# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'YooJin Kim' ; Department of Chemistry-BK21, Sungkyunkwan University Suwon 440-746 Korea ; 'Duk-Young Jung' ; Department of Chemistry-BK21, Sungkyunkwan University Suwon 440-746 Korea ; _publ_contact_author_name 'Prof Duk-Young Jung' _publ_contact_author_address ; Department of Chemistry-BK21, Sungkyunkwan University Suwon 440-746 Korea ; _publ_contact_author_email dyjung@chem.skku.ac.kr _publ_contact_author_fax '82(31)2907075' _publ_contact_author_phone '82(31)2907074' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Conformation Change of Cyclohexanedicarboxylate Ligand toward 2D and 3D La(III)-organic Coordination Networks ; data_la(cis-chdc)(trans-chdc) _database_code_CSD 175051 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'la(cis-chdc)(trans-chdc)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H21 La O8' _chemical_formula_weight 480.24 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' '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 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6994(15) _cell_length_b 8.3352(15) _cell_length_c 18.8774(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.774(9) _cell_angle_gamma 90.00 _cell_volume 1671.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 5.26 _cell_measurement_theta_max 12.48 _exptl_crystal_description 'BLOCK' _exptl_crystal_colour 'COLORLESS' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.598 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3084 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2916 _reflns_number_gt 2688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+11.4688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2916 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.31128(3) 0.07484(4) 0.238733(17) 0.01683(17) Uani 1 1 d . . . O1 O 0.1404(4) 0.2758(5) 0.1989(2) 0.0254(9) Uani 1 1 d . . . O2 O 0.4591(4) -0.0100(6) 0.3442(2) 0.0313(11) Uani 1 1 d . . . O3 O 0.4379(5) 0.2794(5) 0.1754(3) 0.0351(11) Uani 1 1 d . . . O4 O 0.1584(4) 0.0136(6) 0.3198(3) 0.0324(11) Uani 1 1 d . . . O5 O 0.2633(5) -0.0113(6) 0.1101(2) 0.0349(11) Uani 1 1 d . . . O6 O 0.5158(5) -0.0573(6) 0.1994(3) 0.0409(13) Uani 1 1 d . . . O7 O 0.1772(4) -0.1742(5) 0.1810(2) 0.0263(10) Uani 1 1 d . . . O8 O 0.5984(7) 0.0954(7) 0.1222(4) 0.066(2) Uani 1 1 d . . . HO8 H 0.544(9) 0.172(11) 0.140(5) 0.05(3) Uiso 1 1 d . . . C1 C 0.4327(7) 0.4303(7) 0.1671(4) 0.0251(14) Uani 1 1 d . . . C2 C 0.5456(6) 0.5178(8) 0.1442(4) 0.0306(15) Uani 1 1 d . . . H2 H 0.599(6) 0.439(7) 0.128(3) 0.009(15) Uiso 1 1 d . . . C3 C 0.6138(7) 0.6005(9) 0.2108(5) 0.0378(17) Uani 1 1 d . . . H3A H 0.5534 0.6625 0.2338 0.045 Uiso 1 1 calc R . . H3B H 0.6488 0.5193 0.2442 0.045 Uiso 1 1 calc R . . C4 C 0.7198(7) 0.7115(9) 0.1925(6) 0.052(2) Uani 1 1 d . . . H4A H 0.7536 0.7688 0.2352 0.062 Uiso 1 1 calc R . . H4B H 0.7870 0.6466 0.1773 0.062 Uiso 1 1 calc R . . C5 C 0.6776(7) 0.8325(9) 0.1344(5) 0.042(2) Uani 1 1 d . . . H5 H 0.745(8) 0.887(9) 0.126(4) 0.04(2) Uiso 1 1 d . . . C6 C 0.6138(8) 0.7446(9) 0.0683(5) 0.047(2) Uani 1 1 d . . . H6A H 0.5837 0.8228 0.0322 0.056 Uiso 1 1 calc R . . H6B H 0.6752 0.6770 0.0488 0.056 Uiso 1 1 calc R . . C7 C 0.5031(7) 0.6411(8) 0.0861(4) 0.0328(15) Uani 1 1 d . . . H7A H 0.4387 0.7095 0.1021 0.039 Uiso 1 1 calc R . . H7B H 0.4666 0.5856 0.0434 0.039 Uiso 1 1 calc R . . C8 C 0.5896(7) -0.0383(8) 0.1560(4) 0.0316(15) Uani 1 1 d . . . C9 C 0.1999(6) -0.1341(8) 0.1184(3) 0.0240(13) Uani 1 1 d . . . C10 C 0.1445(6) -0.2337(8) 0.0548(3) 0.0232(13) Uani 1 1 d . . . H10 H 0.158(7) -0.349(9) 0.070(4) 0.029(18) Uiso 1 1 d . . . C11 C 0.0009(5) -0.2081(8) 0.0444(3) 0.0213(12) Uani 1 1 d . . . H11A H -0.0346 -0.2525 0.0851 0.026 Uiso 1 1 calc R . . H11B H -0.0163 -0.0938 0.0431 0.026 Uiso 1 1 calc R . . C12 C -0.0646(6) -0.2845(8) -0.0236(3) 0.0227(13) Uani 1 1 d . . . H12A H -0.1505 -0.2456 -0.0316 0.027 Uiso 1 1 calc R . . H12B H -0.0677 -0.3998 -0.0169 0.027 Uiso 1 1 calc R . . C13 C 0.0011(6) -0.2489(8) -0.0905(3) 0.0233(13) Uani 1 1 d . . . H13 H -0.003(7) -0.141(10) -0.100(4) 0.03(2) Uiso 1 1 d . . . C14 C 0.1416(6) -0.2862(9) -0.0768(3) 0.0282(14) Uani 1 1 d . . . H14A H 0.1814 -0.2588 -0.1188 0.034 Uiso 1 1 calc R . . H14B H 0.1533 -0.4002 -0.0680 0.034 Uiso 1 1 calc R . . C15 C 0.2036(6) -0.1918(8) -0.0128(3) 0.0272(14) Uani 1 1 d . . . H15A H 0.1941 -0.0778 -0.0223 0.033 Uiso 1 1 calc R . . H15B H 0.2929 -0.2159 -0.0056 0.033 Uiso 1 1 calc R . . C16 C 0.4370(5) -0.1561(7) 0.3485(3) 0.0202(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0157(2) 0.0179(2) 0.0167(2) 0.00010(12) 0.00109(14) -0.00006(12) O1 0.022(2) 0.029(2) 0.023(2) -0.0006(18) -0.0054(17) -0.0001(18) O2 0.035(3) 0.025(2) 0.031(2) 0.003(2) -0.008(2) -0.001(2) O3 0.036(3) 0.020(2) 0.054(3) 0.003(2) 0.021(2) 0.001(2) O4 0.031(3) 0.028(2) 0.041(3) -0.001(2) 0.013(2) -0.002(2) O5 0.048(3) 0.033(3) 0.023(2) -0.003(2) 0.000(2) -0.016(2) O6 0.040(3) 0.036(3) 0.051(3) 0.013(2) 0.027(3) 0.011(2) O7 0.036(3) 0.025(2) 0.017(2) 0.0007(17) -0.0043(18) -0.0025(19) O8 0.073(5) 0.031(3) 0.107(6) 0.022(3) 0.063(5) 0.016(3) C1 0.030(4) 0.021(3) 0.027(3) -0.003(2) 0.014(3) 0.001(3) C2 0.024(3) 0.021(3) 0.049(4) 0.000(3) 0.017(3) 0.000(3) C3 0.028(4) 0.030(4) 0.054(5) 0.008(3) 0.001(3) -0.001(3) C4 0.021(4) 0.031(4) 0.104(7) 0.002(4) 0.008(4) 0.000(3) C5 0.025(4) 0.025(4) 0.080(6) 0.003(4) 0.030(4) -0.004(3) C6 0.061(5) 0.028(4) 0.060(5) 0.008(4) 0.042(4) 0.000(4) C7 0.040(4) 0.031(4) 0.030(3) 0.001(3) 0.012(3) -0.004(3) C8 0.029(4) 0.023(3) 0.045(4) -0.001(3) 0.012(3) -0.002(3) C9 0.022(3) 0.027(3) 0.023(3) -0.001(3) 0.001(2) 0.003(3) C10 0.021(3) 0.028(3) 0.020(3) 0.000(3) -0.002(2) -0.001(3) C11 0.020(3) 0.026(3) 0.017(3) -0.005(2) -0.001(2) -0.001(2) C12 0.017(3) 0.029(3) 0.021(3) -0.003(3) -0.002(2) -0.002(2) C13 0.024(3) 0.022(3) 0.023(3) -0.004(2) -0.001(2) 0.000(2) C14 0.025(3) 0.040(4) 0.022(3) -0.007(3) 0.011(3) -0.004(3) C15 0.021(3) 0.037(4) 0.023(3) 0.001(3) 0.003(3) -0.003(3) C16 0.015(3) 0.024(3) 0.022(3) 0.000(2) 0.002(2) 0.004(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 O4 2.422(5) . ? La1 O2 2.495(4) . ? La1 O5 2.527(4) . ? La1 O1 2.528(4) . ? La1 O3 2.560(4) . ? La1 O7 2.578(4) 2 ? La1 O6 2.633(5) . ? La1 O7 2.680(4) . ? La1 O1 2.779(4) 2_545 ? La1 C9 2.996(6) . ? La1 C16 3.025(6) . ? O1 C16 1.277(7) 2 ? O1 La1 2.779(4) 2 ? O2 C16 1.245(8) . ? O3 C1 1.268(7) . ? O4 C1 1.246(8) 2_545 ? O5 C9 1.247(8) . ? O6 C8 1.214(9) . ? O7 C9 1.279(8) . ? O7 La1 2.578(4) 2_545 ? O8 C8 1.293(9) . ? C1 O4 1.246(8) 2 ? C1 C2 1.517(9) . ? C2 C7 1.533(10) . ? C2 C3 1.539(11) . ? C3 C4 1.534(10) . ? C4 C5 1.519(12) . ? C5 C8 1.517(10) 1_565 ? C5 C6 1.535(13) . ? C6 C7 1.535(10) . ? C8 C5 1.517(10) 1_545 ? C9 C10 1.521(8) . ? C10 C15 1.531(8) . ? C10 C11 1.540(8) . ? C11 C12 1.527(8) . ? C12 C13 1.544(8) . ? C13 C16 1.496(8) 4 ? C13 C14 1.527(9) . ? C14 C15 1.527(9) . ? C16 O1 1.277(7) 2_545 ? C16 C13 1.496(8) 4_656 ? 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 O4 La1 O2 81.25(17) . . ? O4 La1 O5 118.12(16) . . ? O2 La1 O5 136.43(17) . . ? O4 La1 O1 78.98(15) . . ? O2 La1 O1 142.52(15) . . ? O5 La1 O1 81.05(16) . . ? O4 La1 O3 150.37(15) . . ? O2 La1 O3 103.93(16) . . ? O5 La1 O3 78.43(16) . . ? O1 La1 O3 79.86(15) . . ? O4 La1 O7 77.81(15) . 2 ? O2 La1 O7 77.22(14) . 2 ? O5 La1 O7 141.81(15) . 2 ? O1 La1 O7 67.67(13) . 2 ? O3 La1 O7 75.07(15) . 2 ? O4 La1 O6 137.35(16) . . ? O2 La1 O6 68.71(18) . . ? O5 La1 O6 72.04(19) . . ? O1 La1 O6 142.10(15) . . ? O3 La1 O6 69.13(15) . . ? O7 La1 O6 121.42(17) 2 . ? O4 La1 O7 74.02(15) . . ? O2 La1 O7 111.33(14) . . ? O5 La1 O7 49.51(14) . . ? O1 La1 O7 93.33(14) . . ? O3 La1 O7 127.84(15) . . ? O7 La1 O7 148.61(3) 2 . ? O6 La1 O7 89.11(16) . . ? O4 La1 O1 69.47(15) . 2_545 ? O2 La1 O1 48.61(14) . 2_545 ? O5 La1 O1 99.14(14) . 2_545 ? O1 La1 O1 144.32(8) . 2_545 ? O3 La1 O1 135.46(14) . 2_545 ? O7 La1 O1 119.03(13) 2 2_545 ? O6 La1 O1 67.98(14) . 2_545 ? O7 La1 O1 62.73(12) . 2_545 ? O4 La1 C9 96.82(17) . . ? O2 La1 C9 126.77(16) . . ? O5 La1 C9 24.25(17) . . ? O1 La1 C9 87.15(15) . . ? O3 La1 C9 102.61(17) . . ? O7 La1 C9 154.79(15) 2 . ? O6 La1 C9 79.20(18) . . ? O7 La1 C9 25.27(15) . . ? O1 La1 C9 80.65(15) 2_545 . ? O4 La1 C16 73.29(16) . . ? O2 La1 C16 23.67(16) . . ? O5 La1 C16 120.05(17) . . ? O1 La1 C16 150.83(15) . . ? O3 La1 C16 121.76(16) . . ? O7 La1 C16 97.32(15) 2 . ? O6 La1 C16 67.02(16) . . ? O7 La1 C16 87.66(15) . . ? O1 La1 C16 24.97(14) 2_545 . ? C9 La1 C16 104.74(17) . . ? C16 O1 La1 152.8(4) 2 . ? C16 O1 La1 88.3(4) 2 2 ? La1 O1 La1 112.09(15) . 2 ? C16 O2 La1 102.8(4) . . ? C1 O3 La1 134.5(4) . . ? C1 O4 La1 147.7(4) 2_545 . ? C9 O5 La1 99.5(4) . . ? C8 O6 La1 139.9(5) . . ? C9 O7 La1 138.9(4) . 2_545 ? C9 O7 La1 91.3(4) . . ? La1 O7 La1 113.78(15) 2_545 . ? O4 C1 O3 123.6(6) 2 . ? O4 C1 C2 117.2(5) 2 . ? O3 C1 C2 119.2(6) . . ? C1 C2 C7 110.3(6) . . ? C1 C2 C3 107.4(6) . . ? C7 C2 C3 110.9(6) . . ? C4 C3 C2 112.2(7) . . ? C5 C4 C3 113.5(6) . . ? C8 C5 C4 114.7(7) 1_565 . ? C8 C5 C6 109.1(7) 1_565 . ? C4 C5 C6 109.7(6) . . ? C7 C6 C5 111.8(6) . . ? C2 C7 C6 111.2(6) . . ? O6 C8 O8 122.4(7) . . ? O6 C8 C5 124.3(6) . 1_545 ? O8 C8 C5 113.3(6) . 1_545 ? O5 C9 O7 119.7(6) . . ? O5 C9 C10 121.1(6) . . ? O7 C9 C10 119.2(6) . . ? O5 C9 La1 56.3(3) . . ? O7 C9 La1 63.4(3) . . ? C10 C9 La1 177.3(4) . . ? C9 C10 C15 111.8(5) . . ? C9 C10 C11 108.4(5) . . ? C15 C10 C11 111.4(5) . . ? C12 C11 C10 113.7(5) . . ? C11 C12 C13 113.5(5) . . ? C16 C13 C14 112.0(5) 4 . ? C16 C13 C12 108.5(5) 4 . ? C14 C13 C12 110.9(5) . . ? C13 C14 C15 110.8(5) . . ? C14 C15 C10 111.0(5) . . ? O2 C16 O1 120.1(5) . 2_545 ? O2 C16 C13 119.6(5) . 4_656 ? O1 C16 C13 120.3(5) 2_545 4_656 ? O2 C16 La1 53.5(3) . . ? O1 C16 La1 66.7(3) 2_545 . ? C13 C16 La1 172.1(4) 4_656 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.762 _refine_diff_density_min -1.879 _refine_diff_density_rms 0.171 data_[La2(H2O)2(trans-chdc)1(cis-chdc)2]2H2O _database_code_CSD 175052 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[La2(H2O)2(trans-chdc)1(cis-chdc)2]2H2O' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H38 La2 O16' _chemical_formula_weight 860.37 _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' '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 8.085(2) _cell_length_b 9.0746(8) _cell_length_c 10.606(3) _cell_angle_alpha 71.981(13) _cell_angle_beta 83.635(14) _cell_angle_gamma 83.845(12) _cell_volume 733.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 5.63 _cell_measurement_theta_max 16.46 _exptl_crystal_description 'BLOCK' _exptl_crystal_colour 'COLORLESS' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method ? _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 2.948 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.4327 _exptl_absorpt_correction_T_max 0.6047 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2729 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2530 _reflns_number_observed 2411 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 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^)+(0.0822P)^2^+0.9350P] 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 2528 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_obs 0.0368 _refine_ls_wR_factor_all 0.0992 _refine_ls_wR_factor_obs 0.0967 _refine_ls_goodness_of_fit_all 0.988 _refine_ls_goodness_of_fit_obs 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_restrained_S_obs 0.992 _refine_ls_shift/esd_max 0.250 _refine_ls_shift/esd_mean 0.010 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 0.25497(3) 0.04409(3) 0.97191(2) 0.01646(14) Uani 1 d . . O1 O 0.0096(4) -0.0356(4) 0.8719(3) 0.0230(7) Uani 1 d . . O2 O 0.3358(5) 0.1883(5) 1.1121(4) 0.0332(8) Uani 1 d . . O3 O 0.2241(4) -0.2206(4) 1.1465(4) 0.0360(9) Uani 1 d . . O4 O 0.3902(5) -0.1524(5) 0.8691(4) 0.0360(9) Uani 1 d . . O5 O 0.1741(5) 0.1304(5) 0.7316(4) 0.0342(9) Uani 1 d . . O6 O 0.4777(4) -0.1496(4) 1.1362(3) 0.0259(7) Uani 1 d . . O7 O 0.0690(5) 0.3131(5) 0.9208(4) 0.0402(9) Uani 1 d . . O8 O 0.4959(25) 0.0998(18) 0.5779(16) 0.089(7) Uani 0.47(2) d P . C1 C 0.4671(6) 0.2137(5) 1.1542(5) 0.0245(10) Uani 1 d . . C2 C 0.4538(6) 0.3225(5) 1.2390(5) 0.0219(10) Uani 1 d . . H2 H 0.4759(6) 0.2578(5) 1.3292(5) 0.026 Uiso 1 calc R . C3 C 0.5872(6) 0.4410(6) 1.1942(5) 0.0255(10) Uani 1 d . . H3A H 0.6969(6) 0.3869(6) 1.1900(5) 0.031 Uiso 1 calc R . H3B H 0.5682(6) 0.5101(6) 1.1060(5) 0.031 Uiso 1 calc R . C4 C 0.5805(7) -0.4645(6) 1.2917(5) 0.0285(11) Uani 1 d . . H4A H 0.6615(7) -0.3870(6) 1.2598(5) 0.034 Uiso 1 calc R . H4B H 0.6108(7) -0.5329(6) 1.3775(5) 0.034 Uiso 1 calc R . C5 C 0.4066(6) -0.3834(5) 1.3085(5) 0.0239(10) Uani 1 d . . H5 H 0.4069(6) -0.3417(5) 1.3834(5) 0.029 Uiso 1 calc R . C6 C 0.2736(7) -0.5008(6) 1.3467(5) 0.0302(11) Uani 1 d . . H6A H 0.2890(7) -0.5708(6) 1.4353(5) 0.036 Uiso 1 calc R . H6B H 0.1641(7) -0.4459(6) 1.3490(5) 0.036 Uiso 1 calc R . C7 C 0.2811(6) 0.4044(6) 1.2493(5) 0.0259(10) Uani 1 d . . H7A H 0.1987(6) 0.3281(6) 1.2795(5) 0.031 Uiso 1 calc R . H7B H 0.2550(6) 0.4727(6) 1.1624(5) 0.031 Uiso 1 calc R . C8 C 0.3684(6) -0.2459(5) 1.1871(5) 0.0232(10) Uani 1 d . . C9 C 0.0617(6) 0.0397(6) 0.7519(5) 0.0227(10) Uani 1 d . . C10 C -0.0117(7) 0.0098(7) 0.6376(5) 0.0298(12) Uani 1 d . . H10 H -0.1254(7) -0.0210(7) 0.6678(5) 0.036 Uiso 1 calc R . C11 C -0.0221(10) 0.1565(7) 0.5170(6) 0.045(2) Uani 1 d . . H11A H 0.0879(10) 0.1948(7) 0.4905(6) 0.053 Uiso 1 calc R . H11B H -0.0955(10) 0.2367(7) 0.5416(6) 0.053 Uiso 1 calc R . C12 C 0.0883(8) -0.1226(7) 0.6012(6) 0.0406(14) Uani 1 d . . H12A H 0.0851(8) -0.2151(7) 0.6775(6) 0.049 Uiso 1 calc R . H12B H 0.2037(8) -0.0979(7) 0.5785(6) 0.049 Uiso 1 calc R . HO7A H 0.1211(8) 0.3768(7) 0.9591(6) 0.232(87) Uiso 1 d R . HO7B H 0.0386(8) 0.3272(7) 0.8259(6) 0.170(61) Uiso 1 d 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 0.0104(2) 0.0205(2) 0.0206(2) -0.00902(13) -0.00146(12) -0.00149(12) O1 0.015(2) 0.038(2) 0.019(2) -0.0121(14) -0.0012(13) -0.0039(14) O2 0.026(2) 0.045(2) 0.041(2) -0.030(2) -0.007(2) -0.003(2) O3 0.014(2) 0.034(2) 0.056(2) -0.008(2) -0.004(2) -0.0017(14) O4 0.024(2) 0.043(2) 0.050(2) -0.031(2) -0.009(2) 0.010(2) O5 0.037(2) 0.043(2) 0.024(2) -0.007(2) -0.006(2) -0.015(2) O6 0.022(2) 0.028(2) 0.024(2) -0.0014(14) -0.0008(14) -0.0078(14) O7 0.034(2) 0.033(2) 0.053(3) -0.010(2) -0.010(2) -0.001(2) O8 0.137(17) 0.069(10) 0.069(10) -0.032(8) -0.002(9) -0.019(9) C1 0.026(3) 0.023(2) 0.025(2) -0.009(2) -0.002(2) 0.000(2) C2 0.024(2) 0.022(2) 0.023(2) -0.011(2) -0.007(2) -0.001(2) C3 0.019(2) 0.029(2) 0.032(3) -0.015(2) -0.003(2) 0.001(2) C4 0.033(3) 0.024(2) 0.032(3) -0.009(2) -0.015(2) -0.002(2) C5 0.033(3) 0.019(2) 0.021(2) -0.009(2) -0.002(2) -0.004(2) C6 0.034(3) 0.023(2) 0.032(3) -0.011(2) 0.011(2) -0.005(2) C7 0.022(2) 0.028(2) 0.030(2) -0.013(2) 0.006(2) -0.006(2) C8 0.020(2) 0.020(2) 0.031(2) -0.010(2) 0.004(2) -0.002(2) C9 0.020(2) 0.031(2) 0.020(2) -0.013(2) -0.004(2) 0.000(2) C10 0.031(3) 0.043(3) 0.019(2) -0.011(2) -0.002(2) -0.013(2) C11 0.063(4) 0.034(3) 0.037(3) -0.011(3) -0.018(3) 0.008(3) C12 0.054(4) 0.039(3) 0.030(3) -0.011(2) -0.017(3) 0.006(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 La1 O2 2.440(3) . ? La1 O4 2.466(4) . ? La1 O6 2.473(3) 2_657 ? La1 O1 2.549(3) 2_557 ? La1 O3 2.557(4) . ? La1 O5 2.561(4) . ? La1 O1 2.614(3) . ? La1 O7 2.662(4) . ? La1 O6 2.737(3) . ? La1 C9 2.961(5) . ? La1 C8 3.034(5) . ? La1 La1 4.0300(9) 2_657 ? O1 C9 1.292(6) . ? O1 La1 2.549(3) 2_557 ? O2 C1 1.265(6) . ? O3 C8 1.262(6) . ? O4 C1 1.259(6) 2_657 ? O5 C9 1.248(6) . ? O6 C8 1.266(6) . ? O6 La1 2.473(3) 2_657 ? C1 O4 1.259(6) 2_657 ? C1 C2 1.516(7) . ? C2 C7 1.519(7) . ? C2 C3 1.537(7) . ? C3 C4 1.528(7) 1_565 ? C4 C3 1.528(7) 1_545 ? C4 C5 1.535(7) . ? C5 C8 1.524(7) . ? C5 C6 1.529(7) . ? C6 C7 1.528(7) 1_545 ? C7 C6 1.528(7) 1_565 ? C9 C10 1.515(7) . ? C10 C12 1.502(8) . ? C10 C11 1.537(8) . ? C11 C12 1.540(8) 2_556 ? C12 C11 1.540(8) 2_556 ? 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 O4 136.58(12) . . ? O2 La1 O6 74.82(13) . 2_657 ? O4 La1 O6 75.61(13) . 2_657 ? O2 La1 O1 80.18(12) . 2_557 ? O4 La1 O1 129.95(13) . 2_557 ? O6 La1 O1 153.61(12) 2_657 2_557 ? O2 La1 O3 99.41(14) . . ? O4 La1 O3 73.41(14) . . ? O6 La1 O3 125.47(11) 2_657 . ? O1 La1 O3 66.68(11) 2_557 . ? O2 La1 O5 132.12(13) . . ? O4 La1 O5 73.49(13) . . ? O6 La1 O5 82.62(12) 2_657 . ? O1 La1 O5 108.87(11) 2_557 . ? O3 La1 O5 127.78(13) . . ? O2 La1 O1 146.46(11) . . ? O4 La1 O1 76.44(12) . . ? O6 La1 O1 130.45(11) 2_657 . ? O1 La1 O1 70.12(12) 2_557 . ? O3 La1 O1 83.16(12) . . ? O5 La1 O1 50.40(11) . . ? O2 La1 O7 72.23(13) . . ? O4 La1 O7 142.94(13) . . ? O6 La1 O7 97.38(12) 2_657 . ? O1 La1 O7 66.55(12) 2_557 . ? O3 La1 O7 133.23(13) . . ? O5 La1 O7 69.51(14) . . ? O1 La1 O7 81.69(12) . . ? O2 La1 O6 73.31(12) . . ? O4 La1 O6 70.28(12) . . ? O6 La1 O6 78.77(11) 2_657 . ? O1 La1 O6 102.15(10) 2_557 . ? O3 La1 O6 48.88(11) . . ? O5 La1 O6 142.31(12) . . ? O1 La1 O6 127.18(11) . . ? O7 La1 O6 145.10(13) . . ? O2 La1 C9 148.41(13) . . ? O4 La1 C9 70.77(12) . . ? O6 La1 C9 105.42(12) 2_657 . ? O1 La1 C9 91.48(12) 2_557 . ? O3 La1 C9 105.13(13) . . ? O5 La1 C9 24.80(13) . . ? O1 La1 C9 25.84(12) . . ? O7 La1 C9 76.48(13) . . ? O6 La1 C9 138.23(12) . . ? O2 La1 C8 85.94(13) . . ? O4 La1 C8 70.36(13) . . ? O6 La1 C8 102.54(12) 2_657 . ? O1 La1 C8 83.76(12) 2_557 . ? O3 La1 C8 24.22(12) . . ? O5 La1 C8 140.70(13) . . ? O1 La1 C8 105.40(12) . . ? O7 La1 C8 145.35(13) . . ? O6 La1 C8 24.67(12) . . ? C9 La1 C8 123.67(13) . . ? O2 La1 La1 69.16(9) . 2_657 ? O4 La1 La1 67.57(9) . 2_657 ? O6 La1 La1 41.76(8) 2_657 2_657 ? O1 La1 La1 133.84(7) 2_557 2_657 ? O3 La1 La1 84.81(8) . 2_657 ? O5 La1 La1 117.29(9) . 2_657 ? O1 La1 La1 143.95(7) . 2_657 ? O7 La1 La1 129.48(9) . 2_657 ? O6 La1 La1 37.01(7) . 2_657 ? C9 La1 La1 132.04(9) . 2_657 ? C8 La1 La1 61.06(9) . 2_657 ? C9 O1 La1 138.4(3) . 2_557 ? C9 O1 La1 92.3(3) . . ? La1 O1 La1 109.88(12) 2_557 . ? C1 O2 La1 138.7(3) . . ? C8 O3 La1 99.6(3) . . ? C1 O4 La1 140.4(3) 2_657 . ? C9 O5 La1 95.8(3) . . ? C8 O6 La1 160.2(3) . 2_657 ? C8 O6 La1 90.9(3) . . ? La1 O6 La1 101.23(11) 2_657 . ? O4 C1 O2 123.7(5) 2_657 . ? O4 C1 C2 117.4(5) 2_657 . ? O2 C1 C2 118.8(4) . . ? C1 C2 C7 113.7(4) . . ? C1 C2 C3 112.4(4) . . ? C7 C2 C3 110.5(4) . . ? C4 C3 C2 110.2(4) 1_565 . ? C3 C4 C5 112.0(4) 1_545 . ? C8 C5 C6 112.9(4) . . ? C8 C5 C4 112.1(4) . . ? C6 C5 C4 110.6(4) . . ? C7 C6 C5 112.2(4) 1_545 . ? C2 C7 C6 110.5(4) . 1_565 ? O6 C8 O3 120.6(4) . . ? O6 C8 C5 119.1(4) . . ? O3 C8 C5 120.0(4) . . ? O6 C8 La1 64.4(2) . . ? O3 C8 La1 56.2(3) . . ? C5 C8 La1 171.8(3) . . ? O5 C9 O1 120.4(4) . . ? O5 C9 C10 121.2(4) . . ? O1 C9 C10 118.4(4) . . ? O5 C9 La1 59.4(2) . . ? O1 C9 La1 61.9(2) . . ? C10 C9 La1 168.2(4) . . ? C12 C10 C9 109.7(5) . . ? C12 C10 C11 111.4(5) . . ? C9 C10 C11 111.7(5) . . ? C10 C11 C12 111.3(5) . 2_556 ? C10 C12 C11 112.3(5) . 2_556 ? _refine_diff_density_max 2.006 _refine_diff_density_min -1.620 _refine_diff_density_rms 0.178