 d . . . N2 N 0.8697(3) 0.6609(3) 0.6809(3) 0.0317(9) Uani 1 1 d . . . N3 N 0.9866(3) 0.8605(3) 0.7501(3) 0.0309(9) Uani 1 1 d . . . N4 N 0.8974(3) 0.8691(3) 0.6420(3) 0.0347(10) Uani 1 1 d . . . N5 N 0.7892(3) 0.9070(3) 0.7773(3) 0.0305(9) Uani 1 1 d . . . N6 N 0.6628(3) 0.7687(3) 0.7071(3) 0.0363(10) Uani 1 1 d . . . C1 C 0.8562(4) 0.6689(3) 0.7564(3) 0.0320(11) Uani 1 1 d . . . C2 C 0.8706(4) 0.6024(3) 0.7871(3) 0.0325(11) Uani 1 1 d . . . C3 C 0.8103(4) 0.5081(4) 0.7401(4) 0.0384(12) Uani 1 1 d . . . H3 H 0.7582 0.486 0.6885 0.046 Uiso 1 1 calc R . . C4 C 0.8261(5) 0.4463(4) 0.7683(4) 0.0433(13) Uani 1 1 d . . . H4 H 0.7831 0.3824 0.7364 0.052 Uiso 1 1 calc R . . C5 C 0.9030(5) 0.4757(4) 0.8417(4) 0.0459(14) Uani 1 1 d . . . C6 C 0.9631(5) 0.5704(4) 0.8886(4) 0.0486(15) Uani 1 1 d . . . H6 H 1.0164 0.5921 0.9393 0.058 Uiso 1 1 calc R . . C7 C 0.9463(5) 0.6334(4) 0.8621(4) 0.0427(13) Uani 1 1 d . . . H7 H 0.9868 0.6978 0.8956 0.051 Uiso 1 1 calc R . . C8 C 0.9219(7) 0.4086(5) 0.8719(5) 0.064(2) Uani 1 1 d . . . H8A H 0.9793 0.4426 0.9247 0.097 Uiso 0.5 1 calc PR . . H8B H 0.9379 0.3603 0.8267 0.097 Uiso 0.5 1 calc PR . . H8C H 0.8608 0.3793 0.8839 0.097 Uiso 0.5 1 calc PR . . H8D H 0.8727 0.3456 0.8322 0.097 Uiso 0.5 1 calc PR . . H8E H 0.9141 0.4278 0.9302 0.097 Uiso 0.5 1 calc PR . . H8F H 0.9912 0.4088 0.873 0.097 Uiso 0.5 1 calc PR . . C9 C 0.7927(4) 0.7584(4) 0.8718(3) 0.0333(11) Uani 1 1 d . . . C10 C 0.7336(5) 0.6874(4) 0.8842(4) 0.0448(14) Uani 1 1 d . . . H10 H 0.7198 0.624 0.8441 0.054 Uiso 1 1 calc R . . C11 C 0.6950(5) 0.7084(5) 0.9541(4) 0.0503(15) Uani 1 1 d . . . H11 H 0.6539 0.6589 0.9607 0.06 Uiso 1 1 calc R . . C12 C 0.7143(5) 0.7991(4) 1.0146(3) 0.0429(14) Uani 1 1 d . . . H12 H 0.6899 0.8126 1.0639 0.052 Uiso 1 1 calc R . . C13 C 0.7707(4) 0.8707(4) 1.0015(4) 0.0396(13) Uani 1 1 d . . . H13 H 0.7819 0.9338 1.0408 0.048 Uiso 1 1 calc R . . C14 C 0.8107(4) 0.8507(4) 0.9316(3) 0.0351(12) Uani 1 1 d . . . H14 H 0.8507 0.9003 0.9245 0.042 Uiso 1 1 calc R . . C15 C 0.9736(5) 0.6516(4) 0.5497(4) 0.0463(14) Uani 1 1 d . . . H15A H 0.9191 0.6625 0.5196 0.069 Uiso 1 1 calc R . . H15B H 1.0021 0.6133 0.5075 0.069 Uiso 1 1 calc R . . H15C H 1.0273 0.7115 0.5912 0.069 Uiso 1 1 calc R . . C16 C 0.8187(5) 0.4767(4) 0.5260(4) 0.0533(16) Uani 1 1 d . . . H16A H 0.7655 0.4895 0.4965 0.08 Uiso 1 1 calc R . . H16B H 0.7892 0.4419 0.5544 0.08 Uiso 1 1 calc R . . H16C H 0.8479 0.4396 0.4835 0.08 Uiso 1 1 calc R . . C17 C 1.0235(5) 0.5679(5) 0.6657(4) 0.0501(15) Uani 1 1 d . . . H17A H 1.0762 0.6277 0.7087 0.075 Uiso 1 1 calc R . . H17B H 1.0536 0.5312 0.6238 0.075 Uiso 1 1 calc R . . H17C H 0.995 0.5333 0.6947 0.075 Uiso 1 1 calc R . . C18 C 0.9896(4) 0.8924(3) 0.6934(3) 0.0319(11) Uani 1 1 d . . . C19 C 1.0846(4) 0.9493(4) 0.6867(3) 0.0361(12) Uani 1 1 d . . . C20 C 1.1180(5) 0.9154(4) 0.6137(4) 0.0424(13) Uani 1 1 d . . . H20 H 1.0804 0.8543 0.5673 0.051 Uiso 1 1 calc R . . C21 C 1.2052(5) 0.9695(5) 0.6081(4) 0.0483(15) Uani 1 1 d . . . H21 H 1.2277 0.9444 0.5583 0.058 Uiso 1 1 calc R . . C22 C 1.2604(4) 1.0595(5) 0.6733(4) 0.0479(15) Uani 1 1 d . . . C23 C 1.2249(5) 1.0943(4) 0.7453(4) 0.0479(15) Uani 1 1 d . . . H23 H 1.26 1.1568 0.79 0.058 Uiso 1 1 calc R . . C24 C 1.1397(4) 1.0399(4) 0.7529(4) 0.0400(13) Uani 1 1 d . . . H24 H 1.1186 1.0642 0.8036 0.048 Uiso 1 1 calc R . . C25 C 1.3568(5) 1.1209(6) 0.6688(5) 0.072(2) Uani 1 1 d . . . H25A H 1.3842 1.1815 0.7215 0.107 Uiso 0.5 1 calc PR . . H25B H 1.3407 1.1301 0.6183 0.107 Uiso 0.5 1 calc PR . . H25C H 1.4075 1.0906 0.6637 0.107 Uiso 0.5 1 calc PR . . H25D H 1.3707 1.0866 0.6142 0.107 Uiso 0.5 1 calc PR . . H25E H 1.4142 1.138 0.7173 0.107 Uiso 0.5 1 calc PR . . H25F H 1.3475 1.1776 0.672 0.107 Uiso 0.5 1 calc PR . . C26 C 1.0723(4) 0.8573(3) 0.7997(3) 0.0343(11) Uani 1 1 d . . . C27 C 1.0744(4) 0.8706(4) 0.8826(3) 0.0375(12) Uani 1 1 d . . . H27 H 1.0217 0.8859 0.9061 0.045 Uiso 1 1 calc R . . C28 C 1.1522(5) 0.8618(4) 0.9314(4) 0.0459(14) Uani 1 1 d . . . H28 H 1.153 0.8724 0.9884 0.055 Uiso 1 1 calc R . . C29 C 1.2285(5) 0.8377(4) 0.8978(4) 0.0508(15) Uani 1 1 d . . . H29 H 1.2809 0.8299 0.9305 0.061 Uiso 1 1 calc R . . C30 C 1.2271(5) 0.8251(5) 0.8153(5) 0.0536(16) Uani 1 1 d . . . H30 H 1.28 0.8095 0.792 0.064 Uiso 1 1 calc R . . C31 C 1.1505(4) 0.8346(4) 0.7666(4) 0.0431(13) Uani 1 1 d . . . H31 H 1.151 0.8257 0.7103 0.052 Uiso 1 1 calc R . . C32 C 0.8628(6) 0.8286(5) 0.4590(4) 0.0581(17) Uani 1 1 d . . . H32A H 0.8209 0.7638 0.4404 0.087 Uiso 1 1 calc R . . H32B H 0.9334 0.8332 0.4605 0.087 Uiso 1 1 calc R . . H32C H 0.8365 0.8479 0.4181 0.087 Uiso 1 1 calc R . . C33 C 0.9370(6) 1.0299(5) 0.6058(5) 0.0606(18) Uani 1 1 d . . . H33A H 0.9339 1.0696 0.6637 0.091 Uiso 1 1 calc R . . H33B H 0.9106 1.0499 0.5655 0.091 Uiso 1 1 calc R . . H33C H 1.0078 1.0354 0.6076 0.091 Uiso 1 1 calc R . . C34 C 0.7230(5) 0.8958(5) 0.5648(4) 0.0544(16) Uani 1 1 d . . . H34A H 0.72 0.9365 0.6225 0.082 Uiso 1 1 calc R . . H34B H 0.6817 0.831 0.5463 0.082 Uiso 1 1 calc R . . H34C H 0.6967 0.9148 0.5237 0.082 Uiso 1 1 calc R . . C35 C 0.6899(4) 0.8605(4) 0.7563(3) 0.0311(11) Uani 1 1 d . . . C36 C 0.6150(4) 0.9058(4) 0.7860(4) 0.0360(12) Uani 1 1 d . . . C37 C 0.5363(4) 0.9014(4) 0.7265(4) 0.0462(14) Uani 1 1 d . . . H37 H 0.5283 0.8672 0.6664 0.055 Uiso 1 1 calc R . . C38 C 0.4691(5) 0.9464(5) 0.7540(5) 0.0544(16) Uani 1 1 d . . . H38 H 0.4168 0.9444 0.7127 0.065 Uiso 1 1 calc R . . C39 C 0.4778(4) 0.9948(4) 0.8421(5) 0.0490(15) Uani 1 1 d . . . C40 C 0.5562(5) 0.9973(4) 0.9009(4) 0.0449(14) Uani 1 1 d . . . H40 H 0.5628 1.0294 0.961 0.054 Uiso 1 1 calc R . . C41 C 0.6245(4) 0.9540(4) 0.8737(4) 0.0397(13) Uani 1 1 d . . . H41 H 0.6778 0.9572 0.915 0.048 Uiso 1 1 calc R . . C42 C 0.4080(6) 1.0468(5) 0.8739(6) 0.071(2) Uani 1 1 d . . . H42A H 0.4258 1.0759 0.9372 0.106 Uiso 0.5 1 calc PR . . H42B H 0.3373 1.0031 0.849 0.106 Uiso 0.5 1 calc PR . . H42C H 0.4153 1.0952 0.8563 0.106 Uiso 0.5 1 calc PR . . H42D H 0.3598 1.0403 0.8245 0.106 Uiso 0.5 1 calc PR . . H42E H 0.4483 1.113 0.9126 0.106 Uiso 0.5 1 calc PR . . H42F H 0.3703 1.0209 0.9054 0.106 Uiso 0.5 1 calc PR . . C43 C 0.8363(4) 1.0053(3) 0.8169(3) 0.0305(11) Uani 1 1 d . . . C44 C 0.9361(4) 1.0467(4) 0.8712(3) 0.0346(11) Uani 1 1 d . . . H44 H 0.9694 1.009 0.8822 0.042 Uiso 1 1 calc R . . C45 C 0.9872(5) 1.1428(4) 0.9093(4) 0.0411(13) Uani 1 1 d . . . H45 H 1.0553 1.1697 0.9453 0.049 Uiso 1 1 calc R . . C46 C 0.9406(5) 1.1990(4) 0.8957(4) 0.0437(14) Uani 1 1 d . . . H46 H 0.9759 1.2644 0.9222 0.052 Uiso 1 1 calc R . . C47 C 0.8410(5) 1.1592(4) 0.8427(4) 0.0437(14) Uani 1 1 d . . . H47 H 0.8078 1.1978 0.8335 0.052 Uiso 1 1 calc R . . C48 C 0.7897(4) 1.0629(4) 0.8030(4) 0.0390(12) Uani 1 1 d . . . H48 H 0.7221 1.0363 0.7659 0.047 Uiso 1 1 calc R . . C49 C 0.4632(6) 0.6591(6) 0.5731(6) 0.093(3) Uani 1 1 d . . . H49A H 0.4463 0.715 0.5849 0.139 Uiso 1 1 calc R . . H49B H 0.4005 0.6054 0.553 0.139 Uiso 1 1 calc R . . H49C H 0.4988 0.6473 0.5285 0.139 Uiso 1 1 calc R . . C50 C 0.4823(6) 0.7001(6) 0.7617(7) 0.086(3) Uani 1 1 d . . . H50A H 0.5279 0.7092 0.8138 0.129 Uiso 1 1 calc R . . H50B H 0.4195 0.6467 0.7425 0.129 Uiso 1 1 calc R . . H50C H 0.4658 0.7564 0.7747 0.129 Uiso 1 1 calc R . . C51 C 0.5777(6) 0.5701(4) 0.6502(5) 0.0639(19) Uani 1 1 d . . . H51A H 0.6213 0.5786 0.703 0.096 Uiso 1 1 calc R . . H51B H 0.6136 0.5587 0.6057 0.096 Uiso 1 1 calc R . . H51C H 0.5146 0.5165 0.6294 0.096 Uiso 1 1 calc R . . C52 C 1.4989(17) 1.3912(17) 0.8383(16) 0.195(8) Uiso 1 1 d . . . C53 C 1.5671(12) 1.3504(12) 0.7953(11) 0.147(5) Uiso 1 1 d . . . H53 H 1.5833 1.3612 0.7497 0.177 Uiso 1 1 calc R . . C54 C 1.6036(13) 1.3030(12) 0.8163(11) 0.151(5) Uiso 1 1 d . . . H54 H 1.6487 1.2808 0.7856 0.181 Uiso 1 1 calc R . . C55 C 1.5885(13) 1.2767(12) 0.8790(11) 0.159(6) Uiso 1 1 d . . . H55 H 1.6171 1.2376 0.8924 0.191 Uiso 1 1 calc R . . C56 C 1.5194(12) 1.3209(12) 0.9211(11) 0.151(5) Uiso 1 1 d . . . H56 H 1.5041 1.3122 0.968 0.181 Uiso 1 1 calc R . . C57 C 1.4802(13) 1.3685(12) 0.8993(12) 0.159(6) Uiso 1 1 d . . . H57 H 1.4336 1.3903 0.9282 0.19 Uiso 1 1 calc R . . C58 C 1.462(2) 1.445(2) 0.811(2) 0.296(14) Uiso 1 1 d . . . H58A H 1.49 1.4487 0.7648 0.445 Uiso 0.5 1 calc PR . . H58B H 1.4809 1.5078 0.8594 0.445 Uiso 0.5 1 calc PR . . H58C H 1.3871 1.4164 0.7885 0.445 Uiso 0.5 1 calc PR . . H58D H 1.4154 1.4665 0.8436 0.445 Uiso 0.5 1 calc PR . . H58E H 1.4244 1.4074 0.7491 0.445 Uiso 0.5 1 calc PR . . H58F H 1.5182 1.4988 0.82 0.445 Uiso 0.5 1 calc PR . . C59 C 1.2106(9) 0.4963(9) 0.8627(9) 0.113(4) Uiso 1 1 d . . . C60 C 1.2206(8) 0.4951(9) 0.9366(8) 0.105(3) Uiso 1 1 d . . . H60 H 1.2423 0.5526 0.9886 0.126 Uiso 1 1 calc R . . C61 C 1.2005(8) 0.4130(8) 0.9414(8) 0.100(3) Uiso 1 1 d . . . H61 H 1.2087 0.4146 0.996 0.12 Uiso 1 1 calc R . . C62 C 1.1692(9) 0.3305(9) 0.8678(8) 0.106(3) Uiso 1 1 d . . . H62 H 1.1555 0.2738 0.8705 0.127 Uiso 1 1 calc R . . C63 C 1.1574(10) 0.3287(10) 0.7909(9) 0.123(4) Uiso 1 1 d . . . H63 H 1.1343 0.2709 0.739 0.148 Uiso 1 1 calc R . . C64 C 1.1796(10) 0.4132(10) 0.7879(10) 0.130(4) Uiso 1 1 d . . . H64 H 1.1731 0.4126 0.7338 0.156 Uiso 1 1 calc R . . C65 C 1.231(2) 0.584(2) 0.8471(19) 0.267(12) Uiso 1 1 d . . . H65A H 1.2175 0.5627 0.785 0.401 Uiso 0.5 1 calc PR . . H65B H 1.3025 0.6251 0.8767 0.401 Uiso 0.5 1 calc PR . . H65C H 1.1865 0.6173 0.87 0.401 Uiso 0.5 1 calc PR . . H65D H 1.2535 0.6407 0.9028 0.401 Uiso 0.5 1 calc PR . . H65E H 1.1685 0.5783 0.8111 0.401 Uiso 0.5 1 calc PR . . H65F H 1.2845 0.5861 0.8178 0.401 Uiso 0.5 1 calc PR . . C66 C 0.7941(10) 1.2253(9) 0.5961(8) 0.056(3) Uiso 0.5 1 d PD . . C67 C 0.7579(7) 1.1674(7) 0.6295(6) 0.085(2) Uiso 1 1 d D . . C68 C 0.6559(10) 1.1233(12) 0.6115(11) 0.075(4) Uiso 0.5 1 d PD . . C69 C 0.5793(17) 1.1273(17) 0.5578(15) 0.222(9) Uiso 1 1 d D . . C70 C 0.6217(12) 1.1840(13) 0.5265(13) 0.085(5) Uiso 0.5 1 d PD . . C71 C 0.7191(8) 1.2333(9) 0.5368(8) 0.109(3) Uiso 1 1 d D . . C72 C 0.8877(13) 1.2611(12) 0.6165(11) 0.155(5) Uiso 1 1 d D . . C73 C 0.685(2) 1.176(3) 0.575(3) 0.219(18) Uiso 0.5 1 d PD . . C74 C 0.8222(11) 1.2667(15) 0.5555(13) 0.097(6) Uiso 0.5 1 d PD . . C75 C 0.8613(16) 1.208(4) 0.657(4) 0.32(3) Uiso 0.5 1 d PD . . 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 Zr 0.0341(3) 0.0261(3) 0.0298(3) 0.0123(2) 0.0112(2) 0.0135(2) Cl 0.0557(9) 0.0444(8) 0.0338(7) 0.0107(6) 0.0055(6) 0.0162(7) Si1 0.0439(9) 0.0286(7) 0.0406(8) 0.0126(6) 0.0215(7) 0.0170(7) Si2 0.0525(10) 0.0493(9) 0.0407(9) 0.0291(8) 0.0178(7) 0.0246(8) Si3 0.0352(9) 0.0390(9) 0.0758(13) 0.0199(9) 0.0129(9) 0.0074(7) N1 0.038(2) 0.028(2) 0.031(2) 0.0139(18) 0.0141(19) 0.0144(19) N2 0.039(2) 0.028(2) 0.033(2) 0.0141(18) 0.0143(19) 0.0163(19) N3 0.036(2) 0.028(2) 0.031(2) 0.0152(18) 0.0111(18) 0.0126(18) N4 0.039(2) 0.035(2) 0.035(2) 0.019(2) 0.013(2) 0.014(2) N5 0.032(2) 0.027(2) 0.034(2) 0.0128(18) 0.0116(18) 0.0143(18) N6 0.033(2) 0.031(2) 0.040(2) 0.012(2) 0.012(2) 0.0124(19) C1 0.032(3) 0.028(3) 0.038(3) 0.015(2) 0.012(2) 0.013(2) C2 0.042(3) 0.029(3) 0.034(3) 0.016(2) 0.016(2) 0.019(2) C3 0.043(3) 0.035(3) 0.038(3) 0.016(2) 0.011(2) 0.016(2) C4 0.054(4) 0.028(3) 0.051(3) 0.020(3) 0.021(3) 0.015(3) C5 0.068(4) 0.035(3) 0.046(3) 0.025(3) 0.023(3) 0.023(3) C6 0.065(4) 0.039(3) 0.043(3) 0.022(3) 0.006(3) 0.022(3) C7 0.053(3) 0.031(3) 0.041(3) 0.016(2) 0.012(3) 0.015(3) C8 0.099(6) 0.046(4) 0.066(5) 0.039(4) 0.020(4) 0.034(4) C9 0.039(3) 0.034(3) 0.032(3) 0.017(2) 0.014(2) 0.018(2) C10 0.056(4) 0.036(3) 0.049(3) 0.020(3) 0.026(3) 0.020(3) C11 0.061(4) 0.051(4) 0.059(4) 0.033(3) 0.038(3) 0.026(3) C12 0.069(4) 0.048(3) 0.028(3) 0.018(3) 0.027(3) 0.039(3) C13 0.052(3) 0.040(3) 0.035(3) 0.017(2) 0.017(3) 0.028(3) C14 0.045(3) 0.035(3) 0.034(3) 0.019(2) 0.015(2) 0.021(2) C15 0.056(4) 0.038(3) 0.049(3) 0.017(3) 0.030(3) 0.020(3) C16 0.058(4) 0.034(3) 0.051(4) 0.006(3) 0.021(3) 0.011(3) C17 0.053(4) 0.047(3) 0.063(4) 0.027(3) 0.030(3) 0.029(3) C18 0.038(3) 0.026(2) 0.032(3) 0.011(2) 0.015(2) 0.014(2) C19 0.038(3) 0.036(3) 0.037(3) 0.020(2) 0.012(2) 0.012(2) C20 0.049(3) 0.038(3) 0.036(3) 0.014(2) 0.015(3) 0.016(3) C21 0.045(3) 0.062(4) 0.045(3) 0.031(3) 0.021(3) 0.016(3) C22 0.039(3) 0.061(4) 0.046(3) 0.035(3) 0.010(3) 0.006(3) C23 0.052(4) 0.041(3) 0.041(3) 0.019(3) 0.006(3) 0.004(3) C24 0.046(3) 0.039(3) 0.032(3) 0.015(2) 0.012(2) 0.013(3) C25 0.045(4) 0.101(6) 0.067(5) 0.054(5) 0.014(3) 0.001(4) C26 0.038(3) 0.024(2) 0.037(3) 0.013(2) 0.008(2) 0.010(2) C27 0.044(3) 0.035(3) 0.034(3) 0.017(2) 0.011(2) 0.014(2) C28 0.048(3) 0.047(3) 0.040(3) 0.025(3) 0.005(3) 0.010(3) C29 0.042(3) 0.049(4) 0.061(4) 0.031(3) 0.002(3) 0.014(3) C30 0.043(3) 0.062(4) 0.063(4) 0.033(3) 0.014(3) 0.026(3) C31 0.042(3) 0.045(3) 0.042(3) 0.019(3) 0.013(3) 0.018(3) C32 0.070(5) 0.066(4) 0.046(4) 0.030(3) 0.024(3) 0.026(4) C33 0.072(5) 0.059(4) 0.073(5) 0.048(4) 0.022(4) 0.029(4) C34 0.060(4) 0.068(4) 0.050(4) 0.035(3) 0.014(3) 0.034(4) C35 0.035(3) 0.031(3) 0.031(3) 0.015(2) 0.009(2) 0.015(2) C36 0.031(3) 0.036(3) 0.040(3) 0.016(2) 0.011(2) 0.014(2) C37 0.040(3) 0.047(3) 0.048(3) 0.019(3) 0.008(3) 0.018(3) C38 0.038(3) 0.057(4) 0.067(4) 0.027(3) 0.006(3) 0.024(3) C39 0.037(3) 0.039(3) 0.071(4) 0.022(3) 0.021(3) 0.019(3) C40 0.048(3) 0.040(3) 0.050(3) 0.017(3) 0.023(3) 0.022(3) C41 0.038(3) 0.042(3) 0.043(3) 0.021(3) 0.013(2) 0.018(3) C42 0.052(4) 0.061(4) 0.103(6) 0.031(4) 0.032(4) 0.036(4) C43 0.037(3) 0.028(3) 0.032(3) 0.016(2) 0.014(2) 0.015(2) C44 0.042(3) 0.029(3) 0.034(3) 0.013(2) 0.013(2) 0.017(2) C45 0.043(3) 0.034(3) 0.039(3) 0.013(2) 0.009(2) 0.011(2) C46 0.053(4) 0.027(3) 0.047(3) 0.016(3) 0.016(3) 0.011(3) C47 0.054(4) 0.034(3) 0.052(3) 0.023(3) 0.016(3) 0.024(3) C48 0.045(3) 0.033(3) 0.041(3) 0.018(2) 0.010(3) 0.017(2) C49 0.054(5) 0.063(5) 0.103(7) 0.010(5) -0.025(5) 0.010(4) C50 0.066(5) 0.062(5) 0.140(8) 0.050(5) 0.060(6) 0.021(4) C51 0.056(4) 0.033(3) 0.084(5) 0.018(3) 0.019(4) 0.007(3) #----------------------------------------------------------------------------# # 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 Zr N4 2.219(4) . ? Zr N2 2.221(4) . ? Zr N6 2.227(4) . ? Zr N1 2.284(4) . ? Zr N5 2.303(4) . ? Zr N3 2.305(4) . ? Zr Cl 2.4641(15) . ? Zr C35 2.694(5) . ? Zr C1 2.695(5) . ? Zr C18 2.697(5) . ? Si1 N2 1.750(4) . ? Si1 C17 1.858(6) . ? Si1 C16 1.865(6) . ? Si1 C15 1.875(6) . ? Si2 N4 1.746(5) . ? Si2 C32 1.859(7) . ? Si2 C33 1.867(7) . ? Si2 C34 1.871(7) . ? Si3 N6 1.754(5) . ? Si3 C49 1.860(9) . ? Si3 C51 1.865(7) . ? Si3 C50 1.875(9) . ? N1 C1 1.336(6) . ? N1 C9 1.413(6) . ? N2 C1 1.340(7) . ? N3 C18 1.329(7) . ? N3 C26 1.425(7) . ? N4 C18 1.340(7) . ? N5 C35 1.331(7) . ? N5 C43 1.416(6) . ? N6 C35 1.330(7) . ? C1 C2 1.486(7) . ? C2 C7 1.385(8) . ? C2 C3 1.391(8) . ? C3 C4 1.388(8) . ? C4 C5 1.383(9) . ? C5 C6 1.395(9) . ? C5 C8 1.510(8) . ? C6 C7 1.391(8) . ? C9 C10 1.395(8) . ? C9 C14 1.395(7) . ? C10 C11 1.379(8) . ? C11 C12 1.374(8) . ? C12 C13 1.396(8) . ? C13 C14 1.390(7) . ? C18 C19 1.492(7) . ? C19 C20 1.390(8) . ? C19 C24 1.392(8) . ? C20 C21 1.380(8) . ? C21 C22 1.382(9) . ? C22 C23 1.395(9) . ? C22 C25 1.523(9) . ? C23 C24 1.378(8) . ? C26 C27 1.391(8) . ? C26 C31 1.395(8) . ? C27 C28 1.384(8) . ? C28 C29 1.382(9) . ? C29 C30 1.388(10) . ? C30 C31 1.380(8) . ? C35 C36 1.496(7) . ? C36 C37 1.388(8) . ? C36 C41 1.390(8) . ? C37 C38 1.388(9) . ? C38 C39 1.397(10) . ? C39 C40 1.393(9) . ? C39 C42 1.508(8) . ? C40 C41 1.384(8) . ? C43 C48 1.393(7) . ? C43 C44 1.398(7) . ? C44 C45 1.394(8) . ? C45 C46 1.368(8) . ? C46 C47 1.389(9) . ? C47 C48 1.396(8) . ? C52 C57 1.33(2) . ? C52 C58 1.38(3) . ? C52 C53 1.45(2) . ? C53 C54 1.209(19) . ? C54 C55 1.39(2) . ? C55 C56 1.49(2) . ? C56 C57 1.24(2) . ? C59 C60 1.312(15) . ? C59 C64 1.369(17) . ? C59 C65 1.57(3) . ? C60 C61 1.384(15) . ? C61 C62 1.354(15) . ? C62 C63 1.341(16) . ? C63 C64 1.405(17) . ? C66 C72 1.235(19) . ? C66 C74 1.24(2) . ? C66 C67 1.374(11) . ? C66 C73 1.46(3) . ? C66 C71 1.462(12) . ? C66 C75 1.50(3) . ? C67 C75 1.361(16) . ? C67 C68 1.365(12) . ? C67 C73 1.404(16) . ? C68 C73 1.33(2) . ? C68 C69 1.376(14) . ? C69 C70 1.355(14) . ? C69 C73 1.43(3) . ? C70 C73 1.22(2) . ? C70 C71 1.356(13) . ? C71 C74 1.358(13) . ? C71 C73 1.419(16) . ? C72 C75 1.370(16) . ? C72 C74 1.378(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zr N2 117.64(16) . . ? N4 Zr N6 122.13(17) . . ? N2 Zr N6 118.67(16) . . ? N4 Zr N1 141.57(16) . . ? N2 Zr N1 59.20(15) . . ? N6 Zr N1 81.23(16) . . ? N4 Zr N5 82.19(16) . . ? N2 Zr N5 144.66(15) . . ? N6 Zr N5 58.89(15) . . ? N1 Zr N5 86.79(15) . . ? N4 Zr N3 58.99(15) . . ? N2 Zr N3 81.09(15) . . ? N6 Zr N3 142.53(16) . . ? N1 Zr N3 83.72(15) . . ? N5 Zr N3 86.24(15) . . ? N4 Zr Cl 86.08(12) . . ? N2 Zr Cl 85.89(12) . . ? N6 Zr Cl 85.55(12) . . ? N1 Zr Cl 128.82(11) . . ? N5 Zr Cl 126.50(11) . . ? N3 Zr Cl 129.70(11) . . ? N4 Zr C35 101.57(16) . . ? N2 Zr C35 139.94(16) . . ? N6 Zr C35 29.46(16) . . ? N1 Zr C35 85.35(15) . . ? N5 Zr C35 29.59(15) . . ? N3 Zr C35 115.37(15) . . ? Cl Zr C35 105.66(12) . . ? N4 Zr C1 137.82(16) . . ? N2 Zr C1 29.68(15) . . ? N6 Zr C1 99.13(16) . . ? N1 Zr C1 29.68(15) . . ? N5 Zr C1 116.33(15) . . ? N3 Zr C1 83.51(15) . . ? Cl Zr C1 107.10(12) . . ? C35 Zr C1 112.34(15) . . ? N4 Zr C18 29.65(16) . . ? N2 Zr C18 98.34(16) . . ? N6 Zr C18 141.78(15) . . ? N1 Zr C18 113.13(16) . . ? N5 Zr C18 85.73(15) . . ? N3 Zr C18 29.52(15) . . ? Cl Zr C18 107.62(12) . . ? C35 Zr C18 113.51(15) . . ? C1 Zr C18 110.20(16) . . ? N2 Si1 C17 111.7(3) . . ? N2 Si1 C16 110.7(3) . . ? C17 Si1 C16 110.8(3) . . ? N2 Si1 C15 106.5(2) . . ? C17 Si1 C15 109.8(3) . . ? C16 Si1 C15 107.1(3) . . ? N4 Si2 C32 110.8(3) . . ? N4 Si2 C33 111.2(3) . . ? C32 Si2 C33 110.6(3) . . ? N4 Si2 C34 106.0(3) . . ? C32 Si2 C34 109.0(3) . . ? C33 Si2 C34 109.2(3) . . ? N6 Si3 C49 110.0(4) . . ? N6 Si3 C51 106.7(3) . . ? C49 Si3 C51 108.7(4) . . ? N6 Si3 C50 111.2(3) . . ? C49 Si3 C50 111.2(5) . . ? C51 Si3 C50 108.9(4) . . ? C1 N1 C9 124.9(4) . . ? C1 N1 Zr 92.5(3) . . ? C9 N1 Zr 138.2(3) . . ? C1 N2 Si1 130.9(4) . . ? C1 N2 Zr 95.2(3) . . ? Si1 N2 Zr 133.9(2) . . ? C18 N3 C26 125.1(4) . . ? C18 N3 Zr 91.8(3) . . ? C26 N3 Zr 138.0(3) . . ? C18 N4 Si2 131.2(4) . . ? C18 N4 Zr 95.3(3) . . ? Si2 N4 Zr 133.5(2) . . ? C35 N5 C43 125.5(4) . . ? C35 N5 Zr 91.7(3) . . ? C43 N5 Zr 139.3(3) . . ? C35 N6 Si3 131.1(4) . . ? C35 N6 Zr 95.1(3) . . ? Si3 N6 Zr 133.7(2) . . ? N1 C1 N2 112.6(4) . . ? N1 C1 C2 125.2(5) . . ? N2 C1 C2 122.1(4) . . ? N1 C1 Zr 57.9(3) . . ? N2 C1 Zr 55.2(3) . . ? C2 C1 Zr 174.2(4) . . ? C7 C2 C3 119.1(5) . . ? C7 C2 C1 120.2(5) . . ? C3 C2 C1 120.7(5) . . ? C4 C3 C2 120.2(5) . . ? C5 C4 C3 121.4(5) . . ? C4 C5 C6 118.1(5) . . ? C4 C5 C8 121.7(6) . . ? C6 C5 C8 120.2(6) . . ? C7 C6 C5 121.0(6) . . ? C2 C7 C6 120.2(5) . . ? C10 C9 C14 118.2(5) . . ? C10 C9 N1 124.0(5) . . ? C14 C9 N1 117.8(5) . . ? C11 C10 C9 120.5(5) . . ? C12 C11 C10 121.8(6) . . ? C11 C12 C13 118.2(5) . . ? C14 C13 C12 120.6(5) . . ? C13 C14 C9 120.6(5) . . ? N3 C18 N4 113.2(5) . . ? N3 C18 C19 124.6(5) . . ? N4 C18 C19 122.2(5) . . ? N3 C18 Zr 58.7(3) . . ? N4 C18 Zr 55.0(3) . . ? C19 C18 Zr 173.4(4) . . ? C20 C19 C24 118.5(5) . . ? C20 C19 C18 121.4(5) . . ? C24 C19 C18 120.1(5) . . ? C21 C20 C19 120.6(5) . . ? C20 C21 C22 121.3(6) . . ? C21 C22 C23 117.9(5) . . ? C21 C22 C25 122.5(6) . . ? C23 C22 C25 119.7(6) . . ? C24 C23 C22 121.3(6) . . ? C23 C24 C19 120.4(5) . . ? C27 C26 C31 118.3(5) . . ? C27 C26 N3 118.5(5) . . ? C31 C26 N3 123.0(5) . . ? C28 C27 C26 121.1(5) . . ? C29 C28 C27 120.4(6) . . ? C28 C29 C30 118.8(6) . . ? C31 C30 C29 121.2(6) . . ? C30 C31 C26 120.2(6) . . ? N6 C35 N5 113.6(4) . . ? N6 C35 C36 122.5(5) . . ? N5 C35 C36 123.8(5) . . ? N6 C35 Zr 55.4(3) . . ? N5 C35 Zr 58.7(2) . . ? C36 C35 Zr 174.3(4) . . ? C37 C36 C41 119.2(5) . . ? C37 C36 C35 120.6(5) . . ? C41 C36 C35 120.2(5) . . ? C38 C37 C36 120.7(6) . . ? C37 C38 C39 120.4(6) . . ? C40 C39 C38 118.2(5) . . ? C40 C39 C42 120.2(6) . . ? C38 C39 C42 121.6(6) . . ? C41 C40 C39 121.5(6) . . ? C40 C41 C36 119.9(5) . . ? C48 C43 C44 118.0(5) . . ? C48 C43 N5 123.6(5) . . ? C44 C43 N5 118.4(4) . . ? C45 C44 C43 120.6(5) . . ? C46 C45 C44 121.0(5) . . ? C45 C46 C47 119.3(5) . . ? C46 C47 C48 120.3(5) . . ? C43 C48 C47 120.8(5) . . ? C57 C52 C58 129(3) . . ? C57 C52 C53 113(2) . . ? C58 C52 C53 118(3) . . ? C54 C53 C52 122(2) . . ? C53 C54 C55 129(2) . . ? C54 C55 C56 107.2(17) . . ? C57 C56 C55 124.5(19) . . ? C56 C57 C52 125(2) . . ? C60 C59 C64 118.4(14) . . ? C60 C59 C65 128.1(16) . . ? C64 C59 C65 113.5(16) . . ? C59 C60 C61 122.4(12) . . ? C62 C61 C60 119.5(12) . . ? C63 C62 C61 120.0(13) . . ? C62 C63 C64 119.3(14) . . ? C59 C64 C63 120.4(14) . . ? C72 C66 C74 67.7(10) . . ? C72 C66 C67 115.4(12) . . ? C74 C66 C67 171.5(16) . . ? C72 C66 C73 174.4(14) . . ? C74 C66 C73 117.4(11) . . ? C67 C66 C73 59.3(8) . . ? C72 C66 C71 127.2(12) . . ? C74 C66 C71 59.7(7) . . ? C67 C66 C71 117.3(11) . . ? C73 C66 C71 58.1(7) . . ? C72 C66 C75 59.1(8) . . ? C74 C66 C75 126.5(13) . . ? C67 C66 C75 56.3(8) . . ? C73 C66 C75 115.6(11) . . ? C71 C66 C75 173.5(13) . . ? C75 C67 C68 172.1(17) . . ? C75 C67 C66 66.6(14) . . ? C68 C67 C66 121.1(11) . . ? C75 C67 C73 130.1(18) . . ? C68 C67 C73 57.6(12) . . ? C66 C67 C73 63.5(13) . . ? C73 C68 C67 62.7(10) . . ? C73 C68 C69 63.5(14) . . ? C67 C68 C69 126.2(16) . . ? C70 C69 C68 108.7(19) . . ? C70 C69 C73 51.9(13) . . ? C68 C69 C73 56.8(12) . . ? C73 C70 C69 67.0(16) . . ? C73 C70 C71 66.6(11) . . ? C69 C70 C71 133.7(18) . . ? C70 C71 C74 164.0(15) . . ? C70 C71 C73 52.0(12) . . ? C74 C71 C73 112.6(15) . . ? C70 C71 C66 113.0(12) . . ? C74 C71 C66 52.0(10) . . ? C73 C71 C66 61.0(13) . . ? C66 C72 C75 70.2(16) . . ? C66 C72 C74 56.3(12) . . ? C75 C72 C74 126(2) . . ? C70 C73 C68 121(2) . . ? C70 C73 C67 179(4) . . ? C68 C73 C67 59.7(8) . . ? C70 C73 C71 61.3(9) . . ? C68 C73 C71 178(2) . . ? C67 C73 C71 118.2(19) . . ? C70 C73 C69 61.0(12) . . ? C68 C73 C69 59.7(11) . . ? C67 C73 C69 119.4(15) . . ? C71 C73 C69 122.4(14) . . ? C70 C73 C66 122.3(15) . . ? C68 C73 C66 117.0(13) . . ? C67 C73 C66 57.2(10) . . ? C71 C73 C66 61.0(11) . . ? C69 C73 C66 176.6(15) . . ? C66 C74 C71 68.4(10) . . ? C66 C74 C72 56.0(12) . . ? C71 C74 C72 124.2(17) . . ? C67 C75 C72 108(2) . . ? C67 C75 C66 57.1(10) . . ? C72 C75 C66 50.7(13) . . ? #===END data_(7)-oct1499 _database_code_depnum_ccdc_archive 'CCDC 622823' _audit_creation_date 1999-10-14T15:10:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Na(tmeda)(Me3SiNC(C6H4-Me)NPh)}2]' _chemical_formula_moiety 'C46 H74 N8 Na2 Si2' _chemical_formula_sum 'C46 H74 N8 Na2 Si2' _chemical_formula_weight 841.29 _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 10.7511(3) _cell_length_b 10.9732(3) _cell_length_c 24.2691(6) _cell_angle_alpha 77.1925(15) _cell_angle_beta 88.8729(16) _cell_angle_gamma 63.9531(15) _cell_volume 2498.45(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20535 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.127 _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_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 24926 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.96 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 8603 _reflns_number_gt 6594 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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^)+(0.0360P)^2^+1.3378P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8603 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.181 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' Na Na 0.0362 0.0249 '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' 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 Si1 Si 0.78066(6) 0.06319(6) 0.09660(2) 0.03089(14) Uani 1 1 d . . . Si2 Si 0.67339(6) 0.43971(6) 0.39025(2) 0.03194(15) Uani 1 1 d . . . Na1 Na 0.61011(7) 0.32884(8) 0.19693(3) 0.03165(19) Uani 1 1 d . . . Na2 Na 0.84437(8) 0.15371(8) 0.29914(3) 0.03255(19) Uani 1 1 d . . . N1 N 0.77452(16) 0.16853(16) 0.14033(7) 0.0295(4) Uani 1 1 d . . . N2 N 0.86242(16) 0.25832(16) 0.19785(6) 0.0286(4) Uani 1 1 d . . . N3 N 0.67855(16) 0.32587(16) 0.35062(6) 0.0285(4) Uani 1 1 d . . . N4 N 0.59487(16) 0.21667(16) 0.30098(6) 0.0283(4) Uani 1 1 d . . . N5 N 0.48498(18) 0.60354(18) 0.18465(7) 0.0387(4) Uani 1 1 d . . . N6 N 0.39231(19) 0.45156(18) 0.12302(7) 0.0397(4) Uani 1 1 d . . . N7 N 0.95650(19) -0.10632(19) 0.29689(8) 0.0456(5) Uani 1 1 d . . . N8 N 1.03341(19) 0.0044(2) 0.38253(7) 0.0465(5) Uani 1 1 d . . . C1 C 0.86302(19) 0.21689(19) 0.15008(8) 0.0276(4) Uani 1 1 d . . . C2 C 0.9683(2) 0.2220(2) 0.10839(8) 0.0290(4) Uani 1 1 d . . . C3 C 0.9260(2) 0.3110(2) 0.05463(9) 0.0385(5) Uani 1 1 d . . . H3 H 0.8298 0.3687 0.0437 0.046 Uiso 1 1 calc R . . C4 C 1.0228(3) 0.3163(3) 0.01674(9) 0.0451(6) Uani 1 1 d . . . H4 H 0.9919 0.3793 -0.0195 0.054 Uiso 1 1 calc R . . C5 C 1.1635(2) 0.2315(2) 0.03080(9) 0.0423(5) Uani 1 1 d . . . C6 C 1.2052(2) 0.1406(2) 0.08406(10) 0.0409(5) Uani 1 1 d . . . H6 H 1.3011 0.0796 0.0942 0.049 Uiso 1 1 calc R . . C7 C 1.1096(2) 0.1371(2) 0.12275(9) 0.0351(5) Uani 1 1 d . . . H7 H 1.1409 0.0761 0.1594 0.042 Uiso 1 1 calc R . . C8 C 1.2691(3) 0.2395(3) -0.01045(11) 0.0623(8) Uani 1 1 d . . . H8A H 1.3629 0.1728 0.0068 0.093 Uiso 0.5 1 calc PR . . H8B H 1.2616 0.3342 -0.0195 0.093 Uiso 0.5 1 calc PR . . H8C H 1.251 0.2167 -0.0453 0.093 Uiso 0.5 1 calc PR . . H8D H 1.2208 0.3097 -0.0455 0.093 Uiso 0.5 1 calc PR . . H8E H 1.3221 0.1483 -0.0192 0.093 Uiso 0.5 1 calc PR . . H8F H 1.3327 0.2658 0.0067 0.093 Uiso 0.5 1 calc PR . . C9 C 0.6561(3) -0.0090(3) 0.12241(12) 0.0576(7) Uani 1 1 d . . . H9A H 0.6803 -0.0552 0.1628 0.086 Uiso 1 1 calc R . . H9B H 0.6613 -0.0768 0.101 0.086 Uiso 1 1 calc R . . H9C H 0.5615 0.0671 0.1169 0.086 Uiso 1 1 calc R . . C10 C 0.9559(2) -0.0858(2) 0.09786(11) 0.0484(6) Uani 1 1 d . . . H10A H 0.9918 -0.1361 0.1372 0.073 Uiso 1 1 calc R . . H10B H 1.0196 -0.0499 0.0801 0.073 Uiso 1 1 calc R . . H10C H 0.9482 -0.1493 0.077 0.073 Uiso 1 1 calc R . . C11 C 0.7255(3) 0.1486(3) 0.01955(10) 0.0572(7) Uani 1 1 d . . . H11A H 0.7877 0.1885 0.0037 0.086 Uiso 1 1 calc R . . H11B H 0.6301 0.2229 0.0153 0.086 Uiso 1 1 calc R . . H11C H 0.7298 0.079 -0.0007 0.086 Uiso 1 1 calc R . . C12 C 0.9382(2) 0.3315(2) 0.20557(8) 0.0318(4) Uani 1 1 d . . . C13 C 1.0368(2) 0.2779(3) 0.25226(9) 0.0439(5) Uani 1 1 d . . . H13 H 1.0602 0.187 0.2749 0.053 Uiso 1 1 calc R . . C14 C 1.1010(3) 0.3524(3) 0.26649(11) 0.0537(7) Uani 1 1 d . . . H14 H 1.1677 0.3128 0.2984 0.064 Uiso 1 1 calc R . . C15 C 1.0688(3) 0.4828(3) 0.23470(13) 0.0593(7) Uani 1 1 d . . . H15 H 1.1106 0.5358 0.2452 0.071 Uiso 1 1 calc R . . C16 C 0.9752(3) 0.5383(3) 0.18712(13) 0.0604(7) Uani 1 1 d . . . H16 H 0.955 0.6282 0.1643 0.072 Uiso 1 1 calc R . . C17 C 0.9101(2) 0.4629(2) 0.17238(10) 0.0450(6) Uani 1 1 d . . . H17 H 0.8464 0.5017 0.1395 0.054 Uiso 1 1 calc R . . C18 C 0.59246(19) 0.27184(19) 0.34550(8) 0.0266(4) Uani 1 1 d . . . C19 C 0.4857(2) 0.27843(19) 0.38786(8) 0.0283(4) Uani 1 1 d . . . C20 C 0.5259(2) 0.2093(2) 0.44467(8) 0.0380(5) Uani 1 1 d . . . H20 H 0.622 0.1576 0.4573 0.046 Uiso 1 1 calc R . . C21 C 0.4272(3) 0.2151(3) 0.48315(9) 0.0462(6) Uani 1 1 d . . . H21 H 0.4568 0.1652 0.5216 0.055 Uiso 1 1 calc R . . C22 C 0.2865(3) 0.2924(3) 0.46652(10) 0.0447(6) Uani 1 1 d . . . C23 C 0.2469(2) 0.3634(2) 0.41008(10) 0.0424(5) Uani 1 1 d . . . H23 H 0.151 0.4189 0.3979 0.051 Uiso 1 1 calc R . . C24 C 0.3447(2) 0.3549(2) 0.37118(9) 0.0334(5) Uani 1 1 d . . . H24 H 0.3147 0.4022 0.3325 0.04 Uiso 1 1 calc R . . C25 C 0.1800(3) 0.2990(3) 0.50886(12) 0.0682(8) Uani 1 1 d . . . H25A H 0.0864 0.3579 0.4897 0.102 Uiso 0.5 1 calc PR . . H25B H 0.1944 0.3387 0.5392 0.102 Uiso 0.5 1 calc PR . . H25C H 0.1901 0.2047 0.5252 0.102 Uiso 0.5 1 calc PR . . H25D H 0.2276 0.2429 0.5463 0.102 Uiso 0.5 1 calc PR . . H25E H 0.1196 0.2622 0.4968 0.102 Uiso 0.5 1 calc PR . . H25F H 0.1238 0.3962 0.5109 0.102 Uiso 0.5 1 calc PR . . C26 C 0.4947(2) 0.5680(2) 0.40123(10) 0.0460(6) Uani 1 1 d . . . H26A H 0.4455 0.5176 0.4219 0.069 Uiso 1 1 calc R . . H26B H 0.4433 0.6235 0.3643 0.069 Uiso 1 1 calc R . . H26C H 0.5018 0.63 0.4232 0.069 Uiso 1 1 calc R . . C27 C 0.7665(3) 0.3539(3) 0.46309(10) 0.0526(6) Uani 1 1 d . . . H27A H 0.7216 0.3007 0.4852 0.079 Uiso 1 1 calc R . . H27B H 0.7628 0.4255 0.482 0.079 Uiso 1 1 calc R . . H27C H 0.8636 0.2908 0.4601 0.079 Uiso 1 1 calc R . . C28 C 0.7652(3) 0.5381(3) 0.35129(11) 0.0535(6) Uani 1 1 d . . . H28A H 0.7201 0.5847 0.3127 0.08 Uiso 1 1 calc R . . H28B H 0.8624 0.4732 0.3495 0.08 Uiso 1 1 calc R . . H28C H 0.7613 0.6081 0.3712 0.08 Uiso 1 1 calc R . . C29 C 0.5315(2) 0.1280(2) 0.30155(8) 0.0299(4) Uani 1 1 d . . . C30 C 0.5454(2) 0.0188(2) 0.34744(9) 0.0382(5) Uani 1 1 d . . . H30 H 0.5919 0.0078 0.3824 0.046 Uiso 1 1 calc R . . C31 C 0.4931(3) -0.0732(2) 0.34302(10) 0.0481(6) Uani 1 1 d . . . H31 H 0.5042 -0.1464 0.3749 0.058 Uiso 1 1 calc R . . C32 C 0.4250(3) -0.0610(3) 0.29315(11) 0.0500(6) Uani 1 1 d . . . H32 H 0.389 -0.1247 0.2904 0.06 Uiso 1 1 calc R . . C33 C 0.4100(3) 0.0456(3) 0.24729(10) 0.0511(6) Uani 1 1 d . . . H33 H 0.3634 0.0555 0.2125 0.061 Uiso 1 1 calc R . . C34 C 0.4624(2) 0.1382(2) 0.25159(9) 0.0417(5) Uani 1 1 d . . . H34 H 0.4509 0.211 0.2194 0.05 Uiso 1 1 calc R . . C35 C 0.3718(2) 0.6760(2) 0.13904(9) 0.0415(5) Uani 1 1 d . . . H35A H 0.4101 0.7015 0.1033 0.05 Uiso 1 1 calc R . . H35B H 0.3031 0.7637 0.1479 0.05 Uiso 1 1 calc R . . C36 C 0.2987(2) 0.5921(2) 0.12995(9) 0.0394(5) Uani 1 1 d . . . H36A H 0.2444 0.5832 0.1627 0.047 Uiso 1 1 calc R . . H36B H 0.2323 0.6436 0.0957 0.047 Uiso 1 1 calc R . . C37 C 0.4298(3) 0.5880(3) 0.23982(9) 0.0490(6) Uani 1 1 d . . . H37A H 0.3784 0.5326 0.2411 0.073 Uiso 1 1 calc R . . H37B H 0.3673 0.6803 0.2456 0.073 Uiso 1 1 calc R . . H37C H 0.5067 0.5404 0.2698 0.073 Uiso 1 1 calc R . . C38 C 0.5631(3) 0.6849(3) 0.18358(13) 0.0639(7) Uani 1 1 d . . . H38A H 0.6014 0.6951 0.1468 0.096 Uiso 1 1 calc R . . H38B H 0.6392 0.6365 0.2139 0.096 Uiso 1 1 calc R . . H38C H 0.501 0.7774 0.1893 0.096 Uiso 1 1 calc R . . C39 C 0.3088(3) 0.3797(3) 0.11597(12) 0.0591(7) Uani 1 1 d . . . H39A H 0.37 0.2859 0.1113 0.089 Uiso 1 1 calc R . . H39B H 0.2426 0.4325 0.0823 0.089 Uiso 1 1 calc R . . H39C H 0.258 0.3728 0.1496 0.089 Uiso 1 1 calc R . . C40 C 0.4684(3) 0.4608(3) 0.07292(10) 0.0643(8) Uani 1 1 d . . . H40A H 0.5307 0.3665 0.0689 0.096 Uiso 1 1 calc R . . H40B H 0.5232 0.5103 0.0771 0.096 Uiso 1 1 calc R . . H40C H 0.4024 0.5116 0.0391 0.096 Uiso 1 1 calc R . . C41 C 1.0411(3) -0.1970(3) 0.34945(11) 0.0644(8) Uani 1 1 d . . . H41A H 1.1071 -0.2876 0.342 0.077 Uiso 1 1 calc R . . H41B H 0.9798 -0.2151 0.3777 0.077 Uiso 1 1 calc R . . C42 C 1.1214(3) -0.1358(3) 0.37407(11) 0.0655(8) Uani 1 1 d . . . H42A H 1.1703 -0.1986 0.411 0.079 Uiso 1 1 calc R . . H42B H 1.1927 -0.131 0.3484 0.079 Uiso 1 1 calc R . . C43 C 0.8564(3) -0.1524(3) 0.28054(17) 0.0856(11) Uani 1 1 d . . . H43A H 0.7954 -0.1536 0.311 0.128 Uiso 1 1 calc R . . H43B H 0.9065 -0.2464 0.2741 0.128 Uiso 1 1 calc R . . H43C H 0.8004 -0.0878 0.2457 0.128 Uiso 1 1 calc R . . C44 C 1.0451(3) -0.1054(3) 0.25087(10) 0.0507(6) Uani 1 1 d . . . H44A H 1.113 -0.075 0.2609 0.076 Uiso 1 1 calc R . . H44B H 0.9879 -0.0409 0.2162 0.076 Uiso 1 1 calc R . . H44C H 1.094 -0.1996 0.2445 0.076 Uiso 1 1 calc R . . C45 C 0.9336(3) 0.0002(3) 0.42401(10) 0.0507(6) Uani 1 1 d . . . H45A H 0.8756 0.0947 0.4289 0.076 Uiso 1 1 calc R . . H45B H 0.9839 -0.0606 0.4605 0.076 Uiso 1 1 calc R . . H45C H 0.8745 -0.0362 0.4105 0.076 Uiso 1 1 calc R . . C46 C 1.1200(3) 0.0615(4) 0.40200(12) 0.0704(8) Uani 1 1 d . . . H46A H 1.0607 0.1548 0.4077 0.106 Uiso 1 1 calc R . . H46B H 1.1841 0.0676 0.3735 0.106 Uiso 1 1 calc R . . H46C H 1.1733 0.0002 0.4379 0.106 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 Si1 0.0315(3) 0.0297(3) 0.0327(3) -0.0114(2) 0.0038(2) -0.0130(2) Si2 0.0344(3) 0.0305(3) 0.0334(3) -0.0094(2) 0.0027(2) -0.0158(3) Na1 0.0273(4) 0.0323(4) 0.0318(4) -0.0052(3) 0.0033(3) -0.0113(3) Na2 0.0285(4) 0.0334(4) 0.0299(4) -0.0045(3) 0.0029(3) -0.0100(3) N1 0.0287(9) 0.0294(9) 0.0318(9) -0.0095(7) 0.0036(7) -0.0133(7) N2 0.0279(8) 0.0321(9) 0.0284(8) -0.0089(7) 0.0040(7) -0.0148(7) N3 0.0285(8) 0.0292(9) 0.0290(8) -0.0076(7) 0.0026(7) -0.0136(7) N4 0.0301(9) 0.0295(8) 0.0272(8) -0.0075(7) 0.0041(7) -0.0148(7) N5 0.0358(10) 0.0371(10) 0.0403(10) -0.0077(8) 0.0026(8) -0.0145(8) N6 0.0411(10) 0.0333(10) 0.0336(9) -0.0083(8) 0.0000(8) -0.0065(8) N7 0.0423(11) 0.0345(10) 0.0545(12) -0.0125(9) 0.0104(9) -0.0116(9) N8 0.0387(10) 0.0519(12) 0.0340(10) -0.0073(9) 0.0008(8) -0.0083(9) C1 0.0260(10) 0.0234(9) 0.0278(10) -0.0040(8) 0.0011(8) -0.0069(8) C2 0.0322(10) 0.0301(10) 0.0294(10) -0.0112(8) 0.0054(8) -0.0162(9) C3 0.0408(12) 0.0404(12) 0.0330(11) -0.0044(9) 0.0048(9) -0.0190(10) C4 0.0588(15) 0.0534(14) 0.0319(11) -0.0087(10) 0.0106(10) -0.0337(13) C5 0.0536(14) 0.0562(14) 0.0400(12) -0.0263(11) 0.0209(11) -0.0385(12) C6 0.0337(12) 0.0480(13) 0.0500(14) -0.0226(11) 0.0133(10) -0.0215(10) C7 0.0331(11) 0.0377(11) 0.0360(11) -0.0099(9) 0.0054(9) -0.0167(10) C8 0.0740(18) 0.093(2) 0.0564(16) -0.0397(15) 0.0375(14) -0.0603(17) C9 0.0623(16) 0.0728(18) 0.0684(17) -0.0403(14) 0.0236(13) -0.0472(15) C10 0.0404(13) 0.0402(13) 0.0623(15) -0.0261(11) 0.0038(11) -0.0096(11) C11 0.0807(19) 0.0432(14) 0.0399(13) -0.0128(11) -0.0069(12) -0.0190(13) C12 0.0293(10) 0.0369(11) 0.0350(11) -0.0161(9) 0.0117(8) -0.0169(9) C13 0.0424(13) 0.0599(15) 0.0400(12) -0.0145(11) 0.0054(10) -0.0311(12) C14 0.0515(15) 0.081(2) 0.0509(15) -0.0296(14) 0.0117(12) -0.0430(15) C15 0.0529(16) 0.078(2) 0.0783(19) -0.0503(17) 0.0243(14) -0.0425(15) C16 0.0603(17) 0.0411(14) 0.090(2) -0.0216(14) 0.0231(16) -0.0291(13) C17 0.0452(13) 0.0381(12) 0.0555(14) -0.0129(11) 0.0067(11) -0.0212(11) C18 0.0255(10) 0.0223(9) 0.0254(9) -0.0009(7) 0.0003(7) -0.0070(8) C19 0.0330(11) 0.0261(10) 0.0296(10) -0.0089(8) 0.0055(8) -0.0155(9) C20 0.0402(12) 0.0449(12) 0.0308(11) -0.0053(9) 0.0034(9) -0.0223(10) C21 0.0612(16) 0.0596(15) 0.0292(11) -0.0087(10) 0.0103(10) -0.0381(13) C22 0.0533(14) 0.0592(15) 0.0419(13) -0.0242(11) 0.0224(11) -0.0382(13) C23 0.0329(12) 0.0484(13) 0.0539(14) -0.0196(11) 0.0119(10) -0.0220(10) C24 0.0339(11) 0.0382(11) 0.0322(11) -0.0094(9) 0.0048(9) -0.0191(10) C25 0.0722(19) 0.099(2) 0.0627(17) -0.0370(16) 0.0385(15) -0.0571(18) C26 0.0487(14) 0.0367(12) 0.0549(14) -0.0193(11) 0.0102(11) -0.0172(11) C27 0.0649(16) 0.0475(14) 0.0463(14) -0.0126(11) -0.0105(12) -0.0246(13) C28 0.0640(16) 0.0567(15) 0.0611(16) -0.0240(13) 0.0156(13) -0.0414(14) C29 0.0281(10) 0.0317(10) 0.0323(10) -0.0119(8) 0.0084(8) -0.0138(9) C30 0.0477(13) 0.0334(11) 0.0353(11) -0.0081(9) 0.0036(9) -0.0199(10) C31 0.0676(16) 0.0413(13) 0.0468(14) -0.0132(11) 0.0148(12) -0.0336(12) C32 0.0600(15) 0.0565(15) 0.0592(15) -0.0306(13) 0.0230(12) -0.0416(13) C33 0.0551(15) 0.0721(17) 0.0462(14) -0.0240(13) 0.0075(11) -0.0418(14) C34 0.0462(13) 0.0530(14) 0.0350(12) -0.0090(10) 0.0023(10) -0.0309(12) C35 0.0428(13) 0.0333(11) 0.0362(12) -0.0009(9) 0.0008(10) -0.0094(10) C36 0.0331(11) 0.0354(11) 0.0369(12) -0.0074(9) -0.0028(9) -0.0041(9) C37 0.0556(15) 0.0443(13) 0.0373(12) -0.0078(10) 0.0000(11) -0.0144(12) C38 0.0573(17) 0.0665(18) 0.082(2) -0.0249(15) 0.0109(14) -0.0370(15) C39 0.0649(17) 0.0441(14) 0.0598(16) -0.0144(12) -0.0192(13) -0.0148(13) C40 0.0681(18) 0.0528(16) 0.0366(13) -0.0071(11) 0.0126(12) 0.0028(14) C41 0.083(2) 0.0331(13) 0.0477(15) -0.0015(11) 0.0210(14) -0.0039(13) C42 0.0559(16) 0.0596(17) 0.0352(13) -0.0050(12) -0.0059(11) 0.0125(14) C43 0.0658(19) 0.071(2) 0.146(3) -0.067(2) 0.038(2) -0.0358(17) C44 0.0561(15) 0.0432(13) 0.0396(13) -0.0074(10) 0.0039(11) -0.0116(12) C45 0.0526(14) 0.0479(14) 0.0366(12) -0.0053(10) 0.0056(11) -0.0115(12) C46 0.0523(16) 0.109(2) 0.0487(16) -0.0183(16) -0.0020(13) -0.0345(17) #----------------------------------------------------------------------------# # 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 Si1 N1 1.7150(17) . ? Si1 C9 1.869(2) . ? Si1 C10 1.870(2) . ? Si1 C11 1.872(2) . ? Si2 N3 1.7199(17) . ? Si2 C28 1.866(2) . ? Si2 C26 1.875(2) . ? Si2 C27 1.875(2) . ? Na1 N2 2.4717(17) . ? Na1 N1 2.5201(17) . ? Na1 N4 2.5887(16) . ? Na1 N6 2.6151(19) . ? Na1 N5 2.6535(19) . ? Na2 N4 2.4609(17) . ? Na2 N3 2.5118(17) . ? Na2 N2 2.5147(17) . ? Na2 N7 2.578(2) . ? Na2 N8 2.5841(19) . ? N1 C1 1.323(2) . ? N2 C1 1.335(2) . ? N2 C12 1.411(2) . ? N3 C18 1.320(2) . ? N4 C18 1.345(2) . ? N4 C29 1.409(2) . ? N5 C37 1.460(3) . ? N5 C35 1.466(3) . ? N5 C38 1.467(3) . ? N6 C40 1.462(3) . ? N6 C39 1.464(3) . ? N6 C36 1.472(3) . ? N7 C44 1.455(3) . ? N7 C41 1.460(3) . ? N7 C43 1.468(4) . ? N8 C46 1.464(3) . ? N8 C45 1.466(3) . ? N8 C42 1.469(3) . ? C1 C2 1.514(3) . ? C2 C3 1.389(3) . ? C2 C7 1.390(3) . ? C3 C4 1.387(3) . ? C4 C5 1.384(3) . ? C5 C6 1.387(3) . ? C5 C8 1.517(3) . ? C6 C7 1.386(3) . ? C12 C17 1.390(3) . ? C12 C13 1.399(3) . ? C13 C14 1.376(3) . ? C14 C15 1.360(4) . ? C15 C16 1.383(4) . ? C16 C17 1.397(3) . ? C18 C19 1.514(3) . ? C19 C24 1.387(3) . ? C19 C20 1.391(3) . ? C20 C21 1.389(3) . ? C21 C22 1.384(3) . ? C22 C23 1.387(3) . ? C22 C25 1.512(3) . ? C23 C24 1.385(3) . ? C29 C34 1.392(3) . ? C29 C30 1.399(3) . ? C30 C31 1.377(3) . ? C31 C32 1.377(3) . ? C32 C33 1.377(3) . ? C33 C34 1.384(3) . ? C35 C36 1.499(3) . ? C41 C42 1.504(4) . ? 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 N1 Si1 C9 105.83(10) . . ? N1 Si1 C10 114.20(10) . . ? C9 Si1 C10 108.57(12) . . ? N1 Si1 C11 117.03(10) . . ? C9 Si1 C11 105.99(13) . . ? C10 Si1 C11 104.76(12) . . ? N3 Si2 C28 106.06(10) . . ? N3 Si2 C26 115.15(10) . . ? C28 Si2 C26 108.67(12) . . ? N3 Si2 C27 114.68(10) . . ? C28 Si2 C27 106.56(12) . . ? C26 Si2 C27 105.33(12) . . ? N2 Na1 N1 54.87(5) . . ? N2 Na1 N4 100.36(6) . . ? N1 Na1 N4 116.78(6) . . ? N2 Na1 N6 138.18(6) . . ? N1 Na1 N6 97.85(6) . . ? N4 Na1 N6 121.15(6) . . ? N2 Na1 N5 106.76(6) . . ? N1 Na1 N5 134.27(6) . . ? N4 Na1 N5 107.19(6) . . ? N6 Na1 N5 67.79(6) . . ? N4 Na2 N3 55.29(5) . . ? N4 Na2 N2 102.75(6) . . ? N3 Na2 N2 114.38(6) . . ? N4 Na2 N7 103.80(6) . . ? N3 Na2 N7 142.78(6) . . ? N2 Na2 N7 99.41(6) . . ? N4 Na2 N8 126.23(6) . . ? N3 Na2 N8 97.51(6) . . ? N2 Na2 N8 130.95(6) . . ? N7 Na2 N8 69.01(7) . . ? C1 N1 Si1 130.52(14) . . ? C1 N1 Na1 87.06(11) . . ? Si1 N1 Na1 141.60(9) . . ? C1 N2 C12 121.41(16) . . ? C1 N2 Na1 88.86(11) . . ? C12 N2 Na1 130.26(12) . . ? C1 N2 Na2 131.90(13) . . ? C12 N2 Na2 100.88(11) . . ? Na1 N2 Na2 79.05(5) . . ? C18 N3 Si2 130.68(14) . . ? C18 N3 Na2 87.17(11) . . ? Si2 N3 Na2 140.85(9) . . ? C18 N4 C29 120.84(15) . . ? C18 N4 Na2 88.78(11) . . ? C29 N4 Na2 126.97(12) . . ? C18 N4 Na1 125.00(12) . . ? C29 N4 Na1 109.20(11) . . ? Na2 N4 Na1 77.83(5) . . ? C37 N5 C35 110.61(17) . . ? C37 N5 C38 108.9(2) . . ? C35 N5 C38 109.22(19) . . ? C37 N5 Na1 91.08(12) . . ? C35 N5 Na1 113.13(13) . . ? C38 N5 Na1 122.18(15) . . ? C40 N6 C39 109.1(2) . . ? C40 N6 C36 110.34(18) . . ? C39 N6 C36 108.63(18) . . ? C40 N6 Na1 96.08(14) . . ? C39 N6 Na1 120.26(13) . . ? C36 N6 Na1 111.59(13) . . ? C44 N7 C41 110.02(19) . . ? C44 N7 C43 108.1(2) . . ? C41 N7 C43 112.0(2) . . ? C44 N7 Na2 100.32(13) . . ? C41 N7 Na2 112.39(15) . . ? C43 N7 Na2 113.28(16) . . ? C46 N8 C45 109.7(2) . . ? C46 N8 C42 109.9(2) . . ? C45 N8 C42 110.8(2) . . ? C46 N8 Na2 119.77(16) . . ? C45 N8 Na2 94.15(13) . . ? C42 N8 Na2 111.45(14) . . ? N1 C1 N2 119.87(17) . . ? N1 C1 C2 120.75(17) . . ? N2 C1 C2 119.35(17) . . ? C3 C2 C7 118.26(18) . . ? C3 C2 C1 120.88(17) . . ? C7 C2 C1 120.85(17) . . ? C4 C3 C2 120.7(2) . . ? C5 C4 C3 121.2(2) . . ? C4 C5 C6 117.99(19) . . ? C4 C5 C8 120.9(2) . . ? C6 C5 C8 121.1(2) . . ? C7 C6 C5 121.2(2) . . ? C6 C7 C2 120.6(2) . . ? C17 C12 C13 117.2(2) . . ? C17 C12 N2 123.18(19) . . ? C13 C12 N2 119.30(18) . . ? C14 C13 C12 122.3(2) . . ? C15 C14 C13 119.8(2) . . ? C14 C15 C16 119.9(2) . . ? C15 C16 C17 120.4(2) . . ? C12 C17 C16 120.3(2) . . ? N3 C18 N4 119.95(16) . . ? N3 C18 C19 120.30(17) . . ? N4 C18 C19 119.67(17) . . ? C24 C19 C20 118.03(18) . . ? C24 C19 C18 120.86(17) . . ? C20 C19 C18 121.11(17) . . ? C21 C20 C19 120.7(2) . . ? C22 C21 C20 121.2(2) . . ? C21 C22 C23 117.89(19) . . ? C21 C22 C25 120.7(2) . . ? C23 C22 C25 121.4(2) . . ? C24 C23 C22 121.2(2) . . ? C23 C24 C19 120.93(19) . . ? C34 C29 C30 116.44(19) . . ? C34 C29 N4 118.71(17) . . ? C30 C29 N4 124.48(18) . . ? C31 C30 C29 121.4(2) . . ? C30 C31 C32 121.1(2) . . ? C31 C32 C33 118.7(2) . . ? C32 C33 C34 120.3(2) . . ? C33 C34 C29 122.0(2) . . ? N5 C35 C36 114.02(17) . . ? N6 C36 C35 114.06(18) . . ? N7 C41 C42 113.1(2) . . ? N8 C42 C41 113.2(2) . . ? #===END data_(11)-jun1900 _database_code_depnum_ccdc_archive 'CCDC 622824' _audit_creation_date 2000-06-16T10:43:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[PhNC(NH2)(C6H4Me)]' _chemical_formula_moiety 'C14 H14 N2' _chemical_formula_sum 'C14 H14 N2' _chemical_formula_weight 210.27 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6672(5) _cell_length_b 17.708(2) _cell_length_c 10.1078(9) _cell_angle_alpha 90 _cell_angle_beta 102.654(6) _cell_angle_gamma 90 _cell_volume 1164.38(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12074 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.072 _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_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 6024 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_unetI/netI 0.069 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 25.19 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.953 _diffrn_measured_fraction_theta_max 0.953 _reflns_number_total 1981 _reflns_number_gt 1487 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 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 ; All hydrogen atoms were freely refined. 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^)+(0.0783P)^2^+0.2960P] 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 refall _refine_ls_extinction_method none _refine_ls_number_reflns 1981 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.208 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # 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' 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 N1 N 0.4563(3) 0.28788(10) 0.08888(16) 0.0322(5) Uani 1 1 d . . . N2 N 0.4996(3) 0.27043(12) 0.32252(18) 0.0403(5) Uani 1 1 d . . . H2B H 0.615(4) 0.3010(15) 0.339(2) 0.046(7) Uiso 1 1 d . . . H2A H 0.467(3) 0.2503(13) 0.395(2) 0.038(6) Uiso 1 1 d . . . C1 C 0.4070(3) 0.25573(12) 0.19264(19) 0.0299(5) Uani 1 1 d . . . C2 C 0.2331(3) 0.20088(12) 0.16862(19) 0.0302(5) Uani 1 1 d . . . C3 C 0.1728(3) 0.16520(13) 0.0431(2) 0.0342(5) Uani 1 1 d . . . H3 H 0.257(3) 0.1732(13) -0.027(2) 0.035(5) Uiso 1 1 d . . . C4 C 0.0011(3) 0.11915(13) 0.0155(2) 0.0369(6) Uani 1 1 d . . . H4 H -0.045(3) 0.0954(14) -0.075(2) 0.049(7) Uiso 1 1 d . . . C5 C -0.1180(3) 0.10769(12) 0.1105(2) 0.0362(6) Uani 1 1 d . . . C6 C -0.0567(3) 0.14264(13) 0.2360(2) 0.0380(6) Uani 1 1 d . . . H6 H -0.144(4) 0.1369(14) 0.308(2) 0.048(6) Uiso 1 1 d . . . C7 C 0.1170(3) 0.18780(13) 0.2655(2) 0.0355(6) Uani 1 1 d . . . H7 H 0.164(3) 0.2110(13) 0.360(2) 0.040(6) Uiso 1 1 d . . . C8 C -0.3069(4) 0.05852(17) 0.0793(3) 0.0491(7) Uani 1 1 d . . . H8C H -0.265(6) 0.002(3) 0.095(4) 0.118(14) Uiso 1 1 d . . . H8B H -0.403(6) 0.065(2) 0.132(4) 0.097(12) Uiso 1 1 d . . . H8A H -0.384(6) 0.063(2) -0.012(4) 0.112(13) Uiso 1 1 d . . . C9 C 0.6128(3) 0.34409(12) 0.11258(18) 0.0313(5) Uani 1 1 d . . . C10 C 0.8055(3) 0.32829(14) 0.0887(2) 0.0373(6) Uani 1 1 d . . . H10 H 0.827(4) 0.2776(15) 0.061(3) 0.058(8) Uiso 1 1 d . . . C11 C 0.9540(4) 0.38411(15) 0.1018(2) 0.0431(6) Uani 1 1 d . . . H11 H 1.092(4) 0.3707(16) 0.082(3) 0.061(8) Uiso 1 1 d . . . C12 C 0.9119(4) 0.45703(14) 0.1380(2) 0.0427(6) Uani 1 1 d . . . H12 H 1.022(4) 0.4959(15) 0.142(2) 0.052(7) Uiso 1 1 d . . . C13 C 0.7202(4) 0.47297(15) 0.1624(2) 0.0451(6) Uani 1 1 d . . . H13 H 0.682(4) 0.5243(16) 0.183(2) 0.052(7) Uiso 1 1 d . . . C14 C 0.5715(4) 0.41735(14) 0.1497(2) 0.0417(6) Uani 1 1 d . . . H14 H 0.427(4) 0.4298(15) 0.164(3) 0.058(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0333(10) 0.0375(11) 0.0263(9) -0.0018(7) 0.0072(7) -0.0055(8) N2 0.0395(12) 0.0555(14) 0.0248(10) 0.0029(9) 0.0048(8) -0.0145(10) C1 0.0289(11) 0.0341(12) 0.0263(11) -0.0017(8) 0.0056(8) 0.0014(9) C2 0.0298(11) 0.0321(11) 0.0279(11) 0.0017(8) 0.0045(8) 0.0004(9) C3 0.0337(12) 0.0403(12) 0.0290(11) -0.0008(9) 0.0076(9) -0.0005(10) C4 0.0368(13) 0.0372(13) 0.0349(12) -0.0054(10) 0.0036(9) -0.0021(10) C5 0.0347(12) 0.0326(12) 0.0402(13) 0.0017(9) 0.0056(9) -0.0011(10) C6 0.0371(13) 0.0389(13) 0.0399(12) 0.0012(10) 0.0127(10) -0.0040(10) C7 0.0379(12) 0.0391(13) 0.0305(12) -0.0011(9) 0.0095(9) -0.0052(10) C8 0.0370(15) 0.0502(17) 0.0574(17) 0.0002(13) 0.0044(13) -0.0112(12) C9 0.0326(11) 0.0374(12) 0.0229(10) 0.0027(8) 0.0042(8) -0.0051(9) C10 0.0358(13) 0.0375(13) 0.0382(12) -0.0017(10) 0.0074(9) -0.0017(11) C11 0.0329(13) 0.0547(16) 0.0425(13) -0.0025(11) 0.0102(10) -0.0054(11) C12 0.0438(14) 0.0447(15) 0.0388(13) 0.0013(10) 0.0070(10) -0.0118(12) C13 0.0461(15) 0.0362(14) 0.0524(15) -0.0031(11) 0.0092(11) -0.0025(12) C14 0.0352(14) 0.0435(14) 0.0473(14) -0.0045(11) 0.0104(10) -0.0022(11) #----------------------------------------------------------------------------# # 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 N1 C1 1.297(3) . ? N1 C9 1.424(3) . ? N2 C1 1.348(3) . ? C1 C2 1.491(3) . ? C2 C7 1.395(3) . ? C2 C3 1.395(3) . ? C3 C4 1.383(3) . ? C4 C5 1.389(3) . ? C5 C6 1.391(3) . ? C5 C8 1.506(3) . ? C6 C7 1.385(3) . ? C9 C10 1.386(3) . ? C9 C14 1.394(3) . ? C10 C11 1.385(3) . ? C11 C12 1.388(4) . ? C12 C13 1.383(4) . ? C13 C14 1.383(3) . ? 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 C1 N1 C9 118.48(16) . . ? N1 C1 N2 124.0(2) . . ? N1 C1 C2 118.68(17) . . ? N2 C1 C2 117.27(18) . . ? C7 C2 C3 118.00(19) . . ? C7 C2 C1 121.69(18) . . ? C3 C2 C1 120.14(17) . . ? C4 C3 C2 120.80(19) . . ? C3 C4 C5 121.3(2) . . ? C4 C5 C6 117.9(2) . . ? C4 C5 C8 121.2(2) . . ? C6 C5 C8 120.9(2) . . ? C7 C6 C5 121.2(2) . . ? C6 C7 C2 120.8(2) . . ? C10 C9 C14 118.7(2) . . ? C10 C9 N1 120.2(2) . . ? C14 C9 N1 120.98(19) . . ? C11 C10 C9 120.7(2) . . ? C10 C11 C12 120.5(2) . . ? C13 C12 C11 119.0(2) . . ? C14 C13 C12 120.6(2) . . ? C13 C14 C9 120.5(2) . . ? #===END