# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H24 As Eu N6 S4 ' _chemical_formula_sum 'C6 H24 As Eu N6 S4 ' _chemical_formula_weight 535.48 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4937(19) _cell_length_b 12.292(3) _cell_length_c 14.967(3) _cell_angle_alpha 90 _cell_angle_beta 98.08(3) _cell_angle_gamma 90 _cell_volume 1729.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 6.003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1244 _exptl_absorpt_correction_T_max 0.5603 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9345 _diffrn_reflns_av_R_equivalents 0.0888 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3074 _reflns_number_gt 2831 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+4.9185P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0223(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3074 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.66661(2) 0.49265(2) 0.292376(17) 0.01062(16) Uani 1 1 d . . . As1 As 0.27941(5) 0.52292(5) 0.25724(4) 0.01154(18) Uani 1 1 d . . . S1 S 0.39690(14) 0.37664(12) 0.30325(11) 0.0227(4) Uani 1 1 d . . . S2 S 0.44394(14) 0.62832(12) 0.21456(11) 0.0227(4) Uani 1 1 d . . . S3 S 0.11805(17) 0.49113(14) 0.14642(12) 0.0262(4) Uani 1 1 d . . . S4 S 0.20073(15) 0.60077(14) 0.37025(10) 0.0261(4) Uani 1 1 d . . . N6 N 0.7189(5) 0.3348(4) 0.4019(3) 0.0196(11) Uani 1 1 d . . . H6A H 0.6897 0.3535 0.4544 0.024 Uiso 1 1 calc R . . H6B H 0.6656 0.2778 0.3800 0.024 Uiso 1 1 calc R . . N1 N 0.6031(6) 0.5783(5) 0.4384(3) 0.0299(13) Uani 1 1 d . . . H1A H 0.5079 0.5779 0.4364 0.036 Uiso 1 1 calc R . . H1B H 0.6404 0.5372 0.4858 0.036 Uiso 1 1 calc R . . N4 N 0.7592(5) 0.5788(4) 0.1533(3) 0.0236(11) Uani 1 1 d . . . H4A H 0.7364 0.6499 0.1500 0.028 Uiso 1 1 calc R . . H4B H 0.8547 0.5737 0.1602 0.028 Uiso 1 1 calc R . . N3 N 0.6429(6) 0.3686(5) 0.1569(3) 0.0316(13) Uani 1 1 d . . . H3A H 0.6791 0.3033 0.1752 0.038 Uiso 1 1 calc R . . H3B H 0.5496 0.3589 0.1376 0.038 Uiso 1 1 calc R . . N2 N 0.8113(5) 0.6668(4) 0.3404(4) 0.0290(12) Uani 1 1 d . . . H2A H 0.9026 0.6562 0.3327 0.035 Uiso 1 1 calc R . . H2B H 0.7773 0.7222 0.3042 0.035 Uiso 1 1 calc R . . N5 N 0.9208(5) 0.4233(5) 0.3054(4) 0.0327(14) Uani 1 1 d . . . H5A H 0.9493 0.4266 0.2505 0.039 Uiso 1 1 calc R . . H5B H 0.9775 0.4679 0.3420 0.039 Uiso 1 1 calc R . . C6 C 0.8670(6) 0.2985(6) 0.4216(4) 0.0289(15) Uani 1 1 d . . . H6C H 0.8696 0.2224 0.4395 0.035 Uiso 1 1 calc R . . H6D H 0.9163 0.3403 0.4712 0.035 Uiso 1 1 calc R . . C5 C 0.9401(6) 0.3131(6) 0.3396(4) 0.0306(15) Uani 1 1 d . . . H5C H 1.0409 0.2980 0.3550 0.037 Uiso 1 1 calc R . . H5D H 0.9010 0.2622 0.2933 0.037 Uiso 1 1 calc R . . C4 C 0.6989(9) 0.5253(7) 0.0684(5) 0.0395(18) Uani 1 1 d . . . H4C H 0.7492 0.5496 0.0198 0.047 Uiso 1 1 calc R . . H4D H 0.5995 0.5450 0.0531 0.047 Uiso 1 1 calc R . . C3 C 0.7119(8) 0.4050(6) 0.0791(4) 0.0364(17) Uani 1 1 d . . . H3C H 0.6671 0.3697 0.0246 0.044 Uiso 1 1 calc R . . H3D H 0.8116 0.3848 0.0887 0.044 Uiso 1 1 calc R . . C2 C 0.8062(7) 0.6972(6) 0.4346(5) 0.0390(17) Uani 1 1 d . . . H2C H 0.8418 0.7707 0.4452 0.047 Uiso 1 1 calc R . . H2D H 0.8653 0.6484 0.4750 0.047 Uiso 1 1 calc R . . C1 C 0.6552(7) 0.6902(6) 0.4521(4) 0.0336(16) Uani 1 1 d . . . H1C H 0.6491 0.7123 0.5135 0.040 Uiso 1 1 calc R . . H1D H 0.5966 0.7389 0.4115 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0040(2) 0.0190(2) 0.0087(2) 0.00219(10) 0.00058(13) -0.00043(9) As1 0.0033(3) 0.0217(3) 0.0097(3) -0.0007(2) 0.0012(2) -0.0006(2) S1 0.0096(6) 0.0224(8) 0.0358(9) 0.0080(7) 0.0022(6) -0.0012(5) S2 0.0087(6) 0.0263(8) 0.0327(9) 0.0147(7) 0.0025(6) 0.0006(6) S3 0.0129(8) 0.0528(11) 0.0121(8) -0.0060(6) -0.0014(6) -0.0049(6) S4 0.0219(7) 0.0413(9) 0.0165(8) -0.0137(7) 0.0070(6) -0.0013(7) N6 0.013(2) 0.029(3) 0.017(3) 0.002(2) 0.0018(19) -0.003(2) N1 0.033(3) 0.040(3) 0.019(3) -0.008(3) 0.010(2) -0.012(3) N4 0.017(2) 0.033(3) 0.022(3) 0.006(2) 0.006(2) 0.000(2) N3 0.034(3) 0.038(3) 0.024(3) -0.009(3) 0.003(2) -0.012(3) N2 0.021(3) 0.032(3) 0.035(3) -0.002(3) 0.009(2) -0.009(2) N5 0.013(2) 0.054(4) 0.032(3) 0.016(3) 0.007(2) 0.008(2) C6 0.024(3) 0.045(4) 0.017(3) 0.013(3) 0.002(2) 0.010(3) C5 0.021(3) 0.043(4) 0.029(4) 0.005(3) 0.008(3) 0.014(3) C4 0.047(5) 0.054(5) 0.020(4) -0.001(4) 0.015(3) -0.003(4) C3 0.044(4) 0.045(4) 0.022(4) -0.017(3) 0.010(3) -0.001(3) C2 0.039(4) 0.041(4) 0.033(4) -0.009(3) -0.011(3) -0.015(3) C1 0.047(4) 0.034(4) 0.021(3) -0.006(3) 0.007(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 N3 2.522(5) . ? Eu1 N6 2.544(5) . ? Eu1 N5 2.543(5) . ? Eu1 N1 2.578(5) . ? Eu1 N4 2.596(5) . ? Eu1 N2 2.590(5) . ? Eu1 S2 2.8125(17) . ? Eu1 S1 2.9553(16) . ? Eu1 As1 3.6592(10) . ? As1 S3 2.1309(19) . ? As1 S4 2.1656(17) . ? As1 S1 2.1752(17) . ? As1 S2 2.1925(16) . ? N6 C6 1.466(7) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N1 C1 1.466(8) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N4 C4 1.476(9) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N3 C3 1.481(8) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N2 C2 1.469(9) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N5 C5 1.448(9) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? C6 C5 1.503(8) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C4 C3 1.490(10) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C2 C1 1.495(9) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? 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 N3 Eu1 N6 92.46(17) . . ? N3 Eu1 N5 80.4(2) . . ? N6 Eu1 N5 66.19(15) . . ? N3 Eu1 N1 157.83(16) . . ? N6 Eu1 N1 79.36(17) . . ? N5 Eu1 N1 114.04(18) . . ? N3 Eu1 N4 66.59(17) . . ? N6 Eu1 N4 140.39(15) . . ? N5 Eu1 N4 76.81(16) . . ? N1 Eu1 N4 131.32(18) . . ? N3 Eu1 N2 135.14(16) . . ? N6 Eu1 N2 113.68(17) . . ? N5 Eu1 N2 78.29(19) . . ? N1 Eu1 N2 66.70(18) . . ? N4 Eu1 N2 70.08(17) . . ? N3 Eu1 S2 92.92(14) . . ? N6 Eu1 S2 141.82(10) . . ? N5 Eu1 S2 151.84(12) . . ? N1 Eu1 S2 81.77(13) . . ? N4 Eu1 S2 75.27(11) . . ? N2 Eu1 S2 87.93(13) . . ? N3 Eu1 S1 76.83(12) . . ? N6 Eu1 S1 71.85(12) . . ? N5 Eu1 S1 130.92(14) . . ? N1 Eu1 S1 81.04(12) . . ? N4 Eu1 S1 129.39(11) . . ? N2 Eu1 S1 144.31(11) . . ? S2 Eu1 S1 72.68(5) . . ? N3 Eu1 As1 88.47(13) . . ? N6 Eu1 As1 105.85(10) . . ? N5 Eu1 As1 165.78(15) . . ? N1 Eu1 As1 74.28(13) . . ? N4 Eu1 As1 106.88(11) . . ? N2 Eu1 As1 115.93(12) . . ? S2 Eu1 As1 36.76(4) . . ? S1 Eu1 As1 36.47(3) . . ? S3 As1 S4 113.64(7) . . ? S3 As1 S1 112.05(7) . . ? S4 As1 S1 109.61(7) . . ? S3 As1 S2 110.21(7) . . ? S4 As1 S2 107.73(7) . . ? S1 As1 S2 103.06(6) . . ? S3 As1 Eu1 133.75(6) . . ? S4 As1 Eu1 112.52(5) . . ? S1 As1 Eu1 53.88(5) . . ? S2 As1 Eu1 50.12(4) . . ? As1 S1 Eu1 89.62(6) . . ? As1 S2 Eu1 93.08(6) . . ? C6 N6 Eu1 117.3(3) . . ? C6 N6 H6A 108.0 . . ? Eu1 N6 H6A 108.0 . . ? C6 N6 H6B 108.0 . . ? Eu1 N6 H6B 108.0 . . ? H6A N6 H6B 107.2 . . ? C1 N1 Eu1 113.1(3) . . ? C1 N1 H1A 109.0 . . ? Eu1 N1 H1A 109.0 . . ? C1 N1 H1B 109.0 . . ? Eu1 N1 H1B 109.0 . . ? H1A N1 H1B 107.8 . . ? C4 N4 Eu1 112.1(4) . . ? C4 N4 H4A 109.2 . . ? Eu1 N4 H4A 109.2 . . ? C4 N4 H4B 109.2 . . ? Eu1 N4 H4B 109.2 . . ? H4A N4 H4B 107.9 . . ? C3 N3 Eu1 116.8(4) . . ? C3 N3 H3A 108.1 . . ? Eu1 N3 H3A 108.1 . . ? C3 N3 H3B 108.1 . . ? Eu1 N3 H3B 108.1 . . ? H3A N3 H3B 107.3 . . ? C2 N2 Eu1 113.2(4) . . ? C2 N2 H2A 108.9 . . ? Eu1 N2 H2A 108.9 . . ? C2 N2 H2B 108.9 . . ? Eu1 N2 H2B 108.9 . . ? H2A N2 H2B 107.7 . . ? C5 N5 Eu1 114.4(3) . . ? C5 N5 H5A 108.7 . . ? Eu1 N5 H5A 108.7 . . ? C5 N5 H5B 108.7 . . ? Eu1 N5 H5B 108.7 . . ? H5A N5 H5B 107.6 . . ? N6 C6 C5 109.9(5) . . ? N6 C6 H6C 109.7 . . ? C5 C6 H6C 109.7 . . ? N6 C6 H6D 109.7 . . ? C5 C6 H6D 109.7 . . ? H6C C6 H6D 108.2 . . ? N5 C5 C6 110.1(5) . . ? N5 C5 H5C 109.6 . . ? C6 C5 H5C 109.6 . . ? N5 C5 H5D 109.6 . . ? C6 C5 H5D 109.6 . . ? H5C C5 H5D 108.1 . . ? N4 C4 C3 109.7(6) . . ? N4 C4 H4C 109.7 . . ? C3 C4 H4C 109.7 . . ? N4 C4 H4D 109.7 . . ? C3 C4 H4D 109.7 . . ? H4C C4 H4D 108.2 . . ? N3 C3 C4 109.8(5) . . ? N3 C3 H3C 109.7 . . ? C4 C3 H3C 109.7 . . ? N3 C3 H3D 109.7 . . ? C4 C3 H3D 109.7 . . ? H3C C3 H3D 108.2 . . ? N2 C2 C1 108.4(5) . . ? N2 C2 H2C 110.0 . . ? C1 C2 H2C 110.0 . . ? N2 C2 H2D 110.0 . . ? C1 C2 H2D 110.0 . . ? H2C C2 H2D 108.4 . . ? N1 C1 C2 109.8(6) . . ? N1 C1 H1C 109.7 . . ? C2 C1 H1C 109.7 . . ? N1 C1 H1D 109.7 . . ? C2 C1 H1D 109.7 . . ? H1C C1 H1D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.732 _refine_diff_density_min -2.854 _refine_diff_density_rms 0.241 _database_code_depnum_ccdc_archive 'CCDC 913891' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H26 As Er N6 S4 ' _chemical_formula_sum 'C8 H26 As Er N6 S4 ' _chemical_formula_weight 576.81 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6537(19) _cell_length_b 13.118(3) _cell_length_c 14.603(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.53(3) _cell_angle_gamma 90.00 _cell_volume 1833.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 6.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2253 _exptl_absorpt_correction_T_max 0.3319 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9642 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3253 _reflns_number_gt 2735 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00043(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3253 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.71260(4) 0.51716(3) 0.24027(3) 0.02032(12) Uani 1 1 d . . . Er1 Er 0.337199(16) 0.483467(14) 0.215834(14) 0.01662(8) Uani 1 1 d . . . S1 S 0.55563(10) 0.60258(9) 0.30418(9) 0.0292(3) Uani 1 1 d . . . S2 S 0.59045(10) 0.38602(8) 0.18541(9) 0.0271(3) Uani 1 1 d . . . S3 S 0.77457(12) 0.60464(9) 0.12685(9) 0.0335(3) Uani 1 1 d . . . S4 S 0.88201(11) 0.47482(10) 0.34153(9) 0.0343(3) Uani 1 1 d . . . N1 N 0.3661(4) 0.3525(3) 0.3404(3) 0.0364(10) Uani 1 1 d . . . H1A H 0.3310 0.2933 0.3164 0.044 Uiso 1 1 calc R . . H1B H 0.4582 0.3430 0.3576 0.044 Uiso 1 1 calc R . . N2 N 0.2253(3) 0.5351(3) 0.3535(3) 0.0241(9) Uani 1 1 d . . . H2C H 0.1378 0.5081 0.3442 0.029 Uiso 1 1 calc R . . N3 N 0.2499(3) 0.6628(3) 0.2042(3) 0.0238(9) Uani 1 1 d . . . H3C H 0.3264 0.7013 0.2240 0.029 Uiso 1 1 calc R . . N4 N 0.3650(4) 0.5609(3) 0.0644(3) 0.0317(10) Uani 1 1 d . . . H4A H 0.4547 0.5538 0.0548 0.038 Uiso 1 1 calc R . . H4B H 0.3123 0.5253 0.0199 0.038 Uiso 1 1 calc R . . N5 N 0.0817(3) 0.4569(3) 0.1675(3) 0.0281(9) Uani 1 1 d . . . H5A H 0.0428 0.4367 0.2172 0.034 Uiso 1 1 calc R . . H5B H 0.0433 0.5173 0.1492 0.034 Uiso 1 1 calc R . . N6 N 0.2855(3) 0.3277(3) 0.1174(3) 0.0256(9) Uani 1 1 d . . . H6A H 0.3060 0.3413 0.0603 0.031 Uiso 1 1 calc R . . H6B H 0.3422 0.2771 0.1409 0.031 Uiso 1 1 calc R . . C1 C 0.3004(6) 0.3746(4) 0.4243(4) 0.0442(14) Uani 1 1 d . . . H1C H 0.3542 0.3427 0.4774 0.053 Uiso 1 1 calc R . . H1D H 0.2068 0.3463 0.4175 0.053 Uiso 1 1 calc R . . C2 C 0.2936(5) 0.4876(4) 0.4399(4) 0.0372(12) Uani 1 1 d . . . H2A H 0.2402 0.5018 0.4903 0.045 Uiso 1 1 calc R . . H2B H 0.3870 0.5149 0.4558 0.045 Uiso 1 1 calc R . . C3 C 0.2051(4) 0.6446(3) 0.3616(4) 0.0334(12) Uani 1 1 d . . . H3A H 0.2935 0.6769 0.3840 0.040 Uiso 1 1 calc R . . H3B H 0.1405 0.6579 0.4057 0.040 Uiso 1 1 calc R . . C4 C 0.1481(4) 0.6887(4) 0.2687(3) 0.0303(12) Uani 1 1 d . . . H4C H 0.0574 0.6595 0.2471 0.036 Uiso 1 1 calc R . . H4D H 0.1381 0.7620 0.2731 0.036 Uiso 1 1 calc R . . C5 C 0.2083(5) 0.6957(4) 0.1085(4) 0.0372(13) Uani 1 1 d . . . H5C H 0.1906 0.7685 0.1064 0.045 Uiso 1 1 calc R . . H5D H 0.1235 0.6608 0.0826 0.045 Uiso 1 1 calc R . . C6 C 0.3268(5) 0.6700(3) 0.0536(4) 0.0357(12) Uani 1 1 d . . . H6C H 0.2984 0.6850 -0.0112 0.043 Uiso 1 1 calc R . . H6D H 0.4075 0.7118 0.0749 0.043 Uiso 1 1 calc R . . C7 C 0.0446(4) 0.3821(3) 0.0927(4) 0.0311(12) Uani 1 1 d . . . H7A H 0.0552 0.4126 0.0335 0.037 Uiso 1 1 calc R . . H7B H -0.0520 0.3612 0.0915 0.037 Uiso 1 1 calc R . . C8 C 0.1393(4) 0.2914(3) 0.1098(4) 0.0359(13) Uani 1 1 d . . . H8A H 0.1230 0.2573 0.1663 0.043 Uiso 1 1 calc R . . H8B H 0.1211 0.2433 0.0592 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01895(19) 0.0207(2) 0.0218(3) -0.0004(2) 0.00451(18) 0.00009(15) Er1 0.01851(10) 0.01593(12) 0.01562(13) -0.00140(9) 0.00302(7) 0.00018(7) S1 0.0204(5) 0.0306(7) 0.0369(9) -0.0166(6) 0.0048(5) -0.0020(4) S2 0.0226(5) 0.0224(6) 0.0363(8) -0.0082(5) 0.0043(5) 0.0005(4) S3 0.0392(6) 0.0336(7) 0.0288(9) 0.0094(6) 0.0084(6) -0.0001(5) S4 0.0247(5) 0.0472(8) 0.0306(8) 0.0080(6) 0.0017(5) 0.0007(5) N1 0.052(2) 0.026(2) 0.033(3) 0.005(2) 0.012(2) 0.0073(18) N2 0.0250(17) 0.023(2) 0.025(3) -0.0058(17) 0.0065(16) -0.0032(14) N3 0.0268(18) 0.021(2) 0.023(3) -0.0032(17) 0.0024(16) 0.0012(14) N4 0.044(2) 0.026(2) 0.027(3) 0.0019(19) 0.0099(18) 0.0050(17) N5 0.0261(17) 0.028(2) 0.030(3) -0.0074(19) 0.0017(17) 0.0003(15) N6 0.0271(18) 0.018(2) 0.032(3) -0.0022(18) 0.0069(17) 0.0016(14) C1 0.068(3) 0.042(3) 0.024(4) 0.008(3) 0.012(3) 0.001(3) C2 0.051(3) 0.044(3) 0.019(3) -0.004(2) 0.009(2) 0.000(2) C3 0.033(2) 0.034(3) 0.034(4) -0.013(2) 0.010(2) -0.0039(19) C4 0.032(2) 0.025(3) 0.034(4) -0.009(2) 0.004(2) 0.0050(18) C5 0.051(3) 0.023(3) 0.036(4) 0.001(2) 0.000(3) 0.011(2) C6 0.059(3) 0.022(3) 0.026(3) 0.004(2) 0.005(2) 0.002(2) C7 0.027(2) 0.039(3) 0.028(3) -0.007(2) 0.004(2) -0.0045(19) C8 0.035(2) 0.025(3) 0.048(4) -0.014(2) 0.006(2) -0.0073(19) _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 As1 S4 2.1298(14) . ? As1 S3 2.1628(14) . ? As1 S2 2.1781(12) . ? As1 S1 2.1893(12) . ? Er1 N4 2.480(4) . ? Er1 N1 2.491(4) . ? Er1 N3 2.497(3) . ? Er1 N2 2.498(4) . ? Er1 N5 2.499(3) . ? Er1 N6 2.510(3) . ? Er1 S1 2.7999(12) . ? Er1 S2 2.8448(11) . ? N1 C1 1.481(6) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.456(5) . ? N2 C2 1.482(6) . ? N2 H2C 0.9100 . ? N3 C5 1.469(6) . ? N3 C4 1.487(6) . ? N3 H3C 0.9100 . ? N4 C6 1.482(5) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C7 1.478(6) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 C8 1.480(5) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C1 C2 1.501(6) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.511(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.518(7) . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.502(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 S4 As1 S3 113.94(5) . . ? S4 As1 S2 112.26(5) . . ? S3 As1 S2 109.15(5) . . ? S4 As1 S1 110.42(5) . . ? S3 As1 S1 109.35(5) . . ? S2 As1 S1 100.92(4) . . ? N4 Er1 N1 156.73(13) . . ? N4 Er1 N3 68.21(12) . . ? N1 Er1 N3 134.75(13) . . ? N4 Er1 N2 135.70(12) . . ? N1 Er1 N2 67.56(12) . . ? N3 Er1 N2 67.75(12) . . ? N4 Er1 N5 91.32(13) . . ? N1 Er1 N5 97.03(13) . . ? N3 Er1 N5 78.48(11) . . ? N2 Er1 N5 75.55(12) . . ? N4 Er1 N6 81.90(13) . . ? N1 Er1 N6 81.46(14) . . ? N3 Er1 N6 133.46(12) . . ? N2 Er1 N6 127.39(11) . . ? N5 Er1 N6 67.05(11) . . ? N4 Er1 S1 91.13(10) . . ? N1 Er1 S1 92.45(10) . . ? N3 Er1 S1 74.49(8) . . ? N2 Er1 S1 81.75(8) . . ? N5 Er1 S1 149.72(9) . . ? N6 Er1 S1 143.07(8) . . ? N4 Er1 S2 81.32(9) . . ? N1 Er1 S2 77.73(10) . . ? N3 Er1 S2 134.58(8) . . ? N2 Er1 S2 135.95(9) . . ? N5 Er1 S2 136.87(9) . . ? N6 Er1 S2 69.85(8) . . ? S1 Er1 S2 73.26(3) . . ? As1 S1 Er1 92.26(4) . . ? As1 S2 Er1 91.29(4) . . ? C1 N1 Er1 116.7(3) . . ? C1 N1 H1A 108.1 . . ? Er1 N1 H1A 108.1 . . ? C1 N1 H1B 108.1 . . ? Er1 N1 H1B 108.1 . . ? H1A N1 H1B 107.3 . . ? C3 N2 C2 113.3(4) . . ? C3 N2 Er1 114.2(3) . . ? C2 N2 Er1 112.3(3) . . ? C3 N2 H2C 105.3 . . ? C2 N2 H2C 105.3 . . ? Er1 N2 H2C 105.3 . . ? C5 N3 C4 114.5(3) . . ? C5 N3 Er1 112.9(3) . . ? C4 N3 Er1 114.7(3) . . ? C5 N3 H3C 104.4 . . ? C4 N3 H3C 104.4 . . ? Er1 N3 H3C 104.4 . . ? C6 N4 Er1 115.8(3) . . ? C6 N4 H4A 108.3 . . ? Er1 N4 H4A 108.3 . . ? C6 N4 H4B 108.3 . . ? Er1 N4 H4B 108.3 . . ? H4A N4 H4B 107.4 . . ? C7 N5 Er1 115.9(2) . . ? C7 N5 H5A 108.3 . . ? Er1 N5 H5A 108.3 . . ? C7 N5 H5B 108.3 . . ? Er1 N5 H5B 108.3 . . ? H5A N5 H5B 107.4 . . ? C8 N6 Er1 115.0(3) . . ? C8 N6 H6A 108.5 . . ? Er1 N6 H6A 108.5 . . ? C8 N6 H6B 108.5 . . ? Er1 N6 H6B 108.5 . . ? H6A N6 H6B 107.5 . . ? N1 C1 C2 110.6(4) . . ? N1 C1 H1C 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? N2 C2 C1 108.1(4) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C4 110.0(4) . . ? N2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N3 C4 C3 106.7(3) . . ? N3 C4 H4C 110.4 . . ? C3 C4 H4C 110.4 . . ? N3 C4 H4D 110.4 . . ? C3 C4 H4D 110.4 . . ? H4C C4 H4D 108.6 . . ? N3 C5 C6 107.8(4) . . ? N3 C5 H5C 110.1 . . ? C6 C5 H5C 110.1 . . ? N3 C5 H5D 110.1 . . ? C6 C5 H5D 110.1 . . ? H5C C5 H5D 108.5 . . ? N4 C6 C5 110.7(4) . . ? N4 C6 H6C 109.5 . . ? C5 C6 H6C 109.5 . . ? N4 C6 H6D 109.5 . . ? C5 C6 H6D 109.5 . . ? H6C C6 H6D 108.1 . . ? N5 C7 C8 108.7(4) . . ? N5 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? N5 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? N6 C8 C7 108.1(4) . . ? N6 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? N6 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.920 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.158 _database_code_depnum_ccdc_archive 'CCDC 913892' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 #TrackingRef '3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H46 As2 La2 N10 S6' _chemical_formula_sum 'C16 H46 As2 La2 N10 S6' _chemical_formula_weight 998.71 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' 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 20.323(4) _cell_length_b 15.590(3) _cell_length_c 14.257(3) _cell_angle_alpha 90.00 _cell_angle_beta 131.55(3) _cell_angle_gamma 90.00 _cell_volume 3381(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 4.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2705 _exptl_absorpt_correction_T_max 0.4490 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10562 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3494 _reflns_number_gt 3128 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+5.3721P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3494 _refine_ls_number_parameters 163 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _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 0.055833(10) 0.355042(11) 0.525688(14) 0.02520(6) Uani 1 1 d . . . As1 As -0.16229(2) 0.37910(2) 0.30939(3) 0.03539(9) Uani 1 1 d . . . S3 S -0.09858(6) 0.35367(5) 0.50886(8) 0.03771(19) Uani 1 1 d . . . S2 S -0.07613(5) 0.48399(5) 0.33369(7) 0.03096(17) Uani 1 1 d . . . S1 S -0.10799(6) 0.27316(5) 0.27344(8) 0.0394(2) Uani 1 1 d . . . N1 N 0.12814(17) 0.43565(18) 0.4504(2) 0.0382(6) Uani 1 1 d U . . H1A H 0.1029 0.4159 0.3737 0.046 Uiso 1 1 calc R . . H1B H 0.1146 0.4917 0.4423 0.046 Uiso 1 1 calc R . . N2 N 0.23539(18) 0.37477(19) 0.7028(3) 0.0406(6) Uani 1 1 d U . . H2C H 0.2590 0.3234 0.7082 0.049 Uiso 1 1 calc R . . N4 N 0.0351(2) 0.18818(19) 0.5605(3) 0.0459(7) Uani 1 1 d U . . H4C H -0.0235 0.1790 0.4968 0.055 Uiso 1 1 calc R . . N5 N 0.1273(2) 0.22989(18) 0.4811(3) 0.0447(7) Uani 1 1 d U . . H5A H 0.1230 0.2466 0.4168 0.054 Uiso 1 1 calc R . . H5B H 0.1849 0.2248 0.5492 0.054 Uiso 1 1 calc R . . N3 N 0.1383(2) 0.3075(2) 0.7659(3) 0.0483(7) Uani 1 1 d U . . H3C H 0.1130 0.3403 0.7873 0.058 Uiso 1 1 calc R . . C2 C 0.2682(2) 0.4379(2) 0.6661(3) 0.0465(8) Uani 1 1 d U . . H2A H 0.3312 0.4308 0.7182 0.056 Uiso 1 1 calc R . . H2B H 0.2577 0.4953 0.6801 0.056 Uiso 1 1 calc R . . C1 C 0.2241(2) 0.4284(2) 0.5303(3) 0.0448(8) Uani 1 1 d U . . H1C H 0.2451 0.4727 0.5079 0.054 Uiso 1 1 calc R . . H1D H 0.2387 0.3731 0.5173 0.054 Uiso 1 1 calc R . . C3 C 0.2659(2) 0.3921(3) 0.8283(3) 0.0523(9) Uani 1 1 d U . . H3A H 0.2448 0.4479 0.8282 0.063 Uiso 1 1 calc R . . H3B H 0.3297 0.3933 0.8897 0.063 Uiso 1 1 calc R . . C4 C 0.2336(3) 0.3250(3) 0.8642(3) 0.0598(10) Uani 1 1 d U . . H4A H 0.2656 0.2722 0.8832 0.072 Uiso 1 1 calc R . . H4B H 0.2462 0.3432 0.9398 0.072 Uiso 1 1 calc R . . C8 C 0.0862(3) 0.1466(2) 0.4520(4) 0.0564(10) Uani 1 1 d U . . H8A H 0.1219 0.1040 0.4541 0.068 Uiso 1 1 calc R . . H8B H 0.0291 0.1478 0.3678 0.068 Uiso 1 1 calc R . . C7 C 0.0751(3) 0.1216(3) 0.5411(4) 0.0618(10) Uani 1 1 d U . . H7A H 0.0389 0.0705 0.5099 0.074 Uiso 1 1 calc R . . H7B H 0.1323 0.1074 0.6211 0.074 Uiso 1 1 calc R . . C6 C 0.0460(4) 0.1783(3) 0.6718(5) 0.0802(13) Uani 1 1 d U . . H6A H -0.0051 0.2023 0.6545 0.096 Uiso 1 1 calc R . . H6B H 0.0478 0.1176 0.6881 0.096 Uiso 1 1 calc R . . C5 C 0.1215(4) 0.2173(3) 0.7801(4) 0.0800(13) Uani 1 1 d U . . H5C H 0.1721 0.1828 0.8104 0.096 Uiso 1 1 calc R . . H5D H 0.1174 0.2162 0.8440 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02395(10) 0.02944(10) 0.02287(9) 0.00165(6) 0.01581(8) 0.00247(6) As1 0.02381(16) 0.03830(19) 0.03436(17) -0.00445(14) 0.01520(14) -0.00066(13) S3 0.0395(5) 0.0409(5) 0.0447(5) -0.0011(4) 0.0329(4) -0.0018(3) S2 0.0316(4) 0.0317(4) 0.0252(3) 0.0006(3) 0.0169(3) 0.0028(3) S1 0.0436(5) 0.0360(4) 0.0350(4) -0.0076(3) 0.0246(4) -0.0022(4) N1 0.0389(14) 0.0441(15) 0.0402(14) 0.0046(12) 0.0298(12) 0.0027(12) N2 0.0324(13) 0.0451(15) 0.0387(14) -0.0015(12) 0.0212(12) 0.0062(11) N4 0.0552(16) 0.0427(16) 0.0530(16) 0.0056(13) 0.0415(14) 0.0001(13) N5 0.0528(16) 0.0433(16) 0.0535(16) -0.0003(13) 0.0419(14) 0.0026(13) N3 0.0548(17) 0.0604(18) 0.0346(13) 0.0068(13) 0.0317(13) 0.0121(14) C2 0.0310(16) 0.0469(19) 0.0544(19) -0.0066(16) 0.0254(15) -0.0006(14) C1 0.0413(17) 0.0481(19) 0.0569(19) 0.0020(16) 0.0376(16) 0.0004(15) C3 0.0357(17) 0.067(2) 0.0339(16) -0.0057(16) 0.0146(14) 0.0077(16) C4 0.056(2) 0.072(2) 0.0364(17) 0.0118(17) 0.0245(16) 0.0212(19) C8 0.065(2) 0.042(2) 0.074(2) -0.0082(18) 0.051(2) 0.0022(17) C7 0.068(2) 0.043(2) 0.082(2) 0.0076(19) 0.053(2) 0.0030(18) C6 0.098(3) 0.076(3) 0.069(2) 0.020(2) 0.057(2) -0.005(2) C5 0.092(3) 0.089(3) 0.053(2) 0.020(2) 0.046(2) -0.008(2) _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 N1 2.642(3) . ? La1 N4 2.733(3) . ? La1 N3 2.734(3) . ? La1 N5 2.748(3) . ? La1 N2 2.750(3) . ? La1 S3 2.9844(11) . ? La1 S2 2.9980(13) . ? La1 S2 3.0644(9) 5_566 ? La1 S1 3.1247(18) . ? La1 As1 3.3417(8) . ? As1 S1 2.2269(10) . ? As1 S3 2.2443(12) . ? As1 S2 2.2485(9) . ? S2 La1 3.0644(9) 5_566 ? N1 C1 1.472(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.466(5) . ? N2 C3 1.479(5) . ? N2 H2C 0.9100 . ? N4 C7 1.455(5) . ? N4 C6 1.456(5) . ? N4 H4C 0.9100 . ? N5 C8 1.448(5) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N3 C4 1.479(5) . ? N3 C5 1.492(6) . ? N3 H3C 0.9100 . ? C2 C1 1.507(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C3 C4 1.495(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C8 C7 1.481(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6 C5 1.402(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 La1 N4 136.13(9) . . ? N1 La1 N3 126.44(9) . . ? N4 La1 N3 63.53(9) . . ? N1 La1 N5 73.85(9) . . ? N4 La1 N5 62.30(9) . . ? N3 La1 N5 96.80(9) . . ? N1 La1 N2 64.08(9) . . ? N4 La1 N2 102.15(9) . . ? N3 La1 N2 62.80(10) . . ? N5 La1 N2 73.05(9) . . ? N1 La1 S3 144.01(6) . . ? N4 La1 S3 74.16(7) . . ? N3 La1 S3 80.61(8) . . ? N5 La1 S3 131.73(6) . . ? N2 La1 S3 139.36(7) . . ? N1 La1 S2 73.26(6) . . ? N4 La1 S2 130.68(7) . . ? N3 La1 S2 139.42(7) . . ? N5 La1 S2 123.71(7) . . ? N2 La1 S2 127.00(7) . . ? S3 La1 S2 71.06(3) . . ? N1 La1 S2 90.37(7) . 5_566 ? N4 La1 S2 129.09(6) . 5_566 ? N3 La1 S2 72.42(7) . 5_566 ? N5 La1 S2 150.54(7) . 5_566 ? N2 La1 S2 77.70(6) . 5_566 ? S3 La1 S2 74.72(3) . 5_566 ? S2 La1 S2 72.48(3) . 5_566 ? N1 La1 S1 100.48(6) . . ? N4 La1 S1 69.22(7) . . ? N3 La1 S1 129.10(8) . . ? N5 La1 S1 76.52(7) . . ? N2 La1 S1 148.68(7) . . ? S3 La1 S1 69.13(3) . . ? S2 La1 S1 66.31(4) . . ? S2 La1 S1 131.75(2) 5_566 . ? N1 La1 As1 109.06(6) . . ? N4 La1 As1 90.25(7) . . ? N3 La1 As1 121.47(7) . . ? N5 La1 As1 116.59(7) . . ? N2 La1 As1 167.13(6) . . ? S3 La1 As1 41.07(2) . . ? S2 La1 As1 41.10(2) . . ? S2 La1 As1 91.85(3) 5_566 . ? S1 La1 As1 40.11(3) . . ? S1 As1 S3 101.73(4) . . ? S1 As1 S2 96.93(4) . . ? S3 As1 S2 101.39(4) . . ? S1 As1 La1 64.70(3) . . ? S3 As1 La1 60.89(4) . . ? S2 As1 La1 61.23(2) . . ? As1 S3 La1 78.03(4) . . ? As1 S2 La1 77.67(4) . . ? As1 S2 La1 116.71(3) . 5_566 ? La1 S2 La1 107.52(3) . 5_566 ? As1 S1 La1 75.19(3) . . ? C1 N1 La1 117.2(2) . . ? C1 N1 H1A 108.0 . . ? La1 N1 H1A 108.0 . . ? C1 N1 H1B 108.0 . . ? La1 N1 H1B 108.0 . . ? H1A N1 H1B 107.2 . . ? C2 N2 C3 112.6(3) . . ? C2 N2 La1 112.8(2) . . ? C3 N2 La1 111.6(2) . . ? C2 N2 H2C 106.4 . . ? C3 N2 H2C 106.4 . . ? La1 N2 H2C 106.4 . . ? C7 N4 C6 115.6(3) . . ? C7 N4 La1 118.1(2) . . ? C6 N4 La1 111.6(3) . . ? C7 N4 H4C 103.0 . . ? C6 N4 H4C 103.0 . . ? La1 N4 H4C 103.0 . . ? C8 N5 La1 114.2(2) . . ? C8 N5 H5A 108.7 . . ? La1 N5 H5A 108.7 . . ? C8 N5 H5B 108.7 . . ? La1 N5 H5B 108.7 . . ? H5A N5 H5B 107.6 . . ? C4 N3 C5 108.6(3) . . ? C4 N3 La1 117.8(2) . . ? C5 N3 La1 114.8(2) . . ? C4 N3 H3C 104.7 . . ? C5 N3 H3C 104.7 . . ? La1 N3 H3C 104.7 . . ? N2 C2 C1 111.6(3) . . ? N2 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C1 C2 109.9(3) . . ? N1 C1 H1C 109.7 . . ? C2 C1 H1C 109.7 . . ? N1 C1 H1D 109.7 . . ? C2 C1 H1D 109.7 . . ? H1C C1 H1D 108.2 . . ? N2 C3 C4 111.1(3) . . ? N2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N3 C4 C3 113.7(3) . . ? N3 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? N3 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N5 C8 C7 112.2(3) . . ? N5 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N5 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N4 C7 C8 113.4(3) . . ? N4 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N4 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C5 C6 N4 114.7(4) . . ? C5 C6 H6A 108.6 . . ? N4 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? N4 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C6 C5 N3 116.1(4) . . ? C6 C5 H5C 108.3 . . ? N3 C5 H5C 108.3 . . ? C6 C5 H5D 108.3 . . ? N3 C5 H5D 108.3 . . ? H5C C5 H5D 107.4 . . ? 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 N1 H1A S2 0.90 2.83 3.523(3) 134.5 2 N1 H1B S3 0.90 2.59 3.457(3) 162.1 5_566 N2 H2C S1 0.91 2.67 3.494(3) 151.9 8_556 N5 H5A S1 0.90 2.55 3.448(3) 172.4 2 N3 H3C S2 0.91 3.05 3.436(3) 107.2 5_566 N4 H4C S1 0.91 2.83 3.343(3) 117.3 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.274 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 913893'