Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_name 'Ignazio L. Fragala' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_volume ? _journal_year ? _journal_page_first ? loop_ _publ_author_name 'Ignazio Fragala' 'Anna M. Borzi' 'Francessco Castelli' 'Paolo Dapporta' 'Walter Dastru' 'Roberto Gobetto' ; G.Malandrino ; 'Patrizia Rossi' _publ_contact_author ; Ignazio L. Fragala Dipartimento di Scienze Chimiche Universita di Catania Viale Andrea Doria 6 I-95125 Catania, ITALY ; _publ_contact_author_email lfragala@dipchi.unict.it _publ_section_title ; Synthesis, characterization and mass transport properties of novel thallium ion precursors for MOCVD applications ; data_Tl(hfa)xdiglyme _database_code_CSD 190969 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Tl(hfa)xdiglyme _chemical_melting_point ? _chemical_formula_moiety '(Tl+),(C5 H1 O2 F6 -1), C6 H14 O3' _chemical_formula_sum 'C11 H15 F6 O5 Tl1' _chemical_formula_weight 545.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -4.1627 8.0900 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 8.389(2) _cell_length_b 10.537(2) _cell_length_c 18.202(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1609.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 20.114 _exptl_absorpt_correction_type 'SADABS; SHELDRICK' _exptl_absorpt_correction_T_min 2.81E-07 _exptl_absorpt_correction_T_max 5.74E-06 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Siemens Cu rotating anode' _diffrn_radiation_monochromator 'Gobel mirrors' _diffrn_measurement_device_type 'Siemens/SMART CCD' _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 4640 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.85 _diffrn_reflns_theta_max 56.27 _reflns_number_total 1077 _reflns_number_gt 987 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SIR-97 (Altomare, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PARST-97 (Nardelli, 1997)' _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^)+(0.1478P)^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 1077 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Tl1 Tl 1.10310(9) 0.27984(5) 0.7500 0.0497(5) Uani 1 2 d S . . F1 F 0.8330(12) -0.0179(8) 0.5538(4) 0.078(2) Uani 1 1 d . . . F2 F 0.9845(14) -0.1521(10) 0.6031(6) 0.100(3) Uani 1 1 d . . . F3 F 0.7372(13) -0.1643(9) 0.6185(5) 0.085(2) Uani 1 1 d . . . O1 O 0.9292(11) 0.1095(9) 0.6709(5) 0.061(2) Uani 1 1 d . . . O2 O 0.8478(15) 0.4597(11) 0.7500 0.050(3) Uani 1 2 d S . . O3 O 0.9991(13) 0.4015(8) 0.8876(5) 0.067(2) Uani 1 1 d . . . C1 C 0.844(3) -0.0576(17) 0.7500 0.057(4) Uani 1 2 d S . . C2 C 0.8760(15) -0.0009(13) 0.6816(8) 0.050(3) Uani 1 1 d . . . C3 C 0.8542(18) -0.0841(13) 0.6138(7) 0.056(3) Uani 1 1 d . . . C4 C 0.8406(19) 0.5350(13) 0.8142(8) 0.061(3) Uani 1 1 d . . . H4A H 0.7420 0.5831 0.8148 0.064(14) Uiso 1 1 calc R . . H4B H 0.9289 0.5944 0.8149 0.064(14) Uiso 1 1 calc R . . C5 C 0.8486(17) 0.4498(14) 0.8809(7) 0.060(3) Uani 1 1 d . . . H5A H 0.8214 0.4979 0.9246 0.064(14) Uiso 1 1 calc R . . H5B H 0.7725 0.3811 0.8758 0.064(14) Uiso 1 1 calc R . . C6 C 1.017(2) 0.3255(12) 0.9521(7) 0.072(4) Uani 1 1 d . . . H6A H 1.0026 0.3776 0.9949 0.064(14) Uiso 1 1 calc R . . H6B H 1.1218 0.2889 0.9529 0.064(14) Uiso 1 1 calc R . . H6C H 0.9387 0.2591 0.9519 0.064(14) Uiso 1 1 calc R . . H1C H 0.7499 -0.1320 0.7500 0.064(14) Uiso 1 2 calc SR . . 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 Tl1 0.0683(8) 0.0392(7) 0.0415(7) 0.000 0.000 -0.0006(3) F1 0.120(6) 0.069(5) 0.045(4) -0.004(4) -0.014(4) -0.005(5) F2 0.110(8) 0.103(7) 0.088(6) -0.043(6) -0.026(6) 0.038(7) F3 0.111(7) 0.073(5) 0.071(5) -0.015(4) -0.009(5) -0.026(6) O1 0.090(6) 0.047(5) 0.045(5) 0.005(4) 0.004(4) -0.011(4) O2 0.066(7) 0.045(6) 0.040(6) 0.000 0.000 0.007(6) O3 0.094(7) 0.048(4) 0.060(5) 0.000(4) -0.002(5) 0.007(5) C1 0.081(12) 0.039(9) 0.052(10) 0.000 0.000 -0.016(10) C2 0.066(7) 0.032(6) 0.053(8) 0.001(5) 0.005(5) 0.005(6) C3 0.076(9) 0.043(7) 0.050(7) -0.003(6) -0.008(6) 0.003(8) C4 0.075(9) 0.057(8) 0.051(7) -0.010(6) 0.000(7) 0.005(8) C5 0.061(9) 0.065(8) 0.055(8) -0.016(7) 0.013(6) -0.009(8) C6 0.123(13) 0.040(6) 0.052(7) 0.009(6) -0.007(8) -0.008(9) _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 Tl1 O1 2.725(9) . ? Tl1 O1 2.725(9) 6_557 ? Tl1 O2 2.86(1) . ? Tl1 O3 2.945(9) . ? Tl1 O3 2.945(9) 6_557 ? Tl1 O2 3.25(1) 3_556 ? Tl1 O1 3.304(9) 3_556 ? Tl1 O1 3.304(9) 8_665 ? F1 C3 1.307(16) . ? F2 C3 1.321(18) . ? F3 C3 1.299(17) . ? O1 C2 1.261(18) . ? O2 C4 1.413(15) . ? O2 C4 1.413(15) 6_557 ? O3 C5 1.367(18) . ? O3 C6 1.429(16) . ? C1 C2 1.408(17) 6_557 ? C1 C2 1.408(17) . ? C2 C3 1.52(2) . ? C4 C5 1.51(2) . ? 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 O1 Tl1 O1 63.8(3) . 6_557 ? O1 Tl1 O2 92.0(2) . . ? O1 Tl1 O2 92.0(2) 6_557 . ? O1 Tl1 O3 125.3(3) . . ? O1 Tl1 O3 71.3(3) 6_557 . ? O2 Tl1 O3 59.3(2) . . ? O1 Tl1 O3 125.3(3) 6_557 6_557 ? O1 Tl1 O3 71.3(3) . 6_557 ? O2 Tl1 O3 59.3(2) . 6_557 ? O3 Tl1 O3 117.5(2) . 6_557 ? O1 Tl1 O2 80.0(2) . 3_556 ? O1 Tl1 O2 80.0(2) 6_557 3_556 ? O2 Tl1 O2 170.6(3) . 3_556 ? O3 Tl1 O2 121.6(2) . 3_556 ? O3 Tl1 O2 121.6(2) 6_557 3_556 ? O1 Tl1 O1 155.0(3) . 3_556 ? O1 Tl1 O1 116.4(3) 6_557 3_556 ? O2 Tl1 O1 112.7(2) . 3_556 ? O3 Tl1 O1 73.8(2) . 3_556 ? O3 Tl1 O1 117.5(2) 6_557 3_556 ? O2 Tl1 O1 75.6(2) 3_556 3_556 ? O1 Tl1 O1 116.4(3) . 8_665 ? O1 Tl1 O1 155.0(3) 6_557 8_665 ? O2 Tl1 O1 112.7(2) . 8_665 ? O3 Tl1 O1 117.5(2) . 8_665 ? O3 Tl1 O1 73.8(2) 6_557 8_665 ? O2 Tl1 O1 75.6(2) 3_556 8_665 ? O1 Tl1 O1 51.7(3) 3_556 8_665 ? C2 O1 Tl1 135.7(10) . . ? C4 O2 C4 111.5(15) . 6_557 ? C5 O3 C6 112.3(12) . . ? C2 C1 C2 124.4(17) 6_557 . ? O1 C2 C1 126.6(14) . . ? O1 C2 C3 116.6(13) . . ? C1 C2 C3 116.7(12) . . ? F3 C3 F1 107.5(11) . . ? F3 C3 F2 106.4(11) . . ? F1 C3 F2 106.2(12) . . ? F3 C3 C2 114.2(12) . . ? F1 C3 C2 112.7(11) . . ? F2 C3 C2 109.4(11) . . ? O2 C4 C5 109.2(11) . . ? O3 C5 C4 109.5(11) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 56.27 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.352 _refine_diff_density_min -4.357 _refine_diff_density_rms 0.372