# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; New reactions of beta-diketiminatolanthanoid complexes: sterically induced self-deprotonation of beta-diketiminato ligands ; _publ_requested_category FM loop_ _publ_author_name 'M. Lappert' 'P. B. Hitchcock' 'Andrey Protchenko' data_(1)-apr604 _database_code_depnum_ccdc_archive 'CCDC 254749' _audit_creation_date 2004-04-07T08:20:28-00:00 _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 ; '(C58 H81 N4 Tm1), (C29 H42 N2), 0.5(C7 H8)' ; _chemical_formula_sum 'C90.5 H127 N6 Tm' _chemical_formula_weight 1467.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9404(2) _cell_length_b 16.9293(2) _cell_length_c 24.5836(3) _cell_angle_alpha 70.187(1) _cell_angle_beta 83.689(1) _cell_angle_gamma 75.243(1) _cell_volume 4140.99(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42699 _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 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1562 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.117 _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 0.7243 _exptl_absorpt_correction_T_max 0.8482 #----------------------------------------------------------------------------# # 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 -0.461347E-1 _diffrn_orient_matrix_ub_12 0.130013E-1 _diffrn_orient_matrix_ub_13 0.345381E-1 _diffrn_orient_matrix_ub_21 -0.703352E-1 _diffrn_orient_matrix_ub_22 -0.24212E-1 _diffrn_orient_matrix_ub_23 -0.55261E-2 _diffrn_orient_matrix_ub_31 0.431854E-1 _diffrn_orient_matrix_ub_32 -0.584139E-1 _diffrn_orient_matrix_ub_33 0.254416E-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 0.0581 _diffrn_reflns_av_unetI/netI 0.0421 _diffrn_reflns_number 63879 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 14519 _reflns_number_gt 12932 _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 H atoms of the C34 CH2 group , and the H atom on N2a were located on a difference map and refined. The disordered toluene molecule was included with isotropic C atoms , H atoms omitted, and SADI constraints. Other H atoms were in riding mode. 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^)+(0.0417P)^2^+3.2234P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 14519 _refine_ls_number_parameters 880 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.795 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.072 #----------------------------------------------------------------------------# # 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' Tm Tm -0.3139 5.2483 '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 Tm Tm 0.164317(10) 0.228466(6) 0.238974(4) 0.02233(3) Uani 1 1 d . . . N1 N 0.33402(18) 0.11399(12) 0.25644(8) 0.0259(5) Uani 1 1 d . . . N2 N 0.23474(19) 0.26396(12) 0.31047(8) 0.0282(5) Uani 1 1 d . . . N3 N 0.13606(19) 0.30275(12) 0.14644(8) 0.0272(5) Uani 1 1 d . . . N4 N -0.01560(19) 0.19276(12) 0.25522(9) 0.0274(5) Uani 1 1 d . . . C1 C 0.4375(2) 0.13925(16) 0.25821(11) 0.0320(6) Uani 1 1 d . . . C2 C 0.4362(2) 0.22051(16) 0.26414(12) 0.0355(7) Uani 1 1 d . . . H2 H 0.5059 0.2438 0.2454 0.043 Uiso 1 1 calc R . . C3 C 0.3527(2) 0.27186(16) 0.29196(11) 0.0319(6) Uani 1 1 d . . . C4 C 0.5673(3) 0.08413(19) 0.25365(14) 0.0472(8) Uani 1 1 d . . . H4A H 0.5604 0.0265 0.2559 0.071 Uiso 1 1 calc R . . H4B H 0.6184 0.0794 0.2854 0.071 Uiso 1 1 calc R . . H4C H 0.6076 0.1106 0.2166 0.071 Uiso 1 1 calc R . . C5 C 0.4043(3) 0.34318(18) 0.29921(15) 0.0513(8) Uani 1 1 d . . . H5A H 0.3830 0.3953 0.2655 0.077 Uiso 1 1 calc R . . H5B H 0.4964 0.3242 0.3025 0.077 Uiso 1 1 calc R . . H5C H 0.3668 0.3559 0.3342 0.077 Uiso 1 1 calc R . . C6 C 0.3475(2) 0.02741(15) 0.25409(11) 0.0293(6) Uani 1 1 d . . . C7 C 0.3371(2) -0.03882(16) 0.30596(11) 0.0342(6) Uani 1 1 d . . . C8 C 0.3559(3) -0.12250(16) 0.30399(13) 0.0406(7) Uani 1 1 d . . . H8 H 0.3507 -0.1686 0.3388 0.049 Uiso 1 1 calc R . . C9 C 0.3816(3) -0.13918(17) 0.25266(13) 0.0437(8) Uani 1 1 d . . . H9 H 0.3947 -0.1966 0.2522 0.052 Uiso 1 1 calc R . . C10 C 0.3888(3) -0.07330(17) 0.20161(13) 0.0422(7) Uani 1 1 d . . . H10 H 0.4054 -0.0858 0.1663 0.051 Uiso 1 1 calc R . . C11 C 0.3719(2) 0.01150(16) 0.20106(11) 0.0343(7) Uani 1 1 d . . . C12 C 0.3134(3) -0.02356(17) 0.36408(12) 0.0415(7) Uani 1 1 d . . . H12 H 0.2935 0.0401 0.3567 0.050 Uiso 1 1 calc R . . C13 C 0.2007(3) -0.0577(2) 0.39699(14) 0.0561(9) Uani 1 1 d . . . H13A H 0.1876 -0.0463 0.4340 0.084 Uiso 1 1 calc R . . H13B H 0.2174 -0.1200 0.4042 0.084 Uiso 1 1 calc R . . H13C H 0.1247 -0.0286 0.3739 0.084 Uiso 1 1 calc R . . C14 C 0.4328(4) -0.0642(3) 0.40002(15) 0.0698(11) Uani 1 1 d . . . H14A H 0.4167 -0.0535 0.4372 0.105 Uiso 1 1 calc R . . H14B H 0.5022 -0.0386 0.3791 0.105 Uiso 1 1 calc R . . H14C H 0.4558 -0.1266 0.4067 0.105 Uiso 1 1 calc R . . C15 C 0.3833(3) 0.08183(17) 0.14380(12) 0.0400(7) Uani 1 1 d . . . H15 H 0.3778 0.1365 0.1521 0.048 Uiso 1 1 calc R . . C16 C 0.5103(3) 0.0606(2) 0.11226(14) 0.0557(9) Uani 1 1 d . . . H16A H 0.5137 0.1075 0.0758 0.084 Uiso 1 1 calc R . . H16B H 0.5185 0.0066 0.1042 0.084 Uiso 1 1 calc R . . H16C H 0.5795 0.0543 0.1366 0.084 Uiso 1 1 calc R . . C17 C 0.2752(3) 0.0978(2) 0.10374(14) 0.0542(9) Uani 1 1 d . . . H17A H 0.2851 0.1433 0.0674 0.081 Uiso 1 1 calc R . . H17B H 0.1941 0.1156 0.1225 0.081 Uiso 1 1 calc R . . H17C H 0.2774 0.0445 0.0957 0.081 Uiso 1 1 calc R . . C18 C 0.1826(3) 0.29542(17) 0.35779(11) 0.0366(6) Uani 1 1 d . . . C19 C 0.2287(3) 0.24701(19) 0.41375(12) 0.0492(8) Uani 1 1 d . . . C20 C 0.1829(4) 0.2777(2) 0.45922(15) 0.0700(11) Uani 1 1 d . . . H20 H 0.2163 0.2469 0.4966 0.084 Uiso 1 1 calc R . . C21 C 0.0897(5) 0.3523(3) 0.45118(16) 0.0825(13) Uani 1 1 d . . . H21 H 0.0582 0.3721 0.4830 0.099 Uiso 1 1 calc R . . C22 C 0.0415(4) 0.3986(2) 0.39653(17) 0.0755(11) Uani 1 1 d . . . H22 H -0.0246 0.4491 0.3917 0.091 Uiso 1 1 calc R . . C23 C 0.0885(3) 0.3725(2) 0.34830(14) 0.0524(8) Uani 1 1 d . . . C24 C 0.3275(3) 0.1621(2) 0.42644(13) 0.0558(9) Uani 1 1 d . . . H24 H 0.3287 0.1400 0.3934 0.067 Uiso 1 1 calc R . . C25 C 0.2988(5) 0.0928(3) 0.48135(16) 0.0850(14) Uani 1 1 d . . . H25A H 0.3651 0.0397 0.4867 0.127 Uiso 1 1 calc R . . H25B H 0.2169 0.0813 0.4781 0.127 Uiso 1 1 calc R . . H25C H 0.2958 0.1127 0.5146 0.127 Uiso 1 1 calc R . . C26 C 0.4625(4) 0.1722(3) 0.4306(2) 0.0975(16) Uani 1 1 d . . . H26A H 0.5221 0.1157 0.4386 0.146 Uiso 1 1 calc R . . H26B H 0.4642 0.1955 0.4619 0.146 Uiso 1 1 calc R . . H26C H 0.4868 0.2118 0.3939 0.146 Uiso 1 1 calc R . . C27 C 0.0433(4) 0.4314(2) 0.28819(17) 0.0722(11) Uani 1 1 d . . . H27 H 0.0652 0.3960 0.2616 0.087 Uiso 1 1 calc R . . C28 C 0.1097(5) 0.5059(3) 0.2644(2) 0.1000(17) Uani 1 1 d . . . H28A H 0.0789 0.5418 0.2258 0.150 Uiso 1 1 calc R . . H28B H 0.2012 0.4828 0.2620 0.150 Uiso 1 1 calc R . . H28C H 0.0918 0.5410 0.2902 0.150 Uiso 1 1 calc R . . C29 C -0.0995(4) 0.4656(3) 0.2881(2) 0.1015(15) Uani 1 1 d . . . H29A H -0.1256 0.5025 0.2489 0.152 Uiso 1 1 calc R . . H29B H -0.1240 0.4993 0.3146 0.152 Uiso 1 1 calc R . . H29C H -0.1407 0.4171 0.3005 0.152 Uiso 1 1 calc R . . C30 C 0.0305(2) 0.36449(15) 0.15566(11) 0.0311(6) Uani 1 1 d . . . C31 C -0.0641(2) 0.34586(15) 0.19434(11) 0.0331(6) Uani 1 1 d . . . H31 H -0.1137 0.3946 0.2038 0.040 Uiso 1 1 calc R . . C32 C -0.1072(2) 0.26473(15) 0.22543(11) 0.0295(6) Uani 1 1 d . . . C33 C 0.0309(3) 0.45899(17) 0.12387(14) 0.0499(9) Uani 1 1 d . . . H33A H -0.0527 0.4953 0.1282 0.075 Uiso 1 1 calc R . . H33B H 0.0507 0.4672 0.0827 0.075 Uiso 1 1 calc R . . H33C H 0.0947 0.4752 0.1402 0.075 Uiso 1 1 calc R . . C34 C -0.2302(3) 0.26875(19) 0.22576(16) 0.0502(9) Uani 1 1 d . . . H34A H -0.286(3) 0.321(2) 0.2069(15) 0.069(11) Uiso 1 1 d . . . H34B H -0.267(3) 0.2216(18) 0.2475(12) 0.046(8) Uiso 1 1 d . . . C35 C 0.1838(3) 0.31838(15) 0.08824(10) 0.0306(6) Uani 1 1 d . . . C36 C 0.3074(3) 0.33017(17) 0.07314(12) 0.0401(7) Uani 1 1 d . . . C37 C 0.3500(3) 0.3427(2) 0.01575(14) 0.0544(9) Uani 1 1 d . . . H37 H 0.4333 0.3506 0.0052 0.065 Uiso 1 1 calc R . . C38 C 0.2747(4) 0.3439(2) -0.02585(13) 0.0603(10) Uani 1 1 d . . . H38 H 0.3057 0.3523 -0.0646 0.072 Uiso 1 1 calc R . . C39 C 0.1545(3) 0.33289(19) -0.01080(12) 0.0505(9) Uani 1 1 d . . . H39 H 0.1021 0.3351 -0.0399 0.061 Uiso 1 1 calc R . . C40 C 0.1066(3) 0.31859(16) 0.04559(11) 0.0367(7) Uani 1 1 d . . . C41 C 0.3936(3) 0.3329(2) 0.11618(14) 0.0534(9) Uani 1 1 d . . . H41 H 0.3614 0.3040 0.1557 0.064 Uiso 1 1 calc R . . C42 C 0.3888(5) 0.4256(3) 0.1119(3) 0.1332(19) Uani 1 1 d . . . H42A H 0.4449 0.4255 0.1403 0.200 Uiso 1 1 calc R . . H42B H 0.3020 0.4542 0.1195 0.200 Uiso 1 1 calc R . . H42C H 0.4164 0.4566 0.0729 0.200 Uiso 1 1 calc R . . C43 C 0.5306(3) 0.2858(2) 0.11098(17) 0.0652(10) Uani 1 1 d . . . H43A H 0.5804 0.2899 0.1403 0.098 Uiso 1 1 calc R . . H43B H 0.5649 0.3121 0.0724 0.098 Uiso 1 1 calc R . . H43C H 0.5347 0.2249 0.1169 0.098 Uiso 1 1 calc R . . C44 C -0.0248(3) 0.30149(19) 0.05927(12) 0.0447(8) Uani 1 1 d . . . H44 H -0.0359 0.2794 0.1023 0.054 Uiso 1 1 calc R . . C45 C -0.0426(4) 0.2329(2) 0.03509(15) 0.0658(10) Uani 1 1 d . . . H45A H -0.1283 0.2237 0.0448 0.099 Uiso 1 1 calc R . . H45B H 0.0192 0.1787 0.0520 0.099 Uiso 1 1 calc R . . H45C H -0.0302 0.2525 -0.0070 0.099 Uiso 1 1 calc R . . C46 C -0.1287(3) 0.3831(2) 0.03620(17) 0.0670(11) Uani 1 1 d . . . H46A H -0.2115 0.3688 0.0456 0.101 Uiso 1 1 calc R . . H46B H -0.1181 0.4071 -0.0059 0.101 Uiso 1 1 calc R . . H46C H -0.1233 0.4257 0.0541 0.101 Uiso 1 1 calc R . . C47 C -0.0633(2) 0.12014(15) 0.29157(11) 0.0286(6) Uani 1 1 d . . . C48 C -0.1075(3) 0.11745(18) 0.34800(12) 0.0373(7) Uani 1 1 d . . . C49 C -0.1558(3) 0.0475(2) 0.38213(13) 0.0479(8) Uani 1 1 d . . . H49 H -0.1862 0.0450 0.4203 0.057 Uiso 1 1 calc R . . C50 C -0.1606(3) -0.0182(2) 0.36206(14) 0.0509(9) Uani 1 1 d . . . H50 H -0.1945 -0.0652 0.3861 0.061 Uiso 1 1 calc R . . C51 C -0.1164(3) -0.01541(17) 0.30716(13) 0.0425(7) Uani 1 1 d . . . H51 H -0.1191 -0.0614 0.2938 0.051 Uiso 1 1 calc R . . C52 C -0.0678(2) 0.05277(16) 0.27076(12) 0.0336(6) Uani 1 1 d . . . C53 C -0.1021(3) 0.1875(2) 0.37274(13) 0.0477(8) Uani 1 1 d . . . H53 H -0.0506 0.2250 0.3445 0.057 Uiso 1 1 calc R . . C54 C -0.0375(5) 0.1542(3) 0.4286(2) 0.1085(16) Uani 1 1 d . . . H54A H -0.0372 0.2025 0.4420 0.163 Uiso 1 1 calc R . . H54B H 0.0498 0.1236 0.4236 0.163 Uiso 1 1 calc R . . H54C H -0.0822 0.1144 0.4573 0.163 Uiso 1 1 calc R . . C55 C -0.2308(4) 0.2452(3) 0.3771(2) 0.1023(15) Uani 1 1 d . . . H55A H -0.2724 0.2660 0.3398 0.153 Uiso 1 1 calc R . . H55B H -0.2211 0.2945 0.3871 0.153 Uiso 1 1 calc R . . H55C H -0.2824 0.2124 0.4070 0.153 Uiso 1 1 calc R . . C56 C -0.0235(3) 0.05362(16) 0.20980(12) 0.0380(7) Uani 1 1 d . . . H56 H 0.0295 0.0970 0.1944 0.046 Uiso 1 1 calc R . . C57 C 0.0574(3) -0.0330(2) 0.20828(15) 0.0594(9) Uani 1 1 d . . . H57A H 0.0842 -0.0290 0.1683 0.089 Uiso 1 1 calc R . . H57B H 0.0082 -0.0771 0.2238 0.089 Uiso 1 1 calc R . . H57C H 0.1321 -0.0487 0.2318 0.089 Uiso 1 1 calc R . . C58 C -0.1343(3) 0.0812(2) 0.16957(14) 0.0619(10) Uani 1 1 d . . . H58A H -0.1859 0.1376 0.1700 0.093 Uiso 1 1 calc R . . H58B H -0.1862 0.0384 0.1828 0.093 Uiso 1 1 calc R . . H58C H -0.1021 0.0852 0.1301 0.093 Uiso 1 1 calc R . . N1A N 0.5204(2) -0.34583(12) 0.22368(9) 0.0291(5) Uani 1 1 d . A 1 N2A N 0.4558(2) -0.38562(13) 0.33539(9) 0.0332(5) Uani 1 1 d . A 1 H2Y H 0.465(4) -0.344(3) 0.2942(19) 0.117(16) Uiso 1 1 d . B 1 C1A C 0.5585(2) -0.43028(15) 0.23329(11) 0.0293(6) Uani 1 1 d . A 1 C2A C 0.5484(2) -0.48921(15) 0.28871(11) 0.0308(6) Uani 1 1 d . A 1 H2A H 0.5772 -0.5489 0.2931 0.037 Uiso 1 1 calc R A 1 C3A C 0.4999(3) -0.46773(16) 0.33773(11) 0.0341(6) Uani 1 1 d . A 1 C4A C 0.6142(3) -0.46448(17) 0.18450(12) 0.0406(7) Uani 1 1 d . A 1 H4A1 H 0.5520 -0.4449 0.1541 0.061 Uiso 1 1 calc R A 1 H4A2 H 0.6367 -0.5277 0.1991 0.061 Uiso 1 1 calc R A 1 H4A3 H 0.6901 -0.4430 0.1686 0.061 Uiso 1 1 calc R A 1 C5A C 0.4960(4) -0.53849(18) 0.39455(13) 0.0551(9) Uani 1 1 d . A 1 H5A1 H 0.5401 -0.5290 0.4236 0.083 Uiso 1 1 calc R A 1 H5A2 H 0.5374 -0.5944 0.3898 0.083 Uiso 1 1 calc R A 1 H5A3 H 0.4078 -0.5381 0.4073 0.083 Uiso 1 1 calc R A 1 C6A C 0.5243(2) -0.28354(15) 0.16777(10) 0.0295(6) Uani 1 1 d . A 1 C7A C 0.4246(3) -0.26299(17) 0.12978(12) 0.0400(7) Uani 1 1 d . A 1 C8A C 0.4276(3) -0.19800(19) 0.07688(13) 0.0526(9) Uani 1 1 d . A 1 H8A H 0.3620 -0.1832 0.0504 0.063 Uiso 1 1 calc R A 1 C9A C 0.5235(4) -0.1548(2) 0.06218(13) 0.0565(10) Uani 1 1 d . A 1 H9A H 0.5233 -0.1107 0.0259 0.068 Uiso 1 1 calc R A 1 C10A C 0.6189(3) -0.17519(19) 0.09955(13) 0.0491(8) Uani 1 1 d . A 1 H10A H 0.6847 -0.1450 0.0889 0.059 Uiso 1 1 calc R A 1 C11A C 0.6210(3) -0.23966(16) 0.15313(11) 0.0365(7) Uani 1 1 d . A 1 C12A C 0.3159(3) -0.3070(2) 0.14720(14) 0.0524(8) Uani 1 1 d . A 1 H12A H 0.3486 -0.3649 0.1762 0.063 Uiso 1 1 calc R A 1 C13A C 0.2109(4) -0.2576(3) 0.1775(2) 0.0943(14) Uani 1 1 d . A 1 H13D H 0.1415 -0.2873 0.1888 0.142 Uiso 1 1 calc R A 1 H13E H 0.1796 -0.1990 0.1512 0.142 Uiso 1 1 calc R A 1 H13F H 0.2440 -0.2546 0.2121 0.142 Uiso 1 1 calc R A 1 C14A C 0.2642(4) -0.3227(3) 0.09765(19) 0.0946(14) Uani 1 1 d . A 1 H14D H 0.1949 -0.3519 0.1122 0.142 Uiso 1 1 calc R A 1 H14E H 0.3317 -0.3589 0.0810 0.142 Uiso 1 1 calc R A 1 H14F H 0.2329 -0.2673 0.0678 0.142 Uiso 1 1 calc R A 1 C15A C 0.7296(3) -0.2611(2) 0.19330(14) 0.0504(9) Uani 1 1 d . A 1 H15A H 0.7129 -0.3065 0.2299 0.060 Uiso 1 1 calc R A 1 C16A C 0.7394(3) -0.1825(2) 0.20888(16) 0.0664(10) Uani 1 1 d . A 1 H16D H 0.8098 -0.1991 0.2350 0.100 Uiso 1 1 calc R A 1 H16E H 0.6605 -0.1616 0.2280 0.100 Uiso 1 1 calc R A 1 H16F H 0.7543 -0.1366 0.1736 0.100 Uiso 1 1 calc R A 1 C17A C 0.8552(4) -0.2980(2) 0.1669(2) 0.0802(13) Uani 1 1 d . A 1 H17D H 0.9234 -0.3118 0.1937 0.120 Uiso 1 1 calc R A 1 H17E H 0.8727 -0.2553 0.1303 0.120 Uiso 1 1 calc R A 1 H17F H 0.8500 -0.3506 0.1597 0.120 Uiso 1 1 calc R A 1 C18A C 0.4184(3) -0.35909(15) 0.38515(11) 0.0336(7) Uani 1 1 d . A 1 C19A C 0.5113(3) -0.35068(17) 0.41645(11) 0.0396(7) Uani 1 1 d . A 1 C20A C 0.4719(3) -0.32119(18) 0.46345(12) 0.0469(8) Uani 1 1 d . A 1 H20A H 0.5332 -0.3150 0.4853 0.056 Uiso 1 1 calc R A 1 C21A C 0.3456(4) -0.30088(18) 0.47879(13) 0.0532(9) Uani 1 1 d . A 1 H21A H 0.3207 -0.2812 0.5111 0.064 Uiso 1 1 calc R A 1 C22A C 0.2552(3) -0.30903(19) 0.44734(13) 0.0503(9) Uani 1 1 d . A 1 H22A H 0.1684 -0.2948 0.4582 0.060 Uiso 1 1 calc R A 1 C23A C 0.2898(3) -0.33789(17) 0.39989(12) 0.0412(7) Uani 1 1 d . A 1 C24A C 0.6502(3) -0.3704(2) 0.39996(14) 0.0544(9) Uani 1 1 d . A 1 H24A H 0.6602 -0.3971 0.3686 0.065 Uiso 1 1 calc R A 1 C25A C 0.6973(4) -0.2879(3) 0.37591(19) 0.0837(14) Uani 1 1 d . A 1 H25D H 0.7873 -0.3018 0.3654 0.126 Uiso 1 1 calc R A 1 H25E H 0.6853 -0.2592 0.4053 0.126 Uiso 1 1 calc R A 1 H25F H 0.6496 -0.2494 0.3416 0.126 Uiso 1 1 calc R A 1 C26A C 0.7313(4) -0.4348(2) 0.45062(17) 0.0717(11) Uani 1 1 d . A 1 H26D H 0.8203 -0.4456 0.4379 0.108 Uiso 1 1 calc R A 1 H26E H 0.7038 -0.4892 0.4640 0.108 Uiso 1 1 calc R A 1 H26F H 0.7216 -0.4109 0.4824 0.108 Uiso 1 1 calc R A 1 C27A C 0.1885(3) -0.3445(2) 0.36529(15) 0.0550(9) Uani 1 1 d . A 1 H27A H 0.2317 -0.3664 0.3334 0.066 Uiso 1 1 calc R A 1 C28A C 0.1116(5) -0.4073(3) 0.4015(2) 0.1204(18) Uani 1 1 d . A 1 H28D H 0.0483 -0.4103 0.3774 0.181 Uiso 1 1 calc R A 1 H28E H 0.0689 -0.3878 0.4334 0.181 Uiso 1 1 calc R A 1 H28F H 0.1676 -0.4646 0.4171 0.181 Uiso 1 1 calc R A 1 C29A C 0.0998(4) -0.2580(3) 0.3379(2) 0.1026(17) Uani 1 1 d . A 1 H29D H 0.1488 -0.2170 0.3137 0.154 Uiso 1 1 calc R A 1 H29E H 0.0534 -0.2361 0.3682 0.154 Uiso 1 1 calc R A 1 H29F H 0.0399 -0.2648 0.3139 0.154 Uiso 1 1 calc R A 1 C1B C -0.0428(9) 0.0436(5) -0.0447(4) 0.220(3) Uiso 1 1 d D . 1 C2B C 0.1398(14) -0.0331(6) 0.0216(5) 0.220(3) Uiso 0.50 1 d PD . 1 C3B C 0.1747(9) 0.0129(5) -0.0318(4) 0.220(3) Uiso 1 1 d D C 1 C4B C 0.0732(11) 0.0628(9) -0.0652(7) 0.220(3) Uiso 0.50 1 d PD C 1 C5B C 0.0588(9) 0.0005(9) -0.0188(6) 0.220(3) Uiso 0.50 1 d PD . 1 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 Tm 0.02197(5) 0.02286(5) 0.02120(5) -0.00597(4) -0.00403(4) -0.00370(4) N1 0.0239(10) 0.0265(9) 0.0243(10) -0.0056(8) -0.0029(8) -0.0033(8) N2 0.0287(11) 0.0298(10) 0.0266(10) -0.0086(8) -0.0042(9) -0.0073(8) N3 0.0284(11) 0.0254(9) 0.0255(10) -0.0058(8) -0.0010(8) -0.0052(8) N4 0.0246(10) 0.0261(9) 0.0290(10) -0.0072(8) -0.0043(8) -0.0029(8) C1 0.0251(13) 0.0344(13) 0.0314(13) -0.0056(11) -0.0024(11) -0.0044(11) C2 0.0257(13) 0.0378(13) 0.0443(15) -0.0102(12) 0.0020(11) -0.0153(11) C3 0.0307(13) 0.0300(12) 0.0343(14) -0.0058(11) -0.0084(11) -0.0091(10) C4 0.0231(14) 0.0522(16) 0.0672(19) -0.0254(15) -0.0011(13) -0.0020(12) C5 0.0438(16) 0.0428(14) 0.078(2) -0.0239(15) -0.0072(15) -0.0195(13) C6 0.0231(12) 0.0260(11) 0.0370(13) -0.0112(10) -0.0061(10) 0.0011(10) C7 0.0320(14) 0.0288(12) 0.0371(14) -0.0070(11) -0.0076(11) -0.0012(11) C8 0.0433(16) 0.0243(12) 0.0468(16) -0.0044(12) -0.0085(13) -0.0016(11) C9 0.0472(17) 0.0258(12) 0.0562(17) -0.0163(12) -0.0076(14) 0.0013(12) C10 0.0438(17) 0.0354(13) 0.0461(16) -0.0199(12) -0.0013(13) 0.0022(12) C11 0.0311(14) 0.0314(13) 0.0369(14) -0.0116(11) -0.0035(11) 0.0004(11) C12 0.0551(18) 0.0299(13) 0.0344(14) -0.0040(11) -0.0084(13) -0.0065(12) C13 0.066(2) 0.0454(17) 0.0459(18) -0.0085(14) 0.0068(16) -0.0062(16) C14 0.073(2) 0.083(2) 0.0505(19) -0.0186(18) -0.0209(18) -0.011(2) C15 0.0496(17) 0.0351(13) 0.0337(14) -0.0143(11) 0.0014(13) -0.0036(12) C16 0.057(2) 0.0611(19) 0.0451(17) -0.0173(15) 0.0096(15) -0.0106(16) C17 0.059(2) 0.0499(17) 0.0431(17) -0.0082(14) -0.0071(15) -0.0019(15) C18 0.0428(15) 0.0427(13) 0.0360(14) -0.0224(11) 0.0033(12) -0.0186(12) C19 0.077(2) 0.0525(15) 0.0311(14) -0.0181(12) 0.0042(14) -0.0346(15) C20 0.111(3) 0.072(2) 0.0441(18) -0.0303(16) 0.0063(19) -0.038(2) C21 0.127(3) 0.092(2) 0.0526(19) -0.0519(17) 0.027(2) -0.043(2) C22 0.083(3) 0.078(2) 0.088(2) -0.0653(18) 0.012(2) -0.011(2) C23 0.0523(19) 0.0589(16) 0.0615(18) -0.0403(14) 0.0014(15) -0.0125(15) C24 0.084(2) 0.0537(17) 0.0317(15) -0.0063(13) -0.0171(15) -0.0229(17) C25 0.123(4) 0.073(2) 0.053(2) 0.0004(19) -0.009(2) -0.038(2) C26 0.082(3) 0.093(3) 0.092(3) 0.015(3) -0.036(2) -0.022(2) C27 0.067(2) 0.0682(19) 0.090(2) -0.0592(17) -0.0316(18) 0.0276(17) C28 0.087(3) 0.096(3) 0.084(3) 0.001(3) -0.021(3) 0.002(3) C29 0.064(3) 0.102(3) 0.157(4) -0.083(3) -0.036(3) 0.019(2) C30 0.0361(14) 0.0251(11) 0.0294(13) -0.0062(10) -0.0092(11) -0.0027(10) C31 0.0329(14) 0.0245(11) 0.0401(14) -0.0132(11) -0.0021(12) 0.0007(10) C32 0.0270(13) 0.0283(12) 0.0320(13) -0.0115(10) -0.0017(10) -0.0014(10) C33 0.065(2) 0.0248(13) 0.0492(18) -0.0040(13) 0.0019(16) -0.0042(13) C34 0.0257(15) 0.0349(15) 0.079(2) -0.0062(15) -0.0115(15) 0.0000(12) C35 0.0414(15) 0.0219(11) 0.0234(12) -0.0012(10) -0.0013(11) -0.0069(10) C36 0.0430(16) 0.0365(14) 0.0349(15) -0.0054(12) -0.0004(13) -0.0080(12) C37 0.0476(18) 0.0624(19) 0.0424(17) -0.0058(15) 0.0116(15) -0.0147(15) C38 0.072(2) 0.069(2) 0.0288(16) -0.0072(15) 0.0075(16) -0.0140(18) C39 0.070(2) 0.0519(17) 0.0253(14) -0.0055(13) -0.0059(14) -0.0138(16) C40 0.0475(16) 0.0331(13) 0.0258(13) -0.0042(11) -0.0055(12) -0.0083(12) C41 0.0436(17) 0.072(2) 0.0466(17) -0.0161(15) 0.0019(14) -0.0218(15) C42 0.098(3) 0.111(3) 0.237(5) -0.116(3) -0.058(4) -0.001(3) C43 0.0456(19) 0.077(2) 0.071(2) -0.0132(19) -0.0046(17) -0.0227(17) C44 0.0534(17) 0.0523(16) 0.0285(14) -0.0044(12) -0.0108(13) -0.0204(14) C45 0.086(2) 0.0632(19) 0.0562(19) -0.0127(16) -0.0282(18) -0.0299(18) C46 0.0433(19) 0.071(2) 0.082(3) -0.0153(19) -0.0131(18) -0.0119(17) C47 0.0208(12) 0.0287(12) 0.0332(13) -0.0063(10) -0.0027(10) -0.0045(10) C48 0.0284(14) 0.0436(14) 0.0366(14) -0.0102(12) 0.0011(11) -0.0071(11) C49 0.0441(17) 0.0565(17) 0.0374(16) -0.0065(14) 0.0080(13) -0.0178(14) C50 0.0519(18) 0.0471(16) 0.0481(18) -0.0009(14) 0.0055(15) -0.0244(14) C51 0.0401(15) 0.0320(13) 0.0553(18) -0.0112(13) 0.0033(14) -0.0141(12) C52 0.0257(13) 0.0299(12) 0.0416(15) -0.0085(11) 0.0003(11) -0.0049(10) C53 0.0491(17) 0.0626(17) 0.0439(16) -0.0300(13) 0.0160(13) -0.0244(14) C54 0.153(4) 0.097(3) 0.093(3) -0.042(2) -0.057(3) -0.021(3) C55 0.091(3) 0.110(3) 0.128(3) -0.090(2) -0.019(3) 0.016(3) C56 0.0368(15) 0.0359(13) 0.0480(15) -0.0210(12) 0.0076(12) -0.0135(11) C57 0.0453(19) 0.0613(19) 0.069(2) -0.0338(16) -0.0057(16) 0.0110(15) C58 0.061(2) 0.067(2) 0.0420(17) -0.0167(16) -0.0049(16) 0.0134(17) N1A 0.0319(11) 0.0259(10) 0.0270(10) -0.0063(8) -0.0038(9) -0.0041(8) N2A 0.0431(13) 0.0276(10) 0.0257(11) -0.0059(9) -0.0035(10) -0.0053(9) C1A 0.0246(12) 0.0314(12) 0.0339(13) -0.0125(10) -0.0057(10) -0.0053(10) C2A 0.0352(14) 0.0203(11) 0.0367(14) -0.0086(10) -0.0054(11) -0.0049(10) C3A 0.0396(14) 0.0267(12) 0.0333(14) -0.0032(11) -0.0078(12) -0.0091(11) C4A 0.0486(17) 0.0323(13) 0.0389(15) -0.0146(12) -0.0015(13) -0.0015(12) C5A 0.092(3) 0.0317(14) 0.0339(16) -0.0031(12) 0.0010(16) -0.0129(15) C6A 0.0366(14) 0.0252(11) 0.0233(12) -0.0086(10) -0.0003(11) -0.0001(10) C7A 0.0482(17) 0.0379(14) 0.0318(14) -0.0126(11) -0.0122(12) 0.0002(12) C8A 0.071(2) 0.0453(16) 0.0360(15) -0.0102(13) -0.0207(15) 0.0013(16) C9A 0.088(3) 0.0416(16) 0.0257(15) -0.0018(13) -0.0024(16) -0.0027(17) C10A 0.0566(19) 0.0397(15) 0.0404(16) -0.0048(13) 0.0089(15) -0.0081(14) C11A 0.0383(15) 0.0322(13) 0.0317(14) -0.0063(11) 0.0024(12) -0.0025(11) C12A 0.0481(17) 0.0514(17) 0.0580(18) -0.0143(15) -0.0255(15) -0.0066(14) C13A 0.055(2) 0.121(3) 0.132(4) -0.066(3) 0.008(2) -0.033(2) C14A 0.114(3) 0.098(3) 0.094(3) -0.035(2) -0.047(2) -0.040(2) C15A 0.0404(16) 0.0473(16) 0.0529(19) 0.0023(14) -0.0052(14) -0.0158(13) C16A 0.060(2) 0.081(2) 0.065(2) -0.0273(18) -0.0123(18) -0.0186(18) C17A 0.049(2) 0.065(2) 0.124(3) -0.032(2) -0.011(2) -0.0019(18) C18A 0.0480(16) 0.0248(12) 0.0224(12) -0.0026(10) 0.0010(11) -0.0066(11) C19A 0.0513(17) 0.0352(13) 0.0284(13) -0.0088(11) -0.0041(12) -0.0044(12) C20A 0.070(2) 0.0409(15) 0.0267(14) -0.0098(12) -0.0049(14) -0.0084(14) C21A 0.085(2) 0.0361(15) 0.0298(15) -0.0115(12) 0.0093(16) -0.0030(15) C22A 0.059(2) 0.0410(15) 0.0402(16) -0.0081(13) 0.0127(15) -0.0059(14) C23A 0.0517(17) 0.0316(13) 0.0335(15) -0.0020(12) 0.0029(13) -0.0111(12) C24A 0.0509(19) 0.0725(19) 0.0473(17) -0.0306(15) -0.0071(14) -0.0093(16) C25A 0.057(2) 0.095(3) 0.077(3) 0.001(2) 0.002(2) -0.021(2) C26A 0.060(2) 0.067(2) 0.082(3) -0.025(2) -0.018(2) 0.0038(18) C27A 0.0441(18) 0.0665(19) 0.0528(19) -0.0185(16) 0.0028(15) -0.0128(15) C28A 0.136(3) 0.126(3) 0.109(4) 0.003(3) -0.023(3) -0.095(3) C29A 0.075(3) 0.080(3) 0.138(4) -0.003(3) -0.050(3) -0.016(2) _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 Tm N4 2.161(2) . ? Tm N3 2.2066(19) . ? Tm N1 2.2727(18) . ? Tm N2 2.301(2) . ? N1 C1 1.318(3) . ? N1 C6 1.456(3) . ? N2 C3 1.344(3) . ? N2 C18 1.443(3) . ? N3 C30 1.402(3) . ? N3 C35 1.428(3) . ? N4 C32 1.400(3) . ? N4 C47 1.436(3) . ? C1 C2 1.428(4) . ? C1 C4 1.503(4) . ? C2 C3 1.385(4) . ? C3 C5 1.525(4) . ? C6 C7 1.400(3) . ? C6 C11 1.403(4) . ? C7 C8 1.396(4) . ? C7 C12 1.520(4) . ? C8 C9 1.369(4) . ? C9 C10 1.378(4) . ? C10 C11 1.396(4) . ? C11 C15 1.522(4) . ? C12 C13 1.529(4) . ? C12 C14 1.531(4) . ? C15 C17 1.535(4) . ? C15 C16 1.535(4) . ? C18 C23 1.406(4) . ? C18 C19 1.413(4) . ? C19 C20 1.382(5) . ? C19 C24 1.520(4) . ? C20 C21 1.376(5) . ? C21 C22 1.389(5) . ? C22 C23 1.405(5) . ? C23 C27 1.527(5) . ? C24 C25 1.523(5) . ? C24 C26 1.547(6) . ? C27 C29 1.521(5) . ? C27 C28 1.529(6) . ? C30 C31 1.350(4) . ? C30 C33 1.525(3) . ? C31 C32 1.494(3) . ? C32 C34 1.330(4) . ? C35 C36 1.407(4) . ? C35 C40 1.416(4) . ? C36 C37 1.398(4) . ? C36 C41 1.513(4) . ? C37 C38 1.374(5) . ? C38 C39 1.368(5) . ? C39 C40 1.390(4) . ? C40 C44 1.517(4) . ? C41 C43 1.522(5) . ? C41 C42 1.523(5) . ? C44 C46 1.528(4) . ? C44 C45 1.532(5) . ? C47 C48 1.407(4) . ? C47 C52 1.412(4) . ? C48 C49 1.391(4) . ? C48 C53 1.520(4) . ? C49 C50 1.374(5) . ? C50 C51 1.372(4) . ? C51 C52 1.387(4) . ? C52 C56 1.520(4) . ? C53 C54 1.479(5) . ? C53 C55 1.512(5) . ? C56 C57 1.517(4) . ? C56 C58 1.526(4) . ? N1A C1A 1.328(3) . ? N1A C6A 1.425(3) . ? N2A C3A 1.334(3) . ? N2A C18A 1.426(3) . ? C1A C2A 1.402(3) . ? C1A C4A 1.508(4) . ? C2A C3A 1.387(4) . ? C3A C5A 1.506(4) . ? C6A C11A 1.392(4) . ? C6A C7A 1.411(4) . ? C7A C8A 1.393(4) . ? C7A C12A 1.509(4) . ? C8A C9A 1.375(5) . ? C9A C10A 1.366(5) . ? C10A C11A 1.395(4) . ? C11A C15A 1.520(4) . ? C12A C14A 1.523(5) . ? C12A C13A 1.524(5) . ? C15A C17A 1.531(5) . ? C15A C16A 1.536(5) . ? C18A C23A 1.400(4) . ? C18A C19A 1.402(4) . ? C19A C20A 1.394(4) . ? C19A C24A 1.512(4) . ? C20A C21A 1.379(5) . ? C21A C22A 1.380(5) . ? C22A C23A 1.392(4) . ? C23A C27A 1.516(5) . ? C24A C25A 1.519(5) . ? C24A C26A 1.535(5) . ? C27A C28A 1.511(5) . ? C27A C29A 1.514(5) . ? C1B C2B 1.173(17) 2 ? C1B C5B 1.264(10) . ? C1B C4B 1.389(12) . ? C1B C5B 1.497(16) 2 ? C2B C1B 1.173(17) 2 ? C2B C3B 1.350(12) . ? C3B C5B 1.325(12) . ? C3B C4B 1.369(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Tm N3 96.36(7) . . ? N4 Tm N1 113.87(7) . . ? N3 Tm N1 114.03(7) . . ? N4 Tm N2 116.56(8) . . ? N3 Tm N2 129.77(7) . . ? N1 Tm N2 87.23(7) . . ? C1 N1 C6 118.2(2) . . ? C1 N1 Tm 110.14(15) . . ? C6 N1 Tm 130.38(15) . . ? C3 N2 C18 116.8(2) . . ? C3 N2 Tm 103.00(16) . . ? C18 N2 Tm 138.45(17) . . ? C30 N3 C35 116.13(19) . . ? C30 N3 Tm 95.11(14) . . ? C35 N3 Tm 148.14(16) . . ? C32 N4 C47 115.3(2) . . ? C32 N4 Tm 107.63(15) . . ? C47 N4 Tm 136.71(15) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 C4 122.1(2) . . ? C2 C1 C4 114.7(2) . . ? C3 C2 C1 132.3(2) . . ? N2 C3 C2 125.4(2) . . ? N2 C3 C5 120.6(2) . . ? C2 C3 C5 113.9(2) . . ? C7 C6 C11 121.5(2) . . ? C7 C6 N1 118.2(2) . . ? C11 C6 N1 120.3(2) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 C12 119.3(2) . . ? C6 C7 C12 122.5(2) . . ? C9 C8 C7 121.0(3) . . ? C8 C9 C10 120.5(3) . . ? C9 C10 C11 121.0(3) . . ? C10 C11 C6 117.9(2) . . ? C10 C11 C15 119.1(2) . . ? C6 C11 C15 123.0(2) . . ? C7 C12 C13 111.6(3) . . ? C7 C12 C14 110.2(3) . . ? C13 C12 C14 111.0(3) . . ? C11 C15 C17 111.4(3) . . ? C11 C15 C16 112.2(2) . . ? C17 C15 C16 109.2(3) . . ? C23 C18 C19 121.0(3) . . ? C23 C18 N2 120.7(2) . . ? C19 C18 N2 118.3(2) . . ? C20 C19 C18 119.0(3) . . ? C20 C19 C24 118.1(3) . . ? C18 C19 C24 122.9(3) . . ? C21 C20 C19 121.0(3) . . ? C20 C21 C22 120.0(3) . . ? C21 C22 C23 121.4(3) . . ? C22 C23 C18 117.5(3) . . ? C22 C23 C27 119.1(3) . . ? C18 C23 C27 123.2(3) . . ? C19 C24 C25 113.6(3) . . ? C19 C24 C26 113.0(3) . . ? C25 C24 C26 108.0(3) . . ? C29 C27 C23 111.4(3) . . ? C29 C27 C28 110.5(3) . . ? C23 C27 C28 111.9(3) . . ? C31 C30 N3 124.2(2) . . ? C31 C30 C33 118.6(2) . . ? N3 C30 C33 116.9(2) . . ? C31 C30 Tm 80.48(14) . . ? N3 C30 Tm 53.98(11) . . ? C33 C30 Tm 138.2(2) . . ? C30 C31 C32 133.5(2) . . ? C30 C31 Tm 71.43(14) . . ? C32 C31 Tm 77.93(13) . . ? C34 C32 N4 125.6(2) . . ? C34 C32 C31 117.3(2) . . ? N4 C32 C31 116.9(2) . . ? C36 C35 C40 119.7(2) . . ? C36 C35 N3 121.3(2) . . ? C40 C35 N3 119.0(2) . . ? C37 C36 C35 118.6(3) . . ? C37 C36 C41 119.0(3) . . ? C35 C36 C41 122.4(3) . . ? C38 C37 C36 121.8(3) . . ? C39 C38 C37 119.1(3) . . ? C38 C39 C40 122.2(3) . . ? C39 C40 C35 118.5(3) . . ? C39 C40 C44 118.8(3) . . ? C35 C40 C44 122.7(2) . . ? C36 C41 C43 114.1(3) . . ? C36 C41 C42 111.1(3) . . ? C43 C41 C42 109.3(3) . . ? C40 C44 C46 112.4(2) . . ? C40 C44 C45 112.0(3) . . ? C46 C44 C45 108.5(3) . . ? C48 C47 C52 120.3(2) . . ? C48 C47 N4 119.2(2) . . ? C52 C47 N4 120.5(2) . . ? C49 C48 C47 118.4(3) . . ? C49 C48 C53 119.4(3) . . ? C47 C48 C53 122.2(2) . . ? C50 C49 C48 121.6(3) . . ? C51 C50 C49 119.7(3) . . ? C50 C51 C52 121.6(3) . . ? C51 C52 C47 118.4(3) . . ? C51 C52 C56 119.4(3) . . ? C47 C52 C56 122.2(2) . . ? C54 C53 C55 110.7(3) . . ? C54 C53 C48 113.8(3) . . ? C55 C53 C48 112.5(3) . . ? C57 C56 C52 112.5(2) . . ? C57 C56 C58 109.4(3) . . ? C52 C56 C58 111.8(2) . . ? C1A N1A C6A 123.0(2) . . ? C3A N2A C18A 123.7(2) . . ? N1A C1A C2A 120.9(2) . . ? N1A C1A C4A 120.3(2) . . ? C2A C1A C4A 118.8(2) . . ? C3A C2A C1A 125.5(2) . . ? N2A C3A C2A 121.3(2) . . ? N2A C3A C5A 119.4(2) . . ? C2A C3A C5A 119.4(2) . . ? C11A C6A C7A 121.1(2) . . ? C11A C6A N1A 119.6(2) . . ? C7A C6A N1A 119.1(2) . . ? C8A C7A C6A 117.6(3) . . ? C8A C7A C12A 121.4(3) . . ? C6A C7A C12A 121.0(2) . . ? C9A C8A C7A 121.5(3) . . ? C10A C9A C8A 120.3(3) . . ? C9A C10A C11A 120.9(3) . . ? C6A C11A C10A 118.7(3) . . ? C6A C11A C15A 121.9(2) . . ? C10A C11A C15A 119.4(3) . . ? C7A C12A C14A 114.1(3) . . ? C7A C12A C13A 110.6(3) . . ? C14A C12A C13A 110.9(3) . . ? C11A C15A C17A 111.1(3) . . ? C11A C15A C16A 112.0(2) . . ? C17A C15A C16A 110.1(3) . . ? C23A C18A C19A 121.5(3) . . ? C23A C18A N2A 119.4(3) . . ? C19A C18A N2A 119.0(2) . . ? C20A C19A C18A 117.9(3) . . ? C20A C19A C24A 119.8(3) . . ? C18A C19A C24A 122.2(3) . . ? C21A C20A C19A 121.2(3) . . ? C20A C21A C22A 120.2(3) . . ? C21A C22A C23A 120.7(3) . . ? C22A C23A C18A 118.4(3) . . ? C22A C23A C27A 119.7(3) . . ? C18A C23A C27A 121.9(3) . . ? C19A C24A C25A 110.5(3) . . ? C19A C24A C26A 112.5(3) . . ? C25A C24A C26A 110.3(3) . . ? C28A C27A C29A 108.9(3) . . ? C28A C27A C23A 112.1(3) . . ? C29A C27A C23A 112.4(3) . . ? C2B C1B C5B 119.3(11) 2 . ? C4B C1B C5B 118.1(10) . 2 ? C1B C2B C3B 134.5(13) 2 . ? C2B C3B C4B 112.5(11) . . ? C3B C4B C1B 115.8(11) . . ? C1B C5B C3B 128.9(13) . . ? C1B C5B C1B 114.8(10) . 2 ? C3B C5B C1B 111.0(10) . 2 ? #===END data_(2b)-jun2804 _database_code_depnum_ccdc_archive 'CCDC 254750' _audit_creation_date 2004-06-28T11:50:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C58 H82 N4 Tm1) (C24 B1 F20)' _chemical_formula_sum 'C82 H82 B1 F20 N4 Tm1' _chemical_formula_weight 1683.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 27.9702(3) _cell_length_b 19.9944(3) _cell_length_c 27.9170(4) _cell_angle_alpha 90 _cell_angle_beta 98.971(1) _cell_angle_gamma 90 _cell_volume 15421.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 294752 _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 'light yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6848 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.245 _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 0.7606 _exptl_absorpt_correction_T_max 0.8785 #----------------------------------------------------------------------------# # 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 0.361826E-1 _diffrn_orient_matrix_ub_12 0.838E-4 _diffrn_orient_matrix_ub_13 0.80267E-2 _diffrn_orient_matrix_ub_21 -0.00243 _diffrn_orient_matrix_ub_22 0.7483E-3 _diffrn_orient_matrix_ub_23 0.352897E-1 _diffrn_orient_matrix_ub_31 0.242E-4 _diffrn_orient_matrix_ub_32 -0.500083E-1 _diffrn_orient_matrix_ub_33 0.5415E-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 0.0746 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_number 112592 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 26992 _reflns_number_gt 20129 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+97.3853P] 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 26992 _refine_ls_number_parameters 1953 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.07 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 1.233 _refine_ls_restrained_S_all 1.233 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.579 _refine_diff_density_min -1.498 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Tm Tm -0.3139 5.2483 '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 Tm Tm 0.414389(12) 0.298547(18) 0.346327(12) 0.03758(10) Uani 1 1 d . . . N1 N 0.4437(3) 0.3060(4) 0.2773(3) 0.058(2) Uani 1 1 d . . . N2 N 0.3412(2) 0.3226(5) 0.3064(3) 0.065(2) Uani 1 1 d . . . N3 N 0.4481(2) 0.3652(3) 0.4061(2) 0.0458(17) Uani 1 1 d . . . N4 N 0.4265(3) 0.2167(3) 0.4022(3) 0.0496(18) Uani 1 1 d . . . C1 C 0.4172(4) 0.2581(6) 0.2486(4) 0.079(3) Uani 1 1 d . . . C2 C 0.3680(4) 0.2458(7) 0.2493(4) 0.093(4) Uani 1 1 d . . . H2 H 0.3568 0.2044 0.235 0.111 Uiso 1 1 calc R . . C3 C 0.3313(3) 0.2842(7) 0.2676(4) 0.078(3) Uani 1 1 d . . . C4 C 0.4431(5) 0.2132(6) 0.2174(4) 0.105(5) Uani 1 1 d . . . H4A H 0.4755 0.2312 0.216 0.158 Uiso 1 1 calc R . . H4B H 0.4246 0.2112 0.1846 0.158 Uiso 1 1 calc R . . H4C H 0.446 0.1681 0.2314 0.158 Uiso 1 1 calc R . . C5 C 0.2811(4) 0.2747(8) 0.2409(4) 0.125(6) Uani 1 1 d . . . H5A H 0.259 0.3055 0.2537 0.188 Uiso 1 1 calc R . . H5B H 0.2706 0.2285 0.2451 0.188 Uiso 1 1 calc R . . H5C H 0.2807 0.2837 0.2063 0.188 Uiso 1 1 calc R . . C6 C 0.4844(4) 0.3308(5) 0.2566(3) 0.058(2) Uani 1 1 d . . . C7 C 0.5307(4) 0.3150(5) 0.2793(4) 0.066(3) Uani 1 1 d . . . C8 C 0.5687(4) 0.3371(5) 0.2540(4) 0.076(3) Uani 1 1 d . . . H8 H 0.6013 0.3269 0.2673 0.092 Uiso 1 1 calc R . . C9 C 0.5599(5) 0.3723(6) 0.2114(4) 0.080(3) Uani 1 1 d . . . H9 H 0.5861 0.3848 0.1952 0.097 Uiso 1 1 calc R . . C10 C 0.5157(5) 0.3885(6) 0.1930(4) 0.084(3) Uani 1 1 d . . . H10 H 0.5104 0.4136 0.1638 0.1 Uiso 1 1 calc R . . C11 C 0.4759(4) 0.3704(6) 0.2148(3) 0.071(3) Uani 1 1 d . . . C12 C 0.5421(4) 0.2761(6) 0.3266(4) 0.080(3) Uani 1 1 d . . . H12 H 0.5129 0.28 0.343 0.096 Uiso 1 1 calc R . . C13 C 0.5496(7) 0.2044(8) 0.3193(5) 0.146(7) Uani 1 1 d . . . H13A H 0.5566 0.182 0.3508 0.219 Uiso 1 1 calc R . . H13B H 0.577 0.1981 0.3016 0.219 Uiso 1 1 calc R . . H13C H 0.5203 0.1851 0.3005 0.219 Uiso 1 1 calc R . . C14 C 0.5845(4) 0.3076(10) 0.3613(5) 0.142(7) Uani 1 1 d . . . H14A H 0.578 0.3552 0.3656 0.213 Uiso 1 1 calc R . . H14B H 0.6145 0.3026 0.3476 0.213 Uiso 1 1 calc R . . H14C H 0.5879 0.285 0.3928 0.213 Uiso 1 1 calc R . . C15 C 0.4268(4) 0.3966(7) 0.1940(4) 0.093(4) Uani 1 1 d . . . H15 H 0.4062 0.3926 0.2201 0.112 Uiso 1 1 calc R . . C16 C 0.4279(5) 0.4734(8) 0.1806(5) 0.131(6) Uani 1 1 d . . . H16A H 0.395 0.4885 0.1677 0.197 Uiso 1 1 calc R . . H16B H 0.4489 0.48 0.156 0.197 Uiso 1 1 calc R . . H16C H 0.4404 0.4992 0.2097 0.197 Uiso 1 1 calc R . . C17 C 0.4013(5) 0.3548(10) 0.1499(5) 0.162(8) Uani 1 1 d . . . H17A H 0.3694 0.374 0.1382 0.243 Uiso 1 1 calc R . . H17B H 0.3975 0.3085 0.1601 0.243 Uiso 1 1 calc R . . H17C H 0.4211 0.3558 0.1239 0.243 Uiso 1 1 calc R . . C18 C 0.3030(3) 0.3622(7) 0.3225(4) 0.088(4) Uani 1 1 d . . . C19 C 0.3011(4) 0.4315(7) 0.3120(5) 0.109(5) Uani 1 1 d . . . C20 C 0.2657(7) 0.4701(11) 0.3295(6) 0.221(13) Uani 1 1 d . . . H20 H 0.2647 0.5172 0.3246 0.265 Uiso 1 1 calc R . . C21 C 0.2318(8) 0.4387(14) 0.3541(9) 0.296(19) Uani 1 1 d . . . H21 H 0.2065 0.4642 0.3642 0.355 Uiso 1 1 calc R . . C22 C 0.2350(6) 0.3706(12) 0.3640(7) 0.227(14) Uani 1 1 d . . . H22 H 0.2121 0.3503 0.3812 0.273 Uiso 1 1 calc R . . C23 C 0.2706(4) 0.3324(9) 0.3494(5) 0.124(6) Uani 1 1 d . . . C24 C 0.3334(5) 0.4624(7) 0.2788(4) 0.095(4) Uani 1 1 d . . . H24 H 0.3642 0.4362 0.2823 0.114 Uiso 1 1 calc R . . C25 C 0.3068(5) 0.4543(9) 0.2257(5) 0.139(7) Uani 1 1 d . . . H25A H 0.3267 0.4736 0.2032 0.209 Uiso 1 1 calc R . . H25B H 0.2756 0.4776 0.222 0.209 Uiso 1 1 calc R . . H25C H 0.3014 0.4067 0.2184 0.209 Uiso 1 1 calc R . . C26 C 0.3462(5) 0.5358(8) 0.2919(6) 0.131(6) Uani 1 1 d . . . H26A H 0.3671 0.5535 0.2697 0.196 Uiso 1 1 calc R . . H26B H 0.3632 0.5383 0.3253 0.196 Uiso 1 1 calc R . . H26C H 0.3165 0.5624 0.2889 0.196 Uiso 1 1 calc R . . C27 C 0.2716(4) 0.2573(8) 0.3607(5) 0.110(5) Uani 1 1 d . . . H27 H 0.2978 0.236 0.3454 0.133 Uiso 1 1 calc R . . C28 C 0.2824(4) 0.2457(7) 0.4155(4) 0.100(4) Uani 1 1 d . . . H28A H 0.2833 0.1976 0.4222 0.15 Uiso 1 1 calc R . . H28B H 0.257 0.2666 0.431 0.15 Uiso 1 1 calc R . . H28C H 0.3138 0.2656 0.4284 0.15 Uiso 1 1 calc R . . C29 C 0.2242(6) 0.2217(11) 0.3426(6) 0.219(12) Uani 1 1 d . . . H29A H 0.2275 0.1741 0.3506 0.329 Uiso 1 1 calc R . . H29B H 0.2162 0.2269 0.3073 0.329 Uiso 1 1 calc R . . H29C H 0.1983 0.2411 0.3581 0.329 Uiso 1 1 calc R . . C30 C 0.4735(4) 0.2180(5) 0.4250(3) 0.060(3) Uani 1 1 d . . . C31 C 0.5001(3) 0.2763(5) 0.4351(3) 0.063(3) Uani 1 1 d . . . H31 H 0.5337 0.269 0.4453 0.075 Uiso 1 1 calc R . . C32 C 0.4873(3) 0.3413(5) 0.4332(3) 0.060(2) Uani 1 1 d . . . C33 C 0.4982(4) 0.1508(5) 0.4394(4) 0.095(4) Uani 1 1 d . . . H33A H 0.4734 0.1166 0.4414 0.142 Uiso 1 1 calc R . . H33B H 0.5188 0.1553 0.471 0.142 Uiso 1 1 calc R . . H33C H 0.518 0.1376 0.415 0.142 Uiso 1 1 calc R . . C34 C 0.5225(4) 0.3879(7) 0.4668(4) 0.101(4) Uani 1 1 d . . . H34A H 0.5555 0.3814 0.4601 0.152 Uiso 1 1 calc R . . H34B H 0.5212 0.3768 0.5008 0.152 Uiso 1 1 calc R . . H34C H 0.5129 0.4346 0.4607 0.152 Uiso 1 1 calc R . . C35 C 0.4365(4) 0.4370(5) 0.4101(3) 0.058(2) Uani 1 1 d . . . C36 C 0.4009(4) 0.4526(5) 0.4373(4) 0.071(3) Uani 1 1 d . . . C37 C 0.3896(5) 0.5198(6) 0.4419(5) 0.103(4) Uani 1 1 d . . . H37 H 0.3655 0.5326 0.4606 0.124 Uiso 1 1 calc R . . C38 C 0.4133(6) 0.5669(6) 0.4195(5) 0.117(5) Uani 1 1 d . . . H38 H 0.4057 0.6127 0.4237 0.141 Uiso 1 1 calc R . . C39 C 0.4463(5) 0.5518(5) 0.3923(4) 0.091(4) Uani 1 1 d . . . H39 H 0.4607 0.5864 0.3761 0.109 Uiso 1 1 calc R . . C40 C 0.4602(4) 0.4860(5) 0.3872(4) 0.067(3) Uani 1 1 d . . . C41 C 0.3781(4) 0.3999(6) 0.4665(4) 0.084(3) Uani 1 1 d . . . H41 H 0.3787 0.3565 0.4487 0.101 Uiso 1 1 calc R . . C42 C 0.3242(6) 0.4149(7) 0.4703(7) 0.177(9) Uani 1 1 d . . . H42A H 0.3115 0.3794 0.4891 0.265 Uiso 1 1 calc R . . H42B H 0.3052 0.4166 0.4377 0.265 Uiso 1 1 calc R . . H42C H 0.3219 0.4579 0.4865 0.265 Uiso 1 1 calc R . . C43 C 0.4069(8) 0.3899(8) 0.5161(4) 0.169(9) Uani 1 1 d . . . H43A H 0.3913 0.3558 0.5335 0.253 Uiso 1 1 calc R . . H43B H 0.4085 0.4321 0.5341 0.253 Uiso 1 1 calc R . . H43C H 0.4398 0.3753 0.5129 0.253 Uiso 1 1 calc R . . C44 C 0.4993(4) 0.4703(6) 0.3555(4) 0.075(3) Uani 1 1 d . . . H44 H 0.5051 0.4209 0.3569 0.09 Uiso 1 1 calc R . . C45 C 0.5481(5) 0.5054(8) 0.3728(6) 0.145(7) Uani 1 1 d . . . H45A H 0.56 0.4925 0.4065 0.217 Uiso 1 1 calc R . . H45B H 0.5436 0.5539 0.3709 0.217 Uiso 1 1 calc R . . H45C H 0.5717 0.4918 0.3521 0.217 Uiso 1 1 calc R . . C46 C 0.4820(5) 0.4890(6) 0.3028(4) 0.100(4) Uani 1 1 d . . . H46A H 0.5073 0.478 0.2833 0.151 Uiso 1 1 calc R . . H46B H 0.4752 0.5371 0.3005 0.151 Uiso 1 1 calc R . . H46C H 0.4525 0.464 0.2906 0.151 Uiso 1 1 calc R . . C47 C 0.3968(3) 0.1593(4) 0.4121(3) 0.056(2) Uani 1 1 d . . . C48 C 0.3820(3) 0.1548(4) 0.4583(3) 0.054(2) Uani 1 1 d . . . C49 C 0.3526(3) 0.1000(5) 0.4665(4) 0.069(3) Uani 1 1 d . . . H49 H 0.3433 0.0943 0.4975 0.083 Uiso 1 1 calc R . . C50 C 0.3373(4) 0.0548(5) 0.4306(4) 0.074(3) Uani 1 1 d . . . H50 H 0.3151 0.0205 0.4357 0.089 Uiso 1 1 calc R . . C51 C 0.3540(4) 0.0595(5) 0.3883(4) 0.078(3) Uani 1 1 d . . . H51 H 0.3453 0.0255 0.3647 0.093 Uiso 1 1 calc R . . C52 C 0.3831(4) 0.1114(5) 0.3772(4) 0.067(3) Uani 1 1 d . . . C53 C 0.3961(4) 0.2054(6) 0.4983(3) 0.069(3) Uani 1 1 d . . . H53 H 0.4036 0.2486 0.4831 0.083 Uiso 1 1 calc R . . C54 C 0.4416(4) 0.1834(8) 0.5335(4) 0.107(5) Uani 1 1 d . . . H54A H 0.4499 0.2177 0.5585 0.16 Uiso 1 1 calc R . . H54B H 0.4687 0.1775 0.5155 0.16 Uiso 1 1 calc R . . H54C H 0.4351 0.141 0.5489 0.16 Uiso 1 1 calc R . . C55 C 0.3569(4) 0.2181(6) 0.5287(4) 0.083(3) Uani 1 1 d . . . H55A H 0.3682 0.2516 0.5536 0.125 Uiso 1 1 calc R . . H55B H 0.3493 0.1764 0.5443 0.125 Uiso 1 1 calc R . . H55C H 0.3279 0.2347 0.508 0.125 Uiso 1 1 calc R . . C56 C 0.4018(4) 0.1140(6) 0.3286(4) 0.087(4) Uani 1 1 d . . . H56 H 0.4129 0.1603 0.3223 0.105 Uiso 1 1 calc R . . C57 C 0.4464(6) 0.0622(8) 0.3323(6) 0.149(7) Uani 1 1 d . . . H57A H 0.4601 0.0633 0.302 0.224 Uiso 1 1 calc R . . H57B H 0.4348 0.0169 0.3376 0.224 Uiso 1 1 calc R . . H57C H 0.4713 0.0749 0.3594 0.224 Uiso 1 1 calc R . . C58 C 0.3635(7) 0.0910(8) 0.2870(4) 0.169(9) Uani 1 1 d . . . H58A H 0.3764 0.0941 0.2564 0.253 Uiso 1 1 calc R . . H58B H 0.3348 0.1196 0.2854 0.253 Uiso 1 1 calc R . . H58C H 0.3546 0.0446 0.2925 0.253 Uiso 1 1 calc R . . F1A F 0.1520(2) 0.2388(3) 0.47049(19) 0.0842(18) Uani 1 1 d . . . F2A F 0.1845(3) 0.1265(3) 0.4367(2) 0.102(2) Uani 1 1 d . . . F3A F 0.2470(2) 0.0447(3) 0.4953(2) 0.090(2) Uani 1 1 d . . . F4A F 0.27631(19) 0.0789(3) 0.5891(2) 0.0744(16) Uani 1 1 d . . . F5A F 0.24191(18) 0.1888(3) 0.62547(18) 0.0669(14) Uani 1 1 d . . . F6A F 0.18256(16) 0.2620(3) 0.68863(16) 0.0560(12) Uani 1 1 d . . . F7A F 0.1228(2) 0.1902(3) 0.73227(18) 0.0697(15) Uani 1 1 d . . . F8A F 0.0436(2) 0.1314(3) 0.6816(2) 0.0800(17) Uani 1 1 d . . . F9A F 0.0255(2) 0.1464(3) 0.5823(2) 0.0857(18) Uani 1 1 d . . . F10A F 0.08683(19) 0.2131(3) 0.53730(18) 0.0724(16) Uani 1 1 d . . . F11A F 0.06883(18) 0.3420(3) 0.56939(18) 0.0666(14) Uani 1 1 d . . . F12A F 0.0308(2) 0.4341(3) 0.5083(2) 0.0894(19) Uani 1 1 d . . . F13A F 0.0826(3) 0.4893(3) 0.4431(2) 0.114(2) Uani 1 1 d . . . F14A F 0.1757(3) 0.4467(4) 0.4419(3) 0.125(3) Uani 1 1 d . . . F15A F 0.2138(2) 0.3518(3) 0.5022(2) 0.0886(19) Uani 1 1 d . . . F16A F 0.28323(19) 0.2956(3) 0.5796(2) 0.0843(18) Uani 1 1 d . . . F17A F 0.3404(2) 0.3830(4) 0.6313(3) 0.104(2) Uani 1 1 d . . . F18A F 0.3048(2) 0.4715(3) 0.6907(2) 0.102(2) Uani 1 1 d . . . F19A F 0.2094(2) 0.4669(3) 0.7001(2) 0.0826(18) Uani 1 1 d . . . F20A F 0.15039(18) 0.3814(3) 0.64658(17) 0.0616(14) Uani 1 1 d . . . C1A C 0.1959(3) 0.2211(4) 0.5499(3) 0.052(2) Uani 1 1 d . . . C2A C 0.1834(4) 0.2012(5) 0.5028(3) 0.063(3) Uani 1 1 d . . . C3A C 0.1985(5) 0.1439(6) 0.4827(4) 0.078(3) Uani 1 1 d . . . C4A C 0.2312(4) 0.1027(5) 0.5130(4) 0.067(3) Uani 1 1 d . . . C5A C 0.2452(3) 0.1200(5) 0.5596(4) 0.059(2) Uani 1 1 d . . . C6A C 0.2272(3) 0.1759(5) 0.5772(3) 0.055(2) Uani 1 1 d . . . C7A C 0.1368(3) 0.2450(4) 0.6099(3) 0.045(2) Uani 1 1 d . . . C8A C 0.1441(3) 0.2351(5) 0.6598(3) 0.050(2) Uani 1 1 d . . . C9A C 0.1128(3) 0.1965(5) 0.6833(3) 0.055(2) Uani 1 1 d . . . C10A C 0.0735(3) 0.1669(5) 0.6578(4) 0.056(2) Uani 1 1 d . . . C11A C 0.0644(3) 0.1755(5) 0.6091(4) 0.064(3) Uani 1 1 d . . . C12A C 0.0966(3) 0.2107(5) 0.5871(3) 0.053(2) Uani 1 1 d . . . C13A C 0.1440(3) 0.3396(5) 0.5391(3) 0.051(2) Uani 1 1 d . . . C14A C 0.0979(3) 0.3645(5) 0.5386(3) 0.056(2) Uani 1 1 d . . . C15A C 0.0766(4) 0.4149(5) 0.5061(3) 0.064(3) Uani 1 1 d . . . C16A C 0.1017(5) 0.4412(6) 0.4743(4) 0.081(3) Uani 1 1 d . . . C17A C 0.1486(6) 0.4207(6) 0.4740(4) 0.087(4) Uani 1 1 d . . . C18A C 0.1674(4) 0.3696(5) 0.5051(4) 0.065(3) Uani 1 1 d . . . C19A C 0.2131(3) 0.3323(5) 0.6112(3) 0.053(2) Uani 1 1 d . . . C20A C 0.2621(3) 0.3374(6) 0.6089(4) 0.069(3) Uani 1 1 d . . . C21A C 0.2933(3) 0.3812(5) 0.6357(4) 0.069(3) Uani 1 1 d . . . C22A C 0.2752(4) 0.4260(5) 0.6665(4) 0.073(3) Uani 1 1 d . . . C23A C 0.2276(4) 0.4235(5) 0.6699(3) 0.067(3) Uani 1 1 d . . . C24A C 0.1981(3) 0.3785(5) 0.6426(3) 0.051(2) Uani 1 1 d . . . B1A B 0.1729(4) 0.2841(6) 0.5776(3) 0.052(3) Uani 1 1 d . . . Tm1X Tm 0.097737(12) 0.738048(19) 0.170717(12) 0.04089(11) Uani 1 1 d . A 1 N1X N 0.1559(2) 0.8149(3) 0.1707(2) 0.0405(15) Uani 1 1 d . A 1 N2X N 0.1548(2) 0.6623(3) 0.1973(2) 0.0406(15) Uani 1 1 d . A 1 N3X N 0.0526(2) 0.7178(4) 0.0992(2) 0.0502(18) Uani 1 1 d . A 1 N4X N 0.0301(2) 0.7424(4) 0.2037(2) 0.0552(19) Uani 1 1 d . A 1 C1X C 0.1763(3) 0.8145(4) 0.2184(3) 0.0415(19) Uani 1 1 d . A 1 C2X C 0.1840(3) 0.7579(4) 0.2470(3) 0.0441(19) Uani 1 1 d . A 1 H2X H 0.1914 0.7671 0.2807 0.053 Uiso 1 1 calc R A 1 C3X C 0.1830(3) 0.6883(4) 0.2355(3) 0.044(2) Uani 1 1 d . A 1 C4X C 0.1926(3) 0.8801(4) 0.2434(3) 0.057(2) Uani 1 1 d . A 1 H4X1 H 0.1936 0.915 0.2189 0.086 Uiso 1 1 calc R A 1 H4X2 H 0.2249 0.8745 0.2623 0.086 Uiso 1 1 calc R A 1 H4X3 H 0.1698 0.8931 0.265 0.086 Uiso 1 1 calc R A 1 C5X C 0.2163(3) 0.6458(5) 0.2712(3) 0.061(2) Uani 1 1 d . A 1 H5X1 H 0.2124 0.5987 0.2619 0.091 Uiso 1 1 calc R A 1 H5X2 H 0.2082 0.6519 0.3038 0.091 Uiso 1 1 calc R A 1 H5X3 H 0.2499 0.6595 0.271 0.091 Uiso 1 1 calc R A 1 C6X C 0.1695(3) 0.8685(4) 0.1408(3) 0.050(2) Uani 1 1 d . A 1 C7X C 0.1364(3) 0.9200(4) 0.1227(3) 0.053(2) Uani 1 1 d . A 1 C8X C 0.1523(4) 0.9680(5) 0.0935(3) 0.065(3) Uani 1 1 d . A 1 H8X H 0.1304 1.0019 0.0802 0.078 Uiso 1 1 calc R A 1 C9X C 0.1986(4) 0.9690(5) 0.0828(3) 0.069(3) Uani 1 1 d . A 1 H9X H 0.2085 1.003 0.0627 0.083 Uiso 1 1 calc R A 1 C10X C 0.2300(4) 0.9205(5) 0.1014(3) 0.061(3) Uani 1 1 d . A 1 H10X H 0.2623 0.9221 0.0948 0.074 Uiso 1 1 calc R A 1 C11X C 0.2169(3) 0.8686(4) 0.1298(3) 0.053(2) Uani 1 1 d . A 1 C12X C 0.0860(3) 0.9233(6) 0.1368(4) 0.070(3) Uani 1 1 d . A 1 H12X H 0.0769 0.8771 0.1456 0.084 Uiso 1 1 calc R A 1 C13X C 0.0487(4) 0.9463(6) 0.0929(4) 0.094(4) Uani 1 1 d . A 1 H13D H 0.0497 0.9158 0.0656 0.141 Uiso 1 1 calc R A 1 H13E H 0.0567 0.9917 0.0835 0.141 Uiso 1 1 calc R A 1 H13F H 0.0162 0.946 0.1018 0.141 Uiso 1 1 calc R A 1 C14X C 0.0843(4) 0.9669(7) 0.1795(5) 0.106(4) Uani 1 1 d . A 1 H14D H 0.0514 0.9667 0.1877 0.159 Uiso 1 1 calc R A 1 H14E H 0.0932 1.0127 0.1719 0.159 Uiso 1 1 calc R A 1 H14F H 0.107 0.9502 0.2072 0.159 Uiso 1 1 calc R A 1 C15X C 0.2543(4) 0.8146(5) 0.1477(4) 0.070(3) Uani 1 1 d . A 1 H15X H 0.2369 0.7756 0.1592 0.084 Uiso 1 1 calc R A 1 C16X C 0.2916(4) 0.8391(7) 0.1898(4) 0.098(4) Uani 1 1 d . A 1 H16D H 0.3146 0.8031 0.2004 0.147 Uiso 1 1 calc R A 1 H16E H 0.2751 0.8524 0.2169 0.147 Uiso 1 1 calc R A 1 H16F H 0.3091 0.8776 0.1793 0.147 Uiso 1 1 calc R A 1 C17X C 0.2808(4) 0.7904(5) 0.1067(4) 0.076(3) Uani 1 1 d . A 1 H17D H 0.3042 0.7557 0.1191 0.114 Uiso 1 1 calc R A 1 H17E H 0.2978 0.828 0.0945 0.114 Uiso 1 1 calc R A 1 H17F H 0.2573 0.7719 0.0803 0.114 Uiso 1 1 calc R A 1 C18X C 0.1583(3) 0.5917(4) 0.1881(3) 0.047(2) Uani 1 1 d . A 1 C19X C 0.1356(3) 0.5453(5) 0.2149(4) 0.061(3) Uani 1 1 d . A 1 C20X C 0.1398(4) 0.4775(6) 0.2059(5) 0.080(3) Uani 1 1 d . A 1 H20X H 0.1249 0.4457 0.2242 0.096 Uiso 1 1 calc R A 1 C21X C 0.1659(4) 0.4563(6) 0.1704(5) 0.091(4) Uani 1 1 d . A 1 H21X H 0.169 0.4098 0.1645 0.11 Uiso 1 1 calc R A 1 C22X C 0.1872(4) 0.5020(5) 0.1433(5) 0.081(3) Uani 1 1 d . A 1 H22X H 0.2042 0.4863 0.1186 0.098 Uiso 1 1 calc R A 1 C23X C 0.1845(3) 0.5713(5) 0.1516(4) 0.058(2) Uani 1 1 d . A 1 C24X C 0.1051(3) 0.5659(5) 0.2540(4) 0.068(3) Uani 1 1 d . A 1 H24X H 0.1076 0.6155 0.2579 0.082 Uiso 1 1 calc R A 1 C25X C 0.1230(5) 0.5346(8) 0.3022(5) 0.123(5) Uani 1 1 d . A 1 H25D H 0.157 0.5466 0.3125 0.185 Uiso 1 1 calc R A 1 H25E H 0.12 0.4858 0.2995 0.185 Uiso 1 1 calc R A 1 H25F H 0.1036 0.5508 0.3262 0.185 Uiso 1 1 calc R A 1 C26X C 0.0530(4) 0.5487(7) 0.2382(5) 0.096(4) Uani 1 1 d . A 1 H26D H 0.0414 0.57 0.2069 0.145 Uiso 1 1 calc R A 1 H26E H 0.0339 0.5647 0.2624 0.145 Uiso 1 1 calc R A 1 H26F H 0.0495 0.5 0.2349 0.145 Uiso 1 1 calc R A 1 C27X C 0.2129(3) 0.6179(5) 0.1257(3) 0.060(2) Uani 1 1 d . A 1 H27X H 0.1995 0.6638 0.1287 0.072 Uiso 1 1 calc R A 1 C28X C 0.2644(4) 0.6191(6) 0.1486(4) 0.087(4) Uani 1 1 d . A 1 H28D H 0.2823 0.6506 0.1312 0.13 Uiso 1 1 calc R A 1 H28E H 0.2783 0.5743 0.1473 0.13 Uiso 1 1 calc R A 1 H28F H 0.2667 0.6332 0.1825 0.13 Uiso 1 1 calc R A 1 C29X C 0.2088(5) 0.6021(6) 0.0707(4) 0.095(4) Uani 1 1 d . A 1 H29D H 0.2278 0.6347 0.0555 0.142 Uiso 1 1 calc R A 1 H29E H 0.1748 0.6046 0.0556 0.142 Uiso 1 1 calc R A 1 H29F H 0.2213 0.557 0.0665 0.142 Uiso 1 1 calc R A 1 C30X C 0.0156(3) 0.7605(5) 0.0910(3) 0.054(2) Uani 1 1 d . A 1 C31X C -0.0004(3) 0.7987(5) 0.1285(3) 0.059(2) Uani 1 1 d . A 1 H31X H -0.0164 0.839 0.1172 0.071 Uiso 1 1 calc R A 1 C32X C 0.0025(3) 0.7892(5) 0.1783(3) 0.056(2) Uani 1 1 d . A 1 C33X C -0.0127(3) 0.7721(5) 0.0409(3) 0.070(3) Uani 1 1 d . A 1 H33A' H -0.0085 0.7338 0.02 0.106 Uiso 1 1 calc R A 1 H33B' H -0.0009 0.8128 0.027 0.106 Uiso 1 1 calc R A 1 H33C' H -0.0471 0.7774 0.0431 0.106 Uiso 1 1 calc R A 1 C34X C -0.0274(4) 0.8377(6) 0.2030(4) 0.076(3) Uani 1 1 d . A 1 H34A' H -0.0061 0.8622 0.2283 0.114 Uiso 1 1 calc R A 1 H34B' H -0.0516 0.8128 0.2177 0.114 Uiso 1 1 calc R A 1 H34C' H -0.0437 0.8694 0.1791 0.114 Uiso 1 1 calc R A 1 C35X C 0.0635(3) 0.6773(5) 0.0590(3) 0.059(2) Uani 1 1 d . A 1 C36X C 0.0485(4) 0.6110(6) 0.0576(4) 0.072(3) Uani 1 1 d . A 1 C37X C 0.0599(4) 0.5695(7) 0.0199(5) 0.097(4) Uani 1 1 d . A 1 H37X H 0.0501 0.524 0.0181 0.116 Uiso 1 1 calc R A 1 C38X C 0.0860(5) 0.5962(8) -0.0147(5) 0.103(5) Uani 1 1 d . A 1 H38X H 0.0943 0.5685 -0.0398 0.124 Uiso 1 1 calc R A 1 C39X C 0.0996(4) 0.6621(7) -0.0124(4) 0.083(3) Uani 1 1 d . A 1 H39X H 0.1164 0.6794 -0.0368 0.099 Uiso 1 1 calc R A 1 C40X C 0.0897(4) 0.7044(6) 0.0244(3) 0.068(3) Uani 1 1 d . A 1 C41X C 0.0170(4) 0.5828(6) 0.0918(4) 0.085(3) Uani 1 1 d . A 1 H41X H 0.0243 0.6085 0.1228 0.102 Uiso 1 1 calc R A 1 C42X C 0.0254(5) 0.5086(6) 0.1044(5) 0.109(4) Uani 1 1 d . A 1 H42D H 0.0038 0.4947 0.127 0.164 Uiso 1 1 calc R A 1 H42E H 0.0591 0.5018 0.1194 0.164 Uiso 1 1 calc R A 1 H42F H 0.0186 0.4818 0.0747 0.164 Uiso 1 1 calc R A 1 C43X C -0.0372(4) 0.5939(6) 0.0717(5) 0.097(4) Uani 1 1 d . A 1 H43D H -0.0571 0.5755 0.0946 0.145 Uiso 1 1 calc R A 1 H43E H -0.0453 0.5714 0.0403 0.145 Uiso 1 1 calc R A 1 H43F H -0.0436 0.6419 0.0676 0.145 Uiso 1 1 calc R A 1 C44X C 0.1064(4) 0.7763(6) 0.0246(3) 0.067(3) Uani 1 1 d . A 1 H44X H 0.0946 0.7998 0.0522 0.081 Uiso 1 1 calc R A 1 C45X C 0.0859(5) 0.8139(7) -0.0232(4) 0.107(4) Uani 1 1 d . A 1 H45D H 0.0974 0.8603 -0.0212 0.16 Uiso 1 1 calc R A 1 H45E H 0.0504 0.8134 -0.0276 0.16 Uiso 1 1 calc R A 1 H45F H 0.0969 0.7916 -0.0507 0.16 Uiso 1 1 calc R A 1 C46X C 0.1617(4) 0.7792(6) 0.0332(4) 0.080(3) Uani 1 1 d . A 1 H46D H 0.1723 0.826 0.0335 0.12 Uiso 1 1 calc R A 1 H46E H 0.1741 0.7552 0.0071 0.12 Uiso 1 1 calc R A 1 H46F H 0.1742 0.7583 0.0644 0.12 Uiso 1 1 calc R A 1 C47X C 0.0142(3) 0.7198(5) 0.2489(4) 0.064(3) Uani 1 1 d . A 1 C48X C -0.0274(4) 0.6791(6) 0.2449(5) 0.081(3) Uani 1 1 d . A 1 C49X C -0.0446(6) 0.6603(7) 0.2859(6) 0.112(6) Uani 1 1 d . A 1 H49X H -0.0732 0.634 0.283 0.134 Uiso 1 1 calc R A 1 C50X C -0.0227(7) 0.6775(8) 0.3296(7) 0.129(7) Uani 1 1 d . A 1 H50X H -0.0351 0.6623 0.3575 0.155 Uiso 1 1 calc R A 1 C51X C 0.0193(5) 0.7183(8) 0.3353(4) 0.105(5) Uani 1 1 d . A 1 H51X H 0.0351 0.7305 0.3667 0.126 Uiso 1 1 calc R A 1 C52X C 0.0374(3) 0.7409(6) 0.2931(3) 0.077(3) Uani 1 1 d . A 1 C53X C -0.0540(4) 0.6530(6) 0.1969(5) 0.095(4) Uani 1 1 d . A 1 H53X H -0.0311 0.6562 0.1728 0.114 Uiso 1 1 calc R A 1 C54X C -0.0996(4) 0.6949(8) 0.1764(6) 0.128(5) Uani 1 1 d . A 1 H54D H -0.1149 0.6759 0.1455 0.192 Uiso 1 1 calc R A 1 H54E H -0.09 0.7412 0.1714 0.192 Uiso 1 1 calc R A 1 H54F H -0.1226 0.6941 0.1996 0.192 Uiso 1 1 calc R A 1 C55X C -0.0699(5) 0.5793(8) 0.1982(6) 0.141(6) Uani 1 1 d . A 1 H55D H -0.0866 0.5661 0.1661 0.211 Uiso 1 1 calc R A 1 H55E H -0.0918 0.5739 0.222 0.211 Uiso 1 1 calc R A 1 H55F H -0.0413 0.5509 0.2072 0.211 Uiso 1 1 calc R A 1 C56X C 0.0815(4) 0.7871(10) 0.3003(4) 0.111(6) Uani 1 1 d . A 1 H56X H 0.0945 0.789 0.2689 0.133 Uiso 1 1 calc R A 1 C57X C 0.1222(4) 0.7593(11) 0.3395(4) 0.176(10) Uani 1 1 d . A 1 H57D H 0.1306 0.7139 0.3307 0.264 Uiso 1 1 calc R A 1 H57E H 0.1108 0.7585 0.371 0.264 Uiso 1 1 calc R A 1 H57F H 0.1508 0.7881 0.3416 0.264 Uiso 1 1 calc R A 1 C58X C 0.0686(5) 0.8584(10) 0.3134(6) 0.150(7) Uani 1 1 d . A 1 H58D H 0.0977 0.8863 0.3172 0.225 Uiso 1 1 calc R A 1 H58E H 0.0553 0.8579 0.3439 0.225 Uiso 1 1 calc R A 1 H58F H 0.0444 0.8767 0.2875 0.225 Uiso 1 1 calc R A 1 F1Y F 0.3212(2) 0.6734(3) 0.03007(18) 0.0760(16) Uani 1 1 d . B 1 F2Y F 0.3688(2) 0.5851(4) 0.0904(2) 0.098(2) Uani 1 1 d . B 1 F3Y F 0.4344(2) 0.4999(3) 0.0604(2) 0.0839(18) Uani 1 1 d . B 1 F4Y F 0.4517(2) 0.5061(3) -0.0325(2) 0.0820(17) Uani 1 1 d . B 1 F5Y F 0.4043(2) 0.5935(3) -0.09435(17) 0.0666(15) Uani 1 1 d . B 1 F6Y F 0.43565(17) 0.7203(3) -0.06062(18) 0.0629(14) Uani 1 1 d . B 1 F7Y F 0.48343(17) 0.7865(3) -0.1200(2) 0.0690(15) Uani 1 1 d . B 1 F8Y F 0.4383(2) 0.8292(3) -0.20793(19) 0.0704(15) Uani 1 1 d . B 1 F9Y F 0.3428(2) 0.7998(3) -0.23575(19) 0.0796(17) Uani 1 1 d . B 1 F10Y F 0.29338(18) 0.7341(3) -0.17723(19) 0.0742(16) Uani 1 1 d . B 1 F11Y F 0.2312(2) 0.7519(3) -0.1109(2) 0.095(2) Uani 1 1 d . B 1 F12Y F 0.2003(2) 0.8667(4) -0.0816(2) 0.108(2) Uani 1 1 d . B 1 F13Y F 0.2562(2) 0.9396(3) -0.0108(2) 0.0850(18) Uani 1 1 d . B 1 F14Y F 0.3434(2) 0.8910(3) 0.0300(2) 0.0710(15) Uani 1 1 d . B 1 F15Y F 0.37599(17) 0.7763(3) 0.00006(19) 0.0668(15) Uani 1 1 d . B 1 F16Y F 0.2413(2) 0.6484(3) -0.0390(2) 0.093(2) Uani 1 1 d . B 1 F17Y F 0.1765(2) 0.5566(4) -0.0728(3) 0.109(2) Uani 1 1 d . B 1 F18Y F 0.1859(2) 0.4847(3) -0.1538(2) 0.100(2) Uani 1 1 d . B 1 F19Y F 0.2626(2) 0.5097(3) -0.1998(2) 0.0800(17) Uani 1 1 d . B 1 F20Y F 0.32637(18) 0.6036(3) -0.16894(18) 0.0640(14) Uani 1 1 d . B 1 C1Y C 0.3606(3) 0.6398(4) -0.0363(3) 0.0433(19) Uani 1 1 d . B 1 C2Y C 0.3532(3) 0.6330(5) 0.0117(3) 0.054(2) Uani 1 1 d . B 1 C3Y C 0.3774(4) 0.5869(5) 0.0441(3) 0.059(2) Uani 1 1 d . B 1 C4Y C 0.4106(4) 0.5449(5) 0.0290(3) 0.061(3) Uani 1 1 d . B 1 C5Y C 0.4198(3) 0.5485(5) -0.0168(3) 0.056(2) Uani 1 1 d . B 1 C6Y C 0.3947(3) 0.5944(4) -0.0479(3) 0.050(2) Uani 1 1 d . B 1 C7Y C 0.3617(3) 0.7218(4) -0.1153(3) 0.0420(19) Uani 1 1 d . B 1 C8Y C 0.4099(3) 0.7372(4) -0.1035(3) 0.0446(19) Uani 1 1 d . B 1 C9Y C 0.4360(3) 0.7728(4) -0.1344(3) 0.051(2) Uani 1 1 d . B 1 C10Y C 0.4130(4) 0.7931(4) -0.1785(3) 0.052(2) Uani 1 1 d . B 1 C11Y C 0.3660(4) 0.7800(4) -0.1916(3) 0.054(2) Uani 1 1 d . B 1 C12Y C 0.3414(3) 0.7449(4) -0.1608(3) 0.047(2) Uani 1 1 d . B 1 C13Y C 0.3055(3) 0.7556(4) -0.0559(3) 0.046(2) Uani 1 1 d . B 1 C14Y C 0.2610(3) 0.7833(5) -0.0749(3) 0.057(2) Uani 1 1 d . B 1 C15Y C 0.2442(4) 0.8434(6) -0.0609(4) 0.070(3) Uani 1 1 d . B 1 C16Y C 0.2717(4) 0.8802(5) -0.0256(4) 0.062(3) Uani 1 1 d . B 1 C17Y C 0.3160(3) 0.8555(5) -0.0054(3) 0.051(2) Uani 1 1 d . B 1 C18Y C 0.3314(3) 0.7954(5) -0.0207(3) 0.050(2) Uani 1 1 d . B 1 C19Y C 0.2872(3) 0.6342(4) -0.1028(3) 0.044(2) Uani 1 1 d . B 1 C20Y C 0.2478(3) 0.6175(6) -0.0806(3) 0.067(3) Uani 1 1 d . B 1 C21Y C 0.2146(4) 0.5675(6) -0.0970(4) 0.070(3) Uani 1 1 d . B 1 C22Y C 0.2189(4) 0.5335(5) -0.1367(4) 0.070(3) Uani 1 1 d . B 1 C23Y C 0.2569(4) 0.5451(5) -0.1597(3) 0.056(2) Uani 1 1 d . B 1 C24Y C 0.2897(3) 0.5946(4) -0.1430(3) 0.045(2) Uani 1 1 d . B 1 B1Y B 0.3288(3) 0.6878(5) -0.0772(3) 0.042(2) Uani 1 1 d . B 1 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 Tm 0.03779(19) 0.0417(2) 0.03338(18) -0.00408(16) 0.00590(14) -0.00057(16) N1 0.055(4) 0.071(5) 0.052(4) -0.006(4) 0.022(4) -0.007(4) N2 0.037(4) 0.112(7) 0.043(4) 0.006(4) -0.002(3) -0.001(4) N3 0.052(4) 0.047(4) 0.034(4) -0.006(3) -0.009(3) 0.001(3) N4 0.064(5) 0.030(4) 0.058(4) 0.005(3) 0.020(4) 0.007(3) C1 0.089(8) 0.087(8) 0.060(6) -0.026(6) 0.012(6) -0.014(7) C2 0.092(9) 0.119(11) 0.065(7) -0.025(7) 0.007(6) -0.049(8) C3 0.047(6) 0.132(11) 0.052(6) 0.005(6) -0.001(5) -0.020(6) C4 0.137(11) 0.096(10) 0.095(9) -0.050(8) 0.058(8) -0.031(8) C5 0.080(8) 0.204(17) 0.077(8) 0.029(9) -0.034(7) -0.051(10) C6 0.066(6) 0.058(6) 0.054(6) -0.011(5) 0.022(5) -0.004(5) C7 0.075(7) 0.071(7) 0.059(6) -0.017(5) 0.029(5) -0.011(6) C8 0.074(7) 0.067(7) 0.098(9) -0.008(6) 0.044(6) 0.003(6) C9 0.097(9) 0.067(7) 0.093(9) -0.002(6) 0.064(8) -0.010(7) C10 0.101(9) 0.090(9) 0.067(7) 0.000(6) 0.037(7) 0.013(8) C11 0.082(7) 0.089(8) 0.047(6) -0.012(5) 0.028(5) -0.007(6) C12 0.070(7) 0.103(10) 0.071(7) 0.000(7) 0.023(6) 0.004(7) C13 0.25(2) 0.113(13) 0.092(10) 0.029(9) 0.067(12) 0.008(13) C14 0.044(6) 0.28(2) 0.094(10) 0.039(12) -0.007(6) 0.009(10) C15 0.080(8) 0.149(13) 0.053(7) 0.013(7) 0.014(6) 0.009(8) C16 0.126(12) 0.185(17) 0.085(10) 0.056(10) 0.025(9) 0.050(12) C17 0.119(12) 0.29(2) 0.063(9) -0.041(12) -0.015(8) 0.005(14) C18 0.038(5) 0.147(12) 0.077(7) 0.047(8) 0.005(5) 0.025(6) C19 0.083(8) 0.140(12) 0.111(10) 0.083(9) 0.036(7) 0.060(8) C20 0.25(2) 0.26(2) 0.191(17) 0.172(17) 0.160(17) 0.21(2) C21 0.23(2) 0.37(3) 0.35(3) 0.29(3) 0.23(2) 0.23(2) C22 0.131(13) 0.33(3) 0.25(2) 0.24(2) 0.137(15) 0.160(17) C23 0.050(7) 0.226(18) 0.101(10) 0.094(11) 0.030(6) 0.046(9) C24 0.098(9) 0.110(11) 0.082(8) 0.042(8) 0.026(7) 0.049(8) C25 0.096(10) 0.205(18) 0.121(12) 0.088(12) 0.027(9) 0.017(11) C26 0.127(12) 0.114(13) 0.157(15) 0.033(11) 0.036(11) 0.042(10) C27 0.045(6) 0.191(16) 0.095(9) 0.048(10) 0.010(6) -0.022(8) C28 0.092(9) 0.117(11) 0.087(9) 0.036(8) 0.001(7) 0.007(8) C29 0.140(14) 0.36(3) 0.141(14) 0.123(17) -0.044(11) -0.160(18) C30 0.062(6) 0.059(6) 0.062(6) 0.021(5) 0.023(5) 0.031(5) C31 0.040(5) 0.072(7) 0.074(7) 0.020(6) 0.005(5) 0.000(5) C32 0.064(6) 0.067(7) 0.048(5) 0.006(5) 0.003(5) -0.008(5) C33 0.094(8) 0.078(8) 0.123(10) 0.050(7) 0.052(8) 0.053(7) C34 0.095(9) 0.121(11) 0.074(8) -0.006(7) -0.031(7) -0.028(8) C35 0.079(7) 0.044(5) 0.048(5) -0.009(4) 0.004(5) 0.004(5) C36 0.106(8) 0.048(6) 0.061(6) -0.013(5) 0.021(6) -0.004(6) C37 0.148(12) 0.058(8) 0.117(11) -0.014(7) 0.061(9) 0.007(8) C38 0.211(17) 0.051(7) 0.103(10) -0.020(7) 0.066(11) -0.016(9) C39 0.157(12) 0.044(6) 0.076(8) -0.005(6) 0.035(8) -0.017(7) C40 0.098(8) 0.041(6) 0.061(6) -0.018(5) 0.008(6) -0.007(5) C41 0.109(9) 0.067(7) 0.084(8) -0.013(6) 0.034(7) -0.005(7) C42 0.185(17) 0.093(11) 0.30(2) 0.016(13) 0.176(18) 0.034(11) C43 0.34(3) 0.117(12) 0.053(8) -0.005(8) 0.048(12) -0.064(15) C44 0.083(8) 0.064(7) 0.079(8) -0.001(6) 0.016(6) -0.010(6) C45 0.146(14) 0.133(13) 0.165(15) -0.038(11) 0.057(12) -0.086(11) C46 0.156(12) 0.072(8) 0.084(9) 0.010(7) 0.054(9) 0.023(8) C47 0.067(6) 0.039(5) 0.065(6) -0.004(4) 0.020(5) -0.001(4) C48 0.056(5) 0.049(6) 0.058(6) 0.001(4) 0.013(5) 0.002(4) C49 0.063(6) 0.064(7) 0.084(8) 0.014(6) 0.022(6) 0.012(5) C50 0.091(8) 0.039(6) 0.095(8) -0.001(6) 0.023(7) -0.006(5) C51 0.116(9) 0.044(6) 0.076(7) -0.008(5) 0.025(7) -0.012(6) C52 0.094(8) 0.043(6) 0.069(7) -0.004(5) 0.028(6) -0.008(5) C53 0.072(7) 0.082(7) 0.055(6) -0.002(5) 0.019(5) -0.009(6) C54 0.065(7) 0.178(14) 0.076(8) -0.019(9) 0.006(6) -0.016(8) C55 0.094(8) 0.099(9) 0.061(7) 0.003(6) 0.023(6) 0.023(7) C56 0.108(9) 0.091(9) 0.066(7) 0.025(6) 0.027(7) 0.002(8) C57 0.185(17) 0.120(13) 0.165(16) -0.009(11) 0.098(14) 0.041(12) C58 0.32(3) 0.132(13) 0.058(8) -0.034(8) 0.040(12) -0.127(15) F1A 0.116(5) 0.090(4) 0.042(3) -0.017(3) 0.000(3) -0.001(4) F2A 0.164(7) 0.086(5) 0.059(4) -0.031(3) 0.025(4) -0.019(4) F3A 0.119(5) 0.063(4) 0.100(5) -0.028(3) 0.054(4) -0.008(4) F4A 0.062(3) 0.067(4) 0.097(4) -0.012(3) 0.023(3) 0.003(3) F5A 0.062(3) 0.080(4) 0.057(3) -0.014(3) 0.002(3) 0.014(3) F6A 0.051(3) 0.075(3) 0.038(3) -0.007(2) -0.002(2) 0.007(3) F7A 0.093(4) 0.072(4) 0.048(3) 0.004(3) 0.024(3) 0.012(3) F8A 0.068(4) 0.085(4) 0.094(4) 0.010(3) 0.035(3) -0.003(3) F9A 0.060(3) 0.086(4) 0.103(5) 0.012(4) -0.013(3) -0.023(3) F10A 0.076(4) 0.082(4) 0.049(3) 0.002(3) -0.019(3) -0.018(3) F11A 0.053(3) 0.086(4) 0.061(3) 0.005(3) 0.009(3) 0.013(3) F12A 0.092(5) 0.087(4) 0.079(4) -0.003(3) -0.019(3) 0.026(4) F13A 0.162(7) 0.083(5) 0.084(5) 0.023(4) -0.018(5) -0.003(5) F14A 0.163(7) 0.122(6) 0.095(5) 0.036(5) 0.040(5) -0.016(5) F15A 0.096(5) 0.100(5) 0.079(4) 0.003(4) 0.042(4) -0.018(4) F16A 0.060(3) 0.094(4) 0.106(5) -0.037(4) 0.034(3) -0.002(3) F17A 0.054(4) 0.110(5) 0.146(6) -0.015(5) 0.005(4) -0.017(4) F18A 0.090(4) 0.091(5) 0.108(5) -0.029(4) -0.033(4) -0.017(4) F19A 0.101(4) 0.075(4) 0.064(4) -0.030(3) -0.012(3) 0.016(3) F20A 0.058(3) 0.071(4) 0.057(3) -0.012(3) 0.012(2) 0.010(3) C1A 0.057(5) 0.053(6) 0.049(5) -0.012(4) 0.021(4) -0.013(5) C2A 0.077(7) 0.066(6) 0.045(5) -0.010(5) 0.011(5) -0.005(6) C3A 0.114(9) 0.074(8) 0.052(6) -0.019(6) 0.033(6) -0.017(7) C4A 0.087(8) 0.053(6) 0.070(7) -0.022(6) 0.042(6) -0.018(6) C5A 0.062(6) 0.051(6) 0.067(7) -0.002(5) 0.020(5) -0.006(5) C6A 0.055(5) 0.066(6) 0.047(5) -0.012(5) 0.019(4) -0.006(5) C7A 0.043(5) 0.052(5) 0.040(5) -0.007(4) 0.006(4) 0.006(4) C8A 0.040(4) 0.068(6) 0.041(5) -0.010(4) 0.003(4) 0.015(4) C9A 0.065(6) 0.058(6) 0.043(5) 0.013(4) 0.016(4) 0.028(5) C10A 0.039(5) 0.062(6) 0.066(6) 0.009(5) 0.011(5) 0.002(4) C11A 0.043(5) 0.073(7) 0.070(7) -0.006(5) -0.006(5) 0.004(5) C12A 0.042(5) 0.066(6) 0.047(5) 0.007(4) -0.004(4) 0.005(4) C13A 0.056(5) 0.061(6) 0.034(5) -0.016(4) 0.005(4) -0.011(5) C14A 0.066(6) 0.068(6) 0.034(5) -0.013(4) 0.003(4) 0.000(5) C15A 0.071(7) 0.068(7) 0.047(6) -0.009(5) -0.009(5) -0.003(6) C16A 0.111(10) 0.070(8) 0.057(7) 0.000(6) -0.004(7) 0.004(7) C17A 0.135(12) 0.072(8) 0.055(7) 0.012(6) 0.020(7) -0.034(8) C18A 0.062(6) 0.075(7) 0.060(6) -0.010(5) 0.020(5) -0.008(5) C19A 0.049(5) 0.072(6) 0.039(5) -0.007(4) 0.005(4) 0.003(5) C20A 0.049(6) 0.084(8) 0.078(7) -0.016(6) 0.019(5) 0.001(5) C21A 0.043(5) 0.068(7) 0.091(8) -0.009(6) -0.007(5) -0.010(5) C22A 0.076(7) 0.063(7) 0.068(7) -0.015(6) -0.024(6) 0.000(6) C23A 0.069(7) 0.074(7) 0.052(6) -0.013(5) -0.009(5) 0.024(6) C24A 0.048(5) 0.063(6) 0.038(5) -0.007(4) -0.008(4) 0.011(5) B1A 0.051(6) 0.071(8) 0.035(5) -0.011(5) 0.004(4) -0.005(5) Tm1X 0.03272(18) 0.0567(2) 0.03276(19) 0.00131(17) 0.00371(14) 0.00397(17) N1X 0.039(4) 0.040(4) 0.040(4) -0.001(3) -0.003(3) 0.005(3) N2X 0.033(3) 0.047(4) 0.041(4) 0.002(3) 0.003(3) -0.002(3) N3X 0.044(4) 0.068(5) 0.037(4) -0.013(3) 0.002(3) 0.005(4) N4X 0.041(4) 0.085(6) 0.041(4) 0.003(4) 0.010(3) 0.006(4) C1X 0.038(4) 0.040(5) 0.046(5) 0.002(4) 0.006(4) 0.006(4) C2X 0.045(5) 0.053(5) 0.035(4) 0.008(4) 0.006(4) 0.002(4) C3X 0.039(4) 0.056(6) 0.036(4) 0.013(4) 0.003(4) -0.001(4) C4X 0.077(6) 0.055(6) 0.037(5) -0.001(4) 0.000(4) -0.006(5) C5X 0.059(6) 0.060(6) 0.056(6) 0.008(5) -0.010(5) 0.002(5) C6X 0.062(6) 0.053(6) 0.034(4) 0.008(4) 0.000(4) 0.000(5) C7X 0.063(6) 0.046(5) 0.046(5) 0.000(4) -0.001(4) 0.009(5) C8X 0.081(7) 0.061(7) 0.052(6) 0.011(5) 0.002(5) 0.015(6) C9X 0.115(9) 0.050(6) 0.044(5) 0.011(5) 0.021(6) -0.001(6) C10X 0.078(7) 0.053(6) 0.055(6) 0.013(5) 0.017(5) -0.001(5) C11X 0.064(6) 0.055(6) 0.044(5) 0.010(4) 0.017(4) 0.010(5) C12X 0.046(5) 0.078(7) 0.078(7) 0.014(6) -0.013(5) 0.004(5) C13X 0.084(8) 0.088(9) 0.100(9) 0.021(7) -0.019(7) 0.022(7) C14X 0.073(8) 0.136(12) 0.118(11) -0.002(9) 0.045(8) 0.010(8) C15X 0.072(7) 0.060(7) 0.088(8) 0.033(6) 0.040(6) 0.017(5) C16X 0.071(7) 0.154(13) 0.067(7) 0.023(8) 0.004(6) 0.032(8) C17X 0.069(7) 0.071(7) 0.094(8) 0.005(6) 0.028(6) 0.008(6) C18X 0.031(4) 0.051(5) 0.054(5) -0.001(4) -0.005(4) 0.005(4) C19X 0.041(5) 0.060(6) 0.079(7) -0.005(5) 0.004(5) -0.013(5) C20X 0.047(6) 0.065(7) 0.130(10) 0.013(7) 0.017(6) -0.013(5) C21X 0.064(7) 0.049(7) 0.164(13) -0.009(7) 0.030(8) -0.019(6) C22X 0.058(6) 0.061(7) 0.130(10) -0.023(7) 0.028(7) -0.005(5) C23X 0.045(5) 0.054(6) 0.076(7) -0.010(5) 0.010(5) 0.001(4) C24X 0.058(6) 0.066(7) 0.082(7) 0.011(6) 0.011(5) -0.009(5) C25X 0.101(10) 0.167(15) 0.102(10) 0.049(10) 0.018(8) -0.003(10) C26X 0.074(8) 0.110(10) 0.113(10) -0.002(8) 0.038(7) -0.001(7) C27X 0.063(6) 0.054(6) 0.068(6) 0.001(5) 0.023(5) 0.014(5) C28X 0.062(7) 0.092(9) 0.105(9) 0.033(7) 0.006(6) -0.019(6) C29X 0.124(10) 0.095(9) 0.067(7) -0.013(7) 0.019(7) 0.014(8) C30X 0.050(5) 0.057(6) 0.052(5) 0.001(5) -0.001(4) -0.003(5) C31X 0.053(5) 0.066(6) 0.056(6) -0.004(5) -0.001(4) 0.016(5) C32X 0.045(5) 0.075(7) 0.049(5) -0.002(5) 0.004(4) 0.007(5) C33X 0.069(6) 0.084(8) 0.051(6) 0.003(5) -0.014(5) 0.017(6) C34X 0.072(7) 0.093(8) 0.064(7) -0.006(6) 0.016(5) 0.029(6) C35X 0.050(5) 0.071(7) 0.052(6) -0.001(5) -0.009(4) 0.000(5) C36X 0.053(6) 0.085(8) 0.072(7) -0.015(6) -0.007(5) 0.014(6) C37X 0.075(8) 0.116(11) 0.097(9) -0.044(8) 0.003(7) 0.012(7) C38X 0.083(9) 0.144(14) 0.080(9) -0.055(9) 0.009(7) 0.009(9) C39X 0.072(7) 0.118(11) 0.057(7) -0.030(7) 0.006(5) 0.001(7) C40X 0.064(6) 0.095(8) 0.043(5) -0.011(5) -0.001(5) 0.013(6) C41X 0.081(8) 0.089(9) 0.080(8) -0.022(7) -0.004(6) -0.011(7) C42X 0.126(11) 0.079(9) 0.117(11) -0.011(8) -0.001(9) -0.017(8) C43X 0.076(8) 0.096(9) 0.116(10) -0.012(8) 0.009(7) -0.012(7) C44X 0.079(7) 0.086(8) 0.037(5) 0.002(5) 0.009(5) 0.006(6) C45X 0.119(10) 0.148(13) 0.054(7) 0.018(7) 0.012(7) 0.013(9) C46X 0.092(8) 0.097(9) 0.052(6) -0.008(6) 0.014(6) -0.004(7) C47X 0.045(5) 0.085(8) 0.065(6) 0.018(5) 0.021(5) 0.021(5) C48X 0.066(7) 0.081(8) 0.105(9) 0.014(7) 0.050(7) 0.017(6) C49X 0.149(14) 0.084(10) 0.129(12) 0.015(9) 0.102(12) 0.010(9) C50X 0.164(16) 0.097(11) 0.160(15) 0.068(11) 0.133(14) 0.068(11) C51X 0.104(10) 0.158(14) 0.061(7) 0.033(8) 0.036(7) 0.057(10) C52X 0.052(6) 0.136(10) 0.046(6) 0.017(6) 0.016(5) 0.032(6) C53X 0.066(7) 0.093(10) 0.135(12) 0.000(8) 0.046(8) -0.013(7) C54X 0.073(8) 0.133(13) 0.173(15) -0.028(11) 0.001(9) 0.010(9) C55X 0.095(10) 0.128(13) 0.211(18) -0.022(12) 0.060(11) -0.041(10) C56X 0.046(6) 0.253(19) 0.034(6) -0.005(8) 0.008(5) 0.005(9) C57X 0.071(8) 0.42(3) 0.037(6) -0.004(11) -0.010(6) 0.058(13) C58X 0.079(10) 0.24(2) 0.136(14) -0.054(14) 0.031(9) -0.042(12) F1Y 0.077(4) 0.101(5) 0.056(3) 0.020(3) 0.028(3) 0.017(3) F2Y 0.112(5) 0.125(6) 0.061(4) 0.038(4) 0.025(3) 0.019(4) F3Y 0.099(4) 0.071(4) 0.074(4) 0.024(3) -0.012(3) 0.008(3) F4Y 0.089(4) 0.074(4) 0.077(4) 0.000(3) -0.009(3) 0.033(3) F5Y 0.091(4) 0.065(3) 0.044(3) 0.001(2) 0.014(3) 0.030(3) F6Y 0.050(3) 0.082(4) 0.054(3) 0.009(3) 0.001(2) -0.014(3) F7Y 0.048(3) 0.077(4) 0.085(4) 0.004(3) 0.020(3) -0.010(3) F8Y 0.090(4) 0.058(3) 0.073(4) 0.012(3) 0.044(3) -0.004(3) F9Y 0.103(4) 0.074(4) 0.058(3) 0.029(3) 0.003(3) -0.005(3) F10Y 0.058(3) 0.087(4) 0.071(4) 0.030(3) -0.011(3) -0.002(3) F11Y 0.077(4) 0.110(5) 0.086(4) -0.027(4) -0.029(3) 0.037(4) F12Y 0.098(5) 0.111(5) 0.106(5) -0.018(4) -0.014(4) 0.059(4) F13Y 0.118(5) 0.056(4) 0.090(4) -0.004(3) 0.048(4) 0.019(3) F14Y 0.079(4) 0.060(3) 0.078(4) -0.020(3) 0.027(3) -0.016(3) F15Y 0.048(3) 0.069(4) 0.078(4) -0.022(3) -0.005(3) -0.003(3) F16Y 0.081(4) 0.126(6) 0.081(4) -0.034(4) 0.042(3) -0.048(4) F17Y 0.078(4) 0.135(6) 0.120(6) -0.016(5) 0.033(4) -0.055(4) F18Y 0.085(4) 0.089(5) 0.116(5) -0.014(4) -0.012(4) -0.043(4) F19Y 0.095(4) 0.072(4) 0.068(4) -0.021(3) -0.004(3) -0.005(3) F20Y 0.067(3) 0.070(4) 0.056(3) -0.019(3) 0.014(3) -0.006(3) C1Y 0.037(4) 0.050(5) 0.042(5) -0.001(4) 0.002(4) -0.007(4) C2Y 0.054(5) 0.051(6) 0.057(6) 0.007(5) 0.013(5) -0.004(5) C3Y 0.072(6) 0.065(6) 0.040(5) 0.018(5) 0.004(5) -0.004(5) C4Y 0.065(6) 0.059(6) 0.052(6) 0.015(5) -0.014(5) -0.006(5) C5Y 0.061(6) 0.047(5) 0.054(6) 0.000(5) -0.014(5) 0.009(5) C6Y 0.063(6) 0.044(5) 0.040(5) -0.003(4) -0.001(4) -0.003(4) C7Y 0.042(4) 0.045(5) 0.041(5) -0.007(4) 0.011(4) -0.001(4) C8Y 0.053(5) 0.042(5) 0.039(5) -0.002(4) 0.009(4) 0.003(4) C9Y 0.049(5) 0.043(5) 0.064(6) -0.006(4) 0.025(5) 0.002(4) C10Y 0.073(6) 0.032(5) 0.057(6) -0.004(4) 0.030(5) 0.004(5) C11Y 0.071(6) 0.041(5) 0.049(5) 0.011(4) 0.008(5) 0.009(5) C12Y 0.052(5) 0.030(4) 0.057(5) 0.004(4) 0.005(4) 0.003(4) C13Y 0.048(5) 0.050(5) 0.041(5) 0.002(4) 0.011(4) -0.004(4) C14Y 0.061(6) 0.056(6) 0.050(5) -0.009(4) -0.006(5) 0.008(5) C15Y 0.059(6) 0.087(8) 0.060(6) -0.011(6) 0.002(5) 0.019(6) C16Y 0.078(7) 0.052(6) 0.064(6) 0.005(5) 0.035(6) 0.010(5) C17Y 0.057(6) 0.052(6) 0.046(5) -0.001(4) 0.016(4) -0.016(5) C18Y 0.045(5) 0.056(6) 0.054(5) -0.005(5) 0.016(4) -0.005(4) C19Y 0.041(5) 0.052(5) 0.036(4) 0.004(4) 0.001(4) -0.002(4) C20Y 0.059(6) 0.091(8) 0.051(6) -0.011(5) 0.007(5) -0.018(6) C21Y 0.061(6) 0.081(8) 0.067(7) -0.006(6) 0.014(5) -0.025(6) C22Y 0.063(7) 0.071(7) 0.067(7) 0.009(6) -0.017(6) -0.018(6) C23Y 0.069(6) 0.051(6) 0.043(5) -0.001(4) -0.007(5) -0.002(5) C24Y 0.047(5) 0.044(5) 0.043(5) 0.005(4) 0.006(4) 0.001(4) B1Y 0.044(5) 0.049(6) 0.034(5) -0.003(4) 0.008(4) -0.008(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 Tm N1 2.214(7) . ? Tm N2 2.225(7) . ? Tm N3 2.227(6) . ? Tm N4 2.250(7) . ? N1 C1 1.388(12) . ? N1 C6 1.442(11) . ? N2 C3 1.321(13) . ? N2 C18 1.456(13) . ? N3 C32 1.321(11) . ? N3 C35 1.479(11) . ? N4 C30 1.370(11) . ? N4 C47 1.468(11) . ? C1 C2 1.400(15) . ? C1 C4 1.513(14) . ? C2 C3 1.439(16) . ? C3 C5 1.498(13) . ? C6 C7 1.387(13) . ? C6 C11 1.401(13) . ? C7 C8 1.435(13) . ? C7 C12 1.521(14) . ? C8 C9 1.372(15) . ? C9 C10 1.303(15) . ? C10 C11 1.397(14) . ? C11 C15 1.500(15) . ? C12 C13 1.469(17) . ? C12 C14 1.543(16) . ? C15 C17 1.564(17) . ? C15 C16 1.581(19) . ? C18 C23 1.396(15) . ? C18 C19 1.415(17) . ? C19 C20 1.401(17) . ? C19 C24 1.523(15) . ? C20 C21 1.40(2) . ? C21 C22 1.39(3) . ? C22 C23 1.367(19) . ? C23 C27 1.53(2) . ? C24 C26 1.541(19) . ? C24 C25 1.562(18) . ? C27 C29 1.520(17) . ? C27 C28 1.531(15) . ? C30 C31 1.387(13) . ? C30 C33 1.535(12) . ? C31 C32 1.347(13) . ? C32 C34 1.559(13) . ? C35 C36 1.378(13) . ? C35 C40 1.394(13) . ? C36 C37 1.391(14) . ? C36 C41 1.531(14) . ? C37 C38 1.359(16) . ? C38 C39 1.320(16) . ? C39 C40 1.386(14) . ? C40 C44 1.542(14) . ? C41 C43 1.504(18) . ? C41 C42 1.557(17) . ? C44 C46 1.524(14) . ? C44 C45 1.544(15) . ? C47 C52 1.377(12) . ? C47 C48 1.417(12) . ? C48 C49 1.410(13) . ? C48 C53 1.512(13) . ? C49 C50 1.366(14) . ? C50 C51 1.341(14) . ? C51 C52 1.383(13) . ? C52 C56 1.531(13) . ? C53 C55 1.509(12) . ? C53 C54 1.546(14) . ? C56 C58 1.522(17) . ? C56 C57 1.612(17) . ? F1A C2A 1.380(11) . ? F2A C3A 1.331(11) . ? F3A C4A 1.361(11) . ? F4A C5A 1.373(11) . ? F5A C6A 1.371(9) . ? F6A C8A 1.351(9) . ? F7A C9A 1.359(9) . ? F8A C10A 1.348(10) . ? F9A C11A 1.353(10) . ? F10A C12A 1.376(9) . ? F11A C14A 1.349(10) . ? F12A C15A 1.347(11) . ? F13A C16A 1.351(12) . ? F14A C17A 1.363(12) . ? F15A C18A 1.361(11) . ? F16A C20A 1.367(10) . ? F17A C21A 1.343(11) . ? F18A C22A 1.340(11) . ? F19A C23A 1.361(10) . ? F20A C24A 1.359(9) . ? C1A C2A 1.365(12) . ? C1A C6A 1.398(13) . ? C1A B1A 1.659(13) . ? C2A C3A 1.373(14) . ? C3A C4A 1.408(15) . ? C4A C5A 1.345(13) . ? C5A C6A 1.350(12) . ? C7A C12A 1.385(11) . ? C7A C8A 1.389(11) . ? C7A B1A 1.653(13) . ? C8A C9A 1.402(12) . ? C9A C10A 1.350(12) . ? C10A C11A 1.355(13) . ? C11A C12A 1.362(13) . ? C13A C18A 1.370(12) . ? C13A C14A 1.380(12) . ? C13A B1A 1.663(14) . ? C14A C15A 1.423(13) . ? C15A C16A 1.324(15) . ? C16A C17A 1.375(17) . ? C17A C18A 1.390(15) . ? C19A C24A 1.381(11) . ? C19A C20A 1.385(12) . ? C19A B1A 1.658(13) . ? C20A C21A 1.373(13) . ? C21A C22A 1.391(14) . ? C22A C23A 1.350(14) . ? C23A C24A 1.369(13) . ? Tm1X N3X 2.226(6) . ? Tm1X N4X 2.230(6) . ? Tm1X N1X 2.238(6) . ? Tm1X N2X 2.241(6) . ? N1X C1X 1.365(9) . ? N1X C6X 1.446(10) . ? N2X C3X 1.328(10) . ? N2X C18X 1.442(10) . ? N3X C30X 1.334(11) . ? N3X C35X 1.454(11) . ? N4X C32X 1.345(11) . ? N4X C47X 1.474(11) . ? C1X C2X 1.380(11) . ? C1X C4X 1.522(11) . ? C2X C3X 1.428(11) . ? C3X C5X 1.515(11) . ? C6X C11X 1.405(12) . ? C6X C7X 1.424(12) . ? C7X C8X 1.378(12) . ? C7X C12X 1.523(13) . ? C8X C9X 1.373(14) . ? C9X C10X 1.355(13) . ? C10X C11X 1.391(12) . ? C11X C15X 1.532(12) . ? C12X C14X 1.484(15) . ? C12X C13X 1.550(13) . ? C15X C16X 1.527(15) . ? C15X C17X 1.535(13) . ? C18X C19X 1.403(12) . ? C18X C23X 1.408(12) . ? C19X C20X 1.386(14) . ? C19X C24X 1.543(13) . ? C20X C21X 1.387(15) . ? C21X C22X 1.379(15) . ? C22X C23X 1.409(13) . ? C23X C27X 1.482(12) . ? C24X C26X 1.496(14) . ? C24X C25X 1.499(14) . ? C27X C28X 1.483(13) . ? C27X C29X 1.553(13) . ? C30X C31X 1.423(12) . ? C30X C33X 1.516(11) . ? C31X C32X 1.391(12) . ? C32X C34X 1.515(12) . ? C35X C36X 1.389(14) . ? C35X C40X 1.409(13) . ? C36X C37X 1.414(14) . ? C36X C41X 1.506(15) . ? C37X C38X 1.404(17) . ? C38X C39X 1.370(17) . ? C39X C40X 1.391(13) . ? C40X C44X 1.513(14) . ? C41X C42X 1.535(16) . ? C41X C43X 1.549(15) . ? C44X C46X 1.529(13) . ? C44X C45X 1.561(14) . ? C47X C52X 1.368(14) . ? C47X C48X 1.412(14) . ? C48X C49X 1.362(15) . ? C48X C53X 1.520(17) . ? C49X C50X 1.32(2) . ? C50X C51X 1.42(2) . ? C51X C52X 1.424(14) . ? C52X C56X 1.529(17) . ? C53X C55X 1.542(17) . ? C53X C54X 1.557(17) . ? C56X C58X 1.53(2) . ? C56X C57X 1.552(16) . ? F1Y C2Y 1.364(10) . ? F2Y C3Y 1.350(10) . ? F3Y C4Y 1.355(10) . ? F4Y C5Y 1.351(10) . ? F5Y C6Y 1.365(9) . ? F6Y C8Y 1.341(9) . ? F7Y C9Y 1.353(9) . ? F8Y C10Y 1.372(9) . ? F9Y C11Y 1.359(10) . ? F10Y C12Y 1.366(9) . ? F11Y C14Y 1.355(10) . ? F12Y C15Y 1.354(11) . ? F13Y C16Y 1.352(10) . ? F14Y C17Y 1.353(10) . ? F15Y C18Y 1.345(9) . ? F16Y C20Y 1.352(10) . ? F17Y C21Y 1.363(11) . ? F18Y C22Y 1.377(11) . ? F19Y C23Y 1.355(10) . ? F20Y C24Y 1.358(9) . ? C1Y C6Y 1.391(11) . ? C1Y C2Y 1.393(11) . ? C1Y B1Y 1.643(12) . ? C2Y C3Y 1.391(12) . ? C3Y C4Y 1.367(13) . ? C4Y C5Y 1.345(13) . ? C5Y C6Y 1.378(12) . ? C7Y C8Y 1.372(11) . ? C7Y C12Y 1.388(11) . ? C7Y B1Y 1.658(11) . ? C8Y C9Y 1.406(11) . ? C9Y C10Y 1.359(12) . ? C10Y C11Y 1.335(12) . ? C11Y C12Y 1.375(11) . ? C13Y C18Y 1.378(11) . ? C13Y C14Y 1.390(11) . ? C13Y B1Y 1.655(12) . ? C14Y C15Y 1.370(13) . ? C15Y C16Y 1.367(14) . ? C16Y C17Y 1.371(13) . ? C17Y C18Y 1.368(12) . ? C19Y C24Y 1.384(11) . ? C19Y C20Y 1.388(12) . ? C19Y B1Y 1.658(12) . ? C20Y C21Y 1.392(13) . ? C21Y C22Y 1.323(14) . ? C22Y C23Y 1.345(13) . ? C23Y C24Y 1.379(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Tm N2 89.2(3) . . ? N1 Tm N3 116.1(3) . . ? N2 Tm N3 119.6(3) . . ? N1 Tm N4 128.1(3) . . ? N2 Tm N4 122.1(3) . . ? N3 Tm N4 85.2(2) . . ? C1 N1 C6 113.0(7) . . ? C1 N1 Tm 102.6(6) . . ? C6 N1 Tm 142.6(6) . . ? C3 N2 C18 119.9(8) . . ? C3 N2 Tm 110.1(7) . . ? C18 N2 Tm 128.7(6) . . ? C32 N3 C35 118.7(7) . . ? C32 N3 Tm 115.4(6) . . ? C35 N3 Tm 124.5(5) . . ? C30 N4 C47 117.3(7) . . ? C30 N4 Tm 109.7(5) . . ? C47 N4 Tm 132.2(6) . . ? N1 C1 C2 123.5(10) . . ? N1 C1 C4 118.8(10) . . ? C2 C1 C4 117.6(10) . . ? N1 C1 Tm 49.1(4) . . ? C2 C1 Tm 82.2(6) . . ? C4 C1 Tm 143.6(9) . . ? C1 C2 C3 131.9(11) . . ? N2 C3 C2 122.1(9) . . ? N2 C3 C5 122.9(11) . . ? C2 C3 C5 114.9(11) . . ? C7 C6 C11 122.4(9) . . ? C7 C6 N1 118.6(9) . . ? C11 C6 N1 119.0(9) . . ? C6 C7 C8 114.5(10) . . ? C6 C7 C12 124.6(9) . . ? C8 C7 C12 120.9(10) . . ? C9 C8 C7 122.6(11) . . ? C10 C9 C8 119.9(10) . . ? C9 C10 C11 122.6(11) . . ? C10 C11 C6 117.7(11) . . ? C10 C11 C15 119.1(10) . . ? C6 C11 C15 123.2(9) . . ? C13 C12 C7 113.2(10) . . ? C13 C12 C14 111.9(12) . . ? C7 C12 C14 111.9(10) . . ? C11 C15 C17 113.2(11) . . ? C11 C15 C16 112.4(11) . . ? C17 C15 C16 110.9(12) . . ? C23 C18 C19 121.4(12) . . ? C23 C18 N2 120.2(12) . . ? C19 C18 N2 118.3(10) . . ? C20 C19 C18 118.3(13) . . ? C20 C19 C24 120.3(13) . . ? C18 C19 C24 121.2(11) . . ? C19 C20 C21 119.4(18) . . ? C22 C21 C20 120.5(15) . . ? C23 C22 C21 121.1(14) . . ? C22 C23 C18 119.1(16) . . ? C22 C23 C27 118.4(13) . . ? C18 C23 C27 122.4(12) . . ? C19 C24 C26 112.5(12) . . ? C19 C24 C25 107.2(12) . . ? C26 C24 C25 112.5(11) . . ? C29 C27 C28 106.7(10) . . ? C29 C27 C23 113.9(13) . . ? C28 C27 C23 110.3(13) . . ? N4 C30 C31 123.8(8) . . ? N4 C30 C33 117.6(9) . . ? C31 C30 C33 118.5(9) . . ? C32 C31 C30 132.2(9) . . ? N3 C32 C31 124.4(9) . . ? N3 C32 C34 121.2(9) . . ? C31 C32 C34 114.4(9) . . ? C36 C35 C40 122.0(9) . . ? C36 C35 N3 116.6(8) . . ? C40 C35 N3 121.5(8) . . ? C35 C36 C37 117.6(10) . . ? C35 C36 C41 122.3(9) . . ? C37 C36 C41 119.7(10) . . ? C38 C37 C36 119.5(12) . . ? C39 C38 C37 122.8(12) . . ? C38 C39 C40 120.6(11) . . ? C39 C40 C35 117.4(10) . . ? C39 C40 C44 119.2(10) . . ? C35 C40 C44 123.4(9) . . ? C43 C41 C36 111.8(11) . . ? C43 C41 C42 110.4(12) . . ? C36 C41 C42 113.2(11) . . ? C46 C44 C40 110.9(9) . . ? C46 C44 C45 108.8(10) . . ? C40 C44 C45 113.6(10) . . ? C52 C47 C48 120.8(8) . . ? C52 C47 N4 120.9(8) . . ? C48 C47 N4 118.4(8) . . ? C49 C48 C47 117.1(9) . . ? C49 C48 C53 119.5(9) . . ? C47 C48 C53 123.4(8) . . ? C50 C49 C48 121.3(10) . . ? C51 C50 C49 119.2(10) . . ? C50 C51 C52 123.2(10) . . ? C47 C52 C51 118.2(9) . . ? C47 C52 C56 120.5(9) . . ? C51 C52 C56 121.3(10) . . ? C55 C53 C48 113.6(9) . . ? C55 C53 C54 106.7(8) . . ? C48 C53 C54 112.0(9) . . ? C58 C56 C52 111.6(10) . . ? C58 C56 C57 107.5(13) . . ? C52 C56 C57 106.8(9) . . ? C2A C1A C6A 112.4(8) . . ? C2A C1A B1A 127.5(9) . . ? C6A C1A B1A 119.5(8) . . ? C1A C2A C3A 126.0(10) . . ? C1A C2A F1A 120.8(9) . . ? C3A C2A F1A 113.1(9) . . ? F2A C3A C2A 123.4(12) . . ? F2A C3A C4A 119.5(10) . . ? C2A C3A C4A 117.1(10) . . ? C5A C4A F3A 120.6(11) . . ? C5A C4A C3A 119.6(9) . . ? F3A C4A C3A 119.8(9) . . ? C4A C5A C6A 119.7(10) . . ? C4A C5A F4A 119.3(9) . . ? C6A C5A F4A 121.0(9) . . ? C5A C6A F5A 116.2(9) . . ? C5A C6A C1A 125.1(9) . . ? F5A C6A C1A 118.7(8) . . ? C12A C7A C8A 111.9(8) . . ? C12A C7A B1A 120.2(7) . . ? C8A C7A B1A 127.5(7) . . ? F6A C8A C7A 121.2(8) . . ? F6A C8A C9A 116.0(7) . . ? C7A C8A C9A 122.8(8) . . ? C10A C9A F7A 120.8(8) . . ? C10A C9A C8A 120.7(8) . . ? F7A C9A C8A 118.5(9) . . ? F8A C10A C9A 119.2(9) . . ? F8A C10A C11A 121.9(9) . . ? C9A C10A C11A 118.9(9) . . ? F9A C11A C10A 120.7(9) . . ? F9A C11A C12A 120.3(9) . . ? C10A C11A C12A 118.9(9) . . ? C11A C12A F10A 115.6(8) . . ? C11A C12A C7A 126.5(8) . . ? F10A C12A C7A 117.8(8) . . ? C18A C13A C14A 112.4(9) . . ? C18A C13A B1A 120.2(8) . . ? C14A C13A B1A 127.2(8) . . ? F11A C14A C13A 122.0(8) . . ? F11A C14A C15A 114.0(9) . . ? C13A C14A C15A 124.0(9) . . ? C16A C15A F12A 121.6(10) . . ? C16A C15A C14A 119.7(11) . . ? F12A C15A C14A 118.7(9) . . ? C15A C16A F13A 121.2(12) . . ? C15A C16A C17A 119.4(11) . . ? F13A C16A C17A 119.3(12) . . ? F14A C17A C16A 121.3(12) . . ? F14A C17A C18A 119.7(13) . . ? C16A C17A C18A 118.9(10) . . ? F15A C18A C13A 119.2(9) . . ? F15A C18A C17A 115.3(10) . . ? C13A C18A C17A 125.4(10) . . ? C24A C19A C20A 112.4(8) . . ? C24A C19A B1A 120.1(8) . . ? C20A C19A B1A 127.2(8) . . ? F16A C20A C21A 114.7(8) . . ? F16A C20A C19A 120.4(9) . . ? C21A C20A C19A 124.8(9) . . ? F17A C21A C20A 121.1(10) . . ? F17A C21A C22A 119.8(9) . . ? C20A C21A C22A 119.1(9) . . ? F18A C22A C23A 122.0(10) . . ? F18A C22A C21A 119.5(10) . . ? C23A C22A C21A 118.5(9) . . ? C22A C23A F19A 119.1(9) . . ? C22A C23A C24A 119.9(9) . . ? F19A C23A C24A 120.9(9) . . ? F20A C24A C23A 116.1(8) . . ? F20A C24A C19A 118.7(8) . . ? C23A C24A C19A 125.2(9) . . ? C7A B1A C19A 112.5(7) . . ? C7A B1A C1A 102.1(7) . . ? C19A B1A C1A 115.3(7) . . ? C7A B1A C13A 113.1(7) . . ? C19A B1A C13A 101.3(7) . . ? C1A B1A C13A 113.0(7) . . ? N3X Tm1X N4X 88.8(2) . . ? N3X Tm1X N1X 115.8(2) . . ? N4X Tm1X N1X 129.5(3) . . ? N3X Tm1X N2X 116.7(2) . . ? N4X Tm1X N2X 119.7(2) . . ? N1X Tm1X N2X 89.1(2) . . ? C1X N1X C6X 117.5(6) . . ? C1X N1X Tm1X 100.9(5) . . ? C6X N1X Tm1X 140.0(5) . . ? C3X N2X C18X 118.5(7) . . ? C3X N2X Tm1X 107.7(5) . . ? C18X N2X Tm1X 131.8(5) . . ? C30X N3X C35X 118.3(7) . . ? C30X N3X Tm1X 110.7(5) . . ? C35X N3X Tm1X 129.6(5) . . ? C32X N4X C47X 116.1(7) . . ? C32X N4X Tm1X 105.3(5) . . ? C47X N4X Tm1X 137.0(5) . . ? N1X C1X C2X 124.9(7) . . ? N1X C1X C4X 119.4(7) . . ? C2X C1X C4X 115.7(7) . . ? N1X C1X Tm1X 50.9(4) . . ? C2X C1X Tm1X 82.5(5) . . ? C4X C1X Tm1X 146.6(6) . . ? C1X C2X C3X 132.3(8) . . ? N2X C3X C2X 123.3(7) . . ? N2X C3X C5X 122.4(8) . . ? C2X C3X C5X 114.2(7) . . ? C11X C6X C7X 120.3(8) . . ? C11X C6X N1X 118.0(7) . . ? C7X C6X N1X 121.7(8) . . ? C8X C7X C6X 117.5(9) . . ? C8X C7X C12X 121.4(8) . . ? C6X C7X C12X 121.1(8) . . ? C9X C8X C7X 122.8(9) . . ? C10X C9X C8X 118.8(9) . . ? C9X C10X C11X 122.7(9) . . ? C10X C11X C6X 117.8(8) . . ? C10X C11X C15X 118.9(8) . . ? C6X C11X C15X 123.3(8) . . ? C14X C12X C7X 112.4(8) . . ? C14X C12X C13X 111.1(10) . . ? C7X C12X C13X 110.1(9) . . ? C16X C15X C11X 112.0(9) . . ? C16X C15X C17X 109.0(8) . . ? C11X C15X C17X 111.4(8) . . ? C19X C18X C23X 121.7(8) . . ? C19X C18X N2X 120.4(8) . . ? C23X C18X N2X 118.0(8) . . ? C20X C19X C18X 119.5(9) . . ? C20X C19X C24X 117.4(9) . . ? C18X C19X C24X 123.0(9) . . ? C19X C20X C21X 119.7(10) . . ? C22X C21X C20X 120.7(10) . . ? C21X C22X C23X 121.6(10) . . ? C18X C23X C22X 116.7(9) . . ? C18X C23X C27X 123.5(8) . . ? C22X C23X C27X 119.5(9) . . ? C26X C24X C25X 110.0(9) . . ? C26X C24X C19X 110.5(9) . . ? C25X C24X C19X 112.4(9) . . ? C23X C27X C28X 111.0(8) . . ? C23X C27X C29X 113.1(9) . . ? C28X C27X C29X 110.3(9) . . ? N3X C30X C31X 122.9(8) . . ? N3X C30X C33X 122.4(8) . . ? C31X C30X C33X 114.7(8) . . ? C32X C31X C30X 133.1(9) . . ? N4X C32X C31X 124.2(8) . . ? N4X C32X C34X 121.1(8) . . ? C31X C32X C34X 114.7(8) . . ? C36X C35X C40X 122.3(10) . . ? C36X C35X N3X 117.0(9) . . ? C40X C35X N3X 120.6(9) . . ? C35X C36X C37X 118.6(11) . . ? C35X C36X C41X 122.9(10) . . ? C37X C36X C41X 118.3(11) . . ? C38X C37X C36X 119.3(13) . . ? C39X C38X C37X 120.3(11) . . ? C38X C39X C40X 122.2(12) . . ? C39X C40X C35X 117.2(11) . . ? C39X C40X C44X 119.0(10) . . ? C35X C40X C44X 123.8(9) . . ? C36X C41X C42X 115.1(11) . . ? C36X C41X C43X 110.7(10) . . ? C42X C41X C43X 109.1(10) . . ? C40X C44X C46X 109.9(9) . . ? C40X C44X C45X 112.4(9) . . ? C46X C44X C45X 110.1(9) . . ? C52X C47X C48X 121.3(9) . . ? C52X C47X N4X 121.0(9) . . ? C48X C47X N4X 117.6(9) . . ? C49X C48X C47X 119.1(13) . . ? C49X C48X C53X 117.2(12) . . ? C47X C48X C53X 123.6(9) . . ? C50X C49X C48X 122.0(16) . . ? C49X C50X C51X 120.6(12) . . ? C50X C51X C52X 119.1(13) . . ? C47X C52X C51X 117.9(12) . . ? C47X C52X C56X 124.2(9) . . ? C51X C52X C56X 117.8(11) . . ? C48X C53X C55X 114.2(12) . . ? C48X C53X C54X 113.5(11) . . ? C55X C53X C54X 107.6(11) . . ? C52X C56X C58X 112.3(10) . . ? C52X C56X C57X 111.3(13) . . ? C58X C56X C57X 109.8(13) . . ? C6Y C1Y C2Y 111.8(8) . . ? C6Y C1Y B1Y 122.3(7) . . ? C2Y C1Y B1Y 125.4(7) . . ? F1Y C2Y C3Y 115.4(8) . . ? F1Y C2Y C1Y 120.5(8) . . ? C3Y C2Y C1Y 124.1(9) . . ? F2Y C3Y C4Y 120.7(8) . . ? F2Y C3Y C2Y 119.9(9) . . ? C4Y C3Y C2Y 119.4(8) . . ? C5Y C4Y F3Y 120.2(10) . . ? C5Y C4Y C3Y 120.0(9) . . ? F3Y C4Y C3Y 119.7(9) . . ? C4Y C5Y F4Y 120.5(8) . . ? C4Y C5Y C6Y 118.7(9) . . ? F4Y C5Y C6Y 120.7(8) . . ? F5Y C6Y C5Y 115.6(8) . . ? F5Y C6Y C1Y 118.4(7) . . ? C5Y C6Y C1Y 126.0(8) . . ? C8Y C7Y C12Y 113.1(7) . . ? C8Y C7Y B1Y 124.1(7) . . ? C12Y C7Y B1Y 122.3(7) . . ? F6Y C8Y C7Y 121.9(7) . . ? F6Y C8Y C9Y 114.7(7) . . ? C7Y C8Y C9Y 123.4(8) . . ? F7Y C9Y C10Y 120.7(8) . . ? F7Y C9Y C8Y 119.9(8) . . ? C10Y C9Y C8Y 119.3(8) . . ? C11Y C10Y C9Y 119.8(8) . . ? C11Y C10Y F8Y 121.1(9) . . ? C9Y C10Y F8Y 119.1(9) . . ? C10Y C11Y F9Y 120.2(8) . . ? C10Y C11Y C12Y 119.8(8) . . ? F9Y C11Y C12Y 120.0(8) . . ? F10Y C12Y C11Y 115.7(8) . . ? F10Y C12Y C7Y 119.7(7) . . ? C11Y C12Y C7Y 124.6(8) . . ? C18Y C13Y C14Y 112.5(8) . . ? C18Y C13Y B1Y 122.4(7) . . ? C14Y C13Y B1Y 124.6(7) . . ? F11Y C14Y C15Y 114.7(8) . . ? F11Y C14Y C13Y 120.7(8) . . ? C15Y C14Y C13Y 124.5(9) . . ? F12Y C15Y C16Y 119.6(9) . . ? F12Y C15Y C14Y 120.6(9) . . ? C16Y C15Y C14Y 119.9(9) . . ? F13Y C16Y C15Y 121.5(10) . . ? F13Y C16Y C17Y 120.2(10) . . ? C15Y C16Y C17Y 118.3(9) . . ? F14Y C17Y C18Y 121.3(8) . . ? F14Y C17Y C16Y 118.9(9) . . ? C18Y C17Y C16Y 119.8(9) . . ? F15Y C18Y C17Y 115.4(8) . . ? F15Y C18Y C13Y 119.6(8) . . ? C17Y C18Y C13Y 125.0(8) . . ? C24Y C19Y C20Y 111.6(8) . . ? C24Y C19Y B1Y 126.8(7) . . ? C20Y C19Y B1Y 121.0(7) . . ? F16Y C20Y C19Y 119.8(8) . . ? F16Y C20Y C21Y 116.0(8) . . ? C19Y C20Y C21Y 124.1(9) . . ? C22Y C21Y F17Y 120.9(9) . . ? C22Y C21Y C20Y 120.1(9) . . ? F17Y C21Y C20Y 119.0(9) . . ? C21Y C22Y C23Y 119.6(9) . . ? C21Y C22Y F18Y 120.7(10) . . ? C23Y C22Y F18Y 119.7(10) . . ? C22Y C23Y F19Y 120.5(9) . . ? C22Y C23Y C24Y 119.7(9) . . ? F19Y C23Y C24Y 119.8(9) . . ? F20Y C24Y C23Y 115.6(8) . . ? F20Y C24Y C19Y 119.6(7) . . ? C23Y C24Y C19Y 124.8(8) . . ? C1Y B1Y C13Y 115.4(6) . . ? C1Y B1Y C19Y 100.9(6) . . ? C13Y B1Y C19Y 113.3(7) . . ? C1Y B1Y C7Y 113.0(7) . . ? C13Y B1Y C7Y 100.6(6) . . ? C19Y B1Y C7Y 114.3(6) . . ? #===END data_oct2102 _database_code_depnum_ccdc_archive 'CCDC 254751' _audit_creation_date 2002-10-25T11:53:57-00:00 _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 (Pb(Me3SiNCPhCHCPhNSiMe3)2) _chemical_formula_moiety 'C42 H58 N4 Pb1 Si4' _chemical_formula_sum 'C42 H58 N4 Pb Si4' _chemical_formula_weight 938.47 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3492(2) _cell_length_b 12.1384(2) _cell_length_c 16.5846(3) _cell_angle_alpha 89.975(1) _cell_angle_beta 97.414(1) _cell_angle_gamma 93.140(1) _cell_volume 2262.16(7) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14689 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.867 _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 0.5061 _exptl_absorpt_correction_T_max 0.6639 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_unetI/netI 0.044 _diffrn_reflns_number 20341 _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 -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.947 _diffrn_measured_fraction_theta_max 0.947 _reflns_number_total 8131 _reflns_number_gt 7692 _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^)+(0.0406P)^2^+1.9839P] 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 8131 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.05 _refine_diff_density_min -2.237 _refine_diff_density_rms 0.1 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb Pb 0.608649(11) 0.646830(10) 0.739034(7) 0.02885(6) Uani 1 1 d . . . Si1 Si 0.74470(11) 0.57666(9) 0.93077(6) 0.0391(3) Uani 1 1 d . . . Si2 Si 0.34528(11) 0.77406(11) 0.79415(9) 0.0496(3) Uani 1 1 d . . . Si3 Si 0.65653(11) 0.84158(9) 0.59050(6) 0.0374(2) Uani 1 1 d . . . Si4 Si 0.71881(10) 0.37943(9) 0.66656(7) 0.0396(3) Uani 1 1 d . . . N1 N 0.7176(3) 0.6884(2) 0.86419(18) 0.0306(7) Uani 1 1 d . . . N2 N 0.4968(3) 0.8032(3) 0.79070(19) 0.0335(7) Uani 1 1 d . . . N3 N 0.7263(3) 0.7666(2) 0.67108(17) 0.0273(6) Uani 1 1 d . . . N4 N 0.7717(3) 0.5138(2) 0.69871(19) 0.0309(7) Uani 1 1 d . . . C1 C 0.7466(3) 0.7952(3) 0.8842(2) 0.0310(8) Uani 1 1 d . . . C2 C 0.6847(3) 0.8866(3) 0.8551(2) 0.0313(8) Uani 1 1 d . . . H2 H 0.7291 0.9555 0.8589 0.038 Uiso 1 1 calc R . . C3 C 0.5643(3) 0.8890(3) 0.8208(2) 0.0316(8) Uani 1 1 d . . . C4 C 0.8532(4) 0.8213(3) 0.9463(2) 0.0345(8) Uani 1 1 d . . . C5 C 0.9621(4) 0.7797(4) 0.9373(3) 0.0441(10) Uani 1 1 d . . . H5 H 0.9707 0.7368 0.8907 0.053 Uiso 1 1 calc R . . C6 C 1.0591(4) 0.8012(4) 0.9970(3) 0.0564(12) Uani 1 1 d . . . H6 H 1.134 0.7733 0.9907 0.068 Uiso 1 1 calc R . . C7 C 1.0472(5) 0.8622(4) 1.0647(3) 0.0603(14) Uani 1 1 d . . . H7 H 1.1135 0.8751 1.1054 0.072 Uiso 1 1 calc R . . C8 C 0.9405(5) 0.9047(4) 1.0741(3) 0.0595(13) Uani 1 1 d . . . H8 H 0.9327 0.9472 1.121 0.071 Uiso 1 1 calc R . . C9 C 0.8438(4) 0.8852(3) 1.0147(3) 0.0466(10) Uani 1 1 d . . . H9 H 0.7701 0.9158 1.0207 0.056 Uiso 1 1 calc R . . C10 C 0.5131(4) 1.0007(3) 0.8227(2) 0.0355(8) Uani 1 1 d . . . C11 C 0.5295(4) 1.0661(4) 0.8931(3) 0.0482(10) Uani 1 1 d . . . H11 H 0.5746 1.0406 0.941 0.058 Uiso 1 1 calc R . . C12 C 0.4799(5) 1.1680(4) 0.8931(4) 0.0649(14) Uani 1 1 d . . . H12 H 0.4896 1.2111 0.9415 0.078 Uiso 1 1 calc R . . C13 C 0.4166(5) 1.2073(4) 0.8235(4) 0.0620(14) Uani 1 1 d . . . H13 H 0.3842 1.2778 0.8238 0.074 Uiso 1 1 calc R . . C14 C 0.4005(5) 1.1451(4) 0.7541(3) 0.0568(12) Uani 1 1 d . . . H14 H 0.3572 1.1722 0.706 0.068 Uiso 1 1 calc R . . C15 C 0.4482(4) 1.0409(4) 0.7541(3) 0.0444(10) Uani 1 1 d . . . H15 H 0.4355 0.9973 0.7059 0.053 Uiso 1 1 calc R . . C16 C 0.6117(5) 0.4779(4) 0.9073(3) 0.0642(14) Uani 1 1 d . . . H16A H 0.5397 0.5147 0.9163 0.096 Uiso 1 1 calc R . . H16B H 0.6207 0.4137 0.9428 0.096 Uiso 1 1 calc R . . H16C H 0.6052 0.4539 0.8504 0.096 Uiso 1 1 calc R . . C17 C 0.7555(7) 0.6155(4) 1.0403(3) 0.0721(18) Uani 1 1 d . . . H17A H 0.6851 0.6546 1.0496 0.108 Uiso 1 1 calc R . . H17B H 0.8271 0.6636 1.0554 0.108 Uiso 1 1 calc R . . H17C H 0.7598 0.5487 1.0736 0.108 Uiso 1 1 calc R . . C18 C 0.8773(5) 0.5025(4) 0.9127(3) 0.0606(13) Uani 1 1 d . . . H18A H 0.8711 0.4819 0.8552 0.091 Uiso 1 1 calc R . . H18B H 0.8819 0.4359 0.9461 0.091 Uiso 1 1 calc R . . H18C H 0.9491 0.5506 0.9274 0.091 Uiso 1 1 calc R . . C19 C 0.3342(8) 0.6628(10) 0.8646(11) 0.258(10) Uani 1 1 d . . . H19A H 0.3847 0.604 0.8517 0.387 Uiso 1 1 calc R . . H19B H 0.2513 0.6337 0.8607 0.387 Uiso 1 1 calc R . . H19C H 0.3604 0.6899 0.9201 0.387 Uiso 1 1 calc R . . C20 C 0.2492(6) 0.8829(6) 0.8203(5) 0.099(2) Uani 1 1 d . . . H20A H 0.2547 0.9447 0.7826 0.148 Uiso 1 1 calc R . . H20B H 0.2753 0.9087 0.876 0.148 Uiso 1 1 calc R . . H20C H 0.1666 0.8532 0.816 0.148 Uiso 1 1 calc R . . C21 C 0.2742(7) 0.7190(14) 0.6942(8) 0.235(9) Uani 1 1 d . . . H21A H 0.2777 0.7765 0.653 0.352 Uiso 1 1 calc R . . H21B H 0.191 0.696 0.6979 0.352 Uiso 1 1 calc R . . H21C H 0.3165 0.6555 0.6791 0.352 Uiso 1 1 calc R . . C22 C 0.8462(3) 0.7637(3) 0.6859(2) 0.0290(7) Uani 1 1 d . . . C23 C 0.9127(3) 0.6741(3) 0.7075(2) 0.0331(8) Uani 1 1 d . . . H23 H 0.9924 0.6911 0.7311 0.04 Uiso 1 1 calc R . . C24 C 0.8780(3) 0.5579(3) 0.6993(2) 0.0300(8) Uani 1 1 d . . . C25 C 0.9191(3) 0.8678(3) 0.6723(2) 0.0323(8) Uani 1 1 d . . . C26 C 0.9993(4) 0.8697(4) 0.6153(3) 0.0481(11) Uani 1 1 d . . . H26 H 1.0099 0.8044 0.5862 0.058 Uiso 1 1 calc R . . C27 C 1.0638(5) 0.9669(4) 0.6011(3) 0.0606(13) Uani 1 1 d . . . H27 H 1.1163 0.9685 0.5608 0.073 Uiso 1 1 calc R . . C28 C 1.0518(4) 1.0609(4) 0.6451(3) 0.0537(12) Uani 1 1 d . . . H28 H 1.0959 1.1272 0.6352 0.064 Uiso 1 1 calc R . . C29 C 0.9759(4) 1.0587(3) 0.7034(3) 0.0487(11) Uani 1 1 d . . . H29 H 0.9692 1.1228 0.7349 0.058 Uiso 1 1 calc R . . C30 C 0.9086(4) 0.9621(3) 0.7161(3) 0.0409(9) Uani 1 1 d . . . H30 H 0.8548 0.9615 0.7556 0.049 Uiso 1 1 calc R . . C31 C 0.9830(3) 0.4909(3) 0.6865(2) 0.0341(8) Uani 1 1 d . . . C32 C 1.0240(4) 0.4108(3) 0.7418(3) 0.0419(10) Uani 1 1 d . . . H32 H 0.9844 0.3961 0.7881 0.05 Uiso 1 1 calc R . . C33 C 1.1219(4) 0.3522(4) 0.7301(3) 0.0492(11) Uani 1 1 d . . . H33 H 1.1497 0.2987 0.7687 0.059 Uiso 1 1 calc R . . C34 C 1.1786(4) 0.3712(4) 0.6631(3) 0.0551(12) Uani 1 1 d . . . H34 H 1.2463 0.3317 0.6556 0.066 Uiso 1 1 calc R . . C35 C 1.1373(5) 0.4479(4) 0.6068(3) 0.0610(13) Uani 1 1 d . . . H35 H 1.1746 0.4591 0.5591 0.073 Uiso 1 1 calc R . . C36 C 1.0415(4) 0.5087(4) 0.6194(3) 0.0492(11) Uani 1 1 d . . . H36 H 1.0157 0.5635 0.5812 0.059 Uiso 1 1 calc R . . C37 C 0.4969(4) 0.7939(4) 0.5764(3) 0.0574(12) Uani 1 1 d . . . H37A H 0.4616 0.8102 0.6256 0.086 Uiso 1 1 calc R . . H37B H 0.4897 0.7142 0.566 0.086 Uiso 1 1 calc R . . H37C H 0.4552 0.8322 0.53 0.086 Uiso 1 1 calc R . . C38 C 0.7188(6) 0.8083(6) 0.4951(3) 0.0794(18) Uani 1 1 d . . . H38A H 0.8032 0.8328 0.5006 0.119 Uiso 1 1 calc R . . H38B H 0.6754 0.8462 0.4493 0.119 Uiso 1 1 calc R . . H38C H 0.7104 0.7285 0.4854 0.119 Uiso 1 1 calc R . . C39 C 0.6623(5) 0.9951(4) 0.6040(4) 0.0724(17) Uani 1 1 d . . . H39A H 0.7454 1.0237 0.6116 0.109 Uiso 1 1 calc R . . H39B H 0.6246 1.0134 0.6519 0.109 Uiso 1 1 calc R . . H39C H 0.6199 1.0285 0.5557 0.109 Uiso 1 1 calc R . . C40 C 0.5566(5) 0.3874(5) 0.6330(4) 0.0708(16) Uani 1 1 d . . . H40A H 0.5181 0.4161 0.6777 0.106 Uiso 1 1 calc R . . H40B H 0.5217 0.3136 0.6175 0.106 Uiso 1 1 calc R . . H40C H 0.5445 0.4368 0.5863 0.106 Uiso 1 1 calc R . . C41 C 0.7885(5) 0.3247(4) 0.5804(3) 0.0591(13) Uani 1 1 d . . . H41A H 0.874 0.3195 0.5969 0.089 Uiso 1 1 calc R . . H41B H 0.7757 0.3744 0.5339 0.089 Uiso 1 1 calc R . . H41C H 0.7523 0.2513 0.565 0.089 Uiso 1 1 calc R . . C42 C 0.7354(5) 0.2780(4) 0.7517(3) 0.0584(13) Uani 1 1 d . . . H42A H 0.699 0.3057 0.7977 0.088 Uiso 1 1 calc R . . H42B H 0.82 0.2682 0.7688 0.088 Uiso 1 1 calc R . . H42C H 0.6957 0.2071 0.7332 0.088 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 Pb 0.02718(9) 0.02177(9) 0.03679(10) 0.00069(6) 0.00203(6) -0.00088(6) Si1 0.0595(7) 0.0257(5) 0.0327(5) 0.0041(4) 0.0056(5) 0.0091(5) Si2 0.0308(6) 0.0422(7) 0.0781(9) -0.0030(6) 0.0161(6) 0.0016(5) Si3 0.0431(6) 0.0354(6) 0.0315(5) 0.0077(4) -0.0040(4) 0.0037(5) Si4 0.0379(6) 0.0238(5) 0.0559(7) -0.0075(5) 0.0027(5) -0.0019(5) N1 0.0379(17) 0.0217(15) 0.0326(16) 0.0016(12) 0.0047(13) 0.0055(13) N2 0.0295(16) 0.0279(16) 0.0437(18) -0.0003(13) 0.0057(13) 0.0051(13) N3 0.0285(15) 0.0202(14) 0.0327(15) 0.0036(11) 0.0020(12) 0.0013(12) N4 0.0287(16) 0.0208(14) 0.0423(17) -0.0021(12) 0.0002(13) 0.0039(13) C1 0.0320(19) 0.0283(19) 0.0333(19) 0.0013(14) 0.0077(15) -0.0009(15) C2 0.036(2) 0.0201(17) 0.038(2) -0.0018(14) 0.0060(16) 0.0012(15) C3 0.035(2) 0.0290(19) 0.0326(19) 0.0013(15) 0.0080(15) 0.0071(16) C4 0.039(2) 0.0275(19) 0.037(2) 0.0016(15) 0.0031(16) 0.0019(16) C5 0.039(2) 0.047(2) 0.046(2) 0.0057(19) 0.0022(18) 0.0032(19) C6 0.038(2) 0.057(3) 0.071(3) 0.016(2) -0.002(2) -0.001(2) C7 0.063(3) 0.052(3) 0.055(3) 0.008(2) -0.023(2) -0.014(3) C8 0.079(4) 0.046(3) 0.049(3) -0.005(2) -0.012(2) 0.002(3) C9 0.058(3) 0.035(2) 0.045(2) -0.0015(18) -0.003(2) 0.005(2) C10 0.038(2) 0.0264(19) 0.044(2) 0.0020(16) 0.0103(17) 0.0054(17) C11 0.055(3) 0.038(2) 0.052(3) -0.0067(19) 0.006(2) 0.011(2) C12 0.077(4) 0.043(3) 0.077(4) -0.020(2) 0.017(3) 0.014(3) C13 0.064(3) 0.035(2) 0.091(4) 0.003(2) 0.021(3) 0.021(2) C14 0.060(3) 0.045(3) 0.068(3) 0.014(2) 0.011(2) 0.022(2) C15 0.049(3) 0.035(2) 0.052(2) 0.0033(18) 0.0094(19) 0.0149(19) C16 0.081(4) 0.034(2) 0.077(3) 0.023(2) 0.013(3) -0.007(2) C17 0.140(6) 0.042(3) 0.038(2) 0.004(2) 0.025(3) 0.007(3) C18 0.074(3) 0.053(3) 0.054(3) 0.005(2) -0.007(2) 0.033(3) C19 0.080(6) 0.214(12) 0.51(2) 0.281(16) 0.129(10) 0.067(7) C20 0.062(4) 0.073(4) 0.175(7) -0.001(4) 0.060(4) 0.010(3) C21 0.036(4) 0.43(2) 0.232(12) -0.220(15) 0.030(6) -0.059(8) C22 0.0319(19) 0.0222(17) 0.0325(18) 0.0006(14) 0.0037(14) 0.0005(15) C23 0.0284(19) 0.0241(18) 0.046(2) 0.0017(15) -0.0006(15) 0.0016(15) C24 0.0277(18) 0.0271(18) 0.0341(19) 0.0027(14) -0.0012(14) 0.0050(15) C25 0.0314(19) 0.0250(18) 0.039(2) 0.0040(15) 0.0027(15) -0.0022(15) C26 0.053(3) 0.038(2) 0.055(3) -0.0033(19) 0.017(2) -0.005(2) C27 0.068(3) 0.051(3) 0.066(3) 0.004(2) 0.027(3) -0.014(3) C28 0.055(3) 0.034(2) 0.070(3) 0.012(2) 0.008(2) -0.019(2) C29 0.058(3) 0.025(2) 0.062(3) -0.0022(18) 0.005(2) -0.0063(19) C30 0.045(2) 0.031(2) 0.047(2) 0.0020(17) 0.0092(18) -0.0023(18) C31 0.031(2) 0.0244(18) 0.046(2) -0.0018(15) 0.0022(16) 0.0050(16) C32 0.047(2) 0.031(2) 0.048(2) 0.0075(17) 0.0022(19) 0.0130(19) C33 0.050(3) 0.039(2) 0.058(3) 0.001(2) -0.002(2) 0.021(2) C34 0.048(3) 0.046(3) 0.075(3) 0.000(2) 0.012(2) 0.024(2) C35 0.063(3) 0.054(3) 0.074(3) 0.008(2) 0.030(3) 0.022(3) C36 0.052(3) 0.044(2) 0.055(3) 0.010(2) 0.011(2) 0.019(2) C37 0.047(3) 0.066(3) 0.053(3) 0.011(2) -0.017(2) 0.005(2) C38 0.088(4) 0.114(5) 0.035(3) 0.000(3) 0.009(3) -0.003(4) C39 0.076(4) 0.037(3) 0.097(4) 0.021(3) -0.021(3) 0.014(3) C40 0.049(3) 0.050(3) 0.105(4) -0.026(3) -0.014(3) -0.011(2) C41 0.070(3) 0.043(3) 0.063(3) -0.017(2) 0.010(2) -0.008(2) C42 0.074(4) 0.031(2) 0.072(3) 0.002(2) 0.019(3) -0.004(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 Pb N3 2.311(3) . ? Pb N1 2.315(3) . ? Pb N2 2.548(3) . ? Pb N4 2.669(3) . ? Si1 N1 1.763(3) . ? Si1 C18 1.852(5) . ? Si1 C17 1.864(5) . ? Si1 C16 1.876(6) . ? Si2 N2 1.745(3) . ? Si2 C19 1.796(8) . ? Si2 C20 1.844(6) . ? Si2 C21 1.854(9) . ? Si3 N3 1.746(3) . ? Si3 C37 1.856(5) . ? Si3 C38 1.867(6) . ? Si3 C39 1.874(5) . ? Si4 N4 1.766(3) . ? Si4 C41 1.860(5) . ? Si4 C40 1.861(5) . ? Si4 C42 1.871(5) . ? N1 C1 1.351(5) . ? N2 C3 1.317(5) . ? N3 C22 1.353(5) . ? N4 C24 1.291(5) . ? C1 C2 1.398(5) . ? C1 C4 1.504(5) . ? C2 C3 1.413(5) . ? C3 C10 1.507(5) . ? C4 C5 1.386(6) . ? C4 C9 1.393(6) . ? C5 C6 1.396(6) . ? C6 C7 1.370(8) . ? C7 C8 1.369(8) . ? C8 C9 1.387(6) . ? C10 C15 1.378(6) . ? C10 C11 1.398(6) . ? C11 C12 1.387(7) . ? C12 C13 1.379(8) . ? C13 C14 1.363(7) . ? C14 C15 1.402(6) . ? C22 C23 1.378(5) . ? C22 C25 1.505(5) . ? C23 C24 1.446(5) . ? C24 C31 1.516(5) . ? C25 C30 1.375(6) . ? C25 C26 1.393(6) . ? C26 C27 1.391(6) . ? C27 C28 1.377(7) . ? C28 C29 1.375(7) . ? C29 C30 1.395(6) . ? C31 C36 1.379(6) . ? C31 C32 1.393(5) . ? C32 C33 1.385(6) . ? C33 C34 1.367(7) . ? C34 C35 1.375(7) . ? C35 C36 1.385(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 N3 Pb N1 92.87(10) . . ? N3 Pb N2 92.66(10) . . ? N1 Pb N2 77.49(10) . . ? N3 Pb N4 78.45(10) . . ? N1 Pb N4 92.29(10) . . ? N2 Pb N4 166.20(10) . . ? N1 Si1 C18 113.0(2) . . ? N1 Si1 C17 113.59(19) . . ? C18 Si1 C17 109.7(3) . . ? N1 Si1 C16 105.2(2) . . ? C18 Si1 C16 107.3(3) . . ? C17 Si1 C16 107.5(3) . . ? N2 Si2 C19 106.5(3) . . ? N2 Si2 C20 120.6(3) . . ? C19 Si2 C20 108.3(5) . . ? N2 Si2 C21 109.6(3) . . ? C19 Si2 C21 105.7(8) . . ? C20 Si2 C21 105.1(5) . . ? N3 Si3 C37 107.06(19) . . ? N3 Si3 C38 109.6(2) . . ? C37 Si3 C38 107.5(3) . . ? N3 Si3 C39 116.4(2) . . ? C37 Si3 C39 106.8(3) . . ? C38 Si3 C39 109.0(3) . . ? N4 Si4 C41 114.6(2) . . ? N4 Si4 C40 106.1(2) . . ? C41 Si4 C40 108.2(3) . . ? N4 Si4 C42 112.1(2) . . ? C41 Si4 C42 108.4(2) . . ? C40 Si4 C42 107.1(3) . . ? C1 N1 Si1 124.4(3) . . ? C1 N1 Pb 118.9(2) . . ? Si1 N1 Pb 116.37(15) . . ? C3 N2 Si2 128.8(3) . . ? C3 N2 Pb 115.1(2) . . ? Si2 N2 Pb 115.50(16) . . ? C22 N3 Si3 121.9(2) . . ? C22 N3 Pb 119.5(2) . . ? Si3 N3 Pb 117.80(15) . . ? C24 N4 Si4 127.6(3) . . ? C24 N4 Pb 116.1(2) . . ? Si4 N4 Pb 116.04(15) . . ? N1 C1 C2 126.6(4) . . ? N1 C1 C4 118.4(3) . . ? C2 C1 C4 115.0(3) . . ? C1 C2 C3 127.9(3) . . ? N2 C3 C2 125.5(3) . . ? N2 C3 C10 120.1(3) . . ? C2 C3 C10 114.4(3) . . ? C5 C4 C9 118.9(4) . . ? C5 C4 C1 120.3(4) . . ? C9 C4 C1 120.8(4) . . ? C4 C5 C6 119.6(4) . . ? C7 C6 C5 120.5(5) . . ? C8 C7 C6 120.6(5) . . ? C7 C8 C9 119.5(5) . . ? C8 C9 C4 120.9(5) . . ? C15 C10 C11 118.3(4) . . ? C15 C10 C3 120.1(4) . . ? C11 C10 C3 121.6(4) . . ? C12 C11 C10 120.1(4) . . ? C13 C12 C11 120.6(5) . . ? C14 C13 C12 120.0(4) . . ? C13 C14 C15 119.7(5) . . ? C10 C15 C14 121.1(4) . . ? N3 C22 C23 128.0(3) . . ? N3 C22 C25 117.7(3) . . ? C23 C22 C25 114.2(3) . . ? C22 C23 C24 129.0(4) . . ? N4 C24 C23 126.3(3) . . ? N4 C24 C31 122.5(3) . . ? C23 C24 C31 111.2(3) . . ? C30 C25 C26 118.9(4) . . ? C30 C25 C22 120.8(3) . . ? C26 C25 C22 120.3(3) . . ? C27 C26 C25 120.2(4) . . ? C28 C27 C26 120.2(4) . . ? C29 C28 C27 119.9(4) . . ? C28 C29 C30 119.9(4) . . ? C25 C30 C29 120.8(4) . . ? C36 C31 C32 118.1(4) . . ? C36 C31 C24 120.4(3) . . ? C32 C31 C24 121.6(4) . . ? C33 C32 C31 120.7(4) . . ? C34 C33 C32 120.3(4) . . ? C33 C34 C35 119.8(4) . . ? C34 C35 C36 120.1(5) . . ? C31 C36 C35 121.0(4) . . ? #===END data_apr1504 _database_code_depnum_ccdc_archive 'CCDC 254752' _audit_creation_date 2004-04-15T15:35:39-00:00 _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 'C42 H57 N4 Si4 Yb1' _chemical_formula_sum 'C42 H57 N4 Si4 Yb1' _chemical_formula_weight 903.32 _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 11.2608(1) _cell_length_b 12.8457(2) _cell_length_c 16.0891(3) _cell_angle_alpha 89.620(1) _cell_angle_beta 86.087(1) _cell_angle_gamma 79.121(1) _cell_volume 2280.13(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23658 _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 orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.187 _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 0.4099 _exptl_absorpt_correction_T_max 0.4918 #----------------------------------------------------------------------------# # 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 -0.42113E-2 _diffrn_orient_matrix_ub_12 0.781373E-1 _diffrn_orient_matrix_ub_13 0.54362E-2 _diffrn_orient_matrix_ub_21 -0.615962E-1 _diffrn_orient_matrix_ub_22 0.25252E-2 _diffrn_orient_matrix_ub_23 0.481157E-1 _diffrn_orient_matrix_ub_31 0.663609E-1 _diffrn_orient_matrix_ub_32 -0.131314E-1 _diffrn_orient_matrix_ub_33 0.392003E-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 0.036 _diffrn_reflns_av_unetI/netI 0.0246 _diffrn_reflns_number 35033 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 8023 _reflns_number_gt 7714 _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 two H atoms on C19 were refined; other H atoms were in riding mode. 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^)+(0.0233P)^2^+2.1814P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8023 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.85 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 '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 Yb Yb 0.288433(9) 0.706929(8) 0.767027(6) 0.01779(4) Uani 1 1 d . . . Si1 Si 0.59940(7) 0.67039(6) 0.75466(5) 0.02746(16) Uani 1 1 d . . . Si2 Si 0.22859(7) 0.54618(6) 0.64114(5) 0.02678(16) Uani 1 1 d . . . Si3 Si 0.18543(7) 0.64944(6) 0.98289(5) 0.02905(17) Uani 1 1 d . . . Si4 Si 0.02910(6) 0.91360(6) 0.72333(4) 0.02331(15) Uani 1 1 d . . . N1 N 0.46913(18) 0.73020(17) 0.70655(12) 0.0214(4) Uani 1 1 d . . . N2 N 0.26010(18) 0.67543(17) 0.63059(12) 0.0220(4) Uani 1 1 d . . . N3 N 0.2582(2) 0.72427(16) 0.91125(12) 0.0239(5) Uani 1 1 d . . . N4 N 0.16582(18) 0.86922(16) 0.77099(12) 0.0199(4) Uani 1 1 d . . . C1 C 0.4674(2) 0.7900(2) 0.63732(15) 0.0218(5) Uani 1 1 d . . . C2 C 0.3846(2) 0.7955(2) 0.57584(15) 0.0233(5) Uani 1 1 d . . . H2 H 0.3859 0.8495 0.5353 0.028 Uiso 1 1 calc R . . C3 C 0.2988(2) 0.72902(19) 0.56772(15) 0.0212(5) Uani 1 1 d . . . C4 C 0.5600(2) 0.8590(2) 0.62149(15) 0.0234(5) Uani 1 1 d . . . C5 C 0.5650(2) 0.9395(2) 0.67756(17) 0.0278(6) Uani 1 1 d . . . H5 H 0.5143 0.9466 0.7277 0.033 Uiso 1 1 calc R . . C6 C 0.6435(3) 1.0098(2) 0.66108(18) 0.0318(6) Uani 1 1 d . . . H6 H 0.6445 1.0658 0.6991 0.038 Uiso 1 1 calc R . . C7 C 0.7198(2) 0.9984(2) 0.58963(18) 0.0314(6) Uani 1 1 d . . . H7 H 0.7733 1.0465 0.5783 0.038 Uiso 1 1 calc R . . C8 C 0.7179(3) 0.9169(3) 0.53484(18) 0.0387(7) Uani 1 1 d . . . H8 H 0.7724 0.9074 0.4865 0.046 Uiso 1 1 calc R . . C9 C 0.6372(3) 0.8488(2) 0.54973(18) 0.0364(7) Uani 1 1 d . . . H9 H 0.6346 0.7945 0.5105 0.044 Uiso 1 1 calc R . . C10 C 0.2517(2) 0.72312(19) 0.48346(15) 0.0239(5) Uani 1 1 d . . . C11 C 0.3283(3) 0.7156(2) 0.41095(16) 0.0338(6) Uani 1 1 d . . . H11 H 0.4126 0.7132 0.4145 0.041 Uiso 1 1 calc R . . C12 C 0.2814(4) 0.7116(3) 0.33352(18) 0.0467(9) Uani 1 1 d . . . H12 H 0.3342 0.7047 0.2844 0.056 Uiso 1 1 calc R . . C13 C 0.1590(4) 0.7174(3) 0.32767(19) 0.0504(9) Uani 1 1 d . . . H13 H 0.1275 0.7152 0.2746 0.06 Uiso 1 1 calc R . . C14 C 0.0823(3) 0.7265(2) 0.3984(2) 0.0436(8) Uani 1 1 d . . . H14 H -0.0023 0.7315 0.3941 0.052 Uiso 1 1 calc R . . C15 C 0.1282(3) 0.7284(2) 0.47637(17) 0.0310(6) Uani 1 1 d . . . H15 H 0.0748 0.7333 0.5251 0.037 Uiso 1 1 calc R . . C16 C 0.7226(3) 0.6104(3) 0.6765(2) 0.0453(8) Uani 1 1 d . . . H16C H 0.7534 0.6668 0.6455 0.068 Uiso 1 1 calc R . . H16B H 0.6907 0.5657 0.6377 0.068 Uiso 1 1 calc R . . H16A H 0.7886 0.5671 0.7051 0.068 Uiso 1 1 calc R . . C17 C 0.6564(3) 0.7560(3) 0.83000(19) 0.0397(7) Uani 1 1 d . . . H17C H 0.7217 0.7131 0.8595 0.06 Uiso 1 1 calc R . . H17B H 0.59 0.7869 0.8702 0.06 Uiso 1 1 calc R . . H17A H 0.6874 0.8129 0.7998 0.06 Uiso 1 1 calc R . . C18 C 0.5480(3) 0.5596(3) 0.8153(2) 0.0411(7) Uani 1 1 d . . . H18C H 0.5182 0.5128 0.7772 0.062 Uiso 1 1 calc R . . H18B H 0.4828 0.5891 0.8568 0.062 Uiso 1 1 calc R . . H18A H 0.6163 0.5192 0.8435 0.062 Uiso 1 1 calc R . . C19 C 0.2298(3) 0.5373(2) 0.75483(17) 0.0315(6) Uani 1 1 d . . . H19B H 0.287(4) 0.476(3) 0.775(3) 0.071(12) Uiso 1 1 d . . . H19A H 0.147(3) 0.532(3) 0.783(2) 0.054(10) Uiso 1 1 d . . . C20 C 0.0875(3) 0.5226(3) 0.5969(2) 0.0516(9) Uani 1 1 d . . . H20C H 0.0749 0.451 0.6114 0.077 Uiso 1 1 calc R . . H20B H 0.095 0.5294 0.5362 0.077 Uiso 1 1 calc R . . H20A H 0.0184 0.5748 0.6199 0.077 Uiso 1 1 calc R . . C21 C 0.3591(4) 0.4584(3) 0.5846(2) 0.0544(9) Uani 1 1 d . . . H21C H 0.435 0.477 0.6004 0.082 Uiso 1 1 calc R . . H21B H 0.353 0.4676 0.5244 0.082 Uiso 1 1 calc R . . H21A H 0.358 0.3844 0.5991 0.082 Uiso 1 1 calc R . . C22 C 0.3117(2) 0.8064(2) 0.92539(15) 0.0230(5) Uani 1 1 d . . . C23 C 0.3140(2) 0.8914(2) 0.86930(15) 0.0234(5) Uani 1 1 d . . . H23 H 0.3792 0.9281 0.8729 0.028 Uiso 1 1 calc R . . C24 C 0.2311(2) 0.9288(2) 0.80827(15) 0.0215(5) Uani 1 1 d . . . C25 C 0.3763(2) 0.8148(2) 1.00318(15) 0.0244(5) Uani 1 1 d . . . C26 C 0.4523(3) 0.7271(2) 1.03368(17) 0.0327(6) Uani 1 1 d . . . H26 H 0.4616 0.6606 1.0061 0.039 Uiso 1 1 calc R . . C27 C 0.5147(3) 0.7356(3) 1.10403(18) 0.0384(7) Uani 1 1 d . . . H27 H 0.5671 0.6752 1.124 0.046 Uiso 1 1 calc R . . C28 C 0.5009(3) 0.8315(3) 1.14496(18) 0.0401(7) Uani 1 1 d . . . H28 H 0.5434 0.8373 1.1932 0.048 Uiso 1 1 calc R . . C29 C 0.4252(3) 0.9190(3) 1.11549(18) 0.0392(7) Uani 1 1 d . . . H29 H 0.4149 0.985 1.1439 0.047 Uiso 1 1 calc R . . C30 C 0.3642(3) 0.9109(2) 1.04486(17) 0.0327(6) Uani 1 1 d . . . H30 H 0.3133 0.972 1.0245 0.039 Uiso 1 1 calc R . . C31 C 0.2211(2) 1.0441(2) 0.78810(16) 0.0233(5) Uani 1 1 d . . . C32 C 0.1834(3) 1.1216(2) 0.84945(19) 0.0343(6) Uani 1 1 d . . . H32 H 0.1646 1.1012 0.9049 0.041 Uiso 1 1 calc R . . C33 C 0.1733(3) 1.2277(2) 0.8305(2) 0.0436(8) Uani 1 1 d . . . H33 H 0.1462 1.2799 0.8726 0.052 Uiso 1 1 calc R . . C34 C 0.2022(3) 1.2579(2) 0.7505(2) 0.0443(8) Uani 1 1 d . . . H34 H 0.1941 1.331 0.7371 0.053 Uiso 1 1 calc R . . C35 C 0.2430(3) 1.1822(2) 0.6902(2) 0.0418(8) Uani 1 1 d . . . H35 H 0.2656 1.2031 0.6355 0.05 Uiso 1 1 calc R . . C36 C 0.2515(3) 1.0756(2) 0.70812(17) 0.0293(6) Uani 1 1 d . . . H36 H 0.2781 1.0239 0.6656 0.035 Uiso 1 1 calc R . . C37 C 0.1692(3) 0.7000(3) 1.09266(18) 0.0474(8) Uani 1 1 d . . . H37C H 0.1241 0.7732 1.0945 0.071 Uiso 1 1 calc R . . H37B H 0.2497 0.6979 1.1129 0.071 Uiso 1 1 calc R . . H37A H 0.1253 0.6554 1.128 0.071 Uiso 1 1 calc R . . C38 C 0.2651(3) 0.5090(2) 0.9804(2) 0.0439(8) Uani 1 1 d . . . H38C H 0.2208 0.4672 1.0181 0.066 Uiso 1 1 calc R . . H38B H 0.3474 0.5047 0.9981 0.066 Uiso 1 1 calc R . . H38A H 0.2691 0.4809 0.9236 0.066 Uiso 1 1 calc R . . C39 C 0.0292(3) 0.6577(3) 0.9492(2) 0.0449(8) Uani 1 1 d . . . H39C H -0.0141 0.6138 0.9856 0.067 Uiso 1 1 calc R . . H39B H 0.0332 0.6322 0.8916 0.067 Uiso 1 1 calc R . . H39A H -0.0139 0.7315 0.9526 0.067 Uiso 1 1 calc R . . C40 C -0.0410(3) 0.7939(2) 0.7183(2) 0.0368(7) Uani 1 1 d . . . H40C H -0.1191 0.8127 0.6933 0.055 Uiso 1 1 calc R . . H40B H -0.0535 0.7669 0.7747 0.055 Uiso 1 1 calc R . . H40A H 0.0128 0.7392 0.6842 0.055 Uiso 1 1 calc R . . C41 C 0.0530(2) 0.9637(2) 0.61561(17) 0.0303(6) Uani 1 1 d . . . H41C H 0.1066 0.9085 0.5818 0.045 Uiso 1 1 calc R . . H41B H 0.0902 1.0267 0.6177 0.045 Uiso 1 1 calc R . . H41A H -0.0252 0.9823 0.5907 0.045 Uiso 1 1 calc R . . C42 C -0.0728(3) 1.0162(3) 0.7898(2) 0.0425(8) Uani 1 1 d . . . H42C H -0.0364 1.0795 0.7927 0.064 Uiso 1 1 calc R . . H42B H -0.084 0.9881 0.846 0.064 Uiso 1 1 calc R . . H42A H -0.1516 1.0348 0.7657 0.064 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 Yb 0.02207(7) 0.01693(7) 0.01526(6) 0.00040(4) -0.00060(4) -0.00621(4) Si1 0.0211(4) 0.0328(4) 0.0287(4) 0.0057(3) -0.0042(3) -0.0047(3) Si2 0.0340(4) 0.0237(4) 0.0256(4) 0.0007(3) -0.0049(3) -0.0120(3) Si3 0.0360(4) 0.0293(4) 0.0224(4) 0.0026(3) -0.0007(3) -0.0080(3) Si4 0.0204(4) 0.0249(4) 0.0240(4) 0.0014(3) -0.0034(3) -0.0022(3) N1 0.0205(11) 0.0260(11) 0.0184(10) 0.0010(8) -0.0028(8) -0.0056(9) N2 0.0221(11) 0.0276(12) 0.0180(10) 0.0004(9) -0.0029(8) -0.0085(9) N3 0.0319(12) 0.0209(11) 0.0180(10) -0.0017(8) -0.0038(9) -0.0023(9) N4 0.0220(11) 0.0203(11) 0.0173(10) 0.0018(8) -0.0038(8) -0.0031(8) C1 0.0227(13) 0.0224(13) 0.0203(12) -0.0020(10) 0.0012(10) -0.0046(10) C2 0.0285(14) 0.0232(13) 0.0192(12) 0.0062(10) -0.0030(10) -0.0072(11) C3 0.0230(13) 0.0218(13) 0.0178(12) -0.0006(10) -0.0023(10) -0.0014(10) C4 0.0251(13) 0.0262(14) 0.0204(12) 0.0048(10) -0.0042(10) -0.0077(11) C5 0.0264(14) 0.0303(15) 0.0282(14) -0.0004(11) -0.0023(11) -0.0089(11) C6 0.0309(15) 0.0285(15) 0.0385(16) -0.0013(12) -0.0079(12) -0.0101(12) C7 0.0294(15) 0.0295(15) 0.0388(16) 0.0125(12) -0.0090(12) -0.0126(12) C8 0.0421(18) 0.0469(19) 0.0307(15) 0.0059(13) 0.0060(13) -0.0206(14) C9 0.0447(18) 0.0413(18) 0.0268(14) -0.0040(13) 0.0056(13) -0.0202(14) C10 0.0366(15) 0.0176(13) 0.0184(12) 0.0014(10) -0.0063(11) -0.0058(11) C11 0.0497(18) 0.0287(15) 0.0226(14) -0.0012(11) -0.0007(12) -0.0075(13) C12 0.083(3) 0.0390(18) 0.0188(14) -0.0022(13) 0.0002(15) -0.0143(17) C13 0.091(3) 0.0391(19) 0.0268(16) 0.0037(13) -0.0296(17) -0.0169(18) C14 0.058(2) 0.0366(18) 0.0424(19) 0.0061(14) -0.0304(16) -0.0149(15) C15 0.0388(16) 0.0277(15) 0.0291(14) 0.0006(11) -0.0131(12) -0.0090(12) C16 0.0311(17) 0.0448(19) 0.055(2) 0.0025(16) 0.0056(14) 0.0011(14) C17 0.0306(16) 0.0505(19) 0.0407(17) 0.0048(14) -0.0137(13) -0.0103(14) C18 0.0381(17) 0.0429(18) 0.0432(18) 0.0164(14) -0.0107(14) -0.0075(14) C19 0.0454(18) 0.0251(15) 0.0275(14) 0.0037(11) -0.0031(13) -0.0156(13) C20 0.061(2) 0.046(2) 0.059(2) 0.0072(17) -0.0249(18) -0.0328(17) C21 0.068(2) 0.0340(18) 0.058(2) -0.0119(16) 0.0164(18) -0.0082(16) C22 0.0222(13) 0.0244(14) 0.0205(12) -0.0013(10) -0.0009(10) 0.0002(10) C23 0.0216(13) 0.0259(14) 0.0240(13) 0.0016(10) -0.0026(10) -0.0076(10) C24 0.0203(13) 0.0244(13) 0.0194(12) 0.0003(10) 0.0030(10) -0.0048(10) C25 0.0235(13) 0.0304(14) 0.0194(12) -0.0015(11) -0.0024(10) -0.0049(11) C26 0.0359(16) 0.0325(16) 0.0277(14) -0.0037(12) -0.0084(12) 0.0008(12) C27 0.0342(16) 0.0472(19) 0.0302(15) 0.0022(13) -0.0112(12) 0.0046(13) C28 0.0355(17) 0.060(2) 0.0269(15) -0.0042(14) -0.0105(12) -0.0105(15) C29 0.0470(18) 0.0418(18) 0.0314(15) -0.0099(13) -0.0108(13) -0.0118(14) C30 0.0365(16) 0.0314(16) 0.0302(15) -0.0018(12) -0.0068(12) -0.0049(12) C31 0.0202(13) 0.0226(13) 0.0282(13) 0.0007(11) -0.0075(10) -0.0047(10) C32 0.0371(16) 0.0283(16) 0.0369(16) -0.0037(12) 0.0010(13) -0.0061(12) C33 0.0424(18) 0.0274(16) 0.060(2) -0.0131(15) -0.0082(15) -0.0034(13) C34 0.054(2) 0.0228(15) 0.061(2) 0.0091(15) -0.0241(17) -0.0121(14) C35 0.060(2) 0.0346(17) 0.0383(17) 0.0114(14) -0.0185(15) -0.0222(15) C36 0.0351(15) 0.0275(15) 0.0288(14) 0.0028(11) -0.0096(12) -0.0126(12) C37 0.055(2) 0.062(2) 0.0267(16) -0.0032(15) 0.0082(14) -0.0187(17) C38 0.065(2) 0.0324(17) 0.0345(16) 0.0105(13) -0.0048(15) -0.0101(15) C39 0.0397(18) 0.060(2) 0.0379(17) 0.0042(15) 0.0011(14) -0.0175(16) C40 0.0296(15) 0.0394(17) 0.0442(17) 0.0061(14) -0.0065(13) -0.0124(13) C41 0.0291(15) 0.0339(16) 0.0290(14) 0.0061(12) -0.0091(11) -0.0063(12) C42 0.0302(16) 0.050(2) 0.0416(17) -0.0083(15) -0.0045(13) 0.0066(14) #----------------------------------------------------------------------------# # 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 Yb N1 2.265(2) . ? Yb N4 2.272(2) . ? Yb N2 2.289(2) . ? Yb N3 2.328(2) . ? Yb C19 2.406(3) . ? Si1 N1 1.750(2) . ? Si1 C16 1.864(3) . ? Si1 C17 1.866(3) . ? Si1 C18 1.878(3) . ? Si2 N2 1.767(2) . ? Si2 C19 1.833(3) . ? Si2 C20 1.860(3) . ? Si2 C21 1.862(3) . ? Si3 N3 1.754(2) . ? Si3 C38 1.857(3) . ? Si3 C39 1.860(3) . ? Si3 C37 1.871(3) . ? Si4 N4 1.763(2) . ? Si4 C40 1.860(3) . ? Si4 C42 1.865(3) . ? Si4 C41 1.865(3) . ? N1 C1 1.348(3) . ? N2 C3 1.316(3) . ? N3 C22 1.338(3) . ? N4 C24 1.328(3) . ? C1 C2 1.398(4) . ? C1 C4 1.500(4) . ? C2 C3 1.417(4) . ? C3 C10 1.497(3) . ? C4 C9 1.388(4) . ? C4 C5 1.388(4) . ? C5 C6 1.389(4) . ? C6 C7 1.379(4) . ? C7 C8 1.377(4) . ? C8 C9 1.385(4) . ? C10 C15 1.393(4) . ? C10 C11 1.395(4) . ? C11 C12 1.391(4) . ? C12 C13 1.376(5) . ? C13 C14 1.373(5) . ? C14 C15 1.390(4) . ? C22 C23 1.414(4) . ? C22 C25 1.504(3) . ? C23 C24 1.420(3) . ? C24 C31 1.499(4) . ? C25 C26 1.388(4) . ? C25 C30 1.388(4) . ? C26 C27 1.388(4) . ? C27 C28 1.379(4) . ? C28 C29 1.379(4) . ? C29 C30 1.382(4) . ? C31 C36 1.386(4) . ? C31 C32 1.393(4) . ? C32 C33 1.379(4) . ? C33 C34 1.378(5) . ? C34 C35 1.372(5) . ? C35 C36 1.384(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 Yb N4 106.23(7) . . ? N1 Yb N2 79.93(7) . . ? N4 Yb N2 94.28(7) . . ? N1 Yb N3 117.93(7) . . ? N4 Yb N3 82.37(7) . . ? N2 Yb N3 162.10(8) . . ? N1 Yb C19 119.06(9) . . ? N4 Yb C19 127.46(10) . . ? N2 Yb C19 70.48(9) . . ? N3 Yb C19 97.56(9) . . ? N1 Si1 C16 111.39(13) . . ? N1 Si1 C17 115.41(12) . . ? C16 Si1 C17 110.96(15) . . ? N1 Si1 C18 103.09(12) . . ? C16 Si1 C18 107.84(15) . . ? C17 Si1 C18 107.53(15) . . ? N2 Si2 C19 97.70(11) . . ? N2 Si2 C20 116.58(13) . . ? C19 Si2 C20 115.32(16) . . ? N2 Si2 C21 105.13(14) . . ? C19 Si2 C21 113.87(17) . . ? C20 Si2 C21 107.76(18) . . ? N3 Si3 C38 110.27(13) . . ? N3 Si3 C39 106.26(13) . . ? C38 Si3 C39 109.51(16) . . ? N3 Si3 C37 114.75(13) . . ? C38 Si3 C37 109.29(15) . . ? C39 Si3 C37 106.56(16) . . ? N4 Si4 C40 104.48(12) . . ? N4 Si4 C42 110.23(12) . . ? C40 Si4 C42 109.06(15) . . ? N4 Si4 C41 112.95(11) . . ? C40 Si4 C41 108.95(14) . . ? C42 Si4 C41 110.92(14) . . ? C1 N1 Si1 125.46(17) . . ? C1 N1 Yb 117.43(16) . . ? Si1 N1 Yb 117.11(10) . . ? C3 N2 Si2 133.86(18) . . ? C3 N2 Yb 123.84(17) . . ? Si2 N2 Yb 98.71(9) . . ? C22 N3 Si3 129.00(17) . . ? C22 N3 Yb 101.51(16) . . ? Si3 N3 Yb 129.49(11) . . ? C24 N4 Si4 126.77(17) . . ? C24 N4 Yb 102.72(15) . . ? Si4 N4 Yb 129.86(11) . . ? N1 C1 C2 126.0(2) . . ? N1 C1 C4 119.8(2) . . ? C2 C1 C4 114.2(2) . . ? C1 C2 C3 126.7(2) . . ? N2 C3 C2 122.6(2) . . ? N2 C3 C10 120.6(2) . . ? C2 C3 C10 116.8(2) . . ? C9 C4 C5 118.5(2) . . ? C9 C4 C1 121.9(2) . . ? C5 C4 C1 119.5(2) . . ? C4 C5 C6 120.6(3) . . ? C7 C6 C5 120.2(3) . . ? C8 C7 C6 119.6(3) . . ? C7 C8 C9 120.4(3) . . ? C8 C9 C4 120.6(3) . . ? C15 C10 C11 118.7(2) . . ? C15 C10 C3 119.7(2) . . ? C11 C10 C3 121.6(2) . . ? C12 C11 C10 120.1(3) . . ? C13 C12 C11 120.4(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 120.2(3) . . ? C14 C15 C10 120.5(3) . . ? Si2 C19 Yb 92.86(11) . . ? N3 C22 C23 123.7(2) . . ? N3 C22 C25 122.0(2) . . ? C23 C22 C25 114.4(2) . . ? C22 C23 C24 128.2(2) . . ? N4 C24 C23 124.4(2) . . ? N4 C24 C31 121.1(2) . . ? C23 C24 C31 114.5(2) . . ? C26 C25 C30 118.4(2) . . ? C26 C25 C22 120.7(2) . . ? C30 C25 C22 120.9(2) . . ? C25 C26 C27 120.7(3) . . ? C28 C27 C26 120.1(3) . . ? C29 C28 C27 119.7(3) . . ? C28 C29 C30 120.3(3) . . ? C29 C30 C25 120.9(3) . . ? C36 C31 C32 118.7(3) . . ? C36 C31 C24 120.5(2) . . ? C32 C31 C24 120.9(2) . . ? C33 C32 C31 120.7(3) . . ? C34 C33 C32 120.0(3) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.7(3) . . ? C35 C36 C31 120.1(3) . . ? #===END data_nov1002 _database_code_depnum_ccdc_archive 'CCDC 254753' _audit_creation_date 2002-11-07T10:03:08-00:00 _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 (Yb(Me3SiNCPhCHCPhNSiMe3)(CH2SiMe2NCPhCHCPhNSiMe3)) _chemical_formula_moiety 'C42 H57 N4 Si4 Yb1' _chemical_formula_sum 'C42 H57 N4 Si4 Yb' _chemical_formula_weight 903.32 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2433(2) _cell_length_b 12.9389(2) _cell_length_c 16.2117(2) _cell_angle_alpha 89.319(1) _cell_angle_beta 86.149(1) _cell_angle_gamma 79.253(1) _cell_volume 2311.81(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 27625 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.157 _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 0.4934 _exptl_absorpt_correction_T_max 0.5386 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_number 29992 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 27.91 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 10926 _reflns_number_gt 10399 _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 crystal structure is 74% as the title compound , but disordered with 26% of the unoxidised starting material [Yb(Me3SiNCPhCHCPhNSiMe3)2] . The alternative atom positions for the lower occupancy NSiMe3 sites were included as isotropic N,C, and Si atoms with H atoms omitted. All other atom sites were coincident. *************************************************************************** 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^+7.2677P] 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 10926 _refine_ls_number_parameters 481 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.806 _refine_diff_density_min -2.065 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 '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 Yb Yb 0.215740(16) 0.292350(14) -0.266968(10) 0.03425(6) Uani 1 1 d . . . Si1 Si 0.31438(13) 0.34952(11) -0.48228(8) 0.0471(3) Uani 1 1 d . . . Si2 Si 0.46958(11) 0.08405(10) -0.22360(7) 0.0394(2) Uani 1 1 d . . . Si4 Si -0.09681(11) 0.32670(11) -0.25718(8) 0.0454(3) Uani 1 1 d . . . N1 N 0.2427(3) 0.2736(3) -0.4116(2) 0.0386(7) Uani 1 1 d . A . N2 N 0.3327(3) 0.1288(3) -0.2710(2) 0.0356(7) Uani 1 1 d . A . N4 N 0.0335(3) 0.2686(3) -0.2090(2) 0.0365(7) Uani 1 1 d . A . C1 C 0.1895(4) 0.1915(3) -0.4259(2) 0.0374(8) Uani 1 1 d . . . C2 C 0.1870(4) 0.1065(3) -0.3706(2) 0.0378(8) Uani 1 1 d . A . H2 H 0.123 0.0698 -0.375 0.045 Uiso 1 1 calc R . . C3 C 0.2686(3) 0.0697(3) -0.3092(2) 0.0333(8) Uani 1 1 d . . . C4 C 0.1248(4) 0.1842(3) -0.5033(2) 0.0399(9) Uani 1 1 d . A . C5 C 0.0489(5) 0.2712(4) -0.5334(3) 0.0513(11) Uani 1 1 d . . . H5 H 0.0394 0.3362 -0.5063 0.062 Uiso 1 1 calc R A . C6 C -0.0131(5) 0.2629(5) -0.6035(3) 0.0601(13) Uani 1 1 d . A . H6 H -0.0656 0.3221 -0.6228 0.072 Uiso 1 1 calc R . . C7 C 0.0017(5) 0.1694(5) -0.6446(3) 0.0623(14) Uani 1 1 d . . . H7 H -0.0398 0.1645 -0.6924 0.075 Uiso 1 1 calc R A . C8 C 0.0775(5) 0.0822(5) -0.6160(3) 0.0616(14) Uani 1 1 d . A . H8 H 0.0884 0.018 -0.6446 0.074 Uiso 1 1 calc R . . C9 C 0.1377(5) 0.0892(4) -0.5453(3) 0.0513(11) Uani 1 1 d . . . H9 H 0.1879 0.0291 -0.5253 0.062 Uiso 1 1 calc R A . C10 C 0.2782(4) -0.0455(3) -0.2890(3) 0.0384(9) Uani 1 1 d . A . C11 C 0.3158(5) -0.1213(4) -0.3498(3) 0.0561(12) Uani 1 1 d . . . H11 H 0.3343 -0.101 -0.4043 0.067 Uiso 1 1 calc R A . C12 C 0.3262(5) -0.2271(4) -0.3303(4) 0.0703(16) Uani 1 1 d . A . H12 H 0.353 -0.2785 -0.3713 0.084 Uiso 1 1 calc R . . C13 C 0.2973(6) -0.2567(4) -0.2514(4) 0.0731(18) Uani 1 1 d . . . H13 H 0.3054 -0.3284 -0.238 0.088 Uiso 1 1 calc R A . C14 C 0.2568(6) -0.1822(4) -0.1920(4) 0.0681(16) Uani 1 1 d . A . H14 H 0.2345 -0.2031 -0.1383 0.082 Uiso 1 1 calc R . . C15 C 0.2481(4) -0.0764(4) -0.2099(3) 0.0462(10) Uani 1 1 d . . . H15 H 0.2217 -0.0258 -0.1683 0.055 Uiso 1 1 calc R A . C16 C 0.2335(6) 0.4885(4) -0.4784(4) 0.0700(16) Uani 1 1 d . A . H16C H 0.2792 0.5315 -0.5126 0.105 Uiso 1 1 calc R . . H16B H 0.2255 0.5136 -0.4218 0.105 Uiso 1 1 calc R . . H16A H 0.1535 0.4931 -0.4989 0.105 Uiso 1 1 calc R . . C17 C 0.4707(5) 0.3417(6) -0.4485(4) 0.0725(17) Uani 1 1 d . A . H17C H 0.5139 0.2695 -0.4526 0.109 Uiso 1 1 calc R . . H17B H 0.4666 0.3653 -0.3917 0.109 Uiso 1 1 calc R . . H17A H 0.5131 0.3861 -0.4837 0.109 Uiso 1 1 calc R . . C18 C 0.3304(6) 0.3033(6) -0.5916(3) 0.0765(18) Uani 1 1 d . A . H18C H 0.3749 0.3477 -0.6253 0.115 Uiso 1 1 calc R . . H18B H 0.2506 0.3069 -0.612 0.115 Uiso 1 1 calc R . . H18A H 0.3742 0.2312 -0.5944 0.115 Uiso 1 1 calc R . . C19 C 0.5710(5) -0.0172(5) -0.2892(4) 0.0666(15) Uani 1 1 d . A . H19C H 0.5836 0.0111 -0.344 0.1 Uiso 1 1 calc R . . H19B H 0.5339 -0.0788 -0.2929 0.1 Uiso 1 1 calc R . . H19A H 0.6485 -0.0368 -0.2647 0.1 Uiso 1 1 calc R . . C20 C 0.5402(5) 0.2019(4) -0.2177(4) 0.0589(13) Uani 1 1 d . A . H20C H 0.4869 0.2555 -0.1844 0.088 Uiso 1 1 calc R . . H20B H 0.5535 0.229 -0.2729 0.088 Uiso 1 1 calc R . . H20A H 0.6173 0.1831 -0.1927 0.088 Uiso 1 1 calc R . . C21 C 0.4465(4) 0.0337(4) -0.1164(3) 0.0490(11) Uani 1 1 d . A . H21C H 0.5244 0.0145 -0.0925 0.073 Uiso 1 1 calc R . . H21B H 0.4084 -0.0275 -0.1181 0.073 Uiso 1 1 calc R . . H21A H 0.3948 0.0881 -0.083 0.073 Uiso 1 1 calc R . . C22 C 0.2025(4) 0.2724(3) -0.0693(2) 0.0342(8) Uani 1 1 d . . . C23 C 0.1190(4) 0.2045(3) -0.0788(2) 0.0371(8) Uani 1 1 d . A . H23 H 0.1196 0.15 -0.0399 0.045 Uiso 1 1 calc R . . C24 C 0.0357(4) 0.2097(3) -0.1400(2) 0.0344(8) Uani 1 1 d . . . C25 C 0.2473(4) 0.2772(3) 0.0152(2) 0.0375(9) Uani 1 1 d . A . C26 C 0.1687(5) 0.2852(4) 0.0857(3) 0.0541(12) Uani 1 1 d . . . H26 H 0.0854 0.2877 0.0809 0.065 Uiso 1 1 calc R A . C27 C 0.2132(7) 0.2896(5) 0.1636(3) 0.0748(19) Uani 1 1 d . A . H27 H 0.1597 0.297 0.2112 0.09 Uiso 1 1 calc R . . C28 C 0.3356(8) 0.2833(5) 0.1706(4) 0.081(2) Uani 1 1 d . . . H28 H 0.3654 0.2854 0.2233 0.097 Uiso 1 1 calc R A . C29 C 0.4143(6) 0.2739(5) 0.1019(4) 0.0709(17) Uani 1 1 d . A . H29 H 0.4979 0.2692 0.1073 0.085 Uiso 1 1 calc R . . C30 C 0.3706(5) 0.2712(4) 0.0240(3) 0.0522(11) Uani 1 1 d . . . H30 H 0.4248 0.2652 -0.0232 0.063 Uiso 1 1 calc R A . C31 C -0.0564(4) 0.1407(3) -0.1231(2) 0.0368(8) Uani 1 1 d . A . C32 C -0.0639(4) 0.0615(4) -0.1786(3) 0.0436(9) Uani 1 1 d . . . H32 H -0.0158 0.0552 -0.2286 0.052 Uiso 1 1 calc R A . C33 C -0.1413(4) -0.0081(4) -0.1607(3) 0.0504(11) Uani 1 1 d . A . H33 H -0.1432 -0.063 -0.1978 0.06 Uiso 1 1 calc R . . C34 C -0.2157(4) 0.0020(4) -0.0894(3) 0.0509(11) Uani 1 1 d . . . H34 H -0.2687 -0.0453 -0.0779 0.061 Uiso 1 1 calc R A . C35 C -0.2119(5) 0.0818(5) -0.0352(3) 0.0608(14) Uani 1 1 d . A . H35 H -0.2641 0.0902 0.0131 0.073 Uiso 1 1 calc R . . C36 C -0.1316(5) 0.1502(4) -0.0510(3) 0.0552(12) Uani 1 1 d . . . H36 H -0.1279 0.2032 -0.0126 0.066 Uiso 1 1 calc R A . C40 C -0.0474(5) 0.4370(5) -0.3177(4) 0.0648(15) Uani 1 1 d . A . H40C H 0.0172 0.4087 -0.3585 0.097 Uiso 1 1 calc R . . H40B H -0.0181 0.4835 -0.2806 0.097 Uiso 1 1 calc R . . H40A H -0.1155 0.4761 -0.3455 0.097 Uiso 1 1 calc R . . C41 C -0.1529(5) 0.2406(5) -0.3315(3) 0.0632(14) Uani 1 1 d . A . H41C H -0.1817 0.1838 -0.3016 0.095 Uiso 1 1 calc R . . H41B H -0.0873 0.2116 -0.3713 0.095 Uiso 1 1 calc R . . H41A H -0.2188 0.2817 -0.3601 0.095 Uiso 1 1 calc R . . C42 C -0.2208(5) 0.3848(5) -0.1806(4) 0.0789(18) Uani 1 1 d . A . H42C H -0.2863 0.4267 -0.2092 0.118 Uiso 1 1 calc R . . H42B H -0.1901 0.4291 -0.1425 0.118 Uiso 1 1 calc R . . H42A H -0.2509 0.3289 -0.1502 0.118 Uiso 1 1 calc R . . N3 N 0.2435(7) 0.3216(6) -0.1317(4) 0.0323(13) Uani 0.740(7) 1 d P A 1 Si3 Si 0.27499(17) 0.45086(14) -0.14266(13) 0.0377(5) Uani 0.740(7) 1 d P A 1 C37 C 0.1460(8) 0.5386(6) -0.0864(5) 0.070(2) Uani 0.740(7) 1 d P A 1 H37C H 0.1484 0.6113 -0.1006 0.105 Uiso 0.740(7) 1 calc PR A 1 H37B H 0.1522 0.5289 -0.0273 0.105 Uiso 0.740(7) 1 calc PR A 1 H37A H 0.0701 0.5215 -0.1019 0.105 Uiso 0.740(7) 1 calc PR A 1 C38 C 0.4164(8) 0.4741(7) -0.0980(6) 0.075(3) Uani 0.740(7) 1 d P A 1 H38C H 0.4851 0.4233 -0.1207 0.113 Uiso 0.740(7) 1 calc PR A 1 H38B H 0.409 0.4662 -0.0384 0.113 Uiso 0.740(7) 1 calc PR A 1 H38A H 0.4287 0.5447 -0.1116 0.113 Uiso 0.740(7) 1 calc PR A 1 C39 C 0.2732(6) 0.4606(4) -0.2551(3) 0.0442(15) Uani 0.740(7) 1 d P A 1 H39B H 0.353 0.4635 -0.2824 0.053 Uiso 0.740(7) 1 calc PR A 1 H39A H 0.2121 0.5189 -0.2736 0.053 Uiso 0.740(7) 1 calc PR A 1 N3A N 0.230(2) 0.3500(18) -0.1256(17) 0.041(7) Uiso 0.260(7) 1 d P A 2 Si3A Si 0.2588(7) 0.4774(7) -0.1073(6) 0.069(2) Uiso 0.260(7) 1 d PD A 2 C37A C 0.229(4) 0.531(3) 0.0025(18) 0.133(14) Uiso 0.260(7) 1 d PD A 2 C38A C 0.419(3) 0.488(3) -0.149(2) 0.106(11) Uiso 0.260(7) 1 d PD A 2 C39A C 0.140(2) 0.566(2) -0.1673(17) 0.083(8) Uiso 0.260(7) 1 d PD 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 Yb 0.03883(10) 0.03626(9) 0.02666(8) -0.00252(6) -0.00195(6) -0.00431(7) Si1 0.0598(8) 0.0461(7) 0.0368(6) 0.0034(5) 0.0009(5) -0.0151(6) Si2 0.0362(6) 0.0418(6) 0.0405(6) 0.0005(5) -0.0054(5) -0.0069(5) Si4 0.0377(6) 0.0487(7) 0.0500(7) 0.0108(5) -0.0068(5) -0.0077(5) N1 0.049(2) 0.0311(17) 0.0353(17) 0.0012(13) -0.0043(15) -0.0069(15) N2 0.0407(18) 0.0351(17) 0.0317(16) -0.0002(13) -0.0065(13) -0.0077(14) N4 0.0393(18) 0.0399(18) 0.0322(16) 0.0007(13) -0.0069(13) -0.0112(14) C1 0.037(2) 0.042(2) 0.0319(19) -0.0046(16) -0.0035(15) -0.0030(17) C2 0.040(2) 0.038(2) 0.038(2) 0.0007(16) -0.0071(16) -0.0142(17) C3 0.0358(19) 0.0311(19) 0.0328(18) -0.0011(14) 0.0005(15) -0.0065(15) C4 0.041(2) 0.046(2) 0.033(2) -0.0020(17) -0.0053(16) -0.0080(18) C5 0.058(3) 0.052(3) 0.042(2) -0.003(2) -0.011(2) -0.001(2) C6 0.057(3) 0.070(3) 0.050(3) 0.002(2) -0.019(2) 0.002(3) C7 0.057(3) 0.089(4) 0.045(3) -0.006(3) -0.017(2) -0.017(3) C8 0.071(3) 0.065(3) 0.053(3) -0.013(2) -0.016(3) -0.020(3) C9 0.060(3) 0.050(3) 0.045(2) -0.004(2) -0.013(2) -0.009(2) C10 0.038(2) 0.034(2) 0.045(2) 0.0016(17) -0.0071(17) -0.0094(16) C11 0.057(3) 0.046(3) 0.064(3) -0.011(2) 0.001(2) -0.008(2) C12 0.066(4) 0.042(3) 0.103(5) -0.021(3) -0.011(3) -0.007(3) C13 0.087(4) 0.037(3) 0.104(5) 0.013(3) -0.035(4) -0.024(3) C14 0.093(4) 0.050(3) 0.072(4) 0.018(3) -0.031(3) -0.034(3) C15 0.057(3) 0.039(2) 0.049(2) 0.0047(18) -0.014(2) -0.021(2) C16 0.103(5) 0.045(3) 0.062(3) 0.014(2) -0.004(3) -0.014(3) C17 0.059(3) 0.102(5) 0.062(3) 0.008(3) 0.003(3) -0.032(3) C18 0.089(4) 0.103(5) 0.040(3) -0.011(3) 0.015(3) -0.034(4) C19 0.047(3) 0.077(4) 0.070(4) -0.019(3) -0.003(2) 0.005(3) C20 0.052(3) 0.062(3) 0.069(3) 0.008(3) -0.012(2) -0.025(2) C21 0.046(2) 0.056(3) 0.047(2) 0.009(2) -0.012(2) -0.012(2) C22 0.040(2) 0.0341(19) 0.0283(17) -0.0023(14) -0.0028(15) -0.0062(16) C23 0.045(2) 0.034(2) 0.0350(19) 0.0012(15) -0.0093(16) -0.0110(17) C24 0.039(2) 0.0336(19) 0.0315(18) -0.0022(15) -0.0018(15) -0.0098(16) C25 0.053(2) 0.0294(19) 0.0329(19) -0.0010(15) -0.0102(17) -0.0117(17) C26 0.079(3) 0.051(3) 0.034(2) -0.0039(19) 0.000(2) -0.016(2) C27 0.132(6) 0.061(4) 0.034(2) -0.005(2) -0.002(3) -0.028(4) C28 0.141(7) 0.064(4) 0.047(3) 0.003(3) -0.045(4) -0.028(4) C29 0.091(4) 0.062(3) 0.069(4) 0.001(3) -0.045(3) -0.024(3) C30 0.058(3) 0.052(3) 0.051(3) -0.003(2) -0.020(2) -0.016(2) C31 0.040(2) 0.037(2) 0.0357(19) 0.0031(16) -0.0057(16) -0.0116(17) C32 0.041(2) 0.047(2) 0.044(2) -0.0047(19) -0.0043(18) -0.0127(19) C33 0.051(3) 0.044(2) 0.061(3) -0.004(2) -0.013(2) -0.017(2) C34 0.053(3) 0.047(3) 0.059(3) 0.014(2) -0.014(2) -0.024(2) C35 0.070(3) 0.070(3) 0.049(3) 0.007(2) 0.008(2) -0.034(3) C36 0.074(3) 0.057(3) 0.041(2) -0.005(2) 0.006(2) -0.032(3) C40 0.063(3) 0.063(3) 0.070(3) 0.029(3) -0.014(3) -0.013(3) C41 0.051(3) 0.079(4) 0.065(3) 0.012(3) -0.025(2) -0.019(3) C42 0.053(3) 0.071(4) 0.105(5) 0.006(4) 0.016(3) 0.001(3) N3 0.037(3) 0.028(3) 0.033(3) -0.002(3) 0.000(2) -0.011(3) Si3 0.0512(10) 0.0316(9) 0.0340(10) -0.0042(7) -0.0006(7) -0.0183(7) C37 0.091(6) 0.046(4) 0.071(5) -0.017(3) 0.018(4) -0.014(4) C38 0.088(6) 0.071(5) 0.086(6) 0.005(5) -0.033(5) -0.058(5) C39 0.069(4) 0.029(3) 0.041(3) 0.001(2) -0.005(3) -0.025(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 Yb N4 2.268(3) . ? Yb N2 2.273(3) . ? Yb N3 2.282(7) . ? Yb N1 2.353(3) . ? Yb C39 2.398(5) . ? Si1 N1 1.753(4) . ? Si1 C16 1.858(6) . ? Si1 C17 1.860(6) . ? Si1 C18 1.864(5) . ? Si2 N2 1.764(3) . ? Si2 C20 1.853(5) . ? Si2 C19 1.860(5) . ? Si2 C21 1.867(5) . ? Si4 N4 1.746(4) . ? Si4 C42 1.857(6) . ? Si4 C41 1.867(6) . ? Si4 C40 1.871(5) . ? N1 C1 1.342(5) . ? N2 C3 1.328(5) . ? N4 C24 1.345(5) . ? C1 C2 1.414(6) . ? C1 C4 1.504(5) . ? C2 C3 1.416(5) . ? C3 C10 1.508(5) . ? C4 C5 1.385(6) . ? C4 C9 1.391(6) . ? C5 C6 1.387(7) . ? C6 C7 1.366(8) . ? C7 C8 1.377(8) . ? C8 C9 1.382(7) . ? C10 C15 1.377(6) . ? C10 C11 1.388(6) . ? C11 C12 1.387(8) . ? C12 C13 1.366(9) . ? C13 C14 1.365(9) . ? C14 C15 1.383(7) . ? C22 N3 1.293(8) . ? C22 N3A 1.41(3) . ? C22 C23 1.416(5) . ? C22 C25 1.498(5) . ? C23 C24 1.403(5) . ? C24 C31 1.498(5) . ? C25 C26 1.389(6) . ? C25 C30 1.391(6) . ? C26 C27 1.395(7) . ? C27 C28 1.375(10) . ? C28 C29 1.369(10) . ? C29 C30 1.388(7) . ? C31 C36 1.389(6) . ? C31 C32 1.389(6) . ? C32 C33 1.379(6) . ? C33 C34 1.373(7) . ? C34 C35 1.374(7) . ? C35 C36 1.387(7) . ? N3 Si3 1.778(7) . ? Si3 C39 1.827(6) . ? Si3 C37 1.860(8) . ? Si3 C38 1.866(7) . ? N3A Si3A 1.77(2) . ? Si3A C37A 1.90(2) . ? Si3A C39A 1.91(2) . ? Si3A C38A 1.91(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Yb N2 104.64(12) . . ? N4 Yb N3 80.49(19) . . ? N2 Yb N3 94.7(2) . . ? N4 Yb N1 115.81(12) . . ? N2 Yb N1 82.08(12) . . ? N3 Yb N1 163.69(19) . . ? N4 Yb C39 119.10(18) . . ? N2 Yb C39 129.76(19) . . ? N3 Yb C39 71.1(2) . . ? N1 Yb C39 98.66(16) . . ? N1 Si1 C16 110.0(2) . . ? N1 Si1 C17 106.0(2) . . ? C16 Si1 C17 109.5(3) . . ? N1 Si1 C18 115.5(2) . . ? C16 Si1 C18 108.8(3) . . ? C17 Si1 C18 106.7(3) . . ? N2 Si2 C20 104.7(2) . . ? N2 Si2 C19 110.4(2) . . ? C20 Si2 C19 109.2(3) . . ? N2 Si2 C21 113.30(19) . . ? C20 Si2 C21 108.2(2) . . ? C19 Si2 C21 110.8(3) . . ? N4 Si4 C42 111.6(3) . . ? N4 Si4 C41 115.3(2) . . ? C42 Si4 C41 110.6(3) . . ? N4 Si4 C40 103.4(2) . . ? C42 Si4 C40 107.8(3) . . ? C41 Si4 C40 107.5(3) . . ? C1 N1 Si1 129.1(3) . . ? C1 N1 Yb 103.0(2) . . ? Si1 N1 Yb 127.94(18) . . ? C3 N2 Si2 126.4(3) . . ? C3 N2 Yb 104.8(2) . . ? Si2 N2 Yb 128.40(17) . . ? C24 N4 Si4 125.5(3) . . ? C24 N4 Yb 116.5(3) . . ? Si4 N4 Yb 118.03(17) . . ? N1 C1 C2 124.0(4) . . ? N1 C1 C4 121.7(4) . . ? C2 C1 C4 114.4(4) . . ? C1 C2 C3 128.3(4) . . ? N2 C3 C2 124.7(4) . . ? N2 C3 C10 121.0(3) . . ? C2 C3 C10 114.3(3) . . ? C5 C4 C9 118.3(4) . . ? C5 C4 C1 120.9(4) . . ? C9 C4 C1 120.7(4) . . ? C4 C5 C6 120.5(5) . . ? C7 C6 C5 120.4(5) . . ? C6 C7 C8 120.0(5) . . ? C7 C8 C9 119.9(5) . . ? C8 C9 C4 120.8(5) . . ? C15 C10 C11 119.3(4) . . ? C15 C10 C3 120.2(4) . . ? C11 C10 C3 120.5(4) . . ? C12 C11 C10 120.1(5) . . ? C13 C12 C11 120.0(5) . . ? C14 C13 C12 120.1(5) . . ? C13 C14 C15 120.7(6) . . ? C10 C15 C14 119.8(5) . . ? N3 C22 N3A 15.5(10) . . ? N3 C22 C23 121.5(4) . . ? N3A C22 C23 126.8(12) . . ? N3 C22 C25 122.1(4) . . ? N3A C22 C25 115.8(11) . . ? C23 C22 C25 116.3(3) . . ? C24 C23 C22 127.0(4) . . ? N4 C24 C23 126.2(4) . . ? N4 C24 C31 120.2(3) . . ? C23 C24 C31 113.7(3) . . ? C26 C25 C30 118.9(4) . . ? C26 C25 C22 121.5(4) . . ? C30 C25 C22 119.6(4) . . ? C25 C26 C27 120.2(6) . . ? C28 C27 C26 119.8(6) . . ? C29 C28 C27 120.7(5) . . ? C28 C29 C30 119.8(6) . . ? C29 C30 C25 120.6(5) . . ? C36 C31 C32 118.4(4) . . ? C36 C31 C24 121.7(4) . . ? C32 C31 C24 119.8(4) . . ? C33 C32 C31 120.6(4) . . ? C34 C33 C32 120.7(4) . . ? C33 C34 C35 119.4(4) . . ? C34 C35 C36 120.5(5) . . ? C35 C36 C31 120.4(5) . . ? C22 N3 Si3 132.2(5) . . ? C22 N3 Yb 125.3(5) . . ? Si3 N3 Yb 98.0(3) . . ? N3 Si3 C39 98.0(3) . . ? N3 Si3 C37 105.8(4) . . ? C39 Si3 C37 113.9(4) . . ? N3 Si3 C38 116.2(4) . . ? C39 Si3 C38 115.7(4) . . ? C37 Si3 C38 106.9(4) . . ? Si3 C39 Yb 92.7(2) . . ? C22 N3A Si3A 130.2(17) . . ? C22 N3A Yb 109.7(13) . . ? Si3A N3A Yb 119.9(14) . . ? N3A Si3A C37A 117.7(16) . . ? N3A Si3A C39A 103.2(13) . . ? C37A Si3A C39A 103.6(17) . . ? N3A Si3A C38A 110.4(15) . . ? C37A Si3A C38A 110.3(18) . . ? C39A Si3A C38A 111.1(16) . . ? #===END