# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Michael F. Lappert' 'Peter B. Hitchcock' 'Qi-Gu Huang' 'Xue-Hong Wei' _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; Chemistry Department University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; Lanthanide Metal Amides Revisited ; _publ_requested_category FM data_(2)-jul3903 _database_code_depnum_ccdc_archive 'CCDC 239400' _audit_creation_date 2003-07-31T10:10:24-00:00 _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 'C31 H62 Ce1 N3 O1' _chemical_formula_sum 'C31 H62 Ce1 N3 O1' _chemical_formula_weight 632.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1437(2) _cell_length_b 11.6360(2) _cell_length_c 22.9366(3) _cell_angle_alpha 90 _cell_angle_beta 90.888(1) _cell_angle_gamma 90 _cell_volume 3240.65(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16909 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 24.713 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.43 _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 0.5722 _exptl_absorpt_correction_T_max 0.6758 #----------------------------------------------------------------------------# # 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 -0.719661E-1 _diffrn_orient_matrix_ub_12 -0.373686E-1 _diffrn_orient_matrix_ub_13 0.88968E-2 _diffrn_orient_matrix_ub_21 0.228505E-1 _diffrn_orient_matrix_ub_22 -0.699062E-1 _diffrn_orient_matrix_ub_23 -0.221012E-1 _diffrn_orient_matrix_ub_31 0.328851E-1 _diffrn_orient_matrix_ub_32 -0.332029E-1 _diffrn_orient_matrix_ub_33 0.365194E-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 0.0352 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_number 22202 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 24.72 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 5476 _reflns_number_gt 5031 _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^)+(0.0199P)^2^+3.2931P] 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 5476 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.022 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.634 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' 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 0.254134(9) 0.314659(10) 0.095574(5) 0.01735(6) Uani 1 1 d . . . O O 0.27804(14) 0.55488(15) 0.09444(7) 0.0312(4) Uani 1 1 d . . . N1 N 0.25821(14) 0.24156(16) -0.00099(8) 0.0191(4) Uani 1 1 d . . . N2 N 0.40872(15) 0.25334(16) 0.14970(8) 0.0209(4) Uani 1 1 d . . . N3 N 0.08143(15) 0.30763(16) 0.14152(8) 0.0202(4) Uani 1 1 d . . . C1 C 0.30036(18) 0.1288(2) -0.02025(10) 0.0226(5) Uani 1 1 d . . . C2 C 0.21320(19) 0.0618(2) -0.05593(10) 0.0261(5) Uani 1 1 d . . . H2A H 0.2473 -0.0088 -0.0716 0.031 Uiso 1 1 calc R . . H2B H 0.1532 0.0382 -0.0298 0.031 Uiso 1 1 calc R . . C3 C 0.1642(2) 0.1312(2) -0.10635(11) 0.0316(6) Uani 1 1 d . . . H3A H 0.1048 0.0868 -0.1259 0.038 Uiso 1 1 calc R . . H3B H 0.2218 0.1477 -0.1353 0.038 Uiso 1 1 calc R . . C4 C 0.1182(2) 0.2434(2) -0.08267(10) 0.0287(5) Uani 1 1 d . . . H4A H 0.0547 0.2263 -0.0575 0.034 Uiso 1 1 calc R . . H4B H 0.0911 0.2912 -0.1156 0.034 Uiso 1 1 calc R . . C5 C 0.2051(2) 0.31199(19) -0.04718(10) 0.0233(5) Uani 1 1 d . . . C6 C 0.3256(2) 0.0578(2) 0.03458(11) 0.0299(5) Uani 1 1 d . . . H6A H 0.3809 0.0977 0.0586 0.045 Uiso 1 1 calc R . . H6B H 0.3538 -0.0177 0.0233 0.045 Uiso 1 1 calc R . . H6C H 0.258 0.0481 0.0569 0.045 Uiso 1 1 calc R . . C7 C 0.4082(2) 0.1346(2) -0.05508(12) 0.0343(6) Uani 1 1 d . . . H7A H 0.3958 0.1795 -0.0907 0.052 Uiso 1 1 calc R . . H7B H 0.4315 0.0567 -0.0654 0.052 Uiso 1 1 calc R . . H7C H 0.4658 0.1714 -0.0312 0.052 Uiso 1 1 calc R . . C8 C 0.1465(2) 0.4112(2) -0.01721(11) 0.0302(6) Uani 1 1 d . . . H8A H 0.2001 0.4561 0.0056 0.045 Uiso 1 1 calc R . . H8B H 0.0902 0.3806 0.0088 0.045 Uiso 1 1 calc R . . H8C H 0.1114 0.4606 -0.0467 0.045 Uiso 1 1 calc R . . C9 C 0.2862(2) 0.3692(2) -0.08951(11) 0.0367(6) Uani 1 1 d . . . H9A H 0.3267 0.3096 -0.1104 0.055 Uiso 1 1 calc R . . H9B H 0.3382 0.4174 -0.0674 0.055 Uiso 1 1 calc R . . H9C H 0.2451 0.4168 -0.1176 0.055 Uiso 1 1 calc R . . C10 C 0.51915(18) 0.2917(2) 0.13131(10) 0.0233(5) Uani 1 1 d . . . C11 C 0.5984(2) 0.1907(2) 0.12191(11) 0.0287(6) Uani 1 1 d . . . H11A H 0.5739 0.1468 0.0871 0.034 Uiso 1 1 calc R . . H11B H 0.6729 0.2212 0.1143 0.034 Uiso 1 1 calc R . . C12 C 0.6042(2) 0.1103(2) 0.17417(11) 0.0329(6) Uani 1 1 d . . . H12A H 0.6519 0.0438 0.1654 0.04 Uiso 1 1 calc R . . H12B H 0.6361 0.1512 0.2083 0.04 Uiso 1 1 calc R . . C13 C 0.4893(2) 0.0693(2) 0.18783(11) 0.0310(6) Uani 1 1 d . . . H13A H 0.4927 0.0206 0.2232 0.037 Uiso 1 1 calc R . . H13B H 0.4618 0.0211 0.1552 0.037 Uiso 1 1 calc R . . C14 C 0.4071(2) 0.1685(2) 0.19788(10) 0.0261(5) Uani 1 1 d . . . C15 C 0.5054(2) 0.3538(2) 0.07261(10) 0.0279(5) Uani 1 1 d . . . H15A H 0.4551 0.419 0.077 0.042 Uiso 1 1 calc R . . H15B H 0.475 0.3004 0.0435 0.042 Uiso 1 1 calc R . . H15C H 0.5772 0.3817 0.0598 0.042 Uiso 1 1 calc R . . C16 C 0.5743(2) 0.3793(2) 0.17332(11) 0.0340(6) Uani 1 1 d . . . H16A H 0.5849 0.3439 0.2118 0.051 Uiso 1 1 calc R . . H16B H 0.5271 0.4471 0.1768 0.051 Uiso 1 1 calc R . . H16C H 0.6459 0.4023 0.1579 0.051 Uiso 1 1 calc R . . C17 C 0.2918(2) 0.1150(2) 0.19886(11) 0.0332(6) Uani 1 1 d . . . H17A H 0.237 0.1754 0.2051 0.05 Uiso 1 1 calc R . . H17B H 0.2883 0.0587 0.2306 0.05 Uiso 1 1 calc R . . H17C H 0.2765 0.0766 0.1616 0.05 Uiso 1 1 calc R . . C18 C 0.4284(2) 0.2215(3) 0.25881(11) 0.0366(6) Uani 1 1 d . . . H18A H 0.5017 0.2569 0.26 0.055 Uiso 1 1 calc R . . H18B H 0.4246 0.1612 0.2885 0.055 Uiso 1 1 calc R . . H18C H 0.3726 0.2802 0.2665 0.055 Uiso 1 1 calc R . . C19 C -0.00825(18) 0.2287(2) 0.12302(10) 0.0219(5) Uani 1 1 d . . . C20 C -0.0622(2) 0.1674(2) 0.17473(11) 0.0281(5) Uani 1 1 d . . . H20A H -0.1282 0.1255 0.1604 0.034 Uiso 1 1 calc R . . H20B H -0.0099 0.1102 0.191 0.034 Uiso 1 1 calc R . . C21 C -0.0959(2) 0.2489(2) 0.22286(11) 0.0340(6) Uani 1 1 d . . . H21A H -0.1254 0.2048 0.2561 0.041 Uiso 1 1 calc R . . H21B H -0.1543 0.3014 0.2083 0.041 Uiso 1 1 calc R . . C22 C 0.0044(2) 0.3179(2) 0.24266(11) 0.0315(6) Uani 1 1 d . . . H22A H 0.0595 0.2652 0.2603 0.038 Uiso 1 1 calc R . . H22B H -0.0179 0.3735 0.2729 0.038 Uiso 1 1 calc R . . C23 C 0.05752(19) 0.3836(2) 0.19181(10) 0.0237(5) Uani 1 1 d . . . C24 C -0.09861(19) 0.2864(2) 0.08490(11) 0.0294(6) Uani 1 1 d . . . H24A H -0.1342 0.3474 0.1073 0.044 Uiso 1 1 calc R . . H24B H -0.1537 0.2289 0.0732 0.044 Uiso 1 1 calc R . . H24C H -0.0653 0.3194 0.0501 0.044 Uiso 1 1 calc R . . C25 C 0.04379(19) 0.1350(2) 0.08565(11) 0.0280(5) Uani 1 1 d . . . H25A H 0.0794 0.1703 0.052 0.042 Uiso 1 1 calc R . . H25B H -0.0135 0.0817 0.072 0.042 Uiso 1 1 calc R . . H25C H 0.0988 0.093 0.109 0.042 Uiso 1 1 calc R . . C26 C -0.0157(2) 0.4875(2) 0.17552(11) 0.0327(6) Uani 1 1 d . . . H26A H -0.087 0.4602 0.1605 0.049 Uiso 1 1 calc R . . H26B H 0.0205 0.5333 0.1455 0.049 Uiso 1 1 calc R . . H26C H -0.027 0.535 0.2102 0.049 Uiso 1 1 calc R . . C27 C 0.1671(2) 0.4325(2) 0.21460(11) 0.0302(6) Uani 1 1 d . . . H27A H 0.2164 0.3692 0.2256 0.045 Uiso 1 1 calc R . . H27B H 0.1538 0.4808 0.2487 0.045 Uiso 1 1 calc R . . H27C H 0.2011 0.4786 0.184 0.045 Uiso 1 1 calc R . . C28 C 0.2027(3) 0.6388(3) 0.06998(15) 0.0506(8) Uani 1 1 d . . . H28A H 0.1266 0.6084 0.07 0.061 Uiso 1 1 calc R . . H28B H 0.2227 0.6565 0.0293 0.061 Uiso 1 1 calc R . . C29 C 0.2099(4) 0.7416(3) 0.1053(2) 0.0829(14) Uani 1 1 d . . . H29A H 0.1507 0.7425 0.1345 0.1 Uiso 1 1 calc R . . H29B H 0.2029 0.811 0.0806 0.1 Uiso 1 1 calc R . . C30 C 0.3202(3) 0.7383(3) 0.13487(17) 0.0608(10) Uani 1 1 d . . . H30A H 0.3135 0.7553 0.177 0.073 Uiso 1 1 calc R . . H30B H 0.3703 0.7954 0.1174 0.073 Uiso 1 1 calc R . . C31 C 0.3630(2) 0.6188(3) 0.12597(15) 0.0470(8) Uani 1 1 d . . . H31A H 0.4316 0.6207 0.1032 0.056 Uiso 1 1 calc R . . H31B H 0.3791 0.5819 0.164 0.056 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 Ce 0.01558(8) 0.01947(8) 0.01698(8) -0.00031(5) -0.00053(5) 0.00054(5) O 0.0310(9) 0.0253(9) 0.0370(10) 0.0005(7) -0.0085(7) -0.0015(8) N1 0.0175(9) 0.0191(10) 0.0207(10) -0.0015(8) 0.0002(7) 0.0006(8) N2 0.0182(9) 0.0255(11) 0.0190(10) 0.0013(8) 0.0007(8) 0.0026(8) N3 0.0183(9) 0.0226(10) 0.0196(10) -0.0007(7) 0.0012(8) -0.0001(8) C1 0.0208(11) 0.0233(12) 0.0237(12) -0.0048(10) -0.0009(9) 0.0013(10) C2 0.0278(12) 0.0211(12) 0.0293(13) -0.0064(10) -0.0027(10) 0.0010(10) C3 0.0391(15) 0.0282(14) 0.0272(13) -0.0053(11) -0.0077(11) -0.0028(12) C4 0.0322(13) 0.0281(14) 0.0254(13) 0.0006(10) -0.0080(10) 0.0015(11) C5 0.0284(13) 0.0212(13) 0.0203(12) 0.0016(9) 0.0005(10) -0.0004(10) C6 0.0307(13) 0.0249(13) 0.0339(14) -0.0041(11) -0.0060(11) 0.0066(11) C7 0.0242(13) 0.0390(16) 0.0400(15) -0.0121(12) 0.0050(11) 0.0028(12) C8 0.0391(14) 0.0243(13) 0.0269(13) 0.0014(10) -0.0038(11) 0.0076(11) C9 0.0445(16) 0.0345(15) 0.0314(14) 0.0074(12) 0.0061(12) -0.0052(13) C10 0.0176(11) 0.0281(13) 0.0243(12) -0.0024(10) -0.0007(9) -0.0002(10) C11 0.0185(12) 0.0336(15) 0.0339(14) -0.0049(11) 0.0039(10) 0.0007(10) C12 0.0253(13) 0.0379(15) 0.0356(14) -0.0024(12) -0.0027(11) 0.0112(11) C13 0.0330(13) 0.0326(14) 0.0274(13) 0.0069(11) 0.0000(10) 0.0083(11) C14 0.0251(12) 0.0341(14) 0.0192(12) 0.0054(10) 0.0015(10) 0.0071(11) C15 0.0255(12) 0.0283(13) 0.0299(13) 0.0007(10) 0.0027(10) -0.0065(11) C16 0.0309(14) 0.0351(15) 0.0358(14) -0.0068(12) -0.0076(11) -0.0035(12) C17 0.0296(13) 0.0388(15) 0.0315(14) 0.0140(12) 0.0057(11) 0.0040(12) C18 0.0358(14) 0.0524(17) 0.0215(13) 0.0025(12) 0.0001(11) 0.0127(13) C19 0.0163(11) 0.0251(12) 0.0242(12) 0.0000(10) 0.0013(9) -0.0019(10) C20 0.0254(12) 0.0304(14) 0.0288(13) 0.0029(10) 0.0050(10) -0.0039(11) C21 0.0331(14) 0.0399(16) 0.0292(14) 0.0045(12) 0.0116(11) -0.0020(12) C22 0.0349(14) 0.0375(15) 0.0223(13) -0.0018(10) 0.0057(11) 0.0047(11) C23 0.0243(12) 0.0241(12) 0.0225(12) -0.0016(10) -0.0001(9) 0.0045(10) C24 0.0214(12) 0.0360(14) 0.0309(14) 0.0033(11) -0.0010(10) -0.0041(11) C25 0.0237(12) 0.0291(14) 0.0313(13) -0.0054(11) 0.0054(10) -0.0078(11) C26 0.0345(14) 0.0279(14) 0.0355(14) -0.0055(11) -0.0028(11) 0.0083(11) C27 0.0312(13) 0.0313(14) 0.0280(13) -0.0069(11) -0.0027(10) 0.0024(11) C28 0.0555(19) 0.0324(16) 0.063(2) -0.0007(14) -0.0263(16) 0.0079(15) C29 0.095(3) 0.042(2) 0.110(3) -0.023(2) -0.059(3) 0.020(2) C30 0.0467(19) 0.0437(19) 0.091(3) -0.0239(18) -0.0189(18) 0.0002(16) C31 0.0358(15) 0.0349(16) 0.070(2) -0.0062(15) -0.0162(14) -0.0074(13) #----------------------------------------------------------------------------# # 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 2.3457(18) . ? Ce N3 2.3631(18) . ? Ce N1 2.3738(18) . ? Ce O 2.8104(17) . ? O C28 1.446(3) . ? O C31 1.455(3) . ? N1 C1 1.478(3) . ? N1 C5 1.480(3) . ? N2 C10 1.481(3) . ? N2 C14 1.482(3) . ? N3 C19 1.482(3) . ? N3 C23 1.485(3) . ? C1 C6 1.532(3) . ? C1 C2 1.540(3) . ? C1 C7 1.546(3) . ? C2 C3 1.524(3) . ? C3 C4 1.524(4) . ? C4 C5 1.545(3) . ? C5 C8 1.525(3) . ? C5 C9 1.544(3) . ? C10 C15 1.535(3) . ? C10 C11 1.536(3) . ? C10 C16 1.548(3) . ? C11 C12 1.521(4) . ? C12 C13 1.511(3) . ? C13 C14 1.546(3) . ? C14 C17 1.532(3) . ? C14 C18 1.546(3) . ? C19 C25 1.529(3) . ? C19 C20 1.539(3) . ? C19 C24 1.546(3) . ? C20 C21 1.516(4) . ? C21 C22 1.522(4) . ? C22 C23 1.544(3) . ? C23 C27 1.532(3) . ? C23 C26 1.543(3) . ? C28 C29 1.446(5) . ? C29 C30 1.492(5) . ? C30 C31 1.500(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ce N3 117.52(6) . . ? N2 Ce N1 110.90(6) . . ? N3 Ce N1 115.80(6) . . ? N2 Ce O 103.03(6) . . ? N3 Ce O 97.53(6) . . ? N1 Ce O 110.13(6) . . ? C28 O C31 106.7(2) . . ? C28 O Ce 127.66(15) . . ? C31 O Ce 125.18(15) . . ? C1 N1 C5 115.26(17) . . ? C1 N1 Ce 127.53(13) . . ? C5 N1 Ce 117.03(13) . . ? C10 N2 C14 115.84(17) . . ? C10 N2 Ce 118.59(13) . . ? C14 N2 Ce 125.25(14) . . ? C19 N3 C23 116.07(17) . . ? C19 N3 Ce 123.17(13) . . ? C23 N3 Ce 120.75(14) . . ? N1 C1 C6 107.39(18) . . ? N1 C1 C2 111.70(18) . . ? C6 C1 C2 106.87(19) . . ? N1 C1 C7 114.6(2) . . ? C6 C1 C7 106.7(2) . . ? C2 C1 C7 109.18(19) . . ? C3 C2 C1 113.1(2) . . ? C2 C3 C4 108.95(19) . . ? C3 C4 C5 112.3(2) . . ? N1 C5 C8 107.34(18) . . ? N1 C5 C9 114.4(2) . . ? C8 C5 C9 105.3(2) . . ? N1 C5 C4 112.23(18) . . ? C8 C5 C4 108.0(2) . . ? C9 C5 C4 109.2(2) . . ? N2 C10 C15 107.74(18) . . ? N2 C10 C11 112.45(19) . . ? C15 C10 C11 107.30(19) . . ? N2 C10 C16 113.95(19) . . ? C15 C10 C16 106.0(2) . . ? C11 C10 C16 108.96(19) . . ? C12 C11 C10 112.4(2) . . ? C13 C12 C11 109.0(2) . . ? C12 C13 C14 113.3(2) . . ? N2 C14 C17 107.73(18) . . ? N2 C14 C13 111.70(19) . . ? C17 C14 C13 106.9(2) . . ? N2 C14 C18 113.8(2) . . ? C17 C14 C18 106.8(2) . . ? C13 C14 C18 109.45(19) . . ? N3 C19 C25 107.10(17) . . ? N3 C19 C20 112.74(18) . . ? C25 C19 C20 106.7(2) . . ? N3 C19 C24 113.88(19) . . ? C25 C19 C24 106.76(19) . . ? C20 C19 C24 109.25(19) . . ? C21 C20 C19 113.2(2) . . ? C20 C21 C22 108.9(2) . . ? C21 C22 C23 112.2(2) . . ? N3 C23 C27 107.86(18) . . ? N3 C23 C26 113.39(18) . . ? C27 C23 C26 106.6(2) . . ? N3 C23 C22 112.41(19) . . ? C27 C23 C22 107.28(19) . . ? C26 C23 C22 109.0(2) . . ? O C28 C29 108.0(2) . . ? C28 C29 C30 106.2(3) . . ? C29 C30 C31 105.8(3) . . ? O C31 C30 107.3(2) . . ? #===END data_(7)-oct1203 _database_code_depnum_ccdc_archive 'CCDC 239401' _audit_creation_date 2003-10-14T14:46:33-00:00 _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 ; '[(tmp)TeCl]' ; _chemical_formula_moiety 'C9 H18 Cl1 N1 Te1' _chemical_formula_sum 'C9 H18 Cl1 N1 Te1' _chemical_formula_weight 303.29 _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 8.9236(4) _cell_length_b 11.8002(6) _cell_length_c 10.8180(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1139.14(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8257 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.35 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.799 _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 0.8082 _exptl_absorpt_correction_T_max 0.9437 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.7107 _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 -0.104233 _diffrn_orient_matrix_ub_12 0.288412E-1 _diffrn_orient_matrix_ub_13 0.164124E-1 _diffrn_orient_matrix_ub_21 0.396533E-1 _diffrn_orient_matrix_ub_22 0.573525E-1 _diffrn_orient_matrix_ub_23 0.593117E-1 _diffrn_orient_matrix_ub_31 0.110054E-1 _diffrn_orient_matrix_ub_32 0.665113E-1 _diffrn_orient_matrix_ub_33 -0.582611E-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 0.0844 _diffrn_reflns_av_unetI/netI 0.0453 _diffrn_reflns_number 8575 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 1085 _reflns_number_gt 923 _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 are alternative very low occupancy positions for the Te and Cl atoms sharing a common tetramethylpiperidine (tmp) ligand. 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^+4.8638P] 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 1085 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.612 _refine_diff_density_min -0.796 _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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N N 0.2128(6) 0.25 0.4239(5) 0.0208(13) Uani 1 2 d S . . Te Te 0.04792(5) 0.25 0.29877(4) 0.02076(17) Uani 0.93 2 d SP A 1 Cl Cl -0.1883(2) 0.25 0.4197(2) 0.0307(5) Uani 0.93 2 d SP A 1 C1 C 0.2478(5) 0.3613(4) 0.4866(4) 0.0203(11) Uani 1 1 d . . 1 C2 C 0.4037(6) 0.3554(5) 0.5453(5) 0.0336(14) Uani 1 1 d . . 1 H2B H 0.4799 0.3583 0.4789 0.04 Uiso 1 1 calc R . 1 H2A H 0.4181 0.4228 0.5984 0.04 Uiso 1 1 calc R . 1 C3 C 0.4299(9) 0.25 0.6221(7) 0.038(2) Uani 1 2 d S . 1 H3B H 0.5339 0.25 0.6538 0.046 Uiso 1 2 calc SR . 1 H3A H 0.361 0.25 0.6939 0.046 Uiso 1 2 calc SR . 1 C4 C 0.1298(6) 0.3910(5) 0.5855(5) 0.0342(14) Uani 1 1 d . . 1 H4C H 0.1309 0.3331 0.6505 0.051 Uiso 1 1 calc R . 1 H4B H 0.0303 0.3936 0.5474 0.051 Uiso 1 1 calc R . 1 H4A H 0.1533 0.465 0.6217 0.051 Uiso 1 1 calc R . 1 C5 C 0.2531(6) 0.4571(4) 0.3912(5) 0.0281(12) Uani 1 1 d . . 1 H5C H 0.2775 0.5286 0.4328 0.042 Uiso 1 1 calc R . 1 H5B H 0.1552 0.4639 0.3508 0.042 Uiso 1 1 calc R . 1 H5A H 0.3298 0.4403 0.3291 0.042 Uiso 1 1 calc R . 1 Te1A Te 0.4518(9) 0.25 0.2999(8) 0.0316(17) Uani 0.07 2 d SP A 2 Cl1A Cl 0.691(5) 0.25 0.419(3) 0.043(10) Uani 0.07 2 d SP 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 N 0.024(3) 0.024(3) 0.014(3) 0 -0.007(3) 0 Te 0.0173(3) 0.0263(3) 0.0186(3) 0 -0.0042(2) 0 Cl 0.0184(11) 0.0407(13) 0.0332(12) 0 0.0010(9) 0 C1 0.021(3) 0.018(3) 0.021(2) -0.006(2) 0.000(2) -0.003(2) C2 0.028(3) 0.040(4) 0.033(3) -0.002(3) -0.012(2) -0.008(3) C3 0.031(4) 0.052(5) 0.032(4) 0 -0.015(4) 0 C4 0.034(3) 0.034(3) 0.035(3) -0.007(3) 0.007(3) 0.001(3) C5 0.032(3) 0.020(3) 0.033(3) -0.001(2) 0.002(3) 0.000(2) Te1A 0.030(4) 0.030(4) 0.034(4) 0 0.017(4) 0 Cl1A 0.08(3) 0.024(17) 0.023(17) 0 -0.042(18) 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 N C1 1.510(5) . ? N Te 1.999(5) . ? Te Cl 2.481(2) . ? C1 C2 1.531(7) . ? C1 C5 1.531(7) . ? C1 C4 1.542(7) . ? C2 C3 1.514(7) . ? C3 C2 1.514(7) 8_565 ? N Te1A 2.520(10) . ? Te1A Cl1A 2.49(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N C1 120.8(5) . 8_565 ? C1 N Te 117.1(3) . . ? N Te Cl 105.54(17) . . ? N C1 C2 109.5(4) . . ? N C1 C5 110.3(4) . . ? C2 C1 C5 106.6(4) . . ? N C1 C4 111.6(4) . . ? C2 C1 C4 110.0(4) . . ? C5 C1 C4 108.7(4) . . ? C3 C2 C1 113.9(5) . . ? C2 C3 C2 110.4(6) 8_565 . ? C1 N Te1A 93.7(3) . . ? Cl1A Te1A N 116.6(10) . . ? #===END data_(9)-aug303 _database_code_depnum_ccdc_archive 'CCDC 239402' _audit_creation_date 2003-08-19T14:09:45-00:00 _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 ; '[CeCl2(thf)5][TeCl5(thf)]' ; _chemical_formula_moiety 'C24 H48 Ce1 Cl7 O6 Te1' _chemical_formula_sum 'C24 H48 Ce1 Cl7 O6 Te1' _chemical_formula_weight 948.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c _symmetry_space_group_name_Hall '-P 2yc' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.1777(2) _cell_length_b 11.2908(2) _cell_length_c 13.8665(3) _cell_angle_alpha 90 _cell_angle_beta 104.238(1) _cell_angle_gamma 90 _cell_volume 1848.02(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14776 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.544 _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 0.5477 _exptl_absorpt_correction_T_max 0.8364 #----------------------------------------------------------------------------# # 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 -0.812983E-1 _diffrn_orient_matrix_ub_12 -0.172433E-1 _diffrn_orient_matrix_ub_13 -0.322054E-1 _diffrn_orient_matrix_ub_21 0.205446E-1 _diffrn_orient_matrix_ub_22 -0.18293E-1 _diffrn_orient_matrix_ub_23 -0.63922E-1 _diffrn_orient_matrix_ub_31 0.120816E-1 _diffrn_orient_matrix_ub_32 -0.849251E-1 _diffrn_orient_matrix_ub_33 0.203079E-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 0.0449 _diffrn_reflns_av_unetI/netI 0.0278 _diffrn_reflns_number 19078 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 3248 _reflns_number_gt 2885 _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^)+(0.0091P)^2^+4.3555P] 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 3248 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.189 _refine_diff_density_min -0.56 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' Te Te -0.5308 1.6751 '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 0.5 0.31505(3) 0.25 0.02289(9) Uani 1 2 d S . . Te Te 0 0.79960(3) 0.25 0.02659(10) Uani 1 2 d S . . Cl1 Cl 0 0.59217(12) 0.25 0.0363(3) Uani 1 2 d S . . Cl2 Cl -0.21294(9) 0.79340(11) 0.20466(8) 0.0478(3) Uani 1 1 d . . . Cl3 Cl -0.00265(10) 0.79712(9) 0.06869(7) 0.0428(3) Uani 1 1 d . . . Cl4 Cl 0.61228(9) 0.30968(9) 0.10496(7) 0.0397(2) Uani 1 1 d . . . O1 O 0.5 0.5361(3) 0.25 0.0301(8) Uani 1 2 d S . . O2 O 0.3196(2) 0.3855(2) 0.13737(18) 0.0342(6) Uani 1 1 d . . . O3 O 0.3966(2) 0.1375(2) 0.1645(2) 0.0423(7) Uani 1 1 d . . . O4 O 0 1.0372(4) 0.25 0.086(2) Uani 1 2 d S . . C1 C 0.5088(4) 0.6101(4) 0.1665(3) 0.0429(11) Uani 1 1 d . . . H1A H 0.455 0.5835 0.1046 0.051 Uiso 1 1 calc R . . H1B H 0.5865 0.6075 0.1566 0.051 Uiso 1 1 calc R . . C2 C 0.4801(5) 0.7321(4) 0.1937(4) 0.0713(17) Uani 1 1 d . . . H2A H 0.3975 0.7469 0.1717 0.086 Uiso 1 1 calc R . . H2B H 0.5206 0.7927 0.1641 0.086 Uiso 1 1 calc R . . C3 C 0.2354(3) 0.4629(4) 0.1639(3) 0.0387(10) Uani 1 1 d . . . H3A H 0.2707 0.5381 0.1925 0.046 Uiso 1 1 calc R . . H3B H 0.2011 0.4239 0.2134 0.046 Uiso 1 1 calc R . . C4 C 0.1484(5) 0.4854(5) 0.0704(4) 0.0655(15) Uani 1 1 d . . . H4A H 0.1182 0.5669 0.0693 0.079 Uiso 1 1 calc R . . H4B H 0.0849 0.4285 0.0625 0.079 Uiso 1 1 calc R . . C5 C 0.2096(4) 0.4688(4) -0.0099(3) 0.0483(12) Uani 1 1 d . . . H5A H 0.2498 0.5421 -0.0204 0.058 Uiso 1 1 calc R . . H5B H 0.1567 0.4456 -0.0734 0.058 Uiso 1 1 calc R . . C6 C 0.2914(4) 0.3712(5) 0.0296(3) 0.0542(13) Uani 1 1 d . . . H6A H 0.2563 0.2929 0.0103 0.065 Uiso 1 1 calc R . . H6B H 0.3601 0.3784 0.0039 0.065 Uiso 1 1 calc R . . C7 C 0.2855(4) 0.0980(5) 0.1730(4) 0.0683(16) Uani 1 1 d . . . H7A H 0.291 0.062 0.2391 0.082 Uiso 1 1 calc R . . H7B H 0.2323 0.1658 0.1647 0.082 Uiso 1 1 calc R . . C8 C 0.2458(4) 0.0109(5) 0.0948(4) 0.0602(14) Uani 1 1 d . . . H8A H 0.1711 0.0349 0.0527 0.072 Uiso 1 1 calc R . . H8B H 0.2375 -0.0674 0.1243 0.072 Uiso 1 1 calc R . . C9 C 0.3293(4) 0.0040(4) 0.0343(4) 0.0568(13) Uani 1 1 d . . . H9A H 0.3029 0.0484 -0.0287 0.068 Uiso 1 1 calc R . . H9B H 0.3432 -0.0794 0.0186 0.068 Uiso 1 1 calc R . . C10 C 0.4327(4) 0.0579(5) 0.0969(5) 0.0741(18) Uani 1 1 d . . . H10A H 0.4834 -0.0039 0.1343 0.089 Uiso 1 1 calc R . . H10B H 0.4742 0.1019 0.0552 0.089 Uiso 1 1 calc R . . C11 C -0.0569(4) 1.1062(4) 0.1694(3) 0.0474(11) Uani 1 1 d . . . H11A H -0.1397 1.0944 0.1569 0.057 Uiso 1 1 calc R . . H11B H -0.0329 1.0839 0.1086 0.057 Uiso 1 1 calc R . . C12 C -0.0274(5) 1.2310(5) 0.1955(4) 0.0668(15) Uani 1 1 d . . . H12A H -0.0963 1.281 0.1809 0.08 Uiso 1 1 calc R . . H12B H 0.0255 1.2616 0.1574 0.08 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 Ce 0.02148(15) 0.02387(16) 0.02274(16) 0 0.00430(11) 0 Te 0.0314(2) 0.02671(19) 0.01991(18) 0 0.00306(14) 0 Cl1 0.0477(8) 0.0273(7) 0.0323(7) 0 0.0068(6) 0 Cl2 0.0322(5) 0.0634(7) 0.0449(6) -0.0059(5) 0.0038(5) 0.0058(5) Cl3 0.0575(7) 0.0477(6) 0.0231(5) 0.0013(4) 0.0098(5) -0.0126(5) Cl4 0.0417(6) 0.0482(6) 0.0340(5) -0.0040(5) 0.0187(4) -0.0059(5) O1 0.038(2) 0.0221(18) 0.0284(19) 0 0.0044(16) 0 O2 0.0279(14) 0.0452(16) 0.0250(14) -0.0078(12) -0.0021(11) 0.0104(12) O3 0.0326(15) 0.0347(16) 0.0600(19) -0.0154(14) 0.0122(14) -0.0113(12) O4 0.158(6) 0.034(3) 0.036(3) 0 -0.033(3) 0 C1 0.044(3) 0.041(2) 0.041(2) 0.017(2) 0.004(2) -0.002(2) C2 0.064(4) 0.038(3) 0.120(5) 0.031(3) 0.037(4) 0.012(3) C3 0.028(2) 0.047(2) 0.039(2) -0.005(2) 0.0045(18) 0.0120(19) C4 0.061(3) 0.077(4) 0.051(3) -0.001(3) -0.002(3) 0.033(3) C5 0.048(3) 0.058(3) 0.034(2) 0.008(2) 0.000(2) -0.012(2) C6 0.039(3) 0.091(4) 0.027(2) -0.015(2) -0.0026(19) 0.013(3) C7 0.059(3) 0.073(4) 0.083(4) -0.033(3) 0.036(3) -0.040(3) C8 0.049(3) 0.065(3) 0.064(3) -0.010(3) 0.009(3) -0.020(3) C9 0.068(3) 0.045(3) 0.055(3) -0.007(2) 0.011(3) -0.004(2) C10 0.056(3) 0.042(3) 0.135(5) -0.043(3) 0.043(3) -0.013(2) C11 0.053(3) 0.054(3) 0.032(2) 0.005(2) 0.006(2) -0.002(2) C12 0.098(4) 0.044(3) 0.053(3) 0.012(2) 0.009(3) -0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ce O2 2.492(2) 2_655 ? Ce O2 2.492(2) . ? Ce O1 2.496(3) . ? Ce O3 2.505(3) . ? Ce O3 2.505(3) 2_655 ? Ce Cl4 2.6964(9) . ? Ce Cl4 2.6964(9) 2_655 ? Te Cl1 2.3421(14) . ? Te Cl3 2.5066(10) 2 ? Te Cl3 2.5066(10) . ? Te Cl2 2.5145(11) 2 ? Te Cl2 2.5145(11) . ? Te O4 2.682(5) . ? O1 C1 1.453(4) 2_655 ? O1 C1 1.453(4) . ? O2 C6 1.457(5) . ? O2 C3 1.462(4) . ? O3 C10 1.443(5) . ? O3 C7 1.457(5) . ? O4 C11 1.399(5) 2 ? O4 C11 1.399(5) . ? C1 C2 1.492(7) . ? C2 C2 1.517(12) 2_655 ? C3 C4 1.481(6) . ? C4 C5 1.495(7) . ? C5 C6 1.496(6) . ? C7 C8 1.456(7) . ? C8 C9 1.471(7) . ? C9 C10 1.474(7) . ? C11 C12 1.477(7) . ? C12 C12 1.495(10) 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 O2 Ce O2 142.78(13) 2_655 . ? O2 Ce O1 71.39(6) 2_655 . ? O2 Ce O1 71.39(6) . . ? O2 Ce O3 144.59(9) 2_655 . ? O2 Ce O3 72.29(9) . . ? O1 Ce O3 143.16(7) . . ? O2 Ce O3 72.29(9) 2_655 2_655 ? O2 Ce O3 144.59(9) . 2_655 ? O1 Ce O3 143.16(7) . 2_655 ? O3 Ce O3 73.69(14) . 2_655 ? O2 Ce Cl4 86.80(6) 2_655 . ? O2 Ce Cl4 94.02(6) . . ? O1 Ce Cl4 91.29(2) . . ? O3 Ce Cl4 85.25(7) . . ? O3 Ce Cl4 92.68(7) 2_655 . ? O2 Ce Cl4 94.02(6) 2_655 2_655 ? O2 Ce Cl4 86.80(6) . 2_655 ? O1 Ce Cl4 91.29(2) . 2_655 ? O3 Ce Cl4 92.68(7) . 2_655 ? O3 Ce Cl4 85.25(7) 2_655 2_655 ? Cl4 Ce Cl4 177.42(5) . 2_655 ? Cl1 Te Cl3 89.36(3) . 2 ? Cl1 Te Cl3 89.36(3) . . ? Cl3 Te Cl3 178.72(5) 2 . ? Cl1 Te Cl2 88.40(3) . 2 ? Cl3 Te Cl2 89.47(4) 2 2 ? Cl3 Te Cl2 90.49(4) . 2 ? Cl1 Te Cl2 88.40(3) . . ? Cl3 Te Cl2 90.49(4) 2 . ? Cl3 Te Cl2 89.47(4) . . ? Cl2 Te Cl2 176.81(6) 2 . ? Cl1 Te O4 180.0000(10) . . ? Cl3 Te O4 90.64(3) 2 . ? Cl3 Te O4 90.64(3) . . ? Cl2 Te O4 91.60(3) 2 . ? Cl2 Te O4 91.60(3) . . ? C1 O1 C1 109.8(4) 2_655 . ? C1 O1 Ce 125.1(2) 2_655 . ? C1 O1 Ce 125.1(2) . . ? C6 O2 C3 108.7(3) . . ? C6 O2 Ce 123.8(2) . . ? C3 O2 Ce 126.7(2) . . ? C10 O3 C7 107.5(3) . . ? C10 O3 Ce 127.4(2) . . ? C7 O3 Ce 125.1(3) . . ? C11 O4 C11 112.3(5) 2 . ? C11 O4 Te 123.9(3) 2 . ? C11 O4 Te 123.9(3) . . ? O1 C1 C2 105.2(4) . . ? C1 C2 C2 103.0(3) . 2_655 ? O2 C3 C4 106.1(3) . . ? C3 C4 C5 104.5(4) . . ? C4 C5 C6 103.2(4) . . ? O2 C6 C5 105.2(3) . . ? C8 C7 O3 106.9(4) . . ? C7 C8 C9 108.1(4) . . ? C8 C9 C10 104.7(4) . . ? O3 C10 C9 106.7(4) . . ? O4 C11 C12 107.0(4) . . ? C11 C12 C12 105.6(3) . 2 ? #===END data_(3)-nov2103 _database_code_depnum_ccdc_archive 'CCDC 239403' _audit_creation_date 2003-11-25T09:33:11-00:00 _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 ; '[Li(thf)4][CeBr(Me4pip)3]' ; _chemical_formula_moiety '(C27 H54 Br1 Ce1 N3)(C16 H32 Li1 O4)' _chemical_formula_sum 'C43 H86 Br Ce Li N3 O4' _chemical_formula_weight 936.12 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2421(2) _cell_length_b 12.4515(3) _cell_length_c 17.4343(3) _cell_angle_alpha 87.202(1) _cell_angle_beta 88.215(1) _cell_angle_gamma 84.759(1) _cell_volume 2426.50(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20450 _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 colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 986 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.8 _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 0.5444 _exptl_absorpt_correction_T_max 0.6764 #----------------------------------------------------------------------------# # 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 -0.842042E-1 _diffrn_orient_matrix_ub_12 -0.200435E-1 _diffrn_orient_matrix_ub_13 0.31477E-2 _diffrn_orient_matrix_ub_21 -0.135646E-1 _diffrn_orient_matrix_ub_22 0.326176E-1 _diffrn_orient_matrix_ub_23 -0.529102E-1 _diffrn_orient_matrix_ub_31 0.26652E-1 _diffrn_orient_matrix_ub_32 -0.710808E-1 _diffrn_orient_matrix_ub_33 -0.22154E-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 0.0639 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_number 31019 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.16 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 8495 _reflns_number_gt 7772 _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^)+(0.0381P)^2^+3.3858P] 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 8495 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.088 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.842 _refine_diff_density_min -1.21 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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' 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 0.683070(15) 0.744899(14) 0.278287(10) 0.02389(7) Uani 1 1 d . . . Li Li 0.3227(6) 0.2817(6) 0.1415(4) 0.0457(15) Uani 1 1 d . . . Br Br 0.64753(4) 0.77511(4) 0.10732(2) 0.05529(13) Uani 1 1 d . . . O1 O 0.3135(3) 0.2619(3) 0.25038(16) 0.0558(8) Uani 1 1 d . . . O2 O 0.4829(3) 0.2372(3) 0.10821(19) 0.0682(9) Uani 1 1 d . . . O3 O 0.1996(2) 0.2002(3) 0.10683(17) 0.0552(8) Uani 1 1 d . . . O4 O 0.2850(3) 0.4296(2) 0.10710(17) 0.0607(8) Uani 1 1 d . . . N1 N 0.7984(2) 0.5752(2) 0.29816(16) 0.0306(6) Uani 1 1 d . . . N2 N 0.4834(2) 0.7495(2) 0.32804(16) 0.0287(6) Uani 1 1 d . . . N3 N 0.7877(2) 0.8952(2) 0.30632(15) 0.0273(6) Uani 1 1 d . . . C1 C 0.7687(3) 0.4815(3) 0.2558(2) 0.0393(9) Uani 1 1 d . . . C2 C 0.7531(4) 0.3814(3) 0.3091(3) 0.0475(10) Uani 1 1 d . . . H2A H 0.6787 0.3943 0.3405 0.057 Uiso 1 1 calc R . . H2B H 0.7443 0.319 0.2773 0.057 Uiso 1 1 calc R . . C3 C 0.8571(4) 0.3534(3) 0.3624(3) 0.0525(11) Uani 1 1 d . . . H3A H 0.8397 0.2925 0.3984 0.063 Uiso 1 1 calc R . . H3B H 0.9305 0.3316 0.3321 0.063 Uiso 1 1 calc R . . C4 C 0.8750(4) 0.4519(3) 0.4067(2) 0.0457(9) Uani 1 1 d . . . H4A H 0.9454 0.4356 0.4394 0.055 Uiso 1 1 calc R . . H4B H 0.8043 0.4676 0.441 0.055 Uiso 1 1 calc R . . C5 C 0.8934(3) 0.5526(3) 0.3554(2) 0.0361(8) Uani 1 1 d . . . C6 C 0.8588(4) 0.4512(4) 0.1900(3) 0.0567(11) Uani 1 1 d . . . H6A H 0.9377 0.4306 0.2113 0.085 Uiso 1 1 calc R . . H6B H 0.8635 0.5134 0.1537 0.085 Uiso 1 1 calc R . . H6C H 0.8323 0.3905 0.1633 0.085 Uiso 1 1 calc R . . C7 C 0.6492(4) 0.5120(3) 0.2169(2) 0.0482(10) Uani 1 1 d . . . H7A H 0.6558 0.5759 0.1825 0.072 Uiso 1 1 calc R . . H7B H 0.5866 0.5279 0.2561 0.072 Uiso 1 1 calc R . . H7C H 0.6288 0.4518 0.1872 0.072 Uiso 1 1 calc R . . C8 C 1.0222(3) 0.5409(4) 0.3200(3) 0.0539(11) Uani 1 1 d . . . H8A H 1.035 0.6045 0.2865 0.081 Uiso 1 1 calc R . . H8B H 1.0329 0.476 0.29 0.081 Uiso 1 1 calc R . . H8C H 1.08 0.5349 0.3613 0.081 Uiso 1 1 calc R . . C9 C 0.8881(3) 0.6491(3) 0.4064(2) 0.0421(9) Uani 1 1 d . . . H9A H 0.8999 0.7146 0.3746 0.063 Uiso 1 1 calc R . . H9B H 0.9509 0.6373 0.4443 0.063 Uiso 1 1 calc R . . H9C H 0.8098 0.6574 0.4329 0.063 Uiso 1 1 calc R . . C10 C 0.4442(3) 0.6754(3) 0.3905(2) 0.0346(8) Uani 1 1 d . . . C11 C 0.3678(3) 0.7343(4) 0.4531(2) 0.0482(10) Uani 1 1 d . . . H11A H 0.3366 0.6803 0.4902 0.058 Uiso 1 1 calc R . . H11B H 0.4188 0.7788 0.4813 0.058 Uiso 1 1 calc R . . C12 C 0.2637(3) 0.8062(4) 0.4197(3) 0.0529(11) Uani 1 1 d . . . H12A H 0.2086 0.7619 0.3948 0.063 Uiso 1 1 calc R . . H12B H 0.2187 0.8454 0.4611 0.063 Uiso 1 1 calc R . . C13 C 0.3131(3) 0.8856(3) 0.3615(2) 0.0450(10) Uani 1 1 d . . . H13A H 0.3622 0.9335 0.3882 0.054 Uiso 1 1 calc R . . H13B H 0.2458 0.9312 0.338 0.054 Uiso 1 1 calc R . . C14 C 0.3902(3) 0.8299(3) 0.2973(2) 0.0342(8) Uani 1 1 d . . . C15 C 0.3749(4) 0.5822(3) 0.3636(3) 0.0488(10) Uani 1 1 d . . . H15A H 0.3019 0.6125 0.3382 0.073 Uiso 1 1 calc R . . H15B H 0.3538 0.536 0.4081 0.073 Uiso 1 1 calc R . . H15C H 0.4254 0.5394 0.3274 0.073 Uiso 1 1 calc R . . C16 C 0.5565(3) 0.6226(3) 0.4291(2) 0.0399(8) Uani 1 1 d . . . H16A H 0.6079 0.5841 0.391 0.06 Uiso 1 1 calc R . . H16B H 0.5338 0.5716 0.4703 0.06 Uiso 1 1 calc R . . H16C H 0.5999 0.6784 0.4507 0.06 Uiso 1 1 calc R . . C17 C 0.4517(3) 0.9184(3) 0.2520(3) 0.0467(10) Uani 1 1 d . . . H17A H 0.5051 0.951 0.2857 0.07 Uiso 1 1 calc R . . H17B H 0.3912 0.9739 0.2325 0.07 Uiso 1 1 calc R . . H17C H 0.4981 0.887 0.2087 0.07 Uiso 1 1 calc R . . C18 C 0.3083(3) 0.7840(3) 0.2396(2) 0.0444(9) Uani 1 1 d . . . H18A H 0.2659 0.7264 0.2654 0.067 Uiso 1 1 calc R . . H18B H 0.3569 0.7546 0.1965 0.067 Uiso 1 1 calc R . . H18C H 0.2502 0.8417 0.2203 0.067 Uiso 1 1 calc R . . C19 C 0.8873(3) 0.9242(3) 0.2548(2) 0.0342(8) Uani 1 1 d . . . C20 C 1.0002(3) 0.9437(3) 0.2988(3) 0.0469(10) Uani 1 1 d . . . H20A H 1.0364 0.8737 0.3203 0.056 Uiso 1 1 calc R . . H20B H 1.0591 0.9736 0.2622 0.056 Uiso 1 1 calc R . . C21 C 0.9740(4) 1.0207(4) 0.3637(3) 0.0551(12) Uani 1 1 d . . . H21A H 1.0473 1.0256 0.3929 0.066 Uiso 1 1 calc R . . H21B H 0.9472 1.0938 0.3424 0.066 Uiso 1 1 calc R . . C22 C 0.8774(3) 0.9786(3) 0.4162(2) 0.0463(10) Uani 1 1 d . . . H22A H 0.8582 1.0296 0.4576 0.056 Uiso 1 1 calc R . . H22B H 0.9078 0.9083 0.4404 0.056 Uiso 1 1 calc R . . C23 C 0.7620(3) 0.9642(3) 0.3733(2) 0.0343(8) Uani 1 1 d . . . C24 C 0.8544(4) 1.0218(3) 0.1987(3) 0.0496(10) Uani 1 1 d . . . H24A H 0.8303 1.0857 0.228 0.074 Uiso 1 1 calc R . . H24B H 0.7881 1.0059 0.1671 0.074 Uiso 1 1 calc R . . H24C H 0.9238 1.0354 0.1654 0.074 Uiso 1 1 calc R . . C25 C 0.9240(3) 0.8284(3) 0.2045(2) 0.0417(9) Uani 1 1 d . . . H25A H 0.8555 0.8122 0.1751 0.063 Uiso 1 1 calc R . . H25B H 0.9507 0.7651 0.2373 0.063 Uiso 1 1 calc R . . H25C H 0.9893 0.8466 0.1691 0.063 Uiso 1 1 calc R . . C26 C 0.6972(3) 1.0767(3) 0.3527(3) 0.0445(9) Uani 1 1 d . . . H26A H 0.7475 1.1168 0.3168 0.067 Uiso 1 1 calc R . . H26B H 0.6819 1.1168 0.3996 0.067 Uiso 1 1 calc R . . H26C H 0.6212 1.0678 0.3288 0.067 Uiso 1 1 calc R . . C27 C 0.6795(3) 0.9063(3) 0.4288(2) 0.0418(9) Uani 1 1 d . . . H27A H 0.6054 0.8959 0.4032 0.063 Uiso 1 1 calc R . . H27B H 0.661 0.9498 0.4738 0.063 Uiso 1 1 calc R . . H27C H 0.719 0.8359 0.4454 0.063 Uiso 1 1 calc R . . C28 C 0.4100(5) 0.2722(5) 0.3012(3) 0.0712(14) Uani 1 1 d . . . H28A H 0.4276 0.3486 0.3023 0.085 Uiso 1 1 calc R . . H28B H 0.4831 0.2287 0.284 0.085 Uiso 1 1 calc R . . C29 C 0.3702(6) 0.2329(6) 0.3775(3) 0.095(2) Uani 1 1 d . . . H29A H 0.3991 0.2764 0.418 0.114 Uiso 1 1 calc R . . H29B H 0.4003 0.1564 0.3873 0.114 Uiso 1 1 calc R . . C30 C 0.2383(6) 0.2445(7) 0.3761(3) 0.110(3) Uani 1 1 d . . . H30A H 0.206 0.3172 0.3915 0.132 Uiso 1 1 calc R . . H30B H 0.2039 0.1895 0.4109 0.132 Uiso 1 1 calc R . . C31 C 0.2117(4) 0.2279(5) 0.2938(3) 0.0691(14) Uani 1 1 d . . . H31A H 0.2019 0.151 0.2861 0.083 Uiso 1 1 calc R . . H31B H 0.1378 0.2719 0.2782 0.083 Uiso 1 1 calc R . . C32 C 0.5379(6) 0.1355(7) 0.1225(5) 0.133(3) Uani 1 1 d . . . H32A H 0.4786 0.0835 0.1369 0.159 Uiso 1 1 calc R . . H32B H 0.5956 0.1352 0.1643 0.159 Uiso 1 1 calc R . . C33 C 0.6009(8) 0.1084(6) 0.0479(5) 0.113(3) Uani 1 1 d . . . H33A H 0.6663 0.0502 0.0552 0.136 Uiso 1 1 calc R . . H33B H 0.5449 0.0868 0.01 0.136 Uiso 1 1 calc R . . C34 C 0.6453(7) 0.2074(8) 0.0257(5) 0.137(3) Uani 1 1 d . . . H34A H 0.6586 0.2131 -0.0307 0.165 Uiso 1 1 calc R . . H34B H 0.722 0.214 0.0507 0.165 Uiso 1 1 calc R . . C35 C 0.5534(5) 0.2928(5) 0.0506(3) 0.0778(15) Uani 1 1 d . . . H35A H 0.5908 0.3528 0.0729 0.093 Uiso 1 1 calc R . . H35B H 0.5038 0.3219 0.0071 0.093 Uiso 1 1 calc R . . C36 C 0.0808(5) 0.2361(6) 0.0924(5) 0.125(3) Uani 1 1 d . . . H36A H 0.0738 0.3146 0.0795 0.15 Uiso 1 1 calc R . . H36B H 0.0303 0.2228 0.1389 0.15 Uiso 1 1 calc R . . C37 C 0.0404(4) 0.1792(4) 0.0295(3) 0.0673(13) Uani 1 1 d . . . H37A H 0.05 0.2208 -0.0198 0.081 Uiso 1 1 calc R . . H37B H -0.0446 0.1655 0.0373 0.081 Uiso 1 1 calc R . . C38 C 0.1193(4) 0.0756(4) 0.0307(3) 0.0632(13) Uani 1 1 d . . . H38A H 0.0761 0.0155 0.0535 0.076 Uiso 1 1 calc R . . H38B H 0.1474 0.0578 -0.0219 0.076 Uiso 1 1 calc R . . C39 C 0.2208(5) 0.0950(4) 0.0785(4) 0.0834(18) Uani 1 1 d . . . H39A H 0.2282 0.0406 0.1218 0.1 Uiso 1 1 calc R . . H39B H 0.2961 0.0892 0.0474 0.1 Uiso 1 1 calc R . . C40 C 0.2656(6) 0.5214(4) 0.1521(3) 0.0828(18) Uani 1 1 d . . . H40A H 0.341 0.5557 0.1564 0.099 Uiso 1 1 calc R . . H40B H 0.2367 0.5003 0.2044 0.099 Uiso 1 1 calc R . . C41 C 0.1742(5) 0.5982(4) 0.1131(3) 0.0727(15) Uani 1 1 d . . . H41A H 0.0983 0.6031 0.1436 0.087 Uiso 1 1 calc R . . H41B H 0.2027 0.6711 0.1067 0.087 Uiso 1 1 calc R . . C42 C 0.1570(6) 0.5537(4) 0.0373(3) 0.0860(18) Uani 1 1 d . . . H42A H 0.079 0.5227 0.0361 0.103 Uiso 1 1 calc R . . H42B H 0.1608 0.6103 -0.0044 0.103 Uiso 1 1 calc R . . C43 C 0.2565(7) 0.4691(5) 0.0295(3) 0.094(2) Uani 1 1 d . . . H43A H 0.2324 0.41 -0.001 0.113 Uiso 1 1 calc R . . H43B H 0.3265 0.4993 0.0035 0.113 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 Ce 0.02425(10) 0.02359(10) 0.02377(11) -0.00231(7) -0.00104(7) -0.00102(7) Li 0.044(3) 0.056(4) 0.037(3) 0.001(3) -0.002(3) 0.000(3) Br 0.0669(3) 0.0679(3) 0.0316(2) -0.00116(19) -0.00713(19) -0.0076(2) O1 0.0522(17) 0.078(2) 0.0368(15) 0.0023(14) -0.0053(13) -0.0037(15) O2 0.0484(17) 0.091(3) 0.059(2) 0.0122(18) 0.0110(15) 0.0119(17) O3 0.0495(16) 0.0643(19) 0.0543(18) -0.0215(15) 0.0001(14) -0.0091(14) O4 0.092(2) 0.0453(17) 0.0454(17) -0.0108(14) 0.0005(16) -0.0056(16) N1 0.0309(14) 0.0256(14) 0.0348(16) -0.0028(12) -0.0017(12) 0.0021(11) N2 0.0267(13) 0.0298(15) 0.0296(15) -0.0027(12) -0.0001(11) -0.0025(11) N3 0.0276(13) 0.0257(14) 0.0291(15) -0.0018(11) -0.0019(11) -0.0038(11) C1 0.047(2) 0.0299(18) 0.041(2) -0.0096(16) 0.0021(17) 0.0017(16) C2 0.059(2) 0.0278(19) 0.056(3) -0.0079(18) 0.000(2) -0.0068(17) C3 0.059(3) 0.029(2) 0.066(3) 0.0060(19) 0.000(2) 0.0065(18) C4 0.044(2) 0.037(2) 0.055(3) 0.0096(18) -0.0108(19) 0.0027(17) C5 0.0291(17) 0.0312(18) 0.047(2) 0.0022(16) -0.0032(15) 0.0022(14) C6 0.067(3) 0.050(3) 0.051(3) -0.018(2) 0.014(2) 0.008(2) C7 0.058(2) 0.039(2) 0.050(2) -0.0173(19) -0.013(2) -0.0047(18) C8 0.0314(19) 0.050(2) 0.077(3) 0.008(2) 0.002(2) 0.0034(17) C9 0.042(2) 0.038(2) 0.047(2) 0.0034(17) -0.0173(17) -0.0014(16) C10 0.0314(17) 0.039(2) 0.0335(19) -0.0003(15) 0.0056(15) -0.0063(15) C11 0.042(2) 0.064(3) 0.037(2) -0.0049(19) 0.0106(17) 0.0004(19) C12 0.039(2) 0.065(3) 0.053(3) -0.020(2) 0.0122(19) 0.007(2) C13 0.0337(19) 0.044(2) 0.057(3) -0.0157(19) -0.0040(18) 0.0061(16) C14 0.0285(16) 0.0367(19) 0.037(2) -0.0051(15) -0.0050(15) 0.0015(14) C15 0.042(2) 0.045(2) 0.061(3) 0.001(2) 0.0052(19) -0.0160(18) C16 0.044(2) 0.038(2) 0.037(2) 0.0094(16) 0.0018(16) -0.0044(16) C17 0.040(2) 0.038(2) 0.060(3) 0.0095(18) -0.0132(19) 0.0039(16) C18 0.0345(19) 0.052(2) 0.047(2) -0.0095(19) -0.0107(17) 0.0017(17) C19 0.0257(16) 0.0340(18) 0.043(2) -0.0013(16) -0.0013(15) -0.0054(14) C20 0.0293(18) 0.046(2) 0.066(3) -0.008(2) -0.0078(18) -0.0037(16) C21 0.040(2) 0.049(2) 0.080(3) -0.019(2) -0.019(2) -0.0092(18) C22 0.048(2) 0.043(2) 0.050(2) -0.0187(19) -0.0180(19) 0.0013(18) C23 0.0372(18) 0.0282(17) 0.038(2) -0.0095(15) -0.0066(15) -0.0005(14) C24 0.043(2) 0.046(2) 0.059(3) 0.014(2) 0.0069(19) -0.0098(18) C25 0.0350(19) 0.049(2) 0.041(2) -0.0053(18) 0.0071(16) -0.0052(16) C26 0.041(2) 0.0296(19) 0.063(3) -0.0137(18) -0.0032(18) 0.0025(16) C27 0.050(2) 0.042(2) 0.033(2) -0.0114(17) 0.0002(17) -0.0025(17) C28 0.078(3) 0.080(4) 0.058(3) -0.004(3) -0.022(3) -0.014(3) C29 0.096(4) 0.143(6) 0.048(3) 0.007(3) -0.015(3) -0.025(4) C30 0.104(5) 0.179(8) 0.036(3) -0.005(4) 0.007(3) 0.044(5) C31 0.057(3) 0.099(4) 0.049(3) 0.000(3) 0.004(2) 0.007(3) C32 0.087(5) 0.119(6) 0.173(8) 0.069(6) 0.043(5) 0.038(4) C33 0.133(6) 0.097(5) 0.105(6) -0.037(5) -0.042(5) 0.046(5) C34 0.083(5) 0.163(9) 0.152(8) 0.017(6) 0.068(5) 0.026(5) C35 0.083(4) 0.081(4) 0.074(4) 0.000(3) 0.009(3) -0.032(3) C36 0.051(3) 0.095(5) 0.235(10) -0.089(6) -0.029(4) 0.009(3) C37 0.060(3) 0.081(4) 0.060(3) -0.007(3) -0.010(2) 0.001(3) C38 0.060(3) 0.063(3) 0.070(3) -0.025(3) 0.000(2) -0.011(2) C39 0.099(4) 0.051(3) 0.101(4) -0.017(3) -0.044(4) 0.007(3) C40 0.114(5) 0.070(3) 0.063(3) -0.030(3) -0.023(3) 0.018(3) C41 0.091(4) 0.071(3) 0.054(3) -0.005(2) -0.006(3) 0.010(3) C42 0.126(5) 0.059(3) 0.074(4) -0.007(3) -0.035(4) 0.004(3) C43 0.174(7) 0.067(4) 0.037(3) -0.005(2) 0.004(3) 0.009(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 2.377(3) . ? Ce N2 2.378(3) . ? Ce N1 2.392(3) . ? Ce Br 3.0203(4) . ? Li O1 1.903(7) . ? Li O2 1.916(7) . ? Li O3 1.918(7) . ? Li O4 1.922(8) . ? O1 C31 1.437(6) . ? O1 C28 1.441(5) . ? O2 C32 1.373(7) . ? O2 C35 1.449(6) . ? O3 C36 1.396(6) . ? O3 C39 1.420(5) . ? O4 C40 1.415(5) . ? O4 C43 1.453(6) . ? N1 C1 1.479(4) . ? N1 C5 1.483(4) . ? N2 C10 1.476(5) . ? N2 C14 1.476(4) . ? N3 C19 1.473(5) . ? N3 C23 1.489(4) . ? C1 C7 1.532(5) . ? C1 C2 1.538(6) . ? C1 C6 1.543(5) . ? C2 C3 1.521(6) . ? C3 C4 1.513(6) . ? C4 C5 1.529(5) . ? C5 C9 1.525(5) . ? C5 C8 1.553(5) . ? C10 C16 1.529(5) . ? C10 C11 1.539(5) . ? C10 C15 1.554(5) . ? C11 C12 1.520(6) . ? C12 C13 1.511(6) . ? C13 C14 1.547(5) . ? C14 C17 1.528(6) . ? C14 C18 1.548(5) . ? C19 C25 1.533(5) . ? C19 C20 1.546(5) . ? C19 C24 1.548(5) . ? C20 C21 1.524(6) . ? C21 C22 1.513(7) . ? C22 C23 1.546(5) . ? C23 C27 1.522(6) . ? C23 C26 1.551(5) . ? C28 C29 1.466(8) . ? C29 C30 1.478(8) . ? C30 C31 1.504(7) . ? C32 C33 1.500(10) . ? C33 C34 1.404(11) . ? C34 C35 1.485(9) . ? C36 C37 1.441(7) . ? C37 C38 1.497(7) . ? C38 C39 1.478(6) . ? C40 C41 1.493(7) . ? C41 C42 1.483(7) . ? C42 C43 1.472(8) . ? 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 N2 115.22(9) . . ? N3 Ce N1 113.34(9) . . ? N2 Ce N1 114.60(10) . . ? N3 Ce Br 103.11(7) . . ? N2 Ce Br 102.38(6) . . ? N1 Ce Br 106.35(7) . . ? O1 Li O2 107.9(3) . . ? O1 Li O3 103.9(4) . . ? O2 Li O3 116.5(4) . . ? O1 Li O4 112.6(4) . . ? O2 Li O4 108.6(4) . . ? O3 Li O4 107.4(3) . . ? C31 O1 C28 109.8(4) . . ? C31 O1 Li 125.0(3) . . ? C28 O1 Li 125.1(4) . . ? C32 O2 C35 108.5(4) . . ? C32 O2 Li 123.8(4) . . ? C35 O2 Li 126.1(4) . . ? C36 O3 C39 107.2(4) . . ? C36 O3 Li 128.1(4) . . ? C39 O3 Li 124.0(4) . . ? C40 O4 C43 104.8(4) . . ? C40 O4 Li 128.1(4) . . ? C43 O4 Li 126.7(3) . . ? C1 N1 C5 115.8(3) . . ? C1 N1 Ce 119.2(2) . . ? C5 N1 Ce 124.9(2) . . ? C10 N2 C14 115.8(3) . . ? C10 N2 Ce 123.6(2) . . ? C14 N2 Ce 120.5(2) . . ? C19 N3 C23 115.7(3) . . ? C19 N3 Ce 118.94(19) . . ? C23 N3 Ce 125.4(2) . . ? N1 C1 C7 108.0(3) . . ? N1 C1 C2 112.4(3) . . ? C7 C1 C2 107.2(3) . . ? N1 C1 C6 113.7(3) . . ? C7 C1 C6 105.4(3) . . ? C2 C1 C6 109.5(3) . . ? C3 C2 C1 113.2(3) . . ? C4 C3 C2 108.4(3) . . ? C3 C4 C5 113.6(3) . . ? N1 C5 C9 107.4(3) . . ? N1 C5 C4 112.2(3) . . ? C9 C5 C4 108.1(3) . . ? N1 C5 C8 114.3(3) . . ? C9 C5 C8 106.0(3) . . ? C4 C5 C8 108.6(3) . . ? N2 C10 C16 107.3(3) . . ? N2 C10 C11 112.8(3) . . ? C16 C10 C11 106.8(3) . . ? N2 C10 C15 114.6(3) . . ? C16 C10 C15 106.7(3) . . ? C11 C10 C15 108.3(3) . . ? C12 C11 C10 112.1(3) . . ? C13 C12 C11 108.3(3) . . ? C12 C13 C14 112.9(3) . . ? N2 C14 C17 108.3(3) . . ? N2 C14 C13 112.4(3) . . ? C17 C14 C13 106.8(3) . . ? N2 C14 C18 113.6(3) . . ? C17 C14 C18 105.5(3) . . ? C13 C14 C18 109.7(3) . . ? N3 C19 C25 108.2(3) . . ? N3 C19 C20 112.8(3) . . ? C25 C19 C20 105.8(3) . . ? N3 C19 C24 113.8(3) . . ? C25 C19 C24 106.0(3) . . ? C20 C19 C24 109.7(3) . . ? C21 C20 C19 113.0(3) . . ? C22 C21 C20 108.7(3) . . ? C21 C22 C23 112.6(3) . . ? N3 C23 C27 107.5(3) . . ? N3 C23 C22 111.2(3) . . ? C27 C23 C22 107.5(3) . . ? N3 C23 C26 114.1(3) . . ? C27 C23 C26 106.9(3) . . ? C22 C23 C26 109.3(3) . . ? O1 C28 C29 106.4(5) . . ? C28 C29 C30 105.2(5) . . ? C29 C30 C31 103.7(4) . . ? O1 C31 C30 105.0(5) . . ? O2 C32 C33 104.0(6) . . ? C34 C33 C32 101.1(6) . . ? C33 C34 C35 106.3(6) . . ? O2 C35 C34 103.5(5) . . ? O3 C36 C37 109.4(4) . . ? C36 C37 C38 103.9(4) . . ? C39 C38 C37 105.1(4) . . ? O3 C39 C38 108.3(4) . . ? O4 C40 C41 107.6(4) . . ? C42 C41 C40 105.8(4) . . ? C43 C42 C41 104.2(4) . . ? O4 C43 C42 106.1(4) . . ? #===END data_(10)-may2503 _database_code_depnum_ccdc_archive 'CCDC 239404' _audit_creation_date 2003-05-21T15:25:15-00:00 _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 'C34 H60 Br1 La1 N2 O1 Si2' _chemical_formula_sum 'C34 H60 Br1 La1 N2 O1 Si2' _chemical_formula_weight 787.84 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6659(1) _cell_length_b 12.4805(2) _cell_length_c 17.0322(3) _cell_angle_alpha 101.176(1) _cell_angle_beta 92.494(1) _cell_angle_gamma 101.928(1) _cell_volume 1964.71(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11498 _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 colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.191 _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 0.5205 _exptl_absorpt_correction_T_max 0.6436 #----------------------------------------------------------------------------# # 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 -0.751445E-1 _diffrn_orient_matrix_ub_12 -0.687645E-1 _diffrn_orient_matrix_ub_13 -0.9971E-3 _diffrn_orient_matrix_ub_21 -0.476029E-1 _diffrn_orient_matrix_ub_22 0.434181E-1 _diffrn_orient_matrix_ub_23 0.420685E-1 _diffrn_orient_matrix_ub_31 -0.579097E-1 _diffrn_orient_matrix_ub_32 0.198623E-1 _diffrn_orient_matrix_ub_33 -0.428754E-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 0.0391 _diffrn_reflns_av_unetI/netI 0.0358 _diffrn_reflns_number 20977 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 6846 _reflns_number_gt 5955 _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 thf ligand was disodered over two orientations. The disordered carbon atoms were left isotropic. 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^)+(0.0226P)^2^+6.0407P] 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 6846 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.168 _refine_diff_density_min -0.973 _refine_diff_density_rms 0.081 #----------------------------------------------------------------------------# # 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 La La 0.34352(3) 0.27800(2) 0.284077(14) 0.04101(10) Uani 1 1 d . A . Br Br 0.63224(8) 0.33911(5) 0.35235(4) 0.0864(2) Uani 1 1 d . . . Si1 Si 0.38902(13) 0.17601(9) 0.08226(7) 0.0359(3) Uani 1 1 d . A . Si2 Si 0.32463(15) -0.01782(10) 0.31805(8) 0.0468(3) Uani 1 1 d . A . O O 0.1975(5) 0.4208(3) 0.3246(2) 0.0708(12) Uani 1 1 d . . . N1 N 0.3370(3) 0.2807(3) 0.14731(18) 0.0295(7) Uani 1 1 d . . . N2 N 0.2655(4) 0.1019(3) 0.31392(19) 0.0374(8) Uani 1 1 d . . . C1 C 0.3069(4) 0.3810(3) 0.1296(2) 0.0274(8) Uani 1 1 d . A . C2 C 0.1703(4) 0.3842(3) 0.0973(2) 0.0339(9) Uani 1 1 d . . . C3 C 0.1420(5) 0.4865(4) 0.0883(3) 0.0437(10) Uani 1 1 d . A . H3 H 0.0498 0.4883 0.0675 0.052 Uiso 1 1 calc R . . C4 C 0.2425(5) 0.5847(4) 0.1085(3) 0.0445(11) Uani 1 1 d . . . H4 H 0.2201 0.6535 0.1026 0.053 Uiso 1 1 calc R A . C5 C 0.3768(5) 0.5818(3) 0.1375(2) 0.0383(10) Uani 1 1 d . A . H5 H 0.4472 0.6494 0.1508 0.046 Uiso 1 1 calc R . . C6 C 0.4121(4) 0.4826(3) 0.1480(2) 0.0308(8) Uani 1 1 d . . . C7 C 0.0575(5) 0.2784(4) 0.0659(3) 0.0422(10) Uani 1 1 d . A . H7 H 0.0832 0.2173 0.0898 0.051 Uiso 1 1 calc R . . C8 C -0.0921(5) 0.2874(5) 0.0867(4) 0.0606(14) Uani 1 1 d . . . H8A H -0.1584 0.2158 0.0648 0.091 Uiso 1 1 calc R A . H8B H -0.1202 0.3465 0.0635 0.091 Uiso 1 1 calc R . . H8C H -0.0939 0.3055 0.1452 0.091 Uiso 1 1 calc R . . C9 C 0.0577(6) 0.2445(4) -0.0254(3) 0.0571(13) Uani 1 1 d . . . H9A H -0.0149 0.1759 -0.0455 0.086 Uiso 1 1 calc R A . H9B H 0.1511 0.2313 -0.0389 0.086 Uiso 1 1 calc R . . H9C H 0.0369 0.3047 -0.0502 0.086 Uiso 1 1 calc R . . C10 C 0.5659(4) 0.4879(4) 0.1761(3) 0.0396(10) Uani 1 1 d . A . H10 H 0.5733 0.4123 0.185 0.047 Uiso 1 1 calc R . . C11 C 0.6160(6) 0.5734(4) 0.2550(3) 0.0605(14) Uani 1 1 d . . . H11A H 0.7149 0.5739 0.2709 0.091 Uiso 1 1 calc R A . H11B H 0.5562 0.5529 0.2972 0.091 Uiso 1 1 calc R . . H11C H 0.609 0.6481 0.2475 0.091 Uiso 1 1 calc R . . C12 C 0.6643(6) 0.5175(5) 0.1113(4) 0.0656(15) Uani 1 1 d . . . H12A H 0.7626 0.5205 0.1301 0.098 Uiso 1 1 calc R A . H12B H 0.6566 0.5906 0.1008 0.098 Uiso 1 1 calc R . . H12C H 0.6366 0.4603 0.0618 0.098 Uiso 1 1 calc R . . C13 C 0.2444(6) 0.0471(4) 0.0493(3) 0.0542(12) Uani 1 1 d . . . H13A H 0.2041 0.0234 0.0967 0.081 Uiso 1 1 calc R A . H13B H 0.2835 -0.013 0.0186 0.081 Uiso 1 1 calc R . . H13C H 0.1699 0.0633 0.0155 0.081 Uiso 1 1 calc R . . C14 C 0.4655(6) 0.2204(5) -0.0080(3) 0.0629(15) Uani 1 1 d . . . H14A H 0.5414 0.2878 0.009 0.094 Uiso 1 1 calc R A . H14B H 0.391 0.2367 -0.0418 0.094 Uiso 1 1 calc R . . H14C H 0.5043 0.1602 -0.0387 0.094 Uiso 1 1 calc R . . C15 C 0.5285(6) 0.1329(4) 0.1415(3) 0.0570(13) Uani 1 1 d . . . H15A H 0.4892 0.1096 0.1892 0.085 Uiso 1 1 calc R A . H15B H 0.6098 0.1963 0.1583 0.085 Uiso 1 1 calc R . . H15C H 0.5594 0.0704 0.1082 0.085 Uiso 1 1 calc R . . C16 C 0.1498(5) 0.1272(4) 0.3575(2) 0.0438(11) Uani 1 1 d . A . C17 C 0.0086(6) 0.0844(4) 0.3249(3) 0.0525(12) Uani 1 1 d . . . C18 C -0.1016(7) 0.1163(6) 0.3671(4) 0.0808(19) Uani 1 1 d . A . H18 H -0.1969 0.0873 0.3447 0.097 Uiso 1 1 calc R . . C19 C -0.0751(11) 0.1890(7) 0.4405(5) 0.106(3) Uani 1 1 d . . . H19 H -0.1512 0.2115 0.4679 0.128 Uiso 1 1 calc R A . C20 C 0.0599(11) 0.2283(6) 0.4736(4) 0.091(2) Uani 1 1 d . A . H20 H 0.0768 0.2773 0.5249 0.109 Uiso 1 1 calc R . . C21 C 0.1754(7) 0.1993(4) 0.4349(3) 0.0608(15) Uani 1 1 d . . . C22 C -0.0282(5) 0.0028(4) 0.2441(3) 0.0552(12) Uani 1 1 d . A . H22 H 0.0626 -0.0128 0.2236 0.066 Uiso 1 1 calc R . . C23 C -0.1226(9) -0.1085(6) 0.2514(5) 0.111(3) Uani 1 1 d . . . H23A H -0.0762 -0.1407 0.2906 0.166 Uiso 1 1 calc R A . H23B H -0.1381 -0.1602 0.199 0.166 Uiso 1 1 calc R . . H23C H -0.214 -0.096 0.2693 0.166 Uiso 1 1 calc R . . C24 C -0.0963(8) 0.0530(7) 0.1846(4) 0.092(2) Uani 1 1 d . . . H24A H -0.1183 -0.0007 0.1331 0.138 Uiso 1 1 calc R A . H24B H -0.0315 0.1213 0.1774 0.138 Uiso 1 1 calc R . . H24C H -0.1842 0.0715 0.2041 0.138 Uiso 1 1 calc R . . C25 C 0.3217(8) 0.2415(5) 0.4784(3) 0.079(2) Uani 1 1 d . A . H25 H 0.3919 0.2178 0.4411 0.095 Uiso 1 1 calc R . . C26 C 0.3617(11) 0.3697(5) 0.5050(4) 0.116(3) Uani 1 1 d . . . H26A H 0.4575 0.3926 0.5325 0.174 Uiso 1 1 calc R A . H26B H 0.294 0.3947 0.5418 0.174 Uiso 1 1 calc R . . H26C H 0.359 0.4035 0.4578 0.174 Uiso 1 1 calc R . . C27 C 0.3342(10) 0.1905(6) 0.5530(4) 0.112(3) Uani 1 1 d . . . H27A H 0.4301 0.2187 0.58 0.167 Uiso 1 1 calc R A . H27B H 0.3157 0.1088 0.5365 0.167 Uiso 1 1 calc R . . H27C H 0.2647 0.2115 0.5899 0.167 Uiso 1 1 calc R . . C28 C 0.2316(9) -0.0952(5) 0.3896(5) 0.103(3) Uani 1 1 d . . . H28A H 0.1294 -0.1155 0.3735 0.155 Uiso 1 1 calc R A . H28B H 0.2489 -0.0479 0.4437 0.155 Uiso 1 1 calc R . . H28C H 0.267 -0.1634 0.3895 0.155 Uiso 1 1 calc R . . C29 C 0.3023(8) -0.1165(5) 0.2193(4) 0.085(2) Uani 1 1 d . . . H29A H 0.3508 -0.0783 0.1798 0.127 Uiso 1 1 calc R A . H29B H 0.201 -0.1427 0.2015 0.127 Uiso 1 1 calc R . . H29C H 0.3432 -0.1807 0.2245 0.127 Uiso 1 1 calc R . . C30 C 0.5171(7) 0.0176(6) 0.3498(6) 0.115(3) Uani 1 1 d . . . H30A H 0.5685 0.0586 0.3125 0.172 Uiso 1 1 calc R A . H30B H 0.5506 -0.0513 0.3497 0.172 Uiso 1 1 calc R . . H30C H 0.5341 0.0644 0.4041 0.172 Uiso 1 1 calc R . . C31 C 0.2400(9) 0.5390(7) 0.3390(5) 0.111(3) Uiso 0.511(13) 1 d P A 1 H31A H 0.2319 0.5658 0.2883 0.133 Uiso 0.511(13) 1 calc PR A 1 H31B H 0.3396 0.5643 0.3626 0.133 Uiso 0.511(13) 1 calc PR A 1 C32 C 0.1460(16) 0.5807(12) 0.3940(10) 0.090(5) Uiso 0.511(13) 1 d P A 1 H32A H 0.1898 0.5959 0.4498 0.108 Uiso 0.511(13) 1 calc PR A 1 H32B H 0.1274 0.6515 0.3826 0.108 Uiso 0.511(13) 1 calc PR A 1 C33 C 0.0174(16) 0.4994(12) 0.3851(10) 0.094(5) Uiso 0.511(13) 1 d P A 1 H33A H -0.0617 0.5271 0.3631 0.113 Uiso 0.511(13) 1 calc PR A 1 H33B H -0.0061 0.4802 0.4374 0.113 Uiso 0.511(13) 1 calc PR A 1 C34 C 0.0452(10) 0.3934(8) 0.3242(6) 0.122(3) Uiso 0.511(13) 1 d P A 1 H34A H 0.012 0.3234 0.3436 0.147 Uiso 0.511(13) 1 calc PR A 1 H34B H -0.0016 0.3859 0.2699 0.147 Uiso 0.511(13) 1 calc PR A 1 C31A C 0.2400(9) 0.5390(7) 0.3390(5) 0.111(3) Uiso 0.489(13) 1 d P A 2 H31C H 0.295 0.5635 0.2955 0.133 Uiso 0.489(13) 1 calc PR A 2 H31D H 0.2981 0.569 0.3909 0.133 Uiso 0.489(13) 1 calc PR A 2 C32A C 0.0902(16) 0.5785(13) 0.3406(11) 0.088(5) Uiso 0.489(13) 1 d P A 2 H32C H 0.0724 0.6085 0.3965 0.105 Uiso 0.489(13) 1 calc PR A 2 H32D H 0.092 0.6378 0.3093 0.105 Uiso 0.489(13) 1 calc PR A 2 C33A C 0.001(2) 0.4995(17) 0.3121(13) 0.121(7) Uiso 0.489(13) 1 d P A 2 H33C H -0.0163 0.4965 0.254 0.146 Uiso 0.489(13) 1 calc PR A 2 H33D H -0.088 0.5049 0.3374 0.146 Uiso 0.489(13) 1 calc PR A 2 C34A C 0.0452(10) 0.3934(8) 0.3242(6) 0.122(3) Uiso 0.489(13) 1 d P A 2 H34C H 0.0161 0.3744 0.3757 0.147 Uiso 0.489(13) 1 calc PR A 2 H34D H 0.0027 0.3295 0.2798 0.147 Uiso 0.489(13) 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 La 0.06715(19) 0.02555(13) 0.02986(14) 0.00453(9) 0.00255(11) 0.01062(11) Br 0.1000(5) 0.0620(4) 0.0829(4) 0.0265(3) -0.0460(4) -0.0139(3) Si1 0.0466(7) 0.0268(6) 0.0366(6) 0.0068(5) 0.0101(5) 0.0115(5) Si2 0.0581(8) 0.0321(6) 0.0549(8) 0.0163(6) 0.0064(6) 0.0138(6) O 0.134(4) 0.0343(18) 0.059(2) 0.0157(16) 0.048(2) 0.039(2) N1 0.0324(17) 0.0255(16) 0.0315(17) 0.0059(13) 0.0030(13) 0.0082(13) N2 0.051(2) 0.0282(18) 0.0325(18) 0.0052(14) 0.0050(16) 0.0094(16) C1 0.037(2) 0.0248(19) 0.0223(18) 0.0049(15) 0.0065(15) 0.0105(16) C2 0.037(2) 0.032(2) 0.034(2) 0.0069(17) 0.0014(17) 0.0094(17) C3 0.045(3) 0.041(3) 0.048(3) 0.009(2) -0.005(2) 0.018(2) C4 0.060(3) 0.029(2) 0.048(3) 0.0087(19) -0.002(2) 0.018(2) C5 0.049(3) 0.027(2) 0.037(2) 0.0050(17) -0.0011(19) 0.0070(18) C6 0.041(2) 0.028(2) 0.0242(18) 0.0044(15) 0.0025(16) 0.0090(17) C7 0.039(2) 0.035(2) 0.052(3) 0.009(2) -0.004(2) 0.0081(19) C8 0.042(3) 0.059(3) 0.083(4) 0.020(3) 0.002(3) 0.010(2) C9 0.062(3) 0.044(3) 0.055(3) -0.001(2) -0.013(2) 0.003(2) C10 0.042(2) 0.032(2) 0.043(2) 0.0059(18) -0.0029(19) 0.0060(18) C11 0.064(3) 0.046(3) 0.062(3) -0.001(2) -0.021(3) 0.006(2) C12 0.047(3) 0.074(4) 0.080(4) 0.023(3) 0.019(3) 0.013(3) C13 0.068(3) 0.033(2) 0.055(3) -0.004(2) 0.006(2) 0.009(2) C14 0.087(4) 0.055(3) 0.056(3) 0.017(3) 0.033(3) 0.026(3) C15 0.066(3) 0.047(3) 0.068(3) 0.012(2) 0.011(3) 0.033(3) C16 0.070(3) 0.033(2) 0.034(2) 0.0107(18) 0.010(2) 0.020(2) C17 0.069(3) 0.055(3) 0.044(3) 0.015(2) 0.020(2) 0.031(3) C18 0.084(4) 0.098(5) 0.080(4) 0.028(4) 0.039(4) 0.047(4) C19 0.154(8) 0.121(7) 0.075(5) 0.025(5) 0.067(5) 0.083(6) C20 0.170(8) 0.074(4) 0.045(3) 0.006(3) 0.036(4) 0.063(5) C21 0.114(5) 0.042(3) 0.035(2) 0.010(2) 0.014(3) 0.033(3) C22 0.049(3) 0.065(3) 0.055(3) 0.016(3) 0.012(2) 0.014(2) C23 0.145(7) 0.069(5) 0.106(6) 0.011(4) 0.053(5) -0.008(5) C24 0.100(5) 0.112(6) 0.068(4) 0.019(4) -0.011(4) 0.037(4) C25 0.148(6) 0.049(3) 0.035(3) 0.002(2) -0.013(3) 0.020(4) C26 0.231(10) 0.048(4) 0.050(4) 0.000(3) -0.029(5) 0.006(5) C27 0.210(9) 0.069(4) 0.055(4) 0.020(3) -0.028(5) 0.031(5) C28 0.159(7) 0.061(4) 0.120(6) 0.056(4) 0.065(5) 0.048(4) C29 0.125(6) 0.058(4) 0.082(4) 0.003(3) 0.017(4) 0.052(4) C30 0.080(5) 0.077(5) 0.198(9) 0.063(5) -0.047(5) 0.019(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 La N2 2.332(3) . ? La N1 2.335(3) . ? La O 2.508(3) . ? La Br 2.8664(7) . ? Si1 N1 1.717(3) . ? Si1 C14 1.865(5) . ? Si1 C13 1.874(5) . ? Si1 C15 1.876(5) . ? Si2 N2 1.719(3) . ? Si2 C28 1.849(6) . ? Si2 C30 1.852(7) . ? Si2 C29 1.857(6) . ? O C31 1.415(9) . ? O C34 1.441(10) . ? N1 C1 1.424(5) . ? N2 C16 1.424(6) . ? C1 C2 1.420(5) . ? C1 C6 1.423(5) . ? C2 C3 1.394(6) . ? C2 C7 1.516(6) . ? C3 C4 1.371(6) . ? C4 C5 1.379(6) . ? C5 C6 1.391(5) . ? C6 C10 1.526(6) . ? C7 C8 1.525(6) . ? C7 C9 1.530(6) . ? C10 C11 1.535(6) . ? C10 C12 1.537(7) . ? C16 C17 1.406(7) . ? C16 C21 1.424(6) . ? C17 C18 1.393(7) . ? C17 C22 1.523(7) . ? C18 C19 1.375(10) . ? C19 C20 1.351(11) . ? C20 C21 1.397(9) . ? C21 C25 1.509(9) . ? C22 C24 1.488(8) . ? C22 C23 1.527(8) . ? C25 C26 1.537(8) . ? C25 C27 1.537(8) . ? C31 C32 1.434(15) . ? C32 C33 1.414(19) . ? C33 C34 1.593(17) . ? C32A C33A 1.17(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 N2 La N1 115.06(11) . . ? N2 La O 117.43(12) . . ? N1 La O 97.49(11) . . ? N2 La Br 102.14(9) . . ? N1 La Br 109.62(8) . . ? O La Br 115.53(11) . . ? N1 Si1 C14 113.8(2) . . ? N1 Si1 C13 113.21(19) . . ? C14 Si1 C13 109.3(3) . . ? N1 Si1 C15 105.60(19) . . ? C14 Si1 C15 109.0(3) . . ? C13 Si1 C15 105.5(2) . . ? N2 Si2 C28 112.0(2) . . ? N2 Si2 C30 110.1(3) . . ? C28 Si2 C30 108.2(4) . . ? N2 Si2 C29 113.1(2) . . ? C28 Si2 C29 107.2(3) . . ? C30 Si2 C29 106.0(4) . . ? C31 O C34 107.1(6) . . ? C31 O La 128.7(4) . . ? C34 O La 123.6(4) . . ? C1 N1 Si1 127.0(2) . . ? C1 N1 La 113.3(2) . . ? Si1 N1 La 119.09(16) . . ? C16 N2 Si2 120.6(3) . . ? C16 N2 La 97.0(2) . . ? Si2 N2 La 140.3(2) . . ? C2 C1 C6 118.0(3) . . ? C2 C1 N1 121.5(3) . . ? C6 C1 N1 120.4(3) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 C7 118.7(4) . . ? C1 C2 C7 121.8(3) . . ? C4 C3 C2 122.3(4) . . ? C3 C4 C5 118.7(4) . . ? C4 C5 C6 121.9(4) . . ? C5 C6 C1 119.6(4) . . ? C5 C6 C10 117.5(4) . . ? C1 C6 C10 122.9(3) . . ? C2 C7 C8 114.4(4) . . ? C2 C7 C9 109.6(4) . . ? C8 C7 C9 109.1(4) . . ? C6 C10 C11 112.3(4) . . ? C6 C10 C12 110.3(4) . . ? C11 C10 C12 109.2(4) . . ? C17 C16 N2 121.3(4) . . ? C17 C16 C21 118.4(5) . . ? N2 C16 C21 120.3(5) . . ? C18 C17 C16 119.7(5) . . ? C18 C17 C22 118.6(5) . . ? C16 C17 C22 121.7(4) . . ? C19 C18 C17 121.2(7) . . ? C20 C19 C18 119.7(6) . . ? C19 C20 C21 122.1(6) . . ? C20 C21 C16 118.8(6) . . ? C20 C21 C25 118.5(5) . . ? C16 C21 C25 122.6(5) . . ? C24 C22 C17 111.0(5) . . ? C24 C22 C23 110.4(6) . . ? C17 C22 C23 112.1(5) . . ? C21 C25 C26 112.8(6) . . ? C21 C25 C27 110.9(6) . . ? C26 C25 C27 108.4(5) . . ? O C31 C32 106.0(8) . . ? C33 C32 C31 108.6(12) . . ? C32 C33 C34 105.1(11) . . ? O C34 C33 101.4(8) . . ? #===END data_(5)-sep1703 _database_code_depnum_ccdc_archive 'CCDC 239405' _audit_creation_date 2003-09-19T16:56:54-00:00 _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 ; '[(NC9H6Me2)4Y2(OEt)(OBu)]' ; _chemical_formula_moiety 'C42 H86 N4 O2 Y2' _chemical_formula_sum 'C42 H86 N4 O2 Y2' _chemical_formula_weight 856.97 _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 11.1342(2) _cell_length_b 13.6283(2) _cell_length_c 16.5081(4) _cell_angle_alpha 71.033(1) _cell_angle_beta 90.576(1) _cell_angle_gamma 72.221(1) _cell_volume 2239.13(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10852 _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 colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.615 _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 0.5145 _exptl_absorpt_correction_T_max 0.6071 #----------------------------------------------------------------------------# # 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 -0.61578E-1 _diffrn_orient_matrix_ub_12 0.315163E-1 _diffrn_orient_matrix_ub_13 0.359176E-1 _diffrn_orient_matrix_ub_21 -0.558118E-1 _diffrn_orient_matrix_ub_22 0.543954E-1 _diffrn_orient_matrix_ub_23 -0.536056E-1 _diffrn_orient_matrix_ub_31 -0.460655E-1 _diffrn_orient_matrix_ub_32 -0.527782E-1 _diffrn_orient_matrix_ub_33 0.7805E-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 0.0595 _diffrn_reflns_av_unetI/netI 0.0557 _diffrn_reflns_number 17491 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 23.02 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 6150 _reflns_number_gt 4887 _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 ; Weak diffraction. Disorder in one piperidine ligand was modelled. 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^)+(0.0335P)^2^+5.8719P] 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 6150 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.114 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 Y1 Y 0.90482(4) 0.66905(3) 0.22240(3) 0.02083(15) Uani 1 1 d . A . Y2 Y 0.90844(4) 0.38626(3) 0.29945(3) 0.01963(14) Uani 1 1 d . . . O1 O 0.8356(3) 0.5471(3) 0.1878(2) 0.0258(8) Uani 1 1 d . . . O2 O 0.9786(3) 0.5083(2) 0.33397(19) 0.0220(7) Uani 1 1 d . . . N1 N 1.0695(4) 0.7198(3) 0.1731(3) 0.0312(10) Uani 1 1 d . . . N2 N 0.7354(3) 0.8070(3) 0.2231(2) 0.0245(9) Uani 1 1 d . . . N3 N 0.7310(4) 0.3521(3) 0.3385(3) 0.0259(10) Uani 1 1 d . . . N4 N 1.0773(4) 0.2398(3) 0.3114(2) 0.0226(9) Uani 1 1 d . . . C10 C 0.6753(5) 0.8989(5) 0.1428(3) 0.0407(15) Uani 1 1 d . A . C11 C 0.5342(5) 0.9142(7) 0.1239(4) 0.074(3) Uani 1 1 d . . . H11A H 0.496 0.978 0.0707 0.089 Uiso 1 1 calc R A . H11B H 0.5254 0.8482 0.1151 0.089 Uiso 1 1 calc R . . C12 C 0.4658(6) 0.9328(6) 0.2000(5) 0.066(2) Uani 1 1 d . A . H12A H 0.3747 0.9423 0.189 0.079 Uiso 1 1 calc R . . H12B H 0.4725 0.9999 0.208 0.079 Uiso 1 1 calc R . . C13 C 0.5313(6) 0.8274(6) 0.2853(5) 0.068(2) Uani 1 1 d . . . H13A H 0.4892 0.8378 0.3359 0.082 Uiso 1 1 calc R A . H13B H 0.5218 0.7608 0.2779 0.082 Uiso 1 1 calc R . . C14 C 0.6737(5) 0.8134(4) 0.3003(3) 0.0330(13) Uani 1 1 d . A . C15 C 0.6909(7) 1.0087(5) 0.1397(5) 0.072(2) Uani 1 1 d . . . H15A H 0.7812 0.9983 0.1519 0.108 Uiso 1 1 calc R A . H15B H 0.6439 1.0338 0.183 0.108 Uiso 1 1 calc R . . H15C H 0.6576 1.0637 0.0822 0.108 Uiso 1 1 calc R . . C16 C 0.7430(5) 0.8663(5) 0.0698(3) 0.0478(17) Uani 1 1 d . . . H16A H 0.8334 0.8572 0.0789 0.072 Uiso 1 1 calc R A . H16B H 0.7049 0.9239 0.0141 0.072 Uiso 1 1 calc R . . H16C H 0.7337 0.797 0.0699 0.072 Uiso 1 1 calc R . . C17 C 0.7374(8) 0.7032(6) 0.3693(5) 0.116(4) Uani 1 1 d . . . H17A H 0.7302 0.6448 0.3492 0.174 Uiso 1 1 calc R A . H17B H 0.6961 0.6996 0.4219 0.174 Uiso 1 1 calc R . . H17C H 0.8274 0.6936 0.3818 0.174 Uiso 1 1 calc R . . C18 C 0.6841(6) 0.9046(6) 0.3306(5) 0.072(2) Uani 1 1 d . . . H18A H 0.6415 0.9758 0.2857 0.108 Uiso 1 1 calc R A . H18B H 0.7739 0.896 0.3423 0.108 Uiso 1 1 calc R . . H18C H 0.6437 0.9009 0.3835 0.108 Uiso 1 1 calc R . . C19 C 0.6738(5) 0.2934(4) 0.2968(3) 0.0312(12) Uani 1 1 d . . . C20 C 0.6600(5) 0.1901(4) 0.3647(4) 0.0411(14) Uani 1 1 d . . . H20A H 0.6162 0.1547 0.3361 0.049 Uiso 1 1 calc R . . H20B H 0.7456 0.1372 0.3905 0.049 Uiso 1 1 calc R . . C21 C 0.5855(5) 0.2169(4) 0.4359(4) 0.0422(15) Uani 1 1 d . . . H21A H 0.5822 0.1484 0.4799 0.051 Uiso 1 1 calc R . . H21B H 0.4973 0.2644 0.4114 0.051 Uiso 1 1 calc R . . C22 C 0.6496(5) 0.2756(4) 0.4777(3) 0.0353(13) Uani 1 1 d . . . H22A H 0.7329 0.2237 0.509 0.042 Uiso 1 1 calc R . . H22B H 0.5967 0.2985 0.5204 0.042 Uiso 1 1 calc R . . C23 C 0.6701(4) 0.3770(4) 0.4121(3) 0.0284(12) Uani 1 1 d . . . C24 C 0.5429(5) 0.3622(5) 0.2422(4) 0.0479(16) Uani 1 1 d . . . H24A H 0.481 0.3859 0.2795 0.072 Uiso 1 1 calc R . . H24B H 0.5142 0.3174 0.2155 0.072 Uiso 1 1 calc R . . H24C H 0.5509 0.4268 0.197 0.072 Uiso 1 1 calc R . . C25 C 0.7655(5) 0.2593(5) 0.2348(4) 0.0430(15) Uani 1 1 d . . . H25A H 0.7746 0.3249 0.1917 0.064 Uiso 1 1 calc R . . H25B H 0.7319 0.2191 0.2058 0.064 Uiso 1 1 calc R . . H25C H 0.8486 0.212 0.2673 0.064 Uiso 1 1 calc R . . C26 C 0.7625(5) 0.4094(5) 0.4590(4) 0.0431(15) Uani 1 1 d . . . H26A H 0.7789 0.4738 0.4192 0.065 Uiso 1 1 calc R . . H26B H 0.8425 0.3482 0.4796 0.065 Uiso 1 1 calc R . . H26C H 0.7253 0.4269 0.5082 0.065 Uiso 1 1 calc R . . C27 C 0.5446(5) 0.4748(4) 0.3843(4) 0.0462(16) Uani 1 1 d . . . H27A H 0.4825 0.4571 0.354 0.069 Uiso 1 1 calc R . . H27B H 0.5607 0.5402 0.3459 0.069 Uiso 1 1 calc R . . H27C H 0.5111 0.4891 0.4355 0.069 Uiso 1 1 calc R . . C28 C 1.1201(4) 0.1438(4) 0.3917(3) 0.0270(12) Uani 1 1 d . . . C29 C 1.2636(5) 0.1130(4) 0.4207(3) 0.0355(13) Uani 1 1 d . . . H29A H 1.2781 0.1717 0.4383 0.043 Uiso 1 1 calc R . . H29B H 1.291 0.0442 0.4713 0.043 Uiso 1 1 calc R . . C30 C 1.3428(5) 0.0975(5) 0.3486(4) 0.0424(15) Uani 1 1 d . . . H30A H 1.3344 0.0349 0.3339 0.051 Uiso 1 1 calc R . . H30B H 1.4335 0.0814 0.3676 0.051 Uiso 1 1 calc R . . C31 C 1.2961(5) 0.2036(4) 0.2685(4) 0.0357(13) Uani 1 1 d . . . H31A H 1.3128 0.2641 0.2823 0.043 Uiso 1 1 calc R . . H31B H 1.3448 0.1923 0.2206 0.043 Uiso 1 1 calc R . . C32 C 1.1545(5) 0.2364(4) 0.2394(3) 0.0314(12) Uani 1 1 d . . . C33 C 1.0472(5) 0.1772(4) 0.4613(3) 0.0309(13) Uani 1 1 d . . . H33A H 0.9558 0.1971 0.4447 0.046 Uiso 1 1 calc R . . H33B H 1.0657 0.2403 0.4677 0.046 Uiso 1 1 calc R . . H33C H 1.0731 0.1157 0.5161 0.046 Uiso 1 1 calc R . . C34 C 1.0920(6) 0.0408(4) 0.3878(4) 0.0431(15) Uani 1 1 d . . . H34A H 1.1376 0.0164 0.3437 0.065 Uiso 1 1 calc R . . H34B H 1.0005 0.0588 0.3732 0.065 Uiso 1 1 calc R . . H34C H 1.1201 -0.0181 0.444 0.065 Uiso 1 1 calc R . . C35 C 1.1132(5) 0.3545(4) 0.1758(4) 0.0448(15) Uani 1 1 d . . . H35A H 1.1259 0.4032 0.2052 0.067 Uiso 1 1 calc R . . H35B H 1.0231 0.3776 0.154 0.067 Uiso 1 1 calc R . . H35C H 1.1641 0.3584 0.1275 0.067 Uiso 1 1 calc R . . C36 C 1.1336(6) 0.1635(5) 0.1913(4) 0.0489(16) Uani 1 1 d . . . H36A H 1.0426 0.1844 0.1728 0.073 Uiso 1 1 calc R . . H36B H 1.1649 0.0866 0.2295 0.073 Uiso 1 1 calc R . . H36C H 1.1798 0.1726 0.1406 0.073 Uiso 1 1 calc R . . C37 C 0.7160(5) 0.5793(5) 0.1359(4) 0.0440(15) Uani 1 1 d . . . H37A H 0.6664 0.6559 0.1293 0.053 Uiso 1 1 calc R . . H37B H 0.6665 0.5316 0.1654 0.053 Uiso 1 1 calc R . . C38 C 0.7356(6) 0.5705(5) 0.0508(4) 0.0539(17) Uani 1 1 d . . . H38A H 0.7912 0.4952 0.0581 0.065 Uiso 1 1 calc R . . H38B H 0.7801 0.622 0.0202 0.065 Uiso 1 1 calc R . . C39 C 0.6124(7) 0.5955(7) -0.0041(5) 0.081(2) Uani 1 1 d . . . H39A H 0.5651 0.5477 0.0286 0.097 Uiso 1 1 calc R . . H39B H 0.6332 0.5769 -0.0566 0.097 Uiso 1 1 calc R . . C40 C 0.5264(8) 0.7147(7) -0.0313(6) 0.100(3) Uani 1 1 d . . . H40A H 0.4485 0.724 -0.0654 0.149 Uiso 1 1 calc R . . H40B H 0.5707 0.7627 -0.0663 0.149 Uiso 1 1 calc R . . H40C H 0.5046 0.734 0.0201 0.149 Uiso 1 1 calc R . . C41 C 1.0731(4) 0.4795(4) 0.4033(3) 0.0253(11) Uani 1 1 d . . . H41A H 1.0588 0.4227 0.4539 0.03 Uiso 1 1 calc R . . H41B H 1.0656 0.5448 0.4195 0.03 Uiso 1 1 calc R . . C42 C 1.2040(5) 0.4371(4) 0.3808(4) 0.0357(13) Uani 1 1 d . . . H42A H 1.2664 0.4184 0.4303 0.053 Uiso 1 1 calc R . . H42B H 1.219 0.4936 0.3313 0.053 Uiso 1 1 calc R . . H42C H 1.2124 0.3714 0.366 0.053 Uiso 1 1 calc R . . C1 C 1.1248(5) 0.7052(4) 0.0950(4) 0.0348(13) Uani 0.563(9) 1 d P A 1 C2 C 1.1125(6) 0.8142(5) 0.0230(5) 0.064(2) Uani 0.563(9) 1 d P A 1 H2A H 1.0223 0.8578 0.0013 0.077 Uiso 0.563(9) 1 calc PR A 1 H2B H 1.1581 0.8015 -0.0257 0.077 Uiso 0.563(9) 1 calc PR A 1 C3 C 1.1808(11) 0.8769(8) 0.0731(8) 0.056(4) Uani 0.563(9) 1 d P A 1 H3A H 1.271 0.8318 0.0933 0.068 Uiso 0.563(9) 1 calc PR A 1 H3B H 1.1785 0.9488 0.0315 0.068 Uiso 0.563(9) 1 calc PR A 1 C4 C 1.1081(7) 0.8960(5) 0.1567(5) 0.065(2) Uani 0.563(9) 1 d P A 1 H4A H 1.1492 0.9328 0.1856 0.078 Uiso 0.563(9) 1 calc PR A 1 H4B H 1.0173 0.9403 0.1386 0.078 Uiso 0.563(9) 1 calc PR A 1 C5 C 1.1233(5) 0.7797(4) 0.2154(4) 0.0367(14) Uani 0.563(9) 1 d P A 1 C6 C 1.0471(6) 0.6510(5) 0.0590(4) 0.0466(15) Uani 0.563(9) 1 d P A 1 H6A H 0.9577 0.6975 0.0461 0.07 Uiso 0.563(9) 1 calc PR A 1 H6B H 1.0547 0.5792 0.1017 0.07 Uiso 0.563(9) 1 calc PR A 1 H6C H 1.0788 0.6413 0.006 0.07 Uiso 0.563(9) 1 calc PR A 1 C7 C 1.2640(6) 0.6319(6) 0.1146(5) 0.067(2) Uani 0.563(9) 1 d P A 1 H7A H 1.3149 0.6665 0.1376 0.101 Uiso 0.563(9) 1 calc PR A 1 H7B H 1.2951 0.622 0.0615 0.101 Uiso 0.563(9) 1 calc PR A 1 H7C H 1.2713 0.5603 0.1574 0.101 Uiso 0.563(9) 1 calc PR A 1 C8 C 1.2639(6) 0.7207(6) 0.2522(6) 0.075(2) Uani 0.563(9) 1 d P A 1 H8A H 1.3152 0.7148 0.205 0.112 Uiso 0.563(9) 1 calc PR A 1 H8B H 1.2743 0.647 0.2928 0.112 Uiso 0.563(9) 1 calc PR A 1 H8C H 1.2921 0.7626 0.2823 0.112 Uiso 0.563(9) 1 calc PR A 1 C9 C 1.0512(6) 0.7866(5) 0.2922(4) 0.0523(17) Uani 0.563(9) 1 d P A 1 H9A H 1.0596 0.7124 0.3309 0.078 Uiso 0.563(9) 1 calc PR A 1 H9B H 0.9612 0.8282 0.2718 0.078 Uiso 0.563(9) 1 calc PR A 1 H9C H 1.0864 0.8238 0.3233 0.078 Uiso 0.563(9) 1 calc PR A 1 C1A C 1.1248(5) 0.7052(4) 0.0950(4) 0.0348(13) Uani 0.437(9) 1 d P A 2 C2A C 1.1125(6) 0.8142(5) 0.0230(5) 0.064(2) Uani 0.437(9) 1 d P A 2 H2A1 H 1.1627 0.852 0.0425 0.096 Uiso 0.437(9) 1 calc PR A 2 H2A2 H 1.0231 0.8606 0.0092 0.096 Uiso 0.437(9) 1 calc PR A 2 H2A3 H 1.1439 0.7995 -0.0285 0.096 Uiso 0.437(9) 1 calc PR A 2 C3A C 1.3296(12) 0.7099(14) 0.1569(11) 0.068(6) Uani 0.437(9) 1 d P A 2 H3A1 H 1.312 0.7841 0.1135 0.082 Uiso 0.437(9) 1 calc PR A 2 H3A2 H 1.4229 0.6746 0.17 0.082 Uiso 0.437(9) 1 calc PR A 2 C4A C 1.1081(7) 0.8960(5) 0.1567(5) 0.065(2) Uani 0.437(9) 1 d P A 2 H4A1 H 1.1543 0.8934 0.1068 0.097 Uiso 0.437(9) 1 calc PR A 2 H4A2 H 1.1423 0.9328 0.1886 0.097 Uiso 0.437(9) 1 calc PR A 2 H4A3 H 1.0178 0.9366 0.1367 0.097 Uiso 0.437(9) 1 calc PR A 2 C5A C 1.1233(5) 0.7797(4) 0.2154(4) 0.0367(14) Uani 0.437(9) 1 d P A 2 C6A C 1.0471(6) 0.6510(5) 0.0590(4) 0.0466(15) Uani 0.437(9) 1 d P A 2 H6A1 H 0.9578 0.6977 0.0457 0.07 Uiso 0.437(9) 1 calc PR A 2 H6A2 H 1.0542 0.5795 0.1018 0.07 Uiso 0.437(9) 1 calc PR A 2 H6A3 H 1.0793 0.6408 0.0062 0.07 Uiso 0.437(9) 1 calc PR A 2 C7A C 1.2640(6) 0.6319(6) 0.1146(5) 0.067(2) Uani 0.437(9) 1 d P A 2 H7A1 H 1.3004 0.6237 0.0618 0.081 Uiso 0.437(9) 1 calc PR A 2 H7A2 H 1.2752 0.5585 0.1576 0.081 Uiso 0.437(9) 1 calc PR A 2 C8A C 1.2639(6) 0.7207(6) 0.2522(6) 0.075(2) Uani 0.437(9) 1 d P A 2 H8A1 H 1.2773 0.6477 0.2964 0.09 Uiso 0.437(9) 1 calc PR A 2 H8A2 H 1.2988 0.765 0.2768 0.09 Uiso 0.437(9) 1 calc PR A 2 C9A C 1.0512(6) 0.7866(5) 0.2922(4) 0.0523(17) Uani 0.437(9) 1 d P A 2 H9A1 H 1.0584 0.7125 0.3304 0.078 Uiso 0.437(9) 1 calc PR A 2 H9A2 H 0.9615 0.8292 0.2718 0.078 Uiso 0.437(9) 1 calc PR A 2 H9A3 H 1.0872 0.8227 0.3239 0.078 Uiso 0.437(9) 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 Y1 0.0165(3) 0.0137(3) 0.0289(3) -0.0034(2) 0.0030(2) -0.0044(2) Y2 0.0167(3) 0.0140(3) 0.0268(3) -0.0048(2) 0.0036(2) -0.0055(2) O1 0.0207(17) 0.0213(18) 0.031(2) -0.0038(15) -0.0048(15) -0.0067(14) O2 0.0209(17) 0.0194(18) 0.0237(18) -0.0050(14) 0.0037(15) -0.0065(14) N1 0.027(2) 0.031(3) 0.045(3) -0.017(2) 0.013(2) -0.018(2) N2 0.021(2) 0.024(2) 0.023(2) -0.0071(18) 0.0013(18) -0.0003(18) N3 0.021(2) 0.022(2) 0.031(2) -0.0035(19) 0.0025(19) -0.0086(18) N4 0.027(2) 0.014(2) 0.026(2) -0.0056(18) 0.0089(19) -0.0067(17) C10 0.029(3) 0.046(4) 0.026(3) -0.008(3) 0.000(2) 0.012(3) C11 0.027(3) 0.115(7) 0.036(4) -0.012(4) -0.005(3) 0.023(4) C12 0.045(4) 0.066(5) 0.081(5) -0.032(4) 0.004(4) -0.005(4) C13 0.047(4) 0.069(5) 0.117(6) -0.059(5) 0.044(4) -0.028(4) C14 0.036(3) 0.019(3) 0.033(3) -0.003(2) 0.007(3) 0.000(2) C15 0.100(6) 0.023(4) 0.062(5) -0.003(3) 0.020(4) 0.009(4) C16 0.030(3) 0.063(4) 0.027(3) -0.009(3) 0.001(3) 0.009(3) C17 0.124(7) 0.075(6) 0.051(5) 0.030(4) 0.053(5) 0.050(5) C18 0.045(4) 0.088(6) 0.109(6) -0.078(5) 0.014(4) -0.010(4) C19 0.025(3) 0.034(3) 0.036(3) -0.008(2) 0.000(2) -0.016(2) C20 0.035(3) 0.034(3) 0.061(4) -0.016(3) 0.006(3) -0.021(3) C21 0.037(3) 0.026(3) 0.057(4) -0.003(3) 0.012(3) -0.014(3) C22 0.033(3) 0.035(3) 0.034(3) -0.009(3) 0.012(3) -0.011(3) C23 0.024(3) 0.022(3) 0.039(3) -0.009(2) 0.014(2) -0.008(2) C24 0.030(3) 0.067(4) 0.049(4) -0.012(3) 0.000(3) -0.027(3) C25 0.035(3) 0.062(4) 0.046(4) -0.028(3) 0.006(3) -0.023(3) C26 0.038(3) 0.049(4) 0.055(4) -0.032(3) 0.023(3) -0.016(3) C27 0.025(3) 0.034(3) 0.079(5) -0.021(3) 0.018(3) -0.006(3) C28 0.027(3) 0.017(3) 0.031(3) -0.001(2) 0.004(2) -0.006(2) C29 0.027(3) 0.027(3) 0.043(3) -0.004(3) 0.004(3) -0.004(2) C30 0.026(3) 0.035(3) 0.064(4) -0.019(3) 0.014(3) -0.004(3) C31 0.033(3) 0.035(3) 0.049(4) -0.024(3) 0.023(3) -0.015(3) C32 0.036(3) 0.026(3) 0.031(3) -0.008(2) 0.011(2) -0.008(2) C33 0.029(3) 0.024(3) 0.030(3) -0.001(2) 0.011(2) -0.004(2) C34 0.049(4) 0.024(3) 0.055(4) -0.006(3) 0.011(3) -0.018(3) C35 0.047(4) 0.038(3) 0.037(3) -0.007(3) 0.019(3) -0.005(3) C36 0.046(4) 0.055(4) 0.050(4) -0.029(3) 0.010(3) -0.010(3) C37 0.043(3) 0.045(4) 0.039(4) -0.006(3) -0.001(3) -0.017(3) C38 0.058(4) 0.051(4) 0.051(4) -0.023(3) -0.004(3) -0.008(3) C39 0.084(6) 0.078(6) 0.078(6) -0.028(5) -0.006(5) -0.023(5) C40 0.097(7) 0.078(6) 0.090(7) -0.023(5) -0.010(5) 0.011(5) C41 0.025(3) 0.025(3) 0.026(3) -0.009(2) -0.002(2) -0.008(2) C42 0.025(3) 0.039(3) 0.043(3) -0.015(3) 0.000(3) -0.009(2) C1 0.028(3) 0.026(3) 0.050(4) -0.010(3) 0.015(3) -0.010(2) C2 0.063(4) 0.040(4) 0.077(5) -0.003(4) 0.041(4) -0.016(3) C3 0.056(7) 0.030(6) 0.081(9) -0.003(6) 0.028(7) -0.028(6) C4 0.066(4) 0.042(4) 0.085(5) -0.003(4) 0.002(4) -0.036(4) C5 0.025(3) 0.035(3) 0.053(4) -0.013(3) 0.004(3) -0.015(2) C6 0.053(4) 0.046(4) 0.049(4) -0.018(3) 0.025(3) -0.025(3) C7 0.032(3) 0.079(5) 0.076(5) -0.020(4) 0.024(3) -0.005(3) C8 0.031(3) 0.055(4) 0.143(8) -0.036(5) -0.005(4) -0.019(3) C9 0.055(4) 0.065(5) 0.060(4) -0.034(4) 0.007(3) -0.038(4) C1A 0.028(3) 0.026(3) 0.050(4) -0.010(3) 0.015(3) -0.010(2) C2A 0.063(4) 0.040(4) 0.077(5) -0.003(4) 0.041(4) -0.016(3) C3A 0.014(7) 0.085(12) 0.096(14) -0.016(10) 0.004(8) -0.018(7) C4A 0.066(4) 0.042(4) 0.085(5) -0.003(4) 0.002(4) -0.036(4) C5A 0.025(3) 0.035(3) 0.053(4) -0.013(3) 0.004(3) -0.015(2) C6A 0.053(4) 0.046(4) 0.049(4) -0.018(3) 0.025(3) -0.025(3) C7A 0.032(3) 0.079(5) 0.076(5) -0.020(4) 0.024(3) -0.005(3) C8A 0.031(3) 0.055(4) 0.143(8) -0.036(5) -0.005(4) -0.019(3) C9A 0.055(4) 0.065(5) 0.060(4) -0.034(4) 0.007(3) -0.038(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 Y1 N1 2.223(4) . ? Y1 N2 2.223(4) . ? Y1 O1 2.252(3) . ? Y1 O2 2.262(3) . ? Y2 N3 2.220(4) . ? Y2 N4 2.236(4) . ? Y2 O2 2.259(3) . ? Y2 O1 2.262(3) . ? O1 C37 1.442(6) . ? O2 C41 1.415(5) . ? N1 C5 1.474(7) . ? N1 C1 1.480(7) . ? N2 C14 1.468(6) . ? N2 C10 1.472(6) . ? N3 C19 1.476(6) . ? N3 C23 1.483(6) . ? N4 C28 1.476(6) . ? N4 C32 1.478(6) . ? C10 C11 1.535(8) . ? C10 C16 1.543(7) . ? C10 C15 1.543(9) . ? C11 C12 1.526(9) . ? C12 C13 1.613(10) . ? C13 C14 1.545(8) . ? C14 C17 1.510(8) . ? C14 C18 1.517(8) . ? C19 C25 1.532(7) . ? C19 C20 1.540(7) . ? C19 C24 1.551(7) . ? C20 C21 1.523(8) . ? C21 C22 1.524(8) . ? C22 C23 1.536(7) . ? C23 C26 1.527(7) . ? C23 C27 1.546(7) . ? C28 C33 1.522(7) . ? C28 C34 1.549(7) . ? C28 C29 1.551(7) . ? C29 C30 1.519(7) . ? C30 C31 1.547(8) . ? C31 C32 1.527(7) . ? C32 C36 1.524(7) . ? C32 C35 1.531(7) . ? C37 C38 1.461(8) . ? C38 C39 1.520(9) . ? C39 C40 1.525(10) . ? C41 C42 1.495(7) . ? C1 C6 1.521(8) . ? C1 C7 1.530(8) . ? C1 C2 1.537(8) . ? C2 C3 1.685(13) . ? C3 C4 1.658(13) . ? C4 C5 1.520(8) . ? C5 C9 1.521(8) . ? C5 C8 1.537(8) . ? 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 Y1 N2 114.18(15) . . ? N1 Y1 O1 125.06(14) . . ? N2 Y1 O1 107.79(13) . . ? N1 Y1 O2 108.48(14) . . ? N2 Y1 O2 123.32(12) . . ? O1 Y1 O2 73.04(11) . . ? N3 Y2 N4 116.00(14) . . ? N3 Y2 O2 123.92(13) . . ? N4 Y2 O2 107.68(12) . . ? N3 Y2 O1 102.75(13) . . ? N4 Y2 O1 128.34(12) . . ? O2 Y2 O1 72.90(11) . . ? C37 O1 Y1 122.1(3) . . ? C37 O1 Y2 121.7(3) . . ? Y1 O1 Y2 107.14(13) . . ? C41 O2 Y2 124.2(3) . . ? C41 O2 Y1 127.5(3) . . ? Y2 O2 Y1 106.92(13) . . ? C5 N1 C1 116.1(4) . . ? C5 N1 Y1 119.5(3) . . ? C1 N1 Y1 124.2(3) . . ? C14 N2 C10 115.2(4) . . ? C14 N2 Y1 124.2(3) . . ? C10 N2 Y1 120.6(3) . . ? C19 N3 C23 116.2(4) . . ? C19 N3 Y2 121.0(3) . . ? C23 N3 Y2 122.6(3) . . ? C28 N4 C32 116.6(4) . . ? C28 N4 Y2 122.2(3) . . ? C32 N4 Y2 121.2(3) . . ? N2 C10 C11 111.9(5) . . ? N2 C10 C16 105.8(4) . . ? C11 C10 C16 107.0(5) . . ? N2 C10 C15 114.0(5) . . ? C11 C10 C15 109.9(5) . . ? C16 C10 C15 107.8(5) . . ? C12 C11 C10 109.1(5) . . ? C11 C12 C13 108.2(5) . . ? C14 C13 C12 109.1(5) . . ? N2 C14 C17 105.1(4) . . ? N2 C14 C18 115.0(5) . . ? C17 C14 C18 110.0(6) . . ? N2 C14 C13 110.7(5) . . ? C17 C14 C13 107.8(6) . . ? C18 C14 C13 108.0(5) . . ? N3 C19 C25 106.4(4) . . ? N3 C19 C20 110.4(4) . . ? C25 C19 C20 109.3(5) . . ? N3 C19 C24 115.4(4) . . ? C25 C19 C24 106.7(5) . . ? C20 C19 C24 108.4(4) . . ? C21 C20 C19 111.9(4) . . ? C20 C21 C22 109.4(4) . . ? C21 C22 C23 113.0(4) . . ? N3 C23 C26 107.0(4) . . ? N3 C23 C22 111.8(4) . . ? C26 C23 C22 106.7(4) . . ? N3 C23 C27 113.4(4) . . ? C26 C23 C27 107.0(4) . . ? C22 C23 C27 110.5(4) . . ? N4 C28 C33 106.6(4) . . ? N4 C28 C34 114.6(4) . . ? C33 C28 C34 106.9(4) . . ? N4 C28 C29 111.4(4) . . ? C33 C28 C29 107.6(4) . . ? C34 C28 C29 109.3(4) . . ? C30 C29 C28 111.4(4) . . ? C29 C30 C31 109.1(4) . . ? C32 C31 C30 112.2(4) . . ? N4 C32 C36 114.5(4) . . ? N4 C32 C31 112.0(4) . . ? C36 C32 C31 109.5(4) . . ? N4 C32 C35 105.5(4) . . ? C36 C32 C35 107.8(5) . . ? C31 C32 C35 107.1(4) . . ? O1 C37 C38 110.9(5) . . ? C37 C38 C39 113.0(6) . . ? C38 C39 C40 114.3(7) . . ? O2 C41 C42 112.0(4) . . ? N1 C1 C6 106.4(4) . . ? N1 C1 C7 112.5(5) . . ? C6 C1 C7 108.9(5) . . ? N1 C1 C2 113.3(5) . . ? C6 C1 C2 106.1(5) . . ? C7 C1 C2 109.2(5) . . ? C1 C2 C3 102.7(6) . . ? C4 C3 C2 112.0(6) . . ? C5 C4 C3 103.1(6) . . ? N1 C5 C4 112.9(5) . . ? N1 C5 C9 107.0(4) . . ? C4 C5 C9 108.1(5) . . ? N1 C5 C8 113.7(5) . . ? C4 C5 C8 108.6(5) . . ? C9 C5 C8 106.1(5) . . ? #===END data_(4)-nov103 _database_code_depnum_ccdc_archive 'CCDC 239406' _audit_creation_date 2003-10-31T16:49:23-00:00 _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 'C40 H82 N4 O2 Y2' _chemical_formula_sum 'C40 H82 N4 O2 Y2' _chemical_formula_weight 828.92 _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 8.2061(1) _cell_length_b 10.8889(2) _cell_length_c 13.1412(2) _cell_angle_alpha 87.678(1) _cell_angle_beta 72.188(1) _cell_angle_gamma 74.273(1) _cell_volume 1074.95(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10868 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 444 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.721 _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 0.4166 _exptl_absorpt_correction_T_max 0.5815 #----------------------------------------------------------------------------# # 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 0.357232E-1 _diffrn_orient_matrix_ub_12 -0.78832E-1 _diffrn_orient_matrix_ub_13 0.386435E-1 _diffrn_orient_matrix_ub_21 -0.855524E-1 _diffrn_orient_matrix_ub_22 -0.366428E-1 _diffrn_orient_matrix_ub_23 -0.204296E-1 _diffrn_orient_matrix_ub_31 0.953713E-1 _diffrn_orient_matrix_ub_32 -0.395616E-1 _diffrn_orient_matrix_ub_33 -0.670186E-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 0.0455 _diffrn_reflns_av_unetI/netI 0.0364 _diffrn_reflns_number 18107 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 28.24 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.954 _diffrn_measured_fraction_theta_max 0.954 _reflns_number_total 5068 _reflns_number_gt 4619 _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^)+(0.0416P)^2^+0.6186P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.012(2) _refine_ls_number_reflns 5068 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.631 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 0.57377(2) 0.529120(16) 0.858639(14) 0.01691(8) Uani 1 1 d . . . O O 0.61901(19) 0.55359(13) 1.01759(11) 0.0197(3) Uani 1 1 d . . . N1 N 0.4841(2) 0.72366(16) 0.80160(14) 0.0212(4) Uani 1 1 d . . . N2 N 0.7475(2) 0.37790(16) 0.73271(13) 0.0194(3) Uani 1 1 d . . . C1 C 0.2995(3) 0.7881(2) 0.80398(17) 0.0243(4) Uani 1 1 d . . . C2 C 0.2901(3) 0.8230(2) 0.69014(18) 0.0295(5) Uani 1 1 d . . . H2A H 0.3133 0.7436 0.6477 0.035 Uiso 1 1 calc R . . H2B H 0.1684 0.8755 0.6953 0.035 Uiso 1 1 calc R . . C3 C 0.4224(4) 0.8959(2) 0.63233(19) 0.0352(6) Uani 1 1 d . . . H3A H 0.3915 0.9802 0.6694 0.042 Uiso 1 1 calc R . . H3B H 0.4177 0.9101 0.5583 0.042 Uiso 1 1 calc R . . C4 C 0.6096(3) 0.8197(2) 0.63020(18) 0.0318(5) Uani 1 1 d . . . H4A H 0.6945 0.8699 0.596 0.038 Uiso 1 1 calc R . . H4B H 0.6443 0.7395 0.5864 0.038 Uiso 1 1 calc R . . C5 C 0.6212(3) 0.7873(2) 0.74367(17) 0.0258(4) Uani 1 1 d . . . C6 C 0.2102(4) 0.9064(2) 0.8816(2) 0.0350(5) Uani 1 1 d . . . H6A H 0.2759 0.9708 0.8591 0.053 Uiso 1 1 calc R . . H6B H 0.2105 0.8818 0.9541 0.053 Uiso 1 1 calc R . . H6C H 0.0873 0.942 0.8809 0.053 Uiso 1 1 calc R . . C7 C 0.1906(3) 0.6923(2) 0.84391(18) 0.0284(5) Uani 1 1 d . . . H7A H 0.1941 0.6684 0.9161 0.043 Uiso 1 1 calc R . . H7B H 0.2409 0.616 0.7956 0.043 Uiso 1 1 calc R . . H7C H 0.0672 0.7311 0.8456 0.043 Uiso 1 1 calc R . . C8 C 0.6188(4) 0.9096(2) 0.8006(2) 0.0377(6) Uani 1 1 d . . . H8A H 0.5053 0.9739 0.8089 0.057 Uiso 1 1 calc R . . H8B H 0.7166 0.9431 0.7578 0.057 Uiso 1 1 calc R . . H8C H 0.633 0.8892 0.8713 0.057 Uiso 1 1 calc R . . C9 C 0.8011(3) 0.6924(2) 0.7335(2) 0.0332(5) Uani 1 1 d . . . H9A H 0.8103 0.6705 0.805 0.05 Uiso 1 1 calc R . . H9B H 0.8966 0.7307 0.6953 0.05 Uiso 1 1 calc R . . H9C H 0.812 0.6148 0.6938 0.05 Uiso 1 1 calc R . . C10 C 0.9119(3) 0.2922(2) 0.74714(17) 0.0236(4) Uani 1 1 d . . . C11 C 0.9277(3) 0.1513(2) 0.72587(18) 0.0302(5) Uani 1 1 d . . . H11A H 1.0458 0.0987 0.7277 0.036 Uiso 1 1 calc R . . H11B H 0.8362 0.1241 0.7836 0.036 Uiso 1 1 calc R . . C12 C 0.9045(4) 0.1267(2) 0.61835(19) 0.0343(5) Uani 1 1 d . . . H12A H 1.0032 0.1443 0.5594 0.041 Uiso 1 1 calc R . . H12B H 0.9068 0.0362 0.6103 0.041 Uiso 1 1 calc R . . C13 C 0.7283(3) 0.2131(2) 0.61311(18) 0.0301(5) Uani 1 1 d . . . H13A H 0.6304 0.1876 0.6669 0.036 Uiso 1 1 calc R . . H13B H 0.7168 0.201 0.5416 0.036 Uiso 1 1 calc R . . C14 C 0.7083(3) 0.3553(2) 0.63350(16) 0.0237(4) Uani 1 1 d . . . C15 C 1.0853(3) 0.3245(2) 0.6808(2) 0.0348(5) Uani 1 1 d . . . H15A H 1.1002 0.3151 0.6044 0.052 Uiso 1 1 calc R . . H15B H 1.187 0.2661 0.6974 0.052 Uiso 1 1 calc R . . H15C H 1.0786 0.4126 0.6986 0.052 Uiso 1 1 calc R . . C16 C 0.8979(3) 0.3087(2) 0.86459(18) 0.0301(5) Uani 1 1 d . . . H16A H 0.8872 0.398 0.8811 0.045 Uiso 1 1 calc R . . H16B H 1.0047 0.2537 0.8781 0.045 Uiso 1 1 calc R . . H16C H 0.7927 0.2849 0.9099 0.045 Uiso 1 1 calc R . . C17 C 0.8216(3) 0.4059(2) 0.53222(17) 0.0325(5) Uani 1 1 d . . . H17A H 0.9475 0.3609 0.519 0.049 Uiso 1 1 calc R . . H17B H 0.8043 0.4976 0.5431 0.049 Uiso 1 1 calc R . . H17C H 0.7847 0.3911 0.4706 0.049 Uiso 1 1 calc R . . C18 C 0.5148(3) 0.4293(2) 0.64916(19) 0.0304(5) Uani 1 1 d . . . H18A H 0.4996 0.5202 0.6624 0.046 Uiso 1 1 calc R . . H18B H 0.4372 0.3972 0.7105 0.046 Uiso 1 1 calc R . . H18C H 0.4834 0.4178 0.5847 0.046 Uiso 1 1 calc R . . C19 C 0.7290(3) 0.6236(2) 1.04035(18) 0.0266(5) Uani 1 1 d . . . H19A H 0.8294 0.6235 0.9751 0.032 Uiso 1 1 calc R . . H19B H 0.779 0.5812 1.0965 0.032 Uiso 1 1 calc R . . C20 C 0.6263(4) 0.7589(2) 1.0774(2) 0.0392(6) Uani 1 1 d . . . H20A H 0.7051 0.8042 1.0924 0.059 Uiso 1 1 calc R . . H20B H 0.528 0.7592 1.1426 0.059 Uiso 1 1 calc R . . H20C H 0.5786 0.8015 1.0214 0.059 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 Y 0.02240(12) 0.01524(11) 0.01405(11) 0.00168(6) -0.00553(7) -0.00688(7) O 0.0249(7) 0.0201(7) 0.0179(7) 0.0011(5) -0.0076(6) -0.0111(6) N1 0.0266(9) 0.0174(8) 0.0208(8) 0.0046(6) -0.0078(7) -0.0081(7) N2 0.0240(9) 0.0177(8) 0.0167(8) 0.0001(6) -0.0063(7) -0.0055(7) C1 0.0310(11) 0.0197(10) 0.0215(10) 0.0032(8) -0.0092(9) -0.0050(9) C2 0.0391(13) 0.0264(11) 0.0259(11) 0.0065(9) -0.0162(10) -0.0074(10) C3 0.0562(16) 0.0285(12) 0.0261(11) 0.0102(9) -0.0175(11) -0.0156(11) C4 0.0447(14) 0.0314(12) 0.0226(11) 0.0066(9) -0.0080(10) -0.0191(11) C5 0.0359(12) 0.0207(10) 0.0237(10) 0.0043(8) -0.0084(9) -0.0139(9) C6 0.0423(14) 0.0258(12) 0.0304(12) -0.0020(9) -0.0084(11) -0.0011(10) C7 0.0277(11) 0.0316(12) 0.0268(11) 0.0054(9) -0.0095(9) -0.0085(9) C8 0.0591(17) 0.0282(12) 0.0341(13) 0.0036(10) -0.0151(12) -0.0248(12) C9 0.0341(13) 0.0340(13) 0.0366(13) 0.0079(10) -0.0096(10) -0.0197(11) C10 0.0247(11) 0.0212(10) 0.0219(10) -0.0010(8) -0.0057(8) -0.0027(8) C11 0.0373(13) 0.0210(10) 0.0277(11) -0.0013(8) -0.0089(10) -0.0014(9) C12 0.0479(15) 0.0222(11) 0.0287(12) -0.0066(9) -0.0061(11) -0.0080(10) C13 0.0450(14) 0.0276(11) 0.0221(10) -0.0015(8) -0.0110(10) -0.0158(10) C14 0.0328(12) 0.0241(10) 0.0168(9) 0.0016(8) -0.0087(8) -0.0108(9) C15 0.0268(12) 0.0385(13) 0.0371(13) -0.0004(10) -0.0065(10) -0.0087(10) C16 0.0313(12) 0.0315(12) 0.0265(11) -0.0038(9) -0.0146(10) 0.0002(10) C17 0.0441(14) 0.0351(12) 0.0180(10) 0.0045(9) -0.0068(10) -0.0140(11) C18 0.0354(13) 0.0329(12) 0.0276(11) 0.0030(9) -0.0149(10) -0.0110(10) C19 0.0306(12) 0.0296(11) 0.0265(11) 0.0021(9) -0.0101(9) -0.0180(9) C20 0.0586(17) 0.0256(12) 0.0419(14) 0.0002(10) -0.0207(13) -0.0191(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y N1 2.2258(16) . ? Y N2 2.2332(16) . ? Y O 2.2447(14) 2_667 ? Y O 2.2683(14) . ? O C19 1.429(2) . ? O Y 2.2447(14) 2_667 ? N1 C5 1.477(3) . ? N1 C1 1.478(3) . ? N2 C10 1.479(3) . ? N2 C14 1.479(3) . ? C1 C7 1.529(3) . ? C1 C6 1.541(3) . ? C1 C2 1.548(3) . ? C2 C3 1.516(3) . ? C3 C4 1.527(4) . ? C4 C5 1.544(3) . ? C5 C9 1.526(3) . ? C5 C8 1.546(3) . ? C10 C16 1.526(3) . ? C10 C11 1.535(3) . ? C10 C15 1.548(3) . ? C11 C12 1.525(3) . ? C12 C13 1.516(4) . ? C13 C14 1.538(3) . ? C14 C18 1.527(3) . ? C14 C17 1.549(3) . ? C19 C20 1.500(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 N1 Y N2 116.22(6) . . ? N1 Y O 120.40(6) . 2_667 ? N2 Y O 109.14(6) . 2_667 ? N1 Y O 107.26(6) . . ? N2 Y O 124.42(6) . . ? O Y O 73.09(6) 2_667 . ? C19 O Y 124.82(12) . 2_667 ? C19 O Y 127.72(12) . . ? Y O Y 106.91(6) 2_667 . ? C5 N1 C1 116.35(16) . . ? C5 N1 Y 118.06(13) . . ? C1 N1 Y 125.06(13) . . ? C10 N2 C14 116.31(16) . . ? C10 N2 Y 119.64(12) . . ? C14 N2 Y 124.05(13) . . ? N1 C1 C7 106.92(16) . . ? N1 C1 C6 114.09(18) . . ? C7 C1 C6 106.55(19) . . ? N1 C1 C2 110.92(18) . . ? C7 C1 C2 107.56(18) . . ? C6 C1 C2 110.44(18) . . ? C3 C2 C1 112.80(19) . . ? C2 C3 C4 109.56(19) . . ? C3 C4 C5 111.90(19) . . ? N1 C5 C9 106.63(17) . . ? N1 C5 C4 111.02(18) . . ? C9 C5 C4 108.52(19) . . ? N1 C5 C8 115.27(19) . . ? C9 C5 C8 106.4(2) . . ? C4 C5 C8 108.67(18) . . ? N2 C10 C16 106.42(16) . . ? N2 C10 C11 111.99(18) . . ? C16 C10 C11 107.24(18) . . ? N2 C10 C15 114.64(18) . . ? C16 C10 C15 106.49(19) . . ? C11 C10 C15 109.61(18) . . ? C12 C11 C10 112.65(18) . . ? C13 C12 C11 109.00(18) . . ? C12 C13 C14 113.15(19) . . ? N2 C14 C18 106.68(17) . . ? N2 C14 C13 111.84(17) . . ? C18 C14 C13 108.38(19) . . ? N2 C14 C17 114.10(18) . . ? C18 C14 C17 106.58(18) . . ? C13 C14 C17 108.96(18) . . ? O C19 C20 111.45(19) . . ? #===END data_(1)-sep103 _database_code_depnum_ccdc_archive 'CCDC 239407' _audit_creation_date 2003-09-25T13:52:10-00:00 _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 'C27 H54 N3 Y1' _chemical_formula_sum 'C27 H54 N3 Y' _chemical_formula_weight 509.64 _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 7.7300(1) _cell_length_b 18.2895(2) _cell_length_c 19.8672(3) _cell_angle_alpha 90 _cell_angle_beta 93.598(1) _cell_angle_gamma 90 _cell_volume 2803.25(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18525 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.098 _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 0.506 _exptl_absorpt_correction_T_max 0.6168 #----------------------------------------------------------------------------# # 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 0.682623E-1 _diffrn_orient_matrix_ub_12 -0.257789E-1 _diffrn_orient_matrix_ub_13 -0.339378E-1 _diffrn_orient_matrix_ub_21 -0.547924E-1 _diffrn_orient_matrix_ub_22 0.315318E-1 _diffrn_orient_matrix_ub_23 -0.365264E-1 _diffrn_orient_matrix_ub_31 0.956024E-1 _diffrn_orient_matrix_ub_32 0.364785E-1 _diffrn_orient_matrix_ub_33 0.75897E-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 0.0581 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_number 29190 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 4901 _reflns_number_gt 4215 _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^)+(0.0899P)^2^+20.8834P] 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 4901 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 0.76 _refine_ls_restrained_S_all 0.76 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.538 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.068 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 0.97877(7) 0.76139(2) 0.20756(2) 0.03271(17) Uani 1 1 d . . . N1 N 1.0116(4) 0.86637(17) 0.15494(16) 0.0193(7) Uani 1 1 d . . . N2 N 0.9598(4) 0.65768(17) 0.15084(16) 0.0207(7) Uani 1 1 d . . . N3 N 0.9782(4) 0.76101(18) 0.31862(16) 0.0210(7) Uani 1 1 d . . . C1 C 1.1508(5) 0.9176(2) 0.1752(2) 0.0232(9) Uani 1 1 d . . . C2 C 1.0762(6) 0.9901(2) 0.1993(2) 0.0298(10) Uani 1 1 d . . . H2A H 1.0191 0.9817 0.2419 0.036 Uiso 1 1 calc R . . H2B H 1.1719 1.0253 0.2087 0.036 Uiso 1 1 calc R . . C3 C 0.9457(6) 1.0224(2) 0.1472(2) 0.0321(10) Uani 1 1 d . . . H3A H 1.0053 1.0364 0.1064 0.038 Uiso 1 1 calc R . . H3B H 0.8937 1.067 0.1657 0.038 Uiso 1 1 calc R . . C4 C 0.8024(6) 0.9666(2) 0.1281(2) 0.0287(9) Uani 1 1 d . . . H4A H 0.7319 0.9586 0.1673 0.034 Uiso 1 1 calc R . . H4B H 0.7254 0.9868 0.0909 0.034 Uiso 1 1 calc R . . C5 C 0.8763(5) 0.8932(2) 0.1059(2) 0.0222(8) Uani 1 1 d . . . C6 C 1.2812(6) 0.9329(3) 0.1206(3) 0.0364(11) Uani 1 1 d . . . H6A H 1.2204 0.9559 0.0813 0.055 Uiso 1 1 calc R . . H6B H 1.3331 0.8868 0.1069 0.055 Uiso 1 1 calc R . . H6C H 1.3724 0.9658 0.1391 0.055 Uiso 1 1 calc R . . C7 C 1.2568(6) 0.8822(3) 0.2346(3) 0.0364(11) Uani 1 1 d . . . H7A H 1.3055 0.8357 0.2199 0.055 Uiso 1 1 calc R . . H7B H 1.1815 0.8731 0.2716 0.055 Uiso 1 1 calc R . . H7C H 1.3512 0.915 0.2501 0.055 Uiso 1 1 calc R . . C8 C 0.7299(5) 0.8364(2) 0.1041(2) 0.0289(10) Uani 1 1 d . . . H8A H 0.7745 0.789 0.0902 0.043 Uiso 1 1 calc R . . H8B H 0.6359 0.8521 0.072 0.043 Uiso 1 1 calc R . . H8C H 0.6858 0.832 0.1491 0.043 Uiso 1 1 calc R . . C9 C 0.9328(6) 0.8986(3) 0.0331(2) 0.0327(10) Uani 1 1 d . . . H9A H 0.9803 0.8516 0.0196 0.049 Uiso 1 1 calc R . . H9B H 1.0217 0.9366 0.0307 0.049 Uiso 1 1 calc R . . H9C H 0.8325 0.9113 0.0027 0.049 Uiso 1 1 calc R . . C10 C 1.0862(5) 0.6377(2) 0.1015(2) 0.0226(8) Uani 1 1 d . . . C11 C 0.9974(6) 0.6272(3) 0.0308(2) 0.0317(10) Uani 1 1 d . . . H11A H 0.9556 0.675 0.0131 0.038 Uiso 1 1 calc R . . H11B H 1.0828 0.6081 0.0001 0.038 Uiso 1 1 calc R . . C12 C 0.8441(6) 0.5739(3) 0.0320(2) 0.0371(11) Uani 1 1 d . . . H12A H 0.7841 0.5714 -0.0135 0.045 Uiso 1 1 calc R . . H12B H 0.8875 0.5244 0.044 0.045 Uiso 1 1 calc R . . C13 C 0.7170(6) 0.5985(3) 0.0828(2) 0.0312(10) Uani 1 1 d . . . H13A H 0.6249 0.5612 0.0856 0.037 Uiso 1 1 calc R . . H13B H 0.6615 0.6448 0.0672 0.037 Uiso 1 1 calc R . . C14 C 0.8078(5) 0.6102(2) 0.1537(2) 0.0228(9) Uani 1 1 d . . . C15 C 1.2140(6) 0.7014(2) 0.0992(2) 0.0315(10) Uani 1 1 d . . . H15A H 1.272 0.7085 0.1441 0.047 Uiso 1 1 calc R . . H15B H 1.1513 0.746 0.0855 0.047 Uiso 1 1 calc R . . H15C H 1.3007 0.6904 0.0667 0.047 Uiso 1 1 calc R . . C16 C 1.1971(6) 0.5691(2) 0.1211(2) 0.0319(10) Uani 1 1 d . . . H16A H 1.1212 0.5264 0.1234 0.048 Uiso 1 1 calc R . . H16B H 1.2586 0.577 0.1651 0.048 Uiso 1 1 calc R . . H16C H 1.2813 0.5607 0.087 0.048 Uiso 1 1 calc R . . C17 C 0.6801(5) 0.6508(2) 0.1967(2) 0.0297(10) Uani 1 1 d . . . H17A H 0.6532 0.6987 0.1767 0.045 Uiso 1 1 calc R . . H17B H 0.7325 0.6573 0.2425 0.045 Uiso 1 1 calc R . . H17C H 0.5733 0.6222 0.1984 0.045 Uiso 1 1 calc R . . C18 C 0.8429(6) 0.5360(2) 0.1882(3) 0.0362(11) Uani 1 1 d . . . H18A H 0.9241 0.5078 0.1625 0.054 Uiso 1 1 calc R . . H18B H 0.7339 0.509 0.19 0.054 Uiso 1 1 calc R . . H18C H 0.8932 0.544 0.2341 0.054 Uiso 1 1 calc R . . C19 C 1.1034(5) 0.7150(2) 0.3579(2) 0.0248(9) Uani 1 1 d . . . C20 C 1.0075(6) 0.6561(3) 0.3970(2) 0.0349(11) Uani 1 1 d . . . H20A H 0.9492 0.6216 0.3646 0.042 Uiso 1 1 calc R . . H20B H 1.0926 0.6281 0.4261 0.042 Uiso 1 1 calc R . . C21 C 0.8731(7) 0.6902(3) 0.4406(2) 0.0390(11) Uani 1 1 d . . . H21A H 0.8086 0.6511 0.4627 0.047 Uiso 1 1 calc R . . H21B H 0.9323 0.7206 0.4763 0.047 Uiso 1 1 calc R . . C22 C 0.7470(6) 0.7373(3) 0.3975(2) 0.0337(10) Uani 1 1 d . . . H22A H 0.6678 0.7625 0.4272 0.04 Uiso 1 1 calc R . . H22B H 0.676 0.7054 0.3665 0.04 Uiso 1 1 calc R . . C23 C 0.8394(5) 0.7947(2) 0.3560(2) 0.0246(9) Uani 1 1 d . . . C24 C 1.2155(6) 0.6777(3) 0.3071(2) 0.0332(10) Uani 1 1 d . . . H24A H 1.2762 0.715 0.2821 0.05 Uiso 1 1 calc R . . H24B H 1.1416 0.6486 0.2755 0.05 Uiso 1 1 calc R . . H24C H 1.3005 0.6458 0.3311 0.05 Uiso 1 1 calc R . . C25 C 1.2297(6) 0.7573(3) 0.4065(2) 0.0336(10) Uani 1 1 d . . . H25A H 1.1645 0.7823 0.4404 0.05 Uiso 1 1 calc R . . H25B H 1.2931 0.7933 0.3811 0.05 Uiso 1 1 calc R . . H25C H 1.312 0.723 0.429 0.05 Uiso 1 1 calc R . . C26 C 0.7078(6) 0.8260(2) 0.3027(2) 0.0296(10) Uani 1 1 d . . . H26A H 0.7645 0.8628 0.2758 0.044 Uiso 1 1 calc R . . H26B H 0.6119 0.8487 0.3251 0.044 Uiso 1 1 calc R . . H26C H 0.6629 0.7865 0.2732 0.044 Uiso 1 1 calc R . . C27 C 0.9004(6) 0.8600(3) 0.4011(2) 0.0330(10) Uani 1 1 d . . . H27A H 0.9596 0.8959 0.374 0.049 Uiso 1 1 calc R . . H27B H 0.9805 0.8425 0.4378 0.049 Uiso 1 1 calc R . . H27C H 0.7998 0.883 0.4201 0.049 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 Y 0.0651(3) 0.0158(2) 0.0172(2) -0.00039(15) 0.00236(19) -0.0037(2) N1 0.0186(16) 0.0165(16) 0.0226(17) 0.0008(13) -0.0004(13) 0.0001(13) N2 0.0231(17) 0.0169(16) 0.0227(17) -0.0017(13) 0.0048(14) -0.0009(13) N3 0.0224(17) 0.0230(17) 0.0176(16) 0.0000(13) 0.0008(13) 0.0051(14) C1 0.020(2) 0.024(2) 0.025(2) 0.0009(16) -0.0004(16) -0.0032(16) C2 0.037(2) 0.022(2) 0.030(2) -0.0017(17) -0.0022(19) -0.0063(18) C3 0.040(3) 0.022(2) 0.034(2) -0.0024(18) 0.001(2) 0.0034(19) C4 0.027(2) 0.029(2) 0.030(2) 0.0016(18) -0.0031(18) 0.0057(18) C5 0.023(2) 0.022(2) 0.021(2) 0.0013(16) -0.0024(16) -0.0022(16) C6 0.023(2) 0.042(3) 0.045(3) 0.001(2) 0.010(2) -0.005(2) C7 0.028(2) 0.035(3) 0.045(3) 0.007(2) -0.014(2) -0.005(2) C8 0.027(2) 0.030(2) 0.028(2) 0.0007(18) -0.0064(18) -0.0031(18) C9 0.044(3) 0.034(2) 0.020(2) 0.0003(18) -0.0010(19) -0.004(2) C10 0.024(2) 0.020(2) 0.024(2) -0.0036(16) 0.0078(16) 0.0043(16) C11 0.037(2) 0.037(3) 0.021(2) -0.0017(18) 0.0056(19) 0.005(2) C12 0.040(3) 0.041(3) 0.030(2) -0.014(2) -0.001(2) -0.002(2) C13 0.026(2) 0.035(2) 0.032(2) -0.0105(19) 0.0000(18) -0.0034(19) C14 0.025(2) 0.020(2) 0.024(2) -0.0031(16) 0.0052(17) -0.0034(16) C15 0.029(2) 0.030(2) 0.037(3) -0.0014(19) 0.0133(19) -0.0013(19) C16 0.027(2) 0.029(2) 0.040(3) -0.001(2) 0.0036(19) 0.0065(19) C17 0.025(2) 0.030(2) 0.035(2) -0.0047(19) 0.0117(18) -0.0059(18) C18 0.039(3) 0.025(2) 0.045(3) 0.004(2) 0.012(2) -0.004(2) C19 0.027(2) 0.026(2) 0.022(2) 0.0016(17) -0.0013(17) 0.0063(17) C20 0.037(3) 0.033(2) 0.033(2) 0.010(2) -0.010(2) 0.002(2) C21 0.045(3) 0.040(3) 0.032(3) 0.013(2) 0.004(2) -0.005(2) C22 0.033(2) 0.039(3) 0.029(2) 0.003(2) 0.0062(19) 0.000(2) C23 0.027(2) 0.029(2) 0.018(2) -0.0026(17) 0.0011(16) 0.0074(18) C24 0.029(2) 0.036(3) 0.033(2) -0.004(2) -0.0046(19) 0.0162(19) C25 0.032(2) 0.036(3) 0.031(2) -0.002(2) -0.0070(19) 0.004(2) C26 0.028(2) 0.030(2) 0.030(2) -0.0013(18) -0.0001(18) 0.0115(18) C27 0.035(2) 0.032(2) 0.032(2) -0.0086(19) 0.0049(19) 0.002(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y N2 2.206(3) . ? Y N3 2.207(3) . ? Y N1 2.209(3) . ? N1 C1 1.463(5) . ? N1 C5 1.468(5) . ? N2 C14 1.465(5) . ? N2 C10 1.473(5) . ? N3 C19 1.470(5) . ? N3 C23 1.478(5) . ? C1 C2 1.535(6) . ? C1 C7 1.538(6) . ? C1 C6 1.551(6) . ? C2 C3 1.520(6) . ? C3 C4 1.535(6) . ? C4 C5 1.535(6) . ? C5 C8 1.535(6) . ? C5 C9 1.539(6) . ? C10 C15 1.530(6) . ? C10 C11 1.536(6) . ? C10 C16 1.555(6) . ? C11 C12 1.535(7) . ? C12 C13 1.521(6) . ? C13 C14 1.548(6) . ? C14 C18 1.537(6) . ? C14 C17 1.537(6) . ? C19 C24 1.531(6) . ? C19 C25 1.538(6) . ? C19 C20 1.545(6) . ? C20 C21 1.527(7) . ? C21 C22 1.524(7) . ? C22 C23 1.539(6) . ? C23 C26 1.533(6) . ? C23 C27 1.549(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Y N3 120.25(12) . . ? N2 Y N1 120.76(12) . . ? N3 Y N1 118.91(12) . . ? C1 N1 C5 116.7(3) . . ? C1 N1 Y 122.1(2) . . ? C5 N1 Y 120.4(2) . . ? C14 N2 C10 116.4(3) . . ? C14 N2 Y 121.2(2) . . ? C10 N2 Y 121.9(2) . . ? C19 N3 C23 116.5(3) . . ? C19 N3 Y 119.4(2) . . ? C23 N3 Y 123.3(2) . . ? N1 C1 C2 110.8(3) . . ? N1 C1 C7 106.7(3) . . ? C2 C1 C7 108.4(4) . . ? N1 C1 C6 115.0(3) . . ? C2 C1 C6 109.6(4) . . ? C7 C1 C6 105.9(4) . . ? C3 C2 C1 111.6(4) . . ? C2 C3 C4 110.4(4) . . ? C5 C4 C3 112.1(3) . . ? N1 C5 C4 111.4(3) . . ? N1 C5 C8 106.4(3) . . ? C4 C5 C8 108.1(3) . . ? N1 C5 C9 114.4(3) . . ? C4 C5 C9 110.2(3) . . ? C8 C5 C9 105.9(3) . . ? N2 C10 C15 106.7(3) . . ? N2 C10 C11 111.3(3) . . ? C15 C10 C11 108.7(4) . . ? N2 C10 C16 114.3(3) . . ? C15 C10 C16 105.9(3) . . ? C11 C10 C16 109.6(3) . . ? C12 C11 C10 111.5(4) . . ? C13 C12 C11 110.7(4) . . ? C12 C13 C14 111.7(4) . . ? N2 C14 C18 114.9(3) . . ? N2 C14 C17 106.2(3) . . ? C18 C14 C17 106.2(3) . . ? N2 C14 C13 111.5(3) . . ? C18 C14 C13 110.0(4) . . ? C17 C14 C13 107.6(3) . . ? N3 C19 C24 106.6(3) . . ? N3 C19 C25 114.6(4) . . ? C24 C19 C25 105.9(4) . . ? N3 C19 C20 110.2(3) . . ? C24 C19 C20 109.4(4) . . ? C25 C19 C20 109.9(4) . . ? C21 C20 C19 111.5(4) . . ? C22 C21 C20 110.3(4) . . ? C21 C22 C23 112.6(4) . . ? N3 C23 C26 106.3(3) . . ? N3 C23 C22 111.2(3) . . ? C26 C23 C22 108.3(4) . . ? N3 C23 C27 114.1(3) . . ? C26 C23 C27 106.1(4) . . ? C22 C23 C27 110.5(4) . . ? #===END data_(6)-jun203 _database_code_depnum_ccdc_archive 'CCDC 239408' _audit_creation_date 2003-06-02T16:39:39-00:00 _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 'C40 H82 Ce2 N4 O2' _chemical_formula_sum 'C40 H82 Ce2 N4 O2' _chemical_formula_weight 931.34 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6239(2) _cell_length_b 11.4835(1) _cell_length_c 14.6812(2) _cell_angle_alpha 90 _cell_angle_beta 104.920(1) _cell_angle_gamma 90 _cell_volume 2219.44(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14340 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.059 _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 0.5613 _exptl_absorpt_correction_T_max 0.6444 #----------------------------------------------------------------------------# # 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 0.55244E-2 _diffrn_orient_matrix_ub_12 0.776633E-1 _diffrn_orient_matrix_ub_13 0.317298E-1 _diffrn_orient_matrix_ub_21 -0.649708E-1 _diffrn_orient_matrix_ub_22 0.249063E-1 _diffrn_orient_matrix_ub_23 -0.449499E-1 _diffrn_orient_matrix_ub_31 -0.389668E-1 _diffrn_orient_matrix_ub_32 -0.305166E-1 _diffrn_orient_matrix_ub_33 0.440646E-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 0.0349 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_number 26877 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 5027 _reflns_number_gt 4215 _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^)+(0.0099P)^2^+2.1900P] 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 5027 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.047 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.494 _refine_diff_density_min -0.63 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # 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' 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 0.646043(7) -0.000596(8) 0.038142(6) 0.01572(4) Uani 1 1 d . . . O O 0.49744(10) -0.03809(12) 0.08996(9) 0.0214(3) Uani 1 1 d . . . N1 N 0.73273(11) -0.15110(13) -0.01348(10) 0.0188(3) Uani 1 1 d . . . N2 N 0.73942(11) 0.14499(13) 0.13364(11) 0.0200(3) Uani 1 1 d . . . C1 C 0.81444(14) -0.12744(17) -0.06032(13) 0.0232(4) Uani 1 1 d . . . C2 C 0.91583(15) -0.1811(2) -0.00509(15) 0.0332(5) Uani 1 1 d . . . H2A H 0.9668 -0.1715 -0.0419 0.04 Uiso 1 1 calc R . . H2B H 0.9407 -0.1389 0.0553 0.04 Uiso 1 1 calc R . . C3 C 0.90551(17) -0.3094(2) 0.01505(17) 0.0400(6) Uani 1 1 d . . . H3A H 0.9711 -0.3398 0.0535 0.048 Uiso 1 1 calc R . . H3B H 0.887 -0.3534 -0.0449 0.048 Uiso 1 1 calc R . . C4 C 0.82367(17) -0.3253(2) 0.06792(16) 0.0343(5) Uani 1 1 d . . . H4A H 0.8463 -0.288 0.1306 0.041 Uiso 1 1 calc R . . H4B H 0.8145 -0.4095 0.0778 0.041 Uiso 1 1 calc R . . C5 C 0.72150(15) -0.27256(16) 0.01470(14) 0.0242(4) Uani 1 1 d . . . C6 C 0.82612(19) 0.00496(18) -0.06268(17) 0.0327(5) Uani 1 1 d . . . H6A H 0.7617 0.0398 -0.0976 0.049 Uiso 1 1 calc R . . H6B H 0.8795 0.0246 -0.0939 0.049 Uiso 1 1 calc R . . H6C H 0.8446 0.0353 0.0019 0.049 Uiso 1 1 calc R . . C7 C 0.79095(17) -0.1677(2) -0.16416(14) 0.0321(5) Uani 1 1 d . . . H7A H 0.7262 -0.134 -0.1995 0.048 Uiso 1 1 calc R . . H7B H 0.7864 -0.2528 -0.1669 0.048 Uiso 1 1 calc R . . H7C H 0.8453 -0.1417 -0.192 0.048 Uiso 1 1 calc R . . C8 C 0.66818(19) -0.3528(2) -0.06764(17) 0.0405(5) Uani 1 1 d . . . H8A H 0.6033 -0.318 -0.1013 0.061 Uiso 1 1 calc R . . H8B H 0.6559 -0.4291 -0.0428 0.061 Uiso 1 1 calc R . . H8C H 0.7115 -0.3621 -0.111 0.061 Uiso 1 1 calc R . . C9 C 0.65263(16) -0.26967(18) 0.08257(16) 0.0298(4) Uani 1 1 d . . . H9A H 0.5866 -0.2363 0.0503 0.045 Uiso 1 1 calc R . . H9B H 0.6843 -0.2218 0.1375 0.045 Uiso 1 1 calc R . . H9C H 0.643 -0.3491 0.1032 0.045 Uiso 1 1 calc R . . C10 C 0.73805(16) 0.26593(17) 0.10042(15) 0.0268(4) Uani 1 1 d . . . C11 C 0.84432(17) 0.30520(19) 0.09496(17) 0.0353(5) Uani 1 1 d . . . H11A H 0.8622 0.2642 0.0421 0.042 Uiso 1 1 calc R . . H11B H 0.8427 0.3897 0.0814 0.042 Uiso 1 1 calc R . . C12 C 0.92599(18) 0.2814(2) 0.18528(18) 0.0426(6) Uani 1 1 d . . . H12A H 0.9142 0.3308 0.2367 0.051 Uiso 1 1 calc R . . H12B H 0.9935 0.3013 0.176 0.051 Uiso 1 1 calc R . . C13 C 0.92441(15) 0.1539(2) 0.21251(15) 0.0330(5) Uani 1 1 d . . . H13A H 0.9742 0.1412 0.274 0.04 Uiso 1 1 calc R . . H13B H 0.9453 0.1055 0.1649 0.04 Uiso 1 1 calc R . . C14 C 0.81859(14) 0.11494(18) 0.21964(13) 0.0256(4) Uani 1 1 d . . . C15 C 0.66714(17) 0.26866(19) 0.00079(16) 0.0339(5) Uani 1 1 d . . . H15A H 0.599 0.2434 0.0029 0.051 Uiso 1 1 calc R . . H15B H 0.6932 0.2161 -0.0401 0.051 Uiso 1 1 calc R . . H15C H 0.6638 0.3481 -0.0242 0.051 Uiso 1 1 calc R . . C16 C 0.6939(2) 0.3544(2) 0.15921(19) 0.0431(6) Uani 1 1 d . . . H16A H 0.6266 0.3284 0.1629 0.065 Uiso 1 1 calc R . . H16B H 0.6883 0.4311 0.129 0.065 Uiso 1 1 calc R . . H16C H 0.7391 0.3597 0.2229 0.065 Uiso 1 1 calc R . . C17 C 0.81793(17) -0.01777(19) 0.22813(15) 0.0316(5) Uani 1 1 d . . . H17A H 0.7508 -0.0437 0.2327 0.047 Uiso 1 1 calc R . . H17B H 0.8694 -0.0419 0.2848 0.047 Uiso 1 1 calc R . . H17C H 0.8331 -0.0527 0.1724 0.047 Uiso 1 1 calc R . . C18 C 0.79908(18) 0.1628(2) 0.31231(15) 0.0395(6) Uani 1 1 d . . . H18A H 0.7988 0.2482 0.3107 0.059 Uiso 1 1 calc R . . H18B H 0.8529 0.1359 0.3661 0.059 Uiso 1 1 calc R . . H18C H 0.7332 0.1347 0.3186 0.059 Uiso 1 1 calc R . . C19 C 0.4914(2) -0.0607(2) 0.18329(15) 0.0406(6) Uani 1 1 d . . . H19A H 0.5457 -0.1162 0.2134 0.049 Uiso 1 1 calc R . . H19B H 0.4253 -0.098 0.1811 0.049 Uiso 1 1 calc R . . C20 C 0.5016(2) 0.0464(3) 0.24185(17) 0.0475(6) Uani 1 1 d . . . H20A H 0.4971 0.0259 0.3054 0.071 Uiso 1 1 calc R . . H20B H 0.4471 0.1009 0.2133 0.071 Uiso 1 1 calc R . . H20C H 0.5675 0.0829 0.2454 0.071 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 Ce 0.01384(6) 0.01683(6) 0.01675(6) -0.00072(4) 0.00440(4) 0.00053(4) O 0.0208(6) 0.0284(7) 0.0160(6) 0.0042(5) 0.0064(5) 0.0014(5) N1 0.0179(7) 0.0189(7) 0.0196(8) -0.0017(6) 0.0047(6) 0.0010(6) N2 0.0194(7) 0.0198(8) 0.0221(8) -0.0032(6) 0.0077(6) -0.0008(6) C1 0.0213(9) 0.0295(10) 0.0201(9) -0.0041(8) 0.0074(7) 0.0017(8) C2 0.0183(10) 0.0543(14) 0.0276(11) -0.0062(10) 0.0069(8) 0.0049(9) C3 0.0307(11) 0.0524(15) 0.0365(12) 0.0051(11) 0.0077(9) 0.0237(11) C4 0.0379(12) 0.0305(11) 0.0342(12) 0.0055(9) 0.0085(10) 0.0144(9) C5 0.0250(10) 0.0192(9) 0.0272(10) -0.0006(8) 0.0047(8) 0.0031(8) C6 0.0369(12) 0.0329(12) 0.0355(12) -0.0043(9) 0.0222(10) -0.0067(9) C7 0.0341(11) 0.0420(12) 0.0211(10) -0.0052(9) 0.0087(8) 0.0060(10) C8 0.0475(14) 0.0272(11) 0.0444(14) -0.0085(10) 0.0077(11) -0.0073(10) C9 0.0295(11) 0.0226(10) 0.0399(12) 0.0054(9) 0.0133(9) 0.0004(8) C10 0.0292(10) 0.0194(9) 0.0356(11) -0.0033(8) 0.0155(9) -0.0015(8) C11 0.0397(12) 0.0228(10) 0.0500(14) -0.0059(9) 0.0232(11) -0.0090(9) C12 0.0333(12) 0.0472(14) 0.0515(15) -0.0202(12) 0.0185(11) -0.0207(11) C13 0.0201(10) 0.0502(14) 0.0286(11) -0.0110(10) 0.0062(8) -0.0066(9) C14 0.0225(9) 0.0346(11) 0.0201(9) -0.0064(8) 0.0060(8) -0.0037(8) C15 0.0383(12) 0.0234(10) 0.0415(13) 0.0078(9) 0.0130(10) 0.0037(9) C16 0.0496(14) 0.0271(11) 0.0603(16) -0.0106(11) 0.0283(13) 0.0037(10) C17 0.0328(11) 0.0369(12) 0.0219(10) 0.0044(8) 0.0011(8) 0.0025(9) C18 0.0363(12) 0.0594(16) 0.0248(11) -0.0138(10) 0.0116(9) -0.0083(11) C19 0.0515(15) 0.0518(15) 0.0216(11) 0.0075(10) 0.0151(10) -0.0008(12) C20 0.0404(13) 0.0746(18) 0.0284(12) -0.0096(12) 0.0104(10) 0.0056(13) #----------------------------------------------------------------------------# # 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 2.3275(15) . ? Ce N2 2.3368(15) . ? Ce O 2.3782(12) . ? Ce O 2.3796(13) 3_655 ? O C19 1.418(2) . ? O Ce 2.3796(13) 3_655 ? N1 C5 1.474(2) . ? N1 C1 1.477(2) . ? N2 C10 1.470(2) . ? N2 C14 1.475(2) . ? C1 C6 1.530(3) . ? C1 C2 1.539(3) . ? C1 C7 1.546(3) . ? C2 C3 1.516(3) . ? C3 C4 1.525(3) . ? C4 C5 1.534(3) . ? C5 C9 1.535(3) . ? C5 C8 1.544(3) . ? C10 C15 1.532(3) . ? C10 C11 1.538(3) . ? C10 C16 1.551(3) . ? C11 C12 1.520(4) . ? C12 C13 1.519(3) . ? C13 C14 1.539(3) . ? C14 C17 1.529(3) . ? C14 C18 1.552(3) . ? C19 C20 1.486(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ce N2 118.89(5) . . ? N1 Ce O 120.99(5) . . ? N2 Ce O 108.32(5) . . ? N1 Ce O 105.29(5) . 3_655 ? N2 Ce O 123.38(5) . 3_655 ? O Ce O 72.11(5) . 3_655 ? C19 O Ce 127.48(13) . . ? C19 O Ce 123.89(13) . 3_655 ? Ce O Ce 107.89(5) . 3_655 ? C5 N1 C1 116.75(14) . . ? C5 N1 Ce 120.88(11) . . ? C1 N1 Ce 121.44(11) . . ? C10 N2 C14 116.68(15) . . ? C10 N2 Ce 121.22(12) . . ? C14 N2 Ce 120.75(12) . . ? N1 C1 C6 106.78(15) . . ? N1 C1 C2 111.28(16) . . ? C6 C1 C2 109.01(18) . . ? N1 C1 C7 114.51(16) . . ? C6 C1 C7 105.72(17) . . ? C2 C1 C7 109.25(16) . . ? C3 C2 C1 112.11(18) . . ? C2 C3 C4 109.43(18) . . ? C3 C4 C5 112.33(17) . . ? N1 C5 C9 106.66(15) . . ? N1 C5 C4 111.73(16) . . ? C9 C5 C4 107.70(16) . . ? N1 C5 C8 113.99(17) . . ? C9 C5 C8 106.14(17) . . ? C4 C5 C8 110.21(17) . . ? N2 C10 C15 106.68(16) . . ? N2 C10 C11 111.25(16) . . ? C15 C10 C11 108.35(17) . . ? N2 C10 C16 114.08(17) . . ? C15 C10 C16 106.17(18) . . ? C11 C10 C16 109.98(17) . . ? C12 C11 C10 112.90(18) . . ? C11 C12 C13 110.26(18) . . ? C12 C13 C14 112.04(18) . . ? N2 C14 C17 106.54(15) . . ? N2 C14 C13 111.41(16) . . ? C17 C14 C13 108.70(18) . . ? N2 C14 C18 114.51(17) . . ? C17 C14 C18 106.01(18) . . ? C13 C14 C18 109.35(16) . . ? O C19 C20 112.8(2) . . ? #===END