Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global # 1. SUBMISSION DETAILS _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Monge, M. Angeles' 'Cascales, Concepcion' 'Gomez-Lor, Berta' 'Gutierrez-Puebla, Enrique' 'Iglesias, Marta' 'Ruiz-Valero, Caridad' 'Snejko, Natalia' _publ_contact_author_name 'Dr M. Angeles Monge' _publ_contact_author_address ; Instituto de Ciencia de Materiales de Madrid ICMM Consejo Superior de Investigaciones Cientificas CSIC Cantoblanco Madrid 28049 SPAIN ; _publ_contact_author_phone '34 1 334-9025' _publ_contact_author_fax '34 1 372-0623' _publ_contact_author_email amonge@icmm.csic.es _publ_requested_journal 'Chemical Communication.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; From Rational Octahedral SBU Design to Reticulation Serendipity. A Thermally Stable Rare Earth Polymeric Disulfonate Family with CdI2 - like structure, Bifunctional Catalysis and Optical Properties. ; #============================================================================== # 4. TEXT _publ_section_abstract ; A new family of lanthanide disulfonates Ln(OH)(NDS)H2O, (Ln= Ln, Pr and Nd and NDS=1.5-naphthalenedisulfonate) was designed and hydrothermaly synthesized. This is the first example of a disulfonate ligand coordinated to six different Ln atoms. These materials, with high thermal stability, act as active and selective bifunctional catalysts in oxidation and epoxide ring opening. Strong luminescence from the optically active Nd center was observed. ; ======================================================================== data_NdPF-1 _database_code_CSD 182916 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H9 Nd O8 S2' _chemical_formula_weight 465.53 _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' '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 5.6745(8) _cell_length_b 10.5508(15) _cell_length_c 11.450(2) _cell_angle_alpha 76.456(2) _cell_angle_beta 77.484(2) _cell_angle_gamma 88.034(2) _cell_volume 650.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colorlees _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.377 _exptl_crystal_density_method ? _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 4.349 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.587 _exptl_absorpt_correction_T_max 1.00 _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 ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 4574 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.1842 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 30.98 _reflns_number_total 3420 _reflns_number_observed 2125 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens fourier _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3420 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_obs 0.0540 _refine_ls_wR_factor_all 0.1340 _refine_ls_wR_factor_obs 0.1180 _refine_ls_goodness_of_fit_all 0.639 _refine_ls_goodness_of_fit_obs 0.721 _refine_ls_restrained_S_all 0.639 _refine_ls_restrained_S_obs 0.721 _refine_ls_shift/esd_max -0.621 _refine_ls_shift/esd_mean 0.018 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 0.14134(9) 0.16797(5) 0.47289(5) 0.01747(15) Uani 1 d . . S2 S -0.2998(4) 0.3839(2) 0.2984(2) 0.0218(5) Uani 1 d . . S3 S 0.4271(4) -0.0917(2) 0.3132(2) 0.0184(4) Uani 1 d . . O1 O 0.1404(15) 0.3882(8) 0.5289(8) 0.048(2) Uani 1 d . . O2 O 0.1318(12) -0.0488(6) 0.5798(7) 0.0234(15) Uani 1 d . . O3 O -0.3673(13) 0.5089(7) 0.3243(6) 0.033(2) Uani 1 d . . O4 O -0.0867(12) 0.3325(6) 0.3438(6) 0.030(2) Uani 1 d . . O5 O 0.5022(12) 0.2897(6) 0.3383(6) 0.029(2) Uani 1 d . . O6 O -0.1931(11) 0.1580(6) 0.6572(6) 0.0218(13) Uani 1 d . . O7 O 0.4119(11) 0.0434(6) 0.3257(6) 0.0212(13) Uani 1 d . . O8 O 0.4043(11) 0.1657(6) 0.6182(6) 0.0228(13) Uani 1 d . . C1 C 0.5521(15) -0.0840(8) 0.1552(8) 0.017(2) Uani 1 d . . C2 C 0.7582(17) -0.1521(10) 0.1264(8) 0.025(2) Uani 1 d . . C3 C 0.1332(17) 0.1430(10) -0.0028(8) 0.024(2) Uani 1 d . . C4 C 0.2297(17) 0.0688(10) 0.0887(8) 0.026(2) Uani 1 d . . C5 C 0.4463(15) -0.0030(8) 0.0617(7) 0.017(2) Uani 1 d . . C6 C -0.2226(16) 0.4077(8) 0.1348(8) 0.021(2) Uani 1 d . . C7 C -0.3653(17) 0.3487(9) 0.0813(9) 0.024(2) Uani 1 d . . C8 C -0.3195(17) 0.3725(9) -0.0488(9) 0.025(2) Uani 1 d . . C9 C 0.1349(16) 0.5511(8) 0.1186(8) 0.019(2) Uani 1 d . . C10 C -0.0227(15) 0.4892(8) 0.0659(8) 0.019(2) Uani 1 d . . H2 H 0.8424(191) -0.1985(100) 0.1781(94) 0.030(28) Uiso 1 d . . H3 H 0.0309(195) 0.1934(101) 0.0263(94) 0.031(29) Uiso 1 d . . H4 H 0.1185(160) 0.0423(85) 0.2070(80) 0.017(23) Uiso 1 d . . H7 H -0.5256(135) 0.2902(72) 0.1272(68) 0.000(18) Uiso 1 d . . H8 H -0.4206(159) 0.3187(87) -0.0840(80) 0.015(22) Uiso 1 d . . H9 H 0.1162(148) 0.5498(79) 0.1979(77) 0.005(20) Uiso 1 d . . H2' H 0.1970(160) -0.0685(86) 0.6169(80) 0.000(25) Uiso 1 d . . H11 H 0.2256 0.4071 0.5857 0.050 Uiso 1 d . . H12 H 0.3011 0.3841 0.4454 0.050 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 0.0169(2) 0.0176(2) 0.0187(2) -0.0035(2) -0.0061(2) 0.0003(2) S2 0.0208(11) 0.0217(11) 0.0218(11) -0.0012(9) -0.0065(9) -0.0021(9) S3 0.0184(11) 0.0210(10) 0.0172(10) -0.0060(8) -0.0054(8) 0.0009(8) O1 0.059(5) 0.040(4) 0.073(6) -0.038(4) -0.046(5) 0.018(4) O2 0.018(4) 0.022(3) 0.034(4) -0.007(3) -0.012(3) 0.004(3) O3 0.042(4) 0.031(4) 0.033(4) -0.014(3) -0.014(3) 0.007(3) O4 0.029(4) 0.025(3) 0.034(4) 0.002(3) -0.012(3) -0.004(3) O5 0.030(4) 0.032(4) 0.024(3) -0.005(3) -0.003(3) -0.006(3) O6 0.017(3) 0.025(3) 0.025(3) -0.007(3) -0.006(3) -0.005(2) O7 0.024(3) 0.018(3) 0.023(3) -0.008(3) -0.003(3) 0.000(2) O8 0.027(4) 0.021(3) 0.022(3) -0.003(3) -0.012(3) 0.002(3) C1 0.015(4) 0.021(4) 0.017(4) -0.009(3) -0.001(3) -0.001(3) C2 0.025(5) 0.033(5) 0.017(4) -0.004(4) -0.006(4) 0.011(4) C3 0.020(5) 0.036(6) 0.015(5) -0.009(4) -0.004(4) 0.017(4) C4 0.025(5) 0.037(5) 0.016(4) -0.013(4) 0.001(4) 0.004(4) C5 0.016(4) 0.017(4) 0.018(4) -0.002(3) -0.003(3) 0.001(3) C6 0.024(5) 0.017(4) 0.022(5) -0.002(3) -0.008(4) 0.001(3) C7 0.022(5) 0.018(4) 0.032(5) -0.006(4) -0.003(4) -0.006(4) C8 0.020(5) 0.020(4) 0.035(5) -0.005(4) -0.011(4) 0.002(4) C9 0.021(4) 0.022(4) 0.020(5) -0.010(4) -0.010(4) 0.000(3) C10 0.020(4) 0.022(4) 0.020(4) -0.009(4) -0.011(4) 0.003(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 O2 2.290(7) 2_556 ? Nd1 O2 2.324(7) . ? Nd1 O5 2.471(7) . ? Nd1 O8 2.460(6) . ? Nd1 O6 2.498(6) . ? Nd1 O4 2.519(6) . ? Nd1 O1 2.551(7) . ? Nd1 O7 2.589(6) . ? Nd1 Nd1 3.8013(11) 2_556 ? Nd1 H12 2.4089(6) . ? S2 O5 1.449(7) 1_455 ? S2 O3 1.441(7) . ? S2 O4 1.456(7) . ? S2 C6 1.788(9) . ? S3 O8 1.459(6) 2_656 ? S3 O6 1.458(6) 2_556 ? S3 O7 1.463(6) . ? S3 C1 1.778(8) . ? O1 H11 0.948(7) . ? O1 H12 1.178(9) . ? O2 Nd1 2.290(7) 2_556 ? O2 H2' 0.62(8) . ? O5 S2 1.449(7) 1_655 ? O6 S3 1.458(6) 2_556 ? O8 S3 1.459(6) 2_656 ? C1 C2 1.371(12) . ? C1 C5 1.432(11) . ? C2 C3 1.398(12) 2_655 ? C2 H2 0.89(11) . ? C3 C4 1.359(12) . ? C3 C2 1.398(12) 2_655 ? C3 H3 0.84(11) . ? C4 C5 1.436(12) . ? C4 H4 1.33(9) . ? C5 C5 1.40(2) 2_655 ? C6 C7 1.359(13) . ? C6 C10 1.418(12) . ? C7 C8 1.418(14) . ? C7 H7 1.08(8) . ? C8 C9 1.334(13) 2_565 ? C8 H8 1.02(9) . ? C9 C8 1.334(13) 2_565 ? C9 C10 1.432(11) . ? C9 H9 0.89(8) . ? C10 C10 1.44(2) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd1 O2 69.0(3) 2_556 . ? O2 Nd1 O5 128.1(2) 2_556 . ? O2 Nd1 O5 125.6(2) . . ? O2 Nd1 O8 144.6(2) 2_556 . ? O2 Nd1 O8 76.1(2) . . ? O5 Nd1 O8 77.9(2) . . ? O2 Nd1 O6 81.7(2) 2_556 . ? O2 Nd1 O6 76.2(2) . . ? O5 Nd1 O6 146.1(2) . . ? O8 Nd1 O6 84.2(2) . . ? O2 Nd1 O4 74.6(2) 2_556 . ? O2 Nd1 O4 142.6(2) . . ? O5 Nd1 O4 84.2(2) . . ? O8 Nd1 O4 138.0(2) . . ? O6 Nd1 O4 90.4(2) . . ? O2 Nd1 O1 135.4(2) 2_556 . ? O2 Nd1 O1 135.4(3) . . ? O5 Nd1 O1 73.5(3) . . ? O8 Nd1 O1 69.2(2) . . ? O6 Nd1 O1 73.3(3) . . ? O4 Nd1 O1 69.3(2) . . ? O2 Nd1 O7 76.9(2) 2_556 . ? O2 Nd1 O7 73.6(2) . . ? O5 Nd1 O7 64.7(2) . . ? O8 Nd1 O7 99.5(2) . . ? O6 Nd1 O7 147.7(2) . . ? O4 Nd1 O7 106.7(2) . . ? O1 Nd1 O7 138.2(3) . . ? O2 Nd1 Nd1 34.8(2) 2_556 2_556 ? O2 Nd1 Nd1 34.2(2) . 2_556 ? O5 Nd1 Nd1 136.7(2) . 2_556 ? O8 Nd1 Nd1 110.13(14) . 2_556 ? O6 Nd1 Nd1 76.55(14) . 2_556 ? O4 Nd1 Nd1 109.0(2) . 2_556 ? O1 Nd1 Nd1 149.7(2) . 2_556 ? O7 Nd1 Nd1 72.03(14) . 2_556 ? O2 Nd1 H12 144.4(2) 2_556 . ? O2 Nd1 H12 146.3(2) . . ? O5 Nd1 H12 46.3(2) . . ? O8 Nd1 H12 70.21(14) . . ? O6 Nd1 H12 100.51(14) . . ? O4 Nd1 H12 69.9(2) . . ? O1 Nd1 H12 27.3(2) . . ? O7 Nd1 H12 111.00(14) . . ? Nd1 Nd1 H12 176.92(3) 2_556 . ? O5 S2 O3 113.2(4) 1_455 . ? O5 S2 O4 112.0(4) 1_455 . ? O3 S2 O4 112.6(4) . . ? O5 S2 C6 104.7(4) 1_455 . ? O3 S2 C6 107.0(4) . . ? O4 S2 C6 106.8(4) . . ? O8 S3 O6 111.9(4) 2_656 2_556 ? O8 S3 O7 111.5(4) 2_656 . ? O6 S3 O7 113.6(4) 2_556 . ? O8 S3 C1 106.4(4) 2_656 . ? O6 S3 C1 107.0(4) 2_556 . ? O7 S3 C1 106.0(4) . . ? Nd1 O1 H11 124.4(6) . . ? Nd1 O1 H12 69.6(3) . . ? H11 O1 H12 100.7(7) . . ? Nd1 O2 Nd1 111.0(3) 2_556 . ? Nd1 O2 H2' 127.4(87) 2_556 . ? Nd1 O2 H2' 121.6(87) . . ? S2 O4 Nd1 154.5(4) . . ? S2 O5 Nd1 158.3(4) 1_655 . ? S3 O6 Nd1 128.3(4) 2_556 . ? S3 O7 Nd1 135.4(4) . . ? S3 O8 Nd1 146.8(4) 2_656 . ? C2 C1 C5 121.6(8) . . ? C2 C1 S3 117.9(7) . . ? C5 C1 S3 120.4(6) . . ? C1 C2 C3 119.2(8) . 2_655 ? C1 C2 H2 127.3(67) . . ? C3 C2 H2 113.3(66) 2_655 . ? C4 C3 C2 121.1(8) . 2_655 ? C4 C3 H3 109.6(70) . . ? C2 C3 H3 127.4(70) 2_655 . ? C3 C4 C5 121.2(8) . . ? C3 C4 H4 123.7(38) . . ? C5 C4 H4 114.5(38) . . ? C4 C5 C1 123.0(8) . . ? C4 C5 C5 118.3(9) . 2_655 ? C1 C5 C5 118.6(9) . 2_655 ? C7 C6 C10 122.7(8) . . ? C7 C6 S2 117.6(7) . . ? C10 C6 S2 119.7(7) . . ? C6 C7 C8 119.2(8) . . ? C6 C7 H7 126.7(41) . . ? C8 C7 H7 113.8(41) . . ? C9 C8 C7 120.8(9) 2_565 . ? C9 C8 H8 122.6(51) 2_565 . ? C7 C8 H8 116.1(50) . . ? C8 C9 C10 121.7(9) 2_565 . ? C8 C9 H9 112.5(55) 2_565 . ? C10 C9 H9 125.6(56) . . ? C6 C10 C9 124.5(8) . . ? C6 C10 C10 117.2(9) . 2_565 ? C9 C10 C10 118.3(10) . 2_565 ? _refine_diff_density_max 2.335 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.261 #======================================================================== data_Lapf-1 _database_code_CSD 182917 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H9 La O8 S2' _chemical_formula_weight 460.20 _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' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7263(2) _cell_length_b 10.6104(4) _cell_length_c 11.5533(5) _cell_angle_alpha 76.6150(10) _cell_angle_beta 77.6190(10) _cell_angle_gamma 87.9370(10) _cell_volume 666.94(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.292 _exptl_crystal_density_method ? _exptl_crystal_F_000 444 _exptl_absorpt_coefficient_mu 3.552 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.517 _exptl_absorpt_correction_T_max 1.000 _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 ? _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 7378 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 29.51 _reflns_number_total 3365 _reflns_number_observed 2879 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART CCD' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0373P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens fourier _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3365 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_obs 0.0339 _refine_ls_wR_factor_all 0.0753 _refine_ls_wR_factor_obs 0.0711 _refine_ls_goodness_of_fit_all 0.792 _refine_ls_goodness_of_fit_obs 0.813 _refine_ls_restrained_S_all 0.792 _refine_ls_restrained_S_obs 0.813 _refine_ls_shift/esd_max -0.461 _refine_ls_shift/esd_mean 0.017 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 0.35514(4) 0.83006(2) 0.52767(2) 0.01502(8) Uani 1 d . . S2 S 0.7958(2) 0.61403(11) 0.70464(10) 0.0203(2) Uani 1 d . . S3 S 0.0738(2) 1.09235(10) 0.68960(9) 0.0175(2) Uani 1 d . . O1 O 0.3416(12) 0.6054(5) 0.4746(6) 0.063(2) Uani 1 d . . O2 O 0.3631(7) 1.0505(3) 0.4200(3) 0.0227(7) Uani 1 d . . O3 O 0.8675(6) 0.4883(3) 0.6807(3) 0.0299(8) Uani 1 d . . O4 O 0.5836(6) 0.6627(3) 0.6591(3) 0.0304(8) Uani 1 d . . O5 O -0.0087(6) 0.7094(3) 0.6629(3) 0.0309(8) Uani 1 d . . O6 O 0.6934(6) 0.8423(3) 0.3391(3) 0.0237(7) Uani 1 d . . O7 O 0.0905(6) 0.9582(3) 0.6764(3) 0.0226(7) Uani 1 d . . O8 O 0.0929(6) 0.8324(3) 0.3770(3) 0.0252(7) Uani 1 d . . C1 C -0.0493(8) 1.0833(4) 0.8458(4) 0.0181(9) Uani 1 d . . C2 C -0.2540(9) 1.1512(5) 0.8751(5) 0.0257(11) Uani 1 d . . C3 C 0.3607(9) 0.8573(5) 1.0018(4) 0.0285(11) Uani 1 d . . C4 C 0.2689(9) 0.9322(5) 0.9119(4) 0.0239(10) Uani 1 d . . C5 C 0.0570(8) 1.0035(4) 0.9375(4) 0.0193(9) Uani 1 d . . C6 C 0.7205(8) 0.5918(4) 0.8656(4) 0.0183(9) Uani 1 d . . C7 C 0.8634(9) 0.6490(5) 0.9192(4) 0.0209(9) Uani 1 d . . C8 C 0.8178(9) 0.6282(5) 1.0478(4) 0.0238(10) Uani 1 d . . C9 C 0.3684(8) 0.4484(4) 0.8819(4) 0.0225(10) Uani 1 d . . C10 C 0.5224(8) 0.5099(4) 0.9347(4) 0.0174(9) Uani 1 d . . H2 H -0.2942(123) 1.1957(64) 0.8177(58) 0.059(21) Uiso 1 d . . H3 H 0.5020(101) 0.8168(51) 0.9859(48) 0.035(15) Uiso 1 d . . H4 H 0.3240(113) 0.9325(59) 0.8452(55) 0.047(19) Uiso 1 d . . H7 H 0.9768(96) 0.6969(50) 0.8801(46) 0.026(14) Uiso 1 d . . H8 H 0.9094(92) 0.6659(47) 1.0878(44) 0.028(14) Uiso 1 d . . H9 H 0.4267(88) 0.4617(47) 0.7887(44) 0.027(13) Uiso 1 d . . H11 H 0.2355(129) 0.5766(68) 0.4096(62) 0.079(23) Uiso 1 d . . H12 H 0.4360(88) 0.5968(54) 0.4532(51) 0.000(15) Uiso 1 d . . H21 H 0.2804(111) 1.0697(63) 0.3929(55) 0.039(21) 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 La1 0.01399(13) 0.01593(12) 0.01380(13) -0.00059(9) -0.00275(9) -0.00191(9) S2 0.0202(6) 0.0204(5) 0.0176(5) 0.0004(5) -0.0032(4) -0.0029(4) S3 0.0164(5) 0.0221(5) 0.0136(5) -0.0041(4) -0.0022(4) -0.0007(4) O1 0.073(4) 0.048(3) 0.101(5) -0.050(3) -0.060(4) 0.034(3) O2 0.022(2) 0.023(2) 0.025(2) -0.0012(15) -0.011(2) -0.0017(14) O3 0.038(2) 0.026(2) 0.027(2) -0.011(2) -0.007(2) 0.006(2) O4 0.029(2) 0.029(2) 0.030(2) 0.007(2) -0.014(2) -0.0013(15) O5 0.030(2) 0.036(2) 0.023(2) -0.001(2) -0.001(2) -0.014(2) O6 0.023(2) 0.029(2) 0.020(2) -0.0097(14) -0.0024(14) -0.0047(14) O7 0.023(2) 0.024(2) 0.020(2) -0.0076(14) -0.0012(13) -0.0010(14) O8 0.029(2) 0.030(2) 0.018(2) -0.0036(14) -0.0102(14) 0.0030(15) C1 0.018(2) 0.023(2) 0.014(2) -0.005(2) -0.003(2) -0.001(2) C2 0.026(3) 0.029(2) 0.022(2) -0.004(2) -0.007(2) 0.009(2) C3 0.021(2) 0.037(3) 0.026(3) -0.008(2) -0.003(2) 0.013(2) C4 0.022(2) 0.033(3) 0.016(2) -0.006(2) -0.002(2) 0.005(2) C5 0.016(2) 0.024(2) 0.017(2) -0.004(2) -0.004(2) 0.000(2) C6 0.018(2) 0.016(2) 0.019(2) -0.003(2) -0.003(2) 0.001(2) C7 0.016(2) 0.020(2) 0.023(2) -0.001(2) 0.001(2) -0.006(2) C8 0.022(2) 0.025(2) 0.027(2) -0.008(2) -0.008(2) -0.002(2) C9 0.022(2) 0.022(2) 0.022(2) -0.002(2) -0.006(2) -0.001(2) C10 0.017(2) 0.018(2) 0.017(2) -0.001(2) -0.004(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 O2 2.344(3) 2_676 ? La1 O2 2.379(4) . ? La1 O5 2.508(3) . ? La1 O8 2.527(3) . ? La1 O6 2.568(3) . ? La1 O4 2.570(3) . ? La1 O1 2.602(5) . ? La1 O7 2.630(3) . ? La1 La1 3.8826(5) 2_676 ? S2 O3 1.452(3) . ? S2 O4 1.457(3) . ? S2 O5 1.461(4) 1_655 ? S2 C6 1.778(4) . ? S3 O8 1.455(3) 2_576 ? S3 O6 1.462(3) 2_676 ? S3 O7 1.464(3) . ? S3 C1 1.773(4) . ? O2 La1 2.344(3) 2_676 ? O5 S2 1.461(4) 1_455 ? O6 S3 1.462(3) 2_676 ? O8 S3 1.455(3) 2_576 ? C1 C2 1.374(6) . ? C1 C5 1.426(6) . ? C2 C3 1.406(7) 2_577 ? C3 C4 1.345(7) . ? C3 C2 1.406(7) 2_577 ? C4 C5 1.420(6) . ? C5 C5 1.438(8) 2_577 ? C6 C7 1.360(6) . ? C6 C10 1.428(6) . ? C7 C8 1.418(7) . ? C8 C9 1.357(7) 2_667 ? C9 C8 1.357(7) 2_667 ? C9 C10 1.425(6) . ? C10 C10 1.442(8) 2_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 La1 O2 69.41(15) 2_676 . ? O2 La1 O5 128.48(11) 2_676 . ? O2 La1 O5 125.04(12) . . ? O2 La1 O8 144.39(12) 2_676 . ? O2 La1 O8 75.91(11) . . ? O5 La1 O8 78.68(11) . . ? O2 La1 O6 80.98(11) 2_676 . ? O2 La1 O6 75.68(11) . . ? O5 La1 O6 146.81(10) . . ? O8 La1 O6 82.96(10) . . ? O2 La1 O4 74.32(11) 2_676 . ? O2 La1 O4 142.90(12) . . ? O5 La1 O4 84.13(11) . . ? O8 La1 O4 137.77(11) . . ? O6 La1 O4 91.40(11) . . ? O2 La1 O1 136.1(2) 2_676 . ? O2 La1 O1 136.1(2) . . ? O5 La1 O1 72.1(2) . . ? O8 La1 O1 68.27(14) . . ? O6 La1 O1 75.5(2) . . ? O4 La1 O1 69.80(14) . . ? O2 La1 O7 76.68(11) 2_676 . ? O2 La1 O7 73.20(11) . . ? O5 La1 O7 65.11(10) . . ? O8 La1 O7 101.13(10) . . ? O6 La1 O7 146.46(10) . . ? O4 La1 O7 106.03(10) . . ? O1 La1 O7 137.2(2) . . ? O2 La1 La1 35.00(9) 2_676 2_676 ? O2 La1 La1 34.42(9) . 2_676 ? O5 La1 La1 136.67(8) . 2_676 ? O8 La1 La1 109.98(8) . 2_676 ? O6 La1 La1 75.75(7) . 2_676 ? O4 La1 La1 108.99(8) . 2_676 ? O1 La1 La1 151.2(2) . 2_676 ? O7 La1 La1 71.57(7) . 2_676 ? O3 S2 O4 112.8(2) . . ? O3 S2 O5 112.8(2) . 1_655 ? O4 S2 O5 111.7(2) . 1_655 ? O3 S2 C6 106.4(2) . . ? O4 S2 C6 107.1(2) . . ? O5 S2 C6 105.4(2) 1_655 . ? O8 S3 O6 111.7(2) 2_576 2_676 ? O8 S3 O7 112.6(2) 2_576 . ? O6 S3 O7 113.1(2) 2_676 . ? O8 S3 C1 106.0(2) 2_576 . ? O6 S3 C1 107.1(2) 2_676 . ? O7 S3 C1 105.7(2) . . ? La1 O2 La1 110.59(15) 2_676 . ? S2 O4 La1 153.4(2) . . ? S2 O5 La1 158.5(2) 1_455 . ? S3 O6 La1 128.3(2) 2_676 . ? S3 O7 La1 136.4(2) . . ? S3 O8 La1 145.4(2) 2_576 . ? C2 C1 C5 121.5(4) . . ? C2 C1 S3 118.0(4) . . ? C5 C1 S3 120.4(3) . . ? C1 C2 C3 119.4(5) . 2_577 ? C4 C3 C2 121.4(4) . 2_577 ? C3 C4 C5 121.3(4) . . ? C1 C5 C4 123.7(4) . . ? C1 C5 C5 117.7(5) . 2_577 ? C4 C5 C5 118.7(5) . 2_577 ? C7 C6 C10 122.2(4) . . ? C7 C6 S2 118.0(4) . . ? C10 C6 S2 119.7(3) . . ? C6 C7 C8 120.0(5) . . ? C9 C8 C7 120.4(4) 2_667 . ? C8 C9 C10 121.3(4) 2_667 . ? C9 C10 C6 123.9(4) . . ? C9 C10 C10 119.0(5) . 2_667 ? C6 C10 C10 117.2(5) . 2_667 ? _refine_diff_density_max 1.256 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.160 _eof