Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Pascal D. C. Dietzel' _publ_contact_author_address ;SINTEF Chemistry and Materials Postboks 124, Blindern N-0314 Oslo Norway ; _publ_contact_author_email pascal.dietzel@sintef.no _publ_contact_author_phone +47-22067350 loop_ _publ_author_name _publ_author_address 'Dietzel, Pascal D. C.' ;SINTEF Chemistry and Materials Postboks 124, Blindern N-0314 Oslo Norway ; 'Blom, Richard' ;SINTEF Chemistry and Materials Postboks 124, Blindern N-0314 Oslo Norway ; 'Fjellv\%ag, Helmer' ;Centre for Materials Science and Nanotechnology, University of Oslo Postboks 1033, Blindern N-0315 Oslo Norway ; data_pd113_p63mmc _database_code_depnum_ccdc_archive 'CCDC 290155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 O22 Sc3' _chemical_formula_sum 'C8 H4 O7.33 Sc' _chemical_formula_weight 262.41 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' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z+1/2' 'x-y, -y, -z' 'x, x-y, -z+1/2' 'y, x, -z' '-x+y, y, -z+1/2' '-x, -x+y, -z' '-x, -y, -z' '-x+y, -x, -z-1/2' 'y, -x+y, -z' 'x, y, -z-1/2' 'x-y, x, -z' '-y, x-y, -z-1/2' 'y, x, z-1/2' '-x+y, y, z' '-x, -x+y, z-1/2' '-y, -x, z' 'x-y, -y, z-1/2' 'x, x-y, z' _cell_length_a 14.5490(18) _cell_length_b 14.5490(18) _cell_length_c 17.767(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3256.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2626 _cell_measurement_theta_min 2.2925 _cell_measurement_theta_max 21.5985 _exptl_crystal_description 'hexagonal bipyramid' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker Smart APEX II' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27123 _diffrn_reflns_av_R_equivalents 0.1355 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.54 _reflns_number_total 1569 _reflns_number_gt 955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1 (Crystal Impact, 2005)' _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^)+(0.0821P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1569 _refine_ls_number_parameters 53 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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 C1 C 0.56113(11) 0.43887(11) 0.86292(14) 0.0382(7) Uani 1 2 d S A 4 C2 C 0.52964(12) 0.47036(12) 0.93334(16) 0.0406(7) Uani 1 2 d S A 4 C3 C 0.43237(18) 0.40312(18) 0.96662(12) 0.0567(7) Uani 1 1 d . A 4 O1 O 0.6667 0.3333 0.7500 0.0278(10) Uani 1 12 d S . 4 O4 O 0.83004(12) 0.6601(2) 0.7500 0.0584(9) Uani 1 4 d S B 4 O2 O 0.65002(11) 0.50236(10) 0.83489(7) 0.0424(4) Uani 1 1 d . A 4 O3 O 0.3571(3) 0.3069(3) 0.9430(2) 0.121(2) Uani 0.50 1 d P A 4 H3 H 0.3776 0.2909 0.9035 0.181 Uiso 0.50 1 calc PR A 4 Sc1 Sc 0.74683(3) 0.49365(5) 0.7500 0.0259(2) Uani 1 4 d S . 4 H1 H 0.8645(9) 0.7291(19) 0.7188(11) 0.029(7) Uiso 1 2 d S . . 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 C1 0.0457(13) 0.0457(13) 0.0269(13) -0.0045(6) 0.0045(6) 0.0256(15) C2 0.0441(12) 0.0441(12) 0.0331(14) -0.0081(6) 0.0081(6) 0.0218(14) C3 0.0480(13) 0.0481(14) 0.0535(14) -0.0214(11) 0.0147(11) 0.0088(11) O1 0.0318(15) 0.0318(15) 0.020(2) 0.000 0.000 0.0159(7) O4 0.0649(17) 0.0310(17) 0.068(2) 0.000 0.000 0.0155(9) O2 0.0524(9) 0.0438(9) 0.0322(7) -0.0021(6) 0.0124(7) 0.0250(7) O3 0.081(3) 0.078(3) 0.111(3) -0.070(2) 0.060(2) -0.028(2) Sc1 0.0304(3) 0.0287(4) 0.0182(3) 0.000 0.000 0.0143(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 C1 O2 1.2566(18) . ? C1 O2 1.2566(18) 22_665 ? C1 C2 1.482(4) . ? C2 C3 1.387(3) . ? C2 C3 1.387(3) 22_665 ? C3 O3 1.342(4) . ? C3 C3 1.396(4) 10_557 ? O1 Sc1 2.0200(7) 14_667 ? O1 Sc1 2.0200(7) 3_655 ? O1 Sc1 2.0200(7) . ? O4 Sc1 2.097(3) . ? O4 H1 1.03(2) . ? O2 Sc1 2.1102(12) . ? O3 H3 0.8400 . ? Sc1 O2 2.1102(12) 20_655 ? Sc1 O2 2.1102(12) 11_656 ? Sc1 O2 2.1103(12) 16_557 ? Sc1 Sc1 3.4987(13) 3_655 ? Sc1 Sc1 3.4987(12) 14_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 C1 O2 123.8(2) . 22_665 ? O2 C1 C2 118.10(12) . . ? O2 C1 C2 118.10(12) 22_665 . ? C3 C2 C3 119.2(2) . 22_665 ? C3 C2 C1 120.40(12) . . ? C3 C2 C1 120.40(12) 22_665 . ? O3 C3 C2 127.9(2) . . ? O3 C3 C3 111.68(16) . 10_557 ? C2 C3 C3 120.39(12) . 10_557 ? Sc1 O1 Sc1 120.000(1) 14_667 3_655 ? Sc1 O1 Sc1 120.0 14_667 . ? Sc1 O1 Sc1 120.0 3_655 . ? Sc1 O4 H1 147.5(11) . . ? C1 O2 Sc1 135.36(14) . . ? C3 O3 H3 109.5 . . ? O1 Sc1 O4 180.00(4) . . ? O1 Sc1 O2 92.98(4) . 20_655 ? O4 Sc1 O2 87.02(4) . 20_655 ? O1 Sc1 O2 92.98(4) . 11_656 ? O4 Sc1 O2 87.02(4) . 11_656 ? O2 Sc1 O2 91.25(8) 20_655 11_656 ? O1 Sc1 O2 92.98(4) . . ? O4 Sc1 O2 87.02(4) . . ? O2 Sc1 O2 88.44(8) 20_655 . ? O2 Sc1 O2 174.04(8) 11_656 . ? O1 Sc1 O2 92.98(4) . 16_557 ? O4 Sc1 O2 87.02(4) . 16_557 ? O2 Sc1 O2 174.04(8) 20_655 16_557 ? O2 Sc1 O2 88.44(8) 11_656 16_557 ? O2 Sc1 O2 91.24(8) . 16_557 ? O1 Sc1 Sc1 30.0 . 3_655 ? O4 Sc1 Sc1 150.0 . 3_655 ? O2 Sc1 Sc1 113.19(4) 20_655 3_655 ? O2 Sc1 Sc1 113.19(4) 11_656 3_655 ? O2 Sc1 Sc1 72.32(4) . 3_655 ? O2 Sc1 Sc1 72.32(4) 16_557 3_655 ? O1 Sc1 Sc1 30.0 . 14_667 ? O4 Sc1 Sc1 150.0 . 14_667 ? O2 Sc1 Sc1 72.32(4) 20_655 14_667 ? O2 Sc1 Sc1 72.32(4) 11_656 14_667 ? O2 Sc1 Sc1 113.19(4) . 14_667 ? O2 Sc1 Sc1 113.19(4) 16_557 14_667 ? Sc1 Sc1 Sc1 60.0 3_655 14_667 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.507 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.069 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.018 -0.013 -0.002 1965.5 617.7 _platon_squeeze_details ; R-values before SQUEEZE: R1(I>2s) = 0.1153, wR2(all data) = 0.3933 ;