# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof C. N. R. Rao' _publ_contact_author_address ; CPMU (JNCASR) & SSCU (IISc) JNCASR & SSCU CPMU, JNCASR, Jakkur P. O. Bangalor SSCU, IISc, Bangalore-560012, India Bangalore Karnataka INDIA ; _publ_contact_author_email CNRRAO@JNCASR.AC.IN _publ_section_title ; Organically templated rare earth sulfates with three-dimensional and layered structures ; loop_ _publ_author_name 'C. N. R. Rao' 'J. N. Behera' 'Meenakshi. Dan' data_Phase_I _database_code_depnum_ccdc_archive 'CCDC 224284' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H24 N4 Nd2 O22 S5' _chemical_formula_weight 929.05 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6032(12) _cell_length_b 16.986(3) _cell_length_c 20.412(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.845(3) _cell_angle_gamma 90.00 _cell_volume 2281.4(7) _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 rod _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.705 _exptl_crystal_density_method ? _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 5.070 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.815113 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17943 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4662 _reflns_number_observed 4163 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+9.6779P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4662 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_obs 0.0350 _refine_ls_wR_factor_all 0.0720 _refine_ls_wR_factor_obs 0.0696 _refine_ls_goodness_of_fit_all 1.115 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_all 1.115 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.43026(4) 0.25559(2) 0.494739(14) 0.00996(8) Uani 1 d . . Nd2 Nd 0.63796(4) 0.00980(2) 0.719898(14) 0.01057(8) Uani 1 d . . S1 S 1.1045(2) 0.04254(8) 0.74722(7) 0.0131(3) Uani 1 d . . S2 S 0.5072(2) 0.40011(8) 0.62727(7) 0.0118(3) Uani 1 d . . S3 S 0.5082(2) 0.13423(8) 0.60967(7) 0.0125(3) Uani 1 d . . S4 S -0.1258(2) 0.29242(8) 0.45914(7) 0.0118(3) Uani 1 d . . S5 S 0.3359(2) 0.13561(8) 0.37896(7) 0.0125(3) Uani 1 d . . O1 O 0.0630(6) 0.2620(2) 0.4927(2) 0.0210(9) Uani 1 d . . O2 O 0.3784(6) 0.3434(2) 0.5869(2) 0.0190(9) Uani 1 d . . O3 O 0.3680(8) 0.3748(3) 0.4260(3) 0.0200(10) Uani 1 d . . O4 O 0.6580(6) 0.1760(2) 0.5727(2) 0.0178(9) Uani 1 d . . O5 O -0.2453(6) 0.3324(2) 0.5073(2) 0.0172(9) Uani 1 d . . O6 O 0.3936(6) 0.1187(2) 0.4486(2) 0.0165(9) Uani 1 d . . O7 O 0.3083(6) 0.1627(2) 0.5825(2) 0.0155(8) Uani 1 d . . O8 O -0.2545(6) 0.2275(2) 0.4319(2) 0.0179(9) Uani 1 d . . O9 O 0.2971(6) 0.2202(2) 0.3741(2) 0.0201(9) Uani 1 d . . O10 O 1.2677(6) 0.0033(2) 0.7155(2) 0.0212(9) Uani 1 d . . O11 O 0.6340(9) 0.1043(3) 0.8111(2) 0.0258(11) Uani 1 d . . O12 O 0.9766(6) -0.0181(2) 0.7765(2) 0.0182(9) Uani 1 d . . O13 O 0.6105(6) -0.0750(2) 0.8176(2) 0.0219(9) Uani 1 d . . O14 O 0.4986(6) 0.1114(2) 0.3378(2) 0.0189(9) Uani 1 d . . O15 O 0.9640(6) 0.0813(2) 0.6971(2) 0.0164(8) Uani 1 d . . O16 O 0.5442(6) 0.1486(2) 0.6806(2) 0.0172(9) Uani 1 d . . O17 O 0.5285(6) 0.0482(2) 0.6011(2) 0.0176(9) Uani 1 d . . O18 O 0.1575(6) 0.0882(2) 0.3546(2) 0.0197(9) Uani 1 d . . O19 O 1.1877(7) 0.0971(3) 0.7968(2) 0.0306(11) Uani 1 d . . O20 O 0.5524(7) 0.4673(2) 0.5874(2) 0.0290(11) Uani 1 d . . O21 O 0.6944(6) 0.3617(3) 0.6530(2) 0.0307(11) Uani 1 d . . O22 O -0.0792(6) 0.3467(3) 0.4075(2) 0.0232(10) Uani 1 d . . N1 N 0.8337(8) 0.3256(3) 0.7797(3) 0.0248(12) Uani 1 d . . H21 H 0.7441(8) 0.3158(3) 0.8089(3) 0.037 Uiso 1 calc R . H20 H 0.7696(8) 0.3459(3) 0.7435(3) 0.037 Uiso 1 calc R . H19 H 0.9261(8) 0.3597(3) 0.7967(3) 0.037 Uiso 1 calc R . N2 N 1.0026(8) 0.2481(3) 0.6463(3) 0.0289(13) Uani 1 d . . H16 H 1.0973(8) 0.2560(3) 0.6185(3) 0.043 Uiso 1 calc R . H15 H 0.8983(8) 0.2804(3) 0.6364(3) 0.043 Uiso 1 calc R . H14 H 0.9599(8) 0.1985(3) 0.6432(3) 0.043 Uiso 1 calc R . N3 N 1.0077(9) 0.4773(4) 0.5889(3) 0.039(2) Uani 1 d . . H11 H 1.1044(9) 0.4568(4) 0.6168(3) 0.058 Uiso 1 calc R . H10 H 0.8981(9) 0.4466(4) 0.5872(3) 0.058 Uiso 1 calc R . H9 H 0.9757(9) 0.5251(4) 0.6025(3) 0.058 Uiso 1 calc R . N4 N 0.8180(10) 0.0538(4) 0.4409(3) 0.047(2) Uani 1 d . . H8 H 0.7475(10) 0.0978(4) 0.4453(3) 0.070 Uiso 1 calc R . H7 H 0.7327(10) 0.0141(4) 0.4312(3) 0.070 Uiso 1 calc R . H6 H 0.8998(10) 0.0597(4) 0.4088(3) 0.070 Uiso 1 calc R . C1 C 0.9354(9) 0.2513(3) 0.7632(3) 0.0201(13) Uani 1 d . . H18 H 0.8339(9) 0.2140(3) 0.7455(3) 0.024 Uiso 1 calc R . H17 H 1.0027(9) 0.2289(3) 0.8030(3) 0.024 Uiso 1 calc R . C2 C 1.0891(9) 0.2638(4) 0.7140(3) 0.0220(13) Uani 1 d . . H5 H 1.1378(9) 0.3177(4) 0.7170(3) 0.026 Uiso 1 calc R . H4 H 1.2042(9) 0.2292(4) 0.7243(3) 0.026 Uiso 1 calc R . C3 C 1.0810(9) 0.4828(4) 0.5238(3) 0.0201(13) Uani 1 d . . H13 H 1.1175(9) 0.4308(4) 0.5090(3) 0.024 Uiso 1 calc R . H12 H 1.2013(9) 0.5157(4) 0.5256(3) 0.024 Uiso 1 calc R . C4 C 0.9400(11) 0.0368(4) 0.5028(3) 0.033(2) Uani 1 d . . H3 H 0.8510(11) 0.0311(4) 0.5380(3) 0.040 Uiso 1 calc R . H2 H 1.0315(11) 0.0804(4) 0.5137(3) 0.040 Uiso 1 calc R . H23 H 0.4077(103) 0.4195(44) 0.4271(34) 0.026(20) Uiso 1 d . . H22 H 0.5447(154) 0.1184(61) 0.8178(51) 0.071(41) Uiso 1 d . . H21' H 0.3015(143) 0.3731(57) 0.4051(46) 0.052(38) Uiso 1 d . . H1 H 0.7265(141) 0.1210(52) 0.8317(45) 0.056(31) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.00921(15) 0.01051(14) 0.0102(2) -0.00053(11) 0.00113(10) 0.00029(11) Nd2 0.00959(15) 0.01173(15) 0.0103(2) 0.00117(11) 0.00026(11) -0.00055(11) S1 0.0084(6) 0.0156(7) 0.0153(7) -0.0020(6) 0.0012(5) 0.0006(5) S2 0.0117(6) 0.0124(6) 0.0112(7) -0.0041(5) 0.0004(5) 0.0022(5) S3 0.0138(7) 0.0119(6) 0.0117(7) 0.0026(5) 0.0004(5) 0.0018(5) S4 0.0062(6) 0.0172(7) 0.0119(7) 0.0011(5) 0.0007(5) -0.0001(5) S5 0.0137(7) 0.0123(6) 0.0115(7) -0.0031(5) 0.0002(5) 0.0006(5) O1 0.011(2) 0.031(2) 0.020(2) 0.003(2) -0.002(2) 0.003(2) O2 0.016(2) 0.023(2) 0.018(2) -0.008(2) 0.002(2) -0.002(2) O3 0.020(3) 0.013(2) 0.026(3) 0.003(2) -0.003(2) -0.001(2) O4 0.012(2) 0.020(2) 0.021(2) 0.009(2) 0.003(2) 0.001(2) O5 0.011(2) 0.018(2) 0.023(2) -0.006(2) 0.004(2) -0.003(2) O6 0.028(2) 0.012(2) 0.009(2) 0.001(2) -0.002(2) 0.000(2) O7 0.013(2) 0.017(2) 0.016(2) 0.005(2) 0.000(2) 0.002(2) O8 0.009(2) 0.022(2) 0.022(2) -0.005(2) 0.000(2) -0.005(2) O9 0.026(2) 0.014(2) 0.018(2) -0.003(2) -0.006(2) 0.003(2) O10 0.010(2) 0.026(2) 0.028(2) 0.000(2) 0.008(2) 0.006(2) O11 0.023(3) 0.035(3) 0.020(3) -0.009(2) 0.005(2) -0.001(2) O12 0.009(2) 0.031(2) 0.015(2) 0.010(2) 0.002(2) 0.002(2) O13 0.022(2) 0.027(2) 0.018(2) 0.011(2) 0.007(2) 0.000(2) O14 0.020(2) 0.015(2) 0.023(2) -0.002(2) 0.007(2) 0.000(2) O15 0.014(2) 0.018(2) 0.017(2) 0.005(2) -0.004(2) 0.001(2) O16 0.025(2) 0.016(2) 0.011(2) 0.002(2) -0.001(2) 0.004(2) O17 0.027(2) 0.012(2) 0.014(2) 0.003(2) 0.003(2) 0.001(2) O18 0.013(2) 0.020(2) 0.025(2) -0.007(2) -0.002(2) -0.003(2) O19 0.029(3) 0.033(3) 0.028(3) -0.012(2) -0.011(2) 0.002(2) O20 0.039(3) 0.018(2) 0.030(3) 0.000(2) 0.008(2) -0.005(2) O21 0.021(2) 0.040(3) 0.030(3) -0.008(2) -0.009(2) 0.017(2) O22 0.021(2) 0.031(2) 0.018(2) 0.009(2) 0.001(2) -0.006(2) N1 0.023(3) 0.028(3) 0.023(3) -0.007(2) 0.004(2) 0.002(2) N2 0.028(3) 0.037(3) 0.023(3) -0.007(3) 0.008(2) 0.008(2) N3 0.027(3) 0.066(4) 0.023(3) 0.013(3) 0.002(2) 0.002(3) N4 0.046(4) 0.039(4) 0.053(4) 0.000(3) -0.014(3) 0.011(3) C1 0.022(3) 0.020(3) 0.018(3) 0.002(3) 0.003(2) -0.003(2) C2 0.018(3) 0.023(3) 0.024(3) -0.001(3) 0.001(3) -0.001(2) C3 0.020(3) 0.025(3) 0.015(3) 0.001(3) 0.002(2) 0.001(3) C4 0.036(4) 0.032(4) 0.030(4) 0.002(3) 0.000(3) 0.007(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 Nd1 O1 2.424(4) . ? Nd1 O2 2.448(4) . ? Nd1 O3 2.478(5) . ? Nd1 O4 2.493(4) . ? Nd1 O5 2.503(4) 1_655 ? Nd1 O6 2.512(4) . ? Nd1 O7 2.568(4) . ? Nd1 O8 2.580(4) 1_655 ? Nd1 O9 2.615(4) . ? Nd1 S3 3.1328(14) . ? Nd1 S4 3.1420(14) 1_655 ? Nd1 S5 3.1430(14) . ? Nd2 O10 2.442(4) 1_455 ? Nd2 O11 2.460(5) . ? Nd2 O12 2.474(4) . ? Nd2 O13 2.479(4) . ? Nd2 O14 2.502(4) 3_656 ? Nd2 O15 2.549(4) . ? Nd2 O16 2.549(4) . ? Nd2 O17 2.557(4) . ? Nd2 O18 2.693(4) 3_656 ? Nd2 S1 3.1338(14) . ? Nd2 S3 3.1525(14) . ? Nd2 S5 3.2033(14) 3_656 ? S1 O19 1.446(4) . ? S1 O10 1.464(4) . ? S1 O15 1.476(4) . ? S1 O12 1.489(4) . ? S2 O20 1.447(4) . ? S2 O21 1.456(4) . ? S2 O13 1.483(4) 2_656 ? S2 O2 1.487(4) . ? S3 O16 1.469(4) . ? S3 O7 1.470(4) . ? S3 O4 1.476(4) . ? S3 O17 1.479(4) . ? S4 O22 1.453(4) . ? S4 O1 1.465(4) . ? S4 O8 1.472(4) . ? S4 O5 1.477(4) . ? S4 Nd1 3.1420(14) 1_455 ? S5 O9 1.461(4) . ? S5 O6 1.469(4) . ? S5 O14 1.477(4) . ? S5 O18 1.478(4) . ? S5 Nd2 3.2033(14) 3_656 ? O5 Nd1 2.503(4) 1_455 ? O8 Nd1 2.580(4) 1_455 ? O10 Nd2 2.442(4) 1_655 ? O13 S2 1.482(4) 2_646 ? O14 Nd2 2.502(4) 3_656 ? O18 Nd2 2.693(4) 3_656 ? N1 C1 1.481(7) . ? N2 C2 1.473(8) . ? N3 C3 1.456(8) . ? N4 C4 1.468(9) . ? C1 C2 1.502(8) . ? C3 C3 1.501(11) 3_766 ? C4 C4 1.489(13) 3_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O2 77.38(13) . . ? O1 Nd1 O3 80.5(2) . . ? O2 Nd1 O3 84.8(2) . . ? O1 Nd1 O4 125.73(13) . . ? O2 Nd1 O4 87.46(13) . . ? O3 Nd1 O4 150.1(2) . . ? O1 Nd1 O5 145.57(13) . 1_655 ? O2 Nd1 O5 77.15(13) . 1_655 ? O3 Nd1 O5 74.4(2) . 1_655 ? O4 Nd1 O5 75.64(13) . 1_655 ? O1 Nd1 O6 88.30(14) . . ? O2 Nd1 O6 146.79(13) . . ? O3 Nd1 O6 122.5(2) . . ? O4 Nd1 O6 76.78(12) . . ? O5 Nd1 O6 125.12(13) 1_655 . ? O1 Nd1 O7 70.57(13) . . ? O2 Nd1 O7 76.46(13) . . ? O3 Nd1 O7 148.27(14) . . ? O4 Nd1 O7 55.21(12) . . ? O5 Nd1 O7 124.41(13) 1_655 . ? O6 Nd1 O7 70.52(12) . . ? O1 Nd1 O8 147.95(13) . 1_655 ? O2 Nd1 O8 131.75(12) . 1_655 ? O3 Nd1 O8 88.41(15) . 1_655 ? O4 Nd1 O8 75.41(13) . 1_655 ? O5 Nd1 O8 55.10(12) 1_655 1_655 ? O6 Nd1 O8 72.46(13) . 1_655 ? O7 Nd1 O8 123.14(12) . 1_655 ? O1 Nd1 O9 74.78(13) . . ? O2 Nd1 O9 143.77(13) . . ? O3 Nd1 O9 68.2(2) . . ? O4 Nd1 O9 127.83(13) . . ? O5 Nd1 O9 115.69(13) 1_655 . ? O6 Nd1 O9 54.55(12) . . ? O7 Nd1 O9 114.54(13) . . ? O8 Nd1 O9 73.18(12) 1_655 . ? O1 Nd1 S3 98.24(10) . . ? O2 Nd1 S3 81.38(10) . . ? O3 Nd1 S3 166.08(13) . . ? O4 Nd1 S3 27.54(9) . . ? O5 Nd1 S3 100.43(10) 1_655 . ? O6 Nd1 S3 71.10(9) . . ? O7 Nd1 S3 27.68(8) . . ? O8 Nd1 S3 99.31(9) 1_655 . ? O9 Nd1 S3 125.10(9) . . ? O1 Nd1 S4 159.81(10) . 1_655 ? O2 Nd1 S4 104.49(9) . 1_655 ? O3 Nd1 S4 79.62(12) . 1_655 ? O4 Nd1 S4 74.41(9) . 1_655 ? O5 Nd1 S4 27.47(9) 1_655 1_655 ? O6 Nd1 S4 99.19(10) . 1_655 ? O7 Nd1 S4 129.61(9) . 1_655 ? O8 Nd1 S4 27.65(9) 1_655 1_655 ? O9 Nd1 S4 94.25(10) . 1_655 ? S3 Nd1 S4 101.93(4) . 1_655 ? O1 Nd1 S5 83.19(10) . . ? O2 Nd1 S5 160.30(9) . . ? O3 Nd1 S5 95.24(13) . . ? O4 Nd1 S5 101.48(10) . . ? O5 Nd1 S5 121.92(9) 1_655 . ? O6 Nd1 S5 27.31(9) . . ? O7 Nd1 S5 94.13(9) . . ? O8 Nd1 S5 67.87(9) 1_655 . ? O9 Nd1 S5 27.49(9) . . ? S3 Nd1 S5 98.39(4) . . ? S4 Nd1 S5 94.86(4) 1_655 . ? O10 Nd2 O11 89.0(2) 1_455 . ? O10 Nd2 O12 150.61(14) 1_455 . ? O11 Nd2 O12 80.7(2) . . ? O10 Nd2 O13 82.10(14) 1_455 . ? O11 Nd2 O13 76.4(2) . . ? O12 Nd2 O13 68.76(13) . . ? O10 Nd2 O14 68.01(13) 1_455 3_656 ? O11 Nd2 O14 150.1(2) . 3_656 ? O12 Nd2 O14 109.72(13) . 3_656 ? O13 Nd2 O14 81.52(14) . 3_656 ? O10 Nd2 O15 150.86(13) 1_455 . ? O11 Nd2 O15 83.7(2) . . ? O12 Nd2 O15 55.42(12) . . ? O13 Nd2 O15 122.95(13) . . ? O14 Nd2 O15 125.65(13) 3_656 . ? O10 Nd2 O16 79.30(13) 1_455 . ? O11 Nd2 O16 67.4(2) . . ? O12 Nd2 O16 120.65(13) . . ? O13 Nd2 O16 139.28(13) . . ? O14 Nd2 O16 123.01(13) 3_656 . ? O15 Nd2 O16 71.84(12) . . ? O10 Nd2 O17 76.97(14) 1_455 . ? O11 Nd2 O17 122.1(2) . . ? O12 Nd2 O17 131.58(13) . . ? O13 Nd2 O17 151.34(13) . . ? O14 Nd2 O17 72.64(13) 3_656 . ? O15 Nd2 O17 83.16(12) . . ? O16 Nd2 O17 54.84(12) . . ? O10 Nd2 O18 119.98(13) 1_455 3_656 ? O11 Nd2 O18 150.3(2) . 3_656 ? O12 Nd2 O18 70.63(13) . 3_656 ? O13 Nd2 O18 99.72(13) . 3_656 ? O14 Nd2 O18 53.39(12) 3_656 3_656 ? O15 Nd2 O18 73.75(12) . 3_656 ? O16 Nd2 O18 120.96(12) . 3_656 ? O17 Nd2 O18 74.78(12) . 3_656 ? O10 Nd2 S1 168.78(10) 1_455 . ? O11 Nd2 S1 79.79(15) . . ? O12 Nd2 S1 27.74(9) . . ? O13 Nd2 S1 95.59(10) . . ? O14 Nd2 S1 122.66(9) 3_656 . ? O15 Nd2 S1 27.75(9) . . ? O16 Nd2 S1 95.78(9) . . ? O17 Nd2 S1 108.57(9) . . ? O18 Nd2 S1 71.21(8) 3_656 . ? O10 Nd2 S3 78.06(10) 1_455 . ? O11 Nd2 S3 94.74(13) . . ? O12 Nd2 S3 129.94(9) . . ? O13 Nd2 S3 158.41(10) . . ? O14 Nd2 S3 98.65(10) 3_656 . ? O15 Nd2 S3 74.52(9) . . ? O16 Nd2 S3 27.32(9) . . ? O17 Nd2 S3 27.59(9) . . ? O18 Nd2 S3 97.51(9) 3_656 . ? S1 Nd2 S3 102.23(4) . . ? O10 Nd2 S5 92.81(10) 1_455 3_656 ? O11 Nd2 S5 169.91(13) . 3_656 ? O12 Nd2 S5 92.95(10) . 3_656 ? O13 Nd2 S5 94.02(10) . 3_656 ? O14 Nd2 S5 26.55(9) 3_656 3_656 ? O15 Nd2 S5 99.28(9) . 3_656 ? O16 Nd2 S5 122.66(9) . 3_656 ? O17 Nd2 S5 67.97(9) . 3_656 ? O18 Nd2 S5 27.32(8) 3_656 3_656 ? S1 Nd2 S5 98.31(4) . 3_656 ? S3 Nd2 S5 95.35(4) . 3_656 ? O19 S1 O10 110.5(3) . . ? O19 S1 O15 112.2(3) . . ? O10 S1 O15 109.8(2) . . ? O19 S1 O12 111.0(3) . . ? O10 S1 O12 109.0(2) . . ? O15 S1 O12 104.0(2) . . ? O19 S1 Nd2 123.2(2) . . ? O10 S1 Nd2 126.1(2) . . ? O15 S1 Nd2 53.5(2) . . ? O12 S1 Nd2 50.66(15) . . ? O20 S2 O21 110.3(3) . . ? O20 S2 O13 110.4(3) . 2_656 ? O21 S2 O13 109.7(3) . 2_656 ? O20 S2 O2 109.5(3) . . ? O21 S2 O2 109.7(3) . . ? O13 S2 O2 107.0(2) 2_656 . ? O16 S3 O7 112.5(2) . . ? O16 S3 O4 111.4(2) . . ? O7 S3 O4 105.6(2) . . ? O16 S3 O17 105.8(2) . . ? O7 S3 O17 111.5(2) . . ? O4 S3 O17 110.1(2) . . ? O16 S3 Nd1 129.2(2) . . ? O7 S3 Nd1 54.2(2) . . ? O4 S3 Nd1 51.33(15) . . ? O17 S3 Nd1 124.9(2) . . ? O16 S3 Nd2 52.8(2) . . ? O7 S3 Nd2 132.1(2) . . ? O4 S3 Nd2 122.3(2) . . ? O17 S3 Nd2 53.2(2) . . ? Nd1 S3 Nd2 173.33(5) . . ? O22 S4 O1 109.8(2) . . ? O22 S4 O8 110.6(2) . . ? O1 S4 O8 110.7(2) . . ? O22 S4 O5 110.5(2) . . ? O1 S4 O5 109.4(2) . . ? O8 S4 O5 105.8(2) . . ? O22 S4 Nd1 123.6(2) . 1_455 ? O1 S4 Nd1 126.5(2) . 1_455 ? O8 S4 Nd1 54.4(2) . 1_455 ? O5 S4 Nd1 51.41(15) . 1_455 ? O9 S5 O6 106.7(2) . . ? O9 S5 O14 111.5(2) . . ? O6 S5 O14 110.8(2) . . ? O9 S5 O18 112.5(2) . . ? O6 S5 O18 110.8(2) . . ? O14 S5 O18 104.7(2) . . ? O9 S5 Nd1 55.7(2) . . ? O6 S5 Nd1 51.67(15) . . ? O14 S5 Nd1 120.1(2) . . ? O18 S5 Nd1 135.1(2) . . ? O9 S5 Nd2 137.2(2) . 3_656 ? O6 S5 Nd2 115.9(2) . 3_656 ? O14 S5 Nd2 49.2(2) . 3_656 ? O18 S5 Nd2 56.7(2) . 3_656 ? Nd1 S5 Nd2 162.92(5) . 3_656 ? S4 O1 Nd1 146.5(3) . . ? S2 O2 Nd1 135.2(2) . . ? S3 O4 Nd1 101.1(2) . . ? S4 O5 Nd1 101.1(2) . 1_455 ? S5 O6 Nd1 101.0(2) . . ? S3 O7 Nd1 98.1(2) . . ? S4 O8 Nd1 97.9(2) . 1_455 ? S5 O9 Nd1 96.8(2) . . ? S1 O10 Nd2 137.3(3) . 1_655 ? S1 O12 Nd2 101.6(2) . . ? S2 O13 Nd2 148.8(2) 2_646 . ? S5 O14 Nd2 104.3(2) . 3_656 ? S1 O15 Nd2 98.7(2) . . ? S3 O16 Nd2 99.9(2) . . ? S3 O17 Nd2 99.2(2) . . ? S5 O18 Nd2 95.9(2) . 3_656 ? N1 C1 C2 112.2(5) . . ? N2 C2 C1 111.8(5) . . ? N3 C3 C3 110.0(6) . 3_766 ? N4 C4 C4 110.8(7) . 3_756 ? _refine_diff_density_max 0.959 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.176 #===ENd data_Phase_II _database_code_depnum_ccdc_archive 'CCDC 224285' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H16 N2 Nd2 O18 S4' _chemical_formula_weight 796.91 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6210(4) _cell_length_b 11.7941(6) _cell_length_c 12.2064(7) _cell_angle_alpha 90.8460(10) _cell_angle_beta 100.5770(10) _cell_angle_gamma 102.4460(10) _cell_volume 913.50(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour 'faint pink' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.897 _exptl_crystal_density_method ? _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 6.176 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.575331 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5524 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2611 _reflns_number_observed 2229 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2611 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_obs 0.0283 _refine_ls_wR_factor_all 0.0679 _refine_ls_wR_factor_obs 0.0660 _refine_ls_goodness_of_fit_all 0.976 _refine_ls_goodness_of_fit_obs 1.037 _refine_ls_restrained_S_all 0.976 _refine_ls_restrained_S_obs 1.037 _refine_ls_shift/esd_max 0.311 _refine_ls_shift/esd_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.34661(5) 0.42056(3) 0.12960(3) 0.00938(13) Uani 1 d . . Nd2 Nd 0.73274(5) 0.86706(3) 0.44785(3) 0.00967(13) Uani 1 d . . S1 S 1.1599(3) 0.88028(15) 0.35798(13) 0.0116(4) Uani 1 d . . S2 S 0.5331(3) 0.65708(14) 0.27418(13) 0.0123(4) Uani 1 d . . S3 S 0.7627(3) 0.35265(14) 0.07308(13) 0.0109(4) Uani 1 d . . S4 S 0.2641(3) 0.24731(15) 0.31931(13) 0.0124(4) Uani 1 d . . O1 O 0.9763(7) 0.4161(4) 0.1223(4) 0.0175(11) Uani 1 d . . O2 O 0.6443(7) 0.4353(4) 0.0114(3) 0.0124(10) Uani 1 d . . O3 O 0.3525(8) 0.3751(4) 0.3266(4) 0.0172(11) Uani 1 d . . O4 O 0.1796(10) 0.2974(5) -0.0417(4) 0.0227(13) Uani 1 d . . O5 O 0.6394(7) 0.3119(4) 0.1599(4) 0.0167(11) Uani 1 d . . O6 O 0.3091(7) 0.6012(4) 0.2349(4) 0.0162(11) Uani 1 d . . O7 O 0.6514(7) 0.5855(4) 0.2213(4) 0.0165(11) Uani 1 d . . O8 O 0.1973(7) 0.2125(4) 0.1999(4) 0.0188(11) Uani 1 d . . O9 O 1.3738(7) 0.8838(5) 0.4196(4) 0.0269(13) Uani 1 d . . O10 O 0.5862(7) 0.7805(4) 0.2469(4) 0.0162(11) Uani 1 d . . O11 O 1.0841(7) 0.9777(4) 0.4101(4) 0.0142(11) Uani 1 d . . O12 O 0.5896(7) 0.6565(4) 0.3984(3) 0.0154(11) Uani 1 d . . O13 O 0.4235(7) 0.1871(4) 0.3801(4) 0.0160(11) Uani 1 d . . O14 O 1.0099(7) 0.7760(4) 0.3816(4) 0.0222(12) Uani 1 d . . O15 O 0.6977(10) 1.0473(5) 0.3380(4) 0.0196(13) Uani 1 d . . O16 O 0.0876(7) 0.2203(4) 0.3811(4) 0.0177(11) Uani 1 d . . O17 O 1.1553(8) 0.8951(5) 0.2408(4) 0.0273(13) Uani 1 d . . O18 O 0.7700(7) 0.2563(4) -0.0017(4) 0.0169(11) Uani 1 d . . N1 N 0.5264(9) 0.0453(5) -0.1047(4) 0.0202(14) Uani 1 d . . H12 H 0.5868(9) 0.1204(5) -0.0842(4) 0.024 Uiso 1 calc R . H11 H 0.5130(9) 0.0363(5) -0.1792(4) 0.024 Uiso 1 calc R . N2 N 1.0321(13) 0.5286(9) 0.3927(6) 0.059(3) Uani 1 d . . H10 H 1.0762(13) 0.5140(9) 0.3295(6) 0.071 Uiso 1 calc R . H9 H 0.9787(13) 0.5926(9) 0.3846(6) 0.071 Uiso 1 calc R . C1 C 0.6664(13) -0.0289(7) -0.0501(6) 0.028(2) Uani 1 d . . H8 H 0.8047(13) -0.0053(7) -0.0692(6) 0.034 Uiso 1 calc R . H7 H 0.6086(13) -0.1095(7) -0.0764(6) 0.034 Uiso 1 calc R . C2 C 0.3147(12) 0.0173(7) -0.0756(6) 0.027(2) Uani 1 d . . H6 H 0.2437(12) -0.0615(7) -0.1028(6) 0.032 Uiso 1 calc R . H5 H 0.2314(12) 0.0697(7) -0.1110(6) 0.032 Uiso 1 calc R . C3 C 1.2067(13) 0.5477(10) 0.4857(7) 0.055(3) Uani 1 d . . H4 H 1.3156(13) 0.6129(10) 0.4730(7) 0.066 Uiso 1 calc R . H3 H 1.2663(13) 0.4793(10) 0.4934(7) 0.066 Uiso 1 calc R . C4 C 0.8672(17) 0.4283(7) 0.4128(8) 0.056(3) Uani 1 d . . H2 H 0.7501(17) 0.4142(7) 0.3499(8) 0.067 Uiso 1 calc R . H1 H 0.9244(17) 0.3591(7) 0.4203(8) 0.067 Uiso 1 calc R . H15 H 0.6315(117) 1.0797(62) 0.3634(59) 0.012(23) Uiso 1 d . . H14 H 0.7798(137) 1.1010(77) 0.3223(71) 0.035(30) Uiso 1 d . . H13 H 0.1932(154) 0.3229(85) -0.1145(90) 0.066(34) Uiso 1 d . . H16 H 0.0618(198) 0.2930(112) -0.0441(108) 0.120(56) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0088(2) 0.0100(2) 0.0098(2) 0.00004(15) 0.0038(2) 0.0016(2) Nd2 0.0080(2) 0.0103(2) 0.0105(2) -0.00005(15) 0.00291(15) 0.0006(2) S1 0.0107(9) 0.0136(10) 0.0119(8) -0.0011(7) 0.0046(7) 0.0035(7) S2 0.0150(10) 0.0106(9) 0.0113(8) -0.0006(7) 0.0042(7) 0.0016(8) S3 0.0097(9) 0.0113(9) 0.0129(8) 0.0005(7) 0.0036(7) 0.0037(7) S4 0.0137(10) 0.0118(9) 0.0133(8) 0.0031(7) 0.0054(7) 0.0033(7) O1 0.010(3) 0.020(3) 0.021(3) -0.003(2) 0.002(2) 0.002(2) O2 0.011(3) 0.014(3) 0.015(2) 0.002(2) 0.005(2) 0.008(2) O3 0.026(3) 0.012(3) 0.014(2) 0.008(2) 0.005(2) 0.002(2) O4 0.019(3) 0.027(3) 0.020(3) -0.007(2) 0.008(2) -0.002(3) O5 0.019(3) 0.020(3) 0.017(2) 0.009(2) 0.011(2) 0.009(2) O6 0.012(3) 0.018(3) 0.017(2) -0.005(2) 0.002(2) 0.000(2) O7 0.015(3) 0.016(3) 0.020(2) -0.005(2) 0.006(2) 0.005(2) O8 0.025(3) 0.020(3) 0.012(2) 0.000(2) 0.004(2) 0.006(2) O9 0.009(3) 0.045(4) 0.027(3) 0.000(2) 0.003(2) 0.006(2) O10 0.017(3) 0.015(3) 0.015(2) 0.000(2) 0.003(2) 0.002(2) O11 0.012(3) 0.009(3) 0.023(3) -0.003(2) 0.009(2) 0.001(2) O12 0.023(3) 0.013(3) 0.010(2) 0.002(2) 0.003(2) 0.004(2) O13 0.010(3) 0.022(3) 0.019(2) 0.007(2) 0.007(2) 0.006(2) O14 0.018(3) 0.015(3) 0.036(3) 0.001(2) 0.012(2) 0.000(2) O15 0.020(3) 0.018(3) 0.024(3) 0.002(2) 0.011(3) 0.006(3) O16 0.018(3) 0.022(3) 0.019(2) 0.008(2) 0.010(2) 0.010(2) O17 0.032(3) 0.043(3) 0.014(2) 0.004(2) 0.011(2) 0.016(3) O18 0.016(3) 0.012(3) 0.024(3) -0.004(2) 0.007(2) 0.004(2) N1 0.030(4) 0.018(4) 0.014(3) 0.003(3) 0.008(3) 0.003(3) N2 0.053(6) 0.113(8) 0.031(4) 0.021(5) 0.024(4) 0.047(6) C1 0.032(5) 0.024(5) 0.038(5) 0.010(4) 0.020(4) 0.012(4) C2 0.027(5) 0.026(5) 0.026(4) 0.015(4) 0.004(4) 0.004(4) C3 0.007(5) 0.106(9) 0.048(6) 0.058(6) 0.007(4) -0.001(5) C4 0.071(8) 0.015(5) 0.061(7) -0.017(5) -0.046(6) 0.019(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 Nd1 O1 2.426(4) 1_455 ? Nd1 O2 2.437(4) 2_665 ? Nd1 O4 2.465(5) . ? Nd1 O3 2.466(4) . ? Nd1 O5 2.522(5) . ? Nd1 O6 2.552(4) . ? Nd1 O7 2.555(4) . ? Nd1 O2 2.626(4) . ? Nd1 O8 2.658(5) . ? Nd1 S4 3.156(2) . ? Nd1 S2 3.161(2) . ? Nd1 S3 3.215(2) . ? Nd2 O9 2.389(5) 1_455 ? Nd2 O11 2.451(4) 2_776 ? Nd2 O12 2.482(4) . ? Nd2 O11 2.536(4) . ? Nd2 O13 2.538(4) 2_666 ? Nd2 O16 2.553(5) 2_666 ? Nd2 O14 2.558(5) . ? Nd2 O15 2.560(6) . ? Nd2 O10 2.574(4) . ? Nd2 S2 3.127(2) . ? Nd2 S4 3.162(2) 2_666 ? Nd2 S1 3.191(2) . ? S1 O17 1.440(5) . ? S1 O9 1.468(5) . ? S1 O14 1.473(5) . ? S1 O11 1.524(4) . ? S2 O6 1.474(5) . ? S2 O10 1.480(5) . ? S2 O7 1.482(5) . ? S2 O12 1.495(4) . ? S3 O18 1.461(4) . ? S3 O1 1.463(5) . ? S3 O5 1.478(5) . ? S3 O2 1.505(5) . ? S4 O8 1.468(5) . ? S4 O16 1.485(5) . ? S4 O3 1.490(5) . ? S4 O13 1.490(5) . ? S4 Nd2 3.162(2) 2_666 ? O1 Nd1 2.426(4) 1_655 ? O2 Nd1 2.437(4) 2_665 ? O9 Nd2 2.389(5) 1_655 ? O11 Nd2 2.451(4) 2_776 ? O13 Nd2 2.538(4) 2_666 ? O16 Nd2 2.553(5) 2_666 ? N1 C2 1.479(9) . ? N1 C1 1.487(9) . ? N2 C3 1.441(11) . ? N2 C4 1.484(12) . ? C1 C2 1.518(10) 2_655 ? C2 C1 1.518(10) 2_655 ? C3 C4 1.459(13) 2_766 ? C4 C3 1.459(13) 2_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O2 89.6(2) 1_455 2_665 ? O1 Nd1 O4 78.1(2) 1_455 . ? O2 Nd1 O4 78.7(2) 2_665 . ? O1 Nd1 O3 85.0(2) 1_455 . ? O2 Nd1 O3 148.86(14) 2_665 . ? O4 Nd1 O3 129.5(2) . . ? O1 Nd1 O5 147.8(2) 1_455 . ? O2 Nd1 O5 117.38(14) 2_665 . ? O4 Nd1 O5 89.7(2) . . ? O3 Nd1 O5 80.02(15) . . ? O1 Nd1 O6 70.34(14) 1_455 . ? O2 Nd1 O6 77.12(14) 2_665 . ? O4 Nd1 O6 140.0(2) . . ? O3 Nd1 O6 72.18(15) . . ? O5 Nd1 O6 129.83(14) . . ? O1 Nd1 O7 125.05(14) 1_455 . ? O2 Nd1 O7 77.15(15) 2_665 . ? O4 Nd1 O7 146.0(2) . . ? O3 Nd1 O7 81.01(15) . . ? O5 Nd1 O7 80.60(15) . . ? O6 Nd1 O7 54.76(14) . . ? O1 Nd1 O2 144.93(14) 1_455 . ? O2 Nd1 O2 63.5(2) 2_665 . ? O4 Nd1 O2 74.9(2) . . ? O3 Nd1 O2 129.68(15) . . ? O5 Nd1 O2 54.07(14) . . ? O6 Nd1 O2 120.05(14) . . ? O7 Nd1 O2 72.96(13) . . ? O1 Nd1 O8 76.2(2) 1_455 . ? O2 Nd1 O8 152.05(14) 2_665 . ? O4 Nd1 O8 74.9(2) . . ? O3 Nd1 O8 54.87(14) . . ? O5 Nd1 O8 71.83(15) . . ? O6 Nd1 O8 118.76(14) . . ? O7 Nd1 O8 130.68(15) . . ? O2 Nd1 O8 116.92(14) . . ? O1 Nd1 S4 81.09(12) 1_455 . ? O2 Nd1 S4 170.08(10) 2_665 . ? O4 Nd1 S4 102.49(15) . . ? O3 Nd1 S4 27.38(11) . . ? O5 Nd1 S4 72.54(11) . . ? O6 Nd1 S4 96.41(11) . . ? O7 Nd1 S4 105.45(11) . . ? O2 Nd1 S4 126.38(10) . . ? O8 Nd1 S4 27.58(10) . . ? O1 Nd1 S2 97.67(11) 1_455 . ? O2 Nd1 S2 77.35(10) 2_665 . ? O4 Nd1 S2 155.70(14) . . ? O3 Nd1 S2 73.05(11) . . ? O5 Nd1 S2 104.89(11) . . ? O6 Nd1 S2 27.34(10) . . ? O7 Nd1 S2 27.54(10) . . ? O2 Nd1 S2 97.72(10) . . ? O8 Nd1 S2 127.80(10) . . ? S4 Nd1 S2 100.43(4) . . ? O1 Nd1 S3 159.55(10) 1_455 . ? O2 Nd1 S3 90.96(10) 2_665 . ? O4 Nd1 S3 81.94(15) . . ? O3 Nd1 S3 104.50(12) . . ? O5 Nd1 S3 26.50(10) . . ? O6 Nd1 S3 129.58(11) . . ? O7 Nd1 S3 74.87(10) . . ? O2 Nd1 S3 27.58(10) . . ? O8 Nd1 S3 94.28(10) . . ? S4 Nd1 S3 98.97(4) . . ? S2 Nd1 S3 102.39(4) . . ? O9 Nd2 O11 103.8(2) 1_455 2_776 ? O9 Nd2 O12 86.1(2) 1_455 . ? O11 Nd2 O12 148.78(15) 2_776 . ? O9 Nd2 O11 139.2(2) 1_455 . ? O11 Nd2 O11 66.4(2) 2_776 . ? O12 Nd2 O11 123.61(14) . . ? O9 Nd2 O13 69.1(2) 1_455 2_666 ? O11 Nd2 O13 74.94(14) 2_776 2_666 ? O12 Nd2 O13 81.44(14) . 2_666 ? O11 Nd2 O13 135.95(14) . 2_666 ? O9 Nd2 O16 123.4(2) 1_455 2_666 ? O11 Nd2 O16 70.35(15) 2_776 2_666 ? O12 Nd2 O16 79.44(15) . 2_666 ? O11 Nd2 O16 91.74(15) . 2_666 ? O13 Nd2 O16 54.78(14) 2_666 2_666 ? O9 Nd2 O14 147.6(2) 1_455 . ? O11 Nd2 O14 108.02(15) 2_776 . ? O12 Nd2 O14 69.7(2) . . ? O11 Nd2 O14 54.44(14) . . ? O13 Nd2 O14 125.1(2) 2_666 . ? O16 Nd2 O14 74.20(15) 2_666 . ? O9 Nd2 O15 71.4(2) 1_455 . ? O11 Nd2 O15 79.2(2) 2_776 . ? O12 Nd2 O15 131.7(2) . . ? O11 Nd2 O15 67.9(2) . . ? O13 Nd2 O15 125.1(2) 2_666 . ? O16 Nd2 O15 148.4(2) 2_666 . ? O14 Nd2 O15 108.7(2) . . ? O9 Nd2 O10 77.4(2) 1_455 . ? O11 Nd2 O10 154.68(15) 2_776 . ? O12 Nd2 O10 55.99(14) . . ? O11 Nd2 O10 95.88(14) . . ? O13 Nd2 O10 127.09(15) 2_666 . ? O16 Nd2 O10 130.60(15) 2_666 . ? O14 Nd2 O10 71.33(15) . . ? O15 Nd2 O10 77.3(2) . . ? O9 Nd2 S2 81.10(12) 1_455 . ? O11 Nd2 S2 174.64(11) 2_776 . ? O12 Nd2 S2 28.00(10) . . ? O11 Nd2 S2 111.45(10) . . ? O13 Nd2 S2 105.15(11) 2_666 . ? O16 Nd2 S2 105.19(11) 2_666 . ? O14 Nd2 S2 67.40(11) . . ? O15 Nd2 S2 104.71(12) . . ? O10 Nd2 S2 27.99(11) . . ? O9 Nd2 S4 95.80(13) 1_455 2_666 ? O11 Nd2 S4 73.91(11) 2_776 2_666 ? O12 Nd2 S4 75.68(10) . 2_666 ? O11 Nd2 S4 116.89(11) . 2_666 ? O13 Nd2 S4 27.63(10) 2_666 2_666 ? O16 Nd2 S4 27.57(10) 2_666 2_666 ? O14 Nd2 S4 98.51(12) . 2_666 ? O15 Nd2 S4 146.48(13) . 2_666 ? O10 Nd2 S4 131.39(11) . 2_666 ? S2 Nd2 S4 103.60(4) . 2_666 ? O9 Nd2 S1 150.69(12) 1_455 . ? O11 Nd2 S1 89.81(10) 2_776 . ? O12 Nd2 S1 95.63(11) . . ? O11 Nd2 S1 27.99(10) . . ? O13 Nd2 S1 140.17(11) 2_666 . ? O16 Nd2 S1 85.53(10) 2_666 . ? O14 Nd2 S1 26.93(11) . . ? O15 Nd2 S1 86.2(2) . . ? O10 Nd2 S1 79.42(11) . . ? S2 Nd2 S1 86.82(4) . . ? S4 Nd2 S1 113.02(5) 2_666 . ? O17 S1 O9 111.9(3) . . ? O17 S1 O14 113.8(3) . . ? O9 S1 O14 111.2(3) . . ? O17 S1 O11 110.6(3) . . ? O9 S1 O11 106.6(3) . . ? O14 S1 O11 102.1(3) . . ? O17 S1 Nd2 117.9(2) . . ? O9 S1 Nd2 129.9(2) . . ? O14 S1 Nd2 51.8(2) . . ? O11 S1 Nd2 51.4(2) . . ? O6 S2 O10 113.2(3) . . ? O6 S2 O7 105.2(3) . . ? O10 S2 O7 112.0(3) . . ? O6 S2 O12 110.4(3) . . ? O10 S2 O12 106.0(3) . . ? O7 S2 O12 110.2(3) . . ? O6 S2 Nd2 129.0(2) . . ? O10 S2 Nd2 54.7(2) . . ? O7 S2 Nd2 125.6(2) . . ? O12 S2 Nd2 51.2(2) . . ? O6 S2 Nd1 52.7(2) . . ? O10 S2 Nd1 133.9(2) . . ? O7 S2 Nd1 52.8(2) . . ? O12 S2 Nd1 120.1(2) . . ? Nd2 S2 Nd1 171.17(6) . . ? O18 S3 O1 110.2(3) . . ? O18 S3 O5 111.5(3) . . ? O1 S3 O5 111.5(3) . . ? O18 S3 O2 110.9(3) . . ? O1 S3 O2 109.1(3) . . ? O5 S3 O2 103.4(3) . . ? O18 S3 Nd1 126.6(2) . . ? O1 S3 Nd1 123.2(2) . . ? O5 S3 Nd1 49.6(2) . . ? O2 S3 Nd1 53.9(2) . . ? O8 S4 O16 112.6(3) . . ? O8 S4 O3 106.3(3) . . ? O16 S4 O3 110.0(3) . . ? O8 S4 O13 114.2(3) . . ? O16 S4 O13 103.8(3) . . ? O3 S4 O13 109.8(3) . . ? O8 S4 Nd1 57.0(2) . . ? O16 S4 Nd1 131.2(2) . . ? O3 S4 Nd1 49.6(2) . . ? O13 S4 Nd1 124.3(2) . . ? O8 S4 Nd2 138.9(2) . 2_666 ? O16 S4 Nd2 52.7(2) . 2_666 ? O3 S4 Nd2 114.8(2) . 2_666 ? O13 S4 Nd2 52.2(2) . 2_666 ? Nd1 S4 Nd2 163.81(6) . 2_666 ? S3 O1 Nd1 143.6(3) . 1_655 ? S3 O2 Nd1 144.4(3) . 2_665 ? S3 O2 Nd1 98.5(2) . . ? Nd1 O2 Nd1 116.5(2) 2_665 . ? S4 O3 Nd1 103.0(2) . . ? S3 O5 Nd1 103.9(2) . . ? S2 O6 Nd1 100.0(2) . . ? S2 O7 Nd1 99.6(2) . . ? S4 O8 Nd1 95.4(2) . . ? S1 O9 Nd2 157.5(3) . 1_655 ? S2 O10 Nd2 97.3(2) . . ? S1 O11 Nd2 131.4(3) . 2_776 ? S1 O11 Nd2 100.7(2) . . ? Nd2 O11 Nd2 113.6(2) 2_776 . ? S2 O12 Nd2 100.7(2) . . ? S4 O13 Nd2 100.2(2) . 2_666 ? S1 O14 Nd2 101.2(2) . . ? S4 O16 Nd2 99.7(2) . 2_666 ? C2 N1 C1 112.8(6) . . ? C3 N2 C4 109.3(7) . . ? N1 C1 C2 109.6(6) . 2_655 ? N1 C2 C1 110.0(6) . 2_655 ? N2 C3 C4 109.1(7) . 2_766 ? C3 C4 N2 109.9(7) 2_766 . ? _refine_diff_density_max 1.012 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.187 #===END data_Phase_III _database_code_depnum_ccdc_archive 'CCDC 224286' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C H5 N Nd O8 S2' _chemical_formula_weight 367.42 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.48230(10) _cell_length_b 7.2328(3) _cell_length_c 9.7943(4) _cell_angle_alpha 87.165(2) _cell_angle_beta 83.125(2) _cell_angle_gamma 80.269(2) _cell_volume 379.86(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour 'light pink' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.212 _exptl_crystal_density_method ? _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 7.402 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.619251 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1568 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.18 _reflns_number_total 1059 _reflns_number_observed 970 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1059 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_obs 0.0290 _refine_ls_wR_factor_all 0.0765 _refine_ls_wR_factor_obs 0.0750 _refine_ls_goodness_of_fit_all 1.071 _refine_ls_goodness_of_fit_obs 1.103 _refine_ls_restrained_S_all 1.071 _refine_ls_restrained_S_obs 1.103 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd -0.20657(6) -0.22037(4) 0.04047(3) 0.0097(2) Uani 1 d . . S1 S -0.7041(3) -0.2873(2) -0.1625(2) 0.0090(4) Uani 1 d . . S2 S -0.7073(3) -0.1558(2) 0.2435(2) 0.0096(4) Uani 1 d . . O1 O -0.4662(9) -0.3396(6) -0.1014(5) 0.0165(11) Uani 1 d . . O2 O 0.1005(9) -0.2556(6) 0.2030(5) 0.0172(11) Uani 1 d . . O3 O -0.4727(8) -0.2910(6) 0.2547(5) 0.0158(10) Uani 1 d . . O4 O -0.6334(8) -0.0266(6) 0.1278(5) 0.0150(10) Uani 1 d . . O5 O 0.1270(8) -0.4245(6) -0.1108(5) 0.0144(10) Uani 1 d . . O6 O 0.1547(8) -0.1060(6) -0.1047(4) 0.0116(10) Uani 1 d . . O7 O -0.6665(10) -0.2747(7) -0.3107(5) 0.0211(12) Uani 1 d . . O8 O -0.7912(10) -0.0619(7) 0.3717(5) 0.0245(12) Uani 1 d . . N1 N -0.2250(12) -0.2684(8) 0.4973(6) 0.0212(14) Uani 1 d . . H1 H -0.3607(12) -0.2251(8) 0.5532(6) 0.032 Uiso 1 calc R . H2 H -0.2654(12) -0.2740(8) 0.4124(6) 0.032 Uiso 1 calc R . H3 H -0.1137(12) -0.1919(8) 0.4971(6) 0.032 Uiso 1 calc R . C1 C -0.1150(14) -0.4624(10) 0.5468(8) 0.024(2) Uani 1 d . . H4 H -0.0726(14) -0.4571(10) 0.6398(8) 0.029 Uiso 1 calc R . H5 H -0.2366(14) -0.5457(10) 0.5482(8) 0.029 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0074(3) 0.0074(3) 0.0142(3) -0.0012(2) -0.0006(2) -0.0011(2) S1 0.0071(8) 0.0071(8) 0.0127(9) -0.0012(6) -0.0007(6) -0.0015(6) S2 0.0080(9) 0.0080(8) 0.0129(9) -0.0012(7) -0.0013(6) -0.0015(7) O1 0.020(3) 0.006(2) 0.024(3) -0.003(2) -0.010(2) 0.000(2) O2 0.017(3) 0.013(2) 0.023(3) 0.004(2) -0.006(2) -0.005(2) O3 0.011(3) 0.018(2) 0.019(2) 0.001(2) 0.000(2) -0.004(2) O4 0.011(2) 0.015(2) 0.019(2) 0.009(2) -0.001(2) -0.002(2) O5 0.013(3) 0.006(2) 0.023(3) -0.002(2) 0.005(2) -0.004(2) O6 0.010(2) 0.004(2) 0.020(2) 0.000(2) -0.001(2) 0.001(2) O7 0.025(3) 0.022(3) 0.013(3) 0.001(2) 0.005(2) -0.003(2) O8 0.028(3) 0.021(3) 0.022(3) -0.008(2) 0.005(2) -0.001(2) N1 0.018(3) 0.018(3) 0.027(3) -0.005(3) 0.001(3) -0.005(3) C1 0.019(4) 0.021(4) 0.030(4) 0.010(3) 0.001(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.389(4) . ? Nd1 O2 2.427(5) . ? Nd1 O4 2.490(4) 2_455 ? Nd1 O3 2.491(4) . ? Nd1 O5 2.525(4) . ? Nd1 O6 2.528(4) . ? Nd1 O6 2.543(4) 2 ? Nd1 O4 2.589(5) . ? Nd1 O5 2.604(4) 2_545 ? Nd1 S2 3.172(2) . ? Nd1 S1 3.180(2) 1_655 ? S1 O7 1.442(5) . ? S1 O1 1.483(5) . ? S1 O5 1.499(5) 1_455 ? S1 O6 1.505(4) 1_455 ? S1 Nd1 3.179(2) 1_455 ? S2 O8 1.445(5) . ? S2 O2 1.475(5) 1_455 ? S2 O3 1.490(5) . ? S2 O4 1.496(5) . ? O2 S2 1.475(5) 1_655 ? O4 Nd1 2.490(4) 2_455 ? O5 S1 1.499(5) 1_655 ? O5 Nd1 2.604(4) 2_545 ? O6 S1 1.505(4) 1_655 ? O6 Nd1 2.543(4) 2 ? N1 C1 1.512(9) . ? C1 C1 1.51(2) 2_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Nd1 O2 153.2(2) . . ? O1 Nd1 O4 69.63(15) . 2_455 ? O2 Nd1 O4 136.01(15) . 2_455 ? O1 Nd1 O3 92.2(2) . . ? O2 Nd1 O3 80.4(2) . . ? O4 Nd1 O3 120.62(15) 2_455 . ? O1 Nd1 O5 81.1(2) . . ? O2 Nd1 O5 84.8(2) . . ? O4 Nd1 O5 101.43(15) 2_455 . ? O3 Nd1 O5 132.07(14) . . ? O1 Nd1 O6 110.6(2) . . ? O2 Nd1 O6 78.9(2) . . ? O4 Nd1 O6 70.29(14) 2_455 . ? O3 Nd1 O6 157.13(15) . . ? O5 Nd1 O6 55.13(13) . . ? O1 Nd1 O6 134.62(14) . 2 ? O2 Nd1 O6 72.11(14) . 2 ? O4 Nd1 O6 67.65(14) 2_455 2 ? O3 Nd1 O6 96.50(14) . 2 ? O5 Nd1 O6 121.66(14) . 2 ? O6 Nd1 O6 68.0(2) . 2 ? O1 Nd1 O4 80.2(2) . . ? O2 Nd1 O4 114.6(2) . . ? O4 Nd1 O4 66.5(2) 2_455 . ? O3 Nd1 O4 54.60(14) . . ? O5 Nd1 O4 160.5(2) . . ? O6 Nd1 O4 127.80(13) . . ? O6 Nd1 O4 69.45(14) 2 . ? O1 Nd1 O5 79.35(14) . 2_545 ? O2 Nd1 O5 73.96(15) . 2_545 ? O4 Nd1 O5 147.7(2) 2_455 2_545 ? O3 Nd1 O5 68.08(14) . 2_545 ? O5 Nd1 O5 64.0(2) . 2_545 ? O6 Nd1 O5 114.61(14) . 2_545 ? O6 Nd1 O5 144.64(14) 2 2_545 ? O4 Nd1 O5 117.59(14) . 2_545 ? O1 Nd1 S2 82.19(12) . . ? O2 Nd1 S2 100.75(12) . . ? O4 Nd1 S2 93.35(11) 2_455 . ? O3 Nd1 S2 27.27(11) . . ? O5 Nd1 S2 152.21(10) . . ? O6 Nd1 S2 152.58(10) . . ? O6 Nd1 S2 85.68(10) 2 . ? O4 Nd1 S2 27.81(10) . . ? O5 Nd1 S2 91.12(10) 2_545 . ? O1 Nd1 S1 97.77(12) . 1_655 ? O2 Nd1 S1 79.15(12) . 1_655 ? O4 Nd1 S1 86.91(11) 2_455 1_655 ? O3 Nd1 S1 152.47(11) . 1_655 ? O5 Nd1 S1 27.53(10) . 1_655 ? O6 Nd1 S1 27.69(10) . 1_655 ? O6 Nd1 S1 94.55(10) 2 1_655 ? O4 Nd1 S1 152.48(10) . 1_655 ? O5 Nd1 S1 88.59(10) 2_545 1_655 ? S2 Nd1 S1 179.70(4) . 1_655 ? O7 S1 O1 112.2(3) . . ? O7 S1 O5 112.3(3) . 1_455 ? O1 S1 O5 108.7(3) . 1_455 ? O7 S1 O6 110.8(3) . 1_455 ? O1 S1 O6 110.1(3) . 1_455 ? O5 S1 O6 102.2(3) 1_455 1_455 ? O7 S1 Nd1 129.8(2) . 1_455 ? O1 S1 Nd1 118.0(2) . 1_455 ? O5 S1 Nd1 51.1(2) 1_455 1_455 ? O6 S1 Nd1 51.3(2) 1_455 1_455 ? O8 S2 O2 111.0(3) . 1_455 ? O8 S2 O3 110.8(3) . . ? O2 S2 O3 109.5(3) 1_455 . ? O8 S2 O4 113.4(3) . . ? O2 S2 O4 109.1(3) 1_455 . ? O3 S2 O4 102.7(3) . . ? O8 S2 Nd1 136.0(2) . . ? O2 S2 Nd1 112.8(2) 1_455 . ? O3 S2 Nd1 50.0(2) . . ? O4 S2 Nd1 53.9(2) . . ? S1 O1 Nd1 141.7(3) . . ? S2 O2 Nd1 139.3(3) 1_655 . ? S2 O3 Nd1 102.7(2) . . ? S2 O4 Nd1 144.4(3) . 2_455 ? S2 O4 Nd1 98.3(2) . . ? Nd1 O4 Nd1 113.5(2) 2_455 . ? S1 O5 Nd1 101.3(2) 1_655 . ? S1 O5 Nd1 133.3(3) 1_655 2_545 ? Nd1 O5 Nd1 116.0(2) . 2_545 ? S1 O6 Nd1 101.0(2) 1_655 . ? S1 O6 Nd1 142.9(3) 1_655 2 ? Nd1 O6 Nd1 112.0(2) . 2 ? C1 C1 N1 110.1(7) 2_546 . ? _refine_diff_density_max 0.733 _refine_diff_density_min -1.333 _refine_diff_density_rms 0.207 #===END data_Phase_IV _database_code_depnum_ccdc_archive 'CCDC 224287' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C3 H12 La2 N2 O16 S4' _chemical_formula_weight 738.21 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1008(7) _cell_length_b 7.3085(5) _cell_length_c 20.1323(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.8290(10) _cell_angle_gamma 90.00 _cell_volume 1632.5(2) _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 cubic _exptl_crystal_colour transparent _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.004 _exptl_crystal_density_method ? _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 5.765 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.810963 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6480 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2345 _reflns_number_observed 1922 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0119(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2345 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_obs 0.0239 _refine_ls_wR_factor_all 0.0666 _refine_ls_wR_factor_obs 0.0643 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.167 _refine_ls_restrained_S_all 1.082 _refine_ls_restrained_S_obs 1.167 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group La1 La 0.65162(2) 0.17759(4) 0.517900(12) 0.01104(14) Uani 1 d . . La2 La 0.84961(2) 0.67489(4) 0.474497(12) 0.01090(14) Uani 1 d . . S1 S 0.88138(10) 0.17101(14) 0.42027(6) 0.0114(3) Uani 1 d . . S2 S 0.42958(10) 0.18183(15) 0.61613(6) 0.0117(3) Uani 1 d . . S3 S 0.62870(10) 0.67018(14) 0.57740(6) 0.0111(3) Uani 1 d . . S4 S 1.07734(10) 0.6677(2) 0.38094(6) 0.0126(3) Uani 1 d . . O1 O 0.5022(3) 0.6820(4) 0.5551(2) 0.0193(7) Uani 1 d . . O2 O 0.8234(3) 0.2042(4) 0.6015(2) 0.0208(8) Uani 1 d . . O3 O 0.4473(3) 0.0539(4) 0.55922(14) 0.0183(7) Uani 1 d . . O4 O 0.5450(3) 0.2844(4) 0.62008(14) 0.0176(7) Uani 1 d . . O5 O 0.8133(2) 0.0165(4) 0.44979(14) 0.0164(7) Uani 1 d . . O6 O 0.6878(3) 0.5184(4) 0.53979(14) 0.0155(7) Uani 1 d . . O7 O 0.6979(3) -0.1625(4) 0.55587(15) 0.0160(7) Uani 1 d . . O8 O 0.8128(3) 0.3360(4) 0.44235(14) 0.0153(7) Uani 1 d . . O9 O 0.6706(3) 0.6948(4) 0.3995(2) 0.0211(8) Uani 1 d . . O10 O 0.9955(3) 0.8293(4) 0.5506(2) 0.0178(7) Uani 1 d . . O11 O 0.9633(3) 0.7710(4) 0.37197(15) 0.0186(7) Uani 1 d . . O12 O 1.0556(3) 0.5442(4) 0.43900(14) 0.0179(7) Uani 1 d . . O13 O 0.8820(3) 0.1626(4) 0.3485(2) 0.0207(8) Uani 1 d . . O14 O 0.4112(3) 0.0849(5) 0.6767(2) 0.0281(8) Uani 1 d . . O15 O 0.6439(3) 0.6457(4) 0.64820(15) 0.0219(8) Uani 1 d . . O16 O 1.1042(3) 0.5634(5) 0.32221(15) 0.0235(8) Uani 1 d . . N1 N 0.6787(4) 0.3221(5) 0.7449(2) 0.0246(10) Uani 1 d . . H1 H 0.6535(4) 0.4154(5) 0.7693(2) 0.037 Uiso 1 calc R . H2 H 0.6414(4) 0.3249(5) 0.7051(2) 0.037 Uiso 1 calc R . H3 H 0.7579(4) 0.3308(5) 0.7401(2) 0.037 Uiso 1 calc R . N2 N 0.8714(4) -0.1522(6) 0.6874(2) 0.0402(12) Uani 1 d . . H4 H 0.9511(4) -0.1637(6) 0.6914(2) 0.060 Uiso 1 calc R . H5 H 0.8519(4) -0.0989(6) 0.6488(2) 0.060 Uiso 1 calc R . H6 H 0.8374(4) -0.2624(6) 0.6889(2) 0.060 Uiso 1 calc R . C1 C 0.6505(4) 0.1465(7) 0.7788(2) 0.0243(11) Uani 1 d . . H7 H 0.5642(4) 0.1376(7) 0.7845(2) 0.029 Uiso 1 calc R . H8 H 0.6901(4) 0.1440(7) 0.8224(2) 0.029 Uiso 1 calc R . C2 C 0.8276(4) -0.0384(7) 0.7427(2) 0.0279(12) Uani 1 d . . H9 H 0.8658(4) 0.0808(7) 0.7415(2) 0.033 Uiso 1 calc R . H10 H 0.8502(4) -0.0957(7) 0.7848(2) 0.033 Uiso 1 calc R . C3 C 0.6926(4) -0.0151(7) 0.7381(2) 0.0206(11) Uani 1 d . . H11 H 0.6545(4) -0.1257(7) 0.7538(2) 0.025 Uiso 1 calc R . H12 H 0.6675(4) 0.0026(7) 0.6920(2) 0.025 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0095(2) 0.0088(2) 0.0148(2) -0.00084(10) 0.00001(12) -0.00042(10) La2 0.0094(2) 0.0089(2) 0.0144(2) 0.00045(10) -0.00014(12) 0.00014(10) S1 0.0096(6) 0.0096(6) 0.0151(6) 0.0004(4) -0.0004(5) 0.0002(5) S2 0.0100(6) 0.0117(7) 0.0134(6) -0.0003(4) -0.0007(5) 0.0000(5) S3 0.0097(6) 0.0089(6) 0.0148(6) 0.0000(4) 0.0000(4) 0.0004(4) S4 0.0111(6) 0.0127(7) 0.0141(6) 0.0003(4) -0.0007(5) -0.0001(5) O1 0.014(2) 0.014(2) 0.030(2) 0.0026(13) -0.0025(14) 0.0016(14) O2 0.016(2) 0.019(2) 0.027(2) 0.0036(14) -0.0044(14) -0.0063(15) O3 0.016(2) 0.016(2) 0.022(2) -0.0056(13) -0.0002(13) -0.0011(14) O4 0.016(2) 0.019(2) 0.018(2) -0.0025(13) -0.0002(13) -0.0028(14) O5 0.014(2) 0.011(2) 0.024(2) -0.0008(13) 0.0038(13) 0.0005(14) O6 0.017(2) 0.012(2) 0.018(2) -0.0010(13) 0.0049(13) 0.0006(14) O7 0.017(2) 0.010(2) 0.021(2) -0.0003(13) 0.0009(13) -0.0019(14) O8 0.016(2) 0.010(2) 0.020(2) -0.0014(12) 0.0002(13) 0.0023(13) O9 0.016(2) 0.021(2) 0.026(2) -0.0050(14) -0.0024(14) 0.0040(15) O10 0.012(2) 0.016(2) 0.026(2) -0.0024(13) -0.0063(14) 0.0007(14) O11 0.015(2) 0.019(2) 0.022(2) 0.0023(13) -0.0004(13) 0.0029(14) O12 0.015(2) 0.017(2) 0.021(2) 0.0059(13) 0.0000(13) 0.0002(14) O13 0.022(2) 0.025(2) 0.015(2) 0.0000(13) 0.0016(14) 0.0030(15) O14 0.029(2) 0.031(2) 0.025(2) 0.0114(15) 0.0043(15) -0.002(2) O15 0.029(2) 0.022(2) 0.015(2) 0.0001(13) 0.0005(14) -0.003(2) O16 0.023(2) 0.025(2) 0.022(2) -0.0075(14) 0.0039(14) 0.0023(15) N1 0.027(2) 0.026(3) 0.021(2) -0.008(2) 0.000(2) 0.006(2) N2 0.030(3) 0.038(3) 0.053(3) -0.014(2) 0.004(2) 0.002(2) C1 0.018(3) 0.032(3) 0.023(3) -0.003(2) -0.002(2) 0.001(2) C2 0.029(3) 0.033(3) 0.022(3) -0.004(2) -0.006(2) 0.008(3) C3 0.020(3) 0.022(3) 0.020(2) 0.001(2) -0.002(2) -0.002(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 O1 2.443(3) 3_666 ? La1 O2 2.510(3) . ? La1 O3 2.524(3) 3_656 ? La1 O4 2.529(3) . ? La1 O6 2.559(3) . ? La1 O5 2.578(3) . ? La1 O3 2.603(3) . ? La1 O7 2.646(3) . ? La1 O8 2.651(3) . ? La1 S2 3.2091(11) . ? La1 S1 3.2697(11) . ? La2 O9 2.461(3) . ? La2 O10 2.467(3) . ? La2 O6 2.532(3) . ? La2 O11 2.552(3) . ? La2 O12 2.567(3) 3_766 ? La2 O5 2.575(3) 1_565 ? La2 O8 2.589(3) . ? La2 O12 2.599(3) . ? La2 O7 2.666(3) 1_565 ? La2 S4 3.2008(12) . ? La2 S3 3.2606(11) . ? S1 O13 1.446(3) . ? S1 O10 1.470(3) 3_766 ? S1 O5 1.493(3) . ? S1 O8 1.501(3) . ? S2 O14 1.431(3) . ? S2 O9 1.459(3) 3_666 ? S2 O4 1.485(3) . ? S2 O3 1.497(3) . ? S3 O15 1.441(3) . ? S3 O1 1.463(3) . ? S3 O6 1.506(3) . ? S3 O7 1.514(3) 1_565 ? S4 O16 1.446(3) . ? S4 O11 1.480(3) . ? S4 O2 1.481(3) 3_766 ? S4 O12 1.502(3) . ? O1 La1 2.443(3) 3_666 ? O2 S4 1.481(3) 3_766 ? O3 La1 2.523(3) 3_656 ? O5 La2 2.575(3) 1_545 ? O7 S3 1.514(3) 1_545 ? O7 La2 2.666(3) 1_545 ? O9 S2 1.459(3) 3_666 ? O10 S1 1.470(3) 3_766 ? O12 La2 2.567(3) 3_766 ? N1 C1 1.491(6) . ? N2 C2 1.484(6) . ? C1 C3 1.519(6) . ? C2 C3 1.509(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 150.71(10) 3_666 . ? O1 La1 O3 68.25(10) 3_666 3_656 ? O2 La1 O3 140.41(10) . 3_656 ? O1 La1 O4 91.36(10) 3_666 . ? O2 La1 O4 78.21(10) . . ? O3 La1 O4 120.12(10) 3_656 . ? O1 La1 O6 78.33(10) 3_666 . ? O2 La1 O6 72.38(10) . . ? O3 La1 O6 145.21(10) 3_656 . ? O4 La1 O6 68.55(9) . . ? O1 La1 O5 110.91(10) 3_666 . ? O2 La1 O5 82.25(10) . . ? O3 La1 O5 70.32(9) 3_656 . ? O4 La1 O5 157.72(10) . . ? O6 La1 O5 115.33(9) . . ? O1 La1 O3 74.86(10) 3_666 . ? O2 La1 O3 117.62(10) . . ? O3 La1 O3 66.26(10) 3_656 . ? O4 La1 O3 54.01(9) . . ? O6 La1 O3 114.63(9) . . ? O5 La1 O3 129.80(10) . . ? O1 La1 O7 133.94(10) 3_666 . ? O2 La1 O7 75.10(10) . . ? O3 La1 O7 67.95(9) 3_656 . ? O4 La1 O7 98.43(10) . . ? O6 La1 O7 146.79(9) . . ? O5 La1 O7 65.96(9) . . ? O3 La1 O7 75.19(9) . . ? O1 La1 O8 86.72(10) 3_666 . ? O2 La1 O8 80.72(10) . . ? O3 La1 O8 103.17(9) 3_656 . ? O4 La1 O8 132.35(9) . . ? O6 La1 O8 64.45(9) . . ? O5 La1 O8 53.14(9) . . ? O3 La1 O8 161.08(10) . . ? O7 La1 O8 116.59(8) . . ? O1 La1 S2 80.27(8) 3_666 . ? O2 La1 S2 99.67(8) . . ? O3 La1 S2 93.33(7) 3_656 . ? O4 La1 S2 26.79(7) . . ? O6 La1 S2 90.23(6) . . ? O5 La1 S2 153.35(7) . . ? O3 La1 S2 27.39(7) . . ? O7 La1 S2 88.67(7) . . ? O8 La1 S2 153.51(6) . . ? O1 La1 S1 100.84(8) 3_666 . ? O2 La1 S1 79.27(8) . . ? O3 La1 S1 87.28(7) 3_656 . ? O4 La1 S1 152.57(7) . . ? O6 La1 S1 89.80(6) . . ? O5 La1 S1 26.33(7) . . ? O3 La1 S1 153.06(7) . . ? O7 La1 S1 90.69(7) . . ? O8 La1 S1 26.85(6) . . ? S2 La1 S1 178.88(3) . . ? O9 La2 O10 148.79(10) . . ? O9 La2 O6 76.89(10) . . ? O10 La2 O6 110.29(10) . . ? O9 La2 O11 84.14(10) . . ? O10 La2 O11 92.55(10) . . ? O6 La2 O11 157.14(10) . . ? O9 La2 O12 139.34(10) . 3_766 ? O10 La2 O12 67.49(10) . 3_766 ? O6 La2 O12 69.40(10) . 3_766 ? O11 La2 O12 121.18(9) . 3_766 ? O9 La2 O5 72.91(10) . 1_565 ? O10 La2 O5 76.82(10) . 1_565 ? O6 La2 O5 115.42(9) . 1_565 ? O11 La2 O5 69.83(9) . 1_565 ? O12 La2 O5 142.58(10) 3_766 1_565 ? O9 La2 O8 77.59(10) . . ? O10 La2 O8 133.48(10) . . ? O6 La2 O8 65.71(9) . . ? O11 La2 O8 98.01(10) . . ? O12 La2 O8 68.33(9) 3_766 . ? O5 La2 O8 148.96(9) 1_565 . ? O9 La2 O12 123.56(10) . . ? O10 La2 O12 76.87(10) . . ? O6 La2 O12 128.42(10) . . ? O11 La2 O12 54.30(9) . . ? O12 La2 O12 67.17(10) 3_766 . ? O5 La2 O12 115.89(9) 1_565 . ? O8 La2 O12 73.33(9) . . ? O9 La2 O7 80.64(10) . 1_565 ? O10 La2 O7 80.20(10) . 1_565 ? O6 La2 O7 53.84(9) . 1_565 ? O11 La2 O7 135.46(9) . 1_565 ? O12 La2 O7 96.58(9) 3_766 1_565 ? O5 La2 O7 65.71(9) 1_565 1_565 ? O8 La2 O7 118.82(8) . 1_565 ? O12 La2 O7 155.68(9) . 1_565 ? O9 La2 S4 106.08(8) . . ? O10 La2 S4 81.82(8) . . ? O6 La2 S4 152.20(7) . . ? O11 La2 S4 26.91(7) . . ? O12 La2 S4 94.27(7) 3_766 . ? O5 La2 S4 91.37(6) 1_565 . ? O8 La2 S4 87.62(7) . . ? O12 La2 S4 27.61(7) . . ? O7 La2 S4 153.54(7) 1_565 . ? O9 La2 S3 77.40(8) . . ? O10 La2 S3 95.88(8) . . ? O6 La2 S3 26.51(7) . . ? O11 La2 S3 156.67(7) . . ? O12 La2 S3 82.11(7) 3_766 . ? O5 La2 S3 90.96(6) 1_565 . ? O8 La2 S3 91.88(7) . . ? O12 La2 S3 148.97(7) . . ? O7 La2 S3 27.33(6) 1_565 . ? S4 La2 S3 176.27(3) . . ? O13 S1 O10 111.4(2) . 3_766 ? O13 S1 O5 112.6(2) . . ? O10 S1 O5 108.4(2) 3_766 . ? O13 S1 O8 110.4(2) . . ? O10 S1 O8 110.9(2) 3_766 . ? O5 S1 O8 102.8(2) . . ? O13 S1 La1 129.03(14) . . ? O10 S1 La1 119.55(14) 3_766 . ? O5 S1 La1 50.01(11) . . ? O8 S1 La1 52.93(11) . . ? O14 S2 O9 111.2(2) . 3_666 ? O14 S2 O4 110.5(2) . . ? O9 S2 O4 110.5(2) 3_666 . ? O14 S2 O3 111.6(2) . . ? O9 S2 O3 109.8(2) 3_666 . ? O4 S2 O3 102.9(2) . . ? O14 S2 La1 130.82(15) . . ? O9 S2 La1 117.96(14) 3_666 . ? O4 S2 La1 50.16(12) . . ? O3 S2 La1 53.15(12) . . ? O15 S3 O1 113.0(2) . . ? O15 S3 O6 111.5(2) . . ? O1 S3 O6 108.6(2) . . ? O15 S3 O7 109.8(2) . 1_565 ? O1 S3 O7 110.8(2) . 1_565 ? O6 S3 O7 102.6(2) . 1_565 ? O15 S3 La2 124.28(14) . . ? O1 S3 La2 122.59(14) . . ? O6 S3 La2 48.66(11) . . ? O7 S3 La2 53.93(11) 1_565 . ? O16 S4 O11 111.5(2) . . ? O16 S4 O2 110.9(2) . 3_766 ? O11 S4 O2 109.5(2) . 3_766 ? O16 S4 O12 111.2(2) . . ? O11 S4 O12 104.1(2) . . ? O2 S4 O12 109.3(2) 3_766 . ? O16 S4 La2 132.62(14) . . ? O11 S4 La2 51.31(12) . . ? O2 S4 La2 116.42(14) 3_766 . ? O12 S4 La2 53.30(12) . . ? S3 O1 La1 148.7(2) . 3_666 ? S4 O2 La1 138.8(2) 3_766 . ? S2 O3 La1 145.6(2) . 3_656 ? S2 O3 La1 99.46(15) . . ? La1 O3 La1 113.74(10) 3_656 . ? S2 O4 La1 103.05(15) . . ? S1 O5 La2 137.1(2) . 1_545 ? S1 O5 La1 103.66(15) . . ? La2 O5 La1 116.57(10) 1_545 . ? S3 O6 La2 104.8(2) . . ? S3 O6 La1 137.3(2) . . ? La2 O6 La1 117.42(10) . . ? S3 O7 La1 138.2(2) 1_545 . ? S3 O7 La2 98.74(14) 1_545 1_545 ? La1 O7 La2 111.20(10) . 1_545 ? S1 O8 La2 139.9(2) . . ? S1 O8 La1 100.22(14) . . ? La2 O8 La1 112.23(10) . . ? S2 O9 La2 139.8(2) 3_666 . ? S1 O10 La2 146.2(2) 3_766 . ? S4 O11 La2 101.8(2) . . ? S4 O12 La2 146.1(2) . 3_766 ? S4 O12 La2 99.09(15) . . ? La2 O12 La2 112.83(10) 3_766 . ? N1 C1 C3 110.5(4) . . ? N2 C2 C3 111.5(4) . . ? C2 C3 C1 112.2(4) . . ? _refine_diff_density_max 0.918 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.234 #===END data_Phase_V _database_code_depnum_ccdc_archive 'CCDC 224288' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C7 H24 N3 Nd O13.50 S2.50' _chemical_formula_weight 590.68 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 25.506(5) _cell_length_b 10.102(2) _cell_length_c 13.415(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3456.5(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'faint pink' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_method ? _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 3.384 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.727286 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28171 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.02 _reflns_number_total 4128 _reflns_number_observed 3745 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+37.0884P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4128 _refine_ls_number_parameters 274 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_obs 0.0469 _refine_ls_wR_factor_all 0.0932 _refine_ls_wR_factor_obs 0.0913 _refine_ls_goodness_of_fit_all 1.287 _refine_ls_goodness_of_fit_obs 1.328 _refine_ls_restrained_S_all 1.288 _refine_ls_restrained_S_obs 1.329 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.176162(11) 0.01336(3) 0.21782(2) 0.01139(9) Uani 1 d . . S1 S 0.24700(6) 0.26740(13) 0.22765(10) 0.0124(3) Uani 1 d . . S2 S 0.15105(6) 0.03377(14) -0.01028(10) 0.0143(3) Uani 1 d . . S3 S 0.0000 0.4383(2) 0.2500 0.0274(5) Uani 1 d S . O1 O 0.0921(2) 0.1250(6) 0.2319(5) 0.0309(12) Uani 1 d . . O2 O 0.1142(2) -0.1619(5) 0.2574(4) 0.0260(11) Uani 1 d . . O3 O 0.1691(2) -0.0401(4) -0.0985(3) 0.0186(9) Uani 1 d . . O4 O 0.1894(2) 0.2583(4) 0.2394(3) 0.0167(9) Uani 1 d . . O5 O 0.1953(2) 0.0961(4) 0.0436(3) 0.0211(9) Uani 1 d . . O6 O 0.1272(2) -0.0579(4) 0.0629(3) 0.0183(9) Uani 1 d . . O7 O 0.2388(2) -0.1517(4) 0.1399(3) 0.0167(9) Uani 1 d . . O8 O 0.2650(2) 0.1280(4) 0.2161(3) 0.0168(8) Uani 1 d . . O9 O 0.2718(2) 0.3328(4) 0.3130(3) 0.0200(9) Uani 1 d . . O10 O 0.1131(2) 0.1358(5) -0.0411(4) 0.0269(11) Uani 1 d . . O11 O 0.0447(4) 0.3614(8) 0.2185(6) 0.086(3) Uani 1 d . . O12 O -0.0164(2) 0.5225(6) 0.1661(4) 0.0419(14) Uani 1 d . . N1 N -0.1866(2) 0.4713(6) -0.0324(4) 0.0228(12) Uani 1 d . . H10E H -0.2151(2) 0.4684(6) -0.0731(4) 0.027 Uiso 1 calc R . N2 N -0.1088(2) 0.4768(5) 0.0780(4) 0.0208(11) Uani 1 d . . H20D H -0.0803(2) 0.4791(5) 0.1189(4) 0.025 Uiso 1 calc R . N3 N -0.0137(5) 0.8164(13) -0.0480(9) 0.099(4) Uani 1 d D . H3B H -0.0051(5) 0.8232(13) -0.1098(9) 0.118 Uiso 1 calc R . H3C H -0.0247(5) 0.7420(13) -0.0249(9) 0.118 Uiso 1 calc R . C1 C -0.1398(3) 0.5147(8) -0.0909(5) 0.031(2) Uani 1 d . . H1A H -0.1481(3) 0.5933(8) -0.1293(5) 0.037 Uiso 1 calc R . H1B H -0.1291(3) 0.4454(8) -0.1367(5) 0.037 Uiso 1 calc R . C2 C -0.1967(3) 0.5656(7) 0.0506(5) 0.0247(14) Uani 1 d . . H2A H -0.2307(3) 0.5481(7) 0.0803(5) 0.030 Uiso 1 calc R . H2B H -0.1965(3) 0.6559(7) 0.0259(5) 0.030 Uiso 1 calc R . C3 C -0.1762(3) 0.3351(7) 0.0091(5) 0.0267(14) Uani 1 d . . H3D H -0.2032(3) 0.3117(7) 0.0569(5) 0.032 Uiso 1 calc R . H3E H -0.1766(3) 0.2703(7) -0.0443(5) 0.032 Uiso 1 calc R . C4 C -0.1237(3) 0.3363(6) 0.0587(5) 0.0219(13) Uani 1 d . . H4A H -0.1252(3) 0.2877(6) 0.1210(5) 0.026 Uiso 1 calc R . H4B H -0.0978(3) 0.2946(6) 0.0161(5) 0.026 Uiso 1 calc R . C5 C -0.0959(3) 0.5440(7) -0.0177(5) 0.0268(15) Uani 1 d . . H5D H -0.0628(3) 0.5114(7) -0.0435(5) 0.032 Uiso 1 calc R . H5E H -0.0929(3) 0.6387(7) -0.0073(5) 0.032 Uiso 1 calc R . C6 C -0.1536(3) 0.5465(7) 0.1271(5) 0.0233(14) Uani 1 d . . H6A H -0.1422(3) 0.6317(7) 0.1525(5) 0.028 Uiso 1 calc R . H6B H -0.1666(3) 0.4943(7) 0.1826(5) 0.028 Uiso 1 calc R . C7 C -0.0098(5) 0.9276(12) 0.0155(12) 0.095(5) Uani 1 d D . H7A H 0.0127(5) 0.9003(12) 0.0701(12) 0.114 Uiso 1 calc R . H7B H -0.0445(5) 0.9396(12) 0.0438(12) 0.114 Uiso 1 calc R . O100 O 0.0352(3) 0.7548(7) 0.1403(5) 0.059(2) Uani 1 d D . O200 O -0.0042(4) 0.0113(11) 0.1918(9) 0.041(3) Uani 0.50 d P . H20 H 0.0895(35) -0.1655(84) 0.2259(67) 0.032(25) Uiso 1 d . . H12 H 0.0838(33) 0.1894(87) 0.2325(65) 0.027(25) Uiso 1 d . . H11 H 0.1088(33) -0.1653(83) 0.3095(66) 0.028(25) Uiso 1 d . . H9 H 0.0165(37) 0.8087(87) 0.1916(58) 0.068(36) Uiso 1 d D . H5 H 0.0647(42) 0.0826(105) 0.2234(79) 0.063(34) Uiso 1 d . . H1 H 0.0117(28) 0.6816(61) 0.1630(66) 0.050(27) Uiso 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 Nd1 0.01261(14) 0.01094(14) 0.01061(14) -0.00036(11) 0.00025(12) -0.00022(11) S1 0.0145(6) 0.0122(6) 0.0106(6) -0.0014(5) -0.0004(6) -0.0013(5) S2 0.0185(7) 0.0153(6) 0.0090(6) 0.0010(5) -0.0010(5) 0.0003(5) S3 0.0298(13) 0.0180(10) 0.0344(13) 0.000 0.0030(10) 0.000 O1 0.017(3) 0.026(3) 0.050(4) -0.008(3) -0.003(2) 0.005(2) O2 0.029(3) 0.032(3) 0.017(3) 0.004(2) 0.000(2) -0.010(2) O3 0.029(2) 0.019(2) 0.008(2) 0.000(2) 0.004(2) 0.000(2) O4 0.014(2) 0.015(2) 0.020(2) -0.002(2) 0.002(2) -0.001(2) O5 0.027(2) 0.025(2) 0.012(2) 0.001(2) -0.002(2) -0.008(2) O6 0.019(2) 0.025(2) 0.012(2) 0.002(2) 0.003(2) -0.008(2) O7 0.019(2) 0.015(2) 0.015(2) 0.002(2) 0.001(2) 0.004(2) O8 0.017(2) 0.012(2) 0.022(2) 0.000(2) -0.002(2) 0.002(2) O9 0.025(2) 0.024(2) 0.011(2) -0.003(2) -0.003(2) -0.009(2) O10 0.031(3) 0.028(2) 0.022(2) 0.002(2) -0.001(2) 0.013(2) O11 0.107(7) 0.077(5) 0.074(5) 0.023(4) 0.034(5) 0.068(5) O12 0.038(3) 0.050(3) 0.038(3) 0.006(3) -0.018(3) -0.007(3) N1 0.019(3) 0.032(3) 0.017(3) -0.002(2) -0.005(2) 0.003(2) N2 0.014(2) 0.025(3) 0.024(3) -0.005(2) -0.007(2) -0.002(2) N3 0.106(10) 0.115(10) 0.075(8) 0.021(8) -0.004(7) 0.002(8) C1 0.031(4) 0.046(4) 0.016(3) 0.009(3) 0.001(3) 0.005(3) C2 0.022(3) 0.025(3) 0.028(4) -0.004(3) 0.000(3) 0.005(3) C3 0.030(4) 0.024(3) 0.027(4) -0.004(3) -0.005(3) -0.006(3) C4 0.022(3) 0.016(3) 0.028(4) 0.003(2) -0.001(3) 0.001(2) C5 0.021(3) 0.031(4) 0.029(4) 0.009(3) 0.005(3) -0.005(3) C6 0.027(3) 0.027(3) 0.016(3) -0.009(3) -0.001(3) -0.004(3) C7 0.066(9) 0.086(10) 0.132(14) 0.026(10) 0.000(9) 0.002(8) O100 0.071(5) 0.055(4) 0.051(4) 0.014(3) -0.015(4) -0.028(4) O200 0.028(5) 0.038(6) 0.057(7) -0.007(5) 0.002(5) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1 2.429(5) . ? Nd1 O2 2.432(5) . ? Nd1 O3 2.485(4) 8_556 ? Nd1 O4 2.514(4) . ? Nd1 O6 2.529(4) . ? Nd1 O5 2.530(4) . ? Nd1 O7 2.535(4) . ? Nd1 O8 2.545(4) . ? Nd1 O9 2.593(4) 7_655 ? Nd1 S2 3.1330(15) . ? Nd1 S1 3.1412(15) . ? Nd1 S1 3.1674(15) 7_655 ? S1 O9 1.465(4) . ? S1 O7 1.478(4) 7_665 ? S1 O4 1.480(4) . ? S1 O8 1.489(4) . ? S1 Nd1 3.1672(15) 7_665 ? S2 O10 1.473(5) . ? S2 O3 1.473(4) . ? S2 O6 1.480(4) . ? S2 O5 1.480(5) . ? S3 O11 1.443(7) . ? S3 O11 1.444(7) 4 ? S3 O12 1.471(6) 4 ? S3 O12 1.471(6) . ? O3 Nd1 2.485(4) 8 ? O7 S1 1.478(4) 7_655 ? O9 Nd1 2.593(4) 7_665 ? N1 C2 1.488(8) . ? N1 C1 1.495(8) . ? N1 C3 1.507(8) . ? N2 C5 1.489(8) . ? N2 C4 1.491(8) . ? N2 C6 1.496(8) . ? N3 C7 1.413(9) . ? C1 C5 1.518(10) . ? C2 C6 1.516(9) . ? C3 C4 1.498(9) . ? C7 C7 1.60(2) 5_575 ? O200 O200 1.58(2) 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 O1 Nd1 O2 75.4(2) . . ? O1 Nd1 O3 79.0(2) . 8_556 ? O2 Nd1 O3 79.4(2) . 8_556 ? O1 Nd1 O4 69.7(2) . . ? O2 Nd1 O4 141.1(2) . . ? O3 Nd1 O4 77.79(13) 8_556 . ? O1 Nd1 O6 76.1(2) . . ? O2 Nd1 O6 69.6(2) . . ? O3 Nd1 O6 144.08(14) 8_556 . ? O4 Nd1 O6 116.18(14) . . ? O1 Nd1 O5 95.1(2) . . ? O2 Nd1 O5 124.6(2) . . ? O3 Nd1 O5 153.39(14) 8_556 . ? O4 Nd1 O5 75.84(14) . . ? O6 Nd1 O5 55.23(13) . . ? O1 Nd1 O7 153.3(2) . . ? O2 Nd1 O7 91.2(2) . . ? O3 Nd1 O7 121.74(14) 8_556 . ? O4 Nd1 O7 127.57(13) . . ? O6 Nd1 O7 77.61(14) . . ? O5 Nd1 O7 73.43(14) . . ? O1 Nd1 O8 125.1(2) . . ? O2 Nd1 O8 155.8(2) . . ? O3 Nd1 O8 91.39(14) 8_556 . ? O4 Nd1 O8 55.48(13) . . ? O6 Nd1 O8 124.16(13) . . ? O5 Nd1 O8 70.71(14) . . ? O7 Nd1 O8 74.57(13) . . ? O1 Nd1 O9 137.8(2) . 7_655 ? O2 Nd1 O9 73.3(2) . 7_655 ? O3 Nd1 O9 68.00(13) 8_556 7_655 ? O4 Nd1 O9 124.52(14) . 7_655 ? O6 Nd1 O9 117.23(14) . 7_655 ? O5 Nd1 O9 126.08(14) . 7_655 ? O7 Nd1 O9 54.37(13) . 7_655 ? O8 Nd1 O9 82.46(14) . 7_655 ? O1 Nd1 S2 82.24(15) . . ? O2 Nd1 S2 97.38(14) . . ? O3 Nd1 S2 161.14(10) 8_556 . ? O4 Nd1 S2 94.32(10) . . ? O6 Nd1 S2 27.77(9) . . ? O5 Nd1 S2 27.77(10) . . ? O7 Nd1 S2 76.67(10) . . ? O8 Nd1 S2 98.22(10) . . ? O9 Nd1 S2 129.20(9) 7_655 . ? O1 Nd1 S1 97.18(15) . . ? O2 Nd1 S1 163.59(14) . . ? O3 Nd1 S1 84.91(10) 8_556 . ? O4 Nd1 S1 27.59(10) . . ? O6 Nd1 S1 123.43(10) . . ? O5 Nd1 S1 70.01(10) . . ? O7 Nd1 S1 101.05(10) . . ? O8 Nd1 S1 27.92(9) . . ? O9 Nd1 S1 105.04(11) 7_655 . ? S2 Nd1 S1 96.02(4) . . ? O1 Nd1 S1 155.1(2) . 7_655 ? O2 Nd1 S1 79.76(14) . 7_655 ? O3 Nd1 S1 95.10(10) 8_556 7_655 ? O4 Nd1 S1 133.16(10) . 7_655 ? O6 Nd1 S1 96.69(10) . 7_655 ? O5 Nd1 S1 100.29(11) . 7_655 ? O7 Nd1 S1 27.28(9) . 7_655 ? O8 Nd1 S1 78.85(9) . 7_655 ? O9 Nd1 S1 27.20(9) 7_655 7_655 ? S2 Nd1 S1 102.64(4) . 7_655 ? S1 Nd1 S1 106.45(2) . 7_655 ? O9 S1 O7 105.5(2) . 7_665 ? O9 S1 O4 111.9(3) . . ? O7 S1 O4 111.2(2) 7_665 . ? O9 S1 O8 112.0(3) . . ? O7 S1 O8 111.4(3) 7_665 . ? O4 S1 O8 105.0(2) . . ? O9 S1 Nd1 130.5(2) . . ? O7 S1 Nd1 124.0(2) 7_665 . ? O4 S1 Nd1 51.9(2) . . ? O8 S1 Nd1 53.2(2) . . ? O9 S1 Nd1 54.0(2) . 7_665 ? O7 S1 Nd1 51.8(2) 7_665 7_665 ? O4 S1 Nd1 131.8(2) . 7_665 ? O8 S1 Nd1 123.1(2) . 7_665 ? Nd1 S1 Nd1 174.28(5) . 7_665 ? O10 S2 O3 109.5(3) . . ? O10 S2 O6 110.8(3) . . ? O3 S2 O6 110.1(2) . . ? O10 S2 O5 109.9(3) . . ? O3 S2 O5 111.7(3) . . ? O6 S2 O5 104.8(2) . . ? O10 S2 Nd1 117.1(2) . . ? O3 S2 Nd1 133.4(2) . . ? O6 S2 Nd1 52.8(2) . . ? O5 S2 Nd1 52.8(2) . . ? O11 S3 O11 114.9(8) . 4 ? O11 S3 O12 108.1(5) . 4 ? O11 S3 O12 108.1(4) 4 4 ? O11 S3 O12 108.1(4) . . ? O11 S3 O12 108.1(5) 4 . ? O12 S3 O12 109.3(5) 4 . ? S2 O3 Nd1 139.8(2) . 8 ? S1 O4 Nd1 100.5(2) . . ? S2 O5 Nd1 99.4(2) . . ? S2 O6 Nd1 99.4(2) . . ? S1 O7 Nd1 100.9(2) 7_655 . ? S1 O8 Nd1 98.9(2) . . ? S1 O9 Nd1 98.8(2) . 7_665 ? C2 N1 C1 110.1(5) . . ? C2 N1 C3 109.8(5) . . ? C1 N1 C3 108.8(5) . . ? C5 N2 C4 109.9(5) . . ? C5 N2 C6 109.5(5) . . ? C4 N2 C6 109.3(5) . . ? N1 C1 C5 107.8(5) . . ? N1 C2 C6 107.4(5) . . ? C4 C3 N1 108.3(5) . . ? N2 C4 C3 108.2(5) . . ? N2 C5 C1 107.8(5) . . ? N2 C6 C2 108.4(5) . . ? N3 C7 C7 126.3(17) . 5_575 ? _refine_diff_density_max 0.859 _refine_diff_density_min -1.348 _refine_diff_density_rms 0.163