# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Ali Morsali' _publ_contact_author_email 'MORSALI A@YAHOO.COM' _publ_section_title ; Reversible single-crystal to single-crystal transformation of a hydrogen-bonded polymer to another in a solid-gas reaction ; loop_ _publ_author_name 'Ali Morsali' 'Somaye Khanjani' 'Pascal Retailleau' # Attachment 'S25_08mz328_0m-re-ic.cif' data_[La(4,4?-bipy)(H2O)2(NO3)4].(4,4?-Hbipy)(1) _database_code_depnum_ccdc_archive 'CCDC 712770' #TrackingRef 'S25_08mz328_0m-re-ic.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H12 La N6 O14, C10 H9 N2' _chemical_formula_sum 'C20 H21 La N8 O14' _chemical_formula_weight 736.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.2438(5) _cell_length_b 18.4781(12) _cell_length_c 19.8909(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2662.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 31.41 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.789 _exptl_absorpt_process_details 'Apex2 v2008.2-4 (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker AXS SMART APEX CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 23476 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 31.59 _reflns_number_total 8219 _reflns_number_gt 7934 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex2 v2008.2-4 (Bruker, 2008)' _computing_cell_refinement 'Apex2 v2008.2-4' _computing_data_reduction 'Apex2 v2008.2-4' _computing_structure_solution 'SHELXTL 6.14 (Bruker, 2000-2003)' _computing_structure_refinement 'SHELXTL 6.14' _computing_molecular_graphics 'SHELXTL 6.14' _computing_publication_material 'SHELXTL 6.14' _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^)+(0.0194P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3451 Friedel pairs' _refine_ls_abs_structure_Flack -0.002(7) _refine_ls_number_reflns 8219 _refine_ls_number_parameters 400 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0452 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2340(3) 0.30403(10) 0.89552(11) 0.0150(4) Uani 1 1 d . . . H1 H 0.1973 0.2881 0.9389 0.018 Uiso 1 1 calc R . . C2 C 0.2894(3) 0.25236(10) 0.84896(11) 0.0152(4) Uani 1 1 d . . . H2 H 0.2923 0.2027 0.8613 0.018 Uiso 1 1 calc R . . C3 C 0.3407(3) 0.27313(10) 0.78421(11) 0.0123(4) Uani 1 1 d . . . C4 C 0.3388(3) 0.34762(11) 0.77094(11) 0.0176(4) Uani 1 1 d . . . H4 H 0.3745 0.3652 0.7280 0.021 Uiso 1 1 calc R . . C5 C 0.2848(3) 0.39543(10) 0.82062(11) 0.0164(4) Uani 1 1 d . . . H5 H 0.2869 0.4456 0.8104 0.020 Uiso 1 1 calc R . . C6 C 0.4455(3) 0.09796(10) 0.69309(10) 0.0171(4) Uani 1 1 d . . . H6 H 0.4403 0.0475 0.7021 0.021 Uiso 1 1 calc R . . C7 C 0.3895(3) 0.14530(11) 0.74329(11) 0.0168(4) Uani 1 1 d . . . H7 H 0.3466 0.1271 0.7851 0.020 Uiso 1 1 calc R . . C8 C 0.3967(3) 0.21998(10) 0.73199(11) 0.0124(4) Uani 1 1 d . . . C9 C 0.4595(3) 0.24174(10) 0.66876(10) 0.0166(4) Uani 1 1 d . . . H9 H 0.4663 0.2918 0.6582 0.020 Uiso 1 1 calc R . . C10 C 0.5121(3) 0.19071(11) 0.62131(11) 0.0186(4) Uani 1 1 d . . . H10 H 0.5542 0.2072 0.5788 0.022 Uiso 1 1 calc R . . C11 C 0.8424(3) 0.14127(11) 0.78390(11) 0.0173(4) Uani 1 1 d . . . H11 H 0.8486 0.0902 0.7792 0.021 Uiso 1 1 calc R . . C12 C 0.8837(3) 0.18383(11) 0.72902(11) 0.0150(4) Uani 1 1 d . . . H12 H 0.9185 0.1621 0.6876 0.018 Uiso 1 1 calc R . . C13 C 0.8741(3) 0.25906(10) 0.73468(10) 0.0132(4) Uani 1 1 d . . . C14 C 0.8235(3) 0.28756(11) 0.79668(11) 0.0170(4) Uani 1 1 d . . . H14 H 0.8154 0.3384 0.8029 0.020 Uiso 1 1 calc R . . C15 C 0.7852(3) 0.24095(11) 0.84924(11) 0.0188(4) Uani 1 1 d . . . H15 H 0.7509 0.2612 0.8913 0.023 Uiso 1 1 calc R . . C16 C 1.0786(3) 0.32920(11) 0.57328(10) 0.0180(4) Uani 1 1 d . . . H16 H 1.1579 0.3132 0.5382 0.022 Uiso 1 1 calc R . . C17 C 1.0319(3) 0.28295(11) 0.62473(10) 0.0164(4) Uani 1 1 d . . . H17 H 1.0773 0.2347 0.6248 0.020 Uiso 1 1 calc R . . C18 C 0.9177(3) 0.30668(10) 0.67705(10) 0.0138(4) Uani 1 1 d . . . C19 C 0.8490(3) 0.37771(10) 0.67315(11) 0.0173(4) Uani 1 1 d . . . H19 H 0.7681 0.3954 0.7070 0.021 Uiso 1 1 calc R . . C20 C 0.8987(3) 0.42131(11) 0.62058(11) 0.0204(5) Uani 1 1 d . . . H20 H 0.8524 0.4693 0.6181 0.025 Uiso 1 1 calc R . . La1 La 0.060186(15) 0.472798(5) 0.972549(5) 0.01055(3) Uani 1 1 d . . . N1 N -0.0759(3) 0.62986(8) 0.98979(8) 0.0180(4) Uani 1 1 d . . . N2 N 0.0331(3) 0.49904(9) 1.12652(9) 0.0158(3) Uani 1 1 d . . . N3 N -0.2707(2) 0.36736(8) 0.98812(8) 0.0133(3) Uani 1 1 d . . . N4 N -0.0600(3) 0.49865(9) 0.82651(8) 0.0168(3) Uani 1 1 d . . . N5 N 0.2295(2) 0.37571(9) 0.88245(9) 0.0145(3) Uani 1 1 d . . . N6 N 0.5063(2) 0.11922(9) 0.63268(9) 0.0167(4) Uani 1 1 d . . . N7 N 0.7938(3) 0.16892(10) 0.84386(9) 0.0185(4) Uani 1 1 d . . . N8 N 1.0120(2) 0.39673(9) 0.57276(9) 0.0186(4) Uani 1 1 d . . . H8 H 1.0439 0.4259 0.5398 0.022 Uiso 1 1 calc R . . O1 O -0.1781(2) 0.57371(7) 0.98912(7) 0.0185(3) Uani 1 1 d . . . O2 O 0.09031(19) 0.62209(7) 0.97210(8) 0.0182(3) Uani 1 1 d . . . O3 O -0.1398(3) 0.68869(8) 1.00747(9) 0.0318(4) Uani 1 1 d . . . O4 O 0.1311(2) 0.53869(8) 1.08820(8) 0.0207(3) Uani 1 1 d . . . O5 O -0.0558(2) 0.44777(7) 1.09860(7) 0.0176(3) Uani 1 1 d . . . O6 O 0.0223(2) 0.51072(8) 1.18698(8) 0.0271(4) Uani 1 1 d . . . O7 O -0.2995(2) 0.43526(7) 0.99009(7) 0.0166(3) Uani 1 1 d . . . O8 O -0.10558(18) 0.34667(7) 0.98131(8) 0.0164(3) Uani 1 1 d . . . O9 O -0.3989(2) 0.32376(7) 0.99231(8) 0.0198(3) Uani 1 1 d . . . O10 O 0.0700(2) 0.53432(7) 0.85465(7) 0.0174(3) Uani 1 1 d . . . O11 O -0.1487(2) 0.45491(7) 0.86404(8) 0.0203(3) Uani 1 1 d . . . O12 O -0.0966(2) 0.50586(9) 0.76702(8) 0.0258(4) Uani 1 1 d . . . O13 O 0.39204(18) 0.52079(7) 0.95776(7) 0.0133(3) Uani 1 1 d D . . H13A H 0.478(3) 0.4929(11) 0.9565(12) 0.020 Uiso 1 1 d D . . H13B H 0.416(3) 0.5513(11) 0.9290(10) 0.020 Uiso 1 1 d D . . O14 O 0.2777(2) 0.39339(8) 1.03421(8) 0.0172(3) Uani 1 1 d D . . H14A H 0.370(3) 0.3750(13) 1.0213(13) 0.026 Uiso 1 1 d D . . H14B H 0.270(4) 0.3743(13) 1.0732(9) 0.026 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0160(10) 0.0165(9) 0.0126(10) 0.0006(7) 0.0012(8) 0.0000(7) C2 0.0181(10) 0.0121(8) 0.0154(11) 0.0009(8) 0.0007(8) 0.0019(7) C3 0.0101(9) 0.0137(8) 0.0132(10) 0.0000(7) -0.0004(7) -0.0008(7) C4 0.0202(11) 0.0169(9) 0.0155(11) 0.0031(8) 0.0021(9) 0.0011(8) C5 0.0174(11) 0.0125(8) 0.0193(11) 0.0010(8) 0.0032(8) 0.0010(7) C6 0.0200(10) 0.0134(8) 0.0178(10) -0.0024(7) 0.0005(10) 0.0004(8) C7 0.0196(11) 0.0151(9) 0.0158(11) 0.0006(8) 0.0023(8) 0.0002(7) C8 0.0106(10) 0.0146(8) 0.0121(10) -0.0020(7) -0.0007(7) -0.0014(7) C9 0.0203(11) 0.0160(8) 0.0135(10) -0.0007(7) 0.0004(9) 0.0008(8) C10 0.0217(11) 0.0208(9) 0.0133(10) 0.0001(8) 0.0013(8) -0.0004(8) C11 0.0165(10) 0.0170(9) 0.0185(11) 0.0010(8) -0.0011(8) -0.0022(8) C12 0.0141(10) 0.0176(9) 0.0134(10) -0.0008(7) 0.0009(7) 0.0004(7) C13 0.0106(9) 0.0156(8) 0.0135(10) 0.0003(7) -0.0001(7) -0.0018(7) C14 0.0165(10) 0.0176(9) 0.0168(11) -0.0053(8) -0.0009(9) 0.0003(8) C15 0.0182(11) 0.0242(10) 0.0140(11) -0.0036(9) 0.0006(8) -0.0042(8) C16 0.0176(11) 0.0227(9) 0.0137(10) 0.0005(7) -0.0019(9) -0.0039(8) C17 0.0149(11) 0.0186(9) 0.0157(10) 0.0016(7) -0.0004(8) -0.0017(7) C18 0.0129(10) 0.0150(8) 0.0135(10) 0.0006(7) -0.0029(8) -0.0008(7) C19 0.0171(11) 0.0159(9) 0.0190(11) -0.0010(8) 0.0006(8) -0.0002(8) C20 0.0196(11) 0.0168(9) 0.0249(12) 0.0042(8) -0.0033(8) -0.0016(8) La1 0.01026(4) 0.01001(4) 0.01138(5) -0.00004(4) 0.00012(4) 0.00014(4) N1 0.0264(10) 0.0114(7) 0.0162(9) 0.0004(6) 0.0014(8) 0.0013(7) N2 0.0186(9) 0.0145(7) 0.0143(9) -0.0009(6) 0.0021(7) 0.0034(7) N3 0.0139(8) 0.0123(7) 0.0138(9) -0.0005(6) 0.0004(6) 0.0003(6) N4 0.0183(8) 0.0150(7) 0.0172(9) -0.0026(6) -0.0046(8) 0.0038(8) N5 0.0145(9) 0.0140(7) 0.0151(9) -0.0002(6) -0.0002(7) 0.0003(6) N6 0.0158(9) 0.0184(8) 0.0160(9) -0.0047(7) -0.0006(7) 0.0017(6) N7 0.0180(10) 0.0240(9) 0.0136(9) 0.0042(7) -0.0018(7) -0.0035(7) N8 0.0202(10) 0.0209(8) 0.0146(9) 0.0067(7) -0.0044(7) -0.0069(7) O1 0.0162(7) 0.0118(6) 0.0275(9) -0.0023(6) 0.0022(6) -0.0008(6) O2 0.0172(7) 0.0188(6) 0.0187(7) -0.0007(6) 0.0017(7) -0.0022(5) O3 0.0401(11) 0.0109(6) 0.0446(12) -0.0069(6) 0.0140(8) 0.0029(7) O4 0.0248(8) 0.0215(8) 0.0158(8) 0.0010(6) 0.0025(6) -0.0084(6) O5 0.0184(7) 0.0164(6) 0.0181(7) -0.0024(5) 0.0017(7) -0.0037(6) O6 0.0425(11) 0.0253(8) 0.0134(8) -0.0041(6) 0.0052(7) -0.0042(7) O7 0.0158(7) 0.0102(6) 0.0238(9) 0.0004(5) -0.0007(6) 0.0008(5) O8 0.0107(7) 0.0148(6) 0.0235(9) -0.0007(6) 0.0023(6) 0.0015(5) O9 0.0142(8) 0.0142(6) 0.0308(9) 0.0002(6) 0.0032(6) -0.0022(5) O10 0.0212(7) 0.0144(6) 0.0166(7) 0.0001(5) -0.0045(6) -0.0014(7) O11 0.0205(8) 0.0188(7) 0.0217(8) 0.0019(6) -0.0025(6) -0.0045(6) O12 0.0298(10) 0.0341(8) 0.0135(8) -0.0012(6) -0.0065(6) 0.0006(7) O13 0.0132(6) 0.0120(6) 0.0146(7) 0.0021(5) 0.0020(5) 0.0009(5) O14 0.0137(7) 0.0233(7) 0.0147(8) 0.0055(6) 0.0023(6) 0.0068(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 C1 N5 1.350(2) . ? C1 C2 1.389(3) . ? C1 H1 0.9500 . ? C2 C3 1.394(3) . ? C2 H2 0.9500 . ? C3 C4 1.402(3) . ? C3 C8 1.486(3) . ? C4 C5 1.382(3) . ? C4 H4 0.9500 . ? C5 N5 1.344(3) . ? C5 H5 0.9500 . ? C6 N6 1.339(3) . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.399(3) . ? C7 H7 0.9500 . ? C8 C9 1.397(3) . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 N6 1.341(3) . ? C10 H10 0.9500 . ? C11 N7 1.344(3) . ? C11 C12 1.378(3) . ? C11 H11 0.9500 . ? C12 C13 1.396(3) . ? C12 H12 0.9500 . ? C13 C14 1.390(3) . ? C13 C18 1.479(3) . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 N7 1.337(3) . ? C15 H15 0.9500 . ? C16 N8 1.338(3) . ? C16 C17 1.376(3) . ? C16 H16 0.9500 . ? C17 C18 1.400(3) . ? C17 H17 0.9500 . ? C18 C19 1.406(3) . ? C19 C20 1.368(3) . ? C19 H19 0.9500 . ? C20 N8 1.336(3) . ? C20 H20 0.9500 . ? La1 O14 2.4779(14) . ? La1 O1 2.5621(14) . ? La1 O13 2.5791(14) . ? La1 O10 2.6071(14) . ? La1 O8 2.6275(13) . ? La1 O4 2.6530(15) . ? La1 O11 2.6565(16) . ? La1 O5 2.6843(14) . ? La1 O7 2.7190(15) . ? La1 O2 2.7673(13) . ? La1 N5 2.8167(17) . ? N1 O3 1.233(2) . ? N1 O2 1.262(2) . ? N1 O1 1.275(2) . ? N2 O6 1.224(2) . ? N2 O5 1.273(2) . ? N2 O4 1.274(2) . ? N3 O9 1.232(2) . ? N3 O8 1.263(2) . ? N3 O7 1.272(2) . ? N4 O12 1.220(2) . ? N4 O11 1.274(2) . ? N4 O10 1.279(2) . ? N8 H8 0.8800 . ? O13 H13A 0.809(16) . ? O13 H13B 0.822(16) . ? O14 H14A 0.795(16) . ? O14 H14B 0.853(16) . ? 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 N5 C1 C2 123.55(19) . . ? N5 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 120.25(18) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 116.21(18) . . ? C2 C3 C8 122.45(18) . . ? C4 C3 C8 121.34(19) . . ? C5 C4 C3 119.7(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N5 C5 C4 124.44(18) . . ? N5 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? N6 C6 C7 123.84(18) . . ? N6 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? C6 C7 C8 119.7(2) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 116.16(18) . . ? C9 C8 C3 121.88(17) . . ? C7 C8 C3 121.96(19) . . ? C10 C9 C8 120.42(18) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N6 C10 C9 123.1(2) . . ? N6 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N7 C11 C12 122.87(19) . . ? N7 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 119.56(19) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 117.50(18) . . ? C14 C13 C18 121.23(18) . . ? C12 C13 C18 121.27(18) . . ? C15 C14 C13 119.20(18) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N7 C15 C14 123.4(2) . . ? N7 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N8 C16 C17 119.8(2) . . ? N8 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.26(19) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 117.43(18) . . ? C17 C18 C13 121.05(17) . . ? C19 C18 C13 121.51(19) . . ? C20 C19 C18 119.9(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? N8 C20 C19 120.38(19) . . ? N8 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? O14 La1 O1 142.72(5) . . ? O14 La1 O13 70.57(5) . . ? O1 La1 O13 113.10(4) . . ? O14 La1 O10 133.33(5) . . ? O1 La1 O10 79.44(5) . . ? O13 La1 O10 73.87(5) . . ? O14 La1 O8 74.48(5) . . ? O1 La1 O8 109.22(5) . . ? O13 La1 O8 137.60(4) . . ? O10 La1 O8 117.31(5) . . ? O14 La1 O4 73.70(5) . . ? O1 La1 O4 71.64(5) . . ? O13 La1 O4 76.15(5) . . ? O10 La1 O4 125.07(4) . . ? O8 La1 O4 115.98(5) . . ? O14 La1 O11 133.68(5) . . ? O1 La1 O11 79.13(5) . . ? O13 La1 O11 118.75(5) . . ? O10 La1 O11 48.62(4) . . ? O8 La1 O11 71.53(5) . . ? O4 La1 O11 150.68(5) . . ? O14 La1 O5 68.57(5) . . ? O1 La1 O5 78.14(5) . . ? O13 La1 O5 117.22(5) . . ? O10 La1 O5 157.49(4) . . ? O8 La1 O5 69.04(5) . . ? O4 La1 O5 47.92(4) . . ? O11 La1 O5 124.00(5) . . ? O14 La1 O7 113.25(5) . . ? O1 La1 O7 61.55(4) . . ? O13 La1 O7 174.63(4) . . ? O10 La1 O7 104.64(5) . . ? O8 La1 O7 47.72(4) . . ? O4 La1 O7 101.04(4) . . ? O11 La1 O7 61.75(5) . . ? O5 La1 O7 62.38(5) . . ? O14 La1 O2 122.81(5) . . ? O1 La1 O2 47.78(4) . . ? O13 La1 O2 65.38(4) . . ? O10 La1 O2 63.92(4) . . ? O8 La1 O2 157.00(4) . . ? O4 La1 O2 61.97(5) . . ? O11 La1 O2 99.58(4) . . ? O5 La1 O2 101.50(4) . . ? O7 La1 O2 109.29(4) . . ? O14 La1 N5 70.18(5) . . ? O1 La1 N5 147.00(5) . . ? O13 La1 N5 74.97(5) . . ? O10 La1 N5 72.15(5) . . ? O8 La1 N5 71.11(5) . . ? O4 La1 N5 139.43(5) . . ? O11 La1 N5 69.62(5) . . ? O5 La1 N5 128.38(4) . . ? O7 La1 N5 109.66(5) . . ? O2 La1 N5 126.76(5) . . ? O3 N1 O2 122.54(18) . . ? O3 N1 O1 120.18(19) . . ? O2 N1 O1 117.28(15) . . ? O6 N2 O5 121.84(17) . . ? O6 N2 O4 121.47(18) . . ? O5 N2 O4 116.68(17) . . ? O9 N3 O8 121.52(15) . . ? O9 N3 O7 121.28(16) . . ? O8 N3 O7 117.20(16) . . ? O12 N4 O11 121.90(19) . . ? O12 N4 O10 121.87(18) . . ? O11 N4 O10 116.22(16) . . ? C5 N5 C1 115.78(17) . . ? C5 N5 La1 122.65(12) . . ? C1 N5 La1 120.84(13) . . ? C6 N6 C10 116.80(17) . . ? C15 N7 C11 117.49(18) . . ? C20 N8 C16 122.23(19) . . ? C20 N8 H8 118.9 . . ? C16 N8 H8 118.9 . . ? N1 O1 La1 101.69(12) . . ? N1 O2 La1 92.14(10) . . ? N2 O4 La1 98.45(11) . . ? N2 O5 La1 96.96(11) . . ? N3 O7 La1 95.18(11) . . ? N3 O8 La1 99.87(10) . . ? N4 O10 La1 98.57(11) . . ? N4 O11 La1 96.32(12) . . ? La1 O13 H13A 120.1(17) . . ? La1 O13 H13B 120.7(18) . . ? H13A O13 H13B 105(2) . . ? La1 O14 H14A 129(2) . . ? La1 O14 H14B 130.9(18) . . ? H14A O14 H14B 100(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C1 C2 C3 -1.3(3) . . . . ? C1 C2 C3 C4 2.2(3) . . . . ? C1 C2 C3 C8 -178.48(19) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? C8 C3 C4 C5 179.6(2) . . . . ? C3 C4 C5 N5 -1.0(3) . . . . ? N6 C6 C7 C8 -0.5(3) . . . . ? C6 C7 C8 C9 0.8(3) . . . . ? C6 C7 C8 C3 -179.2(2) . . . . ? C2 C3 C8 C9 -175.7(2) . . . . ? C4 C3 C8 C9 3.6(3) . . . . ? C2 C3 C8 C7 4.3(3) . . . . ? C4 C3 C8 C7 -176.4(2) . . . . ? C7 C8 C9 C10 -0.5(3) . . . . ? C3 C8 C9 C10 179.5(2) . . . . ? C8 C9 C10 N6 0.0(4) . . . . ? N7 C11 C12 C13 -0.5(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C11 C12 C13 C18 179.9(2) . . . . ? C12 C13 C14 C15 -0.1(3) . . . . ? C18 C13 C14 C15 -179.6(2) . . . . ? C13 C14 C15 N7 -0.1(4) . . . . ? N8 C16 C17 C18 -1.1(3) . . . . ? C16 C17 C18 C19 2.3(3) . . . . ? C16 C17 C18 C13 -176.65(19) . . . . ? C14 C13 C18 C17 155.5(2) . . . . ? C12 C13 C18 C17 -24.0(3) . . . . ? C14 C13 C18 C19 -23.4(3) . . . . ? C12 C13 C18 C19 157.1(2) . . . . ? C17 C18 C19 C20 -1.8(3) . . . . ? C13 C18 C19 C20 177.1(2) . . . . ? C18 C19 C20 N8 0.1(3) . . . . ? C4 C5 N5 C1 1.9(3) . . . . ? C4 C5 N5 La1 -168.39(17) . . . . ? C2 C1 N5 C5 -0.7(3) . . . . ? C2 C1 N5 La1 169.78(16) . . . . ? O14 La1 N5 C5 -140.01(17) . . . . ? O1 La1 N5 C5 43.8(2) . . . . ? O13 La1 N5 C5 -65.63(16) . . . . ? O10 La1 N5 C5 11.91(15) . . . . ? O8 La1 N5 C5 140.20(17) . . . . ? O4 La1 N5 C5 -111.61(16) . . . . ? O11 La1 N5 C5 63.50(15) . . . . ? O5 La1 N5 C5 -178.68(14) . . . . ? O7 La1 N5 C5 111.51(16) . . . . ? O2 La1 N5 C5 -23.29(18) . . . . ? O14 La1 N5 C1 50.13(15) . . . . ? O1 La1 N5 C1 -126.08(15) . . . . ? O13 La1 N5 C1 124.51(16) . . . . ? O10 La1 N5 C1 -157.95(16) . . . . ? O8 La1 N5 C1 -29.66(15) . . . . ? O4 La1 N5 C1 78.54(17) . . . . ? O11 La1 N5 C1 -106.36(16) . . . . ? O5 La1 N5 C1 11.47(18) . . . . ? O7 La1 N5 C1 -58.34(16) . . . . ? O2 La1 N5 C1 166.85(14) . . . . ? C7 C6 N6 C10 0.0(3) . . . . ? C9 C10 N6 C6 0.3(3) . . . . ? C14 C15 N7 C11 0.0(3) . . . . ? C12 C11 N7 C15 0.3(3) . . . . ? C19 C20 N8 C16 1.2(3) . . . . ? C17 C16 N8 C20 -0.7(3) . . . . ? O3 N1 O1 La1 -168.53(16) . . . . ? O2 N1 O1 La1 11.18(19) . . . . ? O14 La1 O1 N1 84.81(13) . . . . ? O13 La1 O1 N1 -3.08(12) . . . . ? O10 La1 O1 N1 -70.32(11) . . . . ? O8 La1 O1 N1 174.25(11) . . . . ? O4 La1 O1 N1 62.35(11) . . . . ? O11 La1 O1 N1 -119.86(11) . . . . ? O5 La1 O1 N1 111.66(11) . . . . ? O7 La1 O1 N1 176.51(12) . . . . ? O2 La1 O1 N1 -6.09(10) . . . . ? N5 La1 O1 N1 -101.07(13) . . . . ? O3 N1 O2 La1 169.57(17) . . . . ? O1 N1 O2 La1 -10.13(17) . . . . ? O14 La1 O2 N1 -127.87(11) . . . . ? O1 La1 O2 N1 6.03(10) . . . . ? O13 La1 O2 N1 -170.92(13) . . . . ? O10 La1 O2 N1 105.74(12) . . . . ? O8 La1 O2 N1 6.9(2) . . . . ? O4 La1 O2 N1 -84.04(12) . . . . ? O11 La1 O2 N1 71.74(12) . . . . ? O5 La1 O2 N1 -56.07(12) . . . . ? O7 La1 O2 N1 8.46(12) . . . . ? N5 La1 O2 N1 143.39(11) . . . . ? O6 N2 O4 La1 -179.10(16) . . . . ? O5 N2 O4 La1 -0.52(18) . . . . ? O14 La1 O4 N2 -75.29(12) . . . . ? O1 La1 O4 N2 90.75(12) . . . . ? O13 La1 O4 N2 -148.75(12) . . . . ? O10 La1 O4 N2 152.78(11) . . . . ? O8 La1 O4 N2 -12.20(13) . . . . ? O11 La1 O4 N2 86.32(14) . . . . ? O5 La1 O4 N2 0.29(10) . . . . ? O7 La1 O4 N2 35.93(12) . . . . ? O2 La1 O4 N2 142.04(13) . . . . ? N5 La1 O4 N2 -103.08(12) . . . . ? O6 N2 O5 La1 179.09(16) . . . . ? O4 N2 O5 La1 0.51(17) . . . . ? O14 La1 O5 N2 86.74(11) . . . . ? O1 La1 O5 N2 -76.17(11) . . . . ? O13 La1 O5 N2 33.88(12) . . . . ? O10 La1 O5 N2 -81.28(16) . . . . ? O8 La1 O5 N2 167.69(12) . . . . ? O4 La1 O5 N2 -0.29(10) . . . . ? O11 La1 O5 N2 -144.20(10) . . . . ? O7 La1 O5 N2 -140.09(12) . . . . ? O2 La1 O5 N2 -34.19(11) . . . . ? N5 La1 O5 N2 125.90(11) . . . . ? O9 N3 O7 La1 -178.04(16) . . . . ? O8 N3 O7 La1 1.55(18) . . . . ? O14 La1 O7 N3 -39.24(12) . . . . ? O1 La1 O7 N3 -178.01(12) . . . . ? O10 La1 O7 N3 112.90(11) . . . . ? O8 La1 O7 N3 -0.90(10) . . . . ? O4 La1 O7 N3 -116.10(11) . . . . ? O11 La1 O7 N3 89.25(11) . . . . ? O5 La1 O7 N3 -86.89(11) . . . . ? O2 La1 O7 N3 179.94(10) . . . . ? N5 La1 O7 N3 36.97(11) . . . . ? O9 N3 O8 La1 177.97(16) . . . . ? O7 N3 O8 La1 -1.62(18) . . . . ? O14 La1 O8 N3 144.65(13) . . . . ? O1 La1 O8 N3 3.60(13) . . . . ? O13 La1 O8 N3 179.96(10) . . . . ? O10 La1 O8 N3 -84.20(12) . . . . ? O4 La1 O8 N3 81.98(12) . . . . ? O11 La1 O8 N3 -67.32(12) . . . . ? O5 La1 O8 N3 72.08(12) . . . . ? O7 La1 O8 N3 0.91(10) . . . . ? O2 La1 O8 N3 2.9(2) . . . . ? N5 La1 O8 N3 -141.43(13) . . . . ? O12 N4 O10 La1 -174.37(16) . . . . ? O11 N4 O10 La1 5.30(17) . . . . ? O14 La1 O10 N4 112.70(11) . . . . ? O1 La1 O10 N4 -87.79(11) . . . . ? O13 La1 O10 N4 154.22(11) . . . . ? O8 La1 O10 N4 18.50(12) . . . . ? O4 La1 O10 N4 -146.29(10) . . . . ? O11 La1 O10 N4 -3.04(10) . . . . ? O5 La1 O10 N4 -82.71(15) . . . . ? O7 La1 O10 N4 -31.13(11) . . . . ? O2 La1 O10 N4 -135.74(12) . . . . ? N5 La1 O10 N4 75.20(11) . . . . ? O12 N4 O11 La1 174.50(16) . . . . ? O10 N4 O11 La1 -5.18(17) . . . . ? O14 La1 O11 N4 -112.00(11) . . . . ? O1 La1 O11 N4 88.47(11) . . . . ? O13 La1 O11 N4 -22.04(12) . . . . ? O10 La1 O11 N4 3.03(10) . . . . ? O8 La1 O11 N4 -156.85(12) . . . . ? O4 La1 O11 N4 92.75(14) . . . . ? O5 La1 O11 N4 156.01(10) . . . . ? O7 La1 O11 N4 151.88(12) . . . . ? O2 La1 O11 N4 45.05(11) . . . . ? N5 La1 O11 N4 -80.74(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H14B N7 0.853(16) 1.842(17) 2.687(2) 171(3) 4_457 O14 H14A N3 0.795(16) 2.686(18) 3.431(2) 157(2) 1_655 O14 H14A O9 0.795(16) 2.006(17) 2.800(2) 177(3) 1_655 O13 H13B N6 0.822(16) 1.843(16) 2.662(2) 174(3) 3_656 O13 H13A O7 0.809(16) 2.043(17) 2.8111(19) 158(2) 1_655 N8 H8 O13 0.88 1.96 2.835(2) 171.7 2_664 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.866 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.085 # Attachment '15s27_final-re-icc.cif' data_[La(4,4?-Hbipy)(NO3)5].(4,4?-Hbipy)(2) _database_code_depnum_ccdc_archive 'CCDC 719349' #TrackingRef '15s27_final-re-icc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H9 La N7 O15, C10 H9 N2' _chemical_formula_sum 'C20 H18 La N9 O15' _chemical_formula_weight 763.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -.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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.245(2) _cell_length_b 18.322(3) _cell_length_c 13.475(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.161(5) _cell_angle_gamma 90.00 _cell_volume 2703.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5731 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa-CCD diffractometer' _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 10882 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5538 _reflns_number_gt 4001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0264P)^2^+0.8520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5538 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.332620(18) 0.467796(10) 0.726362(16) 0.03094(8) Uani 1 1 d . . . N6 N 0.3690(3) 0.59749(15) 0.6324(2) 0.0381(7) Uani 1 1 d . . . N7 N 0.4374(3) 0.92748(16) 0.3871(3) 0.0482(9) Uani 1 1 d . . . H7N H 0.4429 0.9670 0.3540 0.058 Uiso 1 1 calc R . . N8 N 0.4540(3) 0.79278(17) 1.0065(2) 0.0425(8) Uani 1 1 d . . . H8N H 0.4113 0.8004 1.0509 0.051 Uiso 1 1 calc R . . N9 N 0.8029(3) 0.72270(17) 0.6443(3) 0.0452(8) Uani 1 1 d . . . C1 C 0.3247(4) 0.65986(19) 0.6598(3) 0.0432(10) Uani 1 1 d . . . H1 H 0.2809 0.6584 0.7105 0.052 Uiso 1 1 calc R . . C2 C 0.3402(3) 0.72663(18) 0.6169(3) 0.0391(9) Uani 1 1 d . . . H2 H 0.3084 0.7687 0.6395 0.047 Uiso 1 1 calc R . . C3 C 0.4029(3) 0.73074(17) 0.5406(3) 0.0318(8) Uani 1 1 d . . . C4 C 0.4489(3) 0.66608(18) 0.5107(3) 0.0426(10) Uani 1 1 d . . . H4 H 0.4918 0.6660 0.4593 0.051 Uiso 1 1 calc R . . C5 C 0.4298(4) 0.60228(19) 0.5583(3) 0.0443(10) Uani 1 1 d . . . H5 H 0.4615 0.5595 0.5375 0.053 Uiso 1 1 calc R . . C6 C 0.4177(3) 0.80079(17) 0.4891(3) 0.0333(8) Uani 1 1 d . . . C7 C 0.5075(4) 0.8097(2) 0.4346(3) 0.0467(10) Uani 1 1 d . . . H7 H 0.5627 0.7722 0.4328 0.056 Uiso 1 1 calc R . . C8 C 0.5153(4) 0.8734(2) 0.3833(3) 0.0552(12) Uani 1 1 d . . . H8 H 0.5749 0.8788 0.3460 0.066 Uiso 1 1 calc R . . C9 C 0.3516(4) 0.9225(2) 0.4400(3) 0.0462(10) Uani 1 1 d . . . H9 H 0.2997 0.9618 0.4420 0.055 Uiso 1 1 calc R . . C10 C 0.3396(3) 0.85949(18) 0.4918(3) 0.0393(9) Uani 1 1 d . . . H10 H 0.2793 0.8559 0.5286 0.047 Uiso 1 1 calc R . . C11 C 0.4481(4) 0.7287(2) 0.9610(3) 0.0542(12) Uani 1 1 d . . . H11 H 0.3970 0.6927 0.9765 0.065 Uiso 1 1 calc R . . C12 C 0.5160(4) 0.7147(2) 0.8915(3) 0.0493(11) Uani 1 1 d . . . H12 H 0.5118 0.6689 0.8611 0.059 Uiso 1 1 calc R . . C13 C 0.5914(3) 0.76772(18) 0.8654(3) 0.0322(8) Uani 1 1 d . . . C14 C 0.5935(3) 0.83472(19) 0.9142(3) 0.0362(9) Uani 1 1 d . . . H14 H 0.6419 0.8723 0.8987 0.043 Uiso 1 1 calc R . . C15 C 0.5250(3) 0.8460(2) 0.9849(3) 0.0410(9) Uani 1 1 d . . . H15 H 0.5279 0.8908 1.0177 0.049 Uiso 1 1 calc R . . C16 C 0.6645(3) 0.75304(18) 0.7886(3) 0.0310(8) Uani 1 1 d . . . C17 C 0.6730(3) 0.6834(2) 0.7509(3) 0.0428(10) Uani 1 1 d . . . H17 H 0.6314 0.6450 0.7730 0.051 Uiso 1 1 calc R . . C18 C 0.7422(4) 0.6708(2) 0.6812(3) 0.0480(10) Uani 1 1 d . . . H18 H 0.7471 0.6232 0.6583 0.058 Uiso 1 1 calc R . . C19 C 0.7945(4) 0.7896(2) 0.6801(3) 0.0530(11) Uani 1 1 d . . . H19 H 0.8365 0.8270 0.6562 0.064 Uiso 1 1 calc R . . C20 C 0.7274(3) 0.8071(2) 0.7506(3) 0.0436(10) Uani 1 1 d . . . H20 H 0.7245 0.8551 0.7724 0.052 Uiso 1 1 calc R . . O7 O 0.3391(2) 0.57834(12) 0.8539(2) 0.0442(7) Uani 1 1 d . . . O4 O 0.1419(2) 0.39066(13) 0.7525(2) 0.0445(7) Uani 1 1 d . . . O10 O 0.4059(3) 0.34741(14) 0.8260(2) 0.0512(7) Uani 1 1 d . . . O11 O 0.3377(3) 0.33035(13) 0.6650(2) 0.0483(7) Uani 1 1 d . . . O1 O 0.3070(3) 0.44765(14) 0.5277(2) 0.0507(7) Uani 1 1 d . . . O5 O 0.1201(2) 0.50644(14) 0.7720(2) 0.0487(7) Uani 1 1 d . . . O2 O 0.1531(2) 0.49492(16) 0.5744(2) 0.0549(7) Uani 1 1 d . . . O9 O 0.3399(3) 0.47218(13) 0.9233(2) 0.0484(7) Uani 1 1 d . . . O3 O 0.1417(3) 0.47475(19) 0.4143(2) 0.0765(10) Uani 1 1 d . . . O8 O 0.3066(3) 0.56961(15) 1.0060(2) 0.0640(9) Uani 1 1 d . . . N2 N 0.0799(3) 0.44231(17) 0.7763(2) 0.0392(7) Uani 1 1 d . . . N1 N 0.1999(3) 0.47207(17) 0.5025(3) 0.0443(8) Uani 1 1 d . . . N3 N 0.3286(3) 0.54062(16) 0.9301(2) 0.0422(8) Uani 1 1 d . . . N4 N 0.3796(3) 0.30353(16) 0.7519(3) 0.0446(9) Uani 1 1 d . . . O6 O -0.0155(2) 0.43232(16) 0.8044(2) 0.0578(8) Uani 1 1 d . . . O12 O 0.3954(3) 0.23797(14) 0.7652(3) 0.0637(9) Uani 1 1 d . . . O14 O 0.5396(2) 0.43879(15) 0.6826(2) 0.0538(8) Uani 1 1 d . . . O13 O 0.5525(2) 0.51840(13) 0.8017(2) 0.0496(7) Uani 1 1 d . . . O15 O 0.7154(3) 0.48498(15) 0.7540(3) 0.0646(9) Uani 1 1 d . . . N5 N 0.6059(3) 0.48095(16) 0.7466(3) 0.0416(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.03696(12) 0.02349(11) 0.03655(13) -0.00247(10) 0.01707(9) -0.00096(9) N6 0.0495(19) 0.0300(16) 0.0391(19) 0.0023(14) 0.0188(16) -0.0008(14) N7 0.070(2) 0.0286(17) 0.052(2) 0.0088(15) 0.027(2) 0.0012(15) N8 0.0441(19) 0.0490(19) 0.042(2) -0.0067(16) 0.0248(17) -0.0025(15) N9 0.048(2) 0.050(2) 0.045(2) 0.0006(16) 0.0249(17) -0.0006(16) C1 0.056(3) 0.034(2) 0.046(2) 0.0052(18) 0.026(2) 0.0042(18) C2 0.052(2) 0.0293(19) 0.041(2) 0.0023(16) 0.021(2) 0.0078(16) C3 0.039(2) 0.0275(18) 0.030(2) -0.0008(15) 0.0105(17) -0.0001(15) C4 0.058(3) 0.034(2) 0.046(2) 0.0011(17) 0.033(2) 0.0012(17) C5 0.063(3) 0.030(2) 0.048(3) -0.0006(17) 0.029(2) 0.0041(18) C6 0.039(2) 0.0290(18) 0.034(2) -0.0001(15) 0.0137(18) -0.0005(15) C7 0.052(2) 0.033(2) 0.063(3) 0.0058(19) 0.030(2) 0.0036(17) C8 0.071(3) 0.040(2) 0.067(3) 0.010(2) 0.043(3) 0.001(2) C9 0.060(3) 0.038(2) 0.044(3) 0.0005(18) 0.020(2) 0.0076(18) C10 0.049(2) 0.037(2) 0.038(2) 0.0036(17) 0.0215(19) 0.0027(17) C11 0.063(3) 0.051(3) 0.060(3) -0.013(2) 0.038(2) -0.021(2) C12 0.066(3) 0.043(2) 0.051(3) -0.0191(19) 0.038(2) -0.0193(19) C13 0.0312(19) 0.036(2) 0.031(2) 0.0023(16) 0.0097(17) -0.0042(15) C14 0.036(2) 0.035(2) 0.042(2) 0.0002(17) 0.0158(18) -0.0034(15) C15 0.043(2) 0.040(2) 0.043(2) -0.0067(18) 0.016(2) 0.0020(17) C16 0.0292(19) 0.0351(19) 0.030(2) 0.0033(15) 0.0096(17) -0.0020(15) C17 0.050(2) 0.039(2) 0.048(3) -0.0062(18) 0.029(2) -0.0068(17) C18 0.056(3) 0.043(2) 0.050(3) -0.0116(19) 0.024(2) -0.0044(19) C19 0.060(3) 0.047(3) 0.066(3) 0.007(2) 0.042(2) -0.002(2) C20 0.053(3) 0.035(2) 0.049(3) 0.0022(18) 0.027(2) 0.0004(17) O7 0.0663(18) 0.0279(13) 0.0443(17) -0.0024(12) 0.0248(15) -0.0095(12) O4 0.0443(16) 0.0312(14) 0.063(2) -0.0072(12) 0.0217(14) 0.0012(11) O10 0.0649(19) 0.0366(15) 0.0514(19) -0.0015(14) 0.0121(16) 0.0104(13) O11 0.0637(19) 0.0349(15) 0.0495(19) -0.0053(14) 0.0197(16) 0.0009(13) O1 0.0529(18) 0.0519(16) 0.0478(18) -0.0079(13) 0.0125(15) 0.0131(13) O5 0.0484(16) 0.0399(16) 0.064(2) -0.0138(13) 0.0248(15) -0.0021(12) O2 0.0470(17) 0.0748(19) 0.0469(18) -0.0038(15) 0.0194(15) 0.0052(14) O9 0.0779(19) 0.0270(14) 0.0474(17) 0.0013(12) 0.0291(15) -0.0018(12) O3 0.074(2) 0.114(3) 0.037(2) 0.0001(19) 0.0062(18) 0.021(2) O8 0.111(3) 0.0488(17) 0.0449(18) -0.0131(14) 0.0438(18) -0.0059(16) N2 0.0369(18) 0.0442(19) 0.0382(19) -0.0073(15) 0.0121(16) -0.0013(15) N1 0.050(2) 0.0444(19) 0.038(2) -0.0014(16) 0.0106(18) -0.0029(16) N3 0.057(2) 0.0355(19) 0.039(2) -0.0020(16) 0.0203(17) -0.0082(15) N4 0.0440(19) 0.0296(19) 0.069(3) -0.0003(18) 0.0312(19) 0.0025(14) O6 0.0352(15) 0.077(2) 0.070(2) -0.0068(16) 0.0305(16) -0.0052(14) O12 0.085(2) 0.0242(15) 0.093(3) 0.0056(15) 0.043(2) 0.0080(13) O14 0.0444(16) 0.0538(16) 0.066(2) -0.0270(15) 0.0183(15) -0.0089(13) O13 0.0467(16) 0.0463(16) 0.0587(19) -0.0156(14) 0.0181(15) -0.0019(12) O15 0.0363(17) 0.066(2) 0.094(3) -0.0144(17) 0.0196(17) -0.0076(14) N5 0.0372(19) 0.0376(19) 0.053(2) 0.0048(16) 0.0173(17) -0.0023(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 O2 2.575(3) . ? La1 O14 2.584(3) . ? La1 O10 2.616(3) . ? La1 O13 2.619(3) . ? La1 O9 2.637(3) . ? La1 O7 2.647(2) . ? La1 O1 2.652(3) . ? La1 O11 2.655(2) . ? La1 O4 2.658(2) . ? La1 O5 2.694(3) . ? La1 N6 2.766(3) . ? La1 N5 3.032(3) . ? N6 C1 1.332(4) . ? N6 C5 1.336(4) . ? N7 C9 1.327(5) . ? N7 C8 1.331(5) . ? N7 H7N 0.8600 . ? N8 C11 1.320(5) . ? N8 C15 1.334(4) . ? N8 H8N 0.8600 . ? N9 C19 1.329(5) . ? N9 C18 1.332(5) . ? C1 C2 1.381(5) . ? C1 H1 0.9300 . ? C2 C3 1.374(5) . ? C2 H2 0.9300 . ? C3 C4 1.388(4) . ? C3 C6 1.486(5) . ? C4 C5 1.373(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.388(5) . ? C6 C10 1.394(5) . ? C7 C8 1.368(5) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.372(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.360(5) . ? C11 H11 0.9300 . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C13 C14 1.390(5) . ? C13 C16 1.486(4) . ? C14 C15 1.370(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C20 1.382(5) . ? C16 C17 1.385(5) . ? C17 C18 1.369(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.378(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? O7 N3 1.265(4) . ? O4 N2 1.260(3) . ? O10 N4 1.263(4) . ? O11 N4 1.259(4) . ? O1 N1 1.257(4) . ? O5 N2 1.265(4) . ? O2 N1 1.273(4) . ? O9 N3 1.266(3) . ? O3 N1 1.221(4) . ? O8 N3 1.226(4) . ? N2 O6 1.230(4) . ? N4 O12 1.222(4) . ? O14 N5 1.266(4) . ? O13 N5 1.260(4) . ? O15 N5 1.215(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O14 116.22(9) . . ? O2 La1 O10 132.00(9) . . ? O14 La1 O10 75.45(9) . . ? O2 La1 O13 137.69(9) . . ? O14 La1 O13 48.79(8) . . ? O10 La1 O13 86.58(9) . . ? O2 La1 O9 129.31(9) . . ? O14 La1 O9 114.38(9) . . ? O10 La1 O9 64.87(8) . . ? O13 La1 O9 77.82(9) . . ? O2 La1 O7 105.63(9) . . ? O14 La1 O7 114.38(8) . . ? O10 La1 O7 110.67(8) . . ? O13 La1 O7 66.02(8) . . ? O9 La1 O7 48.18(7) . . ? O2 La1 O1 48.61(8) . . ? O14 La1 O1 68.74(9) . . ? O10 La1 O1 110.47(8) . . ? O13 La1 O1 108.45(9) . . ? O9 La1 O1 172.36(8) . . ? O7 La1 O1 137.96(8) . . ? O2 La1 O11 90.22(9) . . ? O14 La1 O11 69.47(8) . . ? O10 La1 O11 48.21(9) . . ? O13 La1 O11 111.78(8) . . ? O9 La1 O11 110.15(8) . . ? O7 La1 O11 158.23(9) . . ? O1 La1 O11 63.80(9) . . ? O2 La1 O4 72.42(9) . . ? O14 La1 O4 135.81(8) . . ? O10 La1 O4 69.71(8) . . ? O13 La1 O4 148.86(8) . . ? O9 La1 O4 73.99(8) . . ? O7 La1 O4 102.97(7) . . ? O1 La1 O4 98.86(8) . . ? O11 La1 O4 67.19(8) . . ? O2 La1 O5 63.61(9) . . ? O14 La1 O5 176.63(8) . . ? O10 La1 O5 107.26(9) . . ? O13 La1 O5 128.80(8) . . ? O9 La1 O5 65.70(9) . . ? O7 La1 O5 62.96(8) . . ? O1 La1 O5 111.63(9) . . ? O11 La1 O5 113.80(8) . . ? O4 La1 O5 47.56(7) . . ? O2 La1 N6 68.95(9) . . ? O14 La1 N6 80.64(9) . . ? O10 La1 N6 153.78(9) . . ? O13 La1 N6 69.42(9) . . ? O9 La1 N6 117.42(8) . . ? O7 La1 N6 69.82(8) . . ? O1 La1 N6 69.57(9) . . ? O11 La1 N6 131.00(9) . . ? O4 La1 N6 136.48(8) . . ? O5 La1 N6 96.31(8) . . ? O2 La1 N5 130.60(9) . . ? O14 La1 N5 24.42(8) . . ? O10 La1 N5 80.01(8) . . ? O13 La1 N5 24.38(8) . . ? O9 La1 N5 96.23(9) . . ? O7 La1 N5 90.20(8) . . ? O1 La1 N5 88.66(9) . . ? O11 La1 N5 90.57(8) . . ? O4 La1 N5 149.56(8) . . ? O5 La1 N5 153.13(9) . . ? N6 La1 N5 73.77(8) . . ? C1 N6 C5 116.0(3) . . ? C1 N6 La1 120.4(2) . . ? C5 N6 La1 123.6(2) . . ? C9 N7 C8 122.3(3) . . ? C9 N7 H7N 118.8 . . ? C8 N7 H7N 118.8 . . ? C11 N8 C15 121.3(3) . . ? C11 N8 H8N 119.4 . . ? C15 N8 H8N 119.4 . . ? C19 N9 C18 116.0(3) . . ? N6 C1 C2 123.6(3) . . ? N6 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 117.3(3) . . ? C2 C3 C6 121.8(3) . . ? C4 C3 C6 120.9(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N6 C5 C4 124.4(3) . . ? N6 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C7 C6 C10 117.4(3) . . ? C7 C6 C3 121.4(3) . . ? C10 C6 C3 121.1(3) . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? N7 C8 C7 119.8(4) . . ? N7 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? N7 C9 C10 119.9(3) . . ? N7 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C6 120.1(3) . . ? C9 C10 H10 120.0 . . ? C6 C10 H10 120.0 . . ? N8 C11 C12 120.7(3) . . ? N8 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 120.9(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 116.4(3) . . ? C12 C13 C16 121.1(3) . . ? C14 C13 C16 122.5(3) . . ? C15 C14 C13 120.7(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N8 C15 C14 120.0(3) . . ? N8 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C20 C16 C17 116.2(3) . . ? C20 C16 C13 122.7(3) . . ? C17 C16 C13 121.2(3) . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? N9 C18 C17 123.7(4) . . ? N9 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? N9 C19 C20 124.1(3) . . ? N9 C19 H19 117.9 . . ? C20 C19 H19 117.9 . . ? C19 C20 C16 119.7(4) . . ? C19 C20 H20 120.2 . . ? C16 C20 H20 120.2 . . ? N3 O7 La1 96.62(18) . . ? N2 O4 La1 98.30(19) . . ? N4 O10 La1 98.1(2) . . ? N4 O11 La1 96.3(2) . . ? N1 O1 La1 95.8(2) . . ? N2 O5 La1 96.39(19) . . ? N1 O2 La1 99.0(2) . . ? N3 O9 La1 97.06(19) . . ? O6 N2 O4 122.6(3) . . ? O6 N2 O5 119.9(3) . . ? O4 N2 O5 117.5(3) . . ? O3 N1 O1 123.0(3) . . ? O3 N1 O2 120.4(3) . . ? O1 N1 O2 116.6(3) . . ? O3 N1 La1 176.9(3) . . ? O1 N1 La1 60.00(19) . . ? O2 N1 La1 56.60(19) . . ? O8 N3 O7 120.9(3) . . ? O8 N3 O9 122.2(3) . . ? O7 N3 O9 116.9(3) . . ? O8 N3 La1 169.5(3) . . ? O7 N3 La1 59.16(16) . . ? O9 N3 La1 58.72(17) . . ? O12 N4 O11 122.1(4) . . ? O12 N4 O10 120.6(4) . . ? O11 N4 O10 117.2(3) . . ? O12 N4 La1 177.2(2) . . ? O11 N4 La1 59.55(16) . . ? O10 N4 La1 57.77(17) . . ? N5 O14 La1 98.1(2) . . ? N5 O13 La1 96.5(2) . . ? O15 N5 O13 121.9(3) . . ? O15 N5 O14 121.5(3) . . ? O13 N5 O14 116.6(3) . . ? O15 N5 La1 178.9(3) . . ? O13 N5 La1 59.10(17) . . ? O14 N5 La1 57.52(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 La1 N6 C1 87.3(3) . . . . ? O14 La1 N6 C1 -149.8(3) . . . . ? O10 La1 N6 C1 -125.4(3) . . . . ? O13 La1 N6 C1 -100.5(3) . . . . ? O9 La1 N6 C1 -37.1(3) . . . . ? O7 La1 N6 C1 -29.4(3) . . . . ? O1 La1 N6 C1 139.5(3) . . . . ? O11 La1 N6 C1 158.1(3) . . . . ? O4 La1 N6 C1 58.3(3) . . . . ? O5 La1 N6 C1 28.7(3) . . . . ? N5 La1 N6 C1 -125.8(3) . . . . ? O2 La1 N6 C5 -92.5(3) . . . . ? O14 La1 N6 C5 30.4(3) . . . . ? O10 La1 N6 C5 54.8(4) . . . . ? O13 La1 N6 C5 79.8(3) . . . . ? O9 La1 N6 C5 143.1(3) . . . . ? O7 La1 N6 C5 150.8(3) . . . . ? O1 La1 N6 C5 -40.3(3) . . . . ? O11 La1 N6 C5 -21.7(3) . . . . ? O4 La1 N6 C5 -121.4(3) . . . . ? O5 La1 N6 C5 -151.0(3) . . . . ? N5 La1 N6 C5 54.5(3) . . . . ? C5 N6 C1 C2 -0.8(6) . . . . ? La1 N6 C1 C2 179.4(3) . . . . ? N6 C1 C2 C3 0.9(6) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C6 177.5(4) . . . . ? C2 C3 C4 C5 -0.1(6) . . . . ? C6 C3 C4 C5 -178.0(4) . . . . ? C1 N6 C5 C4 0.3(6) . . . . ? La1 N6 C5 C4 -180.0(3) . . . . ? C3 C4 C5 N6 0.2(6) . . . . ? C2 C3 C6 C7 161.3(4) . . . . ? C4 C3 C6 C7 -20.8(6) . . . . ? C2 C3 C6 C10 -20.3(6) . . . . ? C4 C3 C6 C10 157.5(4) . . . . ? C10 C6 C7 C8 -1.9(6) . . . . ? C3 C6 C7 C8 176.5(4) . . . . ? C9 N7 C8 C7 0.6(7) . . . . ? C6 C7 C8 N7 1.0(7) . . . . ? C8 N7 C9 C10 -1.2(6) . . . . ? N7 C9 C10 C6 0.3(6) . . . . ? C7 C6 C10 C9 1.2(6) . . . . ? C3 C6 C10 C9 -177.2(4) . . . . ? C15 N8 C11 C12 1.0(7) . . . . ? N8 C11 C12 C13 -1.1(7) . . . . ? C11 C12 C13 C14 0.3(6) . . . . ? C11 C12 C13 C16 -179.2(4) . . . . ? C12 C13 C14 C15 0.7(5) . . . . ? C16 C13 C14 C15 -179.8(3) . . . . ? C11 N8 C15 C14 0.0(6) . . . . ? C13 C14 C15 N8 -0.9(6) . . . . ? C12 C13 C16 C20 171.0(4) . . . . ? C14 C13 C16 C20 -8.5(6) . . . . ? C12 C13 C16 C17 -8.9(6) . . . . ? C14 C13 C16 C17 171.6(4) . . . . ? C20 C16 C17 C18 1.0(6) . . . . ? C13 C16 C17 C18 -179.1(4) . . . . ? C19 N9 C18 C17 0.8(6) . . . . ? C16 C17 C18 N9 -1.1(6) . . . . ? C18 N9 C19 C20 -0.5(6) . . . . ? N9 C19 C20 C16 0.5(7) . . . . ? C17 C16 C20 C19 -0.7(6) . . . . ? C13 C16 C20 C19 179.4(4) . . . . ? O2 La1 O7 N3 122.9(2) . . . . ? O14 La1 O7 N3 -108.1(2) . . . . ? O10 La1 O7 N3 -25.2(2) . . . . ? O13 La1 O7 N3 -101.4(2) . . . . ? O9 La1 O7 N3 -6.36(19) . . . . ? O1 La1 O7 N3 167.22(19) . . . . ? O11 La1 O7 N3 -12.5(4) . . . . ? O4 La1 O7 N3 47.8(2) . . . . ? O5 La1 O7 N3 74.2(2) . . . . ? N6 La1 O7 N3 -177.1(2) . . . . ? N5 La1 O7 N3 -104.6(2) . . . . ? O2 La1 O4 N2 -72.9(2) . . . . ? O14 La1 O4 N2 177.31(19) . . . . ? O10 La1 O4 N2 137.2(2) . . . . ? O13 La1 O4 N2 94.5(2) . . . . ? O9 La1 O4 N2 68.6(2) . . . . ? O7 La1 O4 N2 29.7(2) . . . . ? O1 La1 O4 N2 -114.2(2) . . . . ? O11 La1 O4 N2 -170.8(2) . . . . ? O5 La1 O4 N2 -2.88(19) . . . . ? N6 La1 O4 N2 -44.6(2) . . . . ? N5 La1 O4 N2 143.2(2) . . . . ? O2 La1 O10 N4 35.3(2) . . . . ? O14 La1 O10 N4 -77.0(2) . . . . ? O13 La1 O10 N4 -125.2(2) . . . . ? O9 La1 O10 N4 156.6(2) . . . . ? O7 La1 O10 N4 172.00(19) . . . . ? O1 La1 O10 N4 -16.8(2) . . . . ? O11 La1 O10 N4 -1.75(18) . . . . ? O4 La1 O10 N4 75.3(2) . . . . ? O5 La1 O10 N4 105.1(2) . . . . ? N6 La1 O10 N4 -101.9(3) . . . . ? N5 La1 O10 N4 -101.6(2) . . . . ? O2 La1 O11 N4 -151.6(2) . . . . ? O14 La1 O11 N4 90.3(2) . . . . ? O10 La1 O11 N4 1.75(18) . . . . ? O13 La1 O11 N4 65.4(2) . . . . ? O9 La1 O11 N4 -19.1(2) . . . . ? O7 La1 O11 N4 -14.2(3) . . . . ? O1 La1 O11 N4 166.0(2) . . . . ? O4 La1 O11 N4 -80.9(2) . . . . ? O5 La1 O11 N4 -90.6(2) . . . . ? N6 La1 O11 N4 146.56(18) . . . . ? N5 La1 O11 N4 77.8(2) . . . . ? O2 La1 O1 N1 -0.51(19) . . . . ? O14 La1 O1 N1 -167.6(2) . . . . ? O10 La1 O1 N1 128.0(2) . . . . ? O13 La1 O1 N1 -138.7(2) . . . . ? O7 La1 O1 N1 -64.3(2) . . . . ? O11 La1 O1 N1 115.6(2) . . . . ? O4 La1 O1 N1 56.5(2) . . . . ? O5 La1 O1 N1 8.8(2) . . . . ? N6 La1 O1 N1 -80.0(2) . . . . ? N5 La1 O1 N1 -153.2(2) . . . . ? O2 La1 O5 N2 92.7(2) . . . . ? O10 La1 O5 N2 -36.2(2) . . . . ? O13 La1 O5 N2 -135.99(19) . . . . ? O9 La1 O5 N2 -87.3(2) . . . . ? O7 La1 O5 N2 -141.1(2) . . . . ? O1 La1 O5 N2 84.9(2) . . . . ? O11 La1 O5 N2 15.0(2) . . . . ? O4 La1 O5 N2 2.86(18) . . . . ? N6 La1 O5 N2 155.4(2) . . . . ? N5 La1 O5 N2 -138.4(2) . . . . ? O14 La1 O2 N1 13.9(2) . . . . ? O10 La1 O2 N1 -79.9(2) . . . . ? O13 La1 O2 N1 70.5(2) . . . . ? O9 La1 O2 N1 -169.84(18) . . . . ? O7 La1 O2 N1 141.9(2) . . . . ? O1 La1 O2 N1 0.51(19) . . . . ? O11 La1 O2 N1 -53.2(2) . . . . ? O4 La1 O2 N1 -119.1(2) . . . . ? O5 La1 O2 N1 -169.9(2) . . . . ? N6 La1 O2 N1 81.3(2) . . . . ? N5 La1 O2 N1 37.7(3) . . . . ? O2 La1 O9 N3 -68.3(2) . . . . ? O14 La1 O9 N3 108.1(2) . . . . ? O10 La1 O9 N3 166.9(2) . . . . ? O13 La1 O9 N3 75.0(2) . . . . ? O7 La1 O9 N3 6.36(19) . . . . ? O11 La1 O9 N3 -176.1(2) . . . . ? O4 La1 O9 N3 -118.4(2) . . . . ? O5 La1 O9 N3 -68.2(2) . . . . ? N6 La1 O9 N3 16.1(2) . . . . ? N5 La1 O9 N3 91.0(2) . . . . ? La1 O4 N2 O6 -173.9(3) . . . . ? La1 O4 N2 O5 5.1(3) . . . . ? La1 O5 N2 O6 174.0(3) . . . . ? La1 O5 N2 O4 -5.0(3) . . . . ? La1 O1 N1 O3 -179.5(3) . . . . ? La1 O1 N1 O2 0.9(3) . . . . ? La1 O2 N1 O3 179.5(3) . . . . ? La1 O2 N1 O1 -0.9(3) . . . . ? O2 La1 N1 O1 179.1(3) . . . . ? O14 La1 N1 O1 11.5(2) . . . . ? O10 La1 N1 O1 -62.6(2) . . . . ? O13 La1 N1 O1 50.3(2) . . . . ? O9 La1 N1 O1 -163.41(19) . . . . ? O7 La1 N1 O1 133.33(19) . . . . ? O11 La1 N1 O1 -56.6(2) . . . . ? O4 La1 N1 O1 -124.2(2) . . . . ? O5 La1 N1 O1 -171.8(2) . . . . ? N6 La1 N1 O1 90.3(2) . . . . ? N5 La1 N1 O1 28.8(2) . . . . ? O14 La1 N1 O2 -167.5(2) . . . . ? O10 La1 N1 O2 118.3(2) . . . . ? O13 La1 N1 O2 -128.8(2) . . . . ? O9 La1 N1 O2 17.5(3) . . . . ? O7 La1 N1 O2 -45.7(2) . . . . ? O1 La1 N1 O2 -179.1(3) . . . . ? O11 La1 N1 O2 124.3(2) . . . . ? O4 La1 N1 O2 56.7(2) . . . . ? O5 La1 N1 O2 9.1(2) . . . . ? N6 La1 N1 O2 -88.8(2) . . . . ? N5 La1 N1 O2 -150.3(2) . . . . ? La1 O7 N3 O8 -167.7(3) . . . . ? La1 O7 N3 O9 11.1(3) . . . . ? La1 O9 N3 O8 167.6(3) . . . . ? La1 O9 N3 O7 -11.2(3) . . . . ? O2 La1 N3 O8 27.8(13) . . . . ? O14 La1 N3 O8 177.7(13) . . . . ? O10 La1 N3 O8 -110.0(13) . . . . ? O13 La1 N3 O8 163.1(13) . . . . ? O9 La1 N3 O8 -98.1(13) . . . . ? O7 La1 N3 O8 93.5(13) . . . . ? O1 La1 N3 O8 66.5(14) . . . . ? O11 La1 N3 O8 -93.0(13) . . . . ? O4 La1 N3 O8 -40.2(13) . . . . ? O5 La1 N3 O8 1.2(13) . . . . ? N6 La1 N3 O8 96.2(13) . . . . ? N5 La1 N3 O8 170.2(13) . . . . ? O2 La1 N3 O7 -65.7(2) . . . . ? O14 La1 N3 O7 84.2(2) . . . . ? O10 La1 N3 O7 156.6(2) . . . . ? O13 La1 N3 O7 69.7(2) . . . . ? O9 La1 N3 O7 168.4(3) . . . . ? O1 La1 N3 O7 -27.0(4) . . . . ? O11 La1 N3 O7 173.56(19) . . . . ? O4 La1 N3 O7 -133.7(2) . . . . ? O5 La1 N3 O7 -92.3(2) . . . . ? N6 La1 N3 O7 2.7(2) . . . . ? N5 La1 N3 O7 76.8(2) . . . . ? O2 La1 N3 O9 125.9(2) . . . . ? O14 La1 N3 O9 -84.2(2) . . . . ? O10 La1 N3 O9 -11.8(2) . . . . ? O13 La1 N3 O9 -98.7(2) . . . . ? O7 La1 N3 O9 -168.4(3) . . . . ? O1 La1 N3 O9 164.6(2) . . . . ? O11 La1 N3 O9 5.2(3) . . . . ? O4 La1 N3 O9 57.9(2) . . . . ? O5 La1 N3 O9 99.3(2) . . . . ? N6 La1 N3 O9 -165.7(2) . . . . ? N5 La1 N3 O9 -91.6(2) . . . . ? La1 O11 N4 O12 177.4(3) . . . . ? La1 O11 N4 O10 -3.0(3) . . . . ? La1 O10 N4 O12 -177.3(3) . . . . ? La1 O10 N4 O11 3.1(3) . . . . ? O2 La1 N4 O11 30.7(2) . . . . ? O14 La1 N4 O11 -81.0(2) . . . . ? O10 La1 N4 O11 -176.8(3) . . . . ? O13 La1 N4 O11 -120.8(2) . . . . ? O9 La1 N4 O11 162.1(2) . . . . ? O7 La1 N4 O11 172.67(18) . . . . ? O1 La1 N4 O11 -12.6(2) . . . . ? O4 La1 N4 O11 88.4(2) . . . . ? O5 La1 N4 O11 99.7(2) . . . . ? N6 La1 N4 O11 -53.6(3) . . . . ? N5 La1 N4 O11 -101.4(2) . . . . ? O2 La1 N4 O10 -152.53(19) . . . . ? O14 La1 N4 O10 95.8(2) . . . . ? O13 La1 N4 O10 56.0(2) . . . . ? O9 La1 N4 O10 -21.1(2) . . . . ? O7 La1 N4 O10 -10.5(2) . . . . ? O1 La1 N4 O10 164.3(2) . . . . ? O11 La1 N4 O10 176.8(3) . . . . ? O4 La1 N4 O10 -94.7(2) . . . . ? O5 La1 N4 O10 -83.5(2) . . . . ? N6 La1 N4 O10 123.2(2) . . . . ? N5 La1 N4 O10 75.4(2) . . . . ? O2 La1 O14 N5 132.1(2) . . . . ? O10 La1 O14 N5 -97.9(2) . . . . ? O13 La1 O14 N5 0.42(19) . . . . ? O9 La1 O14 N5 -44.8(2) . . . . ? O7 La1 O14 N5 8.5(2) . . . . ? O1 La1 O14 N5 142.8(2) . . . . ? O11 La1 O14 N5 -148.3(2) . . . . ? O4 La1 O14 N5 -136.58(19) . . . . ? N6 La1 O14 N5 71.2(2) . . . . ? O2 La1 O13 N5 -85.3(2) . . . . ? O14 La1 O13 N5 -0.42(19) . . . . ? O10 La1 O13 N5 73.2(2) . . . . ? O9 La1 O13 N5 138.2(2) . . . . ? O7 La1 O13 N5 -172.4(2) . . . . ? O1 La1 O13 N5 -37.3(2) . . . . ? O11 La1 O13 N5 31.1(2) . . . . ? O4 La1 O13 N5 112.8(2) . . . . ? O5 La1 O13 N5 -177.35(18) . . . . ? N6 La1 O13 N5 -96.0(2) . . . . ? La1 O13 N5 O15 -179.4(3) . . . . ? La1 O13 N5 O14 0.7(3) . . . . ? La1 O14 N5 O15 179.4(3) . . . . ? La1 O14 N5 O13 -0.7(3) . . . . ? O2 La1 N5 O13 117.9(2) . . . . ? O14 La1 N5 O13 179.2(3) . . . . ? O10 La1 N5 O13 -104.0(2) . . . . ? O9 La1 N5 O13 -40.9(2) . . . . ? O7 La1 N5 O13 7.0(2) . . . . ? O1 La1 N5 O13 144.9(2) . . . . ? O11 La1 N5 O13 -151.3(2) . . . . ? O4 La1 N5 O13 -109.7(2) . . . . ? O5 La1 N5 O13 4.6(3) . . . . ? N6 La1 N5 O13 75.8(2) . . . . ? O2 La1 N5 O14 -61.3(2) . . . . ? O10 La1 N5 O14 76.8(2) . . . . ? O13 La1 N5 O14 -179.2(3) . . . . ? O9 La1 N5 O14 139.8(2) . . . . ? O7 La1 N5 O14 -172.3(2) . . . . ? O1 La1 N5 O14 -34.3(2) . . . . ? O11 La1 N5 O14 29.5(2) . . . . ? O4 La1 N5 O14 71.0(3) . . . . ? O5 La1 N5 O14 -174.6(2) . . . . ? N6 La1 N5 O14 -103.4(2) . . . . ? _diffrn_measured_fraction_theta_max .999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full .999 _refine_diff_density_max .942 _refine_diff_density_min -.474 _refine_diff_density_rms .088