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 Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis and structures of some heterometallic [(Li, Y)2, (M3, Ce) (M = Li or Na), (Li, Zr2) and (Li, Zr)4] oligomeric diamides derived from 1,2-bis(neopentylamino)benzene ; _publ_requested_category FM loop_ _publ_author_name 'M. Lappert' 'Peter B. Hitchcock' 'Qi-Gu Huang.' 'Xue-Hong Wei.' 'Meisu Zhou.' data_(1)-feb2103 _database_code_depnum_ccdc_archive 'CCDC 289001' _audit_creation_date 2003-02-22T10:14:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((C6H4(NCH2tBu)2YCl2Li(OEt2)2)2) _chemical_formula_moiety 'C48 H92 Cl4 Li2 N4 O4 Y2' _chemical_formula_sum 'C48 H92 Cl4 Li2 N4 O4 Y2' _chemical_formula_weight 1122.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5385(2) _cell_length_b 11.3638(2) _cell_length_c 25.4693(4) _cell_angle_alpha 90 _cell_angle_beta 101.285(1) _cell_angle_gamma 90 _cell_volume 2991.17(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14283 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.149 _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 0.4058 _exptl_absorpt_correction_T_max 0.5067 #----------------------------------------------------------------------------# # 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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_unetI/netI 0.044 _diffrn_reflns_number 18304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 26.04 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 5795 _reflns_number_gt 4824 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; One of the ether ligands was disordered and refined with bond length constraints (SADI) . 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^)+(0.0069P)^2^+9.0949P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 5795 _refine_ls_number_parameters 298 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.592 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # 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' Y Y -2.7962 3.5667 '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' Li Li -0.0003 0.0001 '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 Y Y -0.00579(4) 0.49335(3) -0.094004(14) 0.02428(11) Uani 1 1 d . . . Li Li -0.0074(8) 0.4628(7) -0.2351(3) 0.0411(18) Uani 1 1 d . A . Cl1 Cl -0.07543(12) 0.33637(10) -0.17258(4) 0.0399(3) Uani 1 1 d . . . Cl2 Cl 0.05414(11) 0.62054(10) -0.17424(4) 0.0364(3) Uani 1 1 d . . . O1 O 0.1373(3) 0.3891(3) -0.25911(15) 0.0498(9) Uani 1 1 d . . . O2 O -0.1444(4) 0.5116(4) -0.29309(14) 0.0632(11) Uani 1 1 d D . . N1 N 0.0762(3) 0.3468(3) -0.03543(13) 0.0254(7) Uani 1 1 d . . . N2 N 0.1633(3) 0.5651(3) -0.03190(12) 0.0240(7) Uani 1 1 d . . . C7 C 0.0365(4) 0.2230(3) -0.04192(17) 0.0281(9) Uani 1 1 d . . . H7A H -0.0403 0.2177 -0.0713 0.034 Uiso 1 1 calc R . . H7B H 0.0097 0.1966 -0.0087 0.034 Uiso 1 1 calc R . . C8 C 0.1407(4) 0.1374(4) -0.05427(18) 0.0356(10) Uani 1 1 d . . . C9 C 0.2081(5) 0.1854(5) -0.0973(2) 0.0547(14) Uani 1 1 d . . . H9A H 0.1434 0.2038 -0.1295 0.082 Uiso 1 1 calc R . . H9B H 0.2685 0.1263 -0.106 0.082 Uiso 1 1 calc R . . H9C H 0.2558 0.257 -0.0842 0.082 Uiso 1 1 calc R . . C10 C 0.0698(5) 0.0232(4) -0.0745(2) 0.0529(14) Uani 1 1 d . . . H10A H 0.0259 -0.0081 -0.0469 0.079 Uiso 1 1 calc R . . H10B H 0.1323 -0.0347 -0.0824 0.079 Uiso 1 1 calc R . . H10C H 0.0058 0.0396 -0.1071 0.079 Uiso 1 1 calc R . . C11 C 0.2423(5) 0.1085(5) -0.0044(2) 0.0488(13) Uani 1 1 d . . . H11A H 0.1995 0.0774 0.0235 0.073 Uiso 1 1 calc R . . H11B H 0.2901 0.1802 0.0086 0.073 Uiso 1 1 calc R . . H11C H 0.3025 0.0496 -0.0134 0.073 Uiso 1 1 calc R . . C12 C 0.2195(4) 0.6818(3) -0.03535(16) 0.0268(9) Uani 1 1 d . . . H12A H 0.2177 0.7243 -0.0016 0.032 Uiso 1 1 calc R . . H12B H 0.1635 0.7257 -0.0646 0.032 Uiso 1 1 calc R . . C13 C 0.3603(4) 0.6848(4) -0.04535(17) 0.0305(9) Uani 1 1 d . . . C14 C 0.3758(4) 0.5963(4) -0.08840(17) 0.0350(10) Uani 1 1 d . . . H14A H 0.3128 0.6135 -0.1212 0.052 Uiso 1 1 calc R . . H14B H 0.361 0.5167 -0.0761 0.052 Uiso 1 1 calc R . . H14C H 0.4636 0.6017 -0.0956 0.052 Uiso 1 1 calc R . . C15 C 0.3865(5) 0.8088(4) -0.0639(2) 0.0468(12) Uani 1 1 d . . . H15A H 0.3767 0.8657 -0.036 0.07 Uiso 1 1 calc R . . H15B H 0.3248 0.8273 -0.0969 0.07 Uiso 1 1 calc R . . H15C H 0.4748 0.8129 -0.0706 0.07 Uiso 1 1 calc R . . C16 C 0.4595(4) 0.6569(4) 0.00564(18) 0.0392(11) Uani 1 1 d . . . H16A H 0.4504 0.7136 0.0337 0.059 Uiso 1 1 calc R . . H16B H 0.547 0.6621 -0.0019 0.059 Uiso 1 1 calc R . . H16C H 0.4446 0.5772 0.0178 0.059 Uiso 1 1 calc R . . C17 C 0.2658(6) 0.4393(7) -0.2460(3) 0.081(2) Uani 1 1 d . . . H17A H 0.3062 0.4329 -0.2778 0.097 Uiso 1 1 calc R . . H17B H 0.2575 0.5241 -0.2384 0.097 Uiso 1 1 calc R . . C18 C 0.3501(8) 0.3878(9) -0.2020(4) 0.120(3) Uani 1 1 d . . . H18A H 0.4342 0.4276 -0.1965 0.18 Uiso 1 1 calc R . . H18B H 0.3615 0.3042 -0.2092 0.18 Uiso 1 1 calc R . . H18C H 0.3131 0.396 -0.1698 0.18 Uiso 1 1 calc R . . C19 C 0.1355(6) 0.2668(6) -0.2720(3) 0.0657(17) Uani 1 1 d . . . H19A H 0.1656 0.2206 -0.239 0.079 Uiso 1 1 calc R . . H19B H 0.1955 0.2518 -0.2968 0.079 Uiso 1 1 calc R . . C20 C 0.0040(6) 0.2289(6) -0.2974(3) 0.0696(18) Uani 1 1 d . . . H20A H 0.0048 0.1447 -0.3057 0.104 Uiso 1 1 calc R . . H20B H -0.025 0.2735 -0.3305 0.104 Uiso 1 1 calc R . . H20C H -0.0552 0.2431 -0.2728 0.104 Uiso 1 1 calc R . . C21 C -0.2758(8) 0.5203(9) -0.2814(4) 0.116(3) Uani 1 1 d D A . H21A H -0.2691 0.5436 -0.2435 0.139 Uiso 1 1 calc R . . H21B H -0.3238 0.583 -0.304 0.139 Uiso 1 1 calc R . . C22 C -0.3454(9) 0.4164(9) -0.2904(4) 0.125(4) Uani 1 1 d D . . H22A H -0.4307 0.4273 -0.2812 0.188 Uiso 1 1 calc R A . H22B H -0.2987 0.3538 -0.2682 0.188 Uiso 1 1 calc R . . H22C H -0.356 0.3946 -0.3283 0.188 Uiso 1 1 calc R . . C1 C 0.1352(4) 0.3860(4) 0.01395(15) 0.0256(8) Uani 1 1 d . . 1 C2 C 0.1839(3) 0.5075(4) 0.01559(15) 0.0255(8) Uani 1 1 d . . 1 C3 C 0.2414(4) 0.5523(4) 0.06653(16) 0.0304(9) Uani 1 1 d . . 1 H3 H 0.265 0.633 0.0692 0.036 Uiso 1 1 calc R . 1 C4 C 0.2654(4) 0.4840(4) 0.11325(17) 0.0361(10) Uani 1 1 d . . 1 H4 H 0.3136 0.5158 0.1456 0.043 Uiso 1 1 calc R . 1 C5 C 0.2186(4) 0.3705(4) 0.11204(17) 0.0354(10) Uani 1 1 d . . 1 H5 H 0.2324 0.3237 0.1435 0.043 Uiso 1 1 calc R . 1 C6 C 0.1494(4) 0.3251(4) 0.06275(16) 0.0324(10) Uani 1 1 d . . 1 H6 H 0.1108 0.2495 0.0628 0.039 Uiso 1 1 calc R . 1 C23 C -0.1548(16) 0.5321(18) -0.3481(4) 0.150(8) Uani 0.666(18) 1 d PD A 1 H23C H -0.1582 0.4568 -0.3679 0.18 Uiso 0.666(18) 1 calc PR A 1 H23D H -0.2339 0.5778 -0.3625 0.18 Uiso 0.666(18) 1 calc PR A 1 C24 C -0.0445(17) 0.596(2) -0.3528(9) 0.201(12) Uani 0.666(18) 1 d PD A 1 H24D H -0.0458 0.6121 -0.3907 0.302 Uiso 0.666(18) 1 calc PR A 1 H24E H 0.0327 0.5495 -0.338 0.302 Uiso 0.666(18) 1 calc PR A 1 H24F H -0.043 0.6699 -0.3332 0.302 Uiso 0.666(18) 1 calc PR A 1 C23A C -0.112(3) 0.6185(18) -0.3196(8) 0.096(10) Uiso 0.334(18) 1 d PD A 2 H23A H -0.1646 0.6838 -0.3096 0.115 Uiso 0.334(18) 1 calc PR A 2 H23B H -0.0199 0.6376 -0.3049 0.115 Uiso 0.334(18) 1 calc PR A 2 C24A C -0.128(3) 0.616(2) -0.3746(8) 0.082(8) Uiso 0.334(18) 1 d PD A 2 H24A H -0.0878 0.6858 -0.3869 0.123 Uiso 0.334(18) 1 calc PR A 2 H24B H -0.2209 0.6157 -0.3903 0.123 Uiso 0.334(18) 1 calc PR A 2 H24C H -0.0879 0.545 -0.3856 0.123 Uiso 0.334(18) 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 Y 0.0260(2) 0.0256(2) 0.02105(18) 0.00015(16) 0.00405(14) 0.00041(17) Li 0.041(4) 0.048(5) 0.034(4) -0.003(3) 0.009(3) 0.004(4) Cl1 0.0572(7) 0.0345(6) 0.0268(5) -0.0052(4) 0.0056(5) -0.0062(5) Cl2 0.0441(6) 0.0369(6) 0.0283(5) 0.0051(4) 0.0075(5) -0.0054(5) O1 0.040(2) 0.049(2) 0.064(2) -0.0095(18) 0.0193(17) -0.0015(16) O2 0.060(2) 0.083(3) 0.041(2) 0.009(2) -0.0015(18) 0.013(2) N1 0.0261(17) 0.0227(17) 0.0274(17) 0.0032(14) 0.0057(14) 0.0020(14) N2 0.0227(17) 0.0260(18) 0.0238(17) 0.0012(14) 0.0056(14) -0.0014(14) C7 0.028(2) 0.026(2) 0.030(2) 0.0023(17) 0.0055(18) -0.0028(17) C8 0.034(2) 0.028(2) 0.044(3) -0.0046(19) 0.007(2) 0.0048(19) C9 0.056(3) 0.049(3) 0.068(4) -0.003(3) 0.033(3) 0.013(3) C10 0.054(3) 0.032(3) 0.069(4) -0.012(2) 0.001(3) 0.004(2) C11 0.037(3) 0.041(3) 0.063(3) -0.013(2) -0.002(2) 0.014(2) C12 0.024(2) 0.025(2) 0.031(2) -0.0013(17) 0.0068(17) 0.0013(17) C13 0.023(2) 0.028(2) 0.042(2) 0.0040(19) 0.0087(18) 0.0006(17) C14 0.029(2) 0.042(3) 0.036(2) 0.007(2) 0.0119(19) 0.0071(19) C15 0.040(3) 0.034(3) 0.069(3) 0.011(2) 0.017(3) -0.002(2) C16 0.028(2) 0.045(3) 0.045(3) -0.006(2) 0.007(2) -0.001(2) C17 0.046(4) 0.077(5) 0.121(6) -0.008(5) 0.021(4) -0.007(3) C18 0.085(6) 0.126(8) 0.134(8) -0.040(7) -0.016(6) -0.013(6) C19 0.056(4) 0.071(4) 0.070(4) -0.032(3) 0.012(3) 0.004(3) C20 0.060(4) 0.080(5) 0.075(4) -0.038(4) 0.027(3) -0.011(3) C21 0.093(6) 0.137(9) 0.104(7) 0.018(6) -0.012(5) 0.044(6) C22 0.107(7) 0.125(8) 0.120(7) 0.049(6) -0.035(6) -0.030(6) C1 0.0212(19) 0.029(2) 0.027(2) 0.0023(17) 0.0077(16) 0.0058(16) C2 0.0196(18) 0.031(2) 0.0268(19) -0.0003(18) 0.0061(15) 0.0022(17) C3 0.026(2) 0.034(2) 0.030(2) -0.0018(18) 0.0043(18) -0.0012(18) C4 0.027(2) 0.052(3) 0.027(2) -0.001(2) 0.0017(17) 0.003(2) C5 0.032(2) 0.043(3) 0.030(2) 0.010(2) 0.0027(19) 0.009(2) C6 0.036(2) 0.031(2) 0.030(2) 0.0042(18) 0.0061(19) 0.0073(19) C23 0.162(16) 0.24(2) 0.045(7) 0.039(10) 0.012(8) -0.023(15) C24 0.096(13) 0.30(3) 0.21(2) 0.11(2) 0.038(14) -0.035(16) #----------------------------------------------------------------------------# # 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 Y N2 2.289(3) . ? Y N1 2.289(3) . ? Y Cl1 2.6743(11) . ? Y Cl2 2.6774(11) . ? Y C5 2.689(4) 3_565 ? Y C4 2.695(4) 3_565 ? Y C3 2.757(4) 3_565 ? Y C6 2.767(4) 3_565 ? Y C2 2.997(4) 3_565 ? Y C1 2.997(4) 3_565 ? Li O2 1.934(9) . ? Li O1 1.941(8) . ? Li Cl1 2.358(8) . ? Li Cl2 2.375(8) . ? O1 C19 1.427(7) . ? O1 C17 1.447(7) . ? O2 C23 1.404(10) . ? O2 C23A 1.463(15) . ? O2 C21 1.476(9) . ? N1 C1 1.364(5) . ? N1 C7 1.468(5) . ? N2 C2 1.355(5) . ? N2 C12 1.463(5) . ? C7 C8 1.546(6) . ? C8 C9 1.519(7) . ? C8 C11 1.528(6) . ? C8 C10 1.535(6) . ? C12 C13 1.554(5) . ? C13 C14 1.520(6) . ? C13 C15 1.529(6) . ? C13 C16 1.533(6) . ? C17 C18 1.413(11) . ? C19 C20 1.474(8) . ? C21 C22 1.386(11) . ? C1 C6 1.405(5) . ? C1 C2 1.471(6) . ? C2 C3 1.414(5) . ? C3 C4 1.401(6) . ? C4 C5 1.378(7) . ? C5 C6 1.420(6) . ? C23 C24 1.393(15) . ? C23A C24A 1.377(17) . ? 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 Y N1 70.43(12) . . ? N2 Y Cl1 144.81(9) . . ? N1 Y Cl1 90.90(9) . . ? N2 Y Cl2 93.85(8) . . ? N1 Y Cl2 140.78(9) . . ? Cl1 Y Cl2 81.96(4) . . ? N2 Y C5 115.07(13) . 3_565 ? N1 Y C5 136.52(12) . 3_565 ? Cl1 Y C5 99.11(10) . 3_565 ? Cl2 Y C5 82.68(10) . 3_565 ? N2 Y C4 135.80(13) . 3_565 ? N1 Y C4 115.36(13) . 3_565 ? Cl1 Y C4 78.90(10) . 3_565 ? Cl2 Y C4 101.08(10) . 3_565 ? C5 Y C4 29.67(14) 3_565 3_565 ? N2 Y C3 120.63(11) . 3_565 ? N1 Y C3 86.66(12) . 3_565 ? Cl1 Y C3 86.31(9) . 3_565 ? Cl2 Y C3 130.83(9) . 3_565 ? C5 Y C3 52.34(13) 3_565 3_565 ? C4 Y C3 29.76(12) 3_565 3_565 ? N2 Y C6 86.07(12) . 3_565 ? N1 Y C6 120.87(12) . 3_565 ? Cl1 Y C6 128.86(10) . 3_565 ? Cl2 Y C6 92.35(9) . 3_565 ? C5 Y C6 30.13(13) 3_565 3_565 ? C4 Y C6 52.28(14) 3_565 3_565 ? C3 Y C6 59.78(13) 3_565 3_565 ? N2 Y C2 92.59(11) . 3_565 ? N1 Y C2 76.65(11) . 3_565 ? Cl1 Y C2 112.37(8) . 3_565 ? Cl2 Y C2 141.50(8) . 3_565 ? C5 Y C2 60.36(12) 3_565 3_565 ? C4 Y C2 51.37(11) 3_565 3_565 ? C3 Y C2 28.07(11) 3_565 3_565 ? C6 Y C2 50.31(12) 3_565 3_565 ? N2 Y C1 76.31(11) . 3_565 ? N1 Y C1 93.06(11) . 3_565 ? Cl1 Y C1 136.01(8) . 3_565 ? Cl2 Y C1 118.62(8) . 3_565 ? C5 Y C1 51.53(12) 3_565 3_565 ? C4 Y C1 59.96(12) 3_565 3_565 ? C3 Y C1 50.30(12) 3_565 3_565 ? C6 Y C1 27.85(11) 3_565 3_565 ? C2 Y C1 28.42(11) 3_565 3_565 ? O2 Li O1 113.5(4) . . ? O2 Li Cl1 114.2(4) . . ? O1 Li Cl1 108.1(4) . . ? O2 Li Cl2 110.5(4) . . ? O1 Li Cl2 113.6(4) . . ? Cl1 Li Cl2 95.7(3) . . ? Li Cl1 Y 91.4(2) . . ? Li Cl2 Y 90.9(2) . . ? C19 O1 C17 114.0(4) . . ? C19 O1 Li 121.1(4) . . ? C17 O1 Li 121.0(4) . . ? C23 O2 C23A 51.8(11) . . ? C23 O2 C21 107.3(8) . . ? C23A O2 C21 110.6(13) . . ? C23 O2 Li 135.3(8) . . ? C23A O2 Li 112.5(12) . . ? C21 O2 Li 117.1(5) . . ? C1 N1 C7 119.0(3) . . ? C1 N1 Y 114.1(2) . . ? C7 N1 Y 124.1(3) . . ? C2 N2 C12 119.7(3) . . ? C2 N2 Y 114.4(2) . . ? C12 N2 Y 123.4(2) . . ? N1 C7 C8 115.3(3) . . ? C9 C8 C11 109.1(4) . . ? C9 C8 C10 109.1(4) . . ? C11 C8 C10 108.3(4) . . ? C9 C8 C7 111.8(4) . . ? C11 C8 C7 112.1(4) . . ? C10 C8 C7 106.3(4) . . ? N2 C12 C13 116.1(3) . . ? C14 C13 C15 109.6(4) . . ? C14 C13 C16 108.8(3) . . ? C15 C13 C16 108.5(4) . . ? C14 C13 C12 110.2(3) . . ? C15 C13 C12 107.9(3) . . ? C16 C13 C12 111.8(3) . . ? C18 C17 O1 115.8(7) . . ? O1 C19 C20 110.8(5) . . ? C22 C21 O2 113.4(8) . . ? N1 C1 C6 127.2(4) . . ? N1 C1 C2 115.2(3) . . ? C6 C1 C2 117.5(4) . . ? N1 C1 Y 126.2(2) . 3_565 ? C6 C1 Y 66.9(2) . 3_565 ? C2 C1 Y 75.8(2) . 3_565 ? N2 C2 C3 127.6(4) . . ? N2 C2 C1 115.7(3) . . ? C3 C2 C1 116.6(4) . . ? N2 C2 Y 125.8(2) . 3_565 ? C3 C2 Y 66.5(2) . 3_565 ? C1 C2 Y 75.8(2) . 3_565 ? C4 C3 C2 123.6(4) . . ? C4 C3 Y 72.7(2) . 3_565 ? C2 C3 Y 85.4(2) . 3_565 ? C5 C4 C3 119.6(4) . . ? C5 C4 Y 74.9(2) . 3_565 ? C3 C4 Y 77.6(2) . 3_565 ? C4 C5 C6 118.7(4) . . ? C4 C5 Y 75.4(3) . 3_565 ? C6 C5 Y 78.0(2) . 3_565 ? C1 C6 C5 123.4(4) . . ? C1 C6 Y 85.2(2) . 3_565 ? C5 C6 Y 71.9(2) . 3_565 ? C24 C23 O2 105.6(14) . . ? C24A C23A O2 117.2(19) . . ? #===END data_(2)-mar3104 _database_code_depnum_ccdc_archive 'CCDC 289002' _audit_creation_date 2004-03-26T13:29:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C80 H144 Cl12 Li4 N8 O4 Zr4' _chemical_formula_sum 'C80 H144 Cl12 Li4 N8 O4 Zr4' _chemical_formula_weight 2100.07 _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 10.2596(4) _cell_length_b 15.3225(8) _cell_length_c 18.3381(10) _cell_angle_alpha 70.809(2) _cell_angle_beta 79.492(3) _cell_angle_gamma 78.819(3) _cell_volume 2648.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26494 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_special_details ; 'Very weak high angle data ; data collection limited to 23 degrees theta' ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.729 _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 0.8389 _exptl_absorpt_correction_T_max 0.8929 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.711808E-1 _diffrn_orient_matrix_ub_12 0.8252E-3 _diffrn_orient_matrix_ub_13 0.30362E-1 _diffrn_orient_matrix_ub_21 -0.684924E-1 _diffrn_orient_matrix_ub_22 -0.14065E-2 _diffrn_orient_matrix_ub_23 0.466279E-1 _diffrn_orient_matrix_ub_31 0.166774E-1 _diffrn_orient_matrix_ub_32 -0.698151E-1 _diffrn_orient_matrix_ub_33 0.171304E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_number 25227 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 22.96 _diffrn_reflns_theta_full 22.96 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 7289 _reflns_number_gt 5711 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+5.9985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 7289 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.106 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.496 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # 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' 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' Zr Zr -2.9673 0.5597 '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' 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 Zr1 Zr 0.53544(5) 0.39901(3) 0.78516(3) 0.02932(15) Uani 1 1 d . . . Zr2 Zr 0.55594(5) 0.27309(4) 0.61851(3) 0.02991(16) Uani 1 1 d . . . Li1 Li 0.5358(10) 0.5484(7) 0.5537(6) 0.047(2) Uani 1 1 d . . . Li2 Li 0.7739(10) 0.5668(7) 0.7153(6) 0.046(2) Uani 1 1 d . . . Cl1 Cl 0.56921(14) 0.55772(9) 0.67350(7) 0.0375(3) Uani 1 1 d . . . Cl2 Cl 0.72077(14) 0.43925(10) 0.83134(8) 0.0395(3) Uani 1 1 d . . . Cl3 Cl 0.39096(12) 0.38623(9) 0.68731(7) 0.0352(3) Uani 1 1 d . . . Cl4 Cl 0.70839(12) 0.30255(9) 0.70494(7) 0.0338(3) Uani 1 1 d . . . Cl5 Cl 0.65326(13) 0.41904(9) 0.51341(7) 0.0363(3) Uani 1 1 d . . . Cl6 Cl 0.38088(14) 0.31345(10) 0.53175(8) 0.0408(3) Uani 1 1 d . . . O1 O 0.9508(4) 0.5215(3) 0.6765(3) 0.0618(12) Uani 1 1 d . . . O2 O 0.7566(5) 0.6865(3) 0.7314(3) 0.0665(13) Uani 1 1 d . . . N1 N 0.3588(4) 0.4473(3) 0.8421(2) 0.0327(10) Uani 1 1 d . . . N2 N 0.4878(4) 0.2781(3) 0.8698(2) 0.0323(10) Uani 1 1 d . . . N3 N 0.7087(4) 0.1786(3) 0.5878(2) 0.0340(10) Uani 1 1 d . . . N4 N 0.5022(4) 0.1519(3) 0.6979(2) 0.0319(10) Uani 1 1 d . . . C1 C 0.2810(5) 0.3759(4) 0.8852(3) 0.0342(13) Uani 1 1 d . . . C2 C 0.3508(5) 0.2840(4) 0.8995(3) 0.0364(13) Uani 1 1 d . . . C3 C 0.2805(6) 0.2090(4) 0.9380(4) 0.0514(16) Uani 1 1 d . . . H3 H 0.3267 0.1471 0.9479 0.062 Uiso 1 1 calc R . . C4 C 0.1441(7) 0.2235(5) 0.9622(4) 0.0638(19) Uani 1 1 d . . . H4 H 0.0971 0.1716 0.9875 0.077 Uiso 1 1 calc R . . C5 C 0.0776(7) 0.3120(5) 0.9495(4) 0.0628(19) Uani 1 1 d . . . H5 H -0.0155 0.3214 0.9671 0.075 Uiso 1 1 calc R . . C6 C 0.1427(6) 0.3877(5) 0.9116(4) 0.0495(16) Uani 1 1 d . . . H6 H 0.0941 0.4488 0.903 0.059 Uiso 1 1 calc R . . C7 C 0.2939(6) 0.5454(4) 0.8256(3) 0.0403(14) Uani 1 1 d . . . H7A H 0.1982 0.5472 0.8221 0.048 Uiso 1 1 calc R . . H7B H 0.3346 0.5811 0.7737 0.048 Uiso 1 1 calc R . . C8 C 0.3016(6) 0.5965(4) 0.8840(4) 0.0467(15) Uani 1 1 d . . . C9 C 0.4472(7) 0.5992(6) 0.8885(5) 0.075(2) Uani 1 1 d . . . H9A H 0.4514 0.6311 0.9262 0.113 Uiso 1 1 calc R . . H9B H 0.4896 0.6328 0.8372 0.113 Uiso 1 1 calc R . . H9C H 0.4943 0.5352 0.9052 0.113 Uiso 1 1 calc R . . C10 C 0.2296(8) 0.6962(5) 0.8532(5) 0.078(2) Uani 1 1 d . . . H10A H 0.2327 0.7313 0.8887 0.117 Uiso 1 1 calc R . . H10B H 0.1361 0.6942 0.8498 0.117 Uiso 1 1 calc R . . H10C H 0.274 0.7268 0.8015 0.117 Uiso 1 1 calc R . . C11 C 0.2356(7) 0.5493(5) 0.9655(4) 0.0605(18) Uani 1 1 d . . . H11A H 0.2441 0.5833 1.0009 0.091 Uiso 1 1 calc R . . H11B H 0.2797 0.4847 0.9841 0.091 Uiso 1 1 calc R . . H11C H 0.1405 0.5495 0.964 0.091 Uiso 1 1 calc R . . C12 C 0.5701(6) 0.1849(4) 0.8898(3) 0.0374(13) Uani 1 1 d . . . H12A H 0.64 0.1828 0.8452 0.045 Uiso 1 1 calc R . . H12B H 0.5119 0.138 0.8953 0.045 Uiso 1 1 calc R . . C13 C 0.6397(6) 0.1542(4) 0.9638(3) 0.0440(15) Uani 1 1 d . . . C14 C 0.7474(7) 0.2116(5) 0.9555(4) 0.070(2) Uani 1 1 d . . . H14A H 0.7076 0.277 0.9479 0.106 Uiso 1 1 calc R . . H14B H 0.8134 0.2069 0.9106 0.106 Uiso 1 1 calc R . . H14C H 0.7916 0.1884 1.0028 0.106 Uiso 1 1 calc R . . C15 C 0.5389(8) 0.1637(7) 1.0346(4) 0.088(3) Uani 1 1 d . . . H15A H 0.5014 0.2296 1.0266 0.132 Uiso 1 1 calc R . . H15B H 0.5843 0.1403 1.0814 0.132 Uiso 1 1 calc R . . H15C H 0.4665 0.1274 1.041 0.132 Uiso 1 1 calc R . . C16 C 0.6975(10) 0.0526(5) 0.9758(5) 0.103(3) Uani 1 1 d . . . H16A H 0.6253 0.0165 0.9812 0.154 Uiso 1 1 calc R . . H16B H 0.7416 0.0286 1.0231 0.154 Uiso 1 1 calc R . . H16C H 0.763 0.0469 0.9309 0.154 Uiso 1 1 calc R . . C17 C 0.7305(5) 0.1007(4) 0.6537(3) 0.0353(13) Uani 1 1 d . . . C18 C 0.6189(5) 0.0859(3) 0.7134(3) 0.0321(13) Uani 1 1 d . . . C19 C 0.6355(6) 0.0140(4) 0.7821(3) 0.0405(14) Uani 1 1 d . . . H19 H 0.562 0.004 0.8222 0.049 Uiso 1 1 calc R . . C20 C 0.7563(7) -0.0434(4) 0.7935(4) 0.0495(16) Uani 1 1 d . . . H20 H 0.7651 -0.0923 0.841 0.059 Uiso 1 1 calc R . . C21 C 0.8640(6) -0.0298(4) 0.7360(4) 0.0493(16) Uani 1 1 d . . . H21 H 0.9468 -0.0696 0.7439 0.059 Uiso 1 1 calc R . . C22 C 0.8521(6) 0.0416(4) 0.6671(3) 0.0429(15) Uani 1 1 d . . . H22 H 0.9275 0.0507 0.6281 0.052 Uiso 1 1 calc R . . C23 C 0.8081(6) 0.1894(4) 0.5167(3) 0.0482(16) Uani 1 1 d . . . H23A H 0.8973 0.1597 0.5329 0.058 Uiso 1 1 calc R . . H23B H 0.8124 0.2569 0.4915 0.058 Uiso 1 1 calc R . . C24 C 0.7821(7) 0.1488(5) 0.4562(4) 0.0585(18) Uani 1 1 d . . . C25 C 0.6534(9) 0.1977(7) 0.4236(5) 0.106(3) Uani 1 1 d . . . H25A H 0.6379 0.1697 0.3855 0.158 Uiso 1 1 calc R . . H25B H 0.6599 0.264 0.3981 0.158 Uiso 1 1 calc R . . H25C H 0.5788 0.191 0.4659 0.158 Uiso 1 1 calc R . . C26 C 0.8992(8) 0.1661(6) 0.3895(4) 0.096(3) Uani 1 1 d . . . H26A H 0.8862 0.1408 0.3491 0.144 Uiso 1 1 calc R . . H26B H 0.9838 0.1352 0.4099 0.144 Uiso 1 1 calc R . . H26C H 0.9018 0.2334 0.3671 0.144 Uiso 1 1 calc R . . C27 C 0.7769(10) 0.0448(6) 0.4904(4) 0.089(3) Uani 1 1 d . . . H27A H 0.7586 0.0206 0.4506 0.133 Uiso 1 1 calc R . . H27B H 0.7056 0.0337 0.5346 0.133 Uiso 1 1 calc R . . H27C H 0.8631 0.0129 0.5083 0.133 Uiso 1 1 calc R . . C28 C 0.3752(5) 0.1333(4) 0.7491(3) 0.0374(13) Uani 1 1 d . . . H28A H 0.3197 0.1942 0.7478 0.045 Uiso 1 1 calc R . . H28B H 0.3965 0.1028 0.803 0.045 Uiso 1 1 calc R . . C29 C 0.2884(6) 0.0722(4) 0.7309(3) 0.0477(15) Uani 1 1 d . . . C30 C 0.2397(7) 0.1207(5) 0.6520(4) 0.065(2) Uani 1 1 d . . . H30A H 0.3165 0.1262 0.611 0.098 Uiso 1 1 calc R . . H30B H 0.1922 0.1831 0.6506 0.098 Uiso 1 1 calc R . . H30C H 0.1789 0.084 0.6433 0.098 Uiso 1 1 calc R . . C31 C 0.1662(8) 0.0641(6) 0.7934(4) 0.082(2) Uani 1 1 d . . . H31A H 0.1956 0.0325 0.8448 0.123 Uiso 1 1 calc R . . H31B H 0.1058 0.028 0.7837 0.123 Uiso 1 1 calc R . . H31C H 0.1191 0.1267 0.7918 0.123 Uiso 1 1 calc R . . C32 C 0.3628(8) -0.0235(5) 0.7321(5) 0.075(2) Uani 1 1 d . . . H32A H 0.3949 -0.055 0.7828 0.112 Uiso 1 1 calc R . . H32B H 0.4393 -0.0172 0.691 0.112 Uiso 1 1 calc R . . H32C H 0.3024 -0.0604 0.7234 0.112 Uiso 1 1 calc R . . C33 C 1.0365(6) 0.4535(5) 0.7317(5) 0.069(2) Uani 1 1 d . . . H33A H 0.9979 0.4533 0.7853 0.083 Uiso 1 1 calc R . . H33B H 1.1263 0.4729 0.7213 0.083 Uiso 1 1 calc R . . C34 C 1.0503(7) 0.3576(6) 0.7262(6) 0.092(3) Uani 1 1 d . . . H34A H 1.1069 0.3147 0.7645 0.137 Uiso 1 1 calc R . . H34B H 1.0916 0.3569 0.6737 0.137 Uiso 1 1 calc R . . H34C H 0.9616 0.3379 0.7366 0.137 Uiso 1 1 calc R . . C35 C 1.0229(10) 0.5495(8) 0.6023(5) 0.118(4) Uani 1 1 d . . . H35A H 1.0595 0.4941 0.5846 0.141 Uiso 1 1 calc R . . H35B H 1.0991 0.5791 0.6045 0.141 Uiso 1 1 calc R . . C36 C 0.9374(9) 0.6156(8) 0.5467(5) 0.118(4) Uani 1 1 d . . . H36A H 0.9901 0.6346 0.4953 0.177 Uiso 1 1 calc R . . H36B H 0.9018 0.6707 0.564 0.177 Uiso 1 1 calc R . . H36C H 0.8631 0.5859 0.5436 0.177 Uiso 1 1 calc R . . C37 C 0.8446(12) 0.6961(8) 0.7810(6) 0.128(4) Uani 1 1 d . . . H37A H 0.9331 0.6595 0.7713 0.153 Uiso 1 1 calc R . . H37B H 0.8575 0.7625 0.765 0.153 Uiso 1 1 calc R . . C38 C 0.8045(13) 0.6696(9) 0.8569(6) 0.145(5) Uani 1 1 d . . . H38A H 0.8729 0.6767 0.8846 0.218 Uiso 1 1 calc R . . H38B H 0.7907 0.604 0.874 0.218 Uiso 1 1 calc R . . H38C H 0.7202 0.7084 0.8682 0.218 Uiso 1 1 calc R . . C39 C 0.6595(11) 0.7660(6) 0.7036(6) 0.120(4) Uani 1 1 d . . . H39A H 0.5746 0.7432 0.7055 0.144 Uiso 1 1 calc R . . H39B H 0.6427 0.8028 0.7407 0.144 Uiso 1 1 calc R . . C40 C 0.6882(11) 0.8259(8) 0.6300(7) 0.144(5) Uani 1 1 d . . . H40A H 0.6127 0.8762 0.6181 0.215 Uiso 1 1 calc R . . H40B H 0.7036 0.7915 0.5919 0.215 Uiso 1 1 calc R . . H40C H 0.7688 0.8527 0.6275 0.215 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 Zr1 0.0338(3) 0.0320(3) 0.0237(3) -0.0110(2) -0.0016(2) -0.0058(2) Zr2 0.0333(3) 0.0308(3) 0.0263(3) -0.0117(2) -0.0021(2) -0.0025(2) Li1 0.054(6) 0.048(6) 0.039(6) -0.018(5) -0.013(5) 0.007(5) Li2 0.045(6) 0.045(6) 0.049(6) -0.015(5) -0.004(5) -0.007(5) Cl1 0.0491(8) 0.0374(8) 0.0273(7) -0.0084(6) -0.0065(6) -0.0098(6) Cl2 0.0439(8) 0.0442(8) 0.0327(8) -0.0097(6) -0.0089(6) -0.0118(6) Cl3 0.0311(7) 0.0457(8) 0.0345(8) -0.0223(6) -0.0050(6) 0.0001(6) Cl4 0.0318(7) 0.0398(8) 0.0322(7) -0.0164(6) -0.0027(6) -0.0023(6) Cl5 0.0388(8) 0.0357(8) 0.0310(7) -0.0093(6) 0.0004(6) -0.0031(6) Cl6 0.0442(8) 0.0444(8) 0.0353(8) -0.0109(7) -0.0109(6) -0.0063(6) O1 0.048(3) 0.080(3) 0.056(3) -0.027(3) 0.013(2) -0.014(2) O2 0.092(4) 0.043(3) 0.071(3) -0.022(2) -0.019(3) -0.010(3) N1 0.040(3) 0.035(3) 0.027(2) -0.016(2) -0.001(2) -0.005(2) N2 0.040(3) 0.034(3) 0.024(2) -0.012(2) -0.001(2) -0.006(2) N3 0.040(3) 0.031(3) 0.031(3) -0.013(2) -0.001(2) -0.001(2) N4 0.034(3) 0.034(3) 0.031(3) -0.014(2) -0.005(2) -0.007(2) C1 0.038(3) 0.045(4) 0.026(3) -0.019(3) 0.003(2) -0.013(3) C2 0.042(3) 0.044(4) 0.028(3) -0.017(3) 0.003(2) -0.014(3) C3 0.055(4) 0.045(4) 0.054(4) -0.016(3) 0.007(3) -0.016(3) C4 0.057(5) 0.063(5) 0.074(5) -0.023(4) 0.016(4) -0.033(4) C5 0.041(4) 0.083(6) 0.073(5) -0.039(4) 0.015(3) -0.022(4) C6 0.043(4) 0.057(4) 0.054(4) -0.028(3) 0.002(3) -0.009(3) C7 0.048(4) 0.039(3) 0.037(3) -0.022(3) -0.003(3) 0.000(3) C8 0.049(4) 0.045(4) 0.051(4) -0.025(3) 0.002(3) -0.007(3) C9 0.062(5) 0.096(6) 0.095(6) -0.071(5) 0.004(4) -0.015(4) C10 0.103(6) 0.048(4) 0.090(6) -0.040(4) -0.007(5) 0.002(4) C11 0.076(5) 0.064(5) 0.048(4) -0.034(4) 0.001(3) -0.008(4) C12 0.046(3) 0.030(3) 0.037(3) -0.010(3) -0.004(3) -0.009(3) C13 0.058(4) 0.037(3) 0.040(4) -0.009(3) -0.014(3) -0.012(3) C14 0.081(5) 0.062(5) 0.070(5) 0.001(4) -0.039(4) -0.021(4) C15 0.109(7) 0.131(8) 0.024(4) -0.013(4) -0.006(4) -0.036(6) C16 0.164(9) 0.044(5) 0.115(7) -0.015(5) -0.098(7) 0.011(5) C17 0.039(3) 0.035(3) 0.037(3) -0.019(3) -0.007(3) -0.002(3) C18 0.045(3) 0.026(3) 0.031(3) -0.015(3) -0.006(3) -0.004(2) C19 0.053(4) 0.040(3) 0.032(3) -0.016(3) -0.005(3) -0.007(3) C20 0.073(5) 0.036(4) 0.039(4) -0.009(3) -0.020(3) 0.000(3) C21 0.052(4) 0.039(4) 0.060(4) -0.021(3) -0.025(3) 0.011(3) C22 0.041(4) 0.042(4) 0.051(4) -0.023(3) -0.010(3) 0.002(3) C23 0.047(4) 0.045(4) 0.039(4) -0.011(3) 0.014(3) 0.001(3) C24 0.066(5) 0.059(4) 0.041(4) -0.021(3) 0.000(3) 0.017(3) C25 0.100(7) 0.154(9) 0.068(6) -0.069(6) -0.027(5) 0.045(6) C26 0.102(7) 0.102(7) 0.056(5) -0.028(5) 0.028(5) 0.019(5) C27 0.141(8) 0.083(6) 0.062(5) -0.050(5) -0.004(5) -0.021(5) C28 0.038(3) 0.040(3) 0.034(3) -0.011(3) 0.001(3) -0.013(3) C29 0.049(4) 0.058(4) 0.043(4) -0.017(3) -0.009(3) -0.020(3) C30 0.070(5) 0.074(5) 0.062(5) -0.018(4) -0.016(4) -0.031(4) C31 0.077(5) 0.111(7) 0.068(5) -0.026(5) 0.007(4) -0.056(5) C32 0.104(6) 0.047(4) 0.090(6) -0.023(4) -0.034(5) -0.024(4) C33 0.034(4) 0.082(6) 0.096(6) -0.037(5) -0.014(4) 0.005(4) C34 0.047(5) 0.078(6) 0.162(9) -0.054(6) -0.012(5) -0.008(4) C35 0.107(8) 0.152(10) 0.074(7) -0.027(7) 0.022(6) -0.014(7) C36 0.073(6) 0.192(12) 0.071(6) -0.023(7) -0.010(5) -0.009(7) C37 0.188(12) 0.126(9) 0.112(9) -0.059(7) -0.013(8) -0.090(9) C38 0.208(13) 0.166(12) 0.078(8) -0.012(8) -0.019(8) -0.109(10) C39 0.163(10) 0.056(6) 0.114(9) -0.019(6) -0.010(7) 0.026(6) C40 0.104(8) 0.154(11) 0.122(10) 0.021(8) -0.024(7) 0.002(7) #----------------------------------------------------------------------------# # 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 Zr1 N1 2.054(4) . ? Zr1 N2 2.065(4) . ? Zr1 Cl2 2.4694(14) . ? Zr1 Cl3 2.6016(13) . ? Zr1 Cl4 2.6377(13) . ? Zr1 Cl1 2.6496(14) . ? Zr2 N4 2.049(4) . ? Zr2 N3 2.051(4) . ? Zr2 Cl6 2.4708(14) . ? Zr2 Cl4 2.6096(13) . ? Zr2 Cl3 2.6425(13) . ? Zr2 Cl5 2.6539(14) . ? Li1 Cl1 2.337(10) . ? Li1 Cl5 2.371(10) 2_666 ? Li1 Cl5 2.375(10) . ? Li1 Cl6 2.387(11) 2_666 ? Li2 O1 1.910(11) . ? Li2 O2 1.921(11) . ? Li2 Cl1 2.405(10) . ? Li2 Cl2 2.430(10) . ? O1 C35 1.399(9) . ? O1 C33 1.468(8) . ? O2 C39 1.430(9) . ? O2 C37 1.450(10) . ? N1 C1 1.413(7) . ? N1 C7 1.477(7) . ? N2 C2 1.409(7) . ? N2 C12 1.478(7) . ? N3 C17 1.408(7) . ? N3 C23 1.485(7) . ? N4 C18 1.415(6) . ? N4 C28 1.477(6) . ? C1 C6 1.410(8) . ? C1 C2 1.414(8) . ? C2 C3 1.393(8) . ? C3 C4 1.387(9) . ? C4 C5 1.360(10) . ? C5 C6 1.370(9) . ? C7 C8 1.540(8) . ? C8 C9 1.520(9) . ? C8 C11 1.526(9) . ? C8 C10 1.531(9) . ? C12 C13 1.541(7) . ? C13 C14 1.498(8) . ? C13 C16 1.513(9) . ? C13 C15 1.534(9) . ? C17 C22 1.402(8) . ? C17 C18 1.430(7) . ? C18 C19 1.386(7) . ? C19 C20 1.379(8) . ? C20 C21 1.376(9) . ? C21 C22 1.380(8) . ? C23 C24 1.521(9) . ? C24 C25 1.508(10) . ? C24 C27 1.516(10) . ? C24 C26 1.544(9) . ? C28 C29 1.556(8) . ? C29 C32 1.511(9) . ? C29 C30 1.520(9) . ? C29 C31 1.531(9) . ? C33 C34 1.483(10) . ? C35 C36 1.461(12) . ? C37 C38 1.325(12) . ? C39 C40 1.377(12) . ? 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 Zr1 N2 78.43(17) . . ? N1 Zr1 Cl2 107.80(12) . . ? N2 Zr1 Cl2 104.05(12) . . ? N1 Zr1 Cl3 86.44(12) . . ? N2 Zr1 Cl3 94.40(12) . . ? Cl2 Zr1 Cl3 158.50(5) . . ? N1 Zr1 Cl4 160.64(12) . . ? N2 Zr1 Cl4 91.39(12) . . ? Cl2 Zr1 Cl4 90.54(5) . . ? Cl3 Zr1 Cl4 77.89(4) . . ? N1 Zr1 Cl1 97.32(12) . . ? N2 Zr1 Cl1 173.78(12) . . ? Cl2 Zr1 Cl1 81.50(5) . . ? Cl3 Zr1 Cl1 80.74(4) . . ? Cl4 Zr1 Cl1 91.36(4) . . ? N4 Zr2 N3 80.15(17) . . ? N4 Zr2 Cl6 100.73(12) . . ? N3 Zr2 Cl6 110.18(12) . . ? N4 Zr2 Cl4 95.38(12) . . ? N3 Zr2 Cl4 89.40(12) . . ? Cl6 Zr2 Cl4 156.40(5) . . ? N4 Zr2 Cl3 95.75(12) . . ? N3 Zr2 Cl3 166.07(12) . . ? Cl6 Zr2 Cl3 83.62(4) . . ? Cl4 Zr2 Cl3 77.67(4) . . ? N4 Zr2 Cl5 173.42(12) . . ? N3 Zr2 Cl5 93.56(12) . . ? Cl6 Zr2 Cl5 83.19(5) . . ? Cl4 Zr2 Cl5 82.53(4) . . ? Cl3 Zr2 Cl5 89.91(4) . . ? Cl1 Li1 Cl5 134.3(4) . 2_666 ? Cl1 Li1 Cl5 118.2(4) . . ? Cl5 Li1 Cl5 99.0(4) 2_666 . ? Cl1 Li1 Cl6 100.2(4) . 2_666 ? Cl5 Li1 Cl6 91.4(3) 2_666 2_666 ? Cl5 Li1 Cl6 108.4(4) . 2_666 ? O1 Li2 O2 114.3(5) . . ? O1 Li2 Cl1 126.2(5) . . ? O2 Li2 Cl1 107.8(4) . . ? O1 Li2 Cl2 102.6(4) . . ? O2 Li2 Cl2 115.2(5) . . ? Cl1 Li2 Cl2 87.5(3) . . ? Li1 Cl1 Li2 128.7(4) . . ? Li1 Cl1 Zr1 110.7(3) . . ? Li2 Cl1 Zr1 92.5(2) . . ? Li2 Cl2 Zr1 96.5(2) . . ? Zr1 Cl3 Zr2 101.91(4) . . ? Zr2 Cl4 Zr1 101.83(4) . . ? Li1 Cl5 Li1 81.0(4) 2_666 . ? Li1 Cl5 Zr2 90.4(3) 2_666 . ? Li1 Cl5 Zr2 103.9(3) . . ? Li1 Cl6 Zr2 94.6(2) 2_666 . ? C35 O1 C33 110.7(6) . . ? C35 O1 Li2 130.2(6) . . ? C33 O1 Li2 118.8(5) . . ? C39 O2 C37 115.9(7) . . ? C39 O2 Li2 126.6(6) . . ? C37 O2 Li2 117.3(6) . . ? C1 N1 C7 118.5(4) . . ? C1 N1 Zr1 113.0(3) . . ? C7 N1 Zr1 126.2(3) . . ? C2 N2 C12 117.6(4) . . ? C2 N2 Zr1 112.8(3) . . ? C12 N2 Zr1 128.3(3) . . ? C17 N3 C23 119.3(4) . . ? C17 N3 Zr2 109.0(3) . . ? C23 N3 Zr2 130.3(4) . . ? C18 N4 C28 119.1(4) . . ? C18 N4 Zr2 109.0(3) . . ? C28 N4 Zr2 130.5(3) . . ? C6 C1 N1 126.6(5) . . ? C6 C1 C2 118.2(5) . . ? N1 C1 C2 115.1(5) . . ? C3 C2 N2 126.1(5) . . ? C3 C2 C1 119.0(5) . . ? N2 C2 C1 114.8(5) . . ? C4 C3 C2 121.0(6) . . ? C5 C4 C3 119.9(6) . . ? C4 C5 C6 121.0(6) . . ? C5 C6 C1 120.8(6) . . ? N1 C7 C8 117.2(5) . . ? C9 C8 C11 108.4(6) . . ? C9 C8 C10 109.7(6) . . ? C11 C8 C10 109.8(6) . . ? C9 C8 C7 109.8(5) . . ? C11 C8 C7 112.2(5) . . ? C10 C8 C7 106.9(5) . . ? N2 C12 C13 117.8(4) . . ? C14 C13 C16 111.0(6) . . ? C14 C13 C15 107.7(6) . . ? C16 C13 C15 109.6(7) . . ? C14 C13 C12 111.9(5) . . ? C16 C13 C12 105.7(5) . . ? C15 C13 C12 110.9(5) . . ? C22 C17 N3 125.9(5) . . ? C22 C17 C18 118.4(5) . . ? N3 C17 C18 115.5(5) . . ? C19 C18 N4 125.9(5) . . ? C19 C18 C17 118.7(5) . . ? N4 C18 C17 115.2(5) . . ? C20 C19 C18 121.6(6) . . ? C21 C20 C19 120.0(6) . . ? C20 C21 C22 120.3(6) . . ? C21 C22 C17 120.9(6) . . ? N3 C23 C24 116.3(5) . . ? C25 C24 C27 109.8(7) . . ? C25 C24 C23 110.9(5) . . ? C27 C24 C23 111.1(5) . . ? C25 C24 C26 108.5(6) . . ? C27 C24 C26 109.6(6) . . ? C23 C24 C26 106.9(6) . . ? N4 C28 C29 117.7(5) . . ? C32 C29 C30 109.1(6) . . ? C32 C29 C31 110.5(6) . . ? C30 C29 C31 108.2(6) . . ? C32 C29 C28 112.7(5) . . ? C30 C29 C28 110.4(5) . . ? C31 C29 C28 105.8(5) . . ? O1 C33 C34 112.4(6) . . ? O1 C35 C36 110.9(8) . . ? C38 C37 O2 116.5(9) . . ? C40 C39 O2 118.1(9) . . ? #===END data_(3)-apr504 _database_code_depnum_ccdc_archive 'CCDC 289003' _audit_creation_date 2004-04-05T09:16:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H88 Cl3 Li N6 O Zr2' _chemical_formula_sum 'C52 H88 Cl3 Li N6 O Zr2' _chemical_formula_weight 1109.01 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7426(6) _cell_length_b 23.545(2) _cell_length_c 22.916(2) _cell_angle_alpha 90 _cell_angle_beta 93.723(6) _cell_angle_gamma 90 _cell_volume 5784.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45754 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.538 _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 0.873 _exptl_absorpt_correction_T_max 0.995 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.838985E-1 _diffrn_orient_matrix_ub_12 0.25609E-2 _diffrn_orient_matrix_ub_13 -0.214477E-1 _diffrn_orient_matrix_ub_21 -0.406058E-1 _diffrn_orient_matrix_ub_22 -0.13679E-2 _diffrn_orient_matrix_ub_23 0.380256E-1 _diffrn_orient_matrix_ub_31 0.37597E-2 _diffrn_orient_matrix_ub_32 0.423734E-1 _diffrn_orient_matrix_ub_33 0.25238E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.2311 _diffrn_reflns_av_unetI/netI 0.196 _diffrn_reflns_number 26681 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 22.96 _diffrn_reflns_theta_full 22.96 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 7836 _reflns_number_gt 4171 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+53.2442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 7836 _refine_ls_number_parameters 584 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1951 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.1978 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.513 _refine_diff_density_min -0.54 _refine_diff_density_rms 0.122 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Li Li -0.0003 0.0001 '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 Zr1 Zr 0.10150(10) 0.38043(6) 0.32281(5) 0.0296(3) Uani 1 1 d . . . Zr2 Zr 0.28423(10) 0.39049(5) 0.14666(5) 0.0270(3) Uani 1 1 d . . . Li Li 0.366(2) 0.2949(10) 0.2758(11) 0.048(6) Uani 1 1 d . . . Cl1 Cl 0.1746(3) 0.32337(13) 0.22093(13) 0.0323(8) Uani 1 1 d . . . Cl2 Cl 0.4687(3) 0.35447(15) 0.21135(14) 0.0396(9) Uani 1 1 d . . . Cl3 Cl 0.2860(3) 0.32237(15) 0.36358(14) 0.0401(9) Uani 1 1 d . . . O1 O 0.4049(9) 0.2179(4) 0.2844(4) 0.049(3) Uani 1 1 d . . . N1 N 0.0263(8) 0.3988(4) 0.4004(4) 0.033(3) Uani 1 1 d . . . N2 N -0.0638(8) 0.3303(4) 0.3180(4) 0.031(3) Uani 1 1 d . . . N3 N 0.1757(8) 0.3469(4) 0.0863(4) 0.028(2) Uani 1 1 d . . . N4 N 0.4051(8) 0.3916(4) 0.0807(4) 0.030(2) Uani 1 1 d . . . N5 N 0.0226(7) 0.4346(4) 0.2522(4) 0.023(2) Uani 1 1 d . . . N6 N 0.2412(8) 0.4474(4) 0.3057(4) 0.025(2) Uani 1 1 d . . . C1 C -0.1057(11) 0.3876(6) 0.3991(5) 0.038(3) Uani 1 1 d . . . C2 C -0.1538(11) 0.3524(6) 0.3531(5) 0.031(3) Uani 1 1 d . . . C3 C -0.2820(12) 0.3433(6) 0.3487(6) 0.041(3) Uani 1 1 d . . . H3 H -0.3158 0.3183 0.3192 0.049 Uiso 1 1 calc R . . C4 C -0.3601(14) 0.3684(7) 0.3844(6) 0.055(4) Uani 1 1 d . . . H4 H -0.4475 0.3623 0.3789 0.065 Uiso 1 1 calc R . . C5 C -0.3122(13) 0.4033(7) 0.4294(6) 0.055(5) Uani 1 1 d . . . H5 H -0.3675 0.4203 0.4551 0.066 Uiso 1 1 calc R . . C6 C -0.1868(12) 0.4137(6) 0.4374(5) 0.040(4) Uani 1 1 d . . . H6 H -0.1549 0.4379 0.4681 0.048 Uiso 1 1 calc R . . C7 C 0.0891(11) 0.4241(6) 0.4526(5) 0.037(3) Uani 1 1 d . A . H7A H 0.0383 0.4569 0.464 0.045 Uiso 1 1 calc R . . H7B H 0.1699 0.4394 0.4413 0.045 Uiso 1 1 calc R . . C8 C 0.1158(12) 0.3871(6) 0.5079(5) 0.040(3) Uani 1 1 d . . . C12 C -0.1066(11) 0.2873(6) 0.2740(6) 0.047(4) Uani 1 1 d . . . H12A H -0.0595 0.2929 0.2387 0.057 Uiso 1 1 calc R . . H12B H -0.1956 0.2946 0.2626 0.057 Uiso 1 1 calc R . . C13 C -0.0930(12) 0.2248(6) 0.2927(6) 0.046(4) Uani 1 1 d . . . C14 C 0.0390(13) 0.2094(6) 0.3088(8) 0.070(5) Uani 1 1 d . . . H14A H 0.0902 0.2181 0.276 0.105 Uiso 1 1 calc R . . H14B H 0.0446 0.1688 0.3177 0.105 Uiso 1 1 calc R . . H14C H 0.0693 0.2313 0.3432 0.105 Uiso 1 1 calc R . . C15 C -0.1749(17) 0.2104(8) 0.3416(8) 0.096(7) Uani 1 1 d . . . H15A H -0.2614 0.2206 0.3299 0.144 Uiso 1 1 calc R . . H15B H -0.1469 0.2318 0.3767 0.144 Uiso 1 1 calc R . . H15C H -0.1696 0.1696 0.3498 0.144 Uiso 1 1 calc R . . C16 C -0.1335(17) 0.1887(9) 0.2374(9) 0.105(8) Uani 1 1 d . . . H16A H -0.0797 0.1979 0.2057 0.158 Uiso 1 1 calc R . . H16B H -0.2204 0.1975 0.2248 0.158 Uiso 1 1 calc R . . H16C H -0.126 0.1482 0.2468 0.158 Uiso 1 1 calc R . . C17 C 0.1926(10) 0.3857(5) 0.0410(5) 0.030(3) Uani 1 1 d . . . C18 C 0.3167(11) 0.4081(6) 0.0373(5) 0.034(3) Uani 1 1 d . . . C19 C 0.3349(13) 0.4489(6) -0.0084(6) 0.047(4) Uani 1 1 d . . . H19 H 0.4165 0.4629 -0.0135 0.057 Uiso 1 1 calc R . . C20 C 0.2375(13) 0.4679(7) -0.0446(6) 0.051(4) Uani 1 1 d . . . H20 H 0.2505 0.4969 -0.0724 0.062 Uiso 1 1 calc R . . C21 C 0.1210(14) 0.4452(7) -0.0406(6) 0.057(4) Uani 1 1 d . . . H21 H 0.0555 0.4561 -0.0682 0.068 Uiso 1 1 calc R . . C22 C 0.0974(11) 0.4070(6) 0.0021(5) 0.037(3) Uani 1 1 d . . . H22 H 0.0142 0.3945 0.0056 0.045 Uiso 1 1 calc R . . C23 C 0.0785(10) 0.3035(6) 0.0782(6) 0.036(3) Uani 1 1 d . . . H23A H 0.0071 0.3196 0.0542 0.044 Uiso 1 1 calc R . . H23B H 0.0486 0.2934 0.1168 0.044 Uiso 1 1 calc R . . C24 C 0.1229(12) 0.2491(6) 0.0485(6) 0.038(3) Uani 1 1 d . . . C25 C 0.2220(15) 0.2207(7) 0.0892(7) 0.075(5) Uani 1 1 d . . . H25A H 0.1879 0.2134 0.1271 0.112 Uiso 1 1 calc R . . H25B H 0.2947 0.2457 0.0946 0.112 Uiso 1 1 calc R . . H25C H 0.2472 0.1847 0.072 0.112 Uiso 1 1 calc R . . C26 C 0.0101(14) 0.2083(7) 0.0405(7) 0.076(5) Uani 1 1 d . . . H26A H -0.0219 0.2002 0.0787 0.115 Uiso 1 1 calc R . . H26B H 0.0364 0.1728 0.0227 0.115 Uiso 1 1 calc R . . H26C H -0.0556 0.2262 0.0151 0.115 Uiso 1 1 calc R . . C27 C 0.1727(16) 0.2603(7) -0.0094(7) 0.076(6) Uani 1 1 d . . . H27A H 0.1082 0.2787 -0.0351 0.115 Uiso 1 1 calc R . . H27B H 0.1971 0.2244 -0.0269 0.115 Uiso 1 1 calc R . . H27C H 0.2456 0.2853 -0.0044 0.115 Uiso 1 1 calc R . . C28 C 0.5394(10) 0.4017(6) 0.0737(6) 0.039(4) Uani 1 1 d . . . H28A H 0.5814 0.4087 0.1128 0.047 Uiso 1 1 calc R . . H28B H 0.5482 0.4365 0.0501 0.047 Uiso 1 1 calc R . . C29 C 0.6057(11) 0.3536(6) 0.0451(6) 0.044(4) Uani 1 1 d . . . C30 C 0.5493(14) 0.3385(8) -0.0159(7) 0.082(6) Uani 1 1 d . . . H30A H 0.5468 0.3725 -0.0406 0.123 Uiso 1 1 calc R . . H30B H 0.4644 0.3241 -0.013 0.123 Uiso 1 1 calc R . . H30C H 0.6005 0.3094 -0.0333 0.123 Uiso 1 1 calc R . . C31 C 0.7413(13) 0.3737(8) 0.0372(7) 0.079(6) Uani 1 1 d . . . H31A H 0.7395 0.4078 0.0126 0.119 Uiso 1 1 calc R . . H31B H 0.7873 0.3436 0.0184 0.119 Uiso 1 1 calc R . . H31C H 0.7827 0.3825 0.0755 0.119 Uiso 1 1 calc R . . C32 C 0.6071(16) 0.3002(7) 0.0823(8) 0.082(6) Uani 1 1 d . . . H32A H 0.6492 0.2696 0.0623 0.123 Uiso 1 1 calc R . . H32B H 0.5212 0.2887 0.0885 0.123 Uiso 1 1 calc R . . H32C H 0.6517 0.3077 0.1202 0.123 Uiso 1 1 calc R . . C33 C 0.1094(10) 0.4542(5) 0.2185(5) 0.023(3) Uani 1 1 d . . . C34 C 0.2329(10) 0.4615(5) 0.2493(6) 0.030(3) Uani 1 1 d . . . C35 C 0.3296(11) 0.4821(5) 0.2139(5) 0.035(3) Uani 1 1 d . . . H35 H 0.4113 0.4858 0.232 0.042 Uiso 1 1 calc R . . C36 C 0.3121(12) 0.4968(5) 0.1559(6) 0.037(3) Uani 1 1 d . . . H36 H 0.3786 0.5123 0.1356 0.045 Uiso 1 1 calc R . . C37 C 0.1968(11) 0.4887(6) 0.1278(6) 0.038(3) Uani 1 1 d . . . H37 H 0.1829 0.4988 0.0877 0.045 Uiso 1 1 calc R . . C38 C 0.1003(11) 0.4658(5) 0.1578(5) 0.032(3) Uani 1 1 d . . . H38 H 0.0239 0.4574 0.1363 0.038 Uiso 1 1 calc R . . C39 C -0.1103(9) 0.4378(5) 0.2275(5) 0.031(3) Uani 1 1 d . . . H39A H -0.1569 0.4051 0.2423 0.037 Uiso 1 1 calc R . . H39B H -0.1114 0.4344 0.1844 0.037 Uiso 1 1 calc R . . C40 C -0.1773(11) 0.4926(6) 0.2428(5) 0.037(3) Uani 1 1 d . . . C41 C -0.1160(11) 0.5439(5) 0.2138(6) 0.041(4) Uani 1 1 d . . . H41A H -0.0299 0.5481 0.2302 0.062 Uiso 1 1 calc R . . H41B H -0.1631 0.5785 0.2214 0.062 Uiso 1 1 calc R . . H41C H -0.1161 0.5376 0.1716 0.062 Uiso 1 1 calc R . . C42 C -0.3098(11) 0.4873(6) 0.2169(6) 0.048(4) Uani 1 1 d . . . H42A H -0.3091 0.4809 0.1747 0.071 Uiso 1 1 calc R . . H42B H -0.3556 0.5223 0.2242 0.071 Uiso 1 1 calc R . . H42C H -0.3506 0.4551 0.235 0.071 Uiso 1 1 calc R . . C43 C -0.1767(12) 0.5025(6) 0.3079(5) 0.047(4) Uani 1 1 d . . . H43A H -0.0904 0.5056 0.3243 0.071 Uiso 1 1 calc R . . H43B H -0.2178 0.4707 0.3263 0.071 Uiso 1 1 calc R . . H43C H -0.2214 0.5378 0.3154 0.071 Uiso 1 1 calc R . . C44 C 0.3547(11) 0.4640(5) 0.3411(5) 0.032(3) Uani 1 1 d . . . H44A H 0.4273 0.457 0.3176 0.039 Uiso 1 1 calc R . . H44B H 0.3633 0.4386 0.3756 0.039 Uiso 1 1 calc R . . C45 C 0.3622(11) 0.5259(6) 0.3631(6) 0.039(3) Uani 1 1 d . . . C46 C 0.3950(16) 0.5680(7) 0.3181(7) 0.083(6) Uani 1 1 d . . . H46A H 0.3307 0.5678 0.2857 0.124 Uiso 1 1 calc R . . H46B H 0.4757 0.558 0.3032 0.124 Uiso 1 1 calc R . . H46C H 0.4003 0.606 0.3356 0.124 Uiso 1 1 calc R . . C47 C 0.2364(14) 0.5459(7) 0.3853(8) 0.079(6) Uani 1 1 d . . . H47A H 0.2106 0.5196 0.4154 0.119 Uiso 1 1 calc R . . H47B H 0.1729 0.5466 0.3526 0.119 Uiso 1 1 calc R . . H47C H 0.2461 0.5841 0.402 0.119 Uiso 1 1 calc R . . C48 C 0.4618(19) 0.5276(8) 0.4119(9) 0.125(9) Uani 1 1 d . . . H48A H 0.4417 0.5003 0.4422 0.187 Uiso 1 1 calc R . . H48B H 0.4667 0.5659 0.4286 0.187 Uiso 1 1 calc R . . H48C H 0.5422 0.5175 0.3967 0.187 Uiso 1 1 calc R . . C49 C 0.4575(14) 0.1925(7) 0.3368(7) 0.067(5) Uani 1 1 d . . . H49A H 0.4995 0.2225 0.3611 0.081 Uiso 1 1 calc R . . H49B H 0.5224 0.1652 0.3262 0.081 Uiso 1 1 calc R . . C50 C 0.3684(16) 0.1624(8) 0.3728(8) 0.085(6) Uani 1 1 d . . . H50A H 0.4135 0.1464 0.4075 0.128 Uiso 1 1 calc R . . H50B H 0.3278 0.1317 0.3497 0.128 Uiso 1 1 calc R . . H50C H 0.3052 0.1892 0.3848 0.128 Uiso 1 1 calc R . . C51 C 0.3849(16) 0.1785(9) 0.2387(8) 0.088(6) Uani 1 1 d . . . H51A H 0.3042 0.1871 0.2172 0.106 Uiso 1 1 calc R . . H51B H 0.3787 0.14 0.2556 0.106 Uiso 1 1 calc R . . C52 C 0.4814(18) 0.1784(10) 0.1981(8) 0.116(8) Uani 1 1 d . . . H52A H 0.4622 0.1498 0.1678 0.174 Uiso 1 1 calc R . . H52B H 0.5616 0.1695 0.2189 0.174 Uiso 1 1 calc R . . H52C H 0.4861 0.216 0.1799 0.174 Uiso 1 1 calc R . . C9 C 0.220(2) 0.3459(13) 0.5013(12) 0.053(9) Uiso 0.53(2) 1 d P A 1 H9A H 0.1997 0.3212 0.4677 0.08 Uiso 0.53(2) 1 calc PR A 1 H9B H 0.2318 0.3228 0.5368 0.08 Uiso 0.53(2) 1 calc PR A 1 H9C H 0.2971 0.3668 0.4952 0.08 Uiso 0.53(2) 1 calc PR A 1 C10 C -0.002(2) 0.3507(12) 0.5288(11) 0.048(8) Uiso 0.53(2) 1 d P A 1 H10A H -0.0285 0.3235 0.4981 0.072 Uiso 0.53(2) 1 calc PR A 1 H10B H -0.0706 0.3764 0.536 0.072 Uiso 0.53(2) 1 calc PR A 1 H10C H 0.0236 0.3301 0.5648 0.072 Uiso 0.53(2) 1 calc PR A 1 C11 C 0.143(3) 0.4234(16) 0.5571(15) 0.090(13) Uiso 0.53(2) 1 d P A 1 H11A H 0.074 0.45 0.561 0.135 Uiso 0.53(2) 1 calc PR A 1 H11B H 0.2199 0.4448 0.5514 0.135 Uiso 0.53(2) 1 calc PR A 1 H11C H 0.1547 0.4004 0.5927 0.135 Uiso 0.53(2) 1 calc PR A 1 C9A C 0.257(3) 0.4021(15) 0.5284(14) 0.066(11) Uiso 0.47(2) 1 d P A 2 H9A1 H 0.3105 0.3943 0.4964 0.098 Uiso 0.47(2) 1 calc PR A 2 H9A2 H 0.2833 0.3788 0.5624 0.098 Uiso 0.47(2) 1 calc PR A 2 H9A3 H 0.2627 0.4424 0.539 0.098 Uiso 0.47(2) 1 calc PR A 2 C10A C 0.103(4) 0.3267(17) 0.4931(17) 0.089(15) Uiso 0.47(2) 1 d P A 2 H10D H 0.158 0.3174 0.4619 0.133 Uiso 0.47(2) 1 calc PR A 2 H10E H 0.0166 0.3185 0.4798 0.133 Uiso 0.47(2) 1 calc PR A 2 H10F H 0.1268 0.3037 0.5278 0.133 Uiso 0.47(2) 1 calc PR A 2 C11A C 0.034(3) 0.3984(17) 0.5552(15) 0.074(12) Uiso 0.47(2) 1 d P A 2 H11D H 0.0411 0.4384 0.5665 0.111 Uiso 0.47(2) 1 calc PR A 2 H11E H 0.0593 0.3744 0.5889 0.111 Uiso 0.47(2) 1 calc PR A 2 H11F H -0.0522 0.3898 0.5419 0.111 Uiso 0.47(2) 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 Zr1 0.0244(6) 0.0361(8) 0.0285(7) -0.0006(6) 0.0036(5) 0.0007(6) Zr2 0.0273(7) 0.0270(7) 0.0268(7) -0.0006(6) 0.0037(5) -0.0006(6) Li 0.047(14) 0.040(16) 0.059(16) 0.003(13) 0.029(12) 0.009(11) Cl1 0.0333(17) 0.031(2) 0.0332(19) -0.0005(15) 0.0064(14) -0.0025(14) Cl2 0.0329(17) 0.045(2) 0.041(2) 0.0067(17) 0.0034(15) 0.0014(16) Cl3 0.0348(18) 0.047(2) 0.039(2) 0.0040(17) 0.0017(15) 0.0056(16) O1 0.072(7) 0.036(6) 0.038(6) 0.007(5) 0.003(5) 0.013(5) N1 0.028(6) 0.039(7) 0.033(6) 0.003(5) -0.002(5) 0.002(5) N2 0.031(6) 0.037(7) 0.023(6) -0.001(5) -0.006(5) -0.008(5) N3 0.025(5) 0.026(6) 0.035(6) -0.003(5) 0.006(5) 0.001(5) N4 0.026(5) 0.037(7) 0.026(5) 0.001(5) -0.001(4) -0.003(5) N5 0.010(5) 0.032(6) 0.029(6) -0.004(5) 0.008(4) -0.003(4) N6 0.035(6) 0.030(7) 0.009(5) -0.005(5) 0.000(4) 0.007(5) C1 0.032(7) 0.053(10) 0.030(7) 0.016(8) 0.006(6) 0.011(7) C2 0.038(8) 0.038(9) 0.018(7) 0.005(6) 0.007(6) -0.006(6) C3 0.043(8) 0.043(9) 0.037(8) 0.009(7) -0.001(7) -0.008(7) C4 0.050(9) 0.069(12) 0.045(9) 0.014(9) 0.006(8) 0.005(8) C5 0.046(9) 0.073(13) 0.048(10) 0.023(9) 0.025(8) 0.031(8) C6 0.037(8) 0.050(10) 0.034(8) 0.007(7) 0.015(6) 0.007(7) C7 0.035(7) 0.046(10) 0.031(8) 0.003(7) 0.006(6) 0.008(7) C8 0.051(8) 0.035(9) 0.034(7) -0.007(7) -0.001(6) 0.009(7) C12 0.024(7) 0.065(12) 0.054(10) 0.001(9) 0.011(7) -0.001(7) C13 0.043(9) 0.036(10) 0.063(10) -0.002(8) 0.026(8) 0.001(7) C14 0.066(11) 0.027(10) 0.120(15) 0.004(10) 0.028(10) -0.013(8) C15 0.104(15) 0.054(13) 0.135(18) 0.019(12) 0.058(13) 0.017(11) C16 0.095(14) 0.090(16) 0.135(19) -0.061(14) 0.038(13) -0.045(12) C17 0.032(7) 0.027(8) 0.031(7) 0.004(7) 0.012(6) -0.003(6) C18 0.038(8) 0.037(9) 0.025(7) -0.005(6) 0.003(6) 0.008(6) C19 0.054(9) 0.044(10) 0.045(9) 0.016(8) 0.013(7) -0.022(8) C20 0.046(9) 0.062(12) 0.046(9) 0.024(8) -0.005(7) -0.005(8) C21 0.063(10) 0.069(12) 0.035(9) 0.014(9) -0.018(8) -0.005(9) C22 0.031(7) 0.043(9) 0.035(8) 0.005(7) -0.011(6) -0.018(6) C23 0.025(7) 0.045(9) 0.039(8) -0.002(7) 0.005(6) -0.012(6) C24 0.044(8) 0.029(8) 0.043(9) 0.000(7) 0.003(7) -0.021(7) C25 0.089(12) 0.043(11) 0.090(13) 0.011(10) -0.021(11) 0.010(9) C26 0.078(12) 0.066(13) 0.085(13) -0.006(11) 0.002(10) -0.035(10) C27 0.111(14) 0.064(13) 0.059(11) -0.028(10) 0.036(10) -0.030(11) C28 0.024(7) 0.048(10) 0.046(8) -0.008(7) 0.007(6) 0.005(6) C29 0.030(7) 0.043(10) 0.061(10) -0.015(8) 0.015(7) 0.000(7) C30 0.054(10) 0.101(16) 0.091(14) -0.052(12) 0.003(9) 0.015(10) C31 0.051(10) 0.098(16) 0.091(13) -0.020(12) 0.024(9) 0.002(10) C32 0.086(13) 0.054(13) 0.108(15) -0.005(11) 0.026(11) 0.031(10) C33 0.033(7) 0.019(7) 0.018(7) -0.004(6) -0.005(6) -0.001(5) C34 0.018(6) 0.020(8) 0.055(10) -0.020(7) 0.015(6) -0.001(5) C35 0.036(7) 0.030(8) 0.039(9) 0.002(7) 0.003(6) 0.001(6) C36 0.042(9) 0.025(8) 0.048(9) 0.002(7) 0.020(7) -0.002(6) C37 0.031(8) 0.038(9) 0.044(9) 0.009(7) 0.007(7) 0.013(6) C38 0.024(7) 0.032(8) 0.039(8) -0.001(6) 0.000(6) 0.006(6) C39 0.022(6) 0.027(8) 0.044(8) 0.008(7) 0.008(6) 0.001(6) C40 0.030(7) 0.041(9) 0.040(8) 0.016(7) 0.000(6) 0.009(6) C41 0.032(7) 0.031(9) 0.060(9) -0.005(7) -0.004(7) -0.005(6) C42 0.029(7) 0.057(11) 0.057(10) 0.003(8) 0.006(7) 0.002(7) C43 0.049(9) 0.054(11) 0.040(9) 0.004(8) 0.009(7) 0.023(7) C44 0.039(7) 0.034(9) 0.023(7) -0.011(6) -0.001(6) -0.001(6) C45 0.038(8) 0.037(9) 0.042(9) -0.011(7) 0.001(7) -0.004(6) C46 0.096(13) 0.076(14) 0.082(13) -0.020(11) 0.048(11) -0.038(11) C47 0.079(12) 0.037(11) 0.128(16) -0.017(10) 0.059(11) 0.005(9) C48 0.154(19) 0.070(16) 0.136(19) -0.042(14) -0.101(16) 0.033(14) C49 0.065(11) 0.060(12) 0.075(12) 0.007(10) -0.008(9) 0.028(9) C50 0.088(13) 0.089(16) 0.081(13) 0.033(12) 0.016(11) -0.012(11) C51 0.079(13) 0.107(18) 0.080(14) -0.016(13) 0.025(11) 0.003(12) C52 0.100(16) 0.16(2) 0.084(15) 0.011(16) 0.011(13) 0.011(16) #----------------------------------------------------------------------------# # 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 Zr1 N1 2.047(9) . ? Zr1 N2 2.129(9) . ? Zr1 N5 2.187(9) . ? Zr1 N6 2.229(10) . ? Zr1 Cl3 2.535(3) . ? Zr1 Cl1 2.848(3) . ? Zr2 N3 2.028(9) . ? Zr2 N4 2.056(9) . ? Zr2 C37 2.522(13) . ? Zr2 C36 2.528(13) . ? Zr2 Cl2 2.542(3) . ? Zr2 Cl1 2.654(3) . ? Li O1 1.87(3) . ? Li Cl3 2.33(2) . ? Li Cl2 2.36(2) . ? Li Cl1 2.43(2) . ? O1 C51 1.405(18) . ? O1 C49 1.424(16) . ? N1 C1 1.441(14) . ? N1 C7 1.462(15) . ? N2 C2 1.399(14) . ? N2 C12 1.481(16) . ? N3 C17 1.402(14) . ? N3 C23 1.465(14) . ? N4 C18 1.385(14) . ? N4 C28 1.481(13) . ? N5 C33 1.331(13) . ? N5 C39 1.503(13) . ? N6 C34 1.332(15) . ? N6 C44 1.473(14) . ? C1 C2 1.411(17) . ? C1 C6 1.417(16) . ? C2 C3 1.391(17) . ? C3 C4 1.347(18) . ? C4 C5 1.39(2) . ? C5 C6 1.369(18) . ? C7 C8 1.547(17) . ? C8 C11 1.43(4) . ? C8 C11A 1.46(3) . ? C8 C10A 1.47(4) . ? C8 C9 1.50(3) . ? C8 C9A 1.59(3) . ? C8 C10 1.62(3) . ? C12 C13 1.537(19) . ? C13 C14 1.486(19) . ? C13 C15 1.506(19) . ? C13 C16 1.57(2) . ? C17 C22 1.406(16) . ? C17 C18 1.441(16) . ? C18 C19 1.446(17) . ? C19 C20 1.367(18) . ? C20 C21 1.369(18) . ? C21 C22 1.364(18) . ? C23 C24 1.540(17) . ? C24 C27 1.487(18) . ? C24 C25 1.523(18) . ? C24 C26 1.547(17) . ? C28 C29 1.510(17) . ? C29 C32 1.52(2) . ? C29 C30 1.529(19) . ? C29 C31 1.554(18) . ? C33 C38 1.415(16) . ? C33 C34 1.471(15) . ? C34 C35 1.443(16) . ? C35 C36 1.376(17) . ? C36 C37 1.371(17) . ? C37 C38 1.390(16) . ? C39 C40 1.530(17) . ? C40 C43 1.510(17) . ? C40 C42 1.511(16) . ? C40 C41 1.546(17) . ? C44 C45 1.544(17) . ? C45 C46 1.49(2) . ? C45 C48 1.497(19) . ? C45 C47 1.547(17) . ? C49 C50 1.48(2) . ? C51 C52 1.44(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 N1 Zr1 N2 77.7(4) . . ? N1 Zr1 N5 111.3(4) . . ? N2 Zr1 N5 90.2(3) . . ? N1 Zr1 N6 108.2(4) . . ? N2 Zr1 N6 162.2(3) . . ? N5 Zr1 N6 72.0(3) . . ? N1 Zr1 Cl3 97.9(3) . . ? N2 Zr1 Cl3 110.4(3) . . ? N5 Zr1 Cl3 147.4(2) . . ? N6 Zr1 Cl3 85.8(2) . . ? N1 Zr1 Cl1 163.2(3) . . ? N2 Zr1 Cl1 88.2(3) . . ? N5 Zr1 Cl1 77.5(2) . . ? N6 Zr1 Cl1 88.0(2) . . ? Cl3 Zr1 Cl1 78.29(10) . . ? N3 Zr2 N4 82.4(4) . . ? N3 Zr2 C37 98.9(4) . . ? N4 Zr2 C37 96.2(4) . . ? N3 Zr2 C36 128.1(4) . . ? N4 Zr2 C36 88.4(4) . . ? C37 Zr2 C36 31.5(4) . . ? N3 Zr2 Cl2 128.4(3) . . ? N4 Zr2 Cl2 85.8(3) . . ? C37 Zr2 Cl2 132.3(3) . . ? C36 Zr2 Cl2 101.4(3) . . ? N3 Zr2 Cl1 82.9(3) . . ? N4 Zr2 Cl1 143.8(3) . . ? C37 Zr2 Cl1 118.7(3) . . ? C36 Zr2 Cl1 126.2(3) . . ? Cl2 Zr2 Cl1 77.81(10) . . ? O1 Li Cl3 105.8(11) . . ? O1 Li Cl2 122.0(10) . . ? Cl3 Li Cl2 126.0(11) . . ? O1 Li Cl1 120.0(12) . . ? Cl3 Li Cl1 91.4(7) . . ? Cl2 Li Cl1 85.8(8) . . ? Li Cl1 Zr2 95.8(5) . . ? Li Cl1 Zr1 88.5(5) . . ? Zr2 Cl1 Zr1 113.72(12) . . ? Li Cl2 Zr2 100.6(6) . . ? Li Cl3 Zr1 98.9(6) . . ? C51 O1 C49 112.6(13) . . ? C51 O1 Li 122.6(13) . . ? C49 O1 Li 124.8(12) . . ? C1 N1 C7 119.5(10) . . ? C1 N1 Zr1 112.7(8) . . ? C7 N1 Zr1 127.6(7) . . ? C2 N2 C12 116.8(9) . . ? C2 N2 Zr1 111.6(8) . . ? C12 N2 Zr1 129.5(7) . . ? C17 N3 C23 119.0(10) . . ? C17 N3 Zr2 94.6(7) . . ? C23 N3 Zr2 144.4(8) . . ? C18 N4 C28 120.4(10) . . ? C18 N4 Zr2 95.4(7) . . ? C28 N4 Zr2 138.4(7) . . ? C33 N5 C39 116.6(9) . . ? C33 N5 Zr1 112.3(7) . . ? C39 N5 Zr1 128.4(7) . . ? C34 N6 C44 118.0(10) . . ? C34 N6 Zr1 110.1(7) . . ? C44 N6 Zr1 129.3(7) . . ? C2 C1 C6 120.5(11) . . ? C2 C1 N1 115.8(10) . . ? C6 C1 N1 123.5(12) . . ? C3 C2 N2 128.2(12) . . ? C3 C2 C1 117.2(11) . . ? N2 C2 C1 114.5(10) . . ? C4 C3 C2 122.7(14) . . ? C3 C4 C5 119.7(13) . . ? C6 C5 C4 121.2(13) . . ? C5 C6 C1 118.6(13) . . ? N1 C7 C8 119.5(11) . . ? C11A C8 C10A 107(2) . . ? C11 C8 C9 110(2) . . ? C11 C8 C7 109.1(19) . . ? C11A C8 C7 114.6(17) . . ? C10A C8 C7 110.4(18) . . ? C9 C8 C7 112.5(14) . . ? C11A C8 C9A 110(2) . . ? C10A C8 C9A 111(2) . . ? C7 C8 C9A 103.8(15) . . ? C11 C8 C10 102.0(19) . . ? C9 C8 C10 106.7(17) . . ? C7 C8 C10 115.6(13) . . ? N2 C12 C13 116.4(12) . . ? C14 C13 C15 110.8(14) . . ? C14 C13 C12 112.0(11) . . ? C15 C13 C12 111.9(12) . . ? C14 C13 C16 106.2(13) . . ? C15 C13 C16 109.6(13) . . ? C12 C13 C16 106.0(14) . . ? N3 C17 C22 125.4(10) . . ? N3 C17 C18 116.5(10) . . ? C22 C17 C18 117.9(11) . . ? N4 C18 C17 116.7(11) . . ? N4 C18 C19 126.0(12) . . ? C17 C18 C19 117.2(11) . . ? C20 C19 C18 121.5(12) . . ? C19 C20 C21 119.9(13) . . ? C22 C21 C20 121.2(13) . . ? C21 C22 C17 122.0(12) . . ? N3 C23 C24 113.5(9) . . ? C27 C24 C25 110.3(13) . . ? C27 C24 C23 112.7(12) . . ? C25 C24 C23 108.6(11) . . ? C27 C24 C26 109.2(12) . . ? C25 C24 C26 108.1(12) . . ? C23 C24 C26 107.8(11) . . ? N4 C28 C29 114.6(11) . . ? C28 C29 C32 111.4(12) . . ? C28 C29 C30 113.6(12) . . ? C32 C29 C30 108.1(13) . . ? C28 C29 C31 107.1(12) . . ? C32 C29 C31 110.1(13) . . ? C30 C29 C31 106.4(12) . . ? N5 C33 C38 129.0(10) . . ? N5 C33 C34 114.0(10) . . ? C38 C33 C34 116.9(10) . . ? N6 C34 C35 128.6(11) . . ? N6 C34 C33 116.0(10) . . ? C35 C34 C33 115.5(11) . . ? C36 C35 C34 124.7(12) . . ? C37 C36 C35 118.8(12) . . ? C37 C36 Zr2 74.0(8) . . ? C35 C36 Zr2 80.8(8) . . ? C36 C37 C38 120.1(12) . . ? C36 C37 Zr2 74.5(7) . . ? C38 C37 Zr2 80.8(8) . . ? C37 C38 C33 123.7(11) . . ? N5 C39 C40 114.0(10) . . ? C43 C40 C42 110.2(10) . . ? C43 C40 C39 112.6(11) . . ? C42 C40 C39 106.6(11) . . ? C43 C40 C41 109.2(12) . . ? C42 C40 C41 108.2(10) . . ? C39 C40 C41 109.9(10) . . ? N6 C44 C45 117.0(10) . . ? C46 C45 C48 108.1(14) . . ? C46 C45 C44 114.3(11) . . ? C48 C45 C44 106.7(12) . . ? C46 C45 C47 106.1(13) . . ? C48 C45 C47 110.1(14) . . ? C44 C45 C47 111.5(11) . . ? O1 C49 C50 115.7(13) . . ? O1 C51 C52 113.7(17) . . ? #===END data_(4)-may1703 _database_code_depnum_ccdc_archive 'CCDC 289004' _audit_creation_date 2003-06-09T16:31:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H83 Ce Li1.82 N6 Na1.18 O0.5' _chemical_formula_sum 'C50 H83 Ce Li1.82 N6 Na1.18 O0.5' _chemical_formula_weight 956.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 20.7058(2) _cell_length_b 17.7310(2) _cell_length_c 17.3470(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6368.68(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 68538 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 0.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2022 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.754 _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 0.7834 _exptl_absorpt_correction_T_max 0.8471 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.384556E-1 _diffrn_orient_matrix_ub_12 -0.359951E-1 _diffrn_orient_matrix_ub_13 0.185581E-1 _diffrn_orient_matrix_ub_21 -0.428241E-1 _diffrn_orient_matrix_ub_22 -0.299531E-1 _diffrn_orient_matrix_ub_23 0.196819E-1 _diffrn_orient_matrix_ub_31 -0.32292E-2 _diffrn_orient_matrix_ub_32 -0.314316E-1 _diffrn_orient_matrix_ub_33 -0.400086E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_unetI/netI 0.0237 _diffrn_reflns_number 75050 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7495 _reflns_number_gt 6389 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is a complex disorder of the structure. Firstly , the group 1 cation is Li or Na, disordered over single unresolved sites. The ratio of Li:Na refined to 1.55:1 . Secondly, if one regards the three dangling benzene rings as forming a 'rotor' about the Ce atom , then there is an equal amount of the alterative with the rotor in the opposite direction, sharing common NCH2tBu groups and also common ' wing-tip ' carbon atoms of the benzene rings. Hydrogen atoms were omitted for these 'wing-tip' positions. There is also a poorly defined ether molecule loosely coordinated at Li1 , for which the atoms were left isotropic and SADI constraints were imposed . 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^)+(0.0763P)^2^+14.1269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding , or omitted' _refine_ls_extinction_method none _refine_ls_number_reflns 7495 _refine_ls_number_parameters 354 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.11 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.999 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.103 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' Li Li -0.0003 0.0001 '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' 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 Ce Ce 0.290314(13) 0.25 0.438198(16) 0.02985(11) Uani 1 2 d S . . Li1 Li 0.1384(5) 0.25 0.5329(5) 0.051(3) Uani 0.304(7) 2 d SP . . Li2 Li 0.4280(6) 0.25 0.5259(8) 0.068(3) Uani 0.304(7) 2 d SP . . Li3 Li 0.2854(4) 0.25 0.2457(7) 0.049(3) Uani 0.304(7) 2 d SP . . N1 N 0.1856(2) 0.3241(2) 0.4489(3) 0.0690(14) Uani 1 1 d . . . N2 N 0.3531(2) 0.3238(2) 0.5430(2) 0.0592(12) Uani 1 1 d . . . N3 N 0.3341(2) 0.3240(2) 0.3239(2) 0.0557(10) Uani 1 1 d . . . C3 C 0.1647(3) 0.2894(3) 0.2223(3) 0.0621(13) Uani 1 1 d . . . C4 C 0.1852(2) 0.4060(3) 0.4466(3) 0.0544(12) Uani 1 1 d . . . H4A H 0.206 0.4222 0.398 0.065 Uiso 1 1 calc R . . H4B H 0.2123 0.4247 0.4896 0.065 Uiso 1 1 calc R . . C5 C 0.1188(2) 0.4450(3) 0.4520(3) 0.0549(12) Uani 1 1 d . . . C6 C 0.1320(4) 0.5307(4) 0.4483(4) 0.099(2) Uani 1 1 d . . . H6A H 0.1604 0.5452 0.491 0.149 Uiso 1 1 calc R . . H6B H 0.0911 0.5582 0.4523 0.149 Uiso 1 1 calc R . . H6C H 0.153 0.543 0.3992 0.149 Uiso 1 1 calc R . . C7 C 0.0855(3) 0.4235(4) 0.5271(4) 0.0835(19) Uani 1 1 d . . . H7A H 0.1126 0.4387 0.5708 0.125 Uiso 1 1 calc R . . H7B H 0.0789 0.3688 0.5285 0.125 Uiso 1 1 calc R . . H7C H 0.0437 0.4491 0.5304 0.125 Uiso 1 1 calc R . . C8 C 0.0748(4) 0.4207(6) 0.3869(4) 0.115(3) Uani 1 1 d . . . H8A H 0.0948 0.4337 0.3374 0.173 Uiso 1 1 calc R . . H8B H 0.0332 0.4466 0.3916 0.173 Uiso 1 1 calc R . . H8C H 0.0681 0.3661 0.3895 0.173 Uiso 1 1 calc R . . C11 C 0.2004(3) 0.2895(3) 0.6724(3) 0.0638(14) Uani 1 1 d . . . C12 C 0.3546(3) 0.4058(2) 0.5486(3) 0.0508(11) Uani 1 1 d . . . H12A H 0.3096 0.4242 0.5532 0.061 Uiso 1 1 calc R . . H12B H 0.3725 0.4261 0.4999 0.061 Uiso 1 1 calc R . . C13 C 0.3941(2) 0.4381(3) 0.6161(3) 0.0561(12) Uani 1 1 d . . . C14 C 0.3907(4) 0.5242(3) 0.6096(5) 0.101(3) Uani 1 1 d . . . H14A H 0.3454 0.5404 0.6116 0.151 Uiso 1 1 calc R . . H14B H 0.4099 0.5402 0.5607 0.151 Uiso 1 1 calc R . . H14C H 0.4145 0.547 0.6525 0.151 Uiso 1 1 calc R . . C15 C 0.3656(4) 0.4122(5) 0.6939(3) 0.095(2) Uani 1 1 d . . . H15A H 0.3202 0.4277 0.6971 0.142 Uiso 1 1 calc R . . H15B H 0.3899 0.4353 0.7362 0.142 Uiso 1 1 calc R . . H15C H 0.3685 0.3572 0.6977 0.142 Uiso 1 1 calc R . . C16 C 0.4642(3) 0.4136(5) 0.6130(5) 0.104(3) Uani 1 1 d . . . H16A H 0.4667 0.3586 0.6175 0.155 Uiso 1 1 calc R . . H16B H 0.488 0.4369 0.6557 0.155 Uiso 1 1 calc R . . H16C H 0.4832 0.4295 0.5639 0.155 Uiso 1 1 calc R . . C19 C 0.5070(2) 0.2897(3) 0.4139(3) 0.0600(12) Uani 1 1 d . . . C20 C 0.3357(2) 0.4061(2) 0.3226(3) 0.0494(10) Uani 1 1 d . . . H20A H 0.3612 0.4235 0.3675 0.059 Uiso 1 1 calc R . . H20B H 0.291 0.4248 0.3297 0.059 Uiso 1 1 calc R . . C21 C 0.3634(3) 0.4428(3) 0.2504(3) 0.0578(12) Uani 1 1 d . . . C22 C 0.3604(4) 0.5284(3) 0.2622(4) 0.096(2) Uani 1 1 d . . . H22A H 0.3154 0.5438 0.2701 0.143 Uiso 1 1 calc R . . H22B H 0.3778 0.5539 0.2166 0.143 Uiso 1 1 calc R . . H22C H 0.386 0.5423 0.3075 0.143 Uiso 1 1 calc R . . C23 C 0.3260(5) 0.4201(5) 0.1800(4) 0.124(3) Uani 1 1 d . . . H23A H 0.2806 0.4344 0.1865 0.186 Uiso 1 1 calc R . . H23B H 0.3291 0.3654 0.1729 0.186 Uiso 1 1 calc R . . H23C H 0.3438 0.4458 0.1348 0.186 Uiso 1 1 calc R . . C24 C 0.4323(4) 0.4194(5) 0.2383(5) 0.115(3) Uani 1 1 d . . . H24A H 0.449 0.4433 0.1915 0.173 Uiso 1 1 calc R . . H24B H 0.4345 0.3645 0.2329 0.173 Uiso 1 1 calc R . . H24C H 0.4582 0.4353 0.2827 0.173 Uiso 1 1 calc R . . O1 O 0.0222 0.25 0.5614 0.230(14) Uiso 0.5 2 d SPD . . C25 C -0.0413(13) 0.25 0.5192(16) 0.128(9) Uiso 0.5 2 d SPD . . H25A H -0.0625 0.2941 0.5434 0.154 Uiso 0.25 1 calc PR . . H25B H -0.0625 0.2059 0.5434 0.154 Uiso 0.25 1 calc PR . . C26 C -0.003(2) 0.25 0.6450(17) 0.209(18) Uiso 0.5 2 d SPD . . H26A H -0.0324 0.294 0.6428 0.251 Uiso 0.25 1 calc PR . . H26B H -0.0324 0.206 0.6428 0.251 Uiso 0.25 1 calc PR . . C27 C -0.0742(19) 0.25 0.4406(17) 0.167(14) Uiso 0.5 2 d SPD . . H27A H -0.1212 0.25 0.4475 0.251 Uiso 0.5 2 calc SPR . . H27B H -0.0613 0.2049 0.4118 0.251 Uiso 0.25 1 calc PR . . H27C H -0.0613 0.2951 0.4118 0.251 Uiso 0.25 1 calc PR . . C28 C 0.013(2) 0.25 0.730(2) 0.23(2) Uiso 0.5 2 d SPD . . H28A H -0.0272 0.25 0.7596 0.34 Uiso 0.5 2 calc SPR . . H28B H 0.0381 0.2951 0.7421 0.34 Uiso 0.25 1 calc PR . . H28C H 0.0381 0.2049 0.7421 0.34 Uiso 0.25 1 calc PR . . C1 C 0.1737(4) 0.2922(5) 0.3587(5) 0.0391(17) Uani 0.5 1 d P . 1 C2 C 0.1691(5) 0.3276(5) 0.2858(5) 0.0455(19) Uani 0.5 1 d P . 1 H2 H 0.1693 0.3811 0.2833 0.055 Uiso 0.5 1 calc PR . 1 C9 C 0.2930(4) 0.2919(5) 0.5921(5) 0.0408(18) Uani 0.5 1 d P . 1 C10 C 0.2408(5) 0.3272(5) 0.6308(6) 0.053(2) Uani 0.5 1 d P . 1 H10 H 0.2354 0.3802 0.6259 0.064 Uiso 0.5 1 calc PR . 1 C17 C 0.4009(4) 0.2918(5) 0.3563(5) 0.0408(17) Uani 0.5 1 d P . 1 C18 C 0.4548(5) 0.3277(5) 0.3889(7) 0.056(2) Uani 0.5 1 d P . 1 H18 H 0.4544 0.3811 0.3935 0.067 Uiso 0.5 1 calc PR . 1 Li1A Li 0.1434(7) 0.25 0.3672(6) 0.062(3) Uani 0.304(7) 2 d SP . 2 Li2A Li 0.3161(8) 0.25 0.6216(9) 0.081(4) Uani 0.304(7) 2 d SP . 2 Li3A Li 0.4152(5) 0.25 0.3177(7) 0.055(3) Uani 0.304(7) 2 d SP . 2 C1A C 0.1904(3) 0.2910(4) 0.5342(4) 0.0307(14) Uani 0.5 1 d P . 2 C2A C 0.1983(4) 0.3281(5) 0.6049(5) 0.0367(16) Uani 0.5 1 d P . 2 H2A H 0.2023 0.3815 0.6056 0.044 Uiso 0.5 1 calc PR . 2 C9A C 0.4123(3) 0.2918(4) 0.4976(5) 0.0320(15) Uani 0.5 1 d P . 2 C10A C 0.4600(4) 0.3280(4) 0.4543(5) 0.0399(17) Uani 0.5 1 d P . 2 H10A H 0.4601 0.3815 0.4526 0.048 Uiso 0.5 1 calc PR . 2 C17A C 0.2726(4) 0.2913(4) 0.2850(4) 0.0329(15) Uani 0.5 1 d P . 2 C18A C 0.2168(5) 0.3276(5) 0.2560(6) 0.049(2) Uani 0.5 1 d P . 2 H18A H 0.2146 0.381 0.2596 0.059 Uiso 0.5 1 calc PR . 2 Na1 Na 0.1384(5) 0.25 0.5329(5) 0.051(3) Uani 0.196(7) 2 d SP . 3 Na2 Na 0.4280(6) 0.25 0.5259(8) 0.068(3) Uani 0.196(7) 2 d SP . 3 Na3 Na 0.2854(4) 0.25 0.2457(7) 0.049(3) Uani 0.196(7) 2 d SP . 3 Na1A Na 0.1434(7) 0.25 0.3672(6) 0.062(3) Uani 0.196(7) 2 d SP . 3 Na2A Na 0.3161(8) 0.25 0.6216(9) 0.081(4) Uani 0.196(7) 2 d SP . 3 Na3A Na 0.4152(5) 0.25 0.3177(7) 0.055(3) Uani 0.196(7) 2 d SP . 3 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 Ce 0.03422(17) 0.02295(16) 0.03239(17) 0 -0.00232(11) 0 Li1 0.077(7) 0.042(5) 0.033(4) 0 0.012(4) 0 Li2 0.072(8) 0.056(7) 0.075(8) 0 0.009(6) 0 Li3 0.039(5) 0.048(6) 0.061(6) 0 -0.014(4) 0 N1 0.0383(19) 0.0323(19) 0.136(5) -0.004(2) 0.024(2) 0.0045(16) N2 0.099(3) 0.0254(16) 0.053(2) -0.0050(15) -0.032(2) -0.0036(19) N3 0.083(3) 0.0343(17) 0.050(2) 0.0058(16) 0.023(2) 0.0001(18) C3 0.070(3) 0.047(3) 0.070(3) 0.004(2) -0.014(3) 0.003(2) C4 0.037(2) 0.036(2) 0.091(4) -0.003(2) 0.004(2) 0.0080(18) C5 0.048(2) 0.056(3) 0.061(3) -0.009(2) -0.010(2) 0.027(2) C6 0.124(6) 0.055(4) 0.119(6) 0.006(3) 0.009(5) 0.047(4) C7 0.079(4) 0.089(4) 0.083(4) -0.017(4) 0.018(3) 0.024(3) C8 0.078(4) 0.171(9) 0.097(5) 0.001(6) -0.046(4) 0.013(5) C11 0.094(4) 0.045(3) 0.052(3) -0.002(2) 0.015(3) 0.002(3) C12 0.070(3) 0.030(2) 0.053(2) -0.0050(17) -0.016(2) -0.0049(19) C13 0.050(2) 0.046(2) 0.072(3) -0.022(2) -0.011(2) -0.010(2) C14 0.112(6) 0.047(3) 0.144(7) -0.034(4) -0.026(5) -0.016(3) C15 0.109(5) 0.119(6) 0.056(3) -0.020(4) -0.012(3) -0.010(5) C16 0.055(3) 0.111(6) 0.145(7) -0.016(5) -0.014(4) 0.002(4) C19 0.046(2) 0.047(3) 0.088(4) 0.002(3) 0.002(2) -0.005(2) C20 0.063(3) 0.036(2) 0.050(2) 0.0100(18) 0.016(2) 0.0007(19) C21 0.070(3) 0.052(3) 0.052(3) 0.017(2) 0.005(2) -0.013(2) C22 0.133(6) 0.053(3) 0.101(5) 0.038(3) 0.003(5) -0.015(4) C23 0.192(10) 0.114(6) 0.066(4) 0.024(4) -0.045(5) -0.027(7) C24 0.085(5) 0.113(6) 0.147(7) 0.003(5) 0.064(5) -0.014(5) C1 0.035(4) 0.041(5) 0.041(4) 0.000(3) 0.004(3) 0.004(3) C2 0.053(5) 0.039(4) 0.044(4) 0.006(4) -0.008(4) 0.003(4) C9 0.052(5) 0.032(4) 0.039(4) 0.000(3) -0.007(4) -0.001(4) C10 0.066(6) 0.036(4) 0.057(6) -0.002(4) 0.005(5) 0.001(4) C17 0.038(4) 0.035(4) 0.050(5) 0.004(4) 0.003(3) 0.002(3) C18 0.052(5) 0.031(4) 0.085(7) 0.004(4) -0.006(5) -0.004(4) Li1A 0.081(8) 0.049(6) 0.057(6) 0 0.014(6) 0 Li2A 0.092(10) 0.052(7) 0.097(10) 0 -0.004(8) 0 Li3A 0.057(6) 0.043(5) 0.066(7) 0 -0.005(5) 0 C1A 0.028(3) 0.034(4) 0.030(3) 0.003(3) 0.006(3) 0.004(3) C2A 0.037(4) 0.033(4) 0.040(4) -0.005(3) 0.001(3) 0.000(3) C9A 0.028(3) 0.022(4) 0.045(4) -0.002(3) -0.006(3) 0.003(3) C10A 0.037(4) 0.028(4) 0.055(5) 0.001(3) 0.004(3) -0.006(3) C17A 0.038(4) 0.030(4) 0.031(3) 0.002(3) -0.003(3) -0.001(3) C18A 0.062(6) 0.030(4) 0.055(5) 0.005(4) -0.011(4) 0.005(4) Na1 0.077(7) 0.042(5) 0.033(4) 0 0.012(4) 0 Na2 0.072(8) 0.056(7) 0.075(8) 0 0.009(6) 0 Na3 0.039(5) 0.048(6) 0.061(6) 0 -0.014(4) 0 Na1A 0.081(8) 0.049(6) 0.057(6) 0 0.014(6) 0 Na2A 0.092(10) 0.052(7) 0.097(10) 0 -0.004(8) 0 Na3A 0.057(6) 0.043(5) 0.066(7) 0 -0.005(5) 0 #----------------------------------------------------------------------------# # 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 Ce N1 2.541(4) . ? Ce N3 2.545(4) . ? Ce N2 2.590(4) . ? Ce C1A 2.753(7) . ? Ce C9 2.772(9) . ? Ce C17A 2.781(7) . ? Li1 N1 2.191(9) . ? Li1 O1 2.456(11) . ? Li2 N2 2.050(11) . ? Li2 C19 2.635(13) . ? Li3 N3 2.139(9) . ? Li3 C3 2.627(10) . ? N1 C4 1.454(6) . ? N1 C1A 1.594(9) . ? N1 C1 1.681(10) . ? N1 Li1A 2.121(11) . ? N2 C12 1.457(5) . ? N2 C9A 1.563(9) . ? N2 C9 1.612(10) . ? N2 Li2A 2.039(13) . ? N3 C20 1.457(5) . ? N3 C17A 1.553(9) . ? N3 C17 1.598(9) . ? N3 Li3A 2.133(9) . ? C3 C2 1.296(10) . ? C3 C3 1.399(10) 8_565 ? C4 C5 1.541(6) . ? C5 C8 1.513(8) . ? C5 C7 1.523(8) . ? C5 C6 1.545(8) . ? C11 C10 1.293(11) . ? C11 C2A 1.359(10) . ? C11 C11 1.399(10) 8_565 ? C12 C13 1.539(6) . ? C13 C16 1.517(8) . ? C13 C14 1.531(8) . ? C13 C15 1.542(9) . ? C19 C18 1.346(11) . ? C19 C10A 1.378(10) . ? C19 C19 1.408(10) 8_565 ? C20 C21 1.524(6) . ? C21 C24 1.500(9) . ? C21 C23 1.500(9) . ? C21 C22 1.534(8) . ? O1 C25 1.51(2) . ? O1 C26 1.54(3) . ? C25 C27 1.52(3) . ? C26 C28 1.50(3) . ? C1 C2 1.415(11) . ? C1 C1 1.498(17) 8_565 ? C9 C10 1.418(13) . ? C9 C9 1.485(16) 8_565 ? C17 C18 1.403(13) . ? C17 C17 1.481(16) 8_565 ? Li1A N1 2.121(11) 8_565 ? Li2A N2 2.039(13) 8_565 ? Li3A N3 2.133(9) 8_565 ? C1A C2A 1.401(11) . ? C1A C1A 1.454(15) 8_565 ? C9A C10A 1.397(11) . ? C9A C9A 1.482(14) 8_565 ? C17A C18A 1.414(11) . ? C17A C17A 1.465(15) 8_565 ? 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 Ce N1 62.22(19) 8_565 . ? N1 Ce N3 95.44(15) 8_565 8_565 ? N1 Ce N3 128.85(17) . 8_565 ? N1 Ce N3 128.85(17) 8_565 . ? N1 Ce N3 95.44(15) . . ? N3 Ce N3 62.04(17) 8_565 . ? N1 Ce N2 129.65(17) 8_565 . ? N1 Ce N2 96.67(16) . . ? N3 Ce N2 128.93(16) 8_565 . ? N3 Ce N2 96.18(15) . . ? N1 Ce N2 96.67(16) 8_565 8_565 ? N1 Ce N2 129.65(17) . 8_565 ? N3 Ce N2 96.18(15) 8_565 8_565 ? N3 Ce N2 128.93(16) . 8_565 ? N2 Ce N2 60.68(16) . 8_565 ? N1 Li1 N1 73.6(4) 8_565 . ? N1 Li1 O1 124.8(4) . . ? C9A Li2 C9A 103.2(17) 8_565 . ? N2 Li2 N2 79.3(5) 8_565 . ? N2 Li2 C19 138.3(6) 8_565 . ? N2 Li2 C19 113.9(4) . . ? N2 Li2 C19 113.9(4) 8_565 8_565 ? N2 Li2 C19 138.3(6) . 8_565 ? N3 Li3 N3 75.6(4) . 8_565 ? N3 Li3 C3 135.2(5) . 8_565 ? N3 Li3 C3 112.5(3) 8_565 8_565 ? N3 Li3 C3 112.5(3) . . ? N3 Li3 C3 135.2(5) 8_565 . ? C4 N1 C1A 113.1(5) . . ? C4 N1 C1 108.0(5) . . ? C4 N1 Li1A 126.7(5) . . ? C1A N1 Li1A 114.7(4) . . ? C4 N1 Li1 127.9(4) . . ? C1 N1 Li1 110.6(4) . . ? C4 N1 Ce 121.3(3) . . ? C1A N1 Ce 79.9(3) . . ? C1 N1 Ce 83.3(3) . . ? Li1A N1 Ce 89.0(3) . . ? Li1 N1 Ce 96.9(3) . . ? C12 N2 C9A 112.3(5) . . ? C12 N2 C9 109.3(5) . . ? C12 N2 Li2A 127.1(5) . . ? C9A N2 Li2A 113.5(5) . . ? C12 N2 Li2 129.1(4) . . ? C9 N2 Li2 115.9(4) . . ? C12 N2 Ce 124.1(3) . . ? C9A N2 Ce 81.8(3) . . ? C9 N2 Ce 78.8(3) . . ? Li2A N2 Ce 87.5(4) . . ? Li2 N2 Ce 87.5(4) . . ? C20 N3 C17A 112.6(4) . . ? C20 N3 C17 110.1(5) . . ? C20 N3 Li3A 126.7(4) . . ? C17A N3 Li3A 113.2(4) . . ? C20 N3 Li3 127.9(4) . . ? C17 N3 Li3 114.3(4) . . ? C20 N3 Ce 122.3(3) . . ? C17A N3 Ce 81.6(3) . . ? C17 N3 Ce 81.3(3) . . ? Li3A N3 Ce 90.1(3) . . ? Li3 N3 Ce 90.6(3) . . ? C2 C3 C3 121.4(4) . 8_565 ? C3 C3 C18A 118.9(4) 8_565 . ? N1 C4 C5 116.9(4) . . ? C8 C5 C7 107.2(6) . . ? C8 C5 C4 111.3(5) . . ? C7 C5 C4 110.0(4) . . ? C8 C5 C6 110.8(6) . . ? C7 C5 C6 111.2(5) . . ? C4 C5 C6 106.3(5) . . ? C10 C11 C11 121.2(5) . 8_565 ? C2A C11 C11 120.3(4) . 8_565 ? N2 C12 C13 115.7(4) . . ? C16 C13 C14 109.1(5) . . ? C16 C13 C12 112.0(5) . . ? C14 C13 C12 106.9(5) . . ? C16 C13 C15 108.2(6) . . ? C14 C13 C15 110.1(6) . . ? C12 C13 C15 110.6(4) . . ? C18 C19 C19 120.0(4) . 8_565 ? C10A C19 C19 119.5(4) . 8_565 ? N3 C20 C21 116.5(4) . . ? C24 C21 C23 107.7(7) . . ? C24 C21 C20 110.8(5) . . ? C23 C21 C20 111.1(5) . . ? C24 C21 C22 109.3(5) . . ? C23 C21 C22 110.6(6) . . ? C20 C21 C22 107.3(5) . . ? C25 O1 C26 99.3(19) . . ? C25 O1 Li1 139.3(11) . . ? C26 O1 Li1 121.5(16) . . ? O1 C25 C27 146(3) . . ? C28 C26 O1 147(4) . . ? C2 C1 C1 116.3(5) . 8_565 ? C2 C1 N1 133.9(7) . . ? C1 C1 N1 109.6(3) 8_565 . ? C3 C2 C1 122.3(8) . . ? C10 C9 C9 116.3(5) . 8_565 ? C10 C9 N2 133.1(7) . . ? C9 C9 N2 110.6(3) 8_565 . ? C11 C10 C9 121.9(8) . . ? C18 C17 C17 117.0(5) . 8_565 ? C18 C17 N3 131.9(7) . . ? C17 C17 N3 110.9(3) 8_565 . ? C19 C18 C17 122.8(8) . . ? N1 Li1A N1 76.5(5) . 8_565 ? N2 Li2A N2 79.8(6) 8_565 . ? N3 Li3A N3 75.9(4) 8_565 . ? C10A C9A C9A 117.3(4) . 8_565 ? C10A C9A N2 131.2(6) . . ? C9A C9A N2 111.3(3) 8_565 . ? C19 C10A C9A 123.1(7) . . ? C18A C17A C17A 117.1(5) . 8_565 ? C18A C17A N3 130.9(7) . . ? C17A C17A N3 111.9(3) 8_565 . ? C3 C18A C17A 123.9(7) . . ? #===END data_(5)-jul2403 _database_code_depnum_ccdc_archive 'CCDC 289005' _audit_creation_date 2003-07-21T16:44:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C52 H88 Ce1 N6 Na3 O1' _chemical_formula_sum 'C52 H88 Ce1 N6 Na3 O1' _chemical_formula_weight 1022.37 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 28.8173(8) _cell_length_b 17.9042(4) _cell_length_c 12.1605(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6274.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 633101 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.781 _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 0.453 _exptl_absorpt_correction_T_max 0.790 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.394043E-1 _diffrn_orient_matrix_ub_12 0.04902 _diffrn_orient_matrix_ub_13 -0.3395E-3 _diffrn_orient_matrix_ub_21 0.22071E-2 _diffrn_orient_matrix_ub_22 -0.1962E-3 _diffrn_orient_matrix_ub_23 0.346887E-1 _diffrn_orient_matrix_ub_31 0.721441E-1 _diffrn_orient_matrix_ub_32 -0.267682E-1 _diffrn_orient_matrix_ub_33 -0.8758E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1369 _diffrn_reflns_av_unetI/netI 0.0561 _diffrn_reflns_number 47631 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.944 _diffrn_measured_fraction_theta_max 0.944 _reflns_number_total 5437 _reflns_number_gt 4528 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C27-C28 ethyl group is disordered across the crystallographic mirror plane. There is residual electron density up to 1.3 electrons which could not be interpreted , but probably represents very disordered solvate. 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^+40.0347P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 5437 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.091 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2177 _refine_ls_wR_factor_gt 0.2084 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_restrained_S_all 1.208 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.445 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.128 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' O O 0.0106 0.006 '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 Ce Ce 0.136946(19) 0.25 0.34929(5) 0.0323(2) Uani 1 2 d S . . Na1 Na 0.23639(16) 0.25 0.2135(4) 0.0507(11) Uani 1 2 d S . . Na2 Na 0.13777(17) 0.25 0.6221(4) 0.0526(12) Uani 1 2 d S . . Na3 Na 0.03585(16) 0.25 0.1959(4) 0.0554(12) Uani 1 2 d S . . O O -0.0215(4) 0.25 0.0503(10) 0.088(3) Uani 1 2 d S . . N1 N 0.2124(2) 0.1758(3) 0.3663(5) 0.0419(15) Uani 1 1 d . . . N2 N 0.0935(2) 0.1758(3) 0.4941(5) 0.0412(15) Uani 1 1 d . . . N3 N 0.1059(2) 0.1752(3) 0.1865(6) 0.0410(15) Uani 1 1 d . . . C1 C 0.2191(3) 0.2089(4) 0.4703(6) 0.0394(17) Uani 1 1 d . . . C2 C 0.2230(3) 0.1739(5) 0.5717(7) 0.049(2) Uani 1 1 d . . . H2 H 0.2233 0.1209 0.5729 0.059 Uiso 1 1 calc R . . C3 C 0.2264(4) 0.2117(5) 0.6732(7) 0.057(2) Uani 1 1 d . . . H3 H 0.2287 0.1847 0.7402 0.068 Uiso 1 1 calc R . . C4 C 0.2156(3) 0.0935(4) 0.3635(7) 0.0456(19) Uani 1 1 d . . . H4A H 0.1935 0.0749 0.3075 0.055 Uiso 1 1 calc R . . H4B H 0.2053 0.074 0.4356 0.055 Uiso 1 1 calc R . . C5 C 0.2639(3) 0.0603(5) 0.3380(9) 0.064(3) Uani 1 1 d . . . C6 C 0.2581(5) -0.0247(6) 0.3366(14) 0.116(5) Uani 1 1 d . . . H6A H 0.2472 -0.0416 0.4088 0.173 Uiso 1 1 calc R . . H6B H 0.288 -0.0482 0.32 0.173 Uiso 1 1 calc R . . H6C H 0.2354 -0.0386 0.2803 0.173 Uiso 1 1 calc R . . C7 C 0.2811(6) 0.0881(9) 0.2292(13) 0.140(7) Uani 1 1 d . . . H7A H 0.285 0.1424 0.2325 0.21 Uiso 1 1 calc R . . H7B H 0.2585 0.0755 0.1719 0.21 Uiso 1 1 calc R . . H7C H 0.3109 0.0646 0.2122 0.21 Uiso 1 1 calc R . . C8 C 0.2993(4) 0.0798(8) 0.4281(14) 0.115(5) Uani 1 1 d . . . H8A H 0.2882 0.0607 0.499 0.172 Uiso 1 1 calc R . . H8B H 0.3029 0.1341 0.4324 0.172 Uiso 1 1 calc R . . H8C H 0.3292 0.0569 0.4105 0.172 Uiso 1 1 calc R . . C9 C 0.0533(3) 0.2092(4) 0.4583(7) 0.0400(17) Uani 1 1 d . . . C10 C 0.0140(3) 0.1735(5) 0.4140(7) 0.0442(19) Uani 1 1 d . . . H10 H 0.0138 0.1205 0.4117 0.053 Uiso 1 1 calc R . . C11 C -0.0241(3) 0.2108(5) 0.3740(7) 0.049(2) Uani 1 1 d . . . H11 H -0.0501 0.1839 0.3467 0.058 Uiso 1 1 calc R . . C12 C 0.0947(3) 0.0940(4) 0.5063(7) 0.0459(19) Uani 1 1 d . . . H12A H 0.1267 0.0767 0.4903 0.055 Uiso 1 1 calc R . . H12B H 0.0741 0.0719 0.45 0.055 Uiso 1 1 calc R . . C13 C 0.0803(3) 0.0628(5) 0.6201(7) 0.048(2) Uani 1 1 d . . . C14 C 0.1119(4) 0.0938(6) 0.7092(8) 0.069(3) Uani 1 1 d . . . H14A H 0.1443 0.0819 0.6914 0.103 Uiso 1 1 calc R . . H14B H 0.1038 0.0713 0.7801 0.103 Uiso 1 1 calc R . . H14C H 0.1081 0.1481 0.7136 0.103 Uiso 1 1 calc R . . C15 C 0.0875(4) -0.0216(5) 0.6153(9) 0.070(3) Uani 1 1 d . . . H15A H 0.12 -0.0324 0.5975 0.105 Uiso 1 1 calc R . . H15B H 0.0673 -0.043 0.5586 0.105 Uiso 1 1 calc R . . H15C H 0.0798 -0.0436 0.6869 0.105 Uiso 1 1 calc R . . C16 C 0.0304(3) 0.0811(6) 0.6462(9) 0.071(3) Uani 1 1 d . . . H16A H 0.0265 0.1354 0.6493 0.107 Uiso 1 1 calc R . . H16B H 0.022 0.0593 0.7174 0.107 Uiso 1 1 calc R . . H16C H 0.0102 0.0605 0.5888 0.107 Uiso 1 1 calc R . . C17 C 0.1395(3) 0.2094(5) 0.1200(6) 0.0405(18) Uani 1 1 d . . . C18 C 0.1752(3) 0.1736(5) 0.0593(7) 0.048(2) Uani 1 1 d . . . H18 H 0.1762 0.1206 0.0591 0.057 Uiso 1 1 calc R . . C19 C 0.2086(3) 0.2117(5) 0.0004(7) 0.050(2) Uani 1 1 d . . . H19 H 0.2314 0.185 -0.0399 0.06 Uiso 1 1 calc R . . C20 C 0.1068(3) 0.0941(4) 0.1964(7) 0.0451(19) Uani 1 1 d . . . H20A H 0.0995 0.0812 0.2736 0.054 Uiso 1 1 calc R . . H20B H 0.1389 0.0771 0.1819 0.054 Uiso 1 1 calc R . . C21 C 0.0743(3) 0.0494(5) 0.1222(7) 0.047(2) Uani 1 1 d . . . C22 C 0.0799(4) -0.0334(5) 0.1523(10) 0.075(3) Uani 1 1 d . . . H22A H 0.1122 -0.0485 0.1414 0.113 Uiso 1 1 calc R . . H22B H 0.0597 -0.0638 0.1053 0.113 Uiso 1 1 calc R . . H22C H 0.0713 -0.0409 0.2295 0.113 Uiso 1 1 calc R . . C23 C 0.0869(4) 0.0575(6) 0.0016(8) 0.068(3) Uani 1 1 d . . . H23A H 0.1192 0.0422 -0.0095 0.102 Uiso 1 1 calc R . . H23B H 0.0831 0.1097 -0.0208 0.102 Uiso 1 1 calc R . . H23C H 0.0665 0.0258 -0.0429 0.102 Uiso 1 1 calc R . . C24 C 0.0245(3) 0.0725(6) 0.1382(8) 0.063(3) Uani 1 1 d . . . H24A H 0.0161 0.0672 0.2159 0.094 Uiso 1 1 calc R . . H24B H 0.0043 0.0407 0.0934 0.094 Uiso 1 1 calc R . . H24C H 0.0207 0.1247 0.1158 0.094 Uiso 1 1 calc R . . C25 C -0.0155(9) 0.25 -0.0660(18) 0.121(7) Uani 1 2 d S . . H25A H -0.0312 0.2054 -0.0966 0.145 Uiso 0.5 1 calc PR . . H25B H -0.0312 0.2946 -0.0966 0.145 Uiso 0.5 1 calc PR . . C26 C 0.0298(9) 0.25 -0.102(2) 0.129(8) Uani 1 2 d S . . H26A H 0.0306 0.25 -0.1821 0.193 Uiso 1 2 calc SR . . H26B H 0.0456 0.2053 -0.0739 0.193 Uiso 0.5 1 calc PR . . H26C H 0.0456 0.2947 -0.0739 0.193 Uiso 0.5 1 calc PR . . C27 C -0.0712(9) 0.2205(14) 0.081(2) 0.093(9) Uani 0.5 1 d P . . H27A H -0.083 0.1864 0.0234 0.112 Uiso 0.5 1 calc PR . . H27B H -0.0705 0.1934 0.1519 0.112 Uiso 0.5 1 calc PR . . C28 C -0.1012(10) 0.289(2) 0.089(4) 0.18(2) Uani 0.5 1 d P . . H28A H -0.1329 0.2744 0.1088 0.273 Uiso 0.5 1 calc PR . . H28B H -0.1014 0.3151 0.0185 0.273 Uiso 0.5 1 calc PR . . H28C H -0.0888 0.3223 0.1462 0.273 Uiso 0.5 1 calc PR . . 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 Ce 0.0366(4) 0.0287(3) 0.0317(4) 0 0.0017(2) 0 Na1 0.053(3) 0.057(3) 0.042(3) 0 0.006(2) 0 Na2 0.071(3) 0.053(3) 0.034(3) 0 -0.005(2) 0 Na3 0.045(3) 0.069(3) 0.052(3) 0 0.002(2) 0 O 0.072(7) 0.119(10) 0.073(8) 0 -0.016(6) 0 N1 0.046(4) 0.034(3) 0.045(4) 0.002(3) -0.008(3) 0.003(3) N2 0.053(4) 0.039(4) 0.032(4) 0.004(3) 0.007(3) -0.005(3) N3 0.046(4) 0.035(3) 0.042(4) -0.004(3) -0.003(3) -0.007(3) C1 0.048(4) 0.040(4) 0.031(4) 0.002(3) -0.008(3) 0.007(3) C2 0.071(6) 0.038(4) 0.037(5) 0.006(4) -0.007(4) 0.001(4) C3 0.094(7) 0.054(5) 0.023(5) 0.009(4) -0.016(4) 0.001(5) C4 0.052(5) 0.037(4) 0.047(5) -0.007(4) -0.004(4) 0.008(3) C5 0.060(6) 0.053(5) 0.079(7) 0.003(5) 0.007(5) 0.021(4) C6 0.110(10) 0.061(7) 0.176(16) -0.024(9) 0.011(10) 0.042(7) C7 0.136(13) 0.158(14) 0.127(13) 0.041(11) 0.077(11) 0.085(11) C8 0.062(7) 0.100(10) 0.182(16) -0.032(10) -0.027(9) 0.028(7) C9 0.043(4) 0.040(4) 0.037(5) 0.002(3) 0.006(3) 0.000(3) C10 0.047(4) 0.047(5) 0.039(5) 0.000(4) 0.003(3) -0.006(4) C11 0.039(4) 0.049(4) 0.057(6) -0.009(4) 0.006(4) -0.003(4) C12 0.055(5) 0.032(4) 0.052(5) 0.003(4) 0.007(4) -0.002(3) C13 0.064(5) 0.048(5) 0.033(5) 0.014(4) 0.003(4) -0.007(4) C14 0.092(7) 0.076(7) 0.037(6) 0.011(5) 0.000(5) -0.013(6) C15 0.091(7) 0.047(5) 0.072(7) 0.019(5) -0.002(6) -0.009(5) C16 0.068(6) 0.080(7) 0.066(7) 0.021(6) 0.016(5) 0.000(5) C17 0.041(4) 0.050(4) 0.030(5) -0.008(3) 0.002(3) -0.004(3) C18 0.057(5) 0.037(4) 0.049(5) 0.000(4) 0.003(4) 0.003(4) C19 0.049(5) 0.054(5) 0.048(6) -0.003(4) 0.015(4) 0.004(4) C20 0.057(5) 0.038(4) 0.040(5) 0.000(4) 0.001(4) -0.004(4) C21 0.063(5) 0.042(5) 0.036(5) -0.006(3) 0.006(4) -0.014(4) C22 0.096(8) 0.047(6) 0.083(8) -0.007(5) -0.003(6) -0.014(5) C23 0.080(7) 0.075(7) 0.050(6) -0.020(5) 0.003(5) -0.023(5) C24 0.060(6) 0.066(6) 0.063(7) 0.000(5) -0.004(5) -0.019(5) C25 0.15(2) 0.14(2) 0.075(16) 0 -0.014(14) 0 C26 0.124(19) 0.128(19) 0.13(2) 0 0.019(16) 0 C27 0.099(19) 0.10(2) 0.079(18) 0.004(13) -0.024(15) -0.001(14) C28 0.061(17) 0.18(4) 0.30(6) 0.03(3) 0.03(3) 0.05(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce N2 2.537(6) . ? Ce N3 2.551(6) . ? Ce N1 2.556(6) . ? Na1 N1 2.387(8) . ? Na2 N2 2.412(7) . ? Na3 O 2.422(12) . ? Na3 N3 2.425(7) . ? O C25 1.43(2) . ? O C27 1.57(3) . ? N1 C1 1.410(10) . ? N1 C4 1.477(10) . ? N2 C9 1.374(10) . ? N2 C12 1.472(9) . ? N3 C17 1.403(10) . ? N3 C20 1.457(10) . ? C1 C2 1.388(11) . ? C1 C1 1.470(15) 8_565 ? C2 C3 1.411(12) . ? C3 C3 1.371(17) 8_565 ? C4 C5 1.546(12) . ? C5 C7 1.497(16) . ? C5 C6 1.530(15) . ? C5 C8 1.536(16) . ? C9 C10 1.407(11) . ? C9 C9 1.460(15) 8_565 ? C10 C11 1.374(11) . ? C11 C11 1.404(17) 8_565 ? C12 C13 1.549(11) . ? C13 C16 1.509(13) . ? C13 C14 1.521(13) . ? C13 C15 1.526(12) . ? C17 C18 1.419(11) . ? C17 C17 1.453(16) 8_565 ? C18 C19 1.379(11) . ? C19 C19 1.372(17) 8_565 ? C20 C21 1.527(11) . ? C21 C24 1.507(13) . ? C21 C23 1.518(12) . ? C21 C22 1.536(13) . ? C25 C26 1.38(3) . ? C27 C28 1.51(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 Ce N2 63.2(3) . 8_565 ? N2 Ce N3 95.2(2) . . ? N2 Ce N3 129.8(2) 8_565 . ? N2 Ce N3 129.8(2) . 8_565 ? N2 Ce N3 95.2(2) 8_565 8_565 ? N3 Ce N3 63.3(3) . 8_565 ? N2 Ce N1 129.5(2) . 8_565 ? N2 Ce N1 95.2(2) 8_565 8_565 ? N3 Ce N1 129.3(2) . 8_565 ? N3 Ce N1 95.1(2) 8_565 8_565 ? N2 Ce N1 95.2(2) . . ? N2 Ce N1 129.5(2) 8_565 . ? N3 Ce N1 95.1(2) . . ? N3 Ce N1 129.3(2) 8_565 . ? N1 Ce N1 62.6(3) 8_565 . ? N1 Na1 N1 67.6(3) . 8_565 ? N2 Na2 N2 66.9(3) . 8_565 ? O Na3 N3 122.3(3) . 8_565 ? C25 O C27 110.3(15) . . ? C25 O C27 110.3(15) . 8_565 ? C27 O C27 39.4(19) . 8_565 ? C25 O Na3 129.9(12) . . ? C27 O Na3 116.6(12) . . ? C1 N1 C4 115.6(6) . . ? C1 N1 Na1 115.1(5) . . ? C4 N1 Na1 121.2(5) . . ? C1 N1 Ce 88.4(4) . . ? C4 N1 Ce 124.7(5) . . ? Na1 N1 Ce 83.9(2) . . ? C9 N2 C12 119.1(7) . . ? C9 N2 Na2 114.2(5) . . ? C12 N2 Na2 118.0(5) . . ? C9 N2 Ce 88.1(4) . . ? C12 N2 Ce 125.4(5) . . ? Na2 N2 Ce 84.1(2) . . ? C17 N3 C20 118.1(6) . . ? C17 N3 Na3 111.2(5) . . ? C20 N3 Na3 124.1(5) . . ? C17 N3 Ce 88.6(4) . . ? C20 N3 Ce 117.0(5) . . ? Na3 N3 Ce 88.0(2) . . ? C2 C1 N1 128.2(7) . . ? C2 C1 C1 116.9(5) . 8_565 ? N1 C1 C1 114.9(4) . 8_565 ? C1 C2 C3 124.5(7) . . ? C3 C3 C2 118.7(5) 8_565 . ? N1 C4 C5 116.4(7) . . ? C7 C5 C6 111.0(11) . . ? C7 C5 C8 109.6(12) . . ? C6 C5 C8 107.8(10) . . ? C7 C5 C4 110.2(9) . . ? C6 C5 C4 106.6(9) . . ? C8 C5 C4 111.5(9) . . ? N2 C9 C10 126.9(7) . . ? N2 C9 C9 115.9(4) . 8_565 ? C10 C9 C9 117.0(5) . 8_565 ? C11 C10 C9 123.9(8) . . ? C10 C11 C11 119.1(5) . 8_565 ? N2 C12 C13 116.2(7) . . ? C16 C13 C14 110.0(8) . . ? C16 C13 C15 110.6(8) . . ? C14 C13 C15 107.9(8) . . ? C16 C13 C12 111.4(7) . . ? C14 C13 C12 110.2(7) . . ? C15 C13 C12 106.7(7) . . ? N3 C17 C18 127.1(7) . . ? N3 C17 C17 115.9(4) . 8_565 ? C18 C17 C17 116.9(5) . 8_565 ? C19 C18 C17 123.5(8) . . ? C19 C19 C18 119.6(5) 8_565 . ? N3 C20 C21 117.6(7) . . ? C24 C21 C23 109.1(8) . . ? C24 C21 C20 111.3(7) . . ? C23 C21 C20 112.0(7) . . ? C24 C21 C22 109.6(8) . . ? C23 C21 C22 107.3(8) . . ? C20 C21 C22 107.5(8) . . ? C26 C25 O 115(2) . . ? C28 C27 O 105.3(17) . . ? #===END data_(6)-oct2403 _database_code_depnum_ccdc_archive 'CCDC 289006' _audit_creation_date 2003-10-29T11:53:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C48 H78 Ce1 N6 Na3)(C6 H14)' _chemical_formula_sum 'C54 H92 Ce N6 Na3' _chemical_formula_weight 1034.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 30.4296(3) _cell_length_b 17.9713(2) _cell_length_c 11.8585(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6484.93(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 108666 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.06 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.755 _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 0.6972 _exptl_absorpt_correction_T_max 0.9792 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.76059E-1 _diffrn_orient_matrix_ub_12 0.238799E-1 _diffrn_orient_matrix_ub_13 -0.15832E-2 _diffrn_orient_matrix_ub_21 0.81022E-2 _diffrn_orient_matrix_ub_22 -0.171485E-1 _diffrn_orient_matrix_ub_23 -0.311034E-1 _diffrn_orient_matrix_ub_31 -0.355041E-1 _diffrn_orient_matrix_ub_32 0.472437E-1 _diffrn_orient_matrix_ub_33 -0.104896E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_number 68877 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25.21 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 5944 _reflns_number_gt 4948 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The molecule of hexane solvate was very poorly defined and was included with DFIX restraints and with a common isotropic displacement parameter for the solvate carbon atoms. 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^)+(0.0803P)^2^+9.2905P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 5944 _refine_ls_number_parameters 281 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.767 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # 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' Ce Ce -0.2486 2.6331 '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' 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 Ce Ce 0.361881(10) 0.25 0.44536(3) 0.03179(15) Uani 1 2 d S . . Na1 Na 0.35060(9) 0.25 0.1633(2) 0.0469(6) Uani 1 2 d S . . Na2 Na 0.46173(10) 0.25 0.5653(2) 0.0562(8) Uani 1 2 d S . . Na3 Na 0.27356(10) 0.25 0.6114(3) 0.0591(8) Uani 1 2 d S . . N1 N 0.39689(11) 0.1757(2) 0.2863(3) 0.0360(8) Uani 1 1 d . . . N2 N 0.39831(13) 0.1759(2) 0.6023(3) 0.0426(9) Uani 1 1 d . . . N3 N 0.29115(13) 0.1761(2) 0.4471(3) 0.0396(9) Uani 1 1 d . . . C1 C 0.43649(13) 0.2093(2) 0.3154(3) 0.0343(9) Uani 1 1 d . . . C2 C 0.47469(14) 0.1730(3) 0.3499(4) 0.0406(10) Uani 1 1 d . . . H2 H 0.475 0.1202 0.3514 0.049 Uiso 1 1 calc R . . C3 C 0.51264(15) 0.2116(3) 0.3823(4) 0.0444(11) Uani 1 1 d . . . H3 H 0.5382 0.185 0.4042 0.053 Uiso 1 1 calc R . . C4 C 0.39577(15) 0.0952(3) 0.2758(4) 0.0394(10) Uani 1 1 d . . . H4A H 0.3665 0.0777 0.3007 0.047 Uiso 1 1 calc R . . H4B H 0.4177 0.0741 0.3285 0.047 Uiso 1 1 calc R . . C5 C 0.40476(16) 0.0631(3) 0.1571(4) 0.0495(12) Uani 1 1 d . . . C6 C 0.45292(17) 0.0772(4) 0.1206(5) 0.0653(16) Uani 1 1 d . . . H6A H 0.4582 0.1309 0.1153 0.098 Uiso 1 1 calc R . . H6B H 0.4582 0.0541 0.047 0.098 Uiso 1 1 calc R . . H6C H 0.4729 0.0556 0.1765 0.098 Uiso 1 1 calc R . . C7 C 0.3966(2) -0.0216(3) 0.1637(6) 0.0793(19) Uani 1 1 d . . . H7A H 0.4016 -0.0439 0.0894 0.119 Uiso 1 1 calc R . . H7B H 0.3663 -0.0309 0.1875 0.119 Uiso 1 1 calc R . . H7C H 0.4169 -0.0437 0.2185 0.119 Uiso 1 1 calc R . . C8 C 0.3736(2) 0.0972(4) 0.0712(4) 0.0676(18) Uani 1 1 d . . . H8A H 0.3786 0.0743 -0.0027 0.101 Uiso 1 1 calc R . . H8B H 0.3791 0.1509 0.0661 0.101 Uiso 1 1 calc R . . H8C H 0.3432 0.0886 0.0948 0.101 Uiso 1 1 calc R . . C9 C 0.36984(15) 0.2093(3) 0.6806(4) 0.0419(11) Uani 1 1 d . . . C10 C 0.34008(17) 0.1732(3) 0.7522(4) 0.0501(12) Uani 1 1 d . . . H10 H 0.3392 0.1203 0.7527 0.06 Uiso 1 1 calc R . . C11 C 0.31162(19) 0.2124(3) 0.8229(5) 0.0592(14) Uani 1 1 d . . . H11 H 0.2922 0.1861 0.8713 0.071 Uiso 1 1 calc R . . C12 C 0.39972(17) 0.0951(3) 0.5977(4) 0.0489(12) Uani 1 1 d . . . H12A H 0.4037 0.0802 0.5179 0.059 Uiso 1 1 calc R . . H12B H 0.3708 0.076 0.6223 0.059 Uiso 1 1 calc R . . C13 C 0.43582(18) 0.0559(3) 0.6690(4) 0.0572(14) Uani 1 1 d . . . C14 C 0.4277(2) 0.0644(5) 0.7938(5) 0.094(3) Uani 1 1 d . . . H14A H 0.4302 0.117 0.8146 0.141 Uiso 1 1 calc R . . H14B H 0.4496 0.0354 0.8357 0.141 Uiso 1 1 calc R . . H14C H 0.3982 0.0464 0.812 0.141 Uiso 1 1 calc R . . C15 C 0.4805(2) 0.0844(5) 0.6402(6) 0.090(2) Uani 1 1 d . . . H15A H 0.5028 0.0552 0.6803 0.135 Uiso 1 1 calc R . . H15B H 0.4829 0.1368 0.6625 0.135 Uiso 1 1 calc R . . H15C H 0.4853 0.08 0.5587 0.135 Uiso 1 1 calc R . . C16 C 0.4328(3) -0.0285(4) 0.6374(7) 0.098(3) Uani 1 1 d . . . H16A H 0.4548 -0.0566 0.6802 0.147 Uiso 1 1 calc R . . H16B H 0.4383 -0.0347 0.5565 0.147 Uiso 1 1 calc R . . H16C H 0.4034 -0.0473 0.6556 0.147 Uiso 1 1 calc R . . C17 C 0.27981(13) 0.2092(2) 0.3452(4) 0.0351(9) Uani 1 1 d . . . C18 C 0.27118(14) 0.1734(2) 0.2430(4) 0.0393(10) Uani 1 1 d . . . H18 H 0.2718 0.1206 0.2414 0.047 Uiso 1 1 calc R . . C19 C 0.26168(15) 0.2112(3) 0.1430(4) 0.0441(11) Uani 1 1 d . . . H19 H 0.2553 0.1844 0.0759 0.053 Uiso 1 1 calc R . . C20 C 0.28965(16) 0.0943(3) 0.4520(4) 0.0476(12) Uani 1 1 d . . . H20A H 0.3137 0.0771 0.5019 0.057 Uiso 1 1 calc R . . H20B H 0.2958 0.0748 0.3756 0.057 Uiso 1 1 calc R . . C21 C 0.24632(18) 0.0589(3) 0.4940(5) 0.0621(15) Uani 1 1 d . . . C22 C 0.2343(3) 0.0881(6) 0.6079(7) 0.130(4) Uani 1 1 d . . . H22A H 0.2079 0.0626 0.6351 0.194 Uiso 1 1 calc R . . H22B H 0.2285 0.1417 0.6027 0.194 Uiso 1 1 calc R . . H22C H 0.2586 0.0794 0.6604 0.194 Uiso 1 1 calc R . . C23 C 0.2084(2) 0.0740(4) 0.4140(7) 0.088(2) Uani 1 1 d . . . H23A H 0.2034 0.1278 0.4086 0.132 Uiso 1 1 calc R . . H23B H 0.1817 0.0499 0.4427 0.132 Uiso 1 1 calc R . . H23C H 0.2154 0.0541 0.3392 0.132 Uiso 1 1 calc R . . C24 C 0.2540(3) -0.0248(4) 0.4984(10) 0.119(3) Uani 1 1 d . . . H24A H 0.2616 -0.0429 0.423 0.178 Uiso 1 1 calc R . . H24B H 0.2272 -0.0497 0.5246 0.178 Uiso 1 1 calc R . . H24C H 0.2782 -0.0357 0.5506 0.178 Uiso 1 1 calc R . . C1A C 0.5970(15) 0.25 0.274(3) 0.555(17) Uiso 1 2 d SD . . H1A1 H 0.6123 0.25 0.347 0.832 Uiso 1 2 calc SR . . H1A2 H 0.5785 0.2055 0.2686 0.832 Uiso 0.5 1 calc PR . . H1A3 H 0.5785 0.2945 0.2686 0.832 Uiso 0.5 1 calc PR . . C2A C 0.6300(10) 0.25 0.181(4) 0.555(17) Uiso 1 2 d SD . . H2A1 H 0.649 0.2945 0.1885 0.666 Uiso 0.5 1 calc PR . . H2A2 H 0.649 0.2055 0.1885 0.666 Uiso 0.5 1 calc PR . . C3A C 0.6102(13) 0.25 0.066(4) 0.555(17) Uiso 1 2 d SD . . H3A1 H 0.6206 0.2055 0.0246 0.666 Uiso 0.5 1 calc PR . . H3A2 H 0.6206 0.2945 0.0246 0.666 Uiso 0.5 1 calc PR . . C4A C 0.5610(12) 0.25 0.066(3) 0.555(17) Uiso 1 2 d SD . . H4A1 H 0.5501 0.2946 0.1059 0.666 Uiso 0.5 1 calc PR . . H4A2 H 0.5501 0.2054 0.1059 0.666 Uiso 0.5 1 calc PR . . C5A C 0.5435(16) 0.25 -0.053(3) 0.555(17) Uiso 1 2 d SD . . H5A1 H 0.5546 0.2945 -0.0929 0.666 Uiso 0.5 1 calc PR . . H5A2 H 0.5546 0.2055 -0.0929 0.666 Uiso 0.5 1 calc PR . . C6A C 0.4942(16) 0.25 -0.056(3) 0.555(17) Uiso 1 2 d SD . . H6A1 H 0.4842 0.25 -0.1346 0.832 Uiso 1 2 calc SR . . H6A2 H 0.483 0.2945 -0.0178 0.832 Uiso 0.5 1 calc PR . . H6A3 H 0.483 0.2055 -0.0178 0.832 Uiso 0.5 1 calc PR . . 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 Ce 0.0317(2) 0.0319(2) 0.0318(2) 0 0.00269(14) 0 Na1 0.0436(14) 0.0525(16) 0.0445(15) 0 -0.0050(12) 0 Na2 0.0445(16) 0.074(2) 0.0500(17) 0 0.0002(12) 0 Na3 0.0596(18) 0.0678(19) 0.0500(17) 0 0.0163(14) 0 N1 0.0340(19) 0.038(2) 0.0362(19) -0.0027(16) 0.0019(15) -0.0014(16) N2 0.048(2) 0.046(2) 0.034(2) 0.0032(17) 0.0055(18) 0.0076(18) N3 0.040(2) 0.032(2) 0.046(2) 0.0060(17) 0.0004(17) -0.0021(16) C1 0.035(2) 0.039(2) 0.029(2) -0.0017(18) 0.0036(18) -0.0012(19) C2 0.040(2) 0.037(2) 0.045(3) -0.001(2) -0.002(2) 0.004(2) C3 0.035(2) 0.052(3) 0.046(3) 0.004(2) -0.004(2) 0.007(2) C4 0.042(2) 0.038(3) 0.038(2) -0.004(2) 0.002(2) -0.001(2) C5 0.045(3) 0.058(3) 0.046(3) -0.016(2) -0.001(2) 0.004(2) C6 0.050(3) 0.101(5) 0.045(3) -0.021(3) 0.006(2) 0.010(3) C7 0.078(4) 0.061(4) 0.099(5) -0.035(4) -0.005(4) -0.001(3) C8 0.057(3) 0.099(5) 0.046(3) -0.026(3) -0.008(3) 0.016(3) C9 0.047(3) 0.048(3) 0.031(2) 0.009(2) 0.002(2) 0.006(2) C10 0.061(3) 0.046(3) 0.044(3) 0.009(2) 0.012(2) 0.004(2) C11 0.067(3) 0.060(3) 0.050(3) 0.006(2) 0.023(3) -0.001(3) C12 0.059(3) 0.049(3) 0.039(2) 0.005(2) 0.003(2) 0.017(2) C13 0.064(3) 0.067(4) 0.040(3) 0.013(3) 0.005(2) 0.026(3) C14 0.106(5) 0.133(7) 0.042(3) 0.014(4) -0.007(3) 0.058(5) C15 0.059(4) 0.126(6) 0.086(5) 0.046(5) -0.003(3) 0.026(4) C16 0.127(6) 0.073(5) 0.094(5) 0.012(4) 0.003(5) 0.053(5) C17 0.031(2) 0.032(2) 0.043(2) 0.002(2) 0.0020(18) -0.0016(18) C18 0.041(2) 0.029(2) 0.048(3) -0.002(2) 0.002(2) -0.0029(19) C19 0.048(3) 0.043(2) 0.041(3) -0.007(2) -0.002(2) -0.004(2) C20 0.043(3) 0.037(3) 0.063(3) 0.015(2) 0.001(2) -0.005(2) C21 0.054(3) 0.056(3) 0.076(4) 0.023(3) 0.009(3) -0.017(3) C22 0.105(6) 0.189(10) 0.094(6) -0.012(6) 0.051(5) -0.075(7) C23 0.050(3) 0.096(5) 0.118(6) 0.042(5) -0.002(4) -0.027(3) C24 0.089(5) 0.065(5) 0.201(10) 0.057(6) 0.012(6) -0.029(4) #----------------------------------------------------------------------------# # 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 Ce N3 2.530(4) . ? Ce N3 2.530(4) 8_565 ? Ce N2 2.543(4) 8_565 ? Ce N2 2.543(4) . ? Ce N1 2.545(4) . ? Ce N1 2.545(4) 8_565 ? Na1 N1 2.427(4) 8_565 ? Na1 N1 2.427(4) . ? Na1 C19 2.804(5) . ? Na1 C19 2.804(5) 8_565 ? Na2 N2 2.386(5) . ? Na2 N2 2.386(5) 8_565 ? Na2 C3 2.754(5) 8_565 ? Na2 C3 2.754(5) . ? Na3 N3 2.418(4) . ? Na3 N3 2.418(4) 8_565 ? Na3 C11 2.844(7) 8_565 ? Na3 C11 2.844(7) . ? N1 C1 1.391(5) . ? N1 C4 1.453(6) . ? N2 C9 1.405(6) . ? N2 C12 1.453(6) . ? N3 C17 1.391(6) . ? N3 C20 1.472(6) . ? C1 C2 1.394(6) . ? C1 C1 1.462(9) 8_565 ? C2 C3 1.400(6) . ? C3 C3 1.382(10) 8_565 ? C4 C5 1.546(6) . ? C5 C8 1.521(8) . ? C5 C7 1.544(8) . ? C5 C6 1.549(7) . ? C9 C10 1.401(7) . ? C9 C9 1.463(10) 8_565 ? C10 C11 1.397(7) . ? C11 C11 1.350(11) 8_565 ? C12 C13 1.556(7) . ? C13 C15 1.493(9) . ? C13 C14 1.507(8) . ? C13 C16 1.566(9) . ? C17 C18 1.396(6) . ? C17 C17 1.467(8) 8_565 ? C18 C19 1.396(6) . ? C19 C19 1.394(9) 8_565 ? C20 C21 1.546(7) . ? C21 C22 1.494(10) . ? C21 C23 1.519(9) . ? C21 C24 1.523(9) . ? C1A C2A 1.496(10) . ? C2A C3A 1.490(10) . ? C3A C4A 1.496(10) . ? C4A C5A 1.501(10) . ? C5A C6A 1.501(10) . ? 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 Ce N3 63.37(17) . 8_565 ? N3 Ce N2 129.80(12) . 8_565 ? N3 Ce N2 95.15(12) 8_565 8_565 ? N3 Ce N2 95.15(12) . . ? N3 Ce N2 129.80(12) 8_565 . ? N2 Ce N2 63.18(18) 8_565 . ? N3 Ce N1 94.98(12) . . ? N3 Ce N1 129.63(12) 8_565 . ? N2 Ce N1 129.40(12) 8_565 . ? N2 Ce N1 94.89(12) . . ? N3 Ce N1 129.63(12) . 8_565 ? N3 Ce N1 94.98(12) 8_565 8_565 ? N2 Ce N1 94.89(12) 8_565 8_565 ? N2 Ce N1 129.40(12) . 8_565 ? N1 Ce N1 63.28(16) . 8_565 ? N1 Na1 N1 66.72(18) 8_565 . ? N1 Na1 C19 138.44(16) 8_565 . ? N1 Na1 C19 118.35(14) . . ? N1 Na1 C19 118.35(14) 8_565 8_565 ? N1 Na1 C19 138.44(16) . 8_565 ? C19 Na1 C19 28.79(19) . 8_565 ? N2 Na2 N2 67.9(2) . 8_565 ? N2 Na2 C3 137.74(17) . 8_565 ? N2 Na2 C3 117.39(15) 8_565 8_565 ? N2 Na2 C3 117.39(15) . . ? N2 Na2 C3 137.74(17) 8_565 . ? C3 Na2 C3 29.1(2) 8_565 . ? N3 Na3 N3 66.66(19) . 8_565 ? N3 Na3 C11 138.66(18) . 8_565 ? N3 Na3 C11 119.34(16) 8_565 8_565 ? N3 Na3 C11 119.34(16) . . ? N3 Na3 C11 138.66(18) 8_565 . ? C11 Na3 C11 27.5(2) 8_565 . ? C1 N1 C4 118.3(4) . . ? C1 N1 Na1 114.4(3) . . ? C4 N1 Na1 118.9(3) . . ? C1 N1 Ce 87.2(2) . . ? C4 N1 Ce 125.2(3) . . ? Na1 N1 Ce 85.05(13) . . ? C9 N2 C12 118.0(4) . . ? C9 N2 Na2 112.5(3) . . ? C12 N2 Na2 121.8(3) . . ? C9 N2 Ce 89.5(3) . . ? C12 N2 Ce 120.6(3) . . ? Na2 N2 Ce 85.73(14) . . ? C17 N3 C20 117.0(4) . . ? C17 N3 Na3 114.2(3) . . ? C20 N3 Na3 120.7(3) . . ? C17 N3 Ce 88.8(2) . . ? C20 N3 Ce 123.5(3) . . ? Na3 N3 Ce 84.63(13) . . ? N1 C1 C2 126.3(4) . . ? N1 C1 C1 115.7(2) . 8_565 ? C2 C1 C1 117.9(3) . 8_565 ? N1 C1 Ce 63.5(2) . . ? C2 C1 Ce 128.9(3) . . ? C1 C1 Ce 75.08(9) 8_565 . ? C1 C2 C3 122.5(4) . . ? C1 C2 Na2 85.6(3) . . ? C3 C2 Na2 68.8(3) . . ? C3 C3 C2 119.6(3) 8_565 . ? C3 C3 Na2 75.47(10) 8_565 . ? C2 C3 Na2 82.9(3) . . ? N1 C4 C5 116.5(4) . . ? C8 C5 C7 109.4(5) . . ? C8 C5 C4 110.4(4) . . ? C7 C5 C4 107.0(5) . . ? C8 C5 C6 109.6(5) . . ? C7 C5 C6 109.1(5) . . ? C4 C5 C6 111.1(4) . . ? C10 C9 N2 127.0(5) . . ? C10 C9 C9 117.6(3) . 8_565 ? N2 C9 C9 115.3(3) . 8_565 ? C10 C9 Ce 130.4(3) . . ? N2 C9 Ce 61.5(2) . . ? C9 C9 Ce 75.36(10) 8_565 . ? C11 C10 C9 122.1(5) . . ? C11 C10 Na3 71.3(3) . . ? C9 C10 Na3 83.3(3) . . ? C11 C11 C10 120.3(3) 8_565 . ? C11 C11 Na3 76.27(11) 8_565 . ? C10 C11 Na3 81.0(3) . . ? N2 C12 C13 116.9(5) . . ? C15 C13 C14 109.8(6) . . ? C15 C13 C12 111.3(5) . . ? C14 C13 C12 111.9(4) . . ? C15 C13 C16 109.3(6) . . ? C14 C13 C16 108.9(6) . . ? C12 C13 C16 105.5(5) . . ? N3 C17 C18 127.2(4) . . ? N3 C17 C17 115.3(2) . 8_565 ? C18 C17 C17 117.4(3) . 8_565 ? N3 C17 Ce 62.1(2) . . ? C18 C17 Ce 130.0(3) . . ? C17 C17 Ce 75.14(8) 8_565 . ? C17 C18 C19 123.5(4) . . ? C17 C18 Na1 84.8(3) . . ? C19 C18 Na1 70.7(3) . . ? C19 C19 C18 119.1(3) 8_565 . ? C19 C19 Na1 75.60(10) 8_565 . ? C18 C19 Na1 81.3(3) . . ? N3 C20 C21 116.7(4) . . ? C22 C21 C23 108.3(7) . . ? C22 C21 C24 110.7(7) . . ? C23 C21 C24 108.4(6) . . ? C22 C21 C20 110.8(5) . . ? C23 C21 C20 112.0(5) . . ? C24 C21 C20 106.6(5) . . ? C3A C2A C1A 114.0(11) . . ? C2A C3A C4A 114.0(11) . . ? C3A C4A C5A 110.9(10) . . ? C6A C5A C4A 112.3(11) . . ? #===END