# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 _publ_requested_journal NJC loop_ _publ_author_name 'Glen Berenger Deacon' 'Craig M. Forsyth' 'Peter Junk' 'Stuart G. Leary' _publ_contact_author_name 'Glen Deacon' _publ_contact_author_address ; School of Chemistry Monash University Clayton Victoria AUSTRALIA ; _publ_contact_author_email GLEN.DEACON@SCI.MONASH.EDU.AU _publ_section_title ; A rare earth alloy as a synthetic reagent: contrasting homometallic rare earth and heterobimetallic outcomes. ; # Attachment 'B600868B_1b.cif' data_c:\cforsyth\craig\ladpy\ladpy2\ladpy2ab\ladpy2ab _database_code_depnum_ccdc_archive 'CCDC 298866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 La2 N18' _chemical_formula_sum 'C60 H48 La2 N18' _chemical_formula_weight 1298.98 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.6833(2) _cell_length_b 16.9265(2) _cell_length_c 20.0193(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.219(1) _cell_angle_gamma 90.00 _cell_volume 5428.3(1) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 29214 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6887 _exptl_absorpt_correction_T_max 0.6887 _exptl_absorpt_process_details SORTAV _exptl_special_details ; SORTAV (R.H. Blessing 1997) ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29214 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11588 _reflns_number_gt 9515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0258P)^2^+3.5050P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(13) _refine_ls_number_reflns 11588 _refine_ls_number_parameters 721 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 La1 La 0.91460(3) 0.453616(10) 0.00877(3) 0.01048(5) Uani 1 1 d . . . La2 La 0.91390(3) 0.237174(10) 0.00937(3) 0.01101(5) Uani 1 1 d . . . N1 N 1.0336(4) 0.3599(4) 0.0841(3) 0.0151(14) Uani 1 1 d . . . N2 N 0.9848(4) 0.4530(4) 0.1437(3) 0.0121(15) Uani 1 1 d . . . N3 N 1.0797(4) 0.2395(4) 0.0537(3) 0.0161(13) Uani 1 1 d . . . N4 N 0.9741(4) 0.3324(4) -0.0759(3) 0.0111(14) Uani 1 1 d . . . N5 N 1.0439(3) 0.4496(4) -0.0446(3) 0.0171(14) Uani 1 1 d . . . N6 N 0.8844(4) 0.2323(3) -0.1250(3) 0.0132(14) Uani 1 1 d . . . N7 N 0.7974(4) 0.3523(3) -0.0652(3) 0.0093(14) Uani 1 1 d . . . N8 N 0.8391(4) 0.4510(4) -0.1274(3) 0.0165(16) Uani 1 1 d . . . N9 N 0.7504(4) 0.2386(4) -0.0251(3) 0.0154(13) Uani 1 1 d . . . N10 N 0.8556(4) 0.3373(4) 0.0926(3) 0.0156(16) Uani 1 1 d . . . N11 N 0.7802(3) 0.4506(3) 0.0548(3) 0.0138(13) Uani 1 1 d . . . N12 N 0.9452(4) 0.2398(4) 0.1447(3) 0.0190(16) Uani 1 1 d . . . N13 N 0.9739(4) 0.5968(4) 0.0480(3) 0.0169(14) Uani 1 1 d . . . N14 N 0.8506(4) 0.5947(4) -0.0351(3) 0.0188(14) Uani 1 1 d . . . N15 N 1.1097(3) 0.5821(3) 0.1288(2) 0.0436(12) Uani 1 1 d . . . N16 N 0.9459(4) 0.0938(4) -0.0241(3) 0.0218(13) Uani 1 1 d D . . N17 N 0.8761(3) 0.0985(4) 0.0573(3) 0.0231(13) Uani 1 1 d U . . N18 N 1.0212(3) 0.0975(3) -0.1088(2) 0.0575(15) Uani 1 1 d . . . C1 C 1.0409(4) 0.3958(4) 0.1461(3) 0.0109(15) Uani 1 1 d . . . C2 C 1.1001(4) 0.3782(5) 0.2097(4) 0.0203(16) Uani 1 1 d . . . H2 H 1.1410 0.3385 0.2117 0.024 Uiso 1 1 calc R . . C3 C 1.0983(5) 0.4183(5) 0.2684(4) 0.0256(18) Uani 1 1 d . . . H3 H 1.1381 0.4063 0.3113 0.031 Uiso 1 1 calc R . . C4 C 1.0392(5) 0.4764(5) 0.2661(4) 0.0216(17) Uani 1 1 d . . . H4 H 1.0368 0.5037 0.3070 0.026 Uiso 1 1 calc R . . C5 C 0.9843(5) 0.4932(5) 0.2029(4) 0.0171(16) Uani 1 1 d . . . H5 H 0.9445 0.5341 0.2000 0.020 Uiso 1 1 calc R . . C6 C 1.0991(4) 0.3127(5) 0.0766(3) 0.0127(16) Uani 1 1 d . . . C7 C 1.1798(5) 0.3409(4) 0.0870(4) 0.017(2) Uani 1 1 d . . . H7 H 1.1925 0.3943 0.1003 0.020 Uiso 1 1 calc R . . C8 C 1.2415(4) 0.2910(5) 0.0777(4) 0.0190(18) Uani 1 1 d . . . H8 H 1.2971 0.3095 0.0856 0.023 Uiso 1 1 calc R . . C9 C 1.2214(4) 0.2144(5) 0.0570(4) 0.0231(17) Uani 1 1 d . . . H9 H 1.2629 0.1788 0.0511 0.028 Uiso 1 1 calc R . . C10 C 1.1397(4) 0.1904(4) 0.0450(3) 0.0213(15) Uani 1 1 d . . . H10 H 1.1252 0.1377 0.0302 0.026 Uiso 1 1 calc R . . C11 C 1.0409(4) 0.3785(5) -0.0763(4) 0.0130(16) Uani 1 1 d . . . C12 C 1.1081(5) 0.3552(4) -0.1020(4) 0.0175(19) Uani 1 1 d . . . H12 H 1.1066 0.3056 -0.1244 0.021 Uiso 1 1 calc R . . C13 C 1.1745(5) 0.4037(5) -0.0948(4) 0.0220(17) Uani 1 1 d . . . H13 H 1.2196 0.3873 -0.1117 0.026 Uiso 1 1 calc R . . C14 C 1.1779(5) 0.4768(5) -0.0632(4) 0.0240(18) Uani 1 1 d . . . H14 H 1.2236 0.5117 -0.0589 0.029 Uiso 1 1 calc R . . C15 C 1.1098(4) 0.4968(6) -0.0378(4) 0.0183(16) Uani 1 1 d . . . H15 H 1.1109 0.5461 -0.0149 0.022 Uiso 1 1 calc R . . C16 C 0.9357(4) 0.2902(5) -0.1364(3) 0.0160(17) Uani 1 1 d . . . C17 C 0.9411(4) 0.3056(5) -0.2036(4) 0.0205(17) Uani 1 1 d . . . H17 H 0.9754 0.3471 -0.2118 0.025 Uiso 1 1 calc R . . C18 C 0.8961(5) 0.2596(5) -0.2575(4) 0.0268(18) Uani 1 1 d . . . H18 H 0.8998 0.2689 -0.3033 0.032 Uiso 1 1 calc R . . C19 C 0.8444(5) 0.1987(4) -0.2454(4) 0.0228(16) Uani 1 1 d . . . H19 H 0.8136 0.1660 -0.2822 0.027 Uiso 1 1 calc R . . C20 C 0.8399(5) 0.1883(5) -0.1789(4) 0.0235(18) Uani 1 1 d . . . H20 H 0.8041 0.1484 -0.1702 0.028 Uiso 1 1 calc R . . C21 C 0.7848(4) 0.3898(5) -0.1290(4) 0.0177(17) Uani 1 1 d . . . C22 C 0.7274(4) 0.3671(5) -0.1923(3) 0.0159(15) Uani 1 1 d U . . H22 H 0.6892 0.3252 -0.1935 0.019 Uiso 1 1 calc R . . C23 C 0.7279(4) 0.4070(5) -0.2529(4) 0.0220(17) Uani 1 1 d . . . H23 H 0.6904 0.3921 -0.2961 0.026 Uiso 1 1 calc R . . C24 C 0.7832(5) 0.4685(5) -0.2499(4) 0.0243(19) Uani 1 1 d . . . H24 H 0.7833 0.4976 -0.2904 0.029 Uiso 1 1 calc R . . C25 C 0.8385(5) 0.4865(5) -0.1861(4) 0.0205(18) Uani 1 1 d . . . H25 H 0.8784 0.5270 -0.1845 0.025 Uiso 1 1 calc R . . C26 C 0.7296(4) 0.3107(5) -0.0561(3) 0.0142(17) Uani 1 1 d . . . C27 C 0.6471(5) 0.3395(4) -0.0726(4) 0.017(2) Uani 1 1 d . . . H27 H 0.6332 0.3890 -0.0952 0.020 Uiso 1 1 calc R . . C28 C 0.5871(5) 0.2949(5) -0.0554(4) 0.0207(18) Uani 1 1 d . . . H28 H 0.5317 0.3143 -0.0645 0.025 Uiso 1 1 calc R . . C29 C 0.6077(4) 0.2203(5) -0.0242(4) 0.0211(16) Uani 1 1 d . . . H29 H 0.5666 0.1874 -0.0139 0.025 Uiso 1 1 calc R . . C30 C 0.6897(4) 0.1973(5) -0.0093(3) 0.0204(15) Uani 1 1 d . . . H30 H 0.7045 0.1482 0.0139 0.025 Uiso 1 1 calc R . . C31 C 0.7839(4) 0.3822(5) 0.0891(3) 0.0127(16) Uani 1 1 d . . . C32 C 0.7179(5) 0.3578(5) 0.1154(4) 0.0174(18) Uani 1 1 d . . . H32 H 0.7211 0.3091 0.1396 0.021 Uiso 1 1 calc R . . C33 C 0.6484(4) 0.4056(5) 0.1053(4) 0.0220(18) Uani 1 1 d . . . H33 H 0.6035 0.3912 0.1234 0.026 Uiso 1 1 calc R . . C34 C 0.6459(5) 0.4759(4) 0.0679(4) 0.0196(16) Uani 1 1 d . . . H34 H 0.5988 0.5099 0.0598 0.023 Uiso 1 1 calc R . . C35 C 0.7096(4) 0.4944(5) 0.0441(4) 0.0185(16) Uani 1 1 d . . . H35 H 0.7058 0.5416 0.0176 0.022 Uiso 1 1 calc R . . C36 C 0.8932(4) 0.2981(4) 0.1522(3) 0.0117(15) Uani 1 1 d . . . C37 C 0.8867(5) 0.3155(5) 0.2208(4) 0.0185(16) Uani 1 1 d . . . H37 H 0.8478 0.3538 0.2270 0.022 Uiso 1 1 calc R . . C38 C 0.9366(4) 0.2768(5) 0.2768(4) 0.0244(17) Uani 1 1 d . . . H38 H 0.9342 0.2896 0.3224 0.029 Uiso 1 1 calc R . . C39 C 0.9906(5) 0.2186(4) 0.2670(4) 0.0252(17) Uani 1 1 d . . . H39 H 1.0262 0.1914 0.3055 0.030 Uiso 1 1 calc R . . C40 C 0.9913(5) 0.2016(5) 0.2008(4) 0.0202(17) Uani 1 1 d . . . H40 H 1.0265 0.1601 0.1940 0.024 Uiso 1 1 calc R . . C41 C 0.9115(7) 0.6420(2) 0.0061(6) 0.0178(9) Uani 1 1 d U . . C42 C 0.9084(5) 0.7246(2) -0.0021(4) 0.0231(15) Uani 1 1 d . . . H42 H 0.9485 0.7574 0.0285 0.028 Uiso 1 1 calc R . . C43 C 0.8475(3) 0.7564(3) -0.0543(3) 0.0320(12) Uani 1 1 d . . . H43 H 0.8460 0.8119 -0.0618 0.038 Uiso 1 1 calc R . . C44 C 0.7872(4) 0.7086(4) -0.0968(3) 0.0281(14) Uani 1 1 d . . . H44 H 0.7435 0.7306 -0.1332 0.034 Uiso 1 1 calc R . . C45 C 0.7918(5) 0.6302(6) -0.0854(4) 0.029(2) Uani 1 1 d . . . H45 H 0.7504 0.5978 -0.1152 0.034 Uiso 1 1 calc R . . C46 C 1.0370(5) 0.6266(5) 0.1031(4) 0.0178(17) Uani 1 1 d U . . C47 C 1.0248(3) 0.6941(3) 0.1353(2) 0.0173(11) Uani 1 1 d . . . H47 H 0.9741 0.7229 0.1196 0.021 Uiso 1 1 calc R . . C48 C 1.0860(4) 0.7192(3) 0.1900(3) 0.0431(15) Uani 1 1 d . . . H48 H 1.0777 0.7674 0.2115 0.052 Uiso 1 1 calc R . . C49 C 1.1592(4) 0.6802(4) 0.2169(3) 0.0481(16) Uani 1 1 d . . . H49 H 1.2007 0.7006 0.2557 0.058 Uiso 1 1 calc R . . C50 C 1.1712(3) 0.6106(4) 0.1861(2) 0.0364(13) Uani 1 1 d . . . H50 H 1.2215 0.5818 0.2039 0.044 Uiso 1 1 calc R . . C51 C 0.9169(7) 0.0519(3) 0.0203(4) 0.0273(17) Uani 1 1 d DU . . C52 C 0.9271(3) -0.0298(3) 0.0387(3) 0.0363(13) Uani 1 1 d U . . H52 H 0.9508 -0.0650 0.0125 0.044 Uiso 1 1 calc R . . C53 C 0.9026(3) -0.0574(4) 0.0945(4) 0.0476(16) Uani 1 1 d U . . H53 H 0.9127 -0.1109 0.1085 0.057 Uiso 1 1 calc R . . C54 C 0.8641(4) -0.0087(4) 0.1297(4) 0.0411(17) Uani 1 1 d U . . H54 H 0.8455 -0.0278 0.1675 0.049 Uiso 1 1 calc R . . C55 C 0.8527(5) 0.0685(5) 0.1093(4) 0.0300(18) Uani 1 1 d U . . H55 H 0.8262 0.1026 0.1343 0.036 Uiso 1 1 calc R . . C56 C 0.9655(5) 0.0575(5) -0.0792(4) 0.037(2) Uani 1 1 d . . . C57 C 0.9281(4) -0.0102(4) -0.1065(3) 0.0333(15) Uani 1 1 d . . . H57 H 0.8903 -0.0367 -0.0865 0.040 Uiso 1 1 calc R . . C58 C 0.9461(4) -0.0382(4) -0.1620(4) 0.066(2) Uani 1 1 d . . . H58 H 0.9192 -0.0858 -0.1814 0.080 Uiso 1 1 calc R . . C59 C 0.9994(4) -0.0054(5) -0.1938(3) 0.067(2) Uani 1 1 d . . . H59 H 1.0097 -0.0299 -0.2332 0.081 Uiso 1 1 calc R . . C60 C 1.0391(4) 0.0653(4) -0.1676(3) 0.0540(18) Uani 1 1 d . . . H60 H 1.0766 0.0905 -0.1888 0.065 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 La1 0.01011(9) 0.01026(9) 0.01127(9) 0.0003(3) 0.00333(7) 0.0003(3) La2 0.01123(9) 0.01030(9) 0.01140(9) 0.0001(3) 0.00298(7) -0.0001(3) N1 0.008(3) 0.022(3) 0.015(3) -0.006(2) 0.003(3) 0.000(2) N2 0.013(3) 0.009(3) 0.016(3) -0.001(2) 0.008(3) 0.004(2) N3 0.014(3) 0.014(3) 0.018(3) -0.004(2) 0.002(2) 0.000(2) N4 0.005(3) 0.014(3) 0.015(3) -0.001(2) 0.004(3) -0.003(2) N5 0.014(3) 0.024(4) 0.014(3) 0.004(2) 0.005(2) 0.000(2) N6 0.013(3) 0.012(3) 0.018(3) -0.004(2) 0.009(3) -0.001(2) N7 0.017(3) 0.007(3) 0.004(3) 0.0030(19) 0.003(2) 0.000(2) N8 0.016(4) 0.020(4) 0.011(3) 0.003(3) 0.000(3) 0.005(3) N9 0.013(3) 0.014(3) 0.018(3) 0.000(2) 0.003(2) -0.005(2) N10 0.022(4) 0.015(4) 0.008(3) 0.000(2) 0.001(3) -0.003(2) N11 0.020(3) 0.009(3) 0.016(3) 0.002(2) 0.011(2) 0.002(2) N12 0.023(4) 0.017(3) 0.013(3) 0.004(2) -0.001(3) 0.000(3) N13 0.026(3) 0.012(3) 0.014(3) -0.009(2) 0.008(2) -0.008(3) N14 0.015(3) 0.019(4) 0.021(3) -0.006(3) 0.004(2) 0.001(3) N15 0.043(3) 0.058(3) 0.032(3) 0.006(2) 0.013(2) -0.015(2) N16 0.025(3) 0.020(3) 0.021(3) -0.005(2) 0.007(2) 0.001(2) N17 0.029(3) 0.014(3) 0.026(3) 0.006(2) 0.008(2) -0.004(2) N18 0.067(4) 0.065(4) 0.035(3) -0.004(3) 0.004(3) 0.034(3) C1 0.015(4) 0.011(3) 0.005(3) -0.002(2) 0.000(3) 0.001(3) C2 0.017(3) 0.023(3) 0.023(3) -0.004(3) 0.009(3) 0.008(3) C3 0.034(4) 0.031(4) 0.010(3) -0.004(3) 0.003(3) -0.003(3) C4 0.021(4) 0.027(4) 0.017(4) -0.003(3) 0.005(3) 0.001(3) C5 0.022(4) 0.015(3) 0.016(4) -0.010(3) 0.008(3) -0.003(3) C6 0.012(4) 0.012(4) 0.013(4) 0.001(3) 0.002(3) 0.000(3) C7 0.024(5) 0.009(4) 0.016(4) 0.003(3) 0.004(4) 0.001(3) C8 0.009(4) 0.031(5) 0.016(4) 0.002(3) 0.001(3) 0.004(3) C9 0.018(3) 0.028(4) 0.022(3) -0.005(3) 0.005(2) 0.010(3) C10 0.022(3) 0.014(3) 0.027(3) -0.003(3) 0.003(2) 0.003(2) C11 0.015(4) 0.013(4) 0.010(3) -0.004(3) 0.002(3) 0.000(3) C12 0.020(4) 0.015(4) 0.020(4) -0.003(3) 0.010(3) -0.002(3) C13 0.022(4) 0.025(4) 0.022(3) 0.003(3) 0.010(3) 0.005(3) C14 0.021(3) 0.038(5) 0.017(3) 0.001(3) 0.012(2) -0.007(3) C15 0.016(3) 0.022(4) 0.014(3) 0.001(2) 0.001(2) -0.007(3) C16 0.013(4) 0.022(4) 0.011(3) -0.001(3) 0.000(3) 0.006(3) C17 0.017(4) 0.026(4) 0.020(4) 0.010(3) 0.009(3) 0.003(3) C18 0.039(4) 0.030(4) 0.008(3) -0.005(2) 0.003(3) 0.007(3) C19 0.026(3) 0.022(4) 0.019(3) -0.009(2) 0.003(2) -0.004(3) C20 0.026(4) 0.024(4) 0.018(3) -0.006(3) 0.001(3) -0.005(3) C21 0.010(4) 0.020(4) 0.028(4) -0.002(3) 0.013(3) 0.004(3) C22 0.012(3) 0.025(3) 0.007(3) -0.002(2) -0.003(2) -0.003(2) C23 0.011(3) 0.037(4) 0.015(3) -0.005(3) -0.002(3) -0.005(3) C24 0.029(4) 0.028(4) 0.017(4) 0.014(3) 0.008(3) 0.005(3) C25 0.018(4) 0.018(4) 0.027(4) 0.003(3) 0.009(3) -0.001(3) C26 0.014(4) 0.021(5) 0.008(4) -0.005(3) 0.005(3) -0.005(4) C27 0.007(4) 0.031(5) 0.011(4) 0.007(3) 0.001(3) 0.000(3) C28 0.017(4) 0.027(5) 0.020(4) 0.005(3) 0.007(3) 0.007(3) C29 0.012(3) 0.027(4) 0.028(3) 0.004(3) 0.011(2) -0.002(2) C30 0.022(3) 0.016(3) 0.021(3) -0.001(2) 0.002(2) -0.007(2) C31 0.009(4) 0.018(4) 0.009(3) -0.008(3) 0.001(3) -0.001(3) C32 0.017(4) 0.021(5) 0.014(4) -0.001(3) 0.004(3) -0.006(3) C33 0.007(3) 0.035(5) 0.027(4) 0.004(3) 0.009(3) 0.000(3) C34 0.015(3) 0.016(3) 0.029(3) 0.002(3) 0.008(3) 0.007(2) C35 0.022(3) 0.010(3) 0.025(3) 0.001(3) 0.010(3) 0.001(3) C36 0.013(4) 0.010(3) 0.015(3) -0.001(3) 0.007(3) -0.002(3) C37 0.025(4) 0.021(3) 0.011(3) 0.005(3) 0.006(3) 0.001(3) C38 0.023(3) 0.038(4) 0.015(3) -0.002(3) 0.009(3) 0.002(3) C39 0.025(3) 0.029(4) 0.019(3) 0.012(3) 0.002(2) 0.002(3) C40 0.022(4) 0.016(3) 0.023(4) 0.006(2) 0.007(3) 0.004(2) C41 0.018(2) 0.0223(18) 0.018(2) 0.007(3) 0.0127(16) 0.011(3) C42 0.017(3) 0.0168(19) 0.037(5) 0.002(2) 0.011(3) -0.008(3) C43 0.040(3) 0.016(3) 0.049(3) 0.010(2) 0.027(3) 0.008(2) C44 0.036(3) 0.025(3) 0.023(3) 0.009(2) 0.007(2) 0.017(2) C45 0.028(4) 0.038(5) 0.019(4) -0.003(4) 0.006(3) 0.006(4) C46 0.025(3) 0.013(3) 0.020(3) -0.004(3) 0.015(3) -0.009(3) C47 0.033(3) 0.012(3) 0.012(2) -0.0046(19) 0.013(2) -0.008(2) C48 0.074(4) 0.031(3) 0.036(3) -0.015(3) 0.034(3) -0.029(3) C49 0.052(4) 0.068(4) 0.024(3) -0.009(3) 0.008(3) -0.031(3) C50 0.033(3) 0.054(4) 0.022(3) 0.002(3) 0.008(2) -0.016(3) C51 0.006(2) 0.028(2) 0.037(5) -0.001(2) -0.011(3) -0.004(3) C52 0.028(3) 0.011(2) 0.061(3) 0.009(2) -0.003(3) 0.000(2) C53 0.021(3) 0.033(3) 0.078(5) 0.032(3) -0.003(3) -0.006(2) C54 0.032(4) 0.032(3) 0.049(4) 0.027(3) -0.006(3) -0.007(3) C55 0.031(4) 0.023(4) 0.036(4) 0.013(3) 0.009(3) -0.012(3) C56 0.030(4) 0.037(4) 0.034(4) 0.006(3) -0.006(3) 0.013(3) C57 0.034(4) 0.018(3) 0.039(3) -0.015(3) -0.005(3) 0.002(3) C58 0.061(5) 0.043(4) 0.076(5) -0.030(4) -0.012(4) 0.019(3) C59 0.071(5) 0.070(5) 0.043(4) -0.030(4) -0.013(3) 0.044(4) C60 0.056(4) 0.071(5) 0.030(3) -0.010(3) 0.004(3) 0.034(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 La1 N2 2.626(6) . ? La1 N13 2.652(6) . ? La1 N11 2.653(5) . ? La1 N1 2.658(7) . ? La1 N5 2.662(6) . ? La1 N14 2.662(6) . ? La1 N8 2.664(6) . ? La1 N7 2.709(6) . ? La1 N10 2.930(6) . ? La1 N4 3.001(6) . ? La1 C1 3.118(7) . ? La1 La2 3.6637(8) . ? La2 N6 2.597(6) . ? La2 N16 2.612(6) . ? La2 N12 2.612(6) . ? La2 N9 2.621(6) . ? La2 N3 2.659(6) . ? La2 N17 2.677(6) . ? La2 N4 2.734(6) . ? La2 N10 2.739(6) . ? La2 N7 2.860(6) . ? La2 N1 2.979(7) . ? N1 C1 1.357(9) . ? N1 C6 1.394(9) . ? N2 C1 1.337(9) . ? N2 C5 1.369(9) . ? N3 C6 1.329(9) . ? N3 C10 1.350(9) . ? N4 C11 1.363(9) . ? N4 C16 1.398(9) . ? N5 C15 1.335(9) . ? N5 C11 1.356(9) . ? N6 C20 1.350(9) . ? N6 C16 1.362(9) . ? N7 C26 1.387(9) . ? N7 C21 1.389(9) . ? N8 C25 1.317(9) . ? N8 C21 1.370(9) . ? N9 C30 1.338(8) . ? N9 C26 1.369(10) . ? N10 C36 1.357(9) . ? N10 C31 1.403(9) . ? N11 C31 1.338(9) . ? N11 C35 1.357(9) . ? N12 C40 1.337(9) . ? N12 C36 1.350(9) . ? N13 C41 1.374(11) . ? N13 C46 1.389(9) . ? N14 C45 1.337(10) . ? N14 C41 1.373(11) . ? N15 C50 1.395(6) . ? N15 C46 1.397(9) . ? N16 C51 1.330(9) . ? N16 C56 1.380(9) . ? N17 C55 1.312(8) . ? N17 C51 1.384(10) . ? N18 C60 1.404(7) . ? N18 C56 1.407(9) . ? C1 C2 1.407(9) . ? C2 C3 1.365(9) . ? C3 C4 1.385(11) . ? C4 C5 1.368(9) . ? C6 C7 1.388(10) . ? C7 C8 1.384(10) . ? C8 C9 1.374(11) . ? C9 C10 1.377(10) . ? C11 C12 1.414(10) . ? C12 C13 1.354(10) . ? C13 C14 1.383(10) . ? C14 C15 1.409(11) . ? C16 C17 1.398(9) . ? C17 C18 1.372(11) . ? C18 C19 1.407(10) . ? C19 C20 1.366(9) . ? C21 C22 1.411(10) . ? C22 C23 1.390(9) . ? C23 C24 1.381(10) . ? C24 C25 1.385(10) . ? C26 C27 1.410(10) . ? C27 C28 1.372(10) . ? C28 C29 1.406(11) . ? C29 C30 1.373(10) . ? C31 C32 1.408(9) . ? C32 C33 1.383(10) . ? C33 C34 1.400(10) . ? C34 C35 1.319(10) . ? C36 C37 1.437(9) . ? C37 C38 1.363(10) . ? C38 C39 1.385(10) . ? C39 C40 1.359(10) . ? C41 C42 1.407(5) . ? C42 C43 1.349(9) . ? C43 C44 1.384(8) . ? C44 C45 1.345(11) . ? C46 C47 1.357(9) . ? C47 C48 1.341(7) . ? C48 C49 1.360(8) . ? C49 C50 1.370(8) . ? C51 C52 1.429(6) . ? C52 C53 1.373(8) . ? C53 C54 1.358(9) . ? C54 C55 1.367(10) . ? C56 C57 1.345(10) . ? C57 C58 1.318(9) . ? C58 C59 1.348(10) . ? C59 C60 1.396(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 La1 N13 71.16(18) . . ? N2 La1 N11 79.62(18) . . ? N13 La1 N11 101.31(18) . . ? N2 La1 N1 50.65(19) . . ? N13 La1 N1 102.69(19) . . ? N11 La1 N1 111.18(17) . . ? N2 La1 N5 103.53(19) . . ? N13 La1 N5 82.24(19) . . ? N11 La1 N5 175.93(19) . . ? N1 La1 N5 69.64(18) . . ? N2 La1 N14 111.44(19) . . ? N13 La1 N14 50.23(9) . . ? N11 La1 N14 80.33(18) . . ? N1 La1 N14 152.85(19) . . ? N5 La1 N14 100.69(19) . . ? N2 La1 N8 178.0(2) . . ? N13 La1 N8 110.43(19) . . ? N11 La1 N8 98.71(19) . . ? N1 La1 N8 129.4(2) . . ? N5 La1 N8 78.08(19) . . ? N14 La1 N8 69.29(19) . . ? N2 La1 N7 127.28(18) . . ? N13 La1 N7 153.23(18) . . ? N11 La1 N7 68.08(17) . . ? N1 La1 N7 104.07(10) . . ? N5 La1 N7 107.86(18) . . ? N14 La1 N7 103.05(17) . . ? N8 La1 N7 50.76(19) . . ? N2 La1 N10 62.14(19) . . ? N13 La1 N10 126.97(17) . . ? N11 La1 N10 48.40(18) . . ? N1 La1 N10 65.85(19) . . ? N5 La1 N10 130.72(19) . . ? N14 La1 N10 128.58(18) . . ? N8 La1 N10 115.87(19) . . ? N7 La1 N10 65.24(18) . . ? N2 La1 N4 117.06(18) . . ? N13 La1 N4 129.59(17) . . ? N11 La1 N4 128.91(17) . . ? N1 La1 N4 66.42(18) . . ? N5 La1 N4 47.41(18) . . ? N14 La1 N4 126.32(17) . . ? N8 La1 N4 63.07(18) . . ? N7 La1 N4 63.93(17) . . ? N10 La1 N4 94.65(7) . . ? N2 La1 C1 25.10(17) . . ? N13 La1 C1 85.5(2) . . ? N11 La1 C1 96.65(17) . . ? N1 La1 C1 25.62(18) . . ? N5 La1 C1 85.55(17) . . ? N14 La1 C1 133.01(19) . . ? N8 La1 C1 155.06(19) . . ? N7 La1 C1 119.35(18) . . ? N10 La1 C1 62.37(19) . . ? N4 La1 C1 92.01(17) . . ? N2 La1 La2 89.61(13) . . ? N13 La1 La2 156.06(14) . . ? N11 La1 La2 88.61(12) . . ? N1 La1 La2 53.39(14) . . ? N5 La1 La2 88.84(14) . . ? N14 La1 La2 153.71(14) . . ? N8 La1 La2 89.17(14) . . ? N7 La1 La2 50.67(13) . . ? N10 La1 La2 47.49(12) . . ? N4 La1 La2 47.16(11) . . ? C1 La1 La2 71.66(13) . . ? N6 La2 N16 72.42(18) . . ? N6 La2 N12 178.97(18) . . ? N16 La2 N12 106.61(18) . . ? N6 La2 N9 81.11(18) . . ? N16 La2 N9 102.34(19) . . ? N12 La2 N9 99.5(2) . . ? N6 La2 N3 103.00(19) . . ? N16 La2 N3 80.29(19) . . ? N12 La2 N3 76.44(19) . . ? N9 La2 N3 175.7(2) . . ? N6 La2 N17 110.35(18) . . ? N16 La2 N17 50.41(13) . . ? N12 La2 N17 69.02(18) . . ? N9 La2 N17 76.74(18) . . ? N3 La2 N17 102.74(18) . . ? N6 La2 N4 50.85(18) . . ? N16 La2 N4 104.49(17) . . ? N12 La2 N4 129.46(19) . . ? N9 La2 N4 111.53(18) . . ? N3 La2 N4 70.75(18) . . ? N17 La2 N4 154.80(17) . . ? N6 La2 N10 130.77(19) . . ? N16 La2 N10 149.76(18) . . ? N12 La2 N10 50.3(2) . . ? N9 La2 N10 68.52(19) . . ? N3 La2 N10 107.49(19) . . ? N17 La2 N10 99.54(17) . . ? N4 La2 N10 105.65(8) . . ? N6 La2 N7 64.94(18) . . ? N16 La2 N7 131.06(17) . . ? N12 La2 N7 116.08(18) . . ? N9 La2 N7 49.51(18) . . ? N3 La2 N7 130.98(18) . . ? N17 La2 N7 126.22(17) . . ? N4 La2 N7 65.61(17) . . ? N10 La2 N7 65.86(18) . . ? N6 La2 N1 116.69(18) . . ? N16 La2 N1 128.32(17) . . ? N12 La2 N1 63.60(19) . . ? N9 La2 N1 128.93(18) . . ? N3 La2 N1 48.13(18) . . ? N17 La2 N1 128.55(18) . . ? N4 La2 N1 65.87(18) . . ? N10 La2 N1 64.21(18) . . ? N7 La2 N1 92.86(8) . . ? N6 La2 La1 91.62(13) . . ? N16 La2 La1 157.98(12) . . ? N12 La2 La1 89.23(14) . . ? N9 La2 La1 89.64(14) . . ? N3 La2 La1 88.97(14) . . ? N17 La2 La1 151.57(12) . . ? N4 La2 La1 53.60(13) . . ? N10 La2 La1 52.05(13) . . ? N7 La2 La1 47.11(12) . . ? N1 La2 La1 45.75(13) . . ? C1 N1 C6 118.9(7) . . ? C1 N1 La1 96.5(4) . . ? C6 N1 La1 139.8(5) . . ? C1 N1 La2 130.4(5) . . ? C6 N1 La2 89.0(4) . . ? La1 N1 La2 80.86(18) . . ? C1 N2 C5 120.1(6) . . ? C1 N2 La1 98.5(4) . . ? C5 N2 La1 141.2(5) . . ? C6 N3 C10 120.1(6) . . ? C6 N3 La2 105.0(4) . . ? C10 N3 La2 133.4(5) . . ? C11 N4 C16 117.7(6) . . ? C11 N4 La2 141.7(5) . . ? C16 N4 La2 94.6(4) . . ? C11 N4 La1 90.7(4) . . ? C16 N4 La1 134.0(4) . . ? La2 N4 La1 79.25(15) . . ? C15 N5 C11 120.0(6) . . ? C15 N5 La1 133.0(5) . . ? C11 N5 La1 106.4(4) . . ? C20 N6 C16 119.6(7) . . ? C20 N6 La2 138.4(5) . . ? C16 N6 La2 101.8(4) . . ? C26 N7 C21 115.7(6) . . ? C26 N7 La1 137.7(5) . . ? C21 N7 La1 96.5(4) . . ? C26 N7 La2 92.6(4) . . ? C21 N7 La2 134.2(4) . . ? La1 N7 La2 82.22(18) . . ? C25 N8 C21 118.8(7) . . ? C25 N8 La1 142.1(6) . . ? C21 N8 La1 99.1(4) . . ? C30 N9 C26 117.5(6) . . ? C30 N9 La2 137.1(5) . . ? C26 N9 La2 103.9(4) . . ? C36 N10 C31 119.2(6) . . ? C36 N10 La2 94.4(4) . . ? C31 N10 La2 138.4(5) . . ? C36 N10 La1 133.3(5) . . ? C31 N10 La1 91.5(4) . . ? La2 N10 La1 80.45(17) . . ? C31 N11 C35 117.9(6) . . ? C31 N11 La1 105.8(4) . . ? C35 N11 La1 135.6(5) . . ? C40 N12 C36 119.7(7) . . ? C40 N12 La2 139.9(5) . . ? C36 N12 La2 100.3(4) . . ? C41 N13 C46 124.0(7) . . ? C41 N13 La1 99.9(4) . . ? C46 N13 La1 134.8(5) . . ? C45 N14 C41 117.0(7) . . ? C45 N14 La1 142.6(6) . . ? C41 N14 La1 99.5(4) . . ? C50 N15 C46 118.7(5) . . ? C51 N16 C56 120.5(7) . . ? C51 N16 La2 100.7(4) . . ? C56 N16 La2 136.9(5) . . ? C55 N17 C51 120.2(7) . . ? C55 N17 La2 140.9(5) . . ? C51 N17 La2 96.2(4) . . ? C60 N18 C56 119.1(7) . . ? N2 C1 N1 114.1(6) . . ? N2 C1 C2 119.6(6) . . ? N1 C1 C2 126.3(7) . . ? N2 C1 La1 56.4(4) . . ? N1 C1 La1 57.9(4) . . ? C2 C1 La1 174.0(5) . . ? C3 C2 C1 119.6(7) . . ? C2 C3 C4 120.8(7) . . ? C5 C4 C3 117.7(7) . . ? C4 C5 N2 122.2(8) . . ? N3 C6 C7 120.3(6) . . ? N3 C6 N1 116.7(6) . . ? C7 C6 N1 122.9(7) . . ? C8 C7 C6 119.8(7) . . ? C9 C8 C7 119.3(7) . . ? C8 C9 C10 118.5(7) . . ? N3 C10 C9 121.9(7) . . ? N5 C11 N4 115.4(6) . . ? N5 C11 C12 119.3(7) . . ? N4 C11 C12 125.2(7) . . ? C13 C12 C11 120.0(7) . . ? C12 C13 C14 121.3(7) . . ? C13 C14 C15 116.5(8) . . ? N5 C15 C14 122.9(8) . . ? N6 C16 C17 120.5(7) . . ? N6 C16 N4 112.3(6) . . ? C17 C16 N4 127.0(7) . . ? C18 C17 C16 118.9(8) . . ? C17 C18 C19 120.4(7) . . ? C20 C19 C18 117.8(7) . . ? N6 C20 C19 122.7(8) . . ? N8 C21 N7 113.2(7) . . ? N8 C21 C22 120.4(7) . . ? N7 C21 C22 126.2(7) . . ? C23 C22 C21 118.8(7) . . ? C24 C23 C22 119.7(7) . . ? C23 C24 C25 118.0(7) . . ? N8 C25 C24 124.1(8) . . ? N9 C26 N7 113.6(6) . . ? N9 C26 C27 121.4(6) . . ? N7 C26 C27 124.9(7) . . ? C28 C27 C26 118.9(7) . . ? C27 C28 C29 120.0(7) . . ? C30 C29 C28 117.2(7) . . ? N9 C30 C29 125.0(7) . . ? N11 C31 N10 114.2(6) . . ? N11 C31 C32 121.1(7) . . ? N10 C31 C32 124.6(7) . . ? C33 C32 C31 119.0(7) . . ? C32 C33 C34 118.3(7) . . ? C35 C34 C33 119.3(7) . . ? C34 C35 N11 124.4(8) . . ? N12 C36 N10 114.4(6) . . ? N12 C36 C37 118.6(7) . . ? N10 C36 C37 126.9(7) . . ? C38 C37 C36 119.7(7) . . ? C37 C38 C39 119.8(7) . . ? C40 C39 C38 118.2(7) . . ? N12 C40 C39 123.9(8) . . ? N14 C41 N13 110.4(3) . . ? N14 C41 C42 120.9(9) . . ? N13 C41 C42 128.5(9) . . ? C43 C42 C41 118.8(7) . . ? C42 C43 C44 120.2(5) . . ? C45 C44 C43 118.4(6) . . ? N14 C45 C44 124.5(8) . . ? C47 C46 N13 120.2(7) . . ? C47 C46 N15 120.6(6) . . ? N13 C46 N15 119.0(6) . . ? C48 C47 C46 118.3(6) . . ? C47 C48 C49 124.3(5) . . ? C48 C49 C50 117.9(5) . . ? C49 C50 N15 120.0(5) . . ? N16 C51 N17 112.3(4) . . ? N16 C51 C52 130.5(8) . . ? N17 C51 C52 117.0(7) . . ? C53 C52 C51 119.8(6) . . ? C54 C53 C52 120.6(6) . . ? C53 C54 C55 118.0(7) . . ? N17 C55 C54 124.1(8) . . ? C57 C56 N16 121.2(7) . . ? C57 C56 N18 121.7(8) . . ? N16 C56 N18 117.0(7) . . ? C58 C57 C56 117.4(8) . . ? C57 C58 C59 125.8(7) . . ? C58 C59 C60 118.9(6) . . ? C59 C60 N18 117.2(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.039 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.100 # Attachment 'B600868B_1a.cif' data_C #:\My Documents\Craig\ladpy\ladpyabs\LADPYABS.CIF _database_code_depnum_ccdc_archive 'CCDC 298867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(2,2'-dipyridylamido)bis(mu-2,2'dipyridylamido)dilanthanum(III) ; _chemical_name_common ladpyabs _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 La N9' _chemical_formula_weight 649.49 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5878(1) _cell_length_b 15.3676(2) _cell_length_c 16.5439(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.688(1) _cell_angle_gamma 90.00 _cell_volume 2636.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 23117 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 28.14 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.815 _exptl_absorpt_process_details SORTAV _exptl_special_details ; SORTAV (R.H. Blessing 1997) ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23117 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 28.14 _reflns_number_total 6260 _reflns_number_gt 5308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0510P)^2^+0.0000P] 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 6260 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 La1 La 0.587891(13) 0.601489(9) 0.076220(9) 0.01163(7) Uani 1 1 d . . . N1 N 0.57401(19) 0.42239(16) 0.06815(13) 0.0138(5) Uani 1 1 d . . . N2 N 0.3828(2) 0.35499(14) 0.07298(13) 0.0150(5) Uani 1 1 d . . . N3 N 0.7713(2) 0.48625(14) 0.07463(14) 0.0160(5) Uani 1 1 d . . . N4 N 0.6129(2) 0.58526(14) 0.23096(14) 0.0149(5) Uani 1 1 d . . . N5 N 0.4094(2) 0.56429(14) 0.15980(14) 0.0158(5) Uani 1 1 d . . . N6 N 0.7020(2) 0.57827(16) 0.37577(15) 0.0228(5) Uani 1 1 d . . . N7 N 0.6872(2) 0.74759(14) 0.10445(14) 0.0175(5) Uani 1 1 d . . . N8 N 0.4793(2) 0.74961(14) 0.11231(14) 0.0172(5) Uani 1 1 d . . . N9 N 0.8834(2) 0.71033(14) 0.08006(14) 0.0174(5) Uani 1 1 d . . . C1 C 0.5003(2) 0.37771(16) 0.11609(16) 0.0123(5) Uani 1 1 d . . . C2 C 0.5353(2) 0.36374(17) 0.20125(17) 0.0173(5) Uani 1 1 d . . . H2 H 0.6186 0.3797 0.2308 0.021 Uiso 1 1 calc R . . C3 C 0.4475(3) 0.32671(17) 0.24146(17) 0.0207(6) Uani 1 1 d . . . H3 H 0.4689 0.3181 0.2995 0.025 Uiso 1 1 calc R . . C4 C 0.3269(3) 0.30170(17) 0.19689(17) 0.0189(6) Uani 1 1 d . . . H4 H 0.2656 0.2749 0.2235 0.023 Uiso 1 1 calc R . . C5 C 0.2993(2) 0.31682(17) 0.11373(17) 0.0178(6) Uani 1 1 d . . . H5 H 0.2172 0.2996 0.0831 0.021 Uiso 1 1 calc R . . C6 C 0.7072(3) 0.41324(17) 0.08834(17) 0.0139(5) Uani 1 1 d . . . C7 C 0.7740(3) 0.33686(17) 0.11730(17) 0.0190(6) Uani 1 1 d . . . H7 H 0.7284 0.2862 0.1276 0.023 Uiso 1 1 calc R . . C8 C 0.9066(3) 0.33649(18) 0.13054(18) 0.0216(6) Uani 1 1 d . . . H8 H 0.9532 0.2853 0.1501 0.026 Uiso 1 1 calc R . . C9 C 0.9728(3) 0.41158(18) 0.11513(19) 0.0217(6) Uani 1 1 d . . . H9 H 1.0643 0.4123 0.1236 0.026 Uiso 1 1 calc R . . C10 C 0.9017(2) 0.48399(18) 0.08746(18) 0.0202(6) Uani 1 1 d . . . H10 H 0.9460 0.5351 0.0767 0.024 Uiso 1 1 calc R . . C11 C 0.4858(3) 0.57770(16) 0.23598(16) 0.0145(5) Uani 1 1 d . . . C12 C 0.4283(3) 0.58512(18) 0.30592(19) 0.0207(6) Uani 1 1 d . . . H12 H 0.4801 0.5929 0.3594 0.025 Uiso 1 1 calc R . . C13 C 0.2962(3) 0.58088(19) 0.2951(2) 0.0237(6) Uani 1 1 d . . . H13 H 0.2569 0.5871 0.3416 0.028 Uiso 1 1 calc R . . C14 C 0.2195(3) 0.56761(19) 0.21763(19) 0.0246(6) Uani 1 1 d . . . H14 H 0.1283 0.5643 0.2100 0.030 Uiso 1 1 calc R . . C15 C 0.2808(2) 0.55940(17) 0.15208(18) 0.0188(6) Uani 1 1 d . . . H15 H 0.2295 0.5498 0.0987 0.023 Uiso 1 1 calc R . . C16 C 0.7128(3) 0.59698(15) 0.29729(18) 0.0159(6) Uani 1 1 d . . . C17 C 0.8316(3) 0.62746(17) 0.28041(18) 0.0195(6) Uani 1 1 d . . . H17 H 0.8388 0.6405 0.2254 0.023 Uiso 1 1 calc R . . C18 C 0.9361(3) 0.63787(18) 0.3443(2) 0.0256(7) Uani 1 1 d . . . H18 H 1.0157 0.6587 0.3338 0.031 Uiso 1 1 calc R . . C19 C 0.9244(3) 0.6176(2) 0.42446(19) 0.0302(8) Uani 1 1 d . . . H19 H 0.9953 0.6236 0.4696 0.036 Uiso 1 1 calc R . . C20 C 0.8072(3) 0.5888(2) 0.4356(2) 0.0292(7) Uani 1 1 d . . . H20 H 0.7994 0.5751 0.4904 0.035 Uiso 1 1 calc R . . C21 C 0.5899(2) 0.79677(16) 0.12283(16) 0.0162(5) Uani 1 1 d . . . C22 C 0.5926(3) 0.88271(17) 0.15384(18) 0.0207(6) Uani 1 1 d . . . H22 H 0.6698 0.9160 0.1624 0.025 Uiso 1 1 calc R . . C23 C 0.4811(3) 0.91725(19) 0.17140(19) 0.0242(6) Uani 1 1 d . . . H23 H 0.4811 0.9751 0.1916 0.029 Uiso 1 1 calc R . . C24 C 0.3686(3) 0.86815(19) 0.15977(19) 0.0248(6) Uani 1 1 d . . . H24 H 0.2913 0.8917 0.1715 0.030 Uiso 1 1 calc R . . C25 C 0.3726(3) 0.78424(17) 0.13070(18) 0.0215(6) Uani 1 1 d . . . H25 H 0.2966 0.7497 0.1235 0.026 Uiso 1 1 calc R . . C26 C 0.7977(2) 0.77587(17) 0.08227(16) 0.0159(5) Uani 1 1 d . . . C27 C 0.8229(3) 0.86109(18) 0.05758(18) 0.0223(6) Uani 1 1 d . . . H27 H 0.7633 0.9068 0.0597 0.027 Uiso 1 1 calc R . . C28 C 0.9357(3) 0.8767(2) 0.0303(2) 0.0285(7) Uani 1 1 d . . . H28 H 0.9537 0.9336 0.0134 0.034 Uiso 1 1 calc R . . C29 C 1.0224(3) 0.81079(19) 0.02749(18) 0.0253(6) Uani 1 1 d . . . H29 H 1.1001 0.8208 0.0086 0.030 Uiso 1 1 calc R . . C30 C 0.9915(3) 0.72918(19) 0.05332(17) 0.0224(6) Uani 1 1 d . . . H30 H 1.0512 0.6833 0.0520 0.027 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 La1 0.01305(9) 0.01117(10) 0.01068(10) -0.00084(5) 0.00244(7) -0.00175(5) N1 0.0117(10) 0.0133(10) 0.0158(12) 0.0025(8) 0.0014(9) -0.0014(8) N2 0.0169(11) 0.0159(11) 0.0124(11) 0.0009(9) 0.0031(9) -0.0019(9) N3 0.0124(10) 0.0170(11) 0.0182(12) 0.0013(9) 0.0024(9) -0.0007(8) N4 0.0158(11) 0.0174(11) 0.0116(12) -0.0013(9) 0.0028(9) -0.0020(9) N5 0.0164(11) 0.0142(11) 0.0165(12) -0.0014(9) 0.0027(9) -0.0028(9) N6 0.0272(13) 0.0267(12) 0.0131(12) -0.0018(10) 0.0010(10) 0.0021(11) N7 0.0157(10) 0.0162(12) 0.0213(12) -0.0001(9) 0.0054(10) -0.0045(9) N8 0.0169(11) 0.0134(11) 0.0213(13) 0.0000(9) 0.0036(10) -0.0022(8) N9 0.0174(11) 0.0197(12) 0.0149(11) -0.0034(9) 0.0030(9) -0.0021(9) C1 0.0136(12) 0.0087(11) 0.0141(13) 0.0005(10) 0.0019(10) 0.0013(9) C2 0.0163(12) 0.0164(13) 0.0173(14) 0.0015(11) -0.0012(11) -0.0011(11) C3 0.0248(14) 0.0240(15) 0.0128(13) 0.0057(11) 0.0023(11) 0.0054(11) C4 0.0196(13) 0.0189(14) 0.0203(14) 0.0020(11) 0.0090(11) -0.0021(11) C5 0.0124(11) 0.0206(14) 0.0213(14) -0.0013(11) 0.0055(11) -0.0026(10) C6 0.0123(12) 0.0186(13) 0.0111(13) -0.0029(10) 0.0035(10) -0.0015(10) C7 0.0199(13) 0.0135(13) 0.0241(15) 0.0015(11) 0.0053(12) 0.0008(10) C8 0.0192(13) 0.0214(14) 0.0243(16) -0.0001(12) 0.0048(12) 0.0065(11) C9 0.0118(12) 0.0251(15) 0.0284(17) -0.0081(12) 0.0045(12) 0.0025(10) C10 0.0167(13) 0.0203(14) 0.0256(16) -0.0014(12) 0.0090(12) -0.0045(11) C11 0.0195(13) 0.0098(11) 0.0145(13) 0.0010(10) 0.0043(11) -0.0012(10) C12 0.0247(15) 0.0245(14) 0.0142(15) -0.0023(11) 0.0074(12) -0.0006(12) C13 0.0259(15) 0.0249(14) 0.0241(16) -0.0047(13) 0.0142(13) -0.0022(12) C14 0.0199(14) 0.0248(15) 0.0303(17) -0.0037(13) 0.0080(13) -0.0037(12) C15 0.0185(13) 0.0160(13) 0.0214(15) -0.0024(11) 0.0026(11) -0.0030(11) C16 0.0188(13) 0.0114(13) 0.0160(15) -0.0038(10) 0.0001(11) 0.0025(9) C17 0.0206(13) 0.0159(13) 0.0215(15) 0.0003(12) 0.0031(12) -0.0001(11) C18 0.0196(13) 0.0157(14) 0.0381(19) -0.0037(13) -0.0021(13) 0.0007(11) C19 0.0293(17) 0.0303(17) 0.025(2) -0.0110(12) -0.0077(15) 0.0089(13) C20 0.0363(18) 0.0350(17) 0.0130(15) -0.0032(12) -0.0033(14) 0.0111(14) C21 0.0187(13) 0.0138(13) 0.0158(13) 0.0014(11) 0.0026(10) -0.0034(10) C22 0.0278(15) 0.0173(13) 0.0180(15) -0.0019(11) 0.0065(13) -0.0080(11) C23 0.0365(17) 0.0171(14) 0.0216(16) -0.0011(12) 0.0119(14) -0.0004(12) C24 0.0290(15) 0.0215(15) 0.0277(17) 0.0048(13) 0.0148(14) 0.0059(12) C25 0.0178(13) 0.0189(14) 0.0295(16) 0.0037(12) 0.0083(12) 0.0008(11) C26 0.0149(12) 0.0190(13) 0.0133(13) -0.0038(10) 0.0012(10) -0.0049(10) C27 0.0271(15) 0.0180(14) 0.0237(16) -0.0002(12) 0.0098(13) -0.0042(12) C28 0.0341(17) 0.0250(15) 0.0289(18) -0.0013(13) 0.0120(15) -0.0138(14) C29 0.0218(14) 0.0352(17) 0.0204(15) -0.0015(13) 0.0078(12) -0.0082(12) C30 0.0190(13) 0.0318(16) 0.0166(14) -0.0061(12) 0.0041(11) -0.0006(12) _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 La1 N7 2.483(2) . ? La1 N4 2.532(2) . ? La1 N5 2.621(2) . ? La1 N3 2.633(2) . ? La1 N2 2.636(2) 3_665 ? La1 N1 2.668(2) 3_665 ? La1 N8 2.672(2) . ? La1 N1 2.758(2) . ? La1 C11 3.074(3) . ? La1 C21 3.097(3) . ? La1 La1 4.2015(8) 3_665 ? N1 C6 1.389(3) . ? N1 C1 1.400(3) . ? N1 La1 2.668(2) 3_665 ? N2 C1 1.349(3) . ? N2 C5 1.350(3) . ? N2 La1 2.636(2) 3_665 ? N3 C10 1.353(3) . ? N3 C6 1.354(3) . ? N4 C11 1.370(3) . ? N4 C16 1.373(4) . ? N5 C15 1.343(3) . ? N5 C11 1.368(3) . ? N6 C20 1.341(4) . ? N6 C16 1.357(4) . ? N7 C21 1.361(3) . ? N7 C26 1.366(3) . ? N8 C25 1.339(3) . ? N8 C21 1.358(3) . ? N9 C30 1.340(3) . ? N9 C26 1.361(3) . ? C1 C2 1.399(4) . ? C2 C3 1.371(4) . ? C3 C4 1.393(4) . ? C4 C5 1.367(4) . ? C6 C7 1.404(4) . ? C7 C8 1.377(4) . ? C8 C9 1.400(4) . ? C9 C10 1.370(4) . ? C11 C12 1.417(4) . ? C12 C13 1.374(4) . ? C13 C14 1.387(4) . ? C14 C15 1.378(4) . ? C16 C17 1.422(4) . ? C17 C18 1.376(4) . ? C18 C19 1.391(4) . ? C19 C20 1.366(5) . ? C21 C22 1.415(4) . ? C22 C23 1.378(4) . ? C23 C24 1.390(4) . ? C24 C25 1.380(4) . ? C26 C27 1.413(4) . ? C27 C28 1.381(4) . ? C28 C29 1.374(4) . ? C29 C30 1.385(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 La1 N4 86.87(7) . . ? N7 La1 N5 114.91(7) . . ? N4 La1 N5 51.98(7) . . ? N7 La1 N3 108.96(7) . . ? N4 La1 N3 91.01(7) . . ? N5 La1 N3 118.09(7) . . ? N7 La1 N2 79.69(7) . 3_665 ? N4 La1 N2 164.54(7) . 3_665 ? N5 La1 N2 141.60(7) . 3_665 ? N3 La1 N2 86.23(7) . 3_665 ? N7 La1 N1 117.61(7) . 3_665 ? N4 La1 N1 143.91(7) . 3_665 ? N5 La1 N1 92.35(7) . 3_665 ? N3 La1 N1 103.89(7) . 3_665 ? N2 La1 N1 51.15(6) 3_665 3_665 ? N7 La1 N8 51.15(7) . . ? N4 La1 N8 79.61(7) . . ? N5 La1 N8 71.27(7) . . ? N3 La1 N8 158.00(7) . . ? N2 La1 N8 97.51(7) 3_665 . ? N1 La1 N8 95.14(7) 3_665 . ? N7 La1 N1 158.09(7) . . ? N4 La1 N1 86.80(7) . . ? N5 La1 N1 76.75(6) . . ? N3 La1 N1 50.24(6) . . ? N2 La1 N1 102.89(6) 3_665 . ? N1 La1 N1 78.53(7) 3_665 . ? N8 La1 N1 147.13(6) . . ? N7 La1 C11 98.93(7) . . ? N4 La1 C11 26.08(7) . . ? N5 La1 C11 26.30(7) . . ? N3 La1 C11 108.51(7) . . ? N2 La1 C11 164.63(7) 3_665 . ? N1 La1 C11 118.64(7) 3_665 . ? N8 La1 C11 70.54(7) . . ? N1 La1 C11 84.17(6) . . ? N7 La1 C21 25.29(7) . . ? N4 La1 C21 81.36(7) . . ? N5 La1 C21 92.83(7) . . ? N3 La1 C21 133.34(7) . . ? N2 La1 C21 89.49(7) 3_665 . ? N1 La1 C21 109.08(7) 3_665 . ? N8 La1 C21 25.90(6) . . ? N1 La1 C21 167.55(6) . . ? C11 La1 C21 83.51(7) . . ? N7 La1 La1 154.61(5) . 3_665 ? N4 La1 La1 118.46(5) . 3_665 ? N5 La1 La1 82.86(5) . 3_665 ? N3 La1 La1 74.49(5) . 3_665 ? N2 La1 La1 75.41(5) 3_665 3_665 ? N1 La1 La1 40.04(5) 3_665 3_665 ? N8 La1 La1 127.47(5) . 3_665 ? N1 La1 La1 38.49(4) . 3_665 ? C11 La1 La1 103.75(5) . 3_665 ? C21 La1 La1 148.06(5) . 3_665 ? C6 N1 C1 118.0(2) . . ? C6 N1 La1 129.65(17) . 3_665 ? C1 N1 La1 96.26(15) . 3_665 ? C6 N1 La1 92.74(15) . . ? C1 N1 La1 119.50(16) . . ? La1 N1 La1 101.47(7) 3_665 . ? C1 N2 C5 118.4(2) . . ? C1 N2 La1 99.11(16) . 3_665 ? C5 N2 La1 142.31(18) . 3_665 ? C10 N3 C6 118.8(2) . . ? C10 N3 La1 138.30(18) . . ? C6 N3 La1 99.19(15) . . ? C11 N4 C16 124.8(2) . . ? C11 N4 La1 99.61(17) . . ? C16 N4 La1 134.49(18) . . ? C15 N5 C11 119.6(2) . . ? C15 N5 La1 141.92(19) . . ? C11 N5 La1 95.64(15) . . ? C20 N6 C16 117.5(3) . . ? C21 N7 C26 127.7(2) . . ? C21 N7 La1 103.49(15) . . ? C26 N7 La1 126.18(17) . . ? C25 N8 C21 120.3(2) . . ? C25 N8 La1 144.17(17) . . ? C21 N8 La1 94.84(15) . . ? C30 N9 C26 117.9(2) . . ? N2 C1 C2 121.3(2) . . ? N2 C1 N1 112.8(2) . . ? C2 C1 N1 125.6(2) . . ? C3 C2 C1 119.0(2) . . ? C2 C3 C4 119.8(3) . . ? C5 C4 C3 118.2(2) . . ? N2 C5 C4 123.2(2) . . ? N3 C6 N1 113.3(2) . . ? N3 C6 C7 121.0(2) . . ? N1 C6 C7 125.7(2) . . ? C8 C7 C6 119.0(3) . . ? C7 C8 C9 120.0(3) . . ? C10 C9 C8 117.9(3) . . ? N3 C10 C9 123.2(3) . . ? N5 C11 N4 111.2(2) . . ? N5 C11 C12 119.5(2) . . ? N4 C11 C12 129.2(3) . . ? N5 C11 La1 58.07(13) . . ? N4 C11 La1 54.32(14) . . ? C12 C11 La1 167.64(19) . . ? C13 C12 C11 119.0(3) . . ? C12 C13 C14 121.1(3) . . ? C15 C14 C13 117.4(3) . . ? N5 C15 C14 123.3(3) . . ? N6 C16 N4 122.4(3) . . ? N6 C16 C17 120.5(3) . . ? N4 C16 C17 117.1(3) . . ? C18 C17 C16 119.5(3) . . ? C17 C18 C19 119.5(3) . . ? C20 C19 C18 117.4(3) . . ? N6 C20 C19 125.5(3) . . ? N8 C21 N7 110.3(2) . . ? N8 C21 C22 119.9(2) . . ? N7 C21 C22 129.7(2) . . ? N8 C21 La1 59.26(13) . . ? N7 C21 La1 51.22(12) . . ? C22 C21 La1 173.28(19) . . ? C23 C22 C21 118.7(3) . . ? C22 C23 C24 120.5(3) . . ? C25 C24 C23 118.0(3) . . ? N8 C25 C24 122.5(2) . . ? N9 C26 N7 112.6(2) . . ? N9 C26 C27 120.8(2) . . ? N7 C26 C27 126.5(2) . . ? C28 C27 C26 118.8(3) . . ? C29 C28 C27 120.8(3) . . ? C28 C29 C30 117.1(3) . . ? N9 C30 C29 124.7(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.690 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.126 # Attachment 'B600868B_2.cif' data_c:\mydocu~1\stuart\phd\crysta~1\airsen~1\ni2la8hq\laniabs _database_code_depnum_ccdc_archive 'CCDC 298868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(mu-(O)-8-quinolinolato)(8-quinolinolato-kappa:N,O(La) dinickel(II)lanthanum(III) (NiLaNi) ; _chemical_name_common Ni2La(8OQ)7 _chemical_melting_point >360 _chemical_formula_moiety ? _chemical_formula_sum 'C63 H36 La N7 Ni2 O7' _chemical_formula_weight 1259.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.499(3) _cell_length_b 19.150(4) _cell_length_c 17.485(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.67(3) _cell_angle_gamma 90.00 _cell_volume 5189.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 21168 _cell_measurement_theta_min 3.57 _cell_measurement_theta_max 25.00 _exptl_crystal_description rectangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8570 _exptl_absorpt_correction_T_max 0.9105 _exptl_absorpt_process_details SORTAV _exptl_special_details ; SORTAV (R. H. Blessing 1997) ; _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 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21168 _diffrn_reflns_av_R_equivalents 0.1419 _diffrn_reflns_av_sigmaI/netI 0.1543 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4543 _reflns_number_gt 2281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0400P)^2^+17.4551P] 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 4543 _refine_ls_number_parameters 349 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1692 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 La1 La 0.5000 0.33000(4) 0.2500 0.0431(3) Uani 1 2 d S . . O1A O 0.3866(3) 0.2804(2) 0.3332(2) 0.0358(12) Uani 1 1 d . . . O1B O 0.4244(3) 0.2315(3) 0.1844(2) 0.0373(13) Uani 1 1 d . . . O1C O 0.3466(3) 0.3575(3) 0.2020(2) 0.0440(14) Uani 1 1 d . . . O1D O 0.5170(8) 0.4294(8) 0.1619(8) 0.057(4) Uani 0.50 1 d P . . N1A N 0.2150(4) 0.2877(3) 0.3123(3) 0.0386(16) Uani 1 1 d . . . N1B N 0.3026(4) 0.1496(4) 0.2421(3) 0.0466(18) Uani 1 1 d . . . N1C N 0.2358(4) 0.2641(4) 0.1395(3) 0.0435(17) Uani 1 1 d . . . N1D N 0.4763(13) 0.4569(12) 0.3103(10) 0.047(6) Uiso 0.50 1 d P . . C1A C 0.1313(5) 0.2911(4) 0.3022(4) 0.041(2) Uani 1 1 d . . . H1A H 0.1082 0.2785 0.2536 0.049 Uiso 1 1 calc R . . C1B C 0.2395(5) 0.1088(5) 0.2649(4) 0.054(2) Uani 1 1 d . . . H1B H 0.1926 0.1294 0.2912 0.065 Uiso 1 1 calc R . . C1C C 0.1846(5) 0.2163(5) 0.1093(4) 0.049(2) Uani 1 1 d . . . H1C H 0.1816 0.1717 0.1330 0.059 Uiso 1 1 calc R . . C1D C 0.4611(12) 0.4741(11) 0.3843(11) 0.069(5) Uiso 0.50 1 d P . . Ni2 Ni 0.31089(6) 0.25779(5) 0.23678(5) 0.0399(3) Uani 1 1 d . . . C2A C 0.0737(5) 0.3122(4) 0.3590(4) 0.046(2) Uani 1 1 d . . . H2A H 0.0133 0.3124 0.3492 0.055 Uiso 1 1 calc R . . C2B C 0.2380(6) 0.0368(6) 0.2525(5) 0.064(3) Uani 1 1 d . . . H2B H 0.1905 0.0100 0.2697 0.077 Uiso 1 1 calc R . . C2C C 0.1343(5) 0.2290(6) 0.0432(5) 0.062(3) Uani 1 1 d . . . H2C H 0.0977 0.1936 0.0229 0.074 Uiso 1 1 calc R . . C2D C 0.4673(11) 0.5409(9) 0.4150(10) 0.055(5) Uiso 0.50 1 d P . . C3A C 0.1055(5) 0.3325(4) 0.4282(4) 0.0419(19) Uani 1 1 d . . . H3A H 0.0673 0.3477 0.4669 0.050 Uiso 1 1 calc R . . C3B C 0.3043(6) 0.0047(5) 0.2157(5) 0.059(3) Uani 1 1 d . . . H3B H 0.3031 -0.0443 0.2069 0.071 Uiso 1 1 calc R . . C3C C 0.1388(6) 0.2915(6) 0.0095(4) 0.062(3) Uani 1 1 d . . . H3C H 0.1045 0.3005 -0.0348 0.075 Uiso 1 1 calc R . . C4A C 0.1947(4) 0.3310(4) 0.4425(4) 0.0329(17) Uani 1 1 d . . . C4B C 0.3751(6) 0.0456(5) 0.1907(4) 0.047(2) Uani 1 1 d . . . C4C C 0.1931(6) 0.3442(6) 0.0381(4) 0.054(2) Uani 1 1 d . . . C4D C 0.4928(12) 0.5775(8) 0.2914(7) 0.062(5) Uiso 0.50 1 d PD . . C5A C 0.2340(5) 0.3513(4) 0.5120(4) 0.044(2) Uiso 1 1 d . . . H5A H 0.2000 0.3680 0.5531 0.053 Uiso 1 1 calc R . . C5B C 0.4480(6) 0.0179(5) 0.1527(5) 0.058(2) Uani 1 1 d . . . H5B H 0.4534 -0.0310 0.1446 0.070 Uiso 1 1 calc R . . C5C C 0.2071(7) 0.4096(6) 0.0043(5) 0.073(3) Uani 1 1 d . . . H5C H 0.1729 0.4234 -0.0386 0.087 Uiso 1 1 calc R . . C5D C 0.5000 0.6382(8) 0.2500 0.105(5) Uiso 1 2 d SD . . C6A C 0.3213(5) 0.3467(4) 0.5196(4) 0.049(2) Uani 1 1 d . . . H6A H 0.3473 0.3596 0.5670 0.058 Uiso 1 1 calc R . . C6B C 0.5098(6) 0.0625(5) 0.1281(4) 0.052(2) Uani 1 1 d . . . H6B H 0.5586 0.0438 0.1029 0.062 Uiso 1 1 calc R . . C6C C 0.2684(7) 0.4532(5) 0.0320(5) 0.071(3) Uani 1 1 d D . . H6C H 0.2784 0.4962 0.0065 0.085 Uiso 1 1 calc R . . C6D C 0.5111(12) 0.6211(8) 0.1706(6) 0.065(6) Uiso 0.50 1 d PD . . C7A C 0.3746(5) 0.3237(4) 0.4603(4) 0.0384(19) Uani 1 1 d . . . H7A H 0.4353 0.3217 0.4680 0.046 Uiso 1 1 calc R . . C7B C 0.5046(5) 0.1346(5) 0.1381(4) 0.041(2) Uani 1 1 d . . . H7B H 0.5488 0.1640 0.1192 0.049 Uiso 1 1 calc R . . C7C C 0.3183(5) 0.4367(4) 0.0978(4) 0.057(2) Uani 1 1 d D . . H7C H 0.3614 0.4682 0.1153 0.068 Uiso 1 1 calc R . . C7D C 0.5218(11) 0.5540(9) 0.1343(9) 0.056(5) Uiso 0.50 1 d PD . . C8A C 0.3393(5) 0.3043(4) 0.3910(4) 0.0340(19) Uani 1 1 d . . . C8B C 0.4347(5) 0.1633(5) 0.1758(4) 0.040(2) Uani 1 1 d . . . C8C C 0.3044(5) 0.3745(4) 0.1371(5) 0.048(2) Uiso 1 1 d D . . C8D C 0.5113(12) 0.4964(8) 0.1847(8) 0.058(6) Uiso 0.50 1 d PD . . C9A C 0.2480(5) 0.3084(4) 0.3810(4) 0.0353(19) Uani 1 1 d . . . C9B C 0.3691(5) 0.1184(5) 0.2034(4) 0.038(2) Uani 1 1 d . . . C9C C 0.2439(5) 0.3282(5) 0.1054(4) 0.043(2) Uani 1 1 d D . . C9D C 0.4961(16) 0.5103(6) 0.2639(8) 0.042(4) Uiso 0.50 1 d PD . . C3D C 0.4803(10) 0.6004(9) 0.3680(9) 0.038(4) Uiso 0.50 1 d P . . 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 La1 0.0304(4) 0.0533(5) 0.0457(4) 0.000 0.0113(3) 0.000 O1A 0.025(3) 0.057(3) 0.026(3) -0.003(2) 0.012(2) 0.006(3) O1B 0.028(3) 0.053(4) 0.031(3) 0.001(3) 0.006(2) 0.000(3) O1C 0.036(3) 0.065(4) 0.031(3) -0.003(3) 0.004(2) 0.011(3) O1D 0.036(8) 0.086(12) 0.050(9) 0.013(9) 0.014(7) -0.003(8) N1A 0.025(4) 0.060(5) 0.030(4) 0.005(3) 0.004(3) -0.002(3) N1B 0.028(4) 0.079(6) 0.032(4) 0.007(3) 0.004(3) -0.004(4) N1C 0.030(4) 0.072(5) 0.029(4) -0.005(4) 0.009(3) 0.000(4) C1A 0.027(5) 0.055(6) 0.039(5) -0.003(4) -0.004(4) 0.002(4) C1B 0.037(6) 0.080(8) 0.044(5) 0.018(5) 0.002(4) 0.001(6) C1C 0.032(5) 0.090(7) 0.026(4) -0.001(5) 0.004(4) -0.004(5) Ni2 0.0276(6) 0.0653(8) 0.0269(5) 0.0004(5) 0.0044(4) 0.0015(5) C2A 0.023(5) 0.059(6) 0.056(5) 0.006(4) 0.005(4) 0.002(4) C2B 0.047(7) 0.072(8) 0.073(7) 0.033(6) 0.000(5) -0.009(6) C2C 0.041(6) 0.109(9) 0.036(5) -0.002(6) 0.004(4) -0.004(6) C3A 0.032(5) 0.048(5) 0.046(5) -0.007(4) 0.007(4) -0.001(4) C3B 0.053(7) 0.057(6) 0.067(6) 0.015(5) -0.013(5) -0.006(6) C3C 0.045(6) 0.114(9) 0.029(5) -0.002(6) 0.001(4) 0.022(6) C4A 0.027(4) 0.042(5) 0.030(4) 0.005(4) 0.005(3) -0.007(4) C4B 0.041(6) 0.055(7) 0.044(5) 0.007(5) -0.015(4) -0.016(5) C4C 0.055(6) 0.078(8) 0.029(5) -0.001(5) 0.007(4) 0.021(6) C5B 0.065(7) 0.053(6) 0.056(6) -0.003(5) -0.011(5) 0.006(6) C5C 0.075(8) 0.094(9) 0.050(6) 0.003(7) -0.004(6) 0.036(7) C6A 0.047(6) 0.071(7) 0.028(4) -0.015(4) 0.007(4) -0.010(5) C6B 0.055(7) 0.061(7) 0.039(5) -0.015(5) -0.005(4) 0.011(5) C6C 0.090(9) 0.072(8) 0.051(6) 0.025(6) 0.012(6) 0.022(7) C7A 0.030(4) 0.052(5) 0.033(4) -0.005(4) 0.000(3) -0.006(4) C7B 0.026(5) 0.065(6) 0.032(4) -0.009(4) 0.002(4) 0.002(4) C7C 0.066(7) 0.057(6) 0.047(5) 0.003(5) 0.011(5) 0.009(5) C8A 0.037(5) 0.039(5) 0.026(4) 0.001(4) 0.006(4) 0.000(4) C8B 0.041(5) 0.051(6) 0.027(4) -0.001(4) 0.002(4) 0.001(5) C9A 0.023(5) 0.054(6) 0.029(4) 0.007(4) 0.000(3) -0.001(4) C9B 0.032(5) 0.059(7) 0.024(4) 0.001(4) -0.003(4) -0.017(5) C9C 0.036(5) 0.065(6) 0.028(4) 0.002(5) 0.014(4) 0.006(5) _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 La1 O1D 2.466(13) 2_655 ? La1 O1D 2.466(13) . ? La1 O1A 2.483(4) . ? La1 O1A 2.483(4) 2_655 ? La1 O1B 2.492(5) . ? La1 O1B 2.492(5) 2_655 ? La1 O1C 2.567(5) 2_655 ? La1 O1C 2.567(5) . ? La1 N1D 2.68(2) . ? La1 N1D 2.68(2) 2_655 ? O1A C8A 1.336(7) . ? O1A Ni2 2.088(4) . ? O1B C8B 1.325(8) . ? O1B Ni2 2.056(5) . ? O1C C8C 1.343(8) . ? O1C Ni2 2.080(5) . ? O1D N1D 0.72(2) 2_655 ? O1D C1D 1.23(2) 2_655 ? O1D C8D 1.35(2) . ? N1A C1A 1.310(8) . ? N1A C9A 1.359(8) . ? N1A Ni2 2.079(6) . ? N1B C1B 1.318(9) . ? N1B C9B 1.375(9) . ? N1B Ni2 2.078(7) . ? N1C C1C 1.318(9) . ? N1C C9C 1.369(9) . ? N1C Ni2 2.054(6) . ? N1D O1D 0.72(2) 2_655 ? N1D C8D 0.79(2) 2_655 ? N1D C9D 1.34(2) . ? N1D C1D 1.36(3) . ? N1D C9D 1.71(2) 2_655 ? C1A C2A 1.403(9) . ? C1B C2B 1.396(11) . ? C1C C2C 1.408(10) . ? C1D O1D 1.23(2) 2_655 ? C1D C8D 1.35(2) 2_655 ? C1D C2D 1.39(2) . ? C1D C7D 1.59(2) 2_655 ? C2A C3A 1.356(9) . ? C2B C3B 1.365(11) . ? C2C C3C 1.337(11) . ? C2D C7D 0.914(18) 2_655 ? C2D C3D 1.42(2) . ? C2D C8D 1.97(2) 2_655 ? C3A C4A 1.403(9) . ? C3B C4B 1.421(11) . ? C3C C4C 1.401(12) . ? C4A C5A 1.409(9) . ? C4A C9A 1.430(9) . ? C4B C9B 1.416(10) . ? C4B C5B 1.420(11) . ? C4C C5C 1.404(12) . ? C4C C9C 1.442(10) . ? C4D C6D 1.071(19) 2_655 ? C4D C9D 1.374(18) . ? C4D C5D 1.374(9) . ? C4D C7D 1.397(19) 2_655 ? C4D C3D 1.43(2) . ? C4D C4D 1.47(3) 2_655 ? C4D C8D 1.61(2) 2_655 ? C4D C9D 1.620(18) 2_655 ? C5A C6A 1.361(10) . ? C5B C6B 1.357(11) . ? C5C C6C 1.350(12) . ? C5D C4D 1.374(9) 2_655 ? C5D C6D 1.439(11) 2_655 ? C5D C6D 1.439(11) . ? C6A C7A 1.404(9) . ? C6B C7B 1.394(10) . ? C6C C7C 1.414(8) . ? C6D C3D 0.796(17) 2_655 ? C6D C4D 1.071(19) 2_655 ? C6D C7D 1.445(15) . ? C7A C8A 1.374(9) . ? C7B C8B 1.388(9) . ? C7C C8C 1.392(7) . ? C7D C3D 0.890(19) 2_655 ? C7D C2D 0.914(18) 2_655 ? C7D C4D 1.397(19) 2_655 ? C7D C8D 1.423(9) . ? C7D C1D 1.59(2) 2_655 ? C7D C9D 1.99(2) 2_655 ? C8A C9A 1.427(9) . ? C8B C9B 1.421(10) . ? C8C C9C 1.401(10) . ? C8D N1D 0.79(2) 2_655 ? C8D C9D 0.94(2) 2_655 ? C8D C1D 1.35(2) 2_655 ? C8D C9D 1.433(18) . ? C8D C4D 1.61(2) 2_655 ? C8D C2D 1.97(2) 2_655 ? C9D C9D 0.50(3) 2_655 ? C9D C8D 0.94(2) 2_655 ? C9D C4D 1.620(18) 2_655 ? C9D N1D 1.71(2) 2_655 ? C9D C7D 1.99(2) 2_655 ? C3D C6D 0.796(17) 2_655 ? C3D C7D 0.890(19) 2_655 ? 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 O1D La1 O1D 78.9(7) 2_655 . ? O1D La1 O1A 81.2(3) 2_655 . ? O1D La1 O1A 138.0(3) . . ? O1D La1 O1A 138.0(3) 2_655 2_655 ? O1D La1 O1A 81.2(3) . 2_655 ? O1A La1 O1A 135.0(2) . 2_655 ? O1D La1 O1B 145.0(3) 2_655 . ? O1D La1 O1B 110.5(4) . . ? O1A La1 O1B 69.41(14) . . ? O1A La1 O1B 76.86(15) 2_655 . ? O1D La1 O1B 110.5(4) 2_655 2_655 ? O1D La1 O1B 145.0(3) . 2_655 ? O1A La1 O1B 76.86(15) . 2_655 ? O1A La1 O1B 69.41(14) 2_655 2_655 ? O1B La1 O1B 81.7(2) . 2_655 ? O1D La1 O1C 75.1(3) 2_655 2_655 ? O1D La1 O1C 86.6(3) . 2_655 ? O1A La1 O1C 123.08(14) . 2_655 ? O1A La1 O1C 67.10(14) 2_655 2_655 ? O1B La1 O1C 137.23(16) . 2_655 ? O1B La1 O1C 64.91(16) 2_655 2_655 ? O1D La1 O1C 86.6(3) 2_655 . ? O1D La1 O1C 75.1(3) . . ? O1A La1 O1C 67.10(14) . . ? O1A La1 O1C 123.08(14) 2_655 . ? O1B La1 O1C 64.91(16) . . ? O1B La1 O1C 137.23(16) 2_655 . ? O1C La1 O1C 156.4(2) 2_655 . ? O1D La1 N1D 15.5(4) 2_655 . ? O1D La1 N1D 64.0(6) . . ? O1A La1 N1D 90.9(4) . . ? O1A La1 N1D 132.8(4) 2_655 . ? O1B La1 N1D 143.4(4) . . ? O1B La1 N1D 124.9(4) 2_655 . ? O1C La1 N1D 79.4(4) 2_655 . ? O1C La1 N1D 79.2(4) . . ? O1D La1 N1D 64.0(6) 2_655 2_655 ? O1D La1 N1D 15.5(4) . 2_655 ? O1A La1 N1D 132.8(4) . 2_655 ? O1A La1 N1D 90.9(4) 2_655 2_655 ? O1B La1 N1D 124.9(4) . 2_655 ? O1B La1 N1D 143.4(4) 2_655 2_655 ? O1C La1 N1D 79.2(4) 2_655 2_655 ? O1C La1 N1D 79.4(4) . 2_655 ? N1D La1 N1D 49.5(8) . 2_655 ? C8A O1A Ni2 111.9(4) . . ? C8A O1A La1 135.3(4) . . ? Ni2 O1A La1 90.08(15) . . ? C8B O1B Ni2 113.3(4) . . ? C8B O1B La1 137.8(4) . . ? Ni2 O1B La1 90.57(19) . . ? C8C O1C Ni2 110.0(4) . . ? C8C O1C La1 140.0(4) . . ? Ni2 O1C La1 87.98(16) . . ? N1D O1D C1D 84(3) 2_655 2_655 ? N1D O1D C8D 28(2) 2_655 . ? C1D O1D C8D 63.3(12) 2_655 . ? N1D O1D La1 99(3) 2_655 . ? C1D O1D La1 169.1(13) 2_655 . ? C8D O1D La1 122.8(11) . . ? C1A N1A C9A 117.8(6) . . ? C1A N1A Ni2 130.0(5) . . ? C9A N1A Ni2 112.2(5) . . ? C1B N1B C9B 117.1(7) . . ? C1B N1B Ni2 130.6(6) . . ? C9B N1B Ni2 111.3(5) . . ? C1C N1C C9C 120.4(7) . . ? C1C N1C Ni2 128.5(6) . . ? C9C N1C Ni2 111.0(5) . . ? O1D N1D C8D 126(4) 2_655 2_655 ? O1D N1D C9D 158(3) 2_655 . ? C8D N1D C9D 43.6(17) 2_655 . ? O1D N1D C1D 64(2) 2_655 . ? C8D N1D C1D 73(2) 2_655 . ? C9D N1D C1D 116(2) . . ? O1D N1D C9D 156(3) 2_655 2_655 ? C8D N1D C9D 56.3(17) 2_655 2_655 ? C9D N1D C9D 13.0(8) . 2_655 ? C1D N1D C9D 128.7(18) . 2_655 ? O1D N1D La1 66(2) 2_655 . ? C8D N1D La1 152(2) 2_655 . ? C9D N1D La1 114.9(12) . . ? C1D N1D La1 128.4(15) . . ? C9D N1D La1 102.0(10) 2_655 . ? N1A C1A C2A 123.9(7) . . ? N1B C1B C2B 123.3(9) . . ? N1C C1C C2C 122.3(8) . . ? O1D C1D C8D 62.6(13) 2_655 2_655 ? O1D C1D N1D 31.9(11) 2_655 . ? C8D C1D N1D 33.7(10) 2_655 . ? O1D C1D C2D 151.2(19) 2_655 . ? C8D C1D C2D 91.8(15) 2_655 . ? N1D C1D C2D 125.3(18) . . ? O1D C1D C7D 119.3(16) 2_655 2_655 ? C8D C1D C7D 57.2(9) 2_655 2_655 ? N1D C1D C7D 90.4(14) . 2_655 ? C2D C1D C7D 35.0(9) . 2_655 ? N1C Ni2 O1B 97.2(2) . . ? N1C Ni2 N1B 93.5(3) . . ? O1B Ni2 N1B 80.2(2) . . ? N1C Ni2 N1A 96.2(2) . . ? O1B Ni2 N1A 166.4(2) . . ? N1B Ni2 N1A 101.6(2) . . ? N1C Ni2 O1C 81.6(2) . . ? O1B Ni2 O1C 82.1(2) . . ? N1B Ni2 O1C 160.9(2) . . ? N1A Ni2 O1C 97.3(2) . . ? N1C Ni2 O1A 164.6(3) . . ? O1B Ni2 O1A 86.23(17) . . ? N1B Ni2 O1A 101.8(2) . . ? N1A Ni2 O1A 80.2(2) . . ? O1C Ni2 O1A 84.09(18) . . ? C3A C2A C1A 119.1(7) . . ? C3B C2B C1B 120.5(9) . . ? C3C C2C C1C 119.0(9) . . ? C7D C2D C1D 84.4(18) 2_655 . ? C7D C2D C3D 37.5(14) 2_655 . ? C1D C2D C3D 121.7(16) . . ? C7D C2D C8D 41.5(13) 2_655 2_655 ? C1D C2D C8D 43.4(10) . 2_655 ? C3D C2D C8D 79.0(11) . 2_655 ? C2A C3A C4A 120.0(7) . . ? C2B C3B C4B 119.0(9) . . ? C2C C3C C4C 121.4(8) . . ? C3A C4A C5A 124.3(7) . . ? C3A C4A C9A 116.7(6) . . ? C5A C4A C9A 119.0(6) . . ? C9B C4B C5B 119.7(8) . . ? C9B C4B C3B 116.2(8) . . ? C5B C4B C3B 124.0(9) . . ? C3C C4C C5C 125.9(9) . . ? C3C C4C C9C 117.3(9) . . ? C5C C4C C9C 116.6(9) . . ? C6D C4D C9D 161.9(15) 2_655 . ? C6D C4D C5D 70.9(9) 2_655 . ? C9D C4D C5D 127.2(13) . . ? C6D C4D C7D 70.2(10) 2_655 2_655 ? C9D C4D C7D 91.8(12) . 2_655 ? C5D C4D C7D 141.0(13) . 2_655 ? C6D C4D C3D 33.5(9) 2_655 . ? C9D C4D C3D 128.5(13) . . ? C5D C4D C3D 104.3(12) . . ? C7D C4D C3D 36.7(8) 2_655 . ? C6D C4D C4D 128.6(9) 2_655 2_655 ? C9D C4D C4D 69.5(8) . 2_655 ? C5D C4D C4D 57.8(7) . 2_655 ? C7D C4D C4D 161.2(9) 2_655 2_655 ? C3D C4D C4D 162.1(9) . 2_655 ? C6D C4D C8D 126.1(12) 2_655 2_655 ? C9D C4D C8D 35.8(9) . 2_655 ? C5D C4D C8D 163.1(12) . 2_655 ? C7D C4D C8D 55.9(7) 2_655 2_655 ? C3D C4D C8D 92.6(10) . 2_655 ? C4D C4D C8D 105.3(7) 2_655 2_655 ? C6D C4D C9D 177(2) 2_655 2_655 ? C9D C4D C9D 17.0(10) . 2_655 ? C5D C4D C9D 110.4(11) . 2_655 ? C7D C4D C9D 108.6(11) 2_655 2_655 ? C3D C4D C9D 145.3(12) . 2_655 ? C4D C4D C9D 52.6(6) 2_655 2_655 ? C8D C4D C9D 52.7(8) 2_655 2_655 ? C6A C5A C4A 119.1(7) . . ? C6B C5B C4B 118.8(9) . . ? C6C C5C C4C 120.8(9) . . ? C4D C5D C4D 64.5(13) . 2_655 ? C4D C5D C6D 44.7(8) . 2_655 ? C4D C5D C6D 109.1(11) 2_655 2_655 ? C4D C5D C6D 109.1(11) . . ? C4D C5D C6D 44.7(8) 2_655 . ? C6D C5D C6D 153.8(15) 2_655 . ? C5A C6A C7A 122.7(7) . . ? C5B C6B C7B 122.8(8) . . ? C5C C6C C7C 121.9(9) . . ? C3D C6D C4D 98.5(18) 2_655 2_655 ? C3D C6D C5D 163(2) 2_655 . ? C4D C6D C5D 64.5(8) 2_655 . ? C3D C6D C7D 33.0(15) 2_655 . ? C4D C6D C7D 65.5(10) 2_655 . ? C5D C6D C7D 129.9(11) . . ? C8A C7A C6A 120.4(7) . . ? C8B C7B C6B 119.9(8) . . ? C8C C7C C6C 120.5(8) . . ? C3D C7D C2D 104(2) 2_655 2_655 ? C3D C7D C4D 73.4(16) 2_655 2_655 ? C2D C7D C4D 177(2) 2_655 2_655 ? C3D C7D C8D 143(2) 2_655 . ? C2D C7D C8D 113(2) 2_655 . ? C4D C7D C8D 69.6(11) 2_655 . ? C3D C7D C6D 29.1(13) 2_655 . ? C2D C7D C6D 133(2) 2_655 . ? C4D C7D C6D 44.2(9) 2_655 . ? C8D C7D C6D 113.8(13) . . ? C3D C7D C1D 164(2) 2_655 2_655 ? C2D C7D C1D 60.7(16) 2_655 2_655 ? C4D C7D C1D 122.0(15) 2_655 2_655 ? C8D C7D C1D 53.1(10) . 2_655 ? C6D C7D C1D 165.6(15) . 2_655 ? C3D C7D C9D 117.0(18) 2_655 2_655 ? C2D C7D C9D 139(2) 2_655 2_655 ? C4D C7D C9D 43.7(8) 2_655 2_655 ? C8D C7D C9D 26.0(8) . 2_655 ? C6D C7D C9D 87.9(10) . 2_655 ? C1D C7D C9D 78.6(11) 2_655 2_655 ? O1A C8A C7A 122.9(7) . . ? O1A C8A C9A 118.6(6) . . ? C7A C8A C9A 118.4(6) . . ? O1B C8B C7B 122.7(7) . . ? O1B C8B C9B 118.1(7) . . ? C7B C8B C9B 119.1(8) . . ? O1C C8C C7C 123.3(7) . . ? O1C C8C C9C 119.8(7) . . ? C7C C8C C9C 116.9(8) . . ? N1D C8D C9D 101(2) 2_655 2_655 ? N1D C8D O1D 25.6(17) 2_655 . ? C9D C8D O1D 124.0(18) 2_655 . ? N1D C8D C1D 73(2) 2_655 2_655 ? C9D C8D C1D 168(3) 2_655 2_655 ? O1D C8D C1D 54.0(10) . 2_655 ? N1D C8D C7D 142(2) 2_655 . ? C9D C8D C7D 112.7(16) 2_655 . ? O1D C8D C7D 123.1(13) . . ? C1D C8D C7D 69.7(13) 2_655 . ? N1D C8D C9D 97(2) 2_655 . ? C9D C8D C9D 6.1(12) 2_655 . ? O1D C8D C9D 118.4(14) . . ? C1D C8D C9D 167.8(18) 2_655 . ? C7D C8D C9D 118.5(13) . . ? N1D C8D C4D 156(2) 2_655 2_655 ? C9D C8D C4D 58.4(12) 2_655 2_655 ? O1D C8D C4D 177.4(14) . 2_655 ? C1D C8D C4D 123.4(15) 2_655 2_655 ? C7D C8D C4D 54.5(9) . 2_655 ? C9D C8D C4D 64.0(9) . 2_655 ? N1D C8D C2D 118(2) 2_655 2_655 ? C9D C8D C2D 137.9(17) 2_655 2_655 ? O1D C8D C2D 97.9(10) . 2_655 ? C1D C8D C2D 44.8(10) 2_655 2_655 ? C7D C8D C2D 25.2(8) . 2_655 ? C9D C8D C2D 143.7(13) . 2_655 ? C4D C8D C2D 79.7(10) 2_655 2_655 ? N1A C9A C8A 117.0(6) . . ? N1A C9A C4A 122.6(6) . . ? C8A C9A C4A 120.4(6) . . ? N1B C9B C4B 123.8(7) . . ? N1B C9B C8B 116.6(8) . . ? C4B C9B C8B 119.6(8) . . ? N1C C9C C8C 117.4(7) . . ? N1C C9C C4C 119.5(8) . . ? C8C C9C C4C 123.0(8) . . ? C9D C9D C8D 162(3) 2_655 2_655 ? C9D C9D N1D 130.0(13) 2_655 . ? C8D C9D N1D 35.0(13) 2_655 . ? C9D C9D C4D 110.4(9) 2_655 . ? C8D C9D C4D 85.8(15) 2_655 . ? N1D C9D C4D 119.5(15) . . ? C9D C9D C8D 12(2) 2_655 . ? C8D C9D C8D 153(2) 2_655 . ? N1D C9D C8D 118.9(15) . . ? C4D C9D C8D 121.2(13) . . ? C9D C9D C4D 52.7(7) 2_655 2_655 ? C8D C9D C4D 143.7(16) 2_655 2_655 ? N1D C9D C4D 173(2) . 2_655 ? C4D C9D C4D 57.9(10) . 2_655 ? C8D C9D C4D 63.3(9) . 2_655 ? C9D C9D N1D 36.9(10) 2_655 2_655 ? C8D C9D N1D 125.9(17) 2_655 2_655 ? N1D C9D N1D 93.6(18) . 2_655 ? C4D C9D N1D 146.6(14) . 2_655 ? C8D C9D N1D 27.1(9) . 2_655 ? C4D C9D N1D 89.6(11) 2_655 2_655 ? C9D C9D C7D 154.6(14) 2_655 2_655 ? C8D C9D C7D 41.3(11) 2_655 2_655 ? N1D C9D C7D 75.2(12) . 2_655 ? C4D C9D C7D 44.6(8) . 2_655 ? C8D C9D C7D 165.8(13) . 2_655 ? C4D C9D C7D 102.5(9) 2_655 2_655 ? N1D C9D C7D 165.7(14) 2_655 2_655 ? C6D C3D C7D 118(3) 2_655 2_655 ? C6D C3D C2D 157(2) 2_655 . ? C7D C3D C2D 38.7(14) 2_655 . ? C6D C3D C4D 48.0(14) 2_655 . ? C7D C3D C4D 69.9(16) 2_655 . ? C2D C3D C4D 108.6(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.845 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.120