# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1885 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. S. Trofimenko Department of Chemistry and Biochemistry University of Delaware, Newark, DE 19716 USA ; _publ_contact_author_phone '+302 831 0716' _publ_contact_author_fax '+302 831 6335' _publ_contact_author_email trofimen@udel.edu _publ_requested_journal 'Chemcomm' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Hydrotris [3-(carboxypyrrolidido)pyrazol-1-yl] borate, the first prover... ; loop_ _publ_author_name _publ_author_address 'Trofimenko, S.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Rheingold, A. L.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; 'Incarvito, C. D.' ; University of Delaware Department of Chemistry and Biochemistry Academy Street Newark, DE 19716 U. S. A. ; # 3. Results data_trof31 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H31 B N9 O3 Tl' _chemical_formula_weight 708.76 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Tl' 'Tl' -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 34.899(4) _cell_length_b 9.2258(14) _cell_length_c 17.409(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5605.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method ? _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 5.805 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7771 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.1428 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6329 _reflns_number_observed 2716 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0800P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6329 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1331 _refine_ls_R_factor_obs 0.0403 _refine_ls_wR_factor_all 0.1222 _refine_ls_wR_factor_obs 0.0882 _refine_ls_goodness_of_fit_all 0.625 _refine_ls_goodness_of_fit_obs 0.710 _refine_ls_restrained_S_all 0.625 _refine_ls_restrained_S_obs 0.710 _refine_ls_shift/esd_max 0.649 _refine_ls_shift/esd_mean 0.034 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tl Tl 0.123790(9) 0.02123(3) 0.34177(2) 0.04490(12) Uani 1 d . . O1 O 0.0887(2) 0.2754(7) 0.2664(4) 0.058(2) Uani 1 d . . O2 O 0.1936(2) -0.1081(9) 0.2745(4) 0.077(2) Uani 1 d . . O3 O 0.0688(2) -0.1698(7) 0.4384(4) 0.066(2) Uani 1 d . . N11 N 0.1321(2) 0.2979(7) 0.3918(4) 0.043(2) Uani 1 d . . N12 N 0.1489(2) 0.3326(8) 0.4598(4) 0.045(2) Uani 1 d . . N13 N 0.0818(2) 0.5137(8) 0.2549(4) 0.058(2) Uani 1 d . . N21 N 0.1950(2) 0.0636(9) 0.3994(4) 0.049(2) Uani 1 d . . N22 N 0.2031(2) 0.1554(8) 0.4575(4) 0.050(2) Uani 1 d . . N23 N 0.2565(2) -0.0932(10) 0.2531(4) 0.058(2) Uani 1 d . . N31 N 0.1173(2) 0.0451(8) 0.4960(4) 0.045(2) Uani 1 d . . N32 N 0.1455(2) 0.1049(9) 0.5405(4) 0.049(2) Uani 1 d . . N33 N 0.0374(2) -0.1698(8) 0.5512(4) 0.051(2) Uani 1 d . . C11 C 0.1408(3) 0.4705(11) 0.4775(6) 0.061(3) Uani 1 d . . H11A H 0.1484(3) 0.5189(11) 0.5218(6) 0.073 Uiso 1 calc R . C12 C 0.1193(3) 0.5284(11) 0.4181(6) 0.072(3) Uani 1 d . . H12A H 0.1098(3) 0.6223(11) 0.4139(6) 0.086 Uiso 1 calc R . C13 C 0.1149(2) 0.4151(11) 0.3662(5) 0.047(2) Uani 1 d . . C14 C 0.0937(2) 0.3978(10) 0.2922(5) 0.042(2) Uani 1 d . . C15 C 0.0634(4) 0.4943(13) 0.1806(7) 0.094(4) Uani 1 d . . H15A H 0.0383(4) 0.4505(13) 0.1861(7) 0.113 Uiso 1 calc R . H15B H 0.0789(4) 0.4347(13) 0.1468(7) 0.113 Uiso 1 calc R . C16 C 0.0604(6) 0.6492(16) 0.1505(10) 0.177(9) Uani 1 d . . H16A H 0.0795(6) 0.6658(16) 0.1111(10) 0.213 Uiso 1 calc R . H16B H 0.0353(6) 0.6652(16) 0.1281(10) 0.213 Uiso 1 calc R . C17 C 0.0660(7) 0.7415(18) 0.2105(11) 0.271(16) Uani 1 d . . H17A H 0.0807(7) 0.8247(18) 0.1934(11) 0.325 Uiso 1 calc R . H17B H 0.0415(7) 0.7759(18) 0.2292(11) 0.325 Uiso 1 calc R . C18 C 0.0868(4) 0.6670(11) 0.2735(7) 0.109(5) Uani 1 d . . H18A H 0.1137(4) 0.6936(11) 0.2738(7) 0.130 Uiso 1 calc R . H18B H 0.0757(4) 0.6900(11) 0.3230(7) 0.130 Uiso 1 calc R . C21 C 0.2407(2) 0.1854(12) 0.4563(6) 0.062(3) Uani 1 d . . H21A H 0.2531(2) 0.2477(12) 0.4901(6) 0.075 Uiso 1 calc R . C22 C 0.2576(3) 0.1119(14) 0.3991(6) 0.075(3) Uani 1 d . . H22A H 0.2835(3) 0.1120(14) 0.3863(6) 0.090 Uiso 1 calc R . C23 C 0.2281(2) 0.0352(11) 0.3626(5) 0.054(2) Uani 1 d . . C24 C 0.2251(3) -0.0586(11) 0.2948(5) 0.055(3) Uani 1 d . . C25 C 0.2528(3) -0.1810(14) 0.1840(6) 0.082(4) Uani 1 d . . H25A H 0.2363(3) -0.1347(14) 0.1466(6) 0.099 Uiso 1 calc R . H25B H 0.2428(3) -0.2765(14) 0.1958(6) 0.099 Uiso 1 calc R . C26 C 0.2935(3) -0.1899(19) 0.1552(8) 0.126(6) Uani 1 d . . H26A H 0.3003(3) -0.2904(19) 0.1465(8) 0.152 Uiso 1 calc R . H26B H 0.2956(3) -0.1385(19) 0.1068(8) 0.152 Uiso 1 calc R . C27 C 0.3167(3) -0.1333(25) 0.2051(8) 0.192(11) Uani 1 d . . H27A H 0.3335(3) -0.0653(25) 0.1790(8) 0.231 Uiso 1 calc R . H27B H 0.3326(3) -0.2095(25) 0.2266(8) 0.231 Uiso 1 calc R . C28 C 0.2968(2) -0.0568(14) 0.2687(6) 0.083(4) Uani 1 d . . H28A H 0.3011(2) 0.0470(14) 0.2664(6) 0.100 Uiso 1 calc R . H28B H 0.3049(2) -0.0929(14) 0.3185(6) 0.100 Uiso 1 calc R . C31 C 0.1453(3) 0.0496(12) 0.6111(5) 0.064(3) Uani 1 d . . H31A H 0.1616(3) 0.0760(12) 0.6511(5) 0.077 Uiso 1 calc R . C32 C 0.1163(3) -0.0556(12) 0.6145(6) 0.067(3) Uani 1 d . . H32A H 0.1099(3) -0.1142(12) 0.6559(6) 0.080 Uiso 1 calc R . C33 C 0.0993(2) -0.0526(9) 0.5417(5) 0.046(2) Uani 1 d . . C34 C 0.0679(2) -0.1354(9) 0.5076(5) 0.045(2) Uani 1 d . . C35 C 0.0280(2) -0.1131(11) 0.6268(5) 0.056(3) Uani 1 d . . H35A H 0.0350(2) -0.0117(11) 0.6311(5) 0.067 Uiso 1 calc R . H35B H 0.0408(2) -0.1676(11) 0.6669(5) 0.067 Uiso 1 calc R . C36 C -0.0148(3) -0.1323(17) 0.6314(7) 0.095(4) Uani 1 d . . H36A H -0.0226(3) -0.1543(17) 0.6836(7) 0.115 Uiso 1 calc R . H36B H -0.0279(3) -0.0452(17) 0.6146(7) 0.115 Uiso 1 calc R . C37 C -0.0233(3) -0.2548(18) 0.5796(7) 0.104(5) Uani 1 d . . H37A H -0.0491(3) -0.2462(18) 0.5593(7) 0.125 Uiso 1 calc R . H37B H -0.0213(3) -0.3459(18) 0.6072(7) 0.125 Uiso 1 calc R . C38 C 0.0051(3) -0.2496(13) 0.5162(6) 0.074(4) Uani 1 d . . H38A H 0.0128(3) -0.3463(13) 0.5007(6) 0.089 Uiso 1 calc R . H38C H -0.0050(3) -0.1984(13) 0.4720(6) 0.089 Uiso 1 calc R . B B 0.1717(3) 0.2232(12) 0.5083(6) 0.049(3) Uani 1 d . . H1 H 0.1838(3) 0.2745(12) 0.5511(6) 0.058 Uiso 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 Tl 0.0437(2) 0.0509(2) 0.0401(2) -0.0042(2) -0.0031(2) -0.0050(2) O1 0.067(4) 0.054(4) 0.055(4) -0.008(3) -0.028(3) -0.002(3) O2 0.036(3) 0.119(6) 0.077(5) -0.045(5) -0.003(4) -0.002(4) O3 0.074(5) 0.071(5) 0.052(4) -0.009(4) 0.007(4) -0.014(4) N11 0.051(4) 0.041(4) 0.036(4) 0.005(3) 0.004(3) -0.008(4) N12 0.041(4) 0.054(5) 0.039(4) 0.000(4) -0.006(3) -0.003(4) N13 0.080(5) 0.051(5) 0.045(5) 0.002(4) -0.019(4) 0.001(4) N21 0.040(4) 0.062(5) 0.044(5) 0.005(4) 0.001(3) -0.001(4) N22 0.033(4) 0.069(5) 0.047(5) -0.001(4) -0.007(4) -0.012(4) N23 0.039(4) 0.092(7) 0.044(5) 0.007(4) -0.002(4) 0.011(4) N31 0.043(4) 0.055(4) 0.038(4) 0.010(4) -0.002(3) -0.013(4) N32 0.042(4) 0.071(5) 0.033(4) 0.004(4) -0.002(3) -0.002(4) N33 0.044(4) 0.063(5) 0.045(5) 0.000(4) 0.000(4) -0.011(4) C11 0.080(6) 0.057(6) 0.044(6) -0.012(5) -0.020(5) 0.001(5) C12 0.094(9) 0.056(6) 0.065(7) -0.011(6) -0.023(6) 0.012(6) C13 0.055(6) 0.049(5) 0.037(5) -0.005(4) 0.005(4) 0.006(5) C14 0.040(5) 0.053(6) 0.032(5) -0.002(5) -0.004(4) -0.004(4) C15 0.121(11) 0.092(10) 0.069(8) 0.000(7) -0.050(7) 0.015(8) C16 0.314(27) 0.089(11) 0.129(16) 0.026(11) -0.107(17) 0.023(14) C17 0.522(42) 0.078(12) 0.213(24) 0.038(14) -0.245(28) -0.020(19) C18 0.194(14) 0.044(7) 0.088(10) 0.016(7) -0.068(10) 0.002(8) C21 0.042(5) 0.091(8) 0.054(7) -0.007(6) -0.006(5) -0.012(5) C22 0.032(5) 0.121(10) 0.072(8) -0.013(8) -0.005(5) -0.006(6) C23 0.038(4) 0.072(7) 0.052(6) 0.003(5) -0.012(4) -0.004(5) C24 0.045(5) 0.072(7) 0.049(6) 0.008(5) -0.007(5) 0.015(5) C25 0.057(6) 0.124(10) 0.066(7) -0.025(8) -0.003(6) 0.011(7) C26 0.051(7) 0.220(18) 0.108(12) -0.054(12) -0.001(8) 0.016(9) C27 0.047(7) 0.438(34) 0.092(11) -0.119(17) 0.011(7) 0.026(13) C28 0.035(5) 0.156(12) 0.059(7) 0.002(8) -0.010(5) 0.009(6) C31 0.055(6) 0.095(8) 0.044(6) 0.026(6) -0.019(5) -0.027(6) C32 0.060(7) 0.089(8) 0.051(6) 0.034(6) -0.012(5) -0.017(6) C33 0.040(4) 0.045(6) 0.052(6) 0.003(5) 0.005(4) 0.000(4) C34 0.048(5) 0.042(5) 0.047(6) 0.003(5) -0.003(4) 0.001(4) C35 0.044(5) 0.069(7) 0.054(6) -0.003(5) 0.004(5) -0.003(5) C36 0.054(7) 0.146(13) 0.086(10) 0.013(9) 0.020(7) 0.001(8) C37 0.048(7) 0.167(15) 0.098(11) 0.001(10) 0.005(7) -0.024(8) C38 0.063(7) 0.098(9) 0.062(8) 0.001(7) -0.007(6) -0.033(6) B 0.050(6) 0.062(7) 0.034(6) -0.003(5) -0.010(5) 0.000(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 Tl N11 2.713(7) . ? Tl N31 2.704(7) . ? Tl N21 2.710(7) . ? O1 C14 1.228(10) . ? O2 C24 1.242(10) . ? O3 C34 1.246(10) . ? N11 C13 1.315(11) . ? N11 N12 1.358(8) . ? N12 C11 1.339(11) . ? N12 B 1.539(12) . ? N13 C14 1.318(11) . ? N13 C15 1.456(11) . ? N13 C18 1.461(12) . ? N21 C23 1.347(10) . ? N21 N22 1.349(9) . ? N22 C21 1.339(10) . ? N22 B 1.542(12) . ? N23 C25 1.456(12) . ? N23 C24 1.352(10) . ? N23 C28 1.471(11) . ? N31 N32 1.368(9) . ? N31 C33 1.356(10) . ? N32 C31 1.330(11) . ? N32 B 1.530(12) . ? N33 C34 1.344(10) . ? N33 C35 1.454(11) . ? N33 C38 1.477(10) . ? C11 C12 1.385(13) . ? C12 C13 1.391(13) . ? C13 C14 1.493(11) . ? C15 C16 1.53(2) . ? C16 C17 1.36(2) . ? C17 C18 1.48(2) . ? C21 C22 1.343(13) . ? C22 C23 1.401(12) . ? C23 C24 1.468(13) . ? C25 C26 1.506(13) . ? C26 C27 1.30(2) . ? C27 C28 1.486(15) . ? C31 C32 1.404(13) . ? C32 C33 1.401(12) . ? C33 C34 1.462(11) . ? C35 C36 1.505(12) . ? C36 C37 1.48(2) . ? C37 C38 1.486(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Tl N31 67.2(2) . . ? N11 Tl N21 69.3(2) . . ? N31 Tl N21 72.4(2) . . ? C13 N11 N12 107.4(7) . . ? C13 N11 Tl 128.0(6) . . ? N12 N11 Tl 123.2(5) . . ? N11 N12 C11 109.5(7) . . ? N11 N12 B 123.2(7) . . ? C11 N12 B 127.3(8) . . ? C14 N13 C15 118.5(8) . . ? C14 N13 C18 129.7(8) . . ? C15 N13 C18 111.6(8) . . ? C23 N21 N22 107.4(7) . . ? C23 N21 Tl 125.6(6) . . ? N22 N21 Tl 124.1(5) . . ? C21 N22 N21 108.9(8) . . ? C21 N22 B 128.4(8) . . ? N21 N22 B 122.4(7) . . ? C25 N23 C24 120.2(8) . . ? C25 N23 C28 111.4(8) . . ? C24 N23 C28 128.4(9) . . ? N32 N31 C33 105.7(7) . . ? N32 N31 Tl 122.3(5) . . ? C33 N31 Tl 124.5(6) . . ? C31 N32 N31 111.4(7) . . ? C31 N32 B 127.9(8) . . ? N31 N32 B 120.7(7) . . ? C34 N33 C35 127.3(7) . . ? C34 N33 C38 119.2(8) . . ? C35 N33 C38 112.3(7) . . ? N12 C11 C12 108.0(9) . . ? C11 C12 C13 104.8(9) . . ? N11 C13 C12 110.3(8) . . ? N11 C13 C14 115.5(8) . . ? C12 C13 C14 134.1(9) . . ? O1 C14 N13 121.4(8) . . ? O1 C14 C13 119.0(8) . . ? N13 C14 C13 119.6(8) . . ? N13 C15 C16 102.7(10) . . ? C17 C16 C15 108.2(13) . . ? C18 C17 C16 110.4(15) . . ? N13 C18 C17 103.1(10) . . ? N22 C21 C22 109.8(9) . . ? C23 C22 C21 105.5(8) . . ? N21 C23 C22 108.4(9) . . ? N21 C23 C24 115.9(8) . . ? C22 C23 C24 135.6(9) . . ? O2 C24 N23 118.6(9) . . ? O2 C24 C23 120.6(8) . . ? N23 C24 C23 120.9(8) . . ? N23 C25 C26 102.8(9) . . ? C27 C26 C25 110.2(11) . . ? C26 C27 C28 113.4(10) . . ? C27 C28 N23 101.6(9) . . ? N32 C31 C32 107.9(8) . . ? C33 C32 C31 104.8(8) . . ? C32 C33 N31 110.2(8) . . ? C32 C33 C34 132.5(9) . . ? N31 C33 C34 117.2(8) . . ? O3 C34 N33 120.5(8) . . ? O3 C34 C33 120.4(9) . . ? N33 C34 C33 119.1(8) . . ? N33 C35 C36 103.3(8) . . ? C37 C36 C35 104.9(10) . . ? C36 C37 C38 107.1(10) . . ? N33 C38 C37 102.7(8) . . ? N32 B N22 110.3(8) . . ? N32 B N12 111.1(7) . . ? N22 B N12 108.6(7) . . ? _refine_diff_density_max 0.905 _refine_diff_density_min -0.897 _refine_diff_density_rms 0.117 data_trof86 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H68 B2 F6 La N18 O10 P' _chemical_formula_weight 1434.76 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 25.7439(3) _cell_length_b 19.9574(2) _cell_length_c 25.7150(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.1056(5) _cell_angle_gamma 90.00 _cell_volume 12964.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5872 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.6552 _exptl_absorpt_correction_T_max 0.8019 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi 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 23373 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10194 _reflns_number_gt 9581 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 10194 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2616 _refine_ls_wR_factor_gt 0.2581 _refine_ls_goodness_of_fit_ref 2.205 _refine_ls_restrained_S_all 2.205 _refine_ls_shift/su_max 0.338 _refine_ls_shift/su_mean 0.015 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 0.670513(12) 1.137653(17) -0.863598(11) 0.0279(2) Uani 1 1 d . . . O1 O 0.62572(19) 1.1494(3) -0.78255(17) 0.0445(12) Uani 1 1 d . . . O2 O 0.68049(19) 1.0393(3) -0.93149(17) 0.0442(12) Uani 1 1 d . . . O3 O 0.68206(19) 1.2106(3) -0.94419(18) 0.0491(12) Uani 1 1 d . . . O4 O 0.66151(18) 1.0221(2) -0.82122(18) 0.0443(12) Uani 1 1 d . . . O5 O 0.67202(18) 1.2624(2) -0.83315(19) 0.0448(11) Uani 1 1 d . . . O6 O 0.5481(5) 1.1716(10) -1.1774(4) 0.189(7) Uani 1 1 d . . . N1 N 0.7304(2) 1.1472(3) -0.7680(2) 0.0447(15) Uani 1 1 d . . . N2 N 0.7844(2) 1.1447(3) -0.7494(2) 0.0368(13) Uani 1 1 d . . . N3 N 0.6254(3) 1.2021(4) -0.7032(3) 0.068(2) Uani 1 1 d . . . N4 N 0.7606(2) 1.0611(3) -0.8526(2) 0.0403(13) Uani 1 1 d . . . N5 N 0.8101(2) 1.0701(3) -0.8217(2) 0.0453(15) Uani 1 1 d . . . N6 N 0.7037(3) 0.9313(4) -0.9450(3) 0.0620(19) Uani 1 1 d . . . N7 N 0.7640(2) 1.1974(3) -0.8649(2) 0.0414(13) Uani 1 1 d . . . N8 N 0.8115(2) 1.1936(4) -0.8317(3) 0.0520(16) Uani 1 1 d . . . N9 N 0.7058(3) 1.3140(4) -0.9676(3) 0.0573(18) Uani 1 1 d . . . N10 N 0.57740(18) 1.0679(3) -0.89213(18) 0.0286(11) Uani 1 1 d . . . N11 N 0.5284(2) 1.0827(3) -0.9204(3) 0.0432(15) Uani 1 1 d . . . N12 N 0.6299(3) 0.9162(3) -0.8221(3) 0.0559(18) Uani 1 1 d . . . N13 N 0.58308(18) 1.2194(3) -0.89554(18) 0.0304(11) Uani 1 1 d . . . N14 N 0.5333(2) 1.2100(3) -0.9257(2) 0.0426(14) Uani 1 1 d . . . N15 N 0.6495(2) 1.3708(3) -0.8380(3) 0.0421(14) Uani 1 1 d . . . N16 N 0.5372(2) 1.1438(4) -1.0058(2) 0.0514(19) Uani 1 1 d . . . N17 N 0.5186(3) 1.1848(5) -1.0449(3) 0.092(3) Uani 1 1 d . . . H17A H 0.4929 1.2141 -1.0460 0.110 Uiso 1 1 calc R . . N18 N 0.5193(5) 1.2579(7) -1.1459(8) 0.131(6) Uani 1 1 d . . . B1 B 0.8222(3) 1.1355(4) -0.7898(4) 0.044(2) Uani 1 1 d . . . H20A H 0.8600 1.1363 -0.7709 0.053 Uiso 1 1 calc R . . B2 B 0.5134(3) 1.1457(4) -0.9547(3) 0.0355(18) Uani 1 1 d . . . H30C H 0.4740 1.1480 -0.9651 0.043 Uiso 1 1 calc R . . C1 C 0.7106(3) 1.1593(4) -0.7249(3) 0.0473(17) Uani 1 1 d . . . C2 C 0.7486(3) 1.1610(5) -0.6780(3) 0.065(2) Uani 1 1 d . . . H2A H 0.7438 1.1679 -0.6427 0.078 Uiso 1 1 calc R . . C3 C 0.7950(3) 1.1501(4) -0.6963(3) 0.0473(18) Uani 1 1 d . . . H3A H 0.8292 1.1470 -0.6746 0.057 Uiso 1 1 calc R . . C4 C 0.6516(3) 1.1684(6) -0.7373(3) 0.063(2) Uani 1 1 d . . . C5 C 0.5674(3) 1.2116(6) -0.7178(4) 0.076(3) Uani 1 1 d . . . H5A H 0.5493 1.1693 -0.7305 0.091 Uiso 1 1 calc R . . H5B H 0.5582 1.2465 -0.7454 0.091 Uiso 1 1 calc R . . C6 C 0.5533(5) 1.2338(10) -0.6660(5) 0.135(6) Uani 1 1 d . . . H6A H 0.5221 1.2638 -0.6719 0.162 Uiso 1 1 calc R . . H6B H 0.5463 1.1949 -0.6443 0.162 Uiso 1 1 calc R . . C7 C 0.6025(6) 1.2703(11) -0.6406(6) 0.166(9) Uani 1 1 d . . . H7A H 0.6016 1.3166 -0.6546 0.199 Uiso 1 1 calc R . . H7B H 0.6045 1.2728 -0.6018 0.199 Uiso 1 1 calc R . . C8 C 0.6477(4) 1.2363(8) -0.6515(4) 0.102(4) Uani 1 1 d . . . H8A H 0.6615 1.2034 -0.6234 0.122 Uiso 1 1 calc R . . H8B H 0.6762 1.2681 -0.6554 0.122 Uiso 1 1 calc R . . C9 C 0.7628(3) 1.0049(4) -0.8811(2) 0.0392(15) Uani 1 1 d . . . C10 C 0.8147(3) 0.9760(5) -0.8669(3) 0.061(2) Uani 1 1 d . . . H10A H 0.8270 0.9357 -0.8799 0.074 Uiso 1 1 calc R . . C11 C 0.8426(3) 1.0195(4) -0.8301(3) 0.053(2) Uani 1 1 d . . . H11A H 0.8787 1.0148 -0.8134 0.063 Uiso 1 1 calc R . . C12 C 0.7136(3) 0.9920(4) -0.9197(3) 0.0446(16) Uani 1 1 d . . . C13 C 0.7363(5) 0.8716(5) -0.9332(6) 0.097(4) Uani 1 1 d . . . H13A H 0.7460 0.8641 -0.8945 0.116 Uiso 1 1 calc R . . H13B H 0.7690 0.8754 -0.9479 0.116 Uiso 1 1 calc R . . C14 C 0.7024(7) 0.8168(10) -0.9592(12) 0.217(15) Uani 1 1 d . . . H14A H 0.7238 0.7833 -0.9742 0.261 Uiso 1 1 calc R . . H14B H 0.6841 0.7942 -0.9335 0.261 Uiso 1 1 calc R . . C15 C 0.6640(7) 0.8489(7) -1.0014(8) 0.156(9) Uani 1 1 d . . . H15A H 0.6298 0.8249 -1.0065 0.187 Uiso 1 1 calc R . . H15B H 0.6771 0.8476 -1.0351 0.187 Uiso 1 1 calc R . . C16 C 0.6566(4) 0.9212(5) -0.9855(4) 0.078(3) Uani 1 1 d . . . H16A H 0.6558 0.9522 -1.0158 0.094 Uiso 1 1 calc R . . H16B H 0.6239 0.9268 -0.9711 0.094 Uiso 1 1 calc R . . C17 C 0.7658(3) 1.2487(4) -0.8976(3) 0.0482(18) Uani 1 1 d . . . C18 C 0.8171(3) 1.2768(5) -0.8883(3) 0.069(3) Uani 1 1 d . . . H18A H 0.8301 1.3119 -0.9072 0.083 Uiso 1 1 calc R . . C19 C 0.8438(3) 1.2415(5) -0.8452(4) 0.072(3) Uani 1 1 d . . . H19A H 0.8793 1.2495 -0.8278 0.087 Uiso 1 1 calc R . . C20 C 0.7157(3) 1.2590(5) -0.9384(3) 0.055(2) Uani 1 1 d . . . C21 C 0.7403(4) 1.3774(5) -0.9648(4) 0.072(3) Uani 1 1 d . . . H21A H 0.7537 1.3915 -0.9278 0.086 Uiso 1 1 calc R . . H21B H 0.7704 1.3711 -0.9832 0.086 Uiso 1 1 calc R . . C22 C 0.7000(6) 1.4268(6) -0.9941(6) 0.111(5) Uani 1 1 d . . . H22A H 0.6808 1.4492 -0.9691 0.133 Uiso 1 1 calc R . . H22B H 0.7177 1.4614 -1.0120 0.133 Uiso 1 1 calc R . . C23 C 0.6640(5) 1.3883(7) -1.0323(5) 0.093(3) Uani 1 1 d . . . H23A H 0.6792 1.3804 -1.0643 0.112 Uiso 1 1 calc R . . H23B H 0.6300 1.4123 -1.0428 0.112 Uiso 1 1 calc R . . C24 C 0.6556(4) 1.3225(6) -1.0060(3) 0.081(3) Uani 1 1 d . . . H24A H 0.6251 1.3250 -0.9878 0.097 Uiso 1 1 calc R . . H24B H 0.6499 1.2854 -1.0320 0.097 Uiso 1 1 calc R . . C25 C 0.5749(3) 1.0067(4) -0.8700(3) 0.054(2) Uani 1 1 d . . . C26 C 0.5220(4) 0.9844(6) -0.8802(7) 0.154(9) Uani 1 1 d . . . H26A H 0.5086 0.9439 -0.8685 0.185 Uiso 1 1 calc R . . C27 C 0.4927(4) 1.0359(6) -0.9122(6) 0.110(5) Uani 1 1 d . . . H27A H 0.4555 1.0369 -0.9251 0.132 Uiso 1 1 calc R . . C28 C 0.6239(3) 0.9809(3) -0.8374(3) 0.0408(16) Uani 1 1 d . . . C29 C 0.5908(4) 0.8604(5) -0.8379(6) 0.088(4) Uani 1 1 d . . . H29A H 0.5814 0.8560 -0.8769 0.106 Uiso 1 1 calc R . . H29B H 0.5582 0.8679 -0.8237 0.106 Uiso 1 1 calc R . . C30 C 0.6204(4) 0.7992(5) -0.8131(6) 0.100(4) Uani 1 1 d . . . H30A H 0.6003 0.7781 -0.7882 0.120 Uiso 1 1 calc R . . H30B H 0.6232 0.7661 -0.8411 0.120 Uiso 1 1 calc R . . C31 C 0.6740(6) 0.8169(7) -0.7843(10) 0.224(15) Uani 1 1 d . . . H31A H 0.7011 0.7938 -0.8004 0.269 Uiso 1 1 calc R . . H31B H 0.6786 0.8030 -0.7468 0.269 Uiso 1 1 calc R . . C32 C 0.6803(3) 0.8931(4) -0.7881(4) 0.058(2) Uani 1 1 d . . . H32A H 0.6852 0.9140 -0.7525 0.070 Uiso 1 1 calc R . . H32B H 0.7110 0.9045 -0.8044 0.070 Uiso 1 1 calc R . . C33 C 0.5871(3) 1.2866(3) -0.8829(3) 0.0382(15) Uani 1 1 d . . . C34 C 0.5413(3) 1.3221(5) -0.9095(4) 0.065(2) Uani 1 1 d . . . H34A H 0.5351 1.3690 -0.9095 0.078 Uiso 1 1 calc R . . C35 C 0.5079(3) 1.2730(5) -0.9349(4) 0.060(2) Uani 1 1 d . . . H35A H 0.4735 1.2804 -0.9554 0.072 Uiso 1 1 calc R . . C36 C 0.6389(2) 1.3069(4) -0.8498(3) 0.0398(17) Uani 1 1 d . . . C37 C 0.7020(3) 1.3919(4) -0.8054(3) 0.055(2) Uani 1 1 d . . . H37A H 0.7065 1.3738 -0.7690 0.066 Uiso 1 1 calc R . . H37B H 0.7316 1.3756 -0.8216 0.066 Uiso 1 1 calc R . . C38 C 0.7005(5) 1.4661(5) -0.8049(6) 0.114(5) Uani 1 1 d . . . H38A H 0.7137 1.4828 -0.7685 0.137 Uiso 1 1 calc R . . H38B H 0.7236 1.4842 -0.8283 0.137 Uiso 1 1 calc R . . C39 C 0.6469(4) 1.4883(6) -0.8232(6) 0.097(4) Uani 1 1 d . . . H39A H 0.6463 1.5267 -0.8477 0.116 Uiso 1 1 calc R . . H39B H 0.6312 1.5027 -0.7928 0.116 Uiso 1 1 calc R . . C40 C 0.6156(4) 1.4299(5) -0.8518(4) 0.072(3) Uani 1 1 d . . . H40A H 0.5816 1.4242 -0.8397 0.087 Uiso 1 1 calc R . . H40B H 0.6082 1.4373 -0.8906 0.087 Uiso 1 1 calc R . . C41 C 0.5471(4) 1.1727(8) -1.0837(3) 0.099(5) Uani 1 1 d . . . C42 C 0.5843(5) 1.1227(8) -1.0694(4) 0.109(5) Uani 1 1 d . . . H42A H 0.6091 1.1053 -1.0889 0.131 Uiso 1 1 calc R . . C43 C 0.5763(3) 1.1044(5) -1.0193(3) 0.065(2) Uani 1 1 d . . . H43A H 0.5950 1.0701 -0.9978 0.079 Uiso 1 1 calc R . . C44 C 0.5359(5) 1.2085(15) -1.1339(6) 0.160(10) Uani 1 1 d . . . C45 C 0.5110(5) 1.3062(9) -1.1109(7) 0.105(5) Uani 1 1 d . . . H45A H 0.5415 1.3048 -1.0808 0.126 Uiso 1 1 calc R . . H45B H 0.4794 1.2929 -1.0968 0.126 Uiso 1 1 calc R . . C46 C 0.5033(10) 1.3797(15) -1.1287(17) 0.237(16) Uani 1 1 d . . . H46A H 0.4753 1.4037 -1.1147 0.284 Uiso 1 1 calc R . . H46B H 0.5364 1.4062 -1.1242 0.284 Uiso 1 1 calc R . . C47 C 0.4871(10) 1.3532(10) -1.1784(10) 0.146(7) Uani 1 1 d . . . H47A H 0.4943 1.3883 -1.2032 0.175 Uiso 1 1 calc R . . H47B H 0.4481 1.3499 -1.1834 0.175 Uiso 1 1 calc R . . C48 C 0.5054(7) 1.2859(11) -1.2006(7) 0.140(6) Uani 1 1 d . . . H48A H 0.4765 1.2614 -1.2239 0.168 Uiso 1 1 calc R . . H48B H 0.5363 1.2911 -1.2181 0.168 Uiso 1 1 calc R . . P1 P 0.6400(3) 1.3759(4) 0.5276(2) 0.178(3) Uani 1 1 d . . . F1 F 0.6368(11) 1.3168(7) 0.4926(7) 0.329(14) Uani 1 1 d . . . F2 F 0.7011(11) 1.3700(14) 0.5500(10) 0.387(19) Uani 1 1 d . . . F3 F 0.6366(10) 1.4372(12) 0.5633(9) 0.342(13) Uani 1 1 d . . . F4 F 0.5779(8) 1.3825(12) 0.5044(9) 0.301(12) Uani 1 1 d . . . F5 F 0.6298(9) 1.3357(14) 0.5776(8) 0.335(13) Uani 1 1 d . . . F6 F 0.6483(8) 1.4261(7) 0.4827(5) 0.247(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0268(3) 0.0268(4) 0.0282(3) 0.00124(11) 0.00063(16) -0.00483(12) O1 0.040(3) 0.062(3) 0.029(2) 0.003(2) 0.0009(19) -0.001(2) O2 0.051(3) 0.037(3) 0.039(2) -0.011(2) -0.006(2) 0.004(2) O3 0.047(3) 0.057(4) 0.045(2) 0.011(2) 0.012(2) -0.005(2) O4 0.047(3) 0.031(3) 0.047(2) 0.006(2) -0.010(2) -0.010(2) O5 0.043(3) 0.029(3) 0.057(3) -0.007(2) -0.003(2) -0.004(2) O6 0.123(8) 0.37(2) 0.077(6) 0.055(9) 0.013(6) -0.112(11) N1 0.029(3) 0.057(4) 0.043(3) -0.005(3) -0.005(2) 0.010(2) N2 0.035(3) 0.027(4) 0.040(3) -0.005(2) -0.011(2) -0.001(2) N3 0.069(4) 0.078(6) 0.052(4) -0.009(3) -0.002(3) 0.020(4) N4 0.037(3) 0.042(4) 0.042(3) -0.005(2) 0.008(2) -0.006(2) N5 0.033(3) 0.061(5) 0.039(3) 0.000(3) -0.003(2) 0.008(3) N6 0.060(4) 0.047(5) 0.078(5) -0.023(4) 0.010(3) 0.000(3) N7 0.033(3) 0.044(4) 0.047(3) 0.008(3) 0.007(2) -0.013(2) N8 0.030(3) 0.060(5) 0.064(4) -0.002(3) 0.004(3) -0.015(3) N9 0.060(4) 0.060(5) 0.056(4) 0.028(3) 0.023(3) 0.000(3) N10 0.025(2) 0.026(3) 0.031(2) 0.008(2) -0.0010(18) -0.007(2) N11 0.025(3) 0.036(4) 0.060(4) 0.009(3) -0.011(2) -0.015(2) N12 0.052(4) 0.026(4) 0.079(4) 0.018(3) -0.016(3) -0.008(3) N13 0.028(2) 0.035(3) 0.028(2) 0.013(2) 0.0045(18) -0.002(2) N14 0.032(3) 0.040(4) 0.051(3) -0.001(3) -0.004(2) -0.001(2) N15 0.045(3) 0.019(4) 0.059(4) -0.004(2) 0.002(3) -0.006(2) N16 0.036(3) 0.093(6) 0.023(3) 0.010(3) -0.003(2) -0.020(3) N17 0.047(4) 0.170(9) 0.048(4) 0.057(5) -0.017(3) -0.036(5) N18 0.092(8) 0.068(10) 0.213(17) 0.067(10) -0.021(9) -0.032(6) B1 0.031(4) 0.039(6) 0.057(5) -0.007(3) -0.007(4) -0.001(3) B2 0.030(4) 0.044(5) 0.030(4) 0.012(3) 0.000(3) -0.008(3) C1 0.045(4) 0.056(5) 0.037(3) 0.005(3) -0.004(3) 0.008(3) C2 0.057(5) 0.095(7) 0.035(4) -0.001(4) -0.009(3) 0.016(5) C3 0.053(4) 0.037(5) 0.042(4) -0.002(3) -0.017(3) 0.015(3) C4 0.036(4) 0.117(8) 0.037(4) 0.014(4) 0.009(3) 0.013(4) C5 0.061(5) 0.096(8) 0.074(6) -0.016(5) 0.021(4) 0.008(5) C6 0.106(10) 0.237(19) 0.068(7) -0.032(9) 0.029(7) 0.063(11) C7 0.106(10) 0.28(2) 0.101(10) -0.102(13) -0.006(8) 0.067(13) C8 0.083(7) 0.167(13) 0.050(5) -0.051(7) 0.001(5) 0.004(7) C9 0.046(4) 0.040(4) 0.029(3) 0.010(3) 0.001(2) 0.008(3) C10 0.073(5) 0.064(6) 0.042(4) 0.005(4) -0.001(3) 0.028(4) C11 0.045(4) 0.068(6) 0.042(4) 0.006(3) 0.002(3) 0.019(4) C12 0.043(4) 0.034(5) 0.056(4) 0.000(3) 0.007(3) 0.003(3) C13 0.078(7) 0.058(8) 0.153(12) -0.053(7) 0.020(7) 0.002(5) C14 0.093(11) 0.115(16) 0.41(4) -0.13(2) -0.039(17) 0.016(10) C15 0.146(13) 0.086(11) 0.204(18) -0.119(12) -0.046(13) 0.008(10) C16 0.071(6) 0.072(7) 0.087(6) -0.050(5) 0.002(5) -0.010(5) C17 0.046(4) 0.054(5) 0.046(4) 0.016(3) 0.012(3) -0.013(3) C18 0.045(4) 0.087(7) 0.073(5) 0.038(5) 0.004(4) -0.026(4) C19 0.054(5) 0.074(7) 0.086(6) 0.002(5) 0.006(4) -0.032(5) C20 0.050(4) 0.077(6) 0.042(4) 0.019(4) 0.020(3) -0.007(4) C21 0.097(7) 0.060(6) 0.072(6) 0.028(5) 0.048(5) 0.008(5) C22 0.158(13) 0.061(8) 0.133(11) 0.052(8) 0.074(10) 0.041(8) C23 0.107(9) 0.097(9) 0.079(7) 0.036(7) 0.025(6) 0.012(8) C24 0.087(6) 0.108(9) 0.052(5) 0.046(5) 0.028(4) 0.019(6) C25 0.045(4) 0.039(5) 0.069(5) 0.011(4) -0.011(3) -0.020(3) C26 0.058(6) 0.077(9) 0.29(2) 0.124(11) -0.061(9) -0.044(6) C27 0.068(6) 0.066(8) 0.180(13) 0.055(8) -0.019(7) -0.036(6) C28 0.040(3) 0.024(4) 0.054(4) -0.002(3) -0.004(3) -0.014(3) C29 0.060(6) 0.054(7) 0.132(10) 0.041(6) -0.030(6) -0.022(4) C30 0.080(7) 0.034(7) 0.164(11) 0.039(6) -0.035(7) -0.013(5) C31 0.139(13) 0.039(10) 0.41(3) 0.075(13) -0.158(18) -0.029(8) C32 0.052(4) 0.043(6) 0.071(5) 0.013(4) -0.008(4) -0.001(4) C33 0.039(3) 0.024(4) 0.050(4) -0.009(3) 0.005(3) 0.001(3) C34 0.054(5) 0.041(6) 0.093(6) 0.010(4) -0.005(4) 0.008(4) C35 0.041(4) 0.051(6) 0.082(6) -0.003(4) -0.006(4) 0.004(4) C36 0.027(3) 0.046(5) 0.041(3) -0.005(3) -0.004(2) 0.007(3) C37 0.051(4) 0.041(5) 0.067(5) -0.017(4) -0.003(4) -0.009(4) C38 0.098(8) 0.020(7) 0.195(14) -0.036(7) -0.047(8) -0.003(5) C39 0.077(7) 0.050(7) 0.150(11) -0.003(7) -0.012(7) 0.001(5) C40 0.059(5) 0.061(7) 0.087(6) -0.014(5) -0.010(5) 0.008(5) C41 0.068(6) 0.187(13) 0.032(4) 0.038(6) -0.015(4) -0.075(8) C42 0.072(7) 0.205(15) 0.052(5) -0.036(7) 0.018(5) -0.090(9) C43 0.060(5) 0.091(7) 0.048(4) -0.011(4) 0.015(4) -0.030(5) C44 0.079(8) 0.32(3) 0.077(8) 0.101(13) -0.002(6) -0.060(13) C45 0.078(8) 0.082(11) 0.148(13) 0.040(10) 0.003(8) -0.015(7) C46 0.122(17) 0.20(3) 0.35(5) 0.09(3) -0.05(2) -0.023(17) C47 0.17(2) 0.104(15) 0.166(19) 0.032(12) 0.036(16) -0.043(13) C48 0.130(13) 0.152(18) 0.139(13) 0.033(13) 0.030(10) -0.025(12) P1 0.232(8) 0.202(7) 0.098(3) -0.035(4) 0.027(4) -0.103(6) F1 0.54(4) 0.108(10) 0.256(18) -0.039(10) -0.14(2) -0.008(15) F2 0.30(3) 0.56(5) 0.23(2) -0.08(2) -0.13(2) 0.06(2) F3 0.43(3) 0.31(2) 0.34(3) -0.16(2) 0.20(2) -0.18(2) F4 0.246(19) 0.29(2) 0.31(2) 0.047(19) -0.071(18) -0.126(18) F5 0.30(2) 0.46(3) 0.209(17) 0.05(2) -0.021(16) -0.22(2) F6 0.40(2) 0.206(13) 0.160(10) 0.027(9) 0.107(13) -0.052(14) _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 O1 2.579(5) . ? La1 O4 2.581(5) . ? La1 O3 2.596(5) . ? La1 O5 2.607(5) . ? La1 N1 2.645(6) . ? La1 O2 2.672(4) . ? La1 N7 2.692(5) . ? La1 N10 2.746(5) . ? La1 N4 2.747(6) . ? La1 N13 2.773(5) . ? O1 C4 1.281(9) . ? O2 C12 1.269(8) . ? O3 C20 1.287(9) . ? O4 C28 1.278(7) . ? O5 C36 1.249(8) . ? O6 C44 1.42(3) . ? N1 C1 1.330(9) . ? N1 N2 1.381(8) . ? N2 C3 1.344(10) . ? N2 B1 1.564(12) . ? N3 C4 1.381(11) . ? N3 C5 1.479(11) . ? N3 C8 1.506(10) . ? N4 C9 1.346(9) . ? N4 N5 1.377(8) . ? N5 C11 1.354(10) . ? N5 B1 1.541(10) . ? N6 C12 1.375(10) . ? N6 C16 1.452(11) . ? N6 C13 1.454(13) . ? N7 C17 1.332(8) . ? N7 N8 1.351(8) . ? N8 C19 1.356(10) . ? N8 B1 1.570(11) . ? N9 C20 1.326(10) . ? N9 C24 1.476(12) . ? N9 C21 1.541(12) . ? N10 C25 1.356(9) . ? N10 N11 1.360(7) . ? N11 C27 1.357(11) . ? N11 B2 1.542(9) . ? N12 C28 1.351(9) . ? N12 C32 1.489(9) . ? N12 C29 1.504(10) . ? N13 N14 1.377(7) . ? N13 C33 1.380(10) . ? N14 C35 1.416(11) . ? N14 B2 1.522(10) . ? N15 C36 1.326(9) . ? N15 C40 1.469(11) . ? N15 C37 1.507(9) . ? N16 N17 1.315(9) . ? N16 C43 1.373(12) . ? N16 B2 1.552(9) . ? N17 C41 1.370(15) . ? N18 C44 1.10(3) . ? N18 C45 1.36(2) . ? N18 C48 1.49(2) . ? C1 C2 1.399(10) . ? C1 C4 1.502(10) . ? C2 C3 1.382(12) . ? C5 C6 1.513(13) . ? C6 C7 1.50(2) . ? C7 C8 1.419(16) . ? C9 C10 1.436(10) . ? C9 C12 1.474(9) . ? C10 C11 1.379(12) . ? C13 C14 1.474(19) . ? C14 C15 1.47(3) . ? C15 C16 1.520(14) . ? C17 C18 1.412(10) . ? C17 C20 1.511(10) . ? C18 C19 1.380(12) . ? C21 C22 1.521(15) . ? C22 C23 1.435(18) . ? C23 C24 1.510(14) . ? C25 C26 1.409(11) . ? C25 C28 1.465(10) . ? C26 C27 1.436(14) . ? C29 C30 1.513(13) . ? C30 C31 1.478(15) . ? C31 C32 1.535(17) . ? C33 C34 1.432(10) . ? C33 C36 1.494(9) . ? C34 C35 1.382(12) . ? C37 C38 1.483(13) . ? C38 C39 1.438(14) . ? C39 C40 1.524(14) . ? C41 C42 1.38(2) . ? C41 C44 1.454(14) . ? C42 C43 1.394(13) . ? C45 C46 1.54(3) . ? C45 C47 1.96(3) . ? C46 C47 1.37(4) . ? C47 C48 1.57(3) . ? P1 F1 1.477(16) . ? P1 F3 1.542(19) . ? P1 F2 1.57(3) . ? P1 F6 1.574(13) . ? P1 F5 1.58(2) . ? P1 F4 1.60(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O4 69.49(16) . . ? O1 La1 O3 137.03(16) . . ? O4 La1 O3 150.65(17) . . ? O1 La1 O5 69.73(16) . . ? O4 La1 O5 136.38(16) . . ? O3 La1 O5 72.97(16) . . ? O1 La1 N1 60.93(16) . . ? O4 La1 N1 75.86(17) . . ? O3 La1 N1 124.45(18) . . ? O5 La1 N1 71.34(17) . . ? O1 La1 O2 135.14(16) . . ? O4 La1 O2 69.32(15) . . ? O3 La1 O2 81.38(16) . . ? O5 La1 O2 154.14(16) . . ? N1 La1 O2 123.21(16) . . ? O1 La1 N7 120.62(16) . . ? O4 La1 N7 123.68(16) . . ? O3 La1 N7 60.11(16) . . ? O5 La1 N7 67.60(17) . . ? N1 La1 N7 67.47(18) . . ? O2 La1 N7 96.84(17) . . ? O1 La1 N10 76.05(15) . . ? O4 La1 N10 61.00(14) . . ? O3 La1 N10 107.39(14) . . ? O5 La1 N10 121.70(15) . . ? N1 La1 N10 127.41(17) . . ? O2 La1 N10 69.02(15) . . ? N7 La1 N10 163.26(16) . . ? O1 La1 N4 117.86(16) . . ? O4 La1 N4 66.55(16) . . ? O3 La1 N4 99.79(16) . . ? O5 La1 N4 122.45(16) . . ? N1 La1 N4 67.31(17) . . ? O2 La1 N4 58.21(15) . . ? N7 La1 N4 60.56(19) . . ? N10 La1 N4 114.98(17) . . ? O1 La1 N13 73.86(14) . . ? O4 La1 N13 121.13(15) . . ? O3 La1 N13 69.21(14) . . ? O5 La1 N13 59.45(15) . . ? N1 La1 N13 121.85(17) . . ? O2 La1 N13 114.41(15) . . ? N7 La1 N13 114.35(16) . . ? N10 La1 N13 66.53(17) . . ? N4 La1 N13 168.27(15) . . ? C4 O1 La1 121.6(4) . . ? C12 O2 La1 122.4(4) . . ? C20 O3 La1 120.4(4) . . ? C28 O4 La1 124.1(4) . . ? C36 O5 La1 127.4(4) . . ? C1 N1 N2 103.8(6) . . ? C1 N1 La1 122.7(4) . . ? N2 N1 La1 133.4(4) . . ? C3 N2 N1 110.0(6) . . ? C3 N2 B1 130.8(6) . . ? N1 N2 B1 119.1(6) . . ? C4 N3 C5 119.7(7) . . ? C4 N3 C8 129.2(8) . . ? C5 N3 C8 111.1(7) . . ? C9 N4 N5 107.0(6) . . ? C9 N4 La1 122.0(4) . . ? N5 N4 La1 131.0(4) . . ? C11 N5 N4 110.0(6) . . ? C11 N5 B1 130.5(6) . . ? N4 N5 B1 119.1(6) . . ? C12 N6 C16 120.9(7) . . ? C12 N6 C13 125.2(8) . . ? C16 N6 C13 113.8(8) . . ? C17 N7 N8 107.8(5) . . ? C17 N7 La1 119.2(4) . . ? N8 N7 La1 132.0(4) . . ? N7 N8 C19 108.9(7) . . ? N7 N8 B1 119.5(6) . . ? C19 N8 B1 131.3(7) . . ? C20 N9 C24 121.5(8) . . ? C20 N9 C21 127.4(7) . . ? C24 N9 C21 111.0(7) . . ? C25 N10 N11 107.8(5) . . ? C25 N10 La1 117.0(4) . . ? N11 N10 La1 134.8(4) . . ? C27 N11 N10 110.8(7) . . ? C27 N11 B2 123.2(7) . . ? N10 N11 B2 125.9(5) . . ? C28 N12 C32 120.4(6) . . ? C28 N12 C29 126.5(6) . . ? C32 N12 C29 113.0(6) . . ? N14 N13 C33 106.5(5) . . ? N14 N13 La1 134.6(4) . . ? C33 N13 La1 118.8(4) . . ? N13 N14 C35 108.9(6) . . ? N13 N14 B2 125.3(6) . . ? C35 N14 B2 124.5(6) . . ? C36 N15 C40 129.1(6) . . ? C36 N15 C37 121.2(6) . . ? C40 N15 C37 109.7(6) . . ? N17 N16 C43 109.8(7) . . ? N17 N16 B2 119.2(7) . . ? C43 N16 B2 131.0(6) . . ? N16 N17 C41 106.3(9) . . ? C44 N18 C45 123(2) . . ? C44 N18 C48 128(2) . . ? C45 N18 C48 108.6(14) . . ? N5 B1 N2 111.4(6) . . ? N5 B1 N8 105.6(7) . . ? N2 B1 N8 108.7(6) . . ? N14 B2 N11 112.6(6) . . ? N14 B2 N16 106.6(5) . . ? N11 B2 N16 111.6(6) . . ? N1 C1 C2 114.0(7) . . ? N1 C1 C4 112.2(6) . . ? C2 C1 C4 133.8(7) . . ? C3 C2 C1 102.0(7) . . ? N2 C3 C2 109.9(6) . . ? O1 C4 N3 119.2(6) . . ? O1 C4 C1 119.1(7) . . ? N3 C4 C1 121.4(7) . . ? N3 C5 C6 102.5(8) . . ? C7 C6 C5 101.4(10) . . ? C8 C7 C6 109.7(12) . . ? C7 C8 N3 101.7(9) . . ? N4 C9 C10 109.3(6) . . ? N4 C9 C12 113.1(6) . . ? C10 C9 C12 137.5(7) . . ? C11 C10 C9 104.9(7) . . ? N5 C11 C10 108.8(6) . . ? O2 C12 N6 119.2(7) . . ? O2 C12 C9 118.8(6) . . ? N6 C12 C9 122.0(7) . . ? N6 C13 C14 104.3(11) . . ? C15 C14 C13 105.4(16) . . ? C14 C15 C16 108.5(10) . . ? N6 C16 C15 101.2(9) . . ? N7 C17 C18 110.0(6) . . ? N7 C17 C20 114.5(6) . . ? C18 C17 C20 135.2(6) . . ? C19 C18 C17 103.9(7) . . ? N8 C19 C18 109.2(7) . . ? O3 C20 N9 120.3(7) . . ? O3 C20 C17 116.3(7) . . ? N9 C20 C17 123.4(7) . . ? C22 C21 N9 100.2(9) . . ? C23 C22 C21 106.3(11) . . ? C22 C23 C24 106.8(9) . . ? N9 C24 C23 102.6(9) . . ? N10 C25 C26 109.2(7) . . ? N10 C25 C28 116.9(6) . . ? C26 C25 C28 133.6(7) . . ? C25 C26 C27 105.3(8) . . ? N11 C27 C26 106.5(8) . . ? O4 C28 N12 118.8(6) . . ? O4 C28 C25 118.4(6) . . ? N12 C28 C25 122.8(6) . . ? N12 C29 C30 103.2(7) . . ? C31 C30 C29 111.3(9) . . ? C30 C31 C32 107.8(9) . . ? N12 C32 C31 104.7(7) . . ? N13 C33 C34 110.6(6) . . ? N13 C33 C36 114.6(6) . . ? C34 C33 C36 134.5(7) . . ? C35 C34 C33 104.8(7) . . ? C34 C35 N14 109.0(7) . . ? O5 C36 N15 120.7(6) . . ? O5 C36 C33 118.5(7) . . ? N15 C36 C33 120.9(6) . . ? C38 C37 N15 105.1(7) . . ? C39 C38 C37 109.2(9) . . ? C38 C39 C40 107.9(9) . . ? N15 C40 C39 105.3(7) . . ? N17 C41 C42 112.0(8) . . ? N17 C41 C44 121.2(15) . . ? C42 C41 C44 126.8(15) . . ? C41 C42 C43 102.5(10) . . ? N16 C43 C42 109.3(11) . . ? N18 C44 O6 112.1(16) . . ? N18 C44 C41 134(3) . . ? O6 C44 C41 114(2) . . ? N18 C45 C46 120(2) . . ? N18 C45 C47 79.4(13) . . ? C46 C45 C47 44.0(15) . . ? C47 C46 C45 85(2) . . ? C46 C47 C48 128(2) . . ? C46 C47 C45 51.3(14) . . ? C48 C47 C45 81.3(12) . . ? N18 C48 C47 90.6(15) . . ? F1 P1 F3 173.7(16) . . ? F1 P1 F2 95.5(16) . . ? F3 P1 F2 90.5(13) . . ? F1 P1 F6 93.6(11) . . ? F3 P1 F6 87.8(12) . . ? F2 P1 F6 92.8(15) . . ? F1 P1 F5 95.3(14) . . ? F3 P1 F5 83.2(13) . . ? F2 P1 F5 88.6(14) . . ? F6 P1 F5 170.9(14) . . ? F1 P1 F4 84.5(12) . . ? F3 P1 F4 89.4(15) . . ? F2 P1 F4 179.4(17) . . ? F6 P1 F4 86.7(11) . . ? F5 P1 F4 91.9(13) . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 1.416 _refine_diff_density_min -1.235 _refine_diff_density_rms 0.135 data_trof87 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H65 B2 Cl5 F6 N18 Nd O6 P' _chemical_formula_weight 1502.28 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 26.0247(4) _cell_length_b 19.8463(3) _cell_length_c 26.3284(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.9329(7) _cell_angle_gamma 90.00 _cell_volume 13198.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6104 _exptl_absorpt_coefficient_mu 1.090 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6696 _exptl_absorpt_correction_T_max 0.6696 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi 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 27637 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12673 _reflns_number_gt 10448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 12673 _refine_ls_number_parameters 842 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2638 _refine_ls_wR_factor_gt 0.2425 _refine_ls_goodness_of_fit_ref 2.040 _refine_ls_restrained_S_all 2.045 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_mean 0.007 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 Nd1 Nd 0.826924(12) 0.638766(16) -0.132118(14) 0.03290(17) Uani 1 1 d . . . P1 P 1.0000 0.93826(18) -0.2500 0.0746(11) Uani 1 2 d S . . Cl1 Cl 0.9600(9) 1.0312(12) 0.0808(7) 0.575(6) Uani 1 1 d D . . Cl2 Cl 1.0319(3) 1.0584(4) 0.0052(3) 0.206(3) Uani 1 1 d D . . Cl3 Cl 0.8380(5) 0.4814(7) -0.3530(8) 0.387(9) Uani 1 1 d . . . Cl4 Cl 0.9126(5) 0.5206(3) -0.2572(3) 0.324(7) Uani 1 1 d . . . Cl5 Cl 0.9245(4) 0.5564(3) -0.3562(2) 0.210(3) Uani 1 1 d . . . O1 O 0.83372(17) 0.5237(2) -0.17103(19) 0.0402(11) Uani 1 1 d . . . O2 O 0.82232(19) 0.7619(3) -0.1608(2) 0.0485(13) Uani 1 1 d . . . O3 O 0.9610(6) 0.6508(8) 0.1886(8) 0.206(9) Uani 1 1 d . . . O4 O 0.8194(2) 0.7079(3) -0.0540(2) 0.0535(13) Uani 1 1 d . . . O5 O 0.8210(2) 0.5462(3) -0.0637(2) 0.0466(12) Uani 1 1 d . . . O6 O 0.87003(19) 0.6548(3) -0.2070(2) 0.0435(11) Uani 1 1 d . . . N1 N 0.9180(2) 0.5707(3) -0.1008(2) 0.0350(12) Uani 1 1 d . . . N2 N 0.9659(2) 0.5813(3) -0.0677(2) 0.0373(12) Uani 1 1 d . . . N3 N 0.9135(2) 0.7200(3) -0.0996(2) 0.0390(13) Uani 1 1 d . . . N4 N 0.9647(2) 0.7089(3) -0.0731(3) 0.0428(14) Uani 1 1 d . . . N5 N 0.9825(3) 0.6947(5) 0.0484(4) 0.109(4) Uani 1 1 d . . . N6 N 0.9607(3) 0.6505(4) 0.0113(3) 0.057(2) Uani 1 1 d . . . N7 N 0.8654(2) 0.4187(3) -0.1714(3) 0.0505(16) Uani 1 1 d . . . N8 N 0.8493(3) 0.8680(3) -0.1654(3) 0.0468(16) Uani 1 1 d . . . N9 N 0.9817(4) 0.7539(4) 0.1556(5) 0.092(4) Uani 1 1 d . . . N10 N 0.7371(2) 0.6983(3) -0.1320(3) 0.0434(14) Uani 1 1 d . . . N11 N 0.6881(2) 0.6948(3) -0.1657(3) 0.0484(15) Uani 1 1 d . . . N12 N 0.7389(2) 0.5637(3) -0.1430(3) 0.0417(14) Uani 1 1 d . . . N13 N 0.6905(2) 0.5704(3) -0.1740(3) 0.0465(15) Uani 1 1 d . . . N14 N 0.7658(2) 0.6493(3) -0.2252(2) 0.0392(13) Uani 1 1 d . . . N15 N 0.7129(2) 0.6436(3) -0.2437(3) 0.0411(14) Uani 1 1 d . . . N16 N 0.7977(3) 0.8096(3) -0.0277(3) 0.062(2) Uani 1 1 d . . . N17 N 0.7992(3) 0.4394(4) -0.0509(4) 0.069(2) Uani 1 1 d . . . N18 N 0.8696(3) 0.7014(3) -0.2845(3) 0.0530(16) Uani 1 1 d . . . C1 C 0.9189(2) 0.5051(3) -0.1169(3) 0.0376(15) Uani 1 1 d . . . C2 C 0.9667(3) 0.4752(4) -0.0927(3) 0.055(2) Uani 1 1 d . . . H2A H 0.9772 0.4300 -0.0964 0.066 Uiso 1 1 calc R . . C3 C 0.9953(3) 0.5245(4) -0.0627(3) 0.0489(19) Uani 1 1 d . . . H3B H 1.0303 0.5197 -0.0416 0.059 Uiso 1 1 calc R . . C4 C 0.8697(3) 0.4827(3) -0.1549(3) 0.0397(15) Uani 1 1 d . . . C5 C 0.9065(4) 0.3647(4) -0.1595(5) 0.073(3) Uani 1 1 d . . . H5B H 0.9151 0.3520 -0.1221 0.088 Uiso 1 1 calc R . . H5C H 0.9392 0.3781 -0.1697 0.088 Uiso 1 1 calc R . . C6 C 0.8774(5) 0.3082(6) -0.1942(9) 0.203(13) Uani 1 1 d . . . H6A H 0.8951 0.2999 -0.2230 0.243 Uiso 1 1 calc R . . H6B H 0.8799 0.2664 -0.1733 0.243 Uiso 1 1 calc R . . C7 C 0.8252(5) 0.3224(6) -0.2152(7) 0.138(8) Uani 1 1 d . . . H7A H 0.8027 0.2952 -0.1976 0.166 Uiso 1 1 calc R . . H7B H 0.8158 0.3110 -0.2529 0.166 Uiso 1 1 calc R . . C8 C 0.8155(3) 0.3973(4) -0.2080(4) 0.063(2) Uani 1 1 d . . . H8A H 0.8097 0.4218 -0.2417 0.075 Uiso 1 1 calc R . . H8B H 0.7847 0.4044 -0.1928 0.075 Uiso 1 1 calc R . . C9 C 0.9116(3) 0.7818(3) -0.1193(3) 0.0377(15) Uani 1 1 d . . . C10 C 0.9631(3) 0.8107(4) -0.1052(4) 0.056(2) Uani 1 1 d . . . H10A H 0.9736 0.8543 -0.1138 0.067 Uiso 1 1 calc R . . C11 C 0.9935(3) 0.7627(4) -0.0772(4) 0.058(2) Uani 1 1 d . . . H11A H 1.0305 0.7667 -0.0623 0.069 Uiso 1 1 calc R . . C12 C 0.8586(3) 0.8043(3) -0.1503(3) 0.0384(15) Uani 1 1 d . . . C13 C 0.8863(4) 0.9254(4) -0.1557(5) 0.067(3) Uani 1 1 d . . . H13A H 0.9159 0.9182 -0.1728 0.080 Uiso 1 1 calc R . . H13B H 0.9010 0.9322 -0.1178 0.080 Uiso 1 1 calc R . . C14 C 0.8527(5) 0.9850(5) -0.1797(6) 0.103(5) Uani 1 1 d . . . H14A H 0.8499 1.0176 -0.1521 0.123 Uiso 1 1 calc R . . H14B H 0.8692 1.0081 -0.2051 0.123 Uiso 1 1 calc R . . C15 C 0.8033(5) 0.9619(6) -0.2046(9) 0.185(11) Uani 1 1 d . . . H15A H 0.7972 0.9705 -0.2426 0.222 Uiso 1 1 calc R . . H15B H 0.7763 0.9873 -0.1916 0.222 Uiso 1 1 calc R . . C16 C 0.7966(3) 0.8880(4) -0.1959(4) 0.060(2) Uani 1 1 d . . . H16A H 0.7693 0.8799 -0.1760 0.072 Uiso 1 1 calc R . . H16B H 0.7867 0.8633 -0.2295 0.072 Uiso 1 1 calc R . . C17 C 0.9550(7) 0.6812(13) 0.0889(6) 0.183(12) Uani 1 1 d D . . C18 C 0.9209(6) 0.6383(10) 0.0750(4) 0.126(8) Uani 1 1 d . . . H18A H 0.8970 0.6242 0.0951 0.152 Uiso 1 1 calc R . . C19 C 0.9215(4) 0.6117(6) 0.0243(3) 0.067(3) Uani 1 1 d . . . H19A H 0.9005 0.5768 0.0049 0.081 Uiso 1 1 calc R . . C20 C 0.9639(6) 0.7030(14) 0.1462(7) 0.232(18) Uani 1 1 d D . . C21 C 0.9933(5) 0.8107(6) 0.1152(5) 0.093(4) Uani 1 1 d . . . H21A H 1.0229 0.7978 0.0996 0.112 Uiso 1 1 calc R . . H21B H 0.9615 0.8212 0.0872 0.112 Uiso 1 1 calc R . . C22 C 1.0083(11) 0.8684(8) 0.1550(7) 0.159(9) Uani 1 1 d . . . H22A H 1.0445 0.8835 0.1546 0.191 Uiso 1 1 calc R . . H22B H 0.9842 0.9066 0.1423 0.191 Uiso 1 1 calc R . . C23 C 1.0074(14) 0.8556(8) 0.2094(12) 0.24(2) Uani 1 1 d . . . H23A H 1.0409 0.8695 0.2337 0.285 Uiso 1 1 calc R . . H23B H 0.9774 0.8789 0.2189 0.285 Uiso 1 1 calc R . . C24 C 1.0008(7) 0.7833(8) 0.2091(6) 0.132(6) Uani 1 1 d . . . H24A H 0.9753 0.7718 0.2302 0.159 Uiso 1 1 calc R . . H24B H 1.0352 0.7624 0.2261 0.159 Uiso 1 1 calc R . . C25 C 0.7366(3) 0.7485(3) -0.0981(3) 0.050(2) Uani 1 1 d . . . C26 C 0.6859(4) 0.7801(4) -0.1102(5) 0.071(3) Uani 1 1 d . . . H26A H 0.6743 0.8175 -0.0934 0.085 Uiso 1 1 calc R . . C27 C 0.6577(4) 0.7432(5) -0.1522(5) 0.070(3) Uani 1 1 d . . . H27A H 0.6217 0.7509 -0.1693 0.085 Uiso 1 1 calc R . . C28 C 0.7865(3) 0.7551(4) -0.0588(3) 0.0480(18) Uani 1 1 d . . . C29 C 0.8510(5) 0.8153(5) 0.0099(4) 0.078(3) Uani 1 1 d . . . H29A H 0.8797 0.8180 -0.0088 0.093 Uiso 1 1 calc R . . H29B H 0.8577 0.7766 0.0344 0.093 Uiso 1 1 calc R . . C30 C 0.8460(8) 0.8809(7) 0.0386(6) 0.127(6) Uani 1 1 d . . . H30A H 0.8804 0.9046 0.0486 0.152 Uiso 1 1 calc R . . H30B H 0.8331 0.8723 0.0704 0.152 Uiso 1 1 calc R . . C31 C 0.8058(7) 0.9218(7) -0.0013(7) 0.127(6) Uani 1 1 d . . . H31A H 0.8230 0.9445 -0.0263 0.152 Uiso 1 1 calc R . . H31B H 0.7888 0.9563 0.0164 0.152 Uiso 1 1 calc R . . C32 C 0.7649(6) 0.8701(4) -0.0294(5) 0.089(4) Uani 1 1 d . . . H32A H 0.7367 0.8630 -0.0105 0.107 Uiso 1 1 calc R . . H32B H 0.7487 0.8839 -0.0658 0.107 Uiso 1 1 calc R . . C33 C 0.7387(3) 0.5082(3) -0.1144(3) 0.0406(15) Uani 1 1 d . . . C34 C 0.6883(3) 0.4775(4) -0.1285(3) 0.0517(19) Uani 1 1 d . . . H34A H 0.6777 0.4366 -0.1154 0.062 Uiso 1 1 calc R . . C35 C 0.6585(3) 0.5189(4) -0.1648(3) 0.0512(19) Uani 1 1 d . . . H35A H 0.6220 0.5134 -0.1810 0.061 Uiso 1 1 calc R . . C36 C 0.7894(3) 0.4976(4) -0.0739(3) 0.0481(18) Uani 1 1 d . . . C37 C 0.7671(5) 0.3783(6) -0.0579(8) 0.131(7) Uani 1 1 d . . . H37A H 0.7558 0.3659 -0.0954 0.158 Uiso 1 1 calc R . . H37B H 0.7353 0.3843 -0.0440 0.158 Uiso 1 1 calc R . . C38 C 0.8023(8) 0.3271(11) -0.0283(17) 0.35(3) Uani 1 1 d . . . H38A H 0.7818 0.2956 -0.0116 0.420 Uiso 1 1 calc R . . H38B H 0.8190 0.3010 -0.0520 0.420 Uiso 1 1 calc R . . C39 C 0.8429(6) 0.3605(7) 0.0117(8) 0.130(7) Uani 1 1 d . . . H39A H 0.8768 0.3356 0.0177 0.156 Uiso 1 1 calc R . . H39B H 0.8320 0.3631 0.0451 0.156 Uiso 1 1 calc R . . C40 C 0.8487(4) 0.4292(6) -0.0089(5) 0.091(4) Uani 1 1 d . . . H40A H 0.8804 0.4319 -0.0233 0.110 Uiso 1 1 calc R . . H40B H 0.8517 0.4635 0.0190 0.110 Uiso 1 1 calc R . . C41 C 0.7866(3) 0.6612(4) -0.2661(3) 0.0430(16) Uani 1 1 d . . . C42 C 0.7463(3) 0.6611(4) -0.3131(3) 0.053(2) Uani 1 1 d . . . H42A H 0.7499 0.6667 -0.3479 0.063 Uiso 1 1 calc R . . C43 C 0.7013(3) 0.6511(4) -0.2966(4) 0.050(2) Uani 1 1 d . . . H43A H 0.6667 0.6496 -0.3189 0.059 Uiso 1 1 calc R . . C44 C 0.8451(3) 0.6722(4) -0.2514(3) 0.0417(16) Uani 1 1 d . . . C45 C 0.8440(4) 0.7308(6) -0.3368(4) 0.073(3) Uani 1 1 d . . . H45A H 0.8109 0.7550 -0.3362 0.088 Uiso 1 1 calc R . . H45B H 0.8365 0.6959 -0.3645 0.088 Uiso 1 1 calc R . . C46 C 0.8893(5) 0.7811(7) -0.3442(5) 0.098(4) Uani 1 1 d . . . H46A H 0.8875 0.7891 -0.3817 0.118 Uiso 1 1 calc R . . H46B H 0.8871 0.8247 -0.3267 0.118 Uiso 1 1 calc R . . C47 C 0.9394(4) 0.7424(7) -0.3178(4) 0.084(3) Uani 1 1 d . . . H47A H 0.9463 0.7054 -0.3405 0.101 Uiso 1 1 calc R . . H47B H 0.9705 0.7728 -0.3096 0.101 Uiso 1 1 calc R . . C48 C 0.9273(3) 0.7149(5) -0.2680(4) 0.065(2) Uani 1 1 d . . . H48A H 0.9475 0.6731 -0.2563 0.078 Uiso 1 1 calc R . . H48B H 0.9356 0.7485 -0.2394 0.078 Uiso 1 1 calc R . . C49 C 0.984(2) 1.011(2) 0.0262(16) 0.56(2) Uani 1 1 d D . . H49A H 0.9521 1.0248 0.0010 0.671 Uiso 1 1 d R . . H49B H 0.9887 0.9641 0.0208 0.671 Uiso 1 1 d R . . C50 C 0.9072(10) 0.4993(9) -0.3194(8) 0.160(8) Uani 1 1 d . . . H50A H 0.9288 0.4579 -0.3204 0.192 Uiso 1 1 calc R . . F1 F 1.0244(4) 0.9373(6) -0.1892(4) 0.159(4) Uani 1 1 d . . . F2 F 0.9617(5) 0.8799(5) -0.2397(6) 0.199(7) Uani 1 1 d . . . F3 F 0.9589(2) 0.9935(3) -0.2443(3) 0.104(2) Uani 1 1 d . . . B1 B 0.9830(3) 0.6475(4) -0.0385(4) 0.046(2) Uani 1 1 d . . . B2 B 0.6767(3) 0.6369(4) -0.2062(4) 0.048(2) Uani 1 1 d . . . P2 P 0.8446(4) 1.1283(7) -0.0258(4) 0.166(6) Uani 0.50 1 d P . . F5 F 0.7873(9) 1.1209(15) -0.0494(7) 0.224(16) Uani 0.50 1 d PD . . F4 F 0.8354(11) 1.0671(12) 0.0184(8) 0.46(5) Uani 0.50 1 d PD . . F9 F 0.8406(12) 1.1855(9) 0.0139(6) 0.189(11) Uani 0.50 1 d P . . F8 F 0.9039(6) 1.1265(12) 0.0149(10) 0.53(5) Uani 0.50 1 d PD . . F7 F 0.8813(18) 1.1742(14) -0.0631(12) 0.32(3) Uani 0.50 1 d PD . . F6 F 0.8553(13) 1.0666(11) -0.0613(7) 0.30(2) Uani 0.50 1 d PD . . H1 H 1.022(3) 0.668(4) -0.029(3) 0.038(18) Uiso 1 1 d . . . H2 H 0.630(4) 0.692(6) -0.221(5) 0.10(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0243(2) 0.0290(2) 0.0424(3) -0.00317(14) 0.00201(15) 0.00062(12) P1 0.069(2) 0.0483(18) 0.111(3) 0.000 0.031(2) 0.000 Cl1 0.69(2) 0.75(2) 0.343(18) -0.181(19) 0.249(19) -0.528 Cl2 0.177(5) 0.256(8) 0.176(6) -0.052(6) 0.026(5) -0.022(5) Cl3 0.281(13) 0.355(16) 0.57(3) 0.123(17) 0.192(14) 0.031(11) Cl4 0.74(2) 0.124(4) 0.222(7) -0.028(4) 0.333(11) -0.049(8) Cl5 0.381(10) 0.155(5) 0.135(4) 0.008(3) 0.141(6) 0.012(5) O1 0.027(2) 0.038(2) 0.048(3) -0.007(2) -0.004(2) 0.0084(19) O2 0.037(3) 0.041(3) 0.061(3) 0.005(2) -0.001(2) -0.004(2) O3 0.167(12) 0.191(13) 0.30(2) -0.182(14) 0.130(13) -0.116(10) O4 0.055(3) 0.049(3) 0.058(3) -0.012(3) 0.015(3) -0.010(3) O5 0.043(3) 0.046(3) 0.049(3) 0.003(2) 0.008(2) -0.003(2) O6 0.029(2) 0.049(3) 0.050(3) -0.005(2) 0.005(2) 0.000(2) N1 0.026(3) 0.041(3) 0.037(3) -0.002(2) 0.006(2) 0.000(2) N2 0.031(3) 0.042(3) 0.035(3) -0.005(2) 0.000(2) 0.009(2) N3 0.028(3) 0.044(3) 0.041(3) -0.003(3) 0.001(2) 0.000(2) N4 0.030(3) 0.038(3) 0.054(4) -0.006(3) -0.002(3) -0.003(2) N5 0.067(5) 0.135(8) 0.097(7) -0.080(6) -0.039(5) 0.058(5) N6 0.048(4) 0.071(5) 0.040(4) -0.017(3) -0.010(3) 0.028(3) N7 0.039(3) 0.038(3) 0.064(4) -0.009(3) -0.009(3) 0.000(3) N8 0.043(4) 0.032(3) 0.060(4) 0.003(3) 0.003(3) -0.007(2) N9 0.065(6) 0.039(4) 0.156(10) -0.019(5) -0.002(6) 0.011(4) N10 0.033(3) 0.033(3) 0.066(4) -0.002(3) 0.015(3) 0.001(2) N11 0.032(3) 0.043(3) 0.072(4) -0.001(3) 0.015(3) 0.011(3) N12 0.022(3) 0.029(3) 0.070(4) -0.001(3) 0.004(3) 0.003(2) N13 0.030(3) 0.040(3) 0.066(4) -0.001(3) 0.004(3) -0.003(2) N14 0.028(3) 0.042(3) 0.042(3) 0.002(2) -0.002(2) 0.002(2) N15 0.023(3) 0.036(3) 0.056(4) 0.000(2) -0.005(3) 0.001(2) N16 0.086(5) 0.045(4) 0.066(5) -0.015(3) 0.037(4) -0.008(4) N17 0.051(4) 0.054(4) 0.103(6) 0.026(4) 0.017(4) 0.009(3) N18 0.049(4) 0.062(4) 0.045(4) 0.004(3) 0.007(3) -0.002(3) C1 0.029(3) 0.042(4) 0.038(4) -0.002(3) -0.001(3) 0.006(3) C2 0.050(4) 0.045(4) 0.057(5) -0.010(4) -0.012(4) 0.020(4) C3 0.034(4) 0.051(4) 0.052(5) -0.011(4) -0.008(3) 0.014(3) C4 0.034(3) 0.033(3) 0.046(4) -0.007(3) -0.001(3) 0.002(3) C5 0.049(5) 0.037(4) 0.112(9) -0.016(4) -0.021(5) 0.010(3) C6 0.101(10) 0.052(7) 0.37(3) -0.103(12) -0.105(14) 0.041(7) C7 0.102(9) 0.054(6) 0.203(16) -0.054(8) -0.073(10) 0.021(6) C8 0.047(5) 0.045(5) 0.082(6) -0.008(4) -0.013(4) -0.003(4) C9 0.037(4) 0.035(3) 0.041(4) -0.001(3) 0.008(3) -0.007(3) C10 0.036(4) 0.043(4) 0.087(6) -0.008(4) 0.012(4) -0.007(3) C11 0.037(4) 0.056(5) 0.078(6) -0.014(4) 0.010(4) -0.008(4) C12 0.040(4) 0.032(3) 0.044(4) -0.002(3) 0.011(3) -0.004(3) C13 0.053(5) 0.037(4) 0.103(8) 0.003(4) 0.005(5) -0.013(4) C14 0.088(8) 0.039(5) 0.155(12) 0.022(6) -0.022(8) -0.014(5) C15 0.098(10) 0.046(6) 0.35(3) 0.071(11) -0.074(14) -0.010(6) C16 0.051(5) 0.040(4) 0.075(6) 0.011(4) -0.010(4) -0.003(4) C17 0.112(11) 0.33(3) 0.068(9) -0.102(13) -0.059(8) 0.167(16) C18 0.101(10) 0.24(2) 0.031(5) 0.020(8) 0.007(6) 0.126(13) C19 0.060(6) 0.091(7) 0.051(5) 0.003(5) 0.017(4) 0.050(5) C20 0.046(8) 0.35(4) 0.27(3) 0.19(3) -0.016(12) -0.017(14) C21 0.074(7) 0.097(8) 0.091(8) -0.039(7) -0.015(6) 0.004(6) C22 0.29(3) 0.100(12) 0.096(12) -0.038(9) 0.059(16) -0.060(13) C23 0.33(4) 0.077(12) 0.23(3) -0.011(13) -0.07(3) 0.024(15) C24 0.133(13) 0.130(13) 0.127(12) -0.063(10) 0.019(10) -0.006(10) C25 0.064(5) 0.025(3) 0.074(5) -0.005(3) 0.039(4) 0.002(3) C26 0.065(6) 0.045(5) 0.108(8) -0.010(5) 0.030(6) 0.021(4) C27 0.041(4) 0.057(5) 0.116(9) 0.007(5) 0.026(5) 0.019(4) C28 0.053(4) 0.038(4) 0.059(5) -0.012(3) 0.025(4) -0.009(3) C29 0.103(8) 0.078(6) 0.052(5) -0.029(5) 0.017(5) -0.029(6) C30 0.22(2) 0.070(8) 0.094(10) -0.030(8) 0.048(12) -0.037(10) C31 0.205(17) 0.070(8) 0.136(13) -0.058(9) 0.102(13) -0.060(10) C32 0.145(11) 0.040(5) 0.100(8) -0.026(5) 0.063(8) -0.010(5) C33 0.034(3) 0.035(3) 0.053(4) -0.006(3) 0.011(3) -0.003(3) C34 0.050(4) 0.044(4) 0.058(5) -0.001(4) 0.008(4) -0.015(4) C35 0.041(4) 0.048(4) 0.067(5) -0.015(4) 0.018(4) -0.013(3) C36 0.045(4) 0.045(4) 0.058(5) 0.006(3) 0.020(4) 0.008(3) C37 0.075(8) 0.054(6) 0.25(2) 0.062(10) 0.017(10) 0.000(6) C38 0.118(16) 0.132(17) 0.74(8) 0.27(3) -0.01(3) 0.006(13) C39 0.081(9) 0.110(12) 0.192(19) 0.092(12) 0.018(11) 0.000(7) C40 0.073(7) 0.089(8) 0.112(9) 0.067(7) 0.024(6) 0.025(6) C41 0.039(4) 0.044(4) 0.041(4) -0.001(3) 0.000(3) -0.001(3) C42 0.057(5) 0.050(4) 0.043(4) 0.004(3) -0.006(4) -0.009(4) C43 0.039(4) 0.040(4) 0.060(5) -0.005(3) -0.007(4) 0.002(3) C44 0.036(4) 0.044(4) 0.043(4) -0.005(3) 0.006(3) -0.002(3) C45 0.068(6) 0.097(8) 0.053(5) 0.004(5) 0.012(5) -0.017(5) C46 0.102(9) 0.119(10) 0.082(8) 0.023(7) 0.038(7) -0.029(8) C47 0.061(6) 0.116(9) 0.078(7) 0.025(7) 0.021(5) -0.028(6) C48 0.049(5) 0.086(7) 0.064(6) 0.004(5) 0.024(4) -0.012(4) C49 0.76(7) 0.74(7) 0.31(5) -0.32(4) 0.41(5) -0.556 C50 0.24(2) 0.125(14) 0.157(17) 0.011(12) 0.119(17) 0.023(15) F1 0.165(9) 0.170(9) 0.122(7) 0.055(7) -0.003(7) 0.044(7) F2 0.252(13) 0.101(6) 0.327(16) -0.082(8) 0.231(13) -0.079(7) F3 0.067(4) 0.086(4) 0.151(7) 0.009(4) 0.008(4) 0.023(3) B1 0.031(4) 0.054(5) 0.047(5) -0.015(4) -0.007(3) 0.005(3) B2 0.027(4) 0.040(4) 0.073(6) 0.003(4) 0.005(4) 0.002(3) P2 0.093(6) 0.286(15) 0.113(7) -0.120(9) 0.014(5) -0.041(7) F5 0.19(2) 0.41(4) 0.057(10) 0.012(16) 0.000(12) -0.18(3) F4 1.00(12) 0.31(4) 0.18(3) 0.13(3) 0.35(5) 0.42(6) F9 0.38(3) 0.093(11) 0.069(10) -0.015(8) 0.007(15) -0.029(17) F8 0.029(8) 0.59(6) 0.87(9) -0.67(7) -0.08(2) 0.042(17) F7 0.63(6) 0.19(2) 0.28(3) 0.18(2) 0.37(4) 0.23(3) F6 0.58(6) 0.21(2) 0.083(13) -0.062(14) 0.03(2) -0.25(4) _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 Nd1 O6 2.512(5) . ? Nd1 O4 2.518(5) . ? Nd1 O1 2.526(5) . ? Nd1 O2 2.553(5) . ? Nd1 N14 2.588(6) . ? Nd1 O5 2.602(5) . ? Nd1 N10 2.621(6) . ? Nd1 N1 2.680(5) . ? Nd1 N12 2.691(5) . ? Nd1 N3 2.735(5) . ? P1 F3 1.564(6) 2_754 ? P1 F3 1.564(6) . ? P1 F1 1.574(10) . ? P1 F1 1.574(10) 2_754 ? P1 F2 1.594(8) 2_754 ? P1 F2 1.594(8) . ? Cl1 C49 1.737(18) . ? Cl2 C49 1.61(3) 5_775 ? Cl2 C49 1.763(18) . ? Cl3 C50 1.84(2) . ? Cl4 C50 1.67(2) . ? Cl5 C50 1.621(19) . ? O1 C4 1.237(8) . ? O2 C12 1.245(8) . ? O3 C20 1.54(3) . ? O4 C28 1.256(9) . ? O5 C36 1.255(9) . ? O6 C44 1.240(9) . ? N1 N2 1.354(7) . ? N1 C1 1.370(9) . ? N2 C3 1.351(9) . ? N2 B1 1.534(10) . ? N3 C9 1.327(9) . ? N3 N4 1.365(8) . ? N4 C11 1.324(10) . ? N4 B1 1.527(11) . ? N5 N6 1.335(10) . ? N5 C17 1.44(3) . ? N6 C19 1.386(14) . ? N6 B1 1.556(13) . ? N7 C4 1.338(9) . ? N7 C8 1.480(9) . ? N7 C5 1.494(10) . ? N8 C12 1.329(8) . ? N8 C16 1.468(10) . ? N8 C13 1.475(9) . ? N9 C20 1.11(3) . ? N9 C24 1.495(17) . ? N9 C21 1.627(17) . ? N10 C25 1.338(9) . ? N10 N11 1.368(8) . ? N11 C27 1.344(10) . ? N11 B2 1.548(11) . ? N12 N13 1.331(8) . ? N12 C33 1.334(9) . ? N13 C35 1.377(10) . ? N13 B2 1.564(10) . ? N14 C41 1.338(10) . ? N14 N15 1.350(8) . ? N15 C43 1.362(11) . ? N15 B2 1.525(12) . ? N16 C28 1.344(10) . ? N16 C32 1.467(13) . ? N16 C29 1.501(13) . ? N17 C36 1.302(10) . ? N17 C37 1.459(13) . ? N17 C40 1.494(13) . ? N18 C44 1.331(10) . ? N18 C48 1.485(10) . ? N18 C45 1.496(11) . ? C1 C2 1.387(9) . ? C1 C4 1.490(9) . ? C2 C3 1.360(11) . ? C5 C6 1.526(13) . ? C6 C7 1.366(16) . ? C7 C8 1.526(14) . ? C9 C10 1.422(10) . ? C9 C12 1.492(10) . ? C10 C11 1.342(12) . ? C13 C14 1.517(13) . ? C14 C15 1.374(15) . ? C15 C16 1.502(13) . ? C17 C18 1.22(3) . ? C17 C20 1.531(18) . ? C18 C19 1.439(15) . ? C21 C22 1.539(17) . ? C22 C23 1.46(3) . ? C23 C24 1.44(2) . ? C25 C26 1.426(12) . ? C25 C28 1.459(12) . ? C26 C27 1.380(14) . ? C29 C30 1.527(16) . ? C30 C31 1.52(2) . ? C31 C32 1.534(17) . ? C33 C34 1.412(10) . ? C33 C36 1.496(10) . ? C34 C35 1.355(12) . ? C37 C38 1.46(2) . ? C38 C39 1.46(4) . ? C39 C40 1.488(14) . ? C41 C42 1.417(10) . ? C41 C44 1.495(10) . ? C42 C43 1.358(13) . ? C45 C46 1.591(14) . ? C46 C47 1.528(16) . ? C47 C48 1.523(13) . ? C49 Cl2 1.61(3) 5_775 ? C49 C49 1.85(5) 5_775 ? P2 F5 1.48(2) . ? P2 F9 1.56(2) . ? P2 F6 1.61(3) . ? P2 F8 1.652(18) . ? P2 F4 1.74(2) . ? P2 F7 1.78(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Nd1 O4 135.11(16) . . ? O6 Nd1 O1 73.04(17) . . ? O4 Nd1 O1 148.26(18) . . ? O6 Nd1 O2 69.16(17) . . ? O4 Nd1 O2 73.29(19) . . ? O1 Nd1 O2 138.44(18) . . ? O6 Nd1 N14 62.33(18) . . ? O4 Nd1 N14 125.32(19) . . ? O1 Nd1 N14 77.07(16) . . ? O2 Nd1 N14 70.61(17) . . ? O6 Nd1 O5 138.11(17) . . ? O4 Nd1 O5 77.91(18) . . ? O1 Nd1 O5 70.39(16) . . ? O2 Nd1 O5 150.95(18) . . ? N14 Nd1 O5 125.94(17) . . ? O6 Nd1 N10 120.74(18) . . ? O4 Nd1 N10 60.57(19) . . ? O1 Nd1 N10 123.90(16) . . ? O2 Nd1 N10 65.82(17) . . ? N14 Nd1 N10 67.7(2) . . ? O5 Nd1 N10 96.66(18) . . ? O6 Nd1 N1 77.08(16) . . ? O4 Nd1 N1 105.08(18) . . ? O1 Nd1 N1 61.70(15) . . ? O2 Nd1 N1 123.29(16) . . ? N14 Nd1 N1 128.92(18) . . ? O5 Nd1 N1 68.06(16) . . ? N10 Nd1 N1 161.84(19) . . ? O6 Nd1 N12 121.11(18) . . ? O4 Nd1 N12 99.05(18) . . ? O1 Nd1 N12 66.25(16) . . ? O2 Nd1 N12 121.39(16) . . ? N14 Nd1 N12 68.33(19) . . ? O5 Nd1 N12 59.48(17) . . ? N10 Nd1 N12 60.82(17) . . ? N1 Nd1 N12 114.90(17) . . ? O6 Nd1 N3 71.40(16) . . ? O4 Nd1 N3 69.08(17) . . ? O1 Nd1 N3 121.81(16) . . ? O2 Nd1 N3 60.30(16) . . ? N14 Nd1 N3 121.38(18) . . ? O5 Nd1 N3 112.39(17) . . ? N10 Nd1 N3 113.68(17) . . ? N1 Nd1 N3 66.43(18) . . ? N12 Nd1 N3 167.48(19) . . ? F3 P1 F3 91.0(5) 2_754 . ? F3 P1 F1 89.3(5) 2_754 . ? F3 P1 F1 91.7(5) . . ? F3 P1 F1 91.7(5) 2_754 2_754 ? F3 P1 F1 89.3(5) . 2_754 ? F1 P1 F1 178.6(9) . 2_754 ? F3 P1 F2 91.3(5) 2_754 2_754 ? F3 P1 F2 175.0(7) . 2_754 ? F1 P1 F2 92.7(7) . 2_754 ? F1 P1 F2 86.3(7) 2_754 2_754 ? F3 P1 F2 175.0(7) 2_754 . ? F3 P1 F2 91.3(5) . . ? F1 P1 F2 86.3(7) . . ? F1 P1 F2 92.7(7) 2_754 . ? F2 P1 F2 86.8(8) 2_754 . ? C49 Cl2 C49 66.2(14) 5_775 . ? C4 O1 Nd1 125.2(4) . . ? C12 O2 Nd1 127.0(4) . . ? C28 O4 Nd1 120.7(5) . . ? C36 O5 Nd1 122.6(5) . . ? C44 O6 Nd1 122.9(4) . . ? N2 N1 C1 105.4(5) . . ? N2 N1 Nd1 136.7(4) . . ? C1 N1 Nd1 117.6(4) . . ? C3 N2 N1 110.1(6) . . ? C3 N2 B1 125.3(6) . . ? N1 N2 B1 124.5(5) . . ? C9 N3 N4 106.8(5) . . ? C9 N3 Nd1 118.2(4) . . ? N4 N3 Nd1 133.9(4) . . ? C11 N4 N3 109.3(6) . . ? C11 N4 B1 126.1(7) . . ? N3 N4 B1 124.1(6) . . ? N6 N5 C17 102.7(13) . . ? N5 N6 C19 113.1(9) . . ? N5 N6 B1 117.5(9) . . ? C19 N6 B1 129.3(7) . . ? C4 N7 C8 118.5(6) . . ? C4 N7 C5 127.8(6) . . ? C8 N7 C5 113.6(6) . . ? C12 N8 C16 120.0(6) . . ? C12 N8 C13 128.2(7) . . ? C16 N8 C13 111.8(6) . . ? C20 N9 C24 126.2(16) . . ? C20 N9 C21 127.9(15) . . ? C24 N9 C21 105.9(9) . . ? C25 N10 N11 108.2(6) . . ? C25 N10 Nd1 119.2(5) . . ? N11 N10 Nd1 131.9(4) . . ? C27 N11 N10 107.9(7) . . ? C27 N11 B2 133.2(7) . . ? N10 N11 B2 118.6(6) . . ? N13 N12 C33 107.4(5) . . ? N13 N12 Nd1 131.7(4) . . ? C33 N12 Nd1 121.0(4) . . ? N12 N13 C35 109.9(6) . . ? N12 N13 B2 118.5(6) . . ? C35 N13 B2 130.7(6) . . ? C41 N14 N15 107.4(6) . . ? C41 N14 Nd1 120.1(4) . . ? N15 N14 Nd1 132.5(5) . . ? N14 N15 C43 108.4(7) . . ? N14 N15 B2 120.6(6) . . ? C43 N15 B2 130.7(7) . . ? C28 N16 C32 126.9(9) . . ? C28 N16 C29 119.6(8) . . ? C32 N16 C29 113.3(8) . . ? C36 N17 C37 129.4(9) . . ? C36 N17 C40 120.2(8) . . ? C37 N17 C40 110.3(8) . . ? C44 N18 C48 119.7(7) . . ? C44 N18 C45 126.6(7) . . ? C48 N18 C45 113.3(7) . . ? N1 C1 C2 110.1(6) . . ? N1 C1 C4 114.6(5) . . ? C2 C1 C4 135.3(7) . . ? C3 C2 C1 105.3(6) . . ? N2 C3 C2 109.0(6) . . ? O1 C4 N7 121.0(6) . . ? O1 C4 C1 119.4(6) . . ? N7 C4 C1 119.6(6) . . ? N7 C5 C6 100.1(7) . . ? C7 C6 C5 113.1(9) . . ? C6 C7 C8 109.2(9) . . ? N7 C8 C7 102.5(7) . . ? N3 C9 C10 109.1(6) . . ? N3 C9 C12 115.6(6) . . ? C10 C9 C12 135.3(7) . . ? C11 C10 C9 104.5(7) . . ? N4 C11 C10 110.3(7) . . ? O2 C12 N8 120.1(7) . . ? O2 C12 C9 118.1(6) . . ? N8 C12 C9 121.7(6) . . ? N8 C13 C14 104.1(7) . . ? C15 C14 C13 108.5(8) . . ? C14 C15 C16 112.6(9) . . ? N8 C16 C15 102.7(7) . . ? C18 C17 N5 111.2(11) . . ? C18 C17 C20 115(2) . . ? N5 C17 C20 134(2) . . ? C17 C18 C19 111.4(15) . . ? N6 C19 C18 101.4(12) . . ? N9 C20 C17 116(2) . . ? N9 C20 O3 122.5(18) . . ? C17 C20 O3 120(2) . . ? C22 C21 N9 97.3(11) . . ? C23 C22 C21 118.4(15) . . ? C24 C23 C22 101(2) . . ? C23 C24 N9 113.9(18) . . ? N10 C25 C26 109.6(8) . . ? N10 C25 C28 113.0(6) . . ? C26 C25 C28 137.4(7) . . ? C27 C26 C25 103.3(7) . . ? N11 C27 C26 111.0(8) . . ? O4 C28 N16 119.7(8) . . ? O4 C28 C25 118.2(6) . . ? N16 C28 C25 122.0(7) . . ? N16 C29 C30 102.5(11) . . ? C29 C30 C31 103.9(11) . . ? C30 C31 C32 104.8(11) . . ? N16 C32 C31 101.7(12) . . ? N12 C33 C34 109.6(6) . . ? N12 C33 C36 113.3(6) . . ? C34 C33 C36 136.9(7) . . ? C35 C34 C33 105.2(7) . . ? C34 C35 N13 107.8(7) . . ? O5 C36 N17 122.5(8) . . ? O5 C36 C33 117.7(6) . . ? N17 C36 C33 119.8(7) . . ? N17 C37 C38 104.0(14) . . ? C39 C38 C37 108.8(19) . . ? C38 C39 C40 105.8(13) . . ? C39 C40 N17 104.4(10) . . ? N14 C41 C42 110.2(7) . . ? N14 C41 C44 113.6(6) . . ? C42 C41 C44 136.1(7) . . ? C43 C42 C41 103.6(8) . . ? C42 C43 N15 110.3(7) . . ? O6 C44 N18 121.0(6) . . ? O6 C44 C41 118.2(7) . . ? N18 C44 C41 120.8(7) . . ? N18 C45 C46 100.3(8) . . ? C47 C46 C45 101.9(9) . . ? C48 C47 C46 104.0(9) . . ? N18 C48 C47 102.4(7) . . ? Cl2 C49 Cl1 121.8(15) 5_775 . ? Cl2 C49 Cl2 113.8(14) 5_775 . ? Cl1 C49 Cl2 124.0(17) . . ? Cl2 C49 C49 60.9(17) 5_775 5_775 ? Cl1 C49 C49 173(6) . 5_775 ? Cl2 C49 C49 52.9(10) . 5_775 ? Cl5 C50 Cl4 116.1(13) . . ? Cl5 C50 Cl3 103.1(13) . . ? Cl4 C50 Cl3 111.2(13) . . ? N4 B1 N2 111.8(6) . . ? N4 B1 N6 110.3(6) . . ? N2 B1 N6 109.5(7) . . ? N15 B2 N11 109.6(6) . . ? N15 B2 N13 109.0(6) . . ? N11 B2 N13 105.8(7) . . ? F5 P2 F9 97.5(18) . . ? F5 P2 F6 88.7(9) . . ? F9 P2 F6 172.8(17) . . ? F5 P2 F8 163.7(16) . . ? F9 P2 F8 77.6(12) . . ? F6 P2 F8 95.4(14) . . ? F5 P2 F4 85.7(11) . . ? F9 P2 F4 91.1(12) . . ? F6 P2 F4 85.8(13) . . ? F8 P2 F4 79.0(11) . . ? F5 P2 F7 116.1(18) . . ? F9 P2 F7 97.4(16) . . ? F6 P2 F7 83.0(14) . . ? F8 P2 F7 80.1(12) . . ? F4 P2 F7 155.1(14) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.467 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.173 data_trof88 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52.50 H72 B2 F6 N18 O8 P Sm' _chemical_formula_weight 1400.22 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 '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 25.7018(2) _cell_length_b 19.6629(2) _cell_length_c 25.5878(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.4362(8) _cell_angle_gamma 90.00 _cell_volume 12717.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5744 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7473 _exptl_absorpt_correction_T_max 0.9220 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi 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 25035 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10364 _reflns_number_gt 9219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0655P)^2^+341.9785P] 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 10364 _refine_ls_number_parameters 854 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.2119 _refine_ls_wR_factor_gt 0.2035 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 1.491 _refine_ls_shift/su_mean 0.040 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 Sm1 Sm 0.669220(16) 0.63614(2) 0.637178(18) 0.02470(16) Uani 1 1 d . . . O1 O 0.6766(3) 0.7036(3) 0.5568(3) 0.0387(16) Uani 1 1 d . . . O2 O 0.6761(2) 0.5424(3) 0.5683(3) 0.0382(16) Uani 1 1 d . . . O3 O 0.6230(3) 0.6485(4) 0.7138(3) 0.0383(16) Uani 1 1 d . . . O4 O 0.6618(2) 0.5228(3) 0.6778(3) 0.0361(16) Uani 1 1 d . . . O5 O 0.6734(2) 0.7580(3) 0.6685(3) 0.0371(16) Uani 1 1 d . . . O6 O 0.5467(5) 0.6919(14) 0.3244(5) 0.191(12) Uani 1 1 d . . . N1 N 0.7582(3) 0.6960(4) 0.6321(4) 0.038(2) Uani 1 1 d . . . N2 N 0.8061(3) 0.6934(4) 0.6644(4) 0.041(2) Uani 1 1 d . . . N3 N 0.6975(4) 0.8078(5) 0.5284(4) 0.049(2) Uani 1 1 d . . . N11 N 0.7568(3) 0.5610(4) 0.6436(3) 0.0339(18) Uani 1 1 d . . . N12 N 0.8054(3) 0.5682(4) 0.6741(3) 0.0374(19) Uani 1 1 d . . . N13 N 0.6984(4) 0.4358(5) 0.5520(5) 0.065(3) Uani 1 1 d . . . N21 N 0.7270(3) 0.6455(4) 0.7292(3) 0.0328(19) Uani 1 1 d . . . N22 N 0.7807(3) 0.6425(4) 0.7462(3) 0.0349(19) Uani 1 1 d . . . N23 N 0.6224(4) 0.6993(6) 0.7932(4) 0.064(3) Uani 1 1 d . . . N31 N 0.5796(3) 0.5678(4) 0.6086(3) 0.0279(17) Uani 1 1 d . . . N32 N 0.5314(3) 0.5816(4) 0.5776(3) 0.036(2) Uani 1 1 d . . . N33 N 0.6315(3) 0.4172(4) 0.6786(4) 0.051(3) Uani 1 1 d . . . N41 N 0.5849(3) 0.7181(4) 0.6064(3) 0.0285(17) Uani 1 1 d . . . N42 N 0.5361(3) 0.7105(4) 0.5760(3) 0.0311(17) Uani 1 1 d . . . N43 N 0.6515(3) 0.8697(4) 0.6644(3) 0.0375(19) Uani 1 1 d . . . N51 N 0.5179(3) 0.6879(5) 0.4550(4) 0.051(3) Uani 1 1 d . . . N52 N 0.5388(3) 0.6434(4) 0.4932(3) 0.040(2) Uani 1 1 d . . . N53 N 0.5119(11) 0.772(2) 0.3605(12) 0.20(2) Uani 1 1 d . . . B1 B 0.8177(4) 0.6362(6) 0.7055(5) 0.040(3) Uani 1 1 d . . . H0B H 0.8555 0.6375 0.7237 0.048 Uiso 1 1 calc R . . B2 B 0.5164(4) 0.6458(5) 0.5453(4) 0.026(2) Uani 1 1 d . . . H0A H 0.4769 0.6480 0.5359 0.032 Uiso 1 1 calc R . . C1 C 0.7588(4) 0.7471(5) 0.5983(4) 0.040(2) Uani 1 1 d . . . C2 C 0.8082(5) 0.7798(7) 0.6089(6) 0.065(4) Uani 1 1 d . . . H2A H 0.8193 0.8181 0.5910 0.078 Uiso 1 1 calc R . . C3 C 0.8363(5) 0.7452(7) 0.6497(6) 0.069(4) Uani 1 1 d . . . H3A H 0.8717 0.7551 0.6660 0.082 Uiso 1 1 calc R . . C4 C 0.7084(4) 0.7522(6) 0.5589(4) 0.041(2) Uani 1 1 d . . . C5 C 0.7292(6) 0.8712(6) 0.5287(6) 0.062(3) Uani 1 1 d . . . H5A H 0.7597 0.8647 0.5105 0.074 Uiso 1 1 calc R . . H5B H 0.7419 0.8879 0.5653 0.074 Uiso 1 1 calc R . . C6 C 0.6888(7) 0.9176(9) 0.4984(8) 0.103(6) Uani 1 1 d . . . H6A H 0.6707 0.9432 0.5232 0.124 Uiso 1 1 calc R . . H6B H 0.7060 0.9506 0.4778 0.124 Uiso 1 1 calc R . . C7 C 0.6506(8) 0.8766(10) 0.4625(7) 0.105(6) Uani 1 1 d . . . H7A H 0.6635 0.8670 0.4292 0.126 Uiso 1 1 calc R . . H7B H 0.6161 0.9004 0.4538 0.126 Uiso 1 1 calc R . . C8 C 0.6454(5) 0.8134(7) 0.4919(5) 0.064(4) Uani 1 1 d . . . H8A H 0.6391 0.7739 0.4676 0.077 Uiso 1 1 calc R . . H8B H 0.6160 0.8166 0.5121 0.077 Uiso 1 1 calc R . . C11 C 0.7579(4) 0.5042(5) 0.6161(4) 0.034(2) Uani 1 1 d . . . C12 C 0.8076(4) 0.4731(5) 0.6292(5) 0.045(3) Uani 1 1 d . . . H12A H 0.8186 0.4314 0.6160 0.054 Uiso 1 1 calc R . . C13 C 0.8370(4) 0.5162(6) 0.6653(5) 0.049(3) Uani 1 1 d . . . H13A H 0.8731 0.5105 0.6813 0.058 Uiso 1 1 calc R . . C14 C 0.7082(4) 0.4939(5) 0.5767(4) 0.037(2) Uani 1 1 d . . . C15 C 0.6480(6) 0.4246(8) 0.5140(7) 0.092(6) Uani 1 1 d . . . H15A H 0.6444 0.4570 0.4839 0.111 Uiso 1 1 calc R . . H15B H 0.6171 0.4293 0.5317 0.111 Uiso 1 1 calc R . . C16 C 0.6537(8) 0.3526(10) 0.4956(11) 0.151(11) Uani 1 1 d . . . H16A H 0.6258 0.3233 0.5058 0.181 Uiso 1 1 calc R . . H16B H 0.6506 0.3511 0.4565 0.181 Uiso 1 1 calc R . . C17 C 0.7008(14) 0.331(2) 0.519(3) 0.66(8) Uani 1 1 d . . . H17A H 0.7221 0.3239 0.4909 0.798 Uiso 1 1 calc R . . H17B H 0.6963 0.2867 0.5352 0.798 Uiso 1 1 calc R . . C18 C 0.7313(7) 0.3735(8) 0.5591(11) 0.140(11) Uani 1 1 d . . . H18A H 0.7674 0.3819 0.5520 0.169 Uiso 1 1 calc R . . H18B H 0.7337 0.3539 0.5950 0.169 Uiso 1 1 calc R . . C21 C 0.7057(4) 0.6572(6) 0.7719(4) 0.045(3) Uani 1 1 d . . . C22 C 0.7447(5) 0.6590(8) 0.8176(5) 0.067(4) Uani 1 1 d . . . H22A H 0.7400 0.6653 0.8533 0.081 Uiso 1 1 calc R . . C23 C 0.7911(4) 0.6495(5) 0.7996(4) 0.042(3) Uani 1 1 d . . . H23A H 0.8252 0.6482 0.8212 0.051 Uiso 1 1 calc R . . C24 C 0.6484(5) 0.6687(7) 0.7586(5) 0.054(3) Uani 1 1 d . . . C25 C 0.6440(7) 0.7344(12) 0.8454(6) 0.107(7) Uani 1 1 d . . . H25A H 0.6573 0.7006 0.8733 0.128 Uiso 1 1 calc R . . H25B H 0.6733 0.7655 0.8413 0.128 Uiso 1 1 calc R . . C26 C 0.5998(8) 0.7723(13) 0.8594(8) 0.124(8) Uani 1 1 d . . . H26A H 0.5985 0.8192 0.8451 0.149 Uiso 1 1 calc R . . H26B H 0.6020 0.7742 0.8984 0.149 Uiso 1 1 calc R . . C27 C 0.5508(8) 0.7297(12) 0.8321(7) 0.116(8) Uani 1 1 d . . . H27A H 0.5458 0.6893 0.8537 0.139 Uiso 1 1 calc R . . H27B H 0.5182 0.7575 0.8270 0.139 Uiso 1 1 calc R . . C28 C 0.5645(5) 0.7093(9) 0.7796(6) 0.079(5) Uani 1 1 d . . . H28A H 0.5462 0.6668 0.7661 0.094 Uiso 1 1 calc R . . H28B H 0.5553 0.7456 0.7527 0.094 Uiso 1 1 calc R . . C31 C 0.5768(4) 0.5042(5) 0.6272(4) 0.042(3) Uani 1 1 d . . . C32 C 0.5276(6) 0.4773(8) 0.6097(9) 0.147(11) Uani 1 1 d . . . H32A H 0.5150 0.4335 0.6172 0.177 Uiso 1 1 calc R . . C33 C 0.4999(5) 0.5284(7) 0.5786(8) 0.107(7) Uani 1 1 d . . . H33A H 0.4641 0.5256 0.5609 0.129 Uiso 1 1 calc R . . C34 C 0.6255(4) 0.4819(5) 0.6632(4) 0.036(2) Uani 1 1 d . . . C35 C 0.6816(4) 0.3940(6) 0.7137(6) 0.060(4) Uani 1 1 d . . . H35A H 0.7132 0.4091 0.6997 0.072 Uiso 1 1 calc R . . H35B H 0.6839 0.4112 0.7504 0.072 Uiso 1 1 calc R . . C36 C 0.6763(8) 0.3188(7) 0.7117(13) 0.203(17) Uani 1 1 d . . . H36A H 0.6990 0.2999 0.6878 0.244 Uiso 1 1 calc R . . H36B H 0.6883 0.2997 0.7476 0.244 Uiso 1 1 calc R . . C37 C 0.6226(6) 0.2996(8) 0.6928(9) 0.120(8) Uani 1 1 d . . . H37A H 0.6058 0.2857 0.7229 0.144 Uiso 1 1 calc R . . H37B H 0.6212 0.2607 0.6680 0.144 Uiso 1 1 calc R . . C38 C 0.5938(6) 0.3592(6) 0.6648(8) 0.095(6) Uani 1 1 d . . . H38A H 0.5603 0.3677 0.6776 0.114 Uiso 1 1 calc R . . H38B H 0.5858 0.3517 0.6259 0.114 Uiso 1 1 calc R . . C41 C 0.5896(4) 0.7847(5) 0.6195(4) 0.036(2) Uani 1 1 d . . . C42 C 0.5450(5) 0.8207(6) 0.5942(6) 0.064(4) Uani 1 1 d . . . H42A H 0.5389 0.8683 0.5954 0.076 Uiso 1 1 calc R . . C43 C 0.5124(4) 0.7725(5) 0.5676(5) 0.053(3) Uani 1 1 d . . . H43A H 0.4786 0.7807 0.5466 0.064 Uiso 1 1 calc R . . C44 C 0.6408(3) 0.8045(5) 0.6530(4) 0.031(2) Uani 1 1 d . . . C45 C 0.7039(4) 0.8877(5) 0.6963(5) 0.049(3) Uani 1 1 d . . . H45A H 0.7330 0.8689 0.6802 0.059 Uiso 1 1 calc R . . H45B H 0.7074 0.8706 0.7332 0.059 Uiso 1 1 calc R . . C46 C 0.7043(6) 0.9646(7) 0.6953(9) 0.108(7) Uani 1 1 d . . . H46A H 0.7165 0.9826 0.7316 0.130 Uiso 1 1 calc R . . H46B H 0.7287 0.9810 0.6722 0.130 Uiso 1 1 calc R . . C47 C 0.6523(7) 0.9872(7) 0.6754(11) 0.143(11) Uani 1 1 d . . . H47A H 0.6535 1.0251 0.6502 0.171 Uiso 1 1 calc R . . H47B H 0.6361 1.0045 0.7051 0.171 Uiso 1 1 calc R . . C48 C 0.6181(5) 0.9300(5) 0.6471(6) 0.062(4) Uani 1 1 d . . . H48A H 0.5836 0.9272 0.6590 0.074 Uiso 1 1 calc R . . H48B H 0.6120 0.9357 0.6081 0.074 Uiso 1 1 calc R . . C51 C 0.5456(5) 0.6763(9) 0.4157(5) 0.073(5) Uani 1 1 d . . . C52 C 0.5841(5) 0.6273(9) 0.4285(5) 0.073(5) Uani 1 1 d . . . H52A H 0.6087 0.6112 0.4077 0.088 Uiso 1 1 calc R . . C53 C 0.5786(4) 0.6076(6) 0.4782(5) 0.048(3) Uani 1 1 d . . . H53A H 0.5994 0.5741 0.4991 0.057 Uiso 1 1 calc R . . C54 C 0.5328(9) 0.716(2) 0.3651(8) 0.143(14) Uani 1 1 d . . . C55 C 0.5007(9) 0.8064(18) 0.3105(9) 0.26(3) Uani 1 1 d D . . H55A H 0.4793 0.7775 0.2830 0.317 Uiso 1 1 calc R . . H55B H 0.5336 0.8199 0.2984 0.317 Uiso 1 1 calc R . . C56 C 0.4689(13) 0.8695(15) 0.3230(10) 0.31(3) Uani 1 1 d D . . H56A H 0.4306 0.8593 0.3163 0.367 Uiso 1 1 calc R . . H56B H 0.4752 0.9082 0.3002 0.367 Uiso 1 1 calc R . . C57 C 0.4881(14) 0.8875(13) 0.3823(11) 0.27(3) Uani 1 1 d D . . H57A H 0.5213 0.9142 0.3880 0.329 Uiso 1 1 calc R . . H57B H 0.4607 0.9122 0.3976 0.329 Uiso 1 1 calc R . . C58 C 0.4967(11) 0.8145(14) 0.4046(14) 0.179(17) Uani 1 1 d . . . H58A H 0.5253 0.8138 0.4363 0.214 Uiso 1 1 calc R . . H58B H 0.4639 0.7968 0.4148 0.214 Uiso 1 1 calc R . . O7 O 0.5056(15) 0.3930(12) 0.7655(8) 0.122(11) Uani 0.50 1 d P . . O8 O 0.6361(13) 0.5556(14) 0.8689(11) 0.258(14) Uani 1 1 d D . . C65 C 0.6000(14) 0.5066(14) 0.7952(12) 0.177(12) Uani 1 1 d . . . H65A H 0.5793 0.5486 0.7949 0.265 Uiso 1 1 calc R . . H65B H 0.5767 0.4673 0.7959 0.265 Uiso 1 1 calc R . . H65C H 0.6159 0.5048 0.7632 0.265 Uiso 1 1 calc R . . C66 C 0.6425(11) 0.5056(11) 0.8432(10) 0.117(7) Uani 1 1 d D . . C67 C 0.6738(11) 0.4595(15) 0.8524(11) 0.168(12) Uani 1 1 d . . . H67A H 0.6995 0.4698 0.8846 0.252 Uiso 1 1 calc R . . H67B H 0.6924 0.4538 0.8224 0.252 Uiso 1 1 calc R . . H67C H 0.6550 0.4174 0.8577 0.252 Uiso 1 1 calc R . . O9 O 0.5416(18) 0.970(2) 0.4880(18) 0.22(2) Uani 0.50 1 d PD . . C68 C 0.480(3) 1.024(2) 0.4704(19) 0.130(18) Uani 0.50 1 d P . . C69 C 0.5392(15) 1.0156(19) 0.456(2) 0.36(7) Uani 0.50 1 d PD . . C70 C 0.5802(18) 1.071(3) 0.456(3) 0.39(9) Uani 0.50 1 d PD . . P1 P 0.5000 0.9343(3) 0.7500 0.110(3) Uani 1 2 d SD . . F1 F 0.4905(7) 0.9343(11) 0.6893(3) 0.219(9) Uani 1 1 d D . . F2 F 0.4573(4) 0.9884(7) 0.7497(5) 0.151(5) Uani 1 1 d D . . F3 F 0.4579(11) 0.8799(11) 0.7521(13) 0.37(2) Uani 1 1 d D . . P2 P 0.6568(4) 1.1410(5) 0.5319(3) 0.154(7) Uani 0.50 1 d PD . . F4 F 0.6518(7) 1.1971(8) 0.5693(5) 0.43(6) Uani 0.50 1 d PD . . F5 F 0.6583(9) 1.1912(7) 0.4890(5) 0.53(7) Uani 0.50 1 d PD . . F6 F 0.6617(7) 1.0849(7) 0.4945(5) 0.142(9) Uani 0.50 1 d PD . . F7 F 0.6552(8) 1.0908(9) 0.5748(6) 0.29(3) Uani 0.50 1 d PD . . F8 F 0.5984(4) 1.1376(11) 0.5168(7) 0.27(3) Uani 0.50 1 d PD . . F9 F 0.7152(4) 1.1445(10) 0.5469(7) 0.26(3) Uani 0.50 1 d PD . . 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 Sm1 0.0197(2) 0.0222(2) 0.0309(3) 0.0013(2) 0.00098(17) -0.00323(18) O1 0.035(3) 0.037(4) 0.043(4) 0.002(3) 0.005(3) -0.004(3) O2 0.034(3) 0.030(3) 0.047(4) -0.005(3) -0.002(3) 0.009(3) O3 0.034(3) 0.050(4) 0.030(4) 0.005(3) 0.006(3) 0.006(3) O4 0.029(3) 0.027(3) 0.048(4) 0.007(3) -0.005(3) -0.006(3) O5 0.030(3) 0.024(3) 0.052(4) -0.002(3) -0.005(3) 0.000(3) O6 0.090(9) 0.45(3) 0.030(7) 0.016(11) 0.008(6) -0.137(15) N1 0.028(4) 0.030(4) 0.053(5) 0.002(4) 0.001(4) -0.007(3) N2 0.028(4) 0.043(5) 0.050(5) 0.007(4) 0.005(4) -0.016(4) N3 0.061(6) 0.045(5) 0.046(6) 0.020(4) 0.022(5) -0.001(4) N11 0.027(4) 0.040(5) 0.035(5) -0.004(4) 0.004(3) -0.003(3) N12 0.023(4) 0.043(5) 0.044(5) 0.001(4) 0.000(3) 0.001(3) N13 0.038(5) 0.045(6) 0.103(9) -0.029(6) -0.011(5) 0.010(4) N21 0.025(4) 0.028(4) 0.041(5) 0.007(3) -0.005(3) 0.005(3) N22 0.029(4) 0.026(4) 0.046(5) -0.001(4) -0.003(4) 0.003(3) N23 0.057(6) 0.074(7) 0.059(7) -0.009(6) 0.007(5) 0.012(5) N31 0.023(3) 0.028(4) 0.031(4) 0.013(3) -0.001(3) -0.003(3) N32 0.026(4) 0.027(4) 0.050(5) 0.013(4) -0.008(4) -0.013(3) N33 0.040(5) 0.028(4) 0.073(7) 0.020(4) -0.018(4) -0.011(4) N41 0.024(4) 0.027(4) 0.032(4) 0.007(3) -0.003(3) -0.003(3) N42 0.026(4) 0.025(4) 0.039(5) -0.006(3) -0.002(3) -0.002(3) N43 0.039(4) 0.022(4) 0.049(5) -0.003(4) 0.001(4) -0.001(3) N51 0.035(4) 0.071(7) 0.040(6) 0.022(5) -0.009(4) -0.017(4) N52 0.038(4) 0.049(5) 0.030(5) 0.002(4) -0.004(4) -0.013(4) N53 0.114(18) 0.31(5) 0.13(2) 0.17(3) -0.060(18) -0.12(2) B1 0.024(5) 0.043(6) 0.049(7) -0.009(6) -0.002(5) -0.006(5) B2 0.024(5) 0.022(5) 0.032(6) 0.004(4) 0.000(4) -0.003(4) C1 0.042(5) 0.035(5) 0.045(6) 0.005(5) 0.014(5) -0.006(4) C2 0.049(7) 0.055(8) 0.091(11) 0.016(7) 0.011(7) -0.021(6) C3 0.038(6) 0.069(9) 0.095(11) 0.014(8) 0.001(7) -0.031(6) C4 0.043(6) 0.049(6) 0.033(6) 0.005(5) 0.016(5) 0.002(5) C5 0.081(9) 0.046(7) 0.067(9) 0.011(6) 0.036(7) 0.007(6) C6 0.110(14) 0.095(13) 0.107(14) 0.072(12) 0.026(12) 0.027(11) C7 0.116(15) 0.119(16) 0.076(12) 0.042(11) 0.008(11) 0.024(12) C8 0.061(8) 0.084(10) 0.049(7) 0.034(7) 0.013(6) 0.005(7) C11 0.034(5) 0.033(5) 0.036(6) 0.002(4) 0.005(4) 0.006(4) C12 0.040(5) 0.039(6) 0.055(7) -0.004(5) 0.005(5) 0.017(5) C13 0.031(5) 0.061(7) 0.054(7) 0.005(6) 0.006(5) 0.021(5) C14 0.040(5) 0.029(5) 0.044(6) -0.010(4) 0.014(5) 0.001(4) C15 0.059(8) 0.076(10) 0.126(14) -0.063(10) -0.022(9) 0.015(7) C16 0.086(13) 0.107(15) 0.24(3) -0.129(18) -0.012(15) 0.000(11) C17 0.20(3) 0.29(4) 1.30(17) -0.59(8) -0.41(7) 0.19(3) C18 0.073(11) 0.063(10) 0.25(3) -0.070(14) -0.054(14) 0.020(8) C21 0.041(6) 0.064(7) 0.032(6) 0.001(5) 0.008(5) 0.017(5) C22 0.051(7) 0.108(11) 0.038(7) 0.000(7) -0.004(6) 0.037(7) C23 0.046(6) 0.035(6) 0.037(6) -0.008(4) -0.016(5) 0.012(4) C24 0.045(6) 0.070(8) 0.045(7) -0.001(6) 0.004(5) 0.012(6) C25 0.074(10) 0.18(2) 0.057(10) -0.036(11) -0.008(8) 0.019(12) C26 0.105(14) 0.18(2) 0.084(13) -0.044(14) 0.004(11) 0.052(15) C27 0.100(13) 0.18(2) 0.068(11) -0.022(12) 0.016(10) 0.051(14) C28 0.056(8) 0.115(13) 0.065(9) -0.003(9) 0.012(7) 0.032(8) C31 0.028(5) 0.035(5) 0.057(7) 0.025(5) -0.010(5) -0.011(4) C32 0.073(10) 0.080(11) 0.24(2) 0.112(14) -0.092(13) -0.056(9) C33 0.055(8) 0.064(9) 0.175(18) 0.059(11) -0.054(10) -0.039(7) C34 0.029(5) 0.024(5) 0.053(6) 0.012(4) 0.000(4) -0.008(4) C35 0.043(6) 0.044(6) 0.083(9) 0.025(6) -0.017(6) -0.002(5) C36 0.118(15) 0.026(7) 0.40(4) 0.073(14) -0.14(2) -0.035(9) C37 0.078(11) 0.066(10) 0.19(2) 0.057(12) -0.041(12) -0.022(8) C38 0.078(9) 0.041(7) 0.143(15) 0.040(9) -0.044(10) -0.032(7) C41 0.027(5) 0.040(6) 0.039(6) -0.008(4) 0.001(4) 0.001(4) C42 0.053(7) 0.042(7) 0.090(10) -0.010(6) -0.002(7) 0.009(5) C43 0.042(6) 0.036(6) 0.072(8) -0.014(5) -0.014(6) 0.014(5) C44 0.026(4) 0.031(5) 0.035(5) -0.002(4) 0.006(4) -0.001(4) C45 0.038(6) 0.037(6) 0.066(8) -0.012(5) -0.010(5) 0.000(4) C46 0.065(9) 0.046(8) 0.19(2) -0.043(10) -0.040(11) 0.000(7) C47 0.094(12) 0.031(7) 0.26(3) -0.024(11) -0.069(15) 0.014(8) C48 0.050(7) 0.030(6) 0.093(10) -0.015(6) -0.016(6) 0.015(5) C51 0.053(8) 0.130(13) 0.033(7) 0.004(7) 0.002(6) -0.052(9) C52 0.041(7) 0.132(14) 0.049(8) -0.045(8) 0.014(6) -0.047(8) C53 0.030(5) 0.052(6) 0.060(8) -0.030(6) 0.006(5) -0.018(5) C54 0.071(12) 0.31(4) 0.043(12) 0.070(17) -0.020(9) -0.121(18) C55 0.12(2) 0.46(6) 0.17(3) 0.25(4) -0.079(18) -0.14(3) C56 0.21(3) 0.32(5) 0.31(5) 0.28(4) -0.17(3) -0.15(3) C57 0.23(4) 0.18(3) 0.35(5) 0.19(3) -0.14(4) -0.06(3) C58 0.12(2) 0.15(2) 0.22(3) 0.14(3) -0.09(2) -0.018(17) O7 0.19(3) 0.091(15) 0.066(19) 0.001(11) -0.03(2) -0.076(19) O8 0.38(4) 0.18(2) 0.21(3) -0.04(2) 0.04(2) 0.03(3) C65 0.25(4) 0.12(2) 0.17(3) -0.004(19) 0.05(3) 0.00(2) C66 0.15(2) 0.093(16) 0.117(19) 0.036(15) 0.034(17) -0.009(15) C67 0.17(3) 0.17(3) 0.18(3) 0.09(2) 0.05(2) 0.04(2) O9 0.18(4) 0.35(6) 0.15(4) -0.07(4) 0.09(3) -0.06(4) C68 0.15(5) 0.11(3) 0.12(3) 0.05(3) -0.01(3) 0.00(3) C69 0.45(10) 0.14(5) 0.34(9) -0.13(6) -0.33(8) 0.23(7) C70 0.42(10) 0.37(10) 0.52(13) 0.42(11) 0.44(11) 0.37(10) P1 0.149(7) 0.046(3) 0.162(8) 0.000 0.098(6) 0.000 F1 0.197(16) 0.30(3) 0.178(15) -0.112(16) 0.075(14) -0.049(17) F2 0.112(8) 0.171(12) 0.156(11) -0.055(10) -0.012(8) 0.053(8) F3 0.51(4) 0.20(2) 0.52(4) -0.20(3) 0.38(4) -0.24(3) P2 0.147(11) 0.252(18) 0.052(6) -0.028(8) -0.011(6) 0.125(12) F4 0.30(5) 0.78(13) 0.15(3) -0.27(6) -0.11(3) 0.32(7) F5 1.14(17) 0.16(3) 0.13(3) -0.08(2) -0.28(6) 0.36(7) F6 0.21(3) 0.103(17) 0.120(19) -0.020(14) 0.037(18) 0.047(18) F7 0.37(7) 0.33(7) 0.19(4) 0.06(4) 0.11(5) 0.02(6) F8 0.096(19) 0.57(9) 0.13(3) -0.09(4) -0.030(17) 0.05(3) F9 0.20(3) 0.49(8) 0.076(18) -0.03(3) 0.00(2) 0.10(4) _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 Sm1 O3 2.481(7) . ? Sm1 O4 2.482(6) . ? Sm1 O1 2.484(7) . ? Sm1 O5 2.523(6) . ? Sm1 N21 2.553(8) . ? Sm1 O2 2.579(7) . ? Sm1 N1 2.596(7) . ? Sm1 N31 2.651(7) . ? Sm1 N11 2.673(8) . ? Sm1 N41 2.701(7) . ? O1 C4 1.252(12) . ? O2 C14 1.255(11) . ? O3 C24 1.277(13) . ? O4 C34 1.237(11) . ? O5 C44 1.255(11) . ? O6 C54 1.25(4) . ? N1 C1 1.329(13) . ? N1 N2 1.354(11) . ? N2 C3 1.374(14) . ? N2 B1 1.532(15) . ? N3 C4 1.344(13) . ? N3 C5 1.487(15) . ? N3 C8 1.493(15) . ? N11 C11 1.323(12) . ? N11 N12 1.354(10) . ? N12 C13 1.350(13) . ? N12 B1 1.562(14) . ? N13 C14 1.307(13) . ? N13 C18 1.481(17) . ? N13 C15 1.488(15) . ? N21 C21 1.329(14) . ? N21 N22 1.372(10) . ? N22 C23 1.352(13) . ? N22 B1 1.535(15) . ? N23 C24 1.345(15) . ? N23 C28 1.478(16) . ? N23 C25 1.516(18) . ? N31 C31 1.346(11) . ? N31 N32 1.372(10) . ? N32 C33 1.326(14) . ? N32 B2 1.520(12) . ? N33 C34 1.333(12) . ? N33 C38 1.497(14) . ? N33 C35 1.501(13) . ? N41 C41 1.352(12) . ? N41 N42 1.358(10) . ? N42 C43 1.362(12) . ? N42 B2 1.534(12) . ? N43 C44 1.331(12) . ? N43 C48 1.486(12) . ? N43 C45 1.485(12) . ? N51 N52 1.350(12) . ? N51 C51 1.351(17) . ? N52 C53 1.354(14) . ? N52 B2 1.544(14) . ? N53 C54 1.22(5) . ? N53 C55 1.43(3) . ? N53 C58 1.51(5) . ? C1 C2 1.405(15) . ? C1 C4 1.494(14) . ? C2 C3 1.342(18) . ? C5 C6 1.491(19) . ? C6 C7 1.46(3) . ? C7 C8 1.47(2) . ? C11 C12 1.401(13) . ? C11 C14 1.491(13) . ? C12 C13 1.375(16) . ? C15 C16 1.51(2) . ? C16 C17 1.32(3) . ? C17 C18 1.44(3) . ? C21 C22 1.395(15) . ? C21 C24 1.466(15) . ? C22 C23 1.367(17) . ? C25 C26 1.46(2) . ? C26 C27 1.57(3) . ? C27 C28 1.51(2) . ? C31 C32 1.369(15) . ? C31 C34 1.480(13) . ? C32 C33 1.395(18) . ? C35 C36 1.485(18) . ? C36 C37 1.43(2) . ? C37 C38 1.497(19) . ? C41 C42 1.402(15) . ? C41 C44 1.486(12) . ? C42 C43 1.364(16) . ? C45 C46 1.511(17) . ? C46 C47 1.41(2) . ? C47 C48 1.525(18) . ? C51 C52 1.38(2) . ? C51 C54 1.50(2) . ? C52 C53 1.361(18) . ? C55 C56 1.5500(11) . ? C56 C57 1.5500(11) . ? C57 C58 1.55(3) . ? O7 O7 0.80(4) 2_656 ? O8 C66 1.2098(11) . ? C65 C66 1.49(3) . ? C66 C67 1.21(3) . ? O9 C69 1.213(4) . ? O9 C68 1.29(6) 5_676 ? C68 C69 1.64(9) . ? C68 O9 1.29(6) 5_676 ? C68 C68 1.92(9) 5_676 ? C69 C70 1.516(9) . ? P1 F3 1.527(8) 2_656 ? P1 F3 1.527(8) . ? P1 F2 1.528(8) 2_656 ? P1 F2 1.528(8) . ? P1 F1 1.528(8) . ? P1 F1 1.528(8) 2_656 ? P2 F6 1.482(6) . ? P2 F5 1.482(6) . ? P2 F9 1.482(6) . ? P2 F8 1.482(6) . ? P2 F7 1.482(6) . ? P2 F4 1.482(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sm1 O4 70.9(2) . . ? O3 Sm1 O1 136.1(2) . . ? O4 Sm1 O1 148.2(2) . . ? O3 Sm1 O5 69.8(2) . . ? O4 Sm1 O5 136.3(2) . . ? O1 Sm1 O5 75.5(2) . . ? O3 Sm1 N21 63.0(2) . . ? O4 Sm1 N21 75.8(2) . . ? O1 Sm1 N21 127.4(2) . . ? O5 Sm1 N21 69.8(2) . . ? O3 Sm1 O2 135.4(2) . . ? O4 Sm1 O2 70.4(2) . . ? O1 Sm1 O2 77.9(2) . . ? O5 Sm1 O2 153.1(2) . . ? N21 Sm1 O2 125.6(2) . . ? O3 Sm1 N1 123.2(3) . . ? O4 Sm1 N1 124.3(2) . . ? O1 Sm1 N1 61.1(2) . . ? O5 Sm1 N1 66.3(2) . . ? N21 Sm1 N1 69.1(3) . . ? O2 Sm1 N1 96.9(2) . . ? O3 Sm1 N31 75.6(2) . . ? O4 Sm1 N31 62.1(2) . . ? O1 Sm1 N31 103.5(2) . . ? O5 Sm1 N31 123.6(2) . . ? N21 Sm1 N31 128.5(2) . . ? O2 Sm1 N31 67.2(2) . . ? N1 Sm1 N31 160.8(3) . . ? O3 Sm1 N11 121.6(2) . . ? O4 Sm1 N11 66.8(2) . . ? O1 Sm1 N11 99.0(2) . . ? O5 Sm1 N11 121.2(2) . . ? N21 Sm1 N11 68.9(2) . . ? O2 Sm1 N11 59.1(2) . . ? N1 Sm1 N11 60.9(2) . . ? N31 Sm1 N11 114.6(2) . . ? O3 Sm1 N41 72.4(2) . . ? O4 Sm1 N41 122.6(2) . . ? O1 Sm1 N41 67.5(2) . . ? O5 Sm1 N41 60.8(2) . . ? N21 Sm1 N41 121.8(2) . . ? O2 Sm1 N41 112.2(2) . . ? N1 Sm1 N41 112.5(2) . . ? N31 Sm1 N41 67.1(2) . . ? N11 Sm1 N41 166.0(2) . . ? C4 O1 Sm1 121.2(6) . . ? C14 O2 Sm1 123.4(6) . . ? C24 O3 Sm1 120.0(7) . . ? C34 O4 Sm1 124.6(6) . . ? C44 O5 Sm1 127.2(6) . . ? C1 N1 N2 108.0(8) . . ? C1 N1 Sm1 119.3(6) . . ? N2 N1 Sm1 131.7(6) . . ? N1 N2 C3 107.5(9) . . ? N1 N2 B1 119.2(7) . . ? C3 N2 B1 133.2(9) . . ? C4 N3 C5 128.6(10) . . ? C4 N3 C8 119.5(9) . . ? C5 N3 C8 111.7(9) . . ? C11 N11 N12 106.8(8) . . ? C11 N11 Sm1 122.1(6) . . ? N12 N11 Sm1 131.0(6) . . ? C13 N12 N11 110.2(8) . . ? C13 N12 B1 131.4(8) . . ? N11 N12 B1 117.8(7) . . ? C14 N13 C18 127.3(10) . . ? C14 N13 C15 121.0(10) . . ? C18 N13 C15 111.6(10) . . ? C21 N21 N22 106.8(8) . . ? C21 N21 Sm1 121.0(6) . . ? N22 N21 Sm1 132.2(6) . . ? C23 N22 N21 108.5(8) . . ? C23 N22 B1 131.4(8) . . ? N21 N22 B1 120.0(8) . . ? C24 N23 C28 120.2(11) . . ? C24 N23 C25 129.5(11) . . ? C28 N23 C25 109.9(11) . . ? C31 N31 N32 106.6(7) . . ? C31 N31 Sm1 118.3(5) . . ? N32 N31 Sm1 135.1(5) . . ? C33 N32 N31 108.9(8) . . ? C33 N32 B2 124.7(8) . . ? N31 N32 B2 126.3(7) . . ? C34 N33 C38 128.5(9) . . ? C34 N33 C35 120.5(8) . . ? C38 N33 C35 111.0(8) . . ? C41 N41 N42 106.2(7) . . ? C41 N41 Sm1 118.3(5) . . ? N42 N41 Sm1 135.3(5) . . ? N41 N42 C43 109.5(7) . . ? N41 N42 B2 124.8(7) . . ? C43 N42 B2 124.3(8) . . ? C44 N43 C48 128.1(8) . . ? C44 N43 C45 118.8(8) . . ? C48 N43 C45 113.0(8) . . ? N52 N51 C51 103.6(11) . . ? N51 N52 C53 110.6(10) . . ? N51 N52 B2 116.3(9) . . ? C53 N52 B2 132.9(9) . . ? C54 N53 C55 122(4) . . ? C54 N53 C58 127(2) . . ? C55 N53 C58 111(4) . . ? N2 B1 N22 109.8(8) . . ? N2 B1 N12 106.2(8) . . ? N22 B1 N12 109.0(8) . . ? N32 B2 N42 112.4(7) . . ? N32 B2 N52 110.3(8) . . ? N42 B2 N52 109.1(7) . . ? N1 C1 C2 109.7(10) . . ? N1 C1 C4 112.2(9) . . ? C2 C1 C4 138.0(10) . . ? C3 C2 C1 105.0(10) . . ? C2 C3 N2 109.8(10) . . ? O1 C4 N3 122.0(10) . . ? O1 C4 C1 117.4(9) . . ? N3 C4 C1 120.6(10) . . ? N3 C5 C6 100.5(12) . . ? C7 C6 C5 108.4(16) . . ? C6 C7 C8 105.0(13) . . ? C7 C8 N3 103.1(12) . . ? N11 C11 C12 110.3(9) . . ? N11 C11 C14 112.2(8) . . ? C12 C11 C14 137.3(9) . . ? C13 C12 C11 105.0(9) . . ? N12 C13 C12 107.7(9) . . ? O2 C14 N13 121.1(9) . . ? O2 C14 C11 118.0(8) . . ? N13 C14 C11 120.9(9) . . ? N13 C15 C16 102.8(12) . . ? C17 C16 C15 106.7(15) . . ? C16 C17 C18 118.8(18) . . ? C17 C18 N13 99.4(16) . . ? N21 C21 C22 110.7(10) . . ? N21 C21 C24 112.4(9) . . ? C22 C21 C24 136.8(11) . . ? C23 C22 C21 104.6(11) . . ? N22 C23 C22 109.3(9) . . ? O3 C24 N23 119.7(10) . . ? O3 C24 C21 119.3(10) . . ? N23 C24 C21 120.9(11) . . ? C26 C25 N23 105.8(13) . . ? C25 C26 C27 102.5(16) . . ? C28 C27 C26 104.0(16) . . ? N23 C28 C27 102.2(12) . . ? N31 C31 C32 110.5(9) . . ? N31 C31 C34 113.7(8) . . ? C32 C31 C34 135.7(9) . . ? C31 C32 C33 104.7(10) . . ? N32 C33 C32 109.2(10) . . ? O4 C34 N33 119.3(8) . . ? O4 C34 C31 120.2(8) . . ? N33 C34 C31 120.4(8) . . ? C36 C35 N33 102.6(10) . . ? C37 C36 C35 110.6(14) . . ? C36 C37 C38 108.7(12) . . ? C37 C38 N33 103.8(10) . . ? N41 C41 C42 110.3(9) . . ? N41 C41 C44 115.3(8) . . ? C42 C41 C44 134.2(10) . . ? C43 C42 C41 104.8(10) . . ? N42 C43 C42 109.0(9) . . ? O5 C44 N43 122.1(8) . . ? O5 C44 C41 117.5(8) . . ? N43 C44 C41 120.4(8) . . ? N43 C45 C46 103.8(9) . . ? C47 C46 C45 108.1(11) . . ? C46 C47 C48 111.5(12) . . ? N43 C48 C47 101.2(9) . . ? N51 C51 C52 113.2(12) . . ? N51 C51 C54 119(2) . . ? C52 C51 C54 127(2) . . ? C53 C52 C51 103.2(11) . . ? N52 C53 C52 109.3(12) . . ? N53 C54 O6 117(3) . . ? N53 C54 C51 125(3) . . ? O6 C54 C51 118(4) . . ? N53 C55 C56 103(3) . . ? C55 C56 C57 107(2) . . ? C58 C57 C56 98(2) . . ? N53 C58 C57 106(3) . . ? C67 C66 O8 131(3) . . ? C67 C66 C65 122(3) . . ? O8 C66 C65 107(3) . . ? C69 O9 C68 121(5) . 5_676 ? C69 C68 O9 138(5) . 5_676 ? C69 C68 C68 75(4) . 5_676 ? O9 C68 C68 69(3) 5_676 5_676 ? C68 C69 O9 82(4) . . ? C68 C69 C70 127(4) . . ? O9 C69 C70 126(4) . . ? F3 P1 F3 91(2) 2_656 . ? F3 P1 F2 88.6(13) 2_656 2_656 ? F3 P1 F2 177.8(15) . 2_656 ? F3 P1 F2 177.8(15) 2_656 . ? F3 P1 F2 88.6(13) . . ? F2 P1 F2 91.6(12) 2_656 . ? F3 P1 F1 87.0(14) 2_656 . ? F3 P1 F1 93.0(14) . . ? F2 P1 F1 89.2(9) 2_656 . ? F2 P1 F1 90.7(9) . . ? F3 P1 F1 93.0(14) 2_656 2_656 ? F3 P1 F1 87.1(14) . 2_656 ? F2 P1 F1 90.7(9) 2_656 2_656 ? F2 P1 F1 89.2(9) . 2_656 ? F1 P1 F1 179.9(16) . 2_656 ? F6 P2 F5 90.00(6) . . ? F6 P2 F9 90.01(6) . . ? F5 P2 F9 90.01(7) . . ? F6 P2 F8 89.99(7) . . ? F5 P2 F8 89.99(7) . . ? F9 P2 F8 179.99(11) . . ? F6 P2 F7 90.00(6) . . ? F5 P2 F7 179.99(12) . . ? F9 P2 F7 90.01(6) . . ? F8 P2 F7 90.00(7) . . ? F6 P2 F4 179.99(11) . . ? F5 P2 F4 90.01(6) . . ? F9 P2 F4 90.00(7) . . ? F8 P2 F4 90.00(6) . . ? F7 P2 F4 90.00(6) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.273 _refine_diff_density_min -1.367 _refine_diff_density_rms 0.138