Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _audit_creation_method SHELXL-97 _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof G. Albertin' _publ_contact_author_address ; Dipartimento di Chimica Universit\`a Ca' Foscari di Venezia Dorsoduro 2137 Venice 30123 ITALY ; _publ_contact_author_email ALBERTIN@HELIOS.UNIVE.IT _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Preparation and reactivity of penta- and tetracoordinate platinum(II) hydride complexes with P(OEt)3 and PPh(OEt)2 phosphite ligands ; loop_ _publ_author_name _publ_author_address 'Albertin, Gabriele' ; Dipartimento di Chimica, Universita Ca' Foscari di Venezia, Dorsoduro 2137, 30123 Venezia, Italy ; 'Antoniutti, Stefano' ; Dipartimento di Chimica, Universita Ca' Foscari di Venezia, Dorsoduro 2137, 30123 Venezia, Italy ; 'Busato, Christian' ; Dipartimento di Chimica, Universita Ca' Foscari di Venezia, Dorsoduro 2137, 30123 Venezia, Italy ; 'Castro, Jesus' ; Departamento de Quimica Inorganica Universidade de Vigo 36310-Vigo, Galicia Spain ; 'Garcia-Fontan, M. Soledad' ; Departamento de Quimica Inorganica Universidade de Vigo 36310-Vigo, Galicia Spain ; # 4. DATA data_Pt4P _database_code_depnum_ccdc_archive 'CCDC 269224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H60 O12 P4 Pt, 2(B F4)' _chemical_formula_sum 'C24 H60 B2 F8 O12 P4 Pt' _chemical_formula_weight 1033.31 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 10.6494(16) _cell_length_b 10.6494(16) _cell_length_c 18.205(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2064.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .26 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 3.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715401 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Sheldrick, G. M. SADABS, An empirical absorption correction program for area detector data. University of Gottingen, Germany, 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6872 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.99 _reflns_number_total 1287 _reflns_number_gt 1282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia L.J., 1997)' _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^)+(0.0596P)^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 1287 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Pt Pt 0.0000 0.0000 0.5000 0.02404(15) Uani 1 8 d S . . P P -0.14215(15) -0.16603(15) 0.5000 0.0425(4) Uani 1 2 d S . . O1 O -0.2792(4) -0.1133(5) 0.5000 0.0642(16) Uani 1 2 d S . . O2 O -0.1301(4) -0.2619(3) 0.4352(3) 0.0686(12) Uani 1 1 d . . . C11 C -0.3943(9) -0.1895(11) 0.5000 0.166(10) Uani 1 2 d S . . H11A H -0.4593 -0.1361 0.4769 0.199 Uiso 0.50 1 calc PR . . H11B H -0.3780 -0.2587 0.4649 0.199 Uiso 0.50 1 calc PR . . C12 C -0.4429(13) -0.236(2) 0.4502(18) 0.191(17) Uani 0.50 1 d P . . H12A H -0.4532 -0.1500 0.4323 0.286 Uiso 0.50 1 calc PR . . H12B H -0.5125 -0.2880 0.4323 0.286 Uiso 0.50 1 calc PR . . H12C H -0.3632 -0.2704 0.4323 0.286 Uiso 0.50 1 calc PR . . C21 C -0.1345(8) -0.2173(7) 0.3600(5) 0.089(2) Uani 1 1 d . . . H21A H -0.0675 -0.1545 0.3515 0.107 Uiso 1 1 calc R . . H21B H -0.2166 -0.1773 0.3499 0.107 Uiso 1 1 calc R . . C22 C -0.1159(8) -0.3294(9) 0.3103(6) 0.120(4) Uani 1 1 d . . . H22A H -0.0402 -0.3751 0.3254 0.181 Uiso 1 1 calc R . . H22B H -0.1064 -0.3008 0.2595 0.181 Uiso 1 1 calc R . . H22C H -0.1889 -0.3850 0.3139 0.181 Uiso 1 1 calc R . . F1 F -0.032(6) 0.093(2) 0.8381(17) 0.34(2) Uani 0.50 1 d P . . F2 F -0.042(3) -0.0857(19) 0.771(2) 0.32(2) Uani 0.50 1 d P . . B1 B 0.0000 0.0000 0.8099(7) 0.116(8) Uani 1 4 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 Pt 0.02706(17) 0.02706(17) 0.01798(19) 0.000 0.000 0.000 P 0.0325(8) 0.0319(8) 0.0632(10) 0.000 0.000 -0.0028(6) O1 0.030(2) 0.039(3) 0.124(5) 0.000 0.000 -0.0062(19) O2 0.061(2) 0.045(2) 0.100(3) -0.029(2) -0.023(2) 0.0000(17) C11 0.035(5) 0.058(6) 0.40(3) 0.000 0.000 -0.017(4) C12 0.039(7) 0.159(19) 0.37(5) -0.14(2) -0.007(13) -0.035(9) C21 0.083(5) 0.095(5) 0.090(5) -0.050(4) -0.015(4) 0.005(4) C22 0.090(6) 0.131(7) 0.141(8) -0.099(7) 0.006(5) -0.010(5) F1 0.56(6) 0.097(16) 0.37(4) -0.10(2) 0.09(7) 0.14(3) F2 0.19(3) 0.122(18) 0.66(7) -0.13(3) -0.11(5) 0.021(19) B1 0.166(13) 0.166(13) 0.015(5) 0.000 0.000 0.000 _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 Pt P 2.3276(16) . ? Pt P 2.3276(16) 9_556 ? Pt P 2.3276(16) 10_556 ? Pt P 2.3276(16) 2 ? P O1 1.564(5) . ? P O2 1.565(4) . ? P O2 1.565(4) 11_556 ? O1 C11 1.470(11) . ? O2 C21 1.451(10) . ? C11 C12 1.16(2) . ? C21 C22 1.511(9) . ? F1 B1 1.163(13) . ? F2 B1 1.24(3) . ? 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 P Pt P 180.00(5) . 9_556 ? P Pt P 90.0 . 10_556 ? P Pt P 90.0 9_556 10_556 ? P Pt P 90.0 . 2 ? P Pt P 90.0 9_556 2 ? P Pt P 180.0 10_556 2 ? O1 P O2 108.12(19) . . ? O1 P O2 108.12(19) . 11_556 ? O2 P O2 97.8(4) . 11_556 ? O1 P Pt 109.52(19) . . ? O2 P Pt 116.23(18) . . ? O2 P Pt 116.23(18) 11_556 . ? C11 O1 P 125.4(6) . . ? C21 O2 P 119.7(4) . . ? C12 C11 O1 127.7(13) 11_556 . ? O2 C21 C22 107.6(7) . . ? F1 B1 F1 78.8(14) 4 . ? F1 B1 F1 128(3) 4 2 ? F1 B1 F1 78.8(14) . 2 ? F1 B1 F1 78.8(14) 4 3 ? F1 B1 F1 128(3) . 3 ? F1 B1 F1 78.8(14) 2 3 ? F1 B1 F2 141(3) 4 . ? F1 B1 F2 140(3) . . ? F1 B1 F2 74(3) 2 . ? F1 B1 F2 75(3) 3 . ? F1 B1 F2 140(3) 4 4 ? F1 B1 F2 74(3) . 4 ? F1 B1 F2 75(3) 2 4 ? F1 B1 F2 141(3) 3 4 ? F2 B1 F2 71(2) . 4 ? F1 B1 F2 74(3) 4 3 ? F1 B1 F2 75(3) . 3 ? F1 B1 F2 141(3) 2 3 ? F1 B1 F2 140(3) 3 3 ? F2 B1 F2 110(4) . 3 ? F2 B1 F2 71(2) 4 3 ? F1 B1 F2 75(3) 4 2 ? F1 B1 F2 141(3) . 2 ? F1 B1 F2 140(3) 2 2 ? F1 B1 F2 74(3) 3 2 ? F2 B1 F2 71(2) . 2 ? F2 B1 F2 110(4) 4 2 ? F2 B1 F2 71(2) 3 2 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.409 _refine_diff_density_min -1.558 _refine_diff_density_rms 0.140