Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _audit_creation_method Xtal3.6 _audit_creation_date 00-07-02 _audit_update_record ? _journal_coden_Cambridge 222 loop_ _publ_author_name 'Glen Deacon' 'Craig M. Forsyth' 'Alex Gitlits' 'Brian W. Skelton' 'Allan H. White' _publ_contact_author_name 'Prof Glen Deacon' _publ_contact_author_address ; School of Chemistry Monash University Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email GLEN.DEACON@SCI.MONASH.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Reactions of lanthanoid metals with 3,5-diphenylpyrazole at elevated temperatures - synthesis and structures of hompleptic [Ln3(Ph2pz)9] (Ln = La, Nd), [Ln2(Ph2pz)6] (Ln = Er, Lu), and heteroleptic [Ln(Ph2pz)3(Ph2pzH)2] (Ln = La, Nd, Gd, Tb, Er, or Yb) pyrazolate complexes. ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Pogram for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; data_ag3752 _database_code_depnum_ccdc_archive 'CCDC 190713' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C135 H99 La3 N18' _chemical_formula_moiety ? _chemical_formula_weight 2390.12 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 19.2630(10) _cell_length_b 20.1150(10) _cell_length_c 28.656(2) _cell_angle_alpha 90.00000 _cell_angle_beta 100.1320(10) _cell_angle_gamma 90.00000 _cell_volume 10930.3(11) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 23.6 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.214 _exptl_crystal_description plate _exptl_crystal_size_max .3 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .72 _exptl_absorpt_correction_T_max .84 _diffrn_reflns_number 57235 _reflns_number_total 26637 _reflns_Friedel_coverage 0 _reflns_number_gt 20146 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.16 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .027 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_ref .041 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_number_reflns 20146 _refine_ls_number_parameters 1406 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .035 _refine_diff_density_min -.59 _refine_diff_density_max 1.04 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 540 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 396 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 72 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' La ? 0 12 -.588 2.452 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group La1 .841398(10) .820545(9) .244065(7) .02487(9) Uani ? ? 1.00000 ? ? La2 .987434(10) .715009(9) .187189(7) .02531(9) Uani ? ? 1.00000 ? ? La3 1.152796(10) .596682(9) .237743(7) .02344(9) Uani ? ? 1.00000 ? ? N11 .72706(14) .83593(13) .26740(10) .0281(13) Uani ? ? 1.00000 ? ? N12 .70987(14) .83122(13) .21894(10) .0285(14) Uani ? ? 1.00000 ? ? C13 .63883(17) .83145(16) .20755(12) .0291(16) Uani ? ? 1.00000 ? ? C131 .60078(19) .82339(17) .15827(13) .0345(18) Uani ? ? 1.00000 ? ? C132 .6249(2) .85242(19) .12005(13) .040(2) Uani ? ? 1.00000 ? ? C133 .5884(2) .8436(2) .07411(14) .051(2) Uani ? ? 1.00000 ? ? C134 .5267(2) .8072(2) .06577(15) .054(2) Uani ? ? 1.00000 ? ? C135 .5013(2) .7789(2) .10354(16) .052(2) Uani ? ? 1.00000 ? ? C136 .5381(2) .78649(18) .14941(14) .042(2) Uani ? ? 1.00000 ? ? C14 .61002(18) .83722(16) .24887(13) .0319(17) Uani ? ? 1.00000 ? ? C15 .66706(17) .83973(15) .28568(12) .0284(16) Uani ? ? 1.00000 ? ? C151 .6705(2) .84411(17) .33699(12) .0357(18) Uani ? ? 1.00000 ? ? C152 .7340(2) .8589(2) .36641(14) .054(2) Uani ? ? 1.00000 ? ? C153 .7388(3) .8598(3) .41477(16) .078(3) Uani ? ? 1.00000 ? ? C154 .6801(3) .8456(3) .43493(16) .080(4) Uani ? ? 1.00000 ? ? C155 .6158(3) .8333(3) .40584(16) .065(3) Uani ? ? 1.00000 ? ? C156 .6109(2) .8326(2) .35750(14) .045(2) Uani ? ? 1.00000 ? ? N21 .89353(15) .89743(14) .30831(10) .0327(14) Uani ? ? 1.00000 ? ? N22 .87852(14) .93451(13) .26751(10) .0303(14) Uani ? ? 1.00000 ? ? C23 .90456(17) .99629(16) .27655(13) .0346(18) Uani ? ? 1.00000 ? ? C231 .89569(17) 1.04856(16) .23975(14) .0352(18) Uani ? ? 1.00000 ? ? C232 .86617(19) 1.03378(17) .19314(14) .039(2) Uani ? ? 1.00000 ? ? C233 .8566(2) 1.0819(2) .15833(15) .046(2) Uani ? ? 1.00000 ? ? C234 .8758(2) 1.14723(19) .16994(16) .050(2) Uani ? ? 1.00000 ? ? C235 .9045(2) 1.16321(18) .21593(17) .052(2) Uani ? ? 1.00000 ? ? C236 .9149(2) 1.11470(18) .25051(15) .043(2) Uani ? ? 1.00000 ? ? C24 .9366(2) .99912(18) .32442(14) .041(2) Uani ? ? 1.00000 ? ? C25 .92871(19) .93625(18) .34286(13) .0376(19) Uani ? ? 1.00000 ? ? C251 .9531(2) .9106(2) .39123(14) .044(2) Uani ? ? 1.00000 ? ? C252 .9288(2) .8508(2) .40619(15) .051(2) Uani ? ? 1.00000 ? ? C253 .9503(2) .8274(3) .45209(16) .062(3) Uani ? ? 1.00000 ? ? C254 .9975(2) .8631(3) .48386(15) .064(3) Uani ? ? 1.00000 ? ? C255 1.0230(3) .9216(3) .46933(18) .086(4) Uani ? ? 1.00000 ? ? C256 1.0019(3) .9458(3) .42352(18) .071(3) Uani ? ? 1.00000 ? ? N31 .91208(15) .84170(13) .17738(10) .0306(14) Uani ? ? 1.00000 ? ? N32 .96600(14) .83552(13) .21709(10) .0294(14) Uani ? ? 1.00000 ? ? C332 1.07827(19) .88612(18) .29520(14) .039(2) Uani ? ? 1.00000 ? ? C333 1.1381(2) .8981(2) .32950(15) .047(2) Uani ? ? 1.00000 ? ? C334 1.2019(2) .91054(19) .31555(16) .050(2) Uani ? ? 1.00000 ? ? C335 1.20640(19) .91267(18) .26806(16) .046(2) Uani ? ? 1.00000 ? ? C336 1.14719(19) .90096(17) .23363(15) .040(2) Uani ? ? 1.00000 ? ? C34 1.00024(18) .91043(16) .16800(13) .0341(18) Uani ? ? 1.00000 ? ? C35 .93376(18) .88699(16) .14833(12) .0318(17) Uani ? ? 1.00000 ? ? C351 .8877(2) .90965(17) .10457(13) .0368(18) Uani ? ? 1.00000 ? ? C352 .8154(2) .8998(2) .09780(15) .052(2) Uani ? ? 1.00000 ? ? C353 .7726(2) .9254(3) .05841(16) .066(3) Uani ? ? 1.00000 ? ? C354 .8014(3) .9619(2) .02588(15) .062(3) Uani ? ? 1.00000 ? ? C355 .8730(2) .9712(2) .03199(15) .056(3) Uani ? ? 1.00000 ? ? C356 .9162(2) .9453(2) .07101(14) .046(2) Uani ? ? 1.00000 ? ? C33 1.01866(17) .87815(15) .21097(12) .0299(16) Uani ? ? 1.00000 ? ? C331 1.08252(18) .88768(15) .24750(13) .0325(17) Uani ? ? 1.00000 ? ? N41 .86840(14) .69858(13) .21093(10) .0308(14) Uani ? ? 1.00000 ? ? N42 .90235(14) .69858(13) .25764(11) .0332(14) Uani ? ? 1.00000 ? ? C43 .85266(18) .68372(16) .28471(13) .0322(17) Uani ? ? 1.00000 ? ? C431 .8691(2) .67705(18) .33675(14) .042(2) Uani ? ? 1.00000 ? ? C432 .9368(2) .6585(2) .35946(17) .058(3) Uani ? ? 1.00000 ? ? C433 .9487(3) .6455(3) .40785(19) .080(3) Uani ? ? 1.00000 ? ? C434 .8948(3) .6514(3) .43333(19) .097(4) Uani ? ? 1.00000 ? ? C435 .8295(3) .6713(4) .41164(18) .098(4) Uani ? ? 1.00000 ? ? C436 .8161(2) .6854(3) .36337(16) .067(3) Uani ? ? 1.00000 ? ? C44 .78661(18) .67597(16) .25558(13) .0326(17) Uani ? ? 1.00000 ? ? C45 .79891(17) .68451(15) .20928(12) .0290(16) Uani ? ? 1.00000 ? ? C451 .75006(19) .68379(16) .16376(13) .0339(17) Uani ? ? 1.00000 ? ? C452 .7630(2) .72324(17) .12641(13) .0380(19) Uani ? ? 1.00000 ? ? C453 .7176(2) .7241(2) .08365(14) .048(2) Uani ? ? 1.00000 ? ? C454 .6583(2) .6838(2) .07732(15) .053(2) Uani ? ? 1.00000 ? ? C455 .6450(2) .6437(2) .11401(16) .054(2) Uani ? ? 1.00000 ? ? C456 .6900(2) .6433(2) .15748(14) .044(2) Uani ? ? 1.00000 ? ? N51 .93465(17) .69840(16) .10315(11) .0431(17) Uani ? ? 1.00000 ? ? N52 .99107(17) .74124(15) .10356(10) .0412(17) Uani ? ? 1.00000 ? ? C53 .9944(2) .7568(2) .05804(14) .052(2) Uani ? ? 1.00000 ? ? C531 1.0512(3) .7991(2) .04646(15) .062(3) Uani ? ? 1.00000 ? ? C532 1.0899(3) .8402(2) .0798(2) .072(3) Uani ? ? 1.00000 ? ? C533 1.1454(3) .8789(3) .0696(2) .099(4) Uani ? ? 1.00000 ? ? C534 1.1639(4) .8748(3) .0248(3) .116(5) Uani ? ? 1.00000 ? ? C535 1.1248(4) .8342(4) -.0086(2) .120(5) Uani ? ? 1.00000 ? ? C536 1.0687(3) .7975(3) .00099(18) .092(4) Uani ? ? 1.00000 ? ? C54 .9404(3) .7236(2) .02833(14) .062(3) Uani ? ? 1.00000 ? ? C55 .9043(2) .6878(2) .05743(14) .051(2) Uani ? ? 1.00000 ? ? C551 .8433(2) .6407(2) .04605(15) .058(2) Uani ? ? 1.00000 ? ? C552 .8279(2) .5959(2) .07844(17) .062(3) Uani ? ? 1.00000 ? ? C553 .7703(3) .5525(2) .0674(2) .073(3) Uani ? ? 1.00000 ? ? C554 .7285(3) .5567(3) .0231(2) .094(4) Uani ? ? 1.00000 ? ? C555 .7433(3) .6003(3) -.00972(19) .087(4) Uani ? ? 1.00000 ? ? C556 .7997(3) .6440(3) .00072(17) .079(3) Uani ? ? 1.00000 ? ? N61 1.01085(14) .58971(13) .20688(10) .0306(14) Uani ? ? 1.00000 ? ? N62 1.04754(15) .59164(13) .16855(10) .0313(14) Uani ? ? 1.00000 ? ? C63 1.01882(18) .54490(16) .13720(12) .0337(17) Uani ? ? 1.00000 ? ? C631 1.04536(19) .53516(18) .09249(13) .0389(19) Uani ? ? 1.00000 ? ? C632 1.0687(2) .5893(2) .06949(14) .047(2) Uani ? ? 1.00000 ? ? C633 1.0951(2) .5799(3) .02798(16) .062(3) Uani ? ? 1.00000 ? ? C634 1.0990(2) .5160(3) .00966(16) .068(3) Uani ? ? 1.00000 ? ? C635 1.0745(2) .4629(2) .03134(16) .062(3) Uani ? ? 1.00000 ? ? C636 1.0473(2) .4718(2) .07266(14) .051(2) Uani ? ? 1.00000 ? ? C64 .96440(18) .51274(17) .15389(14) .0380(18) Uani ? ? 1.00000 ? ? C65 .96040(17) .54204(16) .19704(13) .0335(17) Uani ? ? 1.00000 ? ? C651 .91056(18) .52811(16) .22938(15) .040(2) Uani ? ? 1.00000 ? ? C652 .9317(2) .52861(18) .27796(15) .045(2) Uani ? ? 1.00000 ? ? C653 .8847(2) .5134(2) .30784(17) .055(2) Uani ? ? 1.00000 ? ? C654 .8150(2) .4987(2) .2889(2) .064(3) Uani ? ? 1.00000 ? ? C655 .7932(2) .4984(2) .2408(2) .061(3) Uani ? ? 1.00000 ? ? C656 .8407(2) .51254(18) .21027(17) .049(2) Uani ? ? 1.00000 ? ? N71 1.10341(14) .72019(13) .25342(10) .0286(13) Uani ? ? 1.00000 ? ? N72 1.12018(14) .72585(12) .20823(9) .0269(13) Uani ? ? 1.00000 ? ? C73 1.19098(17) .73712(15) .21297(12) .0289(16) Uani ? ? 1.00000 ? ? C731 1.22281(18) .74537(16) .17012(12) .0319(17) Uani ? ? 1.00000 ? ? C732 1.1963(2) .71180(18) .12874(13) .041(2) Uani ? ? 1.00000 ? ? C733 1.2261(2) .7188(2) .08860(14) .047(2) Uani ? ? 1.00000 ? ? C734 1.2826(2) .7596(2) .08873(14) .051(2) Uani ? ? 1.00000 ? ? C735 1.3087(2) .7951(3) .12875(17) .066(3) Uani ? ? 1.00000 ? ? C736 1.2796(2) .7881(2) .16984(14) .052(2) Uani ? ? 1.00000 ? ? C74 1.22033(17) .73810(16) .26056(12) .0313(17) Uani ? ? 1.00000 ? ? C75 1.16424(17) .72822(15) .28523(12) .0283(16) Uani ? ? 1.00000 ? ? C751 1.16499(19) .72741(16) .33678(12) .0332(17) Uani ? ? 1.00000 ? ? C752 1.1043(2) .7402(2) .35492(13) .043(2) Uani ? ? 1.00000 ? ? C753 1.1067(3) .7444(2) .40341(15) .057(3) Uani ? ? 1.00000 ? ? C754 1.1698(3) .7349(2) .43388(15) .064(3) Uani ? ? 1.00000 ? ? C755 1.2295(3) .7204(3) .41642(15) .063(3) Uani ? ? 1.00000 ? ? C756 1.2284(2) .7169(2) .36798(14) .048(2) Uani ? ? 1.00000 ? ? N81 1.28002(14) .57885(13) .26180(9) .0275(13) Uani ? ? 1.00000 ? ? N82 1.26772(14) .58056(13) .21288(9) .0272(13) Uani ? ? 1.00000 ? ? C83 1.33110(17) .57953(15) .19850(12) .0285(16) Uani ? ? 1.00000 ? ? C831 1.33776(18) .58219(16) .14817(12) .0315(17) Uani ? ? 1.00000 ? ? C832 1.2839(2) .56032(18) .11276(13) .0376(19) Uani ? ? 1.00000 ? ? C833 1.2911(2) .5633(2) .06534(13) .045(2) Uani ? ? 1.00000 ? ? C834 1.3530(2) .5885(2) .05307(13) .046(2) Uani ? ? 1.00000 ? ? C835 1.4064(2) .6111(2) .08785(14) .044(2) Uani ? ? 1.00000 ? ? C836 1.3984(2) .60815(19) .13521(13) .038(2) Uani ? ? 1.00000 ? ? C84 1.38464(17) .57659(16) .23839(12) .0309(17) Uani ? ? 1.00000 ? ? C85 1.35008(17) .57636(16) .27768(12) .0291(16) Uani ? ? 1.00000 ? ? C851 1.37856(18) .57611(16) .32812(12) .0305(16) Uani ? ? 1.00000 ? ? C852 1.3346(2) .5699(2) .36154(14) .049(2) Uani ? ? 1.00000 ? ? C853 1.3611(2) .5749(3) .40953(15) .069(3) Uani ? ? 1.00000 ? ? C854 1.4321(2) .5855(2) .42487(14) .054(2) Uani ? ? 1.00000 ? ? C855 1.4768(2) .5900(2) .39252(13) .043(2) Uani ? ? 1.00000 ? ? C856 1.45037(18) .58512(17) .34462(13) .0336(17) Uani ? ? 1.00000 ? ? N91 1.12563(14) .51476(13) .29592(9) .0293(14) Uani ? ? 1.00000 ? ? N92 1.12345(14) .48067(13) .25378(10) .0291(14) Uani ? ? 1.00000 ? ? C93 1.09781(17) .41887(15) .25927(12) .0286(16) Uani ? ? 1.00000 ? ? C931 1.09289(17) .36777(16) .22172(12) .0283(16) Uani ? ? 1.00000 ? ? C932 1.1078(2) .38153(17) .17701(13) .0370(18) Uani ? ? 1.00000 ? ? C933 1.1053(2) .3317(2) .14347(13) .043(2) Uani ? ? 1.00000 ? ? C934 1.0879(2) .26727(18) .15318(14) .043(2) Uani ? ? 1.00000 ? ? C935 1.0731(2) .25271(17) .19761(14) .040(2) Uani ? ? 1.00000 ? ? C936 1.07599(19) .30184(17) .23140(13) .0364(18) Uani ? ? 1.00000 ? ? C94 1.08181(19) .41333(16) .30469(12) .0332(17) Uani ? ? 1.00000 ? ? C95 1.10066(17) .47453(17) .32685(12) .0305(16) Uani ? ? 1.00000 ? ? C951 1.09750(18) .49408(17) .37594(12) .0336(17) Uani ? ? 1.00000 ? ? C952 1.1354(2) .54676(19) .39765(13) .040(2) Uani ? ? 1.00000 ? ? C953 1.1345(2) .5612(2) .44499(14) .048(2) Uani ? ? 1.00000 ? ? C954 1.0947(2) .5239(2) .47091(14) .053(2) Uani ? ? 1.00000 ? ? C955 1.0546(2) .4727(2) .44860(14) .054(2) Uani ? ? 1.00000 ? ? C956 1.0553(2) .4575(2) .40170(13) .047(2) Uani ? ? 1.00000 ? ? H132 .66746 .87868 .12567 .05100 Uiso ? ? 1.00000 ? ? H133 .60581 .86357 .04754 .06400 Uiso ? ? 1.00000 ? ? H134 .50106 .80117 .03385 .06600 Uiso ? ? 1.00000 ? ? H135 .45803 .75367 .09791 .06400 Uiso ? ? 1.00000 ? ? H136 .52059 .76543 .17565 .05300 Uiso ? ? 1.00000 ? ? H14 .56092 .83953 .25115 .04100 Uiso ? ? 1.00000 ? ? H152 .77535 .86909 .35248 .06800 Uiso ? ? 1.00000 ? ? H153 .78381 .86984 .43516 .09800 Uiso ? ? 1.00000 ? ? H154 .68345 .84340 .46916 .09900 Uiso ? ? 1.00000 ? ? H155 .57467 .82446 .42000 .08100 Uiso ? ? 1.00000 ? ? H156 .56558 .82524 .33718 .05700 Uiso ? ? 1.00000 ? ? H232 .85266 .98868 .18518 .04700 Uiso ? ? 1.00000 ? ? H233 .83668 1.07013 .12602 .06100 Uiso ? ? 1.00000 ? ? H234 .86764 1.18158 .14572 .06200 Uiso ? ? 1.00000 ? ? H235 .91786 1.20860 .22397 .06600 Uiso ? ? 1.00000 ? ? H236 .93576 1.12602 .28299 .05500 Uiso ? ? 1.00000 ? ? H24 .95979 1.03684 .34118 .05200 Uiso ? ? 1.00000 ? ? H252 .89562 .82478 .38416 .06300 Uiso ? ? 1.00000 ? ? H253 .93167 .78555 .46177 .08000 Uiso ? ? 1.00000 ? ? H254 1.01247 .84638 .51571 .08000 Uiso ? ? 1.00000 ? ? H255 1.05616 .94722 .49180 .10400 Uiso ? ? 1.00000 ? ? H256 1.02145 .98732 .41351 .08900 Uiso ? ? 1.00000 ? ? H332 1.03374 .87698 .30470 .04900 Uiso ? ? 1.00000 ? ? H333 1.13447 .89730 .36322 .05900 Uiso ? ? 1.00000 ? ? H334 1.24353 .91734 .33955 .06400 Uiso ? ? 1.00000 ? ? H335 1.25106 .92201 .25885 .05800 Uiso ? ? 1.00000 ? ? H336 1.15026 .90257 .19999 .05100 Uiso ? ? 1.00000 ? ? H34 1.02776 .94246 .15441 .04200 Uiso ? ? 1.00000 ? ? H352 .79477 .87451 .12022 .06200 Uiso ? ? 1.00000 ? ? H353 .72233 .91824 .05388 .07800 Uiso ? ? 1.00000 ? ? H354 .77138 .98069 -.00156 .07700 Uiso ? ? 1.00000 ? ? H355 .89300 .99653 .00892 .06500 Uiso ? ? 1.00000 ? ? H356 .96653 .95191 .07521 .05900 Uiso ? ? 1.00000 ? ? H432 .97437 .65449 .34127 .07300 Uiso ? ? 1.00000 ? ? H433 .99466 .63201 .42325 .09500 Uiso ? ? 1.00000 ? ? H434 .90374 .64111 .46661 .12500 Uiso ? ? 1.00000 ? ? H435 .79206 .67567 .43004 .11600 Uiso ? ? 1.00000 ? ? H436 .76995 .70156 .34784 .08300 Uiso ? ? 1.00000 ? ? H44 .74271 .66695 .26548 .04000 Uiso ? ? 1.00000 ? ? H452 .80442 .75110 .13058 .04800 Uiso ? ? 1.00000 ? ? H453 .72620 .75270 .05825 .06000 Uiso ? ? 1.00000 ? ? H454 .62626 .68387 .04745 .06500 Uiso ? ? 1.00000 ? ? H455 .60407 .61555 .10907 .06900 Uiso ? ? 1.00000 ? ? H456 .68051 .61532 .18310 .05500 Uiso ? ? 1.00000 ? ? H532 1.07811 .84284 .11158 .08600 Uiso ? ? 1.00000 ? ? H533 1.17245 .90861 .09444 .12200 Uiso ? ? 1.00000 ? ? H534 1.20269 .89877 .01687 .14600 Uiso ? ? 1.00000 ? ? H535 1.13624 .83139 -.04047 .14300 Uiso ? ? 1.00000 ? ? H536 1.04131 .76837 -.02319 .12200 Uiso ? ? 1.00000 ? ? H54 .93025 .72476 -.00608 .07400 Uiso ? ? 1.00000 ? ? H552 .85768 .59349 .10978 .07600 Uiso ? ? 1.00000 ? ? H553 .75973 .52057 .09190 .09400 Uiso ? ? 1.00000 ? ? H554 .68727 .52590 .01682 .10900 Uiso ? ? 1.00000 ? ? H555 .71472 .60075 -.04049 .11300 Uiso ? ? 1.00000 ? ? H556 .80930 .67750 -.02284 .10200 Uiso ? ? 1.00000 ? ? H632 1.06625 .63388 .08224 .05900 Uiso ? ? 1.00000 ? ? H633 1.10977 .61893 .01131 .07700 Uiso ? ? 1.00000 ? ? H634 1.12014 .50905 -.01834 .08300 Uiso ? ? 1.00000 ? ? H635 1.07609 .41903 .01805 .07700 Uiso ? ? 1.00000 ? ? H636 1.02964 .43420 .08821 .06500 Uiso ? ? 1.00000 ? ? H64 .93538 .47701 .13860 .04600 Uiso ? ? 1.00000 ? ? H652 .97987 .53979 .29135 .05600 Uiso ? ? 1.00000 ? ? H653 .90109 .51252 .34234 .07300 Uiso ? ? 1.00000 ? ? H654 .78175 .48917 .30993 .08100 Uiso ? ? 1.00000 ? ? H655 .74446 .48850 .22701 .07700 Uiso ? ? 1.00000 ? ? H656 .82560 .51176 .17587 .06500 Uiso ? ? 1.00000 ? ? H732 1.15655 .68290 .12824 .05100 Uiso ? ? 1.00000 ? ? H733 1.20688 .69461 .06032 .05900 Uiso ? ? 1.00000 ? ? H734 1.30448 .76332 .06093 .06400 Uiso ? ? 1.00000 ? ? H735 1.34739 .82542 .12856 .08100 Uiso ? ? 1.00000 ? ? H736 1.29868 .81351 .19808 .06300 Uiso ? ? 1.00000 ? ? H74 1.26942 .74367 .27405 .03800 Uiso ? ? 1.00000 ? ? H752 1.05975 .74607 .33348 .05400 Uiso ? ? 1.00000 ? ? H753 1.06389 .75327 .41573 .07100 Uiso ? ? 1.00000 ? ? H754 1.17144 .73941 .46776 .07800 Uiso ? ? 1.00000 ? ? H755 1.27295 .71173 .43846 .08100 Uiso ? ? 1.00000 ? ? H756 1.27135 .70666 .35574 .06000 Uiso ? ? 1.00000 ? ? H832 1.24074 .54325 .12106 .04700 Uiso ? ? 1.00000 ? ? H833 1.25384 .54733 .04102 .05600 Uiso ? ? 1.00000 ? ? H834 1.35760 .58999 .01999 .05600 Uiso ? ? 1.00000 ? ? H835 1.44936 .62843 .07955 .05800 Uiso ? ? 1.00000 ? ? H836 1.43563 .62510 .15984 .04900 Uiso ? ? 1.00000 ? ? H84 1.43468 .57487 .23900 .03900 Uiso ? ? 1.00000 ? ? H852 1.28517 .56113 .35100 .06100 Uiso ? ? 1.00000 ? ? H853 1.32926 .57269 .43237 .08100 Uiso ? ? 1.00000 ? ? H854 1.45107 .58879 .45849 .06700 Uiso ? ? 1.00000 ? ? H855 1.52677 .59668 .40344 .05300 Uiso ? ? 1.00000 ? ? H856 1.48232 .58812 .32204 .04400 Uiso ? ? 1.00000 ? ? H932 1.11990 .42641 .16925 .04500 Uiso ? ? 1.00000 ? ? H933 1.11620 .34213 .11291 .05300 Uiso ? ? 1.00000 ? ? H934 1.08573 .23315 .12929 .05300 Uiso ? ? 1.00000 ? ? H935 1.06098 .20799 .20483 .05100 Uiso ? ? 1.00000 ? ? H936 1.06610 .29080 .26258 .04600 Uiso ? ? 1.00000 ? ? H94 1.06204 .37546 .31819 .04200 Uiso ? ? 1.00000 ? ? H952 1.16246 .57421 .37954 .05000 Uiso ? ? 1.00000 ? ? H953 1.16198 .59836 .46009 .06000 Uiso ? ? 1.00000 ? ? H954 1.09499 .53303 .50399 .06500 Uiso ? ? 1.00000 ? ? H955 1.02566 .44660 .46592 .06500 Uiso ? ? 1.00000 ? ? H956 1.02697 .42128 .38652 .05900 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 La1 .01852(9) .02038(9) .03554(10) -.00005(7) .00428(8) -.00044(7) La2 .02014(10) .02486(10) .03031(10) .00147(7) .00270(8) -.00240(8) La3 .01814(9) .02069(9) .03124(10) -.00127(7) .00366(7) -.00099(7) N11 .0210(14) .0257(14) .0371(15) -.0008(11) .0037(12) -.0032(12) N12 .0234(15) .0269(14) .0345(15) .0006(11) .0026(12) .0005(11) C13 .0218(17) .0247(16) .0395(19) .0010(13) .0020(15) .0021(14) C131 .029(2) .0328(18) .041(2) .0068(15) .0052(16) -.0014(15) C132 .030(2) .044(2) .044(2) .0059(17) .0026(17) -.0002(17) C133 .054(3) .056(3) .041(2) .014(2) -.001(2) .002(2) C134 .046(3) .058(3) .050(2) .015(2) -.011(2) -.009(2) C135 .031(2) .048(2) .073(3) .0063(18) -.005(2) -.019(2) C136 .031(2) .039(2) .052(2) .0030(17) .0016(18) -.0089(18) C14 .0222(17) .0275(17) .047(2) .0009(14) .0090(15) -.0011(15) C15 .0235(17) .0219(16) .041(2) -.0003(13) .0083(15) -.0008(14) C151 .036(2) .035(2) .038(2) .0068(16) .0099(16) .0001(15) C152 .038(2) .085(3) .041(2) .004(2) .0084(19) -.008(2) C153 .056(3) .139(5) .039(2) .021(3) .007(2) -.012(3) C154 .077(4) .127(5) .039(2) .031(3) .019(3) .001(3) C155 .058(3) .092(4) .053(3) .016(3) .029(2) .009(3) C156 .039(2) .046(2) .050(2) .0058(18) .0120(19) .0001(18) N21 .0235(15) .0320(15) .0414(17) .0000(12) .0019(13) -.0045(13) N22 .0226(15) .0238(14) .0443(17) -.0008(11) .0051(13) -.0048(12) C23 .0218(17) .0273(17) .056(2) -.0002(14) .0108(16) -.0101(16) C231 .0221(18) .0219(16) .064(2) .0013(14) .0148(17) -.0041(16) C232 .029(2) .0282(18) .061(2) -.0009(15) .0123(18) -.0031(17) C233 .036(2) .042(2) .065(3) .0026(18) .016(2) .004(2) C234 .040(2) .031(2) .083(3) .0058(17) .025(2) .013(2) C235 .036(2) .027(2) .098(3) .0021(16) .027(2) -.000(2) C236 .027(2) .031(2) .072(3) -.0006(15) .013(2) -.0094(18) C24 .030(2) .035(2) .057(2) -.0046(16) .0048(18) -.0162(18) C25 .0268(19) .039(2) .046(2) -.0007(16) .0036(16) -.0128(17) C251 .032(2) .052(2) .046(2) .0056(18) .0014(17) -.0134(18) C252 .036(2) .063(3) .050(2) .001(2) -.002(2) -.006(2) C253 .047(3) .089(4) .049(3) .013(2) .001(2) .001(2) C254 .046(3) .105(4) .041(2) .018(3) .004(2) -.005(2) C255 .071(4) .125(5) .051(3) -.008(3) -.017(3) -.028(3) C256 .064(3) .075(3) .066(3) -.017(3) -.013(3) -.012(3) N31 .0297(16) .0267(14) .0350(15) -.0018(12) .0049(13) .0003(12) N32 .0227(15) .0234(14) .0424(16) -.0007(11) .0061(13) -.0002(12) C332 .0248(19) .033(2) .060(2) -.0010(15) .0074(17) -.0036(17) C333 .038(2) .039(2) .060(3) .0001(18) .000(2) -.0082(19) C334 .031(2) .035(2) .079(3) -.0021(17) -.004(2) -.011(2) C335 .0220(19) .0283(19) .087(3) -.0040(15) .012(2) -.0021(19) C336 .027(2) .0267(18) .067(3) -.0023(15) .0124(18) -.0002(17) C34 .0270(19) .0266(17) .050(2) -.0060(14) .0115(16) .0005(15) C35 .031(2) .0239(16) .043(2) .0006(14) .0127(16) -.0007(14) C351 .041(2) .0310(18) .038(2) -.0026(16) .0072(17) -.0003(15) C352 .045(2) .059(3) .047(2) -.012(2) -.002(2) .016(2) C353 .047(3) .086(4) .059(3) -.020(3) -.008(2) .027(3) C354 .060(3) .074(3) .046(2) -.013(2) -.006(2) .020(2) C355 .065(3) .059(3) .046(2) -.008(2) .015(2) .011(2) C356 .048(3) .049(2) .042(2) -.004(2) .013(2) .0064(18) C33 .0246(17) .0208(15) .046(2) .0005(13) .0096(15) -.0027(14) C331 .0256(18) .0184(15) .054(2) .0020(13) .0075(16) -.0032(14) N41 .0263(15) .0214(13) .0448(17) .0014(11) .0066(13) .0012(12) N42 .0222(15) .0246(14) .0511(18) .0017(12) .0020(13) .0061(13) C43 .0249(18) .0226(16) .047(2) -.0001(14) .0020(16) .0047(15) C431 .037(2) .038(2) .046(2) -.0060(17) -.0014(18) .0106(17) C432 .048(3) .049(3) .069(3) -.005(2) -.009(2) .011(2) C433 .076(4) .070(3) .075(3) -.012(3) -.033(3) .022(3) C434 .097(5) .124(5) .056(3) -.045(4) -.024(3) .033(3) C435 .077(4) .166(6) .048(3) -.051(4) .005(3) .014(3) C436 .049(3) .102(4) .048(3) -.025(3) .002(2) .005(3) C44 .0238(18) .0289(17) .045(2) -.0010(14) .0070(16) .0013(15) C45 .0240(17) .0198(15) .043(2) -.0014(13) .0046(15) -.0011(14) C451 .030(2) .0271(17) .044(2) .0022(15) .0051(16) -.0074(15) C452 .035(2) .033(2) .046(2) .0033(16) .0053(17) -.0023(16) C453 .049(3) .044(2) .048(2) .010(2) .003(2) -.0034(18) C454 .049(3) .055(3) .050(2) .007(2) -.002(2) -.009(2) C455 .037(2) .060(3) .062(3) -.009(2) -.003(2) -.014(2) C456 .034(2) .040(2) .057(2) -.0056(17) .0067(19) -.0060(18) N51 .0391(19) .049(2) .0384(17) .0137(15) -.0019(15) -.0069(15) N52 .045(2) .0417(18) .0383(17) .0168(15) .0113(15) .0038(14) C53 .063(3) .054(3) .043(2) .030(2) .017(2) .011(2) C531 .077(3) .063(3) .052(3) .034(3) .027(2) .023(2) C532 .091(4) .039(2) .104(4) .022(2) .062(3) .021(2) C533 .111(5) .047(3) .162(6) .024(3) .083(5) .031(3) C534 .111(5) .089(4) .171(7) .040(4) .091(5) .079(4) C535 .115(6) .159(7) .102(5) .054(5) .061(4) .085(5) C536 .091(4) .136(5) .056(3) .054(4) .032(3) .040(3) C54 .073(3) .075(3) .033(2) .037(3) .003(2) -.005(2) C55 .053(3) .057(3) .039(2) .027(2) -.004(2) -.0097(19) C551 .049(3) .070(3) .047(2) .028(2) -.015(2) -.029(2) C552 .052(3) .055(3) .070(3) .016(2) -.015(2) -.023(2) C553 .050(3) .065(3) .093(4) .011(2) -.016(3) -.038(3) C554 .055(3) .098(4) .116(5) .022(3) -.021(3) -.059(4) C555 .067(4) .104(4) .071(3) .023(3) -.035(3) -.052(3) C556 .071(4) .096(4) .060(3) .040(3) -.014(3) -.036(3) N61 .0227(15) .0250(14) .0431(17) -.0044(11) .0031(13) -.0026(12) N62 .0280(15) .0269(14) .0376(16) .0003(12) .0017(13) -.0045(12) C63 .0272(18) .0282(18) .042(2) .0035(14) -.0037(16) -.0076(15) C631 .028(2) .041(2) .042(2) .0060(16) -.0069(16) -.0125(17) C632 .040(2) .056(3) .045(2) -.004(2) .0058(19) -.016(2) C633 .051(3) .084(3) .051(3) -.012(2) .008(2) -.015(2) C634 .042(3) .104(4) .056(3) .010(3) .003(2) -.036(3) C635 .055(3) .066(3) .059(3) .015(2) -.005(2) -.030(2) C636 .051(3) .050(2) .047(2) .015(2) -.009(2) -.018(2) C64 .0275(19) .0256(17) .056(2) -.0001(15) -.0071(17) -.0077(16) C65 .0175(16) .0222(16) .058(2) .0007(13) -.0020(16) -.0011(15) C651 .0253(19) .0184(16) .076(3) -.0018(14) .0098(18) -.0006(16) C652 .033(2) .031(2) .074(3) -.0008(16) .015(2) .0068(19) C653 .050(3) .036(2) .086(3) .005(2) .029(2) .013(2) C654 .052(3) .030(2) .121(4) .006(2) .049(3) .015(2) C655 .029(2) .029(2) .128(4) -.0041(17) .021(2) .009(2) C656 .028(2) .0265(19) .092(3) -.0008(16) .008(2) -.001(2) N71 .0239(15) .0252(14) .0366(15) -.0011(11) .0050(12) -.0060(11) N72 .0236(14) .0212(13) .0355(15) -.0015(11) .0038(12) -.0033(11) C73 .0247(17) .0166(15) .045(2) -.0020(13) .0047(15) -.0027(13) C731 .0247(18) .0279(17) .043(2) -.0009(14) .0048(15) .0006(15) C732 .040(2) .039(2) .044(2) -.0071(17) .0069(18) -.0039(17) C733 .051(3) .050(2) .040(2) -.000(2) .007(2) -.0062(18) C734 .047(3) .062(3) .046(2) -.002(2) .014(2) -.001(2) C735 .045(3) .093(4) .065(3) -.030(3) .024(2) -.012(3) C736 .037(2) .071(3) .048(2) -.023(2) .0111(19) -.011(2) C74 .0233(17) .0272(17) .042(2) -.0048(14) .0010(15) -.0036(14) C75 .0254(17) .0206(15) .0380(18) -.0001(13) .0029(15) -.0063(13) C751 .034(2) .0261(17) .0376(19) -.0065(15) .0021(16) -.0052(14) C752 .044(2) .042(2) .043(2) -.0003(18) .0084(18) -.0048(17) C753 .066(3) .057(3) .051(3) -.001(2) .023(2) -.007(2) C754 .084(4) .068(3) .039(2) -.018(3) .009(2) -.011(2) C755 .057(3) .084(4) .043(2) -.018(3) -.005(2) -.007(2) C756 .041(2) .055(3) .044(2) -.012(2) -.0019(19) -.003(2) N81 .0225(14) .0267(14) .0335(15) .0003(11) .0048(12) .0023(11) N82 .0229(14) .0264(14) .0320(15) .0016(11) .0036(12) -.0010(11) C83 .0244(17) .0239(16) .0371(18) .0013(13) .0055(15) .0005(13) C831 .0275(18) .0306(18) .0373(19) .0037(14) .0087(15) .0007(14) C832 .033(2) .038(2) .041(2) -.0016(16) .0062(17) -.0081(16) C833 .047(2) .049(2) .038(2) .000(2) .0039(18) -.0075(18) C834 .054(3) .050(2) .035(2) .009(2) .0111(19) .0006(17) C835 .037(2) .050(2) .050(2) .0017(18) .0183(19) .0010(18) C836 .033(2) .046(2) .036(2) .0021(17) .0077(16) -.0009(16) C84 .0209(17) .0293(17) .043(2) .0004(14) .0054(15) .0026(15) C85 .0200(16) .0272(17) .0395(19) .0017(13) .0035(14) .0039(14) C851 .0262(18) .0282(17) .0356(18) .0031(14) .0011(15) .0062(14) C852 .029(2) .076(3) .042(2) .001(2) .0062(17) .012(2) C853 .042(3) .124(5) .041(2) .009(3) .010(2) .010(3) C854 .047(3) .076(3) .037(2) .005(2) -.001(2) .006(2) C855 .034(2) .047(2) .043(2) -.0005(18) -.0042(17) .0042(18) C856 .0275(19) .0294(18) .043(2) .0027(14) .0033(16) .0048(15) N91 .0276(15) .0273(14) .0328(15) -.0017(12) .0053(12) -.0018(12) N92 .0255(15) .0251(14) .0376(16) -.0001(12) .0079(12) -.0034(12) C93 .0237(17) .0227(16) .0390(19) .0011(13) .0040(15) .0030(13) C931 .0203(16) .0258(16) .0386(18) .0018(13) .0044(14) -.0010(14) C932 .040(2) .0258(17) .046(2) .0009(15) .0088(18) -.0016(15) C933 .047(2) .042(2) .042(2) .0044(18) .0135(19) -.0047(17) C934 .032(2) .034(2) .060(3) .0045(16) .0034(18) -.0133(18) C935 .029(2) .0252(18) .066(3) -.0006(15) .0078(18) -.0066(17) C936 .029(2) .0296(18) .051(2) .0004(15) .0072(17) .0025(16) C94 .032(2) .0278(17) .040(2) -.0032(15) .0065(16) .0032(15) C95 .0251(18) .0321(18) .0335(18) -.0021(14) .0027(14) .0035(14) C951 .031(2) .0344(19) .0350(19) -.0027(15) .0048(15) .0027(15) C952 .037(2) .043(2) .039(2) -.0059(17) .0040(17) .0014(17) C953 .048(3) .050(2) .044(2) -.007(2) .001(2) -.0075(19) C954 .060(3) .061(3) .039(2) -.013(2) .011(2) -.009(2) C955 .061(3) .064(3) .040(2) -.021(2) .016(2) .000(2) C956 .051(3) .052(2) .040(2) -.014(2) .011(2) -.0029(18) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published La1 N11 . . 2.431(3) ? La1 N12 . . 2.518(3) ? La1 N21 . . 2.478(3) ? La1 N22 . . 2.459(3) ? La1 N31 . . 2.569(3) ? La1 N32 . . 2.665(3) ? La1 N41 . . 2.714(3) ? La1 N42 . . 2.718(3) ? La2 N31 . . 2.922(3) ? La2 N32 . . 2.628(3) ? La2 N41 . . 2.526(3) ? La2 N42 . . 2.835(3) ? La2 N51 . . 2.466(3) ? La2 N52 . . 2.467(3) ? La2 N61 . . 2.605(3) ? La2 N62 . . 2.829(3) ? La2 N71 . . 2.667(2) ? La2 N72 . . 2.531(3) ? La3 N61 . . 2.725(3) ? La3 N62 . . 2.577(3) ? La3 N71 . . 2.726(3) ? La3 N72 . . 2.770(2) ? La3 N81 . . 2.453(3) ? La3 N82 . . 2.463(3) ? La3 N91 . . 2.465(3) ? La3 N92 . . 2.463(3) ? N11 N12 . . 1.373(4) ? N11 C15 . . 1.353(5) ? N12 C13 . . 1.350(4) ? C13 C131 . . 1.481(5) ? C13 C14 . . 1.398(5) ? C131 C132 . . 1.391(5) ? C131 C136 . . 1.401(5) ? C132 C133 . . 1.390(5) ? C132 H132 . . .965 ? C133 C134 . . 1.382(6) ? C133 H133 . . .971 ? C134 C135 . . 1.385(7) ? C134 H134 . . .967 ? C135 C136 . . 1.388(6) ? C135 H135 . . .966 ? C136 H136 . . .974 ? C14 C15 . . 1.384(4) ? C14 H14 . . .961 ? C15 C151 . . 1.463(5) ? C151 C152 . . 1.391(5) ? C151 C156 . . 1.398(6) ? C152 C153 . . 1.373(6) ? C152 H152 . . .973 ? C153 C154 . . 1.386(8) ? C153 H153 . . .978 ? C154 C155 . . 1.389(7) ? C154 H154 . . .973 ? C155 C156 . . 1.372(6) ? C155 H155 . . .968 ? C156 H156 . . .972 ? N21 N22 . . 1.374(4) ? N21 C25 . . 1.347(4) ? N22 C23 . . 1.348(4) ? C23 C231 . . 1.477(5) ? C23 C24 . . 1.403(5) ? C231 C232 . . 1.389(5) ? C231 C236 . . 1.401(5) ? C232 C233 . . 1.379(6) ? C232 H232 . . .960 ? C233 C234 . . 1.389(5) ? C233 H233 . . .968 ? C234 C235 . . 1.375(6) ? C234 H234 . . .972 ? C235 C236 . . 1.380(6) ? C235 H235 . . .965 ? C236 H236 . . .974 ? C24 C25 . . 1.389(5) ? C24 H24 . . .964 ? C25 C251 . . 1.476(5) ? C251 C252 . . 1.386(6) ? C251 C256 . . 1.390(6) ? C252 C253 . . 1.390(6) ? C252 H252 . . .970 ? C253 C254 . . 1.372(6) ? C253 H253 . . .974 ? C254 C255 . . 1.367(8) ? C254 H254 . . .968 ? C255 C256 . . 1.392(7) ? C255 H255 . . .972 ? C256 H256 . . .980 ? N31 N32 . . 1.405(4) ? N31 C35 . . 1.349(5) ? N32 C33 . . 1.363(4) ? C332 C333 . . 1.397(5) ? C332 C331 . . 1.384(6) ? C332 H332 . . .962 ? C333 C334 . . 1.382(6) ? C333 H333 . . .981 ? C334 C335 . . 1.379(7) ? C334 H334 . . .969 ? C335 C336 . . 1.390(5) ? C335 H335 . . .962 ? C336 C331 . . 1.398(5) ? C336 H336 . . .977 ? C34 C35 . . 1.388(5) ? C34 C33 . . 1.382(5) ? C34 H34 . . .959 ? C35 C351 . . 1.475(5) ? C351 C352 . . 1.387(6) ? C351 C356 . . 1.387(6) ? C352 C353 . . 1.375(6) ? C352 H352 . . .959 ? C353 C354 . . 1.378(7) ? C353 H353 . . .965 ? C354 C355 . . 1.373(7) ? C354 H354 . . .967 ? C355 C356 . . 1.374(5) ? C355 H355 . . .966 ? C356 H356 . . .965 ? C33 C331 . . 1.481(4) ? N41 N42 . . 1.383(4) ? N41 C45 . . 1.361(4) ? N42 C43 . . 1.367(5) ? C43 C431 . . 1.475(5) ? C43 C44 . . 1.402(4) ? C431 C432 . . 1.402(6) ? C431 C436 . . 1.388(7) ? C432 C433 . . 1.390(7) ? C432 H432 . . .967 ? C433 C434 . . 1.375(9) ? C433 H433 . . .956 ? C434 C435 . . 1.362(8) ? C434 H434 . . .961 ? C435 C436 . . 1.391(7) ? C435 H435 . . .969 ? C436 H436 . . .976 ? C44 C45 . . 1.399(5) ? C44 H44 . . .955 ? C45 C451 . . 1.468(5) ? C451 C452 . . 1.390(5) ? C451 C456 . . 1.399(5) ? C452 C453 . . 1.374(5) ? C452 H452 . . .966 ? C453 C454 . . 1.386(6) ? C453 H453 . . .964 ? C454 C455 . . 1.385(6) ? C454 H454 . . .963 ? C455 C456 . . 1.387(6) ? C455 H455 . . .961 ? C456 H456 . . .968 ? N51 N52 . . 1.385(5) ? N51 C55 . . 1.354(5) ? N52 C53 . . 1.354(5) ? C53 C531 . . 1.470(7) ? C53 C54 . . 1.393(6) ? C531 C532 . . 1.379(7) ? C531 C536 . . 1.402(7) ? C532 C533 . . 1.393(8) ? C532 H532 . . .979 ? C533 C534 . . 1.393(11) ? C533 H533 . . 1.003 ? C534 C535 . . 1.378(9) ? C534 H534 . . .950 ? C535 C536 . . 1.378(10) ? C535 H535 . . .977 ? C536 H536 . . .986 ? C54 C55 . . 1.378(7) ? C54 H54 . . .971 ? C55 C551 . . 1.500(6) ? C551 C552 . . 1.362(7) ? C551 C556 . . 1.419(6) ? C552 C553 . . 1.404(7) ? C552 H552 . . .978 ? C553 C554 . . 1.381(8) ? C553 H553 . . .999 ? C554 C555 . . 1.354(9) ? C554 H554 . . .997 ? C555 C556 . . 1.389(8) ? C555 H555 . . .954 ? C556 H556 . . .993 ? N61 N62 . . 1.407(4) ? N61 C65 . . 1.359(4) ? N62 C63 . . 1.350(4) ? C63 C631 . . 1.474(5) ? C63 C64 . . 1.386(5) ? C631 C632 . . 1.389(6) ? C631 C636 . . 1.400(6) ? C632 C633 . . 1.387(7) ? C632 H632 . . .972 ? C633 C634 . . 1.395(7) ? C633 H633 . . .985 ? C634 C635 . . 1.362(7) ? C634 H634 . . .972 ? C635 C636 . . 1.388(7) ? C635 H635 . . .963 ? C636 H636 . . .969 ? C64 C65 . . 1.384(5) ? C64 H64 . . .967 ? C65 C651 . . 1.474(6) ? C651 C652 . . 1.380(6) ? C651 C656 . . 1.396(5) ? C652 C653 . . 1.385(7) ? C652 H652 . . .967 ? C653 C654 . . 1.389(6) ? C653 H653 . . .984 ? C654 C655 . . 1.369(8) ? C654 H654 . . .972 ? C655 C656 . . 1.402(7) ? C655 H655 . . .973 ? C656 H656 . . .978 ? N71 N72 . . 1.393(4) ? N71 C75 . . 1.362(4) ? N72 C73 . . 1.366(4) ? C73 C731 . . 1.475(5) ? C73 C74 . . 1.381(5) ? C731 C732 . . 1.382(5) ? C731 C736 . . 1.391(6) ? C732 C733 . . 1.380(6) ? C732 H732 . . .960 ? C733 C734 . . 1.361(6) ? C733 H733 . . .962 ? C734 C735 . . 1.370(6) ? C734 H734 . . .968 ? C735 C736 . . 1.398(7) ? C735 H735 . . .964 ? C736 H736 . . .973 ? C74 C75 . . 1.405(5) ? C74 H74 . . .963 ? C75 C751 . . 1.475(5) ? C751 C752 . . 1.384(6) ? C751 C756 . . 1.398(5) ? C752 C753 . . 1.385(6) ? C752 H752 . . .971 ? C753 C754 . . 1.379(6) ? C753 H753 . . .970 ? C754 C755 . . 1.363(7) ? C754 H754 . . .970 ? C755 C756 . . 1.387(6) ? C755 H755 . . .972 ? C756 H756 . . .975 ? N81 N82 . . 1.381(4) ? N81 C85 . . 1.347(4) ? N82 C83 . . 1.356(5) ? C83 C831 . . 1.471(5) ? C83 C84 . . 1.400(4) ? C831 C832 . . 1.389(5) ? C831 C836 . . 1.388(5) ? C832 C833 . . 1.391(5) ? C832 H832 . . .967 ? C833 C834 . . 1.397(6) ? C833 H833 . . .963 ? C834 C835 . . 1.377(5) ? C834 H834 . . .968 ? C835 C836 . . 1.394(6) ? C835 H835 . . .966 ? C836 H836 . . .975 ? C84 C85 . . 1.405(5) ? C84 H84 . . .962 ? C85 C851 . . 1.453(5) ? C851 C852 . . 1.391(6) ? C851 C856 . . 1.393(5) ? C852 C853 . . 1.384(6) ? C852 H852 . . .964 ? C853 C854 . . 1.378(6) ? C853 H853 . . .973 ? C854 C855 . . 1.374(6) ? C854 H854 . . .971 ? C855 C856 . . 1.381(5) ? C855 H855 . . .968 ? C856 H856 . . .970 ? N91 N92 . . 1.383(4) ? N91 C95 . . 1.350(5) ? N92 C93 . . 1.357(4) ? C93 C931 . . 1.479(5) ? C93 C94 . . 1.394(5) ? C931 C932 . . 1.390(5) ? C931 C936 . . 1.405(5) ? C932 C933 . . 1.383(5) ? C932 H932 . . .968 ? C933 C934 . . 1.380(5) ? C933 H933 . . .958 ? C934 C935 . . 1.384(6) ? C934 H934 . . .965 ? C935 C936 . . 1.378(5) ? C935 H935 . . .961 ? C936 H936 . . .972 ? C94 C95 . . 1.403(5) ? C94 H94 . . .963 ? C95 C951 . . 1.472(5) ? C951 C952 . . 1.373(5) ? C951 C956 . . 1.400(6) ? C952 C953 . . 1.391(6) ? C952 H952 . . .970 ? C953 C954 . . 1.379(6) ? C953 H953 . . .973 ? C954 C955 . . 1.376(6) ? C954 H954 . . .965 ? C955 C956 . . 1.380(6) ? C955 H955 . . .965 ? C956 H956 . . .966 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 La1 N12 . . . 32.15(9) ? N11 La1 N21 . . . 89.11(9) ? N11 La1 N22 . . . 92.30(9) ? N11 La1 N31 . . . 143.86(8) ? N11 La1 N32 . . . 166.17(8) ? N11 La1 N41 . . . 116.74(9) ? N11 La1 N42 . . . 117.70(9) ? N12 La1 N21 . . . 114.52(9) ? N12 La1 N22 . . . 103.19(9) ? N12 La1 N31 . . . 114.29(9) ? N12 La1 N32 . . . 145.05(9) ? N12 La1 N41 . . . 102.84(8) ? N12 La1 N42 . . . 120.36(8) ? N21 La1 N22 . . . 32.32(9) ? N21 La1 N31 . . . 104.52(9) ? N21 La1 N32 . . . 82.93(9) ? N21 La1 N41 . . . 138.30(8) ? N21 La1 N42 . . . 110.41(8) ? N22 La1 N31 . . . 83.23(9) ? N22 La1 N32 . . . 74.96(9) ? N22 La1 N41 . . . 150.90(9) ? N22 La1 N42 . . . 134.81(8) ? N31 La1 N32 . . . 31.06(8) ? N31 La1 N41 . . . 74.35(9) ? N31 La1 N42 . . . 89.07(9) ? N32 La1 N41 . . . 76.28(8) ? N32 La1 N42 . . . 75.83(8) ? N41 La1 N42 . . . 29.49(8) ? N31 La2 N32 . . . 28.70(8) ? N31 La2 N41 . . . 71.39(8) ? N31 La2 N42 . . . 80.24(8) ? N31 La2 N51 . . . 84.94(9) ? N31 La2 N52 . . . 79.54(9) ? N31 La2 N61 . . . 158.27(9) ? N31 La2 N62 . . . 163.73(7) ? N31 La2 N71 . . . 111.98(7) ? N31 La2 N72 . . . 114.32(8) ? N32 La2 N41 . . . 80.25(9) ? N32 La2 N42 . . . 74.43(8) ? N32 La2 N51 . . . 112.45(9) ? N32 La2 N52 . . . 98.77(10) ? N32 La2 N61 . . . 148.55(9) ? N32 La2 N62 . . . 164.55(7) ? N32 La2 N71 . . . 83.80(8) ? N32 La2 N72 . . . 93.04(8) ? N41 La2 N42 . . . 29.17(8) ? N41 La2 N51 . . . 90.43(10) ? N41 La2 N52 . . . 118.16(10) ? N41 La2 N61 . . . 86.90(9) ? N41 La2 N62 . . . 110.93(8) ? N41 La2 N71 . . . 120.00(9) ? N41 La2 N72 . . . 150.94(9) ? N42 La2 N51 . . . 119.27(10) ? N42 La2 N52 . . . 146.68(9) ? N42 La2 N61 . . . 80.37(9) ? N42 La2 N62 . . . 109.84(8) ? N42 La2 N71 . . . 90.84(8) ? N42 La2 N72 . . . 121.79(8) ? N51 La2 N52 . . . 32.62(11) ? N51 La2 N61 . . . 96.11(10) ? N51 La2 N62 . . . 78.98(9) ? N51 La2 N71 . . . 148.21(10) ? N51 La2 N72 . . . 118.02(10) ? N52 La2 N61 . . . 112.58(10) ? N52 La2 N62 . . . 85.51(9) ? N52 La2 N71 . . . 121.31(10) ? N52 La2 N72 . . . 90.73(10) ? N61 La2 N62 . . . 29.66(9) ? N61 La2 N71 . . . 78.00(8) ? N61 La2 N72 . . . 84.41(8) ? N62 La2 N71 . . . 81.33(8) ? N62 La2 N72 . . . 71.98(8) ? N71 La2 N72 . . . 30.96(9) ? N61 La3 N62 . . . 30.62(9) ? N61 La3 N71 . . . 74.99(8) ? N61 La3 N72 . . . 77.79(8) ? N61 La3 N81 . . . 168.39(8) ? N61 La3 N82 . . . 143.20(9) ? N61 La3 N91 . . . 82.23(8) ? N61 La3 N92 . . . 76.21(8) ? N62 La3 N71 . . . 84.98(8) ? N62 La3 N72 . . . 72.33(8) ? N62 La3 N81 . . . 145.36(9) ? N62 La3 N82 . . . 113.44(9) ? N62 La3 N91 . . . 105.20(9) ? N62 La3 N92 . . . 86.04(8) ? N71 La3 N72 . . . 29.36(8) ? N71 La3 N81 . . . 116.58(8) ? N71 La3 N82 . . . 121.68(8) ? N71 La3 N91 . . . 112.09(9) ? N71 La3 N92 . . . 137.27(9) ? N72 La3 N81 . . . 112.63(8) ? N72 La3 N82 . . . 101.67(8) ? N72 La3 N91 . . . 140.34(9) ? N72 La3 N92 . . . 153.94(8) ? N81 La3 N82 . . . 32.62(9) ? N81 La3 N91 . . . 91.87(9) ? N81 La3 N92 . . . 93.43(9) ? N82 La3 N91 . . . 114.59(9) ? N82 La3 N92 . . . 100.17(9) ? N91 La3 N92 . . . 32.59(9) ? La1 N11 N12 . . . 77.42(17) ? La1 N11 C15 . . . 172.3(2) ? N12 N11 C15 . . . 109.0(2) ? La1 N12 N11 . . . 70.44(15) ? La1 N12 C13 . . . 174.6(2) ? N11 N12 C13 . . . 107.4(3) ? N12 C13 C131 . . . 122.7(3) ? N12 C13 C14 . . . 109.4(3) ? C131 C13 C14 . . . 127.8(3) ? C13 C131 C132 . . . 121.8(3) ? C13 C131 C136 . . . 119.8(3) ? C132 C131 C136 . . . 118.4(3) ? C131 C132 C133 . . . 120.6(4) ? C131 C132 H132 . . . 119.3 ? C133 C132 H132 . . . 120.1 ? C132 C133 C134 . . . 120.5(4) ? C132 C133 H133 . . . 120.2 ? C134 C133 H133 . . . 119.3 ? C133 C134 C135 . . . 119.6(4) ? C133 C134 H134 . . . 120.6 ? C135 C134 H134 . . . 119.8 ? C134 C135 C136 . . . 120.2(4) ? C134 C135 H135 . . . 119.9 ? C136 C135 H135 . . . 119.9 ? C131 C136 C135 . . . 120.7(4) ? C131 C136 H136 . . . 119.7 ? C135 C136 H136 . . . 119.6 ? C13 C14 C15 . . . 105.6(3) ? C13 C14 H14 . . . 127.2 ? C15 C14 H14 . . . 127.3 ? N11 C15 C14 . . . 108.7(3) ? N11 C15 C151 . . . 120.2(3) ? C14 C15 C151 . . . 131.1(3) ? C15 C151 C152 . . . 120.1(4) ? C15 C151 C156 . . . 121.2(3) ? C152 C151 C156 . . . 118.7(3) ? C151 C152 C153 . . . 120.6(4) ? C151 C152 H152 . . . 119.5 ? C153 C152 H152 . . . 119.8 ? C152 C153 C154 . . . 120.3(4) ? C152 C153 H153 . . . 120.0 ? C154 C153 H153 . . . 119.7 ? C153 C154 C155 . . . 119.5(4) ? C153 C154 H154 . . . 121.1 ? C155 C154 H154 . . . 119.4 ? C154 C155 C156 . . . 120.2(5) ? C154 C155 H155 . . . 119.4 ? C156 C155 H155 . . . 120.4 ? C151 C156 C155 . . . 120.5(4) ? C151 C156 H156 . . . 119.4 ? C155 C156 H156 . . . 120.1 ? La1 N21 N22 . . . 73.11(16) ? La1 N21 C25 . . . 173.7(2) ? N22 N21 C25 . . . 108.3(3) ? La1 N22 N21 . . . 74.57(16) ? La1 N22 C23 . . . 172.8(3) ? N21 N22 C23 . . . 108.8(3) ? N22 C23 C231 . . . 121.8(3) ? N22 C23 C24 . . . 108.1(3) ? C231 C23 C24 . . . 130.1(3) ? C23 C231 C232 . . . 120.7(3) ? C23 C231 C236 . . . 121.7(3) ? C232 C231 C236 . . . 117.6(3) ? C231 C232 C233 . . . 121.7(3) ? C231 C232 H232 . . . 118.6 ? C233 C232 H232 . . . 119.7 ? C232 C233 C234 . . . 119.7(4) ? C232 C233 H233 . . . 120.0 ? C234 C233 H233 . . . 120.3 ? C233 C234 C235 . . . 119.7(4) ? C233 C234 H234 . . . 119.9 ? C235 C234 H234 . . . 120.4 ? C234 C235 C236 . . . 120.4(3) ? C234 C235 H235 . . . 119.7 ? C236 C235 H235 . . . 119.9 ? C231 C236 C235 . . . 121.0(4) ? C231 C236 H236 . . . 118.8 ? C235 C236 H236 . . . 120.3 ? C23 C24 C25 . . . 106.0(3) ? C23 C24 H24 . . . 127.2 ? C25 C24 H24 . . . 126.8 ? N21 C25 C24 . . . 108.8(3) ? N21 C25 C251 . . . 121.6(3) ? C24 C25 C251 . . . 129.6(3) ? C25 C251 C252 . . . 121.6(3) ? C25 C251 C256 . . . 120.9(4) ? C252 C251 C256 . . . 117.4(4) ? C251 C252 C253 . . . 121.8(4) ? C251 C252 H252 . . . 119.2 ? C253 C252 H252 . . . 119.0 ? C252 C253 C254 . . . 120.1(5) ? C252 C253 H253 . . . 120.0 ? C254 C253 H253 . . . 119.9 ? C253 C254 C255 . . . 118.7(4) ? C253 C254 H254 . . . 119.7 ? C255 C254 H254 . . . 121.6 ? C254 C255 C256 . . . 121.8(5) ? C254 C255 H255 . . . 118.9 ? C256 C255 H255 . . . 119.2 ? C251 C256 C255 . . . 120.1(5) ? C251 C256 H256 . . . 119.2 ? C255 C256 H256 . . . 120.7 ? La1 N31 La2 . . . 95.93(8) ? La1 N31 N32 . . . 78.22(17) ? La1 N31 C35 . . . 146.4(2) ? La2 N31 N32 . . . 63.96(14) ? La2 N31 C35 . . . 116.5(2) ? N32 N31 C35 . . . 107.1(3) ? La1 N32 La2 . . . 101.04(9) ? La1 N32 N31 . . . 70.71(17) ? La1 N32 C33 . . . 146.8(2) ? La2 N32 N31 . . . 87.34(16) ? La2 N32 C33 . . . 112.0(2) ? N31 N32 C33 . . . 107.5(3) ? C333 C332 C331 . . . 120.4(4) ? C333 C332 H332 . . . 120.0 ? C331 C332 H332 . . . 119.6 ? C332 C333 C334 . . . 119.6(4) ? C332 C333 H333 . . . 119.9 ? C334 C333 H333 . . . 120.6 ? C333 C334 C335 . . . 120.3(4) ? C333 C334 H334 . . . 119.1 ? C335 C334 H334 . . . 120.6 ? C334 C335 C336 . . . 120.6(4) ? C334 C335 H335 . . . 119.4 ? C336 C335 H335 . . . 120.0 ? C335 C336 C331 . . . 119.4(4) ? C335 C336 H336 . . . 120.7 ? C331 C336 H336 . . . 119.9 ? C35 C34 C33 . . . 106.0(3) ? C35 C34 H34 . . . 126.8 ? C33 C34 H34 . . . 127.1 ? N31 C35 C34 . . . 110.0(3) ? N31 C35 C351 . . . 121.9(3) ? C34 C35 C351 . . . 127.9(3) ? C35 C351 C352 . . . 120.9(4) ? C35 C351 C356 . . . 119.8(3) ? C352 C351 C356 . . . 119.1(3) ? C351 C352 C353 . . . 120.2(4) ? C351 C352 H352 . . . 120.4 ? C353 C352 H352 . . . 119.3 ? C352 C353 C354 . . . 120.1(4) ? C352 C353 H353 . . . 119.8 ? C354 C353 H353 . . . 120.2 ? C353 C354 C355 . . . 120.1(4) ? C353 C354 H354 . . . 120.3 ? C355 C354 H354 . . . 119.6 ? C354 C355 C356 . . . 120.2(4) ? C354 C355 H355 . . . 119.8 ? C356 C355 H355 . . . 120.0 ? C351 C356 C355 . . . 120.2(4) ? C351 C356 H356 . . . 119.7 ? C355 C356 H356 . . . 120.0 ? N32 C33 C34 . . . 109.3(3) ? N32 C33 C331 . . . 122.3(3) ? C34 C33 C331 . . . 128.3(3) ? C332 C331 C336 . . . 119.7(3) ? C332 C331 C33 . . . 120.6(3) ? C336 C331 C33 . . . 119.6(3) ? La1 N41 La2 . . . 102.41(9) ? La1 N41 N42 . . . 75.42(16) ? La1 N41 C45 . . . 87.26(18) ? La2 N41 N42 . . . 87.92(18) ? La2 N41 C45 . . . 162.2(2) ? N42 N41 C45 . . . 109.2(3) ? La1 N42 La2 . . . 94.71(9) ? La1 N42 N41 . . . 75.09(16) ? La1 N42 C43 . . . 87.17(18) ? La2 N42 N41 . . . 62.91(17) ? La2 N42 C43 . . . 168.5(2) ? N41 N42 C43 . . . 106.9(3) ? N42 C43 C431 . . . 123.1(3) ? N42 C43 C44 . . . 109.8(3) ? C431 C43 C44 . . . 127.0(3) ? C43 C431 C432 . . . 120.7(4) ? C43 C431 C436 . . . 119.8(3) ? C432 C431 C436 . . . 119.4(4) ? C431 C432 C433 . . . 119.4(5) ? C431 C432 H432 . . . 119.7 ? C433 C432 H432 . . . 120.9 ? C432 C433 C434 . . . 120.3(5) ? C432 C433 H433 . . . 119.4 ? C434 C433 H433 . . . 120.2 ? C433 C434 C435 . . . 120.4(5) ? C433 C434 H434 . . . 119.2 ? C435 C434 H434 . . . 120.4 ? C434 C435 C436 . . . 120.6(6) ? C434 C435 H435 . . . 119.6 ? C436 C435 H435 . . . 119.8 ? C431 C436 C435 . . . 119.7(4) ? C431 C436 H436 . . . 119.2 ? C435 C436 H436 . . . 121.0 ? C43 C44 C45 . . . 105.3(3) ? C43 C44 H44 . . . 127.0 ? C45 C44 H44 . . . 127.7 ? N41 C45 C44 . . . 108.8(3) ? N41 C45 C451 . . . 120.4(3) ? C44 C45 C451 . . . 130.7(3) ? C45 C451 C452 . . . 120.3(3) ? C45 C451 C456 . . . 120.4(3) ? C452 C451 C456 . . . 119.3(3) ? C451 C452 C453 . . . 121.5(3) ? C451 C452 H452 . . . 119.5 ? C453 C452 H452 . . . 119.0 ? C452 C453 C454 . . . 119.3(4) ? C452 C453 H453 . . . 120.9 ? C454 C453 H453 . . . 119.8 ? C453 C454 C455 . . . 120.0(4) ? C453 C454 H454 . . . 120.0 ? C455 C454 H454 . . . 120.0 ? C454 C455 C456 . . . 121.0(4) ? C454 C455 H455 . . . 119.2 ? C456 C455 H455 . . . 119.8 ? C451 C456 C455 . . . 119.0(4) ? C451 C456 H456 . . . 120.2 ? C455 C456 H456 . . . 120.8 ? La2 N51 N52 . . . 73.70(17) ? La2 N51 C55 . . . 178.2(3) ? N52 N51 C55 . . . 108.1(3) ? La2 N52 N51 . . . 73.68(18) ? La2 N52 C53 . . . 178.6(3) ? N51 N52 C53 . . . 107.8(3) ? N52 C53 C531 . . . 120.9(4) ? N52 C53 C54 . . . 108.8(4) ? C531 C53 C54 . . . 130.2(4) ? C53 C531 C532 . . . 121.6(4) ? C53 C531 C536 . . . 120.5(4) ? C532 C531 C536 . . . 117.9(5) ? C531 C532 C533 . . . 122.1(5) ? C531 C532 H532 . . . 119.4 ? C533 C532 H532 . . . 118.5 ? C532 C533 C534 . . . 119.4(5) ? C532 C533 H533 . . . 120.5 ? C534 C533 H533 . . . 120.2 ? C533 C534 C535 . . . 118.6(6) ? C533 C534 H534 . . . 122.1 ? C535 C534 H534 . . . 119.3 ? C534 C535 C536 . . . 122.0(6) ? C534 C535 H535 . . . 120.0 ? C536 C535 H535 . . . 118.0 ? C531 C536 C535 . . . 119.9(5) ? C531 C536 H536 . . . 118.7 ? C535 C536 H536 . . . 121.3 ? C53 C54 C55 . . . 106.4(4) ? C53 C54 H54 . . . 127.1 ? C55 C54 H54 . . . 126.5 ? N51 C55 C54 . . . 109.0(4) ? N51 C55 C551 . . . 119.9(4) ? C54 C55 C551 . . . 131.1(4) ? C55 C551 C552 . . . 121.7(4) ? C55 C551 C556 . . . 118.9(4) ? C552 C551 C556 . . . 119.4(4) ? C551 C552 C553 . . . 121.0(4) ? C551 C552 H552 . . . 119.7 ? C553 C552 H552 . . . 119.2 ? C552 C553 C554 . . . 118.7(5) ? C552 C553 H553 . . . 119.5 ? C554 C553 H553 . . . 121.8 ? C553 C554 C555 . . . 121.1(5) ? C553 C554 H554 . . . 116.4 ? C555 C554 H554 . . . 122.4 ? C554 C555 C556 . . . 120.9(5) ? C554 C555 H555 . . . 119.3 ? C556 C555 H555 . . . 119.8 ? C551 C556 C555 . . . 118.8(5) ? C551 C556 H556 . . . 120.3 ? C555 C556 H556 . . . 120.9 ? La2 N61 La3 . . . 98.40(9) ? La2 N61 N62 . . . 84.02(16) ? La2 N61 C65 . . . 123.2(2) ? La3 N61 N62 . . . 68.83(15) ? La3 N61 C65 . . . 138.0(2) ? N62 N61 C65 . . . 107.2(3) ? La2 N62 La3 . . . 96.49(8) ? La2 N62 N61 . . . 66.32(15) ? La2 N62 C63 . . . 127.1(2) ? La3 N62 N61 . . . 80.54(15) ? La3 N62 C63 . . . 135.6(2) ? N61 N62 C63 . . . 107.3(3) ? N62 C63 C631 . . . 120.5(3) ? N62 C63 C64 . . . 110.0(3) ? C631 C63 C64 . . . 129.5(3) ? C63 C631 C632 . . . 119.9(3) ? C63 C631 C636 . . . 120.8(3) ? C632 C631 C636 . . . 119.2(4) ? C631 C632 C633 . . . 119.9(4) ? C631 C632 H632 . . . 120.3 ? C633 C632 H632 . . . 119.8 ? C632 C633 C634 . . . 120.0(5) ? C632 C633 H633 . . . 119.2 ? C634 C633 H633 . . . 120.8 ? C633 C634 C635 . . . 120.4(5) ? C633 C634 H634 . . . 120.1 ? C635 C634 H634 . . . 119.5 ? C634 C635 C636 . . . 120.1(4) ? C634 C635 H635 . . . 120.1 ? C636 C635 H635 . . . 119.9 ? C631 C636 C635 . . . 120.3(4) ? C631 C636 H636 . . . 119.1 ? C635 C636 H636 . . . 120.5 ? C63 C64 C65 . . . 105.9(3) ? C63 C64 H64 . . . 127.1 ? C65 C64 H64 . . . 127.1 ? N61 C65 C64 . . . 109.6(3) ? N61 C65 C651 . . . 121.7(3) ? C64 C65 C651 . . . 128.7(3) ? C65 C651 C652 . . . 121.6(3) ? C65 C651 C656 . . . 119.0(4) ? C652 C651 C656 . . . 119.3(4) ? C651 C652 C653 . . . 120.9(4) ? C651 C652 H652 . . . 119.6 ? C653 C652 H652 . . . 119.5 ? C652 C653 C654 . . . 119.9(4) ? C652 C653 H653 . . . 119.8 ? C654 C653 H653 . . . 120.4 ? C653 C654 C655 . . . 119.9(5) ? C653 C654 H654 . . . 119.8 ? C655 C654 H654 . . . 120.3 ? C654 C655 C656 . . . 120.6(4) ? C654 C655 H655 . . . 120.9 ? C656 C655 H655 . . . 118.5 ? C651 C656 C655 . . . 119.4(4) ? C651 C656 H656 . . . 119.7 ? C655 C656 H656 . . . 121.0 ? La2 N71 La3 . . . 96.90(8) ? La2 N71 N72 . . . 69.14(14) ? La2 N71 C75 . . . 174.6(2) ? La3 N71 N72 . . . 77.09(15) ? La3 N71 C75 . . . 86.24(18) ? N72 N71 C75 . . . 107.4(3) ? La2 N72 La3 . . . 99.05(9) ? La2 N72 N71 . . . 79.90(16) ? La2 N72 C73 . . . 170.9(2) ? La3 N72 N71 . . . 73.55(15) ? La3 N72 C73 . . . 87.51(17) ? N71 N72 C73 . . . 108.2(2) ? N72 C73 C731 . . . 119.3(3) ? N72 C73 C74 . . . 109.2(3) ? C731 C73 C74 . . . 131.5(3) ? C73 C731 C732 . . . 121.0(3) ? C73 C731 C736 . . . 121.1(3) ? C732 C731 C736 . . . 117.9(4) ? C731 C732 C733 . . . 121.3(4) ? C731 C732 H732 . . . 118.8 ? C733 C732 H732 . . . 119.8 ? C732 C733 C734 . . . 120.6(4) ? C732 C733 H733 . . . 119.7 ? C734 C733 H733 . . . 119.8 ? C733 C734 C735 . . . 119.5(4) ? C733 C734 H734 . . . 120.6 ? C735 C734 H734 . . . 119.9 ? C734 C735 C736 . . . 120.6(4) ? C734 C735 H735 . . . 119.7 ? C736 C735 H735 . . . 119.6 ? C731 C736 C735 . . . 120.0(4) ? C731 C736 H736 . . . 120.2 ? C735 C736 H736 . . . 119.8 ? C73 C74 C75 . . . 106.1(3) ? C73 C74 H74 . . . 126.9 ? C75 C74 H74 . . . 127.0 ? N71 C75 C74 . . . 109.1(3) ? N71 C75 C751 . . . 121.7(3) ? C74 C75 C751 . . . 129.2(3) ? C75 C751 C752 . . . 120.9(3) ? C75 C751 C756 . . . 119.7(3) ? C752 C751 C756 . . . 119.3(3) ? C751 C752 C753 . . . 120.4(4) ? C751 C752 H752 . . . 119.7 ? C753 C752 H752 . . . 119.8 ? C752 C753 C754 . . . 119.8(4) ? C752 C753 H753 . . . 119.7 ? C754 C753 H753 . . . 120.4 ? C753 C754 C755 . . . 120.2(4) ? C753 C754 H754 . . . 119.3 ? C755 C754 H754 . . . 120.5 ? C754 C755 C756 . . . 120.9(4) ? C754 C755 H755 . . . 119.0 ? C756 C755 H755 . . . 120.0 ? C751 C756 C755 . . . 119.3(4) ? C751 C756 H756 . . . 120.2 ? C755 C756 H756 . . . 120.5 ? La3 N81 N82 . . . 74.12(16) ? La3 N81 C85 . . . 173.0(2) ? N82 N81 C85 . . . 109.1(3) ? La3 N82 N81 . . . 73.26(17) ? La3 N82 C83 . . . 173.3(2) ? N81 N82 C83 . . . 107.8(2) ? N82 C83 C831 . . . 122.4(3) ? N82 C83 C84 . . . 109.0(3) ? C831 C83 C84 . . . 128.6(3) ? C83 C831 C832 . . . 121.5(3) ? C83 C831 C836 . . . 119.9(3) ? C832 C831 C836 . . . 118.6(3) ? C831 C832 C833 . . . 120.7(4) ? C831 C832 H832 . . . 119.8 ? C833 C832 H832 . . . 119.5 ? C832 C833 C834 . . . 119.8(3) ? C832 C833 H833 . . . 120.2 ? C834 C833 H833 . . . 119.9 ? C833 C834 C835 . . . 120.0(4) ? C833 C834 H834 . . . 119.1 ? C835 C834 H834 . . . 120.9 ? C834 C835 C836 . . . 119.6(4) ? C834 C835 H835 . . . 120.3 ? C836 C835 H835 . . . 120.1 ? C831 C836 C835 . . . 121.2(3) ? C831 C836 H836 . . . 119.0 ? C835 C836 H836 . . . 119.8 ? C83 C84 C85 . . . 105.6(3) ? C83 C84 H84 . . . 127.5 ? C85 C84 H84 . . . 126.9 ? N81 C85 C84 . . . 108.5(3) ? N81 C85 C851 . . . 121.1(3) ? C84 C85 C851 . . . 130.4(3) ? C85 C851 C852 . . . 121.1(3) ? C85 C851 C856 . . . 121.1(3) ? C852 C851 C856 . . . 117.8(3) ? C851 C852 C853 . . . 121.0(4) ? C851 C852 H852 . . . 119.2 ? C853 C852 H852 . . . 119.7 ? C852 C853 C854 . . . 120.0(4) ? C852 C853 H853 . . . 120.0 ? C854 C853 H853 . . . 120.0 ? C853 C854 C855 . . . 120.0(4) ? C853 C854 H854 . . . 120.4 ? C855 C854 H854 . . . 119.6 ? C854 C855 C856 . . . 120.0(3) ? C854 C855 H855 . . . 119.7 ? C856 C855 H855 . . . 120.2 ? C851 C856 C855 . . . 121.2(4) ? C851 C856 H856 . . . 119.4 ? C855 C856 H856 . . . 119.5 ? La3 N91 N92 . . . 73.64(16) ? La3 N91 C95 . . . 170.9(2) ? N92 N91 C95 . . . 108.4(3) ? La3 N92 N91 . . . 73.76(16) ? La3 N92 C93 . . . 171.8(2) ? N91 N92 C93 . . . 108.0(3) ? N92 C93 C931 . . . 122.0(3) ? N92 C93 C94 . . . 109.0(3) ? C931 C93 C94 . . . 128.9(3) ? C93 C931 C932 . . . 122.4(3) ? C93 C931 C936 . . . 120.0(3) ? C932 C931 C936 . . . 117.6(3) ? C931 C932 C933 . . . 120.6(3) ? C931 C932 H932 . . . 119.7 ? C933 C932 H932 . . . 119.8 ? C932 C933 C934 . . . 121.3(4) ? C932 C933 H933 . . . 119.4 ? C934 C933 H933 . . . 119.3 ? C933 C934 C935 . . . 118.8(4) ? C933 C934 H934 . . . 120.4 ? C935 C934 H934 . . . 120.8 ? C934 C935 C936 . . . 120.4(3) ? C934 C935 H935 . . . 119.6 ? C936 C935 H935 . . . 120.1 ? C931 C936 C935 . . . 121.3(4) ? C931 C936 H936 . . . 119.2 ? C935 C936 H936 . . . 119.5 ? C93 C94 C95 . . . 105.7(3) ? C93 C94 H94 . . . 127.3 ? C95 C94 H94 . . . 127.0 ? N91 C95 C94 . . . 108.8(3) ? N91 C95 C951 . . . 123.1(3) ? C94 C95 C951 . . . 128.0(3) ? C95 C951 C952 . . . 122.1(3) ? C95 C951 C956 . . . 119.3(3) ? C952 C951 C956 . . . 118.6(3) ? C951 C952 C953 . . . 120.4(4) ? C951 C952 H952 . . . 119.4 ? C953 C952 H952 . . . 120.2 ? C952 C953 C954 . . . 121.1(4) ? C952 C953 H953 . . . 119.7 ? C954 C953 H953 . . . 119.3 ? C953 C954 C955 . . . 118.5(4) ? C953 C954 H954 . . . 121.2 ? C955 C954 H954 . . . 120.3 ? C954 C955 C956 . . . 121.2(4) ? C954 C955 H955 . . . 119.8 ? C956 C955 H955 . . . 119.0 ? C951 C956 C955 . . . 120.2(4) ? C951 C956 H956 . . . 119.5 ? C955 C956 H956 . . . 120.3 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 4824 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min -39 _reflns_limit_l_max 38 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 11.784 _diffrn_reflns_av_sigmaI/netI .074 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .058 _refine_ls_wR_factor_all .045 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_ag79b3 _database_code_depnum_ccdc_archive 'CCDC 190714' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C135 H99 N18 Nd3' _chemical_formula_moiety ? _chemical_formula_weight 2406.12 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 19.0940(10) _cell_length_b 20.0330(10) _cell_length_c 28.573(2) _cell_angle_alpha 90.00000 _cell_angle_beta 99.7650(10) _cell_angle_gamma 90.00000 _cell_volume 10771.1(11) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.488 _exptl_crystal_description plate _exptl_crystal_size_max .45 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour pale_blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.901 _diffrn_reflns_number 103792 _reflns_number_total 27157 _reflns_Friedel_coverage 0 _reflns_number_gt 22183 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.18 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .042 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .045 _refine_ls_wR_factor_ref .062 _refine_ls_goodness_of_fit_ref 1.569 _refine_ls_number_reflns 22183 _refine_ls_number_parameters 1407 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .023 _refine_diff_density_min -1.221 _refine_diff_density_max 2.193 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 540 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 396 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 72 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Nd ? 0 12 -.535 3.018 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nd1 .844070(13) .819436(12) .244496(9) .02152(11) Uani ? ? 1.00000 ? ? Nd2 .987556(13) .712083(12) .190397(9) .02113(11) Uani ? ? 1.00000 ? ? Nd3 1.150003(12) .596245(12) .238225(9) .02005(11) Uani ? ? 1.00000 ? ? N11 .7320(2) .8363(2) .26772(15) .0250(19) Uani ? ? 1.00000 ? ? N12 .7144(2) .8315(2) .21910(15) .0247(19) Uani ? ? 1.00000 ? ? C13 .6429(2) .8308(2) .20805(18) .025(2) Uani ? ? 1.00000 ? ? C131 .6039(3) .8230(2) .15911(18) .028(2) Uani ? ? 1.00000 ? ? C132 .6261(3) .8522(3) .1203(2) .036(3) Uani ? ? 1.00000 ? ? C133 .5882(3) .8430(3) .0743(2) .042(3) Uani ? ? 1.00000 ? ? C134 .5260(3) .8058(3) .0679(2) .046(3) Uani ? ? 1.00000 ? ? C135 .5030(3) .7764(3) .1062(2) .047(3) Uani ? ? 1.00000 ? ? C136 .5410(3) .7846(3) .1513(2) .039(3) Uani ? ? 1.00000 ? ? C14 .6136(2) .8367(2) .24924(19) .027(2) Uani ? ? 1.00000 ? ? C15 .6713(2) .8395(2) .28594(19) .027(2) Uani ? ? 1.00000 ? ? C151 .6744(3) .8439(3) .3374(2) .034(3) Uani ? ? 1.00000 ? ? C152 .7376(3) .8601(4) .3677(2) .046(3) Uani ? ? 1.00000 ? ? C153 .7416(4) .8608(5) .4156(2) .064(4) Uani ? ? 1.00000 ? ? C154 .6825(4) .8447(5) .4354(2) .066(5) Uani ? ? 1.00000 ? ? C155 .6186(4) .8299(4) .4069(2) .061(4) Uani ? ? 1.00000 ? ? C156 .6137(3) .8303(3) .3580(2) .042(3) Uani ? ? 1.00000 ? ? N21 .8965(2) .8933(2) .30788(16) .029(2) Uani ? ? 1.00000 ? ? N22 .8813(2) .9313(2) .26679(15) .027(2) Uani ? ? 1.00000 ? ? C23 .9075(3) .9931(2) .2764(2) .032(2) Uani ? ? 1.00000 ? ? C231 .8978(3) 1.0460(2) .2404(2) .030(2) Uani ? ? 1.00000 ? ? C232 .8670(3) 1.0311(3) .1933(2) .033(3) Uani ? ? 1.00000 ? ? C233 .8575(3) 1.0808(3) .1588(2) .041(3) Uani ? ? 1.00000 ? ? C234 .8780(3) 1.1462(3) .1708(2) .043(3) Uani ? ? 1.00000 ? ? C235 .9071(3) 1.1612(3) .2161(3) .044(3) Uani ? ? 1.00000 ? ? C236 .9175(3) 1.1114(3) .2517(2) .038(3) Uani ? ? 1.00000 ? ? C24 .9387(3) .9958(3) .3239(2) .037(3) Uani ? ? 1.00000 ? ? C25 .9315(3) .9323(3) .3427(2) .034(3) Uani ? ? 1.00000 ? ? C251 .9551(3) .9071(3) .3914(2) .037(3) Uani ? ? 1.00000 ? ? C252 .9299(3) .8482(3) .4062(2) .044(3) Uani ? ? 1.00000 ? ? C253 .9506(4) .8251(4) .4529(2) .052(4) Uani ? ? 1.00000 ? ? C254 .9971(3) .8613(4) .4844(2) .054(4) Uani ? ? 1.00000 ? ? C255 1.0241(4) .9202(5) .4688(3) .075(5) Uani ? ? 1.00000 ? ? C256 1.0034(4) .9440(4) .4229(3) .062(4) Uani ? ? 1.00000 ? ? N31 .9118(2) .8386(2) .17760(16) .028(2) Uani ? ? 1.00000 ? ? N32 .9666(2) .8317(2) .21650(15) .026(2) Uani ? ? 1.00000 ? ? C332 1.0795(3) .8817(3) .2951(2) .036(3) Uani ? ? 1.00000 ? ? C333 1.1399(3) .8941(3) .3285(2) .046(3) Uani ? ? 1.00000 ? ? C334 1.2040(3) .9083(3) .3150(3) .046(3) Uani ? ? 1.00000 ? ? C335 1.2074(3) .9123(3) .2669(3) .044(3) Uani ? ? 1.00000 ? ? C336 1.1481(3) .9006(3) .2326(2) .041(3) Uani ? ? 1.00000 ? ? C34 .9995(3) .9103(2) .1688(2) .031(2) Uani ? ? 1.00000 ? ? C35 .9322(3) .8867(2) .1491(2) .029(2) Uani ? ? 1.00000 ? ? C351 .8862(3) .9097(3) .1060(2) .034(3) Uani ? ? 1.00000 ? ? C352 .8130(3) .9009(3) .0999(2) .047(3) Uani ? ? 1.00000 ? ? C353 .7702(4) .9278(4) .0607(3) .063(4) Uani ? ? 1.00000 ? ? C354 .7992(4) .9642(4) .0279(2) .056(4) Uani ? ? 1.00000 ? ? C355 .8719(4) .9731(3) .0334(2) .048(3) Uani ? ? 1.00000 ? ? C356 .9152(3) .9464(3) .0723(2) .041(3) Uani ? ? 1.00000 ? ? C33 1.0188(2) .8760(2) .2107(2) .028(2) Uani ? ? 1.00000 ? ? C331 1.0832(3) .8849(2) .2464(2) .031(2) Uani ? ? 1.00000 ? ? N41 .8701(2) .69908(19) .21404(15) .0257(19) Uani ? ? 1.00000 ? ? N42 .9034(2) .6999(2) .26091(17) .030(2) Uani ? ? 1.00000 ? ? C43 .8529(3) .6862(2) .2880(2) .029(2) Uani ? ? 1.00000 ? ? C431 .8678(3) .6783(3) .3401(2) .039(3) Uani ? ? 1.00000 ? ? C432 .9347(4) .6577(3) .3631(2) .051(3) Uani ? ? 1.00000 ? ? C433 .9457(4) .6449(4) .4112(3) .070(4) Uani ? ? 1.00000 ? ? C434 .8889(5) .6524(5) .4361(3) .088(6) Uani ? ? 1.00000 ? ? C435 .8239(5) .6743(5) .4143(3) .078(5) Uani ? ? 1.00000 ? ? C436 .8130(4) .6881(4) .3665(2) .054(4) Uani ? ? 1.00000 ? ? C44 .7867(3) .6777(2) .25850(19) .029(2) Uani ? ? 1.00000 ? ? C45 .8001(3) .6853(2) .21241(19) .027(2) Uani ? ? 1.00000 ? ? C451 .7512(3) .6837(2) .1661(2) .031(2) Uani ? ? 1.00000 ? ? C452 .7647(3) .7236(3) .1294(2) .033(3) Uani ? ? 1.00000 ? ? C453 .7186(3) .7236(3) .0862(2) .041(3) Uani ? ? 1.00000 ? ? C454 .6584(3) .6828(3) .0800(2) .045(3) Uani ? ? 1.00000 ? ? C455 .6466(3) .6417(3) .1168(2) .049(3) Uani ? ? 1.00000 ? ? C456 .6916(3) .6422(3) .1607(2) .038(3) Uani ? ? 1.00000 ? ? N51 .9357(2) .6957(2) .10867(16) .034(2) Uani ? ? 1.00000 ? ? N52 .9924(2) .7392(2) .10922(16) .032(2) Uani ? ? 1.00000 ? ? C53 .9956(3) .7556(3) .0634(2) .041(3) Uani ? ? 1.00000 ? ? C531 1.0530(4) .7994(3) .0519(2) .049(3) Uani ? ? 1.00000 ? ? C532 1.0923(4) .8392(3) .0853(3) .058(4) Uani ? ? 1.00000 ? ? C533 1.1477(5) .8777(4) .0752(3) .073(5) Uani ? ? 1.00000 ? ? C534 1.1642(5) .8762(5) .0293(4) .092(6) Uani ? ? 1.00000 ? ? C535 1.1228(5) .8374(5) -.0049(3) .092(6) Uani ? ? 1.00000 ? ? C536 1.0682(5) .7977(5) .0054(3) .076(5) Uani ? ? 1.00000 ? ? C54 .9411(4) .7233(3) .0332(2) .048(3) Uani ? ? 1.00000 ? ? C55 .9049(3) .6851(3) .0626(2) .039(3) Uani ? ? 1.00000 ? ? C551 .8443(3) .6391(3) .0502(2) .045(3) Uani ? ? 1.00000 ? ? C552 .8274(3) .5929(3) .0823(2) .044(3) Uani ? ? 1.00000 ? ? C553 .7698(4) .5500(3) .0708(3) .055(4) Uani ? ? 1.00000 ? ? C554 .7286(4) .5535(4) .0270(3) .062(4) Uani ? ? 1.00000 ? ? C555 .7440(4) .5977(4) -.0054(3) .061(4) Uani ? ? 1.00000 ? ? C556 .8016(4) .6425(4) .0051(2) .054(4) Uani ? ? 1.00000 ? ? N61 1.0112(2) .5893(2) .20812(15) .0249(19) Uani ? ? 1.00000 ? ? N62 1.0482(2) .5902(2) .16955(15) .027(2) Uani ? ? 1.00000 ? ? C63 1.0186(3) .5424(2) .13872(19) .030(2) Uani ? ? 1.00000 ? ? C631 1.0450(3) .5324(3) .0939(2) .035(3) Uani ? ? 1.00000 ? ? C632 1.0686(3) .5861(3) .0698(2) .040(3) Uani ? ? 1.00000 ? ? C633 1.0947(4) .5759(4) .0285(2) .054(4) Uani ? ? 1.00000 ? ? C634 1.0969(3) .5112(4) .0099(2) .057(4) Uani ? ? 1.00000 ? ? C635 1.0727(4) .4584(4) .0329(2) .054(4) Uani ? ? 1.00000 ? ? C636 1.0460(3) .4684(3) .0742(2) .046(3) Uani ? ? 1.00000 ? ? C64 .9634(3) .5113(3) .1558(2) .035(3) Uani ? ? 1.00000 ? ? C65 .9604(2) .5414(2) .1989(2) .030(2) Uani ? ? 1.00000 ? ? C651 .9099(3) .5282(2) .2318(2) .032(2) Uani ? ? 1.00000 ? ? C652 .9309(3) .5301(3) .2801(2) .039(3) Uani ? ? 1.00000 ? ? C653 .8833(3) .5152(3) .3106(3) .048(3) Uani ? ? 1.00000 ? ? C654 .8139(3) .4988(3) .2919(3) .056(4) Uani ? ? 1.00000 ? ? C655 .7913(3) .4980(3) .2434(3) .052(4) Uani ? ? 1.00000 ? ? C656 .8392(3) .5115(3) .2134(3) .046(3) Uani ? ? 1.00000 ? ? N71 1.1009(2) .7167(2) .25543(14) .0232(18) Uani ? ? 1.00000 ? ? N72 1.1177(2) .72271(18) .21015(14) .0228(18) Uani ? ? 1.00000 ? ? C73 1.1887(2) .7349(2) .21408(19) .027(2) Uani ? ? 1.00000 ? ? C731 1.2213(3) .7429(2) .17102(18) .027(2) Uani ? ? 1.00000 ? ? C732 1.1949(3) .7085(3) .1300(2) .035(3) Uani ? ? 1.00000 ? ? C733 1.2260(3) .7164(3) .0893(2) .041(3) Uani ? ? 1.00000 ? ? C734 1.2811(3) .7587(3) .0901(2) .043(3) Uani ? ? 1.00000 ? ? C735 1.3081(3) .7937(4) .1297(2) .051(4) Uani ? ? 1.00000 ? ? C736 1.2782(3) .7872(3) .1709(2) .045(3) Uani ? ? 1.00000 ? ? C74 1.2185(2) .7358(2) .26170(19) .027(2) Uani ? ? 1.00000 ? ? C75 1.1622(3) .7256(2) .28678(18) .026(2) Uani ? ? 1.00000 ? ? C751 1.1640(3) .7253(3) .33867(18) .030(2) Uani ? ? 1.00000 ? ? C752 1.1029(3) .7373(3) .3577(2) .041(3) Uani ? ? 1.00000 ? ? C753 1.1044(4) .7432(3) .4057(2) .051(4) Uani ? ? 1.00000 ? ? C754 1.1680(4) .7362(4) .4363(2) .058(4) Uani ? ? 1.00000 ? ? C755 1.2296(4) .7223(4) .4180(2) .056(4) Uani ? ? 1.00000 ? ? C756 1.2278(3) .7168(3) .3695(2) .043(3) Uani ? ? 1.00000 ? ? N81 1.2744(2) .5781(2) .26214(15) .0255(19) Uani ? ? 1.00000 ? ? N82 1.2627(2) .5800(2) .21306(14) .0243(18) Uani ? ? 1.00000 ? ? C83 1.3268(2) .5785(2) .19837(17) .024(2) Uani ? ? 1.00000 ? ? C831 1.3343(3) .5811(2) .14847(18) .029(2) Uani ? ? 1.00000 ? ? C832 1.2810(3) .5582(3) .1125(2) .035(3) Uani ? ? 1.00000 ? ? C833 1.2896(3) .5605(3) .0655(2) .040(3) Uani ? ? 1.00000 ? ? C834 1.3522(3) .5867(3) .0530(2) .038(3) Uani ? ? 1.00000 ? ? C835 1.4046(3) .6101(3) .0886(2) .039(3) Uani ? ? 1.00000 ? ? C836 1.3961(3) .6074(3) .1354(2) .034(3) Uani ? ? 1.00000 ? ? C84 1.3801(2) .5761(2) .23870(18) .027(2) Uani ? ? 1.00000 ? ? C85 1.3453(2) .5756(2) .27789(18) .025(2) Uani ? ? 1.00000 ? ? C851 1.3733(3) .5758(2) .32815(18) .028(2) Uani ? ? 1.00000 ? ? C852 1.3293(3) .5687(4) .3619(2) .043(3) Uani ? ? 1.00000 ? ? C853 1.3560(4) .5741(5) .4095(2) .061(4) Uani ? ? 1.00000 ? ? C854 1.4282(3) .5842(3) .4252(2) .045(3) Uani ? ? 1.00000 ? ? C855 1.4728(3) .5901(3) .3928(2) .037(3) Uani ? ? 1.00000 ? ? C856 1.4470(3) .5850(3) .34458(19) .029(2) Uani ? ? 1.00000 ? ? N91 1.1240(2) .5166(2) .29645(14) .0250(19) Uani ? ? 1.00000 ? ? N92 1.1215(2) .4820(2) .25404(15) .0247(19) Uani ? ? 1.00000 ? ? C93 1.0970(2) .4203(2) .25922(18) .026(2) Uani ? ? 1.00000 ? ? C931 1.0920(2) .3687(2) .22241(19) .027(2) Uani ? ? 1.00000 ? ? C932 1.1074(3) .3823(3) .1771(2) .033(3) Uani ? ? 1.00000 ? ? C933 1.1057(3) .3316(3) .1439(2) .038(3) Uani ? ? 1.00000 ? ? C934 1.0888(3) .2671(3) .1544(2) .038(3) Uani ? ? 1.00000 ? ? C935 1.0731(3) .2525(3) .1987(2) .040(3) Uani ? ? 1.00000 ? ? C936 1.0755(3) .3022(3) .2328(2) .032(3) Uani ? ? 1.00000 ? ? C94 1.0806(3) .4143(3) .30517(19) .031(2) Uani ? ? 1.00000 ? ? C95 1.0992(3) .4758(2) .32729(18) .028(2) Uani ? ? 1.00000 ? ? C951 1.0963(3) .4954(2) .37652(18) .028(2) Uani ? ? 1.00000 ? ? C952 1.1345(3) .5488(3) .3987(2) .036(3) Uani ? ? 1.00000 ? ? C953 1.1343(3) .5627(3) .4460(2) .042(3) Uani ? ? 1.00000 ? ? C954 1.0951(3) .5231(3) .4719(2) .045(3) Uani ? ? 1.00000 ? ? C955 1.0551(4) .4710(3) .4500(2) .046(3) Uani ? ? 1.00000 ? ? C956 1.0550(3) .4578(3) .4031(2) .040(3) Uani ? ? 1.00000 ? ? H132 .66828 .87874 .12474 .04300 Uiso ? ? 1.00000 ? ? H133 .60522 .86237 .04787 .05500 Uiso ? ? 1.00000 ? ? H134 .49919 .79995 .03625 .05900 Uiso ? ? 1.00000 ? ? H135 .45902 .75078 .10097 .05800 Uiso ? ? 1.00000 ? ? H136 .52510 .76398 .17789 .04900 Uiso ? ? 1.00000 ? ? H14 .56417 .83810 .25198 .03500 Uiso ? ? 1.00000 ? ? H152 .77889 .87141 .35395 .05800 Uiso ? ? 1.00000 ? ? H153 .78589 .87243 .43596 .07900 Uiso ? ? 1.00000 ? ? H154 .68572 .84287 .46931 .08200 Uiso ? ? 1.00000 ? ? H155 .57746 .81993 .42116 .07400 Uiso ? ? 1.00000 ? ? H156 .56914 .82125 .33766 .05200 Uiso ? ? 1.00000 ? ? H232 .85265 .98657 .18532 .04200 Uiso ? ? 1.00000 ? ? H233 .83686 1.06970 .12650 .05300 Uiso ? ? 1.00000 ? ? H234 .87048 1.18069 .14680 .05600 Uiso ? ? 1.00000 ? ? H235 .92110 1.20620 .22455 .05500 Uiso ? ? 1.00000 ? ? H236 .93886 1.12295 .28377 .04700 Uiso ? ? 1.00000 ? ? H24 .96160 1.03384 .34090 .04700 Uiso ? ? 1.00000 ? ? H252 .89737 .82168 .38447 .05600 Uiso ? ? 1.00000 ? ? H253 .93112 .78407 .46292 .06700 Uiso ? ? 1.00000 ? ? H254 1.01187 .84649 .51650 .06900 Uiso ? ? 1.00000 ? ? H255 1.05786 .94564 .49097 .09000 Uiso ? ? 1.00000 ? ? H256 1.02367 .98501 .41289 .07700 Uiso ? ? 1.00000 ? ? H332 1.03598 .87018 .30499 .04500 Uiso ? ? 1.00000 ? ? H333 1.13652 .89295 .36197 .05800 Uiso ? ? 1.00000 ? ? H334 1.24584 .91550 .33783 .05800 Uiso ? ? 1.00000 ? ? H335 1.25205 .92299 .25744 .05600 Uiso ? ? 1.00000 ? ? H336 1.15108 .90380 .19945 .05200 Uiso ? ? 1.00000 ? ? H34 1.02704 .94326 .15557 .03800 Uiso ? ? 1.00000 ? ? H352 .79266 .87569 .12270 .05900 Uiso ? ? 1.00000 ? ? H353 .71977 .92104 .05627 .07300 Uiso ? ? 1.00000 ? ? H354 .76918 .98388 .00105 .06900 Uiso ? ? 1.00000 ? ? H355 .89192 .99742 .00992 .06000 Uiso ? ? 1.00000 ? ? H356 .96609 .95309 .07677 .05100 Uiso ? ? 1.00000 ? ? H432 .97327 .65371 .34543 .06700 Uiso ? ? 1.00000 ? ? H433 .99130 .63000 .42768 .08900 Uiso ? ? 1.00000 ? ? H434 .89652 .64166 .46987 .10500 Uiso ? ? 1.00000 ? ? H435 .78568 .68121 .43230 .09700 Uiso ? ? 1.00000 ? ? H436 .76747 .70413 .35058 .06800 Uiso ? ? 1.00000 ? ? H44 .74226 .66841 .26816 .03600 Uiso ? ? 1.00000 ? ? H452 .80591 .75196 .13359 .04200 Uiso ? ? 1.00000 ? ? H453 .72772 .75104 .06056 .05000 Uiso ? ? 1.00000 ? ? H454 .62599 .68305 .05063 .05600 Uiso ? ? 1.00000 ? ? H455 .60523 .61292 .11211 .06000 Uiso ? ? 1.00000 ? ? H456 .68215 .61473 .18656 .04900 Uiso ? ? 1.00000 ? ? H532 1.08166 .83992 .11795 .07000 Uiso ? ? 1.00000 ? ? H533 1.17603 .90558 .10040 .09500 Uiso ? ? 1.00000 ? ? H534 1.20319 .90254 .02143 .11100 Uiso ? ? 1.00000 ? ? H535 1.13379 .83751 -.03658 .11600 Uiso ? ? 1.00000 ? ? H536 1.04106 .76884 -.01853 .09600 Uiso ? ? 1.00000 ? ? H54 .93056 .72604 -.00072 .06100 Uiso ? ? 1.00000 ? ? H552 .85681 .59059 .11333 .05700 Uiso ? ? 1.00000 ? ? H553 .75949 .51741 .09427 .07200 Uiso ? ? 1.00000 ? ? H554 .68796 .52403 .01903 .07600 Uiso ? ? 1.00000 ? ? H555 .71519 .59870 -.03629 .07600 Uiso ? ? 1.00000 ? ? H556 .81126 .67492 -.01769 .06800 Uiso ? ? 1.00000 ? ? H632 1.06727 .62992 .08312 .05300 Uiso ? ? 1.00000 ? ? H633 1.11076 .61390 .01159 .06600 Uiso ? ? 1.00000 ? ? H634 1.11575 .50445 -.01879 .07000 Uiso ? ? 1.00000 ? ? H635 1.07434 .41439 .01990 .06900 Uiso ? ? 1.00000 ? ? H636 1.02767 .43097 .08978 .05800 Uiso ? ? 1.00000 ? ? H64 .93379 .47549 .14123 .04200 Uiso ? ? 1.00000 ? ? H652 .97930 .54163 .29325 .05000 Uiso ? ? 1.00000 ? ? H653 .89919 .51577 .34509 .06000 Uiso ? ? 1.00000 ? ? H654 .78107 .48819 .31296 .06700 Uiso ? ? 1.00000 ? ? H655 .74275 .48808 .23147 .06500 Uiso ? ? 1.00000 ? ? H656 .82367 .51010 .17922 .05600 Uiso ? ? 1.00000 ? ? H732 1.15515 .67913 .12930 .04400 Uiso ? ? 1.00000 ? ? H733 1.20706 .69255 .06107 .05000 Uiso ? ? 1.00000 ? ? H734 1.30232 .76385 .06178 .05300 Uiso ? ? 1.00000 ? ? H735 1.34811 .82325 .13004 .06400 Uiso ? ? 1.00000 ? ? H736 1.29645 .81218 .19897 .05600 Uiso ? ? 1.00000 ? ? H74 1.26773 .74150 .27505 .03400 Uiso ? ? 1.00000 ? ? H752 1.05800 .74109 .33615 .05100 Uiso ? ? 1.00000 ? ? H753 1.06214 .75220 .41839 .06500 Uiso ? ? 1.00000 ? ? H754 1.16991 .74161 .47001 .07200 Uiso ? ? 1.00000 ? ? H755 1.27384 .71596 .43982 .07100 Uiso ? ? 1.00000 ? ? H756 1.27033 .70705 .35718 .05500 Uiso ? ? 1.00000 ? ? H832 1.23741 .54107 .12018 .04300 Uiso ? ? 1.00000 ? ? H833 1.25299 .54430 .04110 .05000 Uiso ? ? 1.00000 ? ? H834 1.35829 .58822 .02041 .04800 Uiso ? ? 1.00000 ? ? H835 1.44735 .62838 .08068 .05000 Uiso ? ? 1.00000 ? ? H836 1.43309 .62352 .15977 .04200 Uiso ? ? 1.00000 ? ? H84 1.43032 .57481 .23896 .03300 Uiso ? ? 1.00000 ? ? H852 1.27980 .55929 .35156 .05300 Uiso ? ? 1.00000 ? ? H853 1.32421 .57186 .43247 .07400 Uiso ? ? 1.00000 ? ? H854 1.44622 .58797 .45886 .05800 Uiso ? ? 1.00000 ? ? H855 1.52247 .59689 .40344 .04600 Uiso ? ? 1.00000 ? ? H856 1.47904 .58847 .32223 .03700 Uiso ? ? 1.00000 ? ? H932 1.11863 .42700 .16934 .04200 Uiso ? ? 1.00000 ? ? H933 1.11732 .34175 .11313 .05000 Uiso ? ? 1.00000 ? ? H934 1.08784 .23198 .13130 .05000 Uiso ? ? 1.00000 ? ? H935 1.06094 .20779 .20594 .04900 Uiso ? ? 1.00000 ? ? H936 1.06514 .29174 .26390 .04200 Uiso ? ? 1.00000 ? ? H94 1.06211 .37600 .31901 .03900 Uiso ? ? 1.00000 ? ? H952 1.16122 .57681 .38068 .04500 Uiso ? ? 1.00000 ? ? H953 1.16176 .59906 .46113 .05400 Uiso ? ? 1.00000 ? ? H954 1.09563 .53180 .50510 .05600 Uiso ? ? 1.00000 ? ? H955 1.02724 .44398 .46760 .05700 Uiso ? ? 1.00000 ? ? H956 1.02558 .42208 .38799 .05000 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nd1 .01723(12) .01774(12) .02986(14) .00010(9) .00476(9) -.00036(9) Nd2 .01786(12) .01944(12) .02599(13) .00078(9) .00344(9) -.00169(9) Nd3 .01656(11) .01812(12) .02571(13) -.00086(8) .00430(9) -.00026(9) N11 .021(2) .023(2) .031(2) -.0004(15) .0075(16) -.0017(16) N12 .0188(18) .024(2) .031(2) .0015(15) .0024(16) -.0019(16) C13 .019(2) .027(2) .030(3) .0019(17) .0033(18) .003(2) C131 .022(2) .026(2) .034(3) .0082(18) .003(2) -.004(2) C132 .026(3) .031(3) .049(3) .006(2) .005(2) .001(2) C133 .043(3) .047(3) .036(3) .012(3) .003(3) .002(3) C134 .042(3) .045(3) .045(3) .013(3) -.011(3) -.011(3) C135 .032(3) .043(3) .062(4) .000(2) -.003(3) -.022(3) C136 .030(3) .034(3) .052(4) .003(2) .002(2) -.009(3) C14 .021(2) .023(2) .041(3) .0025(18) .011(2) -.002(2) C15 .023(2) .021(2) .040(3) .0013(18) .013(2) -.000(2) C151 .039(3) .030(3) .034(3) .005(2) .012(2) -.000(2) C152 .036(3) .070(4) .033(3) .008(3) .005(2) -.003(3) C153 .053(4) .098(6) .039(4) .015(4) .004(3) -.004(4) C154 .071(5) .096(6) .037(4) .031(4) .024(3) .005(4) C155 .068(5) .078(5) .045(4) .023(4) .036(4) .012(4) C156 .038(3) .044(3) .048(4) .005(3) .021(3) -.004(3) N21 .020(2) .025(2) .041(3) -.0014(15) .0023(17) -.0037(18) N22 .024(2) .0193(19) .036(2) -.0007(15) .0044(17) -.0031(17) C23 .024(2) .021(2) .052(3) -.0020(18) .011(2) -.005(2) C231 .021(2) .024(2) .046(3) .0007(18) .010(2) -.004(2) C232 .029(3) .024(2) .048(3) -.001(2) .009(2) -.001(2) C233 .035(3) .031(3) .060(4) .003(2) .014(3) .005(3) C234 .036(3) .030(3) .068(4) .003(2) .020(3) .010(3) C235 .035(3) .023(3) .080(5) .005(2) .029(3) -.000(3) C236 .029(3) .023(2) .064(4) -.000(2) .013(3) -.008(2) C24 .028(3) .034(3) .049(3) -.004(2) .005(2) -.013(2) C25 .026(2) .033(3) .041(3) -.003(2) .001(2) -.010(2) C251 .029(3) .045(3) .036(3) .007(2) .002(2) -.011(2) C252 .033(3) .052(4) .043(3) .001(3) -.002(3) -.003(3) C253 .043(4) .069(5) .042(4) .010(3) .005(3) .005(3) C254 .042(3) .085(5) .036(3) .018(3) .005(3) -.006(3) C255 .064(5) .109(7) .044(4) -.009(5) -.014(4) -.022(4) C256 .058(4) .067(5) .054(4) -.013(4) -.010(3) -.010(4) N31 .026(2) .024(2) .037(2) -.0006(16) .0081(18) .0013(17) N32 .0201(19) .023(2) .037(2) -.0001(15) .0086(17) .0016(17) C332 .030(3) .029(3) .050(3) .001(2) .007(2) -.002(2) C333 .036(3) .041(3) .056(4) .002(2) -.002(3) -.005(3) C334 .025(3) .039(3) .070(4) .001(2) -.004(3) -.010(3) C335 .024(3) .027(3) .080(5) -.003(2) .010(3) -.000(3) C336 .026(3) .024(3) .074(4) -.002(2) .013(3) .005(3) C34 .030(3) .021(2) .046(3) -.0045(19) .013(2) .002(2) C35 .031(3) .016(2) .044(3) .0027(18) .014(2) .002(2) C351 .038(3) .031(3) .032(3) -.003(2) .006(2) -.001(2) C352 .040(3) .048(4) .048(4) -.012(3) -.004(3) .018(3) C353 .047(4) .080(5) .053(4) -.017(4) -.014(3) .022(4) C354 .056(4) .066(5) .042(4) -.007(3) -.004(3) .014(3) C355 .060(4) .048(4) .037(3) -.006(3) .009(3) .009(3) C356 .045(3) .042(3) .037(3) -.004(3) .014(3) .003(3) C33 .020(2) .021(2) .044(3) .0002(17) .012(2) -.003(2) C331 .020(2) .017(2) .055(3) .0009(17) .007(2) -.002(2) N41 .024(2) .0163(18) .038(2) .0026(15) .0077(17) .0008(16) N42 .020(2) .022(2) .046(3) .0023(15) -.0003(18) .0044(18) C43 .023(2) .017(2) .046(3) .0024(17) .005(2) .005(2) C431 .037(3) .031(3) .045(3) -.007(2) -.002(2) .009(2) C432 .047(4) .046(4) .054(4) -.000(3) -.008(3) .008(3) C433 .074(5) .059(5) .064(5) -.009(4) -.030(4) .015(4) C434 .096(7) .103(7) .057(5) -.037(6) -.009(5) .033(5) C435 .065(5) .121(8) .045(4) -.034(5) .002(4) .002(5) C436 .047(4) .068(5) .046(4) -.013(3) .002(3) .010(3) C44 .022(2) .028(2) .038(3) -.0012(19) .007(2) .001(2) C45 .024(2) .018(2) .038(3) -.0012(17) .008(2) .000(2) C451 .026(2) .025(2) .042(3) .0025(19) .009(2) -.007(2) C452 .033(3) .024(2) .043(3) .004(2) .003(2) -.005(2) C453 .051(4) .034(3) .037(3) .014(3) .003(3) -.004(2) C454 .041(3) .048(4) .043(3) .008(3) -.000(3) -.011(3) C455 .032(3) .057(4) .057(4) -.006(3) .003(3) -.015(3) C456 .027(3) .038(3) .048(3) -.001(2) .006(2) -.006(3) N51 .033(2) .038(2) .029(2) .0060(19) .0006(18) -.0063(19) N52 .037(2) .031(2) .030(2) .0096(19) .0084(19) .0022(18) C53 .048(3) .044(3) .034(3) .018(3) .015(3) .006(2) C531 .062(4) .045(3) .044(4) .023(3) .022(3) .020(3) C532 .067(5) .032(3) .086(5) .014(3) .044(4) .012(3) C533 .074(5) .050(4) .104(7) .016(4) .043(5) .029(4) C534 .075(6) .083(6) .131(8) .013(5) .054(6) .070(6) C535 .075(6) .126(8) .086(6) .026(6) .047(5) .070(6) C536 .066(5) .105(7) .063(5) .033(5) .028(4) .036(5) C54 .054(4) .056(4) .034(3) .026(3) .003(3) -.002(3) C55 .038(3) .048(3) .028(3) .016(3) -.004(2) -.010(2) C551 .039(3) .052(4) .039(3) .018(3) -.007(3) -.019(3) C552 .038(3) .043(3) .046(3) .010(3) -.004(3) -.017(3) C553 .046(4) .046(4) .070(5) .001(3) .000(3) -.025(3) C554 .054(4) .056(4) .070(5) .012(3) -.008(4) -.034(4) C555 .049(4) .072(5) .054(4) .013(3) -.019(3) -.028(4) C556 .048(4) .066(4) .041(4) .021(3) -.008(3) -.017(3) N61 .022(2) .022(2) .031(2) -.0028(15) .0051(16) -.0031(16) N62 .027(2) .022(2) .032(2) -.0018(16) .0050(17) -.0024(17) C63 .026(2) .026(2) .036(3) .0016(19) -.004(2) -.007(2) C631 .025(2) .039(3) .038(3) .004(2) -.003(2) -.007(2) C632 .036(3) .046(3) .037(3) -.002(2) .001(2) -.009(3) C633 .042(4) .075(5) .045(4) -.011(3) .008(3) -.008(3) C634 .040(3) .090(6) .039(3) .007(3) .001(3) -.026(4) C635 .051(4) .057(4) .051(4) .017(3) -.002(3) -.020(3) C636 .046(3) .045(3) .044(3) .010(3) -.004(3) -.013(3) C64 .025(2) .022(2) .056(4) .001(2) .000(2) -.006(2) C65 .018(2) .020(2) .049(3) -.0003(17) -.002(2) .002(2) C651 .023(2) .013(2) .062(4) -.0002(17) .013(2) -.002(2) C652 .028(3) .027(3) .064(4) -.001(2) .012(3) .009(3) C653 .042(3) .035(3) .071(5) .002(3) .023(3) .008(3) C654 .039(3) .026(3) .115(6) .003(2) .043(4) .011(3) C655 .028(3) .028(3) .103(6) -.007(2) .018(3) .001(3) C656 .023(3) .024(3) .087(5) .001(2) .003(3) -.005(3) N71 .0197(18) .023(2) .027(2) -.0014(15) .0024(15) -.0032(16) N72 .0208(18) .0187(18) .029(2) -.0040(14) .0039(16) -.0053(15) C73 .022(2) .017(2) .042(3) -.0041(17) .010(2) -.004(2) C731 .024(2) .024(2) .033(3) -.0015(18) .007(2) .001(2) C732 .033(3) .033(3) .039(3) -.007(2) .007(2) -.003(2) C733 .048(3) .040(3) .034(3) .005(3) .005(3) -.008(2) C734 .045(3) .050(4) .037(3) .002(3) .021(3) .001(3) C735 .039(3) .068(4) .051(4) -.023(3) .020(3) -.003(3) C736 .034(3) .057(4) .044(3) -.017(3) .012(3) -.015(3) C74 .021(2) .024(2) .037(3) -.0016(18) .002(2) -.002(2) C75 .025(2) .018(2) .035(3) -.0016(17) .004(2) -.0050(19) C751 .029(3) .032(3) .030(3) -.002(2) .003(2) -.007(2) C752 .047(3) .039(3) .039(3) -.001(3) .014(3) -.003(3) C753 .059(4) .051(4) .051(4) .006(3) .029(3) -.008(3) C754 .089(6) .054(4) .033(3) -.021(4) .013(3) -.009(3) C755 .060(4) .070(5) .034(3) -.019(4) -.005(3) -.008(3) C756 .037(3) .049(4) .039(3) -.011(3) -.001(2) -.002(3) N81 .023(2) .024(2) .031(2) .0025(15) .0079(16) .0046(16) N82 .0202(19) .025(2) .028(2) .0005(15) .0047(16) .0008(16) C83 .022(2) .020(2) .031(3) .0001(17) .0074(19) .0026(18) C831 .030(3) .026(2) .033(3) .006(2) .010(2) .000(2) C832 .029(3) .036(3) .039(3) .001(2) .006(2) -.004(2) C833 .042(3) .048(3) .031(3) .001(3) .007(2) -.008(3) C834 .043(3) .041(3) .031(3) .003(2) .012(2) .002(2) C835 .036(3) .045(3) .042(3) -.001(2) .021(3) .000(3) C836 .028(3) .042(3) .031(3) .002(2) .004(2) -.002(2) C84 .022(2) .025(2) .034(3) -.0001(18) .009(2) .003(2) C85 .021(2) .023(2) .031(3) -.0011(17) .0058(19) .0032(19) C851 .025(2) .023(2) .034(3) .0018(18) -.001(2) .004(2) C852 .026(3) .074(4) .031(3) .001(3) .006(2) .005(3) C853 .042(4) .105(6) .037(4) .001(4) .004(3) .006(4) C854 .040(3) .063(4) .031(3) .003(3) .001(2) .005(3) C855 .033(3) .037(3) .041(3) .001(2) .000(2) .002(2) C856 .024(2) .030(3) .035(3) .001(2) .006(2) .005(2) N91 .025(2) .022(2) .029(2) .0029(15) .0067(16) .0007(16) N92 .0207(19) .022(2) .033(2) .0011(15) .0082(16) -.0001(16) C93 .019(2) .021(2) .036(3) -.0004(17) .005(2) .004(2) C931 .020(2) .023(2) .039(3) .0015(18) .007(2) -.001(2) C932 .037(3) .025(2) .038(3) .000(2) .007(2) .000(2) C933 .044(3) .034(3) .039(3) .004(2) .013(3) -.003(2) C934 .033(3) .028(3) .052(4) .007(2) .003(2) -.013(2) C935 .031(3) .022(2) .069(4) -.001(2) .015(3) -.006(3) C936 .026(2) .027(2) .047(3) -.002(2) .011(2) -.003(2) C94 .030(3) .028(3) .033(3) -.004(2) .006(2) .004(2) C95 .026(2) .025(2) .031(3) -.0012(19) .004(2) -.001(2) C951 .022(2) .029(2) .034(3) -.0011(19) .006(2) .003(2) C952 .033(3) .036(3) .036(3) -.005(2) .003(2) .001(2) C953 .046(3) .041(3) .037(3) -.006(3) .005(3) -.007(3) C954 .049(4) .056(4) .031(3) -.010(3) .006(3) -.004(3) C955 .055(4) .052(4) .035(3) -.014(3) .014(3) .001(3) C956 .045(3) .046(3) .029(3) -.009(3) .009(2) -.002(2) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Nd1 N11 . . 2.370(4) ? Nd1 N12 . . 2.471(4) ? Nd1 N21 . . 2.421(4) ? Nd1 N22 . . 2.403(4) ? Nd1 N31 . . 2.513(5) ? Nd1 N32 . . 2.608(4) ? Nd1 N41 . . 2.639(4) ? Nd1 N42 . . 2.657(4) ? Nd1 C43 . . 2.937(5) ? Nd1 C45 . . 2.916(5) ? Nd2 N31 . . 2.910(4) ? Nd2 N32 . . 2.562(4) ? Nd2 N41 . . 2.463(4) ? Nd2 N42 . . 2.792(5) ? Nd2 N51 . . 2.399(4) ? Nd2 N52 . . 2.399(5) ? Nd2 N61 . . 2.536(4) ? Nd2 N62 . . 2.810(4) ? Nd2 N71 . . 2.604(4) ? Nd2 N72 . . 2.462(4) ? Nd3 N61 . . 2.647(4) ? Nd3 N62 . . 2.520(4) ? Nd3 N71 . . 2.664(4) ? Nd3 N72 . . 2.697(4) ? Nd3 C75 . . 2.930(5) ? Nd3 N81 . . 2.385(4) ? Nd3 N82 . . 2.403(4) ? Nd3 N91 . . 2.416(4) ? Nd3 N92 . . 2.412(4) ? N11 N12 . . 1.376(6) ? N11 C15 . . 1.350(7) ? N12 C13 . . 1.348(6) ? C13 C131 . . 1.477(7) ? C13 C14 . . 1.392(8) ? C131 C132 . . 1.382(8) ? C131 C136 . . 1.412(7) ? C132 C133 . . 1.399(8) ? C132 H132 . . .956 ? C133 C134 . . 1.389(9) ? C133 H133 . . .954 ? C134 C135 . . 1.377(10) ? C134 H134 . . .968 ? C135 C136 . . 1.379(9) ? C135 H135 . . .973 ? C136 H136 . . .959 ? C14 C15 . . 1.388(7) ? C14 H14 . . .960 ? C15 C151 . . 1.464(8) ? C151 C152 . . 1.398(8) ? C151 C156 . . 1.415(9) ? C152 C153 . . 1.357(9) ? C152 H152 . . .966 ? C153 C154 . . 1.386(12) ? C153 H153 . . .970 ? C154 C155 . . 1.379(10) ? C154 H154 . . .960 ? C155 C156 . . 1.385(10) ? C155 H155 . . .965 ? C156 H156 . . .962 ? N21 N22 . . 1.387(6) ? N21 C25 . . 1.350(7) ? N22 C23 . . 1.347(6) ? C23 C231 . . 1.467(7) ? C23 C24 . . 1.389(8) ? C231 C232 . . 1.404(8) ? C231 C236 . . 1.386(7) ? C232 C233 . . 1.391(8) ? C232 H232 . . .950 ? C233 C234 . . 1.395(8) ? C233 H233 . . .965 ? C234 C235 . . 1.355(9) ? C234 H234 . . .965 ? C235 C236 . . 1.415(9) ? C235 H235 . . .959 ? C236 H236 . . .965 ? C24 C25 . . 1.396(8) ? C24 H24 . . .968 ? C25 C251 . . 1.476(8) ? C251 C252 . . 1.369(9) ? C251 C256 . . 1.389(9) ? C252 C253 . . 1.402(9) ? C252 H252 . . .960 ? C253 C254 . . 1.363(9) ? C253 H253 . . .966 ? C254 C255 . . 1.389(12) ? C254 H254 . . .959 ? C255 C256 . . 1.390(11) ? C255 H255 . . .969 ? C256 H256 . . .971 ? N31 N32 . . 1.397(5) ? N31 C35 . . 1.361(7) ? N32 C33 . . 1.366(6) ? C332 C333 . . 1.390(8) ? C332 C331 . . 1.407(9) ? C332 H332 . . .949 ? C333 C334 . . 1.374(9) ? C333 H333 . . .969 ? C334 C335 . . 1.388(10) ? C334 H334 . . .952 ? C335 C336 . . 1.388(8) ? C335 H335 . . .962 ? C336 C331 . . 1.398(8) ? C336 H336 . . .960 ? C34 C35 . . 1.396(7) ? C34 C33 . . 1.376(7) ? C34 H34 . . .961 ? C35 C351 . . 1.459(7) ? C351 C352 . . 1.389(8) ? C351 C356 . . 1.399(9) ? C352 C353 . . 1.379(9) ? C352 H352 . . .959 ? C353 C354 . . 1.374(11) ? C353 H353 . . .960 ? C354 C355 . . 1.382(10) ? C354 H354 . . .961 ? C355 C356 . . 1.375(8) ? C355 H355 . . .960 ? C356 H356 . . .968 ? C33 C331 . . 1.469(7) ? N41 N42 . . 1.382(6) ? N41 C45 . . 1.358(6) ? N42 C43 . . 1.363(7) ? C43 C431 . . 1.476(8) ? C43 C44 . . 1.406(7) ? C431 C432 . . 1.396(8) ? C431 C436 . . 1.403(10) ? C432 C433 . . 1.377(11) ? C432 H432 . . .965 ? C433 C434 . . 1.402(14) ? C433 H433 . . .965 ? C434 C435 . . 1.365(13) ? C434 H434 . . .974 ? C435 C436 . . 1.374(11) ? C435 H435 . . .972 ? C436 H436 . . .965 ? C44 C45 . . 1.392(8) ? C44 H44 . . .954 ? C45 C451 . . 1.485(7) ? C451 C452 . . 1.375(8) ? C451 C456 . . 1.397(7) ? C452 C453 . . 1.389(8) ? C452 H452 . . .962 ? C453 C454 . . 1.398(9) ? C453 H453 . . .956 ? C454 C455 . . 1.383(10) ? C454 H454 . . .955 ? C455 C456 . . 1.394(8) ? C455 H455 . . .969 ? C456 H456 . . .963 ? N51 N52 . . 1.388(6) ? N51 C55 . . 1.363(7) ? N52 C53 . . 1.360(8) ? C53 C531 . . 1.485(10) ? C53 C54 . . 1.394(8) ? C531 C532 . . 1.367(9) ? C531 C536 . . 1.406(11) ? C532 C533 . . 1.380(12) ? C532 H532 . . .987 ? C533 C534 . . 1.400(15) ? C533 H533 . . .995 ? C534 C535 . . 1.386(14) ? C534 H534 . . .969 ? C535 C536 . . 1.382(14) ? C535 H535 . . .963 ? C536 H536 . . .976 ? C54 C55 . . 1.403(9) ? C54 H54 . . .957 ? C55 C551 . . 1.475(8) ? C551 C552 . . 1.378(9) ? C551 C556 . . 1.403(8) ? C552 C553 . . 1.392(9) ? C552 H552 . . .967 ? C553 C554 . . 1.362(10) ? C553 H553 . . .980 ? C554 C555 . . 1.349(11) ? C554 H554 . . .970 ? C555 C556 . . 1.411(10) ? C555 H555 . . .959 ? C556 H556 . . .961 ? N61 N62 . . 1.406(6) ? N61 C65 . . 1.358(6) ? N62 C63 . . 1.357(6) ? C63 C631 . . 1.468(8) ? C63 C64 . . 1.384(8) ? C631 C632 . . 1.393(9) ? C631 C636 . . 1.401(9) ? C632 C633 . . 1.371(10) ? C632 H632 . . .959 ? C633 C634 . . 1.405(11) ? C633 H633 . . .978 ? C634 C635 . . 1.366(11) ? C634 H634 . . .960 ? C635 C636 . . 1.377(10) ? C635 H635 . . .959 ? C636 H636 . . .968 ? C64 C65 . . 1.379(8) ? C64 H64 . . .963 ? C65 C651 . . 1.479(8) ? C651 C652 . . 1.371(9) ? C651 C656 . . 1.404(7) ? C652 C653 . . 1.396(10) ? C652 H652 . . .965 ? C653 C654 . . 1.382(9) ? C653 H653 . . .980 ? C654 C655 . . 1.379(12) ? C654 H654 . . .963 ? C655 C656 . . 1.384(10) ? C655 H655 . . .952 ? C656 H656 . . .971 ? N71 N72 . . 1.390(6) ? N71 C75 . . 1.359(6) ? N72 C73 . . 1.363(6) ? C73 C731 . . 1.479(8) ? C73 C74 . . 1.383(7) ? C731 C732 . . 1.380(7) ? C731 C736 . . 1.403(8) ? C732 C733 . . 1.402(9) ? C732 H732 . . .957 ? C733 C734 . . 1.347(9) ? C733 H733 . . .955 ? C734 C735 . . 1.355(9) ? C734 H734 . . .971 ? C735 C736 . . 1.399(10) ? C735 H735 . . .965 ? C736 H736 . . .960 ? C74 C75 . . 1.404(8) ? C74 H74 . . .960 ? C75 C751 . . 1.477(7) ? C751 C752 . . 1.390(9) ? C751 C756 . . 1.387(7) ? C752 C753 . . 1.372(9) ? C752 H752 . . .970 ? C753 C754 . . 1.376(10) ? C753 H753 . . .956 ? C754 C755 . . 1.394(12) ? C754 H754 . . .965 ? C755 C756 . . 1.385(9) ? C755 H755 . . .969 ? C756 H756 . . .959 ? N81 N82 . . 1.383(6) ? N81 C85 . . 1.353(6) ? N82 C83 . . 1.360(6) ? C83 C831 . . 1.458(7) ? C83 C84 . . 1.404(6) ? C831 C832 . . 1.396(7) ? C831 C836 . . 1.401(8) ? C832 C833 . . 1.381(8) ? C832 H832 . . .959 ? C833 C834 . . 1.407(9) ? C833 H833 . . .956 ? C834 C835 . . 1.381(8) ? C834 H834 . . .959 ? C835 C836 . . 1.375(8) ? C835 H835 . . .955 ? C836 H836 . . .960 ? C84 C85 . . 1.396(8) ? C84 H84 . . .957 ? C85 C851 . . 1.445(7) ? C851 C852 . . 1.391(8) ? C851 C856 . . 1.418(7) ? C852 C853 . . 1.373(9) ? C852 H852 . . .960 ? C853 C854 . . 1.390(9) ? C853 H853 . . .967 ? C854 C855 . . 1.367(9) ? C854 H854 . . .967 ? C855 C856 . . 1.385(8) ? C855 H855 . . .956 ? C856 H856 . . .958 ? N91 N92 . . 1.389(6) ? N91 C95 . . 1.346(7) ? N92 C93 . . 1.338(6) ? C93 C931 . . 1.467(7) ? C93 C94 . . 1.406(8) ? C931 C932 . . 1.402(8) ? C931 C936 . . 1.411(7) ? C932 C933 . . 1.388(8) ? C932 H932 . . .955 ? C933 C934 . . 1.377(8) ? C933 H933 . . .963 ? C934 C935 . . 1.381(9) ? C934 H934 . . .962 ? C935 C936 . . 1.389(8) ? C935 H935 . . .957 ? C936 H936 . . .966 ? C94 C95 . . 1.403(7) ? C94 H94 . . .957 ? C95 C951 . . 1.471(7) ? C951 C952 . . 1.386(7) ? C951 C956 . . 1.402(8) ? C952 C953 . . 1.380(8) ? C952 H952 . . .964 ? C953 C954 . . 1.388(9) ? C953 H953 . . .958 ? C954 C955 . . 1.380(9) ? C954 H954 . . .961 ? C955 C956 . . 1.366(9) ? C955 H955 . . .959 ? C956 H956 . . .965 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Nd1 N12 . . . 32.96(14) ? N11 Nd1 N21 . . . 88.96(14) ? N11 Nd1 N22 . . . 91.88(14) ? N11 Nd1 N31 . . . 142.86(13) ? N11 Nd1 N32 . . . 166.30(13) ? N11 Nd1 N41 . . . 116.91(13) ? N11 Nd1 N42 . . . 117.24(14) ? N11 Nd1 C43 . . . 90.07(14) ? N11 Nd1 C45 . . . 89.67(14) ? N12 Nd1 N21 . . . 115.26(14) ? N12 Nd1 N22 . . . 102.87(13) ? N12 Nd1 N31 . . . 112.40(13) ? N12 Nd1 N32 . . . 143.75(13) ? N12 Nd1 N41 . . . 103.19(12) ? N12 Nd1 N42 . . . 121.09(12) ? N12 Nd1 C43 . . . 101.31(13) ? N12 Nd1 C45 . . . 77.13(13) ? N21 Nd1 N22 . . . 33.42(14) ? N21 Nd1 N31 . . . 105.95(14) ? N21 Nd1 N32 . . . 83.86(14) ? N21 Nd1 N41 . . . 136.74(12) ? N21 Nd1 N42 . . . 108.01(13) ? N21 Nd1 C43 . . . 104.63(14) ? N21 Nd1 C45 . . . 149.23(14) ? N22 Nd1 N31 . . . 83.82(14) ? N22 Nd1 N32 . . . 75.73(14) ? N22 Nd1 N41 . . . 151.08(13) ? N22 Nd1 N42 . . . 134.06(12) ? N22 Nd1 C43 . . . 137.90(14) ? N22 Nd1 C45 . . . 177.01(15) ? N31 Nd1 N32 . . . 31.60(13) ? N31 Nd1 N41 . . . 74.83(13) ? N31 Nd1 N42 . . . 90.72(14) ? N31 Nd1 C43 . . . 117.42(14) ? N31 Nd1 C45 . . . 93.40(14) ? N32 Nd1 N41 . . . 75.87(13) ? N32 Nd1 N42 . . . 76.19(13) ? N32 Nd1 C43 . . . 103.01(13) ? N32 Nd1 C45 . . . 102.46(14) ? N41 Nd1 N42 . . . 30.25(13) ? N41 Nd1 C43 . . . 46.27(15) ? N41 Nd1 C45 . . . 27.74(13) ? N42 Nd1 C43 . . . 27.62(15) ? N42 Nd1 C45 . . . 46.88(12) ? C43 Nd1 C45 . . . 44.63(14) ? N31 Nd2 N32 . . . 28.70(12) ? N31 Nd2 N41 . . . 70.76(12) ? N31 Nd2 N42 . . . 80.35(12) ? N31 Nd2 N51 . . . 83.27(14) ? N31 Nd2 N52 . . . 77.33(14) ? N31 Nd2 N61 . . . 159.65(12) ? N31 Nd2 N62 . . . 160.77(12) ? N31 Nd2 N71 . . . 113.20(11) ? N31 Nd2 N72 . . . 114.47(12) ? N32 Nd2 N41 . . . 79.88(13) ? N32 Nd2 N42 . . . 74.58(13) ? N32 Nd2 N51 . . . 110.64(14) ? N32 Nd2 N52 . . . 95.91(14) ? N32 Nd2 N61 . . . 151.70(14) ? N32 Nd2 N62 . . . 164.89(12) ? N32 Nd2 N71 . . . 84.91(12) ? N32 Nd2 N72 . . . 93.10(12) ? N41 Nd2 N42 . . . 29.65(12) ? N41 Nd2 N51 . . . 90.45(15) ? N41 Nd2 N52 . . . 118.36(14) ? N41 Nd2 N61 . . . 88.99(13) ? N41 Nd2 N62 . . . 113.16(12) ? N41 Nd2 N71 . . . 119.55(13) ? N41 Nd2 N72 . . . 151.23(13) ? N42 Nd2 N51 . . . 119.83(14) ? N42 Nd2 N52 . . . 146.97(13) ? N42 Nd2 N61 . . . 82.87(13) ? N42 Nd2 N62 . . . 112.66(12) ? N42 Nd2 N71 . . . 89.91(12) ? N42 Nd2 N72 . . . 121.59(13) ? N51 Nd2 N52 . . . 33.63(15) ? N51 Nd2 N61 . . . 95.25(14) ? N51 Nd2 N62 . . . 77.96(14) ? N51 Nd2 N71 . . . 148.77(15) ? N51 Nd2 N72 . . . 117.95(15) ? N52 Nd2 N61 . . . 112.22(14) ? N52 Nd2 N62 . . . 84.69(14) ? N52 Nd2 N71 . . . 121.22(14) ? N52 Nd2 N72 . . . 89.97(14) ? N61 Nd2 N62 . . . 29.95(13) ? N61 Nd2 N71 . . . 78.09(12) ? N61 Nd2 N72 . . . 84.23(12) ? N62 Nd2 N71 . . . 81.93(12) ? N62 Nd2 N72 . . . 71.80(12) ? N71 Nd2 N72 . . . 31.68(13) ? N61 Nd3 N62 . . . 31.47(14) ? N61 Nd3 N71 . . . 75.14(12) ? N61 Nd3 N72 . . . 77.69(11) ? N61 Nd3 C75 . . . 101.25(12) ? N61 Nd3 N81 . . . 168.06(13) ? N61 Nd3 N82 . . . 142.48(13) ? N61 Nd3 N91 . . . 82.99(12) ? N61 Nd3 N92 . . . 76.45(12) ? N62 Nd3 N71 . . . 86.47(12) ? N62 Nd3 N72 . . . 72.93(12) ? N62 Nd3 C75 . . . 113.60(13) ? N62 Nd3 N81 . . . 144.57(14) ? N62 Nd3 N82 . . . 111.82(14) ? N62 Nd3 N91 . . . 106.44(13) ? N62 Nd3 N92 . . . 86.05(13) ? N71 Nd3 N72 . . . 30.03(13) ? N71 Nd3 C75 . . . 27.61(12) ? N71 Nd3 N81 . . . 116.69(12) ? N71 Nd3 N82 . . . 122.59(13) ? N71 Nd3 N91 . . . 110.56(13) ? N71 Nd3 N92 . . . 136.61(14) ? N72 Nd3 C75 . . . 46.05(12) ? N72 Nd3 N81 . . . 113.23(12) ? N72 Nd3 N82 . . . 102.10(13) ? N72 Nd3 N91 . . . 139.60(13) ? N72 Nd3 N92 . . . 154.03(12) ? C75 Nd3 N81 . . . 90.20(13) ? C75 Nd3 N82 . . . 104.97(14) ? C75 Nd3 N91 . . . 105.48(14) ? C75 Nd3 N92 . . . 138.80(15) ? N81 Nd3 N82 . . . 33.57(14) ? N81 Nd3 N91 . . . 90.75(13) ? N81 Nd3 N92 . . . 92.73(13) ? N82 Nd3 N91 . . . 114.53(13) ? N82 Nd3 N92 . . . 99.76(14) ? N91 Nd3 N92 . . . 33.45(14) ? Nd1 N11 N12 . . . 77.6(3) ? Nd1 N11 C15 . . . 171.8(3) ? N12 N11 C15 . . . 108.3(4) ? Nd1 N12 N11 . . . 69.5(2) ? Nd1 N12 C13 . . . 172.9(3) ? N11 N12 C13 . . . 107.5(4) ? N12 C13 C131 . . . 123.4(5) ? N12 C13 C14 . . . 109.7(4) ? C131 C13 C14 . . . 126.8(4) ? C13 C131 C132 . . . 122.8(4) ? C13 C131 C136 . . . 119.1(5) ? C132 C131 C136 . . . 118.1(5) ? C131 C132 C133 . . . 121.2(5) ? C131 C132 H132 . . . 119.6 ? C133 C132 H132 . . . 119.2 ? C132 C133 C134 . . . 119.2(6) ? C132 C133 H133 . . . 119.9 ? C134 C133 H133 . . . 120.8 ? C133 C134 C135 . . . 120.4(6) ? C133 C134 H134 . . . 119.5 ? C135 C134 H134 . . . 120.1 ? C134 C135 C136 . . . 120.1(6) ? C134 C135 H135 . . . 119.2 ? C136 C135 H135 . . . 120.6 ? C131 C136 C135 . . . 120.8(6) ? C131 C136 H136 . . . 119.0 ? C135 C136 H136 . . . 120.1 ? C13 C14 C15 . . . 105.1(4) ? C13 C14 H14 . . . 127.8 ? C15 C14 H14 . . . 127.1 ? N11 C15 C14 . . . 109.3(5) ? N11 C15 C151 . . . 119.9(4) ? C14 C15 C151 . . . 130.8(5) ? C15 C151 C152 . . . 121.3(5) ? C15 C151 C156 . . . 120.7(5) ? C152 C151 C156 . . . 118.0(5) ? C151 C152 C153 . . . 121.5(6) ? C151 C152 H152 . . . 118.7 ? C153 C152 H152 . . . 119.8 ? C152 C153 C154 . . . 120.0(6) ? C152 C153 H153 . . . 120.2 ? C154 C153 H153 . . . 119.8 ? C153 C154 C155 . . . 120.6(7) ? C153 C154 H154 . . . 120.3 ? C155 C154 H154 . . . 119.1 ? C154 C155 C156 . . . 119.8(7) ? C154 C155 H155 . . . 119.8 ? C156 C155 H155 . . . 120.3 ? C151 C156 C155 . . . 120.1(6) ? C151 C156 H156 . . . 119.2 ? C155 C156 H156 . . . 120.7 ? Nd1 N21 N22 . . . 72.6(2) ? Nd1 N21 C25 . . . 174.9(4) ? N22 N21 C25 . . . 108.3(4) ? Nd1 N22 N21 . . . 74.0(2) ? Nd1 N22 C23 . . . 173.9(4) ? N21 N22 C23 . . . 108.3(4) ? N22 C23 C231 . . . 121.6(5) ? N22 C23 C24 . . . 108.5(5) ? C231 C23 C24 . . . 129.8(5) ? C23 C231 C232 . . . 120.0(4) ? C23 C231 C236 . . . 121.4(5) ? C232 C231 C236 . . . 118.6(5) ? C231 C232 C233 . . . 120.7(5) ? C231 C232 H232 . . . 119.1 ? C233 C232 H232 . . . 120.2 ? C232 C233 C234 . . . 120.0(6) ? C232 C233 H233 . . . 119.8 ? C234 C233 H233 . . . 120.1 ? C233 C234 C235 . . . 119.7(6) ? C233 C234 H234 . . . 119.8 ? C235 C234 H234 . . . 120.5 ? C234 C235 C236 . . . 121.1(5) ? C234 C235 H235 . . . 120.0 ? C236 C235 H235 . . . 118.9 ? C231 C236 C235 . . . 119.9(5) ? C231 C236 H236 . . . 120.2 ? C235 C236 H236 . . . 119.9 ? C23 C24 C25 . . . 106.7(5) ? C23 C24 H24 . . . 127.1 ? C25 C24 H24 . . . 126.2 ? N21 C25 C24 . . . 108.1(5) ? N21 C25 C251 . . . 122.1(5) ? C24 C25 C251 . . . 129.8(5) ? C25 C251 C252 . . . 121.3(5) ? C25 C251 C256 . . . 119.4(6) ? C252 C251 C256 . . . 119.3(6) ? C251 C252 C253 . . . 121.4(6) ? C251 C252 H252 . . . 119.9 ? C253 C252 H252 . . . 118.7 ? C252 C253 C254 . . . 120.0(7) ? C252 C253 H253 . . . 120.1 ? C254 C253 H253 . . . 119.8 ? C253 C254 C255 . . . 118.4(6) ? C253 C254 H254 . . . 121.3 ? C255 C254 H254 . . . 120.3 ? C254 C255 C256 . . . 122.2(7) ? C254 C255 H255 . . . 118.7 ? C256 C255 H255 . . . 119.1 ? C251 C256 C255 . . . 118.6(7) ? C251 C256 H256 . . . 120.9 ? C255 C256 H256 . . . 120.4 ? Nd1 N31 Nd2 . . . 94.62(13) ? Nd1 N31 N32 . . . 78.0(3) ? Nd1 N31 C35 . . . 143.1(3) ? Nd2 N31 N32 . . . 61.7(2) ? Nd2 N31 C35 . . . 120.4(3) ? N32 N31 C35 . . . 107.2(4) ? Nd1 N32 Nd2 . . . 101.18(14) ? Nd1 N32 N31 . . . 70.4(2) ? Nd1 N32 C33 . . . 144.1(3) ? Nd2 N32 N31 . . . 89.6(3) ? Nd2 N32 C33 . . . 114.7(3) ? N31 N32 C33 . . . 107.7(4) ? C333 C332 C331 . . . 119.7(5) ? C333 C332 H332 . . . 120.4 ? C331 C332 H332 . . . 119.9 ? C332 C333 C334 . . . 121.3(6) ? C332 C333 H333 . . . 119.0 ? C334 C333 H333 . . . 119.6 ? C333 C334 C335 . . . 118.9(5) ? C333 C334 H334 . . . 121.4 ? C335 C334 H334 . . . 119.7 ? C334 C335 C336 . . . 121.4(6) ? C334 C335 H335 . . . 118.9 ? C336 C335 H335 . . . 119.7 ? C335 C336 C331 . . . 119.6(6) ? C335 C336 H336 . . . 120.5 ? C331 C336 H336 . . . 119.9 ? C35 C34 C33 . . . 106.0(5) ? C35 C34 H34 . . . 126.9 ? C33 C34 H34 . . . 127.0 ? N31 C35 C34 . . . 109.5(4) ? N31 C35 C351 . . . 122.4(4) ? C34 C35 C351 . . . 128.0(5) ? C35 C351 C352 . . . 121.0(5) ? C35 C351 C356 . . . 119.6(5) ? C352 C351 C356 . . . 119.1(5) ? C351 C352 C353 . . . 119.9(6) ? C351 C352 H352 . . . 119.7 ? C353 C352 H352 . . . 120.3 ? C352 C353 C354 . . . 120.5(7) ? C352 C353 H353 . . . 119.7 ? C354 C353 H353 . . . 119.8 ? C353 C354 C355 . . . 120.2(6) ? C353 C354 H354 . . . 120.5 ? C355 C354 H354 . . . 119.3 ? C354 C355 C356 . . . 119.8(6) ? C354 C355 H355 . . . 119.8 ? C356 C355 H355 . . . 120.4 ? C351 C356 C355 . . . 120.4(6) ? C351 C356 H356 . . . 119.2 ? C355 C356 H356 . . . 120.3 ? N32 C33 C34 . . . 109.6(4) ? N32 C33 C331 . . . 122.5(5) ? C34 C33 C331 . . . 127.8(5) ? C332 C331 C336 . . . 119.1(5) ? C332 C331 C33 . . . 120.3(5) ? C336 C331 C33 . . . 120.5(5) ? Nd1 N41 Nd2 . . . 103.02(14) ? Nd1 N41 N42 . . . 75.6(2) ? Nd1 N41 C45 . . . 87.6(3) ? Nd2 N41 N42 . . . 88.5(3) ? Nd2 N41 C45 . . . 161.6(4) ? N42 N41 C45 . . . 108.9(4) ? Nd1 N42 Nd2 . . . 94.26(14) ? Nd1 N42 N41 . . . 74.2(2) ? Nd1 N42 C43 . . . 87.7(3) ? Nd2 N42 N41 . . . 61.8(3) ? Nd2 N42 C43 . . . 167.5(3) ? N41 N42 C43 . . . 107.1(4) ? Nd1 C43 N42 . . . 64.7(2) ? Nd1 C43 C431 . . . 120.7(3) ? Nd1 C43 C44 . . . 82.8(3) ? N42 C43 C431 . . . 124.0(4) ? N42 C43 C44 . . . 109.6(5) ? C431 C43 C44 . . . 126.3(5) ? C43 C431 C432 . . . 120.8(6) ? C43 C431 C436 . . . 119.6(5) ? C432 C431 C436 . . . 119.6(6) ? C431 C432 C433 . . . 119.8(7) ? C431 C432 H432 . . . 119.8 ? C433 C432 H432 . . . 120.4 ? C432 C433 C434 . . . 119.1(7) ? C432 C433 H433 . . . 121.2 ? C434 C433 H433 . . . 119.7 ? C433 C434 C435 . . . 121.5(8) ? C433 C434 H434 . . . 118.8 ? C435 C434 H434 . . . 119.6 ? C434 C435 C436 . . . 119.4(8) ? C434 C435 H435 . . . 120.7 ? C436 C435 H435 . . . 119.9 ? C431 C436 C435 . . . 120.4(7) ? C431 C436 H436 . . . 119.2 ? C435 C436 H436 . . . 120.4 ? C43 C44 C45 . . . 105.2(5) ? C43 C44 H44 . . . 127.1 ? C45 C44 H44 . . . 127.6 ? Nd1 C45 N41 . . . 64.7(2) ? Nd1 C45 C44 . . . 83.9(3) ? Nd1 C45 C451 . . . 113.8(3) ? N41 C45 C44 . . . 109.1(4) ? N41 C45 C451 . . . 120.1(5) ? C44 C45 C451 . . . 130.7(5) ? C45 C451 C452 . . . 119.7(5) ? C45 C451 C456 . . . 119.2(5) ? C452 C451 C456 . . . 121.0(5) ? C451 C452 C453 . . . 120.4(5) ? C451 C452 H452 . . . 120.3 ? C453 C452 H452 . . . 119.4 ? C452 C453 C454 . . . 119.7(6) ? C452 C453 H453 . . . 120.8 ? C454 C453 H453 . . . 119.5 ? C453 C454 C455 . . . 119.3(5) ? C453 C454 H454 . . . 120.3 ? C455 C454 H454 . . . 120.5 ? C454 C455 C456 . . . 121.6(6) ? C454 C455 H455 . . . 118.9 ? C456 C455 H455 . . . 119.5 ? C451 C456 C455 . . . 118.0(6) ? C451 C456 H456 . . . 120.7 ? C455 C456 H456 . . . 121.3 ? Nd2 N51 N52 . . . 73.2(2) ? Nd2 N51 C55 . . . 178.4(4) ? N52 N51 C55 . . . 108.4(4) ? Nd2 N52 N51 . . . 73.2(3) ? Nd2 N52 C53 . . . 179.1(4) ? N51 N52 C53 . . . 107.6(4) ? N52 C53 C531 . . . 120.7(5) ? N52 C53 C54 . . . 109.5(5) ? C531 C53 C54 . . . 129.7(6) ? C53 C531 C532 . . . 121.9(6) ? C53 C531 C536 . . . 118.3(6) ? C532 C531 C536 . . . 119.8(7) ? C531 C532 C533 . . . 121.9(8) ? C531 C532 H532 . . . 119.5 ? C533 C532 H532 . . . 118.6 ? C532 C533 C534 . . . 119.2(8) ? C532 C533 H533 . . . 120.2 ? C534 C533 H533 . . . 120.6 ? C533 C534 C535 . . . 118.7(9) ? C533 C534 H534 . . . 120.6 ? C535 C534 H534 . . . 120.7 ? C534 C535 C536 . . . 122.2(9) ? C534 C535 H535 . . . 118.2 ? C536 C535 H535 . . . 119.6 ? C531 C536 C535 . . . 118.2(8) ? C531 C536 H536 . . . 120.4 ? C535 C536 H536 . . . 121.4 ? C53 C54 C55 . . . 105.8(5) ? C53 C54 H54 . . . 127.4 ? C55 C54 H54 . . . 126.7 ? N51 C55 C54 . . . 108.6(5) ? N51 C55 C551 . . . 121.5(5) ? C54 C55 C551 . . . 129.9(5) ? C55 C551 C552 . . . 121.4(5) ? C55 C551 C556 . . . 120.1(6) ? C552 C551 C556 . . . 118.5(6) ? C551 C552 C553 . . . 121.5(6) ? C551 C552 H552 . . . 118.6 ? C553 C552 H552 . . . 119.9 ? C552 C553 C554 . . . 119.7(7) ? C552 C553 H553 . . . 119.5 ? C554 C553 H553 . . . 120.7 ? C553 C554 C555 . . . 120.2(7) ? C553 C554 H554 . . . 120.0 ? C555 C554 H554 . . . 119.8 ? C554 C555 C556 . . . 121.7(6) ? C554 C555 H555 . . . 119.2 ? C556 C555 H555 . . . 119.1 ? C551 C556 C555 . . . 118.3(6) ? C551 C556 H556 . . . 120.4 ? C555 C556 H556 . . . 121.2 ? Nd2 N61 Nd3 . . . 98.54(13) ? Nd2 N61 N62 . . . 85.9(2) ? Nd2 N61 C65 . . . 123.3(3) ? Nd3 N61 N62 . . . 69.3(2) ? Nd3 N61 C65 . . . 138.0(3) ? N62 N61 C65 . . . 107.1(4) ? Nd2 N62 Nd3 . . . 94.82(13) ? Nd2 N62 N61 . . . 64.2(2) ? Nd2 N62 C63 . . . 127.6(3) ? Nd3 N62 N61 . . . 79.3(2) ? Nd3 N62 C63 . . . 136.1(3) ? N61 N62 C63 . . . 106.9(4) ? N62 C63 C631 . . . 119.7(5) ? N62 C63 C64 . . . 110.3(5) ? C631 C63 C64 . . . 129.9(5) ? C63 C631 C632 . . . 120.9(5) ? C63 C631 C636 . . . 120.4(5) ? C632 C631 C636 . . . 118.7(6) ? C631 C632 C633 . . . 120.4(6) ? C631 C632 H632 . . . 118.6 ? C633 C632 H632 . . . 121.0 ? C632 C633 C634 . . . 120.0(7) ? C632 C633 H633 . . . 120.0 ? C634 C633 H633 . . . 119.9 ? C633 C634 C635 . . . 120.0(7) ? C633 C634 H634 . . . 119.5 ? C635 C634 H634 . . . 120.5 ? C634 C635 C636 . . . 120.2(7) ? C634 C635 H635 . . . 119.4 ? C636 C635 H635 . . . 120.5 ? C631 C636 C635 . . . 120.7(6) ? C631 C636 H636 . . . 119.5 ? C635 C636 H636 . . . 119.8 ? C63 C64 C65 . . . 105.5(4) ? C63 C64 H64 . . . 127.4 ? C65 C64 H64 . . . 127.1 ? N61 C65 C64 . . . 110.2(5) ? N61 C65 C651 . . . 121.6(5) ? C64 C65 C651 . . . 128.1(4) ? C65 C651 C652 . . . 121.6(4) ? C65 C651 C656 . . . 119.6(5) ? C652 C651 C656 . . . 118.8(6) ? C651 C652 C653 . . . 120.9(5) ? C651 C652 H652 . . . 119.8 ? C653 C652 H652 . . . 119.3 ? C652 C653 C654 . . . 119.5(7) ? C652 C653 H653 . . . 120.1 ? C654 C653 H653 . . . 120.4 ? C653 C654 C655 . . . 120.5(7) ? C653 C654 H654 . . . 119.5 ? C655 C654 H654 . . . 119.9 ? C654 C655 C656 . . . 119.6(6) ? C654 C655 H655 . . . 118.9 ? C656 C655 H655 . . . 121.6 ? C651 C656 C655 . . . 120.7(6) ? C651 C656 H656 . . . 119.5 ? C655 C656 H656 . . . 119.8 ? Nd2 N71 Nd3 . . . 96.43(12) ? Nd2 N71 N72 . . . 68.5(2) ? Nd2 N71 C75 . . . 173.3(3) ? Nd3 N71 N72 . . . 76.3(2) ? Nd3 N71 C75 . . . 87.1(3) ? N72 N71 C75 . . . 107.1(4) ? Nd2 N72 Nd3 . . . 99.09(13) ? Nd2 N72 N71 . . . 79.8(2) ? Nd2 N72 C73 . . . 170.1(3) ? Nd3 N72 N71 . . . 73.7(2) ? Nd3 N72 C73 . . . 88.3(3) ? N71 N72 C73 . . . 108.8(4) ? N72 C73 C731 . . . 120.3(4) ? N72 C73 C74 . . . 108.7(5) ? C731 C73 C74 . . . 131.0(4) ? C73 C731 C732 . . . 120.5(5) ? C73 C731 C736 . . . 120.4(5) ? C732 C731 C736 . . . 119.0(5) ? C731 C732 C733 . . . 120.2(5) ? C731 C732 H732 . . . 119.9 ? C733 C732 H732 . . . 120.0 ? C732 C733 C734 . . . 119.7(5) ? C732 C733 H733 . . . 119.3 ? C734 C733 H733 . . . 120.9 ? C733 C734 C735 . . . 121.7(6) ? C733 C734 H734 . . . 119.1 ? C735 C734 H734 . . . 119.1 ? C734 C735 C736 . . . 120.1(6) ? C734 C735 H735 . . . 121.0 ? C736 C735 H735 . . . 118.9 ? C731 C736 C735 . . . 119.2(6) ? C731 C736 H736 . . . 119.9 ? C735 C736 H736 . . . 120.8 ? C73 C74 C75 . . . 106.1(4) ? C73 C74 H74 . . . 127.2 ? C75 C74 H74 . . . 126.7 ? Nd3 C75 N71 . . . 65.3(2) ? Nd3 C75 C74 . . . 83.9(3) ? Nd3 C75 C751 . . . 117.3(3) ? N71 C75 C74 . . . 109.3(4) ? N71 C75 C751 . . . 122.2(5) ? C74 C75 C751 . . . 128.5(4) ? C75 C751 C752 . . . 121.0(5) ? C75 C751 C756 . . . 120.5(5) ? C752 C751 C756 . . . 118.5(5) ? C751 C752 C753 . . . 122.0(6) ? C751 C752 H752 . . . 118.3 ? C753 C752 H752 . . . 119.7 ? C752 C753 C754 . . . 119.5(7) ? C752 C753 H753 . . . 121.2 ? C754 C753 H753 . . . 119.3 ? C753 C754 C755 . . . 119.5(6) ? C753 C754 H754 . . . 120.2 ? C755 C754 H754 . . . 120.3 ? C754 C755 C756 . . . 120.7(6) ? C754 C755 H755 . . . 119.0 ? C756 C755 H755 . . . 120.3 ? C751 C756 C755 . . . 119.8(6) ? C751 C756 H756 . . . 119.9 ? C755 C756 H756 . . . 120.3 ? Nd3 N81 N82 . . . 73.9(2) ? Nd3 N81 C85 . . . 172.9(3) ? N82 N81 C85 . . . 108.6(4) ? Nd3 N82 N81 . . . 72.5(2) ? Nd3 N82 C83 . . . 173.4(3) ? N81 N82 C83 . . . 108.2(4) ? N82 C83 C831 . . . 123.0(4) ? N82 C83 C84 . . . 108.3(4) ? C831 C83 C84 . . . 128.7(5) ? C83 C831 C832 . . . 121.9(5) ? C83 C831 C836 . . . 120.1(4) ? C832 C831 C836 . . . 118.0(5) ? C831 C832 C833 . . . 120.9(5) ? C831 C832 H832 . . . 120.1 ? C833 C832 H832 . . . 119.1 ? C832 C833 C834 . . . 120.3(5) ? C832 C833 H833 . . . 120.4 ? C834 C833 H833 . . . 119.3 ? C833 C834 C835 . . . 118.8(5) ? C833 C834 H834 . . . 120.3 ? C835 C834 H834 . . . 120.8 ? C834 C835 C836 . . . 120.8(6) ? C834 C835 H835 . . . 119.8 ? C836 C835 H835 . . . 119.4 ? C831 C836 C835 . . . 121.3(5) ? C831 C836 H836 . . . 118.8 ? C835 C836 H836 . . . 120.0 ? C83 C84 C85 . . . 106.3(4) ? C83 C84 H84 . . . 126.4 ? C85 C84 H84 . . . 127.3 ? N81 C85 C84 . . . 108.6(4) ? N81 C85 C851 . . . 120.8(5) ? C84 C85 C851 . . . 130.6(4) ? C85 C851 C852 . . . 121.6(4) ? C85 C851 C856 . . . 120.6(5) ? C852 C851 C856 . . . 117.8(5) ? C851 C852 C853 . . . 120.8(5) ? C851 C852 H852 . . . 119.0 ? C853 C852 H852 . . . 120.1 ? C852 C853 C854 . . . 120.8(7) ? C852 C853 H853 . . . 119.9 ? C854 C853 H853 . . . 119.3 ? C853 C854 C855 . . . 119.5(6) ? C853 C854 H854 . . . 119.9 ? C855 C854 H854 . . . 120.6 ? C854 C855 C856 . . . 120.7(5) ? C854 C855 H855 . . . 119.7 ? C856 C855 H855 . . . 119.6 ? C851 C856 C855 . . . 120.3(5) ? C851 C856 H856 . . . 119.9 ? C855 C856 H856 . . . 119.9 ? Nd3 N91 N92 . . . 73.1(2) ? Nd3 N91 C95 . . . 171.1(3) ? N92 N91 C95 . . . 107.7(4) ? Nd3 N92 N91 . . . 73.4(2) ? Nd3 N92 C93 . . . 172.2(3) ? N91 N92 C93 . . . 109.0(4) ? N92 C93 C931 . . . 123.6(5) ? N92 C93 C94 . . . 108.7(4) ? C931 C93 C94 . . . 127.7(4) ? C93 C931 C932 . . . 121.7(4) ? C93 C931 C936 . . . 120.3(5) ? C932 C931 C936 . . . 117.9(5) ? C931 C932 C933 . . . 120.3(5) ? C931 C932 H932 . . . 119.2 ? C933 C932 H932 . . . 120.5 ? C932 C933 C934 . . . 121.2(6) ? C932 C933 H933 . . . 119.1 ? C934 C933 H933 . . . 119.7 ? C933 C934 C935 . . . 119.6(5) ? C933 C934 H934 . . . 121.0 ? C935 C934 H934 . . . 119.4 ? C934 C935 C936 . . . 120.3(5) ? C934 C935 H935 . . . 119.7 ? C936 C935 H935 . . . 119.9 ? C931 C936 C935 . . . 120.7(5) ? C931 C936 H936 . . . 119.1 ? C935 C936 H936 . . . 120.2 ? C93 C94 C95 . . . 105.4(5) ? C93 C94 H94 . . . 127.6 ? C95 C94 H94 . . . 126.9 ? N91 C95 C94 . . . 109.2(5) ? N91 C95 C951 . . . 122.6(4) ? C94 C95 C951 . . . 128.1(5) ? C95 C951 C952 . . . 122.7(5) ? C95 C951 C956 . . . 119.3(5) ? C952 C951 C956 . . . 117.9(5) ? C951 C952 C953 . . . 120.9(5) ? C951 C952 H952 . . . 119.4 ? C953 C952 H952 . . . 119.7 ? C952 C953 C954 . . . 120.0(6) ? C952 C953 H953 . . . 120.2 ? C954 C953 H953 . . . 119.8 ? C953 C954 C955 . . . 119.7(6) ? C953 C954 H954 . . . 120.4 ? C955 C954 H954 . . . 119.9 ? C954 C955 C956 . . . 120.0(6) ? C954 C955 H955 . . . 120.1 ? C956 C955 H955 . . . 119.9 ? C951 C956 C955 . . . 121.3(6) ? C951 C956 H956 . . . 119.7 ? C955 C956 H956 . . . 119.0 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 4860 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min -39 _reflns_limit_l_max 38 _reflns_number_observed ? _reflns_d_resolution_high .729 _reflns_d_resolution_low 14.04 _diffrn_reflns_av_sigmaI/netI .05 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .06 _refine_ls_wR_factor_all .065 _refine_ls_goodness_of_fit_all 1.463 _refine_ls_shift/su_mean .003 #===END data_ag88er _database_code_depnum_ccdc_archive 'CCDC 190715' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C90 H66 Er2 N12' _chemical_formula_moiety ? _chemical_formula_weight 1650.12 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/c_1 _symmetry_space_group_name_Hall -p_2ybc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 12.770(2) _cell_length_b 19.056(3) _cell_length_c 30.256(5) _cell_angle_alpha 90.00000 _cell_angle_beta 98.217(3) _cell_angle_gamma 90.00000 _cell_volume 7287(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 2.344 _exptl_crystal_description bar _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour pink _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .43 _exptl_absorpt_correction_T_max .84 _diffrn_reflns_number 69257 _reflns_number_total 17511 _reflns_Friedel_coverage 0 _reflns_number_gt 11167 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.21 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .051 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 40 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .07 _refine_ls_wR_factor_ref .082 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_number_reflns 11837 _refine_ls_number_parameters 919 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .019 _refine_diff_density_min -1.036 _refine_diff_density_max 2.113 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 360 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 264 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Er ? 0 8 -.723 4.958 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 48 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er1 .18784(3) .30565(2) .367409(14) .02344(18) Uani ? ? 1.00000 ? ? Er2 .42582(3) .20452(2) .366490(14) .0250(2) Uani ? ? 1.00000 ? ? N11 .1499(6) .3733(4) .4249(3) .029(4) Uani ? ? 1.00000 ? ? N12 .1739(7) .4181(4) .3914(3) .031(4) Uani ? ? 1.00000 ? ? C13 .1644(7) .4862(5) .4061(3) .028(4) Uani ? ? 1.00000 ? ? C131 .1973(8) .5439(5) .3791(4) .031(4) Uani ? ? 1.00000 ? ? C132 .2460(9) .5315(6) .3408(4) .040(6) Uani ? ? 1.00000 ? ? C133 .2796(10) .5882(6) .3177(4) .045(6) Uani ? ? 1.00000 ? ? C134 .2622(11) .6558(6) .3307(4) .048(6) Uani ? ? 1.00000 ? ? C135 .2156(10) .6687(5) .3687(4) .040(5) Uani ? ? 1.00000 ? ? C136 .1803(9) .6132(5) .3919(4) .040(5) Uani ? ? 1.00000 ? ? C14 .1371(8) .4826(5) .4486(3) .030(4) Uani ? ? 1.00000 ? ? C15 .1289(8) .4125(5) .4596(3) .029(4) Uani ? ? 1.00000 ? ? C151 .1086(9) .3800(5) .5016(4) .038(5) Uani ? ? 1.00000 ? ? C152 .0849(13) .3091(6) .5040(4) .057(7) Uani ? ? 1.00000 ? ? C153 .0748(15) .2770(7) .5439(5) .071(9) Uani ? ? 1.00000 ? ? C154 .0826(12) .3165(8) .5824(5) .059(8) Uani ? ? 1.00000 ? ? C155 .1040(13) .3865(8) .5812(4) .061(8) Uani ? ? 1.00000 ? ? C156 .1149(11) .4179(6) .5414(4) .049(6) Uani ? ? 1.00000 ? ? N21 .0670(7) .3081(4) .3051(3) .030(4) Uani ? ? 1.00000 ? ? N22 .0252(7) .2657(4) .3359(3) .031(4) Uani ? ? 1.00000 ? ? C23 -.0584(8) .2328(5) .3134(4) .032(5) Uani ? ? 1.00000 ? ? C231 -.1205(9) .1837(5) .3359(4) .040(5) Uani ? ? 1.00000 ? ? C232 -.1026(9) .1763(6) .3834(4) .046(6) Uani ? ? 1.00000 ? ? C233 -.1695(11) .1300(7) .4045(6) .063(7) Uani ? ? 1.00000 ? ? C234 -.2476(10) .0911(7) .3780(6) .062(7) Uani ? ? 1.00000 ? ? C235 -.2604(12) .0967(7) .3341(7) .072(9) Uani ? ? 1.00000 ? ? C236 -.1988(9) .1415(6) .3131(5) .046(6) Uani ? ? 1.00000 ? ? C24 -.0748(8) .2545(6) .2691(4) .037(5) Uani ? ? 1.00000 ? ? C25 .0070(8) .3028(5) .2654(3) .033(5) Uani ? ? 1.00000 ? ? C251 .0312(8) .3448(6) .2267(3) .033(5) Uani ? ? 1.00000 ? ? C252 .0892(10) .4038(6) .2345(4) .043(6) Uani ? ? 1.00000 ? ? C253 .1150(10) .4454(7) .1991(5) .052(7) Uani ? ? 1.00000 ? ? C254 .0758(12) .4270(8) .1563(4) .059(8) Uani ? ? 1.00000 ? ? C255 .0173(13) .3662(10) .1473(4) .070(9) Uani ? ? 1.00000 ? ? C256 -.0048(11) .3247(8) .1830(4) .057(7) Uani ? ? 1.00000 ? ? N31 .3524(7) .3254(4) .3400(3) .032(4) Uani ? ? 1.00000 ? ? N32 .3794(7) .3225(4) .3866(3) .030(4) Uani ? ? 1.00000 ? ? C33 .4497(8) .3768(5) .3989(4) .037(5) Uani ? ? 1.00000 ? ? C331 .4865(10) .3870(6) .4456(4) .047(6) Uani ? ? 1.00000 ? ? C332 .4327(12) .3595(8) .4781(4) .059(8) Uani ? ? 1.00000 ? ? C333 .4595(16) .3712(11) .5232(6) .085(12) Uani ? ? 1.00000 ? ? C334 .5523(18) .4092(13) .5363(6) .096(14) Uani ? ? 1.00000 ? ? C335 .6107(15) .4352(11) .5063(8) .098(14) Uani ? ? 1.00000 ? ? C336 .5802(12) .4236(8) .4609(6) .070(9) Uani ? ? 1.00000 ? ? C34 .4680(7) .4102(4) .3605(4) .036(5) Uani ? ? 1.00000 ? ? C35 .4089(8) .3790(5) .3244(4) .032(5) Uani ? ? 1.00000 ? ? C351 .4006(9) .3917(6) .2759(4) .042(6) Uani ? ? 1.00000 ? ? C352 .3459(10) .3497(6) .2457(4) .047(6) Uani ? ? 1.00000 ? ? C353 .3415(12) .3598(8) .2010(5) .058(8) Uani ? ? 1.00000 ? ? C354 .3973(12) .4137(9) .1856(5) .061(8) Uani ? ? 1.00000 ? ? C355 .4544(13) .4583(8) .2152(6) .068(9) Uani ? ? 1.00000 ? ? C356 .4564(10) .4482(7) .2602(5) .052(7) Uani ? ? 1.00000 ? ? N41 .2514(6) .1880(4) .3968(2) .027(4) Uani ? ? 1.00000 ? ? N42 .2391(7) .1850(4) .3487(3) .031(4) Uani ? ? 1.00000 ? ? C43 .1705(8) .1335(4) .3364(3) .029(4) Uani ? ? 1.00000 ? ? C431 .1346(8) .1202(5) .2887(3) .029(4) Uani ? ? 1.00000 ? ? C432 .1737(8) .1606(6) .2568(4) .037(5) Uani ? ? 1.00000 ? ? C433 .1330(10) .1546(7) .2129(4) .049(7) Uani ? ? 1.00000 ? ? C434 .0535(10) .1085(7) .1991(4) .048(6) Uani ? ? 1.00000 ? ? C435 .0129(10) .0661(7) .2316(5) .052(7) Uani ? ? 1.00000 ? ? C436 .0553(9) .0726(6) .2760(4) .043(6) Uani ? ? 1.00000 ? ? C44 .1387(7) .1007(4) .3734(3) .0225(16) Uiso ? ? 1.00000 ? ? C45 .1953(7) .1336(5) .4087(4) .032(5) Uani ? ? 1.00000 ? ? C451 .1970(8) .1238(5) .4592(3) .033(5) Uani ? ? 1.00000 ? ? C452 .2794(10) .1477(7) .4901(4) .048(7) Uani ? ? 1.00000 ? ? C453 .2813(11) .1386(8) .5353(4) .058(8) Uani ? ? 1.00000 ? ? C454 .2007(12) .0971(8) .5509(4) .058(8) Uani ? ? 1.00000 ? ? C455 .1214(14) .0754(8) .5217(5) .068(9) Uani ? ? 1.00000 ? ? C456 .1137(10) .0858(6) .4749(4) .047(6) Uani ? ? 1.00000 ? ? N51 .4985(7) .2035(4) .3026(3) .031(4) Uani ? ? 1.00000 ? ? N52 .5632(7) .2446(4) .3330(3) .033(4) Uani ? ? 1.00000 ? ? C53 .6301(9) .2820(5) .3123(4) .037(5) Uani ? ? 1.00000 ? ? C531 .7102(8) .3298(5) .3357(4) .041(6) Uani ? ? 1.00000 ? ? C532 .7420(10) .3240(7) .3819(4) .048(3) Uiso ? ? 1.00000 ? ? C533 .8172(11) .3661(8) .4025(5) .058(8) Uani ? ? 1.00000 ? ? C534 .8691(11) .4146(9) .3818(6) .076(10) Uani ? ? 1.00000 ? ? C535 .8382(10) .4214(7) .3343(6) .061(8) Uani ? ? 1.00000 ? ? C536 .7568(11) .3796(6) .3128(5) .054(7) Uani ? ? 1.00000 ? ? C54 .6104(8) .2662(6) .2667(4) .037(5) Uani ? ? 1.00000 ? ? C55 .5271(8) .2164(5) .2618(3) .030(4) Uani ? ? 1.00000 ? ? C551 .4751(9) .1837(6) .2209(4) .041(6) Uani ? ? 1.00000 ? ? C552 .4179(11) .1217(7) .2231(4) .053(7) Uani ? ? 1.00000 ? ? C553 .3695(12) .0879(9) .1836(6) .073(10) Uani ? ? 1.00000 ? ? C554 .3752(13) .1193(11) .1439(5) .077(11) Uani ? ? 1.00000 ? ? C555 .4305(13) .1806(9) .1405(4) .067(9) Uani ? ? 1.00000 ? ? C556 .4776(12) .2127(8) .1790(4) .058(7) Uani ? ? 1.00000 ? ? N61 .4483(7) .0930(4) .3925(3) .035(4) Uani ? ? 1.00000 ? ? N62 .5111(6) .1364(4) .4207(3) .028(4) Uani ? ? 1.00000 ? ? C63 .5662(8) .0961(6) .4531(3) .033(5) Uani ? ? 1.00000 ? ? C631 .6510(9) .1273(7) .4867(4) .043(6) Uani ? ? 1.00000 ? ? C632 .6569(12) .2003(8) .4904(4) .061(8) Uani ? ? 1.00000 ? ? C633 .7397(14) .2307(9) .5198(6) .072(10) Uani ? ? 1.00000 ? ? C634 .8149(13) .1867(11) .5445(6) .080(11) Uani ? ? 1.00000 ? ? C635 .8076(13) .1151(10) .5411(5) .072(10) Uani ? ? 1.00000 ? ? C636 .7232(11) .0851(8) .5122(4) .058(8) Uani ? ? 1.00000 ? ? C64 .5371(8) .0264(5) .4465(3) .035(5) Uani ? ? 1.00000 ? ? C65 .4636(9) .0258(5) .4084(3) .034(5) Uani ? ? 1.00000 ? ? C651 .4014(8) -.0313(5) .3841(4) .038(6) Uani ? ? 1.00000 ? ? C652 .3300(11) -.0218(6) .3465(4) .046(6) Uani ? ? 1.00000 ? ? C653 .2712(11) -.0761(6) .3250(5) .054(7) Uani ? ? 1.00000 ? ? C654 .2913(11) -.1439(6) .3403(5) .052(7) Uani ? ? 1.00000 ? ? C655 .3628(12) -.1569(5) .3770(6) .056(7) Uani ? ? 1.00000 ? ? C656 .4194(11) -.1018(6) .4003(5) .053(7) Uani ? ? 1.00000 ? ? H132 .25467 .48469 .32988 .04900 Uiso ? ? 1.00000 ? ? H133 .31471 .57997 .29236 .06200 Uiso ? ? 1.00000 ? ? H134 .28550 .69449 .31399 .05800 Uiso ? ? 1.00000 ? ? H135 .20847 .71672 .37901 .05400 Uiso ? ? 1.00000 ? ? H136 .14518 .62243 .41776 .04500 Uiso ? ? 1.00000 ? ? H14 .12654 .52185 .46809 .03700 Uiso ? ? 1.00000 ? ? H152 .08010 .28138 .47728 .06100 Uiso ? ? 1.00000 ? ? H153 .05719 .22751 .54363 .08300 Uiso ? ? 1.00000 ? ? H154 .08070 .29432 .61048 .07700 Uiso ? ? 1.00000 ? ? H155 .10463 .41407 .60829 .07500 Uiso ? ? 1.00000 ? ? H156 .12772 .46806 .54007 .05600 Uiso ? ? 1.00000 ? ? H232 -.04580 .20142 .40092 .05200 Uiso ? ? 1.00000 ? ? H233 -.15954 .12508 .43562 .08300 Uiso ? ? 1.00000 ? ? H234 -.28996 .06193 .39392 .06600 Uiso ? ? 1.00000 ? ? H235 -.31976 .06894 .31779 .08400 Uiso ? ? 1.00000 ? ? H236 -.21096 .14436 .27953 .05300 Uiso ? ? 1.00000 ? ? H24 -.13008 .23973 .24634 .04400 Uiso ? ? 1.00000 ? ? H252 .11508 .41640 .26486 .05700 Uiso ? ? 1.00000 ? ? H253 .15960 .48721 .20547 .07300 Uiso ? ? 1.00000 ? ? H254 .09181 .45529 .13224 .06900 Uiso ? ? 1.00000 ? ? H255 -.00999 .35590 .11719 .07600 Uiso ? ? 1.00000 ? ? H256 -.04553 .28152 .17717 .07100 Uiso ? ? 1.00000 ? ? H332 .37739 .32928 .46709 .07300 Uiso ? ? 1.00000 ? ? H333 .41457 .35336 .54364 .09900 Uiso ? ? 1.00000 ? ? H334 .56846 .41810 .57026 .11600 Uiso ? ? 1.00000 ? ? H335 .67251 .45824 .51700 .11800 Uiso ? ? 1.00000 ? ? H336 .62421 .44054 .43907 .08300 Uiso ? ? 1.00000 ? ? H34 .51296 .44987 .36032 .04000 Uiso ? ? 1.00000 ? ? H352 .30349 .31188 .25600 .05800 Uiso ? ? 1.00000 ? ? H353 .30174 .33022 .17961 .06700 Uiso ? ? 1.00000 ? ? H354 .39575 .41907 .15400 .07600 Uiso ? ? 1.00000 ? ? H355 .49054 .49646 .20404 .08000 Uiso ? ? 1.00000 ? ? H356 .49599 .48001 .28122 .07200 Uiso ? ? 1.00000 ? ? H432 .23243 .19239 .26515 .04500 Uiso ? ? 1.00000 ? ? H433 .16084 .18243 .18975 .06400 Uiso ? ? 1.00000 ? ? H434 .02182 .10375 .16825 .06300 Uiso ? ? 1.00000 ? ? H435 -.04596 .03355 .22257 .06200 Uiso ? ? 1.00000 ? ? H436 .03395 .04213 .29841 .05300 Uiso ? ? 1.00000 ? ? H44 .08645 .06466 .37408 .03000 Uiso ? ? 1.00000 ? ? H452 .33414 .17314 .47869 .06700 Uiso ? ? 1.00000 ? ? H453 .33990 .15902 .55615 .07700 Uiso ? ? 1.00000 ? ? H454 .20174 .08633 .58175 .07700 Uiso ? ? 1.00000 ? ? H455 .06576 .04907 .53294 .08100 Uiso ? ? 1.00000 ? ? H456 .05818 .06725 .45389 .06000 Uiso ? ? 1.00000 ? ? H532 .71005 .28787 .39771 .07100 Uiso ? ? 1.00000 ? ? H533 .83614 .35894 .43517 .06600 Uiso ? ? 1.00000 ? ? H534 .92200 .44101 .40052 .08800 Uiso ? ? 1.00000 ? ? H535 .87221 .45593 .31668 .07400 Uiso ? ? 1.00000 ? ? H536 .73421 .38552 .28152 .06200 Uiso ? ? 1.00000 ? ? H54 .64879 .28500 .24357 .04800 Uiso ? ? 1.00000 ? ? H552 .40913 .10063 .25284 .07000 Uiso ? ? 1.00000 ? ? H553 .32763 .04378 .18442 .09200 Uiso ? ? 1.00000 ? ? H554 .34676 .09700 .11630 .08500 Uiso ? ? 1.00000 ? ? H555 .43353 .20156 .11201 .08500 Uiso ? ? 1.00000 ? ? H556 .51660 .25612 .17692 .07700 Uiso ? ? 1.00000 ? ? H632 .60666 .23023 .47343 .07100 Uiso ? ? 1.00000 ? ? H633 .74835 .28198 .52183 .09600 Uiso ? ? 1.00000 ? ? H634 .86972 .20775 .56506 .09700 Uiso ? ? 1.00000 ? ? H635 .86218 .08562 .55806 .08800 Uiso ? ? 1.00000 ? ? H636 .71641 .03533 .50998 .06700 Uiso ? ? 1.00000 ? ? H64 .56360 -.01303 .46461 .04300 Uiso ? ? 1.00000 ? ? H652 .32067 .02410 .33422 .05800 Uiso ? ? 1.00000 ? ? H653 .21737 -.06714 .30032 .06600 Uiso ? ? 1.00000 ? ? H654 .25478 -.18265 .32508 .05900 Uiso ? ? 1.00000 ? ? H655 .37577 -.20423 .38701 .06300 Uiso ? ? 1.00000 ? ? H656 .47137 -.11080 .42668 .06900 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er1 .0294(2) .01835(17) .0227(2) -.00210(15) .00446(14) -.00105(14) Er2 .0285(2) .01825(17) .0282(2) -.00236(16) .00459(15) .00131(15) N11 .035(4) .031(4) .021(4) -.001(3) .011(3) -.000(3) N12 .046(5) .019(3) .027(4) .002(3) .004(3) -.006(3) C13 .025(5) .026(4) .035(5) -.002(4) .007(4) -.006(4) C131 .031(5) .018(4) .041(6) -.003(4) -.000(4) -.003(4) C132 .045(6) .034(5) .044(6) .003(5) .015(5) .001(4) C133 .053(7) .037(6) .048(7) -.003(5) .018(5) .008(5) C134 .059(8) .035(6) .050(7) .001(5) .006(6) .016(5) C135 .051(7) .022(4) .047(6) .001(4) .001(5) -.002(4) C136 .045(6) .022(4) .050(7) -.000(4) -.003(5) -.000(4) C14 .030(5) .031(5) .028(5) .002(4) .001(4) -.006(4) C15 .036(5) .032(5) .018(4) .002(4) .002(3) -.007(3) C151 .044(6) .033(5) .039(6) -.001(4) .016(5) .002(4) C152 .105(11) .036(6) .039(6) -.009(7) .038(7) -.008(5) C153 .128(14) .042(7) .054(9) -.000(8) .048(9) -.001(6) C154 .073(9) .062(8) .051(8) .006(7) .033(7) .010(6) C155 .088(11) .060(8) .037(7) -.013(8) .019(7) -.013(6) C156 .068(8) .040(6) .042(7) -.018(6) .017(6) -.011(5) N21 .041(5) .025(4) .024(4) -.005(3) .003(3) -.002(3) N22 .032(4) .030(4) .031(4) -.002(3) .008(3) .002(3) C23 .029(5) .026(4) .042(6) .002(4) .010(4) -.001(4) C231 .036(6) .026(5) .060(7) .005(4) .014(5) .000(4) C232 .036(6) .042(6) .066(8) -.011(5) .029(6) -.006(5) C233 .045(5) .035(4) .116(12) .005(3) .036(5) .013(4) C234 .040(5) .040(6) .112(12) .005(3) .034(5) .012(4) C235 .064(9) .034(4) .124(14) .006(3) .034(5) .013(5) C236 .034(6) .032(5) .075(9) -.007(4) .021(6) -.009(5) C24 .033(5) .039(5) .037(6) .002(4) -.002(4) -.006(4) C25 .032(5) .030(5) .036(5) .003(4) .001(4) -.002(4) C251 .023(5) .053(6) .024(5) .001(4) .006(3) .001(4) C252 .056(7) .037(5) .039(6) .004(5) .018(5) .007(5) C253 .053(7) .052(7) .055(8) .016(6) .024(6) .026(6) C254 .076(9) .067(9) .042(7) .026(8) .032(7) .024(6) C255 .069(9) .115(14) .026(6) .028(10) .007(6) .008(7) C256 .062(8) .070(9) .035(6) .008(7) -.003(5) -.005(6) N31 .042(5) .017(3) .037(5) -.006(3) .012(4) .002(3) N32 .035(4) .016(3) .035(5) -.005(3) -.007(3) .002(3) C33 .027(5) .030(5) .051(7) -.017(4) -.001(4) -.006(4) C331 .044(7) .034(6) .058(8) -.006(5) -.005(5) -.013(5) C332 .068(9) .064(8) .040(7) -.011(7) -.014(6) -.004(6) C333 .089(13) .105(14) .058(10) .006(11) -.001(9) -.009(10) C334 .088(14) .129(18) .060(11) .022(13) -.029(10) -.018(12) C335 .068(12) .099(14) .111(17) .010(11) -.042(11) -.049(13) C336 .050(8) .060(9) .094(12) -.006(7) -.008(8) -.025(8) C34 .020(5) .013(4) .070(7) -.002(3) -.008(4) -.008(4) C35 .033(5) .024(4) .042(6) .005(4) .020(4) .013(4) C351 .048(6) .044(6) .039(6) .016(5) .028(5) .011(5) C352 .044(7) .041(6) .060(8) .007(5) .027(6) .002(5) C353 .068(9) .061(8) .042(7) .001(7) .001(6) .011(6) C354 .065(9) .081(10) .040(7) .035(8) .018(6) .008(7) C355 .075(10) .068(9) .069(10) .012(8) .035(8) .030(8) C356 .050(7) .050(7) .058(8) -.000(6) .017(6) .005(6) N41 .022(4) .035(4) .023(4) -.001(3) .006(3) .002(3) N42 .045(5) .026(4) .026(4) -.002(3) .017(3) .004(3) C43 .032(5) .014(4) .043(6) .007(3) .010(4) -.007(3) C431 .033(5) .024(4) .033(5) .007(4) .013(4) -.000(4) C432 .037(6) .036(5) .037(6) -.010(4) .007(4) .001(4) C433 .055(7) .068(8) .025(6) .005(6) .007(5) .002(5) C434 .054(7) .062(8) .028(6) .002(6) .003(5) -.009(5) C435 .041(7) .062(8) .055(8) -.019(6) .016(5) -.017(6) C436 .042(6) .044(6) .041(6) -.014(5) .002(5) -.003(5) C45 .014(4) .025(4) .057(7) .004(3) .001(4) .021(4) C451 .041(6) .028(5) .035(6) -.002(4) .020(4) .005(4) C452 .047(7) .072(8) .027(6) -.003(6) .010(5) .004(5) C453 .061(8) .081(10) .035(7) .008(7) .018(6) .004(6) C454 .066(9) .084(10) .026(6) .004(8) .016(6) .020(6) C455 .083(11) .064(9) .065(10) .011(8) .038(9) .030(8) C456 .053(7) .040(6) .052(7) -.005(5) .025(6) .006(5) N51 .038(4) .027(4) .028(4) .001(3) .003(3) -.004(3) N52 .043(5) .029(4) .028(4) -.009(4) .012(3) .002(3) C53 .044(6) .029(5) .043(6) .002(4) .024(5) .001(4) C531 .029(5) .026(5) .069(8) -.008(4) .012(5) -.003(5) C533 .046(7) .060(8) .063(9) -.002(6) -.010(6) -.016(7) C534 .037(7) .085(11) .117(14) -.020(7) .043(8) -.074(10) C535 .036(7) .039(6) .113(13) -.008(5) .027(7) -.001(7) C536 .060(8) .029(5) .080(10) -.016(5) .030(7) -.009(5) C54 .032(5) .046(6) .037(6) .008(4) .018(4) .010(4) C55 .033(5) .027(4) .032(5) .008(4) .005(4) -.001(4) C551 .036(6) .048(6) .042(6) .004(5) .009(4) -.013(5) C552 .060(8) .059(8) .042(7) .012(6) .010(6) -.014(6) C553 .058(9) .070(10) .089(13) .003(8) .004(8) -.036(9) C554 .061(9) .120(15) .045(8) .022(10) -.006(7) -.033(9) C555 .081(10) .085(11) .032(7) -.007(9) .000(6) -.013(7) C556 .068(8) .070(9) .036(6) .009(7) .010(6) .001(6) N61 .046(5) .024(4) .034(5) -.004(4) .006(4) -.004(3) N62 .025(4) .031(4) .027(4) -.000(3) -.000(3) .005(3) C63 .037(5) .042(5) .020(4) .003(4) .005(4) .007(4) C631 .044(6) .053(7) .031(6) .007(5) .007(5) .002(5) C632 .067(9) .067(9) .043(7) -.003(7) -.015(6) -.012(6) C633 .075(10) .071(10) .065(10) -.000(8) -.008(8) -.023(8) C634 .059(9) .108(14) .069(10) -.002(9) -.004(7) -.031(10) C635 .060(9) .090(12) .060(9) .020(8) -.012(7) -.022(8) C636 .057(8) .075(9) .039(7) .018(7) -.006(6) -.004(6) C64 .041(6) .032(5) .033(5) .006(4) .012(4) .011(4) C65 .050(6) .027(4) .030(5) .004(4) .017(4) .001(4) C651 .037(6) .023(4) .060(7) .004(4) .028(5) .003(4) C652 .068(8) .032(5) .042(7) .007(5) .024(6) -.003(4) C653 .063(8) .035(6) .068(9) -.009(6) .023(7) -.013(6) C654 .050(7) .040(6) .071(9) -.017(5) .024(6) -.012(6) C655 .061(8) .016(4) .100(11) -.000(5) .038(8) -.001(5) C656 .064(8) .029(5) .073(9) -.001(5) .030(7) .005(6) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Er1 Er2 . . 3.6020(7) ? Er1 N11 . . 2.273(8) ? Er1 N12 . . 2.278(8) ? Er1 N21 . . 2.259(7) ? Er1 N22 . . 2.288(8) ? Er1 N31 . . 2.397(9) ? Er1 N32 . . 2.453(8) ? Er1 N41 . . 2.504(8) ? Er1 N42 . . 2.479(8) ? Er2 N31 . . 2.572(8) ? Er2 N32 . . 2.425(7) ? Er2 N41 . . 2.546(8) ? Er2 N42 . . 2.398(9) ? Er2 N51 . . 2.261(9) ? Er2 N52 . . 2.278(9) ? Er2 N61 . . 2.269(8) ? Er2 N62 . . 2.247(8) ? N11 N12 . . 1.394(11) ? N11 C15 . . 1.345(12) ? N12 C13 . . 1.382(12) ? C13 C131 . . 1.465(14) ? C13 C14 . . 1.382(14) ? C131 C132 . . 1.410(17) ? C131 C136 . . 1.403(14) ? C132 C133 . . 1.387(17) ? C132 H132 . . .964 ? C133 C134 . . 1.375(17) ? C133 H133 . . .956 ? C134 C135 . . 1.388(19) ? C134 H134 . . .965 ? C135 C136 . . 1.381(16) ? C135 H135 . . .976 ? C136 H136 . . .971 ? C14 C15 . . 1.385(14) ? C14 H14 . . .974 ? C15 C151 . . 1.470(15) ? C151 C152 . . 1.390(16) ? C151 C156 . . 1.396(16) ? C152 C153 . . 1.38(2) ? C152 H152 . . .960 ? C153 C154 . . 1.38(2) ? C153 H153 . . .969 ? C154 C155 . . 1.36(2) ? C154 H154 . . .953 ? C155 C156 . . 1.371(19) ? C155 H155 . . .971 ? C156 H156 . . .972 ? N21 N22 . . 1.395(12) ? N21 C25 . . 1.335(12) ? N22 C23 . . 1.338(12) ? C23 C231 . . 1.456(16) ? C23 C24 . . 1.390(15) ? C231 C232 . . 1.431(18) ? C231 C236 . . 1.387(15) ? C232 C233 . . 1.44(2) ? C232 H232 . . .962 ? C233 C234 . . 1.40(2) ? C233 H233 . . .935 ? C234 C235 . . 1.32(3) ? C234 H234 . . .952 ? C235 C236 . . 1.38(2) ? C235 H235 . . .996 ? C236 H236 . . 1.007 ? C24 C25 . . 1.409(15) ? C24 H24 . . .955 ? C25 C251 . . 1.487(15) ? C251 C252 . . 1.348(16) ? C251 C256 . . 1.388(16) ? C252 C253 . . 1.410(18) ? C252 H252 . . .960 ? C253 C254 . . 1.368(18) ? C253 H253 . . .981 ? C254 C255 . . 1.38(2) ? C254 H254 . . .950 ? C255 C256 . . 1.40(2) ? C255 H255 . . .947 ? C256 H256 . . .976 ? N31 N32 . . 1.406(12) ? N31 C35 . . 1.372(13) ? N32 C33 . . 1.385(13) ? C33 C331 . . 1.436(17) ? C33 C34 . . 1.375(17) ? C331 C332 . . 1.38(2) ? C331 C336 . . 1.405(19) ? C332 C333 . . 1.38(2) ? C332 H332 . . .935 ? C333 C334 . . 1.40(3) ? C333 H333 . . .96 ? C334 C335 . . 1.35(3) ? C334 H334 . . 1.03 ? C335 C336 . . 1.39(3) ? C335 H335 . . .92 ? C336 H336 . . .981 ? C34 C35 . . 1.371(14) ? C34 H34 . . .950 ? C35 C351 . . 1.476(16) ? C351 C352 . . 1.335(16) ? C351 C356 . . 1.410(18) ? C352 C353 . . 1.36(2) ? C352 H352 . . .978 ? C353 C354 . . 1.37(2) ? C353 H353 . . .950 ? C354 C355 . . 1.37(2) ? C354 H354 . . .960 ? C355 C356 . . 1.37(2) ? C355 H355 . . .949 ? C356 H356 . . .967 ? N41 N42 . . 1.443(11) ? N41 C45 . . 1.339(12) ? N42 C43 . . 1.331(12) ? C43 C431 . . 1.470(14) ? C43 C44 . . 1.393(14) ? C431 C432 . . 1.385(15) ? C431 C436 . . 1.374(15) ? C432 C433 . . 1.360(15) ? C432 H432 . . .969 ? C433 C434 . . 1.362(18) ? C433 H433 . . .984 ? C434 C435 . . 1.43(2) ? C434 H434 . . .966 ? C435 C436 . . 1.379(17) ? C435 H435 . . .982 ? C436 H436 . . .962 ? C44 C45 . . 1.357(13) ? C44 H44 . . .959 ? C45 C451 . . 1.534(16) ? C451 C452 . . 1.380(15) ? C451 C456 . . 1.424(17) ? C452 C453 . . 1.378(18) ? C452 H452 . . .955 ? C453 C454 . . 1.43(2) ? C453 H453 . . .986 ? C454 C455 . . 1.31(2) ? C454 H454 . . .953 ? C455 C456 . . 1.42(2) ? C455 H455 . . .970 ? C456 H456 . . .951 ? N51 N52 . . 1.388(11) ? N51 C55 . . 1.358(13) ? N52 C53 . . 1.338(15) ? C53 C531 . . 1.473(15) ? C53 C54 . . 1.398(15) ? C531 C532 . . 1.405(18) ? C531 C536 . . 1.360(18) ? C532 C533 . . 1.335(18) ? C532 H532 . . .961 ? C533 C534 . . 1.34(2) ? C533 H533 . . .993 ? C534 C535 . . 1.44(3) ? C534 H534 . . .960 ? C535 C536 . . 1.394(18) ? C535 H535 . . .985 ? C536 H536 . . .956 ? C54 C55 . . 1.417(14) ? C54 H54 . . .978 ? C55 C551 . . 1.459(14) ? C551 C552 . . 1.396(18) ? C551 C556 . . 1.385(18) ? C552 C553 . . 1.42(2) ? C552 H552 . . 1.006 ? C553 C554 . . 1.35(3) ? C553 H553 . . .998 ? C554 C555 . . 1.38(3) ? C554 H554 . . .961 ? C555 C556 . . 1.38(2) ? C555 H555 . . .955 ? C556 H556 . . .973 ? N61 N62 . . 1.362(11) ? N61 C65 . . 1.373(13) ? N62 C63 . . 1.359(12) ? C63 C631 . . 1.499(15) ? C63 C64 . . 1.385(15) ? C631 C632 . . 1.40(2) ? C631 C636 . . 1.374(18) ? C632 C633 . . 1.41(2) ? C632 H632 . . .952 ? C633 C634 . . 1.41(2) ? C633 H633 . . .984 ? C634 C635 . . 1.37(3) ? C634 H634 . . .955 ? C635 C636 . . 1.41(2) ? C635 H635 . . .981 ? C636 H636 . . .954 ? C64 C65 . . 1.379(14) ? C64 H64 . . .962 ? C65 C651 . . 1.480(14) ? C651 C652 . . 1.364(16) ? C651 C656 . . 1.437(16) ? C652 C653 . . 1.386(17) ? C652 H652 . . .951 ? C653 C654 . . 1.386(18) ? C653 H653 . . .955 ? C654 C655 . . 1.35(2) ? C654 H654 . . .956 ? C655 C656 . . 1.405(17) ? C655 H655 . . .959 ? C656 H656 . . .978 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Er2 Er1 N11 . . . 125.6(2) ? Er2 Er1 N12 . . . 127.6(2) ? Er2 Er1 N21 . . . 118.8(2) ? Er2 Er1 N22 . . . 122.4(2) ? Er2 Er1 N31 . . . 45.50(18) ? Er2 Er1 N32 . . . 42.09(17) ? Er2 Er1 N41 . . . 44.98(18) ? Er2 Er1 N42 . . . 41.5(2) ? N11 Er1 N12 . . . 35.7(3) ? N11 Er1 N21 . . . 115.6(3) ? N11 Er1 N22 . . . 103.1(3) ? N11 Er1 N31 . . . 118.0(3) ? N11 Er1 N32 . . . 93.4(3) ? N11 Er1 N41 . . . 109.2(3) ? N11 Er1 N42 . . . 142.5(3) ? N12 Er1 N21 . . . 99.8(3) ? N12 Er1 N22 . . . 109.7(3) ? N12 Er1 N31 . . . 94.3(3) ? N12 Er1 N32 . . . 85.5(3) ? N12 Er1 N41 . . . 139.9(3) ? N12 Er1 N42 . . . 168.8(3) ? N21 Er1 N22 . . . 35.7(3) ? N21 Er1 N31 . . . 103.6(3) ? N21 Er1 N32 . . . 137.2(3) ? N21 Er1 N41 . . . 117.6(3) ? N21 Er1 N42 . . . 90.0(3) ? N22 Er1 N31 . . . 134.2(3) ? N22 Er1 N32 . . . 163.2(3) ? N22 Er1 N41 . . . 94.5(3) ? N22 Er1 N42 . . . 81.4(3) ? N31 Er1 N32 . . . 33.7(3) ? N31 Er1 N41 . . . 90.5(3) ? N31 Er1 N42 . . . 78.1(3) ? N32 Er1 N41 . . . 76.8(2) ? N32 Er1 N42 . . . 83.6(3) ? N41 Er1 N42 . . . 33.7(3) ? Er1 Er2 N31 . . . 41.7(2) ? Er1 Er2 N32 . . . 42.7(2) ? Er1 Er2 N41 . . . 44.03(18) ? Er1 Er2 N42 . . . 43.26(19) ? Er1 Er2 N51 . . . 117.4(2) ? Er1 Er2 N52 . . . 121.9(2) ? Er1 Er2 N61 . . . 124.3(2) ? Er1 Er2 N62 . . . 128.7(2) ? N31 Er2 N32 . . . 32.5(3) ? N31 Er2 N41 . . . 85.7(3) ? N31 Er2 N42 . . . 76.3(3) ? N31 Er2 N51 . . . 85.2(3) ? N31 Er2 N52 . . . 80.2(3) ? N31 Er2 N61 . . . 165.7(3) ? N31 Er2 N62 . . . 149.6(3) ? N32 Er2 N41 . . . 76.5(3) ? N32 Er2 N42 . . . 86.0(3) ? N32 Er2 N51 . . . 111.6(3) ? N32 Er2 N52 . . . 91.8(3) ? N32 Er2 N61 . . . 143.5(3) ? N32 Er2 N62 . . . 117.6(3) ? N41 Er2 N42 . . . 33.8(3) ? N41 Er2 N51 . . . 142.5(3) ? N41 Er2 N52 . . . 165.9(3) ? N41 Er2 N61 . . . 80.4(3) ? N41 Er2 N62 . . . 91.3(3) ? N42 Er2 N51 . . . 108.8(3) ? N42 Er2 N52 . . . 139.2(3) ? N42 Er2 N61 . . . 90.3(3) ? N42 Er2 N62 . . . 115.9(3) ? N51 Er2 N52 . . . 35.6(3) ? N51 Er2 N61 . . . 104.0(3) ? N51 Er2 N62 . . . 113.8(3) ? N52 Er2 N61 . . . 113.6(3) ? N52 Er2 N62 . . . 101.2(3) ? N61 Er2 N62 . . . 35.1(3) ? Er1 N11 N12 . . . 72.4(5) ? Er1 N11 C15 . . . 178.8(6) ? N12 N11 C15 . . . 108.4(8) ? Er1 N12 N11 . . . 72.0(5) ? Er1 N12 C13 . . . 179.4(7) ? N11 N12 C13 . . . 107.6(8) ? N12 C13 C131 . . . 118.7(9) ? N12 C13 C14 . . . 107.3(8) ? C131 C13 C14 . . . 133.3(9) ? C13 C131 C132 . . . 121.8(9) ? C13 C131 C136 . . . 118.9(10) ? C132 C131 C136 . . . 119.2(10) ? C131 C132 C133 . . . 119.2(10) ? C131 C132 H132 . . . 121.5 ? C133 C132 H132 . . . 119.3 ? C132 C133 C134 . . . 120.8(12) ? C132 C133 H133 . . . 119.4 ? C134 C133 H133 . . . 119.8 ? C133 C134 C135 . . . 120.5(11) ? C133 C134 H134 . . . 119.4 ? C135 C134 H134 . . . 120.0 ? C134 C135 C136 . . . 119.7(10) ? C134 C135 H135 . . . 120.1 ? C136 C135 H135 . . . 120.2 ? C131 C136 C135 . . . 120.4(11) ? C131 C136 H136 . . . 120.1 ? C135 C136 H136 . . . 119.5 ? C13 C14 C15 . . . 108.0(9) ? C13 C14 H14 . . . 127.0 ? C15 C14 H14 . . . 125.0 ? N11 C15 C14 . . . 108.6(8) ? N11 C15 C151 . . . 121.3(9) ? C14 C15 C151 . . . 130.0(9) ? C15 C151 C152 . . . 121.5(10) ? C15 C151 C156 . . . 122.2(10) ? C152 C151 C156 . . . 116.3(11) ? C151 C152 C153 . . . 121.8(12) ? C151 C152 H152 . . . 118.6 ? C153 C152 H152 . . . 119.4 ? C152 C153 C154 . . . 119.6(13) ? C152 C153 H153 . . . 118.4 ? C154 C153 H153 . . . 121.8 ? C153 C154 C155 . . . 120.3(13) ? C153 C154 H154 . . . 120.2 ? C155 C154 H154 . . . 119.2 ? C154 C155 C156 . . . 119.7(12) ? C154 C155 H155 . . . 119.0 ? C156 C155 H155 . . . 121.0 ? C151 C156 C155 . . . 122.2(11) ? C151 C156 H156 . . . 117.5 ? C155 C156 H156 . . . 120.2 ? Er1 N21 N22 . . . 73.3(4) ? Er1 N21 C25 . . . 170.4(7) ? N22 N21 C25 . . . 109.4(8) ? Er1 N22 N21 . . . 71.0(5) ? Er1 N22 C23 . . . 168.2(7) ? N21 N22 C23 . . . 106.6(8) ? N22 C23 C231 . . . 120.7(9) ? N22 C23 C24 . . . 110.5(9) ? C231 C23 C24 . . . 128.7(9) ? C23 C231 C232 . . . 120.9(9) ? C23 C231 C236 . . . 122.8(11) ? C232 C231 C236 . . . 116.3(11) ? C231 C232 C233 . . . 119.1(11) ? C231 C232 H232 . . . 120.2 ? C233 C232 H232 . . . 120.6 ? C232 C233 C234 . . . 119.4(15) ? C232 C233 H233 . . . 120.2 ? C234 C233 H233 . . . 120.4 ? C233 C234 C235 . . . 120.6(15) ? C233 C234 H234 . . . 115.5 ? C235 C234 H234 . . . 123.9 ? C234 C235 C236 . . . 121.2(14) ? C234 C235 H235 . . . 115.6 ? C236 C235 H235 . . . 123.0 ? C231 C236 C235 . . . 123.3(14) ? C231 C236 H236 . . . 117.8 ? C235 C236 H236 . . . 118.9 ? C23 C24 C25 . . . 105.1(9) ? C23 C24 H24 . . . 126.9 ? C25 C24 H24 . . . 127.9 ? N21 C25 C24 . . . 108.3(9) ? N21 C25 C251 . . . 120.8(9) ? C24 C25 C251 . . . 130.9(9) ? C25 C251 C252 . . . 118.7(9) ? C25 C251 C256 . . . 121.5(10) ? C252 C251 C256 . . . 119.8(11) ? C251 C252 C253 . . . 121.1(11) ? C251 C252 H252 . . . 118.9 ? C253 C252 H252 . . . 119.9 ? C252 C253 C254 . . . 118.8(12) ? C252 C253 H253 . . . 120.1 ? C254 C253 H253 . . . 121.1 ? C253 C254 C255 . . . 121.0(13) ? C253 C254 H254 . . . 119.4 ? C255 C254 H254 . . . 119.6 ? C254 C255 C256 . . . 118.9(12) ? C254 C255 H255 . . . 118.5 ? C256 C255 H255 . . . 122.5 ? C251 C256 C255 . . . 120.2(13) ? C251 C256 H256 . . . 120.0 ? C255 C256 H256 . . . 119.8 ? Er1 N31 Er2 . . . 92.8(3) ? Er1 N31 N32 . . . 75.3(5) ? Er1 N31 C35 . . . 140.0(6) ? Er2 N31 N32 . . . 68.0(4) ? Er2 N31 C35 . . . 126.0(6) ? N32 N31 C35 . . . 108.0(7) ? Er1 N32 Er2 . . . 95.2(3) ? Er1 N32 N31 . . . 71.0(5) ? Er1 N32 C33 . . . 138.3(6) ? Er2 N32 N31 . . . 79.5(5) ? Er2 N32 C33 . . . 126.0(7) ? N31 N32 C33 . . . 107.2(8) ? N32 C33 C331 . . . 118.3(10) ? N32 C33 C34 . . . 107.5(9) ? C331 C33 C34 . . . 134.2(10) ? C33 C331 C332 . . . 121.5(11) ? C33 C331 C336 . . . 122.4(13) ? C332 C331 C336 . . . 116.1(13) ? C331 C332 C333 . . . 124.5(15) ? C331 C332 H332 . . . 114.0 ? C333 C332 H332 . . . 121.4 ? C332 C333 C334 . . . 116.5(18) ? C332 C333 H333 . . . 119.5 ? C334 C333 H333 . . . 124.0 ? C333 C334 C335 . . . 121.8(18) ? C333 C334 H334 . . . 114 ? C335 C334 H334 . . . 124 ? C334 C335 C336 . . . 120.2(18) ? C334 C335 H335 . . . 118 ? C336 C335 H335 . . . 122 ? C331 C336 C335 . . . 120.7(16) ? C331 C336 H336 . . . 118.9 ? C335 C336 H336 . . . 120.4 ? C33 C34 C35 . . . 109.4(9) ? C33 C34 H34 . . . 123.3 ? C35 C34 H34 . . . 127.3 ? N31 C35 C34 . . . 107.8(9) ? N31 C35 C351 . . . 119.8(9) ? C34 C35 C351 . . . 132.4(10) ? C35 C351 C352 . . . 122.6(11) ? C35 C351 C356 . . . 119.4(10) ? C352 C351 C356 . . . 117.9(11) ? C351 C352 C353 . . . 122.6(12) ? C351 C352 H352 . . . 118.9 ? C353 C352 H352 . . . 118.4 ? C352 C353 C354 . . . 119.7(13) ? C352 C353 H353 . . . 122.4 ? C354 C353 H353 . . . 117.8 ? C353 C354 C355 . . . 119.9(14) ? C353 C354 H354 . . . 118.8 ? C355 C354 H354 . . . 121.3 ? C354 C355 C356 . . . 119.7(15) ? C354 C355 H355 . . . 119.0 ? C356 C355 H355 . . . 121.4 ? C351 C356 C355 . . . 120.2(12) ? C351 C356 H356 . . . 120.0 ? C355 C356 H356 . . . 119.9 ? Er1 N41 Er2 . . . 91.0(3) ? Er1 N41 N42 . . . 72.2(4) ? Er1 N41 C45 . . . 129.0(6) ? Er2 N41 N42 . . . 67.5(5) ? Er2 N41 C45 . . . 136.3(6) ? N42 N41 C45 . . . 104.8(7) ? Er1 N42 Er2 . . . 95.2(3) ? Er1 N42 N41 . . . 74.1(5) ? Er1 N42 C43 . . . 124.2(7) ? Er2 N42 N41 . . . 78.8(4) ? Er2 N42 C43 . . . 140.4(7) ? N41 N42 C43 . . . 106.6(8) ? N42 C43 C431 . . . 120.1(9) ? N42 C43 C44 . . . 111.2(8) ? C431 C43 C44 . . . 128.6(8) ? C43 C431 C432 . . . 119.7(8) ? C43 C431 C436 . . . 120.3(9) ? C432 C431 C436 . . . 119.7(9) ? C431 C432 C433 . . . 120.7(10) ? C431 C432 H432 . . . 120.5 ? C433 C432 H432 . . . 118.8 ? C432 C433 C434 . . . 121.1(12) ? C432 C433 H433 . . . 121.5 ? C434 C433 H433 . . . 117.4 ? C433 C434 C435 . . . 118.9(11) ? C433 C434 H434 . . . 123.1 ? C435 C434 H434 . . . 118.0 ? C434 C435 C436 . . . 119.3(11) ? C434 C435 H435 . . . 120.3 ? C436 C435 H435 . . . 120.4 ? C431 C436 C435 . . . 120.3(11) ? C431 C436 H436 . . . 118.1 ? C435 C436 H436 . . . 121.5 ? C43 C44 C45 . . . 104.0(8) ? C43 C44 H44 . . . 128.6 ? C45 C44 H44 . . . 127.3 ? N41 C45 C44 . . . 113.0(9) ? N41 C45 C451 . . . 115.5(8) ? C44 C45 C451 . . . 131.2(9) ? C45 C451 C452 . . . 122.3(10) ? C45 C451 C456 . . . 119.3(9) ? C452 C451 C456 . . . 118.3(10) ? C451 C452 C453 . . . 122.4(12) ? C451 C452 H452 . . . 116.7 ? C453 C452 H452 . . . 120.8 ? C452 C453 C454 . . . 119.0(12) ? C452 C453 H453 . . . 119.3 ? C454 C453 H453 . . . 121.6 ? C453 C454 C455 . . . 118.3(13) ? C453 C454 H454 . . . 122.2 ? C455 C454 H454 . . . 119.5 ? C454 C455 C456 . . . 124.4(15) ? C454 C455 H455 . . . 117.4 ? C456 C455 H455 . . . 118.2 ? C451 C456 C455 . . . 117.2(11) ? C451 C456 H456 . . . 119.1 ? C455 C456 H456 . . . 123.7 ? Er2 N51 N52 . . . 72.8(5) ? Er2 N51 C55 . . . 166.4(7) ? N52 N51 C55 . . . 106.8(8) ? Er2 N52 N51 . . . 71.5(5) ? Er2 N52 C53 . . . 166.4(7) ? N51 N52 C53 . . . 110.4(8) ? N52 C53 C531 . . . 123.4(10) ? N52 C53 C54 . . . 108.2(9) ? C531 C53 C54 . . . 128.5(11) ? C53 C531 C532 . . . 120.8(11) ? C53 C531 C536 . . . 120.7(12) ? C532 C531 C536 . . . 118.5(11) ? C531 C532 C533 . . . 120.2(12) ? C531 C532 H532 . . . 117.9 ? C533 C532 H532 . . . 121.8 ? C532 C533 C534 . . . 124.5(14) ? C532 C533 H533 . . . 116.0 ? C534 C533 H533 . . . 119.5 ? C533 C534 C535 . . . 116.4(13) ? C533 C534 H534 . . . 115.9 ? C535 C534 H534 . . . 127.7 ? C534 C535 C536 . . . 119.5(14) ? C534 C535 H535 . . . 121.3 ? C536 C535 H535 . . . 119.1 ? C531 C536 C535 . . . 120.9(14) ? C531 C536 H536 . . . 119.6 ? C535 C536 H536 . . . 119.5 ? C53 C54 C55 . . . 105.9(10) ? C53 C54 H54 . . . 126.1 ? C55 C54 H54 . . . 128.0 ? N51 C55 C54 . . . 108.8(8) ? N51 C55 C551 . . . 123.0(9) ? C54 C55 C551 . . . 128.2(10) ? C55 C551 C552 . . . 119.9(10) ? C55 C551 C556 . . . 122.6(11) ? C552 C551 C556 . . . 117.5(11) ? C551 C552 C553 . . . 120.8(13) ? C551 C552 H552 . . . 120.4 ? C553 C552 H552 . . . 118.8 ? C552 C553 C554 . . . 118.3(15) ? C552 C553 H553 . . . 122.2 ? C554 C553 H553 . . . 119.4 ? C553 C554 C555 . . . 122.4(15) ? C553 C554 H554 . . . 121 ? C555 C554 H554 . . . 116.4 ? C554 C555 C556 . . . 118.6(14) ? C554 C555 H555 . . . 120.7 ? C556 C555 H555 . . . 120.6 ? C551 C556 C555 . . . 122.2(14) ? C551 C556 H556 . . . 118.6 ? C555 C556 H556 . . . 119.1 ? Er2 N61 N62 . . . 71.6(5) ? Er2 N61 C65 . . . 179.1(8) ? N62 N61 C65 . . . 107.8(8) ? Er2 N62 N61 . . . 73.3(5) ? Er2 N62 C63 . . . 177.8(7) ? N61 N62 C63 . . . 107.8(8) ? N62 C63 C631 . . . 121.0(9) ? N62 C63 C64 . . . 109.8(8) ? C631 C63 C64 . . . 129.0(9) ? C63 C631 C632 . . . 118.3(10) ? C63 C631 C636 . . . 120.8(11) ? C632 C631 C636 . . . 120.9(12) ? C631 C632 C633 . . . 119.2(13) ? C631 C632 H632 . . . 122.0 ? C633 C632 H632 . . . 118.8 ? C632 C633 C634 . . . 119.0(16) ? C632 C633 H633 . . . 121.1 ? C634 C633 H633 . . . 119.7 ? C633 C634 C635 . . . 121.3(15) ? C633 C634 H634 . . . 118 ? C635 C634 H634 . . . 120.2 ? C634 C635 C636 . . . 119.2(15) ? C634 C635 H635 . . . 119.7 ? C636 C635 H635 . . . 121.0 ? C631 C636 C635 . . . 120.3(14) ? C631 C636 H636 . . . 119.6 ? C635 C636 H636 . . . 120.1 ? C63 C64 C65 . . . 105.3(9) ? C63 C64 H64 . . . 127.0 ? C65 C64 H64 . . . 127.7 ? N61 C65 C64 . . . 109.3(9) ? N61 C65 C651 . . . 118.3(9) ? C64 C65 C651 . . . 132.4(9) ? C65 C651 C652 . . . 124.2(9) ? C65 C651 C656 . . . 118.1(10) ? C652 C651 C656 . . . 117.7(10) ? C651 C652 C653 . . . 123.0(11) ? C651 C652 H652 . . . 118.8 ? C653 C652 H652 . . . 118.2 ? C652 C653 C654 . . . 118.5(12) ? C652 C653 H653 . . . 121.1 ? C654 C653 H653 . . . 120.4 ? C653 C654 C655 . . . 121.0(12) ? C653 C654 H654 . . . 120.3 ? C655 C654 H654 . . . 118.7 ? C654 C655 C656 . . . 120.9(11) ? C654 C655 H655 . . . 119.7 ? C656 C655 H655 . . . 119.4 ? C651 C656 C655 . . . 118.8(12) ? C651 C656 H656 . . . 119.9 ? C655 C656 H656 . . . 121.3 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 3304 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min -39 _reflns_limit_l_max 40 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 16.025 _diffrn_reflns_av_sigmaI/netI .067 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .147 _refine_ls_wR_factor_all .192 _refine_ls_goodness_of_fit_all 1.957 _refine_ls_shift/su_mean .0003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #===END data_lupza _database_code_depnum_ccdc_archive 'CCDC 190716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Hexakis(3,5-diphenylpyrazolato)dilutetium(III) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H66 Lu2 N12' _chemical_formula_weight 1665.5 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7838(2) _cell_length_b 18.9626(4) _cell_length_c 30.0967(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.180(1) _cell_angle_gamma 90.00 _cell_volume 7222(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used N/A _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 2.776 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_A_min 0.73 _exptl_absorpt_correction_A_max 0.76 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Enraf Nonius CCD ; _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number N/A? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64198 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.84 _reflns_number_total 16054 _reflns_number_gt 12620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Siemans, 1994)' _computing_publication_material ? _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^)+(0.0897P)^2^+17.0682P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16054 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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 Lu1 Lu 0.19185(2) 0.305879(13) 0.367238(9) 0.01546(9) Uani 1 1 d . . . Lu2 Lu 0.42453(2) 0.204660(13) 0.366751(9) 0.01652(9) Uani 1 1 d . . . N11 N 0.1536(4) 0.3728(3) 0.42419(18) 0.0195(11) Uani 1 1 d . . . N12 N 0.1773(4) 0.4177(3) 0.39095(18) 0.0196(12) Uani 1 1 d . . . C13 C 0.1682(5) 0.4847(3) 0.4048(2) 0.0187(13) Uani 1 1 d . . . C14 C 0.1382(5) 0.4835(3) 0.4479(2) 0.0224(14) Uani 1 1 d . . . H14 H 0.1258 0.5230 0.4658 0.027 Uiso 1 1 calc R . . C15 C 0.1305(5) 0.4128(3) 0.4588(2) 0.0190(13) Uani 1 1 d . . . N21 N 0.0720(5) 0.3092(3) 0.30619(18) 0.0187(12) Uani 1 1 d . . . N22 N 0.0296(4) 0.2657(3) 0.33697(18) 0.0188(11) Uani 1 1 d . . . C23 C -0.0560(5) 0.2340(3) 0.3156(2) 0.0223(14) Uani 1 1 d . . . C24 C -0.0718(5) 0.2562(4) 0.2708(2) 0.0253(15) Uani 1 1 d . . . H24 H -0.1270 0.2419 0.2481 0.030 Uiso 1 1 calc R . . C25 C 0.0093(5) 0.3033(3) 0.2661(2) 0.0199(14) Uani 1 1 d . . . N31 N 0.3522(4) 0.3257(3) 0.33907(18) 0.0198(11) Uani 1 1 d . . . N32 N 0.3813(4) 0.3228(3) 0.38634(18) 0.0197(12) Uani 1 1 d . . . C33 C 0.4512(5) 0.3755(3) 0.3983(2) 0.0220(14) Uani 1 1 d . . . C34 C 0.4701(5) 0.4115(3) 0.3604(2) 0.0231(15) Uani 1 1 d . . . H34 H 0.5165 0.4504 0.3595 0.028 Uiso 1 1 calc R . . C35 C 0.4090(5) 0.3803(3) 0.3241(2) 0.0209(14) Uani 1 1 d . . . N41 N 0.2515(4) 0.1898(3) 0.39767(18) 0.0184(11) Uani 1 1 d . . . N42 N 0.2406(4) 0.1865(3) 0.35028(18) 0.0173(11) Uani 1 1 d . . . C43 C 0.1736(5) 0.1330(3) 0.3374(2) 0.0190(13) Uani 1 1 d . . . C44 C 0.1439(5) 0.1006(3) 0.3751(2) 0.0216(14) Uani 1 1 d . . . H44 H 0.0969 0.0618 0.3756 0.026 Uiso 1 1 calc R . . C45 C 0.1967(5) 0.1363(3) 0.4121(2) 0.0210(14) Uani 1 1 d . . . N51 N 0.4974(5) 0.2031(3) 0.30306(19) 0.0224(12) Uani 1 1 d . . . N52 N 0.5613(4) 0.2437(3) 0.33449(19) 0.0200(11) Uani 1 1 d . . . C53 C 0.6296(5) 0.2812(4) 0.3131(3) 0.0247(15) Uani 1 1 d . . . C54 C 0.6080(5) 0.2649(4) 0.2673(2) 0.0245(15) Uani 1 1 d . . . H54 H 0.6431 0.2834 0.2441 0.029 Uiso 1 1 calc R . . C55 C 0.5252(6) 0.2165(4) 0.2624(2) 0.0228(14) Uani 1 1 d . . . N61 N 0.4456(4) 0.0926(3) 0.39216(18) 0.0206(12) Uani 1 1 d . . . N62 N 0.5100(5) 0.1371(3) 0.42102(19) 0.0231(12) Uani 1 1 d . . . C63 C 0.5647(5) 0.0958(4) 0.4530(2) 0.0213(14) Uani 1 1 d . . . C64 C 0.5357(5) 0.0263(4) 0.4461(2) 0.0235(15) Uani 1 1 d . . . H64 H 0.5611 -0.0131 0.4640 0.028 Uiso 1 1 calc R . . C65 C 0.4611(6) 0.0259(3) 0.4073(2) 0.0231(14) Uani 1 1 d . . . C131 C 0.1979(5) 0.5438(4) 0.3775(2) 0.0213(14) Uani 1 1 d . . . C132 C 0.2466(6) 0.5315(3) 0.3391(2) 0.0263(15) Uani 1 1 d . . . H132 H 0.2575 0.4845 0.3299 0.032 Uiso 1 1 calc R . . C133 C 0.2787(6) 0.5876(4) 0.3147(3) 0.0318(17) Uani 1 1 d . . . H133 H 0.3122 0.5790 0.2890 0.038 Uiso 1 1 calc R . . C134 C 0.2616(6) 0.6567(4) 0.3281(3) 0.0309(17) Uani 1 1 d . . . H134 H 0.2829 0.6951 0.3111 0.037 Uiso 1 1 calc R . . C135 C 0.2144(6) 0.6699(4) 0.3655(3) 0.0302(17) Uani 1 1 d . . . H135 H 0.2043 0.7172 0.3745 0.036 Uiso 1 1 calc R . . C136 C 0.1811(5) 0.6140(3) 0.3902(2) 0.0250(15) Uani 1 1 d . . . H136 H 0.1471 0.6232 0.4157 0.030 Uiso 1 1 calc R . . C151 C 0.1092(5) 0.3788(4) 0.5008(2) 0.0223(14) Uani 1 1 d . . . C152 C 0.0852(7) 0.3075(4) 0.5026(3) 0.037(2) Uani 1 1 d . . . H152 H 0.0790 0.2799 0.4760 0.044 Uiso 1 1 calc R . . C153 C 0.0704(8) 0.2764(5) 0.5422(3) 0.045(2) Uani 1 1 d . . . H153 H 0.0546 0.2276 0.5429 0.054 Uiso 1 1 calc R . . C154 C 0.0786(7) 0.3161(5) 0.5814(3) 0.043(2) Uani 1 1 d . . . H154 H 0.0697 0.2941 0.6090 0.051 Uiso 1 1 calc R . . C155 C 0.0995(7) 0.3872(5) 0.5801(3) 0.042(2) Uani 1 1 d . . . H155 H 0.1044 0.4146 0.6067 0.051 Uiso 1 1 calc R . . C156 C 0.1135(7) 0.4188(4) 0.5396(2) 0.0359(19) Uani 1 1 d . . . H156 H 0.1260 0.4682 0.5385 0.043 Uiso 1 1 calc R . . C231 C -0.1165(5) 0.1842(3) 0.3396(3) 0.0248(16) Uani 1 1 d . . . C232 C -0.0990(6) 0.1766(4) 0.3856(3) 0.0311(17) Uani 1 1 d . . . H232 H -0.0449 0.2038 0.4025 0.037 Uiso 1 1 calc R . . C233 C -0.1558(7) 0.1320(4) 0.4075(3) 0.045(2) Uani 1 1 d . . . H233 H -0.1410 0.1270 0.4392 0.054 Uiso 1 1 calc R . . C234 C -0.2374(7) 0.0929(5) 0.3826(4) 0.051(3) Uani 1 1 d . . . H234 H -0.2793 0.0619 0.3975 0.061 Uiso 1 1 calc R . . C235 C -0.2561(7) 0.0998(4) 0.3369(4) 0.044(2) Uani 1 1 d . . . H235 H -0.3109 0.0730 0.3201 0.053 Uiso 1 1 calc R . . C236 C -0.1968(6) 0.1447(4) 0.3153(3) 0.0322(17) Uani 1 1 d . . . H236 H -0.2104 0.1490 0.2835 0.039 Uiso 1 1 calc R . . C251 C 0.0327(5) 0.3454(4) 0.2278(2) 0.0222(14) Uani 1 1 d . . . C252 C 0.0947(6) 0.4057(4) 0.2350(2) 0.0282(16) Uani 1 1 d . . . H252 H 0.1228 0.4190 0.2647 0.034 Uiso 1 1 calc R . . C253 C 0.1159(6) 0.4466(4) 0.1989(3) 0.0354(19) Uani 1 1 d . . . H253 H 0.1590 0.4874 0.2043 0.042 Uiso 1 1 calc R . . C254 C 0.0756(7) 0.4289(5) 0.1562(3) 0.041(2) Uani 1 1 d . . . H254 H 0.0887 0.4579 0.1319 0.049 Uiso 1 1 calc R . . C255 C 0.0153(7) 0.3683(5) 0.1484(3) 0.047(2) Uani 1 1 d . . . H255 H -0.0129 0.3558 0.1185 0.057 Uiso 1 1 calc R . . C256 C -0.0043(7) 0.3262(5) 0.1834(3) 0.0392(19) Uani 1 1 d . . . H256 H -0.0432 0.2838 0.1774 0.047 Uiso 1 1 calc R . . C331 C 0.4886(6) 0.3860(4) 0.4464(3) 0.0307(17) Uani 1 1 d . . . C332 C 0.4316(7) 0.3604(5) 0.4785(3) 0.042(2) Uani 1 1 d . . . H332 H 0.3688 0.3343 0.4693 0.051 Uiso 1 1 calc R . . C333 C 0.4637(9) 0.3716(6) 0.5234(3) 0.058(3) Uani 1 1 d . . . H333 H 0.4232 0.3532 0.5449 0.069 Uiso 1 1 calc R . . C334 C 0.5540(8) 0.4093(6) 0.5373(4) 0.064(3) Uani 1 1 d . . . H334 H 0.5760 0.4176 0.5684 0.077 Uiso 1 1 calc R . . C335 C 0.6106(8) 0.4342(6) 0.5067(4) 0.062(3) Uani 1 1 d . . . H335 H 0.6736 0.4598 0.5164 0.074 Uiso 1 1 calc R . . C336 C 0.5792(6) 0.4232(5) 0.4602(3) 0.046(2) Uani 1 1 d . . . H336 H 0.6204 0.4414 0.4390 0.055 Uiso 1 1 calc R . . C351 C 0.3998(5) 0.3935(4) 0.2751(2) 0.0254(15) Uani 1 1 d . . . C352 C 0.3436(6) 0.3499(4) 0.2437(3) 0.0306(17) Uani 1 1 d . . . H352 H 0.3061 0.3110 0.2535 0.037 Uiso 1 1 calc R . . C353 C 0.3408(7) 0.3613(5) 0.1988(3) 0.041(2) Uani 1 1 d . . . H353 H 0.3017 0.3303 0.1778 0.049 Uiso 1 1 calc R . . C354 C 0.3940(7) 0.4174(5) 0.1835(3) 0.042(2) Uani 1 1 d . . . H354 H 0.3928 0.4247 0.1522 0.050 Uiso 1 1 calc R . . C355 C 0.4491(7) 0.4627(5) 0.2141(3) 0.048(2) Uani 1 1 d . . . H355 H 0.4856 0.5018 0.2038 0.058 Uiso 1 1 calc R . . C356 C 0.4515(6) 0.4516(4) 0.2601(3) 0.0358(19) Uani 1 1 d . . . H356 H 0.4884 0.4835 0.2810 0.043 Uiso 1 1 calc R . . C431 C 0.1375(5) 0.1210(3) 0.2895(2) 0.0204(14) Uani 1 1 d . . . C432 C 0.1764(6) 0.1626(4) 0.2571(2) 0.0278(16) Uani 1 1 d . . . H432 H 0.2320 0.1951 0.2660 0.033 Uiso 1 1 calc R . . C433 C 0.1348(6) 0.1570(4) 0.2124(3) 0.0343(18) Uani 1 1 d . . . H433 H 0.1613 0.1858 0.1907 0.041 Uiso 1 1 calc R . . C434 C 0.0537(6) 0.1090(4) 0.1991(3) 0.0344(18) Uani 1 1 d . . . H434 H 0.0235 0.1055 0.1685 0.041 Uiso 1 1 calc R . . C435 C 0.0181(7) 0.0667(4) 0.2309(3) 0.0383(19) Uani 1 1 d . . . H435 H -0.0358 0.0330 0.2221 0.046 Uiso 1 1 calc R . . C436 C 0.0599(6) 0.0728(4) 0.2758(3) 0.0321(17) Uani 1 1 d . . . H436 H 0.0344 0.0432 0.2973 0.039 Uiso 1 1 calc R . . C451 C 0.1973(5) 0.1237(3) 0.4604(2) 0.0225(14) Uani 1 1 d . . . C452 C 0.2808(6) 0.1501(4) 0.4908(2) 0.0321(17) Uani 1 1 d . . . H452 H 0.3354 0.1767 0.4803 0.038 Uiso 1 1 calc R . . C453 C 0.2842(6) 0.1375(5) 0.5369(3) 0.038(2) Uani 1 1 d . . . H453 H 0.3410 0.1551 0.5577 0.046 Uiso 1 1 calc R . . C454 C 0.2041(7) 0.0992(5) 0.5516(3) 0.042(2) Uani 1 1 d . . . H454 H 0.2063 0.0902 0.5828 0.051 Uiso 1 1 calc R . . C455 C 0.1204(7) 0.0739(4) 0.5215(3) 0.040(2) Uani 1 1 d . . . H455 H 0.0651 0.0482 0.5320 0.048 Uiso 1 1 calc R . . C456 C 0.1178(6) 0.0862(4) 0.4753(3) 0.0314(17) Uani 1 1 d . . . H456 H 0.0609 0.0686 0.4545 0.038 Uiso 1 1 calc R . . C531 C 0.7089(5) 0.3275(4) 0.3377(3) 0.0253(15) Uani 1 1 d . . . C532 C 0.7411(6) 0.3216(4) 0.3833(3) 0.0325(18) Uani 1 1 d . . . H532 H 0.7077 0.2883 0.4002 0.039 Uiso 1 1 calc R . . C533 C 0.8201(6) 0.3629(5) 0.4042(3) 0.041(2) Uani 1 1 d . . . H533 H 0.8421 0.3567 0.4355 0.050 Uiso 1 1 calc R . . C534 C 0.8681(7) 0.4124(5) 0.3821(4) 0.049(3) Uani 1 1 d . . . H534 H 0.9228 0.4408 0.3976 0.059 Uiso 1 1 calc R . . C535 C 0.8365(7) 0.4213(4) 0.3363(4) 0.046(2) Uani 1 1 d . . . H535 H 0.8689 0.4565 0.3203 0.055 Uiso 1 1 calc R . . C536 C 0.7583(6) 0.3793(4) 0.3141(3) 0.0362(19) Uani 1 1 d . . . H536 H 0.7375 0.3851 0.2827 0.043 Uiso 1 1 calc R . . C551 C 0.4717(6) 0.1820(4) 0.2213(3) 0.0270(16) Uani 1 1 d . . . C552 C 0.4140(6) 0.1204(4) 0.2236(3) 0.0346(18) Uani 1 1 d . . . H552 H 0.4077 0.0998 0.2519 0.042 Uiso 1 1 calc R . . C553 C 0.3652(7) 0.0887(5) 0.1840(3) 0.047(2) Uani 1 1 d . . . H553 H 0.3269 0.0460 0.1853 0.056 Uiso 1 1 calc R . . C554 C 0.3730(8) 0.1197(6) 0.1432(3) 0.053(3) Uani 1 1 d . . . H554 H 0.3400 0.0981 0.1163 0.064 Uiso 1 1 calc R . . C555 C 0.4292(8) 0.1826(5) 0.1410(3) 0.050(2) Uani 1 1 d . . . H555 H 0.4346 0.2037 0.1127 0.060 Uiso 1 1 calc R . . C556 C 0.4760(7) 0.2134(5) 0.1797(3) 0.040(2) Uani 1 1 d . . . H556 H 0.5122 0.2569 0.1783 0.047 Uiso 1 1 calc R . . C631 C 0.6475(6) 0.1291(4) 0.4862(2) 0.0278(16) Uani 1 1 d . . . C632 C 0.6555(7) 0.2018(4) 0.4918(3) 0.0366(19) Uani 1 1 d . . . H632 H 0.6031 0.2315 0.4759 0.044 Uiso 1 1 calc R . . C633 C 0.7384(7) 0.2314(5) 0.5201(3) 0.050(2) Uani 1 1 d . . . H633 H 0.7444 0.2813 0.5223 0.060 Uiso 1 1 calc R . . C634 C 0.8133(7) 0.1891(6) 0.5455(3) 0.052(3) Uani 1 1 d . . . H634 H 0.8700 0.2095 0.5651 0.063 Uiso 1 1 calc R . . C635 C 0.8030(7) 0.1156(6) 0.5415(3) 0.049(2) Uani 1 1 d . . . H635 H 0.8526 0.0860 0.5591 0.059 Uiso 1 1 calc R . . C636 C 0.7217(6) 0.0855(4) 0.5123(3) 0.0356(18) Uani 1 1 d . . . H636 H 0.7161 0.0357 0.5098 0.043 Uiso 1 1 calc R . . C651 C 0.4029(5) -0.0329(3) 0.3841(2) 0.0236(15) Uani 1 1 d . . . C652 C 0.3290(6) -0.0211(4) 0.3455(2) 0.0275(16) Uani 1 1 d . . . H652 H 0.3174 0.0255 0.3343 0.033 Uiso 1 1 calc R . . C653 C 0.2730(6) -0.0764(4) 0.3237(3) 0.0361(19) Uani 1 1 d . . . H653 H 0.2223 -0.0672 0.2981 0.043 Uiso 1 1 calc R . . C654 C 0.2900(7) -0.1451(4) 0.3389(3) 0.039(2) Uani 1 1 d . . . H654 H 0.2520 -0.1831 0.3236 0.047 Uiso 1 1 calc R . . C655 C 0.3626(7) -0.1574(4) 0.3764(3) 0.040(2) Uani 1 1 d . . . H655 H 0.3743 -0.2043 0.3870 0.048 Uiso 1 1 calc R . . C656 C 0.4200(6) -0.1018(4) 0.3992(3) 0.0320(18) Uani 1 1 d . . . H656 H 0.4702 -0.1112 0.4250 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Lu1 0.01955(17) 0.01233(13) 0.01449(14) -0.00063(9) 0.00232(11) -0.00130(10) Lu2 0.01890(16) 0.01234(14) 0.01816(15) 0.00110(9) 0.00212(11) -0.00151(10) N11 0.027(3) 0.016(3) 0.017(3) -0.001(2) 0.005(2) -0.003(2) N12 0.026(3) 0.013(3) 0.019(3) 0.000(2) 0.003(2) 0.000(2) C13 0.020(3) 0.014(3) 0.021(3) -0.002(2) -0.002(3) 0.002(2) C14 0.021(4) 0.020(3) 0.026(4) -0.006(3) 0.004(3) 0.000(3) C15 0.016(3) 0.020(3) 0.021(3) -0.005(2) 0.002(3) 0.003(2) N21 0.029(3) 0.012(2) 0.015(3) 0.0004(19) 0.002(2) -0.001(2) N22 0.024(3) 0.013(3) 0.021(3) 0.000(2) 0.007(2) -0.004(2) C23 0.025(4) 0.017(3) 0.026(4) 0.001(3) 0.008(3) 0.003(3) C24 0.022(4) 0.023(3) 0.029(4) -0.007(3) 0.000(3) 0.005(3) C25 0.017(3) 0.020(3) 0.022(3) -0.002(2) 0.000(3) 0.001(2) N31 0.025(3) 0.016(3) 0.020(3) 0.000(2) 0.007(2) 0.003(2) N32 0.026(3) 0.013(2) 0.020(3) -0.002(2) 0.000(2) -0.001(2) C33 0.018(3) 0.020(3) 0.027(4) 0.000(3) -0.002(3) -0.002(3) C34 0.022(4) 0.014(3) 0.033(4) 0.001(3) 0.002(3) -0.001(3) C35 0.018(3) 0.012(3) 0.034(4) 0.004(3) 0.010(3) 0.001(2) N41 0.021(3) 0.017(3) 0.018(3) 0.001(2) 0.005(2) -0.004(2) N42 0.021(3) 0.015(2) 0.016(3) 0.003(2) 0.005(2) -0.002(2) C43 0.022(3) 0.010(3) 0.027(4) -0.001(2) 0.008(3) 0.003(2) C44 0.025(4) 0.011(3) 0.030(4) -0.002(3) 0.007(3) -0.002(3) C45 0.023(4) 0.016(3) 0.025(4) 0.007(3) 0.004(3) -0.002(3) N51 0.034(3) 0.017(3) 0.016(3) 0.001(2) 0.004(2) 0.001(2) N52 0.017(3) 0.017(3) 0.025(3) 0.000(2) 0.003(2) 0.002(2) C53 0.017(3) 0.020(3) 0.038(4) 0.003(3) 0.007(3) 0.005(3) C54 0.023(4) 0.024(3) 0.028(4) 0.001(3) 0.011(3) 0.004(3) C55 0.026(4) 0.021(3) 0.024(4) -0.001(3) 0.010(3) 0.005(3) N61 0.026(3) 0.015(3) 0.021(3) 0.003(2) 0.005(2) 0.000(2) N62 0.029(3) 0.018(3) 0.021(3) 0.001(2) -0.001(2) -0.001(2) C63 0.018(3) 0.027(3) 0.019(3) 0.003(3) 0.004(3) 0.004(3) C64 0.022(4) 0.026(3) 0.025(4) 0.009(3) 0.011(3) 0.007(3) C65 0.028(4) 0.019(3) 0.025(4) 0.004(3) 0.012(3) 0.001(3) C131 0.023(4) 0.019(3) 0.021(3) -0.002(2) -0.004(3) -0.004(3) C132 0.036(4) 0.015(3) 0.029(4) 0.001(3) 0.007(3) 0.002(3) C133 0.036(4) 0.031(4) 0.030(4) 0.005(3) 0.010(3) 0.000(3) C134 0.040(4) 0.021(4) 0.032(4) 0.009(3) 0.005(3) -0.005(3) C135 0.036(4) 0.012(3) 0.040(4) 0.000(3) -0.002(3) 0.002(3) C136 0.031(4) 0.016(3) 0.027(4) -0.005(3) 0.004(3) -0.001(3) C151 0.026(4) 0.023(3) 0.017(3) -0.001(3) 0.003(3) 0.002(3) C152 0.062(6) 0.025(4) 0.026(4) -0.004(3) 0.018(4) -0.002(4) C153 0.066(6) 0.029(4) 0.045(5) 0.004(4) 0.022(5) 0.000(4) C154 0.055(6) 0.049(5) 0.029(4) 0.013(4) 0.021(4) 0.004(4) C155 0.060(6) 0.045(5) 0.025(4) -0.007(4) 0.015(4) -0.011(4) C156 0.052(5) 0.033(4) 0.025(4) -0.006(3) 0.014(4) -0.006(4) C231 0.014(3) 0.016(3) 0.047(5) -0.001(3) 0.012(3) 0.004(3) C232 0.021(4) 0.040(4) 0.036(4) -0.001(3) 0.015(3) -0.012(3) C233 0.047(5) 0.034(5) 0.059(6) 0.010(4) 0.024(5) 0.003(4) C234 0.035(5) 0.031(4) 0.096(8) 0.014(5) 0.041(6) 0.007(4) C235 0.029(5) 0.026(4) 0.083(7) -0.008(4) 0.026(5) -0.008(3) C236 0.024(4) 0.024(4) 0.050(5) -0.003(3) 0.011(4) 0.000(3) C251 0.019(3) 0.027(4) 0.021(3) 0.002(3) 0.003(3) 0.004(3) C252 0.033(4) 0.026(4) 0.027(4) 0.004(3) 0.006(3) 0.006(3) C253 0.032(4) 0.033(4) 0.044(5) 0.009(4) 0.016(4) 0.011(3) C254 0.047(5) 0.047(5) 0.030(4) 0.015(4) 0.014(4) 0.024(4) C255 0.055(6) 0.072(7) 0.012(4) 0.003(4) -0.002(4) 0.013(5) C256 0.040(5) 0.047(5) 0.028(4) 0.004(4) -0.003(4) 0.000(4) C331 0.033(4) 0.026(4) 0.030(4) -0.010(3) -0.004(3) 0.002(3) C332 0.055(6) 0.045(5) 0.023(4) -0.001(3) -0.009(4) -0.004(4) C333 0.071(7) 0.069(7) 0.030(5) -0.004(5) -0.003(5) 0.000(6) C334 0.055(7) 0.093(9) 0.038(6) -0.019(6) -0.015(5) 0.016(6) C335 0.038(6) 0.070(7) 0.067(7) -0.034(6) -0.028(5) 0.003(5) C336 0.029(5) 0.049(5) 0.057(6) -0.019(4) -0.002(4) -0.002(4) C351 0.023(4) 0.025(4) 0.031(4) 0.010(3) 0.014(3) 0.012(3) C352 0.033(4) 0.030(4) 0.030(4) 0.005(3) 0.007(3) 0.006(3) C353 0.041(5) 0.052(5) 0.027(4) 0.001(4) 0.001(4) 0.008(4) C354 0.040(5) 0.062(6) 0.026(4) 0.017(4) 0.015(4) 0.019(4) C355 0.034(5) 0.058(6) 0.056(6) 0.029(5) 0.022(5) 0.003(4) C356 0.029(4) 0.037(4) 0.044(5) 0.010(4) 0.012(4) -0.003(3) C431 0.020(3) 0.016(3) 0.025(3) 0.000(3) 0.004(3) 0.007(3) C432 0.029(4) 0.027(4) 0.027(4) -0.002(3) 0.005(3) -0.005(3) C433 0.037(5) 0.044(5) 0.024(4) 0.002(3) 0.009(3) -0.004(4) C434 0.035(4) 0.045(5) 0.022(4) -0.003(3) -0.001(3) 0.004(4) C435 0.038(5) 0.043(5) 0.034(4) -0.011(4) 0.003(4) -0.013(4) C436 0.033(4) 0.031(4) 0.033(4) -0.006(3) 0.007(3) -0.012(3) C451 0.026(4) 0.019(3) 0.024(4) 0.004(3) 0.010(3) 0.005(3) C452 0.035(4) 0.036(4) 0.026(4) 0.007(3) 0.005(3) 0.002(3) C453 0.033(5) 0.057(6) 0.024(4) 0.005(4) 0.002(3) 0.008(4) C454 0.049(5) 0.049(5) 0.032(4) 0.016(4) 0.017(4) 0.008(4) C455 0.047(5) 0.032(4) 0.044(5) 0.011(4) 0.018(4) -0.002(4) C456 0.030(4) 0.034(4) 0.034(4) 0.008(3) 0.014(3) -0.001(3) C531 0.022(4) 0.017(3) 0.038(4) -0.002(3) 0.008(3) 0.007(3) C532 0.028(4) 0.023(4) 0.047(5) 0.002(3) 0.006(4) -0.006(3) C533 0.033(5) 0.043(5) 0.046(5) -0.010(4) -0.003(4) 0.000(4) C534 0.025(4) 0.038(5) 0.086(8) -0.031(5) 0.010(5) -0.006(4) C535 0.033(5) 0.026(4) 0.083(8) -0.012(4) 0.020(5) -0.013(3) C536 0.030(4) 0.030(4) 0.051(5) -0.001(4) 0.015(4) -0.008(3) C551 0.023(4) 0.029(4) 0.030(4) -0.007(3) 0.007(3) 0.008(3) C552 0.037(4) 0.031(4) 0.036(4) -0.009(3) 0.003(4) -0.002(3) C553 0.043(5) 0.043(5) 0.052(6) -0.019(4) -0.002(4) 0.006(4) C554 0.055(6) 0.072(7) 0.032(5) -0.026(5) 0.001(4) 0.010(5) C555 0.052(6) 0.063(6) 0.034(5) -0.010(4) 0.005(4) 0.001(5) C556 0.042(5) 0.053(5) 0.025(4) -0.004(4) 0.010(4) 0.001(4) C631 0.028(4) 0.035(4) 0.021(4) 0.000(3) 0.007(3) 0.003(3) C632 0.041(5) 0.037(5) 0.029(4) -0.003(3) -0.005(4) 0.001(3) C633 0.053(6) 0.050(6) 0.042(5) -0.010(4) -0.009(4) -0.011(5) C634 0.033(5) 0.075(7) 0.045(6) -0.023(5) -0.009(4) 0.008(4) C635 0.034(5) 0.075(7) 0.033(5) -0.013(4) -0.007(4) 0.020(5) C636 0.035(4) 0.042(5) 0.029(4) -0.004(3) 0.003(3) 0.012(4) C651 0.026(4) 0.015(3) 0.034(4) -0.003(3) 0.020(3) -0.002(3) C652 0.032(4) 0.017(3) 0.035(4) -0.004(3) 0.011(3) -0.002(3) C653 0.038(5) 0.025(4) 0.047(5) -0.011(3) 0.013(4) -0.005(3) C654 0.046(5) 0.020(4) 0.056(6) -0.011(4) 0.024(4) -0.012(3) C655 0.049(5) 0.013(3) 0.063(6) 0.005(3) 0.029(5) 0.001(3) C656 0.038(4) 0.015(3) 0.047(5) 0.007(3) 0.020(4) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 N21 2.220(6) . ? Lu1 N11 2.242(5) . ? Lu1 N12 2.254(5) . ? Lu1 N22 2.275(5) . ? Lu1 N31 2.357(5) . ? Lu1 N42 2.422(5) . ? Lu1 N32 2.430(6) . ? Lu1 N41 2.462(5) . ? Lu1 Lu2 3.5418(7) . ? Lu2 N62 2.235(6) . ? Lu2 N52 2.243(5) . ? Lu2 N51 2.248(6) . ? Lu2 N61 2.261(5) . ? Lu2 N42 2.358(6) . ? Lu2 N32 2.401(5) . ? Lu2 N41 2.535(5) . ? Lu2 N31 2.568(5) . ? N11 C15 1.355(8) . ? N11 N12 1.379(7) . ? N12 C13 1.348(8) . ? C13 C14 1.403(9) . ? C13 C131 1.471(9) . ? C14 C15 1.388(9) . ? C15 C151 1.476(9) . ? N21 C25 1.355(8) . ? N21 N22 1.405(7) . ? N22 C23 1.332(9) . ? C23 C24 1.398(10) . ? C23 C231 1.473(9) . ? C24 C25 1.391(10) . ? C25 C251 1.467(9) . ? N31 C35 1.379(8) . ? N31 N32 1.420(7) . ? N32 C33 1.356(8) . ? C33 C34 1.379(9) . ? C33 C331 1.470(10) . ? C34 C35 1.383(10) . ? C35 C351 1.484(10) . ? N41 C45 1.339(8) . ? N41 N42 1.415(7) . ? N42 C43 1.347(8) . ? C43 C44 1.391(9) . ? C43 C431 1.467(9) . ? C44 C45 1.392(9) . ? C45 C451 1.473(9) . ? N51 C55 1.347(9) . ? N51 N52 1.390(8) . ? N52 C53 1.358(9) . ? C53 C54 1.400(10) . ? C53 C531 1.461(10) . ? C54 C55 1.394(10) . ? C55 C551 1.477(10) . ? N61 C65 1.350(8) . ? N61 N62 1.392(8) . ? N62 C63 1.356(8) . ? C63 C64 1.377(9) . ? C63 C631 1.488(10) . ? C64 C65 1.399(10) . ? C65 C651 1.462(10) . ? C131 C132 1.408(9) . ? C131 C136 1.409(9) . ? C132 C133 1.387(10) . ? C133 C134 1.399(10) . ? C134 C135 1.374(11) . ? C135 C136 1.397(10) . ? C151 C156 1.387(9) . ? C151 C152 1.391(10) . ? C152 C153 1.365(11) . ? C153 C154 1.390(12) . ? C154 C155 1.376(12) . ? C155 C156 1.393(11) . ? C231 C232 1.378(11) . ? C231 C236 1.393(10) . ? C232 C233 1.346(11) . ? C233 C234 1.405(14) . ? C234 C235 1.369(14) . ? C235 C236 1.365(11) . ? C251 C252 1.390(10) . ? C251 C256 1.401(10) . ? C252 C253 1.392(10) . ? C253 C254 1.356(12) . ? C254 C255 1.385(13) . ? C255 C256 1.372(12) . ? C331 C336 1.371(11) . ? C331 C332 1.379(12) . ? C332 C333 1.372(12) . ? C333 C334 1.372(15) . ? C334 C335 1.337(15) . ? C335 C336 1.414(13) . ? C351 C352 1.379(11) . ? C351 C356 1.392(10) . ? C352 C353 1.364(11) . ? C353 C354 1.376(12) . ? C354 C355 1.377(13) . ? C355 C356 1.395(12) . ? C431 C436 1.368(10) . ? C431 C432 1.400(10) . ? C432 C433 1.379(10) . ? C433 C434 1.396(11) . ? C434 C435 1.374(11) . ? C435 C436 1.383(11) . ? C451 C456 1.367(10) . ? C451 C452 1.399(10) . ? C452 C453 1.400(10) . ? C453 C454 1.379(12) . ? C454 C455 1.386(12) . ? C455 C456 1.405(11) . ? C531 C532 1.379(11) . ? C531 C536 1.414(10) . ? C532 C533 1.360(11) . ? C533 C534 1.348(13) . ? C534 C535 1.392(14) . ? C535 C536 1.375(11) . ? C551 C552 1.390(10) . ? C551 C556 1.394(11) . ? C552 C553 1.399(11) . ? C553 C554 1.378(13) . ? C554 C555 1.400(14) . ? C555 C556 1.363(12) . ? C631 C632 1.391(10) . ? C631 C636 1.409(10) . ? C632 C633 1.381(11) . ? C633 C634 1.392(13) . ? C634 C635 1.403(13) . ? C635 C636 1.385(12) . ? C651 C656 1.389(9) . ? C651 C652 1.407(10) . ? C652 C653 1.381(10) . ? C653 C654 1.388(11) . ? C654 C655 1.375(12) . ? C655 C656 1.407(11) . ? 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 N21 Lu1 N11 114.6(2) . . ? N21 Lu1 N12 99.04(19) . . ? N11 Lu1 N12 35.73(18) . . ? N21 Lu1 N22 36.41(19) . . ? N11 Lu1 N22 102.11(19) . . ? N12 Lu1 N22 109.26(19) . . ? N21 Lu1 N31 103.4(2) . . ? N11 Lu1 N31 118.71(19) . . ? N12 Lu1 N31 94.56(19) . . ? N22 Lu1 N31 134.38(19) . . ? N21 Lu1 N42 91.16(18) . . ? N11 Lu1 N42 141.36(18) . . ? N12 Lu1 N42 169.03(19) . . ? N22 Lu1 N42 81.40(19) . . ? N31 Lu1 N42 79.04(18) . . ? N21 Lu1 N32 137.71(19) . . ? N11 Lu1 N32 93.61(19) . . ? N12 Lu1 N32 85.72(19) . . ? N22 Lu1 N32 163.84(18) . . ? N31 Lu1 N32 34.47(18) . . ? N42 Lu1 N32 83.99(18) . . ? N21 Lu1 N41 118.29(18) . . ? N11 Lu1 N41 108.14(19) . . ? N12 Lu1 N41 139.31(19) . . ? N22 Lu1 N41 93.80(18) . . ? N31 Lu1 N41 92.13(18) . . ? N42 Lu1 N41 33.66(17) . . ? N32 Lu1 N41 77.56(18) . . ? N21 Lu1 Lu2 119.55(14) . . ? N11 Lu1 Lu2 125.78(14) . . ? N12 Lu1 Lu2 128.21(14) . . ? N22 Lu1 Lu2 122.39(13) . . ? N31 Lu1 Lu2 46.44(13) . . ? N42 Lu1 Lu2 41.49(13) . . ? N32 Lu1 Lu2 42.52(12) . . ? N41 Lu1 Lu2 45.70(13) . . ? N62 Lu2 N52 100.1(2) . . ? N62 Lu2 N51 113.4(2) . . ? N52 Lu2 N51 36.1(2) . . ? N62 Lu2 N61 36.07(19) . . ? N52 Lu2 N61 113.17(19) . . ? N51 Lu2 N61 103.42(19) . . ? N62 Lu2 N42 116.02(19) . . ? N52 Lu2 N42 140.59(19) . . ? N51 Lu2 N42 109.9(2) . . ? N61 Lu2 N42 90.05(19) . . ? N62 Lu2 N32 117.47(19) . . ? N52 Lu2 N32 91.12(19) . . ? N51 Lu2 N32 111.07(19) . . ? N61 Lu2 N32 144.51(19) . . ? N42 Lu2 N32 86.03(18) . . ? N62 Lu2 N41 91.69(19) . . ? N52 Lu2 N41 166.03(18) . . ? N51 Lu2 N41 143.2(2) . . ? N61 Lu2 N41 80.79(18) . . ? N42 Lu2 N41 33.36(18) . . ? N32 Lu2 N41 76.69(18) . . ? N62 Lu2 N31 149.93(19) . . ? N52 Lu2 N31 80.33(18) . . ? N51 Lu2 N31 84.78(18) . . ? N61 Lu2 N31 165.77(19) . . ? N42 Lu2 N31 76.12(18) . . ? N32 Lu2 N31 32.98(17) . . ? N41 Lu2 N31 85.71(17) . . ? N62 Lu2 Lu1 129.13(15) . . ? N52 Lu2 Lu1 122.01(13) . . ? N51 Lu2 Lu1 117.45(15) . . ? N61 Lu2 Lu1 124.58(14) . . ? N42 Lu2 Lu1 42.90(13) . . ? N32 Lu2 Lu1 43.16(13) . . ? N41 Lu2 Lu1 44.04(12) . . ? N31 Lu2 Lu1 41.68(12) . . ? C15 N11 N12 107.9(5) . . ? C15 N11 Lu1 179.5(5) . . ? N12 N11 Lu1 72.6(3) . . ? C13 N12 N11 108.7(5) . . ? C13 N12 Lu1 179.5(5) . . ? N11 N12 Lu1 71.7(3) . . ? N12 C13 C14 108.5(6) . . ? N12 C13 C131 120.4(6) . . ? C14 C13 C131 130.9(6) . . ? C15 C14 C13 105.9(6) . . ? N11 C15 C14 109.1(6) . . ? N11 C15 C151 120.1(6) . . ? C14 C15 C151 130.7(6) . . ? C25 N21 N22 107.7(5) . . ? C25 N21 Lu1 170.4(5) . . ? N22 N21 Lu1 73.9(3) . . ? C23 N22 N21 108.3(5) . . ? C23 N22 Lu1 169.9(5) . . ? N21 N22 Lu1 69.6(3) . . ? N22 C23 C24 109.0(6) . . ? N22 C23 C231 120.3(6) . . ? C24 C23 C231 130.8(7) . . ? C25 C24 C23 106.6(6) . . ? N21 C25 C24 108.4(6) . . ? N21 C25 C251 119.7(6) . . ? C24 C25 C251 131.9(6) . . ? C35 N31 N32 106.4(5) . . ? C35 N31 Lu1 139.8(4) . . ? N32 N31 Lu1 75.6(3) . . ? C35 N31 Lu2 126.5(4) . . ? N32 N31 Lu2 67.0(3) . . ? Lu1 N31 Lu2 91.87(18) . . ? C33 N32 N31 107.9(5) . . ? C33 N32 Lu2 126.0(4) . . ? N31 N32 Lu2 80.0(3) . . ? C33 N32 Lu1 139.2(4) . . ? N31 N32 Lu1 70.0(3) . . ? Lu2 N32 Lu1 94.32(18) . . ? N32 C33 C34 109.3(6) . . ? N32 C33 C331 118.1(6) . . ? C34 C33 C331 132.5(6) . . ? C33 C34 C35 107.3(6) . . ? N31 C35 C34 109.0(6) . . ? N31 C35 C351 118.8(6) . . ? C34 C35 C351 132.1(6) . . ? C45 N41 N42 108.1(5) . . ? C45 N41 Lu1 130.5(4) . . ? N42 N41 Lu1 71.6(3) . . ? C45 N41 Lu2 136.6(4) . . ? N42 N41 Lu2 66.4(3) . . ? Lu1 N41 Lu2 90.25(17) . . ? C43 N42 N41 106.9(5) . . ? C43 N42 Lu2 138.1(4) . . ? N41 N42 Lu2 80.2(3) . . ? C43 N42 Lu1 126.2(4) . . ? N41 N42 Lu1 74.7(3) . . ? Lu2 N42 Lu1 95.61(18) . . ? N42 C43 C44 109.6(6) . . ? N42 C43 C431 119.9(6) . . ? C44 C43 C431 130.4(6) . . ? C43 C44 C45 106.1(6) . . ? N41 C45 C44 109.1(6) . . ? N41 C45 C451 120.9(6) . . ? C44 C45 C451 130.0(6) . . ? C55 N51 N52 108.0(5) . . ? C55 N51 Lu2 165.4(5) . . ? N52 N51 Lu2 71.8(3) . . ? C53 N52 N51 108.8(5) . . ? C53 N52 Lu2 166.3(4) . . ? N51 N52 Lu2 72.1(3) . . ? N52 C53 C54 107.5(6) . . ? N52 C53 C531 121.4(7) . . ? C54 C53 C531 131.1(7) . . ? C55 C54 C53 107.0(6) . . ? N51 C55 C54 108.7(6) . . ? N51 C55 C551 121.9(6) . . ? C54 C55 C551 129.4(6) . . ? C65 N61 N62 108.1(5) . . ? C65 N61 Lu2 178.4(5) . . ? N62 N61 Lu2 71.0(3) . . ? C63 N62 N61 107.1(5) . . ? C63 N62 Lu2 177.9(5) . . ? N61 N62 Lu2 73.0(3) . . ? N62 C63 C64 110.1(6) . . ? N62 C63 C631 118.6(6) . . ? C64 C63 C631 131.1(6) . . ? C63 C64 C65 105.6(6) . . ? N61 C65 C64 109.0(6) . . ? N61 C65 C651 120.9(6) . . ? C64 C65 C651 130.1(6) . . ? C132 C131 C136 118.8(6) . . ? C132 C131 C13 120.8(6) . . ? C136 C131 C13 120.4(6) . . ? C133 C132 C131 120.5(6) . . ? C132 C133 C134 119.7(7) . . ? C135 C134 C133 120.8(7) . . ? C134 C135 C136 120.0(7) . . ? C135 C136 C131 120.2(7) . . ? C156 C151 C152 118.7(7) . . ? C156 C151 C15 119.4(6) . . ? C152 C151 C15 121.8(6) . . ? C153 C152 C151 120.9(7) . . ? C152 C153 C154 120.3(8) . . ? C155 C154 C153 119.8(8) . . ? C154 C155 C156 119.8(8) . . ? C151 C156 C155 120.4(7) . . ? C232 C231 C236 118.3(7) . . ? C232 C231 C23 122.7(7) . . ? C236 C231 C23 119.0(7) . . ? C233 C232 C231 122.4(8) . . ? C232 C233 C234 118.7(9) . . ? C235 C234 C233 119.8(8) . . ? C236 C235 C234 120.6(9) . . ? C235 C236 C231 120.2(8) . . ? C252 C251 C256 118.0(7) . . ? C252 C251 C25 120.0(6) . . ? C256 C251 C25 122.0(7) . . ? C251 C252 C253 120.5(7) . . ? C254 C253 C252 120.7(8) . . ? C253 C254 C255 119.6(8) . . ? C256 C255 C254 120.7(8) . . ? C255 C256 C251 120.5(8) . . ? C336 C331 C332 118.4(8) . . ? C336 C331 C33 120.8(8) . . ? C332 C331 C33 120.8(7) . . ? C333 C332 C331 121.5(9) . . ? C334 C333 C332 120.1(10) . . ? C335 C334 C333 119.2(9) . . ? C334 C335 C336 121.6(9) . . ? C331 C336 C335 119.1(9) . . ? C352 C351 C356 118.6(7) . . ? C352 C351 C35 122.6(6) . . ? C356 C351 C35 118.8(7) . . ? C353 C352 C351 121.4(8) . . ? C352 C353 C354 120.5(8) . . ? C353 C354 C355 119.4(8) . . ? C354 C355 C356 120.3(8) . . ? C351 C356 C355 119.7(8) . . ? C436 C431 C432 118.6(7) . . ? C436 C431 C43 121.0(6) . . ? C432 C431 C43 120.2(6) . . ? C433 C432 C431 120.7(7) . . ? C432 C433 C434 119.8(7) . . ? C435 C434 C433 119.2(7) . . ? C434 C435 C436 120.7(7) . . ? C431 C436 C435 120.9(7) . . ? C456 C451 C452 120.3(7) . . ? C456 C451 C45 120.7(7) . . ? C452 C451 C45 119.0(6) . . ? C451 C452 C453 120.0(7) . . ? C454 C453 C452 119.3(8) . . ? C453 C454 C455 120.8(8) . . ? C454 C455 C456 119.8(8) . . ? C451 C456 C455 119.8(8) . . ? C532 C531 C536 117.8(7) . . ? C532 C531 C53 122.9(7) . . ? C536 C531 C53 119.3(7) . . ? C533 C532 C531 120.7(8) . . ? C534 C533 C532 122.2(9) . . ? C533 C534 C535 119.0(8) . . ? C536 C535 C534 120.0(8) . . ? C535 C536 C531 120.2(9) . . ? C552 C551 C556 119.5(7) . . ? C552 C551 C55 121.1(7) . . ? C556 C551 C55 119.4(7) . . ? C551 C552 C553 119.6(8) . . ? C554 C553 C552 119.7(9) . . ? C553 C554 C555 120.6(9) . . ? C556 C555 C554 119.3(9) . . ? C555 C556 C551 121.1(9) . . ? C632 C631 C636 118.8(7) . . ? C632 C631 C63 122.3(7) . . ? C636 C631 C63 118.9(7) . . ? C633 C632 C631 121.0(8) . . ? C632 C633 C634 120.7(9) . . ? C633 C634 C635 118.5(9) . . ? C636 C635 C634 121.1(8) . . ? C635 C636 C631 119.8(8) . . ? C656 C651 C652 118.4(7) . . ? C656 C651 C65 121.0(7) . . ? C652 C651 C65 120.6(6) . . ? C653 C652 C651 120.9(7) . . ? C652 C653 C654 120.7(8) . . ? C655 C654 C653 119.0(7) . . ? C654 C655 C656 121.2(7) . . ? C651 C656 C655 119.8(8) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.272 _refine_diff_density_min -2.926 _refine_diff_density_rms 0.472 #===END data_aglapz _database_code_depnum_ccdc_archive 'CCDC 190717' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C75 H57 La1 N10' _chemical_formula_moiety ? _chemical_formula_weight 1237.26 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 20.394(3) _cell_length_b 13.793(2) _cell_length_c 21.959(4) _cell_angle_alpha 90.00000 _cell_angle_beta 104.779(3) _cell_angle_gamma 90.00000 _cell_volume 5972.6(16) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 2594 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .77 _exptl_crystal_description prism _exptl_crystal_size_max .15 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .04 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .65 _exptl_absorpt_correction_T_max .84 _diffrn_reflns_number 30212 _reflns_number_total 7716 _reflns_Friedel_coverage 0 _reflns_number_gt 5072 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.41 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .083 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .049 _refine_ls_wR_factor_ref .042 _refine_ls_goodness_of_fit_ref .945 _refine_ls_number_reflns 5072 _refine_ls_number_parameters 503 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .007 _refine_diff_density_min -1.524 _refine_diff_density_max 2.25 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 300 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' La ? 0 4 -.588 2.452 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group La .50000 .81524(2) .25000 .02406(15) Uani ? ? 1.00000 ? ? N11 .37361(14) .8341(2) .20372(13) .0280(16) Uani ? ? 1.00000 ? ? N12 .40430(14) .9150(2) .18554(13) .0267(16) Uani ? ? 1.00000 ? ? C13 .35548(18) .9705(3) .14886(16) .028(2) Uani ? ? 1.00000 ? ? C131 .37166(19) 1.0633(3) .12392(16) .029(2) Uani ? ? 1.00000 ? ? C132 .4382(2) 1.0895(3) .12592(19) .034(2) Uani ? ? 1.00000 ? ? C133 .4528(2) 1.1793(3) .10478(18) .037(2) Uani ? ? 1.00000 ? ? C134 .4010(2) 1.2438(3) .0799(2) .039(2) Uani ? ? 1.00000 ? ? C135 .3357(2) 1.2190(3) .0772(2) .041(2) Uani ? ? 1.00000 ? ? C136 .3204(2) 1.1303(3) .0989(2) .035(2) Uani ? ? 1.00000 ? ? C14 .2926(2) .9266(3) .14321(17) .031(2) Uani ? ? 1.00000 ? ? C15 .30596(17) .8412(3) .17831(16) .0272(19) Uani ? ? 1.00000 ? ? C151 .25888(19) .7696(3) .19339(16) .031(2) Uani ? ? 1.00000 ? ? C152 .2823(2) .6822(4) .2219(2) .043(2) Uani ? ? 1.00000 ? ? C153 .2384(3) .6188(4) .2408(2) .053(3) Uani ? ? 1.00000 ? ? C154 .1704(3) .6425(4) .2308(2) .052(3) Uani ? ? 1.00000 ? ? C155 .1471(2) .7285(4) .2023(2) .047(3) Uani ? ? 1.00000 ? ? C156 .1904(2) .7915(3) .18377(19) .039(2) Uani ? ? 1.00000 ? ? N21 .44860(14) .8467(2) .34964(13) .0261(16) Uani ? ? 1.00000 ? ? N22 .38133(15) .8707(2) .33697(15) .0295(17) Uani ? ? 1.00000 ? ? C23 .36044(18) .8899(3) .38951(17) .0265(19) Uani ? ? 1.00000 ? ? C231 .29066(18) .9170(3) .38818(17) .029(2) Uani ? ? 1.00000 ? ? C232 .2374(2) .9045(3) .3351(2) .042(2) Uani ? ? 1.00000 ? ? C233 .1724(2) .9352(4) .3348(2) .046(3) Uani ? ? 1.00000 ? ? C234 .1602(2) .9772(3) .3876(2) .040(2) Uani ? ? 1.00000 ? ? C235 .2126(2) .9871(3) .4414(2) .038(2) Uani ? ? 1.00000 ? ? C236 .2771(2) .9570(3) .4415(2) .031(2) Uani ? ? 1.00000 ? ? C24 .41658(19) .8782(3) .4390(2) .029(2) Uani ? ? 1.00000 ? ? C25 .47000(17) .8503(2) .41275(16) .0249(18) Uani ? ? 1.00000 ? ? C251 .53933(16) .8244(3) .44649(15) .0246(17) Uani ? ? 1.00000 ? ? C252 .57630(18) .7552(3) .42254(18) .028(2) Uani ? ? 1.00000 ? ? C253 .6405(2) .7304(3) .4570(2) .034(2) Uani ? ? 1.00000 ? ? C254 .6683(2) .7700(3) .5152(2) .037(2) Uani ? ? 1.00000 ? ? C255 .6324(2) .8378(3) .53971(19) .032(2) Uani ? ? 1.00000 ? ? C256 .5685(2) .8657(3) .50538(18) .029(2) Uani ? ? 1.00000 ? ? N32 .48740(14) .6419(2) .27642(13) .0262(15) Uani ? ? 1.00000 ? ? C33 .47987(16) .5488(3) .29258(16) .0235(18) Uani ? ? 1.00000 ? ? C331 .45497(17) .5245(3) .34803(16) .0240(19) Uani ? ? 1.00000 ? ? C332 .4196(2) .5921(3) .37475(19) .033(2) Uani ? ? 1.00000 ? ? C333 .3989(2) .5697(3) .4285(2) .039(2) Uani ? ? 1.00000 ? ? C334 .4127(2) .4793(3) .4557(2) .035(2) Uani ? ? 1.00000 ? ? C335 .4470(2) .4122(3) .4301(2) .035(2) Uani ? ? 1.00000 ? ? C336 .46814(19) .4345(3) .37654(18) .030(2) Uani ? ? 1.00000 ? ? C34 .50000 .4879(4) .25000 .026(3) Uani ? ? 1.00000 ? ? H132 .4709(16) 1.047(2) .1430(15) .018(9) Uiso ? ? 1.00000 ? ? H133 .4959(19) 1.196(3) .1065(16) .038(11) Uiso ? ? 1.00000 ? ? H134 .4131(18) 1.305(3) .0659(17) .037(11) Uiso ? ? 1.00000 ? ? H135 .2990(18) 1.258(3) .0621(17) .035(11) Uiso ? ? 1.00000 ? ? H136 .276(2) 1.117(3) .1015(18) .047(12) Uiso ? ? 1.00000 ? ? H14 .246(2) .950(3) .1184(17) .044(11) Uiso ? ? 1.00000 ? ? H152 .3268(19) .664(3) .2306(17) .036(11) Uiso ? ? 1.00000 ? ? H153 .256(2) .562(3) .261(2) .058(15) Uiso ? ? 1.00000 ? ? H154 .140(2) .600(3) .243(2) .056(13) Uiso ? ? 1.00000 ? ? H155 .102(2) .747(3) .1969(19) .049(13) Uiso ? ? 1.00000 ? ? H156 .178(2) .849(3) .1642(19) .045(13) Uiso ? ? 1.00000 ? ? H22 .353(2) .875(3) .2958(18) .045(12) Uiso ? ? 1.00000 ? ? H232 .244(2) .872(3) .3007(19) .047(13) Uiso ? ? 1.00000 ? ? H233 .138(2) .927(3) .2995(18) .041(12) Uiso ? ? 1.00000 ? ? H234 .116(2) 1.001(3) .3884(17) .042(11) Uiso ? ? 1.00000 ? ? H235 .2051(17) 1.012(3) .4818(17) .036(11) Uiso ? ? 1.00000 ? ? H236 .3103(19) .962(3) .4756(18) .039(12) Uiso ? ? 1.00000 ? ? H24 .416(2) .880(3) .482(2) .061(14) Uiso ? ? 1.00000 ? ? H252 .5546(15) .726(2) .3821(15) .015(8) Uiso ? ? 1.00000 ? ? H253 .6617(17) .692(3) .4378(16) .030(10) Uiso ? ? 1.00000 ? ? H254 .7076(18) .749(3) .5380(17) .031(11) Uiso ? ? 1.00000 ? ? H255 .6505(17) .864(2) .5781(16) .026(10) Uiso ? ? 1.00000 ? ? H256 .5466(16) .912(2) .5200(15) .017(9) Uiso ? ? 1.00000 ? ? H332 .4100(17) .649(3) .3560(16) .029(11) Uiso ? ? 1.00000 ? ? H333 .3769(17) .613(3) .4424(16) .026(11) Uiso ? ? 1.00000 ? ? H334 .4039(18) .467(3) .4930(17) .033(11) Uiso ? ? 1.00000 ? ? H335 .4593(18) .353(3) .4484(17) .032(11) Uiso ? ? 1.00000 ? ? H336 .4922(16) .388(2) .3572(14) .017(9) Uiso ? ? 1.00000 ? ? H34 .50000 .423(4) .25000 .027(15) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 La .02173(16) .02775(18) .02448(17) .00000 .00918(12) .00000 N11 .0266(16) .034(2) .0243(16) -.0007(14) .0078(13) .0007(13) N12 .0266(17) .0292(18) .0266(17) -.0005(14) .0112(14) .0000(13) C13 .027(2) .031(2) .025(2) .0046(17) .0065(16) -.0028(16) C131 .032(2) .031(2) .023(2) .0014(17) .0068(17) -.0013(16) C132 .035(2) .036(3) .033(2) .006(2) .010(2) .0060(19) C133 .038(2) .041(2) .037(2) -.007(2) .0148(19) -.004(2) C134 .051(3) .028(2) .037(2) -.003(2) .007(2) .001(2) C135 .038(3) .034(2) .046(3) .005(2) -.001(2) .002(2) C136 .032(2) .039(3) .036(2) .006(2) .009(2) -.002(2) C14 .026(2) .038(2) .028(2) .0011(18) .0056(18) -.0022(18) C15 .024(2) .037(2) .0201(19) -.0004(16) .0059(15) -.0061(15) C151 .029(2) .042(2) .020(2) -.0072(18) .0058(17) -.0049(17) C152 .041(2) .045(3) .045(3) -.001(3) .016(2) .002(2) C153 .061(3) .049(3) .051(3) -.008(3) .018(3) .014(2) C154 .048(3) .072(4) .039(3) -.028(3) .017(2) -.001(3) C155 .034(3) .070(3) .038(3) -.013(3) .011(2) -.000(2) C156 .031(2) .053(3) .029(2) -.011(2) .0021(18) -.002(2) N21 .0207(16) .033(2) .0253(17) .0034(13) .0079(14) -.0008(13) N22 .0229(17) .039(2) .0247(18) .0075(14) .0027(14) -.0008(15) C23 .025(2) .032(2) .025(2) .0012(16) .0111(16) -.0032(16) C231 .026(2) .033(2) .031(2) .0032(17) .0136(18) -.0010(17) C232 .027(2) .062(3) .035(3) .006(2) .006(2) -.010(2) C233 .023(2) .064(3) .048(3) .004(2) .001(2) -.005(2) C234 .025(2) .044(3) .053(3) .007(2) .016(2) .003(2) C235 .034(2) .039(3) .044(3) .0039(19) .019(2) -.004(2) C236 .025(2) .038(2) .031(2) .0010(18) .0100(19) -.0035(18) C24 .026(2) .035(2) .027(2) .0035(17) .0107(18) .0003(18) C25 .025(2) .025(2) .025(2) -.0001(15) .0085(16) -.0014(15) C251 .0195(17) .030(2) .0242(18) -.0024(17) .0060(14) .0050(17) C252 .022(2) .037(2) .027(2) .0008(17) .0091(17) .0003(18) C253 .030(2) .035(2) .040(3) .0052(19) .015(2) .002(2) C254 .026(2) .044(3) .039(3) -.000(2) .005(2) .007(2) C255 .027(2) .042(3) .026(2) -.0038(18) .0037(17) .0011(18) C256 .031(2) .027(2) .034(2) -.0031(18) .0156(19) -.0045(18) N32 .0254(17) .0324(18) .0224(17) .0003(13) .0089(13) -.0001(13) C33 .0182(18) .027(2) .024(2) -.0009(15) .0038(15) -.0012(16) C331 .0170(19) .028(2) .026(2) -.0053(15) .0040(16) -.0029(16) C332 .037(2) .033(3) .033(2) .002(2) .0138(19) .0037(19) C333 .035(2) .044(3) .042(3) .000(2) .021(2) -.005(2) C334 .033(2) .047(3) .028(2) -.008(2) .013(2) .001(2) C335 .034(2) .038(3) .036(2) -.002(2) .013(2) .005(2) C336 .027(2) .031(2) .036(2) -.0004(17) .0142(18) .0003(18) C34 .018(3) .033(3) .028(3) .00000 .007(2) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published La N11 . . 2.531(3) ? La N12 . . 2.509(3) ? La N21 . . 2.692(3) ? La N32 . . 2.489(3) ? La N11 . '2 655' 2.531(3) ? La N12 . '2 655' 2.509(3) ? La N21 . '2 655' 2.692(3) ? La N32 . '2 655' 2.489(3) ? N11 N12 . . 1.386(4) ? N11 C15 . . 1.353(4) ? N12 C13 . . 1.348(4) ? C13 C131 . . 1.463(5) ? C13 C14 . . 1.394(6) ? C131 C132 . . 1.394(6) ? C131 C136 . . 1.398(5) ? C132 C133 . . 1.383(6) ? C132 H132 . . .90(3) ? C133 C134 . . 1.382(6) ? C133 H133 . . .90(4) ? C134 C135 . . 1.362(7) ? C134 H134 . . .95(4) ? C135 C136 . . 1.377(6) ? C135 H135 . . .91(4) ? C136 H136 . . .94(4) ? C14 C15 . . 1.397(5) ? C14 H14 . . 1.01(4) ? C15 C151 . . 1.473(6) ? C151 C152 . . 1.385(6) ? C151 C156 . . 1.392(6) ? C152 C153 . . 1.389(8) ? C152 H152 . . .91(4) ? C153 C154 . . 1.388(8) ? C153 H153 . . .92(4) ? C154 C155 . . 1.368(7) ? C154 H154 . . .94(5) ? C155 C156 . . 1.373(7) ? C155 H155 . . .92(4) ? C156 H156 . . .90(4) ? N21 N22 . . 1.369(4) ? N21 C25 . . 1.343(4) ? N22 C23 . . 1.354(5) ? N22 H22 . . .94(4) ? C23 C231 . . 1.464(5) ? C23 C24 . . 1.372(5) ? C231 C232 . . 1.387(5) ? C231 C236 . . 1.385(6) ? C232 C233 . . 1.390(6) ? C232 H232 . . .92(4) ? C233 C234 . . 1.375(7) ? C233 H233 . . .91(3) ? C234 C235 . . 1.382(6) ? C234 H234 . . .96(4) ? C235 C236 . . 1.379(6) ? C235 H235 . . 1.00(4) ? C236 H236 . . .87(3) ? C24 C25 . . 1.410(6) ? C24 H24 . . .95(5) ? C25 C251 . . 1.463(4) ? C251 C252 . . 1.399(5) ? C251 C256 . . 1.400(5) ? C252 C253 . . 1.378(5) ? C252 H252 . . .97(3) ? C253 C254 . . 1.374(6) ? C253 H253 . . .86(4) ? C254 C255 . . 1.378(6) ? C254 H254 . . .88(3) ? C255 C256 . . 1.383(5) ? C255 H255 . . .90(3) ? C256 H256 . . .89(3) ? N32 C33 . . 1.352(5) ? N32 N32 . '2 655' 1.384(4) ? C33 C331 . . 1.473(5) ? C33 C34 . . 1.395(5) ? C331 C332 . . 1.396(6) ? C331 C336 . . 1.385(5) ? C332 C333 . . 1.385(7) ? C332 H332 . . .89(3) ? C333 C334 . . 1.380(6) ? C333 H333 . . .85(4) ? C334 C335 . . 1.365(6) ? C334 H334 . . .90(4) ? C335 C336 . . 1.386(6) ? C335 H335 . . .91(4) ? C336 H336 . . .97(3) ? C34 H34 . . .90(5) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 La N12 . . . 31.93(10) ? N11 La N21 . . . 75.05(9) ? N11 La N32 . . . 92.13(9) ? N11 La N11 . . '2 655' 168.20(9) ? N11 La N12 . . '2 655' 137.39(10) ? N11 La N21 . . '2 655' 102.99(9) ? N11 La N32 . . '2 655' 99.22(9) ? N12 La N21 . . . 87.82(9) ? N12 La N32 . . . 123.11(9) ? N12 La N11 . . '2 655' 137.39(10) ? N12 La N12 . . '2 655' 113.52(9) ? N12 La N21 . . '2 655' 82.02(9) ? N12 La N32 . . '2 655' 120.45(9) ? N21 La N32 . . . 83.15(9) ? N21 La N11 . . '2 655' 102.99(9) ? N21 La N12 . . '2 655' 82.02(9) ? N21 La N21 . . '2 655' 161.43(9) ? N21 La N32 . . '2 655' 115.42(9) ? N32 La N11 . . '2 655' 99.22(9) ? N32 La N12 . . '2 655' 120.45(9) ? N32 La N21 . . '2 655' 115.42(9) ? N32 La N32 . . '2 655' 32.28(10) ? N11 La N12 '2 655' . '2 655' 31.93(10) ? N11 La N21 '2 655' . '2 655' 75.05(9) ? N11 La N32 '2 655' . '2 655' 92.13(9) ? N12 La N21 '2 655' . '2 655' 87.82(9) ? N12 La N32 '2 655' . '2 655' 123.11(9) ? N21 La N32 '2 655' . '2 655' 83.15(9) ? La N11 N12 . . . 73.15(16) ? La N11 C15 . . . 178.1(2) ? N12 N11 C15 . . . 108.1(3) ? La N12 N11 . . . 74.93(16) ? La N12 C13 . . . 176.5(3) ? N11 N12 C13 . . . 108.1(3) ? N12 C13 C131 . . . 121.2(3) ? N12 C13 C14 . . . 109.2(3) ? C131 C13 C14 . . . 129.5(3) ? C13 C131 C132 . . . 121.7(3) ? C13 C131 C136 . . . 120.6(4) ? C132 C131 C136 . . . 117.7(4) ? C131 C132 C133 . . . 120.9(4) ? C131 C132 H132 . . . 117(2) ? C133 C132 H132 . . . 122(2) ? C132 C133 C134 . . . 120.1(4) ? C132 C133 H133 . . . 121(2) ? C134 C133 H133 . . . 119(2) ? C133 C134 C135 . . . 119.7(4) ? C133 C134 H134 . . . 118(2) ? C135 C134 H134 . . . 123(2) ? C134 C135 C136 . . . 120.9(4) ? C134 C135 H135 . . . 125(2) ? C136 C135 H135 . . . 114(2) ? C131 C136 C135 . . . 120.7(4) ? C131 C136 H136 . . . 119(2) ? C135 C136 H136 . . . 120(2) ? C13 C14 C15 . . . 105.8(3) ? C13 C14 H14 . . . 128(2) ? C15 C14 H14 . . . 126(2) ? N11 C15 C14 . . . 108.8(3) ? N11 C15 C151 . . . 120.9(3) ? C14 C15 C151 . . . 130.1(3) ? C15 C151 C152 . . . 121.0(4) ? C15 C151 C156 . . . 120.4(4) ? C152 C151 C156 . . . 118.4(4) ? C151 C152 C153 . . . 120.5(4) ? C151 C152 H152 . . . 123(2) ? C153 C152 H152 . . . 116(2) ? C152 C153 C154 . . . 120.0(5) ? C152 C153 H153 . . . 118(3) ? C154 C153 H153 . . . 122(3) ? C153 C154 C155 . . . 119.5(5) ? C153 C154 H154 . . . 121(3) ? C155 C154 H154 . . . 120(3) ? C154 C155 C156 . . . 120.7(5) ? C154 C155 H155 . . . 121(3) ? C156 C155 H155 . . . 118(3) ? C151 C156 C155 . . . 120.9(4) ? C151 C156 H156 . . . 115(3) ? C155 C156 H156 . . . 124(3) ? La N21 N22 . . . 116.8(2) ? La N21 C25 . . . 138.8(2) ? N22 N21 C25 . . . 104.2(3) ? N21 N22 C23 . . . 113.0(3) ? N21 N22 H22 . . . 123(3) ? C23 N22 H22 . . . 124(3) ? N22 C23 C231 . . . 123.3(3) ? N22 C23 C24 . . . 105.7(3) ? C231 C23 C24 . . . 131.0(4) ? C23 C231 C232 . . . 122.3(4) ? C23 C231 C236 . . . 119.2(3) ? C232 C231 C236 . . . 118.6(4) ? C231 C232 C233 . . . 120.5(4) ? C231 C232 H232 . . . 120(2) ? C233 C232 H232 . . . 120(2) ? C232 C233 C234 . . . 120.2(4) ? C232 C233 H233 . . . 119(3) ? C234 C233 H233 . . . 121(3) ? C233 C234 C235 . . . 119.7(4) ? C233 C234 H234 . . . 122(2) ? C235 C234 H234 . . . 118(2) ? C234 C235 C236 . . . 120.1(4) ? C234 C235 H235 . . . 122(2) ? C236 C235 H235 . . . 118(2) ? C231 C236 C235 . . . 120.9(3) ? C231 C236 H236 . . . 119(3) ? C235 C236 H236 . . . 121(3) ? C23 C24 C25 . . . 106.5(4) ? C23 C24 H24 . . . 124(3) ? C25 C24 H24 . . . 128(3) ? N21 C25 C24 . . . 110.5(3) ? N21 C25 C251 . . . 122.1(3) ? C24 C25 C251 . . . 127.4(3) ? C25 C251 C252 . . . 121.3(3) ? C25 C251 C256 . . . 119.8(3) ? C252 C251 C256 . . . 118.8(3) ? C251 C252 C253 . . . 119.4(3) ? C251 C252 H252 . . . 117.7(18) ? C253 C252 H252 . . . 122.9(19) ? C252 C253 C254 . . . 121.3(4) ? C252 C253 H253 . . . 114(2) ? C254 C253 H253 . . . 124(2) ? C253 C254 C255 . . . 120.0(4) ? C253 C254 H254 . . . 120(2) ? C255 C254 H254 . . . 120(2) ? C254 C255 C256 . . . 119.7(4) ? C254 C255 H255 . . . 120(2) ? C256 C255 H255 . . . 120(2) ? C251 C256 C255 . . . 120.7(4) ? C251 C256 H256 . . . 119.5(18) ? C255 C256 H256 . . . 119.7(18) ? La N32 C33 . . . 178.0(3) ? La N32 N32 . . '2 655' 73.86(17) ? C33 N32 N32 . . '2 655' 108.1(3) ? N32 C33 C331 . . . 121.3(3) ? N32 C33 C34 . . . 108.9(3) ? C331 C33 C34 . . . 129.8(4) ? C33 C331 C332 . . . 121.3(3) ? C33 C331 C336 . . . 120.7(3) ? C332 C331 C336 . . . 118.0(4) ? C331 C332 C333 . . . 120.7(4) ? C331 C332 H332 . . . 118(3) ? C333 C332 H332 . . . 121(3) ? C332 C333 C334 . . . 119.9(4) ? C332 C333 H333 . . . 117(3) ? C334 C333 H333 . . . 123(3) ? C333 C334 C335 . . . 120.2(4) ? C333 C334 H334 . . . 120(2) ? C335 C334 H334 . . . 120(2) ? C334 C335 C336 . . . 120.1(4) ? C334 C335 H335 . . . 122(3) ? C336 C335 H335 . . . 117(3) ? C331 C336 C335 . . . 121.1(4) ? C331 C336 H336 . . . 117(2) ? C335 C336 H336 . . . 122(2) ? C33 C34 H34 . . . 127.1(2) ? C33 C34 C33 . . '2 655' 105.9(4) ? H34 C34 C33 . . '2 655' 127.1(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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2536 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -30 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .724 _reflns_d_resolution_low 11.277 _diffrn_reflns_av_sigmaI/netI .148 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .095 _refine_ls_wR_factor_all .049 _refine_ls_goodness_of_fit_all .892 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_ag46b3 _database_code_depnum_ccdc_archive 'CCDC 190718' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C75 H57 N10 Nd1' _chemical_formula_moiety ? _chemical_formula_weight 1242.59 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 20.328(2) _cell_length_b 13.805(2) _cell_length_c 21.940(2) _cell_angle_alpha 90.00000 _cell_angle_beta 104.535(2) _cell_angle_gamma 90.00000 _cell_volume 5959.9(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7478 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .926 _exptl_crystal_description bar _exptl_crystal_size_max .25 _exptl_crystal_size_mid .07 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .735 _exptl_absorpt_correction_T_max .862 _diffrn_reflns_number 29675 _reflns_number_total 7576 _reflns_Friedel_coverage 0 _reflns_number_gt 6233 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.27 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .0400 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .034 _refine_ls_goodness_of_fit_ref .989 _refine_ls_number_reflns 6233 _refine_ls_number_parameters 390 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .038 _refine_diff_density_min -.551 _refine_diff_density_max 1.381 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 300 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Nd ? 0 4 -.535 3.018 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nd .50000 .813077(12) .25000 .02139(8) Uani ? ? 1.00000 ? ? N11 .37667(9) .83097(13) .20440(8) .0252(9) Uani ? ? 1.00000 ? ? N12 .40773(9) .91185(13) .18680(8) .0241(9) Uani ? ? 1.00000 ? ? C13 .35900(11) .96777(16) .15006(10) .0251(10) Uani ? ? 1.00000 ? ? C131 .37509(11) 1.06114(16) .12534(10) .0266(11) Uani ? ? 1.00000 ? ? C132 .44199(12) 1.08717(17) .12724(11) .0318(12) Uani ? ? 1.00000 ? ? C133 .45628(13) 1.17722(18) .10540(12) .0350(12) Uani ? ? 1.00000 ? ? C134 .40437(14) 1.24153(18) .08079(12) .0380(13) Uani ? ? 1.00000 ? ? C135 .33804(14) 1.21686(19) .07843(13) .0404(13) Uani ? ? 1.00000 ? ? C136 .32345(12) 1.12802(18) .10046(12) .0354(12) Uani ? ? 1.00000 ? ? C14 .29579(11) .92364(17) .14382(10) .0290(11) Uani ? ? 1.00000 ? ? C15 .30907(11) .83798(16) .17875(10) .0257(11) Uani ? ? 1.00000 ? ? C151 .26158(12) .76660(18) .19365(10) .0294(11) Uani ? ? 1.00000 ? ? C152 .28485(14) .6793(2) .22251(13) .0406(13) Uani ? ? 1.00000 ? ? C153 .24024(16) .6167(2) .24147(14) .0524(17) Uani ? ? 1.00000 ? ? C154 .17242(15) .6394(2) .23118(13) .0508(16) Uani ? ? 1.00000 ? ? C155 .14865(13) .7258(2) .20194(12) .0463(15) Uani ? ? 1.00000 ? ? C156 .19253(13) .7890(2) .18326(11) .0378(13) Uani ? ? 1.00000 ? ? N21 .44979(9) .84578(13) .34792(8) .0231(8) Uani ? ? 1.00000 ? ? N22 .38248(9) .86914(14) .33564(8) .0252(9) Uani ? ? 1.00000 ? ? C23 .36175(11) .88803(16) .38813(10) .0260(11) Uani ? ? 1.00000 ? ? C231 .29167(11) .91474(16) .38741(11) .0273(11) Uani ? ? 1.00000 ? ? C232 .23840(12) .9017(2) .33441(12) .0387(13) Uani ? ? 1.00000 ? ? C233 .17325(12) .9318(2) .33431(13) .0445(14) Uani ? ? 1.00000 ? ? C234 .16068(12) .97342(19) .38763(13) .0391(13) Uani ? ? 1.00000 ? ? C235 .21285(12) .98282(18) .44132(12) .0358(13) Uani ? ? 1.00000 ? ? C236 .27806(11) .95407(17) .44137(11) .0289(11) Uani ? ? 1.00000 ? ? C24 .41829(11) .87706(17) .43782(10) .0267(11) Uani ? ? 1.00000 ? ? C25 .47160(11) .84961(16) .41119(10) .0224(10) Uani ? ? 1.00000 ? ? C251 .54094(10) .82337(15) .44541(10) .0228(10) Uani ? ? 1.00000 ? ? C252 .57784(11) .75305(16) .42258(10) .0256(10) Uani ? ? 1.00000 ? ? C253 .64206(11) .72697(18) .45723(11) .0298(11) Uani ? ? 1.00000 ? ? C254 .66953(11) .76808(19) .51568(11) .0327(12) Uani ? ? 1.00000 ? ? C255 .63329(12) .83768(18) .53893(11) .0314(12) Uani ? ? 1.00000 ? ? C256 .56985(11) .86634(17) .50376(11) .0282(11) Uani ? ? 1.00000 ? ? N32 .48728(9) .64405(13) .27637(8) .0234(9) Uani ? ? 1.00000 ? ? C33 .47963(10) .55138(15) .29242(9) .0213(10) Uani ? ? 1.00000 ? ? C331 .45442(10) .52704(15) .34802(10) .0225(10) Uani ? ? 1.00000 ? ? C332 .41942(12) .59484(17) .37507(11) .0311(12) Uani ? ? 1.00000 ? ? C333 .39819(12) .57160(19) .42869(12) .0359(13) Uani ? ? 1.00000 ? ? C334 .41155(12) .48058(19) .45588(11) .0346(13) Uani ? ? 1.00000 ? ? C335 .44556(12) .41286(18) .42908(12) .0335(12) Uani ? ? 1.00000 ? ? C336 .46678(11) .43548(17) .37578(11) .0285(11) Uani ? ? 1.00000 ? ? C34 .50000 .4902(2) .25000 .0236(14) Uani ? ? 1.00000 ? ? H132 .47847 1.04195 .14365 .04000 Uiso ? ? 1.00000 ? ? H133 .50226 1.19479 .10748 .04300 Uiso ? ? 1.00000 ? ? H134 .41483 1.30277 .06511 .04800 Uiso ? ? 1.00000 ? ? H135 .30183 1.26157 .06110 .05100 Uiso ? ? 1.00000 ? ? H136 .27695 1.11134 .09877 .04400 Uiso ? ? 1.00000 ? ? H14 .25225 .94740 .12051 .03600 Uiso ? ? 1.00000 ? ? H152 .33205 .66232 .22944 .05100 Uiso ? ? 1.00000 ? ? H153 .25730 .55704 .26187 .06700 Uiso ? ? 1.00000 ? ? H154 .14191 .59537 .24421 .06000 Uiso ? ? 1.00000 ? ? H155 .10114 .74208 .19494 .05700 Uiso ? ? 1.00000 ? ? H156 .17575 .84938 .16293 .04800 Uiso ? ? 1.00000 ? ? H22 .35386 .87245 .29511 .03100 Uiso ? ? 1.00000 ? ? H232 .24721 .87259 .29741 .04900 Uiso ? ? 1.00000 ? ? H233 .13678 .92227 .29721 .05400 Uiso ? ? 1.00000 ? ? H234 .11574 .99687 .38672 .04800 Uiso ? ? 1.00000 ? ? H235 .20408 1.00980 .47946 .04500 Uiso ? ? 1.00000 ? ? H236 .31471 .96102 .47873 .03600 Uiso ? ? 1.00000 ? ? H24 .42074 .88659 .48199 .03300 Uiso ? ? 1.00000 ? ? H252 .55837 .72254 .38286 .03200 Uiso ? ? 1.00000 ? ? H253 .66778 .67905 .44090 .03700 Uiso ? ? 1.00000 ? ? H254 .71367 .74895 .54004 .04000 Uiso ? ? 1.00000 ? ? H255 .65232 .86567 .57959 .03900 Uiso ? ? 1.00000 ? ? H256 .54568 .91724 .51933 .03600 Uiso ? ? 1.00000 ? ? H332 .41021 .65817 .35619 .03800 Uiso ? ? 1.00000 ? ? H333 .37415 .61953 .44691 .04400 Uiso ? ? 1.00000 ? ? H334 .39697 .46447 .49324 .04500 Uiso ? ? 1.00000 ? ? H335 .45470 .34977 .44757 .04200 Uiso ? ? 1.00000 ? ? H336 .49077 .38768 .35761 .03500 Uiso ? ? 1.00000 ? ? H34 .50000 .42064 .25000 .02900 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nd .02094(9) .02311(9) .02169(9) .00000 .00826(6) .00000 N11 .0248(9) .0309(11) .0206(9) -.0014(7) .0068(7) .0009(7) N12 .0262(10) .0247(10) .0233(9) -.0012(7) .0094(8) -.0006(7) C13 .0247(11) .0290(12) .0211(11) .0028(9) .0046(9) -.0019(9) C131 .0308(12) .0267(12) .0220(11) .0014(9) .0062(9) -.0031(9) C132 .0335(13) .0327(13) .0304(13) .0043(10) .0100(10) .0016(10) C133 .0366(13) .0357(14) .0336(13) -.0051(11) .0107(10) -.0020(11) C134 .0524(16) .0283(13) .0319(13) -.0025(12) .0079(12) .0015(11) C135 .0425(15) .0327(14) .0409(15) .0056(11) .0009(12) .0041(11) C136 .0309(13) .0355(14) .0372(14) .0038(10) .0039(11) -.0001(11) C14 .0248(12) .0355(13) .0254(12) .0020(10) .0037(9) -.0006(10) C15 .0245(11) .0332(13) .0194(11) -.0015(9) .0052(9) -.0031(9) C151 .0299(12) .0384(14) .0201(11) -.0085(10) .0067(9) -.0045(10) C152 .0392(14) .0429(16) .0415(15) -.0048(12) .0134(11) .0035(12) C153 .062(2) .0464(18) .0511(18) -.0135(15) .0193(15) .0094(14) C154 .0514(18) .067(2) .0368(15) -.0287(15) .0169(13) -.0013(14) C155 .0310(14) .073(2) .0349(14) -.0177(13) .0085(11) -.0067(14) C156 .0312(13) .0528(17) .0273(12) -.0091(11) .0035(10) -.0044(11) N21 .0211(9) .0276(9) .0212(9) .0029(7) .0063(7) -.0015(7) N22 .0196(9) .0343(11) .0217(9) .0046(8) .0051(7) -.0016(8) C23 .0248(12) .0302(12) .0249(11) .0016(9) .0096(9) -.0025(9) C231 .0220(11) .0310(13) .0310(12) .0025(9) .0105(9) -.0007(10) C232 .0265(13) .0569(17) .0326(13) .0058(11) .0072(10) -.0088(12) C233 .0236(13) .0616(19) .0446(16) .0042(12) .0015(11) -.0038(14) C234 .0249(12) .0409(15) .0555(17) .0065(11) .0175(12) .0012(12) C235 .0323(13) .0360(14) .0453(15) .0018(11) .0210(11) -.0046(11) C236 .0260(12) .0329(13) .0301(12) -.0002(10) .0113(10) -.0019(10) C24 .0278(12) .0320(13) .0218(11) .0011(9) .0090(9) -.0015(9) C25 .0229(11) .0223(10) .0235(11) .0004(8) .0086(9) -.0010(9) C251 .0207(10) .0256(12) .0231(10) -.0006(9) .0074(8) .0019(9) C252 .0263(12) .0264(12) .0251(11) .0001(9) .0082(9) .0014(9) C253 .0250(12) .0314(12) .0353(13) .0043(10) .0122(10) .0041(10) C254 .0209(11) .0427(14) .0338(13) .0003(10) .0053(10) .0101(11) C255 .0281(12) .0398(14) .0251(12) -.0062(10) .0044(9) .0007(10) C256 .0280(12) .0285(13) .0288(12) -.0011(10) .0085(10) -.0020(10) N32 .0254(10) .0257(9) .0208(9) .0002(8) .0091(8) -.0005(7) C33 .0186(10) .0239(11) .0226(11) -.0015(8) .0072(8) .0007(9) C331 .0187(10) .0263(12) .0230(11) -.0035(8) .0064(8) -.0001(9) C332 .0349(13) .0290(13) .0326(13) .0006(10) .0142(10) .0016(10) C333 .0359(14) .0396(15) .0383(14) -.0005(11) .0207(11) -.0029(11) C334 .0334(13) .0442(15) .0299(13) -.0048(11) .0150(11) .0019(11) C335 .0328(13) .0347(14) .0351(13) -.0032(10) .0126(10) .0084(11) C336 .0277(12) .0288(12) .0312(12) -.0003(10) .0114(10) .0020(10) C34 .0188(15) .0270(16) .0252(16) .00000 .0059(12) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Nd N11 . . 2.4675(18) ? Nd N12 . . 2.4484(17) ? Nd N21 . . 2.639(2) ? Nd N32 . . 2.4335(19) ? Nd N11 . '2 655' 2.4675(18) ? Nd N12 . '2 655' 2.4484(17) ? Nd N21 . '2 655' 2.639(2) ? Nd N32 . '2 655' 2.4335(19) ? N11 N12 . . 1.385(3) ? N11 C15 . . 1.351(3) ? N12 C13 . . 1.351(3) ? C13 C131 . . 1.467(3) ? C13 C14 . . 1.397(3) ? C131 C132 . . 1.397(3) ? C131 C136 . . 1.402(3) ? C132 C133 . . 1.389(4) ? C132 H132 . . .967 ? C133 C134 . . 1.381(3) ? C133 H133 . . .956 ? C134 C135 . . 1.379(4) ? C134 H134 . . .957 ? C135 C136 . . 1.378(4) ? C135 H135 . . .963 ? C136 H136 . . .965 ? C14 C15 . . 1.398(3) ? C14 H14 . . .962 ? C15 C151 . . 1.472(3) ? C151 C152 . . 1.388(4) ? C151 C156 . . 1.399(3) ? C152 C153 . . 1.390(4) ? C152 H152 . . .962 ? C153 C154 . . 1.376(4) ? C153 H153 . . .960 ? C154 C155 . . 1.382(4) ? C154 H154 . . .962 ? C155 C156 . . 1.382(4) ? C155 H155 . . .966 ? C156 H156 . . .966 ? N21 N22 . . 1.365(2) ? N21 C25 . . 1.348(3) ? N22 C23 . . 1.347(3) ? N22 H22 . . .9337 ? C23 C231 . . 1.468(3) ? C23 C24 . . 1.380(3) ? C231 C232 . . 1.388(3) ? C231 C236 . . 1.392(3) ? C232 C233 . . 1.387(4) ? C232 H232 . . .962 ? C233 C234 . . 1.383(4) ? C233 H233 . . .963 ? C234 C235 . . 1.379(3) ? C234 H234 . . .965 ? C235 C236 . . 1.383(3) ? C235 H235 . . .972 ? C236 H236 . . .964 ? C24 C25 . . 1.406(3) ? C24 H24 . . .967 ? C25 C251 . . 1.466(3) ? C251 C252 . . 1.394(3) ? C251 C256 . . 1.399(3) ? C252 C253 . . 1.383(3) ? C252 H252 . . .959 ? C253 C254 . . 1.385(3) ? C253 H253 . . .966 ? C254 C255 . . 1.384(4) ? C254 H254 . . .959 ? C255 C256 . . 1.384(3) ? C255 H255 . . .960 ? C256 H256 . . .968 ? N32 C33 . . 1.346(3) ? N32 N32 . '2 655' 1.381(3) ? C33 C331 . . 1.476(3) ? C33 C34 . . 1.395(3) ? C331 C332 . . 1.395(3) ? C331 C336 . . 1.398(3) ? C332 C333 . . 1.388(4) ? C332 H332 . . .965 ? C333 C334 . . 1.388(4) ? C333 H333 . . .967 ? C334 C335 . . 1.379(4) ? C334 H334 . . .965 ? C335 C336 . . 1.380(4) ? C335 H335 . . .959 ? C336 H336 . . .964 ? C34 H34 . . .960 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Nd N12 . . . 32.71(6) ? N11 Nd N21 . . . 75.62(6) ? N11 Nd N32 . . . 91.98(6) ? N11 Nd N11 . . '2 655' 168.51(6) ? N11 Nd N12 . . '2 655' 136.87(6) ? N11 Nd N21 . . '2 655' 102.36(6) ? N11 Nd N32 . . '2 655' 99.06(6) ? N12 Nd N21 . . . 88.16(6) ? N12 Nd N32 . . . 123.83(6) ? N12 Nd N11 . . '2 655' 136.87(6) ? N12 Nd N12 . . '2 655' 112.31(6) ? N12 Nd N21 . . '2 655' 80.88(6) ? N12 Nd N32 . . '2 655' 120.76(6) ? N21 Nd N32 . . . 83.37(6) ? N21 Nd N11 . . '2 655' 102.36(6) ? N21 Nd N12 . . '2 655' 80.88(6) ? N21 Nd N21 . . '2 655' 160.29(6) ? N21 Nd N32 . . '2 655' 116.33(6) ? N32 Nd N11 . . '2 655' 99.06(6) ? N32 Nd N12 . . '2 655' 120.76(6) ? N32 Nd N21 . . '2 655' 116.33(6) ? N32 Nd N32 . . '2 655' 32.97(6) ? N11 Nd N12 '2 655' . '2 655' 32.71(6) ? N11 Nd N21 '2 655' . '2 655' 75.62(6) ? N11 Nd N32 '2 655' . '2 655' 91.98(6) ? N12 Nd N21 '2 655' . '2 655' 88.16(6) ? N12 Nd N32 '2 655' . '2 655' 123.83(6) ? N21 Nd N32 '2 655' . '2 655' 83.37(6) ? Nd N11 N12 . . . 72.89(10) ? Nd N11 C15 . . . 178.25(15) ? N12 N11 C15 . . . 108.26(17) ? Nd N12 N11 . . . 74.40(10) ? Nd N12 C13 . . . 177.01(16) ? N11 N12 C13 . . . 108.04(17) ? N12 C13 C131 . . . 121.63(19) ? N12 C13 C14 . . . 109.1(2) ? C131 C13 C14 . . . 129.2(2) ? C13 C131 C132 . . . 121.4(2) ? C13 C131 C136 . . . 120.5(2) ? C132 C131 C136 . . . 118.1(2) ? C131 C132 C133 . . . 120.4(2) ? C131 C132 H132 . . . 119.7 ? C133 C132 H132 . . . 119.9 ? C132 C133 C134 . . . 120.3(2) ? C132 C133 H133 . . . 119.8 ? C134 C133 H133 . . . 119.9 ? C133 C134 C135 . . . 120.0(2) ? C133 C134 H134 . . . 119.5 ? C135 C134 H134 . . . 120.6 ? C134 C135 C136 . . . 120.1(2) ? C134 C135 H135 . . . 120.0 ? C136 C135 H135 . . . 119.9 ? C131 C136 C135 . . . 121.1(2) ? C131 C136 H136 . . . 119.2 ? C135 C136 H136 . . . 119.6 ? C13 C14 C15 . . . 105.59(18) ? C13 C14 H14 . . . 127.2 ? C15 C14 H14 . . . 127.2 ? N11 C15 C14 . . . 109.0(2) ? N11 C15 C151 . . . 120.96(19) ? C14 C15 C151 . . . 129.8(2) ? C15 C151 C152 . . . 121.0(2) ? C15 C151 C156 . . . 120.2(2) ? C152 C151 C156 . . . 118.6(2) ? C151 C152 C153 . . . 120.2(3) ? C151 C152 H152 . . . 119.7 ? C153 C152 H152 . . . 120.1 ? C152 C153 C154 . . . 120.7(3) ? C152 C153 H153 . . . 119.1 ? C154 C153 H153 . . . 120.2 ? C153 C154 C155 . . . 119.5(3) ? C153 C154 H154 . . . 120.1 ? C155 C154 H154 . . . 120.5 ? C154 C155 C156 . . . 120.4(3) ? C154 C155 H155 . . . 119.6 ? C156 C155 H155 . . . 120.0 ? C151 C156 C155 . . . 120.5(2) ? C151 C156 H156 . . . 119.3 ? C155 C156 H156 . . . 120.2 ? Nd N21 N22 . . . 116.94(12) ? Nd N21 C25 . . . 138.65(14) ? N22 N21 C25 . . . 104.37(18) ? N21 N22 C23 . . . 112.96(16) ? N21 N22 H22 . . . 123.6 ? C23 N22 H22 . . . 123.42 ? N22 C23 C231 . . . 123.39(18) ? N22 C23 C24 . . . 106.1(2) ? C231 C23 C24 . . . 130.5(2) ? C23 C231 C232 . . . 121.9(2) ? C23 C231 C236 . . . 119.24(18) ? C232 C231 C236 . . . 118.9(2) ? C231 C232 C233 . . . 120.4(2) ? C231 C232 H232 . . . 119.3 ? C233 C232 H232 . . . 120.2 ? C232 C233 C234 . . . 120.1(2) ? C232 C233 H233 . . . 119.5 ? C234 C233 H233 . . . 120.4 ? C233 C234 C235 . . . 119.7(2) ? C233 C234 H234 . . . 119.8 ? C235 C234 H234 . . . 120.5 ? C234 C235 C236 . . . 120.3(3) ? C234 C235 H235 . . . 120.2 ? C236 C235 H235 . . . 119.5 ? C231 C236 C235 . . . 120.4(2) ? C231 C236 H236 . . . 119.1 ? C235 C236 H236 . . . 120.5 ? C23 C24 C25 . . . 106.1(2) ? C23 C24 H24 . . . 126.9 ? C25 C24 H24 . . . 127.0 ? N21 C25 C24 . . . 110.48(17) ? N21 C25 C251 . . . 122.9(2) ? C24 C25 C251 . . . 126.6(2) ? C25 C251 C252 . . . 121.51(18) ? C25 C251 C256 . . . 119.5(2) ? C252 C251 C256 . . . 118.91(18) ? C251 C252 C253 . . . 120.2(2) ? C251 C252 H252 . . . 119.7 ? C253 C252 H252 . . . 120.1 ? C252 C253 C254 . . . 120.5(2) ? C252 C253 H253 . . . 119.9 ? C254 C253 H253 . . . 119.6 ? C253 C254 C255 . . . 119.8(2) ? C253 C254 H254 . . . 120.4 ? C255 C254 H254 . . . 119.7 ? C254 C255 C256 . . . 120.0(2) ? C254 C255 H255 . . . 119.6 ? C256 C255 H255 . . . 120.3 ? C251 C256 C255 . . . 120.5(2) ? C251 C256 H256 . . . 119.8 ? C255 C256 H256 . . . 119.7 ? Nd N32 C33 . . . 178.35(16) ? Nd N32 N32 . . '2 655' 73.52(11) ? C33 N32 N32 . . '2 655' 108.13(18) ? N32 C33 C331 . . . 121.3(2) ? N32 C33 C34 . . . 109.2(2) ? C331 C33 C34 . . . 129.5(2) ? C33 C331 C332 . . . 121.3(2) ? C33 C331 C336 . . . 120.3(2) ? C332 C331 C336 . . . 118.4(2) ? C331 C332 C333 . . . 120.4(2) ? C331 C332 H332 . . . 119.3 ? C333 C332 H332 . . . 120.3 ? C332 C333 C334 . . . 120.3(2) ? C332 C333 H333 . . . 119.3 ? C334 C333 H333 . . . 120.4 ? C333 C334 C335 . . . 119.7(2) ? C333 C334 H334 . . . 120.3 ? C335 C334 H334 . . . 120.0 ? C334 C335 C336 . . . 120.3(2) ? C334 C335 H335 . . . 120.0 ? C336 C335 H335 . . . 119.7 ? C331 C336 C335 . . . 120.9(2) ? C331 C336 H336 . . . 119.5 ? C335 C336 H336 . . . 119.6 ? C33 C34 H34 . . . 127.30 ? C33 C34 C33 . . '2 655' 105.4(2) ? H34 C34 C33 . . '2 655' 127.3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2548 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -30 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .727 _reflns_d_resolution_low 11.276 _diffrn_reflns_av_sigmaI/netI .062 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type atomblock _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .046 _refine_ls_wR_factor_all .037 _refine_ls_goodness_of_fit_all .952 _refine_ls_shift/su_mean .003 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #===END data_gdphpz _database_code_depnum_ccdc_archive 'CCDC 190719' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C75 H57 Gd1 N10' _chemical_formula_moiety ? _chemical_formula_weight 1255.6 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 20.228(2) _cell_length_b 13.806(2) _cell_length_c 21.879(2) _cell_angle_alpha 90.00000 _cell_angle_beta 104.516(2) _cell_angle_gamma 90.00000 _cell_volume 5915.1(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_temperature 130 _exptl_absorpt_coefficient_mu 1.176 _exptl_crystal_description prism _exptl_crystal_size_max .25 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .74 _exptl_absorpt_correction_T_max .84 _diffrn_reflns_number 29610 _reflns_number_total 7602 _reflns_Friedel_coverage 0 _reflns_number_gt 6568 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.32 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .029 _refine_ls_wR_factor_ref .032 _refine_ls_goodness_of_fit_ref .978 _refine_ls_number_reflns 6568 _refine_ls_number_parameters 503 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .019 _refine_diff_density_min -.481 _refine_diff_density_max 1.457 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 300 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Gd ? 0 4 -.564 3.904 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Gd .50000 .811598(10) .25000 .01863(7) Uani ? ? 1.00000 ? ? N11 .37887(9) .82788(12) .20468(8) .0223(8) Uani ? ? 1.00000 ? ? N12 .40996(9) .90938(13) .18794(7) .0218(8) Uani ? ? 1.00000 ? ? C13 .36139(11) .96567(15) .15129(9) .0231(9) Uani ? ? 1.00000 ? ? C131 .37756(11) 1.05949(16) .12679(9) .0247(9) Uani ? ? 1.00000 ? ? C132 .44473(12) 1.08552(17) .12821(10) .0283(10) Uani ? ? 1.00000 ? ? C133 .45892(13) 1.17535(17) .10593(11) .0315(11) Uani ? ? 1.00000 ? ? C134 .40671(13) 1.23995(18) .08146(11) .0334(12) Uani ? ? 1.00000 ? ? C135 .33997(14) 1.21522(18) .07956(12) .0358(12) Uani ? ? 1.00000 ? ? C136 .32538(12) 1.12601(17) .10213(11) .0315(11) Uani ? ? 1.00000 ? ? C14 .29786(11) .92170(16) .14457(10) .0263(10) Uani ? ? 1.00000 ? ? C15 .31093(11) .83534(16) .17884(9) .0239(9) Uani ? ? 1.00000 ? ? C151 .26283(11) .76417(17) .19351(9) .0270(10) Uani ? ? 1.00000 ? ? C152 .28610(14) .67621(19) .22240(12) .0364(12) Uani ? ? 1.00000 ? ? C153 .24077(16) .6140(2) .24131(14) .0471(15) Uani ? ? 1.00000 ? ? C154 .17279(15) .6373(2) .23107(13) .0462(15) Uani ? ? 1.00000 ? ? C155 .14920(14) .7235(2) .20185(12) .0420(14) Uani ? ? 1.00000 ? ? C156 .19385(12) .7873(2) .18308(11) .0341(12) Uani ? ? 1.00000 ? ? N21 .45143(8) .84509(13) .34642(8) .0211(8) Uani ? ? 1.00000 ? ? N22 .38375(9) .86801(13) .33442(8) .0238(8) Uani ? ? 1.00000 ? ? C23 .36295(11) .88651(16) .38726(9) .0239(9) Uani ? ? 1.00000 ? ? C231 .29266(11) .91256(16) .38716(10) .0260(10) Uani ? ? 1.00000 ? ? C232 .23876(12) .8996(2) .33389(11) .0365(12) Uani ? ? 1.00000 ? ? C233 .17324(13) .9297(2) .33424(13) .0402(13) Uani ? ? 1.00000 ? ? C234 .16081(12) .97041(19) .38797(12) .0357(12) Uani ? ? 1.00000 ? ? C235 .21377(12) .97941(18) .44188(12) .0337(12) Uani ? ? 1.00000 ? ? C236 .27915(11) .95111(17) .44160(11) .0277(10) Uani ? ? 1.00000 ? ? C24 .42019(11) .87583(16) .43689(10) .0250(10) Uani ? ? 1.00000 ? ? C25 .47338(10) .84902(15) .40970(9) .0221(9) Uani ? ? 1.00000 ? ? C251 .54293(10) .82228(15) .44441(9) .0215(9) Uani ? ? 1.00000 ? ? C252 .57998(11) .75043(16) .42277(10) .0234(9) Uani ? ? 1.00000 ? ? C253 .64374(11) .72350(17) .45818(11) .0278(10) Uani ? ? 1.00000 ? ? C254 .67132(11) .76609(18) .51672(11) .0300(11) Uani ? ? 1.00000 ? ? C255 .63531(12) .83728(18) .53890(11) .0294(10) Uani ? ? 1.00000 ? ? C256 .57173(11) .86668(17) .50261(10) .0261(10) Uani ? ? 1.00000 ? ? N32 .48740(9) .64634(13) .27638(7) .0211(8) Uani ? ? 1.00000 ? ? C33 .47947(9) .55330(15) .29257(9) .0196(8) Uani ? ? 1.00000 ? ? C331 .45427(10) .52878(15) .34838(9) .0204(9) Uani ? ? 1.00000 ? ? C332 .41942(12) .59665(17) .37585(10) .0279(10) Uani ? ? 1.00000 ? ? C333 .39796(12) .57293(19) .42955(11) .0320(11) Uani ? ? 1.00000 ? ? C334 .41094(12) .48172(18) .45631(11) .0314(11) Uani ? ? 1.00000 ? ? C335 .44455(12) .41319(17) .42905(11) .0298(11) Uani ? ? 1.00000 ? ? C336 .46616(11) .43674(17) .37542(10) .0263(10) Uani ? ? 1.00000 ? ? C34 .50000 .4917(2) .25000 .0215(13) Uani ? ? 1.00000 ? ? H132 .4801(12) 1.0411(18) .1448(11) .027(6) Uiso ? ? 1.00000 ? ? H133 .5062(15) 1.1904(18) .1077(12) .035(7) Uiso ? ? 1.00000 ? ? H134 .4157(15) 1.301(2) .0651(13) .042(8) Uiso ? ? 1.00000 ? ? H135 .3027(15) 1.263(2) .0639(13) .050(8) Uiso ? ? 1.00000 ? ? H136 .2796(13) 1.1111(18) .1035(11) .033(7) Uiso ? ? 1.00000 ? ? H14 .2542(12) .9477(17) .1213(10) .025(6) Uiso ? ? 1.00000 ? ? H152 .3321(14) .6581(19) .2272(12) .033(7) Uiso ? ? 1.00000 ? ? H153 .2568(14) .554(2) .2596(13) .048(8) Uiso ? ? 1.00000 ? ? H154 .1417(14) .595(2) .2451(12) .040(7) Uiso ? ? 1.00000 ? ? H155 .1030(16) .742(2) .1961(13) .053(9) Uiso ? ? 1.00000 ? ? H156 .1774(14) .848(2) .1635(13) .042(8) Uiso ? ? 1.00000 ? ? H22 .3602(13) .8657(18) .2964(12) .029(7) Uiso ? ? 1.00000 ? ? H232 .2464(14) .871(2) .2967(13) .042(8) Uiso ? ? 1.00000 ? ? H233 .1364(17) .924(2) .2953(15) .065(9) Uiso ? ? 1.00000 ? ? H234 .1158(14) .989(2) .3881(12) .042(7) Uiso ? ? 1.00000 ? ? H235 .2053(13) 1.008(2) .4780(12) .040(7) Uiso ? ? 1.00000 ? ? H236 .3150(12) .9561(17) .4786(11) .029(6) Uiso ? ? 1.00000 ? ? H24 .4240(12) .8805(18) .4813(12) .031(7) Uiso ? ? 1.00000 ? ? H252 .5601(12) .7171(18) .3837(11) .026(6) Uiso ? ? 1.00000 ? ? H253 .6673(13) .6770(17) .4429(12) .029(7) Uiso ? ? 1.00000 ? ? H254 .7163(14) .741(2) .5435(12) .039(7) Uiso ? ? 1.00000 ? ? H255 .6545(13) .866(2) .5798(12) .035(7) Uiso ? ? 1.00000 ? ? H256 .5473(12) .9174(18) .5176(11) .026(6) Uiso ? ? 1.00000 ? ? H332 .4119(13) .657(2) .3571(11) .028(6) Uiso ? ? 1.00000 ? ? H333 .3752(13) .618(2) .4449(11) .032(7) Uiso ? ? 1.00000 ? ? H334 .3974(13) .464(2) .4920(12) .038(7) Uiso ? ? 1.00000 ? ? H335 .4558(13) .352(2) .4469(12) .038(7) Uiso ? ? 1.00000 ? ? H336 .4904(12) .3886(18) .3569(11) .027(6) Uiso ? ? 1.00000 ? ? H34 .50000 .424(3) .25000 .038(10) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Gd .01852(7) .02060(8) .01775(7) .00000 .00636(5) .00000 N11 .0225(8) .0263(10) .0187(8) -.0021(7) .0063(7) .0004(6) N12 .0226(9) .0246(9) .0192(8) -.0002(7) .0071(7) -.0004(6) C13 .0244(10) .0258(11) .0191(9) .0021(8) .0055(8) -.0023(8) C131 .0281(11) .0255(11) .0197(9) .0005(8) .0048(8) -.0022(8) C132 .0300(12) .0292(12) .0257(11) .0020(9) .0071(9) .0002(9) C133 .0325(12) .0336(13) .0295(11) -.0037(10) .0095(9) -.0017(9) C134 .0445(14) .0255(12) .0290(11) -.0035(10) .0070(10) .0014(9) C135 .0378(14) .0286(12) .0369(13) .0044(10) .0018(11) .0025(10) C136 .0286(12) .0306(12) .0332(12) .0022(9) .0035(10) .0008(9) C14 .0224(10) .0301(12) .0247(10) .0023(9) .0029(8) -.0010(9) C15 .0216(10) .0308(12) .0189(9) -.0018(8) .0042(8) -.0040(8) C151 .0271(11) .0354(13) .0181(9) -.0076(9) .0050(8) -.0048(9) C152 .0355(13) .0376(15) .0385(13) -.0046(11) .0135(11) .0012(10) C153 .0580(19) .0404(16) .0456(16) -.0097(13) .0179(13) .0083(13) C154 .0459(16) .060(2) .0353(14) -.0256(14) .0148(12) -.0012(13) C155 .0280(13) .0669(19) .0314(12) -.0177(12) .0078(10) -.0055(12) C156 .0270(12) .0477(16) .0254(11) -.0089(10) .0021(9) -.0030(10) N21 .0195(8) .0242(9) .0203(8) .0013(7) .0059(7) -.0012(7) N22 .0187(8) .0319(10) .0202(9) .0037(7) .0035(7) -.0020(7) C23 .0234(10) .0264(11) .0229(10) .0020(8) .0080(8) -.0030(8) C231 .0210(10) .0299(12) .0280(11) .0017(8) .0080(8) -.0006(8) C232 .0243(12) .0549(16) .0302(12) .0057(11) .0066(9) -.0088(11) C233 .0238(12) .0535(17) .0405(14) .0025(11) .0028(10) -.0032(12) C234 .0235(12) .0384(14) .0486(15) .0053(10) .0154(10) -.0003(11) C235 .0326(13) .0338(13) .0400(13) .0007(10) .0191(11) -.0050(10) C236 .0253(11) .0306(12) .0290(11) -.0017(9) .0100(9) -.0038(9) C24 .0250(11) .0291(11) .0216(10) .0003(8) .0073(8) -.0019(8) C25 .0224(10) .0221(10) .0222(10) -.0002(8) .0062(8) -.0005(8) C251 .0206(9) .0246(11) .0199(9) -.0004(8) .0064(7) .0035(8) C252 .0245(10) .0247(11) .0220(10) -.0001(8) .0080(8) .0015(8) C253 .0254(11) .0291(11) .0305(11) .0048(9) .0101(9) .0035(9) C254 .0204(11) .0386(13) .0297(11) -.0009(9) .0040(9) .0086(10) C255 .0262(11) .0368(13) .0236(11) -.0053(9) .0036(9) .0018(9) C256 .0267(11) .0281(12) .0245(10) .0000(9) .0080(9) -.0016(9) N32 .0229(8) .0241(9) .0178(8) -.0006(7) .0082(7) -.0013(6) C33 .0161(9) .0243(10) .0183(9) -.0017(7) .0041(7) .0016(8) C331 .0166(9) .0255(11) .0194(9) -.0042(7) .0051(7) -.0000(8) C332 .0305(12) .0267(12) .0288(11) -.0010(9) .0116(9) .0017(9) C333 .0319(12) .0352(13) .0337(12) -.0009(10) .0172(10) -.0034(10) C334 .0312(12) .0389(13) .0272(11) -.0061(10) .0132(10) .0019(10) C335 .0307(12) .0288(12) .0319(11) -.0014(9) .0118(9) .0074(9) C336 .0250(10) .0274(11) .0282(11) -.0004(9) .0099(9) .0012(9) C34 .0189(14) .0234(15) .0221(14) .00000 .0048(11) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Gd N11 . . 2.4123(17) ? Gd N12 . . 2.3966(16) ? Gd N21 . . 2.5823(19) ? Gd N32 . . 2.3827(18) ? Gd N11 . '2 655' 2.4123(17) ? Gd N12 . '2 655' 2.3966(16) ? Gd N21 . '2 655' 2.5823(19) ? Gd N32 . '2 655' 2.3827(18) ? N11 N12 . . 1.383(3) ? N11 C15 . . 1.353(3) ? N12 C13 . . 1.348(2) ? C13 C131 . . 1.470(3) ? C13 C14 . . 1.395(3) ? C131 C132 . . 1.398(3) ? C131 C136 . . 1.401(3) ? C132 C133 . . 1.389(3) ? C132 H132 . . .94(2) ? C133 C134 . . 1.383(3) ? C133 H133 . . .97(3) ? C134 C135 . . 1.383(4) ? C134 H134 . . .95(3) ? C135 C136 . . 1.386(4) ? C135 H135 . . .99(3) ? C136 H136 . . .96(3) ? C14 C15 . . 1.398(3) ? C14 H14 . . .97(2) ? C15 C151 . . 1.474(3) ? C151 C152 . . 1.395(3) ? C151 C156 . . 1.393(3) ? C152 C153 . . 1.393(4) ? C152 H152 . . .94(3) ? C153 C154 . . 1.375(4) ? C153 H153 . . .94(3) ? C154 C155 . . 1.379(4) ? C154 H154 . . .96(3) ? C155 C156 . . 1.395(4) ? C155 H155 . . .95(3) ? C156 H156 . . .96(3) ? N21 N22 . . 1.365(2) ? N21 C25 . . 1.345(3) ? N22 C23 . . 1.350(3) ? N22 H22 . . .85(2) ? C23 C231 . . 1.466(3) ? C23 C24 . . 1.383(3) ? C231 C232 . . 1.394(3) ? C231 C236 . . 1.393(3) ? C232 C233 . . 1.391(4) ? C232 H232 . . .95(3) ? C233 C234 . . 1.382(4) ? C233 H233 . . .98(3) ? C234 C235 . . 1.386(3) ? C234 H234 . . .95(3) ? C235 C236 . . 1.380(3) ? C235 H235 . . .94(3) ? C236 H236 . . .94(2) ? C24 C25 . . 1.403(3) ? C24 H24 . . .96(3) ? C25 C251 . . 1.468(3) ? C251 C252 . . 1.396(3) ? C251 C256 . . 1.402(3) ? C252 C253 . . 1.379(3) ? C252 H252 . . .97(2) ? C253 C254 . . 1.392(3) ? C253 H253 . . .91(3) ? C254 C255 . . 1.382(4) ? C254 H254 . . 1.01(2) ? C255 C256 . . 1.392(3) ? C255 H255 . . .97(2) ? C256 H256 . . .96(3) ? N32 C33 . . 1.353(3) ? N32 N32 . '2 655' 1.374(3) ? C33 C331 . . 1.475(3) ? C33 C34 . . 1.399(3) ? C331 C332 . . 1.396(3) ? C331 C336 . . 1.397(3) ? C332 C333 . . 1.390(4) ? C332 H332 . . .93(3) ? C333 C334 . . 1.386(4) ? C333 H333 . . .89(3) ? C334 C335 . . 1.384(4) ? C334 H334 . . .92(3) ? C335 C336 . . 1.389(4) ? C335 H335 . . .94(3) ? C336 H336 . . .97(3) ? C34 H34 . . .94(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Gd N12 . . . 33.41(6) ? N11 Gd N21 . . . 76.34(6) ? N11 Gd N32 . . . 91.69(6) ? N11 Gd N11 . . '2 655' 169.31(6) ? N11 Gd N12 . . '2 655' 136.87(6) ? N11 Gd N21 . . '2 655' 101.70(6) ? N11 Gd N32 . . '2 655' 98.56(6) ? N12 Gd N21 . . . 88.36(6) ? N12 Gd N32 . . . 124.36(6) ? N12 Gd N11 . . '2 655' 136.87(6) ? N12 Gd N12 . . '2 655' 111.43(6) ? N12 Gd N21 . . '2 655' 80.04(6) ? N12 Gd N32 . . '2 655' 120.96(5) ? N21 Gd N32 . . . 83.56(6) ? N21 Gd N11 . . '2 655' 101.70(6) ? N21 Gd N12 . . '2 655' 80.04(6) ? N21 Gd N21 . . '2 655' 159.37(6) ? N21 Gd N32 . . '2 655' 117.07(6) ? N32 Gd N11 . . '2 655' 98.56(6) ? N32 Gd N12 . . '2 655' 120.96(5) ? N32 Gd N21 . . '2 655' 117.07(6) ? N32 Gd N32 . . '2 655' 33.51(6) ? N11 Gd N12 '2 655' . '2 655' 33.41(6) ? N11 Gd N21 '2 655' . '2 655' 76.34(5) ? N11 Gd N32 '2 655' . '2 655' 91.69(6) ? N12 Gd N21 '2 655' . '2 655' 88.36(6) ? N12 Gd N32 '2 655' . '2 655' 124.36(6) ? N21 Gd N32 '2 655' . '2 655' 83.56(6) ? Gd N11 N12 . . . 72.67(10) ? Gd N11 C15 . . . 178.95(15) ? N12 N11 C15 . . . 108.02(16) ? Gd N12 N11 . . . 73.92(10) ? Gd N12 C13 . . . 177.21(16) ? N11 N12 C13 . . . 108.34(16) ? N12 C13 C131 . . . 121.96(18) ? N12 C13 C14 . . . 109.06(19) ? C131 C13 C14 . . . 128.93(18) ? C13 C131 C132 . . . 121.49(19) ? C13 C131 C136 . . . 120.2(2) ? C132 C131 C136 . . . 118.3(2) ? C131 C132 C133 . . . 120.5(2) ? C131 C132 H132 . . . 118.8(16) ? C133 C132 H132 . . . 120.8(16) ? C132 C133 C134 . . . 120.4(2) ? C132 C133 H133 . . . 117.8(15) ? C134 C133 H133 . . . 121.8(15) ? C133 C134 C135 . . . 119.8(2) ? C133 C134 H134 . . . 121.2(18) ? C135 C134 H134 . . . 118.9(18) ? C134 C135 C136 . . . 120.1(2) ? C134 C135 H135 . . . 119.7(19) ? C136 C135 H135 . . . 120.1(19) ? C131 C136 C135 . . . 120.8(2) ? C131 C136 H136 . . . 119.3(15) ? C135 C136 H136 . . . 119.8(15) ? C13 C14 C15 . . . 105.62(18) ? C13 C14 H14 . . . 126.0(15) ? C15 C14 H14 . . . 128.4(15) ? N11 C15 C14 . . . 109.0(2) ? N11 C15 C151 . . . 121.02(18) ? C14 C15 C151 . . . 129.7(2) ? C15 C151 C152 . . . 120.9(2) ? C15 C151 C156 . . . 120.0(2) ? C152 C151 C156 . . . 118.9(2) ? C151 C152 C153 . . . 119.9(3) ? C151 C152 H152 . . . 119.5(16) ? C153 C152 H152 . . . 120.5(16) ? C152 C153 C154 . . . 120.9(3) ? C152 C153 H153 . . . 119.1(18) ? C154 C153 H153 . . . 119.9(18) ? C153 C154 C155 . . . 119.6(3) ? C153 C154 H154 . . . 121.1(16) ? C155 C154 H154 . . . 119.4(16) ? C154 C155 C156 . . . 120.5(3) ? C154 C155 H155 . . . 121(2) ? C156 C155 H155 . . . 119(2) ? C151 C156 C155 . . . 120.2(2) ? C151 C156 H156 . . . 119.6(18) ? C155 C156 H156 . . . 120.2(18) ? Gd N21 N22 . . . 116.93(12) ? Gd N21 C25 . . . 138.87(14) ? N22 N21 C25 . . . 104.19(17) ? N21 N22 C23 . . . 113.08(16) ? N21 N22 H22 . . . 118.0(19) ? C23 N22 H22 . . . 128.8(19) ? N22 C23 C231 . . . 123.74(17) ? N22 C23 C24 . . . 105.8(2) ? C231 C23 C24 . . . 130.4(2) ? C23 C231 C232 . . . 121.7(2) ? C23 C231 C236 . . . 119.38(17) ? C232 C231 C236 . . . 119.0(2) ? C231 C232 C233 . . . 120.3(2) ? C231 C232 H232 . . . 120.5(15) ? C233 C232 H232 . . . 119.2(15) ? C232 C233 C234 . . . 120.2(2) ? C232 C233 H233 . . . 119(2) ? C234 C233 H233 . . . 120(2) ? C233 C234 C235 . . . 119.6(2) ? C233 C234 H234 . . . 119.5(15) ? C235 C234 H234 . . . 120.8(15) ? C234 C235 C236 . . . 120.5(2) ? C234 C235 H235 . . . 119.3(15) ? C236 C235 H235 . . . 120.1(15) ? C231 C236 C235 . . . 120.4(2) ? C231 C236 H236 . . . 119.3(16) ? C235 C236 H236 . . . 120.3(17) ? C23 C24 C25 . . . 105.98(19) ? C23 C24 H24 . . . 129.0(15) ? C25 C24 H24 . . . 124.9(15) ? N21 C25 C24 . . . 110.90(17) ? N21 C25 C251 . . . 123.3(2) ? C24 C25 C251 . . . 125.73(18) ? C25 C251 C252 . . . 121.98(17) ? C25 C251 C256 . . . 119.1(2) ? C252 C251 C256 . . . 118.86(18) ? C251 C252 C253 . . . 120.49(19) ? C251 C252 H252 . . . 120.0(15) ? C253 C252 H252 . . . 119.5(15) ? C252 C253 C254 . . . 120.4(2) ? C252 C253 H253 . . . 119.0(15) ? C254 C253 H253 . . . 120.6(15) ? C253 C254 C255 . . . 119.9(2) ? C253 C254 H254 . . . 119.0(16) ? C255 C254 H254 . . . 121.0(16) ? C254 C255 C256 . . . 120.0(2) ? C254 C255 H255 . . . 119.6(16) ? C256 C255 H255 . . . 120.3(16) ? C251 C256 C255 . . . 120.3(2) ? C251 C256 H256 . . . 119.7(12) ? C255 C256 H256 . . . 119.9(12) ? Gd N32 C33 . . . 178.48(16) ? Gd N32 N32 . . '2 655' 73.25(11) ? C33 N32 N32 . . '2 655' 108.27(17) ? N32 C33 C331 . . . 121.53(18) ? N32 C33 C34 . . . 109.1(2) ? C331 C33 C34 . . . 129.3(2) ? C33 C331 C332 . . . 121.25(19) ? C33 C331 C336 . . . 120.0(2) ? C332 C331 C336 . . . 118.7(2) ? C331 C332 C333 . . . 120.3(2) ? C331 C332 H332 . . . 117.4(17) ? C333 C332 H332 . . . 122.3(17) ? C332 C333 C334 . . . 120.3(2) ? C332 C333 H333 . . . 117.2(17) ? C334 C333 H333 . . . 122.5(17) ? C333 C334 C335 . . . 120.0(2) ? C333 C334 H334 . . . 122.4(17) ? C335 C334 H334 . . . 117.6(17) ? C334 C335 C336 . . . 119.8(2) ? C334 C335 H335 . . . 122.1(18) ? C336 C335 H335 . . . 118.0(18) ? C331 C336 C335 . . . 120.9(2) ? C331 C336 H336 . . . 119.8(15) ? C335 C336 H336 . . . 119.3(15) ? C33 C34 H34 . . . 127.42(13) ? C33 C34 C33 . . '2 655' 105.2(2) ? H34 C34 C33 . . '2 655' 127.42(13) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2564 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -29 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .726 _reflns_d_resolution_low 11.258 _diffrn_reflns_av_sigmaI/netI .046 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 130 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .038 _refine_ls_wR_factor_all .034 _refine_ls_goodness_of_fit_all .955 _refine_ls_shift/su_mean .001 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_1623b _database_code_depnum_ccdc_archive 'CCDC 190720' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C75 H57 Er1 N10' _chemical_formula_moiety ? _chemical_formula_weight 1265.61 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 20.209(2) _cell_length_b 13.816(2) _cell_length_c 21.850(2) _cell_angle_alpha 90.00000 _cell_angle_beta 104.179(2) _cell_angle_gamma 90.00000 _cell_volume 5914.8(12) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6653 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 26.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.474 _exptl_crystal_description prism _exptl_crystal_size_max .30 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .12 _exptl_crystal_size_rad ? _exptl_crystal_colour pink _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .854 _exptl_absorpt_correction_T_max .928 _diffrn_reflns_number 34596 _reflns_number_total 7485 _reflns_Friedel_coverage 0 _reflns_number_gt 6653 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.23 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .027 _refine_ls_wR_factor_ref .032 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_number_reflns 6653 _refine_ls_number_parameters 503 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .089 _refine_diff_density_min -.534 _refine_diff_density_max 2.364 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 300 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Er ? 0 4 -.723 4.958 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er .50000 .809344(10) .25000 .01987(7) Uani ? ? 1.00000 ? ? N11 .38194(9) .82440(13) .20513(8) .0231(8) Uani ? ? 1.00000 ? ? N12 .41326(9) .90638(13) .18927(8) .0220(8) Uani ? ? 1.00000 ? ? C13 .36484(11) .96275(16) .15263(9) .0236(9) Uani ? ? 1.00000 ? ? C131 .38088(11) 1.05671(16) .12828(10) .0253(10) Uani ? ? 1.00000 ? ? C132 .44792(12) 1.08303(18) .12947(11) .0296(11) Uani ? ? 1.00000 ? ? C133 .46176(14) 1.17270(18) .10700(12) .0344(12) Uani ? ? 1.00000 ? ? C134 .40956(14) 1.2367(2) .08264(12) .0365(12) Uani ? ? 1.00000 ? ? C135 .34299(15) 1.2115(2) .08103(13) .0383(13) Uani ? ? 1.00000 ? ? C136 .32900(13) 1.12318(19) .10402(11) .0333(11) Uani ? ? 1.00000 ? ? C14 .30129(11) .91855(18) .14527(10) .0271(10) Uani ? ? 1.00000 ? ? C15 .31396(11) .83171(17) .17908(10) .0248(10) Uani ? ? 1.00000 ? ? C151 .26568(12) .76065(18) .19344(10) .0290(10) Uani ? ? 1.00000 ? ? C152 .28861(15) .6734(2) .22293(13) .0400(14) Uani ? ? 1.00000 ? ? C153 .24307(18) .6115(2) .24163(15) .0512(17) Uani ? ? 1.00000 ? ? C154 .17515(16) .6344(3) .23085(14) .0520(17) Uani ? ? 1.00000 ? ? C155 .15183(15) .7204(3) .20160(13) .0468(15) Uani ? ? 1.00000 ? ? C156 .19657(13) .7834(2) .18259(12) .0363(12) Uani ? ? 1.00000 ? ? N21 .45251(8) .84273(13) .34501(8) .0207(8) Uani ? ? 1.00000 ? ? N22 .38468(9) .86559(14) .33337(8) .0236(8) Uani ? ? 1.00000 ? ? C23 .36408(10) .88449(16) .38640(10) .0238(9) Uani ? ? 1.00000 ? ? C231 .29343(11) .90984(16) .38650(10) .0253(10) Uani ? ? 1.00000 ? ? C232 .23937(12) .8971(2) .33356(12) .0377(13) Uani ? ? 1.00000 ? ? C233 .17410(13) .9262(2) .33438(14) .0430(14) Uani ? ? 1.00000 ? ? C234 .16168(13) .9663(2) .38851(13) .0371(13) Uani ? ? 1.00000 ? ? C235 .21418(12) .9753(2) .44176(12) .0344(12) Uani ? ? 1.00000 ? ? C236 .27987(12) .94753(17) .44105(11) .0278(10) Uani ? ? 1.00000 ? ? C24 .42130(11) .87444(17) .43548(10) .0249(10) Uani ? ? 1.00000 ? ? C25 .47456(10) .84762(16) .40825(10) .0215(9) Uani ? ? 1.00000 ? ? C251 .54402(10) .82136(15) .44302(10) .0211(9) Uani ? ? 1.00000 ? ? C252 .58086(11) .74816(16) .42260(10) .0239(9) Uani ? ? 1.00000 ? ? C253 .64449(12) .72163(18) .45883(11) .0278(10) Uani ? ? 1.00000 ? ? C254 .67147(12) .7654(2) .51654(11) .0315(11) Uani ? ? 1.00000 ? ? C255 .63560(12) .8384(2) .53752(11) .0308(11) Uani ? ? 1.00000 ? ? C256 .57275(12) .86742(17) .50071(10) .0271(10) Uani ? ? 1.00000 ? ? N32 .48758(9) .64769(13) .27644(8) .0216(8) Uani ? ? 1.00000 ? ? C33 .47960(10) .55506(15) .29269(9) .0203(9) Uani ? ? 1.00000 ? ? C331 .45401(10) .53024(16) .34866(9) .0211(9) Uani ? ? 1.00000 ? ? C332 .41983(12) .59730(18) .37672(11) .0300(11) Uani ? ? 1.00000 ? ? C333 .39808(13) .5735(2) .43035(12) .0349(12) Uani ? ? 1.00000 ? ? C334 .41018(13) .4822(2) .45625(12) .0337(12) Uani ? ? 1.00000 ? ? C335 .44341(13) .4143(2) .42821(12) .0331(12) Uani ? ? 1.00000 ? ? C336 .46520(11) .43754(17) .37494(10) .0273(10) Uani ? ? 1.00000 ? ? C34 .50000 .4941(2) .25000 .0224(13) Uani ? ? 1.00000 ? ? H132 .4819(13) 1.0423(18) .1449(11) .027(6) Uiso ? ? 1.00000 ? ? H133 .5031(17) 1.187(2) .1078(15) .042(8) Uiso ? ? 1.00000 ? ? H134 .4184(14) 1.294(2) .0689(13) .034(7) Uiso ? ? 1.00000 ? ? H135 .3079(16) 1.257(3) .0669(15) .059(9) Uiso ? ? 1.00000 ? ? H136 .2826(13) 1.1113(19) .1056(11) .031(7) Uiso ? ? 1.00000 ? ? H14 .2621(12) .9440(17) .1211(10) .021(6) Uiso ? ? 1.00000 ? ? H152 .3339(13) .6553(19) .2275(12) .028(6) Uiso ? ? 1.00000 ? ? H153 .2591(14) .554(2) .2601(13) .046(9) Uiso ? ? 1.00000 ? ? H154 .1456(15) .598(2) .2435(14) .051(9) Uiso ? ? 1.00000 ? ? H155 .1062(16) .737(2) .1930(13) .047(8) Uiso ? ? 1.00000 ? ? H156 .1836(14) .838(2) .1668(13) .033(8) Uiso ? ? 1.00000 ? ? H22 .3591(12) .8592(18) .2958(12) .027(6) Uiso ? ? 1.00000 ? ? H232 .2467(14) .877(2) .2975(13) .043(8) Uiso ? ? 1.00000 ? ? H233 .1429(17) .924(3) .3003(16) .068(11) Uiso ? ? 1.00000 ? ? H234 .1181(13) .9805(19) .3875(11) .031(7) Uiso ? ? 1.00000 ? ? H235 .2062(13) 1.004(2) .4769(13) .041(8) Uiso ? ? 1.00000 ? ? H236 .3147(11) .9568(16) .4769(10) .019(6) Uiso ? ? 1.00000 ? ? H24 .4257(11) .8830(17) .4780(11) .022(6) Uiso ? ? 1.00000 ? ? H252 .5592(13) .7144(18) .3836(12) .025(6) Uiso ? ? 1.00000 ? ? H253 .6651(14) .6734(18) .4442(13) .031(7) Uiso ? ? 1.00000 ? ? H254 .7137(14) .745(2) .5425(13) .042(7) Uiso ? ? 1.00000 ? ? H255 .6543(13) .869(2) .5793(12) .034(7) Uiso ? ? 1.00000 ? ? H256 .5481(11) .9161(18) .5135(10) .021(6) Uiso ? ? 1.00000 ? ? H34 .50000 .427(3) .25000 .032(9) Uiso ? ? 1.00000 ? ? H332 .4121(14) .652(2) .3587(13) .036(7) Uiso ? ? 1.00000 ? ? H333 .3773(12) .619(2) .4448(11) .029(7) Uiso ? ? 1.00000 ? ? H334 .3969(14) .466(2) .4878(14) .046(8) Uiso ? ? 1.00000 ? ? H335 .4527(13) .360(2) .4426(13) .036(7) Uiso ? ? 1.00000 ? ? H336 .4896(12) .3924(18) .3563(11) .025(6) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Er .02064(7) .02111(7) .01924(7) .00000 .00751(5) .00000 N11 .0244(9) .0277(10) .0180(8) -.0024(7) .0065(7) -.0007(7) N12 .0238(9) .0243(9) .0197(8) -.0006(7) .0088(7) -.0003(7) C13 .0246(10) .0271(11) .0194(9) .0018(9) .0062(8) -.0024(8) C131 .0302(11) .0254(11) .0204(9) .0008(9) .0063(8) -.0013(8) C132 .0307(12) .0292(12) .0290(11) .0024(10) .0075(9) -.0004(9) C133 .0369(14) .0357(15) .0322(12) -.0064(11) .0116(11) -.0015(10) C134 .0485(16) .0256(13) .0337(13) -.0038(12) .0070(11) .0017(10) C135 .0442(15) .0302(14) .0369(13) .0054(11) .0030(12) .0041(10) C136 .0312(13) .0330(13) .0342(12) .0040(10) .0051(10) .0018(10) C14 .0224(11) .0336(13) .0236(10) .0018(9) .0027(9) -.0014(9) C15 .0237(10) .0324(12) .0189(9) -.0013(9) .0061(8) -.0042(8) C151 .0297(12) .0372(13) .0204(10) -.0088(10) .0069(9) -.0056(9) C152 .0402(15) .0417(16) .0406(14) -.0057(12) .0147(12) .0019(11) C153 .060(2) .0466(19) .0497(17) -.0122(15) .0197(15) .0090(14) C154 .0528(18) .070(2) .0352(14) -.0327(17) .0150(13) -.0022(14) C155 .0327(14) .075(2) .0324(13) -.0202(14) .0081(11) -.0075(14) C156 .0305(13) .0493(17) .0276(11) -.0091(12) .0042(10) -.0026(11) N21 .0187(8) .0234(9) .0209(8) .0016(7) .0063(7) -.0001(7) N22 .0193(9) .0322(11) .0192(8) .0031(7) .0045(7) -.0021(7) C23 .0235(10) .0263(11) .0234(10) .0024(9) .0090(8) -.0021(8) C231 .0208(10) .0288(12) .0277(10) .0032(9) .0082(8) -.0010(9) C232 .0254(12) .0564(17) .0316(12) .0057(11) .0077(10) -.0103(12) C233 .0230(12) .0607(19) .0425(14) .0068(12) .0028(11) -.0041(14) C234 .0243(12) .0404(15) .0511(15) .0056(11) .0178(11) .0004(12) C235 .0335(13) .0350(13) .0410(14) .0035(10) .0213(11) -.0045(11) C236 .0270(11) .0306(12) .0283(11) .0012(9) .0114(9) -.0020(9) C24 .0254(11) .0302(12) .0201(10) .0014(9) .0077(8) -.0025(9) C25 .0228(10) .0215(10) .0208(9) .0001(8) .0066(8) -.0003(8) C251 .0204(10) .0233(11) .0205(9) -.0001(8) .0069(8) .0030(8) C252 .0243(10) .0270(11) .0220(10) .0000(9) .0088(8) .0018(9) C253 .0243(11) .0299(12) .0318(11) .0049(9) .0119(9) .0060(10) C254 .0206(11) .0432(14) .0296(11) .0004(10) .0041(9) .0107(11) C255 .0280(12) .0392(13) .0245(11) -.0074(10) .0054(9) -.0000(10) C256 .0276(11) .0287(12) .0254(11) .0001(9) .0071(9) -.0022(9) N32 .0240(9) .0238(9) .0190(8) .0007(7) .0093(7) -.0009(7) C33 .0189(9) .0241(11) .0195(9) -.0017(8) .0077(8) .0019(8) C331 .0180(9) .0254(11) .0206(9) -.0035(8) .0062(8) .0009(8) C332 .0349(13) .0259(12) .0327(12) .0004(10) .0151(10) .0033(10) C333 .0386(13) .0362(14) .0366(13) .0020(11) .0222(11) -.0027(11) C334 .0358(13) .0405(14) .0296(12) -.0035(11) .0170(11) .0045(11) C335 .0344(13) .0312(13) .0369(13) .0002(11) .0149(10) .0114(11) C336 .0278(11) .0262(11) .0307(11) .0017(9) .0125(9) .0025(9) C34 .0217(14) .0193(15) .0256(14) .00000 .0050(11) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Er N11 . . 2.3560(18) ? Er N12 . . 2.3433(16) ? Er N21 . . 2.5338(19) ? Er N32 . . 2.3358(19) ? Er N11 . '2 655' 2.3560(18) ? Er N12 . '2 655' 2.3433(16) ? Er N21 . '2 655' 2.5338(19) ? Er N32 . '2 655' 2.3358(19) ? N11 N12 . . 1.382(3) ? N11 C15 . . 1.356(3) ? N12 C13 . . 1.350(3) ? C13 C131 . . 1.469(3) ? C13 C14 . . 1.395(3) ? C131 C132 . . 1.397(3) ? C131 C136 . . 1.397(3) ? C132 C133 . . 1.386(4) ? C132 H132 . . .89(2) ? C133 C134 . . 1.380(4) ? C133 H133 . . .86(3) ? C134 C135 . . 1.382(4) ? C134 H134 . . .88(3) ? C135 C136 . . 1.376(4) ? C135 H135 . . .94(3) ? C136 H136 . . .96(3) ? C14 C15 . . 1.399(3) ? C14 H14 . . .91(2) ? C15 C151 . . 1.471(3) ? C151 C152 . . 1.392(4) ? C151 C156 . . 1.394(4) ? C152 C153 . . 1.390(5) ? C152 H152 . . .93(3) ? C153 C154 . . 1.372(5) ? C153 H153 . . .91(3) ? C154 C155 . . 1.377(5) ? C154 H154 . . .88(3) ? C155 C156 . . 1.390(5) ? C155 H155 . . .92(3) ? C156 H156 . . .84(3) ? N21 N22 . . 1.368(2) ? N21 C25 . . 1.346(3) ? N22 C23 . . 1.349(3) ? N22 H22 . . .86(2) ? C23 C231 . . 1.471(3) ? C23 C24 . . 1.378(3) ? C231 C232 . . 1.394(3) ? C231 C236 . . 1.388(3) ? C232 C233 . . 1.383(4) ? C232 H232 . . .88(3) ? C233 C234 . . 1.383(4) ? C233 H233 . . .85(3) ? C234 C235 . . 1.375(3) ? C234 H234 . . .90(3) ? C235 C236 . . 1.386(4) ? C235 H235 . . .91(3) ? C236 H236 . . .92(2) ? C24 C25 . . 1.401(3) ? C24 H24 . . .92(2) ? C25 C251 . . 1.469(3) ? C251 C252 . . 1.392(3) ? C251 C256 . . 1.404(3) ? C252 C253 . . 1.384(3) ? C252 H252 . . .98(2) ? C253 C254 . . 1.385(3) ? C253 H253 . . .89(3) ? C254 C255 . . 1.383(4) ? C254 H254 . . .94(3) ? C255 C256 . . 1.386(3) ? C255 H255 . . 1.00(3) ? C256 H256 . . .92(2) ? N32 C33 . . 1.348(3) ? N32 N32 . '2 655' 1.368(3) ? C33 C331 . . 1.480(3) ? C33 C34 . . 1.392(3) ? C331 C332 . . 1.385(3) ? C331 C336 . . 1.399(3) ? C332 C333 . . 1.388(4) ? C332 H332 . . .84(3) ? C333 C334 . . 1.380(4) ? C333 H333 . . .86(3) ? C334 C335 . . 1.381(4) ? C334 H334 . . .83(3) ? C335 C336 . . 1.379(4) ? C335 H335 . . .82(3) ? C336 H336 . . .95(3) ? C34 H34 . . .93(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Er N12 . . . 34.21(6) ? N11 Er N21 . . . 77.09(6) ? N11 Er N32 . . . 91.61(6) ? N11 Er N11 . . '2 655' 169.87(6) ? N11 Er N12 . . '2 655' 136.54(6) ? N11 Er N21 . . '2 655' 101.02(6) ? N11 Er N32 . . '2 655' 98.09(6) ? N12 Er N21 . . . 88.79(6) ? N12 Er N32 . . . 125.19(6) ? N12 Er N11 . . '2 655' 136.54(6) ? N12 Er N12 . . '2 655' 110.20(6) ? N12 Er N21 . . '2 655' 79.21(6) ? N12 Er N32 . . '2 655' 121.18(6) ? N21 Er N32 . . . 83.47(6) ? N21 Er N11 . . '2 655' 101.02(6) ? N21 Er N12 . . '2 655' 79.21(6) ? N21 Er N21 . . '2 655' 159.02(6) ? N21 Er N32 . . '2 655' 117.51(6) ? N32 Er N11 . . '2 655' 98.09(6) ? N32 Er N12 . . '2 655' 121.18(6) ? N32 Er N21 . . '2 655' 117.51(6) ? N32 Er N32 . . '2 655' 34.05(7) ? N11 Er N12 '2 655' . '2 655' 34.21(6) ? N11 Er N21 '2 655' . '2 655' 77.09(6) ? N11 Er N32 '2 655' . '2 655' 91.61(6) ? N12 Er N21 '2 655' . '2 655' 88.79(6) ? N12 Er N32 '2 655' . '2 655' 125.19(6) ? N21 Er N32 '2 655' . '2 655' 83.47(6) ? Er N11 N12 . . . 72.39(10) ? Er N11 C15 . . . 179.18(16) ? N12 N11 C15 . . . 108.23(16) ? Er N12 N11 . . . 73.39(10) ? Er N12 C13 . . . 177.72(16) ? N11 N12 C13 . . . 108.15(17) ? N12 C13 C131 . . . 122.18(19) ? N12 C13 C14 . . . 109.2(2) ? C131 C13 C14 . . . 128.6(2) ? C13 C131 C132 . . . 121.5(2) ? C13 C131 C136 . . . 120.4(2) ? C132 C131 C136 . . . 118.1(2) ? C131 C132 C133 . . . 120.3(2) ? C131 C132 H132 . . . 119.9(17) ? C133 C132 H132 . . . 119.8(17) ? C132 C133 C134 . . . 120.5(3) ? C132 C133 H133 . . . 118.8(18) ? C134 C133 H133 . . . 120.7(18) ? C133 C134 C135 . . . 119.7(3) ? C133 C134 H134 . . . 120.5(19) ? C135 C134 H134 . . . 119.8(19) ? C134 C135 C136 . . . 120.0(2) ? C134 C135 H135 . . . 120(2) ? C136 C135 H135 . . . 120(2) ? C131 C136 C135 . . . 121.3(2) ? C131 C136 H136 . . . 121.5(15) ? C135 C136 H136 . . . 117.0(15) ? C13 C14 C15 . . . 105.68(18) ? C13 C14 H14 . . . 123.0(15) ? C15 C14 H14 . . . 131.3(15) ? N11 C15 C14 . . . 108.7(2) ? N11 C15 C151 . . . 121.2(2) ? C14 C15 C151 . . . 129.8(2) ? C15 C151 C152 . . . 120.9(2) ? C15 C151 C156 . . . 120.2(2) ? C152 C151 C156 . . . 118.7(3) ? C151 C152 C153 . . . 120.0(3) ? C151 C152 H152 . . . 119.4(17) ? C153 C152 H152 . . . 120.5(17) ? C152 C153 C154 . . . 121.0(3) ? C152 C153 H153 . . . 118(2) ? C154 C153 H153 . . . 121(2) ? C153 C154 C155 . . . 119.6(3) ? C153 C154 H154 . . . 123(2) ? C155 C154 H154 . . . 117(2) ? C154 C155 C156 . . . 120.4(3) ? C154 C155 H155 . . . 121(2) ? C156 C155 H155 . . . 118(2) ? C151 C156 C155 . . . 120.4(3) ? C151 C156 H156 . . . 118(2) ? C155 C156 H156 . . . 122(2) ? Er N21 N22 . . . 116.93(12) ? Er N21 C25 . . . 138.92(14) ? N22 N21 C25 . . . 104.13(18) ? N21 N22 C23 . . . 113.00(16) ? N21 N22 H22 . . . 119.6(18) ? C23 N22 H22 . . . 126.8(18) ? N22 C23 C231 . . . 123.46(17) ? N22 C23 C24 . . . 105.8(2) ? C231 C23 C24 . . . 130.8(2) ? C23 C231 C232 . . . 122.2(2) ? C23 C231 C236 . . . 119.11(17) ? C232 C231 C236 . . . 118.7(2) ? C231 C232 C233 . . . 120.6(3) ? C231 C232 H232 . . . 120.9(17) ? C233 C232 H232 . . . 118.2(17) ? C232 C233 C234 . . . 120.0(2) ? C232 C233 H233 . . . 119(3) ? C234 C233 H233 . . . 121(3) ? C233 C234 C235 . . . 119.7(2) ? C233 C234 H234 . . . 116.8(15) ? C235 C234 H234 . . . 123.3(15) ? C234 C235 C236 . . . 120.5(3) ? C234 C235 H235 . . . 119.6(16) ? C236 C235 H235 . . . 119.7(16) ? C231 C236 C235 . . . 120.3(2) ? C231 C236 H236 . . . 120.6(16) ? C235 C236 H236 . . . 119.1(16) ? C23 C24 C25 . . . 106.4(2) ? C23 C24 H24 . . . 129.0(14) ? C25 C24 H24 . . . 124.6(14) ? N21 C25 C24 . . . 110.71(17) ? N21 C25 C251 . . . 123.6(2) ? C24 C25 C251 . . . 125.59(19) ? C25 C251 C252 . . . 122.14(18) ? C25 C251 C256 . . . 119.0(2) ? C252 C251 C256 . . . 118.73(18) ? C251 C252 C253 . . . 120.3(2) ? C251 C252 H252 . . . 117.8(15) ? C253 C252 H252 . . . 121.9(15) ? C252 C253 C254 . . . 120.6(2) ? C252 C253 H253 . . . 116.4(16) ? C254 C253 H253 . . . 122.9(16) ? C253 C254 C255 . . . 119.9(2) ? C253 C254 H254 . . . 121.0(18) ? C255 C254 H254 . . . 119.0(18) ? C254 C255 C256 . . . 119.9(2) ? C254 C255 H255 . . . 120.3(15) ? C256 C255 H255 . . . 119.8(15) ? C251 C256 C255 . . . 120.6(2) ? C251 C256 H256 . . . 117.9(13) ? C255 C256 H256 . . . 121.6(13) ? Er N32 C33 . . . 178.65(16) ? Er N32 N32 . . '2 655' 72.98(11) ? C33 N32 N32 . . '2 655' 108.35(18) ? N32 C33 C331 . . . 121.74(19) ? N32 C33 C34 . . . 108.9(2) ? C331 C33 C34 . . . 129.4(2) ? C33 C331 C332 . . . 121.6(2) ? C33 C331 C336 . . . 119.8(2) ? C332 C331 C336 . . . 118.6(2) ? C331 C332 C333 . . . 120.7(2) ? C331 C332 H332 . . . 116(2) ? C333 C332 H332 . . . 123(2) ? C332 C333 C334 . . . 120.1(3) ? C332 C333 H333 . . . 115.1(18) ? C334 C333 H333 . . . 124.8(18) ? C333 C334 C335 . . . 119.7(3) ? C333 C334 H334 . . . 122(2) ? C335 C334 H334 . . . 119(2) ? C334 C335 C336 . . . 120.4(2) ? C334 C335 H335 . . . 123(2) ? C336 C335 H335 . . . 117(2) ? C331 C336 C335 . . . 120.4(2) ? C331 C336 H336 . . . 118.3(15) ? C335 C336 H336 . . . 121.2(15) ? C33 C34 H34 . . . 127.22(13) ? C33 C34 C33 . . '2 655' 105.6(2) ? H34 C34 C33 . . '2 655' 127.22(13) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2580 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min -29 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .728 _reflns_d_resolution_low 11.266 _diffrn_reflns_av_sigmaI/netI .036 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .033 _refine_ls_wR_factor_all .033 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END data_8999b1 _database_code_depnum_ccdc_archive 'CCDC 190721' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C75 H57 N10 Yb1' _chemical_formula_moiety ? _chemical_formula_weight 1271.39 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 20.274(2) _cell_length_b 14.0780(10) _cell_length_c 21.947(2) _cell_angle_alpha 90.00000 _cell_angle_beta 103.668(2) _cell_angle_gamma 90.00000 _cell_volume 6086.7(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6073 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 22.4 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 1.59 _exptl_crystal_description rod _exptl_crystal_size_max .54 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .10 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .56 _exptl_absorpt_correction_T_max .83 _diffrn_reflns_number 33415 _reflns_number_total 7737 _reflns_Friedel_coverage ? _reflns_number_gt 6518 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 29.13 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .030 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .027 _refine_ls_wR_factor_ref .0298 _refine_ls_goodness_of_fit_ref .99 _refine_ls_number_reflns 6518 _refine_ls_number_parameters 503 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .092 _refine_diff_density_min -.78 _refine_diff_density_max .79 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF' _computing_structure_solution xtal _computing_structure_refinement xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 300 .002014 .002014 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 228 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 40 .004028 .002991 'Int Tables Vol IV Tables 2.2B and 2.3.1' Yb ? 0 4 -.883972 5.548 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Yb .50000 .806140(10) .25000 .04323(7) Uani ? ? 1.00000 ? ? N11 .38391(10) .82189(15) .20615(9) .0546(10) Uani ? ? 1.00000 ? ? N12 .41614(9) .90379(14) .19181(8) .0521(10) Uani ? ? 1.00000 ? ? C13 .36823(12) .95971(18) .15640(10) .0532(12) Uani ? ? 1.00000 ? ? C131 .38481(13) 1.05202(18) .13312(11) .0558(12) Uani ? ? 1.00000 ? ? C132 .45120(15) 1.0789(2) .13495(14) .0703(16) Uani ? ? 1.00000 ? ? C133 .4648(2) 1.1670(3) .11197(17) .085(2) Uani ? ? 1.00000 ? ? C134 .4134(2) 1.2285(3) .08765(17) .088(2) Uani ? ? 1.00000 ? ? C135 .3484(3) 1.2034(3) .08489(19) .093(2) Uani ? ? 1.00000 ? ? C136 .33371(18) 1.1162(2) .10757(15) .0776(18) Uani ? ? 1.00000 ? ? C14 .30490(13) .9163(2) .14859(11) .0600(13) Uani ? ? 1.00000 ? ? C15 .31708(12) .83048(19) .18085(11) .0547(12) Uani ? ? 1.00000 ? ? C151 .26825(14) .7603(2) .19365(11) .0621(14) Uani ? ? 1.00000 ? ? C152 .2893(2) .6745(3) .22091(19) .090(2) Uani ? ? 1.00000 ? ? C153 .2426(3) .6128(4) .2377(2) .117(3) Uani ? ? 1.00000 ? ? C154 .1767(3) .6364(5) .2279(2) .120(3) Uani ? ? 1.00000 ? ? C155 .1547(2) .7208(5) .2006(2) .110(3) Uani ? ? 1.00000 ? ? C156 .20013(17) .7834(3) .18289(15) .083(2) Uani ? ? 1.00000 ? ? N21 .45304(9) .84012(14) .34469(8) .0461(9) Uani ? ? 1.00000 ? ? N22 .38622(10) .86290(15) .33380(9) .0505(10) Uani ? ? 1.00000 ? ? C23 .36542(11) .88268(17) .38639(10) .0504(11) Uani ? ? 1.00000 ? ? C231 .29521(11) .90773(18) .38663(11) .0557(12) Uani ? ? 1.00000 ? ? C232 .24213(15) .8948(3) .33495(16) .087(2) Uani ? ? 1.00000 ? ? C233 .17696(16) .9233(3) .3364(2) .099(2) Uani ? ? 1.00000 ? ? C234 .16449(17) .9628(3) .38901(19) .087(2) Uani ? ? 1.00000 ? ? C235 .21571(17) .9717(3) .44068(18) .083(2) Uani ? ? 1.00000 ? ? C236 .28100(14) .9454(2) .43984(14) .0675(16) Uani ? ? 1.00000 ? ? C24 .42217(12) .87283(19) .43443(11) .0539(12) Uani ? ? 1.00000 ? ? C25 .47517(11) .84566(17) .40755(10) .0469(10) Uani ? ? 1.00000 ? ? C251 .54396(11) .81992(15) .44184(10) .0475(11) Uani ? ? 1.00000 ? ? C252 .58028(12) .74745(18) .42244(11) .0530(12) Uani ? ? 1.00000 ? ? C253 .64319(14) .7214(2) .45840(13) .0636(14) Uani ? ? 1.00000 ? ? C254 .66975(14) .7654(3) .51469(14) .0719(16) Uani ? ? 1.00000 ? ? C255 .63467(15) .8378(3) .53466(13) .0705(16) Uani ? ? 1.00000 ? ? C256 .57243(14) .8659(2) .49828(12) .0615(14) Uani ? ? 1.00000 ? ? N32 .48724(10) .64906(14) .27645(8) .0506(10) Uani ? ? 1.00000 ? ? C33 .47944(10) .55815(16) .29243(10) .0461(10) Uani ? ? 1.00000 ? ? C331 .45382(11) .53279(17) .34800(10) .0491(11) Uani ? ? 1.00000 ? ? C332 .42008(15) .5985(2) .37647(13) .0677(15) Uani ? ? 1.00000 ? ? C333 .39727(18) .5741(3) .42936(15) .083(2) Uani ? ? 1.00000 ? ? C334 .40815(17) .4843(3) .45376(15) .0802(19) Uani ? ? 1.00000 ? ? C335 .44090(17) .4187(3) .42570(16) .0779(18) Uani ? ? 1.00000 ? ? C336 .46355(14) .4427(2) .37329(13) .0644(15) Uani ? ? 1.00000 ? ? C34 .50000 .4990(3) .25000 .0503(16) Uani ? ? 1.00000 ? ? H132 .4884(15) 1.038(2) .1532(14) .086(10) Uiso ? ? 1.00000 ? ? H133 .508(2) 1.184(3) .114(2) .112(14) Uiso ? ? 1.00000 ? ? H134 .4246(18) 1.289(2) .0731(17) .094(11) Uiso ? ? 1.00000 ? ? H135 .313(2) 1.246(3) .0694(18) .119(13) Uiso ? ? 1.00000 ? ? H136 .2890(17) 1.099(2) .1068(15) .088(10) Uiso ? ? 1.00000 ? ? H14 .2586(14) .942(2) .1214(12) .073(8) Uiso ? ? 1.00000 ? ? H152 .3346(17) .656(2) .2247(14) .081(10) Uiso ? ? 1.00000 ? ? H153 .263(2) .560(3) .2579(17) .107(14) Uiso ? ? 1.00000 ? ? H154 .148(2) .596(3) .240(2) .136(15) Uiso ? ? 1.00000 ? ? H155 .110(2) .737(3) .1925(17) .111(13) Uiso ? ? 1.00000 ? ? H156 .1854(19) .842(3) .1698(17) .099(13) Uiso ? ? 1.00000 ? ? H22 .3649(12) .8618(17) .2983(11) .047(7) Uiso ? ? 1.00000 ? ? H232 .2481(16) .870(2) .2992(15) .086(10) Uiso ? ? 1.00000 ? ? H233 .146(2) .924(3) .3010(18) .129(15) Uiso ? ? 1.00000 ? ? H234 .1206(17) .974(2) .3910(14) .088(9) Uiso ? ? 1.00000 ? ? H235 .2099(17) 1.000(2) .4767(16) .102(11) Uiso ? ? 1.00000 ? ? H236 .3152(13) .955(2) .4760(12) .068(8) Uiso ? ? 1.00000 ? ? H24 .4254(12) .8818(18) .4745(12) .056(7) Uiso ? ? 1.00000 ? ? H252 .5598(14) .7154(18) .3851(13) .059(7) Uiso ? ? 1.00000 ? ? H253 .6648(15) .6723(19) .4443(13) .064(8) Uiso ? ? 1.00000 ? ? H254 .7115(15) .746(2) .5396(13) .072(8) Uiso ? ? 1.00000 ? ? H255 .6521(15) .868(2) .5725(14) .082(9) Uiso ? ? 1.00000 ? ? H256 .5484(12) .9169(19) .5116(11) .058(7) Uiso ? ? 1.00000 ? ? H332 .4118(13) .657(2) .3570(12) .062(7) Uiso ? ? 1.00000 ? ? H333 .3772(14) .620(2) .4442(13) .073(9) Uiso ? ? 1.00000 ? ? H334 .3932(15) .465(2) .4868(14) .084(9) Uiso ? ? 1.00000 ? ? H335 .4499(19) .366(3) .4425(17) .111(13) Uiso ? ? 1.00000 ? ? H336 .4833(15) .401(2) .3565(13) .073(9) Uiso ? ? 1.00000 ? ? H34 .50000 .428(3) .25000 .062(10) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Yb .04326(8) .04701(8) .04301(7) .00000 .01739(5) .00000 N11 .0539(11) .0688(14) .0438(9) -.0048(9) .0168(8) -.0004(9) N12 .0546(11) .0592(12) .0466(9) -.0002(9) .0203(8) -.0004(9) C13 .0544(13) .0582(14) .0485(12) .0062(11) .0154(10) -.0033(10) C131 .0612(14) .0560(14) .0509(12) .0029(11) .0146(11) -.0018(11) C132 .0677(17) .0672(17) .0766(17) -.0017(15) .0180(14) .0026(15) C133 .090(3) .079(2) .087(2) -.024(2) .026(2) -.0053(17) C134 .116(3) .0614(18) .083(2) -.010(2) .016(2) .0076(17) C135 .107(3) .066(2) .097(3) .013(2) .006(2) .0112(18) C136 .071(2) .072(2) .085(2) .0047(16) .0104(16) .0066(16) C14 .0537(14) .0697(17) .0555(13) .0014(12) .0109(11) -.0032(12) C15 .0517(13) .0697(16) .0440(11) -.0059(11) .0140(10) -.0081(10) C151 .0634(16) .0767(18) .0469(12) -.0180(14) .0144(11) -.0085(12) C152 .089(3) .088(3) .098(2) -.019(2) .032(2) .0056(19) C153 .137(4) .107(3) .111(3) -.037(3) .041(3) .018(3) C154 .116(4) .166(5) .083(2) -.078(4) .031(2) -.003(3) C155 .072(2) .182(5) .078(2) -.051(3) .0187(19) -.016(3) C156 .0624(18) .116(3) .0679(18) -.0250(19) .0099(14) -.0073(19) N21 .0414(9) .0534(10) .0463(9) .0054(8) .0161(8) -.0014(8) N22 .0430(10) .0670(13) .0425(10) .0074(9) .0120(8) -.0028(9) C23 .0479(12) .0576(14) .0495(11) .0052(10) .0189(10) -.0057(10) C231 .0477(12) .0635(15) .0599(13) .0066(11) .0207(10) -.0044(12) C232 .0542(16) .133(3) .0744(19) .0130(17) .0165(14) -.025(2) C233 .0486(16) .142(4) .102(3) .013(2) .0088(17) -.016(3) C234 .0533(17) .093(2) .123(3) .0120(16) .040(2) -.008(2) C235 .071(2) .092(2) .100(2) .0103(16) .0468(19) -.0162(19) C236 .0571(15) .083(2) .0683(16) .0089(14) .0273(13) -.0109(14) C24 .0520(13) .0675(16) .0449(12) .0063(11) .0171(10) -.0065(11) C25 .0470(12) .0496(12) .0460(11) .0029(10) .0150(9) -.0008(10) C251 .0458(11) .0529(13) .0458(11) .0019(9) .0149(9) .0036(9) C252 .0509(13) .0582(15) .0520(13) .0048(11) .0165(10) .0052(11) C253 .0526(14) .0735(18) .0683(16) .0137(13) .0213(13) .0152(14) C254 .0458(14) .101(2) .0673(17) .0016(15) .0092(13) .0229(16) C255 .0594(17) .094(2) .0546(15) -.0123(15) .0059(13) .0004(14) C256 .0605(15) .0669(17) .0562(14) .0011(13) .0124(12) -.0043(12) N32 .0570(11) .0528(11) .0488(10) .0007(9) .0256(9) -.0014(8) C33 .0423(11) .0519(13) .0476(11) -.0032(9) .0175(9) .0015(9) C331 .0464(12) .0537(13) .0504(11) -.0053(10) .0177(9) .0021(10) C332 .0825(19) .0605(17) .0722(16) -.0024(14) .0421(14) .0035(14) C333 .101(2) .081(2) .087(2) -.0007(19) .0605(19) -.0065(18) C334 .091(2) .090(2) .0739(18) -.0088(18) .0470(17) .0139(17) C335 .086(2) .074(2) .085(2) .0029(17) .0421(16) .0259(17) C336 .0686(17) .0610(16) .0714(16) .0030(13) .0321(14) .0103(13) C34 .0464(17) .052(2) .0540(17) .00000 .0158(14) .00000 # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Yb N11 . . 2.333(2) ? Yb N12 . . 2.3206(17) ? Yb N21 . . 2.528(2) ? Yb N32 . . 2.316(2) ? Yb N11 . '2 655' 2.333(2) ? Yb N12 . '2 655' 2.3206(17) ? Yb N21 . '2 655' 2.528(2) ? Yb N32 . '2 655' 2.316(2) ? N11 N12 . . 1.397(3) ? N11 C15 . . 1.343(3) ? N12 C13 . . 1.346(3) ? C13 C131 . . 1.464(4) ? C13 C14 . . 1.395(4) ? C131 C132 . . 1.389(4) ? C131 C136 . . 1.389(4) ? C132 C133 . . 1.391(5) ? C132 H132 . . .96(3) ? C133 C134 . . 1.363(6) ? C133 H133 . . .91(5) ? C134 C135 . . 1.351(7) ? C134 H134 . . .96(4) ? C135 C136 . . 1.383(5) ? C135 H135 . . .94(4) ? C136 H136 . . .93(3) ? C14 C15 . . 1.393(4) ? C14 H14 . . 1.05(3) ? C15 C151 . . 1.472(4) ? C151 C152 . . 1.371(5) ? C151 C156 . . 1.384(4) ? C152 C153 . . 1.398(7) ? C152 H152 . . .94(3) ? C153 C154 . . 1.345(8) ? C153 H153 . . .92(4) ? C154 C155 . . 1.358(9) ? C154 H154 . . .89(5) ? C155 C156 . . 1.394(7) ? C155 H155 . . .92(4) ? C156 H156 . . .91(4) ? N21 N22 . . 1.357(3) ? N21 C25 . . 1.348(3) ? N22 C23 . . 1.348(3) ? N22 H22 . . .80(2) ? C23 C231 . . 1.468(3) ? C23 C24 . . 1.372(3) ? C231 C232 . . 1.379(4) ? C231 C236 . . 1.374(4) ? C232 C233 . . 1.388(5) ? C232 H232 . . .90(3) ? C233 C234 . . 1.359(6) ? C233 H233 . . .88(4) ? C234 C235 . . 1.350(5) ? C234 H234 . . .91(3) ? C235 C236 . . 1.379(5) ? C235 H235 . . .91(4) ? C236 H236 . . .93(2) ? C24 C25 . . 1.396(4) ? C24 H24 . . .88(3) ? C25 C251 . . 1.465(3) ? C251 C252 . . 1.383(3) ? C251 C256 . . 1.396(3) ? C252 C253 . . 1.381(3) ? C252 H252 . . .94(3) ? C253 C254 . . 1.373(4) ? C253 H253 . . .91(3) ? C254 C255 . . 1.373(5) ? C254 H254 . . .93(3) ? C255 C256 . . 1.382(4) ? C255 H255 . . .93(3) ? C256 H256 . . .95(3) ? N32 C33 . . 1.346(3) ? N32 N32 . '2 655' 1.378(3) ? C33 C331 . . 1.478(3) ? C33 C34 . . 1.385(3) ? C331 C332 . . 1.385(4) ? C331 C336 . . 1.380(4) ? C332 C333 . . 1.391(5) ? C332 H332 . . .93(3) ? C333 C334 . . 1.369(5) ? C333 H333 . . .87(3) ? C334 C335 . . 1.366(5) ? C334 H334 . . .89(3) ? C335 C336 . . 1.377(5) ? C335 H335 . . .83(4) ? C336 H336 . . .84(3) ? C34 H34 . . 1.00(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published N11 Yb N12 . . . 34.94(7) ? N11 Yb N21 . . . 77.40(6) ? N11 Yb N32 . . . 91.87(7) ? N11 Yb N11 . . '2 655' 169.09(7) ? N11 Yb N12 . . '2 655' 135.00(7) ? N11 Yb N21 . . '2 655' 100.49(6) ? N11 Yb N32 . . '2 655' 98.56(7) ? N12 Yb N21 . . . 88.34(6) ? N12 Yb N32 . . . 126.36(6) ? N12 Yb N11 . . '2 655' 135.00(7) ? N12 Yb N12 . . '2 655' 107.35(6) ? N12 Yb N21 . . '2 655' 78.74(6) ? N12 Yb N32 . . '2 655' 122.57(6) ? N21 Yb N32 . . . 83.60(7) ? N21 Yb N11 . . '2 655' 100.49(6) ? N21 Yb N12 . . '2 655' 78.74(6) ? N21 Yb N21 . . '2 655' 158.18(6) ? N21 Yb N32 . . '2 655' 118.22(7) ? N32 Yb N11 . . '2 655' 98.56(7) ? N32 Yb N12 . . '2 655' 122.57(6) ? N32 Yb N21 . . '2 655' 118.22(7) ? N32 Yb N32 . . '2 655' 34.62(7) ? N11 Yb N12 '2 655' . '2 655' 34.94(7) ? N11 Yb N21 '2 655' . '2 655' 77.40(6) ? N11 Yb N32 '2 655' . '2 655' 91.87(7) ? N12 Yb N21 '2 655' . '2 655' 88.34(6) ? N12 Yb N32 '2 655' . '2 655' 126.36(7) ? N21 Yb N32 '2 655' . '2 655' 83.60(7) ? Yb N11 N12 . . . 72.03(11) ? Yb N11 C15 . . . 179.7(2) ? N12 N11 C15 . . . 108.20(19) ? Yb N12 N11 . . . 73.02(11) ? Yb N12 C13 . . . 178.14(16) ? N11 N12 C13 . . . 107.50(18) ? N12 C13 C131 . . . 121.8(2) ? N12 C13 C14 . . . 109.4(2) ? C131 C13 C14 . . . 128.8(2) ? C13 C131 C132 . . . 122.1(2) ? C13 C131 C136 . . . 120.5(3) ? C132 C131 C136 . . . 117.4(3) ? C131 C132 C133 . . . 120.4(3) ? C131 C132 H132 . . . 120(2) ? C133 C132 H132 . . . 119(2) ? C132 C133 C134 . . . 120.6(4) ? C132 C133 H133 . . . 119(2) ? C134 C133 H133 . . . 120(2) ? C133 C134 C135 . . . 119.9(4) ? C133 C134 H134 . . . 118(2) ? C135 C134 H134 . . . 122(2) ? C134 C135 C136 . . . 120.5(4) ? C134 C135 H135 . . . 121(3) ? C136 C135 H135 . . . 119(3) ? C131 C136 C135 . . . 121.2(3) ? C131 C136 H136 . . . 118(2) ? C135 C136 H136 . . . 121(2) ? C13 C14 C15 . . . 105.7(2) ? C13 C14 H14 . . . 126.5(16) ? C15 C14 H14 . . . 127.8(16) ? N11 C15 C14 . . . 109.2(2) ? N11 C15 C151 . . . 121.3(2) ? C14 C15 C151 . . . 129.3(2) ? C15 C151 C152 . . . 121.4(3) ? C15 C151 C156 . . . 119.9(3) ? C152 C151 C156 . . . 118.5(3) ? C151 C152 C153 . . . 120.1(4) ? C151 C152 H152 . . . 119(2) ? C153 C152 H152 . . . 121(2) ? C152 C153 C154 . . . 121.0(5) ? C152 C153 H153 . . . 112(3) ? C154 C153 H153 . . . 127(3) ? C153 C154 C155 . . . 119.7(5) ? C153 C154 H154 . . . 119(3) ? C155 C154 H154 . . . 122(3) ? C154 C155 C156 . . . 120.5(4) ? C154 C155 H155 . . . 121(3) ? C156 C155 H155 . . . 119(3) ? C151 C156 C155 . . . 120.2(4) ? C151 C156 H156 . . . 121(2) ? C155 C156 H156 . . . 119(3) ? Yb N21 N22 . . . 117.01(12) ? Yb N21 C25 . . . 138.87(15) ? N22 N21 C25 . . . 104.09(19) ? N21 N22 C23 . . . 113.53(17) ? N21 N22 H22 . . . 117.2(19) ? C23 N22 H22 . . . 129(2) ? N22 C23 C231 . . . 123.54(18) ? N22 C23 C24 . . . 105.2(2) ? C231 C23 C24 . . . 131.3(2) ? C23 C231 C232 . . . 122.3(3) ? C23 C231 C236 . . . 119.6(2) ? C232 C231 C236 . . . 118.1(3) ? C231 C232 C233 . . . 120.3(3) ? C231 C232 H232 . . . 122(2) ? C233 C232 H232 . . . 117(2) ? C232 C233 C234 . . . 120.4(3) ? C232 C233 H233 . . . 119(3) ? C234 C233 H233 . . . 120(3) ? C233 C234 C235 . . . 119.4(3) ? C233 C234 H234 . . . 119.4(18) ? C235 C234 H234 . . . 120.4(19) ? C234 C235 C236 . . . 120.9(4) ? C234 C235 H235 . . . 122(2) ? C236 C235 H235 . . . 117(2) ? C231 C236 C235 . . . 120.7(3) ? C231 C236 H236 . . . 121.1(18) ? C235 C236 H236 . . . 118.2(18) ? C23 C24 C25 . . . 107.0(2) ? C23 C24 H24 . . . 127.5(16) ? C25 C24 H24 . . . 125.5(16) ? N21 C25 C24 . . . 110.18(18) ? N21 C25 C251 . . . 123.9(2) ? C24 C25 C251 . . . 125.8(2) ? C25 C251 C252 . . . 122.4(2) ? C25 C251 C256 . . . 119.0(2) ? C252 C251 C256 . . . 118.5(2) ? C251 C252 C253 . . . 120.5(2) ? C251 C252 H252 . . . 117.6(16) ? C253 C252 H252 . . . 121.9(16) ? C252 C253 C254 . . . 120.5(3) ? C252 C253 H253 . . . 117.5(16) ? C254 C253 H253 . . . 122.0(16) ? C253 C254 C255 . . . 120.0(3) ? C253 C254 H254 . . . 120.0(19) ? C255 C254 H254 . . . 120.0(19) ? C254 C255 C256 . . . 119.9(3) ? C254 C255 H255 . . . 120.8(19) ? C256 C255 H255 . . . 119.3(19) ? C251 C256 C255 . . . 120.6(3) ? C251 C256 H256 . . . 119.2(13) ? C255 C256 H256 . . . 120.1(13) ? Yb N32 C33 . . . 179.24(18) ? Yb N32 N32 . . '2 655' 72.69(11) ? C33 N32 N32 . . '2 655' 108.06(19) ? N32 C33 C331 . . . 122.0(2) ? N32 C33 C34 . . . 108.9(2) ? C331 C33 C34 . . . 129.0(2) ? C33 C331 C332 . . . 121.2(2) ? C33 C331 C336 . . . 120.6(2) ? C332 C331 C336 . . . 118.2(2) ? C331 C332 C333 . . . 120.5(3) ? C331 C332 H332 . . . 116.4(19) ? C333 C332 H332 . . . 123.0(19) ? C332 C333 C334 . . . 120.0(3) ? C332 C333 H333 . . . 114(2) ? C334 C333 H333 . . . 126(2) ? C333 C334 C335 . . . 119.9(3) ? C333 C334 H334 . . . 123(2) ? C335 C334 H334 . . . 117(2) ? C334 C335 C336 . . . 120.3(3) ? C334 C335 H335 . . . 119(3) ? C336 C335 H335 . . . 121(3) ? C331 C336 C335 . . . 121.1(3) ? C331 C336 H336 . . . 120(2) ? C335 C336 H336 . . . 119(2) ? C33 C34 H34 . . . 126.96(15) ? C33 C34 C33 . . '2 655' 106.1(3) ? H34 C34 C33 . . '2 655' 126.96(15) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2588 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -29 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .73 _reflns_d_resolution_low 11.454 _diffrn_reflns_av_sigmaI/netI .045 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 293 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .037 _refine_ls_wR_factor_all .031 _refine_ls_goodness_of_fit_all .95 _refine_ls_shift/su_mean .002 #========================================================================== # Structure Factor lists should be submitted as separate files #========================================================================== #data_ # but for xtal use the refln data is needed in same block loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_F_squared_meas _refln_F_squared_calc _refln_F_squared_sigma _refln_observed_status _refln_F_meas_friedel _refln_F_sigma_friedel _refln_F_squared_meas_friedel _refln_F_squared_sigma_friedel ? ? ? ? ? ? ? ? ? ? ? ? ? ? #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end #===END