# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_platon _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H1 Gd1 O9' _chemical_formula_sum 'C4 H1 Gd1 O9' _chemical_formula_weight 350.30 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' Gd Gd -0.1653 3.9035 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 11.8981(6) _cell_length_b 8.1956(5) _cell_length_c 10.0764(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.396(3) _cell_angle_gamma 90.00 _cell_volume 976.45(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3700 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.75 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644.0 _exptl_absorpt_coefficient_mu 6.816 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.071 _exptl_absorpt_correction_T_max 0.194 _exptl_absorpt_process_details multi-scan _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 APEX-II _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4304 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.44 _reflns_number_total 2234 _reflns_number_gt 1986 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+5.7666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2234 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _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 Gd1 Gd 0.254946(17) 0.50400(3) 0.11831(2) 0.00740(8) Uani 1 1 d . . . O5 O 0.3903(4) 0.2988(6) 0.1530(5) 0.0366(12) Uani 1 1 d . . . O7 O 0.4319(4) 0.6031(8) 0.0527(4) 0.0378(12) Uani 1 1 d . . . O8 O 0.3113(10) 0.7289(16) 0.2589(13) 0.131(4) Uani 1 1 d . . . O4 O 0.2451(4) 0.0914(8) -0.1548(4) 0.0312(11) Uani 1 1 d . . . O9 O 0.0791(4) 0.5885(7) 0.1742(5) 0.0363(11) Uani 1 1 d . . . O1 O 0.1428(3) 0.2624(5) 0.0980(4) 0.0177(8) Uani 1 1 d . . . O3 O 0.2056(4) -0.2672(7) -0.0251(5) 0.0361(12) Uani 1 1 d . . . O6 O 0.2452(4) 0.4231(6) -0.1135(4) 0.0289(10) Uani 1 1 d . . . H6 H 0.2410 0.5046 -0.1610 0.043 Uiso 1 1 calc R . . O2 O 0.0736(11) -0.0897(18) 0.2137(14) 0.138(4) Uani 1 1 d . . . C3 C 0.1769(8) -0.1103(16) -0.0065(9) 0.059(3) Uani 1 1 d . . . C2 C 0.1212(11) -0.0437(13) 0.1018(13) 0.067(3) Uani 1 1 d . . . C1 C 0.1483(6) 0.1254(12) 0.0501(7) 0.0413(18) Uani 1 1 d . . . C4 C 0.2001(6) 0.0341(9) -0.0592(6) 0.0328(15) 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 Gd1 0.01069(11) 0.00459(12) 0.00756(11) -0.00043(8) 0.00389(7) 0.00041(8) O5 0.046(3) 0.025(2) 0.042(3) 0.017(2) 0.018(2) 0.019(2) O7 0.026(2) 0.054(3) 0.034(2) -0.020(2) 0.0057(18) 0.015(2) O8 0.120(8) 0.098(9) 0.171(10) -0.028(9) 0.000(8) 0.039(8) O4 0.030(2) 0.057(3) 0.0068(15) -0.0033(19) 0.0027(14) 0.000(2) O9 0.036(2) 0.041(3) 0.037(2) 0.001(2) 0.0267(19) 0.000(2) O1 0.0146(16) 0.026(2) 0.0136(16) -0.0040(16) 0.0053(13) 0.0031(16) O3 0.037(3) 0.051(3) 0.023(2) -0.010(2) 0.0141(19) 0.000(2) O6 0.044(2) 0.026(3) 0.0186(18) 0.0058(17) 0.0107(17) 0.003(2) O2 0.144(10) 0.103(9) 0.166(12) -0.007(10) 0.016(9) -0.005(10) C3 0.056(5) 0.080(7) 0.044(4) -0.023(5) 0.017(4) -0.002(6) C2 0.084(8) 0.038(5) 0.081(7) -0.005(6) 0.018(6) 0.002(6) C1 0.037(4) 0.052(5) 0.037(4) 0.003(4) 0.013(3) -0.012(4) C4 0.036(3) 0.036(4) 0.025(3) 0.008(3) -0.001(2) -0.020(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 Gd1 O5 2.328(5) . ? Gd1 O9 2.332(5) . ? Gd1 O8 2.376(13) . ? Gd1 O1 2.384(4) . ? Gd1 O3 2.400(6) 1_565 ? Gd1 O7 2.417(5) . ? Gd1 O6 2.419(4) . ? Gd1 O4 2.431(4) 4_566 ? O4 C4 1.246(8) . ? O4 Gd1 2.431(4) 4_565 ? O1 C1 1.226(10) . ? O3 C3 1.348(13) . ? O3 Gd1 2.400(6) 1_545 ? O6 H6 0.8200 . ? O2 C2 1.370(16) . ? C3 C4 1.338(14) . ? C3 C2 1.446(14) . ? C2 C1 1.528(15) . ? C1 C4 1.518(11) . ? 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 O5 Gd1 O9 143.40(18) . . ? O5 Gd1 O8 109.1(3) . . ? O9 Gd1 O8 80.0(3) . . ? O5 Gd1 O1 77.52(17) . . ? O9 Gd1 O1 76.04(17) . . ? O8 Gd1 O1 144.5(4) . . ? O5 Gd1 O3 140.69(15) . 1_565 ? O9 Gd1 O3 75.36(17) . 1_565 ? O8 Gd1 O3 77.7(3) . 1_565 ? O1 Gd1 O3 120.02(16) . 1_565 ? O5 Gd1 O7 71.00(19) . . ? O9 Gd1 O7 143.0(2) . . ? O8 Gd1 O7 72.9(3) . . ? O1 Gd1 O7 138.76(16) . . ? O3 Gd1 O7 74.64(18) 1_565 . ? O5 Gd1 O6 84.53(17) . . ? O9 Gd1 O6 111.52(17) . . ? O8 Gd1 O6 140.2(4) . . ? O1 Gd1 O6 73.92(15) . . ? O3 Gd1 O6 69.55(16) 1_565 . ? O7 Gd1 O6 77.15(16) . . ? O5 Gd1 O4 74.42(17) . 4_566 ? O9 Gd1 O4 74.34(17) . 4_566 ? O8 Gd1 O4 74.3(4) . 4_566 ? O1 Gd1 O4 74.24(16) . 4_566 ? O3 Gd1 O4 141.55(17) 1_565 4_566 ? O7 Gd1 O4 119.99(15) . 4_566 ? O6 Gd1 O4 144.86(19) . 4_566 ? C4 O4 Gd1 132.5(5) . 4_565 ? C1 O1 Gd1 137.8(4) . . ? C3 O3 Gd1 135.3(5) . 1_545 ? Gd1 O6 H6 109.5 . . ? C4 C3 O3 136.2(7) . . ? C4 C3 C2 95.6(9) . . ? O3 C3 C2 127.5(10) . . ? O2 C2 C3 141.7(12) . . ? O2 C2 C1 130.7(11) . . ? C3 C2 C1 87.3(9) . . ? O1 C1 C4 141.3(7) . . ? O1 C1 C2 132.3(7) . . ? C4 C1 C2 85.3(7) . . ? O4 C4 C3 140.0(8) . . ? O4 C4 C1 128.3(7) . . ? C3 C4 C1 91.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Gd1 O1 C1 -39.2(7) . . . . ? O9 Gd1 O1 C1 166.3(7) . . . . ? O8 Gd1 O1 C1 -144.6(8) . . . . ? O3 Gd1 O1 C1 102.7(7) 1_565 . . . ? O7 Gd1 O1 C1 1.4(8) . . . . ? O6 Gd1 O1 C1 48.6(7) . . . . ? O4 Gd1 O1 C1 -116.3(7) 4_566 . . . ? Gd1 O3 C3 C4 139.4(9) 1_545 . . . ? Gd1 O3 C3 C2 -28.7(15) 1_545 . . . ? C4 C3 C2 O2 -175.2(17) . . . . ? O3 C3 C2 O2 -3(3) . . . . ? C4 C3 C2 C1 -1.8(8) . . . . ? O3 C3 C2 C1 169.9(9) . . . . ? Gd1 O1 C1 C4 -27.0(15) . . . . ? Gd1 O1 C1 C2 137.0(9) . . . . ? O2 C2 C1 O1 6(2) . . . . ? C3 C2 C1 O1 -168.4(9) . . . . ? O2 C2 C1 C4 176.2(14) . . . . ? C3 C2 C1 C4 1.6(7) . . . . ? Gd1 O4 C4 C3 33.4(14) 4_565 . . . ? Gd1 O4 C4 C1 -147.6(6) 4_565 . . . ? O3 C3 C4 O4 10.5(19) . . . . ? C2 C3 C4 O4 -178.9(10) . . . . ? O3 C3 C4 C1 -168.7(11) . . . . ? C2 C3 C4 C1 1.8(8) . . . . ? O1 C1 C4 O4 -12.9(16) . . . . ? C2 C1 C4 O4 178.9(8) . . . . ? O1 C1 C4 C3 166.5(11) . . . . ? C2 C1 C4 C3 -1.7(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.810 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 900722'