Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Francisco Montilla Ramos' 'Teresa Aviles' 'Dante Masi' 'Carlo Mealli' 'Manuel Nunes da Ponte' 'Chris Prevett' 'Vitor Rosa' _publ_contact_author_name 'Dr Francisco Montilla Ramos' _publ_contact_author_address ; Departmento de Química Inorgánica Universidad de Sevilla Aptdo 553 Sevilla 41071 SPAIN ; _publ_contact_author_email MONTILLA@US.ES _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Trimethylsilyl-substituted ligands as solubilizers of metal complexes in supercritical carbon dioxide. ; data_teresa _database_code_CSD 200044 _audit_creation_date 2002-02-15T12:39:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C9 H13 CO1 I3 O1 SI1' _chemical_formula_structural 'C9 H13 CO1 I3 O1 SI1' _chemical_formula_sum 'C9 H13 CO I3 O SI' _chemical_formula_weight 604.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.720(3) _cell_length_b 9.2099(11) _cell_length_c 13.7765(10) _cell_angle_alpha 88.762(8) _cell_angle_beta 85.443(15) _cell_angle_gamma 71.088(17) _cell_volume 804.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 2.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 550 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.878 _exptl_absorpt_factor_mur 1.189 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; ? ; _exptl_absorpt_correction_T_min 0.2356 _exptl_absorpt_correction_T_max 0.3023 _exptl_absorpt_correction_t_ave 0.2688 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 0.22157E-1 _diffrn_orient_matrix_UB_12 -0.14719E-1 _diffrn_orient_matrix_UB_13 -0.72233E-1 _diffrn_orient_matrix_UB_21 -0.48616E-1 _diffrn_orient_matrix_UB_22 0.113828 _diffrn_orient_matrix_UB_23 -0.9017E-2 _diffrn_orient_matrix_UB_31 0.148436 _diffrn_orient_matrix_UB_32 0.16E-4 _diffrn_orient_matrix_UB_33 0.0019 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 15 _diffrn_standards_decay_corr_max 1.188 _diffrn_standards_decay_corr_min 1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 4 3 -1 3 1 _diffrn_reflns_number 2943 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_unetI/netI 0.0166 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 2816 _reflns_number_gt 2503 _reflns_threshold_expression >2sigma(i) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_refinement 'shelxl-97 (sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0480p)^2^+2.0012p] 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_number_reflns 2816 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.06 _refine_ls_shift/su_mean 0.008 _refine_diff_density_max 0.567 _refine_diff_density_min -1.388 _refine_diff_density_rms 0.201 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' O O 0.0106 0.006 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' SI SI 0.0817 0.0704 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' CO CO 0.3494 0.9721 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' I I -0.4742 1.8119 'INTERNATIONAL TABLES VOL C TABLES 4.2.6.8 AND 6.1.1.4' 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 CO1 CO 0.34968(11) 0.50400(8) 0.22406(5) 0.03667(19) UANI 1 1 D . . . I1 I 0.29868(7) 0.29741(5) 0.11423(3) 0.05835(15) UANI 1 1 D . . . I2 I 0.14974(8) 0.43115(7) 0.37385(3) 0.06768(17) UANI 1 1 D . . . I3 I -0.20225(7) 1.07864(5) 0.03449(3) 0.05793(15) UANI 1 1 D . . . SI1 SI 0.3626(3) 0.8428(2) 0.34698(13) 0.0458(4) UANI 1 1 D . . . O1 O -0.0496(8) 0.7070(6) 0.1629(5) 0.0835(18) UANI 1 1 D . . . C1 C 0.4854(8) 0.6595(7) 0.2767(4) 0.0409(12) UANI 1 1 D . . . C2 C 0.5252(9) 0.6408(7) 0.1728(4) 0.0424(13) UANI 1 1 D . . . H2 H 0.495(12) 0.725(9) 0.129(6) 0.07(2) UISO 1 1 D . . . C3 C 0.6352(9) 0.4878(8) 0.1493(5) 0.0512(15) UANI 1 1 D . . . H3 H 0.6772 0.4479 0.0868 0.052(18) UISO 1 1 CALC R . . C4 C 0.6716(9) 0.4046(8) 0.2359(6) 0.0596(18) UANI 1 1 D . . . H4 H 0.7413 0.2998 0.241 0.10(3) UISO 1 1 CALC R . . C5 C 0.5839(9) 0.5076(7) 0.3142(5) 0.0495(14) UANI 1 1 D . . . H5 H 0.5887 0.4816 0.3798 0.034(14) UISO 1 1 CALC R . . C6 C 0.1047(10) 0.6294(7) 0.1874(5) 0.0514(15) UANI 1 1 D . . . C7 C 0.1390(12) 0.9699(8) 0.2834(6) 0.0653(19) UANI 1 1 D . . . H7A H 0.0986 1.0718 0.31 0.113(12) UISO 1 1 CALC R . . H7B H 0.0217 0.9318 0.2919 0.113(12) UISO 1 1 CALC R . . H7C H 0.1806 0.9723 0.2152 0.113(12) UISO 1 1 CALC R . . C8 C 0.2735(17) 0.7984(11) 0.4711(5) 0.085(3) UANI 1 1 D . . . H8A H 0.3827 0.715 0.4972 0.113(12) UISO 1 1 CALC R . . H8B H 0.1487 0.7698 0.4686 0.113(12) UISO 1 1 CALC R . . H8C H 0.2428 0.8872 0.512 0.113(12) UISO 1 1 CALC R . . C9 C 0.5717(13) 0.9320(11) 0.3477(8) 0.084(3) UANI 1 1 D . . . H9A H 0.5167 1.0294 0.3806 0.113(12) UISO 1 1 CALC R . . H9B H 0.6198 0.9469 0.2819 0.113(12) UISO 1 1 CALC R . . H9C H 0.6874 0.8662 0.381 0.113(12) 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 CO1 0.0281(4) 0.0372(4) 0.0442(4) -0.0019(3) 0.0012(3) -0.0107(3) I1 0.0564(3) 0.0598(3) 0.0628(3) -0.0201(2) 0.0086(2) -0.0260(2) I2 0.0680(3) 0.0962(4) 0.0512(3) -0.0041(2) 0.0133(2) -0.0474(3) I3 0.0605(3) 0.0485(2) 0.0513(3) -0.00501(18) -0.00614(19) 0.00174(19) SI1 0.0429(9) 0.0505(9) 0.0488(9) -0.0084(7) -0.0042(7) -0.0206(7) O1 0.043(3) 0.062(3) 0.144(6) 0.019(3) -0.025(3) -0.013(2) C1 0.029(3) 0.049(3) 0.045(3) -0.001(2) -0.004(2) -0.013(2) C2 0.037(3) 0.049(3) 0.047(3) 0.001(3) 0.002(2) -0.023(3) C3 0.034(3) 0.064(4) 0.056(4) -0.011(3) 0.011(3) -0.019(3) C4 0.030(3) 0.053(4) 0.090(5) -0.006(4) -0.008(3) -0.003(3) C5 0.035(3) 0.056(4) 0.057(4) 0.010(3) -0.012(3) -0.014(3) C6 0.036(3) 0.044(3) 0.076(4) -0.002(3) -0.001(3) -0.017(3) C7 0.062(4) 0.053(4) 0.077(5) -0.006(3) -0.013(4) -0.012(3) C8 0.126(8) 0.090(6) 0.043(4) -0.013(4) 0.006(4) -0.042(6) C9 0.063(5) 0.087(6) 0.116(7) -0.028(5) -0.002(5) -0.043(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 CO1 C6 1.781(7) . ? CO1 C3 2.067(6) . ? CO1 C2 2.066(6) . ? CO1 C4 2.076(6) . ? CO1 C5 2.089(6) . ? CO1 C1 2.099(6) . ? CO1 I2 2.5686(9) . ? CO1 I1 2.5800(9) . ? I3 I3 2.7362(14) 2_575 ? SI1 C9 1.844(7) . ? SI1 C8 1.849(8) . ? SI1 C7 1.850(7) . ? SI1 C1 1.873(6) . ? O1 C6 1.125(8) . ? C1 C2 1.439(8) . ? C1 C5 1.444(8) . ? C2 C3 1.394(9) . ? C3 C4 1.399(10) . ? C4 C5 1.411(10) . ? 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 C6 CO1 C3 122.5(3) . . ? C6 CO1 C2 95.4(3) . . ? C3 CO1 C2 39.4(3) . . ? C6 CO1 C4 161.0(3) . . ? C3 CO1 C4 39.5(3) . . ? C2 CO1 C4 66.2(3) . . ? C6 CO1 C5 138.9(3) . . ? C3 CO1 C5 66.3(3) . . ? C2 CO1 C5 66.3(2) . . ? C4 CO1 C5 39.6(3) . . ? C6 CO1 C1 101.8(3) . . ? C3 CO1 C1 67.8(2) . . ? C2 CO1 C1 40.4(2) . . ? C4 CO1 C1 67.9(3) . . ? C5 CO1 C1 40.3(2) . . ? C6 CO1 I2 88.8(2) . . ? C3 CO1 I2 148.4(2) . . ? C2 CO1 I2 145.17(17) . . ? C4 CO1 I2 109.0(2) . . ? C5 CO1 I2 88.10(18) . . ? C1 CO1 I2 104.89(16) . . ? C6 CO1 I1 87.3(2) . . ? C3 CO1 I1 91.48(19) . . ? C2 CO1 I1 120.88(17) . . ? C4 CO1 I1 97.7(2) . . ? C5 CO1 I1 133.78(18) . . ? C1 CO1 I1 159.20(16) . . ? I2 CO1 I1 93.81(3) . . ? C9 SI1 C8 112.2(5) . . ? C9 SI1 C7 109.5(4) . . ? C8 SI1 C7 110.9(4) . . ? C9 SI1 C1 105.3(3) . . ? C8 SI1 C1 109.1(4) . . ? C7 SI1 C1 109.7(3) . . ? C2 C1 C5 104.0(5) . . ? C2 C1 SI1 127.6(4) . . ? C5 C1 SI1 128.0(5) . . ? C2 C1 CO1 68.6(3) . . ? C5 C1 CO1 69.5(3) . . ? SI1 C1 CO1 130.7(3) . . ? C3 C2 C1 110.3(6) . . ? C3 C2 CO1 70.3(3) . . ? C1 C2 CO1 71.0(3) . . ? C4 C3 C2 108.3(6) . . ? C4 C3 CO1 70.6(4) . . ? C2 C3 CO1 70.3(3) . . ? C3 C4 C5 108.0(6) . . ? C3 C4 CO1 69.9(3) . . ? C5 C4 CO1 70.7(3) . . ? C4 C5 C1 109.5(6) . . ? C4 C5 CO1 69.7(4) . . ? C1 C5 CO1 70.2(3) . . ? O1 C6 CO1 178.8(7) . . ?