Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Przemyslaw Starynowicz' _publ_contact_author_address ; Faculty of Chemistry University of Wroclaw ul. F. Joliot-Curie 14 Wroclaw 50-383 POLAND ; _publ_contact_author_email PINGWIN07@O2.PL _publ_section_title ; An ytterbium(II) complex with dimethyl ester of oxydiacetic acid ; loop_ _publ_author_name Przemyslaw Starynowicz data_ybdigly _database_code_depnum_ccdc_archive 'CCDC 638192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 Cl2 O23 Yb' _chemical_formula_weight 858.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 10.203(3) _cell_length_b 10.203(3) _cell_length_c 17.908(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1614.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2699 _cell_measurement_theta_min 4 _cell_measurement_theta_max 37 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 3.150 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Kuma KM4 with a CCD counter' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9258 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.1302 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 37.28 _reflns_number_total 1975 _reflns_number_gt 759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD ver. 1.171' _computing_cell_refinement 'CrysAlis RED ver. 1.171' _computing_data_reduction 'CrysAlis RED ver. 1.171' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary vectmap _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1975 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2190 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 0.000 _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 Yb Yb 0.0000 0.0000 0.2500 0.0542(2) Uani 1 6 d S . . Cl Cl 0.3333 -0.3333 0.35343(12) 0.0755(6) Uani 1 3 d S . . O1 O 0.1540(4) 0.1890(4) 0.15028(18) 0.0696(10) Uani 1 1 d . . . O2 O 0.2200(4) 0.4054(5) 0.0893(2) 0.0887(12) Uani 1 1 d . . . O3 O 0.0000 0.2457(4) 0.2500 0.0592(12) Uani 1 2 d S . . O11 O 0.3333 -0.3333 0.4300(5) 0.181(6) Uani 1 3 d S . . O12 O 0.2008(6) -0.3378(7) 0.3280(3) 0.1347(17) Uani 1 1 d . . . C1 C 0.1546(6) 0.3069(6) 0.1434(2) 0.0646(12) Uani 1 1 d . . . C2 C 0.0720(7) 0.3578(5) 0.1942(2) 0.0760(16) Uani 1 1 d . . . H2A H 0.1425 0.4540 0.2169 0.091 Uiso 1 1 calc R . . H2B H -0.0025 0.3701 0.1663 0.091 Uiso 1 1 calc R . . C3 C 0.3023(8) 0.3710(8) 0.0349(3) 0.127(3) Uani 1 1 d . . . H3A H 0.3475 0.4515 -0.0010 0.190 Uiso 1 1 calc R . . H3B H 0.2343 0.2782 0.0099 0.190 Uiso 1 1 calc R . . H3C H 0.3802 0.3604 0.0595 0.190 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb 0.0460(2) 0.0460(2) 0.0705(3) 0.000 0.000 0.02302(11) Cl 0.0757(9) 0.0757(9) 0.0753(13) 0.000 0.000 0.0378(4) O1 0.059(2) 0.066(2) 0.082(2) 0.017(2) 0.0141(18) 0.030(2) O2 0.095(3) 0.081(3) 0.088(2) 0.029(2) 0.007(3) 0.042(2) O3 0.075(3) 0.056(2) 0.054(3) -0.0021(11) -0.004(2) 0.0375(16) O11 0.231(9) 0.231(9) 0.080(5) 0.000 0.000 0.115(5) O12 0.092(3) 0.115(4) 0.210(5) -0.007(4) -0.024(4) 0.061(3) C1 0.059(4) 0.060(3) 0.066(3) 0.007(2) 0.001(3) 0.023(4) C2 0.114(5) 0.058(3) 0.052(3) -0.003(2) -0.015(3) 0.041(3) C3 0.102(5) 0.168(8) 0.143(6) 0.079(6) 0.062(5) 0.093(6) _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 Yb O3 2.507(4) 2 ? Yb O3 2.507(4) . yes Yb O3 2.507(4) 3 ? Yb O1 2.519(3) 4 ? Yb O1 2.519(3) 2 ? Yb O1 2.519(3) 6 ? Yb O1 2.519(3) 3 ? Yb O1 2.519(3) . yes Yb O1 2.519(3) 5 ? Cl O11 1.371(9) . ? Cl O12 1.407(5) . ? Cl O12 1.407(5) 3_655 ? Cl O12 1.407(5) 2_545 ? O1 C1 1.207(6) . ? O2 C1 1.313(6) . ? O2 C3 1.440(6) . ? O3 C2 1.416(5) . ? O3 C2 1.416(5) 6 ? C1 C2 1.498(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 O3 Yb O3 120.0 2 . ? O3 Yb O3 120.0 2 3 ? O3 Yb O3 120.000(1) . 3 ? O3 Yb O1 134.00(8) 2 4 ? O3 Yb O1 76.04(8) . 4 ? O3 Yb O1 63.04(8) 3 4 ? O3 Yb O1 63.04(8) 2 2 ? O3 Yb O1 76.04(8) . 2 ? O3 Yb O1 134.00(8) 3 2 ? O1 Yb O1 152.09(16) 4 2 ? O3 Yb O1 76.04(8) 2 6 ? O3 Yb O1 63.04(8) . 6 ? O3 Yb O1 134.00(8) 3 6 ? O1 Yb O1 75.30(13) 4 6 ? O1 Yb O1 92.00(16) 2 6 ? O3 Yb O1 76.04(8) 2 3 ? O3 Yb O1 134.00(8) . 3 ? O3 Yb O1 63.04(8) 3 3 ? O1 Yb O1 126.07(17) 4 3 ? O1 Yb O1 75.30(13) 2 3 ? O1 Yb O1 152.09(16) 6 3 ? O3 Yb O1 134.00(8) 2 . ? O3 Yb O1 63.04(8) . . ? O3 Yb O1 76.04(8) 3 . ? O1 Yb O1 92.00(16) 4 . ? O1 Yb O1 75.30(13) 2 . ? O1 Yb O1 126.07(17) 6 . ? O1 Yb O1 75.30(13) 3 . ? O3 Yb O1 63.04(8) 2 5 ? O3 Yb O1 134.00(8) . 5 ? O3 Yb O1 76.04(8) 3 5 ? O1 Yb O1 75.30(13) 4 5 ? O1 Yb O1 126.07(17) 2 5 ? O1 Yb O1 75.30(13) 6 5 ? O1 Yb O1 92.00(16) 3 5 ? O1 Yb O1 152.09(16) . 5 ? O11 Cl O12 108.9(2) . . ? O11 Cl O12 108.9(2) . 3_655 ? O12 Cl O12 110.0(2) . 3_655 ? O11 Cl O12 108.9(2) . 2_545 ? O12 Cl O12 110.0(2) . 2_545 ? O12 Cl O12 110.0(2) 3_655 2_545 ? C1 O1 Yb 121.7(3) . . ? C1 O2 C3 116.6(5) . . ? C2 O3 C2 113.5(5) . 6 ? C2 O3 Yb 123.2(3) . . ? C2 O3 Yb 123.2(3) 6 . ? O1 C1 O2 125.9(5) . . ? O1 C1 C2 124.1(4) . . ? O2 C1 C2 110.0(5) . . ? O3 C2 C1 107.7(4) . . ? _diffrn_measured_fraction_theta_max 0.703 _diffrn_reflns_theta_full 37.28 _diffrn_measured_fraction_theta_full 0.702 _refine_diff_density_max 0.691 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.075