# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'Yb3Th_ccdc_deposit_rinumerato.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2010-12-16 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #============================================================================== # # SUBMISSION DETAILS _publ_contact_author_address ;ICCOM-CNR, Florence (Italy) ; # Address of author for correspondence _publ_contact_author_email giuliano.giambastiani@iccom.cnr.it _publ_contact_author_fax 39(055)5225203 _publ_contact_author_phone 39(055)5225288 _publ_contact_letter ; Submission dated :2010-12-16 Please consider this CIF for submission to the Cambridge Crystallographic Data Centre. I certify that all authors have seen and approved of this submission, that all have made significant scientific contributions to the work reported, and that all share responsibility and accountability for the results. This CIF is submitted as a personal communication This CIF is submitted as part of a journal submission Giambastiani, G. et al. ; #============================================================================== # # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name C.Bianchini A.Trifonov B.Shestakov I.Gudilenkov G.Fukin G.Giambastiani L.Luconi A.Rossin L.Sorace 'J.Filippi ' _publ_contact_author_name 'Giambastiani, G. et al.' # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Yb3Th _database_code_depnum_ccdc_archive 'CCDC 794889' #TrackingRef 'Yb3Th_ccdc_deposit_rinumerato.cif' _audit_creation_date 2010-12-16T15:48:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H38 N2 S Yb, C7 H8' _chemical_formula_sum 'C47 H46 N2 S Yb' _chemical_formula_weight 843.96 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 23.695(9) _cell_length_b 10.380(4) _cell_length_c 15.684(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3858(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8825 _cell_measurement_theta_min 4.1491 _cell_measurement_theta_max 28.8081 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.73772 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 -0.0081100622 _diffrn_orient_matrix_ub_12 0.0229066128 _diffrn_orient_matrix_ub_13 -0.0255945381 _diffrn_orient_matrix_ub_21 0.0284827732 _diffrn_orient_matrix_ub_22 -0.0341552645 _diffrn_orient_matrix_ub_23 -0.0151727748 _diffrn_orient_matrix_ub_31 -0.0616085156 _diffrn_orient_matrix_ub_32 -0.0187810983 _diffrn_orient_matrix_ub_33 -0.0036095734 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_unetI/netI 0.0543 _diffrn_reflns_number 15989 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 28.91 _diffrn_reflns_theta_full 28.91 _diffrn_measured_fraction_theta_full 0.881 _diffrn_measured_fraction_theta_max 0.881 _reflns_number_total 7862 _reflns_number_gt 6376 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SIR97 (Giacovazzo et al, 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)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7862 _refine_ls_number_parameters 429 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.005(9) _refine_diff_density_max 1.214 _refine_diff_density_min -0.637 _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' S S 0.1246 0.1234 '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 C1 C 0.43100(19) 0.9556(5) 0.6694(3) 0.0175(12) Uani 1 1 d . . . C2 C 0.4422(2) 0.8253(5) 0.6629(3) 0.0198(11) Uani 1 1 d . . . H2 H 0.4718 0.7878 0.6953 0.024 Uiso 1 1 calc R . . C3 C 0.4104(2) 0.7504(5) 0.6095(3) 0.0239(12) Uani 1 1 d . . . H3 H 0.4173 0.6606 0.6042 0.029 Uiso 1 1 calc R . . C4 C 0.3677(2) 0.8095(6) 0.5632(3) 0.0228(11) Uani 1 1 d . . . H4 H 0.3454 0.7602 0.5249 0.027 Uiso 1 1 calc R . . C5 C 0.3576(2) 0.9412(5) 0.5726(3) 0.0185(10) Uani 1 1 d . . . C6 C 0.3112(2) 1.0057(6) 0.5264(3) 0.0227(12) Uani 1 1 d . . . C7 C 0.3101(2) 1.1379(6) 0.5096(3) 0.0237(12) Uani 1 1 d . . . H7 H 0.3393 1.1957 0.5255 0.028 Uiso 1 1 calc R . . C8 C 0.2581(2) 1.1774(5) 0.4644(3) 0.0165(10) Uani 1 1 d . . . H8 H 0.2483 1.2626 0.448 0.02 Uiso 1 1 calc R . . C9 C 0.2643(3) 0.9440(6) 0.4969(4) 0.0401(16) Uani 1 1 d . . . H9 H 0.2577 0.8543 0.5036 0.048 Uiso 1 1 calc R . . C10 C 0.4686(2) 1.0349(5) 0.7214(3) 0.0178(10) Uani 1 1 d . . . H10 H 0.5021 0.9965 0.7428 0.021 Uiso 1 1 calc R . . C11 C 0.5074(2) 1.2184(5) 0.7758(3) 0.0195(11) Uani 1 1 d . . . C12 C 0.5572(3) 1.2283(6) 0.7274(5) 0.0209(15) Uani 1 1 d . . . C13 C 0.6044(2) 1.2822(6) 0.7663(4) 0.0307(14) Uani 1 1 d . . . H13 H 0.6387 1.2875 0.7352 0.037 Uiso 1 1 calc R . . C14 C 0.6028(2) 1.3278(6) 0.8478(4) 0.0307(13) Uani 1 1 d . . . H14 H 0.6362 1.359 0.8741 0.037 Uiso 1 1 calc R . . C15 C 0.5527(2) 1.3284(5) 0.8918(3) 0.0250(12) Uani 1 1 d . . . H15 H 0.5511 1.3671 0.9466 0.03 Uiso 1 1 calc R . . C16 C 0.5042(2) 1.2733(5) 0.8573(3) 0.0211(11) Uani 1 1 d . . . C17 C 0.5618(3) 1.1889(7) 0.6339(4) 0.0290(17) Uani 1 1 d . . . H17 H 0.5236 1.161 0.6142 0.035 Uiso 1 1 calc R . . C18 C 0.5796(3) 1.3079(7) 0.5806(4) 0.0355(15) Uani 1 1 d . . . H18A H 0.6175 1.3355 0.5978 0.053 Uiso 1 1 calc R . . H18B H 0.5528 1.3783 0.5903 0.053 Uiso 1 1 calc R . . H18C H 0.5798 1.2852 0.5199 0.053 Uiso 1 1 calc R . . C19 C 0.6022(3) 1.0815(7) 0.6170(4) 0.0452(17) Uani 1 1 d . . . H19A H 0.6395 1.1045 0.6392 0.068 Uiso 1 1 calc R . . H19B H 0.6048 1.0666 0.5554 0.068 Uiso 1 1 calc R . . H19C H 0.5888 1.003 0.6451 0.068 Uiso 1 1 calc R . . C20 C 0.4496(2) 1.2729(5) 0.9089(3) 0.0285(12) Uani 1 1 d . . . H20 H 0.4186 1.2388 0.872 0.034 Uiso 1 1 calc R . . C21 C 0.4547(3) 1.1871(8) 0.9859(4) 0.0437(18) Uani 1 1 d . . . H21A H 0.4609 1.098 0.9674 0.065 Uiso 1 1 calc R . . H21B H 0.42 1.192 1.0196 0.065 Uiso 1 1 calc R . . H21C H 0.4867 1.2155 1.0208 0.065 Uiso 1 1 calc R . . C22 C 0.4336(3) 1.4102(6) 0.9374(4) 0.0462(18) Uani 1 1 d . . . H22A H 0.4639 1.4456 0.973 0.069 Uiso 1 1 calc R . . H22B H 0.3985 1.4073 0.9703 0.069 Uiso 1 1 calc R . . H22C H 0.4284 1.4649 0.8871 0.069 Uiso 1 1 calc R . . C23 C 0.3660(2) 1.4428(5) 0.5729(3) 0.0201(11) Uani 1 1 d . . . C24 C 0.4215(2) 1.4097(4) 0.5999(3) 0.0211(11) Uani 1 1 d . . . H24 H 0.4506 1.3735 0.5657 0.025 Uiso 1 1 calc R . . C25 C 0.42505(17) 1.4416(4) 0.6884(5) 0.0253(10) Uani 1 1 d . . . H25 H 0.4579 1.4333 0.7227 0.03 Uiso 1 1 calc R . . C26 C 0.3733(2) 1.4862(5) 0.7165(3) 0.0239(12) Uani 1 1 d . . . H26 H 0.3646 1.5109 0.7733 0.029 Uiso 1 1 calc R . . C27 C 0.3351(2) 1.4891(5) 0.6461(3) 0.0213(12) Uani 1 1 d . . . C28 C 0.2788(2) 1.5345(5) 0.6353(4) 0.0285(13) Uani 1 1 d . . . H28 H 0.2574 1.5622 0.6831 0.034 Uiso 1 1 calc R . . C29 C 0.2563(2) 1.5378(6) 0.5562(4) 0.0364(15) Uani 1 1 d . . . H29 H 0.2192 1.5701 0.5483 0.044 Uiso 1 1 calc R . . C30 C 0.2872(3) 1.4939(6) 0.4852(4) 0.0367(15) Uani 1 1 d . . . H30 H 0.27 1.4974 0.4305 0.044 Uiso 1 1 calc R . . C31 C 0.3402(2) 1.4470(5) 0.4919(3) 0.0287(13) Uani 1 1 d . . . H31 H 0.3598 1.4174 0.4428 0.034 Uiso 1 1 calc R . . C32 C 0.3145(2) 1.0914(6) 0.8273(3) 0.0239(13) Uani 1 1 d . . . C33 C 0.3031(2) 1.2236(6) 0.8368(4) 0.0286(12) Uani 1 1 d . . . H33 H 0.3193 1.2791 0.8783 0.034 Uiso 1 1 calc R . . C34 C 0.2638(2) 1.2592(6) 0.7745(4) 0.0340(14) Uani 1 1 d . . . H34 H 0.2479 1.3427 0.7682 0.041 Uiso 1 1 calc R . . C35 C 0.2514(2) 1.1529(6) 0.7231(4) 0.0314(13) Uani 1 1 d . . . H35 H 0.227 1.1521 0.675 0.038 Uiso 1 1 calc R . . C36 C 0.2819(2) 1.0469(6) 0.7557(3) 0.0254(12) Uani 1 1 d . . . C37 C 0.2839(2) 0.9127(6) 0.7348(3) 0.0322(14) Uani 1 1 d . . . H37 H 0.2625 0.8805 0.6882 0.039 Uiso 1 1 calc R . . C38 C 0.3161(3) 0.8320(6) 0.7815(4) 0.0345(14) Uani 1 1 d . . . H38 H 0.3165 0.7427 0.768 0.041 Uiso 1 1 calc R . . C39 C 0.3490(2) 0.8773(6) 0.8496(4) 0.0330(14) Uani 1 1 d . . . H39 H 0.3724 0.8191 0.8802 0.04 Uiso 1 1 calc R . . C40 C 0.3478(3) 1.0027(6) 0.8721(3) 0.0285(14) Uani 1 1 d . . . H40 H 0.3698 1.0313 0.9191 0.034 Uiso 1 1 calc R . . C41 C 0.4314(4) 1.0741(9) 1.3868(5) 0.069(2) Uiso 1 1 d . . . H41 H 0.4275 0.9928 1.4141 0.082 Uiso 1 1 calc R . . C42 C 0.4745(4) 1.1497(11) 1.4057(6) 0.084(3) Uiso 1 1 d . . . H42 H 0.5019 1.1201 1.4453 0.101 Uiso 1 1 calc R . . C43 C 0.4808(5) 1.2694(9) 1.3702(6) 0.084(3) Uiso 1 1 d . . . H43 H 0.512 1.3211 1.387 0.101 Uiso 1 1 calc R . . C44 C 0.4470(4) 1.3124(8) 1.3167(5) 0.065(2) Uiso 1 1 d . . . H44 H 0.4534 1.3956 1.2932 0.078 Uiso 1 1 calc R . . C45 C 0.4014(5) 1.2442(9) 1.2908(7) 0.085(3) Uiso 1 1 d . . . C46 C 0.3917(4) 1.1139(10) 1.3269(6) 0.090(3) Uiso 1 1 d . . . H46 H 0.3607 1.0616 1.3103 0.108 Uiso 1 1 calc R . . C47 C 0.3735(8) 1.313(2) 1.2116(18) 0.276(11) Uiso 1 1 d . . . H47A H 0.3408 1.2631 1.1925 0.413 Uiso 1 1 calc R . . H47B H 0.401 1.3192 1.1652 0.413 Uiso 1 1 calc R . . H47C H 0.3612 1.3998 1.2281 0.413 Uiso 1 1 calc R . . N1 N 0.38933(17) 1.0136(4) 0.6258(3) 0.0164(9) Uani 1 1 d . . . N2 N 0.45898(16) 1.1539(4) 0.7398(2) 0.0159(9) Uani 1 1 d . . . S1 S 0.21977(9) 1.0447(2) 0.44761(15) 0.0643(6) Uani 1 1 d . . . Yb1 Yb 0.360315(7) 1.228938(15) 0.68874(3) 0.01666(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(2) 0.020(2) 0.015(3) -0.0006(19) 0.0049(18) -0.0013(19) C2 0.019(2) 0.017(2) 0.023(3) 0.0010(19) 0.0061(18) 0.002(2) C3 0.024(3) 0.019(3) 0.029(3) -0.002(2) 0.006(2) -0.001(2) C4 0.025(3) 0.022(3) 0.022(3) -0.003(2) 0.003(2) -0.008(2) C5 0.016(2) 0.015(3) 0.024(2) -0.007(2) 0.004(2) -0.004(2) C6 0.018(3) 0.022(3) 0.028(3) -0.004(2) -0.001(2) -0.004(2) C7 0.021(3) 0.024(3) 0.027(3) -0.003(3) -0.007(2) 0.004(2) C8 0.025(3) 0.008(2) 0.017(2) -0.0008(19) -0.013(2) -0.003(2) C9 0.032(3) 0.032(4) 0.056(4) -0.003(3) -0.018(3) -0.008(3) C10 0.015(2) 0.022(3) 0.017(2) 0.002(2) -0.0009(19) 0.001(2) C11 0.021(3) 0.017(3) 0.020(2) 0.005(2) -0.006(2) -0.001(2) C12 0.015(3) 0.022(3) 0.025(3) -0.001(3) -0.001(2) 0.000(2) C13 0.014(3) 0.045(4) 0.033(3) 0.000(3) 0.000(2) -0.007(3) C14 0.022(3) 0.035(3) 0.035(3) -0.004(3) -0.009(3) -0.006(3) C15 0.026(3) 0.028(3) 0.022(2) -0.007(2) -0.009(2) -0.002(2) C16 0.019(2) 0.020(3) 0.025(3) 0.001(2) -0.003(2) 0.005(2) C17 0.024(4) 0.041(4) 0.022(3) -0.006(3) 0.001(3) -0.007(3) C18 0.021(3) 0.054(4) 0.032(3) 0.002(3) -0.003(3) -0.006(3) C19 0.047(4) 0.052(4) 0.036(3) -0.018(3) 0.013(3) -0.002(3) C20 0.025(3) 0.032(3) 0.028(3) -0.012(3) -0.002(2) -0.002(3) C21 0.037(4) 0.063(5) 0.031(3) 0.015(3) -0.008(3) -0.007(4) C22 0.034(4) 0.056(4) 0.049(4) -0.024(3) 0.004(3) 0.012(3) C23 0.022(3) 0.014(3) 0.024(2) 0.004(2) -0.004(2) -0.002(2) C24 0.019(3) 0.012(2) 0.033(3) 0.005(2) 0.005(2) 0.001(2) C25 0.021(2) 0.018(2) 0.037(2) 0.015(5) -0.016(4) -0.0045(18) C26 0.036(3) 0.015(3) 0.021(3) -0.003(2) -0.003(2) 0.000(2) C27 0.018(3) 0.016(3) 0.030(3) 0.003(2) -0.001(2) -0.001(2) C28 0.022(3) 0.022(3) 0.041(3) 0.010(3) 0.009(3) 0.004(2) C29 0.019(3) 0.034(4) 0.057(4) 0.016(3) -0.006(3) -0.002(3) C30 0.034(3) 0.032(3) 0.044(4) 0.022(3) -0.024(3) -0.012(3) C31 0.034(3) 0.023(3) 0.029(3) 0.009(2) -0.001(3) -0.007(2) C32 0.013(3) 0.035(4) 0.023(3) -0.002(3) 0.007(2) -0.003(3) C33 0.026(3) 0.030(3) 0.030(3) -0.009(3) 0.012(2) -0.003(3) C34 0.021(3) 0.040(4) 0.041(3) 0.008(3) 0.013(3) 0.011(3) C35 0.016(3) 0.042(4) 0.037(3) 0.002(3) -0.004(2) 0.002(3) C36 0.017(3) 0.032(3) 0.027(3) -0.004(2) 0.005(2) -0.008(2) C37 0.033(3) 0.032(4) 0.031(3) -0.007(3) 0.010(3) -0.012(3) C38 0.041(4) 0.020(3) 0.043(3) 0.004(3) 0.023(3) -0.003(3) C39 0.034(4) 0.027(4) 0.037(3) 0.008(3) 0.008(3) 0.003(3) C40 0.033(4) 0.032(4) 0.020(3) 0.005(2) 0.011(2) -0.007(3) N1 0.017(2) 0.019(2) 0.013(2) -0.0006(17) -0.0004(17) -0.0039(18) N2 0.017(2) 0.018(2) 0.0131(19) -0.0002(17) -0.0013(16) -0.0011(17) S1 0.0480(11) 0.0480(11) 0.0967(15) 0.0021(11) -0.0343(11) -0.0058(9) Yb1 0.01469(8) 0.01574(8) 0.01956(8) -0.0005(3) 0.0013(2) 0.00076(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.344(6) . ? C1 C2 1.382(7) . ? C1 C10 1.462(6) . ? C2 C3 1.369(7) . ? C2 H2 0.95 . ? C3 C4 1.387(8) . ? C3 H3 0.95 . ? C4 C5 1.395(8) . ? C4 H4 0.95 . ? C5 N1 1.351(6) . ? C5 C6 1.478(7) . ? C6 C9 1.363(7) . ? C6 C7 1.397(8) . ? C7 C8 1.479(7) . ? C7 Yb1 3.194(5) . ? C7 H7 0.95 . ? C8 S1 1.671(5) . ? C8 H8 0.95 . ? C9 S1 1.675(6) . ? C9 H9 0.95 . ? C10 N2 1.289(6) . ? C10 H10 0.95 . ? C11 C16 1.402(7) . ? C11 C12 1.407(9) . ? C11 N2 1.444(6) . ? C12 C13 1.390(9) . ? C12 C17 1.526(7) . ? C13 C14 1.364(8) . ? C13 H13 0.95 . ? C14 C15 1.371(7) . ? C14 H14 0.95 . ? C15 C16 1.394(7) . ? C15 H15 0.95 . ? C16 C20 1.526(8) . ? C17 C19 1.492(9) . ? C17 C18 1.550(10) . ? C17 H17 1 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C21 1.506(8) . ? C20 C22 1.540(8) . ? C20 H20 1 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C31 1.410(7) . ? C23 C24 1.423(7) . ? C23 C27 1.444(7) . ? C23 Yb1 2.872(5) . ? C24 C25 1.430(9) . ? C24 Yb1 2.751(5) . ? C24 H24 0.95 . ? C25 C26 1.383(7) . ? C25 Yb1 2.688(4) . ? C25 H25 0.95 . ? C26 C27 1.429(7) . ? C26 Yb1 2.723(5) . ? C26 H26 0.95 . ? C27 C28 1.424(7) . ? C27 Yb1 2.845(5) . ? C28 C29 1.350(8) . ? C28 H28 0.95 . ? C29 C30 1.407(9) . ? C29 H29 0.95 . ? C30 C31 1.353(8) . ? C30 H30 0.95 . ? C31 H31 0.95 . ? C32 C40 1.402(8) . ? C32 C33 1.407(8) . ? C32 C36 1.438(7) . ? C32 Yb1 2.818(6) . ? C33 C34 1.400(8) . ? C33 Yb1 2.690(5) . ? C33 H33 0.95 . ? C34 C35 1.399(8) . ? C34 Yb1 2.673(5) . ? C34 H34 0.95 . ? C35 C36 1.412(8) . ? C35 Yb1 2.751(5) . ? C35 H35 0.95 . ? C36 C37 1.432(8) . ? C36 Yb1 2.850(5) . ? C37 C38 1.349(8) . ? C37 H37 0.95 . ? C38 C39 1.405(8) . ? C38 H38 0.95 . ? C39 C40 1.349(9) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? C41 C42 1.322(12) . ? C41 C46 1.393(12) . ? C41 H41 0.95 . ? C42 C43 1.370(14) . ? C42 H42 0.95 . ? C43 C44 1.243(12) . ? C43 H43 0.95 . ? C44 C45 1.354(12) . ? C44 H44 0.95 . ? C45 C46 1.484(13) . ? C45 C47 1.58(3) . ? C46 H46 0.95 . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? N1 Yb1 2.538(4) . ? N2 Yb1 2.591(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 C1 C2 122.8(4) . . ? N1 C1 C10 118.6(4) . . ? C2 C1 C10 118.4(4) . . ? C3 C2 C1 119.6(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 118.1(5) . . ? C2 C3 H3 121 . . ? C4 C3 H3 121 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 121.0(5) . . ? N1 C5 C6 117.7(4) . . ? C4 C5 C6 121.3(5) . . ? C9 C6 C7 112.4(5) . . ? C9 C6 C5 124.1(5) . . ? C7 C6 C5 123.5(5) . . ? C6 C7 C8 112.2(5) . . ? C6 C7 Yb1 96.8(4) . . ? C8 C7 Yb1 130.5(3) . . ? C6 C7 H7 123.9 . . ? C8 C7 H7 123.9 . . ? Yb1 C7 H7 46.5 . . ? C7 C8 S1 107.5(4) . . ? C7 C8 H8 126.3 . . ? S1 C8 H8 126.3 . . ? C6 C9 S1 112.2(5) . . ? C6 C9 H9 123.9 . . ? S1 C9 H9 123.9 . . ? N2 C10 C1 123.8(4) . . ? N2 C10 H10 118.1 . . ? C1 C10 H10 118.1 . . ? C16 C11 C12 120.5(5) . . ? C16 C11 N2 120.1(4) . . ? C12 C11 N2 119.3(5) . . ? C13 C12 C11 117.8(6) . . ? C13 C12 C17 118.2(8) . . ? C11 C12 C17 123.9(7) . . ? C14 C13 C12 121.9(6) . . ? C14 C13 H13 119 . . ? C12 C13 H13 119 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 121.1(5) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 118.4(5) . . ? C15 C16 C20 119.7(5) . . ? C11 C16 C20 122.0(5) . . ? C19 C17 C12 114.6(6) . . ? C19 C17 C18 108.9(6) . . ? C12 C17 C18 108.9(6) . . ? C19 C17 H17 108.1 . . ? C12 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C16 111.0(5) . . ? C21 C20 C22 109.5(5) . . ? C16 C20 C22 111.1(5) . . ? C21 C20 H20 108.4 . . ? C16 C20 H20 108.4 . . ? C22 C20 H20 108.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 C23 C24 132.5(5) . . ? C31 C23 C27 119.0(5) . . ? C24 C23 C27 108.2(4) . . ? C31 C23 Yb1 125.0(3) . . ? C24 C23 Yb1 70.7(3) . . ? C27 C23 Yb1 74.3(3) . . ? C23 C24 C25 106.7(4) . . ? C23 C24 Yb1 80.1(3) . . ? C25 C24 Yb1 72.3(2) . . ? C23 C24 H24 126.7 . . ? C25 C24 H24 126.7 . . ? Yb1 C24 H24 113.4 . . ? C26 C25 C24 109.5(5) . . ? C26 C25 Yb1 76.6(3) . . ? C24 C25 Yb1 77.2(3) . . ? C26 C25 H25 125.2 . . ? C24 C25 H25 125.2 . . ? Yb1 C25 H25 113.1 . . ? C25 C26 C27 108.9(5) . . ? C25 C26 Yb1 73.8(3) . . ? C27 C26 Yb1 80.0(3) . . ? C25 C26 H26 125.6 . . ? C27 C26 H26 125.6 . . ? Yb1 C26 H26 113 . . ? C28 C27 C26 133.8(5) . . ? C28 C27 C23 119.4(5) . . ? C26 C27 C23 106.6(4) . . ? C28 C27 Yb1 122.6(4) . . ? C26 C27 Yb1 70.4(3) . . ? C23 C27 Yb1 76.4(3) . . ? C29 C28 C27 119.1(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 121.0(5) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 122.5(5) . . ? C31 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C30 C31 C23 118.9(6) . . ? C30 C31 H31 120.5 . . ? C23 C31 H31 120.5 . . ? C40 C32 C33 134.0(6) . . ? C40 C32 C36 118.9(6) . . ? C33 C32 C36 107.1(5) . . ? C40 C32 Yb1 120.2(3) . . ? C33 C32 Yb1 70.2(3) . . ? C36 C32 Yb1 76.5(3) . . ? C34 C33 C32 108.1(5) . . ? C34 C33 Yb1 74.2(3) . . ? C32 C33 Yb1 80.3(3) . . ? C34 C33 H33 125.9 . . ? C32 C33 H33 125.9 . . ? Yb1 C33 H33 112.1 . . ? C35 C34 C33 109.5(5) . . ? C35 C34 Yb1 78.2(3) . . ? C33 C34 Yb1 75.5(3) . . ? C35 C34 H34 125.3 . . ? C33 C34 H34 125.3 . . ? Yb1 C34 H34 113.2 . . ? C34 C35 C36 107.4(5) . . ? C34 C35 Yb1 72.0(3) . . ? C36 C35 Yb1 79.3(3) . . ? C34 C35 H35 126.3 . . ? C36 C35 H35 126.3 . . ? Yb1 C35 H35 114.7 . . ? C35 C36 C37 133.7(5) . . ? C35 C36 C32 107.9(5) . . ? C37 C36 C32 118.3(5) . . ? C35 C36 Yb1 71.6(3) . . ? C37 C36 Yb1 122.7(3) . . ? C32 C36 Yb1 74.1(3) . . ? C38 C37 C36 119.9(5) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 121.3(6) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C40 C39 C38 120.7(6) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C32 120.9(6) . . ? C39 C40 H40 119.5 . . ? C32 C40 H40 119.5 . . ? C42 C41 C46 119.8(10) . . ? C42 C41 H41 120.1 . . ? C46 C41 H41 120.1 . . ? C41 C42 C43 122.2(11) . . ? C41 C42 H42 118.9 . . ? C43 C42 H42 118.9 . . ? C44 C43 C42 122.0(11) . . ? C44 C43 H43 119 . . ? C42 C43 H43 119 . . ? C43 C44 C45 121.9(10) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C44 C45 C46 119.1(10) . . ? C44 C45 C47 109.5(11) . . ? C46 C45 C47 130.4(13) . . ? C41 C46 C45 115.0(10) . . ? C41 C46 H46 122.5 . . ? C45 C46 H46 122.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C1 N1 C5 118.2(4) . . ? C1 N1 Yb1 113.3(3) . . ? C5 N1 Yb1 125.4(3) . . ? C10 N2 C11 113.0(4) . . ? C10 N2 Yb1 112.3(3) . . ? C11 N2 Yb1 134.3(3) . . ? C8 S1 C9 95.7(3) . . ? N1 Yb1 N2 67.12(13) . . ? N1 Yb1 C34 122.08(16) . . ? N2 Yb1 C34 130.71(15) . . ? N1 Yb1 C25 124.60(16) . . ? N2 Yb1 C25 74.47(13) . . ? C34 Yb1 C25 113.13(19) . . ? N1 Yb1 C33 117.01(16) . . ? N2 Yb1 C33 100.49(16) . . ? C34 Yb1 C33 30.26(18) . . ? C25 Yb1 C33 107.8(2) . . ? N1 Yb1 C26 153.52(15) . . ? N2 Yb1 C26 98.25(15) . . ? C34 Yb1 C26 84.31(18) . . ? C25 Yb1 C26 29.61(15) . . ? C33 Yb1 C26 86.52(17) . . ? N1 Yb1 C24 105.12(14) . . ? N2 Yb1 C24 83.44(14) . . ? C34 Yb1 C24 128.76(17) . . ? C25 Yb1 C24 30.5(2) . . ? C33 Yb1 C24 135.83(17) . . ? C26 Yb1 C24 49.64(15) . . ? N1 Yb1 C35 94.44(15) . . ? N2 Yb1 C35 134.39(15) . . ? C34 Yb1 C35 29.84(18) . . ? C25 Yb1 C35 140.46(16) . . ? C33 Yb1 C35 49.64(17) . . ? C26 Yb1 C35 110.85(17) . . ? C24 Yb1 C35 142.11(16) . . ? N1 Yb1 C32 87.59(16) . . ? N2 Yb1 C32 87.56(14) . . ? C34 Yb1 C32 48.81(17) . . ? C25 Yb1 C32 129.6(2) . . ? C33 Yb1 C32 29.48(17) . . ? C26 Yb1 C32 114.67(17) . . ? C24 Yb1 C32 159.99(16) . . ? C35 Yb1 C32 48.87(16) . . ? N1 Yb1 C27 143.23(15) . . ? N2 Yb1 C27 123.20(14) . . ? C34 Yb1 C27 80.03(17) . . ? C25 Yb1 C27 48.73(14) . . ? C33 Yb1 C27 96.70(17) . . ? C26 Yb1 C27 29.63(14) . . ? C24 Yb1 C27 49.03(15) . . ? C35 Yb1 C27 96.95(16) . . ? C32 Yb1 C27 125.54(17) . . ? N1 Yb1 C36 74.68(14) . . ? N2 Yb1 C36 105.97(14) . . ? C34 Yb1 C36 48.30(17) . . ? C25 Yb1 C36 156.5(2) . . ? C33 Yb1 C36 48.69(16) . . ? C26 Yb1 C36 131.68(16) . . ? C24 Yb1 C36 169.26(15) . . ? C35 Yb1 C36 29.14(16) . . ? C32 Yb1 C36 29.40(15) . . ? C27 Yb1 C36 125.36(16) . . ? N1 Yb1 C23 114.95(14) . . ? N2 Yb1 C23 112.65(13) . . ? C34 Yb1 C23 105.54(16) . . ? C25 Yb1 C23 48.49(18) . . ? C33 Yb1 C23 125.87(17) . . ? C26 Yb1 C23 48.52(15) . . ? C24 Yb1 C23 29.22(14) . . ? C35 Yb1 C23 112.94(15) . . ? C32 Yb1 C23 153.87(17) . . ? C27 Yb1 C23 29.26(14) . . ? C36 Yb1 C23 140.92(15) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'Yb_2Th_ccdc_deposit_rinumerato.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-12-20 at 13:11:29 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : ybind7m data_Yb_2Th _database_code_depnum_ccdc_archive 'CCDC 794890' #TrackingRef 'Yb_2Th_ccdc_deposit_rinumerato.cif' _audit_creation_date 2010-12-20T13:11:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C40 H38 N2 S Yb, C7 H8' _chemical_formula_sum 'C47 H46 N2 S Yb' _chemical_formula_weight 843.96 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.6885(7) _cell_length_b 10.4564(3) _cell_length_c 15.6524(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3877.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.501 _exptl_absorpt_correction_type multi-scan #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_unetI/netI 0.0249 _diffrn_reflns_number 31999 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 7571 _reflns_number_gt 7371 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0219P)^2^+1.5663P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7571 _refine_ls_number_parameters 465 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.019 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0458 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.054 _refine_ls_shift/su_mean 0.002 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(5) _refine_diff_density_max 1.41 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 C 0.56897(7) 0.04286(17) -0.24897(11) 0.0175(5) Uani 1 1 d . . . C2 C 0.55689(8) 0.17232(18) -0.25440(11) 0.0211(5) Uani 1 1 d . . . H2 H 0.5269 0.2084 -0.222 0.025 Uiso 1 1 calc R . . C3 C 0.58926(10) 0.24808(18) -0.30779(14) 0.0217(5) Uani 1 1 d . . . H3 H 0.5821 0.3372 -0.312 0.026 Uiso 1 1 calc R . . C4 C 0.63216(9) 0.1929(2) -0.35493(13) 0.0215(5) Uani 1 1 d . . . H4 H 0.6545 0.2433 -0.3925 0.026 Uiso 1 1 calc R . . C5 C 0.64222(8) 0.06098(19) -0.34648(13) 0.0167(4) Uani 1 1 d . . . C6 C 0.68678(9) -0.00124(19) -0.39467(13) 0.0228(5) Uani 1 1 d . . . C7 C 0.73224(11) 0.0494(2) -0.43544(17) 0.0438(7) Uani 1 1 d . . . H7 H 0.7397 0.1385 -0.4387 0.053 Uiso 1 1 calc R . . C8 C 0.76725(11) -0.0448(3) -0.4725(2) 0.0545(8) Uani 1 1 d . . . H8 H 0.8009 -0.0254 -0.5028 0.065 Uiso 1 1 calc R . . C9 C 0.74800(10) -0.1657(2) -0.46044(16) 0.0380(6) Uani 1 1 d . . . H9 H 0.7665 -0.2406 -0.4802 0.046 Uiso 1 1 calc R . . C10 C 0.53204(8) -0.03803(18) -0.19753(12) 0.0177(4) Uani 1 1 d . . . H10 H 0.4988 -0.0005 -0.1745 0.021 Uiso 1 1 calc R . . C11 C 0.49319(8) -0.22134(17) -0.14472(13) 0.0170(4) Uani 1 1 d . . . C12 C 0.44363(10) -0.2294(2) -0.19295(16) 0.0243(5) Uani 1 1 d . . . C13 C 0.39621(10) -0.2808(2) -0.15405(17) 0.0310(6) Uani 1 1 d . . . H13 H 0.3618 -0.2843 -0.1851 0.037 Uiso 1 1 calc R . . C14 C 0.39753(9) -0.3271(2) -0.07165(15) 0.0318(6) Uani 1 1 d . . . H14 H 0.364 -0.3584 -0.0456 0.038 Uiso 1 1 calc R . . C15 C 0.44773(9) -0.3277(2) -0.02743(13) 0.0263(5) Uani 1 1 d . . . H15 H 0.449 -0.3644 0.0281 0.032 Uiso 1 1 calc R . . C16 C 0.49655(9) -0.27588(18) -0.06231(13) 0.0206(5) Uani 1 1 d . . . C17 C 0.43937(10) -0.1928(3) -0.28695(15) 0.0272(6) Uani 1 1 d . . . H17 H 0.4778 -0.1664 -0.3069 0.033 Uiso 1 1 calc R . . C18 C 0.39897(11) -0.0817(3) -0.30272(17) 0.0407(6) Uani 1 1 d . . . H18A H 0.3617 -0.103 -0.2797 0.061 Uiso 1 1 calc R . . H18B H 0.3959 -0.0659 -0.3643 0.061 Uiso 1 1 calc R . . H18C H 0.4134 -0.0048 -0.2743 0.061 Uiso 1 1 calc R . . C19 C 0.42058(11) -0.3096(3) -0.34070(16) 0.0374(6) Uani 1 1 d . . . H19A H 0.445 -0.3827 -0.3278 0.056 Uiso 1 1 calc R . . H19B H 0.4234 -0.2887 -0.4016 0.056 Uiso 1 1 calc R . . H19C H 0.3814 -0.3313 -0.3267 0.056 Uiso 1 1 calc R . . C20 C 0.55110(10) -0.2760(2) -0.01123(14) 0.0255(5) Uani 1 1 d . . . H20 H 0.582 -0.2417 -0.0483 0.031 Uiso 1 1 calc R . . C21 C 0.56670(11) -0.4124(2) 0.01548(16) 0.0380(6) Uani 1 1 d . . . H21A H 0.5379 -0.4457 0.0546 0.057 Uiso 1 1 calc R . . H21B H 0.6035 -0.4118 0.0442 0.057 Uiso 1 1 calc R . . H21C H 0.5687 -0.4671 -0.0353 0.057 Uiso 1 1 calc R . . C22 C 0.54687(11) -0.1920(3) 0.06844(16) 0.0395(6) Uani 1 1 d . . . H22A H 0.5345 -0.106 0.0521 0.059 Uiso 1 1 calc R . . H22B H 0.5839 -0.187 0.0961 0.059 Uiso 1 1 calc R . . H22C H 0.5195 -0.2293 0.1082 0.059 Uiso 1 1 calc R . . C23 C 0.63403(8) -0.44745(19) -0.34714(13) 0.0197(5) Uani 1 1 d . . . C24 C 0.57862(8) -0.41467(18) -0.31881(13) 0.0207(4) Uani 1 1 d . . . H24 H 0.5493 -0.3789 -0.3527 0.025 Uiso 1 1 calc R . . C25 C 0.57545(7) -0.44499(14) -0.2319(2) 0.0221(4) Uani 1 1 d . . . H25 H 0.5425 -0.4371 -0.1978 0.027 Uiso 1 1 calc R . . C26 C 0.62800(9) -0.48872(19) -0.20210(13) 0.0221(5) Uani 1 1 d . . . H26 H 0.637 -0.512 -0.145 0.027 Uiso 1 1 calc R . . C27 C 0.66548(8) -0.49171(18) -0.27383(13) 0.0207(4) Uani 1 1 d . . . C28 C 0.72134(9) -0.5340(2) -0.28530(15) 0.0285(5) Uani 1 1 d . . . H28 H 0.7428 -0.5616 -0.2375 0.034 Uiso 1 1 calc R . . C29 C 0.74469(9) -0.5356(2) -0.36492(16) 0.0345(6) Uani 1 1 d . . . H29 H 0.7823 -0.5655 -0.3721 0.041 Uiso 1 1 calc R . . C30 C 0.71367(10) -0.4930(2) -0.43739(15) 0.0305(5) Uani 1 1 d . . . H30 H 0.7307 -0.4951 -0.4923 0.037 Uiso 1 1 calc R . . C31 C 0.65981(10) -0.4495(2) -0.42884(14) 0.0256(5) Uani 1 1 d . . . H31 H 0.6395 -0.4206 -0.4775 0.031 Uiso 1 1 calc R . . C32 C 0.71846(8) -0.0530(2) -0.16399(13) 0.0244(5) Uani 1 1 d . . . C33 C 0.74857(9) -0.1593(2) -0.19512(15) 0.0301(5) Uani 1 1 d . . . H33 H 0.7732 -0.1596 -0.243 0.036 Uiso 1 1 calc R . . C34 C 0.73587(10) -0.2641(2) -0.14336(16) 0.0290(6) Uani 1 1 d . . . H34 H 0.7519 -0.347 -0.1486 0.035 Uiso 1 1 calc R . . C35 C 0.69528(10) -0.2272(2) -0.08192(14) 0.0253(5) Uani 1 1 d . . . H35 H 0.6781 -0.281 -0.0405 0.03 Uiso 1 1 calc R . . C36 C 0.68494(8) -0.0948(2) -0.09366(13) 0.0226(5) Uani 1 1 d . . . C37 C 0.65044(9) -0.0063(2) -0.04987(14) 0.0260(5) Uani 1 1 d . . . H37 H 0.6274 -0.034 -0.0038 0.031 Uiso 1 1 calc R . . C38 C 0.65040(10) 0.1191(2) -0.07392(16) 0.0331(6) Uani 1 1 d . . . H38 H 0.6269 0.1783 -0.0447 0.04 Uiso 1 1 calc R . . C39 C 0.68481(11) 0.1619(2) -0.14148(16) 0.0358(6) Uani 1 1 d . . . H39 H 0.6849 0.2501 -0.1559 0.043 Uiso 1 1 calc R . . C40 C 0.71784(10) 0.0799(2) -0.18641(14) 0.0326(6) Uani 1 1 d . . . H40 H 0.7404 0.1103 -0.2323 0.039 Uiso 1 1 calc R . . C41 C 0.60106(19) -0.2283(6) -0.6301(3) 0.1278(17) Uani 1 1 d . . . C42 C 0.55322(16) -0.3013(4) -0.5984(3) 0.0756(11) Uani 1 1 d . . . H42 H 0.5479 -0.3852 -0.6202 0.091 Uiso 1 1 calc R . . C43 C 0.5193(3) -0.2617(4) -0.5453(3) 0.0915(15) Uani 1 1 d . . . H43 H 0.4885 -0.3142 -0.5281 0.11 Uiso 1 1 calc R . . C44 C 0.5256(2) -0.1435(4) -0.5112(2) 0.0792(12) Uani 1 1 d . . . H44 H 0.499 -0.117 -0.4693 0.095 Uiso 1 1 calc R . . C45 C 0.56541(16) -0.0637(4) -0.5317(2) 0.0725(10) Uani 1 1 d . . . H45 H 0.5669 0.0184 -0.5057 0.087 Uiso 1 1 calc R . . C46 C 0.60687(15) -0.0993(5) -0.5930(3) 0.0958(15) Uani 1 1 d . . . H46 H 0.6366 -0.0432 -0.6092 0.115 Uiso 1 1 calc R . . C47 C 0.6320(4) -0.3029(10) -0.6944(5) 0.358(4) Uani 1 1 d . . . H47A H 0.6371 -0.2512 -0.7461 0.536 Uiso 1 1 calc R . . H47B H 0.6106 -0.3803 -0.7084 0.536 Uiso 1 1 calc R . . H47C H 0.669 -0.327 -0.6716 0.536 Uiso 1 1 calc R . . N1 N 0.61115(6) -0.01398(15) -0.29413(11) 0.0157(4) Uani 1 1 d . . . N2 N 0.54138(6) -0.15638(15) -0.18130(10) 0.0159(4) Uani 1 1 d . . . S1 S 0.68602(2) -0.16466(5) -0.40496(3) 0.02230(11) Uani 1 1 d . . . Yb1 Yb 0.640004(2) -0.233145(6) -0.232212(12) 0.01452(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0174(8) 0.0162(8) 0.0188(12) -0.0007(7) -0.0027(7) 0.0011(6) C2 0.0215(8) 0.0163(9) 0.0254(12) -0.0033(7) -0.0031(7) 0.0008(7) C3 0.0258(11) 0.0130(8) 0.0263(11) -0.0002(7) -0.0067(9) -0.0011(7) C4 0.0247(10) 0.0170(10) 0.0229(10) 0.0031(9) -0.0019(8) -0.0039(8) C5 0.0194(9) 0.0126(9) 0.0182(9) 0.0021(8) -0.0026(7) -0.0016(7) C6 0.0268(10) 0.0185(10) 0.0232(10) 0.0022(8) 0.0045(8) -0.0044(8) C7 0.0501(14) 0.0225(11) 0.0589(16) -0.0039(11) 0.0280(12) -0.0070(11) C8 0.0484(14) 0.0362(14) 0.0788(19) -0.0093(13) 0.0435(14) -0.0120(12) C9 0.0388(12) 0.0296(12) 0.0455(13) -0.0044(10) 0.0227(11) 0.0004(10) C10 0.0166(9) 0.0186(9) 0.0178(8) -0.0052(7) -0.0008(7) 0.0013(8) C11 0.0174(9) 0.0147(9) 0.0189(9) 0.0000(7) 0.0029(8) 0.0018(7) C12 0.0192(10) 0.0233(11) 0.0304(11) 0.0027(9) 0.0000(9) -0.0004(8) C13 0.0189(11) 0.0425(13) 0.0317(13) 0.0029(10) 0.0001(9) -0.0062(9) C14 0.0254(10) 0.0333(12) 0.0367(13) 0.0051(10) 0.0071(9) -0.0071(10) C15 0.0328(11) 0.0237(11) 0.0225(10) 0.0042(8) 0.0079(9) 0.0000(9) C16 0.0251(10) 0.0164(9) 0.0203(10) -0.0002(7) 0.0017(8) 0.0002(8) C17 0.0193(10) 0.0362(13) 0.0262(11) 0.0012(10) -0.0021(9) -0.0054(10) C18 0.0419(13) 0.0446(14) 0.0357(13) 0.0135(11) -0.0097(11) -0.0015(12) C19 0.0300(12) 0.0521(15) 0.0302(12) -0.0014(12) -0.0009(10) -0.0101(12) C20 0.0230(10) 0.0304(12) 0.0230(10) 0.0040(8) 0.0024(9) -0.0009(9) C21 0.0368(13) 0.0387(13) 0.0385(13) 0.0141(11) 0.0002(10) 0.0023(11) C22 0.0351(13) 0.0457(15) 0.0378(13) -0.0025(12) 0.0072(11) -0.0084(12) C23 0.0249(10) 0.0100(9) 0.0242(10) -0.0027(8) 0.0027(8) -0.0014(7) C24 0.0189(9) 0.0121(8) 0.0310(11) -0.0037(8) -0.0034(8) 0.0004(8) C25 0.0222(7) 0.0115(7) 0.0326(8) -0.0056(15) 0.0113(12) -0.0020(6) C26 0.0344(11) 0.0085(9) 0.0235(10) 0.0008(7) 0.0013(8) -0.0011(8) C27 0.0204(9) 0.0124(9) 0.0292(10) -0.0043(8) -0.0008(9) -0.0001(8) C28 0.0248(10) 0.0215(10) 0.0390(12) -0.0061(9) -0.0056(9) 0.0014(9) C29 0.0215(10) 0.0279(11) 0.0542(14) -0.0150(10) 0.0084(10) 0.0000(9) C30 0.0306(11) 0.0264(11) 0.0345(11) -0.0115(9) 0.0126(10) -0.0085(9) C31 0.0321(11) 0.0185(10) 0.0261(11) -0.0052(8) 0.0018(9) -0.0055(9) C32 0.0177(9) 0.0292(11) 0.0263(10) -0.0003(9) -0.0085(8) -0.0053(8) C33 0.0152(9) 0.0431(13) 0.0319(10) -0.0034(10) -0.0034(8) -0.0018(9) C34 0.0194(10) 0.0318(12) 0.0357(13) -0.0070(9) -0.0120(10) 0.0099(9) C35 0.0218(10) 0.0318(12) 0.0223(11) 0.0086(9) -0.0122(9) -0.0034(9) C36 0.0215(9) 0.0253(11) 0.0210(9) -0.0017(8) -0.0099(8) -0.0038(8) C37 0.0249(10) 0.0294(11) 0.0237(11) -0.0060(9) -0.0059(9) -0.0037(9) C38 0.0331(11) 0.0258(12) 0.0404(13) -0.0096(11) -0.0109(10) 0.0016(10) C39 0.0449(13) 0.0195(11) 0.0430(13) 0.0002(10) -0.0191(11) -0.0087(10) C40 0.0333(11) 0.0351(12) 0.0293(11) 0.0077(10) -0.0104(9) -0.0171(10) C41 0.104(2) 0.224(4) 0.056(3) 0.017(3) -0.008(2) 0.129(3) C42 0.064(2) 0.087(2) 0.076(2) 0.035(2) -0.0143(19) 0.011(2) C43 0.105(4) 0.092(3) 0.078(3) 0.023(2) -0.010(3) 0.021(3) C44 0.121(3) 0.065(2) 0.0517(19) 0.0198(17) -0.020(2) 0.000(2) C45 0.084(2) 0.072(2) 0.0617(19) 0.0070(17) -0.0352(18) 0.018(2) C46 0.057(2) 0.145(4) 0.086(3) 0.048(3) -0.0279(18) 0.016(2) C47 0.429(7) 0.553(10) 0.090(5) 0.025(5) 0.018(5) 0.429(7) N1 0.0158(7) 0.0145(7) 0.0168(7) -0.0014(6) 0.0000(6) -0.0016(6) N2 0.0189(8) 0.0133(7) 0.0157(8) -0.0001(6) 0.0012(6) -0.0011(6) S1 0.0247(2) 0.0166(2) 0.0256(2) 0.0009(2) 0.0064(2) 0.0000(2) Yb1 0.01388(3) 0.01298(3) 0.01668(3) 0.00024(9) -0.00058(5) 0.00073(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 C1 N1 1.360(2) . ? C1 C2 1.386(3) . ? C1 C10 1.459(3) . ? C2 C3 1.383(3) . ? C2 H2 0.95 . ? C3 C4 1.382(3) . ? C3 H3 0.95 . ? C4 C5 1.406(3) . ? C4 H4 0.95 . ? C5 N1 1.352(3) . ? C5 C6 1.451(3) . ? C6 C7 1.359(3) . ? C6 S1 1.717(2) . ? C7 C8 1.412(4) . ? C7 H7 0.95 . ? C8 C9 1.357(4) . ? C8 H8 0.95 . ? C9 S1 1.706(2) . ? C9 H9 0.95 . ? C10 N2 1.283(3) . ? C10 H10 0.95 . ? C11 C12 1.398(3) . ? C11 C16 1.413(3) . ? C11 N2 1.447(2) . ? C12 C13 1.386(3) . ? C12 C17 1.524(3) . ? C13 C14 1.378(4) . ? C13 H13 0.95 . ? C14 C15 1.376(3) . ? C14 H14 0.95 . ? C15 C16 1.389(3) . ? C15 H15 0.95 . ? C16 C20 1.520(3) . ? C17 C18 1.525(4) . ? C17 C19 1.548(4) . ? C17 H17 1 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C22 1.528(3) . ? C20 C21 1.532(3) . ? C20 H20 1 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C31 1.417(3) . ? C23 C24 1.427(3) . ? C23 C27 1.444(3) . ? C23 Yb1 2.877(2) . ? C24 C25 1.400(4) . ? C24 Yb1 2.7486(19) . ? C24 H24 0.95 . ? C25 C26 1.406(3) . ? C25 Yb1 2.6917(15) . ? C25 H25 0.95 . ? C26 C27 1.432(3) . ? C26 Yb1 2.729(2) . ? C26 H26 0.95 . ? C27 C28 1.407(3) . ? C27 Yb1 2.8458(19) . ? C28 C29 1.364(3) . ? C28 H28 0.95 . ? C29 C30 1.423(3) . ? C29 H29 0.95 . ? C30 C31 1.361(3) . ? C30 H30 0.95 . ? C31 H31 0.95 . ? C32 C33 1.408(3) . ? C32 C36 1.426(3) . ? C32 C40 1.433(3) . ? C32 Yb1 2.854(2) . ? C33 C34 1.396(3) . ? C33 Yb1 2.747(2) . ? C33 H33 0.95 . ? C34 C35 1.414(3) . ? C34 Yb1 2.683(2) . ? C34 H34 0.95 . ? C35 C36 1.418(3) . ? C35 Yb1 2.693(2) . ? C35 H35 0.95 . ? C36 C37 1.412(3) . ? C36 Yb1 2.816(2) . ? C37 C38 1.364(3) . ? C37 H37 0.95 . ? C38 C39 1.408(4) . ? C38 H38 0.95 . ? C39 C40 1.357(3) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? C41 C42 1.454(7) . ? C41 C46 1.475(8) . ? C41 C47 1.470(9) . ? C42 C43 1.228(7) . ? C42 H42 0.95 . ? C43 C44 1.355(6) . ? C43 H43 0.95 . ? C44 C45 1.300(6) . ? C44 H44 0.95 . ? C45 C46 1.423(6) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? N1 Yb1 2.5804(16) . ? N2 Yb1 2.5956(15) . ? S1 Yb1 3.0020(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.12(16) . . ? N1 C1 C10 118.28(16) . . ? C2 C1 C10 118.43(16) . . ? C3 C2 C1 118.80(18) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 119.42(18) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.94(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.24(18) . . ? N1 C5 C6 116.82(17) . . ? C4 C5 C6 120.94(18) . . ? C7 C6 C5 130.2(2) . . ? C7 C6 S1 110.61(17) . . ? C5 C6 S1 119.17(15) . . ? C6 C7 C8 112.8(2) . . ? C6 C7 H7 123.6 . . ? C8 C7 H7 123.6 . . ? C9 C8 C7 113.3(2) . . ? C9 C8 H8 123.4 . . ? C7 C8 H8 123.4 . . ? C8 C9 S1 110.74(19) . . ? C8 C9 H9 124.6 . . ? S1 C9 H9 124.6 . . ? N2 C10 C1 124.41(17) . . ? N2 C10 H10 117.8 . . ? C1 C10 H10 117.8 . . ? C12 C11 C16 121.07(19) . . ? C12 C11 N2 118.49(17) . . ? C16 C11 N2 120.44(18) . . ? C13 C12 C11 117.8(2) . . ? C13 C12 C17 117.9(2) . . ? C11 C12 C17 124.2(2) . . ? C14 C13 C12 121.9(2) . . ? C14 C13 H13 119 . . ? C12 C13 H13 119 . . ? C15 C14 C13 119.5(2) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 121.3(2) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C11 118.01(19) . . ? C15 C16 C20 120.06(19) . . ? C11 C16 C20 121.91(19) . . ? C12 C17 C18 112.9(2) . . ? C12 C17 C19 110.2(2) . . ? C18 C17 C19 109.4(2) . . ? C12 C17 H17 108.1 . . ? C18 C17 H17 108.1 . . ? C19 C17 H17 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 C22 111.91(19) . . ? C16 C20 C21 110.46(18) . . ? C22 C20 C21 109.1(2) . . ? C16 C20 H20 108.4 . . ? C22 C20 H20 108.4 . . ? C21 C20 H20 108.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 C23 C24 132.86(19) . . ? C31 C23 C27 119.33(18) . . ? C24 C23 C27 107.73(18) . . ? C31 C23 Yb1 123.70(14) . . ? C24 C23 Yb1 70.36(11) . . ? C27 C23 Yb1 74.19(11) . . ? C25 C24 C23 107.28(17) . . ? C25 C24 Yb1 72.85(10) . . ? C23 C24 Yb1 80.36(11) . . ? C25 C24 H24 126.4 . . ? C23 C24 H24 126.4 . . ? Yb1 C24 H24 113 . . ? C24 C25 C26 110.39(19) . . ? C24 C25 Yb1 77.36(10) . . ? C26 C25 Yb1 76.43(10) . . ? C24 C25 H25 124.8 . . ? C26 C25 H25 124.8 . . ? Yb1 C25 H25 113.4 . . ? C25 C26 C27 107.25(19) . . ? C25 C26 Yb1 73.52(10) . . ? C27 C26 Yb1 79.71(11) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? Yb1 C26 H26 112.9 . . ? C28 C27 C26 133.7(2) . . ? C28 C27 C23 118.99(19) . . ? C26 C27 C23 107.22(17) . . ? C28 C27 Yb1 121.84(13) . . ? C26 C27 Yb1 70.62(11) . . ? C23 C27 Yb1 76.58(11) . . ? C29 C28 C27 120.1(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 121.0(2) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 120.7(2) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C23 119.8(2) . . ? C30 C31 H31 120.1 . . ? C23 C31 H31 120.1 . . ? C33 C32 C36 107.88(19) . . ? C33 C32 C40 133.3(2) . . ? C36 C32 C40 118.7(2) . . ? C33 C32 Yb1 71.29(12) . . ? C36 C32 Yb1 73.97(11) . . ? C40 C32 Yb1 122.81(14) . . ? C34 C33 C32 108.1(2) . . ? C34 C33 Yb1 72.55(13) . . ? C32 C33 Yb1 79.68(12) . . ? C34 C33 H33 126 . . ? C32 C33 H33 126 . . ? Yb1 C33 H33 114.1 . . ? C33 C34 C35 109.1(2) . . ? C33 C34 Yb1 77.68(13) . . ? C35 C34 Yb1 75.16(13) . . ? C33 C34 H34 125.5 . . ? C35 C34 H34 125.5 . . ? Yb1 C34 H34 113.9 . . ? C34 C35 C36 107.22(19) . . ? C34 C35 Yb1 74.35(13) . . ? C36 C35 Yb1 79.95(12) . . ? C34 C35 H35 126.4 . . ? C36 C35 H35 126.4 . . ? Yb1 C35 H35 112 . . ? C37 C36 C35 132.6(2) . . ? C37 C36 C32 119.7(2) . . ? C35 C36 C32 107.66(19) . . ? C37 C36 Yb1 119.45(13) . . ? C35 C36 Yb1 70.33(12) . . ? C32 C36 Yb1 76.91(11) . . ? C38 C37 C36 119.8(2) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 120.8(2) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 121.5(2) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C32 119.4(2) . . ? C39 C40 H40 120.3 . . ? C32 C40 H40 120.3 . . ? C42 C41 C46 114.7(4) . . ? C42 C41 C47 110.1(6) . . ? C46 C41 C47 135.1(6) . . ? C43 C42 C41 124.4(5) . . ? C43 C42 H42 117.8 . . ? C41 C42 H42 117.8 . . ? C42 C43 C44 120.1(5) . . ? C42 C43 H43 120 . . ? C44 C43 H43 120 . . ? C45 C44 C43 124.6(5) . . ? C45 C44 H44 117.7 . . ? C43 C44 H44 117.7 . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45 120 . . ? C46 C45 H45 120 . . ? C45 C46 C41 116.1(4) . . ? C45 C46 H46 121.9 . . ? C41 C46 H46 121.9 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.4 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C5 N1 C1 117.48(16) . . ? C5 N1 Yb1 126.75(12) . . ? C1 N1 Yb1 112.79(12) . . ? C10 N2 C11 113.29(16) . . ? C10 N2 Yb1 113.13(12) . . ? C11 N2 Yb1 133.36(11) . . ? C9 S1 C6 92.58(11) . . ? C9 S1 Yb1 140.31(9) . . ? C6 S1 Yb1 99.02(7) . . ? N1 Yb1 N2 66.56(5) . . ? N1 Yb1 C34 121.75(6) . . ? N2 Yb1 C34 129.80(6) . . ? N1 Yb1 C25 125.53(6) . . ? N2 Yb1 C25 75.08(5) . . ? C34 Yb1 C25 112.36(7) . . ? N1 Yb1 C35 115.87(6) . . ? N2 Yb1 C35 99.34(6) . . ? C34 Yb1 C35 30.49(7) . . ? C25 Yb1 C35 107.06(8) . . ? N1 Yb1 C26 155.11(6) . . ? N2 Yb1 C26 98.98(6) . . ? C34 Yb1 C26 83.13(7) . . ? C25 Yb1 C26 30.05(6) . . ? C35 Yb1 C26 85.55(6) . . ? N1 Yb1 C33 94.46(6) . . ? N2 Yb1 C33 133.69(6) . . ? C34 Yb1 C33 29.76(7) . . ? C25 Yb1 C33 139.70(7) . . ? C35 Yb1 C33 49.74(7) . . ? C26 Yb1 C33 109.66(7) . . ? N1 Yb1 C24 106.74(5) . . ? N2 Yb1 C24 83.61(5) . . ? C34 Yb1 C24 128.33(6) . . ? C25 Yb1 C24 29.79(8) . . ? C35 Yb1 C24 134.75(6) . . ? C26 Yb1 C24 49.73(6) . . ? C33 Yb1 C24 142.52(6) . . ? N1 Yb1 C36 86.16(6) . . ? N2 Yb1 C36 86.84(5) . . ? C34 Yb1 C36 48.91(6) . . ? C25 Yb1 C36 129.49(8) . . ? C35 Yb1 C36 29.72(6) . . ? C26 Yb1 C36 114.18(6) . . ? C33 Yb1 C36 48.62(6) . . ? C24 Yb1 C36 159.16(6) . . ? N1 Yb1 C27 144.49(6) . . ? N2 Yb1 C27 123.71(5) . . ? C34 Yb1 C27 79.89(6) . . ? C25 Yb1 C27 48.63(5) . . ? C35 Yb1 C27 96.82(6) . . ? C26 Yb1 C27 29.67(6) . . ? C33 Yb1 C27 96.71(6) . . ? C24 Yb1 C27 48.95(6) . . ? C36 Yb1 C27 125.75(6) . . ? N1 Yb1 C32 74.14(5) . . ? N2 Yb1 C32 105.49(5) . . ? C34 Yb1 C32 48.27(6) . . ? C25 Yb1 C32 155.85(8) . . ? C35 Yb1 C32 48.79(6) . . ? C26 Yb1 C32 130.53(6) . . ? C33 Yb1 C32 29.04(7) . . ? C24 Yb1 C32 170.06(6) . . ? C36 Yb1 C32 29.13(6) . . ? C27 Yb1 C32 125.08(6) . . ? N1 Yb1 C23 116.35(5) . . ? N2 Yb1 C23 112.86(5) . . ? C34 Yb1 C23 105.77(6) . . ? C25 Yb1 C23 48.12(7) . . ? C35 Yb1 C23 126.02(6) . . ? C26 Yb1 C23 48.70(6) . . ? C33 Yb1 C23 113.40(6) . . ? C24 Yb1 C23 29.28(6) . . ? C36 Yb1 C23 154.20(6) . . ? C27 Yb1 C23 29.23(6) . . ? C32 Yb1 C23 141.28(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C5 C6 S1 16.8(2) . . . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'YbPh_ccdc_deposit_rinumerato.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-12-16 at 16:19:39 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : gg41 gg41_ccdc_deposit gg41 gg41_ox gg41 struct data_YbPh _database_code_depnum_ccdc_archive 'CCDC 794891' #TrackingRef 'YbPh_ccdc_deposit_rinumerato.cif' _audit_creation_date 2010-12-16T16:19:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H40 N2 Yb1' _chemical_formula_sum 'C42 H40 N2 Yb' _chemical_formula_weight 745.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.293(4) _cell_length_b 37.396(1) _cell_length_c 10.314(4) _cell_angle_alpha 90 _cell_angle_beta 114.897(5) _cell_angle_gamma 90 _cell_volume 3251(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9194 _cell_measurement_theta_min 4.1354 _cell_measurement_theta_max 26.4033 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.69302 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 0.0246826869 _diffrn_orient_matrix_ub_12 -0.0118650194 _diffrn_orient_matrix_ub_13 0.0589933015 _diffrn_orient_matrix_ub_21 0.0221731339 _diffrn_orient_matrix_ub_22 0.0147362542 _diffrn_orient_matrix_ub_23 0.0474058488 _diffrn_orient_matrix_ub_31 -0.0771627615 _diffrn_orient_matrix_ub_32 0.0004681461 _diffrn_orient_matrix_ub_33 -0.0022067024 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_unetI/netI 0.0728 _diffrn_reflns_number 24993 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 26.46 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.846 _diffrn_measured_fraction_theta_max 0.846 _reflns_number_total 5684 _reflns_number_gt 4174 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5684 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.066 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.283 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # 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' 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 C1 C 0.4090(5) 0.11789(12) -0.0207(5) 0.0146(11) Uani 1 1 d . . . C2 C 0.2716(5) 0.11675(13) -0.1455(5) 0.0175(11) Uani 1 1 d . . . H2 H 0.255 0.0982 -0.2133 0.021 Uiso 1 1 calc R . . C3 C 0.1579(6) 0.14309(13) -0.1700(5) 0.0203(12) Uani 1 1 d . . . H3 H 0.0619 0.1429 -0.2547 0.024 Uiso 1 1 calc R . . C4 C 0.1873(5) 0.16946(13) -0.0687(5) 0.0188(11) Uani 1 1 d . . . H4 H 0.1101 0.1874 -0.0821 0.023 Uiso 1 1 calc R . . C5 C 0.3296(5) 0.16977(13) 0.0530(5) 0.0144(11) Uani 1 1 d . . . C6 C 0.3597(5) 0.19709(12) 0.1655(5) 0.0159(11) Uani 1 1 d . . . C7 C 0.4341(5) 0.18750(13) 0.3095(5) 0.0185(11) Uani 1 1 d . . . H7 H 0.4716 0.1637 0.3348 0.022 Uiso 1 1 calc R . . C8 C 0.4541(5) 0.21195(13) 0.4156(5) 0.0214(12) Uani 1 1 d . . . H8 H 0.5049 0.205 0.5131 0.026 Uiso 1 1 calc R . . C9 C 0.4008(5) 0.24633(14) 0.3803(5) 0.0220(12) Uani 1 1 d . . . H9 H 0.4136 0.2631 0.4535 0.026 Uiso 1 1 calc R . . C10 C 0.3287(5) 0.25660(14) 0.2391(5) 0.0241(12) Uani 1 1 d . . . H10 H 0.2932 0.2805 0.215 0.029 Uiso 1 1 calc R . . C11 C 0.3080(5) 0.23201(13) 0.1320(5) 0.0215(12) Uani 1 1 d . . . H11 H 0.2579 0.2392 0.0348 0.026 Uiso 1 1 calc R . . C12 C 0.5234(6) 0.08872(13) 0.0161(5) 0.0176(11) Uani 1 1 d . . . H12 H 0.4949 0.068 -0.0429 0.021 Uiso 1 1 calc R . . C13 C 0.7426(5) 0.05533(12) 0.1572(5) 0.0158(11) Uani 1 1 d . . . C14 C 0.7046(5) 0.03084(13) 0.2386(5) 0.0196(12) Uani 1 1 d . . . C15 C 0.7865(5) -0.00167(13) 0.2721(5) 0.0220(12) Uani 1 1 d . . . H15 H 0.7589 -0.0193 0.3241 0.026 Uiso 1 1 calc R . . C16 C 0.9057(5) -0.00852(13) 0.2311(5) 0.0232(12) Uani 1 1 d . . . H16 H 0.9614 -0.0306 0.2556 0.028 Uiso 1 1 calc R . . C17 C 0.9452(6) 0.01685(13) 0.1536(5) 0.0235(12) Uani 1 1 d . . . H17 H 1.0285 0.0119 0.1259 0.028 Uiso 1 1 calc R . . C18 C 0.8665(5) 0.04928(13) 0.1155(5) 0.0186(11) Uani 1 1 d . . . C19 C 0.5739(5) 0.03704(13) 0.2890(5) 0.0230(12) Uani 1 1 d . . . H19 H 0.5432 0.0628 0.2733 0.028 Uiso 1 1 calc R . . C20 C 0.6306(6) 0.02921(14) 0.4485(5) 0.0318(14) Uani 1 1 d . . . H20A H 0.6424 0.0033 0.4644 0.048 Uiso 1 1 calc R . . H20B H 0.5527 0.0383 0.4812 0.048 Uiso 1 1 calc R . . H20C H 0.7331 0.0409 0.502 0.048 Uiso 1 1 calc R . . C21 C 0.4274(6) 0.01499(16) 0.2040(6) 0.0404(16) Uani 1 1 d . . . H21A H 0.3902 0.0204 0.1021 0.061 Uiso 1 1 calc R . . H21B H 0.3438 0.0208 0.2349 0.061 Uiso 1 1 calc R . . H21C H 0.4535 -0.0105 0.2201 0.061 Uiso 1 1 calc R . . C22 C 0.9064(5) 0.07630(13) 0.0269(5) 0.0210(12) Uani 1 1 d . . . H22 H 0.8698 0.1002 0.0443 0.025 Uiso 1 1 calc R . . C23 C 0.8164(6) 0.06798(14) -0.1327(5) 0.0304(13) Uani 1 1 d . . . H23A H 0.835 0.043 -0.1503 0.046 Uiso 1 1 calc R . . H23B H 0.8541 0.0838 -0.1877 0.046 Uiso 1 1 calc R . . H23C H 0.7027 0.0718 -0.1622 0.046 Uiso 1 1 calc R . . C24 C 1.0837(6) 0.07901(15) 0.0677(6) 0.0332(14) Uani 1 1 d . . . H24A H 1.141 0.0807 0.1719 0.05 Uiso 1 1 calc R . . H24B H 1.1051 0.1003 0.0235 0.05 Uiso 1 1 calc R . . H24C H 1.1191 0.0577 0.0341 0.05 Uiso 1 1 calc R . . C25 C 0.9495(5) 0.11271(13) 0.4787(5) 0.0185(11) Uani 1 1 d . . . C26 C 0.8099(5) 0.11991(14) 0.4985(5) 0.0216(12) Uani 1 1 d . . . H26 H 0.7344 0.1029 0.4995 0.026 Uiso 1 1 calc R . . C27 C 0.8054(6) 0.15749(14) 0.5164(5) 0.0248(13) Uani 1 1 d . . . H27 H 0.7271 0.1698 0.5357 0.03 Uiso 1 1 calc R . . C28 C 0.9328(5) 0.17366(14) 0.5015(4) 0.0205(12) Uani 1 1 d . . . H28 H 0.9541 0.1986 0.5062 0.025 Uiso 1 1 calc R . . C29 C 1.0242(5) 0.14660(13) 0.4785(4) 0.0185(12) Uani 1 1 d . . . C30 C 1.1691(6) 0.14676(14) 0.4617(5) 0.0223(12) Uani 1 1 d . . . H30 H 1.2178 0.1687 0.4569 0.027 Uiso 1 1 calc R . . C31 C 1.2368(6) 0.11504(15) 0.4525(5) 0.0265(13) Uani 1 1 d . . . H31 H 1.3346 0.1152 0.4439 0.032 Uiso 1 1 calc R . . C32 C 1.1649(6) 0.08198(15) 0.4557(5) 0.0259(13) Uani 1 1 d . . . H32 H 1.2156 0.0604 0.4497 0.031 Uiso 1 1 calc R . . C33 C 1.0237(6) 0.08050(14) 0.4671(5) 0.0237(12) Uani 1 1 d . . . H33 H 0.9757 0.0581 0.4673 0.028 Uiso 1 1 calc R . . C34 C 0.7784(5) 0.17649(13) -0.0070(5) 0.0186(11) Uani 1 1 d . . . C35 C 0.9292(6) 0.17797(13) 0.1141(5) 0.0204(12) Uani 1 1 d . . . H35 H 1.0182 0.1631 0.131 0.024 Uiso 1 1 calc R . . C36 C 0.9208(5) 0.20538(14) 0.2028(5) 0.0230(12) Uani 1 1 d . . . H36 H 1.0065 0.2128 0.2887 0.028 Uiso 1 1 calc R . . C37 C 0.7689(6) 0.22039(13) 0.1478(5) 0.0211(12) Uani 1 1 d . . . H37 H 0.7327 0.2387 0.1908 0.025 Uiso 1 1 calc R . . C38 C 0.6775(5) 0.20278(13) 0.0133(5) 0.0194(11) Uani 1 1 d . . . C39 C 0.5233(5) 0.20844(14) -0.0945(5) 0.0232(12) Uani 1 1 d . . . H39 H 0.4561 0.2259 -0.0818 0.028 Uiso 1 1 calc R . . C40 C 0.4713(6) 0.18869(14) -0.2169(5) 0.0248(12) Uani 1 1 d . . . H40 H 0.368 0.1927 -0.29 0.03 Uiso 1 1 calc R . . C41 C 0.5700(6) 0.16230(13) -0.2362(5) 0.0237(13) Uani 1 1 d . . . H41 H 0.5304 0.1483 -0.3208 0.028 Uiso 1 1 calc R . . C42 C 0.7213(6) 0.15659(13) -0.1351(5) 0.0206(11) Uani 1 1 d . . . H42 H 0.7873 0.1394 -0.1512 0.025 Uiso 1 1 calc R . . N1 N 0.4411(4) 0.14446(9) 0.0774(4) 0.0118(9) Uani 1 1 d . . . N2 N 0.6593(5) 0.08903(10) 0.1222(4) 0.0157(9) Uani 1 1 d . . . Yb1 Yb 0.74223(2) 0.152095(6) 0.234426(19) 0.01678(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(3) 0.010(3) 0.019(3) 0.002(2) 0.013(2) 0.002(2) C2 0.023(3) 0.020(3) 0.009(3) -0.003(2) 0.007(2) 0.000(2) C3 0.020(3) 0.026(3) 0.012(3) 0.003(2) 0.003(2) 0.000(2) C4 0.018(3) 0.019(3) 0.020(3) 0.007(2) 0.008(2) 0.003(2) C5 0.016(3) 0.014(3) 0.015(3) 0.006(2) 0.008(2) -0.002(2) C6 0.018(3) 0.014(3) 0.016(3) -0.003(2) 0.007(2) -0.002(2) C7 0.017(3) 0.016(3) 0.023(3) 0.001(2) 0.009(2) 0.001(2) C8 0.022(3) 0.024(3) 0.017(3) -0.001(2) 0.007(2) -0.001(2) C9 0.017(3) 0.026(3) 0.023(3) -0.009(2) 0.008(2) -0.001(2) C10 0.024(3) 0.021(3) 0.026(3) 0.000(2) 0.010(2) 0.006(2) C11 0.020(3) 0.021(3) 0.021(3) 0.003(2) 0.006(2) 0.006(2) C12 0.027(3) 0.011(3) 0.020(3) -0.002(2) 0.016(3) 0.000(2) C13 0.017(3) 0.015(3) 0.014(3) 0.000(2) 0.004(2) 0.002(2) C14 0.022(3) 0.024(3) 0.013(3) 0.006(2) 0.008(2) 0.010(2) C15 0.027(3) 0.016(3) 0.023(3) 0.004(2) 0.010(2) -0.005(2) C16 0.022(3) 0.019(3) 0.027(3) 0.005(2) 0.008(2) 0.003(2) C17 0.025(3) 0.020(3) 0.026(3) -0.001(2) 0.012(2) 0.003(2) C18 0.022(3) 0.015(3) 0.017(3) 0.001(2) 0.006(2) 0.003(2) C19 0.025(3) 0.014(3) 0.035(3) 0.007(2) 0.017(2) 0.002(2) C20 0.038(3) 0.025(4) 0.045(4) 0.005(3) 0.030(3) -0.003(3) C21 0.024(3) 0.045(4) 0.054(4) 0.000(3) 0.017(3) 0.000(3) C22 0.031(3) 0.012(3) 0.025(3) 0.003(2) 0.017(2) 0.005(2) C23 0.047(4) 0.018(3) 0.033(3) 0.004(2) 0.024(3) 0.009(3) C24 0.039(4) 0.027(4) 0.042(4) 0.003(3) 0.026(3) 0.002(3) C25 0.020(3) 0.016(3) 0.014(3) 0.003(2) 0.001(2) -0.003(2) C26 0.020(3) 0.025(3) 0.016(3) 0.003(2) 0.005(2) -0.003(2) C27 0.019(3) 0.039(4) 0.012(3) 0.002(2) 0.002(2) 0.007(2) C28 0.025(3) 0.020(3) 0.012(3) -0.002(2) 0.004(2) -0.001(2) C29 0.013(3) 0.027(3) 0.010(2) 0.001(2) -0.001(2) -0.001(2) C30 0.023(3) 0.024(3) 0.016(3) 0.003(2) 0.004(2) -0.003(2) C31 0.019(3) 0.039(4) 0.022(3) 0.000(3) 0.010(2) 0.000(3) C32 0.032(3) 0.026(3) 0.016(3) -0.002(2) 0.007(2) 0.012(3) C33 0.027(3) 0.018(3) 0.022(3) 0.002(2) 0.006(2) 0.001(2) C34 0.023(3) 0.020(3) 0.017(3) 0.003(2) 0.012(2) 0.000(2) C35 0.021(3) 0.017(3) 0.023(3) 0.008(2) 0.009(2) 0.000(2) C36 0.021(3) 0.023(3) 0.024(3) 0.005(2) 0.008(2) -0.007(2) C37 0.032(3) 0.016(3) 0.018(3) -0.004(2) 0.013(2) -0.004(2) C38 0.026(3) 0.012(3) 0.022(3) 0.008(2) 0.012(2) 0.001(2) C39 0.022(3) 0.022(3) 0.028(3) 0.011(2) 0.014(2) 0.006(2) C40 0.021(3) 0.029(3) 0.018(3) 0.009(2) 0.003(2) -0.003(2) C41 0.033(3) 0.023(3) 0.014(3) 0.000(2) 0.009(2) -0.007(2) C42 0.033(3) 0.014(3) 0.018(3) 0.002(2) 0.014(2) -0.001(2) N1 0.011(2) 0.010(2) 0.015(2) 0.0006(16) 0.0069(17) -0.0024(16) N2 0.020(2) 0.012(2) 0.018(2) 0.0016(17) 0.012(2) 0.0007(17) Yb1 0.01835(12) 0.01656(12) 0.01433(12) 0.00043(11) 0.00580(9) -0.00094(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.359(5) . ? C1 C2 1.380(6) . ? C1 C12 1.458(6) . ? C2 C3 1.388(6) . ? C2 H2 0.95 . ? C3 C4 1.378(6) . ? C3 H3 0.95 . ? C4 C5 1.388(6) . ? C4 H4 0.95 . ? C5 N1 1.346(5) . ? C5 C6 1.482(6) . ? C6 C11 1.384(6) . ? C6 C7 1.396(6) . ? C7 C8 1.377(6) . ? C7 H7 0.95 . ? C8 C9 1.371(6) . ? C8 H8 0.95 . ? C9 C10 1.377(6) . ? C9 H9 0.95 . ? C10 C11 1.387(6) . ? C10 H10 0.95 . ? C11 H11 0.95 . ? C12 N2 1.276(6) . ? C12 H12 0.95 . ? C13 C14 1.385(6) . ? C13 C18 1.406(6) . ? C13 N2 1.443(5) . ? C14 C15 1.398(6) . ? C14 C19 1.527(6) . ? C15 C16 1.366(6) . ? C15 H15 0.95 . ? C16 C17 1.385(6) . ? C16 H16 0.95 . ? C17 C18 1.385(6) . ? C17 H17 0.95 . ? C18 C22 1.510(6) . ? C19 C21 1.516(6) . ? C19 C20 1.529(6) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C24 1.522(6) . ? C22 C23 1.532(6) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C33 1.417(7) . ? C25 C26 1.422(6) . ? C25 C29 1.445(6) . ? C25 Yb1 2.853(5) . ? C26 C27 1.420(7) . ? C26 Yb1 2.796(5) . ? C26 H26 0.95 . ? C27 C28 1.394(6) . ? C27 Yb1 2.722(5) . ? C27 H27 0.95 . ? C28 C29 1.404(6) . ? C28 Yb1 2.696(4) . ? C28 H28 0.95 . ? C29 C30 1.428(6) . ? C29 Yb1 2.773(4) . ? C30 C31 1.365(7) . ? C30 H30 0.95 . ? C31 C32 1.412(7) . ? C31 H31 0.95 . ? C32 C33 1.368(7) . ? C32 H32 0.95 . ? C33 H33 0.95 . ? C34 C42 1.411(6) . ? C34 C35 1.433(6) . ? C34 C38 1.434(6) . ? C34 Yb1 2.802(5) . ? C35 C36 1.398(7) . ? C35 Yb1 2.703(5) . ? C35 H35 0.95 . ? C36 C37 1.398(6) . ? C36 Yb1 2.699(5) . ? C36 H36 0.95 . ? C37 C38 1.445(6) . ? C37 Yb1 2.751(5) . ? C37 H37 0.95 . ? C38 C39 1.412(6) . ? C38 Yb1 2.829(5) . ? C39 C40 1.364(7) . ? C39 H39 0.95 . ? C40 C41 1.417(7) . ? C40 H40 0.95 . ? C41 C42 1.369(6) . ? C41 H41 0.95 . ? C42 H42 0.95 . ? N1 Yb1 2.592(4) . ? N2 Yb1 2.597(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 C1 C2 122.9(4) . . ? N1 C1 C12 116.5(4) . . ? C2 C1 C12 120.5(4) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 118.5(4) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.1(4) . . ? C3 C4 H4 120 . . ? C5 C4 H4 120 . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 117.5(4) . . ? C4 C5 C6 120.5(4) . . ? C11 C6 C7 118.1(4) . . ? C11 C6 C5 121.6(4) . . ? C7 C6 C5 120.1(4) . . ? C8 C7 C6 121.1(5) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C9 C8 C7 119.9(5) . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C8 C9 C10 120.2(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 120.0(5) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C6 C11 C10 120.7(4) . . ? C6 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? N2 C12 C1 124.5(5) . . ? N2 C12 H12 117.7 . . ? C1 C12 H12 117.7 . . ? C14 C13 C18 121.9(4) . . ? C14 C13 N2 118.9(4) . . ? C18 C13 N2 119.1(4) . . ? C13 C14 C15 118.3(4) . . ? C13 C14 C19 123.2(4) . . ? C15 C14 C19 118.4(4) . . ? C16 C15 C14 121.0(5) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.7(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 121.8(5) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C13 117.2(4) . . ? C17 C18 C22 121.5(4) . . ? C13 C18 C22 121.3(4) . . ? C21 C19 C14 111.7(4) . . ? C21 C19 C20 109.7(4) . . ? C14 C19 C20 112.0(4) . . ? C21 C19 H19 107.8 . . ? C14 C19 H19 107.8 . . ? C20 C19 H19 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 113.0(4) . . ? C18 C22 C23 110.6(4) . . ? C24 C22 C23 110.4(4) . . ? C18 C22 H22 107.5 . . ? C24 C22 H22 107.5 . . ? C23 C22 H22 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C33 C25 C26 132.7(5) . . ? C33 C25 C29 119.6(4) . . ? C26 C25 C29 107.6(4) . . ? C33 C25 Yb1 122.4(3) . . ? C26 C25 Yb1 73.2(3) . . ? C29 C25 Yb1 72.1(2) . . ? C27 C26 C25 106.5(4) . . ? C27 C26 Yb1 72.2(3) . . ? C25 C26 Yb1 77.7(3) . . ? C27 C26 H26 126.7 . . ? C25 C26 H26 126.7 . . ? Yb1 C26 H26 115.8 . . ? C28 C27 C26 110.0(4) . . ? C28 C27 Yb1 74.1(3) . . ? C26 C27 Yb1 78.0(3) . . ? C28 C27 H27 125 . . ? C26 C27 H27 125 . . ? Yb1 C27 H27 114.8 . . ? C27 C28 C29 107.9(5) . . ? C27 C28 Yb1 76.1(3) . . ? C29 C28 Yb1 78.2(3) . . ? C27 C28 H28 126 . . ? C29 C28 H28 126 . . ? Yb1 C28 H28 112.2 . . ? C28 C29 C30 133.3(5) . . ? C28 C29 C25 107.9(4) . . ? C30 C29 C25 118.8(4) . . ? C28 C29 Yb1 72.1(2) . . ? C30 C29 Yb1 117.9(3) . . ? C25 C29 Yb1 78.2(2) . . ? C31 C30 C29 119.4(5) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 121.5(5) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 121.2(5) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C25 119.4(5) . . ? C32 C33 H33 120.3 . . ? C25 C33 H33 120.3 . . ? C42 C34 C35 132.9(5) . . ? C42 C34 C38 119.2(4) . . ? C35 C34 C38 107.8(4) . . ? C42 C34 Yb1 121.5(3) . . ? C35 C34 Yb1 71.1(3) . . ? C38 C34 Yb1 76.3(3) . . ? C36 C35 C34 107.2(4) . . ? C36 C35 Yb1 74.8(3) . . ? C34 C35 Yb1 78.7(3) . . ? C36 C35 H35 126.4 . . ? C34 C35 H35 126.4 . . ? Yb1 C35 H35 112.6 . . ? C35 C36 C37 110.7(4) . . ? C35 C36 Yb1 75.2(3) . . ? C37 C36 Yb1 77.2(3) . . ? C35 C36 H36 124.6 . . ? C37 C36 H36 124.6 . . ? Yb1 C36 H36 114.8 . . ? C36 C37 C38 107.0(4) . . ? C36 C37 Yb1 73.1(3) . . ? C38 C37 Yb1 78.0(3) . . ? C36 C37 H37 126.5 . . ? C38 C37 H37 126.5 . . ? Yb1 C37 H37 114.8 . . ? C39 C38 C34 119.8(4) . . ? C39 C38 C37 132.8(5) . . ? C34 C38 C37 107.3(4) . . ? C39 C38 Yb1 122.4(3) . . ? C34 C38 Yb1 74.2(3) . . ? C37 C38 Yb1 72.0(3) . . ? C40 C39 C38 119.6(5) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.6(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 121.3(5) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C34 119.4(5) . . ? C41 C42 H42 120.3 . . ? C34 C42 H42 120.3 . . ? C5 N1 C1 117.7(4) . . ? C5 N1 Yb1 125.6(3) . . ? C1 N1 Yb1 112.7(3) . . ? C12 N2 C13 116.1(4) . . ? C12 N2 Yb1 113.0(3) . . ? C13 N2 Yb1 130.9(3) . . ? N1 Yb1 N2 65.27(12) . . ? N1 Yb1 C28 138.02(13) . . ? N2 Yb1 C28 132.16(14) . . ? N1 Yb1 C36 124.25(13) . . ? N2 Yb1 C36 134.33(13) . . ? C28 Yb1 C36 74.32(15) . . ? N1 Yb1 C35 119.08(13) . . ? N2 Yb1 C35 104.36(13) . . ? C28 Yb1 C35 95.12(15) . . ? C36 Yb1 C35 29.99(14) . . ? N1 Yb1 C27 111.48(13) . . ? N2 Yb1 C27 115.70(14) . . ? C28 Yb1 C27 29.83(14) . . ? C36 Yb1 C27 101.96(15) . . ? C35 Yb1 C27 124.94(15) . . ? N1 Yb1 C37 96.93(12) . . ? N2 Yb1 C37 138.48(13) . . ? C28 Yb1 C37 86.78(14) . . ? C36 Yb1 C37 29.71(13) . . ? C35 Yb1 C37 49.88(14) . . ? C27 Yb1 C37 105.65(15) . . ? N1 Yb1 C29 156.62(12) . . ? N2 Yb1 C29 109.08(13) . . ? C28 Yb1 C29 29.72(13) . . ? C36 Yb1 C29 76.72(14) . . ? C35 Yb1 C29 84.20(14) . . ? C27 Yb1 C29 48.64(14) . . ? C37 Yb1 C29 100.58(14) . . ? N1 Yb1 C26 107.58(12) . . ? N2 Yb1 C26 86.91(13) . . ? C28 Yb1 C26 49.61(15) . . ? C36 Yb1 C26 122.53(14) . . ? C35 Yb1 C26 132.58(14) . . ? C27 Yb1 C26 29.80(14) . . ? C37 Yb1 C26 134.57(14) . . ? C29 Yb1 C26 49.08(14) . . ? N1 Yb1 C34 88.99(12) . . ? N2 Yb1 C34 91.35(13) . . ? C28 Yb1 C34 122.54(14) . . ? C36 Yb1 C34 48.90(14) . . ? C35 Yb1 C34 30.11(13) . . ? C27 Yb1 C34 150.82(15) . . ? C37 Yb1 C34 49.33(14) . . ? C29 Yb1 C34 114.20(14) . . ? C26 Yb1 C34 160.71(14) . . ? N1 Yb1 C38 76.28(12) . . ? N2 Yb1 C38 109.07(13) . . ? C28 Yb1 C38 116.65(14) . . ? C36 Yb1 C38 48.76(14) . . ? C35 Yb1 C38 49.44(14) . . ? C27 Yb1 C38 133.54(15) . . ? C37 Yb1 C38 29.98(13) . . ? C29 Yb1 C38 125.48(14) . . ? C26 Yb1 C38 163.33(14) . . ? C34 Yb1 C38 29.50(13) . . ? N1 Yb1 C25 130.15(12) . . ? N2 Yb1 C25 83.58(13) . . ? C28 Yb1 C25 48.95(15) . . ? C36 Yb1 C25 105.47(14) . . ? C35 Yb1 C25 105.34(14) . . ? C27 Yb1 C25 48.17(15) . . ? C37 Yb1 C25 130.26(14) . . ? C29 Yb1 C25 29.72(13) . . ? C26 Yb1 C25 29.13(13) . . ? C34 Yb1 C25 131.59(14) . . ? C38 Yb1 C25 153.28(14) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'YbFu_ccdc_deposit_rinumerato.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-12-16 at 14:48:24 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.reqdat # CIF files read : gg36 gg36_ccdc_deposit gg36 gg36_ox gg36 struct data_YbFu _database_code_depnum_ccdc_archive 'CCDC 795224' #TrackingRef 'YbFu_ccdc_deposit_rinumerato.cif' _audit_creation_date 2010-12-16T14:48:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H38 N2 O1 Yb1' _chemical_formula_sum 'C40 H38 N2 O Yb' _chemical_formula_weight 735.76 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.309(4) _cell_length_b 27.522(11) _cell_length_c 11.346(5) _cell_angle_alpha 90 _cell_angle_beta 96.968(3) _cell_angle_gamma 90 _cell_volume 3195(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6150 _cell_measurement_theta_min 4.1597 _cell_measurement_theta_max 26.4847 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.015 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' _symmetry_Int_Tables_number 9 _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.89528 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.4547 _diffrn_orient_matrix_ub_11 0.0431396645 _diffrn_orient_matrix_ub_12 0.0132428786 _diffrn_orient_matrix_ub_13 -0.0322944849 _diffrn_orient_matrix_ub_21 0.0509158248 _diffrn_orient_matrix_ub_22 -0.0167352653 _diffrn_orient_matrix_ub_23 0.0189230352 _diffrn_orient_matrix_ub_31 -0.0189129797 _diffrn_orient_matrix_ub_32 -0.0146612504 _diffrn_orient_matrix_ub_33 -0.050679039 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_unetI/netI 0.0994 _diffrn_reflns_number 15497 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.2 _diffrn_reflns_theta_max 26.55 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.867 _diffrn_measured_fraction_theta_max 0.867 _reflns_number_total 5381 _reflns_number_gt 4223 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SIR97 (Giacovazzo et al, 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)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5381 _refine_ls_number_parameters 401 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.056 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.013(10) _refine_diff_density_max 0.979 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.104 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 1.1749(9) 0.8075(3) 0.6413(7) 0.032(2) Uani 1 1 d . . . C2 C 1.2935(7) 0.7849(3) 0.6658(7) 0.0285(19) Uani 1 1 d . . . H2 H 1.3088 0.762 0.7286 0.034 Uiso 1 1 calc R . . C3 C 1.3891(7) 0.7963(3) 0.5971(7) 0.037(2) Uani 1 1 d . . . H3 H 1.4716 0.7807 0.6122 0.045 Uiso 1 1 calc R . . C4 C 1.3700(7) 0.8294(3) 0.5080(6) 0.036(2) Uani 1 1 d . . . H4 H 1.4384 0.8386 0.4635 0.043 Uiso 1 1 calc R . . C5 C 1.2434(6) 0.8494(2) 0.4845(6) 0.0204(16) Uani 1 1 d . . . C6 C 1.2112(7) 0.8836(2) 0.3862(6) 0.0233(16) Uani 1 1 d . . . C7 C 1.2825(8) 0.9052(3) 0.3103(7) 0.036(2) Uani 1 1 d . . . H7 H 1.3744 0.9027 0.31 0.043 Uiso 1 1 calc R . . C8 C 1.1946(8) 0.9324(3) 0.2305(8) 0.042(2) Uani 1 1 d . . . H8 H 1.2161 0.9522 0.1671 0.051 Uiso 1 1 calc R . . C9 C 1.0758(8) 0.9248(3) 0.2618(7) 0.035(2) Uani 1 1 d . . . H9 H 0.9975 0.9387 0.2235 0.042 Uiso 1 1 calc R . . C10 C 1.0634(8) 0.7936(3) 0.7028(7) 0.0311(19) Uani 1 1 d . . . H10 H 1.0783 0.7694 0.7627 0.037 Uiso 1 1 calc R . . C11 C 0.8446(7) 0.7856(3) 0.7284(6) 0.0244(18) Uani 1 1 d . . . C12 C 0.8081(8) 0.7401(3) 0.6823(7) 0.0289(19) Uani 1 1 d . . . C13 C 0.7015(13) 0.7175(5) 0.7207(12) 0.033(4) Uani 1 1 d . . . H13 H 0.674 0.6867 0.6893 0.04 Uiso 1 1 calc R . . C14 C 0.6340(8) 0.7396(3) 0.8056(8) 0.038(2) Uani 1 1 d . . . H14 H 0.5608 0.7238 0.832 0.045 Uiso 1 1 calc R . . C15 C 0.6729(13) 0.7840(5) 0.8507(13) 0.038(4) Uani 1 1 d . . . H15 H 0.6267 0.7983 0.9093 0.046 Uiso 1 1 calc R . . C16 C 0.7763(7) 0.8085(3) 0.8141(7) 0.0275(19) Uani 1 1 d . . . C17 C 0.8804(8) 0.7136(3) 0.5914(6) 0.037(2) Uani 1 1 d . . . H17 H 0.932 0.7386 0.553 0.044 Uiso 1 1 calc R . . C18 C 0.7875(9) 0.6903(3) 0.4939(7) 0.053(3) Uani 1 1 d . . . H18A H 0.8335 0.6842 0.4247 0.079 Uiso 1 1 calc R . . H18B H 0.7135 0.7121 0.4715 0.079 Uiso 1 1 calc R . . H18C H 0.7556 0.6595 0.5226 0.079 Uiso 1 1 calc R . . C19 C 0.9759(8) 0.6760(3) 0.6467(8) 0.051(2) Uani 1 1 d . . . H19A H 0.9279 0.6495 0.6796 0.077 Uiso 1 1 calc R . . H19B H 1.0353 0.6911 0.7103 0.077 Uiso 1 1 calc R . . H19C H 1.0265 0.663 0.586 0.077 Uiso 1 1 calc R . . C20 C 0.8214(8) 0.8568(3) 0.8675(7) 0.041(2) Uani 1 1 d . . . H20 H 0.8775 0.8724 0.8123 0.049 Uiso 1 1 calc R . . C21 C 0.9057(12) 0.8487(3) 0.9851(7) 0.077(4) Uani 1 1 d . . . H21A H 0.853 0.8338 1.0417 0.115 Uiso 1 1 calc R . . H21B H 0.9399 0.88 1.0164 0.115 Uiso 1 1 calc R . . H21C H 0.9786 0.8272 0.9731 0.115 Uiso 1 1 calc R . . C22 C 0.7085(10) 0.8913(3) 0.8806(10) 0.080(3) Uani 1 1 d . . . H22A H 0.6529 0.894 0.8044 0.119 Uiso 1 1 calc R . . H22B H 0.7431 0.9234 0.9048 0.119 Uiso 1 1 calc R . . H22C H 0.6568 0.8787 0.9409 0.119 Uiso 1 1 calc R . . C23 C 1.0489(7) 0.9454(3) 0.7076(7) 0.0289(19) Uani 1 1 d . . . C24 C 0.9151(8) 0.9577(2) 0.6835(7) 0.031(2) Uani 1 1 d . . . H24 H 0.8511 0.9516 0.7353 0.038 Uiso 1 1 calc R . . C25 C 0.8906(12) 0.9799(4) 0.5730(10) 0.035(3) Uani 1 1 d . . . H25 H 0.809 0.9924 0.5384 0.042 Uiso 1 1 calc R . . C26 C 1.0071(14) 0.9806(4) 0.5219(10) 0.042(3) Uani 1 1 d . . . H26 H 1.0172 0.9923 0.4447 0.051 Uiso 1 1 calc R . . C27 C 1.1075(8) 0.9610(3) 0.6043(7) 0.032(2) Uani 1 1 d . . . C28 C 1.2474(10) 0.9564(4) 0.6065(11) 0.048(3) Uani 1 1 d . . . H28 H 1.2892 0.9661 0.5402 0.058 Uiso 1 1 calc R . . C29 C 1.3168(9) 0.9381(3) 0.7032(10) 0.048(3) Uani 1 1 d . . . H29 H 1.4087 0.935 0.704 0.057 Uiso 1 1 calc R . . C30 C 1.2608(10) 0.9232(3) 0.8033(9) 0.048(3) Uani 1 1 d . . . H30 H 1.314 0.9101 0.8701 0.058 Uiso 1 1 calc R . . C31 C 1.1278(13) 0.9277(4) 0.8046(13) 0.043(4) Uani 1 1 d . . . H31 H 1.09 0.9183 0.8735 0.052 Uiso 1 1 calc R . . C32 C 0.6676(7) 0.8897(3) 0.4437(7) 0.038(2) Uani 1 1 d . . . C33 C 0.7007(12) 0.8431(5) 0.4848(12) 0.037(4) Uani 1 1 d . . . H33 H 0.6763 0.8295 0.5558 0.044 Uiso 1 1 calc R . . C34 C 0.7713(10) 0.8202(4) 0.4110(9) 0.041(3) Uani 1 1 d . . . H34 H 0.8009 0.7876 0.4197 0.05 Uiso 1 1 calc R . . C35 C 0.7949(7) 0.8510(3) 0.3200(8) 0.046(2) Uani 1 1 d . . . H35 H 0.8473 0.8441 0.2587 0.055 Uiso 1 1 calc R . . C36 C 0.7277(8) 0.8945(3) 0.3343(7) 0.037(2) Uani 1 1 d . . . C37 C 0.7055(13) 0.9380(5) 0.2659(13) 0.061(5) Uani 1 1 d . . . H37 H 0.7445 0.9422 0.1949 0.073 Uiso 1 1 calc R . . C38 C 0.6277(12) 0.9733(4) 0.3037(14) 0.081(4) Uani 1 1 d . . . H38 H 0.6118 1.0017 0.2568 0.097 Uiso 1 1 calc R . . C39 C 0.5701(12) 0.9693(5) 0.4091(16) 0.073(5) Uani 1 1 d . . . H39 H 0.517 0.995 0.4319 0.087 Uiso 1 1 calc R . . C40 C 0.5890(8) 0.9290(4) 0.4797(9) 0.050(3) Uani 1 1 d . . . H40 H 0.5507 0.9269 0.5516 0.059 Uiso 1 1 calc R . . N1 N 1.1481(10) 0.8393(3) 0.5498(8) 0.022(2) Uani 1 1 d . . . N2 N 0.9478(6) 0.8112(2) 0.6830(5) 0.0278(15) Uani 1 1 d . . . O1 O 1.0829(4) 0.89407(17) 0.3571(4) 0.0285(12) Uani 1 1 d . . . Yb1 Yb 0.93489(5) 0.885629(9) 0.52503(5) 0.02625(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(6) 0.041(6) 0.018(5) -0.003(4) 0.002(4) -0.013(5) C2 0.018(5) 0.040(5) 0.028(5) 0.002(4) 0.003(4) 0.007(4) C3 0.022(5) 0.029(5) 0.063(6) 0.008(4) 0.013(4) 0.006(4) C4 0.053(5) 0.030(4) 0.028(5) 0.010(4) 0.020(5) 0.026(4) C5 0.016(4) 0.022(4) 0.024(4) 0.000(3) 0.005(3) 0.000(3) C6 0.024(4) 0.016(4) 0.029(4) -0.009(4) 0.003(3) -0.002(4) C7 0.038(5) 0.036(5) 0.038(5) -0.001(4) 0.024(4) 0.002(4) C8 0.053(6) 0.022(5) 0.057(6) 0.011(4) 0.030(5) 0.002(4) C9 0.045(6) 0.034(5) 0.024(5) 0.009(4) -0.001(4) 0.012(4) C10 0.026(5) 0.038(5) 0.031(5) 0.000(4) 0.009(4) 0.000(4) C11 0.016(4) 0.036(5) 0.022(4) 0.016(4) 0.002(3) 0.003(4) C12 0.029(5) 0.032(5) 0.024(5) 0.004(4) -0.002(4) -0.009(4) C13 0.040(9) 0.025(7) 0.035(8) 0.007(5) 0.007(6) 0.005(6) C14 0.026(5) 0.043(6) 0.046(6) 0.022(5) 0.009(4) 0.002(5) C15 0.029(8) 0.051(9) 0.034(7) 0.019(6) 0.001(6) 0.007(6) C16 0.016(4) 0.039(5) 0.028(5) 0.006(4) 0.006(4) 0.000(4) C17 0.049(6) 0.039(5) 0.023(5) 0.002(4) 0.009(4) -0.005(4) C18 0.075(7) 0.041(5) 0.044(6) -0.002(5) 0.018(5) -0.029(5) C19 0.062(6) 0.036(5) 0.061(6) 0.004(5) 0.028(5) 0.008(5) C20 0.044(5) 0.045(5) 0.039(6) 0.001(4) 0.027(4) -0.006(4) C21 0.132(12) 0.075(7) 0.026(6) -0.013(5) 0.023(7) -0.031(8) C22 0.076(8) 0.048(6) 0.128(10) -0.010(7) 0.064(7) 0.002(6) C23 0.025(5) 0.025(4) 0.035(5) -0.005(4) -0.004(4) -0.007(4) C24 0.039(5) 0.020(4) 0.037(5) -0.011(4) 0.012(4) -0.002(4) C25 0.045(7) 0.026(6) 0.034(7) -0.001(5) 0.008(6) 0.010(5) C26 0.085(9) 0.016(5) 0.027(7) -0.006(5) 0.008(7) -0.003(6) C27 0.040(5) 0.016(4) 0.041(6) -0.015(4) 0.009(4) -0.009(4) C28 0.032(8) 0.042(7) 0.072(9) -0.031(6) 0.015(6) -0.016(6) C29 0.032(6) 0.043(6) 0.068(8) -0.030(6) 0.003(6) -0.001(5) C30 0.047(7) 0.038(6) 0.054(7) -0.016(5) -0.021(6) 0.004(5) C31 0.047(8) 0.025(6) 0.056(8) -0.010(5) -0.001(6) 0.007(5) C32 0.025(4) 0.031(5) 0.057(6) -0.008(5) 0.001(4) -0.012(4) C33 0.016(6) 0.057(9) 0.037(8) 0.037(6) 0.000(6) -0.003(6) C34 0.038(7) 0.039(6) 0.045(7) -0.003(5) -0.002(6) 0.004(5) C35 0.025(5) 0.073(7) 0.038(6) -0.022(5) 0.002(4) -0.002(5) C36 0.027(5) 0.048(6) 0.033(5) 0.011(4) -0.011(4) -0.002(4) C37 0.041(9) 0.081(12) 0.054(9) 0.043(8) -0.023(7) -0.022(8) C38 0.037(7) 0.053(8) 0.143(13) 0.046(8) -0.032(8) -0.009(6) C39 0.020(7) 0.050(9) 0.144(15) -0.018(9) -0.008(8) 0.003(6) C40 0.020(5) 0.058(7) 0.071(8) -0.006(6) 0.008(5) 0.006(5) N1 0.028(5) 0.018(5) 0.018(5) 0.005(4) -0.003(4) 0.002(4) N2 0.034(4) 0.031(4) 0.020(4) 0.000(3) 0.010(3) 0.001(3) O1 0.029(3) 0.037(3) 0.021(3) 0.001(2) 0.012(2) 0.005(3) Yb1 0.02383(15) 0.02602(14) 0.02933(16) -0.0021(4) 0.00496(10) 0.0001(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 C1 N1 1.360(12) . ? C1 C2 1.370(11) . ? C1 C10 1.466(12) . ? C2 C3 1.365(10) . ? C2 H2 0.95 . ? C3 C4 1.356(10) . ? C3 H3 0.95 . ? C4 C5 1.412(9) . ? C4 H4 0.95 . ? C5 N1 1.329(12) . ? C5 C6 1.467(9) . ? C6 C7 1.337(10) . ? C6 O1 1.354(8) . ? C7 C8 1.416(11) . ? C7 H7 0.95 . ? C8 C9 1.332(10) . ? C8 H8 0.95 . ? C9 O1 1.367(8) . ? C9 H9 0.95 . ? C10 N2 1.281(9) . ? C10 H10 0.95 . ? C11 C12 1.390(10) . ? C11 C16 1.416(10) . ? C11 N2 1.424(8) . ? C12 C13 1.378(15) . ? C12 C17 1.528(10) . ? C13 C14 1.395(16) . ? C13 H13 0.95 . ? C14 C15 1.366(16) . ? C14 H14 0.95 . ? C15 C16 1.367(15) . ? C15 H15 0.95 . ? C16 C20 1.510(10) . ? C17 C19 1.513(10) . ? C17 C18 1.515(10) . ? C17 H17 1 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C21 1.518(10) . ? C20 C22 1.524(11) . ? C20 H20 1 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C31 1.377(15) . ? C23 C24 1.414(10) . ? C23 C27 1.447(11) . ? C23 Yb1 2.791(7) . ? C24 C25 1.390(13) . ? C24 Yb1 2.701(7) . ? C24 H24 0.95 . ? C25 C26 1.395(10) . ? C25 Yb1 2.701(12) . ? C25 H25 0.95 . ? C26 C27 1.415(14) . ? C26 Yb1 2.719(12) . ? C26 H26 0.95 . ? C27 C28 1.444(13) . ? C27 Yb1 2.810(7) . ? C28 C29 1.333(14) . ? C28 H28 0.95 . ? C29 C30 1.397(13) . ? C29 H29 0.95 . ? C30 C31 1.379(16) . ? C30 H30 0.95 . ? C31 H31 0.95 . ? C32 C33 1.393(14) . ? C32 C40 1.440(11) . ? C32 C36 1.459(11) . ? C32 Yb1 2.800(7) . ? C33 C34 1.332(17) . ? C33 Yb1 2.672(12) . ? C33 H33 0.95 . ? C34 C35 1.381(12) . ? C34 Yb1 2.689(9) . ? C34 H34 0.95 . ? C35 C36 1.401(10) . ? C35 Yb1 2.754(8) . ? C35 H35 0.95 . ? C36 C37 1.430(15) . ? C36 Yb1 2.860(7) . ? C37 C38 1.362(18) . ? C37 H37 0.95 . ? C38 C39 1.403(18) . ? C38 H38 0.95 . ? C39 C40 1.368(15) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? N1 Yb1 2.527(10) . ? N2 Yb1 2.714(6) . ? O1 Yb1 2.592(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.7(9) . . ? N1 C1 C10 115.7(9) . . ? C2 C1 C10 121.1(8) . . ? C3 C2 C1 117.9(7) . . ? C3 C2 H2 121 . . ? C1 C2 H2 121 . . ? C4 C3 C2 122.0(7) . . ? C4 C3 H3 119 . . ? C2 C3 H3 119 . . ? C3 C4 C5 116.7(7) . . ? C3 C4 H4 121.6 . . ? C5 C4 H4 121.6 . . ? N1 C5 C4 122.8(7) . . ? N1 C5 C6 116.3(7) . . ? C4 C5 C6 120.9(6) . . ? C7 C6 O1 110.2(6) . . ? C7 C6 C5 133.1(7) . . ? O1 C6 C5 116.5(6) . . ? C6 C7 C8 106.7(7) . . ? C6 C7 H7 126.6 . . ? C8 C7 H7 126.6 . . ? C9 C8 C7 106.5(7) . . ? C9 C8 H8 126.8 . . ? C7 C8 H8 126.8 . . ? C8 C9 O1 110.2(7) . . ? C8 C9 H9 124.9 . . ? O1 C9 H9 124.9 . . ? N2 C10 C1 125.7(8) . . ? N2 C10 H10 117.1 . . ? C1 C10 H10 117.1 . . ? C12 C11 C16 121.6(7) . . ? C12 C11 N2 119.3(7) . . ? C16 C11 N2 118.9(7) . . ? C13 C12 C11 118.5(9) . . ? C13 C12 C17 118.1(9) . . ? C11 C12 C17 123.4(7) . . ? C12 C13 C14 120.3(11) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.0(12) . . ? C15 C14 H14 120 . . ? C13 C14 H14 120 . . ? C14 C15 C16 122.1(13) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C11 117.4(9) . . ? C15 C16 C20 121.6(10) . . ? C11 C16 C20 120.9(7) . . ? C19 C17 C18 109.5(7) . . ? C19 C17 C12 113.1(6) . . ? C18 C17 C12 112.2(7) . . ? C19 C17 H17 107.2 . . ? C18 C17 H17 107.2 . . ? C12 C17 H17 107.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 C21 109.9(7) . . ? C16 C20 C22 112.7(7) . . ? C21 C20 C22 111.6(8) . . ? C16 C20 H20 107.4 . . ? C21 C20 H20 107.4 . . ? C22 C20 H20 107.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 C23 C24 135.0(9) . . ? C31 C23 C27 119.2(9) . . ? C24 C23 C27 105.5(7) . . ? C31 C23 Yb1 122.6(6) . . ? C24 C23 Yb1 71.6(4) . . ? C27 C23 Yb1 75.7(4) . . ? C25 C24 C23 110.2(8) . . ? C25 C24 Yb1 75.1(6) . . ? C23 C24 Yb1 78.7(4) . . ? C25 C24 H24 124.9 . . ? C23 C24 H24 124.9 . . ? Yb1 C24 H24 113.3 . . ? C24 C25 C26 108.1(10) . . ? C24 C25 Yb1 75.1(6) . . ? C26 C25 Yb1 75.8(9) . . ? C24 C25 H25 126 . . ? C26 C25 H25 126 . . ? Yb1 C25 H25 115.4 . . ? C25 C26 C27 108.5(11) . . ? C25 C26 Yb1 74.4(9) . . ? C27 C26 Yb1 78.8(6) . . ? C25 C26 H26 125.7 . . ? C27 C26 H26 125.7 . . ? Yb1 C26 H26 113.4 . . ? C26 C27 C28 134.0(10) . . ? C26 C27 C23 107.7(9) . . ? C28 C27 C23 118.3(8) . . ? C26 C27 Yb1 71.7(6) . . ? C28 C27 Yb1 122.1(6) . . ? C23 C27 Yb1 74.3(4) . . ? C29 C28 C27 118.9(10) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 123.1(10) . . ? C28 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C31 C30 C29 119.5(10) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C23 C31 C30 121.0(12) . . ? C23 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C40 136.1(10) . . ? C33 C32 C36 104.8(8) . . ? C40 C32 C36 119.0(8) . . ? C33 C32 Yb1 70.2(6) . . ? C40 C32 Yb1 120.1(5) . . ? C36 C32 Yb1 77.3(4) . . ? C34 C33 C32 110.8(11) . . ? C34 C33 Yb1 76.3(7) . . ? C32 C33 Yb1 80.4(6) . . ? C34 C33 H33 124.6 . . ? C32 C33 H33 124.6 . . ? Yb1 C33 H33 110.8 . . ? C33 C34 C35 109.8(10) . . ? C33 C34 Yb1 74.9(7) . . ? C35 C34 Yb1 77.9(5) . . ? C33 C34 H34 125.1 . . ? C35 C34 H34 125.1 . . ? Yb1 C34 H34 114.1 . . ? C34 C35 C36 107.6(8) . . ? C34 C35 Yb1 72.7(5) . . ? C36 C35 Yb1 79.8(5) . . ? C34 C35 H35 126.2 . . ? C36 C35 H35 126.2 . . ? Yb1 C35 H35 113.7 . . ? C35 C36 C37 134.4(10) . . ? C35 C36 C32 106.8(7) . . ? C37 C36 C32 118.7(9) . . ? C35 C36 Yb1 71.4(4) . . ? C37 C36 Yb1 122.5(7) . . ? C32 C36 Yb1 72.8(4) . . ? C38 C37 C36 119.2(12) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 122.6(11) . . ? C37 C38 H38 118.7 . . ? C39 C38 H38 118.7 . . ? C40 C39 C38 121.2(12) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C32 119.2(11) . . ? C39 C40 H40 120.4 . . ? C32 C40 H40 120.4 . . ? C5 N1 C1 117.7(9) . . ? C5 N1 Yb1 121.6(6) . . ? C1 N1 Yb1 120.2(7) . . ? C10 N2 C11 118.0(6) . . ? C10 N2 Yb1 111.8(5) . . ? C11 N2 Yb1 129.4(4) . . ? C6 O1 C9 106.4(6) . . ? C6 O1 Yb1 116.5(4) . . ? C9 O1 Yb1 131.0(4) . . ? N1 Yb1 O1 62.9(2) . . ? N1 Yb1 C33 123.6(2) . . ? O1 Yb1 C33 120.9(3) . . ? N1 Yb1 C34 101.6(3) . . ? O1 Yb1 C34 95.6(3) . . ? C33 Yb1 C34 28.8(4) . . ? N1 Yb1 C24 115.6(3) . . ? O1 Yb1 C24 121.5(2) . . ? C33 Yb1 C24 107.2(4) . . ? C34 Yb1 C24 135.9(3) . . ? N1 Yb1 C25 128.9(3) . . ? O1 Yb1 C25 101.0(3) . . ? C33 Yb1 C25 106.5(4) . . ? C34 Yb1 C25 129.0(3) . . ? C24 Yb1 C25 29.8(3) . . ? N1 Yb1 N2 64.8(2) . . ? O1 Yb1 N2 124.54(17) . . ? C33 Yb1 N2 75.7(3) . . ? C34 Yb1 N2 77.9(2) . . ? C24 Yb1 N2 96.7(2) . . ? C25 Yb1 N2 126.0(3) . . ? N1 Yb1 C26 104.5(4) . . ? O1 Yb1 C26 73.6(3) . . ? C33 Yb1 C26 131.5(4) . . ? C34 Yb1 C26 142.6(3) . . ? C24 Yb1 C26 49.2(3) . . ? C25 Yb1 C26 29.8(2) . . ? N2 Yb1 C26 137.9(3) . . ? N1 Yb1 C35 106.2(3) . . ? O1 Yb1 C35 72.8(2) . . ? C33 Yb1 C35 48.3(4) . . ? C34 Yb1 C35 29.4(3) . . ? C24 Yb1 C35 137.9(2) . . ? C25 Yb1 C35 114.7(3) . . ? N2 Yb1 C35 106.0(2) . . ? C26 Yb1 C35 115.9(3) . . ? N1 Yb1 C23 86.2(3) . . ? O1 Yb1 C23 105.1(2) . . ? C33 Yb1 C23 132.5(4) . . ? C34 Yb1 C23 159.2(3) . . ? C24 Yb1 C23 29.8(2) . . ? C25 Yb1 C23 49.5(3) . . ? N2 Yb1 C23 88.4(2) . . ? C26 Yb1 C23 49.6(3) . . ? C35 Yb1 C23 163.9(2) . . ? N1 Yb1 C32 149.8(3) . . ? O1 Yb1 C32 113.4(2) . . ? C33 Yb1 C32 29.4(3) . . ? C34 Yb1 C32 48.2(3) . . ? C24 Yb1 C32 92.2(2) . . ? C25 Yb1 C32 81.1(3) . . ? N2 Yb1 C32 102.4(2) . . ? C26 Yb1 C32 102.6(3) . . ? C35 Yb1 C32 48.8(2) . . ? C23 Yb1 C32 122.0(2) . . ? N1 Yb1 C27 80.1(3) . . ? O1 Yb1 C27 76.3(2) . . ? C33 Yb1 C27 154.5(4) . . ? C34 Yb1 C27 169.9(3) . . ? C24 Yb1 C27 48.8(2) . . ? C25 Yb1 C27 48.8(3) . . ? N2 Yb1 C27 111.6(2) . . ? C26 Yb1 C27 29.6(3) . . ? C35 Yb1 C27 140.6(3) . . ? C23 Yb1 C27 29.9(2) . . ? C32 Yb1 C27 129.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C5 C6 O1 -12.6(9) . . . . ?