# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Polly Arnold' 'Stephen T. Liddle' _publ_contact_author_name 'Polly Arnold' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NOTTS NG7 2RD UNITED KINGDOM ; _publ_contact_author_email POLLY.ARNOLD@NOTTINGHAM.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Regioselective C-H activation of lanthanide-bound N-heterocyclic carbenes ; data_ndcbns_1 _database_code_depnum_ccdc_archive 'CCDC 280856' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H60 N5 Nd Si4' _chemical_formula_sum 'C25 H60 N5 Nd Si4' _chemical_formula_weight 687.38 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.1289(12) _cell_length_b 11.6659(8) _cell_length_c 17.7378(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.709(2) _cell_angle_gamma 90.00 _cell_volume 3659.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12206 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.74 _exptl_crystal_size_mid 0.69 _exptl_crystal_size_min 0.61 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3896 _exptl_absorpt_correction_T_max 0.4477 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22452 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8348 _reflns_number_gt 6977 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0241P)^2^+3.7417P] 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_extinction_coef ? _refine_ls_number_reflns 8348 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.267386(7) 0.612211(11) 0.377175(7) 0.01899(4) Uani 1 1 d . . . N1 N 0.23700(13) 0.4550(2) 0.54963(13) 0.0288(5) Uani 1 1 d . . . N2 N 0.37346(12) 0.70566(18) 0.43302(13) 0.0244(5) Uani 1 1 d . . . N3 N 0.34567(13) 0.5345(2) 0.56832(13) 0.0276(5) Uani 1 1 d . . . C2 C 0.28170(14) 0.5176(2) 0.51288(15) 0.0221(5) Uani 1 1 d . . . C4 C 0.3406(2) 0.4851(3) 0.63698(19) 0.0524(10) Uani 1 1 d . . . H4A H 0.3780 0.4864 0.6838 0.063 Uiso 1 1 calc R . . C5 C 0.2728(2) 0.4347(3) 0.62536(19) 0.0532(10) Uani 1 1 d . . . H5A H 0.2530 0.3928 0.6624 0.064 Uiso 1 1 calc R . . C6 C 0.16036(15) 0.4094(2) 0.51524(17) 0.0279(6) Uani 1 1 d . . . C7 C 0.13821(16) 0.4407(3) 0.43019(17) 0.0322(6) Uani 1 1 d . . . H7A H 0.1360 0.5243 0.4248 0.048 Uiso 1 1 calc R . . H7B H 0.0885 0.4080 0.4075 0.048 Uiso 1 1 calc R . . H7C H 0.1758 0.4100 0.4034 0.048 Uiso 1 1 calc R . . C8 C 0.16125(18) 0.2788(3) 0.5246(2) 0.0415(8) Uani 1 1 d . . . H8A H 0.1748 0.2593 0.5797 0.062 Uiso 1 1 calc R . . H8B H 0.1985 0.2456 0.4984 0.062 Uiso 1 1 calc R . . H8C H 0.1110 0.2479 0.5018 0.062 Uiso 1 1 calc R . . C9 C 0.10483(18) 0.4625(3) 0.5584(2) 0.0425(8) Uani 1 1 d . . . H9A H 0.1069 0.5462 0.5548 0.064 Uiso 1 1 calc R . . H9B H 0.1184 0.4394 0.6129 0.064 Uiso 1 1 calc R . . H9C H 0.0535 0.4360 0.5354 0.064 Uiso 1 1 calc R . . C10 C 0.41434(16) 0.5960(3) 0.55964(16) 0.0314(6) Uani 1 1 d . . . H10A H 0.4592 0.5520 0.5865 0.038 Uiso 1 1 calc R . . H10B H 0.4157 0.6713 0.5856 0.038 Uiso 1 1 calc R . . C11 C 0.42018(15) 0.6154(2) 0.47587(16) 0.0271(6) Uani 1 1 d . . . H11A H 0.4736 0.6327 0.4758 0.033 Uiso 1 1 calc R . . H11B H 0.4072 0.5425 0.4474 0.033 Uiso 1 1 calc R . . C12 C 0.41017(17) 0.8191(2) 0.43545(17) 0.0320(6) Uani 1 1 d . . . C13 C 0.3504(2) 0.9029(3) 0.3937(2) 0.0448(8) Uani 1 1 d . . . H13A H 0.3104 0.9104 0.4225 0.067 Uiso 1 1 calc R . . H13B H 0.3288 0.8742 0.3416 0.067 Uiso 1 1 calc R . . H13C H 0.3738 0.9779 0.3902 0.067 Uiso 1 1 calc R . . C14 C 0.47568(19) 0.8160(3) 0.39307(18) 0.0417(8) Uani 1 1 d . . . H14A H 0.5139 0.7609 0.4186 0.063 Uiso 1 1 calc R . . H14B H 0.4985 0.8924 0.3944 0.063 Uiso 1 1 calc R . . H14C H 0.4564 0.7928 0.3392 0.063 Uiso 1 1 calc R . . C15 C 0.4404(2) 0.8624(3) 0.51823(19) 0.0436(8) Uani 1 1 d . . . H15A H 0.4003 0.8578 0.5472 0.065 Uiso 1 1 calc R . . H15B H 0.4570 0.9421 0.5167 0.065 Uiso 1 1 calc R . . H15C H 0.4833 0.8148 0.5436 0.065 Uiso 1 1 calc R . . N4 N 0.15132(12) 0.71514(19) 0.34630(13) 0.0255(5) Uani 1 1 d . . . Si1 Si 0.13622(5) 0.81240(6) 0.41345(5) 0.02919(17) Uani 1 1 d . . . C16 C 0.20836(17) 0.7915(2) 0.50677(16) 0.0326(6) Uani 1 1 d . . . H16A H 0.2590 0.7865 0.4959 0.049 Uiso 1 1 calc R . . H16B H 0.1972 0.7206 0.5317 0.049 Uiso 1 1 calc R . . H16C H 0.2064 0.8566 0.5412 0.049 Uiso 1 1 calc R . . C17 C 0.1398(2) 0.9648(3) 0.3818(2) 0.0575(10) Uani 1 1 d . . . H17A H 0.0967 0.9803 0.3389 0.086 Uiso 1 1 calc R . . H17B H 0.1870 0.9781 0.3647 0.086 Uiso 1 1 calc R . . H17C H 0.1377 1.0159 0.4251 0.086 Uiso 1 1 calc R . . C18 C 0.04359(18) 0.7975(3) 0.4439(2) 0.0497(9) Uani 1 1 d . . . H18A H 0.0024 0.8244 0.4022 0.075 Uiso 1 1 calc R . . H18B H 0.0449 0.8436 0.4904 0.075 Uiso 1 1 calc R . . H18C H 0.0352 0.7169 0.4550 0.075 Uiso 1 1 calc R . . Si2 Si 0.08905(5) 0.68956(7) 0.26062(5) 0.03188(18) Uani 1 1 d . . . C19 C 0.11009(19) 0.5474(3) 0.22038(19) 0.0434(8) Uani 1 1 d . . . H19A H 0.1640 0.5433 0.2198 0.065 Uiso 1 1 calc R . . H19B H 0.0799 0.5390 0.1676 0.065 Uiso 1 1 calc R . . H19C H 0.0974 0.4856 0.2528 0.065 Uiso 1 1 calc R . . C20 C -0.01291(19) 0.6830(4) 0.2664(2) 0.0657(12) Uani 1 1 d . . . H20A H -0.0283 0.7571 0.2839 0.099 Uiso 1 1 calc R . . H20B H -0.0196 0.6232 0.3031 0.099 Uiso 1 1 calc R . . H20C H -0.0441 0.6651 0.2153 0.099 Uiso 1 1 calc R . . C21 C 0.0933(2) 0.8016(3) 0.1859(2) 0.0592(11) Uani 1 1 d . . . H21A H 0.0784 0.8759 0.2036 0.089 Uiso 1 1 calc R . . H21B H 0.0588 0.7809 0.1372 0.089 Uiso 1 1 calc R . . H21C H 0.1450 0.8066 0.1780 0.089 Uiso 1 1 calc R . . N5 N 0.31275(12) 0.46332(18) 0.30766(12) 0.0220(4) Uani 1 1 d . . . Si3 Si 0.31955(4) 0.31940(6) 0.32560(4) 0.02353(15) Uani 1 1 d . . . C22 C 0.34535(17) 0.2853(2) 0.43144(16) 0.0319(6) Uani 1 1 d . . . H22A H 0.3069 0.3168 0.4567 0.048 Uiso 1 1 calc R . . H22B H 0.3946 0.3194 0.4544 0.048 Uiso 1 1 calc R . . H22C H 0.3480 0.2020 0.4385 0.048 Uiso 1 1 calc R . . C23 C 0.22811(17) 0.2444(3) 0.28465(18) 0.0361(7) Uani 1 1 d . . . H23A H 0.1893 0.2712 0.3111 0.054 Uiso 1 1 calc R . . H23B H 0.2350 0.1616 0.2920 0.054 Uiso 1 1 calc R . . H23C H 0.2123 0.2614 0.2293 0.054 Uiso 1 1 calc R . . C24 C 0.39528(16) 0.2445(2) 0.28631(18) 0.0332(6) Uani 1 1 d . . . H24A H 0.4447 0.2775 0.3097 0.050 Uiso 1 1 calc R . . H24B H 0.3852 0.2543 0.2301 0.050 Uiso 1 1 calc R . . H24C H 0.3953 0.1626 0.2987 0.050 Uiso 1 1 calc R . . Si4 Si 0.34119(4) 0.52165(6) 0.23012(4) 0.02373(15) Uani 1 1 d . . . C25 C 0.44652(16) 0.5295(3) 0.24290(17) 0.0327(6) Uani 1 1 d . . . H25A H 0.4673 0.4518 0.2447 0.049 Uiso 1 1 calc R . . H25B H 0.4683 0.5695 0.2912 0.049 Uiso 1 1 calc R . . H25C H 0.4589 0.5713 0.1994 0.049 Uiso 1 1 calc R . . C26 C 0.30085(18) 0.4487(2) 0.13549(16) 0.0335(6) Uani 1 1 d . . . H26A H 0.3194 0.3696 0.1373 0.050 Uiso 1 1 calc R . . H26B H 0.3166 0.4901 0.0936 0.050 Uiso 1 1 calc R . . H26C H 0.2455 0.4485 0.1262 0.050 Uiso 1 1 calc R . . C27 C 0.30900(17) 0.6764(2) 0.21897(16) 0.0311(6) Uani 1 1 d . . . H27A H 0.2543 0.6801 0.2150 0.047 Uiso 1 1 calc R . . H27B H 0.3211 0.7087 0.1721 0.047 Uiso 1 1 calc R . . H27C H 0.3350 0.7205 0.2641 0.047 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 Nd1 0.01931(7) 0.01813(7) 0.01961(7) -0.00048(5) 0.00445(5) -0.00244(6) N1 0.0273(12) 0.0328(13) 0.0254(12) 0.0079(10) 0.0043(9) -0.0048(10) N2 0.0249(12) 0.0224(11) 0.0268(11) -0.0034(9) 0.0075(9) -0.0069(9) N3 0.0260(12) 0.0310(12) 0.0241(11) 0.0061(9) 0.0018(9) -0.0035(10) C2 0.0228(13) 0.0190(12) 0.0245(13) 0.0005(10) 0.0053(10) -0.0010(10) C4 0.046(2) 0.074(3) 0.0302(17) 0.0207(16) -0.0070(15) -0.0211(18) C5 0.048(2) 0.077(3) 0.0304(17) 0.0262(17) -0.0003(15) -0.0203(19) C6 0.0233(13) 0.0270(14) 0.0346(15) 0.0059(11) 0.0088(11) -0.0034(11) C7 0.0240(14) 0.0340(15) 0.0363(16) 0.0053(12) 0.0016(12) -0.0083(12) C8 0.0351(17) 0.0282(15) 0.062(2) 0.0119(15) 0.0124(15) -0.0042(13) C9 0.0375(18) 0.0421(18) 0.054(2) -0.0022(15) 0.0231(15) -0.0058(15) C10 0.0242(14) 0.0362(16) 0.0307(14) 0.0013(12) -0.0004(11) -0.0074(12) C11 0.0225(13) 0.0280(13) 0.0313(14) -0.0054(11) 0.0068(11) -0.0049(11) C12 0.0383(16) 0.0280(14) 0.0326(15) -0.0070(12) 0.0145(13) -0.0183(12) C13 0.064(2) 0.0257(15) 0.050(2) 0.0006(14) 0.0238(17) -0.0080(15) C14 0.0471(19) 0.0458(18) 0.0376(17) -0.0090(14) 0.0211(14) -0.0254(15) C15 0.055(2) 0.0389(17) 0.0423(18) -0.0171(14) 0.0234(16) -0.0281(15) N4 0.0227(11) 0.0249(11) 0.0277(11) 0.0035(9) 0.0032(9) -0.0017(9) Si1 0.0284(4) 0.0226(4) 0.0356(4) 0.0000(3) 0.0050(3) 0.0030(3) C16 0.0355(16) 0.0285(14) 0.0341(15) -0.0049(12) 0.0081(13) -0.0020(12) C17 0.074(3) 0.0261(16) 0.069(3) 0.0035(16) 0.009(2) 0.0073(17) C18 0.0345(18) 0.064(2) 0.052(2) -0.0109(18) 0.0117(15) 0.0078(17) Si2 0.0253(4) 0.0381(4) 0.0293(4) 0.0007(3) -0.0003(3) 0.0038(3) C19 0.0406(19) 0.0463(19) 0.0387(18) -0.0079(15) -0.0014(14) -0.0008(15) C20 0.0252(18) 0.099(3) 0.068(3) -0.034(2) -0.0001(17) -0.0026(19) C21 0.079(3) 0.053(2) 0.0386(19) 0.0134(17) -0.0008(19) 0.017(2) N5 0.0227(11) 0.0199(10) 0.0235(11) -0.0015(8) 0.0051(9) -0.0024(9) Si3 0.0243(4) 0.0210(3) 0.0265(4) -0.0036(3) 0.0082(3) -0.0018(3) C22 0.0400(17) 0.0260(14) 0.0318(15) 0.0026(11) 0.0122(13) 0.0051(12) C23 0.0346(17) 0.0313(15) 0.0451(18) -0.0136(13) 0.0145(14) -0.0093(13) C24 0.0313(16) 0.0306(15) 0.0392(16) -0.0032(12) 0.0115(13) 0.0051(12) Si4 0.0253(4) 0.0256(4) 0.0209(3) -0.0028(3) 0.0063(3) -0.0042(3) C25 0.0275(15) 0.0388(16) 0.0336(15) -0.0006(13) 0.0106(12) -0.0043(13) C26 0.0415(17) 0.0326(15) 0.0256(14) -0.0044(12) 0.0054(12) -0.0051(13) C27 0.0397(17) 0.0264(14) 0.0268(14) 0.0023(11) 0.0066(12) -0.0020(12) _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 Nd1 N2 2.243(2) . ? Nd1 N5 2.379(2) . ? Nd1 N4 2.380(2) . ? Nd1 C2 2.609(3) . ? Nd1 C11 2.933(3) . ? N1 C2 1.359(3) . ? N1 C5 1.377(4) . ? N1 C6 1.488(3) . ? N2 C11 1.456(3) . ? N2 C12 1.478(3) . ? N3 C2 1.360(3) . ? N3 C4 1.368(4) . ? N3 C10 1.474(3) . ? C4 C5 1.337(5) . ? C6 C7 1.518(4) . ? C6 C9 1.524(4) . ? C6 C8 1.533(4) . ? C10 C11 1.529(4) . ? C12 C13 1.524(5) . ? C12 C15 1.535(4) . ? C12 C14 1.539(4) . ? N4 Si2 1.708(2) . ? N4 Si1 1.710(2) . ? Si1 C17 1.870(3) . ? Si1 C18 1.882(3) . ? Si1 C16 1.886(3) . ? Si2 C21 1.875(4) . ? Si2 C20 1.875(4) . ? Si2 C19 1.878(3) . ? N5 Si3 1.708(2) . ? N5 Si4 1.713(2) . ? Si3 C23 1.874(3) . ? Si3 C22 1.875(3) . ? Si3 C24 1.886(3) . ? Si4 C25 1.875(3) . ? Si4 C26 1.880(3) . ? Si4 C27 1.894(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 Nd1 N5 102.90(8) . . ? N2 Nd1 N4 119.03(8) . . ? N5 Nd1 N4 129.66(7) . . ? N2 Nd1 C2 84.07(8) . . ? N5 Nd1 C2 101.16(7) . . ? N4 Nd1 C2 109.23(8) . . ? N2 Nd1 C11 28.94(8) . . ? N5 Nd1 C11 85.97(7) . . ? N4 Nd1 C11 143.33(8) . . ? C2 Nd1 C11 64.25(8) . . ? C2 N1 C5 111.0(2) . . ? C2 N1 C6 126.7(2) . . ? C5 N1 C6 122.3(2) . . ? C11 N2 C12 115.2(2) . . ? C11 N2 Nd1 102.87(15) . . ? C12 N2 Nd1 141.73(18) . . ? C2 N3 C4 111.6(2) . . ? C2 N3 C10 126.9(2) . . ? C4 N3 C10 121.5(2) . . ? N1 C2 N3 103.6(2) . . ? N1 C2 Nd1 136.15(18) . . ? N3 C2 Nd1 120.12(17) . . ? C5 C4 N3 106.7(3) . . ? C4 C5 N1 107.1(3) . . ? N1 C6 C7 109.9(2) . . ? N1 C6 C9 108.0(2) . . ? C7 C6 C9 110.0(2) . . ? N1 C6 C8 108.9(2) . . ? C7 C6 C8 109.9(3) . . ? C9 C6 C8 110.0(2) . . ? N3 C10 C11 114.5(2) . . ? N2 C11 C10 117.2(2) . . ? N2 C11 Nd1 48.19(11) . . ? C10 C11 Nd1 108.65(16) . . ? N2 C12 C13 107.0(2) . . ? N2 C12 C15 112.7(2) . . ? C13 C12 C15 108.6(3) . . ? N2 C12 C14 110.8(2) . . ? C13 C12 C14 108.7(3) . . ? C15 C12 C14 108.9(2) . . ? Si2 N4 Si1 124.05(14) . . ? Si2 N4 Nd1 119.63(12) . . ? Si1 N4 Nd1 116.32(11) . . ? N4 Si1 C17 113.57(16) . . ? N4 Si1 C18 115.38(14) . . ? C17 Si1 C18 105.45(18) . . ? N4 Si1 C16 109.83(12) . . ? C17 Si1 C16 108.86(16) . . ? C18 Si1 C16 103.08(15) . . ? N4 Si2 C21 112.63(15) . . ? N4 Si2 C20 115.14(15) . . ? C21 Si2 C20 105.2(2) . . ? N4 Si2 C19 110.04(13) . . ? C21 Si2 C19 107.69(17) . . ? C20 Si2 C19 105.65(18) . . ? Si3 N5 Si4 121.20(13) . . ? Si3 N5 Nd1 129.80(11) . . ? Si4 N5 Nd1 109.00(10) . . ? N5 Si3 C23 111.41(13) . . ? N5 Si3 C22 112.75(12) . . ? C23 Si3 C22 107.09(14) . . ? N5 Si3 C24 114.54(12) . . ? C23 Si3 C24 107.12(13) . . ? C22 Si3 C24 103.31(13) . . ? N5 Si4 C25 113.62(12) . . ? N5 Si4 C26 114.25(12) . . ? C25 Si4 C26 108.41(14) . . ? N5 Si4 C27 108.80(12) . . ? C25 Si4 C27 104.36(13) . . ? C26 Si4 C27 106.72(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.218 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.080 #===end data_ndbnic_2 _database_code_depnum_ccdc_archive 'CCDC 280857' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47.50 H104 I2 N8 Nd2 Si6' _chemical_formula_sum 'C47.50 H104 I2 N8 Nd2 Si6' _chemical_formula_weight 1498.21 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.280(2) _cell_length_b 14.204(3) _cell_length_c 14.632(3) _cell_angle_alpha 63.675(3) _cell_angle_beta 70.505(3) _cell_angle_gamma 74.060(3) _cell_volume 1958.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8975 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.49 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 755 _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4348 _exptl_absorpt_correction_T_max 0.8252 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18558 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6877 _reflns_number_gt 6106 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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. Highly disordered lattice solvent molecules (25 electons per unit cell) were accounted for using the PLATON SQUEEZE procedure (P. v.d. Sluis & A.L. Spek, Acta Cryst. 1990, A46, 194-201). The total volume of the void was 472.62 \%A**3, equating to half a molecule of toluene per dimer, half in the unit cell. Although solvent atoms were not included in the refinement model they are included in the formulae and in the calculation of the formula weight, density, mu, F(000), etc. ; _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^)+(0.0586P)^2^+6.7090P] 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_extinction_coef ? _refine_ls_number_reflns 6877 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.40677(2) 0.38121(2) 0.18437(2) 0.02522(10) Uani 1 1 d . . . I1 I 0.66360(3) 0.48529(3) 0.03873(3) 0.03752(12) Uani 1 1 d . . . N1 N 0.0988(4) 0.2870(4) 0.2500(4) 0.0334(10) Uani 1 1 d . . . N2 N 0.5258(4) 0.2260(3) 0.1984(4) 0.0352(11) Uani 1 1 d . . . N3 N 0.2597(4) 0.1741(4) 0.2204(4) 0.0347(10) Uani 1 1 d . . . C2 C 0.2270(5) 0.2767(4) 0.2120(4) 0.0291(11) Uani 1 1 d . . . C4 C 0.1551(6) 0.1206(5) 0.2650(5) 0.0401(14) Uani 1 1 d . . . C5 C 0.0548(6) 0.1928(5) 0.2818(5) 0.0435(14) Uani 1 1 d . . . H5A H -0.0314 0.1813 0.3105 0.052 Uiso 1 1 calc R . . C6 C 0.0106(5) 0.3864(5) 0.2515(5) 0.0375(13) Uani 1 1 d . . . C7 C 0.0827(5) 0.4687(5) 0.2372(5) 0.0417(14) Uani 1 1 d . . . H7A H 0.1425 0.4885 0.1677 0.063 Uiso 1 1 calc R . . H7B H 0.1299 0.4395 0.2918 0.063 Uiso 1 1 calc R . . H7C H 0.0228 0.5317 0.2430 0.063 Uiso 1 1 calc R . . C8 C -0.0882(6) 0.3618(6) 0.3570(6) 0.0559(18) Uani 1 1 d . . . H8A H -0.0453 0.3355 0.4139 0.084 Uiso 1 1 calc R . . H8B H -0.1350 0.3075 0.3675 0.084 Uiso 1 1 calc R . . H8C H -0.1478 0.4266 0.3574 0.084 Uiso 1 1 calc R . . C9 C -0.0545(6) 0.4261(5) 0.1626(6) 0.0512(16) Uani 1 1 d . . . H9A H 0.0099 0.4355 0.0961 0.077 Uiso 1 1 calc R . . H9B H -0.1087 0.4942 0.1582 0.077 Uiso 1 1 calc R . . H9C H -0.1068 0.3742 0.1763 0.077 Uiso 1 1 calc R . . C10 C 0.3879(6) 0.1230(5) 0.1836(6) 0.0481(16) Uani 1 1 d . . . H10A H 0.3846 0.0950 0.1335 0.058 Uiso 1 1 calc R . . H10B H 0.4133 0.0617 0.2445 0.058 Uiso 1 1 calc R . . C11 C 0.4903(5) 0.1959(4) 0.1298(5) 0.0391(13) Uani 1 1 d . . . H11A H 0.5674 0.1598 0.0943 0.047 Uiso 1 1 calc R . . H11B H 0.4595 0.2614 0.0747 0.047 Uiso 1 1 calc R . . C12 C 0.6379(6) 0.1610(5) 0.2391(6) 0.0501(17) Uani 1 1 d . . . C13 C 0.7585(6) 0.1652(6) 0.1485(7) 0.066(2) Uani 1 1 d . . . H13A H 0.7714 0.2393 0.1056 0.100 Uiso 1 1 calc R . . H13B H 0.7484 0.1335 0.1047 0.100 Uiso 1 1 calc R . . H13C H 0.8323 0.1255 0.1777 0.100 Uiso 1 1 calc R . . C14 C 0.6574(7) 0.2084(6) 0.3055(6) 0.061(2) Uani 1 1 d . . . H14A H 0.6752 0.2812 0.2617 0.092 Uiso 1 1 calc R . . H14B H 0.7293 0.1656 0.3362 0.092 Uiso 1 1 calc R . . H14C H 0.5803 0.2092 0.3618 0.092 Uiso 1 1 calc R . . C15 C 0.6194(7) 0.0438(5) 0.3062(7) 0.072(2) Uani 1 1 d . . . H15A H 0.5402 0.0404 0.3614 0.108 Uiso 1 1 calc R . . H15B H 0.6912 0.0058 0.3386 0.108 Uiso 1 1 calc R . . H15C H 0.6151 0.0108 0.2614 0.108 Uiso 1 1 calc R . . Si1 Si 0.15653(19) -0.02515(14) 0.30286(18) 0.0544(5) Uani 1 1 d . . . C16 C 0.2539(8) -0.1031(6) 0.3991(7) 0.076(3) Uani 1 1 d . . . H16A H 0.2301 -0.1744 0.4395 0.113 Uiso 1 1 calc R . . H16B H 0.2392 -0.0678 0.4471 0.113 Uiso 1 1 calc R . . H16C H 0.3440 -0.1084 0.3620 0.113 Uiso 1 1 calc R . . C17 C 0.2185(11) -0.0575(7) 0.1877(8) 0.094(3) Uani 1 1 d . . . H17A H 0.2077 -0.1306 0.2068 0.141 Uiso 1 1 calc R . . H17B H 0.3091 -0.0507 0.1598 0.141 Uiso 1 1 calc R . . H17C H 0.1723 -0.0086 0.1341 0.141 Uiso 1 1 calc R . . C18 C -0.0092(8) -0.0499(6) 0.3651(9) 0.088(3) Uani 1 1 d . . . H18A H -0.0115 -0.1265 0.3947 0.133 Uiso 1 1 calc R . . H18B H -0.0594 -0.0135 0.3124 0.133 Uiso 1 1 calc R . . H18C H -0.0449 -0.0230 0.4214 0.133 Uiso 1 1 calc R . . N4 N 0.3577(5) 0.4179(4) 0.3336(4) 0.0382(11) Uani 1 1 d . . . Si2 Si 0.30893(17) 0.32571(17) 0.45702(13) 0.0488(4) Uani 1 1 d . . . C19 C 0.1492(8) 0.3689(8) 0.5333(6) 0.075(2) Uani 1 1 d . . . H19A H 0.0924 0.4092 0.4860 0.112 Uiso 1 1 calc R . . H19B H 0.1589 0.4138 0.5647 0.112 Uiso 1 1 calc R . . H19C H 0.1128 0.3061 0.5892 0.112 Uiso 1 1 calc R . . C20 C 0.2903(7) 0.2047(6) 0.4488(5) 0.0557(18) Uani 1 1 d . . . H20A H 0.2167 0.2198 0.4205 0.084 Uiso 1 1 calc R . . H20B H 0.2772 0.1479 0.5191 0.084 Uiso 1 1 calc R . . H20C H 0.3671 0.1823 0.4024 0.084 Uiso 1 1 calc R . . C21 C 0.4232(8) 0.2859(8) 0.5406(6) 0.077(3) Uani 1 1 d . . . H21A H 0.4311 0.3482 0.5495 0.116 Uiso 1 1 calc R . . H21B H 0.5067 0.2571 0.5064 0.116 Uiso 1 1 calc R . . H21C H 0.3917 0.2317 0.6096 0.116 Uiso 1 1 calc R . . Si3 Si 0.3870(2) 0.54016(17) 0.30948(16) 0.0550(5) Uani 1 1 d . . . C22 C 0.2823(10) 0.6006(9) 0.4041(8) 0.099(3) Uani 1 1 d . . . H22A H 0.3101 0.6672 0.3878 0.148 Uiso 1 1 calc R . . H22B H 0.2874 0.5514 0.4758 0.148 Uiso 1 1 calc R . . H22C H 0.1943 0.6153 0.3986 0.148 Uiso 1 1 calc R . . C23 C 0.5535(8) 0.5357(8) 0.3103(7) 0.078(3) Uani 1 1 d . . . H23A H 0.5687 0.6078 0.2904 0.118 Uiso 1 1 calc R . . H23B H 0.6131 0.5061 0.2600 0.118 Uiso 1 1 calc R . . H23C H 0.5663 0.4910 0.3810 0.118 Uiso 1 1 calc R . . C24 C 0.3563(7) 0.6353(6) 0.1770(6) 0.062(2) Uani 1 1 d . . . H24A H 0.3783 0.7046 0.1591 0.093 Uiso 1 1 calc R . . H24B H 0.2662 0.6434 0.1798 0.093 Uiso 1 1 calc R . . H24C H 0.4085 0.6073 0.1234 0.093 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 Nd1 0.02227(15) 0.02746(16) 0.02535(16) -0.00717(12) -0.00755(11) -0.00607(11) I1 0.0341(2) 0.0437(2) 0.0298(2) -0.00098(16) -0.01292(15) -0.01499(16) N1 0.030(2) 0.034(2) 0.033(2) -0.003(2) -0.0132(19) -0.0109(19) N2 0.024(2) 0.026(2) 0.049(3) -0.009(2) -0.010(2) -0.0003(18) N3 0.029(2) 0.030(2) 0.044(3) -0.009(2) -0.012(2) -0.0080(19) C2 0.031(3) 0.027(3) 0.026(3) -0.004(2) -0.009(2) -0.008(2) C4 0.037(3) 0.034(3) 0.050(4) -0.006(3) -0.017(3) -0.015(3) C5 0.031(3) 0.042(3) 0.056(4) -0.008(3) -0.017(3) -0.014(3) C6 0.024(3) 0.047(3) 0.039(3) -0.013(3) -0.007(2) -0.006(2) C7 0.030(3) 0.043(3) 0.053(4) -0.022(3) -0.012(3) 0.001(2) C8 0.037(3) 0.070(5) 0.051(4) -0.024(4) 0.002(3) -0.009(3) C9 0.048(4) 0.049(4) 0.059(4) -0.018(3) -0.032(3) 0.006(3) C10 0.037(3) 0.031(3) 0.077(5) -0.024(3) -0.013(3) -0.005(3) C11 0.036(3) 0.027(3) 0.047(3) -0.014(3) -0.004(3) -0.003(2) C12 0.034(3) 0.037(3) 0.064(4) -0.002(3) -0.021(3) 0.000(3) C13 0.029(3) 0.055(4) 0.097(6) -0.020(4) -0.013(4) 0.003(3) C14 0.043(4) 0.064(5) 0.071(5) -0.008(4) -0.034(4) -0.005(3) C15 0.047(4) 0.036(4) 0.100(6) 0.005(4) -0.031(4) 0.005(3) Si1 0.0494(11) 0.0349(9) 0.0782(14) -0.0116(9) -0.0229(10) -0.0144(8) C16 0.069(5) 0.037(4) 0.102(7) 0.002(4) -0.039(5) -0.009(4) C17 0.110(8) 0.065(6) 0.109(8) -0.018(5) -0.033(6) -0.034(5) C18 0.056(5) 0.052(5) 0.143(9) -0.007(5) -0.035(5) -0.025(4) N4 0.036(3) 0.050(3) 0.033(3) -0.019(2) -0.009(2) -0.008(2) Si2 0.0442(10) 0.0728(13) 0.0271(8) -0.0140(8) -0.0116(7) -0.0109(9) C19 0.060(5) 0.112(7) 0.045(4) -0.031(5) 0.002(4) -0.017(5) C20 0.051(4) 0.067(5) 0.031(3) 0.002(3) -0.014(3) -0.013(3) C21 0.076(6) 0.110(7) 0.046(4) -0.020(4) -0.035(4) -0.007(5) Si3 0.0585(12) 0.0663(13) 0.0544(11) -0.0408(10) -0.0011(9) -0.0162(10) C22 0.104(8) 0.108(8) 0.100(8) -0.080(7) 0.013(6) -0.020(6) C23 0.081(6) 0.116(7) 0.072(5) -0.053(5) -0.014(4) -0.043(5) C24 0.063(5) 0.050(4) 0.073(5) -0.031(4) -0.001(4) -0.015(3) _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 Nd1 N2 2.205(4) . ? Nd1 N4 2.322(5) . ? Nd1 C2 2.656(5) . ? Nd1 C11 2.907(6) . ? Nd1 I1 3.2087(7) 2_665 ? Nd1 I1 3.2492(6) . ? I1 Nd1 3.2087(7) 2_665 ? N1 C2 1.357(7) . ? N1 C5 1.383(7) . ? N1 C6 1.491(7) . ? N2 C11 1.448(8) . ? N2 C12 1.476(7) . ? N3 C2 1.360(7) . ? N3 C4 1.390(7) . ? N3 C10 1.470(7) . ? C4 C5 1.339(9) . ? C4 Si1 1.888(6) . ? C6 C7 1.506(8) . ? C6 C9 1.518(8) . ? C6 C8 1.528(8) . ? C10 C11 1.534(8) . ? C12 C14 1.499(10) . ? C12 C13 1.543(10) . ? C12 C15 1.544(9) . ? Si1 C17 1.806(11) . ? Si1 C18 1.841(8) . ? Si1 C16 1.843(8) . ? N4 Si2 1.707(5) . ? N4 Si3 1.715(5) . ? Si2 C20 1.847(8) . ? Si2 C21 1.875(7) . ? Si2 C19 1.878(8) . ? Si3 C22 1.859(8) . ? Si3 C23 1.867(8) . ? Si3 C24 1.890(9) . ? 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 Nd1 N4 113.74(18) . . ? N2 Nd1 C2 81.91(16) . . ? N4 Nd1 C2 106.31(17) . . ? N2 Nd1 C11 28.96(18) . . ? N4 Nd1 C11 137.80(18) . . ? C2 Nd1 C11 63.23(16) . . ? N2 Nd1 I1 114.12(13) . 2_665 ? N4 Nd1 I1 132.13(12) . 2_665 ? C2 Nd1 I1 80.99(11) . 2_665 ? C11 Nd1 I1 88.42(13) . 2_665 ? N2 Nd1 I1 86.43(12) . . ? N4 Nd1 I1 104.21(12) . . ? C2 Nd1 I1 149.47(11) . . ? C11 Nd1 I1 93.94(11) . . ? I1 Nd1 I1 78.250(15) 2_665 . ? Nd1 I1 Nd1 101.750(15) 2_665 . ? C2 N1 C5 111.1(5) . . ? C2 N1 C6 126.8(4) . . ? C5 N1 C6 121.9(5) . . ? C11 N2 C12 116.7(5) . . ? C11 N2 Nd1 103.5(3) . . ? C12 N2 Nd1 138.5(4) . . ? C2 N3 C4 112.3(5) . . ? C2 N3 C10 126.0(4) . . ? C4 N3 C10 121.7(5) . . ? N1 C2 N3 103.4(4) . . ? N1 C2 Nd1 134.7(4) . . ? N3 C2 Nd1 119.0(3) . . ? C5 C4 N3 105.3(5) . . ? C5 C4 Si1 127.5(4) . . ? N3 C4 Si1 127.1(4) . . ? C4 C5 N1 107.9(5) . . ? N1 C6 C7 110.5(4) . . ? N1 C6 C9 107.5(5) . . ? C7 C6 C9 110.6(5) . . ? N1 C6 C8 109.4(5) . . ? C7 C6 C8 108.8(5) . . ? C9 C6 C8 110.1(5) . . ? N3 C10 C11 114.7(5) . . ? N2 C11 C10 115.6(5) . . ? N2 C11 Nd1 47.5(2) . . ? C10 C11 Nd1 110.8(4) . . ? N2 C12 C14 106.9(5) . . ? N2 C12 C13 111.2(6) . . ? C14 C12 C13 108.1(6) . . ? N2 C12 C15 112.3(5) . . ? C14 C12 C15 109.4(6) . . ? C13 C12 C15 108.8(6) . . ? C17 Si1 C18 110.6(5) . . ? C17 Si1 C16 111.1(5) . . ? C18 Si1 C16 109.4(4) . . ? C17 Si1 C4 110.3(4) . . ? C18 Si1 C4 106.7(3) . . ? C16 Si1 C4 108.5(3) . . ? Si2 N4 Si3 123.5(3) . . ? Si2 N4 Nd1 122.0(3) . . ? Si3 N4 Nd1 114.3(2) . . ? N4 Si2 C20 109.9(3) . . ? N4 Si2 C21 113.0(4) . . ? C20 Si2 C21 107.9(4) . . ? N4 Si2 C19 114.2(3) . . ? C20 Si2 C19 104.8(4) . . ? C21 Si2 C19 106.7(4) . . ? N4 Si3 C22 115.1(4) . . ? N4 Si3 C23 111.9(4) . . ? C22 Si3 C23 106.1(4) . . ? N4 Si3 C24 107.9(3) . . ? C22 Si3 C24 105.5(5) . . ? C23 Si3 C24 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.407 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.123 #===end data_ndcbsn_3 _database_code_depnum_ccdc_archive 'CCDC 280858' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H68 N5 Nd Si5' _chemical_formula_sum 'C28 H68 N5 Nd Si5' _chemical_formula_weight 759.56 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' Nd Nd -0.1943 3.0179 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9100(10) _cell_length_b 12.3766(11) _cell_length_c 17.1729(16) _cell_angle_alpha 108.306(2) _cell_angle_beta 97.810(2) _cell_angle_gamma 104.318(2) _cell_volume 2074.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6741 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.48 _exptl_crystal_description block _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 1.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.9197 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23779 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9420 _reflns_number_gt 7757 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9420 _refine_ls_number_parameters 413 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 1.627855(15) 0.822795(15) 0.721033(11) 0.03057(6) Uani 1 1 d . A . N1 N 1.7514(2) 1.1463(2) 0.86241(16) 0.0317(6) Uani 1 1 d . . . N2 N 1.7668(2) 0.8449(2) 0.63762(17) 0.0329(6) Uani 1 1 d . . . N3 N 1.8845(2) 1.0906(2) 0.79025(17) 0.0331(6) Uani 1 1 d . . . C2 C 1.7715(3) 1.0463(3) 0.8111(2) 0.0357(7) Uani 1 1 d . . . C4 C 1.9346(3) 1.2153(3) 0.8261(2) 0.0331(7) Uani 1 1 d . . . C5 C 1.8495(3) 1.2479(3) 0.8717(2) 0.0358(7) Uani 1 1 d . . . H5 H 1.8560 1.3275 0.9047 0.043 Uiso 1 1 calc R . . C6 C 1.6456(3) 1.1514(3) 0.9090(2) 0.0365(7) Uani 1 1 d . . . C7 C 1.7057(4) 1.1861(3) 1.0022(2) 0.0477(9) Uani 1 1 d . . . H7A H 1.7468 1.1269 1.0097 0.072 Uiso 1 1 calc R . . H7B H 1.6377 1.1887 1.0340 0.072 Uiso 1 1 calc R . . H7C H 1.7713 1.2651 1.0230 0.072 Uiso 1 1 calc R . . C8 C 1.5848(4) 1.2440(4) 0.8948(3) 0.0556(11) Uani 1 1 d . . . H8A H 1.6514 1.3225 0.9156 0.083 Uiso 1 1 calc R . . H8B H 1.5152 1.2483 0.9251 0.083 Uiso 1 1 calc R . . H8C H 1.5486 1.2209 0.8343 0.083 Uiso 1 1 calc R . . C9 C 1.5419(4) 1.0306(3) 0.8765(2) 0.0489(9) Uani 1 1 d . . . H9A H 1.5033 1.0095 0.8166 0.073 Uiso 1 1 calc R . . H9B H 1.4742 1.0343 0.9085 0.073 Uiso 1 1 calc R . . H9C H 1.5811 0.9700 0.8832 0.073 Uiso 1 1 calc R . . C10 C 1.9573(3) 1.0204(3) 0.7412(3) 0.0468(9) Uani 1 1 d . . . H10A H 2.0413 1.0338 0.7788 0.056 Uiso 1 1 calc R . . H10B H 1.9770 1.0513 0.6961 0.056 Uiso 1 1 calc R . . C11 C 1.8887(3) 0.8861(3) 0.7007(2) 0.0382(8) Uani 1 1 d . . . H11A H 1.9500 0.8481 0.6741 0.046 Uiso 1 1 calc R . . H11B H 1.8714 0.8558 0.7463 0.046 Uiso 1 1 calc R . . C12 C 1.7788(3) 0.8173(3) 0.5496(2) 0.0378(8) Uani 1 1 d . . . C13 C 1.6437(3) 0.7865(3) 0.4954(2) 0.0472(9) Uani 1 1 d . . . H13A H 1.5832 0.7224 0.5059 0.071 Uiso 1 1 calc R . . H13B H 1.6465 0.7598 0.4357 0.071 Uiso 1 1 calc R . . H13C H 1.6142 0.8574 0.5095 0.071 Uiso 1 1 calc R . . C14 C 1.8295(4) 0.7096(4) 0.5194(2) 0.0516(10) Uani 1 1 d . . . H14A H 1.9165 0.7280 0.5540 0.077 Uiso 1 1 calc R . . H14B H 1.8340 0.6924 0.4603 0.077 Uiso 1 1 calc R . . H14C H 1.7705 0.6396 0.5245 0.077 Uiso 1 1 calc R . . C15 C 1.8689(4) 0.9233(4) 0.5354(3) 0.0564(11) Uani 1 1 d . . . H15A H 1.8424 0.9948 0.5584 0.085 Uiso 1 1 calc R . . H15B H 1.8628 0.9042 0.4749 0.085 Uiso 1 1 calc R . . H15C H 1.9588 0.9383 0.5641 0.085 Uiso 1 1 calc R . . Si1 Si 2.07564(10) 1.31702(8) 0.80682(6) 0.0393(2) Uani 1 1 d . . . C16 C 2.0957(5) 1.4688(3) 0.8829(3) 0.0670(13) Uani 1 1 d . . . H16A H 2.1660 1.5277 0.8745 0.100 Uiso 1 1 calc R . . H16B H 2.1172 1.4703 0.9406 0.100 Uiso 1 1 calc R . . H16C H 2.0145 1.4883 0.8737 0.100 Uiso 1 1 calc R . . C17 C 2.2283(4) 1.2795(4) 0.8264(3) 0.0613(11) Uani 1 1 d . . . H17A H 2.2211 1.2029 0.7833 0.092 Uiso 1 1 calc R . . H17B H 2.2434 1.2735 0.8823 0.092 Uiso 1 1 calc R . . H17C H 2.3011 1.3423 0.8241 0.092 Uiso 1 1 calc R . . C18 C 2.0341(5) 1.3098(4) 0.6964(3) 0.0693(13) Uani 1 1 d . . . H18A H 1.9484 1.3207 0.6848 0.104 Uiso 1 1 calc R . . H18B H 2.0323 1.2317 0.6577 0.104 Uiso 1 1 calc R . . H18C H 2.0996 1.3731 0.6885 0.104 Uiso 1 1 calc R . . N4 N 1.6928(3) 0.6999(3) 0.78946(9) 0.0425(7) Uani 1 1 d D . . Si2 Si 1.67757(10) 0.56378(9) 0.71481(7) 0.0403(2) Uani 1 1 d . A . C19 C 1.8374(4) 0.5508(4) 0.6917(3) 0.0560(10) Uani 1 1 d . . . H19A H 1.8799 0.6185 0.6766 0.084 Uiso 1 1 calc R A . H19B H 1.8228 0.4758 0.6446 0.084 Uiso 1 1 calc R . . H19C H 1.8931 0.5513 0.7417 0.084 Uiso 1 1 calc R . . C20 C 1.5713(4) 0.5462(3) 0.6126(2) 0.0482(9) Uani 1 1 d . . . H20A H 1.4834 0.5441 0.6202 0.072 Uiso 1 1 calc R A . H20B H 1.5675 0.4715 0.5687 0.072 Uiso 1 1 calc R . . H20C H 1.6077 0.6138 0.5958 0.072 Uiso 1 1 calc R . . C21 C 1.6005(5) 0.4276(5) 0.7377(4) 0.0875(17) Uani 1 1 d . . . H21A H 1.6630 0.4183 0.7799 0.131 Uiso 1 1 calc R A . H21B H 1.5747 0.3569 0.6858 0.131 Uiso 1 1 calc R . . H21C H 1.5236 0.4365 0.7594 0.131 Uiso 1 1 calc R . . Si3 Si 1.7786(3) 0.7581(3) 0.89238(10) 0.0491(8) Uani 0.581(6) 1 d PD A 1 C22 C 1.9225(9) 0.8980(9) 0.9234(6) 0.147(7) Uani 0.581(6) 1 d PD A 1 H22A H 1.9961 0.8763 0.9033 0.221 Uiso 0.581(6) 1 calc PR A 1 H22B H 1.9471 0.9372 0.9850 0.221 Uiso 0.581(6) 1 calc PR A 1 H22C H 1.8987 0.9529 0.8981 0.221 Uiso 0.581(6) 1 calc PR A 1 C23 C 1.6721(10) 0.8024(11) 0.9665(7) 0.101(5) Uani 0.581(6) 1 d PD A 1 H23A H 1.6194 0.8451 0.9451 0.152 Uiso 0.581(6) 1 calc PR A 1 H23B H 1.7267 0.8546 1.0225 0.152 Uiso 0.581(6) 1 calc PR A 1 H23C H 1.6148 0.7305 0.9704 0.152 Uiso 0.581(6) 1 calc PR A 1 C24 C 1.8447(15) 0.6480(12) 0.9237(12) 0.138(8) Uani 0.581(6) 1 d PD A 1 H24A H 1.7727 0.5833 0.9249 0.208 Uiso 0.581(6) 1 calc PR A 1 H24B H 1.9034 0.6884 0.9799 0.208 Uiso 0.581(6) 1 calc PR A 1 H24C H 1.8926 0.6146 0.8829 0.208 Uiso 0.581(6) 1 calc PR A 1 Si3A Si 1.7251(5) 0.7086(3) 0.89183(12) 0.0412(9) Uani 0.419(6) 1 d PD A 2 C22A C 1.6132(12) 0.5992(8) 0.9255(7) 0.097(5) Uani 0.419(6) 1 d PD A 2 H22D H 1.5241 0.6019 0.9114 0.145 Uiso 0.419(6) 1 calc PR A 2 H22E H 1.6408 0.6202 0.9865 0.145 Uiso 0.419(6) 1 calc PR A 2 H22F H 1.6161 0.5183 0.8961 0.145 Uiso 0.419(6) 1 calc PR A 2 C23A C 1.7205(12) 0.8604(6) 0.9585(7) 0.050(3) Uani 0.419(6) 1 d PD A 2 H23D H 1.7696 0.9213 0.9397 0.075 Uiso 0.419(6) 1 calc PR A 2 H23E H 1.7594 0.8777 1.0177 0.075 Uiso 0.419(6) 1 calc PR A 2 H23F H 1.6300 0.8609 0.9527 0.075 Uiso 0.419(6) 1 calc PR A 2 C24A C 1.8933(10) 0.7060(15) 0.9243(13) 0.116(9) Uani 0.419(6) 1 d PD A 2 H24D H 1.8967 0.6240 0.9006 0.174 Uiso 0.419(6) 1 calc PR A 2 H24E H 1.9194 0.7347 0.9860 0.174 Uiso 0.419(6) 1 calc PR A 2 H24F H 1.9527 0.7579 0.9036 0.174 Uiso 0.419(6) 1 calc PR A 2 N5 N 1.4077(2) 0.8038(2) 0.67533(17) 0.0317(6) Uani 1 1 d . . . Si4 Si 1.37709(8) 0.89213(9) 0.62047(6) 0.0347(2) Uani 1 1 d . A . C25 C 1.5316(3) 1.0147(3) 0.6366(2) 0.0410(8) Uani 1 1 d . . . H25A H 1.5538 1.0732 0.6943 0.061 Uiso 1 1 calc R A . H25B H 1.5188 1.0545 0.5964 0.061 Uiso 1 1 calc R . . H25C H 1.6025 0.9801 0.6276 0.061 Uiso 1 1 calc R . . C26 C 1.2603(4) 0.9758(4) 0.6579(3) 0.0537(10) Uani 1 1 d . . . H26A H 1.1731 0.9190 0.6445 0.081 Uiso 1 1 calc R A . H26B H 1.2579 1.0331 0.6296 0.081 Uiso 1 1 calc R . . H26C H 1.2892 1.0189 0.7190 0.081 Uiso 1 1 calc R . . C27 C 1.3080(4) 0.8080(4) 0.5051(2) 0.0485(9) Uani 1 1 d . . . H27A H 1.3632 0.7602 0.4822 0.073 Uiso 1 1 calc R A . H27B H 1.3045 0.8646 0.4764 0.073 Uiso 1 1 calc R . . H27C H 1.2200 0.7549 0.4961 0.073 Uiso 1 1 calc R . . Si5 Si 1.28428(8) 0.71320(9) 0.69958(6) 0.0387(2) Uani 1 1 d . A . C28 C 1.1549(4) 0.6058(3) 0.6044(3) 0.0523(10) Uani 1 1 d . . . H28A H 1.1093 0.6502 0.5793 0.078 Uiso 1 1 calc R A . H28B H 1.0928 0.5501 0.6210 0.078 Uiso 1 1 calc R . . H28C H 1.1949 0.5608 0.5630 0.078 Uiso 1 1 calc R . . C29 C 1.3481(4) 0.6228(5) 0.7552(4) 0.0772(16) Uani 1 1 d . . . H29A H 1.3769 0.5633 0.7157 0.116 Uiso 1 1 calc R A . H29B H 1.2790 0.5820 0.7766 0.116 Uiso 1 1 calc R . . H29C H 1.4216 0.6758 0.8024 0.116 Uiso 1 1 calc R . . C30 C 1.2013(4) 0.7978(4) 0.7756(2) 0.0528(10) Uani 1 1 d . . . H30A H 1.2666 0.8561 0.8258 0.079 Uiso 1 1 calc R A . H30B H 1.1395 0.7416 0.7919 0.079 Uiso 1 1 calc R . . H30C H 1.1548 0.8396 0.7485 0.079 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 Nd1 0.01773(8) 0.02893(9) 0.04397(11) 0.01217(7) 0.00576(7) 0.00746(6) N1 0.0302(14) 0.0339(14) 0.0320(14) 0.0113(12) 0.0088(11) 0.0115(12) N2 0.0209(12) 0.0291(13) 0.0471(17) 0.0109(12) 0.0081(12) 0.0087(11) N3 0.0258(13) 0.0271(13) 0.0422(16) 0.0079(12) 0.0067(12) 0.0074(11) C2 0.0241(15) 0.0339(17) 0.047(2) 0.0107(15) 0.0062(14) 0.0118(14) C4 0.0359(17) 0.0279(16) 0.0342(17) 0.0107(14) 0.0066(14) 0.0091(14) C5 0.0428(19) 0.0293(16) 0.0326(18) 0.0075(14) 0.0095(15) 0.0111(15) C6 0.0364(18) 0.0427(19) 0.0326(18) 0.0130(15) 0.0134(15) 0.0140(15) C7 0.053(2) 0.051(2) 0.0334(19) 0.0088(17) 0.0141(17) 0.0141(18) C8 0.057(2) 0.066(3) 0.065(3) 0.030(2) 0.033(2) 0.037(2) C9 0.045(2) 0.057(2) 0.039(2) 0.0112(18) 0.0191(17) 0.0102(18) C10 0.0236(16) 0.0325(18) 0.069(3) 0.0002(17) 0.0138(17) 0.0050(14) C11 0.0222(15) 0.0296(17) 0.059(2) 0.0084(16) 0.0123(15) 0.0103(13) C12 0.0320(17) 0.0375(18) 0.052(2) 0.0214(16) 0.0160(16) 0.0143(14) C13 0.039(2) 0.052(2) 0.049(2) 0.0201(18) 0.0089(17) 0.0087(17) C14 0.062(3) 0.057(2) 0.047(2) 0.0177(19) 0.024(2) 0.033(2) C15 0.039(2) 0.063(3) 0.080(3) 0.044(2) 0.018(2) 0.0133(19) Si1 0.0471(6) 0.0285(5) 0.0407(5) 0.0116(4) 0.0166(5) 0.0064(4) C16 0.086(3) 0.038(2) 0.069(3) 0.010(2) 0.041(3) 0.005(2) C17 0.040(2) 0.055(3) 0.077(3) 0.019(2) 0.012(2) 0.0010(19) C18 0.103(4) 0.060(3) 0.053(3) 0.028(2) 0.031(3) 0.023(3) N4 0.0397(16) 0.067(2) 0.0359(16) 0.0256(15) 0.0113(13) 0.0319(15) Si2 0.0371(5) 0.0446(6) 0.0475(6) 0.0287(5) 0.0078(4) 0.0124(4) C19 0.054(2) 0.059(3) 0.062(3) 0.018(2) 0.015(2) 0.033(2) C20 0.050(2) 0.047(2) 0.043(2) 0.0216(18) 0.0021(18) 0.0064(18) C21 0.084(4) 0.086(4) 0.102(4) 0.073(3) 0.000(3) 0.002(3) Si3 0.0460(14) 0.087(2) 0.0343(11) 0.0329(12) 0.0173(9) 0.0374(14) C22 0.115(10) 0.192(14) 0.063(6) 0.053(8) -0.038(6) -0.055(9) C23 0.125(12) 0.177(14) 0.058(6) 0.057(9) 0.045(7) 0.111(11) C24 0.211(18) 0.146(14) 0.069(9) 0.025(10) -0.026(12) 0.123(13) Si3A 0.058(2) 0.0461(19) 0.0324(14) 0.0219(12) 0.0158(13) 0.0258(17) C22A 0.185(16) 0.050(7) 0.050(7) 0.028(6) 0.033(8) 0.010(8) C23A 0.065(7) 0.047(6) 0.033(6) 0.008(4) 0.007(5) 0.018(5) C24A 0.105(12) 0.20(2) 0.042(8) -0.003(12) -0.016(8) 0.126(16) N5 0.0205(12) 0.0409(15) 0.0385(15) 0.0199(13) 0.0093(11) 0.0092(11) Si4 0.0259(4) 0.0470(5) 0.0414(5) 0.0245(4) 0.0115(4) 0.0161(4) C25 0.0389(19) 0.045(2) 0.050(2) 0.0257(17) 0.0151(16) 0.0173(16) C26 0.045(2) 0.076(3) 0.066(3) 0.041(2) 0.022(2) 0.039(2) C27 0.039(2) 0.069(3) 0.044(2) 0.030(2) 0.0089(17) 0.0147(19) Si5 0.0210(4) 0.0536(6) 0.0507(6) 0.0308(5) 0.0110(4) 0.0103(4) C28 0.039(2) 0.045(2) 0.062(3) 0.0133(19) 0.0106(19) 0.0018(17) C29 0.040(2) 0.113(4) 0.130(4) 0.100(4) 0.038(3) 0.030(2) C30 0.0330(19) 0.079(3) 0.047(2) 0.026(2) 0.0180(17) 0.0103(19) _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 Nd1 N2 2.248(3) . ? Nd1 N5 2.352(2) . ? Nd1 N4 2.372(2) . ? Nd1 C2 2.648(3) . ? Nd1 C11 2.859(3) . ? Nd1 Si2 3.3530(10) . ? Nd1 Si4 3.4658(9) . ? N1 C2 1.363(4) . ? N1 C5 1.384(4) . ? N1 C6 1.494(4) . ? N2 C11 1.458(4) . ? N2 C12 1.473(4) . ? N3 C2 1.363(4) . ? N3 C4 1.397(4) . ? N3 C10 1.469(4) . ? C4 C5 1.349(4) . ? C4 Si1 1.872(3) . ? C6 C9 1.515(5) . ? C6 C7 1.524(5) . ? C6 C8 1.524(5) . ? C10 C11 1.525(4) . ? C12 C13 1.521(5) . ? C12 C14 1.537(5) . ? C12 C15 1.541(5) . ? Si1 C17 1.852(4) . ? Si1 C18 1.856(4) . ? Si1 C16 1.860(4) . ? N4 Si3A 1.7087(10) . ? N4 Si3 1.7136(10) . ? N4 Si2 1.719(3) . ? Si2 C21 1.873(4) . ? Si2 C19 1.874(4) . ? Si2 C20 1.885(4) . ? Si3 C24 1.873(5) . ? Si3 C23 1.884(7) . ? Si3 C22 1.896(7) . ? Si3A C24A 1.856(8) . ? Si3A C22A 1.877(7) . ? Si3A C23A 1.885(7) . ? N5 Si4 1.713(3) . ? N5 Si5 1.716(3) . ? Si4 C27 1.868(4) . ? Si4 C25 1.888(4) . ? Si4 C26 1.889(4) . ? Si5 C28 1.874(4) . ? Si5 C29 1.878(4) . ? Si5 C30 1.884(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 N2 Nd1 N5 120.38(9) . . ? N2 Nd1 N4 105.13(9) . . ? N5 Nd1 N4 122.01(10) . . ? N2 Nd1 C2 81.59(10) . . ? N5 Nd1 C2 112.92(9) . . ? N4 Nd1 C2 107.20(10) . . ? N2 Nd1 C11 30.29(10) . . ? N5 Nd1 C11 148.88(10) . . ? N4 Nd1 C11 86.03(10) . . ? C2 Nd1 C11 64.70(9) . . ? N2 Nd1 Si2 90.31(7) . . ? N5 Nd1 Si2 113.25(7) . . ? N4 Nd1 Si2 28.99(5) . . ? C2 Nd1 Si2 130.40(7) . . ? C11 Nd1 Si2 84.24(7) . . ? N2 Nd1 Si4 99.00(7) . . ? N5 Nd1 Si4 26.36(6) . . ? N4 Nd1 Si4 148.25(7) . . ? C2 Nd1 Si4 96.37(7) . . ? C11 Nd1 Si4 123.90(8) . . ? Si2 Nd1 Si4 133.21(2) . . ? C2 N1 C5 110.8(3) . . ? C2 N1 C6 127.1(3) . . ? C5 N1 C6 122.0(3) . . ? C11 N2 C12 115.6(3) . . ? C11 N2 Nd1 98.7(2) . . ? C12 N2 Nd1 144.7(2) . . ? C2 N3 C4 113.0(3) . . ? C2 N3 C10 126.4(3) . . ? C4 N3 C10 120.4(3) . . ? N1 C2 N3 103.2(3) . . ? N1 C2 Nd1 136.2(2) . . ? N3 C2 Nd1 118.1(2) . . ? C5 C4 N3 104.1(3) . . ? C5 C4 Si1 126.9(2) . . ? N3 C4 Si1 128.7(2) . . ? C4 C5 N1 108.8(3) . . ? N1 C6 C9 110.1(3) . . ? N1 C6 C7 108.0(3) . . ? C9 C6 C7 110.1(3) . . ? N1 C6 C8 108.8(3) . . ? C9 C6 C8 109.0(3) . . ? C7 C6 C8 110.9(3) . . ? N3 C10 C11 115.4(3) . . ? N2 C11 C10 118.0(3) . . ? N2 C11 Nd1 51.03(15) . . ? C10 C11 Nd1 112.27(19) . . ? N2 C12 C13 107.3(3) . . ? N2 C12 C14 111.7(3) . . ? C13 C12 C14 108.6(3) . . ? N2 C12 C15 113.2(3) . . ? C13 C12 C15 107.9(3) . . ? C14 C12 C15 108.0(3) . . ? C17 Si1 C18 110.2(2) . . ? C17 Si1 C16 109.1(2) . . ? C18 Si1 C16 111.0(2) . . ? C17 Si1 C4 112.87(17) . . ? C18 Si1 C4 108.60(19) . . ? C16 Si1 C4 105.02(17) . . ? Si3A N4 Si3 24.67(10) . . ? Si3A N4 Si2 115.6(2) . . ? Si3 N4 Si2 127.33(19) . . ? Si3A N4 Nd1 134.48(18) . . ? Si3 N4 Nd1 121.59(19) . . ? Si2 N4 Nd1 109.03(7) . . ? N4 Si2 C21 116.7(2) . . ? N4 Si2 C19 112.46(17) . . ? C21 Si2 C19 106.3(2) . . ? N4 Si2 C20 109.08(15) . . ? C21 Si2 C20 105.1(2) . . ? C19 Si2 C20 106.53(19) . . ? N4 Si2 Nd1 41.97(7) . . ? C21 Si2 Nd1 139.3(2) . . ? C19 Si2 Nd1 114.01(14) . . ? C20 Si2 Nd1 68.71(12) . . ? N4 Si3 C24 112.5(7) . . ? N4 Si3 C23 111.0(4) . . ? C24 Si3 C23 106.1(5) . . ? N4 Si3 C22 116.6(4) . . ? C24 Si3 C22 105.6(5) . . ? C23 Si3 C22 104.3(5) . . ? N4 Si3A C24A 110.5(7) . . ? N4 Si3A C22A 119.5(5) . . ? C24A Si3A C22A 108.0(5) . . ? N4 Si3A C23A 106.5(4) . . ? C24A Si3A C23A 106.0(5) . . ? C22A Si3A C23A 105.2(4) . . ? Si4 N5 Si5 121.25(15) . . ? Si4 N5 Nd1 116.08(12) . . ? Si5 N5 Nd1 122.58(13) . . ? N5 Si4 C27 113.63(16) . . ? N5 Si4 C25 109.60(14) . . ? C27 Si4 C25 109.32(17) . . ? N5 Si4 C26 114.35(15) . . ? C27 Si4 C26 105.63(18) . . ? C25 Si4 C26 103.76(18) . . ? N5 Si4 Nd1 37.56(8) . . ? C27 Si4 Nd1 118.62(13) . . ? C25 Si4 Nd1 73.36(11) . . ? C26 Si4 Nd1 134.21(13) . . ? N5 Si5 C28 112.98(16) . . ? N5 Si5 C29 111.00(15) . . ? C28 Si5 C29 107.5(2) . . ? N5 Si5 C30 113.69(16) . . ? C28 Si5 C30 107.28(18) . . ? C29 Si5 C30 103.9(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.534 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.093 #===end data_ceimsn_4 _database_code_depnum_ccdc_archive 'CCDC 280859' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H116 Ce2 I2 N8 Si6' _chemical_formula_sum 'C58 H116 Ce2 I2 N8 Si6' _chemical_formula_weight 1628.17 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7912(12) _cell_length_b 14.8947(15) _cell_length_c 22.118(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.838(2) _cell_angle_gamma 90.00 _cell_volume 3864.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7639 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 2.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.692 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32135 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8860 _reflns_number_gt 6128 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0725P)^2^+24.7871P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, Me from difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8860 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.91835(3) 0.64232(3) 0.533021(17) 0.02564(12) Uani 1 1 d . . . I1 I 0.83808(5) 0.45478(4) 0.47466(3) 0.04591(17) Uani 1 1 d . . . N1 N 0.6093(5) 0.7209(4) 0.5199(3) 0.0307(13) Uani 1 1 d . . . N2 N 0.9641(5) 0.7365(4) 0.4603(3) 0.0324(14) Uani 1 1 d . . . N3 N 0.6991(5) 0.7661(4) 0.4464(3) 0.0304(13) Uani 1 1 d . . . C2 C 0.7073(6) 0.7065(5) 0.4931(3) 0.0303(15) Uani 1 1 d . . . C4 C 0.6005(6) 0.8186(5) 0.4436(3) 0.0342(16) Uani 1 1 d . . . C5 C 0.5455(7) 0.7887(5) 0.4908(4) 0.0359(17) Uani 1 1 d . . . H5A H 0.4750 0.8109 0.5019 0.043 Uiso 1 1 calc R . . C6 C 0.5707(7) 0.6704(5) 0.5725(4) 0.0382(18) Uani 1 1 d . . . C7 C 0.4561(7) 0.6268(7) 0.5508(5) 0.054(2) Uani 1 1 d . . . H7A H 0.4671 0.5822 0.5194 0.081 Uiso 1 1 calc R . . H7B H 0.4027 0.6730 0.5339 0.081 Uiso 1 1 calc R . . H7C H 0.4251 0.5974 0.5852 0.081 Uiso 1 1 calc R . . C8 C 0.5588(10) 0.7359(7) 0.6238(4) 0.064(3) Uani 1 1 d . . . H8A H 0.6337 0.7610 0.6378 0.095 Uiso 1 1 calc R . . H8B H 0.5280 0.7045 0.6575 0.095 Uiso 1 1 calc R . . H8C H 0.5070 0.7845 0.6094 0.095 Uiso 1 1 calc R . . C9 C 0.6579(7) 0.5973(6) 0.5922(4) 0.048(2) Uani 1 1 d . . . H9A H 0.7318 0.6251 0.6047 0.072 Uiso 1 1 calc R . . H9B H 0.6654 0.5564 0.5581 0.072 Uiso 1 1 calc R . . H9C H 0.6322 0.5635 0.6263 0.072 Uiso 1 1 calc R . . C10 C 0.7750(7) 0.7718(5) 0.3978(3) 0.0386(18) Uani 1 1 d . . . H10A H 0.7983 0.8351 0.3934 0.046 Uiso 1 1 calc R . . H10B H 0.7321 0.7532 0.3590 0.046 Uiso 1 1 calc R . . C11 C 0.8825(7) 0.7132(5) 0.4092(3) 0.0331(16) Uani 1 1 d . . . H11A H 0.8578 0.6505 0.4149 0.040 Uiso 1 1 calc R . . H11B H 0.9226 0.7146 0.3720 0.040 Uiso 1 1 calc R . . C12 C 1.0583(7) 0.7960(6) 0.4472(4) 0.043(2) Uani 1 1 d . . . C13 C 1.0174(11) 0.8862(7) 0.4188(6) 0.077(4) Uani 1 1 d . . . H13A H 0.9700 0.9171 0.4462 0.115 Uiso 1 1 calc R . . H13B H 0.9725 0.8752 0.3797 0.115 Uiso 1 1 calc R . . H13C H 1.0835 0.9236 0.4124 0.115 Uiso 1 1 calc R . . C14 C 1.1326(8) 0.7498(7) 0.4022(4) 0.057(3) Uani 1 1 d . . . H14A H 1.1606 0.6922 0.4192 0.086 Uiso 1 1 calc R . . H14B H 1.1975 0.7885 0.3958 0.086 Uiso 1 1 calc R . . H14C H 1.0867 0.7396 0.3634 0.086 Uiso 1 1 calc R . . C15 C 1.1291(9) 0.8135(7) 0.5058(5) 0.062(3) Uani 1 1 d . . . H15A H 1.0862 0.8513 0.5318 0.094 Uiso 1 1 calc R . . H15B H 1.1994 0.8444 0.4978 0.094 Uiso 1 1 calc R . . H15C H 1.1481 0.7564 0.5264 0.094 Uiso 1 1 calc R . . Si1 Si 0.55411(19) 0.91055(15) 0.38811(10) 0.0371(5) Uani 1 1 d . . . C16 C 0.4135(8) 0.9496(7) 0.4080(5) 0.062(3) Uani 1 1 d . . . H16A H 0.3826 0.9942 0.3782 0.093 Uiso 1 1 calc R . . H16B H 0.4222 0.9767 0.4486 0.093 Uiso 1 1 calc R . . H16C H 0.3611 0.8984 0.4078 0.093 Uiso 1 1 calc R . . C17 C 0.5424(9) 0.8689(6) 0.3086(4) 0.054(2) Uani 1 1 d . . . H17A H 0.5039 0.9141 0.2815 0.081 Uiso 1 1 calc R . . H17B H 0.4983 0.8130 0.3057 0.081 Uiso 1 1 calc R . . H17C H 0.6188 0.8576 0.2965 0.081 Uiso 1 1 calc R . . C18 C 0.6574(8) 1.0044(6) 0.3993(4) 0.050(2) Uani 1 1 d . . . H18A H 0.6252 1.0579 0.3783 0.076 Uiso 1 1 calc R . . H18B H 0.7284 0.9877 0.3827 0.076 Uiso 1 1 calc R . . H18C H 0.6731 1.0171 0.4428 0.076 Uiso 1 1 calc R . . N4 N 0.9390(5) 0.6911(4) 0.6352(3) 0.0323(14) Uani 1 1 d . . . Si2 Si 0.9347(2) 0.80309(15) 0.65138(10) 0.0408(5) Uani 1 1 d . . . C19 C 0.8575(10) 0.8314(7) 0.7193(5) 0.065(3) Uani 1 1 d . . . H19A H 0.7791 0.8089 0.7129 0.098 Uiso 1 1 calc R . . H19B H 0.8565 0.8966 0.7247 0.098 Uiso 1 1 calc R . . H19C H 0.8968 0.8033 0.7557 0.098 Uiso 1 1 calc R . . C20 C 1.0794(9) 0.8538(7) 0.6690(5) 0.067(3) Uani 1 1 d . . . H20A H 1.1319 0.8279 0.6422 0.101 Uiso 1 1 calc R . . H20B H 1.1073 0.8413 0.7114 0.101 Uiso 1 1 calc R . . H20C H 1.0747 0.9189 0.6627 0.101 Uiso 1 1 calc R . . C21 C 0.8577(8) 0.8644(5) 0.5865(4) 0.049(2) Uani 1 1 d . . . H21A H 0.7775 0.8458 0.5817 0.073 Uiso 1 1 calc R . . H21B H 0.8925 0.8506 0.5492 0.073 Uiso 1 1 calc R . . H21C H 0.8623 0.9291 0.5942 0.073 Uiso 1 1 calc R . . Si3 Si 0.9613(2) 0.60911(15) 0.68935(9) 0.0375(5) Uani 1 1 d . . . C22 C 0.8511(9) 0.6057(7) 0.7453(4) 0.056(3) Uani 1 1 d . . . H22A H 0.8673 0.5553 0.7734 0.084 Uiso 1 1 calc R . . H22B H 0.7753 0.5981 0.7234 0.084 Uiso 1 1 calc R . . H22C H 0.8535 0.6621 0.7683 0.084 Uiso 1 1 calc R . . C23 C 1.1024(9) 0.6192(8) 0.7342(5) 0.065(3) Uani 1 1 d . . . H23A H 1.1143 0.5678 0.7618 0.097 Uiso 1 1 calc R . . H23B H 1.1050 0.6749 0.7580 0.097 Uiso 1 1 calc R . . H23C H 1.1624 0.6204 0.7066 0.097 Uiso 1 1 calc R . . C24 C 0.9541(9) 0.4971(6) 0.6524(4) 0.048(2) Uani 1 1 d . . . H24A H 0.9609 0.4502 0.6837 0.072 Uiso 1 1 calc R . . H24B H 1.0165 0.4912 0.6267 0.072 Uiso 1 1 calc R . . H24C H 0.8810 0.4907 0.6275 0.072 Uiso 1 1 calc R . . C25 C 0.3311(9) 0.4568(8) 0.6835(6) 0.075(3) Uani 1 1 d . . . H25A H 0.3293 0.4982 0.7178 0.112 Uiso 1 1 calc R . . H25B H 0.2718 0.4111 0.6853 0.112 Uiso 1 1 calc R . . H25C H 0.3174 0.4903 0.6453 0.112 Uiso 1 1 calc R . . C26 C 0.4432(9) 0.4132(6) 0.6865(5) 0.056(2) Uani 1 1 d . . . C27 C 0.5048(9) 0.3930(7) 0.7409(5) 0.059(3) Uani 1 1 d . . . H27A H 0.4726 0.4046 0.7778 0.071 Uiso 1 1 calc R . . C28 C 0.6123(11) 0.3564(9) 0.7429(6) 0.081(4) Uani 1 1 d . . . H28A H 0.6537 0.3440 0.7811 0.098 Uiso 1 1 calc R . . C29 C 0.6599(10) 0.3377(8) 0.6909(5) 0.072(3) Uani 1 1 d . . . H29A H 0.7341 0.3123 0.6925 0.086 Uiso 1 1 calc R . . C30 C 0.5985(10) 0.3562(7) 0.6355(5) 0.065(3) Uani 1 1 d . . . H30A H 0.6311 0.3438 0.5989 0.078 Uiso 1 1 calc R . . C31 C 0.4936(9) 0.3913(6) 0.6332(5) 0.054(2) Uani 1 1 d . . . H31A H 0.4521 0.4017 0.5947 0.065 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 Ce1 0.0325(2) 0.02171(19) 0.02390(19) -0.00156(16) 0.00838(14) -0.00704(16) I1 0.0399(3) 0.0409(3) 0.0570(4) -0.0043(3) 0.0051(3) -0.0003(2) N1 0.029(3) 0.031(3) 0.033(3) 0.004(3) 0.006(3) -0.008(3) N2 0.046(4) 0.025(3) 0.029(3) 0.001(2) 0.015(3) -0.011(3) N3 0.031(3) 0.026(3) 0.036(3) -0.001(3) 0.010(3) -0.004(2) C2 0.040(4) 0.021(3) 0.031(4) 0.003(3) 0.013(3) -0.007(3) C4 0.036(4) 0.030(4) 0.037(4) 0.003(3) 0.006(3) -0.006(3) C5 0.034(4) 0.031(4) 0.041(4) 0.001(3) 0.002(3) -0.004(3) C6 0.040(4) 0.037(4) 0.039(4) 0.009(3) 0.014(3) -0.007(3) C7 0.034(4) 0.060(6) 0.070(6) 0.021(5) 0.009(4) -0.008(4) C8 0.090(8) 0.054(6) 0.053(6) 0.008(5) 0.035(5) 0.000(5) C9 0.043(5) 0.050(5) 0.054(5) 0.022(4) 0.015(4) -0.009(4) C10 0.050(5) 0.037(4) 0.031(4) 0.008(3) 0.013(3) 0.005(4) C11 0.047(4) 0.026(4) 0.029(4) 0.004(3) 0.013(3) -0.003(3) C12 0.054(5) 0.035(4) 0.041(4) 0.002(3) 0.016(4) -0.020(4) C13 0.108(10) 0.033(5) 0.094(9) 0.016(5) 0.030(7) -0.028(6) C14 0.053(5) 0.072(7) 0.052(5) -0.006(5) 0.028(4) -0.024(5) C15 0.069(7) 0.057(6) 0.065(6) -0.013(5) 0.023(5) -0.041(5) Si1 0.0407(12) 0.0294(11) 0.0411(12) 0.0063(9) 0.0043(10) -0.0014(9) C16 0.056(6) 0.062(7) 0.070(7) 0.020(5) 0.019(5) 0.012(5) C17 0.067(6) 0.049(5) 0.042(5) 0.005(4) -0.009(4) -0.002(5) C18 0.060(6) 0.031(4) 0.058(6) 0.011(4) -0.001(5) -0.008(4) N4 0.041(4) 0.032(3) 0.025(3) -0.006(2) 0.011(3) -0.001(3) Si2 0.0560(14) 0.0295(11) 0.0382(12) -0.0127(9) 0.0117(11) -0.0081(10) C19 0.103(9) 0.043(5) 0.053(6) -0.025(5) 0.025(6) -0.005(5) C20 0.075(7) 0.062(7) 0.062(6) -0.025(5) -0.003(5) -0.027(6) C21 0.072(6) 0.016(4) 0.061(5) -0.008(4) 0.014(5) -0.009(4) Si3 0.0522(14) 0.0359(11) 0.0253(10) -0.0023(9) 0.0087(9) 0.0073(10) C22 0.084(7) 0.052(5) 0.037(5) 0.006(4) 0.024(5) 0.014(5) C23 0.076(7) 0.066(7) 0.049(6) -0.009(5) -0.009(5) 0.019(6) C24 0.076(6) 0.034(4) 0.038(4) 0.005(4) 0.018(4) 0.004(4) C25 0.058(7) 0.066(7) 0.100(9) 0.017(7) 0.010(6) -0.015(6) C26 0.058(6) 0.035(5) 0.074(7) 0.003(5) 0.000(5) -0.010(4) C27 0.071(7) 0.056(6) 0.050(6) -0.008(5) -0.001(5) 0.003(5) C28 0.083(9) 0.095(9) 0.065(7) -0.030(7) 0.002(6) 0.018(7) C29 0.060(7) 0.079(8) 0.076(8) -0.022(6) 0.002(6) 0.016(6) C30 0.064(7) 0.060(7) 0.072(7) -0.013(6) 0.012(6) -0.003(5) C31 0.070(7) 0.041(5) 0.053(6) -0.008(4) 0.008(5) -0.020(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce1 N2 2.241(6) . ? Ce1 N4 2.364(6) . ? Ce1 C2 2.728(8) . ? Ce1 C11 2.925(7) . ? Ce1 I1 3.1806(7) . ? Ce1 I1 3.2354(7) 3_766 ? Ce1 Si3 3.479(2) . ? I1 Ce1 3.2354(7) 3_766 ? N1 C2 1.367(9) . ? N1 C5 1.378(10) . ? N1 C6 1.495(9) . ? N2 C11 1.449(10) . ? N2 C12 1.473(9) . ? N3 C2 1.357(9) . ? N3 C4 1.397(10) . ? N3 C10 1.469(9) . ? C4 C5 1.359(11) . ? C4 Si1 1.882(8) . ? C6 C8 1.515(13) . ? C6 C9 1.530(12) . ? C6 C7 1.531(12) . ? C10 C11 1.538(11) . ? C12 C15 1.492(13) . ? C12 C13 1.539(13) . ? C12 C14 1.552(12) . ? Si1 C16 1.852(10) . ? Si1 C18 1.854(9) . ? Si1 C17 1.858(9) . ? N4 Si2 1.707(6) . ? N4 Si3 1.712(7) . ? Si2 C21 1.859(10) . ? Si2 C20 1.870(10) . ? Si2 C19 1.881(9) . ? Si3 C23 1.855(10) . ? Si3 C24 1.856(9) . ? Si3 C22 1.884(9) . ? C25 C26 1.469(15) . ? C26 C27 1.374(14) . ? C26 C31 1.412(14) . ? C27 C28 1.377(15) . ? C28 C29 1.359(16) . ? C29 C30 1.386(16) . ? C30 C31 1.338(15) . ? 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 Ce1 N4 119.0(2) . . ? N2 Ce1 C2 80.0(2) . . ? N4 Ce1 C2 101.7(2) . . ? N2 Ce1 C11 28.9(2) . . ? N4 Ce1 C11 140.8(2) . . ? C2 Ce1 C11 62.0(2) . . ? N2 Ce1 I1 109.97(15) . . ? N4 Ce1 I1 130.98(15) . . ? C2 Ce1 I1 87.28(15) . . ? C11 Ce1 I1 85.89(15) . . ? N2 Ce1 I1 87.84(17) . 3_766 ? N4 Ce1 I1 100.50(15) . 3_766 ? C2 Ce1 I1 157.70(15) . 3_766 ? C11 Ce1 I1 99.02(15) . 3_766 ? I1 Ce1 I1 79.350(18) . 3_766 ? N2 Ce1 Si3 141.38(16) . . ? N4 Ce1 Si3 26.19(16) . . ? C2 Ce1 Si3 114.03(15) . . ? C11 Ce1 Si3 167.01(15) . . ? I1 Ce1 Si3 106.60(4) . . ? I1 Ce1 Si3 87.05(4) 3_766 . ? Ce1 I1 Ce1 100.650(18) . 3_766 ? C2 N1 C5 111.0(6) . . ? C2 N1 C6 126.5(6) . . ? C5 N1 C6 122.5(6) . . ? C11 N2 C12 116.4(6) . . ? C11 N2 Ce1 102.7(4) . . ? C12 N2 Ce1 139.4(5) . . ? C2 N3 C4 113.3(6) . . ? C2 N3 C10 126.3(6) . . ? C4 N3 C10 120.0(6) . . ? N3 C2 N1 103.2(6) . . ? N3 C2 Ce1 117.9(5) . . ? N1 C2 Ce1 134.3(5) . . ? C5 C4 N3 104.0(7) . . ? C5 C4 Si1 127.5(6) . . ? N3 C4 Si1 128.5(5) . . ? C4 C5 N1 108.6(7) . . ? N1 C6 C8 108.6(7) . . ? N1 C6 C9 109.3(6) . . ? C8 C6 C9 110.8(8) . . ? N1 C6 C7 107.4(7) . . ? C8 C6 C7 111.2(8) . . ? C9 C6 C7 109.5(7) . . ? N3 C10 C11 113.6(6) . . ? N2 C11 C10 117.6(6) . . ? N2 C11 Ce1 48.4(3) . . ? C10 C11 Ce1 113.3(4) . . ? N2 C12 C15 107.5(6) . . ? N2 C12 C13 113.2(8) . . ? C15 C12 C13 109.1(8) . . ? N2 C12 C14 110.2(7) . . ? C15 C12 C14 109.4(8) . . ? C13 C12 C14 107.4(8) . . ? C16 Si1 C18 108.9(5) . . ? C16 Si1 C17 110.3(5) . . ? C18 Si1 C17 111.3(5) . . ? C16 Si1 C4 106.3(4) . . ? C18 Si1 C4 108.6(4) . . ? C17 Si1 C4 111.3(4) . . ? Si2 N4 Si3 123.8(4) . . ? Si2 N4 Ce1 119.9(3) . . ? Si3 N4 Ce1 116.3(3) . . ? N4 Si2 C21 109.9(3) . . ? N4 Si2 C20 113.1(4) . . ? C21 Si2 C20 109.0(5) . . ? N4 Si2 C19 114.4(4) . . ? C21 Si2 C19 105.6(5) . . ? C20 Si2 C19 104.4(5) . . ? N4 Si3 C23 112.4(4) . . ? N4 Si3 C24 109.7(3) . . ? C23 Si3 C24 107.9(5) . . ? N4 Si3 C22 114.3(4) . . ? C23 Si3 C22 106.9(5) . . ? C24 Si3 C22 105.2(4) . . ? N4 Si3 Ce1 37.5(2) . . ? C23 Si3 Ce1 123.5(4) . . ? C24 Si3 Ce1 72.2(3) . . ? C22 Si3 Ce1 128.1(3) . . ? C27 C26 C31 116.8(10) . . ? C27 C26 C25 122.0(11) . . ? C31 C26 C25 121.2(10) . . ? C26 C27 C28 121.2(10) . . ? C29 C28 C27 120.9(12) . . ? C28 C29 C30 118.9(11) . . ? C31 C30 C29 120.7(11) . . ? C30 C31 C26 121.6(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.826 _refine_diff_density_min -2.133 _refine_diff_density_rms 0.174 #===end data_nd2daz_5 _database_code_depnum_ccdc_archive 'CCDC 280860' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H116 N14 Nd2 Si6' _chemical_formula_sum 'C58 H116 N14 Nd2 Si6' _chemical_formula_weight 1466.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.2143(6) _cell_length_b 15.5058(9) _cell_length_c 22.3542(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.695(2) _cell_angle_gamma 90.00 _cell_volume 3852.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19674 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4729 _exptl_absorpt_correction_T_max 0.7480 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43739 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8805 _reflns_number_gt 7138 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.0378P)^2^+3.6505P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8805 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.394008(13) 0.837832(9) 0.546736(6) 0.02542(5) Uani 1 1 d . . . N1 N 0.0733(2) 0.76288(16) 0.52309(12) 0.0317(5) Uani 1 1 d . . . N2 N 0.4484(2) 0.75694(16) 0.47242(11) 0.0319(5) Uani 1 1 d . . . N3 N 0.1695(2) 0.72678(16) 0.45072(11) 0.0314(5) Uani 1 1 d . . . C2 C 0.1774(2) 0.77876(19) 0.50031(13) 0.0308(6) Uani 1 1 d . . . C4 C 0.0642(3) 0.6776(2) 0.44255(16) 0.0366(7) Uani 1 1 d . . . C5 C 0.0051(3) 0.7017(2) 0.48857(16) 0.0397(7) Uani 1 1 d . . . H5A H -0.0709 0.6803 0.4961 0.048 Uiso 1 1 calc R . . C6 C 0.0305(3) 0.8079(2) 0.57531(15) 0.0372(7) Uani 1 1 d . . . C7 C 0.1252(3) 0.8715(2) 0.60312(16) 0.0427(8) Uani 1 1 d . . . H7A H 0.1989 0.8403 0.6186 0.064 Uiso 1 1 calc R . . H7B H 0.0951 0.9024 0.6363 0.064 Uiso 1 1 calc R . . H7C H 0.1428 0.9129 0.5723 0.064 Uiso 1 1 calc R . . C8 C 0.0061(4) 0.7403(3) 0.62159(19) 0.0646(12) Uani 1 1 d . . . H8A H -0.0551 0.6998 0.6031 0.097 Uiso 1 1 calc R . . H8B H -0.0229 0.7687 0.6560 0.097 Uiso 1 1 calc R . . H8C H 0.0805 0.7089 0.6354 0.097 Uiso 1 1 calc R . . C9 C -0.0845(3) 0.8569(3) 0.55208(19) 0.0565(10) Uani 1 1 d . . . H9A H -0.1460 0.8162 0.5342 0.085 Uiso 1 1 calc R . . H9B H -0.0676 0.8988 0.5215 0.085 Uiso 1 1 calc R . . H9C H -0.1138 0.8873 0.5857 0.085 Uiso 1 1 calc R . . C10 C 0.2528(3) 0.7265(2) 0.40534(15) 0.0420(8) Uani 1 1 d . . . H10A H 0.2089 0.7458 0.3663 0.050 Uiso 1 1 calc R . . H10B H 0.2800 0.6666 0.4000 0.050 Uiso 1 1 calc R . . C11 C 0.3628(3) 0.7836(2) 0.42112(14) 0.0361(7) Uani 1 1 d . . . H11A H 0.4059 0.7870 0.3853 0.043 Uiso 1 1 calc R . . H11B H 0.3348 0.8425 0.4291 0.043 Uiso 1 1 calc R . . C12 C 0.5537(3) 0.7079(2) 0.45850(15) 0.0383(7) Uani 1 1 d . . . C13 C 0.6316(3) 0.7630(3) 0.42115(17) 0.0487(9) Uani 1 1 d . . . H13A H 0.6550 0.8165 0.4429 0.073 Uiso 1 1 calc R . . H13B H 0.5853 0.7768 0.3820 0.073 Uiso 1 1 calc R . . H13C H 0.7040 0.7307 0.4148 0.073 Uiso 1 1 calc R . . C14 C 0.5189(3) 0.6236(2) 0.4241(2) 0.0544(10) Uani 1 1 d . . . H14A H 0.4700 0.5880 0.4477 0.082 Uiso 1 1 calc R . . H14B H 0.5919 0.5921 0.4179 0.082 Uiso 1 1 calc R . . H14C H 0.4725 0.6372 0.3849 0.082 Uiso 1 1 calc R . . C15 C 0.6274(3) 0.6862(3) 0.51864(17) 0.0495(9) Uani 1 1 d . . . H15A H 0.5791 0.6509 0.5427 0.074 Uiso 1 1 calc R . . H15B H 0.6512 0.7397 0.5405 0.074 Uiso 1 1 calc R . . H15C H 0.6996 0.6542 0.5116 0.074 Uiso 1 1 calc R . . Si1 Si 0.02041(8) 0.59401(6) 0.38252(5) 0.0438(2) Uani 1 1 d . . . C16 C 0.0034(4) 0.6417(3) 0.3050(2) 0.0662(12) Uani 1 1 d . . . H16A H 0.0807 0.6654 0.2971 0.099 Uiso 1 1 calc R . . H16B H -0.0569 0.6878 0.3022 0.099 Uiso 1 1 calc R . . H16C H -0.0226 0.5969 0.2752 0.099 Uiso 1 1 calc R . . C17 C -0.1255(4) 0.5479(3) 0.3981(3) 0.0817(16) Uani 1 1 d . . . H17A H -0.1522 0.5039 0.3678 0.122 Uiso 1 1 calc R . . H17B H -0.1859 0.5939 0.3963 0.122 Uiso 1 1 calc R . . H17C H -0.1153 0.5217 0.4383 0.122 Uiso 1 1 calc R . . C18 C 0.1355(4) 0.5068(2) 0.3890(2) 0.0596(10) Uani 1 1 d . . . H18A H 0.2127 0.5306 0.3810 0.089 Uiso 1 1 calc R . . H18B H 0.1100 0.4613 0.3597 0.089 Uiso 1 1 calc R . . H18C H 0.1443 0.4827 0.4299 0.089 Uiso 1 1 calc R . . N4 N 0.4289(2) 0.79283(17) 0.64752(11) 0.0349(6) Uani 1 1 d . . . Si2 Si 0.42863(9) 0.68477(7) 0.66106(5) 0.0450(2) Uani 1 1 d . . . C19 C 0.3453(5) 0.6527(3) 0.7252(2) 0.0727(14) Uani 1 1 d . . . H19A H 0.3873 0.6047 0.7475 0.109 Uiso 1 1 calc R . . H19B H 0.2634 0.6348 0.7092 0.109 Uiso 1 1 calc R . . H19C H 0.3417 0.7019 0.7524 0.109 Uiso 1 1 calc R . . C20 C 0.5845(4) 0.6381(3) 0.6803(2) 0.0722(13) Uani 1 1 d . . . H20A H 0.5844 0.5958 0.7129 0.108 Uiso 1 1 calc R . . H20B H 0.6414 0.6844 0.6934 0.108 Uiso 1 1 calc R . . H20C H 0.6085 0.6098 0.6446 0.108 Uiso 1 1 calc R . . C21 C 0.3506(3) 0.6275(2) 0.59292(19) 0.0511(9) Uani 1 1 d . . . H21A H 0.3361 0.5673 0.6033 0.077 Uiso 1 1 calc R . . H21B H 0.4014 0.6293 0.5605 0.077 Uiso 1 1 calc R . . H21C H 0.2737 0.6559 0.5794 0.077 Uiso 1 1 calc R . . Si3 Si 0.45436(9) 0.87212(7) 0.70073(4) 0.0453(2) Uani 1 1 d . . . C22 C 0.3374(4) 0.8767(4) 0.75419(18) 0.0694(12) Uani 1 1 d . . . H22A H 0.3771 0.8870 0.7954 0.104 Uiso 1 1 calc R . . H22B H 0.2937 0.8219 0.7528 0.104 Uiso 1 1 calc R . . H22C H 0.2807 0.9237 0.7421 0.104 Uiso 1 1 calc R . . C23 C 0.6052(4) 0.8629(3) 0.74753(19) 0.0678(12) Uani 1 1 d . . . H23A H 0.5976 0.8760 0.7897 0.102 Uiso 1 1 calc R . . H23B H 0.6611 0.9038 0.7327 0.102 Uiso 1 1 calc R . . H23C H 0.6359 0.8041 0.7446 0.102 Uiso 1 1 calc R . . C24 C 0.4468(4) 0.9803(2) 0.66268(16) 0.0523(9) Uani 1 1 d . . . H24A H 0.4610 1.0257 0.6933 0.078 Uiso 1 1 calc R . . H24B H 0.3670 0.9881 0.6394 0.078 Uiso 1 1 calc R . . H24C H 0.5083 0.9835 0.6355 0.078 Uiso 1 1 calc R . . N5 N 0.3118(2) 0.98129(17) 0.50856(12) 0.0374(6) Uani 1 1 d . . . N6 N 0.36337(19) 1.03205(14) 0.48321(10) 0.0246(5) Uani 1 1 d . . . N7 N 0.4105(2) 1.08316(17) 0.45649(13) 0.0403(6) Uani 1 1 d . . . C25 C 0.1987(3) 0.9720(3) 0.33602(19) 0.0585(10) Uani 1 1 d . . . H25A H 0.2309 0.9795 0.3787 0.088 Uiso 1 1 calc R . . H25B H 0.1937 1.0282 0.3158 0.088 Uiso 1 1 calc R . . H25C H 0.2519 0.9339 0.3167 0.088 Uiso 1 1 calc R . . C26 C 0.0770(3) 0.9331(2) 0.33130(16) 0.0439(8) Uani 1 1 d . . . C27 C 0.0110(3) 0.9161(3) 0.27511(17) 0.0542(9) Uani 1 1 d . . . H27A H 0.0458 0.9273 0.2394 0.065 Uiso 1 1 calc R . . C28 C -0.1035(4) 0.8833(3) 0.2706(2) 0.0691(12) Uani 1 1 d . . . H28A H -0.1472 0.8725 0.2319 0.083 Uiso 1 1 calc R . . C29 C -0.1558(4) 0.8658(3) 0.3220(2) 0.0660(11) Uani 1 1 d . . . H29A H -0.2357 0.8442 0.3187 0.079 Uiso 1 1 calc R . . C30 C -0.0912(4) 0.8800(3) 0.37758(19) 0.0606(10) Uani 1 1 d . . . H30A H -0.1256 0.8667 0.4131 0.073 Uiso 1 1 calc R . . C31 C 0.0239(4) 0.9136(2) 0.38225(16) 0.0512(9) Uani 1 1 d . . . H31A H 0.0674 0.9236 0.4211 0.061 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 Nd1 0.02329(8) 0.02617(8) 0.02653(8) 0.00238(6) 0.00232(5) -0.00367(6) N1 0.0221(11) 0.0323(13) 0.0410(14) -0.0013(11) 0.0048(10) -0.0024(9) N2 0.0229(11) 0.0396(14) 0.0334(13) -0.0019(11) 0.0046(10) -0.0033(10) N3 0.0239(12) 0.0317(13) 0.0376(13) -0.0037(10) 0.0002(10) -0.0027(10) C2 0.0240(13) 0.0313(15) 0.0374(16) 0.0014(12) 0.0053(12) 0.0007(11) C4 0.0260(14) 0.0335(16) 0.0498(19) -0.0049(13) 0.0025(13) -0.0041(12) C5 0.0265(14) 0.0366(17) 0.056(2) -0.0043(15) 0.0039(14) -0.0083(13) C6 0.0269(15) 0.0435(17) 0.0425(17) -0.0036(14) 0.0093(13) -0.0005(13) C7 0.0316(16) 0.053(2) 0.0434(18) -0.0107(16) 0.0056(14) -0.0010(14) C8 0.080(3) 0.059(3) 0.062(3) -0.002(2) 0.037(2) -0.007(2) C9 0.0304(18) 0.072(3) 0.066(3) -0.024(2) 0.0027(17) 0.0088(16) C10 0.0327(16) 0.056(2) 0.0379(17) -0.0133(15) 0.0049(13) -0.0071(14) C11 0.0317(15) 0.0457(18) 0.0322(15) -0.0030(13) 0.0086(12) -0.0055(13) C12 0.0311(15) 0.0421(18) 0.0434(18) -0.0064(14) 0.0107(13) -0.0013(13) C13 0.0317(17) 0.067(2) 0.051(2) -0.0076(18) 0.0168(15) -0.0061(16) C14 0.043(2) 0.047(2) 0.075(3) -0.0156(19) 0.0155(18) -0.0004(16) C15 0.0292(16) 0.061(2) 0.059(2) 0.0057(18) 0.0075(15) 0.0075(15) Si1 0.0364(5) 0.0410(5) 0.0536(6) -0.0153(4) 0.0047(4) -0.0071(4) C16 0.066(3) 0.067(3) 0.059(3) -0.015(2) -0.014(2) -0.004(2) C17 0.051(2) 0.082(3) 0.117(4) -0.048(3) 0.027(3) -0.036(2) C18 0.071(3) 0.042(2) 0.065(3) -0.0141(18) 0.006(2) 0.0074(19) N4 0.0300(13) 0.0424(15) 0.0321(13) 0.0081(11) 0.0029(10) -0.0032(11) Si2 0.0405(5) 0.0483(5) 0.0477(5) 0.0232(4) 0.0109(4) 0.0058(4) C19 0.080(3) 0.073(3) 0.070(3) 0.036(2) 0.031(3) 0.002(2) C20 0.060(3) 0.088(3) 0.068(3) 0.032(2) 0.006(2) 0.029(2) C21 0.046(2) 0.0325(17) 0.077(3) 0.0096(17) 0.0177(18) -0.0017(15) Si3 0.0434(5) 0.0634(6) 0.0282(4) 0.0011(4) 0.0010(4) -0.0092(5) C22 0.069(3) 0.100(4) 0.043(2) -0.015(2) 0.018(2) -0.012(3) C23 0.058(3) 0.091(3) 0.050(2) 0.008(2) -0.0119(19) -0.014(2) C24 0.065(2) 0.050(2) 0.0415(19) -0.0119(16) 0.0046(17) -0.0060(18) N5 0.0308(13) 0.0333(13) 0.0478(15) 0.0087(12) 0.0042(11) 0.0003(11) N6 0.0183(10) 0.0238(11) 0.0310(12) 0.0002(9) 0.0002(9) 0.0010(9) N7 0.0302(13) 0.0367(14) 0.0539(17) 0.0054(13) 0.0049(12) -0.0093(11) C25 0.048(2) 0.070(3) 0.056(2) -0.013(2) 0.0030(18) 0.0016(19) C26 0.0418(18) 0.0403(18) 0.049(2) -0.0003(15) 0.0020(15) 0.0084(14) C27 0.053(2) 0.070(3) 0.0387(18) 0.0080(17) 0.0022(16) -0.0042(19) C28 0.060(3) 0.093(3) 0.051(2) 0.016(2) -0.006(2) -0.020(2) C29 0.056(2) 0.077(3) 0.064(3) 0.012(2) 0.007(2) -0.015(2) C30 0.071(3) 0.060(3) 0.054(2) 0.013(2) 0.019(2) -0.005(2) C31 0.067(2) 0.045(2) 0.0400(19) 0.0025(15) 0.0010(17) 0.0094(18) _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 Nd1 N2 2.231(2) . ? Nd1 N4 2.341(2) . ? Nd1 N5 2.513(3) . ? Nd1 N7 2.521(3) 3_676 ? Nd1 C2 2.672(3) . ? Nd1 C11 2.907(3) . ? Nd1 Si3 3.4592(9) . ? Nd1 Si2 3.4712(9) . ? N1 C2 1.357(4) . ? N1 C5 1.386(4) . ? N1 C6 1.493(4) . ? N2 C11 1.453(4) . ? N2 C12 1.473(4) . ? N3 C2 1.364(4) . ? N3 C4 1.397(4) . ? N3 C10 1.468(4) . ? C4 C5 1.350(5) . ? C4 Si1 1.883(3) . ? C6 C7 1.521(5) . ? C6 C8 1.523(5) . ? C6 C9 1.527(5) . ? C10 C11 1.521(4) . ? C12 C15 1.518(5) . ? C12 C14 1.539(5) . ? C12 C13 1.545(5) . ? Si1 C17 1.861(4) . ? Si1 C18 1.861(4) . ? Si1 C16 1.869(5) . ? N4 Si2 1.703(3) . ? N4 Si3 1.708(3) . ? Si2 C21 1.876(4) . ? Si2 C19 1.881(4) . ? Si2 C20 1.887(4) . ? Si3 C23 1.872(4) . ? Si3 C24 1.877(4) . ? Si3 C22 1.891(4) . ? N5 N6 1.168(3) . ? N6 N7 1.162(3) . ? N7 Nd1 2.521(2) 3_676 ? C25 C26 1.483(5) . ? C26 C31 1.387(5) . ? C26 C27 1.395(5) . ? C27 C28 1.372(6) . ? C28 C29 1.385(6) . ? C29 C30 1.370(6) . ? C30 C31 1.383(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Nd1 N4 121.47(9) . . ? N2 Nd1 N5 111.67(9) . . ? N4 Nd1 N5 126.66(9) . . ? N2 Nd1 N7 85.79(9) . 3_676 ? N4 Nd1 N7 97.95(9) . 3_676 ? N5 Nd1 N7 80.86(9) . 3_676 ? N2 Nd1 C2 80.96(9) . . ? N4 Nd1 C2 107.33(9) . . ? N5 Nd1 C2 84.16(9) . . ? N7 Nd1 C2 154.72(9) 3_676 . ? N2 Nd1 C11 29.25(9) . . ? N4 Nd1 C11 145.73(10) . . ? N5 Nd1 C11 86.38(9) . . ? N7 Nd1 C11 96.06(9) 3_676 . ? C2 Nd1 C11 62.63(9) . . ? N2 Nd1 Si3 142.27(7) . . ? N4 Nd1 Si3 26.21(7) . . ? N5 Nd1 Si3 102.47(7) . . ? N7 Nd1 Si3 84.19(7) 3_676 . ? C2 Nd1 Si3 119.06(7) . . ? C11 Nd1 Si3 171.05(7) . . ? N2 Nd1 Si2 98.57(7) . . ? N4 Nd1 Si2 25.82(7) . . ? N5 Nd1 Si2 148.75(7) . . ? N7 Nd1 Si2 109.96(7) 3_676 . ? C2 Nd1 Si2 93.31(7) . . ? C11 Nd1 Si2 120.03(7) . . ? Si3 Nd1 Si2 52.03(3) . . ? C2 N1 C5 110.7(3) . . ? C2 N1 C6 126.3(2) . . ? C5 N1 C6 122.9(2) . . ? C11 N2 C12 116.3(2) . . ? C11 N2 Nd1 102.16(18) . . ? C12 N2 Nd1 138.99(19) . . ? C2 N3 C4 113.0(2) . . ? C2 N3 C10 125.8(2) . . ? C4 N3 C10 120.9(3) . . ? N1 C2 N3 103.4(2) . . ? N1 C2 Nd1 134.4(2) . . ? N3 C2 Nd1 118.37(18) . . ? C5 C4 N3 104.0(3) . . ? C5 C4 Si1 128.8(2) . . ? N3 C4 Si1 127.2(2) . . ? C4 C5 N1 108.9(3) . . ? N1 C6 C7 110.0(2) . . ? N1 C6 C8 108.4(3) . . ? C7 C6 C8 110.4(3) . . ? N1 C6 C9 108.2(3) . . ? C7 C6 C9 109.1(3) . . ? C8 C6 C9 110.7(3) . . ? N3 C10 C11 114.2(3) . . ? N2 C11 C10 116.5(3) . . ? N2 C11 Nd1 48.60(14) . . ? C10 C11 Nd1 112.41(19) . . ? N2 C12 C15 106.5(3) . . ? N2 C12 C14 112.7(3) . . ? C15 C12 C14 109.0(3) . . ? N2 C12 C13 110.9(3) . . ? C15 C12 C13 108.7(3) . . ? C14 C12 C13 108.9(3) . . ? C17 Si1 C18 108.9(2) . . ? C17 Si1 C16 110.0(2) . . ? C18 Si1 C16 110.1(2) . . ? C17 Si1 C4 106.46(18) . . ? C18 Si1 C4 109.38(17) . . ? C16 Si1 C4 111.88(17) . . ? Si2 N4 Si3 126.07(16) . . ? Si2 N4 Nd1 117.41(14) . . ? Si3 N4 Nd1 116.52(13) . . ? N4 Si2 C21 109.49(15) . . ? N4 Si2 C19 114.13(18) . . ? C21 Si2 C19 105.6(2) . . ? N4 Si2 C20 113.21(19) . . ? C21 Si2 C20 108.7(2) . . ? C19 Si2 C20 105.3(2) . . ? N4 Si2 Nd1 36.78(9) . . ? C21 Si2 Nd1 74.45(11) . . ? C19 Si2 Nd1 136.41(15) . . ? C20 Si2 Nd1 116.03(15) . . ? N4 Si3 C23 112.87(19) . . ? N4 Si3 C24 109.53(14) . . ? C23 Si3 C24 107.7(2) . . ? N4 Si3 C22 113.71(18) . . ? C23 Si3 C22 107.5(2) . . ? C24 Si3 C22 105.0(2) . . ? N4 Si3 Nd1 37.27(9) . . ? C23 Si3 Nd1 125.90(16) . . ? C24 Si3 Nd1 72.27(11) . . ? C22 Si3 Nd1 125.10(14) . . ? N6 N5 Nd1 125.3(2) . . ? N7 N6 N5 177.3(3) . . ? N6 N7 Nd1 143.5(2) . 3_676 ? C31 C26 C27 117.6(3) . . ? C31 C26 C25 121.5(3) . . ? C27 C26 C25 120.9(3) . . ? C28 C27 C26 121.0(4) . . ? C27 C28 C29 120.5(4) . . ? C30 C29 C28 119.3(4) . . ? C29 C30 C31 120.3(4) . . ? C30 C31 C26 121.3(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.282 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.086 #===end